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Restraint data statistics:

No restraints used

Powder data statistics

Fitted

Bank Ndata Sum(w*d**2) wRp


Hstgm 1 PXC 1 3991 5019.7
Powder totals

3991 5019.7

-Bknd
Rp

Average

wRp

Rp

DWd Integral

0.0394 0.0312 0.0390 0.0337 1.555 0.895


0.0394 0.0312 0.0390 0.0337 1.555

No serial correlation in fit at 90% confidence for 1.909 < DWd < 2.091
Cycle 129 There were 3991 observations.
Total before-cycle CHI**2 (offset/sig) = 5.0197E+03 ( 1.1704E+01)
Reduced CHI**2 = 1.263

for 15 variables

Reflection data statistics


Histogram 1 Type PXC Nobs= 90 R(F**2) = 0.0411

The value of the determinant is 0.6488*10.0**(

-2)

Atom parameters for phase no. 1


frac
x
y
100*U12 100*U13 100*U23

100*Uiso 100*U11 100*U22 100*U33

Calculated unit cell formula weight: 320.394, density: 6.572gm/cm**3

Atom parameters for phase no. 2


frac
x
y
100*U12 100*U13 100*U23
ZN

100*Uiso 100*U11 100*U22 100*U33

( 1) Values : 1.003 0.333300 0.666700 0.000000


Sigmas :

0.095

Shft/esd:

0.00

0.827

Zn

moved 0.00A

sum(shift/e.s.d)**2 :

0.00

( 2) Values : 0.971 0.333300 0.666700 0.383000 -1.288


Sigmas :

0.272

Shft/esd:

0.00

moved 0.00A

sum(shift/e.s.d)**2 :

0.00

Atomic parameter sum(shift/error)**2 for phase 2 :

0.00

Calculated unit cell formula weight: 162.171, density: 5.680gm/cm**3

Atom parameters for phase no. 3


frac
x
y
100*U12 100*U13 100*U23
FE

Fe

100*Uiso 100*U11 100*U22 100*U33

( 1) Values : 1.000 0.000000 0.000000 0.000000


Sigmas :

0.165

Shft/esd:

0.00

moved 0.00A

sum(shift/e.s.d)**2 :

1.785

0.00

Atomic parameter sum(shift/error)**2 for phase 3 :

0.00

Calculated unit cell formula weight: 111.646, density: 7.883gm/cm**3

Phase/element fractions for phase no. 1

Hist Elem:
Fraction :

1 1 PXC
81.7186

Sigmas : 0.282992
Shift/esd:

0.00

Wt. Frac.:

0.61988

Sigmas : 0.815984E-03

1GSAS S-1
22:33:42 2011 Page 9

GENLES Version Win32 Dec 09

(first 1972236 characters in file skipped)


nst:

1.000 3

Histogram scale factors:

Hist/Typ:

1 PXC

pn

Scale : 0.99851

Dmp/Cnst:

1.000 4

1GSAS S-1
18:45:24 2010 Page 4

GENLES Version Win32 May 01

Absorption coefficients for powder data:

Hist/Typ:

1 PXC

0 pn

Absc 1. :

0.0000

Dmp/Cnst:
Absc 2. :
Dmp/Cnst:

0.000 0

0.0000
0

0.000 0

Diffractometer constants for powder data:


No. Type Lam 1
Lam 2
Kratio pn Cnstr cn Damp
1 PXC 1.7889600 1.7928500
0.5000 0 0.000 0 0

Polariz. pn Cnstr cn type


0.50000 0 0.000 0 0

Extinction coefficients for phase no. 1:

Zero pn Cnstr cn
0.000 0 0.000 0

Hist/Typ:

1 PXC

pn

Extinct.:

0.0000

Dmp/Cnst:

0.000 0

Extinction coefficients for phase no. 2:

Hist/Typ:

1 PXC

pn

Extinct.:

0.0000

Dmp/Cnst:

0.000 0

Extinction coefficients for phase no. 3:

Hist/Typ:

1 PXC

pn

Extinct.:

0.0000

Dmp/Cnst:

0.000 0

Radiation damage coefficients for phase no. 1:

Hist/Typ:

1 PXC

Rad.dam.:

0.0000

Dmp/Cnst:

pn
0

0.000 0

Radiation damage coefficients for phase no. 2:


1GSAS S-1
18:45:24 2010 Page 5

Hist/Typ:

1 PXC

pn

GENLES Version Win32 May 01

Rad.dam.:

0.0000

Dmp/Cnst:

0.000 0

Radiation damage coefficients for phase no. 3:

Hist/Typ:

1 PXC

pn

Rad.dam.:

0.0000

Dmp/Cnst:

0.000 0

Preferred orientation coeffs. for phase no. 1 histogram no. 1:


Axis

pn

Dir./typ:

0.0 2.0 1.0 0

PO ratio:

1.0324 A

Dmp/Cnst:

1.000 5

PO frac.:

1.0000 0

Dmp/Cnst:

0.000 0

Preferred orientation coeffs. for phase no. 2 histogram no. 1:


Axis

pn

Dir./typ:

1.0 1.0 0.0 0

PO ratio:

0.9457 B

Dmp/Cnst:

1.000 6

PO frac.:

1.0000 0

Dmp/Cnst:

0.000 0

Preferred orientation coeffs. for phase no. 3 histogram no. 1:


Axis

Dir./typ:

pn

0.0 0.0 1.0 0

PO ratio:

1.0000 0

Dmp/Cnst:

0.000 0

PO frac.:

1.0000 0

Dmp/Cnst:

0.000 0

Profile coeff. for function type 4, phase no. 1 and histogram no. 1; aniso. axis
0. 0. 1.; damp= 0:
Coeff. :
trns pn

GU pn
shft pn

GV

pn

GW

pn

GP

pn

LX

pn

ptec pn

Value : 2.000E+00 0-2.000E+00 0 1.036E+02 0 0.000E+00 0 1.207E+01


0 0.000E+00 0 0.000E+00 0 1.747E+01 C
Constr. :
0.000 0
Coeff. :
S3 pn

0.000 0
1.000 7
sfec pn
S4 pn

0.000 0
S/L

pn

0.000 0
H/L

pn

0.000 0
eta

pn

0.000 0
S1

pn

0.000 0
S2

pn

Value : 0.000E+00 0 5.000E-04 0 5.000E-04 0 0.000E+00 0 0.000E+00


0 5.049E-01 0 0.000E+00 0-2.411E-01 0
Constr. :
0.000 0
Coeff. :

0.000 0
0.000 0
S5

pn

0.000 0
S6

pn

0.000 0
S7

pn

0.000 0
S8

pn

0.000 0
S9

0.000 0

pn

Value :-3.408E-02 0-1.273E-01 0-8.214E-02 0 1.041E-01 0 2.302E-01 0


Constr. :

0.000 0

0.000 0

0.000 0

1GSAS S-1
18:45:24 2010 Page 6

0.000 0

0.000 0

GENLES Version Win32 May 01

Profile coeff. for function type 2, phase no. 2 and histogram no. 1; aniso. axis
0. 0. 1.; damp= 0:
Coeff. :
asym pn

GU pn
shft pn

GV

pn

GW

pn

LX

pn

LY

pn

trns pn

Value : 2.000E+00 0-2.000E+00 0 1.161E+02 0 8.825E-01 0 0.000E+00


0 0.000E+00 0 0.000E+00 0 1.851E+01 D

Constr. :
0.000 0

0.000 0
1.000 8

Coeff. :
L33 pn

GP
L12

pn
pn

0.000 0
stec pn

0.000 0
ptec pn

0.000 0
sfec pn

0.000 0
L11

pn

0.000 0
L22

pn

Value : 0.000E+00 0 0.000E+00 0 0.000E+00 0 0.000E+00 0 2.014E-02


0 0.000E+00 0 4.535E-02 0-8.464E+00 0
Constr. :
0.000 0
Coeff. :

0.000 0
0.000 0
L13

pn

0.000 0
L23

0.000 0

0.000 0

0.000 0

0.000 0

pn

Value :-4.954E-02 0-6.352E+00 0


Constr. :

0.000 0

0.000 0

Profile coeff. for function type 2, phase no. 3 and histogram no. 1; aniso. axis
0. 0. 1.; damp= 0:
Coeff. :
asym pn

GU pn
shft pn

GV

pn

GW

pn

LX

pn

LY

pn

trns pn

Value : 2.000E+00 0-2.000E+00 0 7.228E+01 0 3.833E+00 0 0.000E+00


0 0.000E+00 0 0.000E+00 0 1.148E+01 E
Constr. :
0.000 0

0.000 0
1.000 9

Coeff. :
L33 pn

GP
L12

pn
pn

0.000 0
stec pn

0.000 0
ptec pn

0.000 0
sfec pn

0.000 0
L11

pn

0.000 0
L22

pn

Value : 0.000E+00 0 0.000E+00 0 0.000E+00 0 0.000E+00 0 0.000E+00


0 3.172E-01 0 0.000E+00 0-1.430E-01 0
Constr. :
0.000 0
Coeff. :

0.000 0
0.000 0
L13

pn

0.000 0
L23

0.000 0

0.000 0

pn

Value :-3.592E+00 0 0.000E+00 0


Constr. :

0.000 0

0.000 0

Diffuse scattering coefficients for powder data:


No diffuse scattering coefficients for histogram

0.000 0

0.000 0

Background coefficients for powder data:


Histogram no.:

1 Damping factor:

0 Use all points: Y

Linear interpolation
Param. :
pn

1 pn

2 pn

3 pn

4 pn

5 pn

Coeff. : 0.66743E+03 0 0.67999E+03 0 0.68187E+03 0 0.70354E+03 0


0.71592E+03 0 0.71593E+03 0
Param. :
pn

7 pn

8 pn

9 pn

10 pn

11 pn

12

Coeff. : 0.71466E+03 0 0.73392E+03 0 0.75705E+03 0 0.69764E+03 0


0.75140E+03 0 0.73024E+03 0
Param. :
pn

13 pn

14 pn

15 pn

16 pn

17 pn

18

Coeff. : 0.72182E+03 0 0.72428E+03 0 0.72155E+03 0 0.70853E+03 0


0.70658E+03 0 0.70277E+03 0
Param. :
pn

19 pn

20 pn

21 pn

22 pn

23 pn

24

Coeff. : 0.69659E+03 0 0.71276E+03 0 0.70310E+03 0 0.71566E+03 0


0.68628E+03 0 0.71041E+03 0
Param. :
pn

25 pn

26 pn

27 pn

28 pn

29 pn

30

Coeff. : 0.69872E+03 0 0.70164E+03 0 0.72888E+03 0 0.73948E+03 0


0.67207E+03 0 0.69605E+03 0
Param. :
pn

31 pn

32 pn

33 pn

34 pn

35 pn

36

Coeff. : 0.67761E+03 0 0.69697E+03 0 0.67072E+03 0 0.67243E+03 0


0.66768E+03 0 0.72771E+03 0

The constraint matrix has 14 terms


1GSAS S-1
18:45:24 2010 Page 7

Restraint data statistics:

GENLES Version Win32 May 01

No restraints used

Powder data statistics

Fitted

Bank Ndata Sum(w*d**2) wRp


DWd Integral
Hstgm 1 PXC 1 3991 5243.5
0 1.497 0.895
Powder totals
0 1.497

3991 5243.5

-Bknd
Rp

pFree

wRp

Rp

Average

wRp

Rp Npfree

0.0403 0.0319 0.0392 0.0342 0.0000 0.0000


0.0403 0.0319 0.0392 0.0342 0.0000 0.0000

No serial correlation in fit at 90% confidence for 1.908 < DWd < 2.092
Cycle 120 There were 3991 observations.
Total before-cycle CHI**2 (offset/sig) = 5.2435E+03 ( 1.4201E+01)
Reduced CHI**2 = 1.318

for 14 variables

Reflection data statistics


Histogram 1 Type PXC Nobs = 90 R(F**2) = 0.1044
After matrix normalization and Marquardt modification:
Full matrix recip. condition value & -log10 = 0.2790E-06

The value of the determinant is 1.3328*10.0**(

6.55

-8)

Atom parameters for phase no. 1


frac
x
y
100*U12 100*U13 100*U23
CU

Cu

100*Uiso 100*U11 100*U22 100*U33

( 1) Values : 1.000 0.250000 0.250000 0.000000


Sigmas :

0.095

Shft/esd:

0.00

moved 0.00A

sum(shift/e.s.d)**2 :

0.00

1.767

( 2) Values : 1.035 0.000000 -0.584000 0.250000


Sigmas :

0.274

Shft/esd:

0.00

moved 0.00A

sum(shift/e.s.d)**2 :

3.565

0.00

Atomic parameter sum(shift/error)**2 for phase 1 :

0.00

Calculated unit cell formula weight: 320.394, density: 6.572gm/cm**3

Atom parameters for phase no. 2


frac
x
y
100*U12 100*U13 100*U23
ZN

Zn

100*Uiso 100*U11 100*U22 100*U33

( 1) Values : 1.003 0.333300 0.666700 0.000000


Sigmas :

0.103

Shft/esd:

0.00

moved 0.00A

sum(shift/e.s.d)**2 :

1.222

0.00

( 2) Values : 0.971 0.333300 0.666700 0.383000 -1.085


Sigmas :

0.281

Shft/esd:

0.00

moved 0.00A

sum(shift/e.s.d)**2 :

0.00

Atomic parameter sum(shift/error)**2 for phase 2 :

0.00

Calculated unit cell formula weight: 162.171, density: 5.680gm/cm**3


1GSAS S-1
18:45:25 2010 Page 8

Atom parameters for phase no. 3

GENLES Version Win32 May 01

frac
x
y
100*U12 100*U13 100*U23
FE

Fe

100*Uiso 100*U11 100*U22 100*U33

( 1) Values : 1.000 0.000000 0.000000 0.000000


Sigmas :

0.174

Shft/esd:

0.00

moved 0.00A

sum(shift/e.s.d)**2 :

1.984

0.00

Atomic parameter sum(shift/error)**2 for phase 3 :

0.00

Calculated unit cell formula weight: 111.646, density: 7.884gm/cm**3

Phase/element fractions for phase no. 1

Hist Elem:

1 1 PXC

Fraction :

80.8896

Sigmas :

109.844

Shift/esd:

0.00

Wt. Frac.:

0.62119

Sigmas : 0.319542

Phase/element fractions for phase no. 2

Hist Elem:

1 1 PXC

Fraction :

71.9441

Sigmas :

97.6995

Shift/esd:

0.00

Wt. Frac.:

0.27965

Sigmas : 0.273563

Phase/element fractions for phase no. 3

Hist Elem:

1 1 PXC

Fraction :

37.0545

Sigmas :

50.3239

Shift/esd:

0.00

Wt. Frac.:

0.99159E-01

Sigmas : 0.121315
Phase/element fraction sum(shift/error)**2 :

0.00

Histogram scale factors:

Histogram:
Scale

1 PXC

: 0.998333

Sigmas :

1.35618

Shift/esd:

0.00

Histogram scale factor sum(shift/error)**2 :

0.00

Preferred orientation coeffs. for phase no. 1 axis no. 1:

Histogram:
Ratio

1 PXC
1.03

Sigmas :

0.604E-02

Shift/esd:

0.00

Fraction :

1.00

Sigmas :

0.00

Shift/esd:

0.00

Preferred orientation coeffs. for phase no. 2 axis no. 1:

Histogram:
Ratio

1 PXC
0.946

Sigmas :

0.580E-02

Shift/esd:

0.00

Fraction :

1.00

Sigmas :

0.00

Shift/esd:

0.00

Preferred orientation sum(shift/error)**2 :

0.00

1GSAS S-1
18:45:25 2010 Page 9

GENLES Version Win32 May 01

Profile coefficients for histogram no. 1 and for phase no. 1:


Coeff. :
GU
sfec
S/L

GV

GW

GP

LX

ptec

trns

shft

Value : 2.000E+00 -2.000E+00 1.036E+02 0.000E+00 1.207E+01


0.000E+00 0.000E+00 1.747E+01 0.000E+00 5.000E-04
Sigmas :

8.120E-02

Shift/esd:

0.01

Coeff. :
S8

H/L

eta

S1

S2

S3

S4

S5

S6

S7

Value : 5.000E-04 0.000E+00 0.000E+00 5.049E-01 0.000E+00 -2.411E-01


-3.408E-02 -1.273E-01 -8.214E-02 1.041E-01
Sigmas :
Shift/esd:
Coeff. :
Value

S9

: 2.302E-01

Sigmas :
Shift/esd:

Profile coefficients for histogram no. 1 and for phase no. 2:


Coeff. :
GU
GP
stec

GV

GW

LX

LY

trns

asym

shft

Value : 2.000E+00 -2.000E+00 1.161E+02 8.825E-01 0.000E+00


0.000E+00 0.000E+00 1.850E+01 0.000E+00 0.000E+00
Sigmas :

7.302E-02

Shift/esd:

-0.03

Coeff. :

ptec

sfec

L11

L22

L33

L12

L13

L23

Value : 0.000E+00 0.000E+00 2.014E-02 0.000E+00 4.535E-02


-8.464E+00 -4.954E-02 -6.352E+00
Sigmas :
Shift/esd:

Profile coefficients for histogram no. 1 and for phase no. 3:


Coeff. :
GU
GP
stec

GV

GW

LX

LY

trns

asym

shft

Value : 2.000E+00 -2.000E+00 7.228E+01 3.833E+00 0.000E+00


0.000E+00 0.000E+00 1.148E+01 0.000E+00 0.000E+00
Sigmas :

1.402E-01

Shift/esd:

0.01

Coeff. :

ptec

sfec

L11

L22

L33

L12

L13

L23

Value : 0.000E+00 0.000E+00 0.000E+00 3.172E-01 0.000E+00 -1.430E01 -3.592E+00 0.000E+00


Sigmas :
Shift/esd:
Profile coef. sum(shift/error)**2 :

CPU times for matrix build

0.00

0.41 sec; matrix inversion

Final variable sum((shift/esd)**2) for cycle 120:

0.02 sec

0.00 Time:

0.42 sec

Convergence was achieved


1GSAS S-1
18:55:41 2010 Page 1

Version

May 01

|---------------------------------------------------------|
|

Program POWPREF Version Win32

| Prepares powder histograms for least-squares refinement |


|

Distributed on Mon Nov 12 12:16:14 2007

|---------------------------------------------------------|

|---------------------------------------------------------------|
|

Allen C. Larson and Robert B. Von Dreele

Manuel Lujan, Jr. Neutron Scattering Center, MS-H805

Los Alamos National Laboratory, Los Alamos, NM 87545

|
|

| Copyright, 2000, The Regents of the University of California. |


|---------------------------------------------------------------|

The last history record is :


HSTRY140 GENLES Win32 May 01 18:45:24 2010 Sdsq= 0.524E+04 S/E=
0.144E-02
Data for bank 1 read from file S-1.raw
The powder pattern has 3991 channels with 1 bins per channel
Histogram weight factors are

1.00000

0.00000

No fixed background points for this powder pattern


The 2 excluded regions are (in deg):
Exclude

from:

0.0000

to:

from:

to:

from:

0.0000 99.8200 1000.0000

to:

from:

to:

Incident spectrum type 0 can be used in the region

0.000 deg to 180.000 deg

The minimum possible weighted residual for this histogram is 0.0351


Histogram no. 1 on file GSAS.P01
updated with new excluded regions, background and incident spectrum data.
CPU time = 0.02 to update histogram
Lattice parameters for phase 1 are:
a,b,c = 4.679209 3.422292 5.124918 angles =
volume =

90.000

99.466

90.000

90.000

90.000 120.000

90.000

90.000

80.951

Lattice parameters for phase 2 are:


a,b,c = 3.245163 3.245163 5.198840 angles =
volume =

47.414

Lattice parameters for phase 3 are:


a,b,c = 2.864996 2.864996 2.864996 angles =
volume =

23.516

Profile function 4 for phase no. 1 has the coefficients p1-p21:


0.200000E+01 -0.200000E+01 0.103617E+03 0.000000E+00
0.120660E+02 0.000000E+00 0.000000E+00 0.174719E+02
0.000000E+00 0.500000E-03 0.500000E-03 0.000000E+00
0.000000E+00 0.504909E+00 0.000000E+00 -0.241143E+00
-0.340766E-01 -0.127270E+00 -0.821388E-01 0.104068E+00

0.230237E+00
cutoff on the wings at 0.001 of maximum

Profile function 2 for phase no. 2 has the coefficients p1-p18:


0.200000E+01 -0.200000E+01 0.116135E+03 0.882512E+00
0.000000E+00 0.000000E+00 0.000000E+00 0.185045E+02
0.000000E+00 0.000000E+00 0.000000E+00 0.000000E+00

90.000

0.201354E-01 0.000000E+00 0.453468E-01 -0.846359E+01


-0.495414E-01 -0.635224E+01
cutoff on the wings at 0.001 of maximum

Profile function 2 for phase no. 3 has the coefficients p1-p18:


0.200000E+01 -0.200000E+01 0.722848E+02 0.383343E+01
0.000000E+00 0.000000E+00 0.000000E+00 0.114832E+02
0.000000E+00 0.000000E+00 0.000000E+00 0.000000E+00
0.000000E+00 0.317166E+00 0.000000E+00 -0.142965E+00
-0.359152E+01 0.000000E+00
cutoff on the wings at 0.001 of maximum

Minimum d-spacing used to generate reflections 1.1335 for phase 1


Minimum d-spacing used to generate reflections 1.1241 for phase 2
Minimum d-spacing used to generate reflections 1.1094 for phase 3
Minimum d-spacing used to generate reflections 1.1335 for phase 1
Minimum d-spacing used to generate reflections 1.1241 for phase 2
Minimum d-spacing used to generate reflections 1.1094 for phase 3
Minimum d-spacing for matching reflections 1.1692
Estimated number of reflections to be generated is 165
Number of reflections generated for phase 1 is

60

Number of reflections generated for phase 2 is

24

Number of reflections generated for phase 3 is

Total number of reflections generated for all phases is

90

CPU time = 0.02 sec. to generate reflections.


CPU time = 0.05 sec. to locate reflection limits.
CPU time = 0.00 sec. to match reflection ranges to powder pattern
The maximum number of reflections contributing to any profile point is 21

CPU time = 0.02 sec. to update file


1GSAS S-1
18:55:48 2010 Page 1

Version

May 01

|----------------------------------------------------|
|
|

Program GENLES Version Win32

General crystal structure refinement program

| Magnetic structure refinement added by M. Yethiraj |


| Revised and corrected by Larson and Von Dreele |
|

Distributed on Mon Nov 12 12:15:58 2007

|----------------------------------------------------|

|---------------------------------------------------------------|
|

Allen C. Larson and Robert B. Von Dreele

Manuel Lujan, Jr. Neutron Scattering Center, MS-H805

Los Alamos National Laboratory, Los Alamos, NM 87545

| Copyright, 2000, The Regents of the University of California. |


|---------------------------------------------------------------|

The experiment file is: GSAS.EXP


The last history record is :
HSTRY141 POWPREF Win32 May 01 18:55:41 2010
Maximum number of cycles is

I/SigI cut-off is 1.00


Structure factors will be extracted from histogram 1
using extraction method codes

The atomic and magnetic scattering factors for 4 types of atoms are:
Atom type b-len
c
g

a(1)

b(1)

a(2)

CU
0.772 13.3380 3.5828
1.6735 64.8126 1.1910

b(2)

7.1676

a(3)

0.2470

<j0> Mag. ff :
0.0909 34.9840
0.0000 0.0000 -0.0124

0.4088 11.4430

<j2> Mag. ff :
0.0000 0.0000

1.3329

1.9182 14.4900
0.0035 2.000

O
0.581 3.0485 13.2771
0.8670 32.9089 0.2508

2.2868

b(3)

0.5128

3.8250

0.3842
1.5463

1.6390
0.3239

ZN
0.568 14.0743 3.2655
2.4100 58.7097 1.3041

7.0318

0.2333

5.1652 10.3163

FE
0.945 11.7695 4.7611
2.3045 76.8805 1.0369

7.3573

0.3072

3.5222 15.3535

<j0> Mag. ff :
0.0706 35.0080
0.0000 0.0000 -0.0114

0.3589 15.3580

<j2> Mag. ff :
0.0000 0.0000

1.9566

6.3230

MoKa

AgKa

Atom type
WKa
AuKa
CU
0.058

1.9405 18.4730
0.0036 2.000

CrKa

FeKa

CuKa

f' -0.734 -1.070 -1.965


0.030
f"

0.320

0.5819
0.5166
TiKa

5.5610
2.1610

CoKa

0.324 -0.443 -1.279

TaKa
0.065

1.193
0.092

0.886

0.589

1.265

0.826

1.643

0.770

O
f' 0.093
-0.003 -0.003

0.072

0.049

0.011

0.006

0.121

0.063 -0.002

0.052

0.032

0.006

0.004

0.106

0.044

0.124

f"
0.000

0.073
0.000

ZN
0.065

f' -0.617 -0.913 -1.549


0.034
f"

0.143

1.371
0.106

1.019

0.678

FE
f' -1.294 -2.055 -1.134
0.039 0.017

0.284
1.430
0.346

0.324 -0.352 -1.084


0.938

b(4)

5.6158 11.3966

4.7300
5.7011

a(4)

1.886

0.886

0.289 -0.890 -3.331

0.133

0.000
0.072
0.153
0.044

f"
0.079

0.762
0.058

0.565

3.197

0.844

0.545

1GSAS S-1
18:55:48 2010 Page 2

1.052

0.490

0.084

GENLES Version Win32 May 01

Space group C 1 2/c 1


The lattice is centric C-centered monoclinic

Laue symmetry 2/m

Multiplicity of a general site is 8


The unique axis is b
The symmetry of the point 0,0,0 contains 1bar

The equivalent positions are:

( 1)

Z ( 2)

-X

Y 1/2-Z

The atom positions read in are: (all variable numbers (pn) are in hexadecimal)

Type seq. At. name mult symm frac pn


u22 pn u33 pn u12 pn u13 pn u23 pn
CU
O

1 Cu
2O

4 -1

pn

pn

pn u11 pn

1.0000 0 0.2500 0 0.2500 0 0.0000 0 1.8 1

4 2(010) 1.0346 0 0.0000 0-0.5840 0 0.2500 0 3.6 2

Space group P 63 m c
The lattice is acentric primitive hexagonal
Multiplicity of a general site is 12
The location of the origin is arbitrary in z

Laue symmetry 6/mmm

The equivalent positions are:

( 1)

( 4)

-X

( 7)

Y-X

(10)

X-Y

Z ( 2)

X-Y

-Y 1/2+Z ( 5)
Y

Z ( 8)

X 1/2+Z ( 3)

Y-X
-X

-Y 1/2+Z (11)

-X

-Y

X-Y

Z ( 6)

Y-X 1/2+Z

Y-X 1/2+Z ( 9)

-Y

-X

X-Y

Z (12)

Z
X 1/2+Z

The atom positions read in are: (all variable numbers (pn) are in hexadecimal)

Type seq. At. name mult symm frac pn


u22 pn u33 pn u12 pn u13 pn u23 pn
ZN
O

1 Zn

pn

pn

pn u11 pn

2 3M(100) 1.0027 0 0.3333 0 0.6667 0 0.0000 0 1.2 3

2O

2 3M(100) 0.9706 0 0.3333 0 0.6667 0 0.3830 0-1.1 4

Space group I m -3 m
The lattice is centric I-centered cubic

Laue symmetry m3m

Multiplicity of a general site is 96


The symmetry of the point 0,0,0 contains 1bar

The equivalent positions are:

( 1)

Z ( 2)

Y ( 3)

( 4)

-Z ( 5)

-Z

Y ( 6)

-Z

( 7)

-Z

-Y ( 8)

-Y

-Z

X ( 9)

-Z

-X

(10)

-X

-Z (11)

-Z

-X

Y (12)

-Y

-Z

(13)

Z (14)

X (15)

(16)

-Z (17)

-Z

X (18)

-Z

(19)

-Z

-X (20)

-X

-Z

Y (21)

-Z

-Y

(22)

-Y

-Z (23)

-Z

-Y

X (24)

1GSAS S-1
18:55:48 2010 Page 3

-X

-Z

GENLES Version Win32 May 01

The atom positions read in are: (all variable numbers (pn) are in hexadecimal)

Type seq. At. name mult symm frac pn


u22 pn u33 pn u12 pn u13 pn u23 pn
FE

1 Fe

pn

pn

2 M3M 0.9996 0 0.0000 0 0.0000 0 0.0000 0 2.0 5

Lattice parameters for phase 1 are:


a

alpha

beta

gamma

4.679209 3.422292 5.124918 90.0000 99.4660 90.0000

Lattice parameters for phase 2 are:


a

alpha

beta

gamma

3.245163 3.245163 5.198840 90.0000 90.0000 120.0000

Lattice parameters for phase 3 are:


a

alpha

beta

gamma

2.864996 2.864996 2.864996 90.0000 90.0000 90.0000

Phase/element fractions for phase no. 1

Hist Elm:

PXC 1 1 nc

Fraction:

80.890

Dmp/Cnst:

pn u11 pn

1.000 1

Phase/element fractions for phase no. 2

Hist Elm:

PXC 1 1 nc

Fraction:

71.944

Dmp/Cnst:

1.000 2

Phase/element fractions for phase no. 3

Hist Elm:

PXC 1 1 nc

Fraction:

37.054

Dmp/Cnst:

1.000 3

Histogram scale factors:

Hist/Typ:

1 PXC

pn

Scale : 0.99833

Dmp/Cnst:

1.000 4

1GSAS S-1
18:55:48 2010 Page 4

Absorption coefficients for powder data:

Hist/Typ:

1 PXC

0 pn

Absc 1. :

0.0000

Dmp/Cnst:
Absc 2. :
Dmp/Cnst:

0.000 0

0.0000
0

0.000 0

GENLES Version Win32 May 01

Diffractometer constants for powder data:


No. Type Lam 1
Lam 2
Kratio pn Cnstr cn Damp
1 PXC 1.7889600 1.7928500
0.5000 0 0.000 0 0

Polariz. pn Cnstr cn type


0.50000 0 0.000 0 0

Extinction coefficients for phase no. 1:

Hist/Typ:

1 PXC

pn

Extinct.:

0.0000

Dmp/Cnst:

0.000 0

Extinction coefficients for phase no. 2:

Hist/Typ:

1 PXC

pn

Extinct.:

0.0000

Dmp/Cnst:

0.000 0

Extinction coefficients for phase no. 3:

Hist/Typ:

1 PXC

pn

Extinct.:

0.0000

Dmp/Cnst:

0.000 0

Radiation damage coefficients for phase no. 1:

Hist/Typ:

1 PXC

Rad.dam.:

0.0000

Dmp/Cnst:

pn
0

0.000 0

Zero pn Cnstr cn
0.000 0 0.000 0

Radiation damage coefficients for phase no. 2:


1GSAS S-1
18:55:48 2010 Page 5

Hist/Typ:

1 PXC

GENLES Version Win32 May 01

pn

Rad.dam.:

0.0000

Dmp/Cnst:

0.000 0

Radiation damage coefficients for phase no. 3:

Hist/Typ:

1 PXC

pn

Rad.dam.:

0.0000

Dmp/Cnst:

0.000 0

Preferred orientation coeffs. for phase no. 1 histogram no. 1:


Axis

pn

Dir./typ:

0.0 2.0 1.0 0

PO ratio:

1.0324 A

Dmp/Cnst:

1.000 5

PO frac.:

1.0000 0

Dmp/Cnst:

0.000 0

Preferred orientation coeffs. for phase no. 2 histogram no. 1:


Axis

pn

Dir./typ:

1.0 1.0 0.0 0

PO ratio:

0.9457 B

Dmp/Cnst:

1.000 6

PO frac.:

1.0000 0

Dmp/Cnst:

0.000 0

Preferred orientation coeffs. for phase no. 3 histogram no. 1:


Axis

pn

Dir./typ:

0.0 0.0 1.0 0

PO ratio:

1.0000 0

Dmp/Cnst:

0.000 0

PO frac.:

1.0000 0

Dmp/Cnst:

0.000 0

Profile coeff. for function type 4, phase no. 1 and histogram no. 1; aniso. axis
0. 0. 1.; damp= 0:
Coeff. :
trns pn

GU pn
shft pn

GV

pn

GW

pn

GP

pn

LX

pn

ptec pn

Value : 2.000E+00 0-2.000E+00 0 1.036E+02 0 0.000E+00 0 1.207E+01


0 0.000E+00 0 0.000E+00 0 1.747E+01 C
Constr. :
0.000 0
Coeff. :
S3 pn

0.000 0
1.000 7
sfec pn
S4 pn

0.000 0
S/L

pn

0.000 0
H/L

pn

0.000 0
eta

pn

0.000 0
S1

pn

0.000 0
S2

pn

Value : 0.000E+00 0 5.000E-04 0 5.000E-04 0 0.000E+00 0 0.000E+00


0 5.049E-01 0 0.000E+00 0-2.411E-01 0
Constr. :
0.000 0
Coeff. :

0.000 0
0.000 0
S5

pn

0.000 0
S6

pn

0.000 0
S7

pn

0.000 0
S8

pn

0.000 0
S9

0.000 0

pn

Value :-3.408E-02 0-1.273E-01 0-8.214E-02 0 1.041E-01 0 2.302E-01 0


Constr. :

0.000 0

1GSAS S-1
18:55:48 2010 Page 6

0.000 0

0.000 0

0.000 0

0.000 0

GENLES Version Win32 May 01

Profile coeff. for function type 2, phase no. 2 and histogram no. 1; aniso. axis
0. 0. 1.; damp= 0:
Coeff. :
asym pn

GU pn
shft pn

GV

pn

GW

pn

LX

pn

LY

pn

trns pn

Value : 2.000E+00 0-2.000E+00 0 1.161E+02 0 8.825E-01 0 0.000E+00


0 0.000E+00 0 0.000E+00 0 1.850E+01 D
Constr. :
0.000 0

0.000 0
1.000 8

Coeff. :
L33 pn

GP
L12

pn
pn

0.000 0
stec pn

0.000 0
ptec pn

0.000 0
sfec pn

0.000 0
L11

pn

0.000 0
L22

pn

Value : 0.000E+00 0 0.000E+00 0 0.000E+00 0 0.000E+00 0 2.014E-02


0 0.000E+00 0 4.535E-02 0-8.464E+00 0
Constr. :
0.000 0
Coeff. :

0.000 0
0.000 0
L13

pn

0.000 0
L23

0.000 0

0.000 0

0.000 0

0.000 0

pn

Value :-4.954E-02 0-6.352E+00 0


Constr. :

0.000 0

0.000 0

Profile coeff. for function type 2, phase no. 3 and histogram no. 1; aniso. axis
0. 0. 1.; damp= 0:
Coeff. :
asym pn

GU pn
shft pn

GV

pn

GW

pn

LX

pn

LY

pn

trns pn

Value : 2.000E+00 0-2.000E+00 0 7.228E+01 0 3.833E+00 0 0.000E+00


0 0.000E+00 0 0.000E+00 0 1.148E+01 E
Constr. :
0.000 0

0.000 0
1.000 9

Coeff. :
L33 pn

GP
L12

pn
pn

0.000 0
stec pn

0.000 0
ptec pn

0.000 0
sfec pn

0.000 0
L11

pn

0.000 0
L22

pn

Value : 0.000E+00 0 0.000E+00 0 0.000E+00 0 0.000E+00 0 0.000E+00


0 3.172E-01 0 0.000E+00 0-1.430E-01 0
Constr. :
0.000 0

0.000 0
0.000 0

0.000 0

0.000 0

0.000 0

0.000 0

0.000 0

Coeff. :

L13

pn

L23

pn

Value :-3.592E+00 0 0.000E+00 0


Constr. :

0.000 0

0.000 0

Diffuse scattering coefficients for powder data:


No diffuse scattering coefficients for histogram

Background coefficients for powder data:


Histogram no.:

1 Damping factor:

0 Use all points: Y

Linear interpolation
Param. :
pn

1 pn

2 pn

3 pn

4 pn

5 pn

Coeff. : 0.66743E+03 0 0.67999E+03 0 0.68187E+03 0 0.70354E+03 0


0.71592E+03 0 0.71593E+03 0
Param. :
pn

7 pn

8 pn

9 pn

10 pn

11 pn

12

Coeff. : 0.71466E+03 0 0.73392E+03 0 0.75705E+03 0 0.69764E+03 0


0.75140E+03 0 0.73024E+03 0
Param. :
pn

13 pn

14 pn

15 pn

16 pn

17 pn

18

Coeff. : 0.72182E+03 0 0.72428E+03 0 0.72155E+03 0 0.70853E+03 0


0.70658E+03 0 0.70277E+03 0
Param. :
pn

19 pn

20 pn

21 pn

22 pn

23 pn

24

Coeff. : 0.69659E+03 0 0.71276E+03 0 0.70310E+03 0 0.71566E+03 0


0.68628E+03 0 0.71041E+03 0
Param. :
pn

25 pn

26 pn

27 pn

28 pn

29 pn

30

Coeff. : 0.69872E+03 0 0.70164E+03 0 0.72888E+03 0 0.73948E+03 0


0.67207E+03 0 0.69605E+03 0
Param. :
pn

31 pn

32 pn

33 pn

34 pn

35 pn

36

Coeff. : 0.67761E+03 0 0.69697E+03 0 0.67072E+03 0 0.67243E+03 0


0.66768E+03 0 0.72771E+03 0

The constraint matrix has 14 terms


1GSAS S-1
18:55:48 2010 Page 7

GENLES Version Win32 May 01

Restraint data statistics:


No restraints used

Powder data statistics

Fitted

Bank Ndata Sum(w*d**2) wRp


DWd Integral
Hstgm 1 PXC 1 3991 5243.5
0 1.497 0.895
Powder totals
0 1.497

3991 5243.5

-Bknd
Rp

pFree

wRp

Rp

Average

wRp

Rp Npfree

0.0403 0.0319 0.0392 0.0342 0.0000 0.0000


0.0403 0.0319 0.0392 0.0342 0.0000 0.0000

No serial correlation in fit at 90% confidence for 1.908 < DWd < 2.092
Cycle 121 There were 3991 observations.
Total before-cycle CHI**2 (offset/sig) = 5.2435E+03 ( 1.4201E+01)
Reduced CHI**2 = 1.318

for 14 variables

Reflection data statistics


Histogram 1 Type PXC Nobs = 90 R(F**2) = 0.1044
After matrix normalization and Marquardt modification:
Full matrix recip. condition value & -log10 = 0.1377E-06

The value of the determinant is 6.5781*10.0**(

-9)

6.86

Atom parameters for phase no. 1


frac
x
y
100*U12 100*U13 100*U23
CU

Cu

100*Uiso 100*U11 100*U22 100*U33

( 1) Values : 1.000 0.250000 0.250000 0.000000


Sigmas :

0.095

Shft/esd:

0.00

moved 0.00A

sum(shift/e.s.d)**2 :

0.00

( 2) Values : 1.035 0.000000 -0.584000 0.250000


Sigmas :

0.274

Shft/esd:

0.00

moved 0.00A

sum(shift/e.s.d)**2 :

1.767

3.565

0.00

Atomic parameter sum(shift/error)**2 for phase 1 :

0.00

Calculated unit cell formula weight: 320.394, density: 6.572gm/cm**3

Atom parameters for phase no. 2


frac
x
y
100*U12 100*U13 100*U23
ZN

Zn

100*Uiso 100*U11 100*U22 100*U33

( 1) Values : 1.003 0.333300 0.666700 0.000000


Sigmas :

0.103

Shft/esd:

0.00

moved 0.00A

sum(shift/e.s.d)**2 :

1.222

0.00

( 2) Values : 0.971 0.333300 0.666700 0.383000 -1.085


Sigmas :

0.281

Shft/esd:

0.00

moved 0.00A

sum(shift/e.s.d)**2 :

0.00

Atomic parameter sum(shift/error)**2 for phase 2 :

0.00

Calculated unit cell formula weight: 162.171, density: 5.680gm/cm**3


1GSAS S-1
18:55:49 2010 Page 8

GENLES Version Win32 May 01

Atom parameters for phase no. 3


frac
x
y
100*U12 100*U13 100*U23
FE

Fe

100*Uiso 100*U11 100*U22 100*U33

( 1) Values : 1.000 0.000000 0.000000 0.000000


Sigmas :

0.174

Shft/esd:

0.00

moved 0.00A

sum(shift/e.s.d)**2 :

1.984

0.00

Atomic parameter sum(shift/error)**2 for phase 3 :

0.00

Calculated unit cell formula weight: 111.646, density: 7.884gm/cm**3

Phase/element fractions for phase no. 1

Hist Elem:

1 1 PXC

Fraction :

80.8844

Sigmas :

156.384

Shift/esd:

0.00

Wt. Frac.:

0.62119

Sigmas : 0.454960

Phase/element fractions for phase no. 2

Hist Elem:

1 1 PXC

Fraction :

71.9394

Sigmas :

139.092

Shift/esd:

0.00

Wt. Frac.:

0.27965

Sigmas : 0.389489

Phase/element fractions for phase no. 3

Hist Elem:

1 1 PXC

Fraction :

37.0521

Sigmas :

71.6419

Shift/esd:

0.00

Wt. Frac.:

0.99159E-01

Sigmas : 0.172716
Phase/element fraction sum(shift/error)**2 :

0.00

Histogram scale factors:

Histogram:
Scale

1 PXC

: 0.998397

Sigmas :

1.93009

Shift/esd:

0.00

Histogram scale factor sum(shift/error)**2 :

0.00

Preferred orientation coeffs. for phase no. 1 axis no. 1:

Histogram:

1 PXC

Ratio

1.03

Sigmas :

0.604E-02

Shift/esd:

0.00

Fraction :

1.00

Sigmas :

0.00

Shift/esd:

0.00

Preferred orientation coeffs. for phase no. 2 axis no. 1:

Histogram:
Ratio

1 PXC
0.946

Sigmas :

0.580E-02

Shift/esd:

0.00

Fraction :

1.00

Sigmas :

0.00

Shift/esd:

0.00

Preferred orientation sum(shift/error)**2 :

0.00

1GSAS S-1
18:55:49 2010 Page 9

GENLES Version Win32 May 01

Profile coefficients for histogram no. 1 and for phase no. 1:


Coeff. :
GU
sfec
S/L

GV

GW

GP

LX

ptec

trns

shft

Value : 2.000E+00 -2.000E+00 1.036E+02 0.000E+00 1.207E+01


0.000E+00 0.000E+00 1.747E+01 0.000E+00 5.000E-04
Sigmas :

8.120E-02

Shift/esd:

0.00

Coeff. :
S8

H/L

eta

S1

S2

S3

S4

S5

S6

S7

Value : 5.000E-04 0.000E+00 0.000E+00 5.049E-01 0.000E+00 -2.411E-01


-3.408E-02 -1.273E-01 -8.214E-02 1.041E-01
Sigmas :
Shift/esd:
Coeff. :
Value

S9

: 2.302E-01

Sigmas :
Shift/esd:

Profile coefficients for histogram no. 1 and for phase no. 2:


Coeff. :
GU
GP
stec

GV

GW

LX

LY

trns

asym

shft

Value : 2.000E+00 -2.000E+00 1.161E+02 8.825E-01 0.000E+00


0.000E+00 0.000E+00 1.850E+01 0.000E+00 0.000E+00
Sigmas :

7.302E-02

Shift/esd:

0.00

Coeff. :

ptec

sfec

L11

L22

L33

L12

L13

L23

Value : 0.000E+00 0.000E+00 2.014E-02 0.000E+00 4.535E-02


-8.464E+00 -4.954E-02 -6.352E+00
Sigmas :
Shift/esd:

Profile coefficients for histogram no. 1 and for phase no. 3:


Coeff. :
GU
GP
stec

GV

GW

LX

LY

trns

asym

shft

Value : 2.000E+00 -2.000E+00 7.228E+01 3.833E+00 0.000E+00


0.000E+00 0.000E+00 1.148E+01 0.000E+00 0.000E+00
Sigmas :

1.402E-01

Shift/esd:

0.00

Coeff. :

ptec

sfec

L11

L22

L33

L12

L13

L23

Value : 0.000E+00 0.000E+00 0.000E+00 3.172E-01 0.000E+00 -1.430E01 -3.592E+00 0.000E+00


Sigmas :
Shift/esd:
Profile coef. sum(shift/error)**2 :

CPU times for matrix build

0.00

0.42 sec; matrix inversion

Final variable sum((shift/esd)**2) for cycle 121:

0.00 sec

0.00 Time:

0.42 sec

Version

May 01

Convergence was achieved

---------------------------------------------Archiving GSAS.EXP as GSAS.O5B


----------------------------------------------

1GSAS S-1
18:57:10 2010 Page 1

|---------------------------------------------------------|
|

Program POWPREF Version Win32

| Prepares powder histograms for least-squares refinement |


|

Distributed on Mon Nov 12 12:16:14 2007

|---------------------------------------------------------|

|---------------------------------------------------------------|
|

Allen C. Larson and Robert B. Von Dreele

Manuel Lujan, Jr. Neutron Scattering Center, MS-H805

Los Alamos National Laboratory, Los Alamos, NM 87545

|
|

| Copyright, 2000, The Regents of the University of California. |


|---------------------------------------------------------------|

The last history record is :


HSTRY143 EXPGUI 1.80 1.46 (4 changes) -- 05/01/10 18:57:09
Data for bank 1 read from file S-1.raw
The powder pattern has 3991 channels with 1 bins per channel
Histogram weight factors are

1.00000

0.00000

No fixed background points for this powder pattern


The 2 excluded regions are (in deg):
Exclude

from:

0.0000

to:

from:

to:

from:

to:

from:

to:

0.0000 99.8200 1000.0000

Incident spectrum type 0 can be used in the region

0.000 deg to 180.000 deg

The minimum possible weighted residual for this histogram is 0.0351


Histogram no. 1 on file GSAS.P01
updated with new excluded regions, background and incident spectrum data.
CPU time = 0.02 to update histogram
Lattice parameters for phase 1 are:
a,b,c = 4.679209 3.422292 5.124918 angles =
volume =

90.000

99.466

90.000

90.000

90.000 120.000

90.000

90.000

80.951

Lattice parameters for phase 2 are:


a,b,c = 3.245163 3.245163 5.198840 angles =
volume =

47.414

Lattice parameters for phase 3 are:


a,b,c = 2.864996 2.864996 2.864996 angles =
volume =

23.516

Profile function 4 for phase no. 1 has the coefficients p1-p21:

90.000

0.200000E+01 -0.200000E+01 0.103617E+03 0.000000E+00


0.120660E+02 0.000000E+00 0.000000E+00 0.174719E+02
0.000000E+00 0.500000E-03 0.500000E-03 0.000000E+00
0.000000E+00 0.504909E+00 0.000000E+00 -0.241143E+00
-0.340766E-01 -0.127270E+00 -0.821388E-01 0.104068E+00

0.230237E+00
cutoff on the wings at 0.001 of maximum

Profile function 2 for phase no. 2 has the coefficients p1-p18:


0.200000E+01 -0.200000E+01 0.116135E+03 0.882512E+00
0.000000E+00 0.000000E+00 0.000000E+00 0.185045E+02
0.000000E+00 0.000000E+00 0.000000E+00 0.000000E+00
0.201354E-01 0.000000E+00 0.453468E-01 -0.846359E+01
-0.495414E-01 -0.635224E+01
cutoff on the wings at 0.001 of maximum

Profile function 2 for phase no. 3 has the coefficients p1-p18:


0.200000E+01 -0.200000E+01 0.722848E+02 0.383343E+01
0.000000E+00 0.000000E+00 0.000000E+00 0.114832E+02
0.000000E+00 0.000000E+00 0.000000E+00 0.000000E+00
0.000000E+00 0.317166E+00 0.000000E+00 -0.142965E+00
-0.359152E+01 0.000000E+00
cutoff on the wings at 0.001 of maximum

Minimum d-spacing used to generate reflections 1.1335 for phase 1


Minimum d-spacing used to generate reflections 1.1241 for phase 2
Minimum d-spacing used to generate reflections 1.1094 for phase 3

Minimum d-spacing used to generate reflections 1.1335 for phase 1


Minimum d-spacing used to generate reflections 1.1241 for phase 2
Minimum d-spacing used to generate reflections 1.1094 for phase 3
Minimum d-spacing for matching reflections 1.1692
Estimated number of reflections to be generated is 165
Number of reflections generated for phase 1 is

60

Number of reflections generated for phase 2 is

24

Number of reflections generated for phase 3 is

Total number of reflections generated for all phases is

90

CPU time = 0.00 sec. to generate reflections.


CPU time = 0.06 sec. to locate reflection limits.
CPU time = 0.00 sec. to match reflection ranges to powder pattern
The maximum number of reflections contributing to any profile point is 21
CPU time = 0.00 sec. to update file
1GSAS S-1
18:57:20 2010 Page 1

Version

May 01

|----------------------------------------------------|
|
|

Program GENLES Version Win32

General crystal structure refinement program

| Magnetic structure refinement added by M. Yethiraj |


| Revised and corrected by Larson and Von Dreele |
|

Distributed on Mon Nov 12 12:15:58 2007

|----------------------------------------------------|

|---------------------------------------------------------------|
|
|

Allen C. Larson and Robert B. Von Dreele

Manuel Lujan, Jr. Neutron Scattering Center, MS-H805

Los Alamos National Laboratory, Los Alamos, NM 87545

| Copyright, 2000, The Regents of the University of California. |


|---------------------------------------------------------------|

The experiment file is: GSAS.EXP


The last history record is :
HSTRY144 POWPREF Win32 May 01 18:57:10 2010
Maximum number of cycles is

I/SigI cut-off is 1.00


Structure factors will be extracted from histogram 1
using extraction method codes

The atomic and magnetic scattering factors for 4 types of atoms are:
Atom type b-len
c
g

a(1)

b(1)

CU
0.772 13.3380 3.5828
1.6735 64.8126 1.1910

a(2)

b(2)

7.1676

a(3)

0.2470

<j0> Mag. ff :
0.0909 34.9840
0.0000 0.0000 -0.0124

0.4088 11.4430

<j2> Mag. ff :
0.0000 0.0000

1.3329

1.9182 14.4900
0.0035 2.000

O
0.581 3.0485 13.2771
0.8670 32.9089 0.2508

2.2868

4.7300
5.7011

b(3)

a(4)

5.6158 11.3966
0.5128
0.3842
1.5463

3.8250
1.6390
0.3239

ZN
0.568 14.0743 3.2655
2.4100 58.7097 1.3041

7.0318

0.2333

5.1652 10.3163

FE
0.945 11.7695 4.7611
2.3045 76.8805 1.0369

7.3573

0.3072

3.5222 15.3535

<j0> Mag. ff :
0.0706 35.0080
0.0000 0.0000 -0.0114

0.3589 15.3580

<j2> Mag. ff :
0.0000 0.0000

1.9566

1.9405 18.4730
0.0036 2.000

6.3230

0.5819
0.5166

5.5610
2.1610

b(4)

Atom type
WKa
AuKa
CU
0.058

CrKa

FeKa

CuKa

f' -0.734 -1.070 -1.965


0.030
f"

MoKa
0.320

AgKa

TiKa

CoKa

0.324 -0.443 -1.279

TaKa
0.065

1.193
0.092

0.886

0.589

1.265

0.826

1.643

0.770

O
f' 0.093
-0.003 -0.003

0.072

0.049

0.011

0.006

0.121

0.063 -0.002

0.052

0.032

0.006

0.004

0.106

0.044

0.124

f"
0.000

0.073
0.000

ZN
0.065

f' -0.617 -0.913 -1.549


0.034
f"

0.143

1.371
0.106

1.019

0.678

FE
f' -1.294 -2.055 -1.134
0.039 0.017
f"
0.079

0.762
0.058

0.565

3.197

0.284
1.430
0.346
0.844

0.324 -0.352 -1.084


0.938

1.886

0.886

0.289 -0.890 -3.331


0.545

1GSAS S-1
18:57:20 2010 Page 2

1.052

0.490

The lattice is centric C-centered monoclinic

Laue symmetry 2/m

Multiplicity of a general site is 8


The unique axis is b
The symmetry of the point 0,0,0 contains 1bar

The equivalent positions are:

Z ( 2)

0.000
0.072
0.153
0.044
0.084

GENLES Version Win32 May 01

Space group C 1 2/c 1

( 1)

0.133

-X

Y 1/2-Z

The atom positions read in are: (all variable numbers (pn) are in hexadecimal)

Type seq. At. name mult symm frac pn


u22 pn u33 pn u12 pn u13 pn u23 pn
CU
O

1 Cu

4 -1

2O

pn

pn

pn u11 pn

1.0000 0 0.2500 0 0.2500 0 0.0000 0 1.8 1

4 2(010) 1.0346 0 0.0000 0-0.5840 0 0.2500 0 3.6 2

Space group P 63 m c
The lattice is acentric primitive hexagonal

Laue symmetry 6/mmm

Multiplicity of a general site is 12


The location of the origin is arbitrary in z

The equivalent positions are:

( 1)

( 4)

-X

( 7)

Y-X

(10)

X-Y

Z ( 2)

X-Y

-Y 1/2+Z ( 5)
Y

Z ( 8)

X 1/2+Z ( 3)

Y-X
-X

-Y 1/2+Z (11)

-X

-Y

X-Y

Z ( 6)

Y-X 1/2+Z

Y-X 1/2+Z ( 9)

-Y

-X

X-Y

Z (12)

Z
X 1/2+Z

The atom positions read in are: (all variable numbers (pn) are in hexadecimal)

Type seq. At. name mult symm frac pn


u22 pn u33 pn u12 pn u13 pn u23 pn
ZN
O

1 Zn
2O

pn

pn

pn u11 pn

2 3M(100) 1.0027 0 0.3333 0 0.6667 0 0.0000 0 1.2 3


2 3M(100) 0.9706 0 0.3333 0 0.6667 0 0.3830 0-1.1 4

Space group I m -3 m

The lattice is centric I-centered cubic

Laue symmetry m3m

Multiplicity of a general site is 96


The symmetry of the point 0,0,0 contains 1bar

The equivalent positions are:

( 1)

Z ( 2)

Y ( 3)

( 4)

-Z ( 5)

-Z

Y ( 6)

-Z

( 7)

-Z

-Y ( 8)

-Y

-Z

X ( 9)

-Z

-X

(10)

-X

-Z (11)

-Z

-X

Y (12)

-Y

-Z

(13)

Z (14)

X (15)

(16)

-Z (17)

-Z

X (18)

-Z

(19)

-Z

-X (20)

-X

-Z

Y (21)

-Z

-Y

(22)

-Y

-Z (23)

-Z

-Y

X (24)

-X

-Z

1GSAS S-1
18:57:20 2010 Page 3

GENLES Version Win32 May 01

The atom positions read in are: (all variable numbers (pn) are in hexadecimal)

Type seq. At. name mult symm frac pn


u22 pn u33 pn u12 pn u13 pn u23 pn
FE

1 Fe

pn

pn

2 M3M 0.9996 0 0.0000 0 0.0000 0 0.0000 0 2.0 5

Lattice parameters for phase 1 are:


a

pn u11 pn

alpha

beta

gamma

4.679209 3.422292 5.124918 90.0000 99.4660 90.0000

Lattice parameters for phase 2 are:


a

alpha

beta

gamma

3.245163 3.245163 5.198840 90.0000 90.0000 120.0000

Lattice parameters for phase 3 are:


a

alpha

beta

gamma

2.864996 2.864996 2.864996 90.0000 90.0000 90.0000

Phase/element fractions for phase no. 1

Hist Elm:

PXC 1 1 nc

Fraction:

80.884

Dmp/Cnst:

1.000 1

Phase/element fractions for phase no. 2

Hist Elm:

PXC 1 1 nc

Fraction:

71.939

Dmp/Cnst:

1.000 2

Phase/element fractions for phase no. 3

Hist Elm:

PXC 1 1 nc

Fraction:

37.052

Dmp/Cnst:

1.000 3

Histogram scale factors:

Hist/Typ:

1 PXC

pn

Scale : 0.99840

Dmp/Cnst:

1.000 4

1GSAS S-1
18:57:20 2010 Page 4

GENLES Version Win32 May 01

Absorption coefficients for powder data:

Hist/Typ:

1 PXC

0 pn

Absc 1. :

0.0000

Dmp/Cnst:
Absc 2. :
Dmp/Cnst:

0.000 0

0.0000
0

0.000 0

Diffractometer constants for powder data:


No. Type Lam 1
Lam 2
Kratio pn Cnstr cn Damp
1 PXC 1.7889600 1.7928500
0.5000 0 0.000 0 0

Polariz. pn Cnstr cn type


0.50000 0 0.000 0 0

Extinction coefficients for phase no. 1:

Hist/Typ:

1 PXC

pn

Extinct.:

0.0000

Dmp/Cnst:

0.000 0

Extinction coefficients for phase no. 2:

Hist/Typ:

1 PXC

pn

Zero pn Cnstr cn
0.000 0 0.000 0

Extinct.:
Dmp/Cnst:

0.0000
0

0.000 0

Extinction coefficients for phase no. 3:

Hist/Typ:

1 PXC

pn

Extinct.:

0.0000

Dmp/Cnst:

0.000 0

Radiation damage coefficients for phase no. 1:

Hist/Typ:

1 PXC

Rad.dam.:

0.0000

Dmp/Cnst:

pn
0

0.000 0

Radiation damage coefficients for phase no. 2:


1GSAS S-1
18:57:20 2010 Page 5

Hist/Typ:

1 PXC

Rad.dam.:

0.0000

Dmp/Cnst:

GENLES Version Win32 May 01

pn
0

0.000 0

Radiation damage coefficients for phase no. 3:

Hist/Typ:

1 PXC

Rad.dam.:

0.0000

Dmp/Cnst:

pn
0

0.000 0

Preferred orientation coeffs. for phase no. 1 histogram no. 1:


Axis

pn

Dir./typ:

0.0 2.0 1.0 0

PO ratio:

1.0324 A

Dmp/Cnst:

1.000 5

PO frac.:

1.0000 0

Dmp/Cnst:

0.000 0

Preferred orientation coeffs. for phase no. 2 histogram no. 1:


Axis

pn

Dir./typ:

1.0 1.0 0.0 0

PO ratio:

0.9457 B

Dmp/Cnst:

1.000 6

PO frac.:

1.0000 0

Dmp/Cnst:

0.000 0

Preferred orientation coeffs. for phase no. 3 histogram no. 1:


Axis

pn

Dir./typ:

0.0 0.0 1.0 0

PO ratio:

1.0000 0

Dmp/Cnst:

0.000 0

PO frac.:

1.0000 0

Dmp/Cnst:

0.000 0

Profile coeff. for function type 4, phase no. 1 and histogram no. 1; aniso. axis
0. 0. 1.; damp= 0:
Coeff. :
trns pn

GU pn
shft pn

GV

pn

GW

pn

GP

pn

LX

pn

ptec pn

Value : 2.000E+00 0-2.000E+00 0 1.036E+02 0 0.000E+00 0 1.207E+01


0 0.000E+00 0 0.000E+00 0 1.747E+01 0
Constr. :
0.000 0
Coeff. :
S3 pn

0.000 0
0.000 0
sfec pn
S4 pn

0.000 0
S/L

pn

0.000 0
H/L

pn

0.000 0
eta

pn

0.000 0
S1

pn

0.000 0
S2

pn

Value : 0.000E+00 0 5.000E-04 0 5.000E-04 0 0.000E+00 0 0.000E+00


0 5.049E-01 0 0.000E+00 0-2.411E-01 0
Constr. :
0.000 0
Coeff. :

0.000 0
0.000 0
S5

0.000 0

pn

S6

pn

0.000 0
S7

pn

0.000 0
S8

pn

0.000 0
S9

0.000 0

pn

Value :-3.408E-02 0-1.273E-01 0-8.214E-02 0 1.041E-01 0 2.302E-01 0


Constr. :

0.000 0

0.000 0

0.000 0

1GSAS S-1
18:57:20 2010 Page 6

0.000 0

0.000 0

GENLES Version Win32 May 01

Profile coeff. for function type 2, phase no. 2 and histogram no. 1; aniso. axis
0. 0. 1.; damp= 0:
Coeff. :
asym pn

GU pn
shft pn

GV

pn

GW

pn

LX

pn

LY

pn

trns pn

Value : 2.000E+00 0-2.000E+00 0 1.161E+02 0 8.825E-01 0 0.000E+00


0 0.000E+00 0 0.000E+00 0 1.850E+01 0
Constr. :
0.000 0

0.000 0
0.000 0

Coeff. :
L33 pn

GP
L12

pn
pn

0.000 0
stec pn

0.000 0
ptec pn

0.000 0
sfec pn

0.000 0
L11

pn

0.000 0
L22

pn

Value : 0.000E+00 0 0.000E+00 0 0.000E+00 0 0.000E+00 0 2.014E-02


0 0.000E+00 0 4.535E-02 0-8.464E+00 0
Constr. :
0.000 0
Coeff. :

0.000 0
0.000 0
L13

pn

0.000 0
L23

0.000 0

pn

Value :-4.954E-02 0-6.352E+00 0


Constr. :

0.000 0

0.000 0

0.000 0

0.000 0

0.000 0

Profile coeff. for function type 2, phase no. 3 and histogram no. 1; aniso. axis
0. 0. 1.; damp= 0:
Coeff. :
asym pn

GU pn
shft pn

GV

pn

GW

pn

LX

pn

LY

pn

trns pn

Value : 2.000E+00 0-2.000E+00 0 7.228E+01 0 3.833E+00 0 0.000E+00


0 0.000E+00 0 0.000E+00 0 1.148E+01 0
Constr. :
0.000 0

0.000 0
0.000 0

Coeff. :
L33 pn

GP
L12

pn
pn

0.000 0
stec pn

0.000 0
ptec pn

0.000 0
sfec pn

0.000 0
L11

pn

0.000 0
L22

pn

Value : 0.000E+00 0 0.000E+00 0 0.000E+00 0 0.000E+00 0 0.000E+00


0 3.172E-01 0 0.000E+00 0-1.430E-01 0
Constr. :
0.000 0
Coeff. :

0.000 0
0.000 0
L13

pn

0.000 0
L23

0.000 0

0.000 0

0.000 0

0.000 0

pn

Value :-3.592E+00 0 0.000E+00 0


Constr. :

0.000 0

0.000 0

Diffuse scattering coefficients for powder data:


No diffuse scattering coefficients for histogram

Background coefficients for powder data:


Histogram no.:

1 Damping factor:

0 Use all points: Y

Linear interpolation
Param. :
pn

1 pn

2 pn

3 pn

4 pn

5 pn

Coeff. : 0.66743E+03 C 0.67999E+03 D 0.68187E+03 E 0.70354E+03 F


0.71592E+03 10 0.71593E+03 11
Param. :
pn

7 pn

8 pn

9 pn

10 pn

11 pn

12

Coeff. : 0.71466E+03 12 0.73392E+03 13 0.75705E+03 14 0.69764E+03 15


0.75140E+03 16 0.73024E+03 17

Param. :
pn

13 pn

14 pn

15 pn

16 pn

17 pn

18

Coeff. : 0.72182E+03 18 0.72428E+03 19 0.72155E+03 1A 0.70853E+03 1B


0.70658E+03 1C 0.70277E+03 1D
Param. :
pn

19 pn

20 pn

21 pn

22 pn

23 pn

24

Coeff. : 0.69659E+03 1E 0.71276E+03 1F 0.70310E+03 20 0.71566E+03 21


0.68628E+03 22 0.71041E+03 23
Param. :
pn

25 pn

26 pn

27 pn

28 pn

29 pn

30

Coeff. : 0.69872E+03 24 0.70164E+03 25 0.72888E+03 26 0.73948E+03 27


0.67207E+03 28 0.69605E+03 29
Param. :
pn

31 pn

32 pn

33 pn

34 pn

35 pn

36

Coeff. : 0.67761E+03 2A 0.69697E+03 2B 0.67072E+03 2C 0.67243E+03 2D


0.66768E+03 2E 0.72771E+03 2F

The constraint matrix has 47 terms


1GSAS S-1
18:57:20 2010 Page 7

GENLES Version Win32 May 01

Restraint data statistics:


No restraints used

Powder data statistics

Fitted

Bank Ndata Sum(w*d**2) wRp


DWd Integral
Hstgm 1 PXC 1 3991 5243.5
0 1.497 0.895
Powder totals
0 1.497

3991 5243.5

-Bknd
Rp

wRp

pFree
Rp

wRp

Average
Rp Npfree

0.0403 0.0319 0.0392 0.0342 0.0000 0.0000


0.0403 0.0319 0.0392 0.0342 0.0000 0.0000

No serial correlation in fit at 90% confidence for 1.925 < DWd < 2.075
Cycle 122 There were 3991 observations.
Total before-cycle CHI**2 (offset/sig) = 5.2435E+03 ( 1.4632E+01)
Reduced CHI**2 = 1.329

for 47 variables

Reflection data statistics


Histogram 1 Type PXC Nobs = 90 R(F**2) = 0.1044
After matrix normalization and Marquardt modification:
Full matrix recip. condition value & -log10 = 0.8774E-07

7.06

The value of the determinant is 5.6850*10.0**( -11)

Atom parameters for phase no. 1


frac
x
y
100*U12 100*U13 100*U23
CU

Cu

100*Uiso 100*U11 100*U22 100*U33

( 1) Values : 1.000 0.250000 0.250000 0.000000


Sigmas :

0.116

Shft/esd:

-3.77

moved 0.00A

sum(shift/e.s.d)**2 : 14.22

( 2) Values : 1.035 0.000000 -0.584000 0.250000


Sigmas :

0.301

Shft/esd:

-2.27

moved 0.00A

1.331

sum(shift/e.s.d)**2 :

2.883

5.15

Atomic parameter sum(shift/error)**2 for phase 1 :

19.37

Calculated unit cell formula weight: 320.394, density: 6.572gm/cm**3

Atom parameters for phase no. 2

frac
x
y
100*U12 100*U13 100*U23
ZN

Zn

100*Uiso 100*U11 100*U22 100*U33

( 1) Values : 1.003 0.333300 0.666700 0.000000


Sigmas :

0.115

Shft/esd:

-3.28

moved 0.00A

0.846

sum(shift/e.s.d)**2 : 10.73

( 2) Values : 0.971 0.333300 0.666700 0.383000 -1.294


Sigmas :

0.301

Shft/esd:

-0.69

moved 0.00A

sum(shift/e.s.d)**2 :

0.48

Atomic parameter sum(shift/error)**2 for phase 2 :

11.21

Calculated unit cell formula weight: 162.171, density: 5.680gm/cm**3


1GSAS S-1
18:57:21 2010 Page 8

GENLES Version Win32 May 01

Atom parameters for phase no. 3


frac
x
y
100*U12 100*U13 100*U23
FE

Fe

100*Uiso 100*U11 100*U22 100*U33

( 1) Values : 1.000 0.000000 0.000000 0.000000


Sigmas :

0.202

Shft/esd:

-0.96

moved 0.00A

sum(shift/e.s.d)**2 :

1.790

0.92

Atomic parameter sum(shift/error)**2 for phase 3 :

0.92

Calculated unit cell formula weight: 111.646, density: 7.884gm/cm**3

Phase/element fractions for phase no. 1

Hist Elem:

1 1 PXC

Fraction :

81.6529

Sigmas :

163.437

Shift/esd:

0.00

Wt. Frac.:

0.61933

Sigmas : 0.471902

Phase/element fractions for phase no. 2

Hist Elem:

1 1 PXC

Fraction :

72.9142

Sigmas :

145.369

Shift/esd:

0.01

Wt. Frac.:

0.27993

Sigmas : 0.401868

Phase/element fractions for phase no. 3

Hist Elem:

1 1 PXC

Fraction :

38.1156

Sigmas :

74.8767

Shift/esd:

0.01

Wt. Frac.:

0.10074

Sigmas : 0.177966
Phase/element fraction sum(shift/error)**2 :

0.00

Histogram scale factors:

Histogram:
Scale

1 PXC

: 0.953754

Sigmas :
Shift/esd:

2.01745
-0.02

Histogram scale factor sum(shift/error)**2 :

0.00

Preferred orientation coeffs. for phase no. 1 axis no. 1:

Histogram:
Ratio

1 PXC
1.03

Sigmas :

0.658E-02

Shift/esd:

-0.08

Fraction :

1.00

Sigmas :

0.00

Shift/esd:

0.00

Preferred orientation coeffs. for phase no. 2 axis no. 1:

Histogram:
Ratio

1 PXC
0.937

Sigmas :

0.642E-02

Shift/esd:

-1.43

Fraction :

1.00

Sigmas :

0.00

Shift/esd:

0.00

Preferred orientation sum(shift/error)**2 :

2.05

1GSAS S-1
18:57:21 2010 Page 9

GENLES Version Win32 May 01

Background coefficients for histogram no. 1:


Param. :

Coeff. : 6.674625E+02 6.799335E+02 6.820866E+02 7.035156E+02


7.161416E+02 7.150842E+02
Sigmas : 5.174069E+00 3.836034E+00 3.707694E+00 3.792577E+00
3.794172E+00 3.771644E+00
Shift/esd:

0.01

-0.02

Param. :

0.06
9

-0.01
10

0.06
11

-0.22
12

Coeff. : 7.156646E+02 7.329962E+02 7.550520E+02 7.198093E+02


7.589705E+02 7.312061E+02
Sigmas : 3.846237E+00 3.983977E+00 4.202489E+00 5.178096E+00
4.611496E+00 5.256813E+00
Shift/esd:

0.26

-0.23

Param. :

13

14

-0.48
15

4.28
16

1.64
17

0.18
18

Coeff. : 7.226389E+02 7.243740E+02 7.168566E+02 7.134785E+02


6.977563E+02 7.017411E+02
Sigmas : 3.951143E+00 3.874477E+00 4.362570E+00 3.875674E+00
4.259560E+00 3.791209E+00
Shift/esd:

0.21

Param. :

19

0.03
20

-1.08
21

1.28
22

-2.07
23

-0.27
24

Coeff. : 6.976803E+02 7.137322E+02 6.964179E+02 7.005140E+02


6.877103E+02 7.045745E+02
Sigmas : 3.791230E+00 4.110448E+00 3.862574E+00 3.975613E+00
3.800890E+00 4.054907E+00
Shift/esd:

0.29

Param. :

25

0.24
26

-1.73
27

-3.81
28

0.38
29

-1.44
30

Coeff. : 6.810071E+02 7.032114E+02 7.075329E+02 7.104913E+02


6.774939E+02 6.854180E+02

Sigmas : 4.311108E+00 4.110377E+00 4.396248E+00 4.558782E+00


3.786750E+00 3.875415E+00
Shift/esd:

-4.11

Param. :

31

0.38
32

-4.85

-6.36

33

1.43

34

35

-2.74
36

Coeff. : 6.783560E+02 6.842520E+02 6.676232E+02 6.721601E+02


6.673372E+02 7.096285E+02
Sigmas : 3.719027E+00 4.070794E+00 3.823352E+00 3.714381E+00
3.984989E+00 6.533993E+00
Shift/esd:

0.20

-3.12

-0.81

-0.07

-0.09

0.47 sec; matrix inversion

0.02 sec

Background coef. sum(shift/error)**2 :

CPU times for matrix build

-2.77

157.25

Final variable sum((shift/esd)**2) for cycle 122:


1GSAS S-1
18:57:21 2010 Page 10

190.80 Time:

0.48 sec

GENLES Version Win32 May 01

Restraint data statistics:


No restraints used

Powder data statistics

Fitted

Bank Ndata Sum(w*d**2) wRp


DWd Integral
Hstgm 1 PXC 1 3991 5030.9
0 1.552 0.895
Powder totals
0 1.552

3991 5030.9

-Bknd
Rp

wRp

pFree
Rp

wRp

Average
Rp Npfree

0.0395 0.0313 0.0389 0.0337 0.0000 0.0000


0.0395 0.0313 0.0389 0.0337 0.0000 0.0000

No serial correlation in fit at 90% confidence for 1.925 < DWd < 2.075
Cycle 123 There were 3991 observations.
Total before-cycle CHI**2 (offset/sig) = 5.0309E+03 ( 1.2238E+01)

Reduced CHI**2 = 1.276

for 47 variables

Reflection data statistics


Histogram 1 Type PXC Nobs = 90 R(F**2) = 0.0411
After matrix normalization and Marquardt modification:
Full matrix recip. condition value & -log10 = 0.6603E-07

7.18

The value of the determinant is 4.6796*10.0**( -11)

Atom parameters for phase no. 1


frac
x
y
100*U12 100*U13 100*U23
CU

Cu

100*Uiso 100*U11 100*U22 100*U33

( 1) Values : 1.000 0.250000 0.250000 0.000000


Sigmas :

0.108

Shft/esd:

0.07

moved 0.00A

sum(shift/e.s.d)**2 :

0.00

( 2) Values : 1.035 0.000000 -0.584000 0.250000


Sigmas :

0.289

Shft/esd:

0.01

moved 0.00A

sum(shift/e.s.d)**2 :

1.338

2.884

0.00

Atomic parameter sum(shift/error)**2 for phase 1 :

0.00

Calculated unit cell formula weight: 320.394, density: 6.572gm/cm**3

Atom parameters for phase no. 2


frac
x
y
100*U12 100*U13 100*U23
ZN

100*Uiso 100*U11 100*U22 100*U33

( 1) Values : 1.003 0.333300 0.666700 0.000000

0.849

Zn

Sigmas :

0.109

Shft/esd:

0.03

moved 0.00A

sum(shift/e.s.d)**2 :

0.00

( 2) Values : 0.971 0.333300 0.666700 0.383000 -1.282


Sigmas :

0.293

Shft/esd:

0.04

moved 0.00A

sum(shift/e.s.d)**2 :

0.00

Atomic parameter sum(shift/error)**2 for phase 2 :

0.00

Calculated unit cell formula weight: 162.171, density: 5.680gm/cm**3


1GSAS S-1
18:57:21 2010 Page 11

GENLES Version Win32 May 01

Atom parameters for phase no. 3


frac
x
y
100*U12 100*U13 100*U23
FE

Fe

100*Uiso 100*U11 100*U22 100*U33

( 1) Values : 1.000 0.000000 0.000000 0.000000


Sigmas :

0.192

Shft/esd:

0.03

moved 0.00A

sum(shift/e.s.d)**2 :

1.796

0.00

Atomic parameter sum(shift/error)**2 for phase 3 :

0.00

Calculated unit cell formula weight: 111.646, density: 7.884gm/cm**3

Phase/element fractions for phase no. 1

Hist Elem:

1 1 PXC

Fraction :

81.6622

Sigmas :

185.582

Shift/esd:

0.00

Wt. Frac.:

0.61937

Sigmas : 0.535760

Phase/element fractions for phase no. 2

Hist Elem:

1 1 PXC

Fraction :

72.8958

Sigmas :

165.725

Shift/esd:

0.00

Wt. Frac.:

0.27984

Sigmas : 0.458171

Phase/element fractions for phase no. 3

Hist Elem:

1 1 PXC

Fraction :

38.1356

Sigmas :

86.6365

Shift/esd:

0.00

Wt. Frac.:

0.10079

Sigmas : 0.205895
Phase/element fraction sum(shift/error)**2 :

Histogram scale factors:

Histogram:

1 PXC

0.00

Scale

: 0.955161

Sigmas :

2.16775

Shift/esd:

0.00

Histogram scale factor sum(shift/error)**2 :

0.00

Preferred orientation coeffs. for phase no. 1 axis no. 1:

Histogram:
Ratio

1 PXC
1.03

Sigmas :

0.634E-02

Shift/esd:

0.06

Fraction :

1.00

Sigmas :

0.00

Shift/esd:

0.00

Preferred orientation coeffs. for phase no. 2 axis no. 1:

Histogram:
Ratio

1 PXC
0.936

Sigmas :

0.625E-02

Shift/esd:

-0.01

Fraction :

1.00

Sigmas :

0.00

Shift/esd:

0.00

Preferred orientation sum(shift/error)**2 :


1GSAS S-1
18:57:21 2010 Page 12

0.00
GENLES Version Win32 May 01

Background coefficients for histogram no. 1:


Param. :

Coeff. : 6.674625E+02 6.799335E+02 6.820866E+02 7.035156E+02


7.161416E+02 7.150842E+02
Sigmas : 5.068086E+00 3.757459E+00 3.631747E+00 3.714891E+00
3.716454E+00 3.694381E+00
Shift/esd:

0.00

Param. :

0.00
8

0.00
9

0.00
10

0.00
11

0.00
12

Coeff. : 7.156647E+02 7.329957E+02 7.550474E+02 7.198322E+02


7.589819E+02 7.312326E+02
Sigmas : 3.767367E+00 3.901240E+00 4.109977E+00 5.052845E+00
4.512517E+00 5.144735E+00
Shift/esd:

0.00

Param. :

13

0.00
14

0.00
15

0.00
16

0.00
17

0.01
18

Coeff. : 7.226299E+02 7.243780E+02 7.168495E+02 7.134834E+02


6.977315E+02 7.017188E+02
Sigmas : 3.869969E+00 3.795094E+00 4.273158E+00 3.796839E+00
4.171697E+00 3.713461E+00
Shift/esd:

0.00

Param. :

19

0.00
20

0.00
21

0.00
22

-0.01
23

-0.01
24

Coeff. : 6.976730E+02 7.138169E+02 6.964020E+02 7.004722E+02


6.876990E+02 7.045287E+02
Sigmas : 3.713902E+00 4.023094E+00 3.783441E+00 3.896210E+00
3.723366E+00 3.971125E+00
Shift/esd:

0.00

Param. :

25

0.02
26

0.00
27

-0.01
28

0.00
29

-0.01
30

Coeff. : 6.810652E+02 7.031996E+02 7.074485E+02 7.103793E+02


6.774891E+02 6.853763E+02
Sigmas : 4.227754E+00 4.026518E+00 4.309865E+00 4.477352E+00
3.710151E+00 3.799015E+00
Shift/esd:

0.01

Param. :

31

0.00
32

-0.02
33

-0.03
34

0.00
35

-0.01
36

Coeff. : 6.783375E+02 6.841684E+02 6.676163E+02 6.721584E+02


6.672989E+02 7.096077E+02
Sigmas : 3.642996E+00 3.995636E+00 3.747547E+00 3.638609E+00
3.905365E+00 6.404764E+00
Shift/esd:

-0.01

-0.02

0.00

0.00

-0.01

0.44 sec; matrix inversion

0.02 sec

Background coef. sum(shift/error)**2 :

CPU times for matrix build

0.00

0.00

Final variable sum((shift/esd)**2) for cycle 123:


1GSAS S-1
18:57:21 2010 Page 13

0.01 Time:

0.45 sec

GENLES Version Win32 May 01

Restraint data statistics:


No restraints used

Powder data statistics

Fitted

Bank Ndata Sum(w*d**2) wRp


DWd Integral
Hstgm 1 PXC 1 3991 5030.7
0 1.552 0.895
Powder totals
0 1.552

3991 5030.7

-Bknd
Rp

wRp

pFree
Rp

wRp

Average
Rp Npfree

0.0395 0.0313 0.0389 0.0337 0.0000 0.0000


0.0395 0.0313 0.0389 0.0337 0.0000 0.0000

No serial correlation in fit at 90% confidence for 1.925 < DWd < 2.075
Cycle 124 There were 3991 observations.
Total before-cycle CHI**2 (offset/sig) = 5.0307E+03 ( 1.2235E+01)
Reduced CHI**2 = 1.276

for 47 variables

Reflection data statistics


Histogram 1 Type PXC Nobs = 90 R(F**2) = 0.0412

After matrix normalization and Marquardt modification:


Full matrix recip. condition value & -log10 = 0.1692E-06

6.77

The value of the determinant is 1.1973*10.0**( -10)

Atom parameters for phase no. 1


frac
x
y
100*U12 100*U13 100*U23
CU

Cu

100*Uiso 100*U11 100*U22 100*U33

( 1) Values : 1.000 0.250000 0.250000 0.000000


Sigmas :

0.108

Shft/esd:

0.00

moved 0.00A

sum(shift/e.s.d)**2 :

0.00

( 2) Values : 1.035 0.000000 -0.584000 0.250000


Sigmas :

0.288

Shft/esd:

0.00

moved 0.00A

sum(shift/e.s.d)**2 :

1.338

2.884

0.00

Atomic parameter sum(shift/error)**2 for phase 1 :

0.00

Calculated unit cell formula weight: 320.394, density: 6.572gm/cm**3

Atom parameters for phase no. 2


frac
x
y
100*U12 100*U13 100*U23
ZN

Zn

100*Uiso 100*U11 100*U22 100*U33

( 1) Values : 1.003 0.333300 0.666700 0.000000


Sigmas :

0.109

Shft/esd:

0.00

moved 0.00A

sum(shift/e.s.d)**2 :

0.00

0.849

( 2) Values : 0.971 0.333300 0.666700 0.383000 -1.282


Sigmas :

0.293

Shft/esd:

0.00

moved 0.00A

sum(shift/e.s.d)**2 :

0.00

Atomic parameter sum(shift/error)**2 for phase 2 :

0.00

Calculated unit cell formula weight: 162.171, density: 5.680gm/cm**3


1GSAS S-1
18:57:22 2010 Page 14

GENLES Version Win32 May 01

Atom parameters for phase no. 3


frac
x
y
100*U12 100*U13 100*U23
FE

Fe

100*Uiso 100*U11 100*U22 100*U33

( 1) Values : 1.000 0.000000 0.000000 0.000000


Sigmas :

0.191

Shft/esd:

0.00

moved 0.00A

sum(shift/e.s.d)**2 :

1.796

0.00

Atomic parameter sum(shift/error)**2 for phase 3 :

0.00

Calculated unit cell formula weight: 111.646, density: 7.884gm/cm**3

Phase/element fractions for phase no. 1

Hist Elem:

1 1 PXC

Fraction :

81.6224

Sigmas :

115.822

Shift/esd:

0.00

Wt. Frac.:

0.61936

Sigmas : 0.334533

Phase/element fractions for phase no. 2

Hist Elem:

1 1 PXC

Fraction :

72.8616

Sigmas :

103.393

Shift/esd:

0.00

Wt. Frac.:

0.27985

Sigmas : 0.285982

Phase/element fractions for phase no. 3

Hist Elem:

1 1 PXC

Fraction :

38.1175

Sigmas :

54.0969

Shift/esd:

0.00

Wt. Frac.:

0.10079

Sigmas : 0.128625
Phase/element fraction sum(shift/error)**2 :

0.00

Histogram scale factors:

Histogram:
Scale

1 PXC

: 0.955611

Sigmas :

1.35473

Shift/esd:

0.00

Histogram scale factor sum(shift/error)**2 :

0.00

Preferred orientation coeffs. for phase no. 1 axis no. 1:

Histogram:
Ratio

1 PXC
1.03

Sigmas :

0.633E-02

Shift/esd:

0.00

Fraction :

1.00

Sigmas :

0.00

Shift/esd:

0.00

Preferred orientation coeffs. for phase no. 2 axis no. 1:

Histogram:
Ratio

1 PXC
0.936

Sigmas :

0.625E-02

Shift/esd:

0.00

Fraction :

1.00

Sigmas :

0.00

Shift/esd:

0.00

Preferred orientation sum(shift/error)**2 :


1GSAS S-1
18:57:22 2010 Page 15

0.00
GENLES Version Win32 May 01

Background coefficients for histogram no. 1:


Param. :

Coeff. : 6.674625E+02 6.799335E+02 6.820866E+02 7.035156E+02


7.161416E+02 7.150842E+02

Sigmas : 5.067976E+00 3.757377E+00 3.631668E+00 3.714810E+00


3.716373E+00 3.694300E+00
Shift/esd:

0.00

Param. :

0.00
8

0.00
9

0.00
10

0.00
11

0.00
12

Coeff. : 7.156647E+02 7.329957E+02 7.550469E+02 7.198322E+02


7.589810E+02 7.312346E+02
Sigmas : 3.767286E+00 3.901166E+00 4.109908E+00 5.052747E+00
4.512459E+00 5.144640E+00
Shift/esd:

0.00

Param. :

13

0.00
14

0.00
15

0.00
16

0.00
17

0.00
18

Coeff. : 7.226301E+02 7.243779E+02 7.168498E+02 7.134827E+02


6.977354E+02 7.017198E+02
Sigmas : 3.869886E+00 3.795011E+00 4.273067E+00 3.796765E+00
4.171740E+00 3.713392E+00
Shift/esd:

0.00

Param. :

19

0.00
20

0.00
21

0.00
22

0.00
23

0.00
24

Coeff. : 6.976731E+02 7.138129E+02 6.964027E+02 7.004733E+02


6.876998E+02 7.045286E+02
Sigmas : 3.713825E+00 4.022741E+00 3.783349E+00 3.896138E+00
3.723287E+00 3.971072E+00
Shift/esd:

0.00

Param. :

25

0.00
26

0.00
27

0.00
28

0.00
29

0.00
30

Coeff. : 6.810660E+02 7.031978E+02 7.074472E+02 7.103776E+02


6.774897E+02 6.853761E+02
Sigmas : 4.227565E+00 4.026418E+00 4.309793E+00 4.477190E+00
3.710065E+00 3.798893E+00
Shift/esd:

0.00

Param. :

31

0.00
32

0.00
33

0.00
34

0.00
35

0.00
36

Coeff. : 6.783377E+02 6.841667E+02 6.676168E+02 6.721582E+02


6.672991E+02 7.096070E+02
Sigmas : 3.642914E+00 3.995396E+00 3.747438E+00 3.638526E+00
3.905242E+00 6.404507E+00
Shift/esd:

0.00

0.00

0.00

0.00

0.00

0.00

Background coef. sum(shift/error)**2 :

CPU times for matrix build

0.00

0.47 sec; matrix inversion

Final variable sum((shift/esd)**2) for cycle 124:

0.02 sec

0.00 Time:

0.48 sec

Version

May 01

Convergence was achieved

---------------------------------------------Archiving GSAS.EXP as GSAS.O5D


----------------------------------------------

1GSAS S-1
18:57:42 2010 Page 1

|---------------------------------------------------------|
|

Program POWPREF Version Win32

| Prepares powder histograms for least-squares refinement |


|

Distributed on Mon Nov 12 12:16:14 2007

|---------------------------------------------------------|

|---------------------------------------------------------------|
|

Allen C. Larson and Robert B. Von Dreele

Manuel Lujan, Jr. Neutron Scattering Center, MS-H805

Los Alamos National Laboratory, Los Alamos, NM 87545

| Copyright, 2000, The Regents of the University of California. |


|---------------------------------------------------------------|

The last history record is :


HSTRY146 EXPGUI 1.80 1.46 (1 changes) -- 05/01/10 18:57:41
Data for bank 1 read from file S-1.raw
The powder pattern has 3991 channels with 1 bins per channel
Histogram weight factors are

1.00000

0.00000

No fixed background points for this powder pattern


The 2 excluded regions are (in deg):
Exclude

from:

0.0000

to:

from:

to:

from:

to:

from:

to:

0.0000 99.8200 1000.0000

Incident spectrum type 0 can be used in the region

0.000 deg to 180.000 deg

The minimum possible weighted residual for this histogram is 0.0351


Histogram no. 1 on file GSAS.P01
updated with new excluded regions, background and incident spectrum data.
CPU time = 0.00 to update histogram
Lattice parameters for phase 1 are:
a,b,c = 4.679209 3.422292 5.124918 angles =
volume =

90.000

99.466

90.000

90.000

90.000 120.000

90.000

90.000

80.951

Lattice parameters for phase 2 are:


a,b,c = 3.245163 3.245163 5.198840 angles =
volume =

47.414

Lattice parameters for phase 3 are:


a,b,c = 2.864996 2.864996 2.864996 angles =
volume =

23.516

Profile function 4 for phase no. 1 has the coefficients p1-p21:


0.200000E+01 -0.200000E+01 0.103617E+03 0.000000E+00
0.120660E+02 0.000000E+00 0.000000E+00 0.174719E+02
0.000000E+00 0.500000E-03 0.500000E-03 0.000000E+00
0.000000E+00 0.504909E+00 0.000000E+00 -0.241143E+00

90.000

-0.340766E-01 -0.127270E+00 -0.821388E-01 0.104068E+00

0.230237E+00
cutoff on the wings at 0.001 of maximum

Profile function 2 for phase no. 2 has the coefficients p1-p18:


0.200000E+01 -0.200000E+01 0.116135E+03 0.882512E+00
0.000000E+00 0.000000E+00 0.000000E+00 0.185045E+02
0.000000E+00 0.000000E+00 0.000000E+00 0.000000E+00
0.201354E-01 0.000000E+00 0.453468E-01 -0.846359E+01
-0.495414E-01 -0.635224E+01
cutoff on the wings at 0.001 of maximum

Profile function 2 for phase no. 3 has the coefficients p1-p18:


0.200000E+01 -0.200000E+01 0.722848E+02 0.383343E+01
0.000000E+00 0.000000E+00 0.000000E+00 0.114832E+02
0.000000E+00 0.000000E+00 0.000000E+00 0.000000E+00
0.000000E+00 0.317166E+00 0.000000E+00 -0.142965E+00
-0.359152E+01 0.000000E+00
cutoff on the wings at 0.001 of maximum

Minimum d-spacing used to generate reflections 1.1335 for phase 1


Minimum d-spacing used to generate reflections 1.1241 for phase 2
Minimum d-spacing used to generate reflections 1.1094 for phase 3
Minimum d-spacing used to generate reflections 1.1335 for phase 1
Minimum d-spacing used to generate reflections 1.1241 for phase 2
Minimum d-spacing used to generate reflections 1.1094 for phase 3
Minimum d-spacing for matching reflections 1.1692

Estimated number of reflections to be generated is 165


Number of reflections generated for phase 1 is

60

Number of reflections generated for phase 2 is

24

Number of reflections generated for phase 3 is

Total number of reflections generated for all phases is

90

CPU time = 0.00 sec. to generate reflections.


CPU time = 0.06 sec. to locate reflection limits.
CPU time = 0.02 sec. to match reflection ranges to powder pattern
The maximum number of reflections contributing to any profile point is 21
CPU time = 0.00 sec. to update file
1GSAS S-1
18:57:48 2010 Page 1

Version

May 01

|----------------------------------------------------|
|
|

Program GENLES Version Win32

General crystal structure refinement program

| Magnetic structure refinement added by M. Yethiraj |


| Revised and corrected by Larson and Von Dreele |
|

Distributed on Mon Nov 12 12:15:58 2007

|----------------------------------------------------|

|---------------------------------------------------------------|
|

Allen C. Larson and Robert B. Von Dreele

Manuel Lujan, Jr. Neutron Scattering Center, MS-H805

Los Alamos National Laboratory, Los Alamos, NM 87545

| Copyright, 2000, The Regents of the University of California. |


|---------------------------------------------------------------|

The experiment file is: GSAS.EXP


The last history record is :
HSTRY147 POWPREF Win32 May 01 18:57:42 2010
Maximum number of cycles is

I/SigI cut-off is 1.00


Structure factors will be extracted from histogram 1
using extraction method codes

The atomic and magnetic scattering factors for 4 types of atoms are:
Atom type b-len
c
g

a(1)

b(1)

CU
0.772 13.3380 3.5828
1.6735 64.8126 1.1910

a(2)

b(2)

7.1676

a(3)

0.2470

<j0> Mag. ff :
0.0909 34.9840
0.0000 0.0000 -0.0124

0.4088 11.4430

<j2> Mag. ff :
0.0000 0.0000

1.3329

1.9182 14.4900
0.0035 2.000

O
0.581 3.0485 13.2771
0.8670 32.9089 0.2508

2.2868

4.7300
5.7011

b(3)

a(4)

5.6158 11.3966
0.5128
0.3842
1.5463

3.8250
1.6390
0.3239

ZN
0.568 14.0743 3.2655
2.4100 58.7097 1.3041

7.0318

0.2333

5.1652 10.3163

FE
0.945 11.7695 4.7611
2.3045 76.8805 1.0369

7.3573

0.3072

3.5222 15.3535

<j0> Mag. ff :
0.0706 35.0080
0.0000 0.0000 -0.0114

0.3589 15.3580

<j2> Mag. ff :
0.0000 0.0000

1.9566

6.3230

MoKa

AgKa

Atom type
WKa
AuKa
CU
0.058

1.9405 18.4730
0.0036 2.000

CrKa

FeKa

CuKa

f' -0.734 -1.070 -1.965


0.030

0.320

b(4)

0.5819
0.5166
TiKa

5.5610
2.1610

CoKa

0.324 -0.443 -1.279

TaKa
0.065

f"

1.193
0.092

0.886

0.589

1.265

0.826

1.643

0.770

O
f' 0.093
-0.003 -0.003

0.072

0.049

0.011

0.006

0.121

0.063 -0.002

0.052

0.032

0.006

0.004

0.106

0.044

0.124

0.000

f"

0.073
0.000

ZN
0.065

f' -0.617 -0.913 -1.549


0.034
f"

0.143

1.371
0.106

1.019

0.678

FE
f' -1.294 -2.055 -1.134
0.039 0.017
f"
0.079

0.762
0.058

0.565

3.197

0.284
1.430
0.346
0.844

0.324 -0.352 -1.084


0.938

1.886

0.886

0.289 -0.890 -3.331


0.545

1GSAS S-1
18:57:48 2010 Page 2

1.052

0.490

0.133

0.000
0.072
0.153
0.044
0.084

GENLES Version Win32 May 01

Space group C 1 2/c 1


The lattice is centric C-centered monoclinic

Laue symmetry 2/m

Multiplicity of a general site is 8


The unique axis is b
The symmetry of the point 0,0,0 contains 1bar

The equivalent positions are:

( 1)

Z ( 2)

-X

Y 1/2-Z

The atom positions read in are: (all variable numbers (pn) are in hexadecimal)

Type seq. At. name mult symm frac pn


u22 pn u33 pn u12 pn u13 pn u23 pn
CU
O

1 Cu

4 -1

2O

pn

pn

pn u11 pn

1.0000 0 0.2500 0 0.2500 0 0.0000 0 1.3 1

4 2(010) 1.0346 0 0.0000 0-0.5840 0 0.2500 0 2.9 2

Space group P 63 m c
The lattice is acentric primitive hexagonal

Laue symmetry 6/mmm

Multiplicity of a general site is 12


The location of the origin is arbitrary in z

The equivalent positions are:

( 1)

( 4)

-X

( 7)

Y-X

(10)

X-Y

Z ( 2)

X-Y

-Y 1/2+Z ( 5)
Y

Z ( 8)

X 1/2+Z ( 3)

Y-X
-X

-Y 1/2+Z (11)

-X

-Y

X-Y

Z ( 6)

Y-X 1/2+Z

Y-X 1/2+Z ( 9)

-Y

-X

X-Y

Z (12)

Z
X 1/2+Z

The atom positions read in are: (all variable numbers (pn) are in hexadecimal)

Type seq. At. name mult symm frac pn


u22 pn u33 pn u12 pn u13 pn u23 pn
ZN
O

1 Zn
2O

pn

pn

pn u11 pn

2 3M(100) 1.0027 0 0.3333 0 0.6667 0 0.0000 0 0.8 3


2 3M(100) 0.9706 0 0.3333 0 0.6667 0 0.3830 0-1.3 4

Space group I m -3 m
The lattice is centric I-centered cubic

Laue symmetry m3m

Multiplicity of a general site is 96


The symmetry of the point 0,0,0 contains 1bar

The equivalent positions are:

( 1)

Z ( 2)

Y ( 3)

( 4)

-Z ( 5)

-Z

Y ( 6)

-Z

( 7)

-Z

-Y ( 8)

-Y

-Z

X ( 9)

-Z

-X

(10)

-X

-Z (11)

-Z

-X

Y (12)

-Y

-Z

(13)

Z (14)

X (15)

(16)

-Z (17)

-Z

X (18)

-Z

(19)

-Z

-X (20)

-X

-Z

Y (21)

-Z

-Y

(22)

-Y

-Z (23)

-Z

-Y

X (24)

-X

-Z

1GSAS S-1
18:57:48 2010 Page 3

GENLES Version Win32 May 01

The atom positions read in are: (all variable numbers (pn) are in hexadecimal)

Type seq. At. name mult symm frac pn


u22 pn u33 pn u12 pn u13 pn u23 pn
FE

1 Fe

pn

pn

2 M3M 0.9996 0 0.0000 0 0.0000 0 0.0000 0 1.8 5

Lattice parameters for phase 1 are:


a

alpha

beta

gamma

4.679209 3.422292 5.124918 90.0000 99.4660 90.0000

Lattice parameters for phase 2 are:


a

pn u11 pn

alpha

beta

gamma

3.245163 3.245163 5.198840 90.0000 90.0000 120.0000

Lattice parameters for phase 3 are:


a

alpha

beta

gamma

2.864996 2.864996 2.864996 90.0000 90.0000 90.0000

Phase/element fractions for phase no. 1

Hist Elm:

PXC 1 1 nc

Fraction:

81.622

Dmp/Cnst:

1.000 1

Phase/element fractions for phase no. 2

Hist Elm:

PXC 1 1 nc

Fraction:

72.862

Dmp/Cnst:

1.000 2

Phase/element fractions for phase no. 3

Hist Elm:

PXC 1 1 nc

Fraction:

38.118

Dmp/Cnst:

1.000 3

Histogram scale factors:

Hist/Typ:

1 PXC

pn

Scale : 0.95561

Dmp/Cnst:

1.000 4

1GSAS S-1
18:57:48 2010 Page 4

GENLES Version Win32 May 01

Absorption coefficients for powder data:

Hist/Typ:

1 PXC

0 pn

Absc 1. :

0.0000

Dmp/Cnst:
Absc 2. :
Dmp/Cnst:

0.000 0

0.0000
0

0.000 0

Diffractometer constants for powder data:


No. Type Lam 1
Lam 2
Kratio pn Cnstr cn Damp
1 PXC 1.7889600 1.7928500
0.5000 0 0.000 0 0

Polariz. pn Cnstr cn type


0.50000 0 0.000 0 0

Extinction coefficients for phase no. 1:

Hist/Typ:

1 PXC

pn

Extinct.:

0.0000

Dmp/Cnst:

0.000 0

Extinction coefficients for phase no. 2:

Hist/Typ:

1 PXC

pn

Extinct.:

0.0000

Dmp/Cnst:

0.000 0

Zero pn Cnstr cn
0.000 0 0.000 0

Extinction coefficients for phase no. 3:

Hist/Typ:

1 PXC

pn

Extinct.:

0.0000

Dmp/Cnst:

0.000 0

Radiation damage coefficients for phase no. 1:

Hist/Typ:

1 PXC

pn

Rad.dam.:

0.0000

Dmp/Cnst:

0.000 0

Radiation damage coefficients for phase no. 2:


1GSAS S-1
18:57:48 2010 Page 5

Hist/Typ:

1 PXC

GENLES Version Win32 May 01

pn

Rad.dam.:

0.0000

Dmp/Cnst:

0.000 0

Radiation damage coefficients for phase no. 3:

Hist/Typ:

1 PXC

pn

Rad.dam.:

0.0000

Dmp/Cnst:

0.000 0

Preferred orientation coeffs. for phase no. 1 histogram no. 1:


Axis

pn

Dir./typ:

0.0 2.0 1.0 0

PO ratio:

1.0322 A

Dmp/Cnst:

1.000 5

PO frac.:

1.0000 0

Dmp/Cnst:

0.000 0

Preferred orientation coeffs. for phase no. 2 histogram no. 1:


Axis

pn

Dir./typ:

1.0 1.0 0.0 0

PO ratio:

0.9364 B

Dmp/Cnst:

1.000 6

PO frac.:

1.0000 0

Dmp/Cnst:

0.000 0

Preferred orientation coeffs. for phase no. 3 histogram no. 1:


Axis

pn

Dir./typ:

0.0 0.0 1.0 0

PO ratio:

1.0000 0

Dmp/Cnst:

0.000 0

PO frac.:

1.0000 0

Dmp/Cnst:

0.000 0

Profile coeff. for function type 4, phase no. 1 and histogram no. 1; aniso. axis
0. 0. 1.; damp= 0:
Coeff. :
trns pn

GU pn
shft pn

GV

pn

GW

pn

GP

pn

LX

pn

ptec pn

Value : 2.000E+00 0-2.000E+00 0 1.036E+02 0 0.000E+00 0 1.207E+01


0 0.000E+00 0 0.000E+00 0 1.747E+01 0
Constr. :
0.000 0

0.000 0
0.000 0

0.000 0

0.000 0

0.000 0

0.000 0

0.000 0

Coeff. :
S3 pn

sfec pn
S4 pn

S/L

pn

H/L

pn

eta

pn

S1

pn

S2

pn

Value : 0.000E+00 0 5.000E-04 0 5.000E-04 0 0.000E+00 0 0.000E+00


0 5.049E-01 0 0.000E+00 0-2.411E-01 0
Constr. :
0.000 0
Coeff. :

0.000 0
0.000 0
S5

0.000 0

pn

S6

pn

0.000 0
S7

pn

0.000 0
S8

pn

0.000 0
S9

0.000 0

pn

Value :-3.408E-02 0-1.273E-01 0-8.214E-02 0 1.041E-01 0 2.302E-01 0


Constr. :

0.000 0

0.000 0

0.000 0

1GSAS S-1
18:57:48 2010 Page 6

0.000 0

0.000 0

GENLES Version Win32 May 01

Profile coeff. for function type 2, phase no. 2 and histogram no. 1; aniso. axis
0. 0. 1.; damp= 0:
Coeff. :
asym pn

GU pn
shft pn

GV

pn

GW

pn

LX

pn

LY

pn

trns pn

Value : 2.000E+00 0-2.000E+00 0 1.161E+02 0 8.825E-01 0 0.000E+00


0 0.000E+00 0 0.000E+00 0 1.850E+01 0
Constr. :
0.000 0

0.000 0
0.000 0

Coeff. :
L33 pn

GP
L12

pn
pn

0.000 0
stec pn

0.000 0
ptec pn

0.000 0
sfec pn

0.000 0
L11

pn

0.000 0
L22

pn

Value : 0.000E+00 0 0.000E+00 0 0.000E+00 0 0.000E+00 0 2.014E-02


0 0.000E+00 0 4.535E-02 0-8.464E+00 0
Constr. :
0.000 0
Coeff. :

0.000 0
0.000 0
L13

pn

0.000 0
L23

0.000 0

0.000 0

0.000 0

0.000 0

pn

Value :-4.954E-02 0-6.352E+00 0


Constr. :

0.000 0

0.000 0

Profile coeff. for function type 2, phase no. 3 and histogram no. 1; aniso. axis
0. 0. 1.; damp= 0:

Coeff. :
asym pn

GU pn
shft pn

GV

pn

GW

pn

LX

pn

LY

pn

trns pn

Value : 2.000E+00 0-2.000E+00 0 7.228E+01 0 3.833E+00 0 0.000E+00


0 0.000E+00 0 0.000E+00 0 1.148E+01 0
Constr. :
0.000 0

0.000 0
0.000 0

Coeff. :
L33 pn

GP
L12

pn
pn

0.000 0
stec pn

0.000 0
ptec pn

0.000 0
sfec pn

0.000 0
L11

pn

0.000 0
L22

pn

Value : 0.000E+00 0 0.000E+00 0 0.000E+00 0 0.000E+00 0 0.000E+00


0 3.172E-01 0 0.000E+00 0-1.430E-01 0
Constr. :
0.000 0
Coeff. :

0.000 0
0.000 0
L13

pn

0.000 0
L23

0.000 0

0.000 0

0.000 0

0.000 0

pn

Value :-3.592E+00 0 0.000E+00 0


Constr. :

0.000 0

0.000 0

Diffuse scattering coefficients for powder data:


No diffuse scattering coefficients for histogram

Background coefficients for powder data:


Histogram no.:

1 Damping factor:

0 Use all points: Y

Linear interpolation
Param. :
pn

1 pn

2 pn

3 pn

4 pn

5 pn

Coeff. : 0.66746E+03 0 0.67993E+03 0 0.68209E+03 0 0.70352E+03 0


0.71614E+03 0 0.71508E+03 0
Param. :
pn

7 pn

8 pn

9 pn

10 pn

11 pn

12

Coeff. : 0.71566E+03 0 0.73300E+03 0 0.75505E+03 0 0.71983E+03 0


0.75898E+03 0 0.73123E+03 0
Param. :
pn

13 pn

14 pn

15 pn

16 pn

17 pn

18

Coeff. : 0.72263E+03 0 0.72438E+03 0 0.71685E+03 0 0.71348E+03 0


0.69773E+03 0 0.70172E+03 0
Param. :
pn

19 pn

20 pn

21 pn

22 pn

23 pn

24

Coeff. : 0.69767E+03 0 0.71381E+03 0 0.69640E+03 0 0.70047E+03 0


0.68770E+03 0 0.70453E+03 0
Param. :
pn

25 pn

26 pn

27 pn

28 pn

29 pn

30

Coeff. : 0.68107E+03 0 0.70320E+03 0 0.70745E+03 0 0.71038E+03 0


0.67749E+03 0 0.68538E+03 0
Param. :
pn

31 pn

32 pn

33 pn

34 pn

35 pn

36

Coeff. : 0.67834E+03 0 0.68417E+03 0 0.66762E+03 0 0.67216E+03 0


0.66730E+03 0 0.70961E+03 0

The constraint matrix has 11 terms


1GSAS S-1
18:57:48 2010 Page 7

GENLES Version Win32 May 01

Restraint data statistics:


No restraints used

Powder data statistics

Fitted

Bank Ndata Sum(w*d**2) wRp


DWd Integral
Hstgm 1 PXC 1 3991 5030.7
0 1.552 0.895
Powder totals
0 1.552

3991 5030.7

-Bknd
Rp

wRp

pFree
Rp

wRp

Average
Rp Npfree

0.0395 0.0313 0.0389 0.0337 0.0000 0.0000


0.0395 0.0313 0.0389 0.0337 0.0000 0.0000

No serial correlation in fit at 90% confidence for 1.907 < DWd < 2.093
Cycle 125 There were 3991 observations.

Total before-cycle CHI**2 (offset/sig) = 5.0307E+03 ( 1.1776E+01)


Reduced CHI**2 = 1.264

for 11 variables

Reflection data statistics


Histogram 1 Type PXC Nobs = 90 R(F**2) = 0.0412
After matrix normalization and Marquardt modification:
Full matrix recip. condition value & -log10 = 0.2978E-06

The value of the determinant is 1.5782*10.0**(

6.53

-8)

Atom parameters for phase no. 1


frac
x
y
100*U12 100*U13 100*U23
CU

Cu

100*Uiso 100*U11 100*U22 100*U33

( 1) Values : 1.000 0.250000 0.250000 0.000000


Sigmas :

0.089

Shft/esd:

0.00

moved 0.00A

sum(shift/e.s.d)**2 :

0.00

( 2) Values : 1.035 0.000000 -0.584000 0.250000


Sigmas :

0.261

Shft/esd:

0.00

moved 0.00A

sum(shift/e.s.d)**2 :

1.338

2.884

0.00

Atomic parameter sum(shift/error)**2 for phase 1 :

0.00

Calculated unit cell formula weight: 320.394, density: 6.572gm/cm**3

Atom parameters for phase no. 2


frac
x
y
100*U12 100*U13 100*U23

100*Uiso 100*U11 100*U22 100*U33

ZN

Zn

( 1) Values : 1.003 0.333300 0.666700 0.000000


Sigmas :

0.098

Shft/esd:

0.00

moved 0.00A

sum(shift/e.s.d)**2 :

0.849

0.00

( 2) Values : 0.971 0.333300 0.666700 0.383000 -1.282


Sigmas :

0.273

Shft/esd:

0.00

moved 0.00A

sum(shift/e.s.d)**2 :

0.00

Atomic parameter sum(shift/error)**2 for phase 2 :

0.00

Calculated unit cell formula weight: 162.171, density: 5.680gm/cm**3


1GSAS S-1
18:57:49 2010 Page 8

GENLES Version Win32 May 01

Atom parameters for phase no. 3


frac
x
y
100*U12 100*U13 100*U23
FE

Fe

100*Uiso 100*U11 100*U22 100*U33

( 1) Values : 1.000 0.000000 0.000000 0.000000


Sigmas :

0.165

Shft/esd:

0.00

moved 0.00A

sum(shift/e.s.d)**2 :

1.796

0.00

Atomic parameter sum(shift/error)**2 for phase 3 :

0.00

Calculated unit cell formula weight: 111.646, density: 7.884gm/cm**3

Phase/element fractions for phase no. 1

Hist Elem:

1 1 PXC

Fraction :

81.6548

Sigmas :

104.933

Shift/esd:

0.00

Wt. Frac.:

0.61936

Sigmas : 0.302961

Phase/element fractions for phase no. 2

Hist Elem:

1 1 PXC

Fraction :

72.8906

Sigmas :

93.6745

Shift/esd:

0.00

Wt. Frac.:

0.27985

Sigmas : 0.258998

Phase/element fractions for phase no. 3

Hist Elem:

1 1 PXC

Fraction :

38.1326

Sigmas :

49.0115

Shift/esd:

0.00

Wt. Frac.:

0.10079

Sigmas : 0.116488
Phase/element fraction sum(shift/error)**2 :

Histogram scale factors:

0.00

Histogram:
Scale

1 PXC

: 0.955232

Sigmas :

1.22854

Shift/esd:

0.00

Histogram scale factor sum(shift/error)**2 :

0.00

Preferred orientation coeffs. for phase no. 1 axis no. 1:

Histogram:
Ratio

1 PXC
1.03

Sigmas :

0.580E-02

Shift/esd:

0.00

Fraction :

1.00

Sigmas :

0.00

Shift/esd:

0.00

Preferred orientation coeffs. for phase no. 2 axis no. 1:

Histogram:
Ratio

1 PXC
0.936

Sigmas :

0.564E-02

Shift/esd:

0.00

Fraction :

1.00

Sigmas :

0.00

Shift/esd:

0.00

Preferred orientation sum(shift/error)**2 :


1GSAS S-1
18:57:49 2010 Page 9

0.00
GENLES Version Win32 May 01

CPU times for matrix build

0.38 sec; matrix inversion

Final variable sum((shift/esd)**2) for cycle 125:

0.00 sec

0.00 Time:

0.38 sec

Version

Oct 01

Convergence was achieved

---------------------------------------------Archiving GSAS.EXP as GSAS.O5F


----------------------------------------------

1GSAS S-1
13:42:28 2011 Page 1

|---------------------------------------------------------|
|

Program POWPREF Version Win32

| Prepares powder histograms for least-squares refinement |


|

Distributed on Mon Nov 12 12:16:14 2007

|---------------------------------------------------------|

|---------------------------------------------------------------|
|

Allen C. Larson and Robert B. Von Dreele

Manuel Lujan, Jr. Neutron Scattering Center, MS-H805

Los Alamos National Laboratory, Los Alamos, NM 87545

| Copyright, 2000, The Regents of the University of California. |


|---------------------------------------------------------------|

The last history record is :

HSTRY149 EXPGUI 1.80 1.46 (7 changes) -- 10/01/11 13:42:26


Data for bank 1 read from file S-1.raw
The powder pattern has 3991 channels with 1 bins per channel
Histogram weight factors are

1.00000

0.00000

No fixed background points for this powder pattern


The 2 excluded regions are (in deg):
Exclude

from:

0.0000

to:

from:

to:

from:

to:

from:

to:

0.0000 99.8200 1000.0000

Incident spectrum type 0 can be used in the region

0.000 deg to 180.000 deg

The minimum possible weighted residual for this histogram is 0.0351


Histogram no. 1 on file GSAS.P01
updated with new excluded regions, background and incident spectrum data.
CPU time = 0.02 to update histogram
Lattice parameters for phase 1 are:
a,b,c = 4.679209 3.422292 5.124918 angles =
volume =

90.000

99.466

90.000

90.000

90.000 120.000

90.000

90.000

80.951

Lattice parameters for phase 2 are:


a,b,c = 3.245163 3.245163 5.198840 angles =
volume =

47.414

Lattice parameters for phase 3 are:


a,b,c = 2.864996 2.864996 2.864996 angles =
volume =

23.516

Profile function 4 for phase no. 1 has the coefficients p1-p21:


0.200000E+01 -0.200000E+01 0.103617E+03 0.000000E+00
0.120660E+02 0.000000E+00 0.000000E+00 0.174719E+02
0.000000E+00 0.500000E-03 0.500000E-03 0.000000E+00
0.000000E+00 0.504909E+00 0.000000E+00 -0.241143E+00
-0.340766E-01 -0.127270E+00 -0.821388E-01 0.104068E+00

90.000

0.230237E+00
cutoff on the wings at 0.001 of maximum

Profile function 2 for phase no. 2 has the coefficients p1-p18:


0.200000E+01 -0.200000E+01 0.116135E+03 0.882512E+00
0.000000E+00 0.000000E+00 0.000000E+00 0.185045E+02
0.000000E+00 0.000000E+00 0.000000E+00 0.000000E+00
0.201354E-01 0.000000E+00 0.453468E-01 -0.846359E+01
-0.495414E-01 -0.635224E+01
cutoff on the wings at 0.001 of maximum

Profile function 2 for phase no. 3 has the coefficients p1-p18:


0.200000E+01 -0.200000E+01 0.722848E+02 0.383343E+01
0.000000E+00 0.000000E+00 0.000000E+00 0.114832E+02
0.000000E+00 0.000000E+00 0.000000E+00 0.000000E+00
0.000000E+00 0.317166E+00 0.000000E+00 -0.142965E+00
-0.359152E+01 0.000000E+00
cutoff on the wings at 0.001 of maximum

Minimum d-spacing used to generate reflections 1.1335 for phase 1


Minimum d-spacing used to generate reflections 1.1241 for phase 2
Minimum d-spacing used to generate reflections 1.1094 for phase 3
Minimum d-spacing used to generate reflections 1.1335 for phase 1
Minimum d-spacing used to generate reflections 1.1241 for phase 2
Minimum d-spacing used to generate reflections 1.1094 for phase 3
Minimum d-spacing for matching reflections 1.1692
Estimated number of reflections to be generated is 165

Number of reflections generated for phase 1 is

60

Number of reflections generated for phase 2 is

24

Number of reflections generated for phase 3 is

Total number of reflections generated for all phases is

90

CPU time = 0.00 sec. to generate reflections.


CPU time = 0.05 sec. to locate reflection limits.
CPU time = 0.02 sec. to match reflection ranges to powder pattern
The maximum number of reflections contributing to any profile point is 21
CPU time = 0.00 sec. to update file
1GSAS S-1
13:42:46 2011 Page 1

Version

Oct 01

|----------------------------------------------------|
|
|

Program GENLES Version Win32

General crystal structure refinement program

| Magnetic structure refinement added by M. Yethiraj |


| Revised and corrected by Larson and Von Dreele |
|

Distributed on Mon Nov 12 12:15:58 2007

|----------------------------------------------------|

|---------------------------------------------------------------|
|

Allen C. Larson and Robert B. Von Dreele

Manuel Lujan, Jr. Neutron Scattering Center, MS-H805

Los Alamos National Laboratory, Los Alamos, NM 87545

| Copyright, 2000, The Regents of the University of California. |


|---------------------------------------------------------------|

The experiment file is: GSAS.EXP


The last history record is :
HSTRY150 POWPREF Win32 Oct 01 13:42:28 2011
Maximum number of cycles is

I/SigI cut-off is 1.00


Structure factors will be extracted from histogram 1
using extraction method codes

The atomic and magnetic scattering factors for 4 types of atoms are:
Atom type b-len
c
g

a(1)

b(1)

a(2)

CU
0.772 13.3380 3.5828
1.6735 64.8126 1.1910

b(2)

7.1676

a(3)

0.2470

<j0> Mag. ff :
0.0909 34.9840
0.0000 0.0000 -0.0124

0.4088 11.4430

<j2> Mag. ff :
0.0000 0.0000

1.3329

1.9182 14.4900
0.0035 2.000

O
0.581 3.0485 13.2771
0.8670 32.9089 0.2508

2.2868

b(3)

0.5128

3.8250

0.3842
1.5463

1.6390
0.3239

ZN
0.568 14.0743 3.2655
2.4100 58.7097 1.3041

7.0318

0.2333

5.1652 10.3163

FE
0.945 11.7695 4.7611
2.3045 76.8805 1.0369

7.3573

0.3072

3.5222 15.3535

<j0> Mag. ff :
0.0706 35.0080
0.0000 0.0000 -0.0114

0.3589 15.3580

<j2> Mag. ff :
0.0000 0.0000

1.9566

6.3230

MoKa

AgKa

Atom type
WKa
AuKa
CU
0.058

CrKa

FeKa

CuKa

f' -0.734 -1.070 -1.965


0.030
f"

0.124

1.9405 18.4730
0.0036 2.000

1.193
0.092

0.886

0.589

0.320
1.265

0.5819
0.5166
TiKa

5.5610
2.1610

CoKa

0.324 -0.443 -1.279


0.826

b(4)

5.6158 11.3966

4.7300
5.7011

a(4)

1.643

0.770

TaKa
0.065

0.133

O
f' 0.093
-0.003 -0.003
f"

0.072

0.049

0.011

0.006

0.121

0.063 -0.002

0.052

0.032

0.006

0.004

0.106

0.044

0.000

0.073
0.000

ZN
0.065

f' -0.617 -0.913 -1.549


0.034
f"

0.143

1.371
0.106

1.019

0.678

FE
f' -1.294 -2.055 -1.134
0.039 0.017
f"
0.079

0.762
0.058

0.565

3.197

0.284
1.430
0.346
0.844

0.324 -0.352 -1.084


0.938

1.886

0.886

0.289 -0.890 -3.331


0.545

1GSAS S-1
13:42:46 2011 Page 2

1.052

0.490

0.000
0.072
0.153
0.044
0.084

GENLES Version Win32 Oct 01

Space group C 1 2/c 1


The lattice is centric C-centered monoclinic

Laue symmetry 2/m

Multiplicity of a general site is 8


The unique axis is b
The symmetry of the point 0,0,0 contains 1bar

The equivalent positions are:

( 1)

Z ( 2)

-X

Y 1/2-Z

The atom positions read in are: (all variable numbers (pn) are in hexadecimal)

Type seq. At. name mult symm frac pn


u22 pn u33 pn u12 pn u13 pn u23 pn

pn

pn

pn u11 pn

CU
O

1 Cu

4 -1

2O

1.0000 0 0.2500 0 0.2500 0 0.0000 0 1.3 0

4 2(010) 1.0346 0 0.0000 0-0.5840 0 0.2500 0 2.9 0

Space group P 63 m c
The lattice is acentric primitive hexagonal

Laue symmetry 6/mmm

Multiplicity of a general site is 12


The location of the origin is arbitrary in z

The equivalent positions are:

( 1)

( 4)

-X

( 7)

Y-X

(10)

X-Y

Z ( 2)

X-Y

-Y 1/2+Z ( 5)
Y

Z ( 8)

X 1/2+Z ( 3)

Y-X
-X

-Y 1/2+Z (11)

-X

-Y

X-Y

Z ( 6)

Y-X 1/2+Z

Y-X 1/2+Z ( 9)

-Y

-X

X-Y

Z (12)

Z
X 1/2+Z

The atom positions read in are: (all variable numbers (pn) are in hexadecimal)

Type seq. At. name mult symm frac pn


u22 pn u33 pn u12 pn u13 pn u23 pn
ZN
O

1 Zn
2O

pn

pn

pn u11 pn

2 3M(100) 1.0027 0 0.3333 0 0.6667 0 0.0000 0 0.8 1


2 3M(100) 0.9706 0 0.3333 0 0.6667 0 0.3830 0-1.3 2

Space group I m -3 m
The lattice is centric I-centered cubic

Laue symmetry m3m

Multiplicity of a general site is 96


The symmetry of the point 0,0,0 contains 1bar

The equivalent positions are:

( 1)

Z ( 2)

Y ( 3)

( 4)

-Z ( 5)

-Z

Y ( 6)

-Z

( 7)

-Z

-Y ( 8)

-Y

-Z

X ( 9)

-Z

-X

(10)

-X

-Z (11)

-Z

-X

Y (12)

-Y

-Z

(13)

Z (14)

X (15)

(16)

-Z (17)

-Z

X (18)

-Z

(19)

-Z

-X (20)

-X

-Z

Y (21)

-Z

-Y

(22)

-Y

-Z (23)

-Z

-Y

X (24)

-X

-Z

1GSAS S-1
13:42:46 2011 Page 3

GENLES Version Win32 Oct 01

The atom positions read in are: (all variable numbers (pn) are in hexadecimal)

Type seq. At. name mult symm frac pn


u22 pn u33 pn u12 pn u13 pn u23 pn
FE

1 Fe

pn

pn

pn u11 pn

2 M3M 0.9996 0 0.0000 0 0.0000 0 0.0000 0 1.8 3

Lattice parameters for phase 1 are:


a

alpha

beta

gamma

4.679209 3.422292 5.124918 90.0000 99.4660 90.0000


These cell parameters will be refined
Reciprocal metric tensor elements:
Element :
g11 pn
pn
2*g23 pn

g22 pn

damp= 0
g33 pn

2*g12 pn

2*g13

Value : 4.69422E-02 4 8.53819E-02 5 3.91322E-02 6 -1.81883E-09 0


1.40976E-02 7 -1.66065E-09 0

Constr. :
1.000 1
4
0.000 0

1.000 2

1.000 3

0.000 0

1.000

Lattice parameters for phase 2 are:


a

alpha

beta

gamma

3.245163 3.245163 5.198840 90.0000 90.0000 120.0000


These cell parameters will be refined
Reciprocal metric tensor elements:
Element :
g11 pn
pn
2*g23 pn

g22 pn

damp= 0
g33 pn

2*g12 pn

2*g13

Value : 1.26609E-01 8 1.26609E-01 9 3.69988E-02 A 1.26609E-01 B


-2.88493E-09 0 -2.88493E-09 0
Constr. :
1.000 5
0
0.000 0

1.000 5

1.000 6

1.000 5

0.000

Lattice parameters for phase 3 are:


a

alpha

beta

gamma

2.864996 2.864996 2.864996 90.0000 90.0000 90.0000


These cell parameters will be refined
Reciprocal metric tensor elements:
Element :
g11 pn
pn
2*g23 pn

g22 pn

damp= 0
g33 pn

2*g12 pn

2*g13

Value : 1.21829E-01 C 1.21829E-01 D 1.21829E-01 E -2.96483E-09 0


-2.96483E-09 0 -2.96483E-09 0
Constr. :
1.000 7
0
0.000 0

1.000 7

Phase/element fractions for phase no. 1

Hist Elm:

PXC 1 1 nc

Fraction:

81.655

1.000 7

0.000 0

0.000

Dmp/Cnst:

1.000 8

Phase/element fractions for phase no. 2

Hist Elm:

PXC 1 1 nc

Fraction:

72.891

Dmp/Cnst:

10

1.000 9

Phase/element fractions for phase no. 3

Hist Elm:

PXC 1 1 nc

Fraction:

38.133

Dmp/Cnst:

11

1.000 10

1GSAS S-1
13:42:46 2011 Page 4

Histogram scale factors:

Hist/Typ:

1 PXC

pn

Scale : 0.95523

Dmp/Cnst:

0.000 0

Absorption coefficients for powder data:

Hist/Typ:

1 PXC

0 pn

Absc 1. :

0.0000

Dmp/Cnst:
Absc 2. :
Dmp/Cnst:

0.000 0

0.0000
0

0.000 0

GENLES Version Win32 Oct 01

Diffractometer constants for powder data:


No. Type Lam 1
Lam 2
Kratio pn Cnstr cn Damp
1 PXC 1.7889600 1.7928500
0.5000 0 0.000 0 0

Polariz. pn Cnstr cn type


0.50000 0 0.000 0 0

Zero pn Cnstr cn
0.000 0 0.000 0

Extinction coefficients for phase no. 1:

Hist/Typ:

1 PXC

pn

Extinct.:

0.0000

Dmp/Cnst:

0.000 0

Extinction coefficients for phase no. 2:

Hist/Typ:

1 PXC

pn

Extinct.:

0.0000

Dmp/Cnst:

0.000 0

Extinction coefficients for phase no. 3:

Hist/Typ:

1 PXC

pn

Extinct.:

0.0000

Dmp/Cnst:

0.000 0

Radiation damage coefficients for phase no. 1:


1GSAS S-1
13:42:46 2011 Page 5

GENLES Version Win32 Oct 01

Hist/Typ:

1 PXC

pn

Rad.dam.:

0.0000

Dmp/Cnst:

0.000 0

Radiation damage coefficients for phase no. 2:

Hist/Typ:

1 PXC

pn

Rad.dam.:

0.0000

Dmp/Cnst:

0.000 0

Radiation damage coefficients for phase no. 3:

Hist/Typ:

1 PXC

pn

Rad.dam.:

0.0000

Dmp/Cnst:

0.000 0

Preferred orientation coeffs. for phase no. 1 histogram no. 1:


Axis

pn

Dir./typ:

0.0 2.0 1.0 0

PO ratio:

1.0322 12

Dmp/Cnst:

1.000 11

PO frac.:

1.0000 0

Dmp/Cnst:

0.000 0

Preferred orientation coeffs. for phase no. 2 histogram no. 1:


Axis

Dir./typ:

pn

1.0 1.0 0.0 0

PO ratio:

0.9364 13

Dmp/Cnst:

1.000 12

PO frac.:

1.0000 0

Dmp/Cnst:

0.000 0

Preferred orientation coeffs. for phase no. 3 histogram no. 1:


Axis

pn

Dir./typ:

0.0 0.0 1.0 0

PO ratio:

1.0000 0

Dmp/Cnst:

0.000 0

PO frac.:

1.0000 0

Dmp/Cnst:

0.000 0

1GSAS S-1
13:42:46 2011 Page 6

GENLES Version Win32 Oct 01

Profile coeff. for function type 4, phase no. 1 and histogram no. 1; aniso. axis
0. 0. 1.; damp= 0:
Coeff. :
trns pn

GU pn
shft pn

GV

pn

GW

pn

GP

pn

LX

pn

ptec pn

Value : 2.000E+00 0-2.000E+00 0 1.036E+02 0 0.000E+00 0 1.207E+01


0 0.000E+00 0 0.000E+00 0 1.747E+01 0
Constr. :
0.000 0
Coeff. :
S3 pn

0.000 0
0.000 0
sfec pn
S4 pn

0.000 0
S/L

pn

0.000 0
H/L

pn

0.000 0
eta

pn

0.000 0
S1

pn

0.000 0
S2

pn

Value : 0.000E+00 0 5.000E-04 0 5.000E-04 0 0.000E+00 0 0.000E+00


0 5.049E-01 0 0.000E+00 0-2.411E-01 0
Constr. :
0.000 0
Coeff. :

0.000 0
0.000 0
S5

pn

0.000 0
S6

pn

0.000 0
S7

pn

0.000 0
S8

pn

0.000 0
S9

pn

0.000 0

Value :-3.408E-02 0-1.273E-01 0-8.214E-02 0 1.041E-01 0 2.302E-01 0


Constr. :

0.000 0

0.000 0

0.000 0

0.000 0

0.000 0

Profile coeff. for function type 2, phase no. 2 and histogram no. 1; aniso. axis
0. 0. 1.; damp= 0:
Coeff. :
asym pn

GU pn
shft pn

GV

pn

GW

pn

LX

pn

LY

pn

trns pn

Value : 2.000E+00 0-2.000E+00 0 1.161E+02 0 8.825E-01 0 0.000E+00


0 0.000E+00 0 0.000E+00 0 1.850E+01 0
Constr. :
0.000 0

0.000 0
0.000 0

Coeff. :
L33 pn

GP
L12

pn
pn

0.000 0
stec pn

0.000 0
ptec pn

0.000 0
sfec pn

0.000 0
L11

pn

0.000 0
L22

pn

Value : 0.000E+00 0 0.000E+00 0 0.000E+00 0 0.000E+00 0 2.014E-02


0 0.000E+00 0 4.535E-02 0-8.464E+00 0
Constr. :
0.000 0
Coeff. :

0.000 0
0.000 0
L13

pn

0.000 0
L23

0.000 0

0.000 0

0.000 0

0.000 0

pn

Value :-4.954E-02 0-6.352E+00 0


Constr. :

0.000 0

0.000 0

Profile coeff. for function type 2, phase no. 3 and histogram no. 1; aniso. axis
0. 0. 1.; damp= 0:
Coeff. :
asym pn

GU pn
shft pn

GV

pn

GW

pn

LX

pn

LY

pn

trns pn

Value : 2.000E+00 0-2.000E+00 0 7.228E+01 0 3.833E+00 0 0.000E+00


0 0.000E+00 0 0.000E+00 0 1.148E+01 0
Constr. :
0.000 0

0.000 0
0.000 0

Coeff. :
L33 pn

GP
L12

pn
pn

0.000 0
stec pn

0.000 0
ptec pn

0.000 0
sfec pn

0.000 0
L11

pn

0.000 0
L22

pn

Value : 0.000E+00 0 0.000E+00 0 0.000E+00 0 0.000E+00 0 0.000E+00


0 3.172E-01 0 0.000E+00 0-1.430E-01 0

Constr. :
0.000 0
Coeff. :

0.000 0
0.000 0
L13

pn

0.000 0
L23

0.000 0

0.000 0

0.000 0

0.000 0

pn

Value :-3.592E+00 0 0.000E+00 0


Constr. :

0.000 0

0.000 0

Diffuse scattering coefficients for powder data:


No diffuse scattering coefficients for histogram

Background coefficients for powder data:


Histogram no.:

1 Damping factor:

0 Use all points: Y

Linear interpolation
Param. :
pn

1 pn

2 pn

3 pn

4 pn

5 pn

Coeff. : 0.66746E+03 0 0.67993E+03 0 0.68209E+03 0 0.70352E+03 0


0.71614E+03 0 0.71508E+03 0
Param. :
pn

7 pn

8 pn

9 pn

10 pn

11 pn

12

Coeff. : 0.71566E+03 0 0.73300E+03 0 0.75505E+03 0 0.71983E+03 0


0.75898E+03 0 0.73123E+03 0
Param. :
pn

13 pn

14 pn

15 pn

16 pn

17 pn

18

Coeff. : 0.72263E+03 0 0.72438E+03 0 0.71685E+03 0 0.71348E+03 0


0.69773E+03 0 0.70172E+03 0
Param. :
pn

19 pn

20 pn

21 pn

22 pn

23 pn

24

Coeff. : 0.69767E+03 0 0.71381E+03 0 0.69640E+03 0 0.70047E+03 0


0.68770E+03 0 0.70453E+03 0
Param. :
pn

25 pn

26 pn

27 pn

28 pn

29 pn

Coeff. : 0.68107E+03 0 0.70320E+03 0 0.70745E+03 0 0.71038E+03 0


0.67749E+03 0 0.68538E+03 0

30

Param. :
pn

31 pn

32 pn

33 pn

34 pn

35 pn

36

Coeff. : 0.67834E+03 0 0.68417E+03 0 0.66762E+03 0 0.67216E+03 0


0.66730E+03 0 0.70961E+03 0
1GSAS S-1
13:42:46 2011 Page 7

GENLES Version Win32 Oct 01

The constraint matrix has 19 terms


1GSAS S-1
13:42:46 2011 Page 8

GENLES Version Win32 Oct 01

Restraint data statistics:


No restraints used

Powder data statistics

Fitted

Bank Ndata Sum(w*d**2) wRp


DWd Integral
Hstgm 1 PXC 1 3991 5030.7
0 1.552 0.895
Powder totals
0 1.552

3991 5030.7

-Bknd
Rp

wRp

pFree
Rp

wRp

Average
Rp Npfree

0.0395 0.0313 0.0389 0.0337 0.0000 0.0000


0.0395 0.0313 0.0389 0.0337 0.0000 0.0000

No serial correlation in fit at 90% confidence for 1.909 < DWd < 2.091
Cycle 126 There were 3991 observations.
Total before-cycle CHI**2 (offset/sig) = 5.0307E+03 ( 1.1827E+01)
Reduced CHI**2 = 1.265

for 15 variables

Reflection data statistics


Histogram 1 Type PXC Nobs = 90 R(F**2) = 0.0412

After matrix normalization and Marquardt modification:


Full matrix recip. condition value & -log10 = 0.2759E-01

The value of the determinant is 6.2223*10.0**(

1.56

-3)

Atom parameters for phase no. 1


frac
x
y
100*U12 100*U13 100*U23

100*Uiso 100*U11 100*U22 100*U33

Calculated unit cell formula weight: 320.394, density: 6.572gm/cm**3

Atom parameters for phase no. 2


frac
x
y
100*U12 100*U13 100*U23
ZN

Zn

100*Uiso 100*U11 100*U22 100*U33

( 1) Values : 1.003 0.333300 0.666700 0.000000


Sigmas :

0.095

Shft/esd:

-0.22

moved 0.00A

sum(shift/e.s.d)**2 :

0.828

0.05

( 2) Values : 0.971 0.333300 0.666700 0.383000 -1.288


Sigmas :

0.272

Shft/esd:

-0.02

moved 0.00A

sum(shift/e.s.d)**2 :

0.00

Atomic parameter sum(shift/error)**2 for phase 2 :

0.05

Calculated unit cell formula weight: 162.171, density: 5.680gm/cm**3

Atom parameters for phase no. 3


frac
x
y
100*U12 100*U13 100*U23

100*Uiso 100*U11 100*U22 100*U33

FE

Fe

( 1) Values : 1.000 0.000000 0.000000 0.000000


Sigmas :

0.166

Shft/esd:

-0.06

moved 0.00A

sum(shift/e.s.d)**2 :

1.786

0.00

Atomic parameter sum(shift/error)**2 for phase 3 :

0.00

Calculated unit cell formula weight: 111.646, density: 7.884gm/cm**3


1GSAS S-1
13:42:47 2011 Page 9

Phase/element fractions for phase no. 1

Hist Elem:
Fraction :

1 1 PXC
81.7149

Sigmas : 0.283123
Shift/esd:

0.21

Wt. Frac.:

0.61985

Sigmas : 0.816423E-03

Phase/element fractions for phase no. 2

Hist Elem:
Fraction :

1 1 PXC
72.7820

Sigmas : 0.672377
Shift/esd:

-0.16

Wt. Frac.:

0.27945

Sigmas : 0.186018E-02

GENLES Version Win32 Oct 01

Phase/element fractions for phase no. 3

Hist Elem:
Fraction :

1 1 PXC
38.0969

Sigmas : 0.776923
Shift/esd:

-0.05

Wt. Frac.:

0.10070

Sigmas : 0.184683E-02
Phase/element fraction sum(shift/error)**2 :

0.07

Lattice parameters for powder data:


Phase 1
a
Value

alpha

beta

: 4.679224 3.421884 5.125341

gamma

volume

90.000

99.460

90.000

80.950

0.000

0.003

0.000

0.003

Sigmas : 0.000221 0.000158 0.000249


Recprocal metric tensor shift factor = 100%
Phase 2
a
Value

alpha

beta

: 3.245154 3.245154 5.198875

gamma
90.000

Sigmas : 0.000056 0.000056 0.000171

volume

90.000 120.000

0.000

0.000

0.000

47.414
0.002

Recprocal metric tensor shift factor = 100%


Phase 3
a
Value

alpha

beta

: 2.865015 2.865015 2.865015

gamma

volume

90.000

90.000

90.000

23.517

0.000

0.000

0.000

0.001

Sigmas : 0.000051 0.000051 0.000051


Recprocal metric tensor shift factor = 100%
Recprocal metric tensor sum(shift/error)**2 :

15.55

Preferred orientation coeffs. for phase no. 1 axis no. 1:

Histogram:
Ratio

1 PXC
1.03

Sigmas :

0.582E-02

Shift/esd:

0.12

Fraction :

1.00

Sigmas :

0.00

Shift/esd:

0.00

Preferred orientation coeffs. for phase no. 2 axis no. 1:

Histogram:
Ratio

1 PXC
0.936

Sigmas :

0.564E-02

Shift/esd:

-0.01

Fraction :

1.00

Sigmas :

0.00

Shift/esd:

0.00

Preferred orientation sum(shift/error)**2 :


1GSAS S-1
13:42:47 2011 Page 10

CPU times for matrix build

0.01
GENLES Version Win32 Oct 01

0.47 sec; matrix inversion

Final variable sum((shift/esd)**2) for cycle 126:


1GSAS S-1
13:42:47 2011 Page 11

0.00 sec

15.36 Time:

0.47 sec

GENLES Version Win32 Oct 01

Restraint data statistics:


No restraints used

Powder data statistics

Fitted

Bank Ndata Sum(w*d**2) wRp


DWd Integral
Hstgm 1 PXC 1 3991 5019.7
0 1.555 0.895
Powder totals
0 1.555

3991 5019.7

-Bknd
Rp

pFree

wRp

Rp

Average

wRp

Rp Npfree

0.0394 0.0312 0.0390 0.0337 0.0000 0.0000


0.0394 0.0312 0.0390 0.0337 0.0000 0.0000

No serial correlation in fit at 90% confidence for 1.909 < DWd < 2.091
Cycle 127 There were 3991 observations.
Total before-cycle CHI**2 (offset/sig) = 5.0197E+03 ( 1.1704E+01)
Reduced CHI**2 = 1.263

for 15 variables

Reflection data statistics


Histogram 1 Type PXC Nobs = 90 R(F**2) = 0.0411
After matrix normalization and Marquardt modification:
Full matrix recip. condition value & -log10 = 0.2780E-01

The value of the determinant is 6.4911*10.0**(

1.56

-3)

Atom parameters for phase no. 1


frac
x
y
100*U12 100*U13 100*U23

100*Uiso 100*U11 100*U22 100*U33

Calculated unit cell formula weight: 320.394, density: 6.572gm/cm**3

Atom parameters for phase no. 2

frac
x
y
100*U12 100*U13 100*U23
ZN

Zn

100*Uiso 100*U11 100*U22 100*U33

( 1) Values : 1.003 0.333300 0.666700 0.000000


Sigmas :

0.095

Shft/esd:

-0.01

moved 0.00A

sum(shift/e.s.d)**2 :

0.827

0.00

( 2) Values : 0.971 0.333300 0.666700 0.383000 -1.288


Sigmas :

0.272

Shft/esd:

0.00

moved 0.00A

sum(shift/e.s.d)**2 :

0.00

Atomic parameter sum(shift/error)**2 for phase 2 :

0.00

Calculated unit cell formula weight: 162.171, density: 5.680gm/cm**3

Atom parameters for phase no. 3


frac
x
y
100*U12 100*U13 100*U23
FE

Fe

100*Uiso 100*U11 100*U22 100*U33

( 1) Values : 1.000 0.000000 0.000000 0.000000


Sigmas :

0.165

Shft/esd:

-0.01

moved 0.00A

sum(shift/e.s.d)**2 :

1.785

0.00

Atomic parameter sum(shift/error)**2 for phase 3 :

0.00

Calculated unit cell formula weight: 111.646, density: 7.883gm/cm**3


1GSAS S-1
13:42:47 2011 Page 12

GENLES Version Win32 Oct 01

Phase/element fractions for phase no. 1

Hist Elem:
Fraction :

1 1 PXC
81.7183

Sigmas : 0.282987
Shift/esd:

0.01

Wt. Frac.:

0.61988

Sigmas : 0.815971E-03

Phase/element fractions for phase no. 2

Hist Elem:
Fraction :

1 1 PXC
72.7772

Sigmas : 0.670117
Shift/esd:

-0.01

Wt. Frac.:

0.27943

Sigmas : 0.185398E-02

Phase/element fractions for phase no. 3

Hist Elem:
Fraction :

1 1 PXC
38.0929

Sigmas : 0.773969
Shift/esd:

-0.01

Wt. Frac.:

0.10069

Sigmas : 0.183983E-02
Phase/element fraction sum(shift/error)**2 :

0.00

Lattice parameters for powder data:


Phase 1
a
Value

alpha

beta

: 4.679241 3.421880 5.125319

gamma

volume

90.000

99.460

90.000

80.950

0.000

0.003

0.000

0.003

Sigmas : 0.000220 0.000156 0.000245


Recprocal metric tensor shift factor = 100%
Phase 2
a
Value

alpha

beta

: 3.245154 3.245154 5.198873

gamma
90.000

Sigmas : 0.000056 0.000056 0.000171

volume

90.000 120.000

0.000

0.000

0.000

47.414
0.002

Recprocal metric tensor shift factor = 100%


Phase 3
a
Value

alpha

beta

: 2.865015 2.865015 2.865015

gamma

volume

90.000

90.000

90.000

23.517

0.000

0.000

0.000

0.001

Sigmas : 0.000051 0.000051 0.000051


Recprocal metric tensor shift factor = 100%
Recprocal metric tensor sum(shift/error)**2 :

0.01

Preferred orientation coeffs. for phase no. 1 axis no. 1:

Histogram:
Ratio

1 PXC
1.03

Sigmas :

0.579E-02

Shift/esd:

0.03

Fraction :

1.00

Sigmas :

0.00

Shift/esd:

0.00

Preferred orientation coeffs. for phase no. 2 axis no. 1:

Histogram:
Ratio

1 PXC
0.936

Sigmas :

0.563E-02

Shift/esd:

0.00

Fraction :

1.00

Sigmas :

0.00

Shift/esd:

0.00

Preferred orientation sum(shift/error)**2 :

0.00

1GSAS S-1
13:42:47 2011 Page 13

CPU times for matrix build

GENLES Version Win32 Oct 01

0.44 sec; matrix inversion

Final variable sum((shift/esd)**2) for cycle 127:


1GSAS S-1
13:42:47 2011 Page 14

0.00 sec

0.02 Time:

0.44 sec

GENLES Version Win32 Oct 01

Restraint data statistics:


No restraints used

Powder data statistics

Fitted

Bank Ndata Sum(w*d**2) wRp


DWd Integral
Hstgm 1 PXC 1 3991 5019.7
0 1.555 0.895
Powder totals
0 1.555

3991 5019.7

-Bknd
Rp

wRp

pFree
Rp

wRp

Average
Rp Npfree

0.0394 0.0312 0.0390 0.0337 0.0000 0.0000


0.0394 0.0312 0.0390 0.0337 0.0000 0.0000

No serial correlation in fit at 90% confidence for 1.909 < DWd < 2.091
Cycle 128 There were 3991 observations.
Total before-cycle CHI**2 (offset/sig) = 5.0197E+03 ( 1.1704E+01)
Reduced CHI**2 = 1.262

for 15 variables

Reflection data statistics


Histogram 1 Type PXC Nobs = 90 R(F**2) = 0.0411
After matrix normalization and Marquardt modification:
Full matrix recip. condition value & -log10 = 0.2780E-01

The value of the determinant is 6.4878*10.0**(

1.56

-3)

Atom parameters for phase no. 1


frac
x
y
100*U12 100*U13 100*U23

100*Uiso 100*U11 100*U22 100*U33

Calculated unit cell formula weight: 320.394, density: 6.572gm/cm**3

Atom parameters for phase no. 2


frac
x
y
100*U12 100*U13 100*U23
ZN

Zn

100*Uiso 100*U11 100*U22 100*U33

( 1) Values : 1.003 0.333300 0.666700 0.000000


Sigmas :

0.095

Shft/esd:

0.00

moved 0.00A

sum(shift/e.s.d)**2 :

0.827

0.00

( 2) Values : 0.971 0.333300 0.666700 0.383000 -1.288


Sigmas :

0.272

Shft/esd:

0.00

moved 0.00A

sum(shift/e.s.d)**2 :

0.00

Atomic parameter sum(shift/error)**2 for phase 2 :

0.00

Calculated unit cell formula weight: 162.171, density: 5.680gm/cm**3

Atom parameters for phase no. 3


frac
x
y
100*U12 100*U13 100*U23
FE

Fe

100*Uiso 100*U11 100*U22 100*U33

( 1) Values : 1.000 0.000000 0.000000 0.000000


Sigmas :

0.165

Shft/esd:

0.00

moved 0.00A

sum(shift/e.s.d)**2 :

1.785

0.00

Atomic parameter sum(shift/error)**2 for phase 3 :

0.00

Calculated unit cell formula weight: 111.646, density: 7.883gm/cm**3


1GSAS S-1
13:42:48 2011 Page 15

Phase/element fractions for phase no. 1

Hist Elem:
Fraction :

1 1 PXC
81.7185

Sigmas : 0.282991
Shift/esd:

0.00

Wt. Frac.:

0.61988

Sigmas : 0.815982E-03

Phase/element fractions for phase no. 2

GENLES Version Win32 Oct 01

Hist Elem:
Fraction :

1 1 PXC
72.7772

Sigmas : 0.670051
Shift/esd:

0.00

Wt. Frac.:

0.27943

Sigmas : 0.185379E-02

Phase/element fractions for phase no. 3

Hist Elem:
Fraction :

1 1 PXC
38.0930

Sigmas : 0.773809
Shift/esd:

0.00

Wt. Frac.:

0.10069

Sigmas : 0.183945E-02
Phase/element fraction sum(shift/error)**2 :

0.00

Lattice parameters for powder data:


Phase 1
a
Value

alpha

beta

: 4.679240 3.421879 5.125321

gamma

volume

90.000

99.460

90.000

80.950

0.000

0.003

0.000

0.003

Sigmas : 0.000220 0.000156 0.000246


Recprocal metric tensor shift factor = 100%
Phase 2
a
Value

alpha

beta

: 3.245154 3.245154 5.198872

Sigmas : 0.000056 0.000056 0.000171

gamma
90.000
0.000

volume

90.000 120.000
0.000

0.000

47.414
0.002

Recprocal metric tensor shift factor = 100%


Phase 3
a
Value

alpha

beta

: 2.865015 2.865015 2.865015

gamma

volume

90.000

90.000

90.000

23.517

0.000

0.000

0.000

0.001

Sigmas : 0.000051 0.000051 0.000051


Recprocal metric tensor shift factor = 100%
Recprocal metric tensor sum(shift/error)**2 :

0.00

Preferred orientation coeffs. for phase no. 1 axis no. 1:

Histogram:
Ratio

1 PXC
1.03

Sigmas :

0.579E-02

Shift/esd:

0.00

Fraction :

1.00

Sigmas :

0.00

Shift/esd:

0.00

Preferred orientation coeffs. for phase no. 2 axis no. 1:

Histogram:
Ratio

1 PXC
0.936

Sigmas :

0.563E-02

Shift/esd:

0.00

Fraction :

1.00

Sigmas :

0.00

Shift/esd:

0.00

Preferred orientation sum(shift/error)**2 :

0.00

1GSAS S-1
13:42:48 2011 Page 16

CPU times for matrix build

GENLES Version Win32 Oct 01

0.42 sec; matrix inversion

Final variable sum((shift/esd)**2) for cycle 128:

0.02 sec

0.00 Time:

0.44 sec

Version

Dec 09

Convergence was achieved


1GSAS S-1
22:33:41 2011 Page 1

|----------------------------------------------------|
|
|

Program GENLES Version Win32

General crystal structure refinement program

| Magnetic structure refinement added by M. Yethiraj |


| Revised and corrected by Larson and Von Dreele |
|

Distributed on Wed Sep 07 19:37:12 2005

|----------------------------------------------------|

|---------------------------------------------------------------|
|

Allen C. Larson and Robert B. Von Dreele

Manuel Lujan, Jr. Neutron Scattering Center, MS-H805

Los Alamos National Laboratory, Los Alamos, NM 87545

| Copyright, 2000, The Regents of the University of California. |


|---------------------------------------------------------------|

The experiment file is: GSAS.EXP

The last history record is :


HSTRY151 GENLES Win32 Oct 01 13:42:47 2011 Sdsq= 0.502E+04 S/E=
0.106E-03
Maximum number of cycles is

I/SigI cut-off is 1.00


Structure factors will be extracted from histogram 1
using extraction method codes

The atomic and magnetic scattering factors for 4 types of atoms are:
Atom type b-len
c
g

a(1)

b(1)

a(2)

CU
0.772 13.3380 3.5828
1.6735 64.8126 1.1910

b(2)

7.1676

a(3)

0.2470

<j0> Mag. ff :
0.0909 34.9840
0.0000 0.0000 -0.0124

0.4088 11.4430

<j2> Mag. ff :
0.0000 0.0000

1.3329

1.9182 14.4900
0.0035 2.000

O
0.581 3.0485 13.2771
0.8670 32.9089 0.2508

2.2868

b(3)

0.5128

3.8250

0.3842
1.5463

1.6390
0.3239

ZN
0.568 14.0743 3.2655
2.4100 58.7097 1.3041

7.0318

0.2333

5.1652 10.3163

FE
0.945 11.7695 4.7611
2.3045 76.8805 1.0369

7.3573

0.3072

3.5222 15.3535

<j0> Mag. ff :
0.0706 35.0080
0.0000 0.0000 -0.0114

0.3589 15.3580

<j2> Mag. ff :
0.0000 0.0000

1.9566

6.3230

MoKa

AgKa

Atom type
WKa
AuKa
CU
0.058

CrKa

FeKa

CuKa

f' -0.734 -1.070 -1.965


0.030
f"

0.124

1.9405 18.4730
0.0036 2.000

1.193
0.092

0.886

0.589

0.320
1.265

0.5819
0.5166
TiKa

5.5610
2.1610

CoKa

0.324 -0.443 -1.279


0.826

b(4)

5.6158 11.3966

4.7300
5.7011

a(4)

1.643

0.770

TaKa
0.065

0.133

O
f' 0.093
-0.003 -0.003
f"

0.072

0.049

0.011

0.006

0.121

0.063 -0.002

0.052

0.032

0.006

0.004

0.106

0.044

0.000

0.073
0.000

ZN
0.065

f' -0.617 -0.913 -1.549


0.034
f"

0.143

1.371
0.106

1.019

0.678

FE
f' -1.294 -2.055 -1.134
0.039 0.017
f"
0.079

0.762
0.058

0.565

3.197

0.284
1.430
0.346
0.844

0.324 -0.352 -1.084


0.938

1.886

0.886

0.289 -0.890 -3.331


0.545

1GSAS S-1
22:33:41 2011 Page 2

1.052

0.490

0.000
0.072
0.153
0.044
0.084

GENLES Version Win32 Dec 09

Space group C 1 2/c 1


The lattice is centric C-centered monoclinic

Laue symmetry 2/m

Multiplicity of a general site is 8


The unique axis is b
The symmetry of the point 0,0,0 contains 1bar

The equivalent positions are:

( 1)

Z ( 2)

-X

Y 1/2-Z

The atom positions read in are: (all variable numbers (pn) are in hexadecimal)

Type seq. At. name mult symm frac pn


u22 pn u33 pn u12 pn u13 pn u23 pn

pn

pn

pn u11 pn

CU
O

1 Cu

4 -1

2O

1.0000 0 0.2500 0 0.2500 0 0.0000 0 1.3 0

4 2(010) 1.0346 0 0.0000 0-0.5840 0 0.2500 0 2.9 0

Space group P 63 m c
The lattice is acentric primitive hexagonal

Laue symmetry 6/mmm

Multiplicity of a general site is 12


The location of the origin is arbitrary in z

The equivalent positions are:

( 1)

( 4)

-X

( 7)

Y-X

(10)

X-Y

Z ( 2)

X-Y

-Y 1/2+Z ( 5)
Y

Z ( 8)

X 1/2+Z ( 3)

Y-X
-X

-Y 1/2+Z (11)

-X

-Y

X-Y

Z ( 6)

Y-X 1/2+Z

Y-X 1/2+Z ( 9)

-Y

-X

X-Y

Z (12)

Z
X 1/2+Z

The atom positions read in are: (all variable numbers (pn) are in hexadecimal)

Type seq. At. name mult symm frac pn


u22 pn u33 pn u12 pn u13 pn u23 pn
ZN
O

1 Zn
2O

pn

pn

pn u11 pn

2 3M(100) 1.0027 0 0.3333 0 0.6667 0 0.0000 0 0.8 1


2 3M(100) 0.9706 0 0.3333 0 0.6667 0 0.3830 0-1.3 2

Space group I m -3 m
The lattice is centric I-centered cubic

Laue symmetry m3m

Multiplicity of a general site is 96


The symmetry of the point 0,0,0 contains 1bar

The equivalent positions are:

( 1)

Z ( 2)

Y ( 3)

( 4)

-Z ( 5)

-Z

Y ( 6)

-Z

( 7)

-Z

-Y ( 8)

-Y

-Z

X ( 9)

-Z

-X

(10)

-X

-Z (11)

-Z

-X

Y (12)

-Y

-Z

(13)

Z (14)

X (15)

(16)

-Z (17)

-Z

X (18)

-Z

(19)

-Z

-X (20)

-X

-Z

Y (21)

-Z

-Y

(22)

-Y

-Z (23)

-Z

-Y

X (24)

-X

-Z

1GSAS S-1
22:33:41 2011 Page 3

GENLES Version Win32 Dec 09

The atom positions read in are: (all variable numbers (pn) are in hexadecimal)

Type seq. At. name mult symm frac pn


u22 pn u33 pn u12 pn u13 pn u23 pn
FE

1 Fe

pn

pn

pn u11 pn

2 M3M 0.9996 0 0.0000 0 0.0000 0 0.0000 0 1.8 3

Lattice parameters for phase 1 are:


a

alpha

beta

gamma

4.679240 3.421879 5.125321 90.0000 99.4599 90.0000


These cell parameters will be refined
Reciprocal metric tensor elements:
Element :
g11 pn
pn
2*g23 pn

g22 pn

damp= 0
g33 pn

2*g12 pn

2*g13

Value : 4.69399E-02 4 8.54025E-02 5 3.91247E-02 6 -1.81881E-09 0


1.40869E-02 7 -1.66051E-09 0

Constr. :
1.000 1
4
0.000 0

1.000 2

1.000 3

0.000 0

1.000

Lattice parameters for phase 2 are:


a

alpha

beta

gamma

3.245154 3.245154 5.198872 90.0000 90.0000 120.0000


These cell parameters will be refined
Reciprocal metric tensor elements:
Element :
g11 pn
pn
2*g23 pn

g22 pn

damp= 0
g33 pn

2*g12 pn

2*g13

Value : 1.26610E-01 8 1.26610E-01 9 3.69983E-02 A 1.26610E-01 B


-2.88492E-09 0 -2.88492E-09 0
Constr. :
1.000 5
0
0.000 0

1.000 5

1.000 6

1.000 5

0.000

Lattice parameters for phase 3 are:


a

alpha

beta

gamma

2.865015 2.865015 2.865015 90.0000 90.0000 90.0000


These cell parameters will be refined
Reciprocal metric tensor elements:
Element :
g11 pn
pn
2*g23 pn

g22 pn

damp= 0
g33 pn

2*g12 pn

2*g13

Value : 1.21828E-01 C 1.21828E-01 D 1.21828E-01 E -2.96479E-09 0


-2.96479E-09 0 -2.96479E-09 0
Constr. :
1.000 7
0
0.000 0

1.000 7

Phase/element fractions for phase no. 1

Hist Elm:

PXC 1 1 nc

Fraction:

81.719

1.000 7

0.000 0

0.000

Dmp/Cnst:

1.000 8

Phase/element fractions for phase no. 2

Hist Elm:

PXC 1 1 nc

Fraction:

72.777

Dmp/Cnst:

10

1.000 9

Phase/element fractions for phase no. 3

Hist Elm:

PXC 1 1 nc

Fraction:

38.093

Dmp/Cnst:

11

1.000 10

1GSAS S-1
22:33:41 2011 Page 4

Histogram scale factors:

Hist/Typ:

1 PXC

pn

Scale : 0.95523

Dmp/Cnst:

0.000 0

Absorption coefficients for powder data:

Hist/Typ:

1 PXC

0 pn

Absc 1. :

0.0000

Dmp/Cnst:
Absc 2. :
Dmp/Cnst:

0.000 0

0.0000
0

0.000 0

GENLES Version Win32 Dec 09

Diffractometer constants for powder data:


No. Type Lam 1
Lam 2
Kratio pn Cnstr cn Damp
1 PXC 1.7889600 1.7928500
0.5000 0 0.000 0 0

Polariz. pn Cnstr cn type


0.50000 0 0.000 0 0

Zero pn Cnstr cn
0.000 0 0.000 0

Extinction coefficients for phase no. 1:

Hist/Typ:

1 PXC

pn

Extinct.:

0.0000

Dmp/Cnst:

0.000 0

Extinction coefficients for phase no. 2:

Hist/Typ:

1 PXC

pn

Extinct.:

0.0000

Dmp/Cnst:

0.000 0

Extinction coefficients for phase no. 3:

Hist/Typ:

1 PXC

pn

Extinct.:

0.0000

Dmp/Cnst:

0.000 0

Radiation damage coefficients for phase no. 1:


1GSAS S-1
22:33:41 2011 Page 5

GENLES Version Win32 Dec 09

Hist/Typ:

1 PXC

pn

Rad.dam.:

0.0000

Dmp/Cnst:

0.000 0

Radiation damage coefficients for phase no. 2:

Hist/Typ:

1 PXC

pn

Rad.dam.:

0.0000

Dmp/Cnst:

0.000 0

Radiation damage coefficients for phase no. 3:

Hist/Typ:

1 PXC

pn

Rad.dam.:

0.0000

Dmp/Cnst:

0.000 0

Preferred orientation coeffs. for phase no. 1 histogram no. 1:


Axis

pn

Dir./typ:

0.0 2.0 1.0 0

PO ratio:

1.0330 12

Dmp/Cnst:

1.000 11

PO frac.:

1.0000 0

Dmp/Cnst:

0.000 0

Preferred orientation coeffs. for phase no. 2 histogram no. 1:


Axis

Dir./typ:

pn

1.0 1.0 0.0 0

PO ratio:

0.9364 13

Dmp/Cnst:

1.000 12

PO frac.:

1.0000 0

Dmp/Cnst:

0.000 0

Preferred orientation coeffs. for phase no. 3 histogram no. 1:


Axis

pn

Dir./typ:

0.0 0.0 1.0 0

PO ratio:

1.0000 0

Dmp/Cnst:

0.000 0

PO frac.:

1.0000 0

Dmp/Cnst:

0.000 0

1GSAS S-1
22:33:41 2011 Page 6

GENLES Version Win32 Dec 09

Profile coeff. for function type 4, phase no. 1 and histogram no. 1; aniso. axis
0. 0. 1.; damp= 0:
Coeff. :
trns pn

GU pn
shft pn

GV

pn

GW

pn

GP

pn

LX

pn

ptec pn

Value : 2.000E+00 0-2.000E+00 0 1.036E+02 0 0.000E+00 0 1.207E+01


0 0.000E+00 0 0.000E+00 0 1.747E+01 0
Constr. :
0.000 0
Coeff. :
S3 pn

0.000 0
0.000 0
sfec pn
S4 pn

0.000 0
S/L

pn

0.000 0
H/L

pn

0.000 0
eta

pn

0.000 0
S1

pn

0.000 0
S2

pn

Value : 0.000E+00 0 5.000E-04 0 5.000E-04 0 0.000E+00 0 0.000E+00


0 5.049E-01 0 0.000E+00 0-2.411E-01 0
Constr. :
0.000 0
Coeff. :

0.000 0
0.000 0
S5

pn

0.000 0
S6

pn

0.000 0
S7

pn

0.000 0
S8

pn

0.000 0
S9

pn

0.000 0

Value :-3.408E-02 0-1.273E-01 0-8.214E-02 0 1.041E-01 0 2.302E-01 0


Constr. :

0.000 0

0.000 0

0.000 0

0.000 0

0.000 0

Profile coeff. for function type 2, phase no. 2 and histogram no. 1; aniso. axis
0. 0. 1.; damp= 0:
Coeff. :
asym pn

GU pn
shft pn

GV

pn

GW

pn

LX

pn

LY

pn

trns pn

Value : 2.000E+00 0-2.000E+00 0 1.161E+02 0 8.825E-01 0 0.000E+00


0 0.000E+00 0 0.000E+00 0 1.850E+01 0
Constr. :
0.000 0

0.000 0
0.000 0

Coeff. :
L33 pn

GP
L12

pn
pn

0.000 0
stec pn

0.000 0
ptec pn

0.000 0
sfec pn

0.000 0
L11

pn

0.000 0
L22

pn

Value : 0.000E+00 0 0.000E+00 0 0.000E+00 0 0.000E+00 0 2.014E-02


0 0.000E+00 0 4.535E-02 0-8.464E+00 0
Constr. :
0.000 0
Coeff. :

0.000 0
0.000 0
L13

pn

0.000 0
L23

0.000 0

0.000 0

0.000 0

0.000 0

pn

Value :-4.954E-02 0-6.352E+00 0


Constr. :

0.000 0

0.000 0

Profile coeff. for function type 2, phase no. 3 and histogram no. 1; aniso. axis
0. 0. 1.; damp= 0:
Coeff. :
asym pn

GU pn
shft pn

GV

pn

GW

pn

LX

pn

LY

pn

trns pn

Value : 2.000E+00 0-2.000E+00 0 7.228E+01 0 3.833E+00 0 0.000E+00


0 0.000E+00 0 0.000E+00 0 1.148E+01 0
Constr. :
0.000 0

0.000 0
0.000 0

Coeff. :
L33 pn

GP
L12

pn
pn

0.000 0
stec pn

0.000 0
ptec pn

0.000 0
sfec pn

0.000 0
L11

pn

0.000 0
L22

pn

Value : 0.000E+00 0 0.000E+00 0 0.000E+00 0 0.000E+00 0 0.000E+00


0 3.172E-01 0 0.000E+00 0-1.430E-01 0

Constr. :
0.000 0
Coeff. :

0.000 0
0.000 0
L13

pn

0.000 0
L23

0.000 0

0.000 0

0.000 0

0.000 0

pn

Value :-3.592E+00 0 0.000E+00 0


Constr. :

0.000 0

0.000 0

Diffuse scattering coefficients for powder data:


No diffuse scattering coefficients for histogram

Background coefficients for powder data:


Histogram no.:

1 Damping factor:

0 Use all points: Y

Linear interpolation
Param. :
pn

1 pn

2 pn

3 pn

4 pn

5 pn

Coeff. : 0.66746E+03 0 0.67993E+03 0 0.68209E+03 0 0.70352E+03 0


0.71614E+03 0 0.71508E+03 0
Param. :
pn

7 pn

8 pn

9 pn

10 pn

11 pn

12

Coeff. : 0.71566E+03 0 0.73300E+03 0 0.75505E+03 0 0.71983E+03 0


0.75898E+03 0 0.73123E+03 0
Param. :
pn

13 pn

14 pn

15 pn

16 pn

17 pn

18

Coeff. : 0.72263E+03 0 0.72438E+03 0 0.71685E+03 0 0.71348E+03 0


0.69773E+03 0 0.70172E+03 0
Param. :
pn

19 pn

20 pn

21 pn

22 pn

23 pn

24

Coeff. : 0.69767E+03 0 0.71381E+03 0 0.69640E+03 0 0.70047E+03 0


0.68770E+03 0 0.70453E+03 0
Param. :
pn

25 pn

26 pn

27 pn

28 pn

29 pn

Coeff. : 0.68107E+03 0 0.70320E+03 0 0.70745E+03 0 0.71038E+03 0


0.67749E+03 0 0.68538E+03 0

30

Param. :
pn

31 pn

32 pn

33 pn

34 pn

35 pn

36

Coeff. : 0.67834E+03 0 0.68417E+03 0 0.66762E+03 0 0.67216E+03 0


0.66730E+03 0 0.70961E+03 0
1GSAS S-1
22:33:41 2011 Page 7

GENLES Version Win32 Dec 09

The constraint matrix has 19 terms


1GSAS S-1
22:33:41 2011 Page 8

GENLES Version Win32 Dec 09

Restraint data statistics:


No restraints used

Powder data statistics

Fitted

Bank Ndata Sum(w*d**2) wRp


Hstgm 1 PXC 1 3991 5019.7
Powder totals

3991 5019.7

-Bknd
Rp

Average

wRp

Rp

DWd Integral

0.0394 0.0312 0.0390 0.0337 1.555 0.895


0.0394 0.0312 0.0390 0.0337 1.555

No serial correlation in fit at 90% confidence for 1.909 < DWd < 2.091
Cycle 129 There were 3991 observations.
Total before-cycle CHI**2 (offset/sig) = 5.0197E+03 ( 1.1704E+01)
Reduced CHI**2 = 1.263

for 15 variables

Reflection data statistics


Histogram 1 Type PXC Nobs= 90 R(F**2) = 0.0411

The value of the determinant is 0.6488*10.0**(

-2)

Atom parameters for phase no. 1


frac
x
y
100*U12 100*U13 100*U23

100*Uiso 100*U11 100*U22 100*U33

Calculated unit cell formula weight: 320.394, density: 6.572gm/cm**3

Atom parameters for phase no. 2


frac
x
y
100*U12 100*U13 100*U23
ZN

Zn

100*Uiso 100*U11 100*U22 100*U33

( 1) Values : 1.003 0.333300 0.666700 0.000000


Sigmas :

0.095

Shft/esd:

0.00

moved 0.00A

sum(shift/e.s.d)**2 :

0.827

0.00

( 2) Values : 0.971 0.333300 0.666700 0.383000 -1.288


Sigmas :

0.272

Shft/esd:

0.00

moved 0.00A

sum(shift/e.s.d)**2 :

0.00

Atomic parameter sum(shift/error)**2 for phase 2 :

0.00

Calculated unit cell formula weight: 162.171, density: 5.680gm/cm**3

Atom parameters for phase no. 3


frac
x
y
100*U12 100*U13 100*U23
FE

Fe

100*Uiso 100*U11 100*U22 100*U33

( 1) Values : 1.000 0.000000 0.000000 0.000000


Sigmas :

0.165

Shft/esd:

0.00

moved 0.00A

sum(shift/e.s.d)**2 :

0.00

1.785

Atomic parameter sum(shift/error)**2 for phase 3 :

0.00

Calculated unit cell formula weight: 111.646, density: 7.883gm/cm**3

Phase/element fractions for phase no. 1

Hist Elem:
Fraction :

1 1 PXC
81.7186

Sigmas : 0.282992
Shift/esd:

0.00

Wt. Frac.:

0.61988

Sigmas : 0.815984E-03
1GSAS S-1
22:33:42 2011 Page 9

Phase/element fractions for phase no. 2

Hist Elem:
Fraction :

1 1 PXC
72.7773

Sigmas : 0.670051
Shift/esd:

0.00

Wt. Frac.:

0.27943

Sigmas : 0.185379E-02

Phase/element fractions for phase no. 3

Hist Elem:
Fraction :

1 1 PXC
38.0931

GENLES Version Win32 Dec 09

Sigmas : 0.773815
Shift/esd:

0.00

Wt. Frac.:

0.10069

Sigmas : 0.183946E-02
Phase/element fraction sum(shift/error)**2 :

0.00

Lattice parameters for powder data:


Phase 1
a
Value

alpha

beta

: 4.679240 3.421879 5.125320

gamma

volume

90.000

99.460

90.000

80.950

0.000

0.003

0.000

0.003

Sigmas : 0.000220 0.000156 0.000246


Recprocal metric tensor shift factor = 100%
Phase 2
a
Value

alpha

beta

: 3.245154 3.245154 5.198873

gamma
90.000

Sigmas : 0.000056 0.000056 0.000171

volume

90.000 120.000

0.000

0.000

0.000

47.414
0.002

Recprocal metric tensor shift factor = 100%


Phase 3
a
Value

alpha

beta

: 2.865015 2.865015 2.865015

gamma

volume

90.000

90.000

90.000

23.517

0.000

0.000

0.000

0.001

Sigmas : 0.000051 0.000051 0.000051


Recprocal metric tensor shift factor = 100%
Recprocal metric tensor sum(shift/error)**2 :

0.00

Preferred orientation coeffs. for phase no. 1 axis no. 1:

Histogram:
Ratio

1 PXC
1.03

Sigmas :

0.579E-02

Shift/esd:

0.00

Fraction :

1.00

Sigmas :

0.00

Shift/esd:

0.00

Preferred orientation coeffs. for phase no. 2 axis no. 1:

Histogram:
Ratio

1 PXC
0.936

Sigmas :

0.563E-02

Shift/esd:

0.00

Fraction :

1.00

Sigmas :

0.00

Shift/esd:

0.00

Preferred orientation sum(shift/error)**2 :

CPU times for matrix build

0.00

0.31 sec; matrix inversion

Final variable sum((shift/esd)**2) for cycle 129:

Convergence was achieved

0.00 sec

0.00 Time:

0.31 sec