J. Phys. Chem. Solids Pergamon Press 1957. Vol. 3. pp. 30-36.

THE CRYSTAL STRUCTURE AND FERRIMAGNETISM

OF YTTRIUM-IRON GARNET, Y,Fe, (FeO,) 3
S. GELLER and M. A. GILLEO
Bell Telephone Laboratories, Incorporated, Murray Hill, New Jersey
(Received 3 April 1957)

Abstract-A refinement of the crystal structure of yttrium-iron garnet (cubic space group--la3d)
has been carried out by application of the least-squares method of calculation to single-crystal X-ray
data. The oxygen parameters are x = -0.0274, y = 0.057,, z = 0.149,; the tetrahedral iron-oxygen
distance is 1.88 a, the octahedral iron-oxygen distance is 2.00 A and the yttrium-oxygen distances
are 2.37 and 2.43 A. None of the oxygen polyhedra is regular even though the space group would
allow the tetrahedra and octahedra to be regular simultaneously.
Interionic distances and angles which are important to the interaction between magnetic ions have
been calculated. The strongest interactions probably occur between FeS+ in 16(a) and 24(d) positions
and between Fes+, 24(d), and MS+, a magnetic rare-earth ion substituted for yttrium, in the 24(c)
positions. Interactions between crystallographically equivalent ions are all small. The number of
interactions per Fes+ ion per formula unit is 3/5 that in a spine1 “ferrite” and, correspondingly, the
Curie temperature observed is 0.64 that of magnetite.
No change of symmetry is observed up to 9OO”C, and the behavior of the lattice constant, a, vs. T
is consistent with the presence of a Curie transition.

INTRODUCTION The first extensive and definitive investigation of

CONSIDERABLEinterest in the rare earth-iron gar-
nets has existed since their discoveryQs2) particu-
larly because they constitute a new family of cubic
ferrimagnetic compounds which belong to space
group 0410)~Iu3d which was not previously en-
countered in studies of magnetic oxides. There are
now the possibilities of testing previously estab-
lished ideas of magnetic interactions on these new
compounds and of expanding some of these ideas
because these compounds represent the first case
in which rare-earth ions are known to contribute to
the spontaneous magnetization.(1*3*4*5)
A quantitative understanding of the interaction
between magnetic ions requires an accurate deter-
mination of the positions of all ions. For yttrium-
iron garnet this has been made possible by the
availability of single crystals produced by NIEL-
SEN.(‘)
The excellent and extensive work of MENZER(‘)
on the natural garnets established the structure,
although, because X-ray diffraction intensities from
powders were used, great accuracy could not be
attributed to the 02- ion parameters.
30
the role of yttrium and aluminum in the garnet
structure was made by YODER and KEITH@) who
studied the system
(Mu,-,Y,) Al, (Si3-,A1,)Q2.
They succeeded in synthesizing the compound
Y,Al,(AlO,),, an yttrium-aluminum garnet. Later,
KEITH and ROY,(~) in an investigation of reaction
products of rare-earth and transition-metal oxides,
produced garnets : Y,Ga2(Ga04),, Sm,Al,(AlO,)s,
Sm,Ga,(GaO,),. Attempts by the latter authors to
produce the garnet Sm,Fe,(FeO,), were un-
successful.
Recently BERTAUTand FORRAT discovered that
spontaneous magnetization, originally attributed
by others to a perovskite-like phase, actually
originated in a garnet phase which was present.
This phase had probably resulted from incomplete
reaction of the mixed oxides. In these Laboratories
the ferrimagnetism in rare earth-iron garnets was
discovered independently and in a different way
which has been described in a previous communi-
cation.@) Our magnetic data on Y3Fe2(Fe04), are
 CRYSTAL STRUCTURE AND FERRIMAGNETISM
in agreement with those of ALBONARD,BARBIERand
PAUTHENET.(~)The work of PAUTHENETon gado-
linium-iron garnet@) has clarified the interpretation
of data previously in disagreement with that of
GILLEO on GdFeO,,@O) Recent work by BERTAUT
and PAUTHENETQ’)establishes the magnetic pro-
perties and cell sizes of a large number of rare
earth-iron garnets.
A neutron diffraction study of yttrium-iron gar-
net has been carried out by BERTAUTet uE.@~)and
by PRINCEW of these Laboratories. A neutron
diffraction study must establish the oxygen para-
meters and the magnetic structure.* The results of
the two investigations are essentially in agreement
with regard to the magnetic nature of the
Y,Fe,(FeO,),, but there are differences in the
oxygen parameters. The single crystal analysis,
which should give more accurate results, leads to a
set of oxygen-ion parameters which, except for the
x-co-ordinate, lie between the two sets obtained by
the different authors.
The crystal used to obtain the data for this analysis is
a sphere of 0.23 mm diameter made from a single crystal
produced by NIELSEN. To obtain adequate intensity of
the most important reflections in reasonable exposure
time, Co& radiation was used. The crystal was aligned
along a [I101 direction and all odd-numbered layer&net
photographs were taken about this direction. The inten-
sities were estimated visually by comparison with an
intensity scale. The following factors were applied to the
layer-line data to convert intensities to lFl* values:
LORENTZ-polarization, TUNELL rotation,(i4) absorption,
and spot extension corrections.(‘6) Tables prepared by
BOND were used for the absorption correction. Be-
cause several reffections were common to two or more
photographs, it was a simple matter to put all reflections
on the same scale. Further data for determination of the
space group were obtained from Buerger precession
photographs taken with a [loo] direction as the precession
axis.
High temperature experiments
Samples used in these experiments were prepared by
coprecipitation of the hydroxides from nitric acid solu-
tion. The washed mixture of hydroxides was dried at
2OO”C, ground in an agate mortar, heated gradually to
6OO’C over a period of 4 hr, kept at 600% for two
* The previously unknown yttrium neutron scattering
cross section must also be determined. For this reason a
neutron diffraction study of YSAII(AIOI)s has also been
carried out by PRINCE.
t WEISSENBERG.
OF YTTRIUM-IRON GARNET 31
hours and then reground. Samples were prepared in
pellet form and fired at 1450% for 16 hr in oxygen.
Powder taken from one of the pellets was put into a thin-
walled glass capiIlary$ which was mounted in a high
temperature camera designed and built by BONDof these
Laboratories. Lattice constants were determined from
photographs taken at various temperatures (Fig. 4) with
CoK radiation.
REFINEMENT OF THE STRUCTURE
The symmetry of the single crystal photographs
is O~+n3m and only the following types of reflec-
tions are present: (Ml), h+K+Z = 2n; (Z.&O),
h = 2n, K = 2n; (hhl), I = 2n, 2h+Z = 4n. Thus
O,(lO)-Iu3d§ is uniquely established as the most
probable space group for YsFe,(FeO,)s. The room
temperature lattice constant, which was determined
from a powder photograph, is 12.376 A (probably
IfrO.004 A). There are eight formula units in the
cubic unit cell; the corresponding X-ray density is
5.17 g/cm3.
The results of this analysis and that of PRINCE
indicate that YsFe&FeO& is isostructural with the
natural garnets. In the garnet type structure the
ys+ ions occupy positions 24(c), Fe3+ ions occupy
positions 24(d) and 16(a), and oxygen ions occupy
positions 96(h). Of these positions only the 96(h)
involve parameters (x, y, z) which must be refined.
It is fortunate that in this structure there is a
substantial number of reflections which have con-
tributions from the oxygen ions only. These have
two indices odd and the third divisible by 4.
Furthermore there is an even larger number of
reflections to which there is no contribution from
the 16(a) Fe 3+ ions. The contribution from the re-
maining ions is eight times the difference between
the scattering of yttrium and iron. These were,
therefore, the only reflections used in the refine-
ment. Those to which the metal atoms contribute
very heavily have been given zero weight.
The contributions of the oxygen ions to the structure
amplitudes were calculated on the IBM 650 computer
using PRINCE’S parameters (Table I). The programming
and calculation were carried out by BOOTH. The
J A fused silica capillary was used for the photograph
taken at 600 and 900°C (Fig. 4).
3 Below the Curie temperature, the crystal possesses
spontaneous magnetization in one direction in each mag-
netic domain so that the symmetry cannot be truly cubic
even though deviations from cubic symmetry are not
detected by X-ray diffraction.
32 S. GELLER AND M. A. GILLEO

scattering factors for the yttrium and iron ions were ob-
tained from the International Tables(18) and for oxygen
ions from the paper by BERGHUIS et a1.(18) Corrections
were made for ionicity; these were, of necessity, some-
what arbitrary. Because several of the reflections resulted
exclusively from oxygen ion contributions, it was not too
difficult to estimate a temperature factor for the oxygens
and a scale factor by which the observed structure ampli-
tudes were placed on an absolute basis. The temperature
factor so deduced for the oxygen ions was 2.0 A”. In the
initial calculations zero temperature factors were assumed
for the Y3+ and Fe3+ ions, although it was recognized that
this was physically impossible.
Table 1. Oxygen parameters obtained by neutron
for space group O,(lO)-Ia3d was worked out by Miss
D. C. LEAGUS of these Laboratories and the calculation
carried out by Mr. A. H. HATCH of IBM. The reflection
amplitudes involved had two indices odd and the third
divisible by 2. Thus only (hhl) reflections were weighted
one-half. _\I1 other (hkl) reflections were weighted one
except those which were not observed. These were given
very low weights, and were included in the calculation
because only then would the program give the calculated
structure amplitude for these reflections. After the first
iteration, changes in co-ordinates were very small, so
that u-e had confidence in the final parameters. The re-
sults of the last three iterations are given in Table 2. The
values given in the last row of this table are considered
to be the final ones.

dzflraction
PRINCE(‘~]
BERTAUTet Al. ~ 1.;:: 1 ::;a: ~ ::i
Some time after PRINCE had obtained the oxygen
parameters from neutron diffraction data, the results of
BERTAUT et CZ~.(‘~)appeared (Table 1). The differences
between the y and z parameters of these two sets are
rather substantial and amount to 0.07 and 0.04A
respectively. Calculations of structure amplitudes were
carried out with the parameters of BERTAUTet al. It ap-
peared that neither set was entirely satisfactory as far as
the X-ray data were concerned. Examination of the re-
sults indicated that the set of parameters which would
best satisfy the X-ray data probably would be somewhere
between the two sets.
The oxygen parameters obtained by PRINCE were used
as a starting point for the least-squares refinement of the
structure. These calculations were carried out on the
IBM 704 computer. The main program used was that
devised by Dr. D. SAYRE of IBM* ; the auxiliary program
* Only diagonal terms in the least-squares matrix are
computed.
A comparison of calculated with observed struc-
ture amplitudes is given in Table 3. If the (hhl)
structure factors are weighted one-half and the
unobserved reflections counted as one-half the
minimum observable reflections, the discrepancy
factor, ( C 1IF01-IF,_\ I/ ;T,IF01), is 9.2 per cent.
If the unobserved reflections are excluded, 8.5 per
cent is the result. The discrepancy factor for the
sixteen observed reflections resulting from
oxygen-ion contributions only is 9.2 per cent. AS
calculated from the least-squares data, the errors in
co-ordinates are
CT(X)= o(y) = rs(z) = 0.0009.
Apparently the evidence speaks for high accuracy
of the oxygen parameters, even though it is possible,
and even probable, that the accuracy is not quite
as high as indicated by the numbers.
It is worth noting that the agreement for the
reflections from oxygen-ions only is as good as it is
for the other reflections. Also the interaction of the
positional and temperature parameters appears to
be negligible. Intensities for neutron diffraction

Table 2. Results of last three least-squares iterations

___~

Temperature

I ~~
Oxygen co-ordinates
factors A*

-0.x0272 0.0:71 0.12490 2.11

0*- 0.179
Y3+ 0.598
Fe*+ I 0.993 10.8
-0.0276 0.0572 0.1494 2.03 0.148 0.655 0.983 9.7
-0.0274 0.0572 0.1492 2.05 0.161 0.631 0.988 9.6

* These values are actually high. They do not consider the half-weighting of the (hhl) amplitudes
and do include the unobserved reflections counted as half the minimum observable F.
 CRYSTAL STRUCTURE AND FERRIMAGNETISM OF Y~RIU~-IRON GARNET 33

Table 3. Comparison of calculated with observed structure amplitudes

Amplitude Amplitude Amplitude

W) Obs. Calc. W) Obs. Calc. Obs. - Calc.
_-
121 84.1 -100*5 671 < 31.5 20.4 581 46.3 49.1
123 57.9 -68.3 673 60.2 -71.1 583 60.5 -71.0
125 169.9 -160.7 677 26.1 -34.8
127 83.8 -89-6 679 95.8 85-4 691 86.1 80-l
129 55.3 -58.7
1,2,11 95-o -95.8 781 25.3 -25.5 7,10,1 90.3 84.7
1,2,13 24.8 -38.5 783 < 25.6 4.6 7,10,3 71.1 68.7
785 < 21.6 6.2 7,10,5 50.0 56.1
233 59.0 -71%5
235 145.6 -141.7 891 39.7 42.7 8,11,1 < 8.7 -6.6
237 30.0 24.5 893 < 18.7 4.0
239 73.3 -76.8 895 14.4 19.9 161 182.5 207.3
2,3,11 68.0 66.6 1,6,11 68.4 67.3
2,3,13 68.5 -76.9 9,10,1 61.9 -71.2
277 90.5 92.5
341 86.1 95.4 147 38.0 42.3 279 40.0 46-9
345 < 33.4 -15.4 149 51.3 -56.5 2,7,11 81.4 82.2
347 41.5 43.8 1,4,11 26.5 -21-4
349 38.5 -38.7 1,4,13 < 8.7 6.0 381 < 34.9 -17‘S
3,4-J 1 23.8 20.3
25.5 125.4 -141.9 5,10,1 128-O -106.6
451 26.0 -25.1 2.57 48.7 41.0 5,10,3 79.9 -71.9
457 59.1 59.7 259 61.4 -69.9 5,10,5 59.5 -59.1
459 < 25.6 -11.0 2,5,11 76.2 74.3
4,5,11 < 16.3 -8.1 299 91.6 -93.8
361 46.4 -44.1
561 78.5 86.8 363 56.2 -59.5 3,10,1 62.4 61.6
563 39.4 41.5 369 77.0 -70.0 3,10,3 74.3 89.4
565 120.4 117.4 3,6,11 116.8 -109.6
567 115.6 112.9 5,12,1 < 16.2 -7.4
569 75.3 75.6 479 < 20.1 4.6 .5,X2,3 27.5 29.8
5,6,11 62.4 69.5 4,7,11 31.3 35.3

which were calculated with the oxygen parameters

obtained by the analysis described herein are still
in good agreement with the intensities observed by
PRINCP . . (13)

DISCUSSION
In the garnet structure each of three positive-
ion positions is associated with a different co-
ordination polyhedron of oxygen ions: for
F+[24(c)] an eight-cornered twelve-sided figure
(Fig. 1); for Fe3+ [16(a)] an octahedron (Fig. 2);
for Fe* [24(d)] a tetrahedron (Fig. 3). None of
these polyhedra is regular with respect to edge FIG. I. Co-ordination polyhedron of oxygen ions about
length even though the oxygen parameters would the yttrium ion
permit the octahedra and tetrahedra to be reguIar (* 2.68, . - 2.81, - - - 2.87, * - . - 2.96 A).
c
34 S. GELLER AND M. A. GILLEO

Table 4. Nearest-neighbor interionic distances in

yttrium-iron garnet

Ion Interionic distances (A)

Y3+ ’ 4Fe3+(n) at 3.46

6Fe3’-(d) at 3.09(2), 3.79(4)
80”- at 2.37(4), 2.43(4)

Fe3+(a) 2y3+ at 3.46

6Fe3+(d) at 3.46
602- at 2.00

Fe3+(d) 6Y3+ at 3.09(2), 3.79(4)

4Fe3+(a) at 3.46
4Fe3+(d) at 3.79
FIG. 2. Co-ordination octahedron of oxygen ions about 402- at 1.88
an F@+(a) ion (. 2.68, . 2.99 8).
0% ~ 2Y3f at 2.37, 2.43
1Fe3+(a) at 2.00
lb-es+(d) at 1.88
902- at 2.68(2), 2.81, 2.87,2.96,2.99(2),
3.16(2)

Table 5. Interionic angles in yttrium-iron garnet

Ions Angles (“)

Fe3+(a)-Ozm-Fe3+(d) I 126.6
FIG. 3. Co-ordination tetrahedron of oxygen ions about Fe3+(a)-O*--_Y3+* 102.8
an Fe3+(d) ion (. 3.16 A, . 2.87 a). Fe3+(a)-0zm-Y3+t 104.7
Feat(d)-02KY3+* 122.2
Fe3+(d)-O*m-Y”+t 92.2
simultaneously.(‘) However in the latter two y”+ -[j” -_y3+ 104.7
polyhedra all center-to-corner (Fe3+-02-) distances
are equal (Table 4): for the octahedra 2.00 A; for Fez+(a)-Oe -Fe3+(a) (4.41): 147.2
Fez+(d)-O*--Fe3+(d) (3.41) ; 86.6
the tetrahedra I .88 A. There are two diRerent 02-
Fe3+(d)~O~~Fe3+(d) (3.68) 78.8
Fe3-+-02- angles in each case: for octahedra 87.2” Fe3+(d)-O? -Fe3+(d) (3.83) 74.7
and 96.6”; for tetrahedra 99.9” and 114.3”. Each Fe3+(d)-Om-Fe3+(d) (3.83) 74.6
oxygen ion is common to two eight-cornered poly-
hedra, one octahedron and one tetrahedron. Thus * Y3+-02~~ distance = 2.43 PI.
each oxygen ion has as nearest positive-ion neigh- A Y3+-Ozm distance ~~ 2.37 A.
bors two Y3+, one Fe3+(a) and one Fe3+(d) ions
: Numbers in parentheses are the longer Fe3+(n or d)-
(Tables 4 and 5). This feature of the structure is Ozm distances. The shorter distances (Table 4) are
most important to the magnetic properties. Fe3+(a)-O* = 2.00, Fe3+(d)-O-- = 1.88 A.
The “exchange” interaction of two magnetic
ions, Me, through an oxygen ion between them was The interaction increases with the overlap and,
first conceived by KRAMERS(~~)and has since been accordingly, will be greatest for short Me-0 dist-
more extensively studied by ANDERSON and ances and for Mel-O-Me2 angles near 180”. There-
VAN VLECK.@) In this interaction the overlap of fore in yttrium-iron garnet the strongest interac-
the 2p electrons (with dumbbell-shaped distribu- tion (Table 5) will probably occur between Fe3+(a)
tion) of the oxygen ion with the electronic distri- and Fe3+(d) for which the Fe3+(a)-02--Fe3+(d)
bution of the magnetic ions is an important feature. angle is 126.6”. Because interaction of this type is
 CRYSTAL STRUCTURE AND FERRIMAGNETISM
known to be negative in ferrites, as was first recog-
nized by N&EL,@~) and because there are 3Fe3+(d)
and 2Fe3+(a) ions per formula unit, there should be
a net magnetic moment corresponding to that of
one Fe3+, i.e. .5pLg, Verification of this expectation
is found in measurements of the saturation mag-
netization, 0, ,0, reported by ALBONARDet al.@) and
by US.(~) The neutron diffraction studies of
BERTAUT et aZ.Q2)and PRINCE of these Labora-
tories establish that the alignment of the ionic
moments is as assumed.
If yttrium is replaced by a rare-earth ion, M3+,
we might expect a strong interaction only with
Fe3+(d) ions for which the M3+-02--Fe3+(d) angle
is 122.2” (Tables). In this case om,,, would corres-
pond to 3ne(M3+)-5 per formula unit as has been
observed by PAUTHENET(~)for all rare-earth ions
from Gd to Lu and verified by us for Gd.
In a comparison of the garnets with the ferrites,
several important differences in magnetic inter-
action are noticed. There is probably no appreci-
able interaction between magnetic ions in equiva-
lent sites in a garnet structure since either oxygen-
magnetic ion distances are too large or the Me,-
O-Me, angle is nearly 90” (Table 5). In the spine1
structure, each octahedral iron ion can interact
appreciably with twelve other octahedral iron ions.
YAFET and KITTEL@“) first suggested that simple
parallel and anti-parallel alignment of magnetic
ion moments may not occur in this case. Non-
parallel moments of Cr3+ in octahedral sites were
first observed in CuCr,O, by PRINCE.
Another difference in these two structures is
found in the number of other magnetic ions with
which a given ion simultaneously interacts most
strongly. In a formula unit of garnet each of two
octahedral ions, 16(a), interacts with six tetrahedral
ions, 24(d), and each of three tetrahedral ions
interacts with four octahedral ions, corresponding
to a total of twenty-four interactions. In a formula
unit of spine1 each of two octahedral ions, 16(d),
interacts with six tetrahedral ions, 8(u), and each
tetrahedral ion interacts with twelve octahedral
ions, also corresponding to a total of twenty-four
interactions. However, there are five magnetic ions
per formula unit of yttrium-iron garnet, but only
three in a spinel. Therefore the number of inter-
actions per ion and, consequently, the strength of
interaction per magnetic ion in garnet is 3/S that in
spinel. Because the strength of interaction] N KT,,
OF YTTRIUM-IRON GARNET 35
a lower Curie temperature, T,, would therefore be
expected for yttrium-iron garnet (T, = 54S°K)*
for which it is 0.64 that of magnetite (848”K).t
The comparison of the interaction distances and
angles in the yttrium-iron garnet with those in a
spine1 may be made by referring to the case of
manganese ferrite (MnFe,O,) for which HASTINGS
and CORLISS(~~) have accurately determined the
oxygen parameter. In this material the Me(a)-O-
Me(d) angle is 123.0” compared with Me(a)-O-
Me(d) angle of 126.6” for yttrium-iron garnet
(Table 5). The distance of an oxygen ion from
positive ions in the tetrahedral sites in manganese
ferrite is 1.95 A compared with 1.88 A for yttrium-
iron garnet. The larger value would be expected in
manganese ferrite because about 80 per cent of the
tetrahedral sites are occupied by Mn2+,(26) an ion
of larger radius than Fe3+. The octahedral ion-
oxygen ion distance is 2.01 a in the ferrite and
2.00 A in the garnet.
The ferrimagnetism of yttrium-iron garnet is
distinguished from that of ferrites in another im-
portant way. In the garnet each Fe3+(u) ion inter-
acts only with Fe3+(d) ions, i.e. all 16(u) or 24(d)
ions are not only crystallographically but also mag-
netically equivalent. This is never the case for the
16(d) ions in magnetic ferrites because these
ferrites are never entirely normal, i.e. the divalent
ions are never solely in the tetrahedral, S(u),
positions but a fraction of these ions is distributed
at random on the octahedral, 16(d), sites.
The yttrium-iron garnet structure is a rather
loose one: The X-ray density of Y,Fe,(FeO,), is
5.17 g /cm3 with a volume of 236-9 A3 per formula
unit. If one Fe per formula unit could be replaced
by a heavier Y with no structure change the den-
sity of the resulting 4YFe0, would be 5.40 g/cm3.
Actually the density of the perovskite-like com-
pound, YFeO,, is 5 -67 g/cm3 and the volume
225.9 A3.(27) Because no metal ion to oxygen ion
distances appear to be unduly long (Table 4) the
arrangement of oxygen ions in the garnet appears to
be inefficient.
The variation of the lattice constant, uo, with
* From measurements on a single crystal furnished by
Nielsen of these Laboratories.
t The structure dependence of the Curie temperature
and the strength of the Fe-O-Fe interaction will be dis-
cussed in more detail elsewhere (M. A. GILLEO, to be
published).
36 S. GELLER
temperature for yttrium-iron garnet differs from
that of a typical natural garnet, grossularite(28)
(Fig. 4). The variation of slope of the a, VS. T
OK
Temperature
FIG. 4. Lattice constant vs. temperature for yttrium-irora
garnet and grossularite.@8)
curve in the neighbourhood of 272°C is consistent
with the presence of a Curie transition at this tem-
perature. The precision of the data (-&to.004 A)
does not permit us to establish the shape of the
curve in more detail than that of the two straight-
line approximations employed.
Acknowledgements-The authors wish to thank
Dr. J. W. NIELSENfor making available the crystals
used in this study, Dr. E. PRINCEfor his interest
and for supplying us with the results of his neutron
diffraction analyses, Messrs. V. B. BALAand D. W.
MITCHELLfor technical assistance, and Mr. H. M.
YATESfor the drawings in this paper.
We wish also to thank Dr. CAROLINEW.
~A~G~LLA~RY for her kindness in sending us the
mass absorption coefficients of the elements for
Co& radiation.
AND M. ,k. GILLEO
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