REPORT & JOURNAL

REVIEW
Crystal Growth & Solid State Chemistry Laboratory
University of Malaya, 50603, Kuala Lumpur

(20 April 2016)

Pb-3,4 pydc solvothermal

synthesis with cooling down
variation

JOURNAL REVIEW:
Variation of Solvent Molecule in Synthesizing Porous Coordination Polymer
Mursel Arc et al.

[Zn2(6-ao2btc)(-obix)2]n

[Zn2(4-ao2btc)(-obix)2]n
ao2btc = dioxygenated form of 3,3, 5,5- azo
benzenetetracarboxylate
obix = 1,2-bis(imidazol-1-ylmethyl)benzene

JOURNAL REVIEW:

[Zn2(4-ao2btc)(-mbix)2]n

[Zn2(4-ao2btc)(-pbix)2].2DMF.10H2O
ao2btc = dioxygenated form of 3,3, 5,5- azo
benzenetetracarboxylate
mbix, pbix = 1,3- and 1,4-bis(imidazol-1-ylmethyl)
benzene

JOURNAL REVIEW
Catalysis
Gas
adsorption

Gas storage/
separation
Application fields of
Coordination
Polymer

Iodine
encapsulation

Sensor
Luminescence

JOURNAL REVIEW

usually contain guest (solvent) molecules in

their pores
After activation, flexible structures can
collapse or their pores may be closed or
contracted
activation plays a key role in the gas

adsorption process of a flexible structure

Starting Materials
1. [Zn2(6-ao2btc)(-obix)2]n

3. [Zn2(4-ao2btc)(-mbix)2]n

H4abtc
Zn(NO3)26H2O
DMF/EtOH / H2O (5:3:1 v/v/v)
1,2-bis(imidazol-1-ylmethyl)
benzene (obix) ligand

same as 1, except the ligand is:

1,3-bis(imidazol-1-ylmethyl)
benzene (mbix)

After 30 min, HNO3 is added

4. [Zn2(4-ao2btc)(-pbix)2].2DMF.10H2O
2. [Zn2(4-ao2btc)(-obix)2]n
H4abtc
Zn(NO3)26H2O
DMF/H2O (10:2 v/v/v)

H4abtc
Zn(Cl)26H2O

DMF/H2O (10:2 v/v)

1,4-bis(imidazol-1-ylmethyl)
benzene (pbix) ligand

After 30 min, HNO3 is added

Result & Discussion

Zn(II) ions are bridged by 3,3- and 5,5carboxylate oxygen atoms of abtc ligand in a
monodentate fashion

Two pbix ligands bridge two Zn(II) ions to form a

Zn2(pbix)2 26-membered ring with dimensions of
10.585 8.432 2 along the c-axis.

Result & Discussion

Effect of Guest Molecule in Pores for Gas Sorption Studies of Flexible Structures.
The compound activated in two different ways, solvent exchange + heating
and direct heating, to investigate pore properties
For activation, the compound is immersed in MeOH for 1 week at room
temperature, and then heated to 105 C

Result & Discussion

4b contains only DMF molecules in the pores,
DMF molecule acted as a column in the
pore

Result & Discussion

The compound seems

nonporous
N2 adsorption seems to have a
flexible structure
4b is higher than 4a -> closing
or contracting of pores

Result & Discussion

The CO2 uptake capacities for

4a and 4b are 18.43 cm3/g
and 48.40 cm3/g
Langmuir surface areas of 4a=
167.4 m2/g, 4b = 350.7 m2/g
Fig: CO2 adsorption-desorption isotherms at 273 K

These results confirm the importance of solvent molecules

in pores for the flexible structure