Self-assembled Transition Metal Coordination Frameworks of ...

g pg __ V g A Zinc(II) & Cadmium(II) complexes
[Zn(HL‘)14(BP‘.)4- cm0H~ 2H20 (2 8)
4
To a hot solution of H11.’ (0.256 g, 0.6 mmol) in 40 ml methanol was added
an equimolar amount of Zn(BF4)2~ 2H2O (0.144 g) dissolved in 10 ml hot methanol.
The orange colored solution was then refluxed for 1 h and allowed to stand at room
temperature for slow evaporation. The orange powder precipitated after evaporation
was washed with methanol and ether and dried in vacuo over P4010. Yield: 0. 194 g
(54%). Elemental Anal. Found (Calc.): C, 48.97 (49.07); H, 3.52 (3.37); N, 19.92
(l9.70)%.
[Z~(HL5)].(BF.)4- 101120 (29)
A solution of the HZLS (0.215 g, 0.5 mmol) in 10 ml chloroform was added to
a solution of Zn(BF4)2- 2H2O (0.120 g, 0.5 mmol) in methanol (20 ml) and refluxed
for 1 h. The yellow crystalline solid which formed after a week was filtered, washed
with methanol and ether and dried in vacuo over P4010. Yield: 0.180 g (58%).
Elemental Anal. Found (Calc.): C, 48.87 (48.69); H, 4.12 (3.92); N, 13.60 (l3.63)%.
Crystals suitable for X-ray structure determination were obtained from slow
evaporation of a chloroform: methanol mixture solution of 29 in air.
6.2.3. Synthesis of Cd(II) complexes
[Cd(H;L')]4(N03),,~ s1-120 (30)
To a hot methanolic solution of H2151 (0.440 g, l mmol) was added an
equimolar amount of Cd(NO;);- 4H;O (0.311 g) dissolved in 10 ml hot methanol. The
orange colored solution was then boiled for 5 minutes and filtered. This was boiled for
45 minutes and allowed to stand at room temperature for slow evaporation. The
orange transparent plates precipitated after evaporation was collected and washed with
ether and dried in 1-'acru0 over P4010. Yield: 0.600 g (84%). Elemental Anal. Found
(Calc.): C, 38.37 (38.86); l-I, 3.29 (3.12); N, 19.69 (19.70); S, 4.87 (4.51)%.
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