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Self-assembled Transition Metal Coordination Frameworks of ...

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Chapter 4 _, W<br />

washed with methanol and ether and dried in vacuo over P40“, Yield: 0.286 g<br />

(93.4%). Elemental Anal. Found (Calc.): C, 45.48 (45.10); H, 3.78 (3.21); N, 18.28<br />

(18.29); S, 5.35 (5.24)%.<br />

[Cu4L22)- 21120] (C104). (9)<br />

A solution <strong>of</strong> CuCl04- 6H;0 (0.378 g, 1 mmol) in 10 ml <strong>of</strong> methanol was<br />

added to a solution <strong>of</strong> H2L2 (0.220 g, 0.5 mmol) in 10 ml chlor<strong>of</strong>orm and refluxed for<br />

‘/2 h and allowed to stand at room temperature. Brown product separated out was<br />

filtered, washed with methanol followed by ether and dried over P4010 in vacuo.<br />

Yield: 0.326 g (83.7%). Elemental Anal. Found (Calc.): C, 38.38 (38.57); H, 2.92<br />

(2.59); N, 10.45 (10.79); S, 4.16 (4.l2)%. Molar conductivity (AM, 104 M DMF): 5<br />

Q" cmz mol".<br />

[Cu;(HL2)Br;]Br- H20 (10)<br />

A solution <strong>of</strong> CuBr2 (0.226 g, 1 mmol) in 10 ml <strong>of</strong> methanol was added to a<br />

solution <strong>of</strong> H21] (0.220 g, 0.5 mmol) in 10 ml chlor<strong>of</strong>orm and refluxed for I/2 h and<br />

allowed to stand at room temperature. Brown product separated out was filtered,<br />

washed with methanol followed by ether and dried over P4010 in vacuo. Yield: 0.313<br />

g (76.3%). Elemental Anal. Found (Calc.): C, 36.00 (36.60); H, 2.14 (2.58); N, 9.96<br />

(10.24); s, 3.66 (3.91)%. Molar conductivity (AM, 10*‘ M DMF): ss Q" cmz mar‘.<br />

[Cu;(HL3) cz_.]~ 21120 (11)<br />

A solution <strong>of</strong> CuCl;- 2H20 (0.265 g, 1.5 mmol) in 10 ml <strong>of</strong> methanol was<br />

added to a solution <strong>of</strong> HZL3 (0.291 g, 0.75 mmol) in 40 ml boiling methanol and<br />

refluxed for 10 minutes and the reddish solution allowed to stand at room temperature.<br />

Brown product separated out was filtered, washed with methanol followed by ether<br />

and dried over P40“, in vacuo. Yield: 0.435 g (88.8%). Elemental Anal. Found<br />

128

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