Self-assembled Transition Metal Coordination Frameworks of ...

Chapter 4 _ f A _,
[Cu;(HL4)Br_;]Br- 31120 (15)
A solution of CuBr2 (0.338 g, 1.5 mmol) in 20 ml of ethanol was added to a
solution of H2L4 (0.320 g, 0.75 mmol) in 40 ml boiling ethanol and refluxed for 20
minutes and allowed to stand at room temperature. Dark colored product separated out
was filtered, washed with methanol followed by ether and dried over P40“) in vacuo.
Yield: 0.320 g (50.6%). Elemental Anal. Found (Calc.): C, 32.44 (32.80); H, 2.45
(2.75); N, 13.37 (l3.30)%. Molar conductivity (AM, 10*‘ M DMF): 93 Q" cmz mol".
[Cu,;(L4)- 2H;0](ClO4)2~ 21120 (16)
A solution of CuClO4- 6H2O (0.378 g, 1 mmol) in 10 ml of methanol was
added to a solution of HZL4 (0.214 g, 0.5 mmol) in 40 ml boiling methanol and
refluxed for ‘/2 h and allowed to stand at room temperature. Dark product separated
out was filtered, washed with methanol and ether and dried over P4010 in vacuo.
Yield: 0.390 g (95.3%). Elemental Anal. Found (Calc.): C, 33.86 (33.75); H, 2.57
(2.96); N, 13.78 (13.a9)%. Molar conductivity (AM, 10"’ M DMF): 164 Q" cmz mol".
[Cu;L4(N_,);]- CH3OH (1 7)
To a boiling solution of H2L“ (0.320 g, 0.75 mmol) in 40 ml boiling ethanol
Cu(CH_,COO)2~ H20 (0.302 g, 1.5 mmol) in 10 ml of ethanol was added followed by
l\laN3 (0.098 g, 1.5 mmol) in hot ethanol and refluxed for 1 h and allowed to stand at
room temperature. Dark colored product separated out was filtered, washed with
methanol, hot water and ether and dried over P4010 in vacuo. Yield: 0.194 g (38.9%).
Elemental Anal. Found (Calc.): C, 43.31 (43.44); H, 2.99 (3.04); N, 29.50 (29.55)%.
Molar conductivity (AM, 10'} M DMF): 12 Q" cmz moi".
[cu2(HL‘)c/_.]- H20 (18)
A solution of CuC12~ ZHZO (0.206 g, 1.2 mmol) in 10 ml of methanol was
added to a solution of H2L° (0.291 g, 0.6 mmol) in 70 ml boiling methanol and
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