Self-assembled Transition Metal Coordination Frameworks of ...

Chapter5 __ ,4 4 4 4 __ _,
after three days was filtered, washed with methanol followed by ether and dried over
P4010 in vacuo. Yield: 0.364 g (63%). Elemental Anal. Found (Calc.): C, 52.54
(52.46); H, 3.69 (4.05); N, 14.75 (14.54); S, 5.45 (5.55)%.
[Mn;(HL3)L3(N3)- 2H;O]- 2H40 (20)
To a boiling solution of HZL3 (0.388 g, 1 mmol) in 60 ml methanol,
Mn(CH3COO);- 4H2O (0.247 g, 1 mmol) in 10 ml of methanol was added with a drop
of dil HCl and refluxed for 5 minutes. lt was then added NaN;, (0.131 g, 2 mmol) in
boiling methanol and refluxed for 1 h and allowed to stand at room temperature.
Orange brown product separated out was filtered, washed with methanol, hot water
and ether and dried over P4010 in vacuo. Yield: 0.335 g (68%). Elemental Anal. Found
(Calc.): C, 50.50 (50.96); H, 3.55 (3.77); N, 21.53 (21.23); S, 6.57 (6.48)%.
[Mn;(H2L4)HL4];(ClO4)6-IOHQO (21)
To a boiling solution of HQL4 (0.212 g, 0.5 mmol) in 20 ml methanol,
Mn(ClO4)2- 6H2O (0.365 g, 1 mmol) in 10 ml of methanol was added with a drop of
HCIO4 and refluxed for 1 h and allowed to stand at room temperature. The orange
white powder precipitated was filtered, washed with methanol and ether and dried in
vacuo over P4010. Yield: 0.290 g (86%). Elemental Anal. Found (Calc.): C, 41.09
(41.16); H, 3.98 (3.38); N, 17.23 (16.70)%.
[Mn/H2L5)HL5 ]Z(c104),,- 131140 (22)
To a boiling solution of H41.‘ (0.169 g, 0.4 mmol) in 20 ml methanol,
Mn(ClO4)2' 6H;4O (0.292 g, 0.8 mmol) in 10 ml of methanol was added with a drop of
HCIO4 and refluxed for 1 h and allowed to stand at room temperature. White yellow
product separated out was filtered, washed with methanol, followed by ether and dried
over P4O|0 in vacuo. Yield: 0.160 g (59%). Elemental Anal. Found (Calc.): C, 44.13
(43.99); H, 4.24 (3.84); N, 12.37 (l2.31)%.
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