Self-assembled Transition Metal Coordination Frameworks of ...

Chapter 2
chloroform solution and dried over P4010 in vacuo. Yield: 80%. M.p. 188 °C.
Elemental analysis: Found (calc.): C, 62.30 (63.00); H, 4.32 (4.14); N, 25.19 (25.55);
S, 7.27 (7.31)%.
1, 5-Bz's(2-benzoylpyridine) thiocarbohydrazone (H 2L2)
2-Benzoylpyridine (0.800 g, 4.4 mmol) in 10 ml methanol was added to
thiocarbohydrazide (0.216 g, 2 mmol), dissolved in hot methanol (40 ml). The
solution was refluxed for 3 h after adding a drop of 6 M HCl, and on cooling a yellow
crystalline solid precipitated. This was then filtered, washed with methanol and ether,
recrystallized in chloroform solution and dried over P4010 in vacuo. Yield: 75%.
Elemental analysis: Found (calc.): C, 68.70 (68.78); H, 4.62 (4.62); N, 19.25 (19.25);
S, 7.07 (7.35)%.
I , 5 -Bis( quinoline-2-carbaldeh yde) th iocarbohydrazone (H 2L3)
Quinoline-2-carboxaldehyde (0.680 g, 4.2 mmol) in 10 ml methanol was
added to thiocarbohydrazide (0.216 g, 2 mmol) dissolved in hot methanol (70 ml).
After adding a drop of hydrochloric acid, the solution was refluxed for 1 h and on
cooling a yellow solid precipitated. It was then washed with methanol and ether,
recrystallized in acetonitrile solution and dried over P40“, in vacuo. Single crystals
suitable for X-ray analysis were obtained by slow evaporation of its acetonitrile
solution. Yield: 75%, M.p 182 “C. Elemental analysis: Found (calc.): C, 65.27
(65.61); H, 4.30 (4.19); N, 22.18 (21.86); S, 8.18 (8.34)%.
1,5-Bi.s‘(di-2-pyridyl ketone) carbohydrazone (H 2L4)
Di-2-pyridyl ketone (0.391 g, 2.1 mmol) in methanol (10 ml) was added to
carbohydrazide (0.092 g, 1 mmol) dissolved in hot methanol (30 ml). After adding 2
drops of glacial acetic acid, the resulting solution was refluxed for 2 h and on cooling
yellow white crystals were precipitated. These crystals were filtered, washed with
40