Self-assembled Transition Metal Coordination Frameworks of ...

Chapter 3 i _ g_ H if 7 7 _, g
methanol and ether and dried in vacuo over P40“). Yield: 0.100 g (57%). Elemental
analysis: Found (calc.): C, 51.46 (51.60); 1-1, 5.01 (4.62); N, 16.17 (16.05); S, 9.09
(9.18)%.
Crystals suitable for X-ray analysis were obtained by slow evaporation of a
methanol solution of 5 in air. The complex 5 crystallized as [Ni(HL7)2]C12' 2‘/zH2O (5'
2‘/1H2O).
[Ni(HL”)L"‘] (:10. 71120 (6)
To a hot solution of HL8 (0.186 g, 0.6 mmol) in 10 ml chloroform was added
an equimolar amount of nicke1(11) perchlorate hexahydrate (0.220 g) dissolved in 20
ml hot methanol. The mixture was refluxed for an hour and allowed to stand at room
temperature. The reddish brown crystals precipitated were filtered, washed with
methanol and ether. It was then dried in vacuo over P.,O|0. Yield: 210 g (78%).
Elemental analysis: Found (calc.): C, 44.65 (45.17); H, 5.32 (5.46); N, 12.28 (12.39);
S, 6.83 (7.09)%.
XRD quality single crystals were obtained by slow evaporation of a solution
of the compound in DMSO. The complex 6 got crystallized with deprotonation, of
HL8 in 6, to form a new complex [Ni(L8)2] (6a).
[NiL”Cl]- 1/21120 (7)
To a hot solution of HL8 (0.186 g, 0.6 mmol) in 10 ml chloroform was added
an equimolar amount of nicke1(1I) chloride hexahydrate (0.143 g) dissolved in 20 ml
hot methanol. The mixture was refluxed for an hour and allowed to stand at room
temperature. The reddish brown compound precipitated was filtered, washed with
methanol and ether and then dried in vac:-:0 over P4010. Yield: 0.138 g (56%).
Elemental analysis: Found (calc.): C, 49.94 (49.49); H, 4.15 (4.40); N, 13.75 (13.58);
S, 7.72 (7.77)%.
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