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[15] General procedure for the synthesis of the complexes
[NiCl2{C5H3N-2,6-(CHNArf)2}]. All complexes were synthesized
by the following method illustrated for the synthesis of
[NiCl2{C5H3N-2,6-(CHNC6H3-2,3-F2)2}] (1).
Synthesis of [NiCl2 {C5H3N-2,6-(CHNC6H3-2,3-F2)2}] (1). A
solution of the ligand {C5H3N-2,6-(CHNC6H3-2,3- F2)2} (120 mg,
0.33 mmol) in anhydrous CH2Cl2 (10 mL) was added to a stirred
solution of NiCl2 Æ 6H2O (0.078 g, 0.33 mmol) in absolute meth-
anol (10 mL). The resulting green solution was stirred at room
temperature for 2 h. After this, an orange suspension is noted and
the solvent evaporated in vacuo. The product was purified by
recrystallization from MeOH. The resulting precipitate was
filtered washed with hexane (3 · 5 mL) and dried under vacuum.
Crystals suitable for single crystal X-ray diffraction studies were
obtained from a dichloromethane/methanol (4:1) solution. An
orange solid (142 mg) was obtained in 88% yield. Mp: 240 ꢁC
(decomp). FT-IR (KBr): mmax 1587, 1490 (C@N), cmÀ1. Elem.
Anal. Calc. for [C19H11Cl2F4N3Ni] (486.92): C, 46.87; H, 2.28;
found: C, 46.87; H, 2.39. MS-FAB+ [M À Cl]+ = 450 (100%),
[M À 2Cl]+ = 415 (68%) m/z.
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Synthesis of [NiCl2{C5H3N-2,6-(CHNC6H3-2,5-F2)2} (2).
{C5H3N-2,6-(CHNC6H3-2,5-F2)2} (120 mg, 0.33 mmol) and
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(KBr): mmax 1595, 1498 (C@N), cmÀ1. Elem. Anal. Calc. for
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