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Nickel(II) complexes with thiosemicarbazide. I. Several new square planar and octahedral complexes of the type NiX2(thio)2

A. Sirota, T. Šramko, and J. Kohout

Slovak Technical University, Bratislava

 

Abstract: Several new tetragonal-planar and octahedral Ni(II) complexes with thiosemicarbazide (I) of the type NiX2(thio)2 (with X = Br, I, NCS, NO2, ClO4 + 3H2O, ClO4, and ClO3; thio = I) were described and their magnetic moments detd. NiBr2(thio)2 (II) was prepd. by adding 4.37 g. anhyd. NiBr2 to 50 ml. hot H2O under the const. mixing, followed by the addn. of 4.12 g. NaBr and 3.65 g. I. II is grey-green with μeff = 0. NiI2(thio)2 (III) was prepd. similarly from NiI2.6H2O, NaI, and I with a molar ratio of Ni:I:I- = 1:2:4. III was an olive-green powder with μeff = 0. II and III are diamagnetic. Ni(NCS)2(thio)2 (IV) was prepd. by adding 7.31 g. Ni(ClO4)2.6H2O to 40 ml. H2O, followed by the addn. of 3.05 g. NH4NCS and 3.65 g. I. The light-blue fine cryst. powder has a μeff = 3.15. Ni(NO2)2(thio)2 (V) was prepd. by dissolving 7.31 g. Ni(ClO4)2.6H2O in 25 ml. H2O, followed by the addn. of 4.14 g. NaNO2 and 3.65 g. I. The red powder had a μeff = 2.99. Ni(ClO4)2(thio)2.3H2O (VI) was prepd. by dissolving 0.02 mole Ni(ClO4)2(thio)2.6H2O in 40 ml. 96% EtOH and adding 0.04 mole I. The cryst. light-blue ppt. had a μeff = 3.15. Ni(ClO4)2(thio)2 (VIa), a grey-green modification, was prepd. by rubbing cryst. VI and drying it at 110° to 0.78 H2O. It became explosive and had a μeff = 1.21. Ni(ClO4)2(thio)2 (VIb), a red cryst. modification was prepd. by dissolving VIa in abs. EtOH and evapg. it in vacuo. It is analogous to NiSO4(thio)2 and is explosive. II, III, and VIa are sq. planar and IV, V, and VI octahedral.

Full paper in Portable Document Format: 2010a752.pdf (in Slovak)

 

Chemical Papers 20 (10) 752–762 (1966)

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