Abstract
The paramagnetic compounds [Ni2(HMTA)(i-Bu2PS2)4] (I) and [Ni2(TEDA)(i-Bu2PS2)4] (II) (μeff = 3.11 and 3.23 μB, respectively) were synthesized by reacting diamagnetic Ni(i-Bu2PS2)2 with hexamethylenetetramine (HMTA) and triethylenediamine (TEDA) in ethanol. The crystal structure of I was established by single-crystal X-ray diffraction analysis (CAD4 diffractometer, MoK α radiation, 1483 F hkl, R = 0.0648). The crystals are monoclinic: a = 35.212(7) Å, b = 9.313(2) Å, c = 22.622(5) Å; β = 129.97(3)°, V = 5685(2) Å3, Z = 4, ρ(calcd) = 1.281 g/cm3, space group C2/c. The structure is built of discrete binuclear molecules. The coordination polyhedron of the Ni atom is a distorted tetragonal pyramid with four S atoms of two bidentate cyclic ligands i-Bu2PS2 – in the base and the N atom of the bidentate bridging ligand HMTA at the axial vertex. Complexes I and II have similar electronic reflection spectra, which agrees with the C 4v symmetry of the ligand field.
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Larionov, S.V., Kokina, T.E., Glinskaya, L.A. et al. Nickel(II) Diisobutyldithiophosphinate Complexes with Hexamethylenetetramine and Triethylenediamine: Synthesis and Properties. Crystal and Molecular Structure of [Ni2(C6H12N4){(i-C4H9)2PS2}4]. Russian Journal of Coordination Chemistry 28, 560–564 (2002). https://doi.org/10.1023/A:1019757629587
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DOI: https://doi.org/10.1023/A:1019757629587