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Synthesis, Characterization, and X‐ray Crystal Structures of (Diphosphine)Ni(dmit) and (Diphosphine)Ni(dmio) (Diphosphine = dppv, dppb) Complexes
Author(s) -
Li YuLong,
Zou LiKe,
Xie Bin,
Lin Xiao,
Zhu ShaSha
Publication year - 2013
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/zaac.201300182
Subject(s) - ligand (biochemistry) , crystallography , chemistry , benzene , nuclear magnetic resonance spectroscopy , crystal structure , stereochemistry , x ray crystallography , diffraction , organic chemistry , physics , biochemistry , receptor , optics
Four complexes with the ligands dmit and dmio were synthesized. Reaction of (PhCO) 2 (dmit) and (PhCO) 2 (dmio) with MeONa afforded the intermediates 2‐thioxo‐1,3‐dithiole‐4,5‐dithiolate dianion and 2‐oxo‐1,3‐dithiole‐4,5‐dithiolate dianion, respectively. Reaction of the two dianions with (diphosphine)NiCl 2 [diphosphine = ( Z )‐1, 2‐bis(diphenylphosphanyl)ethane (dppv), 1,2‐bis(diphenylphosphanyl)benzene (dppb)] gave (dppv)Ni(dmit) ( 1 ), (dppb)Ni(dmit) ( 2 ), (dppv)Ni(dmio) ( 3 ), and (dppb)Ni(dmio) ( 4 ). This synthesis route was found to be an efficient pathway to prepare dmit and dmio ligand complexes. Complexes, 1 – 4 were fully characterized by elemental analysis and IR, 1 H NMR, 13 C NMR, and 31 P NMR spectroscopy. In addition, the molecular structures of 1 , 3 and 4 were established by X‐ray diffraction.