<p>This study aims to explore the synthesis and structural characterization of nickel dithiolato complexes derived from thiolato ligands and phosphine co-ligands, with a focus on understanding their formation pathways and geometrical features. Treatment of nickel(II) chloride with thiolato anions afforded the known hexakis[di(alkylthiolato)nickel [Ni(SR)<sub>2</sub>]<sub>6</sub>, where R = CH<sub>2</sub>Ph (<b>1</b>) or CH<sub>2</sub>CH<sub>2</sub>Ph (<b>2</b>). Cluster <b>1</b> reacts with bis(diphenylphosphino)alkane ligands {dppa = bis(diphenylphosphino)ethane (dppe) and bis(diphenylphosphino)propane (dppp)} to yield the corresponding mononuclear nickel dithiolato complexes, (dppe)Ni(SCH<sub>2</sub>Ph)<sub>2</sub> (<b>3</b>a) and (dppp)Ni(SCH<sub>2</sub>Ph)<sub>2</sub> (<b>3b</b>). Alternatively, complexes <b>3a</b> and <b>3b</b> can also be synthesized directly by the reaction of (dppe/dppp)NiCl₂ with lithium thiolates (RSLi). Complexes <b>3</b> were characterized by a combination of spectroscopic techniques, including UV–Vis, IR, and multinuclear NMR (<sup>1</sup>H, <sup>31</sup>P{<sup>1</sup>H}), in addition to elemental analysis. Single-crystal X-ray diffraction studies of complexes <b>2</b> and <b>3a</b> are presented.</p>

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Synthesis, and characterization of square planar nickel dithiolates

  • Mohammad El-khateeb,
  • Phil Köhler,
  • Wolfgang Weigand

摘要

This study aims to explore the synthesis and structural characterization of nickel dithiolato complexes derived from thiolato ligands and phosphine co-ligands, with a focus on understanding their formation pathways and geometrical features. Treatment of nickel(II) chloride with thiolato anions afforded the known hexakis[di(alkylthiolato)nickel [Ni(SR)2]6, where R = CH2Ph (1) or CH2CH2Ph (2). Cluster 1 reacts with bis(diphenylphosphino)alkane ligands {dppa = bis(diphenylphosphino)ethane (dppe) and bis(diphenylphosphino)propane (dppp)} to yield the corresponding mononuclear nickel dithiolato complexes, (dppe)Ni(SCH2Ph)2 (3a) and (dppp)Ni(SCH2Ph)2 (3b). Alternatively, complexes 3a and 3b can also be synthesized directly by the reaction of (dppe/dppp)NiCl₂ with lithium thiolates (RSLi). Complexes 3 were characterized by a combination of spectroscopic techniques, including UV–Vis, IR, and multinuclear NMR (1H, 31P{1H}), in addition to elemental analysis. Single-crystal X-ray diffraction studies of complexes 2 and 3a are presented.