A New Way to Formation of Perthiocarbonate Ligand── Synthesis and Crystal Structures of [Me4N]n[Cu(CS4)]n(Ⅰ) and [Me4N]4[Cu4(CS4)4](Ⅱ)

Abstract

Abstract: The solutions of tetranuclear copper cluster anionic complexes [Me₄N]₂[Cu₄(SePh)₆] or [Me₄N]₂[Cu₄(SPh)₆] in DMFor CH₃CNreacted with CS₂ in the presence of a small amount of S. From the resulting solutions brown-black block-shaped crystals Ⅰ or brown-red block-shaped crystals Ⅱ were formed, respectively. Crystal data: (Ⅰ) orthorhombic, space group Pbca, a=1.1385(4) nm, b=16683 (4) nm, c=10921(2) nm, V=20742(9) nm³. μ=2846 mm^-1, F (000)=1136 e, D_c=1777 g/cm³, for Z=8, R=00544 for 1821 observed reflections; (Ⅱ) tetragonal, space group P42₁c, a=13952(2) nm, b=13952(2) nm, c=11350(2) nm, V=22094(6) nm³. μ=2677 mm^-1, F (000)=1136e, D_c=1671 g/cm³, for Z=8, R=00645 for 1114 observed reflections.The X-ray crystal structure determination indicated that the molecule of the complex Ⅰ consists of a polymeric anion [Cu₂(CS₄)₂]_n_2- and cations [Me₄N]⁺. In the polymeric anion, the repeated unit is a dinuclear copper complex [Cu₂(CS₄)₂]_2-, which links to four surrounding aggregations through sulfur bridges to form a two dimensional layer structure. The cations [Me₄N]⁺ locate between the layers. The molecule of complex Ⅱ consists of a tetranuclear copper cluster anion with four perthiocarbonate ligands [Cu₄(CS₄)₄]^4- and four cations [Me₄N]⁺. The four copper atoms form a tetrahedron. One of the sulfur atoms in each CS₂- 4 ligand forms the sulfur bridge with two Cu atoms while the other is coordinated to only one copper.

Key words: Perthiocarbonate, Tetranuclear copper cluster anion, Two dimensional layer polymer, Crystal structure

CLC Number:

O614.122

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TANG Ka-Luo, JIN Xiang-Lin, LONG Yao-Ling, CUI Peng, TANG You-Qi . A New Way to Formation of Perthiocarbonate Ligand── Synthesis and Crystal Structures of [Me₄N]_n[Cu(CS₄)]_n(Ⅰ) and [Me₄N]₄[Cu₄(CS₄)₄](Ⅱ)[J]. Chem. J. Chinese Universities, 2001, 22(5): 717.

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A New Way to Formation of Perthiocarbonate Ligand── Synthesis and Crystal Structures of [Me₄N]_n[Cu(CS₄)]_n(Ⅰ) and [Me₄N]₄[Cu₄(CS₄)₄](Ⅱ)

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