Synthesis, Characterization and Crystal Structure of [Ni(S2P{O}OC6H4CH3-p)(dppv)]

被引:0
作者
Xie Bin [1 ,2 ]
Zhu Sha-Sha [3 ]
Li Yu-Long [1 ,2 ]
Zou Li-Ke [1 ,2 ]
Lin Xiao [3 ]
He Lin-Xin [1 ]
Zhang Xiu-Lan [1 ]
Xie Feng [4 ]
机构
[1] Sichuan Univ Sci & Engn, Inst Funct Mat, Zigong 643000, Peoples R China
[2] Sichuan Inst Higher Educ, Univ Key Lab Green Chem, Zigong 643000, Peoples R China
[3] Sichuan Univ Sci Engn, Coll Mat & Chem Engn, Zigong 643000, Peoples R China
[4] Neijiang Normal Univ, Coll Chem & Chem Engn, Neijiang 641100, Peoples R China
关键词
dithiophosphate; synthesis; dppv; crystal structure; CROSS-COUPLING REACTION; COMPLEXES; NICKEL; BIARYLS; CHLOROARENES; ACID;
D O I
暂无
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
O-(p-tolyl)dithiophosphato nickel complex [Ni(S2P{O}OC6H4CH3-p)(dppv)] has been synthesized by the treatment of (dppv)NiCl2 (dppv = Ph2PCH=CHPPh2) with (p-CH3C6H40)(2)P {S} SH center dot Et2NH in THF. The new complex was fully characterized by elemental analysis, IR, H-1 NMR, P-31 NMR spectroscopies and thermo-gravimetric analysis. The molecular structure of the complex was established by X-ray crystallography. The crystal crystallizes in monoclinic, space group P2(1)/c with a = 9.2739(5), b = 17.8803(8), c = 20.1879(12) angstrom, beta = 93.269(5)degrees, V = 3342.1(3) angstrom(3), Z = 4, C33H29NiO2P3S2, M-r = 673.30, D-c = 1.338 g/cm(3), F(000) = 1392 and mu(MoK alpha) = 0.877 mm(-1). The final R = 0.0578 and wR = 0.1045 for 4138 observed reflections with I>2 sigma(I) and R = 0.1050 and wR = 0.1204 for all data. The Ni centre atom adopts a NiP2S2 square-planar geometry with two phosphorus atoms from. the dppv ligand and two sulfur atoms from the O-(p-tolyl)dithiophosphate ligand. The most interesting structural feature of the title complex resides in its 1D helical chain structure constructing via intermolecular C-H center dot center dot center dot O secondary interactions along the b-axis. The adjacent helical chains running in opposite directions are connected into a 1D double-stranded helical chain and further linked into a 2D supramolecular network by weak C-H center dot center dot center dot O interaction.
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页码:1485 / 1490
页数:6
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