PROTONATION OF CHLORIDE IN OS(H)(2)CL-2(PIPR3)(2) - SYNTHESIS OF [(PIPR3)(2)H2OS(MU-CL)(3)OSH2(PIPR3)(2)]CF3SO3

被引:22
作者
KUHLMAN, R
STREIB, WE
CAULTON, KG
机构
[1] INDIANA UNIV,DEPT CHEM,BLOOMINGTON,IN 47405
[2] INDIANA UNIV,CTR MOLEC STRUCT,BLOOMINGTON,IN 47405
关键词
D O I
10.1021/ic00111a028
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
Protonation (CF3SO3H) of Os(H)(2)Cl(2)L(2) (L = (PPr3)-Pr-i) in Et(2)O or CH2Cl2 yields Os-2(H)(4)(mu-Cl)(3)L(4)(+), characterized by IR, H-1 NMR, and P-31 NMR spectroscopy elemental analysis, and X-ray diffraction. The reaction thus involves selectivity for protonation at chloride (vs H or Os) and eliminates HCl. The dimetal cation reacts with [NBu(4)]Cl to regenerate Os(H)(2)Cl(2)L(2). Crystal data (-169 degrees C) for [Os-2(H)(4)Cl-3((PPr3)-Pr-i)(4)]CF3SO3 . CH2Cl2: a = 16.859(4) Angstrom, b = 18.719(5) Angstrom, c = 18.488(5) Angstrom, beta = 113.85(1)degrees with Z = 4 in space group P2(1)/a.
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页码:1788 / 1792
页数:5
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