TRIMETHYLAMINE-N-OXIDE INDUCED DISPROPORTIONATION OF RE2(CO)10 - SYNTHESIS AND X-RAY CRYSTAL-STRUCTURE OF [FAC-RE(CO)3(ONME3)3][REO4]

被引:7
作者
CHRISTIE, SD [1 ]
CLERK, MD [1 ]
ZAWOROTKO, MJ [1 ]
机构
[1] ST MARYS UNIV,DEPT CHEM,HALIFAX B3H 3C3,NS,CANADA
来源
JOURNAL OF CRYSTALLOGRAPHIC AND SPECTROSCOPIC RESEARCH | 1993年 / 23卷 / 07期
关键词
D O I
10.1007/BF01228770
中图分类号
O7 [晶体学];
学科分类号
0702 ; 070205 ; 0703 ; 080501 ;
摘要
An attempted synthesis of [Re(CO3)(mu3-OH)]4, 1, by reacting Re2(CO)10 with an excess of NMe3O in THF resulted instead in isolation of a disproportionation product, [fac-Re(CO)3(ONMe3)3][ReO4], 2. The structure of 2 was determined via X-ray crystallography: triclinic, P1BAR, a = 9.499(5), b = 9.841(2), c = 13.448(2)angstrom, alpha = 109.92(2), beta = 106.89(3), gamma = 93.15(4)-degrees, D(calc) = 2.22 g cm-3 and Z = 2. Least-squares refinement based on 1606 observed (I > 3sigma(I)) reflections gave final values of R = 0.040 and R(w) = 0.047. The cation is a distorted octahedron that exhibits several structural manifestations of steric crowding among the bulky NMe3O ligands.
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页码:591 / 594
页数:4
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