SYNTHESIS AND CRYSTAL-STRUCTURE OF REO2I(PME2PH)3 AND RENI2(PME2PH)3

被引:4
|
作者
SCHMID, S [1 ]
STRAHLE, J [1 ]
机构
[1] UNIV TUBINGEN,INST ANORGAN CHEM,MORGENSTELLE 18,W-7400 TUBINGEN 1,GERMANY
来源
ZEITSCHRIFT FUR KRISTALLOGRAPHIE | 1991年 / 196卷 / 1-4期
关键词
TRANS-DIOXO-IODO-TRIS(DIMETHYLPHOSPHANE)RHENIUM(V); DIIODONITRIDOTRIS(DIMETHYLPHENYLPHOSPHANE)RHENIUM(V); SYNTHESIS; CRYSTAL STRUCTURE;
D O I
10.1524/zkri.1991.196.1-4.243
中图分类号
O7 [晶体学];
学科分类号
0702 ; 070205 ; 0703 ; 080501 ;
摘要
Trans-ReO2I(PMe2Ph)3 (1) is formed by the reaction of [ORe(O2CNPh)I(PPh3)]3 or ReO2I(PPh3)2 with excess of PMe2Ph. It crystallizes in the monoclinic space group P2(1)/n with a = 944.8(4), b = 1364.4(5), c = 2175.6(5) pm, beta = 95.84(3)-degrees, Z = 4. In the trans-dioxo complex the central rhenium(V) atom is octahedrally coordinated. In the linear O = Re = O moiety the distances Re - O are 176.6(4) and 179.0(4) pm indicating double bonds. ReNI2(PMe2Ph)3 (2) is obtained from 1 and Me3SiN(Me)SiMe3 in a complex reaction. 2 forms orthorhombic crystals with the space group Pbca and a = 1681.5(7), b = 1771.7(6), c = 1912.7(9) pm, Z = 8. In the octahedral rhenium(V) complex the phosphane groups are in meridional arrangement, and the two I atoms have cis orientation. As a result of the strong trans-influence of the triply bonded nitrido ligand [Re - N = 168.4(5) pm] the two Re - I distances are different: Re-I(cis) = 274.47(5), Re - I(trans) = 295.33(6) pm.
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页码:243 / 253
页数:11
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