CLUSTERS CONTAINING YNAMINE LIGANDS .3. SYNTHESES AND STRUCTURAL CHARACTERIZATIONS OF RE2(CO)8(MU-MEC2NME2) AND RE2(CO)7[MU-C(ME)C(NME2)C(NME2)C(ME)]

被引：23

作者：

ADAMS, RD

CHEN, G

YIN, JG

机构：

[1] Department of Chemistry, University of South Carolina, Columbia

来源：

ORGANOMETALLICS | 1991年 / 10卷 / 05期

关键词：

D O I：

10.1021/om00051a014

中图分类号：

O61 [无机化学];

学科分类号：

070301 ; 081704 ;

摘要：

The reaction of Re2(CO)8[mu-C(H) = C(H)Bu](mu-H) with MeC2NMe2 at 25-degrees-C yielded the product Re2-(CO)8(mu-MeC2NMe2) (1; 25%). Compound 1 was characterized by single-crystal X-ray diffraction analysis and was found to contain an unsymmetric bridging ynamine ligand in which the amine-substituted carbon atom is coordinated to only one metal atom. Compound 1 reacts with additional MeC2NMe2 at 68-degrees-C to yield the three isomeric products Re2(CO)7[mu-C(Me)C(NMe2)C(NMe2)C(Me)] (2; 54%), Re2(CO)7[mu-C(Me)C(NMe2)C(Me)C(NMe2)] (3; 9.5%), and Re2(CO)7[mu-C(NMe2)C(Me)C(Me)C(NMe2)] (4; 17%). Compound 2 was analyzed crystallographically and was found to contain a metallacyclic ring formed by the head-to-head coupling of two ynamine ligands. This ring is pi-bonded to a Re(CO)3 grouping. On the basis of IR, H-1 NMR, and mass spectrometry compounds 3 and 4 were proposed to have similar structures formed by the head-to-tail and tail-to-tail coupling of two ynamine ligands, respectively. Crystal data: for 1, space group P2(1)/c, a = 9.776 (2) angstrom, b = 11.315 (4) angstrom, c = 15.695 (4) angstrom, beta = 97.56 (1)-degrees, Z = 4, R = 0.034, and R(w) = 0.040 for 1800 reflections; for 2, space group Pca2(1), a = 17.668 (4) angstrom, b = 8.510 (2) angstrom, c = 14.058 (4) angstrom, Z = 4, R = 0.018, and R(w) = 0.021 for 1429 reflections.

引用

页码：1278 / 1282

页数：5

共 17 条

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