Synthesis, characterization and reaction of the cluster complexes containing tetrahedral core MRuCoSe.: The single crystal X-ray structures of the clusters RuCoMo(CO)8(μ3-Se)C5H4C(O)R [R = CH3, C6H4C(O)OCH3]

被引:28
|
作者
Ding, ER
Yin, YQ [1 ]
Sun, J
机构
[1] Chinese Acad Sci, Lanzhou Inst Chem Phys, State Key Lab Oxo Synth & Select Oxidat, Lanzhou 730000, Peoples R China
[2] Chinese Acad Sci, Shanghai Inst Organ Chem, Shanghai 200032, Peoples R China
关键词
transition metal; cluster complex; chiral; crystal structure;
D O I
10.1016/S0022-328X(98)00430-6
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
Several chiral cluster derivatives RuCoMo(mu(3)-Se)(CO)(8)C5H4C(O)R [R=H 2, CH3 3, C6H5 4, C6H4C(O)OCH3 5] were synthesized by the thermal reaction of the precursor (mu(3)-Se)RuCo2(CO)(9) 1 with the functionally substituted cyclopentadienyl tricarbonyl metal complex anions [Mo(CO)(3)(eta(5)-C5H4)C(O)R](-) without using benzophenone ketyl as initiator. Similarly, the reaction of the novel type of dianions Mo-(CO)(3)[(eta(5)-C5H4)C(O)C6H4C(O)(eta(5)C(5)H(4))](CO)(3)MO- With two molecules of cluster 1 gave a terephthaloyl(biscyclopentadienyl) bridged cluster complex (mu(3)-Se)RuCoMo(CO)(8)(eta(5)-C5H4)C(O)C6H4C(O)(eta(5)C(5)H(4))RuCoMo(CO)(8)(mu(3)-Se) 6. The cluster 3 reacted with NaBH4 in MeOH to give the secondary alcohol cluster RuCoMo(mu(3)-Se) (CO)(8)C5H4CH(OH)CH3 7. Cluster 3 reacted with Na2Fe(CO)(4) in THF under reflux followed by acidic treatment with 40% H3PO4 to yield the new cluster HRuFeMo(mu(3)-Se)(CO)(8)C5H4C(O)CH3 8. Cluster 3 and 5 have been solved by single-crystal X-ray diffraction. Crystal data for cluster 3: orthorhombic, space group Pbca, a = 26.387(3) Angstrom, b = 18.273(2) Angstrom, c = 15.963(2) Angstrom, V = 7696(2) Angstrom(3), Z = 16 and R = 0.023, wR = 0.027. Crystal data for cluster 5: triclinic, space group P (1) over bar, a = 8.200(2) Angstrom, b = 19.631(7) Angstrom, c = 7.997(2) Angstrom, alpha = 92.50(2)degrees, beta = 108.66(2)degrees, gamma = 88.97(2)degrees, V = 1218.5(6) Angstrom(3), Z = 2 and R = 0.054, wR = 0.077. (C) 1998 Elsevier Science S.A. All rights reserved.
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页码:157 / 164
页数:8
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