Chen Xiaoyuan, Femia Frank J, Babich John W, Zubieta Jon
Department of Chemistry, Syracuse University, Syracuse, NY 13244, USA.
Inorganica Chim Acta. 2001 Apr 27;315(2):147-152. doi: 10.1016/S0020-1693(01)00302-4.
A series of rhenium(I) tricarbonyl complexes with bidentate P,O donor ligand o-(diphenylphosphino)benzaldehyde (P∩O) and its Schiff base P,N donor ligand o-[diphenylphosphino)benzylidene]analine (P∩N) have been synthesized and structurally characterized. All the complexes of the type [ReX(CO)(3)(LL)] (where LL = P∩O, P∩N) reveal a distorted octahedral structure with the three carbonyl ligands arranged in the facial fashion. Crystal data for 1, C(22)H(15)ClO(4)PRe·1/2C(6)H(14): triclinic, P1, a=8.7430(4), b=9.5767(4), c=13.9449(6) Å, α=93.651(1), β=101.265(1), γ=93.048(1); V=1140.20(9) Å(3), Z=2.2, C(22)H(15)BrO(4)Pre: monoclinic, C2/c, a=31.6800(16), b=8.8880(4), c=18.4517(9) Å, β=124.990(1); V=4256.4(4) Å(3), Z=8. 3, C(28)H(20)ClNO(3)Pre: monoclinic, C2/c, a=22.675(4), b=8.803(2), c=28.218(5) Å, β=100.192(3); V=5543.5(16) Å(3), Z=8.4, C(28)H(20)BrNO(3)Pre: monoclinic, C2/c, a=23.035(1), b=8.7561(4), c=28.269(1) Å, β=100.811(1); V=5600.4(5) Å(3), Z=8.
合成并表征了一系列含双齿P,O供体配体邻(二苯基膦基)苯甲醛(P∩O)及其席夫碱P,N供体配体邻[(二苯基膦基亚苄基)]苯胺(P∩N)的铼(I)三羰基配合物。所有[ReX(CO)₃(LL)]型配合物(其中LL = P∩O,P∩N)均呈现扭曲的八面体结构,三个羰基配体呈面式排列。配合物1,C₂₂H₁₅ClO₄PRe·1/2C₆H₁₄的晶体数据:三斜晶系,P1,a = 8.7430(4),b = 9.5767(4),c = 13.9449(6) Å,α = 93.651(1),β = 101.265(1),γ = 93.048(1);V = 1140.20(9) ų,Z = 2.2;C₂₂H₁₅BrO₄Re:单斜晶系,C2/c,a = 31.6800(16),b = 8.8880(4),c = 18.4517(9) Å,β = 124.990(1);V = 4256.4(4) ų,Z = 8;配合物3,C₂₈H₂₀ClNO₃Re:单斜晶系,C2/c,a = 22.675(4),b = 8.803(2),c = 28.218(5) Å,β = 100.192(3);V = 5543.5(16) ų,Z = 8;配合物4,C₂₈H₂₀BrNO₃Re:单斜晶系,C2/c,a = 23.035(1),b = 8.7561(4),c = 28.269(1) Å,β = 100.811(1);V = 5600.4(5) ų,Z = 8 。