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Synthesis and Crystal Structure of ｛( P Ph_3)_2 Cl Ru( μ- Cl) Ru( P Ph_3) B_(10)H_7〔 O C H( C H_3)_2〕_3｝·0 .4( H_2O)

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Chinese Journal of Structural Chemistry 1999年第5期18卷 378-383页

作者：李雪姚海军等 researchcenterofanalysisandmeasurement FudanUniver ResearchCenterofAnalysisandMe

The title compound has been synthesized by the reaction of 〔RuCl 2(PPh 3) 3〕 and closo 〔B 10 H 10 〕 2- in (CH 3) 2CHOH solution. Crystals suitable for a single crystal X ray diffraction analysis were obtained from n pentane diffused to CH 2Cl 2 solution. The crystal {(PPh 3) 2ClRu( μ Cl)Ru(PPh 3)B 10 H 7〔OCH(CH 3) 2〕 3}·0.4(H 2O) is monoclinic , space group P2 1/n , M r= 1359.47, with a=19.434(4), b =14.340(4), c=25.865(9) , β= 95.48(3)°, V=7175(4)  3, D c =1.258 g/cm 3, Z=4, λ (Mo Kα )=0.71073, μ=6.03 cm -1 , F(000)=2784, R=0.0631, wR 2 = 0.1425, S =1.001. The title compound is a bimetallic species in which the second ruthenium center is bound to the cluster {(PPh 3)RuB 10 H 7〔OCH(CH 3) 2〕 3} via an Ru-Cl-Ru and two Ru-H-B-Ru bridges. The third isoproxy group replaces a hydrogen atom on B(10) of the cage, which indicates the activity of the cage.

关键词： crystal structure metallaborane ruthenaborane

Synthesis and Crystal Structure of〔( PPh_3)( CH_3 COS) _2 NiB_(10) H_(10)〕·0 .4( C_5 H_(12))

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Chinese Journal of Structural Chemistry 1999年第5期18卷 326-330页

作者：窦建民姚海军等 researchcenterofanalysisandmeasurement FudanUniver ResearchCenterofAnalysisandMe

The title compound 〔(PPh 3)(CH 3COS) 2NiB 10 H 10 〕·0.4(C 5H 12 ) has been synthesized by the reaction of 〔NiCl 2(PPh 3) 2〕, closo 〔B 10 H 10 〕 2- and CH 3COSH in CH 2Cl 2 solution. It was recrystallized from n pentane/CH 2Cl 2 solution and its structure was determined by X ray diffraction analysis. The crystal is triclinic, space group P1, M r= 618.23, with a=10.049(1), b=12.638(2), c=14.077(2) , α=110.13(1), β=87.65(1), γ=96.01(1)°, V=1669.3(4)  3, D c =1.230 g/cm 3, Z=2, λ (Mo Kα )=0.71073 , μ =7.76 cm -1 , F (000)=642. The final refinement is converged with R =0.042 (5986 observed reflections with I≥2σ(I)), wR 2 =0.151. The cluster is a nido eleven vertex {NiB 10 } cage with the Ni atom in the open NiB 4 face. Cyclizations resulting in two five membered rings, Ni(7)-S(1)-C(1)-O(1)-B(2) and Ni(7)-S(2)-C(2)-O(2)-B(3), have occurred.

关键词：合成晶体结构镍原子簇合物三苯基膦环化作用

Synthesis and Crystal Structure of 9-Pyridyl-1,8-dioxo-2,3,4,5,6,7-hexahydroxanthene

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Chinese Journal of Structural Chemistry 2005年第6期24卷 701-705页

作者： ZHAOQing-Jie LINHai-Xia HANNa CHENMin-Qin YANGMing-Fa DepartmentofChemistry ShanghaiUniversiryShanghai200436China researchcenterofanalysisandmeasurement FudanUniversiryShanghai200433China

9-Pyridyl-1,8-dioxo-2,3,4,5,6,7-hexahydroxanthene 3 (C18H17NO3) was prepared by the reaction of 4-pyridinecarboxaldehyde and 1,3-cyclohexanedione using Nafion-H as catalyst. The crystal and molecular structures were studied. The crystal is of orthorhombic, space group Pbcn with a = 20.369(4), b = 14.528(2), c = 9.747(17) ?, V = 2884.3(9) ?3, Dc = 1.360 g/cm3, Z = 8, F(000) = 1248 and μ(MoKα) = 0.093 mm-1. The final R = 0.0395, wR = 0.1087 for 1458 observed reflections (I > 2σ(I)), and R = 0.1032, wR = 0.1340 for all 2580 reflections. The outer rings of the xanthene groups adopt an almost ideal envelope conformation, and the heterocyclic central ring exhibits a distorted boat conformation. The pyridyl group is rotated with respect to the xanthene system by 87°.

关键词： crystal structure xathene preparation