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synthesis and crystal structure of [(η~5-C_5H_5)_2NdCl·OC_4H_8]_2

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Science China Chemistry 1987年第11期31卷 1136-1143页

作者：金钟声刘永盛陈文启 Changchun Institute of Applied Chemistry Academia Sinica

All attempts to prepare light lanthanide dicyclopeutadienyt chloride failed,due to the disproportionation reaction. The crystal complex of [（η5-C5H5）***4H8]2 was successfully prepared by the reaction of NdCl3·2C4H8O with cyclopentadienyl sodium （molar ratio 1:1.8）in tetrahydrofuran at room temperatureThe composition of the title compound was determined by the methods of elemental analysis, infrared spectroscopy and photoelectron spectroscopy. The crystal structure of [（η5-C5H5）2NdCl·OC4H8]2 was determined from single crystal X-ray diffraction. Data were collected at-60℃ under dry nitrogen *** complex crystallizes in the monoclinic space group P21/c,with Z=2. Lattice parameters are: a=8.201（3）, b=21.589（6）,c=8.596（3）,β=109.10（3）°.The structure was solved by Patterson and Fourier techniques and refined by least-squares to a final conventional R=0.0636 for 1680 reflections. There are two Nd atoms in the dimeric unit which are bridged asymmetrically by the two

关键词： THF Nd CI C5H5 synthesis and crystal structure of

synthesis and crystal structure of [V_2(μ-S_2)_2(S_2CNEt_2)_4]·2CH_3Cl

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Chinese Journal of Chemistry 1993年第1期11卷 40-44页

作者： LEI,Xin-Jian JIANG,Fei-Long WU,Da-Xu HONG,Mao-Chun HUANG,Zhi-Ying LIU,Han-Qin Fuzhou Laboratory of Structural Chemistry and Fujian Institute of Research on the structure of Matter,Chinese Academy of Sciences,Fuzhou,Fujian 350002

[V_2(μ-S_2)_2(S_2CNEt_2)_4].2CH_3Cl was synthesized by the reaction of NaS_2CNEt_2,Li_2S and VOCl_3 at room *** data:M=1061.3,space group Pbca,with the orthorhombic parameters:a=20.123(3),b=20.485(4),c=10.911(3),V=4497.7,Z=4,D_c=1.57g/cm^3,Mo Kσ radiation(λ=0.71069()?),μ=13.2 cm^(-1),F(000)=*** R=0.041 and R_w=0.047 for 2288 ob- served reflections with I>3σ(1).The coordination sphere of each V atom in title compound is a dis- torted tetragonal prism composed of two bidentate dithiocarbamate and two S_(2^((2-)) *** V—V distance is 2.890 while the V—S distances fall in the range of 2.422—2.505.

关键词： synthesis and crystal structure of S2 S2CNEt2 V2 CH Cl

synthesis and crystal structure of {C(η~5-C_5H_5)_4Nd_4(μ_4-O) (μ_2-Cl)_8)]·[Li(dme)_2THF]_2

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Chinese Journal of Structural Chemistry 1991年第1期10卷 60-66页

作者：李详高刘静芝等 ChangchunInstituteofAppliedChemistry AcademiaSinic ChangchunInstituteofAppliedCh

The reaction of （η5-C5H5）3Nd·THF and NdCl3·2LiCl·nTHF in solution at room temperature gave rise to[（η5-C5H5）4Nd4（μ4-O）(μ2-Cl)8][Li（dme）2THF]2 （Mr = 1654.44）. crystals of the compound were obtained at about - 10℃. The intensity data were collected under nitrogen atmosphere at-60℃. The crystal belongs to the rhombic system with space group Pna21 and the unit cell parameters : a=19. 010（7）,b = 23. 231（6） ,c= 14. 180（4） A ;V = 6261. 91 （A3） , DC= 1. 67 （g/cm3）, λ（MoKa） = 0. 71069A,F（000） = 3240,μ（mm-1） = 3. 660;Z = 4. Least-squares refinement with anisotropic temperature factors for all non-hydrogen atoms led to the final R=0. 054, Rw = 0. 056. The molecule is made up of the anion group and the cation. The oxygen atom links four Nd3+together as μ4-bridge. The eight chlorine atoms form the eight chlorine-bridge bonds among four Nd3+ions. The average bond length is : Nd-O=2. 374,Nd-Cl = 2. 811,Nd-C=2. 777,Nd（a）- Nd（b） = 3. *** bond angles of Nd（a） -Nd （b）-Nd（c） fall in the range of 623°,th

关键词： Nd dme synthesis and crystal structure of C5H5 Li THF Cl

synthesis AND crystal structure OF （DIETHYLENETRIA—MINE）（ACETATE）ZINC PERCHILORATE

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Chinese Journal of Structural Chemistry 1989年第3期8卷 229-231页

作者：金祥林姜亦佳等

The preparation and molecular structure of the novel five-coordinate zinc compound CZn(C4H13N3) (C2H3O2)]ClO4(Mr= 327. 04) are described. The crystal belongs to orthorhombic space group Pn21a with a=8. 352(2) ,6=8. 642(2) ,c=17. 758 (4)A,V=1282A3,Z=4,0c=1.69gcm-3,Dm=1.70gcm-3,F(000) = 672,u(MoKa)= *** complex cation has a distorted trigonal bipyramidal geometry wifr each acetat anion C2H3O2- bridging two zinc atoms so that a chain structure along a axis is formed by the complex cations [Zn(C4H13N3)(C2H3O2)]+.

关键词： ZnO ACETATE DIETHYLENETRIA-MINE synthesis and crystal structure of ZINC PERCHLORATE

synthesis and crystal structure of [(PPh_3)_3(Cu_3S_3MoBr)O]-0. 5CH_2C1_2

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Chinese Journal of Structural Chemistry 1991年第3期10卷 209-212页

作者：林墀昌郑子山等 FuzhouLaboratoryofStructuralChemistry Fujian Depar

[(Ph3P)3 (Cu3S3MoBr)O] 0. 5CH2C12, Mr = 1308. 00, monoclinic, P21/c,a=11. 831(3),b = 28. 471(8),c=19. 232(5) A ,β= 101. 05(3)°,V = 6358 A3,Z = 4,DC=1.37 g/cm3,F(000) = 2620,μ(MoKa) = 20. 47 cm-1. Final R=0. 085 for 4271 observede reflections. The core [Cu3S3MoBr] has a distorted cubic configuration. Two dichloromethane molecules distribute statistically in a unit cell.

关键词： Cu3S3MoBr)O PPh3 synthesis and crystal structure of CH

synthesis and crystal structure of [Na （DB18C6）（CH3OH）]2W6O19 (DB18C

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Chinese Chemical Letters 1994年第1期 67-68页

作者： Xiao Mind LU Hui Ju ZHU Shun Cheng LIU (Department of Chemistry, Capital Teacler's University Beijimg 100037)(Central Laboratory, Capital Teacher's University Beijing 100037)

ＳＹＮＴＨＥＳＩＳＡＮＤＣＲＹＳＴＡＬＳＴＲＵＣＴＵＲＥＯＦ［Ｎａ（ＤＢ１８Ｃ６）(ＣＨ３ＯＨ)］２Ｗ６Ｏ１９（ＤＢ１８Ｃ６）·（ＣＨ３ＯＨ）ＸｉａｏＭｉｎｄＬＵ；ＨｕｉＪｕＺＨＵ；ＳｈｕｎＣｈｅｎｇＬＩＵ(Ｄｅｐａｒ... 详细信息

ＳＹＮＴＨＥＳＩＳＡＮＤＣＲＹＳＴＡＬＳＴＲＵＣＴＵＲＥＯＦ［Ｎａ（ＤＢ１８Ｃ６）(ＣＨ３ＯＨ)］２Ｗ６Ｏ１９（ＤＢ１８Ｃ６）·（ＣＨ３ＯＨ）ＸｉａｏＭｉｎｄＬＵ；ＨｕｉＪｕＺＨＵ；ＳｈｕｎＣｈｅｎｇＬＩＵ(ＤｅｐａｒｔｍｅｎｔｏｆＣｈｅｍ?..

关键词： DB18C6 CH3OH synthesis and crystal structure of Na OH

synthesis and crystal structure of [C_8H_8NdCl(THF)_2]_2

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Chinese Journal of Structural Chemistry 1993年第1期12卷 1-4页

作者：齐贵中林永华等 ChangchunInstituteofAppliedChemistry AcademicSinic ChangchunInstituteofAppliedCh

The title complex was prepared from the reaction of NdClLi0.3 and C8H8, its crystal structure was determined by single-crystal X-ray diffraction. It crystallizes in the monoclinic space group P21/c with cell dimensions o = 11. 819(3), 6=12.651(3), c=13. 478(3)A, β=122.99(2)°, Mr = 856. 00, Z = 2, Dc=1. 68g/cm3, F(000) = 636. 89, V = 1690. 33A3. The structure was solved by direct methods and Fourier techniques. Least squares refinement on the basis of 1842 observed reflections led to final R = 0. 038 and Rw = 0. 040. The molecule is a dimer of C3H8NdCl(THF)2 bridged by two Cl atoms with Nd -Cl bond lengths of 2. 832(2) A and 2. 917(3)A.

关键词： Nd THF synthesis and crystal structure of CI

synthesis and crystal structure of (1,7-Dimethyl-1,4,7,10-TETRAAZACYCLODODECANE)(BROMO) COPPER PERCHLO-RATE

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Chinese Journal of Structural Chemistry 1992年第5期 343-346页

作者： Jin Xiang-Lin Jiang Yi-Jia Zhang Shi-WeiInstitute of Physics Chemistry , Peking University, Beijing 100871

The crystal of complex [Cu(C10H24N4)Br]ClO4(C10H24N4 = 1, 7-dimethyl-1, 4, 7, 10-tetraazacyclododecane) belongs to orthorhombic space group Pca21 with a = 27. 545(14), b = 9.335(8), c=13. 104(9)(?), V = 3369(?)3, Z = 8, Dc=1. 740g/cm3, F(000) = 1784, μ(Mo) = 3. 827mm-1. The five-coordinated Cu (II) is in a square-pyramidal environment with Cu(Ⅱ) being 0. 57(0. 01)(?). above the plane containing the four N atoms of the macrocyclic ligand. Weak hydrogen bonds between two complex cations induce the formation of the dimers of the complex cations.

关键词： Cu BROMO COPPER PERCHLO-RATE Dimethyl-1,4,7,10-TETRAAZACYCLODODECANE synthesis and crystal structure of

synthesis and crystal structure of (C_5H_5)_2Ti(o-NHPhC_6H_4CO_2)_2

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Chinese Journal of Structural Chemistry 1992年第2期11卷 130-133页

作者：王志强吴锵金等 DalianInstituteofChemicalPhysics AcademicSinicaDa DalianInstituteofChemicalPhys

Cp2Ti(o-NHPhC6H4CO2)2, Mr = 602. 54, space group C2/c, a = 33. 77(2), b = 12. 611(6), c=14. 486(9) A ,β=103. 28(4)°,V = 6004(5) (?)3,Z = 8, Dc= 1. 33gcm-1, MoKa(λ=0. 71069(?)) radiation, μ = 3. 21cm-1, F(000) = 2512e, R = 0. 066, Rw= 0. 085 for 2511 radiations. The Ti atom in the molecule is coordinated by two C5H5 groups and two monodentate carboxyl ligands in a distorted tetrahedral geometry with the bonds in the range of Ti-C = 2. 334 - 2. 41(?) ; Ti-O = 1. 914(5) and 1. 919(5)(?);and the bond angles O-Ti-O = 91. 7(2)°; (cent-C5H5)-Ti-(cent-C5H5) = 135. 9(6)°.

关键词： Ti o-NHPhC6H4CO2 synthesis and crystal structure of C5H5 CO