SYNTHESIS AND CRYSTAL STRUCTURE OF V ^（v）O[N（CH2Ch2O）3]

<正> Reaction of ammonium metavanadate with triethanolamine in ethanol yields the title compound (2,2' , 2"-nitrilotriethoxy)oxo-vanadium (Ⅴ ). The crystal and molecular structure has been determined crystallographically. The complex V(v) O[N(CH2CH2O)3] crystallzes in the monoclinic system, space group P21, a = 7.140(1), 6 = 7.474(2), c=8.040(2) A ,β=92. 48(2)°, V=428. 7(1) A3, Mr= 213.1, Z = 2, F(000) = 220,μ= 10. 95cm-1, Dc= 1. 65gcm-3, final R= 0. 032 and Rw = 0. 034 based on 758 independant reflections with I>2σ(I). The vanadium center is in a distorted trigonal bipyramidal environment of a quadridentate chelating ligand and a terminal oxygen atom.     

MOLECULAR AND CRYSTAL STRUCTURE OF （（C6H5）3P）2Ag（CO2H）

<正> C_37 H_31 O_2P_2Ag, Mr = 677. 47. The crystal structure belongs to mon-oclicnic system with space group Cc. Cell constants a =24. 952(2), b = 9. 179(1), c = 15. 262(1) A ,β= 116. 34 (2)°, V= 3132. 9 (3) A3, Z = 4, Dc = 1. 436g/cm3, D0 = 1. 43g/cm3.The final R achieved is 0. 052 for 5677 observed reflections, F (000) = 673. Like other silver complexes, Ag ( I ) in the center of the complex is 4-coordinat-ed. Formic acid anion also acts as a bidentate ligand in this complex beside two triph-enylphosphine groups.     

SYNTHESIS AND CRYSTAL STRUCTURE OF Nb3（Se2）6I

<正> Nb3(Se2)6I,Mr = 1353. 1, tetragonal, space group D64h-P4/mnc, a= 9. 45(1), b = 9. 45(1) , c=19. 08(3)(?), V = 1705. 6(9)(?)3, and Z = 4, Dc=5. 27g/cm3. Final R = 0. 045 and Rw = 0. 053 for 881 independent reflections with I> 3σ(I). In the structure of Nb3(Se2)6I, the Nb(Se2)4 units are almost regular rectangular antiprism, which are packed in chain forms along c axis with the I (0) atoms between these chains.     

SYNTHESIS AND STRUCTURE OF CU8S[S2P（OC2H5）2]6

<正> Cu8C24H60O12P6S13,Mt= 1651. 73,trigonal,R3,a=b = c= 12. 667(4) A,α= β=γ=111. 42(1)°.V=1441(2)A3,Z=1,Dc=1. 903g·cm-3,λ(MoKa) = 0. 71073 A ,μ(MoKa) = 35. 671cm-1, F ( 000 ) = 830, 293K. Final R = 0. 066,Rw= 0. 077 for 850 unique intensity data (I≥3σ(I)). Each unit cell of the crystal comprises of a neutral molecule of formula Cu8S(dtp)6[dtp=S2P(OEt)2],wherein the eight copper atoms are arranged at the corners of regular cube,with each dtp ligand μ4-bridged to each face of the cube and a μ8-S in the center bonded to all the eight copper atoms. Each copper atom is coordinated by four sulfur atoms in a tetrahedral configuration. The bond lengths of Cu-(μ8-S) are in the range of 2. 627(2)-2. 543(2) A ,those of Cu-S(dtp)in the range of 2. 251-2. 280A.The adjacent Cu-Cu bond lengths (2. 950(5)-3. 070(2) A) show a weak interaction between the copper atoms     

SYNTHESIS AND CRYSTAL STRUCTURE OF [C8H8NdCl（THF）2]2

<正> 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.     

[（t—BuCp）2GdCl]2的合成及晶体结构

Wayda最近报道,无水氯化稀土LnCl_3和叔丁基环戊二烯钠(t-BuCp)Na进行交换反应时,由于歧化反应得不到单取代或双取代的轻稀土氯化物衍生物,只能得到中稀土和重稀土氯化物衍生物,并且没有测得这些配合物的晶体结构。我们采用提高反应温度和延长反应时间,使交换反应进行完全,有效地避免了歧化反应的发生,成功地分离到了单取代或双取代的叔丁基环戊二烯基轻稀土氯化物。并测得(t-BuCp)_2LnCl·nTHF(Ln=Pr,n=2;Ln=Yb,n=1)     

[Tb(CH_3COO)_3(H_2O)_2]_2的合成及其结构测定

2-羟基吡啶、希土高氯酸盐和乙酸钴在乙腈中反应,制备了九配位化合物[Tb(CH_3COO)_3·2H_2O]_2该晶体为三斜晶系,P~(?)空间群,其晶胞参数为a=8.870(4)(?),b=9.247(1)(?),c=10.586(1)(?),α=65.13(1)°,β=64.43(2)°,γ=62.16(4)°,V=665.97(?)~3,Z=1,F(000)=394。测定了配合物的红外光谱。讨论了它的生成机制。     

SYNTHESIS AND CRYSTAL STRUCTURE OF [(PPh_3)_3(Cu_3S_3MoBr)O]-0. 5CH_2C1_2

<正> [(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.     

CRYSTAL STRUCTURE OF [Eu(μ-CH_3COC-O)(CH3COO)_2(H_2O)_2]_2·4H_2O

<正> C12H34O20Eu2,Mr=802.30 triclinic, space group P1, a= 8.955(2), b=9.328(1), c=10.536(2) A,α= 91.74(2),β=113.87(2),γ=118.23(2), V=681.7(2)A,Dm(flotation in CC14/ BrCH2CH2Br)=1.95,DX(Z=1) =1.954g cm-3,λ(MoKα)=0.71069 A,μ=6.41 cm-1,F(OOO)=391.92, T =. 295°K,final RF= 0.032 for 7483 observed reflections with |F0|>3a(|Fo|). The compound is isostructural with the known erbium complex,the basic unit being a centrosymmetric dimer composed of two nine-coordinate polyhedra sharing a common edge. An O atom in one or the three bidentate acetato groups about each europium atom serves as a bridge between the metal centars. The dimeric units are linked by hydrogen bonds involving both ligand and lattice water molecules to form a three-dimensional network.     

SYNTHESIS AND CRYSTAL STRUCTURES OF {Pr[(C_2H_5O)_2POO]_3}_n

The synthesis, characterization and crystal structure of rare earth coordination complex of {Pr[(C_2H_5O)_2POO]_3}_n has been studied. It is triclinic with space group P1 in a unit cell of dimensions a=11.788(5), b=12.536(3), c=10.262(2.) , α=112.21(2), β=93.01(3), γ=109.94(3)°; V=1290.9(8)~3, Z=2. As shown in Fig. 1, each Pr atom is connected with other two Pr atoms through three "O-P-O" bridging groups to form a long chain polymer. The coordination number of Pr is six. The six coordinated O atoms form an octahedron. The average bond distance of Pr-O is 2.333 A. The complex has been also studied by infrared spectroscopy and thermal analyses.     

乙二醇二甲醚三苯基氧化膦三氯合铬Cr[(CH_3OCH_2CH_2OCH_3)(OPPh_3)Cl_3]的合成和晶体结构

标题配合物由Cr(CO)_6和PPh_3在50ml乙二醇二甲醚中回流5小时后过滤,在滤液中加S_2Cl_2,静置后得配合物单晶。晶体属单斜晶系,空间群为P2_1,单胞参数a=9.062(3)(?),b=11.088(3)(?),c=12.153(3)(?),β=97.93(1)°,V=1209.4(1.8)(?)~3,Z=2。 晶体结构是采用Patterson法和差Fourier合成解出。经全矩阵最小2乘法修正,最后偏离因子R=0.046,R_w=0.054,结构中Cr各与三个氧和三个氯原子键联,Cr-O(CH_3OCH_2CH_2OCH_3)平均距离为2.091(?),Cr-O(OPPh_3)距离为2.000(?),Cr-Cl(平均)距离为2.274(?)。它们形成了八面体配位构型。     

含硫、氮Schiff碱配合物—二水二分之一二甲基亚砜醋酸四邻香草醛缩胺基硫脲合镉（Ⅱ）的合成及晶体结构

Ｘ射线单晶衍射结果表明，三核镉配合物Ｃｄ３［ＣＨ３Ｏ（Ｏ）Ｃ６Ｈ３ＣＨ＝ＮＮＨＣ（Ｓ）ＮＨ２］４·［ＣＨ３ＣＯＯ］２·１／２［ＣＨ３Ｓ（Ｏ）ＣＨ３］·２Ｈ２Ｏ为单斜晶系，空间群为Ｃ２／ｃ，ａ＝３．４２１４（４），ｂ＝１．１５８１（２），ｃ＝１．７９３２（５）ｎｍ，β＝１１９．７６（１）°，Ｖ＝６．１６８ｎｍ３，Ｍｒ＝１４２７．４３，Ｚ＝４，Ｄｃ＝１．５４ｇ／ｃｍ３，μ＝１２．４８ｃｍ（－１），Ｆ（０００）＝２８６０，最后偏离因子Ｒ＝０．０６６．     

CRYSTAL STRUCTURE OF Fe4S4[SC（CH3）3]4[（C4H9）4N]2

<正> Fe_4S_4[SC(CH_3)_3]_4[(C1H_9)_2,Mr=1193. 23,tetragonal,142d,a = 23. 272(2), c= 13. 080(5) A ,V=7084(3) A3,Z=4,DC=1. 12g·cm-3,UUUU(MoKa) = 10. 8cm-1,F(000) = 2568,R=0. 058 for 1005 observed reflections. The cluster anion contains a cubane-type Fe4S4 core compressed along the 4 axis which is crystallographically imposed. Compared to other salts with different cations ,the core is subject to slight structural distortions in different crystalline environments and crystallographic symmetry of the anion is related to that of the cation.     

CRYSTAL AND MOLECULAR STRUCTURE OF BIS(L-VALINATO)COPPER(II) MONOHYDRATE Cu[(CH_3)_2CHCH(NH_2)COO]_2·H_2O

<正> Mr=313.8, monocllnic, C2, a=21.255(4), b=9.567(4), c=7.399(1)A, β=108.8(1)°, V=1423.8A3, Z=4, Dx=1.464 g.cm-3, MoKα , μ=15.496cm-1 , F(OOO) = 660, T=295K, final R=0.089 for 1644 observed reflections. Two amino acid ligands chelate to copper forming a planar-square configuration. An oxygen atom of water occupying the apical position makes the coordinating polyhedron of copper a square pyramid.