STRUCTURE OF BIS(QUINOLINE-8-OLATO)DIBUTYLTIN(IV)[Sn(C4H9)2(C9H6NO)2]

<正> INTRODUCTION. Studies of six-coordinated diorganotin(Ⅳ) compounds with octahedral geometry have been widely made, which indicate that the transor distorted trans [SnR_2] unit is common for the dialkyltin(Ⅳ) species     

STRUCTURE OF CHLORO [2-2''''-PYRIDYL)-6-MSTHYLBEHZOTHIAZOLE] PYROCATECHOLATOANTIMONY(Ⅲ)

<正> C19H14N2O2ClSSb,Mr = 491.6, space group P1, a = 5.977(1), b= 8.708(1), c = 8.962(1) X, a=93.91(1),B= 103.25(1),r=94.80(1), V = 450.6 A3, Z = 1, Do = 1.79, DC = 1.812 g.cm-3,F(000) = 242,u(MoKa)= 18.1 cm-1,R=0.024 for 2903 reflections. The Sb atom is situated in a distorted square- pyramidal ( octahedral) environment, with Sb-Cl 2.546(2), Sb-0 2.004(2)/2.038(3), and Sb-N 2.442(3)/2.526(3)A.     

双水杨醛缩乙二胺·氯·四氢呋喃合钛(Ⅲ)的合成及单晶结构研究

TiCl_3·3THF与Salen-Na_2在THF中反应得到标题化合物。在混合溶剂中培养出单晶, 用X射线衍射法测定了结构。晶体属正交晶系, 空间群为D~(16)_(2h)—P_(bnm), a=0.7458(2), b=1.4075(6), c=1.8752(2) nm, z=4, 经最小二乘法修正最后偏离因子R=0.086, R_w=0.066。探讨了用TiCl_3·3THF直接与Salen-H_2反应只能得到四价钛的稳定配合物的原因。考察了此配合物与二氧化碳及烷基铝的作用。     

钒氧配合物[VOL(C9H6NO)]·CH2Cl2的合成与晶体结构

A oxovanadium(Ⅴ) complex of [VOL(C₉H₆NO)]·CH₂Cl₂[H₂L=2-hydroxy-1-naphthaldehyde 4-methoxy-benzoylhydrazone, C₉H₆NO^-=8-hydroxyquinoline anion] has been synthesized and characterized by elemental analyses, IR and single crystal X-ray diffraction. The crystal crystallizes in triclinic system, the space group is P1, with the crystal cell parameters a=1.087 0(2) nm, b=1.107 1(2) nm, c=1.269 3(3) nm, α=67.84(3)°, β=79.26(3)°, γ=73.85(3)° and V=1.353 1(6) nm³ , M_r=614.34, R=0.0503, wR=0.1409. The V(Ⅴ) atom is six-coordinated by one O atom of oxo group, two O atoms and one N atom of the tridentate hydrazone ligand, as well as one N atom and one O atom of 8-hydroxyquinoline ligand, thus defining a distorted octahedral VO(ONO)(NO) geometry. A two-dimensional supramolecular layer structure is formed through π-π stacking interactions. CCDC: 268672.     

STRUCTURAL STUDIES OF DICHLORO-(4,7-DIPHENYLPHENANTHBOLINE)DIBUTYLTIN(Ⅳ) ETHANOL SOLVATE,[SnBu_2Cl_2(DPphen)]·C_2H_5OH

<正> C34H40N2OCl2Sn,Mr=682.3, triclinic, P1, a = 10.082(1),b= 10.932(1), c=15.666(2) A,α= 79.85(1),β=84.19(1),γ=84.92(1)°;V =1686.5 A3,Z = 2,Dc = 1.344 g.cm-3,μ(MoKα) = 9.5 cm-1, T=294(1)K. The coordination of tin is essentially octahedral, with the nitrogen atoms from bidentate ligand DPphen and cis-chlorine atoms lying in the equatorial plane and the two carbon atoms from trans-butyl groups in the axial positions. The average Sn-N distance of 2.39A happens to be in the shortest limit for this kind of complexes exhibiting antitumor activity.     

稀土元素的电分析化学研究——Ⅳ.镱-硝酸根(或亚硝酸根)-氯化铵中的极谱催化波

多价阳离子与NO₃^-或NO₂^-作用产生的灵敏的催化电流可用于微量金属离子或NO₃^-,NO₂^-的极谱测定,但对产生催化电流的机理并不十分清楚,本文讨论了Yb³⁺-NO₃^-(或NO₂^-)-NH₄Cl体系,证明有两种不同性质的电流同时存在.当[Yb³⁺]远小于[NO₃^-]或[NO₂^-]时,以平行催化电流为主;而当[Yb³⁺]远大于[NO₃^-]或[NO₂^-]时则以NO₃^-或NO₂^-的催化电还原电流为主要成分. 本文改进了原来提出的一些实验条件,使镱在直流极谱上的测定下限达5×10^-8M.     

[Yb(H2O)8][Cd3Cl9(H2O)]·6H2O

The title compound, namely octa­aqua­ytterbium(III) aqua­nona­chloro­tricadmate(II) hexa­hydrate, [Yb(H₂O)₈][Cd₃Cl₉(H₂O)]·6H₂O, was prepared by evaporation at 278 K from an aqueous solution of the ternary system YbCl₃–CdCl₂–H₂O and was characterized by elemental chemical analysis and by X‐ray powder and single‐crystal diffraction studies. The crystal structure can be viewed as being built from layers of double chains of CdCl₆ and CdCl₅(H₂O) octahedra separated by antiprismatic [Yb(H₂O)₈]³⁺ cations. The stabilization of the structure is ensured by O—H⋯O and O—H⋯Cl hydrogen bonds. A comparison with the structures of SrCd₂Cl₆·8H₂O and CeCd₄Cl₁₁·13H₂O is presented.     

Neutral tellurium rings in the coordination polymers [Ru(Te9)](InCl4)2, [Ru(Te8)]Cl2, and [Rh(Te6)]Cl3

Shiny black, air‐insensitive crystals of tellurium‐rich one‐dimensional coordination polymers were synthesized by melting a mixture of the elements with TeCl₄. The compounds [Ru(Te₉)](InCl₄)₂ and [Ru(Te₈)]Cl₂ crystallize in the monoclinic space group type C2/c, whereas [Rh(Te₆)]Cl₃ adopts the trigonal space group type R$\bar 3Shiny black, air-insensitive crystals of tellurium-rich one-dimensional coordination polymers were synthesized by melting a mixture of the elements with TeCl(4). The compounds [Ru(Te(9))](InCl(4))(2) and [Ru(Te(8))]Cl(2) crystallize in the monoclinic space group type C2/c, whereas [Rh(Te(6))]Cl(3) adopts the trigonal space group type R ?3c. In the crystal structures, linear, positively charged [M(m+) (Te(n)(±0))] (M=Ru, m=2; Rh, m=3) chains run parallel to the c axes. Each of the uncharged Te(n) molecules (n=6, 8, 9) coordinates two transition-metal atoms as a bridging bis-tridentate ligand. Because the coordinating tellurium atoms act as electron-pair donors, the 18-electron rule is fulfilled for the octahedrally coordinated transition-metal cations. Based on DFT calculations, the quantum theory of atoms in molecules (QTAIM) and the electron localizability indicator (ELI) provide insight into the principles of the polar donor bonding in these complexes. Comparison with optimized ring geometries reveals substantial tension in the coordinating tellurium molecules.     

Darstellung,Strukturen und EPR-Spektren der Rhenium(II)-Nitrosylkomplexe [Re(NO)Cl2(PPh3)(OPPh3)(OReO3)], [Re(NO)Cl2(OPPh3)2(OReO3)] und [Re(NO)Cl2(OPPh3)3](ReO4)

Synthesis, Structures, and EPR-Spectra of the Rhenium(II) Nitrosyl Complexes [Re(NO)Cl₂(PPh₃)(OPPh₃)(OReO₃)], [Re(NO)Cl₂(OPPh₃)₂(OReO₃)], and [Re(NO)Cl₂(OPPh₃)₃](ReO₄) The paramagnetic rhenium(II) nitrosyl complexes [Re(NO)Cl₂(PPh₃)(OPPh₃)(OReO₃)], [Re(NO)Cl₂(OPPh₃)₂ · (OReO₃)], and [Re(NO)Cl₂(OPPh₃)₃](ReO₄) are formed during the reaction of [ReOCl₃(PPh₃)₂] with NO gas in CH₂Cl₂/EtOH. These and two other Re^II complexes with 5 d⁵ ”︁low-spin”︁”︁-configuration can be observed during the reaction EPR spectroscopically. Crystal structure analysis shows linear coordinated NO ligands (Re–N–O-angles between 171.9 and 177.3°). Three OPPh₃ ligands are meridionally coordinated in the final product of the reaction, [Re(NO)Cl₂(OPPh₃)₃][ReO₄] (monoclinic, P2₁/c, a = 13.47(1), b = 17.56(1), c = 24.69(2) Å, β = 95.12(4)°, Z = 4). [Re(NO)Cl₂(PPh₃)(OPPh₃)(OReO₃)] (triclinic P 1, a = 10.561(6), b = 11.770(4), c = 18.483(8) Å, α = 77.29(3), β = 73.53(3), γ = 64.70(4)°, Z = 2) and [Re(NO)Cl₂ (OPPh₃)₂(OReO₃)] (monoclinic P2₁/c, a = 10.652(1), b = 31.638(4), c = 11.886(1) Å, β = 115.59(1)°), Z = 4) can be isolated at shorter reaction times besides the complexes [Re(NO)Cl₃(Ph₃P)₂], [Re(NO)Cl₃(Ph₃P) · (Ph₃PO)], and [ReCl₄(Ph₃P)₂].     

Darstellung von trans-[Mo6Cl8]Cl4Br22−ausgehend von kristallisierten [Mo6Cl8]Cl4(H2O)2 und die Kristallstruktur von [(C6H5)4As]2[Mo6Cl8]Cl4Br2

Preparation of trans-[Mo₆Cl₈]Cl₄Br₂^2? Starting from Crystalline [Mo₆Cl₈]Cl₄(H₂O)₂ and Crystal Structure of [(C₆H₅)₄As]₂[Mo₆Cl₈]Cl₄Br₂ The synthesis of the title compound is successful if the crystallized [(Mo₆Cl₈)Cl₄(H₂O)₂] containing the H₂O molecules in trans-position reacts with HBr + [(C₆H₅)₄As]Br in ethanol in a heterogeneous reaction. The X-ray structure investigation confirms the existence of discrete trans-Br-substituted cluster anions of composition [(Mo₆Cl₈)Cl₄Br₂]^2? in the crystal. The reaction in homogeneous solutions proceeds to Br-enriched compounds. [(C₆H₅)₄As]₂[(Mo₆Cl₈)Cl₄Br₂] crystallizes in the triclinic space group P¯1 with a = 11.071(2), b = 11.418(2), c = 12.813(2) Å, α = 116.10(2), β = 95.27(2) and γ = 94.41(2)° (?133°C). The crystal structure at ?133°C was determined from single crystal X-ray diffraction data (R₁ = 0.026). The [(Mo₆Cl₈)Cl₄Br₂]^2?-anions are not completely ordered but distributed statistically among the three positions which are possible within the limits of the ordered [Mo₆Cl₈]-cores (ratio 11:5:4). The frameworks of the anions consist of Mo₆ cluster units with (slightly distorted) octahedral arrangement of the metal atoms (d(Mo? Mo): 2.600(1) up to 2.614(1) Å), which are coordinated by the halogeno ligands in a square-pyramidal manner. The details of the structure will be discussed and compared with similar [(Mo₆X₈)Y₄] cluster units (X, Y ? Cl, Br).     

RAMAN STUDIES OF STRUCTURAL PHASE TRANSITION IN[n-C_(11)H_(28)NH_8]_2ZnCl_4

The perovskite type of compound [n-C_(11)H_(23)N_3]_2ZnCl_4(abr.C_(11)Zn)exhibits two solid-solid phasetransitions at T_(c1)=298.7 K and T_(c2)=360.1 K.A temperature dependence study of Raman spectra of C_(11)Znprovides the evidence of occurence of the structural phase transition related to the dynamics of thealkylammonium ions.The room temperature phase is ordered and contains the all-trans alkyl chains.Theintermediate temperature phase presents a partial conformational disorder and liquidlike state of allconformational disorder occurs at high-temperature phase.     

Cd2(Te6O13)][Cd2Cl6] and Cd7Cl8(Te7O17): novel tellurium(IV) oxide slabs and unusual cadmium chloride architectures

Initial attempts to prepare new Ln-Cd-Te-O-Cl compounds led to the isolation of two novel cadmium tellurium(IV) oxychlorides with two different types of structures, namely, [Cd(2)(Te(6)O(13))][Cd(2)Cl(6)] and Cd(7)Cl(8)(Te(7)O(17)). Both compounds feature novel polymeric tellurium(IV) oxide anions and unusual cadmium chloride substructures. The structure of [Cd(2)(Te(6)O(13))][Cd(2)Cl(6)] is composed of 1D [Cd(2)Cl(6)](2)(-) double chains and (002) [Cd(2)(Te(6)O(13))](2+) layers. The 1D Te(6)O(13)(2)(-) slab of the [Cd(2)(Te(6)O(13))](2+) layer is formed by TeO(3), TeO(4), and TeO(5) groups via corner- and edge-sharing, and it contains six- and seven-membered tellurium(IV) polyhedral rings. The structure of Cd(7)Cl(8)(Te(7)O(17)) features a 3D network with long-narrow tunnels along the b axis. The two types of structural building blocks are 1D [Te(7)O(17)](6)(-) anions and unusual corrugated [Cd(7)Cl(8)](6+) layers based on "cyclohexane-like" Cd(3)Cl(3) rings.     

新一类2,3—二氰基吡嗪除草剂的合成及其活性研究

新一类２，３－二氰基吡嗪除草剂的合成及其活性研究向纪明ａ谢周ｂ英柏宁ｂ（ａ陕西安康师专化学系，陕西．安康，７２５０００；ｂ中山大学化学系，广州，５１０２７５关键词５－芳胺基－６－氯－２，３－二氰基吡嗪除草剂合成中图分类号Ｏ６２６．４１５５位取代的２，...     

过渡金属五卤苯基有机化合物研究——V.Co(Ph_2PR)_2(C_6Cl_5)_2的ESR谱

测量了室温下粉末状Co(Ph_2PR)_2(C_6Cl_6)_2(R=n—Pr,n—Bu)配合物的ESR,求出各配合物的波谱参数和键参数,对其结构进行了讨论。钴(Ⅱ)—有机磷化合物在羰基合成反应中具有一定活性,我们用ESR方法对其结构进行研究。