Preparation and crystal structure of [μ-Ni(C5H5)P(C6H5)3] [μ-C5H5] [ZnC5H5]2, a nickel-bridged cyclopentadienylzinc dimer

[μ-Ni(C₅H₅)P(C₆H₅)₃] [μ-C₅H₅]₂ [ZnC₅H₅]₂ has been obtained from the reaction of Cp₂Zn with Ni(COD)₂ in the presence of Ph₃P and its structure determined by X-ray crystallography. It consists of two cyclopentadienylzinc moieties bridged by the Ni atom of a CpNiPPh₃ group and by a Cp group. A possible mechanism for the formation of the compound is discussed.     

Hydrothermal synthesis, crystal structure, and photoluminescence of a new 2D cadmium(II) complex: {Cd(C8H5O3Cl2)2(C10H8N2)} n

One new cadmium coordination polymer, [Cd(2,4-Dcp)₂(4,4-Bipy)] _n (I) (2,4-HDcp = 2,4-dichlorophenoxyacetic acid, 4,4′-Bipy = 4,4′-bipyridine) with 2D layer structure, has been prepared by the hydrothermal synthesis and characterized by elemental analysis, IR, TGA and single-crystal X-ray diffraction. Complex I crystallizes belong to monoclinic system and has C2/c space group. Each Cd²⁺ ion is six-coordinated and located at an octahedral geometry. The Cd²⁺ ions are linked by bidentate 2,4-Dcp groups into a linear chain in which the benzene rings of 2,4-Dcp ligands point alternately up and down. These chains are further connected into a sandwich-like layer though 4,4′-Bipy ligands. Furthermore, the photoluminescence and life-time of I in the solid state have been studied.     

Hydrothermal synthesis and crystal structure of a layered coordination polymer: [Zn2(C2O4)2(C3N2H4)2] n

A new metal-organic coordination polymer [Zn₂(C₂O₄)₂(C₃N₂H₄)₂] _n (1) has been hydrothermally synthesized with ZnCl₂·2H₂O, oxalic acid and imidazole. The compound has a 2D network, consisting of infinite zinc(II) oxalate chains connected to each other by three-coordinate oxygen atoms. Within the chains, the zinc atoms are each octahedrally coordinated by one nitrogen atom from imidazole and five oxygen atoms from oxalate groups. Furthermore, there are two coordination modes of oxalate to zinc ions: chelate bis-bidentate and chelate/bridging bis-bidentate in compound 1, and the latter is rare among related compounds. Crystal data: monoclinic, P2(1)/c, a?=?8.4310(17), b?=?9.4060(19), c?=?8.2790(17)?Å, β?=?93.15(3)°, V?=?655.5(2)?ų, Z?=?2, R ₁?=?0.0322, wR ₂?=?0.0850.     

Hydrothermal Synthesis and Structure of [Mn(C8H5NO4)·H2O]n·2nH2O

A novel 5-aminoisophthalate compound, [Mn(C8H5NO4)(H2O]n(2nH2O 1, has been synthesized by the hydrothermal assembly of 5-aminoisophthalic acid with manganese acetate. Ele- mental analysis, X-ray crystal structure analyses, IR spectra, FT-Raman and ESR were carried out for the structural determination and characterization of the title compound. Compound 1 crystallizes in triclinic, space group Pī with a = 7.7562(2), b = 8.6121(3), c = 8.7107(2)(A), α = 85.411(2), β = 76.030(2), γ = 66.510(2)o, V = 517.76(3)(A)3, MnC8H11NO7, Mr = 288.12, Z = 2, Dc = 1.848 g/cm3, μ = 1.300 mm-1, F(000) = 294, R = 0.0381 and wR = 0.1043 for 1652 observed reflections (I > 2σ(I)).     

Electroswitchable photoluminescence activity: synthesis, spectroscopy, electrochemistry, photophysics, and X-ray crystal and electronic structures of [Re(bpy)(CO)3(C[triple bond]C[bond]C6H4[bond]C[triple bond]C)Fe(C5Me5)(dppe)][PF6](n) (n = 0, 1)

A novel heterobimetallic alkynyl-bridged complex, [Re(bpy)(CO)(3)(C[triple bond]C[bond]C(6)H(4)[bond]C[triple bond]C)Fe(C(5)Me(5))(dppe)], 1, and its oxidized species, [Re(bpy)(CO)(3)(C[triple bond]C[bond]C(6)H(4)[bond]C[triple bond]C)Fe(C(5)Me(5))(dppe)][PF(6)], 2, have been synthesized and their X-ray crystal structures determined. A related vinylidene complex, [Re(bpy)(CO)(3)(C[triple bond]C[bond]C(6)H(4)[bond](H)C[double bond]C)Fe(C(5)Me(5))(dppe)][PF(6)], 3, has also been synthesized and characterized. The cyclic voltammogram of 1 shows a quasireversible reduction couple at -1.49 V (vs SCE), a fully reversible oxidation at -0.19 V, and a quasireversible oxidation at +0.88 V. In accord with the electrochemical results, density-functional theory calculations on the hydrogen-substituted model complex Re(bpy)(CO)(3)(C[triple bond]C[bond]C(6)H(4)[bond]C[triple bond]C)Fe(C(5)H(5))(dHpe) (Cp = C(5)H(5), dHpe = H(2)P[bond](CH(2))(2)[bond]PH(2)) (1-H) show that the LUMO is mainly bipyridine ligand pi* in character while the HOMO is largely iron(II) d orbital in character. The electronic absorption spectrum of 1 shows low-energy absorption at 390 nm with a 420 nm shoulder in CH(2)Cl(2), while that of 2 exhibits less intense low-energy bands at 432 and 474 nm and additional low-energy bands in the NIR at ca. 830, 1389, and 1773 nm. Unlike the related luminescent rhenium(I)-alkynyl complex [Re(bpy)(CO)(3)(C[triple bond]C[bond]C(6)H(4)[bond]C[triple bond]C[bond]H)], 4, complex 1 is found to be nonemissive, and such a phenomenon is attributed to an intramolecular quenching of the emissive d pi(Re) --> pi*(bpy) (3)MLCT state by the low-lying MLCT and LF excited states of the iron moiety. Interestingly, switching on of the luminescence property derived from the d pi(Re) --> pi*(bpy) (3)MLCT state can be demonstrated in the oxidized species 2 and the related vinylidene analogue 3 due to the absence of the quenching pathway.     

有机杂化硼酸盐[Ni(dien)_2][B_5O_6(OH)_4]_2的水热合成及晶体结构

硼酸盐不仅结构丰富,而且在矿物学、催化、非线性光学材料、激光材料、隔热隔声材料等方面具有重要的应用, 从而促使人们在研究与探索硼酸盐晶体材料方面作了大量工作,制备出许多性能优良的晶体材料.     

Synthesis and crystal structure of a three-dimensional network coordination polymer: [Pb(C5H4NCOO)2(H2O)] n

A new coordination polymer [Pb(C₅H₄NCOO)₂(H₂O)] _n has been prepared by reaction of Pb(NO₃)₂ with isonicotinic acid in the presence of equimolar NaOH. Single-crystal X-ray diffraction analysis reveals that the coordination geometry of each lead(II) centre in [Pb(C₅H₄NCOO)₂(H₂O)] _n is a distorted square antiprism comprised of five O atoms and one N atom from three distinct isonicotinate ligands, and two water molecules. The complex displays a three-dimensional network structure, in which isonicotinate ligands adopt two different bridging coordination modes.     

一个新的二维配位聚合物:{Cu_2[C_(10)H_8Cl_2NO_4]_2[C_(10)H_8N_2]_3}_n的合成及其晶体结构

采用铜(Ⅱ)盐和3,5-二氯水杨醛缩丝氨酸以及4,4′-联吡啶在乙醇水溶液中合成了具有二维层状的配位聚合物.通过元素分析、红外光谱对该配位聚合物进行了表征,并利用X射线单晶衍射仪对其结构进行了鉴定.晶体结构表明,该标题配合物属三斜方晶系,空间群C2/c,晶胞参数为a=2.711(3)nm,b=2.711(3)nm,c=4.977(5)nm;α=90.00°,β=90.00°,γ=120.00°,V=3.167 8 nm3,Z=18,Dc=1.173 g.cm-3,F(000)=11 448,μ=0.807 mm-1,R1=0.078 8,wR2=0.187 2.     

[Cu(en)_2]V_6O_(14)晶体的水热合成、晶体结构和电化学性质

通过水热方法合成了一种三维无机-有机多金属钒酸盐[Cu(en)_2]V_6O_(14),并测定了其晶体结构.该化合物经过X-射线单晶衍射、元素分析、红外光谱表征和热失重分析,并研究了它的电化学性质.     

一维链状配位聚合物[Nd(C8H7NO2)3(H2O)]n的水热合成和晶体结构

利用Nd(NO)36H2O和3-(3-吡啶基)丙烯酸在水热反应条件下反应,合成了一种新型一维链状配位聚合物[Nd(C8H7NO2)3(H2O)]n。用元素分析、IR和TGA-DTA进行了表征, 并用X-射线衍射法测定了晶体结构。结果表明,该晶体属三斜晶系,(分子式C24H23N3O7Nd),P空间群,晶胞参数为a = 6.275(2),b = 12.757(4), c = 15.714(5) 牛琣 = 111.966(5), b = 90.338(6),g = 94.960(6),V = 1161.2(7) ?,Z = 2,Dc = 1.735 g/cm3,m = 2.286 mm-1,Mr = 606.67, F(000) = 602,R = 0.0355, wR = 0.0757。通过3-(3-吡啶基)丙烯酸配体羧基氧原子桥联形成一维链状结构,同时链与链通过氢键及-相互作用形成了三维的网络结构。     

(C5H7N2)3(AsMo12O40)·3C5H6N2·2H2O的水热合成、晶体结构及催化性能

采用水热法合成了一种新的3-氨基吡啶砷钼多金属氧酸盐配合物(C5H7N2)3(AsMo12O40)·3C5H6N2·2H2O。 通过单晶X射线衍射、红外光谱、紫外光谱和差热-热重对其进行了表征。 用催化消除丙酮的反应为模式反应,测试了配合物的催化性能。 研究结果表明,标题配合物是由Keggin结构[AsMo12O40]3-杂多阴离子、[C5H7N2]+阳离子、[C5H6N2]分子和结晶水分子组成。 配合物属于单斜晶系,P21/n空间群;晶胞参数a=1.33820(12) nm,b=2.2542(2) nm,c=1.9848(2) nm,β=100.27(3)°,V=5.8912(10) nm3,Z=4,Rgt(F)=0.0590,wRref(F2)=0.1882。 配合物对催化消除丙酮具有较好的的活性,催化实验结果表明,160 ℃下,0.20 g的催化剂可将初始浓度均为1.3 g/m3,流速为4.5 mL/min的丙酮完全消除。     

The preparation and X-ray crystal structure of [Ru(SC6F52{P(C6H5)2(H4C6H-2)}2]

The complex [Ru(SC₆F₅)₂(PPh₃)₂] has been prepared from [RuCl₂(PPh₃)₃] and [Pb(SC₆F₅)₂] and shown by X-rays to have a pseudo-octahedral structure apparently with two RuHC interactions. It reacts with CO to give [Ru(SC₆F₅)₂-(CO)₂(PPh₃)₂].     

一维配位聚合物[Ni3(H2btec)1.5(OH)3(2,2'-bipy)3]n的水热合成及晶体结构

采用水热法合成了一维配位聚合物[N i3(H2btec)1.5(OH)3(2,2-’b ipy)3]n。对其进行了元素分析、红外光谱和X射线单晶衍射测定。该配合物属于单斜晶系,空间群P2(1)/c,晶胞参数a=10.9214(12),b=18.012(2),c=20.566(2),β=94.933(2),°z=4,V=4030.6(8)3,D c=1.765g/cm3,F(000)=2184,R1=0.0483,wR2=0.0972。     

Complexes of IIB Metal Halides with N,N-Diethylbenzenecarbothioamide crystal structure of [Hg{C6H5C(S)N(C2H5)2}I2]2

Complexes having the empirical formulae M(DEBCTA)₂X₂ (M = Zn or Cd, X = Br or I, DEBCTA = N,N-diethylbenzenecarbothioamide), Zn(DEBCTA)Cl₂, Cd₂(DEBCTA)Cl₄ and Hg(DEBCTA)X₂ (X = Cl, Br or I) were made by reaction of zinc, cadmium or mercury dihalides in ethanol or 1,2-dichloroethane. All complexes have been characterized by elemental analysis, conductance and molecular weight measurements and by infrared and ¹H-NMR spectral studies. In addition, the structure of [Hg(DEBCTA)I₂]₂ has been determined by single-crystal X-ray crystallography and refined to a conventional R factor of 0.097. The compound crystallizes in the monoclinic space group P2₁/n with a = 1383.9(2), b = 834.3(1), c = 1418.2(2) pm, β = 101.03(1)° and Z = 2. The molecule was found to have a dimeric structure involving two asymmetrical iodine bridges in which the Hg atom lies a tetrahedral environment and the ligands lie mutually trans with respect to one another.