{[Gd(DMF)3(DMSO)(H2O)3](μ-CN)[Fe(CN)5]}·2H2O的合成，结构表征和磁性

A new cyano-bridged Gadolinium^Ⅲ-Iron^Ⅲ complex {[Gd(DMF)₃(DMSO)(H₂O)₃](μ-CN)[Fe(CN)₅]}·2H₂O (DMF=N,N-dimethylformamide; DMSO=dimethylsulfoxide) was synthesized by the grinding reaction method. It crysta-llizes in the triclinic, space group P1 with cell parameters: a=0.90363(2) nm, b=1.250 78(3) nm, c=1.41303(1) nm, α=93.174(1)°, β=94.406(1)°, γ=91.817(2)°, and V=1.588 87(5) nm³, D_c=1.582 g·cm^-3, Z=2, M_r=756.72, F(000)=760, μ=2.645 mm^-1. The slightly distorted square-antiprism eightfold-coordinated Gd(Ⅲ) and the approxi-mately oriented octahedrally sixfold-coordinated Fe(Ⅲ) are linked by a cyano-bridge group to construct a dinuclear compound. The {[Gd(DMF)₃(DMSO)(H₂O)₃](μ-CN)[Fe(CN)₅]} species are held together via hydrogen bonds to form a three-dimensional framework. The Gd(Ⅲ)-Fe(Ⅲ) interaction is antiferromagnetic. CCDC: 223430.     

配合物[Mn(phendione)(PDC)(H2O)2]·2H2O的合成与晶体结构

The title compound [Mn(phendione)(PDC)(H₂O)₂]·2H₂O (H₂PDC=pyridine-2，6-dicarboxylic acid) has been prepared in aqueous solution and characterized by single X-ray diffraction structure determination， elemental analysis， IR spectroscopy， and thermal analyses. The compound crystallizes in Monoclinic system， space group C2/c， a=1.017 51(11) nm， b=1.483 25(11) nm， c=1.461 21(13) nm， β=109.86(10)°， V=2.074 1(3) nm³， Z=4， F(000)=1 028， μ=0.701 mm^-1， D_c=1.609 g·cm^-3， R₁=0.028 9， wR₂=0.078 8 [I>2σ(I)]. Crystal structure reveals that complex consists of one-dimensional chain framework bridged by hydrogen bonds that formed by uncoordinated water and oxygen atom of carboxyl group in PDC^2-. Furthermore， the complexes form a three-dimensional super-molecular structure through hydrogen bonds. CCDC: 648570.     

有机-无机复合物[H2(PW12O40){Zn(C10H8N2)2(H2O)}]·1.5[Zn(C10H8N2)3]·1.75H2O的合成、结构及性能

An organic-inorganic hybrid complex, [H₂(PW₁₂O₄₀){Zn(C₁₀H₈N₂)₂(H₂O)}]·1.5[Zn(C₁₀H₈N₂)₃]·1.75H₂O has been synthesized hydrothermally and structurally characterized by X-ray crystallography. The crystal belongs to monoclinic, space grounp C2/c, with a=4.709 4(2) nm, b=1.431 77(7) nm, c=2.621 07(1) nm, β=90.125(4)°, V=17.673 4(2) nm³, Z=8, D_c=3.087 Mg·m^-3, F(000)=14 884, μ(Mo Kα)=16.327 mm^-1. The structure was refined to R₁=0.068 7 and wR₂=0.158 0 for 20 128 observed reflections with I>2σ(I). Single crystal structure shows that the title compound is constructed from [PW₁₂O₄₀]^3- cluster anion and [Zn(C₁₀H₈N₂)₂(H₂O)]²⁺ metal-organic complex cation, in which metal Zn(Ⅱ) cation are coordinately bonded to the terminal oxygen of Keggin polyanions. The title compound exhibits good catalytic activity for oxidation of benzaldehyde to benzoic acid. CCDC: 624772.     

配合物[Zn(p-ABA)2(phen)·(H2O)]·H2O的水热合成、晶体结构及热稳定性

在甲醇水混合溶剂中，以对乙酰氨基苯甲酸(p-ABA)，1，10-邻菲咯啉(phen)为配体与高氯酸锌合成了标题配合物[Zn(p-ABA)₂(phen)·(H₂O)]·H₂O。配合物(C₃₀H₂₆N₄O₈Zn，分子量为637.93)晶体属单斜晶系，空间群P2₁/c。晶体结构表明:锌原子与2个对乙酰氨基苯甲酸的2个氧原子，1个1，10-邻菲咯啉中的2个氮原子以及水分子中的氧原子配位，晶胞参数:a=1.362 77(17) nm， b=1.882 3(2) nm，c=1.252 53(16) nm;β=114.500(2)°，V=2.923 6(6) nm³，D_c=1.449 g·cm^-3，Z=4，F(000)=1 320，R₁=0.041 4，wR₂=0.087 8。形成五配位的三角双锥结构。对配合物热稳定性进行分析，结果表明，配合物在230.0 ℃以下稳定性好。     

新颖一维配位聚合物[Ni(3，5-pdc)(H2O)4]·(H2O)的合成与晶体结构

The hydrothermal reaction of 3,5-pyridinedicarboxylic acid and NiCl₂·6H₂O results in a novel coordination polymer， [Ni(3,5-pdc)(H₂O)₄]·(H₂O). The crystal structure of the compound was determined by X-ray single crystal diffraction. The crystal belongs to monoclinic system with space group P2₁/n, a=1.136 1(3)nm, b=0.709 8(2) nm, c=1.459 7(4) nm, β=107.538(4)°， V=1.122 4(6) nm³, D_c=1.858 g·cm^-1, Z=4, F(000)=648, R₁=0.0264, wR₂=0.0665. CCDC: 224880.     

一维链状配位聚合物[Cu3(TFSSB)2·(H2O)4·4H2O]n的合成和晶体结构

The title complex [Cu₃(TFSSB)₂·(H₂O)₄·4H₂O]_n (TFSSB=taurine 3-formylsalicylic schiff base) was synthesized by TFSSB and copper(Ⅱ) acetate monohydrate in ethanol solution and the crystal structure was determined by X-ray diffraction method. The crystal belongs to monoclinic system, space group P2₁ / n，with cell parameters: a=0.927 9(6) nm, b=1.173 0(2) nm, c=1.471(2) nm, β=106.96(2)°, and V=1.531(2) nm³, Z=2, D_c=1.890 g·cm^-3, μ=2.291 mm^-1, F(000)=882, R₁=0.025 9, wR₂=0.065 9. The Cu1 is five-coordinate, the Cu2 is four-coordinate. CCDC: 253298.     

配合物[Sm(o-MOBA)3(phen)·H2O]2·4H2O的合成与晶体结构

The title complex [Sm(o-MOBA)₃(phen)·H₂O]₂·4H₂O has been synthesized by the reaction of SmCl₃·6H₂O with o-methoxybenzoic acid and 1,10-phenanthroline in 1∶3∶1 molar ratio. The crystal structure was determined by X-ray single crystal diffraction. The crystal belongs to triclinic system, space group P1 with a=1.203(10) nm, b=1.293(10) nm, c=1.306(11) nm, α=64.50(10)°, β=81.93(10)°, γ=74.81(10)°. The molecular structure shows that the Sm³⁺ ion coordinates to nine atoms. The carboxylate groups are bonded to the samarium ion in three modes: monodentate, bidentate chelating, tridentate chelating-bridging. CCDC: 603740.     

桥联双核配合物[(DPC)2Co2(H2O)5]·2H2O的合成与晶体结构

The new complex formulated [(DPC)₂Co₂(H₂O)₅]·2H₂O (HDPC^- is pyridine-2,6-dicarboxylate) has been synthesized and the crystal structure was determined by X-ray diffraction. The crystal structure of the complex belongs to monoclinic system with space group P2₁/c, a=0.83850(10) nm, b=2.7386(4) nm, c=0.9610(2) nm, β=98.280 (10) °, V=2.1838(6) nm³, Z=4, D_c=1.746 g·cm^-3, μ=1.597 mm^-1. In the crystal the two Co²⁺ are in distorted octahedrons. The part of [Co(DPC)₂] possess an approximate D_2d symmetry, while the part of [OCo₍₂₎(OH₂)₅] has an approximate C₂ symmetry.     

［Mn2(CHZ)4(H2O)2］(PA)4·10H2O的制备和分子结构研究

本文论述了苦味酸(PA,三硝基苯酚)锰与碳酰肼(CHZ, NH₂NHCONHNH₂)反应制备目标配合物的方法及该配合物的晶体结构。该配合物的结构式为［O,O′-μ-Mn₂(CHZ)₄(H₂O₂)］(PA)₄·10H₂O。晶体属三斜晶系,P1 空间群。晶体学参数为：a=0.8269(1) nm, b=1.2812(1) nm, c=1.5915(1) nm; α=109.58(1)°, β=95.19(1)°, γ=92.76(1)°, V=1.5765(2)nm³; Z=1, Dc=1.580 g·cm^-3, μ(Mo K_α)=520 m^-1。晶体结构经全矩阵最小二乘法修正,最终偏离因子R=0.0557。该化合物为具有中心对称的双核配合物,以两个碳酰肼分子中羰基氧为桥原子将两个锰离子结合起来,与锰离子形成配位键的原子是碳酰肼分子第一、五氮原子,羰基氧原子和水分子中的氧原子,锰离子的配位数为七。若味酸根作为外界离子以库伦力和氢键与内界离子结合成配合物分子。     

一维交替链状稀土配位聚合物[Er(dpa)(pya)(H2O)]n和[Nd2(pya)6(H2O)4]n的水热合成及结构表征

在水热条件下，稀土氧化物与2，2′-联苯二甲酸及异烟酸反应得到了两个新颖的一维交替链状配位聚合物[Er(dpa)(pya)(H₂O)]_n和[Nd₂(pya)₆(H₂O)₄]_n(H₂dpa=2，2′-联苯二甲酸；Hpya=异烟酸)。测定了它们的晶体结构，并进行了红外光谱和元素分析等 性质的表征。晶体结构测定表明这两个化合物同属单斜晶系，并具有相同的空间群P2₁/n， 晶体学参数分别为配合物1：a= 0.8830(3) nm，b=1.058 5(3) nm，c=2.089 1(6) nm，β=98.429(4)°，D_c=1.883g·cm^-3， V=1.931 4(10) nm³，Z=4； 配合物2：a=0.968 9(4) nm，b=1.978 3(9) nm，c=1.164 2(6) nm，β=112.106(7)°，D_c=1.756 g·cm^-3，V=2.067 5(17) nm³，Z=4。     

配合物[Cu(NPA)2(Im)2(H2O)]·H2O的合成、晶体结构及电化学性质

A novel copper(II) complex [Cu(NPA)₂(Im)₂(H₂O)]·H₂O has been synthesized (NPA=N-phenylanthranilic acid and Im=imidazole) and characterized by IR, elemental analysis and X-ray single crystal diffraction methods. It Crystallizes in Triclinic system, space group P1 with a=0.987 9(2) nm, b=1.075 7(3) nm, c=1.559 7(5) nm, α=104.18(10)°, β=108.14(10)°, γ=92.69(10)°, V=1.513 39(7) nm³, Z=2, D_c=1.447 g·cm^-3, F(000)=684, R₁=0.028 0, wR=0.083 1. The Cu(II) ion in the title complex is coordinated with two oxygen atoms from two N-phenylanthranilic acid in monodenate mode, two nitrogen atoms form two imidazole, and one oxygen atom from water, forming a distorted square-pyramid coordination geometry. CCDC: 638653.     

一种新颖有机-无机杂化配位聚合物[(C10H16N)2（Pb2I6）·2DMF·H2O]n的自组装合成和晶体结构(英)

A novel coordination polymer [(C₁₀H₁₆N)₂（Pb₂I₆）·2DMF·H₂O]_n (C₁₀H₁₆N=N-butyl-2-Methy-Pyridinium) was synthesized by the reaction of Pb(NO₃)₂ with C₆H₁₀NI at room temperature in DMF solvent and structurally characterized by means of X-ray single diffraction. The title compound crystallizes in triclinic system, space group P1 with a=1.1237(2) nm, b=1.25330(16) nm, c=0.808 00(12) nm, α=102.523(4)°, β=92.475(5)°, γ=95.712(10)°, V=1.102 9(3) nm³, Z=1, D_c=2.470 Mg·m^-3, F(000)=738, chemical formula C₂₆H₄₈N₄O₃Pb₂I₆ and M_r=1 640.46, μ（MoKα）=11.849 mm^-1, the final R=0.057 8 and wR=0.166 5 for 3716 observed reflections with I > 2σ(I). The title compound consists of cations ([(C₁₀H₁₆N)⁺] and anion chain(PbI₃^-),they are combined by static attracting forces in the crystal. DMF and H₂O locate between the organic and inorganic moiety. CCDC: 210812.     

二维配位聚合物[K2(5-nbdc)2Cd(Ⅱ)·imH·H2O]∞的合成和晶体结构(英)

The crystal structure of the title complex, [K₂(5-nbdc)₂Cd(Ⅱ)·imH·H₂O]_∞ (5-nbdc=5-nitro-1,3-benzenedicarbonate, imH=imidazole) has been determined by X-ray diffraction analysis. The crystal data are: tetragonal, space group P4₁, M_r=694.93 for CdC₁₉H₁₂N₄O₁₃K₂, a=1.018 6(10) nm, b=1.018 6(10) nm, c=2.436 7(5) nm; Z=4, V=2.528 2(6) nm³, F(000)=1 376, D_c=1.826 Mg·m^-3, μ=1.267 mm^-1. The title polymeric complex exhibits a two-dimensional framework, in which adjacent Cd(Ⅱ) ions are bridged by μ-O₄-5-nitro-1,3-benzenedicarbonate groups forming one-dimensional chains that are further linked by μ-O₃-5-nitro-1,3-benzenedicarbonate groups into two-dimensional anion rectangle sheets with large 32-membered rings. The strong π-π stacks of the benzene rings link these adjacent sheets into a three-dimensional van der Waals network. CCDC: 245527.     

具有二维纳米孔径结构Ni3(H2O)6(TMA)3-(TMA)23-·2H2O(TMA=均苯三甲酸)的合成、晶体结构和磁性研究

A novel coordination polymer nickel 1,3,5-benzenetricarboxylate (TMA) Ni₃(H₂O)₆(TMA)^3-(TMA)₂^3-·2H₂O with two-dimensional porous structure was synthesized and characterized. It crystallizes in the hexagonal system, space group P6₅22, with a=1.665 2(10) nm, c=2.045 4(11) nm, V=4.912(5) nm³, Z=6, D_c=1.916 g·cm^-3, μ(Mo Kα)=0.181 8 mm^-1, F(000)=2 892. The final R₁=0.066 4, wR₂=0.175 6 for 2 710 observed reflections [I>2σ(I)] out of 2 904 unique reflections . This coordination polymer reveals not only two-dimensional porous structure but also particular magnetic properties. CCDC: 274177.     

镧与β-丙氨酸配合物{[La2(β-ala)6(H2O)4](ClO4)6·H2O}n的合成及晶体结构

The complex, {[La₂(β-ala)₆(H₂O)₄](ClO₄)₆·H₂O}_n, was synthesized in aqueous solution and its crystal structure was determined by X-ray diffraction method .The crystal is triclinic with space group of .The cell pa-rameters are a=0.946(1)nm, b=1.2917(1)nm, c=2.1726(3)nm,α=76.79(1)°, β=80.85(1)°,γ=83.35(1)°, V=2.5429(5)nm³, Z=2, D_c=1.958g·cm^-3.The complex is an one-dimensional infinite chain. The coordination number of lanthanum ion is nine, forming a distorted tricapped trigonal prism.     

配合物{Mn(phen)2(H2O)[C8H11O2(COO)]}·(ClO4)·H2O的水热合成、晶体结构及热重分析

Complex {Mn(phen)₂(H₂O)[C₈H₁₁O₂(COO)]}·(ClO₄)·H₂O with bicycle[2.2.1]hept-2-en-5，6-dicarboxylic acid [C₇H₈(COOH)₂]， perchlorate manganese and 1，10-phenanthroline(phen) has been synthesized by means of hydrothermal way and characterized. It crystallizes in the triclinic space group P1， with a=1.022 08(12) nm， b=1.241 49(14) nm， c=1.354 29(15) nm， α=112.724(9)°， β=91.173(6)°， γ=101.250(3)°， V=1.545 9(3) nm³， D_c=1.553 g·cm^-3， Z=2， F(000)=744. Final R₁=0.042 2， wR₂=0.101 5. GooF=1.080， The crystal structure shows that the cadmium ion is coordinated with one oxygen atoms from one C₇H₁₀(COOH)₂ molecule， four nitrogen atoms from the two 1，10-phenanthroline， one oxygen atom from one water molecule， respectively， forming a distorted octahedral coordination geometry. The result of TG analysis shows that the title complex was stable under 200.0 ℃. CCDC: 653822.     

Syntheses, characterization, and structure determination of nine-coordinate Na[YIII(edta)(H2O)3]· 5H2O and eight-coordinate Na[YIII(cydta)(H2O)2]·5H2O complexes

Syntheses and structure determination of the Y^III complexes with ethylenediaminetetraacetic acid (H₄edta) and trans-1,2-cyclohexanediaminetetraacetic acid (H₄cydta) are reported. The crystal and molecular structures of the complexes, as well as their molecular formulas and compositions, were determined by single-crystal X-ray structure analyses, NMR, IR, thermogravimetric measurements, and elementary analyses. The crystal of the Na[Y^III(edta)(H₂O)₃]·5H₂O complex belongs to the orthorhombic crystal system and space group Fdd2. The crystal data are as follows: a = 19.355(5) Å, b = 35.431(11) Å, c = 12.122(3) Å, V = 8313(4) ų, Z = 16, M = 544.23, D_c = 1.739 g·cm⁻³, μ = 2.908 mm⁻¹ and F(000) = 4480. The final R and Rw are 0.0483 and 0.1172 for 3284 (I > 2σ(I)) unique reflections, R and Rw are 0.0678 and 0.1440 for all 8499 reflections, respectively. The Y^IIIN₂O₇ part in the [Y^III(edta)(H₂O)₃]⁻ complex anion has a pseudo-monocapped square antiprismatic nine-coordinate structure, in which the six coordinated atoms (two N and four O) from the edta ligand and three water molecules are coordinated to the central Y^III ion directly. The crystal of the Na[Y^III(cydta)(H₂O)₂]·5H₂O complex belongs to the triclinic crystal system and space group. The crystal data are as follows: a = 8.405(2) Å, b = 9.970(2) Å, c = 14.763(4) Å, α = 88.538(4)°, β = 76.193(4)°, γ = 88.100(4)°, V = 1200.6(5) Å ³, Z = 2, M = 580.31, D_c = 1.605 g·cm⁻³, μ = 2.519 mm⁻¹ and F(000) = 600. The final R and Rw are 0.0381 and 0.0911 for 4198 (I > 2σ(I)) unique reflections, R and Rw are 0.0530 and 0.1041 for all 6186 reflections, respectively. The Y^IIIN₂O₆ part in the [Y^III(cydta)(H₂O)₂]⁻ complex anion has a pseudo square antiprismatic eight-coordinate structure in which the six coordinated atoms (two N and four O) from the cydta ligand and two water molecules are coordinated to the central YIII ion directly. Original Russian Text Copyright ? 2005 by J. Wang, Y. Wang, Zh. H. Zhang, X. D. Zhang, J. Tong, X. Zh. Liu, X. Y. Liu, Y. Zhang, and Zh. J. Pan __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 46, No. 5, pp. 928–938, September–October, 2005.     

多元混配合物[Ni(NPA)2(Phen)(Ac)(H2O)]·H2O的合成、晶体结构

A Nickle(Ⅱ) complex [Ni(NPA)₂(Phen)(Ac)(H₂O)]·H₂O has been synthesized (NPA=N-phenylanthranilic acid， Phen=1，10-phenanthroline and Ac=acetate) and characterized by IR， elemental analysis and X-ray crystal structure determination. It crystallizes in triclinic system， space group P1 with a=0.891 25(2) nm， b=1.451 85(3) nm， c=1.485 54(3) nm， α=67.384(1)°， β=82.932(1)°， γ=85.168(1)°， V=1.759 50(6) nm³， Z=2， D_c=1.405 g·cm^-3， F(000)=778， R₁=0.032 3， wR=0.084 7. The crystal structure shows that the Nikcle(Ⅱ) ion is coordinated with two oxygen atoms from two N-phenylanthranilic acid，two nitrogen atoms from one 1，10-phenanthroline， two oxygen atoms from one acetate and one water respectively， forming a distorted octahedral coordination geometry. CCDC: 657265.     

一种具有一维链状结构的4f-3d双核配合物[Eu(DMSO)3(H2O)3Cr(CN)6]·H2O(DMSO=二甲亚砜)的合成、晶体结构和磁性研究(英)

A new cyano-bridged complex [Eu(DMSO)₃(H₂O)₃Cr(CN)₆]·H₂O with one-dimensional chain molecular structure was synthesized and characterized. The crystal data for the title complex: orthorhombic, P2₁2₁2₁, a=0.972 2(3) nm, b=1.489 5(4) nm, c=1.748 6(5)nm, Z=4, μ=3.171 mm^-1, final R₁=0.020 4, wR₂=0.043 4. From magnetic susceptibility measurements the complex was found to exhibit a weak ferromagnetic interaction between the Eu (Ⅲ)and Cr(Ⅲ)atoms. CCDC: 272212.     

一个新的三维配位聚合物Na[Cu2(malonate)2]·(ClO4)·(H2O)2的合成与表征(英)

通过Cu(ClO₄)₂和丙二酸在水溶液中的自组装合成了一个新的3D配位聚合物：Na[Cu₂(malonate)₂]·(ClO₄)·(H₂O)₂。X-射线结构分析表明该化合物晶体属于正交晶系Pnma空间群(a=1.256 5(3)，b=1.0594 3(2)，c=1.0755 6(14) nm，V=1.431 7(4) nm³，Z=4)。该聚合物的空间堆积在沿b轴和c轴方向分别形成大小为0.98 nm × 0.83 nm和0.40 nm × 0.40 nm的方形孔洞，在沿a轴方向形成大小为0.85 nm × 0.40 nm的砖墙形孔洞。磁性测试结果表明该化合物显示出铁磁性。导电性能测试实验表明它是一个半导体，经拟合得到其活化能为0.80 eV。