THE SYNTHESIS AND STRUCTURE OF THE IMIDAZOLATE-BRIDGED HETEROTRINUCLEAR COMPLEX (en)_2Ni[(Im)Co-(NH_3)_5]_2(CIO_4)_6·5H_2O

<正> (H2NC2H4NH2)2Ni [(C3H3N2) Co (NH3)5]2 (CIO4)6 · 5H2O,NiCo2Cl6O29N18C10H62, Mr = 1288. 00, monoclinic, C2/c, a = 31. 832(4), b = 9. 691 (1), c=15. 425(4)(?),β=90. 71(2)°, Z = 4, V = 4758. 0(?)3, Dc=1. 798g/cm3, μ (MoKa) = 15. 22cm-1, F(000)=2656. The three metal nuclei, one Ni( Ⅱ ) and two Co( Ⅲ ), bridged by two imidazolyl anions (Im = C3H3N2), form an isosceles triangle. The Ni( Ⅱ ) atom is situated on the two-fold axis and coordinated by six nitrogen atoms to form a distorted octahedron with two nitrogen atoms from two Im in cis-positions. The two Co( Ⅲ ) atoms are related by C2 symmetry and each Co( Ⅲ ) is coordinated by six nitrogen atoms to form an octahedral configuration.     

Strandberg型杂多化合物(C_6H_(11)NH_3)_5H(P_2Mo_5O_(23))4H_2O的水热合成及结构

利用水热合成法合成了分子组成为(C6H11NH3)5H(P2Mo5O23)4H2O的杂多化合物, 用单晶X-ray衍射方法测定了它的结构,该晶体属于单斜晶系,空间群P21/c, a = 12.830(3), b = 14.848(3), c = 25.258(5) ? b = 92.95(3), Mr = 1483.62, V = 4805.1(17) 3, Z = 4, Dc = 2.051 g/cm3, m = 1.431 mm-1, F(000) = 3000, I >2s(I) 的可观察衍射点4426个, 最终结构偏差因子R = 0.0464, wR = 0.0801, S = 0.731。在[P2Mo5O23]6-杂多阴离子中5个MoO6八面体通过共边和共角相连, 形成1个近似的五角平面骨架, 2个PO4四面体加在五角平面的两侧。热性质研究表明杂多阴离子骨架在547.4 ℃左右分解。     

新型磷酸钒孔道结构化合物(H3NCH2CH2NH3)3- [ (VO)4(PO4)2 (HPO4)4]的水热 合成及结构表征

以有机分子乙二胺作为模板剂合成了新型磷酸钒孔道化合物(H3NCH2CH2NH3)3^-[(VO)4(PO4)2(HPO4)4,并通过X射线单晶衍射实验进行了结构表征,晶体学数据为：C2/c,a=1.8505(9)nm,b=0.7089(4)nm,c=2.3304(10)nm,β=96.43(3)°,V-3.038(3)nm^3,Z=8,R=0.067,Rw^b=0.1635,该化合物具有非常独特和规整的二维孔道骨架结构,进一步的晶体化学研究表明该化合物为一新的VPO物相。     

新型磷酸钒孔道结构化合物(H3NCH2CH2NH3)3- [ (VO)4(PO4)2 (HPO4)4]的水热 合成及结构表征

以有机分子乙二胺作为模板剂合成了新型磷酸钒孔道化合物(H3NCH2CH2NH3)3^-[(VO)4(PO4)2(HPO4)4,并通过X射线单晶衍射实验进行了结构表征,晶体学数据为：C2/c,a=1.8505(9)nm,b=0.7089(4)nm,c=2.3304(10)nm,β=96.43(3)°,V-3.038(3)nm^3,Z=8,R=0.067,Rw^b=0.1635,该化合物具有非常独特和规整的二维孔道骨架结构,进一步的晶体化学研究表明该化合物为一新的VPO物相。     

Anderson-B-型多金属氧酸盐[Co(2,2-′bipy)_3]H-[Al(OH)_6(Mo_6O_(18))]·5H_2O的合成及晶体结构

以A lC l3.6H2O、Na2MoO4.2H2O、CoC l2.6H2O和2,2′-联吡啶为主要原料合成了Anderson-B-型多金属氧酸盐[Co(2,2-′b ipy)3]H[A l(OH)6(Mo6O18)].5H2O,进行了红外光谱、紫外光谱、差热分析和单晶结构测定。晶体学测定结果表明,化合物属于三斜晶系,Pī空间群,晶胞参数:a=1.216 0(2),b=1.221 5(2),c=1.780 0(4)nm,α=86.83(3)°,β=88.76(3)°,γ=89.82(3)°,V=2.639 4(9)nm3,Z=2,R1=0.079 4,wR2=0.176 6。化合物结构分析表明,在晶体学上,标题化合物分子是由1个[Co(2,2-′b ipy)3]2 配阳离子,1个H 离子,2个1/2[A l(OH)6(Mo6O18)]3-多阴离子和5个结晶水分子组成。多阴离子[A l(OH)6(Mo6-O18)]3-借助水分子和金属配离子通过超分子作用形成二维网状结构,网状结构之间又借助超分子作用形成三维无限伸展结构。差热分析表明,标题化合物的失重过程分为2步,多阴离子骨架破坏温度为547.5℃。     

Dawson结构 [(HOCH_2CH_2)_2NH_2]_6·P_2W_(18)O_(62)·6H_2O的合成、表征、晶体结构

由二乙醇胺与H6P2W18O62·nH2O合成了[(HOCH2CH2)2NH2]6·P2W18O62·6H2O(I).单晶结构解析结果表明晶体属三方晶系,空间群为R-3,晶胞参数:a=b=c=1.36298(16)nm,α=β=γ=106.490(17)°,Z=1,V=2.1374(4)nm3,R=0.0837,Rw=0.2219.化合物分子由一个P2W18O626 阴离子、六个质子化的二乙醇胺、六个结晶水组成.标题化合物具有可逆光色性.热分析表明,化合物阴离子在463℃左右分解.     

钴配合物[Co_2(H_2O)_8(C_(10)H_8N_2)_2]·(HO_3PCH_2CH_2SO_3)(SO_4)(H_2O)_4的合成与晶体结构研究

用硫酸钴、4,4'-联吡啶和2-磺酸基乙基膦酸合成了一个新颖的钴化合物:[Co_2(H_2O)_8(C_(10)H_8N_2)_2]·(HO_3PCH_2CH_2SO_3)(SO_4)(H_2O)_4,并对其进行了红外.元素分析、热重测试,通过单晶衍射仪测定了其晶体结构.结果表明,配合物属单斜晶系C2/c空间群,分子式为C_(22)H_(45)Co_2N_4O_(22)PS_2,分子量为930.57,晶胞参数为a=19.8456(18),b=11.2957(10),c=34.719(3)(A),β=106.095(3)°,晶胞体积为7477.9(12)(A)~3,Z=8,Dc=1.653 g/cm~3,F(000)=3856,μ=1.131 mm~(-1),最终残差因子R_1=0.0726,wR_2= 0.1719(相对于5612个I>2σ(I)的可观测衍射点).在这个化合物中,二齿配体4,4'-联吡啶把Co(II)桥连成[Co(4,4'-bipy)]~(2+)链.化合物中的[Co(4,4'-bipy)]~(2+)链有三个不同的朝向.2-磺酸基乙基膦酸没有参与配位而是做为一个有机模板剂填充在[Co(4,4'-bipy)]~(2+)链形成的空隙中.     

新型杂多蓝化合物[NH_3(CH_2)_2NH_3]_5[Cd(H_2O)][CdMo_(12)~ⅤO_(30)(HPO_4)_6(H_2PO_4)_2]·5H_2O的合成与晶体结构

利用水热法首次合成了具有两种配位环境Cd原子的新型杂多蓝化合物[NH3(CH2)2NH3]5[Cd(H2O)][CdMo12ⅤO30(HPO4)6(H2PO4)2].5H2O.通过元素分析I、CP、TG和X射线单晶衍射确定了其组成,使用IR和EPR进行了结构表征.通过N2吸附脱附测定了比表面积和孔径,为催化研究提供了基础数据.结果表明:该晶体为三斜晶系,P-1空间群;晶胞参数a=1.200 2(2)nm,b=1.465 1(3)nm,c=2.119 2(4)nm,V=3.564 2(12)nm3,β=83.01(3)°,Z=2,F(000)=293 2,R1=0.030 0,wR2=0.071 6.     

CRYSTAL STRUCTURE OF (Br(μ-Met)(μ-Gly)(H_2O)_4]_2[Er(μ-Net)_2(H_2O)_4]_2(ClO_4)_(12)

<正> [Er(u-Met)(u-Gly)(H2O)4]2[Er(u-Met)2(HaO)4]2(ClO4)12(NMet=CH3S-(CH2)2CH(NH2)COOH,Gly=NH2CH2COOH), Mr=3194, trilinic, space group P1, a = 12.375(6),b= 14.041(13), c=19.074(13)A,α=80.85(6),β=80.72(6).γ=62.82(6)° ,Z=1,V= 2896A3,Dc=1.83 g/cm3,R=0.091. The carboxyl groups of Met and Gly in the title complex are bonded to Er atoms as bidentate bridging ligands.There are two different cations located at crystallographic symmetry centers in one unit cell.     

钴的二膦酸配合物[ Co(en) 3 ] [ Co2 (Hedbbp) 2 ]· 7H2O的合成与晶体结构

水热条件下合成了一个新的有机二膦酸钴配合物[Co(en)3][Co2(Hedbbp)2].7H2O,[H4edbbp=N,N’-二(苄基膦酸)乙二胺].X射线单晶衍射结构分析表明:配合物属三斜晶系,空间群P,ī晶胞参数:a=1.505.6(3)nm,b=1.524 8(3)nm,c=1.649 7(3)nm,α=63.10(3)°,β=78.12(3)°,γ=75.62(3)°,晶胞体积为V=3.252 4(11)nm3,Z=2.配合物结构单元中包含一个二膦酸钴的二聚单元阴离子[Co2(Hedbbp)2]2-和一个三乙二胺合钴螯合阳离子单元[Co(en)3]2 和七个水分子.     

Synthesis and Characterization of [NH3（CH2）2NH2（CH2）2NH3]BiCl6

1 INTRODUCTION During the past decade, a series of organic-inor- ganic hybrid compounds based on metal halide units have been prepared and studied[1]. The combination of organic and inorganic components at the mole- cular level affords us the opportunity to design new hybrid materials and modulate the properties of components[2]. As a result, some interesting proper- ties, such as non-linear optical[3], interesting magne- tic[4], efficient luminescence[2], ideal thermal and mechanical sta…     

链状[NH3CH2CH2NH3]AgAsS4的溶剂热合成及表征

利用溶剂热方法合成了链状[NH3CH2CH2NH3]AgAsS4,通过单晶X射线衍射技术对其进行了晶体结构分析,该化合物晶体属单斜晶系,空间群C2/c,晶胞参数a=1.35805(8)nm,b=0.65331(3)nm,c=2.27711(9)nm,β=106.42(3)°,Z=8.化合物具有有趣的梯子状双链结构,该阴离子链由AsS4与AgS3共用顶点交替连接而成,有机阳离子在阴离子链之间存在较强的N—H…S氢键.DSC和Tg分析结果表明化合物在200℃以下是稳定的.     

[In2(HPO3)4]·(NH3CH2CH2NH3)的水热合成与晶体结构

用乙二胺作模板剂在水热条件下合成出一个新的三维开放骨架结构的亚磷酸铟[In2(HPO3)4]·(NH3CH2CH2NH3)(1), 并对其晶体结构进行了测定和表征.     

Zinc diphosphonates templated by organic amines: syntheses and characterizations of [NH3(CH2)2NH3]Zn(hedpH2)2*2H2O and [NH3(CH2)nNH3(CH2)nNH3]Zn2(hedpH)2*2H2O (n=4,5,6) (hedp=1-hydroxyethylidenediphophonate)

Four new zinc diphosphonate compounds with formulas [NH(3)(CH(2))(2)NH(3)]Zn(hedpH(2))(2).2H(2)O, 1, [NH(3)(CH(2))(n)()NH(3)]Zn(2)(hedpH)(2).2H(2)O, (n = 4, 2; n = 5, 3; n = 6, 4) (hedp = 1-hydroxyethylidenediphosphonate) have been synthesized under hydrothermal conditions at 110 degrees C and in the presence of alkylenediamines NH(2)(CH(2))(n)()NH(2) (n = 2, 4, 5, 6). Crystallographic data for 1: monoclinic, space group C2/c, a = 24.7422(15), b = 5.2889(2), c = 16.0338(2) A, beta = 117.903(1) degrees, V = 1856.17(18) A(3), Z = 4; 2: monoclinic, space group P2(1)/n, a = 5.4970(3), b = 12.1041(6), c = 16.2814(12) A, beta = 98.619(5) degrees, V = 1071.07(11) A(3), Z = 2; 3: monoclinic, space group P2(1)/n, a = 5.5251(2), b = 12.5968(3), c = 16.1705(5) A, beta = 99.182(1) degrees, V = 1111.02(6) A(3), Z = 2; 4: triclinic, space group P-1, a = 5.4785(2), b = 14.1940(5), c = 16.0682(6) A, alpha = 81.982(2) degrees, beta = 89.435(2) degrees, gamma = 79.679(2) degrees, V = 1217.11(8) A(3), Z = 2. In compound 1, two of the phosphonate oxygens are protonated. The metal ions are bridged by the hedpH(2)(2-) groups through three of the remaining four phosphonate oxygens, forming a one-dimensional infinite chain. The protonated ethylenediamines locate between the chains in the lattice. In compounds 2-4, only one phosphonate oxygen is protonated. Compounds 2 and 3 have a similar three-dimensional open-network structure composed of [Zn(2)(hedpH)(2)](n) double chains with strong hydrogen bonding interactions between them, thus generating channels along the [100] direction. The protonated diamines and water molecules reside in the channels. Compound 4 contains two types of [Zn(2)(hedpH)(2)](n) double chains which are held together by strong hydrogen bonds, forming a two-dimensional network. The interlayer spaces are occupied by the [NH(3)(CH(2))(6)NH(3)](2+) cations and water molecules. The significant difference between structures 2-4 is also featured by the coordination geometries of the zinc atoms. The geometries of those in 2 can be described as distorted octahedral, and those in 3 as distorted square pyramidal. In 4, two independent zinc atoms are found, each with a distorted octahedral and a tetrahedral geometry, respectively.     

Synthesis and Characterization of （CH3CH2CH2CH2NH3）2SnBr6

1 INTRODUCTION Recently, the researches on inorganic-organic hy-brid compounds represent an advanced field in mate-rial science[1]. At the molecular level, the combina-tion of two extremely different components providesan avenue to design new hybrid materials as well asthe ability to modulate properties of one or more ofthe components[2～6]. Some attractive properties, suchas efficient luminescence[2～4], ideal thermal and me-chanical stability, interesting magnetic[5], non-linearoptical[…     

Solvothermal Syntheses and Crystal Structures of Two New Nonmetal Borates: C4H10N2·B6O8(OH)2 and (NH3CH2CH2NH3)B5O8(OH)

Two new borate compounds, C4H10N2·B6O8(OH)2 1 and (NH3CH2CH2NH3)B5O8(OH)2, have been solvothermally synthesized and structurally characterized by single-crystal X-ray diffraction, IR, elemental analysis and thermal analysis. Compound 1 crystallizes in the monoclinic system, space group P21/c, with a = 8.3318(17), b = 6.2118(12), c = 12.479(3) (A), β = 108.96(3)°, V = 610.8(2) (A)3, Mr = 313.02, Z = 2, Dc= 1.702 g/cm3, μ = 0.150 mm-1, F(000) = 320, R = 0.0387and wR = 0.0924. Its layered structure is linked by infinite covalently coordinated neutral sheets with 3,20-membered window system, which are built up from alternative B6O8(OH)2 subunits donated by two piperzazine nitrogen donors. 2 crystallizes in monoclinic, space group Cc, with a =6.7207(13), b = 11.481(2), c = 12.564(3) (A),β = 95.25(3)°, V= 965.4(3) (A)3, Mr= 261.18, Z= 4, Dc=1.797 g/cm3, μ = 0.164 mm-1, F(000) = 536, R = 0.0396 and wR = 0.0752. Its oxoborate structure is generated from the sheets of 3,9-membered boron rings bonded diamine molecules through electrostatic and H-bonding interactions to form a two-dimensional layered network.     

Synthesis, Structure Characterization and Biological Activity of Layered Vanadium Oxides [ NH3 （ CH2 ）2 NH （ CH2 ）2 NH3 ] [ V6 O14 ]

Introduction Over the past decades, polyoxometalates(POMs)have been attracting extensive interestowing to the widerange of their topological properties and potential appli-cations in catalysis, photochemistry, electrochromism,and magnetism[1,2]. Meanwhile, owing to the potentialapplication of polyoxometalaes as anticancer and antivi-ral drugs, their complexes have attracted increasing in-terest of both inorganic chemists and biochemists[3]. Itis well known that polyoxometalates are excellent …     

Dawson结构α-H6P2W18O62·3(CH3)2NH·H2O的合成、表征和晶体结构

由二甲胺与H6P2W18O62·nH2O合成了电荷转移化合物α-H6P2W18O62·3(CH3)2NH·H2O.单晶结构解析结果表明晶体属单斜晶系,空间群为P21/c,晶胞参数a=1.2964(3)nm,b=1.3621(3)nm,c=4.155 9(8)nm,β=90.02(3)°,V=7.338(3)nm3,Z=4.标题化合物具有可逆光色性.热分析表明,化合物阴离子在430.5℃左右分解.     

[CH3NH3][NH3(CH2)6NH3]H3[P2Mo2W16O62]·H2O的水热合成与表征

首次合成了[CH3NH3][NH3(CH2)6NH3]H3[P2Mo2W16O62]·H2O,通过元素分析、红外光谱和X射线单晶衍射对合成产物进行了表征,并用TGA-DSC研究了化合物的热稳定性.晶体属单斜晶系,P21/m空间群,a=1.2596(3)nm,b=1.8715(4)nm,c=1.9816(4)nm,α=γ=90°,β=90.16(3)°,V=4.671(2)nm3,Z=2,Mr=4358.66,Dc=3.100g·cm-3,μ=19.978mm-1,F(000)=3792,R=0.0835,Rw=0.2026.结果表明,在晶体结构内形成了0.7364nm×0.8354nm的微孔.     

含有十二元环交叉孔道的新颖亚磷酸铟[In4(HPO3)7(H2O)3](NH3CH2CH2NH3)·(H2O)的水热合成与表征

在含有HF的体系中, 用乙二胺作模板剂, 通过水热方法合成了一个新的三维亚磷酸铟[In4(HPO3)7(H2O)3](NH3CH2CH2NH3)·(H2O), 并对其进行了红外光谱、热重、ICP和CHN元素分析等表征. 单晶X射线衍射分析结果表明, 该化合物属于三方晶系, P3空间群, 晶胞参数a=1.37883(7) nm, c=0.93450(9) nm, V=1.53862(2) nm3, Z=2, Dc=2.489 Mg/m3, 最终一致性因子R1[I >2σ(I)]=0.0526, wR2[I>2σ(I)]=0.1328, GOF=1.082. 其结构中的InO6八面体、InO5(H2O)八面体和HPO3假四面体通过O原子共顶点连接, 分别沿a, b轴方向形成含有十二元环的交叉孔道, 客体水分子和双质子化的乙二胺分子存在于孔道中.