Hydrothermal Synthesis and Crystal Structure of a New 3-D Open-framework Zincophosphate

An open-framework zincophosphate, [C4N3H16][Zn4.5（PO4）4] 1, has been hydro- thermally synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in the tetragonal space group P4 with a = 14.512（5）, c = 8.914（3）A, V = 1877.3（11）A3, C4H16NaO16P4Zn4.50, Mr = 780 24： Z = 4, Dc = 2.761 g/cm^3,μ= 6.103 mm^-1, F（000） = 1536, T = 298（2） K, R = 0.0416 and wR = 0.0816. In the structure, ZnO4 and PO4 tetrahedra are linked to each other, forming four-membered rings which are connected variably to form two secondary building units （SBUs）. The SBUs are connected so as to generate two chains along the c axis, which are further linked together alternatively via common oxygen atoms （Zn-O-P） giving rise to 8-ring-channels in the [001] direction, and the protonated guest diethylenetriamine （DETA） molecules sit in the middle of these channels. Other characterizations are also described by elemental analysis, thermal analysis and IR and fluorescent spectra.     

Hydrothermal Synthesis and Crystal Structure of a New Hexa-cobalt-containing POM

A new compound Na3H3[Co（en）3]2[Co4（H2O）2（PW9O34）2]·11H2O 1 （en = ethylenediamine） has been synthesized under hydrothermal conditions and characterized by IR, TGA, and single-crystal X-ray diffraction analysis. Crystal data： monoclinic, space group C21c, a = 26.336（5）, b = 18.135（2）, c = 22.751（4）A, β = 123.039（7）° and Z = 4. X-ray crystallographic study on compound 1 reveals that it includes a Weakley-type sandwich polyoxoanion [Co4（H2O）2（PW9O34）2]^10-, two complex ions [Co（en）3]^2＋, three Na^＋ ions （one Na（1） and two Na（2））, and eleven crystallographic water molecules. The sandwich polyoxoanions are linked by Na2 to form 2D layers parallel to the （100） plane, and these layers are further connected by Nal along the α-axis to generate a 3D structure.     

Synthesis and Crystal Structure of a New(6,3)-Connected Ni(Ⅱ) Coordination Polymer

The coordination polymer [Ni(dpa)(bpp)]n(H2dpa = 2,4'-biphenyl-dicarboxylic acid,bpp = 1,3-di(4-pyridyl)propane) was hydrothermally prepared and characterized by single-crystal X-ray diffraction,FTIR spectra,elemental analysis and thermal analysis.The crystal is of triclinic system,space group P1 with a = 12.516(5),b = 12.943(5),c = 15.130(5) ,α = 94.331(5),β = 91.827(5),γ = 108.382(5)°,C54H44N4Ni2O8,Mr = 497.18,V = 2315.3(15) 3,Dc = 1.426 g/cm3,F(000) = 1032,μ = 0.875 cm-1,Z = 2,the final R = 0.0496 and wR = 0.1100 for 5365 reflections with Ⅰ 2σ(Ⅰ).X-ray diffraction analysis reveals that the carboxylate group of 2,4'-diphenic acids acting as bridging ligands adopts two coordination modes:bis-mondentate and bidentate chelating.The compound exhibits a two-dimensional(6,3)-connected architecture.     

Hydrothermal Synthesis and Crystal Structure of a New Sandwich—type Molybdenum Phosphate

1 INTRODUCTION The synthesis of porous and open-framework transition metal phosphates has received great in- terest due to their various compositions and topolo- gyies, as well as their useful properties such as con- trollable size- and shape-selectivity, rigid frame- works and chemical/thermal stability[1]. Of these phosphates constructed from oxometal polyhedra and PO4 tetrahedron, the most interesting is the [MoV6P4X31]n－ (X=O, OH) family with the dimen- sionalities ranging from …     

一种具有Keggin结构的固体杂多酸的合成及其晶体结构

以钨酸钠、氯化钴、醋酸钴及1,3-丙二胺为原料,利用水热合成法制备了一种具有Keggin结构的杂多酸H6[CoW12O40].2.5H2O;利用单晶X射线衍射分析了产物的晶体结构.结果表明,产物中的过渡金属Co2+离子作为中心原子与4个氧原子形成CoO4四面体;CoO4四面体被4个W3O13金属簇包围,与每个W3O13金属簇之间通过共顶点连接而形成[CoW12O40]6-阴离子;六个氢离子作为抗衡阳离子,最终形成固体杂多酸分子.     

一种多钒氧酸有机铵盐的水热合成、晶体结构及催化性质研究

本文采用水热技术合成了一种多钒氧酸盐[NH3(CH2)4NH3][H2pip]2[V10O28].6H2O(1,pip=哌嗪),并且通过元素分析、红外、热重、单晶X-射线衍射对化合物1进行了表征。化合物1为单斜晶系,空间群为P21/n,晶胞参数为a=1.229 85(10)nm,b=1.075 10(9)nm,c=1.496 71(12)nm,β=93.947 0(10)°,V=1.974 3(3)nm3,Z=2。晶体结构分析表明,化合物1是由[V10O28]6-阴离子簇、质子化的1,4-丁二胺和哌嗪阳离子以及结晶水构成。有机阳离子和结晶水通过O-H…O和N-H…O氢键相互作用将阴离子连接形成三维结构。     

Synthesis, Crystal Structure and Magnetic Properties of a New 3D Cobalt Vanadate

A new cobalt vanadate compound 1 [Co^Ⅱ(H2O)2V2^VO6] has been hydrothermally synthesized and characterized by the elemental analyses and the single crystal X-ray diffraction analysis. Compound 1 crystallizes in the orthorhombic system, space group Pinna, with a=0.55646, b=1.06900, c=1.18452 nm, and Z=4. The magnetic susceptibility of the cobalt vanadate has been measured and indicates possible antiferromagnetic coupling between adjacent cobalt (Ⅱ) (0.5432—0.5697 nm) through bond or space.     

Hydrothermal Synthesis and Crystal Structure of a New Nickel（II） Complex with 3,4-Pyridinedicarboxylic Acid and 1,4-Bis（imidazol-l-ylmethyl）-benzene Ligands

A metal-organic coordination polymer [Ni(PDB)(bix)(H2O)]n(H2PDB=3,4-pyri-dinedicarboxylic acid, bix=1,4-bis(imidazol-1-ylmethyl)-benzene) 1 has been hydrothermally synthesized and characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. Blue crystals crystallize in the triclinic system, space group P1 with a=9.1849(8), b=9.2065(9), c=12.9308(12) , α=103.3070(10), β=104.7160(10), γ=90.5900(10)o, V=1026.42(16)3 , C21H19N5NiO5 , Mr=480.12, Dc=1.553 g/cm3 , F(000)=496, Z=2, μ(MoKα)=0.991 mm1 , the final R=0.0325 and wR=0.0799 for 3561 observed reflections (I>2 (I)). The structure of 1 exhibits a two-dimensional network structure.     

具有新结构类型的化合物Csln[PO3(OH)]2的合成与结构

水热法合成了新结构类型化合物CsIn[P03(0H)]2,并通过单晶X-射线衍射表征结构.标题化合物空间群为P121/c1(No.14),晶体学参数为:M=439.69,mP56,a=0.532 86(6)nm,b=0.91653(7)nm,c=1.478 39(14)nm,β=93.849(9).,V=0.7204(1)nm3,Z=4,Dx=4.054 g·cm-3,μ=8.713 mm-1,F(000)=800,R1= 0.0325,wR2=0.0874.在该化合物中,2个In06八面体和4个PO4四面体形成交连的六元环柱,并沿a轴方向形成近六方密堆积并连接成Cs+离子占据的十二元环结构隧道,六元环和十二元环连接构筑了三维网络结构.与类似化学计量比化合物Na2In2[PO3(0H)]4·H2O比较,标题化合物中十二元环的形成明显取决于隧道阳离子的大小,其拓扑构造可看作扩展的6,3-网格连接,化合物RbIn[PO3(0H)]2与之同构.     

具有新结构类型的化合物CsIn[PO_3(OH)]_2的合成与结构(英文)

水热法合成了新结构类型化合物CsIn[PO3(OH)]2,并通过单晶X--射线衍射表征结构。标题化合物空间群为P121/c1(No.14),晶体学参数为:Mr=439.69,mP56,a=0.53286(6)nm,b=0.91653(7)nm,c=1.47839(14)nm,β=93.849(9)°,V=0.7204(1)nm3,Z=4,Dx=4.054g·cm-3,μ=8.713mm-1,F(000)=800,R1=0.0325,wR2=0.0874。在该化合物中,2个InO6八面体和4个PO4四面体形成交连的六元环柱,并沿a轴方向形成近六方密堆积并连接成Cs 离子占据的十二元环结构隧道,六元环和十二元环连接构筑了三维网络结构。与类似化学计量比化合物Na2In2[PO3(OH)]4·H2O比较,标题化合物中十二元环的形成明显取决于隧道阳离子的大小,其拓扑构造可看作扩展的6,3-网格连接,化合物RbIn[PO3(OH)]2与之同构。     

Syntheses and Characterizations of Two New Coordination Polymers Based on Dicarboxylate and Nitrogen-contained Mixed Ligands

Two new carboxylate coordination polymers [Ni(2,3'-oba)(bib)]n] and [Mn(2,4'-oba)(bib)0.5]n(2,3'-oba = 2-(3-carboxyphenoxy)benzoic acid,2,4'-oba = 2-(4-carboxyphenoxy) ben-zoic acid and bib = 1,4-bis(2-methyl-imidazol-yl)butane) have been synthesized and characterized by elemental analysis,IR and X-ray single-crystal diffraction studies.Compound 1 crystallizes in monoclinic,space group P21/c,while compound 2 in the triclinic space group P.Compound 1 displays a one-dimensional ladder-like chain.The dinuclear paddle-wheel secondary building units(SBUs) constructed by four 2,4'-oba2-ligands in compound 2 are linked by bib into a 2D(4,4) layer structure.     

基于3，4-吡啶二羧酸的二维层状聚合物的合成和晶体结构

A metal-organic coordination polymer {[La(PDC)(N-HPDC)]·H₂O}_n (1) (H₂PDC=pyridine-3,4-dicarboxylic acid) has been hydrothermally synthesized and structurally characterized by X-ray diffraction single-crystal structure determination, elemental analyses and IR spectroscopy. The complex crystallizes in the monoclinic system, space group P2₁/c with a=1.452 8(2) nm, b=0.681 59(11) nm, c=1.464 0(2) nm, β=94.270(2)°, V=1.445 6(4) nm³, D_c=2.243 Mg·m^-3, Z=4, M_r=488.14, F(000)=944, μ(Mo Kα)=3.015 mm^-1, R=0.031 0 and wR=0.076 2 for 2 424 observed reflections (I>2σ(I)). There are La-O-C-O-C-La double chains in the complex. The chelating carboxylate O atoms and pyridyl N atoms lead the compound to 2D layers structure, which is extended to 3D supramolecular architecture through intermolecular hydrogen bonds. It is interesting that the polymer containing one-dimensional channels. CCDC: 708868.     

Hydrothermal Synthesis and Crystal Structure of a New Three-dimensional Heterometallic Coordination Polymer

A new 3d-4f heterometallic polymer {[Sm2Cu(PDC)2(SO4)2(H2O)6]·2H2O}n 1 has been synthesized by Sm2O3, Cu(SO4)2·5H2O and pyridine-3,5-dicarboxylic acid under hydrothermal conditions. The compound crystallizes in triclinic system, space group P1, with a = 6.352(7), b = 10.040(10), c = 10.315(11) , α = 94.958(14), β = 95.556(7), γ = 99.747(14)°, V = 641.7(12)3, Z = 1, Mr = 1030.63, Dc = 2.651 Mg/m3, μ = 5.615 mm-1, F(000) = 491, the final R = 0.0491 and wR = 0.1345 for 2098 observed reflections with I > 2σ(I). The compound is a three-dimensional network structure in which infinite lanthanide-carboxylate chains are linked by [Cu(SO4)2]2- metalloligands to form a mixed-metal coordination network.     

Hydrothermal Synthesis and Crystal Structure of a Three-dimensional Cadmium（II） Complex

A metal-organic coordination polymer [Cd2(PDC)2(bix)(H2O)2]n ·nH2O(H2PDC=2,4-pyridinedicarboxylic acid, bix=1,4-bis(imidazol-1-ylmethyl)-benzene) 1 has been hydrothermally synthesized and characterized by elemental analysis, IR, TG, fluorescence spectrum and single-crystal X-ray diffraction. Brown crystals crystallize in the orthorhombic system, space group P2 12 12 1 with a=11.741(3), b=14.190(4), c=18.963(5) , V=3159.4(14) 3 , C28H26Cd2N6O11, Mr=847.35, Dc=1.781 g/cm3 , F(000)=1680, Z=4, μ(MoKα)=1.415 mm 1 , the final R=0.0381 and wR=0.0882 for 5472 observed reflections (I >2σ(I)). The structure of 1 exhibits a threedimensional network structure.     

由喹喔啉类配体构筑的钴的配合物的水热合成及晶体结构

采用水热法合成了一个配合物[Co(AIP)(HAIP)2].(OH)2(HAIP=2-(9-anthryl)-1H-imidazo[4,5-f][1,10]phenanthroline)1,并对其进行了元素分析、红外光谱、热重表征和X射线单晶衍射测定。配合物1属于单斜晶系,空间群为C2/c,晶胞参数为:a=1.152 9(2),b=3.673 6(7),c=1.584 1(3)nm,α=107.73(3)°,V=6.382(2)nm3,Z=4(291(2)K)。在晶体中,中心离子Co(Ⅲ)分别与来自于2个不同的HAIP配体和1个AIP配体上的6个氮原子形成六配位的变形八面体构型。     

由喹喔啉类配体构筑的钴的配合物的水热合成及晶体结构

采用水热法合成了一个配合物[Co(AIP)(HAIP)₂]·(OH)₂(HAIP=2-(9-anthryl)-1H-imidazo[4,5-f][1,10] phenanthroline)1, 并对其进行了元素分析、红外光谱、热重表征和X射线单晶衍射测定。配合物1属于单斜晶系, 空间群为C2/c, 晶胞参数为:a=1.152 9(2), b=3.673 6(7), c=1.584 1(3) nm, α=107.73(3)°, V=6.382(2) nm³, Z=4(291(2) K)。在晶体中, 中心离子Co(Ⅲ)分别与来自于2个不同的HAIP配体和1个AIP 配体上的6个氮原子形成六配位的变形八面体构型。     

具有新结构类型的化合物CsIn[PO3(OH)]2的合成与结构(英)

水热法合成了新结构类型化合物CsIn[PO₃(OH)]₂，并通过单晶X-射线衍射表征结构。标题化合物空间群为P1 2₁/c 1 (No.14)，晶体学参数为：M_r=439.69，mP56，a=0.532 86(6) nm，b=0.916 53(7) nm，c=1.478 39(14) nm，β=93.849(9)°，V=0.720 4(1) nm³，Z=4，D_x=4.054 g·cm^-3，μ=8.713mm^-1，F(000)=800，R₁= 0.032 5，wR₂=0.087 4。在该化合物中，2个InO₆八面体和4个PO₄四面体形成交连的六元环柱，并沿a轴方向形成近六方密堆积并连接成Cs⁺离子占据的十二元环结构隧道，六元环和十二元环连接构筑了三维网络结构。与类似化学计量比化合物Na₂In₂[PO₃(OH)]₄·H₂O比较，标题化合物中十二元环的形成明显取决于隧道阳离子的大小，其拓扑构造可看作扩展的6，3-网格连接，化合物 RbIn[PO₃(OH)]₂与之同构。     

Hydrothermal Synthesis and Crystal Structure of Complex Mn2(phen)2(p-MBA)4(H2O)

A novel Mn(Ⅱ)complex Mn2(phen)2(p-MBA)4(H2O)has been hydrothermally synthesized by the reaction of P-methyl benzoic acid(p-MBA)with 1,10-phenanthroline(phen).Crystal data for this complex:monoclinic,space group C2/c,a=2.3328(3),b=1.5549(2),c=1.5557(2)nm,β=121.726(2)°,V=4.7997(11)nm3,Mr=1028.85,Dc=1.424 g/cm3,Z=4,F(000)=2128,μ(MoKa)=0.590mm-1,GOOF=1.060,R=0.0333 and wR=0.0767.In the crystal,each Mn(Ⅱ)ion is coordinated by two nitrogen atoms from one o-phenanthroline molecule.three oxygen atoms from three P-methyl benzoic acids and one oxygen atom from one water molecule,giving a six-coordinate distorted octahedral coordination geometry.Two neighboring Mn(Ⅱ)ions are bridged by two P-methyl benzoic acid groups and one water molecule,and their end positions are respectively coordinated by one 1,10-phenanthroline and one p-methyl benzoic acid molecule,giving a binuclear cage structure,of which the Mn(Ⅱ)…Mn(Ⅱ)distance is 0.3502 nm.     

Synthesis and Structural Characterization of a New 3D Lead Coordination Polymer with a Tetrazole-1-acetate Ligand

One new lead coordination polymer,[Pb(tza) 2 ] n (1,Htza=tetrazole-1-acetic acid) has been synthesized under hydrothermal conditions and characterized by elemental analysis,IR spectroscopy,thermogravimetric analysis (TGA),fluorescence spectra and single-crystal X-ray diffraction.Coordination polymer 1 is of monoclinic system,space group C2/c with a=15.4388(16),b=10.4039(11),c=8.3360(8),β=119.2070(10)°,V=1168.7(2)3,C 6 H 6 N 8 O 4 Pb,Z=4,M r=461.38,D c=2.622 g/cm 3,μ(MoKα)=14.463 mm-1,F(000)=848,the final R=0.0373 and wR=0.0904 for 2744 observed reflections with I > 2σ(I).1 is a 3D coordination framework built from Pb-carboxylate chains and the tetrazole nitrogen atoms of tza ligands.Furthermore,the luminescent property of 1 has also been investigated.