Ni(phen)(H2O)(V2O6)的水热合成和晶体结构（英）

A novel compound Ni(phen)(H₂O)(V₂O₆) has been hydrothermally synthesized and structurally determined to be a two-dimensional compound, which contains {V₂O₆}_n^2n- chains interconnected by nickel(Ⅱ) complexes via oxygen atoms. The crystallographic data measured by single-crystal X-ray diffraction analysis are as follows: C₁₂H₁₀N₂NiO₇V₂, M_r=454.81, monoclinic, space group P2₁/c, a=0.784 6(3), b=2.103 6(8), c=0.942 3(4) nm, β=112.872(5)°, V=1.433 0(10) nm³, Z=4, D_c=2.104 Mg·m^-3, μ(Mo Kα)=2.615 mm^-1, F(000)=904, T=298(2) K, 4 480 reflections collected, 2 470 independent (R_int=0.032 2), the final R=0.058 4 and wR₂=0.145 7 for 2 303 observed reflections with I>2σ(I). CCDC: 192520.     

配合物Pb(cbba)_2(phen)_2的水热合成、晶体结构与荧光性能研究(英文)

A new metal-organic complex Pb(cbba)2(phen)2 (1, H2cbba=2-(4′-chlorine-benzoyl)benzoic acid, phen= 1,10-phenanthroline) has been hydrothermally synthesized and structurally characterized by elemental analysis, IR, fluorescence spectrum and single-crystal X-ray diffraction. The compound crystallizes in orthorhombic, space group Pbcn with a=1.474 49(7) nm, b=0.953 90(4) nm, c=3.031 65(14) nm, V=4.264 1(3) nm3, C52H32Cl2N4O6Pb, Mr=1 086.91, Dc=1.693 g·cm-3, μ(Mo Kα)=4.141 mm-1, F(000)=2 144, Z=4, the final R=0.018 3 and wR=0.045 7 for 3 582 observed reflections (I2σ(I)). In the crystal structure, the lead atom is six-coordinated with two carboxylate oxygen atoms from different cbba ligands and four nitrogen atoms from different phen ligands, showing a distorted octahedral geometry. Furthermore, 1 shows yellow photoluminescent property at room temperature.     

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.     

Hydrothermal Synthesis and Crystal Structure of a Polyoxometalate- based Complex [Cu^I（phen）2]4（SiW12O40）

A new hybrid polyoxometalate-based complex, [Cu^I（phen）214（SiW12O40） （phen = 1,10-phenanthroline）, has been synthesized by hydrothermal method and characterized with the aid of elemental analysis, IR, UV spectra and thermal analysis studies. The result of X-ray crystallography analysis exhibits that the title compound crystallizes in the orthorhombic space group P212121, and the formula is C96H64N16Cu4SiW12O40. Crystal data： a = 18.3574（14）, b = 21.1952（16）, c = 27.992（2）A, Mr = 4570.08, V = 10891.4（14）A^3, Z = 4, Dc = 2.787 g/cm^3,μ = 13.478 mm^-1, R = 0.0364, wR = 0.0638 （I 〉 2σ（I）） and F（000） = 8360. The complex consists of one α-Keggin anion [SIW12O40]^4- and four discrete [Cu^I（phen）2]^＋ cations. The valence sum calculations for the Cu atoms suggest that all four Cu atoms are in the ＋1 oxidation state.     

Hydrothermal Synthesis and Spectroscopic and Magnetic Behavior of the Mn7(HOXO3)4(XO4)2(X=As, P) Compounds. Crystal Structure of Mn7(HOAsO3)4(AsO4)2

The Mn₇(HOXO₃)₄(XO₄)₂ (X=As, P) compounds have been synthesized by using hydrothermal conditions. The arsenate phase was obtained under autogeneous pressure at 170°C. However, more drastic conditions at both pressure and temperature were necessary in the attainment of the phosphate compound. The crystal structure of Mn₇(HOAsO₃)₄(AsO₄)₂ was solved using single-crystal data. The unit-cell parameters are a=6.810(3) Å, b=8.239(2) Å, c=10.011(4) Å, α=104.31(2)°, β=108.94(3)°, γ=101.25(2)°. Triclinic, P-1 with Z=1. The isostructural Mn₇(HOPO₃)₄(PO₄)₂ phase was characterized from X-ray powder diffraction techniques. The crystal structure of both compounds consists of zig-zag chains constructed by dimeric edge-sharing Mn₂O₁₀ octahedra linked through the MnO₅ trigonal bipyramids. The three-dimensional framework is completed by the connection between isolated MnO₆ entities to the dimers octahedra and trigonal bipyramids. The existence of hydrogenarsenate and hydrogenphosphate anions has been confirmed by IR and Raman spectroscopies. Magnetic measurements indicate the existence of antiferromagnetic interactions in both compounds, which are slightly stronger in the arsenate phase.     

含新颖一维金属氧簇阳离子的聚金属氧簇化合物[{M(2,2'-bipy)}5O14]4- [2,2'-H2bipy]2(As2W18O62)2•8H2O (M＝Mo, W)的合成、晶体结构与表征

以Na₂WO₄•2H₂O, Na₂MoO₄•2H₂O, Na₂HAsO₄•7H₂O和2,2'-bipyridine为原料, 在水热条件下制得了含一维阳离子的聚金属氧簇化合物: [{M(2,2'-bipy)}₅O₁₄]₄[2,2'-H₂bipy]₂(As₂W₁₈O₆₂)₂•8H₂O (M＝Mo/W; 2,2'-bipy＝2,2'-bipyridyl), 并用元素分析, IR, TG和单晶X-ray衍射等手段进行了表征. 标题化合物属于单斜晶系, C2/c空间群, a＝4.1721(5) nm, b＝2.4629(5) nm, c＝1.7541(5) nm, β＝91.119(3)°, V＝18.021(5) nm³, Z＝2, R₁＝0.0629, wR₂＝0.1605 [I＞2σ(I)]. 标题化合物的阳离子链由五元金属氧簇构筑块[{M(2,2'-bipy)}₅O₁₄]^2＋通过氧原子桥联而成, 构筑块[{M(2,2'-bipy)}₅O₁₄]^2＋中的五个金属原子呈畸变的“A”字型排布, 阳离子展现出新颖的一维锯齿链状结构.     

二维层状结构十钒酸盐[K(H2O)2Ni(H2O)6]2[V10O28]的合成及性质(英)

A novel heteropoly compound, containing two kinds of coordinated cations, [K(H₂O)₂Ni(H₂O)₆]₂[V₁₀O₂₈], has been synthesized through routine process and characterized by elemental analyses, IR, ⁵¹V NMR and single crystal X-ray diffraction. It crystallizes in the triclinic system, space group P1 with a=0.87382(17) nm, b=1.075 4(2) nm, c=1.111 1(2) nm, α=65.10(3)°, β=75.01(3)°, γ=70.63(3)°, V=0.884 8(3) nm³ and Z=1. The X-ray analysis reveals that the two kinds of coordinated cations are linked by three shared coordinated water molecules, and K⁺ cations coordinate with ten oxygen atoms: five of which come from V₁₀O₂₈^6- anion, the other five from water molecules. The title compound exhibits extended 2D array building up of V₁₀O₂₈^6- groups connected by ten-coordinated K⁺ cations. The hexahydrated nickel cations Ni(H₂O)₆²⁺ lie in neat apposition to three adjacent V₁₀O₂₈^6- clusters. CSD: 413271.     

配位聚合物[NaMn(pic)3]n的水热合成和晶体结构

A Coordination polymer [NaMn(pic)₃]_n (1) (picH=picolinic acid) has been synthesized by hydrothermal synthesis and structurally characterized by single crystal structure determination. 1 crystallizes in the orthorhombic space group Pbca, a=1.251 9(4) nm, b=1.715 8(8) nm, c=1.754 7(7) nm, V=3.769(6) nm³, M_r=444.24, D_c=1.566, F(000)=1 800, R₁=0.024 8 and wR₂=0.075 1 for I>2σ(I). According to the crystal structure, each Mn(Ⅱ) ion of 1 is six-coordinated with three oxygen and three nitrogen atoms from three pic anions to form a distorted dodecahedron. Each Na⁺ ion of 1 is penta-coordinated with two oxygen atoms from a pic anion and three oxygen atoms from three pic anions of diffrent unit to form a distorted tetragnal pyramid. The three-dimensional coordination polymer 1 is connected through Na⁺ ion. CCDC: 683029.     

Hydrothermal Synthesis and Crystal Structure of the First Ammonium Indium(III) Phosphate NH4In(OH)PO4 with Spiral Chains of InO4(OH)2

An ammonium indium hydrogen phosphate, NH₄In(OH)PO₄, was synthesized under mild hydrothermal conditions, and the crystal structure was characterized by single-crystal X-ray diffraction method. The compound crystallizes with the RbIn(OH)PO₄ type with the following data: M_r=244.84, tetragonal, tP104, P4₃2₁2 (No.96), a=9.416(2) Å, c=11.159(3) Å, V=989.9(3) ų, Z=8, D_x=3.288 g cm⁻³, λ=0.71073 Å, μ=50.34 cm⁻¹, F(000)=928, T=293 K, R1=0.0606, wR2=0.1472 for 91 variables and 1813 contributing unique reflections. The structure is characterized by chiral InO₄(OH)₂ chains along the c axis formed by sharing OH corners. The chains are isolated by PO₄ tetrahedra leading to a three-dimensional framework structure with channels occupied by NH₄⁺ ions. The framework structure is similar to that of KIn(OH)PO₄ and γ-NaTiOPO₄. The hydrogen bonds formed by NH₄⁺ with the polyhedral oxygen atoms play an important role in the anisotropic changes of the lattice with respect to its alkali metal analogues. The topological construction of the title structure can be considered as an augmented 4,6-net with larger porosity.     

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。     

(NO2Ql)2[Ni(mnt)2]的合成和晶体结构((NO2Ql)+=1-(4-nitrobenzyl)-quilorinium;mnt2-=maleonitriledithiolate)

合成了离子对配合物(NO2Q1)2[Ni(mnt)2],并用元素分析和红外光谱进行了表征.单晶结构分析结果表明三斜晶系,空间群p-1.晶胞参数a=8.2240(16)A,6=10.777(2)A,c=12.137(2)A,α=72.58(3).,β=72.82(3)°,γ=68.78(3)°,V=935.4(3)A3,Z=1.(NO2Ql)+和[Ni(mnt)2]2-分别形成了完全分立的柱状堆积结构.在阴离子堆积柱内,Ni(Ⅱ)离子形成了一维均匀链.阳离子间,比邻的芳环间存在弱的π…π作用.     

Synthesis, crystal structure and properties of a new organic-inorganic hybrid Dawson-like polyoxotungstate [Co(2,2''''-bpy)3]2[Co(2,2''''-bpy)2Cl][Co(2,2''''-bpy)2]H2-[SbW18O60]·4H2O

A new organic-inorganic hybrid polyoxometalate based on Dawson-like polyoxotungstate anion [SbW18O60]9-, formulated [Co(2,2'-bpy)3]2[Co(2,2'-bpy)2Cl][Co(2,2'-bpy)2]H2[SbW18O60]·4H2O (2,2'-bpy= 2,2(-bipyridine) has been synthesized from Sb2O3, Na2WO4, CoCl2, and 2,2'-bipyridine materials by hydrothermal method, and which was characterized by elemental analyses, IR, XPS, EPR, TG, and X-ray single crystal diffraction. Structure analysis shows that the polyoxoanion self-assembled under hydrothermal conditions consists of a Dawson-like polyoxotungstate cluster anion [SbW18O60]9- encapsulating a pyramidal {SbO3} group within the {W18} cluster cage. EPR spectra show that the high-spin octahedral CoⅡ and low-spin CoⅡ ions coexist in the title compound. Magnetic properties indicate that the compound is antiferromagnetic.     

一个新颖的二重互穿的三维无机-有机杂化化合物[Cd(C5H3N2O2)2(H2O)]n的合成和晶体结构

近年来,由于无机-有机杂化化合物表现出独特的结构多样性以及在催化、光化学、电学和磁学等方面的巨大潜在应用.而引起了科学家们的广泛关注[1-4].     

无铅和稀土的大尺寸分子基绿光荧光晶体：(C5H13ClN)2[MnCl4]

通过氯化锰和2-二甲氨基异丙基氯盐酸盐在溶液中的反应,制备了一类绿光分子基晶态材料：（C₅H₁₃ClN）₂[MnCl₄]（1）。该材料在紫外光激发后发出强烈的绿色荧光,并且热分析测试表明其具有较好的热稳定性（分解温度大于450 K）。结构和光谱分析表明其优异的光学性能归因于[MnX₄]^2-四面体中Mn²⁺的⁴T₁（G）→⁶A₁电子跃迁。     

无铅和稀土的大尺寸分子基绿光荧光晶体:(C5H13ClN)2[MnCl4]

通过氯化锰和2-二甲氨基异丙基氯盐酸盐在溶液中的反应,制备了一类绿光分子基晶态材料：（C₅H₁₃ClN）₂[MnCl₄]（1）。该材料在紫外光激发后发出强烈的绿色荧光,并且热分析测试表明其具有较好的热稳定性（分解温度大于450 K）。结构和光谱分析表明其优异的光学性能归因于[MnX₄]^2-四面体中Mn²⁺的⁴T₁（G）→⁶A₁电子跃迁。     

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） nm^3, Mr = 1028.85, Dc = 1.424 g/cm^3, 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.     

超分子化合物[2-(4-pyridyl)benzimidazoleH2].[SnCl6]的水热合成及晶体结构

通过水热法合成了一个新的超分子化合物[PyBImH2]?[SnCl6] (PyBIm=2-(4-吡啶基)苯并咪唑), 并用元素分析、红外光谱、荧光光谱及X射线单晶衍射对其进行了分析测试。化合物属于正交晶系,Pbcn空间群,晶胞参数：a = 7.1468(3),b = 15.0493(6),c = 16.1195(8) ?,V = 1733.72(13) ?₃,Z = 4,Dc = 2.025 g/cm₃,Mr = 528.63,μ(MoKα) = 2.395 mm_-1,F(000) = 1024,R₁= 0.0264,wR₂ = 0.0665。Sn₄₊与6个氯离子配位,形成八面体的配位几何。配位阴离子[SnCl₆]_2-与[2-(4-吡啶基)苯并咪唑阳离子通过氢键及π-π 堆积作用形成三维超分子结构。     

配合物Zn(C3H4N2)2(C8H6O2Br)2的水热合成、晶体结构及性质

在140℃下,以3-溴-4-甲基苯甲酸和咪唑为配体,通过水热法在甲醇/水混合溶剂中反应24 h合成了锌(Ⅱ)配合物Zn(C3H4N2)2(C8H6O2Br)2。通过元素分析、红外光谱、热重分析和X射线粉末衍射对配合物进行了结构表征,同时用X射线单晶衍射分析确定了其晶体结构。结果表明,其晶体属单斜晶系,空间群为C2/c,晶胞参数:a=13.257(3),b=9.765(2),c=20.494(4),β=107.79(3)°,V=2526.3(9)3,Dc=1.655g·cm-3,μ=4.170mm-1,F(000)=1248,Z=4,最终残差因子R1=0.0552,wR2=0.1378。配合物为单核结构,中心锌(Ⅱ)离子与来自2个3-溴-4-甲基苯甲酸根的2个O原子及2个咪唑分子的2个N原子配位,形成了畸变的四方锥几何体。晶体内,分子间则通过N—H…O氢键作用在ab面形成了层状结构。研究了配合物的发光性质。     

多核银配位聚合物[Ag_2(BPE)(CF_3COO)_2]_n和{Ag_5(CF_3COO)_5[(CH_3)_3NCH_2COO]}_n的水热合成与晶体结构

<正>过渡金属配位聚合物因其丰富的网络拓扑结构及其在吸附、催化、分子识别、光、电、磁等方面的潜在应用而成为无机化学和材料化学研究领域中     

具有[344484]笼状结构单元的微孔磷酸镓Ga3P2O8(OH)3(H2O)的合成、晶体结构及表征

Open-framework metal phosphates have been the subject of intense research owing to their interesting structural chemistry and potential applications in catalysis and ion exchange. The gallium phosphate family has exhibits rich structural chemistry. A novel gallium phosphate Ga₃P₂O₈(OH)₃(H₂O)(GaPO-CJ36) has been prepared in a hydrothermal reaction system of GaO(OH)-H₃PO₄-Co(chxn)₃Cl₃-H₂O at 180 ℃ for 7 days. Single-crystal X-ray analysis shows that GaPO-CJ36 crystallizes in the P2₁/c space group with a=1.833 35(12) nm, b=0.503 94(3) nm, c=1.062 90(9) nm, V=0.982 01(12) nm³, and Z=4. The connection of GaO₂(OH)₃(H₂O) octahedra, PO₄ and GaO₄ tetrahedra through vertex oxygen atoms forms a three-dimensional open framework, which contains 8-ring channels along the [010] direction. Its structure is composed of interesting [3⁴4⁴8⁴] cages, which have not been found in known gallium phosphates. CSD: 416779.