Synthesis and Crystal Structure of a Dialkyltin Benzamidoacetate Compound {[n-Bu2Sn（O2CCH2NHCOC6H5）]2O}2·C6H6

A dialkyltin benzamidoacetate compound {[n-Bu2Sn（O2CCH2NHCOC6H5）]2O}2· C6H6 has been synthesized by the reaction of dialkyltin oxide with benzamidoacetic acid in 1：1 molar ratio, and its structure was determined by X-ray single-crystal diffraction. The crystal belongs to orthorhombic, space group Pca21, with a = 1.9134（4）, b = 1.9605（4）, c = 2.0657（4） nm, Z = 4, V = 7.749（3） nm^3, Dc = 1.054 mg·m^-3,μ（MoKa） = 1.337 mm^-1, F（000） = 3576, the final R = 0.0405 and wR = 0.0860. According to the structural analysis, the tin atom adopts a distorted five-coordinate trigonal bipyramidal geometry, and the dimer structure is shaped by one planar four-membered Sn2O2 ring.     

Supramolecular Terbium-SIP Complex Pillared by 4,4＇-Bipyridyl, {[Tb（SIP）（H2O）5]2（bpy）3（H2O）}n： Synthesis,Crystal Structure and Photoluminescence

The supramolecular terbium complex, {[Tb（SIP）（H2O）5]2（bpy）3（H2O）}n （NaH2SIP = 5-sulfoisophthalic acid monosodium salt and bpy = 4,4＇-bipyridyl）, has been synthesized by the hydrothermal reaction of Tb4O7 with NaH2SIP and bpy at 165 ℃, and characterized by single-crystal X-ray diffraction, elemental analysis, IR spectrum, powder X-ray diffraction and photoluminescence spectrum. It crystallizes in a monoclinic system, space group C2/c, with a = 30.6840（1）, b = 10.9206（2）, c = 17.4967（3） A, β= 111.931（1）°, V = 5438.65（14） A^3, Z = 4, C46H52N6O25S2Tb2, Mr = 1470.90, Dc = 1.796 g/cm^3, p = 2.747 mm^-1, F（000） = 2928, the final R = 0.0654 and wR = 0.1322 for 3806 observed reflections with I 〉 2σ（I）. In the neutral [Tb（SIP）（H2O）5]2 motif, the Tb（III） ions are linked by the SIP ligands to form a one-dimensional zigzag chain propagating along the c axis. The zigzag chains are linked together by hydrogen bonds and π-π stacking interactions to form a two-dimensional supramolecular framework. The uncoordinated bpy molecules act as pillars to extend the two-dimensional sheets into a distinctive pillared three-dimensional supramolecular structure through O-H...N hydrogen bonds. The photoluminescence of the complex was investigated at room temperature in the solid state.     

Synthesis, Crystal Structure and Quantum Chemistry of Dibutyltin 3, 4-Dimethoxybenzotate Compound

The dibutyltin 3,4-dimethoxybenzotate compound {[(3,4-(CH3O)2C6H3COO) Sn(Bu-n)2]2O}2 has been synthesized by the reaction of dibutyltin oxide with 3,4-dimethoxybenzoic acid. Its structure was determined by X-ray single-crystal diffraction. The crystal belongs to the triclinic system,space group P1 with a = 1.2003(2),b = 1.2821(3),c = 1.3666(3) nm,α = 80.50(3),β = 65.56(3),γ = 73.36(3)°,Z = 2,V = 1.8318(6) nm3,Dc = 1.530 Mg·m-3,μ(MoKa) = 1.413 mm-1,F(000) = 860,R = 0.0554 and wR = 0.1092. In the complex,each tin atom adopts a distorted tigonal bipyramidal structure,and the dimer structure is shaped by one Sn2O2 planar four-membered ring. The stabilities of the title complex,along with its orbital energies and composition characteristics of some frontier molecular orbitals have been investigated by means of quantum chemistry calculation methods.     

In Situ Hydrothermal Synthesis of a Mononuclear Copper（Ⅱ） Complex： Cu（H2SIP-O）（bpy）（H2O） （H4SIP-O = 4-Hydroxyl-5-sulfoisophthalic Acid）

The mononuclear complex, Cu（H2SIP-O）（bpy）（H2O） （H4SIP-O = 4-hydroxyl- 5-sulfoisophthalic acid and bpy = 2,2＇-dipyridyl）, has been synthesized by the hydrothermal reaction of Cu（OH）2 with NaH2SIP and bpy at 160 ℃, and characterized by single-crystal X-ray diffraction, elemental analysis and IR spectrum. The new ligand 4-hydroxyl-5-sulfoisophthalic acid derived from 5-sulfoisophthalic acid ligand under an in situ hydrothermal condition. The crystal of the complex crystallizes in a triclinic system, space group P1, with a = 7.757（4）, b = 10.663（6）, c = 11.727（7）A, α = 94.272（4）, β = 104.067（7）, γ = 97.400（7）°, V= 927.4（9）A^3, Z = 2, C18H14N2O9SCu, Mr= 497.93, Dc= 1.783 g/cm^3,μ = 1.350 mm^-1, F（000） = 506, the final R = 0.0518 and wR = 0.1513 for 4180 observed reflections with I 〉 2σ（I）. The central Cu（II） ion is five-coordinated by two oxygen atoms from the H2SIP-O^2- ligand and two nitrogen atoms of bpy ligand in a distorted square-planar geometry as well as a water oxygen atom in the apical position to complete a distorted square-pyramidal coordination geometry. The mononuclear copper molecules are linked by hydrogen bonds between coordinated water molecules and sulfonate groups to form a one-dimensional double-chain structure. The chains are further held together through extensive π-π stacking interactions between the aromatic rings to form a three- dimensional supramolecular structure.     

Synthesis and Crystal Structure of [2-Hydroxy- 5-（4-hydroxy-3-phenyliminomethylbenzyl）-benzylidene]-phenyl-amine

The title compound [2-hydroxy-5-（4-hydroxy-3-phenyliminomethyl-benzyl）-benzylidene]-phenyl-amine （C27H22N2O2, Mr = 406.47） was synthesized by 5,5′-methylene-bissalicylal- dehyde with aminobenezene, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group C2/c with a = 4.4026（6）, b = 1.501（13）, c = 0.95818（12） nm, β = 90.868（2）°, V= 4.2813（9） nm^3, Z= 8, Dc= 1.292 g/cm^3,μ = 0.010, F（000） = 1744, R = 0.0576 and wR = 0.1450 for 3766 observed reflections with I 〉 2σ（I）. X-ray analysis reveals that the molecule has a pair of intramolecular OH…N hydrogen bonds.     

Synthesis and Crystal Structure of N-phenyl-N-[（o-nitrophenylacetyl）oxy]benzamide

The compound N-phenyl-N-[（o-nitrophenylacetyl）oxy]benzamide （C21HI6N2Os, Mr = 376） has been synthesized by the reaction of N-hydroxy-N-phenylbenzamide with 2-（2-nitro- phenyl）acetyl chloride in dichlorom-ethane and its structure Was characterized by 1H NMR, 13C NMR, IR, H RMS（ESI） and single-crystal X-ray diffraction. The crystal of the title compound belongs to monoclinic, space group C2/c with a = 32.30（2）, b = 8.400（5）, c = 15.099（9） A, fl = 114.256（10）°, V = 3735（4） A3, Z = 8, D, = 1.339 g/cm3, F（000） = 1568, p = 0.097 mm-1, the final R = 0.0506 and wR = 0.1176 for 2318 observed reflections （1 〉 2a（/））. The title molecule contains three branched chains with its center placed at the midpoint of N. The phenyl ring （C（1）＇-C（6）） makes a dihedral angle of 70.3（1）° with the phenyl ring （C（10）-C（15）） of benzoyl group, and 14.3（1）° with the phenyl ring （C（16） - C（21））, Hydrogen bonds C（5）-H（5）...O（1） and C（12）-H（12）...O（3） together with it-Jr stacking interactions contribute to the stability of the structure.     

Synthesis and Crystal Structure of 2,6-Bis（benzimidazo（1,2-c）- quinazolin-6-yl）pyridine Tetrahydrate

The title compound, 2,6-bis（benzimidazo（1,2-c）quinazolin-6-yl）pyridine tetrahydrate, was synthesized by simple condensation of 2-（2-sminophenyl） benzimidazole with pyfidine- 2,6-dicarboxylic acid and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group C2/c with a = 22.226（8）, b = 16.730（7）, c = 16.820（5）A, β = 115.796（13）°, V = 5631（4）A^3, C33H27NTO4, Mr = 585.62, Z = 8, Dc = 1.381 g/cm^3, λ（MoKα） = 0.71073 A, F（000） = 2448 and μ = 0.09 mm^-1. The structure was refined to the final R = 0.0730 and wR = 0.1573 for 6346 independent reflections （Rint = 0.0801） and 3384 observed reflections （I 〉 2σ（I））. In the crystal, the molecules are linked through intermolecular O-H…O and O-H…N hydrogen bonds. Intermolecular π-π interactions （with distances of about 3.45 A） are pronounced in the crystal structure.     

Synthesis and Single-crystal Structure of a One-dimensional Zinc（Ⅱ） Phosphonate： [Zn3（PhPO3）2（PhPO3H）2（Phen）2]n

A new Zn（II） phosphonate complex, [Zn3（PhPO3）2（PhPO3H）2（Phen）2]n （Phen = 1,10-phenanthroline）, has been synthesized and structurally determined by X-ray single-crystal diffraction. The complex crystallizes in the monoclinic system, space group C2/c with a = 14.997（3）, b = 18.108（4）, c = 17.237（3） A, β = 96.61（3）°, V = 4649.9（16） A3, Z = 4, C48H38N4O12P4Zn3, Mr = 1182.87, Dc = 1.690 g/cm3^,μ = 1.743 mm^-1, F（000） = 2400, the final R = 0.0363 and wR = 0.0963. In the structure, the connectivity between two 5-coordinated Zn（II） atoms and four phosphonates as well as two Phen ligands form a Zn2（PhPO3H）2（PhPO3）2（Phen）2 unit, and such a neighboring unit is bridged by 4-coordinated Zn（II） to give rise to a 1D chain along the c axis. The π-π stacking interactions between Phen rings assemble adjacent chains packed together to form a 3D supermolecular architecture.     

Synthesis and Crystal Structure of a Nitronyl Nitroxide Complex { [Zn（NIT4Py）（fum）（H2O）2]·H2O }n

The title compound {[Zn（NIT4Py）（fum）（HEO）2]·H2O}n, where NIT4Py = 2-（4＇- pyridinyl）-4,4,5,5-tetra-methylimidazoline-looxyl-3-oxide and fum = fumarate, has been prepared and structurally characterized by X-ray diffraction. It crystallizes in triclinic, space group P1^- with a = 6.9533（9）, b = 9.805（1）, c = 15.248（2） A, α= 94.608（2）, β = 92.328（2）, γ = 105.840（2）°, C16H24N3O9Zn, Mr = 467.75, V = 994.8（2） A^3, Z = 2, Dc = 1.562 g/cm^3,μ（MoKα） = 1.289 mm^-1, F（000） = 486, the final R = 0.0243 and wR = 0.0622 for 3505 independent reflections with Rint = 0.0125. The Zn（II） adopts a distorted five-coordinate triangle bipyramidal geometry. The basic framework structure of the complex is a 1-D chain. The intrachain hydrogen bonds are helpful to stabilize the 1-D chain structure. Furthermore, the chains are connected by O-H…O hydrogen bonds to give a 2-D double-layer network.     

Synthesis and Crystal Structure of a Novel 3D Inorganic-organic Hybrid Metallic Coordination Polymer, [Na2Cd（2,6-pyda）（N3）2（H2O）6]n

A novel coordination polymer [Na2Cd（2,6-pyda）（N3）2（H2O）6]n （2,6-H2pyda = 2,6- pyridinedicarboxylic acid） has been synthesized and characterized by elemental analysis, IR and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group C2/c, with a = 24.416（4）, b = 10.7638（17）, c = 6.9224（11） A^°, β= 106.124（2）A^°, V = 1747.7（5） A^°3, Mr = 515.64, De= 1.960 g/cm^3,μ = 1.365 mm^-1, F（000） = 1024, Z = 4, the final R = 0.0426 and wR = 0.1320. In the title complex, there exist two kinds of metal centers in the structure, cadmium ions and sodium ions. The Cd（Ⅱ） atom shows a distorted pentagonal-dipyramidal geometry defined by two O and one N atoms from one deprotonated pyda ligand and four N atoms from four μ-1,1,3 azido groups. The adjacent cadmium atoms are bridged via two μ-1,1,3 azido groups, along the c axis to afford an extended chain. There is also a 2D network which is comprised of binuclear subunits [NaE（H2O）6] connected by O atoms from coordinated water between the adjacent Cdn（pyda）n（Na）2n infinite chains. Furthermore, each cadmium atom is connected with four adjacent sodium atoms through the bridging N3- ligand in μ-1,3 patterns. Thus, the title complex exhibits a novel three-dimensional network structure.     

有机锡氧羧酸簇合物[PhCH_2Sn(O)(O_2CCH=CHAr)]_6的合成、表征和[PhCH_2Sn(O)(O_2CCH=CHPh)]_6的晶体结构

利用(PhCH_2)_3Sn]_2O与ArCH=CHCO_2H反应，合成6个新的[PhCH_2Sn(O) (O_2CCH=CHAr)]_6簇合物。通过元素分析、红外光谱和X射线单晶衍射对其结构进 行了表征。用X射线单晶衍射测定了[PhCH_2Sn(O)(O_2CCH=CHPh)]_6的晶体结构， 结果表明，该簇合物为三斜晶系，空间群P1, a = 1.6771(3) nm, b = 1.8020(4) nm, c = 2.1073(4) nm, α = 108.111(3)°β = 103.614(3)°,γ = 104.679 (3)°,Z = 2, V = 5.5033(18) nm~3, D_c = 1.350 g/cm~3, μ = 1.396 mm~(-1) , F(000) = 2208, R = 0.0606, wR = 0.698。该化合物为鼓型簇状结构，锡原子 呈畸变的八面体构型。     

Synthesis and Crystal Structure of the Ladder-like Organotin Complex: μ-pentaoxygen bridged penta(bis-benzyltin) bis-salicylate

A novel organotin complex of μ-pentaoxygen bridged penta(bis-benzyltin) bis- salicylate has been synthesized by the reaction of bis-benzyltin oxide and salicylic acid and its struc- ture has been determined by X-ray diffraction. The crystal belongs to monoclinic, space group P21/n with a = 1.7206(5), b = 2.1401(6), c = 2.1488(6) nm, β = 93.325(5)o, V = 7.899(4) nm3, Z = 4, Dc = 1.564 g/cm3, μ(MoKα) = 16.17 cm-1, Mr = 1859.94, F(000) = 3692, R1 = 0.0755 and wR2 = 0.1557. According to structural analysis, the coordination geometry of tin is a distorted trigonal bipyramid, and the ladder-like structure is shaped by four Sn2O2 planar four-membered rings.     

Synthesis and Crystal Structure of a Novel Ladder-like Organooxotin Cluster from 2,4,6-Trimethylbenzolic Acid and N-Benzylhydroxylamine

~~Synthesis and Crystal Structure of a Novel Ladder-like Organooxotin Cluster from 2,4,6-Trimethylbenzolic Acid and N-Benzylhydroxylamine@张春华$Department of Chemistry and Materials Science,Hengyang Normal University!Hengyang 421008,China @陈满生$Department of Chemistry and Materials Science,Hengyang Normal University!Hengyang 421008,China @李薇$Department of Chemistry and Materials Science,Hengyang Normal University!Hengyang 421008,China @杨颖群$Department of Chemistry an…     

Synthesis and Crystal Structure of the Organotin Complex [(o-Cl-PhCH_2)_3SnOCOC_(10)H_8N]·0.5C_6H_6

1 INTRODUCTION There is increasing interest in the study of orga-notin carboxylic ester compounds due to their insec-ticidal, fungicidal and antibiotic activities[1, as well 2]as structure diversity. In recent years many organo-tin carboxylic ester compounds with good biologi-cal activity have been synthesized[3, . Previous stu- 4]dies show that the coordination geometry of centralatom Sn …     

[M(en)3]2Sn2Se6(M=Mn,Zn)的制备及其热稳定性

用有机溶剂热生长技术(SolvothermalTechnique)制备过渡金属锰和锌硒化物[Mn(en)3]2Sn2Se6(Ⅰ),[Zn(en)3]2Sn2Se6(Ⅱ).用单晶X射线衍射技术对其进行晶体结构分析.[Zn(en)3]2Sn2Se6样品的热分析结果表明,该化合物的热分解分三步进行.光学性质测试表明它们是半导体材料,[Mn(en)3]2Sn2Se6的能带隙为1.76eV.[Zn(en)3]2Sn2Se6的能带隙为2.49eV.     

Solvothermal Syntheses of (H_2en)_2Sn_2S_6·en and[(H_2hmda)_3(Hhmda)_2](Sn_2S_6)_2Using SnCl_4 and S_8 as Starting Materials

1 INTRODUCTION Since Bedard et al. reported microporous tin(IV) sulfides synthesized by hydrothermal method in the presence of organic amine in 1989[1, 2], a number of thiostannates have been synthesized using hydro- or solvothermal techniques with organic amines as tem- plates. The structures of the resulting tin(IV) sulfi- des are related to the types of organic amines. Two- dimensional polyanions of the types of [Sn3S7]2- and [Sn4S9]2-, which are denoted as SnS-1 and SnS-3, respe…     

Synthesis and Structural Characterization of Manganese Carbonyl Incorporated Polyoxomolybdate (n-Bu_4N)_2[Mo_6O_(16)(OCH_3)_2{HOCH_2C(CH_2O)_3}_2{Mn(CO)_3}_2]

The polyoxoanion incorporated {Mn(CO)3+} complex, (n-Bu4N)2[Mo6O16(OCH3)2{HOCH2C(CH2O)3}2· {Mn(CO)3}2](1), has been synthesized by the reaction of (n-Bu4N)4[Mo8O26] with Mn(CO)5Br in methanol, in the presence of C(CH2OH)4. The complex 1 has been characterized by IR, UV-Vis, X-ray single crystal diffraction, and TG. Crystal data for the complex 1: C25H48MnMo3NO16 (1), Triclinic P1, a=0.9405(3) nm, b=1.3351(4) nm, c=1.5455(4) nm, α=103.206(5)o, β=102.165(5)o, γ=100.784(5)o, V=1.7896(9) nm3, Z=2, R1=0.0703, wR...     

配合物(n-Bu)2Sn(C10H8N2O4)(C2H5OH)的合成和晶体结构

以2-羰基丙酸水杨酰腙作为配体与二正丁基氧化锡(Ⅳ)在苯/乙醇混合溶剂中反应, 合成了新型配合物(n-Bu)2Sn(C10H8N2O4)(C2H5OH)(C10H8N2O42为2-羰基丙酸水杨酰腙负二价离子)。用单晶X-射线衍射分析法测定了该配合物的晶体结构。晶体属四方晶系, I41/a空间群, 晶胞参数a = 2.5113(7), b = 2.5113(7), c = 1.5062(6) nm, V = 9.499(5) nm3, Z = 16, Dc = 1.396 g/cm3, m(MoKa) = 1.105 mm1, F (000) = 4096。对于2499 (I >2s(I))个可观测点, 最终可靠因子R = 0.0349, wR = 0.0793。在该配合物的分子结构中, 中心锡原子与3个O原子、1个N原子和2个C原子形成扭曲的八面体几何构型, 其中3个O原子和1个N原子为赤道配位原子, 而CSnC为配合物的轴。相邻配合物分子间因Sn…O的弱相互作用和分子间氢键的作用而以二聚体的结构形式存在。