Syntheses, Spectroscopic Properties and Crystal Structures of （2-Cl-C6H4CH2）3SnS2CN（C5H10） and （2-Cl-C6H4CH2）3SnS2CN（C4H9N）

1 INTRODUCTION The chemistry of organotin(IV) complexes was extensively studied due to their biological activity and coordination chemistry[1～7]. More recently, phar- maceutical properties of alkyltin(IV) complexes with dithiocarbamate ligands have bee…     

Syntheses and Crystal Structures of Two Coordination Compounds CuLCl（H2O） and Ni（L）2 （HL = 2-Carboxy-1,10-phenanthroline）

Two complexes CuLCl（H2O） 1 and Ni（L）2 2 （HL = 2-carboxy-1,10-phenanthroline） have been synthesized and characterized by single-crystal X-ray crystallography. The structure of 1 has a monoclinic space group P21/n with a = 7.985（2）, b = 16.067（3）, c = 9.694（2） A, β = 98.189（30）°, V= 1231.0（4） A^3, Z = 4, Dc = 1.836 g/cm^3,μ =1.998 mm^-1, F（000） = 684, the final R = 0.0301 and wR = 0.0810. The structure of 2 （C26H14N4NiO10） adopts an orthorhombic system, space group Pbea with a = 9.410（2）, b = 23.2410（5）, c = 23.8680（5） A, V = 5219.9（18） A^3, Z = 8, Mr = 601.12, Dc = 1,530 g/cm^3,μ = 0.809 mm^-1, F（000） = 2448, the final R = 0.0448 and wR = 0.1427. The Cu center of complex 1 exhibits a square pyramidal coordination environment with one oxygen and two nitrogen atoms from deprotonated 2-carboxy-1,10-phenanthroline, one oxygen atom from water and one chloride ion. The Ni center of complex 2 assumes a distorted octahedral coordination geometry consisting of two oxygen atoms and four nitrogen atoms of two deprotonated 2-carboxy-1,10-phenanthroline molecules. Supramolecular assembly has been found via noncovalent bonds, such as hydrogen bonds and π-π stacking interactions.     

Synthesis, Spectroscopic Properties and Crystal Structures of Dibenzyltin（IV） Dithiobenzoate and Chlorodibenzyltin（IV） Thiobenzoate

Two dibenzyltin(IV) complexes with thiobenzoate ligand, (PhCH2)2Sn(SOCPh)2 (1) and (PhCH2)2Sn(C1)SOCPh (2), have been synthesized by the reaction of dibenzyltin(IV) dichloride with thiobenzoic acid in the presence of organic base Et3N and characterized by IR, ^1H NMR spectroscopy and elemental analysis. Their crystal structures were determined by X-ray single crystal diffraction analysis. In the crystals of 1, the tin atom is six-coordinated in a distorted octahedron configuration. In the crystals of 2, the molecular packing in unit cell reveals that the two adjacent molecules are symmetrically linked to each other to form a dimer with intermolecular Sn…C1 distances of 0.3591 (2) nm and the tin atom is five-coordinated in a distorted trigonal bipyramid configuration.     

Syntheses and Crystal Structures of Two Mononuclear Tin（IV） Complexes Derivedfrom Sn（edt）2 （edt = Ethane-1,2-dithiolate）

1INTRODUCTIONRecentlythedesignandsynthesisoftinsulfide-basedsolidstatematerialshasreceivedmuchattentionowningtotheirinterestingoptical,catalyticandelectricalpropertiesfordeviceappli-cations[1].Becauseoftheversatilecoordinationcharacteristicsoftinandsulfur…     

Synthesis, Characterization and Properties of Organotin Complexes Dibutyltin（Ⅳ） Bis（heteroaromatic carboxylate） and Crystal Structure of Dibutyltin（Ⅳ） Bis（2-thiazolylcarboxylate）

The six organotin complexes dibutyltin(IV) bis(heteroaromatic carboxylate) were synthesized by the reaction of (n‐Bu)2SnO with heteroaromatic carboxylic acid in 1:2 molar ratio. These complexes have been characterized by elemental analysis, IR, ¹H, ¹³C and ¹¹⁹Sn NMR. The crystal structure of dibutyltin(IV) bis(2‐thiazolylcarboxylate) was determined by X‐ray single crystal diffraction. This compound is a weakly bridged dimer through weak interaction Sn···O between molecules. The tin atoms took six‐coordinate skew‐trapezoidal bipyramidal geometry. The crystal of complex 3 belongs to monoclinic symmetry with space group P2₁/c, a=1.863(2) nm, b=2.220(3) nm, c=1.0395(10) nm, β=90.275(16)°, Z=8, V=4.292(8) nm³, D_c=1.514 Mg/m³, μ=1.406 mm^‐1, F(000)=1968, S=0.999, R=0.0549, wR=0.1011.     

Syntheses and Crystal Structures of Two Diethyltin Complexes of N-Salicylidene-α-amino Acid

Two novel diethyltin（IV） complexes of N-salicylidenevaline （H2L1） and N-Sali- cylidenetryptophan （H2L^2）, Et2SrtL^1 1 and Et2SnL^2 2, were synthesized and characterized by elemental analysis, IR, ^1H NMR and X-ray single-crystal diffraction analysis. Complex 1 belongs to the trigonal system, space group R-3 with a = b = 19.2730（5）, c = 23.6890（13）A^°, V= 7620.4（5） A^°^3, Z = 6, Dc= 1.553 g/cm^3,μ= 1.518 mm^-1, F（000） = 3600, R = 0.0238 and wR = 0.0636. Complex 2 is of monoelinie system, space group P21/c with a = 13.7550（8）, b = 11.5425（7）, c = 12.7876（7）A^°, β= 93.585（1）°, V = 2026.3（2） A^°^3, Z = 4, Dc= 1.548 g/cm^3,μ = 1.286 mm^-1, F（000） = 976, R = 0.0298 and wR = 0.0722. Complex 1 is a cyclic trimer with a macrocyclic 12-membered ring structure formed by the bidentate bridging coordination of carboxylate group to tin atoms. The tin atom is six-coordinated in a distorted octahedral geometry. In complex 2, the distorted trigonal bipyramidal Et2SnL2 units are linked into polymeric chains by the weak Sn…O interaction involving Sn and the earbonyl O of an adjacent ligand, and the chains are further connected by intermolecular N-H…O hydrogen bonds to form a two-dimensional supramolecular structure.     

Synthesis,Characterization and Crystal Structure of Chlorodibenzyltin（Ⅳ） Complex with Dithiomorpholinocarba—mate Ligand

Chlorodibenzyltin (IV) complex with dithiomorpholinocarbamate ligand was synthesized by the reaction of dibenzyltin dichloride with dithiomorpholinocarbamate in 1:1 stoichiometry. The complex was characterized by elementary analysis, UV, BR and ¹H NMR spectra. The crystal structure was determined by X‐ray single crystal diffraction study. The crystallographic data are as follows: triclinic, space group P1 , a = 0.8723 (2) ran, b = 1.099 (2) nm, c = 1.1036 (3) nm, α = 86.498 (4)°, β = 89.697 (5)°, γ = 82.807 (5)°, Z = 2, V = 1.0479 (4) nm³, D_c= 1.580 g/cm^?3, μ = 1.553 mm^?1, F (000) = 500, R₁ = 0.0442, wR₂ = 0.0974. The crystal consists of discrete molecules containing five‐coordinate tin atoms in a distorted tigonal bipyramidal configuration. The molecules are packed in the unit cell in one‐dimensional chain structure through a weak interaction between the chlorine atom and sulfur atom, the sulfur atom and one of the sulfurs of an adjacent molecule.     

Synthesis and Crystal Structure of（Z）-2-Methyl-5,6-dihydrobenzo[d]thiazol-7（4H）-one O-Prop-2-yn-1-yl Oxime Derivatives

Compound(Z)-2-methyl-5,6-dihydrobenzo[d]thiazol-7(4H)-one O-prop-2-yn-1-yl oxime, C11H12N2 OS, as a synthetic precursor of cytotoxic triazoles has been prepared and characterized by NMR spectra. Meanwhile, the crystal of IV was obtained and determined by X-ray single-crystal diffraction. Crystal data: monoclinic system, space group P21/c, a = 9.725(9), b = 8.068(7), c = 14.452(13)A, β = 98.68(2)°, V = 1120.9(17)A3, Z = 4, F(000) = 464, Dc = 1.305 g/cm3, μ = 0.263 mm-1, R = 0.0457 and w R = 0.1298 for 11511 independent reflections(Rint = 0.0709) and 2289 observed ones(I 2σ(I)).     

Polymeric Three-Dimensional Crystal Structure of a Tributyltin(IV) Derivative with Acetylene Dicarboxylic Acid

Abstract

A novel polymeric complex has been synthesized by refluxing disodium acetylene dicarboxylate with tributyltin chloride in dry methanol. The solid-state structure of the complex has been determined by single-crystal X-ray analysis. The tin(IV) metal exhibits distorted trigonal bipyramidal geometry. Each carboxylate group of the ligand acts in a bidentate fashion, linking adjacent metal atoms to produce polymeric chains, which are cross-linked into a three-dimensional network.     

三苄基锡哌啶氨荒酸酯和二苄基锡双哌啶氨荒酸酯合成及晶体结构

利用三苄基氯化锡,二苄基二氯化锡和哌啶氨荒酸钠反应,合成了三苄基锡哌 啶氨荒酸酯（1）和二苄基锡双哌啶氨荒酸酯（2）。通过元素分析、红外光谱、核 磁共振氢谱和质谱对其结构进行了表征。用X-射线单晶衍射测定了这两个化合物的 晶体结构。化合物1为三斜晶系,空间群P-1,a=1.0271(2)nm,b=1.1131(2)nm,c=1. 2096(2)nm,α=75.56(3)°,β=81.09(3)°,γ=89.81(3)°,Z=2。化合物2为单 斜晶系,空间群P21/c,a=0.9710(3),b=2.436(1),c=1.2393(3)nm,β=90.28(2)°, Z=4。在1的晶体中, 锡原子呈五配位畸变三角双锥构型;2的晶体则是六配位的畸 变八面体构型。     

丙酮酸异烟酰腙四核有机锡配合物的合成、表征及{[nBu2Sn(C9H8N3O3)O]SnBu3n}2的晶体结构

The tetranuclear alkyltin(Ⅳ) compounds {[R2Sn(C9H8N3O3)O]SnR3}2 [R=n-Bu (1), 4-CNC6H4CH2 (2),C6H5CH2 (3), 4-ClC6H4CH2 (4)] were prepared by the reaction of Schiff base ligand pyruvic acid isonicotinyl hydrazone with (R3Sn)2O in the corresponding molar ratio of 1:1. All compounds have been characterized by elemental analysis, IR and ^1H NMR spectra. The crystal structure of compound 1 was determined by X-ray single crystal diffractional analysis. This compound exhibits a dimeric structure containing distannoxane units with two types of the tin atoms. For the first tin atom, it appears to be seven-coordinated with a distorted pentagonal bipyramid geometry, and the other is five-coordinated with a distorted trigonal bipyramidal geometry. The molecules are packed in the unit cell in two-dimensional network structure through an interaction between the N atoms of the pyridine and the tin atoms of an adjacent molecule.     

Untersuchungen über Zinn(IV)-alkoxide. II. Isolierung und Charakterisierung der Verbindung Sn3O(OiBu)10 · 2i-BuOH. Das erste Beispiel für ein partielles Hydrolyseprodukt eines Zinn(IV)-alkoxids

Investigations into Tin(IV) Alkoxides. II. Isolation and Characterization of the Compound Sn₃O(OⁱBu)₁₀₁₀ · 2i-BuOH. The First Example of a Partially Hydrolized Tin(IV) Alkoxide The partial hydrolysis product Sn₃O(OⁱBu)₁₀ · 2i-BuOH was obtained by slow hydrolysis of the reaction product of tin tetrachloride with sodium isobutoxide. The compound forms colourless, moisture sensitive crystals, which easily release the coordinated solvent molecules in dry air. Its crystal and molecular structure has been determinated by single crystal X-ray diffraction. The compound crystallizes in the triclinic space group P1 with a = 1363.5(7), b = 1462.7(10), c = 1637.7(7) pm, α = 95.40(5)°, β = 96.79(4)°, γ = 102.12(5)° and Z = 2. The crystal structure consists of discrete, trimeric molecules with octahedrally coordinated tin atoms which are connected to each other corresponding to the formulation Sn₃(μ₃-O)(μ₂-OⁱBu)₃(O¹Bu)₇ · (i-BuOH)₂ by three isobutoxide groups bridging two metal atoms and a single threefold bridging oxygen atom     

Structural Studies on Dimethyltin(IV) Carboxylates

In order to correlate ¹¹⁹Sn Mössbauer parameters and structural data for dimethyltin(IV) derivatives, the molecular structures of bis(acetato)dimethyltin(IV) and bis(trifluoroacetato)dimethyltin(IV) were determined by single crystal X-ray diffration. Crystals of Me₂Sn(OOCCH₃)₂ are monoclinic, a = 26.282(4), b = 5.282(1), c = 14.434(3) Å, β = 101.17(2)°, Z = 8, space group C2/c, and those of [Me₂Sn(OOCCF₃)₂]_n are monoclinic, a = 8.444(1), b = 17.689(1), c = 15.368(1) Å, β = 93.013(9)°, Z = 8, space group Cc. The structures were solved by the Patterson method and were refined by full-matrix least-squares procedures to R = 0.025 and 0.027 (R_w = 0.023 and 0.030) for 2 298 and 4 182 reflections with I ≥ 3σ(F²), respectively.     

Tin(IV) Complexes of 1,5-Diphenylthiocarbazone and Thiosemicarbazide: Synthesis,X-Ray Characterization,and Biological Activity

Abstract

The reaction of Me₂SnCl₂ with dithizone or thiosemicarbazide produced two novel di-organotin derivatives in good yields, which were characterized by X-ray diffraction. The crystal structures show that the compounds present a distorted pentacoordinated tin(IV) metal center. The antimicrobial activity of the new compounds was studied against Gram-negative (Escherichia coli, Klebsiella pneumonia, Salmonella enteritidis) and Gram-positive (Staphylococcus aureus) bacteria, and the yeast Saccharomyces cerevisiae. It was observed that the coordination of tin metal has a pronounced effect on the microbial activities of the ligands. All the tin complexes have shown higher antimicrobial effect than the free ligands.

GRAPHICAL ABSTRACT     

Synthesis and Crystal Structure of Di-n-butyltin(IV) Complex with 2-Oxo-propionic Acid (4-Pyridinecarbonyl) Hydrazone

Introduction The studies of diorganotin(IV) complexes are of current interest owing to their wide range of applica-tions such as biocides and homogeneous catalysts in industry.1 In recent years there have been more and more reports on the synthesis, antitumour activities and structural elucidation of various diorganotin(IV) deriva-tives of carboxylic acid.2-5 In particular, people take considerable interest in structural studies of diorgano-tin(IV) complexes of carboxylic acid, because there…