Synthesis,Characterization and Crystal Structure of (PhCH2)2Sn(S2CENt2) and (PhCH2)2Sn(S2CNC4H8)2

Two new dibenzyltin bisditiocarbamates(PhCH2)2 Sn(S2CNEt2)2(1) and (PhCH2)2 Sn(S2CNC4H8)2(2) were synthesized by the reaction of dibenzyltin dichloride with dithiocarbamates and characterized by elemental analysis ,IR,^1H NMR and MS spectra.The crystal structures were determined by X-ray single crystal diffraction analysis.In both complexes,the tin atom is six-coordinated in a distorted octahedral configuration.In the crystals of 1,the molecular packing in unit cell reveals that the two adjacent molecules are symmetrically linked to each other in dimers by two Sn S interactions of 0.3816nm.In the crystals of 2,the molecules are packed in the unit cell in one-dimensional chain structure linked by weaker intermolecular S S conmtacts.     

One—dimesional Infinite Chain Organotin Compounds： Synthesis and structural Characterization of Triphenyltin Thiazole—2—carboxylate and Triphenyltin 3—Pyridinylcarboxylate

Triphenyitin thiazole-2-carboxylate(1) and triphenyltin 3-pyridinylcar boxylate(2) were synthesized by the reaction of sodium thiazole-2-carboxylate or sodium 3-pyridinylcarboxylate with the triphenyltin chloride and their crystal structures were determined by single crystal X-ray diffraction analysis.In the structure of 1, the tin atom is five-coordinated in a distorted trigonal bipyramidal structure.Due to the presence of a close intermolecular Sn…S interaction distance of 0.3666nm,the structre can be described as a weakly-bridged on-dimensional chain compound.In the structure of 2,the tin atom is five-coordinated with bridging 3-pyridinylcarboxylate ligands N atom and resulting structure is one-dimensional chain compound.     

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.     

Synthesis, Characterization and Crystal Structure of （Z）-1-[2-（Triarylstannyl）vinyl]-1-indanols and Their Arylhalostannyl Derivatives

(Z)-1-[2-(Tri-o-tolylstannyl)vinyl]-1-indanol (1) and (Z)-1-[2-(tri-p-tolylstannyl)vinyl]-l-indanol (2) were synthesized by the addition reaction of 1-ethynylindanol with tri-o-tolyltin and tri-p-tolyltin hydride. The aryl groups in compound 1 and 2 were substituted by Br2 or I2 to yield monohalide derivatives (3-6). The compounds 1-6 were characterized by elemental analysis, ^1H NMR and FT-IR spectroscopy. The crystal structures of 1, 2 and 4 have been determined by single crystal X-ray diffraction analysis. The Sn atom in 1 and 2 exhibits a tetrahedral geometry distorted towards trigonal bipyramid due to a weak intramolecular interaction between Sn and the hydroxyl O atoms [0.2839(4) nm and 0.2744(5) nm], while the Sn atom in 4 adopts a trigonal bipyramidal geometry with a significant O→Sn(1) interaction [0.2552(5) nm].     

Hydrothermal Processing,Characterization and Theoretical Calculations of a Copper（Ⅱ） Compound with 1,10-Phenanthroline Derivative Ligand：2-（4-Methoxyphenyl）-1H-imidazo[4,5-f][1,10] Phenanthroline

The metal-organic compound [Cu(MOPIP)2(OH)2] 1(MOPIP = 2-(4-methoxy-phenyl)-1H-imidazo[4,5-f][1,10] phenanthroline) was hydrothermally synthesized and structurally characterized by elemental analysis,Fourier-transformed infrared spectroscopy,thermogravimetric analysis,single-crystal X-ray diffraction and theoretical calculations in Gaussian 03.In the crystal structure,the copper(Cu) atoms are tetra-coordinated with four different nitrogen atoms from two different MOPIP ligands,and the Cu atom is one of the five vertexes of the tetrahedron.Presumably due to the steric bulk of the phenyl ligands,compound 1 adopts a slightly distorted tetrahedral configuration.Moreover,it exhibits a zero-dimensional structure with Cu-MOPIP as the building units.Natural Bond Orbital(NBO) analysis was performed by using the NBO method built in Gaussian 03 Program.The calculation results showed a covalent interaction between the coordinated atoms and Cu(Ⅱ) ion.     

Synthesis,Crystal Structure,and Thermal Stability of a Dibutyltin Complex {[4-Et2NC6H3（O）C=NC6H3（O）- 5-NO2]（n-Bu2Sn）}2 and Its Interaction with DNA

The Schiff base organotin(IV) complex {[4-Et2NC6H3(O)C=NC6H3(O)-5-NO2](nBu2Sn)}2 has been synthesized via the reaction between 4-(diethylamino) salicylaldehyde-2-amino-4-nitrophenol Schiff base(H2L) and dibutyltin oxide. Complex C1 has been characterized by IR, 1H NMR, 13 C NMR spectra, and elemental analysis, and its crystal structure was determined by X-ray diffraction. It crystallizes in the monoclinic system, space group P21/n with a = 15.6559(8), b = 9.1657(5), c = 18.8351(10) , β = 107.3440(10)°, Z = 4, V = 2579.9(2) 3, Dc = 1.442 Mg·m-3, μ(MoKα) = 1.025 mm-1, F(000) = 1152, R = 0.0250 and wR = 0.0633. The central Sn atom is coordinated in a hexadentate manner to assume a distorted octahedral configuration. Complex C1 was studied by TGA analysis in air atmosphere. The interaction between complex C1 and the herring sperm DNA was realized through the intercalation of the complex based on the studies by EB fluorescent probe.     

Synthesis and Crystal Structures of Three Ladder Distannoxane Dimers [（PhCH2）2（Cl）SnOSn（X）（CH2Ph）2]2（X=Cl,OMe,OEt）

Three distannoxane dimers[(PhCH2)2(Cl)SnOSn(X)(CH2Ph)2]2(X=Cl,OMe,OEt)were prepared by the hydrolytic reaction of (PhCH2)2SnCl2 with sodium alkoxides.The compounds are assigned tetranuclear distannoxane structures in solid state.which contain the so-called ladder arrangement with a central planar Sn2O2 four-membered ring.The endo-and exo-cyclic Sn atoms are both five-coordinate,and have distorted trigonal bipyramidal geometries.A variety of hydrolyses of(PhCH2)2SnCl2 were performed and these dimers were characterized by IR,^1H NMR spectroscopy and X-ray diffraction analysis.     

Syntheses, Characterization and Crystal Structures of Two-dimensional 4,4＇-Bipyridyl Lead Halides, PbI2 （4,4＇-bpy） and PbBr2 （4,4＇-bpy）

Two-dimensional 4,4-bipyridyllead halides, Pbl2 (4,4‘-bpy) (1) and PbBr2 ( 4,4‘-bpy ) (2), were synthesized. The structures were determined by means of X-ray single crystal diffraction. The structure shows a distorted octahedral configuration with six-coordinated central lead atoms. In crystals 1 and 2, the molecules are packed in a two-dimensional network structure through bridging halide atoms and 4,4‘-bipyridine ligands between the adjacent lead atoms.     

Synthesis,halogenation and structural characterization of (Z)-1-[2-(triphenylstannyl)vinyl]-l-cyclododecanol

Synthesis and characterization of (Z)-1-[2-(triphenylstannyl)vinylj-l-cyclododecanol,c-(CH2)11C(OH)CH=CHSnPh3,are reported,together with its halogenation by I2,Br2 and IC1 to yield derivatives of the types c-(CH2)11C(OH)CH=CHSnPh3_nXn (n=1,2; X=I,Br,Cl,respectively).The molecular structures of two compounds have been determined by X-ray diffraction analysis.The tin atom exhibits a distorted tetrahedral geometry in the crystal of (Z)-1-[2-(triphenylstannyl)vinyl]-1-cyclododecanol,but a trigonal bipyramidal geometry in the monoiodo-derivative (Z)-1-[2-(diphenyliodo-stannyl)vinyl]-l-cyclododecanol and other derivatives,in which significant intramolecular coordinative interaction HO→Sn is observed.And the formation of a five-membered tin containing ring is significant for their antitumour activities.     

Syntheses and Structural Characterization of Dimethyltin Complexs of N-（3-Methoxysalicylidene）-α-amino Acid

Three new dimethyltin complexes of N-(3-methoxysalicylidene)-α-amino acid,(CH3)2Sn(3-CH3O-2-OC6H3CH=NCHRCOO)(R = H,1;CH3,2;(CH3)2CH,3),have been synthe-sized by treating dimethyltin dichloride with the potassium salt of the ligand and characterized by elemental analysis,IR and 1H NMR spectra.The crystal structure of [(CH3)2Sn(3-CH3O-2-OC6H3CH=NCH2COO)(CH3OH)]2 H2O(1a),formed from methanol solution of 1,has been deter-mined.The crystal belongs to the monoclinic system,space group C/2c with a = 20.636(3),b = 7.8854(9),c = 20.668(2) ,β= 113.265(2)°,V = 3089.7(6) 3,Z = 4,Dc = 1.707 g/cm3,= 1.675 mm-1,F(000) = 1592,R = 0.0301 and wR = 0.0841.In complex 1a,the tin atom is six-coordinate and possesses a distorted [SnC2NO3] octahedral geometry with the two methyl groups occupying the trans positions.The weak Sn O interactions and intermolecular hydrogen bonds connected the molecules into an infinite chain.     

Synthesis and Crystal Structure of Bis[（2,6—pyridinedicar—boxylato）（methanol）dibenzyltion（Ⅳ）]

A novel seven‐coordinate dimer bis[(2,6‐pyridinedicarboxylato)(methanol)dibenzyltin(IV)] was synthesized by the reaction of (PhCH₂)₃SnCl with 2,6‐pyridine dicarboxylic acid in 1:1 molar ratio in methanol solution. The structure was characterized by elemental analysis, IR and ¹H NMR spectra, and the crystal structure was determined by X‐ray single crystal diffraction analysis. The crystal belongs to monoclinic space group P2₁/n, a =0.96250(19) nm, b = 1.0947(2) nm, c = 1.9965(4) nm, β = 92.31(3)°, Z = 2, V = 2.1019(7) nm³, D_c = 1.574 g/cm³, μ = 1.248 mm^?1, F(000)=1000, R₁ = 0.0675, wR₂ = 0.0836. In the crystals of the complex, each tin atom is seven‐coordinated in a distorted bipyramidal structure.     

Synthesis,properties and crystal structural characterization of diorganotin(IV) derivatives of 2‐mercapto‐6‐nitrobenzothiazole

The diorganotin(IV) dichlorides R₂SnCl₂ (R: Ph, PhCH₂ or n‐Bu) react with 2‐mercapto‐6‐nitrobenzothiazole (MNBT) in benzene to give [Ph₂SnCl(MNBT)] ( 1 ), [(PhCH₂)₂Sn(MNBT)₂] ( 2 ) and [(n‐Bu)₂Sn(MNBT)₂] ( 3 ). The three complexes have been characterized by elemental analysis and IR, ¹H, ¹³C and ¹¹⁹Sn NMR spectroscopies. X‐ray studies of the crystal structures of 1 , 2 and 3 show the following. The tin environment for complex 1 is distorted cis‐trigonal bipyramid with chlorine and nitrogen atoms in apical positions. The structure of complex 2 is a distorted octahedron with two benzyl groups in the axial sites. The geometry at the tin atom of complex 3 is that of an irregular octahedron. Interestingly, intra‐molecular non‐bonded Cl…S interactions and S…S interaction were recognized in the crystallographic structures of 1 and 3 respectively. As a result, complex 1 is a polymer and complex 3 is a dimer. Copyright © 2003 John Wiley & Sons, Ltd.     

Syntheses,characterizations, and crystal structures of tri‐ and diorganotin (IV) derivatives with 2‐mercapto‐5‐methyl‐1,3,4‐thiadiazole

A series of organotin(IV) complexes with 2‐mercapto‐5‐methyl‐1,3,4‐thiadiazole (HL) of the type R₃ Sn(L) (R = Me 1 ; Bu 2 ; Ph 3 ; PhCH₂ 4 ) and R₂Sn(L)₂ (R = CH₃ 5 ; Ph 6 ; PhCH₂ 7 ; Bu 8 ) have been synthesized. All complexes 1–8 were characterized by elemental analysis, IR,¹H, ¹³ C, and ¹¹⁹Sn NMR spectra. Among these, complexes 1 , 3 , 4 , and 7 were also determined by X‐ray crystallography. The tin atoms of complexes 1 , 3 , and 4 are all penta‐coordinated and the geometries at tin atoms of complexes 3 and 4 are distorted trigonal–bipyramidal. Interestingly, complex 1 has formed a 1D polymeric chain through Sn and N intermolecular interactions. The tin atom of complex 7 is hexa‐coordinated and its geometry is distorted octahedral. © 2006 Wiley Periodicals, Inc. Heteroatom Chem 17:353–364, 2006; Published online in Wiley InterScience ( www.interscience.wiley.com ). DOI 10.1002/hc.20215     

Coordination polymers based on building blocks of dimethyltin(IV) Chloride iso‐thiocyanate and dimethyltin(IV) di‐iso‐thiocyanate with pyrazine‐2‐carboxylate and 4, 4′‐bipyridine

The reaction of 4,4′‐bipy with dimethyltin(IV) chloride iso‐thiocyanate affords the one‐dimensional (1D) coordination polymer, [Me₂Sn(NCS)Cl·(4,4′‐bipy)]_n ( 1 ), whereas reaction of dimethyltin(IV) dichloride with sodium pyrazine‐2‐carboxylate in the presence of potassium iso‐thiocyanate affords the two‐dimensional (2D) coordination polymer, {[Me₂Sn(C₄H₃N₂COO)₂]₂ [Me₂Sn(NCS)₂]}_n ( 2 ). Both coordination polymers were characterized by elemental analysis and infrared spectroscopy in addition to ¹H and ¹³C NMR spectroscopy of the soluble coordination polymer ( 1 ). A single‐crystal structure determination showed that the asymmetric unit in 1 contains Me₂Sn(NCS)Cl and 4,4′‐bipy moieties and a 1D infinite rigid chain structure forms through bridging of the 4,4′‐bipy ligand between tin atoms and the geometry around the tin atom is a distorted octahedral. Coordination polymer 2 contains two distinct tin atom geometrics in which one tin atom is seven coordinate, and the other is six coordinate. The two tin atom environments are best described as a pentagonal bipyramidal in the former and distorted octahedral in the latter where the carboxylate groups bridge the two tin atoms and construct a 2D‐coordination polymer. The ¹¹⁹Sn NMR spectroscopy indicates the octahedral geometry of 1 retains in solution. © 2011 Wiley Periodicals, Inc. Heteroatom Chem 22:699–706, 2011; View this article online at wileyonlinelibrary.com . DOI 10.1002/.20736     

A Novel Tetranuclear Organotin(IV) Carboxylate with Chain Structure: Synthesis,Crystal Structure,and Characterizations

A new tetranuclear organotin carboxylate {[(n‐Bu₂SnO)₂L]₂}_n (complex 1 ) was synthesized by the reaction of di‐n‐butyltin oxide with (p‐carboxymethoxy‐phenoxy) acetic acid (LH₂) and characterized by elemental analyses: IR, UV–visible, ¹H, ¹³C, ¹¹⁹Sn NMR spectroscopy and single crystal X‐ray study. X‐ray crystallography diffraction data revealed that the complex 1 was polymeric fashion with a chain structure containing a ladder‐like tetranuclear organo‐oxotin cluster. In the complex 1 , the ligand LH₂ is coordinated to the central tin(IV) atoms via the carboxylato‐O atoms. The tetranuclear tin system is formed by the bridges through the carbonyl oxygen atom of the carboxylate moieties and making the tin atom of pentacoordinated in distorted trigonal bipyramidal geometry. Single crystal X‐ray data indicate that the complex 1 crystallized in the cubic system with the space group C₂/c.     

Organotin(IV) complexes derived from proteinogenic amino acid: synthesis,structure and evaluation of larvicidal efficacy on Anopheles stephensi mosquito larvae

Five new organotin(IV) complexes of composition [Bz₂SnL¹]_n ( 1 ), [Bz₃SnL¹H⋅H₂O] ( 2 ), [Me₂SnL²⋅H₂O] ( 3 ), [Me₂SnL³] ( 4 ) and [Bz₃SnL³H]_n ( 5 ) (where L¹ = (2S )‐2‐{[(E )‐(4‐hydroxypentan‐2‐ylidene)]amino}‐4‐methylpentanoate, L² = (rac )‐2‐{[(E )‐1‐(2‐hydroxyphenyl)methylidene]amino}‐4‐methylpentanoate and L³ = (2S )‐ or (rac )‐2‐{[(E )‐1‐(2‐hydroxyphenyl)ethylidene]amino}‐4‐methylpentanoate) were synthesized and characterized using ¹H NMR, ¹³C NMR, ¹¹⁹Sn NMR and infrared spectroscopic techniques. The crystal structure of 2 reveals a distorted trigonal‐bipyramidal geometry around the tin atom where the oxygen atoms of the carboxylate ligand and a water ligand occupy the axial positions, while the three benzyl ligands are located at the equatorial positions. On the other hand, the analogous derivative of enantiopure L³H ( 5 ) consists of polymeric chains, in which the ligand‐bridged tin atoms adopt the same trans ‐Bz₃SnO₂ trigonal‐bipyramidal configuration and are now coordinated to a phenolic oxygen atom instead of H₂O. In 2 , the OH hydrogen of the ketoimine substituent has moved to the nearby nitrogen atom while in the salicylidene derivative 5 , the OH is located almost midway between the phenolic oxygen atom and the nitrogen atom of the CN group. For the dibenzyltin derivative 1 , a polymeric chain structure is observed as a result of a long intermolecular Sn⋅⋅⋅O bond involving the exocyclic carbonyl oxygen atom from the tridentate ligand of a neighbouring tin‐complex unit. The tin atom in this complex has distorted octahedral coordination geometry. In contrast, the racemic dimethyltin(IV) complexes 3 and 4 display discrete monomeric structures with a distorted octahedral‐ and trigonal‐bipyramidal geometry, respectively. The structures show that the coordination mode of the Schiff base ligand depends primarily on the number of bulky benzyl ligands (R) at the tin atom, as indeed found in the structures of related complexes where R = phenyl. With three bulky R groups, the tridentate chelating O,N,O coordination mode is preferred, whereas with fewer or less bulky R ligands, only the carboxylate and hydroxy groups are involved, which leads to polymers. Larvicidal efficacies of two of the new tribenzyltin(IV) complexes ( 2 and 5 ) were assessed on the second larval instar of Anopheles stephensi mosquito larvae and compared with two triphenyltin(IV) analogues, [Ph₃SnL¹H]_n and [Ph₃SnL³H]_n . The results demonstrate that the compounds containing Sn–Ph ligands are more effective than those with Sn–Bz ligands. Copyright © 2016 John Wiley & Sons, Ltd.     

Untersuchungen über Zinn(IV)-alkoxide. I Kristall- und Molekülstruktur des Zinn(IV)-isopropanolat-Isopropanolsolvats,Sn(OiPr)4 · i-PrOH

Investigations into Tin(IV) Alkoxides. I. Crystal and Molecular Structure of Tin(IV)-isopropoxide-Isopropanol Solvate, Sn(OⁱPr)₄ · i-PrOH The isopropanol complex of tin(IV)-isopropoxide has been prepared by the reaction of tin tetrachloride with sodium isopropoxide. The compound forms colourless, moisture sensitive crystals, which in dry air easily release the coordinated solvent molecules. The crystal and molecular structure of Sn(OⁱPr)₄ · i-PrOH has been determinated by single crystal X-ray diffraction. The compound crystallizes in the monoclinic space group P2₁/c with a = 1174.2(5), b = 1428.5(3), c = 1234.1(3) pm, β = 95.37(1)° and Z = 4. The crystal structure consists of discrete, dimeric molecules in which the two tin atoms are bridged by two alkoxide groups. The octahedral coordination sphere of each tin atom is completed by one solvent molecule which, in addition, forms one hydrogen bridge to an alkoxide group of the neighboring tin atom.     

Molecular Structure of Diperchloratotetraphenylporphinatotin(IV)

X-ray diffraction data and NMR spectra of diperchloratotetraphenylporphinatotin(IV), Sn(tpp)(ClO₄)₂ provide evidence for a monodentate perchlorato group coordinated to the Sn(IV) atom. The molecule Sn(tpp)(ClO₄)₂ displays an octahedral coordination geometry for the tin atom and its crystal belongs to the monoclinic space group P2₁/n with a = 11.241(3), b = 14.644(3), c = 12.173(3) Å,β = 111.18(2)°, and Z = 2. The structure was solved by direct method, 3996 unique reflections having I > 3σ(I) measured with an automated diffractometer were used to refine the crystal structure to a conventional R factor 0.0431. The tin(IV) ion is centered on a planar tpp moiety. The geometry at the octahedral coordination centre of the Sn(tpp) (ClO₄)₂ molecule has Sn-O(perchlorate) = 2.181 Å and Sn-N = 2.073 Å.     

Diphenyltin(IV) complexes of the 2-quinolinecarboxaldehyde Schiff bases of S-methyl- and S-benzyldithiocarbazate (Hqaldsme and Hqaldsbz): X-ray crystal structures of Hqaldsme and two conformers of its diphenyltin(IV) complex

New organometallic tin(IV) complexes of the empirical formula Sn(NNS)Ph₂Cl (NNS = anionic forms of the 2-quinolinecarboxaldehyde Schiff bases of S-methyl- and S-benzyldithiocarbazate) have been prepared and characterized by IR, electronic, ¹H NMR and ES mass spectroscopic techniques. The molecular structures of the 2-quinolinecarboxaldehyde Schiff base of S-methyldithiocarbazate (Hqaldsme) and its diphenyltin(IV) complex, Sn(qaldsme)Ph₂Cl, have been determined by X-ray diffraction. In the solid state, the ligand remains as the thione tautomer in which the dithiocarbazate chain adopts an E,E configuration and is almost coplanar with the quinoline ring. The Sn(qaldsme)Ph₂Cl complex crystallizes in two distinctly different conformationally isomeric forms, each having the same space group but different lattice parameters. X-ray analysis shows that in each polymorph, the tin atom adopts a distorted octahedral geometry with the Schiff base coordinated to it as a uninegatively charged tridentate chelating agent via the quinoline nitrogen atom, the azomethine nitrogen atom and the thiolate sulfur atom. The two phenyl groups occupy axial positions and the chloride ligand occupies the sixth coordination position of the tin atom. The deprotonated ligand adopts an E,E,Z configuration in the complex.