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1.
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.  相似文献   

2.
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.  相似文献   

3.
The crystal structure of [CoCl ( C7H5N2CH2COPh)4] Br has been determined by means of X-ray crystallography. The molecular structure consists of a discrete [CoCl ( C7H5N2CH2COPh)4] ^ cation and one Br^- anion, in the [CoCl ( C7H5N2CH2COPh)4]^ cation, the coordination geometry of the central Co atom is square-pyramidal with four tertiary N atoms of benzimidazole from four α-( benzimidazol-1-yl) -hypnone ligands in the basal position and one chloride anion in the apical position. In the solid state, [CoCl ( C7H5N2CH2COPh)4]^ and Br^- anion possess intermolecular and intramolecular interactions, which stabilize the crystal structure. The characterization of the title compound were also carried out by using elemeutal analysis, FTIR, UV spectrometries and TG-DSC.  相似文献   

4.
In order to continue our studies on the synthesis, properties and coordination of s-tetrazine, 3,6-di-(pyridin-3-yl)-s-tetrazine (II, 3-dptz) was synthesized and characterized by 1H- NMR, MS and IR spectra. And the coordination reaction of 3-dptz with nitrate of Cu(II) was studied. 3-dptz reacting with CuII salt [Cu(NO3)2·2H2O] generates a new salt, nitrate of 2,5-di-(pyridin-3- yl)-1,3,4-oxadiazolene (III). III was determined by IR spectra and single-crystal X-ray diffraction to give the following crystal data: space group P21/c, a = 4.9112(1), b = 8.4101(3), c = 29.499(1) , β = 93.266(2)o, V = 1216.44(7) nm3, Mr = 287.24, Z = 4, Dc = 1.568 g/cm3,μ= 0.122 mm-1, F(000) = 592, R = 0.0430 and wR = 0.1240. The results show that III is composed of one cation and one nitrate anion. The cation consists of one H+ and one 2,5-di-(pyridin-3-yl)-1,3,4-oxadiazol molecule, with the former being attached to the latter via electrovalent bond with N3 atom. And the O(42) atom in the nitrate anion is disordered. Intra- and intermolecular H-bonds are observed in the crystal of the title compound. The mechanism of metal-assisted decomposition was also discussed briefly.  相似文献   

5.
尹汉东  洪敏  王其宝 《中国化学》2005,23(1):105-108
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.  相似文献   

6.
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.  相似文献   

7.
谢学群  杨春龙  李前进 《结构化学》2007,26(9):1009-1012
The title compound [Mn(DPMT)2Cl2(H2O)2] (DPMT = 1-[[2-(2,4-dichlorophenyl)- 1,3-dioxolan-2-yl]methyl]-1H-1,2,4-triazole) was synthesized by the reaction of MnCl2·4H2O and DPMT in ethanol solution and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c with a = 23.913(4), b = 7.8883(13), c = 8.6291(14) , β = 95.816(3)o, V = 1619.4(5) 3, Z = 2, C24H26Cl6MnN6O6, Mr = 762.15, Dc = 1.563 g/cm3, μ = 0.950 mm-1, S = 1.045, F(000) = 774, R = 0.0462 and wR = 0.0981. The molecular structure is a centrosymmetric conformation, and two ligands are symmetrically located on both sides of the Mn atom. The manganese atom is surrounded by two nitrogen atoms from ligands, two chlorine atoms and two oxygen atoms from water molecules to form a slightly distorted octahedral geometry.  相似文献   

8.
A novel triazole derivative 4-(2-hydrobenzylideneamino)-3-(1,2,4-triazol-4-ylmethyl)-1H-1,2,4-triazole-5(4H)-thione(1) was synthesized and characterized using elemental analysis, FTIR, and 1H NMR, and its crystal structure was determined via X-ray single crystal diffraction analysis. Crystal data: monoclinic, P2(1)/c, a=0.83335(9) nm, b=1.49777(16) nm, c=1.14724(12) nm, β =107.990(2)°, D=1.470 Mg/m3, and Z=4. The geometries and the vibrational frequencies were determined using the density functional theory(DFT) method at the B3LYP/ 6-31G level. To demonstrate the accuracy of the reaction route of compound 1, one of the important intermediates was also tested using the same method. The structural parameters of the two compounds calculated using the DFT study are close to those of the crystals, and the harmonic vibrations of the two compounds computed via the DFT method are in good agreement with those in the observed IR spectral data. The thermodynamic properties of the title compound were calculated, and the compound shows a good structural stability at normal temperature. The test results of biological activities show that it has a certain bactericidal ability.  相似文献   

9.
A penta-coordinated Cu(Ⅱ) complex with 1,4-diazacycloheptane (DACH),[Cu(DACH)2(H2O)]Cl2(1),has been synthesized and characterized by X-ray diffraction,IR spectra,elemental analyses,thermal analyses,UV-Vis and ESR techniques.Complex 1 crystallizes in orthorhombic crystal system,Pbcn space group with a=1.6075(4),b=1.0539(3),c=0.9195(3)nm,V=1.5578(7)nm^3,Mr=352.79,Z=4,Dc=1.487g/cm^3,final R=0.0451 and wR=0.1294.The structure of 1 indicates that the central Cu(Ⅱ) atom is penta-coordinated by four nitrogen aboms of two DACH moieties at the equatorial positions and a water molecule at the axis position.The coordination geometry of Cu(Ⅱ) could be considered as an approximately ideal square-pyramidal environment.Both DACH rings arrange in cis-form and are predominantly in the boat-boat conformation (80%) with some disorder to the chair-chair conformation (20%).The Cl^- anions are hydrogen bonded with the nitrogen donors of the DACH rings and the oxygen donor of the coordinated H2O molecule to form a one-dimensional zigzag linear structure. The solution behaviors of 1 are also discussed in detail by Uvvis and ESR technique.  相似文献   

10.
The crystal and molecular structures of O-ethyl-N-(2,3,4-tri-O-acetyl-p-D-xylopyranosyl)-thiocarbamate were determined by X-ray crystallography. It crystallizes in the orthorhombic system with space group P2(1)2(1)2(1), lattice parameters a=0.90636(18) nm, b=0.94716(19) nm, c=2.1855(4) nm, V=1. 8762 (7) nm3, and Z=4. All the substituents are in equatorial positions. There are four intramolecular interactions, each forming a five-membered ring. The molecules are linked by interactions to form three-dimensional framework. Atoms O6 and O8 show positional disorder.  相似文献   

11.
Synthesis and characterisation of (Z)-1-[2(triphenylstannyl)vinyl]-l-cyclododecanol, c-(CH2)11C(OH)CH=CHSnPh3, are reported, together with its halogenation by I2, Br2 and ICI to yield derivatives of the types c-(CH2)11C(OH)CH=CHSnPhs?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)-l-[2–(triphenylstannyI)vinyl]-l-cyclododecanol, but a trigonal bipyramidal geometry in the monoiodo-derivative (Z)-l-[2]-(diphenyliodo-stannyl)vinyl)-1-cyclododecanol and other derivatives, in which significant intramolecular coordinative interaction HO→Sn ia observed. And the formation of a five-membered tin containing ring is significant for their antitumour activities.  相似文献   

12.
在氮气保护下,1-乙炔茚满醇与三苯基氢化锡进行游离基加成反应,获得加成物(Z)-1-[2-(三苯基锡基)乙烯基]-1-茚满醇(1);将加成物(1)与苯酐反应,得到新型邻苯二甲酸单酯有机锡衍生物(2);衍生物(2)分别与二丁基氧化锡和三苯基氧化锡进行脱水反应,分别获得两个新型邻苯二甲酸酯的有机锡衍生物(3)和(4).将加成物(1)与卤素反应后,与锡原子直接相连的苯基被取代,得到一卤代和二卤代物(5~10).通过元素分析、1HNMR和IR等手段对化合物1~10进行了结构表征,确定了该类邻苯二甲酸单酯和邻苯二甲酸酯的有机锡衍生物的结构.并测定了加成物(1)和一溴代物(6)的晶体结构,在加成物(1)中,由于分子内存在较弱的O→Sn[0.2778(8)nm]配位作用,锡原子呈扭曲三角双锥构型.在一溴代物(6)分子中,存在分子内O→Sn[0.2364(2)nm]配位键,锡原子呈扭曲的三角双锥构型.该系列化合物分子内的O→Sn配位能力和Lewis酸性强弱的顺序为:二卤化物>一卤化物>加成物;氯代物>溴代物>碘代物>加成物.  相似文献   

13.
The Sn atom in the crystal structure of the title compound,catena‐poly­[trimethyl­tin‐μ‐[(2,5‐di­oxo‐2,5‐di­hydro­pyrrol‐1‐yl)­acetato‐O:O′]], [Sn(CH3)3(C6H4NO4)], adopts a distorted trigonal bipyramidal coordination geometry with three methyl groups defining the trigonal plane [mean Sn—C 2.117 (11) Å] and the axial positions occupied by O atoms from different carboxylate groups, with significantly different Sn—O bond lengths [2.207 (5) and 2.358 (6) Å]. The structure forms a polymeric chain of complex molecules linked via carboxylate moieties.  相似文献   

14.
Reaction of 3‐(2‐methoxyphenyl)‐2‐sulfanylpropenoic acid [H2(o‐mpspa)] with SnPh3OH in the presence of di‐isopropylamine resulted in the formation of the complex [HQ][SnPh3(o‐mpspa)] (where HQ = di‐isopropylammonium cation and o‐mpspa = 3‐(2‐methoxyphenyl)‐2‐sulfanylpropenoato), which was characterized by mass spectrometry and vibrational spectroscopy, as well as by 1H, 13C and 119Sn NMR spectroscopy. The single‐crystal X‐ray structural analysis of the new complex shows a trigonal‐bipyramidal coordination geometry around the Sn atom where o‐mpspa behaves as a bidentate chelating ligand. Dimeric units arise from the existence of N? H…O hydrogen bonds between the NH2 group of the di‐isopropylammonium cation and the oxygen atoms of the two neighbouring carboxylato groups. The bacteriostatic activity of the complex is also reported. Copyright © 2007 John Wiley & Sons, Ltd.  相似文献   

15.
Four new complexes, [Ph3Sn(isopropylACDA)] (1), [Ph2SnCl(isopropylACDA)] (2), [Ph3Sn(secbutylACDA)] (3), and [Ph2SnCl(secbutylACDA)] (4), have been prepared from reaction between N-alkylated 2-amino-1-cyclopentene-1-carbodithioic acids (ACDA) with Ph2SnCl2 and Ph3SnCl in 1:1 ratio. All complexes are characterized by FTIR, multinuclear NMR (1H, 13C, and 119Sn) and mass spectrometry. In all complexes, the S–H proton has been removed and coordination takes place through the carbodithioate moiety. The 119Sn NMR data are consistent with five coordination of tin atom in solution. Complexes 2, 3, and 4 have also been confirmed by single X-ray crystallography. All three crystals are triclinic with space group P − 1. In complexes 2 and 4, the geometry around tin atom is distorted trigonal bipyramidal while in 3 the geometry is in between distorted tetrahedral and trigonal bipyramid. In all three structures, ligands are asymmetrically coordinated to tin atom. In addition, crystal structures are further stabilized by N–H···S hydrogen bonding.  相似文献   

16.
The polymeric chains of [Sn(CH3)3(C28H25O3Ge)]n contain trimethyltin moieties bridging two neighboring 3‐(triphenylgermyl)‐3‐o‐methoxypropionate ligands via carboxyl groups. The germanium atom has a distorted tetrahedral geometry and the tin atom has a distorted trigonal‐bipyramidal geometry, the latter with three methyl groups in the equatorial plane and oxygen atoms defining the axial positions. Copyright © 2005 John Wiley & Sons, Ltd.  相似文献   

17.
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.  相似文献   

18.
The crystal structure of catena‐poly­[[tri‐n‐butyl­tin]‐μ‐3‐(1‐naph­thyl­amino­carbonyl)­acrylato‐κ2O1:O3], [Sn(C4H9)3(C14H10NO3)]n, is composed of polymeric chains wherein the metal center exhibits a distorted trigonal‐bipyramidal geometry, with three n‐butyl groups defining the trigonal plane [mean Sn—C 2.133 (7) Å] and the axial positions being occupied by the carboxyl­ate O atoms of two different N‐(1‐naphthyl)­maleamate ligands with inequivalent Sn—O distances [2.167 (4) and 2.457 (4) Å]. The N‐(1‐naphthyl)­maleamate fragment forms an essentially planar seven‐membered ring involving an intramolecular N—H?O hydrogen bond.  相似文献   

19.
The zinc(II) atom in the crystal structure of the title coordination polymer, [Zn(p‐BDOA)·2H2O]n (p‐BDOA2? = benzene‐1,4‐dioxyacetate), exists in a distorted trigonal prismatic geometry. Adjacent zinc(II) ions are linked by the p‐BDOA2? ligands to furnish a one‐dimensional (1‐D) zigzag chain. A three‐dimensional (3‐D) network structure is stabilized by extended hydrogen bonds. Copyright © 2004 John Wiley & Sons, Ltd.  相似文献   

20.
The title compound, [MnSn(C7H7O2S)3(CO)5], is asymmetric but crystallizes in the highly symmetric tetragonal space group I. This is achieved without the need for any disorder, either around the Sn atom or in any of the methyl­sulfonyl groups. The environment around the Sn atom has the following geometry: Sn—Mn = 2.6564 (7) Å, mean Sn—C = 2.175 (5) Å, mean C—Sn—C = 103 (2)° and mean C—Sn—Mn = 115 (6)°. The crystal packing is assisted by weak Sn?O interactions between adjacent columns of mol­ecules, with the resulting geometry at Sn approaching highly distorted trigonal–bipyramidal.  相似文献   

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