三(3,5-二甲基苄基)氯化锡和四(间氰基苄基)锡的合成、晶体结构和量子化学研究

以3,5-二甲基苄基氯和间氰基苄基氯在适当的溶剂中与锡粉反应,合成了三(3,5-二甲基苄基)氯化锡(1)和四(间氰基苄基)锡(2),经X射线衍射方法测定了化合物的晶体结构。化合物1属单斜晶系,空间群为P2₁/m,晶体学参数:a=0.584 03(4) nm,b=1.966 37(14) nm,c=0.856 46 (5) nm, β=95.138(3), V=0.979 62(11) nm³,Z=2,D_c=1.735 g·cm^-3,μ(Mo Kα)=14.53 cm^-1,F(000)=524,R₁=0.043 7,wR₂=0.1232。化合物2属单斜晶系,空间群为C2/c,晶体学参数:a=1.692 21(12) nm,b=1.167 41(8) nm,c= 1.539 41(11) nm,β=116.615(10)°,V=2.718 9(3) nm³,Z=4,D_c=1.424 g·cm^-3,μ(Mo Kα)=9.67cm^-1,F(000)=1 176,R₁=0.017 5,wR₂=0.046 1;中心锡原子为畸变四面体构型。对其结构进行量子化学从头计算,探讨了配合物的稳定性、分子轨道能量以及部分前沿分子轨道的组成特征。     

三(3,5-二氟苄基)氯化锡和四(邻氯苄基)锡的合成、晶体结构及量子化学

3,5-二氟苄基氯和邻氯基苄基氯在适当的溶剂中与锡粉反应,合成了三（3,5-二氟苄基）氯化锡（1）和四（邻氯苄基）锡（2）,经X射线衍射方法测定了新化合物的晶体结构。化合物1属单斜晶系,空间群为C2/c,晶体学参数：a=1.858 33（11）nm,b=1.140 98（7）nm,c=2.690 06（16）nm,β=109.288（10）°,V=5.383 6（6）nm³,Z=8,D_c=1.532 g·cm^-3,μ（Mo Kα）=13.61 cm^-1,F（000）=2 480,R₁=0.085 1,wR₂=0.168 1。化合物2属单斜晶系,空间群为P2₁/m,晶体学参数：a=0.585 54（5）nm,b=1.969 74（18）nm,c=0.857 86（8）nm,β=95.204 0（10）°,V=0.985 34（15）nm³,Z=2,D_c=1.805 g·cm^-3,μ（Mo Kα）=14.91 cm^-1,F（000）=524,R₁=0.054 0,wR₂=0.163 9;中心锡原子为畸变四面体构型。对其结构进行量子化学从头计算,探讨了化合物的稳定性、分子轨道能量以及部分前沿分子轨道的组成特征。测定了化合物的热稳定性。     

一维链状μ-氯(氧)-三苄基锡的合成和结构研究

合成了两种具有新型结构的苄基锡化合物：一维链状μ-氯-三苄基锡(1)和一维链状μ-氧-三苄基锡(2)，经X-射线方法测定了化合物的晶体结构。晶体结构(1)属正交晶系，空间群为P2₁2₁2₁，晶体学参数：a=0.855 3(3) nm，b=1.081 4(4) nm，c=1.968 1(7) nm，V=1.820 4(11) nm³，Z=4，D_c=1.560 g·cm^-3，μ(Mo Kα)=15.47 cm^-1，F(000)=856，R₁=0.059 7，wR₂=0.141 5。晶体结构(2)属正交晶 系，空间群为P2₁2₁2₁，晶体学参数：a=1.982 3(4) nm，b=1.089 1(2) nm，c=0.861 1(17) nm，V=1.859 0(6) nm³，Z=4，D_c=1.458 g·cm^-3， μ(Mo Kα)=13.76 cm^-1，F(000)=820，R₁=0.032 7，wR₂=0.064 8。配合物中锡原子均呈五配位畸变三角双锥构型。     

四(邻氟苄基)锡及一维链状三苄基锡二茂铁甲酸酯的合成、结构及性质

合成了四(邻氟苄基)锡(1)和一维链状三苄基锡二茂铁甲酸酯(2),经X射线衍射方法测定了化合物的晶体结构。化合物1属四方晶系,空间群I4₁/a,晶体学参数a=1.96794(16)nm,b=1.96794(16)nm,c=0.59316(5)nm,V=2.2972(3)nm³,Z=4,D_c=1.605g·cm^-3,μ(MoKα)=11.58cm^-1,F(000)=1112,R₁=0.0208,wR₂=0.0576。化合物2属单斜晶系,空间群为P2₁/n,晶体学参数:a=1.59354(12)nm,b=1.00723(8)nm,c=1.70026(13)nm,β=91.001(10)°,V=2.7286(4)nm³,Z=4,D_c=1.521g·cm^-3,μ(MoKα)=14.74cm^-1,F(000)=1256,R₁=0.0384,wR₂=0.0952。晶体的中心锡原子分别呈四配位畸变四面体构型和五配位畸变三角双锥构型。对其结构进行量子化学从头计算,探讨了配合物的稳定性、分子轨道能量以及部分前沿分子轨道的组成特征。测定了配合物的热稳定性和体外抗癌活性。     

水合二(对叔丁基苄基)二氯化锡的合成及晶体结构

The organotin hydration di(p-tert-butylbenzyl)tin dichloride has been synthesized. The crystal structure of complex has been determined by X-ray diffraction. The crystal belongs to orthorhombic space group Pmma with a=1.108 4(2) nm, b=3.492 0(7) nm, c=0.626 36(12) nm, V=2.424 3(8) nm³, Z=4, D_c=1.376 g·cm^-3, μ(Mo Kα)=12.82 cm^-1, F(000)=1 024, R₁=0.085 9, wR=0.225 7. The bond lengths of Sn-Cl are 0.236 0(2) nm and 0.250 8(4) nm, the Sn-C is 0.212 1(11) nm, the Sn-O is 0.233 2(12) nm. The tin rendered five-coordinate in a distorted trigonal bipyramidal configuration. CCDC: 648618.     

四(邻氟苄基)锡及一维链状三苄基锡二茂铁甲酸酯的合成、结构及性质

合成了四(邻氟苄基)锡(1)和一维链状三苄基锡二茂铁甲酸酯(2),经X射线衍射方法测定了化合物的晶体结构.化合物1属为四方晶系,空间群I4₁/a,晶体学参数a=1.967 94(16) nm,b=1.967 94(16) nm,c=0.593 16(5) nm,V=2.297 2(3) nm³,Z=4,D_c=1. 605 g·cm^-3,μ(Mo Kα)=11.58 cm^-1,F(000)=1 112,R₁=0.020 8,wR₂=0.057 6.化合物2属单斜晶系,空间群为P2₁/n,晶体学参数:a=1.593 54(12) nm,b=1.007 23(8) nm,c=1.700 26(13)56 nm,β=91.001(10)°,V=2.728 6(4) nm³,Z=4,D_c=1.521 g·cm^-3,μ(Mo Kα)=14.74 cm^-1,F(000)=1 256,R₁=0.038 4,wR₂=0.095 2.晶体的中心锡原子分别呈四配位畸变四面体构型和五配位畸变三角双锥构型.对其结构进行量子化学从头计算,探讨了配合物的稳定性、分子轨道能量以及部分前沿分子轨道的组成特征.测定了配合物的热稳定性和体外抗癌活性.     

二(o-氟苄基)锡双(四氢吡咯二硫代氨基甲酸酯)和二(p-氯苄基)锡双(二甲基二硫代氨基甲酸酯)的合成、表征及晶体结构

Di(o-fluorbenzyl)tin bis(dithiotetrahydropyrrolcarbamate) (1) and di(p-chlorbenzyl)tin bis(dithiomethylcarbamate) (2) were synthesized. Their structure were characterized by elementary analysis, IR and ¹H NMR and the crystal structure were determined by X-ray single crystal diffraction. The crystal of complex 1 belongs to orthorhombic with space group Pccn, a=2.096 1(12) nm, b=1.018 5(6) nm, c=1.205 9(7) nm, Z=4, V=2.574(2) nm³, D_c=1.624 g·cm^-3, μ(MoKα)=1.348 mm^-1, F(000)=1 272，R₁=0.038 7, wR₂=0.088 5. The crystal of complex 2 belongs to monoclinic with space group C2/c, a=1.531 3(16), b=1.868 4(19), c=0.951 8(10) nm, β=112.602(14)°, Z=4, V=2.514(5) nm³, D_c=1.612 g·cm^-3, μ(MoKα)=1.572 mm^-1, R₁=0.025 4, wR₂=0.070 4. In the complexes 1 and 2, the structures consist of discrete molecules containing six-coordinate tin atom in a distorted octahedron configuration. In crystal of complex 1, molecules are packed in the unit cell in one-dimensional chain structure through a S…S interaction between adjacent molecule. CCDC: 225420, 1; 225421, 2.     

梯形结构二(对甲基苄基)锡氧(氯)簇合物的合成、结构及量子化学研究

二(对甲基苄基)二氯化锡和氢氧化钠溶液反应,合成了梯形结构二(对甲基苄基)锡氧(氯)簇合物,经X-射线衍射测定了其晶体结构。属三斜晶系,空间群为P1,晶体学参数a=0.979 52(16) nm,b=1.313 8(2) nm,c=1.419 5(2) nm,α=62.965(10)°,β=88.551(12)°,γ=73.709(11)°,V=1.550 5(5) nm³,Z=1,D_c=1.563 g·cm^-3,μ(Mo Kα)=17.38 cm^-1,F(000)=727,R=0.024 2,wR=0.057 9。簇合物为由Sn₂O₂构成的平面四元环形成的1个中心内环和2个由Sn₂OCl(O)构成的平面四元外环组成的梯形结构。锡原子均为五配位三角双锥构型。对其结构进行量子化学从头计算,探讨了配合物的稳定性、分子轨道能量以及一些前沿分子轨道的组成特征。     

二苄基锡双(四氢吡咯荒酸酯)的合成、表征和晶体结构

Dibenzyltin bis(dithiotetrahydropyrrolocarbamate) was synthesized by the reaction of dibenzyltin dichloride with dithiotetrahydropyrrolocarbamate. The compound was characterized by elemental analysis, IR, ¹H NMR and MS. and the crystal structure was determined by X-ray single crystal diffraction. The crystal belongs to or-thorhombic with space group Pccn, a=2.1665(6)nm, b=0.9932(3)nm, c=1.1979(3)nm,α=90°,β=90°,γ=90°,Z=2,V=2.5777(12)nm³,D_c=1.529g·cm^-3,μ(MoKα)=1.330mm^-1,F(000)=1208,R₁=0.0341, wR₂=0.0627. In the crystals, the structures consist of discrete molecules in which the tin atom is six-coordinate in a distorted octahedron configuration. CCDC: 179919.     

三邻氯苄基和三邻氟苄基锡吡咯烷氨荒酸酯的合成及晶体结构

Tri(o-chlorbenzyl)tin dithiotetrahydropyrrolocarbamate 1 and tri(o-fluorbenzyl)tin dithiotetrahydropyrrolocar-bamate 2 were synthesized. Their structures were characterized by elementary analysis， IR and ¹H NMR and the crystal structures were determined by X-ray single crystal diffraction. The crystal 1 belongs to triclinic with space group ， a=0.9076(4)nm， b=1.0663(5)nm， c=1.5193(7)nm， α=75.811(6)°，β=89.344(6)°， γ=72.665(6)°， Z=2， V=1.3577(11)nm³， D_c=1.569g·cm^-3， μ=1.406mm^-1， F(000)=644， R=0.0282， wR=0.0617. The crystal 2 belongs to monoclinic with space group P2₁/c， a=1.355(2)nm， b=1.0143(16)nm， c=1.986(3)nm， β=109.94(2)°， Z=4， V=2.565(7)nm³， D_c=1.539g·cm^-3， μ=1.195mm^-1，F(000)=1200， R=0.0467， wR=0.0788. In the crystals of 1 and 2， the structures consist of discrete molecules containing five-coordinate tin atom in a distorted trigonal bipyramidal configuration. CCDC: 1， 213679; 2， 213680.     

二(o-溴苄基)锡双(二乙基二硫代氨基甲酸)酯和二(o-氯苄基)锡双(吡咯啶二硫代氨基甲酸)酯的合成、结构及体外抗癌活性研究

二（o-溴苄基）二溴化锡和二（o-氯苄基）二氯化锡分别与N,N-二乙基二硫代氨基甲酸钠和吡咯啶二硫代氨基甲酸钠反应,合成了二（o-溴苄基）锡双（二乙基二硫代氨基甲酸）酯（1）和二（o-氯苄基）锡双（吡咯啶二硫代氨基甲酸）酯（2）。用X-射线单晶衍射测定了两个化合物的晶体结构,测试结果表明：化合物1的晶体为单斜晶系,空间群P2₁/c,晶体学参数a=1.82736（4）nm,b=0.90060（2）nm,c=1.98841（5）nm,β=114.8780（10）°,V=2.96871（12）nm³,Z=4,D_c=1.690g·cm^-3,μ（MoKα）=38.50cm^-1,F（000）=1496,R₁=0.0516,wR₂=0.1546。化合物2的晶体为单斜晶系,空间群C2/c,晶体学参数a=2.24128（4）nm,b=0.81878（2）nm,c=1.54269（3）nm,β=106.7870（10）°,V=2.71037（10）nm³,Z=4,D_c=1.623g·cm^-3,μ（MoKα）=14.65cm^-1,F（000）=1336,R₁=0.0229,wR₂=0.0565。晶体中锡原子呈六配位畸变八面体构型。对其结构进行量子化学从头计算,探讨了配合物的稳定性、分子轨道能量以及部分前沿分子轨道的组成特征。测定了配合物的热稳定性和体外抗癌活性。     

三(邻溴苄基)溴化锡和四(对溴苄基)锡的合成及结构研究

邻溴苄基溴或对溴苄基溴与锡反应合成三(邻溴苄基)溴化锡(1)和四(对溴苄基)锡(2).经X射线方法测定了新化合物的晶体结构.晶体结构1属斜方六面体晶系,空间群为R-3,晶体学参数:a=1.3389(3) nm, b=1.3389(3) nm, c=2.1896(8) nm, V=3.3993(16) nm3, Z=6, Dx=2.077 Mg·m-3, μ(Mo Kα)=81.83 cm-1, F(000)=2004, R1=0.0477, wR2=0.1372;晶体结构2属正交晶系,空间群为Fdd2,晶体学参数:a=2.1027(7) nm, b=2.3034(8) nm, c=1.1431(4) nm, V=5. 536(3) nm3, Z=8, Dx=1.917 Mg·m-3, μ(Mo Kα)=67.11 cm-1, F(000)=3056, R1=0.0358, wR2=0.0659.化合物1中Sn-C键长为0.2160(8) nm, Sn-Br键长为0.2491(3) nm;化合物2中Sn-C键长分别为0.2175和0.2178 nm.中心锡与亚甲基碳(或溴)原子构成畸型四面体.     

三(邻氟苄基）氯化锡和四(对氟苄基）锡的合成及结构研究

邻氟苄基氯或对氟苄基氯分别与锡反应合成三(邻氟苄基)氯化锡(1)和四(对氟 苄基)锡(2)．经X射线方法测定了新化合物的晶体结构．晶体结构1属单斜晶系，空 间群为P2(1)／n，晶体学参数：a＝0.5896(9)nm,b-1.262(2)nm,c=2.634(4)nm, V=1.959(5)nm^3,Z=4,Dx=1.632g/cm^3,μ（Mo Kα)=14.69cm^-1,F(000)=952, R1=0.0541,wR2=0.1280;晶体结构2属单余晶系，空间群为Cc,晶体学参数：α=1. 0778(6)nm,b=2.3312(14)nm,c=1.0888(7)nm,V=2.460(3)nm^3,Z=4,Dx=1. 499g/cm^2,μ(Mo Kα)=10.82cm^-1,F(000)=1112,R1=0.0302,wR2=0.0590.在化合 物1和2中Sn-C键长分别为0.2136-0.2148和0.2138-0.2180nm,Sn-Cl键长为0.2378 (4)nm,中心锡与亚甲基碳（氯）原子构成畸型四面体。     

二茂铁甲酸(三邻氯苄基)锡配合物的合成、结构和量子化学研究

The novel complex tri(o-chlorobenzyl)tin ferrocenecarboxylate have been synthesized.The crystal structure of the complex has been determined by X-ray diffraction.The crystal belong to orthorhombic with space group Pbca with a=0.1242(5), b=1.7242(7), c=3.0583(13)nm, V=5.928(4)nm³,Z=8, D_c=1.623g·cm^-3,μ(MoKα)= 0.1631cm^-1,F(000)=2896,R₁=0.0461,wR₂=0.0931. The bond lengths of Sn-C is 0.2148(4), 0.2152(6) and 0.2176(5)nm, respectively. The Sn-O is 0.2073(4)nm. The tin atom has a distorted tetrahedral geometry. The study on title complex has been performed,with quantum chemistry calculation by means of G98W package and taking Lanl2dz basis set. The stability of the complex, some frontier molecular orbital energies, the populations of the atomic net charges in complex and composition characteristics of some frontier molecular orbitals have been investigated. CCDC: 184267.