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有机化学
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有机化学 ›› 2003, Vol. 23 ›› Issue (5): 441-446. 上一篇    下一篇

研究论文

3-三氯锡基丙酸酯及其配合物的合成与结构表征

田来进;俞庆森;刘希杰;商志才;王涛;赵文娜   

  1. 浙江大学化学系;曲阜师范大学化学系;中国科学院上海有机化学研究所
  • 发布日期:2003-05-25

Synthesis and Structural Characterization of 3- Trichlorostannylpropionates and Their Complexes

Tian Laijin;Yu Qingsen;Liu Xijie;Shang Zhicai;Wang Tao;Zhao Wenna   

  1. Department of Chemistry,Zhejiang University;department of Chemistry, Qufu Normal University;Shanghai Institute of Organic Chemistry,Chinese Academy of sciences
  • Published:2003-05-25

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被引次数

3

合成了4个新的3-三氯锡基丙酸酯Cl3SnCH2CH2COOR(R=环戊基，1；环己基，2 ；环戊甲基，3；环己甲基，4)，并通过其与二丁基亚砜(L^1)、2，2’-联吡啶 (L^2)、1，10-菲咯啉(L^3)的低热固相反应合成了6个相应的配合物 Cl3SnCH2CH2COOR·L(L=L^1,a;L^2,b;L^3,c).利用元素分析、红外光谱、核磁共振 对其结构进行了表征，并通过X射线单晶衍射测定了1和2的晶体结构，二者均为具 有分子内羰基氧原子配位的畸变三角双锥结构．1属于单斜品系，空间群P21/c, a=0.9842(2)nm,b=1.0923(8)nm,c=1.23948(11)nm,β=93.894(15)°,V=1.3294(4) nm^3,Mr=366.23,Z=4.2属于单斜晶系，空间群P21/c,a=1.04443(9)nm,b=1.04823 (7)nm,c=1.28113(9)nm,β=90.953(8)°,V=1.40239(19)nm^3,Mr=380.25,Z=4.

关键词: 结构表征;有机锡化合物;晶体结构;丙酸酯;抗癌药;联吡啶 P, 二氮杂菲 P;元素分析;红外分光光度法;质子磁共振谱法;XRD

The synthesis and characterization by means of elemental analysis, IR, NMR spectra of 3-trichlorostannylpropionates, Cl3SnCH2CH2COOR (R = cyclopentyl, 1; cyclohexyl, 2; cyclopentylmethyl, 3; cyclohexylmethyl, 4), are described together with their complexes with dibutylsulfoxide (L1). 2,2'-bipyridyl (L ) and 1,10-phenanthroline (L3), Cl3SnCH2CH2COORo L (L= L1, a; L2, b; L3, c), formed by low-heating solid-state reaction. The crystal structures of 1 and 2 show that the tin atom adopts a distorted trigonal bipyramid geometry via intramolecular carbonyl oxygen to tin coordination [the distances of Sn-0 bond are 0.2351(6) ran for 1 and 0.2362(3) nm for 2]]. Compound 1 belongs to monoclinic with space group P2]/c, a = 0.9842(2) nm, b =1. 0923(8) nm, c = 1.23948(11) nm, /? = 93.894(15)°, V= 1.3294(4) ran3, Mr = 366.23, 7 = 4. Compound2 belongs to monoclinic with space group P2{/c, a = 1.04443(9) nm, b = 1.04823(7) nm, c = 1.28113(9) nm, / = 90. 953(8)°, V= 1.40239(19) nm3, Mr = 380.25, Z = 4

Key words: STRUCTURE CHARACTERISTICS;ORGANO TIN COMPOUNDS;CRYSTAL STRUCTURE, PROPIONATE;ANTICARCINOGEN;BIPYRIDINE P;PHENANTHROLINE, ELEMENTAL ANALYSIS;IR;1HNMR;XRD

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