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作 者:李忠芳[1] 傅芳信[2] 潘华德[2] 邢彦[3] 林永华[3]
机构地区:[1]山东工程学院科技研究院,淄博255012 [2]东北师范大学化学系,长春130024 [3]中国科学院长春应用化学研究所,长春130022
出 处:《化学学报》1999年第7期820-830,共11页Acta Chimica Sinica
基 金:国家自然科学基金(29170084);山东省科委重大项目资助课题
摘 要:合成表征了32个标题化合物ROCOCHR^1CH_2SnCl_3·(2-HOC_6H_4CH=NC_6H_4-X)(R=Me,Et,n-Bu;R^1=H,Me;X=H,4’-Cl,3’-Br,3’-OH,3’,4’-Cl_2,4’-OMe),通过元素分析,UV-vis,IR和~1H NMR进行了表征n-BuOCOCH_2CH_2SnCl_3·(2-HOC_6H_4CH=NC_6H_4OMe-4’)的晶体结构分析表明,该晶体属单斜晶系,a=1.4661(3)nm,b=0.9307(2)nm,c=1.7888(4)nm,β=94.04(3)°;v=2.4348nm^3,Z=4;空间群P2_1/c.该化合物为含有分子内碳基氧配位,Schiff碱以酚羟基上的氧原子配位,中心锡原子为六配位,空间构型为畸变八面体构型的单分子有机锡化合物.Thirty - two title complexes ROCOCHR1CH2SnCl3 (2 - HOC6H4CH = NC6H4 - X) (R = Me, Et, n - Bu; R1 = H, Me; X = H,4' - Cl, 3' - Br, 3' - OH, 3', 4' - Cl2, 4' - OMe) were synthesized and characterized by elemental analysis , UV - vis , IR , 1 H NMR . The crystal structure of n - BuOCOCH2CH2SnCl3 (2 - HOC6H4CH = NC6H4OMe - 4') were determined by the X-ray diffraction analysis. The crystal belongs to monoclinic system, with a = 1.4661 (3)nm, b =0.9307(2)nm, c = 1.7888(4)nm, β = 94.04(3)°, V = 2.4348nm3, Dc = 1.581mg/m3, Z = 4, F(000) =1160, ,μ = 1.405mm-1, R= 0.0354, Rw = 0.0486. space group: P21/c.The complexes exist as a discrete monomer. The tin atom has a distorted octahedral geometry due to intramolecular coordination of the carbonyl oxygen and the phenolic oxygen of the Schiff base ligands. The coordination number of tin atom is 6.
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