摘要
将酯基锡 Me O2 CCH2 CH2 Sn Cl3( 1 )与 Schiff碱 ( 2 -HOC6 H4CH NC6 H5) ( 2 )反应合成配合物Me O2 CCH2 CH2 Sn Cl3· ( 2 -HOC6 H4CH NC6 H5) ( 3) ,在其反应混合液放置过程中发生分解生成酯基锡与无机氯离子形成的配合物 Me O2 CCH2 CH2 Sn Cl4- · H+ ( 4)和酯基锡与 Schiff碱的酚氧负离子取代生成的配合物Me O2 CCH2 CH2 Sn Cl2 · ( 2 -OC6 H4CH NC6 H5) ( 5 ) .用元素分析、IR及 NMR对配合物 3,4 ,5进行了表征 ,并对配合物 4的晶体结构进行了解析 .配合物 4为正交晶系 ,空间群 P2 cn,a=0 .785 2 ( 2 ) nm ,b=1 .2 2 36( 1 0 ) nm,c=1 .695 2 ( 4) nm,α=β=γ=90°,V=1 .62 87nm3,Z=4 ,Dc=1 .79g/ cm3,F ( 0 0 0 ) =860 ,μ=2 2 .2 cm- 1 ( Mo) ,R=0 .0 4 49,ωR=0 .0 382 .配合物 4的空间构型为畸变的八面体构型 ,中心锡原子的配位数为 6.配合物 5为 Schiff碱中的酚氧负离子取代配合物 1中的一个氯离子形成的配合物 ,锡原子的配位数为
Complex MeO 2CCH 2CH 2SnCl - 4·H + (4) and MeO 2CCH 2CH 2SnCl 2·(2 OC 6H 4-CHNC 6H 5)(5) were obtained by decomposing the yellow reaction solution of MeO 2CCH 2CH 2SnCl 3· (2 HOC 6H 4CHNC 6H 5) (3), which is the product of β methoxycarbonylethyltin trichlorides(1) with Schiff base (2 HOC 6H 4CHNC 6H 5)(2), after standing for 15 d. Complexes 4 & 5 were characterized by elemental analysis, IR and NMR. The crystal structure of complex 4 was determined by X ray diffraction analysis. The crystal belongs to orthorhombic system, space group P2 cn, a =0.785 2(2) nm, b = 1.223 6(10) nm , c =1.695 2(4) nm, α= β =γ =90°, V = 1.628 7 nm 3, Z =4, D c =1.79 g/cm 3, F (000) = 860, μ =22.2 cm -1 , R=0.044 9, wR =0.038 2 . Complex 4 exists as a discrete molecule, and the tin atom attains a distorted octahedral geometry via the coordination of intramolecular carbonyl oxygen and chloride ion. The coordination number of tin atom is 6. In complex 5, one chloride ion is replaced by the phenolic oxygen anion. Coordination of carbonyl oxygen atom to tin atom still exists, The coordination number of tin atom is 5.
出处
《高等学校化学学报》
SCIE
EI
CAS
CSCD
北大核心
2002年第2期238-242,共5页
Chemical Journal of Chinese Universities
基金
国家自然科学基金 (批准号 :2 9170 0 84)
山东省科委基金 (批准号 :9830 0 0 0 0 1)资助
