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利用二丁基氧化锡与N ,N 二甲基氨荒酸基乙酸以及N ,N 二乙基氨荒酸基乙酸反应 ,合成了二聚体有机锡化合物{[n Bu2 Sn(O2 CCH2 CS2 NMe2 ) ] 2 O}2 ( 1)和 {[n Bu2 Sn(O2 CCH2 CS2 NEt2 ) ] 2 O}2 ( 2 ) .通过元素分析 ,红外光谱及核磁共振谱对它们进行了表征 .并用X射线单晶衍射法测定了这两个化合物的晶体结构 ,结果表明 :1为单斜晶系 ,C2 /m空间群 ,晶胞参数为 :a =1 3 5 84( 5 )nm ,b =1 92 42 ( 7)nm ,c =1 464 0 ( 5 )nm ,β =10 2 5 0 5 ( 5 )° ,Z =2 ,V =3 73 6( 2 )nm3 ,μ =1 490g/cm3 ,F( 0 0 0 ) =170 4,R1=0 0 492 ,wR2 =0 115 9.2为三斜晶系 ,P1—空间群 ,晶胞参数为 :a =1 1960 ( 14 )nm ,b =1 3 612 ( 16)nm ,c =1 3 684( 16)nm ,α =90 969( 18)° ,β =10 5 2 41( 17)° ,γ =10 3 95 4( 16)° ,Z =1,V =2 0 78( 4 )nm3 ,μ =1 42 9g/cm3 ,F( 0 0 0 ) =916,R1=0 0 45 9,wR2 =0 0 95 7.它们都是以Sn2 O2 四元环为中心对称的二聚体结构 .但锡原子的配位方式不同 ,在 1中 ,内外环锡原子均为五配位的畸变三角双锥构型 ;而在 2中 ,内环锡原子为五配位的畸变三角双锥构型 ,而外环锡原子为六配位的加帽三角双锥构型 .
The reaction of dibutyltin oxide with N, N-dimethylammonioacetic acid and N, N-diethylcarbamoylacetic acid gave the dimeric organotin compound {[n Bu2 Sn (O2 CCH2 CS2 NMe2 )] 2 O} 2 (1) and {[n Bu2 Sn (O2 CCH2 CS2 NEt2)] 2 O} 2 were characterized by elemental analysis, IR and 1H- The crystal structure of the two compounds was determined by the crystal diffraction method. The results show that: 1 is monoclinic, C2 / m space group with unit cell parameters of a = 1 3584 (5) nm and b = 1 92 42 (7) nm, c = 1 464 0 (5) nm, β = 10 2 5 0 5 (5) °, Z = 2, V = 3 73 6 (2) nm 3, μ = 1 490 g / cm 3, F 0 0 0) = 170 4, R1 = 0 0 492, wR2 = 0 115 9.2 is a triclinic, P1-space group with unit cell parameters of a = 1 1960 (14) nm and b = 1 3 612 ( Α = 90 969 (18) °, β = 10 5 2 41 (17) °, γ = 10 3 95 4 (16) °, Z = 1, V = 2 0 78 (4) nm3, μ = 1 429 g / cm3, F (0 0 0) = 916, R1 = 0 0 459, wR2 = 0 0 95 7. All of them are based on the Sn2 O2 quaternary ring being Center symmetrical dimer structure.But the tin atom coordination mode, in 1, the inner and outer ring Atoms are five-coordinate distorted triangular double cone configuration; and in 2, the inner ring tin atom is a five-coordinate distorted triangular double cone configuration, while the outer ring tin atoms hexagonal capped triangular double cone structure .