μ-氧-双(三苄基锡)的合成及晶体结构

SYNTHEIS AND CRYSTAL STRUCTURE OF μOXYGENBIS (TRIBENZYLTIN)

用Ｘ－射线衍射方法测定了μ－氧－双（三苄基锡）的晶体结构，该化合物晶体属三方晶系，空间群为Ｒ３，晶体学参数：ａ＝ｂ＝ｃ＝０．９６４６ｎｍ，α＝β＝γ＝８３．９９（１）°，Ｖ＝０．８８４０ｎｍ３，Ｚ＝１，Ｄｘ＝１．５０３ｇ·ｃｍ－３，μ＝１４．４７３ｃｍ－１，Ｆ（０００）＝４０２，Ｒ＝０．０２８。Ｓｎ－Ｏ键长０．１９１６ｎｍ，Ｓｎ－Ｃ键长０．２１６８ｎｍ，Ｓｎ－Ｏ－Ｓｎ键角为１８０．００（０）°，三个Ｏ－Ｓｎ－Ｃ键角在１０８．１６到１０８．２５（９）°之间，Ｓｎ－ＣＨ２－Ｐｈ键角１１０．８°，三个苯环互相垂直，六个苄基以反交叉式构型，分子以氧原子为中心对称，在质谱中Ｓｎ－Ｃ键裂解形成苄基离子基峰。

The structure of μoxygenbis (tribenzyltin) single crystal was determined by Xray diffraction method The crstal belongs to trigonal with space group R3 and cell parameters: a=b=c=09646 nm, α=β=γ=8399(1)°, V=08840 nm3, Z=1, Dx=1503 g·cm-3, μ=14473 cm-1, F(000)=402, final R=0028 for 2288 unique reflection [I≥3σ(I)] The bond lengths of SnO is 01916 nm, all SnC bonds are 02168 nm The bond angles of SnOSn is 18000(0)°, furthermore, all OSnC angles are between 10816 and 10825(9)°, and SnCH2Ph angles are 1108°, benzene ring plane atright angles The six PhCH2 groups are oriented in staggered conformation The structures of the title compound are symmetry on the oxygen atom The base peak is the benzyl ion, that was formed by breaking the SnC bond in the mass spectrum