Polysulfonylamine. LIII: Triphenylphosphinoxid-Komplexe von Organozinn(IV)-dimesylamiden : Darstellung und Festkörperstrukturen ionischer Komplexe des Typs [R3Sn(OPPh3)2]+[(MeSO2)2N]- und des Molekülkomplexes [Me2Sn{OS(:O, Me)NSO2Me}2(OPPh3)2]
作者： Ilona Lange , Jürgen Krahl , Peter G. Jones , Armand Blaschette
DOI: 10.1016/0022-328X(94)84051-2
关键词: Crystallography 、 Stereochemistry 、 Octahedral molecular geometry 、 Denticity 、 Bond length 、 Triclinic crystal system 、 Monoclinic crystal system 、 X-ray crystallography 、 Crystal structure 、 Triphenylphosphine oxide 、 Chemistry
摘要: Abstract By treating the corresponding organotin dimesylamides with appropriate amounts of triphenylphosphine oxide in dichloromethane or acetonitrile, following novel complexes were obtained: [R3Sn(OPPh3) 2]+[(MeSO2)2N]−, where R = Me (3a) Ph (4); [Me3Sn(OPPh3)2]+ [(MeSO2)2N]−· Ph3PO (3b); [Me2Sn{N(SO2Me)2}2(OPPh3)2] (6). The crystallographic data (at −95°C) are for 3a: triclinic, space group P 1 , a 797.3(2), b 1666.6(4), c 1709.7(5) pm, α 66.22(2), β 86.50(2), γ 89.63(2)°, V 2.0747 nm3 Z 2; 3b: 798.8(2), 1731.7(3), 2061.6(4) 99.14(2), 93.28(2), 92.44(2)°, 2.8609 nm3, 6: monoclinic, P21/c, 1245.2(3), 1591.8(3), 1161.7(2) 99.42(2)°, 2. 2716 As indicated above, 3a, 3b and 4 display ionic crystal structures. In 3b, non-coordinating third molecule resides lattice cavity. structure shows disorder anions could not be satisfactorily refined. tin atom cation has trigonal-bipyramidal geometry axial ligands. Important bond lengths (pm) angles (°) 3a (3b): SnC 210.9–212.1 (210.8–211.5), SnO 223.2 226.1 (221.9 228.4), OP 150.4 151.2 (149.4 coordinating, 148.3 Ph3PO); OSNO 177.3 (175.9), CSNC 118.6–122.0 (119.3–121.4), CSNO 86.6–92.5 (88.6–92.0), SNOP 159.8 (156.5 166.1). centrosymmetric unchanged 6, dimesylamide groups act as monodentate O-ligands, features an all-trans octahedral 209.3, SnO(P) 221.1, SnO(S) 227.4, 150.6 pm; cis- 86.7–93.3, 165.4, SNOS 137.2°.
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