//2-Halogenokomplexe von N-Bromsuccinimid und N-Bromphthalimid. Die Kristallstrukturen von PPh4[X(N-Bromsuccinimid)2] und von PPh4[X(N-Bromphthalimid)2] mit X = CI und Br /i2-Halogeno Complexes of N-Bromosuccinimide and N-Bromophthalimide. The Crystal Structures of PPh4 [X(N-Bromosuccinimide)2] and PPh4 [X(N-Bromophthalimide)2] with X = Cl and Br

نویسندگان

  • Mitra Ghassemzadeh
  • Klaus Harms
  • Kurt Dehnicke
  • Dieter Fenske
چکیده

,«2-Halogeno Complexes, N-Bromosuccinimide, N-Bromophthalimide, IR Spectra, Crystal Structure The ,«2-halogeno complexes PPh4[X(N-bromosuccinimide)2] and PPh4[X(N-bromophthalimide)2] with X = Cl and Br have been prepared by reactions of N-bromosuccinimide and N-bromophthalimide, respectively, with the corresponding tetraphenylphosphonium halides PPh4X in acetonitrile solutions. The compounds form pale yellow crystal needles, which were characterized by IR spectroscopy and by crystal structure determinations. PPh4[Cl(N-Bromosuccinimide)2] (1): Space group Z = 4, structure solution with 2516 observed unique reflections, R = 0.040. Lattice dimensions at -25 °C: a = 1775.9(1), b = 764.3(1), c = 2341.7(2) pm, ß = 101.84(1)°. PPh4[Br(N-Bromosuccinimide)2] (2): Space group P2j/n, Z = 4, structure solution with 5620 observed unique reflections, R = 0.061. Lattice dimensions at 20 °C: a = 1776.9(9), b = 762.2(3), c = 2331(1) pm, ß = 103.02(3)°. PPh4[Cl(N-Bromophthalimide)2] (3): Space group P I, Z = 4, structure solution with 3812 observed unique reflections, R = 0.039. Lattice dimensions at -50 °C: a = 918.5(2), b = 1115.0(3), c = 2584.4(5) pm, a = 88.22(3)°, ß = 83.20(3)°, y = 85.10(3)°. PPh4[Br(N-Bromophthalimide)2] (4): Space group P I, Z = 2, structure solution with 3413 observed unique reflections, R = 0.044. Lattice dimensions at -50 °C: a = 1120.2(2), b = 1308.6(3), c = 1343.2(3) pm, a = 105.10(3)°, ß = 104.16(3)°, y = 92.99(3)°. The structures of 1 -4 consist of PPh4+ ions, anions [X(N-bromosuccinimide)2]~ and [X(N-bromophthalimide)2]~, respectively, in which the halide ions X “ are coordinated by the bromine atoms of N-bromosuccinimide and N-bromophthalimide molecules, respectively. The bond angles Br — X --B r are 86.48(5)° for 1, 85.1(1)° for 2, 102.31(6)° and 93.61(6)° for 3, and 91.86(4)° for 4. The bond angles N B r X are nearly linear.

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تاریخ انتشار 2013