On reactions of hexachlorodiberyllate with trimethylsilyl-N-dimethylamide. crystal structures of (Ph4P)3[Be2Cl5(OSiMe3)][BeCl3(Me2NSiMe3)], (Ph4P[BeCl3(HNMe2)], and (Ph4P)(H2NMe2)[BeCl4]

被引：8
|
作者：
Neumüller, B [1 ]
Dehnicke, K [1 ]
机构：
[1] Univ Marburg, Fachbereich Chem, D-35032 Marburg, Germany
来源：
ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE | 2005年 / 631卷 / 01期
关键词：
beryllium; donor acceptor complexes;
D O I：
10.1002/zaac.200400451
中图分类号：
O61 [无机化学];
学科分类号：
070301 ; 081704 ;
摘要：
Reactions of bis-tetraphenylphosphonium hexachlorodiberyllate, (Ph4P)(2)[Be2Cl6], with trimethylsilyl-N-dimethylamide under different conditions lead to the novel chloroberyllate derivatives (Ph4P)(3)[Be2Cl5(OSiMe3)][BeCl3(Me2NSiMe3)] (1), (Ph4P)[BeCl3-(HNMe2)] (2), and (Ph4P)(H2NMe2)[BeCl4] (3). 1-3 were characterized by IR spectroscopy and crystal structure determinations. 1(.)4CH(2)Cl(2): Space group P (1) over bar, Z = 2, lattice dimensions at 193 K: a = 1115.6(1), b = 2110.7(2), c = 2145.0(3) pm, alpha = 71.38(1)degrees, beta = 85.66(1)degrees, gamma = 85.24(1)degrees, R-1 = 0.0732. The [Be2Cl5(OSiMe3)](2-) ion in the structure of 1 is derived from the [Be2Cl6](2-) ion by substitution of a mu-Cl ligand by the oxygen atom of the (OSiMe3)(-) group. The second anion, [BeCl3(Me2NSiMe3)](-), can be described as donor acceptor complex with a short Be-N bond of 179(1) pm. 2: Space group P (1) over bar, Z = 2, lattice dimensions at 193 K: a = 1063.1(1), b = 1072.0(1), c = 1238.3(1) pm, alpha = 87.55(1)degrees, beta 74.86(1)degrees, gamma = 69.73(1)degrees, R-1 = 0.0299. The anion of 2 forms a centrosymmetric dimer [BeCl3(HNMe2)](2)(2-) via N-(HCl)-Cl-... bridges of the two donor acceptor complex units with Be-N separations of 175.2(2) pm. 3: Space group Pbca, Z = 8, lattice dimensions at 193 K: a = 926.9(1) b = 2164.7(1), c 2732.7(1) pm. R-1 = 0.0495. The structure of 3 contains centrosymmetric ion quadrupoles [(Me2NH2)(BeCl4)](2)(2-) forming by N-(HCI)-C-... bridges between (Me2NH2)(+) and [BeCl4](2-) ions.
引用
收藏
页码：74 / 80
页数：7
相关论文
共 11 条
  • [1] Chloroberyllates with nitrogen donor ligands.: Crystal Structures of (Ph4P)[BeCl3(py)], (Ph4P)2[(BeCl3)2(tmeda)], (Ph4P)[BeCl2{(Me3SiN)2CPh}], and (Ph4P)2[BeCl4] • 2CH2Cl2
    Neumüller, B
    Dehnicke, K
    ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE, 2003, 629 (14): : 2529 - 2534
  • [2] Syntheses, vibrational spectra and crystal structures of the chloroberyllates (Ph4P)2[BeCl4] and (Ph4P)2[Be2Cl6]
    Neumüller, B
    Weller, F
    Dehnicke, K
    ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE, 2003, 629 (12-13): : 2195 - 2199
  • [3] Synthesis and crystal structure of the azido beryllate (Ph4P)2[Be(μ-OSiMe3)(N3)2]2
    Neumueller, Bernhard
    Dehnicke, Kurt
    ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE, 2006, 632 (06): : 931 - 933
  • [4] Crystal structure of (Ph4P)2[Be4Cl4(μ-N3)6]
    Neumüller, B
    Dehnicke, K
    ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE, 2004, 630 (10): : 1374 - 1376
  • [5] (Ph4P)2[Be3(μ-OH)3(H2O)6]Cl5: Crystal Structure and DFT Calculations
    Puchta, Ralph
    Neumueller, Bernhard
    Dehnicke, Kurt
    ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE, 2009, 635 (08): : 1196 - 1199
  • [6] Crystal Structures of the iso-Thiocyanatoberyllates (Ph4P)2[Be(NCS)4] and (Ph4P)4[{Be2(NCS)4(μ-NCS)2}{Be2(NCS)6(μ-H2N2C2S2)}]
    Neumueller, Bernhard
    Dehnicke, Kurt
    ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE, 2010, 636 (07): : 1206 - 1211
  • [7] Synthesis, vibrational spectra, and crystal structure of the disiloxanato-chloroberyllate (Ph4P)2[Be4Cl6(OSiMe2OSiMe2O)2]
    Neumüller, B
    Dehnicke, K
    ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE, 2004, 630 (12): : 1846 - 1850
  • [8] Phosphanimine and phosphoraneiminato complexes of beryllium.: Crystal structures of [BeCl2(HNPPh3)2], [BeCl(HNPPh3)2(Py)]Cl, and [Be3Cl2(NPPh3)4]
    Neumüller, B
    Dehnicke, K
    ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE, 2004, 630 (03): : 369 - 376
  • [9] Azido beryllates with adamantan-like structures:: Synthesis, IR spectra, and crystal structures of (Ph4P)2[Be4X4(μ-N3)6] (X = Cl, Br)
    Neumüller, B
    Dehnicke, K
    ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE, 2004, 630 (03): : 347 - 349
  • [10] (Ph4P)2[Be2F6]•2CH3CN:: Synthesis, IR spectra, crystal structure, and quantum chemical calculations
    Tonner, Ralf
    Frenking, Gernot
    Neumueller, Bernhard
    Dehnicke, Kurt
    ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE, 2007, 633 (08): : 1183 - 1188
12