Synthesis and crystal structure of the potassium iminophosphanide [K4(thf)3(Me3SiNPEt2)2(OSiMe2OSiMe2O)]2

被引:6
作者
Chitsaz, S [1 ]
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 | 2003年 / 629卷 / 04期
关键词
iminophosphanide; potassium; crystal structure;
D O I
10.1002/zaac.200390099
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
potassium iminophosphanide complex [K-4(thf)(3)(Me3SiNPEt2)(2)(OSiMe2OSiMe2O)](2) has been obtained by a melt reaction of Me3SiNPEt3 with potassium hydride at 140degreesC in the presence of silicon grease (-OSiMe2-)(n) and subsequent crystallization from thf solution. The colourless moisture sensitive single crystals are characterized by X-ray diffraction: Space group PI, Z = 1, lattice dimensions at -70degreesC: a = 1135.9(3), b = 1250.0(3), c = 1866.1(4) pm, alpha = 92.65(1)degrees, beta = 100.80(1)degrees, gamma = 93.57(1)degrees, R-1 = 0.0604. The centrosymmetric dimeric cluster aggregate is formed by two of the eight potassium ions which are connected with the central oxygen atom of both the (OSiMe2OSiMe2O)(2-) chains as well as with one of their terminal O atoms each. The remaining potassium ions are connected with the phosphorus atoms of the iminophosphanide groups (Me3SiNPEt2)(-) as well as with its nitrogen atoms. They are terminally solvated by thf molecules.
引用
收藏
页码:592 / 594
页数:3
相关论文
共 37 条
  • [11] Kasani A, 1999, ANGEW CHEM INT EDIT, V38, P1483, DOI 10.1002/(SICI)1521-3773(19990517)38:10<1483::AID-ANIE1483>3.0.CO
  • [12] 2-D
  • [13] KASANI A, 1999, ANGEW CHEM, V111, P1580
  • [14] Linti G, 2002, ANGEW CHEM INT EDIT, V41, P4503, DOI 10.1002/1521-3773(20021202)41:23<4503::AID-ANIE4503>3.0.CO
  • [15] 2-5
  • [16] Linti G., 2002, ANGEW CHEM, V114, P4685
  • [17] SOLUTION-STATE, SOLID-STATE, AND CALCULATED STRUCTURES OF AN ALPHA-LITHIATED MONOPHOSPHAZENE
    LOPEZORTIZ, F
    PELAEZARANGO, E
    TEJERINA, B
    PEREZCARRENO, E
    GARCIAGRANDA, S
    [J]. JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1995, 117 (40) : 9972 - 9981
  • [18] TETRAPHOSPHAFULVALENE DIANIONS - ISOELECTRONIC SPECIES OF TETRATHIAFULVALENE DICATIONS
    MAIGROT, N
    RICARD, L
    CHARRIER, C
    MATHEY, F
    [J]. ANGEWANDTE CHEMIE-INTERNATIONAL EDITION IN ENGLISH, 1992, 31 (08): : 1031 - 1032
  • [19] MAIGROT N, 1992, ANGEW CHEM, V104, P1082
  • [20] SOLID-STATE AND SOLUTION STRUCTURES OF SOME LITHIUM-SALTS OF TETRAPHENYLDISILOXANEDIOLATE(2-) AND THE LITHIUM-BRIDGED COMPOUNDS LI2[M(OSIPH2OSIPH2O)3.3PY] (PY = PYRIDINE, M = ZR OR HF)
    MOTEVALLI, M
    SHAH, D
    SULLIVAN, AC
    [J]. JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS, 1993, (18): : 2849 - 2855