In:
Zeitschrift für Naturforschung B, Walter de Gruyter GmbH, Vol. 50, No. 10 ( 1995-10-1), p. 1455-1463
Abstract:
[S(NPMe 3 ) 3 ]Cl · CH 2 C 12 and [S(NPPh 3 ) 3 ]S 4 N 5 were prepared by the reaction of Me 3 SiNPMe 3 or Me 3 SiNPPh 3 with sulfur dichloride and S 3 N 2 Cl 2 , respectively, in CH 2 Cl 2 solutions as colourless, moisture sensitive crystals. The corresponding selenium compound was prepared from SeCl 4 and Me 3 SiNPMe 3 in acetonitrile solution; it crystallizes from toluene solutions with one mole of toluene per formula unit. All complexes have been characterized by IR spectroscopy and by crystal structure determinations. [S(NPMe 3 ) 3 ]Cl-CH 2 Cl 2 : Space group Pna2 1 , Z = 8 , 3930 observed unique reflections, R = 0.033. Lattice dimensions at -120 °C: a = 1200.9(1), b = 1020.2(1), c = 1790.5(1) pm. [S(NPPh 3 ) 3 ]S 4 N 5 : Space group P6 3 , Z = 2, 2586 observed unique reflections, R = 0.054. Lattice dimensions at -100 °C: a = b = 1334.7(2), c = 1652.6(2) pm. [Se(NPMe 3 ) 3 ]Cl · C 7 H 8 : Space group C2/c, Z = 8 , 1475 observed unique reflections, R = 0.059. Lattice dimensions at -40 °C: a = 1853.6(8), b = 1159.2(4), c = 2053.2(4) pm. β = 101.92(3)°. All compounds contain cations [E(NPR 3 ) 3 ] + (E = S, Se) with pyramidal structures. Bond lengths and bond angles are in average: S-N 162.5 pm, S-N-P 120.5° (R = Me), S-N 161.8 pm, S-N-P 119.2° (R = Ph), Se-N 177.8 pm, Se-N-P 120.3°.
Type of Medium:
Online Resource
ISSN:
1865-7117
,
0932-0776
DOI:
10.1515/znb-1995-1005
Language:
English
Publisher:
Walter de Gruyter GmbH
Publication Date:
1995
detail.hit.zdb_id:
2078109-X
detail.hit.zdb_id:
124635-5
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