Premium
Synthesis and Deprotonation of the Branched Triphosphanyltetrasilane PhSi(SiMe 2 PH 2 ) 3
Author(s) -
von Hänisch Carsten,
Feierabend Michael
Publication year - 2013
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/zaac.201200544
Subject(s) - deprotonation , chemistry , nuclear magnetic resonance spectroscopy , spectroscopy , crystallography , infrared spectroscopy , strontium , phosphorus , mass spectrometry , single crystal , stereochemistry , ion , organic chemistry , physics , chromatography , quantum mechanics
Abstract The branched triphosphanyltetrasilane PhSi(SiMe 2 PH 2 ) 3 ( 1 ) could be obtained in a three‐stage synthesis. It was characterised by multi‐nuclear NMR spectroscopy, mass spectrometry and IR spectroscopy. Deprotonation of 1 with Ga i Pr 3 or [M{N(SiMe 3 ) 2 } 2 (thf) 2 ] (M = Ca, Sr, Ba) yields new phosphorus bridged polynuclear complexes of these metals with phosphorus atoms connected through tetrasilane fragments. While trinuclear complexes with single deprotonated phosphanyl groups could be obtained from the reactions of 1 with Ga i Pr 3 , calcium or barium silazanide (compounds 2 , 3 and 5 ), the tetranuclear complex [Sr 4 {PhSi(SiMe 2 PH) 2 (SiMe 2 P)} 2 (dme) 6 ] ( 4 ) was formed in the reaction of 1 with strontium silazanide. In this compound, two of six phosphorus atoms are deprotonated twice. Compounds 2 – 5 were characterised by single‐crystal X‐ray diffraction, elemental analysis as well as IR spectroscopy and as far as possible by NMR spectroscopic techniques.