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Organic‐Inorganic Hybrids based on Polyoxometalates. Part 8 Synthesis and Spectroscopic Characterization of the Heterosilylated Anions [PW 9 O 34 ( t BuSiO) 3 (SiR)] 3‐ (R = ‐CH 3 , ‐CH=CH 2 , ‐CH 2 ‐CH=CH 2 , ‐(CH 2 ) 4 ‐CH=CH 2 ) ‐ X‐ray Crystal Structure of [ n Bu 4 N] 3 [PW 9 O 34 ( t BuSiO) 3 (SiCH 2 ‐CH=CH 2 )]
Author(s) -
Agustin Dominique,
Coelho Cristina,
Mazeaud Agnès,
Herson Patrick,
Proust Anna,
Thouvenot René
Publication year - 2004
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.200400276
Subject(s) - orthorhombic crystal system , chemistry , infrared spectroscopy , crystallography , ion , characterization (materials science) , spectroscopy , crystal structure , materials science , physics , organic chemistry , nanotechnology , quantum mechanics
The reaction of the open‐structure anion [PW 9 O 34 ( t BuSiOH) 3 ] 3‐ with RSiCl 3 (R = (CH 2 ) n CH=CH 2 (n = 0, 1, 4)) affords [PW 9 O 34 ( t BuSiO) 3 (SiR)] 3‐ heterosilylated capped hybrid compounds. These complexes were characterized by infrared spectroscopy and in solution by multinuclear ( 1 H, 29 Si, 31 P and 183 W) NMR. Crystals of [ n Bu 4 N] 3 [PW 9 O 34 ( t BuSiO) 3 Si(CH 2 ‐CH=CH 2 )] are orthorhombic, space group P2 1 2 1 2 1 (N o 19), with lattice constants a = 15.599(2) Å, b = 23.963(5) Å, c = 26.886(1) Å, V = 10.050(3) Å 3 , and Z = 4.