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Synthesis, Crystal Structure, and IR Investigations of [(NH 3 ) 5 VOV(NH 3 ) 5 ]I 4 · NH 3 and [(NH 3 ) 5 TiOTi(NH 3 ) 5 ]I 4 · NH 3
Author(s) -
Sichla Th.,
Niewa R.,
Zachwieja U.,
Jacobs H.,
Eßmann R.
Publication year - 1996
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.19966221213
Subject(s) - crystallography , crystal structure , octahedron , vanadium , oxygen , transition metal , ammonia , chemistry , hydrogen bond , oxygen atom , metal , x ray crystallography , materials science , molecule , inorganic chemistry , physics , diffraction , biochemistry , organic chemistry , optics , catalysis
The reaction of VI 2 or TiI 3 , respectively, with ammonia in the presence of traces of water or oxygen, respectively, leads to [(NH 3 ) 5 MOM(NH 3 ) 5 ]I 4 · NH 3 with M = V, Ti. Their structures were solved by X‐ray single crystal data: Pbca (No. 61), Z = 4, M = V: a = 12.482(4) Å, b = 14.819(6) Å, c = 13.286(5) Å, N(F o 2⩽ 3σF o 2 ) = 983, N(variables) = 88, R/R w = 0.053/0.063, M = Ti: a = 12.628(4) Å, b = 14.970(4) Å, c = 13.359(3) Å, N(F o 2⩽ 3σF o 2 ) = 1188, N(variables) = 88, R/R w = 0.043/0.047. The structures consist of corner sharing octahedra double units [(NH 3 ) 5 MOM(NH 3 ) 5 ] 4+ with eclipsed conformation which are stacked together according to the motif of a distorted cubic face centered arrangement for the bridging oxygen atoms. IR spectroscopic investigations of the undeuterated vanadium compound and of 5% deuterated samples hint to NH … I hydrogen bridge bonds and to remarkable π‐bonding between the transition metal and the bridging oxygen atoms.