In:
Zeitschrift für Naturforschung B, Walter de Gruyter GmbH, Vol. 42, No. 11 ( 1987-11-1), p. 1391-1397
Abstract:
The reaction of LW(CO) 3 (L = 1,4,7-triazacyclononane) with Br 2 in CHCl 3 yields orange [LW(CO) 3 Br](Br 3 ) which was converted to its BF 4 - salt. [LW(CO) 3 Br]BF 4 crystallizes in the triclinic space group P1̅ (a = 8.273(3), b = 8.628(2), c = 13.034(3) Å , α = 80.10(2), β = 72.69(2), γ = 61.14(2)°, Z = 2); it consists of cations [LW(CO) 3 Br] + , with seven-coordinate W atoms, and BF 4 - anions. The corresponding salt [LW(CO) 3 F](PF 6 ) was obtained from LW(CO) 3 with 20% aqueous HF in the presence of air and addition of NaPF 6 . The analogous reaction with 37% aqueous HCl affords green crystals of [LW(CO) 3 H] 2 [WOCl 5 ]·H 2 O which crystallize in the monoclinic space group P2 1 /c (a = 12.234(4), b = 18.853(7), c = 14.609(5) Å, β = 105.65(3)°, Z = 4). The W atoms in the [LW(CO) 3 H] + cations are seven-coordinate; the six-coordinate [WOCl 5 ] 2- anions are not disordered. The W = O distance is short (1.72(1) Å ), the mean equatorial W-Cl distance is 2.390 Å whereas the W-Cl bond distance trans to the W = O group is 2.562(5) Å.
Type of Medium:
Online Resource
ISSN:
1865-7117
,
0932-0776
DOI:
10.1515/znb-1987-1105
Language:
English
Publisher:
Walter de Gruyter GmbH
Publication Date:
1987
detail.hit.zdb_id:
2078109-X
detail.hit.zdb_id:
124635-5
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