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The preparation and crystal structure of trinuclear molybdenum compound (Me 4 N)[Mo 3 (μ 3 ‐O)(μ‐Cl) 3 (μ‐O 2 CH) 3 Cl 3 ]
Author(s) -
Lin XianTi,
Huang JinLing,
Huang JianQuan
Publication year - 1985
Publication title -
acta chimica sinica english edition
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.28
H-Index - 41
eISSN - 1614-7065
pISSN - 0256-7660
DOI - 10.1002/cjoc.19850030402
Subject(s) - chemistry , orthorhombic crystal system , diffractometer , crystal structure , molybdenum , crystallography , ion , bond length , inorganic chemistry , organic chemistry
The title compound was prepared by the oxidation of MoCl 3 in liquid phase. The crystal belongs to the orthorhombic system with space group D 16 2h ‐ Pmnb and unit cell parameters: a = 11.403 (1), b = 12.345 (2), c = 14.292 (2) Å; V = 2011.8 Å 3 ; Z = 4, D c = 2.396g/cm 3 . Altogether 2303 independent reflections were collected on a CAD‐4 four‐circle diffractometer with Mo Kα radiation in range 2° ≤ θ ≤ 27°. The crystal structure was solved by heavy‐atoms method and refined by full‐matrix least‐squares technique to final discrepancy factors R = 0.050 and R w = 0.056 for 1513 reflections of I ≥ 3σ ( I ). The configuration of the cluster anion was characterized to be of the same Ml type structure as presented in the previous paper. The average bond lengths of Mo—Mo and Mo‐(μ 3 ‐O) are 2.577 Å and 1.982 Å respectively. In addition, the effects of bridging atoms, other ligands and bond orders on Mo—Mo bonds are discussed briefly.