TY - JOUR
T1 - Synthesis and crystal and molecular structure of [(nC4H9)4N]2[MoO2(C5O5)2]; confirmation of exclusively η2-coordination by a croconate ligand
AU - Chen, Qin
AU - Liu, Shuncheng
AU - Zubieta, Jon
N1 - Funding Information:
The research was supported by a grant from the National Science Foundation (CHE8815299).
PY - 1990/9/17
Y1 - 1990/9/17
N2 - The reaction of [(nC4H9)4N]2[Mo2O7] with BaC5O5 in acetonitrile yields red crystals of [(n C4H9)4N]2[MoO2(C5O5)2]. The compound crystallizes in the monoclinic space group C2/c with a=36.502(11), b=14.681(3), c=18.109(5) Å, β=93.84(1)°, V=9682.5(15) Å3, Dcalc=1.22 g cm-3 for Z=8. Structure solution and refinement based on 3593 reflections with Fo≥6σ(Fo) Mo Kα, λ= 0.71073 Å) converged at 0.0693. The structure of the anion consists of a mononuclear Mo(VI) center in ar distorted octahedral environment of the cis-oxo groups and the oxygen donors of two bidentate croconate ligands. The 1,2-chelating geometry of the croconate is unusual in that all previously structurally characterized examples of croconate coordination exhibit additional bonding to a second metal site via the oxygen donor in the 4 position.
AB - The reaction of [(nC4H9)4N]2[Mo2O7] with BaC5O5 in acetonitrile yields red crystals of [(n C4H9)4N]2[MoO2(C5O5)2]. The compound crystallizes in the monoclinic space group C2/c with a=36.502(11), b=14.681(3), c=18.109(5) Å, β=93.84(1)°, V=9682.5(15) Å3, Dcalc=1.22 g cm-3 for Z=8. Structure solution and refinement based on 3593 reflections with Fo≥6σ(Fo) Mo Kα, λ= 0.71073 Å) converged at 0.0693. The structure of the anion consists of a mononuclear Mo(VI) center in ar distorted octahedral environment of the cis-oxo groups and the oxygen donors of two bidentate croconate ligands. The 1,2-chelating geometry of the croconate is unusual in that all previously structurally characterized examples of croconate coordination exhibit additional bonding to a second metal site via the oxygen donor in the 4 position.
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U2 - 10.1016/S0020-1693(00)84832-X
DO - 10.1016/S0020-1693(00)84832-X
M3 - Article
AN - SCOPUS:0000034994
SN - 0020-1693
VL - 175
SP - 241
EP - 245
JO - Inorganica Chimica Acta
JF - Inorganica Chimica Acta
IS - 2
ER -