Xh. Zhou et al., Mobybdenum(VI)-oxygen complex containing citrage ligand: synthesis and characterization of K-6[Mo2O5(cit)(2)]center dot 5H(2)O, SOLID ST SC, 1(4), 1999, pp. 189-198
The complex, K-6[Mo2O5(cit)(2)].5H(2)O was obtained by crystallization from
reaction of [Et4N](3)[Mo2FeS8O2] and potassium citrate (K(3)cit) in methan
ol and water under an atmosphere of pure nitrogen at ambient temperature. T
he complex is triclinic, space group P (1) over bar, a = 11.843(8) Angstrom
, b = 13.717(8) Angstrom, c = 10.287(5) Angstrom, alpha = 108.11(4)degrees,
beta = 99.42(5) (1)degrees, gamma = 66.52(4)degrees, R = 0.034 for 4510 ob
served (I > 3 sigma (I)) reflections. Single crystal structure analysis rev
eals that citrate ligand coordinated to molybdenum atom through two carboxy
lato oxygens and one deprotonated hydroxyl oxygen together with one bridgin
g oxygen atom and two terminal oxygen atoms completes distorted coordinatio
n octahedron around each molybdenum atom. IR spectra are in agreement with
the structure.