A new dinuclear molybdenum(V)-sulfur complex containing citrate ligand: Synthesis and characterization of K 2.5Na 2NH 4[Mo 2O 2S 2(cit) 2].5H 2O

Abstract

The complex, K 2.5Na 2NH 4[Mo 2O 2S 2(cit) 2]·5H 2O (1), was obtained by crystallization from a solution of (NH 4) 2MoS 4, potassium citrate (K 3cit) and hydroxyl sodium in methanol and water under an atmosphere of pure nitrogen at ambient temperature. The crystals are triclinic, space group P1¯, a = 7.376 (3)Å, b = 14.620 (2) Å, c = 14.661 (1) Å, α = 71.10 (1)°, β = 81.77 (1)°, γ = 78.27(2)°, R = 0.0584 for 2545 observed (I > 2σ (I)) reflections. Single crystal structure analysis reveals that citrate ligand coordinated to molybdenum atom through two carboxylato oxygens and one deprotonated hydroxyl oxygen together with two bridging sulfur atoms and a terminal oxygen atom completes distorted coordination octahedron around each molybdenum atom. Principal dimensions are Mo = O 1, 1.707 Å (av); Mo-S b, 2.341 Å (av); Mo-O (hydroxyl), 2.021 Å (av); Mo-O (α-carboxyl), 2.1290 Å (av) and Mo-O (β-carboxyl), 2.268(av) Å. IR spectrum is in agreement with the structure.