Mono- and dinitrosyl complexes of molybdenum: Crystal structure of molybdenum dinitrosyl bis(2-picolinate)

• Published in: Polyhedron Vol. 6; no. 7; pp. 1523 - 1532
• Main Authors: Perpiñán, M.F., Ballester, L., Santos, A., Monge, A., Ruiz-Valero, C., Puebla, E.Gutièrrez
• Format: Journal Article
• Language: English
• Published: Oxford Elsevier Ltd 1987; New York, NY Elsevier Science
• Subjects: Carbonyl and nitrosyl compounds, and their complexes; Carbonyl and nitrosyl metals; Chemistry; Condensed matter: structure, mechanical and thermal properties; Exact sciences and technology; Inorganic chemistry and origins of life; Inorganic compounds; Physics; Preparations and properties; Structure of solids and liquids; crystallography; Structure of specific crystalline solids; Transition metal Nitrosyl Complexes; Organic dithiocarbamate; Nitrogen heterocycle; Molybdenum Nitrosyl Complexes; Six membered ring; Organic dithiocarbonate; Preparation; Organic ligand; Chemical decomposition; X ray diffraction; Crystalline structure
• ISSN: 0277-5387
• DOI: 10.1016/S0277-5387(00)80835-9

The reaction of the [Mo(NO) 2] 2+ moiety with the (X,Y)-donor ligands (X,Y = dithiocarbamates, xanthates, 2-picolinate, o-aminophenoxide, o-aminothiophenoxide or dithizone) leads fundamentally to formation of complexes of type Mo(NO) 2(X,Y) 2. Sometimes secondary products are also formed, as for example the mononitrosyl heptacoordinated complex Mo(NO)(2-pic) 3 (5) (2-pic = 2-picolinate). In the reaction with dithizone a complex of composition Mo(NO) 2(HDtz) 2(H 2Dtz) was isolated. The Mo(NO) 2(R 2dtc) 2 (R 2dtc = N, N-dialkyldithiocarbamates) complexes decompose in CHCl 3 or by reaction with CO in CH 2Cl 2 to give the mononitrosyl derivatives Mo(NO)(R 2dtc) 3. The reaction of complex 6 with PPh 3 yields Mo(2-pic) 3·H 2O. The crystal structure of Mo(NO) 2(2-pic) 2 has been determined. The crystals are orthorhombic, space group Pbca with a = 12.502(3), b = 15.15(4), c = 15.296(6) Å, U = 2897(8) Å 3, z = 8, D c = 1.84 g cm −3 μ(Mo- K α) = 9.23 cm −1, F(000) = 1584. The Mo atom presents a distorted octahedral coordination. The atomic parameters have been refined by least-squares analysis of 1845 observed reflexions to R = 0.025.