Synthesis and coordination chemistry of (carbamoylmethyl)thiophosphonates. Crystal and molecular structure of cis-dioxodichlorobis(diethyl((diethylcarbamoyl)methyl)thiophosphonate)molybdenum(VI)

Journal Article · Wed Jul 15 04:00:00 EDT 1987 · Inorg. Chem.; (United States)

DOI:https://doi.org/10.1021/ic00261a026· OSTI ID:5521894

McCabe, D J; Duesler, E N; Paine, R T

Bifunctional (carbamoylmethyl)thiophosphonates, (RO)/sub 2/P(S)CH/sub 2/C(O)NEt/sub 2/ (R = Et, Bu), have been prepared and characterized by elemental analysis and mass, infrared, and NMR spectroscopy. The coordination chemistry of one ligand (R = Et) with molybdenyl, lanthanide, and uranyl ions has been surveyed. cis-Dioxodichlorobis(diethyl((diethylcarbamoyl)methyl)thiophosphonated)molybdenum(VI), MoO/sub 2/Cl/sub 2/((C/sub 7/H/sub 5/O)/sub 2/P(S)CH/sub 2/C(O)N(C/sub 2/H/sub 5/)/sub 2/)/sub 2/ has been isolated from the combination of MoO/sub 2/Cl/sub 2/ and the thiophosphonate ligand in ethanol/ether mixtures. The resulting complex has been characterized by elemental analyses, infrared and /sup 31/P and /sup 13/C NMR spectroscopy, and single-crystal X-ray diffraction analysis. The crystal parameters are reported. The structure was solved by heavy-atom methods, and blocked least-squares refinements converged at R/sub F/ = 5.6% and R/sub wF/ = 5.9% on 2670 unique reflections with F greater than or equal to 5sigma(F). The structure contains monomeric units of the complex with the six-coordinate Mo atom having a pseudooctohedral coordination geometry. The two (carbamoylmethyl)thiophosphonate ligands are bonded to the Mo atom in a monodentate mode through the carbonyl oxygen atoms. The important bond distances were measured and are reported. 29 references, 1 figure, 3 tables.

• Research Organization: Univ. of New Mexico, Albuquerque
• OSTI ID: 5521894
• Journal Information: Inorg. Chem.; (United States), Journal Name: Inorg. Chem.; (United States) Vol. 26:14; ISSN INOCA
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEAR CHEMISTRY
400201 -- Chemical & Physicochemical Properties
400702* -- Radiochemistry & Nuclear Chemistry-- Properties of Radioactive Materials
ACTINIDE COMPLEXES
CARBONYLS
CHLORINE COMPOUNDS
COMPLEXES
CRYSTAL STRUCTURE
DATA
EXPERIMENTAL DATA
HALOGEN COMPOUNDS
INFORMATION
MOLECULAR STRUCTURE
MOLYBDENUM COMPOUNDS
NUMERICAL DATA
ORGANIC COMPOUNDS
ORGANIC PHOSPHORUS COMPOUNDS
ORGANOMETALLIC COMPOUNDS
RARE EARTH COMPLEXES
REFRACTORY METAL COMPOUNDS
SYNTHESIS
TRANSITION ELEMENT COMPOUNDS
URANIUM COMPLEXES
URANYL COMPLEXES