Cyclopentadienylniobium and -molybdenum phosphorodithioate complexes. X-ray crystal structures of CpNbCl sub 3 (S sub 2 P(OPr sup i ) sub 2 ), CpNbCl(. mu. -Cl) sub 2 Nb(S sub 2 P(OPr sup i ) sub 2 )Cp, and cis-Cp prime Mo(CO) sub 2 (S sub 2 P(OPr sup i ) sub 2 )

Journal Article · Mon Oct 01 00:00:00 EDT 1990 · Organometallics; (United States)

DOI:https://doi.org/10.1021/om00160a017· OSTI ID:5926275

Woodward, S; Riaz, U; Curtis, M D ^[1]; Haggerty, B S; Rheingold, A L ^[2]

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1. Univ. of Michigan, Ann Arbor (United States)
2. Univ. of Delaware, Newark (United States)

Reaction of CpNbCl{sub 4} (Cp = {eta}-C{sub 5}H{sub 5}) with (Pr{sup i}O){sub 2}P(S)(SH) in the presence of NEt{sub 3} yields CpNbCl{sub 3}(S{sub 2}P(S{sub 2}Pr{sup i}){sub 2}) (1). Reduction of 1 with Na/Hg affords the Nb-Nb-bonded complex CpNbCl({mu}-Cl){sub 2}Nb(S{sub 2}P(OR){sub 2})Cp (2). In refluxing toluene, (Pr{sup i}O){sub 2}P(S)(SH) with (Cp{prime}Mo(CO){sub 3}){sub 2} (Cp{prime} = {eta}-C{sub 5}H{sub 4}Me) gives cis-Cp{prime}Mo(CO){sub 2}(S{sub 2}P(OPr{sup i}){sub 2}) (3). Oxidation of 3 with I{sub 2} affords Cp{prime}MoI{sub 2}(CO)(S{sub 2}P(OPr{sup i}){sub 2}) (4). The crystal structures of 1-3 are compared. For 1, triclinic, P{bar 1}, a = 7.122 (3) {angstrom}, b = 11.365 (4) {angstrom}, c = 12.532 (4) {angstrom}, {alpha} = 77.38 (3){degree}, {beta} = 89.08 (3){degree}, {gamma} = 72.87 (3){degree}, V = 944.5 (8) {angstrom}{sup 3}. For 2, triclinic, P{bar 1}, a = 7.251 (3) {angstrom}, b = 12.386 (5) {angstrom}, c = 13.988 (5) {angstrom}, {alpha} = 102.66 (3){degree}, {beta} = 103.56 (3){degree}, {gamma} = 94.66 (3){degree}, V = 1180.0 (8) {angstrom}{sup 3}, Z = 2. For 3, orthorhombic, Pbca, a = 12.703 (3) {angstrom}, b = 16.707 (4) {angstrom}, c = 18.398 (4) {angstrom}, V = 3904.4 (17) {angstrom}{sup 3}, Z = 8.

• OSTI ID: 5926275
• Journal Information: Organometallics; (United States), Vol. 9:10; ISSN 0276-7333
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
MOLYBDENUM COMPLEXES
CRYSTAL STRUCTURE
NIOBIUM COMPLEXES
AMINES
BOND ANGLE
BOND LENGTHS
CHEMICAL PREPARATION
CHEMICAL REACTIONS
CHEMICAL SHIFT
CYCLOPENTADIENE
INFRARED SPECTRA
LIGANDS
MASS SPECTRA
MOLECULAR STRUCTURE
NITRIC OXIDE
NMR SPECTRA
PHOSPHORUS COMPOUNDS
SULFUR
X-RAY DIFFRACTION
ALKENES
CHALCOGENIDES
COHERENT SCATTERING
COMPLEXES
CYCLOALKENES
DIENES
DIFFRACTION
DIMENSIONS
ELEMENTS
HYDROCARBONS
LENGTH
NITROGEN COMPOUNDS
NITROGEN OXIDES
NONMETALS
ORGANIC COMPOUNDS
OXIDES
OXYGEN COMPOUNDS
POLYENES
SCATTERING
SPECTRA
SYNTHESIS
TRANSITION ELEMENT COMPLEXES
400201* - Chemical & Physicochemical Properties