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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 · · Organometallics; (United States)
DOI:https://doi.org/10.1021/om00160a017· OSTI ID:5926275
; ;  [1]; ;  [2]
  1. Univ. of Michigan, Ann Arbor (United States)
  2. Univ. of Delaware, Newark (United States)
+ Show Author Affiliations
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), Journal Name: Organometallics; (United States) Vol. 9:10; ISSN 0276-7333; ISSN ORGND
Country of Publication:
United States
Language:
English

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Related Subjects

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