Tetrathiometalate complexes of rhodium, iridium, palladium, and platinum. Structures of ((C/sub 5/Me/sub 5/)RhCl)/sup 2/WS/sub 4/ and ((C/sub 3/H/sub 5/)Pd)/sub 2/WS/sub 4/
Journal Article
·
· Inorg. Chem.; (United States)
Synthetic routes to tetrathiometalate complexes of rhodium, iridium, palladium, and platinum are described. Acetonitrile solutions of WS/sub 4//sup 2 -/ reacted with (Rh(diene)Cl)/sub 2/ (where diene = 1,5-cyclooctadiene (COD) or norbornadiene (NBD)), (Ir(COD)Cl)/sub 2/, ((/eta//sup 5/-C/sub 5/Me/sub 5/)RhCl/sub 2/)/sub 2/, and (Pd(allyl)Cl)/sub 2/ to give good yields of ..mu..-WS/sub 4/ complexes (Rh(diene))/sub 2/WS/sub 4/, (Ir(COD))/sub 2/WS/sub 4/, ((/eta//sup 5/-C/sub 5/Me/sub 5/)RhCl)/sub 2/WS/sub 4/, and ((allyl)Pd)/sub 2/, respectively. (COD)PtCl/sub 2/ reacted with MS/sub 4//sup 2 -/ to give (COD)PtMS/sub 4/, M = Mo, W. The later complexes react further with PPh/sub 3/ or WS/sub 4//sup 2 -/ to give (PPh/sub 3/)/sub 2/PtMS/sub 4/ and Pt(WS/sub 4/)/sub 2//sup 2 -/, respectively. (Rh(COD))/sub 2/WS/sub 4/ reacted with t-BuNC to give (Rh(t-BuNC)/sub 2/)/sub 2/WS/sub 4/. RhCl/sub 3/ x 3H/sub 2/O react with WS/sub 4//sup 2 -/ to give the octahedral complexes M(WS/sub 4/)/sub 3//sup 3 -/ isolated as their Et/sub 4/N/sup =/ salts. The /sup 183/W NMR spectrum of (Et/sub 4/N)/sub 3/(Rh(WS/sub 4/)/sub 3/) showed a doublet with J(/sup 183/W,/sup 103/Rh) = 4.8 Hz. Thermal gravimetric analyses of (Rh(COD))/sub w/WS/sub 4/ and (COD)PtWS/sub 4/ indicate that loss of organic coligands and stoichiometric amounts of sulfur occur at moderate temperatures. The compound ((/eta//sup 5/-C/sub 5/Me/sub 5/)RhCl)/sub 2/WS/sub 4/ x CHCl/sub 3/ crystallizes in the orthorhombic space group P2/sub 1/2/sub 1/2/sub 1/ with a = 13.179 (2) /angstrom/, b = 28.725 (7) /angstrom/, c = 8.258 (2) /angstrom/, V = 3126 (2) /angstrom//sup 3/, and Z = 4 and was refined to R = 0.052 and R/sub w/ = 0.059.
- Research Organization:
- Univ. of Illinois, Urbana (USA)
- OSTI ID:
- 6221584
- Journal Information:
- Inorg. Chem.; (United States), Journal Name: Inorg. Chem.; (United States) Vol. 27:20; ISSN INOCA
- Country of Publication:
- United States
- Language:
- English
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Dinuclear cyclopentadienyl carbonyl and alkyne complexes of niobium(II) and tantalum(II). Structures of ((C sub 5 H sub 4 Me)Nb(. mu. -Cl)(CO) sub 2 ) sub 2 , ((C sub 5 H sub 4 Me)Nb(. mu. -Cl)(ArC triple bond CAr)) sub 2 , and ((C sub 5 Me sub 5 )Ta(. mu. -Cl)(CO) sub 2 ) sub 2
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Related Subjects
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400201* -- Chemical & Physicochemical Properties
400202 -- Isotope Effects
Isotope Exchange
& Isotope Separation
ALKENES
CHALCOGENIDES
COMPLEXES
CRYSTAL STRUCTURE
CYCLOALKENES
DATA
DIENES
EXPERIMENTAL DATA
HYDROCARBONS
INFORMATION
IRIDIUM COMPLEXES
NORBORNADIENE
NUMERICAL DATA
ORGANIC COMPOUNDS
PALLADIUM COMPLEXES
PLATINUM COMPLEXES
POLYENES
REFRACTORY METAL COMPOUNDS
RHODIUM COMPLEXES
SULFIDES
SULFUR COMPOUNDS
TRANSITION ELEMENT COMPLEXES
TRANSITION ELEMENT COMPOUNDS
TUNGSTEN COMPOUNDS
TUNGSTEN SULFIDES
400201* -- Chemical & Physicochemical Properties
400202 -- Isotope Effects
Isotope Exchange
& Isotope Separation
ALKENES
CHALCOGENIDES
COMPLEXES
CRYSTAL STRUCTURE
CYCLOALKENES
DATA
DIENES
EXPERIMENTAL DATA
HYDROCARBONS
INFORMATION
IRIDIUM COMPLEXES
NORBORNADIENE
NUMERICAL DATA
ORGANIC COMPOUNDS
PALLADIUM COMPLEXES
PLATINUM COMPLEXES
POLYENES
REFRACTORY METAL COMPOUNDS
RHODIUM COMPLEXES
SULFIDES
SULFUR COMPOUNDS
TRANSITION ELEMENT COMPLEXES
TRANSITION ELEMENT COMPOUNDS
TUNGSTEN COMPOUNDS
TUNGSTEN SULFIDES