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Systematic synthesis, solution structural characterization of the square-pyramidal clusters MIr sub 4 (CO) sub 7 (. mu. -CO) sub 2 L(. eta. sup 5 -C sub 5 Me sub 5 )(. mu. sub 4 PPh) (M = Rh, Ir; L = CO, PPh sub 3 ), and X-ray structural determination of the iridium derivatives

Journal Article · · Organometallics; (USA)
DOI:https://doi.org/10.1021/om00117a019· OSTI ID:6438629
; ;  [1]; ;  [2]
  1. Univ. Chemical Laboratory, Cambridge (England)
  2. Universita degli Studi di Bologna (Italy)
+ Show Author Affiliations

The pentanuclear clusters MIr{sub 4}(CO){sub 9}L({eta}{sup 5}-C{sub 5}Me{sub 5})({mu}{sub 4}-PPh) (L = CO, M = Rh (3), Ir (4) and L = PPh{sub 2}Me or PPh{sub 3}, M = Rh (3a) or (3b), Ir (4a) or (4b)) are synthesized in good yields by the reactions of Ir{sub 4}(CO){sub 11}(PPhH{sub 2}) and Ir{sub 4}(CO){sub 10}(PPhH{sub 2})L (L = PPh{sub 2}Me or PPh{sub 3}), respectively, in acetonitrile with (M-({eta}{sup 5}-C{sub 5}Me{sub 5})(NCMe){sub 3})(SbF{sub 6}){sub 2} (M = Rh, Ir) in the presence of 1,8-diazabicyclo(5.4.0)undec-7-ene (DBU). All compounds are characterized by fast-atom bombardment mass spectrometry and a combination of {sup 1}H, {sup 13}C and {sup 31}P NMR. Crystal data for 4: space group P{bar 1}, a = 14.511 (5), b = 15.366 (8), c = 13.962 (2) {angstrom}, {alpha} = 89.99 (3), {beta} = 93.94 (2), {gamma} = 86.15 (3){degree}, Z = 4. Crystal data for 4b: space group P2{sub 1}/a, a = 17.949 (2), b = 9.998 (4), c = 25.606 (5) {angstrom}, {beta} = 108.94 (1){degree}, Z = 4. The solution structures of 3, 4, 3b, and 4b were determined by low-temperature {sup 13}C NMR and are fully consistent with the solid-state structures.

OSTI ID:
6438629
Journal Information:
Organometallics; (USA), Journal Name: Organometallics; (USA) Vol. 9:3; 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
COMPLEXES
CRYSTAL STRUCTURE
DATA
DATA ANALYSIS
EXPERIMENTAL DATA
INFORMATION
IRIDIUM COMPLEXES
MEASURING INSTRUMENTS
MEASURING METHODS
NUMERICAL DATA
ORGANIC COMPOUNDS
ORGANOMETALLIC COMPOUNDS
RHODIUM COMPLEXES
SYNTHESIS
TRANSITION ELEMENT COMPLEXES