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Preparation and structural characterization of ((Ph/sub 3/P)/sub 2/N)(HFeRu/sub 3/(CO)/sub 13/) and ((Ph/sub 3/P)/sub 2/N)(HFe/sub 2/Ru/sub 2/(CO)/sub 13/)

Journal Article · · Inorg. Chem.; (United States)
DOI:https://doi.org/10.1021/ic50225a045· OSTI ID:5949855
 [1]; ; ; ; ; ; ; ;
  1. Brookhaven National Lab., Upton, NY
+ Show Author Affiliations

Reaction of ((Ph/sub 3/P)/sub 2/N) (HFe(CO)/sub 4/) with Ru/sub 3/(CO)/sub 12/ and Fe/sub 2/Ru(CO)/sub 12/ in refluxing THF gives the new clusters ((Ph/sub 3/P)/sub 2/N)(HFeRu/sub 3/(CO)/sub 13/) and ((Ph/sub 3/P)/sub 2/N)(HFe/sub 2/Ru/sub 2/(CO)/sub 13/) in 47% and 4% yields, respectively. ((Ph/sub 3/P)/sub 2/N)-(HFeRu/sub 3/(CO)/sub 13/) has been characterized by its spectroscopic properties and by complete single-crystal x-ray and neutron diffraction studies. ((Ph/sub 3/P)/sub 2/N)(HFeRu/sub 3/(CO)/sub 13/) crystallizes in the space group P1 with Z = 2. Unit cell dimensions from the neutron diffraction study at 15 K are a = 15.053 (2) A, b = 9.073 (1) A, c = 18.992 (3) A, ..cap alpha.. = 104.75 (2)/sup 0/, ..beta.. = 109.58 (2)/sup 0/, and ..gamma.. = 86.95 (2)/sup 0/. The structure was refined to R(F/sup 2/) = 0.052 and R(wF/sup 2/) = 0.057 with measured intensities of 8354 independent reflections. The (HFeRu/sub 3/(CO)/sub 13/)/sup -/ anion has a closed pseudotetrahedral structure with each Ru bearing three terminal carbonyls. Two terminal carbonyls are attached to Fe with two additional carbonyls occupying semibridging positions between Fe and two Ru atoms. The hydride ligand symmetrically bridges one of the Ru-Ru bonds. ((Ph/sub 3/P)/sub 2/N)(HFe/sub 2/Ru/sub 2/(CO)/sub 13/) has also been characterized crystallographically. It crystallizes in the space group P1 with Z=2. The unit cell dimensions at room temperature are a= 14.955 (2) A, b = 18.144 (3) A, c = 9.290 (2) A, ..cap alpha.. = 101.54 (2)/sup 0/, ..beta.. = 95.03 (4)/sup 0/, and ..gamma.. = 84.04 (3)/sup 0/. The structure was solved and refined to R(F) = 0.056 and R(wF) = 0.042 for 5886 independent reflections with I greater than or equal to 3.0sigma(I). The structure of (HFe/sub 2/Ru/sub 2/(CO)/sub 13/)/sup -/ is similar to that of (HFeRu/sub 3/(CO)/sub 13/)/sup -/ except that the anion possesses a full-bridging CO between the two Fe atoms and no semibridging CO's.

OSTI ID:
5949855
Journal Information:
Inorg. Chem.; (United States), Journal Name: Inorg. Chem.; (United States) Vol. 20:11; ISSN INOCA
Country of Publication:
United States
Language:
English

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Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400201* -- Chemical & Physicochemical Properties
400301 -- Organic Chemistry-- Chemical & Physicochemical Properties-- (-1987)
CARBONYLS
COHERENT SCATTERING
COMPLEXES
CRYSTAL LATTICES
CRYSTAL STRUCTURE
DATA
DIFFRACTION
EXPERIMENTAL DATA
INFORMATION
IRON COMPLEXES
LATTICE PARAMETERS
NEUTRON DIFFRACTION
NUMERICAL DATA
ORGANIC COMPOUNDS
ORGANIC NITROGEN COMPOUNDS
ORGANIC PHOSPHORUS COMPOUNDS
RUTHENIUM COMPLEXES
SCATTERING
SYNTHESIS
TRANSITION ELEMENT COMPLEXES
TRICLINIC LATTICES
X-RAY DIFFRACTION