Synthesis of bimetallic Fe-Ni carbonyl clusters: crystal structure of (N(CH/sub 3/)/sub 3/CH/sub 2/Ph)(Fe/sub 3/Ni(CO)/sub 8/(. mu. -CO)/sub 4/(. mu. /sub 3/-H))
Redox condensation of (Fe/sub 3/(CO)/sub 11/)/sup 2 -/ with Ni(CO)/sub 4/ in tetrahydrofuran affords the tetranuclear dianion (Fe/sub 3/Ni(CO)/sub 12/)/sup 2 -/. Subsequent protonation with acids results in formation of the corresponding (Fe/sub 3/Ni(CO)/sub 12/H)/sup -/ anion. This monoanionic species has also been obtained by reaction of (Fe/sub 3/(CO)/sub 11/)/sup 2 -/ with NiCl/sub 2/.xEtOH. Both Fe/sub 3/Ni systems have been isolated in the solid state in high yield with a variety of tetrasubstituted ammonium and phosphonium salts. An X-ray diffraction study of the trimethylbenzylammonium salt of (Fe/sub 3/Ni(CO)/sup 12/H)/sup -/ reveals a structure with a tetrahedron of metal atoms surrounded by eight terminal and four edge-bridging carbonyl groups. The hydride ligand has been located over the center of an Fe/sub 2/Ni face at a distance of 0.60 (3) A from the trimetal plane. The corresponding (Fe/sub 3/Ni(CO)/sub 12/)/sup 2 -/ dianion is suggested to possess an analogous structure on the basis of its IR spectrum. Crystallographic data for (C/sub 10/H/sub 16/N)/sup +/(C/sub 12/HFe/sub 3/NiO/sub 12/)/sup -/: fw 713.64, triclinic, space group P1, Z = 2, a = 7.416 (1) A, b = 13.849 (2) A, c = 14.108 (2) A, ..cap alpha.. = 103.13 (2)/sup 0/, ..beta.. = 103.14 (2)/sup 0/, ..gamma.. = 99.23 (2)/sup 0/, R(F/sup 2/) = 0.030 for 3860 reflections measured at room temperature. 18 references, 3 figures, 4 tables.
- Research Organization:
- Universita di Milano, Italy
- OSTI ID:
- 5953875
- Journal Information:
- Inorg. Chem.; (United States), Vol. 23:10
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
CARBONYLS
CHEMICAL PREPARATION
CRYSTAL STRUCTURE
IRON COMPOUNDS
NICKEL COMPOUNDS
EXPERIMENTAL DATA
TETRAHYDROFURAN
DATA
FURANS
HETEROCYCLIC COMPOUNDS
INFORMATION
NUMERICAL DATA
ORGANIC COMPOUNDS
ORGANIC OXYGEN COMPOUNDS
SYNTHESIS
TRANSITION ELEMENT COMPOUNDS
400201* - Chemical & Physicochemical Properties
400301 - Organic Chemistry- Chemical & Physicochemical Properties- (-1987)