Preparation of [K][In(Fe[sub 2](CO)[sub 8])[sub 2]](THF) and Fe[sub 2]([mu]-InCl(THF))[sub 2](CO)[sub 8] (THF = Tetrahydrofuran)

Journal Article · Wed Jun 09 04:00:00 EDT 1993 · Inorganic Chemistry; (United States)

DOI:https://doi.org/10.1021/ic00064a021· OSTI ID:6000487

Lin, C C; Kong, G; Cho, H; Whittlesey, B R ^[1]

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1. Texas Tech Univ., Lubbock (United States)

The compound [K][In(Fe[sub 2](CO)[sub 8])[sub 2]](THF) (1) (THF = tetrahydrofauran) has been synthesized by the reaction of Fe[sub 3](CO)[sub 12] with activated indium powder in the presence of potassium chloride. A single-crystal X-ray structure determination shows the iron atoms of two Fe[sub 2](CO)[sub 8] units bound to the indium in a pseudotetrahedral fashion and the potassium ion coordinated to a molecule of THF and two carbonyl oxygen atoms from each of four of the iron-indium anions to give a total coordination number of 9. Crystal data: tetragonal space group P4/n (No. 85), a = 11.8502(2) [angstrom], c = 10.696(2) [angstrom], V = 1502.0(5) [angstrom][sup 3], Z = 2, R = 3.61%, R[sub 2] = 5.04%. The complex Fe[sub 2]([mu]-InCl(THF))[sub 2](CO)[sub 8] (2) can be prepared in high yield by the reaction of either Na[sub 2]Fe(CO)[sub 4] or Na[sub 2]Fe[sub 2](CO)[sub 8] with indium(III) chloride or via the reaction of Fe[sub 3](CO)[sub 12] with indium(I) chloride in tetrahydrofuran. Mechanistic studies suggest that these three reactions produce the same intermediate species, Fe(CO)[sub 4](THF) and InCl, which then combine to give the observed product. Fe[sub 2]([mu]-InCl(THF))[sub 2](CO)[sub 8] forms an adduct with bromide ion in the presence of tetrabutylammonium bromide, and the complex [(C[sub 4]H[sub 9])[sub 4]N][sub 2][Fe[sub 2]([mu]-InClBr)[sub 2](CO)[sub 8]] (3) has been characterized crystallographically. Crystal data: triclinic space group PI (No. 2), a = 11.510(2) [angstrom], b = 11.905(1) [angstrom], c = 12.200(2) [angstrom], [alpha] = 90.373(9)[degrees], [gamma] = 107.75(1)[degrees], V = 1396.6(5) [angstrom][sup 3], Z = 1, R = 4.61%, R[sub 2] = 5.94%.

• OSTI ID: 6000487
• Journal Information: Inorganic Chemistry; (United States), Journal Name: Inorganic Chemistry; (United States) Vol. 32:12; ISSN 0020-1669; ISSN INOCAJ
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400201* -- Chemical & Physicochemical Properties
CARBONYLS
CHEMICAL PREPARATION
CHEMICAL REACTION YIELD
COHERENT SCATTERING
COMPLEXES
CRYSTAL LATTICES
CRYSTAL STRUCTURE
DIFFRACTION
INDIUM COMPLEXES
IRON COMPLEXES
LATTICE PARAMETERS
ORGANIC COMPOUNDS
ORGANOMETALLIC COMPOUNDS
REACTION INTERMEDIATES
SCATTERING
SYNTHESIS
TETRAGONAL LATTICES
TRANSITION ELEMENT COMPLEXES
TRICLINIC LATTICES
X-RAY DIFFRACTION
YIELDS