Application of the hydro(solvento)thermal technique to the synthesis of metal carbonyl chalcogenide clusters. 2. Synthesis and X-ray structures of [[l brace]Fe[sub 4]Te[sub 4](CO)[sub 10][r brace][sub 2](Te[sub 2])][sup 2[minus]] and [[l brace]Fe[sub 2]Se(CO)[sub 6][r brace][sub 2]Se[sub 2]][sup 2[minus]]

Journal Article · Wed Mar 17 00:00:00 EST 1993 · Inorganic Chemistry; (United States)

DOI:https://doi.org/10.1021/ic00058a012· OSTI ID:6646380

Huang, Songping; Kanatzidis, M G ^[1]

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1. Michigan State Univ., East Lansing (United States)

The hydrothermal reaction of Fe(CO)[sub 5] with Na[sub 2]Te[sub 2] in the presence of Ph[sub 4]PCl at 110[degrees]C forms (Ph[sub 4]P)[sub 2][[l brace]Fe[sub 4]Te[sub 4](CO)[sub 10][r brace][sub 2](Te[sub 2])] (I) while the reaction of Fe(CO)[sub 5] with Na[sub 2]Se[sub 2] in superheated methanol at 80[degrees]C results in (Ph[sub 4]P)[sub 2][[l brace]Fe[sub 2]Se(CO)[sub 6][r brace][sub 2](Se[sub 2])] (II). The structures of (I) and (II) were determined by X-ray single-crystal analysis. (I) crystallizes in the space group P[bar 1], and (II) in the space group P2[sub 1]/n. The [[l brace]Fe[sub 4]Te[sub 4](CO)[sub 10][r brace][sub 2](Te[sub 2])][sup 2[minus]] anion in (I) forms a ditelluride, Te[sub 2][sup 2[minus]], bridged double cubane-like structure with eight iron atoms in two Fe[sub 4]Te[sub 4] cubes being octahedrally-coordinated by briding tellurium ligands and terminal CO groups. The [[l brace]Fe[sub 2]Se(CO)[sub 6][r brace][sub 2](Se[sub 2])][sup 2[minus]] molecule in (II) adopts a double butterfly' conformation caused by an intramolecular Se-Se linkage between two Fe[sub 2]Se[sub 2](CO)[sub 6] units. All iron atoms in this structure have a distorted octahedral geometry achieved by selenium ligands, CO groups, and a Fe-Fe single bond. The average Fe-Te bond distance is 2.619(4) [Angstrom], and Fe-Se = 2.386(17) [Angstrom]. 30 refs., 4 figs., 5 tabs.

• OSTI ID: 6646380
• Journal Information: Inorganic Chemistry; (United States), Vol. 32:6; ISSN 0020-1669
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
CARBONYLS
MOLECULAR STRUCTURE
IRON COMPOUNDS
SELENIUM COMPOUNDS
TELLURIUM COMPOUNDS
ANIONS
CHEMICAL PREPARATION
CRYSTAL STRUCTURE
LATTICE PARAMETERS
X-RAY DIFFRACTION
CHARGED PARTICLES
COHERENT SCATTERING
DIFFRACTION
IONS
SCATTERING
SYNTHESIS
TRANSITION ELEMENT COMPOUNDS
400201* - Chemical & Physicochemical Properties