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Title: 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]]

Abstract

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.

Authors:
;  [1]
  1. Michigan State Univ., East Lansing (United States)
Publication Date:
OSTI Identifier:
6646380
Resource Type:
Journal Article
Journal Name:
Inorganic Chemistry; (United States)
Additional Journal Information:
Journal Volume: 32:6; Journal ID: ISSN 0020-1669
Country of Publication:
United States
Language:
English
Subject:
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

Citation Formats

Huang, Songping, and Kanatzidis, M G. 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]]. United States: N. p., 1993. Web. doi:10.1021/ic00058a012.
Huang, Songping, & Kanatzidis, M G. 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]]. United States. https://doi.org/10.1021/ic00058a012
Huang, Songping, and Kanatzidis, M G. 1993. "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]]". United States. https://doi.org/10.1021/ic00058a012.
@article{osti_6646380,
title = {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]]},
author = {Huang, Songping and Kanatzidis, M G},
abstractNote = {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.},
doi = {10.1021/ic00058a012},
url = {https://www.osti.gov/biblio/6646380}, journal = {Inorganic Chemistry; (United States)},
issn = {0020-1669},
number = ,
volume = 32:6,
place = {United States},
year = {Wed Mar 17 00:00:00 EST 1993},
month = {Wed Mar 17 00:00:00 EST 1993}
}