Application of the hydro(solvento)thermal technique to the synthesis of metal carbonyl chalcogenide clusters. 2. Synthesis and x-ray structures of [{Fe4Te4(CO)10}2(Te 2)]2- and [{Fe2Se(CO)6}2(Se2)]2-

Song Ping Huang, Mercouri G Kanatzidis

Research output: Contribution to journalArticle

29 Citations (Scopus)

Abstract

The hydrothermal reaction of Fe(CO)5 with Na2Te2 in the presence of Ph4PCl at 110°C forms (Ph4P)2[{Fe4Te4-(CO) 10}2(Te2)] (I) while the reaction of Fe(CO)5 with Na2Se2 in superheated methanol at 80°C results in (Ph4P)2[{Fe2-Se(CO)6} 2(Se2)] (II). The structures of (I) and (II) were determined by X-ray single-crystal analysis. (I) crystallizes in the space group P1, and (II) in the space group P21/n. The cell parameters are a = 14.930(4) Å, b = 24.070(3) Å, c = 13.045(2) Å, α = 93.19(1)°, β = 113.36(1)°, γ = 76.61(2)°, V = 4183(3) Å3, and Z = 2 at 23°C for (I) and a = 10.561(6) Å, b = 14.021(5) Å, c = 20.46(1) Å, β = 91.89(4)°, V = 3028(2) Å3, and Z = 4 at -100°C for (II). The [{Fe4Te4(CO)10}2(Te 2)]2- anion in (I) forms a ditelluride, Te22-, bridged double cubane-like structure with eight iron atoms in two Fe4Te4 cubes being octahedrally-coordinated by bridging tellurium ligands and terminal CO groups. The [{Fe2Se(CO)6}2(Se2)]2- molecule in (II) adopts a double "butterfly" conformation caused by an intramolecular Se-Se linkage between two Fe2Se2(CO)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) Å, and Fe-Sc = 2.386(17) Å.

Original languageEnglish
Pages (from-to)821-825
Number of pages5
JournalInorganic Chemistry
Volume32
Issue number6
Publication statusPublished - 1993

Fingerprint

Carbon Monoxide
Metals
X rays
synthesis
metals
x rays
iron
cubane
ligands
tellurium
selenium
linkages
Iron
atoms
Tellurium
Ligands
methyl alcohol
Atoms
anions
Selenium

ASJC Scopus subject areas

  • Inorganic Chemistry

Cite this

@article{4141cf932b6a41058a4802a6fe7cc546,
title = "Application of the hydro(solvento)thermal technique to the synthesis of metal carbonyl chalcogenide clusters. 2. Synthesis and x-ray structures of [{Fe4Te4(CO)10}2(Te 2)]2- and [{Fe2Se(CO)6}2(Se2)]2-",
abstract = "The hydrothermal reaction of Fe(CO)5 with Na2Te2 in the presence of Ph4PCl at 110°C forms (Ph4P)2[{Fe4Te4-(CO) 10}2(Te2)] (I) while the reaction of Fe(CO)5 with Na2Se2 in superheated methanol at 80°C results in (Ph4P)2[{Fe2-Se(CO)6} 2(Se2)] (II). The structures of (I) and (II) were determined by X-ray single-crystal analysis. (I) crystallizes in the space group P1, and (II) in the space group P21/n. The cell parameters are a = 14.930(4) {\AA}, b = 24.070(3) {\AA}, c = 13.045(2) {\AA}, α = 93.19(1)°, β = 113.36(1)°, γ = 76.61(2)°, V = 4183(3) {\AA}3, and Z = 2 at 23°C for (I) and a = 10.561(6) {\AA}, b = 14.021(5) {\AA}, c = 20.46(1) {\AA}, β = 91.89(4)°, V = 3028(2) {\AA}3, and Z = 4 at -100°C for (II). The [{Fe4Te4(CO)10}2(Te 2)]2- anion in (I) forms a ditelluride, Te22-, bridged double cubane-like structure with eight iron atoms in two Fe4Te4 cubes being octahedrally-coordinated by bridging tellurium ligands and terminal CO groups. The [{Fe2Se(CO)6}2(Se2)]2- molecule in (II) adopts a double {"}butterfly{"} conformation caused by an intramolecular Se-Se linkage between two Fe2Se2(CO)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) {\AA}, and Fe-Sc = 2.386(17) {\AA}.",
author = "Huang, {Song Ping} and Kanatzidis, {Mercouri G}",
year = "1993",
language = "English",
volume = "32",
pages = "821--825",
journal = "Inorganic Chemistry",
issn = "0020-1669",
publisher = "American Chemical Society",
number = "6",

}

TY - JOUR

T1 - Application of the hydro(solvento)thermal technique to the synthesis of metal carbonyl chalcogenide clusters. 2. Synthesis and x-ray structures of [{Fe4Te4(CO)10}2(Te 2)]2- and [{Fe2Se(CO)6}2(Se2)]2-

AU - Huang, Song Ping

AU - Kanatzidis, Mercouri G

PY - 1993

Y1 - 1993

N2 - The hydrothermal reaction of Fe(CO)5 with Na2Te2 in the presence of Ph4PCl at 110°C forms (Ph4P)2[{Fe4Te4-(CO) 10}2(Te2)] (I) while the reaction of Fe(CO)5 with Na2Se2 in superheated methanol at 80°C results in (Ph4P)2[{Fe2-Se(CO)6} 2(Se2)] (II). The structures of (I) and (II) were determined by X-ray single-crystal analysis. (I) crystallizes in the space group P1, and (II) in the space group P21/n. The cell parameters are a = 14.930(4) Å, b = 24.070(3) Å, c = 13.045(2) Å, α = 93.19(1)°, β = 113.36(1)°, γ = 76.61(2)°, V = 4183(3) Å3, and Z = 2 at 23°C for (I) and a = 10.561(6) Å, b = 14.021(5) Å, c = 20.46(1) Å, β = 91.89(4)°, V = 3028(2) Å3, and Z = 4 at -100°C for (II). The [{Fe4Te4(CO)10}2(Te 2)]2- anion in (I) forms a ditelluride, Te22-, bridged double cubane-like structure with eight iron atoms in two Fe4Te4 cubes being octahedrally-coordinated by bridging tellurium ligands and terminal CO groups. The [{Fe2Se(CO)6}2(Se2)]2- molecule in (II) adopts a double "butterfly" conformation caused by an intramolecular Se-Se linkage between two Fe2Se2(CO)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) Å, and Fe-Sc = 2.386(17) Å.

AB - The hydrothermal reaction of Fe(CO)5 with Na2Te2 in the presence of Ph4PCl at 110°C forms (Ph4P)2[{Fe4Te4-(CO) 10}2(Te2)] (I) while the reaction of Fe(CO)5 with Na2Se2 in superheated methanol at 80°C results in (Ph4P)2[{Fe2-Se(CO)6} 2(Se2)] (II). The structures of (I) and (II) were determined by X-ray single-crystal analysis. (I) crystallizes in the space group P1, and (II) in the space group P21/n. The cell parameters are a = 14.930(4) Å, b = 24.070(3) Å, c = 13.045(2) Å, α = 93.19(1)°, β = 113.36(1)°, γ = 76.61(2)°, V = 4183(3) Å3, and Z = 2 at 23°C for (I) and a = 10.561(6) Å, b = 14.021(5) Å, c = 20.46(1) Å, β = 91.89(4)°, V = 3028(2) Å3, and Z = 4 at -100°C for (II). The [{Fe4Te4(CO)10}2(Te 2)]2- anion in (I) forms a ditelluride, Te22-, bridged double cubane-like structure with eight iron atoms in two Fe4Te4 cubes being octahedrally-coordinated by bridging tellurium ligands and terminal CO groups. The [{Fe2Se(CO)6}2(Se2)]2- molecule in (II) adopts a double "butterfly" conformation caused by an intramolecular Se-Se linkage between two Fe2Se2(CO)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) Å, and Fe-Sc = 2.386(17) Å.

UR - http://www.scopus.com/inward/record.url?scp=0007356850&partnerID=8YFLogxK

UR - http://www.scopus.com/inward/citedby.url?scp=0007356850&partnerID=8YFLogxK

M3 - Article

AN - SCOPUS:0007356850

VL - 32

SP - 821

EP - 825

JO - Inorganic Chemistry

JF - Inorganic Chemistry

SN - 0020-1669

IS - 6

ER -