Application of the hydro(solvo)thermal technique to the synthesis of metal carbonyl chalcogenide clusters Part 3. Synthesis, structural characterization, and spectroscopic studies of the clusters [{M(CO)4}n(MS4)]2- (M Mo, W; n=1, 2)

Song Ping Huang, Mercouri G Kanatzidis

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Abstract

The methanothermal reactions of M(CO)6 (M Mo, W) with Na2S2 gave a series of homonuclear clusters [{M(CO)4}n(MS4)]2- (M=Mo, W; n=1, 2), i.e. (Ph4P)2[(CO)4Mo(MoS4)] (I), (Ph4P)2[(CO)4W(WS4)] (II), (Ph4P)2[(CO)4Mo(MoS4)Mo(CO)4] (III) and (Ph4P)2[(CO)4W(WS4)W(CO)4] (IV). The two dimers, I and II, as well as the two trimers, III and IV, are isostructural to each other, respectively. All compounds crystallize in the triclinic space group P1 with Z=2. The cell dimensions are: a=12.393(8), b=19.303(9), c=11.909(6) Å, α=102.39(5), β=111.54(5), γ=73.61(5)°, V=2522(3) Å3 at T=23 °C for I; a=12.390(3), b=19.314(4), c=11.866(2) Å, α=102.66(2), β=111.49(1), γ=73.40(2)°, V=2511(1) Å3 at T=23 °C for II; a=11.416(3), b=22.524(4), c=10.815(4) Å, α=91.03(2), β=100.57(3), γ=88.96(2)°, V=2733(1) Å3 at T=-100 °C for III, a=11.498(1), b=22.600(4), c=10.864(3) Å, α=90.92(2), β=100.85(1), γ=88.58(1)°, V=2771(2) Å3 at T=23 °C for IV. The dimers are each formed by the coordination of the tetrathiometalate as a bidentate chelating ligand to an M(CO)4 fragment while addition of another M(CO)4 fragment to the dimers results in the trimers. All compounds contain both tetrahedral and octahedral metal centers with the formal 6+ and 0 oxidation states, respectively.

Original languageEnglish
Pages (from-to)9-17
Number of pages9
JournalInorganica Chimica Acta
Volume230
Issue number1-2
DOIs
Publication statusPublished - Mar 1 1995

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Carbon Monoxide
Dimers
Metals
dimers
trimers
synthesis
fragments
metals
Chelation
Ligands
Oxidation
ligands
oxidation
cells
Hot Temperature

ASJC Scopus subject areas

  • Inorganic Chemistry
  • Physical and Theoretical Chemistry
  • Materials Chemistry

Cite this

@article{8db08458281d4c1aac367061ad76fff5,
title = "Application of the hydro(solvo)thermal technique to the synthesis of metal carbonyl chalcogenide clusters Part 3. Synthesis, structural characterization, and spectroscopic studies of the clusters [{M(CO)4}n(MS4)]2- (M Mo, W; n=1, 2)",
abstract = "The methanothermal reactions of M(CO)6 (M Mo, W) with Na2S2 gave a series of homonuclear clusters [{M(CO)4}n(MS4)]2- (M=Mo, W; n=1, 2), i.e. (Ph4P)2[(CO)4Mo(MoS4)] (I), (Ph4P)2[(CO)4W(WS4)] (II), (Ph4P)2[(CO)4Mo(MoS4)Mo(CO)4] (III) and (Ph4P)2[(CO)4W(WS4)W(CO)4] (IV). The two dimers, I and II, as well as the two trimers, III and IV, are isostructural to each other, respectively. All compounds crystallize in the triclinic space group P1 with Z=2. The cell dimensions are: a=12.393(8), b=19.303(9), c=11.909(6) {\AA}, α=102.39(5), β=111.54(5), γ=73.61(5)°, V=2522(3) {\AA}3 at T=23 °C for I; a=12.390(3), b=19.314(4), c=11.866(2) {\AA}, α=102.66(2), β=111.49(1), γ=73.40(2)°, V=2511(1) {\AA}3 at T=23 °C for II; a=11.416(3), b=22.524(4), c=10.815(4) {\AA}, α=91.03(2), β=100.57(3), γ=88.96(2)°, V=2733(1) {\AA}3 at T=-100 °C for III, a=11.498(1), b=22.600(4), c=10.864(3) {\AA}, α=90.92(2), β=100.85(1), γ=88.58(1)°, V=2771(2) {\AA}3 at T=23 °C for IV. The dimers are each formed by the coordination of the tetrathiometalate as a bidentate chelating ligand to an M(CO)4 fragment while addition of another M(CO)4 fragment to the dimers results in the trimers. All compounds contain both tetrahedral and octahedral metal centers with the formal 6+ and 0 oxidation states, respectively.",
author = "Huang, {Song Ping} and Kanatzidis, {Mercouri G}",
year = "1995",
month = "3",
day = "1",
doi = "10.1016/0020-1693(94)04199-6",
language = "English",
volume = "230",
pages = "9--17",
journal = "Inorganica Chimica Acta",
issn = "0020-1693",
publisher = "Elsevier BV",
number = "1-2",

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TY - JOUR

T1 - Application of the hydro(solvo)thermal technique to the synthesis of metal carbonyl chalcogenide clusters Part 3. Synthesis, structural characterization, and spectroscopic studies of the clusters [{M(CO)4}n(MS4)]2- (M Mo, W; n=1, 2)

AU - Huang, Song Ping

AU - Kanatzidis, Mercouri G

PY - 1995/3/1

Y1 - 1995/3/1

N2 - The methanothermal reactions of M(CO)6 (M Mo, W) with Na2S2 gave a series of homonuclear clusters [{M(CO)4}n(MS4)]2- (M=Mo, W; n=1, 2), i.e. (Ph4P)2[(CO)4Mo(MoS4)] (I), (Ph4P)2[(CO)4W(WS4)] (II), (Ph4P)2[(CO)4Mo(MoS4)Mo(CO)4] (III) and (Ph4P)2[(CO)4W(WS4)W(CO)4] (IV). The two dimers, I and II, as well as the two trimers, III and IV, are isostructural to each other, respectively. All compounds crystallize in the triclinic space group P1 with Z=2. The cell dimensions are: a=12.393(8), b=19.303(9), c=11.909(6) Å, α=102.39(5), β=111.54(5), γ=73.61(5)°, V=2522(3) Å3 at T=23 °C for I; a=12.390(3), b=19.314(4), c=11.866(2) Å, α=102.66(2), β=111.49(1), γ=73.40(2)°, V=2511(1) Å3 at T=23 °C for II; a=11.416(3), b=22.524(4), c=10.815(4) Å, α=91.03(2), β=100.57(3), γ=88.96(2)°, V=2733(1) Å3 at T=-100 °C for III, a=11.498(1), b=22.600(4), c=10.864(3) Å, α=90.92(2), β=100.85(1), γ=88.58(1)°, V=2771(2) Å3 at T=23 °C for IV. The dimers are each formed by the coordination of the tetrathiometalate as a bidentate chelating ligand to an M(CO)4 fragment while addition of another M(CO)4 fragment to the dimers results in the trimers. All compounds contain both tetrahedral and octahedral metal centers with the formal 6+ and 0 oxidation states, respectively.

AB - The methanothermal reactions of M(CO)6 (M Mo, W) with Na2S2 gave a series of homonuclear clusters [{M(CO)4}n(MS4)]2- (M=Mo, W; n=1, 2), i.e. (Ph4P)2[(CO)4Mo(MoS4)] (I), (Ph4P)2[(CO)4W(WS4)] (II), (Ph4P)2[(CO)4Mo(MoS4)Mo(CO)4] (III) and (Ph4P)2[(CO)4W(WS4)W(CO)4] (IV). The two dimers, I and II, as well as the two trimers, III and IV, are isostructural to each other, respectively. All compounds crystallize in the triclinic space group P1 with Z=2. The cell dimensions are: a=12.393(8), b=19.303(9), c=11.909(6) Å, α=102.39(5), β=111.54(5), γ=73.61(5)°, V=2522(3) Å3 at T=23 °C for I; a=12.390(3), b=19.314(4), c=11.866(2) Å, α=102.66(2), β=111.49(1), γ=73.40(2)°, V=2511(1) Å3 at T=23 °C for II; a=11.416(3), b=22.524(4), c=10.815(4) Å, α=91.03(2), β=100.57(3), γ=88.96(2)°, V=2733(1) Å3 at T=-100 °C for III, a=11.498(1), b=22.600(4), c=10.864(3) Å, α=90.92(2), β=100.85(1), γ=88.58(1)°, V=2771(2) Å3 at T=23 °C for IV. The dimers are each formed by the coordination of the tetrathiometalate as a bidentate chelating ligand to an M(CO)4 fragment while addition of another M(CO)4 fragment to the dimers results in the trimers. All compounds contain both tetrahedral and octahedral metal centers with the formal 6+ and 0 oxidation states, respectively.

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U2 - 10.1016/0020-1693(94)04199-6

DO - 10.1016/0020-1693(94)04199-6

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EP - 17

JO - Inorganica Chimica Acta

JF - Inorganica Chimica Acta

SN - 0020-1693

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