Crystal structure determination of bis(tetraphenylphosphonium) heptasulfide, (Ph4P)2S7

Mercouri G Kanatzidis, N. C. Baenziger, D. Coucouvanis

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Abstract

The S72- anion has been obtained by the reaction of MoS92- with an excess of the sodium salt of the diethyldithiocarbamate anion in acetonitrile solution. The tetraphenylphosphonium salt of S72-, (Ph4P)2S7 (I), crystallizes in the triclinic space group P1 with Z = 2 and lattice parameters a = 11.041 (3) Å, b = 18.589 (4) Å, c = 12.040 (3) Å, α = 74.58 (3)°, β = 69.05 (3)°, γ = 87.76 (4)°, and V = 2220.18 Å3. Diffraction data (Mo Kα radiation, 2θmax = 50°) were collected with a Picker FACS-I automated diffractometer, and the structure was solved and refined by direct methods and full-matrix least-squares procedures to RF = 5.8% and RwF = 8.7% with use of 5102 unique reflections. The S72- ion is found to be a right-handed nonbranched S(1)S(2)S(3)S(4)S(5)S(6)S(7) helix with very short terminal sulfur-sulfur bonds of 1.990 (2) and 1.995 (2) Å for S(1)-S(2) and S(6)-S(7), respectively. The internal bond distances are as follows (in Å): S(2)-S(3), 2.036 (2); S(3)-S(4), 2.062 (2); S(4)-S(5), 2.062 (2); S(5)-S(6), 2.037 (2). The torsion angles in the chain are as follows (in degrees): S(2)-S(3), 73.28 (10)°; S(3)-S(4), 74.41 (10)°; S(4)-S(5), 65.22 (10)°; S(5)-S(6), 79.86 (10)°. The (Ph4P)2S7 salt dissolves in polar solvents to give blue solutions with adsorption bands at 610, 470, 345 (sh), and 304 nm.

Original languageEnglish
Pages (from-to)290-292
Number of pages3
JournalInorganic Chemistry
Volume22
Issue number2
Publication statusPublished - 1983

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Salts
Crystal structure
salts
Sulfur
crystal structure
Anions
sulfur
anions
Ditiocarb
Diffractometers
diffractometers
Torsional stress
helices
Lattice constants
acetonitrile
torsion
lattice parameters
Diffraction
Sodium
sodium

ASJC Scopus subject areas

  • Inorganic Chemistry

Cite this

Crystal structure determination of bis(tetraphenylphosphonium) heptasulfide, (Ph4P)2S7. / Kanatzidis, Mercouri G; Baenziger, N. C.; Coucouvanis, D.

In: Inorganic Chemistry, Vol. 22, No. 2, 1983, p. 290-292.

Research output: Contribution to journalArticle

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title = "Crystal structure determination of bis(tetraphenylphosphonium) heptasulfide, (Ph4P)2S7",
abstract = "The S72- anion has been obtained by the reaction of MoS92- with an excess of the sodium salt of the diethyldithiocarbamate anion in acetonitrile solution. The tetraphenylphosphonium salt of S72-, (Ph4P)2S7 (I), crystallizes in the triclinic space group P1 with Z = 2 and lattice parameters a = 11.041 (3) {\AA}, b = 18.589 (4) {\AA}, c = 12.040 (3) {\AA}, α = 74.58 (3)°, β = 69.05 (3)°, γ = 87.76 (4)°, and V = 2220.18 {\AA}3. Diffraction data (Mo Kα radiation, 2θmax = 50°) were collected with a Picker FACS-I automated diffractometer, and the structure was solved and refined by direct methods and full-matrix least-squares procedures to RF = 5.8{\%} and RwF = 8.7{\%} with use of 5102 unique reflections. The S72- ion is found to be a right-handed nonbranched S(1)S(2)S(3)S(4)S(5)S(6)S(7) helix with very short terminal sulfur-sulfur bonds of 1.990 (2) and 1.995 (2) {\AA} for S(1)-S(2) and S(6)-S(7), respectively. The internal bond distances are as follows (in {\AA}): S(2)-S(3), 2.036 (2); S(3)-S(4), 2.062 (2); S(4)-S(5), 2.062 (2); S(5)-S(6), 2.037 (2). The torsion angles in the chain are as follows (in degrees): S(2)-S(3), 73.28 (10)°; S(3)-S(4), 74.41 (10)°; S(4)-S(5), 65.22 (10)°; S(5)-S(6), 79.86 (10)°. The (Ph4P)2S7 salt dissolves in polar solvents to give blue solutions with adsorption bands at 610, 470, 345 (sh), and 304 nm.",
author = "Kanatzidis, {Mercouri G} and Baenziger, {N. C.} and D. Coucouvanis",
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T1 - Crystal structure determination of bis(tetraphenylphosphonium) heptasulfide, (Ph4P)2S7

AU - Kanatzidis, Mercouri G

AU - Baenziger, N. C.

AU - Coucouvanis, D.

PY - 1983

Y1 - 1983

N2 - The S72- anion has been obtained by the reaction of MoS92- with an excess of the sodium salt of the diethyldithiocarbamate anion in acetonitrile solution. The tetraphenylphosphonium salt of S72-, (Ph4P)2S7 (I), crystallizes in the triclinic space group P1 with Z = 2 and lattice parameters a = 11.041 (3) Å, b = 18.589 (4) Å, c = 12.040 (3) Å, α = 74.58 (3)°, β = 69.05 (3)°, γ = 87.76 (4)°, and V = 2220.18 Å3. Diffraction data (Mo Kα radiation, 2θmax = 50°) were collected with a Picker FACS-I automated diffractometer, and the structure was solved and refined by direct methods and full-matrix least-squares procedures to RF = 5.8% and RwF = 8.7% with use of 5102 unique reflections. The S72- ion is found to be a right-handed nonbranched S(1)S(2)S(3)S(4)S(5)S(6)S(7) helix with very short terminal sulfur-sulfur bonds of 1.990 (2) and 1.995 (2) Å for S(1)-S(2) and S(6)-S(7), respectively. The internal bond distances are as follows (in Å): S(2)-S(3), 2.036 (2); S(3)-S(4), 2.062 (2); S(4)-S(5), 2.062 (2); S(5)-S(6), 2.037 (2). The torsion angles in the chain are as follows (in degrees): S(2)-S(3), 73.28 (10)°; S(3)-S(4), 74.41 (10)°; S(4)-S(5), 65.22 (10)°; S(5)-S(6), 79.86 (10)°. The (Ph4P)2S7 salt dissolves in polar solvents to give blue solutions with adsorption bands at 610, 470, 345 (sh), and 304 nm.

AB - The S72- anion has been obtained by the reaction of MoS92- with an excess of the sodium salt of the diethyldithiocarbamate anion in acetonitrile solution. The tetraphenylphosphonium salt of S72-, (Ph4P)2S7 (I), crystallizes in the triclinic space group P1 with Z = 2 and lattice parameters a = 11.041 (3) Å, b = 18.589 (4) Å, c = 12.040 (3) Å, α = 74.58 (3)°, β = 69.05 (3)°, γ = 87.76 (4)°, and V = 2220.18 Å3. Diffraction data (Mo Kα radiation, 2θmax = 50°) were collected with a Picker FACS-I automated diffractometer, and the structure was solved and refined by direct methods and full-matrix least-squares procedures to RF = 5.8% and RwF = 8.7% with use of 5102 unique reflections. The S72- ion is found to be a right-handed nonbranched S(1)S(2)S(3)S(4)S(5)S(6)S(7) helix with very short terminal sulfur-sulfur bonds of 1.990 (2) and 1.995 (2) Å for S(1)-S(2) and S(6)-S(7), respectively. The internal bond distances are as follows (in Å): S(2)-S(3), 2.036 (2); S(3)-S(4), 2.062 (2); S(4)-S(5), 2.062 (2); S(5)-S(6), 2.037 (2). The torsion angles in the chain are as follows (in degrees): S(2)-S(3), 73.28 (10)°; S(3)-S(4), 74.41 (10)°; S(4)-S(5), 65.22 (10)°; S(5)-S(6), 79.86 (10)°. The (Ph4P)2S7 salt dissolves in polar solvents to give blue solutions with adsorption bands at 610, 470, 345 (sh), and 304 nm.

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