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 language | English |
|---|---|
| Pages (from-to) | 290-292 |
| Number of pages | 3 |
| Journal | Inorganic Chemistry |
| Volume | 22 |
| Issue number | 2 |
| Publication status | Published - 1983 |
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ASJC Scopus subject areas
- Inorganic Chemistry
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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 journal › Article
}
TY - JOUR
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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UR - http://www.scopus.com/inward/citedby.url?scp=33845552211&partnerID=8YFLogxK
M3 - Article
AN - SCOPUS:33845552211
VL - 22
SP - 290
EP - 292
JO - Inorganic Chemistry
JF - Inorganic Chemistry
SN - 0020-1669
IS - 2
ER -