The crystal and molecular structure of tris(tert-butyl thioxanthato)iron(III)

D. F. Lewis, S. J. Lippard, Jon A Zubieta

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Abstract

The structure of tris(tert-butyl thioxanthato)iron(III) has been determined in a single-crystal X-ray diffraction study. The coordination geometry of the iron atom is a distorted octahedron of sulfur atoms contributed by the three chelating thioxanthate ligands. The distortion may be expressed in terms of a twist angle a = 42°, compared to the value of α = 60° required for a regular octahedron. The mean iron-sulfur bond distance is 2.297 (7) Å, and S-Fe-S intrachelate angle, 75.2 (2).° The geometries of coordinated 1,1-dithiolate ligands in the present and several related tris-chelate metal complexes are summarized. There is a significant amount (10-30%) of double-bond character in the C-X bond for coordinated -S2CX (X = OR, SR) ligands, although appreciably less than for analogous dithiocarbamate (X = NR2) compounds (40-50%). The complex Fe(S2CSC4H9)3 crystallizes in the triclinic system, space group P1, with a = 19.44 (1) Å, b = 5.917 (4) Å, c = 11.016 (6) Å, α = 100.36 (1)°, β = 86.30 (1)°, γ = 90.84 (2)°. The measured density of 1.48 ± 0.01 g/cm3 requires two molecules per unit cell (ρcalcd = 1.474 ± 0.001 g/cm3). From 2330 independent, statistically significant reflections collected by diffractometer, the structure was solved by the usual Patterson and Fourier synthesis methods. Least-squares refinement of all atoms including hydrogen converged at values for R1 = 0.060 and R2 = 0.085.

Original languageEnglish (US)
Pages (from-to)823-828
Number of pages6
JournalInorganic Chemistry
Volume11
Issue number4
StatePublished - 1972
Externally publishedYes

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Molecular structure
molecular structure
Iron
Crystal structure
Ligands
Sulfur
iron
Atoms
ligands
crystal structure
sulfur
Geometry
Coordination Complexes
Diffractometers
Chelation
geometry
diffractometers
chelates
atoms
Hydrogen

ASJC Scopus subject areas

  • Inorganic Chemistry

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The crystal and molecular structure of tris(tert-butyl thioxanthato)iron(III). / Lewis, D. F.; Lippard, S. J.; Zubieta, Jon A.

In: Inorganic Chemistry, Vol. 11, No. 4, 1972, p. 823-828.

Research output: Contribution to journalArticle

Lewis, D. F. ; Lippard, S. J. ; Zubieta, Jon A. / The crystal and molecular structure of tris(tert-butyl thioxanthato)iron(III). In: Inorganic Chemistry. 1972 ; Vol. 11, No. 4. pp. 823-828.
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abstract = "The structure of tris(tert-butyl thioxanthato)iron(III) has been determined in a single-crystal X-ray diffraction study. The coordination geometry of the iron atom is a distorted octahedron of sulfur atoms contributed by the three chelating thioxanthate ligands. The distortion may be expressed in terms of a twist angle a = 42°, compared to the value of α = 60° required for a regular octahedron. The mean iron-sulfur bond distance is 2.297 (7) {\AA}, and S-Fe-S intrachelate angle, 75.2 (2).° The geometries of coordinated 1,1-dithiolate ligands in the present and several related tris-chelate metal complexes are summarized. There is a significant amount (10-30{\%}) of double-bond character in the C-X bond for coordinated -S2CX (X = OR, SR) ligands, although appreciably less than for analogous dithiocarbamate (X = NR2) compounds (40-50{\%}). The complex Fe(S2CSC4H9)3 crystallizes in the triclinic system, space group P1, with a = 19.44 (1) {\AA}, b = 5.917 (4) {\AA}, c = 11.016 (6) {\AA}, α = 100.36 (1)°, β = 86.30 (1)°, γ = 90.84 (2)°. The measured density of 1.48 ± 0.01 g/cm3 requires two molecules per unit cell (ρcalcd = 1.474 ± 0.001 g/cm3). From 2330 independent, statistically significant reflections collected by diffractometer, the structure was solved by the usual Patterson and Fourier synthesis methods. Least-squares refinement of all atoms including hydrogen converged at values for R1 = 0.060 and R2 = 0.085.",
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N2 - The structure of tris(tert-butyl thioxanthato)iron(III) has been determined in a single-crystal X-ray diffraction study. The coordination geometry of the iron atom is a distorted octahedron of sulfur atoms contributed by the three chelating thioxanthate ligands. The distortion may be expressed in terms of a twist angle a = 42°, compared to the value of α = 60° required for a regular octahedron. The mean iron-sulfur bond distance is 2.297 (7) Å, and S-Fe-S intrachelate angle, 75.2 (2).° The geometries of coordinated 1,1-dithiolate ligands in the present and several related tris-chelate metal complexes are summarized. There is a significant amount (10-30%) of double-bond character in the C-X bond for coordinated -S2CX (X = OR, SR) ligands, although appreciably less than for analogous dithiocarbamate (X = NR2) compounds (40-50%). The complex Fe(S2CSC4H9)3 crystallizes in the triclinic system, space group P1, with a = 19.44 (1) Å, b = 5.917 (4) Å, c = 11.016 (6) Å, α = 100.36 (1)°, β = 86.30 (1)°, γ = 90.84 (2)°. The measured density of 1.48 ± 0.01 g/cm3 requires two molecules per unit cell (ρcalcd = 1.474 ± 0.001 g/cm3). From 2330 independent, statistically significant reflections collected by diffractometer, the structure was solved by the usual Patterson and Fourier synthesis methods. Least-squares refinement of all atoms including hydrogen converged at values for R1 = 0.060 and R2 = 0.085.

AB - The structure of tris(tert-butyl thioxanthato)iron(III) has been determined in a single-crystal X-ray diffraction study. The coordination geometry of the iron atom is a distorted octahedron of sulfur atoms contributed by the three chelating thioxanthate ligands. The distortion may be expressed in terms of a twist angle a = 42°, compared to the value of α = 60° required for a regular octahedron. The mean iron-sulfur bond distance is 2.297 (7) Å, and S-Fe-S intrachelate angle, 75.2 (2).° The geometries of coordinated 1,1-dithiolate ligands in the present and several related tris-chelate metal complexes are summarized. There is a significant amount (10-30%) of double-bond character in the C-X bond for coordinated -S2CX (X = OR, SR) ligands, although appreciably less than for analogous dithiocarbamate (X = NR2) compounds (40-50%). The complex Fe(S2CSC4H9)3 crystallizes in the triclinic system, space group P1, with a = 19.44 (1) Å, b = 5.917 (4) Å, c = 11.016 (6) Å, α = 100.36 (1)°, β = 86.30 (1)°, γ = 90.84 (2)°. The measured density of 1.48 ± 0.01 g/cm3 requires two molecules per unit cell (ρcalcd = 1.474 ± 0.001 g/cm3). From 2330 independent, statistically significant reflections collected by diffractometer, the structure was solved by the usual Patterson and Fourier synthesis methods. Least-squares refinement of all atoms including hydrogen converged at values for R1 = 0.060 and R2 = 0.085.

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