Synthesis, structure and 77Se/119Sn NMR spectroscopy of the new polyselenide, tris(tetraselenido)stannate(IV), [Sn(Se4)3]2-

Song Ping Huang, Sandeep Dhingra, Mercouri G Kanatzidis

Research output: Contribution to journalArticle

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Abstract

The reaction of sodium pentaselenide with SnCl4 or SnCl2·2H2O in dimethylformamide (DMF), in a 3:1 ratio, forms the new soluble anion [Sn(Se4)3]2- in high (>79%) yields. The compound (Ph4P)2[Sn(Se4)3] (I) crystallizes in the monoclinic space group P21/c with unit cell dimensions, a = 13.320(2), b = 11.678(3), c = 34.817(9) Å, β = 98.85(2)° and V = 4535 Å3. A single-crystal X-ray diffraction study of I shows that three chelating Se4 2- ligands provide an octahedral coordination about the central Sn4+ atom. The crystal structure was solved and refined with conventional techniques to R = 6.0% and Rw = 7.0%. The average SnSe distance is 2.709(13) Å, while the average SeSe bond distance is 2.324(12) Å. The IR spectrum of I (CsI pellet) shows two sets of absorptions at 273, 256 cm-1 and 181, 173 cm-1, respectively, assigned tentatively to ν(SeSe) and ν(SnSe) vibrations. The 119Sn NMR spectrum of I in DMF, shows a single resonance at - 723 ppm (vs Me4Sn). The 77Se NMR spectrum of I in DMF, shows two resonances at 618 and 459 ppm. Thermal decomposition of I results in formation of SnSe2 at 510°C. Further heating, above 600°C, results in SnSe.

Original languageEnglish
Pages (from-to)1389-1395
Number of pages7
JournalPolyhedron
Volume9
Issue number11
DOIs
Publication statusPublished - 1990

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stannates
Dimethylformamide
Nuclear magnetic resonance spectroscopy
Magnetic Resonance Spectroscopy
nuclear magnetic resonance
synthesis
Nuclear magnetic resonance
spectroscopy
Chelation
Vibration
pellets
X-Ray Diffraction
Heating
thermal decomposition
Anions
Pyrolysis
Negative ions
Hot Temperature
Crystal structure
Sodium

ASJC Scopus subject areas

  • Biochemistry
  • Inorganic Chemistry
  • Physical and Theoretical Chemistry
  • Materials Chemistry

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Synthesis, structure and 77Se/119Sn NMR spectroscopy of the new polyselenide, tris(tetraselenido)stannate(IV), [Sn(Se4)3]2- . / Huang, Song Ping; Dhingra, Sandeep; Kanatzidis, Mercouri G.

In: Polyhedron, Vol. 9, No. 11, 1990, p. 1389-1395.

Research output: Contribution to journalArticle

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abstract = "The reaction of sodium pentaselenide with SnCl4 or SnCl2·2H2O in dimethylformamide (DMF), in a 3:1 ratio, forms the new soluble anion [Sn(Se4)3]2- in high (>79{\%}) yields. The compound (Ph4P)2[Sn(Se4)3] (I) crystallizes in the monoclinic space group P21/c with unit cell dimensions, a = 13.320(2), b = 11.678(3), c = 34.817(9) {\AA}, β = 98.85(2)° and V = 4535 {\AA}3. A single-crystal X-ray diffraction study of I shows that three chelating Se4 2- ligands provide an octahedral coordination about the central Sn4+ atom. The crystal structure was solved and refined with conventional techniques to R = 6.0{\%} and Rw = 7.0{\%}. The average SnSe distance is 2.709(13) {\AA}, while the average SeSe bond distance is 2.324(12) {\AA}. The IR spectrum of I (CsI pellet) shows two sets of absorptions at 273, 256 cm-1 and 181, 173 cm-1, respectively, assigned tentatively to ν(SeSe) and ν(SnSe) vibrations. The 119Sn NMR spectrum of I in DMF, shows a single resonance at - 723 ppm (vs Me4Sn). The 77Se NMR spectrum of I in DMF, shows two resonances at 618 and 459 ppm. Thermal decomposition of I results in formation of SnSe2 at 510°C. Further heating, above 600°C, results in SnSe.",
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N2 - The reaction of sodium pentaselenide with SnCl4 or SnCl2·2H2O in dimethylformamide (DMF), in a 3:1 ratio, forms the new soluble anion [Sn(Se4)3]2- in high (>79%) yields. The compound (Ph4P)2[Sn(Se4)3] (I) crystallizes in the monoclinic space group P21/c with unit cell dimensions, a = 13.320(2), b = 11.678(3), c = 34.817(9) Å, β = 98.85(2)° and V = 4535 Å3. A single-crystal X-ray diffraction study of I shows that three chelating Se4 2- ligands provide an octahedral coordination about the central Sn4+ atom. The crystal structure was solved and refined with conventional techniques to R = 6.0% and Rw = 7.0%. The average SnSe distance is 2.709(13) Å, while the average SeSe bond distance is 2.324(12) Å. The IR spectrum of I (CsI pellet) shows two sets of absorptions at 273, 256 cm-1 and 181, 173 cm-1, respectively, assigned tentatively to ν(SeSe) and ν(SnSe) vibrations. The 119Sn NMR spectrum of I in DMF, shows a single resonance at - 723 ppm (vs Me4Sn). The 77Se NMR spectrum of I in DMF, shows two resonances at 618 and 459 ppm. Thermal decomposition of I results in formation of SnSe2 at 510°C. Further heating, above 600°C, results in SnSe.

AB - The reaction of sodium pentaselenide with SnCl4 or SnCl2·2H2O in dimethylformamide (DMF), in a 3:1 ratio, forms the new soluble anion [Sn(Se4)3]2- in high (>79%) yields. The compound (Ph4P)2[Sn(Se4)3] (I) crystallizes in the monoclinic space group P21/c with unit cell dimensions, a = 13.320(2), b = 11.678(3), c = 34.817(9) Å, β = 98.85(2)° and V = 4535 Å3. A single-crystal X-ray diffraction study of I shows that three chelating Se4 2- ligands provide an octahedral coordination about the central Sn4+ atom. The crystal structure was solved and refined with conventional techniques to R = 6.0% and Rw = 7.0%. The average SnSe distance is 2.709(13) Å, while the average SeSe bond distance is 2.324(12) Å. The IR spectrum of I (CsI pellet) shows two sets of absorptions at 273, 256 cm-1 and 181, 173 cm-1, respectively, assigned tentatively to ν(SeSe) and ν(SnSe) vibrations. The 119Sn NMR spectrum of I in DMF, shows a single resonance at - 723 ppm (vs Me4Sn). The 77Se NMR spectrum of I in DMF, shows two resonances at 618 and 459 ppm. Thermal decomposition of I results in formation of SnSe2 at 510°C. Further heating, above 600°C, results in SnSe.

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