Synthesis, {sup 77}Se and {sup 119}Sn NMR study, and X-ray crystal structure of the Sn{sub 4}Se{sub 10}{sup 4-} anion and Raman spectra of SnSe{sub 4}{sup 4-} and Sn{sub 4}Se{sub 10}{sup 4-}

Campbell, J; DiCiommo, D P; Pirani, A M

doi:10.1021/ic00129a010

Title: Synthesis, {sup 77}Se and {sup 119}Sn NMR study, and X-ray crystal structure of the Sn{sub 4}Se{sub 10}{sup 4-} anion and Raman spectra of SnSe{sub 4}{sup 4-} and Sn{sub 4}Se{sub 10}{sup 4-}

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Abstract

The novel selenostannate(IV) anion, Sn{sub 4}Se{sub 10}{sup 4-}, has been obtained by extracting the ternary alloy KSn{sub 0.67}Se{sub 1.93} in ethylenediamine (en) and liquid NH{sub 3} in the presence of 2, 2, 2-crypt (4, 7, 13, 16, 21, 24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane) and characterized in solution by {sup 77}Se and {sup 119}Sn NMR spectroscopy and in the solid state by X-ray crystallography and Raman spectroscopy. The scalar couplings, {sup 1}J({sup 119}Sn-{sup 77}Se) and {sup 2}J({sup 119}Sn-{sup 77}Sn), have been determined and compared with those of related systems. The salt, (2, 2, 2-crypt-K{sup +}){sub 4}Sn{sub 4}Se{sub 10}{sup 4-}, crystallizes in the triclinic system, space group P{bar 1}, with Z = 2 and a = 14.769(2) {Angstrom}, b = 15.580(1) {Angstrom}, c = 26.275(4) {Angstrom}, {alpha} = 79.19(1){degrees}, {beta} = 85.65(1){degrees}, and {gamma} = 85.870(8){degrees} at 24 {degrees}C. The solid state and solution anion geometry is of the adamantanoid type where the Sn{sup IV} atoms occupy the bridgehead positions and the Se atoms occupy the bridging and terminal sites. The terminal [average, 2.425(2) {Angstrom}] and bridging [average, 2.425(2){Angstrom}] and bridging [average, 2.548(2) {Angstrom}] Sn-Se bond distances were found to correlate with their respective {sup 1}J({sup 119}Sn-{sup 77}Se) coupling constants. The Raman spectrum of the Sn{submore »« less

Authors:

Campbell, J; DiCiommo, D P; Pirani, A M ^[1]

McMaster Univ., Hamilton, Ontario (Canada); and others

Publication Date:: Wed Dec 06 00:00:00 EST 1995

Sponsoring Org.:: USDOE

OSTI Identifier:: 457080

Resource Type:: Journal Article

Journal Name:: Inorganic Chemistry

Additional Journal Information:: Journal Volume: 34; Journal Issue: 25; Other Information: PBD: 6 Dec 1995

Country of Publication:: United States

Language:: English

Subject:: 40 CHEMISTRY; 36 MATERIALS SCIENCE; TIN SELENIDES; CHEMICAL PREPARATION; CRYSTAL STRUCTURE; NMR SPECTRA; SELENIUM 77; TIN 119; RAMAN SPECTROSCOPY

Citation Formats


                    Campbell, J, DiCiommo, D P, and Pirani, A M. Synthesis, {sup 77}Se and {sup 119}Sn NMR study, and X-ray crystal structure of the Sn{sub 4}Se{sub 10}{sup 4-} anion and Raman spectra of SnSe{sub 4}{sup 4-} and Sn{sub 4}Se{sub 10}{sup 4-}.  United States: N. p., 1995. 
        Web.  doi:10.1021/ic00129a010.

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                    Campbell, J, DiCiommo, D P, & Pirani, A M. Synthesis, {sup 77}Se and {sup 119}Sn NMR study, and X-ray crystal structure of the Sn{sub 4}Se{sub 10}{sup 4-} anion and Raman spectra of SnSe{sub 4}{sup 4-} and Sn{sub 4}Se{sub 10}{sup 4-}.  United States.  https://doi.org/10.1021/ic00129a010

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                    Campbell, J, DiCiommo, D P, and Pirani, A M. 1995.  
        "Synthesis, {sup 77}Se and {sup 119}Sn NMR study, and X-ray crystal structure of the Sn{sub 4}Se{sub 10}{sup 4-} anion and Raman spectra of SnSe{sub 4}{sup 4-} and Sn{sub 4}Se{sub 10}{sup 4-}".  United States.  https://doi.org/10.1021/ic00129a010.

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@article{osti_457080,

  title        = {Synthesis, {sup 77}Se and {sup 119}Sn NMR study, and X-ray crystal structure of the Sn{sub 4}Se{sub 10}{sup 4-} anion and Raman spectra of SnSe{sub 4}{sup 4-} and Sn{sub 4}Se{sub 10}{sup 4-}},

  author       = {Campbell, J and DiCiommo, D P and Pirani, A M},

  abstractNote = {The novel selenostannate(IV) anion, Sn{sub 4}Se{sub 10}{sup 4-}, has been obtained by extracting the ternary alloy KSn{sub 0.67}Se{sub 1.93} in ethylenediamine (en) and liquid NH{sub 3} in the presence of 2, 2, 2-crypt (4, 7, 13, 16, 21, 24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane) and characterized in solution by {sup 77}Se and {sup 119}Sn NMR spectroscopy and in the solid state by X-ray crystallography and Raman spectroscopy. The scalar couplings, {sup 1}J({sup 119}Sn-{sup 77}Se) and {sup 2}J({sup 119}Sn-{sup 77}Sn), have been determined and compared with those of related systems. The salt, (2, 2, 2-crypt-K{sup +}){sub 4}Sn{sub 4}Se{sub 10}{sup 4-}, crystallizes in the triclinic system, space group P{bar 1}, with Z = 2 and a = 14.769(2) {Angstrom}, b = 15.580(1) {Angstrom}, c = 26.275(4) {Angstrom}, {alpha} = 79.19(1){degrees}, {beta} = 85.65(1){degrees}, and {gamma} = 85.870(8){degrees} at 24 {degrees}C. The solid state and solution anion geometry is of the adamantanoid type where the Sn{sup IV} atoms occupy the bridgehead positions and the Se atoms occupy the bridging and terminal sites. The terminal [average, 2.425(2) {Angstrom}] and bridging [average, 2.425(2){Angstrom}] and bridging [average, 2.548(2) {Angstrom}] Sn-Se bond distances were found to correlate with their respective {sup 1}J({sup 119}Sn-{sup 77}Se) coupling constants. The Raman spectrum of the Sn{sub 4}Se{sub 10}{sup 4-} anion has been assigned and compared to those of related adamantanoid systems and SnSe{sub 4}{sup -4}.},

  doi          = {10.1021/ic00129a010},

  url          = {https://www.osti.gov/biblio/457080},
  journal      = {Inorganic Chemistry},
number       = 25,

  volume       = 34,

  place        = {United States},

  year         = {Wed Dec 06 00:00:00 EST 1995},

  month        = {Wed Dec 06 00:00:00 EST 1995}

}

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