Electrochemical Synthesis of [NEt4]2[enH]2[Ge2Se6] and [NEt4]4[Sn4Se10]

Chang Woo Park; Michael A. Pell; James A Ibers

Electrochemical Synthesis of [NEt₄]₂[enH]₂[Ge₂Se₆] and [NEt₄]₄[Sn₄Se₁₀]

Chang Woo Park^*, Michael A. Pell, James A Ibers

^*Corresponding author for this work

Chemistry

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Abstract

[NEt₄][enH]₂[Ge₂Se₆] and [NEt₄]₄[Sn₄Se₁₀] have been synthesized electrochemically by the reduction of metal chalcogen alloys in an electrolyte solution of NEt₄Br in ethylenediamine. The structures of both compounds have been determined by single-crystal X-ray methods. [NEt₄]₂[Ge₂Se₆] crystallizes in the triclinic space group C_i¹-P1̄ with one formula unit in a cell of dimensions a = 7.805(4) Å, b = 10.747(6) Å, c = 11.445(6) Å, α = 110.33(2)°, β = 97.19(3)°, γ = 92.62(2)°, and V = 889.0(8) Å³ (T = 115 K). Final agreement indices for [NEt₄]₂[enH]₂[Ge₂Se₆] are 0.116 for R_W(F_o²) for all the 2982 data and 0.055 for R₁ for the 1958 reflections with F_o² ≥ 2σ(F_o²) (158 variables). [NEt₄]₄[Sn₄Se₁₀] crystallizes in the cubic space group T_d⁴-P4̄3n with eight formula units in a cell of dimensions a = 22.170(7) and V= 10897(6) Å³3 (T= 115 K). Final agreement indices for [NEt₄]₄[Sn₄Se₁₀] are 0.123 for R_w(F_o² for all the 1490 data and 0.057 for R₁ for the 1138 data with F_o² ≥ 2σ(F_o²) (90 variables). The [Ge₂Se₆]^4- anion is composed of a pair of edge-sharing tetrahedra. Each of the two independent [Sn₄Se₁₀]^4- anions has the adamantane-type structure consisting of four Sn tetrahedra, each of which shares three edges with three similar tetrahedra; the symmetry of one anion is 4̄ (_S4) while that of the other is 23 (T). Although both the [Ge₂Se₆]^4- and [Sn₄Se₁₀]^4-]4' anions are new, each has group 14 structural analogues.

Original language	English (US)
Pages (from-to)	4555-4558
Number of pages	4
Journal	Inorganic Chemistry
Volume	35
Issue number	16
State	Published - Dec 1 1996

ASJC Scopus subject areas

Physical and Theoretical Chemistry
Inorganic Chemistry

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@article{0ed0b4b1a42040a98a8dac0dbddc9b51,

title = "Electrochemical Synthesis of [NEt4]2[enH]2[Ge2Se6] and [NEt4]4[Sn4Se10]",

abstract = "[NEt4][enH]2[Ge2Se6] and [NEt4]4[Sn4Se10] have been synthesized electrochemically by the reduction of metal chalcogen alloys in an electrolyte solution of NEt4Br in ethylenediamine. The structures of both compounds have been determined by single-crystal X-ray methods. [NEt4]2[Ge2Se6] crystallizes in the triclinic space group Ci1-P{\=1} with one formula unit in a cell of dimensions a = 7.805(4) {\AA}, b = 10.747(6) {\AA}, c = 11.445(6) {\AA}, α = 110.33(2)°, β = 97.19(3)°, γ = 92.62(2)°, and V = 889.0(8) {\AA}3 (T = 115 K). Final agreement indices for [NEt4]2[enH]2[Ge2Se6] are 0.116 for RW(Fo2) for all the 2982 data and 0.055 for R1 for the 1958 reflections with Fo2 ≥ 2σ(Fo2) (158 variables). [NEt4]4[Sn4Se10] crystallizes in the cubic space group Td4-P{\=4}3n with eight formula units in a cell of dimensions a = 22.170(7) and V= 10897(6) {\AA}33 (T= 115 K). Final agreement indices for [NEt4]4[Sn4Se10] are 0.123 for Rw(Fo2 for all the 1490 data and 0.057 for R1 for the 1138 data with Fo2 ≥ 2σ(Fo2) (90 variables). The [Ge2Se6]4- anion is composed of a pair of edge-sharing tetrahedra. Each of the two independent [Sn4Se10]4- anions has the adamantane-type structure consisting of four Sn tetrahedra, each of which shares three edges with three similar tetrahedra; the symmetry of one anion is {\=4} (S4) while that of the other is 23 (T). Although both the [Ge2Se6]4- and [Sn4Se10]4-]4' anions are new, each has group 14 structural analogues.",

author = "Park, {Chang Woo} and Pell, {Michael A.} and Ibers, {James A}",

year = "1996",

month = dec,

day = "1",

language = "English (US)",

volume = "35",

pages = "4555--4558",

journal = "Inorganic Chemistry",

issn = "0020-1669",

publisher = "American Chemical Society",

number = "16",

}

TY - JOUR

T1 - Electrochemical Synthesis of [NEt4]2[enH]2[Ge2Se6] and [NEt4]4[Sn4Se10]

AU - Park, Chang Woo

AU - Pell, Michael A.

AU - Ibers, James A

PY - 1996/12/1

Y1 - 1996/12/1

N2 - [NEt4][enH]2[Ge2Se6] and [NEt4]4[Sn4Se10] have been synthesized electrochemically by the reduction of metal chalcogen alloys in an electrolyte solution of NEt4Br in ethylenediamine. The structures of both compounds have been determined by single-crystal X-ray methods. [NEt4]2[Ge2Se6] crystallizes in the triclinic space group Ci1-P1̄ with one formula unit in a cell of dimensions a = 7.805(4) Å, b = 10.747(6) Å, c = 11.445(6) Å, α = 110.33(2)°, β = 97.19(3)°, γ = 92.62(2)°, and V = 889.0(8) Å3 (T = 115 K). Final agreement indices for [NEt4]2[enH]2[Ge2Se6] are 0.116 for RW(Fo2) for all the 2982 data and 0.055 for R1 for the 1958 reflections with Fo2 ≥ 2σ(Fo2) (158 variables). [NEt4]4[Sn4Se10] crystallizes in the cubic space group Td4-P4̄3n with eight formula units in a cell of dimensions a = 22.170(7) and V= 10897(6) Å33 (T= 115 K). Final agreement indices for [NEt4]4[Sn4Se10] are 0.123 for Rw(Fo2 for all the 1490 data and 0.057 for R1 for the 1138 data with Fo2 ≥ 2σ(Fo2) (90 variables). The [Ge2Se6]4- anion is composed of a pair of edge-sharing tetrahedra. Each of the two independent [Sn4Se10]4- anions has the adamantane-type structure consisting of four Sn tetrahedra, each of which shares three edges with three similar tetrahedra; the symmetry of one anion is 4̄ (S4) while that of the other is 23 (T). Although both the [Ge2Se6]4- and [Sn4Se10]4-]4' anions are new, each has group 14 structural analogues.

AB - [NEt4][enH]2[Ge2Se6] and [NEt4]4[Sn4Se10] have been synthesized electrochemically by the reduction of metal chalcogen alloys in an electrolyte solution of NEt4Br in ethylenediamine. The structures of both compounds have been determined by single-crystal X-ray methods. [NEt4]2[Ge2Se6] crystallizes in the triclinic space group Ci1-P1̄ with one formula unit in a cell of dimensions a = 7.805(4) Å, b = 10.747(6) Å, c = 11.445(6) Å, α = 110.33(2)°, β = 97.19(3)°, γ = 92.62(2)°, and V = 889.0(8) Å3 (T = 115 K). Final agreement indices for [NEt4]2[enH]2[Ge2Se6] are 0.116 for RW(Fo2) for all the 2982 data and 0.055 for R1 for the 1958 reflections with Fo2 ≥ 2σ(Fo2) (158 variables). [NEt4]4[Sn4Se10] crystallizes in the cubic space group Td4-P4̄3n with eight formula units in a cell of dimensions a = 22.170(7) and V= 10897(6) Å33 (T= 115 K). Final agreement indices for [NEt4]4[Sn4Se10] are 0.123 for Rw(Fo2 for all the 1490 data and 0.057 for R1 for the 1138 data with Fo2 ≥ 2σ(Fo2) (90 variables). The [Ge2Se6]4- anion is composed of a pair of edge-sharing tetrahedra. Each of the two independent [Sn4Se10]4- anions has the adamantane-type structure consisting of four Sn tetrahedra, each of which shares three edges with three similar tetrahedra; the symmetry of one anion is 4̄ (S4) while that of the other is 23 (T). Although both the [Ge2Se6]4- and [Sn4Se10]4-]4' anions are new, each has group 14 structural analogues.

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ER -

Electrochemical Synthesis of [NEt₄]₂[enH]₂[Ge₂Se₆] and [NEt₄]₄[Sn₄Se₁₀]

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