Low-Dimensional Sulfoantimonates with Metal Complexes as Counterions. Hydrothermal Synthesis and Properties of [M(en)3]Sb2S4 (M = Co, Ni) and [M(en)3]Sb4S7 (M = Fe, Ni)

Hans Oscar Stephan, Mercouri G Kanatzidis

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Abstract

[M(en)3]Sb2S4 (M = Co, Ni) and [M(en)3]Sb4S7 (M = Fe, Ni) were prepared from the MX2/Na3SbS3/en system (X = Cl, Br; en = ethylenediamine) under hydrothermal conditions. Orange-yellow [Ni(en)3]Sb2S4 (1) crystallizes in the monoclinic space group P21/c (No. 14) with a = 10.538(2) Å, b = 14.460(4) Å, c = 12.434(5) Å, β = 99.93(2)°, and Z = 4. Green-yellow [Co(en)3]Sb2S4 (2) crystallizes as a superstructure of 1 with a = 21.131(4) Å, b = 14.619(2) Å, c = 12.540(2) Å, β = 100.50(1)°, and Z = 8. The antimony sulfide frameworks in 1 and 2 consist of SbS3 pyramids sharing two corners to form l/∞[SbS2]- chains. Orange-yellow [Ni(en)3]Sb4S7 (3) crystallizes in the monoclinic space group P21/c (No. 14) with a = 9.930(1) Å, b = 14.212(2) Å, c = 17.242(2) Å, β = 102.55(1)°, and Z = 4. The 1/∞[Sb4S7]2- chains are formed by corner-sharing SbS3 units. Three of these pyramids are arranged to cyclic Sb3S6 trimers which share two of the three exocyclic S-atoms with the fourth SbS3 units to form infinite chains. [Fe(en)3]Sb4S7 (4) is isostructural to 3. In all four compounds the tris(ethylenediamine)metal(II) complexes act as counterions. The thermal, magnetic and optical properties of compounds 1-4 are reported.

Original languageEnglish
Pages (from-to)6050-6057
Number of pages8
JournalInorganic Chemistry
Volume36
Issue number26
Publication statusPublished - 1997

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ethylenediamine
Hydrothermal synthesis
Coordination Complexes
pyramids
Antimony
Sulfides
synthesis
Metal complexes
metals
Magnetic properties
Thermodynamic properties
Optical properties
trimers
antimony
Atoms
sulfides
thermodynamic properties
magnetic properties
optical properties
atoms

ASJC Scopus subject areas

  • Inorganic Chemistry

Cite this

@article{af8de32ccfb44d0fa6cd760a4498eba2,
title = "Low-Dimensional Sulfoantimonates with Metal Complexes as Counterions. Hydrothermal Synthesis and Properties of [M(en)3]Sb2S4 (M = Co, Ni) and [M(en)3]Sb4S7 (M = Fe, Ni)",
abstract = "[M(en)3]Sb2S4 (M = Co, Ni) and [M(en)3]Sb4S7 (M = Fe, Ni) were prepared from the MX2/Na3SbS3/en system (X = Cl, Br; en = ethylenediamine) under hydrothermal conditions. Orange-yellow [Ni(en)3]Sb2S4 (1) crystallizes in the monoclinic space group P21/c (No. 14) with a = 10.538(2) {\AA}, b = 14.460(4) {\AA}, c = 12.434(5) {\AA}, β = 99.93(2)°, and Z = 4. Green-yellow [Co(en)3]Sb2S4 (2) crystallizes as a superstructure of 1 with a = 21.131(4) {\AA}, b = 14.619(2) {\AA}, c = 12.540(2) {\AA}, β = 100.50(1)°, and Z = 8. The antimony sulfide frameworks in 1 and 2 consist of SbS3 pyramids sharing two corners to form l/∞[SbS2]- chains. Orange-yellow [Ni(en)3]Sb4S7 (3) crystallizes in the monoclinic space group P21/c (No. 14) with a = 9.930(1) {\AA}, b = 14.212(2) {\AA}, c = 17.242(2) {\AA}, β = 102.55(1)°, and Z = 4. The 1/∞[Sb4S7]2- chains are formed by corner-sharing SbS3 units. Three of these pyramids are arranged to cyclic Sb3S6 trimers which share two of the three exocyclic S-atoms with the fourth SbS3 units to form infinite chains. [Fe(en)3]Sb4S7 (4) is isostructural to 3. In all four compounds the tris(ethylenediamine)metal(II) complexes act as counterions. The thermal, magnetic and optical properties of compounds 1-4 are reported.",
author = "Stephan, {Hans Oscar} and Kanatzidis, {Mercouri G}",
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T1 - Low-Dimensional Sulfoantimonates with Metal Complexes as Counterions. Hydrothermal Synthesis and Properties of [M(en)3]Sb2S4 (M = Co, Ni) and [M(en)3]Sb4S7 (M = Fe, Ni)

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N2 - [M(en)3]Sb2S4 (M = Co, Ni) and [M(en)3]Sb4S7 (M = Fe, Ni) were prepared from the MX2/Na3SbS3/en system (X = Cl, Br; en = ethylenediamine) under hydrothermal conditions. Orange-yellow [Ni(en)3]Sb2S4 (1) crystallizes in the monoclinic space group P21/c (No. 14) with a = 10.538(2) Å, b = 14.460(4) Å, c = 12.434(5) Å, β = 99.93(2)°, and Z = 4. Green-yellow [Co(en)3]Sb2S4 (2) crystallizes as a superstructure of 1 with a = 21.131(4) Å, b = 14.619(2) Å, c = 12.540(2) Å, β = 100.50(1)°, and Z = 8. The antimony sulfide frameworks in 1 and 2 consist of SbS3 pyramids sharing two corners to form l/∞[SbS2]- chains. Orange-yellow [Ni(en)3]Sb4S7 (3) crystallizes in the monoclinic space group P21/c (No. 14) with a = 9.930(1) Å, b = 14.212(2) Å, c = 17.242(2) Å, β = 102.55(1)°, and Z = 4. The 1/∞[Sb4S7]2- chains are formed by corner-sharing SbS3 units. Three of these pyramids are arranged to cyclic Sb3S6 trimers which share two of the three exocyclic S-atoms with the fourth SbS3 units to form infinite chains. [Fe(en)3]Sb4S7 (4) is isostructural to 3. In all four compounds the tris(ethylenediamine)metal(II) complexes act as counterions. The thermal, magnetic and optical properties of compounds 1-4 are reported.

AB - [M(en)3]Sb2S4 (M = Co, Ni) and [M(en)3]Sb4S7 (M = Fe, Ni) were prepared from the MX2/Na3SbS3/en system (X = Cl, Br; en = ethylenediamine) under hydrothermal conditions. Orange-yellow [Ni(en)3]Sb2S4 (1) crystallizes in the monoclinic space group P21/c (No. 14) with a = 10.538(2) Å, b = 14.460(4) Å, c = 12.434(5) Å, β = 99.93(2)°, and Z = 4. Green-yellow [Co(en)3]Sb2S4 (2) crystallizes as a superstructure of 1 with a = 21.131(4) Å, b = 14.619(2) Å, c = 12.540(2) Å, β = 100.50(1)°, and Z = 8. The antimony sulfide frameworks in 1 and 2 consist of SbS3 pyramids sharing two corners to form l/∞[SbS2]- chains. Orange-yellow [Ni(en)3]Sb4S7 (3) crystallizes in the monoclinic space group P21/c (No. 14) with a = 9.930(1) Å, b = 14.212(2) Å, c = 17.242(2) Å, β = 102.55(1)°, and Z = 4. The 1/∞[Sb4S7]2- chains are formed by corner-sharing SbS3 units. Three of these pyramids are arranged to cyclic Sb3S6 trimers which share two of the three exocyclic S-atoms with the fourth SbS3 units to form infinite chains. [Fe(en)3]Sb4S7 (4) is isostructural to 3. In all four compounds the tris(ethylenediamine)metal(II) complexes act as counterions. The thermal, magnetic and optical properties of compounds 1-4 are reported.

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