TY - JOUR
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)
AU - Stephan, Hans Oscar
AU - Kanatzidis, Mercouri G.
PY - 1997
Y1 - 1997
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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U2 - 10.1021/ic970609+
DO - 10.1021/ic970609+
M3 - Article
AN - SCOPUS:0000492796
VL - 36
SP - 6050
EP - 6057
JO - Inorganic Chemistry
JF - Inorganic Chemistry
SN - 0020-1669
IS - 26
ER -