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New Thioantimonates(III) with Different Sb:S Ratios: Solvothermal Syntheses and Crystal Structures of [(C 3 H 10 NO)(C 3 H 10 N)][Sb 8 S 13 ], [(C 2 H 8 NO)(C 2 H 8 N)(CH 5 N)][Sb 8 S 13 ], [(C 6 H 16 N 2 )(C 6 H 14 N 2 )][Sb 6 S 10 ], and [C 8 H 22 N 2 ][Sb 4 S 7 ]
Author(s) -
Seidlhofer Beatrix,
Spetzler Volker,
QuirogaGonzalez Enrique,
Näther Christian,
Bensch Wolfgang
Publication year - 2011
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/zaac.201100204
Subject(s) - triclinic crystal system , monoclinic crystal system , propylamine , ethylamine , chemistry , crystallography , methylamine , crystal structure , stereochemistry , amine gas treating , organic chemistry
Four new thioantimonates(III) with compositions [(C 3 H 10 NO)(C 3 H 10 N)][Sb 8 S 13 ] ( 1 ) (C 3 H 9 NO = 1‐amino‐3‐propanol, C 3 H 9 N = propylamine), [(C 2 H 8 NO)(C 2 H 8 N)(CH 5 N)][Sb 8 S 13 ] ( 2 ) (C 2 H 7 NO = ethanolamine, C 2 H 7 N = ethylamine, CH 5 N = methylamine), [(C 6 H 16 N 2 )(C 6 H 14 N 2 )][Sb 6 S 10 ] ( 3 ) (C 6 H 14 N 2 = 1,2‐diaminocyclohexane) and [C 8 H 22 N 2 ][Sb 4 S 7 ] ( 4 ) (C 8 H 20 N 2 = 1,8‐diaminooctane) were synthesized under solvothermal conditions. Compound 1 : triclinic space group P $\bar{1}$ , a = 6.9695(6) Å, b = 13.8095(12) Å, c = 18.0354(17) Å, α = 98.367(11), β = 96.097(11) and γ = 101.281(11)°; compound 2 : monoclinic space group P 2 1 / m , a = 7.1668(5), b = 25.8986(14), c = 16.0436(11) Å, β = 96.847(8)°; compound 3 : monoclinic space group P 2 1 / n , a = 11.6194(9), b = 10.2445(5) Å, c = 27.3590(18) Å, β = 91.909(6)°; compound 4 : triclinic space group P $\bar{1}$ , a = 7.0743(6), b = 12.0846(11), c = 13.9933(14) Å, α = 114.723(10), β = 97.595(11), γ = 93.272(11)°. The main structural feature of the two atoms thick layered [Sb 8 S 13 ] 2– anion in 1 are large nearly rectangular pores with dimensions 11.2 × 11.7 Å. The layers are stacked perpendicular to [100] to form tunnels being directed along [100]. In contrast to 1 the structure of 2 contains a [Sb 8 S 13 ] 2– chain anion with Sb 12 S 12 pores measuring about 8.9 × 11.5 Å. Only if longer Sb–S distances are considered as bonding interactions a layered anion is formed. The chain anion [Sb 6 S 10 ] 2– in compound 3 is unique and is constructed by corner‐sharing SbS 3 pyramids. Two symmetry‐related single chains consisting of alternating SbS 3 units and Sb 3 S 3 rings are bound to Sb 4 S 4 rings in chair conformation. Finally, in the structure of 4 the SbS 3 and SbS 4 moieties are joined corner‐linked to form a chain of alternating SbS 4 units and (SbS 3 ) 3 blocks. Neighboring chains are connected into sheets that contain relatively large Sb 10 S 10 heterorings. The sheets are further connected by sulfur atoms generating four atoms thick double sheets.