Solvothermal Synthesis, Crystal Structure, and Thermal Stability of Three‐Layered Thioantimonate(III) Complexes: [Ni(C₃H₁₀N₂)₃]Sb₄S₇, [C₄H₁₄N₂]Sb₈S₁₃·H₂O, and [C₆H₁₈N₂]Sb₁₀S₁₆·H₂O

Abstract

Abstract Three new thioantimonate(III) complexes [Ni(1,2‐PDA) 3 ]Sb 4 S 7 ( 1 ) (1,2‐PDA = 1,2‐propanediamine), [dmenH 2 2+ ]Sb 8 S 13 · H 2 O ( 2 ) (dmen = N , N ‐dimethylethylenediamine), and [deenH 2 2+ ]Sb 10 S 16 · H 2 O ( 3 ) (deen = N , N ‐diethylethylenediamine), prepared under solvothermal conditions, have been characterized by single‐crystal X‐ray diffraction, elemental analysis, and DTA‐TG measurements. In compound 1 , a rectangle‐like Sb 16 S 16 heteroring whose dimensions are about 8.1 × 14.7 Å is observed, this is the largest reported pore in layered thioantimonates to date. Further condensation of the Sb 16 S 16 heterorings resulted in an unprecedented framework of the five‐atom thick Sb x S y n – layer. In 2 , a new member of Sb n S n ( n = 2, 3, 4, 8, 16, 30, 31, 32) heterocycles Sb 15 S 15 heteroring has been obtained as the first example. In compound 3 , the most particular feature is that when the secondary Sb–S bonds are considered the Sb2 atom becomes sevenfold coordinated.(© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2007)