Abstract
Abstract Na3B5O8S was prepared from the reaction of sodium sulphide with boron oxide and sodium carbonate at 500 °C in a graphitized silica tube. It is the first oxothioborate that could be synthesized and characterized by single-crystal X-ray diffraction. Na3B5O8S crystallizes in the monoclinic space group P21/c with a=11.390(2) A , b=6.249(1) A , c=10.934(2) A and β=93.94(2)°. In the structure, polymeric [B5O8S3−]n anions form two-dimensionally infinite layers containing groups of two spirocyclically connected six-membered B3O3 rings with one exocyclic sulphur atom bonded to one of them. Two of the five boron atoms are in tetrahedral BO4 coordination ( BO=1.433–1.504 A ) and three have trigonal planar BO3 or BO2S coordination ( BO=1.353–1.393 A , BS=1.813 A ). The three types of sodium cations between the layers are coordinated by 7 O, 4S+2O and 1S+6O atoms.
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