73513-49-2Relevant articles and documents
Common features in the crystal structures of the compounds bis(dimethylstibanyl)oxane and -sulfane, and the minerals valentinite and stibnite (grauspiessglanz)
Breunig,Lork,Roesler,Becker,Mundt,Schwarz
, p. 1595 - 1607 (2008/10/08)
Bis(dimethylstibanyl)oxane (1) and -sulfane (2), the two simplest organoelement species with an Sb-E-Sb fragment (E = O, S), were prepared by alkaline hydrolysis of bromodimethylstibane and by oxidation of tetramethyldistibane with sulfur [18], respectively. As shown by an x-ray structure analysis of compound 1 (m.p. 1,2121, a = 675.9(2), b = 803.1(2), c = 1666.8(4) pm at -70 ± 2°C; Z = 4; R1 = 0.042), the molecules (O-Sb 198.8 and 209.9 pm, Sb-O-Sb 123.0°) adopt a syn-anti conformation in the solid state and are arranged in zigzag chains along [010] via weak intermolecular O··Sb interactions (258.5 pm, Sb-O··Sb 117.8°, O··Sb-O 173.5°) making use, however, of only one Me2Sb moiety. Primary and secondary bond lengths and angles agree very well with corresponding values published for valentinite, the orthorhombic modification of antimony(III) oxide [3]. Bis(dimethylstibanyl)sulfane (2) (m.p. 29 to 31 °C) crystallizes in the uncommon space group P6522 (a = 927.8(3), c= 1940.9(7) pm at -100 ± 2°C; Z = 6; R1 =0.021). Owing to coordination numbers of (1 + 1) and (2 + 2) for both Me2Sb groups and the sulfur atom, respectively, molecules with an approximate syn-syn conformation (S-Sb 249.8 pm, Sb-S-Sb 92.35°) build up a three-dimensional net of double helices which are linked together by Sb · · S contacts (316.4 pm). These parameters shed more light onto the rather complicated structure and bonding situation in stibnite (antimony(III) sulfide [4]). The molecular packing of compound 2 is compared with the structures of relevant inorganic solids, especially with that of ss-quartz [37].