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The crystal and molecular structures of tris(3,3-dimethylbutyldithiocarbonato)-arsenic(III), -antimony(III) and -bismuth(III), A(S 2 COCH 2 CH 2 CMe 3 ) 3 , have been determined at room temperature. The colorless crystals of A = As(III) are triclinic, space group  P [unk] with unit cell dimensions  a  = 11.837(2) Å,  b  = 13.430(2) Å,  c  = 10.284(1) Å,  α  = 98.39(1)°,  β  = 102.472(9)°,  γ  = 101.73(1)°,  Z  = 2 and  D  x  = 1.316 Mg m −3 . The colorless crystals of A = Sb(III) are monoclinic, space group  P 2 1 / c  with unit cell dimensions  a  = 16.110(3) Å,  b  = 6.077(4) Å,  c  = 31.101(3) Å,  β  = 97.65(1)°,  Z  = 4 and  D  x  = 1.439 Mg m −3 . The yellow crystals of A = Bi(III) are also monoclinic, space group  P 2 1 / c  with unit cell dimensions  a  = 16.149(3) Å,  b  = 6.063(3) Å,  c  = 31.052(7) Å,  β  = 97.25(2)°,  Z  = 4 and  D  x  = 1.632 Mg m −3  The structures were solved by direct methods and each refined by a full-matrix least-squares procedure to final  R  = 0.042 using 3118 reflections for A = As(III); to  R  = 0.051 using 3357 reflections for A = Sb(III); and to final  R  = 0.056 for 2606 reflections for A = Bi(III). The A = As(III) structure comprises isolated molecules with the central atom existing in a distorted capped octahedral geometry. A disorted pentagonal bipyramidal geometry is found in the A = Sb(III) structure where loose association, via Sb … S interactions, are found between centrosymmetrically related pairs. An analogous structure is found for A = Bi (III), however, relatively stronger Bi … S interactions are in existence. A discussion of the different motifs found for A(S 2 COR) 3  structures indicates the importance of crystal packing effects, i.e. the desire to maximise A … S intermolecular contacts, in these structures.

The crystal and molecular structures of A(S 2 COCH 2 CH 2 CMe 3 ) 3 , A = As(III), Sb(III) and Bi(III)