Organotin compounds / Vanadium / Heteropolyoxometal compounds / Single crystal structure analysis / X-ray diffraction Abstract. The synthesis, molecular and crystal structure of ( n BuSn) 9 (V V O) 3 O 14 (OH) 6 Cl 2 (dmso) 2 Á 3 DMSO (1) are described. The yellow compound crystallizes in the monoclinicThe neutral monoorganotin-polyoxovanadium molecule ( n BuSn) 9 (V V O) 3 O 14 (OH) 6 Cl 2 Â (dmso) 2 (1a) shows the same distorted icosahedral arrangement of the metal atoms and a very similar metal-oxygen framework as the well known [( i PrSn) 12 O 14 (OH) 6 ] 2þ ion (2) from which it can be derived formally by substitution of three square pyramidally coordinated {RSnO 4 } groups by three {OVO 4 } groups of the same geometry. In addition, two further {RSnO 4 } groups are replaced by two octahedral {RSnO 3 Cl(dmso)} units.
C10H22Cl2Sn, orthorhombic, P2 1 2 1 2 1 (no. 19), a = 6.5566(6) Å, b = 9.068(1) Å, c = 25.316(2) Å, V = 1505.2 Å 3 , Z = 4, Rgt(F) = 0.062, wRref(F 2 ) = 0.167, T = 258 K.
Source of materialThe title compound was synthesized according to published procedure [1]. Suitable single crystals were grown from the melt.
Experimental detailsBecause of the high flexibility of the n-pentyl rest high anisotropic thermal parameters resulted for all carbon atoms. Because this effect distorted some of the bond lengths and angles all carbon atoms were refined isotropically in addition to a common carboncarbon bond length. Moreover, the most prominent disordering of side chain 2 was taken into account by a second position of the methylene groups C22, C23 and the methyl group C24 with side occupancy factors for both conformations of 0.75 and 0.25, respectively.
Discussion
The title compound, C16H17NO5S, was one of two condensation products from the reaction of 1-(1,3-benzothiazol-2-yl)propan-2-one with methyl chloroacetate. The non-H atoms in each of the four substituent groups on the central quaternary C atom are virtually coplanar. The maximum deviations from the least-squares planes are 0.015 (2) and 0.020 (2) Å for the methyl C atoms in the methyl acetate substituents and 0.033 (1) Å for the linked C atom of the benzothiazole substituent. The S, C and N atoms in the thiazole ring of the benzothiazole substituent lie −0.037 (2), 0.046 (2) and −0.028 (2) Å, respectively, from the mean plane defined by the benzene ring atoms.
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