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Acta Crystallogr Sect E Struct Rep Online. 2010 May 1; 66(Pt 5): e23.
Published online 2010 April 14. doi:  10.1107/S1600536810007476
PMCID: PMC2979267

(Dimethyl sulfoxide-κO)[3-hydr­oxy-2-hydroxy­methyl-2-(3-meth­oxy-2-oxido­benzyl­ideneamino-κ2 O 2,N)propanolato-κO]dioxomolybdenum(VI). Corrigendum

Abstract

The crystal structure of the title compound in the paper by Sui, Fang, Luo, Chen & Zhou [Acta Cryst. (2006), E62, m1994–m1996] has been rerefined to allow for identification of a disordered dimethyl sulfoxide ligand.

The structure reported by Sui et al. (2006) [triangle] has been rerefined. The compound was originally determined by Rao et al. [J. Chem. Soc. Dalton Trans. (1998) [triangle], 2383] and has been redetermined here to a significantly higher precision of the lattice parameters [a = 14.3130 (7) Å, b = 9.2596 (5) Å and c = 14.8563 (7) Å here versus a = 14.305 (3) Å, b = 9.249 (2) Å and c = 14.860 (3) Å reported by Rao et al.], bond lengths and s.u. values [e.g. Mo1—O6 = 1.6937 (17) Å here versus Mo1—O6 1.697 (4) Å reported by Rao et al.; R = 0.022 here versus R = 0.050 reported by Rao et al.]. The results of the current redetermination allow the identification of a disordered dimethyl sulfoxide ligand and a clarification of the nature of the intra- and inter­molecular hydrogen bonding.

Experimental

Crystal data

  • [Mo(C12H15NO5)O2(C2H6OS)]
  • M r = 459.32
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-66-00e23-efi1.jpg
  • a = 14.3130 (7) Å
  • b = 9.2596 (5) Å
  • c = 14.8563 (7) Å
  • β = 115.324 (1)°
  • V = 1779.74 (15) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 0.90 mm−1
  • T = 295 K
  • 0.56 × 0.39 × 0.35 mm

Data collection

  • Bruker APEXII area-detector diffractometer
  • Absorption correction: multi-scan (SADABS; Bruker, 2004 [triangle]) T min = 0.632, T max = 0.746
  • 10668 measured reflections
  • 3278 independent reflections
  • 3056 reflections with I > 2σ(I)
  • R int = 0.024

Refinement

  • R[F 2 > 2σ(F 2)] = 0.022
  • wR(F 2) = 0.064
  • S = 1.07
  • 3278 reflections
  • 259 parameters
  • 40 restraints
  • H-atom parameters constrained
  • Δρmax = 0.36 e Å−3
  • Δρmin = −0.44 e Å−3

Data collection: APEX2 (Bruker, 2004 [triangle]); cell refinement: APEX2 (Bruker, 2004 [triangle]); data reduction: APEX2 (Bruker, 2004 [triangle]); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXL97 (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008 [triangle]).

Table 1
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810007476/ng9064sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810007476/ng9064Isup2.hkl

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: NG9064).

References

  • Bruker (2004). APEX2 (Version 1.22) and SADABS Bruker AXS Inc., Madison, Wisconsin, USA
  • Rao, C. P., Sreedhara, A., Rao, P. V., Verghese, M. B., Rissanen, K., Kolehmainen, E., Lokanath, N. K., Sridhar, M. A. & Prasad, J. S. (1998). J. Chem. Soc. Dalton Trans. pp. 2383.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Sui, Y., Fang, X.-N., Luo, Q.-Y., Chen, H.-M. & Zhou, M.-Q. (2006). Acta Cryst. E62, m1994–m1996.

Articles from Acta Crystallographica Section E: Structure Reports Online are provided here courtesy of International Union of Crystallography