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Volume 66 
Part 10 
Pages m1239-m1240  
October 2010  

Received 22 June 2010
Accepted 20 August 2010
Online 11 September 2010

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Key indicators
Single-crystal X-ray study
T = 295 K
Mean [sigma](C-C) = 0.006 Å
R = 0.041
wR = 0.105
Data-to-parameter ratio = 18.0
Details
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Bis(3-methylphenolato-[kappa]O)(nitrosyl-[kappa]N)[tris(3,5-dimethylpyrazol-1-yl-[kappa]N2)hydridoborato]molybdenum(II)

Wojciech Nitek,a* Piotr P. Romanczyk,b* Tomasz Luberab and Andrzej J. Wlodarczykb

aFaculty of Chemistry, Jagiellonian University, ul. R. Ingardena 3, 30-060 Kraków, Poland, and bFaculty of Chemical Engineering and Technology, Cracow University of Technology, ul. Warszawska 24, 31-155 Kraków, Poland
Correspondence e-mail: nitek@chemia.uj.edu.pl, pr@chemia.pk.edu.pl

The title complex, [Mo(C15H22BN6)(C7H7O)2(NO)], contains an {MoNO}4 core stabilized by [kappa]3-hydrotris(3,5-dimethylpyrazol-1-yl)borate, [TpMe2]-, and two anionic m-cresolate ligands, leading to a distorted octahedral geometry for the Mo atom. The short Mo-O bond lengths [1.935 (2) and 1.971 (2) Å], as well as large Mo-O-Csp2 angles [134.2 (2) and 143.54 (19)°], indicate d[pi]Mo-p[pi]O interactions, which are clearly weaker when compared with {Mo(NO)(TpMe2)} alkoxides. The nitrosyl system is virtually linear [179.3 (3)°] with Mo-N and N-O bond lengths of 1.760 (2) and 1.205 (3) Å, respectively. Intra- and intermolecular C-H(Ph or CH3)...[pi](Ph) interactions between adjacent phenyl rings are found in the crystal structure (dH...Ph in the range 2.743-2.886 Å). One of the Ph rings shows disorder, i.e. swinging in the ring plane.

Related literature

The importance of this class of Mo complexes comes from the fact that some {MoNO}4 alkoxides are efficient catalysts in the cathodic reduction of CHCl3. For the synthesis, spectroscopic characterization and electrochemical properties of [tris(3,5-dimethylpyrazol-1-yl)borato]nitrosylmolybdenum(II) bis-cresolates, see: Wlodarczyk et al. (2008a[Wlodarczyk, A. J., Romanczyk, P. P. & Lubera, T. (2008a). Czasop. Techn. Polit. Krak. 1-Ch, pp. 165-170.]). For the spectroscopic characterization of the mono-cresolate analogue of the title compound, see: McCleverty et al. (1983[McCleverty, J. A., Denti, G., Reynolds, S. J., Drane, A. S., El Murr, N., Rae, A. E., Bailey, N. A., Adams, H. & Smith, J. M. A. (1983). J. Chem. Soc. Dalton Trans. pp. 81-89.]). For related structurally characterized {Mo(NO)(TpMe2)}-alkoxides, see: Romanczyk et al. (2007[Romanczyk, P. P., Guzik, M. N. & Wlodarczyk, A. J. (2007). Polyhedron, 26, 1182-1190.]); Wlodarczyk et al. (2008c[Wlodarczyk, A. J., Romanczyk, P. P., Kurek, S. S., Nitek, W. & McCleverty, J. A. (2008c). Polyhedron, 27, 783-796.]). For the electrocatalytic activity of bis-alkoxide Mo nitrosyls in the reduction of CHCl3, see: Wlodarczyk et al. (2008b[Wlodarczyk, A. J., Romanczyk, P. P., Lubera, T. & Kurek, S. S. (2008b). Electrochem. Commun. 10, 1856-1859.]).

[Scheme 1]

Experimental

Crystal data

  • [Mo(C15H22BN6)(C7H7O)2(NO)]

  • Mr = 637.40

  • Triclinic, [P \overline 1]

  • a = 8.041 (5) Å

  • b = 13.562 (5) Å

  • c = 14.591 (5) Å

  • [alpha] = 86.103 (5)°

  • [beta] = 83.533 (5)°

  • [gamma] = 74.597 (5)°

  • V = 1523.1 (12) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 0.47 mm-1

  • T = 295 K

  • 0.22 × 0.15 × 0.10 mm
Data collection

  • Nonius KappaCCD diffractometer

  • Absorption correction: multi-scan (DENZO-SMN; Otwinowski & Minor, 1997[Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press.]) Tmin = 0.903, Tmax = 0.954

  • 12695 measured reflections

  • 6901 independent reflections

  • 5801 reflections with I > 2[sigma](I)

  • Rint = 0.024
Refinement

  • R[F2 > 2[sigma](F2)] = 0.041

  • wR(F2) = 0.105

  • S = 1.08

  • 6901 reflections

  • 383 parameters

  • H atoms treated by a mixture of independent and constrained refinement

  • [Delta][rho]max = 0.68 e Å-3

  • [Delta][rho]min = -0.51 e Å-3

Data collection: COLLECT (Nonius, 1998[Nonius (1998). COLLECT. Nonius BV, Delft, The Netherlands.]); cell refinement: SCALEPACK (Otwinowski & Minor, 1997[Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press.]); data reduction: DENZO (Otwinowski & Minor, 1997[Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press.]) and SCALEPACK; program(s) used to solve structure: SIR97 (Altomare et al., 1999[Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: ORTEP-3 (Farrugia, 1997[Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.]); software used to prepare material for publication: WinGX (Farrugia, 1999[Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.]).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: RK2216 ).

References

Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119.  [ISI] [CrossRef] [ChemPort] [details]
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.  [CrossRef] [details]
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.  [CrossRef] [ChemPort] [details]
McCleverty, J. A., Denti, G., Reynolds, S. J., Drane, A. S., El Murr, N., Rae, A. E., Bailey, N. A., Adams, H. & Smith, J. M. A. (1983). J. Chem. Soc. Dalton Trans. pp. 81-89.  [CrossRef]
Nonius (1998). COLLECT. Nonius BV, Delft, The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press.
Romanczyk, P. P., Guzik, M. N. & Wlodarczyk, A. J. (2007). Polyhedron, 26, 1182-1190.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Wlodarczyk, A. J., Romanczyk, P. P., Kurek, S. S., Nitek, W. & McCleverty, J. A. (2008c). Polyhedron, 27, 783-796.
Wlodarczyk, A. J., Romanczyk, P. P. & Lubera, T. (2008a). Czasop. Techn. Polit. Krak. 1-Ch, pp. 165-170.
Wlodarczyk, A. J., Romanczyk, P. P., Lubera, T. & Kurek, S. S. (2008b). Electrochem. Commun. 10, 1856-1859.

Acta Cryst (2010). E66, m1239-m1240   [ doi:10.1107/S1600536810033763 ]

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