[Journal logo]

Volume 68 
Part 11 
Pages m1344-m1345  
November 2012  

Received 20 September 2012
Accepted 8 October 2012
Online 13 October 2012

Key indicators
Single-crystal X-ray study
T = 100 K
Mean [sigma](C-C) = 0.005 Å
Disorder in solvent or counterion
R = 0.041
wR = 0.099
Data-to-parameter ratio = 16.6
Details
Open access

Tetrakis(5,7-dimethylquinolin-8-olato-[kappa]2N,O)zirconium(IV) dimethylformamide disolvate

aDepartment of Chemistry, University of the Free State, PO Box 339, Bloemfontein 9300, South Africa
Correspondence e-mail: steynm@ufs.ac.za

In the title compound, [Zr(C11H10NO)4]·2C3H7NO, the ZrIV ion is coordinated by four bidentate 5,7-dimethylquinolin-8-olate ligands in a slightly distorted square-antiprismatic coordination environment. The asymmetric unit also contains two N,N'-dimethylformamide (DMF) solvent molecules. In the crystal, a weak C-H...O hydrogen bond links the complex molecule to a solvent molecule and weak [pi]-[pi] stacking interactions [centroid-centroid distance = 3.671 (3) Å] also occur. One of the DMF solvent molecules was refined as disordered over three sets of sites, with refined occupancies in the ratio of 0.391 (9):0.342 (10):0.267 (7).

Related literature

For N,O- and O,O'-bidentate ligand complexes of zirconium and hafnium, see: Calderazzo et al. (1998[Calderazzo, F., Englert, U., Maichle-Mossmer, C., Marchetti, F., Pampaloni, G., Petroni, D., Pinzino, C., Strähle, J. & Tripepi, G. (1998). Inorg. Chim. Acta, 270, 177-188.]); Demakopoulos et al. (1995[Demakopoulos, I., Klouras, N., Raptopoulou, C. P. & Terzis, A. (1995). Z. Anorg. Allg. Chem. 621, 1761-1766.]); Steyn et al. (2008[Steyn, M., Roodt, A. & Steyl, G. (2008). Acta Cryst. E64, m827.], 2011[Steyn, M., Visser, H. G., Roodt, A. & Muller, T. J. (2011). Acta Cryst. E67, m1240-m1241.]); Viljoen et al. (2008[Viljoen, J. A., Muller, A. & Roodt, A. (2008). Acta Cryst. E64, m838-m839.], 2009a[Viljoen, J. A., Visser, H. G., Roodt, A. & Steyn, M. (2009a). Acta Cryst. E65, m1514-m1515.],b[Viljoen, J. A., Visser, H. G., Roodt, A. & Steyn, M. (2009b). Acta Cryst. E65, m1367-m1368.]; 2010a[Viljoen, J. A., Visser, H. G. & Roodt, A. (2010a). Acta Cryst. E66, m603-m604.],b[Viljoen, J. A., Visser, H. G. & Roodt, A. (2010b). Acta Cryst. E66, m1053-m1054.]); Zherikova et al. (2005[Zherikova, K. V., Morozova, N. B., Kurateva, N. V., Baidina, I. A., Stabnikov, P. A. & Igumenov, I. K. (2005). J. Struct. Chem. 46, 1039-1046.], 2006[Zherikova, K. V., Morozova, N. B., Baidina, I. A., Peresypkina, E. V. & Igumenov, I. K. (2006). J. Struct. Chem. 47, 570-574.], 2008[Zherikova, K. V., Baidina, I. A., Morozova, N. B., Kurateva, N. V. & Igumenov, I. K. (2008). J. Struct. Chem. 49, 1098-1103.]). For our ongoing research of structure reactivity relationships in catalysis, separation chemistry and other industrial reaction mechanisms, see: Roodt et al. (2011[Roodt, A., Visser, H. G. & Brink, A. (2011). Crystallogr. Rev. 17, 241-280.]); Schutte et al. (2011[Schutte, M., Kemp, G., Visser, H. G. & Roodt, A. (2011). Inorg. Chem. 50, 12486-12498.]); Brink et al. (2010[Brink, A., Roodt, A., Steyl, G. & Visser, H. G. (2010). Dalton Trans. 39, 5572-5578.]); Ferreira et al. (2007[Ferreira, A. C., Crous, R., Bennie, L., Meij, A. M. M., Blann, K., Bezuidenhoudt, B. C. B., Young, D. A., Green, M. J. & Roodt, A. (2007). Angew. Chem. Int. Ed. 46, 2273-2275.]); Haumann et al. (2004[Haumann, M., Meijboom, R., Moss, J. R. & Roodt, A. (2004). Dalton Trans. pp. 1679-1686.]).

[Scheme 1]

Experimental

Crystal data
  • [Zr(C11H10NO)4]·2C3H7NO

  • Mr = 926.21

  • Orthorhombic, P n a 21

  • a = 15.572 (5) Å

  • b = 18.706 (5) Å

  • c = 15.853 (5) Å

  • V = 4618 (2) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 0.29 mm-1

  • T = 100 K

  • 0.26 × 0.14 × 0.13 mm

Data collection
  • Bruker APEXII CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2004[Bruker (2004). SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.928, Tmax = 0.963

  • 61276 measured reflections

  • 11142 independent reflections

  • 8497 reflections with I > 2[sigma](I)

  • Rint = 0.064

Refinement
  • R[F2 > 2[sigma](F2)] = 0.041

  • wR(F2) = 0.099

  • S = 1.02

  • 11142 reflections

  • 671 parameters

  • 299 restraints

  • H-atom parameters constrained

  • [Delta][rho]max = 0.42 e Å-3

  • [Delta][rho]min = -0.39 e Å-3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 5375 Friedel pairs

  • Flack parameter: -0.01 (3)

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
C14A-H14E...O201i 0.96 2.43 3.358 (7) 161
Symmetry code: (i) [-x+{\script{3\over 2}}, y+{\script{1\over 2}}, z-{\script{1\over 2}}].

Data collection: APEX2 (Bruker, 2005[Bruker (2005). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2004[Bruker (2004). SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: DIAMOND (Brandenburg & Putz, 2005[Brandenburg, K. & Putz, H. (2005). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); 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: LH5537 ).


Acknowledgements

Financial assistance from the Advanced Metals Initiative (AMI) and the Department of Science and Technology (DST) of South Africa, as well as the New Metals Development Network (NMDN) and the South African Nuclear Energy Corporation Limited (Necsa), is gratefully acknowledged.

References

Brandenburg, K. & Putz, H. (2005). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Brink, A., Roodt, A., Steyl, G. & Visser, H. G. (2010). Dalton Trans. 39, 5572-5578.  [CSD] [CrossRef] [ChemPort] [PubMed]
Bruker (2004). SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2005). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.
Calderazzo, F., Englert, U., Maichle-Mossmer, C., Marchetti, F., Pampaloni, G., Petroni, D., Pinzino, C., Strähle, J. & Tripepi, G. (1998). Inorg. Chim. Acta, 270, 177-188.  [ISI] [CSD] [CrossRef] [ChemPort]
Demakopoulos, I., Klouras, N., Raptopoulou, C. P. & Terzis, A. (1995). Z. Anorg. Allg. Chem. 621, 1761-1766.  [CrossRef] [ChemPort]
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.  [CrossRef] [ChemPort] [details]
Ferreira, A. C., Crous, R., Bennie, L., Meij, A. M. M., Blann, K., Bezuidenhoudt, B. C. B., Young, D. A., Green, M. J. & Roodt, A. (2007). Angew. Chem. Int. Ed. 46, 2273-2275.  [ISI] [CrossRef] [ChemPort]
Flack, H. D. (1983). Acta Cryst. A39, 876-881.  [CrossRef] [details]
Haumann, M., Meijboom, R., Moss, J. R. & Roodt, A. (2004). Dalton Trans. pp. 1679-1686.  [CSD] [CrossRef]
Roodt, A., Visser, H. G. & Brink, A. (2011). Crystallogr. Rev. 17, 241-280.  [CrossRef] [ChemPort]
Schutte, M., Kemp, G., Visser, H. G. & Roodt, A. (2011). Inorg. Chem. 50, 12486-12498.  [ISI] [CSD] [CrossRef] [ChemPort] [PubMed]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Steyn, M., Roodt, A. & Steyl, G. (2008). Acta Cryst. E64, m827.  [CSD] [CrossRef] [details]
Steyn, M., Visser, H. G., Roodt, A. & Muller, T. J. (2011). Acta Cryst. E67, m1240-m1241.  [CSD] [CrossRef] [details]
Viljoen, J. A., Muller, A. & Roodt, A. (2008). Acta Cryst. E64, m838-m839.  [CSD] [CrossRef] [details]
Viljoen, J. A., Visser, H. G. & Roodt, A. (2010a). Acta Cryst. E66, m603-m604.  [CSD] [CrossRef] [details]
Viljoen, J. A., Visser, H. G. & Roodt, A. (2010b). Acta Cryst. E66, m1053-m1054.  [CSD] [CrossRef] [details]
Viljoen, J. A., Visser, H. G., Roodt, A. & Steyn, M. (2009a). Acta Cryst. E65, m1514-m1515.  [CSD] [CrossRef] [details]
Viljoen, J. A., Visser, H. G., Roodt, A. & Steyn, M. (2009b). Acta Cryst. E65, m1367-m1368.  [CrossRef] [details]
Zherikova, K. V., Baidina, I. A., Morozova, N. B., Kurateva, N. V. & Igumenov, I. K. (2008). J. Struct. Chem. 49, 1098-1103.  [ISI] [CrossRef] [ChemPort]
Zherikova, K. V., Morozova, N. B., Baidina, I. A., Peresypkina, E. V. & Igumenov, I. K. (2006). J. Struct. Chem. 47, 570-574.  [ISI] [CrossRef] [ChemPort]
Zherikova, K. V., Morozova, N. B., Kurateva, N. V., Baidina, I. A., Stabnikov, P. A. & Igumenov, I. K. (2005). J. Struct. Chem. 46, 1039-1046.  [ISI] [CrossRef] [ChemPort]


Acta Cryst (2012). E68, m1344-m1345   [ doi:10.1107/S1600536812042092 ]

This is an open-access article distributed under the terms of the Creative Commons Attribution Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.