Tetra­kis(5,7-dimethyl­quinolin-8-olato-κ2N,O)zirconium(IV) dimethyl­form­amide disolvate

Steyn, M.; Visser, H.G.; Roodt, A.

doi:10.1107/S1600536812042092

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 (C-C) = 0.005 Å
Disorder in solvent or counterion
R = 0.041
wR = 0.099
Data-to-parameter ratio = 16.6
Details

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

Maryke Steyn,^a ^* Hendrik G. Visser ^a and Andreas Roodt ^a

^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 Zr^IV 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-HO 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); Demakopoulos et al. (1995); Steyn et al. (2008, 2011); Viljoen et al. (2008, 2009a,b; 2010a,b); Zherikova et al. (2005, 2006, 2008). For our ongoing research of structure reactivity relationships in catalysis, separation chemistry and other industrial reaction mechanisms, see: Roodt et al. (2011); Schutte et al. (2011); Brink et al. (2010); Ferreira et al. (2007); Haumann et al. (2004).

Experimental

Crystal data

[Zr(C₁₁H₁₀NO)₄]·2C₃H₇NO
M_r = 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 radiation
= 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) T_min = 0.928, T_max = 0.963
61276 measured reflections
11142 independent reflections
8497 reflections with I > 2(I)
R_int = 0.064

Refinement

R[F² > 2(F²)] = 0.041
wR(F²) = 0.099
S = 1.02
11142 reflections
671 parameters
299 restraints
H-atom parameters constrained
_max = 0.42 e Å^-3
_min = -0.39 e Å^-3
Absolute structure: Flack (1983), 5375 Friedel pairs
Flack parameter: -0.01 (3)

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
C14A-H14EO201ⁱ	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); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg & Putz, 2005); software used to prepare material for publication: WinGX (Farrugia, 1999).

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.
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.
Demakopoulos, I., Klouras, N., Raptopoulou, C. P. & Terzis, A. (1995). Z. Anorg. Allg. Chem. 621, 1761-1766.
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.
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.
Flack, H. D. (1983). Acta Cryst. A39, 876-881.
Haumann, M., Meijboom, R., Moss, J. R. & Roodt, A. (2004). Dalton Trans. pp. 1679-1686.
Roodt, A., Visser, H. G. & Brink, A. (2011). Crystallogr. Rev. 17, 241-280.
Schutte, M., Kemp, G., Visser, H. G. & Roodt, A. (2011). Inorg. Chem. 50, 12486-12498.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Steyn, M., Roodt, A. & Steyl, G. (2008). Acta Cryst. E64, m827.
Steyn, M., Visser, H. G., Roodt, A. & Muller, T. J. (2011). Acta Cryst. E67, m1240-m1241.
Viljoen, J. A., Muller, A. & Roodt, A. (2008). Acta Cryst. E64, m838-m839.
Viljoen, J. A., Visser, H. G. & Roodt, A. (2010a). Acta Cryst. E66, m603-m604.
Viljoen, J. A., Visser, H. G. & Roodt, A. (2010b). Acta Cryst. E66, m1053-m1054.
Viljoen, J. A., Visser, H. G., Roodt, A. & Steyn, M. (2009a). Acta Cryst. E65, m1514-m1515.
Viljoen, J. A., Visser, H. G., Roodt, A. & Steyn, M. (2009b). Acta Cryst. E65, m1367-m1368.
Zherikova, K. V., Baidina, I. A., Morozova, N. B., Kurateva, N. V. & Igumenov, I. K. (2008). J. Struct. Chem. 49, 1098-1103.
Zherikova, K. V., Morozova, N. B., Baidina, I. A., Peresypkina, E. V. & Igumenov, I. K. (2006). J. Struct. Chem. 47, 570-574.
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.