A monoclinic polymorph of di-μ-oxido-bis­({2-[2-(methyl­amino)ethyl­imino­methyl]phenolato-κ3N,N′,O}oxidovanadium(V))

Romanowski, G.; Wera, M.; Sikorski, A.

doi:10.1107/S160053680803328X

Volume 64
Part 12
Pages m1548-m1549
December 2008

Received 9 October 2008
Accepted 13 October 2008
Online 13 November 2008

Key indicators
Single-crystal X-ray study
T = 295 K
Mean (C-C) = 0.005 Å
Disorder in main residue
R = 0.044
wR = 0.106
Data-to-parameter ratio = 12.6
Details

A monoclinic polymorph of di--oxido-bis({2-[2-(methylamino)ethyliminomethyl]phenolato-³N,N',O}oxidovanadium(V))

Grzegorz Romanowski,^a ^* Michal Wera ^a and Artur Sikorski ^a

^aUniversity of Gdansk, Faculty of Chemistry, Sobieskiego 18/19, 80-952 Gdansk, Poland
Correspondence e-mail: greg@chem.univ.gda.pl

A new monoclinic polymorph of the title compound, [V₂(C₁₀H₁₃N₂O)₂O₄], which is a centrosymmetric dimer, crystallizes in space group P2₁/c, whereas the previously known polymorph crystallizes in the orthorhombic space group Pbca [Mokry & Carrano (1993). Inorg. Chem. 32, 6119-6121]. Each V^V atom is six-coordinated by one oxide group, two N atoms and one O atom from the Schiff base ligand, and by two additional bridging O atoms. The two methylene groups are each disordered over two sites, with occupancy factors of 0.776 (14) and 0.224 (14). In the crystal structure, there are C-HO hydrogen bonds and C-H [pi] interactions between the dimers.

Related literature

For general background, see: Butler & Walker (1993); Carter-Franklin et al. (2003); Eady (2003); Evangelou (2002); Mendz (1991); Rehder et al. (2003); Sakurai (2002). For related structures, see: Mokry & Carrano (1993); Rao et al. (1981); Romanowski et al. (2008); Root et al. (1993). For the synthesis, see: Kwiatkowski et al. (2003).

Experimental

Crystal data

[V₂(C₁₀H₁₃N₂O)₂O₄]
M_r = 520.33
Monoclinic, P 2₁ /c
a = 6.6801 (2) Å
b = 11.9955 (6) Å
c = 13.8643 (7) Å
= 92.156 (4)°
V = 1110.18 (9) Å³
Z = 2
Mo K radiation
= 0.89 mm^-1
T = 295 (2) K
0.6 × 0.1 × 0.1 mm

Data collection

Oxford Diffraction Ruby CCD diffractometer
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2006 $[Oxford Diffraction (2006). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]$ ) T_min = 0.532, T_max = 0.915
6336 measured reflections
1960 independent reflections
1288 reflections with I > 2(I)
R_int = 0.050

Refinement

R[F² > 2(F²)] = 0.044
wR(F²) = 0.106
S = 0.90
1960 reflections
155 parameters
H-atom parameters constrained
_max = 0.36 e Å^-3
_min = -0.39 e Å^-3

Table 1
Selected bond lengths (Å)

O7-V14	1.926 (2)
N9-V14	2.158 (3)
N12-V14	2.146 (3)
V14-O16	1.612 (2)
V14-O15	1.674 (2)
V14-O15ⁱ	2.316 (2)
Symmetry code: (i) -x, -y+2, -z.

Table 2
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
C8-H8AO16ⁱⁱ	0.93	2.60	3.520 (4)	170
C11B-H11CCg1ⁱⁱⁱⁱⁱⁱ	0.97	2.82	3.47 (2)	124
Symmetry codes: (ii) x+1, y, z; (iii) $[x, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]$ . Cg1 is the centroid of the C1-C6 ring.

Data collection: CrysAlis CCD (Oxford Diffraction, 2006 $[Oxford Diffraction (2006). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]$ ); cell refinement: CrysAlis RED (Oxford Diffraction, 2006 $[Oxford Diffraction (2006). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]$ ); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97 and PLATON (Spek, 2003).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HY2159 ).

Acknowledgements

The Polish Ministry of Science and Higher Education under grants BW/8000-5-0462-8 and DS/8210-40-086-8 financially supported this work.

References

Butler, A. & Walker, J. V. (1993). Chem. Rev. 93, 1937-1944.
Carter-Franklin, J. N., Parrish, J. D., Tchirret-Guth, R. A., Little, R. D. & Butler, A. (2003). J. Am. Chem. Soc. 125, 3688-3689.
Eady, R. R. (2003). Coord. Chem. Rev. 237, 23-30.
Evangelou, A. M. (2002). Crit. Rev. Oncol. Hematol. 42, 249-265.
Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA.
Kwiatkowski, E., Romanowski, G., Nowicki, W., Kwiatkowski, M. & Suwinska, K. (2003). Polyhedron, 22, 1009-1018.
Mendz, G. L. (1991). Arch. Biochem. Biophys. 291, 201-211.
Mokry, L. M. & Carrano, C. J. (1993). Inorg. Chem. 32, 6119-6121.
Oxford Diffraction (2006). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.
Rao, S. T., Westhof, E. & Sundaralingam, M. (1981). Acta Cryst. A37, 421-425.
Rehder, D., Antoni, G., Licini, G. M., Schulzke, C. & Meier, B. (2003). Coord. Chem. Rev. 237, 53-63.
Romanowski, G., Kwiatkowski, E., Nowicki, W., Kwiatkowski, M. & Lis, T. (2008). Polyhedron, 27, 1601-1609.
Root, C. A., Hoeschele, J. D., Cornman, C. R., Kampf, J. W. & Pecoraro, V. L. (1993). Inorg. Chem. 32, 3855-3861.
Sakurai, H. (2002). Chem. Rec. 2, 237-248.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13.

metal-organic compounds

A monoclinic polymorph of di--oxido-bis({2-[2-(methylamino)ethyliminomethyl]phenolato-3N,N',O}oxidovanadium(V))