μ-Acetato-aqua-μ-(5-bromo-2-{1,3-bis­[2-(5-bromo-2-oxidobenzyl­idene­amino)­eth­yl]imidazolidin-2-yl}phenolato)methano­ldinickel(II) methanol disolvate monohydrate

Khan, A.R.; Tesema, Y.; Butcher, R.J.; Gultneh, Y.

doi:10.1107/S1600536811035409

Volume 67
Part 10
Pages m1381-m1382
October 2011

Received 10 August 2011
Accepted 30 August 2011
Online 14 September 2011

Key indicators
Single-crystal X-ray study
T = 168 K
Mean (C-C) = 0.007 Å
R = 0.041
wR = 0.092
Data-to-parameter ratio = 18.2
Details

-Acetato-aqua--(5-bromo-2-{1,3-bis[2-(5-bromo-2-oxidobenzylideneamino)ethyl]imidazolidin-2-yl}phenolato)methanoldinickel(II) methanol disolvate monohydrate

Ahmed Raza Khan,^a Yohannes Tesema,^a Ray J. Butcher ^a ^* and Yilma Gultneh ^a

^aDepartment of Chemistry, Howard University, 525 College Street NW, Washington, DC 20059, USA
Correspondence e-mail: rbutcher99@yahoo.com

The crystal structure of the title compound, [Ni₂(C₂₇H₂₄Br₃N₄O₃)(CH₃CO₂)(CH₃OH)(H₂O)]·2CH₃OH·H₂O contains [L(OAc){(CH₃OH)Ni}{(H₂O)Ni}] molecules {H₃L = 2-(5-bromo-2-hydroxyphenyl)-1,3-bis[4-(5-bromo-2-hydroxyphenyl)-3-azabut-3-enyl]-1,3-imidazolidine} with additional water and two methanol solvent molecules. In this instance, one of the two Ni atoms is coordinated to a water and the other to a methanol molecule. The Ni-O and Ni-N distances, as well as the angles about the metal atoms, show quite regular octahedra around the central ions. The Ni-O_phenol-Ni and Ni-O_acetate-Ni angles are not similar [95.26 (13) and 97.34 (13)°, respectively], indicating that this subtle solvate exchange induces significant differences in the conformation adopted. The coordinated methanol ligand is involved in an intramolecular hydrogen bond to the uncoordinated O atom of the bridging acetate ligand, while the coordinated water molecule forms a hydrogen bond with the one of the methanol solvent molecules. The water solvent molecule forms strong hydrogen bonds to both phenolate O atoms. The remaining methanol solvent molecule also forms a hydrogen bond with this solvent water molecule.

Related literature

For nickel complexes of similar ligands, see: Fondo et al. (2005, 2006a,b, 2007, 2009); Khan et al. (2011); Lu et al. (2007); Paital et al. (2007, 2009).

Experimental

Crystal data

[Ni₂(C₂₇H₂₄Br₃N₄O₃)(C₂H₃O₂)(CH₄O)(H₂O)]·2CH₄O·H₂O
M_r = 1000.85
Orthorhombic, P n a 2₁
a = 14.7385 (16) Å
b = 18.552 (2) Å
c = 14.2504 (15) Å
V = 3896.4 (7) Å³
Z = 4
Mo K radiation
= 4.10 mm^-1
T = 168 K
0.49 × 0.12 × 0.06 mm

Data collection

Bruker SMART 1000 CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2000) T_min = 0.676, T_max = 1.000
25239 measured reflections
8737 independent reflections
6627 reflections with I > 2(I)
R_int = 0.054

Refinement

R[F² > 2(F²)] = 0.041
wR(F²) = 0.092
S = 0.96
8737 reflections
479 parameters
7 restraints
H atoms treated by a mixture of independent and constrained refinement
_max = 0.71 e Å^-3
_min = -0.73 e Å^-3
Absolute structure: Flack (1983), 3686 Friedel pairs
Flack parameter: 0.007 (8)

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O1W-H1W1O2Wⁱ	0.80 (2)	2.01 (2)	2.810 (5)	174 (5)
O1W-H1W2O3M	0.82 (2)	1.97 (3)	2.770 (5)	164 (5)
O2W-H2W1O1B	0.80 (2)	1.86 (3)	2.631 (5)	160 (6)
O2W-H2W2O1A	0.83 (2)	1.91 (2)	2.744 (5)	177 (6)
O1M-H1MO2AA	0.84	1.77	2.602 (5)	174
O2M-H2MO2W	0.84	1.89	2.725 (5)	172
O3M-H3MO2Mⁱ	0.84	1.96	2.753 (6)	158
Symmetry code: (i) $[x-{\script{1\over 2}}, -y+{\script{3\over 2}}, z]$ .

Data collection: SMART (Bruker, 2000); cell refinement: SAINT-Plus (Bruker, 2000); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: WM2523 ).

Acknowledgements

RJB wishes to acknowledge the NSF-MRI program (grant CHE-0619278) for funds to purchase the diffractometer. ARK and YT wish to acknowledge the Howard University Graduate School of Arts & Sciences for the award of Teaching Assistanceships.

References

Bruker (2000). SADABS, SMART and SAINT-Plus. Bruker AXS Inc., Madison, Wisconsin, USA.
Flack, H. D. (1983). Acta Cryst. A39, 876-881.
Fondo, M., Garcia-Deibe, A. M., Corbella, M., Ruiz, E., Tercero, J., Sanmartin, J. & Bermejo, M. R. (2005). Inorg. Chem. 44, 5011-5020.
Fondo, M., Garcia-Deibe, A. M., Ocampo, N., Sanmartin, J. & Bermejo, M. R. (2007). Dalton Trans. pp. 414-416.
Fondo, M., Garcia-Deibe, A. M., Ocampo, N., Sanmartin, J., Bermejo, M. R. & Llamas-Saiz, A. L. (2006a). Dalton Trans. pp. 4260-4270.
Fondo, M., Ocampo, N., Garcia-Deibe, A. M., Ruiz, E., Tercero, J. & Sanmartin, J. (2009). Inorg. Chem. 48, 9861-9873.
Fondo, M., Ocampo, N., Garcia-Deibe, A. M., Vicente, R., Corbella, M., Bermejo, M. R. & Sanmartin, J. (2006b). Inorg. Chem. 45, 255-262.
Khan, A. R., Tesema, Y., Butcher, R. J. & Gultneh, Y. (2011). Acta Cryst. E67, m1264-m1265.
Lu, L.-P., Lu, X.-P. & Zhu, M.-L. (2007). Acta Cryst. C63, m374-m376.
Paital, A. R., Ribas, J., Barrios, L. A., Aromi, G. & Ray, D. (2009). Dalton Trans. pp. 256-258.
Paital, A. R., Wong, W. T., Aromi, G. & Ray, D. (2007). Inorg. Chem. 46, 5727-5733.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.

metal-organic compounds