Bis(2,2′-bipyridine-κ2N,N′)(maleato-κ2O1,O1′)nickel(II) 7.34-hydrate

Pavlová, A.; Černák, J.; Harms, K.

doi:10.1107/S1600536808036672

Volume 64
Part 12
Pages m1536-m1537
December 2008

Received 22 October 2008
Accepted 7 November 2008
Online 13 November 2008

Key indicators
Single-crystal X-ray study
T = 100 K
Mean (C-C) = 0.002 Å
Disorder in solvent or counterion
R = 0.023
wR = 0.058
Data-to-parameter ratio = 11.7
Details

Bis(2,2'-bipyridine-²N,N')(maleato-²O¹,O^1')nickel(II) 7.34-hydrate

Anna Pavlová,^a Juraj Cernák ^a ^* and Klaus Harms ^b

^aDepartment of Inorganic Chemistry, Institute of Chemistry, P. J. Safárik University, Moyzesova 11, 041 54 Kosice, Slovakia, and ^bFachbereich Chemie der Philipps-Universität Marberg, Hans-Meerwein Strasse, D-35032 Marburg, Germany
Correspondence e-mail: juraj.cernak@upjs.sk

The title compound, [Ni(C₄H₂O₄)(C₁₀H₈N₂)₂]·7.34H₂O, was obtained by crystallization from an aqueous ethanolic reaction mixture containing nickel(II) acetate, maleic acid, bipyridine, sodium hydroxide and ammonia. The asymmetric unit contains one independent complex molecule and 7.34 water molecules occupying eight crystallographically independent positions. Two of these water molecules are disordered. The nickel(II) atom is coordinated in a distorted octahedral geometry by two O atoms from one carboxylate group of the maleato ligand and by four N atoms from two 2,2'-bipyridine (bipy) ligands. The water molecules, along with the O atoms of the uncoordinated carboxylate group, form an extended hydrophilic three-dimensional hydrogen-bonded system with large cavities in which the hydrophobic bipy ligands are located. One H atom of the maleate ligand is involved in a weak hydrogen bond of the C-HO type. Stacking interactions between the pyridyl rings of the bipy ligands [centroid-centroid distance = 3.549 (15) Å] lead to the formation of pairs of complex molecules.

Related literature

For magnetic studies of nickel(II) complexes, see: Boca (2004); Kamieniarz et al. (2007); Paharová et al. (2003); Cernák et al. (2003). Several complexes containing the [Ni(bipy)₂]²⁺ structural motif completed with various anionic ligands including acetato (Holz et al., 1996), oxalato (Roman et al., 1995) and terephtalato (Deng et al., 1992) have been structurally characterized. The maleato ligand can act as a monodentate (Sequeira et al., 1992), bidentate (Zheng & Kong, 2003), tridentate (Xue et al., 2005) or tetradentate (Chen et al., 2003) ligand. For the crystal structure of the similar [Ni(bipy)(mal)(H₂O)₃]·H₂O complex, see: Li et al. (2006). For [Ni(dpa)₂(suc)_0.5]Cl (dpa = 4,4'-dipyridylamine, suc = succinato dianion), which has similar geometric parameters and a similar type of coordination to the title compound, see: Montney et al. (2007). The maleato ligand in {[Zn(H₂O)₄(L₁)Zn(mal)₂]·H₂O}_n, [L₁ = N-(3-pyridyl)-isonicotinamide] has a similar coordination, see: Kumar et al. (2006).

Experimental

Crystal data

[Ni(C₄H₂O₄)(C₁₀H₈N₂)₂]·7.34H₂O
M_r = 617.35
Monoclinic, I 2/a
a = 20.7108 (6) Å
b = 17.4754 (5) Å
c = 15.6460 (6) Å
= 97.767 (3)°
V = 5610.8 (3) Å³
Z = 8
Mo K radiation
= 0.76 mm^-1
T = 100 (2) K
0.36 × 0.18 × 0.16 mm

Data collection

Stoe IPDS diffractometer
Absorption correction: multi-scan (Blessing, 1995) T_min = 0.772, T_max = 0.888
14173 measured reflections
4944 independent reflections
4176 reflections with I > 2(I)
R_int = 0.024

Refinement

R[F² > 2(F²)] = 0.023
wR(F²) = 0.058
S = 0.96
4944 reflections
422 parameters
8 restraints
H atoms treated by a mixture of independent and constrained refinement
_max = 0.26 e Å^-3
_min = -0.24 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O5-H51O6	0.79 (2)	1.99 (3)	2.7864 (16)	178 (3)
O5-H52O3ⁱ	0.86 (3)	1.88 (3)	2.7466 (17)	177 (2)
O6-H61O12ⁱⁱ	0.84 (2)	1.90 (2)	2.7384 (16)	174 (3)
O7-H71O8ⁱⁱⁱ	0.8500 (11)	1.997 (3)	2.844 (2)	174 (2)
O7-H72O9^iv	0.8500 (10)	1.996 (4)	2.8388 (19)	171 (2)
O8-H81AO1	0.8500 (10)	2.539 (14)	3.3576 (18)	162 (4)
O8-H82O5^v	0.850 (9)	1.991 (9)	2.8406 (17)	178 (2)
O8-H81BO8^vi	0.8500 (11)	2.084 (11)	2.918 (3)	167 (4)
O9-H91O4	0.89 (2)	1.87 (3)	2.7516 (16)	173 (2)
O9-H92O1^vii	0.82 (2)	1.96 (3)	2.7701 (16)	173 (2)
O10-H101O3	0.82 (3)	1.88 (3)	2.6905 (17)	168 (3)
O10-H102O11^viii	0.86 (3)	1.89 (3)	2.7409 (19)	177 (3)
O11-H111O5^ix	0.83 (3)	2.03 (3)	2.8333 (19)	161 (2)
O11-H112O9^viii	0.85 (3)	1.95 (3)	2.7752 (18)	162 (2)
O12-H121O10^viii	0.79 (3)	2.00 (3)	2.7844 (18)	172 (2)
O12-H122O10	0.82 (3)	1.97 (3)	2.7839 (18)	170 (2)
C23-H18O7^vii	0.95	2.38	3.288 (2)	159
Symmetry codes: (i) x, y-1, z; (ii) $[x, -y+{\script{3\over 2}}, z+{\script{1\over 2}}]$ ; (iii) $[x, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]$ ; (iv) -x+1, -y+2, -z; (v) x, y+1, z; (vi) $[-x+{\script{3\over 2}}, y, -z+1]$ ; (vii) $[-x+1, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (viii) $[-x+{\script{3\over 2}}, -y+{\script{5\over 2}}, -z+{\script{1\over 2}}]$ ; (ix) $[-x+{\script{3\over 2}}, y+1, -z+1]$ .

Data collection: X-AREA (Stoe & Cie, 2007); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2006); software used to prepare material for publication: SHELXL97.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: RZ2262 ).

Acknowledgements

This work was supported by the Slovak grant agency APVV under contract Nos. APVV-VVCE-0058-07 and APVV-0006-07, and by grant agency VEGA (1/3550/06). The support from P. J. Safárik University (VVGS PF - 18/2008/CH and VVGS 45/07-08) is acknowledged. AP thanks DAAD for the financial support during her stay at Philipps-Universität, Marburg. The authors thank Professor Werner Massa (Philipps Universität, Marburg) for his kind permission to use the diffractometer.

References

Blessing, R. H. (1995). Acta Cryst. A51, 33-38.
Boca, R. (2004). Coord. Chem. Rev., 248, 757-815.
Brandenburg, K. (2006). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Cernák, J., Lipkowski, J., Cizmár, E., Orendácová, A., Orendác, M., Feher, A. & Meisel, M. W. (2003). Solid State Sci. 5, 579-585.
Chen, Y., Liu, P., Wang, J. & Cheng, W.-D. (2003). Acta Cryst. E59, m393-m395.
Deng, Z. L., Shi, J., Jiang, Z. H., Liao, D. Z., Yan, S. P., Wang, G. L., Wang, H. G. & Wang, R. J. (1992). Polyhedron, 11, 885-887.
Holz, R. C., Evdokimov, E. A. & Gobena, F. T. (1996). Inorg. Chem., 35, 3808-3814.
Kamieniarz, G., Haglauer, M., Musial, G., Caramico D'Auria, A., Esposito, F. & Gatteschi, D. (2007). Inorg. Chim. Acta, 360, 3941-3944.
Kumar, D. K., Das, A. & Dastidar, P. (2006). Cryst. Growth Des. 6, 1903-1909.
Li, M., Fu, X. & Wang, C. (2006). Acta Cryst. E62, m865-m866.
Montney, M. R., Krishnan, S. M., Patel, N. M., Supkowski, R. M. & LaDuca, R. L. (2007). Cryst. Growth Des. 7, 1145-1153.
Paharová, J., Cernák, J., Boca, R. & Zák, Z. (2003). Inorg. Chim. Acta, 346, 25-31.
Roman, P., Luque, A., Guzman-Miralles, C. & Beitia, J. I. (1995). Polyhedron, 14, 2863-2869.
Sequeira, A., Rajagopal, H., Gupta, M. P., Vanhouteghem, F., Lenstra, A. T. H. & Geise, H. J. (1992). Acta Cryst. C48, 1192-1197.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Stoe & Cie (2007). X-AREA. Stoe & Cie, Darmstadt, Germany.
Xue, Y. H., Liu, J. G. & Xu, D. J. (2005). J. Coord. Chem. 58, 1071-1076.
Zheng, Y. Q. & Kong, Z. P. (2003). J. Coord. Chem. 56, 967-973.