(Acetato-κO)(aqua-κO)(2-{bis­[(3,5-dimethyl-1H-pyrazol-1-yl-κN2)methyl]amino-κN}ethanol-κO)nickel(II) perchlorate monohydrate

Zhou, J.; Shu, M.

doi:10.1107/S1600536812007970

Volume 68
Part 4
Page m399
April 2012

Received 16 February 2012
Accepted 22 February 2012
Online 10 March 2012

Key indicators
Single-crystal X-ray study
T = 293 K
Mean (C-C) = 0.008 Å
Disorder in solvent or counterion
R = 0.059
wR = 0.142
Data-to-parameter ratio = 16.3
Details

(Acetato-O)(aqua-O)(2-{bis[(3,5-dimethyl-1H-pyrazol-1-yl-N²)methyl]amino-N}ethanol-O)nickel(II) perchlorate monohydrate

Jia Zhou ^a and Mouhai Shu ^a ^*

^aState Key Laboratory of Metal Matrix Composites, School of Chemistry and Chemical Engineering, Shanghai Jiao Tong University, Shanghai 200240, People's Republic of China
Correspondence e-mail: mhshu@sjtu.edu.cn

In the structure of the title complex, [Ni(CH₃CO₂)(C₁₄H₂₃N₅O)(H₂O)]ClO₄·H₂O, the Ni^II centre has a distorted octahedral environment defined by one O and three N atoms derived from the tetradentate ligand, and two O atoms, one from a water molecule and the other from an acetate anion. The molecules are connected into a three-dimensional architecture by O-HO hydrogen bonds. The perchlorate anion is disordered over two positions; the major component has a site-occupancy factor of 0.525 (19).

Related literature

For the preparation of the tripodal ligand, see: Malachowski et al. (1992). For background to hydrolytic enzymes, see: Koike et al. (1995); Lipscomb & Sträter (1996). For related structures, see: Shin et al. (2011); Sundaravel et al. (2011); Xia et al. (2001).

Experimental

Crystal data

[Ni(C₂H₃O₂)(C₁₄H₂₃N₅O)(H₂O)]ClO₄·H₂O
M_r = 530.61
Monoclinic, P 2₁ /c
a = 9.6055 (11) Å
b = 9.9889 (11) Å
c = 24.258 (3) Å
= 90.284 (2)°
V = 2327.5 (5) Å³
Z = 4
Mo K radiation
= 1.00 mm^-1
T = 293 K
0.43 × 0.37 × 0.21 mm

Data collection

Bruker APEX CCD diffractometer
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 2003) T_min = 0.732, T_max = 1.000
13249 measured reflections
5057 independent reflections
2284 reflections with I > 2(I)
R_int = 0.082

Refinement

R[F² > 2(F²)] = 0.059
wR(F²) = 0.142
S = 0.82
5057 reflections
310 parameters
26 restraints
H atoms treated by a mixture of independent and constrained refinement
_max = 0.66 e Å^-3
_min = -0.50 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O1-H26O3ⁱ	0.86 (1)	1.80 (1)	2.631 (10)	163 (1)
O4-H27O5ⁱⁱ	0.86 (1)	2.03 (1)	2.882 (10)	171 (1)
O4-H28O3	0.86 (1)	1.87 (1)	2.684 (10)	158 (5)
O5-H29O11'	0.86 (1)	1.84 (1)	2.695 (10)	174 (1)
O5-H29O11	0.86 (1)	2.09 (1)	2.940 (10)	168 (1)
O5-H30O12'ⁱⁱⁱ	0.86 (1)	2.59 (1)	3.162 (10)	125 (1)
Symmetry codes: (i) $[-x-1, y+{\script{1\over 2}}, -z+{\script{3\over 2}}]$ ; (ii) x-1, y, z; (iii) -x, -y+2, -z+2.

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL and publCIF (Westrip, 2010).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: TK5060 ).

Acknowledgements

The authors thank Professor D.-J. Xu, Zhejiang University, China, for his helpful suggestions.

References

Bruker (2000). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Koike, T., Kajitani, S., Nakamura, I., Kimura, E. & Shiro, M. (1995). J. Am. Chem. Soc. 117, 1210-1219.
Lipscomb, W. N. & Sträter, N. (1996). Chem. Rev. 96, 2375-2434.
Malachowski, M. R., Davidson, M. G. & Davis, J. D. (1992). Heterocycles, 34, 1227-1230.
Sheldrick, G. M. (2003). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Shin, J. W., Rowthu, S. R., Hyun, M. Y., Song, Y. J., Kim, C., Kim, B. G. & Min, K. S. (2011). Dalton Trans. 40, 5762-5773.
Sundaravel, K., Sankaralingam, M., Suresh, E. & Palaniandavar, M. (2011). Dalton Trans. 40, 8444-8458.
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.
Xia, J., Xu, Y., Li, S., Sun, W., Yu, K. & Tang, W. (2001). Inorg. Chem. 40, 2394-2401.

metal-organic compounds

(Acetato-O)(aqua-O)(2-{bis[(3,5-dimethyl-1H-pyrazol-1-yl-N2)methyl]amino-N}ethanol-O)nickel(II) perchlorate monohydrate