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Volume 66 
Part 10 
Pages m1295-m1296  
October 2010  

Received 15 September 2010
Accepted 16 September 2010
Online 25 September 2010

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Key indicators
Single-crystal X-ray study
T = 110 K
Mean [sigma](C-C) = 0.004 Å
Disorder in solvent or counterion
R = 0.023
wR = 0.064
Data-to-parameter ratio = 9.3
Details
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(2-Aminobenzoato-[kappa]2O,O')(rac-5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-[kappa]4N,N',N'',N''')nickel(II) perchlorate monohydrate

Guang-Chuan Oua and Seik Weng Ngb*

aDepartment of Biology and Chemistry, Hunan University of Science and Engineering, Yongzhou Hunan 425100, People's Republic of China, and bDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia
Correspondence e-mail: seikweng@um.edu.my

In the title salt, [Ni(C7H6NO2)(C16H36N4)]ClO4·H2O, the NiII cation is O,O'-chelated by the benzoate anion and N,N',N'',N'''-chelated by the macrocycle ligand, confering a distorted octahedral geometry on the metal atom. The complex cations, perchlorate anions and uncoordinated water molecules are linked by N-H...O and O-H...O hydrogen bonds into a three-dimensional network. The perchlorate ion is disordered over two positions in a 0.554 (8):0.446 (8) ratio.

Related literature

For two related structures, see: Ou et al. (2008a[Ou, G.-C., Zhang, M. & Yuan, X.-Y. (2008a). Acta Cryst. E64, m1010.],b[Ou, G.-C., Zhang, M., Yuan, X.-Y. & Dai, Y.-Q. (2008b). Acta Cryst. E64, m1588.]).

[Scheme 1]

Experimental

Crystal data

  • [Ni(C7H6NO2)(C16H36N4)]ClO4·H2O

  • Mr = 596.79

  • Monoclinic, C c

  • a = 9.6452 (5) Å

  • b = 21.5350 (11) Å

  • c = 13.5083 (7) Å

  • [beta] = 90.784 (1)°

  • V = 2805.5 (3) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 0.84 mm-1

  • T = 110 K

  • 0.45 × 0.20 × 0.10 mm
Data collection

  • Bruker SMART APEX diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.818, Tmax = 1.000

  • 6638 measured reflections

  • 3832 independent reflections

  • 3667 reflections with I > 2[sigma](I)

  • Rint = 0.016
Refinement

  • R[F2 > 2[sigma](F2)] = 0.023

  • wR(F2) = 0.064

  • S = 1.08

  • 3832 reflections

  • 410 parameters

  • 142 restraints

  • H atoms treated by a mixture of independent and constrained refinement

  • [Delta][rho]max = 0.25 e Å-3

  • [Delta][rho]min = -0.21 e Å-3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 874 Friedel pairs

  • Flack parameter: -0.012 (9)

Table 1
Selected bond lengths (Å)

Ni1-N1 2.124 (2)
Ni1-N2 2.084 (2)
Ni1-N3 2.138 (2)
Ni1-N4 2.087 (2)
Ni1-O1 2.1659 (17)
Ni1-O2 2.1280 (16)

Table 2
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
N1-H1...O1wi 0.86 (2) 2.15 (2) 2.995 (3) 166 (2)
N2-H2...O5'ii 0.86 (2) 2.35 (2) 3.125 (11) 150 (3)
N3-H3...O1 0.86 (2) 2.49 (3) 2.885 (3) 109 (2)
N4-H4...O6'ii 0.86 (3) 2.40 (2) 3.195 (6) 155 (3)
N5-H51...O2 0.85 (3) 2.13 (3) 2.751 (3) 129 (2)
N5-H52...O4'i 0.85 (1) 2.32 (1) 3.155 (6) 168 (3)
O1w-H11...O1 0.84 (2) 1.96 (2) 2.795 (2) 172 (3)
O1w-H12...O3 0.83 (2) 2.26 (2) 3.077 (9) 167 (3)
O1w-H12...O3' 0.83 (2) 2.09 (2) 2.890 (9) 160 (3)
Symmetry codes: (i) [x, -y+1, z+{\script{1\over 2}}]; (ii) [x-{\script{1\over 2}}, -y+{\script{1\over 2}}, z+{\script{1\over 2}}].

Data collection: SMART (Bruker, 2003[Bruker (2003). SAINT and SMART. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2003[Bruker (2003). SAINT and SMART. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: X-SEED (Barbour, 2001[Barbour, L. J. (2001). J. Supramol. Chem. 1, 189-191.]); software used to prepare material for publication: publCIF (Westrip, 2010[Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.]).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: XU5028 ).

Acknowledgements

We thank the Key Subject Construction Project of Hunan Province (No. 2006-180), the Key Scientific Research Project of Hunan Provincial Education Department (No. 08 A023, 05 C736), the NSF of Hunan Province (09 J J3028) and the University of Malaya for supporting this study.

References

Barbour, L. J. (2001). J. Supramol. Chem. 1, 189-191.  [CrossRef] [ChemPort]
Bruker (2003). SAINT and SMART. Bruker AXS Inc., Madison, Wisconsin, USA.
Flack, H. D. (1983). Acta Cryst. A39, 876-881.  [CrossRef] [details]
Ou, G.-C., Zhang, M. & Yuan, X.-Y. (2008a). Acta Cryst. E64, m1010.  [CrossRef] [details]
Ou, G.-C., Zhang, M., Yuan, X.-Y. & Dai, Y.-Q. (2008b). Acta Cryst. E64, m1588.  [CrossRef] [details]
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.  [ISI] [CrossRef] [ChemPort] [details]

Acta Cryst (2010). E66, m1295-m1296   [ doi:10.1107/S1600536810037116 ]

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