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Volume 69 
Part 3 
Page m142  
March 2013  

Received 31 January 2013
Accepted 5 February 2013
Online 9 February 2013

Key indicators
Single-crystal X-ray study
T = 173 K
Mean [sigma](C-C) = 0.006 Å
Disorder in solvent or counterion
R = 0.058
wR = 0.155
Data-to-parameter ratio = 14.0
Details
Open access

Tris(3,4,7,8-tetramethyl-1,10-phenanthrolin-1-ium) hexacyanidocobaltate(III) pentahydrate

aSchool of Biology and Chemical Engineering, Jiangsu University of Science and Technology, Zhenjiang 212003, People's Republic of China
Correspondence e-mail: aihuayuan@163.com

The structure of the title compound, (C16H17N2)3[Co(CN)6]·5H2O, consists of three 3,4,7,8-tetramethyl-1,10-phenanthrolin-1-ium cations, a [Co(CN)6]3- anion and five water molecules of crystallization, one of which is disordered over two sets of sites in a 0.587 (15):0.413 (15) ratio. The [Co(CN)6]3- anion exhibits an octahedral geometry. In the structure, cations and anions are linked alternatively through O-H...O, O-H...N, N-H...O and N-H...N hydrogen bonds, [pi]-[pi] interactions [centroid-centroid distances = 3.523 (2)-4.099 (2) Å] and van der Waals forces, forming a three-dimensional supramolecular network.

Related literature

For general background to hexacyanidometallate-based compounds, see: Andruh et al. (2009[Andruh, M., Costes, J. P., Diaz, C. & Gao, S. (2009). Inorg. Chem. 48, 3342-3359.]); Tokoro & Ohkoshi (2011[Tokoro, H. & Ohkoshi, S. (2011). Dalton Trans. 40, 6825-6833.]). For related structures, see: Qian et al. (2011[Qian, S. Y., Zhou, H., Yuan, A. H. & Song, Y. (2011). Cryst. Growth Des. 11, 5676-5681.]); Shatruk et al. (2007[Shatruk, M., Chambers, K. E., Prosvirin, A. V. & Dunbar, K. R. (2007). Inorg. Chem. 46, 5155-5165.]).

[Scheme 1]

Experimental

Crystal data
  • (C16H17N2)3[Co(CN)6]·5H2O

  • Mr = 1017.08

  • Triclinic, [P \overline 1]

  • a = 12.836 (2) Å

  • b = 14.458 (2) Å

  • c = 16.645 (3) Å

  • [alpha] = 97.216 (2)°

  • [beta] = 110.934 (2)°

  • [gamma] = 112.179 (2)°

  • V = 2547.6 (7) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 0.40 mm-1

  • T = 173 K

  • 0.16 × 0.15 × 0.13 mm

Data collection
  • Bruker SMART APEX CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2004[Bruker (2004). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.939, Tmax = 0.950

  • 19411 measured reflections

  • 9402 independent reflections

  • 6096 reflections with I > 2[sigma](I)

  • Rint = 0.046

Refinement
  • R[F2 > 2[sigma](F2)] = 0.058

  • wR(F2) = 0.155

  • S = 1.05

  • 9402 reflections

  • 671 parameters

  • 2 restraints

  • H-atom parameters constrained

  • [Delta][rho]max = 0.49 e Å-3

  • [Delta][rho]min = -0.53 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
O1-H1A...O5' 0.82 1.84 2.616 (7) 157
O1-H1A...O5 0.82 2.02 2.823 (8) 165
O1-H1B...N5i 0.82 2.27 3.068 (4) 163
O2-H2A...N3ii 0.82 2.25 3.044 (4) 164
O2-H2B...N3 0.82 2.09 2.901 (4) 169
O3-H3A...N2 0.82 2.11 2.909 (4) 163
O3-H3B...O2ii 0.82 2.01 2.813 (3) 168
O4-H4A...O3 0.82 1.89 2.707 (3) 173
O4-H4B...O1 0.82 1.94 2.735 (4) 164
N8-H8N...O4iii 0.95 1.72 2.636 (4) 161
N9-H9N...N5iv 0.95 2.14 2.919 (4) 138
N11-H11N...N4i 0.95 2.11 2.799 (4) 128
Symmetry codes: (i) x, y+1, z; (ii) -x+1, -y+1, -z+1; (iii) x+1, y, z; (iv) -x+2, -y+1, -z+1.

Data collection: SMART (Bruker, 2004[Bruker (2004). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2004[Bruker (2004). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXTL; molecular graphics: DIAMOND (Brandenburg, 2006[Brandenburg, K. (2006). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: SHELXTL.


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: RZ5042 ).


References

Andruh, M., Costes, J. P., Diaz, C. & Gao, S. (2009). Inorg. Chem. 48, 3342-3359.  [ISI] [CrossRef] [PubMed] [ChemPort]
Brandenburg, K. (2006). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Bruker (2004). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Qian, S. Y., Zhou, H., Yuan, A. H. & Song, Y. (2011). Cryst. Growth Des. 11, 5676-5681.  [CSD] [CrossRef] [ChemPort]
Shatruk, M., Chambers, K. E., Prosvirin, A. V. & Dunbar, K. R. (2007). Inorg. Chem. 46, 5155-5165.  [ISI] [CSD] [CrossRef] [PubMed] [ChemPort]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Tokoro, H. & Ohkoshi, S. (2011). Dalton Trans. 40, 6825-6833.  [CrossRef] [ChemPort] [PubMed]


Acta Cryst (2013). E69, m142  [ doi:10.1107/S1600536813003632 ]

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