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

Hu, A.-Y.; Yu, D.-Y.; Yuan, A.-H.

doi:10.1107/S1600536813003632

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 (C-C) = 0.006 Å
Disorder in solvent or counterion
R = 0.058
wR = 0.155
Data-to-parameter ratio = 14.0
Details

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

Ai-Yun Hu,^a Deng-Yong Yu ^a and Ai-Hua Yuan ^a ^*

^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-HO, O-HN, N-HO and N-HN 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); Tokoro & Ohkoshi (2011). For related structures, see: Qian et al. (2011); Shatruk et al. (2007).

Experimental

Crystal data

(C₁₆H₁₇N₂)₃[Co(CN)₆]·5H₂O
M_r = 1017.08
Triclinic, $[P \overline 1]$
a = 12.836 (2) Å
b = 14.458 (2) Å
c = 16.645 (3) Å
= 97.216 (2)°
= 110.934 (2)°
= 112.179 (2)°
V = 2547.6 (7) Å³
Z = 2
Mo K radiation
= 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) T_min = 0.939, T_max = 0.950
19411 measured reflections
9402 independent reflections
6096 reflections with I > 2(I)
R_int = 0.046

Refinement

R[F² > 2(F²)] = 0.058
wR(F²) = 0.155
S = 1.05
9402 reflections
671 parameters
2 restraints
H-atom parameters constrained
_max = 0.49 e Å^-3
_min = -0.53 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O1-H1AO5'	0.82	1.84	2.616 (7)	157
O1-H1AO5	0.82	2.02	2.823 (8)	165
O1-H1BN5ⁱ	0.82	2.27	3.068 (4)	163
O2-H2AN3ⁱⁱ	0.82	2.25	3.044 (4)	164
O2-H2BN3	0.82	2.09	2.901 (4)	169
O3-H3AN2	0.82	2.11	2.909 (4)	163
O3-H3BO2ⁱⁱ	0.82	2.01	2.813 (3)	168
O4-H4AO3	0.82	1.89	2.707 (3)	173
O4-H4BO1	0.82	1.94	2.735 (4)	164
N8-H8NO4ⁱⁱⁱ	0.95	1.72	2.636 (4)	161
N9-H9NN5^iv	0.95	2.14	2.919 (4)	138
N11-H11NN4ⁱ	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); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL; molecular graphics: DIAMOND (Brandenburg, 2006); 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.
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.
Shatruk, M., Chambers, K. E., Prosvirin, A. V. & Dunbar, K. R. (2007). Inorg. Chem. 46, 5155-5165.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Tokoro, H. & Ohkoshi, S. (2011). Dalton Trans. 40, 6825-6833.

metal-organic compounds