Tris(1,10-phenanthroline)nickel(II) dichromate tetra­hydrate

Liu, H.-X.

doi:10.1107/S1600536810000802

Volume 66
Part 2
Page m144
February 2010

Received 18 December 2009
Accepted 7 January 2010
Online 13 January 2010

Key indicators
Single-crystal X-ray study
T = 298 K
Mean (C-C) = 0.015 Å
Disorder in solvent or counterion
R = 0.077
wR = 0.218
Data-to-parameter ratio = 13.6
Details

Tris(1,10-phenanthroline)nickel(II) dichromate tetrahydrate

Hai-Xing Liu ^a ^*

^aCollege of Chemistry and Chemical Engineering, Microscale Science Institute, Weifang University, Weifang 261061, People's Republic of China
Correspondence e-mail: haixingliu@tom.com

The asymmetric unit of the title compound, [Ni(C₁₂H₈N₂)₃][Cr₂O₇]·4H₂O, contains one cation, one anion and four water molecules, three of which are disordered over two sites with equal occupancies. In the cation, the metal centre is coordinated by six N atoms from three 1,10-phenanthroline ligands in a distorted octahedral geometry. The [Cr₂O₇]^2- anion exhibits a staggered conformation. The crystal packing is stabilized by intermolecular O-HO hydrogen bonds and [pi] - [pi] interactions, evidenced by short distances of 3.531 (5) Å between the centroids of aromatic rings.

Related literature

For related structures, see: Ejsmont et al. (2002); Suescun et al. (1999); Wang et al. (2007); Wiehl et al. (2008).

Experimental

Crystal data

[Ni(C₁₂H₈N₂)₃][Cr₂O₇]·4H₂O
M_r = 887.39
Monoclinic, C 2/c
a = 26.899 (2) Å
b = 17.8121 (16) Å
c = 17.3656 (18) Å
= 105.274 (2)°
V = 8026.5 (13) Å³
Z = 8
Mo K radiation
= 1.06 mm^-1
T = 298 K
0.14 × 0.12 × 0.11 mm

Data collection

Bruker APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) T_min = 0.866, T_max = 0.892
21223 measured reflections
7229 independent reflections
2790 reflections with I > 2(I)
R_int = 0.129

Refinement

R[F² > 2(F²)] = 0.077
wR(F²) = 0.218
S = 1.06
7229 reflections
532 parameters
H-atom parameters constrained
_max = 0.80 e Å^-3
_min = -0.37 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O14-H14DO10ⁱ	0.85	2.06	2.91 (3)	177
O14-H14CO10ⁱⁱ	0.85	1.75	2.60 (3)	176
O13-H13DO14	0.85	1.76	2.61 (3)	179
O13-H13CO2ⁱⁱⁱ	0.85	1.98	2.83 (2)	176
O12-H12DO9^iv	0.85	2.16	2.99 (2)	165
O12-H12CO14	0.85	2.11	2.93 (3)	165
O10-H10DO11	0.85	1.93	2.78 (3)	171
O10-H10CO1	0.85	1.91	2.751 (17)	172
O9-H9AO12^v	0.85	2.24	2.99 (2)	147
O9-H9DO9^vi	0.85	1.94	2.78 (3)	176
O9-H9CO8	0.85	2.11	2.962 (17)	177
O8-H8DO11^vii	0.85	1.92	2.76 (2)	167
O8-H8CO6	0.85	2.00	2.836 (11)	168
Symmetry codes: (i) $[-x+{\script{3\over 2}}, -y+{\script{1\over 2}}, -z+1]$ ; (ii) $[x-{\script{1\over 2}}, y-{\script{1\over 2}}, z]$ ; (iii) $[-x+{\script{3\over 2}}, y-{\script{1\over 2}}, -z+{\script{3\over 2}}]$ ; (iv) $[x, -y+1, z-{\script{1\over 2}}]$ ; (v) $[x, -y+1, z+{\script{1\over 2}}]$ ; (vi) $[-x+1, y, -z+{\script{3\over 2}}]$ ; (vii) $[-x+{\script{3\over 2}}, -y+{\script{3\over 2}}, -z+1]$ .

Data collection: APEX2 (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: CV2680 ).

References

Bruker (2000). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Ejsmont, K., Wasielewski, M. & Zaleski, J. (2002). Acta Cryst. E58, m200-m202.
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Suescun, L., Mombrú, A. W. & Mariezcurrena, R. A. (1999). Acta Cryst. C55, 1991-1993.
Wang, J.-J., Li, D.-S., Tang, L., Fu, F., Guo, L. & Zhang, Z.-L. (2007). Z. Kristallogr. New Cryst. Struct. 222, 61-63.
Wiehl, L., Schreuer, J. & Haussuhl, E. (2008). Z. Kristallogr. New Cryst. Struct. 223, 82-84.

metal-organic compounds