Bis(1,10-phenanthroline-κ2N,N′)(sulfato-κ2O,O′)nickel(II) butane-2,3-diol monosolvate

Zhong, K.-L.; Ni, C.

doi:10.1107/S1600536812047241

Volume 68
Part 12
Page m1519
December 2012

Received 8 November 2012
Accepted 16 November 2012
Online 24 November 2012

Key indicators
Single-crystal X-ray study
T = 223 K
Mean (C-C) = 0.006 Å
Disorder in solvent or counterion
R = 0.047
wR = 0.108
Data-to-parameter ratio = 11.1
Details

Bis(1,10-phenanthroline-²N,N')(sulfato-²O,O')nickel(II) butane-2,3-diol monosolvate

Kai-Long Zhong ^a ^* and Chao Ni ^a

^aDepartment of Applied Chemistry, Nanjing College of Chemical Technology, Nanjing, 210048, People's Republic of China
Correspondence e-mail: zklong76@163.com

In the title compound, [Ni(SO₄)(C₁₂H₈N₂)₂]·C₄H₁₀O₂, the Ni^II ion is six-coordinated by four N atoms from two chelating 1,10-phenanthroline ligands and two O atoms from an O,O'-bidentate sulfate anion, resulting in a distorted octahedral geometry for the metal ion. The dihedral angle between the two chelating N₂C₂ groups is 83.82 (12)°. The Ni^II ion, the S atom and the mid-point of the central C-C bond of the butane-2,3-diol solvent molecule lie on a twofold rotation axis. In the crystal, the complex molecules and solvent molecules are held together by pairs of symmetry-related O_diol-HO_sulfate hydrogen bonds involving the uncoordinating O atoms of the sulfate ions. The solvent molecule is disordered over two sets of sites with site occupancies of 0.450 (9) and 0.550 (9).

Related literature

For the ethane-1,2-diol analog of the title complex, see: Zhong et al. (2009). For the propane-1,3-diol analog of the title complex, see: Ni et al. (2010). For an isotypic structure, see: Wang & Zhong (2011).

Experimental

Crystal data

[Ni(SO₄)(C₁₂H₈N₂)₂]·C₄H₁₀O₂
M_r = 605.29
Monoclinic, C 2/c
a = 18.147 (4) Å
b = 13.051 (3) Å
c = 13.259 (3) Å
= 122.43 (3)°
V = 2650.5 (14) Å³
Z = 4
Mo K radiation
= 0.86 mm^-1
T = 223 K
0.35 × 0.30 × 0.20 mm

Data collection

Rigaku Mercury CCD diffractometer
Absorption correction: multi-scan (REQAB: Jacobson, 1998) T_min = 0.736, T_max = 1.000
6326 measured reflections
2325 independent reflections
1964 reflections with I > 2(I)
R_int = 0.035

Refinement

R[F² > 2(F²)] = 0.047
wR(F²) = 0.108
S = 1.14
2325 reflections
210 parameters
56 restraints
H-atom parameters constrained
_max = 0.39 e Å^-3
_min = -0.39 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O3-H3AO2	0.82	1.97	2.729 (7)	154
O3'-H3'AO2	0.82	2.03	2.769 (8)	150

Data collection: CrystalClear (Rigaku, 2007); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in 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: MW2096 ).

Acknowledgements

This work was supported by the Scientific Research Foundation of Nanjing College of Chemical Technology (grant No. NHKY-2010-17).

References

Jacobson, R. (1998). REQAB. Molecular Structure Corporation, The Woodlands, Texas, USA.
Ni, C., Zhong, K.-L. & Cui, J.-D. (2010). Acta Cryst. E66, m746-m747.
Rigaku (2007). CrystalClear. Rigaku Corporation, Tokyo, Japan.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Wang, S.-J. & Zhong, K.-L. (2011). Acta Cryst. E67, m446.
Zhong, K.-L., Ni, C. & Wang, J.-M. (2009). Acta Cryst. E65, m911.

metal-organic compounds

Bis(1,10-phenanthroline-2N,N')(sulfato-2O,O')nickel(II) butane-2,3-diol monosolvate