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Volume 69 
Part 1 
Pages m40-m41  
January 2013  

Received 30 November 2012
Accepted 6 December 2012
Online 12 December 2012

Key indicators
Single-crystal X-ray study
T = 223 K
Mean [sigma](C-C) = 0.015 Å
Disorder in main residue
R = 0.046
wR = 0.135
Data-to-parameter ratio = 10.2
Details
Open access

Bis(1,10-phenanthroline-[kappa]2N,N')(sulfato-O)copper(II) butane-2,3-diol monosolvate

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

The title compound, [Cu(SO4)(C12H8N2)2]·C4H10O2, is comprised of neutral monomeric complex and butane-2,3-diol solvent molecules. In the complex, the CuII ion is in a distorted square-pyramidal coordination environment defined by four N atoms from two chelating 1,10-phenanthroline ligands and one O atom from a monodentate sulfate anion; the O atom is at the apex. The two chelating N2C2 groups subtend a dihedral angle of 85.8 (4)°. In the crystal, the neutral monomeric complex and butane-2,3-diol solvent molecules are held together by O-H...O hydrogen bonding, which leads to additional stabilization of the structure. The presence of pseudosymmetry in the structure suggests the higher symmetry space group C2/c, but attempts to refine the structure in this space group resulted in an unsatisfactory model and high R and wR values. The sulfate anion is disordered over two sets of sites with occupancies of 0.55 (1) and 0.45 (1).

Related literature

For the ethane-1,2-diol solvate of the title complex, see: Zhong (2011a[Zhong, K.-L. (2011a). Acta Cryst. E67, m1215-m1216.]), for the propane-1,2-diol solvate, see: Zhong (2011b[Zhong, K.-L. (2011b). Z. Kristallogr. New Cryst. Struct. 226, 286-288.]) and for the propane-1,3-diol solvate, see: Zhong (2012[Zhong, K.-L. (2012). Acta Cryst. E68, m1555.]). For related structures of transition metal complexes with a sulfate anion, see: Wang & Zhong (2011[Wang, S.-J. & Zhong, K.-L. (2011). Acta Cryst. E67, m446.]); Zhong & Ni (2012[Zhong, K.-L. & Ni, C. (2012). Acta Cryst. E68, m1519.]); Cui et al. (2010[Cui, J.-D., Zhong, K.-L. & Liu, Y.-Y. (2010). Acta Cryst. E66, m564.]); Lu et al. (2006[Lu, W.-J., Zhong, K.-L. & Zhu, Y.-M. (2006). Acta Cryst. E62, m891-m893.]).

[Scheme 1]

Experimental

Crystal data
  • [Cu(SO4)(C12H8N2)2]·C4H10O2

  • Mr = 610.13

  • Monoclinic, C c

  • a = 17.352 (4) Å

  • b = 13.070 (3) Å

  • c = 13.444 (3) Å

  • [beta] = 123.84 (3)°

  • V = 2532.4 (13) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 1.00 mm-1

  • T = 223 K

  • 0.32 × 0.27 × 0.21 mm

Data collection
  • Rigaku Mercury CCD diffractometer

  • Absorption correction: multi-scan (REQAB; Jacobson, 1998[Jacobson, R. (1998). REQAB. Molecular Structure Corporation, The Woodlands, Texas, USA.]) Tmin = 0.741, Tmax = 0.818

  • 7154 measured reflections

  • 4178 independent reflections

  • 3542 reflections with I > 2[sigma](I)

  • Rint = 0.026

Refinement
  • R[F2 > 2[sigma](F2)] = 0.046

  • wR(F2) = 0.135

  • S = 0.99

  • 4178 reflections

  • 408 parameters

  • 124 restraints

  • H-atom parameters constrained

  • [Delta][rho]max = 0.60 e Å-3

  • [Delta][rho]min = -0.53 e Å-3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 1317 Friedel pairs

  • Flack parameter: 0.55 (2)

Table 1
Selected bond lengths (Å)

Cu1-O1 1.922 (11)
Cu1-O1' 1.944 (10)
Cu1-N1 2.000 (7)
Cu1-N4 2.014 (7)
Cu1-N3 2.091 (6)
Cu1-N2 2.186 (7)

Table 2
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
O5-H5B...O3 0.82 1.92 2.73 (2) 172
O5-H5B...O4' 0.82 2.01 2.83 (2) 176
O6-H6...O3' 0.82 2.19 2.919 (16) 148
O6-H6...O4 0.82 1.95 2.720 (14) 156

Data collection: CrystalClear (Rigaku, 2007[Rigaku (2007). CrystalClear. Rigaku Corporation, Tokyo, Japan.]); cell refinement: CrystalClear (Rigaku, 2007[Rigaku (2007). CrystalClear. Rigaku Corporation, Tokyo, Japan.]); data reduction: CrystalClear (Rigaku, 2007[Rigaku (2007). CrystalClear. Rigaku Corporation, Tokyo, Japan.]); 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: XP in SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BQ2380 ).


Acknowledgements

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

References

Cui, J.-D., Zhong, K.-L. & Liu, Y.-Y. (2010). Acta Cryst. E66, m564.  [CSD] [CrossRef] [details]
Flack, H. D. (1983). Acta Cryst. A39, 876-881.  [CrossRef] [details]
Jacobson, R. (1998). REQAB. Molecular Structure Corporation, The Woodlands, Texas, USA.
Lu, W.-J., Zhong, K.-L. & Zhu, Y.-M. (2006). Acta Cryst. E62, m891-m893.  [CSD] [CrossRef] [details]
Rigaku (2007). CrystalClear. Rigaku Corporation, Tokyo, Japan.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Wang, S.-J. & Zhong, K.-L. (2011). Acta Cryst. E67, m446.  [CSD] [CrossRef] [details]
Zhong, K.-L. (2011a). Acta Cryst. E67, m1215-m1216.  [CSD] [CrossRef] [details]
Zhong, K.-L. (2011b). Z. Kristallogr. New Cryst. Struct. 226, 286-288.  [ChemPort]
Zhong, K.-L. (2012). Acta Cryst. E68, m1555.  [CSD] [CrossRef] [details]
Zhong, K.-L. & Ni, C. (2012). Acta Cryst. E68, m1519.  [CSD] [CrossRef] [details]


Acta Cryst (2013). E69, m40-m41   [ doi:10.1107/S1600536812049951 ]

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