Aqua­[1-(1,10-phenanthrolin-2-yl-κ2N,N′)-1H-pyrazol-3-amine-κN2](sulfato-κO)copper(II) methanol monosolvate dihydrate

Yuan, L.; Lian, L.S.; Hui, C.Y.; Xia, Z.Y.; Min, S.J.

doi:10.1107/S1600536812014134

Volume 68
Part 5
Pages m558-m559
May 2012

Received 12 March 2012
Accepted 1 April 2012
Online 13 April 2012

Key indicators
Single-crystal X-ray study
T = 298 K
Mean (C-C) = 0.005 Å
R = 0.047
wR = 0.119
Data-to-parameter ratio = 15.6
Details

Aqua[1-(1,10-phenanthrolin-2-yl-²N,N')-1H-pyrazol-3-amine-N²](sulfato-O)copper(II) methanol monosolvate dihydrate

Liang Yuan,^a Liu Shu Lian,^b Chi Yan Hui,^a Zhao Yan Xia ^c and Shi Jing Min ^a ^*

^aCollege of Chemistry, Chemical Engineering and Materials Science, Shandong Normal University, Jinan 250014, People's Republic of China,^bSchool for Cadres of Shandong Bureau of Quality and Technical Supervision, Jinan 250014, People's Republic of China, and ^cShandong Academy of Medical Science Graduate Education Center, Jinan 250062, People's Republic of China
Correspondence e-mail: shijingmin1955@gmail.com

In the title compound, [Cu(SO₄)(C₁₅H₁₁N₅)(H₂O)]·CH₃OH·2H₂O, the Cu^II ion is in a distorted square-pyramidal geometry, in which three N atoms from the chelating 1-(1,10-phenanthrolin-2-yl)-1H-pyrazol-3-amine ligand and one O atom from a sulfate anion define the basal plane and the O atom from the coordinating water molecule is located at the apex. In the crystal, hydrogen-bonding interactions involving the coordinating and solvent water molecules, the methanol solvent molecule and the amine group (one with an intramolecular interaction to one of the sulfate O atoms) of the complex are observed. [pi] - [pi] interactions between symmetry-related phenantroline moieties, with a shortest centroid-centroid interaction of 3.573 (2)°, are also present.

Related literature

For related structures, see: Li et al. (2011a,b).

Experimental

Crystal data

[Cu(SO₄)(C₁₅H₁₁N₅)(H₂O)]·CH₄O·2H₂O
M_r = 506.98
Monoclinic, P 2₁ /n
a = 8.0190 (13) Å
b = 18.489 (3) Å
c = 14.086 (2) Å
= 104.551 (2)°
V = 2021.4 (6) Å³
Z = 4
Mo K radiation
= 1.24 mm^-1
T = 298 K
0.22 × 0.15 × 0.11 mm

Data collection

Bruker SMART APEX CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) T_min = 0.772, T_max = 0.876
11702 measured reflections
4394 independent reflections
3434 reflections with I > 2(I)
R_int = 0.038

Refinement

R[F² > 2(F²)] = 0.047
wR(F²) = 0.119
S = 1.03
4394 reflections
281 parameters
H-atom parameters constrained
_max = 0.52 e Å^-3
_min = -0.31 e Å^-3

Table 1
Selected bond lengths (Å)

Cu1-O3	1.906 (2)
Cu1-N2	1.934 (2)
Cu1-N3	2.068 (2)
Cu1-N1	2.090 (2)
Cu1-O5	2.220 (2)

Table 2
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O5-H4O7	0.89	1.79	2.671 (4)	167
O5-H5O8	0.89	1.90	2.774 (4)	164
O6-H12O1	0.85	1.89	2.668 (4)	152
O7-H6O6	0.84	2.10	2.878 (5)	153
O7-H7O4ⁱ	0.89	1.84	2.726 (4)	173
O8-H17O6ⁱⁱ	0.90	2.07	2.906 (5)	154
O8-H18O2ⁱⁱⁱ	0.90	2.09	2.957 (4)	163
N5-H5AO4	0.86	2.19	2.916 (4)	143
N5-H5BO2ⁱⁱ	0.86	2.17	3.022 (4)	175
Symmetry codes: (i) x-1, y, z; (ii) $[x+{\script{1\over 2}}, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]$ ; (iii) $[x-{\script{1\over 2}}, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]$ .

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT (Bruker, 200); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: WM2604 ).

Acknowledgements

The authors thank the Natural Science Foundation of Shandong Province of China (No. ZR2009BM026).

References

Bruker (1997). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2000). SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Li, H., Zhang, S. D., Xie, L. M., Yu, L. & Shi, J. M. (2011a). J. Coord. Chem. 64, 1456-1468.
Li, H., Zhang, S. D., Xie, L. M., Yu, L. & Shi, J. M. (2011b). J. Coord. Chem. 64, 3595-3608.
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.

metal-organic compounds

Aqua[1-(1,10-phenanthrolin-2-yl-2N,N')-1H-pyrazol-3-amine-N2](sulfato-O)copper(II) methanol monosolvate dihydrate