catena-Poly[dieth­yl(2-hydroxy­ethyl)­ammonium [[tetra-μ-acetato-κ8O:O′-dicuprate(II)(Cu—Cu)]-μ-acetato-κ2O:O′] dichloro­methane solvate]

Shahid, M.; Mazhar, M.; O'Brien, P.; Afzaal, M.; Raftery, J.

doi:10.1107/S1600536808044048

Volume 65
Part 2
Pages m163-m164
February 2009

Received 20 November 2008
Accepted 27 December 2008
Online 8 January 2009

Key indicators
Single-crystal X-ray study
T = 100 K
Mean (C-C) = 0.005 Å
R = 0.034
wR = 0.080
Data-to-parameter ratio = 19.4
Details

catena-Poly[diethyl(2-hydroxyethyl)ammonium [[tetra--acetato-⁸O:O'-dicuprate(II)(Cu-Cu)]--acetato-²O:O'] dichloromethane solvate]

Muhammad Shahid,^a Muhammad Mazhar,^a ^* Paul O'Brien,^b Mohammad Afzaal ^b and James Raftery ^b

^aDepartment of Chemistry, Quaid-i-Azam University, Islamabad 45320, Pakistan, and ^bThe School of Chemistry, The University of Manchester, Oxford Road, Manchester M13 9PL, England
Correspondence e-mail: mazhar42pk@yahoo.com

The title compound, {(C₆H₁₆NO)[Cu₂(CH₃COO)₅]·CH₂Cl₂}_n, consists of acetate-bridged Cu₂(CH₃COO)₄ units that are connected via another acetate anion at each terminus to form infinite anionic [{Cu₂(CH₃COO)₄}(CH₃COO)]_n chains along [100]. The connecting acetate is hydrogen bonded to the diethyl(2-hydroxyethyl)ammonium cation, and the dichloromethane solvent molecule fills the remaining voids in the structure. The O-Cu-Cu angles along the polymeric chain are nearly linear [175.49 (5)°], but individual O-Cu-Cu-O units along the chain are bent and rotated against each other at the bridging acetate ion. Translation of each Cu₂(CH₃COO)₄ unit along the chain, represented by the least-squares plane of the two copper ions along with four of the acetate O atoms, rotated these units by 35.16 (3)°.

Related literature

Shahid, Mazhar, Helliwell et al. (2008) describe the study of dinuclear Cu complexes; Van Niekerk & Schoening (1953) provide X-ray evidence for Cu-Cu bonds in cupric acetate; Brown & Chidambaram (1973) report the redetermination of the structure of cupric acetate by neutron-diffraction; Shahid, Mazhar, Malik et al. (2008); Hamid et al. (2007) and Zhang et al. (2004) describe geometric parameters of organo-copper complexes.

Experimental

Crystal data

(C₆H₁₆NO)[Cu₂(C₂H₃O₂)₅]·CH₂Cl₂
M_r = 625.42
Orthorhombic, P n a 2₁
a = 17.6366 (11) Å
b = 12.1078 (8) Å
c = 11.9148 (7) Å
V = 2544.3 (3) Å³
Z = 4
Mo K radiation
= 1.94 mm^-1
T = 100 (2) K
0.40 × 0.40 × 0.10 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2001) T_min = 0.657, T_max = 0.830
21202 measured reflections
5939 independent reflections
5693 reflections with I > 2(I)
R_int = 0.029

Refinement

R[F² > 2(F²)] = 0.034
wR(F²) = 0.080
S = 1.08
5939 reflections
306 parameters
1 restraint
H-atom parameters constrained
_max = 0.75 e Å^-3
_min = -0.40 e Å^-3
Absolute structure: Flack (1983), 2726 Friedel pairs
Flack parameter: 0.017 (11)

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N1-H1O10ⁱ	0.93	1.97	2.832 (4)	153
N1-H1O9ⁱ	0.93	2.45	3.056 (3)	123
O11-H11O9ⁱ	0.84	2.04	2.840 (3)	159
Symmetry code: (i) $[x-{\script{1\over 2}}, -y+{\script{3\over 2}}, z]$ .

Data collection: SMART (Bruker, 2001); cell refinement: SAINT-Plus (Bruker, 2003); data reduction: SAINT-Plus; 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: ZL2161 ).

Acknowledgements

MS is grateful to the Higher Education Commission of Pakistan and the Pakistan Science Foundation for financial support via their PhD program.

References

Brown, G. M. & Chidambaram, R. (1973). Acta Cryst. B29, 2393-2403.
Bruker (2001). SMART and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2003). SAINT-Plus. Bruker AXS Inc., Madison, Wisconsin, USA.
Flack, H. D. (1983). Acta Cryst. A39, 876-881.
Hamid, M., Tahir, A. A., Mazhar, M., Zeller, M. & Hunter, A. D. (2007). Inorg. Chem. 46, 4120-4127.
Shahid, M., Mazhar, M., Helliwell, M., Akhtar, J. & Ahmad, K. (2008). Acta Cryst. E64, m1139-m1140.
Shahid, M., Mazhar, M., Malik, M. A., O'Brien, P. & Raftery, J. (2008). Polyhedron, 27, 3337-3342.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Van Niekerk, J. N. & Schoening, F. R. L. (1953). Nature (London), 171, 36-37.
Zhang, Y.-L., Chen, S.-W., Liu, W.-S. & Wang, D.-Q. (2004). Acta Cryst. E60, m196-m197.