Bis(4,4′-methyl­enedicyclo­hexyl­aminium) μ-benzene-1,4-dicarboxyl­ato-bis­[tri­chlorido­zinc(II)] tetra­hydrate

Hsu, C.-Y.; Yeh, C.-W.; Wu, C.-P.; Lin, C.-H.; Chen, J.-D.

doi:10.1107/S1600536808033011

Volume 64
Part 11
Page m1412
November 2008

Received 15 September 2008
Accepted 12 October 2008
Online 15 October 2008

Key indicators
Single-crystal X-ray study
T = 295 K
Mean (C-C) = 0.009 Å
R = 0.057
wR = 0.132
Data-to-parameter ratio = 16.7
Details

Bis(4,4'-methylenedicyclohexylaminium) -benzene-1,4-dicarboxylato-bis[trichloridozinc(II)] tetrahydrate

Chen-Yen Hsu,^a Chun-Wei Yeh,^a Chi-Phi Wu,^a Chia-Her Lin ^a ^* and Jhy-Der Chen ^a

^aDepartment of Chemistry, Chung-Yuan Christian University, Chung-Li 320, Taiwan
Correspondence e-mail: chiaher@cycu.edu.tw

The title compound, (C₁₃H₂₈N₂)₂[Zn₂(C₈H₄O₄)Cl₆]·4H₂O, was prepared by the reaction of ZnCl₂·6H₂O, benzene-1,4-dicarboxylic acid and 4,4'-diaminodicyclohexylmethane in methanol. The [Zn₂Cl₆(C₈H₄O₄)]^4- anions lie on centres of inversion and comprise two ZnCl₃ groups bridged by benzene-1,4-dicarboxylate. In addition to N-HCl and N-HO hydrogen bonds between the cations and anions, solvent water molecules form O-HO and O-HCl hydrogen bonds to give a three-dimensional network.

Related literature

For related structures, see: Clausen et al. (2005); Thirumurugan & Rao (2005); Li et al. (1998, 1999).

Experimental

Crystal data

(C₁₃H₂₈N₂)₂[Zn₂(C₈H₄O₄)Cl₆]·4H₂O
M_r = 1004.36
Monoclinic, P 2₁ /c
a = 14.264 (3) Å
b = 14.202 (2) Å
c = 11.712 (2) Å
= 100.498 (16)°
V = 2333.0 (7) Å³
Z = 2
Mo K radiation
= 1.42 mm^-1
T = 295 (2) K
0.70 × 0.40 × 0.10 mm

Data collection

Bruker P4 diffractometer
Absorption correction: scan (XSCANS; Siemens, 1995) T_min = 0.694, T_max = 0.868
5093 measured reflections
4071 independent reflections
3405 reflections with I > 2(I)
R_int = 0.027
3 standard reflections every 97 reflections intensity decay: none

Refinement

R[F² > 2(F²)] = 0.057
wR(F²) = 0.132
S = 1.05
4071 reflections
244 parameters
2 restraints
H-atom parameters constrained
_max = 1.10 e Å^-3
_min = -0.83 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N1-H1ACl3	0.89	2.41	3.252 (4)	159
N1-H1BCl2ⁱ	0.89	2.51	3.290 (4)	147
N1-H1CO3ⁱ	0.89	1.94	2.828 (5)	178
N2-H2ACl1ⁱⁱ	0.89	2.95	3.725 (5)	146
N2-H2ACl2ⁱⁱ	0.89	2.67	3.321 (4)	131
N2-H2BO2ⁱⁱⁱ	0.89	2.06	2.928 (4)	166
N2-H2CO4^iv	0.89	1.95	2.813 (4)	164
O3-H3BO2	1.00	1.81	2.798 (4)	167.8
O3-H3CCl1^v	1.06	2.24	3.262 (4)	160.3
O4-H4BCl3	0.98	2.21	3.172 (4)	164.9
O4-H4CCl2^vi	0.94	2.38	3.258 (3)	154.9
Symmetry codes: (i) $[x, -y+{\script{3\over 2}}, z+{\script{1\over 2}}]$ ; (ii) x-1, y, z; (iii) -x, -y+1, -z; (iv) $[-x, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (v) -x+1, -y+1, -z; (vi) -x+1, -y+1, -z+1.

Data collection: XSCANS (Siemens, 1995); cell refinement: XSCANS; data reduction: SHELXTL (Sheldrick, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); 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: BI2304 ).

Acknowledgements

The authors are grateful to the National Science Council of Taiwan for support. This research was also supported by the Project of the Specific Research Fields in Chung Yuan Christian University, Taiwan, under grant No. CYCU-97-CR-CH.

References

Clausen, H. F., Poulsen, R. D., Bond, A. D., Chevallier, M.-A. S. & Iversen, B. B. (2005). J. Solid State Chem. 178, 3342-3351.
Li, H., Eddaoudi, M., Groy, T. L. & Yaghi, O. M. (1998). J. Am. Chem. Soc. 120, 8571-8572.
Li, H., Eddaoudi, M., O'Keeffe, M. & Yaghi, O. M. (1999). Nature (London), 402, 276-279.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Siemens (1995). XSCANS. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.
Thirumurugan, A. & Rao, C. N. R. (2005). J. Mater. Chem. 15, 3852-3858.

metal-organic compounds