(IUCr) catena-Poly[[tetraaquanickel(II)]-[mu]3-benzene-1,3,5-tricarboxylato-3':1:2-[kappa]4O1:O3,O3':O5-[tetraaquanickel(II)]-[mu]2-benzene-1,3,5-tricarboxylato-2:3[kappa]2O1:O3-[tetraaquanickel(II)]]

Volume 65
Part 6
Pages m625-m626
June 2009

Received 14 March 2009
Accepted 4 May 2009
Online 14 May 2009

Key indicators
Single-crystal X-ray study
T = 295 K
Mean (C-C) = 0.004 Å
R = 0.028
wR = 0.068
Data-to-parameter ratio = 15.9
Details

catena-Poly[[tetraaquanickel(II)]-₃-benzene-1,3,5-tricarboxylato-3':1:2-⁴O¹:O³,O^3':O⁵-[tetraaquanickel(II)]-₂-benzene-1,3,5-tricarboxylato-2:3²O¹:O³-[tetraaquanickel(II)]]

Shih-Chen Hsu,^a Pei-Hsuan Chiang,^a Chih-Hsien Chang ^a and Chia-Her Lin ^a ^*

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

The microwave solvothermal reaction of nickel nitrate with trimesic acid provided the title compound, [Ni₃(BTC)₂(H₂O)₁₂]_n (BTC = benzene-1,3,5-tricarboxylate anion, C₉H₃O₆), which is a metal coordination polymer composed of one-dimensional zigzag chains. The crystal under investigation was ramecically twinned with an approximate twin domain ratio of 1:1. In the asymmetric unit, there are two types of Ni atoms. One of the NiO₆ groups (2 symmetry) is coordinated to only one carboxylate group and thus terminal, the other is bridging, forming the coordination polymer. The extended chains are connected by the organic BTC anions via ₂-linkages. O-HO hydrogen bonds and [pi] - [pi] interactions between the chains [centroid-centroid distance 3.58 (1) Å] induce the complex to mimic a three-dimensional structure.

Related literature

For background information on the solvothermal synthesis of coordination polymers with organic carboxylate ligands, see: Kitagawa et al. (2004).

Experimental

Crystal data

[Ni₃(C₉H₃O₆)₂(H₂O)₁₂]
M_r = 806.49
Monoclinic, C 2
a = 17.3394 (10) Å
b = 12.8724 (7) Å
c = 6.5462 (3) Å
= 111.609 (2)°
V = 1358.42 (12) Å³
Z = 2
Mo K radiation
= 2.17 mm^-1
T = 295 K
0.25 × 0.18 × 0.15 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2008) T_min = 0.613, T_max = 0.737
6798 measured reflections
3299 independent reflections
3156 reflections with I > 2(I)
R_int = 0.046

Refinement

R[F² > 2(F²)] = 0.028
wR(F²) = 0.068
S = 1.07
3299 reflections
208 parameters
1 restraint
H-atom parameters constrained
_max = 0.48 e Å^-3
_min = -0.38 e Å^-3
Absolute structure: Flack (1983), 1531 Friedel pairs
Flack parameter: 0.549 (12)

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O9-H9BO10ⁱ	0.87	1.90	2.767 (3)	172
O9-H9AO12ⁱⁱ	0.81	2.33	3.102 (3)	160
O6-H6BO1ⁱⁱⁱ	0.97	1.98	2.942 (3)	173
O6-H6AO11^iv	0.85	1.83	2.683 (3)	173
O5-H5BO12^iv	0.92	1.95	2.825 (3)	158
O5-H5AO11	0.81	1.79	2.559 (3)	156
O4-H4CO1ⁱ	0.92	1.97	2.870 (3)	167
O4-H4BO10	0.91	1.77	2.617 (3)	154
O3-H3BO12^v	0.94	1.97	2.907 (3)	171
O3-H3AO4^vi	0.94	2.03	2.917 (3)	156
O2-H2BO5^vii	0.83	1.81	2.638 (3)	173
O2-H2AO12^viii	0.85	2.02	2.861 (4)	171
Symmetry codes: (i) $[-x+{\script{3\over 2}}, y-{\script{1\over 2}}, -z+1]$ ; (ii) $[-x+{\script{3\over 2}}, y+{\script{1\over 2}}, -z+1]$ ; (iii) $[-x+{\script{3\over 2}}, y-{\script{1\over 2}}, -z]$ ; (iv) $[-x+{\script{3\over 2}}, y+{\script{1\over 2}}, -z]$ ; (v) $[x-{\script{1\over 2}}, y+{\script{3\over 2}}, z]$ ; (vi) $[x-{\script{1\over 2}}, y+{\script{1\over 2}}, z]$ ; (vii) x, y+1, z; (viii) $[-x+{\script{3\over 2}}, y+{\script{3\over 2}}, -z+1]$ .

Data collection: APEX2 (Bruker, 2008); cell refinement: SAINT (Bruker, 2008); data reduction: SAINT; 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: ZL2190 ).

Acknowledgements

This research project was supported by the National Science Council of Taiwan (NSC97-2113-M-033-003-MY2) and by the project of the specific research fields of Chung Yuan Christian University, Taiwan, under grant No. CYCU-97-CR-CH.

References

Bruker (2008). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Flack, H. D. (1983). Acta Cryst. A39, 876-881.
Kitagawa, S., Kitaura, R. & Noro, S. (2004). Angew. Chem. Int. Ed. 43, 2334-2375.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.

metal-organic compounds

catena-Poly[[tetraaquanickel(II)]-3-benzene-1,3,5-tricarboxylato-3':1:2-4O1:O3,O3':O5-[tetraaquanickel(II)]-2-benzene-1,3,5-tricarboxylato-2:32O1:O3-[tetraaquanickel(II)]]