catena-Poly[[[diaqua­terbium(III)]-μ-6-carboxy­nicotinato-μ-pyridine-2,5-di­carboxyl­ato] dihydrate]

Sheng Li; Fu-Li Zhang; Shou-Bin Wang; Hui-Ling Bai

doi:10.1107/S1600536809008824

. 2009 Mar 19;65(Pt 4):m410. doi: 10.1107/S1600536809008824

catena-Poly[[[diaquaterbium(III)]-μ-6-carboxynicotinato-μ-pyridine-2,5-dicarboxylato] dihydrate]

Sheng Li ^a,^*, Fu-Li Zhang ^b, Shou-Bin Wang ^c, Hui-Ling Bai ^a

PMCID: PMC2968984 PMID: 21582353

Abstract

The title compound, {[Tb(C₇H₃NO₄)(C₇H₄NO₄)(H₂O)₂]·2H₂O}_n, is isotypic with the analogous Tm^III compound [Li, Zhang, Wang & Bai (2009). Acta Cryst. E65, m411]. The Tb^III atom is octacoordinated by two water molecules and by four carboxylate O atoms and two pyridyl N atoms from two pyridine-2,5-dicarboxylate (2,5-pydc) and two 6-carboxynicotinate (2,5-Hpydc) ligands. The 2,5-pydc and 2,5-Hpydc ligands bridge Tb^III atoms, generating helical coordination polymers along [001]. An extensive network of O—H⋯O hydrogen bonds is formed between the coordination polymers and the uncoordinated water molecules. The refined Flack parameter of 0.54 (2) suggests inversion twinning.

Related literature

For the isotypic Tm^III compound, see Li et al. (2009 ▶). For other related structures, see: Huang et al. (2007 ▶).

Experimental

Crystal data

[Tb(C₇H₃NO₄)(C₇H₄NO₄)(H₂O)₂]·2H₂O
M _r = 562.20
Tetragonal,
a = 15.107 (2) Å
c = 14.8587 (15) Å
V = 3391.1 (7) Å³
Z = 8
Mo Kα radiation
μ = 4.25 mm⁻¹
T = 298 K
0.12 × 0.11 × 0.08 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T _min = 0.617, T _max = 0.713
6901 measured reflections
3001 independent reflections
2886 reflections with I > 2σ(I)
R _int = 0.072

Refinement

R[F ² > 2σ(F ²)] = 0.053
wR(F ²) = 0.131
S = 1.03
3001 reflections
263 parameters
H-atom parameters constrained
Δρ_max = 3.51 e Å⁻³
Δρ_min = −1.17 e Å⁻³
Absolute structure: Flack (1983 ▶), with 1387 Friedel pairs
Flack parameter: 0.54 (2)

Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: SAINT-Plus (Bruker, 2001 ▶); 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 Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809008824/bi2349sup1.cif

e-65-0m410-sup1.cif^{(22.8KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809008824/bi2349Isup2.hkl

e-65-0m410-Isup2.hkl^{(147.4KB, hkl)}

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Table 1. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1⋯O12ⁱ	0.85	1.98	2.801 (12)	162
O9—H91⋯O4ⁱⁱ	0.85	1.86	2.706 (10)	180
O9—H92⋯O4ⁱⁱⁱ	0.85	1.99	2.842 (11)	180
O10—H101⋯O7^iv	0.85	1.83	2.679 (11)	179
O10—H102⋯O9ⁱ	0.85	2.15	3.000 (11)	180
O11—H111⋯O5	0.85	2.00	2.851 (12)	180
O11—H112⋯O2^iv	0.85	1.91	2.758 (12)	180
O12—H121⋯O6^v	0.85	2.15	3.000 (12)	180
O12—H122⋯O6^vi	0.85	2.08	2.930 (13)	180

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Symmetry codes: (i) Inline graphic ; (ii) ; (iii) ; (iv) ; (v) ; (vi) .

Acknowledgments

The authors are grateful for financial support from the Scientific Research Foundation of Outstanding Talented Persons of Henan Province (grant No. 74200510014).

supplementary crystallographic information

Comment

The asymmetric unit of the title compound is shown in Fig. 1. Atom Tb1 displays octa-coordination through two water molecules, four carboxylate O atoms and two pyridyl N atoms from two 2,5-pydc and two 2,5-Hpydc ligands (2,5-pydc = pyridine-2,5-dicarboxylate). The 2,5-pydc and 2,5-Hpydc ligands bridge between Tb^III atoms to generate helical coordination polymers along [001] (Fig. 2). An extensive network of O—H···O hydrogen bonds is formed between the coordination polymers and the lattice water molecules (Table 1 and Fig. 3).

Experimental

A mixture of terbium oxide (0.5 mmol), pyridine-2,5-dicarboxylic acid (0.5 mmol), in H₂O (8 ml) and ethanol (8 ml) was sealed in a 25 ml Teflon-lined stainless steel autoclave and kept at 413 K for three days. Colourless crystals were obtained after cooling to room temperature with a yield of 27%. Elemental analysis calculated for C₁₄H₁₅N₂TbO₁₂: C 30.68, H 2.74, N 5.11%; Found: C 30.62, H 2.72, N 5.06%.