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

Li, S.; Zhang, F.-L.; Wang, S.-B.; Bai, H.-L.

doi:10.1107/S1600536809008824

metal-organic compounds

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ISSN: 2056-9890

Volume 65| Part 4| April 2009| Page m410

doi:10.1107/S1600536809008824

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

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

^aInstitute of Immunology, Key Laboratory of Natural Drugs and Immunological Engineering of Henan Province, College of Medicine, Henan University, Kaifeng 475003, People's Republic of China, ^bFirst Affiliated Hospital, Henan University, Kaifeng 475003, People's Republic of China, and ^cCollege of Chemistry and Chemical Engineering, Henan University, Kaifeng 475003, People's Republic of China
^*Correspondence e-mail: baihl_hd@126.com

(Received 5 February 2009; accepted 10 March 2009; online 19 March 2009)

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, $[I \overline 4]$
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[F² > 2σ(F²)] = 0.053
wR(F²) = 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)

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
Symmetry codes: (i) $[y+{\script{1\over 2}}, -x+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (ii) $[-x+{\script{1\over 2}}, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]$ ; (iii) -y+1, x, -z; (iv) $[-x+{\script{1\over 2}}, -y+{\script{1\over 2}}, z-{\script{1\over 2}}]$ ; (v) -x, -y, z; (vi) y, -x, -z.

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.

Supporting information

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

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

checkCIF report

Comment top

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).

Related literature top

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

Experimental top

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%.

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT-Plus (Bruker, 2001); data reduction: SAINT-Plus (Bruker, 2001); 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 (Sheldrick, 2008).

Figures top

	Fig. 1. Asymmetric unit of the title compound, showing 50% probability displacement ellipsoids for non-H atoms.
	Fig. 2. One-dimensional coordination polymer running along [001].
	Fig. 3. Projection along [001], showing the tetragonal arrangement of coordination polymers. O—H···O hydrogen bonds are shown as dashed lines.

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

Crystal data top

[Tb(C₇H₃NO₄)(C₇H₄NO₄)(H₂O)₂]·2H₂O	D_x = 2.202 Mg m⁻³
M_r = 562.20	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, I4	Cell parameters from 3001 reflections
Hall symbol: I -4	θ = 1.9–25.3°
a = 15.107 (2) Å	µ = 4.25 mm⁻¹
c = 14.8587 (15) Å	T = 298 K
V = 3391.1 (7) Å³	Block, colourless
Z = 8	0.12 × 0.11 × 0.08 mm
F(000) = 2192

Data collection top

Bruker APEXII CCD diffractometer	3001 independent reflections
Radiation source: fine-focus sealed tube	2886 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.072
ϕ and ω scans	θ_max = 25.3°, θ_min = 1.9°
Absorption correction: multi-scan (SADABS; Bruker, 2001)	h = −12→18
T_min = 0.617, T_max = 0.713	k = −18→17
6901 measured reflections	l = −13→17

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.053	H-atom parameters constrained
wR(F²) = 0.131	w = 1/[σ²(F_o²) + (0.1007P)² + 0.8682P] where P = (F_o² + 2F_c²)/3
S = 1.03	(Δ/σ)_max < 0.001
3001 reflections	Δρ_max = 3.51 e Å⁻³
263 parameters	Δρ_min = −1.17 e Å⁻³
0 restraints	Absolute structure: Flack (1983), 1387 Freidel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.54 (2)

Crystal data top

[Tb(C₇H₃NO₄)(C₇H₄NO₄)(H₂O)₂]·2H₂O	Z = 8
M_r = 562.20	Mo Kα radiation
Tetragonal, I4	µ = 4.25 mm⁻¹
a = 15.107 (2) Å	T = 298 K
c = 14.8587 (15) Å	0.12 × 0.11 × 0.08 mm
V = 3391.1 (7) Å³

Data collection top

Bruker APEXII CCD diffractometer	3001 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2001)	2886 reflections with I > 2σ(I)
T_min = 0.617, T_max = 0.713	R_int = 0.072
6901 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.053	H-atom parameters constrained
wR(F²) = 0.131	Δρ_max = 3.51 e Å⁻³
S = 1.03	Δρ_min = −1.17 e Å⁻³
3001 reflections	Absolute structure: Flack (1983), 1387 Freidel pairs
263 parameters	Absolute structure parameter: 0.54 (2)
0 restraints

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Tb1	0.30210 (3)	0.22535 (3)	0.22736 (3)	0.01388 (17)
C1	0.1833 (6)	0.4100 (6)	0.1946 (6)	0.0116 (19)
C2	0.1334 (7)	0.4753 (6)	0.1553 (6)	0.0148 (19)
H2A	0.1128	0.5222	0.1900	0.018*
C3	0.1132 (7)	0.4720 (7)	0.0639 (7)	0.019 (2)
H3A	0.0796	0.5166	0.0376	0.023*
C4	0.1433 (6)	0.4021 (6)	0.0129 (7)	0.015 (2)
C5	0.1879 (7)	0.3364 (7)	0.0575 (8)	0.021 (2)
H5A	0.2046	0.2864	0.0251	0.025*
C6	0.2161 (6)	0.4123 (6)	0.2921 (6)	0.015 (2)
C7	0.1302 (7)	0.3959 (7)	−0.0870 (7)	0.017 (2)
C8	0.1196 (7)	0.1238 (6)	0.1716 (7)	0.014 (2)
C9	0.0975 (6)	0.1488 (6)	0.2710 (7)	0.0129 (18)
C10	0.0233 (6)	0.1192 (7)	0.3157 (7)	0.017 (2)
H10A	−0.0195	0.0865	0.2854	0.021*
C11	0.0131 (7)	0.1383 (7)	0.4052 (7)	0.018 (2)
H11A	−0.0351	0.1158	0.4366	0.022*
C12	0.0768 (6)	0.1929 (6)	0.4506 (6)	0.0115 (18)
C13	0.1449 (7)	0.2207 (7)	0.3980 (7)	0.019 (2)
H13A	0.1865	0.2577	0.4249	0.023*
C14	0.0684 (7)	0.2114 (7)	0.5505 (7)	0.018 (2)
N1	0.1583 (5)	0.2001 (5)	0.3112 (6)	0.0142 (16)
N2	0.2094 (5)	0.3400 (5)	0.1465 (6)	0.0142 (17)
O1	0.2739 (5)	0.3551 (4)	0.3099 (5)	0.0178 (15)
H1	0.3058	0.3643	0.3561	0.027*
O2	0.1862 (6)	0.4677 (6)	0.3436 (5)	0.035 (2)
O3	0.1625 (5)	0.3283 (5)	−0.1271 (5)	0.0212 (16)
O4	0.0921 (6)	0.4561 (5)	−0.1264 (5)	0.0262 (18)
O5	0.1946 (5)	0.1457 (5)	0.1459 (5)	0.0208 (16)
O6	0.0625 (5)	0.0865 (5)	0.1277 (5)	0.0240 (17)
O7	0.0056 (6)	0.1862 (6)	0.5922 (6)	0.033 (2)
O8	0.1326 (5)	0.2550 (5)	0.5846 (5)	0.0214 (16)
O9	0.3704 (5)	0.0819 (5)	0.1997 (5)	0.0240 (17)
H91	0.3822	0.0700	0.2543	0.036*
H92	0.4222	0.0849	0.1778	0.036*
O10	0.4504 (5)	0.2736 (5)	0.2620 (5)	0.0236 (16)
H101	0.4641	0.2868	0.2082	0.035*
H102	0.4875	0.2327	0.2729	0.035*
O11	0.2668 (7)	0.0205 (6)	0.0225 (6)	0.045 (2)
H111	0.2452	0.0578	0.0593	0.068*
H112	0.2812	0.0241	−0.0327	0.068*
O12	0.1257 (7)	−0.0901 (6)	0.0634 (7)	0.046 (2)
H121	0.0724	−0.0890	0.0818	0.068*
H122	0.1145	−0.0821	0.0079	0.068*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Tb1	0.0145 (3)	0.0144 (3)	0.0128 (2)	0.00004 (17)	−0.00014 (19)	0.00015 (19)
C1	0.013 (5)	0.011 (4)	0.011 (4)	−0.002 (4)	0.001 (4)	0.006 (4)
C2	0.022 (5)	0.008 (4)	0.014 (4)	0.002 (4)	0.007 (4)	−0.001 (4)
C3	0.015 (5)	0.020 (5)	0.023 (5)	0.007 (4)	−0.002 (4)	−0.001 (4)
C4	0.017 (5)	0.013 (5)	0.016 (5)	−0.003 (4)	−0.011 (4)	0.000 (4)
C5	0.021 (5)	0.016 (5)	0.026 (5)	0.005 (4)	−0.007 (4)	−0.009 (4)
C6	0.016 (5)	0.012 (4)	0.017 (6)	−0.001 (4)	0.002 (4)	−0.008 (4)
C7	0.012 (5)	0.020 (5)	0.019 (5)	0.000 (4)	0.004 (4)	−0.007 (4)
C8	0.023 (5)	0.006 (4)	0.012 (4)	0.004 (4)	−0.003 (4)	−0.006 (4)
C9	0.018 (4)	0.013 (4)	0.008 (4)	−0.002 (4)	−0.002 (4)	0.006 (4)
C10	0.014 (5)	0.018 (5)	0.020 (5)	−0.001 (4)	−0.003 (4)	−0.004 (4)
C11	0.015 (5)	0.023 (5)	0.018 (5)	0.000 (4)	−0.007 (4)	0.007 (4)
C12	0.008 (4)	0.015 (4)	0.012 (4)	0.004 (4)	0.008 (4)	0.000 (4)
C13	0.018 (5)	0.022 (5)	0.017 (5)	0.001 (4)	−0.002 (4)	−0.006 (4)
C14	0.014 (5)	0.025 (6)	0.014 (5)	0.001 (5)	−0.003 (4)	−0.004 (4)
N1	0.013 (4)	0.012 (4)	0.018 (4)	−0.001 (3)	−0.001 (4)	−0.002 (4)
N2	0.013 (4)	0.015 (4)	0.015 (4)	0.003 (3)	−0.002 (3)	−0.002 (3)
O1	0.021 (3)	0.016 (3)	0.016 (3)	−0.001 (3)	−0.007 (3)	−0.003 (3)
O2	0.050 (5)	0.035 (5)	0.019 (4)	0.019 (4)	−0.006 (4)	−0.002 (4)
O3	0.020 (4)	0.026 (4)	0.017 (4)	0.007 (3)	−0.002 (3)	−0.004 (3)
O4	0.032 (4)	0.024 (4)	0.022 (4)	0.017 (3)	−0.006 (3)	−0.002 (3)
O5	0.017 (4)	0.021 (4)	0.024 (4)	−0.003 (3)	0.003 (3)	−0.004 (3)
O6	0.019 (4)	0.029 (4)	0.024 (4)	−0.005 (3)	0.001 (3)	−0.006 (3)
O7	0.030 (4)	0.045 (5)	0.024 (4)	−0.016 (4)	0.011 (4)	−0.004 (4)
O8	0.019 (4)	0.032 (4)	0.013 (3)	−0.010 (3)	0.002 (3)	−0.007 (3)
O9	0.025 (4)	0.031 (4)	0.016 (3)	0.000 (3)	0.008 (3)	0.007 (3)
O10	0.021 (4)	0.035 (4)	0.014 (4)	−0.001 (3)	0.005 (3)	0.006 (3)
O11	0.064 (6)	0.039 (5)	0.033 (5)	0.012 (5)	0.014 (5)	−0.010 (4)
O12	0.053 (6)	0.045 (6)	0.039 (5)	0.018 (5)	−0.004 (5)	0.011 (5)

Geometric parameters (Å, º) top

Tb1—O1	2.351 (7)	C8—C9	1.560 (14)
Tb1—O5	2.356 (7)	C9—N1	1.341 (12)
Tb1—O8ⁱ	2.358 (7)	C9—C10	1.379 (14)
Tb1—O3ⁱⁱ	2.371 (7)	C10—C11	1.368 (16)
Tb1—O10	2.412 (7)	C10—H10A	0.930
Tb1—O9	2.435 (8)	C11—C12	1.435 (14)
Tb1—N2	2.531 (8)	C11—H11A	0.930
Tb1—N1	2.534 (8)	C12—C13	1.359 (14)
C1—N2	1.335 (13)	C12—C14	1.516 (13)
C1—C2	1.373 (13)	C13—N1	1.343 (15)
C1—C6	1.531 (13)	C13—H13A	0.930
C2—C3	1.393 (15)	C14—O7	1.195 (14)
C2—H2A	0.930	C14—O8	1.277 (12)
C3—C4	1.378 (15)	O1—H1	0.850
C3—H3A	0.930	O3—Tb1ⁱ	2.371 (7)
C4—C5	1.370 (15)	O8—Tb1ⁱⁱ	2.358 (7)
C4—C7	1.500 (15)	O9—H91	0.850
C5—N2	1.363 (15)	O9—H92	0.850
C5—H5A	0.930	O10—H101	0.850
C6—O2	1.221 (13)	O10—H102	0.850
C6—O1	1.256 (12)	O11—H111	0.850
C7—O4	1.226 (13)	O11—H112	0.850
C7—O3	1.279 (13)	O12—H121	0.850
C8—O6	1.219 (12)	O12—H122	0.850
C8—O5	1.242 (13)

O1—Tb1—O5	124.7 (3)	O1—C6—C1	114.1 (8)
O1—Tb1—O8ⁱ	116.1 (3)	O4—C7—O3	123.3 (10)
O5—Tb1—O8ⁱ	83.7 (2)	O4—C7—C4	119.3 (9)
O1—Tb1—O3ⁱⁱ	81.4 (3)	O3—C7—C4	117.4 (9)
O5—Tb1—O3ⁱⁱ	116.7 (3)	O6—C8—O5	127.2 (10)
O8ⁱ—Tb1—O3ⁱⁱ	140.3 (2)	O6—C8—C9	117.9 (9)
O1—Tb1—O10	78.8 (2)	O5—C8—C9	114.9 (8)
O5—Tb1—O10	154.8 (3)	N1—C9—C10	121.9 (10)
O8ⁱ—Tb1—O10	76.4 (2)	N1—C9—C8	114.6 (9)
O3ⁱⁱ—Tb1—O10	72.5 (2)	C10—C9—C8	123.5 (9)
O1—Tb1—O9	155.1 (2)	C11—C10—C9	119.4 (10)
O5—Tb1—O9	75.6 (3)	C11—C10—H10A	120.3
O8ⁱ—Tb1—O9	77.5 (3)	C9—C10—H10A	120.3
O3ⁱⁱ—Tb1—O9	75.8 (2)	C10—C11—C12	120.2 (10)
O10—Tb1—O9	84.9 (3)	C10—C11—H11A	119.9
O1—Tb1—N2	64.9 (3)	C12—C11—H11A	119.9
O5—Tb1—N2	74.0 (3)	C13—C12—C11	114.5 (9)
O8ⁱ—Tb1—N2	73.6 (3)	C13—C12—C14	124.7 (10)
O3ⁱⁱ—Tb1—N2	142.3 (3)	C11—C12—C14	120.7 (9)
O10—Tb1—N2	114.1 (3)	N1—C13—C12	126.4 (10)
O9—Tb1—N2	139.8 (3)	N1—C13—H13A	116.8
O1—Tb1—N1	73.4 (3)	C12—C13—H13A	116.8
O5—Tb1—N1	65.5 (3)	O7—C14—O8	124.1 (10)
O8ⁱ—Tb1—N1	145.1 (3)	O7—C14—C12	121.0 (10)
O3ⁱⁱ—Tb1—N1	72.1 (3)	O8—C14—C12	114.8 (9)
O10—Tb1—N1	137.5 (3)	C9—N1—C13	117.4 (9)
O9—Tb1—N1	108.2 (3)	C9—N1—Tb1	117.1 (7)
N2—Tb1—N1	82.1 (3)	C13—N1—Tb1	124.5 (7)
N2—C1—C2	120.3 (9)	C1—N2—C5	118.7 (9)
N2—C1—C6	115.4 (8)	C1—N2—Tb1	116.8 (6)
C2—C1—C6	124.3 (9)	C5—N2—Tb1	124.4 (7)
C1—C2—C3	120.6 (9)	C6—O1—Tb1	126.1 (6)
C1—C2—H2A	119.7	C6—O1—H1	116.9
C3—C2—H2A	119.7	Tb1—O1—H1	117.0
C4—C3—C2	119.5 (9)	C7—O3—Tb1ⁱ	141.6 (7)
C4—C3—H3A	120.2	C8—O5—Tb1	127.4 (6)
C2—C3—H3A	120.2	C14—O8—Tb1ⁱⁱ	137.7 (6)
C5—C4—C3	116.8 (9)	Tb1—O9—H91	96.6
C5—C4—C7	119.9 (9)	Tb1—O9—H92	114.0
C3—C4—C7	123.3 (9)	H91—O9—H92	100.6
N2—C5—C4	123.9 (9)	Tb1—O10—H101	95.5
N2—C5—H5A	118.0	Tb1—O10—H102	115.7
C4—C5—H5A	118.0	H101—O10—H102	100.9
O2—C6—O1	126.6 (9)	H111—O11—H112	132.5
O2—C6—C1	119.3 (9)	H121—O12—H122	96.9

N2—C1—C2—C3	−3.4 (15)	O3ⁱⁱ—Tb1—N1—C13	41.3 (8)
C6—C1—C2—C3	174.1 (9)	O10—Tb1—N1—C13	6.3 (10)
C1—C2—C3—C4	0.4 (15)	O9—Tb1—N1—C13	109.1 (8)
C2—C3—C4—C5	3.7 (15)	N2—Tb1—N1—C13	−111.0 (8)
C2—C3—C4—C7	−175.7 (10)	C2—C1—N2—C5	2.2 (14)
C3—C4—C5—N2	−5.2 (16)	C6—C1—N2—C5	−175.6 (9)
C7—C4—C5—N2	174.2 (10)	C2—C1—N2—Tb1	179.6 (7)
N2—C1—C6—O2	−170.7 (9)	C6—C1—N2—Tb1	1.9 (10)
C2—C1—C6—O2	11.7 (15)	C4—C5—N2—C1	2.3 (16)
N2—C1—C6—O1	10.2 (12)	C4—C5—N2—Tb1	−174.9 (8)
C2—C1—C6—O1	−167.4 (9)	O1—Tb1—N2—C1	−7.5 (6)
C5—C4—C7—O4	−178.2 (10)	O5—Tb1—N2—C1	134.4 (7)
C3—C4—C7—O4	1.1 (16)	O8ⁱ—Tb1—N2—C1	−137.6 (7)
C5—C4—C7—O3	−0.4 (15)	O3ⁱⁱ—Tb1—N2—C1	21.2 (9)
C3—C4—C7—O3	178.9 (9)	O10—Tb1—N2—C1	−71.1 (7)
O6—C8—C9—N1	−171.3 (9)	O9—Tb1—N2—C1	176.6 (6)
O5—C8—C9—N1	7.9 (12)	N1—Tb1—N2—C1	67.8 (7)
O6—C8—C9—C10	10.5 (13)	O1—Tb1—N2—C5	169.7 (9)
O5—C8—C9—C10	−170.3 (9)	O5—Tb1—N2—C5	−48.3 (8)
N1—C9—C10—C11	−3.6 (15)	O8ⁱ—Tb1—N2—C5	39.7 (8)
C8—C9—C10—C11	174.4 (9)	O3ⁱⁱ—Tb1—N2—C5	−161.5 (7)
C9—C10—C11—C12	3.5 (15)	O10—Tb1—N2—C5	106.2 (8)
C10—C11—C12—C13	−0.9 (14)	O9—Tb1—N2—C5	−6.1 (10)
C10—C11—C12—C14	−177.4 (9)	N1—Tb1—N2—C5	−115.0 (8)
C11—C12—C13—N1	−1.9 (15)	O2—C6—O1—Tb1	161.3 (8)
C14—C12—C13—N1	174.5 (10)	C1—C6—O1—Tb1	−19.6 (12)
C13—C12—C14—O7	178.6 (11)	O5—Tb1—O1—C6	−30.8 (9)
C11—C12—C14—O7	−5.3 (15)	O8ⁱ—Tb1—O1—C6	70.2 (8)
C13—C12—C14—O8	−1.4 (14)	O3ⁱⁱ—Tb1—O1—C6	−147.4 (8)
C11—C12—C14—O8	174.7 (9)	O10—Tb1—O1—C6	138.9 (8)
C10—C9—N1—C13	1.0 (14)	O9—Tb1—O1—C6	−171.0 (7)
C8—C9—N1—C13	−177.2 (8)	N2—Tb1—O1—C6	15.4 (8)
C10—C9—N1—Tb1	169.6 (7)	N1—Tb1—O1—C6	−73.5 (8)
C8—C9—N1—Tb1	−8.6 (10)	O4—C7—O3—Tb1ⁱ	12.3 (17)
C12—C13—N1—C9	1.8 (16)	C4—C7—O3—Tb1ⁱ	−165.4 (7)
C12—C13—N1—Tb1	−165.8 (8)	O6—C8—O5—Tb1	176.0 (8)
O1—Tb1—N1—C9	147.5 (7)	C9—C8—O5—Tb1	−3.1 (12)
O5—Tb1—N1—C9	5.4 (6)	O1—Tb1—O5—C8	−46.5 (9)
O8ⁱ—Tb1—N1—C9	35.5 (9)	O8ⁱ—Tb1—O5—C8	−164.1 (8)
O3ⁱⁱ—Tb1—N1—C9	−126.4 (7)	O3ⁱⁱ—Tb1—O5—C8	51.8 (8)
O10—Tb1—N1—C9	−161.3 (6)	O10—Tb1—O5—C8	157.8 (7)
O9—Tb1—N1—C9	−58.6 (7)	O9—Tb1—O5—C8	117.3 (8)
N2—Tb1—N1—C9	81.4 (7)	N2—Tb1—O5—C8	−89.3 (8)
O1—Tb1—N1—C13	−44.8 (8)	N1—Tb1—O5—C8	−0.9 (8)
O5—Tb1—N1—C13	173.0 (9)	O7—C14—O8—Tb1ⁱⁱ	23.9 (17)
O8ⁱ—Tb1—N1—C13	−156.8 (7)	C12—C14—O8—Tb1ⁱⁱ	−156.1 (7)

Symmetry codes: (i) −x+1/2, −y+1/2, z−1/2; (ii) −x+1/2, −y+1/2, z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1···O12ⁱⁱⁱ	0.85	1.98	2.801 (12)	162
O9—H91···O4ⁱⁱ	0.85	1.86	2.706 (10)	180
O9—H92···O4^iv	0.85	1.99	2.842 (11)	180
O10—H101···O7ⁱ	0.85	1.83	2.679 (11)	179
O10—H102···O9ⁱⁱⁱ	0.85	2.15	3.000 (11)	180
O11—H111···O5	0.85	2.00	2.851 (12)	180
O11—H112···O2ⁱ	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

Symmetry codes: (i) −x+1/2, −y+1/2, z−1/2; (ii) −x+1/2, −y+1/2, z+1/2; (iii) y+1/2, −x+1/2, −z+1/2; (iv) −y+1, x, −z; (v) −x, −y, z; (vi) y, −x, −z.

Experimental details

Crystal data
Chemical formula	[Tb(C₇H₃NO₄)(C₇H₄NO₄)(H₂O)₂]·2H₂O
M_r	562.20
Crystal system, space group	Tetragonal, I4
Temperature (K)	298
a, c (Å)	15.107 (2), 14.8587 (15)
V (Å³)	3391.1 (7)
Z	8
Radiation type	Mo Kα
µ (mm⁻¹)	4.25
Crystal size (mm)	0.12 × 0.11 × 0.08

Data collection
Diffractometer	Bruker APEXII CCD diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2001)
T_min, T_max	0.617, 0.713
No. of measured, independent and observed [I > 2σ(I)] reflections	6901, 3001, 2886
R_int	0.072
(sin θ/λ)_max (Å⁻¹)	0.601

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.053, 0.131, 1.03
No. of reflections	3001
No. of parameters	263
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	3.51, −1.17
Absolute structure	Flack (1983), 1387 Freidel pairs
Absolute structure parameter	0.54 (2)

Computer programs: APEX2 (Bruker, 2004), SAINT-Plus (Bruker, 2001), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1···O12ⁱ	0.85	1.98	2.801 (12)	161.9
O9—H91···O4ⁱⁱ	0.85	1.86	2.706 (10)	179.8
O9—H92···O4ⁱⁱⁱ	0.85	1.99	2.842 (11)	179.9
O10—H101···O7^iv	0.85	1.83	2.679 (11)	179.2
O10—H102···O9ⁱ	0.85	2.15	3.000 (11)	179.8
O11—H111···O5	0.85	2.00	2.851 (12)	179.9
O11—H112···O2^iv	0.85	1.91	2.758 (12)	179.8
O12—H121···O6^v	0.85	2.15	3.000 (12)	179.8
O12—H122···O6^vi	0.85	2.08	2.930 (13)	179.6

Symmetry codes: (i) y+1/2, −x+1/2, −z+1/2; (ii) −x+1/2, −y+1/2, z+1/2; (iii) −y+1, x, −z; (iv) −x+1/2, −y+1/2, z−1/2; (v) −x, −y, z; (vi) y, −x, −z.

Acknowledgements

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

References

Bruker (2001). SADABS and SAINT-Plus. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Bruker (2004). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Flack, H. D. (1983). Acta Cryst. A39, 876–881. CrossRef CAS Web of Science IUCr Journals Google Scholar
Huang, Y. G., Wu, B. L., Yuan, D. Q., Xu, Y. Q., Jiang, F. L. & Hong, M. C. (2007). Inorg. Chem. 46, 1171–1176. Web of Science CSD CrossRef PubMed CAS Google Scholar
Li, S., Chen, Y., He, H.-M. & Ma, Y.-F. (2009). Acta Cryst. E65, m411. CrossRef IUCr Journals Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar

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Volume 65| Part 4| April 2009| Page m410

doi:10.1107/S1600536809008824

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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

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

Related literature

Experimental

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

metal-organic compounds

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