catena-Poly[[[diaqua-terbium(III)]-μ-6-carboxy-nicotinato-μ-pyridine-2,5-di-carboxyl-ato] dihydrate].

The title compound, {[Tb(C(7)H(3)NO(4))(C(7)H(4)NO(4))(H(2)O)(2)]·2H(2)O}(n), is isotypic with the analogous Tm(III) compound [Li, Zhang, Wang & Bai (2009). Acta Cryst. E65, m411]. The Tb(III) atom is octa-coordinated by two water mol-ecules and by four carboxyl-ate O atoms and two pyridyl N atoms from two pyridine-2,5-dicarboxyl-ate (2,5-pydc) and two 6-carboxy-nicotinate (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 mol-ecules. The refined Flack parameter of 0.54 (2) suggests inversion twinning.

Related literature

For the isotypic TmIII 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 = 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

Δρmax = 3.51 e Å−3

Δρmin = −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.

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

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

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

[Tb(C7H3NO4)(C7H4NO4)(H2O)2]·2H2O	Dx = 2.202 Mg m−3
Mr = 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

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

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(Fo2) + (0.1007P)2 + 0.8682P] where P = (Fo2 + 2Fc2)/3
S = 1.03	(Δ/σ)max < 0.001
3001 reflections	Δρmax = 3.51 e Å−3
263 parameters	Δρmin = −1.17 e Å−3
0 restraints	Absolute structure: Flack (1983), 1387 Freidel pairs
Primary atom site location: structure-invariant direct methods	Flack parameter: 0.54 (2)

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.

	x	y	z	Uiso*/Ueq
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*

	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)

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)

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···O4iv	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···O6v	0.85	2.15	3.000 (12)	180
O12—H122···O6vi	0.85	2.08	2.930 (13)	180

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⋯O7iv	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⋯O2iv	0.85	1.91	2.758 (12)	180
O12—H121⋯O6v	0.85	2.15	3.000 (12)	180
O12—H122⋯O6vi	0.85	2.08	2.930 (13)	180

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