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Acta Cryst. (2007). E63, m2182-m2183    [ doi:10.1107/S1600536807034629 ]

catena-Poly[[[diaqua(6-carboxypyridine-2-carboxylato)terbium(III)]-[mu]-pyridine-2,6-dicarboxylato] tetrahydrate]

L.-J. Hao and T.-L. Yu

Abstract top

The title compound, [Tb(C7H3NO4)(C7H4NO4)(H2O)2]·4H2O, is isostructural with its La3+, Ce3+, Pr3+, Nd3+, Sm3+ and Gd3+ analogues. The Tb3+ ion is nine-coordinated by two O and one N atoms from a tridentate 6-carboxypyridine-2-carboxylate ligand, two O and one N atoms from a tridentate pyridine-2,6-dicarboxylate ligand, one O atom belonging to a neighbouring pyridine-2,6-dicarboxylate ligand, and two water molecules. The bridging pyridine-2,6-dicarboxylate ligand gives rise to infinite chains. The crystal structure involves O-H...O hydrogen bonds.

Comment top

The title compound is isostructural those with its La3+ (Guerriero et al., 1987; Ghosh & Bharadwaj, 2005), Ce3+ (Okabe et al., 2002; Ghosh & Bharadwaj, 2003; Rafizadeh et al., 2005; Ramezanipour et al., 2005), Pr3+ (Ghosh & Bharadwaj, 2003; Zhao et al., 2005), Nd3+ (Miao et al., 1992), Sm3+ (Liu et al., 2005, 2006; Rafizadeh et al., 2005; Song et al., 2005), Eu3+ (Brayshaw et al., 2005) and Gd3+ (Hao & Yu, 2007) analogues.

The Tb3+ ion is nine-coordinated by four O and two N atoms from two independent tridentate pyridine-2,6-dicarboxyate ligands, one O atom belonging pyridine-2,6-dicarboxylate ligand and two water molecules (Fig. 1). The bridging pyridine-2,6-dicarboxylate ligand gives rise to infinite chains along the c-axis (Fig. 2). An extensive network of hydrogen bonds exists between water molecules.

Related literature top

The isostructural lanthanide compounds are those with La3+ (Guerriero et al., 1987; Ghosh & Bharadwaj, 2005), Ce3+ (Okabe et al., 2002; Ghosh & Bharadwaj, 2003; Rafizadeh et al., 2005; Ramezanipour et al., 2005), Pr3+ (Ghosh & Bharadwaj, 2003; Zhao et al., 2005), Nd3+ (Miao et al., 1992), Sm3+ (Liu et al., 2005, 2006; Rafizadeh et al., 2005; Song et al., 2005), Eu3+ (Brayshaw et al., 2005) and Gd3+ (Hao & Yu, 2007).

Experimental top

A mixture of Tb(NO3)3 (0.5 mmol), Sodium hydroxide(0.5 mmol), pyridine-2,6-dicarboxylic acid (0.5 mmol), H2O (8 ml) and ethanol (8 ml) in a 25 ml teflon-lined stainless steel autoclave was kept at 433 K for three days. Colorless crystals were obtained after cooling to room temperature with a yield of 36%. Anal. Calc. for C14H19N2O14Tb: C 28.09, H 3.18, N 4.68%; Found: C 28.01, H 3.23, N 4.61%.

Refinement top

The H atoms of the water molecules were located from difference density maps and were refined with distance restraints of d(H···H) = 1.38 (2) Å and d(O–H) = 0.82 (2) Å. All other H atoms were placed in calculated positions with a C–H bond distance of 0.93 Å and Uiso(H) = 1.2Ueq(C).

Computing details top

Data collection: APEX2 (Bruker, Year?); cell refinement: SAINT-Plus (Bruker, 2001); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2001); software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. The asymmetric unit of the title compound showing 30% probability displacement ellipsoids. H atoms shown as spheres of arbitrary radius. Atom O10i is generated by the symmetry code: (x, -y + 3/2, z + 1/2).
[Figure 2] Fig. 2. Part of an infinite chain running along the c-axis. H atoms omitted for clarity.
catena-Poly[[[diaqua(6-carboxypyridine-2-carboxylato)terbium(III)]-µ- pyridine-2,6-dicarboxylato] tetrahydrate] top
Crystal data top
[Tb(C7H3NO4)(C7H4NO4)(H2O)2]·4H2OF(000) = 1176
Mr = 598.24Dx = 1.977 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 3499 reflections
a = 13.9986 (3) Åθ = 1.5–25.0°
b = 11.3819 (2) ŵ = 3.60 mm−1
c = 12.8982 (2) ÅT = 293 K
β = 102.0126 (10)°Cube, colourless
V = 2010.08 (6) Å30.10 × 0.10 × 0.10 mm
Z = 4
Data collection top
Bruker APEXII CCD area-detector
diffractometer		3499 independent reflections
Radiation source: fine-focus sealed tube3237 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.022
φ and ω scansθmax = 25.2°, θmin = 1.5°
Absorption correction: multi-scan
(SADABS; Bruker, 2001)		h = −16→16
Tmin = 0.715, Tmax = 0.715k = −13→13
7168 measured reflectionsl = −7→15
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.042Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.131H atoms treated by a mixture of independent and constrained refinement
S = 1.00 w = 1/[σ2(Fo2) + (0.0953P)2 + 13.066P]
where P = (Fo2 + 2Fc2)/3
3499 reflections(Δ/σ)max < 0.001
317 parametersΔρmax = 1.20 e Å−3
189 restraintsΔρmin = −2.00 e Å−3
Crystal data top
[Tb(C7H3NO4)(C7H4NO4)(H2O)2]·4H2OV = 2010.08 (6) Å3
Mr = 598.24Z = 4
Monoclinic, P21/cMo Kα radiation
a = 13.9986 (3) ŵ = 3.60 mm−1
b = 11.3819 (2) ÅT = 293 K
c = 12.8982 (2) Å0.10 × 0.10 × 0.10 mm
β = 102.0126 (10)°
Data collection top
Bruker APEXII CCD area-detector
diffractometer		3499 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2001)		3237 reflections with I > 2σ(I)
Tmin = 0.715, Tmax = 0.715Rint = 0.022
7168 measured reflectionsθmax = 25.2°
Refinement top
R[F2 > 2σ(F2)] = 0.042 w = 1/[σ2(Fo2) + (0.0953P)2 + 13.066P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.131Δρmax = 1.20 e Å−3
S = 1.00Δρmin = −2.00 e Å−3
3499 reflectionsAbsolute structure: ?
317 parametersFlack parameter: ?
189 restraintsRogers parameter: ?
H atoms treated by a mixture of independent and constrained refinement
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s 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 > 2σ(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
xyzUiso*/Ueq
C10.5673 (6)0.5764 (8)0.8725 (7)0.0353 (9)
C20.5029 (6)0.6849 (8)0.8698 (7)0.0358 (8)
C30.4056 (6)0.6786 (8)0.8673 (7)0.0363 (8)
H30.37490.60620.86790.044*
C40.3521 (7)0.7840 (7)0.8636 (8)0.0369 (8)
H4A0.28520.78150.86100.044*
C50.3989 (6)0.8910 (8)0.8638 (7)0.0364 (8)
H50.36480.96140.86170.044*
C60.4975 (6)0.8894 (8)0.8671 (7)0.0360 (8)
C70.5573 (6)0.9998 (8)0.8682 (7)0.0358 (9)
C80.8806 (5)1.0253 (6)0.8263 (5)0.0179 (7)
C90.8732 (5)1.0388 (6)0.9408 (5)0.0176 (6)
C100.9082 (5)1.1397 (6)1.0001 (5)0.0180 (6)
H100.93441.20280.96960.022*
C110.9018 (5)1.1406 (6)1.1065 (5)0.0182 (6)
H110.92471.20501.14880.022*
C120.8619 (5)1.0469 (6)1.1489 (5)0.0178 (6)
H120.85851.04641.22010.021*
C130.8264 (5)0.9519 (6)1.0829 (5)0.0175 (6)
C140.7743 (5)0.8473 (6)1.1189 (5)0.0173 (7)
H1W0.909 (4)0.718 (4)0.987 (5)0.080*
H2W0.863 (3)0.612 (4)0.952 (8)0.080*
H3W0.595 (6)0.899 (7)0.672 (3)0.080*
H4W0.665 (8)0.841 (10)0.629 (6)0.080*
H5W0.924 (8)0.676 (10)0.190 (8)0.080*
H6W0.988 (9)0.753 (7)0.158 (9)0.080*
H7W0.788 (10)0.465 (5)0.888 (8)0.080*
H8W0.791 (12)0.397 (10)0.977 (5)0.080*
H9W0.023 (10)0.4869 (17)0.898 (8)0.080*
H10W0.038 (10)0.589 (8)0.847 (5)0.080*
H11W0.608 (9)0.300 (12)0.826 (4)0.080*
H12W0.674 (6)0.238 (11)0.899 (9)0.080*
N10.5474 (5)0.7881 (5)0.8674 (5)0.0201 (13)
N20.8315 (4)0.9488 (4)0.9813 (4)0.0111 (10)
O10.5308 (4)0.4780 (5)0.8764 (5)0.0400 (15)
O20.6558 (4)0.5971 (4)0.8704 (4)0.0227 (10)
O30.6432 (4)0.9921 (4)0.8649 (4)0.0257 (11)
O40.5122 (5)1.0991 (5)0.8733 (6)0.0464 (16)
H40.54711.15350.86190.070*
O50.8754 (4)0.6841 (5)0.9368 (4)0.0255 (11)
O60.6333 (4)0.8452 (6)0.6743 (4)0.0372 (15)
O70.8449 (4)0.9295 (4)0.7819 (3)0.0224 (10)
O80.9207 (4)1.1044 (5)0.7853 (4)0.0303 (12)
O90.7268 (4)0.7815 (4)1.0468 (4)0.0175 (10)
O100.7813 (4)0.8336 (4)1.2163 (3)0.0200 (10)
O110.9581 (4)0.6919 (5)0.1491 (4)0.0251 (12)
O120.7991 (8)0.4014 (7)0.9163 (9)0.086 (3)
O130.6236 (7)0.2750 (8)0.8855 (10)0.082 (3)
O140.0299 (5)0.5576 (5)0.9011 (4)0.0338 (13)
Tb10.73015 (2)0.79481 (3)0.85156 (2)0.01780 (18)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0230 (18)0.039 (2)0.044 (2)0.0056 (14)0.0088 (15)0.0012 (15)
C20.0236 (17)0.0396 (19)0.0450 (19)0.0060 (13)0.0087 (14)0.0012 (14)
C30.0239 (17)0.0399 (19)0.0458 (19)0.0059 (13)0.0087 (14)0.0013 (14)
C40.0242 (17)0.0403 (19)0.0469 (19)0.0061 (13)0.0086 (14)0.0012 (14)
C50.0241 (17)0.0399 (19)0.0456 (19)0.0064 (13)0.0086 (14)0.0011 (14)
C60.0239 (17)0.0396 (19)0.0451 (19)0.0063 (13)0.0087 (14)0.0010 (14)
C70.0241 (18)0.039 (2)0.045 (2)0.0065 (14)0.0085 (15)0.0007 (15)
C80.0207 (15)0.0176 (14)0.0149 (14)−0.0021 (12)0.0024 (12)−0.0008 (12)
C90.0205 (13)0.0172 (13)0.0146 (13)−0.0022 (11)0.0024 (10)−0.0009 (10)
C100.0209 (13)0.0175 (13)0.0149 (13)−0.0024 (11)0.0023 (10)−0.0009 (10)
C110.0212 (14)0.0176 (13)0.0150 (13)−0.0024 (11)0.0019 (10)−0.0011 (11)
C120.0208 (13)0.0174 (13)0.0146 (13)−0.0024 (11)0.0022 (10)−0.0009 (10)
C130.0204 (13)0.0172 (13)0.0145 (13)−0.0022 (11)0.0024 (10)−0.0008 (10)
C140.0201 (15)0.0170 (14)0.0142 (14)−0.0023 (12)0.0026 (12)−0.0006 (12)
N10.018 (3)0.026 (3)0.015 (3)−0.002 (2)0.001 (2)−0.001 (2)
N20.011 (2)0.013 (3)0.010 (2)−0.0026 (19)0.0016 (18)−0.0017 (19)
O10.030 (3)0.021 (3)0.065 (4)−0.013 (2)0.003 (3)0.002 (3)
O20.020 (2)0.017 (2)0.031 (3)−0.0016 (19)0.004 (2)−0.002 (2)
O30.027 (3)0.017 (2)0.032 (3)0.007 (2)0.002 (2)−0.003 (2)
O40.048 (4)0.029 (3)0.060 (4)0.015 (3)0.008 (3)−0.004 (3)
O50.026 (3)0.035 (3)0.013 (2)0.007 (2)−0.002 (2)−0.005 (2)
O60.041 (3)0.056 (4)0.012 (2)0.033 (3)0.000 (2)0.001 (2)
O70.035 (3)0.022 (2)0.012 (2)−0.011 (2)0.010 (2)−0.0040 (18)
O80.047 (3)0.025 (3)0.023 (3)−0.016 (2)0.017 (2)0.000 (2)
O90.021 (2)0.021 (2)0.009 (2)−0.0107 (18)0.0010 (18)−0.0008 (17)
O100.027 (3)0.021 (2)0.010 (2)−0.008 (2)0.0006 (19)0.0020 (19)
O110.026 (3)0.030 (3)0.018 (3)−0.003 (2)0.003 (2)0.000 (2)
O120.069 (6)0.039 (4)0.135 (9)0.014 (4)−0.014 (7)0.000 (5)
O130.068 (6)0.044 (5)0.128 (10)0.003 (4)0.008 (6)0.003 (5)
O140.048 (4)0.029 (3)0.030 (3)0.010 (3)0.022 (3)0.001 (2)
Tb10.0184 (3)0.0198 (3)0.0146 (2)−0.00110 (11)0.00191 (15)−0.00124 (11)
Geometric parameters (Å, º) top
C1—O11.237 (10)C13—C141.518 (9)
C1—O21.267 (10)C14—O101.249 (8)
C1—C21.525 (11)C14—O91.269 (8)
C2—N11.332 (11)N1—Tb12.610 (6)
C2—C31.358 (12)N2—Tb12.626 (5)
C3—C41.410 (12)O2—Tb12.512 (5)
C3—H30.9300O3—Tb12.578 (5)
C4—C51.382 (13)O4—H40.8200
C4—H4A0.9300O5—Tb12.449 (5)
C5—C61.373 (11)O5—H1W0.81 (6)
C5—H50.9300O5—H2W0.87 (5)
C6—N11.347 (10)O6—Tb12.470 (5)
C6—C71.509 (12)O6—H3W0.81 (8)
C7—O31.214 (10)O6—H4W0.81 (10)
C7—O41.303 (10)O7—Tb12.517 (5)
C8—O81.237 (8)O9—Tb12.533 (5)
C8—O71.284 (8)O10—Tb1i2.493 (4)
C8—C91.510 (9)O11—H5W0.80 (11)
C9—N21.337 (8)O11—H6W0.81 (10)
C9—C101.410 (9)O12—H7W0.81 (7)
C10—C111.393 (9)O12—H8W0.82 (7)
C10—H100.9300O13—H11W0.81 (8)
C11—C121.369 (9)O13—H12W0.81 (10)
C11—H110.9300O14—H9W0.810 (12)
C12—C131.403 (9)O14—H10W0.81 (9)
C12—H120.9300Tb1—O10ii2.493 (4)
C13—N21.328 (8)Tb1—H2W2.91 (4)
O1—C1—O2125.7 (8)Tb1—O6—H4W112 (8)
O1—C1—C2119.1 (7)H3W—O6—H4W119 (9)
O2—C1—C2115.2 (7)C8—O7—Tb1125.2 (4)
N1—C2—C3121.1 (8)C14—O9—Tb1125.3 (4)
N1—C2—C1116.0 (7)C14—O10—Tb1i143.4 (4)
C3—C2—C1122.9 (8)H5W—O11—H6W118 (11)
C2—C3—C4118.7 (9)H7W—O12—H8W116 (11)
C2—C3—H3120.6H11W—O13—H12W116 (12)
C4—C3—H3120.7H9W—O14—H10W116 (10)
C5—C4—C3120.1 (9)O5—Tb1—O6141.19 (17)
C5—C4—H4A120.0O5—Tb1—O10ii71.34 (16)
C3—C4—H4A120.0O6—Tb1—O10ii70.77 (16)
C6—C5—C4117.5 (8)O5—Tb1—O279.49 (18)
C6—C5—H5121.3O6—Tb1—O298.0 (2)
C4—C5—H5121.2O10ii—Tb1—O274.20 (16)
N1—C6—C5121.9 (8)O5—Tb1—O786.65 (18)
N1—C6—C7115.3 (7)O6—Tb1—O778.3 (2)
C5—C6—C7122.8 (8)O10ii—Tb1—O779.02 (16)
O3—C7—O4123.9 (8)O2—Tb1—O7152.60 (16)
O3—C7—C6119.4 (7)O5—Tb1—O973.05 (17)
O4—C7—C6116.7 (7)O6—Tb1—O9144.46 (17)
O8—C8—O7126.7 (6)O10ii—Tb1—O9136.75 (15)
O8—C8—C9118.3 (6)O2—Tb1—O975.91 (15)
O7—C8—C9115.0 (6)O7—Tb1—O9122.43 (14)
N2—C9—C10122.9 (6)O5—Tb1—O3141.05 (17)
N2—C9—C8115.4 (5)O6—Tb1—O371.56 (17)
C10—C9—C8121.8 (6)O10ii—Tb1—O3140.01 (16)
C11—C10—C9117.0 (6)O2—Tb1—O3124.28 (17)
C11—C10—H10121.5O7—Tb1—O380.72 (16)
C9—C10—H10121.5O9—Tb1—O383.04 (16)
C12—C11—C10120.2 (6)O5—Tb1—N1133.26 (18)
C12—C11—H11119.9O6—Tb1—N173.8 (2)
C10—C11—H11119.9O10ii—Tb1—N1117.83 (17)
C11—C12—C13118.8 (6)O2—Tb1—N162.20 (16)
C11—C12—H12120.6O7—Tb1—N1139.00 (17)
C13—C12—H12120.6O9—Tb1—N172.47 (17)
N2—C13—C12122.3 (6)O3—Tb1—N162.35 (17)
N2—C13—C14114.2 (5)O5—Tb1—N276.67 (17)
C12—C13—C14123.4 (6)O6—Tb1—N2123.7 (2)
O10—C14—O9125.7 (6)O10ii—Tb1—N2129.89 (16)
O10—C14—C13117.6 (6)O2—Tb1—N2135.72 (16)
O9—C14—C13116.7 (6)O7—Tb1—N261.35 (15)
C2—N1—C6120.7 (7)O9—Tb1—N261.70 (14)
C2—N1—Tb1119.8 (5)O3—Tb1—N264.91 (16)
C6—N1—Tb1119.3 (5)N1—Tb1—N2112.22 (16)
C13—N2—C9118.9 (5)O5—Tb1—H2W15.9 (5)
C13—N2—Tb1120.9 (4)O6—Tb1—H2W139 (2)
C9—N2—Tb1119.0 (4)O10ii—Tb1—H2W69 (2)
C1—O2—Tb1126.5 (5)O2—Tb1—H2W63.6 (5)
C7—O3—Tb1123.3 (5)O7—Tb1—H2W101.4 (7)
C7—O4—H4109.5O9—Tb1—H2W70 (2)
Tb1—O5—H1W114 (3)O3—Tb1—H2W149 (2)
Tb1—O5—H2W114 (3)N1—Tb1—H2W119.4 (9)
H1W—O5—H2W112 (7)N2—Tb1—H2W89.0 (16)
Tb1—O6—H3W116 (3)
Symmetry codes: (i) x, −y+3/2, z+1/2; (ii) x, −y+3/2, z−1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5—H1W···O11iii0.81 (6)2.08 (5)2.743 (7)138 (7)
O6—H3W···O1iv0.81 (8)1.97 (4)2.714 (7)154 (9)
O6—H4W···O9ii0.81 (10)2.05 (7)2.719 (7)140 (11)
O11—H5W···O7ii0.80 (11)2.15 (11)2.913 (7)159 (11)
O11—H6W···O8v0.81 (10)2.10 (10)2.893 (7)167 (13)
O14—H9W···O11vi0.81 (1)2.15 (4)2.926 (8)159 (11)
O14—H10W···O8vii0.81 (9)1.92 (9)2.690 (7)157 (11)
O4—H4···O13viii0.821.742.522 (12)160
Symmetry codes: (ii) x, −y+3/2, z−1/2; (iii) x, y, z+1; (iv) −x+1, y+1/2, −z+3/2; (v) −x+2, −y+2, −z+1; (vi) −x+1, −y+1, −z+1; (vii) −x+1, y−1/2, −z+3/2; (viii) x, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5—H1W···O11i0.81 (6)2.08 (5)2.743 (7)138 (7)
O6—H3W···O1ii0.81 (8)1.97 (4)2.714 (7)154 (9)
O6—H4W···O9iii0.81 (10)2.05 (7)2.719 (7)140 (11)
O11—H5W···O7iii0.80 (11)2.15 (11)2.913 (7)159 (11)
O11—H6W···O8iv0.81 (10)2.10 (10)2.893 (7)167 (13)
O14—H9W···O11v0.810 (12)2.15 (4)2.926 (8)159 (11)
O14—H10W···O8vi0.81 (9)1.92 (9)2.690 (7)157 (11)
O4—H4···O13vii0.821.742.522 (12)159.7
Symmetry codes: (i) x, y, z+1; (ii) −x+1, y+1/2, −z+3/2; (iii) x, −y+3/2, z−1/2; (iv) −x+2, −y+2, −z+1; (v) −x+1, −y+1, −z+1; (vi) −x+1, y−1/2, −z+3/2; (vii) x, y+1, z.
references
References top

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