Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807034629/rk2026sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807034629/rk2026Isup2.hkl |
CCDC reference: 1270866
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.011 Å
- R factor = 0.042
- wR factor = 0.131
- Data-to-parameter ratio = 11.0
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT417_ALERT_2_B Short Inter D-H..H-D H2W .. H7W .. 2.06 Ang. PLAT417_ALERT_2_B Short Inter D-H..H-D H4 .. H11W .. 1.97 Ang. PLAT417_ALERT_2_B Short Inter D-H..H-D H4 .. H12W .. 1.99 Ang. PLAT420_ALERT_2_B D-H Without Acceptor O12 - H8W ... ?
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.98 PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.66 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.81 Ratio PLAT342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 11
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K PLAT794_ALERT_5_G Check Predicted Bond Valency for Tb1 (3) 2.59 PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 189
0 ALERT level A = In general: serious problem 4 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 4 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 ALERT type 2 Indicator that the structure model may be wrong or deficient 4 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
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).
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%.
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).
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.
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).
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.
[Tb(C7H3NO4)(C7H4NO4)(H2O)2]·4H2O | F(000) = 1176 |
Mr = 598.24 | Dx = 1.977 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 3499 reflections |
a = 13.9986 (3) Å | θ = 1.5–25.0° |
b = 11.3819 (2) Å | µ = 3.60 mm−1 |
c = 12.8982 (2) Å | T = 293 K |
β = 102.0126 (10)° | Cube, colourless |
V = 2010.08 (6) Å3 | 0.10 × 0.10 × 0.10 mm |
Z = 4 |
Bruker APEXII CCD area-detector diffractometer | 3499 independent reflections |
Radiation source: fine-focus sealed tube | 3237 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.022 |
φ and ω scans | θmax = 25.2°, θmin = 1.5° |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | h = −16→16 |
Tmin = 0.715, Tmax = 0.715 | k = −13→13 |
7168 measured reflections | l = −7→15 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.042 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.131 | H 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 parameters | Δρmax = 1.20 e Å−3 |
189 restraints | Δρmin = −2.00 e Å−3 |
[Tb(C7H3NO4)(C7H4NO4)(H2O)2]·4H2O | V = 2010.08 (6) Å3 |
Mr = 598.24 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 13.9986 (3) Å | µ = 3.60 mm−1 |
b = 11.3819 (2) Å | T = 293 K |
c = 12.8982 (2) Å | 0.10 × 0.10 × 0.10 mm |
β = 102.0126 (10)° |
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 = 0.715 | Rint = 0.022 |
7168 measured reflections |
R[F2 > 2σ(F2)] = 0.042 | 189 restraints |
wR(F2) = 0.131 | H 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 | Δρmax = 1.20 e Å−3 |
317 parameters | Δρmin = −2.00 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
C1 | 0.5673 (6) | 0.5764 (8) | 0.8725 (7) | 0.0353 (9) | |
C2 | 0.5029 (6) | 0.6849 (8) | 0.8698 (7) | 0.0358 (8) | |
C3 | 0.4056 (6) | 0.6786 (8) | 0.8673 (7) | 0.0363 (8) | |
H3 | 0.3749 | 0.6062 | 0.8679 | 0.044* | |
C4 | 0.3521 (7) | 0.7840 (7) | 0.8636 (8) | 0.0369 (8) | |
H4A | 0.2852 | 0.7815 | 0.8610 | 0.044* | |
C5 | 0.3989 (6) | 0.8910 (8) | 0.8638 (7) | 0.0364 (8) | |
H5 | 0.3648 | 0.9614 | 0.8617 | 0.044* | |
C6 | 0.4975 (6) | 0.8894 (8) | 0.8671 (7) | 0.0360 (8) | |
C7 | 0.5573 (6) | 0.9998 (8) | 0.8682 (7) | 0.0358 (9) | |
C8 | 0.8806 (5) | 1.0253 (6) | 0.8263 (5) | 0.0179 (7) | |
C9 | 0.8732 (5) | 1.0388 (6) | 0.9408 (5) | 0.0176 (6) | |
C10 | 0.9082 (5) | 1.1397 (6) | 1.0001 (5) | 0.0180 (6) | |
H10 | 0.9344 | 1.2028 | 0.9696 | 0.022* | |
C11 | 0.9018 (5) | 1.1406 (6) | 1.1065 (5) | 0.0182 (6) | |
H11 | 0.9247 | 1.2050 | 1.1488 | 0.022* | |
C12 | 0.8619 (5) | 1.0469 (6) | 1.1489 (5) | 0.0178 (6) | |
H12 | 0.8585 | 1.0464 | 1.2201 | 0.021* | |
C13 | 0.8264 (5) | 0.9519 (6) | 1.0829 (5) | 0.0175 (6) | |
C14 | 0.7743 (5) | 0.8473 (6) | 1.1189 (5) | 0.0173 (7) | |
H1W | 0.909 (4) | 0.718 (4) | 0.987 (5) | 0.080* | |
H2W | 0.863 (3) | 0.612 (4) | 0.952 (8) | 0.080* | |
H3W | 0.595 (6) | 0.899 (7) | 0.672 (3) | 0.080* | |
H4W | 0.665 (8) | 0.841 (10) | 0.629 (6) | 0.080* | |
H5W | 0.924 (8) | 0.676 (10) | 0.190 (8) | 0.080* | |
H6W | 0.988 (9) | 0.753 (7) | 0.158 (9) | 0.080* | |
H7W | 0.788 (10) | 0.465 (5) | 0.888 (8) | 0.080* | |
H8W | 0.791 (12) | 0.397 (10) | 0.977 (5) | 0.080* | |
H9W | 0.023 (10) | 0.4869 (17) | 0.898 (8) | 0.080* | |
H10W | 0.038 (10) | 0.589 (8) | 0.847 (5) | 0.080* | |
H11W | 0.608 (9) | 0.300 (12) | 0.826 (4) | 0.080* | |
H12W | 0.674 (6) | 0.238 (11) | 0.899 (9) | 0.080* | |
N1 | 0.5474 (5) | 0.7881 (5) | 0.8674 (5) | 0.0201 (13) | |
N2 | 0.8315 (4) | 0.9488 (4) | 0.9813 (4) | 0.0111 (10) | |
O1 | 0.5308 (4) | 0.4780 (5) | 0.8764 (5) | 0.0400 (15) | |
O2 | 0.6558 (4) | 0.5971 (4) | 0.8704 (4) | 0.0227 (10) | |
O3 | 0.6432 (4) | 0.9921 (4) | 0.8649 (4) | 0.0257 (11) | |
O4 | 0.5122 (5) | 1.0991 (5) | 0.8733 (6) | 0.0464 (16) | |
H4 | 0.5471 | 1.1535 | 0.8619 | 0.070* | |
O5 | 0.8754 (4) | 0.6841 (5) | 0.9368 (4) | 0.0255 (11) | |
O6 | 0.6333 (4) | 0.8452 (6) | 0.6743 (4) | 0.0372 (15) | |
O7 | 0.8449 (4) | 0.9295 (4) | 0.7819 (3) | 0.0224 (10) | |
O8 | 0.9207 (4) | 1.1044 (5) | 0.7853 (4) | 0.0303 (12) | |
O9 | 0.7268 (4) | 0.7815 (4) | 1.0468 (4) | 0.0175 (10) | |
O10 | 0.7813 (4) | 0.8336 (4) | 1.2163 (3) | 0.0200 (10) | |
O11 | 0.9581 (4) | 0.6919 (5) | 0.1491 (4) | 0.0251 (12) | |
O12 | 0.7991 (8) | 0.4014 (7) | 0.9163 (9) | 0.086 (3) | |
O13 | 0.6236 (7) | 0.2750 (8) | 0.8855 (10) | 0.082 (3) | |
O14 | 0.0299 (5) | 0.5576 (5) | 0.9011 (4) | 0.0338 (13) | |
Tb1 | 0.73015 (2) | 0.79481 (3) | 0.85156 (2) | 0.01780 (18) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0230 (18) | 0.039 (2) | 0.044 (2) | 0.0056 (14) | 0.0088 (15) | 0.0012 (15) |
C2 | 0.0236 (17) | 0.0396 (19) | 0.0450 (19) | 0.0060 (13) | 0.0087 (14) | 0.0012 (14) |
C3 | 0.0239 (17) | 0.0399 (19) | 0.0458 (19) | 0.0059 (13) | 0.0087 (14) | 0.0013 (14) |
C4 | 0.0242 (17) | 0.0403 (19) | 0.0469 (19) | 0.0061 (13) | 0.0086 (14) | 0.0012 (14) |
C5 | 0.0241 (17) | 0.0399 (19) | 0.0456 (19) | 0.0064 (13) | 0.0086 (14) | 0.0011 (14) |
C6 | 0.0239 (17) | 0.0396 (19) | 0.0451 (19) | 0.0063 (13) | 0.0087 (14) | 0.0010 (14) |
C7 | 0.0241 (18) | 0.039 (2) | 0.045 (2) | 0.0065 (14) | 0.0085 (15) | 0.0007 (15) |
C8 | 0.0207 (15) | 0.0176 (14) | 0.0149 (14) | −0.0021 (12) | 0.0024 (12) | −0.0008 (12) |
C9 | 0.0205 (13) | 0.0172 (13) | 0.0146 (13) | −0.0022 (11) | 0.0024 (10) | −0.0009 (10) |
C10 | 0.0209 (13) | 0.0175 (13) | 0.0149 (13) | −0.0024 (11) | 0.0023 (10) | −0.0009 (10) |
C11 | 0.0212 (14) | 0.0176 (13) | 0.0150 (13) | −0.0024 (11) | 0.0019 (10) | −0.0011 (11) |
C12 | 0.0208 (13) | 0.0174 (13) | 0.0146 (13) | −0.0024 (11) | 0.0022 (10) | −0.0009 (10) |
C13 | 0.0204 (13) | 0.0172 (13) | 0.0145 (13) | −0.0022 (11) | 0.0024 (10) | −0.0008 (10) |
C14 | 0.0201 (15) | 0.0170 (14) | 0.0142 (14) | −0.0023 (12) | 0.0026 (12) | −0.0006 (12) |
N1 | 0.018 (3) | 0.026 (3) | 0.015 (3) | −0.002 (2) | 0.001 (2) | −0.001 (2) |
N2 | 0.011 (2) | 0.013 (3) | 0.010 (2) | −0.0026 (19) | 0.0016 (18) | −0.0017 (19) |
O1 | 0.030 (3) | 0.021 (3) | 0.065 (4) | −0.013 (2) | 0.003 (3) | 0.002 (3) |
O2 | 0.020 (2) | 0.017 (2) | 0.031 (3) | −0.0016 (19) | 0.004 (2) | −0.002 (2) |
O3 | 0.027 (3) | 0.017 (2) | 0.032 (3) | 0.007 (2) | 0.002 (2) | −0.003 (2) |
O4 | 0.048 (4) | 0.029 (3) | 0.060 (4) | 0.015 (3) | 0.008 (3) | −0.004 (3) |
O5 | 0.026 (3) | 0.035 (3) | 0.013 (2) | 0.007 (2) | −0.002 (2) | −0.005 (2) |
O6 | 0.041 (3) | 0.056 (4) | 0.012 (2) | 0.033 (3) | 0.000 (2) | 0.001 (2) |
O7 | 0.035 (3) | 0.022 (2) | 0.012 (2) | −0.011 (2) | 0.010 (2) | −0.0040 (18) |
O8 | 0.047 (3) | 0.025 (3) | 0.023 (3) | −0.016 (2) | 0.017 (2) | 0.000 (2) |
O9 | 0.021 (2) | 0.021 (2) | 0.009 (2) | −0.0107 (18) | 0.0010 (18) | −0.0008 (17) |
O10 | 0.027 (3) | 0.021 (2) | 0.010 (2) | −0.008 (2) | 0.0006 (19) | 0.0020 (19) |
O11 | 0.026 (3) | 0.030 (3) | 0.018 (3) | −0.003 (2) | 0.003 (2) | 0.000 (2) |
O12 | 0.069 (6) | 0.039 (4) | 0.135 (9) | 0.014 (4) | −0.014 (7) | 0.000 (5) |
O13 | 0.068 (6) | 0.044 (5) | 0.128 (10) | 0.003 (4) | 0.008 (6) | 0.003 (5) |
O14 | 0.048 (4) | 0.029 (3) | 0.030 (3) | 0.010 (3) | 0.022 (3) | 0.001 (2) |
Tb1 | 0.0184 (3) | 0.0198 (3) | 0.0146 (2) | −0.00110 (11) | 0.00191 (15) | −0.00124 (11) |
C1—O1 | 1.237 (10) | C13—C14 | 1.518 (9) |
C1—O2 | 1.267 (10) | C14—O10 | 1.249 (8) |
C1—C2 | 1.525 (11) | C14—O9 | 1.269 (8) |
C2—N1 | 1.332 (11) | N1—Tb1 | 2.610 (6) |
C2—C3 | 1.358 (12) | N2—Tb1 | 2.626 (5) |
C3—C4 | 1.410 (12) | O2—Tb1 | 2.512 (5) |
C3—H3 | 0.9300 | O3—Tb1 | 2.578 (5) |
C4—C5 | 1.382 (13) | O4—H4 | 0.8200 |
C4—H4A | 0.9300 | O5—Tb1 | 2.449 (5) |
C5—C6 | 1.373 (11) | O5—H1W | 0.81 (6) |
C5—H5 | 0.9300 | O5—H2W | 0.87 (5) |
C6—N1 | 1.347 (10) | O6—Tb1 | 2.470 (5) |
C6—C7 | 1.509 (12) | O6—H3W | 0.81 (8) |
C7—O3 | 1.214 (10) | O6—H4W | 0.81 (10) |
C7—O4 | 1.303 (10) | O7—Tb1 | 2.517 (5) |
C8—O8 | 1.237 (8) | O9—Tb1 | 2.533 (5) |
C8—O7 | 1.284 (8) | O10—Tb1i | 2.493 (4) |
C8—C9 | 1.510 (9) | O11—H5W | 0.80 (11) |
C9—N2 | 1.337 (8) | O11—H6W | 0.81 (10) |
C9—C10 | 1.410 (9) | O12—H7W | 0.81 (7) |
C10—C11 | 1.393 (9) | O12—H8W | 0.82 (7) |
C10—H10 | 0.9300 | O13—H11W | 0.81 (8) |
C11—C12 | 1.369 (9) | O13—H12W | 0.81 (10) |
C11—H11 | 0.9300 | O14—H9W | 0.810 (12) |
C12—C13 | 1.403 (9) | O14—H10W | 0.81 (9) |
C12—H12 | 0.9300 | Tb1—O10ii | 2.493 (4) |
C13—N2 | 1.328 (8) | Tb1—H2W | 2.91 (4) |
O1—C1—O2 | 125.7 (8) | Tb1—O6—H4W | 112 (8) |
O1—C1—C2 | 119.1 (7) | H3W—O6—H4W | 119 (9) |
O2—C1—C2 | 115.2 (7) | C8—O7—Tb1 | 125.2 (4) |
N1—C2—C3 | 121.1 (8) | C14—O9—Tb1 | 125.3 (4) |
N1—C2—C1 | 116.0 (7) | C14—O10—Tb1i | 143.4 (4) |
C3—C2—C1 | 122.9 (8) | H5W—O11—H6W | 118 (11) |
C2—C3—C4 | 118.7 (9) | H7W—O12—H8W | 116 (11) |
C2—C3—H3 | 120.6 | H11W—O13—H12W | 116 (12) |
C4—C3—H3 | 120.7 | H9W—O14—H10W | 116 (10) |
C5—C4—C3 | 120.1 (9) | O5—Tb1—O6 | 141.19 (17) |
C5—C4—H4A | 120.0 | O5—Tb1—O10ii | 71.34 (16) |
C3—C4—H4A | 120.0 | O6—Tb1—O10ii | 70.77 (16) |
C6—C5—C4 | 117.5 (8) | O5—Tb1—O2 | 79.49 (18) |
C6—C5—H5 | 121.3 | O6—Tb1—O2 | 98.0 (2) |
C4—C5—H5 | 121.2 | O10ii—Tb1—O2 | 74.20 (16) |
N1—C6—C5 | 121.9 (8) | O5—Tb1—O7 | 86.65 (18) |
N1—C6—C7 | 115.3 (7) | O6—Tb1—O7 | 78.3 (2) |
C5—C6—C7 | 122.8 (8) | O10ii—Tb1—O7 | 79.02 (16) |
O3—C7—O4 | 123.9 (8) | O2—Tb1—O7 | 152.60 (16) |
O3—C7—C6 | 119.4 (7) | O5—Tb1—O9 | 73.05 (17) |
O4—C7—C6 | 116.7 (7) | O6—Tb1—O9 | 144.46 (17) |
O8—C8—O7 | 126.7 (6) | O10ii—Tb1—O9 | 136.75 (15) |
O8—C8—C9 | 118.3 (6) | O2—Tb1—O9 | 75.91 (15) |
O7—C8—C9 | 115.0 (6) | O7—Tb1—O9 | 122.43 (14) |
N2—C9—C10 | 122.9 (6) | O5—Tb1—O3 | 141.05 (17) |
N2—C9—C8 | 115.4 (5) | O6—Tb1—O3 | 71.56 (17) |
C10—C9—C8 | 121.8 (6) | O10ii—Tb1—O3 | 140.01 (16) |
C11—C10—C9 | 117.0 (6) | O2—Tb1—O3 | 124.28 (17) |
C11—C10—H10 | 121.5 | O7—Tb1—O3 | 80.72 (16) |
C9—C10—H10 | 121.5 | O9—Tb1—O3 | 83.04 (16) |
C12—C11—C10 | 120.2 (6) | O5—Tb1—N1 | 133.26 (18) |
C12—C11—H11 | 119.9 | O6—Tb1—N1 | 73.8 (2) |
C10—C11—H11 | 119.9 | O10ii—Tb1—N1 | 117.83 (17) |
C11—C12—C13 | 118.8 (6) | O2—Tb1—N1 | 62.20 (16) |
C11—C12—H12 | 120.6 | O7—Tb1—N1 | 139.00 (17) |
C13—C12—H12 | 120.6 | O9—Tb1—N1 | 72.47 (17) |
N2—C13—C12 | 122.3 (6) | O3—Tb1—N1 | 62.35 (17) |
N2—C13—C14 | 114.2 (5) | O5—Tb1—N2 | 76.67 (17) |
C12—C13—C14 | 123.4 (6) | O6—Tb1—N2 | 123.7 (2) |
O10—C14—O9 | 125.7 (6) | O10ii—Tb1—N2 | 129.89 (16) |
O10—C14—C13 | 117.6 (6) | O2—Tb1—N2 | 135.72 (16) |
O9—C14—C13 | 116.7 (6) | O7—Tb1—N2 | 61.35 (15) |
C2—N1—C6 | 120.7 (7) | O9—Tb1—N2 | 61.70 (14) |
C2—N1—Tb1 | 119.8 (5) | O3—Tb1—N2 | 64.91 (16) |
C6—N1—Tb1 | 119.3 (5) | N1—Tb1—N2 | 112.22 (16) |
C13—N2—C9 | 118.9 (5) | O5—Tb1—H2W | 15.9 (5) |
C13—N2—Tb1 | 120.9 (4) | O6—Tb1—H2W | 139 (2) |
C9—N2—Tb1 | 119.0 (4) | O10ii—Tb1—H2W | 69 (2) |
C1—O2—Tb1 | 126.5 (5) | O2—Tb1—H2W | 63.6 (5) |
C7—O3—Tb1 | 123.3 (5) | O7—Tb1—H2W | 101.4 (7) |
C7—O4—H4 | 109.5 | O9—Tb1—H2W | 70 (2) |
Tb1—O5—H1W | 114 (3) | O3—Tb1—H2W | 149 (2) |
Tb1—O5—H2W | 114 (3) | N1—Tb1—H2W | 119.4 (9) |
H1W—O5—H2W | 112 (7) | N2—Tb1—H2W | 89.0 (16) |
Tb1—O6—H3W | 116 (3) |
Symmetry codes: (i) x, −y+3/2, z+1/2; (ii) x, −y+3/2, z−1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H1W···O11iii | 0.81 (6) | 2.08 (5) | 2.743 (7) | 138 (7) |
O6—H3W···O1iv | 0.81 (8) | 1.97 (4) | 2.714 (7) | 154 (9) |
O6—H4W···O9ii | 0.81 (10) | 2.05 (7) | 2.719 (7) | 140 (11) |
O11—H5W···O7ii | 0.80 (11) | 2.15 (11) | 2.913 (7) | 159 (11) |
O11—H6W···O8v | 0.81 (10) | 2.10 (10) | 2.893 (7) | 167 (13) |
O14—H9W···O11vi | 0.81 (1) | 2.15 (4) | 2.926 (8) | 159 (11) |
O14—H10W···O8vii | 0.81 (9) | 1.92 (9) | 2.690 (7) | 157 (11) |
O4—H4···O13viii | 0.82 | 1.74 | 2.522 (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. |
Experimental details
Crystal data | |
Chemical formula | [Tb(C7H3NO4)(C7H4NO4)(H2O)2]·4H2O |
Mr | 598.24 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 293 |
a, b, c (Å) | 13.9986 (3), 11.3819 (2), 12.8982 (2) |
β (°) | 102.0126 (10) |
V (Å3) | 2010.08 (6) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 3.60 |
Crystal size (mm) | 0.10 × 0.10 × 0.10 |
Data collection | |
Diffractometer | Bruker APEXII CCD area-detector |
Absorption correction | Multi-scan (SADABS; Bruker, 2001) |
Tmin, Tmax | 0.715, 0.715 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 7168, 3499, 3237 |
Rint | 0.022 |
(sin θ/λ)max (Å−1) | 0.599 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.042, 0.131, 1.00 |
No. of reflections | 3499 |
No. of parameters | 317 |
No. of restraints | 189 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
w = 1/[σ2(Fo2) + (0.0953P)2 + 13.066P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 1.20, −2.00 |
Computer programs: APEX2 (Bruker, Year?), SAINT-Plus (Bruker, 2001), SAINT-Plus, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 2001), SHELXTL.
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H1W···O11i | 0.81 (6) | 2.08 (5) | 2.743 (7) | 138 (7) |
O6—H3W···O1ii | 0.81 (8) | 1.97 (4) | 2.714 (7) | 154 (9) |
O6—H4W···O9iii | 0.81 (10) | 2.05 (7) | 2.719 (7) | 140 (11) |
O11—H5W···O7iii | 0.80 (11) | 2.15 (11) | 2.913 (7) | 159 (11) |
O11—H6W···O8iv | 0.81 (10) | 2.10 (10) | 2.893 (7) | 167 (13) |
O14—H9W···O11v | 0.810 (12) | 2.15 (4) | 2.926 (8) | 159 (11) |
O14—H10W···O8vi | 0.81 (9) | 1.92 (9) | 2.690 (7) | 157 (11) |
O4—H4···O13vii | 0.82 | 1.74 | 2.522 (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. |
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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.