The isonicotinate (4-pyridylcarboxylate) ligand was used to synthesize the title compound, [Nd(C6H4NO2)3(H2O)2]. It has a one-dimensional chain structure. The Nd atom lies on a crystallographic twofold axis. The NdIII center is in an infinite chain, coordinated by four carboxylate O atoms of bridging isonicotinate groups, two carboxylate O atoms of the chelating isonicotinate group, and two water molecules. Weak interactions between pyridine H and N atoms generate a three-dimensional framework.
Supporting information
CCDC reference: 214786
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.008 Å
- R factor = 0.029
- wR factor = 0.074
- Data-to-parameter ratio = 10.7
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
The ligand sodium isonicotinate (4-pyridylcarboxylate) was prepared as follows: 20 mmol of isonicotinate acid and 20 mmol sodium bicarbonate were mixed together in 20 ml aqueous solvent. The mixture was stirred at room temperature. After the reaction was completed, the solution was concentrated to get the ligand compound. Single purple crystals of the title complex, (I), were grown by evaporation at room temperature. Neodymium(III) nitrate hexahydrate (1 mmol) and sodium isonicotinate (3 mmol) were mixed in water (10 ml). The solution was filtered and the filtrate was placed for about one day for crystallization.
All the H atoms were located in difference Fourier maps and were refined isotropically.
Data collection: CAD-4 Software (Enraf-Nonius, 1989); cell refinement: CAD-4 Software; data reduction: XCAD4 (Harms & Wocadlo, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 2000); software used to prepare material for publication: SHELXTL.
Diaquatris(4-pyridylcarboxylato)neodymium(III)
top
Crystal data top
[Nd(C6H4NO2)3(H2O)2] | F(000) = 1076 |
Mr = 546.58 | Dx = 1.856 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 27 reflections |
a = 9.526 (2) Å | θ = 2.6–26.1° |
b = 19.053 (4) Å | µ = 2.71 mm−1 |
c = 10.787 (2) Å | T = 293 K |
β = 92.19 (3)° | Block, purple |
V = 1956.4 (7) Å3 | 0.40 × 0.37 × 0.22 mm |
Z = 4 | |
Data collection top
Enraf-Nonius CAD-4 diffractometer | 2830 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.025 |
Graphite monochromator | θmax = 25.0°, θmin = 2.1° |
ω scans | h = 0→11 |
Absorption correction: ψ scan (XCAD4; Harms & Wocadlo, 1995) | k = 0→22 |
Tmin = 0.352, Tmax = 0.551 | l = −12→12 |
3656 measured reflections | 3 standard reflections every 200 reflections |
3441 independent reflections | intensity decay: 0.0% |
Refinement top
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)] = 0.029 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.074 | w = 1/[σ2(Fo2) + (0.0342P)2 + 1.6679P] where P = (Fo2 + 2Fc2)/3 |
S = 1.07 | (Δ/σ)max = 0.002 |
3441 reflections | Δρmax = 0.80 e Å−3 |
323 parameters | Δρmin = −1.16 e Å−3 |
0 restraints | |
Crystal data top
[Nd(C6H4NO2)3(H2O)2] | V = 1956.4 (7) Å3 |
Mr = 546.58 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 9.526 (2) Å | µ = 2.71 mm−1 |
b = 19.053 (4) Å | T = 293 K |
c = 10.787 (2) Å | 0.40 × 0.37 × 0.22 mm |
β = 92.19 (3)° | |
Data collection top
Enraf-Nonius CAD-4 diffractometer | 2830 reflections with I > 2σ(I) |
Absorption correction: ψ scan (XCAD4; Harms & Wocadlo, 1995) | Rint = 0.025 |
Tmin = 0.352, Tmax = 0.551 | 3 standard reflections every 200 reflections |
3656 measured reflections | intensity decay: 0.0% |
3441 independent reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.029 | 0 restraints |
wR(F2) = 0.074 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.07 | Δρmax = 0.80 e Å−3 |
3441 reflections | Δρmin = −1.16 e Å−3 |
323 parameters | |
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 > σ(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 | Uiso*/Ueq | |
Nd1 | 0.25241 (2) | 0.51046 (2) | −0.04413 (2) | 0.01957 (9) | |
O1 | 0.3452 (3) | 0.56756 (18) | 0.1506 (3) | 0.0316 (8) | |
O2 | 0.1446 (3) | 0.61303 (16) | 0.0849 (3) | 0.0276 (7) | |
O3 | 0.1012 (4) | 0.46213 (19) | 0.1093 (3) | 0.0349 (8) | |
O4 | −0.0965 (3) | 0.44003 (19) | 0.2017 (3) | 0.0373 (9) | |
O5 | 0.3780 (3) | 0.61452 (17) | −0.1132 (3) | 0.0357 (8) | |
O6 | 0.5803 (3) | 0.57285 (17) | −0.0386 (3) | 0.0328 (8) | |
O1W | 0.1373 (3) | 0.40425 (17) | −0.1363 (3) | 0.0317 (8) | |
H1WA | 0.0614 | 0.3892 | −0.1176 | 0.040 (17)* | |
H1WB | 0.1919 | 0.3689 | −0.1676 | 0.034 (14)* | |
O2W | 0.3869 (4) | 0.47161 (19) | −0.2241 (3) | 0.0359 (8) | |
H2WA | 0.4622 | 0.4508 | −0.2061 | 0.039 (16)* | |
H2WB | 0.3600 | 0.4595 | −0.2906 | 0.05 (2)* | |
N1 | 0.2392 (6) | 0.7218 (3) | 0.5086 (5) | 0.0594 (15) | |
N2 | 0.2602 (5) | 0.4250 (3) | 0.5534 (4) | 0.0474 (12) | |
N3 | 0.7190 (5) | 0.7923 (2) | −0.2603 (5) | 0.0436 (12) | |
C1 | 0.2397 (5) | 0.6480 (3) | 0.2845 (5) | 0.0307 (11) | |
C2 | 0.3105 (7) | 0.6233 (3) | 0.3886 (6) | 0.0503 (16) | |
H2 | 0.356 (6) | 0.578 (3) | 0.379 (5) | 0.055 (18)* | |
C3 | 0.3052 (9) | 0.6607 (4) | 0.4979 (6) | 0.066 (2) | |
H3 | 0.350 (7) | 0.638 (3) | 0.569 (6) | 0.06 (2)* | |
C4 | 0.1732 (6) | 0.7461 (3) | 0.4061 (6) | 0.0454 (15) | |
H4 | 0.142 (6) | 0.788 (3) | 0.410 (5) | 0.049 (18)* | |
C5 | 0.1671 (6) | 0.7108 (3) | 0.2944 (5) | 0.0344 (12) | |
H5 | 0.129 (5) | 0.730 (3) | 0.235 (5) | 0.026 (15)* | |
C6 | 0.2430 (5) | 0.6081 (2) | 0.1653 (4) | 0.0260 (10) | |
C7 | 0.1137 (5) | 0.4339 (2) | 0.3240 (4) | 0.0259 (10) | |
C8 | 0.2597 (6) | 0.4396 (3) | 0.3340 (5) | 0.0356 (13) | |
H8 | 0.315 (6) | 0.448 (3) | 0.282 (5) | 0.037 (16)* | |
C9 | 0.3263 (6) | 0.4345 (3) | 0.4484 (5) | 0.0429 (14) | |
H9 | 0.431 (7) | 0.439 (3) | 0.454 (6) | 0.062 (19)* | |
C10 | 0.1204 (7) | 0.4175 (4) | 0.5430 (5) | 0.0531 (17) | |
H10 | 0.077 (7) | 0.411 (3) | 0.615 (6) | 0.06 (2)* | |
C11 | 0.0429 (6) | 0.4220 (3) | 0.4305 (5) | 0.0434 (14) | |
H11 | −0.063 (6) | 0.419 (3) | 0.430 (5) | 0.044 (15)* | |
C12 | 0.0344 (5) | 0.4458 (2) | 0.2028 (4) | 0.0231 (10) | |
C13 | 0.5088 (5) | 0.6182 (2) | −0.0950 (4) | 0.0255 (10) | |
C14 | 0.5812 (5) | 0.6813 (2) | −0.1492 (4) | 0.0239 (10) | |
C15 | 0.5129 (5) | 0.7233 (3) | −0.2358 (5) | 0.0303 (11) | |
H15 | 0.423 (6) | 0.718 (3) | −0.261 (5) | 0.041 (16)* | |
C16 | 0.7194 (5) | 0.6963 (3) | −0.1179 (6) | 0.0381 (13) | |
H16 | 0.763 (6) | 0.672 (3) | −0.065 (5) | 0.043 (17)* | |
C17 | 0.7824 (6) | 0.7517 (3) | −0.1756 (7) | 0.0507 (17) | |
H17 | 0.858 (6) | 0.765 (3) | −0.147 (5) | 0.046 (18)* | |
C18 | 0.5864 (6) | 0.7779 (3) | −0.2883 (5) | 0.0389 (13) | |
H18 | 0.541 (5) | 0.796 (3) | −0.350 (5) | 0.031 (14)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Nd1 | 0.01718 (14) | 0.02338 (14) | 0.01805 (14) | −0.00097 (10) | −0.00064 (9) | 0.00036 (10) |
O1 | 0.0171 (17) | 0.045 (2) | 0.0328 (19) | 0.0040 (15) | −0.0032 (14) | −0.0111 (15) |
O2 | 0.0201 (17) | 0.0347 (18) | 0.0277 (18) | −0.0015 (14) | −0.0025 (14) | −0.0049 (14) |
O3 | 0.037 (2) | 0.045 (2) | 0.0227 (18) | −0.0063 (16) | 0.0000 (16) | 0.0069 (15) |
O4 | 0.0177 (18) | 0.057 (2) | 0.036 (2) | −0.0001 (16) | −0.0075 (15) | 0.0070 (17) |
O5 | 0.0236 (19) | 0.0344 (19) | 0.049 (2) | −0.0072 (14) | −0.0002 (17) | 0.0101 (16) |
O6 | 0.0319 (19) | 0.0305 (19) | 0.036 (2) | 0.0044 (15) | 0.0031 (16) | 0.0100 (15) |
O1W | 0.0189 (18) | 0.0320 (19) | 0.045 (2) | −0.0037 (14) | 0.0083 (15) | −0.0150 (16) |
O2W | 0.0221 (18) | 0.062 (2) | 0.0230 (19) | 0.0042 (17) | −0.0021 (15) | −0.0084 (17) |
N1 | 0.070 (4) | 0.068 (4) | 0.041 (3) | 0.005 (3) | 0.000 (3) | −0.022 (3) |
N2 | 0.051 (3) | 0.061 (3) | 0.029 (3) | 0.009 (2) | −0.015 (2) | 0.003 (2) |
N3 | 0.045 (3) | 0.030 (2) | 0.057 (3) | −0.005 (2) | 0.011 (2) | 0.012 (2) |
C1 | 0.023 (3) | 0.039 (3) | 0.030 (3) | −0.007 (2) | 0.006 (2) | −0.008 (2) |
C2 | 0.059 (4) | 0.055 (4) | 0.036 (3) | 0.012 (3) | −0.008 (3) | −0.014 (3) |
C3 | 0.084 (5) | 0.069 (5) | 0.042 (4) | 0.019 (4) | −0.015 (4) | −0.016 (3) |
C4 | 0.038 (3) | 0.040 (3) | 0.058 (4) | −0.003 (3) | 0.007 (3) | −0.019 (3) |
C5 | 0.025 (3) | 0.042 (3) | 0.037 (3) | −0.004 (2) | 0.002 (2) | −0.008 (3) |
C6 | 0.020 (2) | 0.028 (2) | 0.030 (3) | −0.010 (2) | 0.004 (2) | −0.006 (2) |
C7 | 0.021 (2) | 0.032 (3) | 0.025 (3) | 0.0014 (19) | −0.004 (2) | 0.000 (2) |
C8 | 0.025 (3) | 0.048 (3) | 0.034 (3) | 0.001 (2) | 0.004 (2) | 0.001 (2) |
C9 | 0.026 (3) | 0.059 (4) | 0.042 (4) | 0.004 (3) | −0.013 (3) | −0.001 (3) |
C10 | 0.047 (4) | 0.089 (5) | 0.023 (3) | 0.003 (3) | 0.003 (3) | 0.014 (3) |
C11 | 0.028 (3) | 0.073 (4) | 0.030 (3) | 0.001 (3) | 0.000 (2) | 0.012 (3) |
C12 | 0.027 (3) | 0.021 (2) | 0.021 (2) | 0.0000 (18) | 0.000 (2) | 0.0031 (18) |
C13 | 0.024 (3) | 0.025 (2) | 0.028 (3) | −0.0012 (19) | 0.005 (2) | 0.0004 (19) |
C14 | 0.020 (2) | 0.023 (2) | 0.030 (3) | −0.0001 (18) | 0.004 (2) | −0.0005 (19) |
C15 | 0.023 (3) | 0.031 (3) | 0.037 (3) | −0.001 (2) | −0.001 (2) | 0.005 (2) |
C16 | 0.024 (3) | 0.037 (3) | 0.052 (4) | −0.007 (2) | −0.008 (3) | 0.019 (3) |
C17 | 0.026 (3) | 0.051 (4) | 0.074 (5) | −0.015 (3) | −0.006 (3) | 0.011 (3) |
C18 | 0.037 (3) | 0.041 (3) | 0.039 (3) | 0.005 (2) | 0.001 (3) | 0.010 (3) |
Geometric parameters (Å, º) top
Nd1—O6i | 2.397 (3) | C1—C2 | 1.370 (8) |
Nd1—O4ii | 2.406 (3) | C1—C5 | 1.388 (7) |
Nd1—O3 | 2.417 (3) | C1—C6 | 1.495 (6) |
Nd1—O5 | 2.446 (3) | C2—C3 | 1.381 (8) |
Nd1—O2W | 2.480 (3) | C2—H2 | 0.98 (6) |
Nd1—O1W | 2.490 (3) | C3—H3 | 0.97 (6) |
Nd1—O1 | 2.497 (3) | C4—C5 | 1.380 (8) |
Nd1—O2 | 2.631 (3) | C4—H4 | 0.85 (6) |
Nd1—C6 | 2.931 (5) | C5—H5 | 0.81 (5) |
O1—C6 | 1.259 (5) | C7—C11 | 1.373 (7) |
O2—C6 | 1.255 (5) | C7—C8 | 1.395 (7) |
O3—C12 | 1.252 (5) | C7—C12 | 1.502 (6) |
O4—C12 | 1.252 (5) | C8—C9 | 1.369 (8) |
O4—Nd1ii | 2.406 (3) | C8—H8 | 0.80 (5) |
O5—C13 | 1.256 (6) | C9—H9 | 1.00 (7) |
O6—C13 | 1.245 (5) | C10—C11 | 1.399 (8) |
O6—Nd1i | 2.397 (3) | C10—H10 | 0.90 (6) |
O1W—H1WA | 0.8108 | C11—H11 | 1.02 (6) |
O1W—H1WB | 0.9232 | C13—C14 | 1.513 (6) |
O2W—H2WA | 0.8358 | C14—C15 | 1.375 (7) |
O2W—H2WB | 0.7865 | C14—C16 | 1.377 (7) |
N1—C3 | 1.329 (9) | C15—C18 | 1.388 (7) |
N1—C4 | 1.334 (8) | C15—H15 | 0.89 (6) |
N2—C9 | 1.330 (7) | C16—C17 | 1.375 (8) |
N2—C10 | 1.340 (8) | C16—H16 | 0.83 (5) |
N3—C18 | 1.316 (7) | C17—H17 | 0.81 (6) |
N3—C17 | 1.324 (8) | C18—H18 | 0.86 (5) |
| | | |
O6i—Nd1—O4ii | 154.96 (13) | C1—C2—C3 | 119.3 (6) |
O6i—Nd1—O3 | 84.14 (12) | C1—C2—H2 | 115 (3) |
O4ii—Nd1—O3 | 105.38 (12) | C3—C2—H2 | 126 (4) |
O6i—Nd1—O5 | 108.91 (11) | N1—C3—C2 | 124.0 (7) |
O4ii—Nd1—O5 | 76.28 (12) | N1—C3—H3 | 122 (4) |
O3—Nd1—O5 | 145.91 (12) | C2—C3—H3 | 114 (4) |
O6i—Nd1—O2W | 74.80 (12) | N1—C4—C5 | 123.8 (6) |
O4ii—Nd1—O2W | 83.53 (12) | N1—C4—H4 | 116 (4) |
O3—Nd1—O2W | 139.60 (13) | C5—C4—H4 | 119 (4) |
O5—Nd1—O2W | 74.35 (12) | C4—C5—C1 | 118.9 (6) |
O6i—Nd1—O1W | 83.51 (12) | C4—C5—H5 | 118 (4) |
O4ii—Nd1—O1W | 77.66 (12) | C1—C5—H5 | 123 (4) |
O3—Nd1—O1W | 72.48 (11) | O2—C6—O1 | 121.3 (4) |
O5—Nd1—O1W | 138.59 (12) | O2—C6—C1 | 121.1 (4) |
O2W—Nd1—O1W | 71.20 (11) | O1—C6—C1 | 117.5 (4) |
O6i—Nd1—O1 | 76.49 (11) | O2—C6—Nd1 | 63.8 (2) |
O4ii—Nd1—O1 | 127.76 (12) | O1—C6—Nd1 | 57.7 (2) |
O3—Nd1—O1 | 77.94 (11) | C1—C6—Nd1 | 171.1 (3) |
O5—Nd1—O1 | 75.01 (12) | C11—C7—C8 | 117.9 (5) |
O2W—Nd1—O1 | 127.71 (11) | C11—C7—C12 | 120.4 (4) |
O1W—Nd1—O1 | 145.70 (12) | C8—C7—C12 | 121.5 (4) |
O6i—Nd1—O2 | 124.21 (11) | C9—C8—C7 | 119.4 (5) |
O4ii—Nd1—O2 | 80.78 (11) | C9—C8—H8 | 110 (4) |
O3—Nd1—O2 | 70.48 (11) | C7—C8—H8 | 130 (4) |
O5—Nd1—O2 | 76.36 (11) | N2—C9—C8 | 124.0 (5) |
O2W—Nd1—O2 | 149.30 (11) | N2—C9—H9 | 118 (4) |
O1W—Nd1—O2 | 129.80 (10) | C8—C9—H9 | 118 (4) |
O1—Nd1—O2 | 50.51 (10) | N2—C10—C11 | 123.8 (6) |
O6i—Nd1—C6 | 99.97 (13) | N2—C10—H10 | 115 (4) |
O4ii—Nd1—C6 | 105.02 (13) | C11—C10—H10 | 121 (4) |
O3—Nd1—C6 | 71.18 (12) | C7—C11—C10 | 118.4 (5) |
O5—Nd1—C6 | 75.51 (12) | C7—C11—H11 | 122 (3) |
O2W—Nd1—C6 | 145.59 (12) | C10—C11—H11 | 120 (3) |
O1W—Nd1—C6 | 142.89 (12) | O4—C12—O3 | 123.4 (4) |
O1—Nd1—C6 | 25.23 (11) | O4—C12—C7 | 117.6 (4) |
O2—Nd1—C6 | 25.35 (11) | O3—C12—C7 | 118.9 (4) |
C6—O1—Nd1 | 97.1 (3) | O6—C13—O5 | 123.9 (4) |
C6—O2—Nd1 | 90.8 (3) | O6—C13—C14 | 119.4 (4) |
C12—O3—Nd1 | 168.7 (3) | O5—C13—C14 | 116.6 (4) |
C12—O4—Nd1ii | 124.1 (3) | C15—C14—C16 | 117.9 (4) |
C13—O5—Nd1 | 119.5 (3) | C15—C14—C13 | 120.9 (4) |
C13—O6—Nd1i | 170.1 (3) | C16—C14—C13 | 121.1 (4) |
Nd1—O1W—H1WA | 124.9 | C14—C15—C18 | 118.7 (5) |
Nd1—O1W—H1WB | 119.6 | C14—C15—H15 | 124 (3) |
H1WA—O1W—H1WB | 110.6 | C18—C15—H15 | 117 (4) |
Nd1—O2W—H2WA | 115.1 | C17—C16—C14 | 118.6 (5) |
Nd1—O2W—H2WB | 129.9 | C17—C16—H16 | 121 (4) |
H2WA—O2W—H2WB | 108.7 | C14—C16—H16 | 120 (4) |
C3—N1—C4 | 116.2 (5) | N3—C17—C16 | 124.4 (6) |
C9—N2—C10 | 116.4 (5) | N3—C17—H17 | 117 (4) |
C18—N3—C17 | 116.4 (5) | C16—C17—H17 | 118 (4) |
C2—C1—C5 | 117.7 (5) | N3—C18—C15 | 123.9 (5) |
C2—C1—C6 | 120.3 (5) | N3—C18—H18 | 124 (4) |
C5—C1—C6 | 122.0 (5) | C15—C18—H18 | 112 (4) |
Symmetry codes: (i) −x+1, −y+1, −z; (ii) −x, −y+1, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···O2ii | 0.81 | 2.01 | 2.782 (4) | 160 |
O1W—H1WB···N3iii | 0.92 | 1.87 | 2.791 (5) | 173 |
O2W—H2WA···O1i | 0.84 | 1.94 | 2.746 (5) | 162 |
O2W—H2WB···N2iv | 0.79 | 2.01 | 2.790 (6) | 170 |
Symmetry codes: (i) −x+1, −y+1, −z; (ii) −x, −y+1, −z; (iii) −x+1, y−1/2, −z−1/2; (iv) x, y, z−1. |
Experimental details
Crystal data |
Chemical formula | [Nd(C6H4NO2)3(H2O)2] |
Mr | 546.58 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 293 |
a, b, c (Å) | 9.526 (2), 19.053 (4), 10.787 (2) |
β (°) | 92.19 (3) |
V (Å3) | 1956.4 (7) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 2.71 |
Crystal size (mm) | 0.40 × 0.37 × 0.22 |
|
Data collection |
Diffractometer | Enraf-Nonius CAD-4 diffractometer |
Absorption correction | ψ scan (XCAD4; Harms & Wocadlo, 1995) |
Tmin, Tmax | 0.352, 0.551 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 3656, 3441, 2830 |
Rint | 0.025 |
(sin θ/λ)max (Å−1) | 0.594 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.029, 0.074, 1.07 |
No. of reflections | 3441 |
No. of parameters | 323 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.80, −1.16 |
Selected geometric parameters (Å, º) topNd1—O6i | 2.397 (3) | Nd1—O2W | 2.480 (3) |
Nd1—O4ii | 2.406 (3) | Nd1—O1W | 2.490 (3) |
Nd1—O3 | 2.417 (3) | Nd1—O1 | 2.497 (3) |
Nd1—O5 | 2.446 (3) | Nd1—O2 | 2.631 (3) |
| | | |
O6i—Nd1—O4ii | 154.96 (13) | O2—C6—C1 | 121.1 (4) |
O6i—Nd1—O3 | 84.14 (12) | O1—C6—C1 | 117.5 (4) |
O4ii—Nd1—O3 | 105.38 (12) | O4—C12—O3 | 123.4 (4) |
O6i—Nd1—O5 | 108.91 (11) | O4—C12—C7 | 117.6 (4) |
O4ii—Nd1—O5 | 76.28 (12) | O3—C12—C7 | 118.9 (4) |
O3—Nd1—O5 | 145.91 (12) | O6—C13—O5 | 123.9 (4) |
O2W—Nd1—O1W | 71.20 (11) | O6—C13—C14 | 119.4 (4) |
O1—Nd1—O2 | 50.51 (10) | O5—C13—C14 | 116.6 (4) |
O2—C6—O1 | 121.3 (4) | | |
Symmetry codes: (i) −x+1, −y+1, −z; (ii) −x, −y+1, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···O2ii | 0.81 | 2.01 | 2.782 (4) | 160 |
O1W—H1WB···N3iii | 0.92 | 1.87 | 2.791 (5) | 173 |
O2W—H2WA···O1i | 0.84 | 1.94 | 2.746 (5) | 162 |
O2W—H2WB···N2iv | 0.79 | 2.01 | 2.790 (6) | 170 |
Symmetry codes: (i) −x+1, −y+1, −z; (ii) −x, −y+1, −z; (iii) −x+1, y−1/2, −z−1/2; (iv) x, y, z−1. |
There has been intent interest in the synthesis and construction of lanthanide complexes with carboxylate ligands, owing to their potential application as luminescent sensor materials in biological devices (Choppin & Bünzli, 1989). Numerous lanthanide complexes have been studied (Bünzli & Piguet, 2002). Most of them have been found to possess a variety of dimeric or infinte chain structures in which the carboxylate groups act as bridges between metal atoms (Pan et al., 2000). In this context, we have attempted to construct neutral lanthanide coordination polymers using the anionic bifunctional isonicotinate linking group, with the aim of getting a three-dimensional framework and functional solid based on molecular building blocks by both metal–ligand ligations and hydrogen-bond interactions.
We obtained the coordination polymer Nd(4-pyridylcarboxylate)3(H2O)2, (I). The compound crystallizes in the monoclinic space group P21/c. This compound has a one-dimensional infinite zigzag chain structure along the a axis direction with a double carboxylate bridge. The Nd metal center lies on a crystallographic twofold axis. On each metal center, there is a chelating carboxylate group. There are also two water molecules bound to the metal centers to yield an eight-coordinate. The Nd center coordinates to four carboxylate O atoms of bridging isonicotinate groups [O3, O4Ai, O5 and O6Aii; symmetry codes: (i) −x,-y + 1,-z; (ii) −x + 1,-y + 1,-z], two carboxylate O atoms of the chelating isonicotinate group (O1 and O2), and two water molecules (O1W and O2W). The Nd center also has a distorted dodecahedral coordination geometry, with O—Nd—O angles ranging from 50.51 (10) to 154.96 (13)° (Table 1). The distances between adjacent Nd atoms are 4.793(?) and 4.954(?)Å. There are O—H···N interactions between pyridyl N atoms and coordinated water O atoms (O1W—H1WB···N3iii and O2W—H2WB···N2iv; symmetry codes: (iii) 1 − x, −1/2 + y, −1/2 − z; (iv) x, y, −1 + z]. The interchain hydrogen bonds formed between pyridine N atoms of isonicotinate bridging groups and coordinated water molecules steer the assembly of bulk. The hydrogen-bond interactions extend the one-dimensional chains to three-dimensional framework.