metal-organic compounds
Poly[diaqua(μ-oxalato)(μ-2-oxidopyridinium-3-carboxylato)lanthanum(III)]
aAcademic Affairs Division, Southern Medical University, Guangzhou, Guangdong 510515, People's Republic of China, and bSchool of Pharmaceutical Sciences, Southern Medical University, Guangzhou, Guangdong 510515, People's Republic of China
*Correspondence e-mail: zzb24@yahoo.com.cn
In the title complex, [La(C6H4NO3)(C2O4)(H2O)2]n, the LaIII ion is coordinated by eight O atoms from two 2-oxidopyridinium-3-carboxylate ligands, two oxalate ligands and two water molecules in a distorted bicapped square-antiprismatic geometry. The carboxylate groups link adjacent LaIII ions, forming two-dimensional layers that are further linked by N—H⋯O and O—H⋯O hydrogen bonds.
Experimental
Crystal data
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Refinement
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Data collection: APEX2 (Bruker, 2004); cell SAINT (Bruker, 2004); data reduction: SAINT; 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
10.1107/S1600536809018194/bi2356sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536809018194/bi2356Isup2.hkl
A mixture of La2O3 (0.245 g, 0.75 mmol), 2-oxynicotinic acid (0.127 g, 1 mmol), oxalic acid (0.09 g, 1 mmol), water (10 ml) and HNO3 (0.024 g, 0.385 mmol) was stirred vigorously for 20 min then sealed in a Teflon-lined stainless-steel autoclave (20 ml capacity). The autoclave was heated and maintained at 433 K for 4 days, then cooled to room temperature at 5 K h-1 to yield colourless block crystals.
H atoms bound to C and N atoms were placed at calculated positions and refined as riding with N—H = 0.86 Å, C—H = 0.93 Å and with Uiso(H) = 1.2 Ueq(C/N). H atoms of the water molecules were tentatively located in difference Fourier maps and refined with distance restraints of O—H = 0.850 (1) Å and H···H = 1.350 (1) Å. In the final cycles of
the O—H distances were normalized to 0.85 Å and the H atoms were refined as riding with Uiso(H) = 1.5 Ueq(O). Atom H4W forms a symmetrical H-bond about a centre of inversion and therefore is included with site occupancy factor 0.5. The alternative position H4W' points towards the centroid of an adjacent pyridyl ring.Data collection: APEX2 (Bruker, 2004); cell
SAINT (Bruker, 2004); data reduction: SAINT (Bruker, 2004); 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).[La(C6H4NO3)(C2O4)(H2O)2] | Z = 2 |
Mr = 401.06 | F(000) = 384 |
Triclinic, P1 | Dx = 2.424 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.0856 (18) Å | Cell parameters from 2827 reflections |
b = 8.5493 (19) Å | θ = 2.5–28.3° |
c = 9.388 (3) Å | µ = 3.93 mm−1 |
α = 109.281 (3)° | T = 293 K |
β = 104.702 (3)° | Block, colourless |
γ = 104.940 (2)° | 0.20 × 0.18 × 0.17 mm |
V = 549.5 (2) Å3 |
Bruker APEXII CCD diffractometer | 1946 independent reflections |
Radiation source: fine-focus sealed tube | 1870 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.020 |
ϕ and ω scans | θmax = 25.2°, θmin = 2.5° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2003) | h = −7→9 |
Tmin = 0.460, Tmax = 0.512 | k = −10→10 |
2843 measured reflections | l = −11→11 |
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)] = 0.025 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.069 | H-atom parameters constrained |
S = 1.10 | w = 1/[σ2(Fo2) + (0.0415P)2 + 0.4664P] where P = (Fo2 + 2Fc2)/3 |
1946 reflections | (Δ/σ)max < 0.001 |
172 parameters | Δρmax = 0.92 e Å−3 |
0 restraints | Δρmin = −1.37 e Å−3 |
[La(C6H4NO3)(C2O4)(H2O)2] | γ = 104.940 (2)° |
Mr = 401.06 | V = 549.5 (2) Å3 |
Triclinic, P1 | Z = 2 |
a = 8.0856 (18) Å | Mo Kα radiation |
b = 8.5493 (19) Å | µ = 3.93 mm−1 |
c = 9.388 (3) Å | T = 293 K |
α = 109.281 (3)° | 0.20 × 0.18 × 0.17 mm |
β = 104.702 (3)° |
Bruker APEXII CCD diffractometer | 1946 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2003) | 1870 reflections with I > 2σ(I) |
Tmin = 0.460, Tmax = 0.512 | Rint = 0.020 |
2843 measured reflections |
R[F2 > 2σ(F2)] = 0.025 | 0 restraints |
wR(F2) = 0.069 | H-atom parameters constrained |
S = 1.10 | Δρmax = 0.92 e Å−3 |
1946 reflections | Δρmin = −1.37 e Å−3 |
172 parameters |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
C1 | 0.5156 (6) | 0.3528 (6) | 0.7873 (5) | 0.0193 (9) | |
C2 | 0.4448 (6) | 0.2225 (6) | 0.8439 (5) | 0.0190 (9) | |
C3 | 0.5510 (7) | 0.2276 (6) | 0.9869 (5) | 0.0278 (10) | |
H3A | 0.5043 | 0.1411 | 1.0209 | 0.033* | |
C4 | 0.7265 (7) | 0.3590 (7) | 1.0820 (6) | 0.0340 (12) | |
H4A | 0.7963 | 0.3617 | 1.1788 | 0.041* | |
C5 | 0.7924 (6) | 0.4829 (7) | 1.0291 (6) | 0.0310 (11) | |
H5A | 0.9085 | 0.5728 | 1.0910 | 0.037* | |
C6 | 0.2549 (6) | 0.0837 (6) | 0.7555 (5) | 0.0195 (9) | |
C7 | 0.0124 (6) | 0.0944 (6) | 0.0035 (5) | 0.0209 (9) | |
C8 | 0.0714 (6) | 0.5526 (5) | 0.4754 (5) | 0.0180 (8) | |
La1 | 0.14649 (3) | 0.16626 (3) | 0.39929 (2) | 0.01432 (11) | |
N1 | 0.6911 (5) | 0.4769 (5) | 0.8873 (5) | 0.0253 (8) | |
H1A | 0.7393 | 0.5561 | 0.8570 | 0.030* | |
O1 | 0.1395 (4) | 0.0964 (4) | 0.6424 (3) | 0.0215 (7) | |
O2 | 0.2093 (4) | −0.0404 (4) | 0.7976 (4) | 0.0285 (7) | |
O3 | 0.4372 (4) | 0.3643 (4) | 0.6604 (4) | 0.0276 (7) | |
O4 | 0.1045 (5) | 0.2240 (4) | 0.1390 (4) | 0.0258 (7) | |
O5 | −0.0601 (5) | 0.1020 (4) | −0.1273 (4) | 0.0275 (7) | |
O6 | 0.1897 (4) | 0.4906 (4) | 0.4461 (4) | 0.0238 (7) | |
O7 | 0.0581 (4) | 0.6932 (4) | 0.4686 (4) | 0.0263 (7) | |
O1W | 0.4501 (5) | 0.2684 (5) | 0.3496 (4) | 0.0400 (9) | |
H1W | 0.5512 | 0.3270 | 0.4309 | 0.060* | |
H2W | 0.4721 | 0.1911 | 0.2808 | 0.060* | |
O2W | 0.3055 (5) | −0.0633 (5) | 0.4169 (4) | 0.0329 (8) | |
H3W | 0.2604 | −0.1491 | 0.4396 | 0.049* | |
H4W | 0.4214 | −0.0254 | 0.4667 | 0.049* | 0.50 |
H4W' | 0.2871 | −0.1202 | 0.3175 | 0.049* | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.018 (2) | 0.016 (2) | 0.018 (2) | 0.0023 (17) | 0.0060 (17) | 0.0040 (17) |
C2 | 0.017 (2) | 0.017 (2) | 0.0160 (19) | 0.0019 (17) | 0.0018 (17) | 0.0062 (17) |
C3 | 0.027 (2) | 0.023 (2) | 0.024 (2) | 0.002 (2) | 0.000 (2) | 0.012 (2) |
C4 | 0.024 (3) | 0.034 (3) | 0.024 (2) | 0.001 (2) | −0.011 (2) | 0.012 (2) |
C5 | 0.017 (2) | 0.029 (3) | 0.029 (2) | 0.001 (2) | −0.0042 (19) | 0.006 (2) |
C6 | 0.016 (2) | 0.020 (2) | 0.016 (2) | −0.0004 (17) | 0.0025 (17) | 0.0074 (17) |
C7 | 0.021 (2) | 0.024 (2) | 0.017 (2) | 0.0035 (18) | 0.0066 (18) | 0.0103 (18) |
C8 | 0.014 (2) | 0.014 (2) | 0.017 (2) | 0.0005 (17) | −0.0001 (16) | 0.0029 (17) |
La1 | 0.01183 (15) | 0.01383 (16) | 0.01434 (15) | 0.00163 (11) | 0.00223 (11) | 0.00694 (11) |
N1 | 0.0186 (19) | 0.022 (2) | 0.027 (2) | −0.0013 (16) | 0.0045 (16) | 0.0110 (17) |
O1 | 0.0154 (15) | 0.0253 (17) | 0.0172 (15) | 0.0003 (13) | −0.0005 (12) | 0.0118 (13) |
O2 | 0.0215 (17) | 0.0269 (18) | 0.0325 (18) | 0.0002 (14) | 0.0028 (14) | 0.0192 (15) |
O3 | 0.0211 (17) | 0.0312 (18) | 0.0235 (16) | −0.0002 (14) | 0.0014 (14) | 0.0163 (14) |
O4 | 0.0326 (19) | 0.0190 (16) | 0.0157 (15) | −0.0002 (14) | 0.0040 (14) | 0.0068 (13) |
O5 | 0.0369 (19) | 0.0238 (16) | 0.0163 (15) | 0.0085 (15) | 0.0030 (14) | 0.0093 (13) |
O6 | 0.0193 (16) | 0.0192 (16) | 0.0336 (17) | 0.0070 (13) | 0.0107 (14) | 0.0116 (14) |
O7 | 0.0294 (18) | 0.0209 (16) | 0.0373 (18) | 0.0110 (14) | 0.0169 (15) | 0.0177 (14) |
O1W | 0.0197 (18) | 0.057 (2) | 0.0307 (19) | 0.0001 (17) | 0.0090 (15) | 0.0158 (18) |
O2W | 0.0285 (18) | 0.040 (2) | 0.043 (2) | 0.0178 (16) | 0.0155 (16) | 0.0276 (17) |
C1—O3 | 1.248 (5) | La1—O6 | 2.574 (3) |
C1—N1 | 1.382 (6) | La1—O5i | 2.582 (3) |
C1—C2 | 1.437 (6) | La1—O3 | 2.585 (3) |
C2—C3 | 1.377 (6) | La1—O1W | 2.598 (3) |
C2—C6 | 1.489 (6) | La1—O4 | 2.606 (3) |
C3—C4 | 1.395 (7) | La1—O7ii | 2.608 (3) |
C3—H3A | 0.930 | La1—O1iii | 2.612 (3) |
C4—C5 | 1.357 (7) | La1—O2W | 2.634 (3) |
C4—H4A | 0.930 | La1—O2iii | 2.691 (3) |
C5—N1 | 1.351 (6) | N1—H1A | 0.860 |
C5—H5A | 0.930 | O1—La1iii | 2.612 (3) |
C6—O2 | 1.252 (5) | O2—La1iii | 2.691 (3) |
C6—O1 | 1.279 (5) | O5—La1i | 2.582 (3) |
C7—O4 | 1.250 (5) | O7—La1ii | 2.608 (3) |
C7—O5 | 1.251 (5) | O1W—H1W | 0.850 |
C7—C7i | 1.550 (9) | O1W—H2W | 0.850 |
C8—O6 | 1.253 (5) | O2W—H3W | 0.850 |
C8—O7 | 1.255 (5) | O2W—H4W | 0.850 |
C8—C8ii | 1.537 (8) | O2W—H4W' | 0.850 |
La1—O1 | 2.553 (3) | ||
O3—C1—N1 | 118.0 (4) | O1—La1—O1iii | 61.92 (11) |
O3—C1—C2 | 127.4 (4) | O6—La1—O1iii | 130.59 (10) |
N1—C1—C2 | 114.6 (4) | O5i—La1—O1iii | 70.65 (10) |
C3—C2—C1 | 120.0 (4) | O3—La1—O1iii | 127.57 (9) |
C3—C2—C6 | 118.0 (4) | O1W—La1—O1iii | 148.31 (12) |
C1—C2—C6 | 121.9 (4) | O4—La1—O1iii | 111.41 (10) |
C2—C3—C4 | 121.8 (4) | O7ii—La1—O1iii | 72.58 (10) |
C2—C3—H3A | 119.1 | O1—La1—O2W | 68.95 (10) |
C4—C3—H3A | 119.1 | O6—La1—O2W | 147.03 (10) |
C5—C4—C3 | 118.1 (4) | O5i—La1—O2W | 64.56 (10) |
C5—C4—H4A | 121.0 | O3—La1—O2W | 78.73 (11) |
C3—C4—H4A | 121.0 | O1W—La1—O2W | 72.87 (12) |
N1—C5—C4 | 120.6 (4) | O4—La1—O2W | 115.38 (10) |
N1—C5—H5A | 119.7 | O7ii—La1—O2W | 138.08 (10) |
C4—C5—H5A | 119.7 | O1iii—La1—O2W | 81.33 (10) |
O2—C6—O1 | 121.1 (4) | O1—La1—O2iii | 105.06 (9) |
O2—C6—C2 | 119.0 (4) | O6—La1—O2iii | 92.61 (10) |
O1—C6—C2 | 119.8 (4) | O5i—La1—O2iii | 66.21 (10) |
O4—C7—O5 | 126.4 (4) | O3—La1—O2iii | 157.15 (11) |
O4—C7—C7i | 116.9 (4) | O1W—La1—O2iii | 131.48 (11) |
O5—C7—C7i | 116.7 (5) | O4—La1—O2iii | 67.14 (10) |
O6—C8—O7 | 126.1 (4) | O7ii—La1—O2iii | 65.52 (10) |
O6—C8—C8ii | 117.3 (4) | O1iii—La1—O2iii | 49.08 (9) |
O7—C8—C8ii | 116.6 (4) | O2W—La1—O2iii | 118.71 (11) |
O1—La1—O6 | 115.01 (10) | C5—N1—C1 | 124.9 (4) |
O1—La1—O5i | 116.73 (10) | C5—N1—H1A | 117.6 |
O6—La1—O5i | 127.50 (10) | C1—N1—H1A | 117.6 |
O1—La1—O3 | 65.68 (10) | C6—O1—La1 | 135.9 (3) |
O6—La1—O3 | 74.38 (10) | C6—O1—La1iii | 96.3 (3) |
O5i—La1—O3 | 136.55 (11) | La1—O1—La1iii | 118.08 (11) |
O1—La1—O1W | 121.99 (10) | C6—O2—La1iii | 93.3 (2) |
O6—La1—O1W | 78.71 (11) | C1—O3—La1 | 136.4 (3) |
O5i—La1—O1W | 81.66 (11) | C7—O4—La1 | 118.5 (3) |
O3—La1—O1W | 65.28 (11) | C7—O5—La1i | 119.4 (3) |
O1—La1—O4 | 172.10 (10) | C8—O6—La1 | 120.7 (3) |
O6—La1—O4 | 65.38 (10) | C8—O7—La1ii | 119.8 (3) |
O5i—La1—O4 | 62.14 (10) | La1—O1W—H1W | 118.9 |
O3—La1—O4 | 120.98 (10) | La1—O1W—H2W | 118.3 |
O1W—La1—O4 | 65.90 (11) | H1W—O1W—H2W | 105.2 |
O1—La1—O7ii | 69.92 (10) | La1—O2W—H3W | 122.1 |
O6—La1—O7ii | 62.13 (9) | La1—O2W—H4W | 119.6 |
O5i—La1—O7ii | 131.12 (11) | H3W—O2W—H4W | 105.2 |
O3—La1—O7ii | 91.67 (11) | La1—O2W—H4W' | 101.0 |
O1W—La1—O7ii | 139.07 (11) | H3W—O2W—H4W' | 100.6 |
O4—La1—O7ii | 104.60 (10) | H4W—O2W—H4W' | 105.2 |
O3—C1—C2—C3 | 179.2 (4) | N1—C1—O3—La1 | 168.2 (3) |
N1—C1—C2—C3 | −0.4 (6) | C2—C1—O3—La1 | −11.5 (7) |
O3—C1—C2—C6 | −3.1 (7) | O1—La1—O3—C1 | 22.7 (4) |
N1—C1—C2—C6 | 177.2 (4) | O6—La1—O3—C1 | 150.2 (4) |
C1—C2—C3—C4 | 1.3 (7) | O5i—La1—O3—C1 | −81.2 (4) |
C6—C2—C3—C4 | −176.5 (4) | O1W—La1—O3—C1 | −125.3 (4) |
C2—C3—C4—C5 | −0.6 (8) | O4—La1—O3—C1 | −162.1 (4) |
C3—C4—C5—N1 | −0.8 (8) | O7ii—La1—O3—C1 | 89.7 (4) |
C3—C2—C6—O2 | −11.8 (6) | O1iii—La1—O3—C1 | 20.6 (5) |
C1—C2—C6—O2 | 170.5 (4) | O2W—La1—O3—C1 | −49.1 (4) |
C3—C2—C6—O1 | 165.6 (4) | O2iii—La1—O3—C1 | 92.9 (5) |
C1—C2—C6—O1 | −12.0 (6) | O5—C7—O4—La1 | 160.6 (4) |
C4—C5—N1—C1 | 1.7 (7) | C7i—C7—O4—La1 | −20.2 (6) |
O3—C1—N1—C5 | 179.3 (4) | O6—La1—O4—C7 | −157.7 (3) |
C2—C1—N1—C5 | −1.0 (6) | O5i—La1—O4—C7 | 20.9 (3) |
O2—C6—O1—La1 | −137.1 (4) | O3—La1—O4—C7 | 150.7 (3) |
C2—C6—O1—La1 | 45.4 (6) | O1W—La1—O4—C7 | 114.1 (3) |
O2—C6—O1—La1iii | 5.4 (4) | O7ii—La1—O4—C7 | −108.3 (3) |
C2—C6—O1—La1iii | −172.0 (3) | O1iii—La1—O4—C7 | −31.6 (4) |
O6—La1—O1—C6 | −98.9 (4) | O2W—La1—O4—C7 | 58.8 (3) |
O5i—La1—O1—C6 | 90.3 (4) | O2iii—La1—O4—C7 | −53.3 (3) |
O3—La1—O1—C6 | −41.3 (4) | O4—C7—O5—La1i | 159.7 (4) |
O1W—La1—O1—C6 | −6.8 (4) | C7i—C7—O5—La1i | −19.6 (6) |
O7ii—La1—O1—C6 | −142.8 (4) | O7—C8—O6—La1 | −165.0 (3) |
O1iii—La1—O1—C6 | 136.7 (5) | C8ii—C8—O6—La1 | 15.1 (6) |
O2W—La1—O1—C6 | 45.5 (4) | O1—La1—O6—C8 | −63.1 (3) |
O2iii—La1—O1—C6 | 160.9 (4) | O5i—La1—O6—C8 | 106.6 (3) |
O6—La1—O1—La1iii | 124.39 (13) | O3—La1—O6—C8 | −116.0 (3) |
O5i—La1—O1—La1iii | −46.43 (16) | O1W—La1—O6—C8 | 176.7 (3) |
O3—La1—O1—La1iii | −178.07 (17) | O4—La1—O6—C8 | 108.2 (3) |
O1W—La1—O1—La1iii | −143.50 (14) | O7ii—La1—O6—C8 | −15.6 (3) |
O7ii—La1—O1—La1iii | 80.43 (14) | O1iii—La1—O6—C8 | 10.4 (4) |
O1iii—La1—O1—La1iii | 0.0 | O2W—La1—O6—C8 | −152.6 (3) |
O2W—La1—O1—La1iii | −91.27 (15) | O2iii—La1—O6—C8 | 44.9 (3) |
O2iii—La1—O1—La1iii | 24.16 (15) | O6—C8—O7—La1ii | −165.3 (3) |
O1—C6—O2—La1iii | −5.2 (4) | C8ii—C8—O7—La1ii | 14.7 (6) |
C2—C6—O2—La1iii | 172.2 (3) |
Symmetry codes: (i) −x, −y, −z; (ii) −x, −y+1, −z+1; (iii) −x, −y, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···O4iv | 0.86 | 1.96 | 2.789 (5) | 162 |
O1W—H1W···O6iv | 0.85 | 2.01 | 2.805 (5) | 155 |
O2W—H4W···O2Wv | 0.85 | 2.00 | 2.853 (7) | 180 |
O2W—H3W···O7vi | 0.85 | 1.97 | 2.753 (5) | 152 |
Symmetry codes: (iv) −x+1, −y+1, −z+1; (v) −x+1, −y, −z+1; (vi) x, y−1, z. |
Experimental details
Crystal data | |
Chemical formula | [La(C6H4NO3)(C2O4)(H2O)2] |
Mr | 401.06 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 8.0856 (18), 8.5493 (19), 9.388 (3) |
α, β, γ (°) | 109.281 (3), 104.702 (3), 104.940 (2) |
V (Å3) | 549.5 (2) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 3.93 |
Crystal size (mm) | 0.20 × 0.18 × 0.17 |
Data collection | |
Diffractometer | Bruker APEXII CCD diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 2003) |
Tmin, Tmax | 0.460, 0.512 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 2843, 1946, 1870 |
Rint | 0.020 |
(sin θ/λ)max (Å−1) | 0.599 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.025, 0.069, 1.10 |
No. of reflections | 1946 |
No. of parameters | 172 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.92, −1.37 |
Computer programs: APEX2 (Bruker, 2004), SAINT (Bruker, 2004), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···O4i | 0.86 | 1.96 | 2.789 (5) | 162 |
O1W—H1W···O6i | 0.85 | 2.01 | 2.805 (5) | 155 |
O2W—H4W···O2Wii | 0.85 | 2.00 | 2.853 (7) | 180 |
O2W—H3W···O7iii | 0.85 | 1.97 | 2.753 (5) | 152 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, −y, −z+1; (iii) x, y−1, z. |
Acknowledgements
The authors acknowledge Southern Medical University for supporting this work.
References
Bruker (2004). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Huang, C.-D., Huang, J.-X., Wu, Y.-Y., Lian, Y.-Y. & Zeng, R.-H. (2009). Acta Cryst. E65, m177–m178. Web of Science CSD CrossRef IUCr Journals Google Scholar
Sheldrick, G. M. (2003). SADABS. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Xu, Y.-J., Yang, X.-X. & Zhao, H.-B. (2009). Acta Cryst. E65, m310. Web of Science CSD CrossRef IUCr Journals Google Scholar
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Whereas a large number of metal derivatives of oxalic acid have been reported, there are few examples of metal derivatives of 2-oxynicotinic acid and oxalic acid: the crystal structures of praseodymium (Xu et al., 2009) and dysprosium (Huang et al., 2009) derivatives have been reported only. We report here a lanthanum(III) complex formed by reaction of lanthanum nitrate, 2-oxynicotinic acid and oxalic acid under hydrothermal conditions.
As illustrated in Fig. 1, each LaIII centre adopts a distorted bicapped square-antiprismatic geometry, defined by eight O atoms from two 2-oxynicotinate ligands, two oxalate ligands, and two water molecules. The 2-oxynicotinate ligands and oxalate ligands link the LaIII ions to form layers in the bc plane in which the shortest La···La separation is 4.429 (3) Å. These layers are connected through O—H···O and N—H···O hydrogen bonding (Table 1) involving 2-oxynicotinate ligands, oxalate ligands and the coordinating water molecules, forming a three-dimensional supramolecular network motif (Fig. 2).