Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807032059/xu2283sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807032059/xu2283Isup2.hkl |
CCDC reference: 294166
A mixture of La(NO3)3.6H2O (0.060 g, 0.25 mmol), pyridine-2,5-dicarboxylic acid (0.084 g, 0.50 mmol) and H2O (15 ml) was sealed in a 25 ml stainless steel reactor with a Teflon liner and heated at 433 K for 72 h. The mixture was cooled slowly to room temperature at a rate of 10 K.h-1. Straw yellow prism crystals of the title complex were collected by filtration and were obtained in 21% yield. Analysis calculated for C14H13LaN2O11 (%): C 32.08, H 2.50, N 5.34; found: C 32.11, H 2.53, N 5.36
Aromatic H atoms were placed in geometrically idealized positions with C—H = 0.93 Å and refined in the riding-model approximation with Uiso(H) = 1.2Ueq(C). Carboxyl H atoms were placed in calculated position with O—H = 0.82 Å and refined in riding mode with Uiso(H) = 1.5Ueq(O). Water H atoms were placed in calculated positions with O—H = 0.85 Å and refined in riding mode with Uiso(H) = 1.2Ueq(O). The highest peak and deepest hole appear at 1.22 Å from H14 and 0.83 Å from H21A, respectively.
In recent years, studies on the syntheses, structures and properties of coordination complexes containing lanthanum and aromatic carboxylate have intensely attracted much attention, because they possess potential application on catalysis, separation, gas deposition and luminescence (Chae et al., 2004; Seo et al., 2000; Bradshaw et al., 2004; Lu et al., 2006). As a multi-functional ligand, pyridine-2,5-dicarboxylic acid has been widely used in the preparation of 3 d-4f heterometallic coordination polymers (Liang et al., 2000; Liang et al., 2001) and transition metallic supra-molecular compounds (Min et al., 2001; Xu et al., 2001; Gao et al., 2005). However the investigation on the lanthanum complexes is relative limited (Song et al., 2005). We report here the crystal structure of the title LaIII polymeric compound.
A segment of the polymeric structure of the title compound is illustrated in Fig. 1. Each LaIII ion is nine-coordinated by two nitrogen atoms from Hpydc and pydc ligands, five oxygen atoms from carboxylate groups of one Hpydc and four pydc ligands and two water molecules. The pydc2- anion acts as chelating-bridging pentadentate ligand towards four LaIII ions. The pyridine nitrogen atom and the ortho-carboxylic oxygen atom chelate one La ion, and this oxygen atom and other two carboxylic oxygen atoms of the pydc ligand bridge another three different La ions. The Hpydc- anion acts as chelating bidentate ligand towards the La ion with a pyridine nitrogen atom and the ortho carboxylic oxygen atom, which is similar to the coordination mode of Hpydc in [Dy(Hpydc)(pydc)(phen)(H2O).H2O]n [phen=1,10-phenanthroline] (Song et al., 2005) and [Ln(Hpydc)(pydc)] [Ln = Sm, Eu, Gd] (Qin et al., 2005). The La···La separations in the same unit and between adjacent units are 4.339 (9) and 5.619 (9) Å, respectively. The La center is in a slightly distorted tricapped trigonal prism coordination geometry. Adjacent La ions are linked together through single-atom carboxylate oxygen atom and carboxylate group in the syn-anti mode, forming a two-dimensional polymeric layer structure as represented in Fig. 2. Selected geometric parameters are listed in Table 1. The La—O bond lengths fall in range from 2.498 (10) to 2.658 (9) Å.
Extensive N—H···O and O—H···O hydrogen bonding occur in the crystal structure of the title compound, and connect adjacent layers into the infinite three-dimensional supramolecular network structure (Table 2 and Fig. 3).
For general background, see: Chae et al. (2004); Seo et al. (2000); Bradshaw et al. (2004); Lu et al. (2006); Liang et al. (2000, 2001); Min et al. (2001); Xu et al. (2001); Gao et al. (2005). For related structures, see: Song et al. (2005); Qin et al. (2005).
Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXTL.
[La2(C7H4NO4)2(C7H3NO4)2(H2O)4]·2H2O | F(000) = 1024 |
Mr = 1048.35 | Dx = 2.088 Mg m−3 |
Monoclinic, P21 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2yb | Cell parameters from 3211 reflections |
a = 9.2203 (18) Å | θ = 2.2–20.5° |
b = 19.744 (4) Å | µ = 2.63 mm−1 |
c = 9.3552 (19) Å | T = 293 K |
β = 101.72 (3)° | Prism, yellow |
V = 1667.5 (6) Å3 | 0.35 × 0.34 × 0.27 mm |
Z = 2 |
Bruker SMART CCD area-detector diffractometer | 5778 independent reflections |
Radiation source: fine-focus sealed tube | 5491 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.093 |
φ and ω scans | θmax = 25.0°, θmin = 3.0° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −10→10 |
Tmin = 0.428, Tmax = 0.490 | k = −23→23 |
12319 measured reflections | l = −11→11 |
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)] = 0.064 | H-atom parameters constrained |
wR(F2) = 0.174 | w = 1/[σ2(Fo2) + (0.0958P)2 + 9.9455P] where P = (Fo2 + 2Fc2)/3 |
S = 1.06 | (Δ/σ)max = 0.001 |
5778 reflections | Δρmax = 1.82 e Å−3 |
505 parameters | Δρmin = −3.93 e Å−3 |
1 restraint | Absolute structure: Flack (1983), 2752 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.50 (4) |
[La2(C7H4NO4)2(C7H3NO4)2(H2O)4]·2H2O | V = 1667.5 (6) Å3 |
Mr = 1048.35 | Z = 2 |
Monoclinic, P21 | Mo Kα radiation |
a = 9.2203 (18) Å | µ = 2.63 mm−1 |
b = 19.744 (4) Å | T = 293 K |
c = 9.3552 (19) Å | 0.35 × 0.34 × 0.27 mm |
β = 101.72 (3)° |
Bruker SMART CCD area-detector diffractometer | 5778 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 5491 reflections with I > 2σ(I) |
Tmin = 0.428, Tmax = 0.490 | Rint = 0.093 |
12319 measured reflections |
R[F2 > 2σ(F2)] = 0.064 | H-atom parameters constrained |
wR(F2) = 0.174 | Δρmax = 1.82 e Å−3 |
S = 1.06 | Δρmin = −3.93 e Å−3 |
5778 reflections | Absolute structure: Flack (1983), 2752 Friedel pairs |
505 parameters | Absolute structure parameter: 0.50 (4) |
1 restraint |
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 | ||
La1 | 0.46937 (8) | 0.05700 (3) | 0.39796 (8) | 0.0112 (2) | |
La2 | 0.28724 (8) | 0.07667 (3) | 0.93428 (8) | 0.0107 (2) | |
N1 | 0.5695 (13) | −0.0629 (6) | 0.5397 (14) | 0.016 (3) | |
N2 | −0.2524 (13) | 0.0334 (6) | 0.3592 (13) | 0.014 (3) | |
N3 | 0.0116 (13) | 0.1009 (6) | 0.9728 (13) | 0.015 (3) | |
N4 | 0.1862 (13) | 0.1969 (6) | 0.7924 (13) | 0.014 (3) | |
O1 | 0.3674 (11) | −0.0545 (5) | 0.2910 (11) | 0.015 (2) | |
O2 | 0.2676 (12) | −0.1539 (5) | 0.3372 (12) | 0.024 (2) | |
O3 | 0.9397 (13) | −0.0864 (6) | 0.8710 (13) | 0.024 (3) | |
O4 | 0.8767 (12) | −0.1922 (5) | 0.9100 (13) | 0.026 (3) | |
H4B | 0.9385 | −0.1884 | 0.9860 | 0.038* | |
O5 | 0.2708 (11) | 0.0173 (5) | 0.5298 (11) | 0.014 (2) | |
O6 | 0.1288 (10) | 0.0513 (5) | 0.6871 (10) | 0.0148 (19) | |
O7 | −0.3646 (11) | −0.0298 (6) | 0.0010 (12) | 0.021 (2) | |
O8 | −0.4868 (10) | 0.0364 (5) | 0.1292 (10) | 0.011 (2) | |
O9 | 0.4727 (13) | 0.2909 (5) | 1.0127 (13) | 0.029 (3) | |
O10 | 0.3905 (11) | 0.1868 (5) | 1.0408 (11) | 0.016 (2) | |
O11 | −0.1719 (12) | 0.2227 (5) | 0.4463 (12) | 0.020 (2) | |
O12 | −0.0761 (13) | 0.3223 (5) | 0.3902 (13) | 0.026 (3) | |
H12A | −0.1476 | 0.3221 | 0.3218 | 0.040* | |
O13 | 0.2497 (11) | 0.0993 (5) | 1.2010 (11) | 0.015 (2) | |
O14 | 0.1265 (12) | 0.1662 (6) | 1.3299 (12) | 0.023 (2) | |
O15 | −0.3697 (10) | 0.0818 (5) | 0.6455 (10) | 0.0145 (19) | |
O16 | −0.5110 (11) | 0.1124 (5) | 0.7993 (11) | 0.017 (2) | |
O17 | 0.3846 (11) | −0.0285 (5) | 0.8125 (11) | 0.016 (2) | |
H17A | 0.4683 | −0.0311 | 0.8705 | 0.019* | |
H17C | 0.3985 | −0.0053 | 0.7400 | 0.019* | |
O18 | 0.1967 (11) | −0.0318 (5) | 1.0239 (11) | 0.016 (2) | |
H18A | 0.2358 | −0.0457 | 1.1090 | 0.019* | |
H18C | 0.1178 | −0.0542 | 0.9929 | 0.019* | |
O19 | 0.3764 (12) | 0.1608 (5) | 0.5188 (12) | 0.018 (2) | |
H19A | 0.2862 | 0.1573 | 0.4756 | 0.022* | |
H19B | 0.3869 | 0.1431 | 0.6031 | 0.022* | |
O20 | 0.5648 (11) | 0.1658 (5) | 0.3042 (12) | 0.019 (2) | |
H20A | 0.5504 | 0.1549 | 0.2145 | 0.022* | |
H20B | 0.6562 | 0.1606 | 0.3414 | 0.022* | |
O21 | 0.7230 (12) | 0.3388 (5) | 0.1594 (13) | 0.027 (3) | |
H21B | 0.6464 | 0.3190 | 0.1118 | 0.033* | |
H21C | 0.7003 | 0.3796 | 0.1734 | 0.033* | |
O22 | 0.1319 (14) | 0.7993 (6) | 0.0723 (16) | 0.040 (3) | |
H22A | 0.1775 | 0.8147 | 0.1540 | 0.048* | |
H22B | 0.1779 | 0.8119 | 0.0068 | 0.048* | |
C1 | 0.3653 (16) | −0.1095 (7) | 0.3636 (16) | 0.016 (3) | |
C2 | 0.4906 (16) | −0.1192 (7) | 0.4931 (16) | 0.015 (3) | |
C3 | 0.5209 (16) | −0.1821 (8) | 0.5549 (17) | 0.017 (3) | |
H3A | 0.4613 | −0.2191 | 0.5205 | 0.021* | |
C4 | 0.6448 (16) | −0.1899 (7) | 0.6723 (17) | 0.018 (3) | |
H4A | 0.6699 | −0.2318 | 0.7156 | 0.021* | |
C5 | 0.7253 (16) | −0.1331 (7) | 0.7187 (17) | 0.016 (3) | |
C6 | 0.8590 (16) | −0.1344 (7) | 0.8433 (17) | 0.017 (3) | |
C7 | 0.6853 (16) | −0.0696 (8) | 0.6544 (16) | 0.016 (3) | |
H7A | 0.7393 | −0.0315 | 0.6913 | 0.019* | |
C8 | 0.1461 (15) | 0.0313 (7) | 0.5627 (16) | 0.014 (3) | |
C9 | 0.0120 (16) | 0.0184 (7) | 0.4480 (16) | 0.013 (3) | |
C10 | 0.0192 (16) | −0.0138 (7) | 0.3160 (16) | 0.015 (3) | |
H10A | 0.1094 | −0.0302 | 0.3007 | 0.018* | |
C11 | −0.1064 (15) | −0.0214 (7) | 0.2089 (17) | 0.014 (3) | |
H11A | −0.1001 | −0.0431 | 0.1221 | 0.017* | |
C12 | −0.2384 (16) | 0.0021 (7) | 0.2280 (16) | 0.014 (3) | |
C13 | −0.3733 (15) | 0.0021 (7) | 0.1096 (16) | 0.014 (3) | |
C14 | −0.1313 (15) | 0.0397 (7) | 0.4643 (16) | 0.014 (3) | |
H14 | −0.1410 | 0.0590 | 0.5526 | 0.017* | |
C15 | 0.1360 (16) | 0.1339 (7) | 1.2190 (16) | 0.014 (3) | |
C16 | −0.0017 (16) | 0.1304 (7) | 1.0937 (16) | 0.013 (3) | |
C17 | −0.1335 (16) | 0.1583 (7) | 1.1211 (17) | 0.016 (3) | |
H17B | −0.1360 | 0.1813 | 1.2073 | 0.019* | |
C18 | −0.2594 (16) | 0.1499 (7) | 1.0130 (16) | 0.014 (3) | |
H18B | −0.3503 | 0.1665 | 1.0259 | 0.017* | |
C19 | −0.2479 (16) | 0.1164 (7) | 0.8852 (16) | 0.014 (3) | |
C20 | −0.3863 (15) | 0.1042 (7) | 0.7739 (16) | 0.013 (3) | |
C21 | −0.1135 (15) | 0.0917 (7) | 0.8690 (15) | 0.014 (3) | |
H21A | −0.1075 | 0.0679 | 0.7846 | 0.017* | |
C22 | 0.3880 (16) | 0.2428 (7) | 0.9726 (16) | 0.017 (3) | |
C23 | 0.2723 (16) | 0.2512 (7) | 0.8339 (16) | 0.016 (3) | |
C24 | 0.2569 (17) | 0.3121 (7) | 0.7608 (17) | 0.018 (3) | |
H24A | 0.3219 | 0.3478 | 0.7911 | 0.022* | |
C25 | 0.1432 (17) | 0.3188 (7) | 0.6423 (17) | 0.017 (3) | |
H25A | 0.1294 | 0.3596 | 0.5917 | 0.021* | |
C26 | 0.0477 (16) | 0.2643 (7) | 0.5970 (16) | 0.015 (3) | |
C27 | −0.0788 (16) | 0.2672 (7) | 0.4702 (16) | 0.015 (3) | |
C28 | 0.0747 (16) | 0.2054 (7) | 0.6777 (16) | 0.015 (3) | |
H28A | 0.0109 | 0.1691 | 0.6503 | 0.018* |
U11 | U22 | U33 | U12 | U13 | U23 | |
La1 | 0.0075 (4) | 0.0194 (4) | 0.0072 (4) | 0.0004 (3) | 0.0030 (3) | −0.0004 (3) |
La2 | 0.0075 (4) | 0.0192 (4) | 0.0057 (4) | 0.0007 (3) | 0.0022 (3) | −0.0004 (3) |
N1 | 0.013 (6) | 0.022 (6) | 0.012 (7) | 0.001 (5) | 0.002 (5) | 0.000 (5) |
N2 | 0.010 (6) | 0.024 (6) | 0.008 (6) | 0.002 (5) | 0.003 (5) | −0.003 (5) |
N3 | 0.012 (6) | 0.024 (6) | 0.008 (6) | 0.000 (5) | 0.002 (5) | −0.001 (5) |
N4 | 0.012 (6) | 0.023 (6) | 0.008 (6) | 0.000 (5) | 0.003 (5) | 0.001 (5) |
O1 | 0.013 (5) | 0.024 (5) | 0.008 (5) | 0.001 (4) | 0.003 (4) | 0.001 (4) |
O2 | 0.018 (6) | 0.032 (6) | 0.019 (6) | −0.008 (5) | −0.005 (5) | 0.002 (5) |
O3 | 0.023 (6) | 0.026 (6) | 0.020 (6) | −0.004 (5) | −0.004 (5) | −0.001 (5) |
O4 | 0.022 (6) | 0.032 (6) | 0.018 (6) | −0.003 (5) | −0.005 (5) | 0.003 (4) |
O5 | 0.011 (5) | 0.025 (5) | 0.009 (5) | 0.002 (4) | 0.005 (4) | −0.001 (4) |
O6 | 0.011 (4) | 0.024 (5) | 0.010 (5) | 0.001 (4) | 0.004 (4) | −0.001 (4) |
O7 | 0.012 (5) | 0.037 (6) | 0.011 (6) | 0.004 (5) | −0.003 (4) | −0.009 (5) |
O8 | 0.003 (4) | 0.023 (5) | 0.007 (5) | 0.002 (3) | −0.001 (4) | −0.004 (4) |
O9 | 0.023 (6) | 0.031 (6) | 0.028 (7) | −0.007 (5) | −0.006 (5) | 0.002 (5) |
O10 | 0.014 (5) | 0.023 (5) | 0.010 (5) | 0.001 (4) | 0.001 (4) | 0.001 (4) |
O11 | 0.013 (5) | 0.029 (6) | 0.015 (6) | −0.001 (5) | −0.002 (4) | −0.002 (4) |
O12 | 0.021 (6) | 0.035 (6) | 0.017 (6) | −0.003 (5) | −0.011 (5) | 0.009 (4) |
O13 | 0.016 (5) | 0.023 (5) | 0.010 (5) | −0.002 (4) | 0.008 (4) | 0.000 (4) |
O14 | 0.017 (6) | 0.035 (6) | 0.016 (6) | 0.005 (5) | 0.001 (5) | −0.012 (5) |
O15 | 0.011 (5) | 0.024 (5) | 0.008 (5) | 0.002 (4) | 0.001 (4) | −0.002 (4) |
O16 | 0.011 (5) | 0.027 (5) | 0.012 (5) | 0.000 (4) | 0.002 (4) | 0.001 (4) |
O17 | 0.014 (5) | 0.025 (5) | 0.009 (5) | 0.004 (4) | 0.004 (4) | 0.003 (4) |
O18 | 0.012 (5) | 0.028 (5) | 0.010 (5) | −0.005 (4) | 0.006 (4) | 0.003 (4) |
O19 | 0.014 (5) | 0.028 (6) | 0.012 (6) | 0.003 (4) | 0.000 (4) | 0.002 (5) |
O20 | 0.013 (5) | 0.030 (6) | 0.013 (6) | −0.002 (4) | 0.001 (4) | 0.001 (4) |
O21 | 0.022 (6) | 0.024 (5) | 0.030 (7) | −0.005 (4) | −0.009 (5) | 0.006 (5) |
O22 | 0.034 (8) | 0.045 (7) | 0.036 (8) | 0.000 (6) | −0.003 (6) | −0.002 (6) |
C1 | 0.012 (7) | 0.023 (7) | 0.011 (8) | 0.001 (6) | 0.003 (6) | −0.001 (6) |
C2 | 0.011 (7) | 0.023 (7) | 0.011 (8) | 0.000 (6) | 0.003 (6) | 0.001 (6) |
C3 | 0.014 (8) | 0.024 (7) | 0.014 (8) | 0.000 (6) | 0.002 (6) | 0.001 (6) |
C4 | 0.013 (8) | 0.026 (7) | 0.014 (8) | 0.001 (6) | 0.001 (6) | 0.001 (6) |
C5 | 0.012 (7) | 0.024 (7) | 0.011 (7) | 0.001 (6) | 0.003 (6) | 0.001 (6) |
C6 | 0.014 (8) | 0.025 (7) | 0.012 (8) | 0.003 (6) | 0.003 (6) | 0.001 (6) |
C7 | 0.012 (7) | 0.024 (7) | 0.012 (8) | 0.001 (6) | 0.003 (6) | 0.000 (6) |
C8 | 0.011 (7) | 0.023 (7) | 0.009 (7) | 0.001 (6) | 0.003 (6) | 0.000 (6) |
C9 | 0.008 (7) | 0.024 (7) | 0.008 (7) | 0.000 (6) | 0.002 (6) | 0.000 (6) |
C10 | 0.011 (7) | 0.024 (7) | 0.010 (7) | 0.000 (6) | 0.004 (6) | −0.001 (6) |
C11 | 0.010 (7) | 0.024 (7) | 0.008 (8) | 0.001 (5) | 0.003 (6) | −0.002 (6) |
C12 | 0.012 (7) | 0.023 (7) | 0.008 (7) | −0.001 (6) | 0.000 (6) | −0.005 (6) |
C13 | 0.008 (7) | 0.023 (7) | 0.009 (8) | −0.001 (5) | 0.002 (6) | −0.001 (6) |
C14 | 0.010 (7) | 0.024 (8) | 0.008 (7) | −0.001 (5) | 0.003 (5) | −0.002 (5) |
C15 | 0.011 (7) | 0.022 (7) | 0.010 (8) | −0.001 (5) | 0.002 (6) | 0.000 (6) |
C16 | 0.010 (7) | 0.023 (7) | 0.007 (7) | 0.001 (6) | 0.005 (6) | 0.001 (5) |
C17 | 0.013 (7) | 0.025 (7) | 0.011 (7) | 0.001 (6) | 0.003 (6) | −0.001 (6) |
C18 | 0.011 (7) | 0.024 (7) | 0.008 (7) | −0.001 (6) | 0.004 (6) | −0.001 (6) |
C19 | 0.012 (7) | 0.023 (7) | 0.008 (7) | −0.001 (6) | 0.004 (6) | 0.000 (6) |
C20 | 0.010 (7) | 0.022 (6) | 0.008 (7) | −0.001 (6) | 0.002 (6) | 0.003 (6) |
C21 | 0.011 (7) | 0.024 (8) | 0.009 (7) | 0.001 (5) | 0.004 (5) | −0.001 (5) |
C22 | 0.013 (7) | 0.024 (7) | 0.013 (8) | 0.001 (6) | 0.002 (6) | −0.002 (6) |
C23 | 0.012 (7) | 0.024 (7) | 0.012 (8) | 0.001 (6) | 0.003 (6) | −0.001 (6) |
C24 | 0.015 (8) | 0.025 (7) | 0.013 (8) | −0.002 (6) | −0.001 (6) | 0.000 (6) |
C25 | 0.015 (7) | 0.023 (7) | 0.012 (8) | −0.001 (6) | 0.000 (6) | 0.002 (6) |
C26 | 0.011 (7) | 0.024 (7) | 0.010 (7) | 0.000 (5) | 0.003 (6) | −0.001 (6) |
C27 | 0.012 (7) | 0.024 (7) | 0.010 (7) | 0.000 (6) | 0.003 (6) | 0.000 (5) |
C28 | 0.012 (7) | 0.024 (7) | 0.010 (8) | 0.000 (6) | 0.003 (6) | −0.001 (6) |
La1—O1 | 2.520 (10) | O16—La2iv | 2.551 (10) |
La1—O5 | 2.531 (10) | O17—H17A | 0.8500 |
La1—O8i | 2.658 (9) | O17—H17C | 0.8500 |
La1—O13ii | 2.584 (10) | O18—H18A | 0.8500 |
La1—O15i | 2.531 (9) | O18—H18C | 0.8500 |
La1—O19 | 2.570 (11) | O19—H19A | 0.8500 |
La1—O20 | 2.543 (10) | O19—H19B | 0.8501 |
La1—N1 | 2.778 (13) | O20—H20A | 0.8500 |
La1—N2i | 2.703 (12) | O20—H20B | 0.8500 |
La2—O6 | 2.522 (9) | O21—H21B | 0.8500 |
La2—O8iii | 2.599 (9) | O21—H21C | 0.8500 |
La2—O10 | 2.498 (10) | O22—H22A | 0.8500 |
La2—O13 | 2.626 (10) | O22—H22B | 0.8500 |
La2—O16i | 2.551 (10) | C1—C2 | 1.51 (2) |
La2—O17 | 2.613 (10) | C2—C3 | 1.38 (2) |
La2—O18 | 2.505 (10) | C3—C4 | 1.42 (2) |
La2—N3 | 2.681 (12) | C3—H3A | 0.9300 |
La2—N4 | 2.786 (12) | C4—C5 | 1.37 (2) |
N1—C2 | 1.351 (19) | C4—H4A | 0.9300 |
N1—C7 | 1.357 (19) | C5—C7 | 1.41 (2) |
N2—C14 | 1.335 (18) | C5—C6 | 1.51 (2) |
N2—C12 | 1.403 (19) | C7—H7A | 0.9300 |
N2—La1iv | 2.703 (12) | C8—C9 | 1.49 (2) |
N3—C16 | 1.300 (19) | C9—C10 | 1.40 (2) |
N3—C21 | 1.361 (18) | C9—C14 | 1.42 (2) |
N4—C28 | 1.337 (19) | C10—C11 | 1.38 (2) |
N4—C23 | 1.344 (19) | C10—H10A | 0.9300 |
O1—C1 | 1.282 (17) | C11—C12 | 1.35 (2) |
O2—C1 | 1.246 (18) | C11—H11A | 0.9300 |
O3—C6 | 1.201 (18) | C12—C13 | 1.488 (19) |
O4—C6 | 1.296 (18) | C14—H14 | 0.9300 |
O4—H4B | 0.8200 | C15—C16 | 1.545 (19) |
O5—C8 | 1.279 (17) | C16—C17 | 1.40 (2) |
O6—C8 | 1.270 (17) | C17—C18 | 1.39 (2) |
O7—C13 | 1.211 (18) | C17—H17B | 0.9300 |
O8—C13 | 1.290 (17) | C18—C19 | 1.39 (2) |
O8—La2v | 2.599 (9) | C18—H18B | 0.9300 |
O8—La1iv | 2.658 (9) | C19—C21 | 1.37 (2) |
O9—C22 | 1.237 (18) | C19—C20 | 1.494 (19) |
O10—C22 | 1.276 (18) | C21—H21A | 0.9300 |
O11—C27 | 1.216 (18) | C22—C23 | 1.512 (19) |
O12—C27 | 1.323 (18) | C23—C24 | 1.38 (2) |
O12—H12A | 0.8200 | C24—C25 | 1.37 (2) |
O13—C15 | 1.291 (17) | C24—H24A | 0.9300 |
O13—La1vi | 2.584 (10) | C25—C26 | 1.40 (2) |
O14—C15 | 1.237 (18) | C25—H25A | 0.9300 |
O15—C20 | 1.317 (18) | C26—C28 | 1.38 (2) |
O15—La1iv | 2.531 (9) | C26—C27 | 1.486 (19) |
O16—C20 | 1.232 (18) | C28—H28A | 0.9300 |
O1—La1—O5 | 71.0 (3) | C15—O13—La2 | 118.8 (9) |
O1—La1—O15i | 129.4 (3) | La1vi—O13—La2 | 112.8 (4) |
O5—La1—O15i | 87.8 (3) | C20—O15—La1iv | 138.1 (8) |
O1—La1—O20 | 136.7 (3) | C20—O16—La2iv | 149.6 (10) |
O5—La1—O20 | 139.9 (3) | La2—O17—H17A | 96.8 |
O15i—La1—O20 | 88.4 (3) | La2—O17—H17C | 92.3 |
O1—La1—O19 | 137.8 (3) | H17A—O17—H17C | 106.2 |
O5—La1—O19 | 72.1 (3) | La2—O18—H18A | 118.8 |
O15i—La1—O19 | 68.2 (3) | La2—O18—H18C | 130.6 |
O20—La1—O19 | 69.4 (4) | H18A—O18—H18C | 108.8 |
O1—La1—O13ii | 79.9 (3) | La1—O19—H19A | 96.2 |
O5—La1—O13ii | 84.7 (3) | La1—O19—H19B | 95.5 |
O15i—La1—O13ii | 145.0 (3) | H19A—O19—H19B | 108.9 |
O20—La1—O13ii | 76.0 (3) | La1—O20—H20A | 97.6 |
O19—La1—O13ii | 76.9 (3) | La1—O20—H20B | 98.1 |
O1—La1—O8i | 66.8 (3) | H20A—O20—H20B | 108.5 |
O5—La1—O8i | 132.7 (3) | H21B—O21—H21C | 108.2 |
O15i—La1—O8i | 136.2 (3) | H22A—O22—H22B | 108.5 |
O20—La1—O8i | 70.9 (3) | O2—C1—O1 | 125.4 (13) |
O19—La1—O8i | 131.8 (3) | O2—C1—C2 | 118.4 (13) |
O13ii—La1—O8i | 67.8 (3) | O1—C1—C2 | 116.2 (12) |
O1—La1—N2i | 94.8 (3) | N1—C2—C3 | 123.9 (13) |
O5—La1—N2i | 144.3 (3) | N1—C2—C1 | 115.4 (12) |
O15i—La1—N2i | 76.1 (3) | C3—C2—C1 | 120.7 (13) |
O20—La1—N2i | 72.3 (3) | C2—C3—C4 | 118.9 (13) |
O19—La1—N2i | 127.4 (3) | C2—C3—H3A | 120.5 |
O13ii—La1—N2i | 126.0 (3) | C4—C3—H3A | 120.5 |
O8i—La1—N2i | 61.0 (3) | C5—C4—C3 | 117.2 (14) |
O1—La1—N1 | 60.4 (4) | C5—C4—H4A | 121.4 |
O5—La1—N1 | 73.0 (3) | C3—C4—H4A | 121.4 |
O15i—La1—N1 | 69.6 (3) | C4—C5—C7 | 121.1 (14) |
O20—La1—N1 | 141.2 (3) | C4—C5—C6 | 122.4 (13) |
O19—La1—N1 | 125.3 (4) | C7—C5—C6 | 116.5 (13) |
O13ii—La1—N1 | 138.8 (3) | O3—C6—O4 | 125.5 (14) |
O8i—La1—N1 | 102.8 (3) | O3—C6—C5 | 121.6 (13) |
N2i—La1—N1 | 71.6 (4) | O4—C6—C5 | 112.8 (12) |
O10—La2—O18 | 137.5 (3) | N1—C7—C5 | 121.4 (14) |
O10—La2—O6 | 129.9 (3) | N1—C7—H7A | 119.3 |
O18—La2—O6 | 88.1 (3) | C5—C7—H7A | 119.3 |
O10—La2—O16i | 72.5 (3) | O6—C8—O5 | 125.1 (13) |
O18—La2—O16i | 136.8 (3) | O6—C8—C9 | 118.3 (12) |
O6—La2—O16i | 86.9 (3) | O5—C8—C9 | 116.5 (13) |
O10—La2—O16i | 72.5 (3) | C10—C9—C14 | 116.1 (13) |
O18—La2—O16i | 136.8 (3) | C10—C9—C8 | 122.1 (13) |
O6—La2—O16i | 86.9 (3) | C14—C9—C8 | 121.8 (13) |
O16i—La2—O16i | 0.0 (4) | C11—C10—C9 | 120.4 (14) |
O10—La2—O8iii | 78.5 (3) | C11—C10—H10A | 119.8 |
O18—La2—O8iii | 77.1 (3) | C9—C10—H10A | 119.8 |
O6—La2—O8iii | 144.6 (3) | C12—C11—C10 | 121.0 (14) |
O16i—La2—O8iii | 82.6 (3) | C12—C11—H11A | 119.5 |
O16i—La2—O8iii | 82.6 (3) | C10—C11—H11A | 119.5 |
O10—La2—O17 | 136.8 (3) | C11—C12—N2 | 120.9 (13) |
O18—La2—O17 | 68.5 (4) | C11—C12—C13 | 122.8 (14) |
O6—La2—O17 | 68.2 (3) | N2—C12—C13 | 116.1 (12) |
O16i—La2—O17 | 69.8 (3) | O7—C13—O8 | 125.8 (13) |
O16i—La2—O17 | 69.8 (3) | O7—C13—C12 | 115.9 (13) |
O8iii—La2—O17 | 76.4 (3) | O8—C13—C12 | 118.2 (12) |
O10—La2—O13 | 65.6 (3) | N2—C14—C9 | 123.3 (13) |
O18—La2—O13 | 73.1 (3) | N2—C14—H14 | 118.4 |
O6—La2—O13 | 137.9 (3) | C9—C14—H14 | 118.4 |
O16i—La2—O13 | 132.3 (3) | O14—C15—O13 | 125.5 (13) |
O16i—La2—O13 | 132.3 (3) | O14—C15—C16 | 118.2 (13) |
O8iii—La2—O13 | 68.1 (3) | O13—C15—C16 | 116.2 (12) |
O17—La2—O13 | 132.3 (3) | N3—C16—C17 | 125.0 (14) |
O10—La2—N3 | 94.9 (3) | N3—C16—C15 | 118.1 (13) |
O18—La2—N3 | 73.6 (3) | C17—C16—C15 | 116.9 (13) |
O6—La2—N3 | 76.7 (3) | C18—C17—C16 | 116.6 (14) |
O16i—La2—N3 | 145.4 (3) | C18—C17—H17B | 121.7 |
O16i—La2—N3 | 145.4 (3) | C16—C17—H17B | 121.7 |
O8iii—La2—N3 | 127.4 (3) | C17—C18—C19 | 119.0 (14) |
O17—La2—N3 | 128.3 (3) | C17—C18—H18B | 120.5 |
O13—La2—N3 | 62.0 (3) | C19—C18—H18B | 120.5 |
O10—La2—N4 | 60.8 (4) | C21—C19—C18 | 119.6 (14) |
O18—La2—N4 | 141.8 (3) | C21—C19—C20 | 122.0 (13) |
O6—La2—N4 | 69.9 (3) | C18—C19—C20 | 118.2 (13) |
O16i—La2—N4 | 74.7 (3) | O16—C20—O15 | 120.4 (13) |
O16i—La2—N4 | 74.7 (3) | O16—C20—C19 | 122.9 (13) |
O8iii—La2—N4 | 137.6 (3) | O15—C20—C19 | 116.7 (12) |
O17—La2—N4 | 125.5 (4) | N3—C21—C19 | 121.9 (13) |
O13—La2—N4 | 102.2 (3) | N3—C21—H21A | 119.0 |
N3—La2—N4 | 71.2 (4) | C19—C21—H21A | 119.0 |
C2—N1—C7 | 117.4 (13) | O9—C22—O10 | 124.5 (14) |
C2—N1—La1 | 116.2 (9) | O9—C22—C23 | 117.9 (13) |
C7—N1—La1 | 126.4 (10) | O10—C22—C23 | 117.5 (12) |
C14—N2—C12 | 118.3 (12) | N4—C23—C24 | 124.0 (14) |
C14—N2—La1iv | 124.0 (9) | N4—C23—C22 | 115.7 (13) |
C12—N2—La1iv | 116.8 (8) | C24—C23—C22 | 120.4 (13) |
C16—N3—C21 | 117.7 (12) | C25—C24—C23 | 118.1 (14) |
C16—N3—La2 | 117.2 (9) | C25—C24—H24A | 120.9 |
C21—N3—La2 | 124.7 (9) | C23—C24—H24A | 120.9 |
C28—N4—C23 | 116.4 (13) | C24—C25—C26 | 120.2 (14) |
C28—N4—La2 | 128.1 (10) | C24—C25—H25A | 119.9 |
C23—N4—La2 | 114.9 (9) | C26—C25—H25A | 119.9 |
C1—O1—La1 | 125.0 (9) | C28—C26—C25 | 116.7 (13) |
C6—O4—H4B | 109.5 | C28—C26—C27 | 119.5 (13) |
C8—O5—La1 | 145.6 (9) | C25—C26—C27 | 123.7 (13) |
C8—O6—La2 | 138.2 (8) | O11—C27—O12 | 125.6 (13) |
C13—O8—La2v | 128.2 (8) | O11—C27—C26 | 122.0 (13) |
C13—O8—La1iv | 119.9 (8) | O12—C27—C26 | 112.4 (12) |
La2v—O8—La1iv | 111.2 (3) | N4—C28—C26 | 124.6 (14) |
C22—O10—La2 | 126.1 (9) | N4—C28—H28A | 117.7 |
C27—O12—H12A | 109.5 | C26—C28—H28A | 117.7 |
C15—O13—La1vi | 128.2 (9) | ||
O1—La1—N1—C2 | −12.5 (9) | La1—O1—C1—O2 | 146.7 (12) |
O5—La1—N1—C2 | 64.9 (10) | La1—O1—C1—C2 | −31.7 (17) |
O15i—La1—N1—C2 | 159.0 (11) | C7—N1—C2—C3 | 0 (2) |
O20—La1—N1—C2 | −141.6 (10) | La1—N1—C2—C3 | −177.3 (12) |
O19—La1—N1—C2 | 117.4 (10) | C7—N1—C2—C1 | −178.7 (13) |
O13ii—La1—N1—C2 | 4.7 (13) | La1—N1—C2—C1 | 4.0 (16) |
O8i—La1—N1—C2 | −66.2 (11) | O2—C1—C2—N1 | −162.9 (14) |
N2i—La1—N1—C2 | −119.4 (11) | O1—C1—C2—N1 | 15.6 (19) |
O1—La1—N1—C7 | 170.5 (13) | O2—C1—C2—C3 | 18 (2) |
O5—La1—N1—C7 | −112.0 (12) | O1—C1—C2—C3 | −163.1 (14) |
O15i—La1—N1—C7 | −18.0 (11) | N1—C2—C3—C4 | −2 (2) |
O20—La1—N1—C7 | 41.5 (14) | C1—C2—C3—C4 | 176.8 (13) |
O19—La1—N1—C7 | −59.6 (13) | C2—C3—C4—C5 | 1 (2) |
O13ii—La1—N1—C7 | −172.3 (10) | C3—C4—C5—C7 | 1 (2) |
O8i—La1—N1—C7 | 116.9 (12) | C3—C4—C5—C6 | 179.6 (13) |
N2i—La1—N1—C7 | 63.6 (11) | C4—C5—C6—O3 | 170.4 (15) |
O10—La2—N3—C16 | −39.9 (11) | C7—C5—C6—O3 | −11 (2) |
O18—La2—N3—C16 | 98.3 (11) | C4—C5—C6—O4 | −8 (2) |
O6—La2—N3—C16 | −169.8 (11) | C7—C5—C6—O4 | 170.9 (14) |
O16i—La2—N3—C16 | −105.9 (11) | C2—N1—C7—C5 | 2 (2) |
O16i—La2—N3—C16 | −105.9 (11) | La1—N1—C7—C5 | 179.4 (11) |
O8iii—La2—N3—C16 | 39.4 (12) | C4—C5—C7—N1 | −3 (2) |
O17—La2—N3—C16 | 142.4 (10) | C6—C5—C7—N1 | 178.4 (13) |
O13—La2—N3—C16 | 19.0 (10) | La2—O6—C8—O5 | 0 (2) |
N4—La2—N3—C16 | −96.7 (11) | La2—O6—C8—C9 | 175.4 (9) |
O10—La2—N3—C21 | 132.3 (10) | La1—O5—C8—O6 | −104.4 (18) |
O18—La2—N3—C21 | −89.5 (10) | La1—O5—C8—C9 | 79.9 (19) |
O6—La2—N3—C21 | 2.4 (10) | O6—C8—C9—C10 | −169.6 (13) |
O16i—La2—N3—C21 | 66.3 (12) | O5—C8—C9—C10 | 6 (2) |
O16i—La2—N3—C21 | 66.3 (12) | O6—C8—C9—C14 | 12 (2) |
O8iii—La2—N3—C21 | −148.4 (9) | O5—C8—C9—C14 | −172.0 (13) |
O17—La2—N3—C21 | −45.4 (12) | C14—C9—C10—C11 | 2 (2) |
O13—La2—N3—C21 | −168.8 (11) | C8—C9—C10—C11 | −176.3 (13) |
N4—La2—N3—C21 | 75.5 (10) | C9—C10—C11—C12 | 0 (2) |
O10—La2—N4—C28 | −172.5 (13) | C10—C11—C12—N2 | −2 (2) |
O18—La2—N4—C28 | −41.6 (15) | C10—C11—C12—C13 | 172.9 (14) |
O6—La2—N4—C28 | 16.9 (11) | C14—N2—C12—C11 | 1 (2) |
O16i—La2—N4—C28 | 109.2 (12) | La1iv—N2—C12—C11 | −169.3 (11) |
O16i—La2—N4—C28 | 109.2 (12) | C14—N2—C12—C13 | −174.5 (12) |
O8iii—La2—N4—C28 | 169.3 (10) | La1iv—N2—C12—C13 | 15.7 (15) |
O17—La2—N4—C28 | 58.7 (13) | La2v—O8—C13—O7 | −16 (2) |
O13—La2—N4—C28 | −119.8 (12) | La1iv—O8—C13—O7 | 153.7 (12) |
N3—La2—N4—C28 | −65.4 (12) | La2v—O8—C13—C12 | 162.2 (9) |
O10—La2—N4—C23 | 16.5 (10) | La1iv—O8—C13—C12 | −27.8 (16) |
O18—La2—N4—C23 | 147.4 (9) | C11—C12—C13—O7 | 11 (2) |
O6—La2—N4—C23 | −154.0 (11) | N2—C12—C13—O7 | −174.1 (13) |
O16i—La2—N4—C23 | −61.7 (10) | C11—C12—C13—O8 | −167.7 (14) |
O16i—La2—N4—C23 | −61.7 (10) | N2—C12—C13—O8 | 7.3 (19) |
O8iii—La2—N4—C23 | −1.6 (13) | C12—N2—C14—C9 | 2 (2) |
O17—La2—N4—C23 | −112.3 (10) | La1iv—N2—C14—C9 | 171.2 (10) |
O13—La2—N4—C23 | 69.2 (11) | C10—C9—C14—N2 | −4 (2) |
N3—La2—N4—C23 | 123.7 (11) | C8—C9—C14—N2 | 175.0 (13) |
O5—La1—O1—C1 | −56.9 (11) | La1vi—O13—C15—O14 | 17 (2) |
O15i—La1—O1—C1 | 13.5 (12) | La2—O13—C15—O14 | −155.8 (12) |
O20—La1—O1—C1 | 158.6 (10) | La1vi—O13—C15—C16 | −158.9 (9) |
O19—La1—O1—C1 | −87.4 (11) | La2—O13—C15—C16 | 28.0 (15) |
O13ii—La1—O1—C1 | −144.7 (11) | C21—N3—C16—C17 | −5 (2) |
O8i—La1—O1—C1 | 145.2 (11) | La2—N3—C16—C17 | 167.4 (12) |
N2i—La1—O1—C1 | 89.5 (11) | C21—N3—C16—C15 | 173.2 (12) |
N1—La1—O1—C1 | 23.8 (10) | La2—N3—C16—C15 | −14.0 (16) |
O1—La1—O5—C8 | −120.5 (16) | O14—C15—C16—N3 | 174.7 (14) |
O15i—La1—O5—C8 | 106.3 (16) | O13—C15—C16—N3 | −8.8 (19) |
O20—La1—O5—C8 | 21.3 (18) | O14—C15—C16—C17 | −7 (2) |
O19—La1—O5—C8 | 38.4 (16) | O13—C15—C16—C17 | 169.9 (13) |
O13ii—La1—O5—C8 | −39.5 (16) | N3—C16—C17—C18 | 4 (2) |
O8i—La1—O5—C8 | −92.5 (16) | C15—C16—C17—C18 | −174.7 (13) |
N2i—La1—O5—C8 | 168.6 (15) | C16—C17—C18—C19 | −1 (2) |
N1—La1—O5—C8 | 175.6 (17) | C17—C18—C19—C21 | 1 (2) |
O10—La2—O6—C8 | 95.6 (14) | C17—C18—C19—C20 | 176.4 (13) |
O18—La2—O6—C8 | −105.5 (13) | La2iv—O16—C20—O15 | 110.5 (19) |
O16i—La2—O6—C8 | 31.6 (13) | La2iv—O16—C20—C19 | −67 (2) |
O16i—La2—O6—C8 | 31.6 (13) | La1iv—O15—C20—O16 | 8 (2) |
O8iii—La2—O6—C8 | −41.0 (16) | La1iv—O15—C20—C19 | −174.1 (9) |
O17—La2—O6—C8 | −37.9 (13) | C21—C19—C20—O16 | 163.5 (14) |
O13—La2—O6—C8 | −167.5 (12) | C18—C19—C20—O16 | −12 (2) |
N3—La2—O6—C8 | −179.1 (14) | C21—C19—C20—O15 | −15 (2) |
N4—La2—O6—C8 | 106.4 (14) | C18—C19—C20—O15 | 170.0 (13) |
O18—La2—O10—C22 | −156.8 (11) | C16—N3—C21—C19 | 4 (2) |
O6—La2—O10—C22 | −9.0 (13) | La2—N3—C21—C19 | −167.7 (10) |
O16i—La2—O10—C22 | 61.3 (11) | C18—C19—C21—N3 | −2 (2) |
O16i—La2—O10—C22 | 61.3 (11) | C20—C19—C21—N3 | −177.7 (12) |
O8iii—La2—O10—C22 | 147.1 (12) | La2—O10—C22—O9 | −158.6 (12) |
O17—La2—O10—C22 | 91.6 (12) | La2—O10—C22—C23 | 22.0 (18) |
O13—La2—O10—C22 | −141.9 (12) | C28—N4—C23—C24 | −4 (2) |
N3—La2—O10—C22 | −85.8 (12) | La2—N4—C23—C24 | 168.3 (12) |
N4—La2—O10—C22 | −20.6 (11) | C28—N4—C23—C22 | 174.1 (12) |
O10—La2—O13—C15 | 85.7 (10) | La2—N4—C23—C22 | −13.8 (16) |
O18—La2—O13—C15 | −104.7 (9) | O9—C22—C23—N4 | 178.0 (14) |
O6—La2—O13—C15 | −37.5 (11) | O10—C22—C23—N4 | −3 (2) |
O16i—La2—O13—C15 | 116.3 (9) | O9—C22—C23—C24 | −4 (2) |
O16i—La2—O13—C15 | 116.3 (9) | O10—C22—C23—C24 | 175.3 (14) |
O8iii—La2—O13—C15 | 172.6 (10) | N4—C23—C24—C25 | 3 (2) |
O17—La2—O13—C15 | −142.4 (9) | C22—C23—C24—C25 | −175.0 (14) |
N3—La2—O13—C15 | −24.7 (9) | C23—C24—C25—C26 | −1 (2) |
N4—La2—O13—C15 | 36.0 (10) | C24—C25—C26—C28 | 0 (2) |
O10—La2—O13—La1vi | −88.4 (4) | C24—C25—C26—C27 | 179.6 (14) |
O18—La2—O13—La1vi | 81.1 (4) | C28—C26—C27—O11 | 10 (2) |
O6—La2—O13—La1vi | 148.4 (4) | C25—C26—C27—O11 | −169.3 (15) |
O16i—La2—O13—La1vi | −57.8 (5) | C28—C26—C27—O12 | −169.6 (13) |
O16i—La2—O13—La1vi | −57.8 (5) | C25—C26—C27—O12 | 11 (2) |
O8iii—La2—O13—La1vi | −1.5 (4) | C23—N4—C28—C26 | 3 (2) |
O17—La2—O13—La1vi | 43.5 (6) | La2—N4—C28—C26 | −167.7 (11) |
N3—La2—O13—La1vi | 161.2 (5) | C25—C26—C28—N4 | −1 (2) |
N4—La2—O13—La1vi | −138.1 (4) | C27—C26—C28—N4 | 179.2 (13) |
Symmetry codes: (i) x+1, y, z; (ii) x, y, z−1; (iii) x+1, y, z+1; (iv) x−1, y, z; (v) x−1, y, z−1; (vi) x, y, z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O22—H22B···O21vii | 0.85 | 2.03 | 2.88 (2) | 176 |
O22—H22A···O2viii | 0.85 | 1.85 | 2.702 (17) | 177 |
O21—H21C···O17ix | 0.85 | 1.99 | 2.833 (15) | 171 |
O21—H21B···O9ii | 0.85 | 1.77 | 2.612 (15) | 171 |
O20—H20B···O11i | 0.85 | 2.09 | 2.759 (14) | 136 |
O20—H20A···O8i | 0.85 | 2.47 | 3.020 (14) | 123 |
O20—H20A···O10ii | 0.85 | 2.06 | 2.687 (14) | 130 |
O19—H19B···O16i | 0.85 | 1.98 | 2.787 (15) | 158 |
O19—H19A···O14ii | 0.85 | 1.80 | 2.605 (15) | 157 |
O18—H18C···O3iv | 0.85 | 1.91 | 2.728 (15) | 162 |
O18—H18A···O1vi | 0.85 | 1.89 | 2.706 (14) | 161 |
O17—H17C···O16i | 0.85 | 2.49 | 2.955 (14) | 115 |
O17—H17C···O5 | 0.85 | 2.12 | 2.791 (14) | 135 |
O17—H17A···O7iii | 0.85 | 1.76 | 2.608 (14) | 174 |
O12—H12A···O21iv | 0.82 | 1.76 | 2.564 (15) | 166 |
O4—H4B···O22x | 0.82 | 1.82 | 2.534 (14) | 145 |
Symmetry codes: (i) x+1, y, z; (ii) x, y, z−1; (iii) x+1, y, z+1; (iv) x−1, y, z; (vi) x, y, z+1; (vii) −x+1, y+1/2, −z; (viii) x, y+1, z; (ix) −x+1, y+1/2, −z+1; (x) x+1, y−1, z+1. |
Experimental details
Crystal data | |
Chemical formula | [La2(C7H4NO4)2(C7H3NO4)2(H2O)4]·2H2O |
Mr | 1048.35 |
Crystal system, space group | Monoclinic, P21 |
Temperature (K) | 293 |
a, b, c (Å) | 9.2203 (18), 19.744 (4), 9.3552 (19) |
β (°) | 101.72 (3) |
V (Å3) | 1667.5 (6) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 2.63 |
Crystal size (mm) | 0.35 × 0.34 × 0.27 |
Data collection | |
Diffractometer | Bruker SMART CCD area-detector |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.428, 0.490 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 12319, 5778, 5491 |
Rint | 0.093 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.064, 0.174, 1.06 |
No. of reflections | 5778 |
No. of parameters | 505 |
No. of restraints | 1 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.82, −3.93 |
Absolute structure | Flack (1983), 2752 Friedel pairs |
Absolute structure parameter | 0.50 (4) |
Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 1997), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1997), SHELXTL.
La1—O1 | 2.520 (10) | La2—O6 | 2.522 (9) |
La1—O5 | 2.531 (10) | La2—O8iii | 2.599 (9) |
La1—O8i | 2.658 (9) | La2—O10 | 2.498 (10) |
La1—O13ii | 2.584 (10) | La2—O13 | 2.626 (10) |
La1—O15i | 2.531 (9) | La2—O16i | 2.551 (10) |
La1—O19 | 2.570 (11) | La2—O17 | 2.613 (10) |
La1—O20 | 2.543 (10) | La2—O18 | 2.505 (10) |
La1—N1 | 2.778 (13) | La2—N3 | 2.681 (12) |
La1—N2i | 2.703 (12) | La2—N4 | 2.786 (12) |
Symmetry codes: (i) x+1, y, z; (ii) x, y, z−1; (iii) x+1, y, z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O22—H22B···O21iv | 0.85 | 2.03 | 2.88 (2) | 176 |
O22—H22A···O2v | 0.85 | 1.85 | 2.702 (17) | 177 |
O21—H21C···O17vi | 0.85 | 1.99 | 2.833 (15) | 171 |
O21—H21B···O9ii | 0.85 | 1.77 | 2.612 (15) | 171 |
O20—H20B···O11i | 0.85 | 2.09 | 2.759 (14) | 136 |
O20—H20A···O8i | 0.85 | 2.47 | 3.020 (14) | 123 |
O20—H20A···O10ii | 0.85 | 2.06 | 2.687 (14) | 130 |
O19—H19B···O16i | 0.85 | 1.98 | 2.787 (15) | 158 |
O19—H19A···O14ii | 0.85 | 1.80 | 2.605 (15) | 157 |
O18—H18C···O3vii | 0.85 | 1.91 | 2.728 (15) | 162 |
O18—H18A···O1viii | 0.85 | 1.89 | 2.706 (14) | 161 |
O17—H17C···O16i | 0.85 | 2.49 | 2.955 (14) | 115 |
O17—H17C···O5 | 0.85 | 2.12 | 2.791 (14) | 135 |
O17—H17A···O7iii | 0.85 | 1.76 | 2.608 (14) | 174 |
O12—H12A···O21vii | 0.82 | 1.76 | 2.564 (15) | 166 |
O4—H4B···O22ix | 0.82 | 1.82 | 2.534 (14) | 145 |
Symmetry codes: (i) x+1, y, z; (ii) x, y, z−1; (iii) x+1, y, z+1; (iv) −x+1, y+1/2, −z; (v) x, y+1, z; (vi) −x+1, y+1/2, −z+1; (vii) x−1, y, z; (viii) x, y, z+1; (ix) x+1, y−1, z+1. |
In recent years, studies on the syntheses, structures and properties of coordination complexes containing lanthanum and aromatic carboxylate have intensely attracted much attention, because they possess potential application on catalysis, separation, gas deposition and luminescence (Chae et al., 2004; Seo et al., 2000; Bradshaw et al., 2004; Lu et al., 2006). As a multi-functional ligand, pyridine-2,5-dicarboxylic acid has been widely used in the preparation of 3 d-4f heterometallic coordination polymers (Liang et al., 2000; Liang et al., 2001) and transition metallic supra-molecular compounds (Min et al., 2001; Xu et al., 2001; Gao et al., 2005). However the investigation on the lanthanum complexes is relative limited (Song et al., 2005). We report here the crystal structure of the title LaIII polymeric compound.
A segment of the polymeric structure of the title compound is illustrated in Fig. 1. Each LaIII ion is nine-coordinated by two nitrogen atoms from Hpydc and pydc ligands, five oxygen atoms from carboxylate groups of one Hpydc and four pydc ligands and two water molecules. The pydc2- anion acts as chelating-bridging pentadentate ligand towards four LaIII ions. The pyridine nitrogen atom and the ortho-carboxylic oxygen atom chelate one La ion, and this oxygen atom and other two carboxylic oxygen atoms of the pydc ligand bridge another three different La ions. The Hpydc- anion acts as chelating bidentate ligand towards the La ion with a pyridine nitrogen atom and the ortho carboxylic oxygen atom, which is similar to the coordination mode of Hpydc in [Dy(Hpydc)(pydc)(phen)(H2O).H2O]n [phen=1,10-phenanthroline] (Song et al., 2005) and [Ln(Hpydc)(pydc)] [Ln = Sm, Eu, Gd] (Qin et al., 2005). The La···La separations in the same unit and between adjacent units are 4.339 (9) and 5.619 (9) Å, respectively. The La center is in a slightly distorted tricapped trigonal prism coordination geometry. Adjacent La ions are linked together through single-atom carboxylate oxygen atom and carboxylate group in the syn-anti mode, forming a two-dimensional polymeric layer structure as represented in Fig. 2. Selected geometric parameters are listed in Table 1. The La—O bond lengths fall in range from 2.498 (10) to 2.658 (9) Å.
Extensive N—H···O and O—H···O hydrogen bonding occur in the crystal structure of the title compound, and connect adjacent layers into the infinite three-dimensional supramolecular network structure (Table 2 and Fig. 3).