Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807053123/bt2565sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807053123/bt2565Isup2.hkl |
CCDC reference: 672574
A mixture of LaCl3.6H2O (2.00 mmol, 0.70 g), benzene-1,4-dicarboxylic acid (1.0 mmol, 0.16 g), succinic acid (1.0 mmol, 0.10 g), NaOH (6.0 ml, 1 mol/L) and H2O (20.0 ml) was heated in a 35 ml stainless steel reactor with a Teflon liner at 453 K for 48 h. The column-like crystals were filtered and washed with ethanol. Yield: 14% based on Nd.
H atoms were included at calculated positions and treated as riding atoms, with C—H distances of 0.93–0.97 Å and Uiso(H) = 1.2Ueq(C)].
Data collection: SMART (Bruker, 1998); cell refinement: SMART (Bruker, 1998); data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL (Bruker, 1998).
[La2(C4H4O4)(C8H4O4)2] | F(000) = 1368 |
Mr = 361.06 | Dx = 2.166 Mg m−3 |
Orthorhombic, Pbca | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2ab | Cell parameters from 168 reflections |
a = 14.2014 (4) Å | θ = 3.3–26.7° |
b = 7.0513 (1) Å | µ = 3.87 mm−1 |
c = 22.1100 (5) Å | T = 291 K |
V = 2214.06 (9) Å3 | Column, colorless |
Z = 8 | 0.33 × 0.27 × 0.18 mm |
Bruker SMART CCD area-detector diffractometer | 2505 independent reflections |
Radiation source: fine-focus sealed tube | 1974 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.029 |
ϕ and ω scans | θmax = 27.5°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −18→18 |
Tmin = 0.293, Tmax = 0.492 | k = −9→5 |
11927 measured reflections | l = −28→29 |
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)] = 0.021 | H-atom parameters constrained |
wR(F2) = 0.051 | w = 1/[σ2(Fo2) + (0.0243P)2 + 1.3924P] where P = (Fo2 + 2Fc2)/3 |
S = 1.02 | (Δ/σ)max = 0.030 |
2505 reflections | Δρmax = 0.31 e Å−3 |
155 parameters | Δρmin = −0.53 e Å−3 |
0 restraints | Extinction correction: SHELXTL (Bruker, 1998), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00116 (9) |
[La2(C4H4O4)(C8H4O4)2] | V = 2214.06 (9) Å3 |
Mr = 361.06 | Z = 8 |
Orthorhombic, Pbca | Mo Kα radiation |
a = 14.2014 (4) Å | µ = 3.87 mm−1 |
b = 7.0513 (1) Å | T = 291 K |
c = 22.1100 (5) Å | 0.33 × 0.27 × 0.18 mm |
Bruker SMART CCD area-detector diffractometer | 2505 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 1974 reflections with I > 2σ(I) |
Tmin = 0.293, Tmax = 0.492 | Rint = 0.029 |
11927 measured reflections |
R[F2 > 2σ(F2)] = 0.021 | 0 restraints |
wR(F2) = 0.051 | H-atom parameters constrained |
S = 1.02 | Δρmax = 0.31 e Å−3 |
2505 reflections | Δρmin = −0.53 e Å−3 |
155 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 | ||
La | 0.833810 (10) | 1.02208 (2) | 0.554317 (6) | 0.01592 (7) | |
O1 | 0.86146 (16) | 1.0440 (3) | 0.44571 (8) | 0.0277 (5) | |
O2 | 1.00219 (14) | 0.9173 (3) | 0.43107 (8) | 0.0279 (5) | |
C1 | 0.92144 (19) | 0.9655 (4) | 0.41250 (12) | 0.0198 (6) | |
C2 | 0.89650 (19) | 0.9240 (4) | 0.34781 (12) | 0.0225 (6) | |
C3 | 0.8095 (2) | 0.9761 (5) | 0.32544 (14) | 0.0326 (8) | |
H3A | 0.7667 | 1.0383 | 0.3503 | 0.039* | |
C4 | 0.7857 (2) | 0.9356 (5) | 0.26579 (14) | 0.0359 (8) | |
H4A | 0.7269 | 0.9697 | 0.2509 | 0.043* | |
C5 | 0.8497 (2) | 0.8446 (5) | 0.22869 (13) | 0.0289 (7) | |
C6 | 0.8238 (2) | 0.7940 (5) | 0.16472 (14) | 0.0341 (8) | |
C7 | 0.9370 (2) | 0.7938 (5) | 0.25116 (13) | 0.0361 (8) | |
H7A | 0.9803 | 0.7333 | 0.2262 | 0.043* | |
C8 | 0.9603 (2) | 0.8325 (5) | 0.31042 (13) | 0.0337 (8) | |
H8A | 1.0189 | 0.7971 | 0.3253 | 0.040* | |
O3 | 0.74602 (16) | 0.8515 (4) | 0.14369 (9) | 0.0424 (6) | |
O4 | 0.88149 (19) | 0.6945 (4) | 0.13534 (10) | 0.0486 (7) | |
O5 | 0.66405 (13) | 0.8794 (3) | 0.54300 (10) | 0.0285 (5) | |
O6 | 0.67149 (13) | 1.1776 (3) | 0.51616 (9) | 0.0247 (4) | |
C9 | 0.6242 (2) | 1.0327 (5) | 0.52874 (16) | 0.0293 (7) | |
C10 | 0.5157 (2) | 1.0426 (5) | 0.52970 (16) | 0.0376 (8) | |
H10A | 0.4907 | 0.9706 | 0.5635 | 0.045* | |
H10B | 0.4946 | 1.1729 | 0.5331 | 0.045* |
U11 | U22 | U33 | U12 | U13 | U23 | |
La | 0.01657 (9) | 0.01669 (11) | 0.01450 (9) | −0.00152 (6) | −0.00020 (6) | 0.00152 (6) |
O1 | 0.0323 (11) | 0.0345 (15) | 0.0162 (10) | 0.0050 (9) | 0.0015 (8) | −0.0020 (9) |
O2 | 0.0243 (10) | 0.0378 (14) | 0.0217 (10) | −0.0031 (10) | −0.0081 (8) | −0.0016 (9) |
C1 | 0.0228 (14) | 0.0197 (17) | 0.0169 (13) | −0.0048 (11) | −0.0036 (11) | −0.0002 (11) |
C2 | 0.0240 (14) | 0.0248 (18) | 0.0186 (14) | −0.0005 (12) | −0.0043 (11) | −0.0025 (12) |
C3 | 0.0340 (16) | 0.039 (2) | 0.0246 (16) | 0.0136 (14) | −0.0038 (13) | −0.0070 (14) |
C4 | 0.0333 (18) | 0.042 (2) | 0.0320 (17) | 0.0112 (15) | −0.0141 (14) | −0.0037 (16) |
C5 | 0.0432 (19) | 0.0241 (19) | 0.0195 (14) | −0.0012 (13) | −0.0091 (13) | −0.0032 (13) |
C6 | 0.055 (2) | 0.0244 (19) | 0.0225 (15) | −0.0097 (15) | −0.0123 (15) | −0.0019 (14) |
C7 | 0.0396 (18) | 0.044 (2) | 0.0243 (15) | 0.0122 (15) | −0.0044 (14) | −0.0143 (15) |
C8 | 0.0294 (16) | 0.048 (2) | 0.0234 (15) | 0.0107 (15) | −0.0088 (13) | −0.0119 (15) |
O3 | 0.0468 (15) | 0.0549 (19) | 0.0256 (11) | −0.0100 (12) | −0.0167 (10) | 0.0095 (11) |
O4 | 0.0760 (18) | 0.0420 (18) | 0.0279 (12) | 0.0110 (14) | −0.0163 (12) | −0.0156 (12) |
O5 | 0.0216 (10) | 0.0155 (13) | 0.0483 (13) | 0.0007 (8) | −0.0087 (9) | 0.0021 (10) |
O6 | 0.0236 (10) | 0.0165 (12) | 0.0339 (11) | −0.0013 (8) | −0.0039 (8) | 0.0024 (9) |
C9 | 0.0193 (15) | 0.022 (2) | 0.0463 (19) | −0.0011 (12) | −0.0118 (14) | 0.0020 (15) |
C10 | 0.042 (2) | 0.026 (2) | 0.045 (2) | 0.0062 (15) | −0.0048 (16) | −0.0042 (17) |
La—O1 | 2.4380 (18) | C4—C5 | 1.382 (4) |
La—O2i | 2.390 (2) | C4—H4A | 0.9300 |
La—O3ii | 2.446 (2) | C5—C7 | 1.383 (4) |
La—O4iii | 2.450 (2) | C5—C6 | 1.504 (4) |
La—O5 | 2.6244 (19) | C6—O4 | 1.259 (4) |
La—O5iv | 2.532 (2) | C6—O3 | 1.265 (4) |
La—O6v | 2.573 (2) | C7—C8 | 1.378 (4) |
La—O6 | 2.6884 (19) | C7—H7A | 0.9300 |
O1—C1 | 1.253 (3) | C8—H8A | 0.9300 |
O2—C1 | 1.265 (3) | O5—C9 | 1.260 (4) |
C1—C2 | 1.502 (3) | O6—C9 | 1.254 (4) |
C2—C3 | 1.380 (4) | C9—C10 | 1.542 (4) |
C2—C8 | 1.386 (4) | C10—C10vi | 1.512 (7) |
C3—C4 | 1.391 (4) | C10—H10A | 0.9700 |
C3—H3A | 0.9300 | C10—H10B | 0.9700 |
O2i—La—O1 | 87.98 (7) | C3—C2—C8 | 119.7 (3) |
O2i—La—O3ii | 106.10 (7) | C3—C2—C1 | 120.0 (2) |
O1—La—O3ii | 147.90 (8) | C8—C2—C1 | 120.3 (2) |
O2i—La—O4iii | 75.13 (8) | C2—C3—C4 | 120.1 (3) |
O1—La—O4iii | 135.66 (8) | C2—C3—H3A | 119.9 |
O3ii—La—O4iii | 76.39 (9) | C4—C3—H3A | 119.9 |
O2i—La—O5iv | 79.84 (7) | C5—C4—C3 | 119.9 (3) |
O1—La—O5iv | 80.66 (7) | C5—C4—H4A | 120.1 |
O3ii—La—O5iv | 73.90 (8) | C3—C4—H4A | 120.1 |
O4iii—La—O5iv | 133.58 (8) | C7—C5—C4 | 119.8 (3) |
O2i—La—O6v | 103.99 (7) | C7—C5—C6 | 119.7 (3) |
O1—La—O6v | 75.02 (7) | C4—C5—C6 | 120.5 (3) |
O3ii—La—O6v | 126.55 (7) | O4—C6—O3 | 123.8 (3) |
O4iii—La—O6v | 70.07 (7) | O4—C6—C5 | 117.3 (3) |
O5iv—La—O6v | 155.16 (7) | O3—C6—C5 | 118.9 (3) |
O2i—La—O5 | 167.61 (7) | C8—C7—C5 | 120.3 (3) |
O1—La—O5 | 94.49 (7) | C8—C7—H7A | 119.8 |
O3ii—La—O5 | 77.94 (7) | C5—C7—H7A | 119.8 |
O4iii—La—O5 | 94.85 (8) | C7—C8—C2 | 120.1 (3) |
O5iv—La—O5 | 112.53 (6) | C7—C8—H8A | 119.9 |
O6v—La—O5 | 65.15 (6) | C2—C8—H8A | 119.9 |
O2i—La—O6 | 143.61 (7) | C6—O3—Lavii | 144.9 (2) |
O1—La—O6 | 78.65 (7) | C6—O4—Laviii | 123.0 (2) |
O3ii—La—O6 | 72.99 (7) | C9—O5—Lav | 152.08 (19) |
O4iii—La—O6 | 136.12 (8) | C9—O5—La | 96.17 (18) |
O5iv—La—O6 | 64.75 (6) | Lav—O5—La | 111.17 (7) |
O6v—La—O6 | 104.90 (6) | C9—O6—Laiv | 132.9 (2) |
O5—La—O6 | 48.61 (7) | C9—O6—La | 93.29 (17) |
O2i—La—C9 | 167.94 (8) | Laiv—O6—La | 107.90 (7) |
O1—La—C9 | 88.44 (9) | O6—C9—O5 | 120.9 (3) |
O3ii—La—C9 | 71.73 (9) | O6—C9—C10 | 120.1 (3) |
O4iii—La—C9 | 115.04 (9) | O5—C9—C10 | 118.9 (3) |
O5iv—La—C9 | 88.21 (7) | O6—C9—La | 62.32 (15) |
O6v—La—C9 | 86.18 (7) | O5—C9—La | 59.41 (15) |
O5—La—C9 | 24.42 (8) | C10—C9—La | 168.4 (2) |
O6—La—C9 | 24.40 (7) | C10vi—C10—C9 | 105.4 (3) |
C1—O1—La | 131.18 (18) | C10vi—C10—H10A | 110.7 |
C1—O2—Lai | 151.6 (2) | C9—C10—H10A | 110.7 |
O1—C1—O2 | 123.0 (2) | C10vi—C10—H10B | 110.7 |
O1—C1—C2 | 118.9 (2) | C9—C10—H10B | 110.7 |
O2—C1—C2 | 118.1 (2) | H10A—C10—H10B | 108.8 |
Symmetry codes: (i) −x+2, −y+2, −z+1; (ii) −x+3/2, −y+2, z+1/2; (iii) x, −y+3/2, z+1/2; (iv) −x+3/2, y+1/2, z; (v) −x+3/2, y−1/2, z; (vi) −x+1, −y+2, −z+1; (vii) −x+3/2, −y+2, z−1/2; (viii) x, −y+3/2, z−1/2. |
Experimental details
Crystal data | |
Chemical formula | [La2(C4H4O4)(C8H4O4)2] |
Mr | 361.06 |
Crystal system, space group | Orthorhombic, Pbca |
Temperature (K) | 291 |
a, b, c (Å) | 14.2014 (4), 7.0513 (1), 22.1100 (5) |
V (Å3) | 2214.06 (9) |
Z | 8 |
Radiation type | Mo Kα |
µ (mm−1) | 3.87 |
Crystal size (mm) | 0.33 × 0.27 × 0.18 |
Data collection | |
Diffractometer | Bruker SMART CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.293, 0.492 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 11927, 2505, 1974 |
Rint | 0.029 |
(sin θ/λ)max (Å−1) | 0.649 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.021, 0.051, 1.02 |
No. of reflections | 2505 |
No. of parameters | 155 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.31, −0.53 |
Computer programs: SMART (Bruker, 1998), SAINT (Bruker, 1998), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1998).
La—O1 | 2.4380 (18) | La—O5 | 2.6244 (19) |
La—O2i | 2.390 (2) | La—O5iv | 2.532 (2) |
La—O3ii | 2.446 (2) | La—O6v | 2.573 (2) |
La—O4iii | 2.450 (2) | La—O6 | 2.6884 (19) |
Symmetry codes: (i) −x+2, −y+2, −z+1; (ii) −x+3/2, −y+2, z+1/2; (iii) x, −y+3/2, z+1/2; (iv) −x+3/2, y+1/2, z; (v) −x+3/2, y−1/2, z. |
The title compound, (I), is isostructural with its [M2(C8H4O4)2(C4H4O4)]n [M = Gd (Wang & Li, 2005), Dy ((Li & Wang, 2005), Nd (Li et al., 2006), Er (He et al., 2006)] analogues. As depicted in Fig.1, The La3+ ion is located at the center of a distorted square antiprism geometry and is coordinated by four oxygen atoms from four BDC and four from three succinate anions. The La—O bond distances ranging from 2.390 (2) to 2.6884 (19) Å.
In (I), the succinate ligand is located on an inversion centre and functions as an octadentate ligand, bis-chelating two La atoms with each O atom bridging to another La atom. In this mode, the La atoms are linked into a two-dimensional polymeric sheet parallel to the (001) plane. These sheets are in turn bridged via benzene-1,4-dicarboxylate ligands, forming a three-dimensional framework.