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The title compound, [La2(betc)(H2betc)(H2O)2]n (betc = benzene-1,2,4,5-tetracarboxylate, C10H2O4, and H2betc is 2,5-dicarboxybenzene-1,4-dicarboxylate, C10H4O4) was obtained by hydrothermal reaction. The compound possesses an infinite three-dimensional network structure. The central LaIII atom is nine-coordinate by eight carboxylate O atoms from six different organic ligands derived from H4betc (1,2,4,5-benzenetetracarboxylic acid), with La—O distances ranging from 2.439 (4) to 2.658 (4) Å, and one water molecule, with La—OW1 = 2.503 (5) Å.
Supporting information
CCDC reference: 239041
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.008 Å
- R factor = 0.029
- wR factor = 0.078
- Data-to-parameter ratio = 9.9
checkCIF/PLATON results
No syntax errors found
Alert level B
CELLV02_ALERT_1_B The supplied cell volume s.u. differs from that
calculated from the cell parameter s.u.'s by > 4
Calculated cell volume su = 8.76
Cell volume su given = 3.00
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio
PLAT088_ALERT_3_C Poor Data / Parameter Ratio .................... 9.93
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ?
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
PLAT213_ALERT_2_C Atom C4 has ADP max/min Ratio ............. 3.50 oblate
PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.54 Ratio
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... La1
PLAT369_ALERT_2_C Long C(sp2)-C(sp2) Bond C2 - C8 ... 1.53 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 3
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.36 Ratio
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
14 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
4 ALERT type 2 Indicator that the structure model may be wrong or deficient
1 ALERT type 3 Indicator that the structure quality may be low
5 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Siemens, 1996); cell refinement: SMART and SAINT (Siemens,1994); data reduction: XPREP in SHELXTL (Siemens, 1994); program(s) used to solve structure: SHELXTL; program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
Poly[diaqua(µ
6-benzene-1,2,4,5-tetracarboxylato)(µ
6-2,5-
dicarboxybenzene-1,4-dicarboxylato)dilanthanum(III)]
top
Crystal data top
[La2(C10H2O4)(C10H4O4)(H2O)2] | Z = 1 |
Mr = 816.10 | F(000) = 388 |
Triclinic, P1 | Dx = 2.465 Mg m−3 |
a = 6.441 (1) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 9.4467 (3) Å | Cell parameters from 2449 reflections |
c = 9.6323 (1) Å | θ = 2.2–25.0° |
α = 88.518 (2)° | µ = 3.93 mm−1 |
β = 74.744 (2)° | T = 293 K |
γ = 76.660 (2)° | Prism, colorless |
V = 549.80 (3) Å3 | 0.30 × 0.20 × 0.16 mm |
Data collection top
Bruker SMART CCD area-detector diffractometer | 1917 independent reflections |
Radiation source: fine-focus sealed tube | 1793 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.023 |
φ and ω scans | θmax = 25.0°, θmin = 2.2° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −7→7 |
Tmin = 0.348, Tmax = 0.533 | k = −11→11 |
2896 measured reflections | l = −11→7 |
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 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.078 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.00 | w = 1/[σ2(Fo2) + (0.0509P)2 + 2.7076P] where P = (Fo2 + 2Fc2)/3 |
1917 reflections | (Δ/σ)max < 0.001 |
193 parameters | Δρmax = 0.91 e Å−3 |
0 restraints | Δρmin = −1.36 e Å−3 |
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 | |
La1 | 0.34895 (4) | 0.94035 (3) | 0.72119 (3) | 0.01164 (13) | |
O1 | 0.5887 (8) | 0.5249 (5) | 0.8024 (5) | 0.0295 (10) | |
H1A | 0.504 (12) | 0.571 (8) | 0.763 (7) | 0.025 (18)* | |
OW1 | 0.6630 (10) | 1.0520 (8) | 0.7279 (7) | 0.0440 (14) | |
HW1B | 0.765 (13) | 1.074 (8) | 0.672 (8) | 0.03 (2)* | |
HW1A | 0.611 (12) | 1.129 (8) | 0.717 (8) | 0.02 (2)* | |
O2 | 0.6096 (7) | 0.7535 (4) | 0.8356 (5) | 0.0278 (10) | |
O3 | 0.7329 (6) | 0.8935 (4) | 1.0664 (4) | 0.0233 (9) | |
O4 | 1.0337 (7) | 0.8687 (4) | 0.8843 (5) | 0.0287 (10) | |
O5 | 0.3410 (6) | 1.1289 (4) | 0.5119 (4) | 0.0203 (8) | |
O6 | 0.0455 (6) | 1.1610 (4) | 0.6952 (4) | 0.0173 (8) | |
O7 | 0.1317 (6) | 1.8503 (4) | 0.5613 (4) | 0.0199 (8) | |
O8 | 0.3527 (6) | 1.6773 (4) | 0.6465 (4) | 0.0210 (8) | |
C1 | 0.8378 (9) | 0.5622 (6) | 0.9301 (6) | 0.0151 (10) | |
C2 | 0.9446 (8) | 0.6525 (5) | 0.9860 (5) | 0.0135 (10) | |
C3 | 0.1655 (8) | 1.4606 (5) | 0.5706 (5) | 0.0125 (10) | |
H3A | 0.2767 | 1.4344 | 0.6178 | 0.015* | |
C4 | 0.0701 (8) | 1.3552 (5) | 0.5332 (5) | 0.0126 (10) | |
C5 | 0.1531 (8) | 1.2036 (5) | 0.5812 (5) | 0.0115 (10) | |
C6 | 0.8976 (9) | 0.4114 (6) | 0.9437 (6) | 0.0166 (11) | |
H6A | 0.8291 | 0.3523 | 0.9041 | 0.020* | |
C7 | 0.6690 (9) | 0.6235 (6) | 0.8517 (6) | 0.0179 (11) | |
C8 | 0.8969 (8) | 0.8185 (6) | 0.9775 (5) | 0.0144 (10) | |
C9 | 0.0960 (8) | 1.6067 (5) | 0.5379 (6) | 0.0132 (10) | |
C10 | 0.1987 (8) | 1.7184 (5) | 0.5842 (5) | 0.0131 (10) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
La1 | 0.01127 (18) | 0.00827 (18) | 0.01676 (19) | −0.00222 (12) | −0.00620 (12) | 0.00152 (11) |
O1 | 0.035 (2) | 0.017 (2) | 0.051 (3) | −0.0089 (19) | −0.035 (2) | 0.008 (2) |
OW1 | 0.034 (3) | 0.063 (5) | 0.043 (3) | −0.033 (3) | −0.006 (3) | −0.001 (3) |
O2 | 0.036 (2) | 0.016 (2) | 0.041 (2) | −0.0022 (18) | −0.030 (2) | 0.0027 (18) |
O3 | 0.018 (2) | 0.024 (2) | 0.028 (2) | −0.0034 (17) | −0.0055 (17) | −0.0041 (17) |
O4 | 0.033 (2) | 0.020 (2) | 0.031 (2) | −0.0157 (18) | 0.0037 (19) | 0.0052 (18) |
O5 | 0.020 (2) | 0.0115 (18) | 0.026 (2) | 0.0025 (15) | −0.0051 (17) | 0.0005 (15) |
O6 | 0.0157 (18) | 0.0143 (18) | 0.0203 (19) | −0.0009 (15) | −0.0046 (15) | 0.0053 (15) |
O7 | 0.027 (2) | 0.0070 (18) | 0.032 (2) | −0.0048 (15) | −0.0192 (18) | 0.0038 (15) |
O8 | 0.024 (2) | 0.0134 (19) | 0.032 (2) | −0.0017 (16) | −0.0193 (18) | 0.0002 (16) |
C1 | 0.016 (3) | 0.012 (2) | 0.018 (3) | −0.003 (2) | −0.007 (2) | 0.001 (2) |
C2 | 0.015 (2) | 0.009 (2) | 0.017 (2) | −0.004 (2) | −0.004 (2) | 0.0010 (19) |
C3 | 0.012 (2) | 0.009 (2) | 0.019 (2) | −0.0006 (19) | −0.010 (2) | 0.0023 (19) |
C4 | 0.013 (2) | 0.004 (2) | 0.020 (3) | 0.0020 (19) | −0.006 (2) | 0.0041 (19) |
C5 | 0.011 (2) | 0.006 (2) | 0.020 (3) | 0.0025 (19) | −0.011 (2) | −0.0016 (19) |
C6 | 0.022 (3) | 0.012 (3) | 0.021 (3) | −0.006 (2) | −0.012 (2) | −0.001 (2) |
C7 | 0.016 (3) | 0.016 (3) | 0.025 (3) | −0.004 (2) | −0.010 (2) | 0.006 (2) |
C8 | 0.017 (3) | 0.013 (3) | 0.018 (3) | −0.005 (2) | −0.012 (2) | −0.001 (2) |
C9 | 0.009 (2) | 0.010 (2) | 0.020 (3) | −0.0007 (19) | −0.005 (2) | −0.001 (2) |
C10 | 0.015 (2) | 0.012 (3) | 0.014 (2) | −0.004 (2) | −0.006 (2) | 0.0005 (19) |
Geometric parameters (Å, º) top
La1—O4i | 2.439 (4) | O6—C5 | 1.246 (6) |
La1—O3ii | 2.478 (4) | O7—C10 | 1.255 (6) |
La1—OW1 | 2.503 (5) | O7—La1vi | 2.609 (4) |
La1—O5iii | 2.563 (4) | O8—C10 | 1.272 (6) |
La1—O6 | 2.564 (4) | O8—La1vi | 2.598 (4) |
La1—O2 | 2.579 (4) | C1—C6 | 1.399 (7) |
La1—O8iv | 2.598 (4) | C1—C2 | 1.407 (7) |
La1—O7iv | 2.609 (4) | C1—C7 | 1.486 (7) |
La1—O5 | 2.658 (4) | C2—C6vii | 1.384 (7) |
O1—C7 | 1.317 (7) | C2—C8 | 1.531 (7) |
O1—H1A | 0.78 (7) | C3—C4 | 1.384 (7) |
OW1—HW1B | 0.79 (8) | C3—C9 | 1.404 (7) |
OW1—HW1A | 0.75 (7) | C3—H3A | 0.9300 |
O2—C7 | 1.218 (7) | C4—C9viii | 1.392 (7) |
O3—C8 | 1.250 (7) | C4—C5 | 1.515 (6) |
O3—La1ii | 2.478 (4) | C6—C2vii | 1.384 (7) |
O4—C8 | 1.249 (7) | C6—H6A | 0.9300 |
O4—La1v | 2.439 (4) | C9—C4viii | 1.392 (7) |
O5—C5 | 1.270 (6) | C9—C10 | 1.501 (7) |
O5—La1iii | 2.563 (4) | | |
| | | |
O4i—La1—O3ii | 77.72 (14) | O7iv—La1—C5 | 74.25 (12) |
O4i—La1—OW1 | 140.14 (18) | O5—La1—C5 | 25.24 (13) |
O3ii—La1—OW1 | 66.59 (18) | C10iv—La1—C5 | 99.05 (13) |
O4i—La1—O5iii | 144.77 (13) | C7—O1—H1A | 104 (5) |
O3ii—La1—O5iii | 136.51 (13) | La1—OW1—HW1B | 138 (5) |
OW1—La1—O5iii | 70.31 (17) | La1—OW1—HW1A | 99 (6) |
O4i—La1—O6 | 81.64 (13) | HW1B—OW1—HW1A | 81 (7) |
O3ii—La1—O6 | 72.51 (13) | C7—O2—La1 | 142.3 (4) |
OW1—La1—O6 | 103.0 (2) | C8—O3—La1ii | 139.0 (3) |
O5iii—La1—O6 | 112.76 (11) | C8—O4—La1v | 169.9 (4) |
O4i—La1—O2 | 89.14 (15) | C5—O5—La1iii | 151.3 (3) |
O3ii—La1—O2 | 88.89 (13) | C5—O5—La1 | 91.6 (3) |
OW1—La1—O2 | 73.5 (2) | La1iii—O5—La1 | 116.01 (13) |
O5iii—La1—O2 | 84.46 (13) | C5—O6—La1 | 96.6 (3) |
O6—La1—O2 | 160.58 (13) | C10—O7—La1vi | 93.9 (3) |
O4i—La1—O8iv | 71.89 (14) | C10—O8—La1vi | 94.0 (3) |
O3ii—La1—O8iv | 142.69 (13) | C6—C1—C2 | 119.5 (5) |
OW1—La1—O8iv | 130.00 (19) | C6—C1—C7 | 119.3 (5) |
O5iii—La1—O8iv | 73.38 (13) | C2—C1—C7 | 121.1 (5) |
O6—La1—O8iv | 122.39 (12) | C6vii—C2—C1 | 118.4 (5) |
O2—La1—O8iv | 69.81 (12) | C6vii—C2—C8 | 116.7 (4) |
O4i—La1—O7iv | 73.08 (14) | C1—C2—C8 | 124.9 (5) |
O3ii—La1—O7iv | 137.92 (13) | C4—C3—C9 | 120.6 (5) |
OW1—La1—O7iv | 146.62 (17) | C4—C3—H3A | 119.7 |
O5iii—La1—O7iv | 80.26 (12) | C9—C3—H3A | 119.7 |
O6—La1—O7iv | 73.82 (12) | C3—C4—C9viii | 120.1 (4) |
O2—La1—O7iv | 119.80 (12) | C3—C4—C5 | 115.0 (4) |
O8iv—La1—O7iv | 50.01 (11) | C9viii—C4—C5 | 124.8 (4) |
O4i—La1—O5 | 127.32 (13) | O6—C5—O5 | 121.6 (4) |
O3ii—La1—O5 | 101.14 (13) | O6—C5—C4 | 119.1 (4) |
OW1—La1—O5 | 78.40 (18) | O5—C5—C4 | 118.9 (4) |
O5iii—La1—O5 | 63.99 (13) | O6—C5—La1 | 58.8 (2) |
O6—La1—O5 | 49.70 (12) | O5—C5—La1 | 63.2 (3) |
O2—La1—O5 | 143.38 (13) | C4—C5—La1 | 167.3 (3) |
O8iv—La1—O5 | 114.33 (12) | C2vii—C6—C1 | 122.1 (5) |
O7iv—La1—O5 | 74.67 (12) | C2vii—C6—H6A | 119.0 |
O4i—La1—C10iv | 68.23 (14) | C1—C6—H6A | 119.0 |
O3ii—La1—C10iv | 145.64 (13) | O2—C7—O1 | 123.2 (5) |
OW1—La1—C10iv | 146.87 (19) | O2—C7—C1 | 122.8 (5) |
O5iii—La1—C10iv | 77.84 (13) | O1—C7—C1 | 114.0 (5) |
O6—La1—C10iv | 97.42 (13) | O4—C8—O3 | 124.9 (5) |
O2—La1—C10iv | 94.93 (13) | O4—C8—C2 | 116.3 (5) |
O8iv—La1—C10iv | 25.28 (13) | O3—C8—C2 | 118.7 (5) |
O7iv—La1—C10iv | 24.93 (12) | C4viii—C9—C3 | 119.3 (5) |
O5—La1—C10iv | 95.95 (13) | C4viii—C9—C10 | 121.8 (4) |
O4i—La1—C5 | 105.03 (14) | C3—C9—C10 | 119.0 (4) |
O3ii—La1—C5 | 85.06 (13) | O7—C10—O8 | 121.1 (4) |
OW1—La1—C5 | 89.48 (19) | O7—C10—C9 | 119.7 (4) |
O5iii—La1—C5 | 89.01 (13) | O8—C10—C9 | 119.2 (4) |
O6—La1—C5 | 24.57 (13) | O7—C10—La1vi | 61.2 (3) |
O2—La1—C5 | 162.97 (14) | O8—C10—La1vi | 60.8 (3) |
O8iv—La1—C5 | 123.18 (12) | C9—C10—La1vi | 170.8 (3) |
Symmetry codes: (i) x−1, y, z; (ii) −x+1, −y+2, −z+2; (iii) −x+1, −y+2, −z+1; (iv) x, y−1, z; (v) x+1, y, z; (vi) x, y+1, z; (vii) −x+2, −y+1, −z+2; (viii) −x, −y+3, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1A···O8iv | 0.78 (7) | 1.82 (7) | 2.592 (5) | 170 (7) |
OW1—HW1B···O6v | 0.79 (8) | 2.22 (8) | 2.824 (6) | 134 (7) |
OW1—HW1B···O7ix | 0.79 (8) | 2.32 (8) | 2.975 (7) | 141 (7) |
Symmetry codes: (iv) x, y−1, z; (v) x+1, y, z; (ix) −x+1, −y+3, −z+1. |
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