Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807051975/zl2067sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807051975/zl2067Isup2.hkl |
CCDC reference: 639897
A mixture of ErCl3 (0.5 mmol, 0.186 g), benzenedicarboxylic acid (0.75 mmol, 0.125 g), NaOH (1.5 mmol; 0.06 g) and H2O (10 ml) was placed in a 20 ml Teflon reactor, which was heated to 433 K for three days and then cooled to room temperature at a rate of 10 K h-1. The crystals obtained were washed with water and dryed in air.
Two types of large apparently unfilled voids are found in the unit cell of the title compound. Their volumes were calculated using PLATON (Spek, 2003) as 142.3 and 75.6 Å3 (5.3% and 2.8% of the unit cell volume), respectively. The larger void is located close to one of phenyl rings of the 1,3-BDC ligands, giving it enough room to rotate around the C—C bond connecting the ring which may result in the disorder; the smaller unfilled void is located close to a disordered water solvate molecule. Based on these observations, one of the phenyl rings and the lattice water molecule were split into two positions. The occupancy ratios refined to 0.595 (2) to 0.405 (2) and 0.661 (1) to 0.339 (1), respectively. Due to the significant overlap of the disordered atoms the following restraints were applied: The phenyl ring C11 C12 C13 C14 C15 C16 and its disordered counterpart were each restrained to be flat and its equivalent bond distances were restrained to be the same within a standard deviation of 0.01 Å. All water H atoms were tentatively located in difference density Fourier maps and were refined with O—H distance restraints of 0.82 (1) Å and with Uiso(H) = 1.5Ueq(O). The hydrogen atoms of the disordered water molecule were set to have each the same coordinates for both disordered H2O molecules. Carbon-bound H atoms were placed at calculated positions and were treated as riding on the parent C atoms with C—H = 0.93 Å, and with Uiso(H) = 1.2Ueq(C).
As a building block, benzene-1,3-dicarboxylic acid (1,3-BDC) is an excellent candidate for the construction of supramolecular complexes (Bourne et al., 2001; Zhang et al., 2003). Recently, we obtained the title coordination polymer by the reaction of ErCl3 with benzene-1,3-dicarboxylic acid in alkaline aqueous solution, and its crystal structure is reported here.
Each of the two crystallographically independent ErIII centres is seven-coordinate and has a distorted pentagonal bipyramidal geometry: one Er centre is coordinated by seven oxygen atoms from six 1,3-BDC ligands, and the other Er centre is surrounded by five oxygen atoms from five 1,3-BDC ligands and two water molecules (Fig. 1). The adjacent Er···Er separations are 4.448 (4) and 4.965 (5) Å, respectively. The dianionic ligands cross-link the metal ions to form a three-dimensional network with channels running along the c axis hosting an uncoordinated disordered water molecule (Fig. 2). The title compound exhibits two types of large voids that seem to be partially filled by diffuse solvent (no corrections for this were applied to the dataset). The larger of the voids has a volume of of 142.3 Å3 (5.3% of the unit cell volume) and is located in close proximity to a disordered phenyl ring of one of the 1,3-BDC ligands. The large void thus gives the phenyl ring additional degrees of freedom which can be seen as a likely cause of the disorder of the phenyl ring. The second type of void in the structure (75.6 Å3, 2.8% of the unit cell volume) is located close to the disordered water solvate molecule (see refinement section for details). These water molecules are hydrogen bonded to coordinated water molecules and carboxylate units that all form a hydrogen bonded chain parallel to the b axis (Table 1).
For related literature, see: Bourne et al. (2001); Zhang et al. (2003). PLATON (Spek, 2003) was used for the analysis of voids in the structure.
Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT (Bruker, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2004); software used to prepare material for publication: SHELXTL (Bruker, 2004).
[Er2(C8H4O4)3(H2O)2]·H2O | F(000) = 1672 |
Mr = 880.90 | Dx = 2.185 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 6000 reflections |
a = 10.5553 (2) Å | θ = 1.7–28.0° |
b = 14.9526 (3) Å | µ = 6.30 mm−1 |
c = 17.4798 (3) Å | T = 293 K |
β = 103.908 (1)° | Block, red |
V = 2677.94 (9) Å3 | 0.25 × 0.19 × 0.16 mm |
Z = 4 |
Bruker APEXII area-detector diffractometer | 6127 independent reflections |
Radiation source: fine-focus sealed tube | 5579 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.028 |
φ and ω scans | θmax = 27.5°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −13→13 |
Tmin = 0.248, Tmax = 0.369 | k = −18→19 |
33045 measured reflections | l = −22→22 |
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)] = 0.019 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.045 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0206P)2 + 2.4501P] where P = (Fo2 + 2Fc2)/3 |
6127 reflections | (Δ/σ)max = 0.002 |
429 parameters | Δρmax = 0.74 e Å−3 |
68 restraints | Δρmin = −0.75 e Å−3 |
[Er2(C8H4O4)3(H2O)2]·H2O | V = 2677.94 (9) Å3 |
Mr = 880.90 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 10.5553 (2) Å | µ = 6.30 mm−1 |
b = 14.9526 (3) Å | T = 293 K |
c = 17.4798 (3) Å | 0.25 × 0.19 × 0.16 mm |
β = 103.908 (1)° |
Bruker APEXII area-detector diffractometer | 6127 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 5579 reflections with I > 2σ(I) |
Tmin = 0.248, Tmax = 0.369 | Rint = 0.028 |
33045 measured reflections |
R[F2 > 2σ(F2)] = 0.019 | 68 restraints |
wR(F2) = 0.045 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.06 | Δρmax = 0.74 e Å−3 |
6127 reflections | Δρmin = −0.75 e Å−3 |
429 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 | 0.4248 (3) | 0.86190 (19) | 0.39035 (18) | 0.0260 (6) | |
C2 | 0.5658 (3) | 0.8382 (2) | 0.41007 (18) | 0.0265 (6) | |
C3 | 0.6091 (3) | 0.7605 (2) | 0.3798 (2) | 0.0345 (7) | |
H3 | 0.5493 | 0.7234 | 0.3468 | 0.041* | |
C4 | 0.7393 (3) | 0.7386 (2) | 0.3985 (2) | 0.0414 (9) | |
H4 | 0.7672 | 0.6862 | 0.3790 | 0.050* | |
C5 | 0.8288 (3) | 0.7944 (2) | 0.44620 (19) | 0.0329 (7) | |
H5 | 0.9170 | 0.7798 | 0.4581 | 0.039* | |
C6 | 0.7880 (3) | 0.87251 (19) | 0.47671 (17) | 0.0231 (6) | |
C7 | 0.6560 (3) | 0.8938 (2) | 0.45889 (17) | 0.0232 (6) | |
H7 | 0.6279 | 0.9454 | 0.4796 | 0.028* | |
C8 | 0.8849 (3) | 0.9284 (2) | 0.53231 (16) | 0.0228 (6) | |
C9 | 0.1432 (3) | 0.7014 (2) | 0.37867 (17) | 0.0261 (6) | |
C10 | 0.1544 (4) | 0.6373 (2) | 0.44503 (19) | 0.0356 (8) | |
C11 | 0.1555 (11) | 0.5435 (4) | 0.4307 (4) | 0.043 (2) | 0.595 (17) |
H11 | 0.1552 | 0.5225 | 0.3806 | 0.051* | 0.595 (17) |
C12 | 0.1570 (14) | 0.4837 (4) | 0.4916 (4) | 0.053 (3) | 0.595 (17) |
H12 | 0.1670 | 0.4228 | 0.4837 | 0.064* | 0.595 (17) |
C13 | 0.1438 (13) | 0.5141 (4) | 0.5636 (4) | 0.043 (2) | 0.595 (17) |
H13 | 0.1346 | 0.4734 | 0.6022 | 0.052* | 0.595 (17) |
C14 | 0.1441 (4) | 0.6070 (2) | 0.57907 (19) | 0.0406 (9) | |
C15 | 0.1481 (17) | 0.6677 (5) | 0.5196 (4) | 0.020 (3) | 0.595 (17) |
H15 | 0.1466 | 0.7288 | 0.5294 | 0.024* | 0.595 (17) |
C12' | 0.241 (2) | 0.4969 (8) | 0.5074 (6) | 0.057 (4) | 0.405 (17) |
H12' | 0.2761 | 0.4402 | 0.5047 | 0.069* | 0.405 (17) |
C13' | 0.2122 (17) | 0.5254 (7) | 0.5762 (6) | 0.045 (3) | 0.405 (17) |
H13' | 0.2377 | 0.4908 | 0.6215 | 0.054* | 0.405 (17) |
C11' | 0.2174 (15) | 0.5528 (6) | 0.4422 (7) | 0.046 (3) | 0.405 (17) |
H11' | 0.2424 | 0.5356 | 0.3969 | 0.055* | 0.405 (17) |
C15' | 0.124 (2) | 0.6645 (8) | 0.5149 (6) | 0.023 (5) | 0.405 (17) |
H15' | 0.0898 | 0.7213 | 0.5185 | 0.028* | 0.405 (17) |
C16 | 0.1198 (3) | 0.6381 (2) | 0.65529 (17) | 0.0277 (6) | |
C17 | −0.1653 (3) | 0.9341 (2) | 0.26831 (18) | 0.0266 (6) | |
C18 | −0.2393 (3) | 0.86014 (19) | 0.22034 (18) | 0.0255 (6) | |
C19 | −0.3618 (3) | 0.8754 (2) | 0.1715 (2) | 0.0376 (8) | |
H19 | −0.3973 | 0.9327 | 0.1679 | 0.045* | |
C20 | −0.4318 (3) | 0.8064 (2) | 0.1280 (2) | 0.0441 (9) | |
H20 | −0.5135 | 0.8175 | 0.0949 | 0.053* | |
C21 | −0.3796 (3) | 0.7207 (2) | 0.1339 (2) | 0.0343 (7) | |
H21 | −0.4271 | 0.6739 | 0.1057 | 0.041* | |
C22 | −0.2561 (3) | 0.70480 (19) | 0.18197 (18) | 0.0252 (6) | |
C23 | −0.1856 (3) | 0.77463 (19) | 0.22438 (17) | 0.0238 (6) | |
H23 | −0.1023 | 0.7643 | 0.2556 | 0.029* | |
C24 | −0.2007 (3) | 0.6126 (2) | 0.18770 (17) | 0.0249 (6) | |
Er1 | 0.123252 (11) | 0.638620 (8) | 0.184714 (7) | 0.01869 (4) | |
Er2 | 0.165788 (12) | 0.917258 (8) | 0.343349 (7) | 0.01900 (4) | |
O1 | 0.3531 (2) | 0.83950 (16) | 0.32336 (13) | 0.0330 (5) | |
O2 | 0.3765 (2) | 0.90475 (15) | 0.43797 (13) | 0.0344 (5) | |
O3 | 0.85407 (19) | 1.00772 (14) | 0.54583 (11) | 0.0250 (4) | |
O4 | 0.9920 (2) | 0.89345 (16) | 0.56502 (12) | 0.0325 (5) | |
O5 | 0.1421 (3) | 0.67059 (18) | 0.31182 (13) | 0.0471 (7) | |
O6 | 0.1334 (2) | 0.78295 (14) | 0.39261 (13) | 0.0342 (5) | |
O7 | 0.0848 (2) | 0.71862 (14) | 0.65904 (13) | 0.0323 (5) | |
O8 | 0.1330 (3) | 0.58356 (15) | 0.71069 (13) | 0.0393 (6) | |
O9 | −0.0799 (2) | 0.60084 (16) | 0.20490 (14) | 0.0366 (5) | |
O10 | −0.2784 (2) | 0.54756 (14) | 0.17309 (14) | 0.0338 (5) | |
O11 | −0.0531 (2) | 0.91931 (17) | 0.30952 (15) | 0.0400 (6) | |
O12 | −0.2207 (2) | 1.00858 (15) | 0.26555 (15) | 0.0430 (6) | |
O2W | 0.2469 (2) | 0.60998 (19) | 0.09076 (15) | 0.0402 (6) | |
H3W | 0.3236 (16) | 0.595 (3) | 0.103 (3) | 0.060* | |
H4W | 0.221 (4) | 0.580 (3) | 0.0511 (16) | 0.060* | |
O3W | 0.3326 (2) | 0.6988 (2) | 0.22505 (18) | 0.0520 (8) | |
H5W | 0.347 (5) | 0.743 (2) | 0.254 (2) | 0.078* | |
H6W | 0.398 (3) | 0.668 (3) | 0.227 (3) | 0.078* | |
O1WA | 0.5067 (13) | 0.5632 (10) | 0.2455 (10) | 0.0634 (18) | 0.339 (12) |
H1WA | 0.5571 (14) | 0.549 (4) | 0.2180 (16) | 0.095* | 0.339 (12) |
H2WA | 0.459 (5) | 0.520 (2) | 0.2300 (15) | 0.095* | 0.339 (12) |
O1WB | 0.4793 (6) | 0.5556 (5) | 0.1995 (5) | 0.0634 (18) | 0.661 (12) |
H1WB | 0.5571 (14) | 0.549 (4) | 0.2180 (16) | 0.095* | 0.661 (12) |
H2WB | 0.459 (5) | 0.520 (2) | 0.2300 (15) | 0.095* | 0.661 (12) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0277 (16) | 0.0197 (14) | 0.0283 (16) | −0.0009 (12) | 0.0022 (13) | −0.0013 (12) |
C2 | 0.0262 (15) | 0.0262 (15) | 0.0246 (15) | 0.0017 (12) | 0.0013 (12) | −0.0026 (12) |
C3 | 0.0336 (17) | 0.0279 (17) | 0.0358 (18) | 0.0034 (13) | −0.0039 (14) | −0.0105 (14) |
C4 | 0.041 (2) | 0.0354 (19) | 0.044 (2) | 0.0154 (15) | 0.0030 (16) | −0.0146 (16) |
C5 | 0.0262 (16) | 0.0369 (18) | 0.0332 (17) | 0.0119 (14) | 0.0026 (13) | −0.0051 (14) |
C6 | 0.0215 (14) | 0.0260 (15) | 0.0207 (14) | 0.0034 (11) | 0.0030 (11) | 0.0033 (11) |
C7 | 0.0250 (15) | 0.0216 (14) | 0.0224 (14) | 0.0028 (11) | 0.0045 (12) | −0.0020 (11) |
C8 | 0.0228 (14) | 0.0307 (16) | 0.0159 (13) | 0.0029 (12) | 0.0067 (11) | 0.0021 (11) |
C9 | 0.0286 (15) | 0.0296 (16) | 0.0198 (14) | 0.0007 (12) | 0.0053 (12) | 0.0041 (12) |
C10 | 0.065 (2) | 0.0231 (16) | 0.0209 (15) | 0.0101 (15) | 0.0143 (15) | 0.0026 (12) |
C11 | 0.083 (6) | 0.026 (3) | 0.023 (3) | 0.003 (3) | 0.020 (4) | −0.002 (2) |
C12 | 0.106 (7) | 0.019 (3) | 0.038 (4) | 0.007 (4) | 0.025 (4) | −0.002 (3) |
C13 | 0.080 (6) | 0.022 (3) | 0.032 (4) | 0.005 (3) | 0.022 (4) | 0.005 (2) |
C14 | 0.081 (3) | 0.0238 (16) | 0.0207 (16) | 0.0138 (17) | 0.0187 (17) | 0.0028 (13) |
C15 | 0.022 (5) | 0.014 (4) | 0.022 (4) | 0.004 (3) | 0.002 (3) | −0.001 (3) |
C12' | 0.097 (9) | 0.041 (6) | 0.040 (5) | 0.024 (6) | 0.029 (6) | 0.002 (4) |
C13' | 0.073 (8) | 0.034 (5) | 0.030 (5) | 0.015 (5) | 0.018 (5) | 0.014 (4) |
C11' | 0.075 (8) | 0.037 (5) | 0.030 (5) | 0.017 (5) | 0.021 (5) | 0.002 (4) |
C15' | 0.026 (9) | 0.024 (6) | 0.019 (6) | 0.001 (4) | 0.003 (4) | −0.002 (4) |
C16 | 0.0399 (18) | 0.0247 (15) | 0.0180 (14) | −0.0029 (13) | 0.0059 (13) | −0.0032 (12) |
C17 | 0.0295 (16) | 0.0238 (15) | 0.0258 (15) | −0.0083 (12) | 0.0053 (13) | −0.0003 (12) |
C18 | 0.0254 (15) | 0.0211 (14) | 0.0289 (16) | −0.0035 (11) | 0.0045 (12) | −0.0014 (12) |
C19 | 0.0329 (18) | 0.0197 (16) | 0.053 (2) | 0.0064 (13) | −0.0043 (16) | −0.0024 (14) |
C20 | 0.0330 (19) | 0.0287 (18) | 0.057 (2) | 0.0042 (14) | −0.0153 (16) | −0.0053 (17) |
C21 | 0.0303 (17) | 0.0240 (16) | 0.0433 (19) | −0.0023 (13) | −0.0014 (14) | −0.0088 (14) |
C22 | 0.0270 (15) | 0.0203 (14) | 0.0304 (16) | 0.0014 (12) | 0.0112 (12) | 0.0012 (12) |
C23 | 0.0198 (14) | 0.0232 (15) | 0.0288 (15) | 0.0001 (11) | 0.0065 (12) | 0.0023 (12) |
C24 | 0.0321 (17) | 0.0214 (14) | 0.0248 (15) | 0.0051 (12) | 0.0138 (13) | 0.0019 (12) |
Er1 | 0.01977 (7) | 0.01790 (7) | 0.01744 (7) | −0.00041 (4) | 0.00257 (5) | 0.00048 (5) |
Er2 | 0.02283 (7) | 0.01816 (7) | 0.01542 (7) | −0.00301 (5) | 0.00344 (5) | −0.00120 (5) |
O1 | 0.0238 (11) | 0.0396 (13) | 0.0324 (12) | −0.0005 (9) | 0.0003 (9) | −0.0148 (10) |
O2 | 0.0303 (12) | 0.0374 (13) | 0.0319 (12) | 0.0081 (10) | 0.0007 (10) | −0.0122 (10) |
O3 | 0.0265 (11) | 0.0291 (11) | 0.0182 (10) | −0.0003 (9) | 0.0029 (8) | −0.0022 (8) |
O4 | 0.0247 (11) | 0.0443 (13) | 0.0248 (11) | 0.0077 (10) | −0.0016 (9) | 0.0003 (10) |
O5 | 0.079 (2) | 0.0455 (15) | 0.0171 (11) | −0.0018 (14) | 0.0119 (12) | 0.0012 (10) |
O6 | 0.0466 (14) | 0.0240 (12) | 0.0356 (12) | 0.0014 (10) | 0.0168 (11) | 0.0102 (9) |
O7 | 0.0494 (14) | 0.0213 (11) | 0.0296 (12) | −0.0020 (10) | 0.0162 (10) | −0.0068 (9) |
O8 | 0.0684 (17) | 0.0319 (13) | 0.0176 (11) | −0.0004 (11) | 0.0105 (11) | 0.0037 (9) |
O9 | 0.0314 (13) | 0.0375 (13) | 0.0462 (14) | 0.0111 (10) | 0.0199 (11) | 0.0119 (11) |
O10 | 0.0384 (13) | 0.0187 (11) | 0.0455 (14) | 0.0026 (9) | 0.0125 (11) | −0.0041 (10) |
O11 | 0.0293 (13) | 0.0465 (15) | 0.0396 (14) | −0.0114 (11) | −0.0010 (11) | −0.0036 (11) |
O12 | 0.0498 (15) | 0.0200 (12) | 0.0528 (16) | −0.0052 (10) | −0.0001 (12) | −0.0092 (11) |
O2W | 0.0273 (12) | 0.0592 (17) | 0.0346 (14) | −0.0048 (12) | 0.0086 (11) | −0.0237 (12) |
O3W | 0.0266 (13) | 0.0621 (19) | 0.0632 (18) | −0.0064 (12) | 0.0028 (12) | −0.0415 (15) |
O1WA | 0.036 (3) | 0.066 (3) | 0.092 (5) | 0.005 (2) | 0.024 (4) | 0.008 (4) |
O1WB | 0.036 (3) | 0.066 (3) | 0.092 (5) | 0.005 (2) | 0.024 (4) | 0.008 (4) |
C1—O2 | 1.251 (4) | C18—C19 | 1.386 (4) |
C1—O1 | 1.277 (4) | C18—C23 | 1.393 (4) |
C1—C2 | 1.488 (4) | C19—C20 | 1.386 (5) |
C1—Er2 | 2.784 (3) | C19—H19 | 0.9300 |
C2—C7 | 1.391 (4) | C20—C21 | 1.390 (5) |
C2—C3 | 1.398 (4) | C20—H20 | 0.9300 |
C3—C4 | 1.374 (5) | C21—C22 | 1.391 (4) |
C3—H3 | 0.9300 | C21—H21 | 0.9300 |
C4—C5 | 1.380 (5) | C22—C23 | 1.388 (4) |
C4—H4 | 0.9300 | C22—C24 | 1.491 (4) |
C5—C6 | 1.395 (4) | C23—H23 | 0.9300 |
C5—H5 | 0.9300 | C24—O9 | 1.250 (4) |
C6—C7 | 1.390 (4) | C24—O10 | 1.258 (4) |
C6—C8 | 1.487 (4) | Er1—O7i | 2.199 (2) |
C7—H7 | 0.9300 | Er1—O5 | 2.234 (2) |
C8—O4 | 1.252 (3) | Er1—O4ii | 2.266 (2) |
C8—O3 | 1.268 (3) | Er1—O12iii | 2.273 (2) |
C9—O6 | 1.253 (4) | Er1—O9 | 2.325 (2) |
C9—O5 | 1.253 (4) | Er1—O3W | 2.333 (2) |
C9—C10 | 1.487 (4) | Er1—O2W | 2.370 (2) |
C10—C15 | 1.397 (6) | Er2—O11 | 2.243 (2) |
C10—C15' | 1.397 (8) | Er2—O6 | 2.243 (2) |
C10—C11 | 1.424 (6) | Er2—O8i | 2.261 (2) |
C10—C11' | 1.434 (8) | Er2—O3iv | 2.2913 (19) |
C11—C12 | 1.388 (7) | Er2—O10v | 2.336 (2) |
C11—H11 | 0.9300 | Er2—O1 | 2.390 (2) |
C12—C13 | 1.376 (7) | Er2—O2 | 2.439 (2) |
C12—H12 | 0.9300 | O3—Er2iv | 2.2913 (19) |
C13—C14 | 1.415 (6) | O4—Er1vi | 2.266 (2) |
C13—H13 | 0.9300 | O7—Er1vii | 2.199 (2) |
C14—C15' | 1.389 (8) | O8—Er2vii | 2.261 (2) |
C14—C15 | 1.389 (6) | O10—Er2iii | 2.336 (2) |
C14—C13' | 1.422 (8) | O12—Er1v | 2.273 (2) |
C14—C16 | 1.491 (4) | O2W—H3W | 0.817 (10) |
C15—H15 | 0.9300 | O2W—H4W | 0.819 (10) |
C12'—C13' | 1.376 (9) | O3W—H5W | 0.819 (10) |
C12'—C11' | 1.388 (9) | O3W—H6W | 0.822 (10) |
C12'—H12' | 0.9300 | O1WA—H1WA | 0.825 (10) |
C13'—H13' | 0.9300 | O1WA—H2WA | 0.822 (10) |
C11'—H11' | 0.9300 | O1WA—H1WB | 0.825 (10) |
C15'—H15' | 0.9300 | O1WA—H2WB | 0.822 (10) |
C16—O8 | 1.248 (4) | O1WB—H1WA | 0.813 (10) |
C16—O7 | 1.265 (4) | O1WB—H2WA | 0.817 (10) |
C17—O11 | 1.249 (4) | O1WB—H1WB | 0.813 (10) |
C17—O12 | 1.254 (4) | O1WB—H2WB | 0.817 (10) |
C17—C18 | 1.490 (4) | ||
O2—C1—O1 | 119.9 (3) | C23—C22—C21 | 119.9 (3) |
O2—C1—C2 | 120.8 (3) | C23—C22—C24 | 120.6 (3) |
O1—C1—C2 | 119.3 (3) | C21—C22—C24 | 119.6 (3) |
O2—C1—Er2 | 61.10 (16) | C22—C23—C18 | 120.3 (3) |
O1—C1—Er2 | 58.93 (15) | C22—C23—H23 | 119.9 |
C2—C1—Er2 | 174.7 (2) | C18—C23—H23 | 119.9 |
C7—C2—C3 | 119.4 (3) | O9—C24—O10 | 121.1 (3) |
C7—C2—C1 | 119.9 (3) | O9—C24—C22 | 120.4 (3) |
C3—C2—C1 | 120.7 (3) | O10—C24—C22 | 118.4 (3) |
C4—C3—C2 | 120.5 (3) | O7i—Er1—O5 | 87.89 (9) |
C4—C3—H3 | 119.7 | O7i—Er1—O4ii | 88.57 (9) |
C2—C3—H3 | 119.7 | O5—Er1—O4ii | 148.43 (9) |
C3—C4—C5 | 120.0 (3) | O7i—Er1—O12iii | 162.37 (9) |
C3—C4—H4 | 120.0 | O5—Er1—O12iii | 83.04 (10) |
C5—C4—H4 | 120.0 | O4ii—Er1—O12iii | 107.00 (9) |
C4—C5—C6 | 120.5 (3) | O7i—Er1—O9 | 97.76 (8) |
C4—C5—H5 | 119.7 | O5—Er1—O9 | 76.46 (10) |
C6—C5—H5 | 119.7 | O4ii—Er1—O9 | 72.98 (8) |
C7—C6—C5 | 119.5 (3) | O12iii—Er1—O9 | 94.78 (9) |
C7—C6—C8 | 120.9 (3) | O7i—Er1—O3W | 78.59 (10) |
C5—C6—C8 | 119.5 (3) | O5—Er1—O3W | 76.44 (10) |
C6—C7—C2 | 120.1 (3) | O4ii—Er1—O3W | 133.26 (9) |
C6—C7—H7 | 120.0 | O12iii—Er1—O3W | 84.59 (10) |
C2—C7—H7 | 120.0 | O9—Er1—O3W | 152.77 (9) |
O4—C8—O3 | 123.4 (3) | O7i—Er1—O2W | 98.02 (9) |
O4—C8—C6 | 117.9 (3) | O5—Er1—O2W | 142.72 (10) |
O3—C8—C6 | 118.7 (3) | O4ii—Er1—O2W | 68.79 (8) |
O6—C9—O5 | 123.8 (3) | O12iii—Er1—O2W | 80.58 (10) |
O6—C9—C10 | 118.1 (3) | O9—Er1—O2W | 138.00 (9) |
O5—C9—C10 | 118.1 (3) | O3W—Er1—O2W | 68.87 (9) |
C15—C10—C11 | 119.2 (5) | O11—Er2—O6 | 82.59 (9) |
C15'—C10—C11 | 117.0 (6) | O11—Er2—O8i | 80.53 (9) |
C15—C10—C11' | 116.4 (6) | O6—Er2—O8i | 112.88 (8) |
C15'—C10—C11' | 119.5 (7) | O11—Er2—O3iv | 85.32 (8) |
C15—C10—C9 | 120.3 (4) | O6—Er2—O3iv | 93.46 (8) |
C15'—C10—C9 | 120.2 (4) | O8i—Er2—O3iv | 147.91 (8) |
C11—C10—C9 | 120.0 (4) | O11—Er2—O10v | 118.58 (8) |
C11'—C10—C9 | 119.4 (5) | O6—Er2—O10v | 157.37 (9) |
C12—C11—C10 | 120.0 (6) | O8i—Er2—O10v | 80.53 (8) |
C12—C11—H11 | 120.0 | O3iv—Er2—O10v | 81.27 (8) |
C10—C11—H11 | 120.0 | O11—Er2—O1 | 143.48 (8) |
C13—C12—C11 | 120.2 (6) | O6—Er2—O1 | 80.12 (8) |
C13—C12—H12 | 119.9 | O8i—Er2—O1 | 77.04 (9) |
C11—C12—H12 | 119.9 | O3iv—Er2—O1 | 127.49 (7) |
C12—C13—C14 | 120.2 (6) | O10v—Er2—O1 | 85.68 (8) |
C12—C13—H13 | 119.9 | O11—Er2—O2 | 153.31 (9) |
C14—C13—H13 | 119.9 | O6—Er2—O2 | 82.50 (8) |
C15'—C14—C13 | 117.5 (6) | O8i—Er2—O2 | 125.81 (9) |
C15—C14—C13 | 119.9 (5) | O3iv—Er2—O2 | 73.63 (7) |
C15'—C14—C13' | 119.0 (6) | O10v—Er2—O2 | 74.89 (8) |
C15—C14—C13' | 115.3 (6) | O1—Er2—O2 | 53.87 (7) |
C15'—C14—C16 | 120.1 (5) | O11—Er2—C1 | 163.29 (9) |
C15—C14—C16 | 120.5 (4) | O6—Er2—C1 | 81.38 (9) |
C13—C14—C16 | 119.0 (4) | O8i—Er2—C1 | 101.46 (9) |
C13'—C14—C16 | 119.8 (5) | O3iv—Er2—C1 | 100.30 (8) |
C14—C15—C10 | 120.1 (6) | O10v—Er2—C1 | 77.99 (8) |
C14—C15—H15 | 119.9 | O1—Er2—C1 | 27.23 (8) |
C10—C15—H15 | 119.9 | O2—Er2—C1 | 26.69 (8) |
C13'—C12'—C11' | 119.8 (10) | C1—O1—Er2 | 93.85 (17) |
C13'—C12'—H12' | 120.1 | C1—O2—Er2 | 92.22 (18) |
C11'—C12'—H12' | 120.1 | C8—O3—Er2iv | 134.08 (18) |
C12'—C13'—C14 | 121.1 (8) | C8—O4—Er1vi | 142.64 (19) |
C12'—C13'—H13' | 119.5 | C9—O5—Er1 | 169.8 (2) |
C14—C13'—H13' | 119.5 | C9—O6—Er2 | 140.3 (2) |
C12'—C11'—C10 | 119.8 (9) | C16—O7—Er1vii | 153.1 (2) |
C12'—C11'—H11' | 120.1 | C16—O8—Er2vii | 139.5 (2) |
O8—C16—O7 | 124.1 (3) | C24—O9—Er1 | 148.6 (2) |
O8—C16—C14 | 118.5 (3) | C24—O10—Er2iii | 110.14 (18) |
O7—C16—C14 | 117.3 (3) | C17—O11—Er2 | 158.2 (2) |
O11—C17—O12 | 123.3 (3) | C17—O12—Er1v | 125.5 (2) |
O11—C17—C18 | 119.3 (3) | Er1—O2W—H3W | 123 (3) |
O12—C17—C18 | 117.4 (3) | Er1—O2W—H4W | 124 (3) |
C19—C18—C23 | 119.3 (3) | H3W—O2W—H4W | 100 (4) |
C19—C18—C17 | 120.6 (3) | Er1—O3W—H5W | 121 (3) |
C23—C18—C17 | 120.1 (3) | Er1—O3W—H6W | 122 (4) |
C20—C19—C18 | 120.7 (3) | H5W—O3W—H6W | 113 (5) |
C20—C19—H19 | 119.6 | H1WA—O1WA—H2WA | 92 (5) |
C18—C19—H19 | 119.6 | H2WA—O1WA—H1WB | 92 (5) |
C19—C20—C21 | 119.7 (3) | H1WA—O1WA—H2WB | 92 (5) |
C19—C20—H20 | 120.1 | H1WB—O1WA—H2WB | 92 (5) |
C21—C20—H20 | 120.1 | H1WA—O1WB—H2WA | 93 (5) |
C20—C21—C22 | 120.0 (3) | H2WA—O1WB—H1WB | 93 (5) |
C20—C21—H21 | 120.0 | H1WA—O1WB—H2WB | 93 (5) |
C22—C21—H21 | 120.0 | H1WB—O1WB—H2WB | 93 (5) |
Symmetry codes: (i) x, −y+3/2, z−1/2; (ii) x−1, −y+3/2, z−1/2; (iii) −x, y−1/2, −z+1/2; (iv) −x+1, −y+2, −z+1; (v) −x, y+1/2, −z+1/2; (vi) x+1, −y+3/2, z+1/2; (vii) x, −y+3/2, z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1WB—H2WB···O12iii | 0.82 (1) | 2.54 (5) | 3.019 (7) | 118 (5) |
O1WB—H1WB···O10viii | 0.81 (1) | 2.07 (2) | 2.709 (6) | 135 (3) |
O3W—H6W···O1WB | 0.82 (1) | 2.00 (3) | 2.742 (7) | 150 (5) |
O2W—H3W···O1WB | 0.82 (1) | 2.13 (3) | 2.837 (8) | 144 (4) |
O2W—H4W···O3ix | 0.82 (1) | 2.00 (1) | 2.820 (3) | 176 (5) |
O1WA—H2WA···O12iii | 0.82 (1) | 2.54 (5) | 3.087 (14) | 125 (5) |
O1WA—H1WA···O10viii | 0.83 (1) | 2.07 (2) | 2.862 (14) | 160 (4) |
O3W—H6W···O1WA | 0.82 (1) | 1.93 (3) | 2.702 (14) | 157 (5) |
O2W—H3W···O1WA | 0.82 (1) | 2.80 (4) | 3.429 (16) | 135 (4) |
O3W—H5W···O1 | 0.82 (1) | 1.88 (1) | 2.692 (3) | 170 (5) |
Symmetry codes: (iii) −x, y−1/2, −z+1/2; (viii) x+1, y, z; (ix) −x+1, y−1/2, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [Er2(C8H4O4)3(H2O)2]·H2O |
Mr | 880.90 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 293 |
a, b, c (Å) | 10.5553 (2), 14.9526 (3), 17.4798 (3) |
β (°) | 103.908 (1) |
V (Å3) | 2677.94 (9) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 6.30 |
Crystal size (mm) | 0.25 × 0.19 × 0.16 |
Data collection | |
Diffractometer | Bruker APEXII area-detector |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.248, 0.369 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 33045, 6127, 5579 |
Rint | 0.028 |
(sin θ/λ)max (Å−1) | 0.649 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.019, 0.045, 1.06 |
No. of reflections | 6127 |
No. of parameters | 429 |
No. of restraints | 68 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.74, −0.75 |
Computer programs: APEX2 (Bruker, 2004), SAINT (Bruker, 2004), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 2004).
D—H···A | D—H | H···A | D···A | D—H···A |
O1WB—H2WB···O12i | 0.817 (10) | 2.54 (5) | 3.019 (7) | 118 (5) |
O1WB—H1WB···O10ii | 0.813 (10) | 2.071 (19) | 2.709 (6) | 135 (3) |
O3W—H6W···O1WB | 0.822 (10) | 2.00 (3) | 2.742 (7) | 150 (5) |
O2W—H3W···O1WB | 0.817 (10) | 2.13 (3) | 2.837 (8) | 144 (4) |
O2W—H4W···O3iii | 0.819 (10) | 2.002 (11) | 2.820 (3) | 176 (5) |
O1WA—H2WA···O12i | 0.822 (10) | 2.54 (5) | 3.087 (14) | 125 (5) |
O1WA—H1WA···O10ii | 0.825 (10) | 2.071 (19) | 2.862 (14) | 160 (4) |
O3W—H6W···O1WA | 0.822 (10) | 1.93 (3) | 2.702 (14) | 157 (5) |
O2W—H3W···O1WA | 0.817 (10) | 2.80 (4) | 3.429 (16) | 135 (4) |
O3W—H5W···O1 | 0.819 (10) | 1.881 (14) | 2.692 (3) | 170 (5) |
Symmetry codes: (i) −x, y−1/2, −z+1/2; (ii) x+1, y, z; (iii) −x+1, y−1/2, −z+1/2. |
As a building block, benzene-1,3-dicarboxylic acid (1,3-BDC) is an excellent candidate for the construction of supramolecular complexes (Bourne et al., 2001; Zhang et al., 2003). Recently, we obtained the title coordination polymer by the reaction of ErCl3 with benzene-1,3-dicarboxylic acid in alkaline aqueous solution, and its crystal structure is reported here.
Each of the two crystallographically independent ErIII centres is seven-coordinate and has a distorted pentagonal bipyramidal geometry: one Er centre is coordinated by seven oxygen atoms from six 1,3-BDC ligands, and the other Er centre is surrounded by five oxygen atoms from five 1,3-BDC ligands and two water molecules (Fig. 1). The adjacent Er···Er separations are 4.448 (4) and 4.965 (5) Å, respectively. The dianionic ligands cross-link the metal ions to form a three-dimensional network with channels running along the c axis hosting an uncoordinated disordered water molecule (Fig. 2). The title compound exhibits two types of large voids that seem to be partially filled by diffuse solvent (no corrections for this were applied to the dataset). The larger of the voids has a volume of of 142.3 Å3 (5.3% of the unit cell volume) and is located in close proximity to a disordered phenyl ring of one of the 1,3-BDC ligands. The large void thus gives the phenyl ring additional degrees of freedom which can be seen as a likely cause of the disorder of the phenyl ring. The second type of void in the structure (75.6 Å3, 2.8% of the unit cell volume) is located close to the disordered water solvate molecule (see refinement section for details). These water molecules are hydrogen bonded to coordinated water molecules and carboxylate units that all form a hydrogen bonded chain parallel to the b axis (Table 1).