Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807057765/zl2078sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807057765/zl2078Isup2.hkl |
CCDC reference: 672726
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean (C-C) = 0.009 Å
- Disorder in main residue
- R factor = 0.034
- wR factor = 0.073
- Data-to-parameter ratio = 12.6
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT420_ALERT_2_B D-H Without Acceptor O2W - H4W ... ? PLAT731_ALERT_1_B Bond Calc 0.83(5), Rep 0.818(10) ...... 5.00 su-Ra O1W -H1W 1.555 1.555 PLAT731_ALERT_1_B Bond Calc 0.81(7), Rep 0.819(10) ...... 7.00 su-Ra O1W -H2W 1.555 1.555 PLAT731_ALERT_1_B Bond Calc 0.83(5), Rep 0.823(10) ...... 5.00 su-Ra O2W -H3W 1.555 1.555 PLAT731_ALERT_1_B Bond Calc 0.83(5), Rep 0.822(10) ...... 5.00 su-Ra O2W -H4W 1.555 1.555 PLAT732_ALERT_1_B Angle Calc 105(8), Rep 104.0(17) ...... 4.71 su-Ra H1W -O1W -H2W 1.555 1.555 1.555 PLAT735_ALERT_1_B D-H Calc 0.83(5), Rep 0.818(10) ...... 5.00 su-Ra O1W -H1W 1.555 1.555 PLAT735_ALERT_1_B D-H Calc 0.81(7), Rep 0.819(10) ...... 7.00 su-Ra O1W -H2W 1.555 1.555 PLAT735_ALERT_1_B D-H Calc 0.83(5), Rep 0.823(10) ...... 5.00 su-Ra O2W -H3W 1.555 1.555
Alert level C PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.05 PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT153_ALERT_1_C The su's on the Cell Axes are Equal (x 100000) 30 Ang. PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.40 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O5 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Tb1 PLAT301_ALERT_3_C Main Residue Disorder ......................... 9.00 Perc. PLAT342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 10 PLAT732_ALERT_1_C Angle Calc 103(5), Rep 103.3(17) ...... 2.94 su-Ra H3W -O2W -H4W 1.555 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 1.95(5), Rep 1.959(14) ...... 3.57 su-Ra H3W -O2 1.555 3.755 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.14 Ratio
Alert level G PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 66
0 ALERT level A = In general: serious problem 9 ALERT level B = Potentially serious problem 11 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 12 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 4 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
De Bettencourt-Dias (2005) and Zhang et al. (2003) have described the use of benzene-1,3-dicarboxylic acid (1,3-BDC) in the construction of supramolecular complexes.
A mixture of Tb(NO3)3 (0.5 mmol, 0.172 g), benzenedicarboxylic acid (0.75 mmol, 0.125 g), NaOH (1.5 mmol; 0.06 g) and H2O (12 ml) was placed in a 23 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.
One of the phenyl rings was found to be split into two positions and the occupancy ratio refined to 0.60 (3) to 0.40 (3). Due to the significant overlap of the disordered atoms the following restraints were applied: The phenyl ring C10 C11 C12 C13 C14 C15 and its disordered counterpart were each restrained to be flat and their 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) = 1.5 Ueq(O). 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) = 1.2 Ueq(C).
Data collection: APEX-II (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-XP (Bruker, 2004); software used to prepare material for publication: SHELXTL (Bruker, 2004).
[Tb2(C8H4O4)3(H2O)2] | F(000) = 1608 |
Mr = 846.21 | Dx = 2.245 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 4289 reflections |
a = 13.2647 (3) Å | θ = 1.7–28.0° |
b = 14.3741 (3) Å | µ = 5.68 mm−1 |
c = 13.5323 (3) Å | T = 296 K |
β = 103.944 (1)° | Block, colorless |
V = 2504.14 (9) Å3 | 0.15 × 0.14 × 0.11 mm |
Z = 4 |
Bruker APEX-II area-detector diffractometer | 5182 independent reflections |
Radiation source: fine-focus sealed tube | 3834 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.077 |
ϕ and ω scan | θmax = 26.5°, θmin = 1.9° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −16→16 |
Tmin = 0.445, Tmax = 0.538 | k = −17→18 |
35926 measured reflections | l = −16→16 |
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)] = 0.034 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.073 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0245P)2 + 8.8675P] where P = (Fo2 + 2Fc2)/3 |
5182 reflections | (Δ/σ)max = 0.001 |
410 parameters | Δρmax = 2.21 e Å−3 |
66 restraints | Δρmin = −1.08 e Å−3 |
[Tb2(C8H4O4)3(H2O)2] | V = 2504.14 (9) Å3 |
Mr = 846.21 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 13.2647 (3) Å | µ = 5.68 mm−1 |
b = 14.3741 (3) Å | T = 296 K |
c = 13.5323 (3) Å | 0.15 × 0.14 × 0.11 mm |
β = 103.944 (1)° |
Bruker APEX-II area-detector diffractometer | 5182 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 3834 reflections with I > 2σ(I) |
Tmin = 0.445, Tmax = 0.538 | Rint = 0.077 |
35926 measured reflections |
R[F2 > 2σ(F2)] = 0.034 | 66 restraints |
wR(F2) = 0.073 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.02 | Δρmax = 2.21 e Å−3 |
5182 reflections | Δρmin = −1.08 e Å−3 |
410 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 | 0.8731 (5) | 0.1394 (4) | 0.1428 (4) | 0.0231 (14) | |
C2 | 0.9120 (5) | 0.2379 (4) | 0.1428 (5) | 0.0273 (15) | |
C3 | 0.8840 (5) | 0.3000 (4) | 0.2099 (5) | 0.0292 (15) | |
H3 | 0.8430 | 0.2801 | 0.2528 | 0.035* | |
C4 | 0.9166 (5) | 0.3912 (4) | 0.2132 (5) | 0.0285 (15) | |
C5 | 0.9762 (6) | 0.4214 (5) | 0.1484 (6) | 0.0418 (19) | |
H5 | 0.9974 | 0.4832 | 0.1498 | 0.050* | |
C6 | 1.0044 (7) | 0.3588 (5) | 0.0808 (6) | 0.051 (2) | |
H6 | 1.0443 | 0.3788 | 0.0370 | 0.061* | |
C7 | 0.9728 (6) | 0.2667 (5) | 0.0792 (6) | 0.0382 (18) | |
H7 | 0.9925 | 0.2245 | 0.0353 | 0.046* | |
C8 | 0.8853 (5) | 0.4571 (4) | 0.2847 (5) | 0.0272 (15) | |
C9 | 0.6369 (6) | 0.4092 (5) | 0.1246 (5) | 0.0339 (17) | |
C10 | 0.6583 (6) | 0.4838 (5) | 0.0566 (5) | 0.0377 (18) | |
C11 | 0.6834 (13) | 0.5728 (7) | 0.0950 (9) | 0.021 (7) | 0.40 (3) |
H11 | 0.6739 | 0.5890 | 0.1587 | 0.025* | 0.40 (3) |
C13 | 0.738 (2) | 0.6150 (13) | −0.0580 (11) | 0.026 (5) | 0.40 (3) |
H13 | 0.7678 | 0.6582 | −0.0932 | 0.032* | 0.40 (3) |
C14 | 0.708 (3) | 0.5288 (13) | −0.1007 (15) | 0.041 (6) | 0.40 (3) |
H14 | 0.7083 | 0.5155 | −0.1677 | 0.049* | 0.40 (3) |
C15 | 0.677 (2) | 0.4638 (14) | −0.0398 (12) | 0.039 (6) | 0.40 (3) |
H15 | 0.6670 | 0.4029 | −0.0634 | 0.047* | 0.40 (3) |
C11' | 0.7033 (11) | 0.5661 (6) | 0.1000 (7) | 0.022 (4) | 0.60 (3) |
H11' | 0.7203 | 0.5736 | 0.1703 | 0.026* | 0.60 (3) |
C13' | 0.6938 (16) | 0.6260 (9) | −0.0677 (7) | 0.033 (4) | 0.60 (3) |
H13' | 0.7037 | 0.6746 | −0.1097 | 0.040* | 0.60 (3) |
C14' | 0.6506 (17) | 0.5431 (9) | −0.1100 (10) | 0.039 (4) | 0.60 (3) |
H14' | 0.6362 | 0.5353 | −0.1802 | 0.047* | 0.60 (3) |
C15' | 0.6286 (15) | 0.4723 (9) | −0.0504 (7) | 0.033 (4) | 0.60 (3) |
H15' | 0.5952 | 0.4185 | −0.0795 | 0.040* | 0.60 (3) |
C12 | 0.7224 (5) | 0.6369 (4) | 0.0379 (5) | 0.0312 (16) | |
C16 | 0.7631 (5) | 0.7280 (4) | 0.0848 (5) | 0.0226 (14) | |
C17 | 0.6837 (5) | 0.0910 (4) | −0.0429 (4) | 0.0225 (14) | |
C18 | 0.7180 (5) | 0.1586 (4) | −0.1142 (5) | 0.0258 (15) | |
C19 | 0.6553 (6) | 0.2320 (5) | −0.1574 (5) | 0.0332 (16) | |
H19 | 0.5897 | 0.2385 | −0.1450 | 0.040* | |
C20 | 0.6886 (6) | 0.2954 (5) | −0.2183 (5) | 0.0378 (18) | |
H20 | 0.6445 | 0.3427 | −0.2497 | 0.045* | |
C21 | 0.7881 (5) | 0.2886 (5) | −0.2329 (5) | 0.0341 (17) | |
H21 | 0.8119 | 0.3332 | −0.2716 | 0.041* | |
C22 | 0.8525 (5) | 0.2159 (4) | −0.1901 (5) | 0.0270 (15) | |
C23 | 0.8166 (5) | 0.1504 (5) | −0.1316 (4) | 0.0256 (15) | |
H23 | 0.8589 | 0.1006 | −0.1038 | 0.031* | |
C24 | 0.9607 (5) | 0.2067 (5) | −0.2044 (5) | 0.0279 (15) | |
O1 | 0.7873 (3) | 0.1236 (3) | 0.1631 (3) | 0.0279 (10) | |
O2 | 0.9288 (4) | 0.0743 (3) | 0.1211 (4) | 0.0335 (11) | |
O3 | 0.9080 (4) | 0.5415 (3) | 0.2778 (4) | 0.0390 (12) | |
O4 | 0.8359 (4) | 0.4262 (3) | 0.3473 (4) | 0.0364 (12) | |
O5 | 0.6263 (4) | 0.3265 (3) | 0.0916 (4) | 0.0436 (13) | |
O6 | 0.6325 (4) | 0.4317 (3) | 0.2125 (4) | 0.0423 (13) | |
O7 | 0.7630 (3) | 0.7967 (3) | 0.0277 (3) | 0.0290 (11) | |
O8 | 0.7966 (4) | 0.7328 (3) | 0.1800 (3) | 0.0311 (11) | |
O9 | 0.6139 (3) | 0.1186 (3) | −0.0012 (3) | 0.0301 (11) | |
O10 | 0.7277 (3) | 0.0131 (3) | −0.0287 (3) | 0.0275 (10) | |
O11 | 1.0184 (4) | 0.1465 (3) | −0.1523 (3) | 0.0329 (11) | |
O12 | 0.9859 (4) | 0.2601 (3) | −0.2675 (4) | 0.0360 (12) | |
O1W | 0.4451 (4) | 0.1564 (5) | 0.0500 (4) | 0.0564 (17) | |
H1W | 0.387 (3) | 0.178 (6) | 0.048 (6) | 0.085* | |
H2W | 0.436 (6) | 0.121 (5) | 0.002 (5) | 0.085* | |
O2W | 0.8967 (4) | −0.0717 (4) | −0.0413 (4) | 0.0432 (13) | |
H3W | 0.948 (3) | −0.075 (6) | −0.066 (5) | 0.065* | |
H4W | 0.849 (3) | −0.059 (6) | −0.091 (3) | 0.065* | |
Tb1 | 0.61128 (2) | 0.18274 (2) | 0.15619 (2) | 0.02036 (8) | |
Tb2 | 0.82716 (2) | −0.06625 (2) | 0.11562 (2) | 0.02429 (9) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.022 (4) | 0.025 (3) | 0.022 (3) | 0.002 (3) | 0.004 (3) | −0.006 (3) |
C2 | 0.026 (4) | 0.023 (4) | 0.035 (4) | −0.004 (3) | 0.011 (3) | −0.002 (3) |
C3 | 0.029 (4) | 0.025 (4) | 0.036 (4) | −0.004 (3) | 0.013 (3) | −0.010 (3) |
C4 | 0.027 (4) | 0.021 (3) | 0.041 (4) | 0.001 (3) | 0.016 (3) | −0.004 (3) |
C5 | 0.058 (5) | 0.017 (4) | 0.058 (5) | −0.009 (4) | 0.031 (4) | −0.006 (3) |
C6 | 0.066 (6) | 0.034 (5) | 0.069 (6) | −0.012 (4) | 0.051 (5) | −0.008 (4) |
C7 | 0.046 (5) | 0.029 (4) | 0.048 (4) | −0.001 (3) | 0.028 (4) | −0.008 (3) |
C8 | 0.021 (4) | 0.024 (4) | 0.039 (4) | 0.000 (3) | 0.012 (3) | −0.007 (3) |
C9 | 0.039 (5) | 0.030 (4) | 0.031 (4) | −0.005 (3) | 0.003 (3) | 0.008 (3) |
C10 | 0.053 (5) | 0.024 (4) | 0.034 (4) | −0.010 (3) | 0.007 (4) | 0.005 (3) |
C11 | 0.013 (8) | 0.018 (9) | 0.026 (10) | 0.006 (7) | −0.006 (6) | −0.001 (7) |
C13 | 0.028 (10) | 0.020 (8) | 0.031 (8) | 0.002 (7) | 0.008 (7) | −0.002 (6) |
C14 | 0.055 (11) | 0.040 (9) | 0.030 (8) | 0.003 (8) | 0.016 (8) | −0.009 (7) |
C15 | 0.040 (11) | 0.033 (9) | 0.046 (9) | −0.007 (8) | 0.012 (7) | −0.006 (7) |
C11' | 0.028 (7) | 0.019 (7) | 0.019 (6) | 0.001 (5) | 0.006 (5) | 0.004 (5) |
C13' | 0.039 (8) | 0.025 (6) | 0.032 (6) | −0.001 (6) | 0.001 (5) | 0.004 (5) |
C14' | 0.050 (9) | 0.033 (7) | 0.032 (6) | −0.005 (6) | 0.006 (6) | 0.001 (5) |
C15' | 0.034 (8) | 0.027 (6) | 0.038 (6) | −0.009 (6) | 0.006 (5) | −0.003 (5) |
C12 | 0.042 (4) | 0.022 (4) | 0.029 (4) | −0.004 (3) | 0.007 (3) | 0.001 (3) |
C16 | 0.016 (3) | 0.024 (4) | 0.028 (3) | −0.002 (3) | 0.005 (3) | −0.002 (3) |
C17 | 0.015 (3) | 0.030 (4) | 0.022 (3) | −0.003 (3) | 0.003 (3) | −0.001 (3) |
C18 | 0.024 (4) | 0.026 (4) | 0.030 (3) | −0.003 (3) | 0.012 (3) | −0.002 (3) |
C19 | 0.024 (4) | 0.038 (4) | 0.038 (4) | 0.007 (3) | 0.010 (3) | 0.001 (3) |
C20 | 0.031 (4) | 0.034 (4) | 0.049 (4) | 0.011 (3) | 0.010 (3) | 0.010 (3) |
C21 | 0.032 (4) | 0.030 (4) | 0.042 (4) | 0.006 (3) | 0.014 (3) | 0.007 (3) |
C22 | 0.026 (4) | 0.025 (4) | 0.032 (4) | 0.005 (3) | 0.013 (3) | 0.003 (3) |
C23 | 0.025 (4) | 0.031 (4) | 0.023 (3) | 0.000 (3) | 0.009 (3) | 0.002 (3) |
C24 | 0.027 (4) | 0.030 (4) | 0.028 (3) | 0.004 (3) | 0.009 (3) | 0.007 (3) |
O1 | 0.021 (3) | 0.031 (3) | 0.033 (3) | −0.006 (2) | 0.010 (2) | −0.006 (2) |
O2 | 0.029 (3) | 0.022 (3) | 0.052 (3) | −0.002 (2) | 0.015 (2) | −0.009 (2) |
O3 | 0.051 (3) | 0.021 (3) | 0.050 (3) | −0.003 (2) | 0.023 (3) | −0.009 (2) |
O4 | 0.040 (3) | 0.026 (3) | 0.049 (3) | −0.004 (2) | 0.023 (2) | −0.009 (2) |
O5 | 0.063 (4) | 0.020 (3) | 0.048 (3) | −0.010 (2) | 0.014 (3) | 0.005 (2) |
O6 | 0.063 (4) | 0.028 (3) | 0.036 (3) | −0.016 (3) | 0.011 (2) | 0.006 (2) |
O7 | 0.036 (3) | 0.017 (2) | 0.033 (2) | −0.004 (2) | 0.008 (2) | 0.0023 (19) |
O8 | 0.030 (3) | 0.035 (3) | 0.028 (2) | −0.004 (2) | 0.008 (2) | −0.004 (2) |
O9 | 0.028 (3) | 0.037 (3) | 0.029 (2) | 0.002 (2) | 0.013 (2) | −0.001 (2) |
O10 | 0.029 (3) | 0.025 (3) | 0.034 (3) | 0.004 (2) | 0.017 (2) | 0.003 (2) |
O11 | 0.028 (3) | 0.034 (3) | 0.041 (3) | 0.002 (2) | 0.018 (2) | 0.009 (2) |
O12 | 0.029 (3) | 0.041 (3) | 0.043 (3) | 0.003 (2) | 0.019 (2) | 0.016 (2) |
O1W | 0.023 (3) | 0.088 (5) | 0.055 (4) | 0.007 (3) | 0.003 (3) | −0.038 (3) |
O2W | 0.043 (3) | 0.049 (3) | 0.045 (3) | 0.006 (3) | 0.025 (2) | 0.003 (3) |
Tb1 | 0.02051 (17) | 0.01598 (16) | 0.02636 (16) | −0.00013 (13) | 0.00914 (12) | −0.00032 (12) |
Tb2 | 0.02325 (18) | 0.01728 (16) | 0.03264 (18) | −0.00032 (13) | 0.00735 (13) | 0.00021 (13) |
C1—O1 | 1.255 (7) | C17—O10 | 1.256 (7) |
C1—O2 | 1.269 (7) | C17—O9 | 1.259 (7) |
C1—C2 | 1.507 (9) | C17—C18 | 1.515 (8) |
C2—C7 | 1.377 (9) | C18—C19 | 1.383 (9) |
C2—C3 | 1.387 (9) | C18—C23 | 1.388 (9) |
C3—C4 | 1.378 (9) | C19—C20 | 1.371 (10) |
C3—H3 | 0.9300 | C19—H19 | 0.9300 |
C4—C5 | 1.385 (9) | C20—C21 | 1.384 (10) |
C4—C8 | 1.483 (9) | C20—H20 | 0.9300 |
C5—C6 | 1.397 (10) | C21—C22 | 1.385 (9) |
C5—H5 | 0.9300 | C21—H21 | 0.9300 |
C6—C7 | 1.388 (10) | C22—C23 | 1.386 (9) |
C6—H6 | 0.9300 | C22—C24 | 1.500 (9) |
C7—H7 | 0.9300 | C23—H23 | 0.9300 |
C8—O3 | 1.259 (7) | C24—O12 | 1.251 (7) |
C8—O4 | 1.269 (8) | C24—O11 | 1.254 (7) |
C9—O6 | 1.248 (8) | O1—Tb1 | 2.465 (4) |
C9—O5 | 1.265 (8) | O1—Tb2 | 2.882 (4) |
C9—C10 | 1.484 (9) | O2—Tb2 | 2.420 (4) |
C10—C11' | 1.390 (10) | O3—Tb1i | 2.258 (4) |
C10—C11 | 1.390 (11) | O4—Tb2i | 2.338 (5) |
C10—C15 | 1.413 (13) | O5—Tb1 | 2.271 (4) |
C10—C15' | 1.417 (11) | O6—Tb2i | 2.258 (5) |
C11—C12 | 1.382 (11) | O7—Tb2ii | 2.352 (4) |
C11—H11 | 0.9300 | O8—Tb1i | 2.370 (4) |
C13—C14 | 1.384 (13) | O9—Tb1 | 2.329 (4) |
C13—C12 | 1.396 (12) | O10—Tb2 | 2.369 (4) |
C13—H13 | 0.9300 | O11—Tb2iii | 2.299 (5) |
C14—C15 | 1.372 (14) | O12—Tb1iv | 2.310 (4) |
C14—H14 | 0.9300 | O1W—Tb1 | 2.354 (5) |
C15—H15 | 0.9300 | O1W—H1W | 0.818 (10) |
C11'—C12 | 1.381 (10) | O1W—H2W | 0.819 (10) |
C11'—H11' | 0.9300 | O2W—Tb2 | 2.513 (5) |
C13'—C14' | 1.385 (12) | O2W—H3W | 0.823 (10) |
C13'—C12 | 1.395 (11) | O2W—H4W | 0.822 (10) |
C13'—H13' | 0.9300 | Tb1—O3v | 2.258 (4) |
C14'—C15' | 1.373 (13) | Tb1—O12vi | 2.310 (4) |
C14'—H14' | 0.9300 | Tb1—O8v | 2.370 (4) |
C15'—H15' | 0.9300 | Tb2—O6v | 2.258 (5) |
C12—C16 | 1.499 (9) | Tb2—O11iii | 2.299 (5) |
C16—O7 | 1.253 (7) | Tb2—O4v | 2.338 (5) |
C16—O8 | 1.260 (7) | Tb2—O7vii | 2.352 (4) |
O1—C1—O2 | 121.8 (6) | C20—C21—C22 | 120.4 (7) |
O1—C1—C2 | 119.9 (6) | C20—C21—H21 | 119.8 |
O2—C1—C2 | 118.3 (6) | C22—C21—H21 | 119.8 |
C7—C2—C3 | 120.4 (6) | C21—C22—C23 | 119.4 (6) |
C7—C2—C1 | 122.3 (6) | C21—C22—C24 | 121.6 (6) |
C3—C2—C1 | 117.3 (6) | C23—C22—C24 | 119.0 (6) |
C4—C3—C2 | 120.1 (6) | C22—C23—C18 | 120.4 (6) |
C4—C3—H3 | 119.9 | C22—C23—H23 | 119.8 |
C2—C3—H3 | 119.9 | C18—C23—H23 | 119.8 |
C3—C4—C5 | 120.0 (6) | O12—C24—O11 | 125.5 (6) |
C3—C4—C8 | 119.5 (6) | O12—C24—C22 | 117.1 (6) |
C5—C4—C8 | 120.4 (6) | O11—C24—C22 | 117.4 (6) |
C4—C5—C6 | 119.8 (6) | C1—O1—Tb1 | 146.1 (4) |
C4—C5—H5 | 120.1 | C1—O1—Tb2 | 84.1 (4) |
C6—C5—H5 | 120.1 | Tb1—O1—Tb2 | 122.75 (16) |
C7—C6—C5 | 119.8 (7) | C1—O2—Tb2 | 105.8 (4) |
C7—C6—H6 | 120.1 | C8—O3—Tb1i | 141.7 (5) |
C5—C6—H6 | 120.1 | C8—O4—Tb2i | 141.2 (4) |
C2—C7—C6 | 119.8 (7) | C9—O5—Tb1 | 137.0 (5) |
C2—C7—H7 | 120.1 | C9—O6—Tb2i | 158.7 (5) |
C6—C7—H7 | 120.1 | C16—O7—Tb2ii | 113.7 (4) |
O3—C8—O4 | 123.9 (6) | C16—O8—Tb1i | 156.2 (4) |
O3—C8—C4 | 117.2 (6) | C17—O9—Tb1 | 135.2 (4) |
O4—C8—C4 | 118.9 (6) | C17—O10—Tb2 | 134.5 (4) |
O6—C9—O5 | 123.6 (6) | C24—O11—Tb2iii | 149.2 (4) |
O6—C9—C10 | 117.6 (6) | C24—O12—Tb1iv | 149.6 (4) |
O5—C9—C10 | 118.8 (6) | Tb1—O1W—H1W | 134 (5) |
C11'—C10—C15 | 114.3 (11) | Tb1—O1W—H2W | 122 (5) |
C11—C10—C15 | 117.0 (11) | H1W—O1W—H2W | 104.0 (17) |
C11'—C10—C15' | 121.1 (8) | Tb2—O2W—H3W | 148 (5) |
C11—C10—C15' | 118.2 (8) | Tb2—O2W—H4W | 108 (5) |
C11'—C10—C9 | 118.7 (7) | H3W—O2W—H4W | 103.3 (17) |
C11—C10—C9 | 119.9 (7) | O3v—Tb1—O5 | 178.18 (19) |
C15—C10—C9 | 121.7 (10) | O3v—Tb1—O12vi | 88.87 (17) |
C15'—C10—C9 | 120.1 (7) | O5—Tb1—O12vi | 89.33 (18) |
C12—C11—C10 | 119.5 (9) | O3v—Tb1—O9 | 91.95 (17) |
C12—C11—H11 | 120.3 | O5—Tb1—O9 | 89.20 (17) |
C10—C11—H11 | 120.3 | O12vi—Tb1—O9 | 136.12 (16) |
C14—C13—C12 | 119.9 (15) | O3v—Tb1—O1W | 85.3 (2) |
C14—C13—H13 | 120.1 | O5—Tb1—O1W | 93.9 (2) |
C12—C13—H13 | 120.1 | O12vi—Tb1—O1W | 70.16 (17) |
C15—C14—C13 | 117.2 (18) | O9—Tb1—O1W | 66.20 (17) |
C15—C14—H14 | 121.4 | O3v—Tb1—O8v | 89.16 (16) |
C13—C14—H14 | 121.4 | O5—Tb1—O8v | 90.58 (16) |
C14—C15—C10 | 124.0 (17) | O12vi—Tb1—O8v | 74.82 (16) |
C14—C15—H15 | 118.0 | O9—Tb1—O8v | 149.05 (16) |
C10—C15—H15 | 118.0 | O1W—Tb1—O8v | 144.62 (18) |
C12—C11'—C10 | 119.6 (8) | O3v—Tb1—O1 | 82.62 (16) |
C12—C11'—H11' | 120.2 | O5—Tb1—O1 | 99.09 (17) |
C10—C11'—H11' | 120.2 | O12vi—Tb1—O1 | 152.00 (15) |
C14'—C13'—C12 | 120.2 (11) | O9—Tb1—O1 | 71.07 (15) |
C14'—C13'—H13' | 119.9 | O1W—Tb1—O1 | 135.00 (16) |
C12—C13'—H13' | 119.9 | O8v—Tb1—O1 | 78.42 (15) |
C15'—C14'—C13' | 121.4 (12) | O6v—Tb2—O11iii | 78.07 (17) |
C15'—C14'—H14' | 119.3 | O6v—Tb2—O4v | 77.30 (18) |
C13'—C14'—H14' | 119.3 | O11iii—Tb2—O4v | 138.85 (15) |
C14'—C15'—C10 | 117.9 (11) | O6v—Tb2—O7vii | 118.50 (16) |
C14'—C15'—H15' | 121.1 | O11iii—Tb2—O7vii | 83.35 (16) |
C10—C15'—H15' | 121.1 | O4v—Tb2—O7vii | 80.15 (16) |
C11'—C12—C13' | 119.7 (8) | O6v—Tb2—O10 | 143.33 (16) |
C11—C12—C13' | 116.9 (8) | O11iii—Tb2—O10 | 135.23 (15) |
C11'—C12—C13 | 119.2 (10) | O4v—Tb2—O10 | 80.73 (15) |
C11—C12—C13 | 121.8 (10) | O7vii—Tb2—O10 | 85.66 (15) |
C11'—C12—C16 | 119.1 (6) | O6v—Tb2—O2 | 89.27 (17) |
C11—C12—C16 | 119.4 (7) | O11iii—Tb2—O2 | 87.20 (15) |
C13'—C12—C16 | 120.9 (7) | O4v—Tb2—O2 | 124.72 (16) |
C13—C12—C16 | 118.3 (9) | O7vii—Tb2—O2 | 147.76 (15) |
O7—C16—O8 | 122.3 (6) | O10—Tb2—O2 | 79.58 (15) |
O7—C16—C12 | 118.7 (5) | O6v—Tb2—O2W | 145.73 (19) |
O8—C16—C12 | 118.9 (6) | O11iii—Tb2—O2W | 71.18 (17) |
O10—C17—O9 | 125.3 (6) | O4v—Tb2—O2W | 136.65 (17) |
O10—C17—C18 | 118.0 (6) | O7vii—Tb2—O2W | 73.04 (17) |
O9—C17—C18 | 116.7 (6) | O10—Tb2—O2W | 64.10 (16) |
C19—C18—C23 | 119.2 (6) | O2—Tb2—O2W | 74.73 (17) |
C19—C18—C17 | 121.1 (6) | O6v—Tb2—O1 | 78.07 (14) |
C23—C18—C17 | 119.6 (6) | O11iii—Tb2—O1 | 128.96 (14) |
C20—C19—C18 | 120.9 (7) | O4v—Tb2—O1 | 76.53 (14) |
C20—C19—H19 | 119.6 | O7vii—Tb2—O1 | 147.41 (14) |
C18—C19—H19 | 119.6 | O10—Tb2—O1 | 68.43 (13) |
C19—C20—C21 | 119.7 (7) | O2—Tb2—O1 | 48.19 (14) |
C19—C20—H20 | 120.2 | O2W—Tb2—O1 | 110.02 (16) |
C21—C20—H20 | 120.2 |
Symmetry codes: (i) −x+3/2, y+1/2, −z+1/2; (ii) x, y+1, z; (iii) −x+2, −y, −z; (iv) x+1/2, −y+1/2, z−1/2; (v) −x+3/2, y−1/2, −z+1/2; (vi) x−1/2, −y+1/2, z+1/2; (vii) x, y−1, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W···O7viii | 0.82 (1) | 2.04 (4) | 2.789 (7) | 151 (7) |
O1W—H2W···O4ix | 0.82 (1) | 2.29 (4) | 3.020 (7) | 149 (7) |
O2W—H3W···O2iii | 0.82 (1) | 1.96 (1) | 2.780 (7) | 176 (9) |
C3—H3···O8v | 0.93 | 2.35 | 3.257 (8) | 164 |
C11′—H11′···O1i | 0.93 | 2.39 | 3.284 (10) | 161 |
Symmetry codes: (i) −x+3/2, y+1/2, −z+1/2; (iii) −x+2, −y, −z; (v) −x+3/2, y−1/2, −z+1/2; (viii) −x+1, −y+1, −z; (ix) x−1/2, −y+1/2, z−1/2. |
Experimental details
Crystal data | |
Chemical formula | [Tb2(C8H4O4)3(H2O)2] |
Mr | 846.21 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 296 |
a, b, c (Å) | 13.2647 (3), 14.3741 (3), 13.5323 (3) |
β (°) | 103.944 (1) |
V (Å3) | 2504.14 (9) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 5.68 |
Crystal size (mm) | 0.15 × 0.14 × 0.11 |
Data collection | |
Diffractometer | Bruker APEX-II area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.445, 0.538 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 35926, 5182, 3834 |
Rint | 0.077 |
(sin θ/λ)max (Å−1) | 0.628 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.034, 0.073, 1.02 |
No. of reflections | 5182 |
No. of parameters | 410 |
No. of restraints | 66 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 2.21, −1.08 |
Computer programs: APEX-II (Bruker, 2004), SAINT (Bruker, 2004), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL-XP (Bruker, 2004), SHELXTL (Bruker, 2004).
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W···O7i | 0.818 (10) | 2.04 (4) | 2.789 (7) | 151 (7) |
O1W—H2W···O4ii | 0.819 (10) | 2.29 (4) | 3.020 (7) | 149 (7) |
O2W—H3W···O2iii | 0.823 (10) | 1.959 (14) | 2.780 (7) | 176 (9) |
C3—H3···O8iv | 0.93 | 2.35 | 3.257 (8) | 164.3 |
C11'—H11'···O1v | 0.93 | 2.39 | 3.284 (10) | 160.8 |
Symmetry codes: (i) −x+1, −y+1, −z; (ii) x−1/2, −y+1/2, z−1/2; (iii) −x+2, −y, −z; (iv) −x+3/2, y−1/2, −z+1/2; (v) −x+3/2, y+1/2, −z+1/2. |
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As a building block, benzene-1,3-dicarboxylic acid (1,3-BDC) is an excellent candidate for the construction of supramolecular complexes (De Bettencourt-Dias, 2005; Zhang et al., 2003). Recently, we obtained the title coordination polymer by the reaction of Tb(NO3)3 with benzene-1,3-dicarboxylic acid in alkaline aqueous solution, and its crystal structure is reported here.
In the asymmetric unit of the title complex, there are two crystallographically independent TbIII ions: one seven-coordinate Tb centre is coordinated by six oxygen atoms from six 1,3-BDC ligands and one water molecule, and the other Tb centre is eight-coordinate and surrounded by seven oxygen atoms from six 1,3-BDC ligands and one water molecules (Fig. 1). The adjacent Tb···Tb separations are 4.690 (4) and 4.698 (5) Å, respectively. The carboxylate groups of 1,3-BDC ligands are distinct, one of which acts as bis(monodentate) bridge, the other acts as chelate and monodentate bridge. They cross-link the metal ions to form a three-dimensional network (Fig. 2). The crystal structure is stabilized by intra/intermolecular O—H···O and C—H···.O hydrogen bonding interactions (Table 1).