metal-organic compounds
Poly[bis(μ4-benzene-1,4-dicarboxylato)(μ4-succinato)diterbium(III)]
aDepartment of Chemistry, College of Chemistry and Biology, Beihua University, Jilin City 132013, People's Republic of China
*Correspondence e-mail: jlschy@126.com
In the title compound, [Tb2(C4H4O4)(C8H4O4)2]n, the coordination around each Tb atom is distorted square-antiprismatic. The benzene-1,4-dicarboxylate and succinate anions bridge the antiprisms, forming a three-dimensional network. The succinate anion is located on a centre of inversion. The structure is isomorphous with the Dy, Gd, Er and Nd complexes.
Experimental
Crystal data
|
Data collection: PROCESS-AUTO (Rigaku, 1998); cell PROCESS-AUTO; data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL-Plus (Sheldrick, 2008); software used to prepare material for publication: SHELXL97.
Supporting information
10.1107/S1600536808011355/bt2699sup1.cif
contains datablocks global, I. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536808011355/bt2699Isup2.hkl
A mixture of 1,4-H2bdc (0.5 mmol), H2suc (0.5 mmol), NaOH (1 mmol) and TbCl3.6H2O (0.5 mmol) was suspended in 12 ml of deionized water and sealed in a 20-ml Teflon-lined autoclave. Upon heating at 185°C for ten days, the autoclave was slowly cooled to room temperature. The crystals were collected, washed with deionized water and dried.
H atoms bonded to C atom were positioned geometrically (C—H = 0.93 Å) and refined as riding, with Uiso(H)=1.2Ueq(carrier).
Data collection: PROCESS-AUTO (Rigaku, 1998); cell
PROCESS-AUTO (Rigaku, 1998); data reduction: PROCESS-AUTO (Rigaku, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL-Plus (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).[Tb2(C4H4O4)(C8H4O4)2] | F(000) = 1432 |
Mr = 381.07 | Dx = 2.418 Mg m−3 |
Orthorhombic, Pbca | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2ab | Cell parameters from 15551 reflections |
a = 13.948 (3) Å | θ = 3.0–27.5° |
b = 6.8724 (14) Å | µ = 6.77 mm−1 |
c = 21.844 (4) Å | T = 293 K |
V = 2093.9 (7) Å3 | Block, colorless |
Z = 8 | 0.29 × 0.27 × 0.20 mm |
Rigaku R-AXIS RAPID diffractometer | 2376 independent reflections |
Radiation source: rotating anode | 2135 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.027 |
Detector resolution: 10.0 pixels mm-1 | θmax = 27.5°, θmin = 3.4° |
ω scans | h = −18→18 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −8→8 |
Tmin = 0.121, Tmax = 0.257 | l = −28→28 |
18548 measured reflections |
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)] = 0.017 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.041 | H-atom parameters constrained |
S = 1.07 | w = 1/[σ2(Fo2) + (0.0163P)2 + 4.6062P] where P = (Fo2 + 2Fc2)/3 |
2376 reflections | (Δ/σ)max = 0.001 |
154 parameters | Δρmax = 1.10 e Å−3 |
0 restraints | Δρmin = −0.44 e Å−3 |
[Tb2(C4H4O4)(C8H4O4)2] | V = 2093.9 (7) Å3 |
Mr = 381.07 | Z = 8 |
Orthorhombic, Pbca | Mo Kα radiation |
a = 13.948 (3) Å | µ = 6.77 mm−1 |
b = 6.8724 (14) Å | T = 293 K |
c = 21.844 (4) Å | 0.29 × 0.27 × 0.20 mm |
Rigaku R-AXIS RAPID diffractometer | 2376 independent reflections |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | 2135 reflections with I > 2σ(I) |
Tmin = 0.121, Tmax = 0.257 | Rint = 0.027 |
18548 measured reflections |
R[F2 > 2σ(F2)] = 0.017 | 0 restraints |
wR(F2) = 0.041 | H-atom parameters constrained |
S = 1.07 | Δρmax = 1.10 e Å−3 |
2376 reflections | Δρmin = −0.44 e Å−3 |
154 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 | ||
C1 | 0.1795 (2) | 0.2005 (4) | 0.33571 (13) | 0.0204 (6) | |
C2 | 0.1524 (2) | 0.1513 (4) | 0.27097 (13) | 0.0187 (6) | |
C3 | 0.0612 (2) | 0.1987 (5) | 0.24969 (14) | 0.0253 (7) | |
H3 | 0.0170 | 0.2563 | 0.2759 | 0.030* | |
C4 | 0.0363 (2) | 0.1603 (5) | 0.18965 (13) | 0.0231 (7) | |
H4 | −0.0247 | 0.1919 | 0.1756 | 0.028* | |
C5 | 0.1021 (2) | 0.0744 (4) | 0.15012 (12) | 0.0148 (5) | |
C6 | 0.1935 (2) | 0.0297 (5) | 0.17129 (14) | 0.0223 (6) | |
H6 | 0.2382 | −0.0253 | 0.1449 | 0.027* | |
C7 | 0.2183 (2) | 0.0667 (5) | 0.23162 (14) | 0.0242 (7) | |
H7 | 0.2792 | 0.0348 | 0.2457 | 0.029* | |
C8 | 0.3754 (2) | 0.5305 (4) | 0.46896 (15) | 0.0202 (6) | |
C9 | 0.4829 (2) | 0.5423 (5) | 0.46975 (14) | 0.0238 (7) | |
H9A | 0.5034 | 0.6766 | 0.4660 | 0.029* | |
H9B | 0.5095 | 0.4688 | 0.4358 | 0.029* | |
C10 | 0.0752 (2) | 0.0328 (4) | 0.08488 (12) | 0.0126 (5) | |
O1 | 0.25854 (17) | 0.1379 (4) | 0.35567 (9) | 0.0256 (5) | |
O2 | 0.12255 (18) | 0.3032 (3) | 0.36600 (10) | 0.0274 (5) | |
O3 | 0.33421 (15) | 0.3741 (3) | 0.45414 (10) | 0.0200 (4) | |
O4 | 0.32547 (15) | 0.6772 (3) | 0.48303 (9) | 0.0178 (4) | |
O5 | 0.13755 (15) | −0.0398 (3) | 0.05016 (9) | 0.0173 (4) | |
O6 | −0.00860 (15) | 0.0752 (3) | 0.06791 (9) | 0.0184 (4) | |
Tb1 | 0.331426 (9) | 0.019240 (18) | 0.445275 (6) | 0.01157 (5) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0303 (17) | 0.0194 (14) | 0.0114 (13) | −0.0055 (12) | −0.0067 (12) | −0.0008 (12) |
C2 | 0.0266 (16) | 0.0182 (14) | 0.0113 (13) | 0.0008 (12) | −0.0074 (12) | −0.0024 (11) |
C3 | 0.0226 (16) | 0.0388 (19) | 0.0146 (14) | 0.0067 (13) | −0.0006 (12) | −0.0092 (14) |
C4 | 0.0151 (14) | 0.0381 (18) | 0.0162 (14) | 0.0072 (13) | −0.0058 (12) | −0.0084 (13) |
C5 | 0.0169 (13) | 0.0180 (13) | 0.0094 (12) | −0.0011 (11) | −0.0012 (10) | −0.0023 (11) |
C6 | 0.0173 (14) | 0.0318 (17) | 0.0179 (15) | 0.0030 (12) | −0.0059 (11) | −0.0072 (13) |
C7 | 0.0241 (16) | 0.0305 (17) | 0.0180 (14) | 0.0078 (13) | −0.0104 (12) | −0.0039 (13) |
C8 | 0.0167 (14) | 0.0154 (14) | 0.0285 (16) | 0.0013 (11) | −0.0058 (12) | −0.0014 (12) |
C9 | 0.0238 (16) | 0.0236 (16) | 0.0240 (16) | −0.0028 (12) | −0.0007 (13) | 0.0018 (13) |
C10 | 0.0161 (13) | 0.0135 (13) | 0.0082 (12) | −0.0042 (10) | −0.0014 (10) | 0.0017 (10) |
O1 | 0.0288 (12) | 0.0363 (13) | 0.0116 (9) | −0.0006 (10) | −0.0090 (9) | 0.0023 (9) |
O2 | 0.0365 (14) | 0.0298 (12) | 0.0159 (10) | 0.0018 (10) | −0.0071 (10) | −0.0108 (10) |
O3 | 0.0136 (10) | 0.0126 (9) | 0.0338 (12) | 0.0003 (8) | −0.0069 (9) | −0.0015 (9) |
O4 | 0.0175 (10) | 0.0150 (9) | 0.0209 (10) | 0.0014 (8) | −0.0025 (8) | −0.0017 (8) |
O5 | 0.0184 (10) | 0.0253 (11) | 0.0083 (9) | 0.0039 (8) | 0.0010 (7) | 0.0000 (8) |
O6 | 0.0134 (10) | 0.0294 (11) | 0.0123 (9) | −0.0010 (9) | −0.0036 (8) | −0.0009 (8) |
Tb1 | 0.01146 (7) | 0.01367 (7) | 0.00960 (7) | −0.00056 (5) | −0.00011 (5) | −0.00135 (5) |
C1—O2 | 1.252 (4) | C9—H9A | 0.9700 |
C1—O1 | 1.261 (4) | C9—H9B | 0.9700 |
C1—C2 | 1.503 (4) | C10—O5 | 1.257 (3) |
C2—C7 | 1.386 (4) | C10—O6 | 1.260 (3) |
C2—C3 | 1.393 (4) | O1—Tb1 | 2.352 (2) |
C3—C4 | 1.382 (4) | O2—Tb1i | 2.370 (2) |
C3—H3 | 0.9300 | O3—Tb1 | 2.447 (2) |
C4—C5 | 1.391 (4) | O3—Tb1i | 2.524 (2) |
C4—H4 | 0.9300 | O4—Tb1iii | 2.492 (2) |
C5—C6 | 1.392 (4) | O4—Tb1i | 2.578 (2) |
C5—C10 | 1.501 (4) | O5—Tb1iv | 2.3359 (19) |
C6—C7 | 1.386 (4) | O6—Tb1v | 2.283 (2) |
C6—H6 | 0.9300 | Tb1—O6vi | 2.283 (2) |
C7—H7 | 0.9300 | Tb1—O5vii | 2.3359 (19) |
C8—O3 | 1.261 (4) | Tb1—O2viii | 2.370 (2) |
C8—O4 | 1.263 (4) | Tb1—O4ix | 2.492 (2) |
C8—C9 | 1.501 (4) | Tb1—O3viii | 2.524 (2) |
C8—Tb1i | 2.932 (3) | Tb1—O4viii | 2.578 (2) |
C9—C9ii | 1.521 (6) | Tb1—C8viii | 2.932 (3) |
O2—C1—O1 | 124.4 (3) | C8—O4—Tb1iii | 130.8 (2) |
O2—C1—C2 | 117.7 (3) | C8—O4—Tb1i | 93.10 (17) |
O1—C1—C2 | 117.9 (3) | Tb1iii—O4—Tb1i | 108.64 (7) |
C7—C2—C3 | 119.8 (3) | C10—O5—Tb1iv | 134.11 (18) |
C7—C2—C1 | 120.7 (3) | C10—O6—Tb1v | 154.76 (19) |
C3—C2—C1 | 119.4 (3) | O6vi—Tb1—O5vii | 86.13 (7) |
C4—C3—C2 | 120.1 (3) | O6vi—Tb1—O1 | 105.02 (8) |
C4—C3—H3 | 120.0 | O5vii—Tb1—O1 | 151.11 (8) |
C2—C3—H3 | 120.0 | O6vi—Tb1—O2viii | 75.44 (8) |
C3—C4—C5 | 120.3 (3) | O5vii—Tb1—O2viii | 134.79 (8) |
C3—C4—H4 | 119.8 | O1—Tb1—O2viii | 74.10 (9) |
C5—C4—H4 | 119.8 | O6vi—Tb1—O3 | 80.00 (7) |
C4—C5—C6 | 119.5 (3) | O5vii—Tb1—O3 | 81.91 (7) |
C4—C5—C10 | 120.4 (3) | O1—Tb1—O3 | 74.17 (8) |
C6—C5—C10 | 120.2 (3) | O2viii—Tb1—O3 | 132.69 (8) |
C7—C6—C5 | 120.3 (3) | O6vi—Tb1—O4ix | 103.49 (7) |
C7—C6—H6 | 119.9 | O5vii—Tb1—O4ix | 74.84 (7) |
C5—C6—H6 | 119.9 | O1—Tb1—O4ix | 126.02 (8) |
C6—C7—C2 | 120.1 (3) | O2viii—Tb1—O4ix | 70.12 (8) |
C6—C7—H7 | 120.0 | O3—Tb1—O4ix | 156.11 (7) |
C2—C7—H7 | 120.0 | O6vi—Tb1—O3viii | 166.21 (7) |
O3—C8—O4 | 119.4 (3) | O5vii—Tb1—O3viii | 96.79 (7) |
O3—C8—C9 | 120.2 (3) | O1—Tb1—O3viii | 78.76 (8) |
O4—C8—C9 | 120.3 (3) | O2viii—Tb1—O3viii | 93.23 (8) |
O3—C8—Tb1i | 58.93 (15) | O3—Tb1—O3viii | 113.73 (5) |
O4—C8—Tb1i | 61.42 (15) | O4ix—Tb1—O3viii | 64.62 (7) |
C9—C8—Tb1i | 170.4 (2) | O6vi—Tb1—O4viii | 143.04 (7) |
C8—C9—C9ii | 107.6 (3) | O5vii—Tb1—O4viii | 79.52 (7) |
C8—C9—H9A | 110.2 | O1—Tb1—O4viii | 75.72 (8) |
C9ii—C9—H9A | 110.2 | O2viii—Tb1—O4viii | 136.68 (8) |
C8—C9—H9B | 110.2 | O3—Tb1—O4viii | 64.43 (7) |
C9ii—C9—H9B | 110.2 | O4ix—Tb1—O4viii | 105.25 (6) |
H9A—C9—H9B | 108.5 | O3viii—Tb1—O4viii | 50.58 (6) |
O5—C10—O6 | 123.8 (2) | O6vi—Tb1—C8viii | 168.43 (8) |
O5—C10—C5 | 118.4 (2) | O5vii—Tb1—C8viii | 90.44 (8) |
O6—C10—C5 | 117.8 (2) | O1—Tb1—C8viii | 73.28 (9) |
C1—O1—Tb1 | 141.6 (2) | O2viii—Tb1—C8viii | 114.33 (9) |
C1—O2—Tb1i | 124.6 (2) | O3—Tb1—C8viii | 88.58 (7) |
C8—O3—Tb1 | 151.30 (19) | O4ix—Tb1—C8viii | 86.20 (8) |
C8—O3—Tb1i | 95.72 (17) | O3viii—Tb1—C8viii | 25.35 (7) |
Tb1—O3—Tb1i | 111.92 (8) | O4viii—Tb1—C8viii | 25.48 (7) |
Symmetry codes: (i) −x+1/2, y+1/2, z; (ii) −x+1, −y+1, −z+1; (iii) x, y+1, z; (iv) −x+1/2, −y, z−1/2; (v) x−1/2, y, −z+1/2; (vi) x+1/2, y, −z+1/2; (vii) −x+1/2, −y, z+1/2; (viii) −x+1/2, y−1/2, z; (ix) x, y−1, z. |
Experimental details
Crystal data | |
Chemical formula | [Tb2(C4H4O4)(C8H4O4)2] |
Mr | 381.07 |
Crystal system, space group | Orthorhombic, Pbca |
Temperature (K) | 293 |
a, b, c (Å) | 13.948 (3), 6.8724 (14), 21.844 (4) |
V (Å3) | 2093.9 (7) |
Z | 8 |
Radiation type | Mo Kα |
µ (mm−1) | 6.77 |
Crystal size (mm) | 0.29 × 0.27 × 0.20 |
Data collection | |
Diffractometer | Rigaku R-AXIS RAPID diffractometer |
Absorption correction | Multi-scan (ABSCOR; Higashi, 1995) |
Tmin, Tmax | 0.121, 0.257 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 18548, 2376, 2135 |
Rint | 0.027 |
(sin θ/λ)max (Å−1) | 0.649 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.017, 0.041, 1.07 |
No. of reflections | 2376 |
No. of parameters | 154 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.10, −0.44 |
Computer programs: PROCESS-AUTO (Rigaku, 1998), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL-Plus (Sheldrick, 2008).
Acknowledgements
The author thanks the Beihua University for supporting this work.
References
He, Q., Zi, J.-F. & Zhang, F.-J. (2006). Acta Cryst. E62, m997–m998. Web of Science CSD CrossRef IUCr Journals Google Scholar
Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. Google Scholar
Li, Z.-F. & Wang, C.-X. (2005). Acta Cryst. E61, m2689–m2690. Web of Science CSD CrossRef IUCr Journals Google Scholar
Li, Z.-F., Wang, C.-X., Li, Y., Cai, D.-J. & Xiao, Y.-J. (2006). Acta Cryst. E62, m251–m252. Web of Science CSD CrossRef IUCr Journals Google Scholar
Rigaku (1998). PROCESS-AUTO. Rigaku Corporation, Tokyo, Japan. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Wang, C.-X. & Li, Z.-F. (2005). Acta Cryst. E61, m2212–m2213. Web of Science CSD CrossRef IUCr Journals Google Scholar
This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.
Lanthanide complexes usually exhibit interesting framework structures and intense luminescence. In all types of rare-earth compounds, carboxylate anions with aromatic rings are widely used in the construction of high-dimensional lanthanide coordination polymers because these anions are able to act as bridging ligands in various ligating modes. However, rare-earth coordination polymers with mixed aromatic and fatty carboxylates are rarely studied (Wang & Li, 2005). In this paper, we present a new mixed carboxylate complex, namely [Tb2(1,4-bdc)2(suc)]n (I), where 1,4-bdc=benzene-1,4-dicarboxylate and suc= succinate.
In (I), each Tb(III) center is coordinated by eight O atoms from 1,4-bdc and suc anions in a distorted square antiprism (Fig. 1). Each carboxylate moiety of the 1,4-bdc bridges two Tb(III) atoms, whereas each carboxylate group of suc links four Tb(III) atoms. In these modes, the central Tb(III) atoms are linked by 1,4-bdc and suc ligands, resulting in a rare three-dimensional framework structure (Fig. 2). The succinate anion is located on a centre of inversion. The structure of the title compound is isomorphous with the Dy (Li & Wang, 2005) Gd (Wang & Li, 2005), Er (He et al., 2006) and the Nd (Li et al., 2006) complex.