Home Crystal structure of poly-[triaqua-(μ4-5′-carboxy-[1,1′-biphenyl]-2,3,3′-tricarboxylate-κ6O1,O2:O3,O4:O5:O6)praseodymium(III), C16H13O11Pr
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Crystal structure of poly-[triaqua-(μ4-5′-carboxy-[1,1′-biphenyl]-2,3,3′-tricarboxylate-κ6O1,O2:O3,O4:O5:O6)praseodymium(III), C16H13O11Pr

  • Rong Fang Li , Xin Fang Liu and Xun Feng EMAIL logo
Published/Copyright: October 29, 2016

Abstract

C16H13O11Pr, triclinic, P1̅, a = 6.915(3) Å, b = 10.895(4) Å, c = 11.644(4) Å, α = 94.137(5)°, β = 101.152(5)°, γ = 96.831°, V = 850.61(5) Å3, Z = 2, Rgt(F) = 0.0352, wRref(F2) = 0.0737, T = 293(2)K.

CCDC no.:: 1509414

A part of the title crystal structure is shown in the figure. Tables 1 and 2 contain details of the measurement method and a list of the atoms including atomic coordinates and displacement parameters.

Table 1

Data collection and handling.

Crystal:Olivine block
Size:0.22 × 0.21 × 0.2 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:29.3 cm−1
Diffractometer, scan mode:CCD, φ and ω
2θmax, completeness:55°, >99%
N(hkl)measured, N(hkl)unique, Rint:16557, 3889, 0.066
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 3448
N(param)refined:253
Programs:SADABS [9], SHELX [10]
Table 2

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2).

AtomxyzUiso*/Ueq
Pr10.09008(4)0.26740(2)0.00558(2)0.01812(8)
O10.2410(5)0.2251(3)0.2222(3)0.0269(7)
O20.3050(5)0.1032(3)0.0796(2)0.0251(7)
O30.0559(5)−0.0985(3)0.1699(3)0.0257(7)
O40.2508(5)−0.2308(3)0.1234(3)0.0303(8)
O50.7096(5)0.4981(3)0.6597(3)0.0325(8)
O60.7897(5)0.6652(3)0.5691(3)0.0299(7)
H60.78730.70200.63270.045*
O70.8840(5)0.4012(3)0.0803(3)0.0271(7)
O80.8960(5)0.5961(3)0.1519(3)0.0270(7)
O90.3894(7)0.2694(5)−0.0822(5)0.0769(16)
H9A0.49980.2368−0.05240.092*
H9B0.36920.3103−0.15310.115*
O100.3172(5)0.4630(3)0.1079(3)0.0337(8)
H10A0.28100.53350.06800.051*
H10B0.30250.47490.18810.051*
O11−0.1324(5)0.0997(3)0.0835(3)0.0289(7)
H11A−0.26830.09860.04440.043*
H11B−0.12030.11840.16660.043*
C10.5218(7)−0.1327(4)0.3403(4)0.0273(10)
H10.4959−0.21890.33310.033*
C20.6810(7)−0.0718(4)0.4234(4)0.0313(11)
H20.7592−0.11700.47410.038*
C30.7240(7)0.0553(4)0.4313(4)0.0280(10)
H30.83080.09550.48800.034*
C40.6104(6)0.1248(4)0.3561(4)0.0220(9)
C50.4442(6)0.0648(4)0.2742(4)0.0188(8)
C60.4007(6)−0.0651(4)0.2674(4)0.0195(9)
C70.2236(6)−0.1343(4)0.1822(4)0.0213(9)
C80.3225(6)0.1353(4)0.1876(4)0.0208(9)
C90.6733(6)0.2613(4)0.3590(4)0.0200(9)
C100.6886(6)0.3400(4)0.4600(4)0.0216(9)
H100.65960.30760.52740.026*
C110.7470(6)0.4673(4)0.4620(4)0.0196(9)
C120.7976(6)0.5159(4)0.3639(4)0.0198(9)
H120.83450.60090.36460.024*
C130.7930(6)0.4367(4)0.2642(3)0.0180(8)
C140.7269(6)0.3098(4)0.2615(4)0.0203(9)
H140.71910.25770.19350.024*
C150.7472(6)0.5443(4)0.5736(4)0.0205(9)
C160.8627(6)0.4815(4)0.1587(4)0.0185(8)

Source of material

H4bptc (biphenyl-2,3,3′,5′-tetracarboxylic acid 0.050 g, 0.15 mmol), Pr(NO3)3⋅6H2O (0.0435 g, 0.10 mmol), and H2O (15 mL) were mixed in a 25 mL Teflon-lined vessel, and the pH was adjusted to 4 with HNO3. The obtained solution was placed in a stainless steel vessel and heated at 145 °C for 3 days, and then slowly cooled to room temperature. Colourless block crystals were obtained; yield: 38% based on Pr(III). Elemental analysis (%): calcd for C16 H13O11Pr: C, 36.81; H, 2.51; Found: C, 36.78; H, 2.58; IR/cm−1 (KBr): 3368 (br), 2579 (w), 1708 (s), 1604 (s), 1564 (m), 1538(sh), 1406(s),1377(s), 1307(s), 1261(s), 905(s), 866(s), 831(s), 804(s), 784(s), 690(s).

Experimental details

An empirical absorption correction was applied using the SADABS program [9]. The hydrogen atoms of organic ligands were placed in the geometrically calculated positions.

Discussion

MOFs possess many intriguing properties including high porosity, more specific surface area and multi metal sites etc. which in the field of chemistry and chemical engineering have many applications, such as gas storage, molecular separation, catalysis, drug delivery, and so on [1; 2; 3; 4; 5]. Biphenyltetracarboxylates are excellent type of organic ligands for synthesizing various MOFs. Differing from other biphenyltetracarboxylic acids reported, the ligand we report in this contribution remains largely unexplored and we are conducting the research to explore lower symmetry MOFs using such aromatic polycarboxylate [6; 7; 8]. In order to further study the coordination behavior and role of the praseodymium(III) cation in the self-assembly processes in the presence of H4bptc, the title complex has been synthesized.

The asymmetric unit of the title structure contains one Hbptc3−, one Pr(III) ion, three coordinated water molecules. The central Pr(III) ion is nine-coordinated with a distorted double septilateral pyramid geometry by six carboxylic oxygen atoms from four Hbptc3− ligands and three oxygen atoms of water molecules. Bond angles around Pr(III) vary from 72.56(10)° to 144.91(9)°. The Pr—O bond lengths are 2.388(3) to 2.632(3)Å. Neighbouring Pr ions are connected by Hbptc3− ligands forming a two-dimensional framework.

Acknowledgements

This work was supported by the Natural Science Foundation of China (Nos. 21273101 and 21302082). Foundation for Science & Technology Innovation Talents in Henan province (Nos. 2014HASTIT014 and 164100510012), the key Foundation of Education Committee of Henan province, China (No 14B150033).

References

1 Yang, Z.; Liu, J.; Liang, X. Q.; Jiang, Y.; Zhang, T.; Han, B.; Sun, F. X.; Liu, L.: Two novel 2D metal-organic frameworks based on biphenyl-2,2′,6,6′-tetracarboxylic acid: synthesis, structures and luminescent properties. Inorg. Chem. Commun. 16 (2012) 92–94.10.1016/j.inoche.2011.12.003Search in Google Scholar

2 Feng, X.; Ling, X. L.; Liu, L.; Song, H. L.; Wang, L. Y.; Ng, S. W.; Su, B. Y.: A series of 3D lanthanide frameworks constructed from aromatic multi-carboxylate, ligand: structural diversity, luminescence and magnetic propertieses. Dalton Trans. 14 (2013) 10292–10303.10.1039/c3dt50810bSearch in Google Scholar PubMed

3 Feng, X.; Feng, Y. Q.; Liu, L.; Chen, J. J.; Ng, S. W.; Wang, L. Y.; Guo, J. Z.; Reticular three-dimensional 3d–4f frameworks constructed through substituted imidazoledicarboxylate: syntheses, luminescence and magnetic properties study. Dalton Trans. 44 (2015) 804–816.10.1039/C4DT02047BSearch in Google Scholar PubMed

4 Li, B.; Zang, S. Q.; Ji, C.; Hou, H. W.; Mak, T. C. W.; Syntheses, structures, and properties of silver–organic frameworks constructed with 1,1′-biphenyl-2,2′,6,6′-tetracarboxylic acid. Cryst. Growth. Des. 12 (2012) 1443–1451.10.1021/cg2015447Search in Google Scholar

5 Zhang, S.; Xie, G.; Zou, Y.; Chen, S.; Gao,S.; Syntheses, structures, and magnetism of two coordination compounds with 3,3′,4,4′-biphenyltetracarboxylic acid and 1,10-phenanthroline. J. Coord. Chem. 65 (2012) 1062–1070.10.1080/00958972.2012.666535Search in Google Scholar

6 Li, R. F.; Liu, X. F.; Wang, Y. F.; Zhang, T.; Feng, X.; One three-dimensional {Mn4}cluster coordination polymer from a new tetracarboxylate linker and N-donor ancillary ligand: crystal structure and magnetic property. J. Inorg. Organomet. Polym. 25 (2015) 1200–1204.10.1007/s10904-015-0228-zSearch in Google Scholar

7 Li, R. F.; Gu, Y. X.; Liu, X. F.; Feng, X.; Ma, L. F.; Syntheses, structures, and properties of two zinc(II) metal-organic frameworks based on biphenyl-2,3,3,5-tetracarboxylic acid and N-Donor ancillary ligands. Z. Anorg. Allg. Chem. 641 (2015) 1114–1118.10.1002/zaac.201400483Search in Google Scholar

8 Li, R. F.; Wang, Y. F.; Liu, X. F.; Feng, X.; Zhang, X. Y.; Du, D. G.: A One-dimensional cobalt coordination polymer based on biphenyl-2,3,3′,5′-tetracarboxylic acid and N-donor ancillary ligands: crystal structure and magnetic property. Chinese J. Struct. Chem. 10 (2015) 1558–1564.Search in Google Scholar

9 Sheldrick, G. M.: SADABS Area Correction Absorption Program. University of Gottingen: Göttingen, Germany, 1994.Search in Google Scholar

10 Sheldrick, G. M.: A short history of SHELX. Acta Crystallogr. A64 (2008) 112–122.10.1107/S0108767307043930Search in Google Scholar PubMed

Received: 2016-6-20
Accepted: 2016-10-11
Published Online: 2016-10-29
Published in Print: 2017-1-1

©2016 Rong Fang Li et al., published by De Gruyter.

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

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