Startseite Crystal structure of catena-poly[triaqua-[bis(m2-4-(1H-1,2,4-triazol-1-yl)benzoato-k2O:O')-(4-(1H-1,2,4-triazol-1-yl)benzoato-k1O)-praseodymium (III) monohydrate], C27H26N9O10Pr
Artikel Open Access

Crystal structure of catena-poly[triaqua-[bis(m2-4-(1H-1,2,4-triazol-1-yl)benzoato-k2O:O')-(4-(1H-1,2,4-triazol-1-yl)benzoato-k1O)-praseodymium (III) monohydrate], C27H26N9O10Pr

  • Li Liu ORCID logo EMAIL logo , Huan-Mei Guo , Li-Li Liu und Xin-Ru Qian
Veröffentlicht/Copyright: 30. März 2023

Abstract

C27H26N9O10Pr, monoclinic, P21/c, a = 13.2280(12) Å, b = 5.5628(5) Å, c = 41.140(3) Å, β = 105.109(2)°, V = 2922.6(4) Å3, Z = 4, Rgt (F) = 0.0426, wRref (F 2) = 0.0803, T = 298.15 K.

CCDC no.: 2237487

The asymmetric unit of the title crystal structure is shown in the figure. Table 1 contains crystallographic data and Table 2 contains the list of the atoms including atomic coordinates and displacement parameters.

Table 1:

Data collection and handling.

Crystal: Colourless plate
Size: 0.28 × 0.21 × 0.13 mm
Wavelength: Mo Kα radiation (0.71073 Å)
μ: 1.74 mm−1
Diffractometer, scan mode: Bruker SMART CCD 6000, φ and ω
θ max, completeness: 25.3°, >99%
N(hkl)measured, N(hkl)unique, R int: 14,265, 5339, 0.051
Criterion for I obs, N(hkl)gt: I obs > 2 σ(I obs), 4110
N(param)refined: 436
Programs: Bruker [1], OLEX2 [2], SHELX [3, 4]
Table 2:

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

Atom x y z U iso*/U eq
C1 1.2889 (4) −0.2360 (11) 0.27171 (15) 0.0424 (12)
H1 1.338578 −0.351155 0.270342 0.051*
C2 1.2109 (4) 0.0914 (10) 0.26737 (13) 0.0373 (10)
H2 1.190663 0.250573 0.262798 0.045*
C3 1.0689 (4) −0.0345 (9) 0.29417 (12) 0.0295 (9)
C4 1.0127 (4) 0.1791 (10) 0.28720 (13) 0.0318 (9)
H4 1.032384 0.298230 0.274208 0.038*
C5 0.9266 (4) 0.2099 (9) 0.30013 (13) 0.0303 (9)
H5 0.889056 0.352904 0.295959 0.036*
C6 0.8954 (4) 0.0339 (9) 0.31898 (12) 0.0263 (9)
C7 0.9503 (4) −0.1802 (9) 0.32431 (13) 0.0305 (9)
H7 0.928635 −0.303008 0.336288 0.037*
C8 1.0375 (4) −0.2134 (9) 0.31194 (13) 0.0304 (9)
H8 1.074359 −0.357476 0.315788 0.036*
C9 0.8065 (4) 0.0782 (10) 0.33473 (12) 0.0261 (9)
C10 −0.0046 (4) 0.2237 (10) 0.40425 (14) 0.0397 (12)
H10 −0.055004 0.327807 0.408309 0.048*
C11 0.0791 (4) −0.0914 (10) 0.40230 (13) 0.0365 (10)
H11 0.101178 −0.250738 0.403678 0.044*
C12 0.2169 (4) 0.0841 (9) 0.37810 (13) 0.0291 (8)
C13 0.2806 (4) −0.1172 (9) 0.38370 (13) 0.0296 (9)
H13 0.265389 −0.247623 0.395748 0.036*
C14 0.3680 (4) −0.1193 (8) 0.37087 (13) 0.0282 (9)
H14 0.409553 −0.256432 0.373580 0.034*
C15 0.3947 (3) 0.0763 (9) 0.35421 (12) 0.0249 (9)
C16 0.3286 (4) 0.2749 (9) 0.34849 (13) 0.0296 (9)
H16 0.344451 0.406806 0.336831 0.036*
C17 0.2394 (4) 0.2773 (9) 0.36007 (13) 0.0301 (8)
H17 0.194498 0.408858 0.355712 0.036*
C18 0.4951 (4) 0.0743 (10) 0.34392 (12) 0.0262 (9)
C19 0.1400 (5) 0.2677 (13) 0.50104 (17) 0.0619 (13)
H19 0.088881 0.151928 0.500450 0.074*
C20 0.2391 (4) 0.5537 (12) 0.51736 (14) 0.0471 (10)
H20 0.275507 0.680830 0.529789 0.056*
C21 0.3358 (4) 0.5366 (11) 0.47282 (13) 0.0386 (9)
C22 0.3665 (4) 0.3818 (10) 0.45126 (13) 0.0374 (9)
H22 0.333842 0.233493 0.446132 0.045*
C23 0.4472 (4) 0.4488 (10) 0.43710 (13) 0.0355 (9)
H23 0.468603 0.343404 0.422657 0.043*
C24 0.4957 (4) 0.6687 (10) 0.44417 (13) 0.0333 (9)
C25 0.4616 (4) 0.8225 (10) 0.46556 (13) 0.0382 (10)
H25 0.493393 0.972128 0.470380 0.046*
C26 0.3823 (4) 0.7607 (10) 0.47989 (14) 0.0397 (9)
H26 0.360288 0.867185 0.494061 0.048*
C27 0.5785 (4) 0.7538 (10) 0.42801 (14) 0.0337 (10)
N1 1.1601 (3) −0.0668 (8) 0.28205 (10) 0.0339 (10)
N2 1.2105 (4) −0.2832 (9) 0.28479 (12) 0.0447 (13)
N3 1.2927 (4) −0.0075 (8) 0.26031 (13) 0.0481 (14)
N4 0.2573 (3) 0.4679 (9) 0.48903 (11) 0.0456 (11)
N5 0.1632 (4) 0.4347 (11) 0.52531 (13) 0.0574 (12)
N6 0.1936 (4) 0.2751 (11) 0.47780 (14) 0.0649 (13)
N7 0.1275 (3) 0.0899 (7) 0.39120 (10) 0.0293 (10)
N8 0.0726 (3) 0.2979 (8) 0.39129 (12) 0.0417 (12)
N9 −0.0042 (3) −0.0131 (8) 0.41102 (12) 0.0442 (13)
O1 0.7716 (3) −0.0958 (6) 0.34764 (9) 0.0356 (9)
O2 0.7762 (3) 0.2935 (6) 0.33534 (8) 0.0312 (9)
O3 0.5393 (3) −0.1237 (6) 0.34317 (9) 0.0327 (9)
O4 0.5300 (2) 0.2743 (6) 0.33683 (9) 0.0342 (9)
O5 0.5998 (3) 0.6152 (7) 0.40617 (9) 0.0389 (10)
O6 0.6198 (3) 0.9533 (7) 0.43624 (10) 0.0498 (10)
O7 0.7178 (3) 0.2043 (6) 0.39729 (9) 0.0360 (9)
H7A 0.664551 0.155846 0.403412 0.054*
H7B 0.733424 0.087091 0.386223 0.054*
O8 0.8248 (3) 0.6583 (7) 0.40586 (8) 0.0357 (9)
H8A 0.830941 0.634587 0.426694 0.054*
H8B 0.871877 0.761406 0.405417 0.054*
O9 0.6196 (3) 0.6184 (7) 0.29602 (9) 0.0405 (10)
H9A 0.597624 0.761949 0.291242 0.061*
H9B 0.649 (4) 0.582 (9) 0.2803 (11) 0.08 (2)*
O10 0.5584 (3) 0.0738 (8) 0.27251 (10) 0.0521 (11)
H10A 0.496423 0.058755 0.259994 0.078*
H10B 0.552237 0.167802 0.288111 0.078*
Pr1 0.66827 (2) 0.56140 (5) 0.35920 (2) 0.02277 (9)

1 Source of materials

The 4-(1H-1,2,4-triazol-1-yl)benzoic acid (Htba) was obtained from Jinan Henghua Technology Co., Ltd. Other chemicals were obtained from Shanghai Aladdin Bio–Chem Technology Co., LTD. Pr2O3 (0.0240 g, 0.1 mmol), Htba (0.0189 g, 0.1 mmol), distilled H2O (10 mL) and five drops of concentrated HCl were mixed in a 20 mL Teflon-lined stainless steel reactor and heated to 140 °C for 72 h. The reactor was cooled to room temperature slowly. Clear light colourless plate crystals of the title complex were obtained, yielding 51% (based on the ligand).

2 Experimental details

The crystal structure was solved by SHELXT program with intrinsic phasing and refined by SHELXT program. All the H-atoms were generated geometrically with isotropic thermal factors. The H-atoms (H9A and H9B) of the free water were restrained. The bond lengths of O9–H9A and O9–H9B were fixed to 0.85 Å with command DFIX and the distance of H9A–H9B was fixed to 1.344 Å with command DANG.

3 Comment

As a rigid carboxylate ligand containing triazole heterocycle, 4-(1H-1,2,4-triazol-1-yl)benzoic acid (Htba), has been applied to build metal complexes with various ions [5], [6], [7], [8]. However, to the best of our knowledge, only limited lanthanide metal (Nd3+/Sm3+/Tb3+) complexes were reported [9, 10]. To enrich the Ln-series of the structure based on Htba ligand, the title 1D Pr(III)-complex was synthesized.

The asymmetric unit contains one Pr(III) ion, three deprotonated Htba ligands, three coordinated water molecules and one free water molecule. The Pr(III) ion is eight-coordinated with five carboxyl oxygen atoms (O1+x, 1 + y, +z , O2, O3+x, 1 + y, +z , O4, O5) from five different ligands and three oxygen atoms (O7, O8, O9) from three different coordinated water molecules. It is worth noting that even though the Htba ligand contains two potential N-coordination sites, no nitrogen participated in the self-assembly process with Pr(III) ion. The bond distances of Pr–O are in the regular range of 2.357(3)–2.529(4) Å, similar to the other Pr(III)-complexes with analogical coordination modes [11, 12]. The Htba ligands in the crystal structure adopt two kinds of connection modes: monodentate terminal mode or bidentate bridging mode. Interestingly, two Pr(III) ions, two bidentate bridging Htba ligands and one monodentate terminal Htba ligand formed a Pr2(tba)3 binuclear unit. These units are interconnected and generated a 1D linear structure. The 1D structures are further expended by O—H ⃛ O and N—H ⃛ O hydrogen bonding interactions and the π-π stacking interactions between the benzene rings and heterocyclic rings, centroid-centroid distance range: 3.750(3)–3.814(3) Å, and finally, constituted a 3D network.


Corresponding author: Li Liu, College of Chemistry and Chemical Engineering, Weifang University, Weifang, Shandong 261061, P. R. China, E-mail:

Funding source: Undergraduate Teaching Reform Project of Shandong Province

Award Identifier / Grant number: Z2022072

Acknowledgements

Special thanks are given to Dr. Yu-Pei Xia for his kind assistance with the structure discussion of the complex.

  1. Author contributions: All the authors have accepted responsibility for the entire content of this submitted manuscript and approved submission.

  2. Research funding: This work was supported by the Undergraduate Teaching Reform Project of Shandong Province (No. Z2022072).

  3. Conflict of interest statement: The authors declare no conflicts of interest regarding this article.

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Received: 2023-01-26
Accepted: 2023-03-16
Published Online: 2023-03-30
Published in Print: 2023-06-27

© 2023 the author(s), published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution 4.0 International License.

Artikel in diesem Heft

  1. Frontmatter
  2. New Crystal Structures
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