Home Crystal structure of diaqua-(hydroxido)-{μ-[2-(hydroxy)-5-[(4-nitrophenyl)diazenyl]benzoato]}-{2-hydroxy-5-[(4-nitrophenyl)diazenyl]benzoato}-(1,10-phenanthroline)-diterbium hydrate, C38H27.4N8O12.2Tb
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Crystal structure of diaqua-(hydroxido)-{μ-[2-(hydroxy)-5-[(4-nitrophenyl)diazenyl]benzoato]}-{2-hydroxy-5-[(4-nitrophenyl)diazenyl]benzoato}-(1,10-phenanthroline)-diterbium hydrate, C38H27.4N8O12.2Tb

  • Ying Wang ORCID logo EMAIL logo , Mouyi Zhang and Lei Guan
Published/Copyright: October 25, 2024

Abstract

C38H27.4N8O12.2Tb, monoclinic, P21/c (no. 14), a = 20.2057(8) Å, b = 15.9219(8) Å, c = 11.4635(4) Å, β = 95.150(1)°, V = 3673.1(3) Å3, Z = 4, R gt(F) = 0.0371, wR ref(F 2) = 0.0838, T = 193.0 K.

CCDC no.: 2322781

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: Yellow block
Size: 0.13 × 0.11 × 0.10 mm
Wavelength: Mo K α radiation (0.71073 Å)
μ: 2.01 mm−1
Diffractometer, scan mode: Bruker D8 VENTURE, φ and ω
θ max, completeness: 27.5°, >99 %
N(hkl)measured, N(hkl)unique, R int: 32944, 8391, 0.059
Criterion for I obs, N(hkl)gt: I obs > 2 σ(I obs), 6,447
N(param)refined: 547
Programs: Bruker, 1 SHELX 2 , 3
Table 2:

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

Atom x y z U iso*/U eq
Tb1 0.16129 (2) 0.31143 (2) 0.67359 (2) 0.02356 (6)
O1 0.72779 (18) 0.5813 (3) 0.7745 (4) 0.0726 (13)
O2 0.6848 (2) 0.4901 (3) 0.6495 (5) 0.0758 (14)
O3 0.15237 (18) 0.5646 (2) 1.0902 (3) 0.0496 (9)
H3 0.125201 0.527959 1.063380 0.074*
O4 0.10943 (15) 0.4432 (2) 0.9530 (3) 0.0410 (8)
O5 0.15747 (14) 0.4300 (2) 0.7867 (2) 0.0344 (7)
O6 0.79977 (16) 0.3053 (3) 0.2056 (3) 0.0567 (10)
O7 0.74366 (17) 0.2162 (3) 0.0956 (3) 0.0533 (10)
O8 0.25993 (13) 0.3681 (2) 0.6451 (2) 0.0324 (7)
O9 0.18893 (13) 0.26111 (19) 0.4937 (2) 0.0284 (7)
O10 0.23107 (13) 0.2453 (2) 0.3242 (2) 0.0318 (7)
O11 0.14253 (14) 0.1571 (2) 0.6690 (3) 0.0348 (7)
H11A 0.177162 0.131867 0.703629 0.052*
H11B 0.140472 0.139337 0.596839 0.052*
O12 0.08697 (14) 0.2811 (2) 0.8296 (2) 0.0388 (8)
H12A 0.071623 0.328605 0.856300 0.058*
H12B 0.109972 0.259013 0.891128 0.058*
N1 0.6814 (2) 0.5398 (3) 0.7300 (5) 0.0579 (13)
N2 0.4373 (2) 0.5789 (3) 0.9277 (3) 0.0435 (10)
N3 0.38947 (19) 0.5351 (3) 0.8843 (3) 0.0385 (9)
N4 0.74812 (18) 0.2679 (3) 0.1747 (3) 0.0389 (10)
N5 0.52695 (17) 0.3340 (3) 0.4250 (3) 0.0369 (10)
N6 0.47205 (16) 0.3010 (2) 0.3883 (3) 0.0316 (8)
N7 0.04233 (16) 0.3017 (2) 0.5763 (3) 0.0299 (8)
N8 0.12715 (16) 0.4246 (2) 0.5212 (3) 0.0297 (8)
C1 0.5055 (3) 0.5061 (4) 0.7888 (6) 0.0621 (17)
H1 0.469423 0.470310 0.763330 0.075*
C2 0.5650 (3) 0.4981 (4) 0.7411 (6) 0.0620 (17)
H2 0.570383 0.457754 0.681686 0.074*
C3 0.6171 (2) 0.5504 (4) 0.7813 (5) 0.0481 (13)
C4 0.6103 (3) 0.6083 (4) 0.8663 (5) 0.0520 (14)
H4 0.646653 0.643146 0.893150 0.062*
C5 0.5504 (3) 0.6160 (4) 0.9132 (5) 0.0503 (14)
H5 0.545274 0.656123 0.973063 0.060*
C6 0.4977 (2) 0.5656 (3) 0.8735 (4) 0.0435 (12)
C7 0.3297 (2) 0.5469 (3) 0.9384 (4) 0.0361 (11)
C8 0.3231 (3) 0.6007 (3) 1.0333 (4) 0.0429 (12)
H8 0.359812 0.633738 1.063908 0.051*
C9 0.2634 (3) 0.6059 (3) 1.0824 (4) 0.0472 (13)
H9 0.259064 0.642419 1.146715 0.057*
C10 0.2094 (2) 0.5574 (3) 1.0376 (4) 0.0372 (11)
C11 0.2147 (2) 0.5057 (3) 0.9411 (3) 0.0320 (10)
C12 0.2755 (2) 0.5006 (3) 0.8927 (3) 0.0315 (10)
H12 0.279745 0.464740 0.827561 0.038*
C13 0.1571 (2) 0.4557 (3) 0.8901 (3) 0.0305 (10)
C14 0.68914 (19) 0.2852 (3) 0.2369 (4) 0.0311 (10)
C15 0.6944 (2) 0.3420 (3) 0.3267 (4) 0.0369 (11)
H15 0.735073 0.370524 0.347232 0.044*
C16 0.6395 (2) 0.3570 (3) 0.3871 (4) 0.0382 (11)
H16 0.642181 0.396031 0.449985 0.046*
C17 0.5799 (2) 0.3146 (3) 0.3556 (4) 0.0329 (10)
C18 0.5758 (2) 0.2582 (3) 0.2632 (4) 0.0365 (11)
H18 0.535100 0.229978 0.241693 0.044*
C19 0.6305 (2) 0.2424 (3) 0.2020 (4) 0.0336 (10)
H19 0.628157 0.203862 0.138508 0.040*
C20 0.41931 (19) 0.3200 (3) 0.4560 (4) 0.0318 (10)
C21 0.4258 (2) 0.3691 (4) 0.5583 (4) 0.0505 (15)
H21 0.467764 0.392245 0.585027 0.061*
C22 0.3722 (2) 0.3834 (4) 0.6193 (4) 0.0520 (16)
H22 0.377564 0.416696 0.688243 0.062*
C23 0.3087 (2) 0.3502 (3) 0.5829 (3) 0.0301 (10)
C24 0.30189 (18) 0.3011 (3) 0.4794 (3) 0.0247 (9)
C25 0.35782 (19) 0.2872 (3) 0.4181 (3) 0.0270 (9)
H25 0.353357 0.254280 0.348759 0.032*
C26 0.23712 (18) 0.2670 (3) 0.4293 (3) 0.0244 (9)
C27 0.0006 (2) 0.2416 (3) 0.6036 (4) 0.0417 (12)
H27 0.014467 0.204463 0.665882 0.050*
C28 −0.0626 (2) 0.2303 (4) 0.5453 (5) 0.0529 (15)
H28 −0.090888 0.186758 0.567884 0.063*
C29 −0.0825 (2) 0.2829 (4) 0.4560 (5) 0.0476 (13)
H29 −0.125237 0.276077 0.415170 0.057*
C30 −0.0407 (2) 0.3472 (3) 0.4235 (4) 0.0345 (10)
C31 0.02220 (18) 0.3538 (3) 0.4866 (3) 0.0256 (9)
C32 0.06724 (19) 0.4197 (3) 0.4574 (3) 0.0267 (9)
C33 0.0478 (2) 0.4753 (3) 0.3649 (4) 0.0322 (10)
C34 −0.0161 (2) 0.4658 (3) 0.3021 (4) 0.0410 (12)
H34 −0.028895 0.502682 0.238951 0.049*
C35 −0.0582 (2) 0.4061 (3) 0.3304 (4) 0.0415 (12)
H35 −0.100741 0.402375 0.288132 0.050*
C36 0.0932 (2) 0.5373 (3) 0.3387 (4) 0.0436 (12)
H36 0.082123 0.575641 0.276471 0.052*
C37 0.1537 (2) 0.5426 (3) 0.4029 (5) 0.0474 (13)
H37 0.184885 0.584496 0.385872 0.057*
C38 0.1686 (2) 0.4854 (3) 0.4936 (4) 0.0391 (11)
H38 0.210417 0.489887 0.538110 0.047*
O13a −0.0044 (10) 0.3737 (17) 0.8785 (19) 0.073 (6)
H13Aa −0.001273 0.404354 0.941542 0.110*
H13Ba −0.031098 0.333086 0.893687 0.110*
  1. aOccupancy: 0.2.

1 Source of materials

A mixture of Tb(NO3)3·6H2O (0.045 g, 0.1 mmol), 2-hydroxy-5-((4-nitrophenyl)azo)benzoic acid monosodium salt (NaHnpaba) (0.015 g, 0.1 mmol) and 1,10-phenanthroline (phen) (0.018 g, 0.1 mmol) in deionized water (15 ml) and ethanol (5 ml) was sealed into a Parr Teflon-lined stainless steel vessel (25 ml), which was heated at 110 °C under autogenous pressure for 3 d. After cooling naturally to room temperature, the yellow blocked crystals were isolated with the yield of 56 % based on NaHnpaba.

2 Experimental details

The multi-scan program SADABS 1 was used for absorption correction. The structure solution and the refinement were successfully carried out using SHELX program. 2 , 3 Hydrogen atoms attached to carbon atoms were placed geometrically and refined using a riding model, with U iso(H) = 1.2U eq(C). Hydrogen atoms bonded to oxygen atoms were found in different maps, and refined with U iso(H) = 1.5U eq(O).

3 Comment

The design and production of coordination polymers (CPs) have attracted widespread attention, due to their potential applications in the areas, such as magnetism, optical devices, gas storage/separation, catalyst, sensors and so on. 4 , 5 , 6 Over the past decade, numerous CPs constructed by aromatic carboxylate linkers have been extensively studied. 7 , 8 Moreover, the topological structures of CPs could be controlled and improved by introduction of other substituent groups onto aromatic carboxylate linkers, such as phenol, nitro, sulfonate and so on. 9 The asymmetric structural unit consists of one Tb center, one Hnpaba and one npaba2− ligands, one phen molecule, two coordinated water molecules and 0.2 free water molecule. Each Tb center is eight-coordinated by three carboxylate oxygen atoms, one phenol oxygen atom, two nitrogen atoms from one phen molecule and two oxygen atoms from two water molecules (Tb–O = 2.238(3)–2.486(3)Å and Tb–N = 2.561(4)Å and 2.562(3)Å), showing distorted double capped triangular prism coordination geometry. The npaba2− anions behavior as tridentate ligands, which bind to adjacent two Tb centers through their carboxylate groups in bridging mode and the monodentate phenol groups, resulting in the formation of a one-dimensional chain. The Hnpaba anion connects to the Tb center via monodentate carboxylate group. The phen molecule acts as a terminated ligand, chelating with Tb center. In addition, the O–H⋯O hydrogen bonds can connect to adjacent one-dimensional chains, and increase thermal stability of the title complex.


Corresponding author: Ying Wang, School of Petrochemical Engineering, Liaoning Petrochemical University, Fushun 113001, China, E-mail:

Funding source: Basic Scientific Research Project of Universities in Liaoning Provincial Education Department

Award Identifier / Grant number: (grant number LJKMZ20220738)

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

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

  3. Research funding: Basic Scientific Research Project of Universities in Liaoning Provincial Education Department (grant number LJKMZ20220738).

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Received: 2024-01-04
Accepted: 2024-10-10
Published Online: 2024-10-25
Published in Print: 2024-12-17

© 2024 the author(s), published by De Gruyter, Berlin/Boston

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

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