Home The crystal structure of poly[μ2-aqua- aqua-(μ3-(E)-2-(4-((2-carbamothioylhydrazineylidene)methyl)phenoxy)acetato-κ3 O:S:S)sodium(I)], C10H14N3O5SNa
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The crystal structure of poly[μ2-aqua- aqua-(μ3-(E)-2-(4-((2-carbamothioylhydrazineylidene)methyl)phenoxy)acetato-κ3 O:S:S)sodium(I)], C10H14N3O5SNa

  • Xi-Shi Tai ORCID logo , Li-Hua Wang and Yu-Pei Xia EMAIL logo
Published/Copyright: February 15, 2022

Abstract

C10H14N3O5SNa, triclinic, P 1 (no. 2), a = 6.7015(5) Å, b = 7.5656(5) Å, c = 14.1332(8) Å, β = 93.159(5)°, V = 654.71(8) Å3, Z = 2, R gt (F) = 0.0357, wR ref (F 2) = 0.0872, T = 273 K.

CCDC no.: 2082889

The molecular 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: Colorless block
Size: 0.11 × 0.10 × 0.08 mm
Wavelength: Mo Kα radiation (0.71073 Å)
μ: 0.30 mm−1
Diffractometer, scan mode: Rigaku SuperNova, ω
θ max, completeness: 25.0°, >99%
N(hkl)measured, N(hkl)unique, R int: 4268, 2284, 0.027
Criterion for I obs, N(hkl)gt: I obs > 2 σ(I obs), 1969
N(param)refined: 205
Programs: Bruker [1], Olex2 [2], SHELX [3], Diamond [4]
Table 2:

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

Atom x y z U iso*/U eq
C1 1.2614 (3) 0.8211 (3) 0.20138 (13) 0.0093 (4)
C2 0.8917 (3) 0.8458 (3) 0.36091 (14) 0.0105 (4)
H2 0.829020 0.911663 0.325921 0.013*
C3 0.8089 (3) 0.7887 (3) 0.45049 (13) 0.0096 (4)
C4 0.6266 (3) 0.8194 (3) 0.47820 (14) 0.0105 (4)
H4 0.560939 0.877113 0.439220 0.013*
C5 0.5405 (3) 0.7665 (3) 0.56205 (14) 0.0105 (4)
H5 0.417806 0.787286 0.578535 0.013*
C6 0.6382 (3) 0.6822 (3) 0.62135 (13) 0.0098 (4)
C7 0.8259 (3) 0.6554 (3) 0.59643 (14) 0.0114 (5)
H7 0.894868 0.602880 0.636993 0.014*
C8 0.9085 (3) 0.7064 (3) 0.51219 (14) 0.0113 (5)
H8 1.031726 0.686224 0.495946 0.014*
C9 0.3739 (3) 0.6464 (3) 0.73119 (14) 0.0103 (4)
H9A 0.259916 0.588714 0.678176 0.012*
H9B 0.403109 0.783253 0.744570 0.012*
C10 0.2982 (3) 0.5538 (3) 0.81928 (13) 0.0099 (5)
H2A 1.047 (4) 0.929 (3) 0.2175 (15) 0.010 (6)*
H4A −0.330 (4) 0.620 (3) 0.9382 (18) 0.029 (7)*
H4B −0.289 (4) 0.641 (4) 1.036 (2) 0.039 (8)*
H5A 0.124 (4) 0.828 (4) 0.8493 (18) 0.039 (8)*
H5B 0.259 (4) 1.004 (3) 0.8610 (17) 0.023 (8)*
N1 1.3532 (3) 0.7232 (2) 0.24710 (11) 0.0134 (4)
H1A 1.316859 0.694239 0.302336 0.016*
H1B 1.448956 0.688713 0.221483 0.016*
N2 1.1127 (3) 0.8718 (2) 0.24420 (12) 0.0107 (4)
N3 1.0488 (3) 0.8073 (2) 0.32929 (11) 0.0105 (4)
Na1 0.000000 0.500000 1.000000 0.0124 (3)
Na2 0.000000 1.000000 1.000000 0.0127 (3)
O1 0.5654 (2) 0.62119 (18) 0.70468 (9) 0.0119 (3)
O2 0.3924 (2) 0.45320 (18) 0.85119 (9) 0.0121 (3)
O3 0.1427 (2) 0.58362 (18) 0.85230 (9) 0.0118 (3)
O4 −0.2275 (2) 0.6722 (2) 0.98521 (12) 0.0132 (3)
O5 0.1361 (3) 0.9456 (2) 0.85079 (11) 0.0141 (4)
S1 1.33292 (8) 0.88919 (7) 0.09353 (3) 0.01171 (17)

Source of material

4-Formylphenoxyacetic acid (0.5 mmol, 0.0901 g), thiosemicarbazide (0.5 mmol, 0.0456 g) and NaOH (0.5 mmol, 0.020 g) were dissolved into 20 mL of a H2O/ethanol solution (v:v = 1:1) with stirring at 50 °C. After 20 min, MgCl2·6H2O (0.5 mmol, 0.1015 g) was added to the mixture. The mixture was continued to react for 4 h at 80 °C with stirring. The mixture was then cooled to room temperature and continued the stirring for 4 h. Filtering the reaction mixture. After 20 days, the crystals of the title compound were obtained by slowing volatilization at room temperature. Elemental analysis (%) calcd. for C10H14N3O5SNa: C, 38.55; H, 4.50; N, 13.49. Found (%): C, 38.66; H, 4.76; N, 13.17.

Experimental details

The hydrogen atoms were positioned geometrically (C–H = 0.93–0.97 Å and N–H = 0.86 Å). Their U iso values were set to 1.2U eq of the parent atoms.

Comment

Metal coordination polymers show excellent properties in many areas of chemical engineering and materials [5], [6], [7], [8], [9], [10], [11], [12]. According to the literature, the studies on synthesis and properties of metal coordination polymer mainly focuses on transition metals. In order to enrich the structure and properties of the metal coordination polymers, our research group is committed to studying the structure and properties of the alkaline earth metal coordination polymers [13], [14], [15], [16]. At the same time, we have also studied the catalytic activity of some metal complexes [16]. In order to further investigate the structure and catalytic property of alkali earth metal coordination polymers, in this work, a new Na(I) coordination polymer has been synthesized by a one-pot method. The title coordination polymer was characterized by EA and single-crystal X-ray diffraction analysis.

As shown in Figure 1, the Na(I) coordination polymer it is made up of one Na(I) ions on inversion centers, one thiosemicarbazide ligand and two coordinated water molecules. Na1 and Na2 atoms adopt a six-coordinated octahedron configuration, where Na1 is coordinated with two O atoms and S atoms of two different L ligands and two O atoms of two water molecules, and Na2 is coordinated with four O atoms of four coordinated water molecules and S atoms of two different L ligands. Thus the title structure contains two different coordinated units: Na(OL)2(SL)2(Owater)2 and Na(Owater)4(SL)2, which forms a chained structure by the Na–O coordination which is further extended by the Na–S coordination S atoms of L ligands. The Na (I) coordination polymer assembles an extended layered structure. All bond lengths and angles are in the expected ranges [17].


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

Funding source: National Natural Science Foundation of China https://doi.org/10.13039/501100001809

Award Identifier / Grant number: 21171132

Funding source: Natural Science Foundation of Shandong https://doi.org/10.13039/501100007129

Award Identifier / Grant number: ZR2014BL003

Funding source: Project of Shandong Province Higher Educational Science and Technology Program https://doi.org/10.13039/501100015642

Award Identifier / Grant number: J14LC01

Funding source: Science Foundation of Weifang

Award Identifier / Grant number: 2020ZJ1054

Funding source: Weifang University of Science and Technology https://doi.org/10.13039/501100010887

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

  2. Research funding: This project was supported by the National Natural Science Foundation of China (No. 21171132), the Natural Science Foundation of Shandong (ZR2014BL003), the Project of Shandong Province Higher Educational Science and Technology Program (J14LC01), Science Foundation of Weifang (2020ZJ1054), and Weifang University of Science and Technology (https://doi.org/10.13039/501100010887).

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

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Received: 2022-01-09
Accepted: 2022-01-24
Published Online: 2022-02-15
Published in Print: 2022-04-26

© 2022 Xi-Shi Tai et al., published by De Gruyter, Berlin/Boston

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

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