Abstract
C10H14N3O5SNa, triclinic,
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.

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] |
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].
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
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Author contributions: All the authors have accepted responsibility for the entire content of this submitted manuscript and approved submission.
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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).
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Conflict of interest statement: The authors declare no conflicts of interest regarding this article.
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© 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.
Articles in the same Issue
- Frontmatter
- New Crystal Structures
- Crystal structure of {2,2′-{cyclohexane-1,2-diylbis[(azanylylidene)methylylidene]}bis(2,4-dibromophenolato)-κ4 N,N′,O,O′}copper(II) ─ diethylformamide (1/1), C23H23Br4CuN3O3
- The crystal structure of 2-(2-methyl-6-phenyl-4H-pyran-4-ylidene)-1H-indene-1,3(2H)-dione, C21H14O3
- Crystal structure of bis((1-methylbenzimidazol-2-yl)methyl)amine, C18H19N5
- Crystal structure of (E)-N′-(1-(2-hydroxy-4-methoxyphenyl)ethylidene) isonicotinohydrazide, C15H15N3O3
- Crystal structure of 2-((4-phenyl-5-(pyridin-4-yl)-4H-1,2,4-triazol-3-yl)thio)acetonitrile, C15H11N5S
- The crystal structure of 2,2′-((1E,1′E)-hydrazine-1,2-diylidenebis(methaneylylidene))bis(4-chlorophenol), C14H10Cl2N2O2
- Dichlorido-{2,6-bis(4,5-dihydro-1H-pyrazol-3-yl)pyridine-κ3 N,N′,N″}zinc(II), C11H9C12N5Zn
- The crystal structure of dichlorido-(2-((4-phenyl-2H-1,2,3-triazol-2-yl)methyl)pyridine-κ2N,N′)palladium(II), C14H12Cl2N4Pd
- The crystal structure of 1-(N1-benzyl-2-methyl-4-nitro-imidazol-5-yl)-4-(prop-2-yn-1-yl) piperazine, C18H21N5O2
- Crystal structure of (μ4-(1,2,4,5-tetra(1,2,4-triazol-1-ylmethyl)-benzene-κ4N:N1:N2:N3)disilver(I) diperchlorate
- The crystal structure of 1-(2-bromoethane)-4-amine-3,5-dinitropyrazole, C5H6Br1N5O4
- Crystal structure of (E)-1-(4-benzyl-3,5-dioxomorpholin-2-ylidene)ethyl acetate, C15H15N1O5
- The crystal structure of poly[diaqua-(μ2-1,2,4,5-tetrakis(1,2,4-triazol-1-ylmethyl)-benzene-κ2N:N′)-bis(μ3-terephthalato-κ3O:O′:O′′)dicadmium(II)], C17H15N6O5Cd
- Crystal structure of (E)-N′-(1-(5-chloro-2-hydroxyphenyl) ethylidene)thiophene-2-carbohydrazide, C13H11ClN2O2S
- The crystal structure of [(2,2′-bipyridine-k2 N,N)-bis(6-phenylpyridine-2-carboxylato-k2 N,O)cobalt(II)]-monohydrate, C36H26N4O5Co
- Crystal structure of (E)-N′-(2-chloro-6-hydroxybenzylidene)-3-hydroxybenzo-hydrazide monohydrate, C14H13ClN2O4
- Crystal structure of 1,1′-(methylene)bis(pyridin-1-ium) bis(1,2-dicyanoethene-1,2-dithiolato-κ2S:S)nickel(II), C42H30N14Ni2S8
- Crystal structure of 1,1′-(1,2-ethanediyl)bis(pyridin-1-ium) bis(1,2-dicyanoethene-1,2-dithiolato-κ2 S:S)nickel(II), C20H14N6NiS4
- The crystal structure of 1-methyl-1H-pyrazol-2-ium nitrate, C4H7O3N3
- The crystal structure of 4,4′-diselanediylbis(8-(hexyloxy)-3,6-dimethyl-1-(piperidin-1-yl)isoquinoline-7-carbonitrile), C46H60N6O2Se2
- The crystal structure of tris(6-methylpyridin-2-yl)phosphine selenide, C18H18N3PSe
- The crystal structure of 1,2-bis(2,4-dinitro-1H-imidazol-1-yl)ethane ─ acetone (1/1), C11H12N8O9
- Crystal structure of [diaqua[2,2′-(1,2-phenylene)bis(1H-imidazole-4-carboxylato-5-carboxy)-κ4N,N′,O,O′]nickel(II)] tetrahydrate, C16H12N4NiO10·4H2O
- The crystal structure of tris(4-methyl-1H-pyrazol-1-yl)methane, C13H16N6
- The crystal structure of 5,6-dichloro-2-(quinolin-8-yl)isoindoline-1,3-dione, C17H8Cl2N2O2
- Crystal structure of (E)-(2-methoxy-benzylidene)-(4-[1,2,4]triazol-1-yl-phenyl)-amine, C16H14N4O
- The crystal structure of (Z)-2-(4-(4-bromophenyl)thiazol-2-yl)-4-(3-hydroxybut-2-enoyl)-5-methyl -1,2-dihydro-3H-pyrazol-3-one – methanol (1/1), C18H18N3O4S
- Crystal structure of tetraaqua-tris(nitrato-κ2 O,O′) erbium(III) monohydrate, Er(NO3)3·5H2O, H10ErN3O14
- The crystal structure of 1-methyl-2-nitro-1H-imidazole 3-oxide, C4H5N3O3
- The crystal structure of 1-methyl-2-nitroimidazole, C4H5N3O2
- The crystal structure of 2-carboxyl-4-nitroimidazole monohydrate, C4H5N3O5
- Crystal structure of bis[hydrido-hexaphenylcarbodiphosphoran][tetra-trifluoromethyl-(μ-diiodo)-diplatinat]
- The crystal structure of poly[μ2-aqua- aqua-(μ3-(E)-2-(4-((2-carbamothioylhydrazineylidene)methyl)phenoxy)acetato-κ3 O:S:S)sodium(I)], C10H14N3O5SNa
- The twinned crystal structure of [4,4′-bipyridine]-1,1′-diium hexachloridostannate(IV), C10H10N2SnCl6
- The crystal structure of [(2,2′-bipyridine-k2 N,N)-bis(6-phenylpyridine-2-carboxylate-k2 N,O)copper(II)], C34H24N4O4Cu
- Crystal structure of trans-1,2-bis(pyridinium-4-yl) ethylene bis(2-carboxy-4-bromobenzoate) – water (1/4), C14H14BrNO6
- Crystal structure of poly[diaqua-(μ3-fumarato)-(μ3-maleato)-(μ4-1,2,4,5-tetrakis((1H-1,2,4-triazol-1-yl)methyl)benzene)tetracadmium(II)] dihydrate, C34H32N12O9Cd4
- Crystal structure of a second modification of Pachypodol, C18H16O7
- Crystal structure of methyl 2-(4-(2-(cyclopentyl-amino)-1-(N-(4-methoxyphenyl)-1-methyl-5-phenyl-1-H-pyrazole-3-carboxamido)-2-oxoethyl)phenyl)acetate, C34H36N4O5
- The crystal structure of catena-poly[(m2-4,4′-bipyridine-κ2 N:N)-bis(6-phenylpyridine-2-carboxylato-κ2 N,O) zinc(II)], C34H24N4O4Zn
- The crystal structure of hexaquamagnesium(II) (2,4-bis(nitroimino)-6-oxo-1,3,5-triazinane-1,3-diide), C3H15MgN7O12
- The crystal structure of 7-Bromo-2-(4-chloro-phenyl)-quinoxaline, C14H9BrClN2
- Crystal structure of methyl 4-{[4-(4-cyanobenzamido)phenyl]amino}benzofuro[2,3-d]pyrimidine-6-carboxylate, C26H17N5O4
- The crystal structure of (4SR)-7-(3,4-dichlorobenzyl)-4,8,8-trimethyl-7,8-dihydroimidazo[5,1c][1,2,4]triazine-3,6(2H,4H)-dione, C15H16Cl2N4O2
- Crystal structure of catena-poly[{μ2-3-carboxy-2,3-bis((4-methylbenzoyl)oxy)propanoato-κ2 O:O′}tris(methanol-κ1 O)lanthanum(III)], C63H63LaO27
Articles in the same Issue
- Frontmatter
- New Crystal Structures
- Crystal structure of {2,2′-{cyclohexane-1,2-diylbis[(azanylylidene)methylylidene]}bis(2,4-dibromophenolato)-κ4 N,N′,O,O′}copper(II) ─ diethylformamide (1/1), C23H23Br4CuN3O3
- The crystal structure of 2-(2-methyl-6-phenyl-4H-pyran-4-ylidene)-1H-indene-1,3(2H)-dione, C21H14O3
- Crystal structure of bis((1-methylbenzimidazol-2-yl)methyl)amine, C18H19N5
- Crystal structure of (E)-N′-(1-(2-hydroxy-4-methoxyphenyl)ethylidene) isonicotinohydrazide, C15H15N3O3
- Crystal structure of 2-((4-phenyl-5-(pyridin-4-yl)-4H-1,2,4-triazol-3-yl)thio)acetonitrile, C15H11N5S
- The crystal structure of 2,2′-((1E,1′E)-hydrazine-1,2-diylidenebis(methaneylylidene))bis(4-chlorophenol), C14H10Cl2N2O2
- Dichlorido-{2,6-bis(4,5-dihydro-1H-pyrazol-3-yl)pyridine-κ3 N,N′,N″}zinc(II), C11H9C12N5Zn
- The crystal structure of dichlorido-(2-((4-phenyl-2H-1,2,3-triazol-2-yl)methyl)pyridine-κ2N,N′)palladium(II), C14H12Cl2N4Pd
- The crystal structure of 1-(N1-benzyl-2-methyl-4-nitro-imidazol-5-yl)-4-(prop-2-yn-1-yl) piperazine, C18H21N5O2
- Crystal structure of (μ4-(1,2,4,5-tetra(1,2,4-triazol-1-ylmethyl)-benzene-κ4N:N1:N2:N3)disilver(I) diperchlorate
- The crystal structure of 1-(2-bromoethane)-4-amine-3,5-dinitropyrazole, C5H6Br1N5O4
- Crystal structure of (E)-1-(4-benzyl-3,5-dioxomorpholin-2-ylidene)ethyl acetate, C15H15N1O5
- The crystal structure of poly[diaqua-(μ2-1,2,4,5-tetrakis(1,2,4-triazol-1-ylmethyl)-benzene-κ2N:N′)-bis(μ3-terephthalato-κ3O:O′:O′′)dicadmium(II)], C17H15N6O5Cd
- Crystal structure of (E)-N′-(1-(5-chloro-2-hydroxyphenyl) ethylidene)thiophene-2-carbohydrazide, C13H11ClN2O2S
- The crystal structure of [(2,2′-bipyridine-k2 N,N)-bis(6-phenylpyridine-2-carboxylato-k2 N,O)cobalt(II)]-monohydrate, C36H26N4O5Co
- Crystal structure of (E)-N′-(2-chloro-6-hydroxybenzylidene)-3-hydroxybenzo-hydrazide monohydrate, C14H13ClN2O4
- Crystal structure of 1,1′-(methylene)bis(pyridin-1-ium) bis(1,2-dicyanoethene-1,2-dithiolato-κ2S:S)nickel(II), C42H30N14Ni2S8
- Crystal structure of 1,1′-(1,2-ethanediyl)bis(pyridin-1-ium) bis(1,2-dicyanoethene-1,2-dithiolato-κ2 S:S)nickel(II), C20H14N6NiS4
- The crystal structure of 1-methyl-1H-pyrazol-2-ium nitrate, C4H7O3N3
- The crystal structure of 4,4′-diselanediylbis(8-(hexyloxy)-3,6-dimethyl-1-(piperidin-1-yl)isoquinoline-7-carbonitrile), C46H60N6O2Se2
- The crystal structure of tris(6-methylpyridin-2-yl)phosphine selenide, C18H18N3PSe
- The crystal structure of 1,2-bis(2,4-dinitro-1H-imidazol-1-yl)ethane ─ acetone (1/1), C11H12N8O9
- Crystal structure of [diaqua[2,2′-(1,2-phenylene)bis(1H-imidazole-4-carboxylato-5-carboxy)-κ4N,N′,O,O′]nickel(II)] tetrahydrate, C16H12N4NiO10·4H2O
- The crystal structure of tris(4-methyl-1H-pyrazol-1-yl)methane, C13H16N6
- The crystal structure of 5,6-dichloro-2-(quinolin-8-yl)isoindoline-1,3-dione, C17H8Cl2N2O2
- Crystal structure of (E)-(2-methoxy-benzylidene)-(4-[1,2,4]triazol-1-yl-phenyl)-amine, C16H14N4O
- The crystal structure of (Z)-2-(4-(4-bromophenyl)thiazol-2-yl)-4-(3-hydroxybut-2-enoyl)-5-methyl -1,2-dihydro-3H-pyrazol-3-one – methanol (1/1), C18H18N3O4S
- Crystal structure of tetraaqua-tris(nitrato-κ2 O,O′) erbium(III) monohydrate, Er(NO3)3·5H2O, H10ErN3O14
- The crystal structure of 1-methyl-2-nitro-1H-imidazole 3-oxide, C4H5N3O3
- The crystal structure of 1-methyl-2-nitroimidazole, C4H5N3O2
- The crystal structure of 2-carboxyl-4-nitroimidazole monohydrate, C4H5N3O5
- Crystal structure of bis[hydrido-hexaphenylcarbodiphosphoran][tetra-trifluoromethyl-(μ-diiodo)-diplatinat]
- The crystal structure of poly[μ2-aqua- aqua-(μ3-(E)-2-(4-((2-carbamothioylhydrazineylidene)methyl)phenoxy)acetato-κ3 O:S:S)sodium(I)], C10H14N3O5SNa
- The twinned crystal structure of [4,4′-bipyridine]-1,1′-diium hexachloridostannate(IV), C10H10N2SnCl6
- The crystal structure of [(2,2′-bipyridine-k2 N,N)-bis(6-phenylpyridine-2-carboxylate-k2 N,O)copper(II)], C34H24N4O4Cu
- Crystal structure of trans-1,2-bis(pyridinium-4-yl) ethylene bis(2-carboxy-4-bromobenzoate) – water (1/4), C14H14BrNO6
- Crystal structure of poly[diaqua-(μ3-fumarato)-(μ3-maleato)-(μ4-1,2,4,5-tetrakis((1H-1,2,4-triazol-1-yl)methyl)benzene)tetracadmium(II)] dihydrate, C34H32N12O9Cd4
- Crystal structure of a second modification of Pachypodol, C18H16O7
- Crystal structure of methyl 2-(4-(2-(cyclopentyl-amino)-1-(N-(4-methoxyphenyl)-1-methyl-5-phenyl-1-H-pyrazole-3-carboxamido)-2-oxoethyl)phenyl)acetate, C34H36N4O5
- The crystal structure of catena-poly[(m2-4,4′-bipyridine-κ2 N:N)-bis(6-phenylpyridine-2-carboxylato-κ2 N,O) zinc(II)], C34H24N4O4Zn
- The crystal structure of hexaquamagnesium(II) (2,4-bis(nitroimino)-6-oxo-1,3,5-triazinane-1,3-diide), C3H15MgN7O12
- The crystal structure of 7-Bromo-2-(4-chloro-phenyl)-quinoxaline, C14H9BrClN2
- Crystal structure of methyl 4-{[4-(4-cyanobenzamido)phenyl]amino}benzofuro[2,3-d]pyrimidine-6-carboxylate, C26H17N5O4
- The crystal structure of (4SR)-7-(3,4-dichlorobenzyl)-4,8,8-trimethyl-7,8-dihydroimidazo[5,1c][1,2,4]triazine-3,6(2H,4H)-dione, C15H16Cl2N4O2
- Crystal structure of catena-poly[{μ2-3-carboxy-2,3-bis((4-methylbenzoyl)oxy)propanoato-κ2 O:O′}tris(methanol-κ1 O)lanthanum(III)], C63H63LaO27