Startseite Crystal structure of poly[aqua-(μ5-2,5-dicarboxybenzoato-κ5O:O:O′:O′′:O′′′)sodium(I)], C9H7NaO7
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Crystal structure of poly[aqua-(μ5-2,5-dicarboxybenzoato-κ5O:O:O′:O′′:O′′′)sodium(I)], C9H7NaO7

  • Cong-Kui Nie , Dan Zhao EMAIL logo und Ye Tian
Veröffentlicht/Copyright: 16. Dezember 2017

Abstract

C9H7NaO7, triclinic, P1̅ (no. 2), a = 7.0533(7) Å, b = 7.1238(7) Å, c = 10.5664(10) Å, α = 87.466(1)°, β = 83.003(1)°, γ = 66.690(1)°, V = 483.95(8) Å3, Z = 2, Rgt(F) = 0.0361, wRref(F2) = 0.0936, T = 296(2) K.

CCDC no.: 1560000

The asymmetric unit of the title crystal structure is shown in the figure. Tables 1 and 2 contain details on crystal structure and measurement conditions and a list of the atoms including atomic coordinates and displacement parameters.

Table 1:

Data collection and handling.

Crystal:Prism, colorless
Size:0.20 × 0.05 × 0.05 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:0.19 cm−1
Diffractometer, scan mode:Bruker SMART APEX-II, ω-scans
θmax, completeness:28.3°, >99%
N(hkl)measured, N(hkl)unique, Rint:6182, 2386, 0.026
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 1840
N(param)refined:155
Programs:Bruker programs [1], SHELX [2, 3]
Table 2:

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

AtomxyzUiso*/Ueq
Na10.77734(10)0.18226(10)0.08591(6)0.02528(19)
C10.1876(2)0.3076(2)0.72296(14)0.0179(3)
C20.3887(2)0.2866(2)0.74057(14)0.0183(3)
C30.5357(2)0.2566(2)0.63487(14)0.0199(3)
H30.67020.24020.64570.024*
C40.4824(2)0.2510(2)0.51276(14)0.0196(3)
C50.2830(3)0.2730(3)0.49619(15)0.0239(4)
H50.24790.26900.41460.029*
C60.1357(3)0.3011(3)0.60092(15)0.0225(3)
H60.00190.31550.58960.027*
C70.0304(2)0.3248(2)0.83580(14)0.0183(3)
C80.4412(2)0.3097(2)0.87183(14)0.0185(3)
C90.6376(3)0.2184(2)0.39754(15)0.0223(3)
O10.05394(18)0.18875(17)0.91401(10)0.0246(3)
O2−0.13675(18)0.49567(18)0.83874(11)0.0262(3)
H2−0.23160.51360.90980.031*
O30.59436(19)0.2156(2)0.29020(11)0.0327(3)
O40.82419(19)0.1925(2)0.42435(11)0.0320(3)
H40.92110.16820.35530.038*
O50.30587(18)0.45865(17)0.93593(10)0.0250(3)
O60.60837(18)0.18840(19)0.90681(11)0.0301(3)
O71.07454(19)0.13720(18)0.21125(11)0.0288(3)
H7B1.19070.03070.18100.035*
H7A1.10820.24390.19070.035*

Source of material

The title compound was prepared by the following procedure: a mixture of Na2CO3 (0.10 g) and 1,2,4-Tricarboxybenzene (0.30 g) was dissolved in 5 mL deionized water, which was then placed in a 30 mL Teflon-lined stainless steel autoclave. The autoclave was sealed and heated at 165 °C under autogenously pressure for seven days. After being slowly cooled to room temperature at a rate of 5 °C/h, some colorless prism shaped crystals were collected by filtration, and washed by distilled water.

Experimental details

The H atoms of C atoms were positioned geometrically and refined with a riding model, with C—H = 0.93 Å and Uiso(H) = 1.2Ueq(C). The H atoms of water and carboxyl were located in difference Fourier maps, and then refined with a riding model, with Uiso(H) = 1.2Ueq(O).

Discussion

During past twenty years, research interest in coordination polymers (CPs) is rapidly increasing not only owing to their versatile intriguing architectures and topologies but also for their potential applications in a variety of areas. Design and construction of CPs with specific architecture and useful properties still remain a significant challenge, because the construction of CPs will be influenced by many experimental and structural factors, such as the coordinating propensities of the ligands, the geometric preference of metal ions, relative stoichiometry of raw materials, reaction temperature and solvent systems. Moreover, weak non-covalent interactions such as hydrogen bonds, π–π and anion-π interactions also play an important role to determine the shape of the molecules and the crystal structures. The selection of suitable organic ligands is crucial for constructing extended coordination frameworks. 1,2,4-Tricarboxybenzene has been used extensively to construct a number of CPs, which usually display interesting electronic, optical and magnetic properties [4], [5], [6], [7].

Structure solution revealed that the title compound features a 3D framework with one Na+ cation, one 2,5-dicarboxybenzoato ligand and one coordinated aqua in each asymmetric unit. Each Na+ cation is 6-coordinated by five oxygen atoms of organic ligands and one aqua ligand into a NaO6 polyhedron with the Na–O distances ranging from 2.3462(13) to 2.5214(14) Å. The calculated total bond valence for Na(1) is 1.136, proving that the Na atom is in the reasonable value of +1 oxidation state [8]. The 2,5-dicarboxybenzoato ligand adopts a μ5 coordination mode connecting five Na+ cations (cf. the figure), to form the 3D framework.

Acknowledgements

I acknowledge support for the publication fee by the Science and Technology Research Project of Henan Province (No. 172102310678) and Key research project of Henan Province Office of Education (No. 17A150013).

References

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Received: 2017-9-22
Accepted: 2017-11-25
Published Online: 2017-12-16
Published in Print: 2018-1-26

©2018 Cong-Kui Nie et al., published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 License.

Artikel in diesem Heft

  1. Cover and Frontmatter
  2. Editorial 2018
  3. Crystal structure of dimethanol-bis{3-(((2-oxidonaphthalen-1-yl)methylene)amino)-2-oxo-2H-chromen-4-olato-κ3O,N:O′}dizinc(II), C42H30Zn2N2O10
  4. Crystal structure of aqua-bis{[2,6-dimethyl-N-(pyridin-2-ylmethylene)aniline-κ2N,N′]}zinc(II) triflate monohydrate [ZnC29H31N4O]CF3SO3⋅H2O
  5. Crystal structure of (E)-1-(4-{[(E)-4-Diethylamino-2-hydroxybenzene methylene]amino}phenyl)ethanone methoxy oxime, C20H27ClN3O3
  6. Crystal structure of (E)-1-(4-(((E)-4-(diethylamino)-2-hydroxybenzylidene)amino)phenyl)ethan-1-one oxime, C19H23N3O2
  7. Crystal structure of poly[(μ2-1,4-bis((2-ethyl-1H-benzo[d]imidazol-1-yl)methyl)benzene-κ2N:N′)-(μ2-4,4′-sulfonyldibenzoato-κ2O:O′)zinc(II)], C40H34N4O6SZn
  8. Crystal structure of catena-poly[diaqua(μ3-pyrazine-2,3-dicarboxylato-κ4O,N:O′:O′′)zinc(II)] 1.25 hydrate, C6H8.5N2O7.25Zn
  9. Crystal structure of fac-(acetylacetonato-κ2O,O′)tricarbonyl(tri-m-tolyl phosphane-κP)rhenium(I), C29H28O5PRe
  10. Crystal structure of bis(μ2-methanolato-κ2O:O)-bis(methanol-κ1O)-bis{3-((4-methoxy-2-oxidobenzylidene)amino)-2-oxo-2H-chromen-4-olato-κ3O,O′,N}dichromium(III), C38H36Cr2N2O14
  11. Crystal structure of poly[aqua-(μ3-pyridine-3,5-dicarboxylato-κ5O,O′:O′′,O′′′,N)zinc(II)], C7H7NO6Zn
  12. Crystal structure of bis((1-(((4-(((benzyloxy)imino)methyl)phenyl)imino)methyl)naphthalen-2-yl)oxy-κ2O,N)copper(II), C52H42CuN4O4
  13. Crystal structure of bis{5-(diethylamino)-2-(((2-oxo-2H-chromen-6-yl)imino)methyl)phenolato-κ2O,N}cobalt(II), C40H38CoN4O6
  14. Crystal structure of diaqua-bis(N,N-dimethylformamide-κ1O)-bis{3-((5-chloro-2-oxidobenzylidene)amino)-2-oxo-2H-chromen-4-olato-κ4N,O,O′:O′}dinickel(II), C38H34Ni2Cl2N4O12
  15. Crystal structure of tetrakis(methanol-κO)bis{3-((4-methoxy-2-oxidobenzylidene)amino)-2-oxo-2H-chromen-4-olato-κ3O,N,O′}bicobalt(II), C38H38Co2N2O14
  16. Crystal structure of (S)-tert-butyl-(1-hydroxypropan-2-yl)carbamate, C8H17NO3
  17. Crystal structure of 4-(4′-(pyridin-4-yl)-[1,1′-biphenyl]-4-yl)pyridin-1-ium catena-poly[{5-carboxy-4′-methyl-[1,1′-biphenyl]-3-carboxylato-κ2O,O′}-(μ2-4′-methyl-[1,1′-biphenyl]-3,5-dicarboxylato-κ4O,O′:O′′,O′′′)lead(II)], C52H40N2O9Pb
  18. Crystal structure of catena-poly[diaqua-(μ2-5-methylisophthalato-κ2O:O′)(μ2-1,4-bis((1H-1,2,4-triazol-1-yl)methyl)benzene-κ2N:N′)], NiC21H22O6N6
  19. Crystal structure of the salt tris(guanidinium) tris(tetrapropylammonium) bis(pyridine-2,4,6-tricarboxylate) – water (1/10), C55H126N14O22
  20. Crystal structure of 5-hydroxy-2-(4-hydroxy-3-methoxyphenyl)-3,7,8-trimethoxy-4H-chromen-4-one, C19H18O8
  21. Crystal structure of poly{[μ2-1,1′-(sulfonylbis(4,1-phenylene))bis(2-methyl-1H-imidazole)-κ2N:N′][μ2-4,4′-oxydibenzoato-κ2O:O′]cobalt(II)} hemihydrate, C34H27N4O7.5SCo
  22. The crystal structure of 25,27-(2,2′-[(2-thioxo-1,3-dithiole-4,5-diyl)disulfanediyl]diethanolate)-26,28-dihydroxycalix[4]arene — dichloromethane (1/1), C36H32Cl2O4S5
  23. The crystal structure of 1,2-bis(3-(pyridin-3-yl)-1,2,4-oxadiazol-5-yl)ethane, C16H12N6O2
  24. Crystal structure of 1-benzyl-3-((4-bromophenyl)amino)-4-(4-methoxyphenyl)-1H-pyrrole-2,5-dione, C24H19BrN2O3
  25. Crystal structure of bis(2-((allylcarbamothioyl)imino)-4-methylthiazol-3-ido-κ2N,S)palladium(II), C16H20N6PdS4
  26. Crystal structure of pyrimidine-2,5-dicarboxylic acid 1.5 hydrate, C12H14N4O11
  27. Crystal structure of trans-diaqua-bis(1H-pyrazole-3-carboxylato-κ2N,O)manganese(II), C8H10N4O6Mn
  28. Crystal structure of catena-(μ3-5-bromoisophthatato-κO,O′: O′′,O′′′′)-(1,2-bis(imidazol-1-yl)ethane-κN:N′)cobalt(II), C16H13CoN4O4Br
  29. Investigation of the compound La5Zn2−xPb1 + x (x = 0.20–0.32)
  30. Crystal structure of (OC-6-13)-diaqua-bis(3,5-di(pyridin-3-yl)-4H-1,2,4-triazol-4-amine-κ1N)-bis(dicyanamido-κ1N)zinc(II) tetrahydrate, ZnC28H32N18O6
  31. Crystal structure of Ga0.62(3)Sb0.38(3)Pd3
  32. Crystal structure of Ga0.47(1)Sb0.53(1)Pd2
  33. A derivative of the Corey lactone – crystal structure of (3aR,4S,5R,6aS)-4-(((tert-butyldimethylsilyl)oxy)methyl)-2-oxohexahydro-2H-cyclopenta[b]furan-5-yl benzoate, C21H30O5Si
  34. A Corey lactone: crystal structure of (3aR,4R,5R,6aS)-5-benzoyloxy-4(hydroxymethyl)hexahydro-2H-cyclopenta[b]furan-2-one, C15H16O5
  35. Hydrothermal synthesis and crystal structure of poly[aqua-(μ2-1,3-bis(4-pyridyl)propane-κ2N:N′)-(μ2-1,4,5,6,7,7-hexachlorobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylato-κ2O:O′)manganese(II) hydrate, C22H20Cl6N2O6Mn
  36. Crystal structure of 2-acetylpyrrole S-methylthiosemicarbazonium hydroiodide, C8H13IN4S
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  38. Crystal structure of poly[aqua-(μ5-2,5-dicarboxybenzoato-κ5O:O:O′:O′′:O′′′)sodium(I)], C9H7NaO7
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  43. Crystal structure of 3-(3-dimethylaminopropyl)-2,3-dihydro-2-thioxoquinazolin-4(1H)-one, C13H17N3OS
  44. The crystal structure of trans-tetraaqua-bis(p-tolylsulfinato-κO)calcium(II)), C14H22O8S2Ca
  45. The crystal structure of (E)-N′-(pyridin-2-ylmethylene)pyrazine-2-carbohydrazide, C11H9N5O
  46. Crystal structure of (E)-3-(pyren-1-yl)-1-(pyridin-4-yl)prop-2-en-1-one, C24H15NO
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  48. Crystal structure of 4-chloro-2-methyl-6-(4-(trifluoromethoxy)phenyl)pyrimidine, C12H8ClF3N2O
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  50. Crystal structure of methyl (Z)-2-(5-fluoro-2-oxoindolin-3-ylidene)hydrazine-1-carbodithioate, C10H8FN3OS2
  51. Crystal structure of tert-butyl (Z)-4-(2-(5-methoxy-3-(2-((methylthio)carbonothioyl)hydrazono)-2-oxoindolin-1-yl)ethyl)piperazine-1-carboxylate, C22H31N5O4S2
  52. The crystal structure of (E)-2-((2-(o-tolylcarbamothioyl)hydrazono)methyl)benzoic acid, C16H15N3O2S
  53. Crystal structure of 2-chloro-1,3-di-tert-pentyl-4,4-diphenyl-1,3,2λ3,4-diazaphosphasiletidine, C22H32ClN2PSi
  54. Crystal structure of tetramethyl 5,5′-(buta-1,3-diyne-1,4-diyl)diisophthalate, C24H18O8
  55. Crystal structural of 2-amino-4-(4-methoxyphenyl)-3-cyano-7,7-dimethyl-5-oxo-4H-5,6,7,8-tetrahydrobenzo[b]pyran, C19H20N2O3
  56. Crystal structure of 1,3,5-tris((trimethylsilyl)methyl)-1,3,5-triazinane-2,4,6-trione, C15H33N3O3Si3
  57. The crystal structure of bis(2-benzoyl-5-hydroxylphenolato-κ2O,O′)copper(II), C26H18CuO6
  58. Crystal structure of 2,6-bis(3-(pyrazin-2-yl)-1H-1,2,4-triazol-5-yl)pyridine – 1-ethyl-3-methyl-1H-imidazol-3-ium bromide (1/1), C23H22N13Br
  59. The crystal structure of (E)-N-benzyl-N′-benzylidene-4-methylbenzenesulfonohydrazide, C21H20N2O2S
  60. Crystal structure of ethyl (E)-5-((2-(3-hydroxybenzoyl)hydrazono)methyl)-3,4-dimethyl-1H-pyrrole-2-carboxylate – water – ethanol (1/1/1), C19H27N3O6
  61. The crystal structure of (E)-4-(3-ethoxy-2-hydroxybenzylideneamino)benzoic acid, C16H15NO4
  62. Crystal structure of (μ2-N,N′-bis((pyridin-4-yl)methyl)ethanediamide-κ2N:N′)-tetrakis(diethylcarbamodithioato-κ2S,S′)dizinc(II), C34H54N8O2S8Zn2
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