Home Physical Sciences The crystal structure of a cobalt-vanadium-oxido hydrate
Article Open Access

The crystal structure of a cobalt-vanadium-oxido hydrate

  • ORCID logo EMAIL logo , , , and
Published/Copyright: September 18, 2023

Abstract

H4O14CoV4.4, monolinic, P2/m (no. 10), a = 8.1091(8) Å, b = 3.5128(2) Å, c = 9.7590(9) Å, β = 111.553(11)°, V = 258.55(4) Å3, Z = 1, R gt (F) = 0.0401, wR ref (F2) = 0.0922, T = 293(2) K.

CCDC no.: 2292462

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: Brown needle
Size: 0.36 × 0.03 × 0.02 mm
Wavelength: Mo Kα radiation (0.71073 Å)
μ: 5.47 mm−1
Diffractometer, scan mode: New Xcalibur, ω
θmax, completeness: 29.1°, >99 %
N(hkl)measured, N(hkl)unique, Rint: 1232, 708, 0.028
Criterion for Iobs, N(hkl)gt: Iobs > 2σ(Iobs), 621
N(param)refined: 67
Programs: CrysAlisPRO [1], Olex2 [2], SHELX [3]
Table 2:

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

Atom x y z Uiso*/Ueq
Co1 1.0000 1.0000 1.0000 0.0117 (3)
V1 0.24584 (13) 0.5000 0.83517 (12) 0.0085 (3)
V2 0.54861 (14) 1.0000 0.81158 (12) 0.0091 (3)
V3a 0.5000 0.5000 0.5000 0.0092 (7)
O1 0.5177 (6) 0.5000 0.8597 (5) 0.0148 (8)
O2 0.3278 (5) 1.0000 0.8811 (5) 0.0125 (8)
O3 0.7663 (6) 1.0000 0.8447 (5) 0.0144 (8)
O4 0.0792 (5) 0.5000 0.9009 (5) 0.0133 (8)
O5 0.1469 (6) 0.5000 0.6596 (5) 0.0176 (9)
O6 0.4616 (6) 1.0000 0.6332 (5) 0.0230 (9)
O7 0.2285 (8) 0.5000 0.4023 (6) 0.0387 (14)
H7A 0.168 (11) 0.5000 0.455 (9) 0.058*
H7B 0.187 (10) 0.5000 0.312 (2) 0.058*
  1. aOccupancy: 0.4.

1 Source of materials

A mixture containing (NH4)VO3 (3.850 g), CoSO4·6H2O (2.750 g), 1,10-phenanthroline (C12H8N2), (2.650 g), and deionized water (H2O) (18.0 mL), with pH value ∼8.0, was prepared by mixing these components and sealed in a 30 mL Teflon-lined stainless steel autoclave (75 % of the total volume of the autoclave). Then, the resulting slurry was heated to 433 K in an oven and maintained at the temperature for five days. Then, the dark brown purity-phase crystals of the title compound (about 42 % yield based on Co) were obtained. The results of elemental analyses provided the chemical compositions: (wt%) for the title compound: H, 1.06; O, 44.24; Co, 10.67; V, 44.03 (in contrast, anal. calcd. (wt%): H, 0.78; O, 43.83; Co, 11.53; V, 43.86).

2 Experimental details

Coordinates of hydrogen atoms were refined without any constraints or restraints.

3 Comment

Inorganic porous materials with high surface area and diverse pore structures as well its unique physicochemical properties, such as adsorption performance, chemical stability and thermostability, are endowed with wide range of industrial applications [4], [5], [6], [7]. With the rapid development of science and technology, the application of inorganic porous materials in many fields has also shown a more extensive and in-depth trend, including but not limited to catalysis, separation, gas storge, sensing, electrochemistry, energy conversion and so on [8, 9]. Therefore, the development of new structural inorganic porous materials and the exploitation of its applications will be of a great significance work. At present, the research of inorganic porous materials mainly focus on the improvement of preparation methods exploring the relationship between structure and performances, and the exploration of new application fields [10], [11], [12].

Single-crystal X-ray diffraction structure study reveals that the title compound has open 3D-network structure. The asymmetric unit of the compound contains dimeric V–O polyanion, [V2O6]2−, bridging Co2+ cation and bridging [V(H2O] unit. Dimeric [V2O6]2− polyanion is made up of two similar triangle pyramidal building units, [VO3], via two-bridging oxygen atoms. The V atoms in [V2O6]2− are in five-coordinated state and show tetragonal-pyramidal configuration, [VO5], with the bond distances (V–O) of 1.603(5) – 2.125(4) Å for V(1) and 1.624(5) – 2.134(4) Å for V(2). The O–V–O bond angles in [V2O6]2− are in the range of 73.22(13) – 153.3(2)°. The other bridging vanadium atom, V(3) is in six-coordinated state with bond distances (V–O) of 2.053(6) – 2.274(3) Å and the O–V–O bond angles in the range of 78.85(16) – 180.0°. The Co atoms in the title compound are also in six-coordinated state with the [CoO6] unit showing a deformed octahedral configuration, the bond lengths (Co–O) vary in the range of 1.945(5) – 2.211(3) Å, and the O–Co–O band angles in the range of 74.81(17) – 180.0°. The 3D title compound displays a ordered mesoporous structure with the aperture about 20 nm, viewed along b-axis. Bond valence calculations (BVS) [13] on V(1), V(2), V(3) and Co(1) sites afford values of 5.131, 5.185, 5.345 and 1.996, respectively.


Corresponding author: Chen Wu-Hua, College of Chemistry and Material Science, Fujian Provincial Colleges and University Engineering, Research Center of Solid Waste Resource Utilization, Longyan University, Longyan 364012, Fujian Province, People’s Republic of China, E-mail:

Funding source: The Natural Science Foundation of Fujian Province

Award Identifier / Grant number: 2022H0050

Funding source: The Longyan Qimai Science and Technology Innovation Foundation of Wuping County

Award Identifier / Grant number: 2022WPQM05

  1. Research funding: This work was funded by The Natural Science Foundation of Fujian Province (2022H0050) and The Longyan Qimai Science and Technology Innovation Foundation of Wuping County (2022WPQM05).

References

1. Oxford Diffraction Ltd. CrysAlisPRO; Oxford Diffraction Ltd.: Abingdon, Oxfordshire, England, 2015.Search in Google Scholar

2. Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K., Puschmann, H. OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Crystallogr. 2009, 42, 339–341; https://doi.org/10.1107/s0021889808042726.Search in Google Scholar

3. Sheldrick, G. M. SHELXTL – integrated space-group and crystal-structure determination. Acta Crystallogr. 2015, A71, 3–8; https://doi.org/10.1107/s2053273314026370.Search in Google Scholar PubMed PubMed Central

4. Selvam, T., Machoke, A., Schwieger, W. Supported ionic liquids on non-porous and porous inorganic materials–a topical review. Appl. Catal. A 2012, 445–446, 92–101; https://doi.org/10.1016/j.apcata.2012.08.007.Search in Google Scholar

5. Yu, X., Li, C., Ma, Y., Li, D., Li, H., Guan, X., Yan, Y., Valtchev, V., Qiu, S., Fang, Q. Crystaline, porous, covalent polyoxometalate-organic frameworks for lithium-ion batteries. Microporous Mesoporous Mater. 2020, 299, 110105; https://doi.org/10.1016/j.micromeso.2020.110105.Search in Google Scholar

6. Meng, X., Wang, S.-Y., Song, S.-Y., Zhang, H.-J. Proton-conducting crystalline porous materials. Chem. Soc. Rev. 2017, 46, 464–480; https://doi.org/10.1039/c6cs00528d.Search in Google Scholar PubMed

7. Dong, J., Wee, V., Peh, S. B., Zhao, D. Molecular-rotor-driven advanced porous materials. Angew. Chem. Int. Ed. 2021, 60, 2–16; https://doi.org/10.1002/anie.202101646.Search in Google Scholar PubMed

8. Diab, M., Mokari, T. Bioinspired hierarchical porous structures for engineering advanced functional inorganic materials. Adv. Mater. 2018, 30, 1706349; https://doi.org/10.1002/adma.201706349.Search in Google Scholar PubMed

9. Boissiere, C., Grosso, D., Chaumonnot, A., Nicole, L., Sanchez, C. Aerosol route to functional nanostructured inorganic and hybrid porous materials. Adv. Mater. 2011, 23, 599–623; https://doi.org/10.1002/adma.201001410.Search in Google Scholar PubMed

10. Bennett, T. D., Coudert, F.-X., James, S. L., Cooper, A. I. The changing state of porous materials. Nat. Mater. 2021, 20, 1179–1187; https://doi.org/10.1038/s41563-021-00957-w.Search in Google Scholar PubMed

11. Yu, J., Corma, A., Li, Y. Functional porous materials chemistry. Adv. Mater. 2020, 32, 2006277; https://doi.org/10.1002/adma.202006277.Search in Google Scholar PubMed

12. Canossa, S., Wuttke, S. Functionalization chemistry of porous materials. Adv. Funct. Mater. 2020, 30, 2003875; https://doi.org/10.1002/adfm.202003875.Search in Google Scholar

13. Brese, N. E., O’Keeffe, M. Bond-valence parameters for solids. Acta Crystallogr. 1991, B47, 192–197; https://doi.org/10.1107/s0108768190011041.Search in Google Scholar


Supplementary Material

This article contains supplementary material (https://doi.org/10.1515/ncrs-2023-0321).


Received: 2023-07-12
Accepted: 2023-09-02
Published Online: 2023-09-18
Published in Print: 2023-12-15

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

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

Articles in the same Issue

  1. Frontmatter
  2. New Crystal Structures
  3. Crystal structure of bis(dimethylammonium) poly[(μ4-1,1′-(1,4-phenylenebis(methylene))bis(1H-pyrazole-3,5-dicarboxylato))-κ6O1, N2:O2:O3:O1′,N2′]nickel (II)], C22H26N6NiO8
  4. Hydrothermal synthesis and crystal structure of catena-poly[diaqua-bis(μ2-4-((pyridin-4-ylmethyl)amino)benzoato-κ2N:O)cobalt(II)] 4,4′-bipyridine – water (1/2/2)
  5. Crystal structure of (2S,3S,4S,5S, Z)-2,3,5,6-tetrakis(benzyloxy)-4-hydroxyhexanal oxime, C34H37NO6
  6. The crystal structure of hexakis(3-thiophenecarboxylato-κ2O,O″)-bis(1,10-phenanthroline-κ2N,N′) trimanganese(II), C54H34N4O12S6Mn3
  7. Crystal structure of catena-poly[(μ2-1,4-di(pyridin-4-yl)benzene-κ2N:N′)-(4-bromobenzoate-κ2O:O′)-(μ-2-bromobenzoate-κ2O,O′)nickel(II)] – water (2/1), C30H21Br2N2NiO4.5
  8. The crystal structure of poly[(μ3-1,3-phenylenedioxydiacetate-κ5O,O,O′,O″,O‴)-bis(4′-(4-(1H-imidazol-1-yl)phenyl)-4,2′:6′,4″-terpyridine-kN) cadmium(II)], C58H42CdN10O6
  9. The crystal structure of 5-chloro-6′-methyl-3-(4-(methylsulfonyl)phenyl)-[2,3′-bipyridin]-1′-ium 4-methylbenzenesulfonate
  10. Crystal structure of poly[(μ-benzoato)-(μ-cis-4–hydroxy-D-proline)lithium], C12H14LiNO5
  11. The crystal structure of catena-poly[aqua-(4-iodopyridine-2,6-dicarboxylato-κ3N,O,O)-copper(II)] monohydrate, C7H6NO6ICu
  12. The crystal structure of catena-[diaqua-(4-acetylphenoxyacetato-κ2O,O)-bis(4-acetylphenoxyacetato-κ3O,O:O)-dihydrate-lanthanum(III)]–4,4′-bipyridine (2/1), C35H35NO14La
  13. The crystal structure of catena-poly[(4-iodopyridine-2,6-dicarboxylato-κ4 O,N,O′,O′′)(4-imidazol-1-yl-pyridine-κN)copper(II)], C15H9N4O4ICu
  14. Crystal structure of polybis(μ 4-3,5-dicarboxylatopyrazol-1-yl)-bis(N,N-dimethylformamide)tri-copper(II)–acetonitrile (1/2), C20H22Cu3N8O10
  15. Crystal structure of poly[(μ2-5-hydroxy-isophthalato-κ4O,O′:O″,O‴)-(μ2-1,5-bis(imidazol-2-methyl)pentane-κ2N:N′)cadmium(II)], C21H24CdN4O5
  16. The crystal structure of poly[bis(μ2-1,4-bi(1-imidazolyl)benzene-κ2N:N′)bis(μ2-4,4′-methylenebis(3-hydroxy-2-naphthoate)-κ2O:O′)cobalt(II)], C35H24CoN4O6
  17. The crystal structure of a cobalt-vanadium-oxido hydrate
  18. The crystal structure of catena-poly[(μ 2-2H-1,2,3-triazole-4,5-dicarboxylato-κ 2 O, O′)-(μ 2-1,3-bis((1H-imidazol-1-yl)methyl)benzene-κ 2 N,N′) zinc(II)], C18H15N7O4Zn
  19. Crystal structure of poly[diaqua-(bis(m2-1,4-bis(imidazol-1-ylmethyl)benzene)-κ2N,N′-manganese] dichloride, C28H32MnN8O2Cl2
  20. The crystal structure of 9,10-dimethoxy-5,6-dihydro-[1,3]dioxolo[4,5-g]isoquinolino [3,2-a]isoquinolin-7-ium (E)-3-(4-nitrophenyl)acrylate pentahydrate, C29H34N2O13
  21. Crystal structure of poly[(μ6-ammoniotris(methylene))tris(hydrogen phosphonato)cadmium(II)], C3H10CdNO9P3
  22. Crystal structure of Zn2[(1,1′-(hexane-1,6-diyl)bis(3-(pyridin-3-yl)urea))·(H2O)2·(DMF)2·(SO4)2], C24H50N8O18S2Zn2
  23. The crystal structure of 2-anilino-1,4-naphthoquinone, C10H11NO2
  24. Crystal structure of (E)-2-(2-(4-(diethylamino)styryl)-1-ethyl-1,4-dihydroquinolin-4-yl) malononitrile, C26H26N4
  25. Crystal structure of ethyl 2-((2,6-dichloro-4-(cyanomethyl)phenyl) amino)benzoate, C17H14Cl2N2O2
  26. Synthesis and crystal structure of 2-(3-oxo-3-phenylpropyl)isoindoline-1,3-dione, C17H13NO3
  27. The crystal structure of bis(acetonitrile-κ1N)tetrakis(μ2-2,6-difluorobenzoato-κ2O:O′)rhodium(II) (Rh–Rh), C32H18F8O8N2Rh2
  28. The crystal structure of a new polymorph of 6-hydroxy-2-naphthoic acid, C11H8O3
  29. The crystal structure of [(8-carboxymethoxy-quinoline-2-carboxylate-κ4N,O,O,O)-2,2′-bipyridine-κ2N-copper(II)] tetrahydrate, C22H23N3O9Cu
  30. The crystal structure of ethyl 4-hydroxy-2-(4-methoxyphenyl)-5-oxo-1-(2-oxo-2H-chromen-6-yl)-2,5-dihydro-1H-pyrrole-3-carboxylate, C23H19NO7
  31. Crystal structure of 7-hydroxy-3,4-dihydronaphthalen-1(2H)-one, C10H10O2
  32. Crystal structure of bis(tetrapropylammonium) dodecacarbonyltetratelluridotetraferrate(2-), (Pr4N)2[Fe4Te4(CO)12]
  33. The crystal structure of poly[bis(μ2−3−aminopyridine−4−carboxylatoκ2N:O)Zinc(II)], [Zn(C6H5N2O2)2] n
  34. The crystal structure of methyl 5-nitro-2-(tosyloxy)benzoate, C15H13NO7S
  35. The crystal structure of 18-crown-6 ― tetraaqua-dichlorido-di-μ2-chloridodicopper(II) (2/1), C12H32O10Cu2Cl4
  36. Crystal structure of 6,6a,7,8,9,10-hexahydro-5H-pyrazino [2,3-e]pyrido[1,2-a]pyrazine, C10H14N4
  37. Crystal structure of catena-poly-{diaqua-bis[μ-(((4-chlorophenyl)sulfonyl)glycinato-κO)](μ2-4, 4′-bipyridine-κ2N:N′)cobalt(II)} dihydrate, C26H30Cl2CoN4O12S2
  38. Crystal structure of bis{N′-[1,3-diphenylprop-2-en-1-ylidene]-N-phenylcarbamohydrazonothioato}zinc(II), C44H36N6S2Zn
  39. Crystal structure of tetraaqua-bis(((4-chlorophenyl)sulfonyl)glycinato-κO)cobalt(II) dihydrate, C16H26Cl2CoN2O14S2
  40. Crystal structure of 2-(5-phenyl-1-(quinolin-2-yl)-4,5-dihydro-1H-pyrazol-3-yl)phenol, C24H19N3O
  41. Crystal structure of 2-((2-fluoro-4-(trifluoromethyl)phenyl)(hydroxy)methyl)-7-methoxy-3,4-dihydronaphthalen-1((2H))-one, C19H16F4O3
  42. Crystal structure of 2-amino-4-(2-fluoro-3-(trifluoromethyl)phenyl)-9-methoxy-1,4,5,6-tetrahydrobenzo[h]quinazolin-3-ium chloride, C20H18ClF4N3O
  43. Crystal structure of (2-phenylimino methylquinoline-κ 2 N,N′)-bis(1–phenylpyrazole-κ 2 C,N)-iridium(III) hexafluorophosphate, C34H26F6IrN6P
  44. Crystal structure of (3-hydroxy-4-methoxyphenyl)(pyrrolidin-1-yl)methanone, C12H15NO3
  45. The crystal structure of bis(trimethylsulfoxonium) catena-poly[µ2-hexabromido-indium(III)sodium(I)] C6H18O2S2NaInBr6
  46. Crystal structure of N-cyclopropyl-3-hydroxy-4-methoxybenzamide, C11H13NO3
  47. The crystal structure of (bis(benzimidazol-2-yl-methyl)amine-κ3N,N,N )-(dihydrogen L-malate-κ2O,O )copper(II) perchlorate dihydrate, CuC20H24ClN5O12
  48. Crystal structure of (1E,1′E)-4,4′-(9,9-diethyl-9H-fluorene-2,7-diyl)dibenzaldehyde dioxime, C31H28N2O2
  49. Crystal structure of diethyl 1,9-bis(4-fluorophenyl)-4,6-diphenylhexahydro-3H-2,7,3,5-(epimethanetriyliminomethanetriyl)cyclopenta [b]pyridine-3,7(2H)-dicarboxylate, C40H36F2N2O4
  50. Crystal structure of bis(benzene-1 carboxylato-O 3,5-carboxyl-κ1O)-[(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-κ4N,N′,N′′,N′′′)nickel(II) ─ benzene-1,3,5-tricarboxylic acid ─ water (1/2/4), C52H66N4NiO28
  51. Crystal structure of 1,4-dibromo-2,5-bis(2-methoxyethoxy)benzene-1,4-diol, C12H16Br2O4
  52. Crystal structure of dicarbonyl[N,N′-(1,2-dimethyl-1,2-ethanediylidene)bis[2,6-bis(1-methylethyl)benzenamine]-N,N′]nickel(0), C30H40N2NiO2
  53. Crystal structure of 1,4-dibromo-2,5-bis(prop-2-yn-1-yloxy)benzene, C12H8Br2O2
  54. Crystal structure of O-(3-(benzo[d]thiazol-2-yl)naphthalen-2-yl) O-phenyl carbonothioate, C24H15NO2S2
  55. The crystal structure of (E)-4-fluoro-N′-(1-(4-hydroxyphenyl)propylidene)benzohydrazide, C16H15FN2O2
  56. Crystal structure of (E)-1-(benzo[d]thiazol-2-yl)-N-(4,5-dihydropyren-2-yl)methanimine, C24H16N2S
  57. Crystal structure of 3-((4-bromophenyl)thio)-1H-indole, C14H10BrNS
  58. Synthesis and crystal structure of 1-((7-hydroxy-3-(4-hydroxy-3-nitrophenyl)-4-oxo-4H-chromen-8-yl)methyl)piperidin-1-ium-4-carboxylate monohydrate, C22H22N2O9
  59. Synthesis and crystal structure of (3E,5S,10S,13S,14S,17Z)-17-ethylidene-10,13-dimethylhexadecahydro-3H-cyclopenta[α]phenanthren-3-one O-(methacryloyl) oxime, C50H74N2O4
  60. Crystal structure of the hydrogen storage active phase La12Mg46LiMn
  61. The crystal structure of the salt: 4-((1,3-dioxoisoindolin-2-yl)carbamoyl)pyridine-1-ium 2-carboxybenzoate, C14H10N3O3·C8H5O4
  62. Crystal structure of (2-(2-pyridine)-benzimidazole-κ2 N,N′)-bis(1-phenylpyrazole-κ2 C,N)iridium(III) hexafluorophosphate, C30H22F6IrN7P
  63. Crystal structure of dichlorido-bis[2-(2,4-difluorophenyl)pyridine-κ1N]platinum(II), C22H14Cl2F4N2Pt
  64. Crystal structure of (5R,8R,9R,10R,12R,13R,14R, 17S,17Z)-2-((3-fluoropyridin-4-yl)methylene)-12-hydroxy-4,4,8,10,14-pentamethyl-17-((R)-2,6,6-trimethyltetrahydro-2H-pyran-2-yl)hexadecahydro-3H-cyclopenta[a]phenanthren-3-one, C36H52FNO3
Downloaded on 30.3.2026 from https://www.degruyterbrill.com/document/doi/10.1515/ncrs-2023-0321/html
Scroll to top button