Startseite 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)
Artikel Open Access

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)

  • Guang-Zhen Liu ORCID logo EMAIL logo und Xin Wang
Veröffentlicht/Copyright: 7. September 2023

Abstract

C23H23Co0.5N4O4, triclinic, P 1 (no. 2), a = 9.6428(5) Å, b = 10.3191(5) Å, c = 11.8710(6) Å, α =  86.664 ( 4 ) , β =  69.399 ( 5 ) , γ =  79.429 ( 4 ) , V = 1086.90(10) Å3, Z = 2, R g t (F) = 0.0432, w R r e f (F2) = 0.1454, T = 293(2) K.

CCDC no.: 2290490

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: Pink block
Size: 0.33 × 0.22 × 0.21 mm
Wavelength: Mo Kα radiation (0.71073 Å)
μ: 0.46 mm−1
Diffractometer, scan mode: SuperNova, ω
θmax, completeness: 25.5°, 98%
N(hkl)measured, N(hkl)unique, Rint: 11,718, 3987, 0.030
Criterion for Iobs, N(hkl)gt: Iobs > 2σ(Iobs), 3510
N(param)refined: 289
Programs: Olex2 [1], SHELX [2, 3]
Table 2:

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

Atom x y z Uiso*/Ueq
Co1 0.5000 0.5000 0.5000 0.02797 (18)
O1 0.36593 (18) 0.56658 (17) 0.67157 (14) 0.0374 (4)
O1W 0.54267 (17) 0.69171 (16) 0.44558 (14) 0.0365 (4)
H1WA 0.5218 0.7129 0.3824 0.055*
H1WB 0.5050 0.7556 0.4953 0.055*
O2 0.33858 (19) 0.78536 (17) 0.65731 (15) 0.0423 (4)
N3 0.3076 (2) 0.5370 (2) 1.43896 (17) 0.0341 (5)
N4 −0.0366 (2) 0.7196 (2) 1.21399 (17) 0.0409 (5)
H4 −0.0866 0.7966 1.2391 0.049*
C1 0.3162 (2) 0.6810 (2) 0.7168 (2) 0.0297 (5)
C2 0.2281 (2) 0.6902 (2) 0.84817 (19) 0.0299 (5)
C3 0.2095 (3) 0.5786 (2) 0.9179 (2) 0.0375 (6)
H3 0.2542 0.4965 0.8818 0.045*
C4 0.1265 (3) 0.5848 (3) 1.0397 (2) 0.0394 (6)
H4A 0.1174 0.5076 1.0842 0.047*
C5 0.0564 (2) 0.7066 (2) 1.0960 (2) 0.0319 (5)
C6 0.0790 (3) 0.8202 (3) 1.0266 (2) 0.0371 (6)
H6 0.0371 0.9025 1.0629 0.044*
C7 0.1625 (2) 0.8125 (2) 0.9048 (2) 0.0333 (5)
H7 0.1750 0.8894 0.8602 0.040*
C8 −0.0563 (3) 0.6125 (3) 1.2990 (2) 0.0413 (6)
H8A −0.0604 0.5343 1.2595 0.050*
H8B −0.1513 0.6355 1.3646 0.050*
C9 0.0699 (2) 0.5822 (3) 1.3493 (2) 0.0332 (5)
C10 0.1700 (3) 0.4660 (3) 1.3284 (2) 0.0417 (6)
H10 0.1597 0.3995 1.2838 0.050*
C11 0.2865 (3) 0.4471 (3) 1.3735 (2) 0.0428 (6)
H11 0.3535 0.3675 1.3572 0.051*
C12 0.2088 (3) 0.6496 (3) 1.4606 (2) 0.0422 (6)
H12 0.2193 0.7134 1.5078 0.051*
C13 0.0927 (3) 0.6763 (3) 1.4170 (2) 0.0428 (6)
H13 0.0289 0.7576 1.4327 0.051*
N1 0.7693 (3) 0.9349 (3) 0.5992 (2) 0.0593 (7)
N2 0.5241 (3) 0.7615 (3) 1.2177 (2) 0.0528 (6)
C14 0.4614 (4) 0.7275 (4) 1.1437 (3) 0.0705 (10)
H14 0.3825 0.6808 1.1756 0.085*
C15 0.5044 (4) 0.7561 (4) 1.0233 (3) 0.0628 (9)
H15 0.4562 0.7280 0.9761 0.075*
C16 0.6206 (3) 0.8275 (3) 0.9722 (2) 0.0391 (6)
C17 0.6863 (3) 0.8631 (3) 1.0487 (2) 0.0544 (8)
H17 0.7648 0.9106 1.0199 0.065*
C18 0.6352 (3) 0.8281 (3) 1.1692 (3) 0.0542 (8)
H18 0.6822 0.8530 1.2187 0.065*
C19 0.6722 (3) 0.8638 (3) 0.8434 (2) 0.0377 (6)
C20 0.8158 (3) 0.8900 (3) 0.7836 (3) 0.0579 (8)
H20 0.8835 0.8836 0.8242 0.069*
C21 0.8588 (4) 0.9256 (4) 0.6640 (3) 0.0671 (9)
H21 0.9554 0.9441 0.6267 0.081*
C22 0.6332 (3) 0.9090 (3) 0.6555 (3) 0.0535 (7)
H22 0.5687 0.9148 0.6120 0.064*
C23 0.5798 (3) 0.8736 (3) 0.7758 (2) 0.0451 (7)
H23 0.4823 0.8566 0.8108 0.054*
O2W −0.1821 (3) 0.9664 (2) 1.34689 (17) 0.0612 (6)
H2WA −0.2295 1.0421 1.3381 0.092*
H2WB −0.1949 0.9537 1.4210 0.092*

1 Source of material

All chemicals for synthesis were of reagent grade and used as received without further purification. The mixtures of 4-[(4-pyridinylmethyl)amino] benzoic acid (0.05 mmol, 12.0 mg), 4,4′-bipyridine (0.1 mmol, 16.2 mg), Co(Ac)2–4H2O (0.1 mmol, 25.1 mg), NaOH (0.1 mmol, 4.0 mg) and H2O (6 mL) was placed in a 23 mL Teflon-lined autoclave at 393 K for 4 days, and then slowly cooled down to room temperature for crystallization. Pink block crystals of the title compound were obtained. The yield was 62 % (based on Co). For C23H23Co0.5N4O4 anal. calcd., % C, 61.54 H, 5.16 N, 12.48 found, % C, 61.45 H, 5.38 N, 12.38.

2 Experimental details

Using Olex2 [1], the structure was solved with the ShelXT [2] structure solution program and refined with the ShelXL [3] refinement package. All hydrogen atoms were added to their calculated positions and refined using a riding model. The Uiso of the H-atoms were constrained to 1.2 times Ueq of their bonding carbon atoms and 1.5 times Ueq of their bonding oxygen atoms for the hydrogen atoms in water molecules.

3 Comment

Coordination polymers (CPs) represent a high-speed growing area in coordination and supramolecular chemistry [4], [5], [6], and especially for Co(II) compounds [7, 8]. The design and synthesis of coordination polymers via self-assembly of metal ions and organic ligands depend on the selection of metal centers and the organic ligands with controlled chemical and physical properties by the Schiff-base ligands [9, 10], because this class of ligand with O,N-bifunctional group has multiple coordination points and various coordination modes. The HL {HL = 4-[(4-pyridinylmethyl)amino]benzoic acid} starting material has one carboxylic group and one nitrogen atom at the terminal positions and one secondary amine group between the phenyl groups, which can supply more varied coordinating patterns (monodentate, bridging, chelating) to construct coordination frameworks. However, HL carboxylic acid ligands have not been extensively exploited, except for some limited cases [11], [12], [13].

The crystal structure of the compound shows a one-dimensional chain structure. The asymmetric unit contains one half crystallographically Co(II) cation, one completely deprotonated L anion and one Bpy molecule and one coordinating water molecule and one crystallization water molecule as shown in the upper part of the figure (A: 1 − x, 1 − y, 1 − z; B: 1 − x, 1 − y, 2 − z; C: x, y, −1 + z). In this complex, each Co(II) cation is six-coordinated with a distorted octahedral geometry, [CoN2O4] by two N atoms from two symmetry-related Bpy ligand, two oxygen atoms from two symmetry-related L anions, two oxygen atoms from two coordination water molecules. The Co–O bond lengths are 2.068(16), and 2.113(18) Å for Co1–O1, Co1–O1W, and one Co–N bond is 2.183(18) Å for Co1–N3, respectively. Two adjacent cobalt(II) are connected together by two L anions adopting monodentate coordination mode to form an infinite one-dimensional chain along the c axis with the Co⋯Co distance of 11.8710(6) Å (lower part of the structure). There are massive H-bonding interactions in the compound via the participation of coordination waters and carboxylate O atoms (O(1W)–H(1WB)⋯O(2): 2.689(2) Å), between crystallization waters and carboxylate O atoms (O(2W)–H(2WA)⋯O(2): 2.732(3) Å), between coordination waters and N atoms of Bpy molecules (O(1W)–H(1WA)⋯N(2): 2.817(3) Å), between crystallization waters and N atoms of Bpy molecules (O(2W)–H(2WB)⋯N(1): 2.873(3) Å), between crystallization waters and amino N atoms of L (N(4)–H(4)⋯O(2W): 2.923(3) Å). The free Bpy molecules as parallel pendent arms are hung on one side of the infinite chain through the hydrogen bonds. At last a three-dimensional supramolecular structure was gained through the H-bonding interactions.


Corresponding author: Guang-Zhen Liu, College of Chemistry and Chemical Engineering, Luoyang Normal University Luoyang, Henan 471934, P.R. China, E-mail:

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

  2. Research funding: None declared.

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

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Received: 2023-03-27
Accepted: 2023-08-24
Published Online: 2023-09-07
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.

Artikel in diesem Heft

  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
Heruntergeladen am 7.9.2025 von https://www.degruyterbrill.com/document/doi/10.1515/ncrs-2023-0148/html
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