Startseite Crystal structure of the 2D coordination polymer poly[diaqua-bis(μ2-3- methoxyisonicotinato-κ2N:O)cobalt(II)] — dimethylformamide (1/1), C20H30CoN4O10
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Crystal structure of the 2D coordination polymer poly[diaqua-bis(μ2-3- methoxyisonicotinato-κ2N:O)cobalt(II)] — dimethylformamide (1/1), C20H30CoN4O10

  • Xiao‐Tian Sun ORCID logo EMAIL logo
Veröffentlicht/Copyright: 15. Februar 2021

Abstract

C20H30CoN4O10, monoclinic, C2/c (no. 15), a = 13.4752(4) Å, b = 12.8563(3) Å, c = 15.0144(5) Å, β = 113.429(4)°, V = 2386.66(14) Å3, Z = 4, Rgt(F) = 0.0291, wRref(F2) = 0.0719, T = 293(2) K.

CCDC no.: 2059326

The asymmetric unit of the title crystal structure is shown in the figure (Hydrogen atoms are omitted for clarity). 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:Violet block
Size:0.35 × 0.31 × 0.25 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:0.78 mm−1
Diffractometer, scan mode:SuperNova, ω
θmax, completeness:28.5°, >99%
N(hkl)measured, N(hkl)unique, Rint:13809, 2692, 0.024
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 2486
N(param)refined:162
Programs:CrysAlisPRO [1], Olex2 [2], SHELX [3], [, 4]
Table 2:

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

AtomxyzUiso*/Ueq
Co10.50000.26859 (2)0.25000.01906 (9)
O10.14822 (10)0.15723 (9)0.19780 (10)0.0398 (3)
O20.38912 (8)0.15437 (8)0.25597 (8)0.0256 (2)
O30.41089 (12)0.15230 (12)0.41147 (9)0.0493 (4)
O40.57023 (9)0.26334 (9)0.40186 (8)0.0310 (3)
H4A0.59900.32160.42450.046*
H4B0.52400.23120.41690.046*
N10.12150 (10)−0.11318 (10)0.26005 (10)0.0250 (3)
C10.03986 (15)0.17600 (15)0.13067 (16)0.0437 (5)
H1A0.02060.12660.07850.066*
H1B0.03440.24520.10510.066*
H1C−0.00830.16880.16320.066*
C20.17226 (12)0.06045 (12)0.23658 (12)0.0258 (3)
C30.09733 (12)−0.01953 (12)0.21677 (12)0.0265 (3)
H30.0273−0.00790.17160.032*
C40.22319 (12)−0.12973 (12)0.32268 (13)0.0284 (3)
H40.2414−0.19450.35240.034*
C50.30271 (12)−0.05408 (12)0.34513 (12)0.0281 (3)
H50.3725−0.06850.38950.034*
C60.27861 (12)0.04285 (12)0.30173 (11)0.0243 (3)
C70.36672 (12)0.12498 (12)0.32547 (12)0.0250 (3)
O50.63074 (11)0.44757 (11)0.49054 (10)0.0474 (3)
N20.78216 (12)0.53833 (12)0.57444 (11)0.0386 (4)
C80.72914 (16)0.45240 (15)0.53709 (13)0.0383 (4)
H80.76870.39110.54650.046*
C90.7244 (2)0.63510 (18)0.5639 (2)0.0719 (8)
H9A0.72090.67000.50620.108*
H9B0.76140.67840.61940.108*
H9C0.65250.62130.55910.108*
C100.89875 (17)0.5407 (2)0.62035 (18)0.0661 (7)
H10A0.92620.47090.62970.099*
H10B0.92100.57490.68210.099*
H10C0.92660.57790.57980.099*

Source of material

The mixtures of 3-methoxy-4-pyridinecarboxylic acid (mpca) (0.1 mmol, 15.3 mg), Co(OAc)2 4H2O (0.1 mmol, 24.9 mg), DMF (2.0 ml) and H2O (2.0 ml) were placed in a 23 ml Teflon liner stainless steel reactor. The vessel was heated to 393 K for four days, then cooled slowly to the room temperature. Light violet crystals were obtained, and further crystals were filtered off, washed with mother liquid, and dried under ambient conditions. Yield 47% (based on mpca).

Experimental details

A suitable crystal was selected and mounted on a SuperNova, Single source at offset/far, EosS2 diffractometer. Using Olex2 [2], the structure was solved with the ShelXT [3] structure solution program using Intrinsic Phasing and refined with the ShelXL [4] refinement package. Hydrogen atoms were placed in calculated positions and refined isotropically with a riding model except for those bound to water, which were initially located in a difference Fourier map and included in the final refinement and Uiso(H) set to 1.5 times of Ueq(O).

Comment

In the past few decades, coordination compounds (CPs) have been becoming one of the most rapidly developing fields in chemical and material science not only because of their highly diversified topologies, but also due to their potential applications in many areas, such as magnetism [5], [, 6], catalysis [6], [, 7], luminescence [8], [, 9], sensing [10], [, 11], conductivity [12], [, 13] and so on. At present, many multi-topic organic ligands have been employed to prepare such materials and rapid progress in this flourishing field has been made [14], [, 15]. However, it is still a great challenge to obtain the desired structure relying on reaction conditions in the self-assembly. Among many organic ligands, isonicotinic acid and its derivatives as bifunctional ligands containing both pyridyl and carboxylate donor groups, thus are useful building blocks in the assembly of CPs. Such as, isonicotinic acid, 3,5-dichloroisonicotinic acid, 2,6-dichloroisonicotinic acid, etc, have been used as educts to construct diverse CPs in our and other previous work [16], [17], [18], [19]. The 3-methoxy-4-pyridinecarboxylate (mpca) is an ideal bifunctional connector in the exploration for CPs due to possess potential coordination sites involving the ingenious combination of carboxyl groups with an pyridyl ring. In this regard, we hope to reveal some structural factors of the H2 mpca for dominating the self-assembly, and this will provide more useful information of the substituent effect. Though as a good bifunctional ligand, mpca remains largely unexplored, and only few CPs have been reported.

The asymmetric unit of compound contains half a cobalt atom, one mpca anion, one ligated water molecule and one free N,N-dimethylformamide (DMF) molecule. Each cobalt atom is six-coordinated by two O donors and two N donors of four symmetry-related mpca ligands in the equatorial plane with two coordinated water molecule in the axial positions. The Co–O bond lengths are 2.1220(10) and 2.0935(11) Å, respectively. The Co–N bond lengths are 2.1948(12) Å. The [CoO4N2] environment are bridged by two N atoms and two O atoms of four mpca molecules resulting in stepwise (4,4) grids layers. Each layer is corrugated with four mpca molecules and four Co atoms forming repeating quadrate grid with a side length of 9.312/9.312 Å. Notably, the presences of coordinated water molecules lead to the formation of hydrogen-bonding interactions. Besides intralayer O(4)–H(4B)···O(3) hydrogen bonds, the paralleled layers are connected by hydrogen-bonds between coordination H2O and O atom of the DMF molecule [O(4)–H(4A)···O(5); d(O4···O5) = 2.6297(17) Å; degree (H–O···O5) = 163.0°] to develop the 2D layer. The adjacent 2D layers are stacked in a parallel fashion and cohered together by van der Waals forces into the entire 3D supramolecular networks of compound.


Corresponding author: Xiao‐Tian Sun, College of Chemistry and Chemical Engineering, Henan Key Laboratory of Function–Oriented Porous Materials, LuoYang Normal University, Luoyang, Henan471934, P. R. China, E-mail:

Award Identifier / Grant number: 11804140

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

  2. Research funding: This work was supported by the National Natural Science Foundation of China (No. 11804140).

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

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Received: 2021-01-07
Accepted: 2021-01-28
Published Online: 2021-02-15
Published in Print: 2021-05-26

© 2021 Xiao‐Tian Sun, 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. The crystal structure of bis(μ2-5-chloro-2-oxido-N-(1-oxidoethylidene)benzohydrazonato-κ5N,O,O′:N′,O′′)hexkis(pyridine-κ1N)trinickel(II) - pyridine (1/1), C63H57Cl2N13Ni3O6
  4. Crystal structure of [(μ2-succinato κ3O,O′:O′′)-bis-(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)]dinickel(II)] diperchlorate, dihydrate C36H82Cl2N8Ni2O15
  5. Crystal structure of catena-poly[aquabis(3-nitrobenzoato-κ2O:O′)-(μ2-pyrazine-N: N′)cadmium(II)], C18H14N4O9Cd
  6. Crystal structure of 4-(2,2-difluoroethyl)-2,4,6-trimethylisoquinoline-1,3(2H,4H)-dione, C14H15F2NO2
  7. The crystal structure of thioxanthen-9-one-10,10-dioxide, C13H8O3S – a second polymorph
  8. Crystal structure of (E)-2-((2-methoxy-3-pyridyl)methylene)-7-fluoro-3,4-dihydronaphthalen-1(2H)-one, C17H14FNO2
  9. The crystal structure of diaquahydrogen 2,5-dimethylbenzenesulphonate, C8H14O5S
  10. The crystal structure of N-(4-(cyclohexylimino)pent-2-en-2-yl)cyclohexanamine, C17H30N2
  11. The twinned crystal structure of 1,3-phenylenedimethanaminium dibromide, C8H14Br2N2
  12. Crystal structure of 2,4,7,9-tetranitro-10H-benzofuro[3,2-b]indole – dimethyl sulfoxide (1/1), C16H11N5O10S
  13. Crystal structure of 2,6-bis(2-(pyridin-3-yl)ethyl)pyrrolo[3,4-f]isoindole-1,3,5,7(2H,6H)-tetraone, C24H18N4O4
  14. The crystal structure of 3,4-dichlorobenzoic acid chloride, C7H3Cl3O
  15. Crystal structure of 1,1′-(1,4-phenylenebis(methylene))bis(pyridin-1-ium) bis(1,2-dicyanoethene-1,2-dithiolato-k2S:S)zinc(II), C26H18N6ZnS4
  16. Crystal structure of tetrakis(μ-naphthalene-1-carboxylato-κ2O,O′)bis(methanol)copper(II), C46H36Cu2O10
  17. Crystal structure of 9-methyl-3-methylene-1,2,3,9-tetrahydro-4H-carbazol-4-one, C14H13NO
  18. Crystal structure of bis(amino(carbamothioylamino)methaniminium) 3-nitrophthalate monohydrate, C12H19N9O7S2
  19. Crystal structure of 3,3′-(1,2-phenylene-bis(methylene))bis(1-ethyl-1H-imidazol-3-ium) bis(hexafluorophosphate), C18H24F12N4P2
  20. The crystal structure of 5-hydroxy-6,8-dimethoxy-2-methyl-4H-benzo[g]chromen-4-one– rubrofusarin B, C16H14O5
  21. The crystal structure of bis(ethanol-kO)- bis(6-aminopicolinato-k2N,O)manganese(II), C16H22O6N4Mn
  22. The crystal structure of 3,3′-((carbonylbis(azanediyl))bis(ethane-2,1-diyl)) bis(1-methyl-1H-benzo[d]imidazol-3-ium) tetrafluoroborate monohydrate, C21H28N6O3B2F8
  23. Crystal structure of dimethanol-dichlorido-bis( μ2-2-(((1,5-dimethyl-3-oxo-2- phenyl-2,3-dihydro-1H-pyrazol-4-yl)imino)methyl)phenolato- κ4O:O,O′,N)dinickel (II), C20H24ClNiN3O4
  24. The crystal structure of methyl 5-(trifluoromethyl)-1H-pyrrole-2-carboxylate, C7H6F3NO2
  25. Crystal structure of (OC‐6‐13)‐aqua‐tris (3‐bromopyridine‐κ1N)‐bis(trifluoroacetato‐κ1O)cadmium(II) C19H14Br3CdF6N3O5
  26. Crystal structure of methyl (E)-3-(4-(2-ethoxy-2-oxoethoxy)phenyl) acrylate, C14H16O5
  27. Crystal structure of methyl 4-acetoxy-3,5-dimethoxybenzoate, C12H14O6
  28. The crystal structure of 2-(1H-benzimidazol-2-yl)-3-bromo-5-chlorophenol, C13H8BrClN2O
  29. The crystal structure of bis(μ2-5-chloro-N-(2-methyl-1-oxidopropylidene)-2-oxidobenzohydrazonate-κ5N,O,O′:N′,O′′)pentakis(pyridine-κ1N)tricopper(II), C47H45Cl2N9Cu3O6
  30. Synthesis and crystal structure of catena-poly[aqua-bis(nitrato-κ2O:O′)- (μ2-((1 H-imidazol-1-yl)methyl)benzene-κ2 N,N′)-H2O-κ2O]cadmium(II), C14H16N6O7Cd
  31. The crystal structure of pentakis(carbonyl)-{μ-[2,3-bis(sulfanyl)propan-1-olato]}-(triphenylphosphane)diiron (FeFe)C26H21Fe2O6PS2
  32. Crystal structure of ethyl-2-(3-benzoylthioureido)propanoate, C13H16N2O3S
  33. Crystal structure of 2-methoxy-4b,5,14,15-tetrahydro-6H-isoquinolino[2′,1′:1,6] pyrazino[2,3-b]quinoxaline, C19H18N4O
  34. Crystal structure of 2,2′-[ethane-1,2-diylbis(azanylylidenemethylylidene)]bis(6-chlorophenol), C16H14Cl2N2O2
  35. The crystal structure of (Z)-3-((2-(2-(2-aminophenoxy)ethoxy)phenyl)amino)-1-phenylbut-2-en-1-one, C24H24N2O3
  36. The crystal structure of 10-(3,5-di(pyridin-4-yl)phenyl)-10H-phenoxazine dihydrate, C28H23N3O3
  37. Crystal structure of poly[dipoly[aqua-di(µ2-pyrazin-2-olato-κ2N:N′) zinc(II)], C8H8N4O3Zn
  38. Crystal structure of poly[tetra(μ2-cyanido-κ2N:O)-bis(N,N-dimethylformamide-κO)-manganese(II)-platinum(II)], C10H14MnN6O2Pt
  39. The crystal structure of aqua-chlorido-6,6′-((ethane-1,2-diylbis(azaneylylidene))bis(methaneylylidene))bis(2,4-dichlorophenolato-κ4N,N′,O,O′)manganese(III), C16H12Cl5MnN2O3
  40. Crystal structure of [di(µ2-cyanido)-dicyanido-bis(dimethyl sulfoxide-κO)- bis(2,2′-(ethane-1,2-diylbis(azanylylidenemethanylylidene))diphenolato-κ4,N,N′,O,O′)- dimanganese(III)-platinum(II)], C40H40Mn2N8O6PtS2
  41. The crystal structure of (azido)-κ1N-6,6′-((cyclohexane-1,2-diylbis(azanylylidene)) bis(methanylylidene))bis(3-bromophenolato-κ4N,N,O,O)-(methanol)-manganese(III)–methanol(1/1), C22H26Br2MnN5O4
  42. Crystal structure of 7-chloro-N-(4-iodobenzyl)-1,2,3,4-tetrahydroacridin-9-amine, C20H18ClIN2
  43. Crystal structure of catena-poly[(1,4,8,11-tetraazacyclotetradecane-κ4N,N,N,N′′′)-bis(μ2-thiocyanato-κ2N:S)-bis(thiocyanato-κS)-nickel(II)palladium(II)], C14H24N8NiPdS4
  44. Crystal structure of 3-chloro-4-(4-ethylpiperazin-1-yl)aniline monohydrate, C12H20ClN3O
  45. Crystal structure of the 2D coordination polymer poly[diaqua-bis(μ2-3- methoxyisonicotinato-κ2N:O)cobalt(II)] — dimethylformamide (1/1), C20H30CoN4O10
  46. Crystal structure of 4-[(5-chloro-2-hydroxybenzylidene)amino]-3-propyl-1H-1,2,4-triazole-5(4H)-thione, C12H13ClN4OS
  47. Crystal structure of N-(5-(2-(benzyl(1-(4-methoxyphenyl)propan-2-yl)amino)-1-hydroxyethyl)-2-(benzyloxy)phenyl)formamide, C33H36N2O4
  48. Crystal structure of 3-(methoxycarbonyl)-7-oxabicyclo[2.2.1]heptane-2-carboxylic acid, C9H12O5
  49. The crystal structure of 1-((dimethylamino)(3-nitrophenyl)methyl)naphthalen-2-ol, C19H18N2O3
  50. Crystal structure of catena-poly[di(μ2-cyanido-κ2C:N)-dicyanido-tetrakis(dimethyl sulfoxide-κO)-manganese(II)-platinum(II)], C12H24MnN4O4PtS4
  51. Crystal structure of 4-amino-N-(2-pyrimidinyl)benzenesulfonamide–1,4-dioxane (1/1), C14H18N4O4S
  52. Crystal structure of bis{1-[(benzotriazol-1-yl)methyl]-1H-1,3-(2-methyl-imidazol)}di-chloridomercury(II), [Hg(C11H11N5)2Cl2], C22H22N10Cl2Hg
  53. Crystal structure of 2, 3-bis((4-methylbenzoyl)oxy) succinic acid–N, N-dimethylformamide (1/1), C23H25NO9
  54. Crystal structure of catena-poly[bis(4-(4-carboxyphenoxy)benzoato-κ1O)-μ2-(1,4-bis(1-imidazolyl)benzene-κ2N:N′)cobalt(II)], C40H28N4O10Co
  55. Crystal structure of 1H-imidazol-3-ium poly[aqua-(μ4-glutarato-κ6O,O′:O′:O′′,O′′′:O′′′)-(nitrato-κ2O,O′)strontium(II)], C8H13N3O8Sr
  56. Crystal structure of (R)-6-(benzo[b]thiophen-5-yl)-2-methyl-2,6-dihydrobenzo [5,6] silino[4,3,2-cd]indole, C23H17NSSi
  57. Crystal structure of catena-poly[bis(μ2-thiocyanato-κ2N:S)-(2-(5-methyl-1H-pyrazol-3-yl)pyridine-κ2N,N′)cadmium(II)]–dioxane (1/1), C15H17CdN5O2S2
  58. Crystal structure of poly[aqua-(μ2-1,4-bis(2′-carboxylatophenoxy)benzene-κ2O:O′)-(μ2-4,4′-bipyridione-κ2N:N′)cadmium(II)] monhydrate, C30H22CdN2O7⋅H2O
  59. Crystal structure of catena-poly[tetraaqua-(μ2-4,4′-bipyridine-k2N:N′)-bis(μ2-4′-methyl-[1,1′-biphenyl]-3,5-dicarboxylato-k4O,O′:O″,O′″)dicadmium(II)] dihydrate, C20H20NO7Cd
  60. Crystal structure of 1‐tert‐butyl‐3‐(2,6‐diisopropyl‐4‐phenoxyphenyl)‐2-methylisothiourea, C24H34N2OS
  61. Crystal structure of catena-poly[triaqua-(μ2-1,3-di(1H-imidazol-1-yl)propane-κ2N:N′)-(4,4′-(1H-1,2,4-triazole-3,5-diyl)dibenzoato-κ1O)cobalt(II)] — N,N′-dimethylformamide (1/1), C28H34N8O8Co
  62. Crystal structure of tetraaqua-bis(1,4-di(1H-imidazol-1-yl)benzene-κ1N)manganese(II) 2,3-dihydroxyterephthalate, C32H32MnN8O10
Heruntergeladen am 4.11.2025 von https://www.degruyterbrill.com/document/doi/10.1515/ncrs-2021-0010/html?lang=de
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