Startseite Crystal structures of diiodido-3-((pyridin-2-ylmethylene)amino)-2-(pyridin-3-yl)-2,3-dihydroquinazolin-4(1H)-one-cadmium(II)
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Crystal structures of diiodido-3-((pyridin-2-ylmethylene)amino)-2-(pyridin-3-yl)-2,3-dihydroquinazolin-4(1H)-one-cadmium(II)

  • Honglin Chen und Ying Xiong ORCID logo EMAIL logo
Veröffentlicht/Copyright: 14. November 2024

Abstract

C19H13CdI2N5O, triclinic, P 1 (no. 2), a = 9.0045(7) Å, b = 9.6113(8) Å, c = 13.1285(12) Å, α = 80.395(3)°, β = 79.861(3)°, γ = 80.512(3)°, V = 1091.99(16) Å3, Z = 2, R gt (F) = 0.0544, wR ref (F 2) = 0.1446, T = 273 K.

CCDC no.: 2383743

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: Yellow block
Size: 0.20 × 0.20 × 0.15 mm
Wavelength: Mo Kα radiation (0.71073 Å)
μ: 3.85 mm−1
Diffractometer, scan mode: Bruker APEX-II, φ and ω
θ max, completeness: 25.0°, >99 %
N(hkl)measured, N(hkl)unique, R int: 32813, 3847, 0.100
Criterion for I obs, N(hkl)gt: I obs > 2 σ(I obs), 3,263
N(param)refined: 253
Programs: Olex2, 1 Bruker, 2 SHELX, 3 Diamond 4
Table 2:

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

Atom x y z U iso */U eq
C1 0.3680 (9) 0.7411 (8) 0.5471 (5) 0.0405 (16)
C2 0.3086 (11) 0.8111 (9) 0.6342 (6) 0.056 (2)
H2 0.207879 0.808160 0.665300 0.067*
C3 0.4000 (13) 0.8841 (10) 0.6733 (7) 0.064 (3)
H3 0.359871 0.930940 0.730747 0.077*
C4 0.5503 (14) 0.8890 (10) 0.6289 (8) 0.067 (3)
H4 0.611343 0.936011 0.658001 0.081*
C5 0.6104 (11) 0.8240 (9) 0.5411 (6) 0.053 (2)
H5 0.710439 0.830119 0.509465 0.064*
C6 0.5193 (9) 0.7496 (7) 0.5008 (5) 0.0396 (16)
C7 0.5851 (8) 0.6764 (7) 0.4110 (5) 0.0358 (15)
C8 0.3197 (8) 0.6366 (8) 0.4008 (6) 0.0374 (15)
C9 0.2471 (9) 0.7629 (8) 0.3309 (6) 0.0424 (17)
C10 0.0905 (11) 0.7928 (12) 0.3453 (9) 0.069 (3)
H10 0.032720 0.734938 0.395337 0.082*
C11 0.0199 (15) 0.9062 (15) 0.2869 (11) 0.090 (4)
H11 −0.085777 0.926936 0.296021 0.107*
C12 0.1075 (17) 0.9879 (13) 0.2152 (11) 0.090 (4)
H12 0.059512 1.067674 0.176983 0.108*
C13 0.3317 (11) 0.8444 (8) 0.2546 (6) 0.0491 (19)
H13 0.437119 0.820697 0.243054 0.059*
C14 0.4749 (9) 0.4865 (8) 0.2356 (6) 0.0423 (16)
H14 0.370049 0.488275 0.253699 0.051*
C15 0.5609 (8) 0.4146 (8) 0.1486 (6) 0.0394 (16)
C16 0.4925 (10) 0.3349 (9) 0.0959 (7) 0.0511 (19)
H16 0.388476 0.330600 0.112697 0.061*
C17 0.5782 (11) 0.2625 (11) 0.0192 (8) 0.065 (3)
H17 0.533798 0.207808 −0.016070 0.078*
C18 0.7319 (12) 0.2726 (12) −0.0045 (8) 0.071 (3)
H18 0.793630 0.223979 −0.055613 0.085*
C19 0.7922 (11) 0.3558 (11) 0.0488 (7) 0.063 (2)
H19 0.895597 0.363142 0.032016 0.075*
Cd1 0.80699 (6) 0.57760 (7) 0.21293 (5) 0.0464 (2)
I1 1.05520 (6) 0.40318 (7) 0.27791 (6) 0.0684 (2)
I2 0.79546 (8) 0.82610 (7) 0.08093 (5) 0.0684 (2)
N1 0.2867 (8) 0.6554 (7) 0.5105 (5) 0.0450 (15)
N2 0.4850 (6) 0.6117 (6) 0.3708 (4) 0.0336 (12)
N3 0.5510 (6) 0.5471 (6) 0.2860 (4) 0.0338 (12)
N4 0.7098 (7) 0.4263 (7) 0.1233 (5) 0.0461 (15)
N5 0.2651 (16) 0.9593 (10) 0.1953 (7) 0.092 (3)
O1 0.7205 (6) 0.6705 (6) 0.3726 (4) 0.0466 (12)

1 Source of materials

Pyridine-3-carboxyaldehyde (0.535 g, 5.0 mmol) was added to a solution of (E)-2-amino-N′-(pyridin-2-ylmethylene)benzohydrazide (1.20 g, 5 mmol) methanol (40 mL), reflow and stir for 24 h, and then the solvent was removed under vacuum. The white product was washed with absolute ethanol and dried under vacuum to yield the ligand L(3-((pyridin-2-ylmethylene)amino)-2-(pyridin-3-yl)-2,3-dihydroquinazolin-4(1H)-one). Cadmium diiodide (73 mg, 0.2 mmol) in methanol (20 mL) was added dropwise to L (62 mg, 0.2 mmol) in DMF (20 mL) with stirring and the reaction was continued for 1 h at room temperature. The mixed solution was filtered off and left for slow evaporation. Bright yellow crystals were obtained after 5 days. The crystals that formed were collected by filtration, washed with methanol, and dried.

2 Experimental details

Using Olex2, 1 the structure was solved using charge flipping and refined with the ShelXL 3 refinement. All hydrogen atoms were positioned geometrically, with the d(C–H) = 0.97–0.99 Å, U iso(H) = 1.2 times U eq(C) and U iso(H) = 1.5 times U eq(O).

3 Comment

Acylhydrazones are a class of Schiff base compounds obtained by condensation of hydrazide and aldehyde or ketone. 5 They have coordination donor atoms nitrogen and oxygen, and are easy to coordinate with transition metal ions to form a series of complex structures with novel structures. 6

The molecular structure of the complex showed that the coordination ratio of ligand L and CdI2 form a mononuclear 1/1 complex. In the molecular structure of the mononuclear complex, the central cadmium ion has five coordinating atoms, and among the five coordinating donor atoms that form coordinating bonds with cadmium ion, three coordinating donor atoms come from the ligand L (namely, one pyridine nitrogen atom, one Schiff base nitrogen atom and one carbonyl oxygen atom). The other two coordinating atoms are from the two iodido ligands. The central cadmium is in detail coordinated by the ligand’s atoms N3, N4 and O1 to form two nearly coplanar five-membered rings. The geometric parameters are all in the expected ranges. 7


Corresponding author: Ying Xiong, School of Chemistry and Materials, Guizhou Normal University, Guiyang 550025, People’s Republic of China, E-mail:

  1. Author contribution: 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 Academic New Seedling Foundation Project of Guizhou Normal University (Grant No. Qianshixinmiao-[2022]B04), the Provincial General Project of University Student Innovation and Entrepreneurship Fund, China (No. 202310663024).

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

References

1. 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.Suche in Google Scholar

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3. Sheldrick, G. M. Crystal Structure Refinement with SHELXL. Acta Crystallogr. 2015, C71, 3–8. https://doi.org/10.1107/s2053229614024218.Suche in Google Scholar

4. Brandenburg, K. DIAMOND. Visual Crystal Structure Information System. Ver. 4.0; Crystal Impact: Bonn, Germany, 2015.Suche in Google Scholar

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Received: 2024-09-30
Accepted: 2024-11-04
Published Online: 2024-11-14
Published in Print: 2025-02-25

© 2024 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 the co-crystal 2,4,6-triamino-1,3,5-triazine-1,3-dioxide — acetic acid (1/2) C7H14N6O6
  4. Crystal structure of the dinuclear mercury(II) complex bis(μ2-bromido)-dibromido-bis{1-[(benzotriazol-1-yl)methyl]-1-H-1,3-(2-ethyl-5-methyl-imidazol)-κ1 N} dimercury(II), C26H30N10Hg2Br4
  5. Crystal structure of poly[hexaqua-pentakis(μ4-2,2′-bipyridine-4,4′-dicarboxylato-κ4 O:O′:O″:O‴)-(μ2-2,2′-bipyridine-4,4′-dicarboxylato-κ2 O:O)tetraytterbium(III)] hydrate, C36H26N6O16Yb2
  6. Hydrothermal synthesis and crystal structure of catena-poly[(1,10-phenanthroline-κ 2 N,N′)-bis(μ 2-nitroisophthalato-κ 3 O,O′:O″)nickel(II)], C20H13NiN3O7
  7. Crystal structure of 72,73,75,76-tetrafluoro-25,44-dimethyl-31,33,36,38-tetraoxo-31,32,33,36,37,38-hexahydro-3(2,7)-benzo[lmn][3,8]phenanthrolina-1,5(4,1)-dipyridin-1-iuma-2,4(1,2),7(1,4)-tribenzenacyclooctaphane-11,51-diium hexafluoridophosphate, [C46H28F4N4O4][PF6]2, a dicationic cyclophane
  8. Crystal structure of (E)-2-(4-(1H-imidazol-1-yl)benzylidene)-7-fluoro-3,4-dihydronaphthalen-1(2H)-one, C20H15FN2O
  9. The salt crystal structure of etoricoxib hydrochloride, C18H16Cl2N2O2S
  10. The structure of t-butyl 7-[2-(4-fluorophenyl)-3-phenyl-4-(phenylcarbamoyl)-5-(propan-2-yl)-1H-pyrrol-1-yl]-3,5-dihydroxyheptanoate, C37H43FN2O5
  11. The crystal structure of (μ4-oxo)-tri(μ4-2,2′-bipyridine-6,6′-bis(olato)-κ5 O,O′:N:N′:O″)tetrazinc(II) – methylformamide (1/1), C33H25N7O8Zn4
  12. The co-crystal structure of 4-chlorobenzophenone–salicylhydrazide(1/1), C20H17ClN2O3
  13. Crystal structure of 9-fluoro-4-(6-methoxypyridin-2-yl)-5,6-dihydrobenzo[h]quinazolin-2-amine, C18H15FN4O
  14. The crystal structure of the co-crystal composed of benzhydrazide and 5-aminoisophthalic acid, C8H7NO4⋅C7H8N2O
  15. The cocrystal structure of praziquantel-hesperetin (1/1), C35H38N2O8
  16. Crystal structure of new barium manganese fluorides dihydrates, Ba10Mn2F25·2H2O
  17. The crystal structure of bis[μ2-(3-(3-(pyridin-2-yl)-1H-pyrazol-1-yl)propanoate-κ2O:N)-bis(2,2′-bipyridine-κ2 N, N′)dicopper(II)]dinitrate, C42H36Cu2N12O10
  18. Crystal structure of (3,6-di(2-pyridyl)-4-phenylaminopyridazine-κ2N,N′)-bis(2-(p-toluene)pyridinyl-κ2C,N)-iridium(III) hexafluorophosphate –dichloromethane (1/1), C45H37Cl2F6IrN7P
  19. The crystal structure of 2-(2′-carboxybenzyl)benzoic acid, C15H12O5
  20. The crystal structure of dichlorido-[(E)-N′,N″-bis((2E,3E)-3-(hydroxyimino)butan-2-ylidene)-2-((E)-3-(hydroxyimino)butan-2-ylidene)hydrazine-1-carbohydrazonhydrazide-κ 4 N 4]cobalt(II), C13H22N9O3Cl2Co
  21. Crystal structure of (−)-flavesine H, C15H22N2O2
  22. Crystal structure of 3-methoxybenzyl 2-(6-methoxynaphthalen-2-yl)propanoate, C22H22O4
  23. Crystal structure of dicarbonyl(2-oxopyridin-1(2H)-olato-κ 2 O,O)iridium(I), C7H4IrNO4
  24. The crystal structure of 4-(3-(triphenylphosphonio)propyl)piperazin-1-ium dibromide trihydrate, C25H37Br2N2O3P
  25. The crystal structure of ethyl 5,6-dihydroxybenzofuran-3-carboxylate, C11H10O5
  26. Crystal structure of 14-(R)-(2′-cyano-phenoxy)-3,19-diacetyl andrographolide, C31H37NO7
  27. The twinned crystal structure of 10-(4-methyl benzoate)-2,8-diethyl-5,5-difluoro-1,3,7,9-tetramethyl-5H-di-pyrrolo[1,2-c:2′,1′-f] [1,3,2]diazaborinin-4-ium-5-uide, C25H29BF2N2O2
  28. The crystal structure of (9H-thioxanthen-9- ylidene)hydrazine monohydrate, C13H11N2SO0.5
  29. The crystal structure of pyridinium diaqua-{1,2-phenylenebis((carboxylatocarbonyl)amido-κ4 N,N′,O,O′)manganese(III), C15H14MnN3O8
  30. Crystal structure of the hydrogen storage active high entropy phase Tb0.82Sm0.18Ni0.83Co0.17Mg
  31. Crystal structure of diaqua-bis[5-methyl-1-(1H-pyrazol-3-yl)-1H-1,2,3-triazole-4-carboxylato-κ 2 N,O)]manganese(II), C14H16MnN10O6
  32. Crystal structures of diiodido-3-((pyridin-2-ylmethylene)amino)-2-(pyridin-3-yl)-2,3-dihydroquinazolin-4(1H)-one-cadmium(II)
  33. Synthesis and crystal structure of methyl 4-(2-ethoxy-2-oxoethoxy)-3,5-dimethoxybenzoate, C14H18O7
  34. Crystal structure of isoxazolo[4,5-b]pyridin-3-amine, C6H5N3O
  35. Crystal structure of 4-chloro-1-isobutyl-1H-imidazo, C14H14ClN3
  36. The crystal structure of 1,1,1,2,2,2-hexakis(2-methyl-2-phenylpropyl)distannane,C60H78Sn2
  37. The crystal structure of (2,7-dimethoxynaphthalene-1,8-diyl)bis((3-nitrophenyl)methanone), C26H18N2O8
  38. Crystal structure of diaqua-tetra((E)-(RS)-1-(2,4-dichlorophenyl)-4,4-dimethyl-2-(1,2,4-triazol-1-yl)pent-1-en-3-ol-κ 1 N)zinc(II) dinitrate dihydrate, C60H76Cl8N14O14Zn
  39. The crystal structure of diphenyl bis(2-((diphenoxyphosphoryl)amino)ethyl)phosphoramidate monohydrate C40H42N3O10P3
  40. Crystal structure of 4,4′-bis(dibromomethyl)-1,1′-biphenyl, C14H10Br4
  41. Crystal structure of CaPtZn
  42. Crystal structure of 3-chloro-5-(trifluoromethyl)pyridine-2-carboxylic acid, C7H3ClF3NO2
  43. The crystal structure of (3′-(2-bromophenyl)-2-phenyl-[2,2′-bioxiran]-3-yl)(phenyl)methanone, C92H68O12Br4
  44. Crystal structure of ethyl 4-(4-benzylpiperazin-1-yl)benzoate, C20H24N2O2
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  48. Crystal structure of 1′,3′-dihydro-2,2′-spirobi[indene]-1,3-dione, C17H12O2
  49. Crystal structure of (E)-2,2′,3,3′-tetrahydro-[1,1′-biindenylidene]-4,4′-diol, C18H16O2
  50. Crystal structure of di-glycylglycinium squarate dihydrate, C12H22N4O12, at 105 K
  51. Crystal structure of {[(4-fluorophenyl)methyl]triphenylphosphonium}dibromocopper(I), [C25H21FP]+[CuBr2]
  52. Crystal structure of poly[diaqua-bis(μ2-5-((pyridin-4-yl-methyl)amino)benzene-1,3-dicarboxylato-κ 2 N:O)cadmium(II)], C28H26CdN4O10
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