Startseite Crystal structure of tetraaqua-bis[4-(1H-1,2,4-triazol-1-yl)benzoato-k1 N]cadmium(II), C18H20CdN6O8
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Crystal structure of tetraaqua-bis[4-(1H-1,2,4-triazol-1-yl)benzoato-k1 N]cadmium(II), C18H20CdN6O8

  • Yi-Min Feng und Yu-Pei Xia ORCID logo EMAIL logo
Veröffentlicht/Copyright: 13. Juli 2022

Abstract

C18H20CdN6O8, triclinic, P 1 (no. 2), a = 6.1132(7) Å, b = 7.1270(9) Å, c = 12.3110(13) Å, α = 80.7010(10)°, β = 88.137(2)°, γ = 73.6530(10)°, V = 507.88(10) Å3, Z = 1, R gt(F) = 0.0285, wR ref(F 2) = 0.0744, T = 298(2) K.

CCDC no.: 2130106

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: Colourless block
Size: 0.49 × 0.40 × 0.39 mm
Wavelength: Mo Kα radiation (0.71073 Å)
μ: 1.14 mm−1
Diffractometer, scan mode: Bruker D8 Advance, φ and ω
θ max, completeness: 25.3°, 98%
N(hkl)measured, N(hkl)unique, R int: 2665, 1836, 0.023
Criterion for I obs, N(hkl)gt: I obs > 2 σ(I obs), 1800
N(param)refined: 168
Programs: Bruker [1], Olex2 [2], SHELX [3, 4]
Table 2:

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

Atom x y z U iso*/U eq
Cd1 0.500000 0.500000 0.500000 0.03121 (15)
O1 0.3459 (4) 0.9730 (3) −0.37289 (17) 0.0437 (5)
O2 0.0123 (4) 1.0665 (4) −0.29116 (18) 0.0496 (6)
O3 0.1834 (4) 0.7694 (4) 0.4822 (2) 0.0459 (6)
O4 0.7043 (4) 0.6973 (4) 0.5618 (2) 0.0429 (5)
N1 0.5912 (4) 0.6459 (3) 0.14238 (18) 0.0274 (5)
N2 0.6134 (4) 0.5599 (4) 0.31996 (19) 0.0326 (5)
N3 0.8183 (4) 0.5642 (4) 0.1655 (2) 0.0362 (6)
C1 0.2220 (5) 0.9834 (4) −0.2892 (2) 0.0317 (6)
C2 0.3307 (4) 0.8891 (4) −0.1777 (2) 0.0267 (5)
C3 0.5641 (5) 0.8233 (4) −0.1588 (2) 0.0340 (6)
H3 0.662761 0.834787 −0.217016 0.041*
C4 0.6526 (5) 0.7403 (4) −0.0537 (2) 0.0335 (6)
H4 0.809457 0.696503 −0.041612 0.040*
C5 0.5056 (4) 0.7233 (4) 0.0327 (2) 0.0252 (5)
C6 0.2721 (5) 0.7801 (5) 0.0140 (2) 0.0387 (7)
H6 0.173452 0.761362 0.071238 0.046*
C7 0.1884 (5) 0.8641 (5) −0.0899 (2) 0.0370 (7)
H7 0.031427 0.905458 −0.101821 0.044*
C8 0.8216 (5) 0.5147 (5) 0.2731 (2) 0.0360 (6)
H8 0.955519 0.453876 0.313707 0.043*
C9 0.4737 (5) 0.6430 (4) 0.2351 (2) 0.0327 (6)
H9 0.316324 0.692255 0.239585 0.039*
H3A 0.119 (8) 0.824 (7) 0.420 (4) 0.072 (13)*
H3B 0.211 (8) 0.860 (7) 0.521 (4) 0.070 (14)*
H4A 0.760 (10) 0.754 (9) 0.513 (5) 0.10 (2)*
H4B 0.603 (9) 0.783 (8) 0.585 (4) 0.078 (16)*

Source of material

All the chemical reagents were purchased and used without further purification. Cd(NO3)2 ⋅ 4H2O (0.0308 g, 0.1 mmol), 1-(4-carboxyphenyl)-1,2,4-triazole) ligand (Hcpt, 0.0189 g, 0.1 mmol) and DMF/H2O (6 mL, 3:3, v/v) were placed in a 10 mL capped vial and used ultrasonic technique to get a clear solution. The vial was transferred to an 85 °C oven, heated for three days and cooled to room temperature at a rate of 10 °C/h. Colourless block crystals of the title complex were obtained, yielding 53% (based on the ligand).

Experimental details

The structure was solved by intrinsic phasing with the SHELXT program and refined with SHELXL program via OLEX2 software. The hydrogen atoms were placed in their idealized positions with isotropic thermal parameters.

Comment

As a polydentate organic ligand, 1-(4-carboxyphenyl)-1,2,4-triazole (Hcpt), which bearing both O and N coordinated sites, has been applied to construct metal complexes [5], [6], [7], [8], [9], [10]. However, it should be noted that most of the published Cd(II)-based complexes are complicated structures. To further enrich the family of Hcpt-based metal complexes, the title complex was synthesized under hydrothermal condition.

The complex crystallizes in the triclinic system with a space group of P 1 (no. 2). The asymmetric unit consists of one deprotonated Hcpt ligand, one half of Cd(II) ion and two coordinated water molecules. The Cd(II) ion is six-coordinated with two triazolyl nitrogen atoms (N2, N21−x, 1−y, 1−z ) derived from two different deprotonated Hcpt ligands and four oxygen atoms (O3, O31−x, 1−y, 1−z , O4, O41−x, 1−y, 1−z ) originated from four coordinated water molecules. The Cd–N and Cd–O bond lengths are in the range of 2.298(2)–2.348(2) Å, which are comparable to the other Cd(II) complexes [11, 12]. The complex is further linked by the coordinated water molecules and carboxylate groups via the classical O–H—O hydrogen bond to form a three-dimensional (3D) network. Apart from the hydrogen bonding, the π-π stacking, distance range: 3.7598(17)–3.9104(17) Å, don’t play an important role in the process of forming the network.


Corresponding author: Yu-Pei Xia, College of Chemistry and Chemical Engineering, Weifang University, Weifang, Shandong 261061, P. R. China, E-mail:

Funding source: Research Fund for the Doctoral Program of Weifang University

Award Identifier / Grant number: 2021BS09

  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 Research Fund for the Doctoral Program of Weifang University (NO. 2021BS09).

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

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Received: 2022-04-21
Accepted: 2022-06-28
Published Online: 2022-07-13
Published in Print: 2022-10-26

© 2022 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. The crystal structure of 3-(1-(2-((5-methylthiophen-2-yl)methylene)hydrazinyl)ethylidene)chroman-2,4-dione, C17H14N2O3S
  4. Crystal structure of chlorido-(η 6-toluene)(5,5′-dimethyl-2,2′-bipyridine-κ2 N,N′)ruthenium(II) hexafluoridophosphate(V) ─ acetone (1/1) C22H26ClN2ORuPF6
  5. Crystal structure of 4-(((2-(3-(1-(3-(3-cyanophenyl)-6-oxopyridazin-1(6H)-yl)ethyl)phenyl) pyrimidin-5-yl)oxy)methyl)-1-methylpiperidin-1-ium chloride monohydrate, C30H33N6O2Cl
  6. The crystal structure of 2-chloro-N-((2-chlorophenyl)carbamoyl)nicotinamide, C13H9Cl2N3O2
  7. Crystal structure of 9-(t-butyl)-3,11-dihydro-6H-pyrazolo [1,5-a]pyrrolo[3′,2′:5,6]pyrido[4,3-d]pyrimidin-6-one hemihydrate, C30H32N10O3
  8. Crystal structure of di-μ2-hydroxido-tetrakis(6-methylpyridine-2-carboxylato-k2 N,O) diiron(III) trihydrate C28H32Fe2N4O13
  9. Crystal structure of catena-poly[qua-(μ2-2-aminoisophthalat-κ3 O,O′:O′′)(1,10-phenanthroline-κ2 N,N′)manganese(II)] C20H15MnN3O5
  10. Crystal structure of poly[(bis(isothiocyano)-bis(μ 2-(E)-N′-(pyridin-4-ylmethylene)isonicotinohydrazide))iron(II) – methanol – 1,4-dioxane (1/2/2), C36H44FeN10O8S2
  11. Crystal structure of (E)-N′-(1-(5-chloro-2-hydroxyphenyl)propylidene)-4-hydroxybenzohydrazide, C16H15ClN2O3
  12. Crystal structure of bis(μ2-benzoato-k2O:O′)-bis(μ2-benzoato-k3O,O′:O′)dinitrato-k2O,O′-bis(phenanthroline-k2 N,N′)dierbium(III), C52H36Er2N6O14
  13. Crystal structure of 4-ethyl-2-{[(4-nitrophenyl)methyl]sulfanyl}-6-oxo-1,6-dihydropyrimidine-5-carbonitrile, C14H12N4O3S
  14. Synthesis and crystal structure of 1-((3R,10S,13R,17S)-10,13-dimethyl-3- (phenylamino)hexadecahydro-1H-cyclopenta[α] phenanthren-17-yl)ethan-1-one, C27H39NO
  15. Crystal structre of 1,4-bis(bromomethyl)-2,3,5,6-tetramethylbenzene, C12H16Br2
  16. Crystal structure of 2-(adamantan-1-yl)-5-(3,5-dinitrophenyl)-1,3,4-oxadiazole, C18H18N4O5
  17. Crystal structure of (E)-N′-benzylidene-4-nitrobenzohydrazide – methanol (1/1), C15H15N3O4
  18. The crystal structure of 3-(2-bromophenyl)-1,5-di-p-tolylpentane-1,5-dione, C25H23BrO2
  19. Crystal structure of catena-poly[(μ 2-4,4′-bipyridine-κ2 N:N′)-bis(4-bromobenzoato-κ1 O)zinc(II)], C24H16Br2N2O4Zn
  20. Crystal structure of 1,1′-(1,2-ethanediyl)bis(pyridin-1-ium) bis(1,2-dicyanoethene-1,2-dithiolato-κ2 S:S)zinc(II), C20H14N6ZnS4
  21. Crystal structure of pentacarbonyl-(μ2-propane-1,3-dithiolato-κ4 S:S,S′:S′)-(diphenyl(o-tolyl)phosphine-κ1 P)diiron (Fe-Fe), C27H23Fe2O5PS2
  22. The crystal structure of the cocrystal 4-hydroxy-3,5-dimethoxybenzoic acid–pyrazine-2-carboxamide(1/1), C14H15N3O6
  23. The crystal structure of dichlorido-bis((RS)-2-(4-chlorophenyl)-2-(1,2,4-triazol-1-ylmethyl)hexanenitrile-κ1 N)zinc(II), C30H34Cl4N8Zn
  24. Crystal structure of the cocrystal 2,4,6-triamino-1,3,5-triazine – 1H-isoindole-1,3(2H)-dione – methanol (1/1/1), C12H15N7O3
  25. The crystal structure of methyl 4-((3,5-di-tert-butyl-4-oxocyclohexa-2,5-dien-1-ylidene)methyl) benzoate, C23H28O3
  26. Crystal structure of (poly[µ2-(1H-pyrazol-1-yl)methyl]-1H-benzotriazole-κ 2 N:N)-(nitrato-κ 2 O:O′) silver(I), C9H8AgN7O3
  27. Crystal structure of tetraaqua-bis[4-(1H-1,2,4-triazol-1-yl)benzoato-k1 N]cadmium(II), C18H20CdN6O8
  28. The crystal structure of diaqua-bis(pyrazolo[1,5-a]pyrimidine-3-carboxylato-κ2N,O)nickel(II) dihydrate, C14H16N6O8Ni
  29. Crystal structure of poly[μ2-aqua-aqua-(μ2-1,3-di(1H-imidazol-1-yl)propane-κ2 N:N′)-(μ2-4,4′-(1H-1,2,4-triazole-3,5-diyl)dibenzoato-κ2 O:O′)-(μ4-4,4′-(1H-1,2,4-triazole-3,5-diyl)dibenzoato-κ5 O,O′:O″:O′″:O′″)dicobalt(II)] – water – dimethylformamide (1/1/1) C44H43N11O12Co2
  30. Crystal structure of N-((Z)-amino(((E)-amino(phenylamino)methylene) amino)methylene)benzenaminium chloride – benzo[f]isoquinolino[3,4-b][1,8]naphthyridine – tetrahydrofurane (1/2/2), C60H54ClN11O2
  31. The crystal structure of Chrysosplenol D, C18H16O8
  32. Crystal structure of poly[deca aqua-bis(μ 4-2-(triazol-1-yl)-benzene-1,3,5-tricarboxylato)- bis(μ 5-2-(triazol-1-yl)-benzene-1,3-dicarboxylato-5-carboxyl acid) pentamanganese(II)] dihydrate, C44H42Mn5N12O36
  33. Synthesis and crystal structure of (E)-1-(4-(((E)-3-(tert-butyl)-2-hydroxybenzylidene)amino)phenyl)ethan-1-one O-methyl oxime, C20H24N2O2
  34. The crystal structure of 4,4′-dichloro-6,6′-dimethoxy-2,2′,3,3′,5,5′- hexanitroazobenzene, C14H6N8O14Cl2
  35. Crystal structure of N 2,N 4-dimesitylpentane-2,4-diamine, C23H34N2
  36. Crystal structure of (1,4,7,10,13,16-hexaoxacyclooctadecane-κ 6O6)potassium(2-methylphenylamino)ethyl-2-methylphenylamide ammoniate (1/3.5), [K(18-crown-6)](o-CH3C6H4)NH(CH2)2N(o-CH3C6H4) 3.5 NH3, C28H53.5KN5.5O6
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  39. Crystal structure of (E)-N′-(1-(5-chloro-2-hydroxyphenyl) ethylidene)-4-hydroxybenzohydrazide, C15H13ClN2O3
  40. {2-(((2-aminoethyl)imino)methyl)-6-bromophenolato-κ3 N,N′,O}iron(III) nitrate, C18H20Br2FeN5O5
  41. Crystal structure of 2-(tert-pentyl)anthracene-9,10-dione, C19H18O2
  42. Crystal structure of 5,5′-(1,4-phenylene)bis(1H-imidazol-3-ium) bis(2-(2-(carboxymethyl)phenyl)acetate), C32H30N4O8
  43. Crystal structure of N 2,N 6-bis(2-(((E)-naphthalen-1-ylmethylene)amino)phenyl)pyridine-2,6-dicarboxamide, C41H29N5O2
  44. The crystal structure of 3-amino-1,2,4-triazolium 2,4,5-trinitroimidazolate, C5H5O6N9
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  49. The crystal structure of (4-(2-bromoethoxy)-phenyl)(phenyl)methanone, C15H13BrO2
  50. Crystal structure of (E)-7-bromo-2-(4-methoxybenzylidene)-3,4-dihydronaphthalen-1(2H)-one, C18H15BrO2
  51. Crystal structure of dichlorido-tetrakis((E)-(RS)-1-(2,4-dichlorophenyl)-4,4-dimethyl-2-(1,2,4-triazol-1-yl)pent-1-en-3-ol-κ 1 N)cadmium(II), C60H68O4N12Cl10Cd
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  53. Crystal structure of bis(μ2-2-oxido-2-phenylacetato-κ3 O,O′:O′)-bis(N-oxido-benzamide-κ2 O,O′)-bis(propan-2-olato-κ1 O)dititanium(IV), C36H38N2O12Ti2
  54. Crystal structure of poly[diaqua-(μ2-1H-benzo[d][1,2,3]triazole-5-carboxylato-κ2 O:O′)(μ2-oxalato-κ4O,O:O″,O′″)europium(III)] monohydrate, C9H10N3O9Eu
  55. Crystal structure of bis((N-methyl-2-oxyethyl)amine)-bis(μ 2-N,N,N-tris(2-oxoethyl)amine)-bis(isopropoxy)-bis(μ 3-oxo)tetratitanium(IV)– isopropanol (1/2), C34H76N4O16Ti4
  56. Synthesis and crystal structure of ethyl 4-((4-iodobenzyl)amino)benzoate, C16H16INO2
  57. Crystal structure of (Z)-2-(tert-butyl)-5-((5-(tert- butyl)-2H-pyrrol-2-ylidene)(mesityl)methyl)-1H-pyrrole, C26H34N2
  58. Crystal structure of dimethylammonium poly[μ4-1,1′-(1,4- phenylenebis(methylene))bis(1H-pyrazole-3,5-dicarboxylato-κ6 N,O:O′:N′,O″:O‴) manganese(II)], C22H26MnN6O8
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