Startseite Crystal structure of dichlorido-bis(1-[(2-ethyl-benzimidazole-1-yl)methyl]-1H–benzotriazole) cadmium(II), C32H32CdN10OCl2
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Crystal structure of dichlorido-bis(1-[(2-ethyl-benzimidazole-1-yl)methyl]-1H–benzotriazole) cadmium(II), C32H32CdN10OCl2

  • Jing Yang ORCID logo EMAIL logo , Tan-Peng Zhou , Meng-Meng Cao und Xia Wang ORCID logo
Veröffentlicht/Copyright: 19. Juni 2024

Abstract

C32H32CdN10OCl2, monoclinic, C2/c (no. 15), a = 28.820(3) Å, b = 13.1075(2) Å, c = 16.7266(19) Å, β = 149.29(3)°, Z = 4, V = 3226.9(15) Å3, R gt (F) = 0.0341, wR ref (F2) = 0.0893, T = 293(2) K.

CCDC no.: 2359939

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: 0.14 × 0.10 × 0.08 mm
Wavelength:

μ:
Cu Kα radiation (1.54184 Å)

7.30 mm−1
Diffractometer, scan mode:

θmax, completeness:
Xcalibur, ω

67.1°, >99 %
N(hkl)measured, N(hkl)unique, Rint: 11088, 2875, 0.041
Criterion for Iobs, N(hkl)gt: Iobs > 2 σ(Iobs), 2552
N(param)refined: 218
Programs: CrysAlisPRO, 1 SHELX 2
Table 2:

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

Atom x y z Uiso*/Ueq
Cd1 −0.5000 0.78023 (3) −1.2500 0.05212 (12)
Cl1 −0.53670 (6) 0.88820 (8) −1.41873 (11) 0.0696 (3)
N1a −0.2758 (7) 0.2827 (10) −0.8888 (14) 0.068 (2)
N1Ab −0.2438 (10) 0.2719 (15) −0.860 (2) 0.068 (2)
N2a −0.2732 (11) 0.3813 (18) −0.874 (2) 0.063 (2)
N2Ab −0.2538 (16) 0.366 (3) −0.860 (3) 0.063 (2)
N3a −0.2049 (8) 0.4157 (15) −0.8165 (16) 0.048 (3)
N3Ab −0.1851 (12) 0.426 (2) −0.796 (2) 0.048 (3)
N4 −0.25840 (17) 0.58587 (19) −0.9229 (3) 0.0468 (6)
N5 −0.38578 (17) 0.6766 (2) −1.1185 (3) 0.0479 (6)
C6a −0.1585 (6) 0.3459 (4) −0.7842 (13) 0.0552 (18)
C5a −0.2052 (5) 0.2574 (5) −0.8332 (10) 0.059 (2)
C4a −0.1771 (5) 0.1638 (4) −0.8218 (9) 0.077 (2)
H4a −0.2083 0.1046 −0.8546 0.092*
C3a −0.1022 (6) 0.1587 (5) −0.7614 (10) 0.089 (3)
H3a −0.0834 0.0962 −0.7538 0.107*
C2a −0.0555 (5) 0.2472 (6) −0.7124 (11) 0.084 (3)
H2a −0.0054 0.2438 −0.6720 0.101*
C1a −0.0836 (6) 0.3408 (5) −0.7238 (13) 0.072 (2)
H1a −0.0524 0.4000 −0.6910 0.087*
C6Ab −0.1363 (9) 0.3531 (6) −0.7651 (18) 0.0552 (18)
C5Ab −0.1732 (7) 0.2569 (7) −0.8066 (15) 0.059 (2)
C4Ab −0.1321 (7) 0.1713 (6) −0.7789 (13) 0.077 (2)
H4Ab −0.1568 0.1069 −0.8066 0.092*
C3Ab −0.0542 (7) 0.1818 (8) −0.7098 (13) 0.089 (3)
H3Ab −0.0268 0.1245 −0.6912 0.107*
C2Ab −0.0174 (7) 0.2780 (9) −0.6684 (15) 0.084 (3)
H2Ab 0.0347 0.2850 −0.6221 0.101*
C1Ab −0.0584 (8) 0.3636 (7) −0.6960 (18) 0.072 (2)
H1Ab −0.0338 0.4280 −0.6683 0.087*
C7 −0.1832 (2) 0.5282 (3) −0.7797 (4) 0.0571 (8)
H7AAa −0.1723 0.5476 −0.7085 0.068*
H7ABa −0.1286 0.5426 −0.7294 0.068*
H7BCb −0.1275 0.5552 −0.7199 0.068*
H7BDb −0.1807 0.5395 −0.7187 0.068*
C8 −0.2216 (2) 0.5829 (3) −1.0164 (4) 0.0562 (8)
H8 −0.1678 0.5458 −0.9334 0.067*
C9 −0.2549 (2) 0.6167 (3) −1.1378 (4) 0.0612 (9)
H9 −0.2230 0.6018 −1.1371 0.073*
C10 −0.3348 (2) 0.6725 (3) −1.2616 (4) 0.0575 (8)
H10 −0.3551 0.6941 −1.3415 0.069*
C11 −0.3849 (2) 0.6967 (2) −1.2684 (4) 0.0512 (7)
H11 −0.4386 0.7338 −1.3516 0.061*
C12 −0.3520 (2) 0.6635 (2) −1.1464 (3) 0.0433 (6)
C13 −0.2725 (2) 0.6070 (2) −1.0244 (4) 0.0451 (6)
C14 −0.3285 (2) 0.6292 (2) −0.9859 (4) 0.0482 (7)
C15 −0.3419 (3) 0.6218 (3) −0.9173 (5) 0.0667 (9)
H15A −0.3579 0.6886 −0.9202 0.080*
H15B −0.2853 0.6012 −0.8086 0.080*
C16 −0.4159 (3) 0.5460 (4) −1.0043 (5) 0.0812 (13)
H16A −0.4715 0.5643 −1.1131 0.122*
H16B −0.4249 0.5473 −0.9609 0.122*
H16C −0.3980 0.4787 −0.9939 0.122*
O1c −0.1312 (5) 0.3773 (7) −0.0224 (9) 0.120 (3)
H1Bc −0.1766 0.3319 −0.1233 0.179*
H1Cc −0.1246 0.4466 −0.0242 0.179*
  1. aOccupancy: 0.571 (7), bOccupancy: 0.429 (7), cOccupancy: 0.5.

1 Source of materials

All starting materials are commercially available without further purification. The 1-[(2-ethyl-benzimidazole-1-yl)methyl]-1H–benzotriazole (ebmb) was prepared according to the literature method with some modifications. 3 The ligand 1-[(2-ethyl-benzimidazole-1-yl)methyl]-1H–benzotriazole (0.02 mmol, 0.0056 g) was dissolved in 2 mL of methanol solution and the solution was slowly added to 2 ml of CdCl2 (0.02 mmol, 0.0046 g) of methanol solution. The prepared solution was placed at room temperature and colorless crystals were obtained after fifteen days.

2 Experimental details

H atoms were generated geometrically and refined as riding atoms with C–H = 0.93 Å and the Uiso(H) = 1.2 times Ueq(C) for aromatic H atoms, with C–H = 0.97 Å and Uiso(H) = 1.2 times Ueq(C) for methylene H atoms, and with C–H = 0.96 Å and Uiso(H) = 1.5 times Ueq(C) for methyl H atoms.

3 Comment

Nitrogen heterocyclic compounds, as common electron-rich groups, are widely used as ligands for synthesizing complexes due to their structural diversity and rich applications. For example, Liu’s team 4 synthesized two complexes, [Ag2(L)2](PF6)2 and [Au2(L)2](PF6)2, using compounds containing bis–N-heterocyclic carbenes as ligands; Wittmann’s team 5 synthesized six Cu(II) complexes using indoles and benzimidazoles as ligands and cross-bridged tetraaza macrocyclic ligand metal complexes synthesized by Hubin’s team. 6

X-ray crystal structure analysis shows that the title complex is a mononuclear structure with cadmium as the central atom. The central cadmium (II) ion forms a mononuclear structure with the two organic ligands in a single-tooth coordination. As shown in Figure, the central atom Cd(II) is associated with two Cl ions (Cl1 and Cl1i) and two N atoms (N5 and N5i from two ebmb ligands). The Cd–Cl and Cd–N bonds around Cd1 are of length: Cd1–Cl1: 2.4401(10) Å; Cd1–Cl1i: 2.4402(10) Å; Cd1–N5: 2.251(3) Å; Cd1–N5i: 2.251(3) Å. The range of bond angles around Cd1 is 105.79(14)°−113.84(8)°. 7 The smallest bond angle is N5–Cd1–N5i, the largest is N5i–Cd1–Cl1 and N5–Cd1–Cl1i. The dihedral angle of the benzotriazole and benzimidazole rings in each ligand is 73.2°. The benzotriazole ring in the ligand ebmb is a disordered atom with an occupancy of 0.571: 0.429. In addition, the distance between the adjacent benzotriazole rings and the adjacent benzoimidazole rings is 3.707 Å and 3.472 Å, indicating that there may be two kinds of intermolecular p-p conjugation between the adjacent cadmium units. The cadmium element is expanded into a two-dimensional network to make the structure more stable.


Corresponding author: Jing Yang, College of Pharmacy, Henan University of Chinese Medicine, Zhengzhou 450046, P.R. China, E-mail:

Funding source: Key Scientific and Research Projects of the Education Department of Henan Province

Award Identifier / Grant number: 21A430024

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

  2. Competing interests: The authors declare no conflicts of interest regarding this article.

  3. Research funding: This work was financially supported by the Key Scientific and Research Projects of the Education Department of Henan Province (No. 21A430024).

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Received: 2024-04-11
Accepted: 2024-06-02
Published Online: 2024-06-19
Published in Print: 2024-10-28

© 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. Editorial
  3. Editorial 2024 – New developments and changes of Zeitschrift für Kristallographie – New Crystal Structures
  4. New Crystal Structures
  5. Hydrogen bonding and π⋅⋅⋅halogen interactions in the crystal structure of bis(theophyllinium) hexachloridoplatinate(IV) monohydrate
  6. The crystal structure of 6-amino-2-carboxypyridin-1-ium perchlorate, C6H7ClN2O6
  7. Crystal structure of poly[(μ4-(3-amino-1H-1,2,4-triazol-1-yl)benzene-1,3-dicarboxylato-κ 4 N:O:O':O')(1-methylpyrroldin-2-one-κ1O)dicopper(II)] – 1-methylpyrroldin-2-one (1/3), C40H48Cu2N12O12
  8. The crystal structure of 18-crown-6-k6O6(2,4,5-trinitroimidazol-1-ido-k1O)potassium(I)
  9. Crystal structure of poly[tetraaqua-bis(μ2-5-bromoisophthalato-κ3O,O:O)-(μ2-1,5-bis(imidazol-2-methyl)pentane-κ2N:N)dicadmium(II)] dihydrate
  10. Crystal structure of (5R,6S,E)-5-acetoxy-2-methyl-6-((2aR,3R,5aS,5bS,11aR,12aS)-2a,5a,8,8-tetramethyl-9-oxotetradecahydro-1H,12H-cyclopenta[a]cyclopropa[e]phenanthren-3-yl)hept-2-enoic acid, C32H48O5
  11. The crystal structure of poly[diaqua-bis(μ2 -thiocyanato-κ2N:O)cobalt(II) monohydrate
  12. The crystal structure of 1,3,5-tri(1H-imidazol-1-yl)benzene–2,3,5,6-tetrachlorobenzene-1,4-dicarboxylic acid (1/1)
  13. Crystal structure of dichlorido-bis(1-[(2-ethyl-benzimidazole-1-yl)methyl]-1H–benzotriazole) cadmium(II), C32H32CdN10OCl2
  14. The crystal structure of N′-(tert-butyl)-N′-(3,5-dimethylbenzoyl)-3-methoxy-N,2-dimethylbenzohydrazide, C23H30N2O3
  15. Crystal stucture of 3-benzamido-N-(2-bromo-4-(perfluoropropan-2-yl)-6-(trifluoromethyl)phenyl)-2-fluorobenzamide
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  18. The crystal structure of poly[hexaqua-tetrakis(μ4-pyridine-2,4-dicarboxylate-κ5N: O: O′: O″: O‴)-bi(μ2-pyridine-2,4-dicarboxylate-κ3N: O: O′)-digadolinium(III)tricopper (II)], [Gd2Cu3(C7H3NO4)6(H2O)6] n
  19. Crystal structure of poly[bis(4-(4-(pyridin-4-yl)phenyl)pyridin-1-ium-κ1N)-(μ4-benzene-1,2,4,5-tetracarboxylato-κ5O:O′: O″:O‴:O⁗)-(μ2-2,5-dicarboxyterephthalato-κ2O:O′)dizinc(II)], C52H32N4O16Zn2
  20. The crystal structure of 4-(3-carboxy-1-ethyl-6-fluoro-4-oxo-1,4-dihydroquinolin-7-yl)piperazin-1-ium 2-carboxy-6-nitrobenzoate monohydrate, C24H25FN4O10
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  27. Crystal and molecular structure of 5-bromopyridine-2,3-diamine
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  29. Crystal structure of thiocyanate-κ1N-bis(μ1-2,6-diformyl-4-methylphenol oxime-κ2N,O)-manganese(III) acetonitrile solvate, C21H21MnN6O6S
  30. The crystal structure of pyrrolidin-1-yl pivalate, C9H13NO4
  31. The crystal structure of 2,2′-(2,2-diphenylethene-1,1-diyl)bis(1,4-dimethoxybenzene), C30H28O4
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  54. The crystal structure of catena-poly[aqua-nitrato-κ3O,O:O′′-(1,10-phenanthroline-κ2N,N)sodium(I)], C24H18N6O7Na2
  55. Retractions
  56. Retraction of: Crystal structure of bis[diaquaisonicotinatosamarium(III)]-µ-isonicotinato-[diisonicotinatocopper(II)], CuSm2(C6H4NO2)8(H2O)4
  57. Retraction of: Crystal structure of aqua(2,2-bipyridine-k 2 N:N′)(nitrato)-(4-aminobenzoato)cadmium(II) nitrate, [Cd(H2O)(NO3)(C10H8N2)(C7H7NO2)][NO3]
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