Startseite Synthesis and crystal structure of {(N′,N″-(((ethane-1,2-diylbis(oxy))bis(2,1-phenylene))-bis(methaneylylidene))bis(2-hydroxybenzohydrazonato)-κ6 N 2 O 4}copper(II), C30H24CuN4O6
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Synthesis and crystal structure of {(N′,N″-(((ethane-1,2-diylbis(oxy))bis(2,1-phenylene))-bis(methaneylylidene))bis(2-hydroxybenzohydrazonato)-κ6 N 2 O 4}copper(II), C30H24CuN4O6

  • Jie-Qiong Cai ORCID logo EMAIL logo
Veröffentlicht/Copyright: 1. November 2022

Abstract

C30H24CuN4O6, triclinic, P 1 (no. 2), a = 10.8014(2) Å, b = 10.8211(2) Å, c = 13.4530(3) Å, α = 100.308(1)°, β = 113.075(1)°, γ = 99.989(1)°, Z = 2, V = 1370.76(5) Å3, R gt (F) = 0.0365, wR ref(F 2) = 0.0937, T = 297 K.

CCDC no.: 2192173

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: Block, clear dark brown
Size: 0.16 × 0.11 × 0.08 mm
Wavelength: Mo Kα radiation (0.71073 Å)
μ: 0.85 mm−1
Diffractometer, scan mode: Bruker APEX-II, φ and ω-scans
θ max, completeness: 28.5°, >99%
N(hkl)measured, N(hkl)unique, R int: 29057, 6884, 0.086
Criterion for I obs, N(hkl)gt: I obs > 2 σ(I obs), 4706
N(param)refined: 372
Programs: Bruker programs [1], SHELX [2], OLEX2 [3]
Table 2:

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

x y z U iso*/U eq
Cu1 0.65860 (3) 0.41570 (2) 0.26394 (2) 0.03707 (8)
O1 0.68369 (16) 0.34256 (15) 0.13155 (12) 0.0477 (4)
O2 1.05565 (19) 0.2293 (2) 0.20330 (14) 0.0674 (5)
H2 1.021606 0.248766 0.246746 0.101*
O3 0.59432 (17) 0.30767 (18) 0.39026 (14) 0.0580 (5)
O4 0.72534 (17) 0.57703 (14) 0.38453 (12) 0.0493 (4)
O5 0.5524 (2) 0.87919 (18) 0.28810 (16) 0.0914 (8)
H5 0.527284 0.802461 0.252121 0.137*
O6 0.43497 (18) 0.25188 (15) 0.18005 (14) 0.0633 (5)
N1 0.81159 (18) 0.33764 (16) 0.33523 (14) 0.0365 (4)
N2 0.86677 (18) 0.29165 (17) 0.26258 (14) 0.0398 (4)
N3 0.55211 (19) 0.63522 (16) 0.25077 (14) 0.0392 (4)
N4 0.51843 (17) 0.50578 (15) 0.19031 (14) 0.0348 (4)
C1 0.8360 (2) 0.25051 (19) 0.07237 (17) 0.0366 (4)
C2 0.3123 (3) 0.1009 (2) −0.0054 (2) 0.0607 (7)
H2A 0.321643 0.029672 0.023948 0.073*
C3 0.7497 (3) 0.4184 (3) 0.6969 (2) 0.0698 (8)
H3 0.723504 0.437752 0.754793 0.084*
C4 0.7922 (2) 0.29865 (19) 0.16011 (17) 0.0377 (5)
C5 0.8508 (3) 0.9410 (3) 0.6100 (2) 0.0672 (8)
H5A 0.917705 0.956372 0.683351 0.081*
C6 0.3570 (2) 0.3347 (2) 0.02261 (18) 0.0403 (5)
C7 0.6977 (4) 1.0166 (3) 0.4665 (3) 0.0893 (11)
H7 0.661872 1.084039 0.443338 0.107*
C8 0.7045 (2) 0.7931 (2) 0.42607 (17) 0.0396 (5)
C9 0.4543 (3) 0.2407 (3) 0.3567 (2) 0.0605 (7)
H9A 0.400290 0.301956 0.363281 0.073*
H9B 0.449002 0.183066 0.403299 0.073*
C10 0.8280 (2) 0.3671 (2) 0.52385 (18) 0.0414 (5)
C11 0.2253 (3) 0.1866 (3) −0.1640 (2) 0.0667 (8)
H11 0.176892 0.173090 −0.241125 0.080*
C12 0.6589 (2) 0.6600 (2) 0.35005 (17) 0.0372 (5)
C13 0.2425 (3) 0.0819 (3) −0.1195 (2) 0.0677 (7)
H13 0.206629 −0.002326 −0.167104 0.081*
C14 0.8744 (2) 0.3346 (2) 0.43724 (18) 0.0430 (5)
H14 0.956998 0.309322 0.457604 0.052*
C15 0.2809 (3) 0.3127 (2) −0.09260 (19) 0.0531 (6)
H15 0.266908 0.383108 −0.122312 0.064*
C16 0.4139 (2) 0.4678 (2) 0.09376 (18) 0.0408 (5)
H16 0.370854 0.530135 0.066988 0.049*
C17 0.6501 (3) 0.8941 (2) 0.3914 (2) 0.0587 (7)
C18 0.6874 (3) 0.3532 (2) 0.50095 (19) 0.0462 (5)
C19 0.8878 (3) 0.4300 (3) 0.7224 (2) 0.0667 (8)
H19 0.954814 0.455697 0.796811 0.080*
C20 0.3686 (2) 0.2262 (2) 0.0657 (2) 0.0465 (5)
C21 0.6494 (3) 0.3787 (3) 0.5878 (2) 0.0642 (7)
H21 0.555860 0.369058 0.572232 0.077*
C22 0.9644 (2) 0.2205 (2) 0.09846 (19) 0.0454 (5)
C23 0.9996 (3) 0.1779 (3) 0.0117 (2) 0.0639 (7)
H23 1.084742 0.158351 0.028294 0.077*
C24 0.7477 (3) 0.2344 (2) −0.03951 (18) 0.0471 (5)
H24 0.662119 0.253432 −0.057555 0.056*
C25 0.9112 (3) 0.1645 (3) −0.0971 (2) 0.0672 (8)
H25 0.937541 0.137195 −0.153677 0.081*
C26 0.8044 (3) 0.8187 (2) 0.53538 (19) 0.0506 (6)
H26 0.841286 0.752067 0.559305 0.061*
C27 0.3996 (3) 0.1646 (3) 0.2382 (2) 0.0639 (7)
H27A 0.441628 0.092793 0.233263 0.077*
H27B 0.299100 0.129373 0.205979 0.077*
C28 0.9259 (3) 0.4031 (2) 0.6358 (2) 0.0547 (6)
H28 1.019292 0.409026 0.652724 0.066*
C29 0.7970 (4) 1.0396 (3) 0.5744 (2) 0.0842 (10)
H29 0.828119 1.122400 0.623849 0.101*
C30 0.7837 (3) 0.1909 (3) −0.1245 (2) 0.0575 (7)
H30 0.722773 0.179531 −0.199059 0.069*

Source of material

Synthesis of the ligand H 2 L:

The ligand was synthesized from the reaction of 2-hydroxybenzohydrazide (304.30 mg, 0.02 mmol) and a dialdehyde [4] (270.28 mg, 0.01 mmol) according to the procedure reported earlier. Yield (350.06 mg, 65%).

Experimental details

Molecular structure was refined using the SHELX-2018 package. Hydrogen atoms were placed in their geometrically idealized positions and constrained to ride on their parent atoms.

Comment

Many Cu complexes with Schiff bases have been synthesized, and their metal complexes have been studied for decades [5], [6], [7], [8]. The various properties of Schiff base Cu complexes have increased interest. Because these compounds can accommodate one, two or more metal centers and form homonuclear and heteronuclear metal complexes with interesting properties [9], [10], [11].

In the crystal structure of the title complex, the complex was constructed only from the C30H24CuN4O6 molecule, with all bond lengths being within the normal range [4]. The crystal structure shows that the title complex belongs to a triclinic system having the space group P 1 . The hexacoordinate Cu(II) atom (Cu1) is located in the N2O4 coordination environment provided by the two deprotonated sites of the L2– ligand, wherein the coordination atom includes N2, O2, O3 and N3, O4, O5 (cf. the figure).


Corresponding author: Jie-Qiong Cai, School of Chemical and Biological Engineering, Lanzhou Jiaotong University, Lanzhou 730070, P. R. China, E-mail:

  1. Author contributions: The author has accepted responsibility for the entire content of this submitted manuscript and approved submission.

  2. Research funding: None declared.

  3. Conflict of interest statement: The author declares no conflicts of interest regarding this article.

References

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Received: 2022-08-09
Accepted: 2022-10-14
Published Online: 2022-11-01
Published in Print: 2023-01-27

© 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. Crystal structure of undecacalcium decaarsenide, Ca11As10
  4. Crystal structure of catena-poly[diiodido-(μ2-1,5-dimethyl-2-phenyl-4-((pyridin-4- ylmethylene)amino)-1,2-dihydro-3H -pyrazol-3-one-κ2 N: O)zinc(II)], C17H16I2N4OZn
  5. The crystal structure of 5,10,15,20-tetrakis(4-(tert-butyl)phenyl)porphyrin-21,23-diido-κ4 N 4-naphthalocyanido-κ4 N 4-neodymium(IV) - chloroform (1/6) C114H90N12Cl18Nd
  6. The crystal structure of 1-(4-bromophenyl)-3-(2-chlorobenzyl)urea, C14H12BrClN2O
  7. Crystal structure of bis[benzyl(methyl)carbamodithioato-κ 2 S,S′]-di-n-butyltin(IV), C26H38N2S4Sn
  8. Crystal structure of (E)-3-(2-(4-(diethylamino)-2-hydroxystyryl)-3,3-dimethyl-3H-indol-1-ium-1-yl)propane-1-sulfonate – methanol (1/2), C25H32N2O4S⋅2CH3OH
  9. Synthesis and crystal structure of {(N′,N″-(((ethane-1,2-diylbis(oxy))bis(2,1-phenylene))-bis(methaneylylidene))bis(2-hydroxybenzohydrazonato)-κ6 N 2 O 4}copper(II), C30H24CuN4O6
  10. The crystal structure of ((E)-2,4-dibromo-6-(((5-(nitro)-2-oxidophenyl)imino)methyl)phenolato-κ 3 N,O,O′)tris(pyridine-κN)manganese(II), C28H21Br2MnN5O4
  11. Synthesis and crystal structure of 1-((3R,10S,13R,17S)-10,13-dimethyl-3-(p-tolylamino)hexadecahydro-1H-cyclopenta-[a]phenanthren-17-yl)ethan-1-one, C28H41NO
  12. The crystal structure of 3-nitrobenzene-1,2-dicarboxylic acid—pyrazine-2-carboxamide(1/1), C13H10N4O7
  13. Crystal structure of poly[tetrakis(μ3-2-aminonicotinato-κ3N,O,O′)-(μ2-oxalato-κ4 O,O′:O″,O′″)-(μ4-oxalato-κ6 N:N′:O,O′:O″,O′″)dicopper(I)-disamarium(III)], [SmCu(C6N2H5O2)2(C2O4)] n
  14. The crystal structure of 2,3,4-trihydroxybenzoic- acid—pyrazine-2-carboxamide—water (1/1/1), C12H13N3O7
  15. Crystal structure of N-ethyl-4-[3-(trifluoromethyl)-phenyl]piperazine-1-carbothioamide, C14H18F3N3S
  16. The crystal structure of 3-anilino-1,4-diphenyl-4H-1,2,4-triazol-1-ium iodide, C20H17N4I
  17. The crystal structure of (tris(2-benzimidazolylmethyl)amine)-benzoato-copper(II) perchlorate monohydrate, CuC31H28N7O7Cl
  18. Crystal structure of [2-hydroxy-3-methyl-benzoato-k1 O-triphenyltin(IV)], C26H22O3Sn
  19. Crystal structure of diaqua-bis(4-(hydroxymethyl)-benzoato-k1 O)zinc(II), C16H18O8Zn
  20. The crystal structure of dicarbonyl-(N-nitroso-N-oxido-phenylamine-κ 2 O,O)-rhodium(I), C8H5N2O4Rh
  21. The crystal structure of oxalic acid – 2-ethoxybenzamide (2/1), C20H24N2O8
  22. The crystal structure of ethyl 7-ethyl-5-methyl-4,7-dihydrotetrazolo[1,5-a]pyrimidine-6-carboxylate, C10H15N5O2
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  24. Crystal structure of 14-O-acetyldelcosine, C26H41NO8
  25. The crystal structure of poly[(1,10-phenanthroline-κ2 N,N′)-(μ 4-2-chlorobenzene-1,3-dicarboxylato-κ5 O:O′:O″:O‴) cadmium(II)] monohydrate, C20H13CdClN2O5
  26. Crystal structure of propane-1,3-diylbis(diphenylphosphine sulfide) ethanol solvate, C27H26P2S2
  27. Crystal structure of bis{[(4-diethylamino-2-hydroxy-benzylidene)-hydrazinocarbonylmethyl]-trimethylammonium} tetrabromozincate, C32H54N8O4ZnBr4
  28. Synthesis and crystal structure of dimethyl 2,2′-(2,5-bis(4-hydroxyphenyl)-2,5-dihydrofuran-3,4-diyl)dibenzoate, C34H30O7
  29. Synthesis and crystal structure of 2-(2-oxo-2-phenylethyl)-4H-chromen-4-one, C17H12O3
  30. The crystal structure of tetra(imidazole-κ1 N)zinc(II) μ2-oxido-hexaoxido-divanadium(VI) C12H16N8O6V2Zn
  31. Crystal structure of S-2-(1-(5-methylpyridin-2-ylamino)octyl)-3-hydroxynaphthalene-1,4-dione, C24H28N2O3
  32. Crystal structure of bis(μ2-5-chloro-2-oxido-N-(1-oxido-2-oxo-2-phenylethylidene)-benzohydrazonato-κ5 N,O,O′:N′,O′′)-oktakis(pyridine-κ1 N)trinickel(II) – methanol – pyridine (1/1/1) C76H65N13Cl2Ni3O9
  33. The crystal structure of methyl 3,5-diaminobenzoate, C8H10N2O2
  34. Crystal structure of 10-(9H-carbazol-9-yl)-5H-dibenzo[a,d][7]annelen-5-one, C27H17NO
  35. Crystal structure of ethyl 1-(2-hydroxyethyl)-4-((4-methoxyphenyl)amino)-5-oxo-2,5-dihydro-1H-pyrrole-3-carboxylate, C16H20N2O5
  36. The crystal structure of 1-(4-bromophenyl)-3-cycloheptylurea, C14H19BrN2O
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  40. Synthesis and crystal structure of 2-(2-(2-fluorophenyl)-2-oxoethyl)-4H-chromen-4-one, C17H11FO3
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  42. Crystal structure of 1-(2-(4-chlorophenethyl)-2-hydroxy-3,3-dimethylbutyl)-1H-1,2,4-triazol-4-ium nitrate, C16H23N4O4Cl
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  45. The crystal structure of ethyl 2′-hydroxy-4′,6′-dimethoxy-3-(4-methoxynaphthalen-1-yl)-5-oxo-2,3,4,5-tetrahydro-[1,1′-biphenyl]-4-carboxylate, C28H28O7
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