Startseite Crystal structure of bis(μ2-benzenesulfonato-κ2O:O′)-bis(μ2-6,6′-((ethane-1,2-diylbis(azaneylylidene))bis(methaneylylidene))-bis(2-methoxyphenolato-κ6O,O′:O′,N,N′,O′′:O′′,O′′′))disodium(I)dicopper(II)
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Crystal structure of bis(μ2-benzenesulfonato-κ2O:O′)-bis(μ2-6,6′-((ethane-1,2-diylbis(azaneylylidene))bis(methaneylylidene))-bis(2-methoxyphenolato-κ6O,O′:O′,N,N′,O′′:O′′,O′′′))disodium(I)dicopper(II)

  • Deyang Ma , Shaoliang Zhang ORCID logo EMAIL logo , Yanlan Wang und Shanshan Li
Veröffentlicht/Copyright: 15. Januar 2024

Abstract

C48H46Cu2N4Na2O14S2, triclinic, P 1 (no. 2), a = 11.2259(11) Å, b = 11.6492(11) Å, c = 11.7594(12) Å, α = 11.2259(11)°, β = 11.6492(11)°, γ = 11.7594(12)°, V = 1248.5(2) Å3, Z = 1, Rgt(F) = 0.0554, wRref(F2) = 0.1605, T = 173 K.

CCDC no.: 2322389

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: Purple block
Size: 0.36 × 0.28 × 0.15 mm
Wavelength: Mo Kα radiation (0.71073 Å)
μ: 1.02 mm−1
Diffractometer, scan mode: Bruker SMART APEX II, φ and ω
θmax, completeness: 25.0°, 96 %
N(hkl)measured, N(hkl)unique, Rint: 6242, 4323, 0.040
Criterion for Iobs, N(hkl)gt: Iobs > 2σ(Iobs), 3289
N(param)refined: 327
Programs: Bruker [1], SHELX [2]
Table 2:

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

Atom x y z Uiso*/Ueq
Cu1 1.03676 (5) 0.70211 (4) 0.01424 (5) 0.0433 (2)
S1 0.46860 (9) 0.77890 (9) 0.18912 (10) 0.0420 (3)
Na1 0.75305 (15) 0.91455 (14) −0.05959 (15) 0.0446 (4)
O1 0.9022 (3) 0.8496 (3) 0.0659 (3) 0.0446 (7)
O2 0.9363 (3) 0.7243 (2) −0.0943 (3) 0.0438 (6)
O3 0.7077 (3) 1.0595 (3) 0.0924 (3) 0.0516 (7)
O4 0.8061 (3) 0.8394 (3) −0.2662 (3) 0.0545 (8)
O5 0.5882 (3) 0.8069 (3) 0.0848 (3) 0.0607 (8)
O6 0.4473 (3) 0.6588 (3) 0.1991 (3) 0.0605 (8)
O7 0.3475 (3) 0.8884 (3) 0.1864 (3) 0.0628 (9)
N1 1.1373 (3) 0.6721 (3) 0.1284 (4) 0.0507 (9)
N2 1.1787 (3) 0.5555 (3) −0.0406 (4) 0.0512 (9)
C1 1.0038 (5) 0.9437 (4) 0.2736 (4) 0.0546 (11)
H1 1.0714 0.9158 0.3150 0.066*
C2 0.9022 (5) 1.0552 (5) 0.2873 (4) 0.0600 (12)
H2 0.9012 1.1038 0.3366 0.072*
C3 0.8000 (5) 1.0976 (4) 0.2287 (4) 0.0516 (10)
H3 0.7290 1.1739 0.2395 0.062*
C4 0.8030 (4) 1.0273 (4) 0.1545 (4) 0.0446 (9)
C5 0.9078 (4) 0.9109 (4) 0.1373 (4) 0.0405 (9)
C6 1.0102 (4) 0.8687 (4) 0.1984 (4) 0.0455 (9)
C7 1.1174 (4) 0.7496 (4) 0.1943 (4) 0.0505 (10)
H7 1.1776 0.7260 0.2428 0.061*
C8 1.2415 (5) 0.5450 (5) 0.1419 (6) 0.0753 (15)
H8A 1.2037 0.4806 0.2200 0.090*
H8B 1.3204 0.5539 0.1523 0.090*
C9 1.2863 (5) 0.4979 (5) 0.0231 (6) 0.0705 (14)
H9A 1.3696 0.5226 −0.0383 0.085*
H9B 1.3067 0.4024 0.0491 0.085*
C10 1.1860 (4) 0.5091 (4) −0.1295 (5) 0.0562 (11)
H10 1.2546 0.4316 −0.1413 0.067*
C11 1.0982 (4) 0.5664 (4) −0.2108 (4) 0.0510 (10)
C12 1.1366 (5) 0.5173 (5) −0.3193 (5) 0.0677 (14)
H12 1.2103 0.4424 −0.3283 0.081*
C13 1.0685 (5) 0.5769 (5) −0.4091 (5) 0.0705 (14)
H13 1.0964 0.5447 −0.4813 0.085*
C14 0.9573 (5) 0.6857 (5) −0.3954 (4) 0.0592 (12)
H14 0.9108 0.7268 −0.4588 0.071*
C15 0.9145 (4) 0.7340 (4) −0.2900 (4) 0.0477 (10)
C16 0.9829 (4) 0.6738 (4) −0.1929 (4) 0.0432 (9)
C17 0.5846 (5) 1.1569 (5) 0.1269 (5) 0.0739 (15)
H17A 0.5436 1.1330 0.2209 0.111*
H17B 0.5217 1.1637 0.0846 0.111*
H17C 0.6044 1.2403 0.0987 0.111*
C18 0.7431 (6) 0.9160 (6) −0.3656 (5) 0.0837 (18)
H18A 0.8100 0.9495 −0.4446 0.126*
H18B 0.6698 0.9886 −0.3378 0.126*
H18C 0.7060 0.8628 −0.3827 0.126*
C19 0.5019 (4) 0.7513 (4) 0.3361 (4) 0.0428 (9)
C20 0.4368 (6) 0.6782 (5) 0.4520 (5) 0.0691 (14)
H20 0.3709 0.6437 0.4554 0.083*
C21 0.4670 (8) 0.6543 (6) 0.5647 (5) 0.099 (2)
H21 0.4204 0.6053 0.6449 0.119*
C22 0.5647 (7) 0.7022 (6) 0.5592 (6) 0.0824 (17)
H22 0.5882 0.6828 0.6351 0.099*
C23 0.6285 (6) 0.7781 (6) 0.4441 (5) 0.0757 (15)
H23 0.6921 0.8149 0.4415 0.091*
C24 0.5992 (5) 0.8007 (5) 0.3316 (4) 0.0571 (11)
H24 0.6457 0.8500 0.2516 0.068*

1 Source of materials

The salen-type Schiff base ligand was synthesized following the procedure described in the literature [3]. The Schiff base (0.1 mmol, 32.8 mg) was dissolved in 10 mL of methanol. To this solution, CuCl2·2H2O (0.1 mmol, 17.0 mg) and sodium benzenesulfonate (0.3 mmol, 54.0 mg) were added. The stirring of this mixture was maintained for additional 2 h and then filtered, yielding a clear solution. The solution was transferred to a test tube and subsequently exposed to diethyl ether vapor in order to enhance diffusion. Following a period of two weeks, single crystals with a purple color and needle-like shape were obtained.

2 Experimental details

Hydrogen atoms were assigned with common isotropic displacement factors Uiso(H) = 1.2 times Ueq (C, phenyl ring and methylene carbon) and Uiso(H) = 1.5 times Ueq(C, methyl carbon). All the H atoms were refined as riding on their parent atom.

3 Comment

Due to the ability of oxygen and nitrogen atoms to bind to metal centers through various coordination modes, salen ligands are highly flexible ligands that facilitate the formation of a wide range of coordination compounds [4], [5], [6]. In recent decades, there has been growing interest in salen-type heterometallic coordination complexes due to their significant impact in the fields of magnetochemistry and bioinorganic chemistry [7], [8], [9], [10]. However, the research on salen-type Schiff-base complexes containing sulfonate ligands is still in its infancy. As part of our ongoing research on the modulating influence of Schiff base ligands on transition metal complexes, we report a Cu(II)–Na(I) complex here.

The asymmetric unit of the title compound consists of one salen ligand, one Cu(II) ion, one Na(I) ion and one benzenesulfonate. The Cu center is four coordinated, which is surrounded by two oxygen atoms and two nitrogen atoms from the salen ligands. Additionally, the Na center is coordinated by four oxygen atoms from the salen ligands and two oxygen atoms from the sulfonate, leading to a six-coordinate configuration. The bond lengths for Cu–O/N in title compound range from 1.910(3) to 1.951(3) Å, and the bond lengths for Na–O range from 2.338(3) to 2.694(3) Å. The bond lengths around metal centers are in the expected ranges [11, 12].


Corresponding author: Shaoliang Zhang, School of Chemistry and Chemical Engineering, Liaocheng University, Liaocheng 252059, Shandong, China, E-mail:

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

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

  3. Research funding: Science and Technology Foundation of Liaocheng University (318051728); Introduction and Cultivation Program for Young Innovative Talents in Shandong Provincial Colleges and Universities (Innovation Team of Functional Organometallic Materials Presided by Prof. Yanlan Wang).

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Received: 2023-11-08
Accepted: 2023-12-28
Published Online: 2024-01-15
Published in Print: 2024-04-25

© 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. Solvothermal synthesis and crystal structure of aqua-tris(p-acetamidobenzoate-κ2O,O′)-(2,2′-bipyridine-κ2N,N′)terbium(III) - water - methanol (1/1/1)
  4. Crystal structure of hexaaquazinc(II) catena-poly[bis(1-(3-carboxyphenyl)-5-methyl-4-oxo-1,4-dihydropyridazine-3-carboxylato-κ2O,O′)-bis(μ2-1-(3-carboxyphenyl)-5-methyl-4-oxo-1,4-dihydropyridazine-3-carboxylato-κ2O:O′)trizinc(II)] hexahydrate C26H36N4O20Zn2
  5. The crystal structure of valinyl-N-ium-4-(5-(thiophen-2-yl)isoxazol-3-yl)phenyl trifluoroacetate
  6. Crystal structure of bis(3,5-diisopropyl-1H-pyrazol-4-ammonium) tetrafluoroterephthalate, 2[C9H18N3][C8F4O4]
  7. Crystal structure of aqua-octakis(μ3-salicylato)-(1,10-phenanthroline)-(acetonitrile)-dicobalt(II)-trititanium(IV), C70H45N3O25Co2Ti3
  8. Crystal structure of catena-poly[aqua-(μ2-4,4′-diimidazole diphenyl ether-κ2N:N′)-(sulfato-κ1O)-cobalt(II)] – dimethylformamide (2/1), C39H37CoN9O8S
  9. Crystal structure of (5R,8R,9R,10R,12R, 13R,14R,17S)-2-(E-3-fluorobenzylidene)-12-hydroxy-4,4,8,10,14-pentamethyl-17-((R)-2,6,6-trimethyltetrahydro-2H-pyran-2-yl) hexadecahydro-3H-cyclopenta[a]phenanthren-3-one, C37H53FO3
  10. Crystal structure of (Z)-4-((4,5,6-trimethoxy-3-oxobenzofuran-2(3H)-ylidene)methyl)phenyl diphenylphosphinate, C30H25O7P
  11. Crystal structure of 3-((5-methylpyridin-2-yl)amino)-1-phenylpropan-1-one, C15H16N2O
  12. The crystal structure of (R)-9-(5-methoxy-2-methyl-2,3-dihydro-1H-cyclopenta[a]naphthalen-1-ylidene)-9H-thioxanthene, C28H22OS
  13. Crystal structure of diaqua-bis[1-(1-(hydroxymethyl)-1H-pyrazol-3-yl)-5-methyl-1H-1,2,3-triazole-4-carboxylato-κ2N,O)] manganese(II), C16H20MnN10O8
  14. The crystal structure of t-butyl 7-[4-(4-fluorophenyl)-2-[(methanesulfonyl)(methyl)amino]-6-(propan-2-yl)pyrimidin-5-yl]-3,5-dihydroxyhept-6-enoate, C26H36FN3O6S
  15. The crystal structure of samarium sulfate pentahydrate, Sm2(SO4)3(H2O)5
  16. The crystal structure of [triaqua-(8-carboxymethoxy-quinoline-2-carboxylate-κ 4 N,O,O,O)-zinc(II)] monohydrate, C12H15NO9Zn
  17. The crystal structure of 2,3-difluoro-11H-benzo-[4,5]imidazo[2,1-a]isoindol-11-one, C14H6F2N2O
  18. The crystal structure of 2,3-di(9H-carbazol-9-yl)-9H-fluoren-9-one, C37H22N2O
  19. The crystal structure of 5-(2-chloro-3-(3,6-di-tert-butyl-9H-carbazol-9-yl)phenyl)-10,11-dihydro-5H-dibenzo[b,f]azepine, C40H39ClN2
  20. Crystal structure of 2-bromo-1-hydroxy-3-(3-methylbut-2-enyloxy)-9H-xanthen-9-one, C18H15BrO4
  21. Crystal structure of bis(μ2-benzenesulfonato-κ2O:O′)-bis(μ2-6,6′-((ethane-1,2-diylbis(azaneylylidene))bis(methaneylylidene))-bis(2-methoxyphenolato-κ6O,O′:O′,N,N′,O′′:O′′,O′′′))disodium(I)dicopper(II)
  22. The crystal structure of (E)-1,2-bis(benzo[e][1,2]azaborinin-2(1H)-yl)ethene, C18H16B2N2
  23. Crystal structure of 3-oxo-urs-12-en-28-benzyl ester, C37H52O3
  24. The crystal structure of ethyl (E)-1-chloro-3-(4-chloro-1-methyl-1H-indole-2-carbonyl)-4-oxo-2-phenylcyclooct-2-ene-1-carboxylate, C27H25Cl2NO4
  25. The crystal structure of 4,4′-((5-bromo-2-iodo-1,3-phenylene)bis(oxy))bis(tert-butylbenzene) ─ ethanol (2/1), C26H28BrIO2
  26. Crystal structure of (E)-1-(4-(benzyloxy)-2-hydroxyphenyl)-3-(dimethylamino)prop-2-en-1-one, C18H19NO3
  27. The crystal structure of N1,N3-bis(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)\ propanediamide hydrate, C25H26N6O4, 2(H2O)
  28. The crystal structure of 2,5-bis[(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)amino]cyclohexa-2,5-diene-1,4-dione, C28H26N6O4
  29. Crystal structure of 3,4-bis[2-(hydroxymethyl)-pyrrolidin-1-yl] cyclobut-3-ene-1,2-dione hydrate, C14H22N2O5
  30. The crystal structure of 2-(3,4–dichlorobenzyl)-1H-benzimidazole, C14H10Cl2N2
  31. The crystal structure of 2-(2-((4,6-dimethoxypyrimidin-2-yl)oxy)phenyl)-4-(piperidin-1-yl)-5H-chromeno[2,3-d]pyrimidine, C28H27N5O4
  32. The crystal structure of 6-(benzofuran-2-yl)-2-oxo-4,5-diphenyl-3,4-dihydro-2H-pyran-3-carbonitrile, C26H17NO3
  33. Crystal structure of N-(4-bromobenzyl)-3-(difluoromethyl)-1-methyl-N-(pyridin-2-yl)-1H-pyrazole-4-carboxamide, C18H15BrF2N4O
  34. The crystal structure of the host-guest complex: N-{5-[2-(2,6-dimethylphenoxy)acetamido]-4-hydroxy-1,6-diphenylhexan-2-yl}-3-methyl-2-(2-oxo-1,3-diazinan-1-yl)butanamide-diethyl ether (2/1)
  35. The crystal structure of (Z)-4-amino-N-(1-(4-hydroxyphenyl)propylidene)benzohydrazide, C16H17N3O2
  36. The crystal structure of diethyl 1,4-dihydro-2,6-dimethyl-4-(3-cyanophenyl)-3,5-pyridinedicarboxylate, C20H22N2O4
  37. Crystal structure of 3-(5-((4-(difluoromethoxy)phenyl) sulfonyl)-3,4,5,6-tetrahydropyrrolo[3,4-c]pyrrol-2(1H)-yl) oxetane-3-carboxamide, C17H19F2N3O5S
  38. Crystal structure of 2-((2,6-dichloro-4-(3,5-dimethylisoxazol-4-yl)phenyl)amino)-N-(2-(4-methylpiperazin-1-yl)ethyl)benzamide hydrate, C25H37Cl2N5O6
  39. Crystal structure of 3-(benzo[d]thiazol-2-yl)-5-bromo-2-hydroxybenzaldehyde, C14H8BrNO2S
  40. Crystal structure of 3-(difluoromethyl)-1-methyl-N-(pyridin-2-yl)-1H-pyrazole-4-carboxamide, C11H10F2N4O
  41. Crystal structure of 3-(2-ethoxy-2-oxoethyl)-1-isopropyl-1H-imidazol-3-ium hexafluoridophosphate(V), C20H34F12N4P2
  42. Crystal structure of ethyl 5,6-dichloro-2-methyl-2,3-dihydro-1 H-benzo[d]imidazole-2-carboxylate, C11H12Cl2N2O2
  43. The crystal of structure of (OC-6-22)-pentakis(acetonitrile)bromidoruthenium(II)bromide monohydrate, C10H15Br2N5Ru
  44. Crystal structure of (2S,3R,4S,5S,6R)-4,5-dihydroxy-6-(hydroxymethyl)-2-(((4aS,5R,6S)-1-oxo-5-vinyl-4,4a,5,6-tetrahydro-1H,3H-pyrano[3,4-c]pyran-6-yl)oxy)tetrahydro-2H-pyran-3-yl 2,3-dihydroxybenzoate hydrate, C23H26O12·H2O
  45. The crystal structure of (E)-4-amino-N′-(1-(4-fluorophenyl)propylidene)benzohydrazide, C16H16FN3O
  46. The crystal structure of 2′-(9H-carbazol-9-yl)-[1,1′-binaphthalen]-2-amine, C32H22N2
  47. Crystal structure of poly[μ3-diiodido-[μ2-di(1H-pyrazol-1-yl)methane-κ2N,N′)]dicopper(I)], C7H8Cu2I2N4
  48. Crystal structure of 3-amino-N′-hydroxy-1H-pyrazole-4-carboximidamide, C4H7N5O
  49. The crystal structure of 1,3-diacetyltetrahydroimidazo[4,5-d]imidazole-2,5(1H,3H)-dione, C8H10O4N4
  50. Crystal structure of catena-poly[aqua-(μ2-1,4-diazabicyclo[2.2.2]octane-k2N: N′)-bis(sorbato-κ1O)-copper(II), C18H28CuN2O5
  51. Crystal structure of catena-poly[triaqua-(μ2 -1-(4-carboxylatophenyl)-4-oxo-1,4-dihydropyridazine-3-carboxylato-κ3O,O′:O′′)manganese(II)], C12H12N2O8Mn
  52. The crystal structure of [hexaaquamagnesium(II)] 4-[(pyridine-4-carbonyl)-amino]-phthalate trihydrate, C14H26N2O14Mg
  53. Crystal structure of 1-(p-tolylphenyl)-4-(2-furoyl)-3-methyl-1H-pyrazol-5-ol, C16H14N2O3
  54. The crystal structure of bis(1,4,7,10,13-pentaoxacyclopentadecane)-potassium(I) dichloridocopper(I), C20H40Cl2CuKO10
  55. The crystal structure of tris(tetra-n-butylammonium) hexanitrato-κ2O,O′-lanthanium(III) C48H108N9O18La
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