Startseite Naturwissenschaften Crystal structure of bis{5-(N,N′-diethylamine)-5′-methoxy -2,2′-[ethylenediyldioxybis(nitrilomethylidyne)]diphenolato}-bis(μ2-acetato-κ2O:O′)trizinc(II), C46H56Zn3N6O14
Artikel Open Access

Crystal structure of bis{5-(N,N′-diethylamine)-5′-methoxy -2,2′-[ethylenediyldioxybis(nitrilomethylidyne)]diphenolato}-bis(μ2-acetato-κ2O:O′)trizinc(II), C46H56Zn3N6O14

  • Xiu-Yan Dong EMAIL logo , Han Zhang , Bai-Jun Wang , Peng-Fei Lan und Wen-Kui Dong
Veröffentlicht/Copyright: 16. September 2017

Abstract

C46H56Zn3N6O14, monoclinic, C2/c (no. 15), a = 10.6703(7) Å, b = 27.091(4) Å, c = 17.9132(16) Å, β = 96.246(8)°, V = 5147.4(10) Å3, Z = 4, Rgt(F) = 0.0647, wRref(F2) = 0.1865, T = 291(1) K.

CCDC no.:: 1531178

The crystal structure of the title complex is shown in the figure (′ = 1 − x, y, 0.5 − z). Tables 1 and 2 contain details on crystal structure and measurement conditions and a list of the atoms including atomic coordinates and displacement parameters.

Table 1

Data collection and handling.

Crystal:clear light colourless block
Size:0.28 × 0.17 × 0.16 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:1.45 mm−1
Diffractometer, scan mode:SuperNova Dual Eos, ω
θmax, completeness:26.0°, 99.7%
N(hkl)measured, N(hkl)unique, Rint:10608, 5060, 0.062
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 2787
N(param)refined:316
Programs:CrysAlisPRO [18], SHELXS, SHELXL [19]
Table 2

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

AtomxyzUiso*/Ueq
Zn10.26347(6)0.59405(3)0.32454(4)0.0471(3)
Zn20.50000.57518(4)0.25000.0430(3)
O10.8214(4)0.5690(2)0.5166(3)0.0753(16)
O20.4419(3)0.57849(16)0.3607(2)0.0470(11)
O30.0921(4)0.5647(2)0.4497(3)0.0708(15)
O40.0765(4)0.66252(19)0.3861(3)0.0718(15)
O50.3457(3)0.62540(15)0.2373(2)0.0459(11)
O60.1932(4)0.53602(17)0.2682(3)0.0578(12)
O70.3725(4)0.51796(16)0.2204(2)0.0545(12)
N10.2172(4)0.5713(2)0.4320(3)0.0544(15)
N20.1549(5)0.6555(2)0.3260(3)0.0584(16)
N30.4969(7)0.7486(2)0.0790(4)0.097(3)
C10.4994(5)0.5716(2)0.4295(3)0.0432(15)
C20.6290(5)0.5732(2)0.4423(3)0.0478(16)
H20.67520.57920.40210.057*
C30.6922(6)0.5661(3)0.5124(4)0.0537(18)
C40.6266(6)0.5558(3)0.5729(4)0.062(2)
H40.66860.55050.62050.074*
C50.4983(6)0.5536(3)0.5606(4)0.0582(19)
H50.45360.54630.60100.070*
C60.4315(5)0.5617(2)0.4913(4)0.0486(16)
C70.8915(6)0.5613(4)0.5877(4)0.090(3)
H7A0.97990.56180.58210.135*
H7B0.86940.52980.60730.135*
H7C0.87250.58690.62160.135*
C80.2954(6)0.5610(3)0.4876(4)0.0566(19)
H80.26180.55180.53130.068*
C90.0069(6)0.5758(3)0.3870(4)0.0572(19)
H9A−0.06910.55660.38980.069*
H9B0.04350.56550.34220.069*
C10−0.0281(6)0.6280(3)0.3790(4)0.073(2)
H10A−0.07570.63270.33020.087*
H10B−0.08350.63600.41680.087*
C110.1762(6)0.6971(3)0.2967(4)0.066(2)
H110.13150.72390.31230.079*
C120.2613(7)0.7069(3)0.2422(4)0.065(2)
C130.3409(5)0.6715(2)0.2130(4)0.0481(16)
C140.4167(6)0.6865(2)0.1581(4)0.0534(17)
H140.46840.66320.13870.064*
C150.4185(7)0.7343(3)0.1313(5)0.076(2)
C160.3410(9)0.7699(3)0.1609(6)0.111(4)
H160.34210.80260.14540.133*
C170.2648(8)0.7551(3)0.2127(6)0.101(3)
H170.21110.77840.23000.121*
C180.5097(12)0.7985(4)0.0545(8)0.144(6)
H18A0.42930.81520.05450.173*
H18B0.53150.79830.00330.173*
C190.6090(13)0.8272(4)0.1034(10)0.195(9)
H19A0.61570.85990.08350.292*
H19B0.68880.81070.10420.292*
H19C0.58550.82920.15360.292*
C200.5733(10)0.7132(4)0.0432(7)0.115(4)
H20A0.65210.72850.03340.138*
H20B0.59260.68520.07630.138*
C210.5059(14)0.6971(5)−0.0255(8)0.181(6)
H21A0.55830.6753−0.05100.272*
H21B0.48300.7251−0.05680.272*
H21C0.43110.6798−0.01510.272*
C220.2622(6)0.5089(3)0.2325(4)0.0540(17)
C230.2031(7)0.4612(3)0.2010(5)0.082(3)
H23A0.17710.46520.14830.122*
H23B0.13110.45330.22650.122*
H23C0.26370.43500.20810.122*

Source of material

A methanol solution (3.0 mL) of zinc(II) acetate (3.29 mg 0.015 mmol) was added to a chloroform solution (2.0 mL) of H2L (5-(N,N′-diethylamine)-5′-methoxy-2,2′-[ethylenediyldioxybis(nitrilomethylidyne)] diphenol) (3.91 mg, 0.010 mmol) at room temperature. After the mixture was stirred for 1 h the mixture was filtered off. The resulting filtrate was left undisturbed for about one week to form prismatic crystals suitable for X-ray crystallographic analysis. Yield: 37.8%. Elemental analysis – Anal. Calcd. for C46H56Zn3N6O14: C, 49.63%; H, 5.07%; N, 7.55%. Found: C, 49.77%; H, 5.01%; N, 7.35%.

Experimental details

Hydrogen atoms were placed in their geometrically idealized positions and constrained to ride on their parent atoms.

Discussion

Salen-like compounds are important N2O2 chelating ligands in inorganic chemistry [1], [2], [3], [4], [5]. They are able to form different types of metal complexes [6], [7], [8], [9]. These compounds can be applied to the biological system [10], used as luminescence materials [11], [12], [13] and supramolecular building units [14], [15], [16], [17].

The title compound consists of three Zn(II), two completely deprotonated (L)2− units and two acetate ligands, to form the trinuclear complex (see the figure). The coordination sphere of terminal Zn(II) atom is completed by N2O2 donors of (L)2− unit and one oxygen atom of the acetate ligand. The sphere of central Zn(II) atom was completed by four phenolic oxygen atoms which have been deprotonated in two [Zn(L)] chelates and two oxygen atoms of the acetate ligands, thus, constitute three octahedral geometries around three hexa-coordinated Zn(II) atoms, respectively. The two acetate ions coordinate to the three Zn(II) atoms via a μ22O:O′ mode.

References

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Received: 2017-3-21
Accepted: 2017-8-15
Published Online: 2017-9-16
Published in Print: 2017-11-27

©2017 Xiu-Yan Dong et al., published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 License.

Artikel in diesem Heft

  1. Cover and Frontmatter
  2. Crystal structure of potassium 1-methyl-1H-1,2,3,4-tetrazole-5-thiolate, C2H3N4SK
  3. Crystal structure of bis(3-(3-ethylureido)-N,N-dimethylpropan-1-aminium) bis (μ3-2-(hydroxymethyl)-2-(oxidomethyl)propane-1,3-bis(olato))-(μ6-oxo)-hexakis(μ2-oxo)-hexaoxo-hexavanadium(V) – dichloromethane (1/1), C27H60Cl2N6O23V6
  4. Crystal structure of bis(μ3-methanolato-κ3O:O:O)-bis(μ2-methanolato-κ2O:O)-dimethanol-bis{6,6′-(1,3-dihydroxyl-2-acetylpropane-1,3-diyl)bis(2-chloro-4-bromophenolato)}tetramanganese(III) C40H40Br4Cl4Mn4O16
  5. Synthesis and crystal structure of tetrakis(μ2-methanolato)-dimethanol-bis(μ2-2-acetyl-1,3-bis(3,5-dibromo-2-oxidophenyl)propane-1,3-bis(olato)-κ5O1,O2,O3:O3,O4,O5)tetramanganese(III), C40H40Br8Mn4O16
  6. Synthesis and crystal structure tetrakis(μ2-methanolato)-dimethanol-bis(μ2-2-acetyl-1,3-bis(3,5-dichloro-2-oxidophenyl)propane-1,3-bis(olato)-κ5O1,O2,O3:O3,O4,O5), tetramanganese(III), C40H40Cl8Mn4O16
  7. Crystal structure of bis{5-methoxy-2-((E)-((4-((E)-1-(methoxyimino)ethyl)phenyl)imino)methyl)phenolato-κ2N,O)}copper(II), C34H34CuN4O6
  8. Crystal structure of (E)-1-(2-hydroxy-3-{[2-hydroxybenzylidene]amino}phenyl)ethan-1-one, C15H13NO3
  9. Crystal structure of bis(μ2-acetato-κ2O:O′)-bis{μ2-4-chloro-2-(8-(4-(diethylamino)-2-oxidophenyl)-3,6-dioxa-2,7-diazaocta-1,7-dien-1-yl)phenolato-κ6O:O,N,N′,O′′:O′′}tricobalt(II), C44H49Cl2Co3N6O12
  10. Crystal structure of bis{μ2-2,4-dichloro-6-(8-(4-(diethylamino)-2-oxidophenyl)-3,6-dioxa-2,7-diazaocta-1,7-dien-1-yl)phenolato-κ5O:O,N,N′,O′}dicobalt(II) acetone solvate, C43H48Br4Co2N6O9
  11. Synthesis and crystal structure of bis(μ2-acetato-κ2O:O′)-bis{μ2-4-chloro-2-(8-(4-(diethylamino)-2-oxidophenyl)-3,6-dioxa-2,7-diazaocta-1,7-dien-1-yl)phenolato-κ6O:O,N,N′,O′:O′}trizinc(II), C44H49Cl2N6O12Zn3
  12. Crystal structure of bis{5-(N,N′-diethylamine)-5′-methoxy -2,2′-[ethylenediyldioxybis(nitrilomethylidyne)]diphenolato}-bis(μ2-acetato-κ2O:O′)trizinc(II), C46H56Zn3N6O14
  13. Crystal structure of tris(cyano-(hydrogen tris(3,5-dimethylpyrazolyl)borate))-iron(III) 4-methoxypyridinium monohydrate, C24H32BN10O2Fe
  14. Synthesis and crystal structure of bis{1-(((4-(1-(hydroxyimino)ethyl)phenyl)imino)methyl)naphthalen-2-olato-κ2O,N}copper(II), C38H30CuN4O4
  15. Crystal structure of (E)-1-(4-{[(E)-2-Hydroxy-1-naphthalenylmethylene] amino}phenyl)ethanone oxime, C19H16N2O2
  16. The pseudosymmetric crystal structure of 2-(2-naphthalenyl)-3-nitro-2H-1-benzopyran, C38H26N2O6
  17. Crystal structure of 2-benzoyl-3-(4-methoxyphenyl)cyclopropane-1,1-dicarbonitrile, C19H14N2O2
  18. N′-(5-ethoxycarbonyl-3,4-dimethyl-pyrrol-2-yl-methylidene)-4-hydroxybenzohydrazide monohydrate, C17H21N3O5
  19. The crystal structure of carbonyl-[4-(2,4-dichlorophenylamino)pent-3-en-2-onato-κ2N,O]-(triphenylphosphine-κP)rhodium(I), RhC30H25Cl2NO2P
  20. Crystal structure of (E)-5-(diethylamino)-2-(((1,1,2-trihydroxyethyl)iminio)methyl)phenolate, C15H24N2O4
  21. Crystal structure of poly[(μ2-1,4-bis((2-ethyl-1H-benzo[d]imidazol-1-yl)methyl)benzene-κ2N:N′)(μ2-isophthalato-κ4O,O′:O′′,O′′′)cadmium(II)], C34H30N4O4Cd
  22. Crystal structure of 5,6-Dihydro-9,10-dimethoxybenzo[g]-1,3-benzodioxolo[5,6-a]chinolizinium 3-(4-hydroxyphenyl)-4-oxo-4H-chromen-7-olate - methanol - water (1/1/1), C36H33NO10
  23. A single crystal study on 2-(methylcarbamoyl)benzoic acid, C9H9NO3
  24. Crystal structure of the salt 1,1′-(ethane-1,2-diyl)bis(1,4-diazabicyclo[2.2.2]octan-1-ium) diperchlorate, C14H28N4(ClO4)2
  25. Crystal structure of 2,5-bis((E)-2-(trifluoromethyl)benzylidene)cyclopentan-1-one, C21H14F6O
  26. Crystal structure of catena-poly[(μ2-benzene-1,4-dicarboxylato-κ2O:O′)-(1-ethyl-6-fluoro-7-(4-methylpiperazin-1-ium-1-yl)-4-oxo-1,4-dihydroquinoline-3-carboxylato-κ2O,O′)zinc(II)] 1.25 hydrate, C25H26.5N3O8.25FZn
  27. Crystal structure of 1-methyl-1,4-diazabicyclo[2.2.2]octan-1-ium poly[aqua-bis(μ2-perchlorato-κ3O,O′:O′′)sodium], C7H17Cl2N2NaO9
  28. Crystal structure of trimethyammonium 2,6-dicarboxyisonicotinate monohydrate, C11H16N2O7
  29. Crystal structure of dodecaguanidinium bis(tetrapropylammonium) heptacarbonate, C43H128N38O21
  30. Crystal structure of poly[tetraaqua-bis(μ6-benzene-1,2,4,5-tetracarboxylato)nickel(II)diyttrium(III)]dihydrate, C20H16NiO22Y2
  31. Halogen bonds and π–π interactions in the crystal structure of 1,3,5-trifluoro-2,4,6-triiodobenzene–N,N-dimethylformamide (1/1), C9H7F3I3NO
  32. Crystal structure of guanidinium tetraethylammonium carbonate dihydrate, C10H30N4O5
  33. The crystal structure of oxonium chlorido-ethylenediaminetetraactetotin(IV) hydrate, C10H17ClN2O10Sn
  34. Crystal structure of 8-((E)-((4-((E)-1-((benzyloxy)imino)ethyl)phenyl)imino)methyl)-7-hydroxy-4-methyl-2H-chromen-2-one, C26H22N2O4
  35. Crystal structure of bis{5-(diethylamino)-2-(((2-oxo-2H-chromen-6-yl)imino)methyl)phenolato-κ2O,N}copper(II), C40H38CuN4O6
  36. Crystal structure of fac-(acetylacetonato-κ2O,O′)tricarbonyl(tri(p-tolyl)phosphine-κP)rhenium(I), C29H28O5PRe
  37. Crystal structure of fac-(acetylacetonato-κ2O,O′)tricarbonyl(benzyldiphenylphosphine-κP)rhenium(I), C27H24O5PRe
  38. Crystal structure of triethylammonium bis{3-(((3-oxidonaphthalen-1-yl)methylene)amino)-2-oxo-2H-chromen-4-olato-κ3O,N,O′}manganese(III), C46H38MnN3O8
  39. Crystal structure of bis(N,N,N-ethyldimethylethanaminium) bis(heptaselenido-κ2Se1,Se7)palladate(II), C12H32N2PdSe14
  40. Crystal structure of bis(4-(1H-pyrazol-5-yl)pyridine-κ2N:N′)-bis(2-(2-((2,6-difluorophenyl)amino)phenyl)acetate-κO)cadmium(II), C44H34N8CdCl4O4
  41. Crystal structure of 4,4′-(1,4-phenylene)bis(pyridin-1-ium) catena-poly[diaqua-bis(μ2-3′,5′-dicarboxy-[1,1′-biphenyl]-2,5-dicarboxylato-κ2O:O′] dihydrate, C48H42O22N2Ca
  42. The crystal structure of (S)-2-benzylsuccinic acid, C11H12O4
  43. Crystal structure of poly[aqua-(μ3-4-(pyridin-4-yl)isophthalato-κ4O,O′:O′′:O′′′)-(μ2-5-carboxy-2-(pyridin-4-yl)benzoato-κ2O:O′)yttrium(III)], C26H17N2O9Y
  44. Crystal structure of ethyl 1-(3,4-dimethylphenyl)-5-methyl-1H-1,2,3-triazole-4-carboxylate, C14H17N3O2
  45. Crystal structure of tetrakis(methanol-κO)-bis{μ2-3-((4-methoxy-2-oxidobenzylidene)amino)-2-oxo-2H-chromen-4-olate-κ4O,N;O′:O′}dizinc(II), C38H38Zn2N2O14
  46. Crystal structure of bromido(4,4′-dimethoxy-2,2′-bipyridine-κ2N,N′)(isopropyl(diphenyl)phosphane-κP)copper(I), C27H29BrCuN2O2P
  47. Crystal structure of bis(4,4,5,5-tetramethyl-1,3,2-dioxaborolane)-9,9-dioctylfluorene, C41H64B2O4
  48. Crystal structure of 11-oxo-2,3,6,7-tetrahydro-1H,5H,11H-pyrano[2,3-f]pyrido[3,2,1-ij]quinoline-10-carbaldehyde - a julolidine derivative, C16H15NO3
  49. Crystal structure of 1,3-dimethyl-5,5-dibenzylbarbituric acid, C20H20N2O3
  50. Crystal structure of bis(N,N,N-trimethylethanaminium) poly[bis(μ2-heptaselenido-κ2Se1,Se7)palladate(II)], C10H28N2PdSe14
  51. Crystal structure of 1-{4-[(5-Chloro-2-hydroxy-benzylidene)amino]phenyl} ethanone O-ethyl-oxime, C17H17ClN2O2
  52. The crystal structure of methyl N-(4-bromophenyl)carbamate, C8H8BrNO2
  53. Synthesis and crystal structure of 1-{4-[(2-hydroxy-benzylidene)amino]phenyl}ethanone oxime, C15H14N2O2
  54. Crystal structure of 1,1′-butanebis(3-methyl-1H-imidazol-3-ium)bis(hexafluorophosphate), C12H20F12N4P2
  55. (E)-N-benzylidene-3-(benzylthio)-5-p-tolyl-4H-1,2,4-triazol-4-amine, C23H20N4S
  56. Crystal structure of ethyl 5-methyl-1-(pyridin-3-yl)-1H-1,2,3-triazole-4-carboxylate, C11H12N4O2
  57. Crystal structure of 5,5-difluoro-10-(4-fluorophenyl)-1,3,7,9-tetramethyl-5H-4l4,5l4-dipyrrolo[1,2-c:2′,1′-f][1,3,2]diazaborinine - a Z′ = 3 structure, C19H18B2F3N2
  58. The crystal structure of the Matrine derivative: 12-(1H-indol-1-yl)dodecahydro-1H,5H,10H-dipyrido[2,1-f:3′,2′,1′-ij][1,6]naphthyridin-10-one hydrate, C23H29N3O
  59. The crystal structure of tris(μ2-1,3-bis(4,4,4-trifluoro-3-oxido-1-(oxo)but-2-en-1-yl)phenyl-κ4O,O′:O′′,O′′′)-bis(1,2-dimethoxyethane-κ2O,O′)dilutetium(III), C50H38F18Lu2O16
  60. The crystal structure of (Z)-2-(3-(2-(4-chlorobenzoyl)hydrazono)-2-oxoindolin-1-yl) acetic acid, C17H12ClN3O4
  61. Synthesis and crystal structure of trans-tetraqua-bis(2-(((7-hydroxy-3-(4-hydroxy-3-sulfonatophenyl)-4-oxo-4H-chromen-8-yl)methyl)ammonio)acetato-κO)cobalt(II) hexahydrate, C36H48CoN2O28S2
  62. The crystal structure of N,N-dimethyl-2,6-di-p-tolylpyrimidin-4-amine, C20H21N3
  63. The crystal structure (E)-4-methyl-N′-(2-nitrobenzylidene)benzenesulfonohydrazide, C14H13N3O4S
  64. Crystal structure of catena-poly[(μ2-1,3-bis(benzimidazol-1-yl)propane κ2N:N′)-(μ2-5-methoxyisophthalato-κ2O:O′)zinc(II)] hydrate, C26H24ZnN4O6
  65. The crystal structure of (E)-N′-(quinolin-2-ylmethylene)furan-2-carbohydrazide monohydrate, C15H13N3O3
  66. Crystal structure of 2,8-diphenyl-3,7,9-trioxa-1-azaspiro[4.5]dec-1-ene, C18H17N1O3
  67. Crystal structure of diethyl 2-(4-chlorophenyl)-1,3-dioxane-5,5-dicarboxylate, C16H19ClO6
  68. Crystal structure of 1-(carboxymethyl)-1H-benzo[d][1,2,3]triazole 3-oxide, C8H7N3O3
  69. Crystal structure of (acetylacetonato-κ2O,O′)-(2-amino-6-chlorobenzoato-κO)-oxido(1,10-phenanthroline-κ2N,N′)vanadium(IV) – trichloromethane (1/1)
  70. Crystal structure of (1E,4E)-1,5-bis(4-chlorophenyl)penta-1,4-dien-3-one, C17H12Cl2O
  71. The crystal structure of trans-dibromido-bis(pyridine-κN)platinum(II), C10H10Br2N2Pt
Heruntergeladen am 25.1.2026 von https://www.degruyterbrill.com/document/doi/10.1515/ncrs-2017-0038/html
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