Home Physical Sciences 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
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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

  • Yu-Hua Yang , Bao-Jun Wang , Peng-Fei Lan and Wen-Kui Dong EMAIL logo
Published/Copyright: September 16, 2017

Abstract

C44H49Cl2Co3N6O12, Triclinic, P1̅, a = 9.7415(9) Å, b = 13.6440(14) Å, c = 17.5241(11) Å, α = 72.807(10)°, β = 83.019(9)°, γ = 72.246(9)°, V = 2450.6(5) Å3, Z = 2, Rgt(F) = 0.0700, wRref(F2) = 0.1505, T = 291(2) K.

CCDC no.:: 1531177

The crystal structure is shown in the figure. 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 brown needle
size:0.13 × 0.08 × 0.07 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:1.18 mm−1
Diffractometer, scan mode:SuperNova ω
θmax, completeness:26.0°, 99.7%
N(hkl)measured, N(hkl)unique, Rint:19011, 9620, 0.079
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 4395
N(param)refined:657
Programs:CrysAlisPRO [17], SHELX [18]
Table 2

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

AtomxyzUiso*/UeqOcc. (<1)
Co10.16016(8)0.61281(8)0.36431(5)0.0527(3)
Co20.34145(7)0.48814(7)0.26741(4)0.0392(2)
Co30.45802(8)0.37486(7)0.15535(5)0.0413(2)
Cl10.4109(2)1.04789(18)0.12451(13)0.0951(8)
Cl20.4638(3)−0.10166(18)0.44141(13)0.1047(8)
O10.2676(4)0.6514(3)0.2774(2)0.0489(12)
O20.1254(6)0.7758(5)0.4501(3)0.0861(19)
O3−0.1255(5)0.7404(5)0.4059(3)0.101(2)
O40.1413(4)0.5000(3)0.3186(2)0.0499(12)
O50.4135(4)0.3265(3)0.2544(2)0.0425(11)
O60.6839(5)0.1871(4)0.1070(3)0.0646(14)
O70.4156(5)0.3001(4)0.0369(3)0.0620(14)
O80.2906(4)0.5068(3)0.1662(2)0.0479(12)
O90.2904(4)0.5092(4)0.4375(2)0.0638(14)
O100.4352(4)0.4300(3)0.3631(2)0.0496(12)
O110.5348(4)0.5157(3)0.2275(2)0.0481(12)
O120.6144(4)0.4447(4)0.1396(2)0.0521(13)
N10.1756(6)0.7499(5)0.3864(3)0.0660(19)
N2−0.0509(6)0.6431(5)0.3867(3)0.072(2)
N3−0.0438(7)0.2409(6)0.2753(4)0.082(2)
N40.5904(5)0.2185(4)0.1611(3)0.0482(15)
N50.3683(5)0.3869(5)0.0686(3)0.0494(15)
C10.3048(7)0.7385(6)0.2463(4)0.0510(19)
C20.3612(6)0.7543(6)0.1780(4)0.0519(18)
H20.37750.69970.15690.062*
C30.3929(7)0.8468(6)0.1413(4)0.0583(19)
H30.42700.85490.09570.070*
C40.3742(7)0.9287(6)0.1721(5)0.067(2)
C50.3233(8)0.9156(7)0.2389(5)0.072(2)
H50.31230.97020.25950.086*
C60.2872(7)0.8226(6)0.2773(4)0.057(2)
C70.2270(8)0.8223(6)0.3457(4)0.067(2)
H70.22550.87990.36170.081*
C80.0525(9)0.7033(8)0.4916(4)0.086(3)
H8A0.05900.70030.53950.103*
H8B0.10180.63270.48600.103*
C9−0.1008(9)0.7290(8)0.4766(5)0.107(4)
H9A−0.13970.67280.50620.128*
H9B−0.15310.79510.48800.128*
C9AA0.1834(6)0.5668(5)0.1257(3)0.0430(16)
C10−0.1402(7)0.5949(7)0.3764(4)0.074(3)
H10−0.23690.62220.38790.088*
C11−0.1056(7)0.5075(7)0.3499(4)0.061(2)
C12−0.2158(7)0.4602(8)0.3511(4)0.082(3)
H12−0.30670.49190.36770.098*
C13−0.1994(7)0.3719(8)0.3299(4)0.081(3)
H13−0.27420.34070.33570.098*
C14−0.0646(7)0.3280(7)0.2983(4)0.063(2)
C150.0467(6)0.3765(6)0.2934(4)0.0553(19)
H150.13350.35060.27100.066*
C160.0308(6)0.4611(6)0.3206(3)0.0513(18)
C170.0853(9)0.2006(7)0.2361(6)0.089(3)
H170.16330.14360.25520.107*
C180.0777(10)0.2601(9)0.1635(6)0.131(4)
H18A0.16080.22760.13860.196*
H18B0.07530.33270.15900.196*
H18C−0.00810.25940.14510.196*
C19−0.1507(9)0.1783(9)0.2901(6)0.116(4)
H19A−0.13320.13480.25810.139*
H19B−0.24710.22710.28300.139*
C20−0.1417(14)0.1049(12)0.3652(7)0.217(7)
H20A−0.15750.03850.36590.325*
H20B−0.21400.13970.39400.325*
H20C−0.04800.09110.38230.325*
C210.4297(6)0.2292(5)0.2963(4)0.0413(16)
C220.3649(6)0.2138(6)0.3622(4)0.0535(18)
H220.31320.27360.37690.064*
C230.3741(7)0.1141(6)0.4065(4)0.065(2)
H230.32850.10710.45000.079*
C240.4508(8)0.0259(6)0.3860(4)0.065(2)
C250.5206(7)0.0359(6)0.3233(4)0.058(2)
H250.5747−0.02560.31120.069*
C260.5142(6)0.1355(5)0.2763(4)0.0475(17)
C270.5921(6)0.1362(5)0.2118(4)0.0447(17)
H270.64930.07060.20630.054*
C280.6739(7)0.2752(6)0.0490(4)0.066(2)
H28A0.76430.26400.02240.079*
H28B0.66110.33840.06450.079*
C290.5525(8)0.2962(6)0.0024(4)0.078(3)
H29A0.54530.3638−0.03250.094*
H29B0.57640.2405−0.02130.094*
C300.2535(7)0.4558(6)0.0406(4)0.0522(19)
H300.22510.44670.00110.063*
C310.1654(6)0.5447(5)0.0637(3)0.0428(16)
C320.0497(6)0.6137(6)0.0216(3)0.0518(18)
H320.03610.5986−0.01850.062*
C33−0.0419(6)0.7007(6)0.0376(4)0.062(2)
H33−0.11470.74540.00760.074*
C34−0.0284(6)0.7244(6)0.0989(4)0.059(2)
C390.4005(6)0.4409(5)0.4222(4)0.0475(18)
C400.4973(7)0.3681(5)0.4801(3)0.063(2)
H40A0.56980.31440.46350.095*
H40B0.44120.33440.51700.095*
H40C0.54280.40910.49670.095*
C410.6193(6)0.5024(5)0.1779(3)0.0446(16)
C420.7381(6)0.5567(6)0.1616(4)0.058(2)
H42A0.70070.62950.13480.087*
H42B0.81480.51950.13570.087*
H42C0.77430.55560.20380.087*
C520.0850(6)0.6562(5)0.1415(4)0.0507(18)
H520.09540.67110.18220.061*
N6−0.1392(16)0.7951(13)0.1280(9)0.055(5)0.50
C35−0.082(2)0.8600(16)0.1661(10)0.070(5)0.50
H35A0.02200.83690.17060.084*0.50
H35B−0.11710.93710.14800.084*0.50
C36−0.167(3)0.813(2)0.2319(12)0.136(11)0.50
H36A−0.26400.85770.23160.204*0.50
H36B−0.12090.80830.27230.204*0.50
H36C−0.16750.74220.23220.204*0.50
C37−0.251(2)0.8669(18)0.0837(12)0.077(7)0.50
H37A−0.32970.89860.11190.093*0.50
H37B−0.28670.82580.06160.093*0.50
C38−0.210(3)0.958(3)0.0268(15)0.110(9)0.50
H38A−0.16310.9317−0.01150.165*0.50
H38B−0.14610.98440.04490.165*0.50
H38C−0.29581.01520.01150.165*0.50
N6′−0.1045(16)0.8246(13)0.1070(9)0.055(5)0.50
C35′−0.139(2)0.812(2)0.1943(13)0.078(6)0.50
H35C−0.24120.83590.20530.093*0.50
H35D−0.09940.73860.22180.093*0.50
C36′−0.061(2)0.8835(16)0.2029(14)0.105(8)0.50
H36D0.03570.86410.18410.157*0.50
H36E−0.05820.87750.25110.157*0.50
H36F−0.10950.95590.17900.157*0.50
C37′−0.220(3)0.899(2)0.0632(13)0.074(7)0.50
H37C−0.29100.94220.08900.089*0.50
H37D−0.26820.86140.04410.089*0.50
C38′−0.145(3)0.969(3)0.0056(14)0.133(11)0.50
H38D−0.21571.0202−0.02640.200*0.50
H38E−0.07380.9250−0.01830.200*0.50
H38F−0.10021.00690.02550.200*0.50

Source of material

A methanol solution (3.0 mL) of cobalt acetate tetrahydrate (370.6 mg 0.015 mmol) was added to a acetone solution (2.0 mL) of H2L 4-(diethylamino)-2-hydroxybenzaldehyde O-(2-(((5-chloro-2-hydroxybenzylidene)amino)oxy)ethyl) oxime (4.01 mg, 0.010 mmol) at room temperature, the color of the mixing solution turned brown immediately. After the mixture was stirred for 1 h, the mixture was filtered. The resulting filtrate was left undisturbed for about one week to form clear light brown block crystals. Yield: 78.5%. Elemental analysis-Anal. Calcd. for C44H49Cl2Co3N6O12: C, 47.97%; H, 4.48%; N, 7.63%. Found: C, 48.25%; H, 4.32%; N, 7.50%.

Experimental details

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

Discussion

Salen and its derivatives are a very important versatile ligand in coordination chemistry as a kind of multidentate ligands [1], [2], [3], [4], and their metal complexes [5], [6], [7] have a very wide range of applications, such as optical and magnetic materials [8], [9], [10], [11], biological activities [12], supramolecular architectures [13], [14], [15].

The crystal structure shows that the title complex consists of three Co(II) atoms, two (L)2− units and two acetate ions. The coordination sphere of terminal Co1 or Co3 atom is completed by N2O2 donors of (L)2− unit and one oxygen atom of acetate. The sphere of central Co2 was completed by four phenolate oxygen atoms and two oxygen atoms of acetate ions, thus, constitute three octahedral geometries around three hexa-coordinated cobalt atoms, respectively. The two acetate ions coordinate to the three Co(II) atoms. The carbon, nitrogen and hydrogen atoms of one of the N,N′-diethylamine groups are disordered over two different positions (cf. Table 2). This disorder is similar to that for previously reported Salamo-type Ni complex [18].

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Received: 2017-3-16
Accepted: 2017-8-29
Published Online: 2017-9-16
Published in Print: 2017-11-27

©2017 Yu-Hua Yang et al., published by De Gruyter, Berlin/Boston

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

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  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
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