Startseite Crystal structure of poly[aqua-bis(nitrato-κ2O,O′)-(μ3-1,3-benzimidazol-3-ium-1,3-diacetato-κ4O,O′:O′′:O′′′)dysprosium(III)], C11H11DyN4O11
Artikel Open Access

Crystal structure of poly[aqua-bis(nitrato-κ2O,O′)-(μ3-1,3-benzimidazol-3-ium-1,3-diacetato-κ4O,O′:O′′:O′′′)dysprosium(III)], C11H11DyN4O11

  • Qian Zhang EMAIL logo , Yue Li und Qiong-Yan Yu
Veröffentlicht/Copyright: 13. Mai 2017

Abstract

C11H11DyN4O11, monoclinic, P21/c (no. 14), a = 12.073(4) Å, b = 14.704(4) Å, c = 8.763(3) Å, β = 94.233(5)°, V = 1551.3(8) Å3, Z = 4, Rgt(F) = 0.0201, wRref(F2) = 0.0555, T = 293 K.

CCDC no.:: 1543469

The asymmetric unit of the title crystal structure is shown in the figure. Tables 1 and 2 contain details of the measurement method and a list of the atoms including atomic coordinates and displacement parameters.

Table 1

Data collection and handling.

Crystal:Colourless block
Size:0.18 × 0.18 × 0.12 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:48.9 cm−1
Diffractometer, scan mode:Bruker P4, ω scans
2θmax, completeness:54°, >99%
N(hkl)measured, N(hkl)unique, Rint:9235, 3379, 0.018
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 2994
N(param)refined:244
Programs:Bruker programs [1], SHELX [2]
Table 2

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

AtomxyzUiso*/Ueq
Dy10.827724(10)0.622154(7)0.153115(12)0.01925(6)
O11.03690(16)0.30317(13)−0.3104(2)0.0297(4)
O21.07952(17)0.19565(14)−0.4752(2)0.0348(5)
O30.78840(16)0.49057(12)−0.0147(2)0.0259(4)
O40.71253(19)0.62053(11)−0.0928(2)0.0271(4)
O51.0187(3)0.4143(2)0.3482(3)0.0701(9)
O60.86727(19)0.49409(15)0.3255(2)0.0385(5)
O70.99773(19)0.52234(14)0.1794(2)0.0386(5)
O80.64434(17)0.56117(13)0.2082(2)0.0293(4)
O90.56479(18)0.57656(16)0.4217(2)0.0405(5)
O100.7271(2)0.63656(14)0.3932(2)0.0333(5)
N10.7357(2)0.40731(15)−0.2986(2)0.0240(5)
N20.81350(19)0.28621(15)−0.3867(3)0.0254(5)
N30.9632(2)0.47502(17)0.2852(3)0.0355(6)
N40.6424(2)0.59069(17)0.3431(3)0.0268(5)
C10.8143(2)0.37567(17)−0.3810(3)0.0248(6)
H1A0.86410.4121−0.42930.030*
C20.6788(2)0.33277(17)−0.2420(3)0.0223(5)
C30.5908(2)0.3274(2)−0.1509(3)0.0314(6)
H3A0.55850.3793−0.11270.038*
C40.5530(3)0.2416(2)−0.1193(4)0.0391(7)
H4A0.49390.2352−0.05780.047*
C50.6016(3)0.1640(2)−0.1776(4)0.0383(7)
H5A0.57350.1072−0.15390.046*
C60.6898(2)0.16848(18)−0.2689(3)0.0299(6)
H6A0.72130.1165−0.30790.036*
C70.7289(2)0.25542(17)−0.2995(3)0.0228(5)
C80.8921(2)0.2306(2)−0.4662(3)0.0312(6)
H8A0.88310.2443−0.57470.037*
H8B0.87360.1670−0.45340.037*
C91.0131(2)0.24475(17)−0.4109(3)0.0225(5)
C100.7089(3)0.50271(17)−0.2752(3)0.0305(7)
H10A0.62980.5110−0.29890.037*
H10B0.74710.5390−0.34730.037*
C110.7386(2)0.53891(17)−0.1157(3)0.0227(5)
O1W0.73540(18)0.76199(12)0.1590(2)0.0304(4)
H1WB0.72780.79500.07770.037*
H1WA0.73480.79640.24100.037*

Source of material

1-(Carboxymethyl)-1H-benzimidazol-3-ium-3-acetate was prepared according to the reported procedures [3]. Sodium carbonate (0.25 mmol) was added to 1-(carboxymethyl)-1H-benzimidazol-3-ium-3-acetate (0.5 mmol) in distilled water (5 mL) while stirring at room temperature. Once the solution became clear, dysprosium nitrate (0.25 mmol) dissolved in distilled water (5 mL) was added dropwise. After continuous stirring for 15 min, the resulting solution was filtered and placed undisturbed for 2 weeks. Colourless crystals suitable for crystal structure analysis were obtained.

Experimental details

Hydrogen atoms bound to carbon were placed in geometrically idealized positions and refined isotropic using riding model with Uiso(H) = 1.2Ueq(C). The hydrogens bound to coordinated water molecules were located in difference Fourier map and refined with Uiso(H) = 1.2Ueq(O).

Comment

In the recent years, the benzimidazole derivatives and their metal complexes have attracted much attention because of the specific topological frameworks and intresting properties of materials [4], [5], [6], [7]. Furthermore, benzimidazole carboxylic acids and their derivatives are widely used due to their biological activites such as antifilarial, antineoplastic, anthelmintic and antiviral activities [8], [9], [10], [11]. Up to now, several complexes have been built by benzimidazole carboxylic acid [12], [13], [14], [15], [16], [17]. To extend this work, a crystal structure of a related samarium complex was reported by us [18].

The asymmetric unit of the title structures consists of one Dy3+ cation, one 1-(carboxymethyl)-1,3-benzimidazol-3-ium-3-acetate ligand, two nitrate ions and one water molecule. The Dy atom is nine-coordinated showing a distorted, tricapped trigonal prism. The coordination sphere is composed of nine oxygen atoms from a chelating carboxylate group, two monodentate coordinating carboxylate groups, two chelating nitrato ligands, and one coordinated water molecule. The sets of atoms O1w, O8, O10 and O2i (i = x + 2, y + 1/2, −z − 1/2), O3, O7 define the triangular base and upperface, respectively, and O1ii (ii = −x + 2, −y + 1, −z), O4, O6 achieve the cappings of the polyhedron. The Dy—O bond lengths range from 2.3333(19) Å to 2.2608(18) Å. Meanwhile, the two carboxylate groups of one ligand take a μ3-coordination mode bridging three Dy3+ ions to form a two dimensional undulating sheet structure.

Furthermore, there are neither obvious π–π stacking interactions, nor hydrogen bonds existing between the adjacent sheets. Therefore, the packing seems to be dominated by van der Waals forces. To simplify the structure of the two dimensional framework, the Dy atom and the ligand both can be viewed as 3-connected node, therefore the topology of the resulting structure may be described as fes topology with a point symbol of (4.82) [19].

Acknowledgement

This work was supported by the Doctor Foundation of Henan institue of Engineering (No. D2012030).

References

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Received: 2016-11-28
Accepted: 2017-4-17
Published Online: 2017-5-13
Published in Print: 2017-7-26

©2017 Qian Zhang et al., published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

Artikel in diesem Heft

  1. Cover and Frontmatter
  2. Crystal structure of poly[diaqua-(μ2-4,4′-bipyridine-κ2N:N′)manganese(II)] bis(4-chlorobenzenesulfonate) – 4,4′-bipyridine – water (1/1/2) C42H40Cl2MnN6O10S2
  3. The crystal structure of 1,2-bis[2-methyl-5-(3-cyanophenyl)-3-thienyl]-3,3,4,4,5,5-hexafluoro-cyclopent-1-ene, C29H16F6N2S2
  4. Crystal structure of the first characterized polymeric copper and sodium complex diaqua-(tris-acetato-κO,O′)(μ2-acetato-κO′′)dinatrium copper(II) monohydrate, C8H18CuNa2O11
  5. The crystal structure of the Schiff base (E)-2,6-diisopropyl-N-(pyridin-3-yl-methylene)aniline, C18H22N2
  6. Crystal structure of methyl 2,7,7-trimethyl-4-(4-nitrophenyl)-5-oxo-1,4,5,6,7,8-hexahydro-quinoline-3-carboxylate, C20H22N2O5
  7. Crystal structure of bis(1,3-bis(diphenylphosphino)propane-κ2P,P′)silver(I) trifluorosulfonate–methanol (1:0.5), [Ag(C27H26P2)]SO3CF3⋅0.5CH3OH
  8. Crystal structure of μ-1,4-bis(diphenylphosphine)butane-2,9-dimethyl-1,10-phenanthroline-κ2N:N′-bis(cyano-κC)dicopper(I)]-water, C58H56Cu2N6O2P2
  9. Crystal structure of N2,N6-bis(1-hydrazinyl-2-methyl-1-oxopropan-2-yl) pyridine-2,6-dicarboxamide, C15H23N7O4
  10. Crystal structure of 1,3-dimethyl-2-phenyl-1H-perimidin-3-ium iodide, C19H17IN2
  11. Crystal structure of diaqua-(2,2′-(butane-1,4-diyl)-bis(5-carboxy-1H-imidazole-4-carboxylato)-κ4O,O′,N,N′)cadmium(II) monohydrate, C14H18O11N4Cd
  12. Crystal structure of ethyl (E)-3-(cyclopropylamino)-2-(2,4-dichloro-5-fluorobenzoyl) acrylate, C15H14Cl2FNO3
  13. Crystal structure of bis-(1-(4-chlorophenyl)-3-phenyl-4-thenoyl-1H-pyrazol-5-ol-κ2O,O′)-(N,N-dimethylformamide)zinc(II), C43H31Cl2N5O5S2Zn
  14. Crystal structure of tetrakis(μ3-2-(N-(2-hydroxyethyl)amino)ethoxo)-tetrachloro-tetra-cobalt(II) methanol solvate, C17H44Cl4Co4N4O9
  15. Crystal structure of 3-amino-1-(4-bromophenyl)-9-methoxy-1H-benzo[f]chromene-2-carbonitrile, C21H15BrN2O2
  16. Crystal structure of 2-amino-4-(4-isopropyl-phenyl)-3-cyano-5-oxo-4H,5H-pyrano[3,2-c]chromene, C22H18N2O3
  17. Crystal structure of 3-amino-8-methoxy-1-(4-methoxy phenyl)-1H-benzo[f]chromene-2-carbonitrile, C22H18N2O3
  18. Crystal structure of monoaqua-[6,6′-((1E,1′E)-(1,2-phenylene bis(azanylylidene))bis(methanylylidene))bis(4-bromo-2-nitrophenolato-κ4N,N′,O,O′)]zinc(II), C20H12Br2N4O7Zn
  19. Crystal structure of 11-(4-(dimethylamino)phenyl)-17-hydroxy-13-methyl-17-(prop-1-yn-1-yl)-1,2,6,7,8,11,12,13,14,15,16,17-dodecahydro-3H-cyclopenta[a]phenanthren-3-one – acetonitril (1/2), C33H41N3O2
  20. Crystal structure of tert-butyl (phenylsulfinyl)carbamate, C11H15NO3S
  21. Crystal structure of catena-poly{diaqua-bis(3-(1H-1,2,4-triazol-1-yl)benzoato-κ2O:N)copper(II)} monohydrate, C18H18CuN6O7
  22. Crystal structure of tetraaqua-bis(3-(4H-1,2,4-triazol-4-yl)benzoato-κN)cobalt(II), C18H20CoN6O8
  23. The crystal structure of 4-bromo-N-cyclopropyl-2,5-difluorobenzenesulfonamide, C9H8BrF2NO2S
  24. Crystal structure of ([3,3′-bipyridine]-6,6′-dicarboxylato-κ2O:O′)-bis(1,2-bis(4-pyridyl)ethane-κ2N:N′)disilver(I) dihydrate, C37H35Ag2N5O6
  25. The crystal structure of (4-(1H-1,2,4-triazol-1-yl)benzoato-κN)-[4-(1H-1,2,4-triazol-1-yl)benzoic acid-κN]silver(I), C18H13AgN6O4
  26. Crystal structure of 3-(4-methoxyphenyl)-1-(4-methylphenyl)prop-2-en-1-one, C17H16O2
  27. Crystal structure of bis(2-((E)-((4-((E)-1-(ethoxyimino)ethyl)phenyl)imino)methyl)-5-methoxyphenolato-κ2O,N)copper(II), C36H38CuN4O6
  28. Crystal structure of poly[1,2-bis(1,2,4-triazol-4-yl)ethane-κ2N:N′]silver(I) bromate monohydrate]silver(I), C6H10AgBrN6O4
  29. The crystal structure of 2,3,5-triphenyl-2,3-dihydro-1H-tetrazol-1-ium 2,3-dioxoindoline-5-sulfonate, C27H19N5O5S
  30. Crystal structure of 3-(2-amino-1,3-selenazol-4-yl)-2H-chromen-2-one – dimethylformamide (1/1), C15H15N3O3Se
  31. Crystal structure of diethyl 3,3′-(diazene-1,2-diyl)(E)-dibenzoate, C18H18N2O4
  32. Crystal structure of cis-bis((1H-benzimidazol-2-yl)methanol-κN,O)-bis(isothiocyanato-κN)nickel(II), C18H16N6NiO2S2
  33. Crystal structure of bis(2-(2′-hydroxy-5′-methoxyphenyl)-1H-benzimidazole)boron – tetrahydrofuran (1/1), C36H37N4O6B
  34. Crystal structure of poly[aqua-bis(nitrato-κ2O,O′)-(μ3-1,3-benzimidazol-3-ium-1,3-diacetato-κ4O,O′:O′′:O′′′)dysprosium(III)], C11H11DyN4O11
  35. Crystal structure of n-butyl-tris(dicyclo-hexylamido)hafnium(IV), C40H75HfN3
  36. Crystal structure of (E)-1-[1-(3-chloro-4-fluoro-phenyl)ethylidene]-2-(2,4-dinitrophenyl)hydrazine, C28H20Cl2F2N8O8
  37. The crystal structure of ethyl 4-((2-hydroxybenzyl)amino)benzoate, a Schiff base, C16H17NO3
  38. Crystal structure of 3-(2-(4-isobutylphenyl)propanoyl)-1-methylimidazolidine-2,4-dione, C17H22N2O3
  39. Crystal structure of poly[(μ3-2-(pyrazin-2-ylthio)acetato-κ3N:O:S)silver(I)], C6H5AgN2O2S
  40. Crystal structure of (E)-1-(3-((E)-((2-hydroxynaphthalen-1-yl)methylene)amino)phenyl)ethanone O-benzyl oxime, C26H22N2O2
  41. Crystal structure of (E)-2,3-dihydroxybenzaldehyde O-(2-((((E)-1-(2,5-dihydroxyphenyl)ethylidene)amino)oxy)ethyl) oxime monohydrate, C17H20N2O7
  42. Crystal structure of 4-(chloromethyl)-3-nitrobenzoic acid, C8H6ClNO4
  43. Crystal stucture of 4-((10H-phenothiazin-10-yl)methyl)-2,6-di-tert-butylphenol, C27H31NOS
  44. The crystal structure of ethyl 1-(4-nitrophenyl)-5-(trifluoromethyl)-1H-pyrazole-4-carboxylate, C13H10F3N3O4
  45. Crystal structure of catena-poly[di-(μ3-oxido-κ3O:O:O)-tetraoxido-(μ2-5′-(pyrazin-2-yl)-1H,2′H-3,3′-bi(1,2,4-triazole)-κ2N:N′)dimolybdenum(VI)], C8H6Mo2N8O6
  46. Crystal structure of (3,6-dioxocyclohexa-1,4-diene-1,4-bis(olato)-κ4O,O′:O′′,O′′′)-bis(tris(2-pyridylmethyl)amine-κ4N,N′,N′′,N′′′))-dizinc(II) bis(hexafluorophosphate(V)), C42H38F12N8O4P2Zn2
  47. Crystal structure of catena-poly[hexakis(μ2-2-acetylphenolato-κ3O:O,O′)trimanganese(II)], C48H42Mn3O12
  48. The crystal structure of 2,2-difluoro-4-(trifluoromethyl)-2,5-dihydro-[1,3,2]dioxaborinino[5,4-c]chromen-3-ium-2-uide, C11H6BF5O3
  49. Crystal structure of methyl (E)-2-(4-(diethylamino)-2-hydroxybenzylidene)hydrazine-1-carboxylate, C13H19N3O3
  50. The crystal structure of tert-butyl 2,6-dihydropyrrolo[3,4-c]pyrazole-5(4H)-carboxylate, C10H15N3O2
  51. Crystal structure of 1,1-bis(η5-adamantylcyclopentadienyl)-3-phenyl-2-trimethylsilyl-2,3-dihydroisotitanazole, C42H55NSiTi
  52. Crystal structure of 2-(4-(2-(4-benzylpiperazin-1-yl)ethyl)benzyl)isoindoline-1,3-dione, C28H29N3O2
  53. Important impurity of Flupirtine – a single crystal study on ethyl (6-amino-5-((ethoxycarbonyl)amino)pyridin-2-yl)(4-fluorobenzyl)carbamate, C18H21FN4O4
  54. Crystal structure of ethyl 3-(4-methoxyphenyl)-1-(2-(4-methoxyphenyl)-2-oxoethyl)-1H-pyrazole-5-carboxylate, C22H22N2O5
  55. Crystal structure of 2,3,9,10-tetramethoxy-5,6-dihydroisoquinolino[2,1-b]isoquinolin-7-ium 5-hydroxy-3-(4-hydroxyphenyl)-4-oxo-4H-chromen-7-olate methanol solvate, C37H35N1O10
  56. The crystal structure of the inner salt of 2-[(aminoiminomethyl)amino]ethylcarbamic acid [systematic name: (2-((diaminomethylene)ammonio)ethyl)carbamate], C4H10N4O2
  57. Crystal structure of (8-hydroxy-5-nitroquinolinium) perchlorate – 8-hydroxy-5-nitroquinoline (1/1), C18H13ClN4O10
  58. The crystal structure of (5-methyl-1,2,4-oxadiazol-3-yl)ferrocene, C13H12FeN2O
  59. Crystal structure of methyl 1-(2-(fluorosulfonyl)ethyl)-2-oxocyclopentanecarboxylate, C9H13FO5S
  60. Crystal structure of the triclinic modification of 1-methyl-4-nitroimidzole, C4H5N3O2
  61. Corrigendum
  62. Crystal structure of 4-bromo-2-(1H-pyrazol-3-yl)phenol, C9H7BrN2O
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