Startseite Crystal structure of ([3,3′-bipyridine]-6,6′-dicarboxylato-κ2O:O′)-bis(1,2-bis(4-pyridyl)ethane-κ2N:N′)disilver(I) dihydrate, C37H35Ag2N5O6
Artikel Open Access

Crystal structure of ([3,3′-bipyridine]-6,6′-dicarboxylato-κ2O:O′)-bis(1,2-bis(4-pyridyl)ethane-κ2N:N′)disilver(I) dihydrate, C37H35Ag2N5O6

  • Hui-Tao Fan EMAIL logo , Zhi-Guo Zhong , Yu-Han Yang und Ling Zhao
Veröffentlicht/Copyright: 20. Mai 2017

Abstract

C37H35Ag2N5O6, monoclinic, C2/c (no. 15), a = 25.806(2) Å, b = 9.3041(3) Å, c = 18.0702(17) Å, β = 130.346(15)°, V = 3306.7(4) Å3, Z = 4, Rgt(F) = 0.0426, wRref(F2) = 0.0983, T = 296(2) K.

CCDC no.:: 1044919

A part of the polymeric title crystal structure is shown in the figure (symmetry code: ′ = 1−x, y, 1.5−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:Colourless block
Size:0.20 × 0.18 × 0.16 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:12.4 cm−1
Diffractometer, scan mode:Xcalibur, φ and ω
2θmax, completeness:50°, >99%
N(hkl)measured, N(hkl)unique, Rint:5989, 2917, 0.043
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 2160
N(param)refined:226
Programs:CrysAlisPRO [1], SHELX [2]
Table 2

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

AtomxyzUiso*/Ueq
Ag10.21618(2)0.83844(5)0.15737(3)0.04489(17)
N20.2789(2)0.7366(4)0.1307(3)0.0339(10)
N30.6276(2)0.4244(4)0.1340(3)0.0339(10)
O10.3632(2)1.0127(5)0.3482(3)0.0691(14)
O20.29350(18)0.8568(4)0.3369(2)0.0447(10)
O1W0.2744(2)0.1201(5)0.1588(3)0.0798(15)
H1WB0.29720.08900.21650.120*
H1WC0.26210.20210.16330.120*
C10.3922(3)0.9251(5)0.4940(4)0.0356(13)
C20.3695(3)0.8708(5)0.5392(4)0.0354(13)
H20.32560.83430.50160.043*
C30.4102(3)0.8691(5)0.6388(4)0.0403(14)
H30.39300.83610.66770.048*
C40.4776(3)0.9173(5)0.6964(4)0.0363(13)
C50.4996(3)0.9696(5)0.6487(4)0.0418(14)
H50.54850.98350.68510.050*
N1a0.4582(3)0.9732(5)0.5492(4)0.0461(13)
C19a0.4582(3)0.9732(5)0.5492(4)0.0461(13)
H19a0.47451.00780.51940.055*
C60.3467(3)0.9323(6)0.3836(4)0.0393(14)
C70.2845(3)0.5944(6)0.1289(4)0.0399(13)
H70.25750.53700.13410.048*
C80.3273(3)0.5275(5)0.1199(4)0.0376(13)
H80.32810.42760.11800.045*
C90.3692(2)0.6068(5)0.1135(3)0.0285(11)
C100.3633(3)0.7551(5)0.1143(4)0.0369(13)
H100.38990.81440.10920.044*
C110.3182(3)0.8151(5)0.1225(4)0.0358(13)
H110.31520.91480.12230.043*
C120.4181(3)0.5323(5)0.1077(4)0.0365(13)
H12A0.44260.46030.15850.044*
H12B0.39210.48230.04600.044*
C130.4691(3)0.6270(5)0.1168(4)0.0342(13)
H13A0.49140.68520.17480.041*
H13B0.44460.69200.06180.041*
C140.5235(2)0.5527(5)0.1220(3)0.0284(11)
C150.5299(3)0.4049(5)0.1229(4)0.0360(13)
H150.49940.34520.11930.043*
C160.5821(3)0.3464(5)0.1290(4)0.0360(12)
H160.58550.24690.12980.043*
C170.6206(3)0.5671(6)0.1330(4)0.0375(13)
H170.65170.62460.13660.045*
C180.5705(3)0.6340(5)0.1269(4)0.0366(13)
H180.56830.73380.12610.044*
  1. aOccupancy: 0.50.

Source of material

An aqueous NH3 solution in excess was added dropwise to a suspension of Ag2O (0.023 g, 0.1 mmol) in MeOH/H2O (6 mL, 5:1 v/v), and the mixture was stirred for 15 min. 5-(4-Carboxyphenyl)pyridine-2-carboxylic acid (H2L) (0.0122 g, 0.05 mmol), 1,2-bis(4-pyridyl)ethane (bpa) (0.0184 g, 0.1 mmol) were then slowly added, and stirring was continued for another 30 min. The resultant colorless solution was allowed to stand in the dark at room temperature for a week. Colorless prism crystals of the title complex were obtained.

Experimental details

Absorption corrections were applied by using a multi-scan program [1]. The structure was refined based on F2 with the SHELXL [2] software package. Hydrogen atoms were located in difference electron density maps, and treated as riding atoms. The Uiso values of the hydrogen atoms of water molecules were set to 1.5Ueq(O) and the Uiso values of all other hydrogen atoms were set to 1.2Ueq(C). Nitrogen atom N1 is disordered over two closely separated positions (N1, C19) in the ratio of 0.5:0.5.

Discussion

In the past decades, the synthesis of silver(I) complexes has attracted great interest because the silver(I) ion principally exhibits linear, trigonal, trigonal-bipyramidal, square-planar and octahedral coordination geometries and has high affinity for hard donor atoms such as nitrogen or oxygen, being a favorable and fashionable building block for MOFs [3], [4], [5]. In addition, luminescent compounds composed of d10 metal centers are of interest because of their potential applications in the areas of chemical sensors and photochemistry [6], [7]. With the aim of constructing unusual coordination architectures, we have engaged in the research of coordination polymer based on H2L with a silver center. In this paper, we present one new silver coordination polymer based on [3,3′-bipyridine]-6,6′-dicarboxylate (L2−) and bpa = 1,2-bis(4-pyridyl)ethane, exhibiting interesting two-dimensional (2D) tongue-and-groove structure.

Single crystal structure analysis reveals that the title structure consists of one crystallographically unique Ag(I) atom, one half of a L2− ligand, one bpa ligand and one lattice water molecule. As shown in the figure, the central Ag1 cation adopts T-shaped coordination with two nitrogen atoms from two different bpa ligands [Ag1—N2 = 2.182(4) and Ag1—N3′′ = 2.190(4) Å, N2—Ag1—N3′′ = 161.30(15)°; ′′ = 0.5 + x, −0.5+y, z] of bpa ligand in the horizontal direction. The coordination sphere is completed by one oxygen donor L2− [Ag1–O2 = 2.480(4) Å] in the axial direction, forming a T-shaped unit. Both Ag—O and Ag—N bonds are within normal ranges [8]. Each bpa ligand as a bidentate ligand links Ag(I) centers to form infinite 1D chains. Interestingly, two kinds of extended modes are observed for these 1D chains (herein designated as A and B). The complete deprotonated L2− anions, act as pillars, interlinking the upper and lower chains to generate bilayer galleries. The width of the galleries is determined by the length of bpa ligand (9.417(9) Å), and their height is fixed by the length of L2− anion (11.338(7) Å). The assembly of these bilayers results in the so-called tongue-and-groove structure. The structure is stabilized by extensive π-π interactions between the interdigitated bilayers.

Acknowledgement

We gratefully acknowledge the financial support by Collaborative Innovation Center of Water Security for Water Source Region of Mid-line of South-to-North Diversion Project, Henan Province, and Key Laboratory of Ecological Security for Water Source Region of Mid-line of South-to-North Diversion Project of Henan Province, the National Natural Science Foundation of China (No. 21401112), the Science and Technology Research Key Project Department of Education in Henan Province (14A150026) and Nanyang Normal University Scientific Research Foundation Project (QN2016015).

References

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Received: 2016-12-24
Accepted: 2017-5-3
Published Online: 2017-5-20
Published in Print: 2017-7-26

©2017 Hui-Tao Fan 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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