Home Crystal structure of poly[(thiophene-3,4-dicarboxylato-κ1O)bis[1,2-bis(4-pyridyl)ethane-κ2N:N′]silver(I)] octahydrate, C30H42Ag2N4O12S
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Crystal structure of poly[(thiophene-3,4-dicarboxylato-κ1O)bis[1,2-bis(4-pyridyl)ethane-κ2N:N′]silver(I)] octahydrate, C30H42Ag2N4O12S

  • Xue-Guo Liu , Wei-Hong Yan , Hui-Tao Fan EMAIL logo and Teng-Teng Qin
Published/Copyright: July 6, 2017
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Zeitschrift für Kristallographie - New Crystal Structures
From the journal Zeitschrift für Kristallographie - New Crystal Structures Volume 232 Issue 5

Abstract

C30H42Ag2N4O12S, monoclinic, Pc (no. 7), a = 11.4150(3) Å, b = 17.3038(9) Å, c = 9.3802(5) Å, β = 104.701(4)°, V = 1792.15(14) Å3, Z = 2, Rgt(F) = 0.0320, wRref(F2) = 0.0638, T = 293(2) K.

CCDC no.:: 1525095

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 prism
Size:0.20 × 0.18 × 0.16 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:12.2 cm−1
Diffractometer, scan mode:Xcalibur Eos, φ and ω
2θmax, completeness:50°, >99%
N(hkl)measured, N(hkl)unique, Rint:6576, 4195, 0.020
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 3760
N(param)refined:453
Programs:SHELX [1], CrysAlisPRO
Table 2

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

AtomxyzUiso*/Ueq
Ag10.07394(3)0.46122(2)0.12248(6)0.05222(13)
Ag2a0.3113(2)0.9996(8)0.3502(4)0.0695(15)
Ag2′b0.3075(6)1.0311(10)0.3366(9)0.0521(15)
C10.4893(5)0.9323(4)0.1988(7)0.0590(17)
H10.45050.88790.21900.071*
C20.5828(7)0.9246(3)0.1327(9)0.0545(14)
H20.60410.87570.10650.065*
C30.6456(5)0.9882(3)0.1045(6)0.0330(13)
C40.6045(5)1.0587(3)0.1416(7)0.0434(14)
H40.64231.10390.12340.052*
C50.5084(5)1.0629(4)0.2049(6)0.0541(16)
H50.48221.11130.22710.065*
C60.7504(5)0.9831(3)0.0382(6)0.0429(15)
H6A0.74741.0258−0.02970.051*
H6B0.74560.9353−0.01710.051*
C70.8713(5)0.9856(4)0.1579(7)0.0510(16)
H7A0.87361.03190.21690.061*
H7B0.87590.94130.22240.061*
C80.9781(5)0.9852(3)0.0933(6)0.0370(14)
C91.0230(5)0.9196(3)0.0469(7)0.0606(17)
H90.98940.87200.06070.073*
C101.1170(5)0.9224(4)−0.0198(8)0.0668(19)
H101.14410.8764−0.05180.080*
C111.1291(5)1.0511(4)0.0066(7)0.0546(17)
H111.16531.0978−0.00660.066*
C121.0356(5)1.0524(3)0.0737(7)0.0517(16)
H121.01111.09910.10600.062*
C130.2790(5)0.4019(3)−0.0059(6)0.0393(14)
H130.25770.35490.02850.047*
C140.3761(5)0.4045(3)−0.0701(6)0.0381(13)
H140.41880.3597−0.07840.046*
C150.4088(5)0.4731(3)−0.1210(6)0.0313(13)
C160.3427(6)0.5379(3)−0.1061(7)0.0450(16)
H160.36250.5858−0.13850.054*
C170.2481(6)0.5308(3)−0.0432(8)0.0452(17)
H170.20370.5750−0.03550.054*
C180.5164(5)0.4782(3)−0.1898(6)0.0398(14)
H18A0.51280.4358−0.25850.048*
H18B0.51200.5262−0.24430.048*
C190.6349(5)0.4748(3)−0.0722(7)0.0458(16)
H19A0.64270.4246−0.02470.055*
H19B0.63460.51380.00200.055*
C200.7432(5)0.4883(4)−0.1372(6)0.0401(16)
C210.8155(5)0.4293(4)−0.1607(7)0.0472(14)
H210.80210.3792−0.13260.057*
C220.9086(6)0.4442(4)−0.2262(8)0.0502(17)
H220.95690.4032−0.24080.060*
C230.8606(5)0.5716(4)−0.2476(7)0.0452(15)
H230.87370.6211−0.27930.054*
C240.7680(5)0.5610(4)−0.1804(7)0.0431(15)
H240.72210.6030−0.16430.052*
C250.1178(4)0.2745(3)0.3646(5)0.0331(11)
C260.0715(5)0.2916(3)0.4814(6)0.0454(13)
H26−0.01030.30060.47310.054*
C270.2887(5)0.2729(4)0.5569(7)0.0633(18)
H270.37000.26760.60610.076*
C280.2463(4)0.2640(3)0.4089(6)0.0399(12)
C290.0407(4)0.2720(3)0.2100(6)0.0369(12)
C300.3244(5)0.2400(3)0.3099(7)0.0505(14)
N10.2151(5)0.4654(3)0.0077(6)0.0388(14)
N20.9328(5)0.5149(4)−0.2699(6)0.0428(13)
N30.4515(5)1.0004(4)0.2355(7)0.0531(16)
N41.1705(5)0.9875(3)−0.0404(6)0.0456(14)
O10.0686(4)0.31415(18)0.1169(5)0.0548(8)
O2−0.0501(3)0.2281(2)0.1861(4)0.0556(10)
O30.2817(3)0.1943(3)0.2104(6)0.0893(16)
O40.4285(3)0.2673(3)0.3376(5)0.0811(14)
O50.5843(4)0.3153(3)0.6076(5)0.0812(14)
H5A0.54190.30460.52160.122*
H5B0.65590.29840.61820.122*
O60.7931(3)0.2026(3)0.3612(5)0.0710(13)
H6C0.84170.21040.30750.107*
H6D0.73160.22710.30710.107*
O70.7764(3)0.1832(3)0.9401(4)0.0712(12)
H7C0.79790.18490.85980.107*
H7D0.80880.22040.99520.107*
O80.5950(3)0.2794(3)0.1875(5)0.0823(14)
H8A0.54300.27570.23300.123*
H8B0.60260.27490.10010.123*
O90.5515(4)0.2484(3)0.8748(5)0.0793(14)
H9A0.62150.22800.89480.119*
H9B0.54920.26230.78630.119*
O100.8111(4)0.2424(3)0.6438(5)0.1015(18)
H10A0.81940.24430.55640.152*
H10B0.87590.25760.70380.152*
O110.0253(4)0.2399(3)0.8564(4)0.0950(17)
H11A0.03900.26240.93750.142*
H11B0.06400.25320.80290.142*
O120.3242(4)0.1822(3)0.9342(5)0.1005(19)
H12A0.38870.19460.91030.151*
H12B0.31720.20941.00690.151*
S10.17910(14)0.29462(12)0.64327(17)0.0768(6)

  1. aOccupancy: 0.72(3); bOccupancy: 0.28(3).

Source of materials

An excess of an aqueous NH3 solution was slowly added to a suspension of AgNO3 (0.0169 g, 0.1 mmol) in MeOH/H2O (6 mL, 5:1 v/v), and the mixture was stirred for 30 min. Thiophene-3,4-dicarboxylic acid (0.0086 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 multi-scan program. Hydrogen atoms attached to C and O of the title complex and water molecules 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). Silver atom Ag2 is disordered over two closely separated positions (Ag2, Ag2′) in the ratio of 0.28:0.72. Flack parameter: 0.00(10).

Comment

In the past decades, the syntheses of silver (I) complexes have attracted great interest because the silver(I) exhibits diverse coordination geometries such as linear, trigonal, square-planar and octahedral ones [2], [3], [4], [5], [6]. In recent years, many MOFs with more than two polymeric substructures in the crystalline state have been reported, which usually occur in an interpenetrating fashion [7, 8] . However, examples of metal-organic frameworks involving more than one coordination polymer with different structural motifs in a single crystal structures are rare [9, 10] . With the aim of constructing unusual coordination architectures, we have engaged in the synthesis of coordination polymers based on a new thiophene-3,4-dicarboxylic acid with silver center.

Single crystal structure analysis reveals that the title complex consists of two crystallographically independent Ag(I), one thiophene-3,4-dicarboxylato ligand, two bpa ligands and eight water molecules. As shown in the Figure, the central Ag1 cation adopts T-shaped coordination with two nitrogen atoms from two bpa ligands [Ag1—N1 = 2.141(2) and Ag1—N2′ = 2.157(7) Å, N2′—Ag1—N1 = 167.32(3)° (′ = −1+x, 1−y, z+1/2′)] in the horizontal direction. The coordination sphere is completed by one oxygen of one deprotonated L2− [Ag1–O1 = 2.547(4) Å] in the axial direction. While the Ag2 adopts linear geometry [Ag2—N3 = 2.118(8) and Ag2—N4′′ = 2.146(7) Å, N3—Ag2—N4′′ = 177.71(3)° (′′ = −1+x, 2−y, z+1/2′)] being coordinated by two nitrogen atoms from two different bpa ligands. In the title complex, each bpa ligand as a bidentate ligand links Ag(I) centers to form infinite 1D chains. There are two kinds of Ag-bpa chains (herein designated as A and B). Within chain A, bpa ligands bridge crystallographically unique Ag1 centers into an infinite Ag-bpa chain, with the thiophene-3,4-dicarboxylic acid ligand dangling on the side. Chain B is exclusively constructed with Ag2 ions and bpa ligands. Interestingly, water molecules are located in the gaps between the two types of chains. Adjacent chains are linked through hydrogen bonding interactions, resulting in three-dimensional frameworks.

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).

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Received: 2016-12-30
Accepted: 2017-6-14
Published Online: 2017-7-6
Published in Print: 2017-9-26

©2017 Xue-Guo Liu et al., published by De Gruyter, Berlin/Boston

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

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https://doi.org/10.1515/ncrs-2016-0369
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Articles in the same Issue

  1. Cover and Frontmatter
  2. Crystal structure of 2-(2-ethoxyphenyl)-7-propyl-5-methylimidazo[5,1-f][1,2,4]triazin-4(3H)-one, C17H20N4O2
  3. Crystal structure of catena-poly[aqua-(μ3-1,3,5-benzenetricarboxylato-κ3O:O′:O′′)-[μ3hydroxy-(1,3-di-(μ2-1,2,4-triazole-4-yl)benzoato-κ2N:N′)copper(II)], C19H16Cu2N6O9
  4. Crystal structure of poly[aqua-(μ3-3,5-di(4H-1,2,4-triazolyl-4-κ3N,N′:N′′)benzenecarboxylato)silver(I)], C11H9AgN6O3
  5. Crystal structure of tetrapropylammonium hydrogen carbonate, C13H29NO3
  6. Crystal structure of poly[μ2-acetato-κ3-O,O′:O′)diaqua(μ3-isophthalato-κ4O,O′:O′′:O′′′)yttrium(III)] monohydrate, C20H24O17Y2
  7. Crystal structure of catena-poly[dichlorido-(μ2-4-(1H-pyrazol-3-yl)-pyridine-κ2N,N′)]cadmium(II), C48H42Cd3Cl16N18
  8. Crystal structure of bis(tetraethylammonium) [1,1′-biphenyl]-2,2′-dicarboxylate trihydrate, C30H54N2O7
  9. Crystal structure of poly[(thiophene-3,4-dicarboxylato-κ1O)bis[1,2-bis(4-pyridyl)ethane-κ2N:N′]silver(I)] octahydrate, C30H42Ag2N4O12S
  10. The crystal structure of amine-(4-(1H-1,2,4-triazol-1-yl)benzoato-κN)silver(I) dihydrate, C9H13AgN4O4
  11. Crystal structure of poly[tetrakis(μ2-cyanido-κ2N:O)-cyanido-tris(pyridine)dicobalt(II/III)], C20H15Co2N8
  12. Crystal structure of bis(pyridine)-bis(2-formyl-4,6-dichlorophenolato)cobalt(II), C24H16Cl4CoN2O4
  13. Crystal structure of (E)-1-(4-(((E)-5-bromo-2-hydroxybenzylidene)amino)phenyl)ethan-1-one O-methyl oxime, C16H15BrN2O2
  14. Crystal structure of catena-poly[(μ2-3-(1H-pyrazol-4-yl)-5-(pyridin-4-yl)-1,2,4-triazole-κ N:N′)-bis(benzoato-κO)zinc(II)], C24H18N6O4Zn
  15. Hydrothermal synthesis and crystal structure of a poly[aqua-(μ4-4-(carboxylatomethyl)benzoato-κ4O:O′:O′′:O′′′)-(μ2-1-(4-(1H-imidazol-1-yl)benzyl)-1H-1,2,4-triazole-κ2N:N′) dimanganese(II)], [Mn2(C9H6O4)2(C12H11N5)(H2O)]
  16. Crystal structure of diaqua-catena-poly[diaqua-bis(μ2-5-(4-(1H-1,2,4-triazol-1-yl)phenyl)tetrazol-2-ido-κ2N:N′)cobalt(II)] dihydrate, C20H24CoN14O4
  17. Crystal structure of bis(μ3-2,2′-azanediylbis(ethan-1-olato)-κ5O:O,N,O′:O′)-tetrachlorido-bis(μ2-2-((2-hydroxyethyl)amino)ethan-1-olato-κ3N,O:O)dicobalt(II)dicobalt(III), C16H38Cl4Co4N4O8
  18. Crystal structure of poly[μ4-(4-(carboxylatomethyl)benzoato-κ4O:O′:O′′:O′′′)-(2-(4-(1H-imidazol-1-yl)phenyl)-1H-benzo[d]imidazole-κN)manganese(II)] [Mn(C9H6O4)(C16H12N4)]
  19. Crystal structure of 4-chloro-6-phenylpyrimidine, C10H7ClN2
  20. The crystal structure of [6-methoxy-2-(2,2,2-trifluoroacetyl)-3,4-dihydronaphthalen-1(2H)-one]difluoroborane, C13H10BF5O3
  21. Crystal structure of 3,3′-(butane-1,4-diylbis(azanylylidene))bis(1-phenylbut-1-en-1-olato)-κ4N,N′,O,O′]copper(II), C24H26N2O2Cu
  22. Crystal structure of tetraaqua-bis((E)-N′-(2-bromobenzylidene)isonicotinohydrazide-κN)zinc(II) dinitrate, C26H28N8O12Br2Zn
  23. Crystal structure of 2-amino-4-(4-bromophenyl)-5-oxo-5,6,7,8-tetrahydro-4H-chromene-3-carbonitrile, C16H13BrN2O2
  24. A single crystal study on tert-butyl-4-((4-(4-bromo-2-fluorophenylamino)-6-methoxyquinazolin-7-yloxy)methyl)piperidine-1-carboxylate, C26H30BrFN4O4
  25. Crystal structure of 1,1′-((1E,1′E)-(((ethane-1,2-diylbis(oxy))bis(2,1-phenylene))bis(azanylylidene))bis(methanylylidene))bis(naphthalen-2-olato-κ3O,O′,N)zinc(II), C36H26N2O4Zn
  26. Crystal structure of diaqua-bis(5′-(pyridin-1-ium-4-yl)-1H-[3,3′-bi(1,2,4-triazol)]-2′-ide-κ2N,N′)cobalt(II) — bis(5-(pyridin-4-yl-κN)-1H,1′H-3,3′-bi(1,2,4-triazole))octamolybdate – water (2/1/8), C27H33CoMo4N21O19
  27. Crystal structure of 3-cyclohexyl-2-(cyclohexylimino)-2,3-dihydro-6,8-diiodo-4H-1,3-benzoxazin-4-one, C20H24I2N2O2
  28. Crystal structure of dinitrato-κO-bis(tris((1H-benzo[d]imidazol-2-yl)methyl)amine-κ4N,N′,N′′,N′′′)-(μ2-cyclohexane-1,4-dicarboxylato-κ4O,O′:O′′,O′′′)dimanganese(II) – methanol – water (1/6/2), C62H80Mn2N16O18
  29. Crystal structure of bis(2-hydroxyethyl(phenyl)carbamodithioate)nickel(II), C18H20N2NiO2S4
  30. Crystal structure of methyl 1-(4-fluorobenzyl)-4-methoxy-5-oxopyrrolidine-3-carboxylate, C14H16FNO4
  31. Crystal structure of di-μ-iodido-bis(6-(p-tolyl)-2,2′-bipyridine-κ2N,N′)dicopper(I) — 2-(diphenylphosphoryl)benzoic acid (1/2), C36H29CuIN2O3P
  32. Crystal structure of 2-amino-4-(3-bromo-4-fluoro-phenyl)-7,7-dimethyl-5-oxo-5,6,7,8-tetrahydro-4H-chromene-3-carbonitrile, C18H16BrFN2O2
  33. Crystal structure of bis(μ2-2-chlorobenzoato-κ3O,O′:O′)-(2-chlorobenzoato-κO)-(2-chlorobenzoato-κO,O′)-bis(1,10-phenanthroline-κ2N,N′)-dicadmium(II) monohydrate, C52H36Cd2Cl4N4O10
  34. Crystal structure of 2-(8a-methyl-5-oxo-hexahydroimidazo [1,2-a]pyridin-1(5H)-yl)-2-oxoethyl acetate, C12H18N2O4
  35. Crystal structure of (E)-N,N-diethyl-2-(5-nitrothiazol-2-yl)-1-phenylethen-1-amine, C15H17N3O2S
  36. Crystal structure of diazido-dimethanolato-bis(μ2-2-(((3-oxidopropyl)imino)methyl)phenolato-κ4O:O,O′,N)dimanganese(III), C22H28Mn2N8O6
  37. The crystal structure of bis(2-(2,2,2-trifluoroacetyl)-3,4-dihydronaphthalen-1-olato-κ2O,O′)copper(II), C24H16CuF6O4
  38. Crystal structure of hexaaquanickel(II) bis((E)-4-((4-(dimethylamino)phenyl)diazenyl)benzenesulfonate), C28H40N6NiO12S2
  39. Crystal structure of catena-poly[aqua-(μ2-hexamethylenetetramine-κ2N:N′)-bis(2,6-difluorobenzoato-κ2O:O′)cadmium(II)]monohydrate, C20H22CdF4N4O6
  40. Crystal structure of 3-benzyl-2,3-dihydro-2-thioxoquinazolin-4(1H)-one, C15H12N2OS
  41. Crystal structure of bis(μ2-ferrocenecarboxylato-κ2O:O′)-bis(1,10-phenanthroline-κ2N,N′)-(μ2-methanolato-κ2O,O)dicopper(II) tetrafluoroborate – acetonitrile (1/1), C49H40BCu2F4Fe2N5O5
  42. The crystal structure of tetrakis(1,3,5-triaza-7-phosphatricyclo[3.3.1.13,7]decane-κP)silver(I) chloride dihydrate, C24H60AgClN12O6P4
  43. Crystal structure of 5-ethyl-2-(p-tolyl)-1,3-dioxane-5-carboxylic acid, C14H18O4
  44. Crystal structure of 2-(4-fluorophenyl)-1,3-dimethyl-1H-perimidin-3-ium iodide, C19H16ClIN2
  45. Crystal structure of catena-poly[(μ2-hexamethylenetetramine-κ2N:N′)-tetrakis(μ2-2,6-difluorobenzoato-κ2O:O′)dicopper(II)], C34H24Cu2F8N4O8
  46. Crystal structure of ethyl 3-hydroxy-5-methyl-2-(4-(m-tolyl)-1H-1,2,3-triazol-1-yl)-[1,1′-biphenyl]-4- carboxylate, C25H24N3O3
  47. The crystal structure of carbonyl(2-oxopyridin-1(2H)-olato-κ2O,O′)-(diphenylcyclohexylphosphine-κP)rhodium(I), C24H25NO3PRh
  48. Crystal structure of bis((pyrazin-2-ylmethyl)(pyrazine-2-carbonyl)amido-κ3N,N′,N′′)copper(II), C20H16CuN10O2
  49. Crystal structure of catena-poly[tetraaqua-(μ2-succinonitrile-κ2N:N′)cobalt(II)] dinitrate, C4H12CoN4O10
  50. The crystal structure of 1,1′-bisisoquinoline, C18H12N2
  51. Crystal structure of bis(hydroxydi(pyridin-2-yl)methanolato-κ3N,N′,O)cobalt(III) perchlorate dihydrate, C22H22ClCoN4O10
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