Startseite Naturwissenschaften The crystal structure of catena-poly[aquachlorido(3,3′-([4,4′-bipyridine]-1,1′-diium-1,1′-diylbis(methylene))dibenzoato-κ2O:O′)copper(II)] chloride dihydrate, C26H26Cl2CuN2O7
Artikel Open Access

The crystal structure of catena-poly[aquachlorido(3,3′-([4,4′-bipyridine]-1,1′-diium-1,1′-diylbis(methylene))dibenzoato-κ2O:O′)copper(II)] chloride dihydrate, C26H26Cl2CuN2O7

  • Xiaoli Gao EMAIL logo , Kai Zhu , Wenmin Wang und Liping Lu EMAIL logo
Veröffentlicht/Copyright: 9. Februar 2018

Abstract

{[Cu(C26H20N2O4)Cl(H2O)]+ ⋅ Cl ⋅ 2H2O}n, monoclinic, Cc (no. 9), a = 17.225(4), b = 14.918(3), c = 11.589(3) Å, β = 118.957(3)°, V = 2605.6(10) Å3, Z = 4, Rgt(F) = 0.0334, ωRref(F2) = 0.0819, T = 293 K.

CCDC no.:: 1556766

A representative part of the polymeric title 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:Block, blue
Size:0.40 × 0.30 × 0.20 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:1.09 mm−1
Diffractometer, scan mode:Bruker APEX-II, φ and ω-scans
2θmax, completeness:25.5°, >99%
N(hkl)measured, N(hkl)unique, Rint:11350, 4799, 0.024
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 4420
N(param)refined:344
Programs:Bruker programs [1], SHELX [2, 3] , DIAMOND [4]
Table 2:

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

AtomxyzUiso*/Ueq
Cu10.75077(4)1.31429(3)0.24947(4)0.03834(16)
Cl10.71116(13)1.39479(10)0.06779(15)0.0741(5)
O10.7418(3)1.2499(2)0.3876(4)0.0557(10)
O20.6202(3)1.1867(3)0.2343(5)0.0736(15)
O30.2760(2)0.2906(2)−0.3243(4)0.0491(9)
O40.4073(2)0.2824(3)−0.1465(4)0.0550(9)
O50.7655(3)1.4224(3)0.3535(4)0.0599(10)
H5A0.77841.47170.33620.090*
H5B0.79251.41640.43390.090*
N10.5237(3)0.8986(2)0.3872(4)0.0380(9)
N20.5587(3)0.6186(3)−0.0709(4)0.0395(9)
C10.6772(3)1.1976(3)0.3498(5)0.0431(11)
C20.6707(3)1.1459(3)0.4570(5)0.0373(10)
C30.7302(4)1.1599(4)0.5883(5)0.0486(12)
H30.77471.20260.61210.058*
C40.7242(4)1.1115(4)0.6833(5)0.0619(16)
H40.76441.12200.77160.074*
C50.6589(4)1.0469(4)0.6503(5)0.0535(13)
H50.65681.01310.71620.064*
C60.5972(3)1.0327(3)0.5205(5)0.0380(10)
C70.6033(3)1.0828(3)0.4236(5)0.0379(10)
H70.56171.07420.33540.045*
C80.5241(3)0.9647(3)0.4829(5)0.0439(11)
H8A0.53210.93370.56150.053*
H8B0.46740.99540.44450.053*
C90.5890(3)0.8375(3)0.4280(5)0.0439(11)
H90.63120.83490.51690.053*
C100.5946(3)0.7794(3)0.3416(5)0.0421(11)
H100.64060.73780.37190.051*
C110.5317(3)0.7820(3)0.2079(5)0.0350(10)
C120.4634(3)0.8446(3)0.1693(5)0.0411(11)
H120.41930.84790.08160.049*
C130.4611(3)0.9009(3)0.2599(5)0.0425(11)
H130.41490.94200.23290.051*
C140.5386(3)0.7226(3)0.1101(5)0.0373(10)
C150.4840(4)0.7321(4)−0.0232(5)0.0546(14)
H150.43910.7749−0.05390.066*
C160.4943(4)0.6803(4)−0.1110(6)0.0550(14)
H160.45600.6877−0.20080.066*
C170.6118(4)0.6063(4)0.0583(6)0.0589(15)
H170.65540.56220.08620.071*
C180.6040(4)0.6565(4)0.1502(6)0.0607(16)
H180.64200.64680.23950.073*
C190.5713(4)0.5659(4)−0.1701(6)0.0508(13)
H19A0.62000.5242−0.12450.061*
H19B0.58710.6064−0.22090.061*
C200.4891(3)0.5144(3)−0.2628(5)0.0420(11)
C210.4411(4)0.5399(4)−0.3936(6)0.0548(14)
H210.46000.5882−0.42440.066*
C220.3652(4)0.4937(4)−0.4785(5)0.0638(17)
H220.33410.5097−0.56710.077*
C230.3357(4)0.4239(3)−0.4321(5)0.0473(12)
H230.28300.3948−0.48870.057*
C240.3835(3)0.3967(3)−0.3023(4)0.0355(10)
C250.4612(3)0.4427(3)−0.2182(5)0.0389(10)
H250.49450.4245−0.13090.047*
C260.3546(4)0.3182(3)−0.2513(5)0.0390(12)
Cl20.32101(10)0.89165(10)0.82117(14)0.0651(4)
O60.3709(4)0.9124(3)0.6061(5)0.0896(15)
H6C0.40200.86820.61650.134*
H6D0.34910.90610.65460.134*
O70.4503(3)0.2405(3)0.1085(4)0.0845(15)
H7A0.43270.24970.03000.127*
H7B0.50410.23300.14270.127*

Source of materials

A mixture of 1,1′-bis(3-carboxylatobenzyl)-4,4′-bipyridium dichloride (0.2487 g, 0.50 mmol) and 2,2′-diimidazoleimidazole (0.2487 g, 0.50 mmol) were stirred in 20 mL of distilled water. After that HCl (0.5 mL, 3 mol/L) was added to make the pH = 3. CuCl2⋅4H2O (0.3524 g, 5 mmol) in 10 mL distilled water was added dropwise with constant stirring. Then, the mixture was stirred for 5 h. The resulting mixture was filtered and the filtrate was kept for slow evaporation at room temperature. After 2 weeks, blue block crystals were obtained.

Experimental details

Hydrogen atoms attached to C and O atoms were placed geometrically and refined using a riding model approximation, with C—H = 0.93–0.96 Å and O—H = 0.82 Å. Hydrogen atoms attached water were located from difference Fourier maps, but we didn’t refine their coordinates nor their Uiso parameters. The title structure was refined as an inversion twin (0.146(16)/0.854(16)).

Comment

Metal-organic frameworks have attracted great attention due to their particular structural diversity and potential application as functional materials [5, 6] . The aromatic multicarboxylate ligands have been extensively employed in the preparations of metal-organic coordination polymers. The ligand has a rigid conformation and would therefore facilitate the construction of the resulting coordination networks with regular shapes that can be reasonably predicted [7], [8], [9].

In this study, we choosed a flexible viologen derivative 1,1′-bis(3-carboxybenzyl)-4,4′-bipyridinium dichloride (BpybcCl2) as educt to get a coordination polymer {[Cu(Bpybc)Cl(H2O)]+⋅Cl⋅2H2O}n. The asymmetric unit contains one Cu(II) cation, one Bpybc, one coordinated water, one chlorido ligand, one chloride counter anion and two not coordinating water molecules (cf. the figure). Each Cu center is coordinated by one water molecule, one chlorido ligand and two oxygen atoms of two distinct Bpybc ligands. The Cu—O and Cu—Cl bond lengths are in the expected ranges (1.931–1.955 Å for Cu–O and 2.225 Å for Cu–Cl). In addition, Cu1⋯O2 and Cu1⋯O4A distances are 2.886 Å and 2.767 Å respectively, suggesting non-negligible interactions between the copper atoms and the uncoordinated carboxylate oxygen atoms, which can be described as a semi-chelating coordination mode [10].

Because the methylene groups are used as knots to link together the pyridine rings and phenyl rings, the whole Bpybc ligand is not linear and exhibits a zigzag conformation. Each Bpybc ligand bridges two metal ions through terminal carboxylate groups in a monodentate coordination mode with a Cu⋯Cu distance of 18.51(7) Å (cf. the figure). Thus the title structure exhibits a one-dimensional zigzag chain along the c-axis.

The most intriguing structural feature is an infinite two-dimensional water-chloride network by O—H⋯O and O—H⋯Cl hydrogen bonds between carboxylate oxygen atoms, coordinated water molecules, one independent chloride ion and two independent lattice water molecules in the crystal structures.

Acknowledgements

We gratefully acknowledge support by the National Natural Science Foundation of China (grant no. 21671124), the Provincial Natural Science Foundation of Shanxi Province of China (grant no. 2015021031).

References

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Received: 2017-7-14
Accepted: 2017-12-21
Published Online: 2018-2-9
Published in Print: 2018-3-28

©2018 Xiaoli Gao 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 and optical properties of diaqua-tris(nitrato-κ2O,O′)-bis(4,4,5,5-tetramethyl-2-(p-pyridyl)imidazoline-1-oxyl 3-oxide-κN)praseodymium(III), C24H36N9O15Pr
  3. Crystal structure of dimethanol-bis(μ2-methanol-κ2O:O)-bis{3-((4-methoxy-2-oxidobenzylidene)amino)-2-oxo-2H-chromen-4-olato-κ3O,N,O′}dimanganese(II), C38H38Mn2N2O14
  4. Crystal structure of catena-poly[diaqua-bis(μ2-2-(2-((2,6-dichlorophenyl)amino)phenyl)acetato-κ3O,O′:O′)calcium(II)], C56H48N4Ca2Cl8O12
  5. Crystal structure of catena-poly[triaqua-(isophthalato-κO)-(μ2-1,6-di(1H-imidazol-1-yl)hexane-κ2N:N′)]nickel(II), C20H28N4NiO7
  6. Crystal structure of cyclo[hexaqua-bis[1-[(2-ethyl-1H-imidazol-1-yl) methyl]-1H-benzotriazole-κ2N:N′]-bis(sulfato-κ1O)dicadmium(II)] monohydrate, C24H42Cd2N10O16S2
  7. Crystal Structure of bis(2-fluorbenzoato-κO)-bis(1,10-phenanthroline-κ2N,N′)manganese(II) dihydrate, C38H28F2MnN4O6
  8. Crystal structure of tetrapropylammonium 5-hydroxyisophthalate tetrahydrate, C20H41NO9
  9. Crystal structural of 2-amino-4-(3-bromophenyl)-3-cyano-7,7-dimethyl-5-oxo-4H-5,6,7,8-tetrahydrobenzo[b]pyran, C18H17BrN2O2
  10. Crystal structural of 2-amino-4-(4-methoxyphenyl)-5-oxo-5,6,7,8-tetrahydro-4H-chromene-3-carbonitrile, C17H16N2O3
  11. Crystal structure of catena-poly[aqua(μ2-1,3-bis(1H-benzo[d]imidazol-1-yl)propane-κ2N:N′)-(μ2-5-(tert-butyl)isophthalate-κ3O,O′:O′′)nickel(II)], C29H30N4NiO5
  12. Crystal structure of catena-poly[(μ2-dicyanamido-κ2N:N′)-(μ2-2-(pyridin-2-yl)ethan-1-olato-κ3N,O:O′)copper(II)], C9H8CuN4O
  13. Crystal structure of bis(5,5′-((butane-1,4-diylbis(azanylylidene))bis(methanylylidene))bis(3-(ethoxycarbonyl)-2,4-dimethylpyrrol-1-ido-k4N,N′,N′′,N′′′)copper(II), C24H32CuN4O4
  14. The crystal structure of the formamide solvate of (17b)-estra-1,3,5(10)-triene-3,17diol, C19H27NO3
  15. Crystal structure of catena-poly[diaqua-bis(μ2-1H-benzo[d]imidazole-5-carboxylato-κ2N:O)nickel(II)] dihydrate, C16H18N4NiO8
  16. Crystal structure of dibromido[(1,2-bis(diisopropylphosphino)-1,2-dicarba-closo-dodecaborane-κ2P,P′]nickel(II), C14H38B10NiBr2P2
  17. The crystal structure of catena-poly[aquachlorido(3,3′-([4,4′-bipyridine]-1,1′-diium-1,1′-diylbis(methylene))dibenzoato-κ2O:O′)copper(II)] chloride dihydrate, C26H26Cl2CuN2O7
  18. The crystal structure of N′-(2-nitrobenzylidene)-2-phenylacetohydrazide, C15H13N3O3
  19. Crystal structure of dichlorido bis[1-[(2-methyl-1H-benzoimidazol-1-yl)methyl]-1H-benzotriazole-κ1N]cadmium(II), C30H26CdCl2N10
  20. Crystal structure of aqua-bis(3-(2-pyridyl)-5-(4-pyridyl)-1H-1,2,4-triazole-κ2N,N′)copper(II) sulfate tetrahydrate, C24H28CuN10O9S
  21. Crystal structure of dibromido-carbonyl-(η6-p-cymene)osmium(II), C11H14Br2OOs
  22. Crystal structure of catena-poly[chlorido-(μ2-chlorido)-bis(imidazole-κN)copper(II)] C6H8Cl2CuN4
  23. Crystal structure of [(1,2-bis(dicyclohexylphosphino)-1,2-dicarba-closo-dodecaborane-κ2P,P′]dibromidonickel(II)), C26H54B10NiBr2P2
  24. Crystal structure of dichlorido[1,1′-bis(diphenylphosphanyl)ferrocene-κ2P,P′]zinc(II), C34H28FeCl2P2Zn
  25. Crystal structure of tris(μ2-2-(pyridin-2-yl)ethan-1-olato-κ3N,O:O)-trithiocyanato-κN-dicobalt(III), C24H24Co2N6O3S3
  26. The crystal structure of diaqua-2,2′-((cyclohexane-1,2-diylbis(azanylylidene))bis(methanylylidene))diphenolato-κ4N,N′,O,O′)manganese(III) perchlorate, C20H24MnClN2O4
  27. Crystal structure of bis(μ3-chlorido)-bis(μ2-chlorido)-tetrakis(μ2-2,6-bis (diphenylmethyl)-4-t-butylphenolato)tetralithium(I)dicobalt(II) toluene solvate, C75.5H70Cl2CoLi2O2
  28. The crystal structure of hexaaqua-bis(μ2-3-(3-(pyridin-4-yl)-1,2,4-oxadiazol-5-yl)propanoato-κ2O:O′)-tetrakis(3-(3-(pyridin-4-yl)-1,2,4-oxadiazol-5-yl)propanoato-κO)dierbium(III) octahydrate, C60H76N18O32Er2
  29. Crystal structure of dimethylammonium bis(naphthalene-2,3-diolato)borate, C22H20BNO4
  30. Crystal structure of 2-amino-4-(4-nitro-phenyl)-7,7-dimethyl-5-oxo-5,6,7,8-tetrahydro-4H-chromene-3-carbonitrile, C18H17N3O4
  31. The crystal structure of (E)-4-chloro-2-(((5-methylpyridin-2-yl)imino)methyl)phenol, C13H11ClN2O
  32. Crystal structure of bis(N,N,N-trimethylbutanaminium) poly[heptaselenidotristannate(IV)], C14H36N2Se7Sn3
  33. The crystal structure of N-((3,5-di-tert-butyl-4-hydroxyphenyl)(phenyl)methyl)-4-methylbenzenesulfonamide, C28H35N3S
  34. Crystal structure of 2-(4-chlorophenyl)-2,3-dihydro-1H-perimidine, C17H13Cl1N2
  35. The Crystal structure of 2-iodo-1-(p-tolyl)propan-1-one, C10H11IO
  36. Crystal structure of ethyl 1-(4-bromobenzyl)-3-phenyl-1H-pyrazole-5-carboxylate, C19H17BrN2O2
  37. Crystal structure of ethyl 1-(4-fluorobenzyl)-3-phenyl-1H-pyrazole-5-carboxylate, C19H17FN2O2
  38. Crystal structure of catena-poly[diaqua-(μ2-2,5-dihydroxyterephthalato-κ4O,O′:O′′,O′′′)cadmium(II)], C8H8O8Cd
  39. Crystal structure of tetraaqua-bis[6-(1H-imidazol-1-yl-κN)nicotinato]zinc(II), C18H20N6O8Zn
  40. Crystal structure of dichlorido-bis(N-phenyl-2-(quinolin-8-yloxy)acetamide-κ2N,O) – acetone (2/1), C35.5H31N4O4.5Cl2Cu
  41. Crystal Structure of ethyl (E)-3,4-dimethyl-5-((2-(4-methylbenzoyl)hydrazono)methyl)-1H-pyrrole-2-carboxylate — water — ethanol (1/1/1), C20H29N3O5
  42. Crystal structure of 5-((4-(1H-benzo[d]imidazol-2-yl)-2-methoxyphenoxy)methyl)-2-chlorothiazole - trichloromethane - methanol (1/1/1), C20H19Cl4N3O3S
  43. The crystal structure of a matrine derivative: 41S,7aS,12S,13aR,13bR)-12-(4-methylpiperazin-1-yl)dodecahydro-1H,5H,10H-dipyrido[2,1-f:3′,2′,1′-ij][1,6]naphthyridin-10-one, C20H34N4O
  44. Crystal structure of cesium beryllophosphate, Be3Cs2P4O14
  45. Crystal Structure of 3-((3-hydroxybenzyl)ammonio)-3-phenylpropanoate, C16H17NO3
  46. Crystal structure of 9,10-dimethoxy-5,6-dihydro-[1,3]dioxolo[4,5-g]isoquinolino[3,2-a]isoquinolin-7-ium chloride — 4-hydroxy-3-methoxybenzoic acid — water (2/1/5), C48H54N2Cl2O17
  47. The crystal structure of (1R, 2R)-N1,N2-diferrocenyl-1,2-cyclohexanedicarboxamide, C28H30Fe2N2O2
  48. Crystal structure of N-(2-methylphenyl)ethoxycarbothioamide, C10H13NOS
  49. Crystal Structure of ethyl (E)-2,4-dimethyl-5-((2-tosylhydrazono)methyl)-1H-pyrrole-3-carboxylate monohydrate, C17H23N3O5
  50. Crystal structure of Diiodo-(N′-((quinolin-8-yl)methylene)isonicotinohydrazide κ3N,N′,O)cadium(II) – dimethylformamide (1/1), C19H19N5O2CdI2
  51. Crystal structure of dinitrato-(N′-((quinolin-8-yl)methylene)isonicotinohydrazide κ3-N,N′,O)copper(II), C16H12N6O7Cu
  52. Crystal structure of benzoato-κO-bis(1,3,5-triaza-7-phosphaadamantane-κP)silver(I) monohydrate C19H31AgN6O3P2
  53. Crystal structure of (E)-2-(anthracen-9-ylmethylene)hydrazine-1-carbothioamide, C16H13N3S
  54. The crystal structure of 8-chloro-7-ethyl-1,3-dimethyl-1H-purine-2,6(3H,7H)-dione, C9H11ClN4O2
  55. Crystal structure of {5,5′-((propane-1,3-diylbis(azanylylidene))bis(methanylylidene))bis(3-(ethoxycarbonyl)-2,4-dimethylpyrrol-1-ido)-κ4N,N′,N′′,N′′′}zinc(II), C23H30N4O4Cu
  56. Crystal structure of bis(4-dimethylamino-pyridin-1-ium)tetrafluorosuccinate, C18H22F4N4O4
  57. Crystal structure of dimethyl 3,9-dibenzyl-6,12-dicyclohexyl-3,9-diazahexacyclo [6.4.0.02,7.04,11.05,10]-dodecane-1,11-dicarboxylate, C40H50N2O4
  58. Crystal structure of diethyl 3,9-diphenyl-6,12-bis(3-methoxyphenyl)-3,9-diazahexacyclo[6.4.0.02,7.04,11.05,10]dodecane-1,11-dicarboxylate, C42H42N2O6
  59. Crystal structure of bis(acetato-κO)-bis(1-(pyridin-2-yl)ethan-1-one oxime-κ2N,N′)nickel(II), C18H22N4NiO6
  60. Crystal structure of (N-(3-ethoxy-2-oxidobenzylidene)-4-fluorobenzohydrazonato-κ3N,O,O′)-diphenyltin(IV), C28H23FN2O3Sn
  61. Crystal structure of {N-(3-ethoxy-2-oxidobenzylidene)-4-fluorobenzohydrazonato-κ3O,N,O′}dimethyltin(IV), C18H19FN2O3Sn
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