Startseite 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
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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

  • Xin Ling-Yun , Zhang Hai-Yan und Liu Guang-Zhen EMAIL logo
Veröffentlicht/Copyright: 18. August 2017

Abstract

C20H24CoN14O4, triclinic, P1̅ (no. 2), a = 7.797(2) Å, b = 8.766(3) Å, c = 9.709(3) Å, α = 73.554(7)°, β = 86.460(7)°, γ = 78.537(7)°, V = 623.7(3) Å3, Z = 1, Rgt(F) = 0.0303, wRref(F2) = 0.0752, T = 293(2) K.

CCDC no.:: 1565201

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:Orange block
Size:0.35 × 0.31 × 0.27 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:7.5 cm−1
Diffractometer, scan mode:Bruker SMART, φ and ω-scans
2θmax, completeness:50.2°, >99%
N(hkl)measured, N(hkl)unique, Rint:4013, 2205, 0.019
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 2028
N(param)refined:181
Programs:Bruker programs [1], SHELX [2]
Table 2

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

AtomxyzUiso*/Ueq
Co10.00000.5000−0.50000.02585(13)
N10.2481(2)0.3879(2)−0.39937(17)0.0307(4)
N20.3920(2)0.3390(3)−0.46331(19)0.0451(5)
N30.5193(2)0.2756(3)−0.3649(2)0.0485(5)
N40.2769(2)0.3586(2)−0.25854(18)0.0333(4)
N50.8944(2)0.1295(2)0.33860(18)0.0339(4)
N61.0521(3)0.1377(3)0.2737(3)0.0620(7)
N70.9939(2)0.3072(2)0.41005(18)0.0316(4)
C10.4444(2)0.2892(2)−0.2408(2)0.0298(4)
C20.5342(2)0.2287(2)−0.1019(2)0.0299(4)
C30.4767(3)0.2932(3)0.0109(3)0.0400(5)
H30.38290.3800−0.00210.048*
C40.5576(3)0.2295(3)0.1427(2)0.0430(5)
H40.51810.27410.21780.052*
C50.7569(3)0.0380(3)0.0510(2)0.0368(5)
H50.8524−0.04720.06340.044*
C60.6762(3)0.1013(2)−0.0812(2)0.0343(5)
H60.71740.0582−0.15690.041*
C70.6975(3)0.0997(2)0.1646(2)0.0354(5)
C80.7827(3)0.0268(3)0.3092(3)0.0454(6)
H8A0.69300.01220.38290.054*
H8B0.8526−0.07890.31250.054*
C90.8626(3)0.2305(3)0.4180(2)0.0369(5)
H90.76150.24600.47240.044*
C101.1053(3)0.2450(3)0.3213(3)0.0493(6)
H101.21280.27600.29540.059*
O1W−0.1399(2)0.3845(2)−0.32325(16)0.0466(4)
H1WA−0.12120.3788−0.23640.070*
H1WB−0.24090.3611−0.32090.070*
O2W0.0117(3)0.6243(3)0.06959(19)0.0625(5)
H2WA0.00340.6924−0.01290.094*
H2WB−0.08890.62640.10900.094*

Source of material

All reagents used in these syntheses were of analytical grade and used as purchased without further purification. The title compound was synthesized by hydrothermal methods. The mixtures of 1-(tetrazo-5-yl)-4-(1,2,4-triazol-1-ylmethyl)benzene (ttmb)(0.1 mmol, 22.7 mg), Co(OAC)2⋅2H2O (0.1 mmol, 24.9 mg), NaOH (0.1 mmol), and H2O (6.0 ml) were placed in a 23 ml Teflon liner stainless steel reactor. The vessel was heated to 393 K for 4 days, and then slowly cooled to room temperature. Orange crystals were obtained, and further crystals were filtered off, washed, and dried under ambient conditions. Yield 56%.

Experimental details

Hydrogen atoms were placed in calculated positions using the riding model except for those bound to water molecules, which were initially located in a difference Fourier map and included in the final refinement by use of geometrical restraints with the O–H distances being fixed at 0.85 Å and Uiso(H) equivalent to 1.5 times of Ueq(O).

Discussion

Over the past decades, there has been much interest in the fabrication of coordination polymers (CPs) because of fascinating structural diversities and framework topologies, as well as their potential applications in the fields of ion-exchange, adsorption, catalysis, magnetism, and luminescence, and so on [3], [4], [5], [6], [7]. Structural design of CPs owing the expected functions is still not easy, and there remains a great challenge to truly understand the factors that affect their formation [8]. It is known that the structures of such complexes can often be adjusted by the intelligent selection of organic ligands with suitable shape, functionality, flexibility, and symmetry, and the coordination geometry of the metal ions, the reaction conditions, and so on [9], and much attention has been focusing on tuning the frameworks through rational selection of structurally related ligands. Among them, tetrazole-based ligands have attracted much attention because its four nitrogen electron-donating atoms allows it to serve as either a multidentate ligand or a bridging building block in supramolecular assemblies [10]. However, ligands based on tetrazole-based ligands as building blocks for constructing coordination complexes have been less studied. In recent times we have elected such technique to form coordination polymers that use tetrazole-based ligands to link metal centers. These CPs provided a class of compounds displaying interesting chemical and physical properties such as second harmonic generation (SHG), fluorescence, ferroelectric, dielectric behaviors and magnetic interaction properties and so on [11], [12], [13], [14].

The asymmetric unit of the title crystal structure contains one half of a Co atom, one ttmb anion, one ligated water and one guest water molecules. The Co(II) ion is coordinated by four nitrogen atoms belonging to four ttmb molecules and two oxygen atoms from two ligated water molecules defining a distorted CoN4O2 octahedral geometry. The Co—N bond lengths are 2.12 and 2.14 Å and the Co—O bond length is 2.09 Å. Extension of the structure through the two pairs of bisymmetric ttmb molecules results in a one-dimensional double-stranded chain running along the c direction. There exist hydrogen bonds between ligated water molecules and uncoordinated nitrogen atoms in ttmb (O1W—H1W⋯N3). These hydrogen bonds connect adjacent chains to form a 2D open bilayer structure. The 2D bilayer form channels, which are occupied by free water molecules connected by hydrogen-bonding including of O1W—H1W⋯O2W, O2W—H2W⋯N6 and O2W—H2W⋯N4. Furthermore, a wide range of 159.3–169.5° for the O—H⋯—O angles provides flexibility to the water molecules in this environment so that they can be accommodated in the channels. The adjacent 2D bilayers stack in a slightly off-set parallel fashion.

Acknowledgement

This work was supported by the Foundation of Science and Technology of Henan Province (No. 152102310348) and the Foundation of Education Committee of Henan Province (No. 15A150063 ).

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Received: 2017-2-13
Accepted: 2017-7-27
Published Online: 2017-8-18
Published in Print: 2017-9-26

©2017 Xin Ling-Yun 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 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-methanolato2O,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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