Home The crystal structure of catena-poly[oktaaqua-bis(μ2-4,4′-ethene-1,2-diyldipyridine-κ2N:N′)-(μ2-3,3′-(1-oxidodiazene-1,2-diyl)diphthalato-κ2O:O′)dicobalt(II)] dihydrate, C28H36N4O19Co2
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The crystal structure of catena-poly[oktaaqua-bis(μ2-4,4′-ethene-1,2-diyldipyridine-κ2N:N′)-(μ2-3,3′-(1-oxidodiazene-1,2-diyl)diphthalato-κ2O:O′)dicobalt(II)] dihydrate, C28H36N4O19Co2

  • Xun Feng ORCID logo EMAIL logo , Nan Chen , Zhengtao Zhang , Jingjing Yu and Yiming Zhang
Published/Copyright: April 30, 2020

Abstract

C28H36N4O19Co2, triclinic, P1̄ (no. 2), a = 7.4890(5) Å, b = 8.8913(4) Å, c = 13.5918(7) Å, α = 88.027(4)°, β = 89.819(5)°, γ = 69.729(5)°, V = 848.44(9) Å3, Z = 1, Rgt(F) = 0.0435, wRref(F2) = 0.1015, T = 293(2) K.

CCDC no.: 1996977

Table 1 contains crystallographic data and Table 2 contains the list of the atoms including atomic coordinates and displacement parameters.

Table 1:

Data collection and handling.

Crystal:Pink block
Size:0.21 × 0.20 × 0.19 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:1.07 mm−1
Diffractometer, scan mode:SuperNova, ω
θmax, completeness:28.2°, >99%
N(hkl)measured, N(hkl)unique, Rint:6761, 3524, 0.026
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 3015
N(param)refined:244
Programs:Olex2 [1], SHELX [2], [3]
Table 2:

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

AtomxyzUiso*/Ueq
Co010.79678(5)0.25430(4)0.83930(3)0.02189(13)
O1a0.5930(7)0.6200(6)0.5629(4)0.0519(13)
O20.5961(3)0.3981(2)0.74286(14)0.0269(5)
O30.5433(3)0.6496(2)0.78887(15)0.0342(5)
O100.7322(3)0.0462(2)0.81323(15)0.0321(5)
H10A0.65290.04430.85650.048*
H10B0.8066−0.05310.81660.048*
O40.2486(3)0.5537(3)0.90275(14)0.0372(5)
O5−0.0067(3)0.7712(3)0.88220(15)0.0425(6)
O60.8503(3)0.4586(2)0.89022(15)0.0324(5)
H6A0.76460.53890.86230.049*
H6B0.80300.48040.94770.049*
O70.5761(3)0.2994(3)0.95033(16)0.0393(5)
H7A0.63030.32631.00250.059*
H7B0.49260.39220.93940.059*
O81.0152(3)0.1283(2)0.94013(14)0.0325(5)
H8A1.11990.08950.90930.049*
H8B1.04390.15330.99420.049*
O90.4199(4)0.9430(3)0.88965(18)0.0516(7)
H9A0.43970.86630.93210.077*
H9B0.42320.88460.83990.077*
N10.4881(4)0.5473(3)0.53571(16)0.0264(5)
N21.0146(3)0.1886(3)0.73295(16)0.0235(5)
C10.3089(4)0.5856(3)0.58647(19)0.0234(6)
C20.3122(4)0.5959(3)0.68920(19)0.0203(6)
C30.1387(4)0.6457(3)0.73878(19)0.0219(6)
C4−0.0314(4)0.6832(3)0.6858(2)0.0272(6)
H4−0.14670.71610.71890.033*
C5−0.0301(5)0.6718(4)0.5846(2)0.0321(7)
H5−0.14430.69660.55020.038*
C60.1396(4)0.6240(3)0.5345(2)0.0289(7)
H60.14020.61750.46640.035*
C70.4995(4)0.5463(3)0.74481(19)0.0213(6)
C80.1282(4)0.6569(3)0.8495(2)0.0257(6)
C91.0299(4)0.0785(4)0.6646(2)0.0296(7)
H90.93240.03680.65960.035*
C101.1815(5)0.0246(4)0.6020(2)0.0324(7)
H101.1862−0.05310.55710.039*
C111.3288(4)0.0871(3)0.6061(2)0.0269(6)
C121.3128(4)0.2005(3)0.6768(2)0.0283(7)
H121.40740.24520.68300.034*
C131.1574(4)0.2464(3)0.7373(2)0.0283(7)
H131.15090.32200.78400.034*
C141.4907(5)0.0422(4)0.5402(2)0.0337(7)
H141.59120.07610.55590.040*
  1. aOccupancy: 0.5.

Source of material

The organic compound oxide azobenzene 2,2′,3,3′-tetracarboxyl acid (abbreviated as H4Oobtc) was synthesized with the help of Jinan Camolai Trading Company of Shandong, China, and 1,2-bis(4-pyridine) ethylene (abbreviated as bpe) was purchased from TCI chemicals. In a representative experiment, Co(CH3COO)2⋅4 H2O (0.2 mmol, 0.049 g), H4Oobtc acid (0.1 mmol, 0.038 g) and bpe (0.1 mmol, 0.019 g) were mixed and dissolved in 30 mL aqueous solution of ethanol-water (V/V = 1 : 1) and then the mixture was adjusted to neutral with KOH (0.2 mol L−1). The solution was filtered after being stirred for 12 h at 120 °C. Two weeks later, pink block crystals of the title compound were obtained by the solvent evaporation approach. Yield: 31 mg (34% based on cobalt element). Elemental analysis (%) for C28H36N4O19Co2 (calcd. C 39.54, H 4.27, N 6.59; Found C 39.39, H 4.34, N 6.49. IR (KBr pellet, cm−1): 3421(s), 3360(s), 1624 (s), 1439(s), 1325(s), 1023(m), 902(s), 857(s), 750(m).

Experimental details

Coordinates of hydrogen atoms were added at calculated positions. Their Uiso values were set to 1.2Ueq of the parent atoms. The atom O1 is half occupied to model a 1/1 disordered 3,3′-(1-oxidodiazene-1,2-diyl)diphthalate (Oaobtc).

Comment

Transition metal coordination polymers (CPs) have attracted great attention due to their intriguing architectures and potential applications. Among the organic linkers, polycarboxylic acids/polycarboxylates can bind several metal centers with specific coordination geometry to construct clusters and construct one to three dimensional compounds with interesting properties [4], [5], [6]. The chemical modified ligands, such as organic compounds containing an azo (—N=N—) group as light-harvesting chromophore are employed to enhance/reduce the light adsorption [7]. Synthesis, structural and magnetic studies of azido, and hydroxyl, chloride bridged Co(II) complexes have been used as models to understand the electron/charge transfer processes [8]. However, only a limited number of one dimensional cobalt coordination compounds based on multi-carboxylates have been characterized structurally. On the other hand, 1,2-bis(4-pyridine)ethylene (abbreviated as bpe) as a rigid N donor ligand has been proved to be a good candidate used as linker constructing coordination polymers in the field of potential functional materials [9]. In order to further study the coordination behavior and role of bpe in the self assembly processes [10] in the presence of substituted aromatic-heterocyclic acid, and to identify compounds that exhibit similar behavior as the 1D chain structure was associated with some moieties.

The asymmetric unit of title structure contains one Co(II), one half of a Oaobtc and one half of a bpe. As illustrated in the left part of the figure, cobalt(II) ion adopts six coordination fashions, showing a pseudo octahedral geometry with a N1O5 donor set around it. Among the donor set, the O6, O8 and O10 atoms from terminal H2O ligands, and another oxygen atoms of carboxylate moieties from Oaobtc, are located in equatorial plane. The N2 atom from bridging bpe and one O7 atom derivated from a coordinated water are located in axis positions, completing the octahedron coordination geometry. All four carboxylate groups Oaobtc link two adjacent Co(II) in mono dentate mode, in an anti-anti fashion. This coordination fashion is essentially different from the either transition metal complexes based on azobenzenetetracarboxylic acid and bis(imidazole) ligand [11] or the lanthanide complexes based azobenzenetetracarboxylic acid and DMF [12]. The average Co–O distances range from 2.0440(19) to 2.176(2) Å, while, bond Co–N distance is 2.115(2) Å, which are in the expected ranges [13], [14]. The bond angle involving Co(II) ranges from 83.51(8) to 173.40(7)°.

The ancillary ligand bpe links neighboring [Co(Oaobtc)H2O] units, with the Co⋯Co separation of 13.682 Å; Oaobtc and bpe ligands connect the [Co(H2O)4] units alternately into one-dimensional zigzag chains along the crystallographic bc plane (right part of the figure). In such a manner, fence-like bump stagger chain with water arms are generated, as displayed in right half of figure. Close inspection finds that there are strong hydrogen bond interactions between the oxygen atoms of carboxylates water. They are listed as follow, O10⋯H10B-O5 #1,#[O1-O5#1 = 2.687(3) Å, O1-H1⋯N1 = 151.6°], O3⋯H6A-O6, [O3-O6 = 2.687(3) Å, O3⋯H6A-O6 = 157.5°], O7⋯H7B-O4, [O7-O4 = 2.759(3) Å, O7⋯H7B-O4 = 158.8°], O8⋯H8B-O5 #2 , [O8⋯O5 #2 = 2.596(3) Å, O8⋯H8B-O5 #2 = 157.3°], O9⋯H9B-O3, [O9⋯O3 = 2.846(3) Å, O9⋯H9B-O3 = 143.2°]. Symmetry codes are #1 1 + X, −1 + Y, +Z; #2 1 − X, 1 − Y, 2 − Z. These hydrogen bonding parameters excellently reflect the hydrogen bond interactions contributing to packing crystal.

Acknowledgements

This work was supported by the National Natural Science Foundation of China (No. U1804131), and Natural Science Foundation of Henan Province, China, (Nos.182102310909 and 182102310897).

References

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Received: 2020-02-23
Accepted: 2020-04-15
Published Online: 2020-04-30
Published in Print: 2020-06-25

©2020 Xun Feng et al., published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution 4.0 Public License.

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  55. The crystal structure of 8-((4-chlorophenylamino)methylene)-6,10-dioxaspiro[4.5]decane-7,9-dione, C15H14ClNO4
  56. The crystal structure of catena-poly[oktaaqua-bis(μ2-4,4′-ethene-1,2-diyldipyridine-κ2N:N′)-(μ2-3,3′-(1-oxidodiazene-1,2-diyl)diphthalato-κ2O:O′)dicobalt(II)] dihydrate, C28H36N4O19Co2
  57. Crystal structure of (E)-1-(2-cyano-3-oxo-1-phenylprop-1-en-1-yl)-3,7-diphenylindolizine-6-carbonitrile, C31H19N3O
  58. Crystal structure of 1,1′-bis(diphenylphosphino)ferrocene-(1,1′-bis(diphenylphosphino)ferrocene-κ2P,P′)-(O-isobutyl sulfurodithioito-κ2S,S′)copper(I), C39H37CuFeOP2S2
  59. Crystal structure of poly[(5-bimethylamino-1-naphthalenesulfonato-κO)-(μ3-hexamethylenetetramino-κ3N:N′:N′′)silver(I)] dihydrate, C36H52Ag2N10O8S2
  60. Crystal structure of poly[μ2-diaqua-(μ2-2-amino-4,5-dicyano-κ2N:N′-imidazol-1-ide)sodium(I)], C5H6N5O2Na
  61. Crystal structure of (1,3-propanediamine-κ2N,N′)(N-(3-aminopropyl)-α-methyl aspartato-κ4N,N′,O,O′)cobalt(III) chloride, C11H24ClCoN4O4
  62. Crystal structure and anti-inflammatory activity of (3E,5E)-3,5-bis(4-fluorobenzylidene)-1-((4-fluorophenyl)sulfonyl)piperidin-4-one-dichloromethane (1/1), C26H20Cl2F3NO3S
  63. Crystal structure of (S)-(+)-1-cyclohexylethylaminium chloride, C8H18NCl
  64. The crystal structure of tris(nitrato-κ2O,O′)-bis(4,4,5,5-tetramethyl-2-(o-pyridyl)imidazoline-1-oxyl 3-oxide-κ2N,O)yttrium(III), C24H32N9O13Y
  65. Hydrogen bonding versus packing effects in the crystal structure of 3-((1R,2S)-1-methylpyrrolidin-1-ium-2-yl)pyridin-1-ium tetraiodidozincate(II), C10H16I4ZnN2
  66. Dimerization of 2-[(2-((2-aminophenyl)thio)phenyl)amino]-cyclohepta-2,4,6-trien-1-one through hydrogen bonding, C19H16N2OS
  67. Crystal structure of 1-(4-chloro-phenyl)-7-ethoxyl-6,8-difluoro-4-oxo-1,4-dihydro-quinoline-3-carboxylic acid, C18H12ClF2NO4
  68. Crystal structure of 7-ethoxy-6,8-difluoro-4-oxo-1-pyridin-2-ylmethyl-1,4-dihydro-quinoline-3-carboxylic acid, C18H14F2N2O4
  69. Crystal structure of octahydro-7aR,8′R-dimethylspiro[isobenzofuran-4(1H), 4′ (3′H)-[1H-7,9a]methanocyclohepta[c]pyran]-1′,3, 9′ (3aH,4′aH)-trione, C20H26O5
  70. Crystal structure of bis(5-ethoxy-2-(((1-hydroxy-2-methyl-3-oxidopropan-2-yl)imino)methyl)phenolato-κ3N,O,O’)manganese(IV) – methanol (1/1), C27H38MnN2O9
  71. Crystal structure of 8a,8a′′-oxybis(8aH-8,9-dioxa-3a1λ4-aza-8aλ4-borabenzo[fg]tetracene), C34H22B2N2O5
  72. Crystal structure of bromido-triphenyl-(triphenylarsine oxide-κO)tin(IV), C36H30AsBrOSn
  73. Crystal structure of catena-poly[chlorido-(μ2-formato-κ2O:O′)-(1,10-phenathroline-κ2N,N′)copper(II)], C26H18Cl2Cu2N4O4
  74. The crystal structure of poly[(μ10-5-carboxyisophthalato-κ10O)disodium], C9H4Na2O6
  75. The crystal structure of 3,5-difluoroisonicotinic acid, C6H3F2NO2
  76. The crystal structure of ethyl-1-(N-(adamantan-1-yl)-carbamothioyl)piperidine-4-carboxylate, C19H30N2O2S
  77. Crystal structure of 5-methyl-3-phenyl-1-tosyl-1,2,3,4-tetrahydropyridine, C19H21NO2S
  78. Crystal structure of bis((3-chlorosalicylidene)-ethylenediaminato-κ4N,N′,O,O′)nickel (II), C16H12Cl2NiN2O2
  79. Crystal structure of (E)-N′-(2-chloro-6-hydroxybenzylidene)-4-hydroxybenzohydrazide — dihydrofuran-2(3H)-one (1/1), C18H17ClN2O5
  80. Crystal structure of bis((3-bromosalicylidene)-ethylenediaminato-κ4N,N′,O,O′) nickel (II), C16H12Br2NiN2O2
  81. Crystal structure of trimethylsulfoxonium tetrachloridocobaltate(II) [(CH3)3SO]2CoCl4
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