Home Crystal structure of the 2D coordination polymer poly[aqua(μ2-2,2′-(1,2-phenylene)diacetato-κ3O,O′:O′)-(μ2-4,4′-bis((1H-1,2,4-triazol-1-yl)methyl)-1,1′-biphenyl-κ2N:N′)cobalt(II)], C28H26CoN6O5
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Crystal structure of the 2D coordination polymer poly[aqua(μ2-2,2′-(1,2-phenylene)diacetato-κ3O,O′:O′)-(μ2-4,4′-bis((1H-1,2,4-triazol-1-yl)methyl)-1,1′-biphenyl-κ2N:N′)cobalt(II)], C28H26CoN6O5

  • Xin Ling-Yun , Li Yun-Ping and Liu Guang-Zhen EMAIL logo
Published/Copyright: March 8, 2018

Abstract

C28H26CoN6O5, monoclinic, P21/c (no. 14), a = 13.2393(8) Å, b = 8.6608(5) Å, c = 22.4553(12) Å, β = 91.073(2)°, V = 2574.3(3) Å3, Z = 4, Rgt(F) = 0.0327, wRref(F2) = 0.0804, T = 293(2) K.

CCDC no.:: 1824812

The asymmetric unit of the 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, pink
Size:0.35 × 0.31 × 0.26 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:0.72 mm−1
Diffractometer, scan mode:Bruker SMART, φ and ω-scans
θmax, completeness:25.4°, >99%
N(hkl)measured, N(hkl)unique, Rint:16323, 4699, 0.038
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 3577
N(param)refined:361
Programs:Bruker programs [1], SHELX [2, 3]
Table 2:

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

AtomxyzUiso*/Ueq
Co10.42169(2)−0.00080(3)0.31041(2)0.03048(10)
O10.43535(11)−0.05030(16)0.22128(6)0.0364(3)
O20.34097(12)0.14089(17)0.18354(6)0.0446(4)
O30.57726(11)0.25837(16)0.16606(6)0.0427(4)
O40.58036(11)0.43043(18)0.09544(6)0.0408(4)
O5W0.40444(11)0.23913(15)0.29330(6)0.0407(4)
H5WA0.37910.23520.25730.061*
H5WB0.46080.30900.29090.061*
N10.57931(13)0.02332(19)0.32356(7)0.0366(4)
N20.74043(15)0.0834(3)0.30574(8)0.0513(5)
N30.73292(13)0.00854(19)0.35856(8)0.0376(4)
N41.10765(13)0.5696(2)0.77934(8)0.0380(4)
N51.09534(15)0.4409(3)0.81235(9)0.0529(5)
N61.25900(13)0.50492(19)0.80771(7)0.0362(4)
C10.39275(17)0.0238(2)0.17847(9)0.0343(5)
C20.4083(2)−0.0483(3)0.11747(9)0.0538(7)
H2A0.4778−0.08280.11540.065*
H2B0.3655−0.13890.11410.065*
C30.38625(17)0.0550(2)0.06473(9)0.0369(5)
C40.29045(18)0.0508(3)0.03806(10)0.0459(6)
H40.2416−0.01470.05320.055*
C50.26695(19)0.1424(3)−0.01062(10)0.0517(7)
H50.20270.1384−0.02800.062*
C60.3385(2)0.2391(3)−0.03330(10)0.0526(7)
H60.32290.3006−0.06620.063*
C70.43258(19)0.2451(3)−0.00762(9)0.0444(6)
H70.48050.3118−0.02310.053*
C80.45836(16)0.1538(2)0.04108(8)0.0354(5)
C90.56563(17)0.1650(3)0.06586(11)0.0524(7)
H9A0.58460.06720.08390.063*
H9B0.61140.18510.03360.063*
C100.57573(15)0.2921(3)0.11189(9)0.0352(5)
C110.63822(17)−0.0273(2)0.36778(10)0.0415(6)
H110.6155−0.08100.40080.050*
C120.64607(17)0.0883(3)0.28686(10)0.0443(6)
H120.62690.13330.25080.053*
C130.82243(18)−0.0323(3)0.39433(11)0.0493(6)
H13A0.8798−0.03880.36820.059*
H13B0.8122−0.13390.41130.059*
C140.84791(16)0.0790(3)0.44417(10)0.0411(5)
C150.78959(18)0.0859(3)0.49457(11)0.0494(6)
H150.73090.02700.49630.059*
C160.81664(17)0.1779(3)0.54209(10)0.0451(6)
H160.77680.17820.57580.054*
C170.90186(16)0.2702(2)0.54089(9)0.0373(5)
C180.95840(18)0.2670(3)0.48959(10)0.0529(7)
H181.01520.32970.48700.063*
C190.93207(18)0.1725(3)0.44206(10)0.0538(6)
H190.97160.17210.40830.065*
C200.93182(16)0.3656(2)0.59330(9)0.0366(5)
C210.86153(16)0.4265(3)0.63187(10)0.0427(5)
H210.79320.40860.62450.051*
C220.89053(17)0.5130(3)0.68099(10)0.0430(6)
H220.84170.55200.70620.052*
C230.99184(17)0.5421(2)0.69304(10)0.0395(5)
C241.06258(17)0.4819(3)0.65524(11)0.0468(6)
H241.13090.49960.66300.056*
C251.03363(17)0.3959(3)0.60604(10)0.0451(6)
H251.08270.35730.58100.054*
C261.02305(18)0.6391(3)0.74612(10)0.0481(6)
H26A1.04230.74120.73260.058*
H26B0.96600.65060.77230.058*
C271.20434(17)0.6050(3)0.77703(10)0.0415(5)
H271.23030.68900.75650.050*
C281.18794(18)0.4085(3)0.82822(10)0.0486(6)
H281.20400.32410.85220.058*

Source of material

All reagents used in these syntheses were of analytical grade and used as purchased without further purification. The mixtures of 1,2-phenylenediacetic acid (phda) (0.1 mmol, 19.4 mg), 4,4′-bis((1H-1,2,4-triazol-1-yl)methyl)-1,1′-biphenyl (btmb) (0.1 mmol, 31.6 mg), Co(H3C2O2)2⋅4H2O (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. Pink crystals were obtained, and further crystals were filtered off, washed with mother liquid, and dried under ambient conditions. Yield 46%.

Experimental details

All hydrogen atoms were placed in calculated positions and refined isotropically with a 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). All calculations were performed using the SHELXL-2014/7 program package [2, 3] .

Discussion

As is known, the self-assembly of discrete coordination polymers (CPs) is highly determined by the ligand with certain features such as flexibility, appropriate angles, and versatile binding modes to coordinate to the metal ion with plastic coordination geometry [4], [5], [6]. Recently, a large number of CPs have been reported by using mixed-ligand strategy [7], [8], [9], most of which was based on the combination of metal-polycarboxylate and N-donor molecules, because this strategy can offer chance for new coordination polymers. Among them, benzene multi-carboxylates with long-spanning carboxyl groups has been used by us and others [10, 11] , making structures including helices and interpenetrating networks that may be attributed to the flexibility of carboxyl groups. At same time, the dipyridyl-type molecules are widely used coligands that can pillar polycarboxylate motifs into high dimensional structures [12], [13], [14].

The asymmetric unit of complex contains one cobalt atom, one phda anion, one btmb molecule and one ligated water molecule. Each Co atom is octahedrally coordinated by three carboxylate O donors of two symmetry-related phda anions and one coordinated water molecule in the equatorial plane with two N donors of two symmetry-related btmb ligands in the axial positions. The Co—O bond lengths are in the range of 2.0586(15)–2.1963(15) Å and the Co—N bond lengths are 2.1113(19) and 2.1508(19) Å, respectively. Both carboxylate groups of the phda ligand bridge adjacent Co(II) centers by a monodentate bridging and a bidentate chelating mode to form zigzag carboxylate chains running along the crystallographic b axis. The adjacent chains are further interconnected to each other through the btmb molecules resulting in stepwise (4,4) grids layer. Each layer is corrugated with two btmb ligands, two phda anion, and four Co atoms forming repeating rhombic grid with a side length of 5.5338(4)–17.7382(8) Å. Furthermore, the presence of coordinated water molecules leads to the formation of extensive H-bonding scheme within the layers (O(5W)–H(2W)⋯O(1)) and (O(5W)–H(1W)⋯O(2)). Interestingly, no H-bonds are observed between the layers, which stack in a slightly off-set parallel fashion and are cohered only by the van der Waals forces to complish its entire structure.

Acknowledgements

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: 2017-11-6
Accepted: 2018-2-20
Published Online: 2018-3-8
Published in Print: 2018-5-24

©2018 Xin Ling-Yun et al., published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 License.

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  51. Synthesis and crystal structure of bis(μ2-acetato-κ2O:O′)-di(ethanol)-bis{μ2-5-(N,N′-diethylamine)-5′-methoxyl-2,2′-[ethylenediyldioxybis(nitrilomethylidyne)]diphenolato-κ6O:O,N,N,O′:O′}trinickel(II) – ethanol – acetonitrile (1/2/2), C58H86Ni3N8O18
  52. Crystal structure of the bis((E)-O-ethyl-N-phenylthiocarbamate) – 4,4′-bipyridine co-crystal (2/1), C28H30N4O2S2
  53. Crystal structure of the (E)-O-methyl-N-phenyl-thiocarbamate – 4,4′-bipyridine (1/1), C18H17N3OS
  54. Crystal structure of bis(μ2-diethyldithiocarbamato-κ3S,S′:S′)-bis(tricyclohexylphosphane-κP)dicopper(I), C46H86Cu2N2P2S4
  55. Crystal structure of N-(3-chlorophenyl)ethoxycarbothioamide, C9H10ClNOS
  56. Crystal structure of bis(μ2-pyrrolidine-1-carbodithioato-κ3S,S′:S;κ3S:S:S′)-bis(tricyclohexylphosphane-P)-di-copper(I), C46H82Cu2N2P2S4
  57. Crystal structure of N-(2-chlorophenyl)methoxycarbothioamide, C8H8ClNOS
  58. Crystal structure of chlorido-methanol-(N-(2-(oxy)-3-methoxybenzylidene)pyridine-4-carbohydrazonato-κ3O,N,O′)-(4-methylphenyl)methyl-tin(IV), C23H24ClN3O4Sn
  59. Crystal structure of N-(3-chlorophenyl)(propan-2-yloxy)carbothioamide, C10H12ClNOS
  60. Crystal structure of 1-[(Z)-[4-(4-methoxyphenyl)butan-2-ylidene]amino]-3-phenylurea, C18H21N3O2
  61. A triclinic polymorph of bis(μ-N,N-bis(2-hydroxyethyl)dithiocarbamato-κ3S,S′:S′) bis(N,N-bis(2-hydroxyethyl)dithiocarbamato-κ2S:S′)zinc(II), C20H40N4O8S8Zn2
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