Home Crystal structure of catena-poly[diaqua-bis(μ2-3,5-di(1H-1,2,4-triazol-1-yl)benzoate-κ2N:N′)cobalt(II))] 2.5 hydrate, C22H23CoN12O8.50
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Crystal structure of catena-poly[diaqua-bis(μ2-3,5-di(1H-1,2,4-triazol-1-yl)benzoate-κ2N:N′)cobalt(II))] 2.5 hydrate, C22H23CoN12O8.50

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Published/Copyright: August 13, 2018

Abstract

C22H23CoN12O8.50, triclinic, P1̄ (no. 2), a = 9.6549(3) Å, b = 10.6027(4) Å, c = 13.4938(4) Å, α = 100.824(3)°, β = 99.707(3)°, γ = 96.642(3)°, V = 1321.76(8) Å3, Z = 2, Rgt(F) = 0.0366, wRref(F2) = 0.0914, T = 288.03(10) K.

CCDC no.: 1858180

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:Clear light pink block
Size:0.27 × 0.21 × 0.15 mm
Wavelength:Mo radiation (0.71073 Å)
μ:0.73 mm−1
Diffractometer, scan mode:SuperNova, φ and ω
θmax, completeness:25.5°, 99%
N(hkl)measured, N(hkl)unique, Rint:14128, 4844, 0.028
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 4245
N(param)refined:412
Programs:CrysAlisPRO [1], SHELX [2, 3]
Table 2:

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

AtomxyzUiso*/Ueq
Co010.50001.00001.00000.01936(12)
Co021.00000.50000.50000.01942(12)
O10.8678(2)0.32659(17)1.20232(13)0.0390(5)
O2a1.0096(6)0.2309(5)1.1044(4)0.0367(9)
O2Ab0.9388(6)0.1854(5)1.0895(4)0.0367(9)
O30.32773(19)0.89171(18)0.22653(13)0.0358(4)
O40.2417(2)1.03115(17)0.33668(13)0.0382(4)
O50.68976(17)1.02834(16)0.94737(12)0.0301(4)
H5A0.74821.09000.98960.045*
H5B0.67491.05660.89150.045*
O61.03655(18)0.67644(15)0.60434(12)0.0308(4)
H6A1.01420.73570.57290.046*
H6B1.12530.69770.62780.046*
O70.0488(3)1.1038(2)0.44923(19)0.0608(6)
H7A−0.02611.04820.43680.091*
H7B0.10821.07410.41470.091*
O80.2284(2)1.23730(19)0.24516(16)0.0502(5)
H8A0.23731.17040.27040.075*
H8B0.14861.22550.20430.075*
N10.6489(2)0.63604(18)1.00752(14)0.0234(4)
N20.5733(2)0.63768(19)1.08453(15)0.0300(5)
N30.5464(2)0.80891(18)1.01085(15)0.0246(4)
N40.8938(2)0.38858(17)0.77082(14)0.0219(4)
N50.9699(2)0.29075(19)0.74506(16)0.0322(5)
N60.9464(2)0.40871(18)0.62279(14)0.0246(4)
N70.3624(2)0.88666(18)0.67502(14)0.0238(4)
N80.2540(2)0.9546(2)0.69348(16)0.0337(5)
N90.3917(2)0.94110(18)0.84193(14)0.0251(4)
N100.5937(2)0.62392(18)0.43906(14)0.0248(4)
N110.5815(2)0.5432(2)0.34465(15)0.0322(5)
N120.7849(2)0.53384(18)0.45077(15)0.0252(4)
C10.7313(2)0.5351(2)0.98384(17)0.0215(5)
C20.7654(2)0.5079(2)0.88717(17)0.0224(5)
H20.73320.55280.83700.027*
C30.8490(2)0.4117(2)0.86740(17)0.0211(5)
C40.8922(2)0.3403(2)0.93998(17)0.0226(5)
H40.94660.27490.92500.027*
C50.8533(2)0.3677(2)1.03540(17)0.0233(5)
C60.7742(2)0.4670(2)1.05818(17)0.0235(5)
H60.75060.48741.12270.028*
C70.6313(3)0.7386(2)0.96515(18)0.0258(5)
H70.67270.75780.91130.031*
C80.5141(3)0.7425(2)1.08300(18)0.0276(5)
H80.45470.76941.12770.033*
C90.8823(3)0.4569(2)0.69663(17)0.0256(5)
H90.83530.52880.69730.031*
C100.9978(3)0.3065(2)0.65592(19)0.0297(6)
H101.04860.25230.61850.036*
C110.9023(3)0.2952(2)1.11814(18)0.0299(6)
C120.3850(2)0.8441(2)0.57319(16)0.0213(5)
C130.4696(2)0.7488(2)0.55503(17)0.0239(5)
H130.50760.70960.60740.029*
C140.4963(2)0.7136(2)0.45687(17)0.0221(5)
C150.4391(2)0.7693(2)0.37761(18)0.0239(5)
H150.45730.74330.31190.029*
C160.3540(2)0.8648(2)0.39733(17)0.0217(5)
C170.3276(2)0.9030(2)0.49574(17)0.0228(5)
H170.27180.96750.50950.027*
C180.4417(2)0.8808(2)0.76462(17)0.0256(5)
H180.52170.83960.77140.031*
C190.2761(3)0.9841(3)0.79417(19)0.0323(6)
H190.21751.03060.83010.039*
C200.3017(2)0.9342(2)0.31297(18)0.0243(5)
C210.7151(2)0.6167(2)0.49999(18)0.0250(5)
H210.74600.66320.56740.030*
C220.6992(3)0.4920(2)0.35664(19)0.0294(5)
H220.72200.43170.30470.035*
O9c0.9241(4)−0.0389(4)1.0463(3)0.0482(10)
H9Ac0.9693−0.07141.00130.072*
H9Bc0.94770.04231.04910.072*
  1. aOccupancy: 0.517(5), bOccupancy: 0.483(5), cOccupancy: 0.5.

Source of material

The title compound was prepared by hydrothermal method. A mixture of Co(OAc)2 ⋅ 4 H2O (0.049 g, 0.2 mmol), 3,5-di(1,2,4-triazole-4)benzenecarboxylic acid (0.0256 g, 0.1 mmol), and H2O (10 mL) was sealed in a 25 mL Teflon-lined stainless steel vessel and heated at 160 °C for 4 days. The reaction mixture was slowly cooled to room temperature at a rate of 5 °C/h, and the red block crystals were collected, washed with water, and dried in air.

Experimental details

The hydrogen atoms were assigned with common isotropic displacement factors Uiso(H) = 1.2 times Ueq (C, aromatic ring), and Uiso(H) = 1.5 times Ueq(O, water). The final refinement by using geometrical restraints, with C—H = 0.93 Å (aromatic ring), and O—H = 0.85 Å (water).

Comment

Coordination polymer (CPs) or organic-inorganic hybrid materials, constructed by inorganic secondary building units and organic bridging ligands has taken wide attention owing to their intriguing structural as well as distinctive properties such as catalytic, luminescence, gas adsorption, and magnetism [4], [5], [6]. It is well known that the structures and properties of the CPs are strongly dependent on the organic ligands and the metal ions [7]. Bifunctional ligands containing carboxylate groups and nitrogen donors have attracted great interests in construction of CPs [8].

The asymmetric unit of the title compound consists of two-half Co(II) ions, two 3,5-di(1,2,4-triazole-4)benzenecarboxylic acid anions (L), two coordinated water molecules and two and a half lattice water molecules (Figure). The two Co1 centers are both six-coordinated with slightly distorted octahedral geometry. The coordinations are completed by four nitrogen atoms from four different L anions, and two oxygen atoms from coordinated water molecules. The Co—N bond lengths are in the range of 2.1506(18)–2.1737(18) Å, and the Co—O bond lengths are 2.0840(16) and 2.0728(16) Å, respectively. In the title compound, each L ligand coordinated to two center Co(II) ions by two nitrogen atoms. Thus adjacent Co(II) ions are connected into 1D chain structure. The carboxyl group of L did not participate in the coordination.

References

Agilent Technologies: CrysAlisPRO Software System, Agilent Technologies UK Ltd, Oxford, UK (2011).Search in Google Scholar

Sheldrick, G. M.: SHELXS97. Program for the solution of crystal structures. University of Göttingen, Germany (1997).Search in Google Scholar

Sheldrick, G. M.: SHELXTL. Structure determination software suite. Version 5.10. Bruker AXS, Madison, WI, USA (1998).Search in Google Scholar

Janiak, C.: Engineering coordination polymers towards applications. Dalton Trans. 14 (2003) 2781–2804.10.1039/b305705bSearch in Google Scholar

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Received: 2018-03-24
Accepted: 2018-07-25
Published Online: 2018-08-13
Published in Print: 2018-11-27

©2018 Hong-Hong Lan, published by De Gruyter, Berlin/Boston

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

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  1. Cover and Frontmatter
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