Home Physical Sciences Crystal structure of bis(pyridine)-bis(2-formyl-4,6-dichlorophenolato)cobalt(II), C24H16Cl4CoN2O4
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Crystal structure of bis(pyridine)-bis(2-formyl-4,6-dichlorophenolato)cobalt(II), C24H16Cl4CoN2O4

  • Qiong Su and Yan-Bin Wang EMAIL logo
Published/Copyright: July 14, 2017

Abstract

C24H16Cl4CoN2O4, triclinic, P1̄, (no. 2) a = 8.6148(13) Å, b = 12.2201(16) Å, c = 13.4807(16) Å, α = 115.198(12)°, β = 101.596(11)°, γ = 96.518(12)°, V = 1225.8(3) Å3, Z = 2, Rgt(F) = 0.0524, wRref(F2) = 0.1109, T = 173(1) K.

CCDC no.:: 1523793

The asymmetric unit of the title crystal structure is shown in the figure. Tables 1 and 2 contain details of the measurement method and a list of the atoms including atomic coordinates and displacement parameters.

Table 1

Data collection and handling.

Crystal:Violet block
Size:0.25 × 0.23 × 0.21 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:11.7 cm−1
Diffractometer, scan mode:SuperNova Dual, ω scans
2θmax, completeness:52°, >99%
N(hkl)measured, N(hkl)unique, Rint:8572, 4822, 0.044
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 3276
N(param)refined:316
Programs:SHELX [1], CrysAlisPRO [2]
Table 2

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

AtomxyzUiso*/Ueq
Co10.32944(7)0.47584(4)0.24647(4)0.02622(16)
Cl40.19575(14)0.13685(9)−0.13505(8)0.0397(3)
Cl10.39082(16)0.79832(9)0.62842(8)0.0492(3)
Cl20.86342(15)1.09512(9)0.59419(10)0.0528(3)
Cl30.78793(17)0.03394(10)−0.06078(10)0.0600(4)
O40.3144(3)0.3253(2)0.10052(19)0.0306(7)
O10.3618(3)0.6353(2)0.38993(18)0.0265(6)
O20.4366(3)0.5898(2)0.18370(19)0.0306(7)
O30.5678(3)0.4619(2)0.3077(2)0.0346(7)
N20.2276(4)0.3698(3)0.3190(2)0.0301(8)
N10.0886(4)0.4832(3)0.1736(2)0.0277(8)
C150.0240(5)0.5759(4)0.2328(3)0.0373(11)
H150.08410.63360.30640.045*
C60.5571(5)0.7703(3)0.3643(3)0.0240(9)
C70.5249(5)0.6946(3)0.2438(3)0.0301(9)
H70.57710.72880.20610.036*
C50.6773(5)0.8816(3)0.4152(3)0.0324(10)
H50.73430.90160.37120.039*
C140.4209(5)0.2647(3)0.0697(3)0.0254(9)
C90.5801(5)0.2850(3)0.1405(3)0.0266(9)
C80.6380(5)0.3844(3)0.2559(3)0.0330(10)
H80.74250.39010.29590.040*
C19−0.0022(5)0.3995(3)0.0678(3)0.0291(9)
H190.03920.33300.02550.035*
C20.5037(5)0.8271(3)0.5460(3)0.0283(9)
C10.4686(5)0.7362(3)0.4293(3)0.0240(9)
C130.3870(5)0.1653(3)−0.0440(3)0.0306(10)
C110.6469(6)0.1195(3)−0.0104(3)0.0357(10)
C40.7097(5)0.9594(3)0.5281(3)0.0313(10)
C30.6222(5)0.9339(3)0.5943(3)0.0327(10)
H30.64380.98910.67130.039*
C120.4947(6)0.0964(3)−0.0827(3)0.0357(11)
H120.46640.0337−0.15750.043*
C18−0.1538(5)0.4091(3)0.0201(3)0.0327(10)
H18−0.21280.3503−0.05350.039*
C16−0.1261(6)0.5899(4)0.1904(4)0.0452(12)
H16−0.16650.65580.23470.054*
C240.1448(6)0.2527(3)0.2521(3)0.0418(11)
H240.14450.21680.17580.050*
C100.6901(5)0.2114(3)0.0999(3)0.0352(10)
H100.79200.22540.14820.042*
C220.0597(6)0.2312(4)0.3980(4)0.0465(13)
H220.00130.18600.42460.056*
C230.0604(6)0.1820(4)0.2882(4)0.0508(13)
H230.00430.10090.23730.061*
C17−0.2173(5)0.5059(4)0.0817(3)0.0421(11)
H17−0.31920.51450.05090.051*
C200.2281(7)0.4136(4)0.4261(3)0.0648(17)
H200.28760.49390.47650.078*
C210.1461(8)0.3485(4)0.4691(4)0.077(2)
H210.15020.38480.54600.093*

Source of materials

A solution of cobalt(II) acetate tetrahydrate (0.01 mmol) in acetone (2 mL) was added dropwise to a solution of 2-formyl-4,6-dichlorophenol (0.01 mmol) in chloroform (2 mL) at room temperature. The color of the mixing solution turned to brown immediately, then 1 mL pyridine was added and stirred for 1 h at room temperature. The mixture was filtered off, and the filtrate was allowed to stand at room temperature for one week to form violet block crystals suitable for X-ray crystallographic analysis (yield 78.0%, m.p. 477–478 K). Elemental analysis- Anal. calcd. for C24H16Cl4CoN2O4: C, 48.27%; H, 2.70%; N, 4.69%; Co, 9.87%; Found: C, 48.31%; H, 2.68%; N, 4.72%; Co, 9.89%.

Experimental details

Hydrogen atoms were placed in their geometrically idealized positions and constrained to ride on their parent atoms.

Comment

Salicylaldehyde derivatives play an important role in the modern coordination chemistry [3], [4], [5], [6], [7]. In general, they can act as bridging bidentate ligands via the phenolic oxygen and formyl group oxygen atoms to build coordination networks [8] as well as interlink the one-dimensional or two-dimensional molecules into frameworks via the hydrogen bonds [9], [10] or π-π stacking interactions [11], [12], [13].

The title compound consists of a mononuclear cobalt(II) complex. The Co centre is hexa-coordinated with a distorted octahedral geometry. Bond lengths and angles are in the expected ranges.

References

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Received: 2017-1-3
Accepted: 2017-6-16
Published Online: 2017-7-14
Published in Print: 2017-9-26

©2017 Qiong Su et al., published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

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