Home The crystal structure of bis(μ2-5-chloro-N-(2-methyl-1-oxidopropylidene)-2-oxidobenzohydrazonate-κ5N,O,O′:N′,O′′)pentakis(pyridine-κ1N)tricopper(II), C47H45Cl2N9Cu3O6
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The crystal structure of bis(μ2-5-chloro-N-(2-methyl-1-oxidopropylidene)-2-oxidobenzohydrazonate-κ5N,O,O′:N′,O′′)pentakis(pyridine-κ1N)tricopper(II), C47H45Cl2N9Cu3O6

  • Yang Liguo ORCID logo EMAIL logo , Zhang Chaoyang , Wang Kai , Zhai Shengxian ORCID logo and Liu Nana
Published/Copyright: February 12, 2021

Abstract

C47H45Cl2N9Cu3O6, monoclinic, C2/c (no. 15), a = 24.084(9) Å, b = 12.152(5) Å, c = 17.404(7) Å, β = 109.984(4)°, V = 4787(3) Å3, Z = 4, Rgt(F) = 0.0455, wRref(F2) = 0.1363, T = 298 K.

CCDC no.: 2057941

The molecular structure is shown in the Figure. 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:Yellow block
Size:0.08 × 0.06 × 0.03 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:1.49 mm−1
Diffractometer, scan mode:Bruker APEX-II, φ and ω
θmax, completeness:25.0°, >99%
N(hkl)measured, N(hkl)unique, Rint:26,523, 4198, 0.085
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 3394
N(param)refined:306
Programs:Bruker [1], SHELX [2], [, 3]
Table 2:

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

AtomxyzUiso*/Ueq
Cu10.50000.79108 (5)0.25000.03580 (18)
Cu20.36073 (2)0.80720 (4)0.37855 (2)0.04015 (17)
Cl10.65323 (4)0.92636 (9)0.66705 (6)0.0608 (3)
O10.52885 (10)0.8181 (2)0.36925 (14)0.0441 (6)
O20.40102 (10)0.8365 (2)0.49188 (14)0.0500 (6)
O30.32620 (10)0.7873 (2)0.25903 (14)0.0449 (6)
N10.28051 (12)0.8209 (2)0.39057 (17)0.0404 (6)
N20.42327 (11)0.7972 (2)0.26899 (16)0.0331 (6)
N30.43176 (11)0.8152 (2)0.35292 (16)0.0338 (6)
N40.50000.5938 (4)0.25000.0482 (10)
N50.36530 (15)0.5991 (3)0.3945 (2)0.0564 (8)
C10.45822 (14)0.8552 (3)0.52629 (19)0.0390 (7)
C20.57809 (15)0.8991 (3)0.6137 (2)0.0431 (8)
C30.53756 (17)0.9051 (3)0.6534 (2)0.0487 (9)
H10.54950.92340.70860.058*
C40.47916 (16)0.8836 (3)0.6103 (2)0.0482 (9)
H20.45210.88800.63760.058*
C50.48689 (13)0.8262 (3)0.39902 (19)0.0346 (7)
C60.56057 (14)0.8730 (3)0.53209 (19)0.0399 (7)
H30.58850.87030.50620.048*
C70.27292 (16)0.8784(3)0.4520 (2)0.0497 (9)
H40.30520.91450.48860.060*
C80.50107 (14)0.8504 (3)0.48715 (19)0.0354 (7)
C90.21897 (18)0.8858 (4)0.4627 (3)0.0584 (10)
H50.21520.92640.50590.070*
C100.36667 (14)0.7839 (3)0.2260 (2)0.0375 (7)
C110.23307 (16)0.7723 (4)0.3378 (2)0.0538 (10)
H60.23730.73460.29360.065*
C120.34836 (15)0.7644 (4)0.1358 (2)0.0497 (9)
H70.38310.74070.12300.060*
C130.17097 (18)0.8331 (4)0.4095 (3)0.0696 (12)
H80.13430.83600.41630.084*
C140.4039 (2)0.5553 (4)0.4601 (3)0.0705 (12)
H90.43250.60080.49520.085*
C150.3264 (2)0.8737 (5)0.0916 (3)0.0791 (14)
H10A0.29290.89900.10460.119*
H10B0.31510.86290.03360.119*
H10C0.35740.92740.10890.119*
C160.17845 (18)0.7755 (5)0.3456 (3)0.0721 (13)
H110.14670.73910.30810.087*
C170.3023 (2)0.6751 (5)0.1093 (3)0.0823 (16)
H12D0.31790.60830.13800.123*
H12G0.29170.66310.05150.123*
H12J0.26790.69700.12150.123*
C180.4724 (2)0.5355 (4)0.2907 (3)0.0695 (12)
H130.45210.57360.31920.083*
C190.3256 (2)0.5334 (4)0.3451 (3)0.0697 (12)
H140.29930.56360.29750.084*
C200.50000.3652 (6)0.25000.089 (2)
H150.50000.28870.25000.107*
C210.3205 (3)0.4237 (5)0.3587 (4)0.0900 (17)
H160.29050.38150.32280.108*
C220.3599 (4)0.3789 (5)0.4253 (5)0.106 (2)
H170.35810.30420.43570.127*
C230.4720 (3)0.4230 (4)0.2932 (4)0.0884 (16)
H280.45290.38640.32390.106*
C240.4043 (3)0.4446 (6)0.4797 (4)0.0967 (19)
H190.43230.41530.52630.116*

Source of material

The N-(5-chloro-acetylsalicyloylhydrazine) was synthesized according to reference [4]. A mixture of N-(5-chloro-acetylsalicyloylhydrazine) (0.196 g, 1 mmol) and acetate copper (0.186 g, 1 mmol) in 10 ml methanol was stirred at room temperature for 1 h. The mixture was filtered to remove impurties, and then left at room temperature. After a few days, yellow block crystals had formed. Yield (0.13 g, 43%).

Experimental details

The H atoms were geometrically placed (C—H = 0.95–0.98 Å) and refined as riding with Uiso(H) = 1.2–1.5 Ueq(C). The N-bound H atoms were located in a difference Fourier map but were refined with a distance restraint of N—H = 0.88 ± 0.01 Å, and with Uiso(H) set to 1.2 Ueq(N) [1], [2], [3].

Comment

Multidenate ligands have been synthesized in recent years for the polynuclear metal complexes [4], [5]. The N atoms and O atoms can coordinated with the transition metals and rare earth metals, so lots of the polynuclear metal complexes can be producted. The magnetic properties of the polynuclear metal complexes have been studied, which have good magnetic properties [6], [7], [8]. So lots of the polynuclear metal complexes were producted [9], [10]. In this paper, one new Cu is described and the structure is similar to reference [8].

The title compound crystallizes in the monoclinic space group C2/c with one half of the complex in the asymmetric unit. The bond lengths of Cu–O are 1.978, 1.911 and 1.974 Å, the bond lengths of Cu–N are 1.987, 2.397, 1.912 and 2.020 Å, respectively. The bond lengths of Cu–N from the pyridine ligands are longer than the other Cu–N bond lengths, which are similar with the reference [8]. Each copper coordination environment in the complex exhibits a distorted pyramidal geometry. The trinuclear complex is centrosymmetric.


Corresponding author: Yang Liguo, College of Chemistry and Environmental Engineering, Anyang Institute of Technology, Anyang455000, Henan, P. R. China, E-mail:

Funding source: Natural Science Foundation of Henan Province of China

Award Identifier / Grant number: 202300410010

Funding source: Research Fund of Anyang Institute of Technology

Award Identifier / Grant number: YPY2019011

Award Identifier / Grant number: YPY2020025

Funding source: Anyang Institute of Technology

  1. Author contributions: All the authors have accepted responsibility for the entire content of this submitted manuscript and approved submission.

  2. Research funding: Natural Science Foundation of Henan Province of China (No. 202300410010), Research Fund of Anyang Institute of Technology (Nos. YPY2019011, YPY2020025), Key discipline of environmental engineer of Anyang Institute of Technology.

  3. Conflict of interest statement: The authors declare no conflicts of interest regarding this article.

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Received: 2020-11-16
Accepted: 2021-01-22
Published Online: 2021-02-12
Published in Print: 2021-05-26

© 2020 Yang Liguo et al., published by De Gruyter, Berlin/Boston

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

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