Startseite The crystal structure of bis(2-benzoyl-5-hydroxylphenolato-κ2O,O′)copper(II), C26H18CuO6
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The crystal structure of bis(2-benzoyl-5-hydroxylphenolato-κ2O,O′)copper(II), C26H18CuO6

  • Hui Wang und Zi-Jing Xiao EMAIL logo
Veröffentlicht/Copyright: 16. November 2017

Abstract

Cu(C13H9O3)2, tetragonal, I41/a (no. 88), a = 14.2364(4) Å, c = 20.5410(7) Å, V = 4163.1(3) Å3, Z = 8, Rgt(F) = 0.0482, wRref(F2) = 0.1476, T = 293 K.

CCDC no.:: 1562796

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:Block, dark green
Size:0.25 × 0.20 × 0.12 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:1.09 mm−1
Diffractometer, scan mode:Enhance (Mo) X-ray Source, ω-scans
2θmax, completeness:26°, >99%
N(hkl)measured, N(hkl)unique, Rint:4426, 2054, 0.021
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 1548
N(param)refined:125
Programs:CrysAlisPRO [1], SHELX [2], Diamond [3]
Table 2:

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

AtomxyzUiso*/Ueq
Cu10.00000.50000.00000.0439(3)
O10.03142(19)0.44901(18)−0.08451(11)0.0473(6)
O20.07890(19)0.41312(17)0.04231(10)0.0446(6)
O30.2021(2)0.11152(18)0.08325(12)0.0519(7)
H30.18860.13080.12080.057(12)*
C10.1074(3)0.3697(3)−0.16793(15)0.0437(9)
C20.2011(4)0.3657(4)−0.1858(2)0.0786(15)
H2A0.24780.3622−0.15410.094*
C30.2250(5)0.3668(5)−0.2518(3)0.098(2)
H3A0.28790.3686−0.26410.117*
C40.1566(5)0.3652(4)−0.2981(2)0.0873(18)
H4A0.17280.3631−0.34200.105*
C50.0655(5)0.3667(4)−0.2805(2)0.0869(18)
H5A0.01910.3650−0.31230.104*
C60.0402(4)0.3708(4)−0.21479(19)0.0666(13)
H6A−0.02290.3743−0.20320.080*
C70.0813(3)0.3796(3)−0.09734(16)0.0396(8)
C80.1129(2)0.3128(2)−0.05008(15)0.0373(8)
C90.1077(2)0.3316(2)0.01821(15)0.0367(8)
C100.1369(2)0.2626(3)0.06196(16)0.0400(8)
H10A0.13330.27470.10640.048*
C110.1705(2)0.1777(2)0.04132(16)0.0399(8)
C120.1743(3)0.1564(3)−0.02592(17)0.0456(9)
H12A0.19500.0979−0.04020.055*
C130.1469(3)0.2232(3)−0.06933(16)0.0448(9)
H13A0.15050.2096−0.11350.054*

Source of materials

2,4-dihydroxylbenzophenone (0.0214 g; 0.1 mmol) dissolved in N,N-dimethylformamide (5 mL) was treated with a small amount of an aqueous NaOH solution. Under continuous stirring, Cu(NO3)2⋅H2O (0.0242 g; 0.1 mmol) disolved in 5 mL water was added to get the resulting green solution. After 14 days, the dark green block crystals of the title complex were obtained by slow evaporation at room temperature.

Experimental details

All the H atoms attached to carbons were placed at calculated positions (0.93 Å) and included in the refinement in the riding model approximation, with Uiso(H) set to 1.2Ueq(C). The hydrogen atom of O—H was located from the difference-Fourier map, fixed and its Uiso parameter was refined.

Comment

Supramolecular features are of interest as they may lead to well-defined bulk materials in energy [4], optics [5], molecular devices [6] etc. In supramolecular systems, inter/intramolecular interactions play a vital role in the self assembly of architecture blocks, including hydrogen bonding, ionic aggregation, guest/host interactions and π-π stacking. As one of the most abundant non-covalent interactions, the hydrogen bond is of current interest [7].

As shown in the figure, the title complex contains one Cu(II) atom and two 2-benzoyl-5-hydroxylphenolato ligands. The copper center is four-coordinated by two carbonyl O atoms (O(1), O(1a)) and two hydroxyl O atoms (O(2), O(2a)) (the symmetry code: a: −x, −y + 1, −z). The Cu-O bond lengths are 1.934(2) Å (carbonyl) and 1.883(2) Å (hydroxyl), respectively. The Cu-O bond length (1.934 Å, carbonyl) is identical to the corresponding Cu(II)-O(carbonyl) (1.934(7) Å) in [Cu(LFQM-115)2] (LFQM = 2-hydroxy-4-O-methylbenzophenone) [8], and between the parameters found in another similar complex (1.926(4) and 1.941(2) Å) [9]. Furthermore, Cu(II)-O bond length (1.883(2) Å, hydroxyl) is similar to the bond length of 1.876(2) Å in [Cu3Ni(hmb)6(OH)]ClO4⋅H2O [10], but shorter than the 1.951(2) Å of CuL⋅H2O [11]. Meanwhile, the six-membered ring composed of Cu(1), O(1), C(7), C(8), C(9) and O(2), is almost coplanar with r.m.s deviation of 0.096 Å.

In the complex, there are intermolecular hydrogen bonds, connecting two adjacent complexes (as indicated in the figure, O3—H3⋯O2b; O3c—H3′⋯O2, symmetry codes: b: y − 1/4, −x + 1/4, −z + 1/4, c: 1/4 − y, 1/4 + x, 1/4 − z). The O⋯O distance and the O—H⋯O angle are 2.750 Å and 177.08°, respectively. As a result, the title compound exhibits a two-dimensional supramolecular net architecture.

Acknowledgements

We gratefully acknowledge financial supports by the Natural Science Foundation of Fujian Province of China (No. 2013J01161, No. 2015H0024).

References

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Received: 2017-8-14
Accepted: 2017-10-23
Published Online: 2017-11-16
Published in Print: 2018-1-26

©2018 Hui Wang et al., published by De Gruyter, Berlin/Boston

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

Artikel in diesem Heft

  1. Cover and Frontmatter
  2. Editorial 2018
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  4. Crystal structure of aqua-bis{[2,6-dimethyl-N-(pyridin-2-ylmethylene)aniline-κ2N,N′]}zinc(II) triflate monohydrate [ZnC29H31N4O]CF3SO3⋅H2O
  5. Crystal structure of (E)-1-(4-{[(E)-4-Diethylamino-2-hydroxybenzene methylene]amino}phenyl)ethanone methoxy oxime, C20H27ClN3O3
  6. Crystal structure of (E)-1-(4-(((E)-4-(diethylamino)-2-hydroxybenzylidene)amino)phenyl)ethan-1-one oxime, C19H23N3O2
  7. Crystal structure of poly[(μ2-1,4-bis((2-ethyl-1H-benzo[d]imidazol-1-yl)methyl)benzene-κ2N:N′)-(μ2-4,4′-sulfonyldibenzoato-κ2O:O′)zinc(II)], C40H34N4O6SZn
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