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X-ray powder diffraction data for Copper (II). bis[(2E)-3-methoxy-2- [(2,4,6-trimethylphenyl)imino]-4-[(2,4,6-trimethylphenyl)imino-κN]- 3-pentanolato-κO] complex

Published online by Cambridge University Press:  15 October 2014

R. Pažout ,
J. Maixner ,
A. Sokolohorskyj  and
J. Merna
R. Pažout*
Affiliation:
Central Laboratories, Institute of Chemical Technology Prague, Technická 5, 166 28 Prague 6, Czech Republic
J. Maixner
Affiliation:
Central Laboratories, Institute of Chemical Technology Prague, Technická 5, 166 28 Prague 6, Czech Republic
A. Sokolohorskyj
Affiliation:
Department of Polymers, Institute of Chemical Technology Prague, Technická 5, 166 28 Prague, Czech Republic
J. Merna
Affiliation:
Department of Polymers, Institute of Chemical Technology Prague, Technická 5, 166 28 Prague, Czech Republic
*
a) Author to whom correspondence should be addressed. Electronic mail: richard.pazout@vscht.cz
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Abstract

X-ray powder diffraction data, unit-cell parameters and space group for a new bis(β-diiminato) Cu(II) complex, C48H62CuN4O4 are reported [a = 13.330 (3) Å, b = 11.137(2) Å, c = 8.832(2) Å, α = 78.88(2), β = 94.73(2), γ = 114.55(2), unit-cell volume V = 1170.26 Å3, Z = 1, and space group P − 1]. All measured lines were indexed and are consistent with the P−1 space group. No detectable impurity was observed.

Keywords

unit-cell parametersspace groupX-ray powder diffraction databis(β-diiminato) Cu(II) complex
Type
New Diffraction Data
Information
Powder Diffraction , Volume 29 , Issue 4 , December 2014 , pp. 389 - 392
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Copyright
Copyright © International Centre for Diffraction Data 2014 

I. INTRODUCTION

β-diiminates are among the most important ligands in current homogeneous catalysis (Bourget-Merle et al., Reference Bourget-Merle, Lappert and Severn2002; Asay et al., Reference Asay, Jones and Driess2011). Diiminate complexes are prepared by the deprotonation of β-diimines followed by their coordination to metal precursor. Catalytic activity of diiminate complexes is strongly influenced by the ligand structure; therefore the preparation of novel β-diimine ligands is desirable. Copper(II). bis[(2E)-3-methoxy-2-[(2,4,6-trimethylphenyl)imi-no]-4-[(2.4.6-trimethylphenyl) imino-κN]-3-pentanolato-κO] complex (Figure 1) is a stable reaction intermediate in synthesis of keto-β-diimine ligands (Yokota et al., Reference Yokota, Tachi and Itoh2002).

Figure 1. Structural formula of the title compound Copper (II). bis[(2E)-3-methoxy-2-[(2,4,6-trimethylphenyl)imino]-4-[(2,4,6-trimethylphenyl)imino-κN]-3-pentanolato-κO] complex.

II. EXPERIMENTAL

A. Sample preparation

Preparation of a Cu (II) complex is based on the oxidative degradation of β-diimine by copper acetate under aerobic conditions reported by Yokota et al. (Reference Yokota, Tachi and Itoh2002). The starting β-diimine ligand was prepared according to Feldman et al. (Reference Feldman, McLain, Parthasarathy, Marshall, Calabrese and Arthur1997). Reaction with copper (II) acetate monohydrate yielded β-diiminate copper(II) acetate. which was converted to the title complex [copper(II).bis[(2E)-3-methoxy-2-[(2,4,6-trimethylphenyl)imino]-4-[(2,4,6-trimethylphenyl) imino-κN] -3-pentanolato-κO]] by treating with molecular oxygen in methanol solution for 3 days at 50 °C.

B. Diffraction data collection and reduction

The diffraction pattern for the title compound was collected at room temperature using an X'Pert PRO θ–θ powder diffractometer with parafocusing Bragg–Brentano geometry and CuKα 1 radiation (λ = 1.5406 Å, generator setting: 40 kV, 30 mA). An ultrafast X'Celerator detector was employed to collect X-ray diffraction data (XRD) data over the angular range from 4 to 60°2θ with a step size of 0.017°2θ and a counting time of 20.32 s step−1. The software package HighScore Plus V 3.0d of PANalytical, Almelo, Netherlands, was used to smooth the data, to fit the background, and to eliminate the Kα 2 component. The top of smoothed peak method was used to determine the peak positions and intensities of the diffraction peaks.

Automatic indexing of the experimental XRD pattern was done using DICVOL06 (Boultif and Louër, Reference Boultif and Louër2004 ).

III. RESULTS

The experimental powder diffraction pattern is depicted in Figure 2. Automatic indexing results obtained by DICVOL06 (Table I) show that the title compound is triclinic with the space group P − 1 and unit-cell parameters: a = 13.330 (3) Å, b = 11.137(2) Å, c = 8.832(2) Å, α = 78.88(2), β = 94.73(2), γ = 114.55(2), unit-cell volume V = 1170.26 Å3, and Z = 1. The figures of merits are F 20 = 61.1(0.0080, 41) (Smith and Snyder, Reference Smith and Snyder1979) and M 20 = 26.2 (de Wolf, Reference De Wolff1968). All lines were indexed and are consistent with the P−1 space group.

Figure 2. (Color online) X-ray powder diffraction pattern of the title compound using and CuKα 1 radiation (λ = 1.5406 Å).

Table I. Indexed XRD data for the title compound, C48H62CuN4O4. Only the peaks with I rel of 1 or greater are presented [a = 13.330 (3) Å, b = 11.137(2) Å, c = 8.832(2) Å, α = 78.88(2), β = 94.73(2), γ = 114.55(2), unit-cell volume V = 1170.26 Å3, Z = 1, and space group P−1]. All measured lines were indexed and are consistent with the P−1 space group. The d-values were calculated using CuKα 1 radiation (λ = 1.5406 Å).

ACKNOWLEDGEMENT

This work was supported by the Technological Agency of the Czech Republic (Project No. TA 03011394).

References

Asay, M., Jones, C., and Driess, M. (2011). “N-Heterocyclic carbene analogues with low-valent Group 13 and Group 14 elements: syntheses, structures, and reactivities of a new generation of multitalented ligands,” Chem. Rev. 111, 354–396.Google Scholar
Boultif, A. and Louër, D. (2004). “Powder pattern indexing with the dichotomy method,” J. Appl. Crystallogr. 37, 724–731.Google Scholar
Bourget-Merle, L., Lappert, M. F., and Severn, J. R. (2002). “The chemistry of beta-diketiminatometal complexes,” Chem. Rev. 102, 3031–3065.Google Scholar
De Wolff, P. M. (1968). “A simplified criterion for the reliability of a powder pattern indexing,” J. Appl. Crystallogr. 1, 108–113.Google Scholar
Feldman, J., McLain, S. J., Parthasarathy, A., Marshall, W. J., Calabrese, J. C., and Arthur, S. D. (1997). “Electrophilic metal precursors and a beta-diimine ligand for nickel(II)- and palladium(II)-catalyzed ethylene polymerizations,” Organometallics 16, 1514–1516.Google Scholar
Smith, G. S. and Snyder, R. L. (1979). “FN: a criterion for rating powder diffraction patterns and evaluating the reliability of powder indexing,” J. Appl. Crystallogr. 12, 60–65.Google Scholar
Yokota, S., Tachi, Y., and Itoh, S. (2002). “Oxidative degradation of β-diketiminate ligand in copper(II) and zinc(II) complexes,” Inorg. Chem. 41, 1342–1344.Google Scholar
Figure 0

Figure 1. Structural formula of the title compound Copper (II). bis[(2E)-3-methoxy-2-[(2,4,6-trimethylphenyl)imino]-4-[(2,4,6-trimethylphenyl)imino-κN]-3-pentanolato-κO] complex.

Figure 1

Figure 2. (Color online) X-ray powder diffraction pattern of the title compound using and CuKα1 radiation (λ = 1.5406 Å).

Figure 2

Table I. Indexed XRD data for the title compound, C48H62CuN4O4. Only the peaks with Irel of 1 or greater are presented [a = 13.330 (3) Å, b = 11.137(2) Å, c = 8.832(2) Å, α = 78.88(2), β = 94.73(2), γ = 114.55(2), unit-cell volume V = 1170.26 Å3, Z = 1, and space group P−1]. All measured lines were indexed and are consistent with the P−1 space group. The d-values were calculated using CuKα1 radiation (λ = 1.5406 Å).