Metal(II) Complexes of Compartmental Polynuclear Schiff Bases Containing Phenolate and Alkoxy Groups
Abstract
:1. Introduction
2. Results and Discussion
2.1. Synthetic Aspects
2.2. General Characteristic Properties of the Complexes
2.3. IR and UV-VIS Spectra of the Complexes
2.4. Description of the Structures
2.4.1. [Cu(LOEt-phda)(H2O)].H2O (1)
2.4.2. [Ni(LOEt-phda)].H2O (2)
2.4.3. [Cu(LOEt-ambza)].H2O·EtOH (3)
2.4.4. [Cu(LOEt-ambza)].H2O (4)
2.4.5. [Ni(LOEt-ambza)] (5)
2.4.6. [Zn2(LOEt-ambza)(μ-OAc)(OAc)] (6)
3. Experimental Section
3.1. Materials and Physical Measurements
3.2. Syntheses
3.2.1. Synthesis of the Ligands
3.2.2. Synthesis of the Complexes
3.3. X-Ray Crystal Structure Analysis
4. Conclusions
Supplementary Materials
Acknowledgments
Author Contributions
Conflicts of Interest
References
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Compound | 1 | 2 | 3 |
---|---|---|---|
Empirical formula | C24H24CuN2O6 | C24H24N2NiO5 | C27H32CuN2O6 |
Formula mass | 500.00 | 479.14 | 544.10 |
Crystal system | Tetragonal | Monoclinic | Monoclinic |
Space group | P-421m | P21/c | P21/n |
a/Å | 21.9174(6) | 12.9329(6) | 10.7944(6) |
b/Å | 21.9174(6) | 14.5517(7) | 20.286(1) |
c/Å | 4.9513(2) | 11.7485(6) | 11.7600(6) |
α/° | 90 | 90 | 90 |
β/° | 90 | 109.983(3) | 94.767(2) |
γ/° | 90 | 90 | 90 |
V/Å3 | 2378.47(16) | 2077.74(18) | 2566.2(2) |
Z | 4 | 4 | 4 |
T/K | 100(2) | 100(2) | 100(2) |
μ/mm−1 | 0.959 | 0.975 | 0.895 |
Dcalc/Mg·m−3 | 1.396 | 1.532 | 1.408 |
Crystal size/mm | 0.24 × 0.15 × 0.11 | 0.24 × 0.18 × 0.13 | 0.16 × 0.15 × 0.11 |
θ max/° | 30.27 | 30.02 | 26.00 |
Data collected | 72696 | 32859 | 5073 |
Unique refl./Rint | 3594/0.0381 | 6067/0.0600 | 5044/----- |
Parameters/Restraints | 164/1 | 297/2 | 339/3 |
Goodness-of-Fit on F2 | 1.082 | 0.843 | 1.155 |
(I > 2σ(I))/wR2 (all data) | 0.0332/0.0975 | 0.0343/0.0894 | 0.0818/0.2113 |
Residual extrema/e·Å−3 | 1.11/−0.59 | 0.56/−0.51 | 0.94/−0.73 |
Compound | 4 | 5 | 6 |
---|---|---|---|
Empirical formula | C25H26CuN2O5 | C25H24N2NiO4 | C29H30N2O8Zn2 |
Formula mass | 498.03 | 475.15 | 665.33 |
Crystal system | Monoclinic | Monoclinic | Triclinic |
Space group | P21/c | P21/c | P-1 |
a/Å | 12.0486(4) | 12.0351(9) | 8.1702(15) |
b/Å | 16.5021(5) | 11.7906(8) | 12.476(2) |
c/Å | 11.2905(3) | 15.4288(11) | 14.531(3) |
α/° | 90 | 90 | 70.908(8) |
β/° | 97.206(2) | 93.783(2) | 78.161(8) |
γ/° | 90 | 90 | 79.352(7) |
V/Å3 | 2227.13(12) | 2184.6(3) | 1358.8(4) |
Z | 4 | 4 | 2 |
T/K | 100(2) | 100(2) | 100(2) |
μ/mm−1 | 1.021 | 0.923 | 1.821 |
Dcalc/Mg·m−3 | 1.485 | 1.445 | 1.626 |
Crystal size/mm | 0.21 × 0.18 × 0.12 | 0.26 × 0.21 × 0.13 | 0.26 × 0.20 × 0.14 |
θ max/° | 30.52 | 28.00 | 25.00 |
Data collected | 86525 | 20418 | 8896 |
Unique refl./Rint | 6786/0.0241 | 5272/0.0389 | 4772/0.0803 |
Parameters/Restraints | 306/2 | 291/0 | 374/0 |
Goodness-of-Fit on F2 | 1.056 | 1.047 | 1.122 |
(I > 2σ(I))/wR2 (all data) | 0.0287/0.0919 | 0.0375/0.0885 | 0.0934/0.2488 |
Residual extrema/e.Å−3 | 0.54/−0.34 | 0.96/−0.59 | 1.89/−1.44 |
Complex | Dihedral angle(s) (°) | O2-O2 bond distance (Ǻ) |
---|---|---|
3 | 118.2, 35.5 | 5.873 |
4 | 64.2, 49.4 | 5.818 |
5 | 128.0, 129.0 | 5.177 |
6 | 69.7, 31.8 | 5.468 |
© 2016 by the authors; licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC-BY) license (http://creativecommons.org/licenses/by/4.0/).
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Mautner, F.A.; Fischer, R.C.; Spell, M.; Acevedo, A.R.; Tran, D.H.; Massoud, S.S. Metal(II) Complexes of Compartmental Polynuclear Schiff Bases Containing Phenolate and Alkoxy Groups. Crystals 2016, 6, 91. https://doi.org/10.3390/cryst6080091
Mautner FA, Fischer RC, Spell M, Acevedo AR, Tran DH, Massoud SS. Metal(II) Complexes of Compartmental Polynuclear Schiff Bases Containing Phenolate and Alkoxy Groups. Crystals. 2016; 6(8):91. https://doi.org/10.3390/cryst6080091
Chicago/Turabian StyleMautner, Franz A., Roland C. Fischer, Mark Spell, Andres R. Acevedo, Diana H. Tran, and Salah S. Massoud. 2016. "Metal(II) Complexes of Compartmental Polynuclear Schiff Bases Containing Phenolate and Alkoxy Groups" Crystals 6, no. 8: 91. https://doi.org/10.3390/cryst6080091
APA StyleMautner, F. A., Fischer, R. C., Spell, M., Acevedo, A. R., Tran, D. H., & Massoud, S. S. (2016). Metal(II) Complexes of Compartmental Polynuclear Schiff Bases Containing Phenolate and Alkoxy Groups. Crystals, 6(8), 91. https://doi.org/10.3390/cryst6080091