Home NQR, NMR, and X-ray crystal structure studies of [4-C2H5-C6H4NH3]2MBr4 (M=Zn, Cd)
Article
Licensed
Unlicensed Requires Authentication

NQR, NMR, and X-ray crystal structure studies of [4-C2H5-C6H4NH3]2MBr4 (M=Zn, Cd)

  • Hideta Ishihara EMAIL logo , Hisashi Honda , Ingrid Svoboda and Hartmut Fuess
Published/Copyright: August 8, 2018
Become an author with De Gruyter Brill
Author Information Explore this Subject
Zeitschrift für Naturforschung B
From the journal Zeitschrift für Naturforschung B Volume 73 Issue 9

Abstract

The crystal structure of [4-C2H5-C6H4NH3]2ZnBr4 (1) has been determined at 150(2) K: triclinic, P1̅, a=724.82(2), b=1194.20(4), c=1322.26(4) pm, α=74.151(3), β=80.887(3), γ=80.434(3)°, and Z=2. There are two crystallographically independent cations in the unit cell of 1: one has its benzene ring perpendicular to the crystallographic a axis of the unit cell and the other one has its benzene ring perpendicular to the c axis. These cations are alternatingly located along the c axis and form organic layers, and the ZnBr4 anions form inorganic layers in between. Zn–Br···H–N hydrogen bonds are formed between cations and anions. In accordance with the crystal structure, four nuclear quadrupole resonance (NQR) lines of 81Br were observed. The temperature dependence of the 81Br NQR frequencies between 77 and 320 K shows a peculiar feature which is not due to a structural phase transition. The measurement of 13C nuclear magnetic resonance spectra at around T=340 K indicates a redistribution of cations. The temperature dependence of 81Br NQR frequencies and differential thermal analysis measurements show that [4-C2H5-C6H4NH3]2CdBr4 (2) undergoes a structural phase transition at around 190 K.

Keywords: crystal structure; hydrogen bonding; NMR spectra; NQR spectra; phase transition; zinc and cadmium complexes

References

[1] H. Ishihara, S. Dou, K. Horiuchi, V. G. Krishnan, H. Paulus, H. Fuess, A. Weiss, Z. Naturforsch.1997, 52a, 550.10.1515/zna-1997-6-714Search in Google Scholar

[2] H. Ishihara, K. Horiuchi, I. Svoboda, H. Fuess, T. M. Gesing, J.-C. Buhl, H. Terao, Z. Naturforsch.2006, 61b, 69.10.1515/znb-2006-0114Search in Google Scholar

[3] H. Ishihara, M. Nakashima, H. Nakashima, R. Tateno, Y. Shibamura, T. Makino, A. Kikuchi, K. Horiuchi, I. Svoboda, H. Fuess, H. Terao, Z. Naturforsch.2011, 66b, 27.10.1515/znb-2011-0105Search in Google Scholar

[4] K. Horiuchi, H. Ishihara, H. Terao, J. Phys.: Condens. Matter,2000, 12, 4799.Search in Google Scholar

[5] P. Sondergeld, H. Fuess, S. A. Mason, H. Ishihara, W. W. Schmahl, Z. Naturforsch.2000, 55a, 801.10.1515/zna-2000-9-1009Search in Google Scholar

[6] K. Horiuchi, H. Ishihara, N. Hatano, S. Okamoto, T. Gushiken, Z. Naturforsch.2002, 57a, 425.10.1515/zna-2002-6-724Search in Google Scholar

[7] T. M. Gesing, E. Lork, H. Terao, H. Ishihara, Z. Naturforsch. 2016, 71b, 241.10.1515/znb-2015-0168Search in Google Scholar

[8] T. P. Das, E. L. Hahn, Nuclear Quadrupole Resonance Spectroscopy, Solid State Physics, Suppl. 1, New York, London, 1958, p. 164.Search in Google Scholar

[9] H. Ishihara, S. Dou, A. Weiss, Ber. Bunsenges. Phys. Chem. 1991, 95, 659.10.1002/bbpc.19910950602Search in Google Scholar

[10] D. Nakamura, R. Ikeda, M. Kubo, Coord. Chem. Rev. 1975, 17, 281.10.1016/S0010-8545(00)80379-3Search in Google Scholar

[11] H. Ishihara, S. Dou, K. Horiuchi, V. G. Krishnan, H. Paulus, H. Fuess, A. Weiss, Z. Naturforsch. 1996, 51a, 1027.10.1515/zna-1996-0909Search in Google Scholar

[12] H. Ishihara, K. Horiuchi, S. Dou, T. M. Gesing, J.-C. Buhl, Z. Naturforsch. 1998, 53a, 717.10.1515/zna-1998-0813Search in Google Scholar

[13] H. Ishihara, N. Hatano, K. Horiuchi, H. Terao, Z. Naturforsch.2002, 57a, 343.10.1515/zna-2002-6-710Search in Google Scholar

[14] H. Ishihara, K. Horiuchi, T. M. Gesing, J.-C. Buhl, Z. Naturforsch. 2002, 57b, 503.10.1515/znb-2002-0505Search in Google Scholar

[15] N. Hatano, M. Nakashima, K. Horiuchi, H. Terao, H. Ishihara, Z. Naturforsch. 2008, 63b, 1181.10.1515/znb-2008-1007Search in Google Scholar

[16] H. Ishihara, N. Hatano, K. Horiuchi, H. Terao, I. Svoboda, H. Fuess, Z. Naturforsch.2011, 66b, 1261.10.1515/znb-2011-1211Search in Google Scholar

[17] M. J. Frisch, G. W. Trucks, H. B. Schlegel, G. E. Scuseria, M. A. Robb, J. R. Cheeseman, J. A. Montgomery Jr., T. Vreven, K. N. Kudin, J. C. Burant, J. M. Millam, S. S. Iyengar, J. Tomasi, V. Barone, B. Mennucci, M. Cossi, G. Scalmani, N. Rega, G. A. Petersson, H. Nakatsuji, M. Hada, M. Ehara, K. Toyota, R. Fukuda, J. Hasegawa, M. Ishida, T. Nakajima, Y. Honda, O. Kitao, H. Nakai, M. Klene, X. Li, J. E. Knox, H. P. Hratchian, J. B. Cross, C. Adamo, J. Jaramillo, R. Gomperts, R. E. Stratmann, O. Yazyev, A. J. Austin, R. Cammi, C. Pomelli, J. W. Ochterski, P. Y. Ayala, K. Morokuma, G. A. Voth, P. Salvador, J. J. Dannenberg, V. G. Zakrzewski, S. Dapprich, A. D. Daniels, M. C. Strain, O. Farkas, D. K. Malick, A. D. Rabuck, K. Raghavachari, J. B. Foresman, J. V. Ortiz, Q. Cui, A. G. Baboul, S. Clifford, J. Cioslowski, B. B. Stefanov, G. Liu, A. Liashenko, P. Piskorz, I. Komaromi, R. L. Martin, D. J. Fox, T. Keith, M. A. Al-Laham, C. Y. Peng, A. Nanayakkara, M. Challacombe, P. M. W. Gill, B. Johnson, W. Chen, M. W. Wong, C. Gonzalez, J. A. Pople, Gaussian 03, Gaussian, Inc., Pittsburgh, PA (USA) 2003.Search in Google Scholar

[18] G. M. Sheldrick, Shelxs/l-97, Programs for Crystal Structure Determination, University of Göttingen, Göttingen (Germany) 1997.Search in Google Scholar

[19] G. M. Sheldrick, Acta Crystallogr.1990, A46, 467.10.1107/S0108767390000277Search in Google Scholar

[20] G. M. Sheldrick, Acta Crystallogr.2008, A64, 112.10.1107/S0108767307043930Search in Google Scholar PubMed

[21] Gamess (version 11), Windows Version, M. W. Schmidt, K. K. Baldridge, J. A. Boatz, S. T. Elbert, M. S. Gordon, J. H. Jensen, S. Koseki, N. Matsunaga, K. A. Nguyen, S. J. Su, T. L. Windus, M. Dupuis, J. A. Montgomery, J. Comput. Chem.1993, 14, 1347.10.1002/jcc.540141112Search in Google Scholar

[22] M. Suenaga, J. Comput. Chem. Jpn.2005, 4, 25.10.2477/jccj.4.25Search in Google Scholar

[23] M. Suenaga, J. Comput. Chem. Jpn.2008, 7, 33.10.2477/jccj.H1920Search in Google Scholar

[24] Mercury 3.9, Windows, the Cambridge Crystallographic Data Centre (CCDC).Search in Google Scholar

Received: 2018-05-31
Accepted: 2018-07-04
Published Online: 2018-08-08
Published in Print: 2018-09-25

©2018 Walter de Gruyter GmbH, Berlin/Boston

Articles in the same Issue

  1. Frontmatter
  2. In this Issue
  3. NQR, NMR, and X-ray crystal structure studies of [4-C2H5-C6H4NH3]2MBr4 (M=Zn, Cd)
  4. Ein ökonomisches Verfahren zur Aufarbeitung von Reaktionsgemischen bei Lewis-Säure-induzierten elektrophilen Aromatensubstitutionen
  5. Orthoamide und Iminiumsalze, XCIVa. Kondensationsreaktion von Orthoamiden von Alkincarbonsäuren mit 2-Methyl-5-phenacyl-1,3,4-thiadiazolen
  6. Highly effectual synthesis of 4,6-diarylpyrimidin-2(1H)-ones using N,N,N′,N′-tetramethylethylenediaminium-N,N′-disulfonic acid hydrogen sulfate as a dual-functional catalyst
  7. Efficient synthesis of pyrido[2,3-d]pyrimidine-7-carboxylic acids catalyzed by a TiO2/SiO2 nanocomposite in aqueous media at room temperature
  8. Synthesis, characterization, and antitumor activity of some novel S-functionalized benzo[d]thiazole-2-thiol derivatives; regioselective coupling to the –SH group
  9. A zinc(II) coordination polymer containing single- and double-stranded helical chains: synthesis, crystal structure, and thermal and luminescence properties
  10. An unexpected lanthanum chloride carbonate hydrate: synthesis, crystal structure, vibrational spectra and thermal degradation of LaCl[CO3]·3H2O
  11. Structures of the diiodine adducts of bis(diisopropylphosphano)methane disulfide and bis(diisopropylphosphano)ethane disulfide
  12. Note
  13. Photoluminescence of Baltic amber
https://doi.org/10.1515/znb-2018-0109
Keywords for this article
crystal structure; hydrogen bonding; NMR spectra; NQR spectra; phase transition; zinc and cadmium complexes

Articles in the same Issue

  1. Frontmatter
  2. In this Issue
  3. NQR, NMR, and X-ray crystal structure studies of [4-C2H5-C6H4NH3]2MBr4 (M=Zn, Cd)
  4. Ein ökonomisches Verfahren zur Aufarbeitung von Reaktionsgemischen bei Lewis-Säure-induzierten elektrophilen Aromatensubstitutionen
  5. Orthoamide und Iminiumsalze, XCIVa. Kondensationsreaktion von Orthoamiden von Alkincarbonsäuren mit 2-Methyl-5-phenacyl-1,3,4-thiadiazolen
  6. Highly effectual synthesis of 4,6-diarylpyrimidin-2(1H)-ones using N,N,N′,N′-tetramethylethylenediaminium-N,N′-disulfonic acid hydrogen sulfate as a dual-functional catalyst
  7. Efficient synthesis of pyrido[2,3-d]pyrimidine-7-carboxylic acids catalyzed by a TiO2/SiO2 nanocomposite in aqueous media at room temperature
  8. Synthesis, characterization, and antitumor activity of some novel S-functionalized benzo[d]thiazole-2-thiol derivatives; regioselective coupling to the –SH group
  9. A zinc(II) coordination polymer containing single- and double-stranded helical chains: synthesis, crystal structure, and thermal and luminescence properties
  10. An unexpected lanthanum chloride carbonate hydrate: synthesis, crystal structure, vibrational spectra and thermal degradation of LaCl[CO3]·3H2O
  11. Structures of the diiodine adducts of bis(diisopropylphosphano)methane disulfide and bis(diisopropylphosphano)ethane disulfide
  12. Note
  13. Photoluminescence of Baltic amber
Sign up now to receive a 20% welcome discount
Institutional Access
How does access work?
Have an idea on how to improve our website?
Please write us.
© 2025 De Gruyter Brill
Downloaded on 25.9.2025 from https://www.degruyterbrill.com/document/doi/10.1515/znb-2018-0109/html?lang=en
Scroll to top button