The chemical identity of “[Ag(py)2]MnO4” organic solvent soluble oxidizing agent and new synthetic routes for the preparation of [Ag(py)n]XO4 (X = Mn, Cl, and Re, n = 2–4) complexes

I. Sajó, Gréta B. Kovács, T. Pasinszki, P. Bombicz, Zoltán May, Imre M. Szilágyi, Anna Jánosity, Kalyan K. Banerji, Rajni Kant, László Kótai

Research output: Contribution to journalArticle

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Abstract

A widely used oxidizing agent in organic chemistry with an assumed structure of “[Ag(py)2]MnO4” and its perchlorate and perrhenate analogues are studied. Their synthesis in pure form is challenging. In order to clarify the chemical nature of the known compounds and find routes to new derivatives, a systematic study is presented for the synthesis of [Ag(py)n]XO4 (X = Mn, Cl, and Re, n = 2–4) complexes. Ten complexes including four new derivatives, [Ag(py)4]MnO4, [Ag(py)4]MnO4·4[Ag(py)2]MnO4, [Ag(py)2]ClO4·0.5 py, and [Ag(py)2]ReO4, are synthesized and characterized. The chemical identity of “Ag(py)2MnO4” is also clarified. A novel route to prepare [Ag(py)2]MnO4 is developed. The reaction of AgXO4 salts with neat pyridine followed by various crystallization techniques is used to prepare [Ag(py)2]XO4, [Ag(py)4]XO4, [Ag(py)4]XO4·4[Ag(py)2]XO4, and [Ag(py)2]XO4·0.5py (X = Cl, Mn) complexes. The solid phase structure of [Ag(py)2]MnO4·0.5py is determined (a = 19.410 Å, b = 7.788 Å, c = 21.177 Å, β = 104.20°, C2/c (15), Z = 4 (3a)). [Ag(py)2]+ cations in the crystal form dimeric units where silver ions are connected by oxygen atoms of two MnO4 anions. The Ag…Ag distance is indicative of argentophilic interactions. The pyridine ring π…π interactions contribute to the stability of the crystal lattice.

Original languageEnglish
JournalJournal of Coordination Chemistry
DOIs
Publication statusAccepted/In press - Jan 1 2018

Fingerprint

Oxidants
Pyridine
Organic solvents
pyridines
routes
Derivatives
organic chemistry
preparation
synthesis
Phase structure
perchlorates
crystal lattices
Crystal lattices
solid phases
oxygen atoms
Silver
Negative ions
Crystallization
Positive ions
silver

Keywords

  • Metal organic permanganates
  • perchlorates
  • perrhenates
  • structure
  • synthesis
  • X-ray diffraction

ASJC Scopus subject areas

  • Physical and Theoretical Chemistry
  • Materials Chemistry

Cite this

The chemical identity of “[Ag(py)2]MnO4” organic solvent soluble oxidizing agent and new synthetic routes for the preparation of [Ag(py)n]XO4 (X = Mn, Cl, and Re, n = 2–4) complexes. / Sajó, I.; Kovács, Gréta B.; Pasinszki, T.; Bombicz, P.; May, Zoltán; Szilágyi, Imre M.; Jánosity, Anna; Banerji, Kalyan K.; Kant, Rajni; Kótai, László.

In: Journal of Coordination Chemistry, 01.01.2018.

Research output: Contribution to journalArticle

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title = "The chemical identity of “[Ag(py)2]MnO4” organic solvent soluble oxidizing agent and new synthetic routes for the preparation of [Ag(py)n]XO4 (X = Mn, Cl, and Re, n = 2–4) complexes",
abstract = "A widely used oxidizing agent in organic chemistry with an assumed structure of “[Ag(py)2]MnO4” and its perchlorate and perrhenate analogues are studied. Their synthesis in pure form is challenging. In order to clarify the chemical nature of the known compounds and find routes to new derivatives, a systematic study is presented for the synthesis of [Ag(py)n]XO4 (X = Mn, Cl, and Re, n = 2–4) complexes. Ten complexes including four new derivatives, [Ag(py)4]MnO4, [Ag(py)4]MnO4·4[Ag(py)2]MnO4, [Ag(py)2]ClO4·0.5 py, and [Ag(py)2]ReO4, are synthesized and characterized. The chemical identity of “Ag(py)2MnO4” is also clarified. A novel route to prepare [Ag(py)2]MnO4 is developed. The reaction of AgXO4 salts with neat pyridine followed by various crystallization techniques is used to prepare [Ag(py)2]XO4, [Ag(py)4]XO4, [Ag(py)4]XO4·4[Ag(py)2]XO4, and [Ag(py)2]XO4·0.5py (X = Cl, Mn) complexes. The solid phase structure of [Ag(py)2]MnO4·0.5py is determined (a = 19.410 {\AA}, b = 7.788 {\AA}, c = 21.177 {\AA}, β = 104.20°, C2/c (15), Z = 4 (3a)). [Ag(py)2]+ cations in the crystal form dimeric units where silver ions are connected by oxygen atoms of two MnO4 – anions. The Ag…Ag distance is indicative of argentophilic interactions. The pyridine ring π…π interactions contribute to the stability of the crystal lattice.",
keywords = "Metal organic permanganates, perchlorates, perrhenates, structure, synthesis, X-ray diffraction",
author = "I. Saj{\'o} and Kov{\'a}cs, {Gr{\'e}ta B.} and T. Pasinszki and P. Bombicz and Zolt{\'a}n May and Szil{\'a}gyi, {Imre M.} and Anna J{\'a}nosity and Banerji, {Kalyan K.} and Rajni Kant and L{\'a}szl{\'o} K{\'o}tai",
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T1 - The chemical identity of “[Ag(py)2]MnO4” organic solvent soluble oxidizing agent and new synthetic routes for the preparation of [Ag(py)n]XO4 (X = Mn, Cl, and Re, n = 2–4) complexes

AU - Sajó, I.

AU - Kovács, Gréta B.

AU - Pasinszki, T.

AU - Bombicz, P.

AU - May, Zoltán

AU - Szilágyi, Imre M.

AU - Jánosity, Anna

AU - Banerji, Kalyan K.

AU - Kant, Rajni

AU - Kótai, László

PY - 2018/1/1

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N2 - A widely used oxidizing agent in organic chemistry with an assumed structure of “[Ag(py)2]MnO4” and its perchlorate and perrhenate analogues are studied. Their synthesis in pure form is challenging. In order to clarify the chemical nature of the known compounds and find routes to new derivatives, a systematic study is presented for the synthesis of [Ag(py)n]XO4 (X = Mn, Cl, and Re, n = 2–4) complexes. Ten complexes including four new derivatives, [Ag(py)4]MnO4, [Ag(py)4]MnO4·4[Ag(py)2]MnO4, [Ag(py)2]ClO4·0.5 py, and [Ag(py)2]ReO4, are synthesized and characterized. The chemical identity of “Ag(py)2MnO4” is also clarified. A novel route to prepare [Ag(py)2]MnO4 is developed. The reaction of AgXO4 salts with neat pyridine followed by various crystallization techniques is used to prepare [Ag(py)2]XO4, [Ag(py)4]XO4, [Ag(py)4]XO4·4[Ag(py)2]XO4, and [Ag(py)2]XO4·0.5py (X = Cl, Mn) complexes. The solid phase structure of [Ag(py)2]MnO4·0.5py is determined (a = 19.410 Å, b = 7.788 Å, c = 21.177 Å, β = 104.20°, C2/c (15), Z = 4 (3a)). [Ag(py)2]+ cations in the crystal form dimeric units where silver ions are connected by oxygen atoms of two MnO4 – anions. The Ag…Ag distance is indicative of argentophilic interactions. The pyridine ring π…π interactions contribute to the stability of the crystal lattice.

AB - A widely used oxidizing agent in organic chemistry with an assumed structure of “[Ag(py)2]MnO4” and its perchlorate and perrhenate analogues are studied. Their synthesis in pure form is challenging. In order to clarify the chemical nature of the known compounds and find routes to new derivatives, a systematic study is presented for the synthesis of [Ag(py)n]XO4 (X = Mn, Cl, and Re, n = 2–4) complexes. Ten complexes including four new derivatives, [Ag(py)4]MnO4, [Ag(py)4]MnO4·4[Ag(py)2]MnO4, [Ag(py)2]ClO4·0.5 py, and [Ag(py)2]ReO4, are synthesized and characterized. The chemical identity of “Ag(py)2MnO4” is also clarified. A novel route to prepare [Ag(py)2]MnO4 is developed. The reaction of AgXO4 salts with neat pyridine followed by various crystallization techniques is used to prepare [Ag(py)2]XO4, [Ag(py)4]XO4, [Ag(py)4]XO4·4[Ag(py)2]XO4, and [Ag(py)2]XO4·0.5py (X = Cl, Mn) complexes. The solid phase structure of [Ag(py)2]MnO4·0.5py is determined (a = 19.410 Å, b = 7.788 Å, c = 21.177 Å, β = 104.20°, C2/c (15), Z = 4 (3a)). [Ag(py)2]+ cations in the crystal form dimeric units where silver ions are connected by oxygen atoms of two MnO4 – anions. The Ag…Ag distance is indicative of argentophilic interactions. The pyridine ring π…π interactions contribute to the stability of the crystal lattice.

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KW - synthesis

KW - X-ray diffraction

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