Synthesis, characterization and dynamical NMR studies of meso-tetra (4-pyridyl)porphyrinatothallium(III) acetate: Tl(tpyp)(OAc)

Jeou Jen Fuh; Suh Shing Tang; Yun Huin Lin; Jyh Horun Chen; Tung Sheng Liu; Shin Shin Wang; Jing Chie Lin

doi:10.1016/S0277-5387(00)83425-7

Synthesis, characterization and dynamical NMR studies of meso-tetra (4-pyridyl)porphyrinatothallium(III) acetate: Tl(tpyp)(OAc)

Jeou Jen Fuh, Suh Shing Tang, Yun Huin Lin, Jyh Horun Chen, Tung Sheng Liu, Shin Shin Wang, Jing Chie Lin

Graduate Institute of Materials Science and Engineering

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Abstract

We have synthesized the compound meso-tetra(4-pyridyl)porphyrinatothallium (III) acetate, Tl(tpyp)(OAc), by using a new procedure, and characterized its structure through ¹H/¹³C NMR spectroscopy, elemental analysis and the FABMS technique. The free energy of activation ΔG^‡₂₃₃ for the acetato group exchange between Tl(tpyp)(OAc) and acetic acid in CD₂Cl₂ solvent has been derived to be 41.6±0.3 kJ mol^-1 through ¹H NMR temperature-dependent measurements. The Correlation Spectroscopy via Long-Range Coupling technique (COLOC) was used to resolve two quaternary carbons, i.e. C_α and C_-1 of Tl(tpyp)(OAc) at 149.6 and 149.8 ppm, respectively, at 21°C. In the slow exchange region, the methyl and carbonyl carbons of the acetato group are separately located at 17.6 ppm [with ³J (Tl-¹³C) coupling constant 314 Hz] and 174.1 ppm [with ²J (Tl-¹³C) coupling constant 256 Hz], for the Tl(tpyp)(OAc) case, and at 21.3 and 178.4 ppm for the HOAc case.

Original language	English
Pages (from-to)	3031-3037
Number of pages	7
Journal	Polyhedron
Volume	13
Issue number	21
DOIs	https://doi.org/10.1016/S0277-5387(00)83425-7
State	Published - Nov 1994

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@article{a92725e92abf46feac56e719a597ba74,

title = "Synthesis, characterization and dynamical NMR studies of meso-tetra (4-pyridyl)porphyrinatothallium(III) acetate: Tl(tpyp)(OAc)",

abstract = "We have synthesized the compound meso-tetra(4-pyridyl)porphyrinatothallium (III) acetate, Tl(tpyp)(OAc), by using a new procedure, and characterized its structure through 1H/13C NMR spectroscopy, elemental analysis and the FABMS technique. The free energy of activation ΔG‡233 for the acetato group exchange between Tl(tpyp)(OAc) and acetic acid in CD2Cl2 solvent has been derived to be 41.6±0.3 kJ mol-1 through 1H NMR temperature-dependent measurements. The Correlation Spectroscopy via Long-Range Coupling technique (COLOC) was used to resolve two quaternary carbons, i.e. Cα and C-1 of Tl(tpyp)(OAc) at 149.6 and 149.8 ppm, respectively, at 21°C. In the slow exchange region, the methyl and carbonyl carbons of the acetato group are separately located at 17.6 ppm [with 3J (Tl-13C) coupling constant 314 Hz] and 174.1 ppm [with 2J (Tl-13C) coupling constant 256 Hz], for the Tl(tpyp)(OAc) case, and at 21.3 and 178.4 ppm for the HOAc case.",

author = "Fuh, {Jeou Jen} and Tang, {Suh Shing} and Lin, {Yun Huin} and Chen, {Jyh Horun} and Liu, {Tung Sheng} and Wang, {Shin Shin} and Lin, {Jing Chie}",

year = "1994",

month = nov,

doi = "10.1016/S0277-5387(00)83425-7",

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volume = "13",

pages = "3031--3037",

journal = "Polyhedron",

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TY - JOUR

T1 - Synthesis, characterization and dynamical NMR studies of meso-tetra (4-pyridyl)porphyrinatothallium(III) acetate

T2 - Tl(tpyp)(OAc)

AU - Fuh, Jeou Jen

AU - Tang, Suh Shing

AU - Lin, Yun Huin

AU - Chen, Jyh Horun

AU - Liu, Tung Sheng

AU - Wang, Shin Shin

AU - Lin, Jing Chie

PY - 1994/11

Y1 - 1994/11

N2 - We have synthesized the compound meso-tetra(4-pyridyl)porphyrinatothallium (III) acetate, Tl(tpyp)(OAc), by using a new procedure, and characterized its structure through 1H/13C NMR spectroscopy, elemental analysis and the FABMS technique. The free energy of activation ΔG‡233 for the acetato group exchange between Tl(tpyp)(OAc) and acetic acid in CD2Cl2 solvent has been derived to be 41.6±0.3 kJ mol-1 through 1H NMR temperature-dependent measurements. The Correlation Spectroscopy via Long-Range Coupling technique (COLOC) was used to resolve two quaternary carbons, i.e. Cα and C-1 of Tl(tpyp)(OAc) at 149.6 and 149.8 ppm, respectively, at 21°C. In the slow exchange region, the methyl and carbonyl carbons of the acetato group are separately located at 17.6 ppm [with 3J (Tl-13C) coupling constant 314 Hz] and 174.1 ppm [with 2J (Tl-13C) coupling constant 256 Hz], for the Tl(tpyp)(OAc) case, and at 21.3 and 178.4 ppm for the HOAc case.

AB - We have synthesized the compound meso-tetra(4-pyridyl)porphyrinatothallium (III) acetate, Tl(tpyp)(OAc), by using a new procedure, and characterized its structure through 1H/13C NMR spectroscopy, elemental analysis and the FABMS technique. The free energy of activation ΔG‡233 for the acetato group exchange between Tl(tpyp)(OAc) and acetic acid in CD2Cl2 solvent has been derived to be 41.6±0.3 kJ mol-1 through 1H NMR temperature-dependent measurements. The Correlation Spectroscopy via Long-Range Coupling technique (COLOC) was used to resolve two quaternary carbons, i.e. Cα and C-1 of Tl(tpyp)(OAc) at 149.6 and 149.8 ppm, respectively, at 21°C. In the slow exchange region, the methyl and carbonyl carbons of the acetato group are separately located at 17.6 ppm [with 3J (Tl-13C) coupling constant 314 Hz] and 174.1 ppm [with 2J (Tl-13C) coupling constant 256 Hz], for the Tl(tpyp)(OAc) case, and at 21.3 and 178.4 ppm for the HOAc case.

UR - http://www.scopus.com/inward/record.url?scp=0039644312&partnerID=8YFLogxK

U2 - 10.1016/S0277-5387(00)83425-7

DO - 10.1016/S0277-5387(00)83425-7

M3 - 期刊論文

AN - SCOPUS:0039644312

VL - 13

SP - 3031

EP - 3037

JO - Polyhedron

JF - Polyhedron

SN - 0277-5387

IS - 21

ER -

Synthesis, characterization and dynamical NMR studies of meso-tetra (4-pyridyl)porphyrinatothallium(III) acetate: Tl(tpyp)(OAc)

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