Electrospray mass spectrometry and X-ray crystallography studies of divalent metal ion complexes of tris (2-pyridylmethyl) amine

Craig S. Allen, Chang Lin Chuang, Mark Cornebise, James Canary

Research output: Contribution to journalArticle

Abstract

Coordination complexes of tris(2-pyridylmethyl)amine (TPA) were prepared and characterized including [Zn(TPA)X]ClO4 (X = Cl, Br, I), [Cu(TPA)Br]ClO4, [Cd(TPA)Br2], [Cd(TPA) (H2O) (NO3]NO3, [Cd(TPA)I2], [Co9TPA)Cl2], [Fe(TPA)Cl2] and [Mn(TPA) Cl2] The solid-state structures of Zn(TPA)ClClO4 (monoclinic space group, P21/c; a = 14.733(3), b = 9.408(2), c = 29.722(4) A ̊, β=90.65(1)°; V=4119(1) A ̊3; Z=8, Zn(TPA)IClO4 (triclinic space group, P1; a = 14.435(3), b = 17.69(4), c = 9.745(2) A ̊, α=100.36(2), β=91.40(2), γ=114.62(1)°; V=2134(2) A ̊3; Z=4) and Cu(TPA)BrClO4 (monoclinic space group, P21/c; a=14.555(3), b=9.519(2), c=30.024(3) A ̊, β=91.66(1)°; V=4158(1) A ̊3; Z=8), contain trigonal bypyramidal metal ions with halide coordinated in an apical position. The X-ray structure of [Cd(TPA)(H2O)(NO3)]NO3 (monoclinic space group, P21/n; a=15.415(4), b=9.333(2), c=17.429(4) a ̊, β=99.39(2)°; V=2474(2) A ̊3; Z=4) contains a seven-coordinate cadmium ion including a bidentate nitrate anion and a water molecule as ligands. The X-ray structure of [Cd(TPA)I2] (monoclinic space group, P21/n; a=10.383(2), b=13.813(2), c=15.391(1) A ̊, β=106.07(1)°; V=2121.1(5) A ̊3; Z=4) contains a cadmium ion with an approximately octahedral geometry. In this structure, the TPA ligand is conformationally distorted in order to accomodate the octahedral coordination geometry. The convenient new technique, electrospray mass spectrometry (ESI-MS), provided mass spectra consistent with X-ray and spectroscopic data. Mass analysis of solutions containing added competing anions was also consistent with solution data.

Original languageEnglish (US)
Pages (from-to)29-37
Number of pages9
JournalInorganica Chimica Acta
Volume239
Issue number1-2
DOIs
StatePublished - 1995

Fingerprint

X ray crystallography
crystallography
Mass spectrometry
Metal ions
Amines
metal ions
amines
mass spectroscopy
Cadmium
X rays
Anions
Negative ions
Ligands
Ions
x rays
Geometry
Coordination Complexes
cadmium
Nitrates
anions

Keywords

  • Cadmium complexes
  • Crystal structures
  • Electrospray mass spectrometry
  • Polydentate amine complexes
  • Zinc complexes

ASJC Scopus subject areas

  • Inorganic Chemistry
  • Physical and Theoretical Chemistry
  • Materials Chemistry

Cite this

Electrospray mass spectrometry and X-ray crystallography studies of divalent metal ion complexes of tris (2-pyridylmethyl) amine. / Allen, Craig S.; Chuang, Chang Lin; Cornebise, Mark; Canary, James.

In: Inorganica Chimica Acta, Vol. 239, No. 1-2, 1995, p. 29-37.

Research output: Contribution to journalArticle

@article{31db5a29af3f4beda6b2b6ce1b8fdd7d,
title = "Electrospray mass spectrometry and X-ray crystallography studies of divalent metal ion complexes of tris (2-pyridylmethyl) amine",
abstract = "Coordination complexes of tris(2-pyridylmethyl)amine (TPA) were prepared and characterized including [Zn(TPA)X]ClO4 (X = Cl, Br, I), [Cu(TPA)Br]ClO4, [Cd(TPA)Br2], [Cd(TPA) (H2O) (NO3]NO3, [Cd(TPA)I2], [Co9TPA)Cl2], [Fe(TPA)Cl2] and [Mn(TPA) Cl2] The solid-state structures of Zn(TPA)ClClO4 (monoclinic space group, P21/c; a = 14.733(3), b = 9.408(2), c = 29.722(4) A ̊, β=90.65(1)°; V=4119(1) A ̊3; Z=8, Zn(TPA)IClO4 (triclinic space group, P1; a = 14.435(3), b = 17.69(4), c = 9.745(2) A ̊, α=100.36(2), β=91.40(2), γ=114.62(1)°; V=2134(2) A ̊3; Z=4) and Cu(TPA)BrClO4 (monoclinic space group, P21/c; a=14.555(3), b=9.519(2), c=30.024(3) A ̊, β=91.66(1)°; V=4158(1) A ̊3; Z=8), contain trigonal bypyramidal metal ions with halide coordinated in an apical position. The X-ray structure of [Cd(TPA)(H2O)(NO3)]NO3 (monoclinic space group, P21/n; a=15.415(4), b=9.333(2), c=17.429(4) a ̊, β=99.39(2)°; V=2474(2) A ̊3; Z=4) contains a seven-coordinate cadmium ion including a bidentate nitrate anion and a water molecule as ligands. The X-ray structure of [Cd(TPA)I2] (monoclinic space group, P21/n; a=10.383(2), b=13.813(2), c=15.391(1) A ̊, β=106.07(1)°; V=2121.1(5) A ̊3; Z=4) contains a cadmium ion with an approximately octahedral geometry. In this structure, the TPA ligand is conformationally distorted in order to accomodate the octahedral coordination geometry. The convenient new technique, electrospray mass spectrometry (ESI-MS), provided mass spectra consistent with X-ray and spectroscopic data. Mass analysis of solutions containing added competing anions was also consistent with solution data.",
keywords = "Cadmium complexes, Crystal structures, Electrospray mass spectrometry, Polydentate amine complexes, Zinc complexes",
author = "Allen, {Craig S.} and Chuang, {Chang Lin} and Mark Cornebise and James Canary",
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doi = "10.1016/0020-1693(95)04710-7",
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TY - JOUR

T1 - Electrospray mass spectrometry and X-ray crystallography studies of divalent metal ion complexes of tris (2-pyridylmethyl) amine

AU - Allen, Craig S.

AU - Chuang, Chang Lin

AU - Cornebise, Mark

AU - Canary, James

PY - 1995

Y1 - 1995

N2 - Coordination complexes of tris(2-pyridylmethyl)amine (TPA) were prepared and characterized including [Zn(TPA)X]ClO4 (X = Cl, Br, I), [Cu(TPA)Br]ClO4, [Cd(TPA)Br2], [Cd(TPA) (H2O) (NO3]NO3, [Cd(TPA)I2], [Co9TPA)Cl2], [Fe(TPA)Cl2] and [Mn(TPA) Cl2] The solid-state structures of Zn(TPA)ClClO4 (monoclinic space group, P21/c; a = 14.733(3), b = 9.408(2), c = 29.722(4) A ̊, β=90.65(1)°; V=4119(1) A ̊3; Z=8, Zn(TPA)IClO4 (triclinic space group, P1; a = 14.435(3), b = 17.69(4), c = 9.745(2) A ̊, α=100.36(2), β=91.40(2), γ=114.62(1)°; V=2134(2) A ̊3; Z=4) and Cu(TPA)BrClO4 (monoclinic space group, P21/c; a=14.555(3), b=9.519(2), c=30.024(3) A ̊, β=91.66(1)°; V=4158(1) A ̊3; Z=8), contain trigonal bypyramidal metal ions with halide coordinated in an apical position. The X-ray structure of [Cd(TPA)(H2O)(NO3)]NO3 (monoclinic space group, P21/n; a=15.415(4), b=9.333(2), c=17.429(4) a ̊, β=99.39(2)°; V=2474(2) A ̊3; Z=4) contains a seven-coordinate cadmium ion including a bidentate nitrate anion and a water molecule as ligands. The X-ray structure of [Cd(TPA)I2] (monoclinic space group, P21/n; a=10.383(2), b=13.813(2), c=15.391(1) A ̊, β=106.07(1)°; V=2121.1(5) A ̊3; Z=4) contains a cadmium ion with an approximately octahedral geometry. In this structure, the TPA ligand is conformationally distorted in order to accomodate the octahedral coordination geometry. The convenient new technique, electrospray mass spectrometry (ESI-MS), provided mass spectra consistent with X-ray and spectroscopic data. Mass analysis of solutions containing added competing anions was also consistent with solution data.

AB - Coordination complexes of tris(2-pyridylmethyl)amine (TPA) were prepared and characterized including [Zn(TPA)X]ClO4 (X = Cl, Br, I), [Cu(TPA)Br]ClO4, [Cd(TPA)Br2], [Cd(TPA) (H2O) (NO3]NO3, [Cd(TPA)I2], [Co9TPA)Cl2], [Fe(TPA)Cl2] and [Mn(TPA) Cl2] The solid-state structures of Zn(TPA)ClClO4 (monoclinic space group, P21/c; a = 14.733(3), b = 9.408(2), c = 29.722(4) A ̊, β=90.65(1)°; V=4119(1) A ̊3; Z=8, Zn(TPA)IClO4 (triclinic space group, P1; a = 14.435(3), b = 17.69(4), c = 9.745(2) A ̊, α=100.36(2), β=91.40(2), γ=114.62(1)°; V=2134(2) A ̊3; Z=4) and Cu(TPA)BrClO4 (monoclinic space group, P21/c; a=14.555(3), b=9.519(2), c=30.024(3) A ̊, β=91.66(1)°; V=4158(1) A ̊3; Z=8), contain trigonal bypyramidal metal ions with halide coordinated in an apical position. The X-ray structure of [Cd(TPA)(H2O)(NO3)]NO3 (monoclinic space group, P21/n; a=15.415(4), b=9.333(2), c=17.429(4) a ̊, β=99.39(2)°; V=2474(2) A ̊3; Z=4) contains a seven-coordinate cadmium ion including a bidentate nitrate anion and a water molecule as ligands. The X-ray structure of [Cd(TPA)I2] (monoclinic space group, P21/n; a=10.383(2), b=13.813(2), c=15.391(1) A ̊, β=106.07(1)°; V=2121.1(5) A ̊3; Z=4) contains a cadmium ion with an approximately octahedral geometry. In this structure, the TPA ligand is conformationally distorted in order to accomodate the octahedral coordination geometry. The convenient new technique, electrospray mass spectrometry (ESI-MS), provided mass spectra consistent with X-ray and spectroscopic data. Mass analysis of solutions containing added competing anions was also consistent with solution data.

KW - Cadmium complexes

KW - Crystal structures

KW - Electrospray mass spectrometry

KW - Polydentate amine complexes

KW - Zinc complexes

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