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 W.
N1 - Funding Information:
We acknowledge Dr John Dewan for carrying out the X-ray analysis of the zinc and copper complexes. We thank Jesus Castagnetto for assistance with computational methods. We warmly thank the Petroleum Research Fund, administered by the American Chemical Society, and the National
Funding Information:
Institutes of Health (GM 49170) for financial support. C.S.A. acknowledges the National Institutes of Health for a Minority Research Opportunity Award.
PY - 1995/11
Y1 - 1995/11
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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U2 - 10.1016/0020-1693(95)04710-7
DO - 10.1016/0020-1693(95)04710-7
M3 - Article
AN - SCOPUS:0002970979
VL - 239
SP - 29
EP - 37
JO - Inorganica Chimica Acta
JF - Inorganica Chimica Acta
SN - 0020-1693
IS - 1-2
ER -