Synthetic and structural studies of the trans bis(2-N-H- pyrrolylcarbaldimine) complexes of nickel(II) and palladium(II)

Sarah Holzer; Frank R. Fronczek; Victor G. Young; Stephen Fox

doi:10.1007/s10870-006-9149-6

Synthetic and structural studies of the trans bis(2-N-H- pyrrolylcarbaldimine) complexes of nickel(II) and palladium(II)

Sarah Holzer, Frank R. Fronczek, Victor G. Young, Stephen Fox

Chemistry (Twin Cities)

Research output: Contribution to journal › Article › peer-review

1 Scopus citations

Abstract

The molecular bis(2-N-H-pyrrolylcarbaldimine)nickel(II) and palladium(II) complexes are isolated in moderate yield (30-35%) from in situ assembly of the Schiff base with metal(II) salt, base, and pyrrole-2-carbaldehyde in aqueous ammonia solution. The nickel(II) complex, 1, is monoclinic, space group P2 ₁/c, with a=11.289(6) Å, b=5.611(3) Å, c=8.287(5) Å, β=111.620(6)°, and V=488.0(5) Å³ with Z=2, for d _calc=1.667 Mg/m³. The palladium analog, 2, is isomorphous, space group P2₁/c, with a=11.481(3) Å, b=5.5738(10) Å, c=8.276(2) Å, β=110.923(12)°, and V=494.7(2) Å³ with Z=2, for d _calc=1.965 Mg/m ³. In both crystal structures, the metal resides on an inversion center. In the IR spectra, ν(C=N) appears at 1561 cm^-1 in 1, and 1557 cm^-1 in 2, while ν(N-H) shows at 3345 cm^-1 and 3335 cm^-1, respectively. The ¹H-nmr spectra reveal the C-H and N-H protons of the imine group as sharp and broad doublets, respectively, at 7.62 and 8.38 δ in 1 and at 7.92 and 9.73 δ in 2.

Original language	English (US)
Pages (from-to)	883-889
Number of pages	7
Journal	Journal of Chemical Crystallography
Volume	36
Issue number	12
DOIs	https://doi.org/10.1007/s10870-006-9149-6
State	Published - Dec 2006

Bibliographical note

Funding Information:
S.F. wishes to thank Dr. H. O’Neil Brotherton of the University of Louisiana at Monroe for determination of elemental analyses, and the Louisiana Board of Regents Support Fund (grant # (1998-01)-RD-A-22) for funding this work, especially for summer salary support. The purchase of the Nonius diffractometer was made possible by grant # LEQSF(1999–2000)-ESH-TR-13 administered by the Louisiana Board of Regents.

Keywords

Diamagnetic
Nickel(II)
Palladium(II)
Planar
Pyrrolate
Schiff-base

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@article{48bad3f6718746a9bc567c350aaa1bb9,

title = "Synthetic and structural studies of the trans bis(2-N-H- pyrrolylcarbaldimine) complexes of nickel(II) and palladium(II)",

abstract = "The molecular bis(2-N-H-pyrrolylcarbaldimine)nickel(II) and palladium(II) complexes are isolated in moderate yield (30-35%) from in situ assembly of the Schiff base with metal(II) salt, base, and pyrrole-2-carbaldehyde in aqueous ammonia solution. The nickel(II) complex, 1, is monoclinic, space group P2 1/c, with a=11.289(6) {\AA}, b=5.611(3) {\AA}, c=8.287(5) {\AA}, β=111.620(6)°, and V=488.0(5) {\AA}3 with Z=2, for d calc=1.667 Mg/m3. The palladium analog, 2, is isomorphous, space group P21/c, with a=11.481(3) {\AA}, b=5.5738(10) {\AA}, c=8.276(2) {\AA}, β=110.923(12)°, and V=494.7(2) {\AA}3 with Z=2, for d calc=1.965 Mg/m 3. In both crystal structures, the metal resides on an inversion center. In the IR spectra, ν(C=N) appears at 1561 cm-1 in 1, and 1557 cm-1 in 2, while ν(N-H) shows at 3345 cm-1 and 3335 cm-1, respectively. The 1H-nmr spectra reveal the C-H and N-H protons of the imine group as sharp and broad doublets, respectively, at 7.62 and 8.38 δ in 1 and at 7.92 and 9.73 δ in 2.",

keywords = "Diamagnetic, Nickel(II), Palladium(II), Planar, Pyrrolate, Schiff-base",

author = "Sarah Holzer and Fronczek, {Frank R.} and Young, {Victor G.} and Stephen Fox",

note = "Funding Information: S.F. wishes to thank Dr. H. O{\textquoteright}Neil Brotherton of the University of Louisiana at Monroe for determination of elemental analyses, and the Louisiana Board of Regents Support Fund (grant # (1998-01)-RD-A-22) for funding this work, especially for summer salary support. The purchase of the Nonius diffractometer was made possible by grant # LEQSF(1999–2000)-ESH-TR-13 administered by the Louisiana Board of Regents.",

year = "2006",

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doi = "10.1007/s10870-006-9149-6",

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AU - Holzer, Sarah

AU - Fronczek, Frank R.

AU - Young, Victor G.

AU - Fox, Stephen

N1 - Funding Information: S.F. wishes to thank Dr. H. O’Neil Brotherton of the University of Louisiana at Monroe for determination of elemental analyses, and the Louisiana Board of Regents Support Fund (grant # (1998-01)-RD-A-22) for funding this work, especially for summer salary support. The purchase of the Nonius diffractometer was made possible by grant # LEQSF(1999–2000)-ESH-TR-13 administered by the Louisiana Board of Regents.

PY - 2006/12

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N2 - The molecular bis(2-N-H-pyrrolylcarbaldimine)nickel(II) and palladium(II) complexes are isolated in moderate yield (30-35%) from in situ assembly of the Schiff base with metal(II) salt, base, and pyrrole-2-carbaldehyde in aqueous ammonia solution. The nickel(II) complex, 1, is monoclinic, space group P2 1/c, with a=11.289(6) Å, b=5.611(3) Å, c=8.287(5) Å, β=111.620(6)°, and V=488.0(5) Å3 with Z=2, for d calc=1.667 Mg/m3. The palladium analog, 2, is isomorphous, space group P21/c, with a=11.481(3) Å, b=5.5738(10) Å, c=8.276(2) Å, β=110.923(12)°, and V=494.7(2) Å3 with Z=2, for d calc=1.965 Mg/m 3. In both crystal structures, the metal resides on an inversion center. In the IR spectra, ν(C=N) appears at 1561 cm-1 in 1, and 1557 cm-1 in 2, while ν(N-H) shows at 3345 cm-1 and 3335 cm-1, respectively. The 1H-nmr spectra reveal the C-H and N-H protons of the imine group as sharp and broad doublets, respectively, at 7.62 and 8.38 δ in 1 and at 7.92 and 9.73 δ in 2.

AB - The molecular bis(2-N-H-pyrrolylcarbaldimine)nickel(II) and palladium(II) complexes are isolated in moderate yield (30-35%) from in situ assembly of the Schiff base with metal(II) salt, base, and pyrrole-2-carbaldehyde in aqueous ammonia solution. The nickel(II) complex, 1, is monoclinic, space group P2 1/c, with a=11.289(6) Å, b=5.611(3) Å, c=8.287(5) Å, β=111.620(6)°, and V=488.0(5) Å3 with Z=2, for d calc=1.667 Mg/m3. The palladium analog, 2, is isomorphous, space group P21/c, with a=11.481(3) Å, b=5.5738(10) Å, c=8.276(2) Å, β=110.923(12)°, and V=494.7(2) Å3 with Z=2, for d calc=1.965 Mg/m 3. In both crystal structures, the metal resides on an inversion center. In the IR spectra, ν(C=N) appears at 1561 cm-1 in 1, and 1557 cm-1 in 2, while ν(N-H) shows at 3345 cm-1 and 3335 cm-1, respectively. The 1H-nmr spectra reveal the C-H and N-H protons of the imine group as sharp and broad doublets, respectively, at 7.62 and 8.38 δ in 1 and at 7.92 and 9.73 δ in 2.

KW - Diamagnetic

KW - Nickel(II)

KW - Palladium(II)

KW - Planar

KW - Pyrrolate

KW - Schiff-base

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EP - 889

JO - Journal of Chemical Crystallography

JF - Journal of Chemical Crystallography

IS - 12

ER -

Synthetic and structural studies of the trans bis(2-N-H- pyrrolylcarbaldimine) complexes of nickel(II) and palladium(II)

Abstract

Bibliographical note

Keywords

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