Homonuclear SQ-DQ correlations in solids: Applications of the broadband BaBa scheme to reveal 31P-31P spatial correlations in two-, three-, four-, and five-spin systems

Gábor Szalontai, Gábor Besenyei, L. Párkányí

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Abstract

In this paper, we report on the use and limitations of the popular double-quantum recoupling sequence back-to-back in studies of 31P-31P spatial proximities in Pd-phosphine complexes at medium field (9.38 T) under the conditions of fast MAS. The effects of internuclear distances in different spin systems and the impact of isotropic chemical shift and chemical shift anisotropy (CSA) offsets on the detectibility of SQ-DQ correlations were of particular interest to us. Selected model compounds with these requirements in mind were synthesized. By optimization of the excitation times of SQ-DQ correlations up to 4.6 Å could be obtained even in four-spin systems; however, certain long-range correlations may be weak or missing. Although under fast MAS, CSA values up to 270 ppm are well tolerated, in multi-spin systems in cases of isotropic chemical shift offsets larger than 50 ppm, the DQ coherences cannot be properly excited.

Original languageEnglish
Pages (from-to)801-811
Number of pages11
JournalMagnetic Resonance in Chemistry
Volume49
Issue number12
DOIs
Publication statusPublished - Dec 2011

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Chemical shift
phosphine
Anisotropy

Keywords

  • P SQ-DQ spectroscopy
  • BaBa excitation-reconversion scheme
  • fast MAS
  • Pd-phosphine complexes
  • two-, three, four, and five-spin systems
  • weak dipolar couplings

ASJC Scopus subject areas

  • Chemistry(all)
  • Materials Science(all)

Cite this

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title = "Homonuclear SQ-DQ correlations in solids: Applications of the broadband BaBa scheme to reveal 31P-31P spatial correlations in two-, three-, four-, and five-spin systems",
abstract = "In this paper, we report on the use and limitations of the popular double-quantum recoupling sequence back-to-back in studies of 31P-31P spatial proximities in Pd-phosphine complexes at medium field (9.38 T) under the conditions of fast MAS. The effects of internuclear distances in different spin systems and the impact of isotropic chemical shift and chemical shift anisotropy (CSA) offsets on the detectibility of SQ-DQ correlations were of particular interest to us. Selected model compounds with these requirements in mind were synthesized. By optimization of the excitation times of SQ-DQ correlations up to 4.6 {\AA} could be obtained even in four-spin systems; however, certain long-range correlations may be weak or missing. Although under fast MAS, CSA values up to 270 ppm are well tolerated, in multi-spin systems in cases of isotropic chemical shift offsets larger than 50 ppm, the DQ coherences cannot be properly excited.",
keywords = "P SQ-DQ spectroscopy, BaBa excitation-reconversion scheme, fast MAS, Pd-phosphine complexes, two-, three, four, and five-spin systems, weak dipolar couplings",
author = "G{\'a}bor Szalontai and G{\'a}bor Besenyei and L. P{\'a}rk{\'a}ny{\'i}",
year = "2011",
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T2 - Applications of the broadband BaBa scheme to reveal 31P-31P spatial correlations in two-, three-, four-, and five-spin systems

AU - Szalontai, Gábor

AU - Besenyei, Gábor

AU - Párkányí, L.

PY - 2011/12

Y1 - 2011/12

N2 - In this paper, we report on the use and limitations of the popular double-quantum recoupling sequence back-to-back in studies of 31P-31P spatial proximities in Pd-phosphine complexes at medium field (9.38 T) under the conditions of fast MAS. The effects of internuclear distances in different spin systems and the impact of isotropic chemical shift and chemical shift anisotropy (CSA) offsets on the detectibility of SQ-DQ correlations were of particular interest to us. Selected model compounds with these requirements in mind were synthesized. By optimization of the excitation times of SQ-DQ correlations up to 4.6 Å could be obtained even in four-spin systems; however, certain long-range correlations may be weak or missing. Although under fast MAS, CSA values up to 270 ppm are well tolerated, in multi-spin systems in cases of isotropic chemical shift offsets larger than 50 ppm, the DQ coherences cannot be properly excited.

AB - In this paper, we report on the use and limitations of the popular double-quantum recoupling sequence back-to-back in studies of 31P-31P spatial proximities in Pd-phosphine complexes at medium field (9.38 T) under the conditions of fast MAS. The effects of internuclear distances in different spin systems and the impact of isotropic chemical shift and chemical shift anisotropy (CSA) offsets on the detectibility of SQ-DQ correlations were of particular interest to us. Selected model compounds with these requirements in mind were synthesized. By optimization of the excitation times of SQ-DQ correlations up to 4.6 Å could be obtained even in four-spin systems; however, certain long-range correlations may be weak or missing. Although under fast MAS, CSA values up to 270 ppm are well tolerated, in multi-spin systems in cases of isotropic chemical shift offsets larger than 50 ppm, the DQ coherences cannot be properly excited.

KW - P SQ-DQ spectroscopy

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KW - two-, three, four, and five-spin systems

KW - weak dipolar couplings

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