Estimating internuclear distances between half-integer quadrupolar nuclei by central-transition double-quantum sideband NMR spectroscopy
2011 (English)In: Canadian journal of chemistry (Print), ISSN 0008-4042, E-ISSN 1480-3291, Vol. 89, no 7, 892-899 p.Article in journal (Refereed) Published
We demonstrate the estimation of homonuclear dipolar couplings, and thereby internuclear distances, between half-integer spin quadrupolar nuclei by central-transition (CT) double-quantum (2Q) sideband nuclear magnetic resonance (NMR) spectroscopy. It is shown that the rotor-encoded sideband amplitudes from CT 2Q coherences in the indirect dimension of the two-dimensional NMR spectrum are sensitive probes of the magnitude of the homonuclear dipolar coupling, but are significantly less affected by other NMR parameters such as the magnitudes and orientations of the electric field gradient tensors. Experimental results of employing the R2(2)(1)R2(2)(-1) recoupling sequence to the (11)B spin pair of bis(catecholato)diboron resulted in an estimation of the internuclear B-B distance as (169.6 +/- 3) pm, i.e., with a relative uncertainty of +/- 2%, and in excellent agreement with the distance of 167.8 pm determined by single-crystal X-ray diffraction.
Place, publisher, year, edition, pages
2011. Vol. 89, no 7, 892-899 p.
solid-state NMR, quadrupolar nuclei, central transition, double-quantum coherence, sideband spectroscopy, distance estimation
IdentifiersURN: urn:nbn:se:su:diva-66561DOI: 10.1139/V11-020ISI: 000295343800019OAI: oai:DiVA.org:su-66561DiVA: diva2:468948
authorCount :22011-12-222011-12-202011-12-22Bibliographically approved