title: Dipolar coupling information in multispin systems: application of a compensated REDOR NMR approach to inorganic phosphates. Rotational echo double resonance.
abstract: An experimental strategy has been developed for measuring multiple dipole-dipole interactions in inorganic compounds using the technique of rotational echo double resonance (REDOR) NMR. Geometry-independent information about the dipole couplings between the observe nuclear species S (arbitrary quantum number) and the heteronuclear species I (spin-12) can be conveniently obtained from the experimental curve of DeltaS/S(0) versus dipolar evolution time by limiting the analysis to the initial data range 0 < delta S/S(0) < 0.30. Numerical simulations have been carried out on a three-spin system of type SI(2) in order to assess the effect of the I-I homonuclear dipole-dipole coupling and the influence of experimental imperfections such as finite pulse length and misadjustments of the 180 degrees pulses applied to the I-spin species. The simulations show further that within the initial data range the effects of such misadjustments can be internally compensated by a modified sequence having an additional 180 degrees pulse on the I channel in the middle of the dipolar evolution periods. Experimental (27)Al¿(31)P¿ REDOR results on the multispin systems Al(PO(3))(3), AlPO(4), [AlPO(4)](12)(C(3)H(7))(4)NF, and Na(3)PO(4) confirm the general utility of this approach. Thus, for applications to unknown systems the compensation strategy obviates calibration procedures with model compounds.
authors.affiliation: Institut für Physikalische Chemie, Westfälische Wilhelms-Universität Münster, Schlossplatz 7, Münster D48149, Germany.
authors.forename: J C
authors.initials: JC
authors.lastname: Chan
authors.forename: H
authors.initials: H
authors.lastname: Eckert
mesh_terms: D003198:Computer Simulation; D016018:Least-Squares Analysis; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D008433:Mathematics; D010710:Phosphates / Q000737:chemistry*; D012815:Signal Processing, Computer-Assisted
chemical_list: D010710:Phosphates