Gabuda S P, Kozlova S G, Terskikh V V, Dybowski C, Neue G, Perry D L
Institute of Inorganic Chemistry, Novosibirsk, Russian Federation.
Solid State Nucl Magn Reson. 1999 Nov;15(2):103-7. doi: 10.1016/s0926-2040(99)00038-7.
Solid Pb3O4 has been studied with 207Pb nuclear magnetic resonance (NMR) spectroscopy. The 207Pb NMR chemical-shift tensor of the Pb2+ site has principal values of delta11 = 1980 +/- 5 ppm, delta22 = 1540 +/- 5 ppm, and delta33 = -1108 +/- 10 ppm; delta(iso) = 804 +/- 10 ppm. The chemical-shift tensor of the Pb4+ site is axial, with principal values delta(parallel) = -1009 +/- 3 ppm and delta(perpendicular) = 1132 +/- 3 ppm; delta(iso) = -1091 +/- 3 ppm. The Pb4+-Pb2+ scalar coupling constant J(Pb-Pb) = 2.3 +/- 0.1 kHz. The main contribution to the Pb2- chemical-shift anisotropy is proposed to arise from an exchange interaction in the Pb2+-Pb2+ pairs, conventionally regarded as molecular [Pb2]4+ ions.
已采用207Pb核磁共振（NMR）光谱法对固态Pb3O4进行了研究。Pb2+位点的207Pb NMR化学位移张量的主值为δ11 = 1980 ± 5 ppm，δ22 = 1540 ± 5 ppm，δ33 = -1108 ± 10 ppm；δ(iso) = 804 ± 10 ppm。Pb4+位点的化学位移张量是轴向的，主值为δ(平行) = -1009 ± 3 ppm和δ(垂直) = 1132 ± 3 ppm；δ(iso) = -1091 ± 3 ppm。Pb4+-Pb2+标量耦合常数J(Pb-Pb) = 2.3 ± 0.1 kHz。据推测，Pb2-化学位移各向异性的主要贡献源于Pb2+-Pb2+对中的交换相互作用，传统上认为该对为分子[Pb2]4+离子。
