Despite the importance of (11)B nuclear magnetic resonance (NMR) in structural studies of borate glasses, no clear means of correlating NMR parameters with the number of nonbridging oxygens on three-coordinate boron has been demonstrated. In this work, a series of anhydrous, polycrystalline, binary borates has been examined by (11)B magic-angle spinning (MAS) NMR to obtain precise measurements of their three-coordinate boron isotropic chemical shifts. The shifts generally increase with the replacement of bridging oxygens by nonbridging oxygens, ranging from 14.6 ppm in crystalline B(2)O(3) to 22.5 ppm in magnesium orthoborate. The underlying physical basis for this trend is satisfactorily accounted for by considering second neighbor effects using bond valence sums. These data are supportive of a structural model for B(2)O(3) glass in which 72% of the boron atoms are in rings. High-field MAS NMR experiments (B(0) = 18.8 T) indicate that the boron shielding is anisotropic, with greater anisotropy measured for three-coordinate borons possessing one or two nonbridging oxygens, than for those with zero or three nonbridging oxygens.

Two B-site ordered double perovskites, La 2 LiReO 6 and Ba 2 YReO 6 , with S = 1 were investigated as geometrically frustrated antiferromagnets, using x-ray and neutron diffraction, superconducting quantum interference device magnetometry, heat capacity, muon spin relaxation ͑SR͒, and 89 Y magic-angle spinning ͑MAS͒ NMR. La 2 LiReO 6 has a monoclinic structure ͑P2 1 / n͒ with cell parameters at room temperature; a = 5.58262͑22͒ Å, b = 5.67582͑20͒ Å, c = 7.88586͑27͒ Å, and ␤ = 90.240͑4͒°. A zero-field cooled/field cooled ͑ZFC/FC͒ divergence at 50 K was observed in the susceptibility. The ZFC susceptibility is zero below ϳ5 K for polycrystalline samples, suggesting a cooperative singlet ground state but weak moments are induced by cooling in very small fields ϳ1 mT. No evidence of long-range ordering is evident in heat capacity, neutrondiffraction, or SR data. The ZF spin dynamics from SR are anomalous and can be fitted to a stretched exponential rather than the Kubo-Toyabe form expected for random frozen spins but the muon spins are decoupled in longitudinal fields ͑LF͒, consistent with spin freezing of the fraction of spins relaxing within the muon time scale. The internal fields sensed by the muons are anomalously small, consistent with an electronic spin-singlet state. Ba 2 YReO 6 is found to be cubic ͑Fm3m͒ with cell parameter a = 8.36278͑2͒ Å at 300 K with no change in symmetry at 3.8 K, at variance with the Jahn-Teller theorem for a t 2g 2 configuration for Re 5+ . 89 Y MAS NMR shows a single peak indicating that Y/Re site disorder is at most 0.5%. The susceptibility shows two broad peaks around 50 and 25 K but no evidence for long-range order from heat capacity, neutron diffraction, or SR. The ZF SR result shows a two-component ground state with both slow and fast relaxations and decoupling results in a 1 kG LF, indicating spin freezing. These results are in sharp contrast to the long-range AF order found in the S =3/ 2 isostructural materials, La 2 LiRuO 6 and Ba 2 YRuO 6 , indicating that the reduction to S = 1 plays a major role in ground state determination.

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