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Inverse Coordination of an Ionic Lattice by a Metal Host

✍ Scribed by Melinda J. Duer; Felipe García; Richard A. Kowenicki; Vesal Naseri; Mary McPartlin; Matthew L. Stead; Robin S. Stein; Dominic S. Wright


Publisher
John Wiley and Sons
Year
2005
Tongue
English
Weight
215 KB
Volume
117
Category
Article
ISSN
0044-8249

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✦ Synopsis


p-CHPh), 0.40 ppm (br s, Me-Al); 31 P NMR (202.5 MHz, 298 K, THF/ [D 6 ]acetone capillary, 85 % H 3 PO 4 /D 2 O): d = À161.8 ppm; 7 Li NMR (194.4 MHz, 298 K, THF/[D 6 ]acetone capillary, sat. LiCl/D 2 O): d = 2.25 (br s, w1 =2 = 29 Hz, Li( 3)), 1.82 (br s, w1 =2 = 29 Hz, Li(1)), 0.36 ppm (s, w1 =2 = 10 Hz, Li(2)); assignments were made solely on the basis of the approximate integration of the spectrum, 1:4:8 ratio of the resonances (theoretical 1:4:12). The 31 P and 7 Li NMR solution spectra do not change with concentration or temperature (180-298 K), proving that no fragmentation of the anion of 1 occurs in solution. Solid state MAS-NMR, 7 Li (155.406 MHz, 32 scans, 15-s recycle delay): d = 3.6 (Li(1) and Li(2)), 0.4 ppm (Li(3)); 7 Li{ 1 H} CPMAS (399.87 MHz for 1 H, 4-ms contact time, 8 scans): d = 3.6 ppm; 6 Li{ 1 H} CPMAS (58.89 MHz/399.87 MHz for 1 H, 3-ms contact time, 4096 scans): d = 3.8 (Li(1)), 2.2 ppm (Li(2)); assignments made on the basis of approximate 2:1 integration. Sixty logarithmically spaced t values were collected between 0.01 s and 160 s for the RAS spectrum; twenty-four transients were collected for each t value; [22] elemental analysis (%) calcd for 1: C 60.0, H 6.8, P 15.0; found (typical): C 59.0, H 7.6, P 12.7.


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