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57849158249
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Data for 2 are as follows. Yield: 236 mg (55, Mp: 174-176 °C. Anal. Caled for C12H19N2SbSe (mol wt 392.01, C, 36.8; H, 4.9. Found: C, 37.0; H, 4.7. 1H NMR (CDCl3, δ 2.57 (6H, s, CH3)2N, 2.65 (6H, s, CH3)2N, 3.59 and 4.06 (4H, AX pattern, NCH2, 7.08 (2H, d, Ar-H3,5, 7.23 (1H, t, Ar-H4, 13C NMR (CDCl3, δ 46.06 (s, CH3) 2N, 46.53 (s, CH3)2N, 64.26 (s, NCH 2, 125.29 (s, Ar-C3,5, 129.2 (s, Ar-C4, 143.15 (s, Ar-C2,6, 151.76 (s, Ar-Cl, 77Se NMR (CDCl3, δ-197. 77Se CP/ MAS NMR: δ-153. Data for 3 are as follows. Yield: 115 mg (41, Mp: 165 °C dec. Anal. Caled for C12H19N 2SbTe (mol wt 440.65, C, 32.7; H, 4.4. Found: C, 38.0; H, 4.7. 1H NMR (THF, δ 2.55 6H, s
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125Te NMR (THF): δ-655.s
-
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18
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57849152047
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Data for 2: C12H19N2SbSe, M r, 392.0, orthorhombic, Pbca, a, 9.8540(8) Å, b, 15.4940(8) Å, c, 18.5060(19) Å, V, 2825.5(4) Å3, Z, 8, T= 150(1) K, 25 990 total reflections, 3245 independent (Rint, 0.126, R1 (obsd data, 0.040, wR2 (all data, 0.061, CCDC 688753. Data for 3: C12H19N2SbTe, Mr, 440.64, orthorhombic, Pbca, a, 9.8740(9) Å. b, 15.6460(15) Å, c, 18.913(2) Å, V, 2921.8(5) Å3, Z, 8, T, 150(1) K, 10 638 total reflections, 3249 independent (Rint, 0.082, R1 (obsd data, 0.046, wR2 all data, 0.097, CCDC 688752
-
int = 0.082, R1 (obsd data) = 0.046, wR2 (all data) = 0.097), CCDC 688752.
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-
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19
-
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0030661896
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For example, see: a
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57849105104
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2 analogues. See: (a) Dostál, L. et al. To be submitted for publication
-
2 analogues. See: (a) Dostál, L. et al. To be submitted for publication
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25
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34447291315
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57849143850
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Similar CP/MAS NMR experiments for 3 were hampered by its high reactivity.
-
Similar CP/MAS NMR experiments for 3 were hampered by its high reactivity.
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Hydrogen and first row: (a) Kendall, R. A.; Dunning, T. H.; Harrison, R. J. J. Chem. Phys. 1992, 96, 6796. Second row:
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57849111865
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We are deeply indebted to one of the referees of this manuscript for helpful suggestions especially proposal of the second alternative description of the nature of the Sb-Se and Sb-Te terminal bonds as strongly polarized single bonds was really stimulating for us.
-
We are deeply indebted to one of the referees of this manuscript for helpful suggestions especially proposal of the second alternative description of the nature of the Sb-Se and Sb-Te terminal bonds as strongly polarized single bonds was really stimulating for us.
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