Issue in Honor of Prof. Charles Rees ARKIVOC 2002 (vi) 82-90
X-ray crystallography
Data were collected with a Siemens SMART CCD area detector, using graphite monochromatized MoKa radiation (. = 0.71073 Å). The structures were solved by direct methods using SHELXS15 and refined on F2, using all data, by full-matrix least-squares procedures using SHELXL.16 Hydrogen atoms were included in calculated positions, with isotropic displacement parameters 1.2 times the isotropic equivalent of their carrier atoms. Crystal data for 15b. C20H14N8, MW 366.39, monoclinic, P21/n, a = 12.686(3), b = 8.366(2), c = 17.310(5) Å, ß = 108.152(3) o, V = 1745.8(8) Å 3, Z = 4, T = -105 oC, F(000) = 760, µ (MoKa) = 0.091 mm-1, Dcalcd = 1.394 g.cm-3, 2.max 53o (CCD area detector, 98% completeness), wR(F2) = 0.0922 (all 3537 data), R = 0.0346 (3031 data with I > 2sI). Crystal data for 17a. C8H7N3O, MW 161.17, monoclinic, P21/n, a = 11.290(6), b = 5.983(3), c = 11.654(6) Å, ß = 98.892(7) o, V = 777.6(7) Å 3, Z = 4, T = -100 oC, F(000) = 336, µ (MoKa) =
0.097 mm-1, Dcalcd = 1.377 g.cm-3, 2.max 53o (CCD area detector, 97% completeness), wR(F2) = 0.1320 (all 1563 data), R = 0.0461 (1270 data with I > 2sI). References
1. Katritzky, A. R.; Rogovoy, B. V.; Chassaing, C.; Vvedensky, V. J. Org. Chem. 2000, 65, 8080. 2. Katritzky, A. R.; Rogovoy, B. V.; Vvedensky, V. Y.; Kovalenko, K.; Steel, P. J.; Markov, V. I.; Forood, B. Synthesis 2001, 897. 3. Katritzky, A. R.; Rogovoy, B. V.; Vvedensky, V. Y.; Hebert, N.; Forood, B. J. Org. Chem. 2001, 66, 6797. 4. Andersen, H. S.; Moller, N. P. H.; Madsen, P. Pat. WO 9740017 A2; Chem. Abstr. 128:3688 5. Belliotti, T. R.; Connor, D. T.; Kostlan, C. R. US Pat. 5212189A; Chem. Abstr. 119:160299. 6. Blankenstein, G.; Moeckel, K. Z. Chem. 1962, 69. 7. Mano, M.; Seo, T.; Matsuno, T.; Imai, K. I. Chem. Pharm. Bull. 1976, 24, 2871. 8. Bansal, R. K.; Bhagchandani, G. J. Indian Chem. Soc. 1982, 59, 277. 9. Gehlen, H.; Möskel, K. Liebigs Ann. 1962, 651, 133. 10. Grigat, E.; Puetter, R. Chem. Ber. 1964, 97, 3560. 11. Ried, W.; Fulde, M.; Bats, J. W. Helvetica Chim. Acta 1989, 72, 969. 12. Fromm, E. Liebigs Ann. 1912, 394, 278. 13. Tateishi, K. Jpn. Kokai Tokkyo Koho 2001, JP 2001181538 A2 20010703; Chem. Abstr. 135:78348. 14. (a) Peters, K.; Peters, E.-M.; Hetzheim, A.; Kockritz, P. Z. Kristallogr. 2000, 215, 380. (b) Dymshits, V. A.; Rubleva, O. G. Zh. Org. Khim. 1993, 29, 2051. (c) Liszkiewicz, H.; Glowiak, T.; Kowalska, M. W.; Rutkowska, M.; Szelag, A.; Barczynska, J.; Kedzierska- Gozdzik, L.; Blaszczyk, F.; Dziewiszek, W. Pol. J. Chem. 1999, 73, 321. 15. Sheldrick, G. M. Acta Crystallogr. Sect. A 1990, 46, 467. 16. Sheldrick, G. M. SHELXTL; Bruker Analytical X-ray Systems, 1997. ISSN 1424-6376 Page 90 ©ARKAT USA, Inc
