V. Dharma Rao, M. Periasamy / Tetrahedron: Asymmetry 11 (2000) 1151±1155
1155
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22. The X-ray diraction measurements were carried out at 293 K on an automated Enraf±Nonious MACH 3
diractometer using graphite monochromated, Mo-Kꢀ (l=0.71073 A) radiation. Intensity data were collected by
the !-scan mode. The data were reduced using the XTAL programme. No absorption correction was applied.
Crystal structure data for compound 2: ꢃ range for data collection is 1.92 to 27.98ꢁ. Empirical formula C36H26O4,
colourless needles (0.8Â0.5Â1.2 mm), crystal system is orthorhombic, space group P212121, unit cell dimensions:
a=8.452(13) A, b=11.382(4) A, c=28.699(9) A; volume 2761(4) A3, Z=4, Dcalcd=1.257 Mg/m3, absorption
coecient is 0.081 mm 1, F(000)=1096, index ranges 0ꢂhꢂ11, 0ꢂkꢂ15, 0ꢂlꢂ37, total re¯ections collected were
3758, of which 2196 were independent re¯ections with R(int)=0.000 and R(sigma)=0.0287. The structure was
solved by direct methods and re®ned by full-matrix least-squares procedure using the SHELX 86 and SHELX 97
programme packages, respectively. The re®nement was carried out using 2196 observed [F>4ꢄ(F)] re¯ections and
converged to a ®nal R1=0.0729, wR2=0.2046 and goodness of ®t is 1.130 with largest dierence peak and hole at
0.231 and 0.196 e A 3, respectively. Crystal structure data for compound 3: ꢃ range for data collection is 1.72 to
27.47ꢁ. Empirical formula C36H24O4, colourless needles (0.6Â0.6Â0.6 mm), crystal system is monoclinic, space
group P21, unit cell dimensions: a=9.737(4) A, b=16.625(5) A, c=17.152(5) A, ꢅ=101.13(3) A; volume
2724.4(17) A3, Z=2, Dcalcd=1.269 Mg/m3, absorption coecient is 0.082 mm 1, F(000)=1088, index ranges
0ꢂhꢂ12, 0ꢂkꢂ21, 0ꢂlꢂ21, total re¯ections collected were 6457, of which 3477 were independent re¯ections
with R(int)=0.0130 and R(sigma)=0.0442. The structure was solved by direct methods and re®ned by full-matrix
least-squares procedure using the SHELX 86 and SHELX 97 programme packages, respectively. The re®nement
was carried out using 3477 observed [F>4ꢄ(F)] re¯ections and converged to a ®nal R1=0.0433, wR2=0.0898
and goodness of ®t is 0.981 with largest dierence peak and hole 0.231 and 0.196 e A 3, respectively. Detailed
X-ray crystallographic data are available from the Cambridge Crystallographic Data Centre, 12 Union Road,
Cambridge, CB2 1EZ, UK.
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