organic compounds
Re®nement
Re®nement on F2
R(F) = 0.045
C10 methyl group of PHI493 and PHI495 were found to be rota-
tionally disordered, in a 0.6:0.4 ratio in PHI493 and in a 0.3:0.7 ratio in
PHI495. The major features in the ®nal difference map of PHI495
w = 1/[ꢅ2(Fo2) + (0.0639P)2]
where P = (Fo2 + 2Fc2)/3
(Á/ꢅ)max = 0.004
wR(F2) = 0.131
S = 1.01
Ê
were ꢂ1.1 A from the Br atom.
3
Ê
Áꢆmax = 0.61 e A
For all compounds, data collection: SMART (Bruker, 1998); cell
re®nement: SAINT (Bruker, 1998); data reduction: SAINT;
program(s) used to solve structure: SHELXS97 (Sheldrick, 1990);
program(s) used to re®ne structure: SHELXL97 (Sheldrick, 1997);
molecular graphics: SHELXTL (Bruker, 1997); software used to
prepare material for publication: SHELXTL.
3
Ê
0.51 e A
2643 re¯ections
200 parameters
H atoms treated by a mixture of
independent and constrained
re®nement
Áꢆmin
=
Table 6
Hydrogen-bonding geometry (A, ) for PHI495.
ꢁ
Ê
Supplementary data for this paper are available from the IUCr electronic
archives (Reference: BK1544). Services for accessing these data are
described at the back of the journal.
DÐHÁ Á ÁA
DÐH
HÁ Á ÁA
DÁ Á ÁA
DÐHÁ Á ÁA
O9ÐH9Á Á ÁO7
O9ÐH9Á Á ÁO7i
N1ÐH1Á Á ÁN11ii
0.89 (6)
0.89 (6)
0.82 (3)
1.70 (6)
2.52 (5)
2.44 (4)
2.508 (4)
3.027 (4)
3.218 (5)
150 (5)
117 (4)
161 (3)
References
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consin, USA.
Symmetry codes: (i) 1 x; y; z; (ii) 2 x; 1 y; z.
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compounds appeared well resolved in the difference Fourier maps
but, with the exception of PHI495, proved dif®cult to re®ne freely.
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command in SHELXL97 (Sheldrick, 1997), where the distances were
Ê
restrained to 0.82 and 0.86 A, respectively, and their Ueq values were
allowed to re®ne freely. All H atoms attached to C atoms were placed
in ideal positions and re®ned using a riding model with aromatic CÐ
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Ê
Ê
H = 0.96 A and methyl CÐH = 0.98 A, and with ®xed isotropic
displacement parameters equal to 1.2 (1.5 for methyl-H atoms) times
the equivalent isotropic displacement parameter of the atom to which
they were attached. The methyl groups were allowed to rotate about
their local threefold axis during re®nement. The H atoms in the
È
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È
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ꢀ
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Sutapa Ghosh et al. C12H8BrF3N2O3, C12H12N2O4S and C12H12N2O4S 1257
Ghosh, Sutapa
