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Crystallographic data (excluding structure factors) for the structure in this paper
were deposited with the Cambridge Crystallographic Data Centre as supplementary publication
numbers CCDC 273128, 273129 and 273130. These data can be obtained free of charge
from The Cambridge Crystallographic Data Centre via www.ccdc.cam.ac.uk/data_request/cif
or on application to CCDC, 12 Union Road, Cambridge, CB2 1EZ, UK. Crystal Data for 6a (CCDC 273128 and 273129): Empirical formula C31H42N4O2S2, formula weight 566.81, temperature 296 (2) K, wavelength 0.71073 Å, monoclinic,
space group P21. Unit cell dimensions a = 7.7147 (4) Å, b = 18.6723 (8) Å, c = 11.1002 (5) Å, β = 104.461 (2)°, V = 1548.34 (13) Å3, Z = 2, Dc = 1.216 Mg m-3, absorption coefficient 0.205 mm-1, F(000) = 608, crystal size 0.30 × 0.08 × 0.05 mm. Theta range for data collection
1.89-24.99°, index ranges -9 ≤ h ≤ 8, -18 ≤ k ≤ 22, -13 ≤ l ≤ 13, reflections collected 10775, unique reflections 2812 [R
int = 0.0940], completeness to θ
max (32.63°) = 99.9%, max. and min. transmission 0.9280 and 0.8000, refinement method
full-matrix least-squares on F2. Ordered Model: Data/restraints/parameters 2812/1/360, goodness-of-fit on F2 = 0.811, final R indices [I > 2σ(I)], R1 = 0.0412, wR2 = 0.0624, R indices (all data), R1 = 0.0993, wR2 = 0.0727, absolute structure parameter 0.00(9), largest diff. peak and hole 0.207
and -0.169 e Å-3. Disordered Model: Data/restraints/parameters 2812/1/381, goodness-of-fit on F2 = 0.791, final R indices [I > 2σ(I)], R1 = 0.0372, wR2 = 0.0464, R indices (all data), R1 = 0.0956, wR2 = 0.0547, absolute structure parameter -0.02 (7), largest diff. peak and hole 0.132
and -0.137 e Å-3. Two of the methyl groups (numbered C-16, C-17) were found to have very high Ueq values. These could be split to give disorder over the two sites. Whilst this significantly
improved wR2, one of the methyl groups (C-16) still had high Ueq values and the data/parameter ratio was worsened. Both models, therefore, have their
merits and data for both were deposited.
<A NAME="RP16705SS-12">12</A>
Crystal data of compound 6b (CCDC 273130): Empirical formula C37H54N4O2S2, formula weight 650.96, temperature 295 (2) K, wavelength 0.71073 Å, monoclinic,
space group P21. Unit cell dimensions a = 13.5162 (13) Å, b = 6.9703 (6) Å, c = 21.051 (2) Å, β = 102.897 (2)°, V = 1933.2 (3) Å3, Z = 2, Dc = 1.118 Mg m-3, absorption coefficient 0.172 mm-1, F(000) = 704, crystal size 0.80 × 0.10 × 0.10 mm. Theta range for data collection
1.98-32.63°, index ranges -10 ≤ h ≤ 20, -10 ≤ k ≤ 10, -31 ≤ l ≤ 29, reflections collected 18951, unique reflections 7507 [R
int = 0.1700], completeness to θ max (32.63°) = 99.1%, max. and min. transmission 0.9830 and 0.8721, refinement method
full-matrix least-squares on F2, data/restraints/parameters 7507/1/416, goodness-of-fit on F2 = 0.653, final R indices [I > 2σ(I)], R1 = 0.0487, wR2 = 0.0758, R indices (all data), R1 = 0.3135, wR2 = 0.1151, absolute structure parameter 0.12 (9), largest diff. peak and hole 0.155
and -0.163 e Å-3.
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