# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2014 data_keinan-49 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Keinan-49 (Galit)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H94 N8 O6 S4' _chemical_formula_weight 1223.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 21.716(4) _cell_length_b 12.428(2) _cell_length_c 27.774(6) _cell_angle_alpha 90.00 _cell_angle_beta 111.59(3) _cell_angle_gamma 90.00 _cell_volume 6970(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20236 _cell_measurement_theta_min 1.93 _cell_measurement_theta_max 25.26 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.166 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2632 _exptl_absorpt_coefficient_mu 0.189 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi- and omega-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20236 _diffrn_reflns_av_R_equivalents 0.0980 _diffrn_reflns_av_sigmaI/netI 0.1308 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6007 _reflns_number_gt 2389 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 2006)' _computing_cell_refinement 'DENZO HKL2000 (Otwinowski & Minor 1997)' _computing_data_reduction 'DENZO HKL2000 (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'TEXSAN (MSC, 1999)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1794P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(3) _refine_ls_number_reflns 6007 _refine_ls_number_parameters 724 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.2215 _refine_ls_R_factor_gt 0.0912 _refine_ls_wR_factor_ref 0.2876 _refine_ls_wR_factor_gt 0.2294 _refine_ls_goodness_of_fit_ref 0.882 _refine_ls_restrained_S_all 0.884 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.19637(11) 0.4183(2) 0.42005(10) 0.0780(8) Uani 1 1 d . . . S4 S 0.61193(11) 0.3926(2) 0.46235(10) 0.0789(9) Uani 1 1 d . . . S3 S 0.46039(12) 0.4169(2) 0.11650(10) 0.0750(9) Uani 1 1 d . . . S2 S 0.04695(10) 0.3960(2) 0.07593(10) 0.0715(8) Uani 1 1 d . . . O1 O 0.0611(3) 0.3715(5) 0.1918(3) 0.089(2) Uani 1 1 d . . . H1 H 0.0590 0.3660 0.1619 0.107 Uiso 1 1 calc R . . O2 O 0.3016(2) 0.4406(4) 0.0583(2) 0.068(2) Uani 1 1 d . . . H2 H 0.3418 0.4454 0.0735 0.082 Uiso 1 1 calc R . . O3 O 0.5985(3) 0.3691(6) 0.3441(3) 0.096(3) Uani 1 1 d . . . H3 H 0.6135 0.3516 0.3747 0.144 Uiso 1 1 calc R . . O4 O 0.3576(3) 0.4391(4) 0.4802(2) 0.0697(18) Uani 1 1 d . . . H4 H 0.3171 0.4418 0.4673 0.084 Uiso 1 1 calc R . . N1 N 0.2340(3) 0.5898(5) 0.3779(3) 0.061(2) Uani 1 1 d . . . N2 N 0.1605(4) 0.4838(6) 0.3214(3) 0.079(3) Uani 1 1 d . . . N3 N 0.1269(3) 0.2240(6) 0.1150(3) 0.072(3) Uani 1 1 d . . . N4 N 0.1603(3) 0.3327(5) 0.0651(3) 0.058(2) Uani 1 1 d . . . N5 N 0.4265(3) 0.5845(6) 0.1594(3) 0.062(2) Uani 1 1 d . . . N6 N 0.4999(3) 0.4875(5) 0.2167(3) 0.057(2) Uani 1 1 d . . . N7 N 0.5321(3) 0.2232(5) 0.4267(3) 0.056(2) Uani 1 1 d . . . N8 N 0.5000(3) 0.3282(6) 0.4751(3) 0.059(2) Uani 1 1 d . . . C1 C 0.1977(3) 0.5032(6) 0.3719(3) 0.048(2) Uani 1 1 d . . . C2 C 0.2239(5) 0.6405(6) 0.3269(4) 0.077(3) Uani 1 1 d . . . H2A H 0.2074 0.7113 0.3287 0.092 Uiso 1 1 d R . . H2B H 0.2636 0.6457 0.3195 0.092 Uiso 1 1 d R . . C3 C 0.1692(4) 0.5731(7) 0.2931(3) 0.072(3) Uani 1 1 d . . . H3A H 0.1838 0.5445 0.2671 0.086 Uiso 1 1 d R . . H3B H 0.1276 0.6091 0.2768 0.086 Uiso 1 1 d R . . C4 C 0.1086(4) 0.4131(6) 0.2986(3) 0.064(3) Uani 1 1 d . . . H4A H 0.1019 0.3808 0.3276 0.076 Uiso 1 1 d R . . H4B H 0.0672 0.4393 0.2745 0.076 Uiso 1 1 d R . . C5 C 0.1292(4) 0.3135(7) 0.2747(3) 0.059(3) Uani 1 1 d . . . C6 C 0.1740(5) 0.2413(9) 0.3032(4) 0.092(4) Uani 1 1 d . . . H6 H 0.1907 0.2487 0.3401 0.111 Uiso 1 1 d R . . C7 C 0.1896(5) 0.1390(7) 0.2843(4) 0.083(4) Uani 1 1 d . . . C8 C 0.1619(4) 0.1290(8) 0.2301(4) 0.075(3) Uani 1 1 d . . . H8 H 0.1696 0.0615 0.2166 0.091 Uiso 1 1 d R . . C9 C 0.1204(4) 0.1996(6) 0.2001(3) 0.062(3) Uani 1 1 d . . . C10 C 0.1038(4) 0.2945(7) 0.2220(4) 0.072(3) Uani 1 1 d . . . C11 C 0.2470(5) 0.0618(8) 0.3208(4) 0.102(4) Uani 1 1 d . . . C12 C 0.2173(5) 0.0335(9) 0.3665(4) 0.115(5) Uani 1 1 d . . . H12A H 0.2504 -0.0169 0.3862 0.139 Uiso 1 1 d R . . H12B H 0.1745 0.0003 0.3558 0.139 Uiso 1 1 d R . . H12C H 0.2182 0.0951 0.3875 0.139 Uiso 1 1 d R . . C13 C 0.3083(6) 0.1208(8) 0.3493(6) 0.156(7) Uani 1 1 d . . . H13A H 0.3342 0.0710 0.3752 0.187 Uiso 1 1 d R . . H13B H 0.2950 0.1795 0.3656 0.187 Uiso 1 1 d R . . H13C H 0.3342 0.1475 0.3304 0.187 Uiso 1 1 d R . . C14 C 0.2436(6) -0.0448(8) 0.2978(5) 0.125(5) Uani 1 1 d . . . H14A H 0.2694 -0.0954 0.3234 0.150 Uiso 1 1 d R . . H14B H 0.2647 -0.0314 0.2736 0.150 Uiso 1 1 d R . . H14C H 0.2002 -0.0737 0.2799 0.150 Uiso 1 1 d R . . C15 C 0.0911(4) 0.1761(7) 0.1446(4) 0.066(3) Uani 1 1 d . . . H15A H 0.0479 0.2081 0.1328 0.079 Uiso 1 1 d R . . H15B H 0.0870 0.1000 0.1390 0.079 Uiso 1 1 d R . . C16 C 0.1137(3) 0.3180(7) 0.0846(3) 0.055(3) Uani 1 1 d . . . C17 C 0.1860(4) 0.1704(7) 0.1134(4) 0.078(3) Uani 1 1 d . . . H17A H 0.2180 0.1553 0.1472 0.094 Uiso 1 1 d R . . H17B H 0.1725 0.1045 0.0945 0.094 Uiso 1 1 d R . . C18 C 0.2121(4) 0.2456(8) 0.0826(4) 0.085(3) Uani 1 1 d . . . H18A H 0.2175 0.2121 0.0533 0.102 Uiso 1 1 d R . . H18B H 0.2534 0.2762 0.1045 0.102 Uiso 1 1 d R . . C19 C 0.1637(4) 0.4226(6) 0.0347(3) 0.056(3) Uani 1 1 d . . . H19A H 0.1838 0.3980 0.0112 0.067 Uiso 1 1 d R . . H19B H 0.1216 0.4546 0.0155 0.067 Uiso 1 1 d R . . C20 C 0.2042(4) 0.5124(7) 0.0618(4) 0.064(3) Uani 1 1 d . . . C21 C 0.2707(4) 0.5192(5) 0.0757(3) 0.045(2) Uani 1 1 d . . . C22 C 0.3099(4) 0.6126(6) 0.1025(3) 0.055(2) Uani 1 1 d . . . C23 C 0.2741(4) 0.6944(6) 0.1196(4) 0.064(3) Uani 1 1 d . . . H23 H 0.3006 0.7513 0.1404 0.077 Uiso 1 1 d R . . C24 C 0.2057(4) 0.6851(6) 0.1098(4) 0.071(3) Uani 1 1 d . . . C25 C 0.1674(4) 0.5948(7) 0.0805(3) 0.063(3) Uani 1 1 d . . . H25 H 0.1223 0.5902 0.0781 0.075 Uiso 1 1 d R . . C26 C 0.1718(3) 0.7644(5) 0.1303(3) 0.059(2) Uani 1 1 d . . . C27 C 0.2133(6) 0.8612(8) 0.1507(5) 0.144(3) Uani 1 1 d . . . H27A H 0.1902 0.9099 0.1650 0.216 Uiso 1 1 calc R . . H27B H 0.2220 0.8962 0.1230 0.216 Uiso 1 1 calc R . . H27C H 0.2543 0.8401 0.1771 0.216 Uiso 1 1 calc R . . C28 C 0.1478(6) 0.7141(9) 0.1662(5) 0.144(3) Uani 1 1 d . . . H28A H 0.1267 0.7669 0.1802 0.216 Uiso 1 1 calc R . . H28B H 0.1842 0.6824 0.1938 0.216 Uiso 1 1 calc R . . H28C H 0.1164 0.6592 0.1488 0.216 Uiso 1 1 calc R . . C29 C 0.1169(6) 0.8183(8) 0.0830(5) 0.144(3) Uani 1 1 d . . . H29A H 0.0933 0.8703 0.0952 0.216 Uiso 1 1 calc R . . H29B H 0.0866 0.7642 0.0631 0.216 Uiso 1 1 calc R . . H29C H 0.1370 0.8534 0.0617 0.216 Uiso 1 1 calc R . . C30 C 0.3754(5) 0.6275(7) 0.1072(4) 0.083(3) Uani 1 1 d . . . H30A H 0.3832 0.7036 0.1043 0.099 Uiso 1 1 calc R . . H30B H 0.3825 0.5909 0.0788 0.099 Uiso 1 1 calc R . . C31 C 0.4636(4) 0.4950(7) 0.1666(4) 0.057(3) Uani 1 1 d . . . C32 C 0.4388(4) 0.6413(7) 0.2077(4) 0.063(3) Uani 1 1 d . . . H32A H 0.4534 0.7133 0.2055 0.076 Uiso 1 1 d R . . H32B H 0.3988 0.6433 0.2148 0.076 Uiso 1 1 d R . . C33 C 0.4923(4) 0.5755(7) 0.2506(4) 0.074(3) Uani 1 1 d . . . H33A H 0.4789 0.5461 0.2772 0.088 Uiso 1 1 d R . . H33B H 0.5334 0.6131 0.2663 0.088 Uiso 1 1 d R . . C34 C 0.5511(5) 0.3990(7) 0.2371(4) 0.081(4) Uani 1 1 d . . . H34A H 0.5614 0.3700 0.2086 0.097 Uiso 1 1 calc R . . H34B H 0.5913 0.4301 0.2617 0.097 Uiso 1 1 calc R . . C35 C 0.5296(4) 0.3098(8) 0.2627(4) 0.077(3) Uani 1 1 d . . . C36 C 0.4869(4) 0.2343(6) 0.2308(4) 0.058(3) Uani 1 1 d . . . H36 H 0.4683 0.2529 0.1948 0.069 Uiso 1 1 d R . . C37 C 0.4648(4) 0.1472(7) 0.2509(3) 0.058(3) Uani 1 1 d . . . C38 C 0.4945(4) 0.1298(7) 0.3030(4) 0.058(3) Uani 1 1 d . . . H38 H 0.4779 0.0752 0.3194 0.070 Uiso 1 1 d R . . C39 C 0.5402(4) 0.2079(7) 0.3373(3) 0.058(3) Uani 1 1 d . . . C40 C 0.5544(4) 0.2948(6) 0.3166(4) 0.061(3) Uani 1 1 d . . . C41 C 0.4188(5) 0.0702(7) 0.2156(4) 0.085(4) Uani 1 1 d . . . C42 C 0.4323(11) 0.0519(13) 0.1662(9) 0.257(11) Uani 1 1 d . . . H42A H 0.4341 0.1200 0.1505 0.386 Uiso 1 1 calc R . . H42B H 0.3974 0.0090 0.1426 0.386 Uiso 1 1 calc R . . H42C H 0.4738 0.0153 0.1744 0.386 Uiso 1 1 calc R . . C43 C 0.3470(6) 0.1213(11) 0.2023(10) 0.284(17) Uani 1 1 d . . . H43A H 0.3435 0.1863 0.1828 0.427 Uiso 1 1 calc R . . H43B H 0.3403 0.1373 0.2338 0.427 Uiso 1 1 calc R . . H43C H 0.3139 0.0710 0.1822 0.427 Uiso 1 1 calc R . . C44 C 0.4092(6) -0.0347(8) 0.2413(7) 0.184(8) Uani 1 1 d . . . H44A H 0.3956 -0.0179 0.2697 0.276 Uiso 1 1 calc R . . H44B H 0.4502 -0.0737 0.2540 0.276 Uiso 1 1 calc R . . H44C H 0.3759 -0.0778 0.2164 0.276 Uiso 1 1 calc R . . C45 C 0.5726(5) 0.1848(8) 0.3981(3) 0.076(3) Uani 1 1 d . . . H45A H 0.5741 0.1082 0.4022 0.091 Uiso 1 1 d R . . H45B H 0.6166 0.2134 0.4127 0.091 Uiso 1 1 d R . . C46 C 0.5464(5) 0.3112(6) 0.4551(3) 0.059(3) Uani 1 1 d . . . C47 C 0.4732(4) 0.1722(7) 0.4284(4) 0.062(3) Uani 1 1 d . . . H47A H 0.4441 0.1720 0.3927 0.074 Uiso 1 1 d R . . H47B H 0.4821 0.0996 0.4407 0.074 Uiso 1 1 d R . . C48 C 0.4491(4) 0.2467(6) 0.4597(3) 0.055(2) Uani 1 1 d . . . H48A H 0.4487 0.2125 0.4905 0.066 Uiso 1 1 d R . . H48B H 0.4072 0.2810 0.4421 0.066 Uiso 1 1 d R . . C49 C 0.4965(4) 0.4200(7) 0.5087(4) 0.065(3) Uani 1 1 d . . . H49A H 0.4775 0.3969 0.5331 0.078 Uiso 1 1 d R . . H49B H 0.5416 0.4413 0.5268 0.078 Uiso 1 1 d R . . C50 C 0.4530(4) 0.5144(6) 0.4736(3) 0.046(2) Uani 1 1 d . . . C51 C 0.3837(4) 0.5252(8) 0.4640(3) 0.063(3) Uani 1 1 d . . . C52 C 0.3531(4) 0.6145(6) 0.4387(3) 0.051(3) Uani 1 1 d . . . C53 C 0.3856(5) 0.6865(7) 0.4215(3) 0.064(3) Uani 1 1 d . . . H53 H 0.3643 0.7509 0.4044 0.077 Uiso 1 1 d R . . C54 C 0.4524(4) 0.6778(7) 0.4283(4) 0.070(3) Uani 1 1 d . . . C55 C 0.4827(4) 0.5927(6) 0.4598(4) 0.060(3) Uani 1 1 d . . . H55 H 0.5299 0.5967 0.4700 0.072 Uiso 1 1 d R . . C56 C 0.4865(5) 0.7598(8) 0.4104(4) 0.190(8) Uani 1 1 d D . . C57 C 0.4406(7) 0.8269(12) 0.3569(5) 0.341(7) Uani 1 1 d D . . H57A H 0.4086 0.7790 0.3337 0.512 Uiso 1 1 calc R . . H57B H 0.4688 0.8549 0.3401 0.512 Uiso 1 1 calc R . . H57C H 0.4181 0.8852 0.3661 0.512 Uiso 1 1 calc R . . C58 C 0.5254(7) 0.8548(12) 0.4570(6) 0.341(7) Uani 1 1 d D . . H58A H 0.5541 0.8195 0.4878 0.512 Uiso 1 1 calc R . . H58B H 0.4927 0.8958 0.4647 0.512 Uiso 1 1 calc R . . H58C H 0.5510 0.9020 0.4443 0.512 Uiso 1 1 calc R . . C59 C 0.5500(6) 0.6987(13) 0.3983(6) 0.341(7) Uani 1 1 d D . . H59A H 0.5777 0.6610 0.4287 0.512 Uiso 1 1 calc R . . H59B H 0.5756 0.7522 0.3891 0.512 Uiso 1 1 calc R . . H59C H 0.5321 0.6487 0.3702 0.512 Uiso 1 1 calc R . . C60 C 0.2766(3) 0.6322(6) 0.4250(3) 0.048(2) Uani 1 1 d . . . H60A H 0.2649 0.6009 0.4525 0.058 Uiso 1 1 calc R . . H60B H 0.2685 0.7090 0.4249 0.058 Uiso 1 1 calc R . . O5 O 0.4145(7) 0.4253(10) 0.3405(4) 0.104(5) Uani 0.50 1 d PD . . O6 O 0.3535(4) 0.3982(6) 0.2551(3) 0.053(3) Uani 0.50 1 d PD . . C61 C 0.3666(6) 0.4674(9) 0.2958(5) 0.061(2) Uani 0.50 1 d PD . . C62 C 0.3101(6) 0.4273(11) 0.2068(7) 0.061(2) Uani 0.50 1 d PD . . H62A H 0.3137 0.5042 0.2023 0.073 Uiso 0.50 1 calc PR . . H62B H 0.3225 0.3909 0.1808 0.073 Uiso 0.50 1 calc PR . . C63 C 0.2500(5) 0.4041(12) 0.1998(6) 0.061(2) Uani 0.50 1 d PD . . H63A H 0.2224 0.4176 0.1644 0.092 Uiso 0.50 1 calc PR . . H63B H 0.2355 0.4478 0.2221 0.092 Uiso 0.50 1 calc PR . . H63C H 0.2470 0.3296 0.2077 0.092 Uiso 0.50 1 calc PR . . C64 C 0.3367(8) 0.5586(7) 0.2766(8) 0.061(2) Uani 0.50 1 d PD . . H64A H 0.3436 0.6094 0.3042 0.092 Uiso 0.50 1 calc PR . . H64B H 0.2901 0.5460 0.2594 0.092 Uiso 0.50 1 calc PR . . H64C H 0.3545 0.5870 0.2523 0.092 Uiso 0.50 1 calc PR . . O7 O 0.3248(5) -0.0038(8) 0.0143(7) 0.350(8) Uani 1 1 d D . . C65 C 0.3296(7) 0.1066(10) 0.0229(9) 0.358(11) Uani 1 1 d D . . H65A H 0.3254 0.1228 0.0557 0.430 Uiso 1 1 calc R . . H65B H 0.2942 0.1431 -0.0043 0.430 Uiso 1 1 calc R . . C66 C 0.3946(8) 0.1445(16) 0.0236(10) 0.358(11) Uani 1 1 d D . . H66A H 0.4222 0.1638 0.0584 0.538 Uiso 1 1 calc R . . H66B H 0.3882 0.2062 0.0015 0.538 Uiso 1 1 calc R . . H66C H 0.4154 0.0882 0.0115 0.538 Uiso 1 1 calc R . . C67 C 0.2832(9) -0.0510(12) 0.0372(7) 0.358(11) Uani 1 1 d D . . H67A H 0.2520 0.0015 0.0406 0.430 Uiso 1 1 calc R . . H67B H 0.3092 -0.0788 0.0713 0.430 Uiso 1 1 calc R . . C68 C 0.2473(12) -0.1408(14) 0.0018(9) 0.358(11) Uani 1 1 d D . . H68A H 0.2074 -0.1576 0.0076 0.538 Uiso 1 1 calc R . . H68B H 0.2752 -0.2033 0.0086 0.538 Uiso 1 1 calc R . . H68C H 0.2362 -0.1189 -0.0336 0.538 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0806(13) 0.0891(16) 0.0704(16) 0.0018(13) 0.0351(12) -0.0165(13) S4 0.0676(13) 0.0868(16) 0.0838(18) -0.0057(14) 0.0296(12) -0.0066(12) S3 0.0863(16) 0.0816(16) 0.0547(15) -0.0094(13) 0.0234(13) 0.0192(14) S2 0.0558(12) 0.0920(16) 0.0595(15) 0.0013(14) 0.0129(11) 0.0252(12) O1 0.105(4) 0.095(4) 0.069(4) -0.033(3) 0.034(3) 0.011(4) O2 0.051(3) 0.075(4) 0.067(4) -0.015(3) 0.009(3) 0.001(3) O3 0.099(4) 0.126(5) 0.059(4) -0.023(4) 0.024(4) -0.054(4) O4 0.091(3) 0.071(4) 0.071(4) 0.017(3) 0.058(3) -0.004(3) N1 0.069(4) 0.067(4) 0.056(4) 0.011(3) 0.032(3) 0.001(3) N2 0.090(5) 0.089(5) 0.059(5) -0.014(4) 0.031(4) -0.023(4) N3 0.062(4) 0.084(5) 0.066(5) -0.005(4) 0.018(4) 0.015(4) N4 0.047(3) 0.051(3) 0.063(5) -0.008(3) 0.008(3) 0.002(3) N5 0.061(4) 0.068(4) 0.050(5) -0.006(4) 0.013(4) 0.008(4) N6 0.061(4) 0.065(4) 0.034(4) 0.001(3) 0.004(3) -0.008(3) N7 0.054(3) 0.058(4) 0.067(5) -0.001(3) 0.035(3) -0.004(3) N8 0.064(4) 0.077(5) 0.047(4) -0.003(4) 0.034(3) -0.013(4) C1 0.044(4) 0.061(5) 0.041(4) -0.003(4) 0.018(3) 0.005(3) C2 0.106(6) 0.054(4) 0.063(6) 0.029(4) 0.023(5) 0.031(5) C3 0.069(5) 0.100(6) 0.026(4) 0.021(5) -0.006(4) 0.014(5) C4 0.056(4) 0.085(5) 0.044(5) -0.023(4) 0.013(4) -0.001(4) C5 0.048(4) 0.083(5) 0.039(5) 0.009(4) 0.009(4) -0.001(4) C6 0.086(6) 0.148(8) 0.041(5) -0.033(6) 0.022(5) -0.057(6) C7 0.081(6) 0.056(5) 0.109(8) -0.016(5) 0.031(6) 0.004(5) C8 0.067(5) 0.091(6) 0.060(6) 0.000(5) 0.013(5) -0.030(5) C9 0.072(5) 0.052(4) 0.047(5) 0.011(4) 0.004(4) -0.003(4) C10 0.073(4) 0.096(6) 0.074(5) 0.023(5) 0.058(4) 0.023(5) C11 0.071(6) 0.098(6) 0.083(7) 0.044(6) -0.035(6) 0.002(5) C12 0.119(8) 0.116(7) 0.077(8) 0.001(6) -0.004(7) -0.063(6) C13 0.097(8) 0.085(7) 0.209(16) 0.022(9) -0.035(10) -0.031(7) C14 0.159(10) 0.072(6) 0.131(11) 0.026(7) 0.040(9) 0.025(7) C15 0.034(4) 0.061(5) 0.093(7) 0.004(5) 0.011(4) 0.002(4) C16 0.029(3) 0.084(5) 0.046(5) -0.025(4) 0.006(3) 0.005(4) C17 0.076(5) 0.067(5) 0.094(7) 0.030(5) 0.035(5) 0.025(5) C18 0.068(5) 0.111(7) 0.057(6) -0.028(5) -0.002(5) 0.034(5) C19 0.056(4) 0.063(5) 0.046(5) 0.011(4) 0.015(4) -0.001(4) C20 0.063(5) 0.062(5) 0.056(5) -0.013(4) 0.009(4) 0.008(4) C21 0.052(4) 0.034(3) 0.048(5) -0.005(3) 0.017(3) 0.002(3) C22 0.072(4) 0.062(5) 0.040(4) -0.001(4) 0.033(3) 0.008(4) C23 0.052(4) 0.045(4) 0.082(6) -0.025(4) 0.009(4) 0.022(4) C24 0.093(5) 0.029(4) 0.098(7) -0.016(4) 0.043(5) -0.016(4) C25 0.071(5) 0.081(5) 0.039(4) -0.008(4) 0.023(4) 0.021(4) C26 0.065(4) 0.041(4) 0.095(5) 0.008(4) 0.058(3) 0.028(3) C27 0.223(6) 0.083(4) 0.184(6) 0.002(4) 0.142(5) 0.049(4) C28 0.223(6) 0.083(4) 0.184(6) 0.002(4) 0.142(5) 0.049(4) C29 0.223(6) 0.083(4) 0.184(6) 0.002(4) 0.142(5) 0.049(4) C30 0.099(6) 0.072(5) 0.075(6) 0.017(5) 0.029(5) -0.032(5) C31 0.061(4) 0.060(5) 0.066(6) 0.005(4) 0.040(4) 0.010(4) C32 0.051(4) 0.074(6) 0.078(6) 0.015(5) 0.039(4) 0.012(4) C33 0.063(5) 0.075(6) 0.098(7) -0.001(5) 0.047(5) -0.009(5) C34 0.091(6) 0.070(6) 0.082(8) 0.017(5) 0.033(6) 0.024(5) C35 0.057(5) 0.095(7) 0.088(7) 0.027(6) 0.038(5) 0.035(5) C36 0.061(5) 0.052(4) 0.054(5) -0.014(4) 0.014(4) 0.001(4) C37 0.044(4) 0.067(5) 0.049(5) -0.012(4) 0.001(4) 0.030(4) C38 0.057(5) 0.058(5) 0.057(6) 0.018(4) 0.017(4) 0.002(4) C39 0.044(4) 0.083(6) 0.048(5) 0.024(5) 0.018(4) 0.027(4) C40 0.049(4) 0.049(4) 0.057(6) 0.013(4) -0.012(4) 0.021(4) C41 0.107(7) 0.062(5) 0.076(7) 0.034(5) 0.022(6) 0.021(5) C42 0.38(2) 0.176(12) 0.22(2) -0.082(13) 0.122(18) -0.185(14) C43 0.056(8) 0.103(10) 0.54(4) -0.039(16) -0.071(14) 0.021(7) C44 0.092(7) 0.060(6) 0.251(17) 0.004(8) -0.112(9) 0.000(6) C45 0.103(6) 0.084(6) 0.052(5) 0.016(5) 0.043(5) 0.029(5) C46 0.079(6) 0.040(4) 0.046(6) 0.001(4) 0.009(5) 0.001(4) C47 0.062(5) 0.072(5) 0.054(5) 0.014(5) 0.026(4) -0.001(5) C48 0.060(4) 0.051(4) 0.065(5) -0.006(4) 0.036(4) 0.004(4) C49 0.059(5) 0.075(6) 0.056(6) 0.012(5) 0.016(4) -0.004(5) C50 0.054(4) 0.050(4) 0.036(4) 0.003(4) 0.019(4) -0.001(4) C51 0.069(5) 0.086(6) 0.031(5) -0.021(5) 0.017(4) -0.018(5) C52 0.048(4) 0.052(4) 0.041(5) -0.001(4) 0.003(4) 0.003(4) C53 0.105(6) 0.054(5) 0.041(5) 0.006(4) 0.036(4) 0.022(5) C54 0.057(5) 0.082(6) 0.064(6) -0.018(5) 0.015(4) -0.039(4) C55 0.036(4) 0.054(5) 0.087(7) -0.013(5) 0.019(4) 0.001(4) C56 0.117(10) 0.136(10) 0.211(16) 0.097(11) -0.063(10) -0.029(9) C57 0.189(8) 0.406(13) 0.429(15) 0.271(11) 0.114(9) -0.062(10) C58 0.189(8) 0.406(13) 0.429(15) 0.271(11) 0.114(9) -0.062(10) C59 0.189(8) 0.406(13) 0.429(15) 0.271(11) 0.114(9) -0.062(10) C60 0.044(4) 0.050(4) 0.052(5) -0.007(4) 0.018(4) -0.019(3) O5 0.136(11) 0.105(8) 0.021(6) 0.030(6) -0.028(7) -0.029(8) O6 0.050(5) 0.062(5) 0.027(5) -0.001(5) -0.010(4) 0.005(5) C61 0.063(4) 0.050(4) 0.089(5) -0.011(4) 0.050(4) -0.011(4) C62 0.063(4) 0.050(4) 0.089(5) -0.011(4) 0.050(4) -0.011(4) C63 0.063(4) 0.050(4) 0.089(5) -0.011(4) 0.050(4) -0.011(4) C64 0.063(4) 0.050(4) 0.089(5) -0.011(4) 0.050(4) -0.011(4) O7 0.59(2) 0.299(11) 0.230(9) 0.160(9) 0.229(11) 0.133(13) C65 0.48(3) 0.330(13) 0.191(9) 0.154(9) 0.038(13) 0.015(16) C66 0.48(3) 0.330(13) 0.191(9) 0.154(9) 0.038(13) 0.015(16) C67 0.48(3) 0.330(13) 0.191(9) 0.154(9) 0.038(13) 0.015(16) C68 0.48(3) 0.330(13) 0.191(9) 0.154(9) 0.038(13) 0.015(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C1 1.713(9) . ? S4 C46 1.697(9) . ? S3 C31 1.676(10) . ? S2 C16 1.686(8) . ? O1 C10 1.381(10) . ? O1 H1 0.8200 . ? O2 C21 1.369(9) . ? O2 H2 0.8200 . ? O3 C40 1.347(10) . ? O3 H3 0.8200 . ? O4 C51 1.362(11) . ? O4 H4 0.8200 . ? N1 C1 1.308(10) . ? N1 C60 1.399(10) . ? N1 C2 1.491(12) . ? N2 C1 1.357(10) . ? N2 C4 1.385(10) . ? N2 C3 1.413(12) . ? N3 C16 1.407(11) . ? N3 C15 1.451(13) . ? N3 C17 1.461(12) . ? N4 C16 1.324(11) . ? N4 C19 1.420(10) . ? N4 C18 1.506(11) . ? N5 C31 1.345(10) . ? N5 C32 1.451(12) . ? N5 C30 1.560(11) . ? N6 C31 1.327(11) . ? N6 C33 1.492(12) . ? N6 C34 1.517(11) . ? N7 C46 1.317(10) . ? N7 C47 1.443(11) . ? N7 C45 1.466(12) . ? N8 C46 1.336(13) . ? N8 C48 1.443(10) . ? N8 C49 1.493(12) . ? C2 C3 1.475(12) . ? C2 H2A 0.9581 . ? C2 H2B 0.9592 . ? C3 H3A 0.9586 . ? C3 H3B 0.9589 . ? C4 C5 1.545(12) . ? C4 H4A 0.9588 . ? C4 H4B 0.9591 . ? C5 C6 1.345(12) . ? C5 C10 1.381(12) . ? C6 C7 1.462(14) . ? C6 H6 0.9591 . ? C7 C8 1.406(14) . ? C7 C11 1.603(12) . ? C8 C9 1.313(11) . ? C8 H8 0.9581 . ? C9 C10 1.433(12) . ? C9 C15 1.464(12) . ? C11 C14 1.461(15) . ? C11 C13 1.470(14) . ? C11 C12 1.660(18) . ? C12 H12A 0.9587 . ? C12 H12B 0.9591 . ? C12 H12C 0.9583 . ? C13 H13A 0.9586 . ? C13 H13B 0.9584 . ? C13 H13C 0.9590 . ? C14 H14A 0.9588 . ? C14 H14B 0.9590 . ? C14 H14C 0.9590 . ? C15 H15A 0.9590 . ? C15 H15B 0.9579 . ? C17 C18 1.511(15) . ? C17 H17A 0.9592 . ? C17 H17B 0.9581 . ? C18 H18A 0.9590 . ? C18 H18B 0.9590 . ? C19 C20 1.448(11) . ? C19 H19A 0.9589 . ? C19 H19B 0.9591 . ? C20 C21 1.353(11) . ? C20 C25 1.503(12) . ? C21 C22 1.469(10) . ? C22 C30 1.393(13) . ? C22 C23 1.462(11) . ? C23 C24 1.413(12) . ? C23 H23 0.9584 . ? C24 C25 1.455(11) . ? C24 C26 1.465(12) . ? C25 H25 0.9591 . ? C26 C28 1.430(15) . ? C26 C27 1.484(13) . ? C26 C29 1.562(14) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C32 C33 1.556(12) . ? C32 H32A 0.9581 . ? C32 H32B 0.9591 . ? C33 H33A 0.9589 . ? C33 H33B 0.9589 . ? C34 C35 1.479(15) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.386(12) . ? C35 C40 1.407(14) . ? C36 C37 1.383(13) . ? C36 H36 0.9592 . ? C37 C38 1.367(12) . ? C37 C41 1.469(13) . ? C38 C39 1.462(11) . ? C38 H38 0.9586 . ? C39 C40 1.310(12) . ? C39 C45 1.599(12) . ? C41 C42 1.52(3) . ? C41 C44 1.536(16) . ? C41 C43 1.597(17) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9580 . ? C45 H45B 0.9592 . ? C47 C48 1.489(13) . ? C47 H47A 0.9594 . ? C47 H47B 0.9580 . ? C48 H48A 0.9588 . ? C48 H48B 0.9591 . ? C49 C50 1.595(11) . ? C49 H49A 0.9588 . ? C49 H49B 0.9591 . ? C50 C55 1.299(12) . ? C50 C51 1.435(12) . ? C51 C52 1.350(12) . ? C52 C53 1.334(13) . ? C52 C60 1.578(11) . ? C53 C54 1.397(13) . ? C53 H53 0.9584 . ? C54 C55 1.376(12) . ? C54 C56 1.451(15) . ? C55 H55 0.9589 . ? C56 C57 1.676(13) . ? C56 C59 1.711(15) . ? C56 C58 1.725(14) . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? O5 C61 1.396(13) . ? O6 C61 1.364(16) . ? O6 C62 1.373(17) . ? C61 C64 1.318(14) . ? C62 C63 1.280(14) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? O7 C65 1.390(14) . ? O7 C67 1.411(16) . ? C65 C66 1.481(17) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C67 C68 1.503(17) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 O1 H1 109.5 . . ? C21 O2 H2 109.5 . . ? C40 O3 H3 109.5 . . ? C51 O4 H4 109.5 . . ? C1 N1 C60 126.1(7) . . ? C1 N1 C2 110.8(7) . . ? C60 N1 C2 123.0(7) . . ? C1 N2 C4 131.3(8) . . ? C1 N2 C3 106.6(7) . . ? C4 N2 C3 119.8(7) . . ? C16 N3 C15 130.3(7) . . ? C16 N3 C17 110.4(7) . . ? C15 N3 C17 119.3(7) . . ? C16 N4 C19 124.5(7) . . ? C16 N4 C18 111.2(7) . . ? C19 N4 C18 124.1(8) . . ? C31 N5 C32 111.6(7) . . ? C31 N5 C30 127.1(8) . . ? C32 N5 C30 121.3(7) . . ? C31 N6 C33 116.7(7) . . ? C31 N6 C34 120.9(8) . . ? C33 N6 C34 122.1(7) . . ? C46 N7 C47 111.2(8) . . ? C46 N7 C45 122.6(8) . . ? C47 N7 C45 126.2(7) . . ? C46 N8 C48 112.2(7) . . ? C46 N8 C49 126.9(7) . . ? C48 N8 C49 120.9(7) . . ? N1 C1 N2 112.3(7) . . ? N1 C1 S1 126.1(6) . . ? N2 C1 S1 121.6(6) . . ? C3 C2 N1 99.6(7) . . ? C3 C2 H2A 108.9 . . ? N1 C2 H2A 105.4 . . ? C3 C2 H2B 118.6 . . ? N1 C2 H2B 113.7 . . ? H2A C2 H2B 109.5 . . ? N2 C3 C2 109.4(7) . . ? N2 C3 H3A 106.1 . . ? C2 C3 H3A 106.1 . . ? N2 C3 H3B 109.5 . . ? C2 C3 H3B 115.7 . . ? H3A C3 H3B 109.5 . . ? N2 C4 C5 112.9(7) . . ? N2 C4 H4A 103.3 . . ? C5 C4 H4A 100.6 . . ? N2 C4 H4B 120.0 . . ? C5 C4 H4B 108.6 . . ? H4A C4 H4B 109.5 . . ? C6 C5 C10 115.4(9) . . ? C6 C5 C4 122.9(8) . . ? C10 C5 C4 121.7(7) . . ? C5 C6 C7 125.6(9) . . ? C5 C6 H6 118.1 . . ? C7 C6 H6 114.9 . . ? C8 C7 C6 113.3(8) . . ? C8 C7 C11 123.4(9) . . ? C6 C7 C11 121.5(9) . . ? C9 C8 C7 123.0(10) . . ? C9 C8 H8 121.0 . . ? C7 C8 H8 115.3 . . ? C8 C9 C10 120.1(8) . . ? C8 C9 C15 117.8(8) . . ? C10 C9 C15 122.1(7) . . ? O1 C10 C5 116.2(8) . . ? O1 C10 C9 122.0(8) . . ? C5 C10 C9 121.8(8) . . ? C14 C11 C13 125.3(11) . . ? C14 C11 C7 111.4(8) . . ? C13 C11 C7 112.4(8) . . ? C14 C11 C12 99.7(9) . . ? C13 C11 C12 102.9(11) . . ? C7 C11 C12 100.4(9) . . ? C11 C12 H12A 98.8 . . ? C11 C12 H12B 117.4 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 111.6 . . ? H12A C12 H12C 109.4 . . ? H12B C12 H12C 109.4 . . ? C11 C13 H13A 104.3 . . ? C11 C13 H13B 105.3 . . ? H13A C13 H13B 109.4 . . ? C11 C13 H13C 118.4 . . ? H13A C13 H13C 109.4 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 110.5 . . ? C11 C14 H14B 100.8 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 116.7 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 C9 113.5(7) . . ? N3 C15 H15A 107.3 . . ? C9 C15 H15A 105.6 . . ? N3 C15 H15B 110.5 . . ? C9 C15 H15B 110.3 . . ? H15A C15 H15B 109.4 . . ? N4 C16 N3 109.9(7) . . ? N4 C16 S2 127.5(7) . . ? N3 C16 S2 122.6(7) . . ? N3 C17 C18 104.6(7) . . ? N3 C17 H17A 112.8 . . ? C18 C17 H17A 112.9 . . ? N3 C17 H17B 108.1 . . ? C18 C17 H17B 108.8 . . ? H17A C17 H17B 109.5 . . ? N4 C18 C17 103.6(8) . . ? N4 C18 H18A 110.5 . . ? C17 C18 H18A 113.6 . . ? N4 C18 H18B 109.5 . . ? C17 C18 H18B 110.1 . . ? H18A C18 H18B 109.4 . . ? N4 C19 C20 116.8(7) . . ? N4 C19 H19A 106.9 . . ? C20 C19 H19A 105.0 . . ? N4 C19 H19B 114.1 . . ? C20 C19 H19B 104.1 . . ? H19A C19 H19B 109.5 . . ? C21 C20 C19 125.2(8) . . ? C21 C20 C25 120.4(7) . . ? C19 C20 C25 114.0(8) . . ? C20 C21 O2 117.7(6) . . ? C20 C21 C22 123.5(7) . . ? O2 C21 C22 118.3(7) . . ? C30 C22 C23 121.7(8) . . ? C30 C22 C21 122.2(8) . . ? C23 C22 C21 115.8(7) . . ? C24 C23 C22 121.8(7) . . ? C24 C23 H23 122.1 . . ? C22 C23 H23 115.8 . . ? C23 C24 C25 121.0(8) . . ? C23 C24 C26 120.9(7) . . ? C25 C24 C26 118.1(8) . . ? C24 C25 C20 116.9(8) . . ? C24 C25 H25 116.2 . . ? C20 C25 H25 126.6 . . ? C28 C26 C24 110.0(7) . . ? C28 C26 C27 114.5(9) . . ? C24 C26 C27 111.8(8) . . ? C28 C26 C29 114.4(8) . . ? C24 C26 C29 107.4(8) . . ? C27 C26 C29 98.2(7) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C22 C30 N5 113.2(8) . . ? C22 C30 H30A 108.9 . . ? N5 C30 H30A 108.9 . . ? C22 C30 H30B 108.9 . . ? N5 C30 H30B 108.9 . . ? H30A C30 H30B 107.8 . . ? N6 C31 N5 107.9(8) . . ? N6 C31 S3 131.1(7) . . ? N5 C31 S3 121.0(7) . . ? N5 C32 C33 106.6(7) . . ? N5 C32 H32A 110.4 . . ? C33 C32 H32A 111.6 . . ? N5 C32 H32B 109.3 . . ? C33 C32 H32B 109.4 . . ? H32A C32 H32B 109.5 . . ? N6 C33 C32 97.3(7) . . ? N6 C33 H33A 110.0 . . ? C32 C33 H33A 116.0 . . ? N6 C33 H33B 110.0 . . ? C32 C33 H33B 113.5 . . ? H33A C33 H33B 109.4 . . ? C35 C34 N6 114.0(9) . . ? C35 C34 H34A 108.8 . . ? N6 C34 H34A 108.8 . . ? C35 C34 H34B 108.8 . . ? N6 C34 H34B 108.8 . . ? H34A C34 H34B 107.7 . . ? C36 C35 C40 119.6(9) . . ? C36 C35 C34 117.2(9) . . ? C40 C35 C34 123.1(9) . . ? C35 C36 C37 121.5(9) . . ? C35 C36 H36 115.4 . . ? C37 C36 H36 122.3 . . ? C38 C37 C36 116.9(8) . . ? C38 C37 C41 123.0(9) . . ? C36 C37 C41 119.5(9) . . ? C37 C38 C39 121.8(8) . . ? C37 C38 H38 120.2 . . ? C39 C38 H38 116.4 . . ? C40 C39 C38 118.3(8) . . ? C40 C39 C45 121.8(8) . . ? C38 C39 C45 119.8(8) . . ? C39 C40 O3 123.4(8) . . ? C39 C40 C35 121.1(8) . . ? O3 C40 C35 115.1(8) . . ? C37 C41 C42 113.0(11) . . ? C37 C41 C44 114.6(9) . . ? C42 C41 C44 113.4(11) . . ? C37 C41 C43 105.2(9) . . ? C42 C41 C43 110.2(14) . . ? C44 C41 C43 99.1(12) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N7 C45 C39 113.3(7) . . ? N7 C45 H45A 105.0 . . ? C39 C45 H45A 106.8 . . ? N7 C45 H45B 110.6 . . ? C39 C45 H45B 111.3 . . ? H45A C45 H45B 109.4 . . ? N7 C46 N8 109.4(8) . . ? N7 C46 S4 124.7(8) . . ? N8 C46 S4 125.8(6) . . ? N7 C47 C48 104.6(7) . . ? N7 C47 H47A 102.8 . . ? C48 C47 H47A 111.4 . . ? N7 C47 H47B 111.1 . . ? C48 C47 H47B 116.5 . . ? H47A C47 H47B 109.5 . . ? N8 C48 C47 102.4(7) . . ? N8 C48 H48A 107.6 . . ? C47 C48 H48A 111.4 . . ? N8 C48 H48B 108.5 . . ? C47 C48 H48B 116.9 . . ? H48A C48 H48B 109.5 . . ? N8 C49 C50 109.6(7) . . ? N8 C49 H49A 110.3 . . ? C50 C49 H49A 109.9 . . ? N8 C49 H49B 105.3 . . ? C50 C49 H49B 112.2 . . ? H49A C49 H49B 109.5 . . ? C55 C50 C51 118.4(8) . . ? C55 C50 C49 119.0(7) . . ? C51 C50 C49 121.7(8) . . ? C52 C51 O4 129.2(8) . . ? C52 C51 C50 117.1(9) . . ? O4 C51 C50 113.7(8) . . ? C53 C52 C51 120.9(8) . . ? C53 C52 C60 118.0(7) . . ? C51 C52 C60 120.9(8) . . ? C52 C53 C54 124.1(8) . . ? C52 C53 H53 121.0 . . ? C54 C53 H53 114.9 . . ? C55 C54 C53 112.0(9) . . ? C55 C54 C56 125.0(8) . . ? C53 C54 C56 122.3(9) . . ? C50 C55 C54 126.1(8) . . ? C50 C55 H55 123.0 . . ? C54 C55 H55 110.8 . . ? C54 C56 C57 116.2(9) . . ? C54 C56 C59 107.8(9) . . ? C57 C56 C59 107.8(9) . . ? C54 C56 C58 113.2(10) . . ? C57 C56 C58 107.0(8) . . ? C59 C56 C58 104.2(8) . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C56 C58 H58A 109.5 . . ? C56 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C56 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C56 C59 H59A 109.5 . . ? C56 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C56 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? N1 C60 C52 116.6(7) . . ? N1 C60 H60A 108.2 . . ? C52 C60 H60A 108.2 . . ? N1 C60 H60B 108.1 . . ? C52 C60 H60B 108.1 . . ? H60A C60 H60B 107.3 . . ? C61 O6 C62 120.1(10) . . ? C64 C61 O6 106.6(12) . . ? C64 C61 O5 141.0(14) . . ? O6 C61 O5 111.2(10) . . ? C63 C62 O6 112.6(14) . . ? C63 C62 H62A 109.1 . . ? O6 C62 H62A 109.1 . . ? C63 C62 H62B 109.1 . . ? O6 C62 H62B 109.1 . . ? H62A C62 H62B 107.8 . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C65 O7 C67 110.6(14) . . ? O7 C65 C66 109.1(14) . . ? O7 C65 H65A 109.9 . . ? C66 C65 H65A 109.9 . . ? O7 C65 H65B 109.9 . . ? C66 C65 H65B 109.9 . . ? H65A C65 H65B 108.3 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? O7 C67 C68 106.1(15) . . ? O7 C67 H67A 110.5 . . ? C68 C67 H67A 110.5 . . ? O7 C67 H67B 110.5 . . ? C68 C67 H67B 110.5 . . ? H67A C67 H67B 108.7 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? loop_ # start Validation Reply Form _vrf_PLAT220_keinan-49 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 9.05 Ratio RESPONSE: Unresolved disorder at the solvent molecules ; _vrf_PLAT222_keinan-49 ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 8.64 Ratio RESPONSE: Unresolved disorder at the solvent molecules ; _vrf_PLAT242_keinan-49 ; PROBLEM: Check Low Ueq as Compared to Neighbors for C26 RESPONSE: C26 is connected to slightly disorderd t-butyl group ; _vrf_PLAT413_keinan-49 ; PROBLEM: Short Inter XH3 .. XHn H32B..H64C ..1.75 Ang. RESPONSE: Unresolved disorder at the solvent molecules ; _vrf_PLAT234_keinan-49 ; PROBLEM: Large Hirshfeld Difference C41 -- C42 .. 0.31 Ang. RESPONSE: C41 is connected to slightly disorderd t-butyl group ; # end Validation Reply Form _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.881 _refine_diff_density_min -0.299 _refine_diff_density_rms 0.089 _database_code_depnum_ccdc_archive 'CCDC 952889' data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H70 N6 O4 S3' _chemical_formula_weight 903.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 31' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' _cell_length_a 12.741(1) _cell_length_b 12.741(1) _cell_length_c 27.303(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3838.4(6) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 158 _cell_measurement_theta_min 2.88 _cell_measurement_theta_max 21.23 _exptl_crystal_description cube _exptl_crystal_colour colorless _exptl_crystal_size_max 0.73 _exptl_crystal_size_mid 0.58 _exptl_crystal_size_min 0.46 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.172 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1458 _exptl_absorpt_coefficient_mu 0.192 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.875 _exptl_absorpt_correction_T_max 0.915 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX2 DUO' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 37973 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.68 _reflns_number_total 9738 _reflns_number_gt 7221 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Instrument Service v2010.7.0.0' _computing_cell_refinement 'APEX2 v2010.7-0 (Bruker AXS)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury 2.4' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1422P)^2^+0.1183P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.12(9) _refine_ls_number_reflns 9738 _refine_ls_number_parameters 559 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0914 _refine_ls_R_factor_gt 0.0673 _refine_ls_wR_factor_ref 0.2091 _refine_ls_wR_factor_gt 0.1920 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S -0.15228(14) 0.49764(12) -0.04885(5) 0.0840(4) Uani 1 1 d . . . S2 S 0.26867(16) 0.15822(13) 0.03058(5) 0.0898(4) Uani 1 1 d . . . S3 S -0.36772(14) -0.04273(14) 0.15699(10) 0.1272(9) Uani 1 1 d . . . N1 N -0.2403(4) 0.2924(3) 0.00487(14) 0.0663(9) Uani 1 1 d . . . N2 N -0.0658(3) 0.3475(3) -0.03042(16) 0.0701(10) Uani 1 1 d . . . N3 N 0.3949(3) 0.3861(3) 0.06520(16) 0.0708(9) Uani 1 1 d . . . N4 N 0.3467(3) 0.2441(4) 0.12031(14) 0.0689(9) Uani 1 1 d . . . N5 N -0.1511(3) 0.0805(3) 0.19978(13) 0.0555(7) Uani 1 1 d . . . N6 N -0.2697(3) 0.1549(4) 0.21598(14) 0.0664(9) Uani 1 1 d . . . O1 O 0.1833(3) 0.3114(3) -0.03283(13) 0.0757(8) Uani 1 1 d . . . H1 H 0.2219 0.2716 -0.0207 0.091 Uiso 1 1 d R . . O2 O 0.0603(3) 0.0726(3) 0.11919(11) 0.0791(9) Uani 1 1 d . . . H2 H 0.1212 0.0942 0.0953 0.095 Uiso 1 1 d R . . O3 O -0.4298(3) 0.1307(3) 0.10183(15) 0.0826(10) Uani 1 1 d . . . H3 H -0.4122 0.0859 0.1168 0.099 Uiso 1 1 calc R . . C1 C -0.1525(4) 0.3775(4) -0.02361(16) 0.0616(10) Uani 1 1 d . . . C2 C -0.2082(5) 0.2053(4) 0.0226(2) 0.0824(14) Uani 1 1 d . . . H2A H -0.2707 0.1231 0.0150 0.099 Uiso 1 1 calc R . . H2B H -0.1948 0.2127 0.0577 0.099 Uiso 1 1 calc R . . C3 C -0.0935(4) 0.2390(4) -0.00442(18) 0.0692(11) Uani 1 1 d . . . H3A H -0.0289 0.2535 0.0182 0.083 Uiso 1 1 calc R . . H3B H -0.1052 0.1752 -0.0270 0.083 Uiso 1 1 calc R . . C4 C 0.0409(4) 0.4109(4) -0.06072(17) 0.0669(10) Uani 1 1 d . . . H4A H 0.0307 0.4659 -0.0821 0.080 Uiso 1 1 calc R . . H4B H 0.0477 0.3523 -0.0812 0.080 Uiso 1 1 calc R . . C5 C 0.1566(4) 0.4817(3) -0.03261(13) 0.0545(9) Uani 1 1 d . . . C6 C 0.2251(4) 0.4294(3) -0.01926(14) 0.0553(9) Uani 1 1 d . . . C7 C 0.3355(4) 0.4985(4) 0.00551(16) 0.0596(9) Uani 1 1 d . . . C8 C 0.3708(4) 0.6174(4) 0.01754(16) 0.0617(10) Uani 1 1 d . . . H8 H 0.4435 0.6629 0.0342 0.074 Uiso 1 1 d R . . C9 C 0.3017(4) 0.6712(3) 0.00600(15) 0.0611(10) Uani 1 1 d . . . C10 C 0.1955(4) 0.6013(4) -0.01936(15) 0.0611(9) Uani 1 1 d . . . H10 H 0.1481 0.6351 -0.0280 0.073 Uiso 1 1 calc R . . C11 C 0.3430(5) 0.8037(4) 0.01970(18) 0.0728(12) Uani 1 1 d . . . C12 C 0.321(2) 0.8114(9) 0.0717(5) 0.278(12) Uani 1 1 d . . . H12A H 0.3626 0.7804 0.0908 0.334 Uiso 1 1 calc R . . H12B H 0.2354 0.7645 0.0782 0.334 Uiso 1 1 calc R . . H12C H 0.3498 0.8945 0.0804 0.334 Uiso 1 1 calc R . . C13 C 0.4669(12) 0.8863(7) 0.0031(7) 0.260(10) Uani 1 1 d . . . H13A H 0.5207 0.8620 0.0169 0.312 Uiso 1 1 calc R . . H13B H 0.4911 0.9673 0.0133 0.312 Uiso 1 1 calc R . . H13C H 0.4700 0.8836 -0.0320 0.312 Uiso 1 1 calc R . . C14 C 0.2658(18) 0.8471(9) -0.0016(7) 0.258(10) Uani 1 1 d . . . H14A H 0.2685 0.8437 -0.0367 0.309 Uiso 1 1 calc R . . H14B H 0.2946 0.9292 0.0085 0.309 Uiso 1 1 calc R . . H14C H 0.1839 0.7967 0.0094 0.309 Uiso 1 1 calc R . . C15 C 0.4172(4) 0.4472(4) 0.01747(19) 0.0701(11) Uani 1 1 d . . . H15A H 0.4077 0.3899 -0.0079 0.084 Uiso 1 1 calc R . . H15B H 0.5007 0.5128 0.0166 0.084 Uiso 1 1 calc R . . C16 C 0.3401(4) 0.2675(4) 0.07225(18) 0.0644(10) Uani 1 1 d . . . C17 C 0.4509(5) 0.4525(5) 0.1093(2) 0.0838(14) Uani 1 1 d . . . H17A H 0.4205 0.5063 0.1178 0.101 Uiso 1 1 d R . . H17B H 0.5384 0.4996 0.1060 0.101 Uiso 1 1 d R . . C18 C 0.4149(5) 0.3550(5) 0.1469(2) 0.0832(14) Uani 1 1 d . . . H18A H 0.4859 0.3590 0.1619 0.100 Uiso 1 1 calc R . . H18B H 0.3657 0.3624 0.1723 0.100 Uiso 1 1 calc R . . C19 C 0.3082(5) 0.1247(5) 0.14023(19) 0.0794(14) Uani 1 1 d . . . H19A H 0.3776 0.1248 0.1550 0.095 Uiso 1 1 calc R . . H19B H 0.2797 0.0664 0.1136 0.095 Uiso 1 1 calc R . . C20 C 0.2084(4) 0.0843(4) 0.17838(16) 0.0590(9) Uani 1 1 d . . . C21 C 0.0916(4) 0.0583(3) 0.16522(15) 0.0552(9) Uani 1 1 d . . . C22 C -0.0006(3) 0.0142(3) 0.20067(15) 0.0520(8) Uani 1 1 d . . . C23 C 0.0273(3) -0.0035(3) 0.24792(15) 0.0557(9) Uani 1 1 d . . . H23 H -0.0344 -0.0337 0.2711 0.067 Uiso 1 1 calc R . . C24 C 0.1416(3) 0.0211(3) 0.26277(15) 0.0512(8) Uani 1 1 d . . . C25 C 0.2298(3) 0.0654(3) 0.22716(16) 0.0579(10) Uani 1 1 d . . . H25 H 0.3078 0.0837 0.2359 0.069 Uiso 1 1 calc R . . C26 C 0.1651(4) 0.0061(4) 0.31637(18) 0.0704(11) Uani 1 1 d . . . C27 C 0.2864(5) 0.0140(7) 0.3239(2) 0.0955(17) Uani 1 1 d . . . H27A H 0.3495 0.0894 0.3110 0.115 Uiso 1 1 calc R . . H27B H 0.2870 -0.0520 0.3072 0.115 Uiso 1 1 calc R . . H27C H 0.2997 0.0096 0.3582 0.115 Uiso 1 1 calc R . . C28 C 0.0672(7) -0.1094(8) 0.3373(3) 0.142(4) Uani 1 1 d . . . H28A H -0.0095 -0.1134 0.3330 0.170 Uiso 1 1 calc R . . H28B H 0.0820 -0.1129 0.3716 0.170 Uiso 1 1 calc R . . H28C H 0.0660 -0.1766 0.3208 0.170 Uiso 1 1 calc R . . C29 C 0.1717(7) 0.1148(8) 0.3451(3) 0.112(2) Uani 1 1 d . . . H29A H 0.2323 0.1894 0.3307 0.134 Uiso 1 1 calc R . . H29B H 0.1924 0.1113 0.3787 0.134 Uiso 1 1 calc R . . H29C H 0.0944 0.1106 0.3437 0.134 Uiso 1 1 calc R . . C30 C -0.1268(3) -0.0162(4) 0.18789(17) 0.0588(9) Uani 1 1 d . . . H30A H -0.1397 -0.0333 0.1531 0.071 Uiso 1 1 calc R . . H30B H -0.1837 -0.0889 0.2054 0.071 Uiso 1 1 calc R . . C31 C -0.2607(3) 0.0678(4) 0.19132(18) 0.0624(10) Uani 1 1 d . . . C32 C -0.0842(5) 0.1750(5) 0.23570(18) 0.0742(12) Uani 1 1 d . . . H32A H -0.0013 0.2281 0.2253 0.089 Uiso 1 1 calc R . . H32B H -0.0840 0.1408 0.2674 0.089 Uiso 1 1 calc R . . C33 C -0.1538(5) 0.2414(5) 0.23735(17) 0.0714(11) Uani 1 1 d . . . H33A H -0.1636 0.2611 0.2708 0.086 Uiso 1 1 calc R . . H33B H -0.1139 0.3154 0.2182 0.086 Uiso 1 1 calc R . . C34 C -0.3641(4) 0.1871(5) 0.2063(2) 0.0728(12) Uani 1 1 d . . . H34A H -0.3793 0.2192 0.2360 0.087 Uiso 1 1 calc R . . H34B H -0.4388 0.1147 0.1971 0.087 Uiso 1 1 calc R . . C35 C -0.3274(3) 0.2790(4) 0.16625(17) 0.0597(10) Uani 1 1 d . . . C36 C -0.3568(3) 0.2477(4) 0.11708(17) 0.0593(10) Uani 1 1 d . . . C37 C -0.3135(3) 0.3385(4) 0.08053(16) 0.0588(10) Uani 1 1 d . . . C38 C -0.2423(4) 0.4572(4) 0.09412(15) 0.0576(9) Uani 1 1 d . . . H38 H -0.2146 0.5169 0.0701 0.069 Uiso 1 1 calc R . . C39 C -0.2098(4) 0.4922(4) 0.14324(15) 0.0554(9) Uani 1 1 d . . . C40 C -0.2555(4) 0.4021(4) 0.17797(15) 0.0574(9) Uani 1 1 d . . . H40 H -0.2379 0.4238 0.2107 0.069 Uiso 1 1 calc R . . C41 C -0.1309(5) 0.6258(4) 0.15669(18) 0.0709(11) Uani 1 1 d . . . C42 C -0.0147(5) 0.6836(6) 0.1257(3) 0.1006(18) Uani 1 1 d . . . H42A H -0.0355 0.6678 0.0917 0.121 Uiso 1 1 calc R . . H42B H 0.0348 0.6495 0.1349 0.121 Uiso 1 1 calc R . . H42C H 0.0293 0.7695 0.1313 0.121 Uiso 1 1 calc R . . C43 C -0.2015(6) 0.6922(5) 0.1428(3) 0.105(2) Uani 1 1 d . . . H43A H -0.2267 0.6761 0.1092 0.126 Uiso 1 1 d R . . H43B H -0.1507 0.7779 0.1475 0.126 Uiso 1 1 d R . . H43C H -0.2715 0.6626 0.1635 0.126 Uiso 1 1 d R . . C44 C -0.0935(9) 0.6461(7) 0.2101(2) 0.131(3) Uani 1 1 d . . . H44A H -0.1646 0.6106 0.2304 0.158 Uiso 1 1 calc R . . H44B H -0.0467 0.7315 0.2165 0.158 Uiso 1 1 calc R . . H44C H -0.0456 0.6090 0.2172 0.158 Uiso 1 1 calc R . . C45 C -0.3385(4) 0.3036(4) 0.02788(18) 0.0701(11) Uani 1 1 d . . . H45A H -0.4136 0.2268 0.0252 0.084 Uiso 1 1 calc R . . H45B H -0.3489 0.3641 0.0105 0.084 Uiso 1 1 calc R . . C46 C 0.0821(13) 0.4169(10) 0.1130(4) 0.179(5) Uani 1 1 d D . . H46A H 0.0479 0.3320 0.1064 0.269 Uiso 1 1 calc R . . H46B H 0.1251 0.4627 0.0846 0.269 Uiso 1 1 calc R . . H46C H 0.0184 0.4336 0.1208 0.269 Uiso 1 1 calc R . . C47 C 0.1682(10) 0.4521(14) 0.1555(5) 0.245(9) Uani 1 1 d D . . H47A H 0.2340 0.4366 0.1486 0.294 Uiso 1 1 calc R . . H47B H 0.1268 0.4092 0.1851 0.294 Uiso 1 1 calc R . . C48 C 0.3159(14) 0.6436(17) 0.1889(6) 0.233(10) Uani 1 1 d D . . H48A H 0.3181 0.5935 0.2152 0.279 Uiso 1 1 calc R . . H48B H 0.3889 0.6733 0.1694 0.279 Uiso 1 1 calc R . . C49 C 0.3038(12) 0.7449(17) 0.2084(4) 0.236(11) Uani 1 1 d D . . H49A H 0.3692 0.7916 0.2307 0.355 Uiso 1 1 calc R . . H49B H 0.2280 0.7134 0.2254 0.355 Uiso 1 1 calc R . . H49C H 0.3062 0.7955 0.1819 0.355 Uiso 1 1 calc R . . O5 O 0.2109(12) 0.5781(10) 0.1596(3) 0.234(5) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.1044(10) 0.0742(8) 0.0902(8) 0.0007(6) -0.0222(7) 0.0572(8) S2 0.1151(11) 0.0706(8) 0.0802(8) -0.0035(6) 0.0046(7) 0.0437(8) S3 0.0743(9) 0.0722(8) 0.244(2) -0.0454(11) -0.0774(12) 0.0431(7) N1 0.084(2) 0.061(2) 0.069(2) -0.0118(17) -0.0076(18) 0.047(2) N2 0.057(2) 0.0430(17) 0.107(3) -0.0059(17) -0.0107(19) 0.0227(16) N3 0.058(2) 0.058(2) 0.089(3) -0.0023(18) -0.0118(18) 0.0230(17) N4 0.057(2) 0.072(2) 0.076(2) 0.0042(18) 0.0013(16) 0.0305(18) N5 0.0387(15) 0.0511(17) 0.079(2) -0.0066(15) -0.0101(14) 0.0239(14) N6 0.061(2) 0.072(2) 0.080(2) 0.0127(18) 0.0139(18) 0.0434(19) O1 0.075(2) 0.0523(16) 0.099(2) -0.0142(15) -0.0111(17) 0.0308(15) O2 0.0721(19) 0.104(3) 0.0661(19) 0.0026(16) -0.0038(15) 0.0478(19) O3 0.0651(18) 0.0512(17) 0.123(3) -0.0134(17) -0.0116(18) 0.0229(14) C1 0.066(2) 0.047(2) 0.069(2) -0.0226(18) -0.026(2) 0.0262(19) C2 0.076(3) 0.050(2) 0.130(4) 0.011(2) 0.011(3) 0.037(2) C3 0.078(3) 0.054(2) 0.084(3) -0.007(2) -0.006(2) 0.039(2) C4 0.066(3) 0.062(2) 0.071(2) -0.004(2) -0.011(2) 0.030(2) C5 0.056(2) 0.0432(19) 0.0515(19) -0.0016(15) -0.0002(16) 0.0153(17) C6 0.054(2) 0.048(2) 0.057(2) -0.0004(16) 0.0053(16) 0.0205(17) C7 0.048(2) 0.055(2) 0.066(2) 0.0122(18) 0.0083(17) 0.0181(18) C8 0.045(2) 0.051(2) 0.065(2) 0.0073(17) 0.0021(17) 0.0069(17) C9 0.058(2) 0.0434(19) 0.069(2) -0.0001(17) 0.0064(19) 0.0162(18) C10 0.066(2) 0.051(2) 0.063(2) 0.0022(17) 0.0041(18) 0.0268(19) C11 0.082(3) 0.043(2) 0.078(3) 0.0013(19) 0.006(2) 0.020(2) C12 0.55(3) 0.091(6) 0.163(9) -0.017(6) 0.092(14) 0.133(12) C13 0.178(10) 0.049(4) 0.48(3) -0.042(8) 0.148(14) 0.000(5) C14 0.38(2) 0.091(6) 0.337(19) -0.092(9) -0.199(18) 0.139(10) C15 0.051(2) 0.062(2) 0.088(3) 0.016(2) 0.011(2) 0.0217(19) C16 0.046(2) 0.063(3) 0.087(3) 0.005(2) 0.0101(19) 0.0300(19) C17 0.061(3) 0.078(3) 0.103(4) -0.010(3) -0.008(2) 0.028(2) C18 0.081(3) 0.095(4) 0.088(3) -0.014(3) -0.022(3) 0.055(3) C19 0.074(3) 0.097(4) 0.091(3) 0.022(3) 0.017(2) 0.061(3) C20 0.051(2) 0.056(2) 0.075(3) 0.0066(18) 0.0011(18) 0.0307(18) C21 0.056(2) 0.0463(19) 0.072(2) 0.0007(17) -0.0021(18) 0.0318(18) C22 0.0408(18) 0.0444(18) 0.072(2) -0.0038(16) -0.0085(16) 0.0220(15) C23 0.048(2) 0.051(2) 0.068(2) 0.0019(17) -0.0009(17) 0.0252(17) C24 0.0400(18) 0.0398(17) 0.072(2) 0.0039(15) -0.0087(16) 0.0185(15) C25 0.0373(18) 0.054(2) 0.090(3) 0.0035(19) -0.0117(17) 0.0278(16) C26 0.051(2) 0.069(3) 0.081(3) 0.008(2) -0.010(2) 0.022(2) C27 0.078(3) 0.125(5) 0.096(4) 0.003(3) -0.023(3) 0.060(3) C28 0.095(4) 0.134(6) 0.123(5) 0.059(5) -0.036(4) 0.003(4) C29 0.105(5) 0.138(6) 0.102(4) -0.033(4) -0.025(3) 0.069(4) C30 0.0453(19) 0.053(2) 0.082(3) -0.0105(18) -0.0136(18) 0.0274(17) C31 0.041(2) 0.052(2) 0.096(3) 0.010(2) -0.0003(19) 0.0246(17) C32 0.087(3) 0.077(3) 0.079(3) -0.017(2) -0.028(2) 0.055(3) C33 0.093(3) 0.074(3) 0.065(2) -0.015(2) -0.016(2) 0.055(3) C34 0.062(2) 0.072(3) 0.100(3) 0.017(2) 0.022(2) 0.045(2) C35 0.0409(19) 0.067(2) 0.085(3) 0.003(2) 0.0088(18) 0.0368(18) C36 0.0440(19) 0.053(2) 0.088(3) -0.0089(19) -0.0041(18) 0.0289(18) C37 0.052(2) 0.061(2) 0.075(3) -0.0142(19) -0.0097(18) 0.0374(19) C38 0.063(2) 0.056(2) 0.065(2) 0.0011(18) -0.0011(18) 0.038(2) C39 0.053(2) 0.053(2) 0.063(2) -0.0065(17) 0.0000(17) 0.0293(18) C40 0.059(2) 0.072(3) 0.058(2) -0.0054(18) 0.0021(17) 0.045(2) C41 0.080(3) 0.061(2) 0.071(3) -0.015(2) 0.001(2) 0.034(2) C42 0.076(3) 0.079(3) 0.113(4) -0.007(3) -0.003(3) 0.013(3) C43 0.115(5) 0.067(3) 0.144(5) -0.029(3) 0.004(4) 0.055(3) C44 0.170(7) 0.086(4) 0.085(4) -0.029(3) -0.017(4) 0.025(5) C45 0.070(3) 0.070(3) 0.082(3) -0.018(2) -0.020(2) 0.043(2) C46 0.225(13) 0.154(9) 0.134(7) -0.038(7) -0.023(8) 0.076(9) C47 0.132(9) 0.241(17) 0.255(19) -0.027(14) 0.083(12) 0.013(11) C48 0.199(14) 0.29(2) 0.138(11) 0.050(12) -0.053(11) 0.065(14) C49 0.123(8) 0.36(3) 0.096(7) 0.033(10) -0.009(6) 0.019(12) O5 0.278(12) 0.277(12) 0.151(6) -0.001(7) -0.091(7) 0.142(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C1 1.678(4) . ? S2 C16 1.671(5) . ? S3 C31 1.674(5) . ? N1 C1 1.349(6) . ? N1 C2 1.446(6) . ? N1 C45 1.469(6) . ? N2 C1 1.351(6) . ? N2 C3 1.432(6) . ? N2 C4 1.445(6) . ? N3 C16 1.325(6) . ? N3 C17 1.438(7) . ? N3 C15 1.471(6) . ? N4 C16 1.357(6) . ? N4 C19 1.451(6) . ? N4 C18 1.433(7) . ? N5 C31 1.343(5) . ? N5 C32 1.453(6) . ? N5 C30 1.448(5) . ? N6 C31 1.350(6) . ? N6 C33 1.452(6) . ? N6 C34 1.477(5) . ? O1 C6 1.372(5) . ? O1 H1 0.9261 . ? O2 C21 1.358(5) . ? O2 H2 0.9428 . ? O3 C36 1.369(5) . ? O3 H3 0.8200 . ? C2 C3 1.496(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.498(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.386(6) . ? C5 C10 1.394(6) . ? C6 C7 1.404(6) . ? C7 C8 1.386(6) . ? C7 C15 1.516(6) . ? C8 C9 1.396(7) . ? C8 H8 0.9299 . ? C9 C10 1.378(6) . ? C9 C11 1.542(6) . ? C10 H10 0.9300 . ? C11 C12 1.461(13) . ? C11 C14 1.468(14) . ? C11 C13 1.464(11) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C17 C18 1.497(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.521(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C25 1.405(6) . ? C20 C21 1.400(6) . ? C21 C22 1.404(6) . ? C22 C23 1.386(6) . ? C22 C30 1.495(5) . ? C23 C24 1.388(5) . ? C23 H23 0.9300 . ? C24 C25 1.376(6) . ? C24 C26 1.525(6) . ? C25 H25 0.9300 . ? C26 C28 1.487(8) . ? C26 C27 1.511(7) . ? C26 C29 1.557(9) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C32 C33 1.501(6) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.495(7) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.397(6) . ? C35 C40 1.402(6) . ? C36 C37 1.414(6) . ? C37 C38 1.370(6) . ? C37 C45 1.491(6) . ? C38 C39 1.409(6) . ? C38 H38 0.9300 . ? C39 C40 1.374(6) . ? C39 C41 1.527(6) . ? C40 H40 0.9300 . ? C41 C42 1.536(8) . ? C41 C44 1.515(8) . ? C41 C43 1.557(8) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9601 . ? C43 H43B 0.9601 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.505(9) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 O5 1.419(14) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 C49 1.474(10) . ? C48 O5 1.417(13) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C2 111.8(4) . . ? C1 N1 C45 125.0(4) . . ? C2 N1 C45 120.8(4) . . ? C1 N2 C3 111.3(4) . . ? C1 N2 C4 126.5(4) . . ? C3 N2 C4 122.2(4) . . ? C16 N3 C17 111.9(4) . . ? C16 N3 C15 125.8(4) . . ? C17 N3 C15 121.5(4) . . ? C16 N4 C19 124.5(4) . . ? C16 N4 C18 110.4(4) . . ? C19 N4 C18 124.3(4) . . ? C31 N5 C32 111.0(3) . . ? C31 N5 C30 120.7(3) . . ? C32 N5 C30 124.8(3) . . ? C31 N6 C33 110.7(3) . . ? C31 N6 C34 123.7(4) . . ? C33 N6 C34 121.4(4) . . ? C6 O1 H1 118.9 . . ? C21 O2 H2 115.1 . . ? C36 O3 H3 109.5 . . ? N1 C1 N2 108.6(4) . . ? N1 C1 S1 126.3(4) . . ? N2 C1 S1 125.0(4) . . ? N1 C2 C3 103.0(4) . . ? N1 C2 H2A 111.2 . . ? C3 C2 H2A 111.2 . . ? N1 C2 H2B 111.2 . . ? C3 C2 H2B 111.2 . . ? H2A C2 H2B 109.1 . . ? N2 C3 C2 104.8(4) . . ? N2 C3 H3A 110.8 . . ? C2 C3 H3A 110.8 . . ? N2 C3 H3B 110.8 . . ? C2 C3 H3B 110.8 . . ? H3A C3 H3B 108.9 . . ? N2 C4 C5 114.2(4) . . ? N2 C4 H4A 108.7 . . ? C5 C4 H4A 108.7 . . ? N2 C4 H4B 108.7 . . ? C5 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? C6 C5 C10 119.5(4) . . ? C6 C5 C4 120.7(3) . . ? C10 C5 C4 119.8(4) . . ? O1 C6 C5 117.6(3) . . ? O1 C6 C7 122.4(4) . . ? C5 C6 C7 120.0(4) . . ? C8 C7 C6 118.4(4) . . ? C8 C7 C15 120.1(4) . . ? C6 C7 C15 121.4(4) . . ? C7 C8 C9 122.9(4) . . ? C7 C8 H8 118.4 . . ? C9 C8 H8 118.7 . . ? C10 C9 C8 116.9(4) . . ? C10 C9 C11 121.2(4) . . ? C8 C9 C11 121.9(4) . . ? C9 C10 C5 122.3(4) . . ? C9 C10 H10 118.8 . . ? C5 C10 H10 118.8 . . ? C12 C11 C14 99.9(12) . . ? C12 C11 C13 115.4(12) . . ? C14 C11 C13 106.9(11) . . ? C12 C11 C9 109.8(5) . . ? C14 C11 C9 112.9(5) . . ? C13 C11 C9 111.5(5) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 C7 115.2(4) . . ? N3 C15 H15A 108.5 . . ? C7 C15 H15A 108.5 . . ? N3 C15 H15B 108.5 . . ? C7 C15 H15B 108.5 . . ? H15A C15 H15B 107.5 . . ? N3 C16 N4 109.6(4) . . ? N3 C16 S2 127.5(4) . . ? N4 C16 S2 122.9(3) . . ? N3 C17 C18 103.4(4) . . ? N3 C17 H17A 111.1 . . ? C18 C17 H17A 110.9 . . ? N3 C17 H17B 111.5 . . ? C18 C17 H17B 110.9 . . ? H17A C17 H17B 109.1 . . ? N4 C18 C17 104.6(4) . . ? N4 C18 H18A 110.8 . . ? C17 C18 H18A 110.8 . . ? N4 C18 H18B 110.8 . . ? C17 C18 H18B 110.8 . . ? H18A C18 H18B 108.9 . . ? N4 C19 C20 113.5(4) . . ? N4 C19 H19A 108.9 . . ? C20 C19 H19A 108.9 . . ? N4 C19 H19B 108.9 . . ? C20 C19 H19B 108.9 . . ? H19A C19 H19B 107.7 . . ? C25 C20 C21 118.5(4) . . ? C25 C20 C19 120.4(4) . . ? C21 C20 C19 120.9(4) . . ? O2 C21 C20 123.7(4) . . ? O2 C21 C22 116.6(3) . . ? C20 C21 C22 119.7(4) . . ? C23 C22 C21 118.4(3) . . ? C23 C22 C30 120.3(4) . . ? C21 C22 C30 121.3(4) . . ? C24 C23 C22 124.1(4) . . ? C24 C23 H23 118.0 . . ? C22 C23 H23 118.0 . . ? C23 C24 C25 115.9(4) . . ? C23 C24 C26 120.1(4) . . ? C25 C24 C26 123.9(3) . . ? C24 C25 C20 123.4(3) . . ? C24 C25 H25 118.3 . . ? C20 C25 H25 118.3 . . ? C28 C26 C27 109.7(5) . . ? C28 C26 C24 111.9(4) . . ? C27 C26 C24 112.4(4) . . ? C28 C26 C29 109.4(6) . . ? C27 C26 C29 105.9(5) . . ? C24 C26 C29 107.3(4) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N5 C30 C22 112.8(3) . . ? N5 C30 H30A 109.0 . . ? C22 C30 H30A 109.0 . . ? N5 C30 H30B 109.0 . . ? C22 C30 H30B 109.0 . . ? H30A C30 H30B 107.8 . . ? N5 C31 N6 109.0(4) . . ? N5 C31 S3 123.9(3) . . ? N6 C31 S3 127.0(3) . . ? N5 C32 C33 102.8(3) . . ? N5 C32 H32A 111.2 . . ? C33 C32 H32A 111.2 . . ? N5 C32 H32B 111.2 . . ? C33 C32 H32B 111.2 . . ? H32A C32 H32B 109.1 . . ? N6 C33 C32 102.9(4) . . ? N6 C33 H33A 111.2 . . ? C32 C33 H33A 111.2 . . ? N6 C33 H33B 111.2 . . ? C32 C33 H33B 111.2 . . ? H33A C33 H33B 109.1 . . ? N6 C34 C35 111.7(3) . . ? N6 C34 H34A 109.3 . . ? C35 C34 H34A 109.3 . . ? N6 C34 H34B 109.3 . . ? C35 C34 H34B 109.3 . . ? H34A C34 H34B 107.9 . . ? C36 C35 C40 118.1(4) . . ? C36 C35 C34 123.0(4) . . ? C40 C35 C34 118.9(4) . . ? O3 C36 C35 122.8(4) . . ? O3 C36 C37 116.8(4) . . ? C35 C36 C37 120.4(4) . . ? C38 C37 C36 119.0(4) . . ? C38 C37 C45 121.0(4) . . ? C36 C37 C45 119.9(4) . . ? C37 C38 C39 122.3(4) . . ? C37 C38 H38 118.8 . . ? C39 C38 H38 118.8 . . ? C40 C39 C38 117.3(4) . . ? C40 C39 C41 122.2(4) . . ? C38 C39 C41 120.5(4) . . ? C39 C40 C35 123.0(4) . . ? C39 C40 H40 118.5 . . ? C35 C40 H40 118.5 . . ? C39 C41 C42 110.0(4) . . ? C39 C41 C44 113.4(4) . . ? C42 C41 C44 107.6(5) . . ? C39 C41 C43 108.0(4) . . ? C42 C41 C43 106.6(5) . . ? C44 C41 C43 111.0(5) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.8 . . ? C41 C43 H43B 110.0 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 108.6 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N1 C45 C37 112.0(3) . . ? N1 C45 H45A 109.2 . . ? C37 C45 H45A 109.2 . . ? N1 C45 H45B 109.2 . . ? C37 C45 H45B 109.2 . . ? H45A C45 H45B 107.9 . . ? C47 C46 H46A 109.5 . . ? C47 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C47 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C46 C47 O5 102.0(11) . . ? C46 C47 H47A 111.4 . . ? O5 C47 H47A 111.4 . . ? C46 C47 H47B 111.4 . . ? O5 C47 H47B 111.4 . . ? H47A C47 H47B 109.2 . . ? C49 C48 O5 103.8(11) . . ? C49 C48 H48A 111.0 . . ? O5 C48 H48A 111.0 . . ? C49 C48 H48B 111.0 . . ? O5 C48 H48B 111.0 . . ? H48A C48 H48B 109.0 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C47 O5 C48 115.2(11) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.485 _refine_diff_density_min -0.296 _refine_diff_density_rms 0.052 _database_code_depnum_ccdc_archive 'CCDC 952890' data_Keinan-106 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'keinan-106 (Senthil)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30.25 H38.50 Cl0.50 N4 O0.50 O2 S2' _chemical_formula_weight 580.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.239(6) _cell_length_b 14.560(3) _cell_length_c 19.951(4) _cell_angle_alpha 90.00 _cell_angle_beta 120.20(3) _cell_angle_gamma 90.00 _cell_volume 6839(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23656 _cell_measurement_theta_min 1.75 _cell_measurement_theta_max 25.05 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.127 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2468 _exptl_absorpt_coefficient_mu 0.226 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f- and \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 11571 _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.05 _reflns_number_total 6051 _reflns_number_gt 4061 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 2006)' _computing_cell_refinement 'DENZO HKL2000 (Otwinowski & Minor 1997)' _computing_data_reduction 'DENZO HKL2000 (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Mercury 2.4' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1900P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0013(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6051 _refine_ls_number_parameters 367 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1092 _refine_ls_R_factor_gt 0.0842 _refine_ls_wR_factor_ref 0.2704 _refine_ls_wR_factor_gt 0.2504 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.67903(4) 0.24679(6) 0.05539(5) 0.0706(3) Uani 1 1 d . . . S2 S 0.68119(5) 0.01396(9) 0.27850(6) 0.0922(4) Uani 1 1 d . . . O1 O 0.75779(9) 0.12848(18) 0.21688(13) 0.0759(7) Uani 1 1 d . . . O2 O 0.64888(12) 0.03799(17) 0.08840(14) 0.0784(7) Uani 1 1 d . . . N1 N 0.70685(10) 0.10354(17) -0.00478(14) 0.0563(6) Uani 1 1 d . . . N2 N 0.77981(10) 0.17493(17) 0.08888(14) 0.0568(6) Uani 1 1 d . . . N3 N 0.78070(12) -0.0497(2) 0.30042(17) 0.0741(8) Uani 1 1 d . . . N4 N 0.70651(13) -0.1205(2) 0.20829(18) 0.0739(8) Uani 1 1 d . . . C1 C 0.72290(12) 0.17390(19) 0.04650(16) 0.0518(7) Uani 1 1 d . . . C2 C 0.75490(14) 0.0536(3) 0.0020(2) 0.0683(9) Uani 1 1 d . . . H2A H 0.7582 0.0620 -0.0437 0.082 Uiso 1 1 calc R . . H2B H 0.7517 -0.0114 0.0095 0.082 Uiso 1 1 calc R . . C3 C 0.80495(14) 0.0952(2) 0.0725(2) 0.0662(8) Uani 1 1 d . . . H3A H 0.8210 0.0525 0.1156 0.079 Uiso 1 1 calc R . . H3B H 0.8343 0.1138 0.0614 0.079 Uiso 1 1 calc R . . C4 C 0.81367(14) 0.2339(2) 0.15499(18) 0.0656(9) Uani 1 1 d . . . H4A H 0.7890 0.2788 0.1590 0.079 Uiso 1 1 calc R . . H4B H 0.8409 0.2668 0.1463 0.079 Uiso 1 1 calc R . . C5 C 0.84525(12) 0.1818(2) 0.23080(16) 0.0557(7) Uani 1 1 d . . . C6 C 0.81606(13) 0.1300(2) 0.25876(17) 0.0607(8) Uani 1 1 d . . . C7 C 0.84549(14) 0.0818(2) 0.32763(18) 0.0662(9) Uani 1 1 d . . . C8 C 0.90409(14) 0.0891(3) 0.37022(19) 0.0706(9) Uani 1 1 d . . . H8 H 0.9236 0.0564 0.4164 0.085 Uiso 1 1 calc R . . C9 C 0.93507(14) 0.1432(2) 0.34712(19) 0.0672(8) Uani 1 1 d . . . C10 C 0.90369(13) 0.1875(2) 0.27543(18) 0.0614(8) Uani 1 1 d . . . H10 H 0.9231 0.2223 0.2570 0.074 Uiso 1 1 calc R . . C11 C 0.99902(15) 0.1554(4) 0.3984(2) 0.0937(13) Uani 1 1 d . . . C12 C 1.0137(3) 0.1788(13) 0.4788(4) 0.289(9) Uani 1 1 d . . . H12A H 0.9923 0.1405 0.4941 0.433 Uiso 1 1 calc R . . H12B H 1.0046 0.2421 0.4810 0.433 Uiso 1 1 calc R . . H12C H 1.0536 0.1690 0.5133 0.433 Uiso 1 1 calc R . . C13 C 1.0242(2) 0.2179(6) 0.3695(4) 0.170(3) Uani 1 1 d . . . H13A H 1.0134 0.2014 0.3172 0.255 Uiso 1 1 calc R . . H13B H 1.0648 0.2153 0.4015 0.255 Uiso 1 1 calc R . . H13C H 1.0113 0.2791 0.3702 0.255 Uiso 1 1 calc R . . C14 C 1.0262(3) 0.0656(7) 0.4154(10) 0.326(11) Uani 1 1 d . . . H14A H 1.0088 0.0262 0.4361 0.489 Uiso 1 1 calc R . . H14B H 1.0659 0.0722 0.4527 0.489 Uiso 1 1 calc R . . H14C H 1.0218 0.0392 0.3686 0.489 Uiso 1 1 calc R . . C15 C 0.81396(17) 0.0208(3) 0.3558(2) 0.0861(12) Uani 1 1 d . . . H15A H 0.8413 -0.0080 0.4042 0.103 Uiso 1 1 calc R . . H15B H 0.7891 0.0586 0.3658 0.103 Uiso 1 1 calc R . . C16 C 0.72332(15) -0.0537(3) 0.26198(19) 0.0695(9) Uani 1 1 d . . . C17 C 0.80507(17) -0.1165(3) 0.2716(3) 0.0880(12) Uani 1 1 d . . . H17A H 0.8284 -0.1605 0.3116 0.106 Uiso 1 1 calc R . . H17B H 0.8280 -0.0867 0.2532 0.106 Uiso 1 1 calc R . . C18 C 0.75456(18) -0.1617(3) 0.2068(3) 0.0947(12) Uani 1 1 d . . . H18A H 0.7527 -0.1500 0.1577 0.114 Uiso 1 1 calc R . . H18B H 0.7556 -0.2276 0.2149 0.114 Uiso 1 1 calc R . . C19 C 0.64822(16) -0.1380(3) 0.1480(2) 0.0809(11) Uani 1 1 d . . . H19A H 0.6230 -0.0972 0.1549 0.097 Uiso 1 1 calc R . . H19B H 0.6381 -0.2007 0.1523 0.097 Uiso 1 1 calc R . . C20 C 0.64064(14) -0.1234(2) 0.06807(19) 0.0666(9) Uani 1 1 d . . . C21 C 0.64316(13) -0.0357(2) 0.04242(19) 0.0636(8) Uani 1 1 d . . . C22 C 0.64134(13) -0.0230(2) -0.02857(18) 0.0606(8) Uani 1 1 d . . . C23 C 0.63402(13) -0.0998(2) -0.0742(2) 0.0648(8) Uani 1 1 d . . . H23 H 0.6323 -0.0917 -0.1216 0.078 Uiso 1 1 calc R . . C24 C 0.62925(14) -0.1876(2) -0.0519(2) 0.0712(9) Uani 1 1 d . . . C25 C 0.63333(14) -0.1974(2) 0.0205(2) 0.0712(9) Uani 1 1 d . . . H25 H 0.6310 -0.2560 0.0372 0.085 Uiso 1 1 calc R . . C26 C 0.62113(18) -0.2716(3) -0.1027(3) 0.0859(11) Uani 1 1 d . . . C27 C 0.5643(5) -0.3123(8) -0.1269(8) 0.300(9) Uani 1 1 d . . . H27A H 0.5362 -0.2646 -0.1459 0.449 Uiso 1 1 calc R . . H27B H 0.5653 -0.3418 -0.0833 0.449 Uiso 1 1 calc R . . H27C H 0.5550 -0.3566 -0.1672 0.449 Uiso 1 1 calc R . . C28 C 0.6714(7) -0.3300(8) -0.0644(6) 0.389(13) Uani 1 1 d . . . H28A H 0.7048 -0.2935 -0.0487 0.584 Uiso 1 1 calc R . . H28B H 0.6692 -0.3769 -0.0996 0.584 Uiso 1 1 calc R . . H28C H 0.6733 -0.3580 -0.0196 0.584 Uiso 1 1 calc R . . C29 C 0.6094(5) -0.2450(4) -0.1835(4) 0.201(5) Uani 1 1 d . . . H29A H 0.5764 -0.2062 -0.2080 0.301 Uiso 1 1 calc R . . H29B H 0.6028 -0.2994 -0.2141 0.301 Uiso 1 1 calc R . . H29C H 0.6415 -0.2125 -0.1792 0.301 Uiso 1 1 calc R . . C30 C 0.64911(14) 0.0708(2) -0.05283(18) 0.0652(8) Uani 1 1 d . . . H30A H 0.6400 0.0689 -0.1065 0.078 Uiso 1 1 calc R . . H30B H 0.6231 0.1133 -0.0492 0.078 Uiso 1 1 calc R . . Cl1 Cl 0.0144(3) 0.5273(8) 0.1901(8) 0.398(8) Uani 0.50 1 d PD . . C31 C 0.0000 0.438(2) 0.2500 0.246(17) Uani 0.50 2 d SPD . . H31A H 0.0328 0.3997 0.2820 0.295 Uiso 0.25 1 calc PR . . H31B H -0.0328 0.3997 0.2180 0.295 Uiso 0.25 1 calc PR . . O32 O 0.0086(7) 0.524(3) 0.0566(19) 0.63(4) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0771(6) 0.0623(6) 0.0748(6) 0.0072(4) 0.0400(5) 0.0182(4) S2 0.0891(7) 0.1283(10) 0.0763(7) 0.0041(6) 0.0542(6) 0.0070(6) O1 0.0576(13) 0.0927(17) 0.0676(14) 0.0176(12) 0.0242(11) -0.0071(11) O2 0.1071(19) 0.0699(15) 0.0710(14) -0.0068(12) 0.0543(14) -0.0096(13) N1 0.0598(14) 0.0508(14) 0.0532(13) 0.0003(11) 0.0247(11) 0.0004(11) N2 0.0569(14) 0.0566(14) 0.0503(13) 0.0041(10) 0.0221(11) 0.0042(11) N3 0.0685(17) 0.085(2) 0.0708(17) 0.0150(15) 0.0364(15) -0.0045(15) N4 0.0739(17) 0.0815(19) 0.0731(18) 0.0087(15) 0.0420(15) -0.0073(15) C1 0.0615(17) 0.0466(15) 0.0489(14) 0.0094(12) 0.0289(13) 0.0055(12) C2 0.073(2) 0.065(2) 0.074(2) -0.0055(16) 0.0428(17) 0.0046(15) C3 0.0684(19) 0.0646(19) 0.0685(19) 0.0059(15) 0.0367(16) 0.0113(15) C4 0.0691(19) 0.0544(17) 0.0594(18) 0.0026(14) 0.0219(16) -0.0053(14) C5 0.0595(16) 0.0543(16) 0.0481(15) 0.0008(12) 0.0230(13) 0.0001(13) C6 0.0561(17) 0.0681(19) 0.0507(16) -0.0026(14) 0.0214(14) -0.0016(14) C7 0.0639(18) 0.081(2) 0.0523(17) 0.0069(15) 0.0286(15) -0.0015(16) C8 0.0649(19) 0.082(2) 0.0561(18) 0.0137(16) 0.0238(15) 0.0028(16) C9 0.0609(17) 0.074(2) 0.0644(19) 0.0118(16) 0.0295(15) 0.0051(15) C10 0.0636(18) 0.0595(18) 0.0633(18) 0.0061(14) 0.0335(15) 0.0024(14) C11 0.0557(19) 0.126(4) 0.084(3) 0.034(2) 0.0241(19) 0.013(2) C12 0.082(4) 0.64(3) 0.118(5) -0.123(10) 0.029(4) -0.093(9) C13 0.072(3) 0.239(8) 0.131(5) 0.070(5) 0.001(3) -0.056(4) C14 0.080(4) 0.203(9) 0.58(3) 0.173(14) 0.081(8) 0.041(5) C15 0.078(2) 0.123(3) 0.0541(18) 0.012(2) 0.0305(18) -0.016(2) C16 0.076(2) 0.083(2) 0.0589(18) 0.0186(18) 0.0410(17) -0.0038(17) C17 0.076(2) 0.097(3) 0.092(3) 0.022(2) 0.043(2) 0.009(2) C18 0.090(3) 0.075(2) 0.129(4) 0.003(2) 0.063(3) 0.000(2) C19 0.078(2) 0.093(3) 0.076(2) 0.0075(19) 0.0416(19) -0.0219(19) C20 0.0692(19) 0.067(2) 0.0642(19) 0.0050(15) 0.0339(16) -0.0106(15) C21 0.0649(18) 0.067(2) 0.0600(18) -0.0047(15) 0.0320(15) -0.0049(15) C22 0.0591(17) 0.0638(19) 0.0564(17) 0.0026(14) 0.0271(14) -0.0034(14) C23 0.0665(19) 0.0616(19) 0.0653(18) -0.0004(15) 0.0324(16) -0.0023(14) C24 0.0660(19) 0.061(2) 0.083(2) -0.0058(16) 0.0343(17) -0.0021(15) C25 0.076(2) 0.060(2) 0.078(2) 0.0055(17) 0.0393(18) -0.0074(16) C26 0.094(3) 0.065(2) 0.095(3) -0.017(2) 0.045(2) -0.004(2) C27 0.312(14) 0.270(13) 0.404(18) -0.264(14) 0.245(14) -0.192(12) C28 0.47(2) 0.236(11) 0.196(9) -0.099(8) -0.032(11) 0.240(14) C29 0.357(14) 0.102(5) 0.112(5) -0.022(4) 0.096(7) 0.014(6) C30 0.0655(18) 0.0601(19) 0.0563(17) 0.0050(14) 0.0204(15) -0.0023(14) Cl1 0.144(5) 0.367(11) 0.432(16) -0.078(10) -0.041(7) 0.034(6) C31 0.25(4) 0.35(5) 0.079(11) 0.000 0.045(16) 0.000 O32 0.145(11) 1.08(7) 0.73(6) 0.71(6) 0.27(3) 0.30(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C1 1.673(3) . ? S2 C16 1.666(4) . ? O1 C6 1.372(4) . ? O2 C21 1.369(4) . ? N1 C1 1.356(4) . ? N1 C2 1.442(4) . ? N1 C30 1.450(4) . ? N2 C1 1.341(4) . ? N2 C4 1.450(4) . ? N2 C3 1.465(4) . ? N3 C16 1.352(4) . ? N3 C15 1.444(5) . ? N3 C17 1.449(5) . ? N4 C16 1.345(5) . ? N4 C19 1.453(5) . ? N4 C18 1.454(5) . ? C2 C3 1.508(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.514(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C10 1.381(4) . ? C5 C6 1.399(4) . ? C6 C7 1.384(5) . ? C7 C8 1.385(5) . ? C7 C15 1.525(5) . ? C8 C9 1.392(5) . ? C8 H8 0.9300 . ? C9 C10 1.401(5) . ? C9 C11 1.523(5) . ? C10 H10 0.9300 . ? C11 C13 1.424(7) . ? C11 C14 1.456(10) . ? C11 C12 1.486(9) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C17 C18 1.486(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.515(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C25 1.383(5) . ? C20 C21 1.390(5) . ? C21 C22 1.404(5) . ? C22 C23 1.392(5) . ? C22 C30 1.499(4) . ? C23 C24 1.382(5) . ? C23 H23 0.9300 . ? C24 C25 1.399(5) . ? C24 C26 1.532(5) . ? C25 H25 0.9300 . ? C26 C28 1.459(10) . ? C26 C27 1.492(10) . ? C26 C29 1.526(9) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? Cl1 C31 1.935(17) . ? C31 Cl1 1.936(17) 2 ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C2 112.1(2) . . ? C1 N1 C30 125.3(3) . . ? C2 N1 C30 121.9(3) . . ? C1 N2 C4 125.8(3) . . ? C1 N2 C3 111.8(2) . . ? C4 N2 C3 121.1(2) . . ? C16 N3 C15 124.4(4) . . ? C16 N3 C17 112.1(3) . . ? C15 N3 C17 122.9(3) . . ? C16 N4 C19 125.4(3) . . ? C16 N4 C18 111.4(3) . . ? C19 N4 C18 122.0(4) . . ? N2 C1 N1 108.4(2) . . ? N2 C1 S1 125.9(2) . . ? N1 C1 S1 125.7(2) . . ? N1 C2 C3 103.8(3) . . ? N1 C2 H2A 111.0 . . ? C3 C2 H2A 111.0 . . ? N1 C2 H2B 111.0 . . ? C3 C2 H2B 111.0 . . ? H2A C2 H2B 109.0 . . ? N2 C3 C2 102.8(3) . . ? N2 C3 H3A 111.2 . . ? C2 C3 H3A 111.2 . . ? N2 C3 H3B 111.2 . . ? C2 C3 H3B 111.2 . . ? H3A C3 H3B 109.1 . . ? N2 C4 C5 113.2(2) . . ? N2 C4 H4A 108.9 . . ? C5 C4 H4A 108.9 . . ? N2 C4 H4B 108.9 . . ? C5 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? C10 C5 C6 118.5(3) . . ? C10 C5 C4 120.3(3) . . ? C6 C5 C4 121.1(3) . . ? O1 C6 C7 120.7(3) . . ? O1 C6 C5 118.7(3) . . ? C7 C6 C5 120.5(3) . . ? C6 C7 C8 118.9(3) . . ? C6 C7 C15 120.6(3) . . ? C8 C7 C15 120.5(3) . . ? C7 C8 C9 123.0(3) . . ? C7 C8 H8 118.5 . . ? C9 C8 H8 118.5 . . ? C8 C9 C10 116.0(3) . . ? C8 C9 C11 121.5(3) . . ? C10 C9 C11 122.4(3) . . ? C5 C10 C9 122.9(3) . . ? C5 C10 H10 118.5 . . ? C9 C10 H10 118.5 . . ? C13 C11 C14 112.1(7) . . ? C13 C11 C12 111.6(7) . . ? C14 C11 C12 97.2(9) . . ? C13 C11 C9 115.1(3) . . ? C14 C11 C9 109.1(5) . . ? C12 C11 C9 110.3(4) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 C7 112.7(3) . . ? N3 C15 H15A 109.1 . . ? C7 C15 H15A 109.1 . . ? N3 C15 H15B 109.1 . . ? C7 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? N3 C16 N4 108.4(3) . . ? N3 C16 S2 125.3(3) . . ? N4 C16 S2 126.3(3) . . ? N3 C17 C18 103.5(3) . . ? N3 C17 H17A 111.1 . . ? C18 C17 H17A 111.1 . . ? N3 C17 H17B 111.1 . . ? C18 C17 H17B 111.1 . . ? H17A C17 H17B 109.0 . . ? N4 C18 C17 104.4(4) . . ? N4 C18 H18A 110.9 . . ? C17 C18 H18A 110.9 . . ? N4 C18 H18B 110.9 . . ? C17 C18 H18B 110.9 . . ? H18A C18 H18B 108.9 . . ? N4 C19 C20 111.1(3) . . ? N4 C19 H19A 109.4 . . ? C20 C19 H19A 109.4 . . ? N4 C19 H19B 109.4 . . ? C20 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? C25 C20 C21 118.6(3) . . ? C25 C20 C19 120.6(3) . . ? C21 C20 C19 120.7(3) . . ? O2 C21 C20 118.9(3) . . ? O2 C21 C22 120.4(3) . . ? C20 C21 C22 120.6(3) . . ? C23 C22 C21 118.3(3) . . ? C23 C22 C30 121.2(3) . . ? C21 C22 C30 120.5(3) . . ? C24 C23 C22 122.6(3) . . ? C24 C23 H23 118.7 . . ? C22 C23 H23 118.7 . . ? C23 C24 C25 117.1(3) . . ? C23 C24 C26 122.1(4) . . ? C25 C24 C26 120.8(3) . . ? C20 C25 C24 122.6(3) . . ? C20 C25 H25 118.7 . . ? C24 C25 H25 118.7 . . ? C28 C26 C27 119.0(10) . . ? C28 C26 C29 110.2(9) . . ? C27 C26 C29 97.3(7) . . ? C28 C26 C24 109.4(5) . . ? C27 C26 C24 108.2(4) . . ? C29 C26 C24 112.3(4) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N1 C30 C22 111.6(3) . . ? N1 C30 H30A 109.3 . . ? C22 C30 H30A 109.3 . . ? N1 C30 H30B 109.3 . . ? C22 C30 H30B 109.3 . . ? H30A C30 H30B 108.0 . . ? Cl1 C31 Cl1 95.5(18) . 2 ? Cl1 C31 H31A 112.6 . . ? Cl1 C31 H31A 112.6 2 . ? Cl1 C31 H31B 112.6 . . ? Cl1 C31 H31B 112.6 2 . ? H31A C31 H31B 110.1 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.817 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.085 _database_code_depnum_ccdc_archive 'CCDC 952891'