# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2007 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Kari Rissanen' _publ_contact_author_address ; Department of Chemistry Univeristy of Jyvaskyla PO Box 35 Helsinki FIN-00014 FINLAND ; _publ_contact_author_email KARI.RISSANEN@JYU.FI _publ_section_title ; Dansylated Resorcinarenes ; loop_ _publ_author_name K.Rissanen A.Ahman J.Aumanen N.K.Beyeh J.Korppi-Tommola ; M.Luostarinen ; H.Mansikkamaki M.Nissinen data_2 _database_code_depnum_ccdc_archive 'CCDC 606001' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C88 H92 N4 O16 S4, C Cl3, C H1.5 N0.5' _chemical_formula_sum 'C90 H93.50 Cl3 N4.50 O16 S4' _chemical_formula_weight 1721.35 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.2474(7) _cell_length_b 16.2674(7) _cell_length_c 20.5931(7) _cell_angle_alpha 83.540(3) _cell_angle_beta 76.736(3) _cell_angle_gamma 71.072(2) _cell_volume 5006.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173.0(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.147 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 0.234 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9547 _exptl_absorpt_correction_T_max 0.9770 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173.0(1) _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 Kappa CCD' _diffrn_measurement_method 'rotation in phi and omega, 2.0 deg.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31628 _diffrn_reflns_av_R_equivalents 0.1413 _diffrn_reflns_av_sigmaI/netI 0.2603 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.69 _diffrn_reflns_theta_max 24.45 _reflns_number_total 16391 _reflns_number_gt 6033 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement Denzo-SMN _computing_data_reduction Denzo-SMN _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.2000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16391 _refine_ls_number_parameters 1042 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.2545 _refine_ls_R_factor_gt 0.1274 _refine_ls_wR_factor_ref 0.3917 _refine_ls_wR_factor_gt 0.3377 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 C1 C -0.1392(6) 0.7395(6) 0.5960(4) 0.024(2) Uani 1 1 d . . . C2 C -0.0479(6) 0.7304(6) 0.5851(5) 0.029(2) Uani 1 1 d . . . H2 H -0.0149 0.6953 0.6163 0.034 Uiso 1 1 calc R . . C3 C -0.0026(6) 0.7704(6) 0.5306(4) 0.024(2) Uani 1 1 d . . . C4 C -0.0529(6) 0.8187(6) 0.4848(4) 0.020(2) Uani 1 1 d . . . C5 C -0.1425(7) 0.8336(6) 0.4923(4) 0.031(2) Uani 1 1 d . . . H5 H -0.1752 0.8690 0.4610 0.037 Uiso 1 1 calc R . . C6 C -0.1840(6) 0.7928(6) 0.5501(5) 0.027(2) Uani 1 1 d . . . C7 C 0.0923(6) 0.7651(6) 0.5248(4) 0.029(2) Uani 1 1 d . . . H7 H 0.1193 0.7690 0.4762 0.035 Uiso 1 1 calc R . . C8 C 0.1454(6) 0.6791(6) 0.5535(4) 0.020(2) Uani 1 1 d . . . C9 C 0.1793(6) 0.6688(6) 0.6105(4) 0.029(2) Uani 1 1 d . . . H9 H 0.1645 0.7186 0.6361 0.035 Uiso 1 1 calc R . . C10 C 0.2333(6) 0.5909(6) 0.6333(4) 0.025(2) Uani 1 1 d . . . C11 C 0.2555(6) 0.5173(6) 0.5943(5) 0.030(2) Uani 1 1 d . . . C12 C 0.2193(6) 0.5248(6) 0.5385(4) 0.029(2) Uani 1 1 d . . . H12 H 0.2311 0.4751 0.5136 0.034 Uiso 1 1 calc R . . C13 C 0.1673(6) 0.6025(6) 0.5195(4) 0.024(2) Uani 1 1 d . . . C14 C 0.2686(6) 0.5797(6) 0.6969(4) 0.026(2) Uani 1 1 d . . . H14 H 0.3334 0.5467 0.6851 0.031 Uiso 1 1 calc R . . C15 C 0.2257(6) 0.5233(6) 0.7507(4) 0.032(2) Uani 1 1 d . . . C16 C 0.1357(6) 0.5263(6) 0.7585(4) 0.029(2) Uani 1 1 d . . . H16 H 0.1023 0.5623 0.7279 0.035 Uiso 1 1 calc R . . C17 C 0.0946(6) 0.4811(6) 0.8068(4) 0.025(2) Uani 1 1 d . . . C18 C 0.1468(6) 0.4285(6) 0.8509(4) 0.031(2) Uani 1 1 d . . . C19 C 0.2338(6) 0.4220(6) 0.8476(4) 0.029(2) Uani 1 1 d . . . H19 H 0.2670 0.3856 0.8781 0.034 Uiso 1 1 calc R . . C20 C 0.2707(6) 0.4716(6) 0.7971(4) 0.028(2) Uani 1 1 d . . . C21 C -0.0028(6) 0.4862(7) 0.8155(4) 0.029(2) Uani 1 1 d . . . H21 H -0.0068 0.4268 0.8308 0.034 Uiso 1 1 calc R . . C22 C -0.0385(5) 0.5096(6) 0.7505(4) 0.020(2) Uani 1 1 d . . . C23 C -0.0905(6) 0.5918(6) 0.7337(4) 0.024(2) Uani 1 1 d . . . H23 H -0.1034 0.6378 0.7627 0.029 Uiso 1 1 calc R . . C24 C -0.1247(5) 0.6093(5) 0.6751(4) 0.019(2) Uani 1 1 d . . . C25 C -0.1046(6) 0.5426(6) 0.6343(4) 0.024(2) Uani 1 1 d . . . C26 C -0.0493(6) 0.4579(6) 0.6482(4) 0.028(2) Uani 1 1 d . . . H26 H -0.0343 0.4128 0.6179 0.033 Uiso 1 1 calc R . . C27 C -0.0178(5) 0.4426(5) 0.7066(4) 0.021(2) Uani 1 1 d . . . C28 C -0.1840(6) 0.7009(6) 0.6574(4) 0.024(2) Uani 1 1 d . . . H28 H -0.2373 0.6925 0.6461 0.028 Uiso 1 1 calc R . . C29 C 0.0951(6) 0.8455(6) 0.5573(4) 0.026(2) Uani 1 1 d . . . H29A H 0.0517 0.8981 0.5420 0.032 Uiso 1 1 calc R . . H29B H 0.0765 0.8388 0.6064 0.032 Uiso 1 1 calc R . . C30 C 0.1880(6) 0.8590(6) 0.5408(5) 0.031(2) Uani 1 1 d . . . H30A H 0.2333 0.8040 0.5504 0.037 Uiso 1 1 calc R . . H30B H 0.2032 0.8748 0.4927 0.037 Uiso 1 1 calc R . . C31 C 0.1891(8) 0.9302(9) 0.5819(7) 0.081(5) Uani 1 1 d . . . H31A H 0.1375 0.9814 0.5788 0.121 Uiso 1 1 calc R . . H31B H 0.2438 0.9457 0.5648 0.121 Uiso 1 1 calc R . . H31C H 0.1866 0.9094 0.6287 0.121 Uiso 1 1 calc R . . C32 C 0.2617(7) 0.6673(7) 0.7266(5) 0.041(3) Uani 1 1 d . . . H32A H 0.1998 0.7065 0.7308 0.049 Uiso 1 1 calc R . . H32B H 0.2747 0.6548 0.7719 0.049 Uiso 1 1 calc R . . C33 C 0.3227(8) 0.7127(7) 0.6856(6) 0.051(3) Uani 1 1 d . . . H33A H 0.3003 0.7746 0.6972 0.061 Uiso 1 1 calc R . . H33B H 0.3215 0.7105 0.6380 0.061 Uiso 1 1 calc R . . C34 C 0.4173(10) 0.6759(9) 0.6941(7) 0.083(4) Uani 1 1 d . . . H34A H 0.4208 0.6866 0.7391 0.124 Uiso 1 1 calc R . . H34B H 0.4547 0.7040 0.6611 0.124 Uiso 1 1 calc R . . H34C H 0.4383 0.6132 0.6876 0.124 Uiso 1 1 calc R . . C35 C -0.0596(6) 0.5482(6) 0.8732(4) 0.022(2) Uani 1 1 d . . . H35A H -0.0288 0.5341 0.9112 0.026 Uiso 1 1 calc R . . H35B H -0.0633 0.6088 0.8575 0.026 Uiso 1 1 calc R . . C36 C -0.1521(7) 0.5426(7) 0.8975(5) 0.043(3) Uani 1 1 d . . . H36A H -0.1861 0.5660 0.8617 0.052 Uiso 1 1 calc R . . H36B H -0.1488 0.4806 0.9061 0.052 Uiso 1 1 calc R . . C37 C -0.2008(8) 0.5902(11) 0.9589(6) 0.088(5) Uani 1 1 d . . . H37A H -0.1944 0.5501 0.9979 0.132 Uiso 1 1 calc R . . H37B H -0.2639 0.6151 0.9571 0.132 Uiso 1 1 calc R . . H37C H -0.1764 0.6370 0.9622 0.132 Uiso 1 1 calc R . . C38 C -0.2194(6) 0.7640(6) 0.7139(4) 0.034(2) Uani 1 1 d . . . H38A H -0.1692 0.7618 0.7345 0.041 Uiso 1 1 calc R . . H38B H -0.2410 0.8236 0.6944 0.041 Uiso 1 1 calc R . . C39 C -0.2912(9) 0.7490(9) 0.7671(6) 0.071(4) Uani 1 1 d . . . H39A H -0.2959 0.7806 0.8068 0.085 Uiso 1 1 calc R . . H39B H -0.2758 0.6862 0.7799 0.085 Uiso 1 1 calc R . . C40 C -0.3825(8) 0.7787(12) 0.7464(7) 0.104(6) Uani 1 1 d . . . H40A H -0.4044 0.8424 0.7432 0.156 Uiso 1 1 calc R . . H40B H -0.4249 0.7571 0.7800 0.156 Uiso 1 1 calc R . . H40C H -0.3762 0.7555 0.7030 0.156 Uiso 1 1 calc R . . C41 C 0.1342(6) 0.8072(6) 0.3460(4) 0.028(2) Uani 1 1 d . . . C42 C 0.1728(6) 0.8711(6) 0.3558(4) 0.032(2) Uani 1 1 d . . . C43 C 0.1241(6) 0.9586(6) 0.3677(4) 0.029(2) Uani 1 1 d . . . H43 H 0.0617 0.9795 0.3700 0.034 Uiso 1 1 calc R . . C44 C 0.1715(9) 1.0144(8) 0.3761(5) 0.054(3) Uani 1 1 d . . . H44 H 0.1409 1.0745 0.3821 0.064 Uiso 1 1 calc R . . C45 C 0.2611(8) 0.9836(10) 0.3757(6) 0.066(4) Uani 1 1 d . . . H45 H 0.2901 1.0223 0.3841 0.079 Uiso 1 1 calc R . . C46 C 0.3095(8) 0.8991(9) 0.3635(5) 0.053(3) Uani 1 1 d . . . C47 C 0.2695(7) 0.8389(7) 0.3514(5) 0.039(3) Uani 1 1 d . . . C48 C 0.3153(8) 0.7562(9) 0.3336(5) 0.060(3) Uani 1 1 d . . . H48 H 0.3782 0.7380 0.3282 0.072 Uiso 1 1 calc R . . C49 C 0.2749(7) 0.6953(7) 0.3228(5) 0.046(3) Uani 1 1 d . . . H49 H 0.3098 0.6381 0.3100 0.055 Uiso 1 1 calc R . . C50 C 0.1838(7) 0.7214(7) 0.3312(5) 0.041(3) Uani 1 1 d . . . H50 H 0.1547 0.6808 0.3269 0.050 Uiso 1 1 calc R . . C51 C 0.4438(9) 0.9371(11) 0.3471(8) 0.106(6) Uani 1 1 d . . . H51A H 0.4206 0.9773 0.3838 0.159 Uiso 1 1 calc R . . H51B H 0.4293 0.9686 0.3057 0.159 Uiso 1 1 calc R . . H51C H 0.5085 0.9125 0.3417 0.159 Uiso 1 1 calc R . . C52 C 0.4278(9) 0.8061(12) 0.4207(8) 0.100(6) Uani 1 1 d . . . H52A H 0.4216 0.8392 0.4594 0.150 Uiso 1 1 calc R . . H52B H 0.4892 0.7681 0.4086 0.150 Uiso 1 1 calc R . . H52C H 0.3874 0.7708 0.4317 0.150 Uiso 1 1 calc R . . C53 C -0.2988(6) 0.7913(6) 0.4405(4) 0.031(2) Uani 1 1 d . . . C54 C -0.3301(6) 0.8793(6) 0.4166(4) 0.024(2) Uani 1 1 d . . . C55 C -0.3817(6) 0.9500(6) 0.4592(4) 0.025(2) Uani 1 1 d . . . H55 H -0.3945 0.9403 0.5062 0.031 Uiso 1 1 calc R . . C56 C -0.4124(6) 1.0323(7) 0.4309(5) 0.035(3) Uani 1 1 d . . . H56 H -0.4477 1.0790 0.4589 0.042 Uiso 1 1 calc R . . C57 C -0.3921(7) 1.0486(7) 0.3605(5) 0.037(3) Uani 1 1 d . . . H57 H -0.4154 1.1056 0.3422 0.045 Uiso 1 1 calc R . . C58 C -0.3397(7) 0.9835(7) 0.3191(4) 0.036(3) Uani 1 1 d . . . C59 C -0.3106(6) 0.8967(6) 0.3465(4) 0.027(2) Uani 1 1 d . . . C60 C -0.2655(6) 0.8282(7) 0.3037(5) 0.039(3) Uani 1 1 d . . . H60 H -0.2533 0.8398 0.2568 0.047 Uiso 1 1 calc R . . C61 C -0.2380(7) 0.7425(7) 0.3295(5) 0.039(3) Uani 1 1 d . . . H61 H -0.2096 0.6961 0.2999 0.046 Uiso 1 1 calc R . . C62 C -0.2523(7) 0.7244(7) 0.3995(5) 0.038(3) Uani 1 1 d . . . H62 H -0.2300 0.6669 0.4172 0.046 Uiso 1 1 calc R . . C63 C -0.3742(13) 1.0776(15) 0.2185(9) 0.142(6) Uani 1 1 d . . . H63A H -0.4366 1.0818 0.2368 0.213 Uiso 1 1 calc R . . H63B H -0.3620 1.0747 0.1699 0.213 Uiso 1 1 calc R . . H63C H -0.3624 1.1289 0.2302 0.213 Uiso 1 1 calc R . . C64 C -0.2205(10) 0.9934(13) 0.2285(7) 0.110(4) Uani 1 1 d . . . H64A H -0.2130 1.0429 0.2469 0.164 Uiso 1 1 calc R . . H64B H -0.2026 0.9964 0.1797 0.164 Uiso 1 1 calc R . . H64C H -0.1834 0.9391 0.2462 0.164 Uiso 1 1 calc R . . C65 C 0.0260(7) 0.2653(6) 0.9090(5) 0.038(3) Uani 1 1 d . . . C66 C -0.0434(7) 0.2964(7) 0.9667(5) 0.040(3) Uani 1 1 d . . . C67 C -0.0376(8) 0.3388(8) 1.0185(5) 0.057(3) Uani 1 1 d . . . H67 H 0.0166 0.3497 1.0179 0.068 Uiso 1 1 calc R . . C68 C -0.1078(8) 0.3662(9) 1.0713(5) 0.064(4) Uani 1 1 d . . . H68 H -0.1007 0.3928 1.1075 0.077 Uiso 1 1 calc R . . C69 C -0.1885(9) 0.3550(10) 1.0719(6) 0.079(5) Uani 1 1 d . . . H69 H -0.2365 0.3746 1.1086 0.095 Uiso 1 1 calc R . . C70 C -0.2011(9) 0.3169(10) 1.0216(7) 0.077(4) Uani 1 1 d . . . C71 C -0.1251(9) 0.2808(8) 0.9663(5) 0.060(4) Uani 1 1 d . . . C72 C -0.1369(9) 0.2465(10) 0.9110(6) 0.078(5) Uani 1 1 d . . . H72 H -0.1937 0.2429 0.9098 0.094 Uiso 1 1 calc R . . C73 C -0.0671(11) 0.2181(9) 0.8583(6) 0.076(4) Uani 1 1 d . . . H73 H -0.0734 0.1883 0.8235 0.091 Uiso 1 1 calc R . . C74 C 0.0110(9) 0.2330(7) 0.8563(5) 0.051(3) Uani 1 1 d . . . H74 H 0.0563 0.2204 0.8171 0.061 Uiso 1 1 calc R . . C75 C -0.2735(11) 0.2082(11) 1.0454(9) 0.142(6) Uani 1 1 d . . . H75A H -0.2220 0.1698 1.0165 0.213 Uiso 1 1 calc R . . H75B H -0.3270 0.1934 1.0443 0.213 Uiso 1 1 calc R . . H75C H -0.2640 0.2010 1.0913 0.213 Uiso 1 1 calc RD . . C76 C -0.3618(9) 0.3489(11) 1.0709(7) 0.110(4) Uani 1 1 d . . . H76A H -0.3675 0.3079 1.1091 0.164 Uiso 1 1 calc RD . . H76B H -0.4160 0.3667 1.0528 0.164 Uiso 1 1 calc R . . H76C H -0.3529 0.4002 1.0854 0.164 Uiso 1 1 calc R . . C77 C 0.4326(6) 0.2998(7) 0.8110(4) 0.032(2) Uani 1 1 d . . . C78 C 0.4389(7) 0.2936(7) 0.8801(5) 0.042(3) Uani 1 1 d . . . C79 C 0.4553(7) 0.3599(8) 0.9088(5) 0.046(3) Uani 1 1 d . . . H79 H 0.4628 0.4104 0.8833 0.056 Uiso 1 1 calc R . . C80 C 0.4604(8) 0.3480(9) 0.9780(6) 0.064(4) Uani 1 1 d . . . H80 H 0.4691 0.3927 0.9990 0.077 Uiso 1 1 calc R . . C81 C 0.4532(9) 0.2751(13) 1.0144(7) 0.087(5) Uani 1 1 d . . . H81 H 0.4602 0.2676 1.0594 0.104 Uiso 1 1 calc R . . C82 C 0.4342(9) 0.2070(10) 0.9836(7) 0.077(5) Uani 1 1 d . . . C83 C 0.4296(7) 0.2166(8) 0.9179(5) 0.050(3) Uani 1 1 d . . . C84 C 0.4156(9) 0.1506(8) 0.8837(7) 0.062(4) Uani 1 1 d . . . H84 H 0.4110 0.0982 0.9075 0.074 Uiso 1 1 calc R . . C85 C 0.4090(8) 0.1611(8) 0.8208(7) 0.064(4) Uani 1 1 d . . . H85 H 0.3984 0.1174 0.8000 0.077 Uiso 1 1 calc R . . C86 C 0.4179(7) 0.2379(8) 0.7839(6) 0.051(3) Uani 1 1 d . . . H86 H 0.4131 0.2448 0.7383 0.061 Uiso 1 1 calc R . . C87 C 0.4735(12) 0.1019(12) 1.0772(8) 0.137(8) Uani 1 1 d . . . H87A H 0.5327 0.1094 1.0645 0.205 Uiso 1 1 calc R . . H87B H 0.4794 0.0407 1.0900 0.205 Uiso 1 1 calc R . . H87C H 0.4384 0.1381 1.1150 0.205 Uiso 1 1 calc R . . C88 C 0.3368(12) 0.1254(12) 1.0399(9) 0.138(8) Uani 1 1 d . . . H88A H 0.3008 0.1738 1.0687 0.206 Uiso 1 1 calc R . . H88B H 0.3362 0.0702 1.0644 0.206 Uiso 1 1 calc R . . H88C H 0.3120 0.1302 1.0000 0.206 Uiso 1 1 calc R . . N4 N 0.4047(6) 0.8691(8) 0.3617(6) 0.070(3) Uani 1 1 d . . . N6 N -0.3147(7) 0.9963(8) 0.2476(5) 0.073(2) Uani 1 1 d . . . N18 N -0.2858(7) 0.3071(8) 1.0194(5) 0.073(2) Uani 1 1 d . . . N20 N 0.4286(8) 0.1283(8) 1.0201(6) 0.086(4) Uani 1 1 d . . . O4 O -0.0140(4) 0.8674(4) 0.4317(3) 0.0265(15) Uani 1 1 d . . . O6 O -0.2786(4) 0.8157(4) 0.5605(3) 0.0242(14) Uani 1 1 d . . . O11 O 0.3072(5) 0.4369(4) 0.6101(3) 0.0400(18) Uani 1 1 d . . . H11 H 0.3299 0.4398 0.6422 0.060 Uiso 1 1 calc R . . O13 O 0.1327(5) 0.6135(4) 0.4606(3) 0.0428(18) Uani 1 1 d . . . H13 H 0.1270 0.5664 0.4525 0.064 Uiso 1 1 calc R . . O18 O 0.1049(4) 0.3818(4) 0.9049(3) 0.0302(16) Uani 1 1 d . . . O20 O 0.3599(4) 0.4687(4) 0.7969(3) 0.0319(16) Uani 1 1 d . . . O25 O -0.1325(4) 0.5473(4) 0.5757(3) 0.0323(16) Uani 1 1 d . . . H25 H -0.1672 0.5974 0.5700 0.049 Uiso 1 1 calc R . . O27 O 0.0347(5) 0.3614(4) 0.7239(3) 0.0376(17) Uani 1 1 d . . . H27 H 0.0422 0.3265 0.6944 0.056 Uiso 1 1 calc R . . O41 O -0.0137(4) 0.9047(4) 0.3173(3) 0.0336(12) Uani 1 1 d . . . O42 O -0.0068(4) 0.7554(4) 0.3575(3) 0.0341(17) Uani 1 1 d . . . O61 O -0.4134(4) 0.7936(4) 0.5543(3) 0.0376(17) Uani 1 1 d . . . O62 O -0.2781(4) 0.6719(4) 0.5349(3) 0.0336(12) Uani 1 1 d . . . O181 O 0.1629(5) 0.2448(5) 0.9617(3) 0.053(2) Uani 1 1 d . . . O182 O 0.1872(5) 0.2500(5) 0.8406(3) 0.051(2) Uani 1 1 d . . . O201 O 0.5163(4) 0.4142(5) 0.7644(4) 0.051(2) Uani 1 1 d . . . O202 O 0.4235(4) 0.3824(5) 0.6978(3) 0.046(2) Uani 1 1 d . . . S4 S 0.01807(16) 0.83263(16) 0.35795(11) 0.0306(6) Uani 1 1 d . . . S6 S -0.32194(16) 0.76202(16) 0.52564(12) 0.0299(6) Uani 1 1 d . . . S18 S 0.13061(18) 0.27839(18) 0.90310(12) 0.0407(7) Uani 1 1 d . . . S20 S 0.43945(17) 0.39258(18) 0.76017(13) 0.0394(7) Uani 1 1 d . . . C96 C -0.3480(15) 0.4652(15) 0.8211(11) 0.047(6) Uiso 0.50 1 d P A 1 Cl1 Cl -0.2657(6) 0.4941(6) 0.7629(4) 0.078(2) Uiso 0.50 1 d P A 1 Cl2 Cl -0.4177(5) 0.5708(5) 0.8434(3) 0.180(3) Uiso 0.50 1 d P A 1 Cl3 Cl -0.3285(7) 0.4214(6) 0.8963(5) 0.113(3) Uiso 0.50 1 d P A 1 C96B C -0.352(2) 0.5019(19) 0.7780(14) 0.078(8) Uiso 0.50 1 d P B 2 Cl1B Cl -0.2389(6) 0.4468(6) 0.7839(4) 0.084(2) Uiso 0.50 1 d P B 2 Cl2B Cl -0.4177(5) 0.5708(5) 0.8434(3) 0.180(3) Uiso 0.50 1 d P B 2 Cl3B Cl -0.3462(8) 0.5561(7) 0.6978(5) 0.133(4) Uiso 0.50 1 d P B 2 N90 N -0.0002(16) 1.0601(15) 0.2221(11) 0.078(7) Uiso 0.50 1 d P . . C91 C -0.046(2) 1.109(2) 0.1860(15) 0.089(9) Uiso 0.50 1 d P . . C92 C -0.0880(15) 1.1588(15) 0.1470(10) 0.050(6) Uiso 0.50 1 d P . . H92A H -0.0775 1.2153 0.1442 0.074 Uiso 0.50 1 calc PR . . H92B H -0.1515 1.1666 0.1632 0.074 Uiso 0.50 1 calc PR . . H92C H -0.0685 1.1342 0.1028 0.074 Uiso 0.50 1 calc PR . . 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 C1 0.020(6) 0.015(5) 0.039(5) 0.000(4) -0.011(4) -0.005(4) C2 0.022(6) 0.027(6) 0.047(6) -0.002(5) -0.020(5) -0.013(5) C3 0.012(5) 0.028(6) 0.032(5) -0.009(4) -0.002(4) -0.006(4) C4 0.015(5) 0.023(5) 0.023(5) -0.011(4) -0.004(4) -0.005(4) C5 0.038(7) 0.040(6) 0.026(5) 0.002(4) -0.009(5) -0.025(5) C6 0.013(5) 0.026(6) 0.045(6) -0.020(5) -0.010(4) -0.001(4) C7 0.021(6) 0.028(6) 0.031(5) -0.005(4) -0.005(4) 0.004(5) C8 0.014(5) 0.029(6) 0.024(5) -0.013(4) -0.006(4) -0.008(4) C9 0.021(6) 0.026(6) 0.031(5) -0.005(4) 0.000(4) 0.002(5) C10 0.009(5) 0.039(6) 0.031(5) -0.004(4) -0.003(4) -0.012(5) C11 0.022(6) 0.026(6) 0.045(6) -0.022(5) -0.010(5) -0.004(5) C12 0.024(6) 0.030(6) 0.030(5) -0.013(4) -0.002(4) -0.004(5) C13 0.015(5) 0.032(6) 0.029(5) -0.009(4) -0.015(4) -0.002(5) C14 0.026(6) 0.029(6) 0.027(5) -0.002(4) -0.001(4) -0.017(5) C15 0.030(6) 0.037(6) 0.036(6) -0.019(5) -0.010(5) -0.012(5) C16 0.022(6) 0.041(6) 0.026(5) -0.006(4) -0.008(4) -0.008(5) C17 0.021(5) 0.044(6) 0.014(4) 0.001(4) -0.007(4) -0.012(5) C18 0.030(6) 0.028(6) 0.025(5) -0.007(4) 0.017(4) -0.006(5) C19 0.010(5) 0.040(6) 0.040(6) -0.011(5) -0.015(4) -0.004(5) C20 0.028(6) 0.040(6) 0.026(5) -0.006(4) -0.012(4) -0.017(5) C21 0.019(5) 0.054(7) 0.020(5) -0.004(4) -0.002(4) -0.022(5) C22 0.006(5) 0.025(6) 0.023(5) 0.003(4) -0.004(4) 0.003(4) C23 0.013(5) 0.025(6) 0.036(5) -0.009(4) -0.007(4) -0.004(4) C24 0.008(5) 0.022(5) 0.025(5) -0.005(4) -0.012(4) 0.007(4) C25 0.019(5) 0.027(6) 0.028(5) -0.010(4) -0.006(4) -0.007(5) C26 0.028(6) 0.040(6) 0.019(5) -0.005(4) -0.008(4) -0.012(5) C27 0.010(5) 0.012(5) 0.034(5) -0.002(4) -0.006(4) 0.007(4) C28 0.012(5) 0.032(6) 0.030(5) -0.007(4) -0.008(4) -0.007(4) C29 0.024(6) 0.016(5) 0.039(5) 0.003(4) -0.011(4) -0.004(4) C30 0.036(6) 0.022(6) 0.040(6) 0.009(4) -0.010(5) -0.018(5) C31 0.039(8) 0.076(10) 0.149(13) -0.066(9) -0.019(8) -0.027(7) C32 0.055(8) 0.037(7) 0.040(6) -0.001(5) -0.023(5) -0.019(6) C33 0.052(8) 0.031(7) 0.089(9) 0.010(6) -0.044(7) -0.025(6) C34 0.085(12) 0.061(9) 0.115(11) 0.021(8) -0.029(9) -0.042(9) C35 0.022(5) 0.035(6) 0.012(4) -0.012(4) -0.001(4) -0.013(5) C36 0.034(7) 0.052(7) 0.033(6) -0.013(5) -0.001(5) -0.002(6) C37 0.040(8) 0.170(16) 0.051(8) -0.040(9) 0.022(6) -0.040(9) C38 0.026(6) 0.035(6) 0.034(5) -0.016(5) 0.000(5) 0.003(5) C39 0.081(11) 0.061(9) 0.056(8) -0.009(6) -0.002(7) -0.006(8) C40 0.019(8) 0.179(18) 0.093(11) -0.020(11) -0.010(7) 0.003(9) C41 0.023(6) 0.023(6) 0.031(5) -0.013(4) 0.002(4) 0.001(5) C42 0.028(6) 0.039(7) 0.035(5) -0.011(5) -0.006(4) -0.014(5) C43 0.023(6) 0.023(6) 0.046(6) -0.015(4) -0.003(4) -0.013(5) C44 0.066(10) 0.052(8) 0.048(7) -0.007(6) 0.006(6) -0.035(7) C45 0.030(8) 0.106(12) 0.070(8) -0.029(8) 0.001(6) -0.033(8) C46 0.037(8) 0.078(10) 0.049(7) -0.031(7) 0.008(6) -0.025(7) C47 0.037(7) 0.047(7) 0.033(6) -0.016(5) -0.002(5) -0.012(6) C48 0.039(8) 0.084(10) 0.053(7) -0.028(7) -0.003(6) -0.011(8) C49 0.016(6) 0.041(7) 0.070(8) -0.022(6) 0.003(5) 0.004(5) C50 0.032(7) 0.036(7) 0.061(7) -0.020(5) -0.023(5) -0.002(5) C51 0.056(10) 0.151(16) 0.135(13) -0.092(12) 0.021(9) -0.063(11) C52 0.038(9) 0.154(16) 0.105(12) -0.030(11) -0.037(8) -0.003(10) C53 0.021(5) 0.029(6) 0.033(5) -0.017(5) -0.005(4) 0.010(5) C54 0.013(5) 0.027(6) 0.032(5) -0.009(4) -0.002(4) -0.005(4) C55 0.021(5) 0.030(6) 0.025(5) 0.002(4) -0.011(4) -0.005(5) C56 0.021(6) 0.047(7) 0.036(6) -0.017(5) -0.001(4) -0.008(5) C57 0.033(6) 0.028(6) 0.047(7) 0.003(5) -0.009(5) -0.005(5) C58 0.029(6) 0.062(8) 0.024(5) -0.007(5) -0.005(5) -0.023(6) C59 0.019(5) 0.029(6) 0.031(5) -0.007(5) -0.006(4) -0.004(5) C60 0.021(6) 0.063(8) 0.028(5) -0.011(5) 0.000(4) -0.006(6) C61 0.028(6) 0.030(7) 0.055(7) -0.010(5) -0.012(5) -0.001(5) C62 0.033(6) 0.043(7) 0.036(6) -0.009(5) -0.014(5) 0.000(5) C63 0.120(12) 0.216(18) 0.106(10) 0.011(10) -0.034(8) -0.074(12) C64 0.072(8) 0.183(13) 0.075(7) -0.019(8) 0.016(6) -0.057(9) C65 0.034(6) 0.033(6) 0.041(6) 0.000(5) 0.003(5) -0.009(5) C66 0.040(7) 0.056(7) 0.031(6) -0.018(5) -0.008(5) -0.020(6) C67 0.038(7) 0.078(9) 0.057(7) -0.028(7) 0.000(6) -0.020(7) C68 0.053(9) 0.097(11) 0.042(7) -0.022(7) 0.013(6) -0.032(8) C69 0.045(9) 0.138(14) 0.058(8) -0.049(9) 0.010(6) -0.031(9) C70 0.052(9) 0.121(13) 0.081(9) -0.034(9) 0.007(7) -0.061(9) C71 0.066(9) 0.081(10) 0.046(7) 0.003(6) 0.001(6) -0.054(8) C72 0.069(10) 0.126(13) 0.069(9) -0.038(9) -0.001(8) -0.069(10) C73 0.107(13) 0.085(11) 0.057(8) -0.018(7) -0.017(8) -0.054(10) C74 0.066(9) 0.052(8) 0.038(6) -0.016(5) -0.003(6) -0.024(7) C75 0.120(12) 0.216(18) 0.106(10) 0.011(10) -0.034(8) -0.074(12) C76 0.072(8) 0.183(13) 0.075(7) -0.019(8) 0.016(6) -0.057(9) C77 0.020(6) 0.044(7) 0.030(5) -0.008(5) -0.004(4) -0.005(5) C78 0.026(6) 0.039(7) 0.056(7) -0.017(6) -0.011(5) 0.003(5) C79 0.033(7) 0.058(8) 0.045(7) 0.000(6) -0.016(5) -0.004(6) C80 0.053(9) 0.068(10) 0.060(8) -0.005(7) -0.017(7) 0.001(7) C81 0.065(10) 0.137(16) 0.047(8) 0.003(10) -0.024(7) -0.009(11) C82 0.051(9) 0.076(11) 0.078(10) 0.043(9) -0.012(7) 0.001(8) C83 0.043(7) 0.053(8) 0.037(6) 0.011(6) -0.009(5) 0.003(6) C84 0.070(10) 0.047(8) 0.071(9) 0.013(7) -0.010(7) -0.029(7) C85 0.056(9) 0.047(9) 0.087(10) -0.020(7) -0.032(8) 0.004(7) C86 0.042(7) 0.052(8) 0.049(7) -0.004(6) -0.001(6) -0.006(6) C87 0.104(14) 0.162(18) 0.115(13) 0.079(13) -0.066(12) 0.003(13) C88 0.110(16) 0.134(17) 0.140(16) 0.067(13) 0.018(12) -0.052(13) N4 0.024(6) 0.096(9) 0.095(8) -0.051(7) 0.007(6) -0.022(6) N6 0.047(5) 0.094(7) 0.080(5) -0.009(5) -0.003(4) -0.029(5) N18 0.047(5) 0.094(7) 0.080(5) -0.009(5) -0.003(4) -0.029(5) N20 0.081(9) 0.085(9) 0.078(8) 0.035(7) -0.017(7) -0.018(7) O4 0.021(4) 0.027(4) 0.029(3) -0.006(3) -0.005(3) -0.003(3) O6 0.016(4) 0.025(4) 0.032(3) -0.006(3) -0.012(3) -0.001(3) O11 0.048(5) 0.018(4) 0.054(5) -0.003(3) -0.033(4) 0.005(4) O13 0.048(5) 0.033(4) 0.056(4) -0.007(3) -0.024(4) -0.014(4) O18 0.023(4) 0.032(4) 0.031(3) -0.009(3) 0.000(3) -0.004(3) O20 0.010(4) 0.045(4) 0.038(4) -0.016(3) -0.009(3) 0.003(3) O25 0.033(4) 0.026(4) 0.039(4) -0.007(3) -0.025(3) 0.003(3) O27 0.049(5) 0.026(4) 0.040(4) -0.010(3) -0.024(4) -0.001(4) O41 0.038(3) 0.019(3) 0.045(3) 0.004(2) -0.022(2) -0.003(2) O42 0.041(4) 0.032(4) 0.032(3) -0.015(3) -0.001(3) -0.015(3) O61 0.008(4) 0.053(5) 0.049(4) 0.013(3) -0.007(3) -0.010(3) O62 0.038(3) 0.019(3) 0.045(3) 0.004(2) -0.022(2) -0.003(2) O181 0.041(5) 0.056(5) 0.050(4) 0.020(4) -0.009(4) -0.006(4) O182 0.045(5) 0.047(5) 0.043(4) -0.019(3) 0.027(4) -0.009(4) O201 0.011(4) 0.061(5) 0.080(5) -0.005(4) -0.009(3) -0.011(4) O202 0.030(4) 0.063(5) 0.031(4) -0.018(3) -0.007(3) 0.010(4) S4 0.0288(15) 0.0350(16) 0.0298(13) -0.0065(11) -0.0042(11) -0.0118(13) S6 0.0156(14) 0.0282(15) 0.0448(15) -0.0040(11) -0.0106(11) -0.0015(11) S18 0.0360(17) 0.0444(18) 0.0358(15) -0.0027(13) -0.0021(13) -0.0079(14) S20 0.0218(15) 0.0484(18) 0.0431(16) -0.0074(13) -0.0055(12) -0.0031(13) _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 C1 C6 1.377(12) . ? C1 C2 1.409(12) . ? C1 C28 1.490(12) . ? C2 C3 1.411(12) . ? C3 C4 1.395(12) . ? C3 C7 1.495(13) . ? C4 C5 1.369(12) . ? C4 O4 1.428(10) . ? C5 C6 1.435(12) . ? C6 O6 1.430(10) . ? C7 C8 1.523(12) . ? C7 C29 1.552(12) . ? C8 C9 1.378(12) . ? C8 C13 1.402(12) . ? C9 C10 1.389(12) . ? C10 C11 1.420(12) . ? C10 C14 1.517(12) . ? C11 O11 1.356(11) . ? C11 C12 1.383(12) . ? C12 C13 1.346(12) . ? C13 O13 1.421(10) . ? C14 C15 1.545(12) . ? C14 C32 1.574(12) . ? C15 C20 1.376(13) . ? C15 C16 1.419(13) . ? C16 C17 1.350(12) . ? C17 C18 1.409(12) . ? C17 C21 1.527(12) . ? C18 C19 1.369(13) . ? C18 O18 1.440(10) . ? C19 C20 1.389(12) . ? C20 O20 1.435(11) . ? C21 C22 1.541(11) . ? C21 C35 1.563(12) . ? C22 C23 1.384(12) . ? C22 C27 1.401(12) . ? C23 C24 1.405(11) . ? C24 C25 1.356(11) . ? C24 C28 1.545(12) . ? C25 O25 1.369(10) . ? C25 C26 1.420(13) . ? C26 C27 1.380(11) . ? C27 O27 1.379(10) . ? C28 C38 1.522(12) . ? C29 C30 1.550(12) . ? C30 C31 1.516(13) . ? C32 C33 1.480(14) . ? C33 C34 1.502(17) . ? C35 C36 1.500(13) . ? C36 C37 1.479(14) . ? C38 C39 1.469(15) . ? C39 C40 1.547(18) . ? C41 C50 1.395(13) . ? C41 C42 1.429(13) . ? C41 S4 1.760(10) . ? C42 C43 1.405(13) . ? C42 C47 1.471(14) . ? C43 C44 1.414(14) . ? C44 C45 1.376(16) . ? C45 C46 1.363(17) . ? C46 C47 1.410(15) . ? C46 N4 1.456(15) . ? C47 C48 1.354(15) . ? C48 C49 1.413(16) . ? C49 C50 1.376(14) . ? C51 N4 1.419(16) . ? C52 N4 1.530(18) . ? C53 C62 1.360(13) . ? C53 C54 1.426(13) . ? C53 S6 1.752(9) . ? C54 C59 1.421(12) . ? C54 C55 1.435(12) . ? C55 C56 1.381(13) . ? C56 C57 1.426(13) . ? C57 C58 1.364(13) . ? C58 C59 1.431(13) . ? C58 N6 1.443(13) . ? C59 C60 1.397(13) . ? C60 C61 1.401(14) . ? C61 C62 1.419(13) . ? C63 N6 1.52(2) . ? C64 N6 1.477(17) . ? C65 C74 1.359(14) . ? C65 C66 1.445(13) . ? C65 S18 1.756(11) . ? C66 C67 1.371(14) . ? C66 C71 1.432(15) . ? C67 C68 1.376(14) . ? C68 C69 1.378(17) . ? C69 C70 1.351(16) . ? C70 N18 1.447(15) . ? C70 C71 1.482(17) . ? C71 C72 1.399(16) . ? C72 C73 1.373(18) . ? C73 C74 1.357(17) . ? C75 N18 1.600(19) . ? C76 N18 1.459(16) . ? C77 C86 1.313(14) . ? C77 C78 1.439(13) . ? C77 S20 1.757(10) . ? C78 C79 1.410(15) . ? C78 C83 1.431(15) . ? C79 C80 1.435(15) . ? C80 C81 1.352(19) . ? C81 C82 1.48(2) . ? C82 C83 1.360(17) . ? C82 N20 1.427(16) . ? C83 C84 1.451(16) . ? C84 C85 1.310(16) . ? C85 C86 1.419(16) . ? C87 N20 1.476(17) . ? C88 N20 1.469(19) . ? O4 S4 1.593(6) . ? O6 S6 1.596(6) . ? O18 S18 1.599(7) . ? O20 S20 1.580(6) . ? O41 S4 1.389(6) . ? O42 S4 1.440(6) . ? O61 S6 1.410(6) . ? O62 S6 1.419(6) . ? O181 S18 1.409(7) . ? O182 S18 1.425(6) . ? O201 S20 1.425(7) . ? O202 S20 1.404(7) . ? C96 Cl3 1.68(2) . ? C96 Cl1 1.73(2) . ? C96 Cl2 1.77(2) . ? C96B Cl3B 1.78(3) . ? C96B Cl1B 1.79(3) . ? N90 C91 1.21(3) . ? C91 C92 1.23(3) . ? 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 C6 C1 C2 115.5(8) . . ? C6 C1 C28 123.4(8) . . ? C2 C1 C28 120.8(8) . . ? C1 C2 C3 123.8(8) . . ? C4 C3 C2 116.2(8) . . ? C4 C3 C7 122.2(8) . . ? C2 C3 C7 121.5(8) . . ? C5 C4 C3 124.2(8) . . ? C5 C4 O4 115.7(8) . . ? C3 C4 O4 119.4(7) . . ? C4 C5 C6 116.0(8) . . ? C1 C6 O6 120.5(8) . . ? C1 C6 C5 124.1(8) . . ? O6 C6 C5 115.2(8) . . ? C3 C7 C8 112.0(8) . . ? C3 C7 C29 108.7(7) . . ? C8 C7 C29 113.1(7) . . ? C9 C8 C13 114.6(8) . . ? C9 C8 C7 125.5(8) . . ? C13 C8 C7 119.8(7) . . ? C8 C9 C10 124.8(9) . . ? C9 C10 C11 117.0(8) . . ? C9 C10 C14 124.5(8) . . ? C11 C10 C14 118.5(8) . . ? O11 C11 C12 116.5(8) . . ? O11 C11 C10 124.0(8) . . ? C12 C11 C10 119.4(9) . . ? C13 C12 C11 120.1(9) . . ? C12 C13 C8 124.0(8) . . ? C12 C13 O13 121.6(8) . . ? C8 C13 O13 114.4(8) . . ? C10 C14 C15 111.8(7) . . ? C10 C14 C32 114.5(8) . . ? C15 C14 C32 110.5(7) . . ? C20 C15 C16 115.8(9) . . ? C20 C15 C14 121.9(8) . . ? C16 C15 C14 122.2(9) . . ? C17 C16 C15 124.0(9) . . ? C16 C17 C18 115.9(8) . . ? C16 C17 C21 123.6(8) . . ? C18 C17 C21 120.4(8) . . ? C19 C18 C17 124.1(8) . . ? C19 C18 O18 117.7(8) . . ? C17 C18 O18 118.1(8) . . ? C18 C19 C20 116.3(9) . . ? C15 C20 C19 123.8(9) . . ? C15 C20 O20 120.5(8) . . ? C19 C20 O20 115.7(8) . . ? C17 C21 C22 113.9(7) . . ? C17 C21 C35 109.0(7) . . ? C22 C21 C35 113.3(8) . . ? C23 C22 C27 118.7(8) . . ? C23 C22 C21 124.1(8) . . ? C27 C22 C21 117.3(7) . . ? C22 C23 C24 122.1(8) . . ? C25 C24 C23 117.7(8) . . ? C25 C24 C28 120.6(7) . . ? C23 C24 C28 121.8(8) . . ? C24 C25 O25 125.8(8) . . ? C24 C25 C26 122.4(8) . . ? O25 C25 C26 111.8(7) . . ? C27 C26 C25 118.4(8) . . ? O27 C27 C26 121.5(8) . . ? O27 C27 C22 117.8(7) . . ? C26 C27 C22 120.7(8) . . ? C1 C28 C38 111.3(7) . . ? C1 C28 C24 111.2(7) . . ? C38 C28 C24 115.2(7) . . ? C30 C29 C7 113.7(7) . . ? C31 C30 C29 110.7(8) . . ? C33 C32 C14 113.6(8) . . ? C32 C33 C34 114.6(9) . . ? C36 C35 C21 114.0(7) . . ? C37 C36 C35 113.9(9) . . ? C39 C38 C28 116.2(9) . . ? C38 C39 C40 113.2(10) . . ? C50 C41 C42 123.3(9) . . ? C50 C41 S4 116.2(7) . . ? C42 C41 S4 120.3(7) . . ? C43 C42 C41 123.7(9) . . ? C43 C42 C47 121.4(9) . . ? C41 C42 C47 114.8(9) . . ? C42 C43 C44 117.3(9) . . ? C45 C44 C43 121.4(12) . . ? C46 C45 C44 121.9(12) . . ? C45 C46 C47 121.3(11) . . ? C45 C46 N4 120.5(11) . . ? C47 C46 N4 118.3(11) . . ? C48 C47 C46 123.8(11) . . ? C48 C47 C42 119.6(10) . . ? C46 C47 C42 116.5(10) . . ? C47 C48 C49 123.8(11) . . ? C50 C49 C48 118.2(10) . . ? C49 C50 C41 120.0(10) . . ? C62 C53 C54 123.1(9) . . ? C62 C53 S6 115.4(8) . . ? C54 C53 S6 121.4(7) . . ? C59 C54 C53 117.6(8) . . ? C59 C54 C55 118.8(8) . . ? C53 C54 C55 123.6(8) . . ? C56 C55 C54 119.2(8) . . ? C55 C56 C57 121.3(9) . . ? C58 C57 C56 120.8(9) . . ? C57 C58 C59 119.2(8) . . ? C57 C58 N6 123.4(10) . . ? C59 C58 N6 117.3(9) . . ? C60 C59 C54 119.9(9) . . ? C60 C59 C58 119.5(8) . . ? C54 C59 C58 120.6(8) . . ? C59 C60 C61 120.4(9) . . ? C60 C61 C62 120.5(9) . . ? C53 C62 C61 118.3(9) . . ? C74 C65 C66 122.2(10) . . ? C74 C65 S18 118.4(8) . . ? C66 C65 S18 119.2(8) . . ? C67 C66 C71 119.5(10) . . ? C67 C66 C65 126.4(10) . . ? C71 C66 C65 114.0(9) . . ? C66 C67 C68 122.1(11) . . ? C67 C68 C69 120.2(12) . . ? C70 C69 C68 121.6(11) . . ? C69 C70 N18 123.0(12) . . ? C69 C70 C71 119.6(11) . . ? N18 C70 C71 117.4(11) . . ? C72 C71 C66 121.2(11) . . ? C72 C71 C70 121.2(12) . . ? C66 C71 C70 116.7(10) . . ? C73 C72 C71 120.7(12) . . ? C74 C73 C72 119.4(12) . . ? C73 C74 C65 121.7(11) . . ? C86 C77 C78 121.6(10) . . ? C86 C77 S20 117.0(8) . . ? C78 C77 S20 121.4(8) . . ? C79 C78 C83 121.5(10) . . ? C79 C78 C77 121.3(10) . . ? C83 C78 C77 117.2(10) . . ? C78 C79 C80 117.2(11) . . ? C81 C80 C79 122.2(13) . . ? C80 C81 C82 119.7(12) . . ? C83 C82 N20 119.7(16) . . ? C83 C82 C81 119.1(12) . . ? N20 C82 C81 121.0(14) . . ? C82 C83 C78 120.2(13) . . ? C82 C83 C84 122.1(12) . . ? C78 C83 C84 117.7(9) . . ? C85 C84 C83 121.9(11) . . ? C84 C85 C86 119.9(12) . . ? C77 C86 C85 121.7(11) . . ? C51 N4 C46 113.0(12) . . ? C51 N4 C52 117.5(12) . . ? C46 N4 C52 111.8(10) . . ? C58 N6 C64 110.1(10) . . ? C58 N6 C63 114.6(11) . . ? C64 N6 C63 111.2(13) . . ? C70 N18 C76 117.0(11) . . ? C70 N18 C75 102.3(12) . . ? C76 N18 C75 98.3(9) . . ? C82 N20 C88 112.3(12) . . ? C82 N20 C87 117.5(14) . . ? C88 N20 C87 110.3(12) . . ? C4 O4 S4 120.2(5) . . ? C6 O6 S6 119.4(5) . . ? C18 O18 S18 119.3(5) . . ? C20 O20 S20 118.6(6) . . ? O41 S4 O42 120.1(4) . . ? O41 S4 O4 104.8(4) . . ? O42 S4 O4 108.6(3) . . ? O41 S4 C41 109.0(4) . . ? O42 S4 C41 110.8(4) . . ? O4 S4 C41 101.8(4) . . ? O61 S6 O62 117.6(4) . . ? O61 S6 O6 103.5(4) . . ? O62 S6 O6 108.7(4) . . ? O61 S6 C53 112.3(4) . . ? O62 S6 C53 108.9(4) . . ? O6 S6 C53 104.9(4) . . ? O181 S18 O182 118.0(5) . . ? O181 S18 O18 105.9(4) . . ? O182 S18 O18 109.5(4) . . ? O181 S18 C65 110.2(5) . . ? O182 S18 C65 110.5(5) . . ? O18 S18 C65 101.2(4) . . ? O202 S20 O201 120.5(4) . . ? O202 S20 O20 109.3(4) . . ? O201 S20 O20 103.5(4) . . ? O202 S20 C77 108.0(5) . . ? O201 S20 C77 110.6(5) . . ? O20 S20 C77 103.7(4) . . ? Cl3 C96 Cl1 120.2(14) . . ? Cl3 C96 Cl2 100.5(12) . . ? Cl1 C96 Cl2 98.2(12) . . ? Cl3B C96B Cl1B 105.1(16) . . ? N90 C91 C92 177(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.5(13) . . . . ? C28 C1 C2 C3 -175.3(8) . . . . ? C1 C2 C3 C4 -2.2(13) . . . . ? C1 C2 C3 C7 174.3(8) . . . . ? C2 C3 C4 C5 4.5(13) . . . . ? C7 C3 C4 C5 -172.1(9) . . . . ? C2 C3 C4 O4 174.4(7) . . . . ? C7 C3 C4 O4 -2.2(12) . . . . ? C3 C4 C5 C6 -2.7(13) . . . . ? O4 C4 C5 C6 -173.0(7) . . . . ? C2 C1 C6 O6 -172.1(8) . . . . ? C28 C1 C6 O6 1.6(13) . . . . ? C2 C1 C6 C5 3.4(13) . . . . ? C28 C1 C6 C5 177.1(8) . . . . ? C4 C5 C6 C1 -1.5(13) . . . . ? C4 C5 C6 O6 174.2(7) . . . . ? C4 C3 C7 C8 -150.2(8) . . . . ? C2 C3 C7 C8 33.5(11) . . . . ? C4 C3 C7 C29 84.1(10) . . . . ? C2 C3 C7 C29 -92.3(10) . . . . ? C3 C7 C8 C9 -111.3(10) . . . . ? C29 C7 C8 C9 12.0(12) . . . . ? C3 C7 C8 C13 72.0(10) . . . . ? C29 C7 C8 C13 -164.7(8) . . . . ? C13 C8 C9 C10 2.0(13) . . . . ? C7 C8 C9 C10 -174.8(8) . . . . ? C8 C9 C10 C11 0.6(13) . . . . ? C8 C9 C10 C14 -178.6(8) . . . . ? C9 C10 C11 O11 -179.7(8) . . . . ? C14 C10 C11 O11 -0.5(13) . . . . ? C9 C10 C11 C12 -3.5(13) . . . . ? C14 C10 C11 C12 175.8(8) . . . . ? O11 C11 C12 C13 -179.9(8) . . . . ? C10 C11 C12 C13 3.6(14) . . . . ? C11 C12 C13 C8 -0.8(14) . . . . ? C11 C12 C13 O13 176.8(8) . . . . ? C9 C8 C13 C12 -2.0(13) . . . . ? C7 C8 C13 C12 175.0(8) . . . . ? C9 C8 C13 O13 -179.7(7) . . . . ? C7 C8 C13 O13 -2.7(12) . . . . ? C9 C10 C14 C15 110.9(10) . . . . ? C11 C10 C14 C15 -68.3(10) . . . . ? C9 C10 C14 C32 -15.7(12) . . . . ? C11 C10 C14 C32 165.1(8) . . . . ? C10 C14 C15 C20 149.4(9) . . . . ? C32 C14 C15 C20 -81.8(11) . . . . ? C10 C14 C15 C16 -35.3(12) . . . . ? C32 C14 C15 C16 93.4(10) . . . . ? C20 C15 C16 C17 -1.3(14) . . . . ? C14 C15 C16 C17 -176.8(8) . . . . ? C15 C16 C17 C18 -0.1(14) . . . . ? C15 C16 C17 C21 178.8(9) . . . . ? C16 C17 C18 C19 0.7(14) . . . . ? C21 C17 C18 C19 -178.3(9) . . . . ? C16 C17 C18 O18 177.5(8) . . . . ? C21 C17 C18 O18 -1.5(12) . . . . ? C17 C18 C19 C20 0.2(14) . . . . ? O18 C18 C19 C20 -176.6(7) . . . . ? C16 C15 C20 C19 2.4(13) . . . . ? C14 C15 C20 C19 177.9(8) . . . . ? C16 C15 C20 O20 -175.5(8) . . . . ? C14 C15 C20 O20 0.1(13) . . . . ? C18 C19 C20 C15 -1.8(14) . . . . ? C18 C19 C20 O20 176.1(8) . . . . ? C16 C17 C21 C22 27.2(13) . . . . ? C18 C17 C21 C22 -153.9(8) . . . . ? C16 C17 C21 C35 -100.4(10) . . . . ? C18 C17 C21 C35 78.5(11) . . . . ? C17 C21 C22 C23 -101.2(10) . . . . ? C35 C21 C22 C23 24.2(11) . . . . ? C17 C21 C22 C27 80.0(10) . . . . ? C35 C21 C22 C27 -154.7(7) . . . . ? C27 C22 C23 C24 1.6(13) . . . . ? C21 C22 C23 C24 -177.2(8) . . . . ? C22 C23 C24 C25 -0.6(13) . . . . ? C22 C23 C24 C28 179.0(8) . . . . ? C23 C24 C25 O25 179.4(8) . . . . ? C28 C24 C25 O25 -0.1(13) . . . . ? C23 C24 C25 C26 -1.5(13) . . . . ? C28 C24 C25 C26 179.0(8) . . . . ? C24 C25 C26 C27 2.4(13) . . . . ? O25 C25 C26 C27 -178.3(8) . . . . ? C25 C26 C27 O27 178.7(8) . . . . ? C25 C26 C27 C22 -1.3(13) . . . . ? C23 C22 C27 O27 179.4(8) . . . . ? C21 C22 C27 O27 -1.7(11) . . . . ? C23 C22 C27 C26 -0.6(13) . . . . ? C21 C22 C27 C26 178.3(8) . . . . ? C6 C1 C28 C38 -84.5(10) . . . . ? C2 C1 C28 C38 88.8(10) . . . . ? C6 C1 C28 C24 145.6(8) . . . . ? C2 C1 C28 C24 -41.1(11) . . . . ? C25 C24 C28 C1 -65.9(10) . . . . ? C23 C24 C28 C1 114.5(9) . . . . ? C25 C24 C28 C38 166.3(8) . . . . ? C23 C24 C28 C38 -13.2(12) . . . . ? C3 C7 C29 C30 -167.0(7) . . . . ? C8 C7 C29 C30 67.9(10) . . . . ? C7 C29 C30 C31 -171.9(9) . . . . ? C10 C14 C32 C33 -69.7(11) . . . . ? C15 C14 C32 C33 163.1(8) . . . . ? C14 C32 C33 C34 -78.7(12) . . . . ? C17 C21 C35 C36 -166.4(8) . . . . ? C22 C21 C35 C36 65.6(10) . . . . ? C21 C35 C36 C37 170.7(10) . . . . ? C1 C28 C38 C39 158.2(9) . . . . ? C24 C28 C38 C39 -74.1(11) . . . . ? C28 C38 C39 C40 -76.1(14) . . . . ? C50 C41 C42 C43 176.9(9) . . . . ? S4 C41 C42 C43 -7.4(12) . . . . ? C50 C41 C42 C47 -2.0(13) . . . . ? S4 C41 C42 C47 173.7(7) . . . . ? C41 C42 C43 C44 -179.6(9) . . . . ? C47 C42 C43 C44 -0.8(13) . . . . ? C42 C43 C44 C45 -2.9(15) . . . . ? C43 C44 C45 C46 3.7(18) . . . . ? C44 C45 C46 C47 -0.6(18) . . . . ? C44 C45 C46 N4 178.4(11) . . . . ? C45 C46 C47 C48 174.4(11) . . . . ? N4 C46 C47 C48 -4.7(16) . . . . ? C45 C46 C47 C42 -2.9(15) . . . . ? N4 C46 C47 C42 178.0(9) . . . . ? C43 C42 C47 C48 -173.8(9) . . . . ? C41 C42 C47 C48 5.1(13) . . . . ? C43 C42 C47 C46 3.7(14) . . . . ? C41 C42 C47 C46 -177.4(8) . . . . ? C46 C47 C48 C49 178.7(10) . . . . ? C42 C47 C48 C49 -4.1(16) . . . . ? C47 C48 C49 C50 -0.5(17) . . . . ? C48 C49 C50 C41 3.8(16) . . . . ? C42 C41 C50 C49 -2.5(15) . . . . ? S4 C41 C50 C49 -178.4(8) . . . . ? C62 C53 C54 C59 -0.6(14) . . . . ? S6 C53 C54 C59 -178.0(7) . . . . ? C62 C53 C54 C55 177.8(9) . . . . ? S6 C53 C54 C55 0.4(13) . . . . ? C59 C54 C55 C56 1.3(13) . . . . ? C53 C54 C55 C56 -177.0(9) . . . . ? C54 C55 C56 C57 -1.4(14) . . . . ? C55 C56 C57 C58 -1.8(14) . . . . ? C56 C57 C58 C59 4.8(14) . . . . ? C56 C57 C58 N6 -178.2(9) . . . . ? C53 C54 C59 C60 2.6(13) . . . . ? C55 C54 C59 C60 -175.9(8) . . . . ? C53 C54 C59 C58 -179.8(9) . . . . ? C55 C54 C59 C58 1.8(13) . . . . ? C57 C58 C59 C60 172.8(9) . . . . ? N6 C58 C59 C60 -4.3(13) . . . . ? C57 C58 C59 C54 -4.9(14) . . . . ? N6 C58 C59 C54 178.0(8) . . . . ? C54 C59 C60 C61 -1.0(14) . . . . ? C58 C59 C60 C61 -178.7(9) . . . . ? C59 C60 C61 C62 -2.7(15) . . . . ? C54 C53 C62 C61 -3.0(15) . . . . ? S6 C53 C62 C61 174.6(7) . . . . ? C60 C61 C62 C53 4.6(15) . . . . ? C74 C65 C66 C67 -172.1(11) . . . . ? S18 C65 C66 C67 2.1(16) . . . . ? C74 C65 C66 C71 6.7(15) . . . . ? S18 C65 C66 C71 -179.0(8) . . . . ? C71 C66 C67 C68 1.0(19) . . . . ? C65 C66 C67 C68 179.8(11) . . . . ? C66 C67 C68 C69 -3(2) . . . . ? C67 C68 C69 C70 0(2) . . . . ? C68 C69 C70 N18 -177.6(14) . . . . ? C68 C69 C70 C71 4(2) . . . . ? C67 C66 C71 C72 172.8(13) . . . . ? C65 C66 C71 C72 -6.2(17) . . . . ? C67 C66 C71 C70 3.4(18) . . . . ? C65 C66 C71 C70 -175.6(11) . . . . ? C69 C70 C71 C72 -175.3(14) . . . . ? N18 C70 C71 C72 6(2) . . . . ? C69 C70 C71 C66 -6(2) . . . . ? N18 C70 C71 C66 175.7(11) . . . . ? C66 C71 C72 C73 7(2) . . . . ? C70 C71 C72 C73 176.0(14) . . . . ? C71 C72 C73 C74 -8(2) . . . . ? C72 C73 C74 C65 9(2) . . . . ? C66 C65 C74 C73 -8.2(18) . . . . ? S18 C65 C74 C73 177.5(10) . . . . ? C86 C77 C78 C79 179.5(10) . . . . ? S20 C77 C78 C79 -3.3(13) . . . . ? C86 C77 C78 C83 0.8(15) . . . . ? S20 C77 C78 C83 178.0(8) . . . . ? C83 C78 C79 C80 -1.4(15) . . . . ? C77 C78 C79 C80 179.9(9) . . . . ? C78 C79 C80 C81 2.4(17) . . . . ? C79 C80 C81 C82 -4(2) . . . . ? C80 C81 C82 C83 4(2) . . . . ? C80 C81 C82 N20 178.3(12) . . . . ? N20 C82 C83 C78 -177.3(11) . . . . ? C81 C82 C83 C78 -2.9(18) . . . . ? N20 C82 C83 C84 2.5(18) . . . . ? C81 C82 C83 C84 176.9(12) . . . . ? C79 C78 C83 C82 1.8(16) . . . . ? C77 C78 C83 C82 -179.5(10) . . . . ? C79 C78 C83 C84 -178.1(10) . . . . ? C77 C78 C83 C84 0.6(15) . . . . ? C82 C83 C84 C85 178.3(12) . . . . ? C78 C83 C84 C85 -1.8(18) . . . . ? C83 C84 C85 C86 1.6(19) . . . . ? C78 C77 C86 C85 -1.1(17) . . . . ? S20 C77 C86 C85 -178.5(9) . . . . ? C84 C85 C86 C77 -0.1(18) . . . . ? C45 C46 N4 C51 -23.5(16) . . . . ? C47 C46 N4 C51 155.5(11) . . . . ? C45 C46 N4 C52 111.7(13) . . . . ? C47 C46 N4 C52 -69.3(13) . . . . ? C57 C58 N6 C64 106.3(14) . . . . ? C59 C58 N6 C64 -76.7(13) . . . . ? C57 C58 N6 C63 -19.9(16) . . . . ? C59 C58 N6 C63 157.1(12) . . . . ? C69 C70 N18 C76 7(2) . . . . ? C71 C70 N18 C76 -175.2(12) . . . . ? C69 C70 N18 C75 -99.6(17) . . . . ? C71 C70 N18 C75 78.7(15) . . . . ? C83 C82 N20 C88 -78.5(17) . . . . ? C81 C82 N20 C88 107.2(17) . . . . ? C83 C82 N20 C87 152.0(13) . . . . ? C81 C82 N20 C87 -22.3(19) . . . . ? C5 C4 O4 S4 -85.6(8) . . . . ? C3 C4 O4 S4 103.6(8) . . . . ? C1 C6 O6 S6 -96.6(8) . . . . ? C5 C6 O6 S6 87.5(8) . . . . ? C19 C18 O18 S18 -73.6(9) . . . . ? C17 C18 O18 S18 109.4(8) . . . . ? C15 C20 O20 S20 -96.4(9) . . . . ? C19 C20 O20 S20 85.6(8) . . . . ? C4 O4 S4 O41 134.5(6) . . . . ? C4 O4 S4 O42 5.0(7) . . . . ? C4 O4 S4 C41 -112.0(6) . . . . ? C50 C41 S4 O41 -127.7(7) . . . . ? C42 C41 S4 O41 56.3(8) . . . . ? C50 C41 S4 O42 6.6(8) . . . . ? C42 C41 S4 O42 -169.4(7) . . . . ? C50 C41 S4 O4 121.9(7) . . . . ? C42 C41 S4 O4 -54.1(8) . . . . ? C6 O6 S6 O61 171.7(6) . . . . ? C6 O6 S6 O62 45.9(7) . . . . ? C6 O6 S6 C53 -70.4(7) . . . . ? C62 C53 S6 O61 -126.2(8) . . . . ? C54 C53 S6 O61 51.5(9) . . . . ? C62 C53 S6 O62 5.9(9) . . . . ? C54 C53 S6 O62 -176.5(7) . . . . ? C62 C53 S6 O6 122.1(8) . . . . ? C54 C53 S6 O6 -60.3(8) . . . . ? C18 O18 S18 O181 121.6(7) . . . . ? C18 O18 S18 O182 -6.6(8) . . . . ? C18 O18 S18 C65 -123.3(7) . . . . ? C74 C65 S18 O181 -133.3(9) . . . . ? C66 C65 S18 O181 52.3(9) . . . . ? C74 C65 S18 O182 -1.0(10) . . . . ? C66 C65 S18 O182 -175.4(8) . . . . ? C74 C65 S18 O18 114.9(9) . . . . ? C66 C65 S18 O18 -59.5(9) . . . . ? C20 O20 S20 O202 45.3(7) . . . . ? C20 O20 S20 O201 174.8(6) . . . . ? C20 O20 S20 C77 -69.7(7) . . . . ? C86 C77 S20 O202 2.4(10) . . . . ? C78 C77 S20 O202 -175.0(7) . . . . ? C86 C77 S20 O201 -131.4(8) . . . . ? C78 C77 S20 O201 51.2(9) . . . . ? C86 C77 S20 O20 118.3(8) . . . . ? C78 C77 S20 O20 -59.1(8) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O11 H11 O202 0.84 2.03 2.781(9) 148.1 . O13 H13 O25 0.84 1.97 2.802(9) 170.9 2_566 O25 H25 O62 0.84 2.05 2.798(8) 147.1 . O27 H27 O42 0.84 2.09 2.874(8) 156.0 2_566 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 24.45 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.058 _refine_diff_density_min -0.807 _refine_diff_density_rms 0.117 # SQUEEZE RESULTS #loop_ # _platon_squeeze_void_nr # _platon_squeeze_void_average_x # _platon_squeeze_void_average_y # _platon_squeeze_void_average_z # _platon_squeeze_void_volume # _platon_squeeze_void_count_electrons # 1 0.000 0.000 0.000 650.4 -4.5 # 2 0.500 0.500 0.500 197.9 -4.7 #_platon_squeeze_details #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 606002' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C136 H136 N8 O24 S8, C3 H7 O, 1.5(C2 H3 N)' _chemical_formula_sum 'C142 H147.50 N9.50 O25 S8' _chemical_formula_weight 2636.27 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 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 29.3447(9) _cell_length_b 22.6903(5) _cell_length_c 22.2725(7) _cell_angle_alpha 90.00 _cell_angle_beta 109.0330(10) _cell_angle_gamma 90.00 _cell_volume 14019.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173.0(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5576 _exptl_absorpt_coefficient_mu 0.199 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9519 _exptl_absorpt_correction_T_max 0.9804 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173.0(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 Kappa CCD' _diffrn_measurement_method 'rotation in phi and omega, 1.0 deg.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_reflns_number 22643 _diffrn_reflns_av_R_equivalents 0.1532 _diffrn_reflns_av_sigmaI/netI 0.2011 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 24.50 _reflns_number_total 11601 _reflns_number_gt 5201 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement Denzo-SMN _computing_data_reduction Denzo-SMN _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.1314P)^2^+13.7122P] 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_number_reflns 11601 _refine_ls_number_parameters 852 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.2200 _refine_ls_R_factor_gt 0.0913 _refine_ls_wR_factor_ref 0.2794 _refine_ls_wR_factor_gt 0.2217 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 C1 C 0.0098(2) 0.1647(3) 0.5952(3) 0.0260(17) Uani 1 1 d . . . C2 C 0.0396(2) 0.1587(3) 0.6573(4) 0.0290(17) Uani 1 1 d . . . H2 H 0.0256 0.1474 0.6885 0.035 Uiso 1 1 calc R . . C3 C 0.0895(2) 0.1686(3) 0.6767(3) 0.0234(16) Uani 1 1 d . . . C4 C 0.1074(2) 0.1874(3) 0.6286(4) 0.0269(17) Uani 1 1 d . . . C5 C 0.0796(2) 0.1959(3) 0.5672(4) 0.0306(18) Uani 1 1 d . . . H5 H 0.0930 0.2102 0.5365 0.037 Uiso 1 1 calc R . . C6 C 0.0308(2) 0.1828(3) 0.5509(3) 0.0276(17) Uani 1 1 d . . . C7 C 0.1211(2) 0.1606(3) 0.7453(3) 0.0269(17) Uani 1 1 d . . . H7 H 0.1523 0.1812 0.7503 0.032 Uiso 1 1 calc R . . C8 C 0.0984(2) 0.1906(3) 0.7899(3) 0.0271(17) Uani 1 1 d . . . C9 C 0.0805(2) 0.1589(3) 0.8317(3) 0.0295(17) Uani 1 1 d . . . H9 H 0.0788 0.1172 0.8285 0.035 Uiso 1 1 calc R . . C10 C 0.0651(2) 0.1863(3) 0.8777(3) 0.0250(17) Uani 1 1 d . . . C11 C 0.0671(2) 0.2470(3) 0.8801(3) 0.0272(17) Uani 1 1 d . . . C12 C 0.0806(2) 0.2809(3) 0.8363(3) 0.0255(17) Uani 1 1 d . . . H12 H 0.0792 0.3227 0.8367 0.031 Uiso 1 1 calc R . . C13 C 0.0962(2) 0.2510(3) 0.7924(3) 0.0237(16) Uani 1 1 d . . . C14 C 0.0444(2) 0.1531(3) 0.9230(3) 0.0281(17) Uani 1 1 d . . . H14 H 0.0597 0.1705 0.9661 0.034 Uiso 1 1 calc R . . C29 C 0.1328(2) 0.0947(3) 0.7595(3) 0.0307(18) Uani 1 1 d . . . H29A H 0.1029 0.0741 0.7588 0.037 Uiso 1 1 calc R . . H29B H 0.1432 0.0779 0.7250 0.037 Uiso 1 1 calc R . . C30 C 0.1715(3) 0.0822(3) 0.8224(4) 0.040(2) Uani 1 1 d . . . H30A H 0.2015 0.1029 0.8235 0.048 Uiso 1 1 calc R . . H30B H 0.1611 0.0983 0.8571 0.048 Uiso 1 1 calc R . . C31 C 0.1824(3) 0.0172(3) 0.8344(5) 0.066(3) Uani 1 1 d . . . H31A H 0.1528 -0.0037 0.8330 0.099 Uiso 1 1 calc R . . H31B H 0.2067 0.0119 0.8763 0.099 Uiso 1 1 calc R . . H31C H 0.1946 0.0014 0.8016 0.099 Uiso 1 1 calc R . . C32 C 0.0554(2) 0.0872(3) 0.9288(4) 0.0350(19) Uani 1 1 d . . . H32A H 0.0356 0.0680 0.9517 0.042 Uiso 1 1 calc R . . H32B H 0.0467 0.0696 0.8859 0.042 Uiso 1 1 calc R . . C33 C 0.1084(3) 0.0757(3) 0.9642(4) 0.055(3) Uani 1 1 d . . . H33A H 0.1280 0.0981 0.9433 0.066 Uiso 1 1 calc R . . H33B H 0.1162 0.0908 1.0081 0.066 Uiso 1 1 calc R . . C34 C 0.1226(4) 0.0124(4) 0.9672(6) 0.086(3) Uani 1 1 d . . . H34A H 0.1117 -0.0044 0.9243 0.129 Uiso 1 1 calc R . . H34B H 0.1076 -0.0091 0.9940 0.129 Uiso 1 1 calc R . . H34C H 0.1577 0.0091 0.9851 0.129 Uiso 1 1 calc R . . C41 C 0.2188(2) 0.1165(3) 0.6637(4) 0.0320(18) Uani 1 1 d . . . C42 C 0.2486(3) 0.1233(3) 0.7306(4) 0.0298(19) Uani 1 1 d . . . C43 C 0.2534(2) 0.1778(3) 0.7629(4) 0.0327(19) Uani 1 1 d . . . H43 H 0.2380 0.2124 0.7417 0.039 Uiso 1 1 calc R . . C44 C 0.2810(3) 0.1790(3) 0.8256(4) 0.039(2) Uani 1 1 d . . . H44 H 0.2836 0.2150 0.8483 0.046 Uiso 1 1 calc R . . C45 C 0.3056(2) 0.1296(3) 0.8576(4) 0.0340(19) Uani 1 1 d . . . H45 H 0.3247 0.1326 0.9011 0.041 Uiso 1 1 calc R . . C46 C 0.3023(3) 0.0771(3) 0.8267(4) 0.0344(19) Uani 1 1 d . . . C47 C 0.2711(2) 0.0723(3) 0.7621(4) 0.0295(18) Uani 1 1 d . . . C48 C 0.2624(3) 0.0177(3) 0.7309(4) 0.0351(19) Uani 1 1 d . . . H48 H 0.2772 -0.0167 0.7532 0.042 Uiso 1 1 calc R . . C49 C 0.2336(3) 0.0126(3) 0.6697(4) 0.045(2) Uani 1 1 d . . . H49 H 0.2281 -0.0250 0.6499 0.054 Uiso 1 1 calc R . . C50 C 0.2117(3) 0.0627(3) 0.6354(4) 0.039(2) Uani 1 1 d . . . H50 H 0.1919 0.0591 0.5923 0.046 Uiso 1 1 calc R . . C51 C 0.3686(3) 0.0105(4) 0.8342(5) 0.064(3) Uani 1 1 d . . . H51A H 0.3570 0.0071 0.7878 0.097 Uiso 1 1 calc R . . H51B H 0.3825 -0.0272 0.8529 0.097 Uiso 1 1 calc R . . H51C H 0.3933 0.0413 0.8471 0.097 Uiso 1 1 calc R . . C52 C 0.3428(4) 0.0258(4) 0.9255(4) 0.070(3) Uani 1 1 d . . . H52A H 0.3684 0.0550 0.9424 0.105 Uiso 1 1 calc R . . H52B H 0.3549 -0.0134 0.9414 0.105 Uiso 1 1 calc R . . H52C H 0.3153 0.0357 0.9393 0.105 Uiso 1 1 calc R . . C53 C 0.0496(3) 0.1746(4) 0.4085(4) 0.047(2) Uani 1 1 d . . . C54 C 0.0474(3) 0.2325(4) 0.3807(4) 0.045(2) Uani 1 1 d . . . C55 C 0.0102(3) 0.2742(4) 0.3766(4) 0.047(2) Uani 1 1 d . . . H55 H -0.0159 0.2643 0.3912 0.057 Uiso 1 1 calc R . . C56 C 0.0126(3) 0.3284(4) 0.3516(4) 0.058(2) Uani 1 1 d . . . H56 H -0.0117 0.3565 0.3503 0.069 Uiso 1 1 calc R . . C57 C 0.0483(3) 0.3442(4) 0.3284(4) 0.060(3) Uani 1 1 d . . . H57 H 0.0485 0.3826 0.3116 0.072 Uiso 1 1 calc R . . C58 C 0.0847(3) 0.3045(4) 0.3291(4) 0.059(3) Uani 1 1 d . . . C59 C 0.0857(3) 0.2489(4) 0.3562(4) 0.050(2) Uani 1 1 d . . . C60 C 0.1235(3) 0.2080(5) 0.3643(5) 0.066(3) Uani 1 1 d . . . H60 H 0.1490 0.2185 0.3489 0.079 Uiso 1 1 calc R . . C61 C 0.1257(3) 0.1560(5) 0.3919(4) 0.067(3) Uani 1 1 d . . . H61 H 0.1527 0.1309 0.3973 0.081 Uiso 1 1 calc R . . C62 C 0.0867(3) 0.1381(4) 0.4138(4) 0.056(2) Uani 1 1 d . . . H62 H 0.0872 0.1002 0.4321 0.068 Uiso 1 1 calc R . . C63 C 0.1340(4) 0.3811(6) 0.3057(8) 0.141(6) Uani 1 1 d . . . H63A H 0.1063 0.4020 0.2767 0.212 Uiso 1 1 calc R . . H63B H 0.1622 0.3868 0.2921 0.212 Uiso 1 1 calc R . . H63C H 0.1408 0.3965 0.3488 0.212 Uiso 1 1 calc R . . C64 C 0.1208(4) 0.2893(7) 0.2466(6) 0.130(6) Uani 1 1 d . . . H64A H 0.1034 0.3139 0.2102 0.195 Uiso 1 1 calc R . . H64B H 0.1038 0.2517 0.2443 0.195 Uiso 1 1 calc R . . H64C H 0.1535 0.2819 0.2460 0.195 Uiso 1 1 calc R . . C65 C 0.1311(2) 0.2510(3) 1.0295(3) 0.0315(18) Uani 1 1 d . . . C66 C 0.1683(2) 0.2229(3) 1.0116(3) 0.0283(17) Uani 1 1 d . . . C67 C 0.1795(2) 0.2358(3) 0.9564(3) 0.0317(18) Uani 1 1 d . . . H67 H 0.1638 0.2677 0.9302 0.038 Uiso 1 1 calc R . . C68 C 0.2129(2) 0.2026(3) 0.9394(3) 0.0357(19) Uani 1 1 d . . . H68 H 0.2189 0.2107 0.9008 0.043 Uiso 1 1 calc R . . C69 C 0.2381(3) 0.1568(3) 0.9795(4) 0.038(2) Uani 1 1 d . . . H69 H 0.2603 0.1337 0.9667 0.046 Uiso 1 1 calc R . . C70 C 0.2315(2) 0.1448(3) 1.0359(4) 0.0334(19) Uani 1 1 d . . . C71 C 0.1947(2) 0.1769(3) 1.0533(3) 0.0318(18) Uani 1 1 d . . . C72 C 0.1824(3) 0.1613(3) 1.1069(3) 0.0340(18) Uani 1 1 d . . . H72 H 0.2000 0.1307 1.1336 0.041 Uiso 1 1 calc R . . C73 C 0.1464(3) 0.1882(3) 1.1221(4) 0.0360(19) Uani 1 1 d . . . H73 H 0.1383 0.1759 1.1581 0.043 Uiso 1 1 calc R . . C74 C 0.1215(2) 0.2344(3) 1.0840(3) 0.0314(18) Uani 1 1 d . . . H74 H 0.0975 0.2549 1.0958 0.038 Uiso 1 1 calc R . . C75 C 0.2783(3) 0.0548(3) 1.0493(4) 0.053(2) Uani 1 1 d . . . H75A H 0.2537 0.0397 1.0111 0.080 Uiso 1 1 calc R . . H75B H 0.2900 0.0226 1.0798 0.080 Uiso 1 1 calc R . . H75C H 0.3052 0.0712 1.0378 0.080 Uiso 1 1 calc R . . C76 C 0.2933(3) 0.1245(3) 1.1350(4) 0.046(2) Uani 1 1 d . . . H76A H 0.3218 0.1371 1.1247 0.069 Uiso 1 1 calc R . . H76B H 0.3025 0.0940 1.1679 0.069 Uiso 1 1 calc R . . H76C H 0.2797 0.1584 1.1507 0.069 Uiso 1 1 calc R . . C77 C 0.0944(2) 0.3400(3) 0.6414(4) 0.0277(17) Uani 1 1 d . . . C87 C 0.2388(3) 0.3950(4) 0.5037(5) 0.074(3) Uani 1 1 d . . . H87A H 0.2678 0.3725 0.5264 0.111 Uiso 1 1 calc R . . H87B H 0.2411 0.4346 0.5221 0.111 Uiso 1 1 calc R . . H87C H 0.2359 0.3980 0.4588 0.111 Uiso 1 1 calc R . . C78 C 0.1419(2) 0.3482(3) 0.6392(3) 0.0267(17) Uani 1 1 d . . . C79 C 0.1831(3) 0.3526(3) 0.6934(4) 0.0357(19) Uani 1 1 d . . . H79 H 0.1804 0.3483 0.7346 0.043 Uiso 1 1 calc R . . C80 C 0.2270(3) 0.3632(3) 0.6865(4) 0.043(2) Uani 1 1 d . . . H80 H 0.2545 0.3674 0.7234 0.052 Uiso 1 1 calc R . . C81 C 0.2327(3) 0.3682(3) 0.6266(4) 0.043(2) Uani 1 1 d . . . H81 H 0.2638 0.3753 0.6235 0.051 Uiso 1 1 calc R . . C82 C 0.1942(3) 0.3630(3) 0.5733(4) 0.040(2) Uani 1 1 d . . . C83 C 0.1468(3) 0.3540(3) 0.5779(4) 0.0321(18) Uani 1 1 d . . . C84 C 0.1050(3) 0.3544(3) 0.5244(4) 0.039(2) Uani 1 1 d . . . H84 H 0.1081 0.3599 0.4836 0.047 Uiso 1 1 calc R . . C85 C 0.0600(3) 0.3473(3) 0.5289(4) 0.049(2) Uani 1 1 d . . . H85 H 0.0325 0.3480 0.4917 0.059 Uiso 1 1 calc R . . C86 C 0.0546(3) 0.3391(3) 0.5882(4) 0.041(2) Uani 1 1 d . . . H86 H 0.0235 0.3330 0.5916 0.049 Uiso 1 1 calc R . . C88 C 0.1907(3) 0.3086(4) 0.4782(4) 0.064(3) Uani 1 1 d . . . H88A H 0.2182 0.2833 0.5001 0.096 Uiso 1 1 calc R . . H88B H 0.1892 0.3141 0.4340 0.096 Uiso 1 1 calc R . . H88C H 0.1609 0.2899 0.4794 0.096 Uiso 1 1 calc R . . N4 N 0.3277(2) 0.0260(3) 0.8566(3) 0.0432(17) Uani 1 1 d . . . N6 N 0.1232(3) 0.3194(4) 0.3049(4) 0.084(3) Uani 1 1 d . . . N11 N 0.2572(2) 0.1009(2) 1.0780(3) 0.0363(16) Uani 1 1 d . . . N13 N 0.1963(2) 0.3652(3) 0.5097(3) 0.0475(18) Uani 1 1 d . . . O4 O 0.15714(16) 0.20475(19) 0.6477(2) 0.0331(12) Uani 1 1 d . . . O6 O 0.00070(17) 0.1935(2) 0.4878(2) 0.0379(13) Uani 1 1 d . . . O11 O 0.05417(15) 0.27645(18) 0.9284(2) 0.0282(11) Uani 1 1 d . . . O13 O 0.11146(16) 0.28258(18) 0.7470(2) 0.0306(12) Uani 1 1 d . . . O41 O 0.22979(17) 0.2225(2) 0.6256(3) 0.0486(15) Uani 1 1 d . . . O42 O 0.16854(18) 0.1562(2) 0.5535(2) 0.0477(14) Uani 1 1 d . . . O61 O 0.0161(2) 0.0920(2) 0.4620(3) 0.0578(16) Uani 1 1 d . . . O62 O -0.04228(18) 0.1568(3) 0.3846(3) 0.0567(16) Uani 1 1 d . . . O111 O 0.06738(17) 0.3342(2) 1.0212(2) 0.0396(13) Uani 1 1 d . . . O112 O 0.12334(17) 0.34593(19) 0.9597(2) 0.0397(13) Uani 1 1 d . . . O131 O 0.10336(18) 0.38952(19) 0.7514(2) 0.0407(13) Uani 1 1 d . . . O132 O 0.03162(16) 0.3281(2) 0.7013(2) 0.0444(14) Uani 1 1 d . . . S4 S 0.19428(7) 0.17736(9) 0.61598(10) 0.0384(6) Uani 1 1 d . . . S6 S 0.00299(8) 0.14838(10) 0.43361(11) 0.0468(6) Uani 1 1 d . . . S11 S 0.09482(7) 0.30851(8) 0.98548(9) 0.0328(5) Uani 1 1 d . . . S13 S 0.08143(7) 0.33950(8) 0.71341(9) 0.0333(5) Uani 1 1 d . . . N14 N 0.1315(6) 0.0573(6) 1.1872(8) 0.066(4) Uiso 0.50 1 d P . . C89 C 0.1046(6) 0.0297(7) 1.1480(8) 0.047(4) Uiso 0.50 1 d P . . C90 C 0.0707(6) -0.0078(6) 1.1098(8) 0.047(4) Uiso 0.50 1 d P . . H90A H 0.0501 -0.0229 1.1333 0.070 Uiso 0.50 1 calc PR . . H90B H 0.0869 -0.0408 1.0968 0.070 Uiso 0.50 1 calc PR . . H90C H 0.0509 0.0136 1.0721 0.070 Uiso 0.50 1 calc PR . . C98 C -0.0146(12) -0.0977(12) 0.751(2) 0.063(11) Uiso 0.25 1 d P . . H98A H -0.0475 -0.0998 0.7530 0.094 Uiso 0.25 1 calc PR . . H98B H 0.0075 -0.1171 0.7888 0.094 Uiso 0.25 1 calc PR . . H98C H -0.0133 -0.1176 0.7129 0.094 Uiso 0.25 1 calc PR . . N15 N 0.0000 0.0209(11) 0.7500 0.090(8) Uiso 0.50 2 d SP . . C97 C 0.0000 -0.0333(19) 0.7500 0.130(14) Uiso 0.50 2 d SP . . C91 C 0.0440(11) 0.4644(13) 0.8569(13) 0.138(10) Uiso 0.50 1 d PD . . H91A H 0.0094 0.4585 0.8329 0.166 Uiso 0.50 1 calc PR A 1 H91B H 0.0577 0.4247 0.8704 0.166 Uiso 0.50 1 calc PR A 1 O90 O 0.0667(8) 0.4858(9) 0.8105(11) 0.057(6) Uiso 0.25 1 d PD B 1 C92 C 0.0459(15) 0.4933(16) 0.910(2) 0.067(11) Uiso 0.25 1 d P B 1 H92A H 0.0771 0.4826 0.9418 0.080 Uiso 0.25 1 calc PR B 1 H92B H 0.0481 0.5356 0.9004 0.080 Uiso 0.25 1 calc PR B 1 C93 C 0.0200(12) 0.4903(13) 0.9333(16) 0.047(8) Uiso 0.25 1 d P B 1 H93A H 0.0145 0.5294 0.9482 0.071 Uiso 0.25 1 calc PR B 1 H93B H 0.0317 0.4635 0.9697 0.071 Uiso 0.25 1 calc PR B 1 H93C H -0.0103 0.4750 0.9038 0.071 Uiso 0.25 1 calc PR B 1 O90B O -0.0078(11) 0.5244(12) 0.8034(14) 0.099(9) Uiso 0.25 1 d PD B 2 C91B C 0.0033(14) 0.4919(16) 0.8638(16) 0.074(11) Uiso 0.25 1 d PD B 2 H91C H 0.0111 0.5181 0.9013 0.088 Uiso 0.25 1 calc PR B 2 H91D H -0.0223 0.4636 0.8643 0.088 Uiso 0.25 1 calc PR B 2 C93B C 0.0834(14) 0.4863(16) 0.878(2) 0.071(11) Uiso 0.25 1 d P B 2 H93D H 0.1081 0.4567 0.8795 0.106 Uiso 0.25 1 calc PR B 2 H93E H 0.0881 0.5012 0.9208 0.106 Uiso 0.25 1 calc PR B 2 H93F H 0.0861 0.5190 0.8504 0.106 Uiso 0.25 1 calc PR B 2 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 C1 0.018(4) 0.031(4) 0.028(5) -0.001(3) 0.006(4) 0.008(3) C2 0.023(4) 0.037(4) 0.032(5) -0.002(4) 0.015(4) 0.000(3) C3 0.036(4) 0.022(4) 0.016(4) 0.002(3) 0.013(4) 0.006(3) C4 0.020(4) 0.032(4) 0.033(5) -0.009(4) 0.014(4) 0.000(3) C5 0.027(4) 0.045(4) 0.027(5) 0.003(4) 0.018(4) 0.001(3) C6 0.028(4) 0.038(4) 0.017(5) -0.002(3) 0.009(4) 0.009(3) C7 0.027(4) 0.035(4) 0.023(5) 0.000(3) 0.014(4) 0.005(3) C8 0.028(4) 0.030(4) 0.027(5) -0.004(3) 0.014(4) -0.006(3) C9 0.026(4) 0.032(4) 0.031(5) -0.001(4) 0.010(4) 0.000(3) C10 0.019(4) 0.037(4) 0.021(4) 0.002(3) 0.008(3) -0.004(3) C11 0.020(4) 0.037(5) 0.025(5) -0.007(3) 0.007(4) 0.003(3) C12 0.025(4) 0.029(4) 0.026(5) 0.007(3) 0.013(4) 0.003(3) C13 0.021(4) 0.029(4) 0.023(4) 0.007(3) 0.009(3) 0.001(3) C14 0.027(4) 0.044(4) 0.015(4) 0.006(3) 0.008(3) 0.001(3) C29 0.031(4) 0.035(4) 0.028(5) -0.001(3) 0.011(4) 0.008(3) C30 0.040(5) 0.043(5) 0.044(6) 0.012(4) 0.023(5) 0.022(4) C31 0.069(7) 0.060(6) 0.076(8) 0.019(5) 0.035(6) 0.029(5) C32 0.028(4) 0.040(4) 0.042(5) 0.009(4) 0.016(4) 0.003(4) C33 0.048(6) 0.055(6) 0.071(7) 0.023(5) 0.031(5) 0.011(4) C34 0.078(8) 0.060(6) 0.124(11) 0.023(6) 0.037(7) -0.002(6) C41 0.023(4) 0.047(5) 0.030(5) -0.008(4) 0.015(4) -0.004(4) C42 0.032(4) 0.027(4) 0.041(6) -0.003(4) 0.027(4) -0.002(4) C43 0.020(4) 0.032(4) 0.049(6) 0.000(4) 0.014(4) 0.004(3) C44 0.032(5) 0.041(5) 0.045(6) -0.014(4) 0.016(4) -0.012(4) C45 0.027(4) 0.032(4) 0.045(6) 0.007(4) 0.016(4) 0.005(4) C46 0.029(4) 0.031(5) 0.046(6) 0.004(4) 0.016(4) 0.005(4) C47 0.026(4) 0.031(4) 0.035(5) 0.002(4) 0.015(4) 0.000(3) C48 0.035(5) 0.030(4) 0.042(6) -0.007(4) 0.015(5) 0.002(4) C49 0.046(5) 0.046(5) 0.051(7) -0.023(5) 0.024(5) -0.016(4) C50 0.040(5) 0.039(5) 0.039(6) -0.010(4) 0.015(4) 0.001(4) C51 0.054(6) 0.051(5) 0.093(8) 0.007(5) 0.031(6) 0.011(5) C52 0.098(8) 0.063(6) 0.047(7) 0.010(5) 0.019(6) 0.015(6) C53 0.023(4) 0.082(6) 0.035(6) -0.021(5) 0.009(4) 0.004(4) C54 0.034(5) 0.072(6) 0.028(5) -0.004(4) 0.007(4) 0.005(4) C55 0.031(5) 0.080(6) 0.038(6) -0.008(5) 0.022(4) -0.004(5) C56 0.045(6) 0.086(7) 0.052(6) 0.012(5) 0.030(5) 0.011(5) C57 0.044(5) 0.092(7) 0.044(6) 0.018(5) 0.014(5) -0.002(5) C58 0.045(6) 0.095(7) 0.042(6) 0.010(5) 0.021(5) -0.002(5) C59 0.026(5) 0.090(7) 0.043(6) 0.003(5) 0.023(4) 0.010(5) C60 0.050(6) 0.106(8) 0.051(7) -0.008(6) 0.030(5) 0.000(6) C61 0.033(5) 0.120(9) 0.046(7) -0.004(6) 0.011(5) 0.031(6) C62 0.048(6) 0.077(6) 0.047(6) -0.012(5) 0.020(5) 0.009(5) C63 0.086(9) 0.154(13) 0.218(18) 0.093(12) 0.096(11) 0.021(9) C64 0.083(9) 0.265(17) 0.071(10) 0.003(10) 0.065(8) 0.012(10) C65 0.028(4) 0.038(4) 0.028(5) -0.005(4) 0.008(4) -0.010(3) C66 0.025(4) 0.033(4) 0.027(5) -0.006(4) 0.010(4) -0.008(3) C67 0.029(4) 0.040(4) 0.026(5) 0.004(4) 0.009(4) -0.002(3) C68 0.030(4) 0.060(5) 0.016(5) -0.003(4) 0.006(4) -0.008(4) C69 0.035(5) 0.042(5) 0.044(6) 0.001(4) 0.022(4) 0.006(4) C70 0.026(4) 0.039(4) 0.036(5) -0.002(4) 0.012(4) 0.001(4) C71 0.033(4) 0.035(4) 0.028(5) -0.003(4) 0.010(4) -0.008(4) C72 0.043(5) 0.037(4) 0.024(5) -0.003(4) 0.013(4) -0.004(4) C73 0.041(5) 0.045(5) 0.024(5) 0.001(4) 0.014(4) -0.003(4) C74 0.028(4) 0.039(4) 0.030(5) 0.001(4) 0.013(4) -0.005(4) C75 0.065(6) 0.051(5) 0.048(6) 0.014(4) 0.024(5) 0.023(5) C76 0.043(5) 0.055(5) 0.039(6) 0.008(4) 0.012(5) 0.007(4) C77 0.022(4) 0.032(4) 0.030(5) 0.006(3) 0.009(4) -0.004(3) C87 0.089(8) 0.086(7) 0.075(8) 0.000(6) 0.064(7) -0.027(6) C78 0.027(4) 0.024(4) 0.030(5) 0.004(3) 0.009(4) 0.005(3) C79 0.032(5) 0.036(4) 0.042(6) 0.002(4) 0.017(4) -0.004(4) C80 0.037(5) 0.055(5) 0.036(6) -0.001(4) 0.010(4) -0.005(4) C81 0.032(5) 0.044(5) 0.055(7) 0.005(4) 0.019(5) -0.004(4) C82 0.050(6) 0.037(5) 0.043(6) 0.006(4) 0.029(5) 0.007(4) C83 0.032(5) 0.036(4) 0.029(5) -0.002(4) 0.010(4) -0.003(3) C84 0.044(5) 0.050(5) 0.029(5) 0.007(4) 0.020(5) 0.005(4) C85 0.043(5) 0.062(6) 0.041(6) 0.010(4) 0.013(5) 0.002(4) C86 0.038(5) 0.047(5) 0.048(6) 0.006(4) 0.029(5) -0.010(4) C88 0.081(7) 0.081(7) 0.043(6) -0.008(5) 0.037(6) 0.006(6) N4 0.043(4) 0.039(4) 0.051(5) 0.003(3) 0.021(4) 0.005(3) N6 0.060(5) 0.135(8) 0.073(7) 0.033(6) 0.044(5) 0.003(5) N11 0.035(4) 0.036(4) 0.036(4) 0.001(3) 0.008(3) 0.006(3) N13 0.052(4) 0.056(4) 0.044(5) 0.008(4) 0.028(4) 0.005(4) O4 0.027(3) 0.041(3) 0.036(3) -0.002(2) 0.017(3) -0.004(2) O6 0.033(3) 0.056(3) 0.028(3) 0.001(3) 0.016(3) 0.008(2) O11 0.026(3) 0.036(3) 0.022(3) -0.004(2) 0.009(2) -0.001(2) O13 0.034(3) 0.036(3) 0.028(3) 0.012(2) 0.018(3) 0.008(2) O41 0.034(3) 0.054(3) 0.066(4) 0.016(3) 0.028(3) -0.001(3) O42 0.038(3) 0.081(4) 0.028(4) -0.005(3) 0.017(3) 0.014(3) O61 0.073(4) 0.050(4) 0.055(4) -0.010(3) 0.026(3) 0.002(3) O62 0.030(3) 0.101(5) 0.034(4) -0.010(3) 0.003(3) -0.008(3) O111 0.045(3) 0.046(3) 0.034(3) -0.007(3) 0.020(3) 0.007(2) O112 0.043(3) 0.036(3) 0.044(4) 0.001(2) 0.019(3) -0.006(2) O131 0.055(3) 0.032(3) 0.041(4) -0.007(3) 0.023(3) -0.005(3) O132 0.027(3) 0.066(3) 0.046(4) 0.015(3) 0.020(3) 0.004(3) S4 0.0313(11) 0.0547(13) 0.0369(14) 0.0020(10) 0.0217(11) 0.0038(10) S6 0.0431(13) 0.0660(16) 0.0361(14) -0.0107(12) 0.0196(12) 0.0002(11) S11 0.0318(11) 0.0359(11) 0.0316(13) -0.0034(9) 0.0117(10) 0.0004(9) S13 0.0347(12) 0.0387(11) 0.0313(13) 0.0070(10) 0.0174(10) 0.0047(9) _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 C1 C2 1.381(9) . ? C1 C6 1.388(9) . ? C1 C14 1.531(9) 2_556 ? C2 C3 1.402(9) . ? C3 C4 1.405(9) . ? C3 C7 1.517(9) . ? C4 C5 1.359(9) . ? C4 O4 1.437(7) . ? C5 C6 1.389(9) . ? C6 O6 1.415(8) . ? C7 C8 1.526(8) . ? C7 C29 1.544(9) . ? C8 C13 1.373(8) . ? C8 C9 1.409(9) . ? C9 C10 1.392(9) . ? C10 C11 1.378(9) . ? C10 C14 1.534(8) . ? C11 C12 1.396(9) . ? C11 O11 1.420(7) . ? C12 C13 1.386(8) . ? C13 O13 1.425(7) . ? C14 C32 1.527(9) . ? C14 C1 1.531(9) 2_556 ? C29 C30 1.516(10) . ? C30 C31 1.512(10) . ? C32 C33 1.519(10) . ? C33 C34 1.489(10) . ? C41 C50 1.357(9) . ? C41 C42 1.469(10) . ? C41 S4 1.749(8) . ? C42 C47 1.403(10) . ? C42 C43 1.413(9) . ? C43 C44 1.368(10) . ? C44 C45 1.396(10) . ? C45 C46 1.364(10) . ? C46 N4 1.421(9) . ? C46 C47 1.436(10) . ? C47 C48 1.403(9) . ? C48 C49 1.354(11) . ? C49 C50 1.402(11) . ? C51 N4 1.485(9) . ? C52 N4 1.451(10) . ? C53 C62 1.340(10) . ? C53 C54 1.445(11) . ? C53 S6 1.744(8) . ? C54 C55 1.425(10) . ? C54 C59 1.448(10) . ? C55 C56 1.363(11) . ? C56 C57 1.357(10) . ? C57 C58 1.392(12) . ? C58 C59 1.395(11) . ? C58 N6 1.442(10) . ? C59 C60 1.413(12) . ? C60 C61 1.320(12) . ? C61 C62 1.442(12) . ? C63 N6 1.432(14) . ? C64 N6 1.449(13) . ? C65 C74 1.385(9) . ? C65 C66 1.428(9) . ? C65 S11 1.766(7) . ? C66 C67 1.403(9) . ? C66 C71 1.443(10) . ? C67 C68 1.382(9) . ? C68 C69 1.413(10) . ? C69 C70 1.359(10) . ? C70 N11 1.408(9) . ? C70 C71 1.457(9) . ? C71 C72 1.399(9) . ? C72 C73 1.356(9) . ? C73 C74 1.395(10) . ? C75 N11 1.463(9) . ? C76 N11 1.463(9) . ? C77 C86 1.365(10) . ? C77 C78 1.423(9) . ? C77 S13 1.765(7) . ? C87 N13 1.462(9) . ? C78 C79 1.405(10) . ? C78 C83 1.425(9) . ? C79 C80 1.368(9) . ? C80 C81 1.403(10) . ? C81 C82 1.351(11) . ? C82 N13 1.440(9) . ? C82 C83 1.443(10) . ? C83 C84 1.405(10) . ? C84 C85 1.365(10) . ? C85 C86 1.393(10) . ? C88 N13 1.446(10) . ? O4 S4 1.604(4) . ? O6 S6 1.602(5) . ? O11 S11 1.606(5) . ? O13 S13 1.604(5) . ? O41 S4 1.426(5) . ? O42 S4 1.432(5) . ? O61 S6 1.424(6) . ? O62 S6 1.431(6) . ? O111 S11 1.428(4) . ? O112 S11 1.437(5) . ? O131 S13 1.436(5) . ? O132 S13 1.421(5) . ? N14 C89 1.153(19) . ? C89 C90 1.37(2) . ? C98 C97 1.52(4) . ? N15 C97 1.23(4) . ? C97 C98 1.52(4) 2_556 ? C91 C93B 1.20(4) . ? C91 C92 1.34(4) . ? C91 C91B 1.40(4) . ? C91 O90 1.481(10) . ? C92 C93 1.06(4) . ? O90B C91B 1.476(10) . ? 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 C2 C1 C6 117.2(6) . . ? C2 C1 C14 120.9(6) . 2_556 ? C6 C1 C14 121.9(6) . 2_556 ? C1 C2 C3 123.4(6) . . ? C2 C3 C4 115.2(6) . . ? C2 C3 C7 121.8(6) . . ? C4 C3 C7 123.0(6) . . ? C5 C4 C3 124.1(6) . . ? C5 C4 O4 118.4(6) . . ? C3 C4 O4 117.1(6) . . ? C4 C5 C6 117.4(6) . . ? C1 C6 C5 122.5(7) . . ? C1 C6 O6 118.5(6) . . ? C5 C6 O6 118.7(6) . . ? C3 C7 C8 110.4(5) . . ? C3 C7 C29 110.1(5) . . ? C8 C7 C29 114.5(5) . . ? C13 C8 C9 116.8(6) . . ? C13 C8 C7 120.5(6) . . ? C9 C8 C7 122.7(6) . . ? C10 C9 C8 122.6(6) . . ? C11 C10 C9 117.1(6) . . ? C11 C10 C14 119.1(6) . . ? C9 C10 C14 123.8(6) . . ? C10 C11 C12 122.7(6) . . ? C10 C11 O11 118.8(6) . . ? C12 C11 O11 118.5(6) . . ? C13 C12 C11 117.3(6) . . ? C8 C13 C12 123.2(6) . . ? C8 C13 O13 116.4(5) . . ? C12 C13 O13 120.5(5) . . ? C32 C14 C1 111.3(5) . 2_556 ? C32 C14 C10 114.8(5) . . ? C1 C14 C10 110.0(5) 2_556 . ? C30 C29 C7 114.9(6) . . ? C31 C30 C29 113.4(7) . . ? C33 C32 C14 111.4(6) . . ? C34 C33 C32 114.3(8) . . ? C50 C41 C42 121.1(7) . . ? C50 C41 S4 117.2(6) . . ? C42 C41 S4 121.6(5) . . ? C47 C42 C43 121.0(7) . . ? C47 C42 C41 116.6(6) . . ? C43 C42 C41 122.4(7) . . ? C44 C43 C42 117.7(7) . . ? C43 C44 C45 122.7(7) . . ? C46 C45 C44 120.3(8) . . ? C45 C46 N4 122.5(7) . . ? C45 C46 C47 119.3(7) . . ? N4 C46 C47 118.2(6) . . ? C48 C47 C42 120.1(7) . . ? C48 C47 C46 121.2(7) . . ? C42 C47 C46 118.7(7) . . ? C49 C48 C47 121.7(7) . . ? C48 C49 C50 120.3(7) . . ? C41 C50 C49 120.1(8) . . ? C62 C53 C54 121.4(7) . . ? C62 C53 S6 117.4(7) . . ? C54 C53 S6 121.1(6) . . ? C55 C54 C53 123.9(7) . . ? C55 C54 C59 118.6(8) . . ? C53 C54 C59 117.5(7) . . ? C56 C55 C54 119.0(7) . . ? C57 C56 C55 122.9(8) . . ? C56 C57 C58 120.6(9) . . ? C57 C58 C59 119.9(7) . . ? C57 C58 N6 122.3(9) . . ? C59 C58 N6 117.8(8) . . ? C58 C59 C60 123.7(8) . . ? C58 C59 C54 119.0(7) . . ? C60 C59 C54 117.2(8) . . ? C61 C60 C59 124.3(8) . . ? C60 C61 C62 119.0(8) . . ? C53 C62 C61 120.5(9) . . ? C74 C65 C66 121.1(7) . . ? C74 C65 S11 115.4(5) . . ? C66 C65 S11 123.4(5) . . ? C67 C66 C65 124.8(7) . . ? C67 C66 C71 119.0(6) . . ? C65 C66 C71 116.1(6) . . ? C68 C67 C66 121.0(7) . . ? C67 C68 C69 120.0(7) . . ? C70 C69 C68 121.8(6) . . ? C69 C70 N11 123.4(6) . . ? C69 C70 C71 119.2(7) . . ? N11 C70 C71 117.4(6) . . ? C72 C71 C66 119.9(6) . . ? C72 C71 C70 121.3(7) . . ? C66 C71 C70 118.6(6) . . ? C73 C72 C71 122.5(7) . . ? C72 C73 C74 118.8(7) . . ? C65 C74 C73 121.4(6) . . ? C86 C77 C78 122.9(6) . . ? C86 C77 S13 114.3(5) . . ? C78 C77 S13 122.3(6) . . ? C79 C78 C77 123.9(6) . . ? C79 C78 C83 119.3(6) . . ? C77 C78 C83 116.7(7) . . ? C80 C79 C78 119.6(7) . . ? C79 C80 C81 122.0(8) . . ? C82 C81 C80 120.2(7) . . ? C81 C82 N13 124.7(7) . . ? C81 C82 C83 120.0(7) . . ? N13 C82 C83 115.3(8) . . ? C84 C83 C78 118.8(6) . . ? C84 C83 C82 122.3(7) . . ? C78 C83 C82 118.8(7) . . ? C85 C84 C83 122.3(7) . . ? C84 C85 C86 119.8(8) . . ? C77 C86 C85 119.4(7) . . ? C46 N4 C52 115.5(6) . . ? C46 N4 C51 113.2(6) . . ? C52 N4 C51 110.7(7) . . ? C63 N6 C58 115.0(9) . . ? C63 N6 C64 114.7(10) . . ? C58 N6 C64 114.1(9) . . ? C70 N11 C75 115.2(6) . . ? C70 N11 C76 113.4(6) . . ? C75 N11 C76 110.7(6) . . ? C82 N13 C88 114.3(6) . . ? C82 N13 C87 114.6(7) . . ? C88 N13 C87 109.5(6) . . ? C4 O4 S4 122.4(4) . . ? C6 O6 S6 118.1(4) . . ? C11 O11 S11 120.0(4) . . ? C13 O13 S13 118.9(4) . . ? O41 S4 O42 120.9(3) . . ? O41 S4 O4 103.0(3) . . ? O42 S4 O4 109.8(3) . . ? O41 S4 C41 109.9(3) . . ? O42 S4 C41 108.0(3) . . ? O4 S4 C41 104.1(3) . . ? O61 S6 O62 120.5(4) . . ? O61 S6 O6 108.2(3) . . ? O62 S6 O6 103.5(3) . . ? O61 S6 C53 108.8(4) . . ? O62 S6 C53 109.9(4) . . ? O6 S6 C53 104.8(3) . . ? O111 S11 O112 119.3(3) . . ? O111 S11 O11 102.6(3) . . ? O112 S11 O11 109.3(3) . . ? O111 S11 C65 109.8(3) . . ? O112 S11 C65 109.6(3) . . ? O11 S11 C65 105.2(3) . . ? O132 S13 O131 119.4(3) . . ? O132 S13 O13 108.5(3) . . ? O131 S13 O13 106.8(3) . . ? O132 S13 C77 110.0(3) . . ? O131 S13 C77 110.0(3) . . ? O13 S13 C77 100.4(3) . . ? N14 C89 C90 170.1(18) . . ? N15 C97 C98 163.2(12) . . ? N15 C97 C98 163.2(12) . 2_556 ? C93B C91 C92 72(3) . . ? C93B C91 C91B 121(3) . . ? C92 C91 C91B 58(2) . . ? C93B C91 O90 63(2) . . ? C92 C91 O90 124(3) . . ? C91B C91 O90 122(3) . . ? C93 C92 C91 125(4) . . ? C91 C91B O90B 94(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.7(10) . . . . ? C14 C1 C2 C3 179.9(6) 2_556 . . . ? C1 C2 C3 C4 2.4(9) . . . . ? C1 C2 C3 C7 -179.0(6) . . . . ? C2 C3 C4 C5 -0.2(9) . . . . ? C7 C3 C4 C5 -178.8(6) . . . . ? C2 C3 C4 O4 172.8(5) . . . . ? C7 C3 C4 O4 -5.8(8) . . . . ? C3 C4 C5 C6 -2.6(10) . . . . ? O4 C4 C5 C6 -175.5(5) . . . . ? C2 C1 C6 C5 -1.3(10) . . . . ? C14 C1 C6 C5 177.1(6) 2_556 . . . ? C2 C1 C6 O6 -175.4(6) . . . . ? C14 C1 C6 O6 3.1(9) 2_556 . . . ? C4 C5 C6 C1 3.4(10) . . . . ? C4 C5 C6 O6 177.4(6) . . . . ? C2 C3 C7 C8 -46.9(8) . . . . ? C4 C3 C7 C8 131.7(6) . . . . ? C2 C3 C7 C29 80.5(7) . . . . ? C4 C3 C7 C29 -101.0(7) . . . . ? C3 C7 C8 C13 -70.0(8) . . . . ? C29 C7 C8 C13 165.1(6) . . . . ? C3 C7 C8 C9 112.4(7) . . . . ? C29 C7 C8 C9 -12.5(10) . . . . ? C13 C8 C9 C10 -5.7(10) . . . . ? C7 C8 C9 C10 172.1(6) . . . . ? C8 C9 C10 C11 1.3(10) . . . . ? C8 C9 C10 C14 178.7(6) . . . . ? C9 C10 C11 C12 4.4(10) . . . . ? C14 C10 C11 C12 -173.1(6) . . . . ? C9 C10 C11 O11 -176.8(6) . . . . ? C14 C10 C11 O11 5.8(9) . . . . ? C10 C11 C12 C13 -5.4(10) . . . . ? O11 C11 C12 C13 175.8(6) . . . . ? C9 C8 C13 C12 4.6(10) . . . . ? C7 C8 C13 C12 -173.2(6) . . . . ? C9 C8 C13 O13 -176.0(6) . . . . ? C7 C8 C13 O13 6.2(9) . . . . ? C11 C12 C13 C8 0.6(10) . . . . ? C11 C12 C13 O13 -178.7(6) . . . . ? C11 C10 C14 C32 -164.9(6) . . . . ? C9 C10 C14 C32 17.8(10) . . . . ? C11 C10 C14 C1 68.7(8) . . . 2_556 ? C9 C10 C14 C1 -108.6(7) . . . 2_556 ? C3 C7 C29 C30 169.2(5) . . . . ? C8 C7 C29 C30 -65.8(8) . . . . ? C7 C29 C30 C31 -179.4(6) . . . . ? C1 C14 C32 C33 -164.0(6) 2_556 . . . ? C10 C14 C32 C33 70.3(8) . . . . ? C14 C32 C33 C34 -175.3(7) . . . . ? C50 C41 C42 C47 3.5(9) . . . . ? S4 C41 C42 C47 -172.5(5) . . . . ? C50 C41 C42 C43 -174.7(6) . . . . ? S4 C41 C42 C43 9.3(8) . . . . ? C47 C42 C43 C44 0.3(9) . . . . ? C41 C42 C43 C44 178.4(6) . . . . ? C42 C43 C44 C45 2.5(10) . . . . ? C43 C44 C45 C46 -0.8(10) . . . . ? C44 C45 C46 N4 178.1(6) . . . . ? C44 C45 C46 C47 -3.6(10) . . . . ? C43 C42 C47 C48 174.4(6) . . . . ? C41 C42 C47 C48 -3.8(9) . . . . ? C43 C42 C47 C46 -4.6(9) . . . . ? C41 C42 C47 C46 177.2(5) . . . . ? C45 C46 C47 C48 -172.7(6) . . . . ? N4 C46 C47 C48 5.5(9) . . . . ? C45 C46 C47 C42 6.3(9) . . . . ? N4 C46 C47 C42 -175.4(6) . . . . ? C42 C47 C48 C49 1.9(10) . . . . ? C46 C47 C48 C49 -179.1(6) . . . . ? C47 C48 C49 C50 0.6(11) . . . . ? C42 C41 C50 C49 -1.2(10) . . . . ? S4 C41 C50 C49 175.0(5) . . . . ? C48 C49 C50 C41 -1.0(10) . . . . ? C62 C53 C54 C55 -176.8(8) . . . . ? S6 C53 C54 C55 5.7(11) . . . . ? C62 C53 C54 C59 2.6(12) . . . . ? S6 C53 C54 C59 -174.9(6) . . . . ? C53 C54 C55 C56 177.5(8) . . . . ? C59 C54 C55 C56 -1.8(12) . . . . ? C54 C55 C56 C57 2.0(14) . . . . ? C55 C56 C57 C58 0.2(15) . . . . ? C56 C57 C58 C59 -2.6(14) . . . . ? C56 C57 C58 N6 180.0(9) . . . . ? C57 C58 C59 C60 -173.9(9) . . . . ? N6 C58 C59 C60 3.6(14) . . . . ? C57 C58 C59 C54 2.7(13) . . . . ? N6 C58 C59 C54 -179.8(8) . . . . ? C55 C54 C59 C58 -0.5(12) . . . . ? C53 C54 C59 C58 -179.9(8) . . . . ? C55 C54 C59 C60 176.3(8) . . . . ? C53 C54 C59 C60 -3.1(12) . . . . ? C58 C59 C60 C61 177.5(10) . . . . ? C54 C59 C60 C61 0.8(15) . . . . ? C59 C60 C61 C62 2.1(15) . . . . ? C54 C53 C62 C61 0.2(13) . . . . ? S6 C53 C62 C61 177.8(7) . . . . ? C60 C61 C62 C53 -2.6(14) . . . . ? C74 C65 C66 C67 178.1(7) . . . . ? S11 C65 C66 C67 -2.4(10) . . . . ? C74 C65 C66 C71 0.1(9) . . . . ? S11 C65 C66 C71 179.6(5) . . . . ? C65 C66 C67 C68 -173.6(6) . . . . ? C71 C66 C67 C68 4.3(10) . . . . ? C66 C67 C68 C69 -3.1(11) . . . . ? C67 C68 C69 C70 -1.7(11) . . . . ? C68 C69 C70 N11 -177.6(7) . . . . ? C68 C69 C70 C71 4.9(11) . . . . ? C67 C66 C71 C72 -176.6(6) . . . . ? C65 C66 C71 C72 1.5(10) . . . . ? C67 C66 C71 C70 -1.1(10) . . . . ? C65 C66 C71 C70 177.1(6) . . . . ? C69 C70 C71 C72 172.0(7) . . . . ? N11 C70 C71 C72 -5.5(10) . . . . ? C69 C70 C71 C66 -3.5(10) . . . . ? N11 C70 C71 C66 178.9(6) . . . . ? C66 C71 C72 C73 -0.6(11) . . . . ? C70 C71 C72 C73 -176.1(7) . . . . ? C71 C72 C73 C74 -1.9(11) . . . . ? C66 C65 C74 C73 -2.6(10) . . . . ? S11 C65 C74 C73 177.9(6) . . . . ? C72 C73 C74 C65 3.5(11) . . . . ? C86 C77 C78 C79 176.2(7) . . . . ? S13 C77 C78 C79 4.5(9) . . . . ? C86 C77 C78 C83 -1.8(10) . . . . ? S13 C77 C78 C83 -173.5(5) . . . . ? C77 C78 C79 C80 -177.0(6) . . . . ? C83 C78 C79 C80 1.0(10) . . . . ? C78 C79 C80 C81 -2.0(11) . . . . ? C79 C80 C81 C82 0.5(11) . . . . ? C80 C81 C82 N13 -177.6(6) . . . . ? C80 C81 C82 C83 1.9(11) . . . . ? C79 C78 C83 C84 -174.8(6) . . . . ? C77 C78 C83 C84 3.4(9) . . . . ? C79 C78 C83 C82 1.3(9) . . . . ? C77 C78 C83 C82 179.4(6) . . . . ? C81 C82 C83 C84 173.2(7) . . . . ? N13 C82 C83 C84 -7.3(10) . . . . ? C81 C82 C83 C78 -2.7(10) . . . . ? N13 C82 C83 C78 176.8(6) . . . . ? C78 C83 C84 C85 -2.5(11) . . . . ? C82 C83 C84 C85 -178.4(7) . . . . ? C83 C84 C85 C86 -0.1(11) . . . . ? C78 C77 C86 C85 -0.8(11) . . . . ? S13 C77 C86 C85 171.5(5) . . . . ? C84 C85 C86 C77 1.8(11) . . . . ? C45 C46 N4 C52 21.6(10) . . . . ? C47 C46 N4 C52 -156.6(7) . . . . ? C45 C46 N4 C51 -107.6(8) . . . . ? C47 C46 N4 C51 74.2(8) . . . . ? C57 C58 N6 C63 25.5(14) . . . . ? C59 C58 N6 C63 -151.9(10) . . . . ? C57 C58 N6 C64 -110.0(11) . . . . ? C59 C58 N6 C64 72.5(12) . . . . ? C69 C70 N11 C75 -21.6(10) . . . . ? C71 C70 N11 C75 155.9(6) . . . . ? C69 C70 N11 C76 107.4(8) . . . . ? C71 C70 N11 C76 -75.2(8) . . . . ? C81 C82 N13 C88 105.5(9) . . . . ? C83 C82 N13 C88 -74.0(8) . . . . ? C81 C82 N13 C87 -22.1(10) . . . . ? C83 C82 N13 C87 158.4(7) . . . . ? C5 C4 O4 S4 -59.8(7) . . . . ? C3 C4 O4 S4 126.8(5) . . . . ? C1 C6 O6 S6 -109.6(6) . . . . ? C5 C6 O6 S6 76.1(7) . . . . ? C10 C11 O11 S11 109.6(6) . . . . ? C12 C11 O11 S11 -71.5(7) . . . . ? C8 C13 O13 S13 139.4(5) . . . . ? C12 C13 O13 S13 -41.2(8) . . . . ? C4 O4 S4 O41 154.6(5) . . . . ? C4 O4 S4 O42 24.6(6) . . . . ? C4 O4 S4 C41 -90.7(5) . . . . ? C50 C41 S4 O41 -131.4(5) . . . . ? C42 C41 S4 O41 44.8(6) . . . . ? C50 C41 S4 O42 2.3(6) . . . . ? C42 C41 S4 O42 178.5(5) . . . . ? C50 C41 S4 O4 118.9(5) . . . . ? C42 C41 S4 O4 -64.9(5) . . . . ? C6 O6 S6 O61 29.0(5) . . . . ? C6 O6 S6 O62 157.9(5) . . . . ? C6 O6 S6 C53 -87.0(5) . . . . ? C62 C53 S6 O61 5.6(8) . . . . ? C54 C53 S6 O61 -176.8(6) . . . . ? C62 C53 S6 O62 -128.3(7) . . . . ? C54 C53 S6 O62 49.3(7) . . . . ? C62 C53 S6 O6 121.1(6) . . . . ? C54 C53 S6 O6 -61.3(7) . . . . ? C11 O11 S11 O111 177.6(5) . . . . ? C11 O11 S11 O112 50.1(5) . . . . ? C11 O11 S11 C65 -67.5(5) . . . . ? C74 C65 S11 O111 10.0(6) . . . . ? C66 C65 S11 O111 -169.5(5) . . . . ? C74 C65 S11 O112 142.9(5) . . . . ? C66 C65 S11 O112 -36.6(7) . . . . ? C74 C65 S11 O11 -99.8(5) . . . . ? C66 C65 S11 O11 80.7(6) . . . . ? C13 O13 S13 O132 -38.2(5) . . . . ? C13 O13 S13 O131 91.7(5) . . . . ? C13 O13 S13 C77 -153.6(5) . . . . ? C86 C77 S13 O132 9.9(6) . . . . ? C78 C77 S13 O132 -177.7(5) . . . . ? C86 C77 S13 O131 -123.6(6) . . . . ? C78 C77 S13 O131 48.8(6) . . . . ? C86 C77 S13 O13 124.1(5) . . . . ? C78 C77 S13 O13 -63.5(6) . . . . ? C93B C91 C92 C93 -169(5) . . . . ? C91B C91 C92 C93 44(4) . . . . ? O90 C91 C92 C93 153(4) . . . . ? C93B C91 C91B O90B 91(4) . . . . ? C92 C91 C91B O90B 128(4) . . . . ? O90 C91 C91B O90B 16(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.725 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.090 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 606003' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H17 N O3 S' _chemical_formula_sum 'C18 H17 N O3 S' _chemical_formula_weight 327.39 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 monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.2180(4) _cell_length_b 11.3823(4) _cell_length_c 17.5254(9) _cell_angle_alpha 90.00 _cell_angle_beta 101.113(2) _cell_angle_gamma 90.00 _cell_volume 1608.58(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173.0(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 0.216 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Dx = 35 mm, 1,5 deg., 20 s./deg. ; _diffrn_ambient_temperature 173(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 Kappa CCD' _diffrn_measurement_method 'rotation in phi and omega, 1.5 deg.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5830 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0468 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3141 _reflns_number_gt 2330 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0404P)^2^+0.3303P] 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_number_reflns 3141 _refine_ls_number_parameters 210 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0654 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.0918 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.11614(6) 0.83899(4) 0.42658(3) 0.02664(14) Uani 1 1 d . . . O1 O 0.04433(15) 0.71100(10) 0.43655(7) 0.0290(3) Uani 1 1 d . . . O2 O 0.14336(16) 0.89817(11) 0.49944(7) 0.0346(3) Uani 1 1 d . . . O3 O 0.00222(16) 0.88582(11) 0.36220(8) 0.0366(3) Uani 1 1 d . . . C1 C 0.3086(2) 0.81435(14) 0.39935(10) 0.0217(4) Uani 1 1 d . . . C2 C 0.4438(2) 0.86275(14) 0.44669(10) 0.0247(4) Uani 1 1 d . . . H2 H 0.4317 0.8997 0.4939 0.030 Uiso 1 1 calc R . . C3 C 0.6004(2) 0.85818(15) 0.42588(10) 0.0261(4) Uani 1 1 d . . . H3 H 0.6948 0.8896 0.4595 0.031 Uiso 1 1 calc R . . C4 C 0.6155(2) 0.80809(15) 0.35679(10) 0.0256(4) Uani 1 1 d . . . H4 H 0.7210 0.8075 0.3422 0.031 Uiso 1 1 calc R . . C5 C 0.4785(2) 0.75699(14) 0.30638(10) 0.0229(4) Uani 1 1 d . . . C6 C 0.4980(2) 0.70126(15) 0.23507(10) 0.0261(4) Uani 1 1 d . . . C7 C 0.3691(2) 0.63781(15) 0.19379(11) 0.0326(5) Uani 1 1 d . . . H7 H 0.3833 0.5972 0.1482 0.039 Uiso 1 1 calc R . . C8 C 0.2158(3) 0.63195(16) 0.21803(11) 0.0338(5) Uani 1 1 d . . . H8 H 0.1294 0.5855 0.1891 0.041 Uiso 1 1 calc R . . C9 C 0.1878(2) 0.69120(15) 0.28198(10) 0.0286(4) Uani 1 1 d . . . H9 H 0.0813 0.6897 0.2954 0.034 Uiso 1 1 calc R . . C13 C 0.1239(2) 0.64098(15) 0.50025(10) 0.0267(4) Uani 1 1 d . . . N1 N 0.6558(2) 0.71022(13) 0.21377(9) 0.0324(4) Uani 1 1 d . . . C10 C 0.3199(2) 0.75531(14) 0.32844(10) 0.0226(4) Uani 1 1 d . . . C11 C 0.6935(3) 0.82707(19) 0.18648(13) 0.0469(6) Uani 1 1 d . . . H11A H 0.8138 0.8357 0.1917 0.070 Uiso 1 1 calc R . . H11B H 0.6518 0.8873 0.2178 0.070 Uiso 1 1 calc R . . H11C H 0.6401 0.8363 0.1318 0.070 Uiso 1 1 calc R . . C12 C 0.6977(3) 0.61783(19) 0.16407(12) 0.0471(6) Uani 1 1 d . . . H12A H 0.8165 0.6212 0.1632 0.071 Uiso 1 1 calc R . . H12B H 0.6340 0.6284 0.1112 0.071 Uiso 1 1 calc R . . H12C H 0.6710 0.5413 0.1842 0.071 Uiso 1 1 calc R . . C14 C 0.2332(2) 0.55625(16) 0.48676(12) 0.0361(5) Uani 1 1 d . . . H14 H 0.2608 0.5478 0.4368 0.043 Uiso 1 1 calc R . . C15 C 0.3025(3) 0.48342(18) 0.54740(13) 0.0462(6) Uani 1 1 d . . . H15 H 0.3795 0.4246 0.5395 0.055 Uiso 1 1 calc R . . C16 C 0.2603(3) 0.49565(17) 0.61942(12) 0.0432(5) Uani 1 1 d . . . H16 H 0.3067 0.4444 0.6607 0.052 Uiso 1 1 calc R . . C17 C 0.1512(3) 0.58199(17) 0.63159(12) 0.0445(5) Uani 1 1 d . . . H17 H 0.1236 0.5909 0.6815 0.053 Uiso 1 1 calc R . . C18 C 0.0816(3) 0.65588(17) 0.57163(11) 0.0377(5) Uani 1 1 d . . . H18 H 0.0060 0.7157 0.5796 0.045 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 0.0212(3) 0.0224(2) 0.0356(3) 0.0032(2) 0.0037(2) 0.00082(19) O1 0.0244(7) 0.0274(7) 0.0335(7) 0.0059(6) 0.0016(6) -0.0047(5) O2 0.0338(8) 0.0296(7) 0.0425(8) -0.0063(6) 0.0124(6) 0.0021(6) O3 0.0244(7) 0.0340(7) 0.0484(8) 0.0136(6) -0.0006(6) 0.0047(6) C1 0.0221(10) 0.0165(8) 0.0256(9) 0.0027(7) 0.0020(8) -0.0004(7) C2 0.0269(10) 0.0211(9) 0.0250(9) -0.0021(7) 0.0024(8) -0.0004(7) C3 0.0213(10) 0.0269(9) 0.0273(9) -0.0054(8) -0.0022(8) -0.0034(8) C4 0.0207(10) 0.0254(9) 0.0298(10) -0.0014(8) 0.0026(8) -0.0006(8) C5 0.0248(10) 0.0176(8) 0.0247(9) 0.0019(7) 0.0007(8) 0.0005(7) C6 0.0311(11) 0.0212(9) 0.0241(9) 0.0008(8) 0.0008(8) 0.0038(8) C7 0.0407(13) 0.0277(10) 0.0257(10) -0.0065(8) -0.0023(9) 0.0016(9) C8 0.0339(12) 0.0294(10) 0.0326(11) -0.0046(9) -0.0070(9) -0.0085(8) C9 0.0249(10) 0.0270(9) 0.0308(10) -0.0002(8) -0.0021(8) -0.0051(8) C13 0.0232(10) 0.0224(9) 0.0324(10) 0.0047(8) 0.0005(8) -0.0040(8) N1 0.0343(10) 0.0360(9) 0.0279(8) -0.0062(7) 0.0087(7) 0.0016(7) C10 0.0239(10) 0.0163(8) 0.0253(9) 0.0035(7) -0.0012(8) -0.0002(7) C11 0.0486(14) 0.0490(13) 0.0476(13) 0.0034(11) 0.0204(11) -0.0037(11) C12 0.0468(14) 0.0580(14) 0.0358(12) -0.0167(10) 0.0064(10) 0.0101(11) C14 0.0413(13) 0.0302(10) 0.0392(11) 0.0036(9) 0.0141(10) 0.0028(9) C15 0.0482(14) 0.0332(11) 0.0589(14) 0.0101(11) 0.0142(11) 0.0134(10) C16 0.0547(15) 0.0297(11) 0.0401(12) 0.0095(10) -0.0034(11) 0.0017(10) C17 0.0640(16) 0.0371(12) 0.0324(11) 0.0020(10) 0.0091(10) 0.0022(11) C18 0.0459(13) 0.0310(10) 0.0378(11) 0.0009(9) 0.0119(10) 0.0077(10) _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 O2 1.4229(13) . ? S1 O3 1.4235(13) . ? S1 O1 1.5940(12) . ? S1 C1 1.7602(18) . ? O1 C13 1.424(2) . ? C1 C2 1.368(2) . ? C1 C10 1.432(2) . ? C2 C3 1.404(2) . ? C2 H2 0.9500 . ? C3 C4 1.365(2) . ? C3 H3 0.9500 . ? C4 C5 1.415(2) . ? C4 H4 0.9500 . ? C5 C10 1.429(2) . ? C5 C6 1.438(2) . ? C6 C7 1.368(3) . ? C6 N1 1.420(2) . ? C7 C8 1.406(3) . ? C7 H7 0.9500 . ? C8 C9 1.365(3) . ? C8 H8 0.9500 . ? C9 C10 1.426(2) . ? C9 H9 0.9500 . ? C13 C14 1.369(3) . ? C13 C18 1.372(3) . ? N1 C12 1.449(2) . ? N1 C11 1.467(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C14 C15 1.381(3) . ? C14 H14 0.9500 . ? C15 C16 1.379(3) . ? C15 H15 0.9500 . ? C16 C17 1.374(3) . ? C16 H16 0.9500 . ? C17 C18 1.381(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? 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 O2 S1 O3 119.98(8) . . ? O2 S1 O1 109.38(7) . . ? O3 S1 O1 103.20(7) . . ? O2 S1 C1 108.94(8) . . ? O3 S1 C1 109.44(8) . . ? O1 S1 C1 104.77(7) . . ? C13 O1 S1 118.27(10) . . ? C2 C1 C10 122.30(16) . . ? C2 C1 S1 116.02(13) . . ? C10 C1 S1 121.49(13) . . ? C1 C2 C3 120.35(16) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C4 C3 C2 119.37(16) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 121.86(17) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C4 C5 C10 119.58(15) . . ? C4 C5 C6 121.05(16) . . ? C10 C5 C6 119.29(16) . . ? C7 C6 N1 123.50(16) . . ? C7 C6 C5 119.22(17) . . ? N1 C6 C5 117.18(15) . . ? C6 C7 C8 120.84(17) . . ? C6 C7 H7 119.6 . . ? C8 C7 H7 119.6 . . ? C9 C8 C7 121.80(17) . . ? C9 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? C8 C9 C10 119.45(18) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C14 C13 C18 122.33(17) . . ? C14 C13 O1 118.44(16) . . ? C18 C13 O1 119.12(16) . . ? C6 N1 C12 116.17(16) . . ? C6 N1 C11 114.32(15) . . ? C12 N1 C11 111.86(15) . . ? C9 C10 C5 119.07(16) . . ? C9 C10 C1 124.48(16) . . ? C5 C10 C1 116.35(15) . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C13 C14 C15 118.46(18) . . ? C13 C14 H14 120.8 . . ? C15 C14 H14 120.8 . . ? C16 C15 C14 120.32(19) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C17 C16 C15 120.05(19) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 120.30(19) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C13 C18 C17 118.52(18) . . ? C13 C18 H18 120.7 . . ? C17 C18 H18 120.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 S1 O1 C13 -47.17(13) . . . . ? O3 S1 O1 C13 -175.96(12) . . . . ? C1 S1 O1 C13 69.49(13) . . . . ? O2 S1 C1 C2 -5.34(15) . . . . ? O3 S1 C1 C2 127.61(13) . . . . ? O1 S1 C1 C2 -122.30(13) . . . . ? O2 S1 C1 C10 179.54(12) . . . . ? O3 S1 C1 C10 -47.50(15) . . . . ? O1 S1 C1 C10 62.59(14) . . . . ? C10 C1 C2 C3 1.5(2) . . . . ? S1 C1 C2 C3 -173.62(13) . . . . ? C1 C2 C3 C4 2.0(3) . . . . ? C2 C3 C4 C5 -2.1(3) . . . . ? C3 C4 C5 C10 -1.2(2) . . . . ? C3 C4 C5 C6 -177.95(16) . . . . ? C4 C5 C6 C7 170.29(16) . . . . ? C10 C5 C6 C7 -6.5(2) . . . . ? C4 C5 C6 N1 -6.2(2) . . . . ? C10 C5 C6 N1 177.01(15) . . . . ? N1 C6 C7 C8 179.76(16) . . . . ? C5 C6 C7 C8 3.5(3) . . . . ? C6 C7 C8 C9 1.7(3) . . . . ? C7 C8 C9 C10 -3.8(3) . . . . ? S1 O1 C13 C14 -99.68(17) . . . . ? S1 O1 C13 C18 84.09(18) . . . . ? C7 C6 N1 C12 -21.8(3) . . . . ? C5 C6 N1 C12 154.50(16) . . . . ? C7 C6 N1 C11 110.8(2) . . . . ? C5 C6 N1 C11 -72.9(2) . . . . ? C8 C9 C10 C5 0.6(2) . . . . ? C8 C9 C10 C1 -175.79(16) . . . . ? C4 C5 C10 C9 -172.40(15) . . . . ? C6 C5 C10 C9 4.4(2) . . . . ? C4 C5 C10 C1 4.3(2) . . . . ? C6 C5 C10 C1 -178.85(14) . . . . ? C2 C1 C10 C9 171.99(16) . . . . ? S1 C1 C10 C9 -13.2(2) . . . . ? C2 C1 C10 C5 -4.5(2) . . . . ? S1 C1 C10 C5 170.27(12) . . . . ? C18 C13 C14 C15 0.1(3) . . . . ? O1 C13 C14 C15 -175.97(17) . . . . ? C13 C14 C15 C16 0.7(3) . . . . ? C14 C15 C16 C17 -1.2(3) . . . . ? C15 C16 C17 C18 0.9(3) . . . . ? C14 C13 C18 C17 -0.4(3) . . . . ? O1 C13 C18 C17 175.63(17) . . . . ? C16 C17 C18 C13 -0.1(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C4 H4 O3 0.95 2.44 3.283(2) 147.9 1_655 C8 H8 O3 0.95 2.60 3.473(2) 152.7 2_545 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.190 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.050 #===END