# Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_Cambridge 0177 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Edwin Weber' _publ_contact_author_email EDWIN.WEBER@CHEMIE.TU-FREIBERG.DE _publ_section_title ; Calix[4]arenes featuring a direct lower rim attachment of dansyl groups. Synthesis, fluorescence properties and first report on crystal structures ; loop_ _publ_author_name 'Edwin Weber' 'Marika Felsmann' 'Conrad Fischer' 'Tobias Gruber' 'Wilhelm Seichter' # Attachment 'S3.cif' data_togr_65_0m _database_code_depnum_ccdc_archive 'CCDC 697366' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H58 N2 O12 S2' _chemical_formula_sum 'C60 H58 N2 O12 S2' _chemical_formula_weight 1063.20 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3908(3) _cell_length_b 13.6976(4) _cell_length_c 17.8554(5) _cell_angle_alpha 91.608(2) _cell_angle_beta 107.3100(10) _cell_angle_gamma 99.1320(10) _cell_volume 2617.64(13) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 7598 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 33.23 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 0.170 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.9010 _exptl_absorpt_correction_T_max 0.9556 _exptl_absorpt_process_details 'SADABS (Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1% _diffrn_reflns_number 92690 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 33.90 _reflns_number_total 20743 _reflns_number_gt 14653 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa APEX 2 (Bruker-AXS)' _computing_cell_refinement 'SAINT-NT (Bruker, 2003)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.1000P)^2^+0.3201P] 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 20743 _refine_ls_number_parameters 691 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0788 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1682 _refine_ls_wR_factor_gt 0.1427 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 S1 S 0.58718(3) 0.72111(2) 0.489962(17) 0.02246(7) Uani 1 1 d . . . S2 S 0.45689(3) 0.69723(3) 0.02315(2) 0.03166(8) Uani 1 1 d . . . O1 O 0.53162(7) 0.73608(6) 0.39845(5) 0.02095(16) Uani 1 1 d . . . O2 O 0.64173(9) 0.63327(8) 0.49806(6) 0.0299(2) Uani 1 1 d . . . O3 O 0.66265(9) 0.81333(8) 0.52751(6) 0.0327(2) Uani 1 1 d . . . O4 O 0.70478(8) 0.85582(7) 0.19222(5) 0.02512(18) Uani 1 1 d . . . O5 O 0.95174(11) 0.93643(14) 0.28202(8) 0.0646(5) Uani 1 1 d . . . O6 O 0.99597(9) 0.97491(9) 0.17216(7) 0.0394(3) Uani 1 1 d . . . O7 O 0.39787(8) 0.74580(7) 0.08343(5) 0.02436(17) Uani 1 1 d . . . O8 O 0.52836(11) 0.63130(10) 0.06893(7) 0.0467(3) Uani 1 1 d . . . O9 O 0.51745(10) 0.77413(10) -0.01160(7) 0.0419(3) Uani 1 1 d . . . O10 O 0.26883(8) 0.53551(6) 0.14836(5) 0.02276(17) Uani 1 1 d . . . O11 O 0.17830(11) 0.30009(9) 0.05600(7) 0.0444(3) Uani 1 1 d . . . O12 O 0.32016(10) 0.34911(8) 0.17289(6) 0.0358(2) Uani 1 1 d . . . N1 N 0.05814(10) 0.78719(9) 0.53451(7) 0.0271(2) Uani 1 1 d . . . N2 N -0.02255(11) 0.56645(9) -0.29379(7) 0.0328(3) Uani 1 1 d . . . C1 C 0.57220(10) 0.68363(9) 0.34344(7) 0.0195(2) Uani 1 1 d . . . C2 C 0.49797(10) 0.59494(9) 0.30606(7) 0.0211(2) Uani 1 1 d . . . C3 C 0.54147(12) 0.54407(10) 0.25403(8) 0.0265(2) Uani 1 1 d . . . H3 H 0.4932 0.4832 0.2271 0.032 Uiso 1 1 calc R . . C4 C 0.65355(12) 0.58033(11) 0.24066(8) 0.0292(3) Uani 1 1 d . . . H4 H 0.6840 0.5424 0.2075 0.035 Uiso 1 1 calc R . . C5 C 0.72117(11) 0.67199(11) 0.27565(8) 0.0271(3) Uani 1 1 d . . . H5 H 0.7964 0.6975 0.2647 0.033 Uiso 1 1 calc R . . C6 C 0.68025(10) 0.72715(9) 0.32664(7) 0.0218(2) Uani 1 1 d . . . C7 C 0.74172(11) 0.83392(10) 0.35448(7) 0.0250(2) Uani 1 1 d . . . H7A H 0.7538 0.8455 0.4115 0.030 Uiso 1 1 calc R . . H7B H 0.8246 0.8472 0.3460 0.030 Uiso 1 1 calc R . . C8 C 0.63920(10) 0.90911(9) 0.22801(7) 0.0212(2) Uani 1 1 d . . . C9 C 0.65978(11) 0.90280(9) 0.30912(7) 0.0224(2) Uani 1 1 d . . . C10 C 0.59599(13) 0.95627(10) 0.34614(8) 0.0279(2) Uani 1 1 d . . . H10 H 0.6116 0.9550 0.4014 0.033 Uiso 1 1 calc R . . C11 C 0.50978(14) 1.01160(11) 0.30394(9) 0.0324(3) Uani 1 1 d . . . H11 H 0.4690 1.0496 0.3303 0.039 Uiso 1 1 calc R . . C12 C 0.48418(13) 1.01058(10) 0.22318(8) 0.0292(3) Uani 1 1 d . . . H12 H 0.4223 1.0457 0.1940 0.035 Uiso 1 1 calc R . . C13 C 0.54735(11) 0.95897(9) 0.18361(7) 0.0227(2) Uani 1 1 d . . . C14 C 0.50955(11) 0.95401(10) 0.09430(7) 0.0264(2) Uani 1 1 d . . . H14A H 0.5304 1.0209 0.0772 0.032 Uiso 1 1 calc R . . H14B H 0.5568 0.9095 0.0752 0.032 Uiso 1 1 calc R . . C15 C 0.31855(10) 0.81613(9) 0.05799(7) 0.0213(2) Uani 1 1 d . . . C16 C 0.37057(11) 0.91576(10) 0.05904(7) 0.0234(2) Uani 1 1 d . . . C17 C 0.28838(12) 0.98156(10) 0.03186(8) 0.0276(3) Uani 1 1 d . . . H17 H 0.3207 1.0496 0.0304 0.033 Uiso 1 1 calc R . . C18 C 0.15955(12) 0.94894(11) 0.00681(8) 0.0300(3) Uani 1 1 d . . . H18 H 0.1050 0.9940 -0.0140 0.036 Uiso 1 1 calc R . . C19 C 0.11092(11) 0.85127(11) 0.01218(8) 0.0272(3) Uani 1 1 d . . . H19 H 0.0229 0.8305 -0.0029 0.033 Uiso 1 1 calc R . . C20 C 0.18951(10) 0.78243(9) 0.03948(7) 0.0222(2) Uani 1 1 d . . . C21 C 0.13648(11) 0.67977(9) 0.05639(7) 0.0233(2) Uani 1 1 d . . . H21A H 0.1755 0.6296 0.0362 0.028 Uiso 1 1 calc R . . H21B H 0.0453 0.6649 0.0297 0.028 Uiso 1 1 calc R . . C22 C 0.23457(10) 0.61050(8) 0.18766(7) 0.0193(2) Uani 1 1 d . . . C23 C 0.16251(10) 0.67581(9) 0.14483(7) 0.0206(2) Uani 1 1 d . . . C24 C 0.12022(12) 0.74329(10) 0.18649(8) 0.0252(2) Uani 1 1 d . . . H24 H 0.0692 0.7872 0.1586 0.030 Uiso 1 1 calc R . . C25 C 0.15158(12) 0.74711(10) 0.26799(8) 0.0276(2) Uani 1 1 d . . . H25 H 0.1188 0.7909 0.2954 0.033 Uiso 1 1 calc R . . C26 C 0.23150(11) 0.68630(10) 0.30918(7) 0.0243(2) Uani 1 1 d . . . H26 H 0.2566 0.6917 0.3651 0.029 Uiso 1 1 calc R . . C27 C 0.27525(10) 0.61788(9) 0.27021(7) 0.0209(2) Uani 1 1 d . . . C28 C 0.37047(11) 0.55772(9) 0.31545(7) 0.0229(2) Uani 1 1 d . . . H28A H 0.3430 0.4870 0.2957 0.027 Uiso 1 1 calc R . . H28B H 0.3763 0.5631 0.3719 0.027 Uiso 1 1 calc R . . C29 C 0.44949(11) 0.70124(9) 0.51756(7) 0.0222(2) Uani 1 1 d . . . C30 C 0.37036(11) 0.77433(9) 0.50780(7) 0.0205(2) Uani 1 1 d . . . C31 C 0.39287(12) 0.86553(9) 0.47416(8) 0.0252(2) Uani 1 1 d . . . H31 H 0.4671 0.8831 0.4600 0.030 Uiso 1 1 calc R . . C32 C 0.30777(13) 0.92803(10) 0.46211(8) 0.0284(3) Uani 1 1 d . . . H32 H 0.3238 0.9890 0.4398 0.034 Uiso 1 1 calc R . . C33 C 0.19671(12) 0.90365(10) 0.48223(8) 0.0275(2) Uani 1 1 d . . . H33 H 0.1385 0.9480 0.4726 0.033 Uiso 1 1 calc R . . C34 C 0.17121(11) 0.81666(10) 0.51555(7) 0.0233(2) Uani 1 1 d . . . C35 C 0.25996(11) 0.75043(9) 0.53046(7) 0.0217(2) Uani 1 1 d . . . C36 C 0.23873(12) 0.66097(10) 0.56641(8) 0.0273(3) Uani 1 1 d . . . H36 H 0.1687 0.6480 0.5854 0.033 Uiso 1 1 calc R . . C37 C 0.31681(13) 0.59301(11) 0.57430(9) 0.0307(3) Uani 1 1 d . . . H37 H 0.2996 0.5329 0.5973 0.037 Uiso 1 1 calc R . . C38 C 0.42305(12) 0.61238(10) 0.54815(8) 0.0270(2) Uani 1 1 d . . . H38 H 0.4758 0.5644 0.5517 0.032 Uiso 1 1 calc R . . C39 C -0.00138(14) 0.86869(12) 0.55030(10) 0.0366(3) Uani 1 1 d . . . H39A H 0.0595 0.9170 0.5902 0.055 Uiso 1 1 calc R . . H39B H -0.0714 0.8429 0.5696 0.055 Uiso 1 1 calc R . . H39C H -0.0323 0.9010 0.5017 0.055 Uiso 1 1 calc R . . C40 C -0.03012(12) 0.71323(12) 0.47404(9) 0.0331(3) Uani 1 1 d . . . H40A H -0.0462 0.7404 0.4225 0.050 Uiso 1 1 calc R . . H40B H -0.1087 0.6971 0.4866 0.050 Uiso 1 1 calc R . . H40C H 0.0058 0.6530 0.4728 0.050 Uiso 1 1 calc R . . C41 C 0.78789(11) 0.91028(11) 0.15693(8) 0.0290(3) Uani 1 1 d . . . H41A H 0.7552 0.9706 0.1373 0.035 Uiso 1 1 calc R . . H41B H 0.7909 0.8695 0.1111 0.035 Uiso 1 1 calc R . . C42 C 0.91925(12) 0.94063(11) 0.21272(9) 0.0304(3) Uani 1 1 d . . . C43 C 1.12574(13) 1.01344(13) 0.21660(11) 0.0411(4) Uani 1 1 d . . . H43A H 1.1785 1.0111 0.1817 0.049 Uiso 1 1 calc R . . H43B H 1.1539 0.9708 0.2599 0.049 Uiso 1 1 calc R . . C44 C 1.1420(2) 1.11651(18) 0.24968(19) 0.0740(7) Uani 1 1 d . . . H44A H 1.1107 1.1583 0.2071 0.111 Uiso 1 1 calc R . . H44B H 1.2308 1.1413 0.2762 0.111 Uiso 1 1 calc R . . H44C H 1.0952 1.1182 0.2876 0.111 Uiso 1 1 calc R . . C45 C 0.32668(13) 0.62605(11) -0.04940(8) 0.0288(3) Uani 1 1 d . . . C46 C 0.25421(12) 0.66589(10) -0.11794(8) 0.0267(2) Uani 1 1 d . . . C47 C 0.27869(15) 0.76649(11) -0.13635(9) 0.0355(3) Uani 1 1 d . . . H47 H 0.3453 0.8121 -0.1013 0.043 Uiso 1 1 calc R . . C48 C 0.20696(17) 0.79722(12) -0.20396(10) 0.0397(3) Uani 1 1 d . . . H48 H 0.2247 0.8642 -0.2155 0.048 Uiso 1 1 calc R . . C49 C 0.10655(15) 0.73164(11) -0.25749(9) 0.0349(3) Uani 1 1 d . . . H49 H 0.0587 0.7548 -0.3046 0.042 Uiso 1 1 calc R . . C50 C 0.07788(12) 0.63469(10) -0.24175(8) 0.0279(2) Uani 1 1 d . . . C51 C 0.15061(12) 0.60024(10) -0.17024(8) 0.0252(2) Uani 1 1 d . . . C52 C 0.11973(13) 0.50168(10) -0.15067(8) 0.0284(3) Uani 1 1 d . . . H52 H 0.0470 0.4596 -0.1835 0.034 Uiso 1 1 calc R . . C53 C 0.19279(15) 0.46647(11) -0.08552(9) 0.0327(3) Uani 1 1 d . . . H53 H 0.1720 0.3997 -0.0742 0.039 Uiso 1 1 calc R . . C54 C 0.29874(14) 0.52859(11) -0.03504(9) 0.0326(3) Uani 1 1 d . . . H54 H 0.3511 0.5030 0.0091 0.039 Uiso 1 1 calc R . . C55 C -0.11913(15) 0.61111(15) -0.34679(11) 0.0466(4) Uani 1 1 d . . . H55A H -0.1487 0.6570 -0.3164 0.070 Uiso 1 1 calc R . . H55B H -0.1890 0.5590 -0.3754 0.070 Uiso 1 1 calc R . . H55C H -0.0850 0.6474 -0.3843 0.070 Uiso 1 1 calc R . . C56 C 0.01650(16) 0.49132(13) -0.33657(10) 0.0409(4) Uani 1 1 d . . . H56A H 0.0397 0.5203 -0.3809 0.061 Uiso 1 1 calc R . . H56B H -0.0525 0.4353 -0.3564 0.061 Uiso 1 1 calc R . . H56C H 0.0885 0.4681 -0.3011 0.061 Uiso 1 1 calc R . . C57 C 0.17114(12) 0.45119(10) 0.12444(9) 0.0306(3) Uani 1 1 d . . . H57A H 0.1090 0.4627 0.0748 0.037 Uiso 1 1 calc R . . H57B H 0.1283 0.4416 0.1652 0.037 Uiso 1 1 calc R . . C58 C 0.22296(12) 0.35894(10) 0.11219(8) 0.0277(2) Uani 1 1 d . . . C59 C 0.38029(16) 0.26434(11) 0.16770(11) 0.0390(3) Uani 1 1 d . . . H59A H 0.4108 0.2661 0.1212 0.047 Uiso 1 1 calc R . . H59B H 0.3206 0.2017 0.1628 0.047 Uiso 1 1 calc R . . C60 C 0.4880(2) 0.27108(15) 0.24220(15) 0.0671(7) Uani 1 1 d . . . H60A H 0.5492 0.3310 0.2444 0.101 Uiso 1 1 calc R . . H60B H 0.5277 0.2125 0.2429 0.101 Uiso 1 1 calc R . . H60C H 0.4573 0.2742 0.2878 0.101 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 0.01847(11) 0.02922(15) 0.01996(13) 0.00323(11) 0.00463(10) 0.00714(10) S2 0.02370(14) 0.0452(2) 0.02704(16) -0.00367(14) 0.00621(12) 0.01292(13) O1 0.0197(3) 0.0243(4) 0.0199(4) 0.0039(3) 0.0056(3) 0.0075(3) O2 0.0276(4) 0.0401(5) 0.0277(5) 0.0113(4) 0.0094(4) 0.0191(4) O3 0.0247(4) 0.0397(6) 0.0289(5) -0.0061(4) 0.0053(4) -0.0011(4) O4 0.0227(4) 0.0284(4) 0.0264(4) 0.0056(4) 0.0103(3) 0.0047(3) O5 0.0318(6) 0.1127(13) 0.0363(6) 0.0223(7) 0.0047(5) -0.0175(7) O6 0.0245(4) 0.0560(7) 0.0395(6) 0.0077(5) 0.0150(4) 0.0008(4) O7 0.0215(4) 0.0313(5) 0.0211(4) 0.0021(3) 0.0047(3) 0.0107(3) O8 0.0401(6) 0.0612(8) 0.0409(6) -0.0025(6) 0.0042(5) 0.0326(6) O9 0.0326(5) 0.0619(8) 0.0331(5) -0.0045(5) 0.0168(4) 0.0019(5) O10 0.0199(3) 0.0198(4) 0.0277(4) -0.0036(3) 0.0066(3) 0.0033(3) O11 0.0441(6) 0.0340(6) 0.0447(6) -0.0146(5) -0.0019(5) 0.0100(5) O12 0.0384(5) 0.0280(5) 0.0361(5) -0.0069(4) 0.0009(4) 0.0138(4) N1 0.0212(4) 0.0332(6) 0.0282(5) 0.0013(4) 0.0074(4) 0.0086(4) N2 0.0275(5) 0.0337(6) 0.0326(6) 0.0024(5) 0.0049(5) 0.0002(4) C1 0.0181(4) 0.0225(5) 0.0191(5) 0.0043(4) 0.0054(4) 0.0072(4) C2 0.0185(4) 0.0217(5) 0.0230(5) 0.0045(4) 0.0044(4) 0.0065(4) C3 0.0250(5) 0.0256(6) 0.0290(6) 0.0010(5) 0.0059(5) 0.0092(4) C4 0.0277(6) 0.0357(7) 0.0283(6) 0.0024(5) 0.0098(5) 0.0149(5) C5 0.0207(5) 0.0373(7) 0.0271(6) 0.0085(5) 0.0102(4) 0.0094(5) C6 0.0176(4) 0.0275(6) 0.0204(5) 0.0069(4) 0.0048(4) 0.0055(4) C7 0.0189(4) 0.0309(6) 0.0215(5) 0.0069(5) 0.0025(4) 0.0004(4) C8 0.0188(4) 0.0217(5) 0.0216(5) 0.0029(4) 0.0053(4) 0.0000(4) C9 0.0209(5) 0.0227(5) 0.0201(5) 0.0024(4) 0.0032(4) -0.0006(4) C10 0.0324(6) 0.0268(6) 0.0228(6) 0.0006(5) 0.0082(5) 0.0013(5) C11 0.0390(7) 0.0297(7) 0.0308(7) -0.0019(5) 0.0126(6) 0.0099(6) C12 0.0315(6) 0.0267(6) 0.0300(6) 0.0041(5) 0.0088(5) 0.0081(5) C13 0.0216(5) 0.0220(5) 0.0228(5) 0.0045(4) 0.0053(4) 0.0010(4) C14 0.0206(5) 0.0338(7) 0.0231(5) 0.0091(5) 0.0051(4) 0.0016(4) C15 0.0188(4) 0.0285(6) 0.0166(5) 0.0034(4) 0.0038(4) 0.0070(4) C16 0.0208(5) 0.0307(6) 0.0184(5) 0.0059(4) 0.0054(4) 0.0043(4) C17 0.0268(5) 0.0305(6) 0.0273(6) 0.0115(5) 0.0089(5) 0.0076(5) C18 0.0257(5) 0.0354(7) 0.0309(6) 0.0137(5) 0.0073(5) 0.0114(5) C19 0.0194(5) 0.0361(7) 0.0262(6) 0.0084(5) 0.0050(4) 0.0079(5) C20 0.0195(4) 0.0281(6) 0.0186(5) 0.0026(4) 0.0042(4) 0.0054(4) C21 0.0200(4) 0.0257(6) 0.0220(5) -0.0009(4) 0.0034(4) 0.0037(4) C22 0.0158(4) 0.0190(5) 0.0229(5) -0.0009(4) 0.0059(4) 0.0026(4) C23 0.0174(4) 0.0200(5) 0.0234(5) -0.0005(4) 0.0053(4) 0.0027(4) C24 0.0246(5) 0.0244(6) 0.0283(6) 0.0017(5) 0.0084(4) 0.0084(4) C25 0.0293(6) 0.0279(6) 0.0287(6) -0.0013(5) 0.0115(5) 0.0092(5) C26 0.0241(5) 0.0268(6) 0.0219(5) -0.0007(4) 0.0069(4) 0.0045(4) C27 0.0174(4) 0.0204(5) 0.0242(5) 0.0018(4) 0.0061(4) 0.0017(4) C28 0.0200(4) 0.0222(5) 0.0250(6) 0.0043(4) 0.0049(4) 0.0031(4) C29 0.0219(5) 0.0271(6) 0.0197(5) 0.0045(4) 0.0073(4) 0.0082(4) C30 0.0218(5) 0.0229(5) 0.0172(5) 0.0010(4) 0.0057(4) 0.0058(4) C31 0.0269(5) 0.0217(5) 0.0286(6) 0.0019(5) 0.0111(5) 0.0042(4) C32 0.0343(6) 0.0212(6) 0.0316(6) 0.0029(5) 0.0120(5) 0.0070(5) C33 0.0294(6) 0.0241(6) 0.0302(6) 0.0011(5) 0.0080(5) 0.0107(5) C34 0.0215(5) 0.0284(6) 0.0201(5) -0.0007(4) 0.0051(4) 0.0079(4) C35 0.0211(4) 0.0268(6) 0.0177(5) 0.0026(4) 0.0050(4) 0.0069(4) C36 0.0249(5) 0.0341(7) 0.0264(6) 0.0107(5) 0.0106(5) 0.0087(5) C37 0.0318(6) 0.0332(7) 0.0329(7) 0.0159(6) 0.0144(5) 0.0115(5) C38 0.0285(5) 0.0303(6) 0.0262(6) 0.0106(5) 0.0096(5) 0.0126(5) C39 0.0301(6) 0.0422(8) 0.0417(8) -0.0025(6) 0.0134(6) 0.0149(6) C40 0.0239(5) 0.0370(7) 0.0354(7) 0.0006(6) 0.0043(5) 0.0060(5) C41 0.0217(5) 0.0404(7) 0.0265(6) 0.0089(5) 0.0099(5) 0.0045(5) C42 0.0232(5) 0.0380(7) 0.0315(7) 0.0084(6) 0.0104(5) 0.0046(5) C43 0.0241(6) 0.0470(9) 0.0531(10) 0.0037(7) 0.0161(6) 0.0011(6) C44 0.0549(12) 0.0601(14) 0.108(2) -0.0143(13) 0.0374(13) -0.0070(10) C45 0.0300(6) 0.0343(7) 0.0248(6) 0.0006(5) 0.0099(5) 0.0113(5) C46 0.0279(5) 0.0303(6) 0.0239(6) 0.0026(5) 0.0097(5) 0.0074(5) C47 0.0406(7) 0.0295(7) 0.0301(7) 0.0002(5) 0.0046(6) 0.0001(6) C48 0.0510(9) 0.0264(7) 0.0364(8) 0.0056(6) 0.0070(7) 0.0030(6) C49 0.0385(7) 0.0309(7) 0.0320(7) 0.0066(6) 0.0051(6) 0.0063(6) C50 0.0258(5) 0.0303(6) 0.0279(6) 0.0035(5) 0.0086(5) 0.0043(5) C51 0.0267(5) 0.0259(6) 0.0263(6) 0.0025(5) 0.0117(5) 0.0069(4) C52 0.0326(6) 0.0273(6) 0.0302(6) 0.0013(5) 0.0167(5) 0.0060(5) C53 0.0444(7) 0.0279(6) 0.0347(7) 0.0078(5) 0.0217(6) 0.0127(6) C54 0.0415(7) 0.0355(7) 0.0272(6) 0.0061(5) 0.0137(6) 0.0190(6) C55 0.0308(7) 0.0535(10) 0.0462(9) 0.0160(8) 0.0005(6) -0.0002(7) C56 0.0445(8) 0.0385(8) 0.0383(8) -0.0049(6) 0.0190(7) -0.0074(7) C57 0.0222(5) 0.0225(6) 0.0418(8) -0.0068(5) 0.0029(5) 0.0029(4) C58 0.0269(5) 0.0218(6) 0.0322(6) -0.0022(5) 0.0077(5) 0.0018(4) C59 0.0442(8) 0.0276(7) 0.0467(9) -0.0003(6) 0.0121(7) 0.0150(6) C60 0.0636(12) 0.0364(9) 0.0807(15) -0.0025(10) -0.0149(11) 0.0216(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 S1 O3 1.4314(11) . ? S1 O2 1.4312(10) . ? S1 O1 1.5991(9) . ? S1 C29 1.7631(12) . ? S2 O8 1.4232(12) . ? S2 O9 1.4251(13) . ? S2 O7 1.6080(9) . ? S2 C45 1.7763(14) . ? O1 C1 1.4250(14) . ? O4 C8 1.3893(15) . ? O4 C41 1.4168(15) . ? O5 C42 1.1874(19) . ? O6 C42 1.3319(16) . ? O6 C43 1.4575(18) . ? O7 C15 1.4168(14) . ? O10 C22 1.3964(14) . ? O10 C57 1.4269(15) . ? O11 C58 1.1984(17) . ? O12 C58 1.3266(17) . ? O12 C59 1.4527(17) . ? N1 C34 1.4277(16) . ? N1 C39 1.4566(18) . ? N1 C40 1.4739(19) . ? N2 C50 1.4231(18) . ? N2 C55 1.451(2) . ? N2 C56 1.464(2) . ? C1 C2 1.3888(17) . ? C1 C6 1.3989(16) . ? C2 C3 1.3932(18) . ? C2 C28 1.5206(16) . ? C3 C4 1.3858(19) . ? C3 H3 0.9500 . ? C4 C5 1.387(2) . ? C4 H4 0.9500 . ? C5 C6 1.3938(18) . ? C5 H5 0.9500 . ? C6 C7 1.5177(18) . ? C7 C9 1.5132(17) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C13 1.3976(16) . ? C8 C9 1.4040(17) . ? C9 C10 1.3889(19) . ? C10 C11 1.391(2) . ? C10 H10 0.9500 . ? C11 C12 1.383(2) . ? C11 H11 0.9500 . ? C12 C13 1.3974(19) . ? C12 H12 0.9500 . ? C13 C14 1.5195(18) . ? C14 C16 1.5174(16) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.3962(18) . ? C15 C20 1.4035(16) . ? C16 C17 1.3951(17) . ? C17 C18 1.3941(18) . ? C17 H17 0.9500 . ? C18 C19 1.382(2) . ? C18 H18 0.9500 . ? C19 C20 1.4009(17) . ? C19 H19 0.9500 . ? C20 C21 1.5152(18) . ? C21 C23 1.5217(17) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.3988(16) . ? C22 C27 1.4027(17) . ? C23 C24 1.3985(17) . ? C24 C25 1.3887(19) . ? C24 H24 0.9500 . ? C25 C26 1.3929(18) . ? C25 H25 0.9500 . ? C26 C27 1.3887(17) . ? C26 H26 0.9500 . ? C27 C28 1.5192(16) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C38 1.3746(18) . ? C29 C30 1.4311(16) . ? C30 C31 1.4210(17) . ? C30 C35 1.4254(16) . ? C31 C32 1.3670(18) . ? C31 H31 0.9500 . ? C32 C33 1.4086(19) . ? C32 H32 0.9500 . ? C33 C34 1.3750(19) . ? C33 H33 0.9500 . ? C34 C35 1.4354(16) . ? C35 C36 1.4193(18) . ? C36 C37 1.3686(19) . ? C36 H36 0.9500 . ? C37 C38 1.4122(18) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.5153(19) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C43 C44 1.477(3) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C54 1.372(2) . ? C45 C46 1.4340(19) . ? C46 C51 1.4260(19) . ? C46 C47 1.429(2) . ? C47 C48 1.361(2) . ? C47 H47 0.9500 . ? C48 C49 1.416(2) . ? C48 H48 0.9500 . ? C49 C50 1.374(2) . ? C49 H49 0.9500 . ? C50 C51 1.4380(19) . ? C51 C52 1.4203(19) . ? C52 C53 1.364(2) . ? C52 H52 0.9500 . ? C53 C54 1.406(2) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.5136(19) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C59 C60 1.507(3) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? 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 O3 S1 O2 118.98(6) . . ? O3 S1 O1 107.37(6) . . ? O2 S1 O1 108.97(5) . . ? O3 S1 C29 109.34(6) . . ? O2 S1 C29 109.79(6) . . ? O1 S1 C29 100.83(5) . . ? O8 S2 O9 119.27(8) . . ? O8 S2 O7 103.54(6) . . ? O9 S2 O7 109.28(6) . . ? O8 S2 C45 108.65(7) . . ? O9 S2 C45 110.30(7) . . ? O7 S2 C45 104.68(6) . . ? C1 O1 S1 118.59(7) . . ? C8 O4 C41 117.44(10) . . ? C42 O6 C43 117.42(12) . . ? C15 O7 S2 119.90(8) . . ? C22 O10 C57 111.31(9) . . ? C58 O12 C59 117.09(12) . . ? C34 N1 C39 114.78(11) . . ? C34 N1 C40 110.94(11) . . ? C39 N1 C40 111.20(11) . . ? C50 N2 C55 115.18(13) . . ? C50 N2 C56 114.32(12) . . ? C55 N2 C56 110.89(14) . . ? C2 C1 C6 123.68(11) . . ? C2 C1 O1 117.96(10) . . ? C6 C1 O1 118.24(10) . . ? C1 C2 C3 116.71(11) . . ? C1 C2 C28 122.57(11) . . ? C3 C2 C28 120.55(11) . . ? C4 C3 C2 121.43(12) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 119.96(12) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 120.87(12) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 116.95(11) . . ? C5 C6 C7 120.91(11) . . ? C1 C6 C7 121.75(11) . . ? C9 C7 C6 109.39(9) . . ? C9 C7 H7A 109.8 . . ? C6 C7 H7A 109.8 . . ? C9 C7 H7B 109.8 . . ? C6 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? O4 C8 C13 121.09(11) . . ? O4 C8 C9 117.44(10) . . ? C13 C8 C9 121.17(11) . . ? C10 C9 C8 118.32(11) . . ? C10 C9 C7 120.25(11) . . ? C8 C9 C7 121.28(11) . . ? C9 C10 C11 121.31(12) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C12 C11 C10 119.22(13) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? C11 C12 C13 121.39(12) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C8 C13 C12 118.22(12) . . ? C8 C13 C14 122.29(12) . . ? C12 C13 C14 119.40(11) . . ? C16 C14 C13 110.62(10) . . ? C16 C14 H14A 109.5 . . ? C13 C14 H14A 109.5 . . ? C16 C14 H14B 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C16 C15 C20 122.96(11) . . ? C16 C15 O7 119.63(10) . . ? C20 C15 O7 117.16(11) . . ? C17 C16 C15 117.29(11) . . ? C17 C16 C14 120.33(12) . . ? C15 C16 C14 122.19(11) . . ? C16 C17 C18 120.96(12) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C19 C18 C17 120.22(12) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 120.94(11) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C19 C20 C15 117.15(11) . . ? C19 C20 C21 120.47(10) . . ? C15 C20 C21 122.05(11) . . ? C20 C21 C23 109.11(10) . . ? C20 C21 H21A 109.9 . . ? C23 C21 H21A 109.9 . . ? C20 C21 H21B 109.9 . . ? C23 C21 H21B 109.9 . . ? H21A C21 H21B 108.3 . . ? O10 C22 C23 120.07(10) . . ? O10 C22 C27 117.95(10) . . ? C23 C22 C27 121.98(11) . . ? C24 C23 C22 117.89(11) . . ? C24 C23 C21 119.71(11) . . ? C22 C23 C21 122.27(11) . . ? C25 C24 C23 121.03(12) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 C26 119.48(12) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C27 C26 C25 121.35(12) . . ? C27 C26 H26 119.3 . . ? C25 C26 H26 119.3 . . ? C26 C27 C22 117.86(11) . . ? C26 C27 C28 121.02(11) . . ? C22 C27 C28 121.01(11) . . ? C27 C28 C2 110.56(9) . . ? C27 C28 H28A 109.5 . . ? C2 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C2 C28 H28B 109.5 . . ? H28A C28 H28B 108.1 . . ? C38 C29 C30 122.57(11) . . ? C38 C29 S1 116.38(9) . . ? C30 C29 S1 121.04(9) . . ? C31 C30 C35 119.16(11) . . ? C31 C30 C29 124.01(11) . . ? C35 C30 C29 116.77(11) . . ? C32 C31 C30 120.05(12) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 121.14(12) . . ? C31 C32 H32 119.4 . . ? C33 C32 H32 119.4 . . ? C34 C33 C32 120.98(12) . . ? C34 C33 H33 119.5 . . ? C32 C33 H33 119.5 . . ? C33 C34 N1 123.01(11) . . ? C33 C34 C35 119.21(11) . . ? N1 C34 C35 117.76(11) . . ? C36 C35 C30 119.52(11) . . ? C36 C35 C34 121.07(11) . . ? C30 C35 C34 119.40(11) . . ? C37 C36 C35 121.51(12) . . ? C37 C36 H36 119.2 . . ? C35 C36 H36 119.2 . . ? C36 C37 C38 119.94(12) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C29 C38 C37 119.45(12) . . ? C29 C38 H38 120.3 . . ? C37 C38 H38 120.3 . . ? N1 C39 H39A 109.5 . . ? N1 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N1 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N1 C40 H40A 109.5 . . ? N1 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N1 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O4 C41 C42 113.20(11) . . ? O4 C41 H41A 108.9 . . ? C42 C41 H41A 108.9 . . ? O4 C41 H41B 108.9 . . ? C42 C41 H41B 108.9 . . ? H41A C41 H41B 107.8 . . ? O5 C42 O6 123.76(13) . . ? O5 C42 C41 126.82(12) . . ? O6 C42 C41 109.42(12) . . ? O6 C43 C44 111.72(16) . . ? O6 C43 H43A 109.3 . . ? C44 C43 H43A 109.3 . . ? O6 C43 H43B 109.3 . . ? C44 C43 H43B 109.3 . . ? H43A C43 H43B 107.9 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C54 C45 C46 121.56(13) . . ? C54 C45 S2 114.92(11) . . ? C46 C45 S2 123.51(11) . . ? C51 C46 C47 118.54(12) . . ? C51 C46 C45 117.21(12) . . ? C47 C46 C45 124.25(13) . . ? C48 C47 C46 120.24(14) . . ? C48 C47 H47 119.9 . . ? C46 C47 H47 119.9 . . ? C47 C48 C49 121.53(14) . . ? C47 C48 H48 119.2 . . ? C49 C48 H48 119.2 . . ? C50 C49 C48 120.42(13) . . ? C50 C49 H49 119.8 . . ? C48 C49 H49 119.8 . . ? C49 C50 N2 122.22(13) . . ? C49 C50 C51 119.44(13) . . ? N2 C50 C51 118.33(12) . . ? C52 C51 C46 119.53(12) . . ? C52 C51 C50 120.72(12) . . ? C46 C51 C50 119.75(12) . . ? C53 C52 C51 121.08(13) . . ? C53 C52 H52 119.5 . . ? C51 C52 H52 119.5 . . ? C52 C53 C54 120.24(13) . . ? C52 C53 H53 119.9 . . ? C54 C53 H53 119.9 . . ? C45 C54 C53 120.17(13) . . ? C45 C54 H54 119.9 . . ? C53 C54 H54 119.9 . . ? N2 C55 H55A 109.5 . . ? N2 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? N2 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N2 C56 H56A 109.5 . . ? N2 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? N2 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O10 C57 C58 110.64(10) . . ? O10 C57 H57A 109.5 . . ? C58 C57 H57A 109.5 . . ? O10 C57 H57B 109.5 . . ? C58 C57 H57B 109.5 . . ? H57A C57 H57B 108.1 . . ? O11 C58 O12 124.30(13) . . ? O11 C58 C57 123.99(13) . . ? O12 C58 C57 111.65(11) . . ? O12 C59 C60 106.80(14) . . ? O12 C59 H59A 110.4 . . ? C60 C59 H59A 110.4 . . ? O12 C59 H59B 110.4 . . ? C60 C59 H59B 110.4 . . ? H59A C59 H59B 108.6 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? 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 O3 S1 O1 C1 112.88(9) . . . . ? O2 S1 O1 C1 -17.24(10) . . . . ? C29 S1 O1 C1 -132.72(9) . . . . ? O8 S2 O7 C15 -179.49(10) . . . . ? O9 S2 O7 C15 52.42(10) . . . . ? C45 S2 O7 C15 -65.72(10) . . . . ? S1 O1 C1 C2 96.51(11) . . . . ? S1 O1 C1 C6 -87.27(11) . . . . ? C6 C1 C2 C3 5.52(17) . . . . ? O1 C1 C2 C3 -178.48(10) . . . . ? C6 C1 C2 C28 -169.74(11) . . . . ? O1 C1 C2 C28 6.25(16) . . . . ? C1 C2 C3 C4 0.22(18) . . . . ? C28 C2 C3 C4 175.58(11) . . . . ? C2 C3 C4 C5 -4.0(2) . . . . ? C3 C4 C5 C6 2.30(19) . . . . ? C4 C5 C6 C1 3.01(18) . . . . ? C4 C5 C6 C7 -169.94(11) . . . . ? C2 C1 C6 C5 -7.13(17) . . . . ? O1 C1 C6 C5 176.89(10) . . . . ? C2 C1 C6 C7 165.76(11) . . . . ? O1 C1 C6 C7 -10.22(16) . . . . ? C5 C6 C7 C9 102.38(13) . . . . ? C1 C6 C7 C9 -70.23(14) . . . . ? C41 O4 C8 C13 67.88(14) . . . . ? C41 O4 C8 C9 -118.33(12) . . . . ? O4 C8 C9 C10 179.41(10) . . . . ? C13 C8 C9 C10 -6.80(17) . . . . ? O4 C8 C9 C7 -5.05(16) . . . . ? C13 C8 C9 C7 168.74(11) . . . . ? C6 C7 C9 C10 108.96(13) . . . . ? C6 C7 C9 C8 -66.49(14) . . . . ? C8 C9 C10 C11 2.67(19) . . . . ? C7 C9 C10 C11 -172.92(12) . . . . ? C9 C10 C11 C12 2.2(2) . . . . ? C10 C11 C12 C13 -3.1(2) . . . . ? O4 C8 C13 C12 179.51(11) . . . . ? C9 C8 C13 C12 5.95(17) . . . . ? O4 C8 C13 C14 2.98(17) . . . . ? C9 C8 C13 C14 -170.58(11) . . . . ? C11 C12 C13 C8 -0.94(19) . . . . ? C11 C12 C13 C14 175.70(12) . . . . ? C8 C13 C14 C16 123.02(12) . . . . ? C12 C13 C14 C16 -53.47(16) . . . . ? S2 O7 C15 C16 -84.30(13) . . . . ? S2 O7 C15 C20 101.35(11) . . . . ? C20 C15 C16 C17 -7.28(18) . . . . ? O7 C15 C16 C17 178.71(11) . . . . ? C20 C15 C16 C14 167.70(12) . . . . ? O7 C15 C16 C14 -6.31(18) . . . . ? C13 C14 C16 C17 100.88(14) . . . . ? C13 C14 C16 C15 -73.95(16) . . . . ? C15 C16 C17 C18 1.71(19) . . . . ? C14 C16 C17 C18 -173.36(13) . . . . ? C16 C17 C18 C19 3.2(2) . . . . ? C17 C18 C19 C20 -2.8(2) . . . . ? C18 C19 C20 C15 -2.43(19) . . . . ? C18 C19 C20 C21 171.06(13) . . . . ? C16 C15 C20 C19 7.64(18) . . . . ? O7 C15 C20 C19 -178.22(11) . . . . ? C16 C15 C20 C21 -165.74(11) . . . . ? O7 C15 C20 C21 8.41(17) . . . . ? C19 C20 C21 C23 -102.10(13) . . . . ? C15 C20 C21 C23 71.07(14) . . . . ? C57 O10 C22 C23 -82.63(13) . . . . ? C57 O10 C22 C27 97.76(12) . . . . ? O10 C22 C23 C24 173.80(10) . . . . ? C27 C22 C23 C24 -6.61(16) . . . . ? O10 C22 C23 C21 -10.16(16) . . . . ? C27 C22 C23 C21 169.43(10) . . . . ? C20 C21 C23 C24 56.96(14) . . . . ? C20 C21 C23 C22 -119.01(12) . . . . ? C22 C23 C24 C25 1.69(18) . . . . ? C21 C23 C24 C25 -174.45(11) . . . . ? C23 C24 C25 C26 3.27(19) . . . . ? C24 C25 C26 C27 -3.56(19) . . . . ? C25 C26 C27 C22 -1.14(18) . . . . ? C25 C26 C27 C28 175.04(11) . . . . ? O10 C22 C27 C26 -174.06(10) . . . . ? C23 C22 C27 C26 6.34(16) . . . . ? O10 C22 C27 C28 9.76(15) . . . . ? C23 C22 C27 C28 -169.84(10) . . . . ? C26 C27 C28 C2 -106.71(13) . . . . ? C22 C27 C28 C2 69.34(14) . . . . ? C1 C2 C28 C27 73.49(14) . . . . ? C3 C2 C28 C27 -101.60(13) . . . . ? O3 S1 C29 C38 -126.55(11) . . . . ? O2 S1 C29 C38 5.68(12) . . . . ? O1 S1 C29 C38 120.55(10) . . . . ? O3 S1 C29 C30 53.77(12) . . . . ? O2 S1 C29 C30 -174.01(10) . . . . ? O1 S1 C29 C30 -59.14(11) . . . . ? C38 C29 C30 C31 -177.96(13) . . . . ? S1 C29 C30 C31 1.70(17) . . . . ? C38 C29 C30 C35 -0.86(18) . . . . ? S1 C29 C30 C35 178.80(9) . . . . ? C35 C30 C31 C32 -1.57(19) . . . . ? C29 C30 C31 C32 175.47(12) . . . . ? C30 C31 C32 C33 -0.3(2) . . . . ? C31 C32 C33 C34 0.8(2) . . . . ? C32 C33 C34 N1 -177.84(12) . . . . ? C32 C33 C34 C35 0.5(2) . . . . ? C39 N1 C34 C33 -26.52(18) . . . . ? C40 N1 C34 C33 100.56(15) . . . . ? C39 N1 C34 C35 155.12(12) . . . . ? C40 N1 C34 C35 -77.79(14) . . . . ? C31 C30 C35 C36 -178.00(12) . . . . ? C29 C30 C35 C36 4.75(17) . . . . ? C31 C30 C35 C34 2.84(17) . . . . ? C29 C30 C35 C34 -174.41(11) . . . . ? C33 C34 C35 C36 178.55(12) . . . . ? N1 C34 C35 C36 -3.04(18) . . . . ? C33 C34 C35 C30 -2.31(18) . . . . ? N1 C34 C35 C30 176.11(11) . . . . ? C30 C35 C36 C37 -5.3(2) . . . . ? C34 C35 C36 C37 173.89(13) . . . . ? C35 C36 C37 C38 1.6(2) . . . . ? C30 C29 C38 C37 -2.7(2) . . . . ? S1 C29 C38 C37 177.59(11) . . . . ? C36 C37 C38 C29 2.4(2) . . . . ? C8 O4 C41 C42 90.35(14) . . . . ? C43 O6 C42 O5 -2.9(3) . . . . ? C43 O6 C42 C41 176.41(13) . . . . ? O4 C41 C42 O5 -12.0(2) . . . . ? O4 C41 C42 O6 168.72(12) . . . . ? C42 O6 C43 C44 -81.5(2) . . . . ? O8 S2 C45 C54 17.66(13) . . . . ? O9 S2 C45 C54 150.12(11) . . . . ? O7 S2 C45 C54 -92.44(11) . . . . ? O8 S2 C45 C46 -162.81(12) . . . . ? O9 S2 C45 C46 -30.36(14) . . . . ? O7 S2 C45 C46 87.08(12) . . . . ? C54 C45 C46 C51 0.78(19) . . . . ? S2 C45 C46 C51 -178.72(10) . . . . ? C54 C45 C46 C47 -179.80(14) . . . . ? S2 C45 C46 C47 0.7(2) . . . . ? C51 C46 C47 C48 -2.4(2) . . . . ? C45 C46 C47 C48 178.16(15) . . . . ? C46 C47 C48 C49 0.3(3) . . . . ? C47 C48 C49 C50 0.8(3) . . . . ? C48 C49 C50 N2 179.74(15) . . . . ? C48 C49 C50 C51 0.1(2) . . . . ? C55 N2 C50 C49 -22.4(2) . . . . ? C56 N2 C50 C49 107.79(17) . . . . ? C55 N2 C50 C51 157.23(14) . . . . ? C56 N2 C50 C51 -72.61(16) . . . . ? C47 C46 C51 C52 -176.06(13) . . . . ? C45 C46 C51 C52 3.40(18) . . . . ? C47 C46 C51 C50 3.36(19) . . . . ? C45 C46 C51 C50 -177.18(12) . . . . ? C49 C50 C51 C52 177.16(13) . . . . ? N2 C50 C51 C52 -2.46(19) . . . . ? C49 C50 C51 C46 -2.3(2) . . . . ? N2 C50 C51 C46 178.13(12) . . . . ? C46 C51 C52 C53 -4.78(19) . . . . ? C50 C51 C52 C53 175.81(13) . . . . ? C51 C52 C53 C54 1.9(2) . . . . ? C46 C45 C54 C53 -3.7(2) . . . . ? S2 C45 C54 C53 175.81(11) . . . . ? C52 C53 C54 C45 2.4(2) . . . . ? C22 O10 C57 C58 -157.55(11) . . . . ? C59 O12 C58 O11 4.1(2) . . . . ? C59 O12 C58 C57 -178.74(13) . . . . ? O10 C57 C58 O11 -133.55(15) . . . . ? O10 C57 C58 O12 49.31(16) . . . . ? C58 O12 C59 C60 178.91(17) . . . . ? 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 C38 H38 O2 0.95 2.44 2.8636(16) 107.1 1 C7 H7A O3 0.99 2.60 3.4727(16) 147.2 1 C54 H54 O8 0.95 2.41 2.839(2) 107.4 1 C14 H14B O9 0.99 2.28 3.0927(19) 138.5 1 C59 H59A O9 0.99 2.42 3.383(2) 165.5 2_665 _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 33.90 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.654 _refine_diff_density_min -0.439 _refine_diff_density_rms 0.067 # Attachment 'S1_NEW.cif' data_togr_66y_0m _database_code_depnum_ccdc_archive 'CCDC 697367' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C74 H90 N2 O8 S2, 3(C2 H3 N)' _chemical_formula_sum 'C80 H99 N5 O8 S2' _chemical_formula_weight 1322.76 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.2063(9) _cell_length_b 14.9874(10) _cell_length_c 21.3373(13) _cell_angle_alpha 81.511(4) _cell_angle_beta 88.632(4) _cell_angle_gamma 66.270(4) _cell_volume 3820.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 5006 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 23.43 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.150 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1420 _exptl_absorpt_coefficient_mu 0.126 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.9344 _exptl_absorpt_correction_T_max 0.9875 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 62113 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.0631 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.44 _reflns_number_total 14014 _reflns_number_gt 8546 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa APEX 2 (Bruker-AXS)' _computing_cell_refinement 'SAINT-NT (Bruker, 2003)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia)' _computing_publication_material SHELXTL _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. 12 atom distances regarding the disordered tert-butyl groups (C45-C46, C45-C47, C45-C48, C45-C46A, C45-C47A, C45-C48A, C68-C69, C68-C70, C68-C71, C68-C69A, C68-C70A, C68-C71A) were restrained to a target value of 1.54 (0.01) angstrom. The bond distances of one acetonitrile were restrained to a target value of 1.45 (0.01) for C1I-C2I and 1.23 (0.01) angstrom for C1I-N1I. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1422P)^2^+4.6045P] 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 14014 _refine_ls_number_parameters 903 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1352 _refine_ls_R_factor_gt 0.0776 _refine_ls_wR_factor_ref 0.2667 _refine_ls_wR_factor_gt 0.2178 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 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 1.24987(8) 0.97170(7) 0.09867(4) 0.0310(3) Uani 1 1 d . A 2 S2 S 1.03082(8) 1.20789(8) 0.37450(5) 0.0348(3) Uani 1 1 d . A 2 O1 O 1.1664(2) 0.96271(19) 0.15260(11) 0.0278(6) Uani 1 1 d . A 2 O2 O 1.2715(3) 1.0543(2) 0.11073(15) 0.0471(8) Uani 1 1 d . A 2 O3 O 1.2044(2) 0.9754(2) 0.03836(12) 0.0372(7) Uani 1 1 d . A 2 O4 O 1.1802(2) 0.93052(19) 0.29690(12) 0.0313(6) Uani 1 1 d . A 2 O5 O 1.0054(2) 1.14141(19) 0.33036(11) 0.0287(6) Uani 1 1 d . A 2 O6 O 1.0352(3) 1.1665(2) 0.43874(13) 0.0450(8) Uani 1 1 d . A 2 O7 O 1.1272(3) 1.2167(3) 0.34821(15) 0.0526(9) Uani 1 1 d . A 2 O8 O 0.9652(2) 1.1597(2) 0.18415(12) 0.0323(6) Uani 1 1 d . A 2 N1 N 1.6293(4) 0.5249(3) 0.1113(2) 0.0659(13) Uani 1 1 d . A 2 N2 N 0.5346(5) 1.5580(5) 0.3482(3) 0.100(2) Uani 1 1 d . A 2 C1 C 1.1011(3) 0.9095(3) 0.14421(16) 0.0268(8) Uani 1 1 d . A 2 C2 C 1.0057(3) 0.9542(3) 0.10465(16) 0.0278(8) Uani 1 1 d . A 2 C3 C 0.9529(3) 0.8948(3) 0.09128(18) 0.0338(9) Uani 1 1 d . A 2 H3 H 0.8899 0.9230 0.0629 0.041 Uiso 1 1 calc R A 2 C4 C 0.9884(3) 0.7959(3) 0.11769(18) 0.0361(10) Uani 1 1 d . A 2 C5 C 1.0772(3) 0.7586(3) 0.16199(18) 0.0345(9) Uani 1 1 d . A 2 H5 H 1.0997 0.6928 0.1831 0.041 Uiso 1 1 calc R A 2 C6 C 1.1339(3) 0.8137(3) 0.17647(17) 0.0306(9) Uani 1 1 d . A 2 C7 C 1.2262(3) 0.7692(3) 0.22808(18) 0.0334(9) Uani 1 1 d . A 2 H7A H 1.2728 0.7000 0.2232 0.040 Uiso 1 1 calc R A 2 H7B H 1.2737 0.8065 0.2237 0.040 Uiso 1 1 calc R A 2 C8 C 1.1537(3) 0.8537(3) 0.32474(16) 0.0264(8) Uani 1 1 d . A 2 C9 C 1.1765(3) 0.7728(3) 0.29355(17) 0.0289(9) Uani 1 1 d . A 2 C10 C 1.1468(4) 0.6975(3) 0.32212(18) 0.0364(10) Uani 1 1 d . A 2 H10 H 1.1620 0.6420 0.3011 0.044 Uiso 1 1 calc R A 2 C11 C 1.0958(4) 0.6999(3) 0.38014(19) 0.0397(10) Uani 1 1 d . A 2 C12 C 1.0733(4) 0.7828(3) 0.40948(18) 0.0363(10) Uani 1 1 d . A 2 H12 H 1.0380 0.7867 0.4489 0.044 Uiso 1 1 calc R A 2 C13 C 1.1011(3) 0.8602(3) 0.38269(17) 0.0295(9) Uani 1 1 d . A 2 C14 C 1.0692(3) 0.9518(3) 0.41420(17) 0.0294(8) Uani 1 1 d . A 2 H14A H 1.0772 0.9327 0.4608 0.035 Uiso 1 1 calc R A 2 H14B H 1.1195 0.9849 0.4012 0.035 Uiso 1 1 calc R A 2 C15 C 0.9227(3) 1.1060(3) 0.34990(16) 0.0268(8) Uani 1 1 d . A 2 C16 C 0.9507(3) 1.0223(3) 0.39561(16) 0.0293(9) Uani 1 1 d . A 2 C17 C 0.8639(3) 1.0008(3) 0.42145(17) 0.0328(9) Uani 1 1 d . A 2 H17 H 0.8806 0.9457 0.4539 0.039 Uiso 1 1 calc R A 2 C18 C 0.7530(3) 1.0570(3) 0.40180(18) 0.0362(10) Uani 1 1 d . A 2 C19 C 0.7325(3) 1.1316(3) 0.35074(18) 0.0365(10) Uani 1 1 d . A 2 H19 H 0.6588 1.1664 0.3337 0.044 Uiso 1 1 calc R A 2 C20 C 0.8155(3) 1.1577(3) 0.32336(17) 0.0313(9) Uani 1 1 d . A 2 C21 C 0.7865(3) 1.2383(3) 0.26604(17) 0.0327(9) Uani 1 1 d . A 2 H21A H 0.8455 1.2633 0.2607 0.039 Uiso 1 1 calc R A 2 H21B H 0.7164 1.2938 0.2729 0.039 Uiso 1 1 calc R A 2 C22 C 0.8640(3) 1.1590(3) 0.16835(17) 0.0284(8) Uani 1 1 d . A 2 C23 C 0.7739(3) 1.1981(3) 0.20643(17) 0.0301(9) Uani 1 1 d . A 2 C24 C 0.6736(3) 1.1977(3) 0.18966(18) 0.0341(9) Uani 1 1 d . A 2 H24 H 0.6122 1.2247 0.2153 0.041 Uiso 1 1 calc R A 2 C25 C 0.6592(3) 1.1589(3) 0.13648(18) 0.0346(9) Uani 1 1 d . A 2 C26 C 0.7514(3) 1.1184(3) 0.10088(17) 0.0330(9) Uani 1 1 d . A 2 H26 H 0.7442 1.0907 0.0648 0.040 Uiso 1 1 calc R A 2 C27 C 0.8545(3) 1.1169(3) 0.11602(17) 0.0289(9) Uani 1 1 d . A 2 C28 C 0.9556(3) 1.0636(3) 0.07888(17) 0.0295(9) Uani 1 1 d . A 2 H28A H 0.9337 1.0732 0.0335 0.035 Uiso 1 1 calc R A 2 H28B H 1.0113 1.0915 0.0824 0.035 Uiso 1 1 calc R A 2 C29 C 0.9365(4) 0.7292(4) 0.0972(2) 0.0468(11) Uani 1 1 d . A 2 C30 C 0.8260(7) 0.7874(5) 0.0614(4) 0.117(3) Uani 1 1 d . A 2 H30A H 0.7731 0.8286 0.0891 0.176 Uiso 1 1 calc R A 2 H30B H 0.7977 0.7417 0.0479 0.176 Uiso 1 1 calc R A 2 H30C H 0.8358 0.8293 0.0240 0.176 Uiso 1 1 calc R A 2 C31 C 1.0161(8) 0.6636(7) 0.0539(4) 0.127(4) Uani 1 1 d . A 2 H31A H 1.0194 0.7038 0.0139 0.191 Uiso 1 1 calc R A 2 H31B H 0.9903 0.6136 0.0452 0.191 Uiso 1 1 calc R A 2 H31C H 1.0901 0.6310 0.0746 0.191 Uiso 1 1 calc R A 2 C32 C 0.9180(6) 0.6639(5) 0.1547(3) 0.0723(18) Uani 1 1 d . A 2 H32A H 0.9892 0.6216 0.1768 0.108 Uiso 1 1 calc R A 2 H32B H 0.8840 0.6226 0.1405 0.108 Uiso 1 1 calc R A 2 H32C H 0.8690 0.7055 0.1837 0.108 Uiso 1 1 calc R A 2 C33 C 1.3736(3) 0.8655(3) 0.11755(19) 0.0371(10) Uani 1 1 d . A 2 C34 C 1.3906(3) 0.7739(3) 0.09922(18) 0.0349(9) Uani 1 1 d . A 2 C35 C 1.3090(4) 0.7550(4) 0.0665(2) 0.0427(11) Uani 1 1 d . A 2 H35 H 1.2389 0.8067 0.0541 0.051 Uiso 1 1 calc R A 2 C36 C 1.3325(4) 0.6635(4) 0.0534(3) 0.0544(13) Uani 1 1 d . A 2 H36 H 1.2768 0.6512 0.0334 0.065 Uiso 1 1 calc R A 2 C37 C 1.4376(4) 0.5852(4) 0.0686(3) 0.0618(14) Uani 1 1 d . A 2 H37 H 1.4513 0.5218 0.0584 0.074 Uiso 1 1 calc R A 2 C38 C 1.5198(4) 0.6000(4) 0.0977(2) 0.0512(12) Uani 1 1 d . A 2 C39 C 1.4962(4) 0.6932(3) 0.1150(2) 0.0418(11) Uani 1 1 d . A 2 C40 C 1.5765(4) 0.7094(4) 0.1515(2) 0.0534(13) Uani 1 1 d . A 2 H40 H 1.6463 0.6565 0.1631 0.064 Uiso 1 1 calc R A 2 C41 C 1.5549(4) 0.7972(4) 0.1695(2) 0.0558(13) Uani 1 1 d . A 2 H41 H 1.6083 0.8051 0.1946 0.067 Uiso 1 1 calc R A 2 C42 C 1.4538(4) 0.8773(4) 0.1515(2) 0.0471(11) Uani 1 1 d . A 2 H42 H 1.4406 0.9399 0.1628 0.056 Uiso 1 1 calc R A 2 C43 C 1.6380(6) 0.4249(4) 0.1173(5) 0.108(3) Uani 1 1 d . A 2 H43A H 1.5807 0.4175 0.1450 0.162 Uiso 1 1 calc R A 2 H43B H 1.7112 0.3795 0.1357 0.162 Uiso 1 1 calc R A 2 H43C H 1.6281 0.4096 0.0754 0.162 Uiso 1 1 calc R A 2 C44 C 1.7127(5) 0.5381(5) 0.0688(4) 0.086(2) Uani 1 1 d . A 2 H44A H 1.7044 0.5195 0.0277 0.129 Uiso 1 1 calc R A 2 H44B H 1.7868 0.4964 0.0874 0.129 Uiso 1 1 calc R A 2 H44C H 1.7025 0.6074 0.0628 0.129 Uiso 1 1 calc R A 2 C45 C 1.0659(4) 0.6150(3) 0.4111(2) 0.0520(13) Uani 1 1 d D A 2 C46 C 1.0016(9) 0.5899(8) 0.3626(4) 0.083(3) Uani 0.710(6) 1 d PD A 1 H46A H 0.9398 0.6501 0.3436 0.124 Uiso 0.710(6) 1 calc PR A 1 H46B H 0.9728 0.5428 0.3838 0.124 Uiso 0.710(6) 1 calc PR A 1 H46C H 1.0510 0.5606 0.3293 0.124 Uiso 0.710(6) 1 calc PR A 1 C47 C 1.1746(7) 0.5272(6) 0.4345(5) 0.085(3) Uani 0.710(6) 1 d PD A 1 H47A H 1.2206 0.5063 0.3983 0.127 Uiso 0.710(6) 1 calc PR A 1 H47B H 1.1582 0.4724 0.4561 0.127 Uiso 0.710(6) 1 calc PR A 1 H47C H 1.2145 0.5470 0.4642 0.127 Uiso 0.710(6) 1 calc PR A 1 C48 C 0.9925(9) 0.6423(7) 0.4681(4) 0.084(3) Uani 0.710(6) 1 d PD A 1 H48A H 1.0303 0.6614 0.4992 0.126 Uiso 0.710(6) 1 calc PR A 1 H48B H 0.9780 0.5853 0.4876 0.126 Uiso 0.710(6) 1 calc PR A 1 H48C H 0.9222 0.6975 0.4537 0.126 Uiso 0.710(6) 1 calc PR A 1 C46A C 1.111(2) 0.5263(12) 0.3739(10) 0.083(3) Uani 0.290(6) 1 d PD A 2 H46D H 1.0824 0.4772 0.3913 0.124 Uiso 0.290(6) 1 calc PR A 2 H46E H 1.1922 0.4964 0.3777 0.124 Uiso 0.290(6) 1 calc PR A 2 H46F H 1.0875 0.5491 0.3291 0.124 Uiso 0.290(6) 1 calc PR A 2 C47A C 1.122(2) 0.5755(17) 0.4776(7) 0.085(3) Uani 0.290(6) 1 d PD A 2 H47D H 1.0907 0.6262 0.5051 0.127 Uiso 0.290(6) 1 calc PR A 2 H47E H 1.2020 0.5587 0.4745 0.127 Uiso 0.290(6) 1 calc PR A 2 H47F H 1.1106 0.5165 0.4954 0.127 Uiso 0.290(6) 1 calc PR A 2 C48A C 0.9399(9) 0.6522(13) 0.4130(10) 0.084(3) Uani 0.290(6) 1 d PD A 2 H48D H 0.9202 0.6009 0.4370 0.126 Uiso 0.290(6) 1 calc PR A 2 H48E H 0.9082 0.6682 0.3697 0.126 Uiso 0.290(6) 1 calc PR A 2 H48F H 0.9107 0.7114 0.4336 0.126 Uiso 0.290(6) 1 calc PR A 2 C49 C 1.2902(4) 0.9168(4) 0.3150(2) 0.0430(11) Uani 1 1 d . . . H49A H 1.3449 0.8584 0.2986 0.052 Uiso 1 1 calc R A 2 H49B H 1.2992 0.9049 0.3619 0.052 Uiso 1 1 calc R A 2 C50 C 1.3107(5) 1.0053(4) 0.2893(3) 0.0606(14) Uani 1 1 d . A . H50A H 1.2555 1.0637 0.3055 0.073 Uiso 1 1 calc R . . H50B H 1.3019 1.0169 0.2425 0.073 Uiso 1 1 calc R . . C51 C 1.4258(6) 0.9922(7) 0.3083(3) 0.101(3) Uani 1 1 d . . . H51A H 1.4351 0.9792 0.3547 0.151 Uiso 1 1 calc R A . H51B H 1.4365 1.0524 0.2922 0.151 Uiso 1 1 calc R . . H51C H 1.4805 0.9366 0.2904 0.151 Uiso 1 1 calc R . . C52 C 0.6611(4) 1.0341(4) 0.4364(2) 0.0451(11) Uani 1 1 d . . . C53 C 0.6759(5) 0.9302(5) 0.4301(3) 0.0672(16) Uani 1 1 d . A . H53A H 0.6760 0.9235 0.3851 0.101 Uiso 1 1 calc R . . H53B H 0.6149 0.9168 0.4502 0.101 Uiso 1 1 calc R . . H53C H 0.7463 0.8830 0.4509 0.101 Uiso 1 1 calc R . . C54 C 0.6688(4) 1.0425(5) 0.5068(2) 0.0598(15) Uani 1 1 d . A . H54A H 0.7387 0.9916 0.5260 0.090 Uiso 1 1 calc R . . H54B H 0.6067 1.0336 0.5286 0.090 Uiso 1 1 calc R . . H54C H 0.6661 1.1078 0.5107 0.090 Uiso 1 1 calc R . . C55 C 0.5463(4) 1.1075(5) 0.4101(3) 0.0645(15) Uani 1 1 d . A . H55A H 0.5368 1.1744 0.4149 0.097 Uiso 1 1 calc R . . H55B H 0.4895 1.0914 0.4334 0.097 Uiso 1 1 calc R . . H55C H 0.5391 1.1037 0.3650 0.097 Uiso 1 1 calc R . . C56 C 0.9202(4) 1.3257(4) 0.3541(2) 0.0476(11) Uani 1 1 d . . . C57 C 0.8171(4) 1.3508(4) 0.3817(2) 0.0519(12) Uani 1 1 d . A . C58 C 0.7920(4) 1.2894(4) 0.4331(2) 0.0509(12) Uani 1 1 d . . . H58 H 0.8466 1.2268 0.4504 0.061 Uiso 1 1 calc R A . C59 C 0.6880(5) 1.3234(4) 0.4563(2) 0.0646(15) Uani 1 1 d . A . H59 H 0.6737 1.2860 0.4926 0.077 Uiso 1 1 calc R . . C60 C 0.6020(6) 1.4104(5) 0.4292(3) 0.084(2) Uani 1 1 d . . . H60 H 0.5301 1.4291 0.4456 0.101 Uiso 1 1 calc R A . C61 C 0.6210(5) 1.4681(5) 0.3796(3) 0.0797(18) Uani 1 1 d . A . C62 C 0.7308(4) 1.4447(4) 0.3580(3) 0.0663(16) Uani 1 1 d . . . C63 C 0.7569(5) 1.5073(4) 0.3092(3) 0.0717(17) Uani 1 1 d . A . H63 H 0.6998 1.5688 0.2925 0.086 Uiso 1 1 calc R . . C64 C 0.8596(5) 1.4830(4) 0.2856(2) 0.0611(14) Uani 1 1 d . . . H64 H 0.8755 1.5280 0.2550 0.073 Uiso 1 1 calc R A . C65 C 0.9401(5) 1.3904(4) 0.3075(2) 0.0530(13) Uani 1 1 d . A . H65 H 1.0112 1.3709 0.2899 0.064 Uiso 1 1 calc R . . C66 C 0.5005(7) 1.5478(7) 0.2808(4) 0.121(3) Uani 1 1 d . . . H66A H 0.5638 1.5351 0.2533 0.182 Uiso 1 1 calc R A 2 H66B H 0.4391 1.6091 0.2626 0.182 Uiso 1 1 calc R A 2 H66C H 0.4772 1.4930 0.2841 0.182 Uiso 1 1 calc R A 2 C67 C 0.4371(6) 1.6014(6) 0.3864(4) 0.113(3) Uani 1 1 d . . . H67A H 0.3980 1.5575 0.3933 0.169 Uiso 1 1 calc R A 2 H67B H 0.3874 1.6657 0.3639 0.169 Uiso 1 1 calc R A 2 H67C H 0.4612 1.6097 0.4274 0.169 Uiso 1 1 calc R A 2 C68 C 0.5442(3) 1.1636(3) 0.11861(19) 0.0432(11) Uani 1 1 d D . . C69 C 0.4931(6) 1.1285(7) 0.1765(3) 0.060(2) Uani 0.842(8) 1 d PD A 1 H69A H 0.4750 1.1759 0.2064 0.091 Uiso 0.842(8) 1 calc PR A 1 H69B H 0.5459 1.0639 0.1970 0.091 Uiso 0.842(8) 1 calc PR A 1 H69C H 0.4255 1.1230 0.1634 0.091 Uiso 0.842(8) 1 calc PR A 1 C70 C 0.4695(5) 1.2705(5) 0.0916(5) 0.083(3) Uani 0.842(8) 1 d PD A 1 H70A H 0.3974 1.2740 0.0781 0.125 Uiso 0.842(8) 1 calc PR A 1 H70B H 0.5041 1.2932 0.0551 0.125 Uiso 0.842(8) 1 calc PR A 1 H70C H 0.4592 1.3126 0.1243 0.125 Uiso 0.842(8) 1 calc PR A 1 C71 C 0.5519(5) 1.0977(6) 0.0684(3) 0.070(2) Uani 0.842(8) 1 d PD A 1 H71A H 0.6049 1.0303 0.0834 0.105 Uiso 0.842(8) 1 calc PR A 1 H71B H 0.5767 1.1231 0.0288 0.105 Uiso 0.842(8) 1 calc PR A 1 H71C H 0.4789 1.0977 0.0610 0.105 Uiso 0.842(8) 1 calc PR A 1 C69A C 0.460(2) 1.202(3) 0.1699(14) 0.060(2) Uani 0.158(8) 1 d PD A 2 H69D H 0.3932 1.1912 0.1617 0.091 Uiso 0.158(8) 1 calc PR A 2 H69E H 0.4398 1.2727 0.1688 0.091 Uiso 0.158(8) 1 calc PR A 2 H69F H 0.4925 1.1667 0.2118 0.091 Uiso 0.158(8) 1 calc PR A 2 C70A C 0.504(3) 1.232(4) 0.0549(15) 0.083(3) Uani 0.158(8) 1 d PD A 2 H70D H 0.4264 1.2434 0.0459 0.125 Uiso 0.158(8) 1 calc PR A 2 H70E H 0.5496 1.2002 0.0211 0.125 Uiso 0.158(8) 1 calc PR A 2 H70F H 0.5088 1.2945 0.0570 0.125 Uiso 0.158(8) 1 calc PR A 2 C71A C 0.561(3) 1.0586(14) 0.109(2) 0.070(2) Uani 0.158(8) 1 d PD A 2 H71D H 0.5847 1.0146 0.1500 0.105 Uiso 0.158(8) 1 calc PR A 2 H71E H 0.6183 1.0350 0.0784 0.105 Uiso 0.158(8) 1 calc PR A 2 H71F H 0.4916 1.0593 0.0939 0.105 Uiso 0.158(8) 1 calc PR A 2 C72 C 0.9772(4) 1.2477(3) 0.1544(2) 0.0439(11) Uani 1 1 d . . . H72A H 0.9166 1.3065 0.1670 0.053 Uiso 1 1 calc R A 2 H72B H 0.9720 1.2524 0.1077 0.053 Uiso 1 1 calc R A 2 C73 C 1.0859(4) 1.2454(4) 0.1737(3) 0.0537(13) Uani 1 1 d . A . H73A H 1.1462 1.1862 0.1614 0.064 Uiso 1 1 calc R . . H73B H 1.0907 1.2406 0.2204 0.064 Uiso 1 1 calc R . . C74 C 1.1012(6) 1.3368(6) 0.1431(3) 0.091(2) Uani 1 1 d . . . H74A H 1.0998 1.3401 0.0969 0.136 Uiso 1 1 calc R A . H74B H 1.1724 1.3338 0.1576 0.136 Uiso 1 1 calc R . . H74C H 1.0412 1.3955 0.1548 0.136 Uiso 1 1 calc R . . N1G N 0.2342(12) 0.4871(8) 0.2302(6) 0.209(6) Uani 1 1 d . . . C1G C 0.2675(11) 0.4098(10) 0.2650(7) 0.153(4) Uani 1 1 d . . . C2G C 0.3085(10) 0.3157(7) 0.3112(7) 0.183(6) Uani 1 1 d . . . H2G1 H 0.3870 0.2959 0.3220 0.274 Uiso 1 1 calc R . . H2G2 H 0.2993 0.2638 0.2919 0.274 Uiso 1 1 calc R . . H2G3 H 0.2659 0.3259 0.3497 0.274 Uiso 1 1 calc R . . N1H N 0.7364(6) 0.8331(7) 0.2702(3) 0.125(3) Uani 1 1 d . . . C1H C 0.7945(5) 0.8732(5) 0.2652(3) 0.0649(16) Uani 1 1 d . . . C2H C 0.8674(4) 0.9223(4) 0.2599(2) 0.0498(12) Uani 1 1 d . . . H2H1 H 0.8743 0.9424 0.3007 0.075 Uiso 1 1 calc R . . H2H2 H 0.8377 0.9807 0.2273 0.075 Uiso 1 1 calc R . . H2H3 H 0.9403 0.8776 0.2480 0.075 Uiso 1 1 calc R . . N1I N 0.6006(14) 0.6813(11) 0.5170(6) 0.243(7) Uani 1 1 d D . . C1I C 0.6235(10) 0.6900(9) 0.4617(5) 0.154(4) Uani 1 1 d D . . C2I C 0.6342(15) 0.6878(14) 0.3945(6) 0.318(14) Uani 1 1 d D . . H2I1 H 0.6744 0.6196 0.3870 0.478 Uiso 1 1 calc R . . H2I2 H 0.6751 0.7273 0.3771 0.478 Uiso 1 1 calc R . . H2I3 H 0.5605 0.7151 0.3736 0.478 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 0.0296(5) 0.0366(6) 0.0244(5) -0.0010(4) 0.0048(4) -0.0121(4) S2 0.0359(6) 0.0378(6) 0.0322(6) -0.0045(4) -0.0040(4) -0.0163(5) O1 0.0294(14) 0.0355(15) 0.0193(13) -0.0029(10) 0.0023(10) -0.0145(12) O2 0.0512(19) 0.053(2) 0.0479(19) -0.0099(15) 0.0102(14) -0.0310(16) O3 0.0394(16) 0.0502(18) 0.0223(14) -0.0038(12) 0.0037(11) -0.0193(14) O4 0.0341(15) 0.0341(15) 0.0279(14) 0.0024(11) 0.0043(11) -0.0188(12) O5 0.0318(14) 0.0335(15) 0.0224(13) -0.0024(11) 0.0031(10) -0.0156(12) O6 0.0581(19) 0.057(2) 0.0255(15) -0.0074(13) -0.0005(13) -0.0288(16) O7 0.053(2) 0.072(2) 0.050(2) -0.0067(16) 0.0014(15) -0.0439(18) O8 0.0298(14) 0.0388(16) 0.0280(14) -0.0013(12) -0.0035(11) -0.0146(12) N1 0.047(3) 0.034(2) 0.100(4) 0.004(2) -0.013(2) -0.0032(19) N2 0.065(3) 0.102(5) 0.090(4) 0.018(3) -0.002(3) 0.000(3) C1 0.030(2) 0.036(2) 0.0172(18) -0.0050(15) 0.0040(14) -0.0164(17) C2 0.031(2) 0.038(2) 0.0150(17) -0.0038(15) 0.0049(14) -0.0158(17) C3 0.036(2) 0.046(3) 0.0219(19) -0.0012(17) -0.0020(16) -0.0205(19) C4 0.045(2) 0.047(3) 0.024(2) -0.0017(18) 0.0022(17) -0.028(2) C5 0.046(2) 0.035(2) 0.0222(19) 0.0038(16) 0.0013(17) -0.019(2) C6 0.032(2) 0.039(2) 0.0196(19) -0.0036(16) 0.0051(15) -0.0133(18) C7 0.034(2) 0.034(2) 0.027(2) -0.0006(16) 0.0023(16) -0.0096(18) C8 0.0260(19) 0.031(2) 0.0212(18) 0.0040(15) -0.0016(14) -0.0133(16) C9 0.030(2) 0.030(2) 0.0218(19) 0.0056(15) -0.0063(15) -0.0102(17) C10 0.049(3) 0.034(2) 0.028(2) 0.0021(17) -0.0048(18) -0.020(2) C11 0.058(3) 0.043(3) 0.026(2) 0.0062(18) -0.0020(18) -0.031(2) C12 0.051(3) 0.046(3) 0.0192(19) 0.0025(17) 0.0016(17) -0.029(2) C13 0.031(2) 0.037(2) 0.0224(19) 0.0026(16) -0.0048(15) -0.0188(18) C14 0.032(2) 0.037(2) 0.0216(19) 0.0036(16) -0.0015(15) -0.0193(18) C15 0.029(2) 0.035(2) 0.0176(18) -0.0039(15) 0.0046(14) -0.0155(17) C16 0.032(2) 0.045(2) 0.0153(18) -0.0048(16) 0.0022(14) -0.0212(18) C17 0.037(2) 0.048(3) 0.0202(19) -0.0027(17) 0.0030(16) -0.024(2) C18 0.038(2) 0.058(3) 0.021(2) -0.0062(18) 0.0050(16) -0.028(2) C19 0.029(2) 0.057(3) 0.025(2) -0.0097(19) -0.0001(16) -0.018(2) C20 0.033(2) 0.041(2) 0.0210(19) -0.0076(16) 0.0033(15) -0.0157(18) C21 0.034(2) 0.036(2) 0.026(2) -0.0044(16) -0.0003(16) -0.0118(18) C22 0.027(2) 0.032(2) 0.0234(19) 0.0059(15) -0.0040(15) -0.0123(17) C23 0.034(2) 0.032(2) 0.0212(19) 0.0035(15) -0.0042(15) -0.0120(17) C24 0.029(2) 0.043(2) 0.025(2) 0.0000(17) 0.0042(16) -0.0110(18) C25 0.031(2) 0.049(3) 0.023(2) 0.0006(17) -0.0015(16) -0.0172(19) C26 0.035(2) 0.047(3) 0.0177(18) -0.0034(16) 0.0007(15) -0.0184(19) C27 0.029(2) 0.036(2) 0.0182(18) 0.0037(15) -0.0027(14) -0.0121(17) C28 0.031(2) 0.038(2) 0.0191(18) 0.0000(15) -0.0003(15) -0.0143(17) C29 0.064(3) 0.057(3) 0.032(2) 0.001(2) -0.004(2) -0.039(3) C30 0.121(6) 0.089(5) 0.162(8) 0.039(5) -0.090(6) -0.078(5) C31 0.184(9) 0.181(9) 0.114(6) -0.106(6) 0.074(6) -0.149(8) C32 0.108(5) 0.081(4) 0.056(3) 0.011(3) -0.013(3) -0.072(4) C33 0.032(2) 0.048(3) 0.031(2) -0.0023(18) 0.0031(16) -0.0158(19) C34 0.042(2) 0.038(2) 0.025(2) -0.0031(17) 0.0084(17) -0.0176(19) C35 0.042(3) 0.052(3) 0.040(2) -0.013(2) 0.0065(19) -0.023(2) C36 0.043(3) 0.056(3) 0.074(4) -0.029(3) 0.006(2) -0.024(2) C37 0.051(3) 0.050(3) 0.088(4) -0.023(3) 0.010(3) -0.020(3) C38 0.044(3) 0.044(3) 0.060(3) 0.001(2) 0.000(2) -0.014(2) C39 0.039(2) 0.042(3) 0.039(2) 0.0053(19) 0.0037(18) -0.015(2) C40 0.038(3) 0.062(3) 0.051(3) 0.001(2) -0.007(2) -0.013(2) C41 0.044(3) 0.073(4) 0.052(3) -0.020(3) -0.004(2) -0.022(3) C42 0.035(2) 0.065(3) 0.047(3) -0.019(2) 0.0040(19) -0.023(2) C43 0.071(4) 0.039(3) 0.186(9) 0.007(4) -0.016(5) 0.001(3) C44 0.051(4) 0.065(4) 0.127(6) -0.017(4) 0.009(4) -0.008(3) C45 0.087(4) 0.049(3) 0.037(3) 0.000(2) 0.005(2) -0.048(3) C46 0.134(8) 0.098(7) 0.060(5) -0.007(5) 0.011(5) -0.093(7) C47 0.109(8) 0.054(5) 0.096(7) 0.026(4) -0.002(5) -0.051(5) C48 0.160(9) 0.085(6) 0.059(5) -0.020(4) 0.047(5) -0.102(7) C46A 0.134(8) 0.098(7) 0.060(5) -0.007(5) 0.011(5) -0.093(7) C47A 0.109(8) 0.054(5) 0.096(7) 0.026(4) -0.002(5) -0.051(5) C48A 0.160(9) 0.085(6) 0.059(5) -0.020(4) 0.047(5) -0.102(7) C49 0.043(3) 0.060(3) 0.035(2) -0.005(2) 0.0084(19) -0.031(2) C50 0.077(4) 0.076(4) 0.052(3) -0.019(3) 0.024(3) -0.054(3) C51 0.127(6) 0.191(8) 0.054(4) -0.021(4) 0.016(4) -0.136(6) C52 0.040(2) 0.078(3) 0.028(2) -0.006(2) 0.0058(18) -0.036(2) C53 0.057(3) 0.090(4) 0.072(4) -0.013(3) 0.021(3) -0.048(3) C54 0.053(3) 0.108(5) 0.035(3) -0.013(3) 0.018(2) -0.049(3) C55 0.042(3) 0.106(5) 0.050(3) -0.002(3) 0.005(2) -0.039(3) C56 0.050(3) 0.056(3) 0.040(3) -0.010(2) 0.000(2) -0.023(2) C57 0.053(3) 0.062(3) 0.035(3) -0.012(2) 0.002(2) -0.016(2) C58 0.069(3) 0.060(3) 0.029(2) -0.007(2) 0.010(2) -0.034(3) C59 0.073(4) 0.059(3) 0.043(3) 0.001(2) 0.018(3) -0.011(3) C60 0.074(4) 0.087(5) 0.067(4) 0.008(3) 0.020(3) -0.015(4) C61 0.062(4) 0.079(4) 0.076(4) 0.003(3) 0.003(3) -0.011(3) C62 0.053(3) 0.062(3) 0.058(3) 0.019(3) 0.009(2) -0.007(3) C63 0.073(4) 0.063(4) 0.058(3) 0.009(3) -0.001(3) -0.012(3) C64 0.063(3) 0.078(4) 0.046(3) -0.010(3) 0.010(2) -0.034(3) C65 0.072(3) 0.061(3) 0.039(3) -0.004(2) 0.004(2) -0.041(3) C66 0.082(5) 0.138(7) 0.112(7) 0.043(5) -0.033(5) -0.031(5) C67 0.070(5) 0.101(6) 0.120(7) 0.010(5) 0.018(4) 0.004(4) C68 0.031(2) 0.066(3) 0.034(2) -0.003(2) 0.0015(17) -0.023(2) C69 0.061(4) 0.103(6) 0.041(3) -0.011(4) 0.011(3) -0.058(5) C70 0.035(4) 0.081(6) 0.122(8) 0.018(5) -0.027(4) -0.022(4) C71 0.052(4) 0.136(7) 0.050(4) -0.038(4) 0.012(3) -0.059(4) C69A 0.061(4) 0.103(6) 0.041(3) -0.011(4) 0.011(3) -0.058(5) C70A 0.035(4) 0.081(6) 0.122(8) 0.018(5) -0.027(4) -0.022(4) C71A 0.052(4) 0.136(7) 0.050(4) -0.038(4) 0.012(3) -0.059(4) C72 0.048(3) 0.048(3) 0.040(3) -0.002(2) 0.000(2) -0.025(2) C73 0.048(3) 0.065(3) 0.062(3) -0.024(3) 0.012(2) -0.033(3) C74 0.108(5) 0.124(6) 0.088(5) -0.026(4) 0.024(4) -0.093(5) N1G 0.290(15) 0.106(7) 0.205(12) -0.029(8) -0.069(10) -0.047(9) C1G 0.174(11) 0.118(9) 0.178(12) -0.060(9) 0.028(9) -0.059(9) C2G 0.174(11) 0.071(6) 0.264(16) -0.023(8) 0.056(10) -0.014(7) N1H 0.129(6) 0.209(8) 0.099(5) -0.056(5) 0.023(4) -0.124(6) C1H 0.057(3) 0.109(5) 0.048(3) -0.027(3) 0.006(2) -0.049(3) C2H 0.053(3) 0.065(3) 0.035(2) -0.009(2) 0.005(2) -0.028(3) N1I 0.300(17) 0.214(13) 0.220(15) -0.044(11) 0.115(13) -0.111(12) C1I 0.134(9) 0.122(8) 0.214(15) -0.026(9) 0.029(9) -0.061(7) C2I 0.31(2) 0.33(2) 0.129(12) -0.017(13) 0.125(14) 0.051(18) _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 O3 1.417(3) . ? S1 O2 1.436(3) . ? S1 O1 1.603(3) . ? S1 C33 1.765(4) . ? S2 O6 1.411(3) . ? S2 O7 1.425(3) . ? S2 O5 1.598(3) . ? S2 C56 1.780(5) . ? O1 C1 1.420(4) . ? O4 C8 1.384(4) . ? O4 C49 1.437(5) . ? O5 C15 1.424(4) . ? O8 C22 1.391(4) . ? O8 C72 1.444(5) . ? N1 C38 1.434(6) . ? N1 C43 1.443(8) . ? N1 C44 1.466(8) . ? N2 C61 1.448(8) . ? N2 C67 1.475(9) . ? N2 C66 1.566(10) . ? C1 C6 1.394(5) . ? C1 C2 1.397(5) . ? C2 C3 1.394(6) . ? C2 C28 1.518(5) . ? C3 C4 1.393(6) . ? C3 H3 0.9500 . ? C4 C5 1.396(6) . ? C4 C29 1.535(6) . ? C5 C6 1.387(6) . ? C5 H5 0.9500 . ? C6 C7 1.528(5) . ? C7 C9 1.528(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.392(5) . ? C8 C13 1.400(5) . ? C9 C10 1.393(5) . ? C10 C11 1.393(6) . ? C10 H10 0.9500 . ? C11 C12 1.396(6) . ? C11 C45 1.535(6) . ? C12 C13 1.394(5) . ? C12 H12 0.9500 . ? C13 C14 1.519(6) . ? C14 C16 1.516(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.395(5) . ? C15 C20 1.397(5) . ? C16 C17 1.391(5) . ? C17 C18 1.401(6) . ? C17 H17 0.9500 . ? C18 C19 1.386(6) . ? C18 C52 1.534(6) . ? C19 C20 1.394(6) . ? C19 H19 0.9500 . ? C20 C21 1.522(5) . ? C21 C23 1.525(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C27 1.392(5) . ? C22 C23 1.397(5) . ? C23 C24 1.383(5) . ? C24 C25 1.398(6) . ? C24 H24 0.9500 . ? C25 C26 1.388(5) . ? C25 C68 1.546(6) . ? C26 C27 1.398(5) . ? C26 H26 0.9500 . ? C27 C28 1.525(5) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.518(8) . ? C29 C31 1.522(9) . ? C29 C32 1.533(7) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C42 1.380(6) . ? C33 C34 1.412(6) . ? C34 C39 1.436(6) . ? C34 C35 1.439(6) . ? C35 C36 1.349(6) . ? C35 H35 0.9500 . ? C36 C37 1.417(7) . ? C36 H36 0.9500 . ? C37 C38 1.371(7) . ? C37 H37 0.9500 . ? C38 C39 1.407(7) . ? C39 C40 1.447(7) . ? C40 C41 1.343(7) . ? C40 H40 0.9500 . ? C41 C42 1.403(7) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C48A 1.530(10) . ? C45 C46 1.533(7) . ? C45 C48 1.536(7) . ? C45 C47 1.536(7) . ? C45 C47A 1.539(10) . ? C45 C46A 1.550(10) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C46A H46D 0.9800 . ? C46A H46E 0.9800 . ? C46A H46F 0.9800 . ? C47A H47D 0.9800 . ? C47A H47E 0.9800 . ? C47A H47F 0.9800 . ? C48A H48D 0.9800 . ? C48A H48E 0.9800 . ? C48A H48F 0.9800 . ? C49 C50 1.484(7) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.510(8) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.516(8) . ? C52 C55 1.530(7) . ? C52 C54 1.534(6) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C65 1.382(7) . ? C56 C57 1.398(7) . ? C57 C62 1.436(7) . ? C57 C58 1.446(7) . ? C58 C59 1.367(7) . ? C58 H58 0.9500 . ? C59 C60 1.393(8) . ? C59 H59 0.9500 . ? C60 C61 1.350(9) . ? C60 H60 0.9500 . ? C61 C62 1.430(8) . ? C62 C63 1.427(8) . ? C63 C64 1.361(8) . ? C63 H63 0.9500 . ? C64 C65 1.385(8) . ? C64 H64 0.9500 . ? C65 H65 0.9500 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 C69 1.520(6) . ? C68 C70 1.536(7) . ? C68 C71 1.536(6) . ? C68 C70A 1.537(10) . ? C68 C71A 1.539(10) . ? C68 C69A 1.544(10) . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C69A H69D 0.9800 . ? C69A H69E 0.9800 . ? C69A H69F 0.9800 . ? C70A H70D 0.9800 . ? C70A H70E 0.9800 . ? C70A H70F 0.9800 . ? C71A H71D 0.9801 . ? C71A H71E 0.9801 . ? C71A H71F 0.9700 . ? C72 C73 1.489(6) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.515(8) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? N1G C1G 1.200(15) . ? C1G C2G 1.500(17) . ? C2G H2G1 0.9800 . ? C2G H2G2 0.9800 . ? C2G H2G3 0.9800 . ? N1H C1H 1.145(8) . ? C1H C2H 1.421(7) . ? C2H H2H1 0.9800 . ? C2H H2H2 0.9800 . ? C2H H2H3 0.9800 . ? N1I C1I 1.212(17) . ? C1I C2I 1.441(17) . ? C2I H2I1 0.9800 . ? C2I H2I2 0.9800 . ? C2I H2I3 0.9800 . ? 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 O3 S1 O2 118.51(19) . . ? O3 S1 O1 109.71(15) . . ? O2 S1 O1 103.66(16) . . ? O3 S1 C33 111.52(19) . . ? O2 S1 C33 107.0(2) . . ? O1 S1 C33 105.37(16) . . ? O6 S2 O7 118.9(2) . . ? O6 S2 O5 109.66(16) . . ? O7 S2 O5 103.16(17) . . ? O6 S2 C56 114.0(2) . . ? O7 S2 C56 106.1(2) . . ? O5 S2 C56 103.38(18) . . ? C1 O1 S1 119.0(2) . . ? C8 O4 C49 112.2(3) . . ? C15 O5 S2 117.4(2) . . ? C22 O8 C72 112.5(3) . . ? C38 N1 C43 115.4(5) . . ? C38 N1 C44 114.1(4) . . ? C43 N1 C44 110.4(5) . . ? C61 N2 C67 114.9(6) . . ? C61 N2 C66 112.6(6) . . ? C67 N2 C66 111.6(6) . . ? C6 C1 C2 121.9(4) . . ? C6 C1 O1 118.6(3) . . ? C2 C1 O1 119.5(3) . . ? C3 C2 C1 117.2(4) . . ? C3 C2 C28 119.7(3) . . ? C1 C2 C28 123.1(3) . . ? C4 C3 C2 122.9(4) . . ? C4 C3 H3 118.6 . . ? C2 C3 H3 118.6 . . ? C3 C4 C5 116.9(4) . . ? C3 C4 C29 121.9(4) . . ? C5 C4 C29 121.1(4) . . ? C6 C5 C4 122.6(4) . . ? C6 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? C5 C6 C1 117.8(3) . . ? C5 C6 C7 119.3(4) . . ? C1 C6 C7 122.8(4) . . ? C9 C7 C6 110.0(3) . . ? C9 C7 H7A 109.6 . . ? C6 C7 H7A 109.7 . . ? C9 C7 H7B 109.7 . . ? C6 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? O4 C8 C9 119.3(3) . . ? O4 C8 C13 119.4(3) . . ? C9 C8 C13 121.2(3) . . ? C8 C9 C10 118.0(4) . . ? C8 C9 C7 121.1(3) . . ? C10 C9 C7 120.7(4) . . ? C11 C10 C9 122.8(4) . . ? C11 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? C10 C11 C12 117.3(4) . . ? C10 C11 C45 121.7(4) . . ? C12 C11 C45 121.1(4) . . ? C13 C12 C11 122.0(4) . . ? C13 C12 H12 119.0 . . ? C11 C12 H12 119.0 . . ? C12 C13 C8 118.6(4) . . ? C12 C13 C14 120.3(3) . . ? C8 C13 C14 121.0(3) . . ? C16 C14 C13 110.4(3) . . ? C16 C14 H14A 109.6 . . ? C13 C14 H14A 109.6 . . ? C16 C14 H14B 109.6 . . ? C13 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? C16 C15 C20 122.3(3) . . ? C16 C15 O5 119.1(3) . . ? C20 C15 O5 118.6(3) . . ? C17 C16 C15 116.9(4) . . ? C17 C16 C14 119.8(3) . . ? C15 C16 C14 123.2(3) . . ? C16 C17 C18 122.9(4) . . ? C16 C17 H17 118.5 . . ? C18 C17 H17 118.5 . . ? C19 C18 C17 116.9(4) . . ? C19 C18 C52 123.2(4) . . ? C17 C18 C52 119.9(4) . . ? C18 C19 C20 122.7(4) . . ? C18 C19 H19 118.7 . . ? C20 C19 H19 118.7 . . ? C19 C20 C15 117.3(4) . . ? C19 C20 C21 119.3(3) . . ? C15 C20 C21 123.4(3) . . ? C20 C21 C23 110.2(3) . . ? C20 C21 H21A 109.6 . . ? C23 C21 H21A 109.6 . . ? C20 C21 H21B 109.6 . . ? C23 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? O8 C22 C27 119.7(3) . . ? O8 C22 C23 119.3(3) . . ? C27 C22 C23 120.9(3) . . ? C24 C23 C22 118.6(4) . . ? C24 C23 C21 120.7(3) . . ? C22 C23 C21 120.8(3) . . ? C23 C24 C25 122.6(4) . . ? C23 C24 H24 118.7 . . ? C25 C24 H24 118.7 . . ? C26 C25 C24 117.0(4) . . ? C26 C25 C68 122.5(4) . . ? C24 C25 C68 120.5(3) . . ? C25 C26 C27 122.5(4) . . ? C25 C26 H26 118.7 . . ? C27 C26 H26 118.8 . . ? C22 C27 C26 118.4(3) . . ? C22 C27 C28 121.1(3) . . ? C26 C27 C28 120.4(3) . . ? C2 C28 C27 110.1(3) . . ? C2 C28 H28A 109.6 . . ? C27 C28 H28A 109.6 . . ? C2 C28 H28B 109.6 . . ? C27 C28 H28B 109.6 . . ? H28A C28 H28B 108.2 . . ? C30 C29 C31 108.5(6) . . ? C30 C29 C32 107.9(5) . . ? C31 C29 C32 108.9(6) . . ? C30 C29 C4 112.6(4) . . ? C31 C29 C4 107.9(4) . . ? C32 C29 C4 111.0(4) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C42 C33 C34 121.6(4) . . ? C42 C33 S1 115.8(4) . . ? C34 C33 S1 122.7(3) . . ? C33 C34 C39 118.0(4) . . ? C33 C34 C35 124.6(4) . . ? C39 C34 C35 117.3(4) . . ? C36 C35 C34 119.8(4) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C37 121.9(5) . . ? C35 C36 H36 119.0 . . ? C37 C36 H36 119.0 . . ? C38 C37 C36 120.7(5) . . ? C38 C37 H37 119.6 . . ? C36 C37 H37 119.6 . . ? C37 C38 C39 118.7(4) . . ? C37 C38 N1 123.1(5) . . ? C39 C38 N1 118.2(4) . . ? C38 C39 C34 121.3(4) . . ? C38 C39 C40 120.7(4) . . ? C34 C39 C40 118.0(4) . . ? C41 C40 C39 121.6(4) . . ? C41 C40 H40 119.2 . . ? C39 C40 H40 119.2 . . ? C40 C41 C42 120.3(5) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C33 C42 C41 120.4(5) . . ? C33 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? N1 C43 H43A 109.5 . . ? N1 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N1 C43 H43C 109.4 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N1 C44 H44A 109.5 . . ? N1 C44 H44B 109.4 . . ? H44A C44 H44B 109.5 . . ? N1 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C48A C45 C46 59.9(9) . . ? C48A C45 C11 108.8(7) . . ? C46 C45 C11 109.4(4) . . ? C48A C45 C48 51.7(8) . . ? C46 C45 C48 107.6(6) . . ? C11 C45 C48 111.9(4) . . ? C48A C45 C47 143.3(8) . . ? C46 C45 C47 112.0(6) . . ? C11 C45 C47 107.5(4) . . ? C48 C45 C47 108.5(6) . . ? C48A C45 C47A 112.3(13) . . ? C46 C45 C47A 140.8(9) . . ? C11 C45 C47A 109.3(8) . . ? C48 C45 C47A 62.8(11) . . ? C47 C45 C47A 48.7(11) . . ? C48A C45 C46A 109.4(12) . . ? C46 C45 C46A 53.1(10) . . ? C11 C45 C46A 111.6(8) . . ? C48 C45 C46A 136.3(8) . . ? C47 C45 C46A 60.9(11) . . ? C47A C45 C46A 105.5(14) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? C45 C46A H46D 109.5 . . ? C45 C46A H46E 109.4 . . ? H46D C46A H46E 109.5 . . ? C45 C46A H46F 109.5 . . ? H46D C46A H46F 109.5 . . ? H46E C46A H46F 109.5 . . ? C45 C47A H47D 109.4 . . ? C45 C47A H47E 109.5 . . ? H47D C47A H47E 109.5 . . ? C45 C47A H47F 109.4 . . ? H47D C47A H47F 109.5 . . ? H47E C47A H47F 109.5 . . ? C45 C48A H48D 109.5 . . ? C45 C48A H48E 109.5 . . ? H48D C48A H48E 109.5 . . ? C45 C48A H48F 109.4 . . ? H48D C48A H48F 109.5 . . ? H48E C48A H48F 109.5 . . ? O4 C49 C50 110.2(4) . . ? O4 C49 H49A 109.6 . . ? C50 C49 H49A 109.6 . . ? O4 C49 H49B 109.6 . . ? C50 C49 H49B 109.6 . . ? H49A C49 H49B 108.1 . . ? C49 C50 C51 110.9(5) . . ? C49 C50 H50A 109.5 . . ? C51 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? C51 C50 H50B 109.5 . . ? H50A C50 H50B 108.0 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.4 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C53 C52 C55 109.9(4) . . ? C53 C52 C54 109.4(4) . . ? C55 C52 C54 107.7(4) . . ? C53 C52 C18 109.5(4) . . ? C55 C52 C18 111.4(4) . . ? C54 C52 C18 108.9(4) . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C52 C55 H55A 109.5 . . ? C52 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C52 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C65 C56 C57 121.3(5) . . ? C65 C56 S2 116.3(4) . . ? C57 C56 S2 122.4(4) . . ? C56 C57 C62 117.8(5) . . ? C56 C57 C58 124.5(5) . . ? C62 C57 C58 117.7(4) . . ? C59 C58 C57 118.6(5) . . ? C59 C58 H58 120.7 . . ? C57 C58 H58 120.7 . . ? C58 C59 C60 123.2(5) . . ? C58 C59 H59 118.4 . . ? C60 C59 H59 118.4 . . ? C61 C60 C59 119.9(6) . . ? C61 C60 H60 120.0 . . ? C59 C60 H60 120.0 . . ? C60 C61 C62 120.3(6) . . ? C60 C61 N2 122.6(6) . . ? C62 C61 N2 117.0(5) . . ? C63 C62 C61 122.6(5) . . ? C63 C62 C57 117.8(5) . . ? C61 C62 C57 119.4(5) . . ? C64 C63 C62 123.1(5) . . ? C64 C63 H63 118.4 . . ? C62 C63 H63 118.4 . . ? C63 C64 C65 117.8(5) . . ? C63 C64 H64 121.1 . . ? C65 C64 H64 121.1 . . ? C56 C65 C64 122.0(5) . . ? C56 C65 H65 119.0 . . ? C64 C65 H65 119.0 . . ? N2 C66 H66A 109.5 . . ? N2 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? N2 C66 H66C 109.4 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N2 C67 H67A 109.4 . . ? N2 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? N2 C67 H67C 109.6 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C69 C68 C70 110.0(5) . . ? C69 C68 C71 107.6(5) . . ? C70 C68 C71 108.6(6) . . ? C69 C68 C70A 137.4(16) . . ? C71 C68 C70A 73(2) . . ? C69 C68 C71A 76.4(15) . . ? C70 C68 C71A 138.6(15) . . ? C70A C68 C71A 108(2) . . ? C70 C68 C69A 74.2(17) . . ? C71 C68 C69A 132.7(14) . . ? C70A C68 C69A 110(2) . . ? C71A C68 C69A 112(2) . . ? C69 C68 C25 110.5(4) . . ? C70 C68 C25 108.6(4) . . ? C71 C68 C25 111.6(4) . . ? C70A C68 C25 108.4(15) . . ? C71A C68 C25 106.7(13) . . ? C69A C68 C25 111.7(13) . . ? C68 C69 H69A 109.4 . . ? C68 C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? C68 C70 H70A 109.5 . . ? C68 C70 H70B 109.5 . . ? C68 C70 H70C 109.5 . . ? C68 C71 H71A 109.5 . . ? C68 C71 H71B 109.4 . . ? C68 C71 H71C 109.5 . . ? C68 C69A H69D 109.5 . . ? C68 C69A H69E 109.5 . . ? H69D C69A H69E 109.5 . . ? C68 C69A H69F 109.4 . . ? H69D C69A H69F 109.5 . . ? H69E C69A H69F 109.5 . . ? C68 C70A H70D 109.4 . . ? C68 C70A H70E 109.3 . . ? H70D C70A H70E 109.5 . . ? C68 C70A H70F 109.7 . . ? H70D C70A H70F 109.5 . . ? H70E C70A H70F 109.5 . . ? C68 C71A H71D 109.5 . . ? C68 C71A H71E 109.5 . . ? H71D C71A H71E 109.5 . . ? C68 C71A H71F 109.5 . . ? H71D C71A H71F 109.5 . . ? H71E C71A H71F 109.5 . . ? O8 C72 C73 110.2(4) . . ? O8 C72 H72A 109.6 . . ? C73 C72 H72A 109.6 . . ? O8 C72 H72B 109.6 . . ? C73 C72 H72B 109.6 . . ? H72A C72 H72B 108.1 . . ? C72 C73 C74 111.5(5) . . ? C72 C73 H73A 109.3 . . ? C74 C73 H73A 109.3 . . ? C72 C73 H73B 109.3 . . ? C74 C73 H73B 109.3 . . ? H73A C73 H73B 108.0 . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? N1G C1G C2G 177.3(13) . . ? C1G C2G H2G1 109.5 . . ? C1G C2G H2G2 109.5 . . ? H2G1 C2G H2G2 109.5 . . ? C1G C2G H2G3 109.4 . . ? H2G1 C2G H2G3 109.5 . . ? H2G2 C2G H2G3 109.5 . . ? N1H C1H C2H 179.1(7) . . ? C1H C2H H2H1 109.5 . . ? C1H C2H H2H2 109.5 . . ? H2H1 C2H H2H2 109.5 . . ? C1H C2H H2H3 109.5 . . ? H2H1 C2H H2H3 109.5 . . ? H2H2 C2H H2H3 109.5 . . ? N1I C1I C2I 166.2(17) . . ? C1I C2I H2I1 110.0 . . ? C1I C2I H2I2 110.0 . . ? H2I1 C2I H2I2 109.0 . . ? C1I C2I H2I3 110.0 . . ? H2I1 C2I H2I3 109.0 . . ? H2I2 C2I H2I3 109.0 . . ? 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 O3 S1 O1 C1 33.3(3) . . . . ? O2 S1 O1 C1 160.9(3) . . . . ? C33 S1 O1 C1 -86.8(3) . . . . ? O6 S2 O5 C15 43.0(3) . . . . ? O7 S2 O5 C15 170.7(3) . . . . ? C56 S2 O5 C15 -78.9(3) . . . . ? S1 O1 C1 C6 101.4(3) . . . . ? S1 O1 C1 C2 -79.2(4) . . . . ? C6 C1 C2 C3 -9.0(5) . . . . ? O1 C1 C2 C3 171.6(3) . . . . ? C6 C1 C2 C28 168.0(3) . . . . ? O1 C1 C2 C28 -11.4(5) . . . . ? C1 C2 C3 C4 2.9(6) . . . . ? C28 C2 C3 C4 -174.3(3) . . . . ? C2 C3 C4 C5 3.7(6) . . . . ? C2 C3 C4 C29 -173.7(4) . . . . ? C3 C4 C5 C6 -4.6(6) . . . . ? C29 C4 C5 C6 172.8(4) . . . . ? C4 C5 C6 C1 -1.2(6) . . . . ? C4 C5 C6 C7 176.8(4) . . . . ? C2 C1 C6 C5 8.2(5) . . . . ? O1 C1 C6 C5 -172.4(3) . . . . ? C2 C1 C6 C7 -169.6(3) . . . . ? O1 C1 C6 C7 9.7(5) . . . . ? C5 C6 C7 C9 -77.3(5) . . . . ? C1 C6 C7 C9 100.5(4) . . . . ? C49 O4 C8 C9 -90.1(4) . . . . ? C49 O4 C8 C13 92.0(4) . . . . ? O4 C8 C9 C10 -178.7(3) . . . . ? C13 C8 C9 C10 -0.9(5) . . . . ? O4 C8 C9 C7 -2.3(5) . . . . ? C13 C8 C9 C7 175.5(3) . . . . ? C6 C7 C9 C8 -90.0(4) . . . . ? C6 C7 C9 C10 86.3(4) . . . . ? C8 C9 C10 C11 -0.1(6) . . . . ? C7 C9 C10 C11 -176.5(4) . . . . ? C9 C10 C11 C12 0.8(6) . . . . ? C9 C10 C11 C45 -178.9(4) . . . . ? C10 C11 C12 C13 -0.5(6) . . . . ? C45 C11 C12 C13 179.1(4) . . . . ? C11 C12 C13 C8 -0.3(6) . . . . ? C11 C12 C13 C14 176.4(4) . . . . ? O4 C8 C13 C12 178.9(3) . . . . ? C9 C8 C13 C12 1.1(5) . . . . ? O4 C8 C13 C14 2.2(5) . . . . ? C9 C8 C13 C14 -175.6(3) . . . . ? C12 C13 C14 C16 -83.0(4) . . . . ? C8 C13 C14 C16 93.7(4) . . . . ? S2 O5 C15 C16 -81.5(4) . . . . ? S2 O5 C15 C20 97.2(3) . . . . ? C20 C15 C16 C17 -10.0(6) . . . . ? O5 C15 C16 C17 168.7(3) . . . . ? C20 C15 C16 C14 165.6(3) . . . . ? O5 C15 C16 C14 -15.7(5) . . . . ? C13 C14 C16 C17 73.9(4) . . . . ? C13 C14 C16 C15 -101.5(4) . . . . ? C15 C16 C17 C18 2.4(6) . . . . ? C14 C16 C17 C18 -173.3(4) . . . . ? C16 C17 C18 C19 5.4(6) . . . . ? C16 C17 C18 C52 -174.8(4) . . . . ? C17 C18 C19 C20 -6.3(6) . . . . ? C52 C18 C19 C20 174.0(4) . . . . ? C18 C19 C20 C15 -0.8(6) . . . . ? C18 C19 C20 C21 178.0(4) . . . . ? C16 C15 C20 C19 9.3(6) . . . . ? O5 C15 C20 C19 -169.4(3) . . . . ? C16 C15 C20 C21 -169.5(4) . . . . ? O5 C15 C20 C21 11.8(5) . . . . ? C19 C20 C21 C23 -77.5(4) . . . . ? C15 C20 C21 C23 101.2(4) . . . . ? C72 O8 C22 C27 91.1(4) . . . . ? C72 O8 C22 C23 -90.7(4) . . . . ? O8 C22 C23 C24 179.4(3) . . . . ? C27 C22 C23 C24 -2.4(6) . . . . ? O8 C22 C23 C21 -2.0(5) . . . . ? C27 C22 C23 C21 176.1(3) . . . . ? C20 C21 C23 C24 86.7(4) . . . . ? C20 C21 C23 C22 -91.8(4) . . . . ? C22 C23 C24 C25 0.5(6) . . . . ? C21 C23 C24 C25 -178.1(4) . . . . ? C23 C24 C25 C26 1.1(6) . . . . ? C23 C24 C25 C68 -177.9(4) . . . . ? C24 C25 C26 C27 -0.9(6) . . . . ? C68 C25 C26 C27 178.1(4) . . . . ? O8 C22 C27 C26 -179.2(3) . . . . ? C23 C22 C27 C26 2.6(6) . . . . ? O8 C22 C27 C28 5.3(5) . . . . ? C23 C22 C27 C28 -172.9(3) . . . . ? C25 C26 C27 C22 -0.9(6) . . . . ? C25 C26 C27 C28 174.6(4) . . . . ? C3 C2 C28 C27 74.4(4) . . . . ? C1 C2 C28 C27 -102.6(4) . . . . ? C22 C27 C28 C2 92.6(4) . . . . ? C26 C27 C28 C2 -82.8(4) . . . . ? C3 C4 C29 C30 -16.3(7) . . . . ? C5 C4 C29 C30 166.5(5) . . . . ? C3 C4 C29 C31 103.4(6) . . . . ? C5 C4 C29 C31 -73.8(6) . . . . ? C3 C4 C29 C32 -137.4(5) . . . . ? C5 C4 C29 C32 45.4(6) . . . . ? O3 S1 C33 C42 144.7(3) . . . . ? O2 S1 C33 C42 13.6(4) . . . . ? O1 S1 C33 C42 -96.3(3) . . . . ? O3 S1 C33 C34 -35.2(4) . . . . ? O2 S1 C33 C34 -166.3(3) . . . . ? O1 S1 C33 C34 83.8(4) . . . . ? C42 C33 C34 C39 -2.2(6) . . . . ? S1 C33 C34 C39 177.6(3) . . . . ? C42 C33 C34 C35 176.9(4) . . . . ? S1 C33 C34 C35 -3.3(6) . . . . ? C33 C34 C35 C36 -177.4(4) . . . . ? C39 C34 C35 C36 1.8(6) . . . . ? C34 C35 C36 C37 -2.7(8) . . . . ? C35 C36 C37 C38 0.3(9) . . . . ? C36 C37 C38 C39 3.0(8) . . . . ? C36 C37 C38 N1 -176.8(5) . . . . ? C43 N1 C38 C37 -24.5(8) . . . . ? C44 N1 C38 C37 104.8(6) . . . . ? C43 N1 C38 C39 155.7(6) . . . . ? C44 N1 C38 C39 -75.0(6) . . . . ? C37 C38 C39 C34 -3.9(7) . . . . ? N1 C38 C39 C34 175.9(4) . . . . ? C37 C38 C39 C40 173.6(5) . . . . ? N1 C38 C39 C40 -6.6(7) . . . . ? C33 C34 C39 C38 -179.3(4) . . . . ? C35 C34 C39 C38 1.5(6) . . . . ? C33 C34 C39 C40 3.1(6) . . . . ? C35 C34 C39 C40 -176.1(4) . . . . ? C38 C39 C40 C41 -178.7(5) . . . . ? C34 C39 C40 C41 -1.1(7) . . . . ? C39 C40 C41 C42 -1.9(8) . . . . ? C34 C33 C42 C41 -0.8(7) . . . . ? S1 C33 C42 C41 179.4(4) . . . . ? C40 C41 C42 C33 2.9(8) . . . . ? C10 C11 C45 C48A -114.4(9) . . . . ? C12 C11 C45 C48A 66.0(10) . . . . ? C10 C11 C45 C46 -50.6(7) . . . . ? C12 C11 C45 C46 129.8(6) . . . . ? C10 C11 C45 C48 -169.7(6) . . . . ? C12 C11 C45 C48 10.7(7) . . . . ? C10 C11 C45 C47 71.3(6) . . . . ? C12 C11 C45 C47 -108.3(6) . . . . ? C10 C11 C45 C47A 122.7(13) . . . . ? C12 C11 C45 C47A -56.9(13) . . . . ? C10 C11 C45 C46A 6.4(12) . . . . ? C12 C11 C45 C46A -173.2(12) . . . . ? C8 O4 C49 C50 -174.3(4) . . . . ? O4 C49 C50 C51 179.7(4) . . . . ? C19 C18 C52 C53 118.2(5) . . . . ? C17 C18 C52 C53 -61.6(5) . . . . ? C19 C18 C52 C55 -3.5(6) . . . . ? C17 C18 C52 C55 176.7(4) . . . . ? C19 C18 C52 C54 -122.2(5) . . . . ? C17 C18 C52 C54 58.0(6) . . . . ? O6 S2 C56 C65 147.6(4) . . . . ? O7 S2 C56 C65 14.8(4) . . . . ? O5 S2 C56 C65 -93.4(4) . . . . ? O6 S2 C56 C57 -34.8(5) . . . . ? O7 S2 C56 C57 -167.6(4) . . . . ? O5 S2 C56 C57 84.2(4) . . . . ? C65 C56 C57 C62 2.7(7) . . . . ? S2 C56 C57 C62 -174.8(4) . . . . ? C65 C56 C57 C58 -176.4(5) . . . . ? S2 C56 C57 C58 6.2(7) . . . . ? C56 C57 C58 C59 179.2(5) . . . . ? C62 C57 C58 C59 0.1(7) . . . . ? C57 C58 C59 C60 5.9(9) . . . . ? C58 C59 C60 C61 -3.5(11) . . . . ? C59 C60 C61 C62 -5.2(11) . . . . ? C59 C60 C61 N2 178.4(7) . . . . ? C67 N2 C61 C60 21.1(11) . . . . ? C66 N2 C61 C60 -108.2(8) . . . . ? C67 N2 C61 C62 -155.4(7) . . . . ? C66 N2 C61 C62 75.3(8) . . . . ? C60 C61 C62 C63 -174.8(7) . . . . ? N2 C61 C62 C63 1.8(10) . . . . ? C60 C61 C62 C57 11.1(10) . . . . ? N2 C61 C62 C57 -172.4(6) . . . . ? C56 C57 C62 C63 -1.9(8) . . . . ? C58 C57 C62 C63 177.2(5) . . . . ? C56 C57 C62 C61 172.6(6) . . . . ? C58 C57 C62 C61 -8.3(8) . . . . ? C61 C62 C63 C64 -175.8(6) . . . . ? C57 C62 C63 C64 -1.5(10) . . . . ? C62 C63 C64 C65 4.1(9) . . . . ? C57 C56 C65 C64 -0.1(8) . . . . ? S2 C56 C65 C64 177.5(4) . . . . ? C63 C64 C65 C56 -3.3(8) . . . . ? C26 C25 C68 C69 133.2(5) . . . . ? C24 C25 C68 C69 -47.9(6) . . . . ? C26 C25 C68 C70 -106.1(6) . . . . ? C24 C25 C68 C70 72.9(6) . . . . ? C26 C25 C68 C71 13.6(6) . . . . ? C24 C25 C68 C71 -167.5(5) . . . . ? C26 C25 C68 C70A -65(2) . . . . ? C24 C25 C68 C70A 114(2) . . . . ? C26 C25 C68 C71A 51.8(17) . . . . ? C24 C25 C68 C71A -129.2(17) . . . . ? C26 C25 C68 C69A 174.0(19) . . . . ? C24 C25 C68 C69A -7(2) . . . . ? C22 O8 C72 C73 179.0(4) . . . . ? O8 C72 C73 C74 179.8(4) . . . . ? 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 C41 H41 N1H 0.95 2.56 3.504(8) 174.1 1_655 C73 H73A O2 0.99 2.39 3.369(6) 168.1 1 C3 H3 O3 0.95 2.48 3.344(6) 150.6 2_775 C35 H35 O3 0.95 2.35 2.995(6) 124.3 1 C17 H17 O6 0.95 2.61 3.500(6) 157.0 2_776 C58 H58 O6 0.95 2.30 2.987(6) 128.1 1 C50 H50A O7 0.99 2.53 3.513(7) 175.4 1 C65 H65 O7 0.95 2.37 2.810(6) 107.6 1 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.44 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.897 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.145 # Attachment 'S2_NEW.cif' data_togr_75_0m _database_code_depnum_ccdc_archive 'CCDC 697368' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C74 H86 N2 O8 S2, C2 H3 N O' _chemical_formula_sum 'C76 H89 N3 O9 S2' _chemical_formula_weight 1252.62 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.3771(5) _cell_length_b 19.9839(5) _cell_length_c 18.8147(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.635(2) _cell_angle_gamma 90.00 _cell_volume 6848.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 6957 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 29.17 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2680 _exptl_absorpt_coefficient_mu 0.137 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.9311 _exptl_absorpt_correction_T_max 0.9771 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 155529 _diffrn_reflns_av_R_equivalents 0.0629 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 29.84 _reflns_number_total 19640 _reflns_number_gt 12956 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa APEX 2 (Bruker-AXS)' _computing_cell_refinement 'SAINT-NT (Bruker, 2003)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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. Six C-C distances regarding the disordered tert-butyl group of the calixarene (C29-C30, C29-C31, C29-C32, C29-C30A, C29-C31A, C29-C32A) were restrained to a target value of 1.54 (0.01) angstroms. ; _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^)+(0.0950P)^2^+4.5731P] 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 19640 _refine_ls_number_parameters 859 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0997 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1869 _refine_ls_wR_factor_gt 0.1509 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.028 _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 0.44273(3) 0.76528(3) 0.81103(3) 0.02599(12) Uani 1 1 d . . . S2 S 0.17345(3) 0.49790(3) 1.01193(3) 0.02514(11) Uani 1 1 d . . . O1 O 0.37061(7) 0.72072(7) 0.81480(7) 0.0225(3) Uani 1 1 d . . . O2 O 0.48304(9) 0.75876(9) 0.88056(9) 0.0369(4) Uani 1 1 d . . . O3 O 0.42151(9) 0.83046(8) 0.78450(9) 0.0347(4) Uani 1 1 d . . . O4 O 0.29049(8) 0.57196(7) 0.82116(7) 0.0250(3) Uani 1 1 d . . . O5 O 0.18885(7) 0.55589(7) 0.95699(7) 0.0224(3) Uani 1 1 d . . . O6 O 0.24328(9) 0.46805(8) 1.03299(9) 0.0362(4) Uani 1 1 d . . . O7 O 0.11444(9) 0.45688(8) 0.97950(8) 0.0320(3) Uani 1 1 d . . . O8 O 0.24022(7) 0.70546(7) 0.92151(7) 0.0234(3) Uani 1 1 d . . . N1 N 0.66007(10) 0.57145(10) 0.65677(11) 0.0329(4) Uani 1 1 d . . . N2 N 0.17506(14) 0.69008(11) 1.29199(11) 0.0433(5) Uani 1 1 d . . . C1 C 0.30851(10) 0.73453(10) 0.76291(10) 0.0219(4) Uani 1 1 d . . . C2 C 0.26224(11) 0.78657(10) 0.77645(11) 0.0221(4) Uani 1 1 d . . . C3 C 0.20412(12) 0.80191(10) 0.72381(11) 0.0268(4) Uani 1 1 d . . . H3 H 0.1724 0.8378 0.7319 0.032 Uiso 1 1 calc R . . C4 C 0.19072(12) 0.76647(11) 0.65959(11) 0.0283(4) Uani 1 1 d . A . C5 C 0.23659(12) 0.71231(11) 0.65106(11) 0.0270(4) Uani 1 1 d . . . H5 H 0.2275 0.6864 0.6084 0.032 Uiso 1 1 calc R . . C6 C 0.29516(11) 0.69450(10) 0.70232(10) 0.0226(4) Uani 1 1 d . . . C7 C 0.33608(11) 0.62890(10) 0.69448(11) 0.0244(4) Uani 1 1 d . . . H7A H 0.3590 0.6294 0.6498 0.029 Uiso 1 1 calc R . . H7B H 0.3752 0.6229 0.7355 0.029 Uiso 1 1 calc R . . C8 C 0.25705(10) 0.54873(10) 0.75538(10) 0.0214(4) Uani 1 1 d . . . C9 C 0.28108(10) 0.57239(10) 0.69236(10) 0.0211(4) Uani 1 1 d . . . C10 C 0.24544(11) 0.54970(10) 0.62699(10) 0.0225(4) Uani 1 1 d . . . H10 H 0.2626 0.5642 0.5841 0.027 Uiso 1 1 calc R . . C11 C 0.18532(10) 0.50643(10) 0.62215(10) 0.0214(4) Uani 1 1 d . . . C12 C 0.16225(11) 0.48492(10) 0.68601(11) 0.0219(4) Uani 1 1 d . . . H12 H 0.1213 0.4556 0.6840 0.026 Uiso 1 1 calc R . . C13 C 0.19756(10) 0.50523(9) 0.75293(10) 0.0206(4) Uani 1 1 d . . . C14 C 0.16721(11) 0.48520(10) 0.82122(10) 0.0231(4) Uani 1 1 d . . . H14A H 0.1406 0.4422 0.8136 0.028 Uiso 1 1 calc R . . H14B H 0.2081 0.4790 0.8605 0.028 Uiso 1 1 calc R . . C15 C 0.12856(10) 0.57533(9) 0.90546(10) 0.0198(4) Uani 1 1 d . . . C16 C 0.11538(10) 0.53893(9) 0.84193(10) 0.0202(4) Uani 1 1 d . . . C17 C 0.05311(11) 0.55539(10) 0.79463(10) 0.0225(4) Uani 1 1 d . . . H17 H 0.0430 0.5312 0.7510 0.027 Uiso 1 1 calc R . . C18 C 0.00510(11) 0.60604(10) 0.80900(10) 0.0217(4) Uani 1 1 d . . . C19 C 0.02383(11) 0.64323(10) 0.87140(10) 0.0224(4) Uani 1 1 d . . . H19 H -0.0072 0.6792 0.8811 0.027 Uiso 1 1 calc R . . C20 C 0.08576(10) 0.63014(10) 0.91989(10) 0.0200(4) Uani 1 1 d . . . C21 C 0.10684(11) 0.67978(10) 0.98055(10) 0.0223(4) Uani 1 1 d . . . H21A H 0.1504 0.6632 1.0124 0.027 Uiso 1 1 calc R . . H21B H 0.0659 0.6848 1.0094 0.027 Uiso 1 1 calc R . . C22 C 0.18951(10) 0.75681(9) 0.91989(10) 0.0201(4) Uani 1 1 d . . . C23 C 0.12401(11) 0.74706(10) 0.94858(10) 0.0207(4) Uani 1 1 d . . . C24 C 0.07126(11) 0.79781(10) 0.94049(10) 0.0236(4) Uani 1 1 d . . . H24 H 0.0267 0.7915 0.9602 0.028 Uiso 1 1 calc R . . C25 C 0.08168(11) 0.85735(10) 0.90456(11) 0.0254(4) Uani 1 1 d . . . C26 C 0.14816(12) 0.86505(10) 0.87699(11) 0.0258(4) Uani 1 1 d . . . H26 H 0.1569 0.9056 0.8531 0.031 Uiso 1 1 calc R . . C27 C 0.20177(11) 0.81582(10) 0.88315(10) 0.0213(4) Uani 1 1 d . . . C28 C 0.27004(11) 0.82396(10) 0.84723(11) 0.0231(4) Uani 1 1 d . . . H28A H 0.3130 0.8065 0.8792 0.028 Uiso 1 1 calc R . . H28B H 0.2785 0.8721 0.8387 0.028 Uiso 1 1 calc R . . C29 C 0.12668(14) 0.78494(12) 0.60183(13) 0.0391(6) Uani 1 1 d D . . C30 C 0.0692(2) 0.8322(2) 0.6310(2) 0.0451(10) Uani 0.721(6) 1 d PD A 1 H30A H 0.0912 0.8764 0.6413 0.068 Uiso 0.721(6) 1 calc PR A 1 H30B H 0.0547 0.8132 0.6750 0.068 Uiso 0.721(6) 1 calc PR A 1 H30C H 0.0259 0.8365 0.5948 0.068 Uiso 0.721(6) 1 calc PR A 1 C31 C 0.1541(3) 0.8216(4) 0.5409(3) 0.078(2) Uani 0.721(6) 1 d PD A 1 H31A H 0.1124 0.8348 0.5058 0.117 Uiso 0.721(6) 1 calc PR A 1 H31B H 0.1867 0.7922 0.5178 0.117 Uiso 0.721(6) 1 calc PR A 1 H31C H 0.1811 0.8616 0.5593 0.117 Uiso 0.721(6) 1 calc PR A 1 C32 C 0.0828(2) 0.7222(2) 0.5756(3) 0.0647(16) Uani 0.721(6) 1 d PD A 1 H32A H 0.0424 0.7348 0.5387 0.097 Uiso 0.721(6) 1 calc PR A 1 H32B H 0.0628 0.7013 0.6160 0.097 Uiso 0.721(6) 1 calc PR A 1 H32C H 0.1152 0.6904 0.5555 0.097 Uiso 0.721(6) 1 calc PR A 1 C30A C 0.0583(5) 0.7716(10) 0.6338(8) 0.092(6) Uani 0.279(6) 1 d PD A 2 H30D H 0.0519 0.8063 0.6693 0.137 Uiso 0.279(6) 1 calc PR A 2 H30E H 0.0617 0.7277 0.6571 0.137 Uiso 0.279(6) 1 calc PR A 2 H30F H 0.0161 0.7722 0.5959 0.137 Uiso 0.279(6) 1 calc PR A 2 C31A C 0.1390(9) 0.8587(4) 0.5822(7) 0.070(5) Uani 0.279(6) 1 d PD A 2 H31D H 0.1085 0.8696 0.5370 0.104 Uiso 0.279(6) 1 calc PR A 2 H31E H 0.1908 0.8656 0.5770 0.104 Uiso 0.279(6) 1 calc PR A 2 H31F H 0.1256 0.8879 0.6203 0.104 Uiso 0.279(6) 1 calc PR A 2 C32A C 0.1362(6) 0.7474(6) 0.5303(4) 0.055(3) Uani 0.279(6) 1 d PD A 2 H32D H 0.1321 0.6991 0.5374 0.082 Uiso 0.279(6) 1 calc PR A 2 H32E H 0.1846 0.7577 0.5166 0.082 Uiso 0.279(6) 1 calc PR A 2 H32F H 0.0980 0.7621 0.4922 0.082 Uiso 0.279(6) 1 calc PR A 2 C33 C 0.48594(11) 0.72398(11) 0.74516(11) 0.0247(4) Uani 1 1 d . . . C34 C 0.46668(11) 0.74726(11) 0.67672(12) 0.0272(4) Uani 1 1 d . . . H34 H 0.4349 0.7847 0.6683 0.033 Uiso 1 1 calc R . . C35 C 0.49394(12) 0.71576(12) 0.61925(12) 0.0299(4) Uani 1 1 d . . . H35 H 0.4779 0.7299 0.5715 0.036 Uiso 1 1 calc R . . C36 C 0.54323(11) 0.66495(11) 0.63150(11) 0.0276(4) Uani 1 1 d . . . H36 H 0.5613 0.6441 0.5919 0.033 Uiso 1 1 calc R . . C37 C 0.56830(11) 0.64229(10) 0.70192(11) 0.0242(4) Uani 1 1 d . . . C38 C 0.62432(11) 0.59223(11) 0.71504(12) 0.0277(4) Uani 1 1 d . . . C39 C 0.63974(14) 0.56493(12) 0.78255(13) 0.0365(5) Uani 1 1 d . . . H39 H 0.6755 0.5305 0.7911 0.044 Uiso 1 1 calc R . . C40 C 0.60300(15) 0.58761(14) 0.83872(14) 0.0408(6) Uani 1 1 d . . . H40 H 0.6129 0.5668 0.8844 0.049 Uiso 1 1 calc R . . C41 C 0.55321(13) 0.63905(13) 0.82958(12) 0.0348(5) Uani 1 1 d . . . H41 H 0.5306 0.6546 0.8690 0.042 Uiso 1 1 calc R . . C42 C 0.53550(11) 0.66897(11) 0.76101(11) 0.0242(4) Uani 1 1 d . . . C43 C 0.70229(14) 0.50956(13) 0.66652(16) 0.0413(6) Uani 1 1 d . . . H43A H 0.7468 0.5172 0.7004 0.062 Uiso 1 1 calc R . . H43B H 0.7159 0.4951 0.6203 0.062 Uiso 1 1 calc R . . H43C H 0.6725 0.4748 0.6854 0.062 Uiso 1 1 calc R . . C44 C 0.70096(13) 0.62373(13) 0.62369(14) 0.0379(5) Uani 1 1 d . . . H44A H 0.6795 0.6676 0.6315 0.057 Uiso 1 1 calc R . . H44B H 0.6982 0.6152 0.5721 0.057 Uiso 1 1 calc R . . H44C H 0.7524 0.6232 0.6455 0.057 Uiso 1 1 calc R . . C45 C 0.14610(11) 0.48711(10) 0.54786(11) 0.0255(4) Uani 1 1 d . . . C46 C 0.11859(14) 0.55096(13) 0.50752(13) 0.0385(5) Uani 1 1 d . . . H46A H 0.1605 0.5796 0.5010 0.058 Uiso 1 1 calc R . . H46B H 0.0855 0.5751 0.5352 0.058 Uiso 1 1 calc R . . H46C H 0.0922 0.5389 0.4605 0.058 Uiso 1 1 calc R . . C47 C 0.20037(13) 0.45156(12) 0.50510(11) 0.0317(5) Uani 1 1 d . . . H47A H 0.1769 0.4438 0.4559 0.048 Uiso 1 1 calc R . . H47B H 0.2148 0.4086 0.5279 0.048 Uiso 1 1 calc R . . H47C H 0.2440 0.4796 0.5042 0.048 Uiso 1 1 calc R . . C48 C 0.08045(12) 0.44125(13) 0.55213(13) 0.0340(5) Uani 1 1 d . . . H48A H 0.0453 0.4636 0.5791 0.051 Uiso 1 1 calc R . . H48B H 0.0972 0.3996 0.5765 0.051 Uiso 1 1 calc R . . H48C H 0.0566 0.4311 0.5036 0.051 Uiso 1 1 calc R . . C49 C 0.35367(13) 0.53296(13) 0.84936(13) 0.0375(5) Uani 1 1 d . . . H49A H 0.3877 0.5290 0.8130 0.045 Uiso 1 1 calc R . . H49B H 0.3382 0.4874 0.8615 0.045 Uiso 1 1 calc R . . C50 C 0.39089(15) 0.56626(17) 0.91407(15) 0.0475(7) Uani 1 1 d . . . H50 H 0.4013 0.6125 0.9096 0.057 Uiso 1 1 calc R . . C51 C 0.41069(19) 0.53994(19) 0.97547(17) 0.0622(9) Uani 1 1 d . . . H51A H 0.4016 0.4939 0.9830 0.075 Uiso 1 1 calc R . . H51B H 0.4345 0.5665 1.0136 0.075 Uiso 1 1 calc R . . C52 C -0.06579(12) 0.62250(11) 0.75977(11) 0.0278(4) Uani 1 1 d . . . C53 C -0.06752(18) 0.69709(13) 0.74062(15) 0.0474(7) Uani 1 1 d . . . H53A H -0.0662 0.7238 0.7845 0.071 Uiso 1 1 calc R . . H53B H -0.1127 0.7071 0.7085 0.071 Uiso 1 1 calc R . . H53C H -0.0249 0.7081 0.7166 0.071 Uiso 1 1 calc R . . C54 C -0.07276(15) 0.58239(14) 0.69011(13) 0.0410(6) Uani 1 1 d . . . H54A H -0.0305 0.5918 0.6649 0.061 Uiso 1 1 calc R . . H54B H -0.1181 0.5951 0.6597 0.061 Uiso 1 1 calc R . . H54C H -0.0741 0.5345 0.7011 0.061 Uiso 1 1 calc R . . C55 C -0.13180(13) 0.60674(17) 0.79930(15) 0.0472(7) Uani 1 1 d . . . H55A H -0.1344 0.5584 0.8073 0.071 Uiso 1 1 calc R . . H55B H -0.1771 0.6218 0.7703 0.071 Uiso 1 1 calc R . . H55C H -0.1260 0.6300 0.8456 0.071 Uiso 1 1 calc R . . C56 C 0.14347(11) 0.54224(10) 1.08368(10) 0.0241(4) Uani 1 1 d . . . C57 C 0.06917(12) 0.54040(11) 1.08748(11) 0.0279(4) Uani 1 1 d . . . H57 H 0.0379 0.5136 1.0547 0.033 Uiso 1 1 calc R . . C58 C 0.03954(12) 0.57800(12) 1.13967(12) 0.0317(5) Uani 1 1 d . . . H58 H -0.0119 0.5776 1.1415 0.038 Uiso 1 1 calc R . . C59 C 0.08466(13) 0.61515(11) 1.18781(12) 0.0315(5) Uani 1 1 d . . . H59 H 0.0640 0.6405 1.2229 0.038 Uiso 1 1 calc R . . C60 C 0.16167(12) 0.61690(10) 1.18691(11) 0.0270(4) Uani 1 1 d . . . C61 C 0.20830(14) 0.65703(11) 1.23760(12) 0.0335(5) Uani 1 1 d . . . C62 C 0.28137(15) 0.66321(13) 1.22961(13) 0.0398(6) Uani 1 1 d . . . H62 H 0.3121 0.6913 1.2614 0.048 Uiso 1 1 calc R . . C63 C 0.31101(14) 0.62885(14) 1.17551(13) 0.0390(6) Uani 1 1 d . . . H63 H 0.3616 0.6342 1.1713 0.047 Uiso 1 1 calc R . . C64 C 0.26927(12) 0.58778(12) 1.12852(12) 0.0301(4) Uani 1 1 d . . . H64 H 0.2911 0.5638 1.0932 0.036 Uiso 1 1 calc R . . C65 C 0.19280(11) 0.58099(10) 1.13265(10) 0.0240(4) Uani 1 1 d . . . C66 C 0.2132(2) 0.74953(16) 1.32227(18) 0.0629(9) Uani 1 1 d . . . H66A H 0.2592 0.7363 1.3514 0.094 Uiso 1 1 calc R . . H66B H 0.1821 0.7733 1.3524 0.094 Uiso 1 1 calc R . . H66C H 0.2241 0.7790 1.2834 0.094 Uiso 1 1 calc R . . C67 C 0.15570(18) 0.64573(16) 1.34831(14) 0.0517(7) Uani 1 1 d . . . H67A H 0.1313 0.6057 1.3265 0.078 Uiso 1 1 calc R . . H67B H 0.1225 0.6691 1.3766 0.078 Uiso 1 1 calc R . . H67C H 0.2003 0.6326 1.3796 0.078 Uiso 1 1 calc R . . C68 C 0.02367(14) 0.91270(12) 0.89189(13) 0.0371(5) Uani 1 1 d . . . C69 C -0.04520(14) 0.89630(15) 0.92565(16) 0.0452(6) Uani 1 1 d . . . H69A H -0.0676 0.8553 0.9041 0.068 Uiso 1 1 calc R . . H69B H -0.0802 0.9333 0.9172 0.068 Uiso 1 1 calc R . . H69C H -0.0320 0.8897 0.9774 0.068 Uiso 1 1 calc R . . C70 C 0.05597(18) 0.97820(14) 0.9244(2) 0.0607(9) Uani 1 1 d . . . H70A H 0.0190 1.0137 0.9163 0.091 Uiso 1 1 calc R . . H70B H 0.0990 0.9905 0.9016 0.091 Uiso 1 1 calc R . . H70C H 0.0705 0.9723 0.9760 0.091 Uiso 1 1 calc R . . C71 C 0.0014(2) 0.9208(2) 0.81051(17) 0.0706(11) Uani 1 1 d . . . H71A H -0.0164 0.8778 0.7898 0.106 Uiso 1 1 calc R . . H71B H 0.0440 0.9354 0.7883 0.106 Uiso 1 1 calc R . . H71C H -0.0377 0.9543 0.8016 0.106 Uiso 1 1 calc R . . C72 C 0.28463(12) 0.69536(11) 0.98999(12) 0.0291(4) Uani 1 1 d . . . H72A H 0.2992 0.6477 0.9946 0.035 Uiso 1 1 calc R . . H72B H 0.2549 0.7057 1.0288 0.035 Uiso 1 1 calc R . . C73 C 0.35181(12) 0.73774(12) 0.99919(12) 0.0305(4) Uani 1 1 d . . . H73 H 0.3870 0.7317 0.9670 0.037 Uiso 1 1 calc R . . C74 C 0.36460(16) 0.78290(14) 1.04966(15) 0.0458(6) Uani 1 1 d . . . H74A H 0.3302 0.7898 1.0825 0.055 Uiso 1 1 calc R . . H74B H 0.4083 0.8088 1.0535 0.055 Uiso 1 1 calc R . . N1G N 0.1837(3) 0.1775(3) 1.0046(3) 0.1390(19) Uani 1 1 d . . . C1G C 0.1600(2) 0.30128(19) 0.9930(2) 0.0672(10) Uani 1 1 d . . . H1G1 H 0.1660 0.3162 0.9440 0.081 Uiso 1 1 calc R . . H1G2 H 0.1964 0.3253 1.0274 0.081 Uiso 1 1 calc R . . C2G C 0.1713(3) 0.2367(3) 0.9987(3) 0.1075(17) Uani 1 1 d . . . O1G O 0.0913(3) 0.3157(3) 1.0068(3) 0.1482(16) Uani 1 1 d . . . H1G H 0.0838 0.3575 1.0021 0.222 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 0.0204(2) 0.0307(3) 0.0279(3) -0.0069(2) 0.00664(18) -0.00305(19) S2 0.0306(3) 0.0236(2) 0.0208(2) 0.00292(18) 0.00174(18) 0.00168(19) O1 0.0195(6) 0.0263(7) 0.0222(7) -0.0013(5) 0.0043(5) -0.0010(5) O2 0.0261(8) 0.0558(11) 0.0287(8) -0.0129(7) 0.0034(6) -0.0034(7) O3 0.0315(8) 0.0266(8) 0.0481(10) -0.0071(7) 0.0134(7) -0.0056(6) O4 0.0256(7) 0.0279(7) 0.0210(7) -0.0047(6) 0.0007(5) 0.0034(6) O5 0.0219(7) 0.0263(7) 0.0188(6) 0.0024(5) 0.0016(5) 0.0009(5) O6 0.0393(9) 0.0357(9) 0.0326(8) 0.0058(7) 0.0012(7) 0.0121(7) O7 0.0432(9) 0.0261(7) 0.0262(8) 0.0008(6) 0.0023(6) -0.0060(7) O8 0.0232(7) 0.0233(7) 0.0237(7) 0.0007(5) 0.0036(5) 0.0060(5) N1 0.0280(9) 0.0342(10) 0.0378(10) -0.0035(8) 0.0092(8) 0.0050(8) N2 0.0632(14) 0.0343(11) 0.0305(10) -0.0072(9) -0.0013(10) 0.0030(10) C1 0.0199(8) 0.0242(9) 0.0221(9) 0.0014(7) 0.0045(7) -0.0028(7) C2 0.0239(9) 0.0207(9) 0.0227(9) 0.0010(7) 0.0066(7) -0.0027(7) C3 0.0296(10) 0.0235(9) 0.0275(10) 0.0034(8) 0.0042(8) 0.0017(8) C4 0.0332(11) 0.0255(10) 0.0248(10) 0.0049(8) -0.0007(8) -0.0024(8) C5 0.0327(11) 0.0280(10) 0.0204(9) -0.0001(8) 0.0033(8) -0.0036(8) C6 0.0228(9) 0.0242(9) 0.0218(9) -0.0001(7) 0.0066(7) -0.0021(7) C7 0.0214(9) 0.0267(10) 0.0263(10) -0.0040(8) 0.0070(7) -0.0017(7) C8 0.0223(9) 0.0210(9) 0.0208(9) -0.0046(7) 0.0026(7) 0.0044(7) C9 0.0185(8) 0.0229(9) 0.0229(9) -0.0034(7) 0.0063(7) 0.0020(7) C10 0.0235(9) 0.0241(9) 0.0212(9) -0.0013(7) 0.0076(7) 0.0014(7) C11 0.0219(9) 0.0229(9) 0.0198(9) -0.0039(7) 0.0039(7) 0.0031(7) C12 0.0225(9) 0.0196(9) 0.0244(9) -0.0038(7) 0.0064(7) 0.0009(7) C13 0.0238(9) 0.0187(8) 0.0203(9) -0.0010(7) 0.0068(7) 0.0035(7) C14 0.0273(10) 0.0222(9) 0.0208(9) 0.0006(7) 0.0065(7) 0.0028(7) C15 0.0200(8) 0.0223(9) 0.0175(8) 0.0027(7) 0.0039(7) -0.0012(7) C16 0.0237(9) 0.0199(8) 0.0181(8) 0.0014(7) 0.0072(7) -0.0012(7) C17 0.0259(9) 0.0251(9) 0.0172(8) -0.0019(7) 0.0049(7) -0.0001(7) C18 0.0237(9) 0.0242(9) 0.0173(8) 0.0007(7) 0.0034(7) 0.0004(7) C19 0.0235(9) 0.0242(9) 0.0201(9) -0.0007(7) 0.0050(7) 0.0030(7) C20 0.0226(9) 0.0228(9) 0.0155(8) -0.0007(7) 0.0060(7) -0.0021(7) C21 0.0253(9) 0.0244(9) 0.0178(8) -0.0017(7) 0.0051(7) -0.0004(7) C22 0.0217(9) 0.0204(9) 0.0180(8) -0.0025(7) 0.0023(7) 0.0034(7) C23 0.0234(9) 0.0222(9) 0.0167(8) -0.0030(7) 0.0029(7) 0.0003(7) C24 0.0227(9) 0.0287(10) 0.0198(9) -0.0033(8) 0.0038(7) 0.0037(8) C25 0.0283(10) 0.0256(10) 0.0225(9) -0.0018(8) 0.0040(8) 0.0063(8) C26 0.0324(10) 0.0204(9) 0.0252(10) 0.0013(7) 0.0055(8) 0.0048(8) C27 0.0235(9) 0.0210(9) 0.0197(9) -0.0020(7) 0.0038(7) 0.0000(7) C28 0.0248(9) 0.0213(9) 0.0238(9) -0.0009(7) 0.0056(7) -0.0020(7) C29 0.0445(14) 0.0371(13) 0.0319(12) 0.0012(10) -0.0087(10) 0.0069(11) C30 0.0351(19) 0.046(2) 0.050(2) -0.0010(17) -0.0104(16) 0.0144(16) C31 0.061(3) 0.125(6) 0.049(3) 0.047(3) 0.007(2) 0.026(3) C32 0.046(2) 0.054(3) 0.084(4) -0.024(2) -0.028(2) 0.014(2) C30A 0.036(6) 0.115(14) 0.111(13) 0.003(10) -0.036(7) 0.001(7) C31A 0.117(12) 0.036(5) 0.044(6) 0.001(5) -0.032(7) 0.019(6) C32A 0.062(7) 0.060(7) 0.034(5) -0.007(5) -0.022(5) 0.024(6) C33 0.0202(9) 0.0306(10) 0.0242(9) -0.0013(8) 0.0069(7) -0.0022(8) C34 0.0213(9) 0.0310(10) 0.0296(10) 0.0029(8) 0.0044(8) 0.0005(8) C35 0.0278(10) 0.0400(12) 0.0225(10) 0.0064(9) 0.0053(8) 0.0015(9) C36 0.0243(10) 0.0377(11) 0.0218(9) -0.0014(8) 0.0068(8) -0.0002(8) C37 0.0205(9) 0.0275(10) 0.0251(10) -0.0006(8) 0.0049(7) -0.0013(7) C38 0.0226(9) 0.0301(10) 0.0310(11) -0.0017(8) 0.0058(8) -0.0002(8) C39 0.0356(12) 0.0337(12) 0.0400(13) 0.0058(10) 0.0045(10) 0.0093(10) C40 0.0447(14) 0.0465(14) 0.0315(12) 0.0124(11) 0.0066(10) 0.0099(11) C41 0.0355(12) 0.0461(13) 0.0241(10) 0.0060(9) 0.0085(9) 0.0066(10) C42 0.0204(9) 0.0307(10) 0.0225(9) 0.0003(8) 0.0061(7) -0.0020(8) C43 0.0341(12) 0.0367(13) 0.0544(16) -0.0083(11) 0.0102(11) 0.0076(10) C44 0.0303(11) 0.0461(14) 0.0400(13) 0.0009(11) 0.0143(10) 0.0037(10) C45 0.0262(10) 0.0282(10) 0.0214(9) -0.0019(8) 0.0005(7) 0.0007(8) C46 0.0414(13) 0.0376(12) 0.0335(12) 0.0048(10) -0.0061(10) 0.0044(10) C47 0.0340(11) 0.0398(12) 0.0209(10) -0.0071(9) 0.0019(8) 0.0020(9) C48 0.0289(11) 0.0405(12) 0.0314(11) -0.0063(10) -0.0005(9) -0.0045(9) C49 0.0347(12) 0.0449(14) 0.0304(11) -0.0030(10) -0.0042(9) 0.0126(10) C50 0.0372(13) 0.0655(18) 0.0375(14) -0.0065(13) -0.0037(11) 0.0092(13) C51 0.065(2) 0.074(2) 0.0413(16) -0.0031(15) -0.0134(14) 0.0173(17) C52 0.0288(10) 0.0320(11) 0.0213(9) 0.0003(8) -0.0017(8) 0.0046(8) C53 0.0649(18) 0.0344(13) 0.0373(13) 0.0049(11) -0.0134(12) 0.0100(12) C54 0.0417(13) 0.0484(14) 0.0288(11) -0.0106(10) -0.0103(10) 0.0105(11) C55 0.0252(11) 0.078(2) 0.0373(13) 0.0074(13) -0.0004(10) 0.0044(12) C56 0.0287(10) 0.0257(9) 0.0178(9) 0.0044(7) 0.0031(7) -0.0015(8) C57 0.0275(10) 0.0300(10) 0.0255(10) 0.0039(8) 0.0013(8) -0.0047(8) C58 0.0279(10) 0.0361(12) 0.0322(11) 0.0045(9) 0.0083(9) -0.0001(9) C59 0.0370(12) 0.0312(11) 0.0273(11) 0.0020(9) 0.0083(9) 0.0035(9) C60 0.0352(11) 0.0227(9) 0.0223(9) 0.0045(8) 0.0011(8) -0.0010(8) C61 0.0490(14) 0.0264(10) 0.0231(10) 0.0018(8) -0.0028(9) -0.0019(10) C62 0.0472(14) 0.0366(13) 0.0319(12) 0.0029(10) -0.0087(10) -0.0121(11) C63 0.0308(11) 0.0504(15) 0.0339(12) 0.0089(11) -0.0026(9) -0.0113(10) C64 0.0280(10) 0.0373(12) 0.0245(10) 0.0073(9) 0.0014(8) -0.0032(9) C65 0.0279(10) 0.0247(9) 0.0189(9) 0.0073(7) 0.0015(7) -0.0006(8) C66 0.087(2) 0.0425(16) 0.0531(18) -0.0179(14) -0.0134(17) 0.0014(16) C67 0.071(2) 0.0561(17) 0.0294(13) -0.0022(12) 0.0112(13) 0.0100(15) C68 0.0379(12) 0.0380(12) 0.0368(12) 0.0049(10) 0.0106(10) 0.0194(10) C69 0.0332(13) 0.0542(16) 0.0488(15) 0.0017(13) 0.0079(11) 0.0218(12) C70 0.0633(19) 0.0289(13) 0.097(3) -0.0020(15) 0.0369(18) 0.0157(13) C71 0.066(2) 0.101(3) 0.0471(17) 0.0273(18) 0.0138(15) 0.056(2) C72 0.0257(10) 0.0324(11) 0.0284(10) 0.0091(9) 0.0009(8) 0.0052(8) C73 0.0268(10) 0.0356(11) 0.0281(10) 0.0037(9) 0.0004(8) 0.0025(9) C74 0.0482(15) 0.0485(15) 0.0372(14) -0.0027(12) -0.0072(11) -0.0003(12) N1G 0.163(5) 0.111(4) 0.146(5) -0.004(4) 0.031(4) -0.008(4) C1G 0.0508(19) 0.064(2) 0.085(3) -0.0150(19) 0.0011(17) 0.0045(16) C2G 0.122(4) 0.088(4) 0.112(4) -0.015(3) 0.013(3) -0.013(3) O1G 0.135(4) 0.141(4) 0.170(4) -0.027(3) 0.027(3) -0.019(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O2 1.4211(17) . ? S1 O3 1.4304(17) . ? S1 O1 1.6060(14) . ? S1 C33 1.763(2) . ? S2 O6 1.4228(17) . ? S2 O7 1.4298(16) . ? S2 O5 1.6028(14) . ? S2 C56 1.763(2) . ? O1 C1 1.427(2) . ? O4 C8 1.387(2) . ? O4 C49 1.440(3) . ? O5 C15 1.426(2) . ? O8 C22 1.384(2) . ? O8 C72 1.445(2) . ? N1 C38 1.413(3) . ? N1 C43 1.458(3) . ? N1 C44 1.472(3) . ? N2 C61 1.422(3) . ? N2 C66 1.457(4) . ? N2 C67 1.461(4) . ? C1 C6 1.388(3) . ? C1 C2 1.388(3) . ? C2 C3 1.391(3) . ? C2 C28 1.517(3) . ? C3 C4 1.394(3) . ? C3 H3 0.9500 . ? C4 C5 1.394(3) . ? C4 C29 1.537(3) . ? C5 C6 1.393(3) . ? C5 H5 0.9500 . ? C6 C7 1.528(3) . ? C7 C9 1.512(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C13 1.393(3) . ? C8 C9 1.401(3) . ? C9 C10 1.390(3) . ? C10 C11 1.396(3) . ? C10 H10 0.9500 . ? C11 C12 1.394(3) . ? C11 C45 1.535(3) . ? C12 C13 1.398(3) . ? C12 H12 0.9500 . ? C13 C14 1.521(3) . ? C14 C16 1.520(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.393(3) . ? C15 C20 1.396(3) . ? C16 C17 1.393(3) . ? C17 C18 1.393(3) . ? C17 H17 0.9500 . ? C18 C19 1.393(3) . ? C18 C52 1.531(3) . ? C19 C20 1.386(3) . ? C19 H19 0.9500 . ? C20 C21 1.523(3) . ? C21 C23 1.523(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.397(3) . ? C22 C27 1.400(3) . ? C23 C24 1.397(3) . ? C24 C25 1.394(3) . ? C24 H24 0.9500 . ? C25 C26 1.398(3) . ? C25 C68 1.533(3) . ? C26 C27 1.386(3) . ? C26 H26 0.9500 . ? C27 C28 1.511(3) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30A 1.487(9) . ? C29 C31 1.503(5) . ? C29 C32 1.537(4) . ? C29 C31A 1.544(8) . ? C29 C30 1.569(4) . ? C29 C32A 1.571(7) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C30A H30D 0.9800 . ? C30A H30E 0.9800 . ? C30A H30F 0.9800 . ? C31A H31D 0.9800 . ? C31A H31E 0.9800 . ? C31A H31F 0.9800 . ? C32A H32D 0.9800 . ? C32A H32E 0.9800 . ? C32A H32F 0.9800 . ? C33 C34 1.371(3) . ? C33 C42 1.434(3) . ? C34 C35 1.400(3) . ? C34 H34 0.9500 . ? C35 C36 1.360(3) . ? C35 H35 0.9500 . ? C36 C37 1.418(3) . ? C36 H36 0.9500 . ? C37 C38 1.433(3) . ? C37 C42 1.436(3) . ? C38 C39 1.377(3) . ? C39 C40 1.403(4) . ? C39 H39 0.9500 . ? C40 C41 1.372(3) . ? C40 H40 0.9500 . ? C41 C42 1.420(3) . ? C41 H41 0.9500 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C48 1.526(3) . ? C45 C46 1.535(3) . ? C45 C47 1.536(3) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.474(4) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.277(4) . ? C50 H50 0.9500 . ? C51 H51A 0.9500 . ? C51 H51B 0.9500 . ? C52 C54 1.527(3) . ? C52 C53 1.533(3) . ? C52 C55 1.537(3) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C57 1.377(3) . ? C56 C65 1.431(3) . ? C57 C58 1.402(3) . ? C57 H57 0.9500 . ? C58 C59 1.364(3) . ? C58 H58 0.9500 . ? C59 C60 1.418(3) . ? C59 H59 0.9500 . ? C60 C65 1.428(3) . ? C60 C61 1.439(3) . ? C61 C62 1.377(4) . ? C62 C63 1.397(4) . ? C62 H62 0.9500 . ? C63 C64 1.365(3) . ? C63 H63 0.9500 . ? C64 C65 1.424(3) . ? C64 H64 0.9500 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 C69 1.525(4) . ? C68 C70 1.531(4) . ? C68 C71 1.540(4) . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 C73 1.488(3) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.308(4) . ? C73 H73 0.9500 . ? C74 H74A 0.9500 . ? C74 H74B 0.9500 . ? N1G C2G 1.208(7) . ? C1G C2G 1.309(7) . ? C1G O1G 1.352(5) . ? C1G H1G1 0.9900 . ? C1G H1G2 0.9900 . ? O1G H1G 0.8400 . ? 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 119.30(11) . . ? O2 S1 O1 103.93(9) . . ? O3 S1 O1 109.39(9) . . ? O2 S1 C33 112.07(10) . . ? O3 S1 C33 107.96(10) . . ? O1 S1 C33 102.88(9) . . ? O6 S2 O7 118.91(10) . . ? O6 S2 O5 104.64(9) . . ? O7 S2 O5 109.15(8) . . ? O6 S2 C56 111.07(10) . . ? O7 S2 C56 108.57(10) . . ? O5 S2 C56 103.31(9) . . ? C1 O1 S1 116.89(12) . . ? C8 O4 C49 112.81(16) . . ? C15 O5 S2 116.60(12) . . ? C22 O8 C72 114.98(15) . . ? C38 N1 C43 116.5(2) . . ? C38 N1 C44 115.80(19) . . ? C43 N1 C44 111.22(19) . . ? C61 N2 C66 115.4(3) . . ? C61 N2 C67 114.2(2) . . ? C66 N2 C67 111.2(2) . . ? C6 C1 C2 122.48(18) . . ? C6 C1 O1 119.25(17) . . ? C2 C1 O1 118.24(17) . . ? C1 C2 C3 117.74(19) . . ? C1 C2 C28 122.77(18) . . ? C3 C2 C28 119.38(18) . . ? C2 C3 C4 122.4(2) . . ? C2 C3 H3 118.8 . . ? C4 C3 H3 118.8 . . ? C3 C4 C5 117.02(19) . . ? C3 C4 C29 121.4(2) . . ? C5 C4 C29 121.5(2) . . ? C6 C5 C4 122.83(19) . . ? C6 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? C1 C6 C5 117.23(19) . . ? C1 C6 C7 122.57(18) . . ? C5 C6 C7 119.82(18) . . ? C9 C7 C6 107.90(16) . . ? C9 C7 H7A 110.1 . . ? C6 C7 H7A 110.1 . . ? C9 C7 H7B 110.1 . . ? C6 C7 H7B 110.1 . . ? H7A C7 H7B 108.4 . . ? O4 C8 C13 119.42(17) . . ? O4 C8 C9 119.35(17) . . ? C13 C8 C9 121.13(17) . . ? C10 C9 C8 118.29(18) . . ? C10 C9 C7 120.09(18) . . ? C8 C9 C7 120.96(17) . . ? C9 C10 C11 122.36(18) . . ? C9 C10 H10 118.8 . . ? C11 C10 H10 118.8 . . ? C12 C11 C10 117.60(17) . . ? C12 C11 C45 123.21(18) . . ? C10 C11 C45 119.14(17) . . ? C11 C12 C13 121.93(18) . . ? C11 C12 H12 119.0 . . ? C13 C12 H12 119.0 . . ? C8 C13 C12 118.65(18) . . ? C8 C13 C14 120.72(17) . . ? C12 C13 C14 120.40(17) . . ? C16 C14 C13 110.07(15) . . ? C16 C14 H14A 109.6 . . ? C13 C14 H14A 109.6 . . ? C16 C14 H14B 109.6 . . ? C13 C14 H14B 109.6 . . ? H14A C14 H14B 108.2 . . ? C16 C15 C20 122.59(17) . . ? C16 C15 O5 118.17(17) . . ? C20 C15 O5 119.24(16) . . ? C17 C16 C15 117.35(17) . . ? C17 C16 C14 119.53(17) . . ? C15 C16 C14 123.06(17) . . ? C18 C17 C16 122.39(18) . . ? C18 C17 H17 118.8 . . ? C16 C17 H17 118.8 . . ? C17 C18 C19 117.34(18) . . ? C17 C18 C52 123.29(18) . . ? C19 C18 C52 119.36(18) . . ? C20 C19 C18 122.92(18) . . ? C20 C19 H19 118.5 . . ? C18 C19 H19 118.5 . . ? C19 C20 C15 117.04(17) . . ? C19 C20 C21 118.39(17) . . ? C15 C20 C21 124.27(17) . . ? C20 C21 C23 108.93(15) . . ? C20 C21 H21A 109.9 . . ? C23 C21 H21A 109.9 . . ? C20 C21 H21B 109.9 . . ? C23 C21 H21B 109.9 . . ? H21A C21 H21B 108.3 . . ? O8 C22 C23 120.04(17) . . ? O8 C22 C27 118.89(17) . . ? C23 C22 C27 120.78(17) . . ? C22 C23 C24 118.54(18) . . ? C22 C23 C21 120.67(17) . . ? C24 C23 C21 120.44(18) . . ? C25 C24 C23 122.29(19) . . ? C25 C24 H24 118.9 . . ? C23 C24 H24 118.9 . . ? C24 C25 C26 117.20(18) . . ? C24 C25 C68 123.62(19) . . ? C26 C25 C68 119.15(19) . . ? C27 C26 C25 122.51(19) . . ? C27 C26 H26 118.7 . . ? C25 C26 H26 118.7 . . ? C26 C27 C22 118.67(18) . . ? C26 C27 C28 120.62(18) . . ? C22 C27 C28 120.61(17) . . ? C27 C28 C2 110.63(16) . . ? C27 C28 H28A 109.5 . . ? C2 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C2 C28 H28B 109.5 . . ? H28A C28 H28B 108.1 . . ? C30A C29 C31 141.5(6) . . ? C30A C29 C32 63.1(8) . . ? C31 C29 C32 111.6(4) . . ? C30A C29 C4 106.3(5) . . ? C31 C29 C4 110.7(3) . . ? C32 C29 C4 110.5(2) . . ? C30A C29 C31A 115.2(10) . . ? C32 C29 C31A 142.2(5) . . ? C4 C29 C31A 106.0(5) . . ? C30A C29 C30 47.3(7) . . ? C31 C29 C30 106.5(3) . . ? C32 C29 C30 104.8(3) . . ? C4 C29 C30 112.6(2) . . ? C31A C29 C30 68.6(7) . . ? C30A C29 C32A 117.2(9) . . ? C31 C29 C32A 59.4(5) . . ? C32 C29 C32A 56.6(5) . . ? C4 C29 C32A 109.2(4) . . ? C31A C29 C32A 102.4(7) . . ? C30 C29 C32A 138.1(4) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? C29 C30A H30D 109.5 . . ? C29 C30A H30E 109.5 . . ? H30D C30A H30E 109.5 . . ? C29 C30A H30F 109.5 . . ? H30D C30A H30F 109.5 . . ? H30E C30A H30F 109.5 . . ? C29 C31A H31D 109.5 . . ? C29 C31A H31E 109.5 . . ? H31D C31A H31E 109.5 . . ? C29 C31A H31F 109.5 . . ? H31D C31A H31F 109.5 . . ? H31E C31A H31F 109.5 . . ? C29 C32A H32D 109.5 . . ? C29 C32A H32E 109.5 . . ? H32D C32A H32E 109.5 . . ? C29 C32A H32F 109.5 . . ? H32D C32A H32F 109.5 . . ? H32E C32A H32F 109.5 . . ? C34 C33 C42 122.23(19) . . ? C34 C33 S1 114.66(16) . . ? C42 C33 S1 123.08(15) . . ? C33 C34 C35 119.9(2) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C36 C35 C34 120.2(2) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C35 C36 C37 121.54(19) . . ? C35 C36 H36 119.2 . . ? C37 C36 H36 119.2 . . ? C36 C37 C38 121.37(19) . . ? C36 C37 C42 119.16(19) . . ? C38 C37 C42 119.45(19) . . ? C39 C38 N1 122.6(2) . . ? C39 C38 C37 119.4(2) . . ? N1 C38 C37 117.97(19) . . ? C38 C39 C40 120.4(2) . . ? C38 C39 H39 119.8 . . ? C40 C39 H39 119.8 . . ? C41 C40 C39 121.8(2) . . ? C41 C40 H40 119.1 . . ? C39 C40 H40 119.1 . . ? C40 C41 C42 119.9(2) . . ? C40 C41 H41 120.1 . . ? C42 C41 H41 120.1 . . ? C41 C42 C33 125.07(19) . . ? C41 C42 C37 118.56(19) . . ? C33 C42 C37 116.37(18) . . ? N1 C43 H43A 109.5 . . ? N1 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N1 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N1 C44 H44A 109.5 . . ? N1 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N1 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C48 C45 C11 112.47(17) . . ? C48 C45 C46 108.33(18) . . ? C11 C45 C46 108.98(17) . . ? C48 C45 C47 108.83(18) . . ? C11 C45 C47 109.53(16) . . ? C46 C45 C47 108.62(19) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O4 C49 C50 108.8(2) . . ? O4 C49 H49A 109.9 . . ? C50 C49 H49A 109.9 . . ? O4 C49 H49B 109.9 . . ? C50 C49 H49B 109.9 . . ? H49A C49 H49B 108.3 . . ? C51 C50 C49 127.3(3) . . ? C51 C50 H50 116.3 . . ? C49 C50 H50 116.3 . . ? C50 C51 H51A 120.0 . . ? C50 C51 H51B 120.0 . . ? H51A C51 H51B 120.0 . . ? C54 C52 C18 111.97(18) . . ? C54 C52 C53 108.2(2) . . ? C18 C52 C53 109.92(19) . . ? C54 C52 C55 109.0(2) . . ? C18 C52 C55 109.03(18) . . ? C53 C52 C55 108.7(2) . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C52 C55 H55A 109.5 . . ? C52 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C52 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C57 C56 C65 121.91(19) . . ? C57 C56 S2 116.05(16) . . ? C65 C56 S2 121.95(16) . . ? C56 C57 C58 120.1(2) . . ? C56 C57 H57 119.9 . . ? C58 C57 H57 119.9 . . ? C59 C58 C57 119.9(2) . . ? C59 C58 H58 120.1 . . ? C57 C58 H58 120.1 . . ? C58 C59 C60 121.7(2) . . ? C58 C59 H59 119.2 . . ? C60 C59 H59 119.2 . . ? C59 C60 C65 119.43(19) . . ? C59 C60 C61 120.9(2) . . ? C65 C60 C61 119.6(2) . . ? C62 C61 N2 123.7(2) . . ? C62 C61 C60 118.8(2) . . ? N2 C61 C60 117.4(2) . . ? C61 C62 C63 121.1(2) . . ? C61 C62 H62 119.5 . . ? C63 C62 H62 119.5 . . ? C64 C63 C62 121.8(2) . . ? C64 C63 H63 119.1 . . ? C62 C63 H63 119.1 . . ? C63 C64 C65 119.7(2) . . ? C63 C64 H64 120.1 . . ? C65 C64 H64 120.1 . . ? C64 C65 C60 118.88(19) . . ? C64 C65 C56 124.2(2) . . ? C60 C65 C56 116.90(19) . . ? N2 C66 H66A 109.5 . . ? N2 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? N2 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N2 C67 H67A 109.5 . . ? N2 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? N2 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C69 C68 C70 108.5(2) . . ? C69 C68 C25 112.3(2) . . ? C70 C68 C25 109.3(2) . . ? C69 C68 C71 108.1(2) . . ? C70 C68 C71 110.2(3) . . ? C25 C68 C71 108.5(2) . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C68 C70 H70A 109.5 . . ? C68 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C68 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C68 C71 H71A 109.5 . . ? C68 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C68 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? O8 C72 C73 112.68(17) . . ? O8 C72 H72A 109.1 . . ? C73 C72 H72A 109.1 . . ? O8 C72 H72B 109.1 . . ? C73 C72 H72B 109.1 . . ? H72A C72 H72B 107.8 . . ? C74 C73 C72 122.9(2) . . ? C74 C73 H73 118.6 . . ? C72 C73 H73 118.6 . . ? C73 C74 H74A 120.0 . . ? C73 C74 H74B 120.0 . . ? H74A C74 H74B 120.0 . . ? C2G C1G O1G 109.6(5) . . ? C2G C1G H1G1 109.7 . . ? O1G C1G H1G1 109.7 . . ? C2G C1G H1G2 109.7 . . ? O1G C1G H1G2 109.7 . . ? H1G1 C1G H1G2 108.2 . . ? N1G C2G C1G 178.2(7) . . ? C1G O1G H1G 109.5 . . ? 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 C1 159.43(14) . . . . ? O3 S1 O1 C1 30.99(16) . . . . ? C33 S1 O1 C1 -83.58(15) . . . . ? O6 S2 O5 C15 154.52(14) . . . . ? O7 S2 O5 C15 26.23(16) . . . . ? C56 S2 O5 C15 -89.14(14) . . . . ? S1 O1 C1 C6 98.81(18) . . . . ? S1 O1 C1 C2 -83.28(19) . . . . ? C6 C1 C2 C3 -5.5(3) . . . . ? O1 C1 C2 C3 176.64(17) . . . . ? C6 C1 C2 C28 170.81(18) . . . . ? O1 C1 C2 C28 -7.0(3) . . . . ? C1 C2 C3 C4 1.0(3) . . . . ? C28 C2 C3 C4 -175.48(19) . . . . ? C2 C3 C4 C5 2.7(3) . . . . ? C2 C3 C4 C29 -179.2(2) . . . . ? C3 C4 C5 C6 -2.1(3) . . . . ? C29 C4 C5 C6 179.8(2) . . . . ? C2 C1 C6 C5 6.0(3) . . . . ? O1 C1 C6 C5 -176.17(17) . . . . ? C2 C1 C6 C7 -166.95(18) . . . . ? O1 C1 C6 C7 10.9(3) . . . . ? C4 C5 C6 C1 -2.0(3) . . . . ? C4 C5 C6 C7 171.12(19) . . . . ? C1 C6 C7 C9 114.4(2) . . . . ? C5 C6 C7 C9 -58.4(2) . . . . ? C49 O4 C8 C13 95.4(2) . . . . ? C49 O4 C8 C9 -88.2(2) . . . . ? O4 C8 C9 C10 -178.35(17) . . . . ? C13 C8 C9 C10 -2.0(3) . . . . ? O4 C8 C9 C7 -7.7(3) . . . . ? C13 C8 C9 C7 168.70(17) . . . . ? C6 C7 C9 C10 92.2(2) . . . . ? C6 C7 C9 C8 -78.3(2) . . . . ? C8 C9 C10 C11 2.4(3) . . . . ? C7 C9 C10 C11 -168.37(18) . . . . ? C9 C10 C11 C12 -1.3(3) . . . . ? C9 C10 C11 C45 176.28(18) . . . . ? C10 C11 C12 C13 -0.2(3) . . . . ? C45 C11 C12 C13 -177.72(18) . . . . ? O4 C8 C13 C12 176.90(16) . . . . ? C9 C8 C13 C12 0.5(3) . . . . ? O4 C8 C13 C14 2.4(3) . . . . ? C9 C8 C13 C14 -173.99(17) . . . . ? C11 C12 C13 C8 0.6(3) . . . . ? C11 C12 C13 C14 175.14(17) . . . . ? C8 C13 C14 C16 82.3(2) . . . . ? C12 C13 C14 C16 -92.2(2) . . . . ? S2 O5 C15 C16 -85.55(18) . . . . ? S2 O5 C15 C20 95.21(18) . . . . ? C20 C15 C16 C17 -5.5(3) . . . . ? O5 C15 C16 C17 175.29(16) . . . . ? C20 C15 C16 C14 171.67(18) . . . . ? O5 C15 C16 C14 -7.5(3) . . . . ? C13 C14 C16 C17 60.0(2) . . . . ? C13 C14 C16 C15 -117.1(2) . . . . ? C15 C16 C17 C18 0.0(3) . . . . ? C14 C16 C17 C18 -177.23(18) . . . . ? C16 C17 C18 C19 3.8(3) . . . . ? C16 C17 C18 C52 -176.60(19) . . . . ? C17 C18 C19 C20 -2.5(3) . . . . ? C52 C18 C19 C20 177.89(18) . . . . ? C18 C19 C20 C15 -2.5(3) . . . . ? C18 C19 C20 C21 171.41(18) . . . . ? C16 C15 C20 C19 6.7(3) . . . . ? O5 C15 C20 C19 -174.10(16) . . . . ? C16 C15 C20 C21 -166.87(18) . . . . ? O5 C15 C20 C21 12.3(3) . . . . ? C19 C20 C21 C23 -62.4(2) . . . . ? C15 C20 C21 C23 111.1(2) . . . . ? C72 O8 C22 C23 -78.1(2) . . . . ? C72 O8 C22 C27 108.0(2) . . . . ? O8 C22 C23 C24 -174.48(17) . . . . ? C27 C22 C23 C24 -0.7(3) . . . . ? O8 C22 C23 C21 -1.2(3) . . . . ? C27 C22 C23 C21 172.60(17) . . . . ? C20 C21 C23 C22 -74.5(2) . . . . ? C20 C21 C23 C24 98.7(2) . . . . ? C22 C23 C24 C25 0.4(3) . . . . ? C21 C23 C24 C25 -172.92(18) . . . . ? C23 C24 C25 C26 -0.6(3) . . . . ? C23 C24 C25 C68 177.3(2) . . . . ? C24 C25 C26 C27 1.2(3) . . . . ? C68 C25 C26 C27 -176.7(2) . . . . ? C25 C26 C27 C22 -1.6(3) . . . . ? C25 C26 C27 C28 174.89(19) . . . . ? O8 C22 C27 C26 175.12(17) . . . . ? C23 C22 C27 C26 1.2(3) . . . . ? O8 C22 C27 C28 -1.3(3) . . . . ? C23 C22 C27 C28 -175.20(17) . . . . ? C26 C27 C28 C2 -98.1(2) . . . . ? C22 C27 C28 C2 78.3(2) . . . . ? C1 C2 C28 C27 -118.5(2) . . . . ? C3 C2 C28 C27 57.7(2) . . . . ? C3 C4 C29 C30A -65.2(8) . . . . ? C5 C4 C29 C30A 112.8(8) . . . . ? C3 C4 C29 C31 103.9(4) . . . . ? C5 C4 C29 C31 -78.1(4) . . . . ? C3 C4 C29 C32 -132.0(3) . . . . ? C5 C4 C29 C32 46.0(4) . . . . ? C3 C4 C29 C31A 57.9(7) . . . . ? C5 C4 C29 C31A -124.1(7) . . . . ? C3 C4 C29 C30 -15.2(3) . . . . ? C5 C4 C29 C30 162.8(3) . . . . ? C3 C4 C29 C32A 167.5(6) . . . . ? C5 C4 C29 C32A -14.5(6) . . . . ? O2 S1 C33 C34 -157.32(16) . . . . ? O3 S1 C33 C34 -23.97(19) . . . . ? O1 S1 C33 C34 91.63(17) . . . . ? O2 S1 C33 C42 24.6(2) . . . . ? O3 S1 C33 C42 157.97(17) . . . . ? O1 S1 C33 C42 -86.44(18) . . . . ? C42 C33 C34 C35 2.0(3) . . . . ? S1 C33 C34 C35 -176.12(17) . . . . ? C33 C34 C35 C36 -4.3(3) . . . . ? C34 C35 C36 C37 0.1(3) . . . . ? C35 C36 C37 C38 -175.2(2) . . . . ? C35 C36 C37 C42 6.3(3) . . . . ? C43 N1 C38 C39 13.4(3) . . . . ? C44 N1 C38 C39 -120.3(3) . . . . ? C43 N1 C38 C37 -164.6(2) . . . . ? C44 N1 C38 C37 61.7(3) . . . . ? C36 C37 C38 C39 -170.9(2) . . . . ? C42 C37 C38 C39 7.5(3) . . . . ? C36 C37 C38 N1 7.1(3) . . . . ? C42 C37 C38 N1 -174.39(19) . . . . ? N1 C38 C39 C40 179.6(2) . . . . ? C37 C38 C39 C40 -2.4(4) . . . . ? C38 C39 C40 C41 -2.7(4) . . . . ? C39 C40 C41 C42 2.6(4) . . . . ? C40 C41 C42 C33 -178.3(2) . . . . ? C40 C41 C42 C37 2.6(3) . . . . ? C34 C33 C42 C41 -174.8(2) . . . . ? S1 C33 C42 C41 3.2(3) . . . . ? C34 C33 C42 C37 4.3(3) . . . . ? S1 C33 C42 C37 -177.78(15) . . . . ? C36 C37 C42 C41 170.9(2) . . . . ? C38 C37 C42 C41 -7.6(3) . . . . ? C36 C37 C42 C33 -8.3(3) . . . . ? C38 C37 C42 C33 173.25(18) . . . . ? C12 C11 C45 C48 -0.9(3) . . . . ? C10 C11 C45 C48 -178.36(18) . . . . ? C12 C11 C45 C46 119.2(2) . . . . ? C10 C11 C45 C46 -58.2(2) . . . . ? C12 C11 C45 C47 -122.1(2) . . . . ? C10 C11 C45 C47 60.5(2) . . . . ? C8 O4 C49 C50 172.7(2) . . . . ? O4 C49 C50 C51 129.5(3) . . . . ? C17 C18 C52 C54 -6.3(3) . . . . ? C19 C18 C52 C54 173.3(2) . . . . ? C17 C18 C52 C53 -126.6(2) . . . . ? C19 C18 C52 C53 53.0(3) . . . . ? C17 C18 C52 C55 114.4(2) . . . . ? C19 C18 C52 C55 -66.0(3) . . . . ? O6 S2 C56 C57 -144.23(16) . . . . ? O7 S2 C56 C57 -11.71(19) . . . . ? O5 S2 C56 C57 104.08(16) . . . . ? O6 S2 C56 C65 39.2(2) . . . . ? O7 S2 C56 C65 171.75(16) . . . . ? O5 S2 C56 C65 -72.45(17) . . . . ? C65 C56 C57 C58 1.0(3) . . . . ? S2 C56 C57 C58 -175.51(16) . . . . ? C56 C57 C58 C59 -1.6(3) . . . . ? C57 C58 C59 C60 -0.1(3) . . . . ? C58 C59 C60 C65 2.4(3) . . . . ? C58 C59 C60 C61 179.2(2) . . . . ? C66 N2 C61 C62 22.2(3) . . . . ? C67 N2 C61 C62 -108.5(3) . . . . ? C66 N2 C61 C60 -155.5(2) . . . . ? C67 N2 C61 C60 73.7(3) . . . . ? C59 C60 C61 C62 -172.7(2) . . . . ? C65 C60 C61 C62 4.1(3) . . . . ? C59 C60 C61 N2 5.2(3) . . . . ? C65 C60 C61 N2 -178.02(19) . . . . ? N2 C61 C62 C63 179.3(2) . . . . ? C60 C61 C62 C63 -3.0(4) . . . . ? C61 C62 C63 C64 -0.1(4) . . . . ? C62 C63 C64 C65 2.1(4) . . . . ? C63 C64 C65 C60 -0.9(3) . . . . ? C63 C64 C65 C56 176.5(2) . . . . ? C59 C60 C65 C64 174.63(19) . . . . ? C61 C60 C65 C64 -2.2(3) . . . . ? C59 C60 C65 C56 -2.9(3) . . . . ? C61 C60 C65 C56 -179.73(18) . . . . ? C57 C56 C65 C64 -176.1(2) . . . . ? S2 C56 C65 C64 0.2(3) . . . . ? C57 C56 C65 C60 1.2(3) . . . . ? S2 C56 C65 C60 177.54(14) . . . . ? C24 C25 C68 C69 2.3(3) . . . . ? C26 C25 C68 C69 -179.9(2) . . . . ? C24 C25 C68 C70 122.7(3) . . . . ? C26 C25 C68 C70 -59.5(3) . . . . ? C24 C25 C68 C71 -117.1(3) . . . . ? C26 C25 C68 C71 60.7(3) . . . . ? C22 O8 C72 C73 -87.5(2) . . . . ? O8 C72 C73 C74 118.3(2) . . . . ? 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 C35 H35 O1G 0.95 2.50 3.329(6) 146.6 2_556 C57 H57 O7 0.95 2.41 2.839(3) 107.3 1 C64 H64 O6 0.95 2.34 2.993(3) 125.8 1 C34 H34 O3 0.95 2.41 2.830(3) 106.4 1 C12 H12 O3 0.95 2.71 3.526(3) 144.3 2_546 C41 H41 O2 0.95 2.28 2.939(3) 125.9 1 O1G H1G O7 0.84 2.12 2.909(6) 154.0 1 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.84 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.732 _refine_diff_density_min -0.919 _refine_diff_density_rms 0.080