Supplementary Material (ESI) for Organic and Biomolecular Chemistry This journal is (C) The Royal Society of Chemistry 2006 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_Cambridge 0177 _publ_contact_author_name 'Volker Bohmer' _publ_contact_author_address # Name and address of author for correspondence ; Bohmer, Volker Abteilung Lehramt Chemie Johannes Gutenberg-University of Mainz Duesbergweg 10-14 55099 Mainz, Germany ; _publ_contact_author_email vboehmer@mail.uni-mainz.de _publ_section_title ; Hydrogen Bonding in Dimers of Tritolyl and Tritosylurea Derivatives of Triphenylmethanes ; loop_ _publ_author_name _publ_author_address Yu.Rudzevich ; Abteilung Lehramt Chemie Johannes Gutenberg-University of Mainz Duesbergweg 10-14 55099 Mainz, Germany ; V.Rudzevich ; Abteilung Lehramt Chemie Johannes Gutenberg-University of Mainz Duesbergweg 10-14 55099 Mainz, Germany ; D.Schollmeyer ; Institut of Organic Chemistry Johannes Gutenberg-University of Mainz Duesbergweg 10-14 55099 Mainz, Germany ; I.Thondorf ; Coordination and Radiochemistry University of Liege, Smart Tilman B16/B6 4000 Liege, Belgium ; 'Volker Boehmer' ; Abteilung Lehramt Chemie Johannes Gutenberg-University of Mainz Duesbergweg 10-14 55099 Mainz, Germany ; data_3a _database_code_depnum_ccdc_archive 'CCDC 614133' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C61.50 H76.50 Cl1.50 N6 O6' _chemical_formula_weight 1048.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.004(4) _cell_length_b 15.738(3) _cell_length_c 26.894(4) _cell_angle_alpha 90.00 _cell_angle_beta 122.233(5) _cell_angle_gamma 90.00 _cell_volume 12174(3) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 25 _cell_measurement_theta_max 29 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.145 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4488 _exptl_absorpt_coefficient_mu 1.170 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.5215 _exptl_absorpt_correction_T_max 0.8647 _exptl_absorpt_process_details 'Corinc (Drager, 1971)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CAD4 Enraf Nonius' _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_method \w/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 20 _diffrn_reflns_number 11539 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 70.09 _reflns_number_total 11539 _reflns_number_gt 6622 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf Nonius Software V5' _computing_cell_refinement 'Enraf Nonius Software V5' _computing_data_reduction 'Corinc (Drager, 1971)' _computing_structure_solution 'SIR-92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1934P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11539 _refine_ls_number_parameters 692 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1510 _refine_ls_R_factor_gt 0.1004 _refine_ls_wR_factor_ref 0.3260 _refine_ls_wR_factor_obs 0.2920 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.097 _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 O1 O 0.16818(9) 0.23262(19) 0.58977(13) 0.0513(7) Uani 1 1 d . . . O2 O 0.21346(10) -0.0008(2) 0.64011(13) 0.0603(8) Uani 1 1 d . . . O3 O 0.16331(9) 0.05804(19) 0.47009(12) 0.0492(7) Uani 1 1 d . . . O4 O -0.00680(10) 0.22797(19) 0.61112(13) 0.0494(7) Uani 1 1 d . . . O5 O 0.05815(10) -0.27324(19) 0.58950(13) 0.0532(7) Uani 1 1 d . . . O6 O -0.05253(9) 0.04272(18) 0.30019(11) 0.0449(7) Uani 1 1 d . . . N1 N 0.03846(12) 0.1101(2) 0.63798(15) 0.0454(8) Uani 1 1 d . . . H1N H 0.0418 0.0601 0.6513 0.055 Uiso 1 1 d R . . N2 N -0.02414(12) 0.1120(3) 0.64717(16) 0.0528(9) Uani 1 1 d . . . H2N H -0.0123 0.0586 0.6627 0.063 Uiso 1 1 d R . . N3 N 0.06242(13) -0.2180(2) 0.51372(16) 0.0523(9) Uani 1 1 d . . . H4N H 0.0486 -0.2109 0.4684 0.063 Uiso 1 1 d R . . N4 N 0.00378(13) -0.3081(3) 0.49384(16) 0.0550(9) Uani 1 1 d . . . H3N H 0.0015 -0.3124 0.4559 0.066 Uiso 1 1 d R . . N5 N -0.02225(11) 0.1469(2) 0.36935(14) 0.0501(9) Uani 1 1 d . . . H5N H -0.0313 0.1900 0.3787 0.060 Uiso 1 1 d R . . N6 N -0.10065(11) 0.1374(2) 0.30641(16) 0.0528(9) Uani 1 1 d . . . H6N H -0.1039 0.1959 0.3244 0.063 Uiso 1 1 d R . . C1 C 0.13025(12) 0.0699(3) 0.54560(16) 0.0395(8) Uani 1 1 d . . . H1 H 0.1620 0.0894 0.5572 0.047 Uiso 1 1 calc R . . C2 C 0.11611(12) 0.1230(2) 0.58109(15) 0.0367(8) Uani 1 1 d . . . C3 C 0.13565(12) 0.2020(3) 0.60135(16) 0.0413(9) Uani 1 1 d . . . C4 C 0.12550(14) 0.2510(3) 0.63690(18) 0.0460(9) Uani 1 1 d . . . C5 C 0.09260(14) 0.2200(3) 0.64794(17) 0.0442(9) Uani 1 1 d . . . H5 H 0.0845 0.2527 0.6709 0.053 Uiso 1 1 calc R . . C6 C 0.07163(13) 0.1426(3) 0.62597(16) 0.0407(9) Uani 1 1 d . . . C7 C 0.08394(13) 0.0924(3) 0.59372(16) 0.0392(8) Uani 1 1 d . . . H7 H 0.0705 0.0378 0.5804 0.047 Uiso 1 1 calc R . . C8 C 0.15030(16) 0.3333(3) 0.6634(2) 0.0598(12) Uani 1 1 d . . . H8A H 0.1840 0.3238 0.6851 0.090 Uiso 1 1 d R . . H8B H 0.1415 0.3548 0.6903 0.090 Uiso 1 1 d R . . H8C H 0.1416 0.3749 0.6320 0.090 Uiso 1 1 d R . . C9 C 0.00224(13) 0.1552(3) 0.63106(16) 0.0415(9) Uani 1 1 d . . . C10 C -0.05907(15) 0.1482(3) 0.65347(18) 0.0516(10) Uani 1 1 d . . . C11 C -0.08690(17) 0.2141(4) 0.6197(2) 0.0695(15) Uani 1 1 d . . . H11 H -0.0837 0.2361 0.5891 0.083 Uiso 1 1 calc R . . C12 C -0.11931(18) 0.2489(4) 0.6294(2) 0.0780(17) Uani 1 1 d . . . H12 H -0.1376 0.2956 0.6062 0.094 Uiso 1 1 calc R . . C13 C -0.12568(16) 0.2166(5) 0.6729(2) 0.0763(17) Uani 1 1 d . . . C14 C -0.09894(17) 0.1500(4) 0.7046(2) 0.0761(17) Uani 1 1 d . . . H14 H -0.1032 0.1265 0.7339 0.091 Uiso 1 1 calc R . . C15 C -0.06593(16) 0.1150(4) 0.6963(2) 0.0625(13) Uani 1 1 d . . . H15 H -0.0478 0.0682 0.7196 0.075 Uiso 1 1 calc R . . C16 C -0.1613(2) 0.2573(6) 0.6843(3) 0.113(3) Uani 1 1 d . . . H16A H -0.1547 0.3182 0.6919 0.170 Uiso 1 1 calc R . . H16B H -0.1590 0.2303 0.7186 0.170 Uiso 1 1 calc R . . H16C H -0.1927 0.2493 0.6498 0.170 Uiso 1 1 calc R . . C17 C 0.14801(17) 0.2800(3) 0.5360(2) 0.0580(11) Uani 1 1 d . . . H17A H 0.1419 0.3391 0.5425 0.070 Uiso 1 1 calc R . . H17B H 0.1182 0.2539 0.5057 0.070 Uiso 1 1 calc R . . C18 C 0.1819(2) 0.2792(4) 0.5158(3) 0.0756(16) Uani 1 1 d . . . H18A H 0.2117 0.3049 0.5467 0.091 Uiso 1 1 calc R . . H18B H 0.1882 0.2196 0.5102 0.091 Uiso 1 1 calc R . . C19 C 0.1638(3) 0.3271(6) 0.4594(3) 0.128(3) Uani 1 1 d . . . H19A H 0.1585 0.3872 0.4651 0.154 Uiso 1 1 calc R . . H19B H 0.1336 0.3025 0.4286 0.154 Uiso 1 1 calc R . . C20 C 0.1983(4) 0.3226(8) 0.4394(5) 0.158(4) Uani 1 1 d U . . H20A H 0.2285 0.3477 0.4696 0.190 Uiso 1 1 calc R . . H20B H 0.2035 0.2628 0.4329 0.190 Uiso 1 1 calc R . . C21 C 0.1771(6) 0.3729(12) 0.3820(8) 0.288(9) Uani 1 1 d U . . H21A H 0.1995 0.3760 0.3697 0.432 Uiso 1 1 d R . . H21B H 0.1695 0.4305 0.3881 0.432 Uiso 1 1 d R . . H21C H 0.1487 0.3444 0.3514 0.432 Uiso 1 1 d R . . C22 C 0.13453(13) -0.0241(2) 0.56165(16) 0.0383(8) Uani 1 1 d . . . C23 C 0.17563(13) -0.0553(3) 0.61009(17) 0.0452(9) Uani 1 1 d . . . C24 C 0.18058(15) -0.1402(3) 0.62686(18) 0.0497(10) Uani 1 1 d . . . C25 C 0.14222(15) -0.1932(3) 0.59560(19) 0.0519(10) Uani 1 1 d . . . H25 H 0.1445 -0.2508 0.6073 0.062 Uiso 1 1 calc R . . C26 C 0.10088(14) -0.1640(3) 0.54805(17) 0.0447(9) Uani 1 1 d . . . C27 C 0.09754(14) -0.0800(3) 0.53067(17) 0.0425(9) Uani 1 1 d . . . H27 H 0.0695 -0.0603 0.4970 0.051 Uiso 1 1 calc R . . C28 C 0.22623(17) -0.1736(4) 0.6765(2) 0.0742(15) Uani 1 1 d . . . H28A H 0.2517 -0.1478 0.6747 0.111 Uiso 1 1 d R . . H28B H 0.2272 -0.2354 0.6730 0.111 Uiso 1 1 d R . . H28C H 0.2296 -0.1593 0.7140 0.111 Uiso 1 1 d R . . C29 C 0.04249(15) -0.2678(3) 0.53565(18) 0.0475(10) Uani 1 1 d . . . C30 C -0.02150(15) -0.3721(3) 0.5015(2) 0.0551(11) Uani 1 1 d . . . C31 C -0.02341(19) -0.3810(4) 0.5516(2) 0.0684(14) Uani 1 1 d . . . H31 H -0.0069 -0.3424 0.5834 0.082 Uiso 1 1 calc R . . C32 C -0.0486(2) -0.4444(4) 0.5553(3) 0.0746(15) Uani 1 1 d . . . H32 H -0.0498 -0.4487 0.5897 0.090 Uiso 1 1 calc R . . C33 C -0.07312(17) -0.5039(3) 0.5101(3) 0.0662(13) Uani 1 1 d . . . C34 C -0.07161(17) -0.4939(3) 0.4609(2) 0.0647(13) Uani 1 1 d . . . H34 H -0.0887 -0.5319 0.4288 0.078 Uiso 1 1 calc R . . C35 C -0.04594(16) -0.4301(3) 0.4564(2) 0.0599(12) Uani 1 1 d . . . H35 H -0.0450 -0.4257 0.4218 0.072 Uiso 1 1 calc R . . C36 C -0.0995(2) -0.5759(4) 0.5172(3) 0.0885(18) Uani 1 1 d . . . H36A H -0.1108 -0.5569 0.5422 0.133 Uiso 1 1 d R . . H36B H -0.0788 -0.6247 0.5356 0.133 Uiso 1 1 d R . . H36C H -0.1260 -0.5924 0.4786 0.133 Uiso 1 1 d R . . C37 C 0.21958(18) 0.0340(4) 0.6914(2) 0.0695(14) Uani 1 1 d . . . H37A H 0.2230 -0.0119 0.7186 0.083 Uiso 1 1 calc R . . H37B H 0.1922 0.0687 0.6820 0.083 Uiso 1 1 calc R . . C38 C 0.2636(2) 0.0899(4) 0.7206(3) 0.0898(19) Uani 1 1 d . . . H38A H 0.2612 0.1315 0.6915 0.108 Uiso 1 1 calc R . . H38B H 0.2653 0.1221 0.7533 0.108 Uiso 1 1 calc R . . C39 C 0.30645(18) 0.0405(4) 0.7433(2) 0.0775(16) Uani 1 1 d . . . H39A H 0.3069 0.0154 0.7099 0.093 Uiso 1 1 calc R . . H39B H 0.3065 -0.0067 0.7677 0.093 Uiso 1 1 calc R . . C40 C 0.3504(3) 0.0936(5) 0.7802(4) 0.127(3) Uani 1 1 d . . . H40A H 0.3484 0.1443 0.7572 0.152 Uiso 1 1 calc R . . H40B H 0.3514 0.1136 0.8157 0.152 Uiso 1 1 calc R . . C41 C 0.3938(3) 0.0492(7) 0.7986(4) 0.160(5) Uani 1 1 d . . . H41A H 0.4200 0.0881 0.8210 0.240 Uiso 1 1 d R . . H41B H 0.3934 0.0292 0.7638 0.240 Uiso 1 1 d R . . H41C H 0.3971 0.0005 0.8232 0.240 Uiso 1 1 d R . . C42 C 0.09890(13) 0.0857(2) 0.48006(16) 0.0391(8) Uani 1 1 d . . . C43 C 0.11705(13) 0.0793(3) 0.44408(18) 0.0430(9) Uani 1 1 d . . . C44 C 0.09050(15) 0.1003(3) 0.38398(18) 0.0483(10) Uani 1 1 d . . . C45 C 0.04423(15) 0.1197(3) 0.35949(17) 0.0480(10) Uani 1 1 d . . . H45 H 0.0252 0.1303 0.3185 0.058 Uiso 1 1 calc R . . C46 C 0.02463(14) 0.1240(3) 0.39380(17) 0.0448(9) Uani 1 1 d . . . C47 C 0.05248(13) 0.1077(3) 0.45404(17) 0.0416(9) Uani 1 1 d . . . H47 H 0.0394 0.1118 0.4776 0.050 Uiso 1 1 calc R . . C48 C 0.11241(18) 0.1041(4) 0.3479(2) 0.0646(13) Uani 1 1 d . . . H48A H 0.1458 0.1153 0.3737 0.097 Uiso 1 1 d R . . H48B H 0.0979 0.1497 0.3187 0.097 Uiso 1 1 d R . . H48C H 0.1078 0.0497 0.3278 0.097 Uiso 1 1 d R . . C49 C -0.05838(13) 0.1053(3) 0.32318(16) 0.0413(9) Uani 1 1 d . . . C50 C -0.14421(14) 0.1056(3) 0.26011(18) 0.0481(10) Uani 1 1 d . . . C51 C -0.15273(16) 0.0197(3) 0.2468(2) 0.0652(13) Uani 1 1 d . . . H51 H -0.1288 -0.0206 0.2690 0.078 Uiso 1 1 calc R . . C52 C -0.19558(18) -0.0073(4) 0.2017(3) 0.0731(15) Uani 1 1 d . . . H52 H -0.2007 -0.0663 0.1929 0.088 Uiso 1 1 calc R . . C53 C -0.23107(15) 0.0488(3) 0.16910(19) 0.0563(11) Uani 1 1 d . . . C54 C -0.22262(18) 0.1322(4) 0.1818(2) 0.0736(15) Uani 1 1 d . . . H54 H -0.2468 0.1722 0.1598 0.088 Uiso 1 1 calc R . . C55 C -0.17975(17) 0.1606(3) 0.2260(2) 0.0698(14) Uani 1 1 d . . . H55 H -0.1747 0.2199 0.2331 0.084 Uiso 1 1 calc R . . C56 C -0.27807(18) 0.0165(4) 0.1208(2) 0.0798(17) Uani 1 1 d . . . H56A H -0.2786 -0.0457 0.1224 0.120 Uiso 1 1 d R . . H56B H -0.2838 0.0342 0.0825 0.120 Uiso 1 1 d R . . H56C H -0.3023 0.0401 0.1261 0.120 Uiso 1 1 d R . . C57 C 0.17042(15) -0.0268(3) 0.4566(2) 0.0587(12) Uani 1 1 d . . . H57A H 0.1534 -0.0346 0.4135 0.070 Uiso 1 1 calc R . . H57B H 0.1584 -0.0685 0.4728 0.070 Uiso 1 1 calc R . . C58 C 0.22101(17) -0.0406(4) 0.4827(2) 0.0681(14) Uani 1 1 d . . . H58A H 0.2364 -0.0467 0.5259 0.082 Uiso 1 1 calc R . . H58B H 0.2343 0.0101 0.4752 0.082 Uiso 1 1 calc R . . C59 C 0.23168(19) -0.1175(4) 0.4590(3) 0.0778(15) Uani 1 1 d . . . H59A H 0.2129 -0.1657 0.4589 0.093 Uiso 1 1 calc R . . H59B H 0.2217 -0.1062 0.4177 0.093 Uiso 1 1 calc R . . C60 C 0.2813(2) -0.1435(4) 0.4918(3) 0.0865(18) Uani 1 1 d . . . H60A H 0.2898 -0.1638 0.5312 0.104 Uiso 1 1 calc R . . H60B H 0.3005 -0.0927 0.4977 0.104 Uiso 1 1 calc R . . C61 C 0.2933(2) -0.2111(5) 0.4631(3) 0.097(2) Uani 1 1 d . . . H61A H 0.3268 -0.2224 0.4870 0.145 Uiso 1 1 d R . . H61B H 0.2848 -0.1921 0.4239 0.145 Uiso 1 1 d R . . H61C H 0.2762 -0.2632 0.4597 0.145 Uiso 1 1 d R . . C1L C 0.0000 0.3549(5) 0.2500 0.179(6) Uani 1 2 d SDU . . H1L H -0.0104 0.4156 0.2440 0.215 Uiso 0.50 1 d PR . . Cl1 Cl -0.0357(2) 0.3024(5) 0.2662(3) 0.192(3) Uani 0.50 1 d PDU . . Cl2 Cl -0.0066(4) 0.3226(8) 0.1861(3) 0.298(5) Uani 0.50 1 d PDU . . Cl3 Cl 0.0564(2) 0.3527(7) 0.3073(3) 0.298(5) Uani 0.50 1 d PDU . . 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 O1 0.0421(15) 0.0617(18) 0.0533(18) -0.0021(14) 0.0277(13) -0.0080(13) O2 0.0473(17) 0.077(2) 0.0409(17) -0.0057(15) 0.0133(13) -0.0006(15) O3 0.0429(15) 0.0662(19) 0.0456(16) -0.0089(14) 0.0284(13) -0.0009(13) O4 0.0517(16) 0.0535(17) 0.0475(17) 0.0035(13) 0.0295(14) 0.0036(13) O5 0.0602(18) 0.0619(18) 0.0419(17) -0.0019(14) 0.0302(14) 0.0042(14) O6 0.0501(15) 0.0567(17) 0.0333(14) -0.0016(12) 0.0259(12) 0.0056(13) N1 0.057(2) 0.0470(18) 0.046(2) 0.0034(15) 0.0360(17) 0.0034(16) N2 0.057(2) 0.063(2) 0.053(2) 0.0090(17) 0.0385(18) 0.0034(17) N3 0.066(2) 0.050(2) 0.0403(19) -0.0010(16) 0.0281(17) -0.0047(17) N4 0.058(2) 0.064(2) 0.042(2) -0.0008(17) 0.0263(17) -0.0056(18) N5 0.0449(18) 0.063(2) 0.0384(19) -0.0054(16) 0.0193(15) 0.0148(16) N6 0.0432(18) 0.064(2) 0.046(2) -0.0058(17) 0.0204(16) 0.0089(16) C1 0.0363(18) 0.055(2) 0.0305(19) -0.0037(16) 0.0201(15) 0.0004(16) C2 0.0338(17) 0.052(2) 0.0244(17) -0.0004(15) 0.0155(14) -0.0009(16) C3 0.0368(19) 0.056(2) 0.0325(19) 0.0007(17) 0.0192(16) 0.0010(17) C4 0.044(2) 0.049(2) 0.037(2) -0.0048(17) 0.0167(17) -0.0010(17) C5 0.049(2) 0.052(2) 0.034(2) -0.0060(17) 0.0233(17) 0.0017(18) C6 0.042(2) 0.054(2) 0.0307(19) 0.0009(16) 0.0225(16) 0.0026(17) C7 0.045(2) 0.048(2) 0.0296(19) -0.0035(15) 0.0227(16) -0.0014(16) C8 0.056(3) 0.065(3) 0.055(3) -0.020(2) 0.027(2) -0.014(2) C9 0.045(2) 0.054(2) 0.0282(19) -0.0048(17) 0.0216(16) -0.0010(18) C10 0.048(2) 0.077(3) 0.035(2) 0.000(2) 0.0252(19) 0.000(2) C11 0.057(3) 0.109(4) 0.054(3) 0.018(3) 0.038(2) 0.020(3) C12 0.062(3) 0.116(5) 0.065(3) 0.020(3) 0.040(3) 0.028(3) C13 0.045(2) 0.149(6) 0.039(3) -0.006(3) 0.025(2) 0.009(3) C14 0.053(3) 0.143(5) 0.043(3) 0.008(3) 0.033(2) -0.002(3) C15 0.049(2) 0.104(4) 0.040(2) 0.009(2) 0.027(2) -0.003(2) C16 0.070(4) 0.206(9) 0.079(4) -0.009(5) 0.050(3) 0.024(5) C17 0.066(3) 0.064(3) 0.046(3) 0.000(2) 0.031(2) -0.015(2) C18 0.087(4) 0.090(4) 0.075(4) -0.012(3) 0.060(3) -0.028(3) C19 0.139(7) 0.187(8) 0.087(5) 0.008(5) 0.080(5) -0.057(6) C20 0.164(5) 0.167(5) 0.155(5) 0.009(3) 0.092(3) -0.011(3) C21 0.289(9) 0.291(9) 0.286(9) 0.005(3) 0.155(5) -0.004(3) C22 0.0420(19) 0.049(2) 0.0292(19) -0.0008(15) 0.0226(16) 0.0039(16) C23 0.042(2) 0.063(3) 0.036(2) -0.0016(18) 0.0242(17) 0.0080(18) C24 0.051(2) 0.061(3) 0.038(2) -0.0024(19) 0.0236(19) 0.012(2) C25 0.058(2) 0.056(2) 0.046(2) 0.001(2) 0.031(2) 0.011(2) C26 0.054(2) 0.050(2) 0.037(2) -0.0050(17) 0.0281(18) 0.0018(18) C27 0.044(2) 0.050(2) 0.035(2) -0.0004(17) 0.0222(17) 0.0018(17) C28 0.061(3) 0.075(3) 0.064(3) 0.010(3) 0.018(3) 0.019(3) C29 0.053(2) 0.049(2) 0.041(2) -0.0052(18) 0.0258(19) 0.0071(19) C30 0.053(2) 0.060(3) 0.050(3) -0.002(2) 0.026(2) 0.005(2) C31 0.079(3) 0.075(3) 0.063(3) -0.017(3) 0.045(3) -0.019(3) C32 0.084(4) 0.089(4) 0.067(3) -0.011(3) 0.051(3) -0.015(3) C33 0.054(3) 0.062(3) 0.079(4) 0.003(3) 0.033(3) -0.001(2) C34 0.056(3) 0.063(3) 0.066(3) -0.011(2) 0.027(2) -0.003(2) C35 0.053(2) 0.069(3) 0.050(3) -0.003(2) 0.022(2) 0.001(2) C36 0.086(4) 0.076(4) 0.117(5) -0.004(4) 0.063(4) -0.013(3) C37 0.063(3) 0.089(4) 0.049(3) -0.002(3) 0.025(2) 0.008(3) C38 0.093(4) 0.072(4) 0.063(4) 0.000(3) 0.013(3) 0.002(3) C39 0.065(3) 0.088(4) 0.057(3) 0.013(3) 0.018(3) -0.007(3) C40 0.096(5) 0.099(5) 0.106(6) 0.017(4) 0.001(4) -0.014(4) C41 0.080(5) 0.213(11) 0.114(7) 0.050(7) 0.003(5) -0.053(6) C42 0.045(2) 0.049(2) 0.0292(19) -0.0040(16) 0.0239(16) -0.0017(16) C43 0.043(2) 0.054(2) 0.041(2) -0.0042(18) 0.0287(18) -0.0014(17) C44 0.055(2) 0.065(3) 0.036(2) -0.0046(18) 0.0315(19) -0.005(2) C45 0.057(2) 0.066(3) 0.0251(19) -0.0013(18) 0.0250(18) 0.003(2) C46 0.046(2) 0.055(2) 0.036(2) -0.0044(17) 0.0234(18) 0.0032(18) C47 0.045(2) 0.052(2) 0.034(2) -0.0025(17) 0.0247(17) 0.0025(17) C48 0.071(3) 0.097(4) 0.050(3) -0.002(3) 0.048(2) -0.004(3) C49 0.046(2) 0.052(2) 0.0274(19) 0.0084(16) 0.0212(16) 0.0101(17) C50 0.044(2) 0.065(3) 0.040(2) -0.0005(19) 0.0251(18) 0.0097(19) C51 0.049(3) 0.070(3) 0.062(3) 0.009(2) 0.020(2) 0.006(2) C52 0.062(3) 0.070(3) 0.073(4) -0.002(3) 0.026(3) -0.002(3) C53 0.046(2) 0.079(3) 0.044(2) -0.006(2) 0.024(2) 0.007(2) C54 0.056(3) 0.082(4) 0.059(3) 0.004(3) 0.015(2) 0.026(3) C55 0.063(3) 0.062(3) 0.070(3) -0.005(2) 0.026(3) 0.015(2) C56 0.057(3) 0.106(4) 0.063(3) -0.014(3) 0.023(3) 0.013(3) C57 0.051(2) 0.069(3) 0.062(3) -0.012(2) 0.034(2) 0.003(2) C58 0.056(3) 0.083(4) 0.070(3) -0.006(3) 0.037(3) 0.006(3) C59 0.069(3) 0.088(4) 0.077(4) 0.007(3) 0.040(3) 0.006(3) C60 0.076(4) 0.107(5) 0.089(4) 0.007(4) 0.053(3) 0.013(3) C61 0.097(5) 0.105(5) 0.110(5) -0.001(4) 0.069(4) 0.020(4) C1L 0.180(7) 0.180(7) 0.177(7) 0.000 0.095(4) 0.000 Cl1 0.191(3) 0.190(4) 0.206(4) 0.009(3) 0.113(3) 0.018(3) Cl2 0.312(6) 0.299(6) 0.288(6) 0.001(3) 0.163(4) -0.006(3) Cl3 0.297(6) 0.299(6) 0.293(6) 0.001(3) 0.153(4) 0.003(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 O1 C3 1.386(4) . ? O1 C17 1.434(5) . ? O2 C23 1.390(5) . ? O2 C37 1.392(6) . ? O3 C43 1.379(5) . ? O3 C57 1.437(5) . ? O4 C9 1.232(5) . ? O5 C29 1.251(5) . ? O6 C49 1.234(5) . ? N1 C9 1.346(5) . ? N1 C6 1.424(5) . ? N1 H1N 0.8477 . ? N2 C9 1.367(5) . ? N2 C10 1.406(5) . ? N2 H2N 0.9291 . ? N3 C29 1.360(5) . ? N3 C26 1.412(5) . ? N3 H4N 1.0516 . ? N4 C29 1.349(5) . ? N4 C30 1.409(6) . ? N4 H3N 0.9837 . ? N5 C49 1.361(5) . ? N5 C46 1.409(5) . ? N5 H5N 0.8366 . ? N6 C49 1.354(5) . ? N6 C50 1.424(5) . ? N6 H6N 1.0729 . ? C1 C42 1.517(5) . ? C1 C22 1.526(6) . ? C1 C2 1.526(5) . ? C1 H1 1.0000 . ? C2 C3 1.377(5) . ? C2 C7 1.393(5) . ? C3 C4 1.408(6) . ? C4 C5 1.390(6) . ? C4 C8 1.501(6) . ? C5 C6 1.376(6) . ? C5 H5 0.9500 . ? C6 C7 1.393(5) . ? C7 H7 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C10 C11 1.371(7) . ? C10 C15 1.392(6) . ? C11 C12 1.374(7) . ? C11 H11 0.9500 . ? C12 C13 1.394(8) . ? C12 H12 0.9500 . ? C13 C14 1.350(8) . ? C13 C16 1.539(7) . ? C14 C15 1.372(7) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.515(7) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.500(9) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.533(12) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.530(18) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C27 1.390(5) . ? C22 C23 1.396(5) . ? C23 C24 1.392(6) . ? C24 C25 1.390(6) . ? C24 C28 1.502(6) . ? C25 C26 1.380(6) . ? C25 H25 0.9500 . ? C26 C27 1.388(6) . ? C27 H27 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C30 C35 1.385(6) . ? C30 C31 1.390(7) . ? C31 C32 1.353(7) . ? C31 H31 0.9500 . ? C32 C33 1.403(8) . ? C32 H32 0.9500 . ? C33 C34 1.361(8) . ? C33 C36 1.520(7) . ? C34 C35 1.378(7) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.542(8) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.466(8) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.527(9) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.460(12) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C47 1.387(5) . ? C42 C43 1.402(5) . ? C43 C44 1.407(6) . ? C44 C45 1.377(6) . ? C44 C48 1.507(5) . ? C45 C46 1.399(5) . ? C45 H45 0.9500 . ? C46 C47 1.397(6) . ? C47 H47 0.9500 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C50 C55 1.366(6) . ? C50 C51 1.389(7) . ? C51 C52 1.375(7) . ? C51 H51 0.9500 . ? C52 C53 1.370(7) . ? C52 H52 0.9500 . ? C53 C54 1.349(7) . ? C53 C56 1.512(7) . ? C54 C55 1.375(7) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.487(6) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.500(8) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.484(8) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.495(9) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C1L Cl2 1.689(6) . ? C1L Cl2 1.689(6) 2 ? C1L Cl3 1.703(6) 2 ? C1L Cl3 1.703(6) . ? C1L Cl1 1.706(5) . ? C1L Cl1 1.706(5) 2 ? C1L H1L 1.0004 . ? Cl1 Cl2 1.358(10) 2 ? Cl1 Cl3 1.884(10) 2 ? Cl2 Cl1 1.358(10) 2 ? Cl2 Cl3 1.855(8) 2 ? Cl3 Cl2 1.855(8) 2 ? Cl3 Cl1 1.884(10) 2 ? 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 C3 O1 C17 113.4(3) . . ? C23 O2 C37 114.9(4) . . ? C43 O3 C57 113.4(3) . . ? C9 N1 C6 123.8(3) . . ? C9 N1 H1N 117.1 . . ? C6 N1 H1N 119.1 . . ? C9 N2 C10 125.2(4) . . ? C9 N2 H2N 113.1 . . ? C10 N2 H2N 120.1 . . ? C29 N3 C26 124.4(4) . . ? C29 N3 H4N 123.1 . . ? C26 N3 H4N 112.2 . . ? C29 N4 C30 127.9(4) . . ? C29 N4 H3N 113.5 . . ? C30 N4 H3N 112.7 . . ? C49 N5 C46 123.2(3) . . ? C49 N5 H5N 111.4 . . ? C46 N5 H5N 125.1 . . ? C49 N6 C50 125.8(4) . . ? C49 N6 H6N 121.1 . . ? C50 N6 H6N 112.8 . . ? C42 C1 C22 112.9(3) . . ? C42 C1 C2 112.1(3) . . ? C22 C1 C2 111.6(3) . . ? C42 C1 H1 106.6 . . ? C22 C1 H1 106.6 . . ? C2 C1 H1 106.6 . . ? C3 C2 C7 119.4(3) . . ? C3 C2 C1 119.7(3) . . ? C7 C2 C1 120.9(3) . . ? C2 C3 O1 120.0(3) . . ? C2 C3 C4 121.5(4) . . ? O1 C3 C4 118.4(4) . . ? C5 C4 C3 118.0(4) . . ? C5 C4 C8 120.9(4) . . ? C3 C4 C8 121.0(4) . . ? C6 C5 C4 120.7(4) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 120.7(4) . . ? C5 C6 N1 120.9(3) . . ? C7 C6 N1 118.4(4) . . ? C6 C7 C2 119.5(4) . . ? C6 C7 H7 120.3 . . ? C2 C7 H7 120.3 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O4 C9 N1 123.2(4) . . ? O4 C9 N2 123.1(4) . . ? N1 C9 N2 113.6(4) . . ? C11 C10 C15 118.1(4) . . ? C11 C10 N2 123.7(4) . . ? C15 C10 N2 118.2(4) . . ? C10 C11 C12 121.0(5) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C11 C12 C13 120.8(5) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C14 C13 C12 117.4(5) . . ? C14 C13 C16 122.2(5) . . ? C12 C13 C16 120.4(6) . . ? C13 C14 C15 122.8(5) . . ? C13 C14 H14 118.6 . . ? C15 C14 H14 118.6 . . ? C14 C15 C10 119.8(5) . . ? C14 C15 H15 120.1 . . ? C10 C15 H15 120.1 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O1 C17 C18 108.1(4) . . ? O1 C17 H17A 110.1 . . ? C18 C17 H17A 110.1 . . ? O1 C17 H17B 110.1 . . ? C18 C17 H17B 110.1 . . ? H17A C17 H17B 108.4 . . ? C19 C18 C17 112.2(5) . . ? C19 C18 H18A 109.2 . . ? C17 C18 H18A 109.2 . . ? C19 C18 H18B 109.2 . . ? C17 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? C18 C19 C20 110.7(8) . . ? C18 C19 H19A 109.5 . . ? C20 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? C21 C20 C19 107.1(11) . . ? C21 C20 H20A 110.3 . . ? C19 C20 H20A 110.3 . . ? C21 C20 H20B 110.3 . . ? C19 C20 H20B 110.3 . . ? H20A C20 H20B 108.6 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.4 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C27 C22 C23 118.2(4) . . ? C27 C22 C1 121.6(3) . . ? C23 C22 C1 120.1(4) . . ? O2 C23 C24 119.3(4) . . ? O2 C23 C22 118.7(4) . . ? C24 C23 C22 121.9(4) . . ? C25 C24 C23 117.9(4) . . ? C25 C24 C28 121.3(4) . . ? C23 C24 C28 120.8(4) . . ? C26 C25 C24 121.7(4) . . ? C26 C25 H25 119.2 . . ? C24 C25 H25 119.2 . . ? C25 C26 C27 119.3(4) . . ? C25 C26 N3 122.5(4) . . ? C27 C26 N3 118.1(4) . . ? C26 C27 C22 121.1(4) . . ? C26 C27 H27 119.5 . . ? C22 C27 H27 119.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O5 C29 N4 123.8(4) . . ? O5 C29 N3 122.6(4) . . ? N4 C29 N3 113.6(4) . . ? C35 C30 C31 117.8(5) . . ? C35 C30 N4 118.1(4) . . ? C31 C30 N4 124.1(4) . . ? C32 C31 C30 120.2(5) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C31 C32 C33 122.4(5) . . ? C31 C32 H32 118.8 . . ? C33 C32 H32 118.8 . . ? C34 C33 C32 116.9(5) . . ? C34 C33 C36 122.7(5) . . ? C32 C33 C36 120.3(5) . . ? C33 C34 C35 121.5(5) . . ? C33 C34 H34 119.2 . . ? C35 C34 H34 119.2 . . ? C34 C35 C30 121.1(5) . . ? C34 C35 H35 119.5 . . ? C30 C35 H35 119.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O2 C37 C38 108.7(5) . . ? O2 C37 H37A 109.9 . . ? C38 C37 H37A 109.9 . . ? O2 C37 H37B 109.9 . . ? C38 C37 H37B 109.9 . . ? H37A C37 H37B 108.3 . . ? C39 C38 C37 112.9(5) . . ? C39 C38 H38A 109.0 . . ? C37 C38 H38A 109.0 . . ? C39 C38 H38B 109.0 . . ? C37 C38 H38B 109.0 . . ? H38A C38 H38B 107.8 . . ? C38 C39 C40 113.1(6) . . ? C38 C39 H39A 109.0 . . ? C40 C39 H39A 109.0 . . ? C38 C39 H39B 109.0 . . ? C40 C39 H39B 109.0 . . ? H39A C39 H39B 107.8 . . ? C41 C40 C39 114.9(7) . . ? C41 C40 H40A 108.5 . . ? C39 C40 H40A 108.5 . . ? C41 C40 H40B 108.5 . . ? C39 C40 H40B 108.5 . . ? H40A C40 H40B 107.5 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C47 C42 C43 118.1(3) . . ? C47 C42 C1 122.2(3) . . ? C43 C42 C1 119.7(3) . . ? O3 C43 C42 118.0(3) . . ? O3 C43 C44 119.9(3) . . ? C42 C43 C44 121.8(4) . . ? C45 C44 C43 118.1(3) . . ? C45 C44 C48 120.9(4) . . ? C43 C44 C48 120.9(4) . . ? C44 C45 C46 121.3(4) . . ? C44 C45 H45 119.3 . . ? C46 C45 H45 119.3 . . ? C47 C46 C45 119.3(4) . . ? C47 C46 N5 119.1(3) . . ? C45 C46 N5 121.5(4) . . ? C42 C47 C46 121.1(3) . . ? C42 C47 H47 119.5 . . ? C46 C47 H47 119.5 . . ? C44 C48 H48A 109.5 . . ? C44 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C44 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O6 C49 N6 123.9(4) . . ? O6 C49 N5 122.2(3) . . ? N6 C49 N5 113.9(3) . . ? C55 C50 C51 117.1(4) . . ? C55 C50 N6 120.0(4) . . ? C51 C50 N6 123.0(4) . . ? C52 C51 C50 120.4(5) . . ? C52 C51 H51 119.8 . . ? C50 C51 H51 119.8 . . ? C53 C52 C51 121.5(5) . . ? C53 C52 H52 119.3 . . ? C51 C52 H52 119.3 . . ? C54 C53 C52 118.0(5) . . ? C54 C53 C56 122.0(5) . . ? C52 C53 C56 120.0(5) . . ? C53 C54 C55 121.3(5) . . ? C53 C54 H54 119.3 . . ? C55 C54 H54 119.3 . . ? C50 C55 C54 121.7(5) . . ? C50 C55 H55 119.2 . . ? C54 C55 H55 119.2 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O3 C57 C58 109.0(4) . . ? O3 C57 H57A 109.9 . . ? C58 C57 H57A 109.9 . . ? O3 C57 H57B 109.9 . . ? C58 C57 H57B 109.9 . . ? H57A C57 H57B 108.3 . . ? C57 C58 C59 113.5(5) . . ? C57 C58 H58A 108.9 . . ? C59 C58 H58A 108.9 . . ? C57 C58 H58B 108.9 . . ? C59 C58 H58B 108.9 . . ? H58A C58 H58B 107.7 . . ? C60 C59 C58 115.1(5) . . ? C60 C59 H59A 108.5 . . ? C58 C59 H59A 108.5 . . ? C60 C59 H59B 108.5 . . ? C58 C59 H59B 108.5 . . ? H59A C59 H59B 107.5 . . ? C59 C60 C61 115.2(6) . . ? C59 C60 H60A 108.5 . . ? C61 C60 H60A 108.5 . . ? C59 C60 H60B 108.5 . . ? C61 C60 H60B 108.5 . . ? H60A C60 H60B 107.5 . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? Cl2 C1L Cl2 145.0(7) . 2 ? Cl2 C1L Cl3 66.3(2) . 2 ? Cl2 C1L Cl3 112.90(18) 2 2 ? Cl2 C1L Cl3 112.90(18) . . ? Cl2 C1L Cl3 66.3(2) 2 . ? Cl3 C1L Cl3 177.6(7) 2 . ? Cl2 C1L Cl1 112.85(19) . . ? Cl2 C1L Cl1 47.2(3) 2 . ? Cl3 C1L Cl1 67.1(3) 2 . ? Cl3 C1L Cl1 111.66(18) . . ? Cl2 C1L Cl1 47.2(3) . 2 ? Cl2 C1L Cl1 112.85(19) 2 2 ? Cl3 C1L Cl1 111.66(18) 2 2 ? Cl3 C1L Cl1 67.1(3) . 2 ? Cl1 C1L Cl1 122.1(6) . 2 ? Cl2 C1L H1L 106.3 . . ? Cl2 C1L H1L 107.1 2 . ? Cl3 C1L H1L 75.2 2 . ? Cl3 C1L H1L 107.2 . . ? Cl1 C1L H1L 105.3 . . ? Cl1 C1L H1L 131.3 2 . ? Cl2 Cl1 C1L 65.8(2) 2 . ? Cl2 Cl1 Cl3 120.5(3) 2 2 ? C1L Cl1 Cl3 56.37(18) . 2 ? Cl1 Cl2 C1L 67.1(2) 2 . ? Cl1 Cl2 Cl3 122.0(3) 2 2 ? C1L Cl2 Cl3 57.19(14) . 2 ? C1L Cl3 Cl2 56.49(13) . 2 ? C1L Cl3 Cl1 56.53(17) . 2 ? Cl2 Cl3 Cl1 98.3(4) 2 2 ? 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 C42 C1 C2 C3 -91.2(4) . . . . ? C22 C1 C2 C3 141.0(3) . . . . ? C42 C1 C2 C7 89.3(4) . . . . ? C22 C1 C2 C7 -38.5(5) . . . . ? C7 C2 C3 O1 179.1(3) . . . . ? C1 C2 C3 O1 -0.4(5) . . . . ? C7 C2 C3 C4 3.0(6) . . . . ? C1 C2 C3 C4 -176.5(4) . . . . ? C17 O1 C3 C2 90.1(4) . . . . ? C17 O1 C3 C4 -93.7(4) . . . . ? C2 C3 C4 C5 -4.3(6) . . . . ? O1 C3 C4 C5 179.6(3) . . . . ? C2 C3 C4 C8 174.3(4) . . . . ? O1 C3 C4 C8 -1.9(6) . . . . ? C3 C4 C5 C6 1.7(6) . . . . ? C8 C4 C5 C6 -176.8(4) . . . . ? C4 C5 C6 C7 2.0(6) . . . . ? C4 C5 C6 N1 179.0(4) . . . . ? C9 N1 C6 C5 49.1(6) . . . . ? C9 N1 C6 C7 -133.8(4) . . . . ? C5 C6 C7 C2 -3.3(6) . . . . ? N1 C6 C7 C2 179.6(3) . . . . ? C3 C2 C7 C6 0.8(6) . . . . ? C1 C2 C7 C6 -179.7(3) . . . . ? C6 N1 C9 O4 3.3(6) . . . . ? C6 N1 C9 N2 -177.9(3) . . . . ? C10 N2 C9 O4 -12.1(6) . . . . ? C10 N2 C9 N1 169.1(4) . . . . ? C9 N2 C10 C11 33.3(7) . . . . ? C9 N2 C10 C15 -147.0(4) . . . . ? C15 C10 C11 C12 2.7(8) . . . . ? N2 C10 C11 C12 -177.6(5) . . . . ? C10 C11 C12 C13 -1.8(10) . . . . ? C11 C12 C13 C14 -0.2(9) . . . . ? C11 C12 C13 C16 178.6(6) . . . . ? C12 C13 C14 C15 1.1(9) . . . . ? C16 C13 C14 C15 -177.6(6) . . . . ? C13 C14 C15 C10 -0.1(9) . . . . ? C11 C10 C15 C14 -1.8(8) . . . . ? N2 C10 C15 C14 178.4(5) . . . . ? C3 O1 C17 C18 -157.5(4) . . . . ? O1 C17 C18 C19 179.8(5) . . . . ? C17 C18 C19 C20 -178.3(7) . . . . ? C18 C19 C20 C21 -180.0(10) . . . . ? C42 C1 C22 C27 -34.3(5) . . . . ? C2 C1 C22 C27 93.1(4) . . . . ? C42 C1 C22 C23 148.6(3) . . . . ? C2 C1 C22 C23 -84.1(4) . . . . ? C37 O2 C23 C24 -84.4(5) . . . . ? C37 O2 C23 C22 99.4(5) . . . . ? C27 C22 C23 O2 177.6(3) . . . . ? C1 C22 C23 O2 -5.2(5) . . . . ? C27 C22 C23 C24 1.5(6) . . . . ? C1 C22 C23 C24 178.7(3) . . . . ? O2 C23 C24 C25 -179.4(4) . . . . ? C22 C23 C24 C25 -3.3(6) . . . . ? O2 C23 C24 C28 -0.5(6) . . . . ? C22 C23 C24 C28 175.6(4) . . . . ? C23 C24 C25 C26 2.3(6) . . . . ? C28 C24 C25 C26 -176.6(4) . . . . ? C24 C25 C26 C27 0.5(6) . . . . ? C24 C25 C26 N3 176.3(4) . . . . ? C29 N3 C26 C25 54.9(6) . . . . ? C29 N3 C26 C27 -129.2(4) . . . . ? C25 C26 C27 C22 -2.4(6) . . . . ? N3 C26 C27 C22 -178.4(3) . . . . ? C23 C22 C27 C26 1.4(6) . . . . ? C1 C22 C27 C26 -175.7(3) . . . . ? C30 N4 C29 O5 -11.0(7) . . . . ? C30 N4 C29 N3 171.0(4) . . . . ? C26 N3 C29 O5 -3.4(6) . . . . ? C26 N3 C29 N4 174.6(4) . . . . ? C29 N4 C30 C35 -151.7(4) . . . . ? C29 N4 C30 C31 28.1(7) . . . . ? C35 C30 C31 C32 -0.2(8) . . . . ? N4 C30 C31 C32 179.9(5) . . . . ? C30 C31 C32 C33 0.9(9) . . . . ? C31 C32 C33 C34 -1.9(9) . . . . ? C31 C32 C33 C36 177.8(6) . . . . ? C32 C33 C34 C35 2.2(8) . . . . ? C36 C33 C34 C35 -177.5(5) . . . . ? C33 C34 C35 C30 -1.6(8) . . . . ? C31 C30 C35 C34 0.5(7) . . . . ? N4 C30 C35 C34 -179.6(4) . . . . ? C23 O2 C37 C38 178.0(4) . . . . ? O2 C37 C38 C39 -67.8(6) . . . . ? C37 C38 C39 C40 -171.4(6) . . . . ? C38 C39 C40 C41 -173.9(7) . . . . ? C22 C1 C42 C47 96.6(4) . . . . ? C2 C1 C42 C47 -30.5(5) . . . . ? C22 C1 C42 C43 -84.5(4) . . . . ? C2 C1 C42 C43 148.4(4) . . . . ? C57 O3 C43 C42 107.9(4) . . . . ? C57 O3 C43 C44 -77.0(5) . . . . ? C47 C42 C43 O3 179.5(4) . . . . ? C1 C42 C43 O3 0.5(6) . . . . ? C47 C42 C43 C44 4.5(6) . . . . ? C1 C42 C43 C44 -174.5(4) . . . . ? O3 C43 C44 C45 178.8(4) . . . . ? C42 C43 C44 C45 -6.2(6) . . . . ? O3 C43 C44 C48 -3.0(6) . . . . ? C42 C43 C44 C48 172.0(4) . . . . ? C43 C44 C45 C46 4.1(7) . . . . ? C48 C44 C45 C46 -174.1(4) . . . . ? C44 C45 C46 C47 -0.5(7) . . . . ? C44 C45 C46 N5 177.5(4) . . . . ? C49 N5 C46 C47 -125.7(4) . . . . ? C49 N5 C46 C45 56.3(6) . . . . ? C43 C42 C47 C46 -0.6(6) . . . . ? C1 C42 C47 C46 178.4(4) . . . . ? C45 C46 C47 C42 -1.4(6) . . . . ? N5 C46 C47 C42 -179.4(4) . . . . ? C50 N6 C49 O6 -0.8(7) . . . . ? C50 N6 C49 N5 -179.1(4) . . . . ? C46 N5 C49 O6 1.7(6) . . . . ? C46 N5 C49 N6 180.0(4) . . . . ? C49 N6 C50 C55 -144.2(5) . . . . ? C49 N6 C50 C51 35.1(7) . . . . ? C55 C50 C51 C52 -1.0(8) . . . . ? N6 C50 C51 C52 179.7(5) . . . . ? C50 C51 C52 C53 -0.7(9) . . . . ? C51 C52 C53 C54 1.1(9) . . . . ? C51 C52 C53 C56 -178.5(5) . . . . ? C52 C53 C54 C55 0.1(9) . . . . ? C56 C53 C54 C55 179.7(5) . . . . ? C51 C50 C55 C54 2.2(8) . . . . ? N6 C50 C55 C54 -178.5(5) . . . . ? C53 C54 C55 C50 -1.8(9) . . . . ? C43 O3 C57 C58 175.5(4) . . . . ? O3 C57 C58 C59 -165.2(4) . . . . ? C57 C58 C59 C60 -168.4(5) . . . . ? C58 C59 C60 C61 -170.8(6) . . . . ? 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 N1 H1N O6 0.85 1.99 2.816(4) 166.1 5_556 N2 H2N O6 0.93 2.46 3.285(5) 147.9 5_556 N3 H4N O4 1.05 1.85 2.846(5) 156.3 5_556 N4 H3N O4 0.98 2.32 3.143(5) 140.3 5_556 N5 H5N O5 0.84 2.03 2.848(4) 166.1 5_556 N6 H6N O5 1.07 2.33 3.191(5) 136.3 5_556 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 70.09 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.942 _refine_diff_density_min -0.962 _refine_diff_density_rms 0.081 data_3b _database_code_depnum_ccdc_archive 'CCDC 614134' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H78 Cl6 N6 O12 S3' _chemical_formula_weight 1420.19 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' Cl Cl 0.1484 0.1585 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.3620(6) _cell_length_b 14.7300(6) _cell_length_c 18.9930(6) _cell_angle_alpha 67.8510(10) _cell_angle_beta 70.2640(10) _cell_angle_gamma 80.3860(10) _cell_volume 3499.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 0.397 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8769 _exptl_absorpt_correction_T_max 0.9429 _exptl_absorpt_process_details 'Corinc (Drager, 1971)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'sealed Tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kappa CCD' _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_method 'CCD Scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62249 _diffrn_reflns_av_R_equivalents 0.1462 _diffrn_reflns_av_sigmaI/netI 0.1075 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 4.04 _diffrn_reflns_theta_max 27.50 _reflns_number_total 15692 _reflns_number_gt 8539 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SIR-92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1309P)^2^+5.0895P] 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 15692 _refine_ls_number_parameters 847 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.1602 _refine_ls_R_factor_gt 0.0909 _refine_ls_wR_factor_ref 0.2816 _refine_ls_wR_factor_obs 0.2362 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.166 _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 0.76227(11) 0.86515(10) 0.35556(10) 0.0479(4) Uani 1 1 d . . . S2 S 0.23404(11) 0.47336(10) 0.79990(8) 0.0397(3) Uani 1 1 d . . . S3 S 0.76400(10) 0.16991(9) 0.55505(9) 0.0359(3) Uani 1 1 d . . . O1 O 0.2670(3) 0.7088(3) 0.2346(2) 0.0383(8) Uani 1 1 d . . . O2 O 0.1958(3) 0.3988(2) 0.3601(2) 0.0385(9) Uani 1 1 d . . . O3 O 0.4355(3) 0.4679(3) 0.1875(2) 0.0459(10) Uani 1 1 d . . . O4 O 0.5536(3) 0.8354(2) 0.3712(2) 0.0391(9) Uani 1 1 d . . . O5 O 0.1892(3) 0.3891(2) 0.6948(2) 0.0401(9) Uani 1 1 d . . . O6 O 0.7149(3) 0.2882(2) 0.4058(2) 0.0385(8) Uani 1 1 d . . . O7 O 0.8620(3) 0.8303(3) 0.3533(3) 0.0588(12) Uani 1 1 d . . . O8 O 0.7441(3) 0.9532(3) 0.2944(3) 0.0579(12) Uani 1 1 d . . . O9 O 0.2775(3) 0.3763(3) 0.8129(2) 0.0482(10) Uani 1 1 d . . . O10 O 0.2772(3) 0.5445(3) 0.8121(2) 0.0468(10) Uani 1 1 d . . . O12 O 0.8048(3) 0.2622(2) 0.5343(2) 0.0408(9) Uani 1 1 d . . . O13 O 0.7397(3) 0.1035(3) 0.6358(2) 0.0429(9) Uani 1 1 d . . . N1 N 0.6084(3) 0.7212(3) 0.3092(3) 0.0349(10) Uani 1 1 d . . . H1N H 0.6604 0.6873 0.2878 0.042 Uiso 1 1 d R . . N2 N 0.7129(3) 0.7719(3) 0.3552(3) 0.0404(11) Uani 1 1 d . . . H2N H 0.7531 0.7250 0.3405 0.048 Uiso 1 1 d R . . N3 N 0.1973(3) 0.5381(3) 0.5942(3) 0.0350(10) Uani 1 1 d . . . H3N H 0.2167 0.6032 0.5807 0.042 Uiso 1 1 d R . . N4 N 0.2353(4) 0.5238(3) 0.7060(3) 0.0409(11) Uani 1 1 d . . . H4N H 0.2580 0.5814 0.6839 0.049 Uiso 1 1 d R . . N5 N 0.5498(3) 0.2544(3) 0.4599(3) 0.0341(9) Uani 1 1 d . . . H5N H 0.4985 0.2310 0.5140 0.041 Uiso 1 1 d R . . N6 N 0.6563(3) 0.1898(3) 0.5360(3) 0.0355(10) Uani 1 1 d . . . H6N H 0.6064 0.1858 0.5803 0.043 Uiso 1 1 d R . . C1 C 0.3453(4) 0.5268(3) 0.3214(3) 0.0327(11) Uani 1 1 d . . . H1 H 0.3143 0.5337 0.2797 0.039 Uiso 1 1 calc R . . C2 C 0.3922(4) 0.6245(3) 0.2982(3) 0.0320(11) Uani 1 1 d . . . C3 C 0.3496(4) 0.7121(4) 0.2562(3) 0.0345(11) Uani 1 1 d . . . C4 C 0.3917(4) 0.8034(4) 0.2307(3) 0.0399(12) Uani 1 1 d . . . C5 C 0.4763(4) 0.8054(4) 0.2506(3) 0.0389(12) Uani 1 1 d . . . H5 H 0.5052 0.8661 0.2352 0.047 Uiso 1 1 calc R . . C6 C 0.5186(4) 0.7188(4) 0.2930(3) 0.0364(12) Uani 1 1 d . . . C7 C 0.4780(4) 0.6300(3) 0.3153(3) 0.0335(11) Uani 1 1 d . . . H7 H 0.5089 0.5715 0.3428 0.040 Uiso 1 1 calc R . . C8 C 0.3484(5) 0.8967(4) 0.1815(4) 0.0528(16) Uani 1 1 d . . . H8A H 0.3350 0.8853 0.1383 0.079 Uiso 1 1 calc R . . H8B H 0.3957 0.9487 0.1589 0.079 Uiso 1 1 calc R . . H8C H 0.2866 0.9167 0.2155 0.079 Uiso 1 1 calc R . . C9 C 0.6195(4) 0.7797(3) 0.3451(3) 0.0366(12) Uani 1 1 d . . . C10 C 0.6996(4) 0.8781(4) 0.4484(4) 0.0430(14) Uani 1 1 d . . . C11 C 0.7088(4) 0.8049(4) 0.5171(4) 0.0465(15) Uani 1 1 d . . . H11 H 0.7452 0.7455 0.5145 0.056 Uiso 1 1 calc R . . C12 C 0.6650(4) 0.8175(4) 0.5900(4) 0.0492(15) Uani 1 1 d . . . H12 H 0.6714 0.7667 0.6374 0.059 Uiso 1 1 calc R . . C13 C 0.6112(4) 0.9052(4) 0.5944(4) 0.0471(15) Uani 1 1 d . . . C14 C 0.6038(4) 0.9785(4) 0.5234(4) 0.0493(16) Uani 1 1 d . . . H14 H 0.5676 1.0381 0.5254 0.059 Uiso 1 1 calc R . . C15 C 0.6476(4) 0.9666(4) 0.4507(4) 0.0477(15) Uani 1 1 d . . . H15 H 0.6426 1.0175 0.4030 0.057 Uiso 1 1 calc R . . C16 C 0.5645(5) 0.9202(5) 0.6725(4) 0.0593(18) Uani 1 1 d . . . H16A H 0.5576 0.8564 0.7157 0.089 Uiso 1 1 calc R . . H16B H 0.4990 0.9531 0.6740 0.089 Uiso 1 1 calc R . . H16C H 0.6063 0.9608 0.6790 0.089 Uiso 1 1 calc R . . C17 C 0.1739(4) 0.7321(4) 0.2855(4) 0.0459(14) Uani 1 1 d . . . H17A H 0.1787 0.7923 0.2953 0.055 Uiso 1 1 calc R . . H17B H 0.1565 0.6778 0.3374 0.055 Uiso 1 1 calc R . . C18 C 0.0954(5) 0.7477(5) 0.2453(4) 0.0524(16) Uani 1 1 d . . . H18A H 0.0298 0.7548 0.2832 0.063 Uiso 1 1 calc R . . H18B H 0.0952 0.6889 0.2320 0.063 Uiso 1 1 calc R . . C19 C 0.1101(6) 0.8378(5) 0.1694(5) 0.071(2) Uani 1 1 d . . . H19A H 0.1707 0.8274 0.1282 0.085 Uiso 1 1 calc R . . H19B H 0.1186 0.8959 0.1806 0.085 Uiso 1 1 calc R . . C20 C 0.0148(9) 0.8575(8) 0.1366(7) 0.110(3) Uani 1 1 d U . . H20A H 0.0043 0.7978 0.1285 0.132 Uiso 1 1 calc R . . H20B H -0.0451 0.8711 0.1770 0.132 Uiso 1 1 calc R . . C21 C 0.0286(14) 0.9372(14) 0.0644(11) 0.193(7) Uani 1 1 d U . . H21A H -0.0256 0.9419 0.0426 0.290 Uiso 1 1 calc R . . H21B H 0.0918 0.9272 0.0263 0.290 Uiso 1 1 calc R . . H21C H 0.0292 0.9979 0.0740 0.290 Uiso 1 1 calc R . . C22 C 0.2636(4) 0.5015(3) 0.4014(3) 0.0315(11) Uani 1 1 d . . . C23 C 0.1894(4) 0.4375(3) 0.4178(3) 0.0343(11) Uani 1 1 d . . . C24 C 0.1167(4) 0.4066(3) 0.4915(3) 0.0353(11) Uani 1 1 d . . . C25 C 0.1194(4) 0.4404(3) 0.5507(3) 0.0354(12) Uani 1 1 d . . . H25 H 0.0711 0.4207 0.6016 0.043 Uiso 1 1 calc R . . C26 C 0.1923(4) 0.5026(3) 0.5353(3) 0.0342(11) Uani 1 1 d . . . C27 C 0.2633(4) 0.5331(3) 0.4614(3) 0.0318(11) Uani 1 1 d . . . H27 H 0.3121 0.5761 0.4519 0.038 Uiso 1 1 calc R . . C28 C 0.0389(4) 0.3379(4) 0.5082(4) 0.0439(13) Uani 1 1 d . . . H28A H 0.0297 0.2886 0.5616 0.066 Uiso 1 1 calc R . . H28B H 0.0602 0.3053 0.4685 0.066 Uiso 1 1 calc R . . H28C H -0.0237 0.3753 0.5052 0.066 Uiso 1 1 calc R . . C29 C 0.2052(4) 0.4776(4) 0.6656(3) 0.0354(12) Uani 1 1 d . . . C30 C 0.1080(4) 0.4663(4) 0.8558(3) 0.0372(12) Uani 1 1 d . . . C31 C 0.0587(4) 0.5488(4) 0.8716(4) 0.0444(13) Uani 1 1 d . . . H31 H 0.0925 0.6077 0.8522 0.053 Uiso 1 1 calc R . . C32 C -0.0406(5) 0.5447(5) 0.9159(4) 0.0526(15) Uani 1 1 d . . . H32 H -0.0749 0.6012 0.9268 0.063 Uiso 1 1 calc R . . C33 C -0.0906(5) 0.4584(6) 0.9446(4) 0.0565(17) Uani 1 1 d . . . C34 C -0.0391(5) 0.3770(6) 0.9282(4) 0.067(2) Uani 1 1 d . . . H34 H -0.0724 0.3178 0.9479 0.081 Uiso 1 1 calc R . . C35 C 0.0601(5) 0.3796(5) 0.8837(4) 0.0552(17) Uani 1 1 d . . . H35 H 0.0945 0.3232 0.8726 0.066 Uiso 1 1 calc R . . C36 C -0.2005(5) 0.4544(8) 0.9939(5) 0.082(3) Uani 1 1 d . . . H36A H -0.2375 0.4282 0.9713 0.124 Uiso 1 1 calc R . . H36B H -0.2270 0.5206 0.9925 0.124 Uiso 1 1 calc R . . H36C H -0.2072 0.4118 1.0491 0.124 Uiso 1 1 calc R . . C37 C 0.1355(6) 0.4495(5) 0.3081(4) 0.0592(18) Uani 1 1 d . . . H37A H 0.1360 0.5214 0.2939 0.071 Uiso 1 1 calc R . . H37B H 0.0663 0.4290 0.3343 0.071 Uiso 1 1 calc R . . C38 C 0.1827(9) 0.4201(8) 0.2332(6) 0.105(3) Uani 1 1 d . . . H38A H 0.1476 0.4588 0.1937 0.126 Uiso 1 1 calc R . . H38B H 0.2521 0.4403 0.2101 0.126 Uiso 1 1 calc R . . C39 C 0.1833(8) 0.3220(7) 0.2423(6) 0.096(3) Uani 1 1 d . . . H39A H 0.1133 0.3087 0.2540 0.115 Uiso 1 1 calc R . . H39B H 0.2009 0.2848 0.2920 0.115 Uiso 1 1 calc R . . C40 C 0.2385(9) 0.2746(7) 0.1875(6) 0.102(3) Uani 1 1 d . . . H40A H 0.3081 0.2921 0.1721 0.122 Uiso 1 1 calc R . . H40B H 0.2167 0.3076 0.1393 0.122 Uiso 1 1 calc R . . C41 C 0.2424(10) 0.1711(9) 0.2014(9) 0.136(5) Uani 1 1 d . . . H41A H 0.3012 0.1543 0.1628 0.204 Uiso 1 1 calc R . . H41B H 0.1829 0.1546 0.1954 0.204 Uiso 1 1 calc R . . H41C H 0.2459 0.1339 0.2556 0.204 Uiso 1 1 calc R . . C42 C 0.4230(4) 0.4416(4) 0.3227(3) 0.0337(11) Uani 1 1 d . . . C43 C 0.4668(4) 0.4166(4) 0.2542(3) 0.0373(12) Uani 1 1 d . . . C44 C 0.5348(4) 0.3371(4) 0.2527(3) 0.0375(12) Uani 1 1 d . . . C45 C 0.5620(4) 0.2845(4) 0.3215(3) 0.0367(12) Uani 1 1 d . . . H45 H 0.6083 0.2303 0.3220 0.044 Uiso 1 1 calc R . . C46 C 0.5229(4) 0.3099(3) 0.3888(3) 0.0319(11) Uani 1 1 d . . . C47 C 0.4522(3) 0.3874(3) 0.3901(3) 0.0297(10) Uani 1 1 d . . . H47 H 0.4239 0.4031 0.4373 0.036 Uiso 1 1 calc R . . C48 C 0.5770(4) 0.3096(4) 0.1797(4) 0.0447(14) Uani 1 1 d . . . H48A H 0.5265 0.3213 0.1528 0.067 Uiso 1 1 calc R . . H48B H 0.5984 0.2400 0.1948 0.067 Uiso 1 1 calc R . . H48C H 0.6340 0.3494 0.1437 0.067 Uiso 1 1 calc R . . C49 C 0.6443(4) 0.2485(3) 0.4625(3) 0.0331(11) Uani 1 1 d . . . C50 C 0.8435(4) 0.1102(4) 0.4913(4) 0.0386(13) Uani 1 1 d . . . C51 C 0.8442(4) 0.0074(4) 0.5163(4) 0.0397(13) Uani 1 1 d . . . H51 H 0.8021 -0.0291 0.5668 0.048 Uiso 1 1 calc R . . C52 C 0.9069(4) -0.0393(4) 0.4666(4) 0.0483(16) Uani 1 1 d . . . H52 H 0.9072 -0.1088 0.4830 0.058 Uiso 1 1 calc R . . C53 C 0.9698(4) 0.0122(4) 0.3928(4) 0.0489(16) Uani 1 1 d . . . C54 C 0.9692(4) 0.1153(4) 0.3701(4) 0.0475(14) Uani 1 1 d . . . H54 H 1.0127 0.1517 0.3203 0.057 Uiso 1 1 calc R . . C55 C 0.9074(4) 0.1633(4) 0.4184(4) 0.0432(13) Uani 1 1 d . . . H55 H 0.9080 0.2326 0.4024 0.052 Uiso 1 1 calc R . . C56 C 1.0370(5) -0.0385(5) 0.3380(5) 0.064(2) Uani 1 1 d . . . H56A H 1.1033 -0.0129 0.3173 0.096 Uiso 1 1 calc R . . H56B H 1.0111 -0.0267 0.2936 0.096 Uiso 1 1 calc R . . H56C H 1.0405 -0.1092 0.3673 0.096 Uiso 1 1 calc R . . C57 C 0.4945(6) 0.5490(5) 0.1308(4) 0.0587(18) Uani 1 1 d . . . H57A H 0.5550 0.5261 0.0964 0.070 Uiso 1 1 calc R . . H57B H 0.5140 0.5846 0.1582 0.070 Uiso 1 1 calc R . . C58 C 0.4257(9) 0.6173(6) 0.0796(5) 0.098(3) Uani 1 1 d . . . H58A H 0.4120 0.5813 0.0497 0.118 Uiso 1 1 calc R . . H58B H 0.3617 0.6304 0.1164 0.118 Uiso 1 1 calc R . . C59 C 0.4658(10) 0.7091(7) 0.0243(7) 0.117(4) Uani 1 1 d . . . H59A H 0.5249 0.6964 -0.0171 0.140 Uiso 1 1 calc R . . H59B H 0.4879 0.7413 0.0528 0.140 Uiso 1 1 calc R . . C60 C 0.3936(9) 0.7799(7) -0.0168(6) 0.100(3) Uani 1 1 d . . . H60A H 0.3615 0.7449 -0.0371 0.120 Uiso 1 1 calc R . . H60B H 0.3414 0.8046 0.0222 0.120 Uiso 1 1 calc R . . C61 C 0.4479(12) 0.8651(9) -0.0850(8) 0.142(5) Uani 1 1 d . . . H61A H 0.3999 0.9142 -0.1062 0.213 Uiso 1 1 calc R . . H61B H 0.4928 0.8417 -0.1271 0.213 Uiso 1 1 calc R . . H61C H 0.4862 0.8949 -0.0659 0.213 Uiso 1 1 calc R . . C1L C 0.8725(5) 0.1320(5) 0.1831(4) 0.0603(18) Uani 1 1 d D . . H1L H 0.8725 0.0606 0.2159 0.072 Uiso 1 1 calc R . . Cl1L Cl 0.81184(14) 0.19785(14) 0.24684(13) 0.0725(6) Uani 1 1 d D . . Cl2L Cl 0.81176(18) 0.14970(17) 0.11278(13) 0.0875(7) Uani 1 1 d D . . Cl3L Cl 0.99695(16) 0.1661(2) 0.13550(18) 0.1085(9) Uani 1 1 d D . . C5L C 0.6909(6) 0.8337(8) 0.0713(5) 0.117(4) Uani 1 1 d D . . H5L H 0.6454 0.7833 0.1152 0.140 Uiso 1 1 d R A . Cl6A Cl 0.7584(5) 0.8698(5) 0.1059(5) 0.123(2) Uani 0.50 1 d PDU A 1 Cl7A Cl 0.5939(7) 0.8891(7) 0.0282(6) 0.142(4) Uani 0.50 1 d PDU A 1 Cl8A Cl 0.8050(5) 0.8407(5) -0.0013(4) 0.1241(19) Uani 0.50 1 d PDU A 1 Cl6L Cl 0.7217(4) 0.9087(4) 0.1307(3) 0.0764(12) Uani 0.50 1 d PDU A 2 Cl7L Cl 0.6088(4) 0.9215(3) 0.0300(3) 0.0649(11) Uani 0.50 1 d PDU A 2 Cl8L Cl 0.7646(4) 0.7625(4) 0.0005(3) 0.1040(15) Uani 0.50 1 d PDU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0388(8) 0.0337(7) 0.0672(11) -0.0160(7) -0.0101(7) -0.0067(6) S2 0.0424(8) 0.0410(7) 0.0332(7) -0.0136(6) -0.0058(6) -0.0051(6) S3 0.0361(7) 0.0265(6) 0.0461(8) -0.0125(6) -0.0166(6) 0.0049(5) O1 0.041(2) 0.0370(19) 0.037(2) -0.0117(16) -0.0183(17) 0.0096(16) O2 0.045(2) 0.0330(18) 0.047(2) -0.0172(17) -0.0255(18) 0.0064(16) O3 0.054(2) 0.054(2) 0.034(2) -0.0183(19) -0.0174(19) 0.0049(19) O4 0.035(2) 0.0308(18) 0.048(2) -0.0130(17) -0.0102(17) 0.0018(15) O5 0.050(2) 0.0264(17) 0.039(2) -0.0080(16) -0.0110(18) -0.0041(16) O6 0.037(2) 0.0326(18) 0.043(2) -0.0106(16) -0.0121(18) 0.0008(15) O7 0.031(2) 0.054(2) 0.094(4) -0.033(3) -0.013(2) -0.0064(18) O8 0.060(3) 0.032(2) 0.065(3) -0.002(2) -0.012(2) -0.0118(19) O9 0.051(2) 0.047(2) 0.043(2) -0.0157(19) -0.013(2) 0.0078(18) O10 0.047(2) 0.056(2) 0.039(2) -0.0194(19) -0.0049(19) -0.0152(19) O12 0.041(2) 0.0279(17) 0.057(3) -0.0176(17) -0.0168(19) 0.0007(15) O13 0.041(2) 0.0368(19) 0.046(2) -0.0070(17) -0.0173(18) 0.0031(16) N1 0.034(2) 0.027(2) 0.038(3) -0.0098(19) -0.0073(19) 0.0008(17) N2 0.034(2) 0.030(2) 0.058(3) -0.018(2) -0.012(2) 0.0000(18) N3 0.044(3) 0.0250(19) 0.034(2) -0.0118(18) -0.006(2) -0.0028(18) N4 0.053(3) 0.037(2) 0.031(2) -0.012(2) -0.004(2) -0.014(2) N5 0.034(2) 0.028(2) 0.036(2) -0.0075(18) -0.0099(19) 0.0018(17) N6 0.034(2) 0.031(2) 0.037(3) -0.0104(19) -0.0090(19) 0.0037(18) C1 0.039(3) 0.027(2) 0.034(3) -0.010(2) -0.016(2) 0.003(2) C2 0.040(3) 0.025(2) 0.025(3) -0.0051(19) -0.008(2) 0.004(2) C3 0.040(3) 0.034(3) 0.026(3) -0.011(2) -0.010(2) 0.006(2) C4 0.048(3) 0.034(3) 0.030(3) -0.006(2) -0.010(2) 0.001(2) C5 0.044(3) 0.030(2) 0.034(3) -0.005(2) -0.009(2) -0.002(2) C6 0.036(3) 0.035(3) 0.032(3) -0.009(2) -0.008(2) 0.003(2) C7 0.039(3) 0.027(2) 0.030(3) -0.007(2) -0.011(2) 0.005(2) C8 0.060(4) 0.034(3) 0.049(4) 0.004(3) -0.021(3) 0.005(3) C9 0.039(3) 0.024(2) 0.036(3) -0.002(2) -0.006(2) -0.006(2) C10 0.033(3) 0.032(3) 0.069(4) -0.019(3) -0.020(3) -0.001(2) C11 0.037(3) 0.028(3) 0.070(4) -0.016(3) -0.012(3) 0.001(2) C12 0.040(3) 0.028(3) 0.078(5) -0.016(3) -0.020(3) 0.000(2) C13 0.036(3) 0.039(3) 0.076(5) -0.028(3) -0.020(3) -0.002(2) C14 0.045(3) 0.029(3) 0.092(5) -0.029(3) -0.040(3) 0.011(2) C15 0.043(3) 0.032(3) 0.076(5) -0.020(3) -0.027(3) 0.001(2) C16 0.052(4) 0.048(3) 0.084(5) -0.032(4) -0.017(4) -0.004(3) C17 0.046(3) 0.047(3) 0.042(3) -0.013(3) -0.019(3) 0.011(3) C18 0.052(4) 0.051(3) 0.062(4) -0.020(3) -0.035(3) 0.017(3) C19 0.088(6) 0.066(4) 0.068(5) -0.024(4) -0.049(4) 0.025(4) C20 0.124(4) 0.104(4) 0.109(4) -0.031(3) -0.046(3) -0.010(3) C21 0.196(8) 0.194(8) 0.193(8) -0.068(4) -0.059(4) -0.012(3) C22 0.030(2) 0.025(2) 0.038(3) -0.010(2) -0.013(2) 0.0047(19) C23 0.039(3) 0.027(2) 0.041(3) -0.014(2) -0.020(2) 0.009(2) C24 0.036(3) 0.024(2) 0.046(3) -0.011(2) -0.016(2) 0.004(2) C25 0.037(3) 0.025(2) 0.037(3) -0.008(2) -0.006(2) 0.001(2) C26 0.039(3) 0.024(2) 0.038(3) -0.014(2) -0.009(2) 0.004(2) C27 0.034(3) 0.023(2) 0.039(3) -0.011(2) -0.013(2) 0.0028(19) C28 0.044(3) 0.032(3) 0.057(4) -0.014(3) -0.019(3) -0.002(2) C29 0.035(3) 0.032(3) 0.032(3) -0.015(2) 0.001(2) 0.001(2) C30 0.040(3) 0.045(3) 0.028(3) -0.012(2) -0.009(2) -0.010(2) C31 0.042(3) 0.050(3) 0.043(3) -0.017(3) -0.013(3) -0.004(3) C32 0.049(4) 0.065(4) 0.046(4) -0.021(3) -0.015(3) -0.001(3) C33 0.043(3) 0.096(5) 0.029(3) -0.019(3) -0.009(3) -0.012(3) C34 0.057(4) 0.075(5) 0.060(5) -0.018(4) 0.000(4) -0.027(4) C35 0.056(4) 0.048(3) 0.055(4) -0.019(3) -0.002(3) -0.016(3) C36 0.049(4) 0.141(8) 0.047(4) -0.025(5) -0.002(3) -0.020(5) C37 0.079(5) 0.054(4) 0.070(5) -0.034(4) -0.052(4) 0.025(3) C38 0.138(9) 0.110(8) 0.108(8) -0.049(6) -0.094(7) 0.032(6) C39 0.120(8) 0.101(7) 0.120(8) -0.077(6) -0.080(7) 0.040(6) C40 0.146(10) 0.086(6) 0.104(8) -0.054(6) -0.064(7) 0.022(6) C41 0.144(11) 0.116(9) 0.193(14) -0.079(9) -0.097(10) 0.039(8) C42 0.035(3) 0.030(2) 0.034(3) -0.014(2) -0.008(2) 0.002(2) C43 0.039(3) 0.040(3) 0.034(3) -0.014(2) -0.011(2) -0.003(2) C44 0.033(3) 0.038(3) 0.045(3) -0.024(3) -0.006(2) -0.003(2) C45 0.030(3) 0.034(3) 0.042(3) -0.017(2) -0.001(2) 0.001(2) C46 0.030(2) 0.028(2) 0.038(3) -0.011(2) -0.013(2) 0.0011(19) C47 0.029(2) 0.028(2) 0.034(3) -0.015(2) -0.008(2) 0.0024(19) C48 0.042(3) 0.049(3) 0.046(4) -0.029(3) -0.005(3) 0.000(3) C49 0.034(3) 0.021(2) 0.043(3) -0.012(2) -0.011(2) 0.0042(19) C50 0.031(3) 0.034(3) 0.060(4) -0.022(3) -0.020(3) 0.006(2) C51 0.032(3) 0.026(2) 0.067(4) -0.017(3) -0.022(3) 0.000(2) C52 0.040(3) 0.033(3) 0.086(5) -0.031(3) -0.031(3) 0.010(2) C53 0.036(3) 0.052(3) 0.078(5) -0.041(3) -0.024(3) 0.010(3) C54 0.037(3) 0.046(3) 0.057(4) -0.023(3) -0.010(3) 0.004(2) C55 0.035(3) 0.034(3) 0.057(4) -0.015(3) -0.012(3) 0.001(2) C56 0.043(4) 0.070(4) 0.100(6) -0.057(4) -0.026(4) 0.013(3) C57 0.092(5) 0.047(3) 0.038(4) -0.012(3) -0.024(4) -0.002(3) C58 0.168(10) 0.075(6) 0.070(6) -0.006(5) -0.061(6) -0.044(6) C59 0.182(12) 0.085(7) 0.109(8) -0.016(6) -0.090(9) -0.019(7) C60 0.160(10) 0.085(6) 0.078(6) -0.041(5) -0.066(7) 0.030(6) C61 0.224(16) 0.106(9) 0.137(11) -0.032(8) -0.121(12) 0.006(9) C1L 0.057(4) 0.042(3) 0.065(5) -0.003(3) -0.012(3) -0.007(3) Cl1L 0.0566(10) 0.0708(11) 0.0943(15) -0.0381(11) -0.0158(10) -0.0055(9) Cl2L 0.0940(16) 0.0924(15) 0.0694(14) -0.0233(12) -0.0268(12) 0.0066(12) Cl3L 0.0556(12) 0.1077(18) 0.134(2) -0.0363(17) 0.0072(13) -0.0196(12) C5L 0.075(6) 0.154(10) 0.058(5) 0.010(6) -0.016(5) 0.038(6) Cl6A 0.119(3) 0.108(3) 0.134(4) -0.036(3) -0.034(3) -0.009(2) Cl7A 0.138(4) 0.145(5) 0.129(4) -0.032(3) -0.051(3) 0.016(3) Cl8A 0.118(3) 0.139(3) 0.104(3) -0.042(2) -0.023(2) -0.002(3) Cl6L 0.070(2) 0.081(2) 0.070(2) -0.0149(18) -0.0195(18) -0.0149(18) Cl7L 0.084(2) 0.0535(18) 0.060(2) -0.0033(16) -0.0442(18) -0.0037(17) Cl8L 0.095(3) 0.118(3) 0.076(2) -0.027(2) -0.017(2) 0.022(2) _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 O7 1.430(4) . ? S1 O8 1.434(4) . ? S1 N2 1.650(4) . ? S1 C10 1.755(7) . ? S2 O10 1.425(4) . ? S2 O9 1.426(4) . ? S2 N4 1.647(5) . ? S2 C30 1.760(6) . ? S3 O12 1.432(4) . ? S3 O13 1.433(4) . ? S3 N6 1.660(5) . ? S3 C50 1.754(5) . ? O1 C3 1.393(6) . ? O1 C17 1.437(7) . ? O2 C23 1.386(6) . ? O2 C37 1.444(7) . ? O3 C43 1.389(6) . ? O3 C57 1.434(8) . ? O4 C9 1.243(6) . ? O5 C29 1.236(6) . ? O6 C49 1.232(6) . ? N1 C9 1.339(7) . ? N1 C6 1.433(7) . ? N1 H1N 0.8925 . ? N2 C9 1.400(7) . ? N2 H2N 0.8894 . ? N3 C29 1.342(7) . ? N3 C26 1.429(7) . ? N3 H3N 0.9584 . ? N4 C29 1.400(7) . ? N4 H4N 0.8564 . ? N5 C49 1.362(6) . ? N5 C46 1.435(7) . ? N5 H5N 1.0119 . ? N6 C49 1.388(7) . ? N6 H6N 0.8914 . ? C1 C22 1.530(7) . ? C1 C42 1.532(7) . ? C1 C2 1.537(7) . ? C1 H1 1.0000 . ? C2 C7 1.399(7) . ? C2 C3 1.402(7) . ? C3 C4 1.410(7) . ? C4 C5 1.398(8) . ? C4 C8 1.512(8) . ? C5 C6 1.392(7) . ? C5 H5 0.9500 . ? C6 C7 1.379(7) . ? C7 H7 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C10 C11 1.376(8) . ? C10 C15 1.398(7) . ? C11 C12 1.384(9) . ? C11 H11 0.9500 . ? C12 C13 1.406(7) . ? C12 H12 0.9500 . ? C13 C14 1.398(9) . ? C13 C16 1.491(9) . ? C14 C15 1.376(9) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.506(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.527(10) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.628(13) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.407(18) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C27 1.383(7) . ? C22 C23 1.418(7) . ? C23 C24 1.396(8) . ? C24 C25 1.404(7) . ? C24 C28 1.507(7) . ? C25 C26 1.390(7) . ? C25 H25 0.9500 . ? C26 C27 1.386(7) . ? C27 H27 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C30 C31 1.382(8) . ? C30 C35 1.386(8) . ? C31 C32 1.387(8) . ? C31 H31 0.9500 . ? C32 C33 1.395(9) . ? C32 H32 0.9500 . ? C33 C34 1.382(10) . ? C33 C36 1.538(9) . ? C34 C35 1.388(9) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.544(12) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.388(12) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.417(12) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.441(13) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C47 1.390(7) . ? C42 C43 1.398(7) . ? C43 C44 1.396(7) . ? C44 C45 1.393(8) . ? C44 C48 1.492(7) . ? C45 C46 1.376(7) . ? C45 H45 0.9500 . ? C46 C47 1.396(6) . ? C47 H47 0.9500 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C50 C55 1.392(8) . ? C50 C51 1.404(7) . ? C51 C52 1.374(8) . ? C51 H51 0.9500 . ? C52 C53 1.388(9) . ? C52 H52 0.9500 . ? C53 C54 1.412(8) . ? C53 C56 1.497(8) . ? C54 C55 1.364(8) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.585(12) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.430(12) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.530(14) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.510(16) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C1L Cl1L 1.749(7) . ? C1L Cl2L 1.749(7) . ? C1L Cl3L 1.770(7) . ? C1L H1L 1.0000 . ? C5L Cl6A 1.588(12) . ? C5L Cl8A 1.737(10) . ? C5L Cl7L 1.741(9) . ? C5L Cl7A 1.778(11) . ? C5L Cl8L 1.937(10) . ? C5L Cl6L 2.033(12) . ? C5L H5L 1.0002 . ? Cl6A Cl8A 2.102(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 S1 O8 119.5(3) . . ? O7 S1 N2 103.4(2) . . ? O8 S1 N2 109.9(3) . . ? O7 S1 C10 109.0(3) . . ? O8 S1 C10 108.4(3) . . ? N2 S1 C10 105.7(2) . . ? O10 S2 O9 120.1(3) . . ? O10 S2 N4 103.6(2) . . ? O9 S2 N4 109.0(2) . . ? O10 S2 C30 109.1(2) . . ? O9 S2 C30 108.8(3) . . ? N4 S2 C30 105.3(3) . . ? O12 S3 O13 120.2(2) . . ? O12 S3 N6 109.2(2) . . ? O13 S3 N6 102.7(2) . . ? O12 S3 C50 107.5(2) . . ? O13 S3 C50 110.0(3) . . ? N6 S3 C50 106.4(2) . . ? C3 O1 C17 114.8(4) . . ? C23 O2 C37 115.6(4) . . ? C43 O3 C57 114.6(5) . . ? C9 N1 C6 123.3(4) . . ? C9 N1 H1N 120.4 . . ? C6 N1 H1N 115.8 . . ? C9 N2 S1 122.4(3) . . ? C9 N2 H2N 114.0 . . ? S1 N2 H2N 118.6 . . ? C29 N3 C26 122.3(4) . . ? C29 N3 H3N 112.9 . . ? C26 N3 H3N 121.9 . . ? C29 N4 S2 124.2(4) . . ? C29 N4 H4N 123.1 . . ? S2 N4 H4N 112.6 . . ? C49 N5 C46 122.1(4) . . ? C49 N5 H5N 114.4 . . ? C46 N5 H5N 122.0 . . ? C49 N6 S3 123.4(4) . . ? C49 N6 H6N 119.5 . . ? S3 N6 H6N 110.4 . . ? C22 C1 C42 109.7(4) . . ? C22 C1 C2 112.9(4) . . ? C42 C1 C2 111.9(4) . . ? C22 C1 H1 107.4 . . ? C42 C1 H1 107.4 . . ? C2 C1 H1 107.4 . . ? C7 C2 C3 117.8(5) . . ? C7 C2 C1 122.7(4) . . ? C3 C2 C1 119.4(5) . . ? O1 C3 C2 119.4(5) . . ? O1 C3 C4 118.7(5) . . ? C2 C3 C4 121.8(5) . . ? C5 C4 C3 118.2(5) . . ? C5 C4 C8 120.3(5) . . ? C3 C4 C8 121.5(5) . . ? C6 C5 C4 120.4(5) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C7 C6 C5 120.5(5) . . ? C7 C6 N1 119.6(5) . . ? C5 C6 N1 119.8(5) . . ? C6 C7 C2 121.2(5) . . ? C6 C7 H7 119.4 . . ? C2 C7 H7 119.4 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O4 C9 N1 125.3(5) . . ? O4 C9 N2 119.8(5) . . ? N1 C9 N2 114.8(4) . . ? C11 C10 C15 120.9(6) . . ? C11 C10 S1 119.9(4) . . ? C15 C10 S1 119.0(5) . . ? C10 C11 C12 120.1(5) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C13 120.4(6) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C14 C13 C12 118.2(6) . . ? C14 C13 C16 120.9(5) . . ? C12 C13 C16 120.9(6) . . ? C15 C14 C13 121.7(5) . . ? C15 C14 H14 119.1 . . ? C13 C14 H14 119.1 . . ? C14 C15 C10 118.8(6) . . ? C14 C15 H15 120.6 . . ? C10 C15 H15 120.6 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O1 C17 C18 108.7(5) . . ? O1 C17 H17A 109.9 . . ? C18 C17 H17A 109.9 . . ? O1 C17 H17B 109.9 . . ? C18 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? C17 C18 C19 113.4(6) . . ? C17 C18 H18A 108.9 . . ? C19 C18 H18A 108.9 . . ? C17 C18 H18B 108.9 . . ? C19 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? C18 C19 C20 110.0(7) . . ? C18 C19 H19A 109.7 . . ? C20 C19 H19A 109.7 . . ? C18 C19 H19B 109.7 . . ? C20 C19 H19B 109.7 . . ? H19A C19 H19B 108.2 . . ? C21 C20 C19 111.3(11) . . ? C21 C20 H20A 109.4 . . ? C19 C20 H20A 109.4 . . ? C21 C20 H20B 109.4 . . ? C19 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C27 C22 C23 118.1(5) . . ? C27 C22 C1 122.1(4) . . ? C23 C22 C1 119.6(4) . . ? O2 C23 C24 119.8(4) . . ? O2 C23 C22 117.7(5) . . ? C24 C23 C22 122.3(5) . . ? C23 C24 C25 117.6(5) . . ? C23 C24 C28 121.6(5) . . ? C25 C24 C28 120.7(5) . . ? C26 C25 C24 120.4(5) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C27 C26 C25 121.0(5) . . ? C27 C26 N3 117.2(4) . . ? C25 C26 N3 121.8(5) . . ? C22 C27 C26 120.6(5) . . ? C22 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O5 C29 N3 125.4(5) . . ? O5 C29 N4 121.1(5) . . ? N3 C29 N4 113.5(4) . . ? C31 C30 C35 121.2(5) . . ? C31 C30 S2 118.4(4) . . ? C35 C30 S2 120.4(5) . . ? C30 C31 C32 119.3(6) . . ? C30 C31 H31 120.4 . . ? C32 C31 H31 120.4 . . ? C31 C32 C33 120.7(6) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C34 C33 C32 118.6(6) . . ? C34 C33 C36 121.0(7) . . ? C32 C33 C36 120.3(7) . . ? C33 C34 C35 121.7(6) . . ? C33 C34 H34 119.2 . . ? C35 C34 H34 119.2 . . ? C30 C35 C34 118.5(6) . . ? C30 C35 H35 120.8 . . ? C34 C35 H35 120.8 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O2 C37 C38 105.4(5) . . ? O2 C37 H37A 110.7 . . ? C38 C37 H37A 110.7 . . ? O2 C37 H37B 110.7 . . ? C38 C37 H37B 110.7 . . ? H37A C37 H37B 108.8 . . ? C39 C38 C37 117.9(9) . . ? C39 C38 H38A 107.8 . . ? C37 C38 H38A 107.8 . . ? C39 C38 H38B 107.8 . . ? C37 C38 H38B 107.8 . . ? H38A C38 H38B 107.2 . . ? C38 C39 C40 127.9(11) . . ? C38 C39 H39A 105.3 . . ? C40 C39 H39A 105.3 . . ? C38 C39 H39B 105.3 . . ? C40 C39 H39B 105.3 . . ? H39A C39 H39B 106.0 . . ? C39 C40 C41 126.2(11) . . ? C39 C40 H40A 105.8 . . ? C41 C40 H40A 105.8 . . ? C39 C40 H40B 105.8 . . ? C41 C40 H40B 105.8 . . ? H40A C40 H40B 106.2 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C47 C42 C43 118.1(5) . . ? C47 C42 C1 122.3(4) . . ? C43 C42 C1 119.7(5) . . ? O3 C43 C44 119.0(5) . . ? O3 C43 C42 118.5(5) . . ? C44 C43 C42 122.3(5) . . ? C45 C44 C43 117.8(5) . . ? C45 C44 C48 121.1(5) . . ? C43 C44 C48 121.1(5) . . ? C46 C45 C44 121.0(5) . . ? C46 C45 H45 119.5 . . ? C44 C45 H45 119.5 . . ? C45 C46 C47 120.3(5) . . ? C45 C46 N5 120.8(4) . . ? C47 C46 N5 118.8(4) . . ? C42 C47 C46 120.4(5) . . ? C42 C47 H47 119.8 . . ? C46 C47 H47 119.8 . . ? C44 C48 H48A 109.5 . . ? C44 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C44 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O6 C49 N5 124.9(5) . . ? O6 C49 N6 121.4(5) . . ? N5 C49 N6 113.7(4) . . ? C55 C50 C51 120.4(5) . . ? C55 C50 S3 120.6(4) . . ? C51 C50 S3 118.9(5) . . ? C52 C51 C50 118.9(6) . . ? C52 C51 H51 120.6 . . ? C50 C51 H51 120.6 . . ? C51 C52 C53 121.7(5) . . ? C51 C52 H52 119.1 . . ? C53 C52 H52 119.1 . . ? C52 C53 C54 118.1(5) . . ? C52 C53 C56 121.8(6) . . ? C54 C53 C56 120.1(6) . . ? C55 C54 C53 121.2(6) . . ? C55 C54 H54 119.4 . . ? C53 C54 H54 119.4 . . ? C54 C55 C50 119.6(5) . . ? C54 C55 H55 120.2 . . ? C50 C55 H55 120.2 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O3 C57 C58 105.1(6) . . ? O3 C57 H57A 110.7 . . ? C58 C57 H57A 110.7 . . ? O3 C57 H57B 110.7 . . ? C58 C57 H57B 110.7 . . ? H57A C57 H57B 108.8 . . ? C59 C58 C57 114.9(9) . . ? C59 C58 H58A 108.5 . . ? C57 C58 H58A 108.5 . . ? C59 C58 H58B 108.5 . . ? C57 C58 H58B 108.5 . . ? H58A C58 H58B 107.5 . . ? C58 C59 C60 114.4(11) . . ? C58 C59 H59A 108.7 . . ? C60 C59 H59A 108.7 . . ? C58 C59 H59B 108.7 . . ? C60 C59 H59B 108.7 . . ? H59A C59 H59B 107.6 . . ? C61 C60 C59 110.3(11) . . ? C61 C60 H60A 109.6 . . ? C59 C60 H60A 109.6 . . ? C61 C60 H60B 109.6 . . ? C59 C60 H60B 109.6 . . ? H60A C60 H60B 108.1 . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? Cl1L C1L Cl2L 111.4(4) . . ? Cl1L C1L Cl3L 109.9(4) . . ? Cl2L C1L Cl3L 110.8(4) . . ? Cl1L C1L H1L 108.2 . . ? Cl2L C1L H1L 108.2 . . ? Cl3L C1L H1L 108.2 . . ? Cl6A C5L Cl8A 78.3(6) . . ? Cl6A C5L Cl7L 116.2(7) . . ? Cl8A C5L Cl7L 108.8(6) . . ? Cl6A C5L Cl7A 134.6(8) . . ? Cl8A C5L Cl7A 111.5(6) . . ? Cl7L C5L Cl7A 18.6(3) . . ? Cl6A C5L Cl8L 113.5(6) . . ? Cl8A C5L Cl8L 42.9(3) . . ? Cl7L C5L Cl8L 111.0(5) . . ? Cl7A C5L Cl8L 99.9(6) . . ? Cl6A C5L Cl6L 24.2(3) . . ? Cl8A C5L Cl6L 98.5(6) . . ? Cl7L C5L Cl6L 97.2(5) . . ? Cl7A C5L Cl6L 114.2(6) . . ? Cl8L C5L Cl6L 137.2(5) . . ? Cl6A C5L H5L 110.1 . . ? Cl8A C5L H5L 139.8 . . ? Cl7L C5L H5L 102.3 . . ? Cl7A C5L H5L 90.7 . . ? Cl8L C5L H5L 102.3 . . ? Cl6L C5L H5L 102.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7 S1 N2 C9 -170.2(5) . . . . ? O8 S1 N2 C9 -41.5(5) . . . . ? C10 S1 N2 C9 75.2(5) . . . . ? O10 S2 N4 C29 176.0(4) . . . . ? O9 S2 N4 C29 47.1(5) . . . . ? C30 S2 N4 C29 -69.5(5) . . . . ? O12 S3 N6 C49 53.3(4) . . . . ? O13 S3 N6 C49 -178.0(4) . . . . ? C50 S3 N6 C49 -62.5(4) . . . . ? C22 C1 C2 C7 94.2(6) . . . . ? C42 C1 C2 C7 -30.1(7) . . . . ? C22 C1 C2 C3 -87.5(6) . . . . ? C42 C1 C2 C3 148.2(5) . . . . ? C17 O1 C3 C2 100.2(5) . . . . ? C17 O1 C3 C4 -83.9(6) . . . . ? C7 C2 C3 O1 176.7(4) . . . . ? C1 C2 C3 O1 -1.7(7) . . . . ? C7 C2 C3 C4 0.9(7) . . . . ? C1 C2 C3 C4 -177.5(5) . . . . ? O1 C3 C4 C5 -178.0(5) . . . . ? C2 C3 C4 C5 -2.2(8) . . . . ? O1 C3 C4 C8 0.7(8) . . . . ? C2 C3 C4 C8 176.5(5) . . . . ? C3 C4 C5 C6 1.5(8) . . . . ? C8 C4 C5 C6 -177.3(5) . . . . ? C4 C5 C6 C7 0.5(8) . . . . ? C4 C5 C6 N1 176.5(5) . . . . ? C9 N1 C6 C7 -129.9(5) . . . . ? C9 N1 C6 C5 54.1(7) . . . . ? C5 C6 C7 C2 -1.9(8) . . . . ? N1 C6 C7 C2 -177.9(5) . . . . ? C3 C2 C7 C6 1.1(7) . . . . ? C1 C2 C7 C6 179.5(5) . . . . ? C6 N1 C9 O4 3.0(8) . . . . ? C6 N1 C9 N2 -179.6(4) . . . . ? S1 N2 C9 O4 -32.9(7) . . . . ? S1 N2 C9 N1 149.6(4) . . . . ? O7 S1 C10 C11 -45.5(5) . . . . ? O8 S1 C10 C11 -177.1(4) . . . . ? N2 S1 C10 C11 65.1(5) . . . . ? O7 S1 C10 C15 129.2(4) . . . . ? O8 S1 C10 C15 -2.4(5) . . . . ? N2 S1 C10 C15 -120.2(4) . . . . ? C15 C10 C11 C12 1.0(8) . . . . ? S1 C10 C11 C12 175.6(4) . . . . ? C10 C11 C12 C13 -0.2(8) . . . . ? C11 C12 C13 C14 -0.3(8) . . . . ? C11 C12 C13 C16 -179.4(5) . . . . ? C12 C13 C14 C15 -0.1(8) . . . . ? C16 C13 C14 C15 179.1(5) . . . . ? C13 C14 C15 C10 0.9(8) . . . . ? C11 C10 C15 C14 -1.3(8) . . . . ? S1 C10 C15 C14 -176.0(4) . . . . ? C3 O1 C17 C18 167.5(5) . . . . ? O1 C17 C18 C19 -66.3(7) . . . . ? C17 C18 C19 C20 -172.5(6) . . . . ? C18 C19 C20 C21 -177.0(10) . . . . ? C42 C1 C22 C27 96.8(5) . . . . ? C2 C1 C22 C27 -28.7(6) . . . . ? C42 C1 C22 C23 -78.2(6) . . . . ? C2 C1 C22 C23 156.4(4) . . . . ? C37 O2 C23 C24 88.0(6) . . . . ? C37 O2 C23 C22 -97.2(6) . . . . ? C27 C22 C23 O2 -174.0(4) . . . . ? C1 C22 C23 O2 1.1(6) . . . . ? C27 C22 C23 C24 0.6(7) . . . . ? C1 C22 C23 C24 175.7(4) . . . . ? O2 C23 C24 C25 173.8(4) . . . . ? C22 C23 C24 C25 -0.6(7) . . . . ? O2 C23 C24 C28 -5.1(7) . . . . ? C22 C23 C24 C28 -179.5(5) . . . . ? C23 C24 C25 C26 0.1(7) . . . . ? C28 C24 C25 C26 179.0(5) . . . . ? C24 C25 C26 C27 0.5(7) . . . . ? C24 C25 C26 N3 -179.8(5) . . . . ? C29 N3 C26 C27 -123.0(5) . . . . ? C29 N3 C26 C25 57.2(7) . . . . ? C23 C22 C27 C26 0.0(7) . . . . ? C1 C22 C27 C26 -175.0(4) . . . . ? C25 C26 C27 C22 -0.6(7) . . . . ? N3 C26 C27 C22 179.7(4) . . . . ? C26 N3 C29 O5 -15.3(8) . . . . ? C26 N3 C29 N4 163.9(5) . . . . ? S2 N4 C29 O5 -11.1(7) . . . . ? S2 N4 C29 N3 169.7(4) . . . . ? O10 S2 C30 C31 28.2(5) . . . . ? O9 S2 C30 C31 160.9(4) . . . . ? N4 S2 C30 C31 -82.4(5) . . . . ? O10 S2 C30 C35 -151.3(5) . . . . ? O9 S2 C30 C35 -18.6(6) . . . . ? N4 S2 C30 C35 98.1(5) . . . . ? C35 C30 C31 C32 -0.2(9) . . . . ? S2 C30 C31 C32 -179.7(5) . . . . ? C30 C31 C32 C33 0.1(9) . . . . ? C31 C32 C33 C34 0.2(10) . . . . ? C31 C32 C33 C36 179.8(6) . . . . ? C32 C33 C34 C35 -0.5(11) . . . . ? C36 C33 C34 C35 179.9(7) . . . . ? C31 C30 C35 C34 -0.1(10) . . . . ? S2 C30 C35 C34 179.4(5) . . . . ? C33 C34 C35 C30 0.5(11) . . . . ? C23 O2 C37 C38 159.3(6) . . . . ? O2 C37 C38 C39 63.5(10) . . . . ? C37 C38 C39 C40 -166.1(9) . . . . ? C38 C39 C40 C41 175.2(10) . . . . ? C22 C1 C42 C47 -38.1(6) . . . . ? C2 C1 C42 C47 88.0(6) . . . . ? C22 C1 C42 C43 141.9(5) . . . . ? C2 C1 C42 C43 -92.0(6) . . . . ? C57 O3 C43 C44 -90.3(6) . . . . ? C57 O3 C43 C42 94.7(6) . . . . ? C47 C42 C43 O3 177.7(4) . . . . ? C1 C42 C43 O3 -2.4(7) . . . . ? C47 C42 C43 C44 2.8(8) . . . . ? C1 C42 C43 C44 -177.2(5) . . . . ? O3 C43 C44 C45 -177.6(5) . . . . ? C42 C43 C44 C45 -2.8(8) . . . . ? O3 C43 C44 C48 2.6(8) . . . . ? C42 C43 C44 C48 177.4(5) . . . . ? C43 C44 C45 C46 0.2(7) . . . . ? C48 C44 C45 C46 -179.9(5) . . . . ? C44 C45 C46 C47 2.2(7) . . . . ? C44 C45 C46 N5 178.8(5) . . . . ? C49 N5 C46 C45 63.6(6) . . . . ? C49 N5 C46 C47 -119.7(5) . . . . ? C43 C42 C47 C46 -0.4(7) . . . . ? C1 C42 C47 C46 179.6(5) . . . . ? C45 C46 C47 C42 -2.1(7) . . . . ? N5 C46 C47 C42 -178.8(4) . . . . ? C46 N5 C49 O6 -0.7(7) . . . . ? C46 N5 C49 N6 -178.7(4) . . . . ? S3 N6 C49 O6 1.7(6) . . . . ? S3 N6 C49 N5 179.7(3) . . . . ? O12 S3 C50 C55 -22.1(5) . . . . ? O13 S3 C50 C55 -154.6(5) . . . . ? N6 S3 C50 C55 94.9(5) . . . . ? O12 S3 C50 C51 155.6(4) . . . . ? O13 S3 C50 C51 23.1(5) . . . . ? N6 S3 C50 C51 -87.4(5) . . . . ? C55 C50 C51 C52 -1.9(8) . . . . ? S3 C50 C51 C52 -179.7(4) . . . . ? C50 C51 C52 C53 0.5(8) . . . . ? C51 C52 C53 C54 1.0(9) . . . . ? C51 C52 C53 C56 -179.0(6) . . . . ? C52 C53 C54 C55 -1.3(9) . . . . ? C56 C53 C54 C55 178.8(6) . . . . ? C53 C54 C55 C50 -0.1(9) . . . . ? C51 C50 C55 C54 1.7(9) . . . . ? S3 C50 C55 C54 179.4(5) . . . . ? C43 O3 C57 C58 -159.5(5) . . . . ? O3 C57 C58 C59 173.4(8) . . . . ? C57 C58 C59 C60 -172.4(8) . . . . ? C58 C59 C60 C61 -168.8(10) . . . . ? 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 N1 H1N O9 0.89 2.29 3.048(6) 142.3 2_666 N1 H1N O5 0.89 2.33 3.076(6) 141.1 2_666 N2 H2N O5 0.89 1.99 2.861(5) 164.9 2_666 N3 H3N O6 0.96 2.14 3.035(5) 154.3 2_666 N3 H3N O12 0.96 2.41 3.037(6) 123.1 2_666 N4 H4N O6 0.86 2.02 2.809(6) 152.9 2_666 N5 H5N O4 1.01 1.95 2.912(6) 157.8 2_666 N6 H6N O4 0.89 2.19 2.936(6) 140.3 2_666 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.434 _refine_diff_density_min -0.779 _refine_diff_density_rms 0.090