# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2008 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Haibing Li' _publ_contact_author_email LHBING@MAIL.CCNU.EDU.CN _publ_section_title ; Synthesis of calix[4]crown containing soft and hard ion bindings site via click chemistry ; loop_ _publ_author_name 'Haibing Li' 'Demei Tian' 'Junyan Zhan' # Attachment '080530am.cif' data_080530am _database_code_depnum_ccdc_archive 'CCDC 701086' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C109 H140 Cl2 N12 O16' _chemical_formula_weight 1945.23 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1987(9) _cell_length_b 20.8765(16) _cell_length_c 24.7757(19) _cell_angle_alpha 70.1190(10) _cell_angle_beta 79.8420(10) _cell_angle_gamma 73.6920(10) _cell_volume 5671.9(7) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9521 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 22.64 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.139 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 0.122 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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_% ? _diffrn_reflns_number 41324 _diffrn_reflns_av_R_equivalents 0.0605 _diffrn_reflns_av_sigmaI/netI 0.0746 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 0.88 _diffrn_reflns_theta_max 25.00 _reflns_number_total 19838 _reflns_number_gt 11537 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19838 _refine_ls_number_parameters 1414 _refine_ls_number_restraints 92 _refine_ls_R_factor_all 0.1439 _refine_ls_R_factor_gt 0.1061 _refine_ls_wR_factor_ref 0.3297 _refine_ls_wR_factor_gt 0.3073 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 2.514 _refine_ls_shift/su_mean 0.026 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.2781(3) 0.28393(19) 0.73679(15) 0.0382(9) Uani 1 1 d . . . C2 C 1.2721(3) 0.23062(19) 0.78953(15) 0.0384(9) Uani 1 1 d . . . C3 C 1.3273(3) 0.2292(2) 0.83411(16) 0.0435(9) Uani 1 1 d . . . H3 H 1.3243 0.1927 0.8695 0.052 Uiso 1 1 calc R . . C4 C 1.3864(3) 0.2783(2) 0.82968(16) 0.0425(9) Uani 1 1 d . . . C5 C 1.3914(3) 0.3298(2) 0.77688(15) 0.0420(9) Uani 1 1 d . . . H5 H 1.4320 0.3642 0.7726 0.050 Uiso 1 1 calc R . . C6 C 1.3398(3) 0.33347(19) 0.72996(15) 0.0398(9) Uani 1 1 d . . . C7 C 1.4442(4) 0.2733(2) 0.88165(17) 0.0516(10) Uani 1 1 d . . . C8 C 1.3590(5) 0.2644(4) 0.9362(2) 0.0880(18) Uani 1 1 d . . . H8A H 1.2900 0.3029 0.9289 0.132 Uiso 1 1 calc R . . H8B H 1.3949 0.2653 0.9683 0.132 Uiso 1 1 calc R . . H8C H 1.3380 0.2196 0.9461 0.132 Uiso 1 1 calc R . . C9 C 1.5468(4) 0.2094(3) 0.8915(2) 0.0678(13) Uani 1 1 d . . . H9A H 1.5191 0.1664 0.9049 0.102 Uiso 1 1 calc R . . H9B H 1.5914 0.2098 0.9205 0.102 Uiso 1 1 calc R . . H9C H 1.5954 0.2113 0.8552 0.102 Uiso 1 1 calc R . . C10 C 1.4910(5) 0.3377(3) 0.8721(2) 0.0694(13) Uani 1 1 d . . . H10A H 1.5519 0.3405 0.8404 0.104 Uiso 1 1 calc R . . H10B H 1.5221 0.3336 0.9074 0.104 Uiso 1 1 calc R . . H10C H 1.4289 0.3802 0.8625 0.104 Uiso 1 1 calc R . . C11 C 1.3502(3) 0.3910(2) 0.67262(16) 0.0456(9) Uani 1 1 d . . . H11A H 1.4138 0.4116 0.6729 0.055 Uiso 1 1 calc R . . H11B H 1.3709 0.3693 0.6412 0.055 Uiso 1 1 calc R . . C12 C 1.2426(3) 0.44954(19) 0.65920(15) 0.0401(9) Uani 1 1 d . . . C13 C 1.1629(3) 0.44767(19) 0.62634(14) 0.0399(9) Uani 1 1 d . . . C14 C 1.0580(4) 0.4958(2) 0.61996(15) 0.0471(10) Uani 1 1 d . . . C15 C 1.0373(4) 0.5501(2) 0.64343(18) 0.0541(11) Uani 1 1 d . . . H15 H 0.9660 0.5840 0.6386 0.065 Uiso 1 1 calc R . . C16 C 1.1169(4) 0.5569(2) 0.67381(18) 0.0541(11) Uani 1 1 d . . . C17 C 1.2180(4) 0.5040(2) 0.68237(16) 0.0475(10) Uani 1 1 d . . . H17 H 1.2719 0.5056 0.7050 0.057 Uiso 1 1 calc R . . C18 C 1.0959(5) 0.6192(3) 0.6971(2) 0.0708(14) Uani 1 1 d . . . C19 C 1.1240(6) 0.5920(3) 0.7608(2) 0.097(2) Uani 1 1 d . . . H19A H 1.1089 0.6318 0.7758 0.145 Uiso 1 1 calc R . . H19B H 1.2051 0.5672 0.7631 0.145 Uiso 1 1 calc R . . H19C H 1.0760 0.5599 0.7837 0.145 Uiso 1 1 calc R . . C20 C 0.9737(6) 0.6650(3) 0.6912(3) 0.110(2) Uani 1 1 d . . . H20A H 0.9572 0.6812 0.6508 0.165 Uiso 1 1 calc R . . H20B H 0.9664 0.7056 0.7042 0.165 Uiso 1 1 calc R . . H20C H 0.9193 0.6376 0.7150 0.165 Uiso 1 1 calc R . . C21 C 1.1772(6) 0.6655(3) 0.6615(3) 0.101(2) Uani 1 1 d . . . H21A H 1.1663 0.6788 0.6206 0.152 Uiso 1 1 calc R . . H21B H 1.2566 0.6394 0.6680 0.152 Uiso 1 1 calc R . . H21C H 1.1606 0.7078 0.6733 0.152 Uiso 1 1 calc R . . C22 C 0.9629(4) 0.4873(2) 0.59196(17) 0.0525(11) Uani 1 1 d . . . H22A H 0.9304 0.5325 0.5636 0.063 Uiso 1 1 calc R . . H22B H 0.9957 0.4523 0.5711 0.063 Uiso 1 1 calc R . . C23 C 0.8690(4) 0.4638(2) 0.63635(17) 0.0514(11) Uani 1 1 d . . . C24 C 0.8751(3) 0.3913(2) 0.66400(16) 0.0440(9) Uani 1 1 d . . . C25 C 0.7903(3) 0.3707(2) 0.70789(15) 0.0432(9) Uani 1 1 d . . . C26 C 0.7028(4) 0.4206(2) 0.7226(2) 0.0613(12) Uani 1 1 d . A . H26 H 0.6451 0.4057 0.7516 0.074 Uiso 1 1 calc R . . C27 C 0.6933(4) 0.4924(3) 0.6974(3) 0.0887(19) Uani 1 1 d D . . C28 C 0.7786(4) 0.5111(2) 0.6538(3) 0.0822(18) Uani 1 1 d . A . H28 H 0.7739 0.5596 0.6349 0.099 Uiso 1 1 calc R . . C29 C 0.5790(7) 0.5472(4) 0.6946(5) 0.060(3) Uani 0.452(11) 1 d PD A 1 C30 C 0.5093(9) 0.5739(6) 0.6427(5) 0.092(5) Uani 0.452(11) 1 d PD A 1 H30A H 0.4633 0.5409 0.6460 0.138 Uiso 0.452(11) 1 calc PR A 1 H30B H 0.5614 0.5780 0.6074 0.138 Uiso 0.452(11) 1 calc PR A 1 H30C H 0.4585 0.6199 0.6414 0.138 Uiso 0.452(11) 1 calc PR A 1 C31 C 0.6183(15) 0.6092(7) 0.6982(7) 0.084(6) Uani 0.452(11) 1 d PD A 1 H31A H 0.6612 0.6290 0.6618 0.127 Uiso 0.452(11) 1 calc PR A 1 H31B H 0.6676 0.5929 0.7298 0.127 Uiso 0.452(11) 1 calc PR A 1 H31C H 0.5511 0.6452 0.7053 0.127 Uiso 0.452(11) 1 calc PR A 1 C32 C 0.4963(19) 0.5274(13) 0.7480(6) 0.130(12) Uani 0.452(11) 1 d PD A 1 H32A H 0.4242 0.5636 0.7441 0.195 Uiso 0.452(11) 1 calc PR A 1 H32B H 0.5306 0.5236 0.7822 0.195 Uiso 0.452(11) 1 calc PR A 1 H32C H 0.4810 0.4823 0.7521 0.195 Uiso 0.452(11) 1 calc PR A 1 C33 C 0.7948(3) 0.2937(2) 0.73957(15) 0.0413(9) Uani 1 1 d . . . H33A H 0.8172 0.2667 0.7117 0.050 Uiso 1 1 calc R . . H33B H 0.7179 0.2884 0.7585 0.050 Uiso 1 1 calc R . . C34 C 0.8806(3) 0.26475(19) 0.78466(15) 0.0369(8) Uani 1 1 d . . . C35 C 0.9917(3) 0.22895(18) 0.77325(14) 0.0366(8) Uani 1 1 d . . . C36 C 1.0754(3) 0.21073(18) 0.81154(14) 0.0363(8) Uani 1 1 d . . . C37 C 1.0407(3) 0.2247(2) 0.86372(15) 0.0408(9) Uani 1 1 d . . . H37 H 1.0960 0.2109 0.8906 0.049 Uiso 1 1 calc R . . C38 C 0.9284(3) 0.2580(2) 0.87872(15) 0.0411(9) Uani 1 1 d . . . C39 C 0.8503(3) 0.2778(2) 0.83790(15) 0.0406(9) Uani 1 1 d . . . H39 H 0.7735 0.3010 0.8464 0.049 Uiso 1 1 calc R . . C40 C 0.8913(4) 0.2704(2) 0.93722(17) 0.0518(11) Uani 1 1 d . . . C41 C 0.8220(8) 0.2183(5) 0.9735(3) 0.150(4) Uani 1 1 d . . . H41A H 0.8733 0.1716 0.9865 0.224 Uiso 1 1 calc R . . H41B H 0.7656 0.2170 0.9505 0.224 Uiso 1 1 calc R . . H41C H 0.7822 0.2326 1.0071 0.224 Uiso 1 1 calc R . . C42 C 0.8121(8) 0.3422(5) 0.9301(3) 0.158(4) Uani 1 1 d . . . H42A H 0.8066 0.3550 0.9651 0.236 Uiso 1 1 calc R . . H42B H 0.7359 0.3415 0.9232 0.236 Uiso 1 1 calc R . . H42C H 0.8425 0.3766 0.8972 0.236 Uiso 1 1 calc R . . C43 C 0.9897(5) 0.2617(4) 0.9690(2) 0.104(2) Uani 1 1 d . . . H43A H 0.9610 0.2720 1.0054 0.156 Uiso 1 1 calc R . . H43B H 1.0370 0.2941 0.9456 0.156 Uiso 1 1 calc R . . H43C H 1.0360 0.2134 0.9770 0.156 Uiso 1 1 calc R . . C44 C 1.2006(3) 0.17830(19) 0.79736(16) 0.0427(9) Uani 1 1 d . . . H44A H 1.2092 0.1656 0.7616 0.051 Uiso 1 1 calc R . . H44B H 1.2277 0.1351 0.8290 0.051 Uiso 1 1 calc R . . C45 C 1.2446(4) 0.4094(3) 0.54417(17) 0.0637(12) Uani 1 1 d . . . H45A H 1.3276 0.4036 0.5456 0.076 Uiso 1 1 calc R . . H45B H 1.2120 0.4582 0.5210 0.076 Uiso 1 1 calc R . . C46 C 1.2266(4) 0.3594(3) 0.51862(17) 0.0604(12) Uani 1 1 d . . . C47 C 1.1545(5) 0.3158(3) 0.5383(2) 0.0771(15) Uani 1 1 d . . . H47 H 1.1058 0.3088 0.5732 0.092 Uiso 1 1 calc R . . C48 C 1.1113(7) 0.2361(4) 0.4941(4) 0.120(3) Uani 1 1 d . . . H48A H 1.1280 0.1933 0.5275 0.144 Uiso 1 1 calc R . . H48B H 1.1437 0.2227 0.4588 0.144 Uiso 1 1 calc R . . C49 C 0.9893(6) 0.2608(4) 0.4927(3) 0.0935(19) Uani 1 1 d . . . H49A H 0.9541 0.2658 0.5307 0.112 Uiso 1 1 calc R . . H49B H 0.9709 0.3075 0.4634 0.112 Uiso 1 1 calc R . . C50 C 0.8364(5) 0.2047(4) 0.5090(3) 0.0892(17) Uani 1 1 d . . . H50A H 0.7853 0.2064 0.4814 0.107 Uiso 1 1 calc R . . H50B H 0.8008 0.2439 0.5252 0.107 Uiso 1 1 calc R . . C51 C 0.8457(5) 0.1365(3) 0.5570(2) 0.0748(14) Uani 1 1 d . . . H51A H 0.7680 0.1319 0.5750 0.090 Uiso 1 1 calc R . . H51B H 0.8802 0.0972 0.5409 0.090 Uiso 1 1 calc R . . C52 C 0.8876(4) 0.1597(2) 0.64422(17) 0.0529(11) Uani 1 1 d . . . H52 H 0.8153 0.1878 0.6534 0.064 Uiso 1 1 calc R . . C53 C 0.9840(4) 0.1391(2) 0.67259(17) 0.0505(10) Uani 1 1 d . . . C54 C 1.0016(4) 0.1456(2) 0.72789(16) 0.0504(10) Uani 1 1 d . . . H54A H 0.9336 0.1383 0.7555 0.060 Uiso 1 1 calc R . . H54B H 1.0687 0.1085 0.7442 0.060 Uiso 1 1 calc R . . C55 C 0.7730(3) 1.0304(2) 0.73190(15) 0.0472(10) Uani 1 1 d . . . C56 C 0.8741(3) 0.9798(2) 0.74866(16) 0.0467(10) Uani 1 1 d . . . C57 C 0.9195(3) 0.9771(2) 0.79695(16) 0.0468(10) Uani 1 1 d . . . H57 H 0.9897 0.9439 0.8074 0.056 Uiso 1 1 calc R . . C58 C 0.8679(3) 1.0204(2) 0.83110(16) 0.0467(10) Uani 1 1 d . . . C59 C 0.7672(3) 1.0697(2) 0.81292(16) 0.0451(9) Uani 1 1 d . . . H59 H 0.7305 1.1008 0.8346 0.054 Uiso 1 1 calc R . . C60 C 0.7180(3) 1.0754(2) 0.76457(16) 0.0471(10) Uani 1 1 d . . . C61 C 0.9167(4) 1.0108(2) 0.88743(17) 0.0528(11) Uani 1 1 d . . . C62 C 0.8948(6) 0.9424(3) 0.9311(2) 0.0817(16) Uani 1 1 d . . . H62A H 0.8121 0.9471 0.9406 0.123 Uiso 1 1 calc R . . H62B H 0.9317 0.9323 0.9661 0.123 Uiso 1 1 calc R . . H62C H 0.9268 0.9039 0.9144 0.123 Uiso 1 1 calc R . . C63 C 1.0447(5) 1.0083(4) 0.8769(2) 0.0873(17) Uani 1 1 d . . . H63A H 1.0855 0.9680 0.8636 0.131 Uiso 1 1 calc R . . H63B H 1.0736 1.0038 0.9128 0.131 Uiso 1 1 calc R . . H63C H 1.0571 1.0516 0.8474 0.131 Uiso 1 1 calc R . . C64 C 0.8607(5) 1.0698(3) 0.9118(2) 0.0764(15) Uani 1 1 d . . . H64A H 0.8748 1.1138 0.8843 0.115 Uiso 1 1 calc R . . H64B H 0.8925 1.0609 0.9481 0.115 Uiso 1 1 calc R . . H64C H 0.7779 1.0734 0.9191 0.115 Uiso 1 1 calc R . . C65 C 0.6016(4) 1.1247(2) 0.75075(18) 0.0543(11) Uani 1 1 d . . . H65A H 0.6010 1.1483 0.7087 0.065 Uiso 1 1 calc R . . H65B H 0.5849 1.1610 0.7703 0.065 Uiso 1 1 calc R . . C66 C 0.5117(3) 1.08163(19) 0.77160(15) 0.0402(9) Uani 1 1 d . . . C67 C 0.4543(3) 1.06778(19) 0.73440(15) 0.0399(9) Uani 1 1 d . . . C68 C 0.3806(3) 1.0236(2) 0.75491(15) 0.0403(9) Uani 1 1 d . . . C69 C 0.3658(3) 0.9921(2) 0.81426(15) 0.0418(9) Uani 1 1 d . . . H69 H 0.3151 0.9617 0.8288 0.050 Uiso 1 1 calc R . . C70 C 0.4217(3) 1.0034(2) 0.85254(15) 0.0394(9) Uani 1 1 d . . . C71 C 0.4929(3) 1.04956(19) 0.83025(15) 0.0404(9) Uani 1 1 d . . . H71 H 0.5300 1.0595 0.8561 0.048 Uiso 1 1 calc R . . C72 C 0.4121(4) 0.9653(2) 0.91744(16) 0.0526(11) Uani 1 1 d . . . C73 C 0.3520(5) 0.9068(3) 0.9334(2) 0.0832(16) Uani 1 1 d . . . H73A H 0.2735 0.9259 0.9220 0.125 Uiso 1 1 calc R . . H73B H 0.3501 0.8838 0.9751 0.125 Uiso 1 1 calc R . . H73C H 0.3934 0.8726 0.9134 0.125 Uiso 1 1 calc R . . C74 C 0.5324(5) 0.9336(4) 0.9384(2) 0.098(2) Uani 1 1 d . . . H74A H 0.5262 0.9094 0.9799 0.147 Uiso 1 1 calc R . . H74B H 0.5722 0.9710 0.9305 0.147 Uiso 1 1 calc R . . H74C H 0.5758 0.9001 0.9180 0.147 Uiso 1 1 calc R . . C75 C 0.3434(6) 1.0193(3) 0.9485(2) 0.097(2) Uani 1 1 d . . . H75A H 0.2659 1.0383 0.9357 0.146 Uiso 1 1 calc R . . H75B H 0.3820 1.0576 0.9391 0.146 Uiso 1 1 calc R . . H75C H 0.3386 0.9963 0.9902 0.146 Uiso 1 1 calc R . . C76 C 0.3245(4) 1.0036(2) 0.71486(18) 0.0507(10) Uani 1 1 d . . . H76A H 0.2403 1.0143 0.7240 0.061 Uiso 1 1 calc R . . H76B H 0.3415 1.0313 0.6744 0.061 Uiso 1 1 calc R . . C77 C 0.3693(3) 0.9266(2) 0.72180(16) 0.0459(10) Uani 1 1 d . . . C78 C 0.4779(3) 0.9026(2) 0.69606(15) 0.0445(9) Uani 1 1 d . . . C79 C 0.5263(3) 0.8305(2) 0.70814(17) 0.0501(10) Uani 1 1 d . . . C80 C 0.4644(4) 0.7845(2) 0.74483(18) 0.0513(10) Uani 1 1 d . . . H80 H 0.4968 0.7356 0.7523 0.062 Uiso 1 1 calc R . . C81 C 0.3560(4) 0.8063(2) 0.77158(17) 0.0507(10) Uani 1 1 d . B . C82 C 0.3113(4) 0.8782(2) 0.75798(17) 0.0502(10) Uani 1 1 d . . . H82 H 0.2367 0.8947 0.7745 0.060 Uiso 1 1 calc R . . C83 C 0.2925(4) 0.7542(2) 0.8144(2) 0.0710(14) Uani 1 1 d D . . C84 C 0.1899(10) 0.7887(6) 0.8488(6) 0.098(5) Uani 0.501(19) 1 d PD B 1 H84A H 0.1519 0.7528 0.8753 0.147 Uiso 0.501(19) 1 calc PR B 1 H84B H 0.1356 0.8236 0.8222 0.147 Uiso 0.501(19) 1 calc PR B 1 H84C H 0.2165 0.8116 0.8708 0.147 Uiso 0.501(19) 1 calc PR B 1 C85 C 0.3755(9) 0.7035(9) 0.8593(6) 0.168(14) Uani 0.501(19) 1 d PD B 1 H85A H 0.3983 0.7299 0.8796 0.251 Uiso 0.501(19) 1 calc PR B 1 H85B H 0.4437 0.6798 0.8398 0.251 Uiso 0.501(19) 1 calc PR B 1 H85C H 0.3372 0.6685 0.8871 0.251 Uiso 0.501(19) 1 calc PR B 1 C86 C 0.2544(16) 0.7120(11) 0.7863(7) 0.25(3) Uani 0.501(19) 1 d PD B 1 H86A H 0.1979 0.6883 0.8127 0.369 Uiso 0.501(19) 1 calc PR B 1 H86B H 0.3206 0.6770 0.7769 0.369 Uiso 0.501(19) 1 calc PR B 1 H86C H 0.2196 0.7432 0.7509 0.369 Uiso 0.501(19) 1 calc PR B 1 C86' C 0.3447(10) 0.6791(5) 0.8104(7) 0.097(6) Uani 0.499(19) 1 d PD B 2 H86D H 0.4242 0.6636 0.8202 0.145 Uiso 0.499(19) 1 calc PR B 2 H86E H 0.3427 0.6791 0.7710 0.145 Uiso 0.499(19) 1 calc PR B 2 H86F H 0.3000 0.6471 0.8373 0.145 Uiso 0.499(19) 1 calc PR B 2 C84' C 0.286(2) 0.7535(11) 0.8746(5) 0.25(3) Uani 0.499(19) 1 d PD B 2 H84D H 0.3627 0.7490 0.8845 0.375 Uiso 0.499(19) 1 calc PR B 2 H84E H 0.2556 0.7138 0.9003 0.375 Uiso 0.499(19) 1 calc PR B 2 H84F H 0.2350 0.7974 0.8790 0.375 Uiso 0.499(19) 1 calc PR B 2 C85' C 0.1684(8) 0.7717(7) 0.7969(9) 0.134(10) Uani 0.499(19) 1 d PD B 2 H85D H 0.1316 0.7335 0.8195 0.200 Uiso 0.499(19) 1 calc PR B 2 H85E H 0.1714 0.7772 0.7558 0.200 Uiso 0.499(19) 1 calc PR B 2 H85F H 0.1241 0.8154 0.8043 0.200 Uiso 0.499(19) 1 calc PR B 2 C87 C 0.6480(4) 0.8044(3) 0.6844(2) 0.0599(12) Uani 1 1 d . . . H87A H 0.6609 0.8333 0.6440 0.072 Uiso 1 1 calc R . . H87B H 0.6600 0.7552 0.6852 0.072 Uiso 1 1 calc R . . C88 C 0.7330(3) 0.8090(2) 0.72104(17) 0.0459(10) Uani 1 1 d . . . C89 C 0.7962(3) 0.8596(2) 0.70112(15) 0.0407(9) Uani 1 1 d . . . C90 C 0.8641(3) 0.8674(2) 0.73689(15) 0.0440(9) Uani 1 1 d . . . C91 C 0.8684(3) 0.8222(2) 0.79272(17) 0.0534(11) Uani 1 1 d . . . H91 H 0.9154 0.8267 0.8174 0.064 Uiso 1 1 calc R . . C92 C 0.8076(4) 0.7711(2) 0.81400(18) 0.0584(12) Uani 1 1 d . C . C93 C 0.7405(4) 0.7651(2) 0.77699(18) 0.0524(11) Uani 1 1 d . . . H93 H 0.6985 0.7298 0.7906 0.063 Uiso 1 1 calc R . . C94 C 0.8106(4) 0.7237(3) 0.8761(2) 0.065(2) Uani 0.827(10) 1 d PD . . C95 C 0.6860(6) 0.7212(5) 0.9019(3) 0.116(3) Uani 0.827(10) 1 d PDU C 1 H95A H 0.6521 0.7014 0.8800 0.174 Uiso 0.827(10) 1 calc PR C 1 H95B H 0.6407 0.7687 0.8996 0.174 Uiso 0.827(10) 1 calc PR C 1 H95C H 0.6864 0.6917 0.9423 0.174 Uiso 0.827(10) 1 calc PR C 1 C96 C 0.8599(9) 0.7488(6) 0.9138(3) 0.145(5) Uani 0.827(10) 1 d PDU C 1 H96A H 0.8608 0.7156 0.9529 0.218 Uiso 0.827(10) 1 calc PR C 1 H96B H 0.8130 0.7950 0.9150 0.218 Uiso 0.827(10) 1 calc PR C 1 H96C H 0.9384 0.7525 0.8984 0.218 Uiso 0.827(10) 1 calc PR C 1 C97 C 0.8713(12) 0.6517(4) 0.8739(4) 0.229(6) Uani 1 1 d DU C 1 H97A H 0.9540 0.6453 0.8739 0.344 Uiso 1 1 calc R C 1 H97B H 0.8557 0.6456 0.8387 0.344 Uiso 1 1 calc R C 1 H97C H 0.8442 0.6169 0.9077 0.344 Uiso 1 1 calc R C 1 C95' C 0.9374(10) 0.6847(12) 0.8874(8) 0.052(8) Uani 0.173(10) 1 d PDU C 2 H95D H 0.9396 0.6484 0.9250 0.079 Uiso 0.173(10) 1 calc PR C 2 H95E H 0.9799 0.7183 0.8871 0.079 Uiso 0.173(10) 1 calc PR C 2 H95F H 0.9725 0.6629 0.8572 0.079 Uiso 0.173(10) 1 calc PR C 2 C96' C 0.743(2) 0.6676(12) 0.8970(14) 0.101(13) Uani 0.173(10) 1 d PDU C 2 H96D H 0.6640 0.6884 0.8868 0.152 Uiso 0.173(10) 1 calc PR C 2 H96E H 0.7432 0.6471 0.9390 0.152 Uiso 0.173(10) 1 calc PR C 2 H96F H 0.7786 0.6308 0.8788 0.152 Uiso 0.173(10) 1 calc PR C 2 C97' C 0.775(2) 0.7690(11) 0.9165(9) 0.076(10) Uani 0.173(10) 1 d PDU C 2 H97D H 0.7843 0.7390 0.9563 0.114 Uiso 0.173(10) 1 calc PR C 2 H97E H 0.6938 0.7941 0.9130 0.114 Uiso 0.173(10) 1 calc PR C 2 H97F H 0.8223 0.8029 0.9060 0.114 Uiso 0.173(10) 1 calc PR C 2 C98 C 0.9259(4) 0.9272(2) 0.71674(17) 0.0539(11) Uani 1 1 d . . . H98A H 1.0080 0.9078 0.7233 0.065 Uiso 1 1 calc R . . H98B H 0.9204 0.9507 0.6749 0.065 Uiso 1 1 calc R . . C99 C 0.4078(4) 1.1640(2) 0.64991(17) 0.0629(13) Uani 1 1 d . . . H99A H 0.4078 1.1955 0.6720 0.075 Uiso 1 1 calc R . . H99B H 0.3280 1.1605 0.6512 0.075 Uiso 1 1 calc R . . C100 C 0.4531(4) 1.1921(2) 0.58974(18) 0.0588(12) Uani 1 1 d . . . C101 C 0.4469(5) 1.1795(3) 0.5418(2) 0.0758(15) Uani 1 1 d . . . H101 H 0.4081 1.1470 0.5395 0.091 Uiso 1 1 calc R . . C102 C 0.5098(7) 1.2273(3) 0.4361(2) 0.104(2) Uani 1 1 d . . . H10D H 0.4324 1.2353 0.4243 0.125 Uiso 1 1 calc R . . H10E H 0.5384 1.2700 0.4152 0.125 Uiso 1 1 calc R . . C103 C 0.5845(7) 1.1693(5) 0.4191(3) 0.131(3) Uani 1 1 d U . . H10F H 0.5460 1.1300 0.4348 0.157 Uiso 1 1 calc R . . H10G H 0.5868 1.1829 0.3766 0.157 Uiso 1 1 calc R . . C104 C 0.7637(5) 1.1092(4) 0.3953(2) 0.100(2) Uani 1 1 d U . . H10H H 0.7464 1.1363 0.3551 0.120 Uiso 1 1 calc R . . H10I H 0.8431 1.1096 0.3988 0.120 Uiso 1 1 calc R . . C105 C 0.7600(7) 1.0403(4) 0.4049(2) 0.137(4) Uani 1 1 d D . . H10J H 0.8009 1.0216 0.3731 0.165 Uiso 0.50 1 calc PR D 1 H10K H 0.6809 1.0335 0.4132 0.165 Uiso 0.50 1 calc PR D 1 H10L H 0.7996 1.0209 0.3733 0.165 Uiso 1 1 d R D 2 H10M H 0.6806 1.0340 0.4139 0.165 Uiso 1 1 d R D 2 C106 C 0.8072(5) 0.9651(3) 0.5022(2) 0.0731(15) Uani 1 1 d . . . H106 H 0.7413 0.9486 0.5037 0.088 Uiso 0.50 1 calc PR E 1 H107 H 0.7412 0.9486 0.5038 0.088 Uiso 0.50 1 d PR E 2 C109 C 0.8607(4) 0.8818(2) 0.60199(15) 0.0544(11) Uani 1 1 d . . . H10N H 0.8363 0.8428 0.5973 0.065 Uiso 1 1 calc R F 1 H10O H 0.9390 0.8630 0.6149 0.065 Uiso 1 1 calc R F 1 Cl1 Cl 0.1062(4) 0.3991(2) 0.8287(2) 0.2433(19) Uani 1 1 d . G 2 Cl2 Cl -0.1042(8) 0.4740(5) 0.7915(4) 0.419(5) Uani 1 1 d . G 2 C115 C 0.0195(7) 0.4115(4) 0.7835(3) 0.0974(19) Uani 1 1 d . G 2 H11C H -0.0004 0.3668 0.7888 0.117 Uiso 1 1 calc R G 2 H11D H 0.0568 0.4269 0.7440 0.117 Uiso 1 1 calc R G 2 C29' C 0.6140(8) 0.5459(5) 0.7279(5) 0.072(3) Uani 0.548(11) 1 d PD A 2 C30' C 0.566(2) 0.6159(8) 0.6833(8) 0.183(15) Uani 0.548(11) 1 d PD A 2 H30D H 0.5119 0.6472 0.7028 0.274 Uiso 0.548(11) 1 calc PR A 2 H30E H 0.5270 0.6077 0.6559 0.274 Uiso 0.548(11) 1 calc PR A 2 H30F H 0.6294 0.6376 0.6626 0.274 Uiso 0.548(11) 1 calc PR A 2 C31' C 0.6686(12) 0.5643(10) 0.7702(8) 0.193(10) Uani 0.548(11) 1 d PD A 2 H31D H 0.6150 0.6028 0.7821 0.289 Uiso 0.548(11) 1 calc PR A 2 H31E H 0.7394 0.5786 0.7514 0.289 Uiso 0.548(11) 1 calc PR A 2 H31F H 0.6863 0.5231 0.8041 0.289 Uiso 0.548(11) 1 calc PR A 2 C32' C 0.5143(15) 0.5154(11) 0.7598(8) 0.155(13) Uani 0.548(11) 1 d PD A 2 H32D H 0.5169 0.5046 0.8014 0.233 Uiso 0.548(11) 1 calc PR A 2 H32E H 0.5187 0.4724 0.7510 0.233 Uiso 0.548(11) 1 calc PR A 2 H32F H 0.4424 0.5494 0.7479 0.233 Uiso 0.548(11) 1 calc PR A 2 N1 N 1.2830(4) 0.3526(3) 0.46910(17) 0.0829(14) Uani 1 1 d . . . N2 N 1.2445(5) 0.3065(3) 0.45544(19) 0.0985(16) Uani 1 1 d . . . N3 N 1.1675(4) 0.2851(3) 0.4977(2) 0.0848(13) Uani 1 1 d . . . N4 N 0.9160(4) 0.1322(2) 0.60104(15) 0.0612(10) Uani 1 1 d . . . N5 N 1.0230(4) 0.0940(3) 0.6028(2) 0.1010(17) Uani 1 1 d . . . N6 N 1.0657(4) 0.0987(3) 0.64600(19) 0.0912(15) Uani 1 1 d . . . N7 N 0.5149(4) 1.2415(3) 0.57416(18) 0.0817(13) Uani 1 1 d . . . N8 N 0.5452(5) 1.2571(3) 0.5183(2) 0.0971(15) Uani 1 1 d . . . N9 N 0.5004(4) 1.2171(2) 0.49860(16) 0.0833(14) Uani 1 1 d . . . C107 C 0.8647(8) 0.9380(5) 0.5439(3) 0.050(2) Uani 0.50 1 d P H 1 N10 N 0.8282(6) 1.0102(4) 0.4604(3) 0.0522(18) Uani 0.50 1 d PD H 1 N11 N 0.9250(6) 1.0177(4) 0.4707(3) 0.0558(18) Uani 0.50 1 d P . 1 N12 N 0.9482(6) 0.9737(4) 0.5220(3) 0.0528(17) Uani 0.50 1 d P . 1 C108 C 0.7943(7) 0.9150(5) 0.5494(3) 0.0440(19) Uani 0.50 1 d P H 2 N10' N 0.7439(6) 0.9831(3) 0.4650(2) 0.0465(16) Uani 0.50 1 d PD H 2 N11' N 0.6685(6) 0.9444(4) 0.4895(3) 0.0579(19) Uani 0.50 1 d P H 2 N12' N 0.6988(6) 0.9037(4) 0.5399(3) 0.0584(19) Uani 0.50 1 d P H 2 O1 O 1.2224(2) 0.28147(13) 0.69477(11) 0.0464(7) Uani 1 1 d . . . H1 H 1.2300 0.3147 0.6647 0.070 Uiso 1 1 calc R . . O2 O 0.9626(2) 0.34606(15) 0.64481(11) 0.0527(7) Uani 1 1 d . . . H2 H 0.9587 0.3048 0.6637 0.079 Uiso 1 1 calc R . . O3 O 1.1872(2) 0.39433(14) 0.60171(10) 0.0471(7) Uani 1 1 d . . . O4 O 1.0203(2) 0.21318(12) 0.72149(9) 0.0393(6) Uani 1 1 d . . . O5 O 0.9432(4) 0.2140(3) 0.47944(16) 0.1057(14) Uani 1 1 d . . . O6 O 0.7282(2) 1.03358(15) 0.68427(11) 0.0514(7) Uani 1 1 d . . . H6 H 0.6681 1.0659 0.6788 0.077 Uiso 1 1 calc R . . O7 O 0.5348(2) 0.95075(15) 0.66019(11) 0.0535(7) Uani 1 1 d . . . H7 H 0.5985 0.9300 0.6476 0.080 Uiso 1 1 calc R . . O8 O 0.4801(2) 1.09519(14) 0.67473(10) 0.0509(7) Uani 1 1 d . . . O9 O 0.7847(2) 0.90635(13) 0.64576(10) 0.0482(7) Uani 1 1 d . H . O10 O 0.6894(4) 1.1440(2) 0.43188(15) 0.0940(12) Uani 1 1 d . . . O11 O 0.5441(11) 0.9747(6) 0.4574(6) 0.294(6) Uani 1 1 d . . . O12 O 0.4975(12) 0.5752(9) 0.9944(6) 0.335(7) Uani 1 1 d . . . O13 O 0.6461(7) 0.2858(5) 0.6312(4) 0.201(3) Uani 1 1 d . . . O14 O 0.6953(12) 0.3702(6) 0.5852(4) 0.290(6) Uani 1 1 d . . . O15 O 0.5254(14) 0.4710(6) 0.5340(7) 0.385(12) Uani 1 1 d . . . O16 O 0.7043(6) 0.4098(3) 0.4628(3) 0.167(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.034(2) 0.038(2) 0.040(2) -0.0146(17) -0.0015(15) -0.0033(17) C2 0.036(2) 0.032(2) 0.041(2) -0.0086(16) -0.0004(16) -0.0029(17) C3 0.040(2) 0.041(2) 0.043(2) -0.0038(17) -0.0058(17) -0.0085(19) C4 0.036(2) 0.043(2) 0.044(2) -0.0113(18) -0.0019(16) -0.0058(18) C5 0.039(2) 0.042(2) 0.043(2) -0.0105(18) -0.0003(16) -0.0114(18) C6 0.033(2) 0.036(2) 0.044(2) -0.0093(17) 0.0011(16) -0.0053(17) C7 0.048(2) 0.057(3) 0.044(2) -0.0059(19) -0.0051(18) -0.016(2) C8 0.088(4) 0.139(5) 0.057(3) -0.043(3) 0.008(3) -0.051(4) C9 0.065(3) 0.070(3) 0.065(3) -0.015(2) -0.024(2) -0.008(3) C10 0.086(4) 0.074(3) 0.063(3) -0.022(3) -0.017(2) -0.035(3) C11 0.040(2) 0.048(2) 0.043(2) -0.0089(18) 0.0035(17) -0.0127(19) C12 0.039(2) 0.038(2) 0.0333(18) -0.0011(16) 0.0040(16) -0.0109(18) C13 0.045(2) 0.034(2) 0.0318(18) -0.0015(16) 0.0040(16) -0.0114(18) C14 0.051(2) 0.047(2) 0.0335(19) 0.0024(18) -0.0009(17) -0.017(2) C15 0.049(3) 0.046(3) 0.053(2) -0.005(2) 0.000(2) -0.004(2) C16 0.054(3) 0.047(3) 0.055(2) -0.011(2) 0.003(2) -0.012(2) C17 0.051(2) 0.043(2) 0.047(2) -0.0097(19) -0.0050(18) -0.013(2) C18 0.077(3) 0.057(3) 0.076(3) -0.027(3) -0.001(3) -0.008(3) C19 0.142(6) 0.080(4) 0.075(4) -0.041(3) 0.003(4) -0.024(4) C20 0.106(5) 0.088(4) 0.136(6) -0.066(4) 0.004(4) 0.007(4) C21 0.147(6) 0.063(4) 0.106(4) -0.034(3) 0.010(4) -0.048(4) C22 0.053(3) 0.049(3) 0.042(2) 0.0087(19) -0.0152(18) -0.014(2) C23 0.046(2) 0.048(3) 0.052(2) 0.004(2) -0.0153(19) -0.015(2) C24 0.042(2) 0.045(2) 0.042(2) -0.0037(18) -0.0160(17) -0.010(2) C25 0.043(2) 0.041(2) 0.041(2) 0.0000(17) -0.0149(17) -0.0107(19) C26 0.043(2) 0.049(3) 0.077(3) -0.002(2) 0.001(2) -0.012(2) C27 0.049(3) 0.041(3) 0.141(5) 0.000(3) 0.017(3) -0.006(2) C28 0.049(3) 0.036(3) 0.123(4) 0.021(3) -0.002(3) -0.009(2) C29 0.044(6) 0.047(7) 0.077(8) -0.005(6) -0.005(6) -0.010(5) C30 0.042(6) 0.053(7) 0.160(14) -0.017(8) -0.015(7) 0.006(5) C31 0.111(14) 0.025(8) 0.111(14) -0.034(8) 0.043(10) -0.023(8) C32 0.065(11) 0.054(13) 0.26(3) -0.036(14) 0.021(15) -0.032(11) C33 0.040(2) 0.050(2) 0.0365(19) -0.0116(17) -0.0041(16) -0.0173(19) C34 0.039(2) 0.033(2) 0.0380(19) -0.0068(16) -0.0047(15) -0.0121(17) C35 0.045(2) 0.0305(19) 0.0324(18) -0.0068(15) 0.0014(16) -0.0117(17) C36 0.038(2) 0.0281(19) 0.0378(19) -0.0029(15) -0.0036(15) -0.0088(16) C37 0.042(2) 0.044(2) 0.0365(19) -0.0098(17) -0.0098(16) -0.0111(18) C38 0.046(2) 0.041(2) 0.0385(19) -0.0119(17) -0.0055(17) -0.0125(19) C39 0.037(2) 0.043(2) 0.040(2) -0.0141(17) 0.0021(16) -0.0078(18) C40 0.056(3) 0.060(3) 0.045(2) -0.027(2) -0.0019(19) -0.012(2) C41 0.210(9) 0.239(9) 0.064(4) -0.079(5) 0.064(5) -0.158(8) C42 0.197(9) 0.166(8) 0.090(5) -0.094(5) -0.038(5) 0.071(7) C43 0.095(4) 0.173(7) 0.072(3) -0.071(4) -0.008(3) -0.033(5) C44 0.044(2) 0.033(2) 0.043(2) -0.0045(17) -0.0069(17) -0.0040(18) C45 0.077(3) 0.066(3) 0.042(2) -0.010(2) 0.005(2) -0.024(3) C46 0.070(3) 0.065(3) 0.036(2) -0.013(2) -0.005(2) -0.003(3) C47 0.090(4) 0.096(4) 0.062(3) -0.045(3) 0.001(3) -0.027(3) C48 0.109(6) 0.132(6) 0.161(7) -0.105(6) -0.026(5) -0.011(5) C49 0.115(5) 0.097(5) 0.083(4) -0.024(3) -0.015(3) -0.049(4) C50 0.086(4) 0.114(5) 0.078(4) -0.038(4) -0.028(3) -0.017(4) C51 0.087(4) 0.085(4) 0.061(3) -0.035(3) -0.024(3) -0.008(3) C52 0.060(3) 0.055(3) 0.049(2) -0.023(2) 0.002(2) -0.017(2) C53 0.060(3) 0.047(2) 0.045(2) -0.0183(19) -0.006(2) -0.007(2) C54 0.069(3) 0.039(2) 0.044(2) -0.0095(18) -0.0069(19) -0.017(2) C55 0.050(2) 0.055(3) 0.035(2) -0.0036(18) -0.0009(17) -0.025(2) C56 0.045(2) 0.055(3) 0.041(2) -0.0142(19) 0.0055(17) -0.020(2) C57 0.041(2) 0.053(3) 0.044(2) -0.0105(19) -0.0051(17) -0.012(2) C58 0.047(2) 0.054(3) 0.041(2) -0.0068(19) -0.0049(17) -0.023(2) C59 0.049(2) 0.042(2) 0.045(2) -0.0110(18) -0.0002(18) -0.017(2) C60 0.050(2) 0.044(2) 0.043(2) -0.0021(18) -0.0014(18) -0.020(2) C61 0.056(3) 0.058(3) 0.044(2) -0.013(2) -0.0071(19) -0.014(2) C62 0.122(5) 0.074(4) 0.047(3) -0.009(2) -0.015(3) -0.028(3) C63 0.070(3) 0.133(5) 0.068(3) -0.034(3) -0.022(3) -0.026(4) C64 0.099(4) 0.078(4) 0.059(3) -0.027(3) -0.025(3) -0.014(3) C65 0.059(3) 0.048(3) 0.050(2) -0.002(2) -0.006(2) -0.019(2) C66 0.037(2) 0.037(2) 0.040(2) -0.0092(17) -0.0065(16) -0.0012(17) C67 0.037(2) 0.037(2) 0.0342(18) -0.0101(16) -0.0023(15) 0.0066(18) C68 0.037(2) 0.040(2) 0.041(2) -0.0144(17) -0.0135(16) 0.0053(18) C69 0.036(2) 0.044(2) 0.042(2) -0.0124(17) -0.0047(16) -0.0051(18) C70 0.038(2) 0.040(2) 0.0389(19) -0.0154(17) -0.0024(16) -0.0043(18) C71 0.046(2) 0.039(2) 0.0373(19) -0.0103(17) -0.0076(16) -0.0112(19) C72 0.060(3) 0.057(3) 0.038(2) -0.0054(19) -0.0080(19) -0.020(2) C73 0.105(4) 0.089(4) 0.050(3) 0.008(3) -0.015(3) -0.046(4) C74 0.086(4) 0.124(5) 0.060(3) 0.024(3) -0.033(3) -0.036(4) C75 0.145(6) 0.098(4) 0.042(3) -0.025(3) 0.024(3) -0.033(4) C76 0.053(3) 0.050(3) 0.051(2) -0.019(2) -0.0224(19) 0.000(2) C77 0.045(2) 0.053(3) 0.043(2) -0.0206(19) -0.0148(18) -0.003(2) C78 0.052(2) 0.049(2) 0.037(2) -0.0202(18) -0.0070(17) -0.008(2) C79 0.046(2) 0.065(3) 0.053(2) -0.036(2) -0.0053(19) -0.012(2) C80 0.051(3) 0.048(2) 0.061(2) -0.024(2) -0.008(2) -0.010(2) C81 0.045(2) 0.060(3) 0.054(2) -0.024(2) -0.0081(19) -0.013(2) C82 0.040(2) 0.066(3) 0.052(2) -0.029(2) -0.0073(18) -0.009(2) C83 0.060(3) 0.062(3) 0.089(4) -0.021(3) -0.001(3) -0.019(3) C84 0.137(13) 0.106(10) 0.063(9) -0.030(8) 0.028(7) -0.067(10) C85 0.116(13) 0.19(2) 0.129(19) 0.073(17) -0.007(11) -0.085(14) C86 0.32(4) 0.45(6) 0.16(2) -0.19(3) 0.13(3) -0.35(5) C86' 0.101(10) 0.083(9) 0.129(13) -0.039(8) 0.006(9) -0.060(8) C84' 0.48(6) 0.37(5) 0.061(10) -0.11(2) 0.09(2) -0.37(5) C85' 0.072(9) 0.078(10) 0.25(3) -0.049(12) 0.006(11) -0.021(8) C87 0.054(3) 0.073(3) 0.075(3) -0.054(3) 0.008(2) -0.019(2) C88 0.040(2) 0.044(2) 0.056(2) -0.028(2) 0.0037(18) -0.0028(19) C89 0.040(2) 0.038(2) 0.041(2) -0.0171(17) -0.0033(16) 0.0030(18) C90 0.037(2) 0.056(3) 0.039(2) -0.0204(19) 0.0031(16) -0.0078(19) C91 0.044(2) 0.072(3) 0.044(2) -0.017(2) -0.0070(18) -0.012(2) C92 0.049(3) 0.058(3) 0.050(2) -0.005(2) 0.005(2) -0.005(2) C93 0.047(2) 0.049(3) 0.058(3) -0.018(2) 0.006(2) -0.009(2) C94 0.066(4) 0.064(4) 0.037(3) 0.005(3) 0.006(3) -0.004(3) C95 0.142(7) 0.140(8) 0.058(4) -0.016(5) 0.016(4) -0.054(7) C96 0.147(9) 0.192(11) 0.062(5) 0.032(6) -0.030(6) -0.062(8) C97 0.306(14) 0.148(9) 0.115(7) 0.027(6) 0.023(9) 0.024(10) C95' 0.064(14) 0.049(14) 0.014(9) 0.029(9) -0.015(9) -0.007(11) C96' 0.091(19) 0.09(2) 0.103(19) 0.003(15) -0.010(15) -0.039(16) C97' 0.102(18) 0.080(16) 0.018(10) -0.014(10) 0.020(12) 0.007(14) C98 0.050(2) 0.074(3) 0.043(2) -0.023(2) 0.0049(18) -0.023(2) C99 0.062(3) 0.056(3) 0.044(2) -0.004(2) -0.004(2) 0.013(2) C100 0.066(3) 0.054(3) 0.045(2) -0.011(2) -0.011(2) 0.001(2) C101 0.098(4) 0.065(3) 0.054(3) -0.023(3) -0.027(3) 0.016(3) C102 0.158(6) 0.076(4) 0.039(3) -0.013(3) -0.013(3) 0.029(4) C103 0.126(5) 0.195(7) 0.075(4) -0.072(4) -0.044(4) 0.016(5) C104 0.082(4) 0.154(6) 0.061(3) -0.057(4) 0.000(3) 0.001(4) C105 0.204(8) 0.110(5) 0.032(3) -0.028(3) -0.022(3) 0.081(5) C106 0.110(4) 0.059(3) 0.048(3) -0.025(3) -0.008(3) -0.005(3) C109 0.066(3) 0.056(3) 0.033(2) -0.0186(19) -0.0064(18) 0.006(2) Cl1 0.213(4) 0.202(3) 0.259(4) -0.031(3) 0.030(3) -0.043(3) Cl2 0.403(10) 0.396(10) 0.433(10) 0.023(8) -0.112(8) -0.199(9) C115 0.099(5) 0.090(5) 0.094(4) -0.011(4) -0.013(4) -0.029(4) C29' 0.059(6) 0.052(6) 0.097(9) -0.021(6) -0.004(6) -0.003(5) C30' 0.23(3) 0.096(14) 0.107(13) -0.006(10) 0.039(16) 0.074(15) C31' 0.137(14) 0.21(2) 0.24(2) -0.17(2) 0.004(15) 0.052(14) C32' 0.115(16) 0.039(8) 0.23(2) -0.016(10) 0.105(15) 0.010(8) N1 0.094(3) 0.096(3) 0.045(2) -0.027(2) 0.001(2) 0.000(3) N2 0.105(4) 0.129(5) 0.057(3) -0.045(3) -0.005(3) -0.001(4) N3 0.087(3) 0.097(3) 0.086(3) -0.058(3) -0.012(3) -0.005(3) N4 0.074(3) 0.063(2) 0.055(2) -0.0309(19) -0.0178(19) -0.005(2) N5 0.085(3) 0.137(4) 0.091(3) -0.081(3) -0.029(3) 0.028(3) N6 0.077(3) 0.120(4) 0.084(3) -0.072(3) -0.033(2) 0.031(3) N7 0.096(3) 0.091(3) 0.058(3) -0.016(2) -0.001(2) -0.036(3) N8 0.123(4) 0.097(4) 0.067(3) -0.022(3) 0.008(3) -0.034(3) N9 0.116(4) 0.068(3) 0.039(2) -0.004(2) -0.006(2) 0.004(3) C107 0.054(6) 0.054(5) 0.037(5) -0.022(4) -0.008(4) 0.007(5) N10 0.063(5) 0.051(4) 0.039(4) -0.017(4) -0.003(3) -0.004(4) N11 0.060(5) 0.063(5) 0.047(4) -0.017(4) -0.012(3) -0.014(4) N12 0.056(4) 0.063(5) 0.046(4) -0.024(4) 0.001(3) -0.019(4) C108 0.037(5) 0.054(5) 0.044(5) -0.023(4) 0.001(4) -0.009(4) N10' 0.053(4) 0.056(4) 0.031(3) -0.016(3) -0.014(3) -0.004(4) N11' 0.047(4) 0.081(5) 0.050(4) -0.019(4) -0.021(3) -0.014(4) N12' 0.058(5) 0.066(5) 0.055(4) -0.015(4) -0.004(4) -0.026(4) O1 0.0539(16) 0.0396(15) 0.0450(15) -0.0102(12) -0.0063(12) -0.0121(13) O2 0.0619(18) 0.0476(17) 0.0406(14) -0.0054(13) 0.0026(13) -0.0148(15) O3 0.0597(17) 0.0489(16) 0.0297(13) -0.0075(12) -0.0005(11) -0.0161(14) O4 0.0497(15) 0.0354(14) 0.0332(12) -0.0110(11) 0.0003(11) -0.0127(12) O5 0.121(4) 0.145(4) 0.068(2) -0.044(2) -0.010(2) -0.044(3) O6 0.0461(16) 0.0607(18) 0.0434(15) -0.0170(13) -0.0069(12) -0.0035(14) O7 0.0508(17) 0.0541(18) 0.0497(15) -0.0167(14) 0.0012(13) -0.0059(15) O8 0.0489(16) 0.0501(17) 0.0328(13) -0.0039(12) -0.0035(11) 0.0095(13) O9 0.0599(17) 0.0425(15) 0.0367(14) -0.0169(12) -0.0085(12) 0.0047(13) O10 0.104(3) 0.107(3) 0.062(2) -0.034(2) -0.008(2) 0.000(3) O11 0.304(13) 0.210(9) 0.369(15) -0.078(9) 0.002(11) -0.097(10) O12 0.287(13) 0.385(16) 0.281(12) -0.122(12) 0.047(10) -0.023(13) O13 0.162(6) 0.228(8) 0.245(8) -0.119(7) -0.063(6) -0.010(6) O14 0.456(17) 0.280(11) 0.170(7) -0.097(8) -0.163(9) -0.030(12) O15 0.413(18) 0.222(12) 0.51(2) -0.172(14) 0.32(2) -0.201(14) O16 0.221(6) 0.105(4) 0.140(4) -0.021(3) 0.073(4) -0.061(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.362(4) . ? C1 C6 1.392(5) . ? C1 C2 1.405(5) . ? C2 C3 1.379(5) . ? C2 C44 1.524(5) . ? C3 C4 1.377(5) . ? C3 H3 0.9500 . ? C4 C5 1.386(5) . ? C4 C7 1.534(6) . ? C5 C6 1.387(5) . ? C5 H5 0.9500 . ? C6 C11 1.529(5) . ? C7 C10 1.536(6) . ? C7 C9 1.533(6) . ? C7 C8 1.544(6) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.519(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C17 1.380(5) . ? C12 C13 1.390(5) . ? C13 C14 1.382(5) . ? C13 O3 1.383(4) . ? C14 C15 1.387(6) . ? C14 C22 1.531(6) . ? C15 C16 1.392(6) . ? C15 H15 0.9500 . ? C16 C17 1.398(6) . ? C16 C18 1.537(6) . ? C17 H17 0.9500 . ? C18 C21 1.530(7) . ? C18 C20 1.530(8) . ? C18 C19 1.550(8) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.505(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C28 1.374(7) . ? C23 C24 1.418(6) . ? C24 O2 1.348(5) . ? C24 C25 1.405(5) . ? C25 C26 1.361(6) . ? C25 C33 1.520(5) . ? C26 C27 1.393(6) . ? C26 H26 0.9500 . ? C27 C28 1.395(7) . ? C27 C29 1.531(9) . ? C27 C29' 1.571(9) . ? C28 H28 0.9500 . ? C29 C32 1.526(9) . ? C29 C30 1.523(9) . ? C29 C31 1.534(9) . ? 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 C34 1.519(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.383(5) . ? C34 C39 1.402(5) . ? C35 O4 1.393(4) . ? C35 C36 1.402(5) . ? C36 C37 1.389(5) . ? C36 C44 1.519(5) . ? C37 C38 1.400(5) . ? C37 H37 0.9500 . ? C38 C39 1.391(5) . ? C38 C40 1.527(5) . ? C39 H39 0.9500 . ? C40 C43 1.485(7) . ? C40 C42 1.509(8) . ? C40 C41 1.513(8) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 O3 1.445(5) . ? C45 C46 1.472(7) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 N1 1.329(6) . ? C46 C47 1.355(7) . ? C47 N3 1.331(6) . ? C47 H47 0.9500 . ? C48 N3 1.417(8) . ? C48 C49 1.434(9) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 O5 1.404(7) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 O5 1.408(7) . ? C50 C51 1.502(8) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 N4 1.467(6) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 N4 1.330(5) . ? C52 C53 1.365(6) . ? C52 H52 0.9500 . ? C53 N6 1.346(6) . ? C53 C54 1.480(5) . ? C54 O4 1.443(4) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 O6 1.360(5) . ? C55 C60 1.399(6) . ? C55 C56 1.401(6) . ? C56 C57 1.382(5) . ? C56 C98 1.501(6) . ? C57 C58 1.394(6) . ? C57 H57 0.9500 . ? C58 C59 1.393(6) . ? C58 C61 1.542(5) . ? C59 C60 1.388(5) . ? C59 H59 0.9500 . ? C60 C65 1.517(6) . ? C61 C64 1.497(7) . ? C61 C63 1.525(7) . ? C61 C62 1.531(6) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 C66 1.522(5) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C71 1.385(5) . ? C66 C67 1.395(5) . ? C67 C68 1.379(5) . ? C67 O8 1.405(4) . ? C68 C69 1.394(5) . ? C68 C76 1.519(5) . ? C69 C70 1.375(5) . ? C69 H69 0.9500 . ? C70 C71 1.387(5) . ? C70 C72 1.532(5) . ? C71 H71 0.9500 . ? C72 C73 1.503(6) . ? C72 C74 1.533(7) . ? C72 C75 1.548(7) . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 C77 1.504(6) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 C82 1.375(6) . ? C77 C78 1.400(6) . ? C78 O7 1.359(5) . ? C78 C79 1.399(6) . ? C79 C80 1.376(6) . ? C79 C87 1.517(6) . ? C80 C81 1.398(6) . ? C80 H80 0.9500 . ? C81 C82 1.386(6) . ? C81 C83 1.519(6) . ? C82 H82 0.9500 . ? C83 C84' 1.474(8) . ? C83 C86 1.497(6) . ? C83 C84 1.531(6) . ? C83 C85 1.542(6) . ? C83 C86' 1.548(8) . ? C83 C85' 1.559(8) . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? C86 H86A 1.0119 . ? C86 H86B 1.0123 . ? C86 H86C 1.0121 . ? C86' H86D 0.9800 . ? C86' H86E 0.9800 . ? C86' H86F 0.9800 . ? C84' H84D 0.9800 . ? C84' H84E 0.9800 . ? C84' H84F 0.9800 . ? C85' H85D 0.9800 . ? C85' H85E 0.9800 . ? C85' H85F 0.9800 . ? C87 C88 1.535(6) . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? C88 C93 1.379(6) . ? C88 C89 1.386(5) . ? C89 C90 1.389(5) . ? C89 O9 1.390(4) . ? C90 C91 1.384(5) . ? C90 C98 1.532(6) . ? C91 C92 1.376(6) . ? C91 H91 0.9500 . ? C92 C93 1.388(6) . ? C92 C94 1.521(6) . ? C93 H93 0.9500 . ? C94 C97 1.492(7) . ? C94 C96 1.490(7) . ? C94 C96' 1.515(9) . ? C94 C97' 1.530(9) . ? C94 C95 1.548(7) . ? C94 C95' 1.557(9) . ? C95 H95A 0.9800 . ? C95 H95B 0.9800 . ? C95 H95C 0.9800 . ? C96 H96A 0.9800 . ? C96 H96B 0.9800 . ? C96 H96C 0.9800 . ? C97 H97A 0.9800 . ? C97 H97B 0.9800 . ? C97 H97C 0.9800 . ? C95' H95D 0.9800 . ? C95' H95E 0.9800 . ? C95' H95F 0.9800 . ? C96' H96D 0.9800 . ? C96' H96E 0.9800 . ? C96' H96F 0.9800 . ? C97' H97D 0.9800 . ? C97' H97E 0.9800 . ? C97' H97F 0.9800 . ? C98 H98A 0.9900 . ? C98 H98B 0.9900 . ? C99 O8 1.448(5) . ? C99 C100 1.473(6) . ? C99 H99A 0.9900 . ? C99 H99B 0.9900 . ? C100 C101 1.320(6) . ? C100 N7 1.357(6) . ? C101 N9 1.287(7) . ? C101 H101 0.9500 . ? C102 C103 1.436(9) . ? C102 N9 1.478(6) . ? C102 H10D 0.9900 . ? C102 H10E 0.9900 . ? C103 O10 1.291(8) . ? C103 H10F 0.9900 . ? C103 H10G 0.9900 . ? C104 C105 1.389(9) . ? C104 O10 1.399(7) . ? C104 H10H 0.9900 . ? C104 H10I 0.9900 . ? C105 N10 1.581(8) . ? C105 N10' 1.581(8) . ? C105 H10J 0.9900 . ? C105 H10K 0.9900 . ? C105 H10L 0.9900 . ? C105 H10M 0.9900 . ? C106 N10 1.186(8) . ? C106 N10' 1.201(8) . ? C106 C107 1.230(10) . ? C106 C108 1.296(10) . ? C106 H106 0.9500 . ? C106 H107 0.9500 . ? C109 O9 1.434(4) . ? C109 C108 1.509(9) . ? C109 C107 1.520(10) . ? C109 H10N 0.9900 . ? C109 H10O 0.9900 . ? Cl1 C115 1.583(8) . ? Cl2 C115 1.726(11) . ? C115 H11C 0.9900 . ? C115 H11D 0.9900 . ? C29' C32' 1.504(8) . ? C29' C30' 1.532(9) . ? C29' C31' 1.534(9) . ? C30' H30D 0.9800 . ? C30' H30E 0.9800 . ? C30' H30F 0.9800 . ? C31' H31D 0.9800 . ? C31' H31E 0.9800 . ? C31' H31F 0.9800 . ? C32' H32D 0.9800 . ? C32' H32E 0.9800 . ? C32' H32F 0.9800 . ? N1 N2 1.339(7) . ? N2 N3 1.323(7) . ? N4 N5 1.324(6) . ? N5 N6 1.313(6) . ? N7 N8 1.318(6) . ? N8 N9 1.366(7) . ? C107 N12 1.357(13) . ? N10 N11 1.313(10) . ? N11 N12 1.313(9) . ? N11 N12 1.654(10) 2_776 ? N12 N11 1.654(10) 2_776 ? N12 N12 1.864(14) 2_776 ? C108 N12' 1.325(12) . ? C108 H107 1.2851 . ? N10' N11' 1.325(10) . ? N10' H10M 1.5144 . ? N10' H107 0.9873 . ? N11' N12' 1.296(10) . ? N11' H107 1.0467 . ? N12' H107 1.2187 . ? O1 H1 0.8400 . ? O2 H2 0.8400 . ? O6 H6 0.8400 . ? O7 H7 0.8400 . ? O15 O15 1.80(4) 2_666 ? 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 O1 C1 C6 124.7(3) . . ? O1 C1 C2 115.1(3) . . ? C6 C1 C2 120.2(3) . . ? C3 C2 C1 118.5(3) . . ? C3 C2 C44 121.5(3) . . ? C1 C2 C44 119.9(3) . . ? C2 C3 C4 123.1(3) . . ? C2 C3 H3 118.5 . . ? C4 C3 H3 118.5 . . ? C3 C4 C5 116.8(4) . . ? C3 C4 C7 119.6(3) . . ? C5 C4 C7 123.6(3) . . ? C4 C5 C6 123.1(4) . . ? C4 C5 H5 118.4 . . ? C6 C5 H5 118.4 . . ? C5 C6 C1 118.2(3) . . ? C5 C6 C11 120.4(3) . . ? C1 C6 C11 121.4(3) . . ? C10 C7 C9 107.0(4) . . ? C10 C7 C4 112.6(3) . . ? C9 C7 C4 108.8(4) . . ? C10 C7 C8 108.9(4) . . ? C9 C7 C8 109.1(4) . . ? C4 C7 C8 110.3(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.4 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C6 114.7(3) . . ? C12 C11 H11A 108.6 . . ? C6 C11 H11A 108.6 . . ? C12 C11 H11B 108.6 . . ? C6 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? C17 C12 C13 118.2(4) . . ? C17 C12 C11 120.6(4) . . ? C13 C12 C11 121.1(3) . . ? C14 C13 O3 119.3(4) . . ? C14 C13 C12 121.6(4) . . ? O3 C13 C12 119.0(3) . . ? C13 C14 C15 118.2(4) . . ? C13 C14 C22 121.8(4) . . ? C15 C14 C22 119.9(4) . . ? C16 C15 C14 122.4(4) . . ? C16 C15 H15 118.8 . . ? C14 C15 H15 118.8 . . ? C15 C16 C17 116.8(4) . . ? C15 C16 C18 122.2(4) . . ? C17 C16 C18 121.0(4) . . ? C12 C17 C16 122.5(4) . . ? C12 C17 H17 118.8 . . ? C16 C17 H17 118.8 . . ? C21 C18 C20 107.2(5) . . ? C21 C18 C16 108.0(4) . . ? C20 C18 C16 112.7(5) . . ? C21 C18 C19 108.5(5) . . ? C20 C18 C19 110.6(5) . . ? C16 C18 C19 109.6(4) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C14 111.2(3) . . ? C23 C22 H22A 109.4 . . ? C14 C22 H22A 109.4 . . ? C23 C22 H22B 109.4 . . ? C14 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C28 C23 C24 117.9(4) . . ? C28 C23 C22 121.6(4) . . ? C24 C23 C22 120.4(4) . . ? O2 C24 C25 123.9(3) . . ? O2 C24 C23 116.6(3) . . ? C25 C24 C23 119.4(4) . . ? C26 C25 C24 119.4(4) . . ? C26 C25 C33 119.4(3) . . ? C24 C25 C33 121.2(4) . . ? C25 C26 C27 123.6(4) . . ? C25 C26 H26 118.2 . . ? C27 C26 H26 118.2 . . ? C26 C27 C28 115.5(5) . . ? C26 C27 C29 123.4(5) . . ? C28 C27 C29 115.7(5) . . ? C26 C27 C29' 120.5(5) . . ? C28 C27 C29' 121.8(5) . . ? C29 C27 C29' 36.9(5) . . ? C23 C28 C27 124.2(4) . . ? C23 C28 H28 117.9 . . ? C27 C28 H28 117.9 . . ? C32 C29 C30 106.8(8) . . ? C32 C29 C27 112.5(12) . . ? C30 C29 C27 121.9(8) . . ? C32 C29 C31 106.3(8) . . ? C30 C29 C31 107.5(7) . . ? C27 C29 C31 100.5(8) . . ? C25 C33 C34 110.5(3) . . ? C25 C33 H33A 109.6 . . ? C34 C33 H33A 109.6 . . ? C25 C33 H33B 109.6 . . ? C34 C33 H33B 109.6 . . ? H33A C33 H33B 108.1 . . ? C35 C34 C39 118.4(3) . . ? C35 C34 C33 121.4(3) . . ? C39 C34 C33 120.1(3) . . ? C34 C35 O4 118.4(3) . . ? C34 C35 C36 121.4(3) . . ? O4 C35 C36 120.1(3) . . ? C37 C36 C35 117.5(3) . . ? C37 C36 C44 119.9(3) . . ? C35 C36 C44 122.6(3) . . ? C36 C37 C38 123.4(3) . . ? C36 C37 H37 118.3 . . ? C38 C37 H37 118.3 . . ? C39 C38 C37 116.4(3) . . ? C39 C38 C40 121.2(3) . . ? C37 C38 C40 122.4(3) . . ? C38 C39 C34 122.5(3) . . ? C38 C39 H39 118.7 . . ? C34 C39 H39 118.7 . . ? C43 C40 C42 110.3(5) . . ? C43 C40 C41 108.3(5) . . ? C42 C40 C41 106.2(6) . . ? C43 C40 C38 113.0(4) . . ? C42 C40 C38 110.2(4) . . ? C41 C40 C38 108.6(4) . . ? C40 C41 H41A 109.4 . . ? 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 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.4 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C36 C44 C2 109.5(3) . . ? C36 C44 H44A 109.8 . . ? C2 C44 H44A 109.8 . . ? C36 C44 H44B 109.8 . . ? C2 C44 H44B 109.8 . . ? H44A C44 H44B 108.2 . . ? O3 C45 C46 106.6(4) . . ? O3 C45 H45A 110.4 . . ? C46 C45 H45A 110.4 . . ? O3 C45 H45B 110.4 . . ? C46 C45 H45B 110.4 . . ? H45A C45 H45B 108.6 . . ? N1 C46 C47 109.8(5) . . ? N1 C46 C45 121.3(5) . . ? C47 C46 C45 128.8(4) . . ? N3 C47 C46 104.3(5) . . ? N3 C47 H47 127.9 . . ? C46 C47 H47 127.9 . . ? N3 C48 C49 114.7(6) . . ? N3 C48 H48A 108.6 . . ? C49 C48 H48A 108.6 . . ? N3 C48 H48B 108.6 . . ? C49 C48 H48B 108.6 . . ? H48A C48 H48B 107.6 . . ? O5 C49 C48 110.8(6) . . ? O5 C49 H49A 109.5 . . ? C48 C49 H49A 109.5 . . ? O5 C49 H49B 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 108.1 . . ? O5 C50 C51 112.8(5) . . ? O5 C50 H50A 109.0 . . ? C51 C50 H50A 109.0 . . ? O5 C50 H50B 109.0 . . ? C51 C50 H50B 109.0 . . ? H50A C50 H50B 107.8 . . ? N4 C51 C50 111.7(4) . . ? N4 C51 H51A 109.3 . . ? C50 C51 H51A 109.3 . . ? N4 C51 H51B 109.3 . . ? C50 C51 H51B 109.3 . . ? H51A C51 H51B 107.9 . . ? N4 C52 C53 105.6(4) . . ? N4 C52 H52 127.2 . . ? C53 C52 H52 127.2 . . ? N6 C53 C52 107.6(4) . . ? N6 C53 C54 120.9(4) . . ? C52 C53 C54 130.8(4) . . ? O4 C54 C53 112.5(3) . . ? O4 C54 H54A 109.1 . . ? C53 C54 H54A 109.1 . . ? O4 C54 H54B 109.1 . . ? C53 C54 H54B 109.1 . . ? H54A C54 H54B 107.8 . . ? O6 C55 C60 121.0(4) . . ? O6 C55 C56 118.6(4) . . ? C60 C55 C56 120.4(4) . . ? C57 C56 C55 118.3(4) . . ? C57 C56 C98 121.7(4) . . ? C55 C56 C98 119.8(4) . . ? C56 C57 C58 123.5(4) . . ? C56 C57 H57 118.2 . . ? C58 C57 H57 118.2 . . ? C57 C58 C59 116.0(4) . . ? C57 C58 C61 121.3(4) . . ? C59 C58 C61 122.6(4) . . ? C60 C59 C58 123.1(4) . . ? C60 C59 H59 118.5 . . ? C58 C59 H59 118.5 . . ? C59 C60 C55 118.6(4) . . ? C59 C60 C65 120.4(4) . . ? C55 C60 C65 120.7(4) . . ? C64 C61 C63 106.9(4) . . ? C64 C61 C62 108.9(4) . . ? C63 C61 C62 110.8(4) . . ? C64 C61 C58 112.2(4) . . ? C63 C61 C58 110.6(3) . . ? C62 C61 C58 107.5(3) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C60 C65 C66 108.1(3) . . ? C60 C65 H65A 110.1 . . ? C66 C65 H65A 110.1 . . ? C60 C65 H65B 110.1 . . ? C66 C65 H65B 110.1 . . ? H65A C65 H65B 108.4 . . ? C71 C66 C67 118.1(3) . . ? C71 C66 C65 118.5(3) . . ? C67 C66 C65 123.2(3) . . ? C68 C67 C66 121.5(3) . . ? C68 C67 O8 119.8(3) . . ? C66 C67 O8 118.5(3) . . ? C67 C68 C69 118.0(3) . . ? C67 C68 C76 122.1(3) . . ? C69 C68 C76 119.6(4) . . ? C70 C69 C68 122.6(4) . . ? C70 C69 H69 118.7 . . ? C68 C69 H69 118.7 . . ? C69 C70 C71 117.5(3) . . ? C69 C70 C72 122.9(3) . . ? C71 C70 C72 119.5(3) . . ? C70 C71 C66 122.3(3) . . ? C70 C71 H71 118.9 . . ? C66 C71 H71 118.9 . . ? C73 C72 C74 107.6(4) . . ? C73 C72 C70 113.2(4) . . ? C74 C72 C70 109.6(4) . . ? C73 C72 C75 108.2(4) . . ? C74 C72 C75 110.0(5) . . ? C70 C72 C75 108.2(4) . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C72 C74 H74A 109.5 . . ? C72 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C72 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C72 C75 H75A 109.5 . . ? C72 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C72 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C77 C76 C68 109.8(3) . . ? C77 C76 H76A 109.7 . . ? C68 C76 H76A 109.7 . . ? C77 C76 H76B 109.7 . . ? C68 C76 H76B 109.7 . . ? H76A C76 H76B 108.2 . . ? C82 C77 C78 118.6(4) . . ? C82 C77 C76 121.3(4) . . ? C78 C77 C76 119.7(4) . . ? O7 C78 C79 121.5(3) . . ? O7 C78 C77 118.4(4) . . ? C79 C78 C77 120.1(4) . . ? C80 C79 C78 118.7(4) . . ? C80 C79 C87 121.0(4) . . ? C78 C79 C87 120.1(4) . . ? C79 C80 C81 123.0(4) . . ? C79 C80 H80 118.5 . . ? C81 C80 H80 118.5 . . ? C82 C81 C80 116.2(4) . . ? C82 C81 C83 122.0(4) . . ? C80 C81 C83 121.7(4) . . ? C77 C82 C81 123.3(4) . . ? C77 C82 H82 118.3 . . ? C81 C82 H82 118.3 . . ? C84' C83 C86 133.7(10) . . ? C84' C83 C81 114.0(7) . . ? C86 C83 C81 112.2(7) . . ? C84' C83 C84 52.7(8) . . ? C86 C83 C84 109.6(5) . . ? C81 C83 C84 113.0(6) . . ? C84' C83 C85 54.5(9) . . ? C86 C83 C85 108.3(6) . . ? C81 C83 C85 107.8(6) . . ? C84 C83 C85 105.6(5) . . ? C84' C83 C86' 109.8(7) . . ? C86 C83 C86' 48.6(8) . . ? C81 C83 C86' 111.4(6) . . ? C84 C83 C86' 135.5(7) . . ? C85 C83 C86' 62.4(8) . . ? C84' C83 C85' 108.7(7) . . ? C86 C83 C85' 56.8(8) . . ? C81 C83 C85' 108.8(7) . . ? C84 C83 C85' 59.2(7) . . ? C85 C83 C85' 143.4(9) . . ? C86' C83 C85' 103.5(6) . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? C83 C84 H84C 109.4 . . ? C83 C85 H85A 109.5 . . ? C83 C85 H85B 109.5 . . ? C83 C85 H85C 109.5 . . ? C83 C86 H86A 112.6 . . ? C83 C86 H86B 112.8 . . ? C83 C86 H86C 112.7 . . ? C83 C86' H86D 109.4 . . ? C83 C86' H86E 109.4 . . ? H86D C86' H86E 109.5 . . ? C83 C86' H86F 109.6 . . ? H86D C86' H86F 109.5 . . ? H86E C86' H86F 109.5 . . ? C83 C84' H84D 109.4 . . ? C83 C84' H84E 109.5 . . ? H84D C84' H84E 109.5 . . ? C83 C84' H84F 109.5 . . ? H84D C84' H84F 109.5 . . ? H84E C84' H84F 109.5 . . ? C83 C85' H85D 109.5 . . ? C83 C85' H85E 109.5 . . ? H85D C85' H85E 109.5 . . ? C83 C85' H85F 109.4 . . ? H85D C85' H85F 109.5 . . ? H85E C85' H85F 109.5 . . ? C79 C87 C88 109.5(3) . . ? C79 C87 H87A 109.8 . . ? C88 C87 H87A 109.8 . . ? C79 C87 H87B 109.8 . . ? C88 C87 H87B 109.8 . . ? H87A C87 H87B 108.2 . . ? C93 C88 C89 118.8(4) . . ? C93 C88 C87 119.1(4) . . ? C89 C88 C87 121.9(4) . . ? C90 C89 C88 121.0(3) . . ? C90 C89 O9 119.7(3) . . ? C88 C89 O9 119.1(3) . . ? C91 C90 C89 118.0(4) . . ? C91 C90 C98 120.7(4) . . ? C89 C90 C98 121.2(3) . . ? C92 C91 C90 122.7(4) . . ? C92 C91 H91 118.6 . . ? C90 C91 H91 118.6 . . ? C91 C92 C93 117.5(4) . . ? C91 C92 C94 121.8(4) . . ? C93 C92 C94 120.7(4) . . ? C88 C93 C92 121.9(4) . . ? C88 C93 H93 119.0 . . ? C92 C93 H93 119.0 . . ? C97 C94 C96 114.1(6) . . ? C97 C94 C96' 62.1(11) . . ? C96 C94 C96' 125.4(13) . . ? C97 C94 C92 106.4(5) . . ? C96 C94 C92 113.6(5) . . ? C96' C94 C92 119.5(13) . . ? C97 C94 C97' 142.6(11) . . ? C96 C94 C97' 38.9(10) . . ? C96' C94 C97' 108.1(8) . . ? C92 C94 C97' 109.2(10) . . ? C97 C94 C95 107.1(6) . . ? C96 C94 C95 106.7(5) . . ? C96' C94 C95 45.0(11) . . ? C92 C94 C95 108.6(5) . . ? C97' C94 C95 72.1(11) . . ? C97 C94 C95' 52.2(9) . . ? C96 C94 C95' 66.3(9) . . ? C96' C94 C95' 106.0(8) . . ? C92 C94 C95' 108.6(8) . . ? C97' C94 C95' 104.5(8) . . ? C95 C94 C95' 141.5(8) . . ? C94 C95 H95A 109.4 . . ? C94 C95 H95B 109.5 . . ? C94 C95 H95C 109.5 . . ? C94 C96 H96A 109.5 . . ? C94 C96 H96B 109.4 . . ? C94 C96 H96C 109.5 . . ? C94 C97 H97A 109.4 . . ? C94 C97 H97B 109.5 . . ? C94 C97 H97C 109.5 . . ? C94 C95' H95D 109.5 . . ? C94 C95' H95E 109.3 . . ? H95D C95' H95E 109.5 . . ? C94 C95' H95F 109.6 . . ? H95D C95' H95F 109.5 . . ? H95E C95' H95F 109.5 . . ? C94 C96' H96D 109.6 . . ? C94 C96' H96E 109.4 . . ? H96D C96' H96E 109.5 . . ? C94 C96' H96F 109.4 . . ? H96D C96' H96F 109.5 . . ? H96E C96' H96F 109.5 . . ? C94 C97' H97D 109.5 . . ? C94 C97' H97E 109.4 . . ? H97D C97' H97E 109.5 . . ? C94 C97' H97F 109.5 . . ? H97D C97' H97F 109.5 . . ? H97E C97' H97F 109.5 . . ? C56 C98 C90 110.9(3) . . ? C56 C98 H98A 109.5 . . ? C90 C98 H98A 109.5 . . ? C56 C98 H98B 109.5 . . ? C90 C98 H98B 109.5 . . ? H98A C98 H98B 108.0 . . ? O8 C99 C100 108.3(3) . . ? O8 C99 H99A 110.0 . . ? C100 C99 H99A 110.0 . . ? O8 C99 H99B 110.0 . . ? C100 C99 H99B 110.0 . . ? H99A C99 H99B 108.4 . . ? C101 C100 N7 105.7(4) . . ? C101 C100 C99 132.8(5) . . ? N7 C100 C99 121.6(4) . . ? N9 C101 C100 110.9(5) . . ? N9 C101 H101 124.6 . . ? C100 C101 H101 124.6 . . ? C103 C102 N9 114.0(5) . . ? C103 C102 H10D 108.8 . . ? N9 C102 H10D 108.8 . . ? C103 C102 H10E 108.7 . . ? N9 C102 H10E 108.8 . . ? H10D C102 H10E 107.7 . . ? O10 C103 C102 122.8(7) . . ? O10 C103 H10F 106.6 . . ? C102 C103 H10F 106.6 . . ? O10 C103 H10G 106.7 . . ? C102 C103 H10G 106.7 . . ? H10F C103 H10G 106.6 . . ? C105 C104 O10 116.3(6) . . ? C105 C104 H10H 108.2 . . ? O10 C104 H10H 108.2 . . ? C105 C104 H10I 108.2 . . ? O10 C104 H10I 108.2 . . ? H10H C104 H10I 107.4 . . ? C104 C105 N10 94.3(6) . . ? C104 C105 N10' 127.3(5) . . ? N10 C105 N10' 47.7(4) . . ? C104 C105 H10J 112.9 . . ? N10 C105 H10J 112.9 . . ? N10' C105 H10J 115.3 . . ? C104 C105 H10K 112.9 . . ? N10 C105 H10K 112.9 . . ? N10' C105 H10K 68.2 . . ? H10J C105 H10K 110.3 . . ? C104 C105 H10L 114.0 . . ? N10 C105 H10L 113.2 . . ? N10' C105 H10L 114.5 . . ? H10J C105 H10L 1.4 . . ? H10K C105 H10L 109.0 . . ? C104 C105 H10M 112.1 . . ? N10 C105 H10M 112.0 . . ? N10' C105 H10M 67.7 . . ? H10J C105 H10M 111.7 . . ? H10K C105 H10M 1.4 . . ? H10L C105 H10M 110.4 . . ? N10 C106 N10' 64.7(6) . . ? N10 C106 C107 124.7(9) . . ? N10' C106 C107 170.3(9) . . ? N10 C106 C108 174.3(8) . . ? N10' C106 C108 120.7(8) . . ? C107 C106 C108 49.8(6) . . ? N10 C106 H106 117.7 . . ? N10' C106 H106 53.0 . . ? C107 C106 H106 117.7 . . ? C108 C106 H106 67.9 . . ? N10 C106 H107 117.8 . . ? N10' C106 H107 53.1 . . ? C107 C106 H107 117.6 . . ? C108 C106 H107 67.8 . . ? H106 C106 H107 0.1 . . ? O9 C109 C108 103.8(4) . . ? O9 C109 C107 113.7(4) . . ? C108 C109 C107 41.2(4) . . ? O9 C109 H10N 108.8 . . ? C108 C109 H10N 75.4 . . ? C107 C109 H10N 108.8 . . ? O9 C109 H10O 108.8 . . ? C108 C109 H10O 143.7 . . ? C107 C109 H10O 108.8 . . ? H10N C109 H10O 107.7 . . ? Cl1 C115 Cl2 111.4(6) . . ? Cl1 C115 H11C 109.3 . . ? Cl2 C115 H11C 109.3 . . ? Cl1 C115 H11D 109.4 . . ? Cl2 C115 H11D 109.4 . . ? H11C C115 H11D 108.0 . . ? C32' C29' C30' 107.8(8) . . ? C32' C29' C31' 108.4(8) . . ? C30' C29' C31' 105.7(7) . . ? C32' C29' C27 107.1(9) . . ? C30' C29' C27 110.6(11) . . ? C31' C29' C27 116.9(8) . . ? C29' C30' H30D 109.4 . . ? C29' C30' H30E 109.5 . . ? H30D C30' H30E 109.5 . . ? C29' C30' H30F 109.5 . . ? H30D C30' H30F 109.5 . . ? H30E C30' H30F 109.5 . . ? C29' C31' H31D 109.5 . . ? C29' C31' H31E 109.5 . . ? H31D C31' H31E 109.5 . . ? C29' C31' H31F 109.4 . . ? H31D C31' H31F 109.5 . . ? H31E C31' H31F 109.5 . . ? C29' C32' H32D 109.5 . . ? C29' C32' H32E 109.4 . . ? H32D C32' H32E 109.5 . . ? C29' C32' H32F 109.5 . . ? H32D C32' H32F 109.5 . . ? H32E C32' H32F 109.5 . . ? C46 N1 N2 107.7(5) . . ? N3 N2 N1 106.6(4) . . ? N2 N3 C47 111.6(5) . . ? N2 N3 C48 118.7(5) . . ? C47 N3 C48 129.7(6) . . ? N5 N4 C52 110.4(4) . . ? N5 N4 C51 120.1(4) . . ? C52 N4 C51 129.5(4) . . ? N6 N5 N4 107.7(4) . . ? N5 N6 C53 108.7(4) . . ? N8 N7 C100 109.2(5) . . ? N7 N8 N9 106.3(4) . . ? C101 N9 N8 108.0(4) . . ? C101 N9 C102 132.1(6) . . ? N8 N9 C102 119.7(5) . . ? C106 C107 N12 97.0(8) . . ? C106 C107 C109 137.2(10) . . ? N12 C107 C109 125.8(8) . . ? C106 N10 N11 102.2(7) . . ? C106 N10 C105 124.3(7) . . ? N11 N10 C105 132.8(7) . . ? N10 N11 N12 106.5(7) . . ? N10 N11 N12 174.8(7) . 2_776 ? N12 N11 N12 76.9(6) . 2_776 ? N11 N12 C107 109.6(7) . . ? N11 N12 N11 103.1(6) . 2_776 ? C107 N12 N11 147.1(7) . 2_776 ? N11 N12 N12 59.8(5) . 2_776 ? C107 N12 N12 168.7(8) . 2_776 ? N11 N12 N12 43.3(4) 2_776 2_776 ? C106 C108 N12' 98.8(7) . . ? C106 C108 C109 131.8(8) . . ? N12' C108 C109 129.2(7) . . ? C106 C108 H107 43.2 . . ? N12' C108 H107 55.7 . . ? C109 C108 H107 174.4 . . ? C106 N10' N11' 101.7(6) . . ? C106 N10' C105 123.2(6) . . ? N11' N10' C105 135.1(7) . . ? C106 N10' H10M 155.4 . . ? N11' N10' H10M 99.4 . . ? C105 N10' H10M 37.2 . . ? C106 N10' H107 50.3 . . ? N11' N10' H107 51.3 . . ? C105 N10' H107 173.5 . . ? H10M N10' H107 148.5 . . ? N12' N11' N10' 109.0(6) . . ? N12' N11' H107 61.6 . . ? N10' N11' H107 47.4 . . ? N11' N12' C108 109.6(7) . . ? N11' N12' H107 49.1 . . ? C108 N12' H107 60.5 . . ? C1 O1 H1 109.5 . . ? C24 O2 H2 109.5 . . ? C13 O3 C45 115.4(3) . . ? C35 O4 C54 111.1(3) . . ? C49 O5 C50 115.5(5) . . ? C55 O6 H6 109.5 . . ? C78 O7 H7 109.5 . . ? C67 O8 C99 112.9(3) . . ? C89 O9 C109 114.1(3) . . ? C103 O10 C104 116.0(5) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.121 _refine_diff_density_min -0.962 _refine_diff_density_rms 0.108