# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author ; Toupet Loic G.M.C.M.-UMR6626 Universite de Rennes Campus de Beaulieu 35042 RENNES cedex , FRANCE ; _publ_contact_author_email loic.toupet@univ-rennes1.fr _publ_contact_author_fax '(33) 2 23 23 67 17' _publ_contact_author_phone '(33) 2 23 23 64 97' _publ_requested_coeditor_name ? _publ_contact_letter ? _publ_author_name 'Loic Toupet' data_mj48 _database_code_depnum_ccdc_archive 'CCDC 822184' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84.50 H136 B2 Cl6 O28 P2' _chemical_formula_weight 1896.19 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 16.0969(4) _cell_length_b 22.4367(5) _cell_length_c 27.7516(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10022.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 14444 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 29.14 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.257 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4036 _exptl_absorpt_coefficient_mu 0.274 _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 120(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 Saphire 3 Xcalibur' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 19.64 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 79214 _diffrn_reflns_av_R_equivalents 0.0994 _diffrn_reflns_av_sigmaI/netI 0.2294 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 27.00 _reflns_number_total 21429 _reflns_number_gt 8413 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,Version 1.171.26' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.26' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.26' _computing_structure_solution 'SIR-97_(Altomare & al., 1998)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON_(Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1316P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _chemical_absolute_configuration rm _refine_ls_abs_structure_Flack 0.08(12) _refine_ls_number_reflns 21429 _refine_ls_number_parameters 1029 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.2114 _refine_ls_R_factor_gt 0.0935 _refine_ls_wR_factor_ref 0.2645 _refine_ls_wR_factor_gt 0.2283 _refine_ls_goodness_of_fit_ref 0.932 _refine_ls_restrained_S_all 0.933 _refine_ls_shift/su_max 0.236 _refine_ls_shift/su_mean 0.020 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 C91 C 0.5517(12) 0.0608(6) 0.4007(5) 0.137(6) Uani 1 1 d . . . H91A H 0.6049 0.0389 0.3995 0.164 Uiso 1 1 calc R . . H91B H 0.5188 0.0494 0.3720 0.164 Uiso 1 1 calc R . . Cl1 Cl 0.4974(3) 0.0401(2) 0.45272(19) 0.1513(17) Uani 1 1 d . . . Cl2 Cl 0.5712(3) 0.13536(19) 0.39879(18) 0.1441(16) Uani 1 1 d . . . C92 C 0.9938(9) -0.1027(7) 0.4336(5) 0.124(5) Uani 1 1 d . . . H92A H 0.9923 -0.0684 0.4561 0.149 Uiso 1 1 calc R . . H92B H 0.9400 -0.1039 0.4163 0.149 Uiso 1 1 calc R . . Cl3 Cl 1.0049(3) -0.1663(2) 0.46583(16) 0.1480(17) Uani 1 1 d . . . Cl4 Cl 1.0747(3) -0.0914(2) 0.39116(16) 0.1454(16) Uani 1 1 d . . . C93 C 0.7767(11) -0.2688(7) 0.3130(5) 0.151(7) Uani 1 1 d . . . H93A H 0.7916 -0.3096 0.3025 0.181 Uiso 1 1 calc R . . H93B H 0.7153 -0.2664 0.3119 0.181 Uiso 1 1 calc R . . Cl5 Cl 0.8030(3) -0.26371(19) 0.36933(15) 0.1415(16) Uani 1 1 d . . . Cl6 Cl 0.8112(2) -0.22355(14) 0.27153(12) 0.0981(10) Uani 1 1 d . . . C101 C 1.2807(9) -0.2737(6) 0.4871(6) 0.130(5) Uani 1 1 d . . . H10A H 1.3262 -0.3027 0.4875 0.196 Uiso 1 1 calc R . . H10B H 1.2567 -0.2717 0.4547 0.196 Uiso 1 1 calc R . . H10C H 1.2377 -0.2861 0.5101 0.196 Uiso 1 1 calc R . . C102 C 1.3132(10) -0.2136(8) 0.5011(6) 0.132(6) Uani 1 1 d . . . H10D H 1.3375 -0.2159 0.5338 0.158 Uiso 1 1 calc R . . H10E H 1.3579 -0.2019 0.4785 0.158 Uiso 1 1 calc R . . C103 C 1.2484(11) -0.1685(9) 0.5005(6) 0.130(5) Uani 1 1 d . . . H10F H 1.2063 -0.1788 0.5252 0.156 Uiso 1 1 calc R . . H10G H 1.2206 -0.1694 0.4687 0.156 Uiso 1 1 calc R . . C104 C 1.2790(14) -0.1061(10) 0.5099(5) 0.170(8) Uani 1 1 d . . . H10H H 1.3259 -0.0975 0.4879 0.204 Uiso 1 1 calc R . . H10I H 1.3002 -0.1038 0.5433 0.204 Uiso 1 1 calc R . . C105 C 1.2111(15) -0.0582(9) 0.5028(7) 0.237(14) Uani 1 1 d . . . H10J H 1.2343 -0.0187 0.5098 0.355 Uiso 1 1 calc R . . H10K H 1.1647 -0.0661 0.5248 0.355 Uiso 1 1 calc R . . H10L H 1.1911 -0.0593 0.4695 0.355 Uiso 1 1 calc R . . C106 C 1.1172(16) 0.0619(11) 0.1771(9) 0.105(8) Uiso 0.50 1 d PD . . H10M H 1.0932 0.1019 0.1747 0.157 Uiso 0.50 1 calc PR . . H10N H 1.1769 0.0650 0.1835 0.157 Uiso 0.50 1 calc PR . . H10O H 1.0903 0.0401 0.2035 0.157 Uiso 0.50 1 calc PR . . C107 C 1.104(2) 0.0305(14) 0.1325(10) 0.127(10) Uiso 0.50 1 d PD . . H10P H 1.0447 0.0347 0.1240 0.152 Uiso 0.50 1 calc PR . . H10Q H 1.1363 0.0515 0.1073 0.152 Uiso 0.50 1 calc PR . . C108 C 1.1203(16) -0.0186(11) 0.1299(9) 0.090(7) Uiso 0.50 1 d P . . H10R H 1.0936 -0.0405 0.1567 0.108 Uiso 0.50 1 calc PR . . H10S H 1.1811 -0.0238 0.1327 0.108 Uiso 0.50 1 calc PR . . C109 C 1.096(2) -0.0393(13) 0.0903(10) 0.127(10) Uiso 0.50 1 d PD . . H10T H 1.0379 -0.0503 0.0987 0.153 Uiso 0.50 1 calc PR . . H10U H 1.1258 -0.0777 0.0897 0.153 Uiso 0.50 1 calc PR . . C110 C 1.086(2) -0.0279(14) 0.0369(9) 0.136(11) Uiso 0.50 1 d PD . . H11A H 1.0561 -0.0610 0.0221 0.204 Uiso 0.50 1 calc PR . . H11B H 1.1414 -0.0245 0.0222 0.204 Uiso 0.50 1 calc PR . . H11C H 1.0555 0.0093 0.0319 0.204 Uiso 0.50 1 calc PR . . P1 P 0.65355(11) 0.00290(7) 0.22375(7) 0.0293(4) Uani 1 1 d . . . P2 P 0.90260(14) 0.21627(11) 0.29297(9) 0.0540(7) Uani 1 1 d . . . B1 B 0.6646(6) 0.0660(4) 0.2697(3) 0.039(2) Uani 1 1 d . . . H1A H 0.6869 0.0500 0.2999 0.058 Uiso 1 1 calc R . . H1B H 0.6100 0.0839 0.2757 0.058 Uiso 1 1 calc R . . H1C H 0.7025 0.0964 0.2570 0.058 Uiso 1 1 calc R . . B2 B 0.9504(7) 0.2893(5) 0.3148(6) 0.081(4) Uani 1 1 d . . . H2A H 0.9558 0.2883 0.3499 0.121 Uiso 1 1 calc R . . H2B H 0.9146 0.3226 0.3054 0.121 Uiso 1 1 calc R . . H2C H 1.0054 0.2944 0.3002 0.121 Uiso 1 1 calc R . . O2 O 0.5870(3) 0.38436(19) 0.39220(18) 0.0367(13) Uani 1 1 d . . . O3 O 0.4337(3) 0.33932(19) 0.35494(18) 0.0322(12) Uani 1 1 d . . . O4 O 0.4550(3) 0.21986(18) 0.31722(17) 0.0277(11) Uani 1 1 d . . . O5 O 0.6522(3) 0.29224(18) 0.28993(17) 0.0304(11) Uani 1 1 d . . . O6 O 0.5562(3) 0.2598(2) 0.20439(18) 0.0389(13) Uani 1 1 d . . . H6 H 0.5831 0.2919 0.2038 0.058 Uiso 1 1 calc R . . O12 O 0.3124(3) 0.2105(2) 0.3754(2) 0.0465(15) Uani 1 1 d . . . O13 O 0.2777(3) 0.0894(2) 0.3584(2) 0.0470(15) Uani 1 1 d . . . O14 O 0.3833(3) 0.03445(19) 0.29119(17) 0.0294(11) Uani 1 1 d . . . O15 O 0.3787(3) 0.19119(19) 0.25053(18) 0.0344(12) Uani 1 1 d . . . O16 O 0.3361(3) 0.1052(2) 0.1786(2) 0.0433(13) Uani 1 1 d . . . O22 O 0.2542(3) -0.0522(2) 0.2912(2) 0.0483(15) Uani 1 1 d . . . O23 O 0.3583(3) -0.14238(19) 0.3334(2) 0.0412(14) Uani 1 1 d . . . O24 O 0.5261(3) -0.09908(18) 0.34633(16) 0.0283(11) Uani 1 1 d . . . O25 O 0.4545(3) -0.02453(18) 0.23583(16) 0.0281(12) Uani 1 1 d . . . O32 O 0.5049(3) -0.1872(2) 0.41847(19) 0.0443(15) Uani 1 1 d . . . O33 O 0.6161(4) -0.1328(2) 0.4853(2) 0.0513(16) Uani 1 1 d . . . O34 O 0.7017(3) -0.03155(19) 0.44616(17) 0.0342(12) Uani 1 1 d . . . O35 O 0.6674(3) -0.1259(2) 0.33969(18) 0.0403(13) Uani 1 1 d . . . O36 O 0.8373(4) -0.1102(3) 0.3598(3) 0.082(2) Uani 1 1 d . . . H36 H 0.8852 -0.1022 0.3496 0.122 Uiso 1 1 calc R . . O42 O 0.6584(4) -0.0030(2) 0.5423(2) 0.0567(15) Uani 1 1 d . . . O43 O 0.7154(4) 0.1141(2) 0.5437(2) 0.0522(16) Uani 1 1 d . . . O44 O 0.7971(3) 0.1525(2) 0.4604(2) 0.0455(15) Uani 1 1 d . . . O45 O 0.8387(3) -0.01141(19) 0.46424(19) 0.0407(13) Uani 1 1 d . . . O46 O 0.9826(4) 0.0600(3) 0.4668(3) 0.0709(19) Uani 1 1 d . . . O52 O 0.8620(3) 0.2554(2) 0.5062(2) 0.0498(15) Uani 1 1 d . . . O53 O 0.7706(4) 0.3370(2) 0.4476(2) 0.0514(15) Uani 1 1 d . . . O54 O 0.6797(3) 0.2783(2) 0.37265(17) 0.0340(12) Uani 1 1 d . . . O55 O 0.8639(3) 0.18188(19) 0.3908(2) 0.0399(14) Uani 1 1 d . . . C1 C 0.6613(5) 0.3188(3) 0.3366(3) 0.0334(18) Uani 1 1 d . . . H1 H 0.7082 0.3480 0.3349 0.040 Uiso 1 1 calc R . . C2 C 0.5830(4) 0.3533(3) 0.3477(3) 0.0267(17) Uani 1 1 d . . . H2 H 0.5711 0.3820 0.3210 0.032 Uiso 1 1 calc R . . C3 C 0.5114(4) 0.3085(3) 0.3523(3) 0.0298(17) Uani 1 1 d . . . H3 H 0.5193 0.2827 0.3813 0.036 Uiso 1 1 calc R . . C4 C 0.5071(4) 0.2697(3) 0.3057(3) 0.0295(18) Uani 1 1 d . . . H4 H 0.4815 0.2932 0.2789 0.035 Uiso 1 1 calc R . . C5 C 0.5907(4) 0.2457(3) 0.2898(2) 0.0257(16) Uani 1 1 d . . . H5 H 0.6084 0.2136 0.3125 0.031 Uiso 1 1 calc R . . C6 C 0.5908(4) 0.2213(3) 0.2396(2) 0.0250(16) Uani 1 1 d . . . H6A H 0.6488 0.2121 0.2303 0.030 Uiso 1 1 calc R . . H6B H 0.5594 0.1834 0.2394 0.030 Uiso 1 1 calc R . . C7 C 0.6422(5) 0.4333(3) 0.3911(3) 0.049(2) Uani 1 1 d . . . H7A H 0.6428 0.4528 0.4227 0.073 Uiso 1 1 calc R . . H7B H 0.6239 0.4618 0.3666 0.073 Uiso 1 1 calc R . . H7C H 0.6983 0.4192 0.3832 0.073 Uiso 1 1 calc R . . C8 C 0.4046(5) 0.3437(3) 0.4023(3) 0.044(2) Uani 1 1 d . . . H8A H 0.3519 0.3655 0.4026 0.067 Uiso 1 1 calc R . . H8B H 0.4455 0.3650 0.4220 0.067 Uiso 1 1 calc R . . H8C H 0.3961 0.3036 0.4155 0.067 Uiso 1 1 calc R . . C11 C 0.3769(5) 0.2192(3) 0.2961(3) 0.0377(19) Uani 1 1 d . . . H11 H 0.3570 0.2611 0.2921 0.045 Uiso 1 1 calc R . . C12 C 0.3162(4) 0.1854(3) 0.3292(3) 0.0358(19) Uani 1 1 d . . . H12 H 0.2595 0.1878 0.3146 0.043 Uiso 1 1 calc R . . C13 C 0.3404(4) 0.1201(3) 0.3322(3) 0.0304(18) Uani 1 1 d . . . H13 H 0.3942 0.1166 0.3500 0.036 Uiso 1 1 calc R . . C14 C 0.3503(4) 0.0923(3) 0.2825(3) 0.0299(17) Uani 1 1 d . . . H14 H 0.2948 0.0888 0.2667 0.036 Uiso 1 1 calc R . . C15 C 0.4069(4) 0.1300(3) 0.2520(3) 0.0275(17) Uani 1 1 d . . . H15 H 0.4633 0.1295 0.2672 0.033 Uiso 1 1 calc R . . C16 C 0.4167(4) 0.1130(3) 0.1997(3) 0.040(2) Uani 1 1 d . . . H16A H 0.4473 0.1447 0.1823 0.048 Uiso 1 1 calc R . . H16B H 0.4489 0.0756 0.1970 0.048 Uiso 1 1 calc R . . C17 C 0.2438(6) 0.2394(5) 0.3866(4) 0.087(4) Uani 1 1 d . . . H17A H 0.2483 0.2549 0.4196 0.130 Uiso 1 1 calc R . . H17B H 0.1963 0.2122 0.3845 0.130 Uiso 1 1 calc R . . H17C H 0.2359 0.2726 0.3642 0.130 Uiso 1 1 calc R . . C18 C 0.3032(7) 0.0585(4) 0.3974(4) 0.079(3) Uani 1 1 d . . . H18A H 0.2553 0.0393 0.4126 0.118 Uiso 1 1 calc R . . H18B H 0.3293 0.0859 0.4204 0.118 Uiso 1 1 calc R . . H18C H 0.3434 0.0281 0.3875 0.118 Uiso 1 1 calc R . . C19 C 0.3384(6) 0.1025(3) 0.1280(3) 0.050(2) Uani 1 1 d . . . H19A H 0.2820 0.0969 0.1155 0.075 Uiso 1 1 calc R . . H19B H 0.3734 0.0689 0.1179 0.075 Uiso 1 1 calc R . . H19C H 0.3616 0.1397 0.1152 0.075 Uiso 1 1 calc R . . C21 C 0.3741(4) -0.0095(3) 0.2547(2) 0.0208(15) Uani 1 1 d . . . H21 H 0.3375 0.0058 0.2283 0.025 Uiso 1 1 calc R . . C22 C 0.3387(4) -0.0641(3) 0.2754(3) 0.0329(18) Uani 1 1 d . . . H22 H 0.3370 -0.0954 0.2498 0.039 Uiso 1 1 calc R . . C23 C 0.3891(5) -0.0869(3) 0.3165(3) 0.0341(19) Uani 1 1 d . . . H23 H 0.3855 -0.0574 0.3434 0.041 Uiso 1 1 calc R . . C24 C 0.4802(4) -0.0942(3) 0.3029(2) 0.0286(17) Uani 1 1 d . . . H24 H 0.4867 -0.1320 0.2842 0.034 Uiso 1 1 calc R . . C25 C 0.5125(4) -0.0424(3) 0.2723(3) 0.0295(17) Uani 1 1 d . . . H25 H 0.5239 -0.0077 0.2938 0.035 Uiso 1 1 calc R . . C26 C 0.5924(4) -0.0588(3) 0.2459(3) 0.0269(17) Uani 1 1 d . . . H26A H 0.5778 -0.0846 0.2182 0.032 Uiso 1 1 calc R . . H26B H 0.6274 -0.0827 0.2679 0.032 Uiso 1 1 calc R . . C27 C 0.1946(5) -0.0925(5) 0.2701(4) 0.086(4) Uani 1 1 d . . . H27A H 0.1388 -0.0828 0.2819 0.129 Uiso 1 1 calc R . . H27B H 0.2084 -0.1335 0.2792 0.129 Uiso 1 1 calc R . . H27C H 0.1959 -0.0887 0.2349 0.129 Uiso 1 1 calc R . . C28 C 0.3237(6) -0.1405(4) 0.3790(4) 0.067(3) Uani 1 1 d . . . H28A H 0.3038 -0.1803 0.3879 0.101 Uiso 1 1 calc R . . H28B H 0.2769 -0.1125 0.3792 0.101 Uiso 1 1 calc R . . H28C H 0.3656 -0.1273 0.4023 0.101 Uiso 1 1 calc R . . C31 C 0.5848(5) -0.1443(3) 0.3515(3) 0.040(2) Uani 1 1 d . . . H31 H 0.5689 -0.1784 0.3303 0.048 Uiso 1 1 calc R . . C32 C 0.5853(5) -0.1657(3) 0.4044(3) 0.042(2) Uani 1 1 d . . . H32 H 0.6269 -0.1985 0.4080 0.051 Uiso 1 1 calc R . . C33 C 0.6103(5) -0.1134(3) 0.4370(3) 0.039(2) Uani 1 1 d . . . H33 H 0.5662 -0.0821 0.4350 0.047 Uiso 1 1 calc R . . C34 C 0.6886(5) -0.0872(3) 0.4217(3) 0.0365(19) Uani 1 1 d . . . H34 H 0.7345 -0.1150 0.4311 0.044 Uiso 1 1 calc R . . C35 C 0.6944(5) -0.0762(4) 0.3673(3) 0.050(2) Uani 1 1 d . . . H35 H 0.6582 -0.0414 0.3592 0.060 Uiso 1 1 calc R . . C36 C 0.7839(5) -0.0623(5) 0.3500(4) 0.064(3) Uani 1 1 d . . . H36A H 0.7835 -0.0543 0.3150 0.077 Uiso 1 1 calc R . . H36B H 0.8046 -0.0261 0.3666 0.077 Uiso 1 1 calc R . . C37 C 0.4997(6) -0.2499(4) 0.4123(3) 0.064(3) Uani 1 1 d . . . H37A H 0.4446 -0.2638 0.4224 0.096 Uiso 1 1 calc R . . H37B H 0.5423 -0.2694 0.4320 0.096 Uiso 1 1 calc R . . H37C H 0.5085 -0.2599 0.3783 0.096 Uiso 1 1 calc R . . C38 C 0.5470(7) -0.1251(5) 0.5144(3) 0.073(3) Uani 1 1 d . . . H38A H 0.5590 -0.1400 0.5468 0.110 Uiso 1 1 calc R . . H38B H 0.5000 -0.1473 0.5008 0.110 Uiso 1 1 calc R . . H38C H 0.5330 -0.0827 0.5161 0.110 Uiso 1 1 calc R . . C41 C 0.7637(5) -0.0291(3) 0.4814(3) 0.039(2) Uani 1 1 d . . . H41 H 0.7703 -0.0699 0.4953 0.047 Uiso 1 1 calc R . . C42 C 0.7373(6) 0.0125(4) 0.5216(3) 0.052(2) Uani 1 1 d . . . H42 H 0.7802 0.0107 0.5476 0.062 Uiso 1 1 calc R . . C43 C 0.7307(5) 0.0762(3) 0.5046(3) 0.041(2) Uani 1 1 d . . . H43 H 0.6846 0.0797 0.4807 0.049 Uiso 1 1 calc R . . C44 C 0.8121(5) 0.0941(3) 0.4812(3) 0.043(2) Uani 1 1 d . . . H44 H 0.8557 0.0977 0.5067 0.052 Uiso 1 1 calc R . . C45 C 0.8403(5) 0.0475(3) 0.4437(3) 0.045(2) Uani 1 1 d . . . H45 H 0.8009 0.0486 0.4159 0.054 Uiso 1 1 calc R . . C46 C 0.9287(5) 0.0547(4) 0.4246(3) 0.047(2) Uani 1 1 d . . . H46A H 0.9447 0.0196 0.4051 0.056 Uiso 1 1 calc R . . H46B H 0.9330 0.0907 0.4042 0.056 Uiso 1 1 calc R . . C47 C 0.6624(8) -0.0319(7) 0.5850(4) 0.118(5) Uani 1 1 d . . . H47A H 0.6061 -0.0408 0.5963 0.177 Uiso 1 1 calc R . . H47B H 0.6908 -0.0067 0.6087 0.177 Uiso 1 1 calc R . . H47C H 0.6933 -0.0692 0.5809 0.177 Uiso 1 1 calc R . . C48 C 0.6348(6) 0.1418(5) 0.5424(4) 0.091(4) Uani 1 1 d . . . H48A H 0.6276 0.1666 0.5712 0.137 Uiso 1 1 calc R . . H48B H 0.5917 0.1110 0.5417 0.137 Uiso 1 1 calc R . . H48C H 0.6303 0.1668 0.5136 0.137 Uiso 1 1 calc R . . C49 C 1.0651(7) 0.0685(6) 0.4553(5) 0.117(5) Uani 1 1 d . . . H49A H 1.0980 0.0711 0.4850 0.176 Uiso 1 1 calc R . . H49B H 1.0712 0.1055 0.4369 0.176 Uiso 1 1 calc R . . H49C H 1.0849 0.0349 0.4359 0.176 Uiso 1 1 calc R . . C51 C 0.8635(5) 0.1843(3) 0.4411(3) 0.040(2) Uani 1 1 d . . . H51 H 0.9168 0.1676 0.4538 0.048 Uiso 1 1 calc R . . C52 C 0.8558(5) 0.2496(3) 0.4560(3) 0.040(2) Uani 1 1 d . . . H52 H 0.9024 0.2724 0.4409 0.048 Uiso 1 1 calc R . . C53 C 0.7747(5) 0.2750(3) 0.4378(3) 0.046(2) Uani 1 1 d . . . H53 H 0.7277 0.2545 0.4545 0.056 Uiso 1 1 calc R . . C54 C 0.7658(4) 0.2661(3) 0.3846(3) 0.0280(17) Uani 1 1 d . . . H54 H 0.8022 0.2952 0.3674 0.034 Uiso 1 1 calc R . . C55 C 0.7865(5) 0.2040(3) 0.3680(3) 0.040(2) Uani 1 1 d . . . H55 H 0.7398 0.1769 0.3772 0.048 Uiso 1 1 calc R . . C56 C 0.8020(5) 0.1976(3) 0.3145(3) 0.041(2) Uani 1 1 d . . . H56A H 0.7611 0.2228 0.2974 0.049 Uiso 1 1 calc R . . H56B H 0.7905 0.1557 0.3055 0.049 Uiso 1 1 calc R . . C57 C 0.9245(7) 0.2931(4) 0.5221(4) 0.074(3) Uani 1 1 d . . . H57A H 0.9235 0.2950 0.5574 0.110 Uiso 1 1 calc R . . H57B H 0.9157 0.3331 0.5089 0.110 Uiso 1 1 calc R . . H57C H 0.9785 0.2779 0.5114 0.110 Uiso 1 1 calc R . . C58 C 0.72388(13) 0.35212(9) 0.48749(8) 0.070(3) Uani 1 1 d . . . H58A H 0.7241 0.3955 0.4915 0.105 Uiso 1 1 calc R . . H58B H 0.7477 0.3334 0.5162 0.105 Uiso 1 1 calc R . . H58C H 0.6667 0.3382 0.4831 0.105 Uiso 1 1 calc R . . C61 C 0.61356(13) 0.02830(9) 0.16583(8) 0.0309(18) Uani 1 1 d R . . C62 C 0.63129(13) 0.08653(9) 0.15215(8) 0.049(2) Uani 1 1 d R . . H62 H 0.6581 0.1127 0.1741 0.058 Uiso 1 1 calc R . . C63 C 0.60981(13) 0.10640(9) 0.10638(8) 0.060(3) Uani 1 1 d R . . H63 H 0.6219 0.1462 0.0970 0.072 Uiso 1 1 calc R . . C64 C 0.57060(13) 0.06806(9) 0.07428(8) 0.052(2) Uani 1 1 d R . . H64 H 0.5559 0.0816 0.0430 0.062 Uiso 1 1 calc R . . C65 C 0.55286(13) 0.00983(9) 0.08796(8) 0.043(2) Uani 1 1 d R . . H65 H 0.5261 -0.0164 0.0660 0.052 Uiso 1 1 calc R . . C66 C 0.57434(13) -0.01004(9) 0.13373(8) 0.037(2) Uani 1 1 d R . . H66 H 0.5622 -0.0498 0.1431 0.045 Uiso 1 1 calc R . . C67 C 0.75271(13) -0.03102(9) 0.20887(8) 0.0351(19) Uani 1 1 d R . . C68 C 0.75806(13) -0.08973(9) 0.19318(8) 0.053(2) Uani 1 1 d R . . H68 H 0.7091 -0.1131 0.1900 0.064 Uiso 1 1 calc R . . C69 C 0.83502(13) -0.11431(9) 0.18218(8) 0.077(3) Uani 1 1 d R . . H69 H 0.8387 -0.1544 0.1715 0.093 Uiso 1 1 calc R . . C70 C 0.90663(13) -0.08019(9) 0.18687(8) 0.074(3) Uani 1 1 d R . . H70 H 0.9592 -0.0970 0.1794 0.089 Uiso 1 1 calc R . . C71 C 0.90129(13) -0.02148(9) 0.20256(8) 0.083(3) Uani 1 1 d R . . H71 H 0.9502 0.0018 0.2058 0.100 Uiso 1 1 calc R . . C72 C 0.82432(13) 0.00311(9) 0.21356(8) 0.066(3) Uani 1 1 d R . . H72 H 0.8207 0.0432 0.2243 0.080 Uiso 1 1 calc R . . C73 C 0.89378(13) 0.22196(9) 0.22902(8) 0.068(3) Uani 1 1 d R . . C74 C 0.83162(13) 0.19113(9) 0.20478(8) 0.143(7) Uani 1 1 d R . . H74 H 0.7931 0.1675 0.2223 0.172 Uiso 1 1 calc R . . C75 C 0.82582(13) 0.19490(9) 0.15490(8) 0.111(5) Uani 1 1 d R . . H75 H 0.7833 0.1738 0.1383 0.133 Uiso 1 1 calc R . . C76 C 0.88218(13) 0.22950(9) 0.12926(8) 0.154(7) Uani 1 1 d R . . H76 H 0.8782 0.2321 0.0952 0.185 Uiso 1 1 calc R . . C77 C 0.94434(13) 0.26033(9) 0.15350(8) 0.133(6) Uani 1 1 d R . . H77 H 0.9829 0.2840 0.1360 0.159 Uiso 1 1 calc R . . C78 C 0.95014(13) 0.25656(9) 0.20338(8) 0.090(4) Uani 1 1 d R . . H78 H 0.9926 0.2776 0.2199 0.108 Uiso 1 1 calc R . . C79 C 0.96319(13) 0.15033(9) 0.30486(8) 0.065(3) Uani 1 1 d R . . C80 C 0.93397(13) 0.09247(9) 0.29904(8) 0.082(3) Uani 1 1 d R . . H80 H 0.8778 0.0858 0.2901 0.098 Uiso 1 1 calc R . . C81 C 0.98697(13) 0.04440(9) 0.30633(8) 0.101(4) Uani 1 1 d R . . H81 H 0.9670 0.0049 0.3024 0.121 Uiso 1 1 calc R . . C82 C 1.06919(13) 0.05418(9) 0.31944(8) 0.137(7) Uani 1 1 d R . . H82 H 1.1054 0.0213 0.3244 0.164 Uiso 1 1 calc R . . C83 C 1.09841(13) 0.11203(9) 0.32527(8) 0.126(6) Uani 1 1 d R . . H83 H 1.1546 0.1187 0.3342 0.151 Uiso 1 1 calc R . . C84 C 1.04541(13) 0.16011(9) 0.31798(8) 0.097(4) Uani 1 1 d R . . H84 H 1.0654 0.1996 0.3220 0.117 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C91 0.26(2) 0.084(9) 0.064(9) -0.008(7) 0.008(11) 0.015(11) Cl1 0.142(4) 0.124(3) 0.187(5) 0.006(3) -0.011(3) 0.016(3) Cl2 0.134(3) 0.134(3) 0.164(4) 0.012(3) 0.002(3) 0.039(3) C92 0.109(10) 0.172(14) 0.090(10) 0.033(10) 0.036(9) 0.054(10) Cl3 0.180(4) 0.140(3) 0.124(3) 0.029(3) 0.032(3) 0.038(3) Cl4 0.136(3) 0.166(4) 0.135(4) 0.016(3) 0.032(3) 0.001(3) C93 0.214(17) 0.154(14) 0.083(10) 0.061(10) -0.072(11) -0.049(13) Cl5 0.159(4) 0.138(3) 0.127(3) 0.031(3) -0.046(3) -0.059(3) Cl6 0.092(2) 0.094(2) 0.109(2) -0.0133(19) 0.0112(19) -0.0320(18) C101 0.112(11) 0.100(11) 0.180(15) 0.021(11) 0.025(11) -0.011(9) C102 0.109(12) 0.162(15) 0.124(12) -0.054(11) 0.036(10) -0.031(12) C103 0.131(14) 0.154(16) 0.106(12) 0.002(11) 0.034(10) 0.027(13) C104 0.24(2) 0.21(2) 0.061(10) 0.001(12) 0.041(12) 0.07(2) C105 0.37(3) 0.191(18) 0.154(16) 0.073(14) 0.107(19) 0.21(2) P1 0.0254(10) 0.0187(9) 0.0436(12) -0.0033(9) 0.0057(9) -0.0011(8) P2 0.0392(13) 0.0591(15) 0.0635(17) -0.0156(13) -0.0095(12) 0.0082(11) B1 0.034(5) 0.034(5) 0.048(6) 0.000(4) -0.017(5) -0.003(4) B2 0.052(7) 0.055(7) 0.136(12) -0.036(8) 0.010(8) -0.011(6) O2 0.046(3) 0.026(3) 0.038(3) 0.001(2) -0.005(3) -0.002(2) O3 0.035(3) 0.022(3) 0.040(3) -0.004(2) 0.010(3) -0.005(2) O4 0.021(2) 0.013(2) 0.049(3) -0.005(2) 0.004(2) 0.0036(19) O5 0.021(2) 0.026(3) 0.044(3) 0.005(2) -0.003(2) -0.003(2) O6 0.039(3) 0.030(3) 0.048(3) 0.000(3) -0.001(3) -0.006(2) O12 0.035(3) 0.038(3) 0.066(4) -0.019(3) 0.015(3) 0.000(3) O13 0.037(3) 0.031(3) 0.073(4) 0.001(3) 0.022(3) -0.003(2) O14 0.025(3) 0.021(2) 0.042(3) -0.002(2) 0.002(2) 0.005(2) O15 0.033(3) 0.027(3) 0.044(3) 0.003(2) -0.008(2) 0.003(2) O16 0.043(3) 0.046(3) 0.041(4) 0.000(3) -0.013(3) 0.000(3) O22 0.028(3) 0.040(3) 0.077(4) -0.005(3) 0.001(3) 0.008(2) O23 0.040(3) 0.020(3) 0.063(4) 0.012(2) 0.012(3) -0.008(2) O24 0.042(3) 0.018(2) 0.025(3) -0.002(2) -0.003(2) 0.003(2) O25 0.035(3) 0.017(2) 0.032(3) 0.005(2) -0.003(2) -0.001(2) O32 0.063(4) 0.017(3) 0.053(4) 0.002(2) -0.002(3) -0.020(2) O33 0.065(4) 0.043(3) 0.046(4) 0.004(3) -0.012(3) -0.003(3) O34 0.035(3) 0.026(3) 0.042(3) -0.002(2) -0.018(3) -0.002(2) O35 0.039(3) 0.033(3) 0.049(4) -0.010(3) 0.000(3) -0.004(2) O36 0.026(3) 0.102(5) 0.117(6) 0.007(5) -0.008(4) 0.001(4) O42 0.056(4) 0.055(4) 0.060(4) 0.008(3) -0.007(3) -0.009(3) O43 0.052(4) 0.052(4) 0.052(4) -0.008(3) -0.022(3) -0.005(3) O44 0.034(3) 0.026(3) 0.076(4) 0.010(3) -0.010(3) -0.008(2) O45 0.037(3) 0.022(3) 0.063(4) 0.010(2) -0.015(3) -0.005(2) O46 0.041(4) 0.084(5) 0.088(5) 0.005(4) -0.012(4) -0.006(3) O52 0.054(4) 0.047(3) 0.049(4) 0.007(3) -0.023(3) -0.011(3) O53 0.069(4) 0.028(3) 0.058(4) -0.008(3) -0.014(3) -0.005(3) O54 0.033(3) 0.029(3) 0.039(3) 0.009(2) -0.012(2) -0.005(2) O55 0.038(3) 0.021(3) 0.060(4) -0.004(2) -0.012(3) 0.000(2) C1 0.038(5) 0.027(4) 0.035(5) 0.006(3) -0.003(4) 0.000(3) C2 0.037(4) 0.022(4) 0.020(4) 0.004(3) 0.001(3) -0.007(3) C3 0.022(4) 0.026(4) 0.041(5) 0.005(3) 0.000(4) 0.001(3) C4 0.017(4) 0.016(4) 0.055(5) -0.001(3) -0.002(3) -0.006(3) C5 0.027(4) 0.019(3) 0.031(4) 0.010(3) 0.000(3) -0.010(3) C6 0.026(4) 0.023(3) 0.026(4) 0.002(3) -0.002(3) -0.006(3) C7 0.061(6) 0.026(4) 0.059(6) -0.004(4) -0.008(5) -0.010(4) C8 0.048(5) 0.026(4) 0.059(6) -0.006(4) 0.024(5) -0.006(4) C11 0.040(5) 0.020(4) 0.053(5) 0.003(4) -0.011(4) 0.011(3) C12 0.022(4) 0.039(4) 0.046(5) -0.001(4) -0.006(4) -0.008(3) C13 0.016(4) 0.023(4) 0.052(5) 0.003(3) 0.003(4) 0.003(3) C14 0.023(4) 0.022(4) 0.045(5) 0.005(3) 0.002(4) -0.006(3) C15 0.030(4) 0.019(4) 0.033(5) -0.006(3) -0.006(4) 0.009(3) C16 0.026(4) 0.024(4) 0.070(6) 0.017(4) -0.006(4) 0.002(3) C17 0.076(8) 0.085(8) 0.098(9) -0.035(7) 0.016(7) 0.038(6) C18 0.098(9) 0.055(6) 0.084(8) 0.014(6) 0.029(7) -0.009(6) C19 0.062(6) 0.027(4) 0.062(6) -0.003(4) -0.009(5) 0.003(4) C21 0.013(3) 0.025(4) 0.025(4) -0.004(3) -0.002(3) -0.002(3) C22 0.035(4) 0.024(4) 0.039(5) -0.006(3) 0.004(4) 0.003(3) C23 0.040(5) 0.017(4) 0.045(5) -0.012(3) 0.017(4) -0.004(3) C24 0.038(4) 0.020(4) 0.027(4) -0.002(3) 0.004(4) 0.000(3) C25 0.036(4) 0.014(3) 0.039(5) 0.003(3) 0.002(4) -0.016(3) C26 0.028(4) 0.016(3) 0.036(5) 0.003(3) 0.002(4) 0.004(3) C27 0.020(5) 0.102(8) 0.137(11) -0.030(8) -0.004(6) 0.002(5) C28 0.080(7) 0.054(6) 0.068(7) 0.011(5) 0.036(6) 0.004(5) C31 0.053(6) 0.028(4) 0.040(5) -0.011(4) -0.001(4) -0.002(4) C32 0.061(6) 0.019(4) 0.047(6) -0.004(4) -0.018(5) -0.001(4) C33 0.051(5) 0.030(4) 0.037(5) 0.006(4) -0.014(4) -0.004(4) C34 0.033(4) 0.032(4) 0.045(5) 0.008(4) -0.007(4) 0.003(4) C35 0.048(6) 0.051(5) 0.050(6) 0.006(4) -0.022(5) 0.005(4) C36 0.041(6) 0.094(8) 0.057(7) 0.003(6) -0.006(5) -0.004(5) C37 0.081(7) 0.050(6) 0.061(7) 0.003(5) -0.009(5) -0.027(5) C38 0.108(9) 0.074(7) 0.038(6) -0.004(5) 0.002(6) -0.036(6) C41 0.048(5) 0.022(4) 0.047(5) 0.009(4) -0.015(4) -0.002(4) C42 0.056(6) 0.049(5) 0.050(6) 0.020(5) -0.031(5) -0.023(4) C43 0.053(6) 0.032(4) 0.038(5) -0.010(4) -0.020(4) 0.000(4) C44 0.035(5) 0.029(4) 0.066(6) -0.002(4) -0.018(4) -0.006(4) C45 0.038(5) 0.048(5) 0.049(5) 0.004(4) -0.017(4) -0.006(4) C46 0.044(5) 0.033(5) 0.063(6) 0.002(4) -0.005(5) 0.006(4) C47 0.098(9) 0.220(15) 0.035(6) 0.038(8) -0.016(6) -0.074(10) C48 0.058(7) 0.113(9) 0.102(10) -0.038(7) -0.020(7) 0.003(7) C49 0.041(7) 0.136(11) 0.174(15) -0.017(10) -0.021(8) -0.007(7) C51 0.050(5) 0.023(4) 0.046(6) 0.004(4) -0.024(4) 0.007(4) C52 0.045(5) 0.035(4) 0.039(5) -0.001(4) -0.029(4) -0.006(4) C53 0.045(5) 0.035(5) 0.059(6) 0.003(4) -0.012(4) -0.003(4) C54 0.028(4) 0.021(4) 0.035(5) -0.007(3) -0.006(4) -0.004(3) C55 0.034(5) 0.028(4) 0.057(6) -0.003(4) -0.025(4) -0.006(3) C56 0.047(5) 0.023(4) 0.054(6) -0.007(4) -0.014(4) -0.001(3) C57 0.091(8) 0.069(7) 0.061(7) 0.015(5) -0.038(6) -0.037(6) C58 0.102(9) 0.055(6) 0.054(7) -0.011(5) 0.001(6) -0.004(6) C61 0.023(4) 0.029(4) 0.041(5) 0.005(4) 0.014(4) 0.003(3) C62 0.059(6) 0.029(4) 0.058(6) 0.005(4) 0.006(5) 0.003(4) C63 0.072(7) 0.049(5) 0.059(7) 0.030(5) 0.001(5) 0.007(5) C64 0.043(5) 0.069(6) 0.044(6) 0.016(5) -0.004(4) 0.022(5) C65 0.050(5) 0.037(5) 0.043(5) 0.003(4) -0.003(4) 0.006(4) C66 0.040(5) 0.020(4) 0.052(6) 0.004(4) 0.013(4) 0.001(3) C67 0.034(4) 0.053(5) 0.019(4) 0.017(4) 0.012(4) 0.001(4) C68 0.039(5) 0.033(4) 0.088(7) -0.007(5) 0.017(5) 0.011(4) C69 0.069(7) 0.053(6) 0.110(9) 0.000(6) 0.037(7) 0.014(5) C70 0.062(7) 0.055(6) 0.106(9) -0.002(6) 0.019(6) 0.017(5) C71 0.036(6) 0.106(9) 0.107(9) -0.032(7) 0.016(6) -0.014(6) C72 0.043(5) 0.053(5) 0.104(8) -0.010(6) 0.021(5) -0.008(4) C73 0.050(6) 0.071(6) 0.083(8) -0.001(6) 0.020(6) 0.020(5) C74 0.156(14) 0.238(19) 0.036(7) -0.003(9) 0.018(8) -0.087(13) C75 0.067(8) 0.116(10) 0.149(14) 0.019(9) 0.004(9) -0.040(7) C76 0.167(17) 0.24(2) 0.060(9) -0.016(11) 0.006(10) 0.085(15) C77 0.114(12) 0.158(14) 0.125(14) -0.028(12) -0.015(11) -0.026(10) C78 0.083(8) 0.096(9) 0.092(9) -0.013(7) 0.004(8) -0.011(7) C79 0.054(6) 0.049(6) 0.092(8) -0.014(5) -0.002(6) 0.016(5) C80 0.098(9) 0.077(8) 0.069(8) -0.030(6) -0.002(6) 0.029(7) C81 0.142(12) 0.042(6) 0.119(11) -0.012(6) -0.003(9) 0.031(7) C82 0.113(12) 0.181(16) 0.117(12) 0.029(11) 0.009(10) 0.110(12) C83 0.032(6) 0.115(11) 0.231(18) 0.067(11) 0.005(9) 0.013(7) C84 0.047(7) 0.071(7) 0.173(13) 0.020(8) 0.014(8) -0.003(6) _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 C91 Cl2 1.702(13) . ? C91 Cl1 1.749(15) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C92 Cl3 1.694(14) . ? C92 Cl4 1.774(13) . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? C93 Cl6 1.632(13) . ? C93 Cl5 1.624(12) . ? C93 H93A 0.9900 . ? C93 H93B 0.9900 . ? C101 C102 1.498(17) . ? C101 H10A 0.9800 . ? C101 H10B 0.9800 . ? C101 H10C 0.9800 . ? C102 C103 1.45(2) . ? C102 H10D 0.9900 . ? C102 H10E 0.9900 . ? C103 C104 1.51(2) . ? C103 H10F 0.9900 . ? C103 H10G 0.9900 . ? C104 C105 1.55(2) . ? C104 H10H 0.9900 . ? C104 H10I 0.9900 . ? C105 H10J 0.9800 . ? C105 H10K 0.9800 . ? C105 H10L 0.9800 . ? C106 C107 1.440(16) . ? C106 H10M 0.9800 . ? C106 H10N 0.9800 . ? C106 H10O 0.9800 . ? C107 C108 1.13(3) . ? C107 C109 1.96(4) . ? C107 H10P 0.9900 . ? C107 H10Q 0.9900 . ? C108 C109 1.26(3) . ? C108 H10R 0.9900 . ? C108 H10S 0.9900 . ? C109 C110 1.510(16) . ? C109 H10T 0.9900 . ? C109 H10U 0.9900 . ? C110 H11A 0.9800 . ? C110 H11B 0.9800 . ? C110 H11C 0.9800 . ? P1 C26 1.806(6) . ? P1 C67 1.816(3) . ? P1 C61 1.823(3) . ? P1 B1 1.913(9) . ? P2 C56 1.777(8) . ? P2 C73 1.785(3) . ? P2 C79 1.803(3) . ? P2 B2 1.908(11) . ? B1 H1A 0.9800 . ? B1 H1B 0.9800 . ? B1 H1C 0.9800 . ? B2 H2A 0.9800 . ? B2 H2B 0.9800 . ? B2 H2C 0.9800 . ? O2 C7 1.413(8) . ? O2 C2 1.418(8) . ? O3 C8 1.398(9) . ? O3 C3 1.430(8) . ? O4 C11 1.386(8) . ? O4 C4 1.433(7) . ? O5 C1 1.434(8) . ? O5 C5 1.439(7) . ? O6 C6 1.417(8) . ? O6 H6 0.8400 . ? O12 C17 1.317(10) . ? O12 C12 1.402(9) . ? O13 C18 1.349(11) . ? O13 C13 1.423(8) . ? O14 C21 1.422(7) . ? O14 C14 1.423(7) . ? O15 C11 1.412(9) . ? O15 C15 1.446(7) . ? O16 C19 1.405(9) . ? O16 C16 1.434(9) . ? O22 C27 1.443(10) . ? O22 C22 1.454(8) . ? O23 C28 1.384(10) . ? O23 C23 1.420(8) . ? O24 C31 1.394(8) . ? O24 C24 1.418(8) . ? O25 C25 1.434(8) . ? O25 C21 1.436(7) . ? O32 C37 1.421(9) . ? O32 C32 1.436(9) . ? O33 C38 1.385(11) . ? O33 C33 1.413(9) . ? O34 C41 1.398(9) . ? O34 C34 1.435(8) . ? O35 C31 1.430(9) . ? O35 C35 1.421(9) . ? O36 C36 1.403(11) . ? O36 H36 0.8400 . ? O42 C47 1.354(11) . ? O42 C42 1.437(10) . ? O43 C43 1.400(9) . ? O43 C48 1.439(11) . ? O44 C51 1.391(9) . ? O44 C44 1.453(9) . ? O45 C41 1.357(9) . ? O45 C45 1.440(9) . ? O46 C49 1.380(12) . ? O46 C46 1.463(10) . ? O52 C52 1.403(9) . ? O52 C57 1.387(9) . ? O53 C58 1.379(6) . ? O53 C53 1.421(9) . ? O54 C1 1.384(8) . ? O54 C54 1.450(8) . ? O55 C51 1.397(9) . ? O55 C55 1.484(8) . ? C1 C2 1.511(10) . ? C1 H1 1.0000 . ? C2 C3 1.535(9) . ? C2 H2 1.0000 . ? C3 C4 1.562(10) . ? C3 H3 1.0000 . ? C4 C5 1.515(9) . ? C4 H4 1.0000 . ? C5 C6 1.496(9) . ? C5 H5 1.0000 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C11 C12 1.541(10) . ? C11 H11 1.0000 . ? C12 C13 1.518(9) . ? C12 H12 1.0000 . ? C13 C14 1.521(10) . ? C13 H13 1.0000 . ? C14 C15 1.504(9) . ? C14 H14 1.0000 . ? C15 C16 1.511(11) . ? C15 H15 1.0000 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C21 C22 1.468(9) . ? C21 H21 1.0000 . ? C22 C23 1.489(10) . ? C22 H22 1.0000 . ? C23 C24 1.523(10) . ? C23 H23 1.0000 . ? C24 C25 1.530(9) . ? C24 H24 1.0000 . ? C25 C26 1.524(9) . ? C25 H25 1.0000 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C31 C32 1.544(11) . ? C31 H31 1.0000 . ? C32 C33 1.536(10) . ? C32 H32 1.0000 . ? C33 C34 1.454(10) . ? C33 H33 1.0000 . ? C34 C35 1.533(11) . ? C34 H34 1.0000 . ? C35 C36 1.552(12) . ? C35 H35 1.0000 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C41 C42 1.515(12) . ? C41 H41 1.0000 . ? C42 C43 1.507(10) . ? C42 H42 1.0000 . ? C43 C44 1.516(11) . ? C43 H43 1.0000 . ? C44 C45 1.541(11) . ? C44 H44 1.0000 . ? C45 C46 1.527(11) . ? C45 H45 1.0000 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C51 C52 1.528(10) . ? C51 H51 1.0000 . ? C52 C53 1.511(10) . ? C52 H52 1.0000 . ? C53 C54 1.496(10) . ? C53 H53 1.0000 . ? C54 C55 1.506(9) . ? C54 H54 1.0000 . ? C55 C56 1.510(11) . ? C55 H55 1.0000 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C61 C62 1.3900 . ? C61 C66 1.3900 . ? C62 C63 1.3900 . ? C62 H62 0.9500 . ? C63 C64 1.3900 . ? C63 H63 0.9500 . ? C64 C65 1.3900 . ? C64 H64 0.9500 . ? C65 C66 1.3900 . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C67 C68 1.3900 . ? C67 C72 1.3900 . ? C68 C69 1.3900 . ? C68 H68 0.9500 . ? C69 C70 1.3900 . ? C69 H69 0.9500 . ? C70 C71 1.3900 . ? C70 H70 0.9500 . ? C71 C72 1.3900 . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? C73 C74 1.3900 . ? C73 C78 1.3900 . ? C74 C75 1.3900 . ? C74 H74 0.9500 . ? C75 C76 1.3900 . ? C75 H75 0.9500 . ? C76 C77 1.3900 . ? C76 H76 0.9500 . ? C77 C78 1.3900 . ? C77 H77 0.9500 . ? C78 H78 0.9500 . ? C79 C80 1.3900 . ? C79 C84 1.3900 . ? C80 C81 1.3900 . ? C80 H80 0.9500 . ? C81 C82 1.3900 . ? C81 H81 0.9500 . ? C82 C83 1.3900 . ? C82 H82 0.9500 . ? C83 C84 1.3900 . ? C83 H83 0.9500 . ? C84 H84 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 C91 Cl1 112.3(7) . . ? Cl2 C91 H91A 109.1 . . ? Cl1 C91 H91A 109.1 . . ? Cl2 C91 H91B 109.2 . . ? Cl1 C91 H91B 109.2 . . ? H91A C91 H91B 107.9 . . ? Cl3 C92 Cl4 113.1(7) . . ? Cl3 C92 H92A 109.0 . . ? Cl4 C92 H92A 109.0 . . ? Cl3 C92 H92B 108.9 . . ? Cl4 C92 H92B 108.9 . . ? H92A C92 H92B 107.8 . . ? Cl6 C93 Cl5 123.1(9) . . ? Cl6 C93 H93A 106.6 . . ? Cl5 C93 H93A 106.6 . . ? Cl6 C93 H93B 106.5 . . ? Cl5 C93 H93B 106.6 . . ? H93A C93 H93B 106.5 . . ? C102 C101 H10A 109.5 . . ? C102 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C102 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? C103 C102 C101 111.9(14) . . ? C103 C102 H10D 109.2 . . ? C101 C102 H10D 109.2 . . ? C103 C102 H10E 109.2 . . ? C101 C102 H10E 109.3 . . ? H10D C102 H10E 107.9 . . ? C102 C103 C104 114.2(16) . . ? C102 C103 H10F 108.7 . . ? C104 C103 H10F 108.8 . . ? C102 C103 H10G 108.6 . . ? C104 C103 H10G 108.7 . . ? H10F C103 H10G 107.6 . . ? C103 C104 C105 113(2) . . ? C103 C104 H10H 109.0 . . ? C105 C104 H10H 109.0 . . ? C103 C104 H10I 108.9 . . ? C105 C104 H10I 108.9 . . ? H10H C104 H10I 107.7 . . ? C104 C105 H10J 109.4 . . ? C104 C105 H10K 109.5 . . ? H10J C105 H10K 109.5 . . ? C104 C105 H10L 109.4 . . ? H10J C105 H10L 109.5 . . ? H10K C105 H10L 109.5 . . ? C107 C106 H10M 109.4 . . ? C107 C106 H10N 109.6 . . ? H10M C106 H10N 109.5 . . ? C107 C106 H10O 109.5 . . ? H10M C106 H10O 109.5 . . ? H10N C106 H10O 109.5 . . ? C108 C107 C106 120(3) . . ? C108 C107 C109 37.1(17) . . ? C106 C107 C109 156(3) . . ? C108 C107 H10P 107.5 . . ? C106 C107 H10P 107.4 . . ? C109 C107 H10P 82.4 . . ? C108 C107 H10Q 107.5 . . ? C106 C107 H10Q 107.3 . . ? C109 C107 H10Q 89.8 . . ? H10P C107 H10Q 106.9 . . ? C107 C108 C109 110(3) . . ? C107 C108 H10R 109.8 . . ? C109 C108 H10R 109.8 . . ? C107 C108 H10S 109.7 . . ? C109 C108 H10S 109.5 . . ? H10R C108 H10S 108.1 . . ? C108 C109 C110 146(3) . . ? C108 C109 C107 32.9(16) . . ? C110 C109 C107 117(2) . . ? C108 C109 H10T 100.5 . . ? C110 C109 H10T 100.2 . . ? C107 C109 H10T 97.0 . . ? C108 C109 H10U 100.5 . . ? C110 C109 H10U 100.4 . . ? C107 C109 H10U 132.2 . . ? H10T C109 H10U 104.4 . . ? C109 C110 H11A 110.0 . . ? C109 C110 H11B 109.1 . . ? H11A C110 H11B 109.5 . . ? C109 C110 H11C 109.3 . . ? H11A C110 H11C 109.5 . . ? H11B C110 H11C 109.5 . . ? C26 P1 C67 103.6(2) . . ? C26 P1 C61 110.3(3) . . ? C67 P1 C61 103.94(14) . . ? C26 P1 B1 113.0(4) . . ? C67 P1 B1 112.3(3) . . ? C61 P1 B1 112.9(3) . . ? C56 P2 C73 106.2(3) . . ? C56 P2 C79 103.8(3) . . ? C73 P2 C79 106.49(16) . . ? C56 P2 B2 117.6(5) . . ? C73 P2 B2 106.6(5) . . ? C79 P2 B2 115.3(4) . . ? P1 B1 H1A 109.5 . . ? P1 B1 H1B 109.5 . . ? H1A B1 H1B 109.5 . . ? P1 B1 H1C 109.5 . . ? H1A B1 H1C 109.5 . . ? H1B B1 H1C 109.5 . . ? P2 B2 H2A 109.5 . . ? P2 B2 H2B 109.5 . . ? H2A B2 H2B 109.5 . . ? P2 B2 H2C 109.5 . . ? H2A B2 H2C 109.5 . . ? H2B B2 H2C 109.5 . . ? C7 O2 C2 113.0(6) . . ? C8 O3 C3 112.0(6) . . ? C11 O4 C4 116.4(5) . . ? C1 O5 C5 112.0(5) . . ? C6 O6 H6 109.5 . . ? C17 O12 C12 116.8(7) . . ? C18 O13 C13 116.3(7) . . ? C21 O14 C14 118.2(5) . . ? C11 O15 C15 113.7(5) . . ? C19 O16 C16 112.9(6) . . ? C27 O22 C22 112.7(6) . . ? C28 O23 C23 114.6(6) . . ? C31 O24 C24 119.8(5) . . ? C25 O25 C21 113.4(5) . . ? C37 O32 C32 110.7(6) . . ? C38 O33 C33 117.5(7) . . ? C41 O34 C34 118.0(5) . . ? C31 O35 C35 112.7(6) . . ? C36 O36 H36 109.5 . . ? C47 O42 C42 115.1(7) . . ? C43 O43 C48 113.8(6) . . ? C51 O44 C44 119.1(6) . . ? C41 O45 C45 115.0(6) . . ? C49 O46 C46 113.4(8) . . ? C52 O52 C57 115.2(7) . . ? C58 O53 C53 114.9(5) . . ? C1 O54 C54 119.6(5) . . ? C51 O55 C55 114.2(6) . . ? O54 C1 O5 113.7(5) . . ? O54 C1 C2 111.6(6) . . ? O5 C1 C2 108.2(6) . . ? O54 C1 H1 107.7 . . ? O5 C1 H1 107.7 . . ? C2 C1 H1 107.7 . . ? O2 C2 C1 113.0(6) . . ? O2 C2 C3 106.5(5) . . ? C1 C2 C3 107.9(5) . . ? O2 C2 H2 109.8 . . ? C1 C2 H2 109.8 . . ? C3 C2 H2 109.8 . . ? O3 C3 C4 105.9(5) . . ? O3 C3 C2 110.2(5) . . ? C4 C3 C2 109.3(6) . . ? O3 C3 H3 110.5 . . ? C4 C3 H3 110.5 . . ? C2 C3 H3 110.5 . . ? O4 C4 C5 108.0(5) . . ? O4 C4 C3 106.0(5) . . ? C5 C4 C3 113.6(5) . . ? O4 C4 H4 109.7 . . ? C5 C4 H4 109.7 . . ? C3 C4 H4 109.7 . . ? O5 C5 C4 110.7(5) . . ? O5 C5 C6 105.5(5) . . ? C4 C5 C6 113.7(6) . . ? O5 C5 H5 108.9 . . ? C4 C5 H5 108.9 . . ? C6 C5 H5 108.9 . . ? O6 C6 C5 114.7(5) . . ? O6 C6 H6A 108.6 . . ? C5 C6 H6A 108.6 . . ? O6 C6 H6B 108.6 . . ? C5 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O3 C8 H8A 109.5 . . ? O3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O4 C11 O15 111.4(6) . . ? O4 C11 C12 109.2(6) . . ? O15 C11 C12 109.2(6) . . ? O4 C11 H11 109.0 . . ? O15 C11 H11 109.0 . . ? C12 C11 H11 109.0 . . ? O12 C12 C13 110.5(6) . . ? O12 C12 C11 112.0(6) . . ? C13 C12 C11 110.1(6) . . ? O12 C12 H12 108.0 . . ? C13 C12 H12 108.0 . . ? C11 C12 H12 108.0 . . ? O13 C13 C12 108.2(5) . . ? O13 C13 C14 109.8(6) . . ? C12 C13 C14 112.0(6) . . ? O13 C13 H13 108.9 . . ? C12 C13 H13 108.9 . . ? C14 C13 H13 108.9 . . ? O14 C14 C15 112.5(5) . . ? O14 C14 C13 105.1(5) . . ? C15 C14 C13 110.0(5) . . ? O14 C14 H14 109.7 . . ? C15 C14 H14 109.7 . . ? C13 C14 H14 109.7 . . ? O15 C15 C14 111.1(5) . . ? O15 C15 C16 104.1(5) . . ? C14 C15 C16 117.6(6) . . ? O15 C15 H15 107.9 . . ? C14 C15 H15 107.9 . . ? C16 C15 H15 107.9 . . ? O16 C16 C15 109.2(6) . . ? O16 C16 H16A 109.8 . . ? C15 C16 H16A 109.8 . . ? O16 C16 H16B 109.8 . . ? C15 C16 H16B 109.8 . . ? H16A C16 H16B 108.3 . . ? O12 C17 H17A 109.5 . . ? O12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O13 C18 H18A 109.5 . . ? O13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O16 C19 H19A 109.5 . . ? O16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O14 C21 O25 109.1(5) . . ? O14 C21 C22 109.8(5) . . ? O25 C21 C22 107.3(5) . . ? O14 C21 H21 110.2 . . ? O25 C21 H21 110.2 . . ? C22 C21 H21 110.2 . . ? O22 C22 C21 109.2(5) . . ? O22 C22 C23 110.1(6) . . ? C21 C22 C23 112.1(6) . . ? O22 C22 H22 108.5 . . ? C21 C22 H22 108.5 . . ? C23 C22 H22 108.5 . . ? O23 C23 C22 111.4(6) . . ? O23 C23 C24 108.9(6) . . ? C22 C23 C24 111.9(6) . . ? O23 C23 H23 108.2 . . ? C22 C23 H23 108.2 . . ? C24 C23 H23 108.2 . . ? O24 C24 C23 107.4(6) . . ? O24 C24 C25 110.7(5) . . ? C23 C24 C25 112.5(6) . . ? O24 C24 H24 108.7 . . ? C23 C24 H24 108.7 . . ? C25 C24 H24 108.7 . . ? O25 C25 C26 106.2(6) . . ? O25 C25 C24 112.5(5) . . ? C26 C25 C24 111.8(5) . . ? O25 C25 H25 108.8 . . ? C26 C25 H25 108.8 . . ? C24 C25 H25 108.8 . . ? C25 C26 P1 116.0(4) . . ? C25 C26 H26A 108.3 . . ? P1 C26 H26A 108.3 . . ? C25 C26 H26B 108.3 . . ? P1 C26 H26B 108.3 . . ? H26A C26 H26B 107.4 . . ? O22 C27 H27A 109.5 . . ? O22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O22 C27 H27C 109.4 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O23 C28 H28A 109.5 . . ? O23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O24 C31 O35 113.4(6) . . ? O24 C31 C32 109.1(6) . . ? O35 C31 C32 107.6(6) . . ? O24 C31 H31 108.9 . . ? O35 C31 H31 108.9 . . ? C32 C31 H31 108.9 . . ? O32 C32 C33 109.5(7) . . ? O32 C32 C31 111.0(6) . . ? C33 C32 C31 108.9(6) . . ? O32 C32 H32 109.2 . . ? C33 C32 H32 109.1 . . ? C31 C32 H32 109.2 . . ? O33 C33 C34 110.2(6) . . ? O33 C33 C32 109.9(6) . . ? C34 C33 C32 111.4(7) . . ? O33 C33 H33 108.4 . . ? C34 C33 H33 108.4 . . ? C32 C33 H33 108.4 . . ? O34 C34 C33 109.9(6) . . ? O34 C34 C35 108.5(6) . . ? C33 C34 C35 113.8(6) . . ? O34 C34 H34 108.1 . . ? C33 C34 H34 108.1 . . ? C35 C34 H34 108.2 . . ? O35 C35 C34 112.8(6) . . ? O35 C35 C36 106.0(7) . . ? C34 C35 C36 113.1(7) . . ? O35 C35 H35 108.3 . . ? C34 C35 H35 108.2 . . ? C36 C35 H35 108.2 . . ? O36 C36 C35 110.8(8) . . ? O36 C36 H36A 109.5 . . ? C35 C36 H36A 109.5 . . ? O36 C36 H36B 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 108.1 . . ? O32 C37 H37A 109.5 . . ? O32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O33 C38 H38A 109.5 . . ? O33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O33 C38 H38C 109.4 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O45 C41 O34 113.6(6) . . ? O45 C41 C42 109.1(6) . . ? O34 C41 C42 109.8(6) . . ? O45 C41 H41 108.1 . . ? O34 C41 H41 108.1 . . ? C42 C41 H41 108.1 . . ? O42 C42 C43 107.0(7) . . ? O42 C42 C41 113.2(6) . . ? C43 C42 C41 112.0(7) . . ? O42 C42 H42 108.2 . . ? C43 C42 H42 108.2 . . ? C41 C42 H42 108.2 . . ? O43 C43 C42 110.2(7) . . ? O43 C43 C44 108.9(6) . . ? C42 C43 C44 108.9(7) . . ? O43 C43 H43 109.6 . . ? C42 C43 H43 109.6 . . ? C44 C43 H43 109.6 . . ? O44 C44 C43 105.4(6) . . ? O44 C44 C45 113.1(7) . . ? C43 C44 C45 111.4(6) . . ? O44 C44 H44 108.9 . . ? C43 C44 H44 108.9 . . ? C45 C44 H44 108.9 . . ? O45 C45 C46 104.5(6) . . ? O45 C45 C44 110.5(7) . . ? C46 C45 C44 116.0(6) . . ? O45 C45 H45 108.5 . . ? C46 C45 H45 108.5 . . ? C44 C45 H45 108.5 . . ? O46 C46 C45 106.4(7) . . ? O46 C46 H46A 110.4 . . ? C45 C46 H46A 110.5 . . ? O46 C46 H46B 110.4 . . ? C45 C46 H46B 110.4 . . ? H46A C46 H46B 108.6 . . ? O42 C47 H47A 109.5 . . ? O42 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? O42 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? O43 C48 H48A 109.5 . . ? O43 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? O43 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O46 C49 H49A 109.5 . . ? O46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? O46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? O44 C51 O55 111.6(6) . . ? O44 C51 C52 108.9(7) . . ? O55 C51 C52 107.9(6) . . ? O44 C51 H51 109.5 . . ? O55 C51 H51 109.5 . . ? C52 C51 H51 109.5 . . ? O52 C52 C53 111.0(7) . . ? O52 C52 C51 110.6(6) . . ? C53 C52 C51 109.9(6) . . ? O52 C52 H52 108.4 . . ? C53 C52 H52 108.4 . . ? C51 C52 H52 108.4 . . ? O53 C53 C54 108.4(6) . . ? O53 C53 C52 110.2(6) . . ? C54 C53 C52 111.3(7) . . ? O53 C53 H53 109.0 . . ? C54 C53 H53 108.9 . . ? C52 C53 H53 109.0 . . ? O54 C54 C55 108.4(5) . . ? O54 C54 C53 107.0(6) . . ? C55 C54 C53 113.8(6) . . ? O54 C54 H54 109.2 . . ? C55 C54 H54 109.2 . . ? C53 C54 H54 109.2 . . ? C56 C55 O55 104.4(6) . . ? C56 C55 C54 115.2(6) . . ? O55 C55 C54 111.4(5) . . ? C56 C55 H55 108.5 . . ? O55 C55 H55 108.5 . . ? C54 C55 H55 108.5 . . ? C55 C56 P2 117.3(5) . . ? C55 C56 H56A 108.0 . . ? P2 C56 H56A 108.0 . . ? C55 C56 H56B 108.0 . . ? P2 C56 H56B 108.0 . . ? H56A C56 H56B 107.2 . . ? O52 C57 H57A 109.5 . . ? O52 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? O52 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? O53 C58 H58A 109.5 . . ? O53 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? O53 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C62 C61 C66 120.0 . . ? C62 C61 P1 117.53(9) . . ? C66 C61 P1 122.13(9) . . ? C63 C62 C61 120.0 . . ? C63 C62 H62 120.0 . . ? C61 C62 H62 120.0 . . ? C62 C63 C64 120.0 . . ? C62 C63 H63 120.0 . . ? C64 C63 H63 120.0 . . ? C65 C64 C63 120.0 . . ? C65 C64 H64 120.0 . . ? C63 C64 H64 120.0 . . ? C66 C65 C64 120.0 . . ? C66 C65 H65 120.0 . . ? C64 C65 H65 120.0 . . ? C65 C66 C61 120.0 . . ? C65 C66 H66 120.0 . . ? C61 C66 H66 120.0 . . ? C68 C67 C72 120.0 . . ? C68 C67 P1 121.52(9) . . ? C72 C67 P1 118.48(9) . . ? C69 C68 C67 120.0 . . ? C69 C68 H68 120.0 . . ? C67 C68 H68 120.0 . . ? C68 C69 C70 120.0 . . ? C68 C69 H69 120.0 . . ? C70 C69 H69 120.0 . . ? C71 C70 C69 120.0 . . ? C71 C70 H70 120.0 . . ? C69 C70 H70 120.0 . . ? C72 C71 C70 120.0 . . ? C72 C71 H71 120.0 . . ? C70 C71 H71 120.0 . . ? C71 C72 C67 120.0 . . ? C71 C72 H72 120.0 . . ? C67 C72 H72 120.0 . . ? C74 C73 C78 120.0 . . ? C74 C73 P2 120.19(11) . . ? C78 C73 P2 119.80(11) . . ? C73 C74 C75 120.0 . . ? C73 C74 H74 120.0 . . ? C75 C74 H74 120.0 . . ? C76 C75 C74 120.0 . . ? C76 C75 H75 120.0 . . ? C74 C75 H75 120.0 . . ? C77 C76 C75 120.0 . . ? C77 C76 H76 120.0 . . ? C75 C76 H76 120.0 . . ? C76 C77 C78 120.0 . . ? C76 C77 H77 120.0 . . ? C78 C77 H77 120.0 . . ? C77 C78 C73 120.0 . . ? C77 C78 H78 120.0 . . ? C73 C78 H78 120.0 . . ? C80 C79 C84 120.0 . . ? C80 C79 P2 124.20(10) . . ? C84 C79 P2 115.69(10) . . ? C81 C80 C79 120.0 . . ? C81 C80 H80 120.0 . . ? C79 C80 H80 120.0 . . ? C80 C81 C82 120.0 . . ? C80 C81 H81 120.0 . . ? C82 C81 H81 120.0 . . ? C81 C82 C83 120.0 . . ? C81 C82 H82 120.0 . . ? C83 C82 H82 120.0 . . ? C84 C83 C82 120.0 . . ? C84 C83 H83 120.0 . . ? C82 C83 H83 120.0 . . ? C83 C84 C79 120.0 . . ? C83 C84 H84 120.0 . . ? C79 C84 H84 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C101 C102 C103 C104 -174.7(13) . . . . ? C102 C103 C104 C105 172.9(13) . . . . ? C106 C107 C108 C109 172(3) . . . . ? C107 C108 C109 C110 40(7) . . . . ? C106 C107 C109 C108 -16(6) . . . . ? C108 C107 C109 C110 -156(4) . . . . ? C106 C107 C109 C110 -173(6) . . . . ? C54 O54 C1 O5 92.0(7) . . . . ? C54 O54 C1 C2 -145.3(6) . . . . ? C5 O5 C1 O54 55.8(7) . . . . ? C5 O5 C1 C2 -68.8(6) . . . . ? C7 O2 C2 C1 70.4(7) . . . . ? C7 O2 C2 C3 -171.2(6) . . . . ? O54 C1 C2 O2 57.5(7) . . . . ? O5 C1 C2 O2 -176.7(5) . . . . ? O54 C1 C2 C3 -60.0(8) . . . . ? O5 C1 C2 C3 65.8(7) . . . . ? C8 O3 C3 C4 141.7(5) . . . . ? C8 O3 C3 C2 -100.2(6) . . . . ? O2 C2 C3 O3 67.8(7) . . . . ? C1 C2 C3 O3 -170.5(6) . . . . ? O2 C2 C3 C4 -176.2(5) . . . . ? C1 C2 C3 C4 -54.6(7) . . . . ? C11 O4 C4 C5 -129.4(6) . . . . ? C11 O4 C4 C3 108.5(6) . . . . ? O3 C3 C4 O4 -76.1(6) . . . . ? C2 C3 C4 O4 165.3(5) . . . . ? O3 C3 C4 C5 165.5(5) . . . . ? C2 C3 C4 C5 46.8(7) . . . . ? C1 O5 C5 C4 58.5(7) . . . . ? C1 O5 C5 C6 -178.0(5) . . . . ? O4 C4 C5 O5 -164.7(5) . . . . ? C3 C4 C5 O5 -47.5(7) . . . . ? O4 C4 C5 C6 76.7(7) . . . . ? C3 C4 C5 C6 -166.1(5) . . . . ? O5 C5 C6 O6 -71.3(7) . . . . ? C4 C5 C6 O6 50.2(7) . . . . ? C4 O4 C11 O15 88.1(6) . . . . ? C4 O4 C11 C12 -151.3(6) . . . . ? C15 O15 C11 O4 59.5(7) . . . . ? C15 O15 C11 C12 -61.1(7) . . . . ? C17 O12 C12 C13 -128.4(8) . . . . ? C17 O12 C12 C11 108.4(8) . . . . ? O4 C11 C12 O12 57.2(7) . . . . ? O15 C11 C12 O12 179.2(5) . . . . ? O4 C11 C12 C13 -66.2(8) . . . . ? O15 C11 C12 C13 55.8(7) . . . . ? C18 O13 C13 C12 -124.1(7) . . . . ? C18 O13 C13 C14 113.4(8) . . . . ? O12 C12 C13 O13 62.4(7) . . . . ? C11 C12 C13 O13 -173.3(6) . . . . ? O12 C12 C13 C14 -176.5(6) . . . . ? C11 C12 C13 C14 -52.2(8) . . . . ? C21 O14 C14 C15 -80.9(7) . . . . ? C21 O14 C14 C13 159.4(5) . . . . ? O13 C13 C14 O14 -67.2(6) . . . . ? C12 C13 C14 O14 172.5(5) . . . . ? O13 C13 C14 C15 171.5(5) . . . . ? C12 C13 C14 C15 51.2(7) . . . . ? C11 O15 C15 C14 61.2(7) . . . . ? C11 O15 C15 C16 -171.3(6) . . . . ? O14 C14 C15 O15 -170.4(5) . . . . ? C13 C14 C15 O15 -53.6(7) . . . . ? O14 C14 C15 C16 69.8(8) . . . . ? C13 C14 C15 C16 -173.4(6) . . . . ? C19 O16 C16 C15 166.7(5) . . . . ? O15 C15 C16 O16 -73.6(7) . . . . ? C14 C15 C16 O16 49.9(8) . . . . ? C14 O14 C21 O25 113.7(6) . . . . ? C14 O14 C21 C22 -129.0(6) . . . . ? C25 O25 C21 O14 54.3(6) . . . . ? C25 O25 C21 C22 -64.7(6) . . . . ? C27 O22 C22 C21 124.6(8) . . . . ? C27 O22 C22 C23 -112.0(8) . . . . ? O14 C21 C22 O22 66.5(7) . . . . ? O25 C21 C22 O22 -175.0(5) . . . . ? O14 C21 C22 C23 -55.8(7) . . . . ? O25 C21 C22 C23 62.7(7) . . . . ? C28 O23 C23 C22 -111.9(8) . . . . ? C28 O23 C23 C24 124.2(7) . . . . ? O22 C22 C23 O23 63.5(7) . . . . ? C21 C22 C23 O23 -174.8(5) . . . . ? O22 C22 C23 C24 -174.4(5) . . . . ? C21 C22 C23 C24 -52.7(7) . . . . ? C31 O24 C24 C23 132.3(6) . . . . ? C31 O24 C24 C25 -104.5(7) . . . . ? O23 C23 C24 O24 -73.0(7) . . . . ? C22 C23 C24 O24 163.5(5) . . . . ? O23 C23 C24 C25 164.9(6) . . . . ? C22 C23 C24 C25 41.4(8) . . . . ? C21 O25 C25 C26 177.9(5) . . . . ? C21 O25 C25 C24 55.4(7) . . . . ? O24 C24 C25 O25 -162.6(5) . . . . ? C23 C24 C25 O25 -42.4(8) . . . . ? O24 C24 C25 C26 78.0(7) . . . . ? C23 C24 C25 C26 -161.7(6) . . . . ? O25 C25 C26 P1 75.2(6) . . . . ? C24 C25 C26 P1 -161.8(5) . . . . ? C67 P1 C26 C25 166.2(5) . . . . ? C61 P1 C26 C25 -83.1(6) . . . . ? B1 P1 C26 C25 44.3(7) . . . . ? C24 O24 C31 O35 95.0(7) . . . . ? C24 O24 C31 C32 -145.1(6) . . . . ? C35 O35 C31 O24 57.0(8) . . . . ? C35 O35 C31 C32 -63.8(7) . . . . ? C37 O32 C32 C33 -145.4(6) . . . . ? C37 O32 C32 C31 94.4(7) . . . . ? O24 C31 C32 O32 58.9(7) . . . . ? O35 C31 C32 O32 -177.7(5) . . . . ? O24 C31 C32 C33 -61.7(8) . . . . ? O35 C31 C32 C33 61.7(8) . . . . ? C38 O33 C33 C34 142.0(7) . . . . ? C38 O33 C33 C32 -94.9(8) . . . . ? O32 C32 C33 O33 62.0(8) . . . . ? C31 C32 C33 O33 -176.5(7) . . . . ? O32 C32 C33 C34 -175.6(6) . . . . ? C31 C32 C33 C34 -54.1(9) . . . . ? C41 O34 C34 C33 109.0(7) . . . . ? C41 O34 C34 C35 -125.9(7) . . . . ? O33 C33 C34 O34 -69.7(7) . . . . ? C32 C33 C34 O34 168.1(6) . . . . ? O33 C33 C34 C35 168.4(6) . . . . ? C32 C33 C34 C35 46.2(9) . . . . ? C31 O35 C35 C34 55.8(8) . . . . ? C31 O35 C35 C36 -179.9(6) . . . . ? O34 C34 C35 O35 -169.1(6) . . . . ? C33 C34 C35 O35 -46.4(9) . . . . ? O34 C34 C35 C36 70.6(9) . . . . ? C33 C34 C35 C36 -166.7(7) . . . . ? O35 C35 C36 O36 -63.1(9) . . . . ? C34 C35 C36 O36 61.0(10) . . . . ? C45 O45 C41 O34 61.4(8) . . . . ? C45 O45 C41 C42 -61.4(8) . . . . ? C34 O34 C41 O45 92.2(7) . . . . ? C34 O34 C41 C42 -145.3(6) . . . . ? C47 O42 C42 C43 -134.6(9) . . . . ? C47 O42 C42 C41 101.6(10) . . . . ? O45 C41 C42 O42 -179.7(6) . . . . ? O34 C41 C42 O42 55.2(8) . . . . ? O45 C41 C42 C43 59.3(8) . . . . ? O34 C41 C42 C43 -65.8(8) . . . . ? C48 O43 C43 C42 -113.5(8) . . . . ? C48 O43 C43 C44 127.1(8) . . . . ? O42 C42 C43 O43 62.1(8) . . . . ? C41 C42 C43 O43 -173.4(6) . . . . ? O42 C42 C43 C44 -178.5(6) . . . . ? C41 C42 C43 C44 -54.0(8) . . . . ? C51 O44 C44 C43 172.3(6) . . . . ? C51 O44 C44 C45 -65.7(8) . . . . ? O43 C43 C44 O44 -67.0(8) . . . . ? C42 C43 C44 O44 172.7(6) . . . . ? O43 C43 C44 C45 169.9(6) . . . . ? C42 C43 C44 C45 49.7(9) . . . . ? C41 O45 C45 C46 -176.5(6) . . . . ? C41 O45 C45 C44 58.1(8) . . . . ? O44 C44 C45 O45 -169.0(6) . . . . ? C43 C44 C45 O45 -50.4(8) . . . . ? O44 C44 C45 C46 72.4(9) . . . . ? C43 C44 C45 C46 -169.1(7) . . . . ? C49 O46 C46 C45 -178.3(8) . . . . ? O45 C45 C46 O46 -71.0(7) . . . . ? C44 C45 C46 O46 50.9(9) . . . . ? C44 O44 C51 O55 103.0(7) . . . . ? C44 O44 C51 C52 -138.0(6) . . . . ? C55 O55 C51 O44 57.1(7) . . . . ? C55 O55 C51 C52 -62.6(7) . . . . ? C57 O52 C52 C53 -114.6(8) . . . . ? C57 O52 C52 C51 123.1(8) . . . . ? O44 C51 C52 O52 63.6(8) . . . . ? O55 C51 C52 O52 -175.1(6) . . . . ? O44 C51 C52 C53 -59.4(8) . . . . ? O55 C51 C52 C53 61.9(9) . . . . ? C58 O53 C53 C54 137.8(6) . . . . ? C58 O53 C53 C52 -100.1(7) . . . . ? O52 C52 C53 O53 62.6(8) . . . . ? C51 C52 C53 O53 -174.7(7) . . . . ? O52 C52 C53 C54 -177.1(6) . . . . ? C51 C52 C53 C54 -54.4(9) . . . . ? C1 O54 C54 C55 -109.8(7) . . . . ? C1 O54 C54 C53 127.1(6) . . . . ? O53 C53 C54 O54 -72.2(7) . . . . ? C52 C53 C54 O54 166.4(5) . . . . ? O53 C53 C54 C55 168.1(6) . . . . ? C52 C53 C54 C55 46.7(9) . . . . ? C51 O55 C55 C56 179.5(5) . . . . ? C51 O55 C55 C54 54.6(8) . . . . ? O54 C54 C55 C56 77.7(8) . . . . ? C53 C54 C55 C56 -163.4(6) . . . . ? O54 C54 C55 O55 -163.7(6) . . . . ? C53 C54 C55 O55 -44.7(9) . . . . ? O55 C55 C56 P2 -40.2(7) . . . . ? C54 C55 C56 P2 82.2(7) . . . . ? C73 P2 C56 C55 -166.0(5) . . . . ? C79 P2 C56 C55 81.9(5) . . . . ? B2 P2 C56 C55 -46.8(8) . . . . ? C26 P1 C61 C62 156.8(2) . . . . ? C67 P1 C61 C62 -92.66(12) . . . . ? B1 P1 C61 C62 29.3(3) . . . . ? C26 P1 C61 C66 -29.9(2) . . . . ? C67 P1 C61 C66 80.61(13) . . . . ? B1 P1 C61 C66 -157.4(3) . . . . ? C66 C61 C62 C63 0.0 . . . . ? P1 C61 C62 C63 173.41(9) . . . . ? C61 C62 C63 C64 0.0 . . . . ? C62 C63 C64 C65 0.0 . . . . ? C63 C64 C65 C66 0.0 . . . . ? C64 C65 C66 C61 0.0 . . . . ? C62 C61 C66 C65 0.0 . . . . ? P1 C61 C66 C65 -173.10(10) . . . . ? C26 P1 C67 C68 31.1(3) . . . . ? C61 P1 C67 C68 -84.18(12) . . . . ? B1 P1 C67 C68 153.5(3) . . . . ? C26 P1 C67 C72 -148.7(2) . . . . ? C61 P1 C67 C72 95.94(12) . . . . ? B1 P1 C67 C72 -26.4(3) . . . . ? C72 C67 C68 C69 0.0 . . . . ? P1 C67 C68 C69 -179.87(11) . . . . ? C67 C68 C69 C70 0.0 . . . . ? C68 C69 C70 C71 0.0 . . . . ? C69 C70 C71 C72 0.0 . . . . ? C70 C71 C72 C67 0.0 . . . . ? C68 C67 C72 C71 0.0 . . . . ? P1 C67 C72 C71 179.88(11) . . . . ? C56 P2 C73 C74 -25.2(3) . . . . ? C79 P2 C73 C74 84.94(15) . . . . ? B2 P2 C73 C74 -151.4(4) . . . . ? C56 P2 C73 C78 155.9(2) . . . . ? C79 P2 C73 C78 -94.00(15) . . . . ? B2 P2 C73 C78 29.7(4) . . . . ? C78 C73 C74 C75 0.0 . . . . ? P2 C73 C74 C75 -178.94(11) . . . . ? C73 C74 C75 C76 0.0 . . . . ? C74 C75 C76 C77 0.0 . . . . ? C75 C76 C77 C78 0.0 . . . . ? C76 C77 C78 C73 0.0 . . . . ? C74 C73 C78 C77 0.0 . . . . ? P2 C73 C78 C77 178.94(11) . . . . ? C56 P2 C79 C80 39.1(3) . . . . ? C73 P2 C79 C80 -72.75(18) . . . . ? B2 P2 C79 C80 169.2(5) . . . . ? C56 P2 C79 C84 -144.6(3) . . . . ? C73 P2 C79 C84 103.50(14) . . . . ? B2 P2 C79 C84 -14.6(5) . . . . ? C84 C79 C80 C81 0.0 . . . . ? P2 C79 C80 C81 176.09(13) . . . . ? C79 C80 C81 C82 0.0 . . . . ? C80 C81 C82 C83 0.0 . . . . ? C81 C82 C83 C84 0.0 . . . . ? C82 C83 C84 C79 0.0 . . . . ? C80 C79 C84 C83 0.0 . . . . ? P2 C79 C84 C83 -176.41(12) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.658 _refine_diff_density_min -0.608 _refine_diff_density_rms 0.103 data_mg67 _database_code_depnum_ccdc_archive 'CCDC 826891' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H116 Cl N O32' _chemical_formula_weight 1495.07 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 Monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 15.2970(10) _cell_length_b 15.7262(8) _cell_length_c 16.6710(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.778(6) _cell_angle_gamma 90.00 _cell_volume 4010.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 12114 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.1 _exptl_crystal_description Prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 0.129 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; The compound is rather poor diffracting. It crystallizes with half molecule of pentane inside the ligand, one molecule of pentane, half molecule of CH2CL2 and one water molecule outside. It must be noticed there are two disorders : O-methyl group O46-C49 and aromatic group C62.... C67. The disordered aromatic group is refined in isotropical mode due to correlations in anisotropical mode The Alerts level A are mainly due to the external pentane molecule which is difficult to refine. ; _diffrn_ambient_temperature 120(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 Saphire 3 Xcalibur' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 19.64 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29504 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.1131 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 27.00 _reflns_number_total 15107 _reflns_number_gt 7789 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,Version 1.171.26' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.26' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.26' _computing_structure_solution 'SIR-97_(Altomare& al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'MERCURY(CCDC, 2006)' _computing_publication_material 'WINGX (Farrugia, 1999)' _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^)+(0.1258P)^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 ? _chemical_absolute_configuration rm _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.22(16) _refine_ls_number_reflns 15107 _refine_ls_number_parameters 917 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1298 _refine_ls_R_factor_gt 0.0680 _refine_ls_wR_factor_ref 0.1911 _refine_ls_wR_factor_gt 0.1679 _refine_ls_goodness_of_fit_ref 0.830 _refine_ls_restrained_S_all 0.847 _refine_ls_shift/su_max 0.699 _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 N1 N 0.1643(3) 0.0950(3) 0.0969(3) 0.0436(11) Uani 1 1 d . B . O2 O 0.2995(2) -0.1522(2) 0.3796(2) 0.0476(9) Uani 1 1 d . . . O3 O 0.4376(2) -0.1225(2) 0.2751(2) 0.0433(9) Uani 1 1 d . . . O4 O 0.4189(2) 0.02654(19) 0.1807(2) 0.0382(8) Uani 1 1 d . . . O5 O 0.1901(2) -0.0373(2) 0.2147(2) 0.0422(8) Uani 1 1 d . . . O12 O 0.5996(3) -0.0022(2) 0.1965(3) 0.0614(11) Uani 1 1 d . . . O13 O 0.6593(3) 0.1596(2) 0.1489(3) 0.0618(12) Uani 1 1 d . . . O14 O 0.5186(2) 0.27018(19) 0.1095(2) 0.0378(8) Uani 1 1 d . . . O15 O 0.4376(2) 0.05926(19) 0.0459(2) 0.0403(8) Uani 1 1 d . . . O16 O 0.4439(2) 0.1711(2) -0.0885(2) 0.0499(10) Uani 1 1 d . . . H16 H 0.4928 0.1946 -0.0823 0.075 Uiso 1 1 calc R . . O22 O 0.6641(2) 0.3791(2) 0.1150(3) 0.0576(11) Uani 1 1 d . . . O23 O 0.5827(2) 0.5268(2) 0.1824(2) 0.0475(9) Uani 1 1 d . . . O24 O 0.4037(2) 0.48688(19) 0.2241(2) 0.0369(8) Uani 1 1 d . . . O25 O 0.4404(2) 0.3737(2) 0.0361(2) 0.0410(8) Uani 1 1 d . . . O26 O 0.3127(2) 0.5006(2) 0.0289(2) 0.0506(10) Uani 1 1 d . . . O32 O 0.4803(2) 0.5941(2) 0.3426(2) 0.0514(10) Uani 1 1 d . . . O33 O 0.3574(2) 0.5692(2) 0.4629(2) 0.0460(9) Uani 1 1 d . . . O34 O 0.2140(2) 0.46384(19) 0.4161(2) 0.0370(8) Uani 1 1 d . . . O35 O 0.2762(2) 0.5698(2) 0.2279(2) 0.0429(9) Uani 1 1 d . . . O36 O 0.1173(2) 0.4983(3) 0.1773(2) 0.0552(10) Uani 1 1 d . . . O42 O 0.2258(3) 0.4765(2) 0.5863(2) 0.0590(11) Uani 1 1 d . . . O43 O 0.1621(3) 0.3131(2) 0.6204(2) 0.0560(10) Uani 1 1 d . . . O44 O 0.1151(2) 0.2209(2) 0.4802(2) 0.0387(8) Uani 1 1 d . . . O45 O 0.0639(2) 0.4427(2) 0.4270(2) 0.0418(9) Uani 1 1 d . A . C46A C -0.0168(6) 0.3271(4) 0.3796(6) 0.079(3) Uani 0.618(11) 1 d P A 1 H46A H -0.0180 0.2645 0.3741 0.095 Uiso 0.618(11) 1 calc PR A 1 H46B H -0.0639 0.3432 0.4168 0.095 Uiso 0.618(11) 1 calc PR A 1 O46A O -0.0345(5) 0.3605(6) 0.3095(6) 0.093(3) Uani 0.618(11) 1 d P A 1 C49A C -0.1234(14) 0.355(2) 0.2854(13) 0.257(19) Uani 0.618(11) 1 d P A 1 H49A H -0.1315 0.3843 0.2337 0.385 Uiso 0.618(11) 1 calc PR A 1 H49B H -0.1598 0.3829 0.3258 0.385 Uiso 0.618(11) 1 calc PR A 1 H49C H -0.1404 0.2956 0.2800 0.385 Uiso 0.618(11) 1 calc PR A 1 C46B C -0.0168(6) 0.3271(4) 0.3796(6) 0.079(3) Uani 0.382(11) 1 d P A 2 H46C H -0.0229 0.3592 0.3288 0.095 Uiso 0.382(11) 1 calc PR A 2 H46D H -0.0127 0.2662 0.3651 0.095 Uiso 0.382(11) 1 calc PR A 2 O46B O -0.0822(6) 0.3361(6) 0.4150(6) 0.039(3) Uani 0.382(11) 1 d P A 2 C49B C -0.1589(9) 0.3118(9) 0.3742(10) 0.048(4) Uani 0.382(11) 1 d P A 2 H49D H -0.2093 0.3213 0.4087 0.072 Uiso 0.382(11) 1 calc PR A 2 H49E H -0.1555 0.2514 0.3601 0.072 Uiso 0.382(11) 1 calc PR A 2 H49F H -0.1656 0.3457 0.3251 0.072 Uiso 0.382(11) 1 calc PR A 2 O52 O 0.1480(3) 0.1082(2) 0.6076(2) 0.0543(10) Uani 1 1 d . . . O53 O 0.2188(3) -0.0229(2) 0.5156(2) 0.0666(12) Uani 1 1 d . . . O54 O 0.2080(2) 0.00493(19) 0.3484(2) 0.0385(8) Uani 1 1 d . . . O55 O 0.0174(2) 0.1231(2) 0.4236(2) 0.0434(9) Uani 1 1 d . . . O56 O -0.0186(3) -0.0028(2) 0.3048(2) 0.0551(10) Uani 1 1 d . . . O61 O 0.2357(2) 0.2198(2) 0.1299(3) 0.0553(10) Uani 1 1 d . . . O62 O 0.0602(3) -0.0013(3) 0.0547(3) 0.0691(12) Uani 1 1 d . B . C1 C 0.2000(3) -0.0660(3) 0.2963(3) 0.0378(12) Uani 1 1 d . . . H1 H 0.1479 -0.1007 0.3115 0.045 Uiso 1 1 calc R . . C2 C 0.2809(3) -0.1198(3) 0.3017(3) 0.0357(12) Uani 1 1 d . . . H2 H 0.2734 -0.1691 0.2643 0.043 Uiso 1 1 calc R . . C3 C 0.3615(3) -0.0702(3) 0.2767(3) 0.0396(12) Uani 1 1 d . . . H3 H 0.3718 -0.0234 0.3163 0.048 Uiso 1 1 calc R . . C4 C 0.3481(3) -0.0309(3) 0.1942(3) 0.0381(12) Uani 1 1 d . . . H4 H 0.3496 -0.0770 0.1529 0.046 Uiso 1 1 calc R . . C5 C 0.2605(3) 0.0157(3) 0.1874(3) 0.0350(11) Uani 1 1 d . . . H5 H 0.2632 0.0685 0.2208 0.042 Uiso 1 1 calc R . . C6 C 0.2369(3) 0.0388(3) 0.1035(3) 0.0414(13) Uani 1 1 d . . . H6A H 0.2881 0.0658 0.0782 0.050 Uiso 1 1 calc R . . H6B H 0.2233 -0.0139 0.0733 0.050 Uiso 1 1 calc R . . C7 C 0.2355(4) -0.2102(3) 0.4070(4) 0.0550(16) Uani 1 1 d . . . H7A H 0.2514 -0.2297 0.4610 0.083 Uiso 1 1 calc R . . H7B H 0.2323 -0.2590 0.3705 0.083 Uiso 1 1 calc R . . H7C H 0.1785 -0.1818 0.4082 0.083 Uiso 1 1 calc R . . C8 C 0.4995(4) -0.1013(4) 0.3374(4) 0.0542(15) Uani 1 1 d . . . H8A H 0.5503 -0.1390 0.3341 0.081 Uiso 1 1 calc R . . H8B H 0.4720 -0.1081 0.3898 0.081 Uiso 1 1 calc R . . H8C H 0.5183 -0.0421 0.3309 0.081 Uiso 1 1 calc R . . C11 C 0.4708(3) 0.0131(3) 0.1120(3) 0.0394(12) Uani 1 1 d . . . H11 H 0.4705 -0.0489 0.0986 0.047 Uiso 1 1 calc R . . C12 C 0.5626(4) 0.0405(3) 0.1297(4) 0.0512(15) Uani 1 1 d . . . H12 H 0.5985 0.0263 0.0818 0.061 Uiso 1 1 calc R . . C13 C 0.5696(4) 0.1355(3) 0.1437(4) 0.0483(14) Uani 1 1 d . . . H13 H 0.5413 0.1493 0.1958 0.058 Uiso 1 1 calc R . . C14 C 0.5248(3) 0.1857(3) 0.0781(3) 0.0377(12) Uani 1 1 d . . . H14 H 0.5619 0.1859 0.0291 0.045 Uiso 1 1 calc R . . C15 C 0.4336(3) 0.1511(3) 0.0569(3) 0.0371(12) Uani 1 1 d . . . H15 H 0.3937 0.1637 0.1024 0.045 Uiso 1 1 calc R . . C16 C 0.3926(3) 0.1850(3) -0.0193(3) 0.0423(13) Uani 1 1 d . . . H16A H 0.3349 0.1576 -0.0275 0.051 Uiso 1 1 calc R . . H16B H 0.3827 0.2468 -0.0132 0.051 Uiso 1 1 calc R . . C17 C 0.6492(6) -0.0754(6) 0.1767(6) 0.113(4) Uani 1 1 d . . . H17A H 0.6724 -0.1014 0.2260 0.170 Uiso 1 1 calc R . . H17B H 0.6978 -0.0589 0.1422 0.170 Uiso 1 1 calc R . . H17C H 0.6118 -0.1163 0.1483 0.170 Uiso 1 1 calc R . . C18 C 0.6802(5) 0.2004(6) 0.2216(5) 0.098(3) Uani 1 1 d . . . H18A H 0.7421 0.2164 0.2221 0.147 Uiso 1 1 calc R . . H18B H 0.6688 0.1618 0.2664 0.147 Uiso 1 1 calc R . . H18C H 0.6442 0.2516 0.2270 0.147 Uiso 1 1 calc R . . C21 C 0.5238(3) 0.3391(3) 0.0541(3) 0.0415(13) Uani 1 1 d . . . H21 H 0.5507 0.3184 0.0034 0.050 Uiso 1 1 calc R . . C22 C 0.5808(3) 0.4082(3) 0.0899(3) 0.0405(13) Uani 1 1 d . . . H22 H 0.5892 0.4531 0.0482 0.049 Uiso 1 1 calc R . . C23 C 0.5374(3) 0.4500(3) 0.1633(3) 0.0370(12) Uani 1 1 d . . . H23 H 0.5418 0.4103 0.2101 0.044 Uiso 1 1 calc R . . C24 C 0.4440(3) 0.4715(3) 0.1484(3) 0.0352(11) Uani 1 1 d . . . H24 H 0.4405 0.5244 0.1153 0.042 Uiso 1 1 calc R . . C25 C 0.3928(3) 0.4007(3) 0.1058(3) 0.0355(12) Uani 1 1 d . . . H25 H 0.3864 0.3514 0.1432 0.043 Uiso 1 1 calc R . . C26 C 0.3046(3) 0.4285(3) 0.0778(3) 0.0461(13) Uani 1 1 d . . . H26A H 0.2760 0.3821 0.0471 0.055 Uiso 1 1 calc R . . H26B H 0.2679 0.4420 0.1245 0.055 Uiso 1 1 calc R . . C27 C 0.7148(5) 0.3496(5) 0.0493(6) 0.106(3) Uani 1 1 d . . . H27A H 0.7714 0.3288 0.0694 0.160 Uiso 1 1 calc R . . H27B H 0.7241 0.3964 0.0116 0.160 Uiso 1 1 calc R . . H27C H 0.6836 0.3033 0.0219 0.160 Uiso 1 1 calc R . . C28 C 0.6482(4) 0.5190(4) 0.2454(4) 0.0659(18) Uani 1 1 d . . . H28A H 0.6761 0.5743 0.2546 0.099 Uiso 1 1 calc R . . H28B H 0.6925 0.4775 0.2294 0.099 Uiso 1 1 calc R . . H28C H 0.6205 0.4999 0.2948 0.099 Uiso 1 1 calc R . . C29 C 0.2326(4) 0.5348(4) 0.0048(4) 0.0649(18) Uani 1 1 d . . . H29A H 0.2425 0.5847 -0.0291 0.097 Uiso 1 1 calc R . . H29B H 0.1995 0.5515 0.0521 0.097 Uiso 1 1 calc R . . H29C H 0.1995 0.4921 -0.0258 0.097 Uiso 1 1 calc R . . C31 C 0.3689(3) 0.5689(3) 0.2394(3) 0.0393(12) Uani 1 1 d . . . H31 H 0.3960 0.6109 0.2021 0.047 Uiso 1 1 calc R . . C32 C 0.3888(3) 0.5952(3) 0.3259(3) 0.0402(12) Uani 1 1 d . . . H32 H 0.3663 0.6542 0.3345 0.048 Uiso 1 1 calc R . . C33 C 0.3450(3) 0.5363(3) 0.3844(3) 0.0354(11) Uani 1 1 d . . . H33 H 0.3718 0.4785 0.3809 0.042 Uiso 1 1 calc R . . C34 C 0.2478(3) 0.5307(3) 0.3650(3) 0.0339(11) Uani 1 1 d . . . H34 H 0.2196 0.5857 0.3803 0.041 Uiso 1 1 calc R . . C35 C 0.2275(3) 0.5133(3) 0.2787(3) 0.0375(12) Uani 1 1 d . . . H35 H 0.2447 0.4534 0.2664 0.045 Uiso 1 1 calc R . . C36 C 0.1338(3) 0.5249(4) 0.2565(3) 0.0481(14) Uani 1 1 d . . . H36A H 0.0971 0.4915 0.2935 0.058 Uiso 1 1 calc R . . H36B H 0.1179 0.5856 0.2620 0.058 Uiso 1 1 calc R . . C37 C 0.5219(5) 0.6716(4) 0.3303(5) 0.076(2) Uani 1 1 d . . . H37A H 0.5842 0.6661 0.3438 0.114 Uiso 1 1 calc R . . H37B H 0.4957 0.7151 0.3645 0.114 Uiso 1 1 calc R . . H37C H 0.5152 0.6883 0.2739 0.114 Uiso 1 1 calc R . . C38 C 0.4160(4) 0.5206(4) 0.5106(4) 0.0637(17) Uani 1 1 d . . . H38A H 0.4215 0.5463 0.5640 0.096 Uiso 1 1 calc R . . H38B H 0.4734 0.5193 0.4852 0.096 Uiso 1 1 calc R . . H38C H 0.3936 0.4625 0.5157 0.096 Uiso 1 1 calc R . . C39 C 0.0338(4) 0.5201(5) 0.1512(4) 0.0677(18) Uani 1 1 d . . . H39A H 0.0244 0.4994 0.0964 0.101 Uiso 1 1 calc R . . H39B H 0.0274 0.5821 0.1523 0.101 Uiso 1 1 calc R . . H39C H -0.0093 0.4943 0.1867 0.101 Uiso 1 1 calc R . . C41 C 0.1400(3) 0.4789(3) 0.4622(3) 0.0395(12) Uani 1 1 d . . . H41 H 0.1312 0.5418 0.4661 0.047 Uiso 1 1 calc R . . C42 C 0.1512(4) 0.4440(3) 0.5458(3) 0.0456(13) Uani 1 1 d . . . H42 H 0.0980 0.4574 0.5776 0.055 Uiso 1 1 calc R . . C43 C 0.1621(3) 0.3476(3) 0.5407(3) 0.0408(13) Uani 1 1 d . . . H43 H 0.2187 0.3338 0.5143 0.049 Uiso 1 1 calc R . . C44 C 0.0881(3) 0.3074(3) 0.4944(3) 0.0407(13) Uani 1 1 d . A . H44 H 0.0344 0.3074 0.5280 0.049 Uiso 1 1 calc R . . C45 C 0.0692(3) 0.3520(3) 0.4171(3) 0.0388(12) Uani 1 1 d . . . H45 H 0.1169 0.3389 0.3786 0.047 Uiso 1 1 calc R A 1 C47 C 0.2176(5) 0.5635(4) 0.6084(4) 0.084(2) Uani 1 1 d . . . H47A H 0.2714 0.5822 0.6357 0.126 Uiso 1 1 calc R . . H47B H 0.1681 0.5701 0.6446 0.126 Uiso 1 1 calc R . . H47C H 0.2077 0.5980 0.5602 0.126 Uiso 1 1 calc R . . C48 C 0.2458(5) 0.2808(5) 0.6450(5) 0.093(3) Uani 1 1 d . . . H48A H 0.2421 0.2578 0.6994 0.139 Uiso 1 1 calc R . . H48B H 0.2889 0.3269 0.6442 0.139 Uiso 1 1 calc R . . H48C H 0.2638 0.2358 0.6081 0.139 Uiso 1 1 calc R . . C51 C 0.0572(3) 0.1540(3) 0.4958(3) 0.0423(13) Uani 1 1 d . . . H51 H 0.0108 0.1743 0.5328 0.051 Uiso 1 1 calc R . . C52 C 0.1068(4) 0.0814(3) 0.5349(3) 0.0466(14) Uani 1 1 d . . . H52 H 0.0654 0.0339 0.5465 0.056 Uiso 1 1 calc R . . C53 C 0.1772(4) 0.0499(3) 0.4794(3) 0.0469(14) Uani 1 1 d . . . H53 H 0.2214 0.0958 0.4713 0.056 Uiso 1 1 calc R . . C54 C 0.1369(3) 0.0247(3) 0.3989(3) 0.0414(13) Uani 1 1 d . . . H54 H 0.1004 -0.0274 0.4061 0.050 Uiso 1 1 calc R . . C55 C 0.0803(3) 0.0949(3) 0.3647(3) 0.0416(13) Uani 1 1 d . . . H55 H 0.1189 0.1441 0.3517 0.050 Uiso 1 1 calc R . . C56 C 0.0300(4) 0.0719(3) 0.2913(3) 0.0447(13) Uani 1 1 d . . . H56A H -0.0100 0.1190 0.2764 0.054 Uiso 1 1 calc R . . H56B H 0.0706 0.0627 0.2464 0.054 Uiso 1 1 calc R . . C57 C 0.1110(7) 0.0802(9) 0.6761(4) 0.145(5) Uani 1 1 d . . . H57A H 0.1441 0.1020 0.7224 0.217 Uiso 1 1 calc R . . H57B H 0.1116 0.0179 0.6770 0.217 Uiso 1 1 calc R . . H57C H 0.0505 0.1004 0.6784 0.217 Uiso 1 1 calc R . . C58 C 0.3110(5) -0.0141(5) 0.5283(5) 0.096(3) Uani 1 1 d . . . H58A H 0.3343 -0.0661 0.5530 0.145 Uiso 1 1 calc R . . H58B H 0.3225 0.0344 0.5639 0.145 Uiso 1 1 calc R . . H58C H 0.3394 -0.0046 0.4767 0.145 Uiso 1 1 calc R . . C59 C -0.0721(4) -0.0267(5) 0.2370(4) 0.0713(19) Uani 1 1 d . . . H59A H -0.1047 -0.0785 0.2496 0.107 Uiso 1 1 calc R . . H59B H -0.0349 -0.0371 0.1906 0.107 Uiso 1 1 calc R . . H59C H -0.1132 0.0194 0.2244 0.107 Uiso 1 1 calc R . . C61 C 0.1702(4) 0.1830(3) 0.1102(3) 0.0471(14) Uani 1 1 d . B . C62 C 0.0819(4) 0.2169(4) 0.0940(5) 0.080(2) Uani 1 1 d . . . C63A C 0.0461(12) 0.2930(12) 0.1238(13) 0.085(6) Uiso 0.464(10) 1 d P B 1 H63A H 0.0812 0.3379 0.1447 0.102 Uiso 0.464(10) 1 calc PR B 1 C64A C -0.0518(13) 0.2973(13) 0.1198(13) 0.101(6) Uiso 0.464(10) 1 d P B 1 H64A H -0.0791 0.3505 0.1292 0.121 Uiso 0.464(10) 1 calc PR B 1 C65A C -0.1056(13) 0.2259(12) 0.1026(12) 0.095(6) Uiso 0.464(10) 1 d P B 1 H65A H -0.1674 0.2303 0.1066 0.114 Uiso 0.464(10) 1 calc PR B 1 C66A C -0.0661(11) 0.1467(12) 0.0791(13) 0.083(5) Uiso 0.464(10) 1 d P B 1 H66A H -0.0998 0.0974 0.0673 0.100 Uiso 0.464(10) 1 calc PR B 1 C63B C 0.0600(8) 0.3013(8) 0.0791(9) 0.061(4) Uiso 0.536(10) 1 d P B 2 H63B H 0.1001 0.3467 0.0873 0.074 Uiso 0.536(10) 1 calc PR B 2 C64B C -0.0289(8) 0.3149(8) 0.0503(8) 0.072(4) Uiso 0.536(10) 1 d P B 2 H64B H -0.0520 0.3709 0.0478 0.086 Uiso 0.536(10) 1 calc PR B 2 C65B C -0.0793(9) 0.2477(8) 0.0267(9) 0.072(4) Uiso 0.536(10) 1 d P B 2 H65B H -0.1367 0.2582 0.0065 0.086 Uiso 0.536(10) 1 calc PR B 2 C66B C -0.0502(9) 0.1659(9) 0.0310(10) 0.075(4) Uiso 0.536(10) 1 d P B 2 H66B H -0.0821 0.1214 0.0056 0.090 Uiso 0.536(10) 1 calc PR B 2 C67 C 0.0295(4) 0.1475(5) 0.0746(5) 0.082(2) Uani 1 1 d . B . C68 C 0.0810(4) 0.0719(4) 0.0738(4) 0.0536(15) Uani 1 1 d . . . O63 O 0.5807(3) 0.2701(2) -0.1395(2) 0.0561(10) Uani 1 1 d . . . H63C H 0.6407 0.2818 -0.1172 0.050 Uiso 1 1 d . . . H63D H 0.5654 0.3156 -0.1152 0.050 Uiso 1 1 d . . . C81 C 0.1170(11) 0.2233(12) -0.1283(10) 0.105(6) Uani 0.50 1 d P . . H81A H 0.1045 0.2268 -0.1867 0.126 Uiso 0.50 1 calc PR . . H81B H 0.0601 0.2244 -0.1006 0.126 Uiso 0.50 1 calc PR . . Cl1 Cl 0.16677(15) 0.12668(18) -0.10862(15) 0.0436(6) Uani 0.50 1 d P . . Cl2 Cl 0.1732(3) 0.3089(3) -0.1012(3) 0.1068(17) Uani 0.50 1 d P . . C71 C 0.5552(12) 0.2685(12) 0.4419(12) 0.110(6) Uiso 0.50 1 d P . . H71A H 0.5599 0.2985 0.4933 0.165 Uiso 0.50 1 calc PR . . H71B H 0.5722 0.3068 0.3984 0.165 Uiso 0.50 1 calc PR . . H71C H 0.5939 0.2189 0.4427 0.165 Uiso 0.50 1 calc PR . . C72 C 0.4607(16) 0.2394(18) 0.4283(17) 0.160(9) Uiso 0.50 1 d P . . H72A H 0.4426 0.2143 0.4799 0.209 Uiso 0.50 1 calc PR . . H72B H 0.4262 0.2923 0.4218 0.209 Uiso 0.50 1 calc PR . . C73 C 0.4287(11) 0.1843(11) 0.3692(11) 0.095(5) Uiso 0.50 1 d P . . H73A H 0.3902 0.1416 0.3945 0.124 Uiso 0.50 1 calc PR . . H73B H 0.4783 0.1536 0.3451 0.124 Uiso 0.50 1 calc PR . . C74 C 0.3797(8) 0.2284(9) 0.3060(9) 0.069(4) Uiso 0.50 1 d P . . H74A H 0.4160 0.2756 0.2856 0.090 Uiso 0.50 1 calc PR . . H74B H 0.3695 0.1883 0.2610 0.090 Uiso 0.50 1 calc PR . . C75 C 0.3010(7) 0.2606(7) 0.3290(7) 0.050(3) Uiso 0.50 1 d P . . H75A H 0.2724 0.2885 0.2831 0.075 Uiso 0.50 1 calc PR . . H75B H 0.3104 0.3021 0.3721 0.075 Uiso 0.50 1 calc PR . . H75C H 0.2639 0.2143 0.3482 0.075 Uiso 0.50 1 calc PR . . C76 C -0.0178(8) 0.2529(8) -0.3143(8) 0.149(4) Uiso 1 1 d . . . H76A H 0.0357 0.2190 -0.3188 0.223 Uiso 1 1 calc R . . H76B H -0.0099 0.3075 -0.3417 0.223 Uiso 1 1 calc R . . H76C H -0.0668 0.2222 -0.3392 0.223 Uiso 1 1 calc R . . C77 C -0.0376(3) 0.2692(3) -0.2231(3) 0.0435(13) Uiso 1 1 d . . . H77A H -0.0375 0.2093 -0.2048 0.057 Uiso 1 1 calc R . . H77B H 0.0208 0.2905 -0.2063 0.057 Uiso 1 1 calc R . . C78 C -0.0844(5) 0.3030(5) -0.1627(5) 0.087(2) Uiso 1 1 d . . . H78A H -0.1025 0.3606 -0.1803 0.114 Uiso 1 1 calc R . . H78B H -0.0434 0.3108 -0.1168 0.114 Uiso 1 1 calc R . . C79 C -0.1662 0.2598 -0.1292 0.070 Uiso 1 1 d D . . H79A H -0.1351 0.2252 -0.0883 0.091 Uiso 1 1 calc R . . H79B H -0.1869 0.3096 -0.0984 0.091 Uiso 1 1 calc R . . C80 C -0.2370(5) 0.2191(5) -0.1270(5) 0.080(2) Uiso 1 1 d D . . H80A H -0.2568 0.2157 -0.0715 0.120 Uiso 1 1 calc R . . H80B H -0.2279 0.1616 -0.1480 0.120 Uiso 1 1 calc R . . H80C H -0.2813 0.2484 -0.1599 0.120 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.045(3) 0.044(3) 0.042(3) -0.001(2) -0.003(2) -0.012(2) O2 0.067(2) 0.0359(19) 0.039(2) 0.0099(17) 0.0063(18) -0.0052(18) O3 0.051(2) 0.0336(18) 0.045(2) 0.0023(16) -0.0008(18) 0.0059(16) O4 0.050(2) 0.0287(17) 0.037(2) -0.0016(15) 0.0163(16) -0.0001(16) O5 0.056(2) 0.0348(18) 0.036(2) -0.0050(16) 0.0049(17) -0.0029(17) O12 0.063(3) 0.049(2) 0.072(3) 0.025(2) 0.010(2) 0.010(2) O13 0.047(2) 0.047(2) 0.091(4) 0.011(2) -0.007(2) 0.0006(18) O14 0.050(2) 0.0280(18) 0.035(2) 0.0016(15) 0.0094(16) 0.0036(15) O15 0.059(2) 0.0290(17) 0.033(2) -0.0017(15) 0.0078(16) 0.0018(16) O16 0.063(2) 0.047(2) 0.040(2) 0.0029(17) 0.0113(19) -0.0147(18) O22 0.049(2) 0.051(2) 0.073(3) -0.005(2) 0.014(2) 0.0025(19) O23 0.045(2) 0.043(2) 0.054(3) 0.0036(18) -0.0008(18) -0.0065(17) O24 0.0423(19) 0.0282(18) 0.040(2) -0.0020(15) 0.0054(16) 0.0004(15) O25 0.050(2) 0.0367(19) 0.036(2) 0.0020(15) 0.0014(16) 0.0001(16) O26 0.047(2) 0.052(2) 0.053(3) 0.0102(19) 0.0015(18) 0.0119(18) O32 0.046(2) 0.045(2) 0.063(3) -0.0099(19) 0.0017(19) -0.0102(18) O33 0.052(2) 0.049(2) 0.037(2) -0.0074(18) -0.0065(17) -0.0061(18) O34 0.0419(19) 0.0303(18) 0.039(2) -0.0040(15) 0.0074(16) -0.0007(15) O35 0.040(2) 0.045(2) 0.044(2) 0.0076(17) 0.0047(16) 0.0067(16) O36 0.036(2) 0.090(3) 0.040(2) -0.002(2) -0.0043(17) 0.008(2) O42 0.081(3) 0.051(2) 0.044(2) -0.0099(19) -0.008(2) -0.028(2) O43 0.079(3) 0.052(2) 0.037(2) -0.0015(18) 0.004(2) -0.013(2) O44 0.0390(19) 0.0323(18) 0.045(2) -0.0062(16) 0.0089(16) -0.0075(15) O45 0.039(2) 0.0335(18) 0.053(2) -0.0050(16) 0.0042(17) 0.0054(15) C46A 0.084(6) 0.047(4) 0.104(7) 0.010(4) -0.052(6) -0.008(4) O46A 0.067(5) 0.122(7) 0.089(7) 0.005(6) -0.021(5) -0.039(5) C49A 0.154(19) 0.47(5) 0.14(2) 0.13(2) -0.098(16) -0.16(3) C46B 0.084(6) 0.047(4) 0.104(7) 0.010(4) -0.052(6) -0.008(4) O46B 0.017(5) 0.062(6) 0.039(6) -0.008(5) -0.003(4) 0.002(4) C49B 0.037(8) 0.051(9) 0.056(11) -0.008(7) -0.004(7) -0.015(7) O52 0.079(3) 0.050(2) 0.035(2) -0.0014(17) 0.006(2) -0.020(2) O53 0.112(4) 0.043(2) 0.045(3) 0.0089(19) 0.006(2) 0.017(2) O54 0.047(2) 0.0278(17) 0.041(2) -0.0023(15) 0.0140(16) -0.0048(15) O55 0.041(2) 0.0393(19) 0.050(2) -0.0119(17) 0.0124(17) -0.0105(16) O56 0.069(3) 0.056(2) 0.041(2) -0.0072(19) 0.0077(19) -0.024(2) O61 0.045(2) 0.046(2) 0.075(3) -0.005(2) -0.004(2) -0.0074(19) O62 0.071(3) 0.062(3) 0.074(3) -0.013(2) -0.006(2) -0.016(2) C1 0.053(3) 0.028(2) 0.033(3) -0.005(2) 0.009(2) -0.012(2) C2 0.052(3) 0.023(2) 0.032(3) 0.001(2) 0.006(2) 0.000(2) C3 0.054(3) 0.032(3) 0.033(3) -0.001(2) 0.008(2) 0.001(2) C4 0.052(3) 0.028(3) 0.035(3) -0.005(2) 0.005(2) -0.003(2) C5 0.047(3) 0.029(2) 0.029(3) 0.000(2) 0.006(2) -0.008(2) C6 0.052(3) 0.034(3) 0.038(3) -0.001(2) 0.004(2) 0.007(2) C7 0.074(4) 0.039(3) 0.053(4) 0.013(3) 0.017(3) -0.005(3) C8 0.058(4) 0.041(3) 0.064(4) 0.010(3) -0.002(3) 0.000(3) C11 0.053(3) 0.027(3) 0.039(3) 0.002(2) 0.016(2) 0.005(2) C12 0.060(4) 0.040(3) 0.054(4) 0.014(3) 0.021(3) 0.008(3) C13 0.054(4) 0.036(3) 0.056(4) 0.013(3) 0.005(3) 0.008(3) C14 0.040(3) 0.031(3) 0.042(3) 0.001(2) 0.008(2) 0.000(2) C15 0.051(3) 0.024(2) 0.036(3) 0.001(2) 0.013(2) 0.006(2) C16 0.043(3) 0.032(3) 0.051(4) 0.002(2) 0.009(3) -0.003(2) C17 0.104(6) 0.118(7) 0.119(7) 0.063(6) 0.051(5) 0.074(6) C18 0.094(6) 0.126(7) 0.073(6) 0.044(5) -0.034(5) -0.039(5) C21 0.042(3) 0.038(3) 0.045(3) 0.014(2) 0.015(2) 0.006(2) C22 0.031(3) 0.038(3) 0.052(4) -0.003(2) 0.007(2) 0.003(2) C23 0.044(3) 0.025(3) 0.041(3) 0.003(2) -0.002(2) -0.003(2) C24 0.044(3) 0.028(2) 0.033(3) 0.001(2) 0.005(2) 0.004(2) C25 0.036(3) 0.032(2) 0.039(3) 0.001(2) 0.006(2) 0.001(2) C26 0.046(3) 0.046(3) 0.046(4) -0.002(3) 0.005(3) 0.001(3) C27 0.051(4) 0.086(5) 0.183(10) -0.002(6) 0.051(5) 0.000(4) C28 0.046(3) 0.056(4) 0.095(5) -0.017(4) -0.017(3) 0.001(3) C29 0.053(4) 0.084(4) 0.058(4) 0.011(4) 0.004(3) 0.020(3) C31 0.036(3) 0.032(3) 0.051(4) 0.008(2) 0.010(2) 0.003(2) C32 0.040(3) 0.032(3) 0.049(3) -0.004(2) -0.002(2) 0.003(2) C33 0.034(3) 0.030(2) 0.042(3) -0.003(2) 0.006(2) 0.004(2) C34 0.042(3) 0.022(2) 0.037(3) -0.003(2) 0.004(2) 0.005(2) C35 0.035(3) 0.039(3) 0.039(3) 0.004(2) 0.002(2) 0.001(2) C36 0.038(3) 0.064(4) 0.042(4) -0.006(3) -0.002(3) 0.008(3) C37 0.076(5) 0.041(4) 0.110(6) 0.002(4) -0.017(4) -0.023(3) C38 0.055(4) 0.079(4) 0.057(4) -0.002(3) -0.018(3) 0.009(3) C39 0.057(4) 0.089(5) 0.057(4) 0.008(4) -0.012(3) 0.007(4) C41 0.042(3) 0.029(3) 0.048(3) -0.013(2) 0.011(3) -0.002(2) C42 0.055(3) 0.044(3) 0.038(3) -0.011(3) 0.007(3) -0.013(3) C43 0.037(3) 0.044(3) 0.041(3) -0.003(3) -0.001(2) 0.002(2) C44 0.041(3) 0.032(3) 0.049(4) -0.014(2) 0.007(3) -0.003(2) C45 0.036(3) 0.034(3) 0.046(3) -0.007(2) -0.006(2) 0.001(2) C47 0.108(6) 0.066(4) 0.079(5) -0.044(4) 0.024(4) -0.035(4) C48 0.082(5) 0.112(6) 0.083(6) 0.040(5) -0.043(4) -0.051(5) C51 0.039(3) 0.039(3) 0.049(4) -0.006(3) 0.015(3) -0.016(2) C52 0.056(3) 0.046(3) 0.039(3) -0.003(3) 0.010(3) -0.018(3) C53 0.070(4) 0.035(3) 0.036(3) -0.004(2) 0.003(3) -0.008(3) C54 0.050(3) 0.032(3) 0.043(3) 0.005(2) 0.018(3) -0.005(2) C55 0.045(3) 0.038(3) 0.042(3) 0.003(2) 0.020(3) -0.010(2) C56 0.054(3) 0.045(3) 0.035(3) 0.002(3) 0.007(3) -0.001(3) C57 0.147(8) 0.257(14) 0.029(4) -0.004(6) 0.013(5) -0.104(9) C58 0.108(6) 0.083(5) 0.097(6) -0.023(5) -0.056(5) 0.039(5) C59 0.074(4) 0.083(5) 0.057(4) -0.017(4) -0.001(4) -0.007(4) C61 0.051(4) 0.045(3) 0.046(4) -0.001(3) -0.001(3) 0.000(3) C62 0.048(4) 0.058(4) 0.132(7) -0.031(4) -0.034(4) 0.017(3) C67 0.039(4) 0.072(4) 0.135(7) -0.026(5) -0.036(4) -0.001(3) C68 0.058(4) 0.054(4) 0.048(4) 0.001(3) 0.005(3) -0.007(3) O63 0.066(3) 0.050(2) 0.053(3) -0.0001(19) 0.005(2) -0.0080(19) C81 0.091(11) 0.153(16) 0.071(12) -0.035(11) -0.018(9) -0.050(12) Cl1 0.0296(12) 0.0777(18) 0.0233(13) -0.0008(12) -0.0073(10) -0.0107(13) Cl2 0.102(3) 0.085(3) 0.131(4) 0.022(2) -0.080(3) -0.042(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 N1 C68 1.374(7) . ? N1 C61 1.405(7) . ? N1 C6 1.423(6) . ? O2 C2 1.420(6) . ? O2 C7 1.418(6) . ? O3 C3 1.426(6) . ? O3 C8 1.435(7) . ? O4 C11 1.418(6) . ? O4 C4 1.431(6) . ? O5 C1 1.440(6) . ? O5 C5 1.441(6) . ? O12 C12 1.412(7) . ? O12 C17 1.419(8) . ? O13 C13 1.425(7) . ? O13 C18 1.404(9) . ? O14 C21 1.427(6) . ? O14 C14 1.432(6) . ? O15 C11 1.408(6) . ? O15 C15 1.457(5) . ? O16 C16 1.420(6) . ? O16 H16 0.8400 . ? O22 C22 1.412(6) . ? O22 C27 1.428(9) . ? O23 C23 1.427(6) . ? O23 C28 1.447(7) . ? O24 C31 1.419(6) . ? O24 C24 1.432(6) . ? O25 C21 1.415(6) . ? O25 C25 1.443(6) . ? O26 C29 1.392(6) . ? O26 C26 1.402(6) . ? O32 C37 1.392(7) . ? O32 C32 1.425(6) . ? O33 C38 1.415(6) . ? O33 C33 1.417(6) . ? O34 C41 1.398(6) . ? O34 C34 1.452(6) . ? O35 C31 1.429(6) . ? O35 C35 1.442(6) . ? O36 C36 1.405(6) . ? O36 C39 1.386(6) . ? O42 C42 1.413(6) . ? O42 C47 1.423(7) . ? O43 C43 1.435(6) . ? O43 C48 1.432(8) . ? O44 C51 1.401(6) . ? O44 C44 1.442(6) . ? O45 C45 1.438(6) . ? O45 C41 1.415(6) . ? C46A O46A 1.307(11) . ? C46A C45 1.500(8) . ? C46A H46A 0.9900 . ? C46A H46B 0.9900 . ? O46A C49A 1.415(18) . ? C49A H49A 0.9800 . ? C49A H49B 0.9800 . ? C49A H49C 0.9800 . ? O46B C49B 1.403(16) . ? C49B H49D 0.9800 . ? C49B H49E 0.9800 . ? C49B H49F 0.9800 . ? O52 C57 1.354(8) . ? O52 C52 1.422(6) . ? O53 C58 1.430(8) . ? O53 C53 1.440(6) . ? O54 C54 1.418(6) . ? O54 C1 1.418(6) . ? O55 C51 1.426(6) . ? O55 C55 1.453(6) . ? O56 C56 1.411(6) . ? O56 C59 1.436(7) . ? O61 C61 1.200(6) . ? O62 C68 1.235(7) . ? C1 C2 1.501(7) . ? C1 H1 1.0000 . ? C2 C3 1.524(7) . ? C2 H2 1.0000 . ? C3 C4 1.519(7) . ? C3 H3 1.0000 . ? C4 C5 1.530(7) . ? C4 H4 1.0000 . ? C5 C6 1.484(7) . ? C5 H5 1.0000 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C11 C12 1.495(8) . ? C11 H11 1.0000 . ? C12 C13 1.515(8) . ? C12 H12 1.0000 . ? C13 C14 1.506(7) . ? C13 H13 1.0000 . ? C14 C15 1.534(7) . ? C14 H14 1.0000 . ? C15 C16 1.507(7) . ? C15 H15 1.0000 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C21 C22 1.512(7) . ? C21 H21 1.0000 . ? C22 C23 1.547(7) . ? C22 H22 1.0000 . ? C23 C24 1.486(7) . ? C23 H23 1.0000 . ? C24 C25 1.530(7) . ? C24 H24 1.0000 . ? C25 C26 1.487(7) . ? C25 H25 1.0000 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C31 C32 1.527(7) . ? C31 H31 1.0000 . ? C32 C33 1.507(7) . ? C32 H32 1.0000 . ? C33 C34 1.521(6) . ? C33 H33 1.0000 . ? C34 C35 1.493(7) . ? C34 H34 1.0000 . ? C35 C36 1.487(7) . ? C35 H35 1.0000 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C41 C42 1.506(8) . ? C41 H41 1.0000 . ? C42 C43 1.528(7) . ? C42 H42 1.0000 . ? C43 C44 1.501(7) . ? C43 H43 1.0000 . ? C44 C45 1.494(8) . ? C44 H44 1.0000 . ? C45 H45 1.0000 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C51 C52 1.513(8) . ? C51 H51 1.0000 . ? C52 C53 1.512(8) . ? C52 H52 1.0000 . ? C53 C54 1.522(7) . ? C53 H53 1.0000 . ? C54 C55 1.510(7) . ? C54 H54 1.0000 . ? C55 C56 1.482(7) . ? C55 H55 1.0000 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C61 C62 1.473(8) . ? C62 C67 1.389(9) . ? C62 C63A 1.41(2) . ? C62 C63B 1.391(14) . ? C63A C64A 1.50(2) . ? C63A H63A 0.9500 . ? C64A C65A 1.42(2) . ? C64A H64A 0.9500 . ? C65A C66A 1.44(2) . ? C65A H65A 0.9500 . ? C66A C67 1.466(18) . ? C66A H66A 0.9500 . ? C63B C64B 1.451(17) . ? C63B H63B 0.9500 . ? C64B C65B 1.364(17) . ? C64B H64B 0.9500 . ? C65B C66B 1.363(18) . ? C65B H65B 0.9500 . ? C66B C67 1.440(15) . ? C66B H66B 0.9500 . ? C67 C68 1.425(9) . ? O63 H63C 1.0025 . ? O63 H63D 0.8571 . ? C81 Cl2 1.658(15) . ? C81 Cl1 1.73(2) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C71 C72 1.53(3) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 C73 1.40(3) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.46(2) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.365(16) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 C77 1.576(13) . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 C78 1.352(9) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 C79 1.535(8) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 C80 1.258(7) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C68 N1 C61 111.2(5) . . ? C68 N1 C6 125.3(5) . . ? C61 N1 C6 123.5(4) . . ? C2 O2 C7 113.2(4) . . ? C3 O3 C8 112.5(4) . . ? C11 O4 C4 117.7(4) . . ? C1 O5 C5 114.3(4) . . ? C12 O12 C17 114.4(5) . . ? C13 O13 C18 112.4(5) . . ? C21 O14 C14 117.7(4) . . ? C11 O15 C15 115.4(4) . . ? C16 O16 H16 109.5 . . ? C22 O22 C27 112.0(5) . . ? C23 O23 C28 114.8(4) . . ? C31 O24 C24 118.6(4) . . ? C21 O25 C25 114.0(4) . . ? C29 O26 C26 113.3(4) . . ? C37 O32 C32 114.3(4) . . ? C38 O33 C33 113.4(4) . . ? C41 O34 C34 119.7(4) . . ? C31 O35 C35 115.8(3) . . ? C36 O36 C39 111.9(4) . . ? C42 O42 C47 113.5(5) . . ? C43 O43 C48 112.8(5) . . ? C51 O44 C44 119.6(4) . . ? C45 O45 C41 113.5(4) . . ? O46A C46A C45 115.9(8) . . ? O46A C46A H46A 108.3 . . ? C45 C46A H46A 108.3 . . ? O46A C46A H46B 108.3 . . ? C45 C46A H46B 108.3 . . ? H46A C46A H46B 107.4 . . ? C46A O46A C49A 114.7(11) . . ? O46A C49A H49A 109.5 . . ? O46A C49A H49B 109.5 . . ? H49A C49A H49B 109.5 . . ? O46A C49A H49C 109.5 . . ? H49A C49A H49C 109.5 . . ? H49B C49A H49C 109.5 . . ? O46B C49B H49D 109.5 . . ? O46B C49B H49E 109.5 . . ? H49D C49B H49E 109.5 . . ? O46B C49B H49F 109.5 . . ? H49D C49B H49F 109.5 . . ? H49E C49B H49F 109.5 . . ? C57 O52 C52 115.9(5) . . ? C58 O53 C53 114.5(5) . . ? C54 O54 C1 118.3(4) . . ? C51 O55 C55 113.2(4) . . ? C56 O56 C59 112.8(5) . . ? O5 C1 O54 109.7(4) . . ? O5 C1 C2 108.0(4) . . ? O54 C1 C2 110.0(4) . . ? O5 C1 H1 109.7 . . ? O54 C1 H1 109.7 . . ? C2 C1 H1 109.7 . . ? O2 C2 C1 114.4(4) . . ? O2 C2 C3 106.3(4) . . ? C1 C2 C3 111.4(4) . . ? O2 C2 H2 108.2 . . ? C1 C2 H2 108.2 . . ? C3 C2 H2 108.2 . . ? O3 C3 C2 111.9(4) . . ? O3 C3 C4 108.6(4) . . ? C2 C3 C4 110.9(4) . . ? O3 C3 H3 108.5 . . ? C2 C3 H3 108.5 . . ? C4 C3 H3 108.5 . . ? O4 C4 C3 107.7(4) . . ? O4 C4 C5 110.5(4) . . ? C3 C4 C5 111.7(4) . . ? O4 C4 H4 109.0 . . ? C3 C4 H4 109.0 . . ? C5 C4 H4 109.0 . . ? O5 C5 C6 105.4(4) . . ? O5 C5 C4 110.9(4) . . ? C6 C5 C4 112.8(4) . . ? O5 C5 H5 109.2 . . ? C6 C5 H5 109.2 . . ? C4 C5 H5 109.2 . . ? N1 C6 C5 113.9(4) . . ? N1 C6 H6A 108.8 . . ? C5 C6 H6A 108.8 . . ? N1 C6 H6B 108.8 . . ? C5 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O3 C8 H8A 109.5 . . ? O3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O15 C11 O4 110.8(4) . . ? O15 C11 C12 109.4(4) . . ? O4 C11 C12 109.4(4) . . ? O15 C11 H11 109.1 . . ? O4 C11 H11 109.1 . . ? C12 C11 H11 109.1 . . ? O12 C12 C11 112.5(4) . . ? O12 C12 C13 108.7(5) . . ? C11 C12 C13 112.3(4) . . ? O12 C12 H12 107.7 . . ? C11 C12 H12 107.7 . . ? C13 C12 H12 107.7 . . ? O13 C13 C12 109.8(4) . . ? O13 C13 C14 109.5(4) . . ? C12 C13 C14 112.0(5) . . ? O13 C13 H13 108.5 . . ? C12 C13 H13 108.5 . . ? C14 C13 H13 108.5 . . ? O14 C14 C13 104.7(4) . . ? O14 C14 C15 110.4(4) . . ? C13 C14 C15 112.6(4) . . ? O14 C14 H14 109.7 . . ? C13 C14 H14 109.7 . . ? C15 C14 H14 109.7 . . ? O15 C15 C16 105.2(4) . . ? O15 C15 C14 109.9(4) . . ? C16 C15 C14 115.8(4) . . ? O15 C15 H15 108.5 . . ? C16 C15 H15 108.5 . . ? C14 C15 H15 108.5 . . ? O16 C16 C15 113.7(4) . . ? O16 C16 H16A 108.8 . . ? C15 C16 H16A 108.8 . . ? O16 C16 H16B 108.8 . . ? C15 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? O12 C17 H17A 109.5 . . ? O12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O13 C18 H18A 109.5 . . ? O13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O25 C21 O14 111.8(4) . . ? O25 C21 C22 108.7(4) . . ? O14 C21 C22 109.1(4) . . ? O25 C21 H21 109.1 . . ? O14 C21 H21 109.1 . . ? C22 C21 H21 109.1 . . ? O22 C22 C21 113.4(4) . . ? O22 C22 C23 107.4(4) . . ? C21 C22 C23 111.5(4) . . ? O22 C22 H22 108.1 . . ? C21 C22 H22 108.1 . . ? C23 C22 H22 108.2 . . ? O23 C23 C24 108.0(4) . . ? O23 C23 C22 108.8(4) . . ? C24 C23 C22 112.8(4) . . ? O23 C23 H23 109.1 . . ? C24 C23 H23 109.1 . . ? C22 C23 H23 109.1 . . ? O24 C24 C23 108.4(4) . . ? O24 C24 C25 108.0(4) . . ? C23 C24 C25 113.4(4) . . ? O24 C24 H24 109.0 . . ? C23 C24 H24 109.0 . . ? C25 C24 H24 109.0 . . ? O25 C25 C26 107.4(4) . . ? O25 C25 C24 109.1(4) . . ? C26 C25 C24 112.8(4) . . ? O25 C25 H25 109.1 . . ? C26 C25 H25 109.1 . . ? C24 C25 H25 109.1 . . ? O26 C26 C25 109.5(4) . . ? O26 C26 H26A 109.8 . . ? C25 C26 H26A 109.8 . . ? O26 C26 H26B 109.8 . . ? C25 C26 H26B 109.8 . . ? H26A C26 H26B 108.2 . . ? O22 C27 H27A 109.5 . . ? O22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O23 C28 H28A 109.5 . . ? O23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O26 C29 H29A 109.5 . . ? O26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O35 C31 O24 111.0(4) . . ? O35 C31 C32 107.9(4) . . ? O24 C31 C32 110.2(4) . . ? O35 C31 H31 109.2 . . ? O24 C31 H31 109.2 . . ? C32 C31 H31 109.2 . . ? O32 C32 C31 111.3(4) . . ? O32 C32 C33 108.1(4) . . ? C31 C32 C33 111.1(4) . . ? O32 C32 H32 108.8 . . ? C31 C32 H32 108.8 . . ? C33 C32 H32 108.7 . . ? O33 C33 C32 108.5(4) . . ? O33 C33 C34 109.6(4) . . ? C32 C33 C34 109.9(4) . . ? O33 C33 H33 109.6 . . ? C32 C33 H33 109.6 . . ? C34 C33 H33 109.6 . . ? O34 C34 C35 111.1(4) . . ? O34 C34 C33 105.8(4) . . ? C35 C34 C33 113.9(4) . . ? O34 C34 H34 108.6 . . ? C35 C34 H34 108.6 . . ? C33 C34 H34 108.6 . . ? O35 C35 C36 106.4(4) . . ? O35 C35 C34 110.6(4) . . ? C36 C35 C34 113.9(4) . . ? O35 C35 H35 108.6 . . ? C36 C35 H35 108.6 . . ? C34 C35 H35 108.6 . . ? O36 C36 C35 111.0(4) . . ? O36 C36 H36A 109.4 . . ? C35 C36 H36A 109.4 . . ? O36 C36 H36B 109.4 . . ? C35 C36 H36B 109.4 . . ? H36A C36 H36B 108.0 . . ? O32 C37 H37A 109.5 . . ? O32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O33 C38 H38A 109.5 . . ? O33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O36 C39 H39A 109.5 . . ? O36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? O36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O34 C41 O45 111.8(4) . . ? O34 C41 C42 111.3(4) . . ? O45 C41 C42 108.6(4) . . ? O34 C41 H41 108.3 . . ? O45 C41 H41 108.3 . . ? C42 C41 H41 108.3 . . ? O42 C42 C41 113.0(4) . . ? O42 C42 C43 107.3(4) . . ? C41 C42 C43 108.7(4) . . ? O42 C42 H42 109.2 . . ? C41 C42 H42 109.2 . . ? C43 C42 H42 109.2 . . ? O43 C43 C42 108.8(4) . . ? O43 C43 C44 107.9(4) . . ? C42 C43 C44 111.4(4) . . ? O43 C43 H43 109.6 . . ? C42 C43 H43 109.6 . . ? C44 C43 H43 109.6 . . ? O44 C44 C45 110.7(4) . . ? O44 C44 C43 105.4(4) . . ? C45 C44 C43 112.4(4) . . ? O44 C44 H44 109.4 . . ? C45 C44 H44 109.4 . . ? C43 C44 H44 109.4 . . ? O45 C45 C44 112.2(4) . . ? O45 C45 C46A 104.9(4) . . ? C44 C45 C46A 113.2(5) . . ? O45 C45 H45 108.8 . . ? C44 C45 H45 108.8 . . ? C46A C45 H45 108.8 . . ? O42 C47 H47A 109.5 . . ? O42 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? O42 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? O43 C48 H48A 109.5 . . ? O43 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? O43 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O55 C51 O44 111.3(4) . . ? O55 C51 C52 108.3(4) . . ? O44 C51 C52 109.4(4) . . ? O55 C51 H51 109.3 . . ? O44 C51 H51 109.3 . . ? C52 C51 H51 109.3 . . ? O52 C52 C53 108.0(5) . . ? O52 C52 C51 111.0(4) . . ? C53 C52 C51 109.9(4) . . ? O52 C52 H52 109.3 . . ? C53 C52 H52 109.3 . . ? C51 C52 H52 109.3 . . ? O53 C53 C52 108.6(4) . . ? O53 C53 C54 109.5(4) . . ? C52 C53 C54 110.0(5) . . ? O53 C53 H53 109.6 . . ? C52 C53 H53 109.6 . . ? C54 C53 H53 109.6 . . ? O54 C54 C53 106.1(4) . . ? O54 C54 C55 112.2(4) . . ? C53 C54 C55 111.4(4) . . ? O54 C54 H54 109.0 . . ? C53 C54 H54 109.1 . . ? C55 C54 H54 109.0 . . ? O55 C55 C56 106.9(4) . . ? O55 C55 C54 110.5(4) . . ? C56 C55 C54 114.9(4) . . ? O55 C55 H55 108.1 . . ? C56 C55 H55 108.1 . . ? C54 C55 H55 108.1 . . ? O56 C56 C55 109.9(4) . . ? O56 C56 H56A 109.7 . . ? C55 C56 H56A 109.7 . . ? O56 C56 H56B 109.7 . . ? C55 C56 H56B 109.7 . . ? H56A C56 H56B 108.2 . . ? O52 C57 H57A 109.5 . . ? O52 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? O52 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? O53 C58 H58A 109.5 . . ? O53 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? O53 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? O56 C59 H59A 109.5 . . ? O56 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? O56 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? O61 C61 N1 124.8(5) . . ? O61 C61 C62 129.5(5) . . ? N1 C61 C62 105.7(5) . . ? C67 C62 C63A 121.6(9) . . ? C67 C62 C63B 124.9(7) . . ? C63A C62 C63B 32.6(8) . . ? C67 C62 C61 106.4(5) . . ? C63A C62 C61 127.0(9) . . ? C63B C62 C61 126.6(8) . . ? C62 C63A C64A 114.5(15) . . ? C62 C63A H63A 122.8 . . ? C64A C63A H63A 122.8 . . ? C63A C64A C65A 123.4(18) . . ? C63A C64A H64A 118.3 . . ? C65A C64A H64A 118.3 . . ? C66A C65A C64A 119.6(18) . . ? C66A C65A H65A 120.2 . . ? C64A C65A H65A 120.2 . . ? C65A C66A C67 115.4(15) . . ? C65A C66A H66A 122.3 . . ? C67 C66A H66A 122.3 . . ? C64B C63B C62 115.0(11) . . ? C64B C63B H63B 122.5 . . ? C62 C63B H63B 122.5 . . ? C63B C64B C65B 120.3(12) . . ? C63B C64B H64B 119.8 . . ? C65B C64B H64B 119.8 . . ? C66B C65B C64B 122.2(13) . . ? C66B C65B H65B 118.9 . . ? C64B C65B H65B 118.9 . . ? C65B C66B C67 119.4(12) . . ? C65B C66B H66B 120.3 . . ? C67 C66B H66B 120.3 . . ? C62 C67 C68 109.9(5) . . ? C62 C67 C66A 124.6(9) . . ? C68 C67 C66A 123.1(9) . . ? C62 C67 C66B 116.2(8) . . ? C68 C67 C66B 128.8(8) . . ? C66A C67 C66B 35.8(7) . . ? O62 C68 N1 123.5(6) . . ? O62 C68 C67 129.7(6) . . ? N1 C68 C67 106.7(5) . . ? H63C O63 H63D 85.7 . . ? Cl2 C81 Cl1 115.8(9) . . ? Cl2 C81 H81A 108.3 . . ? Cl1 C81 H81A 108.4 . . ? Cl2 C81 H81B 108.3 . . ? Cl1 C81 H81B 108.3 . . ? H81A C81 H81B 107.4 . . ? C72 C71 H71A 109.4 . . ? C72 C71 H71B 109.1 . . ? H71A C71 H71B 109.5 . . ? C72 C71 H71C 109.9 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C73 C72 C71 128(2) . . ? C73 C72 H72A 105.0 . . ? C71 C72 H72A 105.1 . . ? C73 C72 H72B 105.5 . . ? C71 C72 H72B 105.9 . . ? H72A C72 H72B 106.0 . . ? C72 C73 C74 112.7(17) . . ? C72 C73 H73A 109.4 . . ? C74 C73 H73A 108.9 . . ? C72 C73 H73B 108.9 . . ? C74 C73 H73B 109.1 . . ? H73A C73 H73B 107.8 . . ? C75 C74 C73 114.8(14) . . ? C75 C74 H74A 108.6 . . ? C73 C74 H74A 108.5 . . ? C75 C74 H74B 108.6 . . ? C73 C74 H74B 108.6 . . ? H74A C74 H74B 107.6 . . ? C74 C75 H75A 109.5 . . ? C74 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C74 C75 H75C 109.4 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C77 C76 H76A 109.5 . . ? C77 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C77 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C78 C77 C76 153.3(7) . . ? C78 C77 H77A 98.2 . . ? C76 C77 H77A 98.2 . . ? C78 C77 H77B 98.2 . . ? C76 C77 H77B 98.2 . . ? H77A C77 H77B 103.8 . . ? C77 C78 C79 122.7(6) . . ? C77 C78 H78A 106.7 . . ? C79 C78 H78A 106.7 . . ? C77 C78 H78B 106.6 . . ? C79 C78 H78B 106.6 . . ? H78A C78 H78B 106.6 . . ? C80 C79 C78 160.3(5) . . ? C80 C79 H79A 96.1 . . ? C78 C79 H79A 96.1 . . ? C80 C79 H79B 96.1 . . ? C78 C79 H79B 96.1 . . ? H79A C79 H79B 103.4 . . ? C79 C80 H80A 109.5 . . ? C79 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C79 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C45 C46A O46A C49A -163.6(18) . . . . ? C5 O5 C1 O54 57.6(5) . . . . ? C5 O5 C1 C2 -62.4(4) . . . . ? C54 O54 C1 O5 108.3(4) . . . . ? C54 O54 C1 C2 -133.0(4) . . . . ? C7 O2 C2 C1 65.0(5) . . . . ? C7 O2 C2 C3 -171.6(4) . . . . ? O5 C1 C2 O2 179.4(4) . . . . ? O54 C1 C2 O2 59.6(5) . . . . ? O5 C1 C2 C3 58.8(5) . . . . ? O54 C1 C2 C3 -61.0(5) . . . . ? C8 O3 C3 C2 -111.0(5) . . . . ? C8 O3 C3 C4 126.3(4) . . . . ? O2 C2 C3 O3 59.7(5) . . . . ? C1 C2 C3 O3 -175.1(4) . . . . ? O2 C2 C3 C4 -178.9(4) . . . . ? C1 C2 C3 C4 -53.7(5) . . . . ? C11 O4 C4 C3 122.9(4) . . . . ? C11 O4 C4 C5 -114.8(4) . . . . ? O3 C3 C4 O4 -66.8(5) . . . . ? C2 C3 C4 O4 169.8(4) . . . . ? O3 C3 C4 C5 171.7(4) . . . . ? C2 C3 C4 C5 48.4(5) . . . . ? C1 O5 C5 C6 -179.3(4) . . . . ? C1 O5 C5 C4 58.3(5) . . . . ? O4 C4 C5 O5 -169.7(4) . . . . ? C3 C4 C5 O5 -49.8(5) . . . . ? O4 C4 C5 C6 72.3(5) . . . . ? C3 C4 C5 C6 -167.8(4) . . . . ? C68 N1 C6 C5 -103.8(6) . . . . ? C61 N1 C6 C5 79.0(6) . . . . ? O5 C5 C6 N1 69.4(5) . . . . ? C4 C5 C6 N1 -169.4(4) . . . . ? C15 O15 C11 O4 59.7(5) . . . . ? C15 O15 C11 C12 -61.1(5) . . . . ? C4 O4 C11 O15 91.2(4) . . . . ? C4 O4 C11 C12 -148.1(4) . . . . ? C17 O12 C12 C11 94.5(6) . . . . ? C17 O12 C12 C13 -140.4(6) . . . . ? O15 C11 C12 O12 178.9(4) . . . . ? O4 C11 C12 O12 57.3(5) . . . . ? O15 C11 C12 C13 55.9(6) . . . . ? O4 C11 C12 C13 -65.7(5) . . . . ? C18 O13 C13 C12 -122.7(6) . . . . ? C18 O13 C13 C14 114.0(6) . . . . ? O12 C12 C13 O13 62.9(6) . . . . ? C11 C12 C13 O13 -171.9(5) . . . . ? O12 C12 C13 C14 -175.3(4) . . . . ? C11 C12 C13 C14 -50.1(6) . . . . ? C21 O14 C14 C13 147.4(4) . . . . ? C21 O14 C14 C15 -91.1(5) . . . . ? O13 C13 C14 O14 -71.8(5) . . . . ? C12 C13 C14 O14 166.3(4) . . . . ? O13 C13 C14 C15 168.2(4) . . . . ? C12 C13 C14 C15 46.3(6) . . . . ? C11 O15 C15 C16 -177.4(4) . . . . ? C11 O15 C15 C14 57.2(5) . . . . ? O14 C14 C15 O15 -164.7(4) . . . . ? C13 C14 C15 O15 -48.1(6) . . . . ? O14 C14 C15 C16 76.2(5) . . . . ? C13 C14 C15 C16 -167.2(4) . . . . ? O15 C15 C16 O16 -64.2(5) . . . . ? C14 C15 C16 O16 57.4(6) . . . . ? C25 O25 C21 O14 55.4(5) . . . . ? C25 O25 C21 C22 -65.1(5) . . . . ? C14 O14 C21 O25 102.0(5) . . . . ? C14 O14 C21 C22 -137.7(4) . . . . ? C27 O22 C22 C21 64.3(6) . . . . ? C27 O22 C22 C23 -172.1(5) . . . . ? O25 C21 C22 O22 176.0(4) . . . . ? O14 C21 C22 O22 53.9(5) . . . . ? O25 C21 C22 C23 54.7(5) . . . . ? O14 C21 C22 C23 -67.4(5) . . . . ? C28 O23 C23 C24 140.5(5) . . . . ? C28 O23 C23 C22 -96.8(5) . . . . ? O22 C22 C23 O23 69.1(5) . . . . ? C21 C22 C23 O23 -166.1(4) . . . . ? O22 C22 C23 C24 -171.1(4) . . . . ? C21 C22 C23 C24 -46.3(6) . . . . ? C31 O24 C24 C23 117.7(4) . . . . ? C31 O24 C24 C25 -119.0(4) . . . . ? O23 C23 C24 O24 -75.7(5) . . . . ? C22 C23 C24 O24 164.1(4) . . . . ? O23 C23 C24 C25 164.4(4) . . . . ? C22 C23 C24 C25 44.1(5) . . . . ? C21 O25 C25 C26 -175.4(4) . . . . ? C21 O25 C25 C24 62.0(5) . . . . ? O24 C24 C25 O25 -170.1(3) . . . . ? C23 C24 C25 O25 -50.0(5) . . . . ? O24 C24 C25 C26 70.5(5) . . . . ? C23 C24 C25 C26 -169.3(4) . . . . ? C29 O26 C26 C25 -175.6(5) . . . . ? O25 C25 C26 O26 -65.1(5) . . . . ? C24 C25 C26 O26 55.2(6) . . . . ? C35 O35 C31 O24 60.6(5) . . . . ? C35 O35 C31 C32 -60.2(5) . . . . ? C24 O24 C31 O35 100.5(4) . . . . ? C24 O24 C31 C32 -140.0(4) . . . . ? C37 O32 C32 C31 92.2(6) . . . . ? C37 O32 C32 C33 -145.4(5) . . . . ? O35 C31 C32 O32 178.8(4) . . . . ? O24 C31 C32 O32 57.4(5) . . . . ? O35 C31 C32 C33 58.2(5) . . . . ? O24 C31 C32 C33 -63.1(5) . . . . ? C38 O33 C33 C32 -109.1(5) . . . . ? C38 O33 C33 C34 130.9(4) . . . . ? O32 C32 C33 O33 64.1(5) . . . . ? C31 C32 C33 O33 -173.5(4) . . . . ? O32 C32 C33 C34 -176.1(4) . . . . ? C31 C32 C33 C34 -53.7(5) . . . . ? C41 O34 C34 C35 -106.0(5) . . . . ? C41 O34 C34 C33 129.9(4) . . . . ? O33 C33 C34 O34 -69.1(4) . . . . ? C32 C33 C34 O34 171.7(4) . . . . ? O33 C33 C34 C35 168.6(4) . . . . ? C32 C33 C34 C35 49.4(5) . . . . ? C31 O35 C35 C36 180.0(4) . . . . ? C31 O35 C35 C34 55.9(5) . . . . ? O34 C34 C35 O35 -168.1(3) . . . . ? C33 C34 C35 O35 -48.8(5) . . . . ? O34 C34 C35 C36 72.3(5) . . . . ? C33 C34 C35 C36 -168.4(4) . . . . ? C39 O36 C36 C35 -171.0(5) . . . . ? O35 C35 C36 O36 64.7(5) . . . . ? C34 C35 C36 O36 -173.3(4) . . . . ? C34 O34 C41 O45 101.5(5) . . . . ? C34 O34 C41 C42 -136.7(4) . . . . ? C45 O45 C41 O34 59.8(5) . . . . ? C45 O45 C41 C42 -63.5(5) . . . . ? C47 O42 C42 C41 70.9(6) . . . . ? C47 O42 C42 C43 -169.2(5) . . . . ? O34 C41 C42 O42 56.5(5) . . . . ? O45 C41 C42 O42 -179.9(4) . . . . ? O34 C41 C42 C43 -62.6(5) . . . . ? O45 C41 C42 C43 61.0(5) . . . . ? C48 O43 C43 C42 -110.7(5) . . . . ? C48 O43 C43 C44 128.3(5) . . . . ? O42 C42 C43 O43 64.3(5) . . . . ? C41 C42 C43 O43 -173.1(4) . . . . ? O42 C42 C43 C44 -176.9(4) . . . . ? C41 C42 C43 C44 -54.3(6) . . . . ? C51 O44 C44 C45 -105.9(5) . . . . ? C51 O44 C44 C43 132.3(5) . . . . ? O43 C43 C44 O44 -72.1(5) . . . . ? C42 C43 C44 O44 168.6(4) . . . . ? O43 C43 C44 C45 167.2(4) . . . . ? C42 C43 C44 C45 47.9(6) . . . . ? C41 O45 C45 C44 56.6(5) . . . . ? C41 O45 C45 C46A 179.9(6) . . . . ? O44 C44 C45 O45 -165.2(4) . . . . ? C43 C44 C45 O45 -47.6(6) . . . . ? O44 C44 C45 C46A 76.3(6) . . . . ? C43 C44 C45 C46A -166.0(5) . . . . ? O46A C46A C45 O45 61.2(10) . . . . ? O46A C46A C45 C44 -176.2(8) . . . . ? C55 O55 C51 O44 57.1(5) . . . . ? C55 O55 C51 C52 -63.1(5) . . . . ? C44 O44 C51 O55 101.4(5) . . . . ? C44 O44 C51 C52 -139.0(4) . . . . ? C57 O52 C52 C53 -133.0(8) . . . . ? C57 O52 C52 C51 106.6(8) . . . . ? O55 C51 C52 O52 -179.8(4) . . . . ? O44 C51 C52 O52 58.8(5) . . . . ? O55 C51 C52 C53 60.9(5) . . . . ? O44 C51 C52 C53 -60.5(5) . . . . ? C58 O53 C53 C52 -121.8(6) . . . . ? C58 O53 C53 C54 118.1(6) . . . . ? O52 C52 C53 O53 63.1(5) . . . . ? C51 C52 C53 O53 -175.8(4) . . . . ? O52 C52 C53 C54 -177.1(4) . . . . ? C51 C52 C53 C54 -56.0(5) . . . . ? C1 O54 C54 C53 139.6(4) . . . . ? C1 O54 C54 C55 -98.6(5) . . . . ? O53 C53 C54 O54 -66.8(5) . . . . ? C52 C53 C54 O54 173.9(4) . . . . ? O53 C53 C54 C55 170.9(4) . . . . ? C52 C53 C54 C55 51.6(5) . . . . ? C51 O55 C55 C56 -175.2(4) . . . . ? C51 O55 C55 C54 59.0(5) . . . . ? O54 C54 C55 O55 -170.5(4) . . . . ? C53 C54 C55 O55 -51.8(5) . . . . ? O54 C54 C55 C56 68.4(5) . . . . ? C53 C54 C55 C56 -172.9(4) . . . . ? C59 O56 C56 C55 177.4(5) . . . . ? O55 C55 C56 O56 -70.0(5) . . . . ? C54 C55 C56 O56 53.1(6) . . . . ? C68 N1 C61 O61 -179.1(6) . . . . ? C6 N1 C61 O61 -1.6(9) . . . . ? C68 N1 C61 C62 0.3(7) . . . . ? C6 N1 C61 C62 177.8(5) . . . . ? O61 C61 C62 C67 -179.0(7) . . . . ? N1 C61 C62 C67 1.6(8) . . . . ? O61 C61 C62 C63A -24.0(17) . . . . ? N1 C61 C62 C63A 156.6(13) . . . . ? O61 C61 C62 C63B 17.0(14) . . . . ? N1 C61 C62 C63B -162.3(10) . . . . ? C67 C62 C63A C64A -9(2) . . . . ? C63B C62 C63A C64A 97(2) . . . . ? C61 C62 C63A C64A -161.0(12) . . . . ? C62 C63A C64A C65A 12(3) . . . . ? C63A C64A C65A C66A -7(3) . . . . ? C64A C65A C66A C67 0(3) . . . . ? C67 C62 C63B C64B 7.7(18) . . . . ? C63A C62 C63B C64B -88(2) . . . . ? C61 C62 C63B C64B 168.9(10) . . . . ? C62 C63B C64B C65B -11(2) . . . . ? C63B C64B C65B C66B 2(2) . . . . ? C64B C65B C66B C67 11(2) . . . . ? C63A C62 C67 C68 -159.5(13) . . . . ? C63B C62 C67 C68 161.4(10) . . . . ? C61 C62 C67 C68 -2.9(9) . . . . ? C63A C62 C67 C66A 3.0(19) . . . . ? C63B C62 C67 C66A -36.1(18) . . . . ? C61 C62 C67 C66A 159.6(12) . . . . ? C63A C62 C67 C66B 43.6(16) . . . . ? C63B C62 C67 C66B 4.5(16) . . . . ? C61 C62 C67 C66B -159.8(10) . . . . ? C65A C66A C67 C62 2(2) . . . . ? C65A C66A C67 C68 162.7(13) . . . . ? C65A C66A C67 C66B -85(2) . . . . ? C65B C66B C67 C62 -14.2(19) . . . . ? C65B C66B C67 C68 -166.0(11) . . . . ? C65B C66B C67 C66A 99(2) . . . . ? C61 N1 C68 O62 176.2(6) . . . . ? C6 N1 C68 O62 -1.3(9) . . . . ? C61 N1 C68 C67 -2.0(7) . . . . ? C6 N1 C68 C67 -179.5(6) . . . . ? C62 C67 C68 O62 -175.0(7) . . . . ? C66A C67 C68 O62 22.2(15) . . . . ? C66B C67 C68 O62 -21.8(16) . . . . ? C62 C67 C68 N1 3.1(9) . . . . ? C66A C67 C68 N1 -159.7(11) . . . . ? C66B C67 C68 N1 156.2(11) . . . . ? C71 C72 C73 C74 -106(3) . . . . ? C72 C73 C74 C75 -70(2) . . . . ? C76 C77 C78 C79 84.7(17) . . . . ? C77 C78 C79 C80 -38.9(18) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.929 _refine_diff_density_min -0.926 _refine_diff_density_rms 0.074