# 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 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Liangbing Gan' _publ_contact_author_email gan@pku.edu.cn loop_ _publ_author_name 'Liangbing Gan' 'Shuming Liu' 'Yuanhua Shao' data_gang100 _database_code_depnum_ccdc_archive 'CCDC 854104' #TrackingRef 'gang100.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C101 H50 N2 O5' _chemical_formula_weight 1371.43 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 32.301(7) _cell_length_b 11.246(2) _cell_length_c 36.097(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13112(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5680 _exptl_absorpt_coefficient_mu 0.085 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9874 _exptl_absorpt_correction_T_max 0.9874 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'synchrotron diffraction' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45802 _diffrn_reflns_av_R_equivalents 0.0648 _diffrn_reflns_av_sigmaI/netI 0.0460 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12863 _reflns_number_gt 10172 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.1566P)^2^+8.0190P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0037(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12863 _refine_ls_number_parameters 978 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0871 _refine_ls_R_factor_gt 0.0735 _refine_ls_wR_factor_ref 0.2360 _refine_ls_wR_factor_gt 0.2215 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.43695(5) 0.48062(12) 0.11588(4) 0.0262(3) Uani 1 1 d . . . C2 C 0.40632(5) 0.54227(12) 0.09284(4) 0.0235(3) Uani 1 1 d . . . C3 C 0.40937(4) 0.52830(12) 0.05353(4) 0.0222(3) Uani 1 1 d . . . C4 C 0.44263(4) 0.46688(12) 0.03921(4) 0.0233(3) Uani 1 1 d . . . C5 C 0.47880(5) 0.43616(12) 0.06221(4) 0.0260(3) Uani 1 1 d . . . C6 C 0.37755(4) 0.57711(12) 0.02603(4) 0.0215(3) Uani 1 1 d . . . C7 C 0.37326(4) 0.48592(12) -0.00574(4) 0.0228(3) Uani 1 1 d . . . C8 C 0.40955(4) 0.43097(12) -0.01832(4) 0.0233(3) Uani 1 1 d . . . C9 C 0.40950(5) 0.36455(13) -0.05099(4) 0.0271(4) Uani 1 1 d . . . H9 H 0.4344 0.3298 -0.0598 0.033 Uiso 1 1 calc R . . C10 C 0.37301(5) 0.34964(13) -0.07048(5) 0.0285(4) Uani 1 1 d . . . H10 H 0.3734 0.3059 -0.0930 0.034 Uiso 1 1 calc R . . C11 C 0.33559(5) 0.39741(13) -0.05786(4) 0.0266(3) Uani 1 1 d . . . C12 C 0.33650(5) 0.46528(13) -0.02532(4) 0.0254(3) Uani 1 1 d . . . H12 H 0.3114 0.4983 -0.0162 0.030 Uiso 1 1 calc R . . C13 C 0.29443(5) 0.37312(14) -0.07798(5) 0.0304(4) Uani 1 1 d . . . C14 C 0.30098(6) 0.3356(2) -0.11829(6) 0.0529(6) Uani 1 1 d . . . H14A H 0.3168 0.2614 -0.1190 0.079 Uiso 1 1 calc R . . H14B H 0.3162 0.3980 -0.1314 0.079 Uiso 1 1 calc R . . H14C H 0.2741 0.3235 -0.1302 0.079 Uiso 1 1 calc R . . C15 C 0.26655(5) 0.48414(16) -0.07800(5) 0.0369(4) Uani 1 1 d . . . H15A H 0.2810 0.5499 -0.0903 0.055 Uiso 1 1 calc R . . H15B H 0.2601 0.5066 -0.0524 0.055 Uiso 1 1 calc R . . H15C H 0.2408 0.4666 -0.0913 0.055 Uiso 1 1 calc R . . C16 C 0.27191(6) 0.27375(16) -0.05716(6) 0.0419(5) Uani 1 1 d . . . H16A H 0.2447 0.2605 -0.0684 0.063 Uiso 1 1 calc R . . H16B H 0.2684 0.2967 -0.0312 0.063 Uiso 1 1 calc R . . H16C H 0.2882 0.2004 -0.0586 0.063 Uiso 1 1 calc R . . C17 C 0.45474(5) 0.37166(13) 0.16981(4) 0.0295(4) Uani 1 1 d . . . C18 C 0.49719(6) 0.35083(16) 0.16439(5) 0.0372(4) Uani 1 1 d . . . H18 H 0.5120 0.3947 0.1462 0.045 Uiso 1 1 calc R . . C19 C 0.51756(6) 0.26587(16) 0.18572(5) 0.0392(4) Uani 1 1 d . . . H19 H 0.5461 0.2518 0.1813 0.047 Uiso 1 1 calc R . . C20 C 0.49779(6) 0.20143(14) 0.21297(5) 0.0363(4) Uani 1 1 d . . . C21 C 0.45613(6) 0.22760(14) 0.21989(5) 0.0352(4) Uani 1 1 d . . . H21 H 0.4420 0.1872 0.2392 0.042 Uiso 1 1 calc R . . C22 C 0.43502(6) 0.31194(13) 0.19885(5) 0.0327(4) Uani 1 1 d . . . H22 H 0.4069 0.3291 0.2043 0.039 Uiso 1 1 calc R . . C23 C 0.52058(6) 0.10701(16) 0.23622(5) 0.0416(5) Uani 1 1 d . . . C24 C 0.56078(10) 0.0680(3) 0.21789(9) 0.1132(10) Uani 1 1 d . . . H24A H 0.5817 0.1302 0.2210 0.170 Uiso 1 1 calc R . . H24B H 0.5560 0.0544 0.1914 0.170 Uiso 1 1 calc R . . H24C H 0.5705 -0.0057 0.2294 0.170 Uiso 1 1 calc R . . C25 C 0.52936(9) 0.15961(19) 0.27429(6) 0.0652(7) Uani 1 1 d . . . H25A H 0.5446 0.1016 0.2893 0.098 Uiso 1 1 calc R . . H25B H 0.5032 0.1791 0.2865 0.098 Uiso 1 1 calc R . . H25C H 0.5460 0.2320 0.2715 0.098 Uiso 1 1 calc R . . C26 C 0.37214(5) 0.59965(12) 0.10816(4) 0.0251(3) Uani 1 1 d . . . C27 C 0.49316(9) -0.00206(19) 0.24119(8) 0.0778(8) Uani 1 1 d . . . H27A H 0.4839 -0.0303 0.2169 0.117 Uiso 1 1 calc R . . H27B H 0.4690 0.0190 0.2563 0.117 Uiso 1 1 calc R . . H27C H 0.5089 -0.0650 0.2536 0.117 Uiso 1 1 calc R . . C28 C 0.33602(4) 0.61474(12) 0.08433(4) 0.0241(3) Uani 1 1 d . . . C29 C 0.33760(4) 0.60849(12) 0.04633(4) 0.0228(3) Uani 1 1 d . . . C30 C 0.38434(4) 0.69899(12) 0.00528(4) 0.0214(3) Uani 1 1 d . . . C31 C 0.41789(4) 0.77357(13) -0.00012(4) 0.0243(3) Uani 1 1 d . . . C32 C 0.46019(4) 0.77281(13) 0.01801(4) 0.0253(3) Uani 1 1 d . . . C33 C 0.47007(5) 0.90287(13) 0.02511(5) 0.0282(4) Uani 1 1 d . . . C34 C 0.48715(4) 0.94997(13) 0.05701(5) 0.0310(4) Uani 1 1 d . . . C35 C 0.50149(5) 0.88450(14) 0.09087(5) 0.0329(4) Uani 1 1 d . . . C36 C 0.47863(5) 0.94564(14) 0.12226(5) 0.0318(4) Uani 1 1 d . . . C37 C 0.45358(5) 0.89209(14) 0.14808(5) 0.0302(4) Uani 1 1 d . . . C38 C 0.44219(5) 0.76093(14) 0.14743(4) 0.0290(4) Uani 1 1 d . . . C39 C 0.39669(5) 0.75589(14) 0.15639(4) 0.0282(4) Uani 1 1 d . . . C40 C 0.36699(5) 0.68294(13) 0.13935(4) 0.0262(3) Uani 1 1 d . . . C41 C 0.32479(5) 0.73045(13) 0.13629(4) 0.0272(4) Uani 1 1 d . . . C42 C 0.30647(4) 0.68991(13) 0.10261(4) 0.0260(3) Uani 1 1 d . . . C43 C 0.27966(4) 0.76114(13) 0.08209(5) 0.0274(4) Uani 1 1 d . . . C44 C 0.28435(4) 0.76604(13) 0.04261(5) 0.0266(3) Uani 1 1 d . . . C45 C 0.31478(4) 0.69493(13) 0.02584(4) 0.0247(3) Uani 1 1 d . . . C46 C 0.34290(4) 0.74776(13) -0.00075(4) 0.0245(3) Uani 1 1 d . . . C47 C 0.33630(5) 0.86438(14) -0.01238(4) 0.0274(4) Uani 1 1 d . . . C48 C 0.37101(5) 0.93978(13) -0.01874(4) 0.0288(4) Uani 1 1 d . . . C49 C 0.41038(5) 0.89546(13) -0.01172(4) 0.0277(4) Uani 1 1 d . . . C50 C 0.44127(5) 0.97236(13) 0.00397(5) 0.0297(4) Uani 1 1 d . . . C51 C 0.43132(5) 1.08999(13) 0.01351(5) 0.0325(4) Uani 1 1 d . . . C52 C 0.44737(5) 1.13613(13) 0.04751(5) 0.0341(4) Uani 1 1 d . . . C53 C 0.47334(5) 1.06672(13) 0.06938(5) 0.0327(4) Uani 1 1 d . . . C54 C 0.46808(5) 1.06294(13) 0.10910(5) 0.0333(4) Uani 1 1 d . . . C55 C 0.43605(5) 1.12825(13) 0.12547(5) 0.0331(4) Uani 1 1 d . . . C56 C 0.41138(5) 1.07341(14) 0.15376(5) 0.0316(4) Uani 1 1 d . . . C57 C 0.41908(5) 0.95547(14) 0.16317(5) 0.0307(4) Uani 1 1 d . . . C58 C 0.38507(5) 0.87357(14) 0.16889(4) 0.0294(4) Uani 1 1 d . . . C59 C 0.34435(5) 0.91580(14) 0.16719(4) 0.0296(4) Uani 1 1 d . . . C60 C 0.31343(5) 0.84231(14) 0.14999(4) 0.0289(4) Uani 1 1 d . . . C61 C 0.28579(5) 0.91768(14) 0.12916(5) 0.0299(4) Uani 1 1 d . . . C62 C 0.26950(4) 0.87901(14) 0.09539(5) 0.0284(4) Uani 1 1 d . . . C63 C 0.26857(4) 0.95763(14) 0.06386(5) 0.0298(4) Uani 1 1 d . . . C64 C 0.27850(4) 0.88799(14) 0.03121(5) 0.0289(4) Uani 1 1 d . . . C65 C 0.30337(5) 0.93598(14) 0.00348(5) 0.0298(4) Uani 1 1 d . . . C66 C 0.36010(5) 1.06009(13) -0.00797(5) 0.0320(4) Uani 1 1 d . . . C67 C 0.38973(5) 1.13369(13) 0.00824(5) 0.0341(4) Uani 1 1 d . . . C68 C 0.37924(5) 1.20606(13) 0.04015(5) 0.0342(4) Uani 1 1 d . . . C69 C 0.41488(5) 1.20712(13) 0.06481(5) 0.0338(4) Uani 1 1 d . . . C70 C 0.40951(5) 1.20221(12) 0.10288(6) 0.0333(4) Uani 1 1 d . . . C71 C 0.36793(5) 1.19554(12) 0.11843(5) 0.0309(4) Uani 1 1 d . . . C72 C 0.36922(5) 1.11616(13) 0.15008(5) 0.0301(4) Uani 1 1 d . . . C73 C 0.33641(5) 1.03841(14) 0.15682(5) 0.0298(4) Uani 1 1 d . . . C74 C 0.30045(5) 1.03941(14) 0.13266(5) 0.0300(4) Uani 1 1 d . . . C75 C 0.29920(5) 1.11575(13) 0.10223(5) 0.0309(4) Uani 1 1 d . . . C76 C 0.33364(5) 1.19504(13) 0.09483(5) 0.0307(4) Uani 1 1 d . . . C77 C 0.33928(5) 1.20045(13) 0.05496(5) 0.0320(4) Uani 1 1 d . . . C78 C 0.30849(5) 1.12502(13) 0.03778(5) 0.0315(4) Uani 1 1 d . . . C79 C 0.28360(5) 1.07370(14) 0.06712(5) 0.0302(4) Uani 1 1 d . . . C80 C 0.31863(5) 1.05659(14) 0.00678(5) 0.0320(4) Uani 1 1 d . . . C81 C 0.59381(8) 0.5675(2) 0.18554(7) 0.0442(8) Uiso 0.544(3) 1 d PG A 1 H81 H 0.5771 0.5096 0.1735 0.053 Uiso 0.544(3) 1 calc PR A 1 C82 C 0.59000(10) 0.6869(2) 0.17612(9) 0.0915(18) Uiso 0.544(3) 1 d PG A 1 H82 H 0.5707 0.7105 0.1577 0.110 Uiso 0.544(3) 1 calc PR A 1 C83 C 0.61442(13) 0.7716(2) 0.19368(12) 0.0953(19) Uiso 0.544(3) 1 d PG A 1 H83 H 0.6118 0.8532 0.1872 0.114 Uiso 0.544(3) 1 calc PR A 1 C84 C 0.64266(13) 0.7370(3) 0.22066(12) 0.0833(15) Uiso 0.544(3) 1 d PG A 1 H84 H 0.6593 0.7949 0.2327 0.100 Uiso 0.544(3) 1 calc PR A 1 C85 C 0.64647(11) 0.6177(4) 0.23009(10) 0.0941(18) Uiso 0.544(3) 1 d PG A 1 H85 H 0.6658 0.5940 0.2485 0.113 Uiso 0.544(3) 1 calc PR A 1 C86 C 0.62205(10) 0.5329(3) 0.21253(8) 0.0670(12) Uiso 0.544(3) 1 d PGD A 1 C87 C 0.62783(19) 0.4101(5) 0.22474(18) 0.0837(16) Uiso 0.544(3) 1 d PD A 1 H87A H 0.6548 0.4023 0.2369 0.126 Uiso 0.544(3) 1 calc PR A 1 H87B H 0.6267 0.3569 0.2033 0.126 Uiso 0.544(3) 1 calc PR A 1 H87C H 0.6058 0.3888 0.2422 0.126 Uiso 0.544(3) 1 calc PR A 1 C81' C 0.59020(13) 0.5494(3) 0.18166(12) 0.171(6) Uiso 0.456(3) 1 d PG A 2 H81' H 0.5795 0.4742 0.1745 0.205 Uiso 0.456(3) 1 calc PR A 2 C82' C 0.57494(14) 0.6527(4) 0.16552(13) 0.0680(15) Uiso 0.456(3) 1 d PG A 2 H82' H 0.5538 0.6481 0.1473 0.082 Uiso 0.456(3) 1 calc PR A 2 C83' C 0.59063(17) 0.7627(3) 0.17604(15) 0.093(2) Uiso 0.456(3) 1 d PG A 2 H83' H 0.5802 0.8333 0.1650 0.112 Uiso 0.456(3) 1 calc PR A 2 C84' C 0.62158(18) 0.7695(4) 0.20271(17) 0.090(2) Uiso 0.456(3) 1 d PG A 2 H84' H 0.6323 0.8447 0.2099 0.108 Uiso 0.456(3) 1 calc PR A 2 C85' C 0.63685(17) 0.6662(5) 0.21885(16) 0.110(3) Uiso 0.456(3) 1 d PG A 2 H85' H 0.6580 0.6708 0.2371 0.133 Uiso 0.456(3) 1 calc PR A 2 C86' C 0.62116(15) 0.5561(4) 0.20832(14) 0.086(2) Uiso 0.456(3) 1 d PGD A 2 C87' C 0.6434(4) 0.4752(11) 0.2326(3) 0.156(4) Uiso 0.456(3) 1 d PD A 2 H87D H 0.6616 0.5209 0.2490 0.234 Uiso 0.456(3) 1 calc PR A 2 H87E H 0.6600 0.4203 0.2177 0.234 Uiso 0.456(3) 1 calc PR A 2 H87F H 0.6235 0.4300 0.2476 0.234 Uiso 0.456(3) 1 calc PR A 2 C88 C 0.57230(8) 0.2184(2) 0.10032(9) 0.0584(14) Uani 0.485(2) 1 d PG B 1 H88 H 0.5441 0.2209 0.0928 0.070 Uiso 0.485(2) 1 calc PR B 1 C89 C 0.59586(10) 0.3218(2) 0.10032(12) 0.123(4) Uani 0.485(2) 1 d PG B 1 H89 H 0.5838 0.3950 0.0928 0.148 Uiso 0.485(2) 1 calc PR B 1 C90 C 0.63710(10) 0.3181(3) 0.11126(15) 0.091(2) Uani 0.485(2) 1 d PG B 1 H90 H 0.6532 0.3888 0.1113 0.109 Uiso 0.485(2) 1 calc PR B 1 C91 C 0.65478(9) 0.2110(4) 0.12220(14) 0.095(3) Uani 0.485(2) 1 d PG B 1 H91 H 0.6830 0.2085 0.1297 0.114 Uiso 0.485(2) 1 calc PR B 1 C92 C 0.63121(10) 0.1076(3) 0.12220(13) 0.0646(16) Uani 0.485(2) 1 d PGD B 1 C93 C 0.58997(9) 0.1113(2) 0.11126(11) 0.0558(13) Uani 0.485(2) 1 d PG B 1 H93 H 0.5739 0.0406 0.1113 0.067 Uiso 0.485(2) 1 calc PR B 1 C94" C 0.59078(12) -0.0113(3) 0.10892(10) 0.0266(8) Uani 0.412(2) 1 d P B 3 C88' C 0.58547(7) 0.2012(2) 0.09983(7) 0.082(2) Uani 0.515(2) 1 d PG B 2 H88' H 0.5602 0.1791 0.0882 0.099 Uiso 0.515(2) 1 calc PR B 2 C89' C 0.59676(9) 0.3203(2) 0.10177(9) 0.0408(10) Uani 0.515(2) 1 d PG B 2 H89' H 0.5793 0.3796 0.0915 0.049 Uiso 0.515(2) 1 calc PR B 2 C90' C 0.63367(10) 0.3528(3) 0.11880(11) 0.0757(18) Uani 0.515(2) 1 d PG B 2 H90' H 0.6414 0.4342 0.1201 0.091 Uiso 0.515(2) 1 calc PR B 2 C91' C 0.65930(9) 0.2661(3) 0.13388(11) 0.0727(16) Uani 0.515(2) 1 d PG B 2 H91' H 0.6845 0.2882 0.1455 0.087 Uiso 0.515(2) 1 calc PR B 2 C92' C 0.64801(10) 0.1470(3) 0.13195(10) 0.0708(16) Uani 0.515(2) 1 d PGD B 2 C93' C 0.61109(9) 0.1145(2) 0.11492(9) 0.0956(18) Uani 0.515(2) 1 d PG B 2 H93' H 0.6034 0.0331 0.1136 0.115 Uiso 0.515(2) 1 calc PR B 2 C94' C 0.67083(12) 0.0410(4) 0.15042(12) 0.0417(10) Uani 0.438(2) 1 d PD B 2 H94A H 0.6529 -0.0293 0.1500 0.062 Uiso 0.438(2) 1 calc PR B 2 H94B H 0.6776 0.0613 0.1761 0.062 Uiso 0.438(2) 1 calc PR B 2 H94C H 0.6964 0.0241 0.1368 0.062 Uiso 0.438(2) 1 calc PR B 2 C96 C 0.28791(12) 0.3465(3) 0.19434(11) 0.0557(17) Uiso 0.315(2) 1 d PG C 1 H96 H 0.2806 0.2876 0.1766 0.067 Uiso 0.315(2) 1 calc PR C 1 C97 C 0.32103(13) 0.4223(4) 0.18758(13) 0.0415(13) Uiso 0.315(2) 1 d PG C 1 H97 H 0.3364 0.4153 0.1652 0.050 Uiso 0.315(2) 1 calc PR C 1 C98 C 0.33167(17) 0.5086(4) 0.21348(17) 0.0582(18) Uiso 0.315(2) 1 d PG C 1 H98 H 0.3543 0.5604 0.2088 0.070 Uiso 0.315(2) 1 calc PR C 1 C99 C 0.3092(2) 0.5189(5) 0.24615(16) 0.074(4) Uiso 0.1887(13) 1 d PGD C 1 C100 C 0.2761(2) 0.4431(6) 0.25291(13) 0.097(3) Uiso 0.315(2) 1 d PG C 1 H100 H 0.2607 0.4502 0.2752 0.116 Uiso 0.315(2) 1 calc PR C 1 C101 C 0.26542(15) 0.3569(5) 0.22701(14) 0.094(3) Uiso 0.315(2) 1 d PG C 1 H101 H 0.2428 0.3050 0.2316 0.113 Uiso 0.315(2) 1 calc PR C 1 C95" C 0.2520(5) 0.4102(14) 0.2950(5) 0.102(4) Uiso 0.2516(17) 1 d P C 3 C96' C 0.30187(18) 0.3493(5) 0.19117(15) 0.040(2) Uiso 0.185(2) 1 d PG C 2 H96' H 0.3116 0.3034 0.1709 0.049 Uiso 0.185(2) 1 calc PR C 2 C97' C 0.3197(2) 0.4590(5) 0.1989(2) 0.0288(18) Uiso 0.185(2) 1 d PG C 2 H97' H 0.3417 0.4881 0.1839 0.035 Uiso 0.185(2) 1 calc PR C 2 C98' C 0.3054(3) 0.5261(6) 0.2286(2) 0.085(5) Uiso 0.185(2) 1 d PGD C 2 C99' C 0.2733(3) 0.4836(8) 0.2506(2) 0.044(4) Uiso 0.1113(13) 1 d PG C 2 H99' H 0.2635 0.5294 0.2709 0.053 Uiso 0.1113(13) 1 calc PR C 2 C10' C 0.2555(3) 0.3739(9) 0.2428(2) 0.103(6) Uiso 0.185(2) 1 d PG C 2 H10' H 0.2335 0.3448 0.2578 0.124 Uiso 0.185(2) 1 calc PR C 2 C11' C 0.2698(2) 0.3068(6) 0.2131(2) 0.042(2) Uiso 0.185(2) 1 d PG C 2 H11' H 0.2576 0.2318 0.2078 0.050 Uiso 0.185(2) 1 calc PR C 2 C95 C 0.3229(8) 0.6063(17) 0.2743(5) 0.119(9) Uiso 0.15 1 d PD C 1 H95D H 0.3483 0.5776 0.2863 0.179 Uiso 0.15 1 calc PR C 1 H95E H 0.3012 0.6162 0.2930 0.179 Uiso 0.15 1 calc PR C 1 H95F H 0.3284 0.6829 0.2624 0.179 Uiso 0.15 1 calc PR C 1 N1 N 0.44533(4) 0.43624(11) 0.00330(4) 0.0244(3) Uani 1 1 d . . . H1 H 0.4681(7) 0.4012(19) -0.0060(6) 0.042(5) Uiso 1 1 d . . . N2 N 0.42862(4) 0.44490(11) 0.14834(4) 0.0285(3) Uani 1 1 d . . . O1 O 0.51077(3) 0.39802(10) 0.05011(3) 0.0323(3) Uani 1 1 d . . . O2 O 0.47499(3) 0.45394(10) 0.09921(3) 0.0296(3) Uani 1 1 d . . . O3 O 0.46482(4) 0.68214(10) 0.13685(3) 0.0338(3) Uani 1 1 d . . . O4 O 0.52553(4) 0.80216(11) 0.09292(4) 0.0425(3) Uani 1 1 d . . . O5 O 0.48118(3) 0.68881(9) 0.02765(3) 0.0283(3) Uani 1 1 d . . . C94 C 0.6499(3) -0.0115(8) 0.1283(3) 0.028(2) Uiso 0.15 1 d PD B 1 H94D H 0.6299 -0.0629 0.1410 0.041 Uiso 0.15 1 calc PR B 1 H94E H 0.6748 -0.0034 0.1435 0.041 Uiso 0.15 1 calc PR B 1 H94F H 0.6572 -0.0468 0.1044 0.041 Uiso 0.15 1 calc PR B 1 C95' C 0.3270(3) 0.6414(9) 0.2376(3) 0.035(2) Uiso 0.1484(17) 1 d PD C 2 H95A H 0.3516 0.6497 0.2219 0.053 Uiso 0.1484(17) 1 calc PR C 2 H95B H 0.3353 0.6414 0.2637 0.053 Uiso 0.1484(17) 1 calc PR C 2 H95C H 0.3082 0.7081 0.2330 0.053 Uiso 0.1484(17) 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0316(7) 0.0148(6) 0.0324(7) -0.0019(5) -0.0032(6) 0.0000(6) C2 0.0280(7) 0.0109(5) 0.0317(7) 0.0014(5) -0.0027(6) -0.0029(5) C3 0.0236(6) 0.0110(5) 0.0321(7) 0.0011(5) -0.0032(6) -0.0016(5) C4 0.0240(6) 0.0125(6) 0.0333(7) 0.0015(5) -0.0023(6) -0.0008(5) C5 0.0279(7) 0.0137(6) 0.0364(8) 0.0015(6) -0.0031(6) -0.0006(5) C6 0.0202(6) 0.0149(6) 0.0295(7) -0.0004(5) -0.0015(5) -0.0010(5) C7 0.0249(6) 0.0135(6) 0.0300(7) -0.0012(5) 0.0000(6) -0.0017(5) C8 0.0215(6) 0.0155(6) 0.0329(7) 0.0019(5) -0.0010(6) -0.0010(5) C9 0.0278(7) 0.0198(6) 0.0337(8) -0.0020(6) 0.0024(6) 0.0025(6) C10 0.0308(7) 0.0207(6) 0.0340(8) -0.0049(6) -0.0009(6) 0.0006(6) C11 0.0268(7) 0.0199(6) 0.0330(8) -0.0015(6) -0.0026(6) -0.0006(6) C12 0.0229(6) 0.0201(6) 0.0332(7) -0.0020(6) -0.0015(6) 0.0004(5) C13 0.0279(7) 0.0263(7) 0.0370(8) -0.0075(6) -0.0053(6) 0.0019(6) C14 0.0360(9) 0.0779(13) 0.0447(10) -0.0275(10) -0.0085(8) 0.0069(10) C15 0.0326(8) 0.0347(8) 0.0433(9) -0.0044(7) -0.0080(7) 0.0041(7) C16 0.0323(8) 0.0300(8) 0.0635(12) -0.0017(8) -0.0078(8) -0.0052(7) C17 0.0436(8) 0.0148(6) 0.0301(7) -0.0017(6) -0.0082(7) 0.0028(6) C18 0.0422(9) 0.0345(8) 0.0350(8) 0.0060(7) -0.0052(7) -0.0001(7) C19 0.0425(9) 0.0356(9) 0.0395(9) 0.0028(7) -0.0094(8) 0.0048(8) C20 0.0544(10) 0.0217(7) 0.0327(8) -0.0024(6) -0.0106(7) 0.0028(7) C21 0.0552(10) 0.0197(7) 0.0307(8) -0.0012(6) -0.0040(7) -0.0003(7) C22 0.0466(9) 0.0192(7) 0.0321(8) -0.0033(6) -0.0037(7) 0.0001(6) C23 0.0608(11) 0.0268(8) 0.0372(9) 0.0017(7) -0.0114(8) 0.0077(8) C24 0.133(2) 0.1146(17) 0.0916(18) 0.0559(14) 0.0370(16) 0.0933(15) C25 0.1054(16) 0.0319(9) 0.0584(12) -0.0014(9) -0.0433(11) 0.0069(11) C26 0.0308(7) 0.0135(6) 0.0310(7) 0.0025(5) 0.0008(6) -0.0038(5) C27 0.1069(17) 0.0287(9) 0.0979(16) 0.0191(10) -0.0566(14) -0.0051(11) C28 0.0235(6) 0.0139(6) 0.0347(7) -0.0004(5) 0.0023(6) -0.0061(5) C29 0.0194(6) 0.0150(6) 0.0341(7) -0.0028(5) -0.0009(6) -0.0047(5) C30 0.0216(6) 0.0145(6) 0.0281(7) -0.0018(5) -0.0008(5) 0.0031(5) C31 0.0230(6) 0.0180(6) 0.0318(7) 0.0012(6) 0.0032(6) 0.0042(5) C32 0.0201(6) 0.0185(6) 0.0373(8) -0.0010(6) 0.0066(6) -0.0001(5) C33 0.0210(6) 0.0172(6) 0.0463(9) 0.0002(6) 0.0089(6) -0.0024(5) C34 0.0171(6) 0.0198(7) 0.0561(10) -0.0030(7) 0.0056(6) -0.0029(6) C35 0.0193(6) 0.0246(7) 0.0548(10) -0.0090(7) -0.0016(7) -0.0030(6) C36 0.0213(6) 0.0238(7) 0.0504(9) -0.0112(7) -0.0085(6) 0.0004(6) C37 0.0262(7) 0.0239(7) 0.0405(8) -0.0099(6) -0.0130(6) 0.0041(6) C38 0.0324(7) 0.0226(7) 0.0321(7) -0.0042(6) -0.0106(6) 0.0035(6) C39 0.0337(7) 0.0227(7) 0.0281(7) -0.0008(6) -0.0034(6) 0.0009(6) C40 0.0315(7) 0.0188(6) 0.0283(7) 0.0024(6) 0.0016(6) -0.0009(6) C41 0.0282(7) 0.0218(6) 0.0318(7) 0.0002(6) 0.0055(6) -0.0055(6) C42 0.0223(6) 0.0203(6) 0.0353(8) -0.0026(6) 0.0054(6) -0.0077(5) C43 0.0162(6) 0.0238(7) 0.0420(8) -0.0061(6) 0.0034(6) -0.0061(5) C44 0.0160(6) 0.0245(7) 0.0392(8) -0.0054(6) -0.0032(6) -0.0026(6) C45 0.0191(6) 0.0204(6) 0.0347(8) -0.0055(6) -0.0031(6) -0.0025(5) C46 0.0234(6) 0.0208(6) 0.0291(7) -0.0029(5) -0.0021(6) 0.0025(6) C47 0.0257(7) 0.0252(7) 0.0314(7) -0.0001(6) -0.0043(6) 0.0071(6) C48 0.0359(8) 0.0204(7) 0.0302(7) 0.0039(6) 0.0026(6) 0.0074(6) C49 0.0289(7) 0.0212(7) 0.0332(7) 0.0045(6) 0.0071(6) 0.0024(6) C50 0.0264(7) 0.0195(7) 0.0432(8) 0.0046(6) 0.0126(6) -0.0011(6) C51 0.0317(7) 0.0164(6) 0.0494(9) 0.0077(6) 0.0127(7) -0.0030(6) C52 0.0281(7) 0.0129(6) 0.0612(10) 0.0015(7) 0.0092(7) -0.0046(6) C53 0.0223(7) 0.0170(6) 0.0587(10) -0.0047(7) 0.0052(7) -0.0066(6) C54 0.0191(6) 0.0197(6) 0.0613(10) -0.0108(7) -0.0048(7) -0.0058(6) C55 0.0262(7) 0.0170(6) 0.0562(10) -0.0129(7) -0.0057(7) -0.0040(6) C56 0.0279(7) 0.0213(7) 0.0455(9) -0.0143(6) -0.0081(7) 0.0006(6) C57 0.0285(7) 0.0267(7) 0.0369(8) -0.0108(6) -0.0102(6) 0.0020(6) C58 0.0340(7) 0.0240(7) 0.0302(7) -0.0051(6) -0.0035(6) 0.0010(6) C59 0.0329(7) 0.0258(7) 0.0301(7) -0.0062(6) 0.0032(6) 0.0000(6) C60 0.0282(7) 0.0265(7) 0.0320(7) -0.0032(6) 0.0066(6) -0.0031(6) C61 0.0208(6) 0.0280(7) 0.0410(8) -0.0081(6) 0.0074(6) -0.0011(6) C62 0.0143(6) 0.0269(7) 0.0441(9) -0.0070(6) 0.0031(6) -0.0010(6) C63 0.0161(6) 0.0291(7) 0.0444(9) -0.0076(7) -0.0022(6) 0.0068(6) C64 0.0175(6) 0.0283(7) 0.0411(8) -0.0064(6) -0.0068(6) 0.0056(6) C65 0.0276(7) 0.0252(7) 0.0368(8) -0.0001(6) -0.0082(6) 0.0099(6) C66 0.0386(8) 0.0197(7) 0.0379(8) 0.0086(6) 0.0033(7) 0.0107(6) C67 0.0387(8) 0.0155(6) 0.0480(9) 0.0097(6) 0.0062(7) 0.0031(6) C68 0.0381(8) 0.0115(6) 0.0531(10) 0.0067(6) 0.0027(7) 0.0017(6) C69 0.0318(8) 0.0101(6) 0.0596(10) -0.0020(6) 0.0058(7) -0.0034(6) C70 0.0265(7) 0.0096(6) 0.0638(11) -0.0083(6) -0.0016(7) -0.0025(5) C71 0.0314(7) 0.0128(6) 0.0487(9) -0.0099(6) 0.0015(7) 0.0025(6) C72 0.0281(7) 0.0199(6) 0.0423(8) -0.0118(6) -0.0022(6) 0.0026(6) C73 0.0295(7) 0.0240(7) 0.0359(8) -0.0113(6) 0.0012(6) 0.0032(6) C74 0.0226(7) 0.0259(7) 0.0415(8) -0.0100(6) 0.0033(6) 0.0044(6) C75 0.0225(7) 0.0200(7) 0.0501(9) -0.0084(6) 0.0015(6) 0.0087(6) C76 0.0274(7) 0.0141(6) 0.0507(9) -0.0058(6) 0.0023(7) 0.0071(6) C77 0.0328(7) 0.0126(6) 0.0505(9) 0.0023(6) -0.0002(7) 0.0091(6) C78 0.0281(7) 0.0196(6) 0.0467(9) 0.0026(6) -0.0043(7) 0.0114(6) C79 0.0213(6) 0.0239(7) 0.0453(9) -0.0035(6) -0.0007(6) 0.0115(6) C80 0.0332(8) 0.0230(7) 0.0400(8) 0.0046(6) -0.0068(7) 0.0115(6) C88 0.062(3) 0.044(2) 0.069(3) -0.014(2) -0.008(2) 0.007(2) C89 0.110(6) 0.170(9) 0.091(5) -0.030(6) -0.013(5) -0.020(6) C90 0.064(3) 0.061(3) 0.148(6) 0.045(3) -0.001(4) -0.019(3) C91 0.043(3) 0.066(3) 0.175(7) 0.027(4) 0.011(4) -0.005(3) C92 0.063(3) 0.039(2) 0.092(4) 0.005(2) 0.014(3) -0.008(2) C93 0.063(3) 0.0307(19) 0.074(3) -0.0046(19) -0.013(2) -0.0046(19) C94" 0.0409(19) 0.0127(14) 0.0262(17) -0.0048(12) 0.0088(15) -0.0159(14) C88' 0.048(2) 0.161(7) 0.038(2) -0.008(3) -0.0022(19) -0.008(3) C89' 0.0358(19) 0.0439(19) 0.043(2) 0.0250(16) 0.0074(16) 0.0082(17) C90' 0.072(3) 0.082(4) 0.073(3) 0.009(3) 0.008(3) 0.016(3) C91' 0.085(3) 0.061(3) 0.072(3) -0.001(3) -0.018(3) 0.002(3) C92' 0.080(3) 0.062(3) 0.070(3) -0.007(3) -0.004(3) -0.012(3) C93' 0.122(4) 0.120(4) 0.045(2) -0.029(2) 0.017(3) -0.086(3) C94' 0.0323(18) 0.044(2) 0.049(2) 0.0209(17) 0.0147(16) 0.0197(16) N1 0.0213(5) 0.0176(5) 0.0345(6) -0.0016(5) -0.0008(5) 0.0015(5) N2 0.0399(7) 0.0143(5) 0.0314(6) -0.0009(5) -0.0042(6) -0.0004(5) O1 0.0252(5) 0.0308(6) 0.0409(6) 0.0015(5) -0.0024(5) 0.0035(5) O2 0.0310(5) 0.0239(5) 0.0339(6) 0.0012(4) -0.0056(4) 0.0039(4) O3 0.0325(5) 0.0224(5) 0.0464(6) -0.0067(5) -0.0075(5) 0.0056(5) O4 0.0328(6) 0.0351(6) 0.0595(8) -0.0084(6) -0.0034(6) 0.0138(5) O5 0.0221(5) 0.0187(5) 0.0441(6) -0.0015(4) 0.0012(4) 0.0027(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.267(2) . ? C1 O2 1.4008(19) . ? C1 C2 1.467(2) . ? C2 C26 1.393(2) . ? C2 C3 1.431(2) . ? C3 C4 1.378(2) . ? C3 C6 1.531(2) . ? C4 N1 1.344(2) . ? C4 C5 1.474(2) . ? C5 O1 1.2005(19) . ? C5 O2 1.356(2) . ? C6 C29 1.525(2) . ? C6 C7 1.545(2) . ? C6 C30 1.5773(19) . ? C7 C8 1.401(2) . ? C7 C12 1.401(2) . ? C8 N1 1.3957(19) . ? C8 C9 1.396(2) . ? C9 C10 1.383(2) . ? C10 C11 1.399(2) . ? C11 C12 1.401(2) . ? C11 C13 1.539(2) . ? C13 C14 1.530(3) . ? C13 C16 1.530(3) . ? C13 C15 1.539(2) . ? C17 C22 1.399(2) . ? C17 C18 1.405(3) . ? C17 N2 1.411(2) . ? C18 C19 1.392(3) . ? C19 C20 1.379(3) . ? C20 C21 1.400(3) . ? C20 C23 1.541(2) . ? C21 C22 1.393(2) . ? C23 C24 1.522(4) . ? C23 C25 1.523(3) . ? C23 C27 1.523(3) . ? C26 C28 1.459(2) . ? C26 C40 1.474(2) . ? C28 C29 1.374(2) . ? C28 C42 1.436(2) . ? C29 C45 1.427(2) . ? C30 C31 1.384(2) . ? C30 C46 1.463(2) . ? C31 C49 1.454(2) . ? C31 C32 1.515(2) . ? C32 O5 1.2137(18) . ? C32 C33 1.519(2) . ? C33 C34 1.382(2) . ? C33 C50 1.435(2) . ? C34 C53 1.457(2) . ? C34 C35 1.500(3) . ? C35 O4 1.211(2) . ? C35 C36 1.517(2) . ? C36 C37 1.373(2) . ? C36 C54 1.443(2) . ? C37 C57 1.431(2) . ? C37 C38 1.520(2) . ? C38 O3 1.2106(19) . ? C38 C39 1.506(2) . ? C39 C40 1.404(2) . ? C39 C58 1.448(2) . ? C40 C41 1.468(2) . ? C41 C60 1.401(2) . ? C41 C42 1.427(2) . ? C42 C43 1.393(2) . ? C43 C44 1.434(2) . ? C43 C62 1.448(2) . ? C44 C45 1.404(2) . ? C44 C64 1.444(2) . ? C45 C46 1.449(2) . ? C46 C47 1.393(2) . ? C47 C48 1.424(2) . ? C47 C65 1.452(2) . ? C48 C49 1.389(2) . ? C48 C66 1.451(2) . ? C49 C50 1.437(2) . ? C50 C51 1.404(2) . ? C51 C52 1.430(3) . ? C51 C67 1.443(2) . ? C52 C53 1.391(2) . ? C52 C69 1.459(2) . ? C53 C54 1.445(3) . ? C54 C55 1.400(2) . ? C55 C56 1.435(2) . ? C55 C70 1.446(2) . ? C56 C57 1.392(2) . ? C56 C72 1.450(2) . ? C57 C58 1.448(2) . ? C58 C59 1.400(2) . ? C59 C60 1.438(2) . ? C59 C73 1.452(2) . ? C60 C61 1.442(2) . ? C61 C62 1.397(2) . ? C61 C74 1.454(2) . ? C62 C63 1.442(2) . ? C63 C79 1.398(2) . ? C63 C64 1.451(2) . ? C64 C65 1.392(2) . ? C65 C80 1.448(2) . ? C66 C67 1.394(2) . ? C66 C80 1.442(2) . ? C67 C68 1.450(3) . ? C68 C77 1.399(2) . ? C68 C69 1.455(3) . ? C69 C70 1.386(3) . ? C70 C71 1.458(2) . ? C71 C76 1.397(2) . ? C71 C72 1.450(2) . ? C72 C73 1.395(2) . ? C73 C74 1.453(2) . ? C74 C75 1.394(2) . ? C75 C79 1.444(2) . ? C75 C76 1.450(2) . ? C76 C77 1.452(3) . ? C77 C78 1.447(2) . ? C78 C80 1.397(2) . ? C78 C79 1.449(2) . ? C81 C82 1.3900 . ? C81 C86 1.3900 . ? C82 C83 1.3900 . ? C83 C84 1.3900 . ? C84 C85 1.3900 . ? C85 C86 1.3900 . ? C86 C87 1.462(6) . ? C81' C82' 1.3900 . ? C81' C86' 1.3900 . ? C82' C83' 1.3900 . ? C83' C84' 1.3900 . ? C84' C85' 1.3900 . ? C85' C86' 1.3900 . ? C86' C87' 1.454(11) . ? C88 C89 1.3900 . ? C88 C93 1.3900 . ? C89 C90 1.3900 . ? C90 C91 1.3900 . ? C91 C92 1.3900 . ? C92 C93 1.3900 . ? C92 C94 1.486(9) . ? C88' C89' 1.3900 . ? C88' C93' 1.3900 . ? C89' C90' 1.3900 . ? C90' C91' 1.3900 . ? C91' C92' 1.3900 . ? C92' C93' 1.3900 . ? C92' C94' 1.552(5) . ? C96 C97 1.3900 . ? C96 C101 1.3900 . ? C97 C98 1.3900 . ? C98 C99 1.3900 . ? C99 C100 1.3900 . ? C99 C95 1.483(15) . ? C100 C101 1.3900 . ? C96' C97' 1.3900 . ? C96' C11' 1.3900 . ? C97' C98' 1.3900 . ? C98' C99' 1.3900 . ? C98' C95' 1.508(11) . ? C99' C10' 1.3900 . ? C10' C11' 1.3900 . ? 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 N2 C1 O2 121.04(14) . . ? N2 C1 C2 122.06(14) . . ? O2 C1 C2 116.70(13) . . ? C26 C2 C3 119.92(13) . . ? C26 C2 C1 121.91(14) . . ? C3 C2 C1 117.64(13) . . ? C4 C3 C2 118.73(13) . . ? C4 C3 C6 117.38(13) . . ? C2 C3 C6 123.89(12) . . ? N1 C4 C3 122.75(13) . . ? N1 C4 C5 115.56(13) . . ? C3 C4 C5 121.61(14) . . ? O1 C5 O2 119.27(14) . . ? O1 C5 C4 124.10(15) . . ? O2 C5 C4 116.62(13) . . ? C29 C6 C3 109.84(12) . . ? C29 C6 C7 115.75(11) . . ? C3 C6 C7 107.68(11) . . ? C29 C6 C30 98.32(10) . . ? C3 C6 C30 121.75(11) . . ? C7 C6 C30 103.71(11) . . ? C8 C7 C12 118.21(13) . . ? C8 C7 C6 117.29(12) . . ? C12 C7 C6 124.09(13) . . ? N1 C8 C9 119.72(13) . . ? N1 C8 C7 119.55(13) . . ? C9 C8 C7 120.60(13) . . ? C10 C9 C8 119.70(14) . . ? C9 C10 C11 121.61(15) . . ? C10 C11 C12 117.65(14) . . ? C10 C11 C13 121.62(14) . . ? C12 C11 C13 120.69(13) . . ? C7 C12 C11 122.07(14) . . ? C14 C13 C16 109.36(15) . . ? C14 C13 C11 112.23(14) . . ? C16 C13 C11 107.96(14) . . ? C14 C13 C15 107.69(15) . . ? C16 C13 C15 108.33(14) . . ? C11 C13 C15 111.20(13) . . ? C22 C17 C18 117.95(15) . . ? C22 C17 N2 114.82(15) . . ? C18 C17 N2 127.20(15) . . ? C19 C18 C17 119.92(16) . . ? C20 C19 C18 122.44(18) . . ? C19 C20 C21 117.51(16) . . ? C19 C20 C23 121.99(17) . . ? C21 C20 C23 120.46(16) . . ? C22 C21 C20 121.10(16) . . ? C21 C22 C17 120.83(17) . . ? C24 C23 C25 110.2(2) . . ? C24 C23 C27 108.4(2) . . ? C25 C23 C27 108.35(19) . . ? C24 C23 C20 111.68(18) . . ? C25 C23 C20 108.23(15) . . ? C27 C23 C20 109.97(17) . . ? C2 C26 C28 116.98(14) . . ? C2 C26 C40 133.36(14) . . ? C28 C26 C40 106.63(12) . . ? C29 C28 C42 120.91(13) . . ? C29 C28 C26 123.54(13) . . ? C42 C28 C26 109.21(13) . . ? C28 C29 C45 117.61(13) . . ? C28 C29 C6 121.52(13) . . ? C45 C29 C6 110.22(12) . . ? C31 C30 C46 117.92(12) . . ? C31 C30 C6 134.61(13) . . ? C46 C30 C6 105.62(11) . . ? C30 C31 C49 118.76(13) . . ? C30 C31 C32 129.92(13) . . ? C49 C31 C32 106.28(12) . . ? O5 C32 C31 129.19(13) . . ? O5 C32 C33 125.72(14) . . ? C31 C32 C33 104.89(12) . . ? C34 C33 C50 119.55(14) . . ? C34 C33 C32 126.40(14) . . ? C50 C33 C32 107.36(13) . . ? C33 C34 C53 118.59(15) . . ? C33 C34 C35 127.86(14) . . ? C53 C34 C35 106.69(15) . . ? O4 C35 C34 128.55(17) . . ? O4 C35 C36 127.81(17) . . ? C34 C35 C36 103.64(13) . . ? C37 C36 C54 119.02(14) . . ? C37 C36 C35 126.51(14) . . ? C54 C36 C35 106.46(15) . . ? C36 C37 C57 119.93(14) . . ? C36 C37 C38 123.88(14) . . ? C57 C37 C38 107.50(13) . . ? O3 C38 C39 129.02(14) . . ? O3 C38 C37 124.67(15) . . ? C39 C38 C37 105.63(13) . . ? C40 C39 C58 119.57(14) . . ? C40 C39 C38 126.49(14) . . ? C58 C39 C38 106.59(13) . . ? C39 C40 C41 117.04(13) . . ? C39 C40 C26 128.97(14) . . ? C41 C40 C26 106.16(13) . . ? C60 C41 C42 118.62(14) . . ? C60 C41 C40 122.93(14) . . ? C42 C41 C40 109.45(13) . . ? C43 C42 C41 121.81(14) . . ? C43 C42 C28 120.50(14) . . ? C41 C42 C28 107.70(13) . . ? C42 C43 C44 118.99(13) . . ? C42 C43 C62 119.42(14) . . ? C44 C43 C62 108.56(14) . . ? C45 C44 C43 118.72(14) . . ? C45 C44 C64 120.63(14) . . ? C43 C44 C64 107.81(13) . . ? C44 C45 C29 121.74(14) . . ? C44 C45 C46 119.40(13) . . ? C29 C45 C46 107.39(12) . . ? C47 C46 C45 119.31(13) . . ? C47 C46 C30 122.52(13) . . ? C45 C46 C30 108.74(13) . . ? C46 C47 C48 119.25(14) . . ? C46 C47 C65 121.01(14) . . ? C48 C47 C65 108.07(13) . . ? C49 C48 C47 118.52(14) . . ? C49 C48 C66 120.52(15) . . ? C47 C48 C66 108.71(14) . . ? C48 C49 C50 119.46(14) . . ? C48 C49 C31 122.94(14) . . ? C50 C49 C31 109.77(13) . . ? C51 C50 C33 122.06(15) . . ? C51 C50 C49 120.32(14) . . ? C33 C50 C49 109.40(13) . . ? C50 C51 C52 118.00(15) . . ? C50 C51 C67 120.10(15) . . ? C52 C51 C67 109.10(14) . . ? C53 C52 C51 120.13(14) . . ? C53 C52 C69 119.84(17) . . ? C51 C52 C69 107.77(14) . . ? C52 C53 C54 120.59(15) . . ? C52 C53 C34 121.08(16) . . ? C54 C53 C34 108.28(14) . . ? C55 C54 C36 121.03(16) . . ? C55 C54 C53 119.37(15) . . ? C36 C54 C53 109.02(14) . . ? C54 C55 C56 119.04(14) . . ? C54 C55 C70 120.13(17) . . ? C56 C55 C70 108.63(14) . . ? C57 C56 C55 118.97(15) . . ? C57 C56 C72 120.40(14) . . ? C55 C56 C72 108.29(14) . . ? C56 C57 C37 121.40(15) . . ? C56 C57 C58 120.36(14) . . ? C37 C57 C58 109.17(14) . . ? C59 C58 C39 122.69(14) . . ? C59 C58 C57 119.38(14) . . ? C39 C58 C57 109.89(14) . . ? C58 C59 C60 118.48(14) . . ? C58 C59 C73 119.98(14) . . ? C60 C59 C73 108.17(14) . . ? C41 C60 C59 119.12(14) . . ? C41 C60 C61 120.40(15) . . ? C59 C60 C61 108.50(14) . . ? C62 C61 C60 120.33(14) . . ? C62 C61 C74 119.45(15) . . ? C60 C61 C74 107.85(13) . . ? C61 C62 C63 120.38(14) . . ? C61 C62 C43 119.28(14) . . ? C63 C62 C43 107.73(14) . . ? C79 C63 C62 119.95(15) . . ? C79 C63 C64 119.71(15) . . ? C62 C63 C64 107.81(14) . . ? C65 C64 C44 119.84(14) . . ? C65 C64 C63 120.15(14) . . ? C44 C64 C63 108.06(14) . . ? C64 C65 C80 120.03(15) . . ? C64 C65 C47 119.43(14) . . ? C80 C65 C47 107.60(14) . . ? C67 C66 C80 119.93(15) . . ? C67 C66 C48 119.95(15) . . ? C80 C66 C48 107.40(14) . . ? C66 C67 C51 119.50(14) . . ? C66 C67 C68 120.41(16) . . ? C51 C67 C68 107.69(15) . . ? C77 C68 C67 119.60(15) . . ? C77 C68 C69 119.76(17) . . ? C67 C68 C69 107.80(15) . . ? C70 C69 C68 120.49(15) . . ? C70 C69 C52 119.51(15) . . ? C68 C69 C52 107.60(16) . . ? C69 C70 C55 120.51(15) . . ? C69 C70 C71 119.94(16) . . ? C55 C70 C71 107.42(15) . . ? C76 C71 C72 120.03(14) . . ? C76 C71 C70 119.72(16) . . ? C72 C71 C70 107.97(14) . . ? C73 C72 C71 120.09(15) . . ? C73 C72 C56 119.31(14) . . ? C71 C72 C56 107.64(14) . . ? C72 C73 C59 120.40(14) . . ? C72 C73 C74 119.84(15) . . ? C59 C73 C74 107.67(13) . . ? C75 C74 C73 120.05(14) . . ? C75 C74 C61 120.12(15) . . ? C73 C74 C61 107.77(14) . . ? C74 C75 C79 119.99(14) . . ? C74 C75 C76 120.10(15) . . ? C79 C75 C76 107.90(15) . . ? C71 C76 C75 119.87(15) . . ? C71 C76 C77 120.31(15) . . ? C75 C76 C77 107.74(14) . . ? C68 C77 C78 119.80(16) . . ? C68 C77 C76 119.79(16) . . ? C78 C77 C76 108.30(14) . . ? C80 C78 C77 120.34(15) . . ? C80 C78 C79 119.73(14) . . ? C77 C78 C79 107.56(15) . . ? C63 C79 C75 120.06(15) . . ? C63 C79 C78 120.21(15) . . ? C75 C79 C78 108.51(14) . . ? C78 C80 C66 119.90(15) . . ? C78 C80 C65 120.13(15) . . ? C66 C80 C65 108.15(13) . . ? C82 C81 C86 120.0 . . ? C83 C82 C81 120.0 . . ? C82 C83 C84 120.0 . . ? C85 C84 C83 120.0 . . ? C86 C85 C84 120.0 . . ? C85 C86 C81 120.0 . . ? C85 C86 C87 116.0(3) . . ? C81 C86 C87 124.0(3) . . ? C82' C81' C86' 120.0 . . ? C83' C82' C81' 120.0 . . ? C84' C83' C82' 120.0 . . ? C83' C84' C85' 120.0 . . ? C84' C85' C86' 120.0 . . ? C85' C86' C81' 120.0 . . ? C85' C86' C87' 102.3(6) . . ? C81' C86' C87' 137.7(6) . . ? C89 C88 C93 120.0 . . ? C90 C89 C88 120.0 . . ? C91 C90 C89 120.0 . . ? C90 C91 C92 120.0 . . ? C91 C92 C93 120.0 . . ? C91 C92 C94 122.2(4) . . ? C93 C92 C94 117.3(4) . . ? C92 C93 C88 120.0 . . ? C89' C88' C93' 120.0 . . ? C88' C89' C90' 120.0 . . ? C91' C90' C89' 120.0 . . ? C92' C91' C90' 120.0 . . ? C91' C92' C93' 120.0 . . ? C91' C92' C94' 126.4(3) . . ? C93' C92' C94' 113.3(3) . . ? C92' C93' C88' 120.0 . . ? C97 C96 C101 120.0 . . ? C98 C97 C96 120.0 . . ? C97 C98 C99 120.0 . . ? C100 C99 C98 120.0 . . ? C100 C99 C95 121.1(11) . . ? C98 C99 C95 118.8(11) . . ? C99 C100 C101 120.0 . . ? C100 C101 C96 120.0 . . ? C97' C96' C11' 120.0 . . ? C96' C97' C98' 120.0 . . ? C99' C98' C97' 120.0 . . ? C99' C98' C95' 121.3(7) . . ? C97' C98' C95' 118.6(7) . . ? C98' C99' C10' 120.0 . . ? C11' C10' C99' 120.0 . . ? C10' C11' C96' 120.0 . . ? C4 N1 C8 119.75(12) . . ? C1 N2 C17 124.46(14) . . ? C5 O2 C1 122.30(12) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.37 _refine_diff_density_min -0.46 _refine_diff_density_rms 0.08 # Attachment 'sa1287.cif' data_sa1287 _database_code_depnum_ccdc_archive 'CCDC 854105' #TrackingRef 'sa1287.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C83.50 H31 Cl10.50 N2 O7.13' _chemical_formula_weight 1548.41 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.802(3) _cell_length_b 15.015(2) _cell_length_c 15.464(3) _cell_angle_alpha 75.086(6) _cell_angle_beta 88.761(7) _cell_angle_gamma 72.662(6) _cell_volume 3164.5(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1563 _exptl_absorpt_coefficient_mu 0.529 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8324 _exptl_absorpt_correction_T_max 0.8574 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24270 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0630 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 25.37 _reflns_number_total 11502 _reflns_number_gt 9743 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11502 _refine_ls_number_parameters 939 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1435 _refine_ls_R_factor_gt 0.1281 _refine_ls_wR_factor_ref 0.3325 _refine_ls_wR_factor_gt 0.3187 _refine_ls_goodness_of_fit_ref 1.947 _refine_ls_restrained_S_all 1.983 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.3400(2) 0.3210(2) 0.2157(2) 0.1044(10) Uani 1 1 d . . . Cl2 Cl 0.2444(2) 0.2359(2) 0.11201(15) 0.0911(9) Uani 1 1 d . . . Cl3 Cl 0.27829(15) 0.15854(14) 0.30271(13) 0.0606(6) Uani 1 1 d . . . Cl4 Cl 0.7697(3) 0.2510(5) 0.2344(4) 0.103(2) Uani 0.686(8) 1 d PDU A 1 Cl5 Cl 0.7377(4) 0.1750(3) 0.4142(3) 0.0996(18) Uani 0.686(8) 1 d PDU A 1 Cl4' Cl 0.7256(10) 0.3221(9) 0.1959(7) 0.100(4) Uani 0.314(8) 1 d PDU A 2 Cl5' Cl 0.7853(8) 0.1708(8) 0.3476(11) 0.126(5) Uani 0.314(8) 1 d PDU A 2 Cl6 Cl 0.58161(18) 0.2541(2) 0.28909(19) 0.0840(8) Uani 1 1 d . A . Cl7 Cl 0.1607(2) 0.5306(2) -0.0019(2) 0.1032(10) Uani 1 1 d . . . Cl8 Cl -0.02903(18) 0.65001(19) 0.01060(19) 0.0886(8) Uani 1 1 d . . . Cl9 Cl 0.06600(16) 0.49731(15) 0.16305(14) 0.0645(6) Uani 1 1 d . . . O1 O 0.1729(3) 0.3739(3) 0.3760(2) 0.0279(9) Uani 1 1 d . . . H1 H 0.1859 0.4264 0.3622 0.033 Uiso 1 1 d R . . O2 O 0.0042(3) 0.4441(3) 0.6263(3) 0.0284(9) Uani 1 1 d . . . H2 H 0.0182 0.4950 0.6239 0.034 Uiso 1 1 d R . . O3 O 0.3815(3) 0.4788(3) 0.4771(3) 0.0347(10) Uani 1 1 d . . . O4 O 0.2412(3) 0.5434(3) 0.6939(3) 0.0426(11) Uani 1 1 d . . . O5 O 0.4280(3) 0.5454(3) 0.6295(3) 0.0393(11) Uani 1 1 d . . . O6 O 0.1550(3) 0.6468(3) 0.5157(3) 0.0374(10) Uani 1 1 d . . . O7 O 0.2467(3) 0.6860(3) 0.4084(3) 0.0477(12) Uani 1 1 d . . . N1 N 0.0485(3) 0.6064(3) 0.6183(3) 0.0287(11) Uani 1 1 d . . . N2 N 0.2124(3) 0.5384(3) 0.3332(3) 0.0277(11) Uani 1 1 d . . . C1 C 0.2154(4) 0.3621(4) 0.4624(4) 0.0253(12) Uani 1 1 d . . . C2 C 0.1057(4) 0.4088(4) 0.6253(4) 0.0244(12) Uani 1 1 d . . . C4 C 0.2612(4) 0.4667(4) 0.7505(4) 0.0283(13) Uani 1 1 d . . . C5 C 0.4614(4) 0.4605(5) 0.6712(4) 0.0322(13) Uani 1 1 d . . . C6 C 0.1917(4) 0.4616(4) 0.4840(3) 0.0243(12) Uani 1 1 d . . . C7 C 0.1437(4) 0.4799(4) 0.5564(4) 0.0243(12) Uani 1 1 d . . . C8 C 0.1105(4) 0.5821(4) 0.5645(4) 0.0299(13) Uani 1 1 d . . . C9 C 0.2036(4) 0.6296(4) 0.4426(4) 0.0245(12) Uani 1 1 d . . . C10 C 0.2033(4) 0.5432(4) 0.4154(4) 0.0291(13) Uani 1 1 d . . . C11 C 0.6110(4) 0.1307(4) 0.7930(4) 0.0345(14) Uani 1 1 d . . . C12 C 0.4816(4) 0.0018(4) 0.6487(4) 0.0357(14) Uani 1 1 d . . . C13 C 0.4896(4) 0.0206(4) 0.8735(4) 0.0333(14) Uani 1 1 d . . . C14 C 0.3190(4) 0.0701(4) 0.8908(4) 0.0336(14) Uani 1 1 d . . . C15 C 0.4982(5) 0.0961(5) 0.9067(4) 0.0364(15) Uani 1 1 d . . . C16 C 0.3468(4) 0.3368(4) 0.8698(4) 0.0314(13) Uani 1 1 d . . . C17 C 0.3278(4) 0.1486(4) 0.9239(4) 0.0324(14) Uani 1 1 d . . . C18 C 0.3922(5) 0.0371(4) 0.5940(4) 0.0324(14) Uani 1 1 d . . . C19 C 0.5412(4) 0.0601(4) 0.6076(4) 0.0323(13) Uani 1 1 d . . . C20 C 0.3089(4) 0.0077(4) 0.7332(4) 0.0329(14) Uani 1 1 d . . . C21 C 0.5272(4) 0.3798(4) 0.6393(4) 0.0327(13) Uani 1 1 d . . . C22 C 0.4264(4) 0.2559(5) 0.9083(4) 0.0331(14) Uani 1 1 d . . . C23 C 0.5424(4) -0.0004(4) 0.7958(4) 0.0342(14) Uani 1 1 d . . . C24 C 0.5738(4) 0.3071(4) 0.7187(4) 0.0309(13) Uani 1 1 d . . . C25 C 0.5999(4) 0.0854(4) 0.6598(4) 0.0347(14) Uani 1 1 d . . . C26 C 0.3569(4) 0.4179(4) 0.8026(4) 0.0299(13) Uani 1 1 d . . . C27 C 0.2299(4) 0.1035(4) 0.8363(4) 0.0323(14) Uani 1 1 d . . . C28 C 0.5160(4) 0.2509(4) 0.8667(4) 0.0306(13) Uani 1 1 d . . . C29 C 0.3986(4) 0.0069(4) 0.8657(4) 0.0326(14) Uani 1 1 d . . . C30 C 0.4833(5) -0.0275(4) 0.7420(4) 0.0342(14) Uani 1 1 d . . . C31 C 0.6007(4) 0.0538(4) 0.7574(4) 0.0360(14) Uani 1 1 d . . . C32 C 0.2461(4) 0.2324(4) 0.8876(4) 0.0295(13) Uani 1 1 d . . . C33 C 0.1484(4) 0.3685(4) 0.7262(4) 0.0262(12) Uani 1 1 d . . . C34 C 0.3088(4) 0.0372(4) 0.6367(4) 0.0328(14) Uani 1 1 d . . . C35 C 0.6084(4) 0.1816(4) 0.6375(4) 0.0299(13) Uani 1 1 d . . . C36 C 0.3928(5) -0.0240(4) 0.7859(5) 0.0406(16) Uani 1 1 d . . . C37 C 0.5220(4) 0.3272(4) 0.7963(4) 0.0332(14) Uani 1 1 d . . . C38 C 0.4165(4) 0.1606(4) 0.9338(4) 0.0329(14) Uani 1 1 d . . . C39 C 0.4871(4) 0.1326(4) 0.5296(4) 0.0289(13) Uani 1 1 d . . . C40 C 0.4911(4) 0.2274(4) 0.5095(4) 0.0280(12) Uani 1 1 d . . . C41 C 0.1295(4) 0.2375(4) 0.6786(4) 0.0292(13) Uani 1 1 d . . . C42 C 0.2286(4) 0.1959(4) 0.5327(3) 0.0251(12) Uani 1 1 d . . . C43 C 0.1863(4) 0.2054(4) 0.8342(4) 0.0332(14) Uani 1 1 d . . . C44 C 0.5166(4) 0.3520(4) 0.5641(4) 0.0265(12) Uani 1 1 d . . . C45 C 0.2568(4) 0.3233(4) 0.8586(4) 0.0310(13) Uani 1 1 d . . . C46 C 0.6162(4) 0.2098(4) 0.7176(4) 0.0328(14) Uani 1 1 d . . . C47 C 0.2239(4) 0.0722(4) 0.7603(4) 0.0314(13) Uani 1 1 d . . . C48 C 0.3979(4) 0.1175(4) 0.5220(4) 0.0320(13) Uani 1 1 d . . . C49 C 0.5541(4) 0.2524(4) 0.5621(4) 0.0285(13) Uani 1 1 d . . . C3 C 0.4286(4) 0.3959(4) 0.4991(4) 0.0269(12) Uani 1 1 d . . . C51 C 0.1757(4) 0.2944(4) 0.5289(4) 0.0270(12) Uani 1 1 d . . . C52 C 0.1394(4) 0.2709(4) 0.7559(4) 0.0307(13) Uani 1 1 d . . . C53 C 0.4441(4) 0.4140(4) 0.7653(4) 0.0324(13) Uani 1 1 d . . . C54 C 0.1731(4) 0.1407(4) 0.6802(4) 0.0289(13) Uani 1 1 d . . . C55 C 0.2243(4) 0.1196(4) 0.6030(4) 0.0295(13) Uani 1 1 d . . . C56 C 0.3164(4) 0.1979(4) 0.4925(4) 0.0289(13) Uani 1 1 d . . . C57 C 0.4077(4) 0.3109(4) 0.4768(3) 0.0267(12) Uani 1 1 d . . . C58 C 0.2068(4) 0.3935(4) 0.7775(4) 0.0267(12) Uani 1 1 d . . . C59 C 0.5614(4) 0.1517(4) 0.8663(4) 0.0327(14) Uani 1 1 d . . . C50 C 0.3213(4) 0.2964(4) 0.4671(3) 0.0254(12) Uani 1 1 d . . . C60 C 0.1264(4) 0.3146(4) 0.6008(4) 0.0263(12) Uani 1 1 d . . . C61 C 0.0175(4) 0.7025(4) 0.6293(4) 0.0310(13) Uani 1 1 d . . . C62 C 0.0099(5) 0.7088(4) 0.7181(4) 0.0369(14) Uani 1 1 d . . . H62A H 0.0256 0.6519 0.7664 0.044 Uiso 1 1 calc R . . C63 C -0.0212(5) 0.8004(5) 0.7345(4) 0.0397(15) Uani 1 1 d . . . H63A H -0.0241 0.8050 0.7947 0.048 Uiso 1 1 calc R . . C64 C -0.0482(4) 0.8856(4) 0.6645(4) 0.0340(14) Uani 1 1 d . . . C65 C -0.0412(4) 0.8744(4) 0.5777(4) 0.0343(14) Uani 1 1 d . . . H65A H -0.0593 0.9303 0.5285 0.041 Uiso 1 1 calc R . . C66 C -0.0087(4) 0.7843(4) 0.5607(4) 0.0315(13) Uani 1 1 d . . . H66A H -0.0048 0.7797 0.5005 0.038 Uiso 1 1 calc R . . C67 C -0.0806(5) 0.9874(5) 0.6811(5) 0.0398(15) Uani 1 1 d . . . C68 C 0.0083(5) 1.0182(5) 0.6907(5) 0.0519(19) Uani 1 1 d . . . H68A H 0.0424 1.0197 0.6356 0.078 Uiso 1 1 calc R . . H68B H 0.0497 0.9719 0.7414 0.078 Uiso 1 1 calc R . . H68C H -0.0107 1.0828 0.7012 0.078 Uiso 1 1 calc R . . C69 C -0.1330(6) 0.9848(5) 0.7696(5) 0.0505(19) Uani 1 1 d . . . H69A H -0.1897 0.9650 0.7647 0.076 Uiso 1 1 calc R . . H69B H -0.1516 1.0492 0.7802 0.076 Uiso 1 1 calc R . . H69C H -0.0907 0.9384 0.8198 0.076 Uiso 1 1 calc R . . C70 C -0.1443(6) 1.0605(5) 0.6043(5) 0.0537(19) Uani 1 1 d . . . H70A H -0.2011 1.0416 0.5975 0.080 Uiso 1 1 calc R . . H70B H -0.1104 1.0633 0.5490 0.080 Uiso 1 1 calc R . . H70C H -0.1628 1.1243 0.6164 0.080 Uiso 1 1 calc R . . C71 C 0.2072(4) 0.6172(4) 0.2603(4) 0.0292(13) Uani 1 1 d . . . C72 C 0.1297(5) 0.7016(4) 0.2413(4) 0.0364(14) Uani 1 1 d . . . H72A H 0.0821 0.7091 0.2834 0.044 Uiso 1 1 calc R . . C73 C 0.1207(5) 0.7740(4) 0.1632(4) 0.0370(14) Uani 1 1 d . . . H73A H 0.0670 0.8301 0.1523 0.044 Uiso 1 1 calc R . . C74 C 0.1907(4) 0.7659(4) 0.0987(4) 0.0343(14) Uani 1 1 d . . . C75 C 0.2666(4) 0.6817(4) 0.1176(4) 0.0340(14) Uani 1 1 d . . . H75A H 0.3152 0.6752 0.0764 0.041 Uiso 1 1 calc R . . C76 C 0.2745(4) 0.6063(4) 0.1947(4) 0.0315(13) Uani 1 1 d . . . H76A H 0.3250 0.5478 0.2030 0.038 Uiso 1 1 calc R . . C77 C 0.1769(5) 0.8435(4) 0.0102(4) 0.0388(15) Uani 1 1 d . . . C78 C 0.0966(6) 0.8378(6) -0.0460(5) 0.062(2) Uani 1 1 d . . . H78A H 0.0390 0.8458 -0.0125 0.093 Uiso 1 1 calc R . . H78B H 0.1143 0.7747 -0.0594 0.093 Uiso 1 1 calc R . . H78C H 0.0849 0.8892 -0.1021 0.093 Uiso 1 1 calc R . . C79 C 0.1477(7) 0.9463(5) 0.0262(5) 0.060(2) Uani 1 1 d . . . H79A H 0.0899 0.9558 0.0593 0.090 Uiso 1 1 calc R . . H79B H 0.1358 0.9951 -0.0317 0.090 Uiso 1 1 calc R . . H79C H 0.1988 0.9527 0.0609 0.090 Uiso 1 1 calc R . . C80 C 0.2662(5) 0.8320(5) -0.0421(5) 0.0498(18) Uani 1 1 d . . . H80A H 0.2856 0.7681 -0.0538 0.075 Uiso 1 1 calc R . . H80B H 0.3172 0.8383 -0.0069 0.075 Uiso 1 1 calc R . . H80C H 0.2534 0.8821 -0.0991 0.075 Uiso 1 1 calc R . . C81 C 0.2545(6) 0.2623(6) 0.2151(5) 0.056(2) Uani 1 1 d . . . H81A H 0.1920 0.3069 0.2243 0.067 Uiso 1 1 calc R . . C82 C 0.6883(6) 0.2709(6) 0.3110(5) 0.060(2) Uani 1 1 d D . . H82A H 0.6780 0.3363 0.3211 0.071 Uiso 1 1 calc R A 1 C83 C 0.0812(5) 0.5830(5) 0.0687(5) 0.0498(18) Uani 1 1 d . . . H83A H 0.1076 0.6287 0.0893 0.060 Uiso 1 1 calc R . . O1W O 0.373(2) 0.225(2) 0.7087(19) 0.028(10) Uiso 0.132(14) 1 d P . . Cl12 Cl 0.6082 0.4372 1.0632(15) 0.342(10) Uiso 0.50 1 d P . . Cl11 Cl 0.5093 0.6182 -0.0404 0.212(5) Uiso 0.50 1 d P . . Cl10 Cl 0.3834 0.4969 0.0025 0.239(6) Uiso 0.50 1 d P . . C84 C 0.5000 0.5000 0.0000 0.40(3) Uiso 1 2 d S . . 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 Cl1 0.105(2) 0.121(2) 0.119(2) -0.046(2) 0.0354(18) -0.071(2) Cl2 0.119(2) 0.0944(18) 0.0472(12) -0.0171(12) -0.0206(13) -0.0127(17) Cl3 0.0685(13) 0.0556(12) 0.0501(11) -0.0191(9) -0.0110(9) -0.0024(10) Cl4 0.078(3) 0.151(5) 0.106(4) -0.079(4) 0.045(2) -0.039(3) Cl5 0.103(3) 0.099(3) 0.075(3) -0.004(2) -0.022(2) -0.013(2) Cl4' 0.133(8) 0.101(7) 0.098(6) -0.072(5) 0.031(5) -0.045(6) Cl5' 0.095(7) 0.102(6) 0.167(10) -0.012(6) -0.014(6) -0.027(5) Cl6 0.0593(14) 0.0998(19) 0.110(2) -0.0483(16) 0.0014(13) -0.0313(13) Cl7 0.121(2) 0.106(2) 0.106(2) -0.0547(18) 0.0556(19) -0.0493(19) Cl8 0.0681(15) 0.0887(18) 0.0983(19) 0.0090(15) -0.0271(13) -0.0343(14) Cl9 0.0730(14) 0.0628(13) 0.0585(12) -0.0087(10) 0.0007(10) -0.0278(11) O1 0.034(2) 0.026(2) 0.024(2) -0.0062(16) -0.0043(16) -0.0101(18) O2 0.0188(19) 0.029(2) 0.039(2) -0.0081(17) 0.0008(16) -0.0096(17) O3 0.029(2) 0.026(2) 0.048(3) -0.0029(19) -0.0057(19) -0.0123(19) O4 0.038(3) 0.034(2) 0.052(3) 0.005(2) -0.013(2) -0.019(2) O5 0.039(2) 0.025(2) 0.047(3) -0.004(2) 0.004(2) -0.0039(19) O6 0.042(3) 0.027(2) 0.042(2) -0.0048(19) 0.010(2) -0.013(2) O7 0.046(3) 0.042(3) 0.052(3) -0.010(2) 0.007(2) -0.012(2) N1 0.028(3) 0.025(2) 0.030(3) -0.005(2) -0.001(2) -0.005(2) N2 0.030(3) 0.023(2) 0.027(3) -0.002(2) -0.004(2) -0.007(2) C1 0.029(3) 0.022(3) 0.023(3) 0.000(2) -0.009(2) -0.008(2) C2 0.017(3) 0.022(3) 0.033(3) -0.006(2) -0.003(2) -0.005(2) C4 0.025(3) 0.034(3) 0.031(3) -0.014(3) 0.003(2) -0.012(3) C5 0.022(3) 0.041(4) 0.037(3) -0.008(3) 0.001(2) -0.017(3) C6 0.024(3) 0.025(3) 0.023(3) -0.004(2) -0.004(2) -0.008(2) C7 0.024(3) 0.021(3) 0.026(3) -0.003(2) -0.001(2) -0.006(2) C8 0.036(3) 0.032(3) 0.020(3) 0.001(2) -0.003(2) -0.014(3) C9 0.022(3) 0.020(3) 0.028(3) 0.001(2) 0.004(2) -0.009(2) C10 0.026(3) 0.029(3) 0.029(3) -0.001(2) -0.008(2) -0.010(2) C11 0.023(3) 0.029(3) 0.040(4) 0.004(3) -0.012(3) -0.002(3) C12 0.036(3) 0.017(3) 0.051(4) -0.009(3) -0.002(3) -0.004(3) C13 0.033(3) 0.027(3) 0.027(3) 0.008(2) -0.011(2) -0.001(3) C14 0.040(3) 0.030(3) 0.025(3) 0.010(3) -0.002(3) -0.017(3) C15 0.037(3) 0.039(3) 0.025(3) 0.007(3) -0.013(3) -0.011(3) C16 0.035(3) 0.036(3) 0.025(3) -0.008(3) -0.001(2) -0.013(3) C17 0.043(4) 0.038(3) 0.016(3) -0.006(2) 0.009(2) -0.013(3) C18 0.041(4) 0.022(3) 0.030(3) -0.005(2) -0.005(3) -0.004(3) C19 0.030(3) 0.028(3) 0.034(3) -0.009(3) 0.004(3) -0.001(3) C20 0.039(3) 0.020(3) 0.037(3) 0.002(2) -0.009(3) -0.013(3) C21 0.022(3) 0.028(3) 0.048(4) -0.008(3) 0.003(3) -0.010(2) C22 0.039(3) 0.044(4) 0.022(3) -0.010(3) -0.002(2) -0.019(3) C23 0.031(3) 0.025(3) 0.037(3) 0.007(3) -0.008(3) -0.008(3) C24 0.024(3) 0.034(3) 0.034(3) -0.003(3) -0.004(2) -0.013(3) C25 0.033(3) 0.024(3) 0.040(3) -0.003(3) -0.005(3) -0.002(3) C26 0.038(3) 0.028(3) 0.023(3) -0.007(2) -0.001(2) -0.009(3) C27 0.035(3) 0.026(3) 0.030(3) 0.008(2) -0.001(3) -0.016(3) C28 0.033(3) 0.034(3) 0.026(3) -0.005(3) -0.007(2) -0.014(3) C29 0.041(3) 0.026(3) 0.021(3) 0.014(2) 0.003(2) -0.014(3) C30 0.039(4) 0.018(3) 0.038(3) 0.002(2) -0.001(3) -0.006(3) C31 0.027(3) 0.031(3) 0.041(4) 0.001(3) -0.009(3) -0.004(3) C32 0.030(3) 0.035(3) 0.020(3) -0.002(2) 0.004(2) -0.009(3) C33 0.025(3) 0.027(3) 0.022(3) -0.002(2) 0.004(2) -0.006(2) C34 0.040(4) 0.020(3) 0.037(3) -0.007(3) -0.008(3) -0.007(3) C35 0.022(3) 0.029(3) 0.036(3) -0.005(3) 0.004(2) -0.008(2) C36 0.043(4) 0.025(3) 0.050(4) -0.005(3) -0.010(3) -0.007(3) C37 0.031(3) 0.033(3) 0.034(3) -0.004(3) -0.010(3) -0.011(3) C38 0.036(3) 0.036(3) 0.021(3) 0.001(2) -0.004(2) -0.009(3) C39 0.034(3) 0.027(3) 0.026(3) -0.009(2) 0.000(2) -0.008(3) C40 0.021(3) 0.031(3) 0.027(3) -0.005(2) 0.006(2) -0.003(2) C41 0.024(3) 0.032(3) 0.031(3) -0.002(2) -0.001(2) -0.012(3) C42 0.033(3) 0.023(3) 0.019(3) -0.002(2) -0.005(2) -0.010(2) C43 0.031(3) 0.039(3) 0.028(3) 0.002(3) 0.001(2) -0.017(3) C44 0.023(3) 0.030(3) 0.025(3) 0.001(2) 0.006(2) -0.012(2) C45 0.035(3) 0.036(3) 0.026(3) -0.012(3) -0.001(2) -0.013(3) C46 0.020(3) 0.035(3) 0.038(3) -0.003(3) -0.006(2) -0.004(3) C47 0.031(3) 0.029(3) 0.033(3) 0.002(2) 0.000(2) -0.015(3) C48 0.041(4) 0.024(3) 0.029(3) -0.010(2) -0.001(3) -0.005(3) C49 0.029(3) 0.029(3) 0.022(3) 0.005(2) 0.005(2) -0.011(3) C3 0.030(3) 0.027(3) 0.022(3) 0.003(2) 0.008(2) -0.014(3) C51 0.029(3) 0.024(3) 0.027(3) -0.004(2) -0.009(2) -0.008(2) C52 0.023(3) 0.034(3) 0.034(3) -0.006(3) -0.001(2) -0.010(3) C53 0.029(3) 0.033(3) 0.034(3) -0.009(3) -0.005(2) -0.007(3) C54 0.025(3) 0.026(3) 0.036(3) -0.003(2) -0.002(2) -0.013(2) C55 0.041(3) 0.024(3) 0.029(3) -0.004(2) -0.003(3) -0.021(3) C56 0.034(3) 0.025(3) 0.030(3) -0.012(2) -0.002(2) -0.008(3) C57 0.034(3) 0.028(3) 0.016(3) -0.002(2) 0.005(2) -0.011(3) C58 0.023(3) 0.026(3) 0.026(3) -0.005(2) 0.004(2) -0.002(2) C59 0.029(3) 0.028(3) 0.035(3) 0.001(3) -0.014(3) -0.006(3) C50 0.033(3) 0.019(3) 0.020(3) -0.004(2) 0.003(2) -0.004(2) C60 0.022(3) 0.021(3) 0.034(3) -0.004(2) -0.004(2) -0.007(2) C61 0.021(3) 0.029(3) 0.044(4) -0.008(3) -0.006(2) -0.009(2) C62 0.038(4) 0.032(3) 0.038(3) -0.003(3) 0.001(3) -0.010(3) C63 0.040(4) 0.039(4) 0.043(4) -0.016(3) 0.005(3) -0.011(3) C64 0.023(3) 0.035(3) 0.049(4) -0.018(3) 0.004(3) -0.010(3) C65 0.035(3) 0.025(3) 0.037(3) -0.003(3) 0.002(3) -0.006(3) C66 0.038(3) 0.028(3) 0.025(3) -0.005(2) -0.001(2) -0.007(3) C67 0.035(4) 0.036(4) 0.053(4) -0.020(3) 0.008(3) -0.012(3) C68 0.054(5) 0.051(4) 0.065(5) -0.026(4) 0.009(4) -0.029(4) C69 0.061(5) 0.040(4) 0.058(5) -0.027(3) 0.022(4) -0.016(4) C70 0.061(5) 0.029(4) 0.061(5) -0.007(3) 0.003(4) -0.003(3) C71 0.036(3) 0.025(3) 0.027(3) -0.002(2) -0.011(2) -0.012(3) C72 0.035(3) 0.034(3) 0.038(3) -0.004(3) 0.002(3) -0.011(3) C73 0.040(4) 0.027(3) 0.037(3) -0.004(3) -0.003(3) -0.004(3) C74 0.039(3) 0.035(3) 0.030(3) -0.002(3) -0.012(3) -0.018(3) C75 0.035(3) 0.040(3) 0.030(3) -0.005(3) 0.002(3) -0.019(3) C76 0.033(3) 0.034(3) 0.021(3) 0.005(2) -0.004(2) -0.011(3) C77 0.044(4) 0.032(3) 0.039(4) 0.001(3) -0.005(3) -0.016(3) C78 0.076(6) 0.069(5) 0.033(4) 0.016(4) -0.012(4) -0.034(5) C79 0.083(6) 0.033(4) 0.058(5) -0.003(3) 0.015(4) -0.016(4) C80 0.058(5) 0.046(4) 0.037(4) 0.004(3) -0.004(3) -0.016(4) C81 0.054(5) 0.055(5) 0.058(5) -0.019(4) 0.002(4) -0.011(4) C82 0.056(5) 0.063(5) 0.070(5) -0.031(4) 0.008(4) -0.022(4) C83 0.053(4) 0.052(4) 0.051(4) -0.014(4) 0.000(3) -0.024(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 C81 1.746(9) . ? Cl2 C81 1.757(8) . ? Cl3 C81 1.730(8) . ? Cl4 C82 1.688(8) . ? Cl5 C82 1.843(8) . ? Cl4' C82 1.890(11) . ? Cl5' C82 1.719(11) . ? Cl6 C82 1.725(8) . ? Cl7 C83 1.741(8) . ? Cl8 C83 1.761(8) . ? Cl9 C83 1.740(7) . ? O1 C1 1.436(6) . ? O1 H1 0.8403 . ? O2 C2 1.437(6) . ? O2 H2 0.8407 . ? O3 C3 1.195(7) . ? O4 C4 1.212(7) . ? O5 C5 1.225(7) . ? O6 C9 1.365(7) . ? O6 C8 1.389(7) . ? O7 C9 1.217(7) . ? N1 C8 1.261(7) . ? N1 C61 1.432(7) . ? N2 C10 1.294(7) . ? N2 C71 1.392(7) . ? C1 C51 1.493(8) . ? C1 C6 1.550(7) . ? C1 C50 1.575(8) . ? C2 C60 1.499(7) . ? C2 C7 1.529(8) . ? C2 C33 1.591(7) . ? C2 H2 1.5310 . ? C4 C58 1.519(8) . ? C4 C26 1.522(8) . ? C5 C53 1.495(9) . ? C5 C21 1.498(9) . ? C6 C7 1.356(8) . ? C6 C10 1.451(8) . ? C7 C8 1.502(8) . ? C9 C10 1.464(8) . ? C11 C59 1.390(9) . ? C11 C31 1.448(9) . ? C11 C46 1.454(8) . ? C12 C30 1.394(9) . ? C12 C19 1.449(9) . ? C12 C18 1.464(9) . ? C13 C15 1.398(9) . ? C13 C29 1.434(9) . ? C13 C23 1.470(9) . ? C14 C29 1.394(9) . ? C14 C17 1.441(8) . ? C14 C27 1.462(8) . ? C15 C38 1.437(9) . ? C15 C59 1.460(9) . ? C16 C22 1.423(9) . ? C16 C26 1.427(8) . ? C16 C45 1.427(8) . ? C17 C38 1.393(9) . ? C17 C32 1.456(8) . ? C18 C34 1.387(9) . ? C18 C48 1.439(8) . ? C19 C25 1.392(9) . ? C19 C39 1.458(8) . ? C20 C36 1.387(9) . ? C20 C34 1.443(8) . ? C20 C47 1.469(9) . ? C21 C44 1.360(8) . ? C21 C24 1.440(8) . ? C22 C38 1.434(8) . ? C22 C28 1.451(9) . ? C23 C31 1.382(9) . ? C23 C30 1.429(9) . ? C24 C46 1.411(8) . ? C24 C37 1.459(9) . ? C25 C35 1.440(8) . ? C25 C31 1.459(9) . ? C26 C53 1.394(8) . ? C27 C47 1.387(9) . ? C27 C43 1.464(9) . ? C28 C37 1.386(8) . ? C28 C59 1.442(8) . ? C29 C36 1.438(9) . ? C30 C36 1.481(9) . ? C32 C45 1.378(8) . ? C32 C43 1.431(8) . ? C33 C58 1.376(8) . ? C33 C52 1.464(8) . ? C34 C55 1.463(8) . ? C35 C49 1.425(8) . ? C35 C46 1.425(9) . ? C37 C53 1.437(8) . ? C39 C40 1.395(8) . ? C39 C48 1.418(8) . ? C40 C49 1.439(8) . ? C40 C57 1.460(8) . ? C41 C54 1.398(8) . ? C41 C60 1.429(8) . ? C41 C52 1.435(8) . ? C42 C55 1.377(8) . ? C42 C56 1.434(8) . ? C42 C51 1.440(8) . ? C43 C52 1.390(8) . ? C44 C49 1.441(8) . ? C44 C3 1.531(8) . ? C45 C58 1.458(8) . ? C47 C54 1.444(8) . ? C48 C56 1.410(8) . ? C3 C57 1.520(8) . ? C51 C60 1.367(8) . ? C54 C55 1.453(8) . ? C56 C50 1.453(8) . ? C57 C50 1.378(8) . ? C61 C66 1.360(8) . ? C61 C62 1.400(9) . ? C62 C63 1.403(9) . ? C62 H62A 0.9500 . ? C63 C64 1.403(9) . ? C63 H63A 0.9500 . ? C64 C65 1.393(9) . ? C64 C67 1.546(8) . ? C65 C66 1.385(8) . ? C65 H65A 0.9500 . ? C66 H66A 0.9500 . ? C67 C70 1.505(10) . ? C67 C68 1.541(9) . ? C67 C69 1.556(9) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 C72 1.401(8) . ? C71 C76 1.412(8) . ? C72 C73 1.380(8) . ? C72 H72A 0.9500 . ? C73 C74 1.424(9) . ? C73 H73A 0.9500 . ? C74 C75 1.387(9) . ? C74 C77 1.524(8) . ? C75 C76 1.397(8) . ? C75 H75A 0.9500 . ? C76 H76A 0.9500 . ? C77 C80 1.523(10) . ? C77 C78 1.523(10) . ? C77 C79 1.556(9) . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 H81A 1.0000 . ? C82 H82A 1.0000 . ? C83 H83A 1.0000 . ? Cl12 Cl10 1.255(14) 2_666 ? Cl12 C84 1.761(10) 1_556 ? Cl12 Cl11 2.210(6) 2_666 ? Cl11 C84 1.7699(2) . ? Cl11 Cl10 1.9327(3) 2_665 ? Cl11 Cl12 2.210(6) 2_666 ? Cl10 Cl12 1.255(14) 2_666 ? Cl10 C84 1.7390(3) . ? Cl10 Cl11 1.9327(3) 2_665 ? C84 Cl10 1.7390(3) 2_665 ? C84 Cl12 1.761(10) 2_666 ? C84 Cl12 1.761(10) 1_554 ? C84 Cl11 1.7699(2) 2_665 ? 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 C1 O1 H1 84.4 . . ? C2 O2 H2 79.8 . . ? C9 O6 C8 120.9(4) . . ? C8 N1 C61 122.1(5) . . ? C10 N2 C71 124.4(5) . . ? O1 C1 C51 106.9(4) . . ? O1 C1 C6 109.8(4) . . ? C51 C1 C6 111.0(5) . . ? O1 C1 C50 107.9(4) . . ? C51 C1 C50 99.6(4) . . ? C6 C1 C50 120.7(4) . . ? O2 C2 C60 105.6(4) . . ? O2 C2 C7 111.1(4) . . ? C60 C2 C7 110.5(5) . . ? O2 C2 C33 108.2(4) . . ? C60 C2 C33 98.8(4) . . ? C7 C2 C33 121.0(4) . . ? O2 C2 H2 32.7 . . ? C60 C2 H2 136.5 . . ? C7 C2 H2 86.3 . . ? C33 C2 H2 106.1 . . ? O4 C4 C58 130.2(5) . . ? O4 C4 C26 124.5(5) . . ? C58 C4 C26 104.9(5) . . ? O5 C5 C53 127.6(6) . . ? O5 C5 C21 127.9(6) . . ? C53 C5 C21 104.5(5) . . ? C7 C6 C10 117.8(5) . . ? C7 C6 C1 122.5(5) . . ? C10 C6 C1 118.4(5) . . ? C6 C7 C8 118.9(5) . . ? C6 C7 C2 125.9(5) . . ? C8 C7 C2 114.6(5) . . ? N1 C8 O6 121.2(5) . . ? N1 C8 C7 120.8(5) . . ? O6 C8 C7 117.8(5) . . ? O7 C9 O6 116.3(5) . . ? O7 C9 C10 126.0(5) . . ? O6 C9 C10 117.6(5) . . ? N2 C10 C6 120.0(5) . . ? N2 C10 C9 122.1(5) . . ? C6 C10 C9 117.9(5) . . ? C59 C11 C31 120.3(6) . . ? C59 C11 C46 119.2(5) . . ? C31 C11 C46 107.7(5) . . ? C30 C12 C19 118.6(6) . . ? C30 C12 C18 121.2(6) . . ? C19 C12 C18 107.7(5) . . ? C15 C13 C29 120.1(6) . . ? C15 C13 C23 119.5(6) . . ? C29 C13 C23 108.2(5) . . ? C29 C14 C17 120.4(6) . . ? C29 C14 C27 119.7(6) . . ? C17 C14 C27 108.3(5) . . ? C13 C15 C38 120.6(6) . . ? C13 C15 C59 120.2(6) . . ? C38 C15 C59 108.3(5) . . ? C22 C16 C26 121.6(6) . . ? C22 C16 C45 120.0(5) . . ? C26 C16 C45 111.0(5) . . ? C38 C17 C14 120.4(6) . . ? C38 C17 C32 120.1(6) . . ? C14 C17 C32 107.8(5) . . ? C34 C18 C48 121.6(5) . . ? C34 C18 C12 118.6(5) . . ? C48 C18 C12 107.2(5) . . ? C25 C19 C12 120.9(6) . . ? C25 C19 C39 119.3(5) . . ? C12 C19 C39 107.3(5) . . ? C36 C20 C34 120.9(6) . . ? C36 C20 C47 119.5(6) . . ? C34 C20 C47 107.7(5) . . ? C44 C21 C24 118.7(5) . . ? C44 C21 C5 128.1(5) . . ? C24 C21 C5 106.1(5) . . ? C16 C22 C38 119.8(6) . . ? C16 C22 C28 117.5(5) . . ? C38 C22 C28 108.5(5) . . ? C31 C23 C30 121.3(6) . . ? C31 C23 C13 119.6(6) . . ? C30 C23 C13 107.6(5) . . ? C46 C24 C21 121.6(5) . . ? C46 C24 C37 118.7(5) . . ? C21 C24 C37 108.9(5) . . ? C19 C25 C35 120.9(5) . . ? C19 C25 C31 119.7(6) . . ? C35 C25 C31 106.9(5) . . ? C53 C26 C16 119.8(5) . . ? C53 C26 C4 124.5(5) . . ? C16 C26 C4 106.5(5) . . ? C47 C27 C14 120.4(6) . . ? C47 C27 C43 120.0(5) . . ? C14 C27 C43 107.0(5) . . ? C37 C28 C59 121.7(6) . . ? C37 C28 C22 119.2(5) . . ? C59 C28 C22 107.9(5) . . ? C14 C29 C13 119.4(6) . . ? C14 C29 C36 119.8(6) . . ? C13 C29 C36 108.8(6) . . ? C12 C30 C23 120.6(6) . . ? C12 C30 C36 119.0(6) . . ? C23 C30 C36 108.2(5) . . ? C23 C31 C11 120.8(6) . . ? C23 C31 C25 118.9(6) . . ? C11 C31 C25 108.1(5) . . ? C45 C32 C43 118.5(5) . . ? C45 C32 C17 120.2(6) . . ? C43 C32 C17 108.6(5) . . ? C58 C33 C52 117.9(5) . . ? C58 C33 C2 134.7(5) . . ? C52 C33 C2 105.1(5) . . ? C18 C34 C20 121.0(6) . . ? C18 C34 C55 118.0(5) . . ? C20 C34 C55 108.5(5) . . ? C49 C35 C46 118.4(5) . . ? C49 C35 C25 119.3(5) . . ? C46 C35 C25 109.7(5) . . ? C20 C36 C29 121.2(6) . . ? C20 C36 C30 119.1(6) . . ? C29 C36 C30 107.2(6) . . ? C28 C37 C53 122.6(6) . . ? C28 C37 C24 119.4(5) . . ? C53 C37 C24 107.9(5) . . ? C17 C38 C22 119.6(6) . . ? C17 C38 C15 119.0(6) . . ? C22 C38 C15 108.0(5) . . ? C40 C39 C48 118.5(5) . . ? C40 C39 C19 120.5(5) . . ? C48 C39 C19 108.4(5) . . ? C39 C40 C49 119.9(5) . . ? C39 C40 C57 122.4(5) . . ? C49 C40 C57 109.4(5) . . ? C54 C41 C60 121.9(5) . . ? C54 C41 C52 119.9(5) . . ? C60 C41 C52 107.7(5) . . ? C55 C42 C56 120.8(5) . . ? C55 C42 C51 122.2(5) . . ? C56 C42 C51 106.9(5) . . ? C52 C43 C32 119.9(5) . . ? C52 C43 C27 120.1(6) . . ? C32 C43 C27 108.3(5) . . ? C21 C44 C49 121.1(5) . . ? C21 C44 C3 124.4(5) . . ? C49 C44 C3 106.3(5) . . ? C32 C45 C16 120.1(6) . . ? C32 C45 C58 122.3(5) . . ? C16 C45 C58 108.9(5) . . ? C24 C46 C35 119.4(5) . . ? C24 C46 C11 121.1(6) . . ? C35 C46 C11 107.7(5) . . ? C27 C47 C54 119.3(5) . . ? C27 C47 C20 119.4(5) . . ? C54 C47 C20 107.8(5) . . ? C56 C48 C39 119.5(5) . . ? C56 C48 C18 119.5(6) . . ? C39 C48 C18 109.3(5) . . ? C35 C49 C40 119.9(5) . . ? C35 C49 C44 120.4(5) . . ? C40 C49 C44 110.6(5) . . ? O3 C3 C57 127.2(5) . . ? O3 C3 C44 126.8(5) . . ? C57 C3 C44 105.7(5) . . ? C60 C51 C42 119.3(5) . . ? C60 C51 C1 125.7(5) . . ? C42 C51 C1 110.0(5) . . ? C43 C52 C41 119.8(6) . . ? C43 C52 C33 121.8(5) . . ? C41 C52 C33 109.0(5) . . ? C26 C53 C37 118.4(6) . . ? C26 C53 C5 127.4(5) . . ? C37 C53 C5 107.1(5) . . ? C41 C54 C47 120.8(5) . . ? C41 C54 C55 118.2(5) . . ? C47 C54 C55 108.7(5) . . ? C42 C55 C54 118.4(5) . . ? C42 C55 C34 120.7(6) . . ? C54 C55 C34 107.4(5) . . ? C48 C56 C42 119.1(5) . . ? C48 C56 C50 122.0(5) . . ? C42 C56 C50 109.7(5) . . ? C50 C57 C40 119.2(5) . . ? C50 C57 C3 128.8(5) . . ? C40 C57 C3 106.3(5) . . ? C33 C58 C45 119.6(5) . . ? C33 C58 C4 129.9(5) . . ? C45 C58 C4 106.1(5) . . ? C11 C59 C28 119.9(5) . . ? C11 C59 C15 119.6(6) . . ? C28 C59 C15 107.3(5) . . ? C57 C50 C56 118.3(5) . . ? C57 C50 C1 133.7(5) . . ? C56 C50 C1 105.0(5) . . ? C51 C60 C41 119.3(5) . . ? C51 C60 C2 124.4(5) . . ? C41 C60 C2 110.6(5) . . ? C66 C61 C62 119.9(6) . . ? C66 C61 N1 124.5(6) . . ? C62 C61 N1 115.4(5) . . ? C61 C62 C63 118.9(6) . . ? C61 C62 H62A 120.6 . . ? C63 C62 H62A 120.6 . . ? C64 C63 C62 121.9(6) . . ? C64 C63 H63A 119.1 . . ? C62 C63 H63A 119.1 . . ? C65 C64 C63 116.4(6) . . ? C65 C64 C67 120.9(6) . . ? C63 C64 C67 122.7(6) . . ? C66 C65 C64 122.3(6) . . ? C66 C65 H65A 118.9 . . ? C64 C65 H65A 118.9 . . ? C61 C66 C65 120.6(6) . . ? C61 C66 H66A 119.7 . . ? C65 C66 H66A 119.7 . . ? C70 C67 C68 108.7(6) . . ? C70 C67 C64 111.4(6) . . ? C68 C67 C64 108.2(5) . . ? C70 C67 C69 109.7(6) . . ? C68 C67 C69 108.5(6) . . ? C64 C67 C69 110.3(5) . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C67 C69 H69A 109.5 . . ? C67 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C67 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C67 C70 H70A 109.5 . . ? C67 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C67 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? N2 C71 C72 122.8(6) . . ? N2 C71 C76 118.7(5) . . ? C72 C71 C76 117.7(5) . . ? C73 C72 C71 121.8(6) . . ? C73 C72 H72A 119.1 . . ? C71 C72 H72A 119.1 . . ? C72 C73 C74 120.9(6) . . ? C72 C73 H73A 119.6 . . ? C74 C73 H73A 119.6 . . ? C75 C74 C73 117.0(5) . . ? C75 C74 C77 122.5(6) . . ? C73 C74 C77 120.3(6) . . ? C74 C75 C76 122.6(6) . . ? C74 C75 H75A 118.7 . . ? C76 C75 H75A 118.7 . . ? C75 C76 C71 119.9(6) . . ? C75 C76 H76A 120.1 . . ? C71 C76 H76A 120.1 . . ? C80 C77 C78 109.5(6) . . ? C80 C77 C74 112.5(5) . . ? C78 C77 C74 108.4(5) . . ? C80 C77 C79 107.9(6) . . ? C78 C77 C79 107.6(6) . . ? C74 C77 C79 110.9(6) . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C77 C79 H79A 109.5 . . ? C77 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C77 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C77 C80 H80A 109.5 . . ? C77 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C77 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? Cl3 C81 Cl1 110.7(5) . . ? Cl3 C81 Cl2 110.9(4) . . ? Cl1 C81 Cl2 111.9(5) . . ? Cl3 C81 H81A 107.7 . . ? Cl1 C81 H81A 107.7 . . ? Cl2 C81 H81A 107.7 . . ? Cl4 C82 Cl5' 64.8(6) . . ? Cl4 C82 Cl6 115.2(5) . . ? Cl5' C82 Cl6 118.5(6) . . ? Cl4 C82 Cl5 105.3(5) . . ? Cl5' C82 Cl5 40.5(5) . . ? Cl6 C82 Cl5 103.6(4) . . ? Cl4 C82 Cl4' 35.0(4) . . ? Cl5' C82 Cl4' 99.5(7) . . ? Cl6 C82 Cl4' 103.5(5) . . ? Cl5 C82 Cl4' 139.4(7) . . ? Cl4 C82 H82A 110.8 . . ? Cl5' C82 H82A 126.8 . . ? Cl6 C82 H82A 110.8 . . ? Cl5 C82 H82A 110.8 . . ? Cl4' C82 H82A 86.7 . . ? Cl9 C83 Cl7 112.0(4) . . ? Cl9 C83 Cl8 110.0(4) . . ? Cl7 C83 Cl8 110.6(4) . . ? Cl9 C83 H83A 108.0 . . ? Cl7 C83 H83A 108.0 . . ? Cl8 C83 H83A 108.0 . . ? Cl10 Cl12 C84 68.0(6) 2_666 1_556 ? Cl10 Cl12 Cl11 112.4(10) 2_666 2_666 ? C84 Cl12 Cl11 51.4(2) 1_556 2_666 ? C84 Cl11 Cl10 55.817(10) . 2_665 ? C84 Cl11 Cl12 51.1(2) . 2_666 ? Cl10 Cl11 Cl12 103.92(2) 2_665 2_666 ? Cl12 Cl10 C84 69.9(2) 2_666 . ? Cl12 Cl10 Cl11 117.9(2) 2_666 2_665 ? C84 Cl10 Cl11 57.348(9) . 2_665 ? Cl10 C84 Cl10 180.0 2_665 . ? Cl10 C84 Cl12 138.0(4) 2_665 2_666 ? Cl10 C84 Cl12 42.0(4) . 2_666 ? Cl10 C84 Cl12 42.0(4) 2_665 1_554 ? Cl10 C84 Cl12 138.0(4) . 1_554 ? Cl12 C84 Cl12 180.0(13) 2_666 1_554 ? Cl10 C84 Cl11 66.835(7) 2_665 . ? Cl10 C84 Cl11 113.165(7) . . ? Cl12 C84 Cl11 77.494(9) 2_666 . ? Cl12 C84 Cl11 102.506(9) 1_554 . ? Cl10 C84 Cl11 113.165(6) 2_665 2_665 ? Cl10 C84 Cl11 66.835(6) . 2_665 ? Cl12 C84 Cl11 102.506(9) 2_666 2_665 ? Cl12 C84 Cl11 77.494(9) 1_554 2_665 ? Cl11 C84 Cl11 180.0 . 2_665 ? 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 O1 C1 C6 C7 120.0(6) . . . . ? C51 C1 C6 C7 2.1(7) . . . . ? C50 C1 C6 C7 -113.7(6) . . . . ? O1 C1 C6 C10 -46.9(6) . . . . ? C51 C1 C6 C10 -164.8(5) . . . . ? C50 C1 C6 C10 79.4(6) . . . . ? C10 C6 C7 C8 -3.6(8) . . . . ? C1 C6 C7 C8 -170.5(5) . . . . ? C10 C6 C7 C2 166.2(5) . . . . ? C1 C6 C7 C2 -0.7(8) . . . . ? O2 C2 C7 C6 -118.4(6) . . . . ? C60 C2 C7 C6 -1.5(7) . . . . ? C33 C2 C7 C6 113.1(6) . . . . ? O2 C2 C7 C8 51.8(6) . . . . ? C60 C2 C7 C8 168.7(4) . . . . ? C33 C2 C7 C8 -76.7(6) . . . . ? C61 N1 C8 O6 2.8(8) . . . . ? C61 N1 C8 C7 178.1(5) . . . . ? C9 O6 C8 N1 -163.6(5) . . . . ? C9 O6 C8 C7 20.9(7) . . . . ? C6 C7 C8 N1 163.9(5) . . . . ? C2 C7 C8 N1 -7.0(8) . . . . ? C6 C7 C8 O6 -20.6(8) . . . . ? C2 C7 C8 O6 168.5(5) . . . . ? C8 O6 C9 O7 -174.2(5) . . . . ? C8 O6 C9 C10 2.6(7) . . . . ? C71 N2 C10 C6 168.1(5) . . . . ? C71 N2 C10 C9 -11.4(9) . . . . ? C7 C6 C10 N2 -152.3(6) . . . . ? C1 C6 C10 N2 15.2(8) . . . . ? C7 C6 C10 C9 27.2(7) . . . . ? C1 C6 C10 C9 -165.3(5) . . . . ? O7 C9 C10 N2 -31.3(9) . . . . ? O6 C9 C10 N2 152.2(5) . . . . ? O7 C9 C10 C6 149.2(6) . . . . ? O6 C9 C10 C6 -27.3(7) . . . . ? C29 C13 C15 C38 0.2(8) . . . . ? C23 C13 C15 C38 138.2(6) . . . . ? C29 C13 C15 C59 -139.9(6) . . . . ? C23 C13 C15 C59 -1.9(8) . . . . ? C29 C14 C17 C38 -1.9(8) . . . . ? C27 C14 C17 C38 -145.0(5) . . . . ? C29 C14 C17 C32 141.1(5) . . . . ? C27 C14 C17 C32 -2.1(6) . . . . ? C30 C12 C18 C34 -2.6(9) . . . . ? C19 C12 C18 C34 -143.9(5) . . . . ? C30 C12 C18 C48 140.0(6) . . . . ? C19 C12 C18 C48 -1.3(7) . . . . ? C30 C12 C19 C25 0.9(8) . . . . ? C18 C12 C19 C25 143.3(6) . . . . ? C30 C12 C19 C39 -140.8(6) . . . . ? C18 C12 C19 C39 1.6(7) . . . . ? O5 C5 C21 C44 -52.3(9) . . . . ? C53 C5 C21 C44 126.7(6) . . . . ? O5 C5 C21 C24 158.2(6) . . . . ? C53 C5 C21 C24 -22.8(6) . . . . ? C26 C16 C22 C38 -145.5(6) . . . . ? C45 C16 C22 C38 1.6(8) . . . . ? C26 C16 C22 C28 -10.3(8) . . . . ? C45 C16 C22 C28 136.9(6) . . . . ? C15 C13 C23 C31 0.9(8) . . . . ? C29 C13 C23 C31 143.3(5) . . . . ? C15 C13 C23 C30 -143.0(5) . . . . ? C29 C13 C23 C30 -0.5(6) . . . . ? C44 C21 C24 C46 6.1(9) . . . . ? C5 C21 C24 C46 158.9(5) . . . . ? C44 C21 C24 C37 -137.6(6) . . . . ? C5 C21 C24 C37 15.3(6) . . . . ? C12 C19 C25 C35 -137.7(6) . . . . ? C39 C19 C25 C35 -0.4(9) . . . . ? C12 C19 C25 C31 -0.8(8) . . . . ? C39 C19 C25 C31 136.5(6) . . . . ? C22 C16 C26 C53 8.0(9) . . . . ? C45 C16 C26 C53 -141.8(6) . . . . ? C22 C16 C26 C4 156.4(5) . . . . ? C45 C16 C26 C4 6.6(7) . . . . ? O4 C4 C26 C53 -40.8(9) . . . . ? C58 C4 C26 C53 132.4(6) . . . . ? O4 C4 C26 C16 172.6(6) . . . . ? C58 C4 C26 C16 -14.1(6) . . . . ? C29 C14 C27 C47 0.5(8) . . . . ? C17 C14 C27 C47 143.9(5) . . . . ? C29 C14 C27 C43 -141.4(5) . . . . ? C17 C14 C27 C43 2.1(6) . . . . ? C16 C22 C28 C37 4.6(8) . . . . ? C38 C22 C28 C37 144.6(5) . . . . ? C16 C22 C28 C59 -139.8(5) . . . . ? C38 C22 C28 C59 0.1(6) . . . . ? C17 C14 C29 C13 0.2(8) . . . . ? C27 C14 C29 C13 139.2(6) . . . . ? C17 C14 C29 C36 -138.3(6) . . . . ? C27 C14 C29 C36 0.8(8) . . . . ? C15 C13 C29 C14 0.7(8) . . . . ? C23 C13 C29 C14 -141.5(5) . . . . ? C15 C13 C29 C36 143.2(5) . . . . ? C23 C13 C29 C36 1.0(6) . . . . ? C19 C12 C30 C23 0.2(8) . . . . ? C18 C12 C30 C23 -137.1(6) . . . . ? C19 C12 C30 C36 138.2(6) . . . . ? C18 C12 C30 C36 0.9(9) . . . . ? C31 C23 C30 C12 -1.3(9) . . . . ? C13 C23 C30 C12 141.8(6) . . . . ? C31 C23 C30 C36 -143.3(6) . . . . ? C13 C23 C30 C36 -0.2(6) . . . . ? C30 C23 C31 C11 139.2(6) . . . . ? C13 C23 C31 C11 0.4(8) . . . . ? C30 C23 C31 C25 1.3(9) . . . . ? C13 C23 C31 C25 -137.5(6) . . . . ? C59 C11 C31 C23 -0.5(8) . . . . ? C46 C11 C31 C23 -141.7(6) . . . . ? C59 C11 C31 C25 141.3(5) . . . . ? C46 C11 C31 C25 0.1(7) . . . . ? C19 C25 C31 C23 -0.3(9) . . . . ? C35 C25 C31 C23 141.9(6) . . . . ? C19 C25 C31 C11 -143.0(6) . . . . ? C35 C25 C31 C11 -0.7(7) . . . . ? C38 C17 C32 C45 3.2(8) . . . . ? C14 C17 C32 C45 -139.9(5) . . . . ? C38 C17 C32 C43 144.3(5) . . . . ? C14 C17 C32 C43 1.3(6) . . . . ? O2 C2 C33 C58 -116.6(6) . . . . ? C60 C2 C33 C58 133.6(6) . . . . ? C7 C2 C33 C58 13.2(9) . . . . ? O2 C2 C33 C52 81.7(5) . . . . ? C60 C2 C33 C52 -28.1(5) . . . . ? C7 C2 C33 C52 -148.5(5) . . . . ? C48 C18 C34 C20 -134.1(6) . . . . ? C12 C18 C34 C20 3.0(8) . . . . ? C48 C18 C34 C55 3.5(9) . . . . ? C12 C18 C34 C55 140.5(6) . . . . ? C36 C20 C34 C18 -1.7(9) . . . . ? C47 C20 C34 C18 140.9(6) . . . . ? C36 C20 C34 C55 -142.7(6) . . . . ? C47 C20 C34 C55 -0.1(6) . . . . ? C19 C25 C35 C49 1.5(9) . . . . ? C31 C25 C35 C49 -140.2(5) . . . . ? C19 C25 C35 C46 142.7(6) . . . . ? C31 C25 C35 C46 1.1(7) . . . . ? C34 C20 C36 C29 136.9(6) . . . . ? C47 C20 C36 C29 -1.4(9) . . . . ? C34 C20 C36 C30 -0.2(9) . . . . ? C47 C20 C36 C30 -138.5(6) . . . . ? C14 C29 C36 C20 -0.3(9) . . . . ? C13 C29 C36 C20 -142.6(6) . . . . ? C14 C29 C36 C30 141.2(5) . . . . ? C13 C29 C36 C30 -1.1(6) . . . . ? C12 C30 C36 C20 0.5(9) . . . . ? C23 C30 C36 C20 143.2(6) . . . . ? C12 C30 C36 C29 -141.9(6) . . . . ? C23 C30 C36 C29 0.8(6) . . . . ? C59 C28 C37 C53 142.6(6) . . . . ? C22 C28 C37 C53 3.2(9) . . . . ? C59 C28 C37 C24 1.4(8) . . . . ? C22 C28 C37 C24 -138.0(6) . . . . ? C46 C24 C37 C28 0.2(8) . . . . ? C21 C24 C37 C28 145.1(5) . . . . ? C46 C24 C37 C53 -146.2(5) . . . . ? C21 C24 C37 C53 -1.3(7) . . . . ? C14 C17 C38 C22 138.8(6) . . . . ? C32 C17 C38 C22 0.3(8) . . . . ? C14 C17 C38 C15 2.7(8) . . . . ? C32 C17 C38 C15 -135.8(6) . . . . ? C16 C22 C38 C17 -2.7(8) . . . . ? C28 C22 C38 C17 -141.5(5) . . . . ? C16 C22 C38 C15 137.7(6) . . . . ? C28 C22 C38 C15 -1.1(6) . . . . ? C13 C15 C38 C17 -1.9(8) . . . . ? C59 C15 C38 C17 142.4(5) . . . . ? C13 C15 C38 C22 -142.5(5) . . . . ? C59 C15 C38 C22 1.8(6) . . . . ? C25 C19 C39 C40 -2.6(9) . . . . ? C12 C19 C39 C40 139.8(6) . . . . ? C25 C19 C39 C48 -143.8(6) . . . . ? C12 C19 C39 C48 -1.3(6) . . . . ? C48 C39 C40 C49 141.9(5) . . . . ? C19 C39 C40 C49 4.6(8) . . . . ? C48 C39 C40 C57 -3.1(8) . . . . ? C19 C39 C40 C57 -140.5(6) . . . . ? C45 C32 C43 C52 -1.0(8) . . . . ? C17 C32 C43 C52 -142.9(6) . . . . ? C45 C32 C43 C27 141.9(6) . . . . ? C17 C32 C43 C27 0.0(6) . . . . ? C47 C27 C43 C52 -0.4(9) . . . . ? C14 C27 C43 C52 141.6(5) . . . . ? C47 C27 C43 C32 -143.3(6) . . . . ? C14 C27 C43 C32 -1.3(6) . . . . ? C24 C21 C44 C49 -2.3(8) . . . . ? C5 C21 C44 C49 -148.5(6) . . . . ? C24 C21 C44 C3 141.8(5) . . . . ? C5 C21 C44 C3 -4.4(9) . . . . ? C43 C32 C45 C16 -141.7(6) . . . . ? C17 C32 C45 C16 -4.3(8) . . . . ? C43 C32 C45 C58 2.2(9) . . . . ? C17 C32 C45 C58 139.6(6) . . . . ? C22 C16 C45 C32 1.9(8) . . . . ? C26 C16 C45 C32 152.3(5) . . . . ? C22 C16 C45 C58 -146.3(5) . . . . ? C26 C16 C45 C58 4.0(7) . . . . ? C21 C24 C46 C35 -3.5(9) . . . . ? C37 C24 C46 C35 136.8(6) . . . . ? C21 C24 C46 C11 -141.9(6) . . . . ? C37 C24 C46 C11 -1.6(8) . . . . ? C49 C35 C46 C24 -2.7(8) . . . . ? C25 C35 C46 C24 -144.3(6) . . . . ? C49 C35 C46 C11 140.6(5) . . . . ? C25 C35 C46 C11 -1.0(7) . . . . ? C59 C11 C46 C24 1.4(8) . . . . ? C31 C11 C46 C24 143.1(6) . . . . ? C59 C11 C46 C35 -141.2(6) . . . . ? C31 C11 C46 C35 0.5(7) . . . . ? C14 C27 C47 C54 -138.0(6) . . . . ? C43 C27 C47 C54 -1.0(9) . . . . ? C14 C27 C47 C20 -2.1(8) . . . . ? C43 C27 C47 C20 134.8(6) . . . . ? C36 C20 C47 C27 2.6(8) . . . . ? C34 C20 C47 C27 -140.6(5) . . . . ? C36 C20 C47 C54 142.9(6) . . . . ? C34 C20 C47 C54 -0.3(6) . . . . ? C40 C39 C48 C56 1.5(8) . . . . ? C19 C39 C48 C56 143.5(5) . . . . ? C40 C39 C48 C18 -141.5(5) . . . . ? C19 C39 C48 C18 0.5(7) . . . . ? C34 C18 C48 C56 -1.2(9) . . . . ? C12 C18 C48 C56 -142.5(6) . . . . ? C34 C18 C48 C39 141.7(6) . . . . ? C12 C18 C48 C39 0.5(7) . . . . ? C46 C35 C49 C40 -137.5(6) . . . . ? C25 C35 C49 C40 0.4(8) . . . . ? C46 C35 C49 C44 6.4(8) . . . . ? C25 C35 C49 C44 144.3(6) . . . . ? C39 C40 C49 C35 -3.5(8) . . . . ? C57 C40 C49 C35 145.7(5) . . . . ? C39 C40 C49 C44 -150.6(5) . . . . ? C57 C40 C49 C44 -1.4(6) . . . . ? C21 C44 C49 C35 -3.9(8) . . . . ? C3 C44 C49 C35 -153.6(5) . . . . ? C21 C44 C49 C40 143.0(5) . . . . ? C3 C44 C49 C40 -6.7(6) . . . . ? C21 C44 C3 O3 37.4(9) . . . . ? C49 C44 C3 O3 -174.2(5) . . . . ? C21 C44 C3 C57 -136.6(6) . . . . ? C49 C44 C3 C57 11.9(6) . . . . ? C55 C42 C51 C60 6.2(8) . . . . ? C56 C42 C51 C60 -139.3(5) . . . . ? C55 C42 C51 C1 162.7(5) . . . . ? C56 C42 C51 C1 17.2(6) . . . . ? O1 C1 C51 C60 -120.9(6) . . . . ? C6 C1 C51 C60 -1.3(7) . . . . ? C50 C1 C51 C60 127.0(6) . . . . ? O1 C1 C51 C42 84.4(5) . . . . ? C6 C1 C51 C42 -155.9(4) . . . . ? C50 C1 C51 C42 -27.7(5) . . . . ? C32 C43 C52 C41 142.0(6) . . . . ? C27 C43 C52 C41 3.4(9) . . . . ? C32 C43 C52 C33 -0.7(9) . . . . ? C27 C43 C52 C33 -139.4(6) . . . . ? C54 C41 C52 C43 -4.9(8) . . . . ? C60 C41 C52 C43 -150.4(5) . . . . ? C54 C41 C52 C33 142.1(5) . . . . ? C60 C41 C52 C33 -3.4(6) . . . . ? C58 C33 C52 C43 1.3(8) . . . . ? C2 C33 C52 C43 166.7(5) . . . . ? C58 C33 C52 C41 -144.9(5) . . . . ? C2 C33 C52 C41 20.4(6) . . . . ? C16 C26 C53 C37 0.0(8) . . . . ? C4 C26 C53 C37 -142.5(6) . . . . ? C16 C26 C53 C5 146.5(6) . . . . ? C4 C26 C53 C5 4.1(10) . . . . ? C28 C37 C53 C26 -5.6(9) . . . . ? C24 C37 C53 C26 139.4(6) . . . . ? C28 C37 C53 C5 -158.3(5) . . . . ? C24 C37 C53 C5 -13.3(6) . . . . ? O5 C5 C53 C26 51.8(10) . . . . ? C21 C5 C53 C26 -127.3(6) . . . . ? O5 C5 C53 C37 -158.7(6) . . . . ? C21 C5 C53 C37 22.2(6) . . . . ? C60 C41 C54 C47 144.0(6) . . . . ? C52 C41 C54 C47 3.5(8) . . . . ? C60 C41 C54 C55 6.0(8) . . . . ? C52 C41 C54 C55 -134.5(6) . . . . ? C27 C47 C54 C41 -0.5(8) . . . . ? C20 C47 C54 C41 -140.9(5) . . . . ? C27 C47 C54 C55 141.0(5) . . . . ? C20 C47 C54 C55 0.6(6) . . . . ? C56 C42 C55 C54 133.9(6) . . . . ? C51 C42 C55 C54 -6.9(8) . . . . ? C56 C42 C55 C34 -1.9(8) . . . . ? C51 C42 C55 C34 -142.7(6) . . . . ? C41 C54 C55 C42 0.9(8) . . . . ? C47 C54 C55 C42 -141.8(5) . . . . ? C41 C54 C55 C34 142.0(5) . . . . ? C47 C54 C55 C34 -0.7(6) . . . . ? C18 C34 C55 C42 -1.9(8) . . . . ? C20 C34 C55 C42 140.5(5) . . . . ? C18 C34 C55 C54 -141.9(5) . . . . ? C20 C34 C55 C54 0.5(6) . . . . ? C39 C48 C56 C42 -141.8(6) . . . . ? C18 C48 C56 C42 -2.6(8) . . . . ? C39 C48 C56 C50 1.7(8) . . . . ? C18 C48 C56 C50 140.9(6) . . . . ? C55 C42 C56 C48 4.2(8) . . . . ? C51 C42 C56 C48 150.2(5) . . . . ? C55 C42 C56 C50 -143.5(5) . . . . ? C51 C42 C56 C50 2.6(6) . . . . ? C39 C40 C57 C50 1.5(8) . . . . ? C49 C40 C57 C50 -146.7(5) . . . . ? C39 C40 C57 C3 157.2(5) . . . . ? C49 C40 C57 C3 9.0(6) . . . . ? O3 C3 C57 C50 -34.0(9) . . . . ? C44 C3 C57 C50 139.9(6) . . . . ? O3 C3 C57 C40 173.4(6) . . . . ? C44 C3 C57 C40 -12.7(5) . . . . ? C52 C33 C58 C45 -0.2(8) . . . . ? C2 C33 C58 C45 -160.1(6) . . . . ? C52 C33 C58 C4 152.8(6) . . . . ? C2 C33 C58 C4 -7.1(10) . . . . ? C32 C45 C58 C33 -1.6(8) . . . . ? C16 C45 C58 C33 145.8(5) . . . . ? C32 C45 C58 C4 -160.4(5) . . . . ? C16 C45 C58 C4 -12.9(6) . . . . ? O4 C4 C58 C33 33.4(10) . . . . ? C26 C4 C58 C33 -139.3(6) . . . . ? O4 C4 C58 C45 -170.9(6) . . . . ? C26 C4 C58 C45 16.4(6) . . . . ? C31 C11 C59 C28 -136.7(6) . . . . ? C46 C11 C59 C28 0.1(8) . . . . ? C31 C11 C59 C15 -0.6(8) . . . . ? C46 C11 C59 C15 136.3(6) . . . . ? C37 C28 C59 C11 -1.6(9) . . . . ? C22 C28 C59 C11 141.8(5) . . . . ? C37 C28 C59 C15 -142.4(6) . . . . ? C22 C28 C59 C15 1.0(6) . . . . ? C13 C15 C59 C11 1.8(8) . . . . ? C38 C15 C59 C11 -142.7(5) . . . . ? C13 C15 C59 C28 142.8(5) . . . . ? C38 C15 C59 C28 -1.7(6) . . . . ? C40 C57 C50 C56 1.7(8) . . . . ? C3 C57 C50 C56 -147.9(5) . . . . ? C40 C57 C50 C1 158.7(5) . . . . ? C3 C57 C50 C1 9.2(10) . . . . ? C48 C56 C50 C57 -3.3(8) . . . . ? C42 C56 C50 C57 143.2(5) . . . . ? C48 C56 C50 C1 -166.3(5) . . . . ? C42 C56 C50 C1 -19.8(6) . . . . ? O1 C1 C50 C57 117.5(6) . . . . ? C51 C1 C50 C57 -131.2(6) . . . . ? C6 C1 C50 C57 -9.7(9) . . . . ? O1 C1 C50 C56 -83.3(5) . . . . ? C51 C1 C50 C56 28.0(5) . . . . ? C6 C1 C50 C56 149.5(5) . . . . ? C42 C51 C60 C41 0.8(8) . . . . ? C1 C51 C60 C41 -151.7(5) . . . . ? C42 C51 C60 C2 151.5(5) . . . . ? C1 C51 C60 C2 -1.0(9) . . . . ? C54 C41 C60 C51 -6.9(8) . . . . ? C52 C41 C60 C51 137.8(5) . . . . ? C54 C41 C60 C2 -161.3(5) . . . . ? C52 C41 C60 C2 -16.7(6) . . . . ? O2 C2 C60 C51 122.6(5) . . . . ? C7 C2 C60 C51 2.4(7) . . . . ? C33 C2 C60 C51 -125.6(6) . . . . ? O2 C2 C60 C41 -84.5(5) . . . . ? C7 C2 C60 C41 155.3(5) . . . . ? C33 C2 C60 C41 27.3(5) . . . . ? C8 N1 C61 C66 48.4(8) . . . . ? C8 N1 C61 C62 -135.2(6) . . . . ? C66 C61 C62 C63 -2.6(9) . . . . ? N1 C61 C62 C63 -179.2(5) . . . . ? C61 C62 C63 C64 2.4(10) . . . . ? C62 C63 C64 C65 -0.8(9) . . . . ? C62 C63 C64 C67 -178.6(6) . . . . ? C63 C64 C65 C66 -0.5(9) . . . . ? C67 C64 C65 C66 177.3(6) . . . . ? C62 C61 C66 C65 1.3(9) . . . . ? N1 C61 C66 C65 177.6(5) . . . . ? C64 C65 C66 C61 0.2(10) . . . . ? C65 C64 C67 C70 27.7(8) . . . . ? C63 C64 C67 C70 -154.7(6) . . . . ? C65 C64 C67 C68 -91.7(7) . . . . ? C63 C64 C67 C68 85.9(7) . . . . ? C65 C64 C67 C69 149.8(6) . . . . ? C63 C64 C67 C69 -32.6(8) . . . . ? C10 N2 C71 C72 -54.5(8) . . . . ? C10 N2 C71 C76 136.2(6) . . . . ? N2 C71 C72 C73 -172.2(6) . . . . ? C76 C71 C72 C73 -2.8(9) . . . . ? C71 C72 C73 C74 -0.4(10) . . . . ? C72 C73 C74 C75 1.0(9) . . . . ? C72 C73 C74 C77 176.3(6) . . . . ? C73 C74 C75 C76 1.6(9) . . . . ? C77 C74 C75 C76 -173.5(6) . . . . ? C74 C75 C76 C71 -4.9(9) . . . . ? N2 C71 C76 C75 175.2(5) . . . . ? C72 C71 C76 C75 5.3(8) . . . . ? C75 C74 C77 C80 -15.5(8) . . . . ? C73 C74 C77 C80 169.5(6) . . . . ? C75 C74 C77 C78 105.7(7) . . . . ? C73 C74 C77 C78 -69.3(8) . . . . ? C75 C74 C77 C79 -136.4(7) . . . . ? C73 C74 C77 C79 48.6(8) . . . . ? Cl12 Cl10 C84 Cl10 -172(100) 2_666 . . 2_665 ? Cl11 Cl10 C84 Cl10 -26(100) 2_665 . . 2_665 ? Cl11 Cl10 C84 Cl12 145.7(9) 2_665 . . 2_666 ? Cl12 Cl10 C84 Cl12 180.0 2_666 . . 1_554 ? Cl11 Cl10 C84 Cl12 -34.3(9) 2_665 . . 1_554 ? Cl12 Cl10 C84 Cl11 34.3(9) 2_666 . . . ? Cl11 Cl10 C84 Cl11 180.0 2_665 . . . ? Cl12 Cl10 C84 Cl11 -145.7(9) 2_666 . . 2_665 ? Cl12 Cl11 C84 Cl10 157.3(7) 2_666 . . 2_665 ? Cl10 Cl11 C84 Cl10 180.0 2_665 . . . ? Cl12 Cl11 C84 Cl10 -22.7(7) 2_666 . . . ? Cl10 Cl11 C84 Cl12 -157.3(7) 2_665 . . 2_666 ? Cl10 Cl11 C84 Cl12 22.7(7) 2_665 . . 1_554 ? Cl12 Cl11 C84 Cl12 180.0 2_666 . . 1_554 ? Cl10 Cl11 C84 Cl11 41(100) 2_665 . . 2_665 ? Cl12 Cl11 C84 Cl11 -161(100) 2_666 . . 2_665 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.37 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.949 _refine_diff_density_min -0.952 _refine_diff_density_rms 0.153 # Attachment 'sa700.cif' data_sa700 _database_code_depnum_ccdc_archive 'CCDC 854106' #TrackingRef 'sa700.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C80 H28 N2 O7, 3(C H Cl3)' _chemical_formula_sum 'C83 H31 Cl9 N2 O7' _chemical_formula_weight 1487.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.7838(19) _cell_length_b 15.0011(18) _cell_length_c 15.416(2) _cell_angle_alpha 75.211(4) _cell_angle_beta 88.656(5) _cell_angle_gamma 72.633(4) _cell_volume 3149.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 817 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 0.466 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9125 _exptl_absorpt_correction_T_max 0.9505 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Saturn724+ CCD' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32471 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0429 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11070 _reflns_number_gt 9826 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material 'SHELX97 (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^)+(0.1010P)^2^+6.8904P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11070 _refine_ls_number_parameters 935 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0951 _refine_ls_R_factor_gt 0.0863 _refine_ls_wR_factor_ref 0.2250 _refine_ls_wR_factor_gt 0.2177 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.136 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.34020(18) 0.32039(18) 0.21597(17) 0.1047(7) Uani 1 1 d . . . Cl2 Cl 0.24342(16) 0.23603(15) 0.11255(11) 0.0866(6) Uani 1 1 d . . . Cl3 Cl 0.27843(11) 0.15810(11) 0.30271(9) 0.0605(4) Uani 1 1 d . . . Cl4 Cl 0.7693(3) 0.2527(4) 0.2346(3) 0.1008(16) Uani 0.653(7) 1 d PDU A 1 Cl5 Cl 0.7379(3) 0.1741(3) 0.4153(3) 0.1011(14) Uani 0.653(7) 1 d PDU A 1 Cl4' Cl 0.7238(8) 0.3258(7) 0.1929(5) 0.111(3) Uani 0.347(7) 1 d PDU A 2 Cl5' Cl 0.7845(5) 0.1721(5) 0.3435(8) 0.129(4) Uani 0.347(7) 1 d PDU A 2 Cl6 Cl 0.58207(13) 0.25333(15) 0.28950(15) 0.0841(5) Uani 1 1 d . A . Cl7 Cl 0.16215(17) 0.52978(17) -0.00235(16) 0.0991(7) Uani 1 1 d . . . Cl8 Cl -0.02756(13) 0.64906(14) 0.00951(14) 0.0859(6) Uani 1 1 d . . . Cl9 Cl 0.06635(12) 0.49675(11) 0.16271(10) 0.0638(4) Uani 1 1 d . . . O1 O 0.1731(2) 0.3742(2) 0.37575(18) 0.0296(6) Uani 1 1 d . . . H1 H 0.1916 0.4193 0.3442 0.036 Uiso 1 1 d R . . O2 O 0.00474(19) 0.4442(2) 0.62583(19) 0.0293(6) Uani 1 1 d . . . H2 H -0.0065 0.4976 0.6385 0.035 Uiso 1 1 d R . . O3 O 0.3822(2) 0.4794(2) 0.4768(2) 0.0356(7) Uani 1 1 d . . . O4 O 0.2406(2) 0.5431(2) 0.6948(2) 0.0428(8) Uani 1 1 d . . . O5 O 0.4279(2) 0.5454(2) 0.6298(2) 0.0413(8) Uani 1 1 d . . . O6 O 0.1557(2) 0.6462(2) 0.5160(2) 0.0392(7) Uani 1 1 d . . . O7 O 0.2470(3) 0.6858(2) 0.4086(2) 0.0487(9) Uani 1 1 d . . . N1 N 0.0490(2) 0.6065(2) 0.6183(2) 0.0288(7) Uani 1 1 d . . . N2 N 0.2137(2) 0.5379(2) 0.3334(2) 0.0295(8) Uani 1 1 d . . . C1 C 0.2153(3) 0.3628(3) 0.4620(3) 0.0255(8) Uani 1 1 d . . . C2 C 0.1053(3) 0.4086(3) 0.6259(3) 0.0254(8) Uani 1 1 d . . . C4 C 0.2617(3) 0.4668(3) 0.7509(3) 0.0303(9) Uani 1 1 d . . . C5 C 0.4610(3) 0.4614(3) 0.6715(3) 0.0319(9) Uani 1 1 d . . . C6 C 0.1915(3) 0.4605(3) 0.4844(3) 0.0245(8) Uani 1 1 d . . . C7 C 0.1432(3) 0.4806(3) 0.5574(3) 0.0244(8) Uani 1 1 d . . . C8 C 0.1116(3) 0.5809(3) 0.5649(3) 0.0274(9) Uani 1 1 d . . . C9 C 0.2032(3) 0.6306(3) 0.4412(3) 0.0260(8) Uani 1 1 d . . . C10 C 0.2037(3) 0.5434(3) 0.4139(3) 0.0265(8) Uani 1 1 d . . . C11 C 0.6099(3) 0.1321(3) 0.7935(3) 0.0334(10) Uani 1 1 d . . . C12 C 0.4814(3) 0.0029(3) 0.6488(3) 0.0341(10) Uani 1 1 d . . . C13 C 0.4898(3) 0.0211(3) 0.8738(3) 0.0328(10) Uani 1 1 d . . . C14 C 0.3174(3) 0.0702(3) 0.8917(3) 0.0330(10) Uani 1 1 d . . . C15 C 0.4987(3) 0.0958(3) 0.9074(3) 0.0364(10) Uani 1 1 d . . . C16 C 0.3475(3) 0.3373(3) 0.8711(3) 0.0316(9) Uani 1 1 d . . . C17 C 0.3266(3) 0.1488(3) 0.9250(3) 0.0346(10) Uani 1 1 d . . . C18 C 0.3933(3) 0.0365(3) 0.5945(3) 0.0325(9) Uani 1 1 d . . . C19 C 0.5416(3) 0.0614(3) 0.6070(3) 0.0327(9) Uani 1 1 d . . . C20 C 0.3083(3) 0.0087(3) 0.7333(3) 0.0317(9) Uani 1 1 d . . . C21 C 0.5278(3) 0.3792(3) 0.6404(3) 0.0296(9) Uani 1 1 d . . . C22 C 0.4254(3) 0.2569(3) 0.9084(3) 0.0329(9) Uani 1 1 d . . . C23 C 0.5416(3) -0.0004(3) 0.7976(3) 0.0349(10) Uani 1 1 d . . . C24 C 0.5732(3) 0.3061(3) 0.7199(3) 0.0326(9) Uani 1 1 d . . . C25 C 0.5991(3) 0.0860(3) 0.6601(3) 0.0339(10) Uani 1 1 d . . . C26 C 0.3567(3) 0.4178(3) 0.8026(3) 0.0306(9) Uani 1 1 d . . . C27 C 0.2299(3) 0.1044(3) 0.8361(3) 0.0323(9) Uani 1 1 d . . . C28 C 0.5150(3) 0.2513(3) 0.8685(3) 0.0326(9) Uani 1 1 d . . . C29 C 0.3978(3) 0.0073(3) 0.8659(3) 0.0347(10) Uani 1 1 d . . . C30 C 0.4827(3) -0.0270(3) 0.7418(3) 0.0342(10) Uani 1 1 d . . . C31 C 0.6001(3) 0.0542(3) 0.7575(3) 0.0343(10) Uani 1 1 d . . . C32 C 0.2454(3) 0.2326(3) 0.8880(3) 0.0322(9) Uani 1 1 d . . . C33 C 0.1477(3) 0.3695(3) 0.7264(3) 0.0255(8) Uani 1 1 d . . . C34 C 0.3087(3) 0.0385(3) 0.6360(3) 0.0315(9) Uani 1 1 d . . . C35 C 0.6080(3) 0.1829(3) 0.6365(3) 0.0314(9) Uani 1 1 d . . . C36 C 0.3929(3) -0.0231(3) 0.7855(3) 0.0345(10) Uani 1 1 d . . . C37 C 0.5216(3) 0.3268(3) 0.7968(3) 0.0319(9) Uani 1 1 d . . . C38 C 0.4154(3) 0.1608(3) 0.9338(3) 0.0352(10) Uani 1 1 d . . . C39 C 0.4877(3) 0.1335(3) 0.5294(3) 0.0306(9) Uani 1 1 d . . . C40 C 0.4914(3) 0.2272(3) 0.5104(3) 0.0300(9) Uani 1 1 d . . . C41 C 0.1290(3) 0.2376(3) 0.6792(3) 0.0278(9) Uani 1 1 d . . . C42 C 0.2282(3) 0.1960(3) 0.5320(3) 0.0277(9) Uani 1 1 d . . . C43 C 0.1860(3) 0.2054(3) 0.8349(3) 0.0318(9) Uani 1 1 d . . . C44 C 0.5161(3) 0.3518(3) 0.5636(3) 0.0285(9) Uani 1 1 d . . . C45 C 0.2561(3) 0.3238(3) 0.8587(3) 0.0300(9) Uani 1 1 d . . . C46 C 0.6160(3) 0.2100(3) 0.7182(3) 0.0318(9) Uani 1 1 d . . . C47 C 0.2243(3) 0.0729(3) 0.7598(3) 0.0311(9) Uani 1 1 d . . . C48 C 0.3975(3) 0.1181(3) 0.5219(3) 0.0304(9) Uani 1 1 d . . . C49 C 0.5543(3) 0.2526(3) 0.5635(3) 0.0312(9) Uani 1 1 d . . . C3 C 0.4300(3) 0.3960(3) 0.4983(3) 0.0290(9) Uani 1 1 d . . . C51 C 0.1750(3) 0.2937(3) 0.5292(3) 0.0253(8) Uani 1 1 d . . . C52 C 0.1389(3) 0.2715(3) 0.7560(3) 0.0276(9) Uani 1 1 d . . . C53 C 0.4438(3) 0.4140(3) 0.7665(3) 0.0331(9) Uani 1 1 d . . . C54 C 0.1720(3) 0.1412(3) 0.6795(3) 0.0317(9) Uani 1 1 d . . . C55 C 0.2238(3) 0.1197(3) 0.6029(3) 0.0294(9) Uani 1 1 d . . . C56 C 0.3171(3) 0.1979(3) 0.4924(3) 0.0275(9) Uani 1 1 d . . . C57 C 0.4086(3) 0.3102(3) 0.4772(2) 0.0260(8) Uani 1 1 d . . . C58 C 0.2058(3) 0.3943(3) 0.7780(3) 0.0266(8) Uani 1 1 d . . . C59 C 0.5601(3) 0.1517(3) 0.8675(3) 0.0345(10) Uani 1 1 d . . . C50 C 0.3211(3) 0.2968(3) 0.4674(3) 0.0266(8) Uani 1 1 d . . . C60 C 0.1266(3) 0.3146(3) 0.6004(3) 0.0264(8) Uani 1 1 d . . . C61 C 0.0175(3) 0.7023(3) 0.6298(3) 0.0290(9) Uani 1 1 d . . . C62 C 0.0101(3) 0.7109(3) 0.7173(3) 0.0375(10) Uani 1 1 d . . . H62A H 0.0265 0.6546 0.7662 0.045 Uiso 1 1 calc R . . C63 C -0.0212(3) 0.8017(3) 0.7335(3) 0.0394(11) Uani 1 1 d . . . H63A H -0.0243 0.8064 0.7939 0.047 Uiso 1 1 calc R . . C64 C -0.0484(3) 0.8863(3) 0.6636(3) 0.0344(10) Uani 1 1 d . . . C65 C -0.0420(3) 0.8751(3) 0.5770(3) 0.0365(10) Uani 1 1 d . . . H65A H -0.0604 0.9309 0.5277 0.044 Uiso 1 1 calc R . . C66 C -0.0093(3) 0.7845(3) 0.5602(3) 0.0351(10) Uani 1 1 d . . . H66A H -0.0056 0.7794 0.4999 0.042 Uiso 1 1 calc R . . C67 C -0.0803(3) 0.9865(3) 0.6816(3) 0.0410(11) Uani 1 1 d . . . C68 C 0.0086(4) 1.0178(4) 0.6901(4) 0.0528(13) Uani 1 1 d . . . H68A H 0.0408 1.0219 0.6336 0.079 Uiso 1 1 calc R . . H68B H 0.0518 0.9702 0.7389 0.079 Uiso 1 1 calc R . . H68C H -0.0102 1.0812 0.7032 0.079 Uiso 1 1 calc R . . C69 C -0.1334(4) 0.9852(4) 0.7684(4) 0.0514(13) Uani 1 1 d . . . H69A H -0.1865 0.9594 0.7654 0.077 Uiso 1 1 calc R . . H69B H -0.1577 1.0512 0.7754 0.077 Uiso 1 1 calc R . . H69C H -0.0898 0.9442 0.8199 0.077 Uiso 1 1 calc R . . C70 C -0.1457(4) 1.0611(4) 0.6036(4) 0.0547(14) Uani 1 1 d . . . H70A H -0.1993 1.0386 0.5930 0.082 Uiso 1 1 calc R . . H70B H -0.1101 1.0690 0.5492 0.082 Uiso 1 1 calc R . . H70C H -0.1696 1.1232 0.6188 0.082 Uiso 1 1 calc R . . C71 C 0.2082(3) 0.6176(3) 0.2584(3) 0.0300(9) Uani 1 1 d . . . C72 C 0.1304(3) 0.7016(3) 0.2421(3) 0.0380(10) Uani 1 1 d . . . H72A H 0.0831 0.7093 0.2847 0.046 Uiso 1 1 calc R . . C73 C 0.1228(3) 0.7731(3) 0.1634(3) 0.0392(11) Uani 1 1 d . . . H73A H 0.0693 0.8294 0.1526 0.047 Uiso 1 1 calc R . . C74 C 0.1912(3) 0.7656(3) 0.0989(3) 0.0351(10) Uani 1 1 d . . . C75 C 0.2666(3) 0.6818(3) 0.1166(3) 0.0347(10) Uani 1 1 d . . . H75A H 0.3144 0.6745 0.0745 0.042 Uiso 1 1 calc R . . C76 C 0.2749(3) 0.6073(3) 0.1947(3) 0.0337(10) Uani 1 1 d . . . H76A H 0.3265 0.5495 0.2039 0.040 Uiso 1 1 calc R . . C77 C 0.1768(4) 0.8437(3) 0.0093(3) 0.0423(11) Uani 1 1 d . . . C78 C 0.0980(4) 0.8367(5) -0.0474(4) 0.0627(16) Uani 1 1 d . . . H78A H 0.0418 0.8377 -0.0122 0.094 Uiso 1 1 calc R . . H78B H 0.1192 0.7763 -0.0659 0.094 Uiso 1 1 calc R . . H78C H 0.0820 0.8917 -0.1008 0.094 Uiso 1 1 calc R . . C79 C 0.1491(5) 0.9450(4) 0.0272(4) 0.0628(16) Uani 1 1 d . . . H79A H 0.0888 0.9565 0.0567 0.094 Uiso 1 1 calc R . . H79B H 0.1421 0.9943 -0.0300 0.094 Uiso 1 1 calc R . . H79C H 0.1987 0.9485 0.0661 0.094 Uiso 1 1 calc R . . C80 C 0.2668(4) 0.8315(4) -0.0422(3) 0.0527(14) Uani 1 1 d . . . H80A H 0.2848 0.7686 -0.0562 0.079 Uiso 1 1 calc R . . H80B H 0.3182 0.8350 -0.0053 0.079 Uiso 1 1 calc R . . H80C H 0.2555 0.8832 -0.0981 0.079 Uiso 1 1 calc R . . C81 C 0.2544(4) 0.2632(4) 0.2150(4) 0.0557(14) Uani 1 1 d . . . H81A H 0.1921 0.3081 0.2248 0.067 Uiso 1 1 calc R . . C82 C 0.6887(4) 0.2701(4) 0.3110(4) 0.0627(16) Uani 1 1 d D . . H82A H 0.6779 0.3354 0.3218 0.075 Uiso 1 1 calc R A 1 C83 C 0.0818(4) 0.5834(4) 0.0672(4) 0.0527(13) Uani 1 1 d . . . H83A H 0.1078 0.6293 0.0878 0.063 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 Cl1 0.1120(17) 0.1243(18) 0.1136(17) -0.0453(14) 0.0367(14) -0.0786(15) Cl2 0.1150(15) 0.0959(13) 0.0415(8) -0.0168(8) -0.0122(9) -0.0208(11) Cl3 0.0724(10) 0.0554(8) 0.0477(8) -0.0171(6) -0.0085(7) -0.0067(7) Cl4 0.083(2) 0.151(4) 0.099(3) -0.074(3) 0.0484(19) -0.050(2) Cl5 0.103(3) 0.098(2) 0.082(2) -0.0058(18) -0.0199(19) -0.0122(19) Cl4' 0.167(7) 0.106(5) 0.098(5) -0.060(4) 0.033(4) -0.071(5) Cl5' 0.088(4) 0.085(4) 0.193(9) -0.011(5) -0.024(5) -0.012(3) Cl6 0.0638(10) 0.0983(14) 0.1050(14) -0.0430(11) 0.0056(9) -0.0326(9) Cl7 0.1111(16) 0.1052(15) 0.0999(15) -0.0473(13) 0.0521(13) -0.0467(13) Cl8 0.0709(11) 0.0838(12) 0.0933(13) 0.0075(10) -0.0242(10) -0.0328(9) Cl9 0.0736(10) 0.0610(9) 0.0574(8) -0.0086(7) 0.0027(7) -0.0269(8) O1 0.0385(16) 0.0277(15) 0.0214(14) -0.0021(11) -0.0026(12) -0.0115(12) O2 0.0274(15) 0.0270(15) 0.0342(15) -0.0068(12) 0.0015(12) -0.0103(12) O3 0.0314(16) 0.0238(16) 0.0461(18) 0.0014(13) -0.0048(13) -0.0086(13) O4 0.0367(17) 0.0330(18) 0.054(2) 0.0042(15) -0.0085(15) -0.0161(14) O5 0.0453(19) 0.0267(17) 0.0475(19) -0.0037(14) 0.0075(15) -0.0100(14) O6 0.0502(19) 0.0266(16) 0.0423(18) -0.0080(13) 0.0116(15) -0.0153(14) O7 0.055(2) 0.0394(19) 0.052(2) -0.0083(16) 0.0094(17) -0.0181(17) N1 0.0283(18) 0.0262(18) 0.0310(18) -0.0071(14) 0.0008(15) -0.0070(14) N2 0.0320(19) 0.0240(18) 0.0288(19) 0.0006(14) -0.0011(14) -0.0092(14) C1 0.030(2) 0.024(2) 0.0214(19) -0.0024(15) -0.0033(16) -0.0095(16) C2 0.0237(19) 0.026(2) 0.026(2) -0.0036(16) 0.0002(15) -0.0094(16) C4 0.034(2) 0.027(2) 0.032(2) -0.0113(18) 0.0022(18) -0.0097(18) C5 0.028(2) 0.031(2) 0.037(2) -0.0056(19) -0.0008(18) -0.0119(18) C6 0.0253(19) 0.023(2) 0.0242(19) -0.0028(15) -0.0032(15) -0.0079(16) C7 0.0237(19) 0.0216(19) 0.0243(19) -0.0007(15) -0.0033(15) -0.0059(15) C8 0.032(2) 0.023(2) 0.025(2) 0.0000(16) -0.0008(17) -0.0095(17) C9 0.027(2) 0.0175(19) 0.028(2) 0.0012(15) 0.0029(16) -0.0055(16) C10 0.026(2) 0.024(2) 0.026(2) -0.0005(16) -0.0016(16) -0.0060(16) C11 0.025(2) 0.031(2) 0.036(2) 0.0003(18) -0.0092(18) -0.0029(17) C12 0.035(2) 0.021(2) 0.041(2) -0.0051(18) -0.0008(19) -0.0027(17) C13 0.035(2) 0.026(2) 0.025(2) 0.0089(17) -0.0046(17) -0.0032(18) C14 0.037(2) 0.029(2) 0.026(2) 0.0075(17) -0.0006(18) -0.0125(19) C15 0.040(2) 0.036(2) 0.024(2) 0.0080(18) -0.0106(18) -0.009(2) C16 0.038(2) 0.036(2) 0.022(2) -0.0086(17) -0.0020(17) -0.0115(19) C17 0.042(3) 0.040(2) 0.0178(19) 0.0027(17) 0.0027(17) -0.015(2) C18 0.045(3) 0.018(2) 0.034(2) -0.0062(17) -0.0018(19) -0.0087(18) C19 0.034(2) 0.023(2) 0.034(2) -0.0048(17) 0.0071(18) -0.0004(17) C20 0.039(2) 0.020(2) 0.036(2) 0.0003(17) 0.0022(19) -0.0146(18) C21 0.025(2) 0.028(2) 0.036(2) -0.0036(17) 0.0040(17) -0.0123(17) C22 0.035(2) 0.040(2) 0.024(2) -0.0067(18) -0.0050(17) -0.0127(19) C23 0.034(2) 0.020(2) 0.038(2) 0.0062(17) -0.0084(19) -0.0018(17) C24 0.024(2) 0.033(2) 0.039(2) -0.0019(19) -0.0043(18) -0.0113(18) C25 0.030(2) 0.023(2) 0.040(2) -0.0023(18) 0.0023(18) -0.0003(17) C26 0.034(2) 0.029(2) 0.031(2) -0.0105(17) -0.0037(17) -0.0101(18) C27 0.036(2) 0.027(2) 0.032(2) 0.0051(17) 0.0044(18) -0.0176(18) C28 0.032(2) 0.038(2) 0.027(2) -0.0062(18) -0.0062(17) -0.0112(19) C29 0.045(3) 0.024(2) 0.028(2) 0.0088(17) -0.0024(19) -0.0115(19) C30 0.038(2) 0.0147(19) 0.040(2) 0.0025(17) 0.0005(19) -0.0005(17) C31 0.028(2) 0.028(2) 0.035(2) 0.0029(18) -0.0049(18) -0.0008(17) C32 0.037(2) 0.036(2) 0.021(2) -0.0015(17) 0.0057(17) -0.0135(19) C33 0.026(2) 0.024(2) 0.0241(19) -0.0034(16) 0.0057(16) -0.0065(16) C34 0.040(2) 0.0180(19) 0.035(2) -0.0045(17) -0.0031(19) -0.0086(17) C35 0.022(2) 0.031(2) 0.037(2) -0.0054(18) 0.0052(17) -0.0063(17) C36 0.042(2) 0.018(2) 0.037(2) 0.0039(17) -0.0017(19) -0.0092(18) C37 0.031(2) 0.033(2) 0.033(2) -0.0059(18) -0.0056(18) -0.0129(18) C38 0.040(2) 0.037(2) 0.023(2) 0.0023(18) -0.0050(18) -0.010(2) C39 0.035(2) 0.029(2) 0.027(2) -0.0099(17) 0.0047(17) -0.0050(18) C40 0.029(2) 0.029(2) 0.027(2) -0.0037(17) 0.0076(17) -0.0040(17) C41 0.025(2) 0.027(2) 0.032(2) -0.0044(17) 0.0006(16) -0.0107(16) C42 0.032(2) 0.026(2) 0.026(2) -0.0088(16) -0.0042(17) -0.0086(17) C43 0.033(2) 0.036(2) 0.025(2) -0.0013(17) 0.0072(17) -0.0139(18) C44 0.026(2) 0.027(2) 0.030(2) 0.0002(17) 0.0048(17) -0.0116(17) C45 0.035(2) 0.033(2) 0.0224(19) -0.0059(17) 0.0058(17) -0.0118(18) C46 0.022(2) 0.032(2) 0.036(2) -0.0009(18) -0.0049(17) -0.0076(17) C47 0.035(2) 0.025(2) 0.033(2) 0.0014(17) 0.0023(18) -0.0172(18) C48 0.040(2) 0.023(2) 0.028(2) -0.0086(17) 0.0020(18) -0.0072(18) C49 0.028(2) 0.031(2) 0.029(2) -0.0014(17) 0.0076(17) -0.0070(17) C3 0.026(2) 0.031(2) 0.029(2) 0.0002(17) 0.0050(16) -0.0126(18) C51 0.028(2) 0.024(2) 0.0244(19) -0.0035(16) -0.0039(16) -0.0105(16) C52 0.024(2) 0.029(2) 0.028(2) -0.0016(17) 0.0059(16) -0.0101(16) C53 0.033(2) 0.033(2) 0.035(2) -0.0087(18) -0.0032(18) -0.0126(18) C54 0.032(2) 0.030(2) 0.036(2) -0.0041(18) -0.0010(18) -0.0169(18) C55 0.037(2) 0.024(2) 0.029(2) -0.0045(17) -0.0040(17) -0.0153(17) C56 0.036(2) 0.024(2) 0.0212(19) -0.0055(16) -0.0022(16) -0.0085(17) C57 0.031(2) 0.027(2) 0.0178(18) -0.0011(15) 0.0044(15) -0.0096(17) C58 0.026(2) 0.026(2) 0.026(2) -0.0075(16) 0.0037(16) -0.0054(16) C59 0.029(2) 0.035(2) 0.030(2) 0.0031(18) -0.0086(18) -0.0042(18) C50 0.034(2) 0.023(2) 0.0196(18) -0.0026(15) 0.0010(16) -0.0065(17) C60 0.0229(19) 0.026(2) 0.029(2) 0.0002(16) -0.0037(16) -0.0111(16) C61 0.023(2) 0.027(2) 0.040(2) -0.0123(18) 0.0035(17) -0.0077(16) C62 0.042(3) 0.029(2) 0.037(2) -0.0041(19) 0.006(2) -0.0081(19) C63 0.045(3) 0.038(3) 0.033(2) -0.012(2) 0.007(2) -0.009(2) C64 0.026(2) 0.030(2) 0.050(3) -0.016(2) 0.0066(19) -0.0076(17) C65 0.041(3) 0.026(2) 0.040(2) -0.0059(19) 0.000(2) -0.0079(19) C66 0.041(2) 0.032(2) 0.030(2) -0.0079(18) -0.0007(19) -0.0078(19) C67 0.040(3) 0.033(2) 0.053(3) -0.017(2) 0.006(2) -0.011(2) C68 0.054(3) 0.051(3) 0.066(4) -0.023(3) 0.010(3) -0.027(3) C69 0.059(3) 0.040(3) 0.063(3) -0.028(3) 0.018(3) -0.015(2) C70 0.055(3) 0.030(3) 0.068(4) -0.015(2) 0.001(3) 0.004(2) C71 0.037(2) 0.028(2) 0.023(2) 0.0024(16) -0.0039(17) -0.0142(18) C72 0.042(3) 0.038(3) 0.030(2) -0.0007(19) 0.0048(19) -0.014(2) C73 0.044(3) 0.029(2) 0.037(2) 0.0004(19) -0.002(2) -0.007(2) C74 0.045(3) 0.033(2) 0.028(2) 0.0029(18) -0.0052(19) -0.021(2) C75 0.039(2) 0.039(2) 0.029(2) -0.0015(18) 0.0036(18) -0.022(2) C76 0.037(2) 0.035(2) 0.027(2) -0.0006(18) -0.0032(18) -0.0127(19) C77 0.053(3) 0.039(3) 0.032(2) 0.003(2) -0.004(2) -0.020(2) C78 0.066(4) 0.076(4) 0.038(3) 0.013(3) -0.015(3) -0.031(3) C79 0.091(5) 0.039(3) 0.048(3) 0.002(2) 0.011(3) -0.016(3) C80 0.069(4) 0.053(3) 0.032(3) 0.008(2) 0.004(2) -0.027(3) C81 0.062(4) 0.044(3) 0.059(3) -0.020(3) -0.004(3) -0.008(3) C82 0.054(3) 0.063(4) 0.082(4) -0.038(3) 0.009(3) -0.018(3) C83 0.055(3) 0.055(3) 0.054(3) -0.014(3) -0.005(3) -0.025(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 C81 1.732(6) . ? Cl2 C81 1.751(6) . ? Cl3 C81 1.744(6) . ? Cl4 C82 1.668(6) . ? Cl5 C82 1.853(7) . ? Cl4' C82 1.929(9) . ? Cl5' C82 1.682(8) . ? Cl6 C82 1.721(6) . ? Cl7 C83 1.737(6) . ? Cl8 C83 1.744(6) . ? Cl9 C83 1.758(6) . ? O1 C1 1.431(5) . ? O1 H1 0.8401 . ? O2 C2 1.421(5) . ? O2 H2 0.8401 . ? O3 C3 1.203(5) . ? O4 C4 1.204(5) . ? O5 C5 1.214(5) . ? O6 C9 1.371(5) . ? O6 C8 1.391(5) . ? O7 C9 1.205(5) . ? N1 C8 1.264(5) . ? N1 C61 1.427(5) . ? N2 C10 1.266(5) . ? N2 C71 1.419(5) . ? C1 C51 1.514(5) . ? C1 C6 1.528(5) . ? C1 C50 1.573(6) . ? C2 C60 1.502(6) . ? C2 C7 1.531(5) . ? C2 C33 1.580(5) . ? C4 C26 1.512(6) . ? C4 C58 1.525(6) . ? C5 C53 1.507(6) . ? C5 C21 1.509(6) . ? C6 C7 1.369(6) . ? C6 C10 1.482(5) . ? C7 C8 1.471(5) . ? C9 C10 1.471(6) . ? C11 C59 1.391(6) . ? C11 C46 1.445(6) . ? C11 C31 1.458(6) . ? C12 C30 1.388(6) . ? C12 C18 1.447(6) . ? C12 C19 1.459(6) . ? C13 C15 1.390(7) . ? C13 C23 1.439(6) . ? C13 C29 1.447(6) . ? C14 C29 1.401(6) . ? C14 C17 1.442(6) . ? C14 C27 1.449(6) . ? C15 C59 1.439(6) . ? C15 C38 1.447(7) . ? C16 C22 1.400(6) . ? C16 C26 1.426(6) . ? C16 C45 1.449(6) . ? C17 C38 1.391(6) . ? C17 C32 1.453(6) . ? C18 C34 1.387(6) . ? C18 C48 1.449(6) . ? C19 C25 1.381(7) . ? C19 C39 1.451(6) . ? C20 C36 1.392(6) . ? C20 C47 1.449(6) . ? C20 C34 1.451(6) . ? C21 C44 1.379(6) . ? C21 C24 1.438(6) . ? C22 C28 1.436(6) . ? C22 C38 1.447(6) . ? C23 C31 1.394(6) . ? C23 C30 1.441(7) . ? C24 C46 1.397(6) . ? C24 C37 1.445(6) . ? C25 C35 1.450(6) . ? C25 C31 1.453(6) . ? C26 C53 1.381(6) . ? C27 C47 1.388(6) . ? C27 C43 1.454(6) . ? C28 C37 1.391(6) . ? C28 C59 1.446(6) . ? C29 C36 1.436(6) . ? C30 C36 1.466(6) . ? C32 C45 1.382(6) . ? C32 C43 1.424(6) . ? C33 C58 1.372(6) . ? C33 C52 1.468(5) . ? C34 C55 1.456(6) . ? C35 C49 1.392(6) . ? C35 C46 1.436(6) . ? C37 C53 1.438(6) . ? C39 C40 1.379(6) . ? C39 C48 1.431(6) . ? C40 C49 1.444(6) . ? C40 C57 1.450(6) . ? C41 C54 1.395(6) . ? C41 C52 1.429(6) . ? C41 C60 1.439(5) . ? C42 C55 1.383(6) . ? C42 C51 1.431(6) . ? C42 C56 1.441(6) . ? C43 C52 1.399(6) . ? C44 C49 1.427(6) . ? C44 C3 1.513(6) . ? C45 C58 1.457(6) . ? C47 C54 1.450(6) . ? C48 C56 1.397(6) . ? C3 C57 1.523(6) . ? C51 C60 1.349(6) . ? C54 C55 1.446(6) . ? C56 C50 1.453(6) . ? C57 C50 1.385(6) . ? C61 C66 1.372(6) . ? C61 C62 1.386(6) . ? C62 C63 1.386(6) . ? C62 H62A 0.9500 . ? C63 C64 1.397(7) . ? C63 H63A 0.9500 . ? C64 C65 1.386(7) . ? C64 C67 1.530(6) . ? C65 C66 1.389(6) . ? C65 H65A 0.9500 . ? C66 H66A 0.9500 . ? C67 C69 1.534(7) . ? C67 C70 1.534(7) . ? C67 C68 1.540(7) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 C76 1.379(6) . ? C71 C72 1.400(6) . ? C72 C73 1.380(6) . ? C72 H72A 0.9500 . ? C73 C74 1.402(7) . ? C73 H73A 0.9500 . ? C74 C75 1.378(7) . ? C74 C77 1.537(6) . ? C75 C76 1.396(6) . ? C75 H75A 0.9500 . ? C76 H76A 0.9500 . ? C77 C78 1.517(7) . ? C77 C80 1.521(8) . ? C77 C79 1.547(8) . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 H81A 1.0000 . ? C82 H82A 1.0000 . ? C83 H83A 1.0000 . ? 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 C1 O1 H1 100.9 . . ? C2 O2 H2 105.1 . . ? C9 O6 C8 121.1(3) . . ? C8 N1 C61 123.0(4) . . ? C10 N2 C71 124.7(4) . . ? O1 C1 C51 106.6(3) . . ? O1 C1 C6 110.3(3) . . ? C51 C1 C6 110.8(3) . . ? O1 C1 C50 108.1(3) . . ? C51 C1 C50 99.0(3) . . ? C6 C1 C50 120.8(3) . . ? O2 C2 C60 105.8(3) . . ? O2 C2 C7 110.2(3) . . ? C60 C2 C7 110.5(3) . . ? O2 C2 C33 109.0(3) . . ? C60 C2 C33 99.6(3) . . ? C7 C2 C33 120.4(3) . . ? O4 C4 C26 125.6(4) . . ? O4 C4 C58 128.9(4) . . ? C26 C4 C58 105.2(3) . . ? O5 C5 C53 128.2(4) . . ? O5 C5 C21 128.3(4) . . ? C53 C5 C21 103.4(3) . . ? C7 C6 C10 117.3(3) . . ? C7 C6 C1 124.0(3) . . ? C10 C6 C1 117.5(3) . . ? C6 C7 C8 119.1(3) . . ? C6 C7 C2 124.3(3) . . ? C8 C7 C2 115.8(3) . . ? N1 C8 O6 120.2(4) . . ? N1 C8 C7 120.8(4) . . ? O6 C8 C7 118.9(3) . . ? O7 C9 O6 116.2(4) . . ? O7 C9 C10 126.2(4) . . ? O6 C9 C10 117.3(3) . . ? N2 C10 C9 122.3(4) . . ? N2 C10 C6 120.2(4) . . ? C9 C10 C6 117.5(3) . . ? C59 C11 C46 120.5(4) . . ? C59 C11 C31 119.6(4) . . ? C46 C11 C31 107.5(4) . . ? C30 C12 C18 121.1(4) . . ? C30 C12 C19 119.3(4) . . ? C18 C12 C19 108.0(4) . . ? C15 C13 C23 120.0(4) . . ? C15 C13 C29 120.3(4) . . ? C23 C13 C29 107.9(4) . . ? C29 C14 C17 119.8(4) . . ? C29 C14 C27 119.3(4) . . ? C17 C14 C27 108.3(4) . . ? C13 C15 C59 120.7(4) . . ? C13 C15 C38 119.8(4) . . ? C59 C15 C38 107.8(4) . . ? C22 C16 C26 122.2(4) . . ? C22 C16 C45 119.6(4) . . ? C26 C16 C45 109.6(4) . . ? C38 C17 C14 120.3(4) . . ? C38 C17 C32 119.7(4) . . ? C14 C17 C32 107.5(4) . . ? C34 C18 C12 119.6(4) . . ? C34 C18 C48 119.5(4) . . ? C12 C18 C48 107.6(4) . . ? C25 C19 C39 119.8(4) . . ? C25 C19 C12 119.8(4) . . ? C39 C19 C12 107.3(4) . . ? C36 C20 C47 120.1(4) . . ? C36 C20 C34 120.2(4) . . ? C47 C20 C34 107.5(4) . . ? C44 C21 C24 119.0(4) . . ? C44 C21 C5 126.7(4) . . ? C24 C21 C5 106.8(4) . . ? C16 C22 C28 118.1(4) . . ? C16 C22 C38 120.5(4) . . ? C28 C22 C38 108.2(4) . . ? C31 C23 C13 119.9(4) . . ? C31 C23 C30 119.4(4) . . ? C13 C23 C30 108.7(4) . . ? C46 C24 C21 121.6(4) . . ? C46 C24 C37 119.5(4) . . ? C21 C24 C37 108.9(4) . . ? C19 C25 C35 119.9(4) . . ? C19 C25 C31 120.5(4) . . ? C35 C25 C31 107.8(4) . . ? C53 C26 C16 119.4(4) . . ? C53 C26 C4 125.1(4) . . ? C16 C26 C4 107.5(4) . . ? C47 C27 C14 120.8(4) . . ? C47 C27 C43 120.3(4) . . ? C14 C27 C43 107.4(4) . . ? C37 C28 C22 119.0(4) . . ? C37 C28 C59 120.7(4) . . ? C22 C28 C59 107.8(4) . . ? C14 C29 C36 120.0(4) . . ? C14 C29 C13 119.7(4) . . ? C36 C29 C13 108.3(4) . . ? C12 C30 C23 121.1(4) . . ? C12 C30 C36 119.2(4) . . ? C23 C30 C36 107.3(4) . . ? C23 C31 C25 119.8(4) . . ? C23 C31 C11 120.0(4) . . ? C25 C31 C11 107.8(4) . . ? C45 C32 C43 118.5(4) . . ? C45 C32 C17 120.7(4) . . ? C43 C32 C17 108.5(4) . . ? C58 C33 C52 117.6(4) . . ? C58 C33 C2 135.3(4) . . ? C52 C33 C2 104.7(3) . . ? C18 C34 C20 120.3(4) . . ? C18 C34 C55 119.8(4) . . ? C20 C34 C55 108.1(4) . . ? C49 C35 C46 118.6(4) . . ? C49 C35 C25 120.0(4) . . ? C46 C35 C25 108.1(4) . . ? C20 C36 C29 120.4(4) . . ? C20 C36 C30 119.7(4) . . ? C29 C36 C30 107.8(4) . . ? C28 C37 C53 122.0(4) . . ? C28 C37 C24 120.0(4) . . ? C53 C37 C24 108.5(4) . . ? C17 C38 C22 119.6(4) . . ? C17 C38 C15 120.1(4) . . ? C22 C38 C15 107.8(4) . . ? C40 C39 C48 118.5(4) . . ? C40 C39 C19 120.2(4) . . ? C48 C39 C19 108.3(4) . . ? C39 C40 C49 120.2(4) . . ? C39 C40 C57 122.5(4) . . ? C49 C40 C57 109.5(4) . . ? C54 C41 C52 120.9(4) . . ? C54 C41 C60 121.0(4) . . ? C52 C41 C60 107.7(3) . . ? C55 C42 C51 121.5(4) . . ? C55 C42 C56 120.5(4) . . ? C51 C42 C56 107.4(3) . . ? C52 C43 C32 119.6(4) . . ? C52 C43 C27 119.9(4) . . ? C32 C43 C27 108.3(4) . . ? C21 C44 C49 119.2(4) . . ? C21 C44 C3 125.4(4) . . ? C49 C44 C3 107.7(4) . . ? C32 C45 C16 119.8(4) . . ? C32 C45 C58 122.6(4) . . ? C16 C45 C58 109.5(4) . . ? C24 C46 C35 118.7(4) . . ? C24 C46 C11 120.2(4) . . ? C35 C46 C11 108.8(4) . . ? C27 C47 C20 119.4(4) . . ? C27 C47 C54 119.4(4) . . ? C20 C47 C54 108.5(4) . . ? C56 C48 C39 119.3(4) . . ? C56 C48 C18 120.7(4) . . ? C39 C48 C18 108.7(4) . . ? C35 C49 C44 122.3(4) . . ? C35 C49 C40 119.7(4) . . ? C44 C49 C40 109.6(4) . . ? O3 C3 C44 126.9(4) . . ? O3 C3 C57 127.5(4) . . ? C44 C3 C57 105.0(3) . . ? C60 C51 C42 120.3(4) . . ? C60 C51 C1 124.7(4) . . ? C42 C51 C1 109.8(3) . . ? C43 C52 C41 119.4(4) . . ? C43 C52 C33 122.0(4) . . ? C41 C52 C33 109.3(3) . . ? C26 C53 C37 118.6(4) . . ? C26 C53 C5 126.7(4) . . ? C37 C53 C5 107.2(4) . . ? C41 C54 C55 118.9(4) . . ? C41 C54 C47 120.0(4) . . ? C55 C54 C47 107.8(4) . . ? C42 C55 C54 118.4(4) . . ? C42 C55 C34 120.1(4) . . ? C54 C55 C34 108.0(4) . . ? C48 C56 C42 119.1(4) . . ? C48 C56 C50 122.6(4) . . ? C42 C56 C50 109.3(3) . . ? C50 C57 C40 119.8(4) . . ? C50 C57 C3 128.4(4) . . ? C40 C57 C3 106.3(3) . . ? C33 C58 C45 119.6(4) . . ? C33 C58 C4 129.8(4) . . ? C45 C58 C4 105.7(3) . . ? C11 C59 C15 119.8(4) . . ? C11 C59 C28 119.2(4) . . ? C15 C59 C28 108.3(4) . . ? C57 C50 C56 117.2(4) . . ? C57 C50 C1 134.3(4) . . ? C56 C50 C1 105.7(3) . . ? C51 C60 C41 119.3(4) . . ? C51 C60 C2 125.6(3) . . ? C41 C60 C2 109.6(3) . . ? C66 C61 C62 118.9(4) . . ? C66 C61 N1 124.1(4) . . ? C62 C61 N1 116.9(4) . . ? C63 C62 C61 120.1(4) . . ? C63 C62 H62A 119.9 . . ? C61 C62 H62A 119.9 . . ? C62 C63 C64 121.9(4) . . ? C62 C63 H63A 119.1 . . ? C64 C63 H63A 119.1 . . ? C65 C64 C63 116.6(4) . . ? C65 C64 C67 121.6(4) . . ? C63 C64 C67 121.8(4) . . ? C64 C65 C66 121.9(4) . . ? C64 C65 H65A 119.0 . . ? C66 C65 H65A 119.0 . . ? C61 C66 C65 120.6(4) . . ? C61 C66 H66A 119.7 . . ? C65 C66 H66A 119.7 . . ? C64 C67 C69 111.3(4) . . ? C64 C67 C70 110.9(4) . . ? C69 C67 C70 108.6(4) . . ? C64 C67 C68 108.2(4) . . ? C69 C67 C68 109.4(4) . . ? C70 C67 C68 108.4(4) . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C67 C69 H69A 109.5 . . ? C67 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C67 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C67 C70 H70A 109.5 . . ? C67 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C67 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C76 C71 C72 119.2(4) . . ? C76 C71 N2 119.0(4) . . ? C72 C71 N2 121.3(4) . . ? C73 C72 C71 119.4(4) . . ? C73 C72 H72A 120.3 . . ? C71 C72 H72A 120.3 . . ? C72 C73 C74 122.4(4) . . ? C72 C73 H73A 118.8 . . ? C74 C73 H73A 118.8 . . ? C75 C74 C73 116.8(4) . . ? C75 C74 C77 122.2(4) . . ? C73 C74 C77 120.7(4) . . ? C74 C75 C76 122.0(4) . . ? C74 C75 H75A 119.0 . . ? C76 C75 H75A 119.0 . . ? C71 C76 C75 120.1(4) . . ? C71 C76 H76A 120.0 . . ? C75 C76 H76A 120.0 . . ? C78 C77 C80 109.2(5) . . ? C78 C77 C74 108.8(4) . . ? C80 C77 C74 111.7(4) . . ? C78 C77 C79 109.5(5) . . ? C80 C77 C79 107.8(4) . . ? C74 C77 C79 109.9(4) . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C77 C79 H79A 109.5 . . ? C77 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C77 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C77 C80 H80A 109.5 . . ? C77 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C77 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? Cl1 C81 Cl3 110.5(3) . . ? Cl1 C81 Cl2 112.7(4) . . ? Cl3 C81 Cl2 109.9(3) . . ? Cl1 C81 H81A 107.9 . . ? Cl3 C81 H81A 107.9 . . ? Cl2 C81 H81A 107.9 . . ? Cl4 C82 Cl5' 63.9(5) . . ? Cl4 C82 Cl6 115.9(4) . . ? Cl5' C82 Cl6 118.5(4) . . ? Cl4 C82 Cl5 106.3(4) . . ? Cl5' C82 Cl5 42.5(4) . . ? Cl6 C82 Cl5 103.5(3) . . ? Cl4 C82 Cl4' 35.9(3) . . ? Cl5' C82 Cl4' 99.6(6) . . ? Cl6 C82 Cl4' 103.0(4) . . ? Cl5 C82 Cl4' 141.4(5) . . ? Cl4 C82 H82A 110.3 . . ? Cl5' C82 H82A 127.8 . . ? Cl6 C82 H82A 110.3 . . ? Cl5 C82 H82A 110.3 . . ? Cl4' C82 H82A 86.0 . . ? Cl7 C83 Cl8 111.1(3) . . ? Cl7 C83 Cl9 111.3(3) . . ? Cl8 C83 Cl9 110.0(3) . . ? Cl7 C83 H83A 108.1 . . ? Cl8 C83 H83A 108.1 . . ? Cl9 C83 H83A 108.1 . . ? 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 O1 C1 C6 C7 119.9(4) . . . . ? C51 C1 C6 C7 2.2(5) . . . . ? C50 C1 C6 C7 -112.7(4) . . . . ? O1 C1 C6 C10 -47.0(5) . . . . ? C51 C1 C6 C10 -164.8(3) . . . . ? C50 C1 C6 C10 80.3(4) . . . . ? C10 C6 C7 C8 -3.8(5) . . . . ? C1 C6 C7 C8 -170.8(3) . . . . ? C10 C6 C7 C2 166.2(3) . . . . ? C1 C6 C7 C2 -0.8(6) . . . . ? O2 C2 C7 C6 -118.0(4) . . . . ? C60 C2 C7 C6 -1.3(5) . . . . ? C33 C2 C7 C6 113.8(4) . . . . ? O2 C2 C7 C8 52.3(4) . . . . ? C60 C2 C7 C8 168.9(3) . . . . ? C33 C2 C7 C8 -75.9(5) . . . . ? C61 N1 C8 O6 2.1(6) . . . . ? C61 N1 C8 C7 178.4(4) . . . . ? C9 O6 C8 N1 -161.8(4) . . . . ? C9 O6 C8 C7 21.8(5) . . . . ? C6 C7 C8 N1 163.3(4) . . . . ? C2 C7 C8 N1 -7.6(5) . . . . ? C6 C7 C8 O6 -20.4(5) . . . . ? C2 C7 C8 O6 168.8(3) . . . . ? C8 O6 C9 O7 -172.8(4) . . . . ? C8 O6 C9 C10 1.3(5) . . . . ? C71 N2 C10 C9 -12.0(6) . . . . ? C71 N2 C10 C6 167.7(4) . . . . ? O7 C9 C10 N2 -32.3(7) . . . . ? O6 C9 C10 N2 154.2(4) . . . . ? O7 C9 C10 C6 148.0(4) . . . . ? O6 C9 C10 C6 -25.5(5) . . . . ? C7 C6 C10 N2 -153.3(4) . . . . ? C1 C6 C10 N2 14.5(5) . . . . ? C7 C6 C10 C9 26.4(5) . . . . ? C1 C6 C10 C9 -165.8(3) . . . . ? C23 C13 C15 C59 -0.6(6) . . . . ? C29 C13 C15 C59 -139.1(4) . . . . ? C23 C13 C15 C38 137.8(4) . . . . ? C29 C13 C15 C38 -0.7(6) . . . . ? C29 C14 C17 C38 -1.7(6) . . . . ? C27 C14 C17 C38 -143.2(4) . . . . ? C29 C14 C17 C32 140.2(4) . . . . ? C27 C14 C17 C32 -1.3(5) . . . . ? C30 C12 C18 C34 -0.4(6) . . . . ? C19 C12 C18 C34 -143.2(4) . . . . ? C30 C12 C18 C48 140.3(4) . . . . ? C19 C12 C18 C48 -2.5(5) . . . . ? C30 C12 C19 C25 0.1(6) . . . . ? C18 C12 C19 C25 143.8(4) . . . . ? C30 C12 C19 C39 -141.1(4) . . . . ? C18 C12 C19 C39 2.6(5) . . . . ? O5 C5 C21 C44 -52.0(7) . . . . ? C53 C5 C21 C44 127.1(4) . . . . ? O5 C5 C21 C24 159.0(4) . . . . ? C53 C5 C21 C24 -21.9(4) . . . . ? C26 C16 C22 C28 -7.4(6) . . . . ? C45 C16 C22 C28 137.0(4) . . . . ? C26 C16 C22 C38 -143.9(4) . . . . ? C45 C16 C22 C38 0.5(6) . . . . ? C15 C13 C23 C31 -0.4(6) . . . . ? C29 C13 C23 C31 142.7(4) . . . . ? C15 C13 C23 C30 -142.8(4) . . . . ? C29 C13 C23 C30 0.3(4) . . . . ? C44 C21 C24 C46 8.1(6) . . . . ? C5 C21 C24 C46 159.8(4) . . . . ? C44 C21 C24 C37 -137.3(4) . . . . ? C5 C21 C24 C37 14.5(4) . . . . ? C39 C19 C25 C35 -2.1(6) . . . . ? C12 C19 C25 C35 -138.5(4) . . . . ? C39 C19 C25 C31 136.4(4) . . . . ? C12 C19 C25 C31 -0.1(6) . . . . ? C22 C16 C26 C53 5.0(6) . . . . ? C45 C16 C26 C53 -142.5(4) . . . . ? C22 C16 C26 C4 155.4(4) . . . . ? C45 C16 C26 C4 7.9(5) . . . . ? O4 C4 C26 C53 -40.4(7) . . . . ? C58 C4 C26 C53 133.6(4) . . . . ? O4 C4 C26 C16 171.4(4) . . . . ? C58 C4 C26 C16 -14.6(4) . . . . ? C29 C14 C27 C47 2.2(6) . . . . ? C17 C14 C27 C47 144.0(4) . . . . ? C29 C14 C27 C43 -141.1(4) . . . . ? C17 C14 C27 C43 0.6(5) . . . . ? C16 C22 C28 C37 2.1(6) . . . . ? C38 C22 C28 C37 143.4(4) . . . . ? C16 C22 C28 C59 -140.3(4) . . . . ? C38 C22 C28 C59 1.1(5) . . . . ? C17 C14 C29 C36 -137.7(4) . . . . ? C27 C14 C29 C36 -0.4(6) . . . . ? C17 C14 C29 C13 0.6(6) . . . . ? C27 C14 C29 C13 138.0(4) . . . . ? C15 C13 C29 C14 0.6(6) . . . . ? C23 C13 C29 C14 -142.3(4) . . . . ? C15 C13 C29 C36 143.2(4) . . . . ? C23 C13 C29 C36 0.3(4) . . . . ? C18 C12 C30 C23 -138.1(4) . . . . ? C19 C12 C30 C23 0.7(6) . . . . ? C18 C12 C30 C36 -0.8(6) . . . . ? C19 C12 C30 C36 138.0(4) . . . . ? C31 C23 C30 C12 -1.7(6) . . . . ? C13 C23 C30 C12 140.9(4) . . . . ? C31 C23 C30 C36 -143.4(4) . . . . ? C13 C23 C30 C36 -0.8(4) . . . . ? C13 C23 C31 C25 -136.6(4) . . . . ? C30 C23 C31 C25 1.8(6) . . . . ? C13 C23 C31 C11 0.9(6) . . . . ? C30 C23 C31 C11 139.3(4) . . . . ? C19 C25 C31 C23 -0.9(6) . . . . ? C35 C25 C31 C23 141.9(4) . . . . ? C19 C25 C31 C11 -143.0(4) . . . . ? C35 C25 C31 C11 -0.2(5) . . . . ? C59 C11 C31 C23 -0.4(6) . . . . ? C46 C11 C31 C23 -142.7(4) . . . . ? C59 C11 C31 C25 141.6(4) . . . . ? C46 C11 C31 C25 -0.7(5) . . . . ? C38 C17 C32 C45 2.2(6) . . . . ? C14 C17 C32 C45 -139.9(4) . . . . ? C38 C17 C32 C43 143.6(4) . . . . ? C14 C17 C32 C43 1.6(5) . . . . ? O2 C2 C33 C58 -116.3(5) . . . . ? C60 C2 C33 C58 133.2(5) . . . . ? C7 C2 C33 C58 12.4(7) . . . . ? O2 C2 C33 C52 82.2(4) . . . . ? C60 C2 C33 C52 -28.4(4) . . . . ? C7 C2 C33 C52 -149.1(3) . . . . ? C12 C18 C34 C20 1.2(6) . . . . ? C48 C18 C34 C20 -134.9(4) . . . . ? C12 C18 C34 C55 139.6(4) . . . . ? C48 C18 C34 C55 3.5(6) . . . . ? C36 C20 C34 C18 -0.8(6) . . . . ? C47 C20 C34 C18 141.5(4) . . . . ? C36 C20 C34 C55 -143.5(4) . . . . ? C47 C20 C34 C55 -1.2(4) . . . . ? C19 C25 C35 C49 3.8(6) . . . . ? C31 C25 C35 C49 -139.3(4) . . . . ? C19 C25 C35 C46 144.1(4) . . . . ? C31 C25 C35 C46 1.0(5) . . . . ? C47 C20 C36 C29 0.0(6) . . . . ? C34 C20 C36 C29 137.7(4) . . . . ? C47 C20 C36 C30 -138.0(4) . . . . ? C34 C20 C36 C30 -0.3(6) . . . . ? C14 C29 C36 C20 -0.7(6) . . . . ? C13 C29 C36 C20 -143.2(4) . . . . ? C14 C29 C36 C30 141.7(4) . . . . ? C13 C29 C36 C30 -0.9(4) . . . . ? C12 C30 C36 C20 1.1(6) . . . . ? C23 C30 C36 C20 143.7(4) . . . . ? C12 C30 C36 C29 -141.5(4) . . . . ? C23 C30 C36 C29 1.0(4) . . . . ? C22 C28 C37 C53 5.5(6) . . . . ? C59 C28 C37 C53 142.9(4) . . . . ? C22 C28 C37 C24 -136.9(4) . . . . ? C59 C28 C37 C24 0.6(6) . . . . ? C46 C24 C37 C28 0.1(6) . . . . ? C21 C24 C37 C28 146.3(4) . . . . ? C46 C24 C37 C53 -146.8(4) . . . . ? C21 C24 C37 C53 -0.7(5) . . . . ? C14 C17 C38 C22 139.0(4) . . . . ? C32 C17 C38 C22 1.7(6) . . . . ? C14 C17 C38 C15 1.6(6) . . . . ? C32 C17 C38 C15 -135.7(4) . . . . ? C16 C22 C38 C17 -3.1(6) . . . . ? C28 C22 C38 C17 -143.3(4) . . . . ? C16 C22 C38 C15 139.0(4) . . . . ? C28 C22 C38 C15 -1.2(5) . . . . ? C13 C15 C38 C17 -0.4(6) . . . . ? C59 C15 C38 C17 142.8(4) . . . . ? C13 C15 C38 C22 -142.3(4) . . . . ? C59 C15 C38 C22 0.9(5) . . . . ? C25 C19 C39 C40 -2.2(6) . . . . ? C12 C19 C39 C40 139.0(4) . . . . ? C25 C19 C39 C48 -142.8(4) . . . . ? C12 C19 C39 C48 -1.6(5) . . . . ? C48 C39 C40 C49 141.5(4) . . . . ? C19 C39 C40 C49 4.7(6) . . . . ? C48 C39 C40 C57 -4.5(6) . . . . ? C19 C39 C40 C57 -141.2(4) . . . . ? C45 C32 C43 C52 -1.1(6) . . . . ? C17 C32 C43 C52 -143.6(4) . . . . ? C45 C32 C43 C27 141.3(4) . . . . ? C17 C32 C43 C27 -1.2(4) . . . . ? C47 C27 C43 C52 -0.9(6) . . . . ? C14 C27 C43 C52 142.6(4) . . . . ? C47 C27 C43 C32 -143.2(4) . . . . ? C14 C27 C43 C32 0.3(4) . . . . ? C24 C21 C44 C49 -3.7(6) . . . . ? C5 C21 C44 C49 -149.4(4) . . . . ? C24 C21 C44 C3 141.7(4) . . . . ? C5 C21 C44 C3 -3.9(6) . . . . ? C43 C32 C45 C16 -142.5(4) . . . . ? C17 C32 C45 C16 -4.7(6) . . . . ? C43 C32 C45 C58 2.7(6) . . . . ? C17 C32 C45 C58 140.5(4) . . . . ? C22 C16 C45 C32 3.3(6) . . . . ? C26 C16 C45 C32 151.8(4) . . . . ? C22 C16 C45 C58 -146.0(4) . . . . ? C26 C16 C45 C58 2.5(5) . . . . ? C21 C24 C46 C35 -4.7(6) . . . . ? C37 C24 C46 C35 137.1(4) . . . . ? C21 C24 C46 C11 -142.7(4) . . . . ? C37 C24 C46 C11 -0.9(6) . . . . ? C49 C35 C46 C24 -2.8(6) . . . . ? C25 C35 C46 C24 -143.8(4) . . . . ? C49 C35 C46 C11 139.5(4) . . . . ? C25 C35 C46 C11 -1.5(5) . . . . ? C59 C11 C46 C24 1.1(6) . . . . ? C31 C11 C46 C24 143.0(4) . . . . ? C59 C11 C46 C35 -140.6(4) . . . . ? C31 C11 C46 C35 1.3(5) . . . . ? C14 C27 C47 C20 -2.9(6) . . . . ? C43 C27 C47 C20 135.7(4) . . . . ? C14 C27 C47 C54 -140.3(4) . . . . ? C43 C27 C47 C54 -1.6(6) . . . . ? C36 C20 C47 C27 1.8(6) . . . . ? C34 C20 C47 C27 -140.6(4) . . . . ? C36 C20 C47 C54 143.3(4) . . . . ? C34 C20 C47 C54 0.9(5) . . . . ? C40 C39 C48 C56 2.5(6) . . . . ? C19 C39 C48 C56 143.9(4) . . . . ? C40 C39 C48 C18 -141.3(4) . . . . ? C19 C39 C48 C18 0.1(5) . . . . ? C34 C18 C48 C56 -1.0(6) . . . . ? C12 C18 C48 C56 -141.7(4) . . . . ? C34 C18 C48 C39 142.2(4) . . . . ? C12 C18 C48 C39 1.5(5) . . . . ? C46 C35 C49 C44 7.2(6) . . . . ? C25 C35 C49 C44 143.5(4) . . . . ? C46 C35 C49 C40 -137.6(4) . . . . ? C25 C35 C49 C40 -1.3(6) . . . . ? C21 C44 C49 C35 -3.9(6) . . . . ? C3 C44 C49 C35 -154.8(4) . . . . ? C21 C44 C49 C40 144.0(4) . . . . ? C3 C44 C49 C40 -7.0(4) . . . . ? C39 C40 C49 C35 -3.0(6) . . . . ? C57 C40 C49 C35 147.0(4) . . . . ? C39 C40 C49 C44 -151.8(4) . . . . ? C57 C40 C49 C44 -1.9(5) . . . . ? C21 C44 C3 O3 35.6(6) . . . . ? C49 C44 C3 O3 -175.8(4) . . . . ? C21 C44 C3 C57 -136.1(4) . . . . ? C49 C44 C3 C57 12.6(4) . . . . ? C55 C42 C51 C60 6.7(6) . . . . ? C56 C42 C51 C60 -137.9(4) . . . . ? C55 C42 C51 C1 162.4(4) . . . . ? C56 C42 C51 C1 17.8(4) . . . . ? O1 C1 C51 C60 -121.5(4) . . . . ? C6 C1 C51 C60 -1.4(5) . . . . ? C50 C1 C51 C60 126.5(4) . . . . ? O1 C1 C51 C42 84.2(4) . . . . ? C6 C1 C51 C42 -155.8(3) . . . . ? C50 C1 C51 C42 -27.9(4) . . . . ? C32 C43 C52 C41 142.3(4) . . . . ? C27 C43 C52 C41 4.2(6) . . . . ? C32 C43 C52 C33 -0.9(6) . . . . ? C27 C43 C52 C33 -139.0(4) . . . . ? C54 C41 C52 C43 -5.1(6) . . . . ? C60 C41 C52 C43 -150.2(4) . . . . ? C54 C41 C52 C33 142.3(4) . . . . ? C60 C41 C52 C33 -2.9(4) . . . . ? C58 C33 C52 C43 1.2(6) . . . . ? C2 C33 C52 C43 166.7(4) . . . . ? C58 C33 C52 C41 -145.2(4) . . . . ? C2 C33 C52 C41 20.3(4) . . . . ? C16 C26 C53 C37 2.6(6) . . . . ? C4 C26 C53 C37 -142.2(4) . . . . ? C16 C26 C53 C5 148.3(4) . . . . ? C4 C26 C53 C5 3.5(7) . . . . ? C28 C37 C53 C26 -7.9(6) . . . . ? C24 C37 C53 C26 138.2(4) . . . . ? C28 C37 C53 C5 -159.6(4) . . . . ? C24 C37 C53 C5 -13.5(5) . . . . ? O5 C5 C53 C26 51.9(7) . . . . ? C21 C5 C53 C26 -127.2(4) . . . . ? O5 C5 C53 C37 -159.3(4) . . . . ? C21 C5 C53 C37 21.6(4) . . . . ? C52 C41 C54 C55 -133.6(4) . . . . ? C60 C41 C54 C55 7.0(6) . . . . ? C52 C41 C54 C47 2.6(6) . . . . ? C60 C41 C54 C47 143.2(4) . . . . ? C27 C47 C54 C41 0.8(6) . . . . ? C20 C47 C54 C41 -140.7(4) . . . . ? C27 C47 C54 C55 141.2(4) . . . . ? C20 C47 C54 C55 -0.3(4) . . . . ? C51 C42 C55 C54 -6.5(6) . . . . ? C56 C42 C55 C54 133.7(4) . . . . ? C51 C42 C55 C34 -142.5(4) . . . . ? C56 C42 C55 C34 -2.4(6) . . . . ? C41 C54 C55 C42 -0.4(6) . . . . ? C47 C54 C55 C42 -141.3(4) . . . . ? C41 C54 C55 C34 140.5(4) . . . . ? C47 C54 C55 C34 -0.4(4) . . . . ? C18 C34 C55 C42 -1.9(6) . . . . ? C20 C34 C55 C42 141.0(4) . . . . ? C18 C34 C55 C54 -141.9(4) . . . . ? C20 C34 C55 C54 1.0(4) . . . . ? C39 C48 C56 C42 -142.6(4) . . . . ? C18 C48 C56 C42 -3.2(6) . . . . ? C39 C48 C56 C50 0.9(6) . . . . ? C18 C48 C56 C50 140.4(4) . . . . ? C55 C42 C56 C48 4.9(6) . . . . ? C51 C42 C56 C48 149.9(4) . . . . ? C55 C42 C56 C50 -143.1(4) . . . . ? C51 C42 C56 C50 1.9(4) . . . . ? C39 C40 C57 C50 2.9(6) . . . . ? C49 C40 C57 C50 -146.2(4) . . . . ? C39 C40 C57 C3 158.9(4) . . . . ? C49 C40 C57 C3 9.8(4) . . . . ? O3 C3 C57 C50 -31.9(7) . . . . ? C44 C3 C57 C50 139.7(4) . . . . ? O3 C3 C57 C40 174.9(4) . . . . ? C44 C3 C57 C40 -13.5(4) . . . . ? C52 C33 C58 C45 0.3(5) . . . . ? C2 C33 C58 C45 -159.4(4) . . . . ? C52 C33 C58 C4 151.7(4) . . . . ? C2 C33 C58 C4 -8.0(7) . . . . ? C32 C45 C58 C33 -2.4(6) . . . . ? C16 C45 C58 C33 146.0(4) . . . . ? C32 C45 C58 C4 -159.9(4) . . . . ? C16 C45 C58 C4 -11.6(4) . . . . ? O4 C4 C58 C33 35.1(7) . . . . ? C26 C4 C58 C33 -138.6(4) . . . . ? O4 C4 C58 C45 -170.4(4) . . . . ? C26 C4 C58 C45 15.8(4) . . . . ? C46 C11 C59 C15 136.9(4) . . . . ? C31 C11 C59 C15 -0.5(6) . . . . ? C46 C11 C59 C28 -0.5(6) . . . . ? C31 C11 C59 C28 -137.9(4) . . . . ? C13 C15 C59 C11 1.1(6) . . . . ? C38 C15 C59 C11 -141.7(4) . . . . ? C13 C15 C59 C28 142.5(4) . . . . ? C38 C15 C59 C28 -0.3(5) . . . . ? C37 C28 C59 C11 -0.3(6) . . . . ? C22 C28 C59 C11 141.3(4) . . . . ? C37 C28 C59 C15 -142.1(4) . . . . ? C22 C28 C59 C15 -0.5(5) . . . . ? C40 C57 C50 C56 0.6(5) . . . . ? C3 C57 C50 C56 -149.5(4) . . . . ? C40 C57 C50 C1 158.7(4) . . . . ? C3 C57 C50 C1 8.6(7) . . . . ? C48 C56 C50 C57 -2.4(6) . . . . ? C42 C56 C50 C57 144.2(4) . . . . ? C48 C56 C50 C1 -166.4(4) . . . . ? C42 C56 C50 C1 -19.7(4) . . . . ? O1 C1 C50 C57 117.3(5) . . . . ? C51 C1 C50 C57 -131.8(4) . . . . ? C6 C1 C50 C57 -11.0(6) . . . . ? O1 C1 C50 C56 -82.8(4) . . . . ? C51 C1 C50 C56 28.0(4) . . . . ? C6 C1 C50 C56 148.9(3) . . . . ? C42 C51 C60 C41 0.1(6) . . . . ? C1 C51 C60 C41 -151.8(4) . . . . ? C42 C51 C60 C2 151.2(4) . . . . ? C1 C51 C60 C2 -0.7(6) . . . . ? C54 C41 C60 C51 -6.9(6) . . . . ? C52 C41 C60 C51 138.2(4) . . . . ? C54 C41 C60 C2 -162.3(4) . . . . ? C52 C41 C60 C2 -17.2(4) . . . . ? O2 C2 C60 C51 121.5(4) . . . . ? C7 C2 C60 C51 2.1(5) . . . . ? C33 C2 C60 C51 -125.5(4) . . . . ? O2 C2 C60 C41 -85.1(4) . . . . ? C7 C2 C60 C41 155.5(3) . . . . ? C33 C2 C60 C41 27.9(4) . . . . ? C8 N1 C61 C66 49.1(6) . . . . ? C8 N1 C61 C62 -134.0(4) . . . . ? C66 C61 C62 C63 -2.0(7) . . . . ? N1 C61 C62 C63 -179.1(4) . . . . ? C61 C62 C63 C64 1.6(7) . . . . ? C62 C63 C64 C65 -0.3(7) . . . . ? C62 C63 C64 C67 -178.3(4) . . . . ? C63 C64 C65 C66 -0.6(7) . . . . ? C67 C64 C65 C66 177.3(4) . . . . ? C62 C61 C66 C65 1.1(7) . . . . ? N1 C61 C66 C65 178.0(4) . . . . ? C64 C65 C66 C61 0.3(7) . . . . ? C65 C64 C67 C69 148.5(5) . . . . ? C63 C64 C67 C69 -33.7(6) . . . . ? C65 C64 C67 C70 27.4(6) . . . . ? C63 C64 C67 C70 -154.7(5) . . . . ? C65 C64 C67 C68 -91.3(5) . . . . ? C63 C64 C67 C68 86.5(5) . . . . ? C10 N2 C71 C76 135.9(4) . . . . ? C10 N2 C71 C72 -52.3(6) . . . . ? C76 C71 C72 C73 -1.2(7) . . . . ? N2 C71 C72 C73 -173.0(4) . . . . ? C71 C72 C73 C74 -0.8(7) . . . . ? C72 C73 C74 C75 1.2(7) . . . . ? C72 C73 C74 C77 175.9(4) . . . . ? C73 C74 C75 C76 0.4(7) . . . . ? C77 C74 C75 C76 -174.2(4) . . . . ? C72 C71 C76 C75 2.7(6) . . . . ? N2 C71 C76 C75 174.7(4) . . . . ? C74 C75 C76 C71 -2.3(7) . . . . ? C75 C74 C77 C78 104.0(6) . . . . ? C73 C74 C77 C78 -70.4(6) . . . . ? C75 C74 C77 C80 -16.6(6) . . . . ? C73 C74 C77 C80 168.9(4) . . . . ? C75 C74 C77 C79 -136.2(5) . . . . ? C73 C74 C77 C79 49.4(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 N2 0.84 1.87 2.620(4) 148.0 . O2 H2 N1 0.84 1.99 2.679(4) 138.4 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.447 _refine_diff_density_min -0.650 _refine_diff_density_rms 0.085 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.369 0.236 0.695 26 0 ' ' 2 0.500 0.500 0.000 152 56 ' ' 3 0.631 0.764 0.305 26 0 ' '