# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_a _database_code_depnum_ccdc_archive 'CCDC 905498' #TrackingRef '14606_web_deposit_cif_file_0_Gan,Liangbing_1349923400.7a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C76 H26 I N O10), C7 H8' _chemical_formula_sum 'C159 H60 I2 N2 O20' _chemical_formula_weight 2571.89 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' I I -0.4742 1.8119 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5690(13) _cell_length_b 12.6230(15) _cell_length_c 20.413(3) _cell_angle_alpha 97.570(11) _cell_angle_beta 102.490(12) _cell_angle_gamma 113.570(8) _cell_volume 2587.1(5) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6712 _cell_measurement_theta_min 1.82 _cell_measurement_theta_max 25.35 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.651 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1294 _exptl_absorpt_coefficient_mu 0.696 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9149 _exptl_absorpt_correction_T_max 0.9660 _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 39780 _diffrn_reflns_av_R_equivalents 0.0853 _diffrn_reflns_av_sigmaI/netI 0.0705 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.36 _reflns_number_total 9444 _reflns_number_gt 8647 _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^)+(0.0101P)^2^+9.1924P] 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 9444 _refine_ls_number_parameters 829 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1003 _refine_ls_R_factor_gt 0.0900 _refine_ls_wR_factor_ref 0.1491 _refine_ls_wR_factor_gt 0.1444 _refine_ls_goodness_of_fit_ref 1.307 _refine_ls_restrained_S_all 1.307 _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 I1 I 0.66470(4) 0.85000(4) 0.33956(2) 0.03955(14) Uani 1 1 d . . . O1 O 0.5677(4) 0.6467(4) 0.1876(2) 0.0425(12) Uani 1 1 d . . . O2 O 0.2692(5) 0.5036(4) 0.0814(2) 0.0419(11) Uani 1 1 d . . . O3 O 0.3939(5) 0.4047(4) 0.1957(2) 0.0426(12) Uani 1 1 d . . . O4 O 0.5137(4) 0.6253(4) 0.4064(2) 0.0386(11) Uani 1 1 d . . . O5 O 0.5554(6) 0.4694(5) 0.3752(3) 0.0681(17) Uani 1 1 d . . . O6 O 0.4255(4) 0.9186(4) 0.3382(2) 0.0335(10) Uani 1 1 d . . . O7 O 0.3888(4) 0.9749(4) 0.3924(2) 0.0416(12) Uani 1 1 d . . . O8 O 0.1940(4) 0.8064(3) 0.1013(2) 0.0305(10) Uani 1 1 d . . . O9 O 0.2753(4) 0.9291(4) 0.1440(2) 0.0335(10) Uani 1 1 d . . . O10 O 0.4294(4) 0.6031(3) 0.2890(2) 0.0291(9) Uani 1 1 d . . . N1 N 0.4253(5) 0.7537(4) 0.0931(3) 0.0308(12) Uani 1 1 d . . . C1 C 0.4739(6) 0.7149(5) 0.2709(3) 0.0286(14) Uani 1 1 d . . . C2 C 0.4996(6) 0.6911(5) 0.2005(3) 0.0301(14) Uani 1 1 d . . . C3 C 0.4135(6) 0.7280(5) 0.1502(3) 0.0281(14) Uani 1 1 d . . . C4 C 0.3161(6) 0.7370(5) 0.1849(3) 0.0239(13) Uani 1 1 d . . . C5 C 0.3641(5) 0.7516(5) 0.2536(3) 0.0258(13) Uani 1 1 d . . . C6 C 0.1844(6) 0.7349(5) 0.1501(3) 0.0264(13) Uani 1 1 d . . . C7 C 0.1277(6) 0.7707(5) 0.2058(3) 0.0294(14) Uani 1 1 d . . . C8 C 0.1868(6) 0.8011(5) 0.2751(3) 0.0262(13) Uani 1 1 d . . . C9 C 0.3179(6) 0.8020(5) 0.3079(3) 0.0269(13) Uani 1 1 d . . . C10 C 0.2797(6) 1.0067(5) 0.0971(3) 0.0332(15) Uani 1 1 d . . . C11 C 0.3490(7) 1.1274(6) 0.1482(4) 0.051(2) Uani 1 1 d . . . H11A H 0.4384 1.1415 0.1730 0.076 Uiso 1 1 calc R . . H11B H 0.2994 1.1291 0.1813 0.076 Uiso 1 1 calc R . . H11C H 0.3540 1.1896 0.1233 0.076 Uiso 1 1 calc R . . C12 C 0.3615(7) 0.9959(6) 0.0509(3) 0.0440(18) Uani 1 1 d . . . H12A H 0.3149 0.9174 0.0182 0.066 Uiso 1 1 calc R . . H12B H 0.4466 1.0052 0.0791 0.066 Uiso 1 1 calc R . . H12C H 0.3762 1.0581 0.0252 0.066 Uiso 1 1 calc R . . C13 C 0.1415(6) 0.9831(6) 0.0576(4) 0.0428(17) Uani 1 1 d . . . H13A H 0.0986 0.9053 0.0244 0.064 Uiso 1 1 calc R . . H13B H 0.1462 1.0454 0.0328 0.064 Uiso 1 1 calc R . . H13C H 0.0904 0.9834 0.0901 0.064 Uiso 1 1 calc R . . C14 C 0.4648(7) 1.1032(6) 0.4033(4) 0.0461(18) Uani 1 1 d . . . C15 C 0.4210(9) 1.1497(8) 0.4613(5) 0.084(3) Uani 1 1 d . . . H15A H 0.4484 1.1235 0.5025 0.126 Uiso 1 1 calc R . . H15B H 0.3247 1.1186 0.4466 0.126 Uiso 1 1 calc R . . H15C H 0.4617 1.2370 0.4721 0.126 Uiso 1 1 calc R . . C16 C 0.6108(7) 1.1382(7) 0.4284(4) 0.063(2) Uani 1 1 d . . . H16A H 0.6388 1.1098 0.3905 0.094 Uiso 1 1 calc R . . H16B H 0.6285 1.1023 0.4668 0.094 Uiso 1 1 calc R . . H16C H 0.6598 1.2251 0.4442 0.094 Uiso 1 1 calc R . . C17 C 0.4292(9) 1.1405(7) 0.3386(5) 0.073(3) Uani 1 1 d . . . H17A H 0.4617 1.1095 0.3037 0.109 Uiso 1 1 calc R . . H17B H 0.4696 1.2277 0.3483 0.109 Uiso 1 1 calc R . . H17C H 0.3330 1.1088 0.3211 0.109 Uiso 1 1 calc R . . C18 C 0.3953(6) 0.5826(6) 0.3496(3) 0.0315(14) Uani 1 1 d . . . C19 C 0.5891(7) 0.5640(7) 0.4111(4) 0.0435(18) Uani 1 1 d . . . C20 C 0.7163(7) 0.6389(8) 0.4657(4) 0.060(2) Uani 1 1 d . . . H20A H 0.7712 0.5963 0.4698 0.089 Uiso 1 1 calc R . . H20B H 0.6994 0.6560 0.5099 0.089 Uiso 1 1 calc R . . H20C H 0.7624 0.7139 0.4533 0.089 Uiso 1 1 calc R . . C21 C 0.2901(7) 0.3628(6) 0.2075(3) 0.0378(16) Uani 1 1 d . . . C22 C 0.1605(7) 0.4571(5) 0.0872(3) 0.0321(15) Uani 1 1 d . . . C23 C 0.5371(6) 0.7555(5) 0.0736(3) 0.0311(14) Uani 1 1 d . . . C24 C 0.5190(6) 0.6697(6) 0.0178(3) 0.0351(15) Uani 1 1 d . . . H24A H 0.4331 0.6087 -0.0066 0.042 Uiso 1 1 calc R . . C25 C 0.6271(7) 0.6733(6) -0.0021(3) 0.0389(16) Uani 1 1 d . . . H25A H 0.6148 0.6150 -0.0409 0.047 Uiso 1 1 calc R . . C26 C 0.7520(7) 0.7601(6) 0.0334(4) 0.0413(17) Uani 1 1 d . . . H26A H 0.8257 0.7612 0.0196 0.050 Uiso 1 1 calc R . . C27 C 0.7701(7) 0.8458(7) 0.0892(4) 0.0472(18) Uani 1 1 d . . . H27A H 0.8565 0.9055 0.1141 0.057 Uiso 1 1 calc R . . C28 C 0.6620(7) 0.8448(6) 0.1089(4) 0.0439(17) Uani 1 1 d . . . H28A H 0.6740 0.9052 0.1464 0.053 Uiso 1 1 calc R . . C29 C 0.1076(6) 0.7757(5) 0.3222(3) 0.0327(15) Uani 1 1 d . . . C30 C 0.1682(6) 0.7341(6) 0.3757(3) 0.0327(15) Uani 1 1 d . . . C31 C 0.0910(6) 0.6557(6) 0.4069(3) 0.0369(16) Uani 1 1 d . . . C32 C 0.1227(7) 0.5619(6) 0.4237(3) 0.0383(16) Uani 1 1 d . . . C33 C 0.2289(6) 0.5538(6) 0.4071(3) 0.0342(15) Uani 1 1 d . . . C34 C 0.2211(6) 0.4377(6) 0.3802(3) 0.0374(16) Uani 1 1 d . . . C35 C 0.3033(6) 0.4485(6) 0.3357(3) 0.0345(15) Uani 1 1 d . . . C36 C 0.2611(7) 0.3594(6) 0.2774(3) 0.0377(16) Uani 1 1 d . . . C37 C 0.1528(7) 0.2971(5) 0.1559(3) 0.0373(16) Uani 1 1 d . . . C38 C 0.0970(6) 0.3359(5) 0.1032(3) 0.0338(15) Uani 1 1 d . . . C39 C 0.0558(6) 0.5021(6) 0.0821(3) 0.0322(15) Uani 1 1 d . . . C40 C 0.0637(6) 0.6125(5) 0.1086(3) 0.0280(14) Uani 1 1 d . . . C41 C -0.0517(6) 0.6186(6) 0.1201(3) 0.0311(14) Uani 1 1 d . . . C42 C -0.0139(6) 0.7128(5) 0.1808(3) 0.0311(14) Uani 1 1 d . . . C43 C -0.0924(6) 0.6986(6) 0.2253(3) 0.0371(16) Uani 1 1 d . . . C44 C -0.0280(6) 0.7325(6) 0.2987(3) 0.0364(16) Uani 1 1 d . . . C45 C -0.1097(7) 0.6446(6) 0.3291(4) 0.0413(17) Uani 1 1 d . . . C46 C -0.0513(7) 0.6088(7) 0.3833(3) 0.0429(18) Uani 1 1 d . . . C47 C -0.1073(7) 0.4841(7) 0.3851(3) 0.0435(18) Uani 1 1 d . . . C48 C 0.0007(7) 0.4549(7) 0.4109(3) 0.0440(18) Uani 1 1 d . . . C49 C -0.0076(7) 0.3443(7) 0.3851(4) 0.0447(18) Uani 1 1 d . . . C50 C 0.1053(7) 0.3362(6) 0.3701(3) 0.0397(16) Uani 1 1 d . . . C51 C 0.0593(7) 0.2426(6) 0.3083(4) 0.0416(17) Uani 1 1 d . . . C52 C 0.1347(7) 0.2575(6) 0.2628(3) 0.0401(17) Uani 1 1 d . . . C53 C 0.0677(7) 0.2204(6) 0.1890(4) 0.0410(17) Uani 1 1 d . . . C54 C -0.0683(8) 0.1749(6) 0.1652(4) 0.0457(18) Uani 1 1 d . . . C55 C -0.1262(7) 0.2142(6) 0.1098(3) 0.0427(18) Uani 1 1 d . . . C56 C -0.0425(7) 0.2988(5) 0.0835(3) 0.0376(16) Uani 1 1 d . . . C57 C -0.0681(6) 0.3972(6) 0.0689(3) 0.0349(15) Uani 1 1 d . . . C58 C -0.1795(6) 0.4028(6) 0.0775(3) 0.0379(16) Uani 1 1 d . . . C59 C -0.1714(6) 0.5177(6) 0.1046(3) 0.0353(16) Uani 1 1 d . . . C60 C -0.2540(6) 0.5021(6) 0.1506(4) 0.0412(17) Uani 1 1 d . . . C61 C -0.2133(6) 0.5904(6) 0.2104(4) 0.0413(17) Uani 1 1 d . . . C62 C -0.2259(6) 0.5569(7) 0.2746(4) 0.0408(17) Uani 1 1 d . . . C63 C -0.2794(6) 0.4382(7) 0.2762(4) 0.0464(19) Uani 1 1 d . . . C64 C -0.2199(7) 0.4006(7) 0.3329(4) 0.0477(19) Uani 1 1 d . . . C65 C -0.2271(7) 0.2842(7) 0.3055(4) 0.0481(19) Uani 1 1 d . . . C66 C -0.1239(7) 0.2581(6) 0.3315(4) 0.0479(19) Uani 1 1 d . . . C67 C -0.0834(7) 0.1934(6) 0.2844(4) 0.0451(18) Uani 1 1 d . . . C68 C 0.2836(6) 0.7287(5) 0.3616(3) 0.0277(14) Uani 1 1 d . . . C69 C -0.1456(7) 0.1604(6) 0.2138(4) 0.0493(19) Uani 1 1 d . . . C70 C -0.2521(7) 0.1898(6) 0.1870(4) 0.050(2) Uani 1 1 d . . . C71 C -0.2388(7) 0.2231(6) 0.1221(4) 0.0454(18) Uani 1 1 d . . . C72 C -0.2674(6) 0.3159(7) 0.1057(3) 0.0446(18) Uani 1 1 d . . . C73 C 0.3137(6) 0.6401(5) 0.3765(3) 0.0308(14) Uani 1 1 d . . . C74 C -0.3114(6) 0.3776(7) 0.1519(4) 0.0450(18) Uani 1 1 d . . . C75 C -0.2932(6) 0.2511(7) 0.2318(4) 0.052(2) Uani 1 1 d . . . C76 C -0.3232(6) 0.3467(7) 0.2142(4) 0.048(2) Uani 1 1 d . . . C77 C 0.946(2) -0.0258(17) 0.6197(11) 0.089(7) Uani 0.50 1 d P . . H77A H 0.8951 0.0170 0.6294 0.134 Uiso 0.50 1 calc PR . . H77B H 1.0293 0.0060 0.6571 0.134 Uiso 0.50 1 calc PR . . H77C H 0.8953 -0.1108 0.6163 0.134 Uiso 0.50 1 calc PR . . C78 C 0.9724(8) -0.0118(8) 0.5598(5) 0.065(3) Uani 1 1 d . . . H78A H 0.9541 -0.0191 0.6032 0.078 Uiso 0.50 1 d PR . . C79 C 0.9278(8) 0.0518(8) 0.5225(6) 0.068(3) Uani 1 1 d . . . H79A H 0.8767 0.0867 0.5384 0.081 Uiso 1 1 calc R . . C80 C 0.9554(9) 0.0658(8) 0.4632(5) 0.071(3) Uani 1 1 d . . . H80A H 0.9261 0.1121 0.4371 0.085 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 I1 0.0240(2) 0.0437(3) 0.0390(3) 0.0029(2) 0.00209(18) 0.00907(19) O1 0.043(3) 0.056(3) 0.043(3) 0.016(2) 0.020(2) 0.031(3) O2 0.043(3) 0.035(3) 0.049(3) 0.008(2) 0.020(2) 0.017(2) O3 0.051(3) 0.037(3) 0.038(3) 0.003(2) 0.013(2) 0.020(2) O4 0.033(2) 0.050(3) 0.026(2) 0.005(2) 0.003(2) 0.016(2) O5 0.065(4) 0.060(4) 0.080(4) 0.003(3) 0.003(3) 0.041(3) O6 0.033(2) 0.029(2) 0.032(2) -0.0028(19) 0.0110(19) 0.010(2) O7 0.040(3) 0.032(3) 0.036(3) -0.012(2) 0.019(2) 0.002(2) O8 0.036(2) 0.028(2) 0.024(2) 0.0042(18) 0.0038(19) 0.014(2) O9 0.038(3) 0.026(2) 0.026(2) 0.0006(18) 0.0039(19) 0.009(2) O10 0.032(2) 0.030(2) 0.023(2) 0.0046(18) 0.0069(18) 0.013(2) N1 0.032(3) 0.028(3) 0.028(3) 0.003(2) 0.009(2) 0.010(2) C1 0.026(3) 0.033(3) 0.022(3) 0.006(3) 0.005(3) 0.011(3) C2 0.027(3) 0.032(3) 0.028(3) 0.001(3) 0.009(3) 0.010(3) C3 0.024(3) 0.022(3) 0.032(4) 0.000(3) 0.004(3) 0.008(3) C4 0.029(3) 0.020(3) 0.025(3) 0.005(2) 0.010(3) 0.011(3) C5 0.022(3) 0.020(3) 0.032(3) 0.007(3) 0.009(3) 0.004(3) C6 0.027(3) 0.031(3) 0.024(3) 0.010(3) 0.008(3) 0.015(3) C7 0.026(3) 0.030(3) 0.036(4) 0.011(3) 0.013(3) 0.015(3) C8 0.028(3) 0.021(3) 0.029(3) 0.002(3) 0.007(3) 0.011(3) C9 0.027(3) 0.025(3) 0.022(3) 0.000(2) 0.004(3) 0.009(3) C10 0.034(4) 0.029(3) 0.037(4) 0.015(3) 0.010(3) 0.013(3) C11 0.054(5) 0.031(4) 0.063(5) 0.016(4) 0.014(4) 0.015(4) C12 0.037(4) 0.050(4) 0.038(4) 0.012(3) 0.011(3) 0.012(3) C13 0.042(4) 0.044(4) 0.050(4) 0.025(4) 0.012(3) 0.023(4) C14 0.049(4) 0.032(4) 0.044(4) -0.007(3) 0.018(4) 0.007(3) C15 0.081(7) 0.056(6) 0.089(7) -0.032(5) 0.042(6) 0.012(5) C16 0.051(5) 0.050(5) 0.053(5) -0.012(4) 0.012(4) 0.000(4) C17 0.082(7) 0.042(5) 0.091(7) 0.010(5) 0.020(6) 0.030(5) C18 0.034(4) 0.036(4) 0.021(3) 0.003(3) 0.004(3) 0.016(3) C19 0.043(4) 0.060(5) 0.038(4) 0.016(4) 0.012(3) 0.032(4) C20 0.045(5) 0.095(7) 0.043(5) 0.020(4) 0.003(4) 0.039(5) C21 0.051(5) 0.027(4) 0.034(4) 0.009(3) 0.009(3) 0.017(3) C22 0.046(4) 0.027(3) 0.017(3) -0.004(3) 0.009(3) 0.013(3) C23 0.035(4) 0.033(4) 0.031(3) 0.011(3) 0.013(3) 0.018(3) C24 0.030(3) 0.040(4) 0.033(4) 0.008(3) 0.009(3) 0.013(3) C25 0.049(4) 0.042(4) 0.032(4) 0.009(3) 0.018(3) 0.024(4) C26 0.041(4) 0.058(5) 0.051(5) 0.030(4) 0.033(4) 0.032(4) C27 0.029(4) 0.050(5) 0.058(5) 0.015(4) 0.016(3) 0.009(3) C28 0.042(4) 0.037(4) 0.053(5) 0.009(3) 0.018(4) 0.016(3) C29 0.032(3) 0.033(4) 0.030(3) -0.004(3) 0.011(3) 0.014(3) C30 0.033(4) 0.036(4) 0.022(3) -0.002(3) 0.006(3) 0.013(3) C31 0.033(4) 0.047(4) 0.022(3) -0.003(3) 0.010(3) 0.012(3) C32 0.041(4) 0.048(4) 0.019(3) 0.002(3) 0.009(3) 0.015(3) C33 0.035(4) 0.043(4) 0.016(3) 0.005(3) 0.000(3) 0.014(3) C34 0.036(4) 0.048(4) 0.022(3) 0.015(3) 0.006(3) 0.012(3) C35 0.035(4) 0.034(4) 0.030(3) 0.009(3) 0.000(3) 0.014(3) C36 0.047(4) 0.036(4) 0.037(4) 0.015(3) 0.011(3) 0.024(3) C37 0.050(4) 0.021(3) 0.038(4) 0.000(3) 0.016(3) 0.014(3) C38 0.044(4) 0.023(3) 0.023(3) -0.006(3) 0.006(3) 0.008(3) C39 0.032(4) 0.035(4) 0.021(3) 0.008(3) 0.007(3) 0.007(3) C40 0.028(3) 0.031(3) 0.023(3) 0.008(3) 0.006(3) 0.012(3) C41 0.032(3) 0.041(4) 0.023(3) 0.010(3) 0.005(3) 0.020(3) C42 0.033(3) 0.035(4) 0.033(4) 0.012(3) 0.008(3) 0.022(3) C43 0.029(3) 0.046(4) 0.041(4) 0.010(3) 0.013(3) 0.020(3) C44 0.038(4) 0.041(4) 0.037(4) 0.003(3) 0.012(3) 0.026(3) C45 0.036(4) 0.053(5) 0.038(4) 0.008(3) 0.021(3) 0.018(4) C46 0.041(4) 0.055(5) 0.030(4) 0.002(3) 0.018(3) 0.017(4) C47 0.037(4) 0.058(5) 0.035(4) 0.016(3) 0.022(3) 0.013(4) C48 0.041(4) 0.064(5) 0.022(3) 0.013(3) 0.017(3) 0.014(4) C49 0.051(5) 0.048(5) 0.032(4) 0.021(3) 0.017(3) 0.014(4) C50 0.050(4) 0.043(4) 0.031(4) 0.020(3) 0.013(3) 0.021(4) C51 0.050(4) 0.029(4) 0.041(4) 0.014(3) 0.011(3) 0.014(3) C52 0.051(4) 0.026(4) 0.036(4) 0.004(3) 0.007(3) 0.014(3) C53 0.046(4) 0.027(4) 0.041(4) 0.005(3) 0.008(3) 0.011(3) C54 0.060(5) 0.021(3) 0.039(4) 0.002(3) 0.011(4) 0.005(3) C55 0.046(4) 0.024(4) 0.033(4) -0.006(3) 0.003(3) -0.001(3) C56 0.041(4) 0.022(3) 0.030(4) -0.007(3) 0.002(3) 0.004(3) C57 0.036(4) 0.037(4) 0.020(3) 0.000(3) 0.005(3) 0.009(3) C58 0.033(4) 0.037(4) 0.023(3) 0.000(3) -0.008(3) 0.005(3) C59 0.027(3) 0.052(4) 0.019(3) 0.006(3) -0.003(3) 0.015(3) C60 0.020(3) 0.055(5) 0.039(4) 0.007(3) 0.000(3) 0.013(3) C61 0.028(4) 0.056(5) 0.042(4) 0.009(4) 0.006(3) 0.023(3) C62 0.022(3) 0.058(5) 0.040(4) 0.008(3) 0.014(3) 0.015(3) C63 0.026(4) 0.061(5) 0.043(4) 0.008(4) 0.011(3) 0.011(4) C64 0.033(4) 0.059(5) 0.039(4) 0.006(4) 0.020(3) 0.005(4) C65 0.037(4) 0.049(5) 0.040(4) 0.009(4) 0.016(3) -0.001(4) C66 0.039(4) 0.040(4) 0.050(5) 0.022(4) 0.015(4) 0.000(3) C67 0.051(5) 0.030(4) 0.045(4) 0.017(3) 0.018(4) 0.004(3) C68 0.022(3) 0.032(3) 0.017(3) -0.006(3) 0.001(2) 0.007(3) C69 0.046(4) 0.027(4) 0.053(5) 0.007(3) 0.009(4) -0.001(3) C70 0.040(4) 0.036(4) 0.048(5) 0.005(3) 0.007(4) -0.004(3) C71 0.041(4) 0.029(4) 0.035(4) -0.005(3) -0.001(3) -0.003(3) C72 0.026(4) 0.048(4) 0.031(4) -0.005(3) -0.005(3) -0.001(3) C73 0.027(3) 0.030(3) 0.023(3) -0.001(3) 0.000(3) 0.006(3) C74 0.017(3) 0.053(5) 0.042(4) 0.011(4) -0.001(3) -0.001(3) C75 0.021(4) 0.044(5) 0.060(5) 0.011(4) 0.005(3) -0.011(3) C76 0.018(3) 0.055(5) 0.049(5) 0.011(4) 0.011(3) -0.006(3) C77 0.091(16) 0.059(12) 0.106(18) 0.032(12) 0.005(13) 0.030(11) C78 0.043(5) 0.063(6) 0.055(6) -0.004(5) 0.014(4) -0.005(4) C79 0.050(5) 0.053(6) 0.090(8) -0.003(5) 0.012(5) 0.023(4) C80 0.053(6) 0.051(5) 0.077(7) -0.001(5) -0.002(5) 0.008(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 I1 C1 2.183(6) . ? O1 C2 1.187(7) . ? O2 C22 1.197(7) . ? O3 C21 1.198(8) . ? O4 C19 1.375(8) . ? O4 C18 1.438(7) . ? O5 C19 1.178(8) . ? O6 C9 1.435(7) . ? O6 O7 1.465(5) . ? O7 C14 1.458(8) . ? O8 C6 1.424(7) . ? O8 O9 1.473(5) . ? O9 C10 1.452(7) . ? O10 C18 1.403(7) . ? O10 C1 1.425(7) . ? N1 C3 1.271(7) . ? N1 C23 1.426(7) . ? C1 C5 1.507(8) . ? C1 C2 1.543(8) . ? C2 C3 1.523(8) . ? C3 C4 1.486(8) . ? C4 C5 1.352(8) . ? C4 C6 1.523(8) . ? C5 C9 1.504(8) . ? C6 C7 1.534(8) . ? C6 C40 1.573(8) . ? C7 C8 1.358(8) . ? C7 C42 1.435(8) . ? C8 C29 1.448(8) . ? C8 C9 1.514(8) . ? C9 C68 1.541(8) . ? C10 C12 1.502(9) . ? C10 C13 1.514(8) . ? C10 C11 1.514(9) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C17 1.491(11) . ? C14 C16 1.510(10) . ? C14 C15 1.521(10) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C35 1.543(9) . ? C18 C73 1.544(8) . ? C19 C20 1.484(10) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C37 1.521(9) . ? C21 C36 1.535(9) . ? C22 C39 1.520(9) . ? C22 C38 1.525(9) . ? C23 C24 1.380(8) . ? C23 C28 1.383(9) . ? C24 C25 1.382(9) . ? C24 H24A 0.9500 . ? C25 C26 1.374(9) . ? C25 H25A 0.9500 . ? C26 C27 1.378(10) . ? C26 H26A 0.9500 . ? C27 C28 1.390(9) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C44 1.382(8) . ? C29 C30 1.440(9) . ? C30 C31 1.373(9) . ? C30 C68 1.451(8) . ? C31 C32 1.434(9) . ? C31 C46 1.448(9) . ? C32 C33 1.381(9) . ? C32 C48 1.452(9) . ? C33 C34 1.455(9) . ? C33 C73 1.459(9) . ? C34 C50 1.385(9) . ? C34 C35 1.432(9) . ? C35 C36 1.370(9) . ? C36 C52 1.445(9) . ? C37 C38 1.381(9) . ? C37 C53 1.436(9) . ? C38 C56 1.432(9) . ? C39 C40 1.386(9) . ? C39 C57 1.450(8) . ? C40 C41 1.435(8) . ? C41 C59 1.391(9) . ? C41 C42 1.449(8) . ? C42 C43 1.397(8) . ? C43 C44 1.442(9) . ? C43 C61 1.447(9) . ? C44 C45 1.451(9) . ? C45 C46 1.391(10) . ? C45 C62 1.452(9) . ? C46 C47 1.452(10) . ? C47 C64 1.396(9) . ? C47 C48 1.452(10) . ? C48 C49 1.384(10) . ? C49 C66 1.439(10) . ? C49 C50 1.443(10) . ? C50 C51 1.443(9) . ? C51 C52 1.387(9) . ? C51 C67 1.449(10) . ? C52 C53 1.452(9) . ? C53 C54 1.384(10) . ? C54 C55 1.435(10) . ? C54 C69 1.454(10) . ? C55 C56 1.385(9) . ? C55 C71 1.422(10) . ? C56 C57 1.439(9) . ? C57 C58 1.366(9) . ? C58 C59 1.440(9) . ? C58 C72 1.448(9) . ? C59 C60 1.457(9) . ? C60 C61 1.388(9) . ? C60 C74 1.448(10) . ? C61 C62 1.447(9) . ? C62 C63 1.381(10) . ? C63 C76 1.438(10) . ? C63 C64 1.449(10) . ? C64 C65 1.464(11) . ? C65 C66 1.379(10) . ? C65 C75 1.451(10) . ? C66 C67 1.452(10) . ? C67 C69 1.386(10) . ? C68 C73 1.350(8) . ? C69 C70 1.444(11) . ? C70 C75 1.399(11) . ? C70 C71 1.462(10) . ? C71 C72 1.401(10) . ? C72 C74 1.444(10) . ? C74 C76 1.396(10) . ? C75 C76 1.449(11) . ? C77 C78 1.34(2) . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C77 H78A 0.3787 . ? C78 C79 1.347(13) . ? C78 C80 1.387(12) 2_756 ? C78 H78A 0.9600 . ? C79 C80 1.334(12) . ? C79 H79A 0.9500 . ? C80 C78 1.387(12) 2_756 ? C80 H80A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C19 O4 C18 120.0(5) . . ? C9 O6 O7 106.1(4) . . ? C14 O7 O6 106.4(4) . . ? C6 O8 O9 104.0(4) . . ? C10 O9 O8 106.2(4) . . ? C18 O10 C1 125.5(4) . . ? C3 N1 C23 117.5(5) . . ? O10 C1 C5 111.2(5) . . ? O10 C1 C2 105.6(5) . . ? C5 C1 C2 102.9(5) . . ? O10 C1 I1 114.1(4) . . ? C5 C1 I1 117.2(4) . . ? C2 C1 I1 104.3(4) . . ? O1 C2 C3 127.0(6) . . ? O1 C2 C1 126.5(6) . . ? C3 C2 C1 106.5(5) . . ? N1 C3 C4 126.3(6) . . ? N1 C3 C2 128.7(6) . . ? C4 C3 C2 104.8(5) . . ? C5 C4 C3 109.3(5) . . ? C5 C4 C6 124.3(5) . . ? C3 C4 C6 126.4(5) . . ? C4 C5 C9 124.7(5) . . ? C4 C5 C1 112.3(5) . . ? C9 C5 C1 123.0(5) . . ? O8 C6 C4 112.6(5) . . ? O8 C6 C7 112.2(5) . . ? C4 C6 C7 109.3(5) . . ? O8 C6 C40 103.3(4) . . ? C4 C6 C40 119.3(5) . . ? C7 C6 C40 99.4(4) . . ? C8 C7 C42 118.7(6) . . ? C8 C7 C6 125.1(5) . . ? C42 C7 C6 109.6(5) . . ? C7 C8 C29 120.1(5) . . ? C7 C8 C9 124.2(5) . . ? C29 C8 C9 108.8(5) . . ? O6 C9 C5 102.3(4) . . ? O6 C9 C8 114.7(5) . . ? C5 C9 C8 110.3(5) . . ? O6 C9 C68 113.0(4) . . ? C5 C9 C68 115.7(5) . . ? C8 C9 C68 101.4(5) . . ? O9 C10 C12 110.4(5) . . ? O9 C10 C13 110.6(5) . . ? C12 C10 C13 113.3(6) . . ? O9 C10 C11 100.5(5) . . ? C12 C10 C11 110.8(6) . . ? C13 C10 C11 110.5(6) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O7 C14 C17 110.1(6) . . ? O7 C14 C16 110.3(6) . . ? C17 C14 C16 111.8(7) . . ? O7 C14 C15 101.0(6) . . ? C17 C14 C15 113.3(7) . . ? C16 C14 C15 109.9(6) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O10 C18 O4 109.2(5) . . ? O10 C18 C35 107.6(5) . . ? O4 C18 C35 114.3(5) . . ? O10 C18 C73 119.9(5) . . ? O4 C18 C73 104.0(5) . . ? C35 C18 C73 101.9(5) . . ? O5 C19 O4 123.6(7) . . ? O5 C19 C20 127.9(7) . . ? O4 C19 C20 108.5(7) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O3 C21 C37 127.9(6) . . ? O3 C21 C36 129.4(6) . . ? C37 C21 C36 102.6(6) . . ? O2 C22 C39 129.8(6) . . ? O2 C22 C38 126.1(6) . . ? C39 C22 C38 104.1(5) . . ? C24 C23 C28 120.3(6) . . ? C24 C23 N1 119.5(6) . . ? C28 C23 N1 120.2(6) . . ? C23 C24 C25 119.4(6) . . ? C23 C24 H24A 120.3 . . ? C25 C24 H24A 120.3 . . ? C26 C25 C24 120.8(6) . . ? C26 C25 H25A 119.6 . . ? C24 C25 H25A 119.6 . . ? C25 C26 C27 119.8(6) . . ? C25 C26 H26A 120.1 . . ? C27 C26 H26A 120.1 . . ? C26 C27 C28 120.0(7) . . ? C26 C27 H27A 120.0 . . ? C28 C27 H27A 120.0 . . ? C23 C28 C27 119.6(7) . . ? C23 C28 H28A 120.2 . . ? C27 C28 H28A 120.2 . . ? C44 C29 C30 121.0(6) . . ? C44 C29 C8 121.0(6) . . ? C30 C29 C8 108.3(5) . . ? C31 C30 C29 119.6(6) . . ? C31 C30 C68 122.7(6) . . ? C29 C30 C68 108.8(5) . . ? C30 C31 C32 118.7(6) . . ? C30 C31 C46 120.5(6) . . ? C32 C31 C46 108.2(6) . . ? C33 C32 C31 118.3(6) . . ? C33 C32 C48 119.9(6) . . ? C31 C32 C48 108.7(6) . . ? C32 C33 C34 120.1(6) . . ? C32 C33 C73 122.7(6) . . ? C34 C33 C73 108.3(5) . . ? C50 C34 C35 122.7(6) . . ? C50 C34 C33 119.3(6) . . ? C35 C34 C33 109.8(6) . . ? C36 C35 C34 119.1(6) . . ? C36 C35 C18 129.4(6) . . ? C34 C35 C18 106.6(5) . . ? C35 C36 C52 118.7(6) . . ? C35 C36 C21 130.8(6) . . ? C52 C36 C21 105.5(6) . . ? C38 C37 C53 118.2(6) . . ? C38 C37 C21 127.7(6) . . ? C53 C37 C21 107.6(6) . . ? C37 C38 C56 119.4(6) . . ? C37 C38 C22 126.1(6) . . ? C56 C38 C22 106.9(6) . . ? C40 C39 C57 118.5(6) . . ? C40 C39 C22 131.7(6) . . ? C57 C39 C22 105.7(5) . . ? C39 C40 C41 118.8(6) . . ? C39 C40 C6 132.0(5) . . ? C41 C40 C6 106.6(5) . . ? C59 C41 C40 122.1(6) . . ? C59 C41 C42 118.9(6) . . ? C40 C41 C42 109.9(5) . . ? C43 C42 C7 122.2(6) . . ? C43 C42 C41 120.3(6) . . ? C7 C42 C41 107.5(5) . . ? C42 C43 C44 118.1(6) . . ? C42 C43 C61 120.1(6) . . ? C44 C43 C61 108.0(6) . . ? C29 C44 C43 119.1(6) . . ? C29 C44 C45 119.1(6) . . ? C43 C44 C45 107.6(6) . . ? C46 C45 C44 120.1(6) . . ? C46 C45 C62 119.7(7) . . ? C44 C45 C62 108.7(6) . . ? C45 C46 C31 119.5(6) . . ? C45 C46 C47 119.8(6) . . ? C31 C46 C47 107.7(6) . . ? C64 C47 C46 120.1(7) . . ? C64 C47 C48 119.7(7) . . ? C46 C47 C48 108.1(6) . . ? C49 C48 C32 120.2(7) . . ? C49 C48 C47 120.7(7) . . ? C32 C48 C47 107.3(7) . . ? C48 C49 C66 119.4(7) . . ? C48 C49 C50 119.5(7) . . ? C66 C49 C50 107.9(7) . . ? C34 C50 C49 120.9(7) . . ? C34 C50 C51 118.3(6) . . ? C49 C50 C51 108.6(6) . . ? C52 C51 C50 118.5(6) . . ? C52 C51 C67 122.0(6) . . ? C50 C51 C67 107.6(6) . . ? C51 C52 C36 122.3(6) . . ? C51 C52 C53 118.6(7) . . ? C36 C52 C53 109.8(6) . . ? C54 C53 C37 122.2(7) . . ? C54 C53 C52 120.2(7) . . ? C37 C53 C52 108.0(6) . . ? C53 C54 C55 119.2(6) . . ? C53 C54 C69 120.3(7) . . ? C55 C54 C69 108.2(7) . . ? C56 C55 C71 120.4(7) . . ? C56 C55 C54 118.1(7) . . ? C71 C55 C54 108.6(6) . . ? C55 C56 C38 122.1(7) . . ? C55 C56 C57 120.2(7) . . ? C38 C56 C57 109.3(5) . . ? C58 C57 C56 119.5(6) . . ? C58 C57 C39 123.0(6) . . ? C56 C57 C39 109.6(6) . . ? C57 C58 C59 118.4(6) . . ? C57 C58 C72 120.9(7) . . ? C59 C58 C72 108.3(6) . . ? C41 C59 C58 119.2(6) . . ? C41 C59 C60 121.1(6) . . ? C58 C59 C60 107.7(6) . . ? C61 C60 C74 120.5(7) . . ? C61 C60 C59 119.3(6) . . ? C74 C60 C59 107.9(6) . . ? C60 C61 C62 119.3(7) . . ? C60 C61 C43 120.1(6) . . ? C62 C61 C43 108.8(6) . . ? C63 C62 C61 120.5(7) . . ? C63 C62 C45 120.6(7) . . ? C61 C62 C45 106.9(6) . . ? C62 C63 C76 120.3(7) . . ? C62 C63 C64 119.9(7) . . ? C76 C63 C64 107.6(7) . . ? C47 C64 C63 119.9(7) . . ? C47 C64 C65 119.1(7) . . ? C63 C64 C65 108.6(6) . . ? C66 C65 C75 121.2(7) . . ? C66 C65 C64 120.0(7) . . ? C75 C65 C64 106.8(7) . . ? C65 C66 C49 121.0(7) . . ? C65 C66 C67 119.3(7) . . ? C49 C66 C67 108.1(7) . . ? C69 C67 C51 118.6(7) . . ? C69 C67 C66 120.5(7) . . ? C51 C67 C66 107.8(6) . . ? C73 C68 C30 119.1(6) . . ? C73 C68 C9 129.6(5) . . ? C30 C68 C9 107.3(5) . . ? C67 C69 C70 119.7(7) . . ? C67 C69 C54 120.2(7) . . ? C70 C69 C54 107.5(7) . . ? C75 C70 C69 120.4(7) . . ? C75 C70 C71 119.6(7) . . ? C69 C70 C71 107.5(7) . . ? C72 C71 C55 120.0(7) . . ? C72 C71 C70 119.5(7) . . ? C55 C71 C70 108.2(7) . . ? C71 C72 C74 120.5(7) . . ? C71 C72 C58 118.9(7) . . ? C74 C72 C58 108.1(6) . . ? C68 C73 C33 118.3(6) . . ? C68 C73 C18 133.1(6) . . ? C33 C73 C18 105.8(5) . . ? C76 C74 C72 120.2(7) . . ? C76 C74 C60 119.5(7) . . ? C72 C74 C60 107.9(6) . . ? C70 C75 C76 120.5(7) . . ? C70 C75 C65 118.8(7) . . ? C76 C75 C65 108.3(7) . . ? C74 C76 C63 119.9(7) . . ? C74 C76 C75 119.7(7) . . ? C63 C76 C75 108.7(7) . . ? C78 C77 H77A 109.5 . . ? C78 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C78 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C78 C77 H78A 5.0 . . ? H77A C77 H78A 105.5 . . ? H77B C77 H78A 108.6 . . ? H77C C77 H78A 114.1 . . ? C77 C78 C79 120.6(14) . . ? C77 C78 C80 118.4(14) . 2_756 ? C79 C78 C80 121.0(9) . 2_756 ? C77 C78 H78A 2.0 . . ? C79 C78 H78A 119.1 . . ? C80 C78 H78A 119.9 2_756 . ? C80 C79 C78 119.9(9) . . ? C80 C79 H79A 120.0 . . ? C78 C79 H79A 120.0 . . ? C79 C80 C78 119.0(10) . 2_756 ? C79 C80 H80A 120.5 . . ? C78 C80 H80A 120.5 2_756 . ? 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 C9 O6 O7 C14 -157.0(5) . . . . ? C6 O8 O9 C10 -175.7(4) . . . . ? C18 O10 C1 C5 -69.8(7) . . . . ? C18 O10 C1 C2 179.4(5) . . . . ? C18 O10 C1 I1 65.4(6) . . . . ? O10 C1 C2 O1 -53.9(8) . . . . ? C5 C1 C2 O1 -170.5(6) . . . . ? I1 C1 C2 O1 66.7(7) . . . . ? O10 C1 C2 C3 122.4(5) . . . . ? C5 C1 C2 C3 5.7(6) . . . . ? I1 C1 C2 C3 -117.1(4) . . . . ? C23 N1 C3 C4 171.1(5) . . . . ? C23 N1 C3 C2 -3.8(9) . . . . ? O1 C2 C3 N1 -23.9(11) . . . . ? C1 C2 C3 N1 159.9(6) . . . . ? O1 C2 C3 C4 160.4(6) . . . . ? C1 C2 C3 C4 -15.8(6) . . . . ? N1 C3 C4 C5 -154.6(6) . . . . ? C2 C3 C4 C5 21.3(6) . . . . ? N1 C3 C4 C6 23.4(9) . . . . ? C2 C3 C4 C6 -160.7(5) . . . . ? C3 C4 C5 C9 159.6(5) . . . . ? C6 C4 C5 C9 -18.5(9) . . . . ? C3 C4 C5 C1 -18.6(7) . . . . ? C6 C4 C5 C1 163.4(5) . . . . ? O10 C1 C5 C4 -104.8(5) . . . . ? C2 C1 C5 C4 7.7(6) . . . . ? I1 C1 C5 C4 121.5(5) . . . . ? O10 C1 C5 C9 77.0(7) . . . . ? C2 C1 C5 C9 -170.5(5) . . . . ? I1 C1 C5 C9 -56.7(6) . . . . ? O9 O8 C6 C4 -67.6(5) . . . . ? O9 O8 C6 C7 56.3(5) . . . . ? O9 O8 C6 C40 162.4(4) . . . . ? C5 C4 C6 O8 134.1(6) . . . . ? C3 C4 C6 O8 -43.6(8) . . . . ? C5 C4 C6 C7 8.7(8) . . . . ? C3 C4 C6 C7 -169.0(5) . . . . ? C5 C4 C6 C40 -104.7(7) . . . . ? C3 C4 C6 C40 77.6(7) . . . . ? O8 C6 C7 C8 -124.8(6) . . . . ? C4 C6 C7 C8 0.9(8) . . . . ? C40 C6 C7 C8 126.6(6) . . . . ? O8 C6 C7 C42 84.4(6) . . . . ? C4 C6 C7 C42 -149.9(5) . . . . ? C40 C6 C7 C42 -24.2(6) . . . . ? C42 C7 C8 C29 -0.4(9) . . . . ? C6 C7 C8 C29 -148.8(6) . . . . ? C42 C7 C8 C9 147.3(6) . . . . ? C6 C7 C8 C9 -1.1(9) . . . . ? O7 O6 C9 C5 -179.9(4) . . . . ? O7 O6 C9 C8 60.8(6) . . . . ? O7 O6 C9 C68 -54.8(6) . . . . ? C4 C5 C9 O6 -106.3(6) . . . . ? C1 C5 C9 O6 71.7(6) . . . . ? C4 C5 C9 C8 16.1(8) . . . . ? C1 C5 C9 C8 -165.9(5) . . . . ? C4 C5 C9 C68 130.5(6) . . . . ? C1 C5 C9 C68 -51.6(7) . . . . ? C7 C8 C9 O6 108.4(6) . . . . ? C29 C8 C9 O6 -100.9(6) . . . . ? C7 C8 C9 C5 -6.4(8) . . . . ? C29 C8 C9 C5 144.3(5) . . . . ? C7 C8 C9 C68 -129.5(6) . . . . ? C29 C8 C9 C68 21.3(6) . . . . ? O8 O9 C10 C12 -70.2(6) . . . . ? O8 O9 C10 C13 56.0(6) . . . . ? O8 O9 C10 C11 172.8(5) . . . . ? O6 O7 C14 C17 61.6(7) . . . . ? O6 O7 C14 C16 -62.2(7) . . . . ? O6 O7 C14 C15 -178.4(6) . . . . ? C1 O10 C18 O4 -77.6(6) . . . . ? C1 O10 C18 C35 157.7(5) . . . . ? C1 O10 C18 C73 42.1(8) . . . . ? C19 O4 C18 O10 -72.7(7) . . . . ? C19 O4 C18 C35 48.0(7) . . . . ? C19 O4 C18 C73 158.2(5) . . . . ? C18 O4 C19 O5 -8.9(10) . . . . ? C18 O4 C19 C20 169.2(6) . . . . ? C3 N1 C23 C24 111.6(7) . . . . ? C3 N1 C23 C28 -70.6(8) . . . . ? C28 C23 C24 C25 0.5(10) . . . . ? N1 C23 C24 C25 178.3(6) . . . . ? C23 C24 C25 C26 0.8(10) . . . . ? C24 C25 C26 C27 -0.8(10) . . . . ? C25 C26 C27 C28 -0.6(11) . . . . ? C24 C23 C28 C27 -1.9(10) . . . . ? N1 C23 C28 C27 -179.7(6) . . . . ? C26 C27 C28 C23 2.0(11) . . . . ? C7 C8 C29 C44 -7.1(9) . . . . ? C9 C8 C29 C44 -159.2(6) . . . . ? C7 C8 C29 C30 139.3(6) . . . . ? C9 C8 C29 C30 -12.9(7) . . . . ? C44 C29 C30 C31 -3.9(9) . . . . ? C8 C29 C30 C31 -150.3(6) . . . . ? C44 C29 C30 C68 144.3(6) . . . . ? C8 C29 C30 C68 -2.0(7) . . . . ? C29 C30 C31 C32 141.3(6) . . . . ? C68 C30 C31 C32 -2.4(9) . . . . ? C29 C30 C31 C46 4.0(9) . . . . ? C68 C30 C31 C46 -139.7(6) . . . . ? C30 C31 C32 C33 -0.7(9) . . . . ? C46 C31 C32 C33 141.4(6) . . . . ? C30 C31 C32 C48 -142.0(6) . . . . ? C46 C31 C32 C48 0.0(7) . . . . ? C31 C32 C33 C34 -140.2(6) . . . . ? C48 C32 C33 C34 -3.2(9) . . . . ? C31 C32 C33 C73 3.2(9) . . . . ? C48 C32 C33 C73 140.1(6) . . . . ? C32 C33 C34 C50 1.4(9) . . . . ? C73 C33 C34 C50 -146.7(6) . . . . ? C32 C33 C34 C35 150.7(6) . . . . ? C73 C33 C34 C35 2.6(7) . . . . ? C50 C34 C35 C36 5.6(10) . . . . ? C33 C34 C35 C36 -142.4(6) . . . . ? C50 C34 C35 C18 163.0(6) . . . . ? C33 C34 C35 C18 15.0(7) . . . . ? O10 C18 C35 C36 1.9(9) . . . . ? O4 C18 C35 C36 -119.7(7) . . . . ? C73 C18 C35 C36 128.8(7) . . . . ? O10 C18 C35 C34 -152.4(5) . . . . ? O4 C18 C35 C34 86.1(6) . . . . ? C73 C18 C35 C34 -25.4(6) . . . . ? C34 C35 C36 C52 0.1(9) . . . . ? C18 C35 C36 C52 -151.5(6) . . . . ? C34 C35 C36 C21 151.4(7) . . . . ? C18 C35 C36 C21 -0.2(12) . . . . ? O3 C21 C36 C35 51.3(11) . . . . ? C37 C21 C36 C35 -129.7(7) . . . . ? O3 C21 C36 C52 -154.6(7) . . . . ? C37 C21 C36 C52 24.3(6) . . . . ? O3 C21 C37 C38 -54.4(11) . . . . ? C36 C21 C37 C38 126.6(7) . . . . ? O3 C21 C37 C53 155.0(7) . . . . ? C36 C21 C37 C53 -24.0(7) . . . . ? C53 C37 C38 C56 -0.1(9) . . . . ? C21 C37 C38 C56 -148.0(6) . . . . ? C53 C37 C38 C22 145.5(6) . . . . ? C21 C37 C38 C22 -2.5(11) . . . . ? O2 C22 C38 C37 49.4(10) . . . . ? C39 C22 C38 C37 -129.5(7) . . . . ? O2 C22 C38 C56 -161.6(6) . . . . ? C39 C22 C38 C56 19.4(6) . . . . ? O2 C22 C39 C40 -43.7(11) . . . . ? C38 C22 C39 C40 135.3(7) . . . . ? O2 C22 C39 C57 160.4(6) . . . . ? C38 C22 C39 C57 -20.7(6) . . . . ? C57 C39 C40 C41 -1.5(9) . . . . ? C22 C39 C40 C41 -155.0(6) . . . . ? C57 C39 C40 C6 157.5(6) . . . . ? C22 C39 C40 C6 4.0(11) . . . . ? O8 C6 C40 C39 108.7(7) . . . . ? C4 C6 C40 C39 -17.1(9) . . . . ? C7 C6 C40 C39 -135.6(7) . . . . ? O8 C6 C40 C41 -90.4(5) . . . . ? C4 C6 C40 C41 143.8(5) . . . . ? C7 C6 C40 C41 25.3(6) . . . . ? C39 C40 C41 C59 -1.0(9) . . . . ? C6 C40 C41 C59 -165.0(5) . . . . ? C39 C40 C41 C42 145.3(6) . . . . ? C6 C40 C41 C42 -18.6(7) . . . . ? C8 C7 C42 C43 7.3(9) . . . . ? C6 C7 C42 C43 160.2(6) . . . . ? C8 C7 C42 C41 -138.3(6) . . . . ? C6 C7 C42 C41 14.7(7) . . . . ? C59 C41 C42 C43 4.2(9) . . . . ? C40 C41 C42 C43 -143.4(6) . . . . ? C59 C41 C42 C7 150.5(6) . . . . ? C40 C41 C42 C7 2.9(7) . . . . ? C7 C42 C43 C44 -6.6(9) . . . . ? C41 C42 C43 C44 134.7(6) . . . . ? C7 C42 C43 C61 -142.3(6) . . . . ? C41 C42 C43 C61 -1.0(9) . . . . ? C30 C29 C44 C43 -134.5(7) . . . . ? C8 C29 C44 C43 7.7(9) . . . . ? C30 C29 C44 C45 0.5(9) . . . . ? C8 C29 C44 C45 142.6(6) . . . . ? C42 C43 C44 C29 -1.0(10) . . . . ? C61 C43 C44 C29 139.6(6) . . . . ? C42 C43 C44 C45 -140.5(6) . . . . ? C61 C43 C44 C45 0.1(7) . . . . ? C29 C44 C45 C46 2.9(10) . . . . ? C43 C44 C45 C46 142.5(6) . . . . ? C29 C44 C45 C62 -140.3(6) . . . . ? C43 C44 C45 C62 -0.8(7) . . . . ? C44 C45 C46 C31 -2.9(10) . . . . ? C62 C45 C46 C31 136.4(6) . . . . ? C44 C45 C46 C47 -139.6(7) . . . . ? C62 C45 C46 C47 -0.3(9) . . . . ? C30 C31 C46 C45 -0.6(10) . . . . ? C32 C31 C46 C45 -141.9(6) . . . . ? C30 C31 C46 C47 140.7(6) . . . . ? C32 C31 C46 C47 -0.5(7) . . . . ? C45 C46 C47 C64 -0.3(10) . . . . ? C31 C46 C47 C64 -141.5(6) . . . . ? C45 C46 C47 C48 142.0(6) . . . . ? C31 C46 C47 C48 0.9(7) . . . . ? C33 C32 C48 C49 3.0(10) . . . . ? C31 C32 C48 C49 143.7(6) . . . . ? C33 C32 C48 C47 -140.1(6) . . . . ? C31 C32 C48 C47 0.5(7) . . . . ? C64 C47 C48 C49 -1.2(10) . . . . ? C46 C47 C48 C49 -143.7(6) . . . . ? C64 C47 C48 C32 141.7(6) . . . . ? C46 C47 C48 C32 -0.8(7) . . . . ? C32 C48 C49 C66 -137.3(7) . . . . ? C47 C48 C49 C66 0.9(10) . . . . ? C32 C48 C49 C50 -0.9(10) . . . . ? C47 C48 C49 C50 137.3(7) . . . . ? C35 C34 C50 C49 -144.4(7) . . . . ? C33 C34 C50 C49 0.7(9) . . . . ? C35 C34 C50 C51 -6.4(10) . . . . ? C33 C34 C50 C51 138.8(6) . . . . ? C48 C49 C50 C34 -0.9(10) . . . . ? C66 C49 C50 C34 139.9(6) . . . . ? C48 C49 C50 C51 -142.6(6) . . . . ? C66 C49 C50 C51 -1.7(8) . . . . ? C34 C50 C51 C52 1.5(10) . . . . ? C49 C50 C51 C52 144.3(6) . . . . ? C34 C50 C51 C67 -142.0(6) . . . . ? C49 C50 C51 C67 0.8(7) . . . . ? C50 C51 C52 C36 4.1(10) . . . . ? C67 C51 C52 C36 142.1(7) . . . . ? C50 C51 C52 C53 -139.1(7) . . . . ? C67 C51 C52 C53 -1.1(10) . . . . ? C35 C36 C52 C51 -4.9(10) . . . . ? C21 C36 C52 C51 -162.7(6) . . . . ? C35 C36 C52 C53 141.2(6) . . . . ? C21 C36 C52 C53 -16.7(7) . . . . ? C38 C37 C53 C54 6.9(10) . . . . ? C21 C37 C53 C54 160.8(6) . . . . ? C38 C37 C53 C52 -139.1(6) . . . . ? C21 C37 C53 C52 14.8(7) . . . . ? C51 C52 C53 C54 2.1(10) . . . . ? C36 C52 C53 C54 -145.4(6) . . . . ? C51 C52 C53 C37 148.9(6) . . . . ? C36 C52 C53 C37 1.4(8) . . . . ? C37 C53 C54 C55 -6.1(10) . . . . ? C52 C53 C54 C55 136.0(7) . . . . ? C37 C53 C54 C69 -144.0(7) . . . . ? C52 C53 C54 C69 -1.9(10) . . . . ? C53 C54 C55 C56 -1.5(10) . . . . ? C69 C54 C55 C56 140.9(6) . . . . ? C53 C54 C55 C71 -143.2(7) . . . . ? C69 C54 C55 C71 -0.7(7) . . . . ? C71 C55 C56 C38 145.4(6) . . . . ? C54 C55 C56 C38 8.4(10) . . . . ? C71 C55 C56 C57 0.6(9) . . . . ? C54 C55 C56 C57 -136.4(7) . . . . ? C37 C38 C56 C55 -7.6(9) . . . . ? C22 C38 C56 C55 -159.1(6) . . . . ? C37 C38 C56 C57 140.5(6) . . . . ? C22 C38 C56 C57 -11.0(7) . . . . ? C55 C56 C57 C58 -3.8(9) . . . . ? C38 C56 C57 C58 -152.6(6) . . . . ? C55 C56 C57 C39 146.3(6) . . . . ? C38 C56 C57 C39 -2.5(7) . . . . ? C40 C39 C57 C58 4.0(9) . . . . ? C22 C39 C57 C58 163.7(6) . . . . ? C40 C39 C57 C56 -144.8(6) . . . . ? C22 C39 C57 C56 14.9(7) . . . . ? C56 C57 C58 C59 142.3(6) . . . . ? C39 C57 C58 C59 -3.6(9) . . . . ? C56 C57 C58 C72 4.5(9) . . . . ? C39 C57 C58 C72 -141.5(6) . . . . ? C40 C41 C59 C58 1.4(9) . . . . ? C42 C41 C59 C58 -142.1(6) . . . . ? C40 C41 C59 C60 139.4(6) . . . . ? C42 C41 C59 C60 -4.1(9) . . . . ? C57 C58 C59 C41 0.9(9) . . . . ? C72 C58 C59 C41 143.6(6) . . . . ? C57 C58 C59 C60 -142.1(6) . . . . ? C72 C58 C59 C60 0.6(7) . . . . ? C41 C59 C60 C61 0.9(10) . . . . ? C58 C59 C60 C61 143.1(6) . . . . ? C41 C59 C60 C74 -141.6(6) . . . . ? C58 C59 C60 C74 0.5(7) . . . . ? C74 C60 C61 C62 1.5(9) . . . . ? C59 C60 C61 C62 -136.4(7) . . . . ? C74 C60 C61 C43 140.1(7) . . . . ? C59 C60 C61 C43 2.3(10) . . . . ? C42 C43 C61 C60 -2.3(10) . . . . ? C44 C43 C61 C60 -141.9(6) . . . . ? C42 C43 C61 C62 140.3(6) . . . . ? C44 C43 C61 C62 0.6(7) . . . . ? C60 C61 C62 C63 -0.9(9) . . . . ? C43 C61 C62 C63 -143.8(6) . . . . ? C60 C61 C62 C45 141.8(6) . . . . ? C43 C61 C62 C45 -1.1(8) . . . . ? C46 C45 C62 C63 0.4(10) . . . . ? C44 C45 C62 C63 143.8(6) . . . . ? C46 C45 C62 C61 -142.3(6) . . . . ? C44 C45 C62 C61 1.1(8) . . . . ? C61 C62 C63 C76 0.1(10) . . . . ? C45 C62 C63 C76 -137.6(7) . . . . ? C61 C62 C63 C64 137.9(7) . . . . ? C45 C62 C63 C64 0.2(10) . . . . ? C46 C47 C64 C63 1.0(10) . . . . ? C48 C47 C64 C63 -137.1(7) . . . . ? C46 C47 C64 C65 138.7(7) . . . . ? C48 C47 C64 C65 0.6(10) . . . . ? C62 C63 C64 C47 -0.9(10) . . . . ? C76 C63 C64 C47 141.6(7) . . . . ? C62 C63 C64 C65 -142.6(7) . . . . ? C76 C63 C64 C65 -0.1(7) . . . . ? C47 C64 C65 C66 0.3(10) . . . . ? C63 C64 C65 C66 142.3(7) . . . . ? C47 C64 C65 C75 -142.7(6) . . . . ? C63 C64 C65 C75 -0.7(8) . . . . ? C75 C65 C66 C49 137.1(7) . . . . ? C64 C65 C66 C49 -0.6(10) . . . . ? C75 C65 C66 C67 -1.7(10) . . . . ? C64 C65 C66 C67 -139.4(7) . . . . ? C48 C49 C66 C65 0.0(10) . . . . ? C50 C49 C66 C65 -140.9(7) . . . . ? C48 C49 C66 C67 142.8(6) . . . . ? C50 C49 C66 C67 2.0(8) . . . . ? C52 C51 C67 C69 0.1(10) . . . . ? C50 C51 C67 C69 142.0(7) . . . . ? C52 C51 C67 C66 -141.5(7) . . . . ? C50 C51 C67 C66 0.4(7) . . . . ? C65 C66 C67 C69 1.4(10) . . . . ? C49 C66 C67 C69 -142.2(7) . . . . ? C65 C66 C67 C51 142.1(6) . . . . ? C49 C66 C67 C51 -1.5(8) . . . . ? C31 C30 C68 C73 3.1(9) . . . . ? C29 C30 C68 C73 -144.0(6) . . . . ? C31 C30 C68 C9 162.9(5) . . . . ? C29 C30 C68 C9 15.8(6) . . . . ? O6 C9 C68 C73 -102.1(7) . . . . ? C5 C9 C68 C73 15.4(9) . . . . ? C8 C9 C68 C73 134.7(6) . . . . ? O6 C9 C68 C30 101.0(5) . . . . ? C5 C9 C68 C30 -141.5(5) . . . . ? C8 C9 C68 C30 -22.3(6) . . . . ? C51 C67 C69 C70 -137.0(7) . . . . ? C66 C67 C69 C70 -0.4(10) . . . . ? C51 C67 C69 C54 0.1(10) . . . . ? C66 C67 C69 C54 136.7(7) . . . . ? C53 C54 C69 C67 0.9(11) . . . . ? C55 C54 C69 C67 -141.1(7) . . . . ? C53 C54 C69 C70 142.6(7) . . . . ? C55 C54 C69 C70 0.7(7) . . . . ? C67 C69 C70 C75 -0.2(10) . . . . ? C54 C69 C70 C75 -142.1(7) . . . . ? C67 C69 C70 C71 141.6(6) . . . . ? C54 C69 C70 C71 -0.4(8) . . . . ? C56 C55 C71 C72 1.8(10) . . . . ? C54 C55 C71 C72 142.4(6) . . . . ? C56 C55 C71 C70 -140.1(6) . . . . ? C54 C55 C71 C70 0.5(7) . . . . ? C75 C70 C71 C72 -0.1(10) . . . . ? C69 C70 C71 C72 -142.2(7) . . . . ? C75 C70 C71 C55 142.1(6) . . . . ? C69 C70 C71 C55 -0.1(8) . . . . ? C55 C71 C72 C74 -138.5(7) . . . . ? C70 C71 C72 C74 -0.7(9) . . . . ? C55 C71 C72 C58 -1.1(9) . . . . ? C70 C71 C72 C58 136.6(7) . . . . ? C57 C58 C72 C71 -2.1(9) . . . . ? C59 C58 C72 C71 -143.6(6) . . . . ? C57 C58 C72 C74 140.1(6) . . . . ? C59 C58 C72 C74 -1.5(7) . . . . ? C30 C68 C73 C33 -0.6(8) . . . . ? C9 C68 C73 C33 -155.3(6) . . . . ? C30 C68 C73 C18 157.5(6) . . . . ? C9 C68 C73 C18 2.9(11) . . . . ? C32 C33 C73 C68 -2.5(9) . . . . ? C34 C33 C73 C68 144.6(6) . . . . ? C32 C33 C73 C18 -166.1(6) . . . . ? C34 C33 C73 C18 -19.0(6) . . . . ? O10 C18 C73 C68 -14.7(10) . . . . ? O4 C18 C73 C68 107.6(7) . . . . ? C35 C18 C73 C68 -133.3(7) . . . . ? O10 C18 C73 C33 145.4(5) . . . . ? O4 C18 C73 C33 -92.3(5) . . . . ? C35 C18 C73 C33 26.8(6) . . . . ? C71 C72 C74 C76 1.3(9) . . . . ? C58 C72 C74 C76 -140.1(6) . . . . ? C71 C72 C74 C60 143.2(6) . . . . ? C58 C72 C74 C60 1.8(7) . . . . ? C61 C60 C74 C76 -1.2(10) . . . . ? C59 C60 C74 C76 140.8(6) . . . . ? C61 C60 C74 C72 -143.5(6) . . . . ? C59 C60 C74 C72 -1.5(7) . . . . ? C69 C70 C75 C76 137.7(7) . . . . ? C71 C70 C75 C76 0.4(10) . . . . ? C69 C70 C75 C65 -0.2(10) . . . . ? C71 C70 C75 C65 -137.4(7) . . . . ? C66 C65 C75 C70 1.1(10) . . . . ? C64 C65 C75 C70 143.7(7) . . . . ? C66 C65 C75 C76 -141.3(7) . . . . ? C64 C65 C75 C76 1.2(8) . . . . ? C72 C74 C76 C63 138.1(7) . . . . ? C60 C74 C76 C63 0.4(10) . . . . ? C72 C74 C76 C75 -0.9(9) . . . . ? C60 C74 C76 C75 -138.6(7) . . . . ? C62 C63 C76 C74 0.1(10) . . . . ? C64 C63 C76 C74 -142.2(7) . . . . ? C62 C63 C76 C75 143.2(7) . . . . ? C64 C63 C76 C75 0.8(7) . . . . ? C70 C75 C76 C74 0.1(10) . . . . ? C65 C75 C76 C74 141.8(6) . . . . ? C70 C75 C76 C63 -143.0(6) . . . . ? C65 C75 C76 C63 -1.3(8) . . . . ? C77 C78 C79 C80 179.5(12) . . . . ? C80 C78 C79 C80 -1.5(14) 2_756 . . . ? C78 C79 C80 C78 1.5(14) . . . 2_756 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.626 _refine_diff_density_min -0.693 _refine_diff_density_rms 0.086 data_shelx _database_code_depnum_ccdc_archive 'CCDC 905499' #TrackingRef '14607_web_deposit_cif_file_1_Gan,Liangbing_1349923400.9a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C71 H17 Cl6 N O8' _chemical_formula_weight 1224.56 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 14.3061(15) _cell_length_b 14.457(2) _cell_length_c 15.4664(19) _cell_angle_alpha 76.592(15) _cell_angle_beta 66.580(13) _cell_angle_gamma 61.681(10) _cell_volume 2580.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 8853 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 27.9 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 0.401 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9241 _exptl_absorpt_correction_T_max 0.9534 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; Rigaku CrystalClear-SM Expert 2.0 r2 ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'Rigaku Saturn 724CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 14.22 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 21757 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0553 _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 16 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 25.02 _reflns_number_total 9068 _reflns_number_gt 6558 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0802P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9068 _refine_ls_number_parameters 816 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.0642 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1434 _refine_ls_wR_factor_gt 0.1379 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.004 _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 N1 N 0.43321(19) 0.22497(17) 0.46519(16) 0.0216(5) Uani 1 1 d . A . O1 O 0.58031(15) 0.41588(15) 0.14382(14) 0.0248(4) Uani 1 1 d . . . O2 O 0.65143(16) 0.46499(16) 0.27938(15) 0.0330(5) Uani 1 1 d . . . O3 O 0.47330(16) 0.41438(16) 0.42422(15) 0.0311(5) Uani 1 1 d . . . O4 O 0.20163(17) 0.33964(16) 0.47566(14) 0.0250(5) Uani 1 1 d . . . O5 O 0.33033(15) 0.34976(14) 0.13282(12) 0.0218(4) Uani 1 1 d . A . O6 O 0.27781(18) 0.28337(16) 0.20120(13) 0.0324(5) Uani 1 1 d D . . O8 O 0.53461(15) 0.21118(14) 0.30137(13) 0.0227(4) Uani 1 1 d . A . O7 O 0.56042(15) 0.22214(14) 0.14673(13) 0.0220(4) Uani 1 1 d . A . C1 C 0.1413(2) 0.9605(2) 0.2262(2) 0.0260(7) Uani 1 1 d . . . C2 C 0.1035(2) 0.9600(2) 0.3285(2) 0.0247(6) Uani 1 1 d . . . C3 C 0.0154(2) 0.9241(2) 0.3659(2) 0.0239(6) Uani 1 1 d . . . C4 C -0.0031(2) 0.9053(2) 0.2879(2) 0.0236(6) Uani 1 1 d . . . C5 C 0.0762(2) 0.9266(2) 0.20091(19) 0.0230(6) Uani 1 1 d . . . C6 C 0.1268(2) 0.8628(2) 0.12503(19) 0.0231(6) Uani 1 1 d . . . C7 C 0.2453(2) 0.8304(2) 0.07273(18) 0.0221(6) Uani 1 1 d . . . C8 C 0.3082(2) 0.8639(2) 0.0957(2) 0.0235(6) Uani 1 1 d . . . C9 C 0.2554(2) 0.9304(2) 0.1739(2) 0.0273(7) Uani 1 1 d . . . C10 C 0.3353(2) 0.9005(2) 0.2214(2) 0.0259(7) Uani 1 1 d . . . C11 C 0.3003(2) 0.8986(2) 0.3189(2) 0.0260(7) Uani 1 1 d . . . C12 C 0.1810(2) 0.9283(2) 0.3745(2) 0.0270(7) Uani 1 1 d . . . C13 C 0.1748(2) 0.8595(2) 0.4582(2) 0.0259(7) Uani 1 1 d . . . C14 C 0.0904(2) 0.8248(2) 0.49420(19) 0.0253(7) Uani 1 1 d . . . C15 C 0.0088(2) 0.8581(2) 0.44760(19) 0.0237(6) Uani 1 1 d . . . C16 C -0.0178(2) 0.7709(2) 0.45389(19) 0.0232(6) Uani 1 1 d . . . C17 C -0.0372(2) 0.7540(2) 0.37952(19) 0.0219(6) Uani 1 1 d . . . C18 C -0.0281(2) 0.8212(2) 0.29433(19) 0.0231(6) Uani 1 1 d . . . C19 C 0.0238(2) 0.7552(2) 0.2146(2) 0.0211(6) Uani 1 1 d . . . C20 C 0.1001(2) 0.7756(2) 0.13316(19) 0.0229(6) Uani 1 1 d . . . C21 C 0.2042(2) 0.6885(2) 0.08591(18) 0.0213(6) Uani 1 1 d . . . C22 C 0.2921(2) 0.7223(2) 0.05072(17) 0.0205(6) Uani 1 1 d . . . C23 C 0.3975(2) 0.6515(2) 0.05589(17) 0.0191(6) Uani 1 1 d . . . C24 C 0.4650(2) 0.6871(2) 0.07535(18) 0.0213(6) Uani 1 1 d . . . C25 C 0.4212(2) 0.7921(2) 0.0945(2) 0.0249(7) Uani 1 1 d . . . C26 C 0.4395(2) 0.8143(2) 0.1712(2) 0.0249(7) Uani 1 1 d . . . C27 C 0.5029(2) 0.7332(2) 0.2202(2) 0.0270(7) Uani 1 1 d . . . C28 C 0.4645(2) 0.7307(2) 0.3226(2) 0.0272(7) Uani 1 1 d . . . C29 C 0.3653(3) 0.8119(2) 0.3701(2) 0.0289(7) Uani 1 1 d . . . C30 C 0.2886(3) 0.7866(2) 0.4547(2) 0.0286(7) Uani 1 1 d . . . C31 C 0.3148(3) 0.6813(2) 0.4830(2) 0.0270(7) Uani 1 1 d . . . C32 C 0.2280(2) 0.6445(2) 0.51735(18) 0.0249(6) Uani 1 1 d . . . C33 C 0.1176(2) 0.7153(2) 0.52612(18) 0.0245(6) Uani 1 1 d . . . C34 C 0.0507(2) 0.6825(2) 0.50223(18) 0.0224(6) Uani 1 1 d . . . C35 C 0.0970(2) 0.5810(2) 0.47411(19) 0.0221(6) Uani 1 1 d . . . C36 C 0.0710(2) 0.5633(2) 0.40058(18) 0.0193(6) Uani 1 1 d . . . C37 C 0.0079(2) 0.6476(2) 0.3526(2) 0.0226(6) Uani 1 1 d . . . C38 C 0.0450(2) 0.6497(2) 0.25082(19) 0.0210(6) Uani 1 1 d . . . C39 C 0.1434(2) 0.5665(2) 0.20509(19) 0.0208(6) Uani 1 1 d . . . C40 C 0.2273(2) 0.5857(2) 0.12265(18) 0.0178(6) Uani 1 1 d . . . C41 C 0.3380(2) 0.5101(2) 0.12421(18) 0.0183(6) Uani 1 1 d . A . C42 C 0.4222(2) 0.5440(2) 0.09230(18) 0.0181(6) Uani 1 1 d . . . C43 C 0.5258(2) 0.5046(2) 0.11981(17) 0.0178(6) Uani 1 1 d . . . C44 C 0.5385(2) 0.6031(2) 0.12077(19) 0.0217(6) Uani 1 1 d . . . C45 C 0.5602(2) 0.6261(2) 0.1913(2) 0.0255(7) Uani 1 1 d . . . C46 C 0.5820(2) 0.5546(2) 0.2770(2) 0.0275(7) Uani 1 1 d . . . C47 C 0.4956(2) 0.6236(2) 0.3592(2) 0.0266(7) Uani 1 1 d . . . C48 C 0.4205(2) 0.5981(2) 0.4364(2) 0.0254(6) Uani 1 1 d . . . C49 C 0.4024(2) 0.5005(2) 0.45013(19) 0.0239(6) Uani 1 1 d . . . C50 C 0.2761(2) 0.5378(2) 0.48930(19) 0.0235(6) Uani 1 1 d . . . C51 C 0.2115(2) 0.5056(2) 0.46902(18) 0.0198(6) Uani 1 1 d . . . C52 C 0.2414(2) 0.4129(2) 0.41221(18) 0.0196(6) Uani 1 1 d . . . C53 C 0.1658(2) 0.4728(2) 0.35220(19) 0.0183(6) Uani 1 1 d . . . C54 C 0.2012(2) 0.4755(2) 0.25651(19) 0.0184(6) Uani 1 1 d . A . C55 C 0.3223(2) 0.4172(2) 0.19280(18) 0.0184(6) Uani 1 1 d . . . C56 C 0.3948(2) 0.35302(19) 0.25313(18) 0.0176(6) Uani 1 1 d . A . C57 C 0.5040(2) 0.2599(2) 0.22131(19) 0.0197(6) Uani 1 1 d . . . C58 C 0.4446(2) 0.2586(2) 0.38088(19) 0.0199(6) Uani 1 1 d . . . C59 C 0.3599(2) 0.3511(2) 0.34692(19) 0.0184(6) Uani 1 1 d . A . C60 C 0.5160(2) 0.1332(2) 0.49425(19) 0.0203(6) Uani 1 1 d . . . C61 C 0.6313(2) 0.0904(2) 0.44328(19) 0.0234(6) Uani 1 1 d . A . H61A H 0.6603 0.1229 0.3847 0.028 Uiso 1 1 calc R . . C62 C 0.7026(2) 0.0002(2) 0.4791(2) 0.0283(7) Uani 1 1 d . . . H62A H 0.7811 -0.0290 0.4446 0.034 Uiso 1 1 calc R A . C63 C 0.6627(2) -0.0487(2) 0.5637(2) 0.0275(7) Uani 1 1 d . A . H63A H 0.7128 -0.1123 0.5860 0.033 Uiso 1 1 calc R . . C64 C 0.5491(3) -0.0044(2) 0.6159(2) 0.0275(7) Uani 1 1 d . . . H64A H 0.5211 -0.0361 0.6754 0.033 Uiso 1 1 calc R A . C65 C 0.4759(2) 0.0870(2) 0.5810(2) 0.0245(6) Uani 1 1 d . A . H65A H 0.3979 0.1178 0.6171 0.029 Uiso 1 1 calc R . . C66 C 0.2588(4) 0.2289(4) 0.1477(4) 0.0269(13) Uani 0.654(5) 1 d PDU A 1 C67 C 0.3733(4) 0.1343(4) 0.1077(4) 0.0380(14) Uani 0.654(5) 1 d PDU A 1 H67A H 0.3967 0.0885 0.1599 0.057 Uiso 0.654(5) 1 calc PR A 1 H67B H 0.4301 0.1601 0.0682 0.057 Uiso 0.654(5) 1 calc PR A 1 H67C H 0.3654 0.0945 0.0697 0.057 Uiso 0.654(5) 1 calc PR A 1 C68 C 0.2117(5) 0.2939(4) 0.0694(4) 0.0482(16) Uani 0.654(5) 1 d PDU A 1 H68A H 0.1407 0.3545 0.0961 0.072 Uiso 0.654(5) 1 calc PR A 1 H68B H 0.1979 0.2503 0.0401 0.072 Uiso 0.654(5) 1 calc PR A 1 H68C H 0.2660 0.3185 0.0217 0.072 Uiso 0.654(5) 1 calc PR A 1 C69 C 0.1761(7) 0.1897(7) 0.2245(5) 0.037(2) Uani 0.654(5) 1 d PDU A 1 H69A H 0.1109 0.2493 0.2598 0.056 Uiso 0.654(5) 1 calc PR A 1 H69B H 0.2135 0.1382 0.2676 0.056 Uiso 0.654(5) 1 calc PR A 1 H69C H 0.1507 0.1565 0.1953 0.056 Uiso 0.654(5) 1 calc PR A 1 C66' C 0.2159(7) 0.2539(7) 0.1692(7) 0.0269(13) Uani 0.346(5) 1 d PDU A 2 C67' C 0.2919(8) 0.1955(7) 0.0797(6) 0.043(3) Uani 0.346(5) 1 d PDU A 2 H67D H 0.3124 0.2441 0.0285 0.064 Uiso 0.346(5) 1 calc PR A 2 H67E H 0.2523 0.1664 0.0629 0.064 Uiso 0.346(5) 1 calc PR A 2 H67F H 0.3604 0.1382 0.0897 0.064 Uiso 0.346(5) 1 calc PR A 2 C68' C 0.1202(7) 0.3576(6) 0.1546(7) 0.038(3) Uani 0.346(5) 1 d PDU A 2 H68D H 0.0746 0.3924 0.2145 0.057 Uiso 0.346(5) 1 calc PR A 2 H68E H 0.0728 0.3441 0.1323 0.057 Uiso 0.346(5) 1 calc PR A 2 H68F H 0.1515 0.4032 0.1077 0.057 Uiso 0.346(5) 1 calc PR A 2 C69' C 0.1765(12) 0.1873(11) 0.2534(8) 0.021(3) Uani 0.346(5) 1 d PDU A 2 H69D H 0.1368 0.2277 0.3101 0.031 Uiso 0.346(5) 1 calc PR A 2 H69E H 0.2417 0.1237 0.2617 0.031 Uiso 0.346(5) 1 calc PR A 2 H69F H 0.1253 0.1676 0.2428 0.031 Uiso 0.346(5) 1 calc PR A 2 C70 C 0.8259(3) 0.2583(2) 0.1749(2) 0.0315(7) Uani 1 1 d . . . H70 H 0.7432 0.3051 0.1946 0.038 Uiso 1 1 calc R . . C71 C 0.7279(3) 0.9729(3) 0.1188(2) 0.0361(8) Uani 1 1 d . . . H71 H 0.6962 1.0500 0.1011 0.043 Uiso 1 1 calc R . . Cl1 Cl 0.89788(9) 0.33024(9) 0.09546(8) 0.0642(3) Uani 1 1 d . . . Cl2 Cl 0.86644(9) 0.21385(9) 0.27578(7) 0.0643(3) Uani 1 1 d . . . Cl3 Cl 0.85229(7) 0.15107(7) 0.11987(6) 0.0414(2) Uani 1 1 d . . . Cl4 Cl 0.74495(7) 0.95491(7) 0.22851(6) 0.0402(2) Uani 1 1 d . . . Cl5 Cl 0.85801(7) 0.91020(7) 0.03171(6) 0.0490(3) Uani 1 1 d . . . Cl6 Cl 0.63293(9) 0.92505(11) 0.12657(8) 0.0716(4) Uani 1 1 d . . . H4A H 0.250(3) 0.313(3) 0.500(3) 0.046(12) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0228(12) 0.0199(12) 0.0187(13) 0.0009(10) -0.0063(10) -0.0080(10) O1 0.0217(10) 0.0213(11) 0.0306(11) -0.0028(8) -0.0102(9) -0.0068(8) O2 0.0247(11) 0.0291(12) 0.0419(13) -0.0025(10) -0.0147(10) -0.0059(10) O3 0.0243(11) 0.0229(11) 0.0416(12) -0.0055(10) -0.0155(9) -0.0015(9) O4 0.0231(11) 0.0233(11) 0.0214(11) 0.0044(9) -0.0021(9) -0.0112(9) O5 0.0299(11) 0.0197(10) 0.0198(10) -0.0015(8) -0.0065(8) -0.0149(8) O6 0.0496(13) 0.0335(12) 0.0230(11) -0.0010(9) -0.0036(10) -0.0317(11) O8 0.0201(10) 0.0175(10) 0.0208(10) -0.0016(8) -0.0045(8) -0.0022(8) O7 0.0209(10) 0.0160(10) 0.0205(10) -0.0023(8) -0.0023(8) -0.0044(8) C1 0.0295(16) 0.0107(13) 0.0309(17) 0.0010(12) -0.0092(13) -0.0051(12) C2 0.0282(15) 0.0089(13) 0.0291(16) -0.0070(11) -0.0055(13) -0.0025(11) C3 0.0189(14) 0.0130(13) 0.0293(16) -0.0098(12) -0.0040(12) 0.0017(11) C4 0.0178(14) 0.0111(13) 0.0296(16) -0.0031(11) -0.0086(12) 0.0048(11) C5 0.0236(14) 0.0123(13) 0.0246(15) 0.0005(11) -0.0114(12) 0.0008(11) C6 0.0240(15) 0.0149(14) 0.0224(15) 0.0033(11) -0.0101(12) -0.0020(11) C7 0.0296(15) 0.0167(14) 0.0151(14) 0.0050(11) -0.0078(12) -0.0085(12) C8 0.0263(15) 0.0170(14) 0.0234(15) 0.0033(11) -0.0040(12) -0.0118(12) C9 0.0312(16) 0.0171(14) 0.0320(17) 0.0002(12) -0.0065(13) -0.0131(12) C10 0.0293(15) 0.0162(14) 0.0347(17) -0.0026(12) -0.0065(13) -0.0146(12) C11 0.0320(16) 0.0197(14) 0.0339(17) -0.0072(12) -0.0103(13) -0.0148(13) C12 0.0319(16) 0.0136(14) 0.0332(17) -0.0100(12) -0.0077(13) -0.0066(12) C13 0.0319(16) 0.0212(15) 0.0234(15) -0.0137(12) -0.0059(13) -0.0075(12) C14 0.0284(15) 0.0205(15) 0.0172(14) -0.0099(12) -0.0032(12) -0.0026(12) C15 0.0202(14) 0.0189(14) 0.0191(15) -0.0066(12) 0.0017(11) -0.0026(11) C16 0.0140(13) 0.0241(15) 0.0186(14) -0.0044(12) 0.0020(11) -0.0028(11) C17 0.0093(12) 0.0250(15) 0.0252(15) -0.0049(12) -0.0027(11) -0.0033(11) C18 0.0145(13) 0.0225(15) 0.0266(16) -0.0020(12) -0.0074(12) -0.0028(11) C19 0.0168(13) 0.0198(14) 0.0276(15) -0.0027(12) -0.0126(12) -0.0037(11) C20 0.0239(14) 0.0230(15) 0.0239(15) 0.0027(12) -0.0158(12) -0.0072(12) C21 0.0240(14) 0.0234(15) 0.0170(14) -0.0013(11) -0.0093(12) -0.0085(12) C22 0.0273(15) 0.0191(14) 0.0104(13) 0.0020(11) -0.0050(11) -0.0086(12) C23 0.0206(14) 0.0216(14) 0.0089(13) -0.0003(11) 0.0002(10) -0.0088(12) C24 0.0243(14) 0.0183(14) 0.0161(14) 0.0008(11) 0.0004(11) -0.0115(12) C25 0.0263(15) 0.0244(15) 0.0234(15) 0.0008(12) -0.0024(12) -0.0160(13) C26 0.0271(15) 0.0199(15) 0.0302(16) 0.0004(12) -0.0046(13) -0.0167(12) C27 0.0219(15) 0.0303(16) 0.0355(17) -0.0027(13) -0.0059(13) -0.0189(13) C28 0.0260(15) 0.0307(17) 0.0391(18) -0.0086(14) -0.0150(13) -0.0168(13) C29 0.0354(17) 0.0267(16) 0.0368(17) -0.0093(13) -0.0170(14) -0.0156(14) C30 0.0352(17) 0.0315(17) 0.0271(16) -0.0120(13) -0.0132(13) -0.0137(14) C31 0.0332(16) 0.0331(17) 0.0211(15) -0.0053(13) -0.0174(13) -0.0108(13) C32 0.0313(16) 0.0297(16) 0.0137(14) -0.0005(12) -0.0102(12) -0.0110(13) C33 0.0272(15) 0.0273(16) 0.0119(13) -0.0074(11) -0.0014(11) -0.0075(13) C34 0.0184(14) 0.0254(15) 0.0119(13) -0.0017(11) 0.0036(11) -0.0073(12) C35 0.0197(14) 0.0206(14) 0.0163(14) 0.0009(11) -0.0002(11) -0.0066(12) C36 0.0137(13) 0.0198(14) 0.0190(14) 0.0005(11) -0.0011(11) -0.0072(11) C37 0.0161(13) 0.0271(15) 0.0274(15) -0.0020(12) -0.0063(12) -0.0120(12) C38 0.0145(13) 0.0244(15) 0.0271(15) -0.0039(12) -0.0093(12) -0.0077(11) C39 0.0200(14) 0.0233(15) 0.0240(15) -0.0027(12) -0.0087(12) -0.0114(12) C40 0.0187(13) 0.0185(14) 0.0190(14) -0.0014(11) -0.0102(11) -0.0068(11) C41 0.0198(13) 0.0213(14) 0.0132(13) -0.0050(11) -0.0044(11) -0.0075(11) C42 0.0198(14) 0.0175(14) 0.0134(13) -0.0064(10) -0.0010(11) -0.0065(11) C43 0.0179(13) 0.0187(14) 0.0135(13) -0.0030(11) -0.0019(11) -0.0070(11) C44 0.0170(13) 0.0229(15) 0.0226(15) -0.0024(12) -0.0001(11) -0.0113(12) C45 0.0173(14) 0.0269(16) 0.0306(16) -0.0054(13) -0.0003(12) -0.0127(12) C46 0.0189(14) 0.0295(17) 0.0391(18) -0.0051(13) -0.0103(13) -0.0122(13) C47 0.0237(15) 0.0324(17) 0.0328(17) -0.0054(13) -0.0182(13) -0.0104(13) C48 0.0271(15) 0.0318(17) 0.0245(15) -0.0008(13) -0.0168(13) -0.0118(13) C49 0.0300(16) 0.0304(17) 0.0175(14) 0.0008(12) -0.0168(12) -0.0116(14) C50 0.0243(15) 0.0266(15) 0.0173(14) 0.0001(12) -0.0076(12) -0.0091(12) C51 0.0201(14) 0.0179(14) 0.0137(13) 0.0023(11) -0.0020(11) -0.0065(11) C52 0.0164(13) 0.0183(14) 0.0182(14) 0.0019(11) -0.0036(11) -0.0059(11) C53 0.0173(13) 0.0167(14) 0.0237(15) -0.0011(11) -0.0073(11) -0.0089(11) C54 0.0176(13) 0.0174(13) 0.0226(15) -0.0036(11) -0.0046(11) -0.0099(11) C55 0.0209(14) 0.0153(13) 0.0208(14) -0.0028(11) -0.0069(11) -0.0084(11) C56 0.0149(13) 0.0134(13) 0.0224(15) -0.0006(11) -0.0044(11) -0.0062(11) C57 0.0217(14) 0.0188(14) 0.0185(15) 0.0026(12) -0.0065(12) -0.0104(11) C58 0.0195(14) 0.0165(14) 0.0195(15) -0.0024(11) -0.0024(11) -0.0071(11) C59 0.0170(13) 0.0111(13) 0.0246(15) 0.0002(11) -0.0066(11) -0.0049(10) C60 0.0218(14) 0.0138(13) 0.0256(15) -0.0017(11) -0.0107(12) -0.0053(11) C61 0.0246(15) 0.0278(16) 0.0195(14) -0.0009(12) -0.0093(12) -0.0110(12) C62 0.0231(15) 0.0299(16) 0.0307(17) -0.0100(13) -0.0126(13) -0.0039(13) C63 0.0315(16) 0.0192(15) 0.0358(17) -0.0013(13) -0.0216(14) -0.0055(12) C64 0.0390(18) 0.0228(15) 0.0272(16) 0.0053(12) -0.0170(14) -0.0165(13) C65 0.0250(15) 0.0220(15) 0.0255(15) -0.0008(12) -0.0081(12) -0.0098(12) C66 0.023(3) 0.028(3) 0.036(3) 0.003(2) -0.011(3) -0.016(3) C67 0.038(3) 0.024(3) 0.046(3) -0.005(2) -0.002(2) -0.017(2) C68 0.056(4) 0.042(3) 0.063(4) -0.002(3) -0.033(3) -0.024(3) C69 0.039(4) 0.025(3) 0.049(5) -0.005(3) -0.007(3) -0.020(3) C66' 0.023(3) 0.028(3) 0.036(3) 0.003(2) -0.011(3) -0.016(3) C67' 0.062(6) 0.040(6) 0.030(5) -0.013(4) -0.008(4) -0.026(5) C68' 0.037(5) 0.036(5) 0.055(6) 0.007(4) -0.026(4) -0.023(4) C69' 0.024(5) 0.017(5) 0.026(6) 0.000(4) -0.005(4) -0.016(4) C70 0.0238(15) 0.0329(17) 0.0313(17) -0.0041(14) -0.0089(13) -0.0064(13) C71 0.0344(18) 0.0334(18) 0.0309(18) -0.0004(14) -0.0086(14) -0.0095(14) Cl1 0.0621(6) 0.0648(7) 0.0679(7) -0.0110(5) 0.0005(5) -0.0436(6) Cl2 0.0672(7) 0.0643(7) 0.0459(6) -0.0192(5) -0.0359(5) 0.0045(5) Cl3 0.0487(5) 0.0361(5) 0.0463(5) -0.0018(4) -0.0249(4) -0.0164(4) Cl4 0.0395(5) 0.0472(5) 0.0355(5) 0.0035(4) -0.0151(4) -0.0204(4) Cl5 0.0392(5) 0.0372(5) 0.0383(5) -0.0011(4) -0.0003(4) -0.0021(4) Cl6 0.0564(6) 0.1163(10) 0.0626(7) -0.0335(7) -0.0117(5) -0.0467(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C58 1.255(3) . ? N1 C60 1.422(3) . ? O1 C43 1.205(3) . ? O2 C46 1.205(3) . ? O3 C49 1.204(3) . ? O4 C52 1.433(3) . ? O4 H4A 0.81(4) . ? O5 C55 1.433(3) . ? O5 O6 1.479(2) . ? O6 C66' 1.419(8) . ? O6 C66 1.436(5) . ? O8 C58 1.391(3) . ? O8 C57 1.398(3) . ? O7 C57 1.189(3) . ? C1 C9 1.395(4) . ? C1 C5 1.440(4) . ? C1 C2 1.454(4) . ? C2 C12 1.392(4) . ? C2 C3 1.447(4) . ? C3 C15 1.396(4) . ? C3 C4 1.441(4) . ? C4 C18 1.394(4) . ? C4 C5 1.454(4) . ? C5 C6 1.395(4) . ? C6 C7 1.442(4) . ? C6 C20 1.448(4) . ? C7 C8 1.385(4) . ? C7 C22 1.441(4) . ? C8 C25 1.444(4) . ? C8 C9 1.444(4) . ? C9 C10 1.444(4) . ? C10 C11 1.384(4) . ? C10 C26 1.465(4) . ? C11 C29 1.444(4) . ? C11 C12 1.464(4) . ? C12 C13 1.438(4) . ? C13 C14 1.389(4) . ? C13 C30 1.446(4) . ? C14 C15 1.445(4) . ? C14 C33 1.451(4) . ? C15 C16 1.453(4) . ? C16 C17 1.382(4) . ? C16 C34 1.450(4) . ? C17 C18 1.445(4) . ? C17 C37 1.448(4) . ? C18 C19 1.458(4) . ? C19 C20 1.381(4) . ? C19 C38 1.425(4) . ? C20 C21 1.455(4) . ? C21 C40 1.391(4) . ? C21 C22 1.425(4) . ? C22 C23 1.387(4) . ? C23 C24 1.435(4) . ? C23 C42 1.445(4) . ? C24 C25 1.395(4) . ? C24 C44 1.433(4) . ? C25 C26 1.442(4) . ? C26 C27 1.378(4) . ? C27 C45 1.447(4) . ? C27 C28 1.453(4) . ? C28 C29 1.387(4) . ? C28 C47 1.434(4) . ? C29 C30 1.438(4) . ? C30 C31 1.388(4) . ? C31 C48 1.437(4) . ? C31 C32 1.443(4) . ? C32 C33 1.385(4) . ? C32 C50 1.451(4) . ? C33 C34 1.439(4) . ? C34 C35 1.388(4) . ? C35 C36 1.435(4) . ? C35 C51 1.457(4) . ? C36 C37 1.387(4) . ? C36 C53 1.440(4) . ? C37 C38 1.445(4) . ? C38 C39 1.388(4) . ? C39 C54 1.433(4) . ? C39 C40 1.442(4) . ? C40 C41 1.442(4) . ? C41 C42 1.381(4) . ? C41 C55 1.555(4) . ? C42 C43 1.513(4) . ? C43 C44 1.522(4) . ? C44 C45 1.391(4) . ? C45 C46 1.519(4) . ? C46 C47 1.520(4) . ? C47 C48 1.367(4) . ? C48 C49 1.504(4) . ? C49 C50 1.510(4) . ? C50 C51 1.370(4) . ? C51 C52 1.566(4) . ? C52 C59 1.521(4) . ? C52 C53 1.522(4) . ? C53 C54 1.358(4) . ? C54 C55 1.525(4) . ? C55 C56 1.504(4) . ? C56 C59 1.331(4) . ? C56 C57 1.482(4) . ? C58 C59 1.474(4) . ? C60 C65 1.383(4) . ? C60 C61 1.396(4) . ? C61 C62 1.378(4) . ? C61 H61A 0.9500 . ? C62 C63 1.378(4) . ? C62 H62A 0.9500 . ? C63 C64 1.383(4) . ? C63 H63A 0.9500 . ? C64 C65 1.393(4) . ? C64 H64A 0.9500 . ? C65 H65A 0.9500 . ? C66 C68 1.524(6) . ? C66 C69 1.530(7) . ? C66 C67 1.548(6) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C66' C67' 1.511(8) . ? C66' C69' 1.513(8) . ? C66' C68' 1.522(8) . ? C67' H67D 0.9800 . ? C67' H67E 0.9800 . ? C67' H67F 0.9800 . ? C68' H68D 0.9800 . ? C68' H68E 0.9800 . ? C68' H68F 0.9800 . ? C69' H69D 0.9800 . ? C69' H69E 0.9800 . ? C69' H69F 0.9800 . ? C70 Cl1 1.751(3) . ? C70 Cl3 1.753(3) . ? C70 Cl2 1.756(3) . ? C70 H70 1.0000 . ? C71 Cl6 1.750(4) . ? C71 Cl4 1.752(3) . ? C71 Cl5 1.753(3) . ? C71 H71 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 C58 N1 C60 124.1(2) . . ? C52 O4 H4A 98(3) . . ? C55 O5 O6 102.44(16) . . ? C66' O6 C66 22.1(4) . . ? C66' O6 O5 115.0(4) . . ? C66 O6 O5 106.8(2) . . ? C58 O8 C57 108.7(2) . . ? C9 C1 C5 119.9(3) . . ? C9 C1 C2 119.8(3) . . ? C5 C1 C2 108.5(2) . . ? C12 C2 C3 119.6(3) . . ? C12 C2 C1 120.2(3) . . ? C3 C2 C1 107.4(3) . . ? C15 C3 C4 120.1(3) . . ? C15 C3 C2 119.8(3) . . ? C4 C3 C2 108.4(2) . . ? C18 C4 C3 119.8(3) . . ? C18 C4 C5 119.5(3) . . ? C3 C4 C5 108.1(3) . . ? C6 C5 C1 120.4(3) . . ? C6 C5 C4 119.9(3) . . ? C1 C5 C4 107.6(2) . . ? C5 C6 C7 119.3(3) . . ? C5 C6 C20 119.8(2) . . ? C7 C6 C20 108.3(2) . . ? C8 C7 C22 119.5(3) . . ? C8 C7 C6 120.8(3) . . ? C22 C7 C6 107.4(2) . . ? C7 C8 C25 120.3(3) . . ? C7 C8 C9 119.8(3) . . ? C25 C8 C9 108.0(3) . . ? C1 C9 C8 119.9(3) . . ? C1 C9 C10 120.0(3) . . ? C8 C9 C10 108.4(3) . . ? C11 C10 C9 120.5(3) . . ? C11 C10 C26 119.2(3) . . ? C9 C10 C26 107.5(3) . . ? C10 C11 C29 120.2(3) . . ? C10 C11 C12 120.0(3) . . ? C29 C11 C12 107.3(2) . . ? C2 C12 C13 120.6(3) . . ? C2 C12 C11 119.5(3) . . ? C13 C12 C11 107.9(3) . . ? C14 C13 C12 120.0(3) . . ? C14 C13 C30 119.6(3) . . ? C12 C13 C30 108.1(2) . . ? C13 C14 C15 120.0(3) . . ? C13 C14 C33 119.7(3) . . ? C15 C14 C33 107.4(3) . . ? C3 C15 C14 120.1(3) . . ? C3 C15 C16 119.7(3) . . ? C14 C15 C16 108.4(2) . . ? C17 C16 C34 119.8(3) . . ? C17 C16 C15 120.1(3) . . ? C34 C16 C15 107.5(3) . . ? C16 C17 C18 120.0(3) . . ? C16 C17 C37 119.7(3) . . ? C18 C17 C37 107.9(2) . . ? C4 C18 C17 120.2(3) . . ? C4 C18 C19 120.6(2) . . ? C17 C18 C19 107.6(2) . . ? C20 C19 C38 120.4(2) . . ? C20 C19 C18 119.1(3) . . ? C38 C19 C18 108.1(2) . . ? C19 C20 C6 121.0(3) . . ? C19 C20 C21 119.4(2) . . ? C6 C20 C21 107.3(2) . . ? C40 C21 C22 119.2(2) . . ? C40 C21 C20 120.5(2) . . ? C22 C21 C20 107.9(2) . . ? C23 C22 C21 118.5(2) . . ? C23 C22 C7 120.3(3) . . ? C21 C22 C7 109.0(2) . . ? C22 C23 C24 120.2(2) . . ? C22 C23 C42 122.3(2) . . ? C24 C23 C42 109.7(2) . . ? C25 C24 C44 122.2(3) . . ? C25 C24 C23 119.6(3) . . ? C44 C24 C23 109.8(2) . . ? C24 C25 C26 118.0(3) . . ? C24 C25 C8 119.9(3) . . ? C26 C25 C8 108.5(2) . . ? C27 C26 C25 120.0(3) . . ? C27 C26 C10 120.3(3) . . ? C25 C26 C10 107.6(3) . . ? C26 C27 C45 121.2(3) . . ? C26 C27 C28 120.1(3) . . ? C45 C27 C28 108.4(3) . . ? C29 C28 C47 121.6(3) . . ? C29 C28 C27 119.5(3) . . ? C47 C28 C27 109.3(3) . . ? C28 C29 C30 118.8(3) . . ? C28 C29 C11 120.6(3) . . ? C30 C29 C11 108.4(3) . . ? C31 C30 C29 118.4(3) . . ? C31 C30 C13 120.4(3) . . ? C29 C30 C13 108.2(3) . . ? C30 C31 C48 122.3(3) . . ? C30 C31 C32 119.9(3) . . ? C48 C31 C32 109.1(3) . . ? C33 C32 C31 119.8(3) . . ? C33 C32 C50 122.4(3) . . ? C31 C32 C50 109.3(2) . . ? C32 C33 C34 118.2(3) . . ? C32 C33 C14 120.3(3) . . ? C34 C33 C14 108.5(3) . . ? C35 C34 C33 119.4(3) . . ? C35 C34 C16 120.4(3) . . ? C33 C34 C16 108.1(2) . . ? C34 C35 C36 119.5(3) . . ? C34 C35 C51 121.9(3) . . ? C36 C35 C51 109.1(2) . . ? C37 C36 C35 120.3(3) . . ? C37 C36 C53 121.3(2) . . ? C35 C36 C53 107.9(2) . . ? C36 C37 C38 119.2(2) . . ? C36 C37 C17 120.2(3) . . ? C38 C37 C17 107.8(2) . . ? C39 C38 C19 120.3(2) . . ? C39 C38 C37 118.1(2) . . ? C19 C38 C37 108.6(2) . . ? C38 C39 C54 121.6(2) . . ? C38 C39 C40 120.5(2) . . ? C54 C39 C40 107.6(2) . . ? C21 C40 C41 122.6(2) . . ? C21 C40 C39 118.7(2) . . ? C41 C40 C39 109.3(2) . . ? C42 C41 C40 117.9(2) . . ? C42 C41 C55 132.3(2) . . ? C40 C41 C55 106.4(2) . . ? C41 C42 C23 119.3(2) . . ? C41 C42 C43 129.9(2) . . ? C23 C42 C43 106.6(2) . . ? O1 C43 C42 127.4(2) . . ? O1 C43 C44 127.4(3) . . ? C42 C43 C44 105.0(2) . . ? C45 C44 C24 119.0(3) . . ? C45 C44 C43 125.4(2) . . ? C24 C44 C43 107.0(2) . . ? C44 C45 C27 118.9(3) . . ? C44 C45 C46 125.7(3) . . ? C27 C45 C46 107.0(3) . . ? O2 C46 C45 128.5(3) . . ? O2 C46 C47 128.2(3) . . ? C45 C46 C47 103.3(2) . . ? C48 C47 C28 119.8(3) . . ? C48 C47 C46 126.1(3) . . ? C28 C47 C46 106.9(2) . . ? C47 C48 C31 118.5(3) . . ? C47 C48 C49 125.5(3) . . ? C31 C48 C49 108.0(2) . . ? O3 C49 C48 126.6(3) . . ? O3 C49 C50 127.7(3) . . ? C48 C49 C50 105.1(2) . . ? C51 C50 C32 119.4(3) . . ? C51 C50 C49 128.6(3) . . ? C32 C50 C49 106.8(2) . . ? C50 C51 C35 118.5(3) . . ? C50 C51 C52 132.9(2) . . ? C35 C51 C52 106.0(2) . . ? O4 C52 C59 108.3(2) . . ? O4 C52 C53 108.4(2) . . ? C59 C52 C53 108.0(2) . . ? O4 C52 C51 109.2(2) . . ? C59 C52 C51 122.6(2) . . ? C53 C52 C51 99.4(2) . . ? C54 C53 C36 119.0(2) . . ? C54 C53 C52 125.2(2) . . ? C36 C53 C52 109.3(2) . . ? C53 C54 C39 120.1(2) . . ? C53 C54 C55 125.3(2) . . ? C39 C54 C55 109.1(2) . . ? O5 C55 C56 109.6(2) . . ? O5 C55 C54 111.7(2) . . ? C56 C55 C54 109.0(2) . . ? O5 C55 C41 103.3(2) . . ? C56 C55 C41 123.1(2) . . ? C54 C55 C41 99.7(2) . . ? C59 C56 C57 108.0(2) . . ? C59 C56 C55 125.5(2) . . ? C57 C56 C55 124.2(2) . . ? O7 C57 O8 120.6(2) . . ? O7 C57 C56 132.5(3) . . ? O8 C57 C56 106.8(2) . . ? N1 C58 O8 126.8(2) . . ? N1 C58 C59 126.2(2) . . ? O8 C58 C59 106.9(2) . . ? C56 C59 C58 108.9(2) . . ? C56 C59 C52 126.8(2) . . ? C58 C59 C52 122.4(2) . . ? C65 C60 C61 119.7(3) . . ? C65 C60 N1 115.3(2) . . ? C61 C60 N1 124.9(2) . . ? C62 C61 C60 119.1(3) . . ? C62 C61 H61A 120.5 . . ? C60 C61 H61A 120.5 . . ? C61 C62 C63 121.5(3) . . ? C61 C62 H62A 119.2 . . ? C63 C62 H62A 119.2 . . ? C62 C63 C64 119.5(3) . . ? C62 C63 H63A 120.3 . . ? C64 C63 H63A 120.3 . . ? C63 C64 C65 119.7(3) . . ? C63 C64 H64A 120.1 . . ? C65 C64 H64A 120.1 . . ? C60 C65 C64 120.4(3) . . ? C60 C65 H65A 119.8 . . ? C64 C65 H65A 119.8 . . ? O6 C66 C68 116.3(4) . . ? O6 C66 C69 101.9(5) . . ? C68 C66 C69 111.4(5) . . ? O6 C66 C67 106.0(4) . . ? C68 C66 C67 111.0(4) . . ? C69 C66 C67 109.8(4) . . ? O6 C66' C67' 109.7(7) . . ? O6 C66' C69' 101.2(9) . . ? C67' C66' C69' 114.4(7) . . ? O6 C66' C68' 104.3(6) . . ? C67' C66' C68' 113.1(7) . . ? C69' C66' C68' 112.9(7) . . ? C66' C67' H67D 109.5 . . ? C66' C67' H67E 109.5 . . ? H67D C67' H67E 109.5 . . ? C66' C67' H67F 109.5 . . ? H67D C67' H67F 109.5 . . ? H67E C67' H67F 109.5 . . ? C66' C68' H68D 109.5 . . ? C66' C68' H68E 109.5 . . ? H68D C68' H68E 109.5 . . ? C66' C68' H68F 109.5 . . ? H68D C68' H68F 109.5 . . ? H68E C68' H68F 109.5 . . ? C66' C69' H69D 109.5 . . ? C66' C69' H69E 109.5 . . ? H69D C69' H69E 109.5 . . ? C66' C69' H69F 109.5 . . ? H69D C69' H69F 109.5 . . ? H69E C69' H69F 109.5 . . ? Cl1 C70 Cl3 109.92(17) . . ? Cl1 C70 Cl2 111.00(19) . . ? Cl3 C70 Cl2 109.94(17) . . ? Cl1 C70 H70 108.6 . . ? Cl3 C70 H70 108.6 . . ? Cl2 C70 H70 108.6 . . ? Cl6 C71 Cl4 109.91(17) . . ? Cl6 C71 Cl5 110.68(19) . . ? Cl4 C71 Cl5 110.59(19) . . ? Cl6 C71 H71 108.5 . . ? Cl4 C71 H71 108.5 . . ? Cl5 C71 H71 108.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C55 O5 O6 C66' 145.4(4) . . . . ? C55 O5 O6 C66 167.5(3) . . . . ? C9 C1 C2 C12 -0.8(4) . . . . ? C5 C1 C2 C12 142.1(3) . . . . ? C9 C1 C2 C3 -142.2(3) . . . . ? C5 C1 C2 C3 0.7(3) . . . . ? C12 C2 C3 C15 0.0(4) . . . . ? C1 C2 C3 C15 141.7(3) . . . . ? C12 C2 C3 C4 -143.1(3) . . . . ? C1 C2 C3 C4 -1.4(3) . . . . ? C15 C3 C4 C18 0.3(4) . . . . ? C2 C3 C4 C18 143.2(2) . . . . ? C15 C3 C4 C5 -141.3(2) . . . . ? C2 C3 C4 C5 1.6(3) . . . . ? C9 C1 C5 C6 0.7(4) . . . . ? C2 C1 C5 C6 -142.2(3) . . . . ? C9 C1 C5 C4 143.2(3) . . . . ? C2 C1 C5 C4 0.3(3) . . . . ? C18 C4 C5 C6 -0.3(4) . . . . ? C3 C4 C5 C6 141.5(3) . . . . ? C18 C4 C5 C1 -143.0(3) . . . . ? C3 C4 C5 C1 -1.2(3) . . . . ? C1 C5 C6 C7 0.6(4) . . . . ? C4 C5 C6 C7 -137.4(3) . . . . ? C1 C5 C6 C20 138.0(3) . . . . ? C4 C5 C6 C20 0.0(4) . . . . ? C5 C6 C7 C8 -1.5(4) . . . . ? C20 C6 C7 C8 -143.3(3) . . . . ? C5 C6 C7 C22 140.4(3) . . . . ? C20 C6 C7 C22 -1.4(3) . . . . ? C22 C7 C8 C25 2.0(4) . . . . ? C6 C7 C8 C25 139.5(3) . . . . ? C22 C7 C8 C9 -136.3(3) . . . . ? C6 C7 C8 C9 1.2(4) . . . . ? C5 C1 C9 C8 -1.0(4) . . . . ? C2 C1 C9 C8 137.7(3) . . . . ? C5 C1 C9 C10 -139.8(3) . . . . ? C2 C1 C9 C10 -1.1(4) . . . . ? C7 C8 C9 C1 0.1(4) . . . . ? C25 C8 C9 C1 -142.8(3) . . . . ? C7 C8 C9 C10 143.0(3) . . . . ? C25 C8 C9 C10 0.2(3) . . . . ? C1 C9 C10 C11 1.9(4) . . . . ? C8 C9 C10 C11 -141.1(3) . . . . ? C1 C9 C10 C26 143.2(3) . . . . ? C8 C9 C10 C26 0.2(3) . . . . ? C9 C10 C11 C29 136.4(3) . . . . ? C26 C10 C11 C29 -0.6(4) . . . . ? C9 C10 C11 C12 -0.8(4) . . . . ? C26 C10 C11 C12 -137.8(3) . . . . ? C3 C2 C12 C13 0.6(4) . . . . ? C1 C2 C12 C13 -136.2(3) . . . . ? C3 C2 C12 C11 138.7(3) . . . . ? C1 C2 C12 C11 1.9(4) . . . . ? C10 C11 C12 C2 -1.1(4) . . . . ? C29 C11 C12 C2 -143.1(3) . . . . ? C10 C11 C12 C13 141.7(3) . . . . ? C29 C11 C12 C13 -0.3(3) . . . . ? C2 C12 C13 C14 -0.5(4) . . . . ? C11 C12 C13 C14 -142.8(3) . . . . ? C2 C12 C13 C30 141.6(3) . . . . ? C11 C12 C13 C30 -0.7(3) . . . . ? C12 C13 C14 C15 -0.1(4) . . . . ? C30 C13 C14 C15 -137.9(3) . . . . ? C12 C13 C14 C33 136.5(3) . . . . ? C30 C13 C14 C33 -1.3(4) . . . . ? C4 C3 C15 C14 138.2(3) . . . . ? C2 C3 C15 C14 -0.6(4) . . . . ? C4 C3 C15 C16 -0.6(4) . . . . ? C2 C3 C15 C16 -139.3(3) . . . . ? C13 C14 C15 C3 0.7(4) . . . . ? C33 C14 C15 C3 -140.6(2) . . . . ? C13 C14 C15 C16 143.5(2) . . . . ? C33 C14 C15 C16 2.2(3) . . . . ? C3 C15 C16 C17 -0.4(4) . . . . ? C14 C15 C16 C17 -143.5(2) . . . . ? C3 C15 C16 C34 141.3(2) . . . . ? C14 C15 C16 C34 -1.7(3) . . . . ? C34 C16 C17 C18 -135.4(3) . . . . ? C15 C16 C17 C18 1.7(4) . . . . ? C34 C16 C17 C37 2.0(4) . . . . ? C15 C16 C17 C37 139.2(3) . . . . ? C3 C4 C18 C17 0.9(4) . . . . ? C5 C4 C18 C17 138.2(3) . . . . ? C3 C4 C18 C19 -137.7(3) . . . . ? C5 C4 C18 C19 -0.4(4) . . . . ? C16 C17 C18 C4 -1.9(4) . . . . ? C37 C17 C18 C4 -143.8(3) . . . . ? C16 C17 C18 C19 141.4(3) . . . . ? C37 C17 C18 C19 -0.5(3) . . . . ? C4 C18 C19 C20 1.4(4) . . . . ? C17 C18 C19 C20 -141.8(3) . . . . ? C4 C18 C19 C38 143.7(3) . . . . ? C17 C18 C19 C38 0.5(3) . . . . ? C38 C19 C20 C6 -139.3(3) . . . . ? C18 C19 C20 C6 -1.7(4) . . . . ? C38 C19 C20 C21 -1.8(4) . . . . ? C18 C19 C20 C21 135.8(3) . . . . ? C5 C6 C20 C19 1.0(4) . . . . ? C7 C6 C20 C19 142.5(3) . . . . ? C5 C6 C20 C21 -141.0(3) . . . . ? C7 C6 C20 C21 0.6(3) . . . . ? C19 C20 C21 C40 -0.4(4) . . . . ? C6 C20 C21 C40 142.2(3) . . . . ? C19 C20 C21 C22 -142.2(3) . . . . ? C6 C20 C21 C22 0.5(3) . . . . ? C40 C21 C22 C23 -1.1(4) . . . . ? C20 C21 C22 C23 141.2(3) . . . . ? C40 C21 C22 C7 -143.7(3) . . . . ? C20 C21 C22 C7 -1.4(3) . . . . ? C8 C7 C22 C23 2.4(4) . . . . ? C6 C7 C22 C23 -140.1(3) . . . . ? C8 C7 C22 C21 144.2(3) . . . . ? C6 C7 C22 C21 1.7(3) . . . . ? C21 C22 C23 C24 -143.6(3) . . . . ? C7 C22 C23 C24 -5.3(4) . . . . ? C21 C22 C23 C42 2.4(4) . . . . ? C7 C22 C23 C42 140.7(3) . . . . ? C22 C23 C24 C25 3.7(4) . . . . ? C42 C23 C24 C25 -146.1(2) . . . . ? C22 C23 C24 C44 152.5(2) . . . . ? C42 C23 C24 C44 2.6(3) . . . . ? C44 C24 C25 C26 -8.1(4) . . . . ? C23 C24 C25 C26 136.6(3) . . . . ? C44 C24 C25 C8 -144.1(3) . . . . ? C23 C24 C25 C8 0.7(4) . . . . ? C7 C8 C25 C24 -3.6(4) . . . . ? C9 C8 C25 C24 139.0(3) . . . . ? C7 C8 C25 C26 -143.2(3) . . . . ? C9 C8 C25 C26 -0.6(3) . . . . ? C24 C25 C26 C27 2.9(4) . . . . ? C8 C25 C26 C27 143.4(3) . . . . ? C24 C25 C26 C10 -139.8(2) . . . . ? C8 C25 C26 C10 0.8(3) . . . . ? C11 C10 C26 C27 -1.2(4) . . . . ? C9 C10 C26 C27 -143.1(3) . . . . ? C11 C10 C26 C25 141.3(3) . . . . ? C9 C10 C26 C25 -0.6(3) . . . . ? C25 C26 C27 C45 5.4(4) . . . . ? C10 C26 C27 C45 143.3(3) . . . . ? C25 C26 C27 C28 -135.6(3) . . . . ? C10 C26 C27 C28 2.3(4) . . . . ? C26 C27 C28 C29 -1.7(4) . . . . ? C45 C27 C28 C29 -147.2(3) . . . . ? C26 C27 C28 C47 144.9(3) . . . . ? C45 C27 C28 C47 -0.6(3) . . . . ? C47 C28 C29 C30 -4.4(4) . . . . ? C27 C28 C29 C30 138.0(3) . . . . ? C47 C28 C29 C11 -142.4(3) . . . . ? C27 C28 C29 C11 0.0(4) . . . . ? C10 C11 C29 C28 1.2(4) . . . . ? C12 C11 C29 C28 143.1(3) . . . . ? C10 C11 C29 C30 -140.7(3) . . . . ? C12 C11 C29 C30 1.3(3) . . . . ? C28 C29 C30 C31 -2.7(4) . . . . ? C11 C29 C30 C31 139.9(3) . . . . ? C28 C29 C30 C13 -144.4(3) . . . . ? C11 C29 C30 C13 -1.7(3) . . . . ? C14 C13 C30 C31 3.0(4) . . . . ? C12 C13 C30 C31 -139.3(3) . . . . ? C14 C13 C30 C29 143.7(3) . . . . ? C12 C13 C30 C29 1.5(3) . . . . ? C29 C30 C31 C48 6.3(4) . . . . ? C13 C30 C31 C48 143.2(3) . . . . ? C29 C30 C31 C32 -137.7(3) . . . . ? C13 C30 C31 C32 -0.8(4) . . . . ? C30 C31 C32 C33 -3.1(4) . . . . ? C48 C31 C32 C33 -151.4(3) . . . . ? C30 C31 C32 C50 145.8(3) . . . . ? C48 C31 C32 C50 -2.6(3) . . . . ? C31 C32 C33 C34 141.8(3) . . . . ? C50 C32 C33 C34 -2.8(4) . . . . ? C31 C32 C33 C14 4.8(4) . . . . ? C50 C32 C33 C14 -139.9(3) . . . . ? C13 C14 C33 C32 -2.6(4) . . . . ? C15 C14 C33 C32 138.8(3) . . . . ? C13 C14 C33 C34 -143.3(3) . . . . ? C15 C14 C33 C34 -1.9(3) . . . . ? C32 C33 C34 C35 1.9(4) . . . . ? C14 C33 C34 C35 143.5(2) . . . . ? C32 C33 C34 C16 -140.8(2) . . . . ? C14 C33 C34 C16 0.8(3) . . . . ? C17 C16 C34 C35 0.1(4) . . . . ? C15 C16 C34 C35 -141.7(3) . . . . ? C17 C16 C34 C33 142.4(3) . . . . ? C15 C16 C34 C33 0.5(3) . . . . ? C33 C34 C35 C36 -141.9(3) . . . . ? C16 C34 C35 C36 -3.8(4) . . . . ? C33 C34 C35 C51 0.8(4) . . . . ? C16 C34 C35 C51 138.9(3) . . . . ? C34 C35 C36 C37 5.3(4) . . . . ? C51 C35 C36 C37 -141.7(2) . . . . ? C34 C35 C36 C53 150.5(2) . . . . ? C51 C35 C36 C53 3.5(3) . . . . ? C35 C36 C37 C38 133.8(3) . . . . ? C53 C36 C37 C38 -6.7(4) . . . . ? C35 C36 C37 C17 -3.2(4) . . . . ? C53 C36 C37 C17 -143.6(3) . . . . ? C16 C17 C37 C36 -0.5(4) . . . . ? C18 C17 C37 C36 141.5(2) . . . . ? C16 C17 C37 C38 -141.8(2) . . . . ? C18 C17 C37 C38 0.3(3) . . . . ? C20 C19 C38 C39 0.8(4) . . . . ? C18 C19 C38 C39 -141.0(3) . . . . ? C20 C19 C38 C37 141.4(3) . . . . ? C18 C19 C38 C37 -0.3(3) . . . . ? C36 C37 C38 C39 -0.1(4) . . . . ? C17 C37 C38 C39 141.7(3) . . . . ? C36 C37 C38 C19 -141.7(3) . . . . ? C17 C37 C38 C19 0.0(3) . . . . ? C19 C38 C39 C54 143.2(3) . . . . ? C37 C38 C39 C54 6.2(4) . . . . ? C19 C38 C39 C40 2.5(4) . . . . ? C37 C38 C39 C40 -134.6(3) . . . . ? C22 C21 C40 C41 -1.9(4) . . . . ? C20 C21 C40 C41 -139.4(3) . . . . ? C22 C21 C40 C39 141.1(3) . . . . ? C20 C21 C40 C39 3.6(4) . . . . ? C38 C39 C40 C21 -4.6(4) . . . . ? C54 C39 C40 C21 -150.2(3) . . . . ? C38 C39 C40 C41 142.9(3) . . . . ? C54 C39 C40 C41 -2.7(3) . . . . ? C21 C40 C41 C42 3.5(4) . . . . ? C39 C40 C41 C42 -142.5(2) . . . . ? C21 C40 C41 C55 165.4(2) . . . . ? C39 C40 C41 C55 19.4(3) . . . . ? C40 C41 C42 C23 -2.2(4) . . . . ? C55 C41 C42 C23 -158.4(3) . . . . ? C40 C41 C42 C43 151.5(3) . . . . ? C55 C41 C42 C43 -4.8(5) . . . . ? C22 C23 C42 C41 -0.7(4) . . . . ? C24 C23 C42 C41 148.4(2) . . . . ? C22 C23 C42 C43 -159.9(2) . . . . ? C24 C23 C42 C43 -10.8(3) . . . . ? C41 C42 C43 O1 32.2(4) . . . . ? C23 C42 C43 O1 -171.6(2) . . . . ? C41 C42 C43 C44 -141.9(3) . . . . ? C23 C42 C43 C44 14.3(3) . . . . ? C25 C24 C44 C45 4.9(4) . . . . ? C23 C24 C44 C45 -142.8(2) . . . . ? C25 C24 C44 C43 154.5(2) . . . . ? C23 C24 C44 C43 6.7(3) . . . . ? O1 C43 C44 C45 -39.9(4) . . . . ? C42 C43 C44 C45 134.2(3) . . . . ? O1 C43 C44 C24 173.0(2) . . . . ? C42 C43 C44 C24 -12.9(3) . . . . ? C24 C44 C45 C27 3.4(4) . . . . ? C43 C44 C45 C27 -140.0(3) . . . . ? C24 C44 C45 C46 147.3(3) . . . . ? C43 C44 C45 C46 3.8(4) . . . . ? C26 C27 C45 C44 -8.6(4) . . . . ? C28 C27 C45 C44 136.4(3) . . . . ? C26 C27 C45 C46 -158.6(2) . . . . ? C28 C27 C45 C46 -13.6(3) . . . . ? C44 C45 C46 O2 54.7(4) . . . . ? C27 C45 C46 O2 -157.9(3) . . . . ? C44 C45 C46 C47 -125.8(3) . . . . ? C27 C45 C46 C47 21.6(3) . . . . ? C29 C28 C47 C48 8.2(4) . . . . ? C27 C28 C47 C48 -137.5(3) . . . . ? C29 C28 C47 C46 160.3(3) . . . . ? C27 C28 C47 C46 14.5(3) . . . . ? O2 C46 C47 C48 -52.6(5) . . . . ? C45 C46 C47 C48 127.9(3) . . . . ? O2 C46 C47 C28 157.6(3) . . . . ? C45 C46 C47 C28 -21.9(3) . . . . ? C28 C47 C48 C31 -4.6(4) . . . . ? C46 C47 C48 C31 -150.9(3) . . . . ? C28 C47 C48 C49 140.5(3) . . . . ? C46 C47 C48 C49 -5.8(5) . . . . ? C30 C31 C48 C47 -2.6(4) . . . . ? C32 C31 C48 C47 144.8(3) . . . . ? C30 C31 C48 C49 -153.3(3) . . . . ? C32 C31 C48 C49 -5.9(3) . . . . ? C47 C48 C49 O3 35.3(5) . . . . ? C31 C48 C49 O3 -176.6(3) . . . . ? C47 C48 C49 C50 -136.5(3) . . . . ? C31 C48 C49 C50 11.6(3) . . . . ? C33 C32 C50 C51 1.1(4) . . . . ? C31 C32 C50 C51 -146.7(3) . . . . ? C33 C32 C50 C49 157.7(2) . . . . ? C31 C32 C50 C49 9.9(3) . . . . ? O3 C49 C50 C51 -30.9(5) . . . . ? C48 C49 C50 C51 140.7(3) . . . . ? O3 C49 C50 C32 175.4(3) . . . . ? C48 C49 C50 C32 -13.0(3) . . . . ? C32 C50 C51 C35 1.6(4) . . . . ? C49 C50 C51 C35 -149.3(3) . . . . ? C32 C50 C51 C52 160.4(3) . . . . ? C49 C50 C51 C52 9.5(5) . . . . ? C34 C35 C51 C50 -2.5(4) . . . . ? C36 C35 C51 C50 143.6(3) . . . . ? C34 C35 C51 C52 -166.5(2) . . . . ? C36 C35 C51 C52 -20.5(3) . . . . ? C50 C51 C52 O4 113.6(3) . . . . ? C35 C51 C52 O4 -85.6(2) . . . . ? C50 C51 C52 C59 -14.5(4) . . . . ? C35 C51 C52 C59 146.3(2) . . . . ? C50 C51 C52 C53 -133.0(3) . . . . ? C35 C51 C52 C53 27.7(2) . . . . ? C37 C36 C53 C54 7.3(4) . . . . ? C35 C36 C53 C54 -137.4(3) . . . . ? C37 C36 C53 C52 160.4(2) . . . . ? C35 C36 C53 C52 15.7(3) . . . . ? O4 C52 C53 C54 -121.4(3) . . . . ? C59 C52 C53 C54 -4.2(4) . . . . ? C51 C52 C53 C54 124.6(3) . . . . ? O4 C52 C53 C36 87.5(3) . . . . ? C59 C52 C53 C36 -155.3(2) . . . . ? C51 C52 C53 C36 -26.4(2) . . . . ? C36 C53 C54 C39 -1.2(4) . . . . ? C52 C53 C54 C39 -149.7(3) . . . . ? C36 C53 C54 C55 149.8(3) . . . . ? C52 C53 C54 C55 1.3(4) . . . . ? C38 C39 C54 C53 -5.6(4) . . . . ? C40 C39 C54 C53 139.5(3) . . . . ? C38 C39 C54 C55 -160.9(2) . . . . ? C40 C39 C54 C55 -15.7(3) . . . . ? O6 O5 C55 C56 65.8(2) . . . . ? O6 O5 C55 C54 -55.2(2) . . . . ? O6 O5 C55 C41 -161.44(18) . . . . ? C53 C54 C55 O5 123.7(3) . . . . ? C39 C54 C55 O5 -82.7(3) . . . . ? C53 C54 C55 C56 2.4(4) . . . . ? C39 C54 C55 C56 156.0(2) . . . . ? C53 C54 C55 C41 -127.8(3) . . . . ? C39 C54 C55 C41 25.9(3) . . . . ? C42 C41 C55 O5 -113.4(3) . . . . ? C40 C41 C55 O5 88.3(2) . . . . ? C42 C41 C55 C56 11.0(4) . . . . ? C40 C41 C55 C56 -147.2(2) . . . . ? C42 C41 C55 C54 131.4(3) . . . . ? C40 C41 C55 C54 -26.8(3) . . . . ? O5 C55 C56 C59 -125.3(3) . . . . ? C54 C55 C56 C59 -2.8(4) . . . . ? C41 C55 C56 C59 113.1(3) . . . . ? O5 C55 C56 C57 35.1(3) . . . . ? C54 C55 C56 C57 157.6(2) . . . . ? C41 C55 C56 C57 -86.5(3) . . . . ? C58 O8 C57 O7 -168.1(2) . . . . ? C58 O8 C57 C56 8.6(3) . . . . ? C59 C56 C57 O7 170.3(3) . . . . ? C55 C56 C57 O7 7.0(5) . . . . ? C59 C56 C57 O8 -5.9(3) . . . . ? C55 C56 C57 O8 -169.2(2) . . . . ? C60 N1 C58 O8 3.9(5) . . . . ? C60 N1 C58 C59 177.8(3) . . . . ? C57 O8 C58 N1 166.8(3) . . . . ? C57 O8 C58 C59 -8.1(3) . . . . ? C57 C56 C59 C58 1.0(3) . . . . ? C55 C56 C59 C58 164.0(2) . . . . ? C57 C56 C59 C52 -163.5(2) . . . . ? C55 C56 C59 C52 -0.4(4) . . . . ? N1 C58 C59 C56 -170.6(3) . . . . ? O8 C58 C59 C56 4.3(3) . . . . ? N1 C58 C59 C52 -5.3(4) . . . . ? O8 C58 C59 C52 169.6(2) . . . . ? O4 C52 C59 C56 121.1(3) . . . . ? C53 C52 C59 C56 3.9(4) . . . . ? C51 C52 C59 C56 -110.4(3) . . . . ? O4 C52 C59 C58 -41.4(4) . . . . ? C53 C52 C59 C58 -158.7(2) . . . . ? C51 C52 C59 C58 87.1(3) . . . . ? C58 N1 C60 C65 -157.3(3) . . . . ? C58 N1 C60 C61 24.4(4) . . . . ? C65 C60 C61 C62 2.4(4) . . . . ? N1 C60 C61 C62 -179.3(3) . . . . ? C60 C61 C62 C63 0.2(4) . . . . ? C61 C62 C63 C64 -2.5(5) . . . . ? C62 C63 C64 C65 2.1(5) . . . . ? C61 C60 C65 C64 -2.8(4) . . . . ? N1 C60 C65 C64 178.9(3) . . . . ? C63 C64 C65 C60 0.5(4) . . . . ? C66' O6 C66 C68 72.4(14) . . . . ? O5 O6 C66 C68 -43.1(4) . . . . ? C66' O6 C66 C69 -48.9(13) . . . . ? O5 O6 C66 C69 -164.4(4) . . . . ? C66' O6 C66 C67 -163.7(16) . . . . ? O5 O6 C66 C67 80.8(4) . . . . ? C66 O6 C66' C67' -14.5(10) . . . . ? O5 O6 C66' C67' 58.0(7) . . . . ? C66 O6 C66' C69' 106.8(15) . . . . ? O5 O6 C66' C69' 179.2(5) . . . . ? C66 O6 C66' C68' -135.9(17) . . . . ? O5 O6 C66' C68' -63.4(6) . . . . ? 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 0.000 0.500 1.000 227 104 ' ' 2 0.264 0.679 0.287 25 1 ' ' 3 0.736 0.321 0.713 25 1 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.274 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.070 data_c _database_code_depnum_ccdc_archive 'CCDC 905500' #TrackingRef '14608_web_deposit_cif_file_2_Gan,Liangbing_1349923400.12a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C65 H5 N O5' _chemical_formula_sum 'C65 H5 N O5' _chemical_formula_weight 879.70 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 monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 18.742(4) _cell_length_b 13.442(3) _cell_length_c 18.553(4) _cell_angle_alpha 90.00 _cell_angle_beta 114.400(3) _cell_angle_gamma 90.00 _cell_volume 4256.6(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 13510 _cell_measurement_theta_min 1.19 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.373 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_absorpt_coefficient_mu 0.088 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9827 _exptl_absorpt_correction_T_max 0.9922 _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 'rotating anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'MM007-HF CCD(Saturn 724+)' _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 30994 _diffrn_reflns_av_R_equivalents 0.0512 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 27.47 _reflns_number_total 9714 _reflns_number_gt 7523 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Olex2 Ver 1.1' _computing_publication_material 'SHELX97 (Sheldrick, 2008)' _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^)+(0.0793P)^2^+1.5604P] 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 9714 _refine_ls_number_parameters 640 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0789 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1607 _refine_ls_wR_factor_gt 0.1519 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.46489(8) 0.39054(11) -0.02807(8) 0.0247(3) Uani 1 1 d . . . O2 O 0.52572(8) 0.42538(12) 0.13980(9) 0.0301(4) Uani 1 1 d . . . O3 O 0.47740(9) 0.21628(12) 0.15234(9) 0.0324(4) Uani 1 1 d . . . O4 O 0.51794(9) 0.25122(11) -0.10808(8) 0.0280(3) Uani 1 1 d . . . O5 O 0.51909(9) 0.04847(11) 0.08787(9) 0.0300(3) Uani 1 1 d . . . N1 N 0.53939(10) 0.16693(13) 0.00719(10) 0.0227(4) Uani 1 1 d . . . C1 C 0.49340(12) 0.21430(15) -0.06389(12) 0.0230(4) Uani 1 1 d . . . C2 C 0.41060(12) 0.19977(15) -0.07457(11) 0.0227(4) Uani 1 1 d . . . C3 C 0.41111(12) 0.13711(15) -0.01298(12) 0.0226(4) Uani 1 1 d . . . C4 C 0.49406(12) 0.11111(15) 0.03694(12) 0.0240(4) Uani 1 1 d . . . C5 C 0.33928(12) 0.23680(16) -0.13110(11) 0.0226(4) Uani 1 1 d . . . C6 C 0.30771(12) 0.33768(16) -0.16448(10) 0.0226(4) Uani 1 1 d . . . C7 C 0.33646(11) 0.42888(15) -0.13079(11) 0.0217(4) Uani 1 1 d . . . C8 C 0.40830(11) 0.44405(15) -0.05506(11) 0.0207(4) Uani 1 1 d . . . C9 C 0.38759(11) 0.52598(14) -0.01093(12) 0.0222(4) Uani 1 1 d . . . C10 C 0.40811(11) 0.52681(15) 0.06909(11) 0.0222(4) Uani 1 1 d . . . C11 C 0.46102(12) 0.45216(15) 0.12965(11) 0.0232(4) Uani 1 1 d . . . C12 C 0.41140(12) 0.42124(16) 0.17309(11) 0.0235(4) Uani 1 1 d . . . C13 C 0.39335(12) 0.32586(16) 0.18684(11) 0.0242(4) Uani 1 1 d . . . C14 C 0.41667(12) 0.23184(16) 0.15735(11) 0.0246(4) Uani 1 1 d . . . C15 C 0.34318(12) 0.16786(15) 0.12692(11) 0.0222(4) Uani 1 1 d . . . C16 C 0.31333(12) 0.11222(14) 0.05765(12) 0.0235(4) Uani 1 1 d . . . C17 C 0.34213(12) 0.11106(14) -0.00660(12) 0.0228(4) Uani 1 1 d . . . C18 C 0.27417(12) 0.11812(15) -0.07855(12) 0.0242(4) Uani 1 1 d . . . C19 C 0.27278(12) 0.17910(15) -0.13943(11) 0.0246(4) Uani 1 1 d . . . C20 C 0.20140(12) 0.23045(17) -0.18865(11) 0.0276(5) Uani 1 1 d . . . C21 C 0.13279(12) 0.21303(18) -0.17880(12) 0.0289(5) Uani 1 1 d . . . C22 C 0.13459(12) 0.14781(16) -0.11558(13) 0.0287(5) Uani 1 1 d . . . C23 C 0.08294(12) 0.19027(16) -0.08309(13) 0.0281(5) Uani 1 1 d . . . C24 C 0.10355(12) 0.18547(16) -0.00252(13) 0.0278(5) Uani 1 1 d . . . C25 C 0.17767(12) 0.14021(16) 0.04939(13) 0.0261(4) Uani 1 1 d . . . C26 C 0.22786(12) 0.10082(15) 0.01849(13) 0.0253(4) Uani 1 1 d . . . C27 C 0.20409(12) 0.10444(15) -0.06565(12) 0.0256(4) Uani 1 1 d . . . C28 C 0.20942(13) 0.19707(16) 0.12102(12) 0.0261(4) Uani 1 1 d . . . C29 C 0.15656(12) 0.27682(17) 0.11558(12) 0.0275(5) Uani 1 1 d . . . C30 C 0.09111(12) 0.27004(17) 0.03880(13) 0.0275(5) Uani 1 1 d . . . C31 C 0.18523(13) 0.36906(17) 0.14823(12) 0.0276(5) Uani 1 1 d . . . C32 C 0.15073(13) 0.45968(17) 0.10523(13) 0.0286(5) Uani 1 1 d . . . C33 C 0.21355(13) 0.53040(17) 0.11941(13) 0.0291(5) Uani 1 1 d . . . C34 C 0.21206(12) 0.59132(15) 0.05895(13) 0.0264(4) Uani 1 1 d . . . C35 C 0.14786(12) 0.58519(16) -0.01910(13) 0.0283(5) Uani 1 1 d . . . C36 C 0.08754(12) 0.51740(17) -0.03243(13) 0.0301(5) Uani 1 1 d . . . C37 C 0.08905(12) 0.45400(17) 0.03073(13) 0.0289(5) Uani 1 1 d . . . C38 C 0.05816(11) 0.35711(17) -0.00258(13) 0.0282(5) Uani 1 1 d . . . C39 C 0.03759(11) 0.36285(18) -0.08767(12) 0.0280(5) Uani 1 1 d . . . C40 C 0.04953(11) 0.28091(17) -0.12644(12) 0.0286(5) Uani 1 1 d . . . C41 C 0.08140(12) 0.29462(18) -0.18516(12) 0.0292(5) Uani 1 1 d . . . C42 C 0.10007(12) 0.38849(18) -0.20232(12) 0.0294(5) Uani 1 1 d . . . C43 C 0.08702(12) 0.47481(18) -0.16192(12) 0.0303(5) Uani 1 1 d . . . C44 C 0.05557(12) 0.46150(17) -0.10586(13) 0.0289(5) Uani 1 1 d . . . C45 C 0.15011(12) 0.54342(17) -0.14699(13) 0.0284(5) Uani 1 1 d . . . C46 C 0.20236(12) 0.50004(17) -0.17783(12) 0.0283(5) Uani 1 1 d . . . C47 C 0.17136(12) 0.40558(17) -0.21223(11) 0.0265(5) Uani 1 1 d . . . C48 C 0.22228(12) 0.32702(17) -0.20480(11) 0.0261(5) Uani 1 1 d . . . C49 C 0.28326(11) 0.50980(16) -0.13608(12) 0.0241(4) Uani 1 1 d . . . C50 C 0.31394(12) 0.56666(15) -0.06376(12) 0.0234(4) Uani 1 1 d . . . C51 C 0.26354(12) 0.61103(15) -0.03541(14) 0.0276(5) Uani 1 1 d . . . C52 C 0.18009(12) 0.59834(16) -0.07748(13) 0.0277(5) Uani 1 1 d . . . C53 C 0.28362(13) 0.60754(15) 0.04772(13) 0.0273(5) Uani 1 1 d . . . C54 C 0.35317(12) 0.56270(15) 0.09773(12) 0.0254(4) Uani 1 1 d . . . C55 C 0.35470(12) 0.49884(16) 0.16137(12) 0.0259(4) Uani 1 1 d . . . C56 C 0.28673(13) 0.48269(16) 0.17154(12) 0.0269(5) Uani 1 1 d . . . C57 C 0.26880(13) 0.38364(17) 0.18857(11) 0.0272(5) Uani 1 1 d . . . C58 C 0.32025(12) 0.30720(16) 0.19190(11) 0.0240(4) Uani 1 1 d . . . C59 C 0.29030(12) 0.21256(16) 0.15636(11) 0.0246(4) Uani 1 1 d . . . C60 C 0.62348(11) 0.16706(15) 0.04386(12) 0.0231(4) Uani 1 1 d . . . C61 C 0.66627(13) 0.13833(16) 0.00260(13) 0.0273(5) Uani 1 1 d . . . H61 H 0.6409 0.1183 -0.0512 0.033 Uiso 1 1 calc R . . C62 C 0.74756(13) 0.13917(16) 0.04133(14) 0.0290(5) Uani 1 1 d . . . H62 H 0.7782 0.1205 0.0136 0.035 Uiso 1 1 calc R . . C63 C 0.78416(13) 0.16698(17) 0.11998(14) 0.0329(5) Uani 1 1 d . . . H63 H 0.8397 0.1655 0.1466 0.039 Uiso 1 1 calc R . . C64 C 0.74001(13) 0.19680(18) 0.15959(13) 0.0319(5) Uani 1 1 d . . . H64 H 0.7653 0.2167 0.2134 0.038 Uiso 1 1 calc R . . C65 C 0.65941(13) 0.19815(17) 0.12194(12) 0.0295(5) Uani 1 1 d . . . H65 H 0.6290 0.2200 0.1491 0.035 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 O1 0.0189(7) 0.0284(8) 0.0260(7) 0.0004(6) 0.0086(6) 0.0000(6) O2 0.0195(7) 0.0404(9) 0.0280(8) 0.0018(7) 0.0074(6) 0.0035(6) O3 0.0239(8) 0.0382(9) 0.0349(8) -0.0060(7) 0.0118(7) -0.0006(7) O4 0.0287(8) 0.0329(8) 0.0264(7) 0.0021(6) 0.0155(7) 0.0025(6) O5 0.0296(8) 0.0276(8) 0.0328(8) 0.0090(7) 0.0130(7) 0.0072(6) N1 0.0205(8) 0.0244(9) 0.0238(8) 0.0013(7) 0.0097(7) 0.0032(7) C1 0.0247(10) 0.0221(10) 0.0231(9) -0.0004(8) 0.0107(8) 0.0049(8) C2 0.0253(10) 0.0224(10) 0.0212(9) -0.0054(8) 0.0106(8) 0.0003(8) C3 0.0241(10) 0.0191(9) 0.0248(9) -0.0027(8) 0.0102(8) 0.0016(8) C4 0.0229(10) 0.0226(10) 0.0272(10) -0.0015(8) 0.0110(9) 0.0027(8) C5 0.0242(10) 0.0286(11) 0.0151(8) -0.0033(8) 0.0083(8) -0.0014(8) C6 0.0212(10) 0.0334(11) 0.0115(8) 0.0021(8) 0.0050(7) 0.0000(8) C7 0.0163(9) 0.0271(10) 0.0204(9) 0.0034(8) 0.0062(8) -0.0004(8) C8 0.0151(9) 0.0234(10) 0.0235(9) 0.0063(8) 0.0080(8) -0.0006(7) C9 0.0202(10) 0.0179(9) 0.0285(10) 0.0030(8) 0.0102(8) -0.0030(7) C10 0.0187(9) 0.0229(10) 0.0240(9) -0.0051(8) 0.0079(8) -0.0063(8) C11 0.0223(10) 0.0243(10) 0.0187(9) -0.0067(8) 0.0041(8) -0.0034(8) C12 0.0235(10) 0.0318(11) 0.0147(8) -0.0047(8) 0.0073(8) -0.0031(8) C13 0.0202(10) 0.0346(12) 0.0137(8) -0.0012(8) 0.0029(8) -0.0008(8) C14 0.0213(10) 0.0335(11) 0.0162(9) 0.0047(8) 0.0049(8) 0.0036(8) C15 0.0238(10) 0.0225(10) 0.0191(9) 0.0082(8) 0.0077(8) 0.0038(8) C16 0.0233(10) 0.0180(10) 0.0297(10) 0.0060(8) 0.0113(9) -0.0016(8) C17 0.0246(10) 0.0154(9) 0.0276(10) -0.0023(8) 0.0099(9) 0.0005(7) C18 0.0243(10) 0.0178(10) 0.0302(10) -0.0062(8) 0.0111(9) -0.0049(8) C19 0.0247(10) 0.0264(11) 0.0197(9) -0.0112(8) 0.0060(8) -0.0029(8) C20 0.0258(11) 0.0382(12) 0.0154(9) -0.0089(9) 0.0050(8) -0.0058(9) C21 0.0185(10) 0.0413(13) 0.0203(9) -0.0102(9) 0.0016(8) -0.0068(9) C22 0.0221(10) 0.0306(11) 0.0301(10) -0.0075(9) 0.0075(9) -0.0116(9) C23 0.0162(10) 0.0315(12) 0.0326(11) -0.0021(9) 0.0060(9) -0.0092(8) C24 0.0190(10) 0.0312(12) 0.0340(11) -0.0002(9) 0.0117(9) -0.0088(8) C25 0.0230(10) 0.0242(10) 0.0325(11) 0.0046(9) 0.0128(9) -0.0069(8) C26 0.0248(10) 0.0193(10) 0.0316(11) -0.0005(8) 0.0115(9) -0.0056(8) C27 0.0251(11) 0.0194(10) 0.0305(10) -0.0048(8) 0.0098(9) -0.0066(8) C28 0.0286(11) 0.0284(11) 0.0244(10) 0.0064(8) 0.0141(9) -0.0001(9) C29 0.0240(10) 0.0388(12) 0.0262(10) 0.0046(9) 0.0168(9) -0.0011(9) C30 0.0208(10) 0.0359(12) 0.0308(11) 0.0001(9) 0.0157(9) -0.0037(9) C31 0.0284(11) 0.0368(12) 0.0225(10) -0.0013(9) 0.0154(9) -0.0017(9) C32 0.0268(11) 0.0325(12) 0.0327(11) -0.0052(9) 0.0186(9) -0.0002(9) C33 0.0254(11) 0.0348(12) 0.0299(11) -0.0097(9) 0.0143(9) 0.0020(9) C34 0.0235(10) 0.0224(10) 0.0349(11) -0.0048(9) 0.0136(9) 0.0041(8) C35 0.0254(11) 0.0237(11) 0.0375(12) 0.0040(9) 0.0146(10) 0.0064(8) C36 0.0192(10) 0.0356(12) 0.0354(11) 0.0020(10) 0.0112(9) 0.0088(9) C37 0.0174(10) 0.0355(12) 0.0367(12) -0.0012(10) 0.0140(9) 0.0051(8) C38 0.0137(9) 0.0390(12) 0.0343(11) 0.0021(10) 0.0124(9) 0.0014(8) C39 0.0128(9) 0.0404(13) 0.0276(10) 0.0031(9) 0.0051(8) 0.0006(8) C40 0.0128(9) 0.0401(13) 0.0264(10) -0.0022(9) 0.0017(8) -0.0058(8) C41 0.0156(10) 0.0441(13) 0.0198(9) -0.0024(9) -0.0007(8) -0.0046(9) C42 0.0168(10) 0.0434(13) 0.0194(9) 0.0033(9) -0.0013(8) -0.0010(9) C43 0.0164(10) 0.0414(13) 0.0265(10) 0.0122(10) 0.0023(8) 0.0084(9) C44 0.0167(10) 0.0368(12) 0.0308(11) 0.0040(9) 0.0073(9) 0.0054(8) C45 0.0197(10) 0.0316(12) 0.0305(11) 0.0157(9) 0.0069(9) 0.0098(8) C46 0.0237(11) 0.0371(12) 0.0205(9) 0.0135(9) 0.0056(8) 0.0016(9) C47 0.0181(10) 0.0433(13) 0.0129(8) 0.0076(9) 0.0012(7) 0.0017(9) C48 0.0209(10) 0.0395(12) 0.0132(8) 0.0006(8) 0.0023(8) -0.0028(9) C49 0.0187(10) 0.0298(11) 0.0230(9) 0.0136(8) 0.0079(8) 0.0024(8) C50 0.0215(10) 0.0197(10) 0.0281(10) 0.0087(8) 0.0093(8) -0.0006(8) C51 0.0226(10) 0.0170(10) 0.0419(12) 0.0057(9) 0.0121(9) 0.0014(8) C52 0.0225(10) 0.0224(10) 0.0372(11) 0.0082(9) 0.0112(9) 0.0067(8) C53 0.0263(11) 0.0172(10) 0.0393(12) -0.0043(9) 0.0146(10) 0.0002(8) C54 0.0244(10) 0.0216(10) 0.0286(10) -0.0072(8) 0.0093(9) -0.0034(8) C55 0.0254(11) 0.0277(11) 0.0223(9) -0.0112(8) 0.0075(8) -0.0029(8) C56 0.0313(11) 0.0288(11) 0.0231(10) -0.0073(9) 0.0139(9) -0.0004(9) C57 0.0280(11) 0.0386(13) 0.0169(9) -0.0016(9) 0.0111(8) 0.0013(9) C58 0.0242(10) 0.0343(12) 0.0135(8) 0.0042(8) 0.0078(8) 0.0001(8) C59 0.0265(11) 0.0307(11) 0.0161(8) 0.0051(8) 0.0083(8) -0.0018(9) C60 0.0186(10) 0.0215(10) 0.0290(10) 0.0012(8) 0.0096(8) 0.0030(8) C61 0.0301(11) 0.0230(10) 0.0301(10) 0.0016(9) 0.0136(9) 0.0036(9) C62 0.0257(11) 0.0227(10) 0.0426(12) 0.0018(9) 0.0182(10) 0.0038(8) C63 0.0238(11) 0.0317(12) 0.0377(12) 0.0133(10) 0.0073(10) 0.0035(9) C64 0.0248(11) 0.0425(13) 0.0226(10) 0.0059(9) 0.0038(9) -0.0019(9) C65 0.0289(11) 0.0376(12) 0.0235(10) 0.0023(9) 0.0122(9) 0.0015(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C8 1.206(2) . ? O2 C11 1.203(2) . ? O3 C14 1.198(2) . ? O4 C1 1.201(2) . ? O5 C4 1.207(2) . ? N1 C1 1.396(3) . ? N1 C4 1.406(3) . ? N1 C60 1.436(2) . ? C1 C2 1.494(3) . ? C2 C5 1.406(3) . ? C2 C3 1.416(3) . ? C3 C17 1.391(3) . ? C3 C4 1.486(3) . ? C5 C19 1.421(3) . ? C5 C6 1.507(3) . ? C6 C7 1.380(3) . ? C6 C48 1.468(3) . ? C7 C49 1.451(3) . ? C7 C8 1.505(3) . ? C8 C9 1.515(3) . ? C9 C10 1.371(3) . ? C9 C50 1.431(3) . ? C10 C54 1.424(3) . ? C10 C11 1.527(3) . ? C11 C12 1.519(3) . ? C12 C13 1.376(3) . ? C12 C55 1.440(3) . ? C13 C58 1.434(3) . ? C13 C14 1.512(3) . ? C14 C15 1.521(3) . ? C15 C16 1.389(3) . ? C15 C59 1.445(3) . ? C16 C26 1.468(3) . ? C16 C17 1.498(3) . ? C17 C18 1.417(3) . ? C18 C19 1.387(3) . ? C18 C27 1.441(3) . ? C19 C20 1.446(3) . ? C20 C21 1.391(3) . ? C20 C48 1.423(3) . ? C21 C41 1.432(3) . ? C21 C22 1.454(3) . ? C22 C27 1.378(3) . ? C22 C23 1.452(3) . ? C23 C24 1.382(3) . ? C23 C40 1.452(3) . ? C24 C30 1.443(3) . ? C24 C25 1.457(3) . ? C25 C26 1.393(3) . ? C25 C28 1.432(3) . ? C26 C27 1.436(3) . ? C28 C59 1.396(3) . ? C28 C29 1.435(3) . ? C29 C31 1.387(3) . ? C29 C30 1.449(3) . ? C30 C38 1.396(3) . ? C31 C57 1.443(3) . ? C31 C32 1.453(3) . ? C32 C37 1.390(3) . ? C32 C33 1.450(3) . ? C33 C34 1.380(3) . ? C33 C56 1.460(3) . ? C34 C35 1.453(3) . ? C34 C53 1.456(3) . ? C35 C36 1.393(3) . ? C35 C52 1.452(3) . ? C36 C37 1.440(3) . ? C36 C44 1.451(3) . ? C37 C38 1.455(3) . ? C38 C39 1.464(3) . ? C39 C40 1.383(3) . ? C39 C44 1.442(3) . ? C40 C41 1.454(3) . ? C41 C42 1.381(3) . ? C42 C47 1.440(3) . ? C42 C43 1.456(3) . ? C43 C44 1.403(3) . ? C43 C45 1.433(3) . ? C45 C52 1.388(3) . ? C45 C46 1.445(3) . ? C46 C49 1.395(3) . ? C46 C47 1.432(3) . ? C47 C48 1.391(3) . ? C49 C50 1.442(3) . ? C50 C51 1.391(3) . ? C51 C53 1.429(3) . ? C51 C52 1.441(3) . ? C53 C54 1.387(3) . ? C54 C55 1.450(3) . ? C55 C56 1.380(3) . ? C56 C57 1.440(3) . ? C57 C58 1.393(3) . ? C58 C59 1.436(3) . ? C60 C61 1.373(3) . ? C60 C65 1.386(3) . ? C61 C62 1.390(3) . ? C61 H61 0.9500 . ? C62 C63 1.383(3) . ? C62 H62 0.9500 . ? C63 C64 1.374(3) . ? C63 H63 0.9500 . ? C64 C65 1.378(3) . ? C64 H64 0.9500 . ? C65 H65 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C4 112.14(17) . . ? C1 N1 C60 125.15(17) . . ? C4 N1 C60 122.54(16) . . ? O4 C1 N1 124.93(19) . . ? O4 C1 C2 129.30(18) . . ? N1 C1 C2 105.54(17) . . ? C5 C2 C3 120.00(19) . . ? C5 C2 C1 131.92(19) . . ? C3 C2 C1 108.08(17) . . ? C17 C3 C2 121.44(18) . . ? C17 C3 C4 131.14(19) . . ? C2 C3 C4 107.42(17) . . ? O5 C4 N1 125.26(19) . . ? O5 C4 C3 128.35(19) . . ? N1 C4 C3 106.04(17) . . ? C2 C5 C19 114.12(19) . . ? C2 C5 C6 135.76(18) . . ? C19 C5 C6 105.58(17) . . ? C7 C6 C48 117.20(18) . . ? C7 C6 C5 126.84(17) . . ? C48 C6 C5 106.39(17) . . ? C6 C7 C49 120.42(18) . . ? C6 C7 C8 125.05(18) . . ? C49 C7 C8 106.64(17) . . ? O1 C8 C7 126.95(19) . . ? O1 C8 C9 125.92(18) . . ? C7 C8 C9 105.83(16) . . ? C10 C9 C50 119.88(19) . . ? C10 C9 C8 124.83(18) . . ? C50 C9 C8 107.31(17) . . ? C9 C10 C54 118.96(19) . . ? C9 C10 C11 126.69(18) . . ? C54 C10 C11 107.34(17) . . ? O2 C11 C12 129.33(19) . . ? O2 C11 C10 128.17(19) . . ? C12 C11 C10 102.49(16) . . ? C13 C12 C55 118.70(19) . . ? C13 C12 C11 127.19(19) . . ? C55 C12 C11 107.28(18) . . ? C12 C13 C58 119.33(19) . . ? C12 C13 C14 125.57(19) . . ? C58 C13 C14 107.73(18) . . ? O3 C14 C13 126.9(2) . . ? O3 C14 C15 128.0(2) . . ? C13 C14 C15 104.74(17) . . ? C16 C15 C59 119.77(18) . . ? C16 C15 C14 127.22(18) . . ? C59 C15 C14 106.36(17) . . ? C15 C16 C26 117.00(18) . . ? C15 C16 C17 127.01(18) . . ? C26 C16 C17 106.46(17) . . ? C3 C17 C18 114.10(19) . . ? C3 C17 C16 135.91(18) . . ? C18 C17 C16 105.65(18) . . ? C19 C18 C17 120.91(19) . . ? C19 C18 C27 119.93(19) . . ? C17 C18 C27 111.18(19) . . ? C18 C19 C5 120.89(18) . . ? C18 C19 C20 119.85(19) . . ? C5 C19 C20 110.43(19) . . ? C21 C20 C48 122.0(2) . . ? C21 C20 C19 120.1(2) . . ? C48 C20 C19 107.78(18) . . ? C20 C21 C41 119.1(2) . . ? C20 C21 C22 119.5(2) . . ? C41 C21 C22 108.60(19) . . ? C27 C22 C23 119.6(2) . . ? C27 C22 C21 119.88(19) . . ? C23 C22 C21 107.50(19) . . ? C24 C23 C40 120.1(2) . . ? C24 C23 C22 119.6(2) . . ? C40 C23 C22 107.99(19) . . ? C23 C24 C30 120.2(2) . . ? C23 C24 C25 119.9(2) . . ? C30 C24 C25 107.28(18) . . ? C26 C25 C28 119.51(19) . . ? C26 C25 C24 120.55(19) . . ? C28 C25 C24 107.92(19) . . ? C25 C26 C27 118.40(19) . . ? C25 C26 C16 122.75(19) . . ? C27 C26 C16 108.63(18) . . ? C22 C27 C26 121.9(2) . . ? C22 C27 C18 120.5(2) . . ? C26 C27 C18 106.86(18) . . ? C59 C28 C25 118.01(19) . . ? C59 C28 C29 120.4(2) . . ? C25 C28 C29 108.87(18) . . ? C31 C29 C28 120.4(2) . . ? C31 C29 C30 120.2(2) . . ? C28 C29 C30 107.56(19) . . ? C38 C30 C24 120.0(2) . . ? C38 C30 C29 119.4(2) . . ? C24 C30 C29 108.36(19) . . ? C29 C31 C57 119.3(2) . . ? C29 C31 C32 120.34(19) . . ? C57 C31 C32 108.20(19) . . ? C37 C32 C33 119.7(2) . . ? C37 C32 C31 119.9(2) . . ? C33 C32 C31 107.82(19) . . ? C34 C33 C32 120.0(2) . . ? C34 C33 C56 119.82(19) . . ? C32 C33 C56 107.6(2) . . ? C33 C34 C35 120.5(2) . . ? C33 C34 C53 119.65(19) . . ? C35 C34 C53 107.35(19) . . ? C36 C35 C52 120.3(2) . . ? C36 C35 C34 119.4(2) . . ? C52 C35 C34 107.94(19) . . ? C35 C36 C37 120.1(2) . . ? C35 C36 C44 119.7(2) . . ? C37 C36 C44 108.6(2) . . ? C32 C37 C36 120.4(2) . . ? C32 C37 C38 119.5(2) . . ? C36 C37 C38 108.27(19) . . ? C30 C38 C37 120.59(19) . . ? C30 C38 C39 119.8(2) . . ? C37 C38 C39 106.99(19) . . ? C40 C39 C44 120.5(2) . . ? C40 C39 C38 119.4(2) . . ? C44 C39 C38 108.53(19) . . ? C39 C40 C23 120.37(19) . . ? C39 C40 C41 119.6(2) . . ? C23 C40 C41 107.74(19) . . ? C42 C41 C21 119.5(2) . . ? C42 C41 C40 120.7(2) . . ? C21 C41 C40 108.2(2) . . ? C41 C42 C47 120.8(2) . . ? C41 C42 C43 119.8(2) . . ? C47 C42 C43 107.49(19) . . ? C44 C43 C45 120.3(2) . . ? C44 C43 C42 119.4(2) . . ? C45 C43 C42 108.15(19) . . ? C43 C44 C39 120.1(2) . . ? C43 C44 C36 119.5(2) . . ? C39 C44 C36 107.59(19) . . ? C52 C45 C43 120.4(2) . . ? C52 C45 C46 120.14(19) . . ? C43 C45 C46 107.7(2) . . ? C49 C46 C47 118.6(2) . . ? C49 C46 C45 120.1(2) . . ? C47 C46 C45 108.51(19) . . ? C48 C47 C46 119.56(19) . . ? C48 C47 C42 120.0(2) . . ? C46 C47 C42 108.15(19) . . ? C47 C48 C20 118.4(2) . . ? C47 C48 C6 122.38(19) . . ? C20 C48 C6 108.58(18) . . ? C46 C49 C50 119.39(19) . . ? C46 C49 C7 121.7(2) . . ? C50 C49 C7 109.62(17) . . ? C51 C50 C9 121.24(19) . . ? C51 C50 C49 120.48(19) . . ? C9 C50 C49 109.63(18) . . ? C50 C51 C53 118.47(19) . . ? C50 C51 C52 119.9(2) . . ? C53 C51 C52 108.88(19) . . ? C45 C52 C51 119.90(19) . . ? C45 C52 C35 119.7(2) . . ? C51 C52 C35 107.65(19) . . ? C54 C53 C51 119.46(19) . . ? C54 C53 C34 120.4(2) . . ? C51 C53 C34 108.17(19) . . ? C53 C54 C10 121.5(2) . . ? C53 C54 C55 119.93(19) . . ? C10 C54 C55 109.21(18) . . ? C56 C55 C12 122.1(2) . . ? C56 C55 C54 119.69(19) . . ? C12 C55 C54 108.48(18) . . ? C55 C56 C57 119.2(2) . . ? C55 C56 C33 120.5(2) . . ? C57 C56 C33 108.12(19) . . ? C58 C57 C56 118.2(2) . . ? C58 C57 C31 120.4(2) . . ? C56 C57 C31 108.26(19) . . ? C57 C58 C13 122.1(2) . . ? C57 C58 C59 120.06(19) . . ? C13 C58 C59 109.13(18) . . ? C28 C59 C58 119.36(19) . . ? C28 C59 C15 122.78(19) . . ? C58 C59 C15 110.05(18) . . ? C61 C60 C65 121.61(19) . . ? C61 C60 N1 121.01(18) . . ? C65 C60 N1 117.38(18) . . ? C60 C61 C62 118.5(2) . . ? C60 C61 H61 120.7 . . ? C62 C61 H61 120.7 . . ? C63 C62 C61 120.5(2) . . ? C63 C62 H62 119.7 . . ? C61 C62 H62 119.7 . . ? C64 C63 C62 119.8(2) . . ? C64 C63 H63 120.1 . . ? C62 C63 H63 120.1 . . ? C63 C64 C65 120.6(2) . . ? C63 C64 H64 119.7 . . ? C65 C64 H64 119.7 . . ? C64 C65 C60 118.9(2) . . ? C64 C65 H65 120.5 . . ? C60 C65 H65 120.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 N1 C1 O4 -166.01(19) . . . . ? C60 N1 C1 O4 9.2(3) . . . . ? C4 N1 C1 C2 8.9(2) . . . . ? C60 N1 C1 C2 -175.90(17) . . . . ? O4 C1 C2 C5 -11.2(4) . . . . ? N1 C1 C2 C5 174.2(2) . . . . ? O4 C1 C2 C3 169.5(2) . . . . ? N1 C1 C2 C3 -5.1(2) . . . . ? C5 C2 C3 C17 -0.2(3) . . . . ? C1 C2 C3 C17 179.15(18) . . . . ? C5 C2 C3 C4 -179.60(17) . . . . ? C1 C2 C3 C4 -0.2(2) . . . . ? C1 N1 C4 O5 164.6(2) . . . . ? C60 N1 C4 O5 -10.7(3) . . . . ? C1 N1 C4 C3 -9.1(2) . . . . ? C60 N1 C4 C3 175.55(17) . . . . ? C17 C3 C4 O5 12.7(4) . . . . ? C2 C3 C4 O5 -168.0(2) . . . . ? C17 C3 C4 N1 -173.9(2) . . . . ? C2 C3 C4 N1 5.4(2) . . . . ? C3 C2 C5 C19 -23.0(3) . . . . ? C1 C2 C5 C19 157.9(2) . . . . ? C3 C2 C5 C6 128.9(2) . . . . ? C1 C2 C5 C6 -50.3(4) . . . . ? C2 C5 C6 C7 -19.6(4) . . . . ? C19 C5 C6 C7 133.8(2) . . . . ? C2 C5 C6 C48 -164.3(2) . . . . ? C19 C5 C6 C48 -10.9(2) . . . . ? C48 C6 C7 C49 -0.3(3) . . . . ? C5 C6 C7 C49 -141.6(2) . . . . ? C48 C6 C7 C8 144.58(19) . . . . ? C5 C6 C7 C8 3.2(3) . . . . ? C6 C7 C8 O1 28.5(3) . . . . ? C49 C7 C8 O1 177.27(19) . . . . ? C6 C7 C8 C9 -139.0(2) . . . . ? C49 C7 C8 C9 9.8(2) . . . . ? O1 C8 C9 C10 -28.4(3) . . . . ? C7 C8 C9 C10 139.28(19) . . . . ? O1 C8 C9 C50 -176.86(19) . . . . ? C7 C8 C9 C50 -9.2(2) . . . . ? C50 C9 C10 C54 4.0(3) . . . . ? C8 C9 C10 C54 -140.9(2) . . . . ? C50 C9 C10 C11 150.80(19) . . . . ? C8 C9 C10 C11 5.9(3) . . . . ? C9 C10 C11 O2 51.9(3) . . . . ? C54 C10 C11 O2 -158.2(2) . . . . ? C9 C10 C11 C12 -128.2(2) . . . . ? C54 C10 C11 C12 21.8(2) . . . . ? O2 C11 C12 C13 -51.7(3) . . . . ? C10 C11 C12 C13 128.4(2) . . . . ? O2 C11 C12 C55 158.1(2) . . . . ? C10 C11 C12 C55 -21.77(19) . . . . ? C55 C12 C13 C58 -2.2(3) . . . . ? C11 C12 C13 C58 -149.42(19) . . . . ? C55 C12 C13 C14 144.01(19) . . . . ? C11 C12 C13 C14 -3.2(3) . . . . ? C12 C13 C14 O3 37.7(3) . . . . ? C58 C13 C14 O3 -172.91(19) . . . . ? C12 C13 C14 C15 -135.8(2) . . . . ? C58 C13 C14 C15 13.6(2) . . . . ? O3 C14 C15 C16 -36.2(3) . . . . ? C13 C14 C15 C16 137.2(2) . . . . ? O3 C14 C15 C59 173.0(2) . . . . ? C13 C14 C15 C59 -13.6(2) . . . . ? C59 C15 C16 C26 -1.0(3) . . . . ? C14 C15 C16 C26 -148.3(2) . . . . ? C59 C15 C16 C17 140.5(2) . . . . ? C14 C15 C16 C17 -6.8(3) . . . . ? C2 C3 C17 C18 23.1(3) . . . . ? C4 C3 C17 C18 -157.7(2) . . . . ? C2 C3 C17 C16 -129.4(2) . . . . ? C4 C3 C17 C16 49.9(4) . . . . ? C15 C16 C17 C3 19.9(4) . . . . ? C26 C16 C17 C3 164.6(2) . . . . ? C15 C16 C17 C18 -134.1(2) . . . . ? C26 C16 C17 C18 10.6(2) . . . . ? C3 C17 C18 C19 -22.7(3) . . . . ? C16 C17 C18 C19 137.75(19) . . . . ? C3 C17 C18 C27 -171.55(17) . . . . ? C16 C17 C18 C27 -11.1(2) . . . . ? C17 C18 C19 C5 -0.5(3) . . . . ? C27 C18 C19 C5 145.7(2) . . . . ? C17 C18 C19 C20 -144.8(2) . . . . ? C27 C18 C19 C20 1.3(3) . . . . ? C2 C5 C19 C18 23.4(3) . . . . ? C6 C5 C19 C18 -136.62(19) . . . . ? C2 C5 C19 C20 170.72(17) . . . . ? C6 C5 C19 C20 10.7(2) . . . . ? C18 C19 C20 C21 -4.8(3) . . . . ? C5 C19 C20 C21 -152.48(19) . . . . ? C18 C19 C20 C48 141.27(19) . . . . ? C5 C19 C20 C48 -6.5(2) . . . . ? C48 C20 C21 C41 0.1(3) . . . . ? C19 C20 C21 C41 141.2(2) . . . . ? C48 C20 C21 C22 -137.3(2) . . . . ? C19 C20 C21 C22 3.8(3) . . . . ? C20 C21 C22 C27 0.5(3) . . . . ? C41 C21 C22 C27 -140.9(2) . . . . ? C20 C21 C22 C23 141.7(2) . . . . ? C41 C21 C22 C23 0.3(2) . . . . ? C27 C22 C23 C24 -0.9(3) . . . . ? C21 C22 C23 C24 -142.2(2) . . . . ? C27 C22 C23 C40 141.5(2) . . . . ? C21 C22 C23 C40 0.2(2) . . . . ? C40 C23 C24 C30 0.8(3) . . . . ? C22 C23 C24 C30 138.6(2) . . . . ? C40 C23 C24 C25 -136.3(2) . . . . ? C22 C23 C24 C25 1.5(3) . . . . ? C23 C24 C25 C26 -0.5(3) . . . . ? C30 C24 C25 C26 -142.5(2) . . . . ? C23 C24 C25 C28 141.8(2) . . . . ? C30 C24 C25 C28 -0.1(2) . . . . ? C28 C25 C26 C27 -139.2(2) . . . . ? C24 C25 C26 C27 -1.1(3) . . . . ? C28 C25 C26 C16 2.0(3) . . . . ? C24 C25 C26 C16 140.1(2) . . . . ? C15 C16 C26 C25 -2.2(3) . . . . ? C17 C16 C26 C25 -150.9(2) . . . . ? C15 C16 C26 C27 142.26(19) . . . . ? C17 C16 C26 C27 -6.5(2) . . . . ? C23 C22 C27 C26 -0.8(3) . . . . ? C21 C22 C27 C26 135.8(2) . . . . ? C23 C22 C27 C18 -140.5(2) . . . . ? C21 C22 C27 C18 -3.9(3) . . . . ? C25 C26 C27 C22 1.7(3) . . . . ? C16 C26 C27 C22 -144.5(2) . . . . ? C25 C26 C27 C18 146.14(19) . . . . ? C16 C26 C27 C18 -0.1(2) . . . . ? C19 C18 C27 C22 3.0(3) . . . . ? C17 C18 C27 C22 152.19(19) . . . . ? C19 C18 C27 C26 -141.97(19) . . . . ? C17 C18 C27 C26 7.2(2) . . . . ? C26 C25 C28 C59 1.4(3) . . . . ? C24 C25 C28 C59 -141.49(19) . . . . ? C26 C25 C28 C29 143.3(2) . . . . ? C24 C25 C28 C29 0.4(2) . . . . ? C59 C28 C29 C31 -2.6(3) . . . . ? C25 C28 C29 C31 -143.50(19) . . . . ? C59 C28 C29 C30 140.27(19) . . . . ? C25 C28 C29 C30 -0.6(2) . . . . ? C23 C24 C30 C38 0.0(3) . . . . ? C25 C24 C30 C38 141.8(2) . . . . ? C23 C24 C30 C29 -142.1(2) . . . . ? C25 C24 C30 C29 -0.3(2) . . . . ? C31 C29 C30 C38 1.2(3) . . . . ? C28 C29 C30 C38 -141.8(2) . . . . ? C31 C29 C30 C24 143.5(2) . . . . ? C28 C29 C30 C24 0.5(2) . . . . ? C28 C29 C31 C57 -0.7(3) . . . . ? C30 C29 C31 C57 -139.0(2) . . . . ? C28 C29 C31 C32 137.3(2) . . . . ? C30 C29 C31 C32 -1.0(3) . . . . ? C29 C31 C32 C37 -0.5(3) . . . . ? C57 C31 C32 C37 141.7(2) . . . . ? C29 C31 C32 C33 -142.2(2) . . . . ? C57 C31 C32 C33 -0.1(2) . . . . ? C37 C32 C33 C34 -0.3(3) . . . . ? C31 C32 C33 C34 141.5(2) . . . . ? C37 C32 C33 C56 -142.0(2) . . . . ? C31 C32 C33 C56 -0.2(2) . . . . ? C32 C33 C34 C35 0.0(3) . . . . ? C56 C33 C34 C35 137.1(2) . . . . ? C32 C33 C34 C53 -137.1(2) . . . . ? C56 C33 C34 C53 0.0(3) . . . . ? C33 C34 C35 C36 0.2(3) . . . . ? C53 C34 C35 C36 141.9(2) . . . . ? C33 C34 C35 C52 -142.1(2) . . . . ? C53 C34 C35 C52 -0.4(2) . . . . ? C52 C35 C36 C37 137.6(2) . . . . ? C34 C35 C36 C37 -0.1(3) . . . . ? C52 C35 C36 C44 -1.5(3) . . . . ? C34 C35 C36 C44 -139.2(2) . . . . ? C33 C32 C37 C36 0.4(3) . . . . ? C31 C32 C37 C36 -136.8(2) . . . . ? C33 C32 C37 C38 139.0(2) . . . . ? C31 C32 C37 C38 1.7(3) . . . . ? C35 C36 C37 C32 -0.3(3) . . . . ? C44 C36 C37 C32 142.9(2) . . . . ? C35 C36 C37 C38 -142.9(2) . . . . ? C44 C36 C37 C38 0.2(2) . . . . ? C24 C30 C38 C37 -137.9(2) . . . . ? C29 C30 C38 C37 0.1(3) . . . . ? C24 C30 C38 C39 -1.1(3) . . . . ? C29 C30 C38 C39 136.9(2) . . . . ? C32 C37 C38 C30 -1.5(3) . . . . ? C36 C37 C38 C30 141.5(2) . . . . ? C32 C37 C38 C39 -143.1(2) . . . . ? C36 C37 C38 C39 -0.1(2) . . . . ? C30 C38 C39 C40 1.4(3) . . . . ? C37 C38 C39 C40 143.4(2) . . . . ? C30 C38 C39 C44 -142.0(2) . . . . ? C37 C38 C39 C44 0.0(2) . . . . ? C44 C39 C40 C23 138.4(2) . . . . ? C38 C39 C40 C23 -0.6(3) . . . . ? C44 C39 C40 C41 0.8(3) . . . . ? C38 C39 C40 C41 -138.2(2) . . . . ? C24 C23 C40 C39 -0.4(3) . . . . ? C22 C23 C40 C39 -142.6(2) . . . . ? C24 C23 C40 C41 141.56(19) . . . . ? C22 C23 C40 C41 -0.6(2) . . . . ? C20 C21 C41 C42 1.2(3) . . . . ? C22 C21 C41 C42 142.72(19) . . . . ? C20 C21 C41 C40 -142.20(19) . . . . ? C22 C21 C41 C40 -0.7(2) . . . . ? C39 C40 C41 C42 0.2(3) . . . . ? C23 C40 C41 C42 -142.11(19) . . . . ? C39 C40 C41 C21 143.10(19) . . . . ? C23 C40 C41 C21 0.8(2) . . . . ? C21 C41 C42 C47 -1.3(3) . . . . ? C40 C41 C42 C47 137.5(2) . . . . ? C21 C41 C42 C43 -139.4(2) . . . . ? C40 C41 C42 C43 -0.6(3) . . . . ? C41 C42 C43 C44 0.0(3) . . . . ? C47 C42 C43 C44 -143.00(19) . . . . ? C41 C42 C43 C45 142.67(19) . . . . ? C47 C42 C43 C45 -0.4(2) . . . . ? C45 C43 C44 C39 -137.1(2) . . . . ? C42 C43 C44 C39 1.0(3) . . . . ? C45 C43 C44 C36 -0.2(3) . . . . ? C42 C43 C44 C36 137.9(2) . . . . ? C40 C39 C44 C43 -1.4(3) . . . . ? C38 C39 C44 C43 141.56(19) . . . . ? C40 C39 C44 C36 -142.81(19) . . . . ? C38 C39 C44 C36 0.2(2) . . . . ? C35 C36 C44 C43 1.4(3) . . . . ? C37 C36 C44 C43 -141.9(2) . . . . ? C35 C36 C44 C39 143.0(2) . . . . ? C37 C36 C44 C39 -0.2(2) . . . . ? C44 C43 C45 C52 -0.8(3) . . . . ? C42 C43 C45 C52 -143.10(19) . . . . ? C44 C43 C45 C46 142.2(2) . . . . ? C42 C43 C45 C46 -0.1(2) . . . . ? C52 C45 C46 C49 2.6(3) . . . . ? C43 C45 C46 C49 -140.50(19) . . . . ? C52 C45 C46 C47 143.65(19) . . . . ? C43 C45 C46 C47 0.5(2) . . . . ? C49 C46 C47 C48 -1.4(3) . . . . ? C45 C46 C47 C48 -143.07(19) . . . . ? C49 C46 C47 C42 140.94(19) . . . . ? C45 C46 C47 C42 -0.7(2) . . . . ? C41 C42 C47 C48 0.2(3) . . . . ? C43 C42 C47 C48 142.79(19) . . . . ? C41 C42 C47 C46 -141.92(19) . . . . ? C43 C42 C47 C46 0.7(2) . . . . ? C46 C47 C48 C20 138.9(2) . . . . ? C42 C47 C48 C20 1.0(3) . . . . ? C46 C47 C48 C6 -1.7(3) . . . . ? C42 C47 C48 C6 -139.6(2) . . . . ? C21 C20 C48 C47 -1.2(3) . . . . ? C19 C20 C48 C47 -146.37(18) . . . . ? C21 C20 C48 C6 144.39(19) . . . . ? C19 C20 C48 C6 -0.8(2) . . . . ? C7 C6 C48 C47 2.5(3) . . . . ? C5 C6 C48 C47 151.14(18) . . . . ? C7 C6 C48 C20 -141.41(19) . . . . ? C5 C6 C48 C20 7.2(2) . . . . ? C47 C46 C49 C50 -139.6(2) . . . . ? C45 C46 C49 C50 -2.4(3) . . . . ? C47 C46 C49 C7 3.7(3) . . . . ? C45 C46 C49 C7 140.9(2) . . . . ? C6 C7 C49 C46 -2.9(3) . . . . ? C8 C7 C49 C46 -153.37(18) . . . . ? C6 C7 C49 C50 143.55(18) . . . . ? C8 C7 C49 C50 -7.0(2) . . . . ? C10 C9 C50 C51 2.6(3) . . . . ? C8 C9 C50 C51 152.95(18) . . . . ? C10 C9 C50 C49 -145.18(19) . . . . ? C8 C9 C50 C49 5.2(2) . . . . ? C46 C49 C50 C51 0.4(3) . . . . ? C7 C49 C50 C51 -146.93(19) . . . . ? C46 C49 C50 C9 148.45(19) . . . . ? C7 C49 C50 C9 1.1(2) . . . . ? C9 C50 C51 C53 -5.4(3) . . . . ? C49 C50 C51 C53 138.9(2) . . . . ? C9 C50 C51 C52 -142.9(2) . . . . ? C49 C50 C51 C52 1.4(3) . . . . ? C43 C45 C52 C51 137.7(2) . . . . ? C46 C45 C52 C51 -0.8(3) . . . . ? C43 C45 C52 C35 0.8(3) . . . . ? C46 C45 C52 C35 -137.7(2) . . . . ? C50 C51 C52 C45 -1.2(3) . . . . ? C53 C51 C52 C45 -142.3(2) . . . . ? C50 C51 C52 C35 140.3(2) . . . . ? C53 C51 C52 C35 -0.9(2) . . . . ? C36 C35 C52 C45 0.4(3) . . . . ? C34 C35 C52 C45 142.35(19) . . . . ? C36 C35 C52 C51 -141.1(2) . . . . ? C34 C35 C52 C51 0.8(2) . . . . ? C50 C51 C53 C54 1.6(3) . . . . ? C52 C51 C53 C54 143.4(2) . . . . ? C50 C51 C53 C34 -141.17(19) . . . . ? C52 C51 C53 C34 0.6(2) . . . . ? C33 C34 C53 C54 -0.5(3) . . . . ? C35 C34 C53 C54 -142.5(2) . . . . ? C33 C34 C53 C51 142.0(2) . . . . ? C35 C34 C53 C51 -0.1(2) . . . . ? C51 C53 C54 C10 5.0(3) . . . . ? C34 C53 C54 C10 143.2(2) . . . . ? C51 C53 C54 C55 -137.9(2) . . . . ? C34 C53 C54 C55 0.3(3) . . . . ? C9 C10 C54 C53 -7.8(3) . . . . ? C11 C10 C54 C53 -160.47(19) . . . . ? C9 C10 C54 C55 138.58(19) . . . . ? C11 C10 C54 C55 -14.1(2) . . . . ? C13 C12 C55 C56 6.8(3) . . . . ? C11 C12 C55 C56 159.95(18) . . . . ? C13 C12 C55 C54 -138.83(18) . . . . ? C11 C12 C55 C54 14.3(2) . . . . ? C53 C54 C55 C56 0.3(3) . . . . ? C10 C54 C55 C56 -146.68(19) . . . . ? C53 C54 C55 C12 146.89(19) . . . . ? C10 C54 C55 C12 -0.1(2) . . . . ? C12 C55 C56 C57 -4.8(3) . . . . ? C54 C55 C56 C57 137.2(2) . . . . ? C12 C55 C56 C33 -142.8(2) . . . . ? C54 C55 C56 C33 -0.8(3) . . . . ? C34 C33 C56 C55 0.7(3) . . . . ? C32 C33 C56 C55 142.5(2) . . . . ? C34 C33 C56 C57 -141.4(2) . . . . ? C32 C33 C56 C57 0.4(2) . . . . ? C55 C56 C57 C58 -1.8(3) . . . . ? C33 C56 C57 C58 140.90(19) . . . . ? C55 C56 C57 C31 -143.11(19) . . . . ? C33 C56 C57 C31 -0.4(2) . . . . ? C29 C31 C57 C58 2.6(3) . . . . ? C32 C31 C57 C58 -140.0(2) . . . . ? C29 C31 C57 C56 142.9(2) . . . . ? C32 C31 C57 C56 0.3(2) . . . . ? C56 C57 C58 C13 6.3(3) . . . . ? C31 C57 C58 C13 142.9(2) . . . . ? C56 C57 C58 C59 -137.7(2) . . . . ? C31 C57 C58 C59 -1.1(3) . . . . ? C12 C13 C58 C57 -4.3(3) . . . . ? C14 C13 C58 C57 -155.99(18) . . . . ? C12 C13 C58 C59 143.12(18) . . . . ? C14 C13 C58 C59 -8.5(2) . . . . ? C25 C28 C59 C58 141.52(19) . . . . ? C29 C28 C59 C58 4.1(3) . . . . ? C25 C28 C59 C15 -4.6(3) . . . . ? C29 C28 C59 C15 -142.0(2) . . . . ? C57 C58 C59 C28 -2.2(3) . . . . ? C13 C58 C59 C28 -150.42(18) . . . . ? C57 C58 C59 C15 147.85(18) . . . . ? C13 C58 C59 C15 -0.4(2) . . . . ? C16 C15 C59 C28 4.4(3) . . . . ? C14 C15 C59 C28 157.83(19) . . . . ? C16 C15 C59 C58 -144.41(18) . . . . ? C14 C15 C59 C58 9.0(2) . . . . ? C1 N1 C60 C61 -53.2(3) . . . . ? C4 N1 C60 C61 121.6(2) . . . . ? C1 N1 C60 C65 126.2(2) . . . . ? C4 N1 C60 C65 -59.0(3) . . . . ? C65 C60 C61 C62 1.2(3) . . . . ? N1 C60 C61 C62 -179.48(18) . . . . ? C60 C61 C62 C63 0.9(3) . . . . ? C61 C62 C63 C64 -1.9(3) . . . . ? C62 C63 C64 C65 0.8(3) . . . . ? C63 C64 C65 C60 1.3(3) . . . . ? C61 C60 C65 C64 -2.3(3) . . . . ? N1 C60 C65 C64 178.37(19) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.353 _refine_diff_density_min -0.272 _refine_diff_density_rms 0.075 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 0.006 0.000 -0.005 1138 374 ' ' 2 0.254 0.352 -0.007 26 3 ' ' 3 0.746 0.352 0.507 26 4 ' ' 4 0.746 0.648 0.007 26 4 ' ' 5 0.254 0.648 0.493 26 2 ' ' data_b _database_code_depnum_ccdc_archive 'CCDC 905501' #TrackingRef '14609_web_deposit_cif_file_3_Gan,Liangbing_1349923400.12b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C67 H6 Cl6 I N O5' _chemical_formula_weight 1244.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.754(3) _cell_length_b 12.843(3) _cell_length_c 14.630(3) _cell_angle_alpha 78.32(3) _cell_angle_beta 82.27(3) _cell_angle_gamma 68.22(3) _cell_volume 2174.6(8) _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 0.32 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.900 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 1.173 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7053 _exptl_absorpt_correction_T_max 0.9546 _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 19429 _diffrn_reflns_av_R_equivalents 0.1181 _diffrn_reflns_av_sigmaI/netI 0.1329 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 27.43 _reflns_number_total 9832 _reflns_number_gt 7173 _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 SHELXL _refine_ls_extinction_coef 0.0000(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9832 _refine_ls_number_parameters 717 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2178 _refine_ls_R_factor_gt 0.1914 _refine_ls_wR_factor_ref 0.4514 _refine_ls_wR_factor_gt 0.4383 _refine_ls_goodness_of_fit_ref 2.223 _refine_ls_restrained_S_all 2.223 _refine_ls_shift/su_max 1.239 _refine_ls_shift/su_mean 0.002 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 I1 I -0.60460(9) 0.38906(9) 1.27535(7) 0.0367(4) Uani 1 1 d . . . Cl1 Cl 0.6730(4) 0.3739(4) 0.5974(3) 0.0524(11) Uani 1 1 d . . . Cl2 Cl 0.7886(5) 0.1537(4) 0.5420(4) 0.0572(13) Uani 1 1 d . . . Cl3 Cl 0.6261(4) 0.3309(4) 0.4240(3) 0.0533(12) Uani 1 1 d . . . Cl4 Cl 0.1790(5) 0.2632(4) 0.2557(4) 0.0673(15) Uani 1 1 d . . . Cl5 Cl 0.2100(4) 0.0297(4) 0.2506(4) 0.0541(12) Uani 1 1 d . . . Cl6 Cl 0.0167(5) 0.1658(6) 0.3562(4) 0.0813(19) Uani 1 1 d . . . O1 O -0.2118(9) 0.5131(7) 0.9391(8) 0.034(2) Uani 1 1 d . . . O2 O -0.2730(8) 0.2107(8) 0.8657(7) 0.031(2) Uani 1 1 d . . . O3 O -0.0453(9) 0.1037(8) 0.9177(7) 0.033(2) Uani 1 1 d . . . O4 O 0.0581(9) 0.1385(9) 1.0646(7) 0.034(2) Uani 1 1 d . . . O5 O 0.0035(9) 0.3782(9) 0.9888(7) 0.035(2) Uani 1 1 d . . . N1 N -0.2484(11) 0.3493(9) 0.9327(9) 0.031(3) Uani 1 1 d . . . C1 C -0.4871(12) 0.3744(11) 1.1578(9) 0.027(3) Uani 1 1 d . . . C2 C -0.3781(13) 0.3779(11) 1.1667(11) 0.032(3) Uani 1 1 d . . . H2 H -0.3580 0.3847 1.2248 0.039 Uiso 1 1 calc R . . C3 C -0.3052(13) 0.3713(11) 1.0913(10) 0.031(3) Uani 1 1 d . . . H3 H -0.2337 0.3762 1.0960 0.037 Uiso 1 1 calc R . . C4 C -0.3310(12) 0.3578(10) 1.0077(10) 0.026(3) Uani 1 1 d . . . C5 C -0.4351(11) 0.3515(10) 0.9979(9) 0.024(3) Uani 1 1 d . . . H5 H -0.4525 0.3423 0.9396 0.029 Uiso 1 1 calc R . . C6 C -0.5145(12) 0.3588(10) 1.0749(9) 0.026(3) Uani 1 1 d . . . H6 H -0.5856 0.3532 1.0700 0.031 Uiso 1 1 calc R . . C7 C -0.1945(12) 0.4328(11) 0.9035(11) 0.031(3) Uani 1 1 d . . . C8 C -0.1191(12) 0.3970(11) 0.8169(11) 0.031(3) Uani 1 1 d . . . C9 C -0.1380(12) 0.3035(11) 0.7972(10) 0.029(3) Uani 1 1 d . . . C10 C -0.2262(12) 0.2763(11) 0.8659(9) 0.026(3) Uani 1 1 d . . . C11 C -0.0436(13) 0.4415(11) 0.7621(11) 0.035(4) Uani 1 1 d . . . C12 C -0.0268(11) 0.4193(11) 0.6696(9) 0.026(3) Uani 1 1 d . . . C13 C -0.0428(12) 0.3248(12) 0.6497(9) 0.029(3) Uani 1 1 d . . . C14 C -0.0819(12) 0.2524(12) 0.7183(10) 0.031(3) Uani 1 1 d . . . C15 C -0.0087(11) 0.1331(11) 0.7055(9) 0.025(3) Uani 1 1 d . . . C16 C 0.0513(12) 0.1427(13) 0.6104(11) 0.034(3) Uani 1 1 d . . . C17 C 0.0296(14) 0.2618(13) 0.5793(10) 0.035(3) Uani 1 1 d . . . C18 C 0.0418(13) 0.0432(11) 0.7687(10) 0.030(3) Uani 1 1 d . . . C19 C 0.0326(12) 0.0426(11) 0.8746(9) 0.026(3) Uani 1 1 d . . . C20 C 0.1516(13) -0.0205(11) 0.9062(10) 0.032(3) Uani 1 1 d . . . C21 C 0.2193(12) -0.0734(10) 0.8309(11) 0.026(3) Uani 1 1 d . . . C22 C 0.1550(17) -0.0368(13) 0.7494(12) 0.049(5) Uani 1 1 d . . . C23 C 0.2032(12) 0.0128(11) 0.9670(10) 0.028(3) Uani 1 1 d . . . C24 C 0.1503(14) 0.1105(12) 1.0213(9) 0.032(3) Uani 1 1 d . . . C25 C 0.2333(13) 0.1700(12) 1.0040(9) 0.028(3) Uani 1 1 d . . . C26 C 0.3397(13) 0.0939(12) 0.9733(9) 0.032(3) Uani 1 1 d . . . C27 C 0.3224(13) -0.0053(12) 0.9522(10) 0.033(3) Uani 1 1 d . . . C28 C 0.2096(12) 0.2856(12) 0.9714(9) 0.029(3) Uani 1 1 d . . . C29 C 0.0937(13) 0.3745(11) 0.9489(10) 0.027(3) Uani 1 1 d . . . C30 C 0.1157(14) 0.4424(11) 0.8561(11) 0.034(4) Uani 1 1 d . . . C31 C 0.2364(13) 0.4170(12) 0.8460(11) 0.032(3) Uani 1 1 d . . . C32 C 0.2917(14) 0.3248(13) 0.9123(11) 0.038(4) Uani 1 1 d . . . C33 C 0.0523(13) 0.4784(11) 0.7766(11) 0.036(4) Uani 1 1 d . . . C34 C 0.1125(14) 0.4920(11) 0.6860(12) 0.038(4) Uani 1 1 d . . . C35 C 0.0653(14) 0.4553(12) 0.6178(11) 0.038(4) Uani 1 1 d . . . C36 C 0.1309(14) 0.4010(12) 0.5472(10) 0.035(3) Uani 1 1 d . . . C37 C 0.2514(14) 0.3788(13) 0.5365(10) 0.039(4) Uani 1 1 d . . . C38 C 0.2981(13) 0.4137(12) 0.5996(12) 0.038(4) Uani 1 1 d . . . C39 C 0.2272(13) 0.4694(11) 0.6740(11) 0.033(3) Uani 1 1 d . . . C40 C 0.1126(13) 0.3005(13) 0.5247(9) 0.034(3) Uani 1 1 d . . . C41 C 0.2245(13) 0.2176(13) 0.5046(9) 0.033(3) Uani 1 1 d . . . C42 C 0.2436(14) 0.1038(14) 0.5352(10) 0.038(4) Uani 1 1 d . . . C43 C 0.1577(13) 0.0626(14) 0.5906(10) 0.036(3) Uani 1 1 d . . . C44 C 0.2079(14) -0.0296(12) 0.6604(11) 0.035(3) Uani 1 1 d . . . C45 C 0.3297(13) -0.0530(11) 0.6489(11) 0.034(3) Uani 1 1 d . . . C46 C 0.3926(13) -0.0890(11) 0.7294(12) 0.036(4) Uani 1 1 d . . . C47 C 0.3355(13) -0.1000(11) 0.8210(11) 0.034(3) Uani 1 1 d . . . C48 C 0.3891(12) -0.0626(11) 0.8823(10) 0.030(3) Uani 1 1 d . . . C49 C 0.4773(14) -0.0272(13) 0.8324(12) 0.040(4) Uani 1 1 d . . . C50 C 0.4793(13) -0.0392(10) 0.7342(10) 0.032(3) Uani 1 1 d . . . C51 C 0.4984(13) 0.0399(12) 0.6628(11) 0.033(3) Uani 1 1 d . . . C52 C 0.5179(12) 0.1362(13) 0.6816(11) 0.034(3) Uani 1 1 d . . . C53 C 0.5158(13) 0.1510(11) 0.7738(9) 0.027(3) Uiso 1 1 d . . . C54 C 0.4949(12) 0.0678(14) 0.8485(10) 0.035(3) Uani 1 1 d . . . C55 C 0.4251(14) 0.1262(12) 0.9227(11) 0.037(4) Uani 1 1 d . . . C56 C 0.3988(14) 0.2487(14) 0.8927(11) 0.037(4) Uani 1 1 d . . . C57 C 0.4571(12) 0.2631(11) 0.8009(10) 0.026(3) Uani 1 1 d . . . C58 C 0.4048(13) 0.3571(12) 0.7314(11) 0.033(3) Uani 1 1 d . . . C59 C 0.2921(13) 0.4347(10) 0.7571(11) 0.033(3) Uani 1 1 d . . . C60 C 0.4078(13) 0.3429(12) 0.6363(10) 0.032(3) Uani 1 1 d . . . C61 C 0.4597(12) 0.2359(12) 0.6106(9) 0.030(3) Uani 1 1 d . . . C62 C 0.3106(14) 0.2672(14) 0.5104(9) 0.036(3) Uani 1 1 d . . . C63 C 0.4145(14) 0.1961(13) 0.5497(11) 0.037(4) Uani 1 1 d . . . C64 C 0.4360(14) 0.0768(14) 0.5794(12) 0.042(4) Uani 1 1 d . . . C65 C 0.3525(13) 0.0276(12) 0.5741(10) 0.031(3) Uani 1 1 d . . . C66 C 0.7293(14) 0.3025(13) 0.5018(11) 0.039(4) Uani 1 1 d . . . H66 H 0.7907 0.3292 0.4682 0.047 Uiso 1 1 calc R . . C67 C 0.1084(14) 0.1673(15) 0.2554(12) 0.043(4) Uani 1 1 d . . . H67 H 0.0633 0.1927 0.1990 0.052 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 I1 0.0222(6) 0.0512(6) 0.0352(6) -0.0108(4) 0.0057(4) -0.0121(4) Cl1 0.041(3) 0.066(3) 0.056(3) -0.020(2) 0.000(2) -0.022(2) Cl2 0.053(3) 0.052(2) 0.067(3) -0.006(2) -0.017(3) -0.016(2) Cl3 0.056(3) 0.074(3) 0.041(2) 0.006(2) -0.014(2) -0.040(3) Cl4 0.079(4) 0.059(3) 0.072(3) -0.007(2) -0.003(3) -0.036(3) Cl5 0.035(3) 0.058(2) 0.073(3) -0.018(2) 0.012(2) -0.023(2) Cl6 0.051(4) 0.135(5) 0.081(4) -0.060(4) 0.025(3) -0.047(4) O1 0.023(6) 0.026(4) 0.053(6) -0.013(4) 0.004(5) -0.007(4) O2 0.016(5) 0.035(5) 0.047(6) -0.011(4) 0.004(4) -0.014(4) O3 0.024(6) 0.037(5) 0.037(5) -0.002(4) 0.004(4) -0.014(5) O4 0.026(6) 0.049(6) 0.026(5) -0.008(4) 0.001(4) -0.013(5) O5 0.022(6) 0.050(6) 0.037(5) -0.019(5) 0.008(4) -0.014(5) N1 0.021(7) 0.030(5) 0.042(6) -0.009(5) 0.001(5) -0.008(5) C1 0.018(7) 0.039(7) 0.022(6) -0.012(5) 0.002(5) -0.006(6) C2 0.017(7) 0.037(7) 0.046(8) -0.016(6) -0.002(6) -0.010(6) C3 0.023(8) 0.030(6) 0.039(7) 0.000(6) -0.009(6) -0.011(6) C4 0.013(7) 0.026(6) 0.033(6) -0.006(5) -0.004(5) -0.001(5) C5 0.006(6) 0.032(6) 0.035(7) -0.006(5) -0.003(5) -0.007(5) C6 0.016(7) 0.030(6) 0.030(6) -0.007(5) 0.000(5) -0.005(5) C7 0.016(7) 0.034(7) 0.044(8) -0.007(6) 0.000(6) -0.010(6) C8 0.008(6) 0.032(6) 0.050(8) 0.000(6) -0.001(6) -0.009(5) C9 0.014(7) 0.029(6) 0.036(7) 0.002(6) -0.002(6) -0.001(6) C10 0.022(8) 0.031(6) 0.030(6) -0.008(5) -0.001(6) -0.014(6) C11 0.028(9) 0.027(6) 0.045(8) 0.004(6) 0.015(7) -0.013(6) C12 0.009(6) 0.035(6) 0.030(6) 0.005(5) -0.003(5) -0.007(5) C13 0.010(7) 0.044(7) 0.028(6) 0.003(6) -0.007(5) -0.005(6) C14 0.013(7) 0.048(8) 0.037(7) -0.011(6) -0.006(6) -0.013(6) C15 0.011(6) 0.038(7) 0.035(7) -0.008(6) 0.002(5) -0.019(6) C16 0.013(7) 0.057(9) 0.040(8) -0.019(7) -0.001(6) -0.016(7) C17 0.023(8) 0.053(9) 0.029(7) -0.011(6) 0.000(6) -0.012(7) C18 0.032(8) 0.033(6) 0.040(7) -0.010(6) -0.003(6) -0.026(6) C19 0.019(7) 0.035(6) 0.033(7) -0.011(6) 0.003(6) -0.017(6) C20 0.026(8) 0.026(6) 0.041(7) -0.003(6) 0.010(6) -0.011(6) C21 0.014(7) 0.016(5) 0.050(8) -0.009(5) 0.001(6) -0.005(5) C22 0.063(13) 0.044(8) 0.060(10) -0.035(8) 0.041(10) -0.045(9) C23 0.021(8) 0.027(6) 0.034(7) 0.001(5) 0.002(6) -0.010(6) C24 0.029(9) 0.042(7) 0.019(6) 0.004(6) -0.001(6) -0.011(7) C25 0.027(8) 0.039(7) 0.021(6) -0.003(5) -0.005(5) -0.013(6) C26 0.024(8) 0.039(7) 0.027(6) 0.007(6) -0.015(6) -0.006(6) C27 0.022(8) 0.039(7) 0.031(7) 0.011(6) -0.007(6) -0.010(6) C28 0.013(7) 0.047(8) 0.028(6) -0.006(6) -0.003(5) -0.011(6) C29 0.029(8) 0.031(6) 0.032(6) -0.013(5) 0.000(6) -0.019(6) C30 0.027(9) 0.026(6) 0.048(8) -0.015(6) 0.020(7) -0.009(6) C31 0.020(8) 0.035(7) 0.049(8) -0.015(7) -0.002(7) -0.015(6) C32 0.036(10) 0.052(8) 0.044(8) -0.034(7) 0.021(7) -0.031(8) C33 0.021(8) 0.028(6) 0.053(9) -0.010(6) 0.015(7) -0.007(6) C34 0.031(9) 0.018(6) 0.055(9) 0.006(6) 0.004(8) -0.006(6) C35 0.023(8) 0.033(7) 0.044(8) 0.015(6) -0.002(7) -0.006(6) C36 0.035(9) 0.036(7) 0.032(7) 0.010(6) -0.004(6) -0.019(7) C37 0.032(9) 0.045(8) 0.032(7) 0.002(6) 0.017(7) -0.018(7) C38 0.024(8) 0.033(7) 0.054(9) -0.001(7) 0.015(7) -0.016(6) C39 0.020(8) 0.023(6) 0.048(8) 0.007(6) -0.004(7) -0.004(6) C40 0.023(8) 0.053(9) 0.017(6) 0.011(6) -0.007(5) -0.010(7) C41 0.024(8) 0.056(9) 0.020(6) -0.011(6) 0.002(5) -0.014(7) C42 0.027(9) 0.059(9) 0.030(7) -0.023(7) 0.003(6) -0.012(7) C43 0.024(8) 0.062(9) 0.033(7) -0.029(7) 0.006(6) -0.022(7) C44 0.032(9) 0.042(8) 0.044(8) -0.020(7) 0.002(7) -0.021(7) C45 0.017(8) 0.026(6) 0.054(9) -0.018(6) 0.012(7) -0.003(6) C46 0.018(8) 0.022(6) 0.058(9) -0.015(6) 0.003(7) 0.006(6) C47 0.014(7) 0.025(6) 0.054(9) 0.003(6) 0.004(7) -0.002(5) C48 0.015(7) 0.028(6) 0.036(7) -0.001(6) -0.008(6) 0.003(5) C49 0.020(8) 0.040(8) 0.053(9) -0.007(7) 0.000(7) -0.001(7) C50 0.024(8) 0.024(6) 0.041(8) -0.006(6) 0.009(6) -0.002(6) C51 0.015(7) 0.034(7) 0.045(8) -0.011(6) 0.000(6) -0.003(6) C52 0.011(7) 0.050(8) 0.044(8) -0.007(7) 0.006(6) -0.016(6) C54 0.009(7) 0.072(10) 0.030(7) -0.016(7) -0.004(5) -0.016(7) C55 0.024(9) 0.036(7) 0.042(8) 0.005(6) -0.009(7) -0.004(6) C56 0.024(8) 0.059(9) 0.043(8) -0.025(7) 0.004(7) -0.024(7) C57 0.016(7) 0.033(6) 0.034(7) -0.011(6) 0.001(6) -0.013(6) C58 0.019(8) 0.044(8) 0.046(8) -0.017(7) 0.007(6) -0.022(6) C59 0.022(8) 0.023(6) 0.058(9) -0.017(6) 0.010(7) -0.012(6) C60 0.022(8) 0.039(7) 0.035(7) -0.003(6) 0.009(6) -0.017(6) C61 0.018(7) 0.042(7) 0.029(6) -0.005(6) 0.005(6) -0.012(6) C62 0.024(8) 0.062(9) 0.022(6) -0.007(6) 0.007(6) -0.020(7) C63 0.025(9) 0.051(8) 0.038(8) -0.010(7) 0.017(7) -0.023(7) C64 0.027(9) 0.049(9) 0.049(9) -0.024(8) 0.026(7) -0.012(7) C65 0.025(8) 0.043(7) 0.033(7) -0.018(6) 0.008(6) -0.017(6) C66 0.028(9) 0.042(8) 0.048(9) 0.009(7) -0.001(7) -0.021(7) C67 0.018(8) 0.071(11) 0.048(9) -0.025(8) -0.005(7) -0.015(8) _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 I1 C1 2.113(13) . ? Cl1 C66 1.753(17) . ? Cl2 C66 1.779(15) . ? Cl3 C66 1.744(18) . ? Cl4 C67 1.776(18) . ? Cl5 C67 1.770(17) . ? Cl6 C67 1.756(17) . ? O1 C7 1.183(17) . ? O2 C10 1.200(16) . ? O3 C19 1.206(16) . ? O4 C24 1.221(17) . ? O5 C29 1.207(17) . ? N1 C4 1.406(18) . ? N1 C10 1.418(17) . ? N1 C7 1.445(18) . ? C1 C6 1.377(18) . ? C1 C2 1.43(2) . ? C2 C3 1.34(2) . ? C2 H2 0.9500 . ? C3 C4 1.368(19) . ? C3 H3 0.9500 . ? C4 C5 1.388(18) . ? C5 C6 1.403(18) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.52(2) . ? C8 C11 1.383(19) . ? C8 C9 1.40(2) . ? C9 C14 1.418(19) . ? C9 C10 1.498(19) . ? C11 C12 1.41(2) . ? C11 C33 1.52(2) . ? C12 C13 1.39(2) . ? C12 C35 1.48(2) . ? C13 C14 1.40(2) . ? C13 C17 1.447(19) . ? C14 C15 1.505(19) . ? C15 C18 1.33(2) . ? C15 C16 1.500(19) . ? C16 C43 1.40(2) . ? C16 C17 1.44(2) . ? C17 C40 1.42(2) . ? C18 C22 1.46(2) . ? C18 C19 1.537(18) . ? C19 C20 1.52(2) . ? C20 C23 1.39(2) . ? C20 C21 1.425(19) . ? C21 C47 1.386(19) . ? C21 C22 1.44(2) . ? C22 C44 1.39(2) . ? C23 C27 1.44(2) . ? C23 C24 1.514(19) . ? C24 C25 1.49(2) . ? C25 C28 1.39(2) . ? C25 C26 1.424(19) . ? C26 C55 1.38(2) . ? C26 C27 1.47(2) . ? C27 C48 1.38(2) . ? C28 C32 1.44(2) . ? C28 C29 1.52(2) . ? C29 C30 1.510(19) . ? C30 C33 1.41(2) . ? C30 C31 1.44(2) . ? C31 C32 1.39(2) . ? C31 C59 1.41(2) . ? C32 C56 1.39(2) . ? C33 C34 1.45(2) . ? C34 C39 1.37(2) . ? C34 C35 1.46(2) . ? C35 C36 1.37(2) . ? C36 C37 1.45(2) . ? C36 C40 1.50(2) . ? C37 C38 1.39(2) . ? C37 C62 1.45(2) . ? C38 C39 1.44(2) . ? C38 C60 1.46(2) . ? C39 C59 1.46(2) . ? C40 C41 1.46(2) . ? C41 C42 1.38(2) . ? C41 C62 1.48(2) . ? C42 C43 1.47(2) . ? C42 C65 1.48(2) . ? C43 C44 1.41(2) . ? C44 C45 1.46(2) . ? C45 C46 1.41(2) . ? C45 C65 1.43(2) . ? C46 C47 1.44(2) . ? C46 C50 1.48(2) . ? C47 C48 1.44(2) . ? C48 C49 1.42(2) . ? C49 C54 1.39(2) . ? C49 C50 1.47(2) . ? C50 C51 1.37(2) . ? C51 C52 1.43(2) . ? C51 C64 1.45(2) . ? C52 C53 1.40(2) . ? C52 C61 1.49(2) . ? C53 C54 1.44(2) . ? C53 C57 1.464(17) . ? C54 C55 1.45(2) . ? C55 C56 1.47(2) . ? C56 C57 1.46(2) . ? C57 C58 1.42(2) . ? C58 C60 1.43(2) . ? C58 C59 1.464(19) . ? C60 C61 1.391(19) . ? C61 C63 1.39(2) . ? C62 C63 1.42(2) . ? C63 C64 1.44(2) . ? C64 C65 1.44(2) . ? C66 H66 1.0000 . ? C67 H67 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 C4 N1 C10 125.0(12) . . ? C4 N1 C7 122.0(11) . . ? C10 N1 C7 111.7(12) . . ? C6 C1 C2 120.8(13) . . ? C6 C1 I1 120.3(11) . . ? C2 C1 I1 118.9(10) . . ? C3 C2 C1 118.5(14) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 121.8(15) . . ? C2 C3 H3 119.1 . . ? C4 C3 H3 119.1 . . ? C3 C4 C5 120.7(13) . . ? C3 C4 N1 118.0(14) . . ? C5 C4 N1 121.3(13) . . ? C4 C5 C6 119.5(13) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C1 C6 C5 118.6(14) . . ? C1 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? O1 C7 N1 125.4(13) . . ? O1 C7 C8 129.6(14) . . ? N1 C7 C8 104.9(11) . . ? C11 C8 C9 121.7(14) . . ? C11 C8 C7 130.9(13) . . ? C9 C8 C7 107.4(12) . . ? C8 C9 C14 120.8(13) . . ? C8 C9 C10 110.1(12) . . ? C14 C9 C10 128.9(13) . . ? O2 C10 N1 125.5(13) . . ? O2 C10 C9 129.4(12) . . ? N1 C10 C9 105.1(12) . . ? C8 C11 C12 113.0(14) . . ? C8 C11 C33 137.6(15) . . ? C12 C11 C33 106.6(12) . . ? C13 C12 C11 120.6(12) . . ? C13 C12 C35 119.3(13) . . ? C11 C12 C35 110.7(13) . . ? C12 C13 C14 122.0(13) . . ? C12 C13 C17 120.8(13) . . ? C14 C13 C17 109.9(13) . . ? C13 C14 C9 113.0(13) . . ? C13 C14 C15 106.4(12) . . ? C9 C14 C15 133.8(13) . . ? C18 C15 C16 117.1(13) . . ? C18 C15 C14 129.9(13) . . ? C16 C15 C14 106.2(12) . . ? C43 C16 C17 120.1(14) . . ? C43 C16 C15 121.0(14) . . ? C17 C16 C15 106.0(12) . . ? C40 C17 C16 121.2(14) . . ? C40 C17 C13 120.2(15) . . ? C16 C17 C13 109.1(13) . . ? C15 C18 C22 121.6(14) . . ? C15 C18 C19 124.8(12) . . ? C22 C18 C19 104.8(13) . . ? O3 C19 C20 126.0(13) . . ? O3 C19 C18 125.9(14) . . ? C20 C19 C18 105.7(11) . . ? C23 C20 C21 118.4(14) . . ? C23 C20 C19 125.5(12) . . ? C21 C20 C19 107.7(13) . . ? C47 C21 C20 122.1(14) . . ? C47 C21 C22 119.9(14) . . ? C20 C21 C22 109.5(12) . . ? C44 C22 C21 120.9(17) . . ? C44 C22 C18 120.5(18) . . ? C21 C22 C18 110.9(12) . . ? C20 C23 C27 119.8(13) . . ? C20 C23 C24 127.6(13) . . ? C27 C23 C24 106.8(13) . . ? O4 C24 C25 127.7(14) . . ? O4 C24 C23 128.3(15) . . ? C25 C24 C23 103.9(12) . . ? C28 C25 C26 116.9(13) . . ? C28 C25 C24 126.2(14) . . ? C26 C25 C24 108.5(12) . . ? C55 C26 C25 125.0(14) . . ? C55 C26 C27 117.9(14) . . ? C25 C26 C27 108.3(14) . . ? C48 C27 C23 121.5(14) . . ? C48 C27 C26 120.4(14) . . ? C23 C27 C26 108.1(13) . . ? C25 C28 C32 120.7(14) . . ? C25 C28 C29 126.3(14) . . ? C32 C28 C29 106.6(13) . . ? O5 C29 C30 127.9(14) . . ? O5 C29 C28 127.3(13) . . ? C30 C29 C28 103.9(12) . . ? C33 C30 C31 120.3(13) . . ? C33 C30 C29 128.2(14) . . ? C31 C30 C29 105.7(14) . . ? C32 C31 C59 119.0(14) . . ? C32 C31 C30 111.2(13) . . ? C59 C31 C30 121.0(15) . . ? C56 C32 C31 121.7(14) . . ? C56 C32 C28 120.2(15) . . ? C31 C32 C28 109.4(15) . . ? C30 C33 C34 117.4(15) . . ? C30 C33 C11 126.0(13) . . ? C34 C33 C11 106.8(14) . . ? C39 C34 C33 123.7(16) . . ? C39 C34 C35 115.6(15) . . ? C33 C34 C35 109.2(14) . . ? C36 C35 C34 122.4(15) . . ? C36 C35 C12 121.0(14) . . ? C34 C35 C12 106.0(13) . . ? C35 C36 C37 120.6(15) . . ? C35 C36 C40 119.6(14) . . ? C37 C36 C40 107.5(13) . . ? C38 C37 C36 118.1(13) . . ? C38 C37 C62 118.9(15) . . ? C36 C37 C62 109.6(15) . . ? C37 C38 C39 120.1(15) . . ? C37 C38 C60 121.2(13) . . ? C39 C38 C60 107.6(14) . . ? C34 C39 C38 123.2(16) . . ? C34 C39 C59 118.5(14) . . ? C38 C39 C59 108.7(13) . . ? C17 C40 C41 119.1(14) . . ? C17 C40 C36 118.8(13) . . ? C41 C40 C36 107.0(14) . . ? C42 C41 C40 118.7(14) . . ? C42 C41 C62 121.4(15) . . ? C40 C41 C62 108.4(14) . . ? C41 C42 C43 122.6(14) . . ? C41 C42 C65 120.3(15) . . ? C43 C42 C65 105.2(14) . . ? C16 C43 C44 119.5(14) . . ? C16 C43 C42 118.2(15) . . ? C44 C43 C42 110.5(14) . . ? C22 C44 C43 119.8(16) . . ? C22 C44 C45 119.8(16) . . ? C43 C44 C45 107.0(14) . . ? C46 C45 C65 119.7(15) . . ? C46 C45 C44 119.1(14) . . ? C65 C45 C44 109.2(14) . . ? C45 C46 C47 119.7(14) . . ? C45 C46 C50 118.6(14) . . ? C47 C46 C50 108.1(14) . . ? C21 C47 C46 120.6(15) . . ? C21 C47 C48 119.5(13) . . ? C46 C47 C48 107.0(14) . . ? C27 C48 C49 119.9(14) . . ? C27 C48 C47 118.3(14) . . ? C49 C48 C47 110.7(13) . . ? C54 C49 C48 121.6(14) . . ? C54 C49 C50 117.0(14) . . ? C48 C49 C50 107.2(14) . . ? C51 C50 C49 120.9(14) . . ? C51 C50 C46 121.0(15) . . ? C49 C50 C46 106.8(13) . . ? C50 C51 C52 120.8(14) . . ? C50 C51 C64 121.3(15) . . ? C52 C51 C64 107.4(13) . . ? C53 C52 C51 119.9(14) . . ? C53 C52 C61 119.4(13) . . ? C51 C52 C61 107.4(13) . . ? C52 C53 C54 118.8(12) . . ? C52 C53 C57 120.4(12) . . ? C54 C53 C57 107.8(12) . . ? C49 C54 C53 122.5(13) . . ? C49 C54 C55 117.8(15) . . ? C53 C54 C55 108.5(13) . . ? C26 C55 C54 122.3(15) . . ? C26 C55 C56 116.2(14) . . ? C54 C55 C56 108.4(14) . . ? C32 C56 C57 120.4(15) . . ? C32 C56 C55 120.2(14) . . ? C57 C56 C55 106.8(13) . . ? C58 C57 C56 119.9(13) . . ? C58 C57 C53 119.0(12) . . ? C56 C57 C53 108.5(12) . . ? C57 C58 C60 120.9(12) . . ? C57 C58 C59 116.8(13) . . ? C60 C58 C59 108.7(14) . . ? C31 C59 C39 118.8(14) . . ? C31 C59 C58 122.1(14) . . ? C39 C59 C58 106.7(13) . . ? C61 C60 C58 120.4(14) . . ? C61 C60 C38 117.3(14) . . ? C58 C60 C38 108.3(13) . . ? C63 C61 C60 123.3(15) . . ? C63 C61 C52 107.2(13) . . ? C60 C61 C52 119.7(13) . . ? C63 C62 C37 119.8(15) . . ? C63 C62 C41 119.1(14) . . ? C37 C62 C41 107.4(14) . . ? C61 C63 C62 119.3(14) . . ? C61 C63 C64 109.9(15) . . ? C62 C63 C64 119.6(16) . . ? C63 C64 C65 121.6(16) . . ? C63 C64 C51 108.1(15) . . ? C65 C64 C51 117.8(15) . . ? C45 C65 C64 121.6(15) . . ? C45 C65 C42 108.0(13) . . ? C64 C65 C42 117.8(14) . . ? Cl3 C66 Cl1 111.2(9) . . ? Cl3 C66 Cl2 110.0(9) . . ? Cl1 C66 Cl2 109.8(9) . . ? Cl3 C66 H66 108.6 . . ? Cl1 C66 H66 108.6 . . ? Cl2 C66 H66 108.6 . . ? Cl6 C67 Cl5 110.5(10) . . ? Cl6 C67 Cl4 110.0(9) . . ? Cl5 C67 Cl4 109.2(9) . . ? Cl6 C67 H67 109.0 . . ? Cl5 C67 H67 109.0 . . ? Cl4 C67 H67 109.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 3(2) . . . . ? I1 C1 C2 C3 -178.4(10) . . . . ? C1 C2 C3 C4 -2(2) . . . . ? C2 C3 C4 C5 1(2) . . . . ? C2 C3 C4 N1 -178.7(13) . . . . ? C10 N1 C4 C3 141.7(14) . . . . ? C7 N1 C4 C3 -52.5(18) . . . . ? C10 N1 C4 C5 -38(2) . . . . ? C7 N1 C4 C5 128.1(15) . . . . ? C3 C4 C5 C6 -0.2(19) . . . . ? N1 C4 C5 C6 179.1(11) . . . . ? C2 C1 C6 C5 -3(2) . . . . ? I1 C1 C6 C5 178.9(9) . . . . ? C4 C5 C6 C1 1.3(19) . . . . ? C4 N1 C7 O1 1(2) . . . . ? C10 N1 C7 O1 168.7(15) . . . . ? C4 N1 C7 C8 -175.7(12) . . . . ? C10 N1 C7 C8 -8.2(16) . . . . ? O1 C7 C8 C11 7(3) . . . . ? N1 C7 C8 C11 -176.4(16) . . . . ? O1 C7 C8 C9 -173.0(16) . . . . ? N1 C7 C8 C9 3.8(16) . . . . ? C11 C8 C9 C14 -2(2) . . . . ? C7 C8 C9 C14 178.2(13) . . . . ? C11 C8 C9 C10 -178.2(14) . . . . ? C7 C8 C9 C10 1.6(16) . . . . ? C4 N1 C10 O2 -2(2) . . . . ? C7 N1 C10 O2 -168.7(14) . . . . ? C4 N1 C10 C9 176.1(12) . . . . ? C7 N1 C10 C9 9.1(15) . . . . ? C8 C9 C10 O2 171.2(15) . . . . ? C14 C9 C10 O2 -5(3) . . . . ? C8 C9 C10 N1 -6.5(16) . . . . ? C14 C9 C10 N1 177.2(13) . . . . ? C9 C8 C11 C12 25(2) . . . . ? C7 C8 C11 C12 -154.5(15) . . . . ? C9 C8 C11 C33 -132.4(18) . . . . ? C7 C8 C11 C33 48(3) . . . . ? C8 C11 C12 C13 -26(2) . . . . ? C33 C11 C12 C13 138.1(13) . . . . ? C8 C11 C12 C35 -172.6(12) . . . . ? C33 C11 C12 C35 -8.2(16) . . . . ? C11 C12 C13 C14 4(2) . . . . ? C35 C12 C13 C14 147.2(14) . . . . ? C11 C12 C13 C17 -143.3(14) . . . . ? C35 C12 C13 C17 0(2) . . . . ? C12 C13 C14 C9 20(2) . . . . ? C17 C13 C14 C9 170.3(13) . . . . ? C12 C13 C14 C15 -135.3(13) . . . . ? C17 C13 C14 C15 15.0(16) . . . . ? C8 C9 C14 C13 -21.2(19) . . . . ? C10 C9 C14 C13 154.7(14) . . . . ? C8 C9 C14 C15 125.0(17) . . . . ? C10 C9 C14 C15 -59(2) . . . . ? C13 C14 C15 C18 133.9(15) . . . . ? C9 C14 C15 C18 -14(3) . . . . ? C13 C14 C15 C16 -15.5(15) . . . . ? C9 C14 C15 C16 -163.3(16) . . . . ? C18 C15 C16 C43 -2(2) . . . . ? C14 C15 C16 C43 151.7(14) . . . . ? C18 C15 C16 C17 -143.8(13) . . . . ? C14 C15 C16 C17 10.2(16) . . . . ? C43 C16 C17 C40 3(2) . . . . ? C15 C16 C17 C40 144.8(14) . . . . ? C43 C16 C17 C13 -143.3(14) . . . . ? C15 C16 C17 C13 -1.5(17) . . . . ? C12 C13 C17 C40 -5(2) . . . . ? C14 C13 C17 C40 -155.4(14) . . . . ? C12 C13 C17 C16 141.9(14) . . . . ? C14 C13 C17 C16 -8.7(18) . . . . ? C16 C15 C18 C22 5.6(19) . . . . ? C14 C15 C18 C22 -141.1(15) . . . . ? C16 C15 C18 C19 148.2(13) . . . . ? C14 C15 C18 C19 1(2) . . . . ? C15 C18 C19 O3 27(2) . . . . ? C22 C18 C19 O3 174.3(13) . . . . ? C15 C18 C19 C20 -136.2(14) . . . . ? C22 C18 C19 C20 11.4(13) . . . . ? O3 C19 C20 C23 -27(2) . . . . ? C18 C19 C20 C23 135.8(13) . . . . ? O3 C19 C20 C21 -174.4(13) . . . . ? C18 C19 C20 C21 -11.5(14) . . . . ? C23 C20 C21 C47 5.0(19) . . . . ? C19 C20 C21 C47 154.9(13) . . . . ? C23 C20 C21 C22 -142.9(13) . . . . ? C19 C20 C21 C22 7.0(15) . . . . ? C47 C21 C22 C44 1(2) . . . . ? C20 C21 C22 C44 149.9(13) . . . . ? C47 C21 C22 C18 -148.2(12) . . . . ? C20 C21 C22 C18 0.5(16) . . . . ? C15 C18 C22 C44 -8(2) . . . . ? C19 C18 C22 C44 -157.2(14) . . . . ? C15 C18 C22 C21 141.3(13) . . . . ? C19 C18 C22 C21 -7.6(14) . . . . ? C21 C20 C23 C27 0.8(19) . . . . ? C19 C20 C23 C27 -143.3(14) . . . . ? C21 C20 C23 C24 150.4(13) . . . . ? C19 C20 C23 C24 6(2) . . . . ? C20 C23 C24 O4 44(2) . . . . ? C27 C23 C24 O4 -163.6(14) . . . . ? C20 C23 C24 C25 -132.3(15) . . . . ? C27 C23 C24 C25 20.4(14) . . . . ? O4 C24 C25 C28 -49(2) . . . . ? C23 C24 C25 C28 127.4(14) . . . . ? O4 C24 C25 C26 164.6(13) . . . . ? C23 C24 C25 C26 -19.4(14) . . . . ? C28 C25 C26 C55 7(2) . . . . ? C24 C25 C26 C55 157.8(14) . . . . ? C28 C25 C26 C27 -139.1(13) . . . . ? C24 C25 C26 C27 11.3(15) . . . . ? C20 C23 C27 C48 -5(2) . . . . ? C24 C23 C27 C48 -159.9(12) . . . . ? C20 C23 C27 C26 141.0(13) . . . . ? C24 C23 C27 C26 -14.3(14) . . . . ? C55 C26 C27 C48 -1(2) . . . . ? C25 C26 C27 C48 148.2(13) . . . . ? C55 C26 C27 C23 -147.2(13) . . . . ? C25 C26 C27 C23 2.1(15) . . . . ? C26 C25 C28 C32 -2(2) . . . . ? C24 C25 C28 C32 -146.7(14) . . . . ? C26 C25 C28 C29 145.9(14) . . . . ? C24 C25 C28 C29 1(2) . . . . ? C25 C28 C29 O5 35(2) . . . . ? C32 C28 C29 O5 -173.2(13) . . . . ? C25 C28 C29 C30 -134.8(14) . . . . ? C32 C28 C29 C30 16.9(14) . . . . ? O5 C29 C30 C33 -35(2) . . . . ? C28 C29 C30 C33 135.1(14) . . . . ? O5 C29 C30 C31 172.9(13) . . . . ? C28 C29 C30 C31 -17.4(13) . . . . ? C33 C30 C31 C32 -143.0(13) . . . . ? C29 C30 C31 C32 12.1(15) . . . . ? C33 C30 C31 C59 4(2) . . . . ? C29 C30 C31 C59 159.3(12) . . . . ? C59 C31 C32 C56 -1(2) . . . . ? C30 C31 C32 C56 146.4(14) . . . . ? C59 C31 C32 C28 -149.0(13) . . . . ? C30 C31 C32 C28 -1.2(16) . . . . ? C25 C28 C32 C56 -5(2) . . . . ? C29 C28 C32 C56 -158.4(14) . . . . ? C25 C28 C32 C31 143.3(13) . . . . ? C29 C28 C32 C31 -10.2(15) . . . . ? C31 C30 C33 C34 -1.9(19) . . . . ? C29 C30 C33 C34 -150.9(13) . . . . ? C31 C30 C33 C11 139.3(14) . . . . ? C29 C30 C33 C11 -10(2) . . . . ? C8 C11 C33 C30 22(3) . . . . ? C12 C11 C33 C30 -136.3(14) . . . . ? C8 C11 C33 C34 166.7(16) . . . . ? C12 C11 C33 C34 8.1(15) . . . . ? C30 C33 C34 C39 1(2) . . . . ? C11 C33 C34 C39 -146.6(14) . . . . ? C30 C33 C34 C35 142.9(13) . . . . ? C11 C33 C34 C35 -5.1(15) . . . . ? C39 C34 C35 C36 0.6(19) . . . . ? C33 C34 C35 C36 -144.3(14) . . . . ? C39 C34 C35 C12 145.3(12) . . . . ? C33 C34 C35 C12 0.3(15) . . . . ? C13 C12 C35 C36 4(2) . . . . ? C11 C12 C35 C36 150.3(14) . . . . ? C13 C12 C35 C34 -141.6(13) . . . . ? C11 C12 C35 C34 5.1(16) . . . . ? C34 C35 C36 C37 -1(2) . . . . ? C12 C35 C36 C37 -140.3(14) . . . . ? C34 C35 C36 C40 136.9(15) . . . . ? C12 C35 C36 C40 -3(2) . . . . ? C35 C36 C37 C38 0(2) . . . . ? C40 C36 C37 C38 -142.0(13) . . . . ? C35 C36 C37 C62 140.7(13) . . . . ? C40 C36 C37 C62 -1.4(16) . . . . ? C36 C37 C38 C39 1(2) . . . . ? C62 C37 C38 C39 -136.3(14) . . . . ? C36 C37 C38 C60 140.0(14) . . . . ? C62 C37 C38 C60 3(2) . . . . ? C33 C34 C39 C38 139.5(15) . . . . ? C35 C34 C39 C38 0.2(19) . . . . ? C33 C34 C39 C59 -3(2) . . . . ? C35 C34 C39 C59 -142.2(13) . . . . ? C37 C38 C39 C34 -1(2) . . . . ? C60 C38 C39 C34 -145.1(14) . . . . ? C37 C38 C39 C59 144.7(14) . . . . ? C60 C38 C39 C59 0.4(16) . . . . ? C16 C17 C40 C41 -4(2) . . . . ? C13 C17 C40 C41 138.9(15) . . . . ? C16 C17 C40 C36 -137.1(15) . . . . ? C13 C17 C40 C36 6(2) . . . . ? C35 C36 C40 C17 -2(2) . . . . ? C37 C36 C40 C17 140.7(14) . . . . ? C35 C36 C40 C41 -140.3(14) . . . . ? C37 C36 C40 C41 2.3(15) . . . . ? C17 C40 C41 C42 3(2) . . . . ? C36 C40 C41 C42 141.7(13) . . . . ? C17 C40 C41 C62 -140.6(14) . . . . ? C36 C40 C41 C62 -2.4(14) . . . . ? C40 C41 C42 C43 -3(2) . . . . ? C62 C41 C42 C43 136.6(15) . . . . ? C40 C41 C42 C65 -139.9(14) . . . . ? C62 C41 C42 C65 -1(2) . . . . ? C17 C16 C43 C44 137.5(15) . . . . ? C15 C16 C43 C44 1(2) . . . . ? C17 C16 C43 C42 -2(2) . . . . ? C15 C16 C43 C42 -138.1(14) . . . . ? C41 C42 C43 C16 2(2) . . . . ? C65 C42 C43 C16 144.5(13) . . . . ? C41 C42 C43 C44 -140.9(14) . . . . ? C65 C42 C43 C44 1.7(15) . . . . ? C21 C22 C44 C43 -139.5(15) . . . . ? C18 C22 C44 C43 7(2) . . . . ? C21 C22 C44 C45 -4(2) . . . . ? C18 C22 C44 C45 142.8(15) . . . . ? C16 C43 C44 C22 -4(2) . . . . ? C42 C43 C44 C22 138.5(15) . . . . ? C16 C43 C44 C45 -144.5(14) . . . . ? C42 C43 C44 C45 -2.2(15) . . . . ? C22 C44 C45 C46 4(2) . . . . ? C43 C44 C45 C46 144.4(13) . . . . ? C22 C44 C45 C65 -138.9(14) . . . . ? C43 C44 C45 C65 1.9(16) . . . . ? C65 C45 C46 C47 137.4(14) . . . . ? C44 C45 C46 C47 -1(2) . . . . ? C65 C45 C46 C50 1.5(18) . . . . ? C44 C45 C46 C50 -137.1(13) . . . . ? C20 C21 C47 C46 -143.4(14) . . . . ? C22 C21 C47 C46 1(2) . . . . ? C20 C21 C47 C48 -7(2) . . . . ? C22 C21 C47 C48 137.8(14) . . . . ? C45 C46 C47 C21 -1(2) . . . . ? C50 C46 C47 C21 138.7(13) . . . . ? C45 C46 C47 C48 -142.5(13) . . . . ? C50 C46 C47 C48 -2.4(14) . . . . ? C23 C27 C48 C49 143.4(14) . . . . ? C26 C27 C48 C49 2(2) . . . . ? C23 C27 C48 C47 3(2) . . . . ? C26 C27 C48 C47 -138.8(14) . . . . ? C21 C47 C48 C27 3(2) . . . . ? C46 C47 C48 C27 144.6(13) . . . . ? C21 C47 C48 C49 -141.1(13) . . . . ? C46 C47 C48 C49 0.6(15) . . . . ? C27 C48 C49 C54 -3(2) . . . . ? C47 C48 C49 C54 139.9(15) . . . . ? C27 C48 C49 C50 -141.8(13) . . . . ? C47 C48 C49 C50 1.5(16) . . . . ? C54 C49 C50 C51 0(2) . . . . ? C48 C49 C50 C51 141.0(14) . . . . ? C54 C49 C50 C46 -143.6(14) . . . . ? C48 C49 C50 C46 -2.9(15) . . . . ? C45 C46 C50 C51 0.0(19) . . . . ? C47 C46 C50 C51 -140.5(13) . . . . ? C45 C46 C50 C49 143.9(12) . . . . ? C47 C46 C50 C49 3.3(15) . . . . ? C49 C50 C51 C52 1(2) . . . . ? C46 C50 C51 C52 139.4(14) . . . . ? C49 C50 C51 C64 -139.7(15) . . . . ? C46 C50 C51 C64 -1(2) . . . . ? C50 C51 C52 C53 -1(2) . . . . ? C64 C51 C52 C53 144.1(14) . . . . ? C50 C51 C52 C61 -141.8(14) . . . . ? C64 C51 C52 C61 3.3(16) . . . . ? C51 C52 C53 C54 1(2) . . . . ? C61 C52 C53 C54 136.7(14) . . . . ? C51 C52 C53 C57 -136.1(15) . . . . ? C61 C52 C53 C57 0(2) . . . . ? C48 C49 C54 C53 -135.4(16) . . . . ? C50 C49 C54 C53 -1(2) . . . . ? C48 C49 C54 C55 4(2) . . . . ? C50 C49 C54 C55 138.7(14) . . . . ? C52 C53 C54 C49 0(2) . . . . ? C57 C53 C54 C49 141.9(15) . . . . ? C52 C53 C54 C55 -142.3(14) . . . . ? C57 C53 C54 C55 -0.8(17) . . . . ? C25 C26 C55 C54 -141.8(15) . . . . ? C27 C26 C55 C54 2(2) . . . . ? C25 C26 C55 C56 -5(2) . . . . ? C27 C26 C55 C56 138.5(14) . . . . ? C49 C54 C55 C26 -3(2) . . . . ? C53 C54 C55 C26 141.4(14) . . . . ? C49 C54 C55 C56 -142.9(15) . . . . ? C53 C54 C55 C56 1.8(18) . . . . ? C31 C32 C56 C57 0(2) . . . . ? C28 C32 C56 C57 144.1(15) . . . . ? C31 C32 C56 C55 -137.0(16) . . . . ? C28 C32 C56 C55 7(2) . . . . ? C26 C55 C56 C32 -2(2) . . . . ? C54 C55 C56 C32 139.9(15) . . . . ? C26 C55 C56 C57 -144.4(14) . . . . ? C54 C55 C56 C57 -2.1(18) . . . . ? C32 C56 C57 C58 1(2) . . . . ? C55 C56 C57 C58 143.1(14) . . . . ? C32 C56 C57 C53 -140.3(14) . . . . ? C55 C56 C57 C53 1.6(17) . . . . ? C52 C53 C57 C58 -2(2) . . . . ? C54 C53 C57 C58 -142.4(13) . . . . ? C52 C53 C57 C56 140.3(14) . . . . ? C54 C53 C57 C56 -0.5(17) . . . . ? C56 C57 C58 C60 -136.8(15) . . . . ? C53 C57 C58 C60 1(2) . . . . ? C56 C57 C58 C59 -0.6(19) . . . . ? C53 C57 C58 C59 136.9(14) . . . . ? C32 C31 C59 C39 139.0(14) . . . . ? C30 C31 C59 C39 -5.6(19) . . . . ? C32 C31 C59 C58 2(2) . . . . ? C30 C31 C59 C58 -142.7(14) . . . . ? C34 C39 C59 C31 4.9(19) . . . . ? C38 C39 C59 C31 -142.5(13) . . . . ? C34 C39 C59 C58 147.9(13) . . . . ? C38 C39 C59 C58 0.5(15) . . . . ? C57 C58 C59 C31 -1(2) . . . . ? C60 C58 C59 C31 140.2(14) . . . . ? C57 C58 C59 C39 -142.4(13) . . . . ? C60 C58 C59 C39 -1.3(15) . . . . ? C57 C58 C60 C61 2(2) . . . . ? C59 C58 C60 C61 -137.6(14) . . . . ? C57 C58 C60 C38 140.8(14) . . . . ? C59 C58 C60 C38 1.5(16) . . . . ? C37 C38 C60 C61 -4(2) . . . . ? C39 C38 C60 C61 139.4(13) . . . . ? C37 C38 C60 C58 -145.0(14) . . . . ? C39 C38 C60 C58 -1.2(16) . . . . ? C58 C60 C61 C63 138.2(15) . . . . ? C38 C60 C61 C63 3(2) . . . . ? C58 C60 C61 C52 -3(2) . . . . ? C38 C60 C61 C52 -138.8(14) . . . . ? C53 C52 C61 C63 -144.5(14) . . . . ? C51 C52 C61 C63 -3.5(16) . . . . ? C53 C52 C61 C60 2(2) . . . . ? C51 C52 C61 C60 143.3(14) . . . . ? C38 C37 C62 C63 0(2) . . . . ? C36 C37 C62 C63 -140.2(14) . . . . ? C38 C37 C62 C41 140.2(14) . . . . ? C36 C37 C62 C41 -0.1(16) . . . . ? C42 C41 C62 C63 -1(2) . . . . ? C40 C41 C62 C63 141.9(13) . . . . ? C42 C41 C62 C37 -141.4(13) . . . . ? C40 C41 C62 C37 1.5(15) . . . . ? C60 C61 C63 C62 1(2) . . . . ? C52 C61 C63 C62 145.9(13) . . . . ? C60 C61 C63 C64 -143.1(14) . . . . ? C52 C61 C63 C64 2.3(16) . . . . ? C37 C62 C63 C61 -2(2) . . . . ? C41 C62 C63 C61 -137.5(14) . . . . ? C37 C62 C63 C64 138.1(15) . . . . ? C41 C62 C63 C64 3(2) . . . . ? C61 C63 C64 C65 140.7(14) . . . . ? C62 C63 C64 C65 -3(2) . . . . ? C61 C63 C64 C51 -0.3(17) . . . . ? C62 C63 C64 C51 -143.8(14) . . . . ? C50 C51 C64 C63 142.9(13) . . . . ? C52 C51 C64 C63 -2.0(16) . . . . ? C50 C51 C64 C65 0(2) . . . . ? C52 C51 C64 C65 -144.7(13) . . . . ? C46 C45 C65 C64 -2.1(19) . . . . ? C44 C45 C65 C64 140.1(14) . . . . ? C46 C45 C65 C42 -143.0(12) . . . . ? C44 C45 C65 C42 -0.8(16) . . . . ? C63 C64 C65 C45 -136.1(15) . . . . ? C51 C64 C65 C45 1(2) . . . . ? C63 C64 C65 C42 1(2) . . . . ? C51 C64 C65 C42 138.6(14) . . . . ? C41 C42 C65 C45 143.2(13) . . . . ? C43 C42 C65 C45 -0.5(15) . . . . ? C41 C42 C65 C64 0.6(19) . . . . ? C43 C42 C65 C64 -143.1(13) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 5.622 _refine_diff_density_min -2.234 _refine_diff_density_rms 0.323 data_d _database_code_depnum_ccdc_archive 'CCDC 905502' #TrackingRef 'web_deposit_cif_file_4_Gan,Liangbing_1349923400.12d.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H9 N O7' _chemical_formula_sum 'C68 H9 N O7' _chemical_formula_weight 951.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 19.163(6) _cell_length_b 13.468(4) _cell_length_c 18.553(7) _cell_angle_alpha 90.00 _cell_angle_beta 114.320(4) _cell_angle_gamma 90.00 _cell_volume 4363(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10406 _cell_measurement_theta_min 1.2044 _cell_measurement_theta_max 27.4564 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 0.095 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5590 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _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 'Saturn724+ CCD' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26101 _diffrn_reflns_av_R_equivalents 0.1254 _diffrn_reflns_av_sigmaI/netI 0.1319 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7651 _reflns_number_gt 4255 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELX-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELX-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Mercury: visualization and analysis of crystal structures, C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor, M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006. ; _computing_publication_material 'SHELX-97 (Sheldrick, 2008)' _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^)+(0.1657P)^2^+3.9512P] 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 7651 _refine_ls_number_parameters 715 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.1840 _refine_ls_R_factor_gt 0.1190 _refine_ls_wR_factor_ref 0.3354 _refine_ls_wR_factor_gt 0.2952 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.065 _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 O1 O 0.4601(2) 0.3939(3) 0.4673(3) 0.0305(11) Uani 1 1 d . . . O2 O 0.5208(3) 0.4217(4) 0.6380(3) 0.0415(13) Uani 1 1 d . A . O3 O 0.4702(3) 0.2123(4) 0.6499(3) 0.0378(12) Uani 1 1 d . . . O4 O 0.5050(3) 0.2515(4) 0.3853(3) 0.0345(11) Uani 1 1 d . . . O5 O 0.5066(3) 0.0466(4) 0.5821(3) 0.0390(12) Uani 1 1 d . A . O6 O 0.8866(3) 0.1728(6) 0.7151(4) 0.083(2) Uani 1 1 d . A . N1 N 0.5268(3) 0.1684(4) 0.5017(3) 0.0273(12) Uani 1 1 d . A . C1 C 0.9972(10) 0.0677(10) 0.6148(13) 0.066(5) Uani 0.61(3) 1 d PDU A 1 H1A H 0.9759 0.0457 0.5596 0.100 Uiso 0.61(3) 1 calc PR A 1 H1B H 0.9838 0.0197 0.6468 0.100 Uiso 0.61(3) 1 calc PR A 1 H1C H 1.0531 0.0723 0.6347 0.100 Uiso 0.61(3) 1 calc PR A 1 C2 C 0.9642(6) 0.1698(11) 0.6202(10) 0.057(4) Uani 0.61(3) 1 d PDU A 1 H2B H 0.9861 0.1927 0.6759 0.068 Uiso 0.61(3) 1 calc PR A 1 H2A H 0.9780 0.2187 0.5884 0.068 Uiso 0.61(3) 1 calc PR A 1 O7 O 0.8821(6) 0.1631(10) 0.5912(6) 0.044(3) Uani 0.61(3) 1 d PDU A 1 C1' C 0.990(2) 0.091(3) 0.573(2) 0.104(10) Uani 0.39(3) 1 d PDU A 2 H1'A H 0.9670 0.1355 0.5275 0.156 Uiso 0.39(3) 1 calc PR A 2 H1'B H 0.9739 0.0225 0.5564 0.156 Uiso 0.39(3) 1 calc PR A 2 H1'C H 1.0464 0.0949 0.5928 0.156 Uiso 0.39(3) 1 calc PR A 2 C2' C 0.9656(14) 0.122(3) 0.6385(17) 0.087(7) Uani 0.39(3) 1 d PDU A 2 H2'A H 0.9795 0.0703 0.6804 0.105 Uiso 0.39(3) 1 calc PR A 2 H2'B H 0.9889 0.1856 0.6626 0.105 Uiso 0.39(3) 1 calc PR A 2 O7' O 0.8835(13) 0.130(2) 0.5965(13) 0.075(7) Uani 0.39(3) 1 d PDU A 2 C3 C 0.8523(4) 0.1619(6) 0.6450(4) 0.047(2) Uani 1 1 d D . . C4 C 0.7653(4) 0.1616(5) 0.6041(4) 0.0355(17) Uani 1 1 d . A . C5 C 0.7247(4) 0.1894(6) 0.6483(4) 0.0380(18) Uani 1 1 d . . . H5 H 0.7512 0.2060 0.7026 0.046 Uiso 1 1 calc R A . C6 C 0.6456(4) 0.1928(5) 0.6126(4) 0.0362(17) Uani 1 1 d . A . H6 H 0.6173 0.2152 0.6411 0.043 Uiso 1 1 calc R . . C7 C 0.6084(4) 0.1630(5) 0.5348(4) 0.0325(16) Uani 1 1 d . . . C8 C 0.6481(3) 0.1337(5) 0.4907(4) 0.0281(15) Uani 1 1 d . A . H8 H 0.6212 0.1141 0.4371 0.034 Uiso 1 1 calc R . . C9 C 0.7267(4) 0.1331(5) 0.5253(4) 0.0306(15) Uani 1 1 d . . . H9 H 0.7546 0.1134 0.4956 0.037 Uiso 1 1 calc R A . C10 C 0.4830(4) 0.1112(5) 0.5320(4) 0.0313(16) Uani 1 1 d . . . C11 C 0.4026(4) 0.1391(5) 0.4832(4) 0.0293(15) Uani 1 1 d . A . C12 C 0.3996(4) 0.2011(5) 0.4209(4) 0.0286(15) Uani 1 1 d . . . C13 C 0.4824(4) 0.2144(5) 0.4309(4) 0.0283(15) Uani 1 1 d . A . C14 C 0.3310(4) 0.2408(5) 0.3658(3) 0.0304(15) Uani 1 1 d . A . C15 C 0.2644(3) 0.1855(5) 0.3575(3) 0.0260(15) Uani 1 1 d . . . C16 C 0.2669(4) 0.1213(5) 0.4186(4) 0.0286(15) Uani 1 1 d . A . C17 C 0.3327(4) 0.1135(5) 0.4893(4) 0.0310(15) Uani 1 1 d . . . C18 C 0.3068(4) 0.1142(5) 0.5553(4) 0.0290(15) Uani 1 1 d . A . C19 C 0.2235(4) 0.1046(5) 0.5178(4) 0.0295(15) Uani 1 1 d . . . C20 C 0.1995(4) 0.1116(5) 0.4335(4) 0.0345(17) Uani 1 1 d . A . C21 C 0.1303(4) 0.1581(5) 0.3842(4) 0.0366(17) Uani 1 1 d . . . C22 C 0.1293(4) 0.2230(5) 0.3225(4) 0.0383(18) Uani 1 1 d . A . C23 C 0.1962(4) 0.2399(5) 0.3105(4) 0.0352(17) Uani 1 1 d . A . C24 C 0.2185(4) 0.3340(6) 0.2962(4) 0.0354(17) Uani 1 1 d . . . C25 C 0.3016(4) 0.3439(5) 0.3339(4) 0.0317(16) Uani 1 1 d . A . C26 C 0.3330(4) 0.4316(5) 0.3698(4) 0.0325(16) Uani 1 1 d . . . C27 C 0.2824(4) 0.5158(5) 0.3674(4) 0.0321(16) Uani 1 1 d . A . C28 C 0.2019(4) 0.5085(5) 0.3261(4) 0.0377(17) Uani 1 1 d . . . C29 C 0.1704(4) 0.4143(6) 0.2890(4) 0.0398(18) Uani 1 1 d . A . C30 C 0.1007(4) 0.3997(6) 0.3016(4) 0.0366(17) Uani 1 1 d . . . C31 C 0.0810(4) 0.3050(6) 0.3172(4) 0.0372(18) Uani 1 1 d . A . C32 C 0.0509(4) 0.2920(6) 0.3761(4) 0.044(2) Uani 1 1 d . . . C33 C 0.0822(4) 0.2005(6) 0.4194(5) 0.0396(18) Uani 1 1 d . A . C34 C 0.1044(4) 0.1931(5) 0.5003(4) 0.0378(17) Uani 1 1 d . . . C35 C 0.1759(4) 0.1446(5) 0.5494(4) 0.0362(17) Uani 1 1 d . A . C36 C 0.2081(4) 0.2012(5) 0.6220(4) 0.0320(16) Uani 1 1 d . . . C37 C 0.2876(4) 0.2128(5) 0.6576(4) 0.0305(16) Uani 1 1 d . A . C38 C 0.3375(4) 0.1676(5) 0.6244(4) 0.0358(17) Uani 1 1 d . . . C39 C 0.4106(4) 0.2291(5) 0.6561(4) 0.0304(15) Uani 1 1 d . A . C40 C 0.3898(4) 0.3246(5) 0.6863(3) 0.0291(15) Uani 1 1 d . . . C41 C 0.3202(4) 0.3084(5) 0.6930(4) 0.0326(16) Uani 1 1 d . A . C42 C 0.2709(4) 0.3824(6) 0.6917(4) 0.0371(17) Uani 1 1 d . . . C43 C 0.2886(4) 0.4831(5) 0.6749(4) 0.0323(16) Uani 1 1 d . A . C44 C 0.3568(4) 0.4976(6) 0.6648(4) 0.0408(19) Uani 1 1 d . . . C45 C 0.4096(4) 0.4182(5) 0.6738(4) 0.0351(17) Uani 1 1 d . A . C46 C 0.4581(4) 0.4493(5) 0.6295(4) 0.0311(16) Uani 1 1 d . . . C47 C 0.4057(3) 0.5269(5) 0.5705(4) 0.0269(15) Uani 1 1 d . A . C48 C 0.3555(4) 0.5632(5) 0.6021(4) 0.0336(16) Uani 1 1 d . A . C49 C 0.2871(4) 0.6098(5) 0.5533(4) 0.0312(16) Uani 1 1 d . . . C50 C 0.2670(4) 0.6144(5) 0.4694(4) 0.0328(16) Uani 1 1 d . A . C51 C 0.3129(4) 0.5710(5) 0.4406(4) 0.0334(16) Uani 1 1 d . . . C52 C 0.3854(4) 0.5270(5) 0.4890(4) 0.0319(16) Uani 1 1 d . A . C53 C 0.4047(4) 0.4481(5) 0.4447(4) 0.0274(15) Uani 1 1 d . A . C54 C 0.1833(4) 0.6040(5) 0.4281(4) 0.0363(17) Uani 1 1 d . . . C55 C 0.1542(4) 0.5912(5) 0.4891(4) 0.0405(18) Uani 1 1 d . A . C56 C 0.0920(4) 0.5258(6) 0.4739(4) 0.0384(18) Uani 1 1 d . . . C57 C 0.0606(4) 0.4702(6) 0.4012(4) 0.0356(17) Uani 1 1 d . A . C58 C 0.0897(4) 0.4834(6) 0.3433(4) 0.0370(17) Uani 1 1 d . A . C59 C 0.1517(4) 0.5521(5) 0.3584(4) 0.0342(16) Uani 1 1 d . A . C60 C 0.0409(4) 0.3725(6) 0.4191(4) 0.0363(17) Uani 1 1 d . A . C61 C 0.0622(4) 0.3648(6) 0.5030(4) 0.0428(19) Uani 1 1 d . . . C62 C 0.0948(4) 0.4613(6) 0.5379(4) 0.0418(19) Uani 1 1 d . A . C63 C 0.1572(4) 0.4644(6) 0.6122(4) 0.0373(17) Uani 1 1 d . . . C64 C 0.2179(4) 0.5331(5) 0.6259(4) 0.0315(16) Uani 1 1 d . A . C65 C 0.2172(4) 0.5941(5) 0.5659(4) 0.0336(16) Uani 1 1 d . A . C66 C 0.1884(4) 0.3732(6) 0.6531(4) 0.0356(17) Uani 1 1 d . A . C67 C 0.1586(4) 0.2822(6) 0.6204(4) 0.0371(17) Uani 1 1 d . A . C68 C 0.0959(4) 0.2776(6) 0.5448(4) 0.0407(18) Uani 1 1 d . A . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.023(2) 0.037(3) 0.036(3) -0.004(2) 0.016(2) -0.002(2) O2 0.026(3) 0.060(3) 0.035(3) 0.000(2) 0.010(2) -0.004(2) O3 0.035(3) 0.049(3) 0.032(3) -0.006(2) 0.016(2) -0.001(2) O4 0.028(3) 0.048(3) 0.032(3) 0.000(2) 0.017(2) 0.000(2) O5 0.034(3) 0.042(3) 0.041(3) 0.002(2) 0.017(2) 0.010(2) O6 0.043(4) 0.146(7) 0.046(4) 0.018(4) 0.006(3) 0.009(4) N1 0.019(3) 0.035(3) 0.028(3) 0.003(2) 0.010(2) 0.006(2) C1 0.059(8) 0.069(8) 0.073(9) 0.002(6) 0.029(6) -0.004(6) C2 0.050(5) 0.061(6) 0.058(5) 0.005(4) 0.021(4) -0.006(4) O7 0.035(4) 0.051(5) 0.047(4) -0.003(3) 0.020(3) 0.004(3) C1' 0.097(12) 0.104(13) 0.105(13) -0.004(9) 0.036(9) 0.000(9) C2' 0.084(8) 0.085(8) 0.090(8) -0.001(5) 0.033(5) -0.001(5) O7' 0.071(8) 0.075(8) 0.080(8) 0.001(4) 0.031(5) -0.002(4) C3 0.037(4) 0.055(5) 0.045(5) -0.001(4) 0.013(4) 0.002(4) C4 0.032(4) 0.038(4) 0.030(4) 0.003(3) 0.006(3) 0.002(3) C5 0.033(4) 0.052(5) 0.029(4) 0.008(3) 0.012(3) 0.004(3) C6 0.033(4) 0.045(4) 0.041(4) 0.006(3) 0.025(3) -0.006(3) C7 0.025(4) 0.039(4) 0.035(4) -0.006(3) 0.013(3) -0.009(3) C8 0.019(3) 0.039(4) 0.021(3) -0.004(3) 0.003(3) -0.001(3) C9 0.031(4) 0.035(4) 0.031(4) 0.009(3) 0.018(3) 0.010(3) C10 0.034(4) 0.034(4) 0.027(4) -0.004(3) 0.014(3) 0.005(3) C11 0.027(4) 0.037(4) 0.031(4) -0.008(3) 0.019(3) -0.009(3) C12 0.030(4) 0.030(4) 0.024(3) -0.012(3) 0.009(3) -0.006(3) C13 0.023(3) 0.032(4) 0.029(4) -0.005(3) 0.011(3) 0.003(3) C14 0.027(4) 0.049(4) 0.017(3) -0.003(3) 0.010(3) 0.003(3) C15 0.020(3) 0.034(4) 0.021(3) -0.011(3) 0.005(3) -0.008(3) C16 0.027(4) 0.032(4) 0.027(3) -0.006(3) 0.013(3) 0.000(3) C17 0.032(4) 0.025(4) 0.041(4) -0.003(3) 0.019(3) -0.002(3) C18 0.030(4) 0.029(4) 0.032(4) 0.000(3) 0.017(3) 0.001(3) C19 0.028(4) 0.037(4) 0.029(4) 0.003(3) 0.016(3) -0.004(3) C20 0.023(4) 0.026(4) 0.051(4) -0.002(3) 0.012(3) -0.010(3) C21 0.032(4) 0.038(4) 0.036(4) -0.004(3) 0.011(3) -0.011(3) C22 0.017(3) 0.047(5) 0.043(4) -0.010(3) 0.004(3) 0.001(3) C23 0.030(4) 0.050(5) 0.022(3) -0.008(3) 0.006(3) 0.004(3) C24 0.037(4) 0.048(5) 0.016(3) -0.005(3) 0.006(3) -0.001(3) C25 0.028(4) 0.051(5) 0.018(3) 0.001(3) 0.011(3) 0.003(3) C26 0.036(4) 0.040(4) 0.026(4) 0.000(3) 0.017(3) -0.003(3) C27 0.035(4) 0.031(4) 0.037(4) 0.006(3) 0.022(3) 0.002(3) C28 0.040(4) 0.046(5) 0.028(4) 0.010(3) 0.015(3) 0.010(3) C29 0.038(4) 0.053(5) 0.020(3) 0.004(3) 0.003(3) 0.002(4) C30 0.019(3) 0.058(5) 0.031(4) 0.001(3) 0.008(3) 0.006(3) C31 0.024(4) 0.054(5) 0.024(4) 0.000(3) 0.001(3) -0.006(3) C32 0.012(3) 0.071(6) 0.040(4) -0.008(4) 0.003(3) -0.004(3) C33 0.025(4) 0.045(5) 0.052(5) -0.004(4) 0.019(3) -0.010(3) C34 0.026(4) 0.042(4) 0.053(5) 0.004(4) 0.024(4) -0.010(3) C35 0.033(4) 0.044(4) 0.037(4) -0.007(3) 0.020(3) -0.007(3) C36 0.039(4) 0.033(4) 0.036(4) 0.011(3) 0.028(3) -0.006(3) C37 0.028(4) 0.044(4) 0.026(3) 0.006(3) 0.017(3) -0.002(3) C38 0.033(4) 0.042(4) 0.031(4) 0.009(3) 0.012(3) -0.003(3) C39 0.031(4) 0.041(4) 0.021(3) 0.000(3) 0.013(3) 0.003(3) C40 0.029(4) 0.039(4) 0.020(3) -0.001(3) 0.011(3) 0.005(3) C41 0.041(4) 0.031(4) 0.028(4) 0.002(3) 0.017(3) -0.002(3) C42 0.039(4) 0.051(5) 0.028(4) -0.002(3) 0.021(3) -0.003(4) C43 0.035(4) 0.049(4) 0.020(3) -0.012(3) 0.018(3) -0.008(3) C44 0.042(4) 0.055(5) 0.021(3) -0.018(3) 0.008(3) -0.009(4) C45 0.028(4) 0.045(4) 0.027(4) 0.003(3) 0.007(3) 0.003(3) C46 0.023(4) 0.040(4) 0.026(4) -0.016(3) 0.006(3) -0.007(3) C47 0.022(3) 0.033(4) 0.024(3) -0.004(3) 0.008(3) 0.000(3) C48 0.032(4) 0.034(4) 0.034(4) -0.009(3) 0.013(3) -0.005(3) C49 0.027(4) 0.029(4) 0.038(4) -0.001(3) 0.014(3) -0.004(3) C50 0.035(4) 0.026(4) 0.037(4) 0.005(3) 0.013(3) 0.002(3) C51 0.036(4) 0.036(4) 0.037(4) 0.000(3) 0.025(3) -0.004(3) C52 0.028(4) 0.033(4) 0.031(4) 0.004(3) 0.008(3) -0.004(3) C53 0.029(4) 0.038(4) 0.022(3) 0.006(3) 0.017(3) -0.001(3) C54 0.027(4) 0.040(4) 0.043(4) 0.009(3) 0.015(3) 0.009(3) C55 0.040(4) 0.038(4) 0.052(5) 0.003(3) 0.027(4) 0.008(3) C56 0.027(4) 0.048(5) 0.045(4) 0.001(4) 0.020(3) -0.001(3) C57 0.018(3) 0.053(5) 0.032(4) 0.004(3) 0.007(3) 0.008(3) C58 0.025(4) 0.054(5) 0.027(4) 0.010(3) 0.006(3) 0.000(3) C59 0.026(4) 0.038(4) 0.036(4) 0.008(3) 0.010(3) 0.008(3) C60 0.019(3) 0.057(5) 0.036(4) 0.003(3) 0.014(3) 0.002(3) C61 0.026(4) 0.059(5) 0.048(5) -0.014(4) 0.021(4) -0.008(4) C62 0.033(4) 0.056(5) 0.048(4) 0.003(4) 0.027(4) 0.013(4) C63 0.026(4) 0.051(5) 0.042(4) -0.010(3) 0.021(3) 0.003(3) C64 0.027(4) 0.045(4) 0.025(3) -0.015(3) 0.014(3) 0.003(3) C65 0.033(4) 0.028(4) 0.039(4) -0.005(3) 0.014(3) -0.001(3) C66 0.035(4) 0.052(5) 0.029(4) -0.001(3) 0.022(3) 0.004(3) C67 0.040(4) 0.054(5) 0.026(4) 0.005(3) 0.022(3) 0.000(4) C68 0.033(4) 0.047(5) 0.052(5) 0.003(4) 0.028(4) -0.006(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 O1 C53 1.212(7) . ? O2 C46 1.204(8) . ? O3 C39 1.214(8) . ? O4 C13 1.206(8) . ? O5 C10 1.216(8) . ? O6 C3 1.199(9) . ? N1 C13 1.384(8) . ? N1 C10 1.415(9) . ? N1 C7 1.428(8) . ? C1 C2 1.535(10) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 O7 1.442(9) . ? C2 H2B 0.9900 . ? C2 H2A 0.9900 . ? O7 C3 1.339(8) . ? C1' C2' 1.537(10) . ? C1' H1'A 0.9800 . ? C1' H1'B 0.9800 . ? C1' H1'C 0.9800 . ? C2' O7' 1.444(10) . ? C2' H2'A 0.9900 . ? C2' H2'B 0.9900 . ? O7' C3 1.340(10) . ? C3 C4 1.520(10) . ? C4 C9 1.394(9) . ? C4 C5 1.395(9) . ? C5 C6 1.382(9) . ? C5 H5 0.9500 . ? C6 C7 1.380(9) . ? C6 H6 0.9500 . ? C7 C8 1.384(9) . ? C8 C9 1.373(9) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.478(9) . ? C11 C12 1.408(9) . ? C11 C17 1.433(9) . ? C12 C14 1.398(9) . ? C12 C13 1.530(9) . ? C14 C15 1.430(9) . ? C14 C25 1.523(10) . ? C15 C16 1.411(9) . ? C15 C23 1.438(9) . ? C16 C17 1.400(9) . ? C16 C20 1.433(9) . ? C17 C18 1.497(9) . ? C18 C38 1.374(9) . ? C18 C19 1.461(9) . ? C19 C35 1.381(9) . ? C19 C20 1.439(9) . ? C20 C21 1.411(10) . ? C21 C22 1.434(10) . ? C21 C33 1.448(10) . ? C22 C23 1.407(10) . ? C22 C31 1.419(10) . ? C23 C24 1.398(10) . ? C24 C29 1.391(10) . ? C24 C25 1.459(9) . ? C25 C26 1.367(10) . ? C26 C27 1.481(9) . ? C26 C53 1.515(9) . ? C27 C28 1.415(10) . ? C27 C51 1.444(9) . ? C28 C59 1.450(10) . ? C28 C29 1.451(10) . ? C29 C30 1.460(10) . ? C30 C31 1.393(10) . ? C30 C58 1.432(10) . ? C31 C32 1.442(10) . ? C32 C60 1.404(10) . ? C32 C33 1.458(11) . ? C33 C34 1.385(10) . ? C34 C35 1.451(10) . ? C34 C68 1.453(10) . ? C35 C36 1.447(9) . ? C36 C37 1.398(9) . ? C36 C67 1.438(10) . ? C37 C41 1.463(9) . ? C37 C38 1.466(10) . ? C38 C39 1.522(9) . ? C39 C40 1.521(9) . ? C40 C45 1.363(10) . ? C40 C41 1.407(9) . ? C41 C42 1.367(10) . ? C42 C66 1.446(10) . ? C42 C43 1.462(10) . ? C43 C44 1.408(10) . ? C43 C64 1.449(9) . ? C44 C45 1.434(10) . ? C44 C48 1.454(10) . ? C45 C46 1.532(10) . ? C46 C47 1.547(9) . ? C47 C52 1.397(9) . ? C47 C48 1.404(9) . ? C48 C49 1.399(9) . ? C49 C50 1.443(9) . ? C49 C65 1.466(9) . ? C50 C51 1.337(9) . ? C50 C54 1.472(9) . ? C51 C52 1.435(9) . ? C52 C53 1.481(9) . ? C54 C59 1.372(10) . ? C54 C55 1.463(10) . ? C55 C56 1.415(10) . ? C55 C65 1.439(10) . ? C56 C57 1.440(10) . ? C56 C62 1.454(10) . ? C57 C58 1.410(9) . ? C57 C60 1.444(10) . ? C58 C59 1.440(10) . ? C60 C61 1.443(10) . ? C61 C68 1.409(11) . ? C61 C62 1.472(11) . ? C62 C63 1.406(10) . ? C63 C64 1.424(10) . ? C63 C66 1.439(10) . ? C64 C65 1.379(9) . ? C66 C67 1.382(10) . ? C67 C68 1.424(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 N1 C10 112.8(5) . . ? C13 N1 C7 124.5(6) . . ? C10 N1 C7 121.8(5) . . ? O7 C2 C1 109.6(11) . . ? O7 C2 H2B 109.8 . . ? C1 C2 H2B 109.8 . . ? O7 C2 H2A 109.8 . . ? C1 C2 H2A 109.8 . . ? H2B C2 H2A 108.2 . . ? C3 O7 C2 117.2(10) . . ? C2' C1' H1'A 109.5 . . ? C2' C1' H1'B 109.5 . . ? H1'A C1' H1'B 109.5 . . ? C2' C1' H1'C 109.5 . . ? H1'A C1' H1'C 109.5 . . ? H1'B C1' H1'C 109.5 . . ? O7' C2' C1' 103(2) . . ? O7' C2' H2'A 111.2 . . ? C1' C2' H2'A 111.2 . . ? O7' C2' H2'B 111.2 . . ? C1' C2' H2'B 111.2 . . ? H2'A C2' H2'B 109.2 . . ? C3 O7' C2' 110.6(19) . . ? O6 C3 O7 126.5(8) . . ? O6 C3 O7' 124.7(13) . . ? O7 C3 O7' 19.4(13) . . ? O6 C3 C4 122.8(7) . . ? O7 C3 C4 110.1(7) . . ? O7' C3 C4 111.4(12) . . ? C9 C4 C5 120.5(6) . . ? C9 C4 C3 121.6(6) . . ? C5 C4 C3 117.9(6) . . ? C6 C5 C4 119.6(7) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C7 C6 C5 118.9(7) . . ? C7 C6 H6 120.5 . . ? C5 C6 H6 120.5 . . ? C6 C7 C8 121.9(6) . . ? C6 C7 N1 115.9(6) . . ? C8 C7 N1 122.1(6) . . ? C9 C8 C7 119.3(6) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C8 C9 C4 119.7(6) . . ? C8 C9 H9 120.1 . . ? C4 C9 H9 120.1 . . ? O5 C10 N1 126.6(6) . . ? O5 C10 C11 128.1(7) . . ? N1 C10 C11 104.9(5) . . ? C12 C11 C17 119.0(6) . . ? C12 C11 C10 109.5(5) . . ? C17 C11 C10 131.5(6) . . ? C14 C12 C11 122.3(6) . . ? C14 C12 C13 131.4(6) . . ? C11 C12 C13 106.3(5) . . ? O4 C13 N1 126.5(6) . . ? O4 C13 C12 128.1(6) . . ? N1 C13 C12 105.3(5) . . ? C12 C14 C15 114.2(6) . . ? C12 C14 C25 135.9(6) . . ? C15 C14 C25 105.2(5) . . ? C16 C15 C14 120.0(6) . . ? C16 C15 C23 121.4(6) . . ? C14 C15 C23 110.4(6) . . ? C17 C16 C15 121.2(6) . . ? C17 C16 C20 110.3(6) . . ? C15 C16 C20 118.4(6) . . ? C16 C17 C11 114.7(6) . . ? C16 C17 C18 107.0(6) . . ? C11 C17 C18 134.3(6) . . ? C38 C18 C19 117.0(6) . . ? C38 C18 C17 127.4(6) . . ? C19 C18 C17 106.0(5) . . ? C35 C19 C20 117.7(6) . . ? C35 C19 C18 123.1(6) . . ? C20 C19 C18 108.0(5) . . ? C21 C20 C16 121.0(6) . . ? C21 C20 C19 121.9(6) . . ? C16 C20 C19 107.8(6) . . ? C20 C21 C22 119.2(6) . . ? C20 C21 C33 119.1(6) . . ? C22 C21 C33 108.6(6) . . ? C23 C22 C31 118.3(7) . . ? C23 C22 C21 120.8(6) . . ? C31 C22 C21 108.9(6) . . ? C24 C23 C22 123.1(6) . . ? C24 C23 C15 107.7(6) . . ? C22 C23 C15 118.8(6) . . ? C29 C24 C23 118.7(7) . . ? C29 C24 C25 121.7(7) . . ? C23 C24 C25 110.5(6) . . ? C26 C25 C24 119.1(6) . . ? C26 C25 C14 125.5(6) . . ? C24 C25 C14 105.0(6) . . ? C25 C26 C27 119.7(6) . . ? C25 C26 C53 128.6(6) . . ? C27 C26 C53 104.5(6) . . ? C28 C27 C51 118.3(6) . . ? C28 C27 C26 121.2(6) . . ? C51 C27 C26 111.1(6) . . ? C27 C28 C59 120.6(6) . . ? C27 C28 C29 117.8(6) . . ? C59 C28 C29 109.4(7) . . ? C24 C29 C28 120.3(7) . . ? C24 C29 C30 119.6(7) . . ? C28 C29 C30 105.8(6) . . ? C31 C30 C58 119.7(6) . . ? C31 C30 C29 120.0(6) . . ? C58 C30 C29 109.2(6) . . ? C30 C31 C22 120.1(7) . . ? C30 C31 C32 119.7(7) . . ? C22 C31 C32 107.8(7) . . ? C60 C32 C31 121.8(7) . . ? C60 C32 C33 117.5(7) . . ? C31 C32 C33 108.5(7) . . ? C34 C33 C21 119.4(7) . . ? C34 C33 C32 122.0(7) . . ? C21 C33 C32 106.2(6) . . ? C33 C34 C35 120.1(6) . . ? C33 C34 C68 120.2(7) . . ? C35 C34 C68 107.1(6) . . ? C19 C35 C36 119.9(6) . . ? C19 C35 C34 121.8(6) . . ? C36 C35 C34 106.1(6) . . ? C37 C36 C67 120.4(6) . . ? C37 C36 C35 117.6(6) . . ? C67 C36 C35 110.9(6) . . ? C36 C37 C41 119.4(6) . . ? C36 C37 C38 121.8(6) . . ? C41 C37 C38 108.8(6) . . ? C18 C38 C37 120.5(6) . . ? C18 C38 C39 128.2(6) . . ? C37 C38 C39 105.5(6) . . ? O3 C39 C40 126.2(6) . . ? O3 C39 C38 127.9(6) . . ? C40 C39 C38 105.3(6) . . ? C45 C40 C41 119.9(6) . . ? C45 C40 C39 125.9(6) . . ? C41 C40 C39 107.6(6) . . ? C42 C41 C40 124.0(6) . . ? C42 C41 C37 117.9(6) . . ? C40 C41 C37 110.0(6) . . ? C41 C42 C66 123.6(7) . . ? C41 C42 C43 117.4(6) . . ? C66 C42 C43 106.1(6) . . ? C44 C43 C64 122.1(6) . . ? C44 C43 C42 117.8(6) . . ? C64 C43 C42 109.0(6) . . ? C43 C44 C45 122.0(7) . . ? C43 C44 C48 118.7(6) . . ? C45 C44 C48 108.9(6) . . ? C40 C45 C44 118.5(6) . . ? C40 C45 C46 128.1(6) . . ? C44 C45 C46 106.8(6) . . ? O2 C46 C45 129.7(7) . . ? O2 C46 C47 128.6(6) . . ? C45 C46 C47 101.8(5) . . ? C52 C47 C48 121.2(6) . . ? C52 C47 C46 125.3(6) . . ? C48 C47 C46 107.2(5) . . ? C49 C48 C47 120.5(6) . . ? C49 C48 C44 119.5(6) . . ? C47 C48 C44 109.6(6) . . ? C48 C49 C50 118.7(6) . . ? C48 C49 C65 120.5(6) . . ? C50 C49 C65 108.9(6) . . ? C51 C50 C49 119.0(6) . . ? C51 C50 C54 120.4(6) . . ? C49 C50 C54 107.8(6) . . ? C50 C51 C52 123.9(6) . . ? C50 C51 C27 121.5(7) . . ? C52 C51 C27 106.8(6) . . ? C47 C52 C51 116.4(6) . . ? C47 C52 C53 125.3(6) . . ? C51 C52 C53 110.4(6) . . ? O1 C53 C52 128.5(6) . . ? O1 C53 C26 124.3(6) . . ? C52 C53 C26 106.0(5) . . ? C59 C54 C55 120.6(7) . . ? C59 C54 C50 120.1(6) . . ? C55 C54 C50 106.8(6) . . ? C56 C55 C65 120.6(7) . . ? C56 C55 C54 118.5(7) . . ? C65 C55 C54 109.3(6) . . ? C55 C56 C57 120.2(6) . . ? C55 C56 C62 117.7(7) . . ? C57 C56 C62 108.3(6) . . ? C58 C57 C56 120.2(6) . . ? C58 C57 C60 120.8(7) . . ? C56 C57 C60 107.9(6) . . ? C57 C58 C30 120.3(7) . . ? C57 C58 C59 119.2(6) . . ? C30 C58 C59 108.5(6) . . ? C54 C59 C58 121.2(6) . . ? C54 C59 C28 119.0(6) . . ? C58 C59 C28 107.1(6) . . ? C32 C60 C61 120.9(7) . . ? C32 C60 C57 117.6(6) . . ? C61 C60 C57 109.2(6) . . ? C68 C61 C60 121.0(7) . . ? C68 C61 C62 118.6(7) . . ? C60 C61 C62 106.9(7) . . ? C63 C62 C56 120.9(7) . . ? C63 C62 C61 119.5(7) . . ? C56 C62 C61 107.7(7) . . ? C62 C63 C64 119.8(7) . . ? C62 C63 C66 119.5(7) . . ? C64 C63 C66 109.2(6) . . ? C65 C64 C63 120.5(6) . . ? C65 C64 C43 118.6(6) . . ? C63 C64 C43 107.1(6) . . ? C64 C65 C55 120.6(6) . . ? C64 C65 C49 120.6(6) . . ? C55 C65 C49 107.1(6) . . ? C67 C66 C63 121.2(7) . . ? C67 C66 C42 117.6(7) . . ? C63 C66 C42 108.6(6) . . ? C66 C67 C68 120.0(7) . . ? C66 C67 C36 120.9(7) . . ? C68 C67 C36 105.6(6) . . ? C61 C68 C67 121.0(7) . . ? C61 C68 C34 118.2(7) . . ? C67 C68 C34 110.4(7) . . ? 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 C1 C2 O7 C3 103.7(19) . . . . ? C1' C2' O7' C3 -177(3) . . . . ? C2 O7 C3 O6 5.6(17) . . . . ? C2 O7 C3 O7' -86(4) . . . . ? C2 O7 C3 C4 176.2(9) . . . . ? C2' O7' C3 O6 -6(3) . . . . ? C2' O7' C3 O7 96(5) . . . . ? C2' O7' C3 C4 -174.3(19) . . . . ? O6 C3 C4 C9 -169.5(8) . . . . ? O7 C3 C4 C9 19.4(11) . . . . ? O7' C3 C4 C9 -1.3(17) . . . . ? O6 C3 C4 C5 9.5(12) . . . . ? O7 C3 C4 C5 -161.5(9) . . . . ? O7' C3 C4 C5 177.7(15) . . . . ? C9 C4 C5 C6 -2.8(11) . . . . ? C3 C4 C5 C6 178.2(7) . . . . ? C4 C5 C6 C7 3.6(11) . . . . ? C5 C6 C7 C8 -2.6(11) . . . . ? C5 C6 C7 N1 180.0(6) . . . . ? C13 N1 C7 C6 129.0(7) . . . . ? C10 N1 C7 C6 -62.6(8) . . . . ? C13 N1 C7 C8 -48.4(9) . . . . ? C10 N1 C7 C8 120.0(7) . . . . ? C6 C7 C8 C9 0.6(10) . . . . ? N1 C7 C8 C9 177.9(6) . . . . ? C7 C8 C9 C4 0.3(10) . . . . ? C5 C4 C9 C8 0.8(10) . . . . ? C3 C4 C9 C8 179.8(7) . . . . ? C13 N1 C10 O5 162.3(6) . . . . ? C7 N1 C10 O5 -7.3(10) . . . . ? C13 N1 C10 C11 -11.2(7) . . . . ? C7 N1 C10 C11 179.1(5) . . . . ? O5 C10 C11 C12 -166.7(6) . . . . ? N1 C10 C11 C12 6.8(7) . . . . ? O5 C10 C11 C17 12.9(12) . . . . ? N1 C10 C11 C17 -173.6(7) . . . . ? C17 C11 C12 C14 1.6(10) . . . . ? C10 C11 C12 C14 -178.7(6) . . . . ? C17 C11 C12 C13 179.8(6) . . . . ? C10 C11 C12 C13 -0.6(7) . . . . ? C10 N1 C13 O4 -165.2(6) . . . . ? C7 N1 C13 O4 4.1(10) . . . . ? C10 N1 C13 C12 10.9(7) . . . . ? C7 N1 C13 C12 -179.8(6) . . . . ? C14 C12 C13 O4 -12.1(12) . . . . ? C11 C12 C13 O4 170.0(6) . . . . ? C14 C12 C13 N1 171.9(6) . . . . ? C11 C12 C13 N1 -6.0(7) . . . . ? C11 C12 C14 C15 -23.6(9) . . . . ? C13 C12 C14 C15 158.8(6) . . . . ? C11 C12 C14 C25 127.7(8) . . . . ? C13 C12 C14 C25 -50.0(11) . . . . ? C12 C14 C15 C16 21.3(9) . . . . ? C25 C14 C15 C16 -138.4(6) . . . . ? C12 C14 C15 C23 170.2(5) . . . . ? C25 C14 C15 C23 10.5(7) . . . . ? C14 C15 C16 C17 2.9(9) . . . . ? C23 C15 C16 C17 -142.6(6) . . . . ? C14 C15 C16 C20 145.0(6) . . . . ? C23 C15 C16 C20 -0.5(9) . . . . ? C15 C16 C17 C11 -24.9(9) . . . . ? C20 C16 C17 C11 -169.7(6) . . . . ? C15 C16 C17 C18 136.0(6) . . . . ? C20 C16 C17 C18 -8.8(7) . . . . ? C12 C11 C17 C16 22.7(9) . . . . ? C10 C11 C17 C16 -156.8(7) . . . . ? C12 C11 C17 C18 -131.3(8) . . . . ? C10 C11 C17 C18 49.1(12) . . . . ? C16 C17 C18 C38 -134.5(7) . . . . ? C11 C17 C18 C38 21.0(12) . . . . ? C16 C17 C18 C19 9.9(7) . . . . ? C11 C17 C18 C19 165.4(7) . . . . ? C38 C18 C19 C35 -1.3(10) . . . . ? C17 C18 C19 C35 -150.1(7) . . . . ? C38 C18 C19 C20 141.3(6) . . . . ? C17 C18 C19 C20 -7.4(7) . . . . ? C17 C16 C20 C21 151.4(6) . . . . ? C15 C16 C20 C21 5.5(9) . . . . ? C17 C16 C20 C19 4.2(7) . . . . ? C15 C16 C20 C19 -141.7(6) . . . . ? C35 C19 C20 C21 0.5(10) . . . . ? C18 C19 C20 C21 -144.5(6) . . . . ? C35 C19 C20 C16 147.3(6) . . . . ? C18 C19 C20 C16 2.3(7) . . . . ? C16 C20 C21 C22 -5.5(10) . . . . ? C19 C20 C21 C22 137.1(7) . . . . ? C16 C20 C21 C33 -142.2(7) . . . . ? C19 C20 C21 C33 0.3(10) . . . . ? C20 C21 C22 C23 0.4(10) . . . . ? C33 C21 C22 C23 141.2(7) . . . . ? C20 C21 C22 C31 -141.4(6) . . . . ? C33 C21 C22 C31 -0.6(8) . . . . ? C31 C22 C23 C24 2.1(10) . . . . ? C21 C22 C23 C24 -136.3(7) . . . . ? C31 C22 C23 C15 142.8(6) . . . . ? C21 C22 C23 C15 4.4(10) . . . . ? C16 C15 C23 C24 141.7(6) . . . . ? C14 C15 C23 C24 -6.6(7) . . . . ? C16 C15 C23 C22 -4.4(9) . . . . ? C14 C15 C23 C22 -152.8(6) . . . . ? C22 C23 C24 C29 -3.6(10) . . . . ? C15 C23 C24 C29 -148.0(6) . . . . ? C22 C23 C24 C25 143.9(6) . . . . ? C15 C23 C24 C25 -0.5(7) . . . . ? C29 C24 C25 C26 6.3(9) . . . . ? C23 C24 C25 C26 -140.1(6) . . . . ? C29 C24 C25 C14 153.1(6) . . . . ? C23 C24 C25 C14 6.7(7) . . . . ? C12 C14 C25 C26 -19.2(11) . . . . ? C15 C14 C25 C26 133.8(7) . . . . ? C12 C14 C25 C24 -163.3(7) . . . . ? C15 C14 C25 C24 -10.3(6) . . . . ? C24 C25 C26 C27 -2.0(9) . . . . ? C14 C25 C26 C27 -141.5(7) . . . . ? C24 C25 C26 C53 143.4(7) . . . . ? C14 C25 C26 C53 3.9(11) . . . . ? C25 C26 C27 C28 -2.4(10) . . . . ? C53 C26 C27 C28 -155.2(6) . . . . ? C25 C26 C27 C51 143.5(6) . . . . ? C53 C26 C27 C51 -9.2(7) . . . . ? C51 C27 C28 C59 -2.5(10) . . . . ? C26 C27 C28 C59 141.1(7) . . . . ? C51 C27 C28 C29 -140.8(6) . . . . ? C26 C27 C28 C29 2.7(10) . . . . ? C23 C24 C29 C28 137.7(7) . . . . ? C25 C24 C29 C28 -6.0(10) . . . . ? C23 C24 C29 C30 3.9(9) . . . . ? C25 C24 C29 C30 -139.9(7) . . . . ? C27 C28 C29 C24 1.5(10) . . . . ? C59 C28 C29 C24 -141.1(7) . . . . ? C27 C28 C29 C30 140.9(6) . . . . ? C59 C28 C29 C30 -1.8(7) . . . . ? C24 C29 C30 C31 -2.8(10) . . . . ? C28 C29 C30 C31 -142.5(6) . . . . ? C24 C29 C30 C58 141.0(6) . . . . ? C28 C29 C30 C58 1.3(7) . . . . ? C58 C30 C31 C22 -138.7(7) . . . . ? C29 C30 C31 C22 1.3(10) . . . . ? C58 C30 C31 C32 -1.1(9) . . . . ? C29 C30 C31 C32 138.9(7) . . . . ? C23 C22 C31 C30 -0.9(10) . . . . ? C21 C22 C31 C30 142.0(6) . . . . ? C23 C22 C31 C32 -143.0(6) . . . . ? C21 C22 C31 C32 -0.1(7) . . . . ? C30 C31 C32 C60 -0.2(10) . . . . ? C22 C31 C32 C60 142.1(7) . . . . ? C30 C31 C32 C33 -141.5(6) . . . . ? C22 C31 C32 C33 0.7(8) . . . . ? C20 C21 C33 C34 -1.0(10) . . . . ? C22 C21 C33 C34 -141.9(7) . . . . ? C20 C21 C33 C32 141.9(6) . . . . ? C22 C21 C33 C32 1.0(8) . . . . ? C60 C32 C33 C34 -2.6(10) . . . . ? C31 C32 C33 C34 140.7(7) . . . . ? C60 C32 C33 C21 -144.3(6) . . . . ? C31 C32 C33 C21 -1.1(8) . . . . ? C21 C33 C34 C35 0.9(10) . . . . ? C32 C33 C34 C35 -136.0(7) . . . . ? C21 C33 C34 C68 137.9(7) . . . . ? C32 C33 C34 C68 0.9(10) . . . . ? C20 C19 C35 C36 -137.7(7) . . . . ? C18 C19 C35 C36 1.6(11) . . . . ? C20 C19 C35 C34 -0.6(10) . . . . ? C18 C19 C35 C34 138.7(7) . . . . ? C33 C34 C35 C19 -0.1(11) . . . . ? C68 C34 C35 C19 -142.0(7) . . . . ? C33 C34 C35 C36 142.0(7) . . . . ? C68 C34 C35 C36 0.1(7) . . . . ? C19 C35 C36 C37 -0.2(10) . . . . ? C34 C35 C36 C37 -143.2(6) . . . . ? C19 C35 C36 C67 144.0(7) . . . . ? C34 C35 C36 C67 1.0(7) . . . . ? C67 C36 C37 C41 -0.4(9) . . . . ? C35 C36 C37 C41 140.3(6) . . . . ? C67 C36 C37 C38 -142.1(7) . . . . ? C35 C36 C37 C38 -1.4(10) . . . . ? C19 C18 C38 C37 -0.3(9) . . . . ? C17 C18 C38 C37 140.8(7) . . . . ? C19 C18 C38 C39 -149.5(7) . . . . ? C17 C18 C38 C39 -8.4(12) . . . . ? C36 C37 C38 C18 1.7(10) . . . . ? C41 C37 C38 C18 -143.6(6) . . . . ? C36 C37 C38 C39 157.0(6) . . . . ? C41 C37 C38 C39 11.7(7) . . . . ? C18 C38 C39 O3 -35.0(11) . . . . ? C37 C38 C39 O3 172.3(6) . . . . ? C18 C38 C39 C40 136.3(7) . . . . ? C37 C38 C39 C40 -16.4(6) . . . . ? O3 C39 C40 C45 35.9(10) . . . . ? C38 C39 C40 C45 -135.6(6) . . . . ? O3 C39 C40 C41 -172.9(6) . . . . ? C38 C39 C40 C41 15.6(7) . . . . ? C45 C40 C41 C42 -3.3(10) . . . . ? C39 C40 C41 C42 -156.6(6) . . . . ? C45 C40 C41 C37 144.6(6) . . . . ? C39 C40 C41 C37 -8.7(7) . . . . ? C36 C37 C41 C42 1.8(9) . . . . ? C38 C37 C41 C42 148.0(6) . . . . ? C36 C37 C41 C40 -148.3(6) . . . . ? C38 C37 C41 C40 -2.0(7) . . . . ? C40 C41 C42 C66 141.8(7) . . . . ? C37 C41 C42 C66 -3.8(10) . . . . ? C40 C41 C42 C43 5.8(10) . . . . ? C37 C41 C42 C43 -139.7(6) . . . . ? C41 C42 C43 C44 -2.8(9) . . . . ? C66 C42 C43 C44 -145.7(6) . . . . ? C41 C42 C43 C64 142.0(6) . . . . ? C66 C42 C43 C64 -0.9(7) . . . . ? C64 C43 C44 C45 -142.5(7) . . . . ? C42 C43 C44 C45 -2.6(9) . . . . ? C64 C43 C44 C48 -1.4(9) . . . . ? C42 C43 C44 C48 138.5(6) . . . . ? C41 C40 C45 C44 -2.3(9) . . . . ? C39 C40 C45 C44 145.7(6) . . . . ? C41 C40 C45 C46 -149.8(7) . . . . ? C39 C40 C45 C46 -1.8(11) . . . . ? C43 C44 C45 C40 5.2(10) . . . . ? C48 C44 C45 C40 -139.2(6) . . . . ? C43 C44 C45 C46 159.0(6) . . . . ? C48 C44 C45 C46 14.6(7) . . . . ? C40 C45 C46 O2 -52.4(11) . . . . ? C44 C45 C46 O2 157.2(7) . . . . ? C40 C45 C46 C47 128.0(7) . . . . ? C44 C45 C46 C47 -22.5(6) . . . . ? O2 C46 C47 C52 51.4(10) . . . . ? C45 C46 C47 C52 -129.0(7) . . . . ? O2 C46 C47 C48 -156.7(7) . . . . ? C45 C46 C47 C48 23.0(6) . . . . ? C52 C47 C48 C49 -6.6(10) . . . . ? C46 C47 C48 C49 -160.0(6) . . . . ? C52 C47 C48 C44 138.0(6) . . . . ? C46 C47 C48 C44 -15.3(7) . . . . ? C43 C44 C48 C49 -0.2(9) . . . . ? C45 C44 C48 C49 145.6(6) . . . . ? C43 C44 C48 C47 -145.2(6) . . . . ? C45 C44 C48 C47 0.5(8) . . . . ? C47 C48 C49 C50 3.6(10) . . . . ? C44 C48 C49 C50 -137.5(7) . . . . ? C47 C48 C49 C65 142.2(7) . . . . ? C44 C48 C49 C65 1.0(9) . . . . ? C48 C49 C50 C51 2.4(10) . . . . ? C65 C49 C50 C51 -140.5(7) . . . . ? C48 C49 C50 C54 144.2(6) . . . . ? C65 C49 C50 C54 1.3(8) . . . . ? C49 C50 C51 C52 -5.8(11) . . . . ? C54 C50 C51 C52 -142.8(7) . . . . ? C49 C50 C51 C27 139.1(7) . . . . ? C54 C50 C51 C27 2.1(10) . . . . ? C28 C27 C51 C50 0.1(10) . . . . ? C26 C27 C51 C50 -146.8(7) . . . . ? C28 C27 C51 C52 150.2(6) . . . . ? C26 C27 C51 C52 3.2(7) . . . . ? C48 C47 C52 C51 3.4(10) . . . . ? C46 C47 C52 C51 151.7(6) . . . . ? C48 C47 C52 C53 -142.4(7) . . . . ? C46 C47 C52 C53 6.0(11) . . . . ? C50 C51 C52 C47 3.0(10) . . . . ? C27 C51 C52 C47 -146.2(6) . . . . ? C50 C51 C52 C53 153.6(7) . . . . ? C27 C51 C52 C53 4.4(7) . . . . ? C47 C52 C53 O1 -30.6(11) . . . . ? C51 C52 C53 O1 -178.1(6) . . . . ? C47 C52 C53 C26 137.4(7) . . . . ? C51 C52 C53 C26 -10.1(7) . . . . ? C25 C26 C53 O1 30.6(11) . . . . ? C27 C26 C53 O1 180.0(6) . . . . ? C25 C26 C53 C52 -138.0(7) . . . . ? C27 C26 C53 C52 11.4(6) . . . . ? C51 C50 C54 C59 -2.0(10) . . . . ? C49 C50 C54 C59 -143.2(6) . . . . ? C51 C50 C54 C55 140.1(7) . . . . ? C49 C50 C54 C55 -1.0(8) . . . . ? C59 C54 C55 C56 -1.2(10) . . . . ? C50 C54 C55 C56 -143.2(7) . . . . ? C59 C54 C55 C65 142.3(6) . . . . ? C50 C54 C55 C65 0.3(8) . . . . ? C65 C55 C56 C57 -136.7(7) . . . . ? C54 C55 C56 C57 2.7(10) . . . . ? C65 C55 C56 C62 -0.9(10) . . . . ? C54 C55 C56 C62 138.4(7) . . . . ? C55 C56 C57 C58 -2.5(10) . . . . ? C62 C56 C57 C58 -141.9(7) . . . . ? C55 C56 C57 C60 141.7(7) . . . . ? C62 C56 C57 C60 2.3(8) . . . . ? C56 C57 C58 C30 139.1(7) . . . . ? C60 C57 C58 C30 -0.5(9) . . . . ? C56 C57 C58 C59 0.9(10) . . . . ? C60 C57 C58 C59 -138.7(7) . . . . ? C31 C30 C58 C57 1.4(9) . . . . ? C29 C30 C58 C57 -142.5(6) . . . . ? C31 C30 C58 C59 143.6(6) . . . . ? C29 C30 C58 C59 -0.3(8) . . . . ? C55 C54 C59 C58 -0.4(10) . . . . ? C50 C54 C59 C58 136.6(7) . . . . ? C55 C54 C59 C28 -137.3(7) . . . . ? C50 C54 C59 C28 -0.3(10) . . . . ? C57 C58 C59 C54 0.6(10) . . . . ? C30 C58 C59 C54 -142.1(7) . . . . ? C57 C58 C59 C28 141.9(7) . . . . ? C30 C58 C59 C28 -0.8(7) . . . . ? C27 C28 C59 C54 2.5(10) . . . . ? C29 C28 C59 C54 144.0(7) . . . . ? C27 C28 C59 C58 -139.8(7) . . . . ? C29 C28 C59 C58 1.6(7) . . . . ? C31 C32 C60 C61 -137.1(7) . . . . ? C33 C32 C60 C61 1.0(10) . . . . ? C31 C32 C60 C57 1.1(9) . . . . ? C33 C32 C60 C57 139.2(7) . . . . ? C58 C57 C60 C32 -0.8(9) . . . . ? C56 C57 C60 C32 -144.8(6) . . . . ? C58 C57 C60 C61 142.0(6) . . . . ? C56 C57 C60 C61 -2.0(8) . . . . ? C32 C60 C61 C68 2.2(10) . . . . ? C57 C60 C61 C68 -139.1(7) . . . . ? C32 C60 C61 C62 142.3(7) . . . . ? C57 C60 C61 C62 1.0(8) . . . . ? C55 C56 C62 C63 0.2(10) . . . . ? C57 C56 C62 C63 140.8(7) . . . . ? C55 C56 C62 C61 -142.3(7) . . . . ? C57 C56 C62 C61 -1.7(8) . . . . ? C68 C61 C62 C63 -1.4(10) . . . . ? C60 C61 C62 C63 -142.6(6) . . . . ? C68 C61 C62 C56 141.7(7) . . . . ? C60 C61 C62 C56 0.4(8) . . . . ? C56 C62 C63 C64 1.4(10) . . . . ? C61 C62 C63 C64 139.6(7) . . . . ? C56 C62 C63 C66 -138.1(7) . . . . ? C61 C62 C63 C66 0.0(10) . . . . ? C62 C63 C64 C65 -2.3(10) . . . . ? C66 C63 C64 C65 140.9(6) . . . . ? C62 C63 C64 C43 -142.0(6) . . . . ? C66 C63 C64 C43 1.3(7) . . . . ? C44 C43 C64 C65 2.3(9) . . . . ? C42 C43 C64 C65 -140.7(6) . . . . ? C44 C43 C64 C63 142.8(6) . . . . ? C42 C43 C64 C63 -0.2(7) . . . . ? C63 C64 C65 C55 1.6(10) . . . . ? C43 C64 C65 C55 136.8(7) . . . . ? C63 C64 C65 C49 -136.6(7) . . . . ? C43 C64 C65 C49 -1.4(9) . . . . ? C56 C55 C65 C64 0.0(10) . . . . ? C54 C55 C65 C64 -142.6(7) . . . . ? C56 C55 C65 C49 143.2(7) . . . . ? C54 C55 C65 C49 0.5(8) . . . . ? C48 C49 C65 C64 -0.1(10) . . . . ? C50 C49 C65 C64 142.0(6) . . . . ? C48 C49 C65 C55 -143.2(6) . . . . ? C50 C49 C65 C55 -1.1(7) . . . . ? C62 C63 C66 C67 0.6(10) . . . . ? C64 C63 C66 C67 -142.8(7) . . . . ? C62 C63 C66 C42 141.5(6) . . . . ? C64 C63 C66 C42 -1.9(8) . . . . ? C41 C42 C66 C67 4.2(10) . . . . ? C43 C42 C66 C67 144.2(6) . . . . ? C41 C42 C66 C63 -138.3(7) . . . . ? C43 C42 C66 C63 1.7(7) . . . . ? C63 C66 C67 C68 0.1(10) . . . . ? C42 C66 C67 C68 -137.5(7) . . . . ? C63 C66 C67 C36 135.0(7) . . . . ? C42 C66 C67 C36 -2.6(9) . . . . ? C37 C36 C67 C66 0.8(9) . . . . ? C35 C36 C67 C66 -142.2(6) . . . . ? C37 C36 C67 C68 141.3(6) . . . . ? C35 C36 C67 C68 -1.8(7) . . . . ? C60 C61 C68 C67 137.8(7) . . . . ? C62 C61 C68 C67 2.1(10) . . . . ? C60 C61 C68 C34 -3.8(10) . . . . ? C62 C61 C68 C34 -139.4(7) . . . . ? C66 C67 C68 C61 -1.5(11) . . . . ? C36 C67 C68 C61 -142.4(7) . . . . ? C66 C67 C68 C34 142.7(7) . . . . ? C36 C67 C68 C34 1.8(8) . . . . ? C33 C34 C68 C61 2.3(10) . . . . ? C35 C34 C68 C61 144.1(7) . . . . ? C33 C34 C68 C67 -143.1(7) . . . . ? C35 C34 C68 C67 -1.2(8) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.475 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.109 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 0.500 0.115 0.250 386 186 ' ' 2 0.500 -0.116 0.750 386 186 ' ' 3 1.000 0.042 0.250 15 7 ' ' 4 0.747 0.356 0.006 26 6 ' ' 5 0.253 0.356 0.494 26 6 ' ' 6 0.000 0.352 0.750 30 7 ' ' 7 0.253 0.644 -0.006 26 5 ' ' 8 0.747 0.644 0.506 26 5 ' ' 9 0.000 0.648 0.250 30 6 ' ' 10 0.000 0.957 0.750 16 5 ' ' _platon_squeeze_details ; ;