# Electronic Supplementary Material (ESI) for Chemical Communications # 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_datam _audit_creation_date 2013-11-01 _audit_creation_method ; Olex2 1.2 (compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C Cl2, C69 H64 O' _chemical_formula_sum 'C70 H64 Cl2 O' _chemical_formula_weight 992.11 _chemical_melting_point ? 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 14.7164(10) _cell_length_b 17.2279(12) _cell_length_c 22.4826(16) _cell_angle_alpha 90.00 _cell_angle_beta 103.120(2) _cell_angle_gamma 90.00 _cell_volume 5551.3(7) _cell_formula_units_Z 4 _cell_measurement_reflns_used 0 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 0.000 _cell_measurement_theta_min 0.000 _exptl_absorpt_coefficient_mu 0.161 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_crystal_colour ? _exptl_crystal_density_diffrn 1.187 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description ? _exptl_crystal_F_000 2104 _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.1262 _diffrn_reflns_av_unetI/netI 0.1020 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 58920 _diffrn_reflns_theta_full 25.12 _diffrn_reflns_theta_max 25.12 _diffrn_reflns_theta_min 1.42 _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _reflns_number_gt 5659 _reflns_number_total 9847 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'SAINT v6.02A (Bruker, 2001)' _computing_data_collection ? _computing_data_reduction 'SAINT v6.02A (Bruker, 2001)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELX, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 0.465 _refine_diff_density_min -0.816 _refine_diff_density_rms 0.072 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 670 _refine_ls_number_reflns 9847 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1319 _refine_ls_R_factor_gt 0.0777 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1027P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1877 _refine_ls_wR_factor_ref 0.2083 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(C27) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 3.a Aromatic/amide H refined with riding coordinates: C11(H11), C12(H12), C14(H14), C15(H15), C21(H21), C22(H22), C24(H24), C25(H25), C31(H31), C32(H32), C34(H34), C35(H35), C41(H41), C42(H42), C44(H44), C45(H45), C51(H51), C52(H52), C53(H53), C55(H55), C56(H56), C57(H57), C61(H61), C62(H62), C63(H63), C65(H65), C66(H66), C67(H67) 3.b Idealised Me refined as rotating group: C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C27(H27A,H27B, H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C37(H37A,H37B,H37C), C38(H38A, H38B,H38C), C39(H39A,H39B,H39C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Cl80 Cl 0.66292(13) 0.44167(11) 0.28271(9) 0.0970(6) Uani 1 1 d . . . Cl81 Cl 0.50554(15) 0.5061(2) 0.19953(11) 0.1717(13) Uani 1 1 d . . . O70 O 0.54370(16) 0.33171(14) 0.02677(11) 0.0283(6) Uani 1 1 d . . . C10 C 1.0053(2) 0.2533(2) 0.09386(16) 0.0220(8) Uani 1 1 d . . . C11 C 1.0686(2) 0.2816(2) 0.14435(16) 0.0254(8) Uani 1 1 d . . . H11 H 1.0477 0.3138 0.1716 0.030 Uiso 1 1 calc R . . C12 C 1.1615(3) 0.2630(2) 0.15505(17) 0.0303(9) Uani 1 1 d . . . H12 H 1.2025 0.2835 0.1891 0.036 Uiso 1 1 calc R . . C13 C 1.1960(3) 0.2138(2) 0.11599(17) 0.0297(9) Uani 1 1 d . . . C14 C 1.1329(3) 0.1839(2) 0.06666(18) 0.0317(9) Uani 1 1 d . . . H14 H 1.1538 0.1506 0.0400 0.038 Uiso 1 1 calc R . . C15 C 1.0385(3) 0.2022(2) 0.05565(18) 0.0302(9) Uani 1 1 d . . . H15 H 0.9971 0.1801 0.0225 0.036 Uiso 1 1 calc R . . C16 C 1.3016(3) 0.1973(3) 0.12701(19) 0.0407(11) Uani 1 1 d . . . C17 C 1.3382(3) 0.1677(3) 0.1922(2) 0.0511(13) Uani 1 1 d . . . H17A H 1.3105 0.1183 0.1968 0.077 Uiso 1 1 calc R . . H17B H 1.3223 0.2041 0.2206 0.077 Uiso 1 1 calc R . . H17C H 1.4048 0.1622 0.2002 0.077 Uiso 1 1 calc R . . C18 C 1.3239(3) 0.1384(3) 0.0825(2) 0.0647(16) Uani 1 1 d . . . H18A H 1.3047 0.1582 0.0417 0.097 Uiso 1 1 calc R . . H18B H 1.2914 0.0909 0.0859 0.097 Uiso 1 1 calc R . . H18C H 1.3899 0.1287 0.0918 0.097 Uiso 1 1 calc R . . C19 C 1.3506(3) 0.2745(3) 0.1182(2) 0.0639(15) Uani 1 1 d . . . H19A H 1.3235 0.2953 0.0785 0.096 Uiso 1 1 calc R . . H19B H 1.4159 0.2651 0.1215 0.096 Uiso 1 1 calc R . . H19C H 1.3429 0.3108 0.1490 0.096 Uiso 1 1 calc R . . C20 C 0.7786(2) 0.2087(2) -0.06414(16) 0.0218(8) Uani 1 1 d . . . C21 C 0.7892(3) 0.1306(2) -0.04851(17) 0.0269(9) Uani 1 1 d . . . H21 H 0.7582 0.1101 -0.0204 0.032 Uiso 1 1 calc R . . C22 C 0.8455(3) 0.0832(2) -0.07433(18) 0.0322(9) Uani 1 1 d . . . H22 H 0.8522 0.0314 -0.0626 0.039 Uiso 1 1 calc R . . C23 C 0.8921(3) 0.1104(2) -0.11717(18) 0.0306(9) Uani 1 1 d . . . C24 C 0.8789(3) 0.1877(2) -0.13408(18) 0.0316(9) Uani 1 1 d . . . H24 H 0.9074 0.2074 -0.1638 0.038 Uiso 1 1 calc R . . C25 C 0.8241(3) 0.2361(2) -0.10767(16) 0.0265(9) Uani 1 1 d . . . H25 H 0.8175 0.2879 -0.1193 0.032 Uiso 1 1 calc R . . C26 C 0.9558(3) 0.0561(3) -0.1444(2) 0.0487(12) Uani 1 1 d . . . C27 C 0.9993(6) 0.0967(4) -0.1902(4) 0.131(3) Uani 1 1 d U . . H27A H 1.0426 0.1351 -0.1698 0.196 Uiso 1 1 calc R . . H27B H 0.9514 0.1215 -0.2204 0.196 Uiso 1 1 calc R . . H27C H 1.0316 0.0596 -0.2097 0.196 Uiso 1 1 calc R . . C28 C 1.0271(4) 0.0177(4) -0.0928(3) 0.092(2) Uani 1 1 d . . . H28A H 1.0698 0.0562 -0.0718 0.138 Uiso 1 1 calc R . . H28B H 1.0610 -0.0211 -0.1095 0.138 Uiso 1 1 calc R . . H28C H 0.9954 -0.0062 -0.0646 0.138 Uiso 1 1 calc R . . C29 C 0.8955(4) -0.0099(3) -0.1800(3) 0.0750(17) Uani 1 1 d . . . H29A H 0.8459 0.0121 -0.2106 0.113 Uiso 1 1 calc R . . H29B H 0.8696 -0.0406 -0.1523 0.113 Uiso 1 1 calc R . . H29C H 0.9337 -0.0421 -0.1993 0.113 Uiso 1 1 calc R . . C30 C 0.5674(2) 0.1938(2) -0.05173(16) 0.0228(8) Uani 1 1 d . . . C31 C 0.5082(3) 0.1631(2) -0.01784(18) 0.0294(9) Uani 1 1 d . . . H31 H 0.5123 0.1806 0.0218 0.035 Uiso 1 1 calc R . . C32 C 0.4430(3) 0.1069(2) -0.04200(19) 0.0336(10) Uani 1 1 d . . . H32 H 0.4051 0.0866 -0.0179 0.040 Uiso 1 1 calc R . . C33 C 0.4329(3) 0.0800(2) -0.10158(19) 0.0309(9) Uani 1 1 d . . . C34 C 0.4921(3) 0.1122(2) -0.13504(18) 0.0322(9) Uani 1 1 d . . . H34 H 0.4871 0.0956 -0.1750 0.039 Uiso 1 1 calc R . . C35 C 0.5576(2) 0.1674(2) -0.11140(17) 0.0265(9) Uani 1 1 d . . . H35 H 0.5958 0.1874 -0.1355 0.032 Uiso 1 1 calc R . . C36 C 0.3621(3) 0.0175(2) -0.1293(2) 0.0387(11) Uani 1 1 d . . . C37 C 0.4156(3) -0.0537(3) -0.1431(2) 0.0544(13) Uani 1 1 d . . . H37A H 0.4603 -0.0689 -0.1069 0.082 Uiso 1 1 calc R . . H37B H 0.4475 -0.0413 -0.1747 0.082 Uiso 1 1 calc R . . H37C H 0.3728 -0.0955 -0.1564 0.082 Uiso 1 1 calc R . . C38 C 0.2981(3) 0.0482(3) -0.1867(2) 0.0629(15) Uani 1 1 d . . . H38A H 0.2648 0.0925 -0.1769 0.094 Uiso 1 1 calc R . . H38B H 0.2544 0.0085 -0.2044 0.094 Uiso 1 1 calc R . . H38C H 0.3343 0.0630 -0.2154 0.094 Uiso 1 1 calc R . . C39 C 0.3024(3) -0.0093(3) -0.0847(3) 0.0632(15) Uani 1 1 d . . . H39A H 0.3427 -0.0265 -0.0472 0.095 Uiso 1 1 calc R . . H39B H 0.2625 -0.0512 -0.1027 0.095 Uiso 1 1 calc R . . H39C H 0.2650 0.0333 -0.0764 0.095 Uiso 1 1 calc R . . C40 C 0.7127(2) 0.4324(2) 0.07120(15) 0.0201(8) Uani 1 1 d . . . C41 C 0.7847(2) 0.4582(2) 0.11836(16) 0.0232(8) Uani 1 1 d . . . H41 H 0.8291 0.4229 0.1383 0.028 Uiso 1 1 calc R . . C42 C 0.7917(3) 0.5357(2) 0.13638(16) 0.0238(8) Uani 1 1 d . . . H42 H 0.8404 0.5511 0.1683 0.029 Uiso 1 1 calc R . . C43 C 0.7274(3) 0.5904(2) 0.10748(16) 0.0257(8) Uani 1 1 d . . . C44 C 0.6549(3) 0.5637(2) 0.06110(17) 0.0319(9) Uani 1 1 d . . . H44 H 0.6102 0.5988 0.0413 0.038 Uiso 1 1 calc R . . C45 C 0.6472(3) 0.4865(2) 0.04349(17) 0.0286(9) Uani 1 1 d . . . H45 H 0.5973 0.4709 0.0125 0.034 Uiso 1 1 calc R . . C46 C 0.7342(3) 0.6767(2) 0.12410(17) 0.0328(10) Uani 1 1 d . . . C47 C 0.7502(4) 0.7229(2) 0.0687(2) 0.0577(14) Uani 1 1 d . . . H47A H 0.7563 0.7771 0.0789 0.087 Uiso 1 1 calc R . . H47B H 0.6981 0.7155 0.0348 0.087 Uiso 1 1 calc R . . H47C H 0.8062 0.7050 0.0581 0.087 Uiso 1 1 calc R . . C48 C 0.6425(3) 0.7037(2) 0.13906(19) 0.0428(11) Uani 1 1 d . . . H48A H 0.6486 0.7567 0.1525 0.064 Uiso 1 1 calc R . . H48B H 0.6286 0.6717 0.1708 0.064 Uiso 1 1 calc R . . H48C H 0.5928 0.6997 0.1032 0.064 Uiso 1 1 calc R . . C49 C 0.8148(3) 0.6936(2) 0.1788(2) 0.0440(11) Uani 1 1 d . . . H49A H 0.8190 0.7486 0.1861 0.066 Uiso 1 1 calc R . . H49B H 0.8722 0.6753 0.1703 0.066 Uiso 1 1 calc R . . H49C H 0.8039 0.6676 0.2143 0.066 Uiso 1 1 calc R . . C50 C 0.8523(2) 0.21161(19) 0.16820(16) 0.0208(8) Uani 1 1 d . . . C51 C 0.9209(3) 0.1645(2) 0.20062(17) 0.0270(9) Uani 1 1 d . . . H51 H 0.9765 0.1575 0.1882 0.032 Uiso 1 1 calc R . . C52 C 0.9057(3) 0.1267(2) 0.25331(17) 0.0299(9) Uani 1 1 d . . . H52 H 0.9518 0.0940 0.2750 0.036 Uiso 1 1 calc R . . C53 C 0.8253(3) 0.1365(2) 0.27352(17) 0.0305(9) Uani 1 1 d . . . H53 H 0.8179 0.1107 0.3084 0.037 Uiso 1 1 calc R . . C54 C 0.7533(3) 0.1858(2) 0.24155(16) 0.0253(8) Uani 1 1 d . . . C55 C 0.6671(3) 0.2041(2) 0.25658(17) 0.0314(9) Uani 1 1 d . . . H55 H 0.6526 0.1828 0.2913 0.038 Uiso 1 1 calc R . . C56 C 0.6054(3) 0.2530(2) 0.22010(17) 0.0314(9) Uani 1 1 d . . . H56 H 0.5495 0.2643 0.2309 0.038 Uiso 1 1 calc R . . C57 C 0.6230(2) 0.2872(2) 0.16642(16) 0.0259(8) Uani 1 1 d . . . H57 H 0.5793 0.3199 0.1423 0.031 Uiso 1 1 calc R . . C58 C 0.7065(2) 0.27093(19) 0.15098(15) 0.0212(8) Uani 1 1 d . . . C59 C 0.7699(2) 0.2209(2) 0.18994(16) 0.0226(8) Uani 1 1 d . . . C60 C 0.9290(2) 0.3675(2) -0.01018(15) 0.0223(8) Uani 1 1 d . . . C61 C 1.0224(3) 0.3764(2) -0.00981(17) 0.0275(9) Uani 1 1 d . . . H61 H 1.0672 0.3456 0.0153 0.033 Uiso 1 1 calc R . . C62 C 1.0486(3) 0.4326(2) -0.04798(17) 0.0326(9) Uani 1 1 d . . . H62 H 1.1115 0.4380 -0.0480 0.039 Uiso 1 1 calc R . . C63 C 0.9853(3) 0.4794(2) -0.08495(17) 0.0328(10) Uani 1 1 d . . . H63 H 1.0058 0.5163 -0.1091 0.039 Uiso 1 1 calc R . . C64 C 0.8890(3) 0.4726(2) -0.08697(16) 0.0270(9) Uani 1 1 d . . . C65 C 0.8148(3) 0.5166(2) -0.12223(17) 0.0325(10) Uani 1 1 d . . . H65 H 0.8277 0.5568 -0.1467 0.039 Uiso 1 1 calc R . . C66 C 0.7242(3) 0.5004(2) -0.12067(17) 0.0344(10) Uani 1 1 d . . . H66 H 0.6766 0.5294 -0.1450 0.041 Uiso 1 1 calc R . . C67 C 0.7003(3) 0.4409(2) -0.08324(16) 0.0286(9) Uani 1 1 d . . . H67 H 0.6383 0.4297 -0.0839 0.034 Uiso 1 1 calc R . . C68 C 0.7713(2) 0.40035(19) -0.04603(16) 0.0220(8) Uani 1 1 d . . . C69 C 0.8641(2) 0.4158(2) -0.04886(15) 0.0217(8) Uani 1 1 d . . . C70 C 0.8389(2) 0.25926(19) 0.11232(15) 0.0211(8) Uani 1 1 d . . . C71 C 0.9062(2) 0.27805(19) 0.07588(15) 0.0205(8) Uani 1 1 d . . . C72 C 0.8764(2) 0.32154(19) 0.02547(15) 0.0206(8) Uani 1 1 d . . . C73 C 0.7725(2) 0.33517(19) -0.00050(15) 0.0191(8) Uani 1 1 d . . . C74 C 0.7136(2) 0.34880(19) 0.04938(15) 0.0209(8) Uani 1 1 d . . . C75 C 0.7521(2) 0.29364(19) 0.10205(15) 0.0210(8) Uani 1 1 d . . . C76 C 0.6189(2) 0.3133(2) 0.01749(15) 0.0218(8) Uani 1 1 d . . . C77 C 0.6376(2) 0.2524(2) -0.02454(16) 0.0225(8) Uani 1 1 d . . . C78 C 0.7253(2) 0.26119(19) -0.03239(15) 0.0202(8) Uani 1 1 d . . . C80 C 0.6227(4) 0.4856(4) 0.2120(3) 0.0771(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl80 0.0933(13) 0.0871(12) 0.1099(13) 0.0160(10) 0.0215(10) -0.0111(10) Cl81 0.0684(14) 0.313(4) 0.1258(18) 0.045(2) 0.0064(12) 0.0053(18) O70 0.0170(14) 0.0322(15) 0.0372(15) -0.0056(12) 0.0088(11) 0.0044(11) C10 0.019(2) 0.0218(19) 0.027(2) 0.0041(16) 0.0095(16) 0.0019(15) C11 0.022(2) 0.029(2) 0.027(2) 0.0012(17) 0.0093(16) 0.0033(16) C12 0.023(2) 0.038(2) 0.028(2) 0.0066(18) 0.0006(16) -0.0009(18) C13 0.023(2) 0.035(2) 0.034(2) 0.0115(18) 0.0098(17) 0.0030(17) C14 0.026(2) 0.034(2) 0.039(2) 0.0000(19) 0.0156(18) 0.0085(18) C15 0.024(2) 0.031(2) 0.035(2) -0.0008(18) 0.0050(17) 0.0025(17) C16 0.021(2) 0.062(3) 0.040(2) 0.009(2) 0.0087(18) 0.007(2) C17 0.028(3) 0.077(4) 0.048(3) 0.020(3) 0.007(2) 0.016(2) C18 0.031(3) 0.104(4) 0.062(3) -0.002(3) 0.017(2) 0.030(3) C19 0.032(3) 0.093(4) 0.067(3) 0.024(3) 0.012(2) -0.005(3) C20 0.0164(19) 0.0227(19) 0.027(2) -0.0031(16) 0.0060(15) -0.0011(15) C21 0.030(2) 0.0209(19) 0.034(2) 0.0018(17) 0.0168(17) -0.0013(17) C22 0.036(2) 0.0175(19) 0.045(2) 0.0024(18) 0.0120(19) 0.0041(17) C23 0.027(2) 0.026(2) 0.041(2) -0.0072(18) 0.0131(18) 0.0015(17) C24 0.032(2) 0.032(2) 0.037(2) -0.0032(18) 0.0206(18) -0.0051(18) C25 0.031(2) 0.0183(19) 0.033(2) -0.0020(16) 0.0125(17) -0.0016(16) C26 0.044(3) 0.043(3) 0.068(3) -0.011(2) 0.030(2) 0.013(2) C27 0.175(7) 0.074(4) 0.201(8) -0.003(5) 0.164(7) 0.032(5) C28 0.051(4) 0.108(5) 0.111(5) -0.032(4) 0.005(3) 0.046(4) C29 0.077(4) 0.060(4) 0.089(4) -0.029(3) 0.021(3) 0.022(3) C30 0.0183(19) 0.0218(19) 0.030(2) 0.0002(16) 0.0083(16) 0.0029(15) C31 0.028(2) 0.030(2) 0.033(2) -0.0041(18) 0.0114(17) -0.0038(18) C32 0.022(2) 0.033(2) 0.050(3) 0.000(2) 0.0167(19) -0.0044(18) C33 0.021(2) 0.024(2) 0.047(2) -0.0034(18) 0.0065(18) 0.0035(16) C34 0.025(2) 0.038(2) 0.033(2) -0.0104(19) 0.0055(17) -0.0013(18) C35 0.020(2) 0.028(2) 0.033(2) -0.0042(18) 0.0104(16) -0.0022(17) C36 0.021(2) 0.032(2) 0.063(3) -0.013(2) 0.010(2) -0.0044(18) C37 0.045(3) 0.030(2) 0.091(4) -0.022(3) 0.020(3) -0.006(2) C38 0.035(3) 0.050(3) 0.092(4) -0.019(3) -0.012(3) -0.010(2) C39 0.041(3) 0.048(3) 0.105(4) -0.024(3) 0.026(3) -0.022(2) C40 0.0160(19) 0.0215(19) 0.0248(19) -0.0013(16) 0.0091(15) 0.0028(15) C41 0.021(2) 0.0227(19) 0.028(2) 0.0055(16) 0.0101(16) 0.0052(16) C42 0.023(2) 0.023(2) 0.027(2) -0.0025(16) 0.0096(16) -0.0039(16) C43 0.031(2) 0.024(2) 0.024(2) 0.0011(16) 0.0110(17) 0.0029(17) C44 0.038(2) 0.027(2) 0.031(2) 0.0007(18) 0.0087(18) 0.0170(18) C45 0.026(2) 0.031(2) 0.028(2) -0.0033(17) 0.0039(17) 0.0049(17) C46 0.048(3) 0.019(2) 0.033(2) -0.0003(17) 0.0147(19) 0.0068(18) C47 0.102(4) 0.022(2) 0.058(3) 0.006(2) 0.039(3) 0.002(3) C48 0.057(3) 0.030(2) 0.041(3) -0.006(2) 0.010(2) 0.019(2) C49 0.051(3) 0.022(2) 0.060(3) -0.013(2) 0.014(2) -0.003(2) C50 0.022(2) 0.0132(17) 0.029(2) -0.0017(15) 0.0081(16) 0.0005(15) C51 0.024(2) 0.0221(19) 0.036(2) 0.0001(17) 0.0094(17) 0.0030(16) C52 0.036(2) 0.021(2) 0.031(2) 0.0053(17) 0.0039(18) 0.0060(18) C53 0.043(3) 0.023(2) 0.027(2) 0.0020(17) 0.0101(18) -0.0027(18) C54 0.032(2) 0.0202(19) 0.025(2) -0.0035(16) 0.0078(17) -0.0054(17) C55 0.037(2) 0.033(2) 0.028(2) -0.0014(18) 0.0164(18) -0.0059(19) C56 0.024(2) 0.038(2) 0.037(2) -0.0046(19) 0.0178(18) -0.0026(18) C57 0.021(2) 0.028(2) 0.030(2) -0.0027(17) 0.0080(16) 0.0006(16) C58 0.019(2) 0.0181(18) 0.0260(19) -0.0031(16) 0.0046(15) -0.0018(15) C59 0.025(2) 0.0171(18) 0.026(2) -0.0037(16) 0.0078(16) -0.0018(15) C60 0.024(2) 0.0197(19) 0.025(2) -0.0079(16) 0.0098(16) -0.0062(16) C61 0.023(2) 0.031(2) 0.031(2) -0.0060(17) 0.0103(17) -0.0048(17) C62 0.030(2) 0.035(2) 0.037(2) -0.0078(19) 0.0164(19) -0.0083(19) C63 0.046(3) 0.027(2) 0.030(2) -0.0063(18) 0.0194(19) -0.0140(19) C64 0.039(2) 0.0190(19) 0.026(2) -0.0088(16) 0.0132(18) -0.0071(17) C65 0.051(3) 0.020(2) 0.029(2) 0.0022(17) 0.0151(19) -0.0052(19) C66 0.048(3) 0.025(2) 0.029(2) 0.0050(17) 0.0051(19) 0.011(2) C67 0.029(2) 0.025(2) 0.032(2) 0.0001(17) 0.0079(17) 0.0047(17) C68 0.027(2) 0.0168(18) 0.0233(19) -0.0041(15) 0.0082(16) -0.0007(16) C69 0.024(2) 0.0196(19) 0.0224(19) -0.0075(15) 0.0081(16) -0.0039(16) C70 0.020(2) 0.0185(18) 0.0251(19) -0.0016(15) 0.0064(15) 0.0008(15) C71 0.021(2) 0.0156(18) 0.0259(19) -0.0055(15) 0.0079(15) -0.0001(15) C72 0.0200(19) 0.0170(18) 0.0261(19) -0.0055(16) 0.0084(15) 0.0002(15) C73 0.0172(19) 0.0201(18) 0.0219(18) 0.0002(15) 0.0079(15) -0.0001(15) C74 0.0205(19) 0.0190(18) 0.0245(19) 0.0019(15) 0.0075(15) 0.0043(15) C75 0.023(2) 0.0169(18) 0.0238(19) -0.0025(15) 0.0064(15) -0.0023(15) C76 0.022(2) 0.0199(19) 0.0242(19) 0.0052(15) 0.0066(16) 0.0029(16) C77 0.019(2) 0.0228(19) 0.026(2) 0.0036(16) 0.0045(15) -0.0004(15) C78 0.023(2) 0.0167(18) 0.0201(18) 0.0010(15) 0.0027(15) -0.0011(15) C80 0.070(4) 0.087(4) 0.078(4) 0.009(3) 0.024(3) 0.000(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl80 C80 1.739(6) . ? Cl81 C80 1.719(6) . ? O70 C76 1.214(4) . ? C10 C11 1.383(5) . ? C10 C15 1.394(5) . ? C10 C71 1.485(5) . ? C11 H11 0.9300 . ? C11 C12 1.372(5) . ? C12 H12 0.9300 . ? C12 C13 1.395(5) . ? C13 C14 1.375(5) . ? C13 C16 1.545(5) . ? C14 H14 0.9300 . ? C14 C15 1.391(5) . ? C15 H15 0.9300 . ? C16 C17 1.530(6) . ? C16 C18 1.512(6) . ? C16 C19 1.547(7) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.389(5) . ? C20 C25 1.387(5) . ? C20 C78 1.483(5) . ? C21 H21 0.9300 . ? C21 C22 1.381(5) . ? C22 H22 0.9300 . ? C22 C23 1.385(5) . ? C23 C24 1.386(5) . ? C23 C26 1.545(5) . ? C24 H24 0.9300 . ? C24 C25 1.384(5) . ? C25 H25 0.9300 . ? C26 C27 1.504(7) . ? C26 C28 1.528(7) . ? C26 C29 1.549(7) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C31 1.386(5) . ? C30 C35 1.393(5) . ? C30 C77 1.475(5) . ? C31 H31 0.9300 . ? C31 C32 1.384(5) . ? C32 H32 0.9300 . ? C32 C33 1.393(5) . ? C33 C34 1.388(5) . ? C33 C36 1.530(5) . ? C34 H34 0.9300 . ? C34 C35 1.373(5) . ? C35 H35 0.9300 . ? C36 C37 1.526(6) . ? C36 C38 1.510(6) . ? C36 C39 1.547(6) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C41 1.391(5) . ? C40 C45 1.383(5) . ? C40 C74 1.522(5) . ? C41 H41 0.9300 . ? C41 C42 1.393(5) . ? C42 H42 0.9300 . ? C42 C43 1.388(5) . ? C43 C44 1.390(5) . ? C43 C46 1.530(5) . ? C44 H44 0.9300 . ? C44 C45 1.384(5) . ? C45 H45 0.9300 . ? C46 C47 1.540(6) . ? C46 C48 1.536(5) . ? C46 C49 1.531(6) . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 C51 1.369(5) . ? C50 C59 1.417(5) . ? C50 C70 1.476(5) . ? C51 H51 0.9300 . ? C51 C52 1.414(5) . ? C52 H52 0.9300 . ? C52 C53 1.371(5) . ? C53 H53 0.9300 . ? C53 C54 1.419(5) . ? C54 C55 1.420(5) . ? C54 C59 1.378(5) . ? C55 H55 0.9300 . ? C55 C56 1.367(5) . ? C56 H56 0.9300 . ? C56 C57 1.419(5) . ? C57 H57 0.9300 . ? C57 C58 1.379(5) . ? C58 C59 1.418(5) . ? C58 C75 1.466(5) . ? C60 C61 1.382(5) . ? C60 C69 1.408(5) . ? C60 C72 1.466(5) . ? C61 H61 0.9300 . ? C61 C62 1.405(5) . ? C62 H62 0.9300 . ? C62 C63 1.363(6) . ? C63 H63 0.9300 . ? C63 C64 1.413(5) . ? C64 C65 1.415(5) . ? C64 C69 1.403(5) . ? C65 H65 0.9300 . ? C65 C66 1.371(6) . ? C66 H66 0.9300 . ? C66 C67 1.420(5) . ? C67 H67 0.9300 . ? C67 C68 1.372(5) . ? C68 C69 1.407(5) . ? C68 C73 1.517(5) . ? C70 C71 1.458(5) . ? C70 C75 1.379(5) . ? C71 C72 1.346(5) . ? C72 C73 1.526(5) . ? C73 C74 1.583(5) . ? C73 C78 1.548(5) . ? C74 C75 1.524(5) . ? C74 C76 1.542(5) . ? C76 C77 1.479(5) . ? C77 C78 1.350(5) . ? 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 C11 C10 C15 117.6(3) . . ? C11 C10 C71 124.0(3) . . ? C15 C10 C71 118.2(3) . . ? C10 C11 H11 119.3 . . ? C12 C11 C10 121.4(3) . . ? C12 C11 H11 119.3 . . ? C11 C12 H12 119.3 . . ? C11 C12 C13 121.4(4) . . ? C13 C12 H12 119.3 . . ? C12 C13 C16 120.5(4) . . ? C14 C13 C12 117.4(3) . . ? C14 C13 C16 122.1(4) . . ? C13 C14 H14 119.2 . . ? C13 C14 C15 121.5(4) . . ? C15 C14 H14 119.2 . . ? C10 C15 H15 119.7 . . ? C14 C15 C10 120.6(4) . . ? C14 C15 H15 119.7 . . ? C13 C16 C19 107.6(4) . . ? C17 C16 C13 109.7(3) . . ? C17 C16 C19 109.7(4) . . ? C18 C16 C13 112.3(4) . . ? C18 C16 C17 109.2(4) . . ? C18 C16 C19 108.3(4) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C78 120.7(3) . . ? C25 C20 C21 117.6(3) . . ? C25 C20 C78 121.6(3) . . ? C20 C21 H21 119.7 . . ? C22 C21 C20 120.6(3) . . ? C22 C21 H21 119.7 . . ? C21 C22 H22 119.0 . . ? C21 C22 C23 122.1(3) . . ? C23 C22 H22 119.0 . . ? C22 C23 C24 117.0(3) . . ? C22 C23 C26 120.7(4) . . ? C24 C23 C26 122.2(4) . . ? C23 C24 H24 119.3 . . ? C25 C24 C23 121.3(3) . . ? C25 C24 H24 119.3 . . ? C20 C25 H25 119.4 . . ? C24 C25 C20 121.3(3) . . ? C24 C25 H25 119.4 . . ? C23 C26 C29 108.8(4) . . ? C27 C26 C23 112.3(4) . . ? C27 C26 C28 113.3(5) . . ? C27 C26 C29 105.7(5) . . ? C28 C26 C23 109.7(4) . . ? C28 C26 C29 106.8(4) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 C35 117.7(3) . . ? C31 C30 C77 120.1(3) . . ? C35 C30 C77 122.2(3) . . ? C30 C31 H31 119.4 . . ? C32 C31 C30 121.1(4) . . ? C32 C31 H31 119.4 . . ? C31 C32 H32 119.2 . . ? C31 C32 C33 121.5(4) . . ? C33 C32 H32 119.2 . . ? C32 C33 C36 122.7(4) . . ? C34 C33 C32 116.5(3) . . ? C34 C33 C36 120.8(4) . . ? C33 C34 H34 118.7 . . ? C35 C34 C33 122.6(4) . . ? C35 C34 H34 118.7 . . ? C30 C35 H35 119.7 . . ? C34 C35 C30 120.6(3) . . ? C34 C35 H35 119.7 . . ? C33 C36 C39 112.3(4) . . ? C37 C36 C33 108.2(3) . . ? C37 C36 C39 106.7(4) . . ? C38 C36 C33 109.7(4) . . ? C38 C36 C37 111.0(4) . . ? C38 C36 C39 108.8(4) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37B 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38B 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 C74 119.1(3) . . ? C45 C40 C41 117.4(3) . . ? C45 C40 C74 123.3(3) . . ? C40 C41 H41 119.3 . . ? C40 C41 C42 121.5(3) . . ? C42 C41 H41 119.3 . . ? C41 C42 H42 119.4 . . ? C43 C42 C41 121.1(3) . . ? C43 C42 H42 119.4 . . ? C42 C43 C44 116.9(3) . . ? C42 C43 C46 123.0(3) . . ? C44 C43 C46 120.1(3) . . ? C43 C44 H44 118.9 . . ? C45 C44 C43 122.1(3) . . ? C45 C44 H44 118.9 . . ? C40 C45 C44 121.0(4) . . ? C40 C45 H45 119.5 . . ? C44 C45 H45 119.5 . . ? C43 C46 C47 108.6(3) . . ? C43 C46 C48 109.6(3) . . ? C43 C46 C49 112.2(3) . . ? C48 C46 C47 108.9(3) . . ? C49 C46 C47 108.5(4) . . ? C49 C46 C48 109.0(3) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47B 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48B 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49B 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C51 C50 C59 117.9(3) . . ? C51 C50 C70 136.3(3) . . ? C59 C50 C70 105.8(3) . . ? C50 C51 H51 120.6 . . ? C50 C51 C52 118.8(3) . . ? C52 C51 H51 120.6 . . ? C51 C52 H52 118.9 . . ? C53 C52 C51 122.2(3) . . ? C53 C52 H52 118.9 . . ? C52 C53 H53 119.7 . . ? C52 C53 C54 120.5(3) . . ? C54 C53 H53 119.7 . . ? C53 C54 C55 128.1(3) . . ? C59 C54 C53 115.7(3) . . ? C59 C54 C55 116.2(3) . . ? C54 C55 H55 120.0 . . ? C56 C55 C54 120.1(3) . . ? C56 C55 H55 120.0 . . ? C55 C56 H56 118.6 . . ? C55 C56 C57 122.8(3) . . ? C57 C56 H56 118.6 . . ? C56 C57 H57 120.9 . . ? C58 C57 C56 118.3(3) . . ? C58 C57 H57 120.9 . . ? C57 C58 C59 117.8(3) . . ? C57 C58 C75 136.1(3) . . ? C59 C58 C75 106.1(3) . . ? C50 C59 C58 110.5(3) . . ? C54 C59 C50 124.8(3) . . ? C54 C59 C58 124.7(3) . . ? C61 C60 C69 118.2(3) . . ? C61 C60 C72 134.8(3) . . ? C69 C60 C72 106.8(3) . . ? C60 C61 H61 120.5 . . ? C60 C61 C62 118.9(4) . . ? C62 C61 H61 120.5 . . ? C61 C62 H62 118.8 . . ? C63 C62 C61 122.4(4) . . ? C63 C62 H62 118.8 . . ? C62 C63 H63 119.6 . . ? C62 C63 C64 120.8(4) . . ? C64 C63 H63 119.6 . . ? C63 C64 C65 127.9(4) . . ? C69 C64 C63 116.0(4) . . ? C69 C64 C65 116.1(3) . . ? C64 C65 H65 119.7 . . ? C66 C65 C64 120.6(3) . . ? C66 C65 H65 119.7 . . ? C65 C66 H66 118.8 . . ? C65 C66 C67 122.3(4) . . ? C67 C66 H66 118.8 . . ? C66 C67 H67 120.9 . . ? C68 C67 C66 118.2(4) . . ? C68 C67 H67 120.9 . . ? C67 C68 C69 119.2(3) . . ? C67 C68 C73 132.8(3) . . ? C69 C68 C73 107.9(3) . . ? C64 C69 C60 123.6(3) . . ? C64 C69 C68 123.4(3) . . ? C68 C69 C60 112.9(3) . . ? C71 C70 C50 128.7(3) . . ? C75 C70 C50 108.7(3) . . ? C75 C70 C71 122.2(3) . . ? C70 C71 C10 122.3(3) . . ? C72 C71 C10 120.1(3) . . ? C72 C71 C70 117.6(3) . . ? C60 C72 C73 108.3(3) . . ? C71 C72 C60 130.5(3) . . ? C71 C72 C73 120.9(3) . . ? C68 C73 C72 103.3(3) . . ? C68 C73 C74 116.3(3) . . ? C68 C73 C78 111.2(3) . . ? C72 C73 C74 114.5(3) . . ? C72 C73 C78 110.9(3) . . ? C78 C73 C74 100.9(3) . . ? C40 C74 C73 114.5(3) . . ? C40 C74 C75 111.6(3) . . ? C40 C74 C76 116.8(3) . . ? C75 C74 C73 106.9(3) . . ? C75 C74 C76 104.6(3) . . ? C76 C74 C73 101.2(3) . . ? C58 C75 C74 126.6(3) . . ? C70 C75 C58 108.9(3) . . ? C70 C75 C74 124.4(3) . . ? O70 C76 C74 125.4(3) . . ? O70 C76 C77 127.2(3) . . ? C77 C76 C74 107.4(3) . . ? C30 C77 C76 122.4(3) . . ? C78 C77 C30 128.5(3) . . ? C78 C77 C76 109.1(3) . . ? C20 C78 C73 119.6(3) . . ? C77 C78 C20 128.4(3) . . ? C77 C78 C73 111.9(3) . . ? Cl81 C80 Cl80 111.1(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O70 C76 C77 C30 -13.5(5) . . . . ? O70 C76 C77 C78 166.3(3) . . . . ? C10 C11 C12 C13 -1.0(6) . . . . ? C10 C71 C72 C60 -17.1(5) . . . . ? C10 C71 C72 C73 168.7(3) . . . . ? C11 C10 C15 C14 -3.3(5) . . . . ? C11 C10 C71 C70 -67.8(5) . . . . ? C11 C10 C71 C72 110.0(4) . . . . ? C11 C12 C13 C14 -0.8(5) . . . . ? C11 C12 C13 C16 176.6(4) . . . . ? C12 C13 C14 C15 0.5(6) . . . . ? C12 C13 C16 C17 54.3(5) . . . . ? C12 C13 C16 C18 175.9(4) . . . . ? C12 C13 C16 C19 -65.0(5) . . . . ? C13 C14 C15 C10 1.6(6) . . . . ? C14 C13 C16 C17 -128.4(4) . . . . ? C14 C13 C16 C18 -6.8(6) . . . . ? C14 C13 C16 C19 112.4(4) . . . . ? C15 C10 C11 C12 3.0(5) . . . . ? C15 C10 C71 C70 116.4(4) . . . . ? C15 C10 C71 C72 -65.9(5) . . . . ? C16 C13 C14 C15 -176.9(4) . . . . ? C20 C21 C22 C23 -1.1(6) . . . . ? C21 C20 C25 C24 -0.8(5) . . . . ? C21 C20 C78 C73 123.7(4) . . . . ? C21 C20 C78 C77 -53.4(5) . . . . ? C21 C22 C23 C24 -1.0(6) . . . . ? C21 C22 C23 C26 179.0(4) . . . . ? C22 C23 C24 C25 2.2(6) . . . . ? C22 C23 C26 C27 179.7(5) . . . . ? C22 C23 C26 C28 -53.4(6) . . . . ? C22 C23 C26 C29 63.0(5) . . . . ? C23 C24 C25 C20 -1.3(6) . . . . ? C24 C23 C26 C27 -0.3(7) . . . . ? C24 C23 C26 C28 126.6(5) . . . . ? C24 C23 C26 C29 -117.0(5) . . . . ? C25 C20 C21 C22 2.0(5) . . . . ? C25 C20 C78 C73 -52.6(5) . . . . ? C25 C20 C78 C77 130.4(4) . . . . ? C26 C23 C24 C25 -177.8(4) . . . . ? C30 C31 C32 C33 -1.4(6) . . . . ? C30 C77 C78 C20 -8.4(6) . . . . ? C30 C77 C78 C73 174.3(3) . . . . ? C31 C30 C35 C34 -0.8(5) . . . . ? C31 C30 C77 C76 -37.2(5) . . . . ? C31 C30 C77 C78 143.0(4) . . . . ? C31 C32 C33 C34 0.5(6) . . . . ? C31 C32 C33 C36 179.5(4) . . . . ? C32 C33 C34 C35 0.2(6) . . . . ? C32 C33 C36 C37 -115.6(4) . . . . ? C32 C33 C36 C38 123.1(4) . . . . ? C32 C33 C36 C39 1.9(5) . . . . ? C33 C34 C35 C30 0.0(6) . . . . ? C34 C33 C36 C37 63.3(5) . . . . ? C34 C33 C36 C38 -57.9(5) . . . . ? C34 C33 C36 C39 -179.1(4) . . . . ? C35 C30 C31 C32 1.5(5) . . . . ? C35 C30 C77 C76 142.7(3) . . . . ? C35 C30 C77 C78 -37.1(6) . . . . ? C36 C33 C34 C35 -178.9(4) . . . . ? C40 C41 C42 C43 -0.5(5) . . . . ? C40 C74 C75 C58 70.5(4) . . . . ? C40 C74 C75 C70 -106.7(4) . . . . ? C40 C74 C76 O70 -28.4(5) . . . . ? C40 C74 C76 C77 153.0(3) . . . . ? C41 C40 C45 C44 1.7(5) . . . . ? C41 C40 C74 C73 -85.7(4) . . . . ? C41 C40 C74 C75 36.0(4) . . . . ? C41 C40 C74 C76 156.2(3) . . . . ? C41 C42 C43 C44 1.5(5) . . . . ? C41 C42 C43 C46 -177.8(3) . . . . ? C42 C43 C44 C45 -0.9(6) . . . . ? C42 C43 C46 C47 115.5(4) . . . . ? C42 C43 C46 C48 -125.7(4) . . . . ? C42 C43 C46 C49 -4.4(5) . . . . ? C43 C44 C45 C40 -0.7(6) . . . . ? C44 C43 C46 C47 -63.8(5) . . . . ? C44 C43 C46 C48 55.1(5) . . . . ? C44 C43 C46 C49 176.3(3) . . . . ? C45 C40 C41 C42 -1.1(5) . . . . ? C45 C40 C74 C73 89.2(4) . . . . ? C45 C40 C74 C75 -149.1(3) . . . . ? C45 C40 C74 C76 -28.8(5) . . . . ? C46 C43 C44 C45 178.4(3) . . . . ? C50 C51 C52 C53 -1.0(5) . . . . ? C50 C70 C71 C10 -3.8(5) . . . . ? C50 C70 C71 C72 178.4(3) . . . . ? C50 C70 C75 C58 0.9(4) . . . . ? C50 C70 C75 C74 178.5(3) . . . . ? C51 C50 C59 C54 -0.1(5) . . . . ? C51 C50 C59 C58 -179.7(3) . . . . ? C51 C50 C70 C71 -8.2(7) . . . . ? C51 C50 C70 C75 179.2(4) . . . . ? C51 C52 C53 C54 0.1(6) . . . . ? C52 C53 C54 C55 -178.3(4) . . . . ? C52 C53 C54 C59 0.7(5) . . . . ? C53 C54 C55 C56 -179.9(4) . . . . ? C53 C54 C59 C50 -0.8(5) . . . . ? C53 C54 C59 C58 178.8(3) . . . . ? C54 C55 C56 C57 0.2(6) . . . . ? C55 C54 C59 C50 178.4(3) . . . . ? C55 C54 C59 C58 -2.0(5) . . . . ? C55 C56 C57 C58 -0.7(6) . . . . ? C56 C57 C58 C59 -0.1(5) . . . . ? C56 C57 C58 C75 -178.9(4) . . . . ? C57 C58 C59 C50 -178.8(3) . . . . ? C57 C58 C59 C54 1.6(5) . . . . ? C57 C58 C75 C70 178.1(4) . . . . ? C57 C58 C75 C74 0.6(6) . . . . ? C59 C50 C51 C52 1.0(5) . . . . ? C59 C50 C70 C71 171.9(3) . . . . ? C59 C50 C70 C75 -0.7(4) . . . . ? C59 C54 C55 C56 1.1(5) . . . . ? C59 C58 C75 C70 -0.8(4) . . . . ? C59 C58 C75 C74 -178.3(3) . . . . ? C60 C61 C62 C63 0.8(5) . . . . ? C60 C72 C73 C68 -8.2(3) . . . . ? C60 C72 C73 C74 -135.7(3) . . . . ? C60 C72 C73 C78 110.9(3) . . . . ? C61 C60 C69 C64 -0.2(5) . . . . ? C61 C60 C69 C68 178.9(3) . . . . ? C61 C60 C72 C71 8.2(7) . . . . ? C61 C60 C72 C73 -177.0(4) . . . . ? C61 C62 C63 C64 -0.8(6) . . . . ? C62 C63 C64 C65 179.6(4) . . . . ? C62 C63 C64 C69 0.3(5) . . . . ? C63 C64 C65 C66 177.4(4) . . . . ? C63 C64 C69 C60 0.1(5) . . . . ? C63 C64 C69 C68 -178.8(3) . . . . ? C64 C65 C66 C67 1.4(6) . . . . ? C65 C64 C69 C60 -179.2(3) . . . . ? C65 C64 C69 C68 1.8(5) . . . . ? C65 C66 C67 C68 2.2(6) . . . . ? C66 C67 C68 C69 -3.7(5) . . . . ? C66 C67 C68 C73 179.3(3) . . . . ? C67 C68 C69 C60 -177.3(3) . . . . ? C67 C68 C69 C64 1.7(5) . . . . ? C67 C68 C73 C72 -177.9(4) . . . . ? C67 C68 C73 C74 -51.6(5) . . . . ? C67 C68 C73 C78 63.2(5) . . . . ? C68 C73 C74 C40 -35.1(4) . . . . ? C68 C73 C74 C75 -159.4(3) . . . . ? C68 C73 C74 C76 91.5(3) . . . . ? C68 C73 C78 C20 81.1(4) . . . . ? C68 C73 C78 C77 -101.4(3) . . . . ? C69 C60 C61 C62 -0.3(5) . . . . ? C69 C60 C72 C71 -166.1(3) . . . . ? C69 C60 C72 C73 8.7(4) . . . . ? C69 C64 C65 C66 -3.3(5) . . . . ? C69 C68 C73 C72 4.8(3) . . . . ? C69 C68 C73 C74 131.1(3) . . . . ? C69 C68 C73 C78 -114.1(3) . . . . ? C70 C50 C51 C52 -178.9(4) . . . . ? C70 C50 C59 C54 179.8(3) . . . . ? C70 C50 C59 C58 0.2(4) . . . . ? C70 C71 C72 C60 160.7(3) . . . . ? C70 C71 C72 C73 -13.5(5) . . . . ? C71 C10 C11 C12 -172.9(3) . . . . ? C71 C10 C15 C14 172.9(3) . . . . ? C71 C70 C75 C58 -172.3(3) . . . . ? C71 C70 C75 C74 5.4(5) . . . . ? C71 C72 C73 C68 167.1(3) . . . . ? C71 C72 C73 C74 39.7(4) . . . . ? C71 C72 C73 C78 -73.7(4) . . . . ? C72 C60 C61 C62 -174.0(4) . . . . ? C72 C60 C69 C64 175.2(3) . . . . ? C72 C60 C69 C68 -5.8(4) . . . . ? C72 C73 C74 C40 85.3(4) . . . . ? C72 C73 C74 C75 -38.9(4) . . . . ? C72 C73 C74 C76 -148.1(3) . . . . ? C72 C73 C78 C20 -33.2(4) . . . . ? C72 C73 C78 C77 144.3(3) . . . . ? C73 C68 C69 C60 0.4(4) . . . . ? C73 C68 C69 C64 179.5(3) . . . . ? C73 C74 C75 C58 -163.5(3) . . . . ? C73 C74 C75 C70 19.3(4) . . . . ? C73 C74 C76 O70 -153.5(3) . . . . ? C73 C74 C76 C77 27.9(3) . . . . ? C74 C40 C41 C42 174.1(3) . . . . ? C74 C40 C45 C44 -173.3(3) . . . . ? C74 C73 C78 C20 -154.9(3) . . . . ? C74 C73 C78 C77 22.7(4) . . . . ? C74 C76 C77 C30 165.2(3) . . . . ? C74 C76 C77 C78 -15.1(4) . . . . ? C75 C58 C59 C50 0.3(4) . . . . ? C75 C58 C59 C54 -179.3(3) . . . . ? C75 C70 C71 C10 167.9(3) . . . . ? C75 C70 C71 C72 -9.9(5) . . . . ? C75 C74 C76 O70 95.5(4) . . . . ? C75 C74 C76 C77 -83.1(3) . . . . ? C76 C74 C75 C58 -56.7(4) . . . . ? C76 C74 C75 C70 126.1(3) . . . . ? C76 C77 C78 C20 171.8(3) . . . . ? C76 C77 C78 C73 -5.5(4) . . . . ? C77 C30 C31 C32 -178.7(3) . . . . ? C77 C30 C35 C34 179.3(3) . . . . ? C78 C20 C21 C22 -174.4(3) . . . . ? C78 C20 C25 C24 175.6(3) . . . . ? C78 C73 C74 C40 -155.6(3) . . . . ? C78 C73 C74 C75 80.2(3) . . . . ? C78 C73 C74 C76 -29.0(3) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 969865' ####################################################################### # # 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_p-1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H32 O' _chemical_formula_weight 684.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 11.797(2) _cell_length_b 17.099(3) _cell_length_c 18.309(3) _cell_angle_alpha 72.282(4) _cell_angle_beta 89.938(4) _cell_angle_gamma 85.625(4) _cell_volume 3506.9(11) _cell_formula_units_Z 4 _cell_measurement_temperature 408(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9668 _exptl_absorpt_correction_T_max 0.9843 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 408(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 37714 _diffrn_reflns_av_R_equivalents 0.1132 _diffrn_reflns_av_sigmaI/netI 0.1393 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12347 _reflns_number_gt 6515 _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^)+(0.0331P)^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 12347 _refine_ls_number_parameters 974 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0982 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1101 _refine_ls_wR_factor_gt 0.1013 _refine_ls_goodness_of_fit_ref 0.821 _refine_ls_restrained_S_all 0.821 _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 1.17690(14) 0.11982(10) 0.16352(10) 0.0329(5) Uani 1 1 d . . . C1 C 1.0799(2) 0.14158(14) 0.13932(15) 0.0229(6) Uani 1 1 d . . . C2 C 0.97575(19) 0.10441(14) 0.17154(14) 0.0203(6) Uani 1 1 d . . . C3 C 0.88912(19) 0.13281(14) 0.11880(14) 0.0197(6) Uani 1 1 d . . . C4 C 0.92029(19) 0.20322(14) 0.04974(14) 0.0187(6) Uani 1 1 d . . . C5 C 1.04813(19) 0.21717(14) 0.06722(14) 0.0203(6) Uani 1 1 d . . . C6 C 1.0554(2) 0.29128(14) 0.09455(14) 0.0204(6) Uani 1 1 d . . . C7 C 0.9658(2) 0.34418(14) 0.09932(13) 0.0197(6) Uani 1 1 d . . . C8 C 0.84938(19) 0.33428(14) 0.07872(13) 0.0199(6) Uani 1 1 d . . . C9 C 0.82905(19) 0.27078(14) 0.05298(14) 0.0205(6) Uani 1 1 d . . . C11 C 1.1609(2) 0.31922(14) 0.11783(13) 0.0197(6) Uani 1 1 d . . . C12 C 1.2744(2) 0.29373(15) 0.12253(14) 0.0257(6) Uani 1 1 d . . . H12A H 1.3000 0.2467 0.1101 0.031 Uiso 1 1 calc R . . C13 C 1.3520(2) 0.34082(15) 0.14688(15) 0.0287(7) Uani 1 1 d . . . H13A H 1.4291 0.3238 0.1500 0.034 Uiso 1 1 calc R . . C14 C 1.3178(2) 0.40991(16) 0.16577(15) 0.0295(7) Uani 1 1 d . . . H14A H 1.3716 0.4390 0.1813 0.035 Uiso 1 1 calc R . . C15 C 1.2011(2) 0.43810(15) 0.16198(14) 0.0242(6) Uani 1 1 d . . . C16 C 1.1507(2) 0.51003(15) 0.17606(15) 0.0295(7) Uani 1 1 d . . . H16A H 1.1958 0.5439 0.1926 0.035 Uiso 1 1 calc R . . C17 C 1.0361(2) 0.52983(15) 0.16543(15) 0.0294(7) Uani 1 1 d . . . H17A H 1.0052 0.5774 0.1748 0.035 Uiso 1 1 calc R . . C18 C 0.9625(2) 0.48051(14) 0.14060(14) 0.0251(6) Uani 1 1 d . . . H18A H 0.8849 0.4954 0.1340 0.030 Uiso 1 1 calc R . . C19 C 1.0082(2) 0.41039(14) 0.12647(14) 0.0218(6) Uani 1 1 d . . . C20 C 1.1273(2) 0.39145(14) 0.13719(13) 0.0206(6) Uani 1 1 d . . . C21 C 0.71342(19) 0.24954(14) 0.03759(14) 0.0212(6) Uani 1 1 d . . . C22 C 0.6315(2) 0.30363(15) -0.00827(15) 0.0281(6) Uani 1 1 d . . . H22A H 0.6472 0.3579 -0.0320 0.034 Uiso 1 1 calc R . . C23 C 0.5246(2) 0.27812(16) -0.01979(16) 0.0313(7) Uani 1 1 d . . . H23A H 0.4709 0.3154 -0.0520 0.038 Uiso 1 1 calc R . . C24 C 0.4980(2) 0.19951(16) 0.01541(15) 0.0315(7) Uani 1 1 d . . . H24A H 0.4259 0.1842 0.0083 0.038 Uiso 1 1 calc R . . C25 C 0.5794(2) 0.14120(15) 0.06265(15) 0.0261(6) Uani 1 1 d . . . C26 C 0.5553(2) 0.05922(16) 0.10081(15) 0.0290(7) Uani 1 1 d . . . H26A H 0.4835 0.0425 0.0949 0.035 Uiso 1 1 calc R . . C27 C 0.6350(2) 0.00465(16) 0.14579(15) 0.0293(7) Uani 1 1 d . . . H27A H 0.6170 -0.0487 0.1712 0.035 Uiso 1 1 calc R . . C28 C 0.7455(2) 0.02816(15) 0.15455(14) 0.0240(6) Uani 1 1 d . . . H28A H 0.7998 -0.0102 0.1849 0.029 Uiso 1 1 calc R . . C29 C 0.7732(2) 0.10703(14) 0.11857(14) 0.0217(6) Uani 1 1 d . . . C30 C 0.68915(19) 0.16605(15) 0.07285(14) 0.0218(6) Uani 1 1 d . . . C41 C 0.9731(2) 0.04718(14) 0.25058(14) 0.0236(6) Uani 1 1 d . . . C42 C 0.8866(2) 0.05815(16) 0.29919(16) 0.0344(7) Uani 1 1 d . . . H42A H 0.8278 0.0988 0.2804 0.041 Uiso 1 1 calc R . . C43 C 0.8867(2) 0.00981(18) 0.37459(17) 0.0429(8) Uani 1 1 d . . . H43A H 0.8289 0.0183 0.4066 0.051 Uiso 1 1 calc R . . C44 C 0.9733(3) -0.05161(18) 0.40260(17) 0.0443(8) Uani 1 1 d . . . H44A H 0.9731 -0.0848 0.4534 0.053 Uiso 1 1 calc R . . C45 C 1.0594(2) -0.06373(16) 0.35581(16) 0.0371(7) Uani 1 1 d . . . H45A H 1.1174 -0.1050 0.3750 0.045 Uiso 1 1 calc R . . C46 C 1.0602(2) -0.01446(14) 0.27987(15) 0.0282(7) Uani 1 1 d . . . H46A H 1.1190 -0.0226 0.2485 0.034 Uiso 1 1 calc R . . C51 C 1.12836(19) 0.22162(15) 0.00090(14) 0.0215(6) Uani 1 1 d . . . C52 C 1.1520(2) 0.29690(16) -0.04973(15) 0.0268(6) Uani 1 1 d . . . H52A H 1.1230 0.3450 -0.0404 0.032 Uiso 1 1 calc R . . C53 C 1.2171(2) 0.30288(19) -0.11345(16) 0.0381(7) Uani 1 1 d . . . H53A H 1.2321 0.3543 -0.1461 0.046 Uiso 1 1 calc R . . C54 C 1.2599(2) 0.2323(2) -0.12850(18) 0.0448(8) Uani 1 1 d . . . H54A H 1.3020 0.2357 -0.1722 0.054 Uiso 1 1 calc R . . C55 C 1.2397(2) 0.1562(2) -0.07792(19) 0.0439(8) Uani 1 1 d . . . H55A H 1.2698 0.1084 -0.0874 0.053 Uiso 1 1 calc R . . C56 C 1.1755(2) 0.15035(16) -0.01362(16) 0.0311(7) Uani 1 1 d . . . H56A H 1.1636 0.0989 0.0202 0.037 Uiso 1 1 calc R . . C61 C 0.90885(18) 0.18550(14) -0.02682(14) 0.0192(6) Uani 1 1 d . . . C62 C 0.89987(19) 0.25078(15) -0.09389(14) 0.0231(6) Uani 1 1 d . . . H62A H 0.8937 0.3043 -0.0911 0.028 Uiso 1 1 calc R . . C63 C 0.8999(2) 0.23826(15) -0.16486(15) 0.0262(6) Uani 1 1 d . . . H63A H 0.8953 0.2831 -0.2092 0.031 Uiso 1 1 calc R . . C64 C 0.9067(2) 0.15912(15) -0.17000(15) 0.0280(6) Uani 1 1 d . . . H64A H 0.9064 0.1503 -0.2177 0.034 Uiso 1 1 calc R . . C65 C 0.9138(2) 0.09378(15) -0.10412(15) 0.0271(6) Uani 1 1 d . . . H65A H 0.9180 0.0404 -0.1075 0.032 Uiso 1 1 calc R . . C66 C 0.91497(19) 0.10571(15) -0.03234(15) 0.0228(6) Uani 1 1 d . . . H66A H 0.9198 0.0607 0.0118 0.027 Uiso 1 1 calc R . . C71 C 0.75665(19) 0.39266(14) 0.09308(14) 0.0199(6) Uani 1 1 d . . . C72 C 0.70534(19) 0.37427(15) 0.16366(14) 0.0236(6) Uani 1 1 d . . . H72A H 0.7255 0.3244 0.2009 0.028 Uiso 1 1 calc R . . C73 C 0.6247(2) 0.42930(15) 0.17922(15) 0.0267(6) Uani 1 1 d . . . H73A H 0.5907 0.4164 0.2268 0.032 Uiso 1 1 calc R . . C74 C 0.5942(2) 0.50338(15) 0.12450(16) 0.0312(7) Uani 1 1 d . . . H74A H 0.5403 0.5407 0.1353 0.037 Uiso 1 1 calc R . . C75 C 0.6437(2) 0.52213(16) 0.05381(16) 0.0357(7) Uani 1 1 d . . . H75A H 0.6219 0.5716 0.0165 0.043 Uiso 1 1 calc R . . C76 C 0.7257(2) 0.46759(15) 0.03802(15) 0.0303(7) Uani 1 1 d . . . H76A H 0.7601 0.4811 -0.0094 0.036 Uiso 1 1 calc R . . O1A O 0.31325(16) 0.83345(12) 0.46192(11) 0.0467(5) Uani 1 1 d . . . C1A C 0.4128(2) 0.80622(16) 0.47165(16) 0.0315(7) Uani 1 1 d . . . C2A C 0.4943(2) 0.80650(15) 0.41143(15) 0.0265(6) Uani 1 1 d . . . C3A C 0.5987(2) 0.77540(14) 0.44375(15) 0.0254(6) Uani 1 1 d . . . C4A C 0.5982(2) 0.74462(15) 0.53177(14) 0.0251(6) Uani 1 1 d . . . C5A C 0.4698(2) 0.76394(15) 0.55284(14) 0.0263(6) Uani 1 1 d . . . C6A C 0.4102(2) 0.68728(15) 0.58846(14) 0.0274(6) Uani 1 1 d . . . C7A C 0.4593(2) 0.60877(15) 0.60172(14) 0.0272(6) Uani 1 1 d . . . C8A C 0.5769(2) 0.59059(15) 0.58433(14) 0.0266(6) Uani 1 1 d . . . C9A C 0.6413(2) 0.65315(15) 0.55009(14) 0.0257(6) Uani 1 1 d . . . C11A C 0.3705(2) 0.55052(16) 0.63353(15) 0.0305(7) Uani 1 1 d . . . C12A C 0.3641(2) 0.46570(17) 0.65507(15) 0.0358(7) Uani 1 1 d . . . H12B H 0.4275 0.4305 0.6535 0.043 Uiso 1 1 calc R . . C13A C 0.2579(2) 0.43467(17) 0.67954(15) 0.0367(7) Uani 1 1 d . . . H13B H 0.2517 0.3783 0.6917 0.044 Uiso 1 1 calc R . . C14A C 0.1651(2) 0.48353(18) 0.68592(16) 0.0405(8) Uani 1 1 d . . . H14B H 0.0981 0.4600 0.7041 0.049 Uiso 1 1 calc R . . C15A C 0.1687(2) 0.56962(18) 0.66540(16) 0.0372(7) Uani 1 1 d . . . C16A C 0.0792(2) 0.6317(2) 0.66772(16) 0.0457(8) Uani 1 1 d . . . H16B H 0.0086 0.6154 0.6864 0.055 Uiso 1 1 calc R . . C17A C 0.0962(2) 0.71308(18) 0.64328(18) 0.0448(8) Uani 1 1 d . . . H17B H 0.0369 0.7512 0.6458 0.054 Uiso 1 1 calc R . . C18A C 0.2029(2) 0.74186(18) 0.61380(16) 0.0398(8) Uani 1 1 d . . . H18B H 0.2126 0.7979 0.5961 0.048 Uiso 1 1 calc R . . C19A C 0.2914(2) 0.68444(16) 0.61226(15) 0.0306(7) Uani 1 1 d . . . C20A C 0.2717(2) 0.59969(16) 0.63888(15) 0.0293(7) Uani 1 1 d . . . C21A C 0.7079(2) 0.76549(15) 0.40818(15) 0.0261(6) Uani 1 1 d . . . C22A C 0.7383(2) 0.81818(16) 0.33941(15) 0.0307(7) Uani 1 1 d . . . H22B H 0.6870 0.8614 0.3126 0.037 Uiso 1 1 calc R . . C23A C 0.8457(2) 0.80791(17) 0.30880(16) 0.0359(7) Uani 1 1 d . . . H23B H 0.8641 0.8431 0.2614 0.043 Uiso 1 1 calc R . . C24A C 0.9233(2) 0.74611(17) 0.34888(17) 0.0382(7) Uani 1 1 d . . . H24B H 0.9944 0.7398 0.3284 0.046 Uiso 1 1 calc R . . C25A C 0.8970(2) 0.69201(16) 0.42049(16) 0.0323(7) Uani 1 1 d . . . C26A C 0.9772(2) 0.62898(17) 0.46291(18) 0.0394(8) Uani 1 1 d . . . H26B H 1.0491 0.6221 0.4437 0.047 Uiso 1 1 calc R . . C27A C 0.9480(2) 0.57850(17) 0.53215(17) 0.0391(8) Uani 1 1 d . . . H27B H 1.0018 0.5381 0.5605 0.047 Uiso 1 1 calc R . . C28A C 0.8407(2) 0.58513(16) 0.56205(16) 0.0349(7) Uani 1 1 d . . . H28B H 0.8244 0.5491 0.6096 0.042 Uiso 1 1 calc R . . C29A C 0.7579(2) 0.64403(15) 0.52265(15) 0.0272(6) Uani 1 1 d . . . C30A C 0.7872(2) 0.69989(15) 0.45087(15) 0.0268(6) Uani 1 1 d . . . C41A C 0.4598(2) 0.83481(16) 0.32922(15) 0.0283(7) Uani 1 1 d . . . C42A C 0.4898(2) 0.78651(17) 0.28187(15) 0.0329(7) Uani 1 1 d . . . H42B H 0.5348 0.7374 0.3016 0.039 Uiso 1 1 calc R . . C43A C 0.4535(2) 0.81082(18) 0.20594(16) 0.0390(8) Uani 1 1 d . . . H43B H 0.4737 0.7781 0.1749 0.047 Uiso 1 1 calc R . . C44A C 0.3867(2) 0.8841(2) 0.17629(18) 0.0457(8) Uani 1 1 d . . . H44B H 0.3629 0.9012 0.1251 0.055 Uiso 1 1 calc R . . C45A C 0.3559(2) 0.93125(17) 0.22276(16) 0.0340(7) Uani 1 1 d . . . H45B H 0.3101 0.9799 0.2028 0.041 Uiso 1 1 calc R . . C46A C 0.3915(2) 0.90807(16) 0.29849(16) 0.0337(7) Uani 1 1 d . . . H46B H 0.3702 0.9411 0.3291 0.040 Uiso 1 1 calc R . . C51A C 0.6822(2) 0.78663(15) 0.56839(14) 0.0262(6) Uani 1 1 d . . . C52A C 0.7100(2) 0.86634(16) 0.53201(16) 0.0364(7) Uani 1 1 d . . . H52B H 0.6826 0.8934 0.4824 0.044 Uiso 1 1 calc R . . C53A C 0.7787(2) 0.90653(18) 0.56917(17) 0.0434(8) Uani 1 1 d . . . H53B H 0.7948 0.9607 0.5451 0.052 Uiso 1 1 calc R . . C54A C 0.8223(2) 0.86530(18) 0.64142(17) 0.0424(8) Uani 1 1 d . . . H54B H 0.8686 0.8912 0.6664 0.051 Uiso 1 1 calc R . . C55A C 0.7968(2) 0.78538(18) 0.67663(16) 0.0419(8) Uani 1 1 d . . . H55B H 0.8269 0.7574 0.7253 0.050 Uiso 1 1 calc R . . C56A C 0.7282(2) 0.74679(17) 0.64107(15) 0.0338(7) Uani 1 1 d . . . H56B H 0.7120 0.6929 0.6660 0.041 Uiso 1 1 calc R . . C61A C 0.4577(2) 0.82076(15) 0.60308(16) 0.0284(7) Uani 1 1 d . . . C62A C 0.4623(2) 0.78751(17) 0.68256(16) 0.0348(7) Uani 1 1 d . . . H62B H 0.4705 0.7306 0.7042 0.042 Uiso 1 1 calc R . . C63A C 0.4551(2) 0.83648(18) 0.73045(17) 0.0438(8) Uani 1 1 d . . . H63B H 0.4563 0.8125 0.7834 0.053 Uiso 1 1 calc R . . C64A C 0.4463(2) 0.91990(18) 0.69978(19) 0.0454(8) Uani 1 1 d . . . H64B H 0.4447 0.9532 0.7316 0.054 Uiso 1 1 calc R . . C65A C 0.4400(3) 0.95458(18) 0.62198(19) 0.0489(9) Uani 1 1 d . . . H65B H 0.4325 1.0116 0.6013 0.059 Uiso 1 1 calc R . . C66A C 0.4445(2) 0.90629(16) 0.57357(17) 0.0407(8) Uani 1 1 d . . . H66B H 0.4386 0.9311 0.5208 0.049 Uiso 1 1 calc R . . C71A C 0.6225(2) 0.50210(15) 0.60580(15) 0.0290(7) Uani 1 1 d . . . C72A C 0.6503(2) 0.46376(16) 0.55132(17) 0.0359(7) Uani 1 1 d . . . H72B H 0.6394 0.4928 0.4996 0.043 Uiso 1 1 calc R . . C73A C 0.6946(2) 0.38150(17) 0.57326(18) 0.0398(8) Uani 1 1 d . . . H73B H 0.7129 0.3559 0.5362 0.048 Uiso 1 1 calc R . . C74A C 0.7111(2) 0.33879(17) 0.64929(19) 0.0400(8) Uani 1 1 d . . . H74B H 0.7423 0.2845 0.6638 0.048 Uiso 1 1 calc R . . C75A C 0.6814(2) 0.37620(17) 0.70488(18) 0.0416(8) Uani 1 1 d . . . H75B H 0.6911 0.3467 0.7566 0.050 Uiso 1 1 calc R . . C76A C 0.6371(2) 0.45779(16) 0.68310(16) 0.0339(7) Uani 1 1 d . . . H76B H 0.6172 0.4829 0.7203 0.041 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 0.0202(11) 0.0249(10) 0.0473(13) -0.0023(9) -0.0104(9) 0.0009(8) C1 0.0228(16) 0.0155(14) 0.0329(16) -0.0118(12) -0.0045(13) 0.0014(12) C2 0.0197(14) 0.0158(13) 0.0260(16) -0.0077(12) -0.0004(12) 0.0001(11) C3 0.0198(14) 0.0152(13) 0.0266(16) -0.0105(12) 0.0010(12) 0.0011(11) C4 0.0172(14) 0.0136(13) 0.0254(15) -0.0066(12) -0.0029(11) 0.0001(11) C5 0.0164(14) 0.0181(14) 0.0264(16) -0.0069(12) -0.0024(11) 0.0001(11) C6 0.0230(15) 0.0157(13) 0.0221(15) -0.0046(12) -0.0002(11) -0.0033(11) C7 0.0220(14) 0.0166(14) 0.0196(14) -0.0038(12) -0.0005(11) -0.0028(11) C8 0.0226(15) 0.0164(14) 0.0192(15) -0.0030(12) -0.0008(11) -0.0019(11) C9 0.0197(14) 0.0177(14) 0.0232(15) -0.0051(12) -0.0020(11) -0.0002(11) C11 0.0195(14) 0.0194(14) 0.0197(15) -0.0050(12) -0.0030(11) -0.0014(11) C12 0.0255(16) 0.0248(15) 0.0278(16) -0.0094(13) -0.0023(12) -0.0030(12) C13 0.0208(15) 0.0317(16) 0.0339(17) -0.0103(14) -0.0050(12) -0.0019(13) C14 0.0256(16) 0.0301(16) 0.0345(17) -0.0103(14) -0.0060(13) -0.0104(13) C15 0.0278(16) 0.0202(14) 0.0244(16) -0.0059(12) -0.0027(12) -0.0051(12) C16 0.0361(18) 0.0238(15) 0.0324(17) -0.0121(13) -0.0032(13) -0.0120(13) C17 0.0357(17) 0.0214(15) 0.0329(17) -0.0102(13) -0.0002(13) -0.0051(13) C18 0.0227(15) 0.0226(15) 0.0315(16) -0.0103(13) -0.0018(12) -0.0025(12) C19 0.0259(15) 0.0185(14) 0.0197(15) -0.0031(12) 0.0004(12) -0.0050(12) C20 0.0215(15) 0.0201(14) 0.0205(15) -0.0056(12) -0.0002(11) -0.0052(12) C21 0.0189(14) 0.0215(14) 0.0261(15) -0.0112(12) 0.0012(12) -0.0017(12) C22 0.0252(15) 0.0207(15) 0.0386(18) -0.0101(13) -0.0032(13) 0.0008(12) C23 0.0210(15) 0.0334(17) 0.0422(19) -0.0177(15) -0.0106(13) 0.0060(13) C24 0.0207(15) 0.0329(17) 0.0446(19) -0.0174(15) -0.0068(13) -0.0011(13) C25 0.0206(15) 0.0270(16) 0.0359(17) -0.0174(14) -0.0006(12) -0.0023(12) C26 0.0206(15) 0.0304(16) 0.0409(18) -0.0172(14) 0.0030(13) -0.0072(13) C27 0.0290(16) 0.0229(15) 0.0377(18) -0.0109(14) 0.0069(13) -0.0057(13) C28 0.0238(15) 0.0232(15) 0.0254(16) -0.0083(13) -0.0009(12) -0.0009(12) C29 0.0215(14) 0.0211(15) 0.0247(15) -0.0099(12) 0.0002(12) -0.0034(12) C30 0.0180(14) 0.0260(15) 0.0257(16) -0.0140(13) 0.0025(11) -0.0030(12) C41 0.0256(15) 0.0211(15) 0.0254(16) -0.0081(13) -0.0033(12) -0.0045(12) C42 0.0351(17) 0.0344(17) 0.0324(18) -0.0084(15) 0.0010(14) -0.0022(14) C43 0.0446(19) 0.049(2) 0.0311(19) -0.0060(16) 0.0085(15) -0.0038(16) C44 0.055(2) 0.0425(19) 0.0287(18) -0.0006(15) -0.0029(16) -0.0073(17) C45 0.0421(19) 0.0284(16) 0.0355(19) -0.0019(15) -0.0165(15) -0.0025(14) C46 0.0290(16) 0.0221(15) 0.0348(18) -0.0100(14) -0.0072(13) -0.0046(13) C51 0.0140(14) 0.0270(15) 0.0275(16) -0.0143(13) -0.0047(11) -0.0011(12) C52 0.0224(15) 0.0319(16) 0.0284(17) -0.0126(14) -0.0021(12) -0.0026(12) C53 0.0292(17) 0.055(2) 0.0322(18) -0.0146(16) 0.0014(14) -0.0109(15) C54 0.0238(17) 0.081(3) 0.041(2) -0.034(2) 0.0050(14) -0.0145(17) C55 0.0242(17) 0.064(2) 0.064(2) -0.051(2) 0.0023(16) 0.0025(16) C56 0.0202(15) 0.0332(16) 0.0472(19) -0.0230(15) -0.0017(14) -0.0024(13) C61 0.0132(13) 0.0203(14) 0.0234(15) -0.0055(12) -0.0010(11) -0.0030(11) C62 0.0215(15) 0.0187(14) 0.0284(17) -0.0061(13) -0.0011(12) -0.0016(11) C63 0.0290(16) 0.0248(15) 0.0218(16) -0.0028(13) -0.0028(12) -0.0019(12) C64 0.0310(16) 0.0320(17) 0.0244(16) -0.0126(14) -0.0021(12) -0.0066(13) C65 0.0283(16) 0.0205(15) 0.0360(18) -0.0132(14) -0.0007(13) -0.0059(12) C66 0.0215(15) 0.0196(14) 0.0275(16) -0.0071(12) -0.0030(12) -0.0021(11) C71 0.0179(14) 0.0175(14) 0.0255(16) -0.0080(12) -0.0034(11) -0.0028(11) C72 0.0219(15) 0.0198(14) 0.0269(16) -0.0039(12) -0.0029(12) -0.0012(12) C73 0.0226(15) 0.0296(16) 0.0290(17) -0.0108(14) 0.0028(12) -0.0019(13) C74 0.0278(16) 0.0251(16) 0.0423(19) -0.0144(15) 0.0038(14) 0.0062(13) C75 0.0379(18) 0.0226(15) 0.0397(19) -0.0028(14) 0.0034(14) 0.0116(13) C76 0.0342(17) 0.0244(15) 0.0305(17) -0.0059(13) 0.0070(13) -0.0006(13) O1A 0.0291(12) 0.0598(14) 0.0405(13) -0.0029(11) -0.0051(10) 0.0113(10) C1A 0.0276(17) 0.0289(16) 0.0366(18) -0.0084(14) -0.0033(14) -0.0006(13) C2A 0.0268(16) 0.0227(15) 0.0289(17) -0.0061(13) -0.0010(13) -0.0021(12) C3A 0.0269(16) 0.0204(15) 0.0292(16) -0.0075(13) -0.0024(13) -0.0032(12) C4A 0.0215(15) 0.0254(15) 0.0265(16) -0.0053(13) -0.0020(12) -0.0019(12) C5A 0.0262(15) 0.0262(15) 0.0240(16) -0.0045(13) -0.0028(12) -0.0005(12) C6A 0.0270(16) 0.0291(16) 0.0257(16) -0.0072(13) -0.0001(12) -0.0052(13) C7A 0.0299(16) 0.0279(16) 0.0239(16) -0.0072(13) -0.0016(12) -0.0053(13) C8A 0.0299(16) 0.0227(15) 0.0257(16) -0.0057(13) -0.0064(12) -0.0007(13) C9A 0.0276(16) 0.0248(15) 0.0232(16) -0.0052(13) -0.0067(12) -0.0017(13) C11A 0.0355(17) 0.0323(17) 0.0255(16) -0.0098(13) -0.0041(13) -0.0086(14) C12A 0.0387(18) 0.0370(18) 0.0343(18) -0.0124(15) -0.0007(14) -0.0119(14) C13A 0.0439(19) 0.0320(17) 0.0346(18) -0.0080(14) 0.0036(14) -0.0141(15) C14A 0.0412(19) 0.046(2) 0.0324(18) -0.0056(16) 0.0011(14) -0.0167(16) C15A 0.0316(18) 0.051(2) 0.0312(18) -0.0129(16) 0.0006(14) -0.0132(15) C16A 0.0265(18) 0.069(2) 0.0370(19) -0.0066(17) 0.0010(14) -0.0136(17) C17A 0.0281(18) 0.040(2) 0.064(2) -0.0133(17) -0.0066(16) 0.0011(15) C18A 0.0299(17) 0.0426(18) 0.049(2) -0.0169(16) 0.0039(15) -0.0020(15) C19A 0.0274(16) 0.0359(17) 0.0296(17) -0.0112(14) -0.0015(13) -0.0036(14) C20A 0.0274(16) 0.0357(17) 0.0250(16) -0.0093(13) -0.0007(12) -0.0047(14) C21A 0.0245(15) 0.0284(16) 0.0274(16) -0.0111(13) -0.0021(13) -0.0043(13) C22A 0.0286(16) 0.0327(16) 0.0273(17) -0.0042(14) -0.0038(13) -0.0020(13) C23A 0.0319(17) 0.0381(18) 0.0339(18) -0.0044(15) 0.0046(14) -0.0060(14) C24A 0.0292(17) 0.0465(19) 0.041(2) -0.0148(16) 0.0097(15) -0.0112(15) C25A 0.0238(16) 0.0338(17) 0.0424(19) -0.0159(15) 0.0011(14) -0.0045(13) C26A 0.0266(17) 0.0396(18) 0.053(2) -0.0180(17) 0.0022(15) 0.0046(14) C27A 0.0328(18) 0.0381(18) 0.044(2) -0.0100(16) -0.0008(15) 0.0019(14) C28A 0.0317(17) 0.0305(17) 0.0410(19) -0.0092(15) -0.0041(14) 0.0000(14) C29A 0.0272(16) 0.0247(15) 0.0312(17) -0.0106(13) -0.0016(13) -0.0033(13) C30A 0.0272(16) 0.0245(15) 0.0328(17) -0.0144(14) -0.0014(13) -0.0027(12) C41A 0.0199(15) 0.0348(17) 0.0311(17) -0.0099(14) -0.0005(12) -0.0083(13) C42A 0.0311(16) 0.0348(17) 0.0327(18) -0.0090(15) -0.0033(13) -0.0082(13) C43A 0.0352(18) 0.054(2) 0.0334(19) -0.0179(16) -0.0003(14) -0.0164(16) C44A 0.0257(17) 0.065(2) 0.0349(19) 0.0053(18) -0.0079(14) -0.0185(16) C45A 0.0206(16) 0.0423(18) 0.0320(18) -0.0021(15) -0.0034(13) 0.0042(13) C46A 0.0219(15) 0.0371(17) 0.0376(19) -0.0056(15) -0.0017(13) 0.0013(13) C51A 0.0281(16) 0.0282(16) 0.0230(16) -0.0086(13) -0.0017(12) -0.0031(12) C52A 0.0441(19) 0.0350(18) 0.0277(17) -0.0049(14) -0.0040(14) -0.0065(14) C53A 0.058(2) 0.0361(18) 0.0351(19) -0.0048(15) -0.0062(16) -0.0265(16) C54A 0.0454(19) 0.054(2) 0.0347(19) -0.0201(17) -0.0039(15) -0.0226(16) C55A 0.0404(19) 0.053(2) 0.0267(17) -0.0016(16) -0.0092(14) -0.0103(16) C56A 0.0415(18) 0.0313(16) 0.0284(17) -0.0081(14) -0.0018(14) -0.0059(14) C61A 0.0236(15) 0.0272(16) 0.0355(18) -0.0109(14) 0.0008(13) -0.0028(12) C62A 0.0454(18) 0.0288(16) 0.0309(18) -0.0092(14) 0.0044(14) -0.0072(14) C63A 0.061(2) 0.0405(19) 0.0333(19) -0.0160(16) 0.0037(15) -0.0038(16) C64A 0.054(2) 0.041(2) 0.047(2) -0.0237(18) 0.0092(17) -0.0008(16) C65A 0.065(2) 0.0249(17) 0.058(2) -0.0154(17) 0.0030(18) 0.0013(15) C66A 0.055(2) 0.0262(17) 0.0377(19) -0.0056(15) 0.0048(15) -0.0006(15) C71A 0.0286(16) 0.0257(16) 0.0324(18) -0.0082(14) -0.0015(13) -0.0028(13) C72A 0.0357(17) 0.0320(17) 0.0402(19) -0.0121(15) -0.0035(14) -0.0006(14) C73A 0.0420(19) 0.0394(19) 0.044(2) -0.0218(17) -0.0003(15) -0.0030(15) C74A 0.0348(18) 0.0266(17) 0.058(2) -0.0108(17) -0.0071(16) -0.0039(14) C75A 0.0448(19) 0.0321(18) 0.044(2) -0.0057(16) -0.0109(15) -0.0046(15) C76A 0.0387(18) 0.0296(17) 0.0315(18) -0.0070(14) -0.0049(14) -0.0008(14) _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 C1 1.216(3) . ? C1 C2 1.467(3) . ? C1 C5 1.563(3) . ? C2 C3 1.362(3) . ? C2 C41 1.482(3) . ? C3 C29 1.469(3) . ? C3 C4 1.524(3) . ? C4 C61 1.530(3) . ? C4 C9 1.533(3) . ? C4 C5 1.593(3) . ? C5 C6 1.506(3) . ? C5 C51 1.526(3) . ? C6 C7 1.358(3) . ? C6 C11 1.475(3) . ? C7 C8 1.461(3) . ? C7 C19 1.486(3) . ? C8 C9 1.345(3) . ? C8 C71 1.502(3) . ? C9 C21 1.487(3) . ? C11 C12 1.370(3) . ? C11 C20 1.414(3) . ? C12 C13 1.421(3) . ? C12 H12A 0.9300 . ? C13 C14 1.362(3) . ? C13 H13A 0.9300 . ? C14 C15 1.418(3) . ? C14 H14A 0.9300 . ? C15 C20 1.388(3) . ? C15 C16 1.419(3) . ? C16 C17 1.367(3) . ? C16 H16A 0.9300 . ? C17 C18 1.420(3) . ? C17 H17A 0.9300 . ? C18 C19 1.373(3) . ? C18 H18A 0.9300 . ? C19 C20 1.417(3) . ? C21 C22 1.374(3) . ? C21 C30 1.427(3) . ? C22 C23 1.402(3) . ? C22 H22A 0.9300 . ? C23 C24 1.363(3) . ? C23 H23A 0.9300 . ? C24 C25 1.413(3) . ? C24 H24A 0.9300 . ? C25 C26 1.414(3) . ? C25 C30 1.422(3) . ? C26 C27 1.354(3) . ? C26 H26A 0.9300 . ? C27 C28 1.417(3) . ? C27 H27A 0.9300 . ? C28 C29 1.373(3) . ? C28 H28A 0.9300 . ? C29 C30 1.428(3) . ? C41 C42 1.392(3) . ? C41 C46 1.395(3) . ? C42 C43 1.376(4) . ? C42 H42A 0.9300 . ? C43 C44 1.386(4) . ? C43 H43A 0.9300 . ? C44 C45 1.372(4) . ? C44 H44A 0.9300 . ? C45 C46 1.390(4) . ? C45 H45A 0.9300 . ? C46 H46A 0.9300 . ? C51 C52 1.386(3) . ? C51 C56 1.400(3) . ? C52 C53 1.378(3) . ? C52 H52A 0.9300 . ? C53 C54 1.377(4) . ? C53 H53A 0.9300 . ? C54 C55 1.387(4) . ? C54 H54A 0.9300 . ? C55 C56 1.381(4) . ? C55 H55A 0.9300 . ? C56 H56A 0.9300 . ? C61 C62 1.383(3) . ? C61 C66 1.395(3) . ? C62 C63 1.380(3) . ? C62 H62A 0.9300 . ? C63 C64 1.381(3) . ? C63 H63A 0.9300 . ? C64 C65 1.370(3) . ? C64 H64A 0.9300 . ? C65 C66 1.390(3) . ? C65 H65A 0.9300 . ? C66 H66A 0.9300 . ? C71 C72 1.384(3) . ? C71 C76 1.391(3) . ? C72 C73 1.378(3) . ? C72 H72A 0.9300 . ? C73 C74 1.377(3) . ? C73 H73A 0.9300 . ? C74 C75 1.376(4) . ? C74 H74A 0.9300 . ? C75 C76 1.384(3) . ? C75 H75A 0.9300 . ? C76 H76A 0.9300 . ? O1A C1A 1.223(3) . ? C1A C2A 1.461(4) . ? C1A C5A 1.568(3) . ? C2A C3A 1.364(3) . ? C2A C41A 1.481(4) . ? C3A C21A 1.464(3) . ? C3A C4A 1.536(3) . ? C4A C51A 1.534(3) . ? C4A C9A 1.542(3) . ? C4A C5A 1.597(3) . ? C5A C6A 1.503(3) . ? C5A C61A 1.527(3) . ? C6A C7A 1.371(3) . ? C6A C19A 1.467(3) . ? C7A C8A 1.455(3) . ? C7A C11A 1.495(3) . ? C8A C9A 1.352(3) . ? C8A C71A 1.499(3) . ? C9A C29A 1.477(3) . ? C11A C12A 1.390(3) . ? C11A C20A 1.405(3) . ? C12A C13A 1.417(4) . ? C12A H12B 0.9300 . ? C13A C14A 1.352(3) . ? C13A H13B 0.9300 . ? C14A C15A 1.408(4) . ? C14A H14B 0.9300 . ? C15A C20A 1.386(3) . ? C15A C16A 1.448(4) . ? C16A C17A 1.357(4) . ? C16A H16B 0.9300 . ? C17A C18A 1.431(4) . ? C17A H17B 0.9300 . ? C18A C19A 1.383(3) . ? C18A H18B 0.9300 . ? C19A C20A 1.419(3) . ? C21A C22A 1.373(3) . ? C21A C30A 1.432(3) . ? C22A C23A 1.406(3) . ? C22A H22B 0.9300 . ? C23A C24A 1.369(4) . ? C23A H23B 0.9300 . ? C24A C25A 1.406(4) . ? C24A H24B 0.9300 . ? C25A C26A 1.414(4) . ? C25A C30A 1.422(3) . ? C26A C27A 1.360(4) . ? C26A H26B 0.9300 . ? C27A C28A 1.389(4) . ? C27A H27B 0.9300 . ? C28A C29A 1.378(3) . ? C28A H28B 0.9300 . ? C29A C30A 1.430(3) . ? C41A C42A 1.396(3) . ? C41A C46A 1.397(3) . ? C42A C43A 1.383(4) . ? C42A H42B 0.9300 . ? C43A C44A 1.386(4) . ? C43A H43B 0.9300 . ? C44A C45A 1.370(4) . ? C44A H44B 0.9300 . ? C45A C46A 1.377(4) . ? C45A H45B 0.9300 . ? C46A H46B 0.9300 . ? C51A C56A 1.387(3) . ? C51A C52A 1.387(3) . ? C52A C53A 1.402(4) . ? C52A H52B 0.9300 . ? C53A C54A 1.374(4) . ? C53A H53B 0.9300 . ? C54A C55A 1.378(4) . ? C54A H54B 0.9300 . ? C55A C56A 1.363(4) . ? C55A H55B 0.9300 . ? C56A H56B 0.9300 . ? C61A C62A 1.391(4) . ? C61A C66A 1.393(3) . ? C62A C63A 1.383(4) . ? C62A H62B 0.9300 . ? C63A C64A 1.360(4) . ? C63A H63B 0.9300 . ? C64A C65A 1.366(4) . ? C64A H64B 0.9300 . ? C65A C66A 1.382(4) . ? C65A H65B 0.9300 . ? C66A H66B 0.9300 . ? C71A C72A 1.377(3) . ? C71A C76A 1.391(3) . ? C72A C73A 1.399(3) . ? C72A H72B 0.9300 . ? C73A C74A 1.367(4) . ? C73A H73B 0.9300 . ? C74A C75A 1.389(4) . ? C74A H74B 0.9300 . ? C75A C76A 1.389(3) . ? C75A H75B 0.9300 . ? C76A H76B 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 127.3(2) . . ? O1 C1 C5 123.5(2) . . ? C2 C1 C5 109.20(19) . . ? C3 C2 C1 109.2(2) . . ? C3 C2 C41 128.9(2) . . ? C1 C2 C41 121.9(2) . . ? C2 C3 C29 130.6(2) . . ? C2 C3 C4 113.0(2) . . ? C29 C3 C4 116.4(2) . . ? C3 C4 C61 113.77(19) . . ? C3 C4 C9 100.66(18) . . ? C61 C4 C9 109.22(19) . . ? C3 C4 C5 104.45(18) . . ? C61 C4 C5 111.56(18) . . ? C9 C4 C5 116.76(18) . . ? C6 C5 C51 110.23(19) . . ? C6 C5 C1 104.89(19) . . ? C51 C5 C1 112.92(19) . . ? C6 C5 C4 112.04(18) . . ? C51 C5 C4 114.31(19) . . ? C1 C5 C4 101.83(18) . . ? C7 C6 C11 109.5(2) . . ? C7 C6 C5 125.0(2) . . ? C11 C6 C5 125.4(2) . . ? C6 C7 C8 122.9(2) . . ? C6 C7 C19 108.8(2) . . ? C8 C7 C19 128.4(2) . . ? C9 C8 C7 119.2(2) . . ? C9 C8 C71 123.1(2) . . ? C7 C8 C71 117.6(2) . . ? C8 C9 C21 124.1(2) . . ? C8 C9 C4 123.6(2) . . ? C21 C9 C4 111.52(19) . . ? C12 C11 C20 118.1(2) . . ? C12 C11 C6 136.2(2) . . ? C20 C11 C6 105.6(2) . . ? C11 C12 C13 118.5(2) . . ? C11 C12 H12A 120.8 . . ? C13 C12 H12A 120.8 . . ? C14 C13 C12 122.5(2) . . ? C14 C13 H13A 118.8 . . ? C12 C13 H13A 118.8 . . ? C13 C14 C15 120.8(2) . . ? C13 C14 H14A 119.6 . . ? C15 C14 H14A 119.6 . . ? C20 C15 C14 115.5(2) . . ? C20 C15 C16 115.8(2) . . ? C14 C15 C16 128.5(2) . . ? C17 C16 C15 120.4(2) . . ? C17 C16 H16A 119.8 . . ? C15 C16 H16A 119.8 . . ? C16 C17 C18 122.5(2) . . ? C16 C17 H17A 118.7 . . ? C18 C17 H17A 118.7 . . ? C19 C18 C17 118.7(2) . . ? C19 C18 H18A 120.6 . . ? C17 C18 H18A 120.6 . . ? C18 C19 C20 117.8(2) . . ? C18 C19 C7 136.7(2) . . ? C20 C19 C7 105.47(19) . . ? C15 C20 C11 124.6(2) . . ? C15 C20 C19 124.8(2) . . ? C11 C20 C19 110.6(2) . . ? C22 C21 C30 119.1(2) . . ? C22 C21 C9 124.8(2) . . ? C30 C21 C9 116.1(2) . . ? C21 C22 C23 120.9(2) . . ? C21 C22 H22A 119.6 . . ? C23 C22 H22A 119.6 . . ? C24 C23 C22 121.1(2) . . ? C24 C23 H23A 119.5 . . ? C22 C23 H23A 119.5 . . ? C23 C24 C25 120.3(2) . . ? C23 C24 H24A 119.8 . . ? C25 C24 H24A 119.8 . . ? C24 C25 C26 122.2(2) . . ? C24 C25 C30 118.9(2) . . ? C26 C25 C30 118.9(2) . . ? C27 C26 C25 121.0(2) . . ? C27 C26 H26A 119.5 . . ? C25 C26 H26A 119.5 . . ? C26 C27 C28 120.6(2) . . ? C26 C27 H27A 119.7 . . ? C28 C27 H27A 119.7 . . ? C29 C28 C27 120.6(2) . . ? C29 C28 H28A 119.7 . . ? C27 C28 H28A 119.7 . . ? C28 C29 C30 119.5(2) . . ? C28 C29 C3 123.1(2) . . ? C30 C29 C3 117.1(2) . . ? C25 C30 C21 119.6(2) . . ? C25 C30 C29 119.4(2) . . ? C21 C30 C29 121.0(2) . . ? C42 C41 C46 118.5(2) . . ? C42 C41 C2 119.9(2) . . ? C46 C41 C2 121.5(2) . . ? C43 C42 C41 121.1(3) . . ? C43 C42 H42A 119.4 . . ? C41 C42 H42A 119.4 . . ? C42 C43 C44 119.6(3) . . ? C42 C43 H43A 120.2 . . ? C44 C43 H43A 120.2 . . ? C45 C44 C43 120.3(3) . . ? C45 C44 H44A 119.8 . . ? C43 C44 H44A 119.8 . . ? C44 C45 C46 120.1(3) . . ? C44 C45 H45A 119.9 . . ? C46 C45 H45A 119.9 . . ? C45 C46 C41 120.3(3) . . ? C45 C46 H46A 119.9 . . ? C41 C46 H46A 119.9 . . ? C52 C51 C56 117.6(2) . . ? C52 C51 C5 120.8(2) . . ? C56 C51 C5 121.5(2) . . ? C53 C52 C51 122.2(3) . . ? C53 C52 H52A 118.9 . . ? C51 C52 H52A 118.9 . . ? C54 C53 C52 119.6(3) . . ? C54 C53 H53A 120.2 . . ? C52 C53 H53A 120.2 . . ? C53 C54 C55 119.4(3) . . ? C53 C54 H54A 120.3 . . ? C55 C54 H54A 120.3 . . ? C56 C55 C54 120.8(3) . . ? C56 C55 H55A 119.6 . . ? C54 C55 H55A 119.6 . . ? C55 C56 C51 120.3(3) . . ? C55 C56 H56A 119.9 . . ? C51 C56 H56A 119.9 . . ? C62 C61 C66 118.3(2) . . ? C62 C61 C4 119.0(2) . . ? C66 C61 C4 122.6(2) . . ? C63 C62 C61 121.5(2) . . ? C63 C62 H62A 119.3 . . ? C61 C62 H62A 119.2 . . ? C62 C63 C64 120.0(2) . . ? C62 C63 H63A 120.0 . . ? C64 C63 H63A 120.0 . . ? C65 C64 C63 119.3(2) . . ? C65 C64 H64A 120.4 . . ? C63 C64 H64A 120.4 . . ? C64 C65 C66 121.2(2) . . ? C64 C65 H65A 119.4 . . ? C66 C65 H65A 119.4 . . ? C65 C66 C61 119.8(2) . . ? C65 C66 H66A 120.1 . . ? C61 C66 H66A 120.1 . . ? C72 C71 C76 119.0(2) . . ? C72 C71 C8 119.8(2) . . ? C76 C71 C8 121.0(2) . . ? C73 C72 C71 120.5(2) . . ? C73 C72 H72A 119.7 . . ? C71 C72 H72A 119.7 . . ? C74 C73 C72 120.2(2) . . ? C74 C73 H73A 119.9 . . ? C72 C73 H73A 119.9 . . ? C75 C74 C73 119.9(2) . . ? C75 C74 H74A 120.1 . . ? C73 C74 H74A 120.1 . . ? C74 C75 C76 120.2(3) . . ? C74 C75 H75A 119.9 . . ? C76 C75 H75A 119.9 . . ? C75 C76 C71 120.1(2) . . ? C75 C76 H76A 120.0 . . ? C71 C76 H76A 120.0 . . ? O1A C1A C2A 126.1(3) . . ? O1A C1A C5A 123.4(2) . . ? C2A C1A C5A 110.5(2) . . ? C3A C2A C1A 109.6(2) . . ? C3A C2A C41A 128.5(2) . . ? C1A C2A C41A 121.8(2) . . ? C2A C3A C21A 130.5(2) . . ? C2A C3A C4A 113.1(2) . . ? C21A C3A C4A 116.3(2) . . ? C51A C4A C3A 112.5(2) . . ? C51A C4A C9A 108.0(2) . . ? C3A C4A C9A 102.72(19) . . ? C51A C4A C5A 111.9(2) . . ? C3A C4A C5A 104.53(19) . . ? C9A C4A C5A 116.9(2) . . ? C6A C5A C61A 110.0(2) . . ? C6A C5A C1A 106.7(2) . . ? C61A C5A C1A 111.1(2) . . ? C6A C5A C4A 112.8(2) . . ? C61A C5A C4A 113.7(2) . . ? C1A C5A C4A 102.0(2) . . ? C7A C6A C19A 109.8(2) . . ? C7A C6A C5A 124.3(2) . . ? C19A C6A C5A 125.9(2) . . ? C6A C7A C8A 123.3(2) . . ? C6A C7A C11A 107.7(2) . . ? C8A C7A C11A 129.0(2) . . ? C9A C8A C7A 119.6(2) . . ? C9A C8A C71A 122.3(2) . . ? C7A C8A C71A 118.1(2) . . ? C8A C9A C29A 125.5(2) . . ? C8A C9A C4A 123.1(2) . . ? C29A C9A C4A 111.3(2) . . ? C12A C11A C20A 117.8(2) . . ? C12A C11A C7A 136.1(3) . . ? C20A C11A C7A 106.0(2) . . ? C11A C12A C13A 117.9(3) . . ? C11A C12A H12B 121.1 . . ? C13A C12A H12B 121.1 . . ? C14A C13A C12A 122.8(3) . . ? C14A C13A H13B 118.6 . . ? C12A C13A H13B 118.6 . . ? C13A C14A C15A 120.9(3) . . ? C13A C14A H14B 119.6 . . ? C15A C14A H14B 119.6 . . ? C20A C15A C14A 115.9(3) . . ? C20A C15A C16A 115.1(3) . . ? C14A C15A C16A 129.0(3) . . ? C17A C16A C15A 121.4(3) . . ? C17A C16A H16B 119.3 . . ? C15A C16A H16B 119.3 . . ? C16A C17A C18A 121.8(3) . . ? C16A C17A H17B 119.1 . . ? C18A C17A H17B 119.1 . . ? C19A C18A C17A 118.6(3) . . ? C19A C18A H18B 120.7 . . ? C17A C18A H18B 120.7 . . ? C18A C19A C20A 118.5(2) . . ? C18A C19A C6A 135.8(3) . . ? C20A C19A C6A 105.7(2) . . ? C15A C20A C11A 124.7(3) . . ? C15A C20A C19A 124.6(3) . . ? C11A C20A C19A 110.7(2) . . ? C22A C21A C30A 120.0(2) . . ? C22A C21A C3A 123.1(2) . . ? C30A C21A C3A 116.8(2) . . ? C21A C22A C23A 121.1(2) . . ? C21A C22A H22B 119.5 . . ? C23A C22A H22B 119.5 . . ? C24A C23A C22A 120.0(3) . . ? C24A C23A H23B 120.0 . . ? C22A C23A H23B 120.0 . . ? C23A C24A C25A 120.9(3) . . ? C23A C24A H24B 119.5 . . ? C25A C24A H24B 119.5 . . ? C24A C25A C26A 121.3(3) . . ? C24A C25A C30A 119.7(2) . . ? C26A C25A C30A 119.0(3) . . ? C27A C26A C25A 119.1(3) . . ? C27A C26A H26B 120.4 . . ? C25A C26A H26B 120.4 . . ? C26A C27A C28A 122.4(3) . . ? C26A C27A H27B 118.8 . . ? C28A C27A H27B 118.8 . . ? C29A C28A C27A 121.3(3) . . ? C29A C28A H28B 119.4 . . ? C27A C28A H28B 119.4 . . ? C28A C29A C30A 117.7(2) . . ? C28A C29A C9A 124.1(2) . . ? C30A C29A C9A 118.2(2) . . ? C25A C30A C29A 120.5(2) . . ? C25A C30A C21A 118.3(2) . . ? C29A C30A C21A 121.2(2) . . ? C42A C41A C46A 118.7(3) . . ? C42A C41A C2A 120.5(2) . . ? C46A C41A C2A 120.7(2) . . ? C43A C42A C41A 120.8(3) . . ? C43A C42A H42B 119.6 . . ? C41A C42A H42B 119.6 . . ? C42A C43A C44A 119.7(3) . . ? C42A C43A H43B 120.1 . . ? C44A C43A H43B 120.1 . . ? C45A C44A C43A 119.7(3) . . ? C45A C44A H44B 120.1 . . ? C43A C44A H44B 120.1 . . ? C44A C45A C46A 121.4(3) . . ? C44A C45A H45B 119.3 . . ? C46A C45A H45B 119.3 . . ? C45A C46A C41A 119.8(3) . . ? C45A C46A H46B 120.1 . . ? C41A C46A H46B 120.1 . . ? C56A C51A C52A 118.2(2) . . ? C56A C51A C4A 120.3(2) . . ? C52A C51A C4A 121.5(2) . . ? C51A C52A C53A 120.7(3) . . ? C51A C52A H52B 119.6 . . ? C53A C52A H52B 119.6 . . ? C54A C53A C52A 119.5(3) . . ? C54A C53A H53B 120.3 . . ? C52A C53A H53B 120.3 . . ? C53A C54A C55A 119.6(3) . . ? C53A C54A H54B 120.2 . . ? C55A C54A H54B 120.2 . . ? C56A C55A C54A 120.9(3) . . ? C56A C55A H55B 119.5 . . ? C54A C55A H55B 119.5 . . ? C55A C56A C51A 121.1(3) . . ? C55A C56A H56B 119.5 . . ? C51A C56A H56B 119.5 . . ? C62A C61A C66A 116.8(2) . . ? C62A C61A C5A 119.9(2) . . ? C66A C61A C5A 123.3(2) . . ? C63A C62A C61A 122.1(3) . . ? C63A C62A H62B 119.0 . . ? C61A C62A H62B 119.0 . . ? C64A C63A C62A 119.7(3) . . ? C64A C63A H63B 120.1 . . ? C62A C63A H63B 120.1 . . ? C63A C64A C65A 119.7(3) . . ? C63A C64A H64B 120.1 . . ? C65A C64A H64B 120.1 . . ? C64A C65A C66A 121.1(3) . . ? C64A C65A H65B 119.5 . . ? C66A C65A H65B 119.5 . . ? C65A C66A C61A 120.6(3) . . ? C65A C66A H66B 119.7 . . ? C61A C66A H66B 119.7 . . ? C72A C71A C76A 119.3(2) . . ? C72A C71A C8A 121.9(2) . . ? C76A C71A C8A 118.7(2) . . ? C71A C72A C73A 120.5(3) . . ? C71A C72A H72B 119.8 . . ? C73A C72A H72B 119.8 . . ? C74A C73A C72A 119.9(3) . . ? C74A C73A H73B 120.0 . . ? C72A C73A H73B 120.0 . . ? C73A C74A C75A 120.2(3) . . ? C73A C74A H74B 119.9 . . ? C75A C74A H74B 119.9 . . ? C74A C75A C76A 119.9(3) . . ? C74A C75A H75B 120.1 . . ? C76A C75A H75B 120.1 . . ? C75A C76A C71A 120.2(3) . . ? C75A C76A H76B 119.9 . . ? C71A C76A H76B 119.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -165.3(2) . . . . ? C5 C1 C2 C3 15.6(3) . . . . ? O1 C1 C2 C41 16.1(4) . . . . ? C5 C1 C2 C41 -162.9(2) . . . . ? C1 C2 C3 C29 171.0(2) . . . . ? C41 C2 C3 C29 -10.6(4) . . . . ? C1 C2 C3 C4 -9.5(3) . . . . ? C41 C2 C3 C4 169.0(2) . . . . ? C2 C3 C4 C61 121.6(2) . . . . ? C29 C3 C4 C61 -58.8(3) . . . . ? C2 C3 C4 C9 -121.7(2) . . . . ? C29 C3 C4 C9 57.9(2) . . . . ? C2 C3 C4 C5 -0.3(2) . . . . ? C29 C3 C4 C5 179.31(18) . . . . ? O1 C1 C5 C6 -77.0(3) . . . . ? C2 C1 C5 C6 102.1(2) . . . . ? O1 C1 C5 C51 43.0(3) . . . . ? C2 C1 C5 C51 -137.9(2) . . . . ? O1 C1 C5 C4 166.1(2) . . . . ? C2 C1 C5 C4 -14.8(2) . . . . ? C3 C4 C5 C6 -102.6(2) . . . . ? C61 C4 C5 C6 134.1(2) . . . . ? C9 C4 C5 C6 7.5(3) . . . . ? C3 C4 C5 C51 131.1(2) . . . . ? C61 C4 C5 C51 7.8(3) . . . . ? C9 C4 C5 C51 -118.8(2) . . . . ? C3 C4 C5 C1 9.0(2) . . . . ? C61 C4 C5 C1 -114.3(2) . . . . ? C9 C4 C5 C1 119.1(2) . . . . ? C51 C5 C6 C7 124.3(2) . . . . ? C1 C5 C6 C7 -113.9(3) . . . . ? C4 C5 C6 C7 -4.2(3) . . . . ? C51 C5 C6 C11 -53.6(3) . . . . ? C1 C5 C6 C11 68.3(3) . . . . ? C4 C5 C6 C11 177.9(2) . . . . ? C11 C6 C7 C8 178.9(2) . . . . ? C5 C6 C7 C8 0.7(4) . . . . ? C11 C6 C7 C19 -0.1(3) . . . . ? C5 C6 C7 C19 -178.3(2) . . . . ? C6 C7 C8 C9 -0.8(4) . . . . ? C19 C7 C8 C9 178.0(2) . . . . ? C6 C7 C8 C71 174.8(2) . . . . ? C19 C7 C8 C71 -6.5(4) . . . . ? C7 C8 C9 C21 173.7(2) . . . . ? C71 C8 C9 C21 -1.6(4) . . . . ? C7 C8 C9 C4 5.0(4) . . . . ? C71 C8 C9 C4 -170.3(2) . . . . ? C3 C4 C9 C8 103.7(3) . . . . ? C61 C4 C9 C8 -136.3(2) . . . . ? C5 C4 C9 C8 -8.6(3) . . . . ? C3 C4 C9 C21 -66.3(2) . . . . ? C61 C4 C9 C21 53.7(3) . . . . ? C5 C4 C9 C21 -178.6(2) . . . . ? C7 C6 C11 C12 -177.7(3) . . . . ? C5 C6 C11 C12 0.5(4) . . . . ? C7 C6 C11 C20 0.5(3) . . . . ? C5 C6 C11 C20 178.7(2) . . . . ? C20 C11 C12 C13 0.3(3) . . . . ? C6 C11 C12 C13 178.3(3) . . . . ? C11 C12 C13 C14 0.1(4) . . . . ? C12 C13 C14 C15 0.1(4) . . . . ? C13 C14 C15 C20 -0.8(4) . . . . ? C13 C14 C15 C16 -176.9(3) . . . . ? C20 C15 C16 C17 0.2(4) . . . . ? C14 C15 C16 C17 176.3(3) . . . . ? C15 C16 C17 C18 0.3(4) . . . . ? C16 C17 C18 C19 -0.2(4) . . . . ? C17 C18 C19 C20 -0.4(4) . . . . ? C17 C18 C19 C7 -178.5(3) . . . . ? C6 C7 C19 C18 178.0(3) . . . . ? C8 C7 C19 C18 -0.9(5) . . . . ? C6 C7 C19 C20 -0.3(3) . . . . ? C8 C7 C19 C20 -179.2(2) . . . . ? C14 C15 C20 C11 1.3(4) . . . . ? C16 C15 C20 C11 178.0(2) . . . . ? C14 C15 C20 C19 -177.5(2) . . . . ? C16 C15 C20 C19 -0.8(4) . . . . ? C12 C11 C20 C15 -1.1(4) . . . . ? C6 C11 C20 C15 -179.7(2) . . . . ? C12 C11 C20 C19 177.9(2) . . . . ? C6 C11 C20 C19 -0.7(3) . . . . ? C18 C19 C20 C15 0.9(4) . . . . ? C7 C19 C20 C15 179.6(2) . . . . ? C18 C19 C20 C11 -178.0(2) . . . . ? C7 C19 C20 C11 0.6(3) . . . . ? C8 C9 C21 C22 52.9(4) . . . . ? C4 C9 C21 C22 -137.2(2) . . . . ? C8 C9 C21 C30 -128.1(3) . . . . ? C4 C9 C21 C30 41.8(3) . . . . ? C30 C21 C22 C23 0.9(4) . . . . ? C9 C21 C22 C23 179.8(2) . . . . ? C21 C22 C23 C24 1.4(4) . . . . ? C22 C23 C24 C25 -1.9(4) . . . . ? C23 C24 C25 C26 179.4(2) . . . . ? C23 C24 C25 C30 0.1(4) . . . . ? C24 C25 C26 C27 -180.0(2) . . . . ? C30 C25 C26 C27 -0.7(4) . . . . ? C25 C26 C27 C28 -1.2(4) . . . . ? C26 C27 C28 C29 1.0(4) . . . . ? C27 C28 C29 C30 0.9(4) . . . . ? C27 C28 C29 C3 -173.4(2) . . . . ? C2 C3 C29 C28 -29.3(4) . . . . ? C4 C3 C29 C28 151.1(2) . . . . ? C2 C3 C29 C30 156.2(2) . . . . ? C4 C3 C29 C30 -23.3(3) . . . . ? C24 C25 C30 C21 2.2(4) . . . . ? C26 C25 C30 C21 -177.2(2) . . . . ? C24 C25 C30 C29 -178.1(2) . . . . ? C26 C25 C30 C29 2.6(4) . . . . ? C22 C21 C30 C25 -2.7(4) . . . . ? C9 C21 C30 C25 178.3(2) . . . . ? C22 C21 C30 C29 177.6(2) . . . . ? C9 C21 C30 C29 -1.4(3) . . . . ? C28 C29 C30 C25 -2.7(3) . . . . ? C3 C29 C30 C25 172.0(2) . . . . ? C28 C29 C30 C21 177.0(2) . . . . ? C3 C29 C30 C21 -8.3(3) . . . . ? C3 C2 C41 C42 -45.9(4) . . . . ? C1 C2 C41 C42 132.4(2) . . . . ? C3 C2 C41 C46 138.9(3) . . . . ? C1 C2 C41 C46 -42.9(3) . . . . ? C46 C41 C42 C43 0.3(4) . . . . ? C2 C41 C42 C43 -175.1(2) . . . . ? C41 C42 C43 C44 -0.8(4) . . . . ? C42 C43 C44 C45 0.7(4) . . . . ? C43 C44 C45 C46 -0.1(4) . . . . ? C44 C45 C46 C41 -0.5(4) . . . . ? C42 C41 C46 C45 0.4(4) . . . . ? C2 C41 C46 C45 175.7(2) . . . . ? C6 C5 C51 C52 -31.4(3) . . . . ? C1 C5 C51 C52 -148.4(2) . . . . ? C4 C5 C51 C52 95.8(3) . . . . ? C6 C5 C51 C56 152.2(2) . . . . ? C1 C5 C51 C56 35.2(3) . . . . ? C4 C5 C51 C56 -80.6(3) . . . . ? C56 C51 C52 C53 1.5(4) . . . . ? C5 C51 C52 C53 -175.0(2) . . . . ? C51 C52 C53 C54 0.6(4) . . . . ? C52 C53 C54 C55 -2.0(4) . . . . ? C53 C54 C55 C56 1.2(4) . . . . ? C54 C55 C56 C51 0.9(4) . . . . ? C52 C51 C56 C55 -2.3(4) . . . . ? C5 C51 C56 C55 174.2(2) . . . . ? C3 C4 C61 C62 160.2(2) . . . . ? C9 C4 C61 C62 48.6(3) . . . . ? C5 C4 C61 C62 -82.0(2) . . . . ? C3 C4 C61 C66 -24.4(3) . . . . ? C9 C4 C61 C66 -136.0(2) . . . . ? C5 C4 C61 C66 93.5(3) . . . . ? C66 C61 C62 C63 -1.7(3) . . . . ? C4 C61 C62 C63 174.0(2) . . . . ? C61 C62 C63 C64 1.3(4) . . . . ? C62 C63 C64 C65 -0.3(4) . . . . ? C63 C64 C65 C66 -0.3(4) . . . . ? C64 C65 C66 C61 0.0(4) . . . . ? C62 C61 C66 C65 1.0(3) . . . . ? C4 C61 C66 C65 -174.4(2) . . . . ? C9 C8 C71 C72 87.6(3) . . . . ? C7 C8 C71 C72 -87.8(3) . . . . ? C9 C8 C71 C76 -96.2(3) . . . . ? C7 C8 C71 C76 88.4(3) . . . . ? C76 C71 C72 C73 0.0(4) . . . . ? C8 C71 C72 C73 176.3(2) . . . . ? C71 C72 C73 C74 0.0(4) . . . . ? C72 C73 C74 C75 0.7(4) . . . . ? C73 C74 C75 C76 -1.4(4) . . . . ? C74 C75 C76 C71 1.4(4) . . . . ? C72 C71 C76 C75 -0.8(4) . . . . ? C8 C71 C76 C75 -177.0(2) . . . . ? O1A C1A C2A C3A 176.5(2) . . . . ? C5A C1A C2A C3A -4.6(3) . . . . ? O1A C1A C2A C41A -5.4(4) . . . . ? C5A C1A C2A C41A 173.5(2) . . . . ? C1A C2A C3A C21A -177.7(2) . . . . ? C41A C2A C3A C21A 4.4(4) . . . . ? C1A C2A C3A C4A 3.8(3) . . . . ? C41A C2A C3A C4A -174.1(2) . . . . ? C2A C3A C4A C51A -123.1(2) . . . . ? C21A C3A C4A C51A 58.2(3) . . . . ? C2A C3A C4A C9A 121.0(2) . . . . ? C21A C3A C4A C9A -57.7(3) . . . . ? C2A C3A C4A C5A -1.5(3) . . . . ? C21A C3A C4A C5A 179.8(2) . . . . ? O1A C1A C5A C6A 63.9(3) . . . . ? C2A C1A C5A C6A -115.1(2) . . . . ? O1A C1A C5A C61A -56.1(3) . . . . ? C2A C1A C5A C61A 125.0(2) . . . . ? O1A C1A C5A C4A -177.6(2) . . . . ? C2A C1A C5A C4A 3.4(3) . . . . ? C51A C4A C5A C6A -125.0(2) . . . . ? C3A C4A C5A C6A 112.9(2) . . . . ? C9A C4A C5A C6A 0.2(3) . . . . ? C51A C4A C5A C61A 1.1(3) . . . . ? C3A C4A C5A C61A -121.0(2) . . . . ? C9A C4A C5A C61A 126.3(2) . . . . ? C51A C4A C5A C1A 120.9(2) . . . . ? C3A C4A C5A C1A -1.2(2) . . . . ? C9A C4A C5A C1A -113.9(2) . . . . ? C61A C5A C6A C7A -128.2(3) . . . . ? C1A C5A C6A C7A 111.1(3) . . . . ? C4A C5A C6A C7A -0.1(3) . . . . ? C61A C5A C6A C19A 53.5(3) . . . . ? C1A C5A C6A C19A -67.2(3) . . . . ? C4A C5A C6A C19A -178.4(2) . . . . ? C19A C6A C7A C8A -179.9(2) . . . . ? C5A C6A C7A C8A 1.6(4) . . . . ? C19A C6A C7A C11A 1.6(3) . . . . ? C5A C6A C7A C11A -176.9(2) . . . . ? C6A C7A C8A C9A -3.2(4) . . . . ? C11A C7A C8A C9A 174.9(2) . . . . ? C6A C7A C8A C71A 176.5(2) . . . . ? C11A C7A C8A C71A -5.4(4) . . . . ? C7A C8A C9A C29A -174.0(2) . . . . ? C71A C8A C9A C29A 6.3(4) . . . . ? C7A C8A C9A C4A 3.3(4) . . . . ? C71A C8A C9A C4A -176.4(2) . . . . ? C51A C4A C9A C8A 125.3(3) . . . . ? C3A C4A C9A C8A -115.6(3) . . . . ? C5A C4A C9A C8A -1.8(4) . . . . ? C51A C4A C9A C29A -57.1(3) . . . . ? C3A C4A C9A C29A 62.0(2) . . . . ? C5A C4A C9A C29A 175.8(2) . . . . ? C6A C7A C11A C12A 176.6(3) . . . . ? C8A C7A C11A C12A -1.7(5) . . . . ? C6A C7A C11A C20A -1.3(3) . . . . ? C8A C7A C11A C20A -179.7(2) . . . . ? C20A C11A C12A C13A 1.2(4) . . . . ? C7A C11A C12A C13A -176.5(3) . . . . ? C11A C12A C13A C14A -3.0(4) . . . . ? C12A C13A C14A C15A 2.4(4) . . . . ? C13A C14A C15A C20A 0.0(4) . . . . ? C13A C14A C15A C16A 179.7(3) . . . . ? C20A C15A C16A C17A 1.8(4) . . . . ? C14A C15A C16A C17A -177.8(3) . . . . ? C15A C16A C17A C18A 0.2(5) . . . . ? C16A C17A C18A C19A -1.7(4) . . . . ? C17A C18A C19A C20A 1.0(4) . . . . ? C17A C18A C19A C6A -179.2(3) . . . . ? C7A C6A C19A C18A 178.9(3) . . . . ? C5A C6A C19A C18A -2.6(5) . . . . ? C7A C6A C19A C20A -1.3(3) . . . . ? C5A C6A C19A C20A 177.2(2) . . . . ? C14A C15A C20A C11A -1.8(4) . . . . ? C16A C15A C20A C11A 178.5(2) . . . . ? C14A C15A C20A C19A 177.1(3) . . . . ? C16A C15A C20A C19A -2.6(4) . . . . ? C12A C11A C20A C15A 1.2(4) . . . . ? C7A C11A C20A C15A 179.6(2) . . . . ? C12A C11A C20A C19A -177.9(2) . . . . ? C7A C11A C20A C19A 0.5(3) . . . . ? C18A C19A C20A C15A 1.2(4) . . . . ? C6A C19A C20A C15A -178.6(2) . . . . ? C18A C19A C20A C11A -179.7(2) . . . . ? C6A C19A C20A C11A 0.4(3) . . . . ? C2A C3A C21A C22A 31.9(4) . . . . ? C4A C3A C21A C22A -149.7(2) . . . . ? C2A C3A C21A C30A -151.8(3) . . . . ? C4A C3A C21A C30A 26.6(3) . . . . ? C30A C21A C22A C23A 1.5(4) . . . . ? C3A C21A C22A C23A 177.7(2) . . . . ? C21A C22A C23A C24A -2.1(4) . . . . ? C22A C23A C24A C25A 0.4(4) . . . . ? C23A C24A C25A C26A -178.8(3) . . . . ? C23A C24A C25A C30A 1.9(4) . . . . ? C24A C25A C26A C27A 179.6(3) . . . . ? C30A C25A C26A C27A -1.1(4) . . . . ? C25A C26A C27A C28A 1.8(4) . . . . ? C26A C27A C28A C29A -0.2(4) . . . . ? C27A C28A C29A C30A -1.9(4) . . . . ? C27A C28A C29A C9A 178.4(2) . . . . ? C8A C9A C29A C28A -41.1(4) . . . . ? C4A C9A C29A C28A 141.4(2) . . . . ? C8A C9A C29A C30A 139.2(3) . . . . ? C4A C9A C29A C30A -38.4(3) . . . . ? C24A C25A C30A C29A 178.3(2) . . . . ? C26A C25A C30A C29A -1.0(4) . . . . ? C24A C25A C30A C21A -2.4(4) . . . . ? C26A C25A C30A C21A 178.3(2) . . . . ? C28A C29A C30A C25A 2.5(4) . . . . ? C9A C29A C30A C25A -177.8(2) . . . . ? C28A C29A C30A C21A -176.8(2) . . . . ? C9A C29A C30A C21A 2.9(3) . . . . ? C22A C21A C30A C25A 0.7(4) . . . . ? C3A C21A C30A C25A -175.7(2) . . . . ? C22A C21A C30A C29A -180.0(2) . . . . ? C3A C21A C30A C29A 3.6(3) . . . . ? C3A C2A C41A C42A 47.7(4) . . . . ? C1A C2A C41A C42A -130.0(3) . . . . ? C3A C2A C41A C46A -135.8(3) . . . . ? C1A C2A C41A C46A 46.5(4) . . . . ? C46A C41A C42A C43A 0.4(4) . . . . ? C2A C41A C42A C43A 177.0(2) . . . . ? C41A C42A C43A C44A 0.2(4) . . . . ? C42A C43A C44A C45A -1.0(4) . . . . ? C43A C44A C45A C46A 1.1(4) . . . . ? C44A C45A C46A C41A -0.5(4) . . . . ? C42A C41A C46A C45A -0.3(4) . . . . ? C2A C41A C46A C45A -176.9(2) . . . . ? C3A C4A C51A C56A -153.5(2) . . . . ? C9A C4A C51A C56A -40.9(3) . . . . ? C5A C4A C51A C56A 89.1(3) . . . . ? C3A C4A C51A C52A 29.7(3) . . . . ? C9A C4A C51A C52A 142.4(2) . . . . ? C5A C4A C51A C52A -87.6(3) . . . . ? C56A C51A C52A C53A -2.6(4) . . . . ? C4A C51A C52A C53A 174.2(2) . . . . ? C51A C52A C53A C54A 2.3(4) . . . . ? C52A C53A C54A C55A -0.6(4) . . . . ? C53A C54A C55A C56A -0.6(4) . . . . ? C54A C55A C56A C51A 0.2(4) . . . . ? C52A C51A C56A C55A 1.4(4) . . . . ? C4A C51A C56A C55A -175.4(2) . . . . ? C6A C5A C61A C62A 37.9(3) . . . . ? C1A C5A C61A C62A 155.9(2) . . . . ? C4A C5A C61A C62A -89.7(3) . . . . ? C6A C5A C61A C66A -143.6(2) . . . . ? C1A C5A C61A C66A -25.6(3) . . . . ? C4A C5A C61A C66A 88.8(3) . . . . ? C66A C61A C62A C63A -0.5(4) . . . . ? C5A C61A C62A C63A 178.0(2) . . . . ? C61A C62A C63A C64A -1.8(4) . . . . ? C62A C63A C64A C65A 2.7(5) . . . . ? C63A C64A C65A C66A -1.2(5) . . . . ? C64A C65A C66A C61A -1.2(5) . . . . ? C62A C61A C66A C65A 2.0(4) . . . . ? C5A C61A C66A C65A -176.5(3) . . . . ? C9A C8A C71A C72A -68.6(3) . . . . ? C7A C8A C71A C72A 111.7(3) . . . . ? C9A C8A C71A C76A 111.3(3) . . . . ? C7A C8A C71A C76A -68.3(3) . . . . ? C76A C71A C72A C73A -1.1(4) . . . . ? C8A C71A C72A C73A 178.8(2) . . . . ? C71A C72A C73A C74A -0.3(4) . . . . ? C72A C73A C74A C75A 1.5(4) . . . . ? C73A C74A C75A C76A -1.4(4) . . . . ? C74A C75A C76A C71A 0.0(4) . . . . ? C72A C71A C76A C75A 1.3(4) . . . . ? C8A C71A C76A C75A -178.6(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.570 _refine_diff_density_min -0.252 _refine_diff_density_rms 0.048 _database_code_depnum_ccdc_archive 'CCDC 969866'