Supplementary Material (ESI) for Journal of Materials Chemistry This journal is (c) The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 1145 loop_ _publ_author_name 'Dirk Volkmer' 'Ceno Agena' 'Marc Fricke' 'Jochen Mattay' _publ_contact_author_name 'Dr Dirk Volkmer' _publ_contact_author_address ; Faculty of Chemistry, AC1 University of Bielefeld PO Box 100 131 Bielefeld 33501 GERMANY ; _publ_contact_author_phone '49 521 106 6142' _publ_contact_author_fax '49 521 106 6003' _publ_contact_author_email dirk.volkmer@uni-bielefeld.de _publ_requested_journal 'Journal of Materials Chemistry' _publ_requested_coeditor_name 'Stephen Mann' _publ_section_title ; Interfacial Electrostatics Guiding the Crystallization of CaCO3 Underneath Monolayers of Calixarenes and Resorcarenes ; #========================================================================= data_blade _database_code_depnum_ccdc_archive 'CCDC 232971' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H136 O28' _chemical_formula_weight 1665.99 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 9.9409(7) _cell_length_b 17.2656(11) _cell_length_c 27.3161(18) _cell_angle_alpha 71.9090(10) _cell_angle_beta 83.8170(10) _cell_angle_gamma 84.9220(10) _cell_volume 4423.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 188(2) _cell_measurement_reflns_used 4746 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 24.42 _exptl_crystal_description blade-like _exptl_crystal_colour colorless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.251 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 0.092 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 188(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 'Bruker AXS SMART' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 39701 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_sigmaI/netI 0.0723 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 25.02 _reflns_number_total 15548 _reflns_number_gt 9189 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS SMART' _computing_cell_refinement 'Bruker AXS SAINT' _computing_data_reduction 'Bruker AXS SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Crystal Impact: DIAMOND; Bruker AXS: SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15548 _refine_ls_number_parameters 1093 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1704 _refine_ls_R_factor_gt 0.1129 _refine_ls_wR_factor_ref 0.3800 _refine_ls_wR_factor_gt 0.3395 _refine_ls_goodness_of_fit_ref 1.326 _refine_ls_restrained_S_all 1.328 _refine_ls_shift/su_max 1.396 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5957(5) 0.6604(3) 0.87922(19) 0.0422(13) Uani 1 1 d . . . H1 H 0.6179 0.6332 0.9136 0.051 Uiso 1 1 calc R . . C2 C 0.6047(5) 0.7451(3) 0.85843(17) 0.0339(11) Uani 1 1 d . . . C3 C 0.5689(4) 0.7857(3) 0.80863(16) 0.0294(10) Uani 1 1 d . . . C4 C 0.5299(4) 0.7388(3) 0.78046(17) 0.0308(10) Uani 1 1 d . . . H4 H 0.5058 0.7658 0.7463 0.037 Uiso 1 1 calc R . . C5 C 0.5237(4) 0.6534(3) 0.79923(17) 0.0297(10) Uani 1 1 d . . . C6 C 0.5541(5) 0.6165(3) 0.84937(18) 0.0343(11) Uani 1 1 d . . . O1 O 0.6481(4) 0.79137(19) 0.88567(12) 0.0421(9) Uani 1 1 d . . . C7 C 0.7077(5) 0.7491(3) 0.93221(19) 0.0419(12) Uani 1 1 d . . . H7A H 0.7842 0.7126 0.9246 0.050 Uiso 1 1 calc R . . H7B H 0.6398 0.7145 0.9564 0.050 Uiso 1 1 calc R . . C8 C 0.7575(6) 0.8033(3) 0.9575(2) 0.0444(13) Uani 1 1 d . . . O2 O 0.7517(7) 0.8774(2) 0.9371(2) 0.110(2) Uani 1 1 d . . . O3 O 0.8020(4) 0.7682(2) 1.00126(14) 0.0534(10) Uani 1 1 d . . . H3 H 0.8310 0.7204 1.0028 0.080 Uiso 1 1 calc R . . O4 O 0.5423(4) 0.53291(19) 0.86762(12) 0.0436(9) Uani 1 1 d . . . C9 C 0.5349(5) 0.4929(3) 0.92194(19) 0.0427(13) Uani 1 1 d . . . H9A H 0.4789 0.4452 0.9299 0.051 Uiso 1 1 calc R . . H9B H 0.4885 0.5309 0.9399 0.051 Uiso 1 1 calc R . . C10 C 0.6712(5) 0.4644(3) 0.94305(18) 0.0374(12) Uani 1 1 d . . . O5 O 0.7753(4) 0.4867(3) 0.91012(15) 0.0672(13) Uani 1 1 d . . . H5 H 0.8437 0.4563 0.9207 0.101 Uiso 1 1 calc R . . O6 O 0.6782(4) 0.4228(3) 0.98733(13) 0.0595(11) Uani 1 1 d . . . C11 C 0.4879(5) 0.6015(3) 0.76663(17) 0.0319(10) Uani 1 1 d . . . H11 H 0.5601 0.5565 0.7697 0.038 Uiso 1 1 calc R . . C12 C 0.4841(5) 0.6484(3) 0.70917(17) 0.0382(12) Uani 1 1 d . . . H12A H 0.4185 0.6961 0.7056 0.046 Uiso 1 1 calc R . . H12B H 0.5745 0.6695 0.6957 0.046 Uiso 1 1 calc R . . C13 C 0.4457(7) 0.5992(3) 0.67602(19) 0.0546(15) Uani 1 1 d . . . H13A H 0.5040 0.5481 0.6826 0.066 Uiso 1 1 calc R . . H13B H 0.3507 0.5841 0.6863 0.066 Uiso 1 1 calc R . . C14 C 0.4596(6) 0.6446(4) 0.61867(19) 0.0547(15) Uani 1 1 d . . . H14A H 0.4127 0.6993 0.6129 0.066 Uiso 1 1 calc R . . H14B H 0.5568 0.6524 0.6075 0.066 Uiso 1 1 calc R . . C15 C 0.4033(8) 0.6026(4) 0.5855(2) 0.0680(18) Uani 1 1 d . . . H15A H 0.3045 0.5993 0.5949 0.082 Uiso 1 1 calc R . . H15B H 0.4437 0.5460 0.5942 0.082 Uiso 1 1 calc R . . C16 C 0.4256(8) 0.6411(5) 0.5279(2) 0.0738(19) Uani 1 1 d . . . H16A H 0.3919 0.6991 0.5195 0.089 Uiso 1 1 calc R . . H16B H 0.5243 0.6402 0.5180 0.089 Uiso 1 1 calc R . . C17 C 0.3604(8) 0.6028(5) 0.4959(2) 0.085(2) Uani 1 1 d . . . H17A H 0.2610 0.6098 0.5029 0.102 Uiso 1 1 calc R . . H17B H 0.3850 0.5434 0.5077 0.102 Uiso 1 1 calc R . . C18 C 0.3935(9) 0.6331(6) 0.4387(3) 0.096(3) Uani 1 1 d . . . H18A H 0.3761 0.6931 0.4272 0.116 Uiso 1 1 calc R . . H18B H 0.4917 0.6217 0.4313 0.116 Uiso 1 1 calc R . . C19 C 0.3188(10) 0.5986(7) 0.4069(3) 0.110(3) Uani 1 1 d . B . H19A H 0.2206 0.6108 0.4137 0.132 Uiso 1 1 calc R . . H19B H 0.3350 0.5385 0.4186 0.132 Uiso 1 1 calc R . . C20 C 0.3554(11) 0.6295(8) 0.3480(3) 0.149(5) Uani 1 1 d D . . H20A H 0.4553 0.6255 0.3412 0.179 Uiso 1 1 calc R A 1 H20B H 0.3247 0.6878 0.3350 0.179 Uiso 1 1 calc R A 1 C21A C 0.2906(11) 0.5806(7) 0.3166(4) 0.079(4) Uiso 0.660(14) 1 d PD B 1 H21A H 0.3305 0.5968 0.2803 0.095 Uiso 0.660(14) 1 calc PR B 1 H21B H 0.3114 0.5213 0.3319 0.095 Uiso 0.660(14) 1 calc PR B 1 C22A C 0.1483(13) 0.5968(10) 0.3177(6) 0.130(6) Uiso 0.660(14) 1 d PD B 1 H22A H 0.1097 0.5661 0.2984 0.195 Uiso 0.660(14) 1 calc PR B 1 H22B H 0.1279 0.6554 0.3019 0.195 Uiso 0.660(14) 1 calc PR B 1 H22C H 0.1089 0.5803 0.3536 0.195 Uiso 0.660(14) 1 calc PR B 1 C21B C 0.241(2) 0.6549(19) 0.3106(8) 0.110(10) Uiso 0.340(14) 1 d PD B 2 H21C H 0.1837 0.6085 0.3162 0.132 Uiso 0.340(14) 1 calc PR B 2 H21D H 0.1836 0.7008 0.3175 0.132 Uiso 0.340(14) 1 calc PR B 2 C22B C 0.302(4) 0.680(3) 0.2569(8) 0.22(2) Uiso 0.340(14) 1 d PD B 2 H22D H 0.2303 0.6969 0.2333 0.323 Uiso 0.340(14) 1 calc PR B 2 H22E H 0.3571 0.6336 0.2501 0.323 Uiso 0.340(14) 1 calc PR B 2 H22F H 0.3600 0.7253 0.2517 0.323 Uiso 0.340(14) 1 calc PR B 2 C23 C 0.2166(6) 0.4447(3) 0.81514(18) 0.0443(13) Uani 1 1 d . . . H23 H 0.2101 0.3873 0.8248 0.053 Uiso 1 1 calc R . . C24 C 0.3405(5) 0.4775(3) 0.80018(18) 0.0352(11) Uani 1 1 d . . . C25 C 0.3533(5) 0.5618(3) 0.78758(16) 0.0317(11) Uani 1 1 d . . . C26 C 0.2364(4) 0.6097(3) 0.79252(16) 0.0283(10) Uani 1 1 d . . . H26 H 0.2439 0.6666 0.7858 0.034 Uiso 1 1 calc R . . C27 C 0.1090(5) 0.5789(3) 0.80680(16) 0.0318(11) Uani 1 1 d . . . C28 C 0.1009(5) 0.4953(3) 0.81612(17) 0.0348(11) Uani 1 1 d . . . O7 O 0.4586(4) 0.4300(2) 0.79538(16) 0.0561(10) Uani 1 1 d . . . C29 C 0.4544(8) 0.3473(4) 0.8006(3) 0.077(2) Uani 1 1 d . . . H29A H 0.5317 0.3311 0.7791 0.092 Uiso 1 1 calc R . . H29B H 0.3698 0.3385 0.7874 0.092 Uiso 1 1 calc R . . C30 C 0.4604(6) 0.2926(4) 0.8568(3) 0.0559(15) Uani 1 1 d . . . O8 O 0.4709(6) 0.3242(3) 0.8907(2) 0.0978(17) Uani 1 1 d . . . O9 O 0.4572(7) 0.2186(3) 0.8638(3) 0.1052(19) Uani 1 1 d . . . H9 H 0.4595 0.1935 0.8955 0.158 Uiso 1 1 calc R . . O10 O -0.0269(4) 0.4650(2) 0.82680(15) 0.0555(10) Uani 1 1 d . . . C31 C -0.0335(8) 0.3817(4) 0.8269(3) 0.081(2) Uani 1 1 d . . . H31A H 0.0292 0.3730 0.7982 0.098 Uiso 1 1 calc R . . H31B H -0.0004 0.3450 0.8596 0.098 Uiso 1 1 calc R . . C32 C -0.1552(13) 0.3599(6) 0.8224(4) 0.114(3) Uani 1 1 d . . . O11 O -0.2632(7) 0.4122(6) 0.8270(3) 0.134(3) Uani 1 1 d . . . H11A H -0.2436 0.4421 0.8440 0.201 Uiso 1 1 calc R . . O12 O -0.1825(10) 0.2975(4) 0.8137(3) 0.164(3) Uani 1 1 d . . . C33 C -0.0155(5) 0.6371(3) 0.81076(17) 0.0328(11) Uani 1 1 d . . . H33 H -0.0935 0.6031 0.8283 0.039 Uiso 1 1 calc R . . C34 C -0.0533(5) 0.6888(3) 0.75609(18) 0.0391(12) Uani 1 1 d . . . H34A H -0.1339 0.7254 0.7595 0.047 Uiso 1 1 calc R . . H34B H 0.0224 0.7234 0.7384 0.047 Uiso 1 1 calc R . . C35 C -0.0833(6) 0.6369(3) 0.7232(2) 0.0477(13) Uani 1 1 d . . . H35A H -0.1698 0.6107 0.7373 0.057 Uiso 1 1 calc R . . H35B H -0.0109 0.5930 0.7257 0.057 Uiso 1 1 calc R . . C36 C -0.0933(6) 0.6852(3) 0.66656(19) 0.0503(14) Uani 1 1 d . . . H36A H -0.1719 0.7253 0.6638 0.060 Uiso 1 1 calc R . . H36B H -0.0107 0.7160 0.6536 0.060 Uiso 1 1 calc R . . C37 C -0.1088(7) 0.6331(4) 0.6331(2) 0.0617(16) Uani 1 1 d . . . H37A H -0.1917 0.6027 0.6463 0.074 Uiso 1 1 calc R . . H37B H -0.0308 0.5925 0.6366 0.074 Uiso 1 1 calc R . . C38 C -0.1179(7) 0.6787(4) 0.5751(2) 0.0609(16) Uani 1 1 d . . . H38A H -0.1988 0.7172 0.5713 0.073 Uiso 1 1 calc R . . H38B H -0.0373 0.7113 0.5621 0.073 Uiso 1 1 calc R . . C39 C -0.1265(8) 0.6246(4) 0.5424(2) 0.0714(19) Uani 1 1 d . . . H39A H -0.2056 0.5910 0.5564 0.086 Uiso 1 1 calc R . . H39B H -0.0445 0.5869 0.5461 0.086 Uiso 1 1 calc R . . C40 C -0.1388(7) 0.6657(4) 0.4856(2) 0.0666(18) Uani 1 1 d . . . H40A H -0.2189 0.7048 0.4816 0.080 Uiso 1 1 calc R . . H40B H -0.0579 0.6974 0.4710 0.080 Uiso 1 1 calc R . . C41 C -0.1521(9) 0.6098(5) 0.4550(3) 0.084(2) Uani 1 1 d . . . H41A H -0.2296 0.5757 0.4711 0.100 Uiso 1 1 calc R . . H41B H -0.0694 0.5728 0.4575 0.100 Uiso 1 1 calc R . . C42 C -0.1729(8) 0.6505(4) 0.3977(2) 0.0727(19) Uani 1 1 d . . . H42A H -0.2529 0.6897 0.3948 0.087 Uiso 1 1 calc R . . H42B H -0.0929 0.6818 0.3808 0.087 Uiso 1 1 calc R . . C43 C -0.1936(13) 0.5905(6) 0.3691(3) 0.125(4) Uani 1 1 d . . . H43A H -0.1144 0.5507 0.3726 0.149 Uiso 1 1 calc R . . H43B H -0.2746 0.5598 0.3857 0.149 Uiso 1 1 calc R . . C44 C -0.2119(12) 0.6302(6) 0.3121(3) 0.133(4) Uani 1 1 d . . . H44A H -0.2238 0.5880 0.2960 0.200 Uiso 1 1 calc R . . H44B H -0.1316 0.6599 0.2951 0.200 Uiso 1 1 calc R . . H44C H -0.2921 0.6682 0.3082 0.200 Uiso 1 1 calc R . . C45 C 0.0754(5) 0.6923(3) 0.92699(18) 0.0357(11) Uani 1 1 d . . . H45 H 0.0928 0.6634 0.9617 0.043 Uiso 1 1 calc R . . C46 C 0.0409(5) 0.6503(3) 0.89517(17) 0.0319(11) Uani 1 1 d . . . C47 C 0.0135(4) 0.6886(3) 0.84484(17) 0.0314(10) Uani 1 1 d . . . C48 C 0.0242(5) 0.7727(3) 0.82704(18) 0.0350(11) Uani 1 1 d . . . H48 H 0.0071 0.8005 0.7922 0.042 Uiso 1 1 calc R . . C49 C 0.0585(5) 0.8186(3) 0.85722(17) 0.0321(10) Uani 1 1 d . . . C50 C 0.0850(5) 0.7756(3) 0.90905(18) 0.0348(11) Uani 1 1 d . . . O13 O 0.0259(3) 0.56660(18) 0.91528(12) 0.0349(8) Uani 1 1 d . . . C51 C 0.1441(5) 0.5209(3) 0.93329(19) 0.0387(12) Uani 1 1 d . . . H51A H 0.1700 0.5353 0.9632 0.046 Uiso 1 1 calc R . . H51B H 0.2194 0.5332 0.9057 0.046 Uiso 1 1 calc R . . C52 C 0.1181(5) 0.4317(3) 0.94906(17) 0.0376(12) Uani 1 1 d . . . O14 O 0.2264(3) 0.3866(2) 0.96466(15) 0.0478(9) Uani 1 1 d . . . H14 H 0.2079 0.3373 0.9755 0.072 Uiso 1 1 calc R . . O15 O 0.0091(4) 0.4065(2) 0.94741(14) 0.0471(9) Uani 1 1 d . . . O16 O 0.1160(4) 0.8208(2) 0.93934(12) 0.0422(9) Uani 1 1 d . . . C53 C 0.1425(7) 0.7733(4) 0.9926(2) 0.0608(16) Uani 1 1 d . . . H53A H 0.2262 0.7377 0.9922 0.073 Uiso 1 1 calc R . . H53B H 0.0664 0.7380 1.0087 0.073 Uiso 1 1 calc R . . C54 C 0.1582(7) 0.8286(5) 1.0231(2) 0.0687(19) Uani 1 1 d . . . O17 O 0.1524(10) 0.9014(3) 1.0062(2) 0.157(4) Uani 1 1 d . . . O18 O 0.1874(6) 0.7874(4) 1.07021(18) 0.0931(16) Uani 1 1 d . . . H18 H 0.1812 0.8190 1.0884 0.140 Uiso 1 1 calc R . . C55 C 0.0677(5) 0.9114(3) 0.83702(17) 0.0334(11) Uani 1 1 d . . . H55 H 0.0108 0.9349 0.8621 0.040 Uiso 1 1 calc R . . C56 C 0.0081(5) 0.9480(3) 0.78380(19) 0.0410(12) Uani 1 1 d . . . H56A H 0.0623 0.9245 0.7587 0.049 Uiso 1 1 calc R . . H56B H -0.0853 0.9301 0.7872 0.049 Uiso 1 1 calc R . . C57 C 0.0032(6) 1.0398(3) 0.7615(2) 0.0487(14) Uani 1 1 d . . . H57A H 0.0965 1.0585 0.7558 0.058 Uiso 1 1 calc R . . H57B H -0.0485 1.0643 0.7866 0.058 Uiso 1 1 calc R . . C58 C -0.0632(7) 1.0697(4) 0.7101(2) 0.0677(18) Uani 1 1 d . . . H58A H -0.0213 1.0375 0.6875 0.081 Uiso 1 1 calc R . . H58B H -0.1604 1.0581 0.7172 0.081 Uiso 1 1 calc R . . C59 C -0.0530(8) 1.1557(5) 0.6820(3) 0.089(2) Uani 1 1 d . . . H59A H 0.0437 1.1680 0.6734 0.106 Uiso 1 1 calc R . . H59B H -0.0945 1.1889 0.7040 0.106 Uiso 1 1 calc R . . C60 C -0.1275(9) 1.1786(6) 0.6305(4) 0.111(3) Uani 1 1 d . . . H60A H -0.2242 1.1670 0.6400 0.133 Uiso 1 1 calc R . . H60B H -0.1236 1.2382 0.6135 0.133 Uiso 1 1 calc R . . C61 C -0.0743(7) 1.1367(6) 0.5924(4) 0.100(3) Uani 1 1 d . . . H61A H -0.0825 1.0773 0.6084 0.121 Uiso 1 1 calc R . . H61B H 0.0233 1.1463 0.5835 0.121 Uiso 1 1 calc R . . C62 C -0.1515(9) 1.1663(7) 0.5397(4) 0.132(5) Uani 1 1 d . . . H62A H -0.2490 1.1569 0.5492 0.159 Uiso 1 1 calc R . . H62B H -0.1436 1.2259 0.5244 0.159 Uiso 1 1 calc R . . C63 C -0.1034(8) 1.1268(6) 0.4989(4) 0.119(4) Uani 1 1 d . . . H63A H -0.1112 1.0671 0.5137 0.143 Uiso 1 1 calc R . . H63B H -0.0064 1.1367 0.4885 0.143 Uiso 1 1 calc R . . C64 C -0.1830(8) 1.1581(6) 0.4505(4) 0.107(3) Uani 1 1 d . . . H64A H -0.2796 1.1471 0.4609 0.129 Uiso 1 1 calc R . . H64B H -0.1768 1.2179 0.4363 0.129 Uiso 1 1 calc R . . C65 C -0.1361(11) 1.1218(6) 0.4105(5) 0.128(4) Uani 1 1 d . . . H65A H -0.1344 1.0619 0.4265 0.154 Uiso 1 1 calc R . . H65B H -0.0409 1.1362 0.3995 0.154 Uiso 1 1 calc R . . C66 C -0.2131(11) 1.1426(8) 0.3598(5) 0.148(5) Uani 1 1 d . . . H66A H -0.1695 1.1110 0.3376 0.222 Uiso 1 1 calc R . . H66B H -0.2098 1.2010 0.3413 0.222 Uiso 1 1 calc R . . H66C H -0.3078 1.1285 0.3692 0.222 Uiso 1 1 calc R . . C67 C 0.3648(5) 1.0372(3) 0.83851(18) 0.0396(12) Uani 1 1 d . . . H67 H 0.3805 1.0842 0.8477 0.047 Uiso 1 1 calc R . . C68 C 0.2352(5) 1.0105(3) 0.84457(16) 0.0339(11) Uani 1 1 d . . . C69 C 0.2109(5) 0.9384(3) 0.83384(16) 0.0297(10) Uani 1 1 d . . . C70 C 0.3225(5) 0.8964(3) 0.81728(17) 0.0316(11) Uani 1 1 d . . . H70 H 0.3084 0.8471 0.8106 0.038 Uiso 1 1 calc R . . C71 C 0.4541(5) 0.9220(3) 0.80980(16) 0.0303(10) Uani 1 1 d . . . C72 C 0.4705(5) 0.9956(3) 0.81922(18) 0.0367(12) Uani 1 1 d . C . O19 O 0.1217(4) 1.05159(19) 0.86100(13) 0.0425(9) Uani 1 1 d . . . C73 C 0.1289(6) 1.1336(3) 0.8575(2) 0.0472(13) Uani 1 1 d . . . H73A H 0.0409 1.1636 0.8486 0.057 Uiso 1 1 calc R . . H73B H 0.1995 1.1588 0.8302 0.057 Uiso 1 1 calc R . . C74 C 0.1649(6) 1.1383(4) 0.9120(3) 0.0638(18) Uani 1 1 d . . . O20 O 0.2000(8) 1.0805(4) 0.9452(2) 0.125(3) Uani 1 1 d . . . O21 O 0.1568(5) 1.2126(3) 0.91271(19) 0.0791(14) Uani 1 1 d . . . H21 H 0.1593 1.2134 0.9432 0.119 Uiso 1 1 calc R . . O22 O 0.5988(4) 1.0265(2) 0.80667(15) 0.0559(10) Uani 1 1 d . . . C76 C 0.7097(8) 1.1064(4) 0.8472(3) 0.077(2) Uani 1 1 d . . . C75A C 0.6545(11) 1.0309(6) 0.8499(3) 0.054(3) Uani 0.570(8) 1 d P C 1 H75A H 0.7276 0.9872 0.8583 0.065 Uiso 0.570(8) 1 calc PR C 1 H75B H 0.5837 1.0184 0.8791 0.065 Uiso 0.570(8) 1 calc PR C 1 O23A O 0.7087(8) 1.1671(4) 0.8014(3) 0.058(2) Uani 0.570(8) 1 d P C 1 H23A H 0.7369 1.2094 0.8048 0.086 Uiso 0.570(8) 1 calc PR C 1 O24A O 0.7881(8) 1.1098(6) 0.8790(3) 0.066(3) Uani 0.570(8) 1 d P C 1 C75B C 0.6368(14) 1.0991(7) 0.8052(5) 0.052(4) Uani 0.430(8) 1 d P C 2 H75C H 0.5543 1.1362 0.8029 0.062 Uiso 0.430(8) 1 calc PR C 2 H75D H 0.6946 1.1202 0.7726 0.062 Uiso 0.430(8) 1 calc PR C 2 O23B O 0.7575(12) 1.1647(7) 0.8498(5) 0.070(3) Uani 0.430(8) 1 d P C 2 O24B O 0.6547(16) 1.0520(7) 0.8947(4) 0.095(5) Uani 0.430(8) 1 d P C 2 H24B H 0.6168 1.0791 0.9136 0.142 Uiso 0.430(8) 1 calc PR C 2 C77 C 0.5733(5) 0.8784(3) 0.78754(16) 0.0314(11) Uani 1 1 d . . . H77 H 0.6567 0.8929 0.7994 0.038 Uiso 1 1 calc R . . C78 C 0.5844(5) 0.9136(3) 0.72856(17) 0.0360(11) Uani 1 1 d . . . H78A H 0.5067 0.8968 0.7152 0.043 Uiso 1 1 calc R . . H78B H 0.5778 0.9739 0.7191 0.043 Uiso 1 1 calc R . . C79 C 0.7148(5) 0.8868(3) 0.70252(19) 0.0447(13) Uani 1 1 d . . . H79A H 0.7181 0.8268 0.7100 0.054 Uiso 1 1 calc R . . H79B H 0.7925 0.8999 0.7178 0.054 Uiso 1 1 calc R . . C80 C 0.7311(6) 0.9263(4) 0.6441(2) 0.0576(15) Uani 1 1 d . . . H80A H 0.7124 0.9859 0.6365 0.069 Uiso 1 1 calc R . . H80B H 0.8265 0.9169 0.6316 0.069 Uiso 1 1 calc R . . C81 C 0.6397(6) 0.8952(4) 0.6141(2) 0.0563(15) Uani 1 1 d . . . H81A H 0.6412 0.8349 0.6277 0.068 Uiso 1 1 calc R . . H81B H 0.5455 0.9165 0.6197 0.068 Uiso 1 1 calc R . . C82 C 0.6805(6) 0.9194(4) 0.5576(2) 0.0596(16) Uani 1 1 d . . . H82A H 0.7764 0.9005 0.5525 0.071 Uiso 1 1 calc R . . H82B H 0.6752 0.9797 0.5441 0.071 Uiso 1 1 calc R . . C83 C 0.5951(7) 0.8861(4) 0.5251(2) 0.0673(18) Uani 1 1 d . . . H83A H 0.5925 0.8262 0.5405 0.081 Uiso 1 1 calc R . . H83B H 0.5010 0.9098 0.5269 0.081 Uiso 1 1 calc R . . C84 C 0.6496(7) 0.9053(4) 0.4687(2) 0.0685(18) Uani 1 1 d . . . H84A H 0.6508 0.9653 0.4533 0.082 Uiso 1 1 calc R . . H84B H 0.7443 0.8826 0.4670 0.082 Uiso 1 1 calc R . . C85 C 0.5703(7) 0.8727(4) 0.4367(2) 0.0664(18) Uani 1 1 d . . . H85A H 0.4782 0.8999 0.4352 0.080 Uiso 1 1 calc R . . H85B H 0.5607 0.8136 0.4540 0.080 Uiso 1 1 calc R . . C86 C 0.6320(7) 0.8841(4) 0.3821(2) 0.0657(17) Uani 1 1 d . . . H86A H 0.6417 0.9432 0.3649 0.079 Uiso 1 1 calc R . . H86B H 0.7242 0.8571 0.3837 0.079 Uiso 1 1 calc R . . C87 C 0.5556(7) 0.8522(5) 0.3492(2) 0.0727(19) Uani 1 1 d . . . H87A H 0.5416 0.7938 0.3672 0.087 Uiso 1 1 calc R . . H87B H 0.4651 0.8814 0.3460 0.087 Uiso 1 1 calc R . . C88 C 0.6209(8) 0.8600(5) 0.2965(3) 0.089(2) Uani 1 1 d . . . H88A H 0.5639 0.8368 0.2780 0.133 Uiso 1 1 calc R . . H88B H 0.7100 0.8305 0.2990 0.133 Uiso 1 1 calc R . . H88C H 0.6317 0.9178 0.2776 0.133 Uiso 1 1 calc R . . O25A O 0.4995(8) 0.8828(6) 1.0482(4) 0.093(3) Uiso 0.657(8) 1 d P D 1 O26A O 0.4722(8) 0.7767(5) 1.0172(3) 0.087(3) Uiso 0.657(8) 1 d P D 1 H26A H 0.5093 0.7476 1.0436 0.130 Uiso 0.657(8) 1 calc PR D 1 C89A C 0.4749(12) 0.8518(8) 1.0142(5) 0.083(3) Uiso 0.657(8) 1 d P D 1 C90A C 0.4361(14) 0.9104(9) 0.9624(5) 0.103(4) Uiso 0.657(8) 1 d P D 1 H90A H 0.3377 0.9121 0.9610 0.155 Uiso 0.657(8) 1 calc PR D 1 H90B H 0.4819 0.8915 0.9343 0.155 Uiso 0.657(8) 1 calc PR D 1 H90C H 0.4636 0.9651 0.9588 0.155 Uiso 0.657(8) 1 calc PR D 1 O27B O 0.4241(12) 0.8577(7) 0.9395(4) 0.058(4) Uiso 0.343(8) 1 d P D 2 O28B O 0.4937(13) 0.9179(9) 1.0150(6) 0.066(4) Uiso 0.343(8) 1 d P D 2 O29 O 0.2938(3) 0.01257(15) 0.02223(9) 0.0201(6) Uani 1 1 d . . . O30 O 0.0628(11) 0.0187(6) 0.0511(3) 0.005(3) Uiso 0.50 1 d P . . O31 O 0.0325(12) 0.0385(7) 0.0429(4) 0.000(3) Uiso 0.25 1 d P . . O32 O 0.0862(16) 0.0256(10) 0.0498(6) 0.000(5) Uiso 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.055(3) 0.032(3) 0.039(3) -0.003(2) -0.024(2) 0.001(2) C2 0.043(3) 0.025(2) 0.035(3) -0.009(2) -0.008(2) -0.003(2) C3 0.034(3) 0.027(2) 0.025(2) -0.0030(19) -0.0094(19) -0.0011(19) C4 0.034(3) 0.027(2) 0.027(2) 0.0013(19) -0.0078(19) -0.0032(19) C5 0.027(2) 0.028(2) 0.032(2) -0.006(2) -0.0082(19) -0.0008(19) C6 0.042(3) 0.020(2) 0.039(3) -0.003(2) -0.014(2) -0.005(2) O1 0.066(2) 0.0265(17) 0.0366(18) -0.0069(15) -0.0254(17) -0.0015(16) C7 0.056(3) 0.033(3) 0.038(3) -0.007(2) -0.022(2) 0.001(2) C8 0.058(3) 0.033(3) 0.044(3) -0.011(2) -0.018(3) 0.005(2) O2 0.197(6) 0.027(2) 0.121(4) -0.017(3) -0.102(4) 0.009(3) O3 0.071(3) 0.043(2) 0.052(2) -0.0170(18) -0.031(2) 0.007(2) O4 0.066(2) 0.0237(17) 0.0383(19) 0.0021(15) -0.0267(17) -0.0046(16) C9 0.044(3) 0.033(3) 0.043(3) 0.006(2) -0.013(2) -0.009(2) C10 0.054(3) 0.025(2) 0.035(3) -0.007(2) -0.016(2) -0.006(2) O5 0.037(2) 0.082(3) 0.054(2) 0.025(2) -0.0110(19) -0.015(2) O6 0.053(2) 0.077(3) 0.034(2) 0.0051(19) -0.0122(17) 0.005(2) C11 0.030(3) 0.028(2) 0.038(3) -0.009(2) -0.009(2) -0.0016(19) C12 0.043(3) 0.041(3) 0.028(2) -0.005(2) 0.000(2) -0.008(2) C13 0.083(4) 0.047(3) 0.037(3) -0.013(3) -0.008(3) -0.012(3) C14 0.065(4) 0.064(4) 0.034(3) -0.013(3) -0.005(3) -0.011(3) C15 0.100(5) 0.062(4) 0.042(3) -0.011(3) -0.015(3) -0.012(4) C16 0.085(5) 0.091(5) 0.042(3) -0.012(3) -0.007(3) -0.015(4) C17 0.112(6) 0.092(6) 0.049(4) -0.004(4) -0.022(4) -0.034(5) C18 0.111(7) 0.126(7) 0.051(4) -0.016(4) -0.012(4) -0.035(5) C19 0.112(7) 0.163(9) 0.067(5) -0.045(6) -0.003(5) -0.040(6) C20 0.126(8) 0.250(15) 0.062(5) -0.025(7) -0.013(5) -0.045(9) C23 0.069(4) 0.029(3) 0.035(3) -0.006(2) -0.008(3) -0.009(3) C24 0.038(3) 0.029(3) 0.037(3) -0.007(2) -0.009(2) 0.000(2) C25 0.046(3) 0.026(2) 0.024(2) -0.0051(19) -0.013(2) -0.002(2) C26 0.037(3) 0.022(2) 0.026(2) -0.0040(18) -0.0096(19) -0.003(2) C27 0.038(3) 0.029(2) 0.026(2) -0.0034(19) -0.010(2) -0.005(2) C28 0.044(3) 0.035(3) 0.028(2) -0.008(2) -0.005(2) -0.017(2) O7 0.060(3) 0.0250(19) 0.078(3) -0.0103(18) -0.005(2) 0.0025(17) C29 0.092(5) 0.047(4) 0.091(5) -0.026(4) -0.001(4) 0.005(4) C30 0.061(4) 0.037(3) 0.069(4) -0.020(3) 0.007(3) 0.001(3) O8 0.143(5) 0.071(3) 0.081(4) -0.023(3) -0.012(3) -0.014(3) O9 0.112(4) 0.048(3) 0.148(5) -0.024(3) 0.012(4) -0.013(3) O10 0.051(2) 0.045(2) 0.070(3) -0.0091(19) -0.0080(19) -0.0246(18) C31 0.101(6) 0.064(4) 0.084(5) -0.015(4) -0.019(4) -0.041(4) C32 0.158(10) 0.074(6) 0.116(7) -0.028(5) 0.009(7) -0.062(7) O11 0.084(4) 0.178(8) 0.177(7) -0.106(6) 0.005(4) -0.028(5) O12 0.246(10) 0.101(5) 0.157(7) -0.020(5) -0.074(6) -0.076(6) C33 0.030(3) 0.034(3) 0.033(2) -0.006(2) -0.007(2) -0.009(2) C34 0.040(3) 0.040(3) 0.038(3) -0.011(2) -0.009(2) 0.001(2) C35 0.051(3) 0.048(3) 0.046(3) -0.013(3) -0.017(3) -0.003(3) C36 0.059(4) 0.053(3) 0.039(3) -0.010(3) -0.014(3) -0.007(3) C37 0.084(5) 0.053(4) 0.052(4) -0.019(3) -0.016(3) -0.003(3) C38 0.078(4) 0.065(4) 0.044(3) -0.018(3) -0.015(3) -0.010(3) C39 0.099(5) 0.064(4) 0.053(4) -0.019(3) -0.016(4) 0.001(4) C40 0.092(5) 0.063(4) 0.052(4) -0.024(3) -0.014(3) -0.009(4) C41 0.116(6) 0.073(5) 0.066(4) -0.027(4) -0.017(4) 0.008(4) C42 0.096(5) 0.079(5) 0.050(4) -0.027(3) -0.010(3) -0.009(4) C43 0.231(12) 0.095(6) 0.067(5) -0.039(5) -0.030(6) -0.035(7) C44 0.217(12) 0.135(9) 0.066(5) -0.043(6) -0.045(6) -0.017(8) C45 0.037(3) 0.036(3) 0.029(2) -0.003(2) -0.004(2) -0.004(2) C46 0.031(3) 0.032(3) 0.033(3) -0.007(2) -0.004(2) -0.008(2) C47 0.028(2) 0.031(3) 0.033(2) -0.006(2) -0.0011(19) -0.0021(19) C48 0.036(3) 0.033(3) 0.032(2) -0.006(2) -0.002(2) -0.002(2) C49 0.031(3) 0.031(2) 0.033(2) -0.007(2) -0.003(2) -0.005(2) C50 0.034(3) 0.036(3) 0.035(3) -0.010(2) -0.004(2) -0.005(2) O13 0.0380(19) 0.0246(17) 0.0374(18) 0.0014(14) -0.0101(14) -0.0075(14) C51 0.042(3) 0.030(3) 0.044(3) -0.005(2) -0.019(2) -0.006(2) C52 0.044(3) 0.038(3) 0.025(2) 0.002(2) -0.008(2) -0.007(2) O14 0.040(2) 0.0360(19) 0.060(2) 0.0003(18) -0.0175(17) -0.0030(16) O15 0.039(2) 0.036(2) 0.056(2) 0.0072(17) -0.0169(17) -0.0122(16) O16 0.060(2) 0.0361(19) 0.0323(18) -0.0096(15) -0.0141(16) -0.0020(16) C53 0.075(4) 0.056(4) 0.046(3) -0.002(3) -0.008(3) -0.014(3) C54 0.080(5) 0.090(5) 0.037(3) -0.021(4) -0.012(3) 0.002(4) O17 0.340(11) 0.056(3) 0.099(4) -0.037(3) -0.135(6) 0.051(5) O18 0.104(4) 0.123(5) 0.053(3) -0.024(3) -0.017(3) -0.003(4) C55 0.039(3) 0.025(2) 0.033(2) -0.006(2) -0.001(2) 0.000(2) C56 0.041(3) 0.031(3) 0.047(3) -0.004(2) -0.008(2) -0.004(2) C57 0.047(3) 0.039(3) 0.055(3) -0.003(3) -0.017(3) -0.005(2) C58 0.065(4) 0.060(4) 0.065(4) 0.010(3) -0.024(3) -0.017(3) C59 0.086(5) 0.069(5) 0.092(6) 0.008(4) -0.022(4) -0.006(4) C60 0.080(6) 0.106(7) 0.102(7) 0.035(6) -0.021(5) 0.002(5) C61 0.046(4) 0.109(7) 0.129(7) -0.005(6) -0.039(5) 0.010(4) C62 0.051(5) 0.156(10) 0.122(8) 0.062(7) -0.020(5) -0.012(5) C63 0.049(5) 0.090(6) 0.161(10) 0.052(6) -0.027(6) -0.007(4) C64 0.040(4) 0.123(8) 0.132(8) 0.002(7) -0.008(5) -0.009(4) C65 0.097(8) 0.091(7) 0.156(11) 0.028(7) -0.016(8) -0.022(6) C66 0.114(8) 0.157(10) 0.178(12) -0.072(9) 0.064(8) -0.053(8) C67 0.055(3) 0.029(3) 0.039(3) -0.014(2) -0.007(2) -0.011(2) C68 0.052(3) 0.027(2) 0.021(2) -0.0039(19) -0.008(2) -0.003(2) C69 0.040(3) 0.023(2) 0.026(2) -0.0044(19) -0.0077(19) -0.006(2) C70 0.042(3) 0.021(2) 0.033(2) -0.0065(19) -0.009(2) -0.006(2) C71 0.040(3) 0.024(2) 0.025(2) -0.0007(18) -0.0113(19) -0.007(2) C72 0.048(3) 0.028(3) 0.035(3) -0.007(2) -0.009(2) -0.015(2) O19 0.059(2) 0.0267(18) 0.042(2) -0.0132(15) -0.0003(17) 0.0015(16) C73 0.061(4) 0.034(3) 0.049(3) -0.017(2) -0.004(3) 0.001(3) C74 0.051(4) 0.048(4) 0.110(6) -0.049(4) -0.017(3) 0.009(3) O20 0.242(8) 0.071(4) 0.068(3) -0.026(3) -0.057(4) 0.029(4) O21 0.093(4) 0.060(3) 0.097(4) -0.035(3) -0.032(3) 0.002(2) O22 0.056(2) 0.059(3) 0.059(2) -0.020(2) -0.0088(19) -0.027(2) C76 0.102(6) 0.054(4) 0.084(5) -0.026(4) -0.040(4) 0.002(4) C75A 0.063(7) 0.061(7) 0.031(5) 0.000(5) -0.011(4) -0.009(5) O23A 0.067(5) 0.040(4) 0.063(5) -0.010(4) -0.009(4) -0.006(3) O24A 0.080(6) 0.076(6) 0.056(5) -0.034(5) -0.030(4) -0.001(5) C75B 0.066(9) 0.034(7) 0.058(8) -0.009(6) -0.018(7) -0.015(6) O23B 0.090(8) 0.058(7) 0.073(8) -0.023(6) -0.033(6) -0.027(6) O24B 0.160(14) 0.062(7) 0.053(7) -0.004(6) -0.027(7) 0.013(8) C77 0.039(3) 0.025(2) 0.029(2) -0.0036(19) -0.006(2) -0.009(2) C78 0.037(3) 0.028(2) 0.037(3) -0.001(2) -0.008(2) -0.001(2) C79 0.050(3) 0.042(3) 0.043(3) -0.012(2) -0.003(2) -0.008(2) C80 0.054(4) 0.058(4) 0.055(4) -0.013(3) 0.006(3) -0.007(3) C81 0.052(4) 0.064(4) 0.046(3) -0.006(3) -0.007(3) -0.004(3) C82 0.060(4) 0.067(4) 0.048(3) -0.016(3) 0.004(3) 0.001(3) C83 0.065(4) 0.080(5) 0.044(3) 0.001(3) -0.005(3) -0.011(3) C84 0.072(4) 0.082(5) 0.048(4) -0.018(3) 0.001(3) -0.002(4) C85 0.066(4) 0.071(4) 0.048(3) 0.001(3) -0.006(3) 0.000(3) C86 0.068(4) 0.077(5) 0.046(3) -0.011(3) 0.003(3) -0.004(3) C87 0.075(5) 0.079(5) 0.056(4) -0.006(3) -0.005(3) -0.011(4) C88 0.097(6) 0.108(6) 0.059(4) -0.018(4) -0.014(4) -0.005(5) O29 0.0310(16) 0.0141(14) 0.0151(13) -0.0013(11) -0.0073(11) -0.0064(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.386(7) . ? C1 C2 1.403(7) . ? C2 O1 1.369(5) . ? C2 C3 1.391(6) . ? C3 C4 1.381(6) . ? C3 C77 1.527(6) . ? C4 C5 1.407(6) . ? C5 C6 1.373(6) . ? C5 C11 1.529(6) . ? C6 O4 1.384(5) . ? O1 C7 1.417(5) . ? C7 C8 1.468(7) . ? C8 O2 1.225(6) . ? C8 O3 1.269(6) . ? O4 C9 1.426(5) . ? C9 C10 1.512(7) . ? C10 O6 1.206(5) . ? C10 O5 1.298(6) . ? C11 C12 1.529(6) . ? C11 C25 1.530(6) . ? C12 C13 1.516(7) . ? C13 C14 1.516(7) . ? C14 C15 1.500(8) . ? C15 C16 1.507(8) . ? C16 C17 1.476(9) . ? C17 C18 1.497(9) . ? C18 C19 1.482(10) . ? C19 C20 1.544(11) . ? C20 C21B 1.551(17) . ? C20 C21A 1.591(12) . ? C21A C22A 1.416(13) . ? C21B C22B 1.471(18) . ? C23 C24 1.370(7) . ? C23 C28 1.385(7) . ? C24 O7 1.390(6) . ? C24 C25 1.402(6) . ? C25 C26 1.384(6) . ? C26 C27 1.386(6) . ? C27 C28 1.395(6) . ? C27 C33 1.540(6) . ? C28 O10 1.384(6) . ? O7 C29 1.394(7) . ? C29 C30 1.537(9) . ? C30 O8 1.229(7) . ? C30 O9 1.234(7) . ? O10 C31 1.445(8) . ? C31 C32 1.327(12) . ? C32 O12 1.232(10) . ? C32 O11 1.362(12) . ? C33 C47 1.536(6) . ? C33 C34 1.550(6) . ? C34 C35 1.517(7) . ? C35 C36 1.523(7) . ? C36 C37 1.495(8) . ? C37 C38 1.542(8) . ? C38 C39 1.494(8) . ? C39 C40 1.504(8) . ? C40 C41 1.481(9) . ? C41 C42 1.534(9) . ? C42 C43 1.518(10) . ? C43 C44 1.518(11) . ? C45 C50 1.376(7) . ? C45 C46 1.377(6) . ? C46 C47 1.373(6) . ? C46 O13 1.393(5) . ? C47 C48 1.390(6) . ? C48 C49 1.393(7) . ? C49 C50 1.421(6) . ? C49 C55 1.532(6) . ? C50 O16 1.374(6) . ? O13 C51 1.401(5) . ? C51 C52 1.503(7) . ? C52 O15 1.213(6) . ? C52 O14 1.300(6) . ? O16 C53 1.470(6) . ? C53 C54 1.476(9) . ? C54 O17 1.196(9) . ? C54 O18 1.312(7) . ? C55 C69 1.521(7) . ? C55 C56 1.554(6) . ? C56 C57 1.509(7) . ? C57 C58 1.535(7) . ? C58 C59 1.451(9) . ? C59 C60 1.586(11) . ? C60 C61 1.471(13) . ? C61 C62 1.623(12) . ? C62 C63 1.496(15) . ? C63 C64 1.540(12) . ? C64 C65 1.437(15) . ? C65 C66 1.583(15) . ? C67 C72 1.371(7) . ? C67 C68 1.383(7) . ? C68 O19 1.388(6) . ? C68 C69 1.410(6) . ? C69 C70 1.383(6) . ? C70 C71 1.392(6) . ? C71 C72 1.400(6) . ? C71 C77 1.520(6) . ? C72 O22 1.393(6) . ? O19 C73 1.397(6) . ? C73 C74 1.596(9) . ? C74 O20 1.176(8) . ? C74 O21 1.283(7) . ? O22 C75B 1.328(12) . ? O22 C75A 1.381(10) . ? C76 O23B 1.176(11) . ? C76 O24A 1.245(9) . ? C76 O23A 1.361(10) . ? C76 O24B 1.430(14) . ? C76 C75A 1.437(12) . ? C76 C75B 1.464(14) . ? C77 C78 1.531(6) . ? C78 C79 1.517(7) . ? C79 C80 1.525(7) . ? C80 C81 1.519(8) . ? C81 C82 1.488(8) . ? C82 C83 1.549(9) . ? C83 C84 1.522(8) . ? C84 C85 1.496(9) . ? C85 C86 1.510(8) . ? C86 C87 1.487(9) . ? C87 C88 1.486(9) . ? O25A C89A 1.259(14) . ? O26A C89A 1.277(14) . ? C89A C90A 1.528(16) . ? O31 O32 0.587(18) . ? 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 C6 C1 C2 119.7(4) . . ? O1 C2 C3 117.2(4) . . ? O1 C2 C1 122.2(4) . . ? C3 C2 C1 120.5(4) . . ? C4 C3 C2 117.3(4) . . ? C4 C3 C77 122.9(4) . . ? C2 C3 C77 119.8(4) . . ? C3 C4 C5 124.0(4) . . ? C6 C5 C4 116.6(4) . . ? C6 C5 C11 119.9(4) . . ? C4 C5 C11 123.5(4) . . ? C5 C6 O4 115.6(4) . . ? C5 C6 C1 121.9(4) . . ? O4 C6 C1 122.5(4) . . ? C2 O1 C7 117.2(3) . . ? O1 C7 C8 113.5(4) . . ? O2 C8 O3 124.0(5) . . ? O2 C8 C7 120.5(5) . . ? O3 C8 C7 115.5(4) . . ? C6 O4 C9 119.3(4) . . ? O4 C9 C10 114.0(4) . . ? O6 C10 O5 124.4(5) . . ? O6 C10 C9 120.4(5) . . ? O5 C10 C9 115.2(4) . . ? C5 C11 C12 113.7(4) . . ? C5 C11 C25 111.1(4) . . ? C12 C11 C25 109.8(4) . . ? C13 C12 C11 115.0(4) . . ? C14 C13 C12 113.3(5) . . ? C15 C14 C13 114.4(5) . . ? C14 C15 C16 116.6(5) . . ? C17 C16 C15 115.9(6) . . ? C16 C17 C18 117.3(6) . . ? C19 C18 C17 116.5(7) . . ? C18 C19 C20 116.0(8) . . ? C19 C20 C21B 119.9(12) . . ? C19 C20 C21A 113.9(9) . . ? C21B C20 C21A 48.9(12) . . ? C22A C21A C20 110.3(10) . . ? C22B C21B C20 109.3(17) . . ? C24 C23 C28 120.0(5) . . ? C23 C24 O7 122.2(4) . . ? C23 C24 C25 121.1(4) . . ? O7 C24 C25 116.7(4) . . ? C26 C25 C24 117.1(4) . . ? C26 C25 C11 120.2(4) . . ? C24 C25 C11 122.6(4) . . ? C25 C26 C27 123.5(4) . . ? C26 C27 C28 117.0(4) . . ? C26 C27 C33 119.8(4) . . ? C28 C27 C33 123.2(4) . . ? O10 C28 C23 121.5(4) . . ? O10 C28 C27 117.4(4) . . ? C23 C28 C27 121.0(4) . . ? C24 O7 C29 121.1(5) . . ? O7 C29 C30 112.9(5) . . ? O8 C30 O9 125.1(7) . . ? O8 C30 C29 119.0(5) . . ? O9 C30 C29 115.8(6) . . ? C28 O10 C31 115.7(5) . . ? C32 C31 O10 115.7(8) . . ? O12 C32 C31 127.3(12) . . ? O12 C32 O11 115.3(11) . . ? C31 C32 O11 117.4(8) . . ? C47 C33 C27 108.8(3) . . ? C47 C33 C34 113.5(4) . . ? C27 C33 C34 110.3(4) . . ? C35 C34 C33 112.7(4) . . ? C34 C35 C36 113.3(4) . . ? C37 C36 C35 113.5(5) . . ? C36 C37 C38 115.8(5) . . ? C39 C38 C37 114.5(5) . . ? C38 C39 C40 116.9(5) . . ? C41 C40 C39 115.0(6) . . ? C40 C41 C42 115.9(6) . . ? C43 C42 C41 113.5(6) . . ? C44 C43 C42 113.9(7) . . ? C50 C45 C46 120.6(4) . . ? C47 C46 C45 122.4(4) . . ? C47 C46 O13 118.3(4) . . ? C45 C46 O13 119.1(4) . . ? C46 C47 C48 116.4(4) . . ? C46 C47 C33 119.3(4) . . ? C48 C47 C33 124.1(4) . . ? C47 C48 C49 123.9(4) . . ? C48 C49 C50 117.0(4) . . ? C48 C49 C55 123.1(4) . . ? C50 C49 C55 119.9(4) . . ? O16 C50 C45 123.2(4) . . ? O16 C50 C49 117.2(4) . . ? C45 C50 C49 119.6(4) . . ? C46 O13 C51 114.3(3) . . ? O13 C51 C52 108.9(4) . . ? O15 C52 O14 125.5(5) . . ? O15 C52 C51 123.3(4) . . ? O14 C52 C51 111.2(4) . . ? C50 O16 C53 115.0(4) . . ? O16 C53 C54 110.2(5) . . ? O17 C54 O18 124.5(6) . . ? O17 C54 C53 124.2(6) . . ? O18 C54 C53 111.2(6) . . ? C69 C55 C49 113.3(4) . . ? C69 C55 C56 110.1(4) . . ? C49 C55 C56 111.4(4) . . ? C57 C56 C55 116.4(4) . . ? C56 C57 C58 112.1(5) . . ? C59 C58 C57 115.6(6) . . ? C58 C59 C60 110.4(7) . . ? C61 C60 C59 116.5(7) . . ? C60 C61 C62 113.6(7) . . ? C63 C62 C61 117.0(8) . . ? C62 C63 C64 113.5(8) . . ? C65 C64 C63 114.1(9) . . ? C64 C65 C66 120.6(9) . . ? C72 C67 C68 119.7(4) . . ? C67 C68 O19 123.3(4) . . ? C67 C68 C69 121.0(4) . . ? O19 C68 C69 115.7(4) . . ? C70 C69 C68 116.7(4) . . ? C70 C69 C55 121.9(4) . . ? C68 C69 C55 121.3(4) . . ? C69 C70 C71 124.1(4) . . ? C70 C71 C72 116.3(4) . . ? C70 C71 C77 123.1(4) . . ? C72 C71 C77 120.3(4) . . ? C67 C72 O22 121.0(4) . . ? C67 C72 C71 121.9(4) . . ? O22 C72 C71 117.0(4) . . ? C68 O19 C73 118.9(4) . . ? O19 C73 C74 108.4(4) . . ? O20 C74 O21 126.5(7) . . ? O20 C74 C73 122.7(5) . . ? O21 C74 C73 110.7(6) . . ? C75B O22 C75A 63.4(7) . . ? C75B O22 C72 129.0(7) . . ? C75A O22 C72 111.5(5) . . ? O23B C76 O24A 52.7(6) . . ? O23B C76 O23A 69.0(8) . . ? O24A C76 O23A 118.4(9) . . ? O23B C76 O24B 116.6(10) . . ? O24A C76 O24B 76.9(8) . . ? O23A C76 O24B 157.1(9) . . ? O23B C76 C75A 173.6(10) . . ? O24A C76 C75A 121.3(8) . . ? O23A C76 C75A 117.4(7) . . ? O24B C76 C75A 57.6(7) . . ? O23B C76 C75B 127.5(10) . . ? O24A C76 C75B 170.9(10) . . ? O23A C76 C75B 59.2(6) . . ? O24B C76 C75B 108.3(9) . . ? C75A C76 C75B 58.8(6) . . ? O22 C75A C76 117.7(7) . . ? O22 C75B C76 119.5(10) . . ? C71 C77 C3 112.3(4) . . ? C71 C77 C78 109.0(3) . . ? C3 C77 C78 115.3(4) . . ? C79 C78 C77 113.8(4) . . ? C78 C79 C80 114.1(4) . . ? C81 C80 C79 114.7(5) . . ? C82 C81 C80 113.0(5) . . ? C81 C82 C83 115.5(5) . . ? C84 C83 C82 113.5(5) . . ? C85 C84 C83 114.5(6) . . ? C84 C85 C86 114.6(6) . . ? C87 C86 C85 116.0(6) . . ? C88 C87 C86 115.4(6) . . ? O25A C89A O26A 129.1(12) . . ? O25A C89A C90A 117.3(12) . . ? O26A C89A C90A 113.5(11) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.335 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.094 #============================================================================== data_march _database_code_depnum_ccdc_archive 'CCDC 232972' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C154 H232 O26' _chemical_formula_weight 2499.40 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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.9691(15) _cell_length_b 18.4700(8) _cell_length_c 49.942(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.5210(10) _cell_angle_gamma 90.00 _cell_volume 30586(2) _cell_formula_units_Z 8 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 6886 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 24.29 _exptl_crystal_description block-shaped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.086 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10912 _exptl_absorpt_coefficient_mu 0.072 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 'Bruker AXS SMART' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 77537 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.0549 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -59 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 25.02 _reflns_number_total 26912 _reflns_number_gt 17358 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS SMART' _computing_cell_refinement 'Bruker AXS SAINT' _computing_data_reduction 'Bruker AXS SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Crystal Impact: DIAMOND; Bruker AXS: SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1316P)^2^+74.1607P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 26912 _refine_ls_number_parameters 1665 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1249 _refine_ls_R_factor_gt 0.0834 _refine_ls_wR_factor_ref 0.2601 _refine_ls_wR_factor_gt 0.2259 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.010 _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 0.20093(7) 0.30172(12) 0.20007(5) 0.0335(5) Uani 1 1 d . . . O2 O 0.28428(8) 0.31153(18) 0.21145(6) 0.0599(8) Uani 1 1 d . . . O3 O 0.27681(8) 0.28045(15) 0.16673(5) 0.0480(7) Uani 1 1 d . . . O4 O 0.31166(7) 0.09816(12) 0.23984(4) 0.0321(5) Uani 1 1 d . . . O5 O 0.32546(11) 0.15299(16) 0.29256(6) 0.0653(9) Uani 1 1 d . . . O6 O 0.37297(11) 0.22554(19) 0.28690(6) 0.0742(10) Uani 1 1 d . . . O7 O 0.40236(7) 0.13725(13) 0.20430(5) 0.0394(6) Uani 1 1 d . . . O8 O 0.47214(10) 0.1992(2) 0.26899(7) 0.0793(11) Uani 1 1 d . . . O9 O 0.42274(9) 0.25369(16) 0.23473(6) 0.0544(7) Uani 1 1 d . . . O10 O 0.48087(6) 0.28482(12) 0.16021(5) 0.0321(5) Uani 1 1 d . . . O11 O 0.50517(9) 0.42374(16) 0.17947(8) 0.0683(9) Uani 1 1 d . . . O12 O 0.45304(10) 0.43100(18) 0.19598(8) 0.0715(10) Uani 1 1 d . . . O13 O 0.40896(7) 0.44864(14) 0.12854(5) 0.0363(6) Uani 1 1 d . . . O14 O 0.35451(9) 0.49276(18) 0.15546(6) 0.0600(8) Uani 1 1 d . . . O15 O 0.30685(7) 0.42340(15) 0.12583(6) 0.0501(7) Uani 1 1 d . . . O16 O 0.32561(7) 0.68857(13) 0.11973(5) 0.0348(5) Uani 1 1 d . . . O17 O 0.31247(9) 0.78632(16) 0.15735(6) 0.0548(7) Uani 1 1 d . . . O18 O 0.35292(9) 0.72098(15) 0.19259(6) 0.0544(7) Uani 1 1 d . . . O19 O 0.23103(7) 0.62486(12) 0.14349(5) 0.0332(5) Uani 1 1 d . . . O20 O 0.27122(10) 0.69298(19) 0.21318(6) 0.0693(9) Uani 1 1 d . . . O21 O 0.27574(11) 0.58789(18) 0.19283(6) 0.0740(10) Uani 1 1 d . . . O22 O 0.14683(6) 0.48073(12) 0.19049(4) 0.0296(5) Uani 1 1 d . . . O23 O 0.16968(9) 0.41873(16) 0.24359(5) 0.0503(7) Uani 1 1 d . . . O24 O 0.23442(9) 0.4325(2) 0.24679(6) 0.0668(9) Uani 1 1 d . . . C1 C 0.17475(9) 0.24364(17) 0.19903(6) 0.0274(7) Uani 1 1 d . . . C2 C 0.13331(10) 0.25906(17) 0.19118(6) 0.0290(7) Uani 1 1 d . . . C3 C 0.10731(10) 0.20170(18) 0.18948(7) 0.0306(7) Uani 1 1 d . . . H3 H 0.0793 0.2115 0.1846 0.037 Uiso 1 1 calc R . . C4 C 0.12028(10) 0.13004(18) 0.19452(7) 0.0308(7) Uani 1 1 d . . . C5 C 0.16140(10) 0.11812(18) 0.20380(7) 0.0307(7) Uani 1 1 d . . . H5 H 0.1711 0.0702 0.2084 0.037 Uiso 1 1 calc R . . C6 C 0.18944(9) 0.17469(18) 0.20664(6) 0.0287(7) Uani 1 1 d . . . C7 C 0.08924(11) 0.06880(19) 0.19144(8) 0.0386(8) Uani 1 1 d . . . C8 C 0.07466(14) 0.0735(3) 0.21751(10) 0.0594(12) Uani 1 1 d . . . H8A H 0.0980 0.0720 0.2347 0.089 Uiso 1 1 calc R . . H8B H 0.0568 0.0326 0.2174 0.089 Uiso 1 1 calc R . . H8C H 0.0600 0.1190 0.2169 0.089 Uiso 1 1 calc R . . C9 C 0.10842(13) -0.0060(2) 0.19214(10) 0.0552(11) Uani 1 1 d . . . H9A H 0.1222 -0.0082 0.1779 0.083 Uiso 1 1 calc R . . H9B H 0.0874 -0.0432 0.1881 0.083 Uiso 1 1 calc R . . H9C H 0.1279 -0.0145 0.2109 0.083 Uiso 1 1 calc R . . C10 C 0.05177(11) 0.0786(2) 0.16518(9) 0.0461(9) Uani 1 1 d . . . H10A H 0.0408 0.1273 0.1668 0.055 Uiso 1 1 calc R . . H10B H 0.0315 0.0433 0.1671 0.055 Uiso 1 1 calc R . . C11 C 0.05279(14) 0.0719(2) 0.13461(9) 0.0579(11) Uani 1 1 d . . . C12 C 0.08820(18) 0.1115(3) 0.12914(10) 0.0809(17) Uani 1 1 d . . . H12A H 0.0867 0.1049 0.1094 0.121 Uiso 1 1 calc R . . H12B H 0.1137 0.0916 0.1415 0.121 Uiso 1 1 calc R . . H12C H 0.0868 0.1632 0.1331 0.121 Uiso 1 1 calc R . . C13 C 0.0130(2) 0.1036(4) 0.11601(12) 0.102(2) Uani 1 1 d . . . H13A H 0.0118 0.1551 0.1204 0.154 Uiso 1 1 calc R . . H13B H -0.0095 0.0781 0.1196 0.154 Uiso 1 1 calc R . . H13C H 0.0111 0.0980 0.0961 0.154 Uiso 1 1 calc R . . C14 C 0.05406(16) -0.0074(3) 0.12553(12) 0.0747(14) Uani 1 1 d . . . H14A H 0.0327 -0.0348 0.1297 0.112 Uiso 1 1 calc R . . H14B H 0.0803 -0.0284 0.1359 0.112 Uiso 1 1 calc R . . H14C H 0.0500 -0.0094 0.1052 0.112 Uiso 1 1 calc R . . C15 C 0.21770(10) 0.3024(2) 0.17724(7) 0.0367(8) Uani 1 1 d . . . H15A H 0.2092 0.3472 0.1661 0.044 Uiso 1 1 calc R . . H15B H 0.2070 0.2607 0.1646 0.044 Uiso 1 1 calc R . . C16 C 0.26307(11) 0.2986(2) 0.18793(8) 0.0397(9) Uani 1 1 d . . . C17 C 0.32055(12) 0.2750(3) 0.17378(9) 0.0572(11) Uani 1 1 d . . . H17A H 0.3319 0.2460 0.1912 0.069 Uiso 1 1 calc R . . H17B H 0.3329 0.3239 0.1771 0.069 Uiso 1 1 calc R . . C18 C 0.32936(15) 0.2393(3) 0.14947(11) 0.0674(13) Uani 1 1 d . . . H18A H 0.3183 0.1901 0.1471 0.101 Uiso 1 1 calc R . . H18B H 0.3586 0.2373 0.1532 0.101 Uiso 1 1 calc R . . H18C H 0.3169 0.2673 0.1322 0.101 Uiso 1 1 calc R . . C19 C 0.23403(10) 0.15790(19) 0.21885(7) 0.0316(7) Uani 1 1 d . . . H19A H 0.2382 0.1281 0.2360 0.038 Uiso 1 1 calc R . . H19B H 0.2486 0.2041 0.2249 0.038 Uiso 1 1 calc R . . C20 C 0.29219(9) 0.09166(18) 0.21065(6) 0.0282(7) Uani 1 1 d . . . C21 C 0.25332(9) 0.11889(17) 0.19968(7) 0.0288(7) Uani 1 1 d . . . C22 C 0.23304(10) 0.10856(17) 0.17093(7) 0.0290(7) Uani 1 1 d . . . H22 H 0.2062 0.1259 0.1633 0.035 Uiso 1 1 calc R . . C23 C 0.25076(10) 0.07387(18) 0.15311(7) 0.0305(7) Uani 1 1 d . . . C24 C 0.28980(10) 0.04779(18) 0.16523(7) 0.0323(7) Uani 1 1 d . . . H24 H 0.3025 0.0243 0.1534 0.039 Uiso 1 1 calc R . . C25 C 0.31099(10) 0.05452(18) 0.19383(7) 0.0297(7) Uani 1 1 d . . . C26 C 0.22830(11) 0.0647(2) 0.12145(7) 0.0381(8) Uani 1 1 d . . . C27 C 0.2005(3) 0.1260(4) 0.11048(11) 0.161(5) Uani 1 1 d . . . H27A H 0.1787 0.1248 0.1189 0.242 Uiso 1 1 calc R . . H27B H 0.1891 0.1220 0.0899 0.242 Uiso 1 1 calc R . . H27C H 0.2154 0.1717 0.1154 0.242 Uiso 1 1 calc R . . C28 C 0.25629(19) 0.0653(9) 0.10493(12) 0.247(8) Uani 1 1 d . . . H28A H 0.2769 0.0279 0.1121 0.370 Uiso 1 1 calc R . . H28B H 0.2693 0.1128 0.1066 0.370 Uiso 1 1 calc R . . H28C H 0.2414 0.0555 0.0851 0.370 Uiso 1 1 calc R . . C29 C 0.2062(5) 0.0002(5) 0.11500(17) 0.302(11) Uani 1 1 d . . . H29A H 0.2103 -0.0114 0.0968 0.363 Uiso 1 1 calc R . . H29B H 0.1785 0.0202 0.1096 0.363 Uiso 1 1 calc R . . C30 C 0.19856(13) -0.0712(2) 0.12341(9) 0.0525(10) Uani 1 1 d . . . C31 C 0.1580(3) -0.0757(10) 0.1258(3) 0.247(8) Uani 1 1 d . . . H31A H 0.1542 -0.0364 0.1379 0.370 Uiso 1 1 calc R . . H31B H 0.1547 -0.1224 0.1341 0.370 Uiso 1 1 calc R . . H31C H 0.1380 -0.0713 0.1070 0.370 Uiso 1 1 calc R . . C32 C 0.1971(2) -0.1244(5) 0.10055(18) 0.140(3) Uani 1 1 d . . . H32A H 0.1788 -0.1064 0.0825 0.210 Uiso 1 1 calc R . . H32B H 0.1873 -0.1711 0.1050 0.210 Uiso 1 1 calc R . . H32C H 0.2242 -0.1304 0.0991 0.210 Uiso 1 1 calc R . . C33 C 0.2279(2) -0.0939(3) 0.15114(13) 0.100(2) Uani 1 1 d . . . H33A H 0.2553 -0.0927 0.1499 0.150 Uiso 1 1 calc R . . H33B H 0.2215 -0.1432 0.1556 0.150 Uiso 1 1 calc R . . H33C H 0.2261 -0.0607 0.1660 0.150 Uiso 1 1 calc R . . C34 C 0.33580(11) 0.1619(2) 0.24728(7) 0.0393(8) Uani 1 1 d . . . H34A H 0.3216 0.2033 0.2358 0.047 Uiso 1 1 calc R . . H34B H 0.3617 0.1546 0.2435 0.047 Uiso 1 1 calc R . . C35 C 0.34363(12) 0.1774(2) 0.27794(8) 0.0439(9) Uani 1 1 d . . . C36 C 0.3811(2) 0.2492(4) 0.31688(11) 0.101(2) Uani 1 1 d . . . H36A H 0.3580 0.2776 0.3185 0.121 Uiso 1 1 calc R . . H36B H 0.3845 0.2062 0.3292 0.121 Uiso 1 1 calc R . . C37 C 0.4147(3) 0.2897(4) 0.32523(14) 0.140(3) Uani 1 1 d . . . H37A H 0.4375 0.2616 0.3234 0.210 Uiso 1 1 calc R . . H37B H 0.4201 0.3040 0.3450 0.210 Uiso 1 1 calc R . . H37C H 0.4110 0.3332 0.3134 0.210 Uiso 1 1 calc R . . C38 C 0.35177(10) 0.01729(19) 0.20629(7) 0.0333(8) Uani 1 1 d . . . H38A H 0.3668 0.0414 0.2243 0.040 Uiso 1 1 calc R . . H38B H 0.3473 -0.0337 0.2106 0.040 Uiso 1 1 calc R . . C39 C 0.40072(10) 0.07959(18) 0.18567(7) 0.0319(7) Uani 1 1 d . . . C40 C 0.37714(10) 0.01892(18) 0.18666(7) 0.0318(7) Uani 1 1 d . . . C41 C 0.37630(10) -0.03770(18) 0.16831(7) 0.0335(8) Uani 1 1 d . . . H41 H 0.3602 -0.0789 0.1687 0.040 Uiso 1 1 calc R . . C42 C 0.39825(11) -0.03664(19) 0.14914(8) 0.0386(8) Uani 1 1 d . . . C43 C 0.42051(11) 0.02520(19) 0.14870(8) 0.0389(8) Uani 1 1 d . . . H43 H 0.4355 0.0274 0.1358 0.047 Uiso 1 1 calc R . . C44 C 0.42184(10) 0.08442(19) 0.16634(7) 0.0352(8) Uani 1 1 d . . . C45 C 0.39446(13) -0.1006(2) 0.12841(9) 0.0475(10) Uani 1 1 d . . . C46 C 0.34935(15) -0.1092(3) 0.11130(10) 0.0636(12) Uani 1 1 d . . . H46A H 0.3462 -0.1477 0.0973 0.095 Uiso 1 1 calc R . . H46B H 0.3391 -0.0636 0.1017 0.095 Uiso 1 1 calc R . . H46C H 0.3342 -0.1218 0.1241 0.095 Uiso 1 1 calc R . . C47 C 0.41654(19) -0.0847(3) 0.10684(11) 0.0761(16) Uani 1 1 d . . . H47A H 0.4450 -0.0741 0.1169 0.114 Uiso 1 1 calc R . . H47B H 0.4040 -0.0429 0.0953 0.114 Uiso 1 1 calc R . . H47C H 0.4147 -0.1271 0.0947 0.114 Uiso 1 1 calc R . . C48 C 0.40768(12) -0.1735(2) 0.14358(10) 0.0505(10) Uani 1 1 d . . . H48A H 0.3907 -0.1809 0.1559 0.061 Uiso 1 1 calc R . . H48B H 0.3996 -0.2113 0.1288 0.061 Uiso 1 1 calc R . . C49 C 0.45102(14) -0.1916(3) 0.16164(13) 0.0702(14) Uani 1 1 d . . . C50 C 0.4665(2) -0.1397(4) 0.18616(19) 0.151(4) Uani 1 1 d . . . H50A H 0.4934 -0.1548 0.1979 0.227 Uiso 1 1 calc R . . H50B H 0.4482 -0.1400 0.1975 0.227 Uiso 1 1 calc R . . H50C H 0.4678 -0.0907 0.1789 0.227 Uiso 1 1 calc R . . C51 C 0.45043(19) -0.2678(3) 0.17371(16) 0.102(2) Uani 1 1 d . . . H51A H 0.4776 -0.2807 0.1858 0.153 Uiso 1 1 calc R . . H51B H 0.4414 -0.3027 0.1582 0.153 Uiso 1 1 calc R . . H51C H 0.4319 -0.2687 0.1849 0.153 Uiso 1 1 calc R . . C52 C 0.4806(3) -0.1955(6) 0.1451(3) 0.192(5) Uani 1 1 d . . . H52A H 0.4900 -0.1467 0.1428 0.288 Uiso 1 1 calc R . . H52B H 0.4672 -0.2169 0.1265 0.288 Uiso 1 1 calc R . . H52C H 0.5037 -0.2256 0.1554 0.288 Uiso 1 1 calc R . . C53 C 0.43663(11) 0.1305(2) 0.22926(8) 0.0441(9) Uani 1 1 d . . . H53A H 0.4605 0.1174 0.2237 0.053 Uiso 1 1 calc R . . H53B H 0.4317 0.0906 0.2410 0.053 Uiso 1 1 calc R . . C54 C 0.44559(12) 0.1976(3) 0.24642(9) 0.0501(10) Uani 1 1 d . . . C55 C 0.43064(16) 0.3208(3) 0.25117(11) 0.0697(14) Uani 1 1 d . . . H55A H 0.4344 0.3104 0.2713 0.084 Uiso 1 1 calc R . . H55B H 0.4554 0.3442 0.2498 0.084 Uiso 1 1 calc R . . C56 C 0.39604(17) 0.3680(3) 0.23957(12) 0.0782(16) Uani 1 1 d . . . H56A H 0.3922 0.3770 0.2195 0.117 Uiso 1 1 calc R . . H56B H 0.4007 0.4141 0.2498 0.117 Uiso 1 1 calc R . . H56C H 0.3719 0.3449 0.2415 0.117 Uiso 1 1 calc R . . C57 C 0.44573(11) 0.1515(2) 0.16478(8) 0.0417(9) Uani 1 1 d . . . H57A H 0.4740 0.1368 0.1676 0.050 Uiso 1 1 calc R . . H57B H 0.4460 0.1834 0.1807 0.050 Uiso 1 1 calc R . . C58 C 0.45011(9) 0.26119(18) 0.13634(7) 0.0288(7) Uani 1 1 d . . . C59 C 0.43100(10) 0.19556(18) 0.13763(7) 0.0309(7) Uani 1 1 d . . . C60 C 0.40051(10) 0.17346(19) 0.11346(7) 0.0345(8) Uani 1 1 d . . . H60 H 0.3865 0.1298 0.1142 0.041 Uiso 1 1 calc R . . C61 C 0.38974(10) 0.21269(19) 0.08828(7) 0.0330(8) Uani 1 1 d . . . C62 C 0.41070(10) 0.27629(19) 0.08790(7) 0.0328(8) Uani 1 1 d . . . H62 H 0.4041 0.3035 0.0709 0.039 Uiso 1 1 calc R . . C63 C 0.44109(9) 0.30192(17) 0.11152(7) 0.0293(7) Uani 1 1 d . . . C64 C 0.35695(11) 0.1829(2) 0.06220(8) 0.0405(9) Uani 1 1 d . . . C65 C 0.31919(12) 0.1638(3) 0.07054(10) 0.0630(13) Uani 1 1 d . . . H65A H 0.3261 0.1265 0.0853 0.095 Uiso 1 1 calc R . . H65B H 0.2980 0.1456 0.0539 0.095 Uiso 1 1 calc R . . H65C H 0.3096 0.2072 0.0777 0.095 Uiso 1 1 calc R . . C66 C 0.34269(14) 0.2396(3) 0.03854(9) 0.0643(13) Uani 1 1 d . . . H66A H 0.3318 0.2818 0.0456 0.096 Uiso 1 1 calc R . . H66B H 0.3216 0.2186 0.0225 0.096 Uiso 1 1 calc R . . H66C H 0.3655 0.2546 0.0325 0.096 Uiso 1 1 calc R . . C67 C 0.36982(12) 0.1117(2) 0.05118(9) 0.0515(10) Uani 1 1 d . . . H67A H 0.3705 0.0742 0.0655 0.062 Uiso 1 1 calc R . . H67B H 0.3475 0.0983 0.0340 0.062 Uiso 1 1 calc R . . C68 C 0.40911(13) 0.1024(3) 0.04361(9) 0.0546(11) Uani 1 1 d . . . C69 C 0.44672(12) 0.1013(3) 0.06967(9) 0.0545(11) Uani 1 1 d . . . H69A H 0.4501 0.1488 0.0789 0.082 Uiso 1 1 calc R . . H69B H 0.4704 0.0904 0.0640 0.082 Uiso 1 1 calc R . . H69C H 0.4437 0.0641 0.0828 0.082 Uiso 1 1 calc R . . C70 C 0.40570(19) 0.0271(4) 0.02956(14) 0.101(2) Uani 1 1 d . . . H70A H 0.4003 -0.0095 0.0421 0.151 Uiso 1 1 calc R . . H70B H 0.4310 0.0155 0.0261 0.151 Uiso 1 1 calc R . . H70C H 0.3836 0.0275 0.0116 0.151 Uiso 1 1 calc R . . C71 C 0.41420(17) 0.1613(4) 0.02306(11) 0.0885(18) Uani 1 1 d . . . H71A H 0.3898 0.1635 0.0066 0.133 Uiso 1 1 calc R . . H71B H 0.4374 0.1494 0.0169 0.133 Uiso 1 1 calc R . . H71C H 0.4187 0.2083 0.0327 0.133 Uiso 1 1 calc R . . C72 C 0.46725(11) 0.3167(2) 0.18151(7) 0.0383(8) Uani 1 1 d . . . H72A H 0.4797 0.2912 0.1996 0.046 Uiso 1 1 calc R . . H72B H 0.4376 0.3111 0.1763 0.046 Uiso 1 1 calc R . . C73 C 0.47794(12) 0.3957(2) 0.18513(9) 0.0478(10) Uani 1 1 d . . . C74 C 0.4567(2) 0.5131(3) 0.19694(15) 0.0937(19) Uani 1 1 d . . . H74A H 0.4852 0.5270 0.2062 0.112 Uiso 1 1 calc R . . H74B H 0.4481 0.5326 0.1775 0.112 Uiso 1 1 calc R . . C75 C 0.4332(3) 0.5419(4) 0.21156(18) 0.127(3) Uani 1 1 d . . . H75A H 0.4053 0.5254 0.2031 0.190 Uiso 1 1 calc R . . H75B H 0.4340 0.5949 0.2107 0.190 Uiso 1 1 calc R . . H75C H 0.4433 0.5261 0.2313 0.190 Uiso 1 1 calc R . . C76 C 0.46539(9) 0.36906(18) 0.11010(7) 0.0310(7) Uani 1 1 d . . . H76A H 0.4794 0.3853 0.1297 0.037 Uiso 1 1 calc R . . H76B H 0.4864 0.3552 0.1016 0.037 Uiso 1 1 calc R . . C77 C 0.41585(9) 0.47313(18) 0.10394(6) 0.0287(7) Uani 1 1 d . . . C78 C 0.44225(9) 0.43263(17) 0.09373(7) 0.0284(7) Uani 1 1 d . . . C79 C 0.44860(10) 0.45653(18) 0.06908(7) 0.0308(7) Uani 1 1 d . . . H79 H 0.4664 0.4297 0.0619 0.037 Uiso 1 1 calc R . . C80 C 0.43006(10) 0.51803(19) 0.05431(7) 0.0317(7) Uani 1 1 d . . . C81 C 0.40640(10) 0.55829(19) 0.06641(7) 0.0323(7) Uani 1 1 d . . . H81 H 0.3946 0.6018 0.0573 0.039 Uiso 1 1 calc R . . C82 C 0.39915(9) 0.53794(19) 0.09129(7) 0.0309(7) Uani 1 1 d . . . C83 C 0.43763(11) 0.5414(2) 0.02674(7) 0.0406(9) Uani 1 1 d . . . C84 C 0.48192(13) 0.5670(3) 0.03459(9) 0.0594(12) Uani 1 1 d . . . H84A H 0.4878 0.5816 0.0174 0.089 Uiso 1 1 calc R . . H84B H 0.4999 0.5273 0.0438 0.089 Uiso 1 1 calc R . . H84C H 0.4861 0.6082 0.0476 0.089 Uiso 1 1 calc R . . C85 C 0.41047(16) 0.6046(3) 0.01265(9) 0.0632(13) Uani 1 1 d . . . H85A H 0.3823 0.5925 0.0104 0.095 Uiso 1 1 calc R . . H85B H 0.4133 0.6138 -0.0059 0.095 Uiso 1 1 calc R . . H85C H 0.4183 0.6480 0.0244 0.095 Uiso 1 1 calc R . . C86 C 0.43416(13) 0.4770(2) 0.00630(8) 0.0508(10) Uani 1 1 d . . . H86A H 0.4447 0.4942 -0.0088 0.061 Uiso 1 1 calc R . . H86B H 0.4532 0.4395 0.0170 0.061 Uiso 1 1 calc R . . C87 C 0.39420(15) 0.4377(3) -0.00866(9) 0.0659(13) Uani 1 1 d . . . C88 C 0.36994(17) 0.4192(4) 0.01053(11) 0.0857(18) Uani 1 1 d . . . H88A H 0.3458 0.3921 -0.0001 0.129 Uiso 1 1 calc R . . H88B H 0.3619 0.4638 0.0179 0.129 Uiso 1 1 calc R . . H88C H 0.3863 0.3895 0.0263 0.129 Uiso 1 1 calc R . . C89 C 0.4057(3) 0.3664(4) -0.01992(18) 0.138(3) Uani 1 1 d . . . H89A H 0.3812 0.3399 -0.0302 0.207 Uiso 1 1 calc R . . H89B H 0.4220 0.3369 -0.0041 0.207 Uiso 1 1 calc R . . H89C H 0.4214 0.3769 -0.0327 0.207 Uiso 1 1 calc R . . C90 C 0.3677(2) 0.4809(4) -0.03395(12) 0.123(3) Uani 1 1 d . . . H90A H 0.3830 0.4914 -0.0469 0.185 Uiso 1 1 calc R . . H90B H 0.3595 0.5265 -0.0273 0.185 Uiso 1 1 calc R . . H90C H 0.3437 0.4525 -0.0438 0.185 Uiso 1 1 calc R . . C91 C 0.37187(10) 0.4110(2) 0.12347(8) 0.0386(8) Uani 1 1 d . . . H91A H 0.3774 0.3612 0.1310 0.046 Uiso 1 1 calc R . . H91B H 0.3581 0.4077 0.1029 0.046 Uiso 1 1 calc R . . C92 C 0.34441(11) 0.4483(2) 0.13708(8) 0.0411(9) Uani 1 1 d . . . C93 C 0.27673(13) 0.4549(3) 0.13678(12) 0.0676(14) Uani 1 1 d . . . H93A H 0.2774 0.5084 0.1356 0.081 Uiso 1 1 calc R . . H93B H 0.2822 0.4410 0.1568 0.081 Uiso 1 1 calc R . . C94 C 0.23686(13) 0.4275(4) 0.11956(12) 0.0883(19) Uani 1 1 d . . . H94A H 0.2311 0.4438 0.1000 0.132 Uiso 1 1 calc R . . H94B H 0.2161 0.4460 0.1271 0.132 Uiso 1 1 calc R . . H94C H 0.2369 0.3744 0.1201 0.132 Uiso 1 1 calc R . . C95 C 0.37552(10) 0.5873(2) 0.10433(7) 0.0348(8) Uani 1 1 d . . . H95A H 0.3852 0.6375 0.1037 0.042 Uiso 1 1 calc R . . H95B H 0.3817 0.5739 0.1245 0.042 Uiso 1 1 calc R . . C96 C 0.30650(10) 0.63672(18) 0.09969(7) 0.0312(7) Uani 1 1 d . . . C97 C 0.32982(10) 0.58670(19) 0.09066(7) 0.0326(8) Uani 1 1 d . . . C98 C 0.31011(10) 0.5391(2) 0.06918(7) 0.0366(8) Uani 1 1 d . . . H98 H 0.3257 0.5055 0.0626 0.044 Uiso 1 1 calc R . . C99 C 0.26832(11) 0.5387(2) 0.05692(8) 0.0400(9) Uani 1 1 d . . . C100 C 0.24653(10) 0.5888(2) 0.06678(7) 0.0389(8) Uani 1 1 d . . . H100 H 0.2180 0.5888 0.0589 0.047 Uiso 1 1 calc R . . C101 C 0.26472(10) 0.63948(19) 0.08780(7) 0.0332(8) Uani 1 1 d . . . C102 C 0.24782(12) 0.4862(3) 0.03279(9) 0.0556(11) Uani 1 1 d . . . C103 C 0.26773(18) 0.4104(3) 0.04036(16) 0.114(3) Uani 1 1 d . . . H10C H 0.2524 0.3747 0.0266 0.172 Uiso 1 1 calc R . . H10D H 0.2677 0.3965 0.0593 0.172 Uiso 1 1 calc R . . H10E H 0.2955 0.4123 0.0400 0.172 Uiso 1 1 calc R . . C104 C 0.20432(16) 0.4718(4) 0.03088(13) 0.095(2) Uani 1 1 d . . . H10F H 0.1886 0.5164 0.0255 0.143 Uiso 1 1 calc R . . H10G H 0.2032 0.4551 0.0492 0.143 Uiso 1 1 calc R . . H10H H 0.1930 0.4344 0.0166 0.143 Uiso 1 1 calc R . . C105 C 0.25547(19) 0.5056(4) 0.00550(13) 0.103(2) Uani 1 1 d . . . H10I H 0.2410 0.4692 -0.0086 0.123 Uiso 1 1 calc R . . H10J H 0.2846 0.4978 0.0087 0.123 Uiso 1 1 calc R . . C106 C 0.2446(2) 0.5835(4) -0.00940(11) 0.0891(18) Uani 1 1 d . . . C107 C 0.2762(2) 0.6374(4) 0.00684(14) 0.108(2) Uani 1 1 d . . . H10K H 0.2759 0.6797 -0.0051 0.163 Uiso 1 1 calc R . . H10L H 0.3029 0.6146 0.0122 0.163 Uiso 1 1 calc R . . H10M H 0.2702 0.6526 0.0239 0.163 Uiso 1 1 calc R . . C108 C 0.2500(3) 0.5702(6) -0.03815(14) 0.155(4) Uani 1 1 d . . . H10N H 0.2309 0.5331 -0.0484 0.232 Uiso 1 1 calc R . . H10O H 0.2776 0.5537 -0.0355 0.232 Uiso 1 1 calc R . . H10P H 0.2451 0.6153 -0.0491 0.232 Uiso 1 1 calc R . . C109 C 0.2045(2) 0.6122(6) -0.0130(2) 0.170(4) Uani 1 1 d . . . H10Q H 0.1995 0.6539 -0.0258 0.255 Uiso 1 1 calc R . . H10R H 0.2027 0.6273 0.0053 0.255 Uiso 1 1 calc R . . H10S H 0.1843 0.5746 -0.0211 0.255 Uiso 1 1 calc R . . C110 C 0.33319(12) 0.6669(2) 0.14819(7) 0.0417(9) Uani 1 1 d . . . H11A H 0.3602 0.6442 0.1554 0.050 Uiso 1 1 calc R . . H11B H 0.3128 0.6309 0.1493 0.050 Uiso 1 1 calc R . . C111 C 0.33131(11) 0.7323(2) 0.16583(8) 0.0381(8) Uani 1 1 d . . . C112 C 0.35287(16) 0.7791(3) 0.21229(9) 0.0653(13) Uani 1 1 d . . . H11C H 0.3646 0.8236 0.2071 0.078 Uiso 1 1 calc R . . H11D H 0.3249 0.7897 0.2119 0.078 Uiso 1 1 calc R . . C113 C 0.3769(3) 0.7549(4) 0.24028(11) 0.118(3) Uani 1 1 d . . . H11E H 0.3643 0.7123 0.2456 0.177 Uiso 1 1 calc R . . H11F H 0.3787 0.7938 0.2540 0.177 Uiso 1 1 calc R . . H11G H 0.4041 0.7423 0.2402 0.177 Uiso 1 1 calc R . . C114 C 0.23994(10) 0.69803(19) 0.09596(8) 0.0345(8) Uani 1 1 d . . . H11H H 0.2553 0.7171 0.1148 0.041 Uiso 1 1 calc R . . H11I H 0.2357 0.7384 0.0823 0.041 Uiso 1 1 calc R . . C115 C 0.19633(9) 0.63307(17) 0.12021(7) 0.0279(7) Uani 1 1 d . . . C116 C 0.19930(9) 0.67114(18) 0.09661(7) 0.0301(7) Uani 1 1 d . . . C117 C 0.16463(10) 0.67998(19) 0.07404(7) 0.0330(8) Uani 1 1 d . . . H117 H 0.1662 0.7067 0.0582 0.040 Uiso 1 1 calc R . . C118 C 0.12732(10) 0.65141(18) 0.07338(7) 0.0316(7) Uani 1 1 d . . . C119 C 0.12628(10) 0.61238(18) 0.09698(7) 0.0314(7) Uani 1 1 d . . . H119 H 0.1014 0.5915 0.0970 0.038 Uiso 1 1 calc R . . C120 C 0.16010(10) 0.60268(17) 0.12057(7) 0.0304(7) Uani 1 1 d . . . C121 C 0.08997(10) 0.6612(2) 0.04697(7) 0.0382(8) Uani 1 1 d . . . C122 C 0.10207(14) 0.6422(3) 0.02077(9) 0.0681(14) Uani 1 1 d . . . H12D H 0.1145 0.5941 0.0232 0.102 Uiso 1 1 calc R . . H12E H 0.1213 0.6781 0.0184 0.102 Uiso 1 1 calc R . . H12F H 0.0780 0.6421 0.0040 0.102 Uiso 1 1 calc R . . C123 C 0.05560(13) 0.6112(3) 0.04767(10) 0.0594(12) Uani 1 1 d . . . H12G H 0.0321 0.6200 0.0310 0.089 Uiso 1 1 calc R . . H12H H 0.0484 0.6207 0.0648 0.089 Uiso 1 1 calc R . . H12I H 0.0642 0.5607 0.0477 0.089 Uiso 1 1 calc R . . C124 C 0.07688(12) 0.7428(2) 0.04304(8) 0.0451(9) Uani 1 1 d . . . H12J H 0.1017 0.7712 0.0453 0.054 Uiso 1 1 calc R . . H12K H 0.0599 0.7484 0.0231 0.054 Uiso 1 1 calc R . . C125 C 0.05441(12) 0.7809(2) 0.06101(8) 0.0468(9) Uani 1 1 d . . . C126 C 0.05612(16) 0.8631(3) 0.05543(11) 0.0686(13) Uani 1 1 d . . . H12L H 0.0418 0.8896 0.0663 0.103 Uiso 1 1 calc R . . H12M H 0.0433 0.8729 0.0353 0.103 Uiso 1 1 calc R . . H12N H 0.0843 0.8790 0.0612 0.103 Uiso 1 1 calc R . . C127 C 0.00907(14) 0.7628(3) 0.05073(12) 0.0778(15) Uani 1 1 d . . . H12O H 0.0051 0.7125 0.0556 0.117 Uiso 1 1 calc R . . H12P H -0.0016 0.7689 0.0302 0.117 Uiso 1 1 calc R . . H12Q H -0.0052 0.7953 0.0598 0.117 Uiso 1 1 calc R . . C128 C 0.07244(16) 0.7686(3) 0.09244(9) 0.0674(13) Uani 1 1 d . . . H12R H 0.0674 0.7185 0.0969 0.101 Uiso 1 1 calc R . . H12S H 0.0600 0.8018 0.1025 0.101 Uiso 1 1 calc R . . H12T H 0.1016 0.7774 0.0982 0.101 Uiso 1 1 calc R . . C129 C 0.23302(11) 0.67654(19) 0.16525(7) 0.0353(8) Uani 1 1 d . . . H12U H 0.2059 0.6822 0.1673 0.042 Uiso 1 1 calc R . . H12V H 0.2413 0.7241 0.1598 0.042 Uiso 1 1 calc R . . C130 C 0.26219(12) 0.6538(2) 0.19296(8) 0.0459(9) Uani 1 1 d . . . C131 C 0.3047(3) 0.5635(4) 0.21965(12) 0.125(3) Uani 1 1 d . . . H13D H 0.3296 0.5927 0.2238 0.150 Uiso 1 1 calc R . . H13E H 0.2931 0.5716 0.2351 0.150 Uiso 1 1 calc R . . C132 C 0.3136(2) 0.4946(4) 0.21885(15) 0.128(3) Uani 1 1 d . . . H13F H 0.2894 0.4653 0.2164 0.191 Uiso 1 1 calc R . . H13G H 0.3343 0.4811 0.2366 0.191 Uiso 1 1 calc R . . H13H H 0.3239 0.4860 0.2030 0.191 Uiso 1 1 calc R . . C133 C 0.15824(11) 0.56075(18) 0.14620(7) 0.0359(8) Uani 1 1 d . . . H13I H 0.1407 0.5879 0.1549 0.043 Uiso 1 1 calc R . . H13J H 0.1857 0.5599 0.1601 0.043 Uiso 1 1 calc R . . C134 C 0.13824(9) 0.44515(17) 0.16449(6) 0.0262(7) Uani 1 1 d . . . C135 C 0.14303(9) 0.48341(17) 0.14150(6) 0.0270(7) Uani 1 1 d . . . C136 C 0.13321(9) 0.44794(18) 0.11560(7) 0.0295(7) Uani 1 1 d . . . H136 H 0.1366 0.4729 0.0999 0.035 Uiso 1 1 calc R . . C137 C 0.11858(9) 0.37736(18) 0.11187(7) 0.0304(7) Uani 1 1 d . . . C138 C 0.11414(10) 0.34206(18) 0.13521(7) 0.0329(8) Uani 1 1 d . . . H138 H 0.1041 0.2939 0.1331 0.039 Uiso 1 1 calc R . . C139 C 0.12390(9) 0.37477(18) 0.16163(7) 0.0285(7) Uani 1 1 d . . . C140 C 0.10848(11) 0.3380(2) 0.08316(7) 0.0369(8) Uani 1 1 d . . . C141 C 0.11636(14) 0.3856(3) 0.06037(8) 0.0562(11) Uani 1 1 d . . . H14D H 0.1452 0.3964 0.0656 0.084 Uiso 1 1 calc R . . H14E H 0.1012 0.4310 0.0587 0.084 Uiso 1 1 calc R . . H14F H 0.1077 0.3601 0.0422 0.084 Uiso 1 1 calc R . . C142 C 0.13707(14) 0.2733(3) 0.08776(10) 0.0619(12) Uani 1 1 d . . . H14G H 0.1344 0.2503 0.0696 0.093 Uiso 1 1 calc R . . H14H H 0.1303 0.2382 0.1003 0.093 Uiso 1 1 calc R . . H14I H 0.1649 0.2898 0.0964 0.093 Uiso 1 1 calc R . . C143 C 0.06497(12) 0.3064(2) 0.07352(9) 0.0521(10) Uani 1 1 d . . . H14J H 0.0633 0.2731 0.0577 0.063 Uiso 1 1 calc R . . H14K H 0.0627 0.2760 0.0893 0.063 Uiso 1 1 calc R . . C144 C 0.02664(12) 0.3537(3) 0.06408(9) 0.0554(11) Uani 1 1 d . . . C145 C 0.02651(14) 0.4138(3) 0.08493(11) 0.0755(15) Uani 1 1 d . . . H14L H 0.0486 0.4476 0.0862 0.113 Uiso 1 1 calc R . . H14M H 0.0301 0.3928 0.1036 0.113 Uiso 1 1 calc R . . H14N H 0.0008 0.4398 0.0785 0.113 Uiso 1 1 calc R . . C146 C 0.01815(16) 0.3865(4) 0.03472(11) 0.0838(17) Uani 1 1 d . . . H14O H 0.0396 0.4208 0.0349 0.126 Uiso 1 1 calc R . . H14P H -0.0078 0.4117 0.0293 0.126 Uiso 1 1 calc R . . H14Q H 0.0173 0.3478 0.0211 0.126 Uiso 1 1 calc R . . C147 C -0.00866(16) 0.3017(4) 0.06217(13) 0.0918(18) Uani 1 1 d . . . H14R H -0.0341 0.3286 0.0558 0.138 Uiso 1 1 calc R . . H14S H -0.0052 0.2806 0.0808 0.138 Uiso 1 1 calc R . . H14T H -0.0091 0.2630 0.0487 0.138 Uiso 1 1 calc R . . C148 C 0.18841(10) 0.48237(19) 0.20720(7) 0.0344(8) Uani 1 1 d . . . H14U H 0.1971 0.5332 0.2116 0.041 Uiso 1 1 calc R . . H14V H 0.2049 0.4610 0.1963 0.041 Uiso 1 1 calc R . . C149 C 0.19536(12) 0.4406(2) 0.23440(7) 0.0416(9) Uani 1 1 d . . . C150 C 0.24558(18) 0.3833(5) 0.27142(11) 0.111(3) Uani 1 1 d . . . H15C H 0.2399 0.4069 0.2876 0.133 Uiso 1 1 calc R . . H15D H 0.2294 0.3384 0.2667 0.133 Uiso 1 1 calc R . . C151 C 0.2864(2) 0.3666(5) 0.27868(13) 0.127(3) Uani 1 1 d . . . H15E H 0.2921 0.3457 0.2623 0.191 Uiso 1 1 calc R . . H15F H 0.2935 0.3316 0.2942 0.191 Uiso 1 1 calc R . . H15G H 0.3024 0.4108 0.2846 0.191 Uiso 1 1 calc R . . C152 C 0.11706(11) 0.33535(18) 0.18638(7) 0.0346(8) Uani 1 1 d . . . H15H H 0.1297 0.3638 0.2037 0.042 Uiso 1 1 calc R . . H15I H 0.0877 0.3338 0.1834 0.042 Uiso 1 1 calc R . . O25 O 0.5855(2) 0.0004(4) 0.22444(16) 0.076(2) Uiso 0.50 1 d P A 1 C153 C 0.5653(4) -0.0650(7) 0.2359(3) 0.094(4) Uiso 0.50 1 d P A 1 C154 C 0.5348(3) -0.0476(6) 0.2443(2) 0.071(3) Uiso 0.50 1 d P A 1 O26 O 0.5371(2) 0.0948(4) 0.13597(16) 0.0779(19) Uiso 0.50 1 d P B 1 C155 C 0.5429(4) 0.0435(8) 0.1551(3) 0.106(4) Uiso 0.50 1 d P B 1 C156 C 0.5588(5) 0.0894(10) 0.1768(4) 0.128(5) Uiso 0.50 1 d P B 1 O1W O 0.5899(3) 0.0442(7) 0.2172(2) 0.130(4) Uiso 0.50 1 d P C 2 O2W O 0.5465(6) 0.0266(11) 0.1822(4) 0.224(7) Uiso 0.50 1 d P D 3 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 0.0399(13) 0.0353(13) 0.0341(13) -0.0091(10) 0.0242(11) -0.0116(10) O2 0.0467(16) 0.086(2) 0.0525(19) -0.0177(16) 0.0231(15) -0.0221(15) O3 0.0437(15) 0.0638(18) 0.0470(16) 0.0031(13) 0.0294(13) 0.0024(13) O4 0.0336(12) 0.0405(13) 0.0215(11) -0.0014(10) 0.0080(9) -0.0068(10) O5 0.114(3) 0.0540(18) 0.0363(16) -0.0031(13) 0.0363(17) -0.0142(18) O6 0.091(2) 0.078(2) 0.0402(17) -0.0113(15) 0.0015(16) -0.0378(19) O7 0.0386(13) 0.0405(14) 0.0342(13) -0.0055(11) 0.0044(11) -0.0027(11) O8 0.0547(19) 0.120(3) 0.051(2) -0.0339(19) -0.0005(16) -0.0020(19) O9 0.0626(18) 0.0553(18) 0.0465(16) -0.0193(14) 0.0192(14) -0.0176(15) O10 0.0291(12) 0.0364(13) 0.0303(12) -0.0017(10) 0.0089(10) -0.0040(10) O11 0.0622(19) 0.0544(18) 0.103(3) -0.0307(17) 0.0478(19) -0.0264(16) O12 0.070(2) 0.063(2) 0.098(3) -0.0323(18) 0.051(2) -0.0177(16) O13 0.0296(12) 0.0549(15) 0.0285(12) 0.0050(11) 0.0150(10) -0.0034(11) O14 0.0605(18) 0.075(2) 0.0593(19) -0.0174(16) 0.0396(16) -0.0101(16) O15 0.0335(14) 0.0602(18) 0.0642(18) 0.0054(14) 0.0260(13) -0.0005(12) O16 0.0350(13) 0.0405(14) 0.0316(13) -0.0038(10) 0.0143(10) -0.0033(11) O17 0.0593(18) 0.0476(17) 0.0612(19) -0.0065(14) 0.0242(15) 0.0054(15) O18 0.076(2) 0.0494(17) 0.0365(15) -0.0113(12) 0.0167(14) 0.0047(15) O19 0.0333(12) 0.0366(13) 0.0268(12) -0.0010(10) 0.0055(10) 0.0058(10) O20 0.075(2) 0.086(2) 0.0403(17) -0.0215(16) 0.0085(15) -0.0110(18) O21 0.098(3) 0.069(2) 0.0313(16) 0.0005(14) -0.0126(16) 0.0250(19) O22 0.0334(12) 0.0316(12) 0.0246(11) -0.0026(9) 0.0106(10) 0.0031(10) O23 0.0619(18) 0.0626(18) 0.0306(14) 0.0033(12) 0.0206(13) 0.0031(14) O24 0.0505(18) 0.113(3) 0.0330(15) 0.0199(16) 0.0082(13) 0.0210(17) C1 0.0332(17) 0.0302(18) 0.0239(16) -0.0048(13) 0.0161(14) -0.0088(14) C2 0.0364(18) 0.0316(18) 0.0229(16) -0.0006(13) 0.0148(14) -0.0039(14) C3 0.0294(17) 0.0349(19) 0.0282(17) 0.0021(14) 0.0101(14) -0.0006(14) C4 0.0320(18) 0.0344(19) 0.0266(17) -0.0003(14) 0.0101(14) -0.0063(14) C5 0.0370(18) 0.0316(18) 0.0250(17) 0.0013(14) 0.0122(14) -0.0011(15) C6 0.0320(17) 0.0375(19) 0.0203(16) -0.0069(13) 0.0136(13) -0.0064(15) C7 0.0353(19) 0.037(2) 0.045(2) 0.0038(16) 0.0144(16) -0.0095(16) C8 0.061(3) 0.065(3) 0.061(3) 0.009(2) 0.032(2) -0.019(2) C9 0.051(2) 0.036(2) 0.071(3) 0.007(2) 0.007(2) -0.0085(18) C10 0.035(2) 0.041(2) 0.060(3) 0.0017(18) 0.0098(18) -0.0104(17) C11 0.060(3) 0.054(3) 0.049(2) -0.006(2) 0.003(2) -0.021(2) C12 0.121(5) 0.083(4) 0.043(3) -0.015(2) 0.032(3) -0.049(3) C13 0.111(5) 0.097(4) 0.062(3) -0.011(3) -0.026(3) 0.015(4) C14 0.072(3) 0.068(3) 0.080(4) -0.024(3) 0.019(3) -0.022(3) C15 0.042(2) 0.041(2) 0.0354(19) -0.0022(15) 0.0241(16) -0.0066(16) C16 0.044(2) 0.037(2) 0.045(2) -0.0031(17) 0.0254(19) -0.0102(17) C17 0.047(2) 0.077(3) 0.058(3) 0.012(2) 0.031(2) 0.005(2) C18 0.064(3) 0.066(3) 0.093(4) 0.000(3) 0.053(3) 0.003(2) C19 0.0310(17) 0.040(2) 0.0251(17) -0.0041(14) 0.0110(14) -0.0019(15) C20 0.0278(17) 0.0349(18) 0.0215(16) -0.0013(13) 0.0073(13) -0.0069(14) C21 0.0314(17) 0.0311(18) 0.0267(17) -0.0022(13) 0.0131(14) -0.0074(14) C22 0.0281(16) 0.0315(18) 0.0263(17) -0.0019(13) 0.0069(14) -0.0018(14) C23 0.0340(18) 0.0329(18) 0.0240(17) -0.0031(14) 0.0084(14) -0.0043(14) C24 0.0344(18) 0.0362(19) 0.0282(17) -0.0042(14) 0.0125(15) -0.0004(15) C25 0.0294(17) 0.0314(18) 0.0302(17) 0.0001(14) 0.0121(14) -0.0045(14) C26 0.041(2) 0.046(2) 0.0241(17) -0.0046(15) 0.0048(15) 0.0063(17) C27 0.270(10) 0.143(6) 0.026(3) -0.004(3) -0.016(4) 0.147(7) C28 0.058(4) 0.66(3) 0.025(3) -0.022(7) 0.015(3) 0.008(8) C29 0.51(2) 0.123(7) 0.089(5) 0.062(5) -0.166(9) -0.194(10) C30 0.061(3) 0.043(2) 0.048(2) -0.0081(19) 0.010(2) 0.002(2) C31 0.098(7) 0.47(3) 0.178(11) -0.082(13) 0.049(7) 0.034(10) C32 0.131(6) 0.136(7) 0.147(7) -0.091(6) 0.035(5) -0.002(5) C33 0.122(5) 0.066(4) 0.089(4) 0.028(3) 0.002(4) -0.024(3) C34 0.0367(19) 0.051(2) 0.0297(18) -0.0074(16) 0.0107(15) -0.0117(17) C35 0.058(2) 0.040(2) 0.0286(19) -0.0010(16) 0.0059(18) -0.0040(19) C36 0.128(5) 0.112(5) 0.045(3) -0.016(3) 0.002(3) -0.029(4) C37 0.213(9) 0.128(6) 0.062(4) -0.025(4) 0.018(5) -0.077(6) C38 0.0306(17) 0.040(2) 0.0307(18) 0.0026(15) 0.0117(14) -0.0001(15) C39 0.0295(17) 0.0305(18) 0.0316(18) 0.0011(14) 0.0040(14) 0.0026(14) C40 0.0275(17) 0.0362(19) 0.0311(18) 0.0048(14) 0.0087(14) 0.0028(14) C41 0.0336(18) 0.0294(18) 0.041(2) 0.0026(15) 0.0165(15) -0.0033(14) C42 0.043(2) 0.035(2) 0.043(2) 0.0012(16) 0.0215(17) 0.0000(16) C43 0.043(2) 0.039(2) 0.044(2) 0.0029(16) 0.0261(17) -0.0023(16) C44 0.0334(18) 0.0352(19) 0.0367(19) 0.0071(15) 0.0107(15) -0.0016(15) C45 0.064(3) 0.037(2) 0.054(2) -0.0056(18) 0.035(2) -0.0024(19) C46 0.078(3) 0.061(3) 0.047(3) -0.011(2) 0.012(2) -0.002(2) C47 0.129(5) 0.051(3) 0.078(3) -0.010(2) 0.075(4) -0.007(3) C48 0.054(2) 0.037(2) 0.069(3) -0.0059(19) 0.032(2) -0.0019(18) C49 0.053(3) 0.057(3) 0.105(4) 0.008(3) 0.032(3) 0.005(2) C50 0.109(6) 0.094(5) 0.175(8) -0.020(5) -0.063(5) 0.026(4) C51 0.088(4) 0.068(4) 0.142(6) 0.027(4) 0.025(4) 0.021(3) C52 0.110(6) 0.243(12) 0.274(13) 0.117(10) 0.134(8) 0.084(7) C53 0.038(2) 0.057(2) 0.033(2) 0.0015(17) 0.0048(16) -0.0067(18) C54 0.040(2) 0.073(3) 0.040(2) -0.015(2) 0.0162(19) -0.014(2) C55 0.075(3) 0.073(3) 0.065(3) -0.037(3) 0.028(3) -0.026(3) C56 0.082(4) 0.066(3) 0.093(4) -0.036(3) 0.038(3) -0.015(3) C57 0.043(2) 0.040(2) 0.039(2) 0.0049(16) 0.0100(17) -0.0092(17) C58 0.0247(16) 0.0329(18) 0.0297(17) -0.0045(14) 0.0100(14) -0.0012(14) C59 0.0321(17) 0.0328(18) 0.0308(18) -0.0007(14) 0.0141(14) -0.0018(14) C60 0.0377(19) 0.0354(19) 0.0346(19) -0.0056(15) 0.0174(16) -0.0076(15) C61 0.0326(18) 0.0367(19) 0.0324(18) -0.0064(15) 0.0140(15) -0.0033(15) C62 0.0348(18) 0.039(2) 0.0265(17) -0.0020(14) 0.0128(15) -0.0005(15) C63 0.0296(17) 0.0312(18) 0.0303(17) 0.0004(14) 0.0142(14) 0.0005(14) C64 0.038(2) 0.048(2) 0.0344(19) -0.0060(16) 0.0099(16) -0.0080(17) C65 0.041(2) 0.092(4) 0.054(3) -0.016(2) 0.012(2) -0.012(2) C66 0.065(3) 0.067(3) 0.045(3) -0.002(2) -0.006(2) -0.001(2) C67 0.044(2) 0.061(3) 0.045(2) -0.018(2) 0.0081(18) -0.012(2) C68 0.051(2) 0.072(3) 0.043(2) -0.021(2) 0.0185(19) -0.006(2) C69 0.048(2) 0.063(3) 0.056(3) -0.007(2) 0.021(2) 0.000(2) C70 0.085(4) 0.107(5) 0.107(5) -0.065(4) 0.024(3) -0.002(3) C71 0.076(4) 0.148(6) 0.049(3) 0.007(3) 0.031(3) -0.002(4) C72 0.041(2) 0.046(2) 0.0284(18) -0.0030(15) 0.0125(15) -0.0086(17) C73 0.041(2) 0.052(2) 0.053(2) -0.0164(19) 0.0191(19) -0.0118(19) C74 0.103(4) 0.078(4) 0.119(5) -0.035(4) 0.063(4) -0.020(3) C75 0.174(8) 0.088(5) 0.129(6) -0.020(4) 0.064(6) 0.012(5) C76 0.0272(17) 0.0359(19) 0.0314(18) 0.0027(14) 0.0114(14) -0.0027(14) C77 0.0246(16) 0.042(2) 0.0202(16) -0.0012(14) 0.0084(13) -0.0058(14) C78 0.0275(16) 0.0308(18) 0.0277(17) -0.0018(14) 0.0098(14) -0.0059(14) C79 0.0319(17) 0.0366(19) 0.0283(17) -0.0028(14) 0.0155(14) -0.0014(15) C80 0.0335(18) 0.040(2) 0.0238(17) 0.0006(14) 0.0126(14) -0.0026(15) C81 0.0308(17) 0.0369(19) 0.0296(18) 0.0010(14) 0.0101(14) 0.0011(15) C82 0.0229(16) 0.044(2) 0.0268(17) -0.0031(15) 0.0091(13) -0.0033(14) C83 0.049(2) 0.048(2) 0.0317(19) 0.0063(16) 0.0232(17) 0.0037(18) C84 0.061(3) 0.078(3) 0.048(2) 0.009(2) 0.030(2) -0.012(2) C85 0.091(3) 0.067(3) 0.045(2) 0.023(2) 0.039(2) 0.023(3) C86 0.062(3) 0.066(3) 0.031(2) -0.0005(18) 0.0243(19) 0.004(2) C87 0.076(3) 0.083(3) 0.035(2) -0.008(2) 0.013(2) -0.007(3) C88 0.081(4) 0.113(5) 0.054(3) -0.008(3) 0.007(3) -0.042(3) C89 0.146(7) 0.129(6) 0.133(6) -0.085(5) 0.035(5) -0.018(5) C90 0.123(6) 0.156(7) 0.054(4) 0.023(4) -0.025(3) -0.033(5) C91 0.0340(19) 0.046(2) 0.042(2) 0.0039(17) 0.0206(16) -0.0032(16) C92 0.038(2) 0.048(2) 0.045(2) 0.0090(19) 0.0239(18) -0.0005(17) C93 0.049(3) 0.063(3) 0.108(4) 0.012(3) 0.050(3) 0.010(2) C94 0.036(2) 0.144(6) 0.089(4) 0.036(4) 0.027(3) 0.011(3) C95 0.0308(18) 0.043(2) 0.0317(18) -0.0050(15) 0.0108(15) 0.0007(15) C96 0.0324(18) 0.0357(19) 0.0278(17) -0.0005(14) 0.0126(14) -0.0014(15) C97 0.0311(17) 0.041(2) 0.0285(17) 0.0023(15) 0.0130(14) 0.0012(15) C98 0.0338(19) 0.046(2) 0.0317(19) -0.0074(16) 0.0129(15) 0.0027(16) C99 0.0336(19) 0.051(2) 0.035(2) -0.0081(17) 0.0109(16) -0.0027(17) C100 0.0288(18) 0.051(2) 0.0360(19) -0.0037(17) 0.0097(15) 0.0006(16) C101 0.0319(18) 0.040(2) 0.0308(18) 0.0033(15) 0.0144(15) 0.0011(15) C102 0.038(2) 0.074(3) 0.051(2) -0.028(2) 0.0099(19) -0.005(2) C103 0.071(4) 0.094(5) 0.151(6) -0.074(5) -0.002(4) 0.008(3) C104 0.063(3) 0.131(5) 0.094(4) -0.066(4) 0.028(3) -0.036(3) C105 0.076(4) 0.159(7) 0.070(4) -0.050(4) 0.019(3) -0.013(4) C106 0.098(4) 0.121(5) 0.048(3) -0.002(3) 0.022(3) 0.006(4) C107 0.132(6) 0.118(6) 0.085(4) 0.017(4) 0.047(4) -0.010(5) C108 0.160(8) 0.255(12) 0.054(4) -0.002(5) 0.041(4) 0.022(8) C109 0.095(6) 0.232(12) 0.171(9) -0.038(8) 0.028(6) 0.023(7) C110 0.048(2) 0.043(2) 0.0323(19) -0.0047(16) 0.0097(17) 0.0050(17) C111 0.0352(19) 0.045(2) 0.039(2) -0.0049(17) 0.0179(16) -0.0054(17) C112 0.096(4) 0.056(3) 0.049(3) -0.025(2) 0.031(3) -0.009(3) C113 0.214(8) 0.089(4) 0.041(3) -0.016(3) 0.025(4) 0.008(5) C114 0.0323(18) 0.037(2) 0.0377(19) 0.0034(15) 0.0165(15) 0.0014(15) C115 0.0287(17) 0.0285(17) 0.0257(16) -0.0015(13) 0.0074(14) 0.0053(14) C116 0.0295(17) 0.0308(18) 0.0321(18) 0.0016(14) 0.0129(14) 0.0059(14) C117 0.0346(18) 0.0378(19) 0.0288(18) 0.0070(14) 0.0131(15) 0.0092(15) C118 0.0298(17) 0.0360(19) 0.0284(17) 0.0010(14) 0.0082(14) 0.0066(14) C119 0.0275(17) 0.0348(19) 0.0325(18) -0.0009(14) 0.0103(14) -0.0018(14) C120 0.0363(18) 0.0263(17) 0.0305(18) -0.0016(14) 0.0134(15) 0.0004(14) C121 0.0337(18) 0.049(2) 0.0289(18) 0.0011(16) 0.0056(15) 0.0069(16) C122 0.060(3) 0.104(4) 0.034(2) -0.015(2) 0.007(2) 0.014(3) C123 0.047(2) 0.061(3) 0.057(3) 0.004(2) -0.002(2) -0.002(2) C124 0.044(2) 0.057(2) 0.033(2) 0.0074(17) 0.0115(17) 0.0080(19) C125 0.046(2) 0.051(2) 0.049(2) 0.0015(19) 0.0222(19) 0.0037(18) C126 0.079(3) 0.061(3) 0.069(3) 0.012(2) 0.028(3) 0.015(3) C127 0.055(3) 0.090(4) 0.097(4) 0.003(3) 0.036(3) 0.015(3) C128 0.097(4) 0.066(3) 0.043(2) 0.003(2) 0.028(2) 0.020(3) C129 0.0396(19) 0.0359(19) 0.0322(18) -0.0059(15) 0.0143(15) -0.0040(16) C130 0.051(2) 0.053(3) 0.033(2) -0.0057(18) 0.0125(18) -0.007(2) C131 0.175(7) 0.099(5) 0.047(3) 0.003(3) -0.041(4) 0.049(5) C132 0.135(6) 0.101(5) 0.098(5) 0.031(4) -0.032(4) 0.027(5) C133 0.048(2) 0.0328(19) 0.0267(17) 0.0024(14) 0.0108(15) -0.0055(16) C134 0.0232(15) 0.0312(18) 0.0243(16) -0.0019(13) 0.0077(13) 0.0028(13) C135 0.0226(15) 0.0306(17) 0.0271(17) 0.0003(13) 0.0069(13) 0.0006(13) C136 0.0258(16) 0.0371(19) 0.0260(17) 0.0032(14) 0.0086(13) 0.0023(14) C137 0.0261(16) 0.0342(19) 0.0284(17) -0.0005(14) 0.0052(14) 0.0029(14) C138 0.0337(18) 0.0301(18) 0.0344(19) -0.0030(14) 0.0102(15) -0.0036(14) C139 0.0283(16) 0.0322(18) 0.0254(16) 0.0005(13) 0.0093(13) 0.0005(14) C140 0.0393(19) 0.042(2) 0.0271(18) -0.0085(15) 0.0075(15) 0.0009(16) C141 0.068(3) 0.071(3) 0.032(2) -0.014(2) 0.020(2) -0.014(2) C142 0.070(3) 0.062(3) 0.052(3) -0.018(2) 0.017(2) 0.017(2) C143 0.057(3) 0.055(3) 0.038(2) -0.0103(18) 0.0065(19) -0.008(2) C144 0.039(2) 0.072(3) 0.047(2) -0.004(2) 0.0017(18) 0.001(2) C145 0.048(3) 0.102(4) 0.071(3) -0.008(3) 0.010(2) 0.019(3) C146 0.065(3) 0.115(5) 0.055(3) 0.015(3) -0.004(2) 0.004(3) C147 0.062(3) 0.108(5) 0.093(4) 0.004(4) 0.007(3) -0.019(3) C148 0.0359(19) 0.0362(19) 0.0288(18) -0.0034(15) 0.0072(15) -0.0015(15) C149 0.050(2) 0.048(2) 0.0272(18) -0.0042(16) 0.0129(18) 0.0086(18) C150 0.073(4) 0.205(8) 0.049(3) 0.062(4) 0.013(3) 0.041(4) C151 0.152(7) 0.162(7) 0.067(4) 0.042(4) 0.033(4) 0.088(6) C152 0.0405(19) 0.0331(19) 0.0351(19) 0.0000(15) 0.0187(16) -0.0026(15) _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 1.401(4) . ? O1 C15 1.438(4) . ? O2 C16 1.197(5) . ? O3 C16 1.337(4) . ? O3 C17 1.460(5) . ? O4 C20 1.405(4) . ? O4 C34 1.427(4) . ? O5 C35 1.198(5) . ? O6 C35 1.323(5) . ? O6 C36 1.498(6) . ? O7 C39 1.404(4) . ? O7 C53 1.434(4) . ? O8 C54 1.212(5) . ? O9 C54 1.326(5) . ? O9 C55 1.464(5) . ? O10 C58 1.398(4) . ? O10 C72 1.423(4) . ? O11 C73 1.194(5) . ? O12 C73 1.334(5) . ? O12 C74 1.521(7) . ? O13 C77 1.400(4) . ? O13 C91 1.421(4) . ? O14 C92 1.198(5) . ? O15 C92 1.336(5) . ? O15 C93 1.454(5) . ? O16 C96 1.393(4) . ? O16 C110 1.418(4) . ? O17 C111 1.197(5) . ? O18 C111 1.326(5) . ? O18 C112 1.456(5) . ? O19 C115 1.397(4) . ? O19 C129 1.432(4) . ? O20 C130 1.200(5) . ? O21 C130 1.307(5) . ? O21 C131 1.469(6) . ? O22 C134 1.400(4) . ? O22 C148 1.428(4) . ? O23 C149 1.202(5) . ? O24 C149 1.317(5) . ? O24 C150 1.479(6) . ? C1 C6 1.381(5) . ? C1 C2 1.405(5) . ? C2 C3 1.381(5) . ? C2 C152 1.510(5) . ? C3 C4 1.396(5) . ? C4 C5 1.381(5) . ? C4 C7 1.541(5) . ? C5 C6 1.409(5) . ? C6 C19 1.515(5) . ? C7 C9 1.531(5) . ? C7 C10 1.542(5) . ? C7 C8 1.545(5) . ? C10 C11 1.544(6) . ? C11 C13 1.524(7) . ? C11 C12 1.535(7) . ? C11 C14 1.537(7) . ? C15 C16 1.506(5) . ? C17 C18 1.497(6) . ? C19 C21 1.517(4) . ? C20 C21 1.389(5) . ? C20 C25 1.400(5) . ? C21 C22 1.398(4) . ? C22 C23 1.391(5) . ? C23 C24 1.392(5) . ? C23 C26 1.535(4) . ? C24 C25 1.390(5) . ? C25 C38 1.526(5) . ? C26 C29 1.401(8) . ? C26 C28 1.467(7) . ? C26 C27 1.478(6) . ? C29 C30 1.435(8) . ? C30 C31 1.463(10) . ? C30 C32 1.494(7) . ? C30 C33 1.498(7) . ? C34 C35 1.495(5) . ? C36 C37 1.342(9) . ? C38 C40 1.517(5) . ? C39 C44 1.392(5) . ? C39 C40 1.401(5) . ? C40 C41 1.385(5) . ? C41 C42 1.404(5) . ? C42 C43 1.386(5) . ? C42 C45 1.548(5) . ? C43 C44 1.396(5) . ? C44 C57 1.509(5) . ? C45 C47 1.540(6) . ? C45 C48 1.543(6) . ? C45 C46 1.545(6) . ? C48 C49 1.534(6) . ? C49 C50 1.513(9) . ? C49 C52 1.515(9) . ? C49 C51 1.534(7) . ? C53 C54 1.483(6) . ? C55 C56 1.455(7) . ? C57 C59 1.525(5) . ? C58 C59 1.395(5) . ? C58 C63 1.398(5) . ? C59 C60 1.394(5) . ? C60 C61 1.396(5) . ? C61 C62 1.388(5) . ? C61 C64 1.538(5) . ? C62 C63 1.396(5) . ? C63 C76 1.518(4) . ? C64 C66 1.539(6) . ? C64 C65 1.546(5) . ? C64 C67 1.547(6) . ? C67 C68 1.546(6) . ? C68 C69 1.529(6) . ? C68 C71 1.544(7) . ? C68 C70 1.545(7) . ? C72 C73 1.502(5) . ? C74 C75 1.370(9) . ? C76 C78 1.511(5) . ? C77 C82 1.392(5) . ? C77 C78 1.404(5) . ? C78 C79 1.390(4) . ? C79 C80 1.397(5) . ? C80 C81 1.386(5) . ? C80 C83 1.544(4) . ? C81 C82 1.397(5) . ? C82 C95 1.510(5) . ? C83 C85 1.528(6) . ? C83 C84 1.546(6) . ? C83 C86 1.548(5) . ? C86 C87 1.541(6) . ? C87 C88 1.507(7) . ? C87 C90 1.532(8) . ? C87 C89 1.535(8) . ? C91 C92 1.508(5) . ? C93 C94 1.476(7) . ? C95 C97 1.526(5) . ? C96 C101 1.392(5) . ? C96 C97 1.398(5) . ? C97 C98 1.389(5) . ? C98 C99 1.394(5) . ? C99 C100 1.385(5) . ? C99 C102 1.536(5) . ? C100 C101 1.399(5) . ? C101 C114 1.520(5) . ? C102 C105 1.513(8) . ? C102 C104 1.517(6) . ? C102 C103 1.555(8) . ? C105 C106 1.609(10) . ? C106 C109 1.455(10) . ? C106 C107 1.516(9) . ? C106 C108 1.527(8) . ? C110 C111 1.508(5) . ? C112 C113 1.454(7) . ? C114 C116 1.516(5) . ? C115 C120 1.391(5) . ? C115 C116 1.404(5) . ? C116 C117 1.378(5) . ? C117 C118 1.398(5) . ? C118 C119 1.392(5) . ? C118 C121 1.544(5) . ? C119 C120 1.390(5) . ? C120 C133 1.515(5) . ? C121 C123 1.525(6) . ? C121 C122 1.538(5) . ? C121 C124 1.569(5) . ? C124 C125 1.537(5) . ? C125 C128 1.511(6) . ? C125 C127 1.540(6) . ? C125 C126 1.550(6) . ? C129 C130 1.495(5) . ? C131 C132 1.314(9) . ? C133 C135 1.516(5) . ? C134 C139 1.384(5) . ? C134 C135 1.403(4) . ? C135 C136 1.392(4) . ? C136 C137 1.391(5) . ? C137 C138 1.387(5) . ? C137 C140 1.545(5) . ? C138 C139 1.391(5) . ? C139 C152 1.518(4) . ? C140 C142 1.528(5) . ? C140 C141 1.532(5) . ? C140 C143 1.556(5) . ? C143 C144 1.542(6) . ? C144 C145 1.523(7) . ? C144 C146 1.526(7) . ? C144 C147 1.543(7) . ? C148 C149 1.513(5) . ? C150 C151 1.392(8) . ? O25 C153 1.596(15) . ? C153 C154 1.303(16) . ? O26 C155 1.316(16) . ? C155 C156 1.35(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 O1 C15 113.8(2) . . ? C16 O3 C17 116.0(3) . . ? C20 O4 C34 113.1(2) . . ? C35 O6 C36 114.5(4) . . ? C39 O7 C53 110.9(3) . . ? C54 O9 C55 115.8(3) . . ? C58 O10 C72 114.6(2) . . ? C73 O12 C74 116.2(4) . . ? C77 O13 C91 113.8(2) . . ? C92 O15 C93 115.9(3) . . ? C96 O16 C110 114.9(3) . . ? C111 O18 C112 116.3(3) . . ? C115 O19 C129 112.3(2) . . ? C130 O21 C131 115.2(4) . . ? C134 O22 C148 115.5(2) . . ? C149 O24 C150 114.9(4) . . ? C6 C1 O1 121.0(3) . . ? C6 C1 C2 121.6(3) . . ? O1 C1 C2 117.3(3) . . ? C3 C2 C1 117.5(3) . . ? C3 C2 C152 119.9(3) . . ? C1 C2 C152 122.4(3) . . ? C2 C3 C4 123.1(3) . . ? C5 C4 C3 117.1(3) . . ? C5 C4 C7 122.8(3) . . ? C3 C4 C7 120.0(3) . . ? C4 C5 C6 122.2(3) . . ? C1 C6 C5 118.0(3) . . ? C1 C6 C19 123.0(3) . . ? C5 C6 C19 118.9(3) . . ? C9 C7 C4 111.8(3) . . ? C9 C7 C10 111.9(3) . . ? C4 C7 C10 112.3(3) . . ? C9 C7 C8 106.9(3) . . ? C4 C7 C8 106.6(3) . . ? C10 C7 C8 106.9(3) . . ? C7 C10 C11 123.5(3) . . ? C13 C11 C12 109.9(5) . . ? C13 C11 C14 107.0(4) . . ? C12 C11 C14 107.5(4) . . ? C13 C11 C10 105.6(4) . . ? C12 C11 C10 114.3(3) . . ? C14 C11 C10 112.3(4) . . ? O1 C15 C16 111.6(3) . . ? O2 C16 O3 124.1(3) . . ? O2 C16 C15 126.4(3) . . ? O3 C16 C15 109.5(3) . . ? O3 C17 C18 107.7(4) . . ? C6 C19 C21 116.8(3) . . ? C21 C20 C25 121.9(3) . . ? C21 C20 O4 118.0(3) . . ? C25 C20 O4 120.0(3) . . ? C20 C21 C22 118.0(3) . . ? C20 C21 C19 119.9(3) . . ? C22 C21 C19 122.1(3) . . ? C23 C22 C21 122.4(3) . . ? C22 C23 C24 117.1(3) . . ? C22 C23 C26 121.5(3) . . ? C24 C23 C26 121.3(3) . . ? C25 C24 C23 123.0(3) . . ? C24 C25 C20 117.5(3) . . ? C24 C25 C38 120.2(3) . . ? C20 C25 C38 122.2(3) . . ? C29 C26 C28 107.1(9) . . ? C29 C26 C27 108.5(8) . . ? C28 C26 C27 105.3(7) . . ? C29 C26 C23 113.2(4) . . ? C28 C26 C23 111.3(4) . . ? C27 C26 C23 111.0(3) . . ? C26 C29 C30 148.8(5) . . ? C29 C30 C31 110.6(10) . . ? C29 C30 C32 110.2(7) . . ? C31 C30 C32 103.1(7) . . ? C29 C30 C33 113.0(5) . . ? C31 C30 C33 107.8(7) . . ? C32 C30 C33 111.7(5) . . ? O4 C34 C35 109.0(3) . . ? O5 C35 O6 123.5(4) . . ? O5 C35 C34 126.3(4) . . ? O6 C35 C34 110.2(3) . . ? C37 C36 O6 110.1(6) . . ? C40 C38 C25 113.0(3) . . ? C44 C39 C40 121.6(3) . . ? C44 C39 O7 119.5(3) . . ? C40 C39 O7 118.9(3) . . ? C41 C40 C39 118.0(3) . . ? C41 C40 C38 121.3(3) . . ? C39 C40 C38 120.7(3) . . ? C40 C41 C42 122.6(3) . . ? C43 C42 C41 117.0(3) . . ? C43 C42 C45 123.2(3) . . ? C41 C42 C45 119.7(3) . . ? C42 C43 C44 122.8(3) . . ? C39 C44 C43 118.0(3) . . ? C39 C44 C57 120.8(3) . . ? C43 C44 C57 121.2(3) . . ? C47 C45 C48 111.8(3) . . ? C47 C45 C46 106.5(4) . . ? C48 C45 C46 106.0(3) . . ? C47 C45 C42 111.6(3) . . ? C48 C45 C42 112.9(3) . . ? C46 C45 C42 107.7(3) . . ? C49 C48 C45 124.4(4) . . ? C50 C49 C52 109.9(7) . . ? C50 C49 C48 111.7(4) . . ? C52 C49 C48 114.1(6) . . ? C50 C49 C51 108.0(6) . . ? C52 C49 C51 105.5(6) . . ? C48 C49 C51 107.2(4) . . ? O7 C53 C54 113.2(3) . . ? O8 C54 O9 124.6(4) . . ? O8 C54 C53 121.1(4) . . ? O9 C54 C53 114.3(3) . . ? C56 C55 O9 107.4(4) . . ? C44 C57 C59 116.6(3) . . ? C59 C58 C63 122.1(3) . . ? C59 C58 O10 118.8(3) . . ? C63 C58 O10 118.9(3) . . ? C60 C59 C58 117.4(3) . . ? C60 C59 C57 124.3(3) . . ? C58 C59 C57 118.3(3) . . ? C59 C60 C61 122.8(3) . . ? C62 C61 C60 117.3(3) . . ? C62 C61 C64 123.1(3) . . ? C60 C61 C64 119.5(3) . . ? C61 C62 C63 122.6(3) . . ? C62 C63 C58 117.6(3) . . ? C62 C63 C76 121.7(3) . . ? C58 C63 C76 120.6(3) . . ? C61 C64 C66 112.3(3) . . ? C61 C64 C65 108.9(3) . . ? C66 C64 C65 105.4(4) . . ? C61 C64 C67 112.5(3) . . ? C66 C64 C67 111.5(3) . . ? C65 C64 C67 105.7(3) . . ? C68 C67 C64 124.3(3) . . ? C69 C68 C71 109.0(4) . . ? C69 C68 C70 107.3(4) . . ? C71 C68 C70 109.9(4) . . ? C69 C68 C67 112.6(3) . . ? C71 C68 C67 112.5(4) . . ? C70 C68 C67 105.3(4) . . ? O10 C72 C73 111.2(3) . . ? O11 C73 O12 123.8(4) . . ? O11 C73 C72 125.5(4) . . ? O12 C73 C72 110.8(3) . . ? C75 C74 O12 110.2(5) . . ? C78 C76 C63 116.7(3) . . ? C82 C77 O13 120.7(3) . . ? C82 C77 C78 121.5(3) . . ? O13 C77 C78 117.6(3) . . ? C79 C78 C77 117.4(3) . . ? C79 C78 C76 121.1(3) . . ? C77 C78 C76 121.2(3) . . ? C78 C79 C80 123.2(3) . . ? C81 C80 C79 116.6(3) . . ? C81 C80 C83 122.3(3) . . ? C79 C80 C83 121.1(3) . . ? C80 C81 C82 123.1(3) . . ? C77 C82 C81 117.8(3) . . ? C77 C82 C95 122.2(3) . . ? C81 C82 C95 120.0(3) . . ? C85 C83 C80 111.5(3) . . ? C85 C83 C84 108.0(4) . . ? C80 C83 C84 107.5(3) . . ? C85 C83 C86 112.1(3) . . ? C80 C83 C86 111.9(3) . . ? C84 C83 C86 105.3(3) . . ? C87 C86 C83 123.4(4) . . ? C88 C87 C90 109.1(5) . . ? C88 C87 C89 107.8(6) . . ? C90 C87 C89 107.8(5) . . ? C88 C87 C86 113.9(4) . . ? C90 C87 C86 111.8(5) . . ? C89 C87 C86 106.1(5) . . ? O13 C91 C92 111.9(3) . . ? O14 C92 O15 124.7(3) . . ? O14 C92 C91 125.7(3) . . ? O15 C92 C91 109.6(3) . . ? O15 C93 C94 107.9(4) . . ? C82 C95 C97 116.2(3) . . ? C101 C96 O16 118.7(3) . . ? C101 C96 C97 121.8(3) . . ? O16 C96 C97 119.3(3) . . ? C98 C97 C96 118.1(3) . . ? C98 C97 C95 122.9(3) . . ? C96 C97 C95 119.1(3) . . ? C97 C98 C99 122.4(3) . . ? C100 C99 C98 117.3(3) . . ? C100 C99 C102 121.9(3) . . ? C98 C99 C102 120.7(3) . . ? C99 C100 C101 122.9(3) . . ? C96 C101 C100 117.4(3) . . ? C96 C101 C114 121.5(3) . . ? C100 C101 C114 121.0(3) . . ? C105 C102 C104 116.4(4) . . ? C105 C102 C99 112.6(4) . . ? C104 C102 C99 111.7(3) . . ? C105 C102 C103 103.8(5) . . ? C104 C102 C103 102.7(5) . . ? C99 C102 C103 108.5(4) . . ? C102 C105 C106 123.1(5) . . ? C109 C106 C107 109.7(7) . . ? C109 C106 C108 110.1(7) . . ? C107 C106 C108 108.8(6) . . ? C109 C106 C105 117.3(7) . . ? C107 C106 C105 108.3(5) . . ? C108 C106 C105 102.1(6) . . ? O16 C110 C111 109.3(3) . . ? O17 C111 O18 124.1(3) . . ? O17 C111 C110 125.6(3) . . ? O18 C111 C110 110.3(3) . . ? C113 C112 O18 107.4(4) . . ? C116 C114 C101 113.0(3) . . ? C120 C115 O19 120.0(3) . . ? C120 C115 C116 121.6(3) . . ? O19 C115 C116 118.5(3) . . ? C117 C116 C115 117.8(3) . . ? C117 C116 C114 122.0(3) . . ? C115 C116 C114 120.1(3) . . ? C116 C117 C118 123.1(3) . . ? C119 C118 C117 116.8(3) . . ? C119 C118 C121 122.8(3) . . ? C117 C118 C121 120.4(3) . . ? C120 C119 C118 122.7(3) . . ? C119 C120 C115 118.0(3) . . ? C119 C120 C133 121.9(3) . . ? C115 C120 C133 120.0(3) . . ? C123 C121 C122 108.2(4) . . ? C123 C121 C118 111.6(3) . . ? C122 C121 C118 108.2(3) . . ? C123 C121 C124 112.6(3) . . ? C122 C121 C124 105.2(3) . . ? C118 C121 C124 110.7(3) . . ? C125 C124 C121 123.3(3) . . ? C128 C125 C124 114.6(3) . . ? C128 C125 C127 111.1(4) . . ? C124 C125 C127 111.7(4) . . ? C128 C125 C126 107.9(4) . . ? C124 C125 C126 106.7(3) . . ? C127 C125 C126 104.3(4) . . ? O19 C129 C130 111.7(3) . . ? O20 C130 O21 124.5(4) . . ? O20 C130 C129 122.0(4) . . ? O21 C130 C129 113.5(3) . . ? C132 C131 O21 111.7(5) . . ? C120 C133 C135 117.2(3) . . ? C139 C134 O22 120.0(3) . . ? C139 C134 C135 121.5(3) . . ? O22 C134 C135 118.4(3) . . ? C136 C135 C134 117.7(3) . . ? C136 C135 C133 123.9(3) . . ? C134 C135 C133 118.3(3) . . ? C137 C136 C135 122.5(3) . . ? C138 C137 C136 117.5(3) . . ? C138 C137 C140 120.3(3) . . ? C136 C137 C140 122.1(3) . . ? C137 C138 C139 122.3(3) . . ? C134 C139 C138 118.5(3) . . ? C134 C139 C152 120.8(3) . . ? C138 C139 C152 120.6(3) . . ? C142 C140 C141 107.3(3) . . ? C142 C140 C137 106.4(3) . . ? C141 C140 C137 112.1(3) . . ? C142 C140 C143 106.4(3) . . ? C141 C140 C143 112.0(3) . . ? C137 C140 C143 112.1(3) . . ? C144 C143 C140 123.5(4) . . ? C145 C144 C146 109.0(4) . . ? C145 C144 C143 113.2(3) . . ? C146 C144 C143 113.8(4) . . ? C145 C144 C147 108.6(4) . . ? C146 C144 C147 106.2(4) . . ? C143 C144 C147 105.5(4) . . ? O22 C148 C149 110.9(3) . . ? O23 C149 O24 124.9(4) . . ? O23 C149 C148 126.0(3) . . ? O24 C149 C148 109.1(3) . . ? C151 C150 O24 109.3(5) . . ? C2 C152 C139 115.4(3) . . ? C154 C153 O25 115.5(11) . . ? O26 C155 C156 93.4(13) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.256 _refine_diff_density_min -1.173 _refine_diff_density_rms 0.068