# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2007 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Gennady Ananchenko' _publ_contact_author_address ; National Research Council Canada Steacie Institute for Molecular Sciences Ottawa K1A 0R6 CANADA ; _publ_contact_author_email GENNADY.ANANCHENKO@NRC-CNRC.GC.CA _publ_section_title ; Alfa-C=O provides access to the cavity in acyl calix[4]arenes: A comparative study of crystal structures ; loop_ _publ_author_name 'Gennady Ananchenko' 'A. W. Coleman' 'Florent Perret' 'Michaela Pojarova' 'John Ripmeester' ; K.A.Udachin ; # Attachment 'gena69_rC4.cif' data_gena69 _database_code_depnum_ccdc_archive 'CCDC 632663' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common para-butylcalix(4)arene _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H56 O4' _chemical_formula_weight 648.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 10.3228(4) _cell_length_b 11.9213(4) _cell_length_c 15.8916(6) _cell_angle_alpha 71.948(2) _cell_angle_beta 88.950(2) _cell_angle_gamma 74.630(2) _cell_volume 1788.53(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9564 _exptl_absorpt_correction_T_max 0.9852 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71070 _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 67314 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0475 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 36.30 _reflns_number_total 17177 _reflns_number_gt 10898 _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^)+(0.1052P)^2^+0.4763P] 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 17177 _refine_ls_number_parameters 505 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.1102 _refine_ls_R_factor_gt 0.0696 _refine_ls_wR_factor_ref 0.2191 _refine_ls_wR_factor_gt 0.1891 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C41 C 0.0670(5) 0.7151(6) 0.4443(3) 0.0280(6) Uani 0.37 1 d PD A 3 H41A H 0.0570 0.7984 0.4479 0.034 Uiso 0.37 1 calc PR A 3 H41B H -0.0042 0.7209 0.4010 0.034 Uiso 0.37 1 calc PR A 3 C42 C 0.0475(5) 0.6316(6) 0.5345(3) 0.0312(6) Uani 0.37 1 d PD A 3 H42A H 0.1115 0.6347 0.5788 0.037 Uiso 0.37 1 calc PR A 3 H42B H 0.0707 0.5463 0.5327 0.037 Uiso 0.37 1 calc PR A 3 C43 C -0.0936(4) 0.6627(5) 0.5653(3) 0.0389(6) Uani 0.37 1 d PD A 3 H43A H -0.1568 0.6727 0.5158 0.047 Uiso 0.37 1 calc PR A 3 H43B H -0.1015 0.5900 0.6143 0.047 Uiso 0.37 1 calc PR A 3 C44 C -0.1424(8) 0.7685(5) 0.5957(6) 0.0563(9) Uani 0.37 1 d PD A 3 H44A H -0.1212 0.7442 0.6597 0.068 Uiso 0.37 1 calc PR A 3 H44B H -0.2402 0.8006 0.5828 0.068 Uiso 0.37 1 calc PR A 3 H44C H -0.0988 0.8322 0.5649 0.068 Uiso 0.37 1 calc PR A 3 C41B C 0.0808(7) 0.7244(7) 0.4527(5) 0.0280(6) Uani 0.28 1 d PD B 33 H41X H 0.0001 0.7407 0.4128 0.034 Uiso 0.28 1 d P C 33 H41Y H 0.0861 0.8040 0.4571 0.034 Uiso 0.28 1 d P D 33 C42B C 0.0637(7) 0.6397(7) 0.5458(4) 0.0312(6) Uani 0.28 1 d PD B 33 H42X H 0.0521 0.5624 0.5404 0.037 Uiso 0.28 1 calc PR B 33 H42Y H 0.1465 0.6192 0.5843 0.037 Uiso 0.28 1 calc PR B 33 C43B C -0.0577(5) 0.6990(6) 0.5899(4) 0.0389(6) Uani 0.28 1 d PD B 33 H43X H -0.0579 0.6444 0.6512 0.047 Uiso 0.28 1 calc PR B 33 H43Y H -0.0468 0.7773 0.5938 0.047 Uiso 0.28 1 calc PR B 33 C44B C -0.1916(6) 0.7239(6) 0.5417(6) 0.0563(9) Uani 0.28 1 d PD B 33 H44D H -0.1982 0.7881 0.4845 0.068 Uiso 0.28 1 calc PR B 33 H44E H -0.2643 0.7510 0.5774 0.068 Uiso 0.28 1 calc PR B 33 H44F H -0.1993 0.6487 0.5318 0.068 Uiso 0.28 1 calc PR B 33 C41A C 0.0479(4) 0.6626(4) 0.4244(2) 0.0280(6) Uani 0.35 1 d PD E 4 H41C H -0.0091 0.7287 0.3745 0.034 Uiso 0.35 1 calc PR E 4 H41D H 0.0125 0.5901 0.4358 0.034 Uiso 0.35 1 calc PR E 4 C42A C 0.0307(4) 0.7035(4) 0.5049(2) 0.0312(6) Uani 0.35 1 d PD E 4 H42C H 0.0601 0.7791 0.4939 0.037 Uiso 0.35 1 calc PR E 4 H42D H 0.0877 0.6393 0.5558 0.037 Uiso 0.35 1 calc PR E 4 C43A C -0.1185(4) 0.7286(5) 0.5276(3) 0.0389(6) Uani 0.35 1 d PD E 4 H43C H -0.1781 0.7731 0.4727 0.047 Uiso 0.35 1 calc PR E 4 H43D H -0.1407 0.6502 0.5565 0.047 Uiso 0.35 1 calc PR E 4 C44A C -0.1386(8) 0.8029(6) 0.5876(6) 0.0563(9) Uani 0.35 1 d PD E 4 H44G H -0.0672 0.7665 0.6357 0.068 Uiso 0.35 1 calc PR E 4 H44H H -0.2263 0.8053 0.6127 0.068 Uiso 0.35 1 calc PR E 4 H44I H -0.1356 0.8864 0.5546 0.068 Uiso 0.35 1 calc PR E 4 O2 O 0.75741(9) 0.62118(7) 0.13655(6) 0.02186(16) Uani 1 1 d . . . H2 H 0.7693 0.6279 0.1867 0.026 Uiso 1 1 calc R . . O3 O 0.76451(9) 0.62047(7) 0.30459(6) 0.02454(17) Uani 1 1 d . . . H3 H 0.7108 0.5771 0.3210 0.029 Uiso 1 1 calc R . . C12 C 0.71949(10) 0.73625(9) 0.07412(7) 0.01659(17) Uani 1 1 d . F . C13 C 0.64535(10) 0.75216(10) -0.00341(7) 0.01756(18) Uani 1 1 d D . . C14 C 0.61296(11) 0.86730(10) -0.06770(7) 0.01872(18) Uani 1 1 d . F . H14 H 0.5623 0.8793 -0.1206 0.022 Uiso 1 1 calc R . . C15 C 0.65246(10) 0.96549(10) -0.05696(7) 0.01835(18) Uani 1 1 d D . . C16 C 0.72479(11) 0.94614(10) 0.02190(7) 0.01832(18) Uani 1 1 d . F . H16 H 0.7513 1.0124 0.0307 0.022 Uiso 1 1 calc R . . C17 C 0.75940(10) 0.83288(10) 0.08813(7) 0.01687(17) Uani 1 1 d . . . C18 C 0.83525(11) 0.81693(10) 0.17367(7) 0.01915(18) Uani 1 1 d . F . H18B H 0.8894 0.8767 0.1621 0.023 Uiso 1 1 calc R . . H18A H 0.8979 0.7335 0.1948 0.023 Uiso 1 1 calc R . . C19 C 0.6290(5) 1.0876(5) -0.1289(3) 0.0220(5) Uani 0.667(2) 1 d PD F 1 H19A H 0.6020 1.1540 -0.1018 0.026 Uiso 0.667(2) 1 calc PR F 1 H19B H 0.5538 1.0973 -0.1707 0.026 Uiso 0.667(2) 1 calc PR F 1 C20 C 0.75487(19) 1.10077(17) -0.18090(12) 0.0248(3) Uani 0.667(2) 1 d PD F 1 H20A H 0.7398 1.1873 -0.2184 0.030 Uiso 0.667(2) 1 calc PR F 1 H20B H 0.8328 1.0804 -0.1382 0.030 Uiso 0.667(2) 1 calc PR F 1 C21 C 0.7890(2) 1.01856(18) -0.23978(13) 0.0281(3) Uani 0.667(2) 1 d PD F 1 H21A H 0.7860 0.9346 -0.2052 0.034 Uiso 0.667(2) 1 calc PR F 1 H21B H 0.7204 1.0498 -0.2903 0.034 Uiso 0.667(2) 1 calc PR F 1 C22 C 0.9278(7) 1.0140(7) -0.2751(5) 0.0448(7) Uani 0.667(2) 1 d PD F 1 H22A H 0.9349 1.0977 -0.3029 0.054 Uiso 0.667(2) 1 calc PR F 1 H22B H 0.9409 0.9705 -0.3191 0.054 Uiso 0.667(2) 1 calc PR F 1 H22C H 0.9970 0.9708 -0.2260 0.054 Uiso 0.667(2) 1 calc PR F 1 C19A C 0.6166(12) 1.0857(11) -0.1317(7) 0.0220(5) Uani 0.333(2) 1 d PD F 2 H19C H 0.6330 1.1510 -0.1107 0.026 Uiso 0.333(2) 1 calc PR F 2 H19D H 0.5198 1.1084 -0.1506 0.026 Uiso 0.333(2) 1 calc PR F 2 C20A C 0.7000(4) 1.0760(3) -0.2103(2) 0.0248(3) Uani 0.333(2) 1 d PD F 2 H20C H 0.6908 1.0044 -0.2263 0.030 Uiso 0.333(2) 1 calc PR F 2 H20D H 0.6624 1.1502 -0.2617 0.030 Uiso 0.333(2) 1 calc PR F 2 C21A C 0.8482(4) 1.0629(4) -0.1949(3) 0.0281(3) Uani 0.333(2) 1 d PD F 2 H21C H 0.8821 1.0036 -0.1356 0.034 Uiso 0.333(2) 1 calc PR F 2 H21D H 0.8613 1.1430 -0.1969 0.034 Uiso 0.333(2) 1 calc PR F 2 C22A C 0.9272(15) 1.0180(16) -0.2663(10) 0.0448(7) Uani 0.333(2) 1 d PD F 2 H22D H 0.8923 1.0761 -0.3251 0.054 Uiso 0.333(2) 1 calc PR F 2 H22E H 0.9172 0.9372 -0.2626 0.054 Uiso 0.333(2) 1 calc PR F 2 H22F H 1.0227 1.0121 -0.2570 0.054 Uiso 0.333(2) 1 calc PR F 2 C23 C 0.70384(12) 0.73841(10) 0.30595(7) 0.0208(2) Uani 1 1 d . F . C24 C 0.74042(11) 0.83553(10) 0.24539(7) 0.01927(19) Uani 1 1 d . . . C25 C 0.68216(13) 0.95378(10) 0.24862(7) 0.0224(2) Uani 1 1 d . F . H25 H 0.7078 1.0206 0.2085 0.027 Uiso 1 1 calc R . . C26 C 0.58773(14) 0.97654(11) 0.30891(8) 0.0268(2) Uani 1 1 d D . . C27 C 0.55306(15) 0.87721(12) 0.36773(8) 0.0299(3) Uani 1 1 d . F . H27 H 0.4884 0.8916 0.4092 0.036 Uiso 1 1 calc R . . C28 C 0.60973(14) 0.75714(11) 0.36802(8) 0.0275(2) Uani 1 1 d D . . H1 H 0.6442 0.4999 0.1311 0.030 Uiso 1 1 d . . . H4 H 0.5682 0.5296 0.2706 0.030 Uiso 1 1 d . . . O1 O 0.5770(3) 0.4865(3) 0.1641(2) 0.0229(5) Uani 0.65 1 d PD A 3 O4 O 0.5709(4) 0.5120(3) 0.3255(2) 0.0230(5) Uani 0.65 1 d PD A 3 C1 C 0.45890(15) 0.56392(18) 0.11761(11) 0.0158(3) Uani 0.65 1 d PGD A 3 C2 C 0.33757(17) 0.56597(16) 0.15733(9) 0.0180(4) Uani 0.65 1 d PG A 3 C3 C 0.21786(14) 0.64328(18) 0.11070(11) 0.0177(4) Uani 0.65 1 d PG A 3 H3X H 0.1349 0.6447 0.1378 0.021 Uiso 0.65 1 calc PR A 3 C4 C 0.21948(18) 0.7185(2) 0.02436(11) 0.0167(4) Uani 0.65 1 d PGD A 3 C5 C 0.3408(2) 0.7165(2) -0.01536(10) 0.0165(3) Uani 0.65 1 d PG A 3 H5 H 0.3419 0.7679 -0.0744 0.020 Uiso 0.65 1 calc PR A 3 C6 C 0.46052(17) 0.6392(2) 0.03127(12) 0.0154(3) Uani 0.65 1 d PGD A 3 C7 C 0.5951(4) 0.6461(4) -0.0118(2) 0.0165(4) Uani 0.65 1 d PD A 3 H7A H 0.6645 0.5681 0.0165 0.020 Uiso 0.65 1 calc PR A 3 H7B H 0.5834 0.6551 -0.0754 0.020 Uiso 0.65 1 calc PR A 3 C8 C 0.0898(7) 0.8037(6) -0.0302(5) 0.0252(3) Uani 0.65 1 d PD A 3 H8A H 0.0440 0.8610 0.0016 0.030 Uiso 0.65 1 calc PR A 3 H8B H 0.1140 0.8531 -0.0878 0.030 Uiso 0.65 1 calc PR A 3 C9 C -0.0070(4) 0.7374(4) -0.0478(3) 0.0181(5) Uani 0.65 1 d PD A 3 H9A H -0.0931 0.7983 -0.0746 0.022 Uiso 0.65 1 calc PR A 3 H9B H -0.0254 0.6828 0.0095 0.022 Uiso 0.65 1 calc PR A 3 C10 C 0.0460(4) 0.6591(3) -0.1107(2) 0.0248(5) Uani 0.65 1 d PD A 3 H10A H 0.0741 0.7115 -0.1654 0.030 Uiso 0.65 1 calc PR A 3 H10B H 0.1261 0.5918 -0.0809 0.030 Uiso 0.65 1 calc PR A 3 C11 C -0.0572(3) 0.6064(3) -0.13488(11) 0.0302(5) Uani 0.65 1 d PD A 3 H11A H -0.0837 0.5528 -0.0810 0.036 Uiso 0.65 1 calc PR A 3 H11B H -0.0199 0.5587 -0.1743 0.036 Uiso 0.65 1 calc PR A 3 H11C H -0.1362 0.6728 -0.1653 0.036 Uiso 0.65 1 calc PR A 3 C29 C 0.5712(3) 0.6527(3) 0.43670(11) 0.0334(3) Uani 0.65 1 d PRD A 3 H29X H 0.6452 0.5765 0.4468 0.040 Uiso 0.65 1 calc PR A 3 H29Y H 0.5600 0.6709 0.4935 0.040 Uiso 0.65 1 calc PR A 3 C34 C 0.44943(10) 0.56715(13) 0.35068(9) 0.0198(3) Uani 0.65 1 d PGD A 3 C35 C 0.44665(11) 0.63258(13) 0.40977(9) 0.0213(3) Uani 0.65 1 d PGD A 3 C36 C 0.32484(13) 0.68385(12) 0.43972(8) 0.0240(3) Uani 0.65 1 d PG A 3 H36 H 0.3229 0.7286 0.4801 0.029 Uiso 0.65 1 calc PR A 3 C37 C 0.20581(10) 0.66969(12) 0.41057(8) 0.0250(3) Uani 0.65 1 d PGD A 3 C38 C 0.20859(10) 0.60426(12) 0.35148(8) 0.0241(3) Uani 0.65 1 d PG A 3 H38 H 0.1272 0.5946 0.3316 0.029 Uiso 0.65 1 calc PR A 3 C39 C 0.33039(12) 0.55299(12) 0.32153(8) 0.0201(3) Uani 0.65 1 d PG A 3 C40 C 0.3326(2) 0.4850(2) 0.25348(14) 0.0210(4) Uani 0.65 1 d P A 3 H40A H 0.2511 0.4551 0.2577 0.025 Uiso 0.65 1 calc PR A 3 H40B H 0.4121 0.4126 0.2683 0.025 Uiso 0.65 1 calc PR A 3 O1A O 0.5920(7) 0.4813(7) 0.1509(5) 0.0229(5) Uani 0.35 1 d PD E 4 O4A O 0.5732(8) 0.4980(6) 0.3150(5) 0.0230(5) Uani 0.35 1 d PD E 4 C1A C 0.4737(3) 0.5571(4) 0.1028(2) 0.0158(3) Uani 0.35 1 d PGD E 4 C2A C 0.3527(4) 0.5518(3) 0.1415(2) 0.0180(4) Uani 0.35 1 d PG E 4 C3A C 0.2317(3) 0.6274(4) 0.0957(3) 0.0177(4) Uani 0.35 1 d PG E 4 H3A H 0.1490 0.6237 0.1221 0.021 Uiso 0.35 1 calc PR E 4 C4A C 0.2318(4) 0.7084(4) 0.0112(3) 0.0167(4) Uani 0.35 1 d PG E 4 C5A C 0.3528(5) 0.7138(5) -0.0275(2) 0.0165(3) Uani 0.35 1 d PG E 4 H5A H 0.3528 0.7692 -0.0852 0.020 Uiso 0.35 1 calc PR E 4 C6A C 0.4737(4) 0.6382(5) 0.0183(3) 0.0154(3) Uani 0.35 1 d PGD E 4 C7A C 0.6016(8) 0.6527(7) -0.0265(5) 0.0165(4) Uani 0.35 1 d PD E 4 H7A1 H 0.5853 0.6755 -0.0916 0.020 Uiso 0.35 1 calc PR E 4 H7A2 H 0.6732 0.5743 -0.0060 0.020 Uiso 0.35 1 calc PR E 4 C8A C 0.0925(13) 0.7957(11) -0.0271(10) 0.0252(3) Uani 0.35 1 d P E 4 H8A1 H 0.1036 0.8652 -0.0778 0.030 Uiso 0.35 1 calc PR E 4 H8A2 H 0.0473 0.8293 0.0188 0.030 Uiso 0.35 1 calc PR E 4 C9A C 0.0018(9) 0.7263(8) -0.0594(6) 0.0181(5) Uani 0.35 1 d P E 4 H9A1 H -0.0089 0.6577 -0.0079 0.022 Uiso 0.35 1 calc PR E 4 H9A2 H -0.0887 0.7837 -0.0795 0.022 Uiso 0.35 1 calc PR E 4 C10A C 0.0515(8) 0.6787(7) -0.1286(5) 0.0248(5) Uani 0.35 1 d P E 4 H10C H 0.1391 0.6167 -0.1075 0.030 Uiso 0.35 1 calc PR E 4 H10D H 0.0673 0.7460 -0.1792 0.030 Uiso 0.35 1 calc PR E 4 C11A C -0.0478(6) 0.6177(5) -0.1621(2) 0.0302(5) Uani 0.35 1 d P E 4 H11D H -0.0687 0.5546 -0.1117 0.036 Uiso 0.35 1 calc PR E 4 H11E H -0.0049 0.5802 -0.2060 0.036 Uiso 0.35 1 calc PR E 4 H11F H -0.1312 0.6806 -0.1893 0.036 Uiso 0.35 1 calc PR E 4 C29A C 0.5613(6) 0.6507(5) 0.4322(2) 0.0334(3) Uani 0.35 1 d PRD E 4 H29B H 0.5376 0.6713 0.4873 0.040 Uiso 0.35 1 calc PR E 4 H29A H 0.6382 0.5761 0.4483 0.040 Uiso 0.35 1 calc PR E 4 C34A C 0.4452(2) 0.5498(3) 0.3359(2) 0.0198(3) Uani 0.35 1 d PGD E 4 C35A C 0.4288(2) 0.6157(3) 0.3957(2) 0.0213(3) Uani 0.35 1 d PGD E 4 C36A C 0.3022(3) 0.6553(2) 0.42484(17) 0.0240(3) Uani 0.35 1 d PG E 4 H36A H 0.2910 0.7003 0.4657 0.029 Uiso 0.35 1 calc PR E 4 C37A C 0.1920(2) 0.6290(2) 0.39431(17) 0.0250(3) Uani 0.35 1 d PGD E 4 C38A C 0.2083(2) 0.5631(2) 0.33460(17) 0.0241(3) Uani 0.35 1 d PG E 4 H38A H 0.1330 0.5451 0.3137 0.029 Uiso 0.35 1 calc PR E 4 C39A C 0.3349(3) 0.5235(2) 0.30541(17) 0.0201(3) Uani 0.35 1 d PG E 4 C40A C 0.3497(5) 0.4614(4) 0.2337(3) 0.0210(4) Uani 0.35 1 d P E 4 H40C H 0.2734 0.4255 0.2338 0.025 Uiso 0.35 1 calc PR E 4 H40D H 0.4339 0.3938 0.2472 0.025 Uiso 0.35 1 calc PR E 4 C30 C 0.5262(8) 1.1052(6) 0.3144(4) 0.0335(4) Uani 0.754(4) 1 d PD F 10 H30A H 0.5456 1.1661 0.2608 0.040 Uiso 0.754(4) 1 calc PR F 10 H30B H 0.4272 1.1205 0.3154 0.040 Uiso 0.754(4) 1 calc PR F 10 C31 C 0.5808(4) 1.1223(5) 0.3965(3) 0.0427(8) Uani 0.754(4) 1 d PD F 10 H31A H 0.5617 1.0609 0.4499 0.051 Uiso 0.754(4) 1 calc PR F 10 H31B H 0.5328 1.2047 0.3993 0.051 Uiso 0.754(4) 1 calc PR F 10 C32 C 0.7337(3) 1.1093(2) 0.39820(17) 0.0436(6) Uani 0.754(4) 1 d PD F 10 H32A H 0.7648 1.1082 0.4571 0.052 Uiso 0.754(4) 1 calc PR F 10 H32B H 0.7813 1.0300 0.3900 0.052 Uiso 0.754(4) 1 calc PR F 10 C33 C 0.7704(3) 1.2122(3) 0.3271(2) 0.0469(6) Uani 0.754(4) 1 d PD F 10 H33A H 0.7430 1.2118 0.2684 0.056 Uiso 0.754(4) 1 calc PR F 10 H33B H 0.8680 1.2002 0.3317 0.056 Uiso 0.754(4) 1 calc PR F 10 H33C H 0.7241 1.2909 0.3350 0.056 Uiso 0.754(4) 1 calc PR F 10 C30A C 0.527(3) 1.1051(18) 0.3072(12) 0.0335(4) Uani 0.246(4) 1 d PD F 11 H30C H 0.4291 1.1271 0.2915 0.040 Uiso 0.246(4) 1 calc PR F 11 H30D H 0.5661 1.1600 0.2599 0.040 Uiso 0.246(4) 1 calc PR F 11 C31A C 0.5476(14) 1.1284(17) 0.3943(10) 0.0427(8) Uani 0.246(4) 1 d PD F 11 H31C H 0.5115 1.2172 0.3854 0.051 Uiso 0.246(4) 1 calc PR F 11 H31D H 0.4947 1.0849 0.4390 0.051 Uiso 0.246(4) 1 calc PR F 11 C32A C 0.6903(9) 1.0888(7) 0.4303(5) 0.0436(6) Uani 0.246(4) 1 d PD F 11 H32C H 0.7303 1.0015 0.4355 0.052 Uiso 0.246(4) 1 calc PR F 11 H32D H 0.6946 1.0973 0.4901 0.052 Uiso 0.246(4) 1 calc PR F 11 C33A C 0.7707(8) 1.1689(9) 0.3675(7) 0.0469(6) Uani 0.246(4) 1 d PD F 11 H33D H 0.7783 1.1504 0.3113 0.056 Uiso 0.246(4) 1 calc PR F 11 H33E H 0.8609 1.1513 0.3953 0.056 Uiso 0.246(4) 1 calc PR F 11 H33F H 0.7237 1.2557 0.3560 0.056 Uiso 0.246(4) 1 calc PR F 11 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 C41 0.0251(10) 0.0313(11) 0.0240(10) -0.0067(7) 0.0046(8) -0.0043(8) C42 0.0321(11) 0.0357(11) 0.0235(11) -0.0052(8) 0.0087(9) -0.0108(9) C43 0.0280(12) 0.0577(19) 0.0345(15) -0.0178(11) 0.0063(10) -0.0139(12) C44 0.0355(12) 0.041(2) 0.093(2) -0.018(2) 0.0134(14) -0.0148(17) C41B 0.0251(10) 0.0313(11) 0.0240(10) -0.0067(7) 0.0046(8) -0.0043(8) C42B 0.0321(11) 0.0357(11) 0.0235(11) -0.0052(8) 0.0087(9) -0.0108(9) C43B 0.0280(12) 0.0577(19) 0.0345(15) -0.0178(11) 0.0063(10) -0.0139(12) C44B 0.0355(12) 0.041(2) 0.093(2) -0.018(2) 0.0134(14) -0.0148(17) C41A 0.0251(10) 0.0313(11) 0.0240(10) -0.0067(7) 0.0046(8) -0.0043(8) C42A 0.0321(11) 0.0357(11) 0.0235(11) -0.0052(8) 0.0087(9) -0.0108(9) C43A 0.0280(12) 0.0577(19) 0.0345(15) -0.0178(11) 0.0063(10) -0.0139(12) C44A 0.0355(12) 0.041(2) 0.093(2) -0.018(2) 0.0134(14) -0.0148(17) O2 0.0233(4) 0.0191(3) 0.0219(4) -0.0062(3) 0.0002(3) -0.0041(3) O3 0.0294(4) 0.0168(3) 0.0248(4) -0.0055(3) 0.0002(3) -0.0031(3) C12 0.0152(4) 0.0183(4) 0.0180(4) -0.0078(3) 0.0028(3) -0.0051(3) C13 0.0157(4) 0.0203(4) 0.0194(4) -0.0102(3) 0.0014(3) -0.0048(3) C14 0.0162(4) 0.0219(4) 0.0189(4) -0.0088(4) 0.0002(3) -0.0036(3) C15 0.0163(4) 0.0200(4) 0.0191(4) -0.0075(3) 0.0032(3) -0.0040(3) C16 0.0177(4) 0.0204(4) 0.0196(4) -0.0084(3) 0.0040(3) -0.0074(3) C17 0.0152(4) 0.0208(4) 0.0175(4) -0.0084(3) 0.0032(3) -0.0070(3) C18 0.0182(4) 0.0232(5) 0.0191(4) -0.0087(4) 0.0007(3) -0.0083(4) C19 0.0213(10) 0.0199(5) 0.0217(6) -0.0056(4) -0.0003(6) -0.0016(6) C20 0.0260(7) 0.0237(7) 0.0217(7) -0.0023(5) 0.0005(5) -0.0074(6) C21 0.0265(7) 0.0279(7) 0.0230(7) -0.0039(6) 0.0033(6) -0.0010(6) C22 0.0341(7) 0.0432(10) 0.0543(17) -0.0165(10) 0.0179(9) -0.0059(7) C19A 0.0213(10) 0.0199(5) 0.0217(6) -0.0056(4) -0.0003(6) -0.0016(6) C20A 0.0260(7) 0.0237(7) 0.0217(7) -0.0023(5) 0.0005(5) -0.0074(6) C21A 0.0265(7) 0.0279(7) 0.0230(7) -0.0039(6) 0.0033(6) -0.0010(6) C22A 0.0341(7) 0.0432(10) 0.0543(17) -0.0165(10) 0.0179(9) -0.0059(7) C23 0.0264(5) 0.0183(4) 0.0165(4) -0.0056(3) 0.0009(4) -0.0037(4) C24 0.0229(5) 0.0203(4) 0.0160(4) -0.0071(3) 0.0003(3) -0.0065(4) C25 0.0300(5) 0.0200(4) 0.0187(5) -0.0074(4) 0.0002(4) -0.0074(4) C26 0.0367(6) 0.0223(5) 0.0213(5) -0.0098(4) 0.0028(4) -0.0044(5) C27 0.0417(7) 0.0257(5) 0.0199(5) -0.0090(4) 0.0090(5) -0.0037(5) C28 0.0388(6) 0.0228(5) 0.0167(5) -0.0037(4) 0.0079(4) -0.0047(5) O1 0.0192(8) 0.0183(5) 0.0271(11) -0.0036(6) -0.0039(7) -0.0022(5) O4 0.0242(4) 0.0200(8) 0.0242(9) -0.0077(6) 0.0027(5) -0.0041(5) C1 0.0162(6) 0.0152(5) 0.0171(8) -0.0061(5) 0.0002(5) -0.0048(4) C2 0.0191(6) 0.0174(6) 0.0184(8) -0.0046(5) 0.0009(5) -0.0075(5) C3 0.0167(6) 0.0188(7) 0.0195(8) -0.0072(5) 0.0023(5) -0.0064(5) C4 0.0166(6) 0.0158(6) 0.0195(8) -0.0081(5) 0.0003(5) -0.0043(4) C5 0.0179(6) 0.0166(4) 0.0165(7) -0.0064(5) 0.0002(5) -0.0059(4) C6 0.0168(6) 0.0160(4) 0.0157(7) -0.0075(5) 0.0021(4) -0.0057(4) C7 0.0201(6) 0.0189(6) 0.0124(12) -0.0078(7) 0.0007(7) -0.0051(4) C8 0.0206(5) 0.0180(8) 0.0322(7) -0.0013(6) -0.0053(5) -0.0050(5) C9 0.0121(7) 0.0186(8) 0.0237(12) -0.0091(7) 0.0027(7) -0.0020(6) C10 0.0208(6) 0.0259(12) 0.0256(15) -0.0038(9) 0.0022(9) -0.0080(8) C11 0.0336(8) 0.0316(9) 0.0256(13) -0.0103(11) -0.0078(11) -0.0071(7) C29 0.0487(9) 0.0249(6) 0.0194(6) -0.0013(4) 0.0124(6) -0.0056(6) C34 0.0231(5) 0.0173(7) 0.0164(7) -0.0020(5) 0.0024(5) -0.0053(5) C35 0.0274(7) 0.0186(7) 0.0166(7) -0.0020(5) 0.0035(6) -0.0086(5) C36 0.0328(8) 0.0187(8) 0.0194(7) -0.0047(5) 0.0070(6) -0.0075(6) C37 0.0271(7) 0.0240(9) 0.0197(7) -0.0029(6) 0.0047(6) -0.0050(6) C38 0.0241(6) 0.0248(9) 0.0201(8) -0.0028(6) 0.0032(5) -0.0066(7) C39 0.0246(6) 0.0179(8) 0.0157(7) -0.0012(5) 0.0022(5) -0.0073(6) C40 0.0229(7) 0.0210(9) 0.0185(10) -0.0027(5) 0.0028(6) -0.0094(7) O1A 0.0192(8) 0.0183(5) 0.0271(11) -0.0036(6) -0.0039(7) -0.0022(5) O4A 0.0242(4) 0.0200(8) 0.0242(9) -0.0077(6) 0.0027(5) -0.0041(5) C1A 0.0162(6) 0.0152(5) 0.0171(8) -0.0061(5) 0.0002(5) -0.0048(4) C2A 0.0191(6) 0.0174(6) 0.0184(8) -0.0046(5) 0.0009(5) -0.0075(5) C3A 0.0167(6) 0.0188(7) 0.0195(8) -0.0072(5) 0.0023(5) -0.0064(5) C4A 0.0166(6) 0.0158(6) 0.0195(8) -0.0081(5) 0.0003(5) -0.0043(4) C5A 0.0179(6) 0.0166(4) 0.0165(7) -0.0064(5) 0.0002(5) -0.0059(4) C6A 0.0168(6) 0.0160(4) 0.0157(7) -0.0075(5) 0.0021(4) -0.0057(4) C7A 0.0201(6) 0.0189(6) 0.0124(12) -0.0078(7) 0.0007(7) -0.0051(4) C8A 0.0206(5) 0.0180(8) 0.0322(7) -0.0013(6) -0.0053(5) -0.0050(5) C9A 0.0121(7) 0.0186(8) 0.0237(12) -0.0091(7) 0.0027(7) -0.0020(6) C10A 0.0208(6) 0.0259(12) 0.0256(15) -0.0038(9) 0.0022(9) -0.0080(8) C11A 0.0336(8) 0.0316(9) 0.0256(13) -0.0103(11) -0.0078(11) -0.0071(7) C29A 0.0487(9) 0.0249(6) 0.0194(6) -0.0013(4) 0.0124(6) -0.0056(6) C34A 0.0231(5) 0.0173(7) 0.0164(7) -0.0020(5) 0.0024(5) -0.0053(5) C35A 0.0274(7) 0.0186(7) 0.0166(7) -0.0020(5) 0.0035(6) -0.0086(5) C36A 0.0328(8) 0.0187(8) 0.0194(7) -0.0047(5) 0.0070(6) -0.0075(6) C37A 0.0271(7) 0.0240(9) 0.0197(7) -0.0029(6) 0.0047(6) -0.0050(6) C38A 0.0241(6) 0.0248(9) 0.0201(8) -0.0028(6) 0.0032(5) -0.0066(7) C39A 0.0246(6) 0.0179(8) 0.0157(7) -0.0012(5) 0.0022(5) -0.0073(6) C40A 0.0229(7) 0.0210(9) 0.0185(10) -0.0027(5) 0.0028(6) -0.0094(7) C30 0.0422(8) 0.0256(6) 0.0350(11) -0.0168(7) 0.0066(8) -0.0050(5) C31 0.075(2) 0.0328(9) 0.0267(7) -0.0174(6) 0.0170(14) -0.0159(16) C32 0.0667(17) 0.0285(9) 0.0287(11) -0.0117(9) -0.0139(10) 0.0027(10) C33 0.0390(10) 0.0460(14) 0.0537(16) -0.0185(11) 0.0026(11) -0.0051(10) C30A 0.0422(8) 0.0256(6) 0.0350(11) -0.0168(7) 0.0066(8) -0.0050(5) C31A 0.075(2) 0.0328(9) 0.0267(7) -0.0174(6) 0.0170(14) -0.0159(16) C32A 0.0667(17) 0.0285(9) 0.0287(11) -0.0117(9) -0.0139(10) 0.0027(10) C33A 0.0390(10) 0.0460(14) 0.0537(16) -0.0185(11) 0.0026(11) -0.0051(10) _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 C41 C42 1.516(6) . ? C41 C37 1.540(5) . ? C42 C43 1.517(5) . ? C43 C44 1.452(7) . ? C41B C42B 1.549(7) . ? C42B C43B 1.538(7) . ? C43B C44B 1.505(7) . ? C41A C42A 1.496(5) . ? C41A C37A 1.543(4) . ? C42A C43A 1.548(5) . ? C43A C44A 1.469(7) . ? O2 C12 1.3803(13) . ? O3 C23 1.3860(14) . ? C12 C13 1.3973(15) . ? C12 C17 1.4002(14) . ? C13 C14 1.3928(15) . ? C13 C7A 1.518(9) . ? C13 C7 1.529(4) . ? C14 C15 1.3946(15) . ? C15 C16 1.3946(15) . ? C15 C19 1.509(5) . ? C15 C19A 1.510(10) . ? C16 C17 1.3913(15) . ? C17 C18 1.5155(15) . ? C18 C24 1.5190(15) . ? C19 C20 1.544(5) . ? C20 C21 1.528(3) . ? C21 C22 1.524(7) . ? C19A C20A 1.521(11) . ? C20A C21A 1.512(5) . ? C21A C22A 1.533(13) . ? C23 C24 1.3918(15) . ? C23 C28 1.3975(17) . ? C24 C25 1.3950(16) . ? C25 C26 1.3886(18) . ? C26 C27 1.3894(18) . ? C26 C30A 1.49(2) . ? C26 C30 1.525(6) . ? C27 C28 1.3939(18) . ? C28 C29 1.518(3) . ? C28 C29A 1.554(5) . ? O1 C1 1.378(3) . ? O4 C34 1.368(3) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C2 C40 1.542(3) . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C4 C8 1.533(6) . ? C5 C6 1.3900 . ? C6 C7 1.548(4) . ? C8 C9 1.506(9) . ? C9 C10 1.567(5) . ? C10 C11 1.482(5) . ? C29 C35 1.463(3) . ? C34 C35 1.3900 . ? C34 C39 1.3900 . ? C35 C36 1.3900 . ? C36 C37 1.3900 . ? C37 C38 1.3900 . ? C38 C39 1.3900 . ? C39 C40 1.536(2) . ? O1A C1A 1.383(7) . ? O4A C34A 1.385(7) . ? C1A C2A 1.3900 . ? C1A C6A 1.3900 . ? C2A C3A 1.3900 . ? C2A C40A 1.532(6) . ? C3A C4A 1.3900 . ? C4A C5A 1.3900 . ? C4A C8A 1.538(12) . ? C5A C6A 1.3900 . ? C6A C7A 1.513(8) . ? C8A C9A 1.586(18) . ? C9A C10A 1.417(12) . ? C10A C11A 1.587(11) . ? C29A C35A 1.692(6) . ? C34A C35A 1.3900 . ? C34A C39A 1.3900 . ? C35A C36A 1.3900 . ? C36A C37A 1.3900 . ? C37A C38A 1.3900 . ? C38A C39A 1.3900 . ? C39A C40A 1.526(4) . ? C30 C31 1.522(6) . ? C31 C32 1.544(5) . ? C32 C33 1.516(4) . ? C30A C31A 1.523(17) . ? C31A C32A 1.488(14) . ? C32A C33A 1.548(11) . ? 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 C42 C41 C37 112.7(4) . . ? C41 C42 C43 114.8(4) . . ? C44 C43 C42 120.9(5) . . ? C43B C42B C41B 112.6(6) . . ? C44B C43B C42B 114.0(5) . . ? C42A C41A C37A 117.2(3) . . ? C41A C42A C43A 110.2(3) . . ? C44A C43A C42A 108.1(4) . . ? O2 C12 C13 118.65(9) . . ? O2 C12 C17 119.78(9) . . ? C13 C12 C17 121.54(10) . . ? C14 C13 C12 118.13(9) . . ? C14 C13 C7A 116.1(3) . . ? C12 C13 C7A 125.7(3) . . ? C14 C13 C7 122.63(15) . . ? C12 C13 C7 119.11(15) . . ? C7A C13 C7 8.9(4) . . ? C13 C14 C15 122.16(10) . . ? C14 C15 C16 117.87(10) . . ? C14 C15 C19 123.0(3) . . ? C16 C15 C19 119.0(3) . . ? C14 C15 C19A 118.3(6) . . ? C16 C15 C19A 123.8(6) . . ? C19 C15 C19A 5.5(8) . . ? C17 C16 C15 122.10(10) . . ? C16 C17 C12 118.19(9) . . ? C16 C17 C18 120.25(9) . . ? C12 C17 C18 121.54(9) . . ? C17 C18 C24 111.78(9) . . ? C15 C19 C20 112.7(3) . . ? C21 C20 C19 113.3(3) . . ? C22 C21 C20 111.8(3) . . ? C15 C19A C20A 110.8(7) . . ? C21A C20A C19A 114.9(6) . . ? C20A C21A C22A 109.9(7) . . ? O3 C23 C24 118.44(10) . . ? O3 C23 C28 119.85(10) . . ? C24 C23 C28 121.70(10) . . ? C23 C24 C25 118.33(10) . . ? C23 C24 C18 121.99(10) . . ? C25 C24 C18 119.60(10) . . ? C26 C25 C24 121.83(11) . . ? C25 C26 C27 118.05(11) . . ? C25 C26 C30A 119.1(9) . . ? C27 C26 C30A 122.9(9) . . ? C25 C26 C30 122.1(3) . . ? C27 C26 C30 119.8(3) . . ? C30A C26 C30 4.1(9) . . ? C26 C27 C28 122.33(12) . . ? C27 C28 C23 117.74(11) . . ? C27 C28 C29 119.40(15) . . ? C23 C28 C29 122.83(15) . . ? C27 C28 C29A 119.8(2) . . ? C23 C28 C29A 122.3(2) . . ? C29 C28 C29A 4.9(3) . . ? O1 C1 C2 119.62(17) . . ? O1 C1 C6 120.37(17) . . ? C2 C1 C6 120.0 . . ? C1 C2 C3 120.0 . . ? C1 C2 C40 121.26(13) . . ? C3 C2 C40 118.73(13) . . ? C4 C3 C2 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 C8 121.9(3) . . ? C5 C4 C8 118.1(3) . . ? C4 C5 C6 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 C7 118.89(17) . . ? C1 C6 C7 120.94(17) . . ? C13 C7 C6 113.5(3) . . ? C9 C8 C4 113.9(4) . . ? C8 C9 C10 113.6(4) . . ? C11 C10 C9 112.3(3) . . ? C35 C29 C28 112.61(16) . . ? O4 C34 C35 119.15(16) . . ? O4 C34 C39 120.76(16) . . ? C35 C34 C39 120.0 . . ? C36 C35 C34 120.0 . . ? C36 C35 C29 120.12(13) . . ? C34 C35 C29 119.81(13) . . ? C35 C36 C37 120.0 . . ? C38 C37 C36 120.0 . . ? C38 C37 C41 115.7(2) . . ? C36 C37 C41 124.2(2) . . ? C37 C38 C39 120.0 . . ? C38 C39 C34 120.0 . . ? C38 C39 C40 119.88(11) . . ? C34 C39 C40 120.08(11) . . ? C39 C40 C2 112.96(16) . . ? O1A C1A C2A 118.3(4) . . ? O1A C1A C6A 121.7(4) . . ? C2A C1A C6A 120.0 . . ? C1A C2A C3A 120.0 . . ? C1A C2A C40A 121.0(3) . . ? C3A C2A C40A 119.0(3) . . ? C2A C3A C4A 120.0 . . ? C5A C4A C3A 120.0 . . ? C5A C4A C8A 125.5(6) . . ? C3A C4A C8A 114.1(6) . . ? C6A C5A C4A 120.0 . . ? C5A C6A C1A 120.0 . . ? C5A C6A C7A 117.0(4) . . ? C1A C6A C7A 123.0(4) . . ? C6A C7A C13 108.7(6) . . ? C4A C8A C9A 110.8(9) . . ? C10A C9A C8A 115.5(9) . . ? C9A C10A C11A 113.2(7) . . ? C28 C29A C35A 117.5(3) . . ? O4A C34A C35A 119.9(4) . . ? O4A C34A C39A 119.6(4) . . ? C35A C34A C39A 120.0 . . ? C36A C35A C34A 120.0 . . ? C36A C35A C29A 119.3(2) . . ? C34A C35A C29A 120.7(2) . . ? C35A C36A C37A 120.0 . . ? C38A C37A C36A 120.0 . . ? C38A C37A C41A 114.8(2) . . ? C36A C37A C41A 125.1(2) . . ? C37A C38A C39A 120.0 . . ? C38A C39A C34A 120.0 . . ? C38A C39A C40A 119.6(2) . . ? C34A C39A C40A 120.2(2) . . ? C39A C40A C2A 111.7(3) . . ? C31 C30 C26 112.1(4) . . ? C30 C31 C32 113.4(4) . . ? C33 C32 C31 112.8(2) . . ? C26 C30A C31A 114.3(13) . . ? C32A C31A C30A 114.6(14) . . ? C31A C32A C33A 109.4(9) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 36.30 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.737 _refine_diff_density_min -0.647 _refine_diff_density_rms 0.067 # Attachment 'mishka8_rC6.cif' data_mishka8 _database_code_depnum_ccdc_archive 'CCDC 632664' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common para-n-hexylcalix(4)arene _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H72 O4' _chemical_formula_weight 761.10 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 11.0862(15) _cell_length_b 14.413(2) _cell_length_c 14.802(2) _cell_angle_alpha 78.182(2) _cell_angle_beta 74.463(2) _cell_angle_gamma 88.892(2) _cell_volume 2228.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellowish _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.134 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9661 _exptl_absorpt_correction_T_max 0.9965 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71070 _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 28230 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 30.01 _reflns_number_total 12547 _reflns_number_gt 9747 _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^)+(0.0676P)^2^+0.6171P] 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 12547 _refine_ls_number_parameters 513 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.1410 _refine_ls_wR_factor_gt 0.1263 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.11695(8) 0.36933(6) 0.45795(6) 0.02960(18) Uani 1 1 d . A 1 H1 H 0.1924 0.3781 0.4496 0.036 Uiso 1 1 calc R A 1 O2 O 0.11643(8) 0.18813(6) 0.44610(6) 0.03052(18) Uani 1 1 d . A 1 H2 H 0.1061 0.2438 0.4502 0.037 Uiso 1 1 calc R A 1 O3 O 0.36401(8) 0.19037(6) 0.42640(6) 0.02923(18) Uani 1 1 d . A 1 H3 H 0.2898 0.1826 0.4296 0.035 Uiso 1 1 calc R A 1 O4 O 0.36376(8) 0.37161(6) 0.43661(5) 0.02773(17) Uani 1 1 d . A 1 H4 H 0.3748 0.3160 0.4325 0.033 Uiso 1 1 calc R A 1 C1 C 0.33093(10) 0.45549(7) 0.56413(7) 0.0229(2) Uani 1 1 d . A 1 C2 C 0.22371(11) 0.50739(8) 0.53324(8) 0.0258(2) Uani 1 1 d . A 1 H2A H 0.2204 0.5703 0.5475 0.031 Uiso 1 1 calc R A 1 H2B H 0.2381 0.5144 0.4646 0.031 Uiso 1 1 calc R A 1 C3 C 0.09979(10) 0.45396(7) 0.58434(8) 0.0242(2) Uani 1 1 d . A 1 C4 C 0.03247(11) 0.46942(8) 0.67328(8) 0.0262(2) Uani 1 1 d . A 1 H4A H 0.0629 0.5148 0.6990 0.031 Uiso 1 1 calc R A 1 C5 C -0.07875(11) 0.41944(8) 0.72516(8) 0.0261(2) Uani 1 1 d . A 1 C6 C -0.12261(10) 0.35216(8) 0.68511(8) 0.0261(2) Uani 1 1 d . A 1 H6 H -0.1976 0.3188 0.7186 0.031 Uiso 1 1 calc R A 1 C7 C -0.05811(10) 0.33317(8) 0.59672(8) 0.0245(2) Uani 1 1 d . A 1 C8 C -0.10823(11) 0.25667(8) 0.55782(9) 0.0278(2) Uani 1 1 d . A 1 H8A H -0.1989 0.2531 0.5807 0.033 Uiso 1 1 calc R A 1 H8B H -0.0861 0.2747 0.4884 0.033 Uiso 1 1 calc R A 1 C9 C -0.05884(10) 0.15919(8) 0.58646(8) 0.0258(2) Uani 1 1 d . A 1 C10 C -0.12296(10) 0.09686(8) 0.67022(9) 0.0278(2) Uani 1 1 d . A 1 H10 H -0.1973 0.1156 0.7075 0.033 Uiso 1 1 calc R A 1 C11 C -0.07970(11) 0.00775(8) 0.69996(9) 0.0285(2) Uani 1 1 d . A 1 C12 C 0.03196(11) -0.01817(8) 0.64277(9) 0.0286(2) Uani 1 1 d . A 1 H12 H 0.0622 -0.0777 0.6613 0.034 Uiso 1 1 calc R A 1 C13 C 0.09970(11) 0.04132(8) 0.55938(8) 0.0267(2) Uani 1 1 d . A 1 C14 C 0.22553(11) 0.01201(8) 0.50395(9) 0.0284(2) Uani 1 1 d . A 1 H14A H 0.2404 0.0407 0.4365 0.034 Uiso 1 1 calc R A 1 H14B H 0.2245 -0.0563 0.5104 0.034 Uiso 1 1 calc R A 1 C15 C 0.33051(10) 0.04267(8) 0.54082(8) 0.0254(2) Uani 1 1 d . A 1 C16 C 0.36481(11) -0.01628(8) 0.61552(8) 0.0275(2) Uani 1 1 d . A 1 H16 H 0.3251 -0.0758 0.6406 0.033 Uiso 1 1 calc R A 1 C17 C 0.45684(11) 0.01058(8) 0.65445(8) 0.0273(2) Uani 1 1 d . A 1 C18 C 0.51505(10) 0.09957(8) 0.61630(8) 0.0267(2) Uani 1 1 d . A 1 H18 H 0.5758 0.1187 0.6422 0.032 Uiso 1 1 calc R A 1 C19 C 0.48523(10) 0.16125(8) 0.54027(8) 0.0241(2) Uani 1 1 d . A 1 C20 C 0.55202(10) 0.25778(8) 0.50028(8) 0.0257(2) Uani 1 1 d . A 1 H20A H 0.6367 0.2534 0.5071 0.031 Uiso 1 1 calc R A 1 H20B H 0.5577 0.2757 0.4324 0.031 Uiso 1 1 calc R A 1 C21 C 0.48668(10) 0.33444(8) 0.54964(7) 0.0224(2) Uani 1 1 d . A 1 C22 C 0.51726(10) 0.35378(8) 0.62967(7) 0.0236(2) Uani 1 1 d . A 1 H22 H 0.5792 0.3194 0.6518 0.028 Uiso 1 1 calc R A 1 C23 C 0.45806(10) 0.42278(8) 0.67714(7) 0.0241(2) Uani 1 1 d . A 1 C24 C 0.36507(11) 0.47265(8) 0.64321(8) 0.0249(2) Uani 1 1 d . A 1 H24 H 0.3244 0.5190 0.6744 0.030 Uiso 1 1 calc R A 1 C25 C 0.05306(10) 0.38502(8) 0.54713(8) 0.0240(2) Uani 1 1 d . A 1 C26 C 0.39347(10) 0.38680(8) 0.51778(7) 0.0224(2) Uani 1 1 d . A 1 C27 C 0.39229(10) 0.13134(8) 0.50379(8) 0.0243(2) Uani 1 1 d . A 1 C28 C 0.05244(10) 0.12976(8) 0.53148(8) 0.0257(2) Uani 1 1 d . A 1 C29 C -0.14589(12) 0.43552(9) 0.82333(9) 0.0302(2) Uani 1 1 d . A 1 H29A H -0.2337 0.4170 0.8375 0.036 Uiso 1 1 calc R A 1 H29B H -0.1407 0.5026 0.8233 0.036 Uiso 1 1 calc R A 1 C30 C -0.09177(12) 0.38000(9) 0.90187(8) 0.0316(2) Uani 1 1 d . A 1 H30A H -0.0943 0.3131 0.9005 0.038 Uiso 1 1 calc R A 1 H30B H -0.0047 0.4001 0.8888 0.038 Uiso 1 1 calc R A 1 C31 C -0.16207(13) 0.39346(10) 1.00159(9) 0.0369(3) Uani 1 1 d . A 1 H31A H -0.1571 0.4602 1.0033 0.044 Uiso 1 1 calc R A 1 H31B H -0.2497 0.3756 1.0135 0.044 Uiso 1 1 calc R A 1 C32 C -0.11259(14) 0.33627(10) 1.08133(9) 0.0387(3) Uani 1 1 d . A 1 H32A H -0.0252 0.3547 1.0699 0.046 Uiso 1 1 calc R A 1 H32B H -0.1166 0.2696 1.0791 0.046 Uiso 1 1 calc R A 1 C33 C -0.18363(17) 0.34886(12) 1.18082(10) 0.0485(4) Uani 1 1 d . A 1 H33A H -0.1761 0.4150 1.1841 0.058 Uiso 1 1 calc R A 1 H33B H -0.2717 0.3334 1.1912 0.058 Uiso 1 1 calc R A 1 C34 C -0.13803(19) 0.28826(13) 1.26012(11) 0.0553(4) Uani 1 1 d . A 1 H34A H -0.1507 0.2225 1.2604 0.083 Uiso 1 1 calc R A 1 H34B H -0.1840 0.3017 1.3206 0.083 Uiso 1 1 calc R A 1 H34C H -0.0504 0.3021 1.2498 0.083 Uiso 1 1 calc R A 1 C35 C -0.14706(12) -0.05819(9) 0.79189(9) 0.0325(3) Uani 1 1 d . A 1 H35A H -0.1453 -0.1224 0.7811 0.039 Uiso 1 1 calc R A 1 H35B H -0.2341 -0.0412 0.8096 0.039 Uiso 1 1 calc R A 1 C36 C -0.09064(11) -0.05607(8) 0.87527(9) 0.0296(2) Uani 1 1 d . A 1 H36A H -0.0031 -0.0717 0.8571 0.036 Uiso 1 1 calc R A 1 H36B H -0.0944 0.0077 0.8873 0.036 Uiso 1 1 calc R A 1 C37 C -0.15771(12) -0.12475(8) 0.96700(9) 0.0313(2) Uani 1 1 d . A 1 H37A H -0.1473 -0.1889 0.9561 0.038 Uiso 1 1 calc R A 1 H37B H -0.2466 -0.1129 0.9812 0.038 Uiso 1 1 calc R A 1 C38 C -0.11237(12) -0.11849(9) 1.05422(9) 0.0320(2) Uani 1 1 d . A 1 H38A H -0.0237 -0.1308 1.0405 0.038 Uiso 1 1 calc R A 1 H38B H -0.1227 -0.0545 1.0655 0.038 Uiso 1 1 calc R A 1 C39 C -0.18177(13) -0.18795(9) 1.14493(10) 0.0370(3) Uani 1 1 d . A 1 H39A H -0.2707 -0.1766 1.1574 0.044 Uiso 1 1 calc R A 1 H39B H -0.1697 -0.2520 1.1339 0.044 Uiso 1 1 calc R A 1 C40 C -0.14016(17) -0.18126(12) 1.23346(12) 0.0522(4) Uani 1 1 d . A 1 H40A H -0.0526 -0.1938 1.2225 0.078 Uiso 1 1 calc R A 1 H40B H -0.1875 -0.2271 1.2874 0.078 Uiso 1 1 calc R A 1 H40C H -0.1542 -0.1187 1.2463 0.078 Uiso 1 1 calc R A 1 C41 C 0.48799(12) -0.05514(9) 0.73764(8) 0.0310(2) Uani 1 1 d . A 1 H41A H 0.5657 -0.0330 0.7458 0.037 Uiso 1 1 calc R A 1 H41B H 0.5003 -0.1181 0.7238 0.037 Uiso 1 1 calc R A 1 C42 C 0.38487(12) -0.06026(9) 0.82987(9) 0.0321(2) Uani 1 1 d . A 1 H42A H 0.3078 -0.0833 0.8214 0.039 Uiso 1 1 calc R A 1 H42B H 0.3714 0.0032 0.8422 0.039 Uiso 1 1 calc R A 1 C43 C 0.41281(12) -0.12404(9) 0.91671(9) 0.0331(3) Uani 1 1 d . A 1 H43A H 0.4243 -0.1881 0.9056 0.040 Uiso 1 1 calc R A 1 H43B H 0.4903 -0.1018 0.9252 0.040 Uiso 1 1 calc R A 1 C44 C 0.30831(13) -0.12539(10) 1.00709(9) 0.0367(3) Uani 1 1 d . A 1 H44A H 0.2320 -0.1496 0.9985 0.044 Uiso 1 1 calc R A 1 H44B H 0.2946 -0.0607 1.0155 0.044 Uiso 1 1 calc R A 1 C45 C 0.33137(15) -0.18425(10) 1.09790(10) 0.0407(3) Uani 1 1 d . A 1 H45A H 0.2545 -0.1896 1.1492 0.049 Uiso 1 1 calc R A 1 H45B H 0.3524 -0.2477 1.0878 0.049 Uiso 1 1 calc R A 1 C46 C 0.43491(15) -0.14381(12) 1.12896(11) 0.0470(3) Uani 1 1 d . A 1 H46A H 0.5126 -0.1421 1.0804 0.071 Uiso 1 1 calc R A 1 H46B H 0.4423 -0.1830 1.1879 0.071 Uiso 1 1 calc R A 1 H46C H 0.4155 -0.0807 1.1383 0.071 Uiso 1 1 calc R A 1 C47 C 0.48990(11) 0.44167(8) 0.76487(8) 0.0274(2) Uani 1 1 d . A 1 H47A H 0.4861 0.5091 0.7640 0.033 Uiso 1 1 calc R A 1 H47B H 0.5750 0.4232 0.7630 0.033 Uiso 1 1 calc R A 1 C48 C 0.40100(11) 0.38780(8) 0.85773(8) 0.0273(2) Uani 1 1 d . A 1 H48A H 0.3160 0.4060 0.8589 0.033 Uiso 1 1 calc R A 1 H48B H 0.4052 0.3204 0.8583 0.033 Uiso 1 1 calc R A 1 C49 C 0.42977(11) 0.40554(8) 0.94798(8) 0.0257(2) Uani 1 1 d . A 1 H49A H 0.5169 0.3925 0.9442 0.031 Uiso 1 1 calc R A 1 H49B H 0.4186 0.4721 0.9501 0.031 Uiso 1 1 calc R A 1 C50 C 0.34830(11) 0.34584(8) 1.04027(8) 0.0273(2) Uani 1 1 d . A 1 H50A H 0.3603 0.2793 1.0388 0.033 Uiso 1 1 calc R A 1 H50B H 0.2610 0.3583 1.0439 0.033 Uiso 1 1 calc R A 1 C51 C 0.37727(12) 0.36556(8) 1.12969(8) 0.0281(2) Uani 1 1 d . A 1 H51A H 0.4642 0.3520 1.1264 0.034 Uiso 1 1 calc R A 1 H51B H 0.3670 0.4324 1.1303 0.034 Uiso 1 1 calc R A 1 C52 C 0.29506(15) 0.30789(10) 1.22256(9) 0.0408(3) Uani 1 1 d . A 1 H52A H 0.2087 0.3203 1.2262 0.061 Uiso 1 1 calc R A 1 H52B H 0.3161 0.3253 1.2759 0.061 Uiso 1 1 calc R A 1 H52C H 0.3084 0.2416 1.2244 0.061 Uiso 1 1 calc R A 1 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 0.0279(4) 0.0393(4) 0.0226(4) -0.0047(3) -0.0100(3) 0.0040(3) O2 0.0330(4) 0.0359(4) 0.0258(4) -0.0081(3) -0.0120(3) 0.0008(3) O3 0.0280(4) 0.0421(5) 0.0218(4) -0.0102(3) -0.0114(3) 0.0048(3) O4 0.0316(4) 0.0354(4) 0.0182(3) -0.0057(3) -0.0099(3) -0.0013(3) C1 0.0230(5) 0.0238(5) 0.0207(5) -0.0004(4) -0.0067(4) -0.0030(4) C2 0.0283(5) 0.0233(5) 0.0248(5) 0.0006(4) -0.0092(4) 0.0001(4) C3 0.0247(5) 0.0231(5) 0.0248(5) 0.0001(4) -0.0105(4) 0.0030(4) C4 0.0277(5) 0.0243(5) 0.0282(5) -0.0047(4) -0.0110(4) 0.0033(4) C5 0.0252(5) 0.0269(5) 0.0263(5) -0.0037(4) -0.0089(4) 0.0062(4) C6 0.0210(5) 0.0272(5) 0.0295(5) -0.0024(4) -0.0087(4) 0.0029(4) C7 0.0222(5) 0.0267(5) 0.0276(5) -0.0035(4) -0.0132(4) 0.0043(4) C8 0.0217(5) 0.0337(6) 0.0328(6) -0.0084(4) -0.0148(4) 0.0032(4) C9 0.0212(5) 0.0314(5) 0.0311(5) -0.0111(4) -0.0143(4) 0.0010(4) C10 0.0203(5) 0.0334(6) 0.0339(6) -0.0117(5) -0.0108(4) -0.0008(4) C11 0.0249(5) 0.0302(5) 0.0347(6) -0.0094(4) -0.0128(5) -0.0041(4) C12 0.0281(5) 0.0270(5) 0.0368(6) -0.0110(4) -0.0158(5) 0.0009(4) C13 0.0251(5) 0.0314(5) 0.0309(5) -0.0151(4) -0.0138(4) 0.0019(4) C14 0.0297(6) 0.0315(5) 0.0306(5) -0.0157(4) -0.0127(5) 0.0047(4) C15 0.0240(5) 0.0327(5) 0.0249(5) -0.0156(4) -0.0089(4) 0.0065(4) C16 0.0270(5) 0.0309(5) 0.0276(5) -0.0126(4) -0.0080(4) 0.0073(4) C17 0.0267(5) 0.0350(6) 0.0239(5) -0.0123(4) -0.0090(4) 0.0111(4) C18 0.0234(5) 0.0377(6) 0.0246(5) -0.0150(4) -0.0101(4) 0.0088(4) C19 0.0207(5) 0.0331(5) 0.0215(5) -0.0129(4) -0.0058(4) 0.0059(4) C20 0.0195(5) 0.0384(6) 0.0208(5) -0.0098(4) -0.0053(4) 0.0018(4) C21 0.0198(5) 0.0284(5) 0.0182(4) -0.0040(4) -0.0040(4) -0.0028(4) C22 0.0210(5) 0.0301(5) 0.0198(5) -0.0037(4) -0.0069(4) -0.0020(4) C23 0.0247(5) 0.0286(5) 0.0187(5) -0.0036(4) -0.0059(4) -0.0060(4) C24 0.0266(5) 0.0248(5) 0.0227(5) -0.0049(4) -0.0055(4) -0.0028(4) C25 0.0245(5) 0.0269(5) 0.0220(5) -0.0020(4) -0.0112(4) 0.0052(4) C26 0.0223(5) 0.0282(5) 0.0157(4) -0.0012(4) -0.0056(4) -0.0049(4) C27 0.0230(5) 0.0336(5) 0.0201(5) -0.0123(4) -0.0075(4) 0.0071(4) C28 0.0237(5) 0.0325(5) 0.0268(5) -0.0111(4) -0.0128(4) -0.0003(4) C29 0.0286(6) 0.0317(6) 0.0298(6) -0.0080(4) -0.0062(5) 0.0060(4) C30 0.0312(6) 0.0364(6) 0.0272(5) -0.0086(5) -0.0068(5) 0.0067(5) C31 0.0406(7) 0.0411(7) 0.0285(6) -0.0104(5) -0.0065(5) 0.0109(5) C32 0.0454(8) 0.0420(7) 0.0296(6) -0.0109(5) -0.0095(5) 0.0101(6) C33 0.0580(9) 0.0573(9) 0.0297(7) -0.0110(6) -0.0100(6) 0.0128(7) C34 0.0724(12) 0.0584(10) 0.0340(7) -0.0058(7) -0.0158(7) 0.0057(8) C35 0.0268(6) 0.0317(6) 0.0402(6) -0.0058(5) -0.0117(5) -0.0065(4) C36 0.0232(5) 0.0297(5) 0.0369(6) -0.0079(5) -0.0086(5) -0.0026(4) C37 0.0272(6) 0.0283(5) 0.0395(6) -0.0061(5) -0.0111(5) -0.0040(4) C38 0.0266(6) 0.0301(6) 0.0403(6) -0.0066(5) -0.0110(5) -0.0032(4) C39 0.0340(6) 0.0346(6) 0.0423(7) -0.0032(5) -0.0133(6) -0.0046(5) C40 0.0594(10) 0.0538(9) 0.0446(8) -0.0024(7) -0.0211(7) -0.0102(7) C41 0.0314(6) 0.0361(6) 0.0285(5) -0.0095(5) -0.0116(5) 0.0117(5) C42 0.0314(6) 0.0377(6) 0.0283(6) -0.0079(5) -0.0091(5) 0.0081(5) C43 0.0347(6) 0.0347(6) 0.0293(6) -0.0061(5) -0.0085(5) 0.0064(5) C44 0.0315(6) 0.0410(7) 0.0345(6) -0.0051(5) -0.0059(5) 0.0011(5) C45 0.0501(8) 0.0355(7) 0.0306(6) -0.0034(5) -0.0031(6) -0.0029(6) C46 0.0488(8) 0.0567(9) 0.0351(7) -0.0078(6) -0.0120(6) 0.0069(7) C47 0.0287(5) 0.0338(6) 0.0222(5) -0.0082(4) -0.0089(4) -0.0043(4) C48 0.0306(6) 0.0311(5) 0.0221(5) -0.0062(4) -0.0093(4) -0.0043(4) C49 0.0287(5) 0.0291(5) 0.0212(5) -0.0068(4) -0.0082(4) -0.0016(4) C50 0.0321(6) 0.0289(5) 0.0221(5) -0.0050(4) -0.0093(4) -0.0044(4) C51 0.0344(6) 0.0291(5) 0.0226(5) -0.0060(4) -0.0101(4) -0.0016(4) C52 0.0549(8) 0.0423(7) 0.0233(6) 0.0002(5) -0.0117(6) -0.0110(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C25 1.3823(13) . ? O2 C28 1.3840(14) . ? O3 C27 1.3846(13) . ? O4 C26 1.3865(12) . ? C1 C26 1.3887(15) . ? C1 C24 1.3906(15) . ? C1 C2 1.5160(15) . ? C2 C3 1.5159(16) . ? C3 C4 1.3881(16) . ? C3 C25 1.3986(15) . ? C4 C5 1.3890(16) . ? C5 C6 1.3914(16) . ? C5 C29 1.5070(16) . ? C6 C7 1.3915(16) . ? C7 C25 1.3937(16) . ? C7 C8 1.5201(16) . ? C8 C9 1.5180(16) . ? C9 C10 1.3949(17) . ? C9 C28 1.3955(16) . ? C10 C11 1.3896(17) . ? C11 C12 1.3924(17) . ? C11 C35 1.5053(17) . ? C12 C13 1.3848(17) . ? C13 C28 1.3943(16) . ? C13 C14 1.5178(16) . ? C14 C15 1.5187(16) . ? C15 C16 1.3846(16) . ? C15 C27 1.3960(17) . ? C16 C17 1.3945(16) . ? C17 C18 1.3858(17) . ? C17 C41 1.5067(16) . ? C18 C19 1.3944(16) . ? C19 C27 1.3963(15) . ? C19 C20 1.5172(16) . ? C20 C21 1.5152(15) . ? C21 C26 1.3945(15) . ? C21 C22 1.3965(14) . ? C22 C23 1.3882(15) . ? C23 C24 1.3901(16) . ? C23 C47 1.5097(15) . ? C29 C30 1.5252(17) . ? C30 C31 1.5228(17) . ? C31 C32 1.5180(19) . ? C32 C33 1.5181(19) . ? C33 C34 1.509(2) . ? C35 C36 1.5314(17) . ? C36 C37 1.5211(17) . ? C37 C38 1.5246(18) . ? C38 C39 1.5240(18) . ? C39 C40 1.522(2) . ? C41 C42 1.5173(17) . ? C42 C43 1.5204(17) . ? C43 C44 1.5140(18) . ? C44 C45 1.5168(19) . ? C45 C46 1.512(2) . ? C47 C48 1.5265(16) . ? C48 C49 1.5242(15) . ? C49 C50 1.5198(16) . ? C50 C51 1.5235(15) . ? C51 C52 1.5170(17) . ? 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 C26 C1 C24 118.24(10) . . ? C26 C1 C2 121.40(9) . . ? C24 C1 C2 120.29(10) . . ? C3 C2 C1 111.03(9) . . ? C4 C3 C25 118.06(10) . . ? C4 C3 C2 119.81(10) . . ? C25 C3 C2 122.04(10) . . ? C3 C4 C5 122.23(11) . . ? C4 C5 C6 117.87(10) . . ? C4 C5 C29 120.44(11) . . ? C6 C5 C29 121.64(11) . . ? C5 C6 C7 122.23(11) . . ? C6 C7 C25 117.96(10) . . ? C6 C7 C8 120.00(10) . . ? C25 C7 C8 122.03(10) . . ? C9 C8 C7 113.68(9) . . ? C10 C9 C28 118.00(10) . . ? C10 C9 C8 120.50(10) . . ? C28 C9 C8 121.49(11) . . ? C11 C10 C9 122.32(11) . . ? C10 C11 C12 117.48(11) . . ? C10 C11 C35 122.19(11) . . ? C12 C11 C35 120.30(11) . . ? C13 C12 C11 122.48(11) . . ? C12 C13 C28 118.27(11) . . ? C12 C13 C14 120.02(10) . . ? C28 C13 C14 121.62(11) . . ? C13 C14 C15 110.80(9) . . ? C16 C15 C27 117.80(10) . . ? C16 C15 C14 120.28(11) . . ? C27 C15 C14 121.88(10) . . ? C15 C16 C17 122.26(11) . . ? C18 C17 C16 118.14(11) . . ? C18 C17 C41 121.70(11) . . ? C16 C17 C41 120.13(11) . . ? C17 C18 C19 121.95(10) . . ? C18 C19 C27 117.85(11) . . ? C18 C19 C20 120.16(10) . . ? C27 C19 C20 121.98(10) . . ? C21 C20 C19 113.01(9) . . ? C26 C21 C22 117.99(10) . . ? C26 C21 C20 121.40(9) . . ? C22 C21 C20 120.61(10) . . ? C23 C22 C21 121.99(10) . . ? C22 C23 C24 117.96(10) . . ? C22 C23 C47 121.55(10) . . ? C24 C23 C47 120.46(10) . . ? C23 C24 C1 122.10(10) . . ? O1 C25 C7 119.02(10) . . ? O1 C25 C3 119.31(10) . . ? C7 C25 C3 121.65(10) . . ? O4 C26 C1 118.81(10) . . ? O4 C26 C21 119.46(10) . . ? C1 C26 C21 121.72(10) . . ? O3 C27 C15 119.25(10) . . ? O3 C27 C19 118.73(10) . . ? C15 C27 C19 121.98(10) . . ? O2 C28 C13 118.79(10) . . ? O2 C28 C9 119.75(10) . . ? C13 C28 C9 121.44(11) . . ? C5 C29 C30 112.79(9) . . ? C31 C30 C29 112.97(10) . . ? C32 C31 C30 113.92(11) . . ? C31 C32 C33 113.90(12) . . ? C34 C33 C32 113.66(13) . . ? C11 C35 C36 113.54(10) . . ? C37 C36 C35 112.95(10) . . ? C36 C37 C38 114.67(10) . . ? C39 C38 C37 113.33(10) . . ? C40 C39 C38 114.22(11) . . ? C17 C41 C42 111.63(10) . . ? C41 C42 C43 113.82(10) . . ? C44 C43 C42 111.78(11) . . ? C43 C44 C45 115.10(11) . . ? C46 C45 C44 113.82(12) . . ? C23 C47 C48 112.25(9) . . ? C49 C48 C47 113.78(9) . . ? C50 C49 C48 113.85(9) . . ? C49 C50 C51 113.06(9) . . ? C52 C51 C50 113.74(10) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.385 _refine_diff_density_min -0.352 _refine_diff_density_rms 0.044 data_gena27 _database_code_depnum_ccdc_archive 'CCDC 632665' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common para-hexanoylcalix(4)arene _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H64 O8' _chemical_formula_weight 817.03 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 11.611(3) _cell_length_b 17.372(4) _cell_length_c 33.165(7) _cell_angle_alpha 88.536(3) _cell_angle_beta 88.251(4) _cell_angle_gamma 87.077(4) _cell_volume 6676(2) _cell_formula_units_Z 6 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.219 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2640 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9608 _exptl_absorpt_correction_T_max 0.9880 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71070 _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 83305 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_sigmaI/netI 0.0680 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 29.59 _reflns_number_total 36683 _reflns_number_gt 23258 _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^)+(0.1113P)^2^+2.8750P] 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 36683 _refine_ls_number_parameters 1822 _refine_ls_number_restraints 280 _refine_ls_R_factor_all 0.1089 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.2156 _refine_ls_wR_factor_gt 0.1869 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.990 _refine_ls_shift/su_max 0.415 _refine_ls_shift/su_mean 0.012 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 0.54601(13) 0.77685(8) 0.63970(4) 0.0275(3) Uani 1 1 d . A 1 H1 H 0.5412 0.8142 0.6231 0.033 Uiso 1 1 calc R A 1 O2 O 0.76364(13) 0.80093(9) 0.65660(4) 0.0307(3) Uani 1 1 d . A 1 H2 H 0.687(5) 0.790(3) 0.6507(16) 0.16(2) Uiso 1 1 d . B 1 O3 O 0.75948(13) 0.92476(9) 0.60814(5) 0.0334(3) Uani 1 1 d . A 1 H3 H 0.7709 0.8881 0.6248 0.040 Uiso 1 1 calc R A 1 O4 O 0.53784(12) 0.90015(8) 0.59143(4) 0.0279(3) Uani 1 1 d . A 1 H4 H 0.6036 0.9166 0.5947 0.034 Uiso 1 1 calc R A 1 C1 C 0.45124(15) 0.82588(10) 0.54219(6) 0.0213(4) Uani 1 1 d . A 1 C2 C 0.38627(16) 0.78037(10) 0.57472(6) 0.0217(4) Uani 1 1 d . A 1 H2A H 0.3686 0.8140 0.5980 0.026 Uiso 1 1 calc R A 1 H2B H 0.3120 0.7659 0.5639 0.026 Uiso 1 1 calc R A 1 C3 C 0.45256(16) 0.70786(10) 0.58929(5) 0.0211(4) Uani 1 1 d . A 1 C4 C 0.43587(17) 0.63757(11) 0.57174(6) 0.0233(4) Uani 1 1 d . A 1 H4A H 0.3811 0.6353 0.5511 0.028 Uiso 1 1 calc R A 1 C5 C 0.49785(18) 0.57033(11) 0.58374(6) 0.0268(4) Uani 1 1 d D A 1 C6 C 0.57814(18) 0.57476(12) 0.61388(6) 0.0282(4) Uani 1 1 d . A 1 H6 H 0.6217 0.5294 0.6218 0.034 Uiso 1 1 calc R A 1 C7 C 0.59629(17) 0.64326(11) 0.63261(5) 0.0245(4) Uani 1 1 d . A 1 C8 C 0.68592(17) 0.64626(12) 0.66488(6) 0.0270(4) Uani 1 1 d . A 1 H8A H 0.6927 0.5956 0.6792 0.032 Uiso 1 1 calc R A 1 H8B H 0.6597 0.6853 0.6848 0.032 Uiso 1 1 calc R A 1 C9 C 0.80369(17) 0.66603(12) 0.64750(5) 0.0254(4) Uani 1 1 d . A 1 C10 C 0.88135(17) 0.60740(12) 0.63492(6) 0.0265(4) Uani 1 1 d . A 1 H10 H 0.8603 0.5554 0.6379 0.032 Uiso 1 1 calc R A 1 C11 C 0.98928(17) 0.62301(12) 0.61808(6) 0.0262(4) Uani 1 1 d D A 1 C12 C 1.01886(17) 0.69958(13) 0.61363(6) 0.0289(4) Uani 1 1 d . A 1 H12 H 1.0920 0.7107 0.6019 0.035 Uiso 1 1 calc R A 1 C13 C 0.94425(17) 0.75976(12) 0.62587(6) 0.0261(4) Uani 1 1 d . A 1 C14 C 0.97809(18) 0.84214(12) 0.61997(6) 0.0299(4) Uani 1 1 d . A 1 H14A H 1.0629 0.8440 0.6216 0.036 Uiso 1 1 calc R A 1 H14B H 0.9425 0.8735 0.6420 0.036 Uiso 1 1 calc R A 1 C15 C 0.94045(17) 0.87672(11) 0.57963(6) 0.0270(4) Uani 1 1 d . A 1 C16 C 1.01230(17) 0.86833(11) 0.54580(6) 0.0276(4) Uani 1 1 d . A 1 H16 H 1.0862 0.8430 0.5485 0.033 Uiso 1 1 calc R A 1 C17 C 0.97912(16) 0.89601(11) 0.50791(6) 0.0254(4) Uani 1 1 d D A 1 C18 C 0.87078(17) 0.93330(11) 0.50455(6) 0.0252(4) Uani 1 1 d . A 1 H18 H 0.8473 0.9525 0.4789 0.030 Uiso 1 1 calc R A 1 C19 C 0.79586(16) 0.94320(10) 0.53775(6) 0.0245(4) Uani 1 1 d . A 1 C20 C 0.67630(16) 0.98082(11) 0.53252(6) 0.0256(4) Uani 1 1 d . A 1 H20A H 0.6794 1.0210 0.5108 0.031 Uiso 1 1 calc R A 1 H20B H 0.6504 1.0062 0.5578 0.031 Uiso 1 1 calc R A 1 C21 C 0.59014(16) 0.92214(10) 0.52193(6) 0.0225(4) Uani 1 1 d . A 1 C22 C 0.57406(16) 0.90498(11) 0.48212(6) 0.0249(4) Uani 1 1 d . A 1 H22 H 0.6155 0.9317 0.4615 0.030 Uiso 1 1 calc R A 1 C23 C 0.49870(17) 0.84942(11) 0.47141(6) 0.0245(4) Uani 1 1 d D A 1 C24 C 0.43799(16) 0.81003(11) 0.50176(6) 0.0227(4) Uani 1 1 d . A 1 H24 H 0.3869 0.7719 0.4947 0.027 Uiso 1 1 calc R A 1 C25 C 0.53202(16) 0.70938(11) 0.62001(5) 0.0220(4) Uani 1 1 d . A 1 C26 C 0.83672(17) 0.74148(12) 0.64301(6) 0.0258(4) Uani 1 1 d . A 1 C27 C 0.83232(17) 0.91464(11) 0.57505(6) 0.0256(4) Uani 1 1 d . A 1 C28 C 0.52674(16) 0.88224(10) 0.55153(6) 0.0217(4) Uani 1 1 d . A 1 O5 O 0.5365(4) 0.4384(3) 0.5720(2) 0.0499(11) Uani 0.65 1 d PD A 1 C29 C 0.4739(6) 0.4955(4) 0.5642(3) 0.0285(9) Uani 0.65 1 d PD A 1 C30 C 0.3766(5) 0.4897(3) 0.53541(17) 0.0253(9) Uani 0.65 1 d PD A 1 H30A H 0.3908 0.5247 0.5119 0.030 Uiso 0.65 1 calc PR A 1 H30B H 0.3040 0.5085 0.5491 0.030 Uiso 0.65 1 calc PR A 1 C31 C 0.3599(4) 0.4091(2) 0.51994(13) 0.0288(9) Uani 0.65 1 d PD A 1 H31A H 0.3443 0.3737 0.5431 0.035 Uiso 0.65 1 calc PR A 1 H31B H 0.4317 0.3898 0.5059 0.035 Uiso 0.65 1 calc PR A 1 C32 C 0.2599(3) 0.4093(2) 0.49094(11) 0.0328(7) Uani 0.65 1 d PD A 1 H32A H 0.2713 0.4499 0.4699 0.039 Uiso 0.65 1 calc PR A 1 H32B H 0.1874 0.4233 0.5061 0.039 Uiso 0.65 1 calc PR A 1 C33 C 0.2458(4) 0.3329(2) 0.47017(13) 0.0460(9) Uani 0.65 1 d PD A 1 H33A H 0.1816 0.3397 0.4513 0.055 Uiso 0.65 1 calc PR A 1 H33B H 0.3171 0.3199 0.4541 0.055 Uiso 0.65 1 calc PR A 1 C34 C 0.2228(4) 0.2678(2) 0.49790(17) 0.0612(11) Uani 0.65 1 d PD A 1 H34A H 0.2884 0.2581 0.5156 0.092 Uiso 0.65 1 calc PR A 1 H34B H 0.2117 0.2217 0.4823 0.092 Uiso 0.65 1 calc PR A 1 H34C H 0.1530 0.2801 0.5143 0.092 Uiso 0.65 1 calc PR A 1 O5A O 0.5696(9) 0.4414(7) 0.5750(5) 0.0499(11) Uani 0.35 1 d PD C 2 C29A C 0.4966(12) 0.4912(7) 0.5676(5) 0.0285(9) Uani 0.35 1 d PD C 2 C30A C 0.3945(11) 0.4811(7) 0.5430(4) 0.0253(9) Uani 0.35 1 d PD C 2 H30C H 0.3980 0.5154 0.5188 0.030 Uiso 0.35 1 calc PR C 2 H30D H 0.3236 0.4960 0.5589 0.030 Uiso 0.35 1 calc PR C 2 C31A C 0.3887(8) 0.3988(5) 0.5301(3) 0.0288(9) Uani 0.35 1 d PD C 2 H31C H 0.4604 0.3841 0.5146 0.035 Uiso 0.35 1 calc PR C 2 H31D H 0.3857 0.3649 0.5545 0.035 Uiso 0.35 1 calc PR C 2 C32A C 0.2875(6) 0.3850(4) 0.5050(2) 0.0328(7) Uani 0.35 1 d PD C 2 H32C H 0.2874 0.4212 0.4814 0.039 Uiso 0.35 1 calc PR C 2 H32D H 0.2156 0.3959 0.5211 0.039 Uiso 0.35 1 calc PR C 2 C33A C 0.2881(7) 0.3035(4) 0.4902(2) 0.0460(9) Uani 0.35 1 d PD C 2 H33C H 0.2920 0.2674 0.5137 0.055 Uiso 0.35 1 calc PR C 2 H33D H 0.3587 0.2935 0.4732 0.055 Uiso 0.35 1 calc PR C 2 C34A C 0.1842(7) 0.2861(5) 0.4659(3) 0.0612(11) Uani 0.35 1 d PD C 2 H34D H 0.1137 0.2946 0.4826 0.092 Uiso 0.35 1 calc PR C 2 H34E H 0.1908 0.2323 0.4576 0.092 Uiso 0.35 1 calc PR C 2 H34F H 0.1809 0.3202 0.4420 0.092 Uiso 0.35 1 calc PR C 2 O6 O 1.1745(4) 0.5750(3) 0.59768(11) 0.0329(8) Uani 0.72 1 d PD A 1 C35 C 1.0734(5) 0.5597(4) 0.6051(3) 0.0286(7) Uani 0.72 1 d PD A 1 C36 C 1.0418(5) 0.4759(3) 0.60756(12) 0.0304(9) Uani 0.72 1 d PD A 1 H36A H 1.0020 0.4654 0.6338 0.036 Uiso 0.72 1 calc PR A 1 H36B H 1.1130 0.4422 0.6060 0.036 Uiso 0.72 1 calc PR A 1 C37 C 0.9624(3) 0.45727(19) 0.57287(10) 0.0325(7) Uani 0.72 1 d PD A 1 H37A H 0.8914 0.4912 0.5745 0.039 Uiso 0.72 1 calc PR A 1 H37B H 1.0023 0.4684 0.5467 0.039 Uiso 0.72 1 calc PR A 1 C38 C 0.9290(3) 0.37299(19) 0.57418(11) 0.0432(8) Uani 0.72 1 d PD A 1 H38A H 0.9997 0.3395 0.5699 0.052 Uiso 0.72 1 calc PR A 1 H38B H 0.8970 0.3606 0.6015 0.052 Uiso 0.72 1 calc PR A 1 C39 C 0.8409(4) 0.3535(2) 0.54301(12) 0.0593(10) Uani 0.72 1 d PD A 1 H39A H 0.8171 0.3002 0.5486 0.071 Uiso 0.72 1 calc PR A 1 H39B H 0.7716 0.3885 0.5465 0.071 Uiso 0.72 1 calc PR A 1 C40 C 0.8831(4) 0.3594(3) 0.50020(13) 0.0653(11) Uani 0.72 1 d PD A 1 H40A H 0.8959 0.4134 0.4930 0.098 Uiso 0.72 1 calc PR A 1 H40B H 0.8254 0.3400 0.4826 0.098 Uiso 0.72 1 calc PR A 1 H40C H 0.9557 0.3286 0.4969 0.098 Uiso 0.72 1 calc PR A 1 O6A O 1.1710(12) 0.5826(10) 0.5895(4) 0.0329(8) Uani 0.28 1 d PD D 2 C35A C 1.0834(14) 0.5649(10) 0.6076(7) 0.0286(7) Uani 0.28 1 d PD D 2 C36A C 1.0390(15) 0.4885(8) 0.5990(4) 0.0304(9) Uani 0.28 1 d PD D 2 H36C H 0.9914 0.4717 0.6225 0.036 Uiso 0.28 1 calc PR D 2 H36D H 1.1056 0.4509 0.5963 0.036 Uiso 0.28 1 calc PR D 2 C37A C 0.9689(9) 0.4851(5) 0.5622(3) 0.0325(7) Uani 0.28 1 d PD D 2 H37C H 0.8989 0.5194 0.5656 0.039 Uiso 0.28 1 calc PR D 2 H37D H 1.0142 0.5050 0.5388 0.039 Uiso 0.28 1 calc PR D 2 C38A C 0.9335(8) 0.4066(5) 0.5532(3) 0.0432(8) Uani 0.28 1 d PD D 2 H38C H 1.0038 0.3726 0.5494 0.052 Uiso 0.28 1 calc PR D 2 H38D H 0.8896 0.3864 0.5769 0.052 Uiso 0.28 1 calc PR D 2 C39A C 0.8623(10) 0.4020(6) 0.5172(3) 0.0593(10) Uani 0.28 1 d PD D 2 H39C H 0.9044 0.4262 0.4942 0.071 Uiso 0.28 1 calc PR D 2 H39D H 0.7905 0.4340 0.5220 0.071 Uiso 0.28 1 calc PR D 2 C40A C 0.8286(11) 0.3248(7) 0.5042(4) 0.0653(11) Uani 0.28 1 d PD D 2 H40D H 0.8968 0.2956 0.4936 0.098 Uiso 0.28 1 calc PR D 2 H40E H 0.7712 0.3315 0.4832 0.098 Uiso 0.28 1 calc PR D 2 H40F H 0.7955 0.2966 0.5274 0.098 Uiso 0.28 1 calc PR D 2 O7 O 1.1618(5) 0.8599(4) 0.4781(2) 0.0364(10) Uani 0.65 1 d PD A -1 C41 C 1.0636(6) 0.8872(5) 0.4728(2) 0.0257(10) Uani 0.65 1 d PD A -1 C42 C 1.0245(7) 0.9125(4) 0.4312(2) 0.0279(10) Uani 0.65 1 d PD A -1 H42A H 1.0089 0.9691 0.4309 0.033 Uiso 0.65 1 calc PR A -1 H42B H 0.9509 0.8885 0.4262 0.033 Uiso 0.65 1 calc PR A -1 C43 C 1.1097(11) 0.8925(9) 0.3969(3) 0.0382(5) Uani 0.65 1 d PD A -1 H43A H 1.1151 0.8359 0.3939 0.046 Uiso 0.65 1 calc PR A -1 H43B H 1.1869 0.9090 0.4038 0.046 Uiso 0.65 1 calc PR A -1 C44 C 1.0753(12) 0.9307(8) 0.3567(3) 0.0406(7) Uani 0.65 1 d PD A -1 H44A H 1.0029 0.9091 0.3481 0.049 Uiso 0.65 1 calc PR A -1 H44B H 1.0598 0.9866 0.3606 0.049 Uiso 0.65 1 calc PR A -1 C45 C 1.1669(9) 0.9195(5) 0.3235(3) 0.0529(17) Uani 0.65 1 d PD A -1 H45A H 1.1796 0.8637 0.3184 0.063 Uiso 0.65 1 calc PR A -1 H45B H 1.2404 0.9388 0.3325 0.063 Uiso 0.65 1 calc PR A -1 C46 C 1.133(2) 0.9614(11) 0.2843(4) 0.0841(18) Uani 0.65 1 d PD A -1 H46A H 1.0545 0.9494 0.2778 0.126 Uiso 0.65 1 calc PR A -1 H46B H 1.1866 0.9445 0.2624 0.126 Uiso 0.65 1 calc PR A -1 H46C H 1.1372 1.0171 0.2875 0.126 Uiso 0.65 1 calc PR A -1 O7A O 1.1498(11) 0.8463(8) 0.4762(5) 0.0364(10) Uani 0.35 1 d PD E 2 C41A C 1.0545(13) 0.8775(11) 0.4722(4) 0.0257(10) Uani 0.35 1 d PD E 2 C42A C 1.0135(14) 0.8998(9) 0.4307(4) 0.0279(10) Uani 0.35 1 d PD E 2 H42C H 0.9822 0.9539 0.4308 0.033 Uiso 0.35 1 calc PR E 2 H42D H 0.9501 0.8668 0.4241 0.033 Uiso 0.35 1 calc PR E 2 C43A C 1.108(2) 0.8920(16) 0.3983(5) 0.0382(5) Uani 0.35 1 d PD E 2 H43C H 1.1770 0.9176 0.4073 0.046 Uiso 0.35 1 calc PR E 2 H43D H 1.1302 0.8367 0.3950 0.046 Uiso 0.35 1 calc PR E 2 C45A C 1.1522(19) 0.9018(11) 0.3230(5) 0.0529(17) Uani 0.35 1 d PD E 2 H45C H 1.2332 0.9028 0.3313 0.063 Uiso 0.35 1 calc PR E 2 H45D H 1.1372 0.8480 0.3165 0.063 Uiso 0.35 1 calc PR E 2 C46A C 1.137(4) 0.952(2) 0.2855(8) 0.0841(18) Uani 0.35 1 d PD E 2 H46D H 1.0600 0.9458 0.2749 0.126 Uiso 0.35 1 calc PR E 2 H46E H 1.1957 0.9367 0.2651 0.126 Uiso 0.35 1 calc PR E 2 H46F H 1.1448 1.0061 0.2922 0.126 Uiso 0.35 1 calc PR E 2 C44A C 1.073(2) 0.9269(16) 0.3579(5) 0.0406(7) Uani 0.35 1 d PD E 2 H44C H 0.9940 0.9124 0.3525 0.049 Uiso 0.35 1 calc PR E 2 H44D H 1.0722 0.9838 0.3594 0.049 Uiso 0.35 1 calc PR E 2 O8 O 0.5338(2) 0.87564(13) 0.40248(5) 0.0657(6) Uani 1 1 d D A 1 C47 C 0.4850(2) 0.83542(13) 0.42760(6) 0.0335(5) Uani 1 1 d D A 1 C48 C 0.4086(2) 0.77414(13) 0.41565(6) 0.0350(5) Uani 1 1 d D A 1 H48A H 0.3289 0.7872 0.4255 0.042 Uiso 1 1 calc R A 1 H48B H 0.4344 0.7246 0.4287 0.042 Uiso 1 1 calc R A 1 C49 C 0.4086(2) 0.76423(17) 0.37015(7) 0.0475(6) Uani 1 1 d D A 1 H49A H 0.3876 0.8145 0.3569 0.057 Uiso 1 1 calc R A 1 H49B H 0.4873 0.7478 0.3605 0.057 Uiso 1 1 calc R A 1 C50 C 0.3252(2) 0.70552(14) 0.35810(7) 0.0386(5) Uani 1 1 d D A 1 H50A H 0.2463 0.7225 0.3674 0.046 Uiso 1 1 calc R A 1 H50B H 0.3454 0.6556 0.3718 0.046 Uiso 1 1 calc R A 1 C51 C 0.3261(2) 0.69404(17) 0.31261(8) 0.0491(6) Uani 1 1 d D A 1 H51A H 0.3135 0.7448 0.2988 0.059 Uiso 1 1 calc R A 1 H51B H 0.4032 0.6725 0.3038 0.059 Uiso 1 1 calc R A 1 C52 C 0.2365(2) 0.64159(17) 0.29985(8) 0.0504(7) Uani 1 1 d D A 1 H52A H 0.2479 0.5913 0.3136 0.076 Uiso 1 1 calc R A 1 H52B H 0.2433 0.6350 0.2706 0.076 Uiso 1 1 calc R A 1 H52C H 0.1597 0.6640 0.3070 0.076 Uiso 1 1 calc R A 1 O1I O 0.23707(12) 0.37141(8) 0.74660(4) 0.0258(3) Uani 1 1 d . F 1 H1I H 0.296(2) 0.3722(15) 0.7507(8) 0.031 Uiso 1 1 d . G 1 O2I O 0.45531(12) 0.39960(8) 0.75935(4) 0.0251(3) Uani 1 1 d . F 1 H2I H 0.4544 0.4375 0.7431 0.030 Uiso 1 1 calc R F 1 O3I O 0.44953(12) 0.51339(8) 0.70455(4) 0.0246(3) Uani 1 1 d . F 1 H3I H 0.3827 0.5100 0.6960 0.029 Uiso 1 1 calc R F 1 O4I O 0.22890(12) 0.48479(8) 0.69096(4) 0.0254(3) Uani 1 1 d . F 1 H4I H 0.2276 0.4485 0.7082 0.031 Uiso 1 1 calc R F 1 C1I C 0.04867(16) 0.52676(10) 0.72223(5) 0.0202(3) Uani 1 1 d . F 1 C2I C 0.01751(16) 0.44482(11) 0.73268(5) 0.0222(4) Uani 1 1 d . F 1 H2I1 H 0.0537 0.4097 0.7124 0.027 Uiso 1 1 calc R F 1 H2I2 H -0.0672 0.4413 0.7316 0.027 Uiso 1 1 calc R F 1 C3I C 0.05707(16) 0.41928(10) 0.77435(5) 0.0207(4) Uani 1 1 d . F 1 C4I C -0.01463(16) 0.43146(10) 0.80792(6) 0.0217(4) Uani 1 1 d . F 1 H4I1 H -0.0904 0.4534 0.8044 0.026 Uiso 1 1 calc R F 1 C5I C 0.02171(16) 0.41231(10) 0.84679(5) 0.0207(4) Uani 1 1 d D F 1 C6I C 0.13298(16) 0.38023(10) 0.85151(6) 0.0217(4) Uani 1 1 d . F 1 H6I H 0.1588 0.3679 0.8779 0.026 Uiso 1 1 calc R F 1 C7I C 0.20723(16) 0.36580(10) 0.81857(6) 0.0203(3) Uani 1 1 d . F 1 C8I C 0.32740(16) 0.33003(10) 0.82462(6) 0.0218(4) Uani 1 1 d . F 1 H8I1 H 0.3506 0.2988 0.8009 0.026 Uiso 1 1 calc R F 1 H8I2 H 0.3257 0.2949 0.8486 0.026 Uiso 1 1 calc R F 1 C9I C 0.41724(15) 0.38944(10) 0.83033(5) 0.0203(3) Uani 1 1 d . F 1 C10I C 0.44410(17) 0.41073(11) 0.86868(6) 0.0255(4) Uani 1 1 d . F 1 H10I H 0.4068 0.3873 0.8914 0.031 Uiso 1 1 calc R F 1 C11I C 0.52469(18) 0.46585(12) 0.87489(6) 0.0268(4) Uani 1 1 d D F 1 C12I C 0.57764(16) 0.50117(11) 0.84167(6) 0.0228(4) Uani 1 1 d . F 1 H12I H 0.6309 0.5398 0.8458 0.027 Uiso 1 1 calc R F 1 C13I C 0.55414(15) 0.48111(10) 0.80254(5) 0.0190(3) Uani 1 1 d . F 1 C14I C 0.61175(15) 0.52218(10) 0.76692(5) 0.0203(3) Uani 1 1 d . F 1 H14C H 0.6872 0.5396 0.7751 0.024 Uiso 1 1 calc R F 1 H14D H 0.6263 0.4854 0.7448 0.024 Uiso 1 1 calc R F 1 C15I C 0.53934(15) 0.59110(10) 0.75142(5) 0.0191(3) Uani 1 1 d . F 1 C16I C 0.55224(16) 0.66390(11) 0.76692(5) 0.0209(4) Uani 1 1 d . F 1 H16I H 0.6081 0.6701 0.7868 0.025 Uiso 1 1 calc R F 1 C17I C 0.48477(16) 0.72758(10) 0.75382(6) 0.0217(4) Uani 1 1 d D F 1 C18I C 0.40348(16) 0.71814(11) 0.72453(5) 0.0219(4) Uani 1 1 d . F 1 H18I H 0.3564 0.7614 0.7159 0.026 Uiso 1 1 calc R F 1 C19I C 0.38959(15) 0.64703(11) 0.70763(5) 0.0206(4) Uani 1 1 d . F 1 C20I C 0.29956(16) 0.63882(11) 0.67611(5) 0.0220(4) Uani 1 1 d . F 1 H20C H 0.3257 0.5974 0.6575 0.026 Uiso 1 1 calc R F 1 H20D H 0.2907 0.6875 0.6601 0.026 Uiso 1 1 calc R F 1 C21I C 0.18406(16) 0.61996(11) 0.69543(5) 0.0205(4) Uani 1 1 d . F 1 C22I C 0.10621(16) 0.67861(11) 0.70740(5) 0.0216(4) Uani 1 1 d . F 1 H22I H 0.1257 0.7306 0.7027 0.026 Uiso 1 1 calc R F 1 C23I C 0.00069(16) 0.66391(11) 0.72600(5) 0.0210(4) Uani 1 1 d D F 1 C24I C -0.02666(16) 0.58751(11) 0.73305(5) 0.0215(4) Uani 1 1 d . F 1 H24I H -0.0989 0.5768 0.7456 0.026 Uiso 1 1 calc R F 1 C25I C 0.16739(16) 0.38608(10) 0.78015(5) 0.0204(3) Uani 1 1 d . F 1 C26I C 0.47516(15) 0.42439(10) 0.79772(5) 0.0200(3) Uani 1 1 d . F 1 C27I C 0.45839(15) 0.58439(10) 0.72154(5) 0.0194(3) Uani 1 1 d . F 1 C28I C 0.15359(15) 0.54410(10) 0.70308(5) 0.0198(3) Uani 1 1 d . F 1 O5I O -0.16091(13) 0.44771(9) 0.87567(4) 0.0345(3) Uani 1 1 d D F 1 C29I C -0.06132(17) 0.42562(11) 0.88155(6) 0.0250(4) Uani 1 1 d D F 1 C30I C -0.02008(18) 0.40988(13) 0.92384(6) 0.0300(4) Uani 1 1 d D F 1 H30E H 0.0456 0.4425 0.9284 0.036 Uiso 1 1 calc R F 1 H30F H 0.0087 0.3554 0.9261 0.036 Uiso 1 1 calc R F 1 C31I C -0.1115(2) 0.42494(13) 0.95667(6) 0.0332(5) Uani 1 1 d D F 1 H31E H -0.1814 0.3977 0.9503 0.040 Uiso 1 1 calc R F 1 H31F H -0.1328 0.4808 0.9569 0.040 Uiso 1 1 calc R F 1 C32I C -0.0723(2) 0.39883(15) 0.99842(7) 0.0414(6) Uani 1 1 d D F 1 H32E H -0.0010 0.4248 1.0043 0.050 Uiso 1 1 calc R F 1 H32F H -0.0531 0.3427 0.9983 0.050 Uiso 1 1 calc R F 1 C33I C -0.1613(3) 0.4154(2) 1.03212(8) 0.0616(9) Uani 1 1 d D F 1 H33E H -0.1259 0.4031 1.0584 0.074 Uiso 1 1 calc R F 1 H33F H -0.1843 0.4711 1.0314 0.074 Uiso 1 1 calc R F 1 C34I C -0.2673(3) 0.3697(2) 1.02874(11) 0.0871(13) Uani 1 1 d D F 1 H34G H -0.3030 0.3820 1.0028 0.131 Uiso 1 1 calc R F 1 H34H H -0.3223 0.3830 1.0508 0.131 Uiso 1 1 calc R F 1 H34I H -0.2454 0.3145 1.0304 0.131 Uiso 1 1 calc R F 1 O6I O 0.5439(2) 0.42995(14) 0.94402(6) 0.0453(6) Uani 0.77 1 d PD F 1 C35I C 0.5618(3) 0.47806(17) 0.91736(9) 0.0263(6) Uani 0.77 1 d PD F 1 C36I C 0.6171(8) 0.5534(4) 0.92502(19) 0.0308(4) Uani 0.77 1 d PD F 1 H36E H 0.5714 0.5965 0.9122 0.037 Uiso 0.77 1 calc PR F 1 H36F H 0.6957 0.5521 0.9126 0.037 Uiso 0.77 1 calc PR F 1 C37I C 0.6240(4) 0.56737(18) 0.97032(13) 0.0308(8) Uani 0.77 1 d PD F 1 H37E H 0.5450 0.5736 0.9823 0.037 Uiso 0.77 1 calc PR F 1 H37F H 0.6632 0.5220 0.9836 0.037 Uiso 0.77 1 calc PR F 1 C38I C 0.6891(3) 0.6384(3) 0.97799(15) 0.0309(8) Uani 0.77 1 d PD F 1 H38E H 0.6508 0.6832 0.9639 0.037 Uiso 0.77 1 calc PR F 1 H38F H 0.7683 0.6313 0.9663 0.037 Uiso 0.77 1 calc PR F 1 C39I C 0.6961(5) 0.6562(2) 1.02293(12) 0.0408(9) Uani 0.77 1 d PD F 1 H39E H 0.6169 0.6634 1.0346 0.049 Uiso 0.77 1 calc PR F 1 H39F H 0.7342 0.6114 1.0370 0.049 Uiso 0.77 1 calc PR F 1 C40I C 0.7611(5) 0.7268(3) 1.03059(13) 0.0445(11) Uani 0.77 1 d PD F 1 H40G H 0.8400 0.7200 1.0194 0.067 Uiso 0.77 1 calc PR F 1 H40H H 0.7634 0.7346 1.0597 0.067 Uiso 0.77 1 calc PR F 1 H40I H 0.7223 0.7719 1.0176 0.067 Uiso 0.77 1 calc PR F 1 O6J O 0.4697(7) 0.4735(5) 0.9437(2) 0.0453(6) Uani 0.23 1 d PD H 2 C35J C 0.5275(10) 0.5012(7) 0.9159(4) 0.0263(6) Uani 0.23 1 d P H 2 C36J C 0.618(3) 0.5535(13) 0.9255(7) 0.0308(4) Uani 0.23 1 d PD H 2 H36G H 0.6139 0.5970 0.9056 0.037 Uiso 0.23 1 calc PR H 2 H36H H 0.6931 0.5255 0.9212 0.037 Uiso 0.23 1 calc PR H 2 C37J C 0.6164(17) 0.5873(9) 0.9669(5) 0.0308(8) Uani 0.23 1 d PD H 2 H37G H 0.6203 0.5445 0.9872 0.037 Uiso 0.23 1 calc PR H 2 H37H H 0.5422 0.6168 0.9715 0.037 Uiso 0.23 1 calc PR H 2 C38J C 0.7141(16) 0.6398(13) 0.9738(6) 0.0309(8) Uani 0.23 1 d PD H 2 H38G H 0.7158 0.6815 0.9529 0.037 Uiso 0.23 1 calc PR H 2 H38H H 0.7894 0.6104 0.9731 0.037 Uiso 0.23 1 calc PR H 2 C39J C 0.688(2) 0.6733(10) 1.0158(5) 0.0408(9) Uani 0.23 1 d PD H 2 H39G H 0.6052 0.6884 1.0187 0.049 Uiso 0.23 1 calc PR H 2 H39H H 0.7075 0.6338 1.0369 0.049 Uiso 0.23 1 calc PR H 2 C40J C 0.759(2) 0.7427(11) 1.0209(6) 0.0445(11) Uani 0.23 1 d PD H 2 H40J H 0.8265 0.7397 1.0025 0.067 Uiso 0.23 1 calc PR H 2 H40K H 0.7840 0.7437 1.0488 0.067 Uiso 0.23 1 calc PR H 2 H40L H 0.7118 0.7897 1.0148 0.067 Uiso 0.23 1 calc PR H 2 O7I O 0.4130(5) 0.8547(3) 0.76757(17) 0.0349(10) Uani 0.62 1 d PD F 1 C41I C 0.4911(7) 0.8054(4) 0.7715(3) 0.0230(10) Uani 0.62 1 d PD F 1 C42I C 0.6002(9) 0.8244(5) 0.7919(3) 0.0248(6) Uani 0.62 1 d PD F 1 H42E H 0.6675 0.8068 0.7749 0.030 Uiso 0.62 1 calc PR F 1 H42F H 0.6044 0.7956 0.8180 0.030 Uiso 0.62 1 calc PR F 1 C43I C 0.6077(9) 0.9100(5) 0.7995(3) 0.0253(8) Uani 0.62 1 d PD F 1 H43E H 0.6123 0.9385 0.7733 0.030 Uiso 0.62 1 calc PR F 1 H43F H 0.5369 0.9291 0.8142 0.030 Uiso 0.62 1 calc PR F 1 C44I C 0.7124(8) 0.9259(4) 0.8238(3) 0.0240(9) Uani 0.62 1 d PD F 1 H44E H 0.7109 0.8938 0.8489 0.029 Uiso 0.62 1 calc PR F 1 H44F H 0.7831 0.9102 0.8081 0.029 Uiso 0.62 1 calc PR F 1 C45I C 0.7183(8) 1.0087(5) 0.8347(3) 0.0275(10) Uani 0.62 1 d PD F 1 H45E H 0.6447 1.0252 0.8485 0.033 Uiso 0.62 1 calc PR F 1 H45F H 0.7253 1.0401 0.8095 0.033 Uiso 0.62 1 calc PR F 1 C46I C 0.8166(8) 1.0261(6) 0.8616(2) 0.0342(12) Uani 0.62 1 d PD F 1 H46G H 0.8065 0.9994 0.8878 0.051 Uiso 0.62 1 calc PR F 1 H46H H 0.8166 1.0817 0.8656 0.051 Uiso 0.62 1 calc PR F 1 H46I H 0.8900 1.0083 0.8488 0.051 Uiso 0.62 1 calc PR F 1 O7J O 0.4318(9) 0.8591(6) 0.7582(3) 0.0349(10) Uani 0.38 1 d PD I 2 C41J C 0.5039(12) 0.8079(7) 0.7674(5) 0.0230(10) Uani 0.38 1 d PD I 2 C42J C 0.6025(15) 0.8210(9) 0.7947(6) 0.0248(6) Uani 0.38 1 d PD I 2 H42G H 0.6752 0.7995 0.7822 0.030 Uiso 0.38 1 calc PR I 2 H42H H 0.5897 0.7930 0.8207 0.030 Uiso 0.38 1 calc PR I 2 C43J C 0.6147(15) 0.9057(9) 0.8027(6) 0.0253(8) Uani 0.38 1 d PD I 2 H43G H 0.6263 0.9332 0.7765 0.030 Uiso 0.38 1 calc PR I 2 H43H H 0.5416 0.9267 0.8151 0.030 Uiso 0.38 1 calc PR I 2 C44J C 0.7125(14) 0.9228(7) 0.8297(5) 0.0240(9) Uani 0.38 1 d PD I 2 H44G H 0.7847 0.8958 0.8198 0.029 Uiso 0.38 1 calc PR I 2 H44H H 0.6952 0.9039 0.8575 0.029 Uiso 0.38 1 calc PR I 2 C45J C 0.7284(15) 1.0125(9) 0.8296(5) 0.0275(10) Uani 0.38 1 d P I 2 H45G H 0.7416 1.0313 0.8015 0.033 Uiso 0.38 1 calc PR I 2 H45H H 0.6568 1.0389 0.8403 0.033 Uiso 0.38 1 calc PR I 2 C46J C 0.8256(13) 1.0320(11) 0.8539(5) 0.0342(12) Uani 0.38 1 d PD I 2 H46J H 0.8223 1.0036 0.8798 0.051 Uiso 0.38 1 calc PR I 2 H46K H 0.8213 1.0875 0.8587 0.051 Uiso 0.38 1 calc PR I 2 H46L H 0.8983 1.0179 0.8395 0.051 Uiso 0.38 1 calc PR I 2 O8I O -0.18339(12) 0.71031(9) 0.74861(5) 0.0338(3) Uani 1 1 d D F 1 C47I C -0.08546(17) 0.72601(11) 0.73855(6) 0.0248(4) Uani 1 1 d D F 1 C48I C -0.04773(18) 0.80752(11) 0.74079(6) 0.0278(4) Uani 1 1 d D F 1 H48C H -0.1165 0.8430 0.7446 0.033 Uiso 1 1 calc R F 1 H48D H -0.0084 0.8221 0.7150 0.033 Uiso 1 1 calc R F 1 C49I C 0.0338(2) 0.81636(12) 0.77545(7) 0.0383(5) Uani 1 1 d D F 1 H49C H -0.0013 0.7942 0.8004 0.046 Uiso 1 1 calc R F 1 H49D H 0.1069 0.7863 0.7696 0.046 Uiso 1 1 calc R F 1 C50I C 0.06070(18) 0.89902(12) 0.78269(7) 0.0298(4) Uani 1 1 d D F 1 H50C H 0.0935 0.9215 0.7574 0.036 Uiso 1 1 calc R F 1 H50D H -0.0123 0.9286 0.7892 0.036 Uiso 1 1 calc R F 1 C51I C 0.1436(3) 0.90881(14) 0.81604(8) 0.0480(6) Uani 1 1 d D F 1 H51C H 0.1144 0.8817 0.8406 0.058 Uiso 1 1 calc R F 1 H51D H 0.2189 0.8834 0.8082 0.058 Uiso 1 1 calc R F 1 C52I C 0.1626(2) 0.99017(15) 0.82621(8) 0.0459(6) Uani 1 1 d D F 1 H52D H 0.1858 1.0188 0.8017 0.069 Uiso 1 1 calc R F 1 H52E H 0.2234 0.9911 0.8460 0.069 Uiso 1 1 calc R F 1 H52F H 0.0909 1.0141 0.8376 0.069 Uiso 1 1 calc R F 1 O1Q O 0.55144(12) 0.13006(8) 0.95973(4) 0.0261(3) Uani 1 1 d . J 1 H1Q H 0.5436 0.1626 0.9407 0.031 Uiso 1 1 calc R J 1 O2Q O 0.54696(13) 0.23600(8) 0.89982(4) 0.0263(3) Uani 1 1 d . J 1 H2Q H 0.608(4) 0.248(3) 0.9035(14) 0.129(18) Uiso 1 1 d . K 1 O3Q O 0.76770(12) 0.26134(8) 0.91258(4) 0.0276(3) Uani 1 1 d . J 1 H3Q H 0.7777 0.2291 0.9316 0.033 Uiso 1 1 calc R J 1 O4Q O 0.77252(12) 0.15855(8) 0.97350(4) 0.0278(3) Uani 1 1 d . J 1 H4Q H 0.7037 0.1458 0.9741 0.033 Uiso 1 1 calc R J 1 C1Q C 0.81019(16) 0.02162(11) 0.97512(5) 0.0208(4) Uani 1 1 d . J 1 C2Q C 0.69268(16) 0.00770(11) 0.99432(5) 0.0224(4) Uani 1 1 d . J 1 H2Q1 H 0.6670 0.0525 1.0108 0.027 Uiso 1 1 calc R J 1 H2Q2 H 0.6986 -0.0384 1.0125 0.027 Uiso 1 1 calc R J 1 C3Q C 0.60398(15) -0.00430(11) 0.96273(5) 0.0206(4) Uani 1 1 d . J 1 C4Q C 0.58824(16) -0.07755(11) 0.94879(6) 0.0234(4) Uani 1 1 d . J 1 H4Q1 H 0.6325 -0.1201 0.9598 0.028 Uiso 1 1 calc R J 1 C5Q C 0.50940(16) -0.09064(10) 0.91912(6) 0.0221(4) Uani 1 1 d D J 1 C6Q C 0.44475(15) -0.02810(10) 0.90306(5) 0.0205(4) Uani 1 1 d . J 1 H6Q H 0.3898 -0.0366 0.8832 0.025 Uiso 1 1 calc R J 1 C7Q C 0.45896(15) 0.04670(10) 0.91549(5) 0.0190(3) Uani 1 1 d . J 1 C8Q C 0.39167(15) 0.11395(10) 0.89583(5) 0.0203(3) Uani 1 1 d . J 1 H8Q1 H 0.3767 0.1550 0.9158 0.024 Uiso 1 1 calc R J 1 H8Q2 H 0.3163 0.0967 0.8874 0.024 Uiso 1 1 calc R J 1 C9Q C 0.45652(15) 0.14656(10) 0.85927(5) 0.0194(3) Uani 1 1 d . J 1 C10Q C 0.44098(16) 0.11741(11) 0.82121(5) 0.0215(4) Uani 1 1 d . J 1 H10Q H 0.3855 0.0798 0.8182 0.026 Uiso 1 1 calc R J 1 C11Q C 0.50480(17) 0.14209(11) 0.78743(5) 0.0243(4) Uani 1 1 d D J 1 C12Q C 0.58443(16) 0.19844(11) 0.79218(6) 0.0247(4) Uani 1 1 d . J 1 H12Q H 0.6288 0.2151 0.7694 0.030 Uiso 1 1 calc R J 1 C13Q C 0.60067(16) 0.23084(10) 0.82920(6) 0.0222(4) Uani 1 1 d . J 1 C14Q C 0.68784(16) 0.29235(11) 0.83299(6) 0.0243(4) Uani 1 1 d . J 1 H14E H 0.6908 0.3235 0.8076 0.029 Uiso 1 1 calc R J 1 H14F H 0.6617 0.3272 0.8550 0.029 Uiso 1 1 calc R J 1 C15Q C 0.80813(16) 0.25924(10) 0.84171(6) 0.0219(4) Uani 1 1 d . J 1 C16Q C 0.88647(17) 0.24359(10) 0.81031(6) 0.0237(4) Uani 1 1 d . J 1 H16Q H 0.8640 0.2542 0.7834 0.028 Uiso 1 1 calc R J 1 C17Q C 0.99774(16) 0.21260(10) 0.81720(6) 0.0236(4) Uani 1 1 d D J 1 C18Q C 1.02853(16) 0.19569(10) 0.85692(6) 0.0240(4) Uani 1 1 d . J 1 H18Q H 1.1036 0.1740 0.8619 0.029 Uiso 1 1 calc R J 1 C19Q C 0.95224(16) 0.20977(10) 0.88930(6) 0.0229(4) Uani 1 1 d . J 1 C20Q C 0.98652(17) 0.18775(11) 0.93203(6) 0.0258(4) Uani 1 1 d . J 1 H20E H 1.0712 0.1899 0.9339 0.031 Uiso 1 1 calc R J 1 H20F H 0.9503 0.2259 0.9508 0.031 Uiso 1 1 calc R J 1 C21Q C 0.95102(16) 0.10780(11) 0.94507(5) 0.0222(4) Uani 1 1 d . J 1 C22Q C 1.02401(16) 0.04414(11) 0.93715(5) 0.0233(4) Uani 1 1 d . J 1 H22Q H 1.0971 0.0515 0.9244 0.028 Uiso 1 1 calc R J 1 C23Q C 0.99303(16) -0.03037(11) 0.94744(5) 0.0222(4) Uani 1 1 d D J 1 C24Q C 0.88613(16) -0.04053(11) 0.96638(5) 0.0217(4) Uani 1 1 d . J 1 H24Q H 0.8645 -0.0912 0.9735 0.026 Uiso 1 1 calc R J 1 C25Q C 0.53852(15) 0.05722(10) 0.94556(5) 0.0196(3) Uani 1 1 d . J 1 C26Q C 0.53568(15) 0.20390(10) 0.86261(6) 0.0207(4) Uani 1 1 d . J 1 C27Q C 0.84249(16) 0.24314(10) 0.88111(6) 0.0222(4) Uani 1 1 d . J 1 C28Q C 0.84429(16) 0.09552(11) 0.96439(5) 0.0220(4) Uani 1 1 d . J 1 O5Q O 0.57302(17) -0.22073(10) 0.91429(7) 0.0463(5) Uani 0.94 1 d PD J 1 C29Q C 0.4990(2) -0.17076(12) 0.90512(7) 0.0275(6) Uani 0.94 1 d PD J 1 C30Q C 0.3989(3) -0.18985(16) 0.88030(9) 0.0251(7) Uani 0.94 1 d PD J 1 H30G H 0.4022 -0.1602 0.8544 0.030 Uiso 0.94 1 calc PR J 1 H30H H 0.3262 -0.1738 0.8948 0.030 Uiso 0.94 1 calc PR J 1 C31Q C 0.39773(18) -0.27537(15) 0.87157(10) 0.0255(5) Uani 0.94 1 d PD J 1 H31G H 0.4694 -0.2909 0.8563 0.031 Uiso 0.94 1 calc PR J 1 H31H H 0.3975 -0.3050 0.8975 0.031 Uiso 0.94 1 calc PR J 1 C32Q C 0.2951(2) -0.29648(12) 0.84775(9) 0.0265(5) Uani 0.94 1 d PD J 1 H32G H 0.2963 -0.2680 0.8215 0.032 Uiso 0.94 1 calc PR J 1 H32H H 0.2232 -0.2800 0.8627 0.032 Uiso 0.94 1 calc PR J 1 C33Q C 0.2937(2) -0.38239(13) 0.84016(8) 0.0300(5) Uani 0.94 1 d PD J 1 H33G H 0.3683 -0.3995 0.8273 0.036 Uiso 0.94 1 calc PR J 1 H33H H 0.2866 -0.4103 0.8664 0.036 Uiso 0.94 1 calc PR J 1 C34Q C 0.1978(3) -0.40426(15) 0.81393(10) 0.0441(7) Uani 0.94 1 d PD J 1 H34J H 0.1236 -0.3850 0.8256 0.066 Uiso 0.94 1 calc PR J 1 H34K H 0.1984 -0.4605 0.8123 0.066 Uiso 0.94 1 calc PR J 1 H34L H 0.2089 -0.3815 0.7868 0.066 Uiso 0.94 1 calc PR J 1 O5R O 0.518(3) -0.2244(14) 0.9365(10) 0.0463(5) Uani 0.06 1 d PD L 2 C29R C 0.4843(19) -0.1759(10) 0.9146(13) 0.0275(6) Uani 0.06 1 d PD L 2 C30R C 0.388(5) -0.192(2) 0.8865(18) 0.0251(7) Uani 0.06 1 d PD L 2 H30I H 0.3150 -0.1742 0.9000 0.030 Uiso 0.06 1 calc PR L 2 H30J H 0.3986 -0.1590 0.8622 0.030 Uiso 0.06 1 calc PR L 2 C31R C 0.370(4) -0.271(2) 0.8720(17) 0.0255(5) Uani 0.06 1 d PD L 2 H31I H 0.3543 -0.3048 0.8960 0.031 Uiso 0.06 1 calc PR L 2 H31J H 0.4439 -0.2913 0.8595 0.031 Uiso 0.06 1 calc PR L 2 C32R C 0.277(4) -0.2814(19) 0.8425(16) 0.0265(5) Uani 0.06 1 d PD L 2 H32I H 0.2906 -0.2486 0.8182 0.032 Uiso 0.06 1 calc PR L 2 H32J H 0.2013 -0.2646 0.8548 0.032 Uiso 0.06 1 calc PR L 2 C33R C 0.273(3) -0.3645(18) 0.8304(13) 0.0300(5) Uani 0.06 1 d PD L 2 H33I H 0.3431 -0.3776 0.8135 0.036 Uiso 0.06 1 calc PR L 2 H33J H 0.2770 -0.3978 0.8551 0.036 Uiso 0.06 1 calc PR L 2 C34R C 0.170(4) -0.383(3) 0.8079(17) 0.0441(7) Uani 0.06 1 d PD L 2 H34M H 0.1078 -0.3435 0.8132 0.066 Uiso 0.06 1 calc PR L 2 H34N H 0.1442 -0.4334 0.8167 0.066 Uiso 0.06 1 calc PR L 2 H34O H 0.1889 -0.3830 0.7789 0.066 Uiso 0.06 1 calc PR L 2 O6Q O 0.56645(18) 0.11943(14) 0.71973(6) 0.0453(6) Uani 0.85 1 d PD J 1 C35Q C 0.4932(8) 0.1087(6) 0.7464(2) 0.0315(7) Uani 0.85 1 d PD J 1 C36Q C 0.3973(3) 0.05445(19) 0.74123(11) 0.0263(8) Uani 0.85 1 d PD J 1 H36I H 0.3230 0.0821 0.7482 0.032 Uiso 0.85 1 calc PR J 1 H36J H 0.4077 0.0108 0.7608 0.032 Uiso 0.85 1 calc PR J 1 C37Q C 0.3892(4) 0.02184(16) 0.69916(11) 0.0283(7) Uani 0.85 1 d PD J 1 H37I H 0.4596 -0.0106 0.6928 0.034 Uiso 0.85 1 calc PR J 1 H37J H 0.3842 0.0647 0.6789 0.034 Uiso 0.85 1 calc PR J 1 C38Q C 0.2829(5) -0.0265(3) 0.69674(13) 0.0308(7) Uani 0.85 1 d PD J 1 H38I H 0.2807 -0.0625 0.7204 0.037 Uiso 0.85 1 calc PR J 1 H38J H 0.2127 0.0082 0.6983 0.037 Uiso 0.85 1 calc PR J 1 C39Q C 0.2807(6) -0.0730(2) 0.65826(14) 0.0343(8) Uani 0.85 1 d PD J 1 H39I H 0.3541 -0.1042 0.6555 0.041 Uiso 0.85 1 calc PR J 1 H39J H 0.2175 -0.1091 0.6611 0.041 Uiso 0.85 1 calc PR J 1 C40Q C 0.2641(5) -0.0247(2) 0.62001(14) 0.0383(8) Uani 0.85 1 d PD J 1 H40M H 0.1909 0.0059 0.6221 0.057 Uiso 0.85 1 calc PR J 1 H40N H 0.2628 -0.0585 0.5969 0.057 Uiso 0.85 1 calc PR J 1 H40O H 0.3278 0.0100 0.6163 0.057 Uiso 0.85 1 calc PR J 1 O6R O 0.5229(12) 0.1503(8) 0.7170(4) 0.0453(6) Uani 0.15 1 d PD M 2 C35R C 0.494(5) 0.104(3) 0.7476(14) 0.0315(7) Uani 0.15 1 d P M 2 C36R C 0.386(2) 0.0677(16) 0.7387(7) 0.0263(8) Uani 0.15 1 d PD M 2 H36K H 0.3198 0.1053 0.7432 0.032 Uiso 0.15 1 calc PR M 2 H36L H 0.3754 0.0234 0.7576 0.032 Uiso 0.15 1 calc PR M 2 C37R C 0.384(2) 0.0399(14) 0.6958(7) 0.0283(7) Uani 0.15 1 d PD M 2 H37K H 0.3665 0.0841 0.6772 0.034 Uiso 0.15 1 calc PR M 2 H37L H 0.4603 0.0164 0.6880 0.034 Uiso 0.15 1 calc PR M 2 C38R C 0.294(3) -0.018(2) 0.6927(8) 0.0308(7) Uani 0.15 1 d PD M 2 H38K H 0.2186 0.0085 0.6993 0.037 Uiso 0.15 1 calc PR M 2 H38L H 0.3081 -0.0575 0.7143 0.037 Uiso 0.15 1 calc PR M 2 C39R C 0.281(4) -0.0602(16) 0.6543(8) 0.0343(8) Uani 0.15 1 d PD M 2 H39K H 0.2212 -0.0985 0.6588 0.041 Uiso 0.15 1 calc PR M 2 H39L H 0.3547 -0.0889 0.6476 0.041 Uiso 0.15 1 calc PR M 2 C40R C 0.248(3) -0.0087(19) 0.6189(9) 0.0383(8) Uani 0.15 1 d PD M 2 H40P H 0.1684 0.0114 0.6227 0.057 Uiso 0.15 1 calc PR M 2 H40Q H 0.2555 -0.0383 0.5941 0.057 Uiso 0.15 1 calc PR M 2 H40R H 0.2998 0.0343 0.6168 0.057 Uiso 0.15 1 calc PR M 2 O7Q O 1.1889(5) 0.1793(4) 0.7916(3) 0.0320(9) Uani 0.61 1 d PD J 1 C41Q C 1.0891(6) 0.2017(6) 0.7850(2) 0.0241(10) Uani 0.61 1 d PD J 1 C42Q C 1.0561(9) 0.2168(7) 0.7416(2) 0.0313(9) Uani 0.61 1 d PD J 1 H42I H 1.0299 0.2717 0.7384 0.038 Uiso 0.61 1 calc PR J 1 H42J H 0.9898 0.1854 0.7360 0.038 Uiso 0.61 1 calc PR J 1 C43Q C 1.1512(9) 0.1993(6) 0.7102(3) 0.0389(13) Uani 0.61 1 d PD J 1 H43I H 1.1598 0.1430 0.7063 0.047 Uiso 0.61 1 calc PR J 1 H43J H 1.2252 0.2168 0.7197 0.047 Uiso 0.61 1 calc PR J 1 C44Q C 1.1232(10) 0.2399(8) 0.6700(3) 0.0586(15) Uani 0.61 1 d PD J 1 H44I H 1.1212 0.2965 0.6728 0.070 Uiso 0.61 1 calc PR J 1 H44J H 1.0474 0.2251 0.6607 0.070 Uiso 0.61 1 calc PR J 1 C45Q C 1.2231(5) 0.2125(4) 0.63936(16) 0.0617(14) Uani 0.61 1 d PD J 1 H45I H 1.2987 0.2229 0.6506 0.074 Uiso 0.61 1 calc PR J 1 H45J H 1.2207 0.1562 0.6358 0.074 Uiso 0.61 1 calc PR J 1 C46Q C 1.2115(6) 0.2528(4) 0.59972(16) 0.0784(15) Uani 0.61 1 d PD J 1 H46M H 1.1310 0.2533 0.5917 0.118 Uiso 0.61 1 calc PR J 1 H46N H 1.2608 0.2259 0.5795 0.118 Uiso 0.61 1 calc PR J 1 H46O H 1.2351 0.3059 0.6017 0.118 Uiso 0.61 1 calc PR J 1 O7R O 1.1720(9) 0.1677(7) 0.7908(4) 0.0320(9) Uani 0.39 1 d PD N 2 C41R C 1.0770(11) 0.1954(10) 0.7816(4) 0.0241(10) Uani 0.39 1 d PD N 2 C42R C 1.0423(15) 0.2232(12) 0.7400(4) 0.0313(9) Uani 0.39 1 d PD N 2 H42K H 0.9734 0.1960 0.7325 0.038 Uiso 0.39 1 calc PR N 2 H42L H 1.0200 0.2789 0.7409 0.038 Uiso 0.39 1 calc PR N 2 C43R C 1.1349(15) 0.2110(11) 0.7075(4) 0.0389(13) Uani 0.39 1 d PD N 2 H43K H 1.2042 0.2366 0.7159 0.047 Uiso 0.39 1 calc PR N 2 H43L H 1.1556 0.1550 0.7067 0.047 Uiso 0.39 1 calc PR N 2 C44R C 1.1099(16) 0.2383(14) 0.6652(5) 0.0586(15) Uani 0.39 1 d PD N 2 H44K H 1.0437 0.2088 0.6573 0.070 Uiso 0.39 1 calc PR N 2 H44L H 1.0797 0.2924 0.6677 0.070 Uiso 0.39 1 calc PR N 2 C45R C 1.1851(9) 0.2389(6) 0.6309(3) 0.0617(14) Uani 0.39 1 d P N 2 H45K H 1.1418 0.2561 0.6067 0.074 Uiso 0.39 1 calc PR N 2 H45L H 1.2185 0.1861 0.6262 0.074 Uiso 0.39 1 calc PR N 2 C46R C 1.2821(8) 0.2937(5) 0.6375(3) 0.0784(15) Uani 0.39 1 d PD N 2 H46P H 1.2485 0.3441 0.6455 0.118 Uiso 0.39 1 calc PR N 2 H46Q H 1.3280 0.2996 0.6124 0.118 Uiso 0.39 1 calc PR N 2 H46R H 1.3318 0.2723 0.6588 0.118 Uiso 0.39 1 calc PR N 2 O8Q O 1.17531(12) -0.08403(9) 0.92755(5) 0.0343(3) Uani 1 1 d D J 1 C47Q C 1.07627(17) -0.09587(12) 0.93777(6) 0.0264(4) Uani 1 1 d D J 1 C48Q C 1.03500(19) -0.17702(12) 0.93900(7) 0.0329(5) Uani 1 1 d D J 1 H48E H 1.0015 -0.1885 0.9662 0.039 Uiso 1 1 calc R J 1 H48F H 1.1018 -0.2138 0.9343 0.039 Uiso 1 1 calc R J 1 C49Q C 0.9439(2) -0.18885(14) 0.90712(8) 0.0466(6) Uani 1 1 d D J 1 H49E H 0.8674 -0.1705 0.9181 0.056 Uiso 1 1 calc R J 1 H49F H 0.9618 -0.1564 0.8830 0.056 Uiso 1 1 calc R J 1 C50Q C 0.9363(2) -0.27039(13) 0.89437(8) 0.0386(5) Uani 1 1 d D J 1 H50E H 0.9243 -0.3034 0.9187 0.046 Uiso 1 1 calc R J 1 H50F H 1.0110 -0.2875 0.8815 0.046 Uiso 1 1 calc R J 1 C51Q C 0.8403(2) -0.28282(14) 0.86519(8) 0.0450(6) Uani 1 1 d D J 1 H51E H 0.7650 -0.2758 0.8798 0.054 Uiso 1 1 calc R J 1 H51F H 0.8430 -0.2429 0.8434 0.054 Uiso 1 1 calc R J 1 C52Q C 0.8473(3) -0.36037(16) 0.84661(9) 0.0537(7) Uani 1 1 d D J 1 H52G H 0.9196 -0.3668 0.8307 0.081 Uiso 1 1 calc R J 1 H52H H 0.7819 -0.3648 0.8290 0.081 Uiso 1 1 calc R J 1 H52I H 0.8451 -0.4004 0.8679 0.081 Uiso 1 1 calc R J 1 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 0.0330(8) 0.0261(7) 0.0233(7) -0.0052(5) 0.0018(6) 0.0003(6) O2 0.0291(8) 0.0339(8) 0.0283(7) -0.0050(6) -0.0007(6) 0.0077(6) O3 0.0303(8) 0.0298(8) 0.0392(8) 0.0008(6) 0.0048(6) 0.0013(6) O4 0.0258(7) 0.0306(7) 0.0280(7) -0.0083(6) -0.0020(6) -0.0016(6) C1 0.0164(8) 0.0208(8) 0.0264(9) -0.0009(7) -0.0004(7) 0.0021(7) C2 0.0177(9) 0.0228(9) 0.0248(9) -0.0043(7) 0.0017(7) -0.0001(7) C3 0.0208(9) 0.0224(8) 0.0199(8) -0.0024(7) 0.0057(7) -0.0009(7) C4 0.0236(9) 0.0254(9) 0.0205(8) -0.0032(7) 0.0052(7) -0.0015(7) C5 0.0315(11) 0.0235(9) 0.0248(9) -0.0027(7) 0.0079(8) 0.0012(8) C6 0.0308(11) 0.0256(9) 0.0271(10) 0.0010(8) 0.0073(8) 0.0048(8) C7 0.0241(9) 0.0290(9) 0.0195(8) 0.0018(7) 0.0071(7) 0.0019(7) C8 0.0262(10) 0.0328(10) 0.0209(9) 0.0029(8) 0.0038(7) 0.0053(8) C9 0.0240(10) 0.0343(10) 0.0171(8) 0.0025(7) 0.0003(7) 0.0055(8) C10 0.0265(10) 0.0325(10) 0.0199(9) 0.0006(8) -0.0026(7) 0.0063(8) C11 0.0233(10) 0.0350(10) 0.0196(8) -0.0027(8) -0.0038(7) 0.0087(8) C12 0.0207(9) 0.0434(12) 0.0219(9) 0.0035(8) -0.0036(7) 0.0045(8) C13 0.0220(9) 0.0358(10) 0.0203(9) 0.0027(8) -0.0039(7) 0.0029(8) C14 0.0220(10) 0.0363(11) 0.0317(10) 0.0025(9) -0.0062(8) -0.0014(8) C15 0.0214(9) 0.0257(9) 0.0342(10) 0.0020(8) -0.0062(8) -0.0029(7) C16 0.0188(9) 0.0257(9) 0.0384(11) 0.0042(8) -0.0038(8) -0.0016(7) C17 0.0196(9) 0.0218(9) 0.0349(10) 0.0012(8) -0.0012(8) -0.0030(7) C18 0.0221(9) 0.0202(9) 0.0334(10) 0.0026(7) -0.0051(8) -0.0027(7) C19 0.0204(9) 0.0176(8) 0.0359(10) 0.0010(7) -0.0044(8) -0.0025(7) C20 0.0219(9) 0.0192(8) 0.0358(10) 0.0006(8) -0.0038(8) -0.0009(7) C21 0.0166(8) 0.0174(8) 0.0331(10) 0.0016(7) -0.0024(7) 0.0028(6) C22 0.0206(9) 0.0240(9) 0.0295(10) 0.0039(7) 0.0000(7) 0.0028(7) C23 0.0222(9) 0.0254(9) 0.0257(9) 0.0003(7) -0.0021(7) 0.0021(7) C24 0.0192(9) 0.0210(8) 0.0276(9) -0.0018(7) -0.0025(7) 0.0022(7) C25 0.0221(9) 0.0240(9) 0.0196(8) -0.0029(7) 0.0064(7) 0.0004(7) C26 0.0235(10) 0.0343(10) 0.0189(8) -0.0002(7) -0.0034(7) 0.0070(8) C27 0.0207(9) 0.0224(9) 0.0340(10) -0.0004(8) -0.0011(8) -0.0037(7) C28 0.0177(9) 0.0199(8) 0.0270(9) -0.0017(7) -0.0017(7) 0.0038(7) O5 0.053(3) 0.0306(10) 0.0658(17) -0.0126(10) -0.028(2) 0.017(2) C29 0.028(3) 0.0222(12) 0.0342(18) -0.0036(11) 0.0011(18) 0.0063(15) C30 0.027(2) 0.0218(15) 0.027(2) -0.0055(15) 0.0002(15) 0.0006(13) C31 0.035(3) 0.0225(16) 0.029(2) -0.0042(15) 0.0016(15) -0.0026(15) C32 0.0353(19) 0.0325(19) 0.032(2) -0.0080(13) -0.0038(14) -0.0062(14) C33 0.043(2) 0.047(2) 0.051(2) -0.0144(17) -0.0053(16) -0.0129(16) C34 0.053(2) 0.0363(19) 0.096(3) -0.010(2) -0.024(2) -0.0040(17) O5A 0.053(3) 0.0306(10) 0.0658(17) -0.0126(10) -0.028(2) 0.017(2) C29A 0.028(3) 0.0222(12) 0.0342(18) -0.0036(11) 0.0011(18) 0.0063(15) C30A 0.027(2) 0.0218(15) 0.027(2) -0.0055(15) 0.0002(15) 0.0006(13) C31A 0.035(3) 0.0225(16) 0.029(2) -0.0042(15) 0.0016(15) -0.0026(15) C32A 0.0353(19) 0.0325(19) 0.032(2) -0.0080(13) -0.0038(14) -0.0062(14) C33A 0.043(2) 0.047(2) 0.051(2) -0.0144(17) -0.0053(16) -0.0129(16) C34A 0.053(2) 0.0363(19) 0.096(3) -0.010(2) -0.024(2) -0.0040(17) O6 0.0231(8) 0.0514(16) 0.023(2) -0.0054(15) 0.0001(12) 0.0079(9) C35 0.0238(14) 0.0413(14) 0.0209(14) -0.0083(10) -0.0066(12) 0.0054(11) C36 0.0289(12) 0.035(2) 0.027(2) -0.0025(15) -0.0069(16) 0.0109(14) C37 0.0406(15) 0.0289(19) 0.0277(17) 0.0007(12) -0.0018(13) 0.0009(15) C38 0.055(2) 0.0331(17) 0.0422(18) -0.0012(12) -0.0013(16) -0.0056(15) C39 0.072(3) 0.048(2) 0.060(2) -0.0184(17) 0.005(2) -0.0224(19) C40 0.067(3) 0.075(3) 0.055(2) -0.006(2) -0.012(2) -0.009(2) O6A 0.0231(8) 0.0514(16) 0.023(2) -0.0054(15) 0.0001(12) 0.0079(9) C35A 0.0238(14) 0.0413(14) 0.0209(14) -0.0083(10) -0.0066(12) 0.0054(11) C36A 0.0289(12) 0.035(2) 0.027(2) -0.0025(15) -0.0069(16) 0.0109(14) C37A 0.0406(15) 0.0289(19) 0.0277(17) 0.0007(12) -0.0018(13) 0.0009(15) C38A 0.055(2) 0.0331(17) 0.0422(18) -0.0012(12) -0.0013(16) -0.0056(15) C39A 0.072(3) 0.048(2) 0.060(2) -0.0184(17) 0.005(2) -0.0224(19) C40A 0.067(3) 0.075(3) 0.055(2) -0.006(2) -0.012(2) -0.009(2) O7 0.0233(14) 0.042(3) 0.0430(12) 0.0036(16) 0.0012(11) 0.0023(14) C41 0.0227(14) 0.020(2) 0.0351(11) 0.0010(11) -0.0009(10) -0.0053(14) C42 0.0251(18) 0.024(3) 0.0356(11) -0.0025(14) -0.0029(11) -0.0071(16) C43 0.0380(13) 0.0393(12) 0.0368(13) -0.0016(11) -0.0011(10) 0.0026(10) C44 0.0483(15) 0.0348(17) 0.0380(13) 0.0004(11) -0.0014(11) 0.0046(12) C45 0.070(3) 0.047(4) 0.0402(15) 0.006(2) 0.0091(18) 0.006(3) C46 0.120(4) 0.082(5) 0.0441(18) 0.020(2) 0.017(2) 0.026(4) O7A 0.0233(14) 0.042(3) 0.0430(12) 0.0036(16) 0.0012(11) 0.0023(14) C41A 0.0227(14) 0.020(2) 0.0351(11) 0.0010(11) -0.0009(10) -0.0053(14) C42A 0.0251(18) 0.024(3) 0.0356(11) -0.0025(14) -0.0029(11) -0.0071(16) C43A 0.0380(13) 0.0393(12) 0.0368(13) -0.0016(11) -0.0011(10) 0.0026(10) C45A 0.070(3) 0.047(4) 0.0402(15) 0.006(2) 0.0091(18) 0.006(3) C46A 0.120(4) 0.082(5) 0.0441(18) 0.020(2) 0.017(2) 0.026(4) C44A 0.0483(15) 0.0348(17) 0.0380(13) 0.0004(11) -0.0014(11) 0.0046(12) O8 0.0961(16) 0.0748(14) 0.0303(9) 0.0019(9) 0.0025(10) -0.0494(12) C47 0.0375(12) 0.0379(11) 0.0255(10) -0.0003(9) -0.0027(9) -0.0033(9) C48 0.0389(12) 0.0401(12) 0.0265(10) -0.0035(9) -0.0045(9) -0.0035(10) C49 0.0554(16) 0.0594(16) 0.0298(11) -0.0101(11) 0.0005(11) -0.0200(13) C50 0.0424(13) 0.0405(12) 0.0338(11) -0.0081(10) -0.0031(10) -0.0068(10) C51 0.0522(16) 0.0584(16) 0.0387(13) -0.0145(12) 0.0013(11) -0.0167(13) C52 0.0523(16) 0.0564(16) 0.0441(14) -0.0189(12) -0.0086(12) -0.0057(13) O1I 0.0209(7) 0.0290(7) 0.0275(7) -0.0059(6) 0.0016(6) 0.0000(6) O2I 0.0293(7) 0.0242(7) 0.0216(6) -0.0041(5) -0.0027(5) 0.0016(6) O3I 0.0248(7) 0.0265(7) 0.0227(6) -0.0074(5) -0.0002(5) -0.0018(5) O4I 0.0265(7) 0.0244(7) 0.0249(7) -0.0027(5) 0.0006(5) 0.0044(5) C1I 0.0197(9) 0.0234(8) 0.0178(8) -0.0015(7) -0.0046(7) -0.0021(7) C2I 0.0188(9) 0.0251(9) 0.0231(9) -0.0017(7) -0.0044(7) -0.0028(7) C3I 0.0202(9) 0.0192(8) 0.0234(9) -0.0016(7) -0.0036(7) -0.0041(7) C4I 0.0170(8) 0.0193(8) 0.0289(9) 0.0006(7) -0.0023(7) -0.0022(7) C5I 0.0195(9) 0.0181(8) 0.0247(9) -0.0002(7) -0.0002(7) -0.0029(7) C6I 0.0219(9) 0.0189(8) 0.0243(9) 0.0011(7) -0.0031(7) -0.0016(7) C7I 0.0190(9) 0.0164(8) 0.0258(9) -0.0004(7) -0.0020(7) -0.0025(6) C8I 0.0206(9) 0.0188(8) 0.0260(9) 0.0014(7) -0.0022(7) 0.0007(7) C9I 0.0169(8) 0.0189(8) 0.0249(9) -0.0002(7) -0.0008(7) 0.0020(6) C10I 0.0247(10) 0.0285(10) 0.0233(9) 0.0005(7) 0.0008(7) -0.0034(8) C11I 0.0279(10) 0.0303(10) 0.0227(9) -0.0029(8) -0.0006(8) -0.0057(8) C12I 0.0199(9) 0.0243(9) 0.0245(9) -0.0029(7) -0.0027(7) -0.0014(7) C13I 0.0159(8) 0.0192(8) 0.0213(8) -0.0010(6) 0.0004(6) 0.0038(6) C14I 0.0161(8) 0.0242(9) 0.0206(8) -0.0029(7) 0.0006(6) -0.0001(7) C15I 0.0158(8) 0.0228(8) 0.0182(8) 0.0003(7) 0.0034(6) -0.0003(6) C16I 0.0176(8) 0.0258(9) 0.0195(8) -0.0019(7) 0.0016(7) -0.0025(7) C17I 0.0185(9) 0.0220(8) 0.0248(9) -0.0020(7) 0.0014(7) -0.0013(7) C18I 0.0188(9) 0.0234(9) 0.0230(9) 0.0014(7) 0.0005(7) 0.0010(7) C19I 0.0176(8) 0.0268(9) 0.0174(8) 0.0009(7) 0.0024(6) -0.0033(7) C20I 0.0210(9) 0.0265(9) 0.0183(8) 0.0010(7) -0.0008(7) -0.0008(7) C21I 0.0188(9) 0.0276(9) 0.0153(8) -0.0001(7) -0.0034(6) -0.0011(7) C22I 0.0224(9) 0.0244(9) 0.0182(8) -0.0004(7) -0.0041(7) -0.0015(7) C23I 0.0187(9) 0.0261(9) 0.0183(8) -0.0024(7) -0.0029(7) 0.0011(7) C24I 0.0175(9) 0.0279(9) 0.0193(8) -0.0015(7) -0.0027(7) -0.0010(7) C25I 0.0197(9) 0.0174(8) 0.0243(9) -0.0029(7) -0.0009(7) -0.0020(6) C26I 0.0181(8) 0.0199(8) 0.0216(8) -0.0024(7) -0.0018(7) 0.0045(6) C27I 0.0194(9) 0.0213(8) 0.0175(8) -0.0024(6) 0.0037(6) -0.0018(7) C28I 0.0187(8) 0.0248(9) 0.0157(8) -0.0026(7) -0.0022(6) 0.0018(7) O5I 0.0260(8) 0.0446(9) 0.0317(8) 0.0009(7) 0.0036(6) 0.0070(6) C29I 0.0249(10) 0.0227(9) 0.0271(9) -0.0001(7) 0.0015(7) -0.0009(7) C30I 0.0291(11) 0.0334(11) 0.0275(10) -0.0023(8) -0.0011(8) 0.0006(8) C31I 0.0342(12) 0.0370(11) 0.0283(10) -0.0038(9) 0.0002(9) -0.0001(9) C32I 0.0471(14) 0.0448(13) 0.0318(11) -0.0011(10) -0.0016(10) 0.0037(11) C33I 0.067(2) 0.082(2) 0.0327(13) -0.0030(13) 0.0035(13) 0.0240(17) C34I 0.072(2) 0.113(3) 0.071(2) 0.042(2) 0.0271(19) 0.014(2) O6I 0.0654(16) 0.0478(13) 0.0253(9) 0.0047(9) -0.0070(10) -0.0276(11) C35I 0.0255(17) 0.0314(17) 0.0221(10) -0.0027(12) -0.0020(11) -0.0003(11) C36I 0.0324(11) 0.0358(11) 0.0249(10) -0.0067(8) -0.0029(8) -0.0055(9) C37I 0.0416(15) 0.028(2) 0.0232(13) -0.0046(15) -0.0023(10) -0.0037(17) C38I 0.028(2) 0.0355(12) 0.0295(15) -0.0071(11) -0.0009(14) -0.0069(16) C39I 0.0519(18) 0.041(2) 0.0313(19) -0.0038(15) -0.0097(15) -0.0086(18) C40I 0.0501(16) 0.042(2) 0.043(3) -0.0100(17) -0.009(2) -0.0074(18) O6J 0.0654(16) 0.0478(13) 0.0253(9) 0.0047(9) -0.0070(10) -0.0276(11) C35J 0.0255(17) 0.0314(17) 0.0221(10) -0.0027(12) -0.0020(11) -0.0003(11) C36J 0.0324(11) 0.0358(11) 0.0249(10) -0.0067(8) -0.0029(8) -0.0055(9) C37J 0.0416(15) 0.028(2) 0.0232(13) -0.0046(15) -0.0023(10) -0.0037(17) C38J 0.028(2) 0.0355(12) 0.0295(15) -0.0071(11) -0.0009(14) -0.0069(16) C39J 0.0519(18) 0.041(2) 0.0313(19) -0.0038(15) -0.0097(15) -0.0086(18) C40J 0.0501(16) 0.042(2) 0.043(3) -0.0100(17) -0.009(2) -0.0074(18) O7I 0.0275(19) 0.0253(10) 0.052(3) -0.0052(15) -0.0052(16) 0.0015(12) C41I 0.0185(18) 0.0217(10) 0.029(2) -0.0025(11) 0.0028(15) -0.0016(10) C42I 0.0213(10) 0.0215(11) 0.0319(16) -0.0056(10) -0.0011(9) -0.0003(8) C43I 0.0242(14) 0.0207(12) 0.0314(18) -0.0034(12) -0.0038(11) -0.0012(10) C44I 0.0242(10) 0.0231(10) 0.025(2) -0.0043(13) -0.0013(14) -0.0013(8) C45I 0.0319(18) 0.0222(12) 0.029(2) -0.0010(14) -0.0025(16) -0.0042(11) C46I 0.0397(18) 0.0322(18) 0.032(3) -0.006(2) -0.005(2) -0.0072(13) O7J 0.0275(19) 0.0253(10) 0.052(3) -0.0052(15) -0.0052(16) 0.0015(12) C41J 0.0185(18) 0.0217(10) 0.029(2) -0.0025(11) 0.0028(15) -0.0016(10) C42J 0.0213(10) 0.0215(11) 0.0319(16) -0.0056(10) -0.0011(9) -0.0003(8) C43J 0.0242(14) 0.0207(12) 0.0314(18) -0.0034(12) -0.0038(11) -0.0012(10) C44J 0.0242(10) 0.0231(10) 0.025(2) -0.0043(13) -0.0013(14) -0.0013(8) C45J 0.0319(18) 0.0222(12) 0.029(2) -0.0010(14) -0.0025(16) -0.0042(11) C46J 0.0397(18) 0.0322(18) 0.032(3) -0.006(2) -0.005(2) -0.0072(13) O8I 0.0239(7) 0.0356(8) 0.0414(8) -0.0077(7) 0.0055(6) 0.0025(6) C47I 0.0230(9) 0.0284(9) 0.0227(9) -0.0043(7) -0.0028(7) 0.0032(7) C48I 0.0283(10) 0.0253(9) 0.0296(10) -0.0043(8) -0.0017(8) 0.0031(8) C49I 0.0560(15) 0.0265(10) 0.0334(11) -0.0048(9) -0.0146(10) -0.0028(10) C50I 0.0275(10) 0.0267(10) 0.0355(11) -0.0052(8) 0.0005(8) -0.0025(8) C51I 0.0631(17) 0.0352(12) 0.0470(14) -0.0072(11) -0.0191(13) -0.0025(12) C52I 0.0366(13) 0.0455(14) 0.0574(16) -0.0154(12) -0.0037(11) -0.0119(11) O1Q 0.0325(8) 0.0229(7) 0.0229(6) -0.0039(5) 0.0016(6) -0.0006(6) O2Q 0.0263(8) 0.0245(7) 0.0283(7) -0.0073(5) -0.0028(6) 0.0014(6) O3Q 0.0287(7) 0.0255(7) 0.0284(7) -0.0017(5) 0.0015(6) -0.0004(6) O4Q 0.0250(7) 0.0291(7) 0.0292(7) -0.0077(6) -0.0015(6) 0.0038(6) C1Q 0.0191(9) 0.0285(9) 0.0150(8) -0.0015(7) -0.0037(6) -0.0012(7) C2Q 0.0219(9) 0.0277(9) 0.0173(8) 0.0007(7) 0.0002(7) -0.0008(7) C3Q 0.0176(8) 0.0281(9) 0.0161(8) 0.0010(7) 0.0022(6) -0.0016(7) C4Q 0.0218(9) 0.0240(9) 0.0241(9) 0.0013(7) -0.0008(7) 0.0016(7) C5Q 0.0209(9) 0.0218(9) 0.0237(9) -0.0016(7) 0.0001(7) -0.0010(7) C6Q 0.0172(8) 0.0239(9) 0.0203(8) -0.0017(7) 0.0014(7) 0.0000(7) C7Q 0.0153(8) 0.0232(8) 0.0183(8) -0.0008(7) 0.0036(6) 0.0002(6) C8Q 0.0161(8) 0.0230(8) 0.0214(8) -0.0017(7) 0.0014(7) 0.0007(7) C9Q 0.0141(8) 0.0202(8) 0.0234(8) 0.0002(7) -0.0009(6) 0.0032(6) C10Q 0.0175(8) 0.0238(9) 0.0230(8) 0.0007(7) -0.0021(7) 0.0006(7) C11Q 0.0223(9) 0.0301(10) 0.0204(8) 0.0010(7) -0.0024(7) -0.0012(7) C12Q 0.0199(9) 0.0303(10) 0.0238(9) 0.0038(7) -0.0003(7) -0.0017(7) C13Q 0.0177(9) 0.0204(8) 0.0281(9) 0.0029(7) -0.0029(7) 0.0017(7) C14Q 0.0212(9) 0.0213(9) 0.0301(10) 0.0031(7) -0.0016(7) -0.0015(7) C15Q 0.0201(9) 0.0159(8) 0.0296(9) 0.0001(7) -0.0020(7) -0.0012(7) C16Q 0.0241(9) 0.0185(8) 0.0288(9) 0.0003(7) -0.0020(7) -0.0046(7) C17Q 0.0216(9) 0.0167(8) 0.0325(10) -0.0014(7) 0.0006(7) -0.0020(7) C18Q 0.0189(9) 0.0191(8) 0.0344(10) 0.0005(7) -0.0031(7) -0.0032(7) C19Q 0.0218(9) 0.0181(8) 0.0293(9) -0.0006(7) -0.0040(7) -0.0043(7) C20Q 0.0208(9) 0.0258(9) 0.0318(10) -0.0013(8) -0.0062(8) -0.0057(7) C21Q 0.0198(9) 0.0273(9) 0.0200(8) -0.0013(7) -0.0058(7) -0.0025(7) C22Q 0.0197(9) 0.0307(10) 0.0199(8) -0.0015(7) -0.0042(7) -0.0016(7) C23Q 0.0213(9) 0.0273(9) 0.0181(8) -0.0022(7) -0.0035(7) 0.0018(7) C24Q 0.0222(9) 0.0248(9) 0.0184(8) -0.0004(7) -0.0039(7) -0.0013(7) C25Q 0.0194(9) 0.0220(8) 0.0171(8) -0.0029(6) 0.0042(6) -0.0007(7) C26Q 0.0172(8) 0.0198(8) 0.0246(9) -0.0010(7) -0.0025(7) 0.0050(7) C27Q 0.0210(9) 0.0178(8) 0.0282(9) -0.0023(7) 0.0004(7) -0.0041(7) C28Q 0.0220(9) 0.0252(9) 0.0190(8) -0.0035(7) -0.0052(7) 0.0011(7) O5Q 0.0435(11) 0.0264(8) 0.0694(13) -0.0067(9) -0.0226(10) 0.0089(8) C29Q 0.0265(11) 0.0228(9) 0.0333(14) -0.0019(8) -0.0015(9) 0.0011(8) C30Q 0.0218(11) 0.0219(9) 0.0314(15) -0.0060(9) 0.0027(11) 0.0002(8) C31Q 0.0209(13) 0.0220(9) 0.0336(10) -0.0035(8) 0.0006(11) -0.0009(9) C32Q 0.0234(13) 0.0217(11) 0.0345(13) -0.0064(10) -0.0014(9) 0.0007(9) C33Q 0.0298(12) 0.0226(11) 0.0380(13) -0.0012(9) -0.0057(9) -0.0017(9) C34Q 0.0450(17) 0.0310(14) 0.0578(17) -0.0091(13) -0.0180(13) -0.0030(11) O5R 0.0435(11) 0.0264(8) 0.0694(13) -0.0067(9) -0.0226(10) 0.0089(8) C29R 0.0265(11) 0.0228(9) 0.0333(14) -0.0019(8) -0.0015(9) 0.0011(8) C30R 0.0218(11) 0.0219(9) 0.0314(15) -0.0060(9) 0.0027(11) 0.0002(8) C31R 0.0209(13) 0.0220(9) 0.0336(10) -0.0035(8) 0.0006(11) -0.0009(9) C32R 0.0234(13) 0.0217(11) 0.0345(13) -0.0064(10) -0.0014(9) 0.0007(9) C33R 0.0298(12) 0.0226(11) 0.0380(13) -0.0012(9) -0.0057(9) -0.0017(9) C34R 0.0450(17) 0.0310(14) 0.0578(17) -0.0091(13) -0.0180(13) -0.0030(11) O6Q 0.0400(13) 0.0711(17) 0.0261(9) -0.0093(10) 0.0074(9) -0.0180(10) C35Q 0.0311(11) 0.0420(17) 0.0220(11) -0.0016(10) -0.0011(9) -0.0072(11) C36Q 0.0278(13) 0.0296(18) 0.0216(10) -0.0034(11) -0.0025(9) 0.0013(12) C37Q 0.0328(12) 0.0282(18) 0.0239(12) -0.0047(12) -0.0014(9) 0.0004(14) C38Q 0.0340(18) 0.0346(18) 0.0240(13) -0.0066(12) -0.0004(11) -0.0023(11) C39Q 0.0410(13) 0.0305(19) 0.0319(15) -0.0068(13) -0.0084(12) 0.0006(17) C40Q 0.046(2) 0.037(2) 0.0312(12) -0.0076(14) -0.0101(12) 0.0085(16) O6R 0.0400(13) 0.0711(17) 0.0261(9) -0.0093(10) 0.0074(9) -0.0180(10) C35R 0.0311(11) 0.0420(17) 0.0220(11) -0.0016(10) -0.0011(9) -0.0072(11) C36R 0.0278(13) 0.0296(18) 0.0216(10) -0.0034(11) -0.0025(9) 0.0013(12) C37R 0.0328(12) 0.0282(18) 0.0239(12) -0.0047(12) -0.0014(9) 0.0004(14) C38R 0.0340(18) 0.0346(18) 0.0240(13) -0.0066(12) -0.0004(11) -0.0023(11) C39R 0.0410(13) 0.0305(19) 0.0319(15) -0.0068(13) -0.0084(12) 0.0006(17) C40R 0.046(2) 0.037(2) 0.0312(12) -0.0076(14) -0.0101(12) 0.0085(16) O7Q 0.0167(17) 0.032(2) 0.0476(10) -0.0024(14) 0.0055(13) -0.0041(14) C41Q 0.0222(17) 0.0171(16) 0.0338(15) -0.0059(12) -0.0016(12) -0.0071(14) C42Q 0.031(2) 0.029(2) 0.0338(12) -0.0047(11) 0.0029(13) 0.0041(16) C43Q 0.043(3) 0.030(3) 0.0426(17) -0.0107(16) 0.0083(17) 0.003(2) C44Q 0.102(3) 0.0350(14) 0.038(2) -0.0102(18) 0.023(2) -0.0108(19) C45Q 0.074(4) 0.069(4) 0.038(3) 0.000(2) 0.018(2) 0.017(3) C46Q 0.094(4) 0.079(3) 0.055(3) 0.024(2) 0.030(2) 0.024(3) O7R 0.0167(17) 0.032(2) 0.0476(10) -0.0024(14) 0.0055(13) -0.0041(14) C41R 0.0222(17) 0.0171(16) 0.0338(15) -0.0059(12) -0.0016(12) -0.0071(14) C42R 0.031(2) 0.029(2) 0.0338(12) -0.0047(11) 0.0029(13) 0.0041(16) C43R 0.043(3) 0.030(3) 0.0426(17) -0.0107(16) 0.0083(17) 0.003(2) C44R 0.102(3) 0.0350(14) 0.038(2) -0.0102(18) 0.023(2) -0.0108(19) C45R 0.074(4) 0.069(4) 0.038(3) 0.000(2) 0.018(2) 0.017(3) C46R 0.094(4) 0.079(3) 0.055(3) 0.024(2) 0.030(2) 0.024(3) O8Q 0.0217(7) 0.0414(9) 0.0396(8) -0.0092(7) 0.0020(6) 0.0038(6) C47Q 0.0254(10) 0.0308(10) 0.0227(9) -0.0049(8) -0.0046(7) 0.0046(8) C48Q 0.0323(11) 0.0276(10) 0.0382(11) -0.0046(9) -0.0029(9) 0.0053(8) C49Q 0.0533(16) 0.0353(12) 0.0525(15) -0.0128(11) -0.0178(12) 0.0007(11) C50Q 0.0353(12) 0.0314(11) 0.0492(14) -0.0083(10) 0.0015(10) -0.0013(9) C51Q 0.0463(15) 0.0369(12) 0.0528(15) -0.0119(11) -0.0063(12) -0.0021(11) C52Q 0.0520(17) 0.0460(15) 0.0647(18) -0.0132(13) -0.0035(14) -0.0096(12) _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 C25 1.375(2) . ? O2 C26 1.379(2) . ? O3 C27 1.374(2) . ? O4 C28 1.378(2) . ? C1 C24 1.390(3) . ? C1 C28 1.394(3) . ? C1 C2 1.525(3) . ? C2 C3 1.518(3) . ? C3 C4 1.391(3) . ? C3 C25 1.397(3) . ? C4 C5 1.396(3) . ? C5 C6 1.394(3) . ? C5 C29 1.509(7) . ? C6 C7 1.385(3) . ? C7 C25 1.399(3) . ? C7 C8 1.519(3) . ? C8 C9 1.520(3) . ? C9 C26 1.388(3) . ? C9 C10 1.389(3) . ? C10 C11 1.393(3) . ? C11 C12 1.394(3) . ? C11 C35 1.496(6) . ? C12 C13 1.384(3) . ? C13 C26 1.404(3) . ? C13 C14 1.510(3) . ? C14 C15 1.520(3) . ? C15 C16 1.384(3) . ? C15 C27 1.399(3) . ? C16 C17 1.392(3) . ? C17 C18 1.392(3) . ? C17 C41 1.506(7) . ? C18 C19 1.391(3) . ? C19 C27 1.391(3) . ? C19 C20 1.517(3) . ? C20 C21 1.519(3) . ? C21 C22 1.381(3) . ? C21 C28 1.400(3) . ? C22 C23 1.395(3) . ? C23 C24 1.396(3) . ? C23 C47 1.494(3) . ? O5 C29 1.226(7) . ? C29 C30 1.511(6) . ? C30 C31 1.527(6) . ? C31 C32 1.530(5) . ? C32 C33 1.530(5) . ? C33 C34 1.469(6) . ? O5A C29A 1.206(13) . ? C29A C30A 1.480(13) . ? C30A C31A 1.507(13) . ? C31A C32A 1.495(9) . ? C32A C33A 1.510(9) . ? C33A C34A 1.516(10) . ? O6 C35 1.234(6) . ? C35 C36 1.518(7) . ? C36 C37 1.547(5) . ? C37 C38 1.533(4) . ? C38 C39 1.532(5) . ? C39 C40 1.491(6) . ? O6A C35A 1.215(16) . ? C35A C36A 1.485(16) . ? C36A C37A 1.491(13) . ? C37A C38A 1.483(10) . ? C38A C39A 1.478(12) . ? C39A C40A 1.493(12) . ? O7 C41 1.229(8) . ? C41 C42 1.513(8) . ? C42 C43 1.520(9) . ? C43 C44 1.529(9) . ? C44 C45 1.517(9) . ? C45 C46 1.523(10) . ? O7A C41A 1.216(14) . ? C41A C42A 1.502(15) . ? C42A C43A 1.518(16) . ? C43A C44A 1.516(16) . ? C45A C46A 1.510(17) . ? C45A C44A 1.512(16) . ? O8 C47 1.219(3) . ? C47 C48 1.489(3) . ? C48 C49 1.523(3) . ? C49 C50 1.511(3) . ? C50 C51 1.526(3) . ? C51 C52 1.495(3) . ? O1I C25I 1.377(2) . ? O2I C26I 1.383(2) . ? O3I C27I 1.379(2) . ? O4I C28I 1.377(2) . ? C1I C24I 1.383(3) . ? C1I C28I 1.400(3) . ? C1I C2I 1.516(3) . ? C2I C3I 1.518(3) . ? C3I C4I 1.384(3) . ? C3I C25I 1.394(3) . ? C4I C5I 1.395(3) . ? C5I C6I 1.392(3) . ? C5I C29I 1.495(3) . ? C6I C7I 1.391(3) . ? C7I C25I 1.399(3) . ? C7I C8I 1.515(3) . ? C8I C9I 1.524(3) . ? C9I C10I 1.383(3) . ? C9I C26I 1.398(3) . ? C10I C11I 1.396(3) . ? C11I C12I 1.390(3) . ? C11I C35I 1.509(3) . ? C12I C13I 1.391(3) . ? C13I C26I 1.395(3) . ? C13I C14I 1.520(2) . ? C14I C15I 1.516(2) . ? C15I C16I 1.394(3) . ? C15I C27I 1.398(3) . ? C16I C17I 1.391(3) . ? C17I C18I 1.393(3) . ? C17I C41I 1.492(7) . ? C18I C19I 1.388(3) . ? C19I C27I 1.394(3) . ? C19I C20I 1.515(3) . ? C20I C21I 1.516(3) . ? C21I C22I 1.385(3) . ? C21I C28I 1.397(3) . ? C22I C23I 1.387(3) . ? C23I C24I 1.393(3) . ? C23I C47I 1.492(3) . ? O5I C29I 1.219(2) . ? C29I C30I 1.510(3) . ? C30I C31I 1.516(3) . ? C31I C32I 1.522(3) . ? C32I C33I 1.522(4) . ? C33I C34I 1.506(5) . ? O6I C35I 1.221(4) . ? C35I C36I 1.517(6) . ? C36I C37I 1.533(6) . ? C37I C38I 1.511(5) . ? C38I C39I 1.536(5) . ? C39I C40I 1.503(6) . ? O6J C35J 1.226(14) . ? C35J C36J 1.47(2) . ? C36J C37J 1.506(17) . ? C37J C38J 1.518(16) . ? C38J C39J 1.538(17) . ? C39J C40J 1.507(17) . ? O7I C41I 1.222(8) . ? C41I C42I 1.510(9) . ? C42I C43I 1.522(9) . ? C43I C44I 1.520(9) . ? C44I C45I 1.497(12) . ? C45I C46I 1.516(12) . ? O7J C41J 1.229(13) . ? C41J C42J 1.512(14) . ? C42J C43J 1.515(14) . ? C43J C44J 1.513(15) . ? C44J C45J 1.58(2) . ? C45J C46J 1.47(2) . ? O8I C47I 1.218(2) . ? C47I C48I 1.508(3) . ? C48I C49I 1.527(3) . ? C49I C50I 1.512(3) . ? C50I C51I 1.506(3) . ? C51I C52I 1.490(3) . ? O1Q C25Q 1.378(2) . ? O2Q C26Q 1.380(2) . ? O3Q C27Q 1.370(2) . ? O4Q C28Q 1.376(2) . ? C1Q C24Q 1.389(3) . ? C1Q C28Q 1.397(3) . ? C1Q C2Q 1.516(3) . ? C2Q C3Q 1.517(3) . ? C3Q C4Q 1.388(3) . ? C3Q C25Q 1.399(3) . ? C4Q C5Q 1.395(3) . ? C5Q C6Q 1.393(3) . ? C5Q C29Q 1.490(3) . ? C6Q C7Q 1.392(3) . ? C7Q C25Q 1.401(3) . ? C7Q C8Q 1.517(2) . ? C8Q C9Q 1.520(2) . ? C9Q C10Q 1.392(3) . ? C9Q C26Q 1.398(3) . ? C10Q C11Q 1.395(3) . ? C11Q C12Q 1.395(3) . ? C11Q C35Q 1.505(8) . ? C12Q C13Q 1.385(3) . ? C13Q C26Q 1.405(3) . ? C13Q C14Q 1.519(3) . ? C14Q C15Q 1.516(3) . ? C15Q C16Q 1.385(3) . ? C15Q C27Q 1.395(3) . ? C16Q C17Q 1.397(3) . ? C17Q C18Q 1.395(3) . ? C17Q C41Q 1.490(8) . ? C18Q C19Q 1.390(3) . ? C19Q C27Q 1.404(3) . ? C19Q C20Q 1.518(3) . ? C20Q C21Q 1.517(3) . ? C21Q C22Q 1.384(3) . ? C21Q C28Q 1.401(3) . ? C22Q C23Q 1.392(3) . ? C23Q C24Q 1.391(3) . ? C23Q C47Q 1.490(3) . ? O5Q C29Q 1.229(3) . ? C29Q C30Q 1.500(3) . ? C30Q C31Q 1.522(3) . ? C31Q C32Q 1.515(3) . ? C32Q C33Q 1.521(3) . ? C33Q C34Q 1.503(3) . ? O5R C29R 1.16(4) . ? C29R C30R 1.519(19) . ? C30R C31R 1.49(2) . ? C31R C32R 1.503(19) . ? C32R C33R 1.510(19) . ? C33R C34R 1.488(19) . ? O6Q C35Q 1.225(8) . ? C35Q C36Q 1.512(10) . ? C36Q C37Q 1.527(4) . ? C37Q C38Q 1.533(4) . ? C38Q C39Q 1.529(4) . ? C39Q C40Q 1.515(4) . ? O6R C35R 1.32(6) . ? C35R C36R 1.48(6) . ? C36R C37R 1.514(18) . ? C37R C38R 1.493(19) . ? C38R C39R 1.503(18) . ? C39R C40R 1.505(19) . ? O7Q C41Q 1.227(8) . ? C41Q C42Q 1.515(9) . ? C42Q C43Q 1.520(9) . ? C43Q C44Q 1.525(10) . ? C44Q C45Q 1.582(11) . ? C45Q C46Q 1.480(7) . ? O7R C41R 1.224(13) . ? C41R C42R 1.512(14) . ? C42R C43R 1.509(15) . ? C43R C44R 1.503(15) . ? C44R C45R 1.414(17) . ? C45R C46R 1.536(15) . ? O8Q C47Q 1.215(2) . ? C47Q C48Q 1.511(3) . ? C48Q C49Q 1.543(3) . ? C49Q C50Q 1.496(3) . ? C50Q C51Q 1.526(3) . ? C51Q C52Q 1.493(3) . ? 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 C24 C1 C28 118.09(17) . . ? C24 C1 C2 119.71(17) . . ? C28 C1 C2 122.18(17) . . ? C3 C2 C1 113.51(15) . . ? C4 C3 C25 118.14(17) . . ? C4 C3 C2 120.10(17) . . ? C25 C3 C2 121.75(16) . . ? C3 C4 C5 121.39(18) . . ? C6 C5 C4 118.58(18) . . ? C6 C5 C29 122.5(3) . . ? C4 C5 C29 118.9(3) . . ? C7 C6 C5 121.97(19) . . ? C6 C7 C25 117.88(18) . . ? C6 C7 C8 120.57(18) . . ? C25 C7 C8 121.53(18) . . ? C7 C8 C9 112.43(15) . . ? C26 C9 C10 118.04(18) . . ? C26 C9 C8 122.24(18) . . ? C10 C9 C8 119.72(19) . . ? C9 C10 C11 121.6(2) . . ? C10 C11 C12 118.69(18) . . ? C10 C11 C35 121.5(3) . . ? C12 C11 C35 119.8(3) . . ? C13 C12 C11 121.59(19) . . ? C12 C13 C26 117.90(19) . . ? C12 C13 C14 120.28(18) . . ? C26 C13 C14 121.81(18) . . ? C13 C14 C15 112.13(17) . . ? C16 C15 C27 118.21(18) . . ? C16 C15 C14 119.84(18) . . ? C27 C15 C14 121.90(18) . . ? C15 C16 C17 121.75(18) . . ? C18 C17 C16 118.34(18) . . ? C18 C17 C41 122.9(3) . . ? C16 C17 C41 118.7(3) . . ? C19 C18 C17 121.87(18) . . ? C27 C19 C18 117.95(18) . . ? C27 C19 C20 121.71(18) . . ? C18 C19 C20 120.28(18) . . ? C19 C20 C21 111.42(15) . . ? C22 C21 C28 117.54(17) . . ? C22 C21 C20 120.31(17) . . ? C28 C21 C20 122.12(17) . . ? C21 C22 C23 121.79(18) . . ? C22 C23 C24 119.09(18) . . ? C22 C23 C47 118.28(18) . . ? C24 C23 C47 122.62(18) . . ? C1 C24 C23 120.92(18) . . ? O1 C25 C3 119.83(16) . . ? O1 C25 C7 118.12(17) . . ? C3 C25 C7 122.01(17) . . ? O2 C26 C9 119.60(18) . . ? O2 C26 C13 118.22(19) . . ? C9 C26 C13 122.15(18) . . ? O3 C27 C19 118.47(18) . . ? O3 C27 C15 119.66(18) . . ? C19 C27 C15 121.87(19) . . ? O4 C28 C1 118.61(17) . . ? O4 C28 C21 118.83(17) . . ? C1 C28 C21 122.55(17) . . ? O5 C29 C5 118.3(5) . . ? O5 C29 C30 119.9(6) . . ? C5 C29 C30 121.8(4) . . ? C29 C30 C31 115.4(4) . . ? C30 C31 C32 111.5(3) . . ? C31 C32 C33 114.9(3) . . ? C34 C33 C32 114.4(4) . . ? O5A C29A C30A 124.9(12) . . ? C29A C30A C31A 111.4(9) . . ? C32A C31A C30A 113.9(7) . . ? C31A C32A C33A 112.9(7) . . ? C32A C33A C34A 114.5(7) . . ? O6 C35 C11 118.8(5) . . ? O6 C35 C36 119.2(6) . . ? C11 C35 C36 121.2(5) . . ? C35 C36 C37 111.0(4) . . ? C38 C37 C36 112.6(3) . . ? C39 C38 C37 114.7(3) . . ? C40 C39 C38 114.7(4) . . ? O6A C35A C36A 116.9(16) . . ? C35A C36A C37A 116.1(13) . . ? C38A C37A C36A 114.2(9) . . ? C39A C38A C37A 115.2(8) . . ? C38A C39A C40A 119.0(10) . . ? O7 C41 C17 120.2(7) . . ? O7 C41 C42 121.3(7) . . ? C17 C41 C42 118.5(6) . . ? C41 C42 C43 115.0(7) . . ? C42 C43 C44 112.7(8) . . ? C45 C44 C43 113.2(9) . . ? C44 C45 C46 112.2(11) . . ? O7A C41A C42A 120.0(13) . . ? C41A C42A C43A 113.0(13) . . ? C44A C43A C42A 113.2(16) . . ? C46A C45A C44A 113.2(19) . . ? C45A C44A C43A 113.9(17) . . ? O8 C47 C48 121.5(2) . . ? O8 C47 C23 119.5(2) . . ? C48 C47 C23 119.02(18) . . ? C47 C48 C49 112.64(19) . . ? C50 C49 C48 112.3(2) . . ? C49 C50 C51 112.7(2) . . ? C52 C51 C50 113.3(2) . . ? C24I C1I C28I 117.96(17) . . ? C24I C1I C2I 119.55(16) . . ? C28I C1I C2I 122.45(16) . . ? C1I C2I C3I 111.82(15) . . ? C4I C3I C25I 118.23(17) . . ? C4I C3I C2I 120.35(17) . . ? C25I C3I C2I 121.37(16) . . ? C3I C4I C5I 121.58(17) . . ? C6I C5I C4I 118.65(17) . . ? C6I C5I C29I 122.75(17) . . ? C4I C5I C29I 118.59(17) . . ? C7I C6I C5I 121.68(17) . . ? C6I C7I C25I 117.76(17) . . ? C6I C7I C8I 120.49(16) . . ? C25I C7I C8I 121.75(16) . . ? C7I C8I C9I 113.20(15) . . ? C10I C9I C26I 117.53(17) . . ? C10I C9I C8I 120.27(16) . . ? C26I C9I C8I 122.20(16) . . ? C9I C10I C11I 121.64(18) . . ? C12I C11I C10I 119.11(18) . . ? C12I C11I C35I 121.9(2) . . ? C10I C11I C35I 118.55(19) . . ? C11I C12I C13I 121.27(18) . . ? C12I C13I C26I 117.73(16) . . ? C12I C13I C14I 119.79(16) . . ? C26I C13I C14I 122.46(16) . . ? C15I C14I C13I 112.56(14) . . ? C16I C15I C27I 117.91(16) . . ? C16I C15I C14I 120.20(16) . . ? C27I C15I C14I 121.89(16) . . ? C17I C16I C15I 121.14(17) . . ? C16I C17I C18I 119.14(17) . . ? C16I C17I C41I 122.7(3) . . ? C18I C17I C41I 118.1(3) . . ? C19I C18I C17I 121.61(17) . . ? C18I C19I C27I 117.73(17) . . ? C18I C19I C20I 120.13(17) . . ? C27I C19I C20I 122.12(17) . . ? C19I C20I C21I 111.32(14) . . ? C22I C21I C28I 117.65(17) . . ? C22I C21I C20I 120.25(17) . . ? C28I C21I C20I 122.06(17) . . ? C21I C22I C23I 122.14(17) . . ? C22I C23I C24I 118.51(17) . . ? C22I C23I C47I 123.18(17) . . ? C24I C23I C47I 118.31(17) . . ? C1I C24I C23I 121.69(17) . . ? O1I C25I C3I 118.13(16) . . ? O1I C25I C7I 119.77(16) . . ? C3I C25I C7I 122.08(17) . . ? O2I C26I C13I 119.19(16) . . ? O2I C26I C9I 118.12(16) . . ? C13I C26I C9I 122.66(16) . . ? O3I C27I C19I 119.33(16) . . ? O3I C27I C15I 118.20(16) . . ? C19I C27I C15I 122.44(17) . . ? O4I C28I C21I 118.72(16) . . ? O4I C28I C1I 119.24(16) . . ? C21I C28I C1I 122.03(17) . . ? O5I C29I C5I 120.36(18) . . ? O5I C29I C30I 120.84(18) . . ? C5I C29I C30I 118.79(17) . . ? C29I C30I C31I 114.27(18) . . ? C30I C31I C32I 113.04(19) . . ? C31I C32I C33I 114.1(2) . . ? C34I C33I C32I 112.5(3) . . ? O6I C35I C11I 120.5(3) . . ? O6I C35I C36I 122.8(4) . . ? C11I C35I C36I 116.7(3) . . ? C35I C36I C37I 111.3(5) . . ? C38I C37I C36I 111.3(4) . . ? C37I C38I C39I 113.5(4) . . ? C40I C39I C38I 113.5(4) . . ? O6J C35J C36J 118.5(13) . . ? C35J C36J C37J 119.0(17) . . ? C36J C37J C38J 114.5(15) . . ? C37J C38J C39J 105.1(13) . . ? C40J C39J C38J 109.6(16) . . ? O7I C41I C17I 121.3(7) . . ? O7I C41I C42I 120.0(7) . . ? C17I C41I C42I 118.6(6) . . ? C41I C42I C43I 113.3(7) . . ? C44I C43I C42I 111.7(7) . . ? C45I C44I C43I 113.5(7) . . ? C44I C45I C46I 115.3(8) . . ? O7J C41J C42J 122.8(12) . . ? C41J C42J C43J 112.3(12) . . ? C44J C43J C42J 115.0(12) . . ? C43J C44J C45J 109.7(12) . . ? C46J C45J C44J 111.9(14) . . ? O8I C47I C23I 120.26(18) . . ? O8I C47I C48I 120.59(18) . . ? C23I C47I C48I 119.06(17) . . ? C47I C48I C49I 111.63(17) . . ? C50I C49I C48I 113.63(18) . . ? C51I C50I C49I 114.46(19) . . ? C52I C51I C50I 115.2(2) . . ? C24Q C1Q C28Q 117.98(17) . . ? C24Q C1Q C2Q 119.87(17) . . ? C28Q C1Q C2Q 122.11(17) . . ? C1Q C2Q C3Q 111.50(14) . . ? C4Q C3Q C25Q 117.57(17) . . ? C4Q C3Q C2Q 120.36(17) . . ? C25Q C3Q C2Q 122.03(17) . . ? C3Q C4Q C5Q 122.02(17) . . ? C6Q C5Q C4Q 118.79(17) . . ? C6Q C5Q C29Q 122.31(18) . . ? C4Q C5Q C29Q 118.89(17) . . ? C7Q C6Q C5Q 121.37(17) . . ? C6Q C7Q C25Q 117.98(16) . . ? C6Q C7Q C8Q 120.00(16) . . ? C25Q C7Q C8Q 122.00(16) . . ? C7Q C8Q C9Q 111.77(14) . . ? C10Q C9Q C26Q 117.96(17) . . ? C10Q C9Q C8Q 120.00(16) . . ? C26Q C9Q C8Q 122.00(16) . . ? C9Q C10Q C11Q 121.64(17) . . ? C10Q C11Q C12Q 118.59(17) . . ? C10Q C11Q C35Q 122.5(4) . . ? C12Q C11Q C35Q 118.9(4) . . ? C13Q C12Q C11Q 121.96(17) . . ? C12Q C13Q C26Q 117.79(17) . . ? C12Q C13Q C14Q 120.26(17) . . ? C26Q C13Q C14Q 121.95(17) . . ? C15Q C14Q C13Q 113.06(15) . . ? C16Q C15Q C27Q 118.38(17) . . ? C16Q C15Q C14Q 120.23(17) . . ? C27Q C15Q C14Q 121.39(17) . . ? C15Q C16Q C17Q 121.78(18) . . ? C18Q C17Q C16Q 118.38(18) . . ? C18Q C17Q C41Q 117.4(3) . . ? C16Q C17Q C41Q 124.1(3) . . ? C19Q C18Q C17Q 121.73(18) . . ? C18Q C19Q C27Q 118.02(18) . . ? C18Q C19Q C20Q 120.52(17) . . ? C27Q C19Q C20Q 121.45(17) . . ? C21Q C20Q C19Q 112.80(15) . . ? C22Q C21Q C28Q 118.05(18) . . ? C22Q C21Q C20Q 119.93(17) . . ? C28Q C21Q C20Q 122.01(17) . . ? C21Q C22Q C23Q 121.68(18) . . ? C24Q C23Q C22Q 118.78(17) . . ? C24Q C23Q C47Q 122.81(18) . . ? C22Q C23Q C47Q 118.42(17) . . ? C1Q C24Q C23Q 121.63(18) . . ? O1Q C25Q C3Q 118.20(16) . . ? O1Q C25Q C7Q 119.53(16) . . ? C3Q C25Q C7Q 122.25(17) . . ? O2Q C26Q C9Q 118.27(16) . . ? O2Q C26Q C13Q 119.68(17) . . ? C9Q C26Q C13Q 122.03(17) . . ? O3Q C27Q C15Q 119.08(17) . . ? O3Q C27Q C19Q 119.26(17) . . ? C15Q C27Q C19Q 121.66(17) . . ? O4Q C28Q C1Q 119.57(17) . . ? O4Q C28Q C21Q 118.53(17) . . ? C1Q C28Q C21Q 121.88(17) . . ? O5Q C29Q C5Q 119.2(2) . . ? O5Q C29Q C30Q 120.7(2) . . ? C5Q C29Q C30Q 120.1(2) . . ? C29Q C30Q C31Q 112.7(2) . . ? C32Q C31Q C30Q 113.6(2) . . ? C31Q C32Q C33Q 112.95(19) . . ? C34Q C33Q C32Q 114.1(2) . . ? O5R C29R C30R 119(3) . . ? C31R C30R C29R 122(3) . . ? C30R C31R C32R 119(3) . . ? C31R C32R C33R 111(2) . . ? C34R C33R C32R 115(3) . . ? O6Q C35Q C11Q 120.3(6) . . ? O6Q C35Q C36Q 121.8(6) . . ? C11Q C35Q C36Q 117.5(6) . . ? C35Q C36Q C37Q 115.7(4) . . ? C36Q C37Q C38Q 110.7(3) . . ? C39Q C38Q C37Q 113.7(4) . . ? C40Q C39Q C38Q 114.5(4) . . ? O6R C35R C36R 109(4) . . ? C35R C36R C37R 113(3) . . ? C38R C37R C36R 109.7(19) . . ? C37R C38R C39R 121(2) . . ? C38R C39R C40R 114(2) . . ? O7Q C41Q C17Q 123.8(7) . . ? O7Q C41Q C42Q 118.0(7) . . ? C17Q C41Q C42Q 118.1(6) . . ? C41Q C42Q C43Q 115.4(7) . . ? C42Q C43Q C44Q 110.6(7) . . ? C43Q C44Q C45Q 105.7(8) . . ? C46Q C45Q C44Q 111.3(6) . . ? O7R C41R C42R 126.0(13) . . ? C43R C42R C41R 114.5(12) . . ? C44R C43R C42R 118.6(13) . . ? C45R C44R C43R 128.7(14) . . ? C44R C45R C46R 109.5(12) . . ? O8Q C47Q C23Q 120.42(19) . . ? O8Q C47Q C48Q 120.20(18) . . ? C23Q C47Q C48Q 119.33(18) . . ? C47Q C48Q C49Q 112.35(18) . . ? C50Q C49Q C48Q 114.7(2) . . ? C49Q C50Q C51Q 114.6(2) . . ? C52Q C51Q C50Q 114.0(2) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 29.59 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.260 _refine_diff_density_min -0.640 _refine_diff_density_rms 0.064 # Attachment 'gena36_C6EtOH.cif' data_gena36 _database_code_depnum_ccdc_archive 'CCDC 632666' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common para-hexanoylcalix(4)arene _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H70 O9' _chemical_formula_weight 863.10 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 12.053(3) _cell_length_b 12.441(3) _cell_length_c 16.015(3) _cell_angle_alpha 91.504(3) _cell_angle_beta 99.841(3) _cell_angle_gamma 95.036(3) _cell_volume 2355.0(8) _cell_formula_units_Z 2 _cell_measurement_temperature 398(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.217 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 932 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71070 _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 28400 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0591 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 29.64 _reflns_number_total 12854 _reflns_number_gt 8734 _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^)+(0.1111P)^2^+1.6933P] 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 12854 _refine_ls_number_parameters 573 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1063 _refine_ls_R_factor_gt 0.0742 _refine_ls_wR_factor_ref 0.2260 _refine_ls_wR_factor_gt 0.2076 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.152 _refine_ls_shift/su_mean 0.007 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 0.03690(12) 0.93532(10) 0.35969(9) 0.0258(3) Uani 1 1 d . . . H1 H 0.0433 0.9602 0.3136 0.031 Uiso 1 1 calc R . . O2 O -0.17271(12) 0.97150(10) 0.38903(9) 0.0259(3) Uani 1 1 d . . . H2 H -0.1068 0.9629 0.3860 0.031 Uiso 1 1 calc R . . O3 O -0.20694(11) 1.02888(11) 0.22938(9) 0.0271(3) Uani 1 1 d . . . H3 H -0.2176 1.0227 0.2783 0.033 Uiso 1 1 calc R . . O4 O 0.00150(11) 1.01130(10) 0.20420(9) 0.0261(3) Uani 1 1 d . . . H4 H -0.0614 1.0326 0.2017 0.031 Uiso 1 1 calc R . . C1 C 0.07993(14) 0.85871(13) 0.15439(11) 0.0195(4) Uani 1 1 d . . . C2 C 0.16571(15) 0.85976(13) 0.23613(11) 0.0203(4) Uani 1 1 d . . . H2B H 0.2351 0.8346 0.2234 0.024 Uiso 1 1 calc R . . H2A H 0.1829 0.9334 0.2591 0.024 Uiso 1 1 calc R . . C3 C 0.12386(14) 0.78946(13) 0.30260(11) 0.0190(4) Uani 1 1 d . . . C4 C 0.14580(14) 0.68178(13) 0.30622(11) 0.0190(4) Uani 1 1 d . . . H4A H 0.1881 0.6540 0.2687 0.023 Uiso 1 1 calc R . . C5 C 0.10593(14) 0.61467(13) 0.36470(11) 0.0193(4) Uani 1 1 d . . . C6 C 0.04297(14) 0.65660(14) 0.42120(11) 0.0197(4) Uani 1 1 d . . . H6 H 0.0165 0.6118 0.4605 0.024 Uiso 1 1 calc R . . C7 C 0.01911(15) 0.76322(14) 0.41996(11) 0.0196(4) Uani 1 1 d . . . C8 C -0.05601(15) 0.80416(14) 0.47852(11) 0.0208(4) Uani 1 1 d . . . H8B H -0.0466 0.7646 0.5303 0.025 Uiso 1 1 calc R . . H8A H -0.0336 0.8799 0.4935 0.025 Uiso 1 1 calc R . . C9 C -0.17933(15) 0.79029(14) 0.43607(10) 0.0190(3) Uani 1 1 d . . . C10 C -0.24084(15) 0.69099(14) 0.43773(11) 0.0197(4) Uani 1 1 d . . . H10 H -0.2066 0.6358 0.4671 0.024 Uiso 1 1 calc R . . C11 C -0.35315(15) 0.67180(14) 0.39627(11) 0.0199(4) Uani 1 1 d . . . C12 C -0.40340(15) 0.75613(14) 0.35276(11) 0.0213(4) Uani 1 1 d . . . H12 H -0.4780 0.7446 0.3249 0.026 Uiso 1 1 calc R . . C13 C -0.34449(15) 0.85641(14) 0.35024(11) 0.0205(4) Uani 1 1 d . . . C14 C -0.40013(15) 0.94437(14) 0.29897(11) 0.0220(4) Uani 1 1 d . . . H14B H -0.4791 0.9410 0.3049 0.026 Uiso 1 1 calc R . . H14A H -0.3643 1.0142 0.3221 0.026 Uiso 1 1 calc R . . C15 C -0.39271(15) 0.93512(13) 0.20550(11) 0.0201(4) Uani 1 1 d . . . C16 C -0.48159(15) 0.88481(14) 0.14794(11) 0.0211(4) Uani 1 1 d . . . H16 H -0.5468 0.8576 0.1669 0.025 Uiso 1 1 calc R . . C17 C -0.47594(15) 0.87376(14) 0.06179(11) 0.0198(4) Uani 1 1 d . . . C18 C -0.37703(15) 0.91291(13) 0.03397(11) 0.0200(4) Uani 1 1 d . . . H18 H -0.3725 0.9045 -0.0232 0.024 Uiso 1 1 calc R . . C19 C -0.28517(14) 0.96409(13) 0.08957(11) 0.0191(3) Uani 1 1 d . . . C20 C -0.17792(15) 1.00454(14) 0.05788(12) 0.0213(4) Uani 1 1 d . . . H20B H -0.1478 1.0726 0.0875 0.026 Uiso 1 1 calc R . . H20A H -0.1969 1.0181 -0.0020 0.026 Uiso 1 1 calc R . . C21 C -0.08658(14) 0.92642(14) 0.07004(11) 0.0207(4) Uani 1 1 d . . . C22 C -0.08512(15) 0.84631(15) 0.00865(12) 0.0238(4) Uani 1 1 d . . . H22 H -0.1406 0.8410 -0.0398 0.029 Uiso 1 1 calc R . . C23 C -0.00321(15) 0.77366(15) 0.01735(12) 0.0234(4) Uani 1 1 d . . . C24 C 0.07901(15) 0.78046(14) 0.09060(11) 0.0207(4) Uani 1 1 d . . . H24 H 0.1340 0.7319 0.0968 0.025 Uiso 1 1 calc R . . C25 C 0.05989(15) 0.82861(13) 0.35962(11) 0.0199(4) Uani 1 1 d . . . C26 C -0.23248(15) 0.87216(13) 0.39227(11) 0.0202(4) Uani 1 1 d . . . C27 C -0.29538(15) 0.97509(13) 0.17491(11) 0.0206(4) Uani 1 1 d . . . C28 C -0.00246(15) 0.93130(13) 0.14251(11) 0.0199(4) Uani 1 1 d . . . O5 O 0.08895(12) 0.44412(11) 0.42286(9) 0.0300(3) Uani 1 1 d . . . O6 O -0.51130(12) 0.54521(12) 0.35258(10) 0.0344(4) Uani 1 1 d . . . O7 O -0.66570(12) 0.80048(12) 0.02693(9) 0.0318(3) Uani 1 1 d . . . O8 O -0.08394(18) 0.6812(2) -0.11155(13) 0.0808(7) Uani 1 1 d . . . O9 O 0.36510(19) 0.63374(17) 0.20221(14) 0.0616(6) Uani 1 1 d . . . H9 H 0.3398 0.6913 0.1893 0.074 Uiso 1 1 calc R . . C29 C 0.12738(15) 0.49878(14) 0.37048(11) 0.0211(4) Uani 1 1 d . . . C30 C 0.19736(16) 0.45033(14) 0.31255(12) 0.0230(4) Uani 1 1 d . . . H30B H 0.2720 0.4893 0.3220 0.028 Uiso 1 1 calc R . . H30A H 0.1627 0.4594 0.2542 0.028 Uiso 1 1 calc R . . C31 C 0.20945(17) 0.33147(14) 0.32562(13) 0.0270(4) Uani 1 1 d . . . H31B H 0.2399 0.3222 0.3848 0.032 Uiso 1 1 calc R . . H31A H 0.1350 0.2922 0.3132 0.032 Uiso 1 1 calc R . . C32 C 0.28484(15) 0.28278(14) 0.27143(12) 0.0225(4) Uani 1 1 d . . . H32B H 0.3612 0.3174 0.2873 0.027 Uiso 1 1 calc R . . H32A H 0.2583 0.2969 0.2124 0.027 Uiso 1 1 calc R . . C33 C 0.28696(19) 0.16228(16) 0.28072(17) 0.0375(5) Uani 1 1 d . . . H33B H 0.3168 0.1487 0.3393 0.045 Uiso 1 1 calc R . . H33A H 0.2101 0.1284 0.2678 0.045 Uiso 1 1 calc R . . C34 C 0.35663(19) 0.11101(18) 0.22437(17) 0.0415(6) Uani 1 1 d . . . H34C H 0.4340 0.1407 0.2393 0.050 Uiso 1 1 calc R . . H34B H 0.3285 0.1251 0.1663 0.050 Uiso 1 1 calc R . . H34A H 0.3520 0.0345 0.2315 0.050 Uiso 1 1 calc R . . C35 C -0.41846(16) 0.56463(15) 0.39637(11) 0.0230(4) Uani 1 1 d . . . C36 C -0.36750(16) 0.48040(14) 0.45405(12) 0.0242(4) Uani 1 1 d . . . H36B H -0.3645 0.5048 0.5125 0.029 Uiso 1 1 calc R . . H36A H -0.2904 0.4751 0.4456 0.029 Uiso 1 1 calc R . . C37 C -0.43145(16) 0.36799(14) 0.44028(12) 0.0240(4) Uani 1 1 d . . . H37B H -0.5069 0.3712 0.4532 0.029 Uiso 1 1 calc R . . H37A H -0.4389 0.3445 0.3812 0.029 Uiso 1 1 calc R . . C38 C -0.37052(16) 0.28671(15) 0.49594(13) 0.0258(4) Uani 1 1 d . . . H38B H -0.3673 0.3085 0.5550 0.031 Uiso 1 1 calc R . . H38A H -0.2934 0.2878 0.4856 0.031 Uiso 1 1 calc R . . C39 C -0.42696(17) 0.17172(15) 0.48040(14) 0.0297(4) Uani 1 1 d . . . H39B H -0.5028 0.1696 0.4934 0.036 Uiso 1 1 calc R . . H39A H -0.4333 0.1508 0.4209 0.036 Uiso 1 1 calc R . . C40 C -0.3614(2) 0.09136(17) 0.53387(18) 0.0428(6) Uani 1 1 d . . . H40C H -0.3547 0.1119 0.5928 0.051 Uiso 1 1 calc R . . H40B H -0.2874 0.0909 0.5194 0.051 Uiso 1 1 calc R . . H40A H -0.4007 0.0205 0.5231 0.051 Uiso 1 1 calc R . . C41 C -0.57653(16) 0.82189(15) 0.00232(12) 0.0241(4) Uani 1 1 d . . . C42 C -0.56570(16) 0.80001(16) -0.08855(12) 0.0273(4) Uani 1 1 d . . . H42B H -0.5036 0.7558 -0.0900 0.033 Uiso 1 1 calc R . . H42A H -0.5470 0.8680 -0.1135 0.033 Uiso 1 1 calc R . . C43 C -0.67141(17) 0.74370(16) -0.14203(13) 0.0293(4) Uani 1 1 d . . . H43B H -0.7338 0.7875 -0.1404 0.035 Uiso 1 1 calc R . . H43A H -0.6898 0.6752 -0.1178 0.035 Uiso 1 1 calc R . . C44 C -0.65882(19) 0.72353(19) -0.23392(14) 0.0358(5) Uani 1 1 d . . . H44B H -0.5938 0.6831 -0.2352 0.043 Uiso 1 1 calc R . . H44A H -0.6440 0.7924 -0.2588 0.043 Uiso 1 1 calc R . . C45 C -0.7627(2) 0.66167(19) -0.28809(15) 0.0394(5) Uani 1 1 d . . . H45B H -0.7422 0.6380 -0.3412 0.047 Uiso 1 1 calc R . . H45A H -0.7834 0.5976 -0.2589 0.047 Uiso 1 1 calc R . . C46 C -0.8649(2) 0.7247(2) -0.30779(18) 0.0513(7) Uani 1 1 d . . . H46C H -0.8454 0.7890 -0.3360 0.062 Uiso 1 1 calc R . . H46B H -0.8896 0.7440 -0.2560 0.062 Uiso 1 1 calc R . . H46A H -0.9247 0.6810 -0.3440 0.062 Uiso 1 1 calc R . . C47 C -0.00708(18) 0.68925(18) -0.05159(13) 0.0337(5) Uani 1 1 d . . . C48 C 0.08392(16) 0.61349(15) -0.04474(12) 0.0249(4) Uani 1 1 d . . . H48B H 0.0840 0.5739 0.0066 0.030 Uiso 1 1 calc R . . H48A H 0.1567 0.6554 -0.0397 0.030 Uiso 1 1 calc R . . C49 C 0.07017(16) 0.53297(15) -0.12017(12) 0.0260(4) Uani 1 1 d . . . H49B H -0.0025 0.4910 -0.1253 0.031 Uiso 1 1 calc R . . H49A H 0.0704 0.5724 -0.1716 0.031 Uiso 1 1 calc R . . C50 C 0.16234(16) 0.45683(15) -0.11252(12) 0.0259(4) Uani 1 1 d . . . H50B H 0.1630 0.4180 -0.0607 0.031 Uiso 1 1 calc R . . H50A H 0.2350 0.4986 -0.1084 0.031 Uiso 1 1 calc R . . C51 C 0.14665(18) 0.37565(16) -0.18761(13) 0.0303(4) Uani 1 1 d . . . H51B H 0.0766 0.3303 -0.1890 0.036 Uiso 1 1 calc R . . H51A H 0.1398 0.4146 -0.2397 0.036 Uiso 1 1 calc R . . C52 C 0.2424(2) 0.30481(19) -0.18449(16) 0.0433(6) Uani 1 1 d . . . H52C H 0.2504 0.2667 -0.1328 0.052 Uiso 1 1 calc R . . H52B H 0.3113 0.3488 -0.1866 0.052 Uiso 1 1 calc R . . H52A H 0.2264 0.2539 -0.2321 0.052 Uiso 1 1 calc R . . C53 C 0.3466(4) 0.5651(3) 0.1328(2) 0.0796(11) Uani 1 1 d . . . H53B H 0.3210 0.6076 0.0846 0.096 Uiso 1 1 calc R . . H53A H 0.2831 0.5142 0.1390 0.096 Uiso 1 1 calc R . . C54 C 0.4281(5) 0.5051(5) 0.1099(4) 0.156(2) Uani 1 1 d . . . H54A H 0.4896 0.5526 0.0973 0.188 Uiso 1 1 calc R . . H54B H 0.3961 0.4599 0.0606 0.188 Uiso 1 1 calc R . . H54C H 0.4554 0.4608 0.1558 0.188 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 0.0305(7) 0.0158(6) 0.0299(7) 0.0016(5) 0.0035(6) -0.0008(5) O2 0.0283(7) 0.0174(6) 0.0319(7) 0.0000(5) 0.0067(6) 0.0001(5) O3 0.0266(7) 0.0268(6) 0.0270(7) 0.0012(5) 0.0038(5) -0.0015(5) O4 0.0255(6) 0.0183(6) 0.0339(7) -0.0017(5) 0.0050(6) -0.0005(5) C1 0.0165(7) 0.0174(7) 0.0244(8) 0.0051(6) 0.0057(6) -0.0039(6) C2 0.0166(7) 0.0168(7) 0.0262(8) 0.0027(6) 0.0022(6) -0.0031(6) C3 0.0144(7) 0.0195(7) 0.0208(8) 0.0020(6) -0.0009(6) -0.0032(6) C4 0.0157(7) 0.0200(7) 0.0201(8) 0.0003(6) 0.0007(6) -0.0002(6) C5 0.0173(7) 0.0186(7) 0.0204(8) 0.0025(6) -0.0010(6) 0.0004(6) C6 0.0180(8) 0.0207(8) 0.0185(8) 0.0029(6) -0.0007(6) -0.0018(6) C7 0.0183(8) 0.0202(8) 0.0186(8) -0.0005(6) -0.0005(6) -0.0006(6) C8 0.0211(8) 0.0211(8) 0.0184(8) -0.0012(6) -0.0002(6) -0.0004(6) C9 0.0190(8) 0.0213(8) 0.0167(7) -0.0009(6) 0.0041(6) 0.0010(6) C10 0.0213(8) 0.0217(8) 0.0170(7) 0.0021(6) 0.0053(6) 0.0034(6) C11 0.0210(8) 0.0221(8) 0.0173(7) 0.0018(6) 0.0060(6) 0.0006(6) C12 0.0202(8) 0.0276(8) 0.0171(7) 0.0025(6) 0.0049(6) 0.0040(7) C13 0.0233(8) 0.0226(8) 0.0180(7) 0.0022(6) 0.0072(6) 0.0080(6) C14 0.0222(8) 0.0236(8) 0.0224(8) 0.0039(6) 0.0075(7) 0.0072(7) C15 0.0212(8) 0.0194(7) 0.0215(8) 0.0053(6) 0.0058(6) 0.0062(6) C16 0.0186(8) 0.0205(8) 0.0261(8) 0.0069(6) 0.0072(7) 0.0051(6) C17 0.0188(8) 0.0205(8) 0.0210(8) 0.0055(6) 0.0046(6) 0.0036(6) C18 0.0210(8) 0.0202(7) 0.0203(8) 0.0056(6) 0.0057(6) 0.0049(6) C19 0.0172(7) 0.0166(7) 0.0252(8) 0.0069(6) 0.0067(6) 0.0037(6) C20 0.0185(8) 0.0216(8) 0.0250(8) 0.0082(6) 0.0066(7) 0.0016(6) C21 0.0171(7) 0.0221(8) 0.0245(8) 0.0074(6) 0.0083(6) 0.0000(6) C22 0.0185(8) 0.0321(9) 0.0212(8) 0.0036(7) 0.0046(7) 0.0017(7) C23 0.0198(8) 0.0285(9) 0.0229(8) 0.0001(7) 0.0070(7) 0.0018(7) C24 0.0178(8) 0.0212(8) 0.0242(8) 0.0048(6) 0.0069(6) 0.0007(6) C25 0.0184(8) 0.0165(7) 0.0220(8) -0.0004(6) -0.0019(6) -0.0029(6) C26 0.0244(8) 0.0189(7) 0.0182(7) -0.0014(6) 0.0068(6) 0.0011(6) C27 0.0212(8) 0.0158(7) 0.0258(8) 0.0036(6) 0.0048(7) 0.0046(6) C28 0.0193(8) 0.0170(7) 0.0236(8) 0.0044(6) 0.0067(6) -0.0034(6) O5 0.0365(7) 0.0254(6) 0.0323(7) 0.0112(5) 0.0138(6) 0.0077(6) O6 0.0228(7) 0.0356(7) 0.0403(8) 0.0099(6) -0.0044(6) -0.0053(6) O7 0.0219(6) 0.0441(8) 0.0290(7) 0.0060(6) 0.0064(6) -0.0041(6) O8 0.0671(11) 0.1162(15) 0.0513(11) -0.0460(10) -0.0305(9) 0.0602(11) O9 0.0636(12) 0.0546(11) 0.0670(13) 0.0100(10) 0.0120(11) 0.0038(10) C29 0.0196(8) 0.0204(8) 0.0225(8) 0.0034(6) 0.0009(7) 0.0017(6) C30 0.0243(8) 0.0213(8) 0.0234(8) 0.0032(6) 0.0030(7) 0.0033(7) C31 0.0308(9) 0.0196(8) 0.0323(9) 0.0051(7) 0.0085(8) 0.0049(7) C32 0.0213(8) 0.0222(8) 0.0240(8) 0.0023(6) 0.0038(7) 0.0019(7) C33 0.0349(10) 0.0216(9) 0.0620(14) 0.0061(9) 0.0242(10) 0.0038(8) C34 0.0334(11) 0.0292(10) 0.0656(15) -0.0021(10) 0.0200(11) 0.0027(9) C35 0.0222(8) 0.0260(8) 0.0208(8) 0.0020(6) 0.0047(7) -0.0003(7) C36 0.0234(9) 0.0212(8) 0.0268(9) 0.0021(7) 0.0026(7) -0.0018(7) C37 0.0222(8) 0.0241(8) 0.0241(8) -0.0002(7) 0.0025(7) -0.0041(7) C38 0.0234(9) 0.0213(8) 0.0297(9) -0.0003(7) 0.0005(7) -0.0048(7) C39 0.0279(9) 0.0222(8) 0.0357(10) -0.0026(7) 0.0004(8) -0.0037(7) C40 0.0353(11) 0.0219(9) 0.0662(16) 0.0070(10) -0.0026(11) -0.0038(9) C41 0.0215(8) 0.0260(8) 0.0255(9) 0.0056(7) 0.0046(7) 0.0038(7) C42 0.0237(9) 0.0307(9) 0.0278(9) 0.0010(7) 0.0056(7) 0.0018(7) C43 0.0297(10) 0.0276(9) 0.0310(10) 0.0017(7) 0.0079(8) -0.0004(8) C44 0.0328(10) 0.0420(12) 0.0328(10) -0.0009(9) 0.0108(9) -0.0043(9) C45 0.0386(12) 0.0431(12) 0.0346(11) -0.0072(9) 0.0097(9) -0.0099(10) C46 0.0482(14) 0.0461(13) 0.0487(14) -0.0017(11) -0.0140(12) -0.0105(11) C47 0.0295(10) 0.0463(12) 0.0249(9) -0.0074(8) -0.0002(8) 0.0136(9) C48 0.0228(8) 0.0282(9) 0.0237(8) -0.0011(7) 0.0050(7) 0.0008(7) C49 0.0242(9) 0.0290(9) 0.0251(9) -0.0011(7) 0.0060(7) 0.0014(7) C50 0.0257(9) 0.0230(8) 0.0286(9) -0.0005(7) 0.0043(7) 0.0010(7) C51 0.0318(10) 0.0269(9) 0.0319(10) -0.0024(7) 0.0070(8) -0.0003(8) C52 0.0587(14) 0.0335(11) 0.0412(12) -0.0019(9) 0.0132(11) 0.0161(10) C53 0.108(3) 0.079(2) 0.0531(18) 0.0152(16) 0.0118(19) 0.018(2) C54 0.181(5) 0.198(5) 0.104(4) -0.042(4) 0.027(4) 0.104(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C25 1.380(2) . ? O2 C26 1.382(2) . ? O3 C27 1.368(2) . ? O4 C28 1.376(2) . ? C1 C24 1.391(2) . ? C1 C28 1.393(2) . ? C1 C2 1.522(2) . ? C2 C3 1.519(2) . ? C3 C4 1.389(2) . ? C3 C25 1.396(3) . ? C4 C5 1.389(2) . ? C5 C6 1.395(3) . ? C5 C29 1.490(2) . ? C6 C7 1.382(2) . ? C7 C25 1.404(2) . ? C7 C8 1.518(3) . ? C8 C9 1.518(2) . ? C9 C10 1.387(2) . ? C9 C26 1.392(2) . ? C10 C11 1.399(2) . ? C11 C12 1.400(2) . ? C11 C35 1.488(2) . ? C12 C13 1.385(3) . ? C13 C26 1.396(2) . ? C13 C14 1.520(2) . ? C14 C15 1.517(2) . ? C15 C16 1.380(2) . ? C15 C27 1.404(3) . ? C16 C17 1.397(3) . ? C17 C18 1.396(2) . ? C17 C41 1.493(2) . ? C18 C19 1.391(2) . ? C19 C27 1.397(3) . ? C19 C20 1.518(2) . ? C20 C21 1.523(2) . ? C21 C22 1.385(3) . ? C21 C28 1.401(2) . ? C22 C23 1.388(3) . ? C23 C24 1.396(2) . ? C23 C47 1.496(3) . ? O5 C29 1.220(2) . ? O6 C35 1.216(2) . ? O7 C41 1.217(2) . ? O8 C47 1.210(3) . ? O9 C53 1.358(4) . ? C29 C30 1.504(3) . ? C30 C31 1.515(3) . ? C31 C32 1.511(3) . ? C32 C33 1.512(3) . ? C33 C34 1.500(3) . ? C35 C36 1.516(3) . ? C36 C37 1.528(2) . ? C37 C38 1.520(3) . ? C38 C39 1.524(3) . ? C39 C40 1.520(3) . ? C41 C42 1.503(3) . ? C42 C43 1.512(3) . ? C43 C44 1.521(3) . ? C44 C45 1.528(3) . ? C45 C46 1.510(4) . ? C47 C48 1.500(3) . ? C48 C49 1.526(3) . ? C49 C50 1.514(3) . ? C50 C51 1.525(3) . ? C51 C52 1.507(3) . ? C53 C54 1.377(6) . ? 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 C24 C1 C28 118.11(16) . . ? C24 C1 C2 119.94(16) . . ? C28 C1 C2 121.89(16) . . ? C3 C2 C1 112.77(13) . . ? C4 C3 C25 117.91(16) . . ? C4 C3 C2 120.06(16) . . ? C25 C3 C2 122.00(15) . . ? C3 C4 C5 121.41(17) . . ? C4 C5 C6 119.21(16) . . ? C4 C5 C29 123.04(16) . . ? C6 C5 C29 117.75(15) . . ? C7 C6 C5 121.40(16) . . ? C6 C7 C25 117.93(17) . . ? C6 C7 C8 119.92(16) . . ? C25 C7 C8 122.01(15) . . ? C9 C8 C7 110.83(14) . . ? C10 C9 C26 118.27(16) . . ? C10 C9 C8 119.07(15) . . ? C26 C9 C8 122.60(15) . . ? C9 C10 C11 121.67(16) . . ? C10 C11 C12 118.29(16) . . ? C10 C11 C35 121.75(16) . . ? C12 C11 C35 119.95(16) . . ? C13 C12 C11 121.47(16) . . ? C12 C13 C26 118.45(16) . . ? C12 C13 C14 119.93(16) . . ? C26 C13 C14 121.55(16) . . ? C15 C14 C13 113.23(15) . . ? C16 C15 C27 117.89(16) . . ? C16 C15 C14 120.52(16) . . ? C27 C15 C14 121.57(15) . . ? C15 C16 C17 121.53(17) . . ? C18 C17 C16 118.92(16) . . ? C18 C17 C41 122.18(16) . . ? C16 C17 C41 118.90(16) . . ? C19 C18 C17 121.65(16) . . ? C18 C19 C27 117.43(16) . . ? C18 C19 C20 120.60(16) . . ? C27 C19 C20 121.96(15) . . ? C19 C20 C21 113.82(14) . . ? C22 C21 C28 117.52(16) . . ? C22 C21 C20 120.14(16) . . ? C28 C21 C20 122.33(16) . . ? C21 C22 C23 121.86(16) . . ? C22 C23 C24 119.11(17) . . ? C22 C23 C47 118.85(16) . . ? C24 C23 C47 122.04(17) . . ? C1 C24 C23 120.99(17) . . ? O1 C25 C3 120.39(16) . . ? O1 C25 C7 117.46(16) . . ? C3 C25 C7 122.14(16) . . ? O2 C26 C9 119.38(15) . . ? O2 C26 C13 118.77(15) . . ? C9 C26 C13 121.85(16) . . ? O3 C27 C19 117.72(16) . . ? O3 C27 C15 119.72(16) . . ? C19 C27 C15 122.55(16) . . ? O4 C28 C1 117.93(15) . . ? O4 C28 C21 119.68(16) . . ? C1 C28 C21 122.39(16) . . ? O5 C29 C5 119.65(17) . . ? O5 C29 C30 120.48(16) . . ? C5 C29 C30 119.87(15) . . ? C29 C30 C31 113.19(16) . . ? C32 C31 C30 113.99(16) . . ? C31 C32 C33 112.43(16) . . ? C34 C33 C32 113.51(19) . . ? O6 C35 C11 121.15(17) . . ? O6 C35 C36 120.49(16) . . ? C11 C35 C36 118.35(15) . . ? C35 C36 C37 114.63(15) . . ? C38 C37 C36 111.34(15) . . ? C37 C38 C39 113.36(15) . . ? C40 C39 C38 112.27(16) . . ? O7 C41 C17 120.31(17) . . ? O7 C41 C42 121.20(17) . . ? C17 C41 C42 118.47(16) . . ? C41 C42 C43 113.81(16) . . ? C42 C43 C44 112.84(17) . . ? C43 C44 C45 113.70(18) . . ? C46 C45 C44 115.0(2) . . ? O8 C47 C23 120.2(2) . . ? O8 C47 C48 120.47(19) . . ? C23 C47 C48 119.32(16) . . ? C47 C48 C49 113.57(16) . . ? C50 C49 C48 113.12(16) . . ? C49 C50 C51 112.61(16) . . ? C52 C51 C50 113.36(18) . . ? O9 C53 C54 123.3(4) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 29.64 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.792 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.080 # Attachment 'gena47_C4.cif' data_gena47 _database_code_depnum_ccdc_archive 'CCDC 632667' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common parabutanoylcalix(4)arene _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H48 O8' _chemical_formula_weight 704.82 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 9.0322(7) _cell_length_b 13.6639(11) _cell_length_c 15.2661(12) _cell_angle_alpha 86.4720(10) _cell_angle_beta 76.9620(10) _cell_angle_gamma 86.2500(10) _cell_volume 1829.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.280 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9578 _exptl_absorpt_correction_T_max 0.9786 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71070 _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 23054 _diffrn_reflns_av_R_equivalents 0.0151 _diffrn_reflns_av_sigmaI/netI 0.0182 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 29.58 _reflns_number_total 10102 _reflns_number_gt 8820 _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^)+(0.0689P)^2^+0.6336P] 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 10102 _refine_ls_number_parameters 473 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0493 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1273 _refine_ls_wR_factor_gt 0.1211 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.77278(9) 0.15515(6) 0.26995(5) 0.02280(16) Uani 1 1 d . . . H1 H 0.8358 0.1563 0.2202 0.027 Uiso 1 1 calc R . . O2 O 0.98747(9) 0.19802(6) 0.12711(6) 0.02457(16) Uani 1 1 d . . . H2 H 0.9717 0.2527 0.1016 0.029 Uiso 1 1 calc R . . O3 O 0.88024(9) 0.37620(6) 0.08824(6) 0.02584(17) Uani 1 1 d . . . H3 H 0.8027 0.3782 0.1306 0.031 Uiso 1 1 calc R . . O4 O 0.68145(9) 0.34751(6) 0.24673(6) 0.02638(17) Uani 1 1 d . . . H4 H 0.6883 0.2879 0.2632 0.032 Uiso 1 1 calc R . . O5 O 1.00316(10) 0.16571(6) 0.63048(5) 0.02795(18) Uani 1 1 d . . . O6 O 1.70499(11) 0.17424(8) 0.06159(9) 0.0454(3) Uani 1 1 d . . . O7 O 1.44831(9) 0.61215(7) 0.10676(6) 0.02998(19) Uani 1 1 d . . . O8 O 0.73347(11) 0.67819(6) 0.50846(6) 0.0329(2) Uani 1 1 d . . . C1 C 0.84943(11) 0.14880(7) 0.33879(7) 0.01848(19) Uani 1 1 d . . . C2 C 0.78048(11) 0.19456(7) 0.41842(7) 0.01888(19) Uani 1 1 d . . . C3 C 0.85562(12) 0.18705(7) 0.48856(7) 0.01943(19) Uani 1 1 d . . . H3A H 0.8092 0.2165 0.5435 0.023 Uiso 1 1 calc R . . C4 C 0.99743(11) 0.13739(7) 0.48047(7) 0.01808(18) Uani 1 1 d . . . C5 C 1.06359(11) 0.09299(7) 0.39997(7) 0.01795(18) Uani 1 1 d . . . H5 H 1.1605 0.0593 0.3938 0.022 Uiso 1 1 calc R . . C6 C 0.99075(11) 0.09690(7) 0.32853(7) 0.01736(18) Uani 1 1 d . . . C7 C 1.06609(12) 0.04542(7) 0.24297(7) 0.01843(18) Uani 1 1 d . . . H7A H 1.1158 -0.0175 0.2596 0.022 Uiso 1 1 calc R . . H7B H 0.9865 0.0300 0.2115 0.022 Uiso 1 1 calc R . . C8 C 1.07228(12) 0.13468(7) 0.55870(7) 0.01959(19) Uani 1 1 d . . . C9 C 1.23367(12) 0.09211(7) 0.54592(7) 0.01923(19) Uani 1 1 d . . . H9A H 1.2983 0.1275 0.4942 0.023 Uiso 1 1 calc R . . H9B H 1.2362 0.0224 0.5311 0.023 Uiso 1 1 calc R . . C10 C 1.30013(13) 0.09825(8) 0.62816(7) 0.0239(2) Uani 1 1 d . . . H10A H 1.2328 0.0660 0.6808 0.029 Uiso 1 1 calc R . . H10B H 1.3034 0.1681 0.6410 0.029 Uiso 1 1 calc R . . C11 C 1.45969(13) 0.04987(9) 0.61567(8) 0.0264(2) Uani 1 1 d . . . H11A H 1.4559 -0.0204 0.6075 0.032 Uiso 1 1 calc R . . H11B H 1.4999 0.0588 0.6690 0.032 Uiso 1 1 calc R . . H11C H 1.5261 0.0801 0.5625 0.032 Uiso 1 1 calc R . . C12 C 1.13875(11) 0.18318(7) 0.12505(7) 0.01778(18) Uani 1 1 d . . . C13 C 1.18353(11) 0.10521(7) 0.17878(6) 0.01745(18) Uani 1 1 d . . . C14 C 1.33826(12) 0.08376(7) 0.17023(7) 0.01943(19) Uani 1 1 d . . . H14 H 1.3714 0.0298 0.2046 0.023 Uiso 1 1 calc R . . C15 C 1.44636(12) 0.14000(8) 0.11214(7) 0.0211(2) Uani 1 1 d . . . C16 C 1.39699(12) 0.22070(8) 0.06361(7) 0.02080(19) Uani 1 1 d . . . H16 H 1.4701 0.2612 0.0266 0.025 Uiso 1 1 calc R . . C17 C 1.24360(12) 0.24303(7) 0.06819(7) 0.01790(18) Uani 1 1 d . . . C18 C 1.19231(12) 0.32855(7) 0.01212(7) 0.01938(19) Uani 1 1 d . . . H18A H 1.1090 0.3080 -0.0140 0.023 Uiso 1 1 calc R . . H18B H 1.2782 0.3454 -0.0384 0.023 Uiso 1 1 calc R . . C19 C 1.61268(13) 0.11423(9) 0.09655(8) 0.0260(2) Uani 1 1 d . . . C20 C 1.66411(12) 0.01132(8) 0.12336(8) 0.0244(2) Uani 1 1 d . . . H20A H 1.5905 -0.0351 0.1134 0.029 Uiso 1 1 calc R . . H20B H 1.6629 0.0079 0.1885 0.029 Uiso 1 1 calc R . . C21 C 1.82226(13) -0.02092(9) 0.07171(8) 0.0250(2) Uani 1 1 d . . . H21A H 1.8949 0.0284 0.0771 0.030 Uiso 1 1 calc R . . H21B H 1.8216 -0.0238 0.0072 0.030 Uiso 1 1 calc R . . C22 C 1.87596(14) -0.12099(9) 0.10612(9) 0.0294(2) Uani 1 1 d . . . H22A H 1.8906 -0.1162 0.1674 0.035 Uiso 1 1 calc R . . H22B H 1.9724 -0.1424 0.0666 0.035 Uiso 1 1 calc R . . H22C H 1.7994 -0.1687 0.1065 0.035 Uiso 1 1 calc R . . C23 C 0.98270(12) 0.43995(7) 0.10275(7) 0.01915(19) Uani 1 1 d . . . C24 C 1.13730(12) 0.41947(7) 0.06488(7) 0.01853(18) Uani 1 1 d . . . C25 C 1.24123(12) 0.48485(8) 0.07648(7) 0.01959(19) Uani 1 1 d . . . H25 H 1.3464 0.4718 0.0514 0.024 Uiso 1 1 calc R . . C26 C 1.19503(12) 0.56954(8) 0.12416(7) 0.01977(19) Uani 1 1 d . . . C27 C 1.04038(12) 0.58766(8) 0.16149(7) 0.02053(19) Uani 1 1 d . . . H27 H 1.0082 0.6452 0.1940 0.025 Uiso 1 1 calc R . . C28 C 0.93241(11) 0.52324(8) 0.15213(7) 0.01945(19) Uani 1 1 d . . . C29 C 0.76629(12) 0.54334(8) 0.19761(7) 0.0219(2) Uani 1 1 d . . . H29A H 0.7423 0.6151 0.1965 0.026 Uiso 1 1 calc R . . H29B H 0.7012 0.5133 0.1635 0.026 Uiso 1 1 calc R . . C30 C 1.31375(12) 0.63668(8) 0.13260(7) 0.0224(2) Uani 1 1 d . . . C31 C 1.26666(15) 0.73628(9) 0.17081(10) 0.0319(3) Uani 1 1 d . . . H31A H 1.1784 0.7296 0.2223 0.038 Uiso 1 1 calc R . . H31B H 1.2339 0.7808 0.1243 0.038 Uiso 1 1 calc R . . C32 C 1.39347(15) 0.78197(9) 0.20205(11) 0.0362(3) Uani 1 1 d . . . H32A H 1.4849 0.7837 0.1521 0.043 Uiso 1 1 calc R . . H32B H 1.3613 0.8504 0.2181 0.043 Uiso 1 1 calc R . . C33 C 1.4337(2) 0.72523(13) 0.28267(12) 0.0500(4) Uani 1 1 d . . . H33A H 1.3429 0.7220 0.3318 0.060 Uiso 1 1 calc R . . H33B H 1.5126 0.7584 0.3024 0.060 Uiso 1 1 calc R . . H33C H 1.4716 0.6586 0.2660 0.060 Uiso 1 1 calc R . . C34 C 0.69357(11) 0.40415(8) 0.31540(7) 0.0209(2) Uani 1 1 d . . . C35 C 0.73025(11) 0.50247(8) 0.29442(7) 0.0210(2) Uani 1 1 d . . . C36 C 0.73895(12) 0.56044(8) 0.36401(8) 0.0224(2) Uani 1 1 d . . . H36 H 0.7630 0.6272 0.3508 0.027 Uiso 1 1 calc R . . C37 C 0.71337(12) 0.52355(8) 0.45340(7) 0.0225(2) Uani 1 1 d . . . C38 C 0.67772(12) 0.42532(8) 0.47172(7) 0.0224(2) Uani 1 1 d . . . H38 H 0.6607 0.3993 0.5321 0.027 Uiso 1 1 calc R . . C39 C 0.66661(11) 0.36481(8) 0.40413(7) 0.0209(2) Uani 1 1 d . . . C40 C 0.63345(11) 0.25745(8) 0.42683(7) 0.0213(2) Uani 1 1 d . . . H40A H 0.5717 0.2501 0.4891 0.026 Uiso 1 1 calc R . . H40B H 0.5739 0.2349 0.3855 0.026 Uiso 1 1 calc R . . C41 C 0.72108(13) 0.59042(8) 0.52572(8) 0.0256(2) Uani 1 1 d . . . C42 C 0.70797(14) 0.54687(9) 0.62099(8) 0.0284(2) Uani 1 1 d . . . H42A H 0.7847 0.4915 0.6198 0.034 Uiso 1 1 calc R . . H42B H 0.6062 0.5200 0.6422 0.034 Uiso 1 1 calc R . . C43 C 0.73020(15) 0.61953(10) 0.68823(9) 0.0332(3) Uani 1 1 d . . . H43A H 0.6723 0.6820 0.6792 0.040 Uiso 1 1 calc R . . H43B H 0.6888 0.5929 0.7501 0.040 Uiso 1 1 calc R . . C44 C 0.89612(17) 0.63979(10) 0.67847(10) 0.0375(3) Uani 1 1 d . . . H44A H 0.9540 0.5781 0.6871 0.045 Uiso 1 1 calc R . . H44B H 0.9054 0.6854 0.7238 0.045 Uiso 1 1 calc R . . H44C H 0.9363 0.6689 0.6182 0.045 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 0.0207(4) 0.0260(4) 0.0228(4) 0.0030(3) -0.0073(3) -0.0040(3) O2 0.0188(4) 0.0271(4) 0.0284(4) 0.0046(3) -0.0077(3) -0.0018(3) O3 0.0252(4) 0.0281(4) 0.0266(4) 0.0066(3) -0.0110(3) -0.0083(3) O4 0.0240(4) 0.0246(4) 0.0305(4) 0.0024(3) -0.0066(3) -0.0024(3) O5 0.0289(4) 0.0336(4) 0.0194(4) -0.0035(3) -0.0029(3) 0.0060(3) O6 0.0220(4) 0.0372(5) 0.0743(8) 0.0251(5) -0.0109(5) -0.0071(4) O7 0.0205(4) 0.0325(4) 0.0352(5) -0.0073(4) -0.0001(3) -0.0050(3) O8 0.0446(5) 0.0208(4) 0.0323(4) 0.0042(3) -0.0083(4) 0.0004(3) C1 0.0178(4) 0.0168(4) 0.0208(5) 0.0049(3) -0.0048(4) -0.0038(3) C2 0.0161(4) 0.0159(4) 0.0227(5) 0.0051(3) -0.0016(4) -0.0014(3) C3 0.0195(4) 0.0171(4) 0.0192(4) 0.0025(3) -0.0006(4) 0.0005(3) C4 0.0186(4) 0.0170(4) 0.0175(4) 0.0029(3) -0.0025(3) -0.0005(3) C5 0.0178(4) 0.0161(4) 0.0186(4) 0.0027(3) -0.0024(3) -0.0004(3) C6 0.0182(4) 0.0147(4) 0.0179(4) 0.0025(3) -0.0019(3) -0.0024(3) C7 0.0212(4) 0.0155(4) 0.0179(4) 0.0014(3) -0.0031(4) -0.0025(3) C8 0.0220(5) 0.0171(4) 0.0186(4) 0.0022(3) -0.0034(4) -0.0001(3) C9 0.0204(4) 0.0185(4) 0.0182(4) 0.0008(3) -0.0038(4) 0.0000(3) C10 0.0247(5) 0.0269(5) 0.0210(5) -0.0021(4) -0.0074(4) 0.0006(4) C11 0.0243(5) 0.0305(5) 0.0253(5) 0.0018(4) -0.0087(4) -0.0003(4) C12 0.0185(4) 0.0186(4) 0.0166(4) -0.0007(3) -0.0045(3) -0.0018(3) C13 0.0203(4) 0.0164(4) 0.0154(4) 0.0002(3) -0.0033(3) -0.0028(3) C14 0.0216(5) 0.0179(4) 0.0188(4) 0.0020(3) -0.0055(4) -0.0007(3) C15 0.0191(4) 0.0214(5) 0.0225(5) 0.0026(4) -0.0052(4) -0.0018(4) C16 0.0206(5) 0.0204(5) 0.0205(5) 0.0032(4) -0.0033(4) -0.0031(4) C17 0.0209(4) 0.0171(4) 0.0158(4) 0.0012(3) -0.0047(3) -0.0016(3) C18 0.0224(5) 0.0191(4) 0.0161(4) 0.0030(3) -0.0044(4) -0.0006(4) C19 0.0206(5) 0.0262(5) 0.0313(6) 0.0070(4) -0.0077(4) -0.0026(4) C20 0.0200(5) 0.0241(5) 0.0275(5) 0.0033(4) -0.0034(4) 0.0001(4) C21 0.0227(5) 0.0295(5) 0.0222(5) -0.0034(4) -0.0034(4) 0.0006(4) C22 0.0285(6) 0.0273(5) 0.0321(6) -0.0089(5) -0.0060(5) 0.0046(4) C23 0.0198(5) 0.0202(4) 0.0182(4) 0.0058(3) -0.0072(4) -0.0023(4) C24 0.0216(5) 0.0183(4) 0.0152(4) 0.0041(3) -0.0048(3) 0.0001(3) C25 0.0189(4) 0.0204(4) 0.0184(4) 0.0035(4) -0.0032(3) -0.0004(3) C26 0.0202(5) 0.0193(4) 0.0193(4) 0.0032(4) -0.0043(4) -0.0019(4) C27 0.0210(5) 0.0196(4) 0.0197(4) 0.0034(4) -0.0033(4) 0.0004(4) C28 0.0179(4) 0.0205(4) 0.0188(4) 0.0068(4) -0.0042(3) 0.0006(3) C29 0.0173(4) 0.0217(5) 0.0246(5) 0.0078(4) -0.0037(4) 0.0016(4) C30 0.0227(5) 0.0220(5) 0.0221(5) 0.0013(4) -0.0038(4) -0.0030(4) C31 0.0304(6) 0.0213(5) 0.0464(7) -0.0040(5) -0.0135(5) 0.0009(4) C32 0.0320(6) 0.0236(5) 0.0543(8) -0.0088(5) -0.0092(6) -0.0056(5) C33 0.0531(9) 0.0543(9) 0.0496(9) -0.0266(7) -0.0249(7) 0.0161(7) C34 0.0138(4) 0.0220(5) 0.0250(5) 0.0050(4) -0.0029(4) 0.0012(3) C35 0.0142(4) 0.0217(5) 0.0245(5) 0.0072(4) -0.0018(4) 0.0023(3) C36 0.0183(4) 0.0193(4) 0.0269(5) 0.0066(4) -0.0020(4) 0.0019(4) C37 0.0193(5) 0.0205(5) 0.0258(5) 0.0045(4) -0.0033(4) 0.0026(4) C38 0.0186(5) 0.0213(5) 0.0242(5) 0.0067(4) -0.0015(4) 0.0026(4) C39 0.0142(4) 0.0196(4) 0.0262(5) 0.0069(4) -0.0016(4) 0.0009(3) C40 0.0155(4) 0.0201(5) 0.0256(5) 0.0055(4) -0.0008(4) -0.0004(3) C41 0.0248(5) 0.0225(5) 0.0275(5) 0.0042(4) -0.0042(4) 0.0015(4) C42 0.0252(5) 0.0283(5) 0.0301(6) 0.0060(4) -0.0045(4) -0.0012(4) C43 0.0342(6) 0.0345(6) 0.0287(6) 0.0034(5) -0.0048(5) 0.0022(5) C44 0.0427(7) 0.0319(6) 0.0396(7) 0.0057(5) -0.0140(6) -0.0044(5) _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 1.3786(12) . ? O2 C12 1.3617(12) . ? O3 C23 1.3733(12) . ? O4 C34 1.3685(14) . ? O5 C8 1.2182(13) . ? O6 C19 1.2194(14) . ? O7 C30 1.2214(14) . ? O8 C41 1.2189(14) . ? C1 C2 1.3992(14) . ? C1 C6 1.4006(14) . ? C2 C3 1.3867(14) . ? C2 C40 1.5185(14) . ? C3 C4 1.3934(14) . ? C4 C5 1.3958(14) . ? C4 C8 1.4968(14) . ? C5 C6 1.3919(14) . ? C6 C7 1.5209(14) . ? C7 C13 1.5162(13) . ? C8 C9 1.5087(14) . ? C9 C10 1.5177(14) . ? C10 C11 1.5223(16) . ? C12 C13 1.3990(14) . ? C12 C17 1.4007(14) . ? C13 C14 1.3874(14) . ? C14 C15 1.3979(14) . ? C15 C16 1.3956(14) . ? C15 C19 1.4890(15) . ? C16 C17 1.3861(14) . ? C17 C18 1.5158(13) . ? C18 C24 1.5169(14) . ? C19 C20 1.5133(16) . ? C20 C21 1.5193(15) . ? C21 C22 1.5234(17) . ? C23 C28 1.3976(15) . ? C23 C24 1.4025(14) . ? C24 C25 1.3838(14) . ? C25 C26 1.3951(14) . ? C26 C27 1.3965(14) . ? C26 C30 1.4878(15) . ? C27 C28 1.3918(15) . ? C28 C29 1.5194(14) . ? C29 C35 1.5189(15) . ? C30 C31 1.5111(16) . ? C31 C32 1.5185(18) . ? C32 C33 1.515(2) . ? C34 C39 1.4005(15) . ? C34 C35 1.4052(14) . ? C35 C36 1.3827(16) . ? C36 C37 1.3993(15) . ? C37 C38 1.3975(15) . ? C37 C41 1.4918(16) . ? C38 C39 1.3861(16) . ? C39 C40 1.5199(14) . ? C41 C42 1.5194(16) . ? C42 C43 1.5245(18) . ? C43 C44 1.514(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 O1 C1 C2 117.82(9) . . ? O1 C1 C6 120.31(9) . . ? C2 C1 C6 121.87(9) . . ? C3 C2 C1 118.17(9) . . ? C3 C2 C40 119.92(9) . . ? C1 C2 C40 121.75(9) . . ? C2 C3 C4 121.67(9) . . ? C3 C4 C5 118.76(9) . . ? C3 C4 C8 118.25(9) . . ? C5 C4 C8 123.00(9) . . ? C6 C5 C4 121.50(9) . . ? C5 C6 C1 118.01(9) . . ? C5 C6 C7 119.47(9) . . ? C1 C6 C7 122.53(9) . . ? C13 C7 C6 113.74(8) . . ? O5 C8 C4 120.25(10) . . ? O5 C8 C9 121.59(10) . . ? C4 C8 C9 118.15(9) . . ? C8 C9 C10 113.33(9) . . ? C9 C10 C11 112.46(9) . . ? O2 C12 C13 117.66(9) . . ? O2 C12 C17 119.90(9) . . ? C13 C12 C17 122.41(9) . . ? C14 C13 C12 117.82(9) . . ? C14 C13 C7 121.40(9) . . ? C12 C13 C7 120.77(9) . . ? C13 C14 C15 121.31(9) . . ? C16 C15 C14 119.07(9) . . ? C16 C15 C19 118.46(9) . . ? C14 C15 C19 122.40(9) . . ? C17 C16 C15 121.44(9) . . ? C16 C17 C12 117.78(9) . . ? C16 C17 C18 120.70(9) . . ? C12 C17 C18 121.51(9) . . ? C17 C18 C24 113.62(8) . . ? O6 C19 C15 120.67(10) . . ? O6 C19 C20 120.91(10) . . ? C15 C19 C20 118.41(9) . . ? C19 C20 C21 113.64(9) . . ? C20 C21 C22 112.20(10) . . ? O3 C23 C28 120.41(9) . . ? O3 C23 C24 117.77(9) . . ? C28 C23 C24 121.80(9) . . ? C25 C24 C23 118.35(9) . . ? C25 C24 C18 119.76(9) . . ? C23 C24 C18 121.89(9) . . ? C24 C25 C26 121.46(10) . . ? C25 C26 C27 118.87(10) . . ? C25 C26 C30 118.12(9) . . ? C27 C26 C30 123.01(10) . . ? C28 C27 C26 121.44(10) . . ? C27 C28 C23 118.07(9) . . ? C27 C28 C29 119.67(9) . . ? C23 C28 C29 122.24(9) . . ? C35 C29 C28 111.88(8) . . ? O7 C30 C26 120.02(10) . . ? O7 C30 C31 120.36(10) . . ? C26 C30 C31 119.59(10) . . ? C30 C31 C32 112.89(10) . . ? C33 C32 C31 111.87(12) . . ? O4 C34 C39 120.30(10) . . ? O4 C34 C35 118.18(9) . . ? C39 C34 C35 121.50(10) . . ? C36 C35 C34 118.26(10) . . ? C36 C35 C29 120.51(9) . . ? C34 C35 C29 121.18(10) . . ? C35 C36 C37 121.82(10) . . ? C38 C37 C36 118.35(10) . . ? C38 C37 C41 122.38(10) . . ? C36 C37 C41 119.26(10) . . ? C39 C38 C37 121.74(10) . . ? C38 C39 C34 118.32(10) . . ? C38 C39 C40 119.85(9) . . ? C34 C39 C40 121.76(10) . . ? C2 C40 C39 110.64(8) . . ? O8 C41 C37 120.22(11) . . ? O8 C41 C42 121.33(11) . . ? C37 C41 C42 118.42(10) . . ? C41 C42 C43 114.28(10) . . ? C44 C43 C42 112.21(11) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 29.58 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.522 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.049 # Attachment 'gena51_C10.cif' data_gena51 _database_code_depnum_ccdc_archive 'CCDC 632668' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common para-decanoylcalix(4)arene _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H96 O8' _chemical_formula_weight 1041.45 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.630(2) _cell_length_b 15.163(3) _cell_length_c 33.741(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.117(3) _cell_angle_gamma 90.00 _cell_volume 5875.1(17) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9706 _exptl_absorpt_correction_T_max 0.9985 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71070 _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 30096 _diffrn_reflns_av_R_equivalents 0.1214 _diffrn_reflns_av_sigmaI/netI 0.0815 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 20.00 _reflns_number_total 5480 _reflns_number_gt 3650 _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^)+(0.0842P)^2^+55.0413P] 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 5480 _refine_ls_number_parameters 764 _refine_ls_number_restraints 281 _refine_ls_R_factor_all 0.1637 _refine_ls_R_factor_gt 0.1234 _refine_ls_wR_factor_ref 0.2900 _refine_ls_wR_factor_gt 0.2780 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.6807(6) 0.9459(4) 0.22798(18) 0.0211(16) Uani 1 1 d D . . H1 H 0.684(18) 0.892(2) 0.221(4) 0.21(10) Uiso 1 1 d D . . O2 O 0.4472(6) 0.9402(4) 0.20711(18) 0.0236(16) Uani 1 1 d D . . H2 H 0.521(3) 0.944(17) 0.213(7) 0.27(13) Uiso 1 1 d D . . O3 O 0.4531(6) 0.7626(5) 0.20629(19) 0.0256(17) Uani 1 1 d D . . H3 H 0.446(14) 0.8176(17) 0.203(4) 0.14(7) Uiso 1 1 d D . . O4 O 0.6861(6) 0.7699(4) 0.22846(19) 0.0246(17) Uani 1 1 d D . . H4 H 0.617(4) 0.760(14) 0.217(5) 0.23(11) Uiso 1 1 d D . . O5 O 0.7563(6) 1.1448(6) 0.3942(2) 0.049(2) Uani 1 1 d . . . O6 O 0.1099(6) 1.0423(4) 0.32887(18) 0.0274(17) Uani 1 1 d . . . O7 O 0.1293(6) 0.6442(4) 0.32992(18) 0.0290(17) Uani 1 1 d . . . O8 O 0.7947(8) 0.5647(6) 0.3918(3) 0.075(3) Uani 1 1 d . A . C1 C 0.7146(7) 0.9781(6) 0.2664(3) 0.013(2) Uani 1 1 d U . . C2 C 0.8083(7) 0.9409(6) 0.2908(3) 0.015(2) Uani 1 1 d U . . C3 C 0.8426(8) 0.9796(6) 0.3283(3) 0.016(2) Uani 1 1 d U . . H3A H 0.9088 0.9569 0.3454 0.020 Uiso 1 1 calc R . . C4 C 0.7834(8) 1.0498(6) 0.3414(3) 0.018(2) Uani 1 1 d . . . C5 C 0.6900(7) 1.0846(6) 0.3164(2) 0.012(2) Uani 1 1 d U . . H5 H 0.6500 1.1337 0.3252 0.015 Uiso 1 1 calc R . . C6 C 0.6526(7) 1.0499(6) 0.2786(2) 0.012(2) Uani 1 1 d U . . C7 C 0.5472(7) 1.0891(5) 0.2524(3) 0.011(2) Uani 1 1 d . . . H7B H 0.5436 1.1529 0.2581 0.013 Uiso 1 1 calc R . . H7A H 0.5567 1.0824 0.2239 0.013 Uiso 1 1 calc R . . C8 C 0.8195(8) 1.0921(6) 0.3819(3) 0.020(2) Uani 1 1 d . . . C9 C 0.9337(8) 1.0664(6) 0.4071(3) 0.025(3) Uani 1 1 d . . . H9B H 0.9329 1.0022 0.4124 0.029 Uiso 1 1 calc R . . H9A H 0.9977 1.0784 0.3917 0.029 Uiso 1 1 calc R . . C10 C 0.9582(7) 1.1145(6) 0.4468(3) 0.022(2) Uani 1 1 d U . . H10B H 0.8964 1.1004 0.4628 0.027 Uiso 1 1 calc R . . H10A H 0.9561 1.1789 0.4417 0.027 Uiso 1 1 calc R . . C11 C 1.0753(8) 1.0901(6) 0.4705(3) 0.025(3) Uani 1 1 d . . . H11B H 1.1367 1.1048 0.4544 0.029 Uiso 1 1 calc R . . H11A H 1.0774 1.0255 0.4750 0.029 Uiso 1 1 calc R . . C12 C 1.1035(8) 1.1365(6) 0.5115(3) 0.024(2) Uani 1 1 d . . . H12B H 1.1021 1.2011 0.5071 0.029 Uiso 1 1 calc R . . H12A H 1.0421 1.1220 0.5276 0.029 Uiso 1 1 calc R . . C13 C 1.2197(8) 1.1111(6) 0.5347(3) 0.021(2) Uani 1 1 d . . . H13B H 1.2811 1.1257 0.5185 0.025 Uiso 1 1 calc R . . H13A H 1.2211 1.0464 0.5389 0.025 Uiso 1 1 calc R . . C14 C 1.2479(7) 1.1560(6) 0.5749(3) 0.022(2) Uani 1 1 d . . . H14B H 1.1854 1.1429 0.5908 0.027 Uiso 1 1 calc R . . H14A H 1.2490 1.2206 0.5707 0.027 Uiso 1 1 calc R . . C15 C 1.3663(8) 1.1273(6) 0.5992(3) 0.022(2) Uani 1 1 d . . . H15B H 1.3650 1.0627 0.6033 0.026 Uiso 1 1 calc R . . H15A H 1.4286 1.1403 0.5832 0.026 Uiso 1 1 calc R . . C16 C 1.3959(8) 1.1713(6) 0.6392(3) 0.026(3) Uani 1 1 d . . . H16B H 1.3333 1.1589 0.6552 0.032 Uiso 1 1 calc R . . H16A H 1.3983 1.2359 0.6351 0.032 Uiso 1 1 calc R . . C17 C 1.5099(8) 1.1423(7) 0.6626(3) 0.029(3) Uani 1 1 d . . . H17C H 1.5726 1.1547 0.6472 0.034 Uiso 1 1 calc R . . H17B H 1.5072 1.0789 0.6679 0.034 Uiso 1 1 calc R . . H17A H 1.5244 1.1744 0.6882 0.034 Uiso 1 1 calc R . . C18 C 0.3895(8) 0.9731(6) 0.2370(3) 0.016(2) Uani 1 1 d U . . C19 C 0.4349(7) 1.0470(6) 0.2585(2) 0.013(2) Uani 1 1 d U . . C20 C 0.3762(7) 1.0764(6) 0.2883(3) 0.013(2) Uani 1 1 d U . . H20 H 0.4075 1.1248 0.3044 0.016 Uiso 1 1 calc R . . C21 C 0.2724(7) 1.0382(6) 0.2960(2) 0.011(2) Uani 1 1 d U . . C22 C 0.2312(8) 0.9665(6) 0.2730(3) 0.021(2) Uani 1 1 d . . . H22 H 0.1600 0.9405 0.2774 0.026 Uiso 1 1 calc R . . C23 C 0.2880(7) 0.9305(5) 0.2438(3) 0.012(2) Uani 1 1 d U . . C24 C 0.2414(8) 0.8465(6) 0.2220(3) 0.021(2) Uani 1 1 d U . . H24B H 0.1558 0.8441 0.2205 0.025 Uiso 1 1 calc R . . H24A H 0.2591 0.8474 0.1942 0.025 Uiso 1 1 calc R . . C25 C 0.2082(8) 1.0693(6) 0.3285(3) 0.018(2) Uani 1 1 d . . . C26 C 0.2690(8) 1.1287(6) 0.3598(3) 0.025(3) Uani 1 1 d . . . H26B H 0.2124 1.1498 0.3768 0.030 Uiso 1 1 calc R . . H26A H 0.2978 1.1808 0.3467 0.030 Uiso 1 1 calc R . . C27 C 0.3709(8) 1.0856(6) 0.3866(3) 0.025(3) Uani 1 1 d . . . H27B H 0.3488 1.0244 0.3924 0.029 Uiso 1 1 calc R . . H27A H 0.4375 1.0822 0.3716 0.029 Uiso 1 1 calc R . . C28 C 0.4103(8) 1.1321(7) 0.4257(3) 0.032(3) Uani 1 1 d . . . H28B H 0.3467 1.1294 0.4420 0.038 Uiso 1 1 calc R . . H28A H 0.4237 1.1950 0.4201 0.038 Uiso 1 1 calc R . . C29 C 0.5193(9) 1.0954(6) 0.4503(3) 0.030(3) Uani 1 1 d . . . H29B H 0.5082 1.0314 0.4541 0.036 Uiso 1 1 calc R . . H29A H 0.5844 1.1025 0.4349 0.036 Uiso 1 1 calc R . . C30 C 0.5533(8) 1.1375(7) 0.4909(3) 0.027(3) Uani 1 1 d . . . H30B H 0.4896 1.1278 0.5067 0.032 Uiso 1 1 calc R . . H30A H 0.5605 1.2019 0.4871 0.032 Uiso 1 1 calc R . . C31 C 0.6656(8) 1.1042(7) 0.5150(3) 0.031(3) Uani 1 1 d . . . H31B H 0.7300 1.1156 0.4997 0.037 Uiso 1 1 calc R . . H31A H 0.6596 1.0395 0.5182 0.037 Uiso 1 1 calc R . . C32 C 0.6963(8) 1.1458(7) 0.5566(3) 0.028(3) Uani 1 1 d . . . H32B H 0.7005 1.2106 0.5534 0.034 Uiso 1 1 calc R . . H32A H 0.6329 1.1331 0.5721 0.034 Uiso 1 1 calc R . . C33 C 0.8095(8) 1.1140(7) 0.5801(3) 0.028(3) Uani 1 1 d . . . H33B H 0.8737 1.1299 0.5653 0.033 Uiso 1 1 calc R . . H33A H 0.8073 1.0489 0.5819 0.033 Uiso 1 1 calc R . . C34 C 0.8351(9) 1.1519(7) 0.6220(3) 0.036(3) Uani 1 1 d . . . H34C H 0.7761 1.1315 0.6377 0.043 Uiso 1 1 calc R . . H34B H 0.8334 1.2165 0.6205 0.043 Uiso 1 1 calc R . . H34A H 0.9123 1.1324 0.6350 0.043 Uiso 1 1 calc R . . C35 C 0.4008(8) 0.7284(6) 0.2369(3) 0.018(2) Uani 1 1 d U . . C36 C 0.2953(8) 0.7656(6) 0.2435(3) 0.017(2) Uani 1 1 d U . . C37 C 0.2416(8) 0.7313(6) 0.2739(3) 0.019(2) Uani 1 1 d U . . H37 H 0.1697 0.7555 0.2787 0.023 Uiso 1 1 calc R . . C38 C 0.2917(8) 0.6618(6) 0.2974(3) 0.018(2) Uani 1 1 d . . . C39 C 0.3972(8) 0.6247(6) 0.2896(3) 0.016(2) Uani 1 1 d U . . H39 H 0.4303 0.5760 0.3051 0.019 Uiso 1 1 calc R . . C40 C 0.4532(8) 0.6587(6) 0.2593(3) 0.019(2) Uani 1 1 d U . . C41 C 0.5676(8) 0.6176(6) 0.2516(3) 0.025(3) Uani 1 1 d . . . H41B H 0.5663 0.5535 0.2571 0.030 Uiso 1 1 calc R . . H41A H 0.5751 0.6256 0.2230 0.030 Uiso 1 1 calc R . . C42 C 0.2313(9) 0.6254(6) 0.3297(3) 0.026(3) Uani 1 1 d . . . C43 C 0.2975(9) 0.5712(7) 0.3633(3) 0.031(3) Uani 1 1 d . . . H43B H 0.3331 0.5199 0.3517 0.038 Uiso 1 1 calc R . . H43A H 0.2426 0.5486 0.3805 0.038 Uiso 1 1 calc R . . C44 C 0.3931(9) 0.6250(6) 0.3890(3) 0.033(3) Uani 1 1 d . . . H44B H 0.4542 0.6387 0.3725 0.040 Uiso 1 1 calc R . . H44A H 0.3591 0.6818 0.3959 0.040 Uiso 1 1 calc R . . C45 C 0.4497(10) 0.5819(7) 0.4271(3) 0.044(3) Uani 1 1 d U . . H45B H 0.4809 0.5239 0.4204 0.052 Uiso 1 1 calc R . . H45A H 0.3897 0.5711 0.4443 0.052 Uiso 1 1 calc R . . C46 C 0.5472(8) 0.6349(6) 0.4506(3) 0.027(3) Uani 1 1 d . . . H46B H 0.6060 0.6458 0.4329 0.033 Uiso 1 1 calc R . . H46A H 0.5151 0.6930 0.4566 0.033 Uiso 1 1 calc R . . C47 C 0.6089(11) 0.5971(8) 0.4892(4) 0.064(4) Uani 1 1 d . . . H47B H 0.5502 0.5851 0.5067 0.077 Uiso 1 1 calc R . . H47A H 0.6428 0.5397 0.4831 0.077 Uiso 1 1 calc R . . C48 C 0.7009(9) 0.6500(7) 0.5117(3) 0.033(3) Uani 1 1 d . . . H48B H 0.6664 0.7075 0.5172 0.040 Uiso 1 1 calc R . . H48A H 0.7589 0.6619 0.4938 0.040 Uiso 1 1 calc R . . C49 C 0.7642(11) 0.6172(9) 0.5496(4) 0.062(4) Uani 1 1 d . . . H49B H 0.7059 0.6051 0.5673 0.074 Uiso 1 1 calc R . . H49A H 0.7985 0.5597 0.5439 0.074 Uiso 1 1 calc R . . C50 C 0.8560(10) 0.6685(8) 0.5727(3) 0.055(4) Uani 1 1 d . . . H50B H 0.9128 0.6826 0.5546 0.066 Uiso 1 1 calc R . . H50A H 0.8209 0.7252 0.5792 0.066 Uiso 1 1 calc R . . C51 C 0.9215(12) 0.6355(9) 0.6095(4) 0.073(4) Uani 1 1 d . . . H51C H 0.9531 0.5772 0.6048 0.088 Uiso 1 1 calc R . . H51B H 0.8704 0.6307 0.6299 0.088 Uiso 1 1 calc R . . H51A H 0.9857 0.6760 0.6190 0.088 Uiso 1 1 calc R . . C52 C 0.7246(8) 0.7341(6) 0.2654(3) 0.020(2) Uani 1 1 d U . . C53 C 0.6715(8) 0.6588(6) 0.2777(3) 0.022(2) Uani 1 1 d U . . C54 C 0.7161(9) 0.6238(6) 0.3150(3) 0.030(3) Uani 1 1 d . . . H54 H 0.6808 0.5726 0.3239 0.035 Uiso 1 1 calc R . . C55 C 0.8100(8) 0.6610(6) 0.3397(3) 0.024(2) Uani 1 1 d U A . C56 C 0.8605(8) 0.7362(6) 0.3260(3) 0.020(2) Uani 1 1 d U . . H56 H 0.9253 0.7621 0.3426 0.023 Uiso 1 1 calc R . . C57 C 0.8203(8) 0.7750(6) 0.2892(3) 0.021(2) Uani 1 1 d . . . C58 C 0.8716(7) 0.8618(6) 0.2781(3) 0.015(2) Uani 1 1 d U . . H58B H 0.9542 0.8647 0.2909 0.019 Uiso 1 1 calc R . . H58A H 0.8693 0.8638 0.2486 0.019 Uiso 1 1 calc R . . C59 C 0.8549(9) 0.6213(7) 0.3789(3) 0.043(3) Uani 1 1 d D . . C60 C 0.968(2) 0.655(2) 0.4011(6) 0.023(4) Uani 0.55 1 d PDU A 1 H60A H 0.9644 0.7205 0.4028 0.028 Uiso 0.55 1 calc PR A 1 H60B H 1.0317 0.6403 0.3858 0.028 Uiso 0.55 1 calc PR A 1 C61 C 0.997(3) 0.617(2) 0.4435(8) 0.039(4) Uani 0.55 1 d PDU A 1 H61A H 0.9356 0.6336 0.4593 0.047 Uiso 0.55 1 calc PR A 1 H61B H 1.0002 0.5519 0.4421 0.047 Uiso 0.55 1 calc PR A 1 C62 C 1.1139(18) 0.653(2) 0.4636(5) 0.023(4) Uani 0.55 1 d PDU A 1 H62A H 1.1105 0.7179 0.4637 0.027 Uiso 0.55 1 calc PR A 1 H62B H 1.1745 0.6350 0.4476 0.027 Uiso 0.55 1 calc PR A 1 C63 C 1.150(2) 0.620(2) 0.5066(6) 0.046(5) Uani 0.55 1 d PDU A 1 H63A H 1.0874 0.6364 0.5222 0.055 Uiso 0.55 1 calc PR A 1 H63B H 1.1546 0.5553 0.5062 0.055 Uiso 0.55 1 calc PR A 1 C64 C 1.263(2) 0.656(2) 0.5281(6) 0.032(5) Uani 0.55 1 d PDU A 1 H64A H 1.2563 0.7208 0.5298 0.039 Uiso 0.55 1 calc PR A 1 H64B H 1.3243 0.6428 0.5117 0.039 Uiso 0.55 1 calc PR A 1 C65 C 1.3013(18) 0.6199(16) 0.5699(5) 0.044(6) Uani 0.55 1 d PDU A 1 H65A H 1.2399 0.6322 0.5864 0.053 Uiso 0.55 1 calc PR A 1 H65B H 1.3097 0.5551 0.5683 0.053 Uiso 0.55 1 calc PR A 1 C66 C 1.414(2) 0.6583(18) 0.5905(5) 0.049(8) Uani 0.55 1 d PD A 1 H66A H 1.4029 0.7225 0.5933 0.059 Uiso 0.55 1 calc PR A 1 H66B H 1.4728 0.6502 0.5725 0.059 Uiso 0.55 1 calc PR A 1 C67 C 1.4663(16) 0.6222(13) 0.6317(5) 0.048(5) Uani 0.55 1 d PD A 1 H67A H 1.4791 0.5580 0.6296 0.057 Uiso 0.55 1 calc PR A 1 H67B H 1.5429 0.6503 0.6405 0.057 Uiso 0.55 1 calc PR A 1 C68 C 1.390(2) 0.6384(17) 0.6627(7) 0.068(7) Uani 0.55 1 d PD A 1 H68A H 1.4131 0.6935 0.6770 0.081 Uiso 0.55 1 calc PR A 1 H68B H 1.3975 0.5894 0.6819 0.081 Uiso 0.55 1 calc PR A 1 H68C H 1.3085 0.6431 0.6496 0.081 Uiso 0.55 1 calc PR A 1 C60A C 0.953(9) 0.661(7) 0.409(3) 0.023(4) Uani 0.07 1 d PD A 2 H60C H 0.9374 0.7239 0.4131 0.028 Uiso 0.07 1 calc PR A 2 H60D H 1.0276 0.6557 0.3986 0.028 Uiso 0.07 1 calc PR A 2 C61A C 0.962(6) 0.612(12) 0.4491(18) 0.039(4) Uani 0.07 1 d PDU A 2 H61C H 0.9435 0.5487 0.4445 0.047 Uiso 0.07 1 calc PR A 2 H61D H 0.9066 0.6371 0.4655 0.047 Uiso 0.07 1 calc PR A 2 C62A C 1.087(5) 0.622(10) 0.4711(15) 0.023(4) Uani 0.07 1 d PDU A 2 H62C H 1.1382 0.5790 0.4605 0.027 Uiso 0.07 1 calc PR A 2 H62D H 1.1159 0.6821 0.4663 0.027 Uiso 0.07 1 calc PR A 2 C63A C 1.092(7) 0.608(10) 0.5161(16) 0.046(5) Uani 0.07 1 d PDU A 2 H63C H 1.0883 0.5439 0.5219 0.055 Uiso 0.07 1 calc PR A 2 H63D H 1.0242 0.6367 0.5252 0.055 Uiso 0.07 1 calc PR A 2 C64A C 1.205(8) 0.647(10) 0.5385(16) 0.032(5) Uani 0.07 1 d PDU A 2 H64C H 1.2730 0.6186 0.5292 0.039 Uiso 0.07 1 calc PR A 2 H64D H 1.2083 0.7109 0.5332 0.039 Uiso 0.07 1 calc PR A 2 C65A C 1.209(5) 0.630(8) 0.5834(16) 0.044(6) Uani 0.07 1 d PD A 2 H65C H 1.1596 0.6741 0.5944 0.053 Uiso 0.07 1 calc PR A 2 H65D H 1.1782 0.5709 0.5875 0.053 Uiso 0.07 1 calc PR A 2 C66A C 1.334(7) 0.637(5) 0.606(3) 0.049(8) Uani 0.07 1 d PD A 2 H66C H 1.3333 0.6644 0.6326 0.059 Uiso 0.07 1 calc PR A 2 H66D H 1.3810 0.6749 0.5908 0.059 Uiso 0.07 1 calc PR A 2 C67A C 1.387(10) 0.545(6) 0.611(3) 0.048(5) Uani 0.07 1 d PD A 2 H67C H 1.3251 0.4998 0.6038 0.057 Uiso 0.07 1 calc PR A 2 H67D H 1.4453 0.5373 0.5929 0.057 Uiso 0.07 1 calc PR A 2 C68A C 1.445(15) 0.531(9) 0.655(3) 0.068(7) Uani 0.07 1 d PD A 2 H68D H 1.4377 0.5854 0.6698 0.081 Uiso 0.07 1 calc PR A 2 H68E H 1.5272 0.5171 0.6553 0.081 Uiso 0.07 1 calc PR A 2 H68F H 1.4063 0.4826 0.6665 0.081 Uiso 0.07 1 calc PR A 2 C60B C 0.957(3) 0.655(3) 0.4084(10) 0.023(4) Uani 0.38 1 d PD A 4 H60E H 0.9366 0.7148 0.4165 0.028 Uiso 0.38 1 calc PR A 4 H60F H 1.0234 0.6611 0.3936 0.028 Uiso 0.38 1 calc PR A 4 C61B C 1.000(4) 0.604(3) 0.4465(11) 0.039(4) Uani 0.38 1 d PDU A 4 H61E H 1.0276 0.5450 0.4395 0.047 Uiso 0.38 1 calc PR A 4 H61F H 0.9357 0.5958 0.4620 0.047 Uiso 0.38 1 calc PR A 4 C62B C 1.100(3) 0.653(3) 0.4722(8) 0.023(4) Uani 0.38 1 d PDU A 4 H62E H 1.0756 0.7148 0.4750 0.027 Uiso 0.38 1 calc PR A 4 H62F H 1.1675 0.6533 0.4577 0.027 Uiso 0.38 1 calc PR A 4 C63B C 1.139(3) 0.615(3) 0.5139(9) 0.046(5) Uani 0.38 1 d PDU A 4 H63E H 1.0752 0.6216 0.5301 0.055 Uiso 0.38 1 calc PR A 4 H63F H 1.1554 0.5513 0.5119 0.055 Uiso 0.38 1 calc PR A 4 C64B C 1.246(3) 0.662(3) 0.5344(8) 0.032(5) Uani 0.38 1 d PDU A 4 H64E H 1.2349 0.7265 0.5305 0.039 Uiso 0.38 1 calc PR A 4 H64F H 1.3132 0.6445 0.5214 0.039 Uiso 0.38 1 calc PR A 4 C65B C 1.275(3) 0.643(3) 0.5791(7) 0.044(6) Uani 0.38 1 d PD A 4 H65E H 1.2122 0.6674 0.5925 0.053 Uiso 0.38 1 calc PR A 4 H65F H 1.2773 0.5787 0.5832 0.053 Uiso 0.38 1 calc PR A 4 C66B C 1.390(3) 0.682(3) 0.5984(7) 0.049(8) Uani 0.38 1 d PD A 4 H66E H 1.3920 0.7437 0.5888 0.059 Uiso 0.38 1 calc PR A 4 H66F H 1.4519 0.6497 0.5876 0.059 Uiso 0.38 1 calc PR A 4 C67B C 1.424(3) 0.6845(16) 0.6443(7) 0.048(5) Uani 0.38 1 d PD A 4 H67E H 1.5034 0.7096 0.6514 0.057 Uiso 0.38 1 calc PR A 4 H67F H 1.3693 0.7225 0.6561 0.057 Uiso 0.38 1 calc PR A 4 C68B C 1.422(4) 0.5930(18) 0.6606(11) 0.068(7) Uani 0.38 1 d PD A 4 H68G H 1.3485 0.5643 0.6491 0.081 Uiso 0.38 1 calc PR A 4 H68H H 1.4277 0.5955 0.6899 0.081 Uiso 0.38 1 calc PR A 4 H68I H 1.4874 0.5592 0.6535 0.081 Uiso 0.38 1 calc PR A 4 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 0.030(4) 0.013(4) 0.020(4) -0.002(3) 0.003(3) -0.007(3) O2 0.025(4) 0.027(4) 0.020(4) -0.002(3) 0.009(3) -0.002(3) O3 0.032(4) 0.023(4) 0.027(4) -0.003(3) 0.019(3) -0.004(3) O4 0.024(4) 0.024(4) 0.026(4) -0.006(3) 0.006(3) -0.002(3) O5 0.030(5) 0.073(6) 0.040(5) -0.022(5) -0.005(4) 0.020(5) O6 0.015(4) 0.034(4) 0.035(4) -0.005(3) 0.011(3) 0.001(3) O7 0.018(4) 0.040(4) 0.026(4) -0.004(3) -0.004(3) 0.003(4) O8 0.084(7) 0.069(6) 0.062(6) 0.034(5) -0.016(5) -0.044(6) C1 0.013(3) 0.012(3) 0.013(3) 0.0022(19) 0.0032(19) -0.0028(19) C2 0.011(4) 0.019(4) 0.016(4) 0.004(3) 0.007(3) -0.007(3) C3 0.011(5) 0.019(5) 0.021(5) 0.010(4) 0.006(4) -0.005(4) C4 0.016(6) 0.017(6) 0.018(6) 0.003(5) -0.004(5) -0.012(5) C5 0.011(4) 0.011(4) 0.016(4) 0.003(3) 0.003(3) -0.002(3) C6 0.012(3) 0.012(3) 0.013(3) 0.0030(19) 0.0017(19) -0.0024(19) C7 0.012(5) 0.002(5) 0.018(5) -0.002(4) 0.000(4) -0.001(4) C8 0.019(6) 0.023(6) 0.018(6) -0.003(5) 0.001(5) 0.006(5) C9 0.016(6) 0.030(6) 0.026(6) 0.003(5) -0.001(5) -0.002(5) C10 0.012(5) 0.025(5) 0.030(5) -0.006(4) 0.004(4) 0.011(4) C11 0.027(6) 0.016(6) 0.030(6) -0.010(5) 0.003(5) 0.006(5) C12 0.027(6) 0.026(6) 0.020(6) -0.006(5) 0.008(5) -0.014(5) C13 0.023(6) 0.018(6) 0.023(6) -0.016(5) 0.011(5) -0.007(5) C14 0.015(6) 0.028(6) 0.026(6) -0.013(5) 0.011(5) -0.003(5) C15 0.024(6) 0.023(6) 0.020(6) -0.001(5) 0.010(5) 0.012(5) C16 0.030(7) 0.022(6) 0.027(6) -0.004(5) 0.006(5) -0.010(5) C17 0.025(6) 0.032(6) 0.025(6) -0.006(5) -0.009(5) 0.006(5) C18 0.020(4) 0.010(4) 0.016(4) 0.004(3) -0.002(3) 0.003(3) C19 0.015(4) 0.011(4) 0.011(4) 0.007(3) 0.000(3) 0.006(3) C20 0.013(4) 0.010(4) 0.016(4) 0.003(3) 0.000(3) -0.004(3) C21 0.011(4) 0.009(4) 0.013(4) 0.000(3) 0.000(3) 0.008(3) C22 0.020(6) 0.028(6) 0.016(6) 0.001(5) 0.003(5) 0.001(5) C23 0.014(5) 0.003(5) 0.017(5) 0.002(4) -0.006(4) 0.003(4) C24 0.011(5) 0.028(5) 0.022(5) -0.002(4) -0.001(4) 0.001(4) C25 0.005(6) 0.020(6) 0.027(6) 0.006(5) -0.004(5) -0.004(5) C26 0.013(6) 0.034(7) 0.027(6) -0.006(5) 0.001(5) 0.011(5) C27 0.033(7) 0.011(6) 0.031(7) -0.005(5) 0.007(5) -0.008(5) C28 0.023(6) 0.041(7) 0.032(6) -0.001(6) 0.005(5) -0.003(6) C29 0.037(7) 0.022(6) 0.031(7) -0.005(5) 0.006(6) 0.006(5) C30 0.030(6) 0.033(6) 0.018(6) 0.004(5) 0.007(5) 0.005(5) C31 0.026(7) 0.030(6) 0.038(7) -0.014(5) 0.009(5) 0.006(5) C32 0.027(6) 0.031(6) 0.027(6) -0.004(5) 0.005(5) -0.011(5) C33 0.018(6) 0.030(7) 0.037(7) -0.007(5) 0.010(5) 0.000(5) C34 0.030(6) 0.043(7) 0.032(7) -0.008(6) -0.002(5) -0.004(6) C35 0.008(5) 0.019(5) 0.025(5) -0.013(4) 0.001(4) -0.006(4) C36 0.013(4) 0.014(4) 0.023(4) -0.004(3) 0.001(3) -0.006(3) C37 0.014(5) 0.016(5) 0.027(5) -0.008(4) 0.001(4) -0.009(4) C38 0.019(6) 0.007(5) 0.027(6) -0.001(5) 0.002(5) -0.005(5) C39 0.020(4) 0.006(4) 0.019(4) -0.005(3) -0.003(3) -0.001(3) C40 0.019(5) 0.012(5) 0.024(5) -0.011(4) -0.003(4) -0.003(4) C41 0.030(6) 0.009(6) 0.039(6) -0.005(5) 0.012(5) 0.007(5) C42 0.026(7) 0.016(6) 0.032(7) -0.010(5) -0.003(6) -0.010(5) C43 0.034(7) 0.030(7) 0.029(6) 0.001(5) 0.004(5) -0.004(6) C44 0.044(7) 0.029(7) 0.029(6) 0.000(5) 0.010(6) 0.013(6) C45 0.053(6) 0.028(6) 0.047(6) 0.023(5) -0.003(5) 0.006(5) C46 0.029(6) 0.019(6) 0.032(6) -0.010(5) -0.001(5) 0.000(5) C47 0.072(10) 0.051(8) 0.060(9) 0.033(7) -0.018(8) -0.026(8) C48 0.028(6) 0.030(6) 0.040(7) -0.005(6) 0.002(6) -0.010(6) C49 0.067(9) 0.067(9) 0.049(8) 0.006(7) 0.002(8) -0.035(8) C50 0.049(8) 0.063(9) 0.044(8) -0.017(7) -0.020(7) -0.008(7) C51 0.087(11) 0.080(11) 0.051(9) 0.004(8) 0.004(8) -0.030(9) C52 0.019(4) 0.021(4) 0.023(4) -0.002(4) 0.008(4) 0.010(4) C53 0.019(4) 0.020(4) 0.028(4) -0.006(4) 0.009(4) 0.008(4) C54 0.038(7) 0.005(6) 0.048(7) 0.001(5) 0.013(6) 0.000(5) C55 0.023(4) 0.018(4) 0.031(4) -0.003(4) 0.006(4) 0.010(4) C56 0.011(5) 0.025(5) 0.026(5) -0.002(4) 0.013(4) 0.003(4) C57 0.015(6) 0.024(6) 0.026(6) -0.005(5) 0.010(5) 0.009(5) C58 0.008(4) 0.018(4) 0.022(4) 0.000(3) 0.006(3) -0.003(3) C59 0.052(8) 0.025(7) 0.058(9) 0.004(6) 0.023(7) -0.019(6) C60 0.018(6) 0.018(5) 0.034(8) -0.002(6) 0.006(6) 0.013(5) C61 0.039(6) 0.038(6) 0.041(6) 0.002(5) 0.012(4) -0.003(5) C62 0.024(6) 0.019(5) 0.026(6) -0.004(5) 0.010(5) -0.006(4) C63 0.049(6) 0.043(6) 0.047(7) 0.000(5) 0.010(5) -0.002(5) C64 0.037(6) 0.027(6) 0.035(6) 0.003(5) 0.012(5) -0.003(5) C65 0.054(9) 0.042(10) 0.039(9) 0.003(7) 0.013(7) 0.002(8) C66 0.094(16) 0.043(17) 0.013(10) 0.008(10) 0.016(10) 0.024(13) C67 0.067(14) 0.024(12) 0.061(14) 0.011(10) 0.038(11) 0.001(10) C68 0.10(2) 0.03(2) 0.079(14) 0.009(17) 0.059(14) 0.041(16) C60A 0.018(6) 0.018(5) 0.034(8) -0.002(6) 0.006(6) 0.013(5) C61A 0.039(6) 0.038(6) 0.041(6) 0.002(5) 0.012(4) -0.003(5) C62A 0.024(6) 0.019(5) 0.026(6) -0.004(5) 0.010(5) -0.006(4) C63A 0.049(6) 0.043(6) 0.047(7) 0.000(5) 0.010(5) -0.002(5) C64A 0.037(6) 0.027(6) 0.035(6) 0.003(5) 0.012(5) -0.003(5) C65A 0.054(9) 0.042(10) 0.039(9) 0.003(7) 0.013(7) 0.002(8) C66A 0.094(16) 0.043(17) 0.013(10) 0.008(10) 0.016(10) 0.024(13) C67A 0.067(14) 0.024(12) 0.061(14) 0.011(10) 0.038(11) 0.001(10) C68A 0.10(2) 0.03(2) 0.079(14) 0.009(17) 0.059(14) 0.041(16) C60B 0.018(6) 0.018(5) 0.034(8) -0.002(6) 0.006(6) 0.013(5) C61B 0.039(6) 0.038(6) 0.041(6) 0.002(5) 0.012(4) -0.003(5) C62B 0.024(6) 0.019(5) 0.026(6) -0.004(5) 0.010(5) -0.006(4) C63B 0.049(6) 0.043(6) 0.047(7) 0.000(5) 0.010(5) -0.002(5) C64B 0.037(6) 0.027(6) 0.035(6) 0.003(5) 0.012(5) -0.003(5) C65B 0.054(9) 0.042(10) 0.039(9) 0.003(7) 0.013(7) 0.002(8) C66B 0.094(16) 0.043(17) 0.013(10) 0.008(10) 0.016(10) 0.024(13) C67B 0.067(14) 0.024(12) 0.061(14) 0.011(10) 0.038(11) 0.001(10) C68B 0.10(2) 0.03(2) 0.079(14) 0.009(17) 0.059(14) 0.041(16) _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 1.384(10) . ? O2 C18 1.390(11) . ? O3 C35 1.379(11) . ? O4 C52 1.367(11) . ? O5 C8 1.204(11) . ? O6 C25 1.217(10) . ? O7 C42 1.222(11) . ? O8 C59 1.230(12) . ? C1 C2 1.377(12) . ? C1 C6 1.403(12) . ? C2 C3 1.395(12) . ? C2 C58 1.505(12) . ? C3 C4 1.376(12) . ? C4 C5 1.372(12) . ? C4 C8 1.508(13) . ? C5 C6 1.383(12) . ? C6 C7 1.516(12) . ? C7 C19 1.497(12) . ? C8 C9 1.511(13) . ? C9 C10 1.511(12) . ? C10 C11 1.513(12) . ? C11 C12 1.538(12) . ? C12 C13 1.501(13) . ? C13 C14 1.506(12) . ? C14 C15 1.549(12) . ? C15 C16 1.497(12) . ? C16 C17 1.497(13) . ? C18 C19 1.393(12) . ? C18 C23 1.395(12) . ? C19 C20 1.377(12) . ? C20 C21 1.399(12) . ? C21 C22 1.376(12) . ? C21 C25 1.497(13) . ? C22 C23 1.384(12) . ? C23 C24 1.526(12) . ? C24 C36 1.510(12) . ? C25 C26 1.481(13) . ? C26 C27 1.520(12) . ? C27 C28 1.503(13) . ? C28 C29 1.506(13) . ? C29 C30 1.505(13) . ? C30 C31 1.512(13) . ? C31 C32 1.527(13) . ? C32 C33 1.505(13) . ? C33 C34 1.513(13) . ? C35 C40 1.383(13) . ? C35 C36 1.400(12) . ? C36 C37 1.383(12) . ? C37 C38 1.390(12) . ? C38 C39 1.413(12) . ? C38 C42 1.494(13) . ? C39 C40 1.394(12) . ? C40 C41 1.528(13) . ? C41 C53 1.513(13) . ? C42 C43 1.507(13) . ? C43 C44 1.533(14) . ? C44 C45 1.498(13) . ? C45 C46 1.508(14) . ? C46 C47 1.498(14) . ? C47 C48 1.453(14) . ? C48 C49 1.458(14) . ? C49 C50 1.445(15) . ? C50 C51 1.441(16) . ? C52 C53 1.393(13) . ? C52 C57 1.409(13) . ? C53 C54 1.389(13) . ? C54 C55 1.385(13) . ? C55 C56 1.396(13) . ? C55 C59 1.470(14) . ? C56 C57 1.387(13) . ? C57 C58 1.516(13) . ? C59 C60 1.502(16) . ? C59 C60B 1.511(18) . ? C59 C60A 1.52(2) . ? C60 C61 1.531(17) . ? C61 C62 1.519(17) . ? C62 C63 1.524(16) . ? C63 C64 1.497(17) . ? C64 C65 1.514(17) . ? C65 C66 1.502(17) . ? C66 C67 1.528(17) . ? C67 C68 1.496(17) . ? C60A C61A 1.53(2) . ? C61A C62A 1.53(2) . ? C62A C63A 1.53(2) . ? C63A C64A 1.53(2) . ? C64A C65A 1.53(2) . ? C65A C66A 1.53(2) . ? C66A C67A 1.53(2) . ? C67A C68A 1.53(2) . ? C60B C61B 1.515(19) . ? C61B C62B 1.521(19) . ? C62B C63B 1.522(19) . ? C63B C64B 1.511(19) . ? C64B C65B 1.518(19) . ? C65B C66B 1.509(19) . ? C66B C67B 1.535(19) . ? C67B C68B 1.495(19) . ? 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 C2 C1 O1 119.7(8) . . ? C2 C1 C6 122.5(8) . . ? O1 C1 C6 117.7(8) . . ? C1 C2 C3 117.0(8) . . ? C1 C2 C58 122.2(8) . . ? C3 C2 C58 120.8(8) . . ? C4 C3 C2 122.0(8) . . ? C5 C4 C3 119.2(8) . . ? C5 C4 C8 118.2(9) . . ? C3 C4 C8 122.6(8) . . ? C4 C5 C6 121.5(8) . . ? C5 C6 C1 117.7(8) . . ? C5 C6 C7 119.7(8) . . ? C1 C6 C7 122.6(8) . . ? C19 C7 C6 113.2(7) . . ? O5 C8 C4 119.9(8) . . ? O5 C8 C9 120.4(8) . . ? C4 C8 C9 119.6(9) . . ? C10 C9 C8 113.6(8) . . ? C9 C10 C11 112.3(7) . . ? C10 C11 C12 114.2(8) . . ? C13 C12 C11 113.5(8) . . ? C12 C13 C14 113.8(7) . . ? C13 C14 C15 113.4(7) . . ? C16 C15 C14 114.2(7) . . ? C15 C16 C17 113.8(8) . . ? O2 C18 C19 118.7(8) . . ? O2 C18 C23 118.1(8) . . ? C19 C18 C23 123.2(8) . . ? C20 C19 C18 116.8(8) . . ? C20 C19 C7 120.5(8) . . ? C18 C19 C7 122.5(8) . . ? C19 C20 C21 122.9(8) . . ? C22 C21 C20 117.2(8) . . ? C22 C21 C25 119.4(8) . . ? C20 C21 C25 123.3(8) . . ? C21 C22 C23 123.4(9) . . ? C22 C23 C18 116.5(8) . . ? C22 C23 C24 120.0(8) . . ? C18 C23 C24 123.5(8) . . ? C36 C24 C23 111.0(7) . . ? O6 C25 C26 122.7(9) . . ? O6 C25 C21 118.7(8) . . ? C26 C25 C21 118.5(8) . . ? C25 C26 C27 113.7(8) . . ? C28 C27 C26 114.9(8) . . ? C27 C28 C29 115.0(9) . . ? C30 C29 C28 114.9(8) . . ? C29 C30 C31 115.4(8) . . ? C30 C31 C32 114.4(8) . . ? C33 C32 C31 114.1(8) . . ? C32 C33 C34 113.4(8) . . ? O3 C35 C40 119.2(8) . . ? O3 C35 C36 118.0(8) . . ? C40 C35 C36 122.8(9) . . ? C37 C36 C35 118.5(9) . . ? C37 C36 C24 117.3(8) . . ? C35 C36 C24 124.0(8) . . ? C36 C37 C38 120.7(9) . . ? C37 C38 C39 119.6(8) . . ? C37 C38 C42 119.6(9) . . ? C39 C38 C42 120.8(8) . . ? C40 C39 C38 120.6(8) . . ? C35 C40 C39 117.8(8) . . ? C35 C40 C41 122.6(8) . . ? C39 C40 C41 119.6(8) . . ? C53 C41 C40 111.7(7) . . ? O7 C42 C38 119.1(9) . . ? O7 C42 C43 120.3(9) . . ? C38 C42 C43 120.5(9) . . ? C42 C43 C44 111.9(8) . . ? C45 C44 C43 115.7(9) . . ? C44 C45 C46 114.2(9) . . ? C47 C46 C45 118.0(9) . . ? C48 C47 C46 117.1(9) . . ? C47 C48 C49 119.9(10) . . ? C50 C49 C48 121.1(11) . . ? C51 C50 C49 121.5(12) . . ? O4 C52 C53 120.1(9) . . ? O4 C52 C57 117.4(9) . . ? C53 C52 C57 122.6(9) . . ? C54 C53 C52 117.7(9) . . ? C54 C53 C41 121.3(9) . . ? C52 C53 C41 121.0(9) . . ? C55 C54 C53 122.5(9) . . ? C54 C55 C56 117.7(9) . . ? C54 C55 C59 120.6(9) . . ? C56 C55 C59 121.7(9) . . ? C57 C56 C55 123.0(9) . . ? C56 C57 C52 116.6(9) . . ? C56 C57 C58 119.9(9) . . ? C52 C57 C58 123.2(9) . . ? C2 C58 C57 113.1(7) . . ? O8 C59 C55 117.6(9) . . ? O8 C59 C60 124.6(13) . . ? C55 C59 C60 117.7(13) . . ? O8 C59 C60B 115.6(17) . . ? C55 C59 C60B 125.8(17) . . ? C60 C59 C60B 11(3) . . ? O8 C59 C60A 116(3) . . ? C55 C59 C60A 124(3) . . ? C60 C59 C60A 13(6) . . ? C60B C59 C60A 4(7) . . ? C59 C60 C61 112.3(16) . . ? C62 C61 C60 109.3(16) . . ? C61 C62 C63 113.7(16) . . ? C64 C63 C62 115.5(17) . . ? C63 C64 C65 115.4(17) . . ? C66 C65 C64 113.5(16) . . ? C65 C66 C67 118.2(19) . . ? C68 C67 C66 112.6(17) . . ? C59 C60A C61A 110(3) . . ? C60A C61A C62A 108(3) . . ? C63A C62A C61A 110(3) . . ? C62A C63A C64A 109(3) . . ? C65A C64A C63A 108(3) . . ? C66A C65A C64A 111(3) . . ? C65A C66A C67A 109(4) . . ? C68A C67A C66A 110(4) . . ? C59 C60B C61B 121(2) . . ? C60B C61B C62B 111(2) . . ? C61B C62B C63B 116(2) . . ? C64B C63B C62B 110(2) . . ? C63B C64B C65B 114(2) . . ? C66B C65B C64B 113(2) . . ? C65B C66B C67B 121(2) . . ? C68B C67B C66B 109(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.419 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.082 # Attachment 'gena66a_C8n.cif' data_gena66a _database_code_depnum_ccdc_archive 'CCDC 632669' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common para-octanoylcalix(4)arene _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H80 O8' _chemical_formula_weight 929.24 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 21.7615(12) _cell_length_b 15.6647(8) _cell_length_c 32.8323(16) _cell_angle_alpha 90.00 _cell_angle_beta 107.905(3) _cell_angle_gamma 90.00 _cell_volume 10650.1(10) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.159 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4032 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9563 _exptl_absorpt_correction_T_max 0.9706 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71070 _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 160632 _diffrn_reflns_av_R_equivalents 0.1461 _diffrn_reflns_av_sigmaI/netI 0.0925 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 26.34 _reflns_number_total 21484 _reflns_number_gt 10048 _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^)+(0.1224P)^2^+15.8509P] 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 21484 _refine_ls_number_parameters 1473 _refine_ls_number_restraints 290 _refine_ls_R_factor_all 0.1881 _refine_ls_R_factor_gt 0.0839 _refine_ls_wR_factor_ref 0.2921 _refine_ls_wR_factor_gt 0.2006 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.038 _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 O6A O 0.47833(11) 0.70564(15) 0.25216(6) 0.0521(6) Uani 0.831(2) 1 d PD A -7 C23A C 0.46172(12) 0.71646(18) 0.21342(8) 0.0355(7) Uani 0.831(2) 1 d PD A -7 C24A C 0.39739(12) 0.6830(2) 0.18574(8) 0.0433(7) Uani 0.831(2) 1 d PD A -7 H24X H 0.4048 0.6307 0.1710 0.052 Uiso 0.831(2) 1 calc PR A -7 H24Y H 0.3774 0.7260 0.1636 0.052 Uiso 0.831(2) 1 calc PR A -7 C25A C 0.35062(13) 0.6624(3) 0.21057(10) 0.0698(11) Uani 0.831(2) 1 d PD A -7 H25X H 0.3681 0.6140 0.2301 0.084 Uiso 0.831(2) 1 calc PR A -7 H25Y H 0.3480 0.7123 0.2285 0.084 Uiso 0.831(2) 1 calc PR A -7 C26A C 0.28278(14) 0.6397(3) 0.18263(12) 0.0808(15) Uani 0.831(2) 1 d PD A -7 H26X H 0.2855 0.5888 0.1654 0.097 Uiso 0.831(2) 1 calc PR A -7 H26Y H 0.2569 0.6237 0.2015 0.097 Uiso 0.831(2) 1 calc PR A -7 C27A C 0.24738(15) 0.7090(3) 0.15271(13) 0.0767(14) Uani 0.831(2) 1 d PD A -7 H27X H 0.2674 0.7153 0.1296 0.092 Uiso 0.831(2) 1 calc PR A -7 H27Y H 0.2538 0.7635 0.1688 0.092 Uiso 0.831(2) 1 calc PR A -7 C28A C 0.17513(16) 0.6954(3) 0.13224(13) 0.0836(15) Uani 0.831(2) 1 d PD A -7 H28X H 0.1550 0.6906 0.1554 0.100 Uiso 0.831(2) 1 calc PR A -7 H28Y H 0.1570 0.7470 0.1154 0.100 Uiso 0.831(2) 1 calc PR A -7 C29A C 0.15562(16) 0.6201(3) 0.10394(13) 0.0889(15) Uani 0.831(2) 1 d PD A -7 H29X H 0.1728 0.5681 0.1207 0.107 Uiso 0.831(2) 1 calc PR A -7 H29Y H 0.1757 0.6243 0.0807 0.107 Uiso 0.831(2) 1 calc PR A -7 C30A C 0.08355(15) 0.6104(3) 0.08415(13) 0.0774(14) Uani 0.831(2) 1 d PD A -7 H30X H 0.0629 0.6092 0.1068 0.093 Uiso 0.831(2) 1 calc PR A -7 H30Y H 0.0743 0.5570 0.0678 0.093 Uiso 0.831(2) 1 calc PR A -7 H30Z H 0.0667 0.6587 0.0650 0.093 Uiso 0.831(2) 1 calc PR A -7 O6K O 0.4784(5) 0.6967(8) 0.2502(2) 0.0521(6) Uani 0.169(2) 1 d PD A -27 C23K C 0.4646(3) 0.7039(8) 0.2112(2) 0.0355(7) Uani 0.169(2) 1 d PD A -27 C24K C 0.3945(2) 0.6896(7) 0.1842(2) 0.0433(7) Uani 0.169(2) 1 d PD A -27 H24S H 0.3928 0.6488 0.1609 0.052 Uiso 0.169(2) 1 calc PR A -27 H24T H 0.3754 0.7442 0.1711 0.052 Uiso 0.169(2) 1 calc PR A -27 C25K C 0.3553(3) 0.6543(6) 0.2119(2) 0.0698(11) Uani 0.169(2) 1 d PD A -27 H25S H 0.3367 0.7023 0.2239 0.084 Uiso 0.169(2) 1 calc PR A -27 H25T H 0.3841 0.6215 0.2361 0.084 Uiso 0.169(2) 1 calc PR A -27 C26K C 0.3008(3) 0.5965(5) 0.1858(3) 0.0808(15) Uani 0.169(2) 1 d PD A -27 H26S H 0.3188 0.5523 0.1711 0.097 Uiso 0.169(2) 1 calc PR A -27 H26T H 0.2805 0.5673 0.2051 0.097 Uiso 0.169(2) 1 calc PR A -27 C27K C 0.2501(3) 0.6485(6) 0.1527(4) 0.0767(14) Uani 0.169(2) 1 d PD A -27 H27S H 0.2427 0.7030 0.1657 0.092 Uiso 0.169(2) 1 calc PR A -27 H27T H 0.2661 0.6621 0.1283 0.092 Uiso 0.169(2) 1 calc PR A -27 C28K C 0.1868(2) 0.6002(5) 0.1364(4) 0.0836(15) Uani 0.169(2) 1 d PD A -27 H28S H 0.1826 0.5781 0.1075 0.100 Uiso 0.169(2) 1 calc PR A -27 H28T H 0.1883 0.5505 0.1554 0.100 Uiso 0.169(2) 1 calc PR A -27 C29K C 0.1276(3) 0.6526(8) 0.1343(2) 0.0889(15) Uani 0.169(2) 1 d PD A -27 H29S H 0.0888 0.6192 0.1190 0.107 Uiso 0.169(2) 1 calc PR A -27 H29T H 0.1280 0.7047 0.1173 0.107 Uiso 0.169(2) 1 calc PR A -27 C30K C 0.1223(6) 0.6790(10) 0.1777(3) 0.0774(14) Uani 0.169(2) 1 d PD A -27 H30S H 0.0879 0.6461 0.1839 0.093 Uiso 0.169(2) 1 calc PR A -27 H30T H 0.1123 0.7400 0.1773 0.093 Uiso 0.169(2) 1 calc PR A -27 H30P H 0.1634 0.6678 0.1999 0.093 Uiso 0.169(2) 1 calc PR A -27 O5A O 0.30230(10) 0.77960(13) -0.01923(6) 0.0462(5) Uani 0.826(2) 1 d PD B -6 C8A C 0.31182(13) 0.85668(18) -0.01723(8) 0.0376(7) Uani 0.826(2) 1 d PD B -6 C9A C 0.25909(13) 0.91751(18) -0.04109(7) 0.0390(7) Uani 0.826(2) 1 d PD B -6 H9A1 H 0.2588 0.9675 -0.0227 0.047 Uiso 0.826(2) 1 calc PR B -6 H9A2 H 0.2167 0.8886 -0.0473 0.047 Uiso 0.826(2) 1 calc PR B -6 C10A C 0.26810(13) 0.94826(19) -0.08311(8) 0.0411(8) Uani 0.826(2) 1 d PD B -6 H10A H 0.2811 0.8994 -0.0978 0.049 Uiso 0.826(2) 1 calc PR B -6 H10B H 0.3032 0.9911 -0.0768 0.049 Uiso 0.826(2) 1 calc PR B -6 C11A C 0.20604(13) 0.9879(2) -0.11291(8) 0.0447(9) Uani 0.826(2) 1 d PD B -6 H11A H 0.1733 0.9425 -0.1234 0.054 Uiso 0.826(2) 1 calc PR B -6 H11B H 0.1887 1.0295 -0.0966 0.054 Uiso 0.826(2) 1 calc PR B -6 C12A C 0.21775(13) 1.0327(2) -0.15103(8) 0.0476(9) Uani 0.826(2) 1 d PD B -6 H12A H 0.2390 0.9925 -0.1657 0.057 Uiso 0.826(2) 1 calc PR B -6 H12B H 0.2474 1.0815 -0.1406 0.057 Uiso 0.826(2) 1 calc PR B -6 C13A C 0.15547(15) 1.0653(2) -0.18307(9) 0.0622(11) Uani 0.826(2) 1 d PD B -6 H13A H 0.1338 1.1045 -0.1682 0.075 Uiso 0.826(2) 1 calc PR B -6 H13B H 0.1262 1.0163 -0.1937 0.075 Uiso 0.826(2) 1 calc PR B -6 C14A C 0.16611(16) 1.1117(2) -0.22118(10) 0.0632(12) Uani 0.826(2) 1 d PD B -6 H14A H 0.1915 1.0743 -0.2343 0.076 Uiso 0.826(2) 1 calc PR B -6 H14B H 0.1236 1.1216 -0.2428 0.076 Uiso 0.826(2) 1 calc PR B -6 C15A C 0.20081(18) 1.1969(2) -0.21012(13) 0.0733(12) Uani 0.826(2) 1 d PD B -6 H15A H 0.1754 1.2352 -0.1979 0.088 Uiso 0.826(2) 1 calc PR B -6 H15B H 0.2059 1.2226 -0.2361 0.088 Uiso 0.826(2) 1 calc PR B -6 H15C H 0.2434 1.1878 -0.1892 0.088 Uiso 0.826(2) 1 calc PR B -6 O5K O 0.2940(4) 0.7915(4) -0.0226(3) 0.0462(5) Uani 0.174(2) 1 d PD B -16 C8K C 0.3099(3) 0.8664(4) -0.0183(3) 0.0376(7) Uani 0.174(2) 1 d PD B -16 C9K C 0.2594(4) 0.9358(5) -0.03568(17) 0.0390(7) Uani 0.174(2) 1 d PD B -16 H9K1 H 0.2762 0.9915 -0.0227 0.047 Uiso 0.174(2) 1 calc PR B -16 H9K2 H 0.2198 0.9225 -0.0281 0.047 Uiso 0.174(2) 1 calc PR B -16 C10K C 0.2434(3) 0.9409(7) -0.08436(18) 0.0411(8) Uani 0.174(2) 1 d PD B -16 H10C H 0.2752 0.9782 -0.0918 0.049 Uiso 0.174(2) 1 calc PR B -16 H10D H 0.2463 0.8833 -0.0960 0.049 Uiso 0.174(2) 1 calc PR B -16 C11K C 0.1754(3) 0.9766(7) -0.10425(17) 0.0447(9) Uani 0.174(2) 1 d PD B -16 H11C H 0.1708 1.0313 -0.0904 0.054 Uiso 0.174(2) 1 calc PR B -16 H11D H 0.1431 0.9360 -0.0999 0.054 Uiso 0.174(2) 1 calc PR B -16 C12K C 0.1639(4) 0.9907(4) -0.15222(18) 0.0476(9) Uani 0.174(2) 1 d PD B -16 H12C H 0.1856 0.9451 -0.1636 0.057 Uiso 0.174(2) 1 calc PR B -16 H12D H 0.1170 0.9880 -0.1676 0.057 Uiso 0.174(2) 1 calc PR B -16 C13K C 0.1903(5) 1.0777(5) -0.15970(18) 0.0622(11) Uani 0.174(2) 1 d PD B -16 H13C H 0.2355 1.0839 -0.1410 0.075 Uiso 0.174(2) 1 calc PR B -16 H13D H 0.1643 1.1237 -0.1525 0.075 Uiso 0.174(2) 1 calc PR B -16 C14K C 0.1877(6) 1.0851(4) -0.2066(2) 0.0632(12) Uani 0.174(2) 1 d PD B -16 H14C H 0.2230 1.0509 -0.2115 0.076 Uiso 0.174(2) 1 calc PR B -16 H14D H 0.1462 1.0618 -0.2251 0.076 Uiso 0.174(2) 1 calc PR B -16 C15K C 0.1943(9) 1.1779(5) -0.2187(4) 0.0733(12) Uani 0.174(2) 1 d PD B -16 H15D H 0.1631 1.2131 -0.2102 0.088 Uiso 0.174(2) 1 calc PR B -16 H15E H 0.1858 1.1822 -0.2498 0.088 Uiso 0.174(2) 1 calc PR B -16 H15F H 0.2382 1.1980 -0.2040 0.088 Uiso 0.174(2) 1 calc PR B -16 O6 O 0.30623(10) 1.19007(16) -0.05007(8) 0.0602(7) Uani 0.8086(19) 1 d PD C -5 C23 C 0.25354(15) 1.2228(2) -0.06586(9) 0.0496(8) Uani 0.8086(19) 1 d PD C -5 C24 C 0.24566(14) 1.29985(19) -0.09461(10) 0.0546(10) Uani 0.8086(19) 1 d PD C -5 H24A H 0.2360 1.3498 -0.0791 0.066 Uiso 0.8086(19) 1 calc PR C -5 H24B H 0.2076 1.2904 -0.1201 0.066 Uiso 0.8086(19) 1 calc PR C -5 C25 C 0.30283(14) 1.32223(19) -0.10998(11) 0.0551(10) Uani 0.8086(19) 1 d PD C -5 H25A H 0.3093 1.2764 -0.1290 0.066 Uiso 0.8086(19) 1 calc PR C -5 H25B H 0.3424 1.3261 -0.0851 0.066 Uiso 0.8086(19) 1 calc PR C -5 C26 C 0.29191(15) 1.4070(2) -0.13413(12) 0.0786(13) Uani 0.8086(19) 1 d PD C -5 H26A H 0.2508 1.4035 -0.1578 0.094 Uiso 0.8086(19) 1 calc PR C -5 H26B H 0.2871 1.4526 -0.1144 0.094 Uiso 0.8086(19) 1 calc PR C -5 C27 C 0.34511(17) 1.4323(2) -0.15250(11) 0.0851(14) Uani 0.8086(19) 1 d PD C -5 H27A H 0.3397 1.4933 -0.1607 0.102 Uiso 0.8086(19) 1 calc PR C -5 H27B H 0.3872 1.4262 -0.1299 0.102 Uiso 0.8086(19) 1 calc PR C -5 C28 C 0.34681(17) 1.3806(2) -0.19106(11) 0.0766(14) Uani 0.8086(19) 1 d PD C -5 H28A H 0.3862 1.3963 -0.1983 0.092 Uiso 0.8086(19) 1 calc PR C -5 H28B H 0.3505 1.3195 -0.1830 0.092 Uiso 0.8086(19) 1 calc PR C -5 C29 C 0.2897(2) 1.3913(3) -0.23031(12) 0.0991(19) Uani 0.8086(19) 1 d PD C -5 H29A H 0.2823 1.4529 -0.2364 0.119 Uiso 0.8086(19) 1 calc PR C -5 H29B H 0.2510 1.3678 -0.2246 0.119 Uiso 0.8086(19) 1 calc PR C -5 C30 C 0.2983(2) 1.3469(3) -0.26993(12) 0.1028(18) Uani 0.8086(19) 1 d PD C -5 H30A H 0.3025 1.2852 -0.2649 0.123 Uiso 0.8086(19) 1 calc PR C -5 H30B H 0.3373 1.3687 -0.2754 0.123 Uiso 0.8086(19) 1 calc PR C -5 H30C H 0.2606 1.3585 -0.2948 0.123 Uiso 0.8086(19) 1 calc PR C -5 O6F O 0.3090(3) 1.1742(6) -0.0383(3) 0.0602(7) Uani 0.1914(19) 1 d PD C -15 C23F C 0.2608(4) 1.2144(6) -0.0584(2) 0.0496(8) Uani 0.1914(19) 1 d PD C -15 C24F C 0.2616(5) 1.2534(3) -0.1010(2) 0.0546(10) Uani 0.1914(19) 1 d PD C -15 H24C H 0.2989 1.2311 -0.1089 0.066 Uiso 0.1914(19) 1 calc PR C -15 H24D H 0.2216 1.2374 -0.1238 0.066 Uiso 0.1914(19) 1 calc PR C -15 C25F C 0.2662(5) 1.3503(3) -0.09704(19) 0.0551(10) Uani 0.1914(19) 1 d PD C -15 H25C H 0.3088 1.3660 -0.0769 0.066 Uiso 0.1914(19) 1 calc PR C -15 H25D H 0.2326 1.3713 -0.0849 0.066 Uiso 0.1914(19) 1 calc PR C -15 C26F C 0.2576(3) 1.3942(5) -0.13995(18) 0.0786(13) Uani 0.1914(19) 1 d PD C -15 H26C H 0.2141 1.3806 -0.1595 0.094 Uiso 0.1914(19) 1 calc PR C -15 H26D H 0.2599 1.4568 -0.1355 0.094 Uiso 0.1914(19) 1 calc PR C -15 C27F C 0.3079(3) 1.3680(5) -0.1612(2) 0.0851(14) Uani 0.1914(19) 1 d PD C -15 H27E H 0.2958 1.3121 -0.1754 0.102 Uiso 0.1914(19) 1 calc PR C -15 H27F H 0.3503 1.3613 -0.1389 0.102 Uiso 0.1914(19) 1 calc PR C -15 C28F C 0.3141(3) 1.4337(5) -0.19423(19) 0.0766(14) Uani 0.1914(19) 1 d PD C -15 H28E H 0.3360 1.4853 -0.1791 0.092 Uiso 0.1914(19) 1 calc PR C -15 H28F H 0.2704 1.4506 -0.2123 0.092 Uiso 0.1914(19) 1 calc PR C -15 C29F C 0.3523(4) 1.3993(5) -0.2230(2) 0.0991(19) Uani 0.1914(19) 1 d PD C -15 H29C H 0.3649 1.4471 -0.2385 0.119 Uiso 0.1914(19) 1 calc PR C -15 H29D H 0.3922 1.3709 -0.2052 0.119 Uiso 0.1914(19) 1 calc PR C -15 C30F C 0.3108(7) 1.3354(6) -0.2551(3) 0.1028(18) Uani 0.1914(19) 1 d PD C -15 H30D H 0.3379 1.3050 -0.2694 0.123 Uiso 0.1914(19) 1 calc PR C -15 H30E H 0.2765 1.3659 -0.2766 0.123 Uiso 0.1914(19) 1 calc PR C -15 H30F H 0.2916 1.2943 -0.2401 0.123 Uiso 0.1914(19) 1 calc PR C -15 O7A O 0.55632(12) 1.16096(15) 0.33569(6) 0.0636(6) Uani 0.8208(19) 1 d PD A -4 C38A C 0.57955(15) 1.09392(19) 0.32993(8) 0.0436(8) Uani 0.8208(19) 1 d PD A -4 C39A C 0.59979(15) 1.02801(18) 0.36515(7) 0.0417(8) Uani 0.8208(19) 1 d PD A -4 H39A H 0.5762 0.9742 0.3550 0.050 Uiso 0.8208(19) 1 calc PR A -4 H39B H 0.6465 1.0163 0.3714 0.050 Uiso 0.8208(19) 1 calc PR A -4 C40A C 0.58703(15) 1.05560(19) 0.40589(7) 0.0443(9) Uani 0.8208(19) 1 d PD A -4 H40A H 0.5399 1.0625 0.4002 0.053 Uiso 0.8208(19) 1 calc PR A -4 H40B H 0.6076 1.1118 0.4148 0.053 Uiso 0.8208(19) 1 calc PR A -4 C41A C 0.61261(18) 0.9920(2) 0.44208(8) 0.0576(10) Uani 0.8208(19) 1 d PD A -4 H41A H 0.6593 0.9831 0.4468 0.069 Uiso 0.8208(19) 1 calc PR A -4 H41B H 0.5906 0.9365 0.4336 0.069 Uiso 0.8208(19) 1 calc PR A -4 C42A C 0.60233(18) 1.0218(2) 0.48409(9) 0.0640(11) Uani 0.8208(19) 1 d PD A -4 H42A H 0.5557 1.0325 0.4789 0.077 Uiso 0.8208(19) 1 calc PR A -4 H42B H 0.6154 0.9753 0.5054 0.077 Uiso 0.8208(19) 1 calc PR A -4 C43A C 0.6397(2) 1.1020(2) 0.50269(9) 0.0777(15) Uani 0.8208(19) 1 d PD A -4 H43A H 0.6252 1.1489 0.4817 0.093 Uiso 0.8208(19) 1 calc PR A -4 H43B H 0.6860 1.0919 0.5066 0.093 Uiso 0.8208(19) 1 calc PR A -4 C44A C 0.63240(19) 1.1309(3) 0.54540(10) 0.1008(19) Uani 0.8208(19) 1 d PD A -4 H44A H 0.6420 1.0823 0.5657 0.121 Uiso 0.8208(19) 1 calc PR A -4 H44B H 0.6640 1.1767 0.5576 0.121 Uiso 0.8208(19) 1 calc PR A -4 C45A C 0.56535(19) 1.1632(3) 0.54018(13) 0.1057(17) Uani 0.8208(19) 1 d PDU A -4 H45A H 0.5532 1.2050 0.5169 0.127 Uiso 0.8208(19) 1 calc PR A -4 H45B H 0.5643 1.1903 0.5668 0.127 Uiso 0.8208(19) 1 calc PR A -4 H45C H 0.5349 1.1153 0.5334 0.127 Uiso 0.8208(19) 1 calc PR A -4 O7K O 0.5521(5) 1.1472(5) 0.3378(3) 0.0636(6) Uani 0.1792(19) 1 d PD A -14 C38K C 0.5737(5) 1.0805(4) 0.3299(2) 0.0436(8) Uani 0.1792(19) 1 d PD A -14 C39K C 0.5768(4) 1.0034(4) 0.35840(16) 0.0417(8) Uani 0.1792(19) 1 d PD A -14 H39C H 0.6226 0.9863 0.3708 0.050 Uiso 0.1792(19) 1 calc PR A -14 H39D H 0.5537 0.9555 0.3405 0.050 Uiso 0.1792(19) 1 calc PR A -14 C40K C 0.5479(3) 1.0174(6) 0.39496(16) 0.0443(9) Uani 0.1792(19) 1 d PD A -14 H40C H 0.5101 1.0558 0.3850 0.053 Uiso 0.1792(19) 1 calc PR A -14 H40D H 0.5327 0.9620 0.4028 0.053 Uiso 0.1792(19) 1 calc PR A -14 C41K C 0.5966(3) 1.0561(6) 0.43437(17) 0.0576(10) Uani 0.1792(19) 1 d PD A -14 H41C H 0.6175 1.1060 0.4257 0.069 Uiso 0.1792(19) 1 calc PR A -14 H41D H 0.6306 1.0135 0.4474 0.069 Uiso 0.1792(19) 1 calc PR A -14 C42K C 0.5645(4) 1.0842(7) 0.46768(17) 0.0640(11) Uani 0.1792(19) 1 d PD A -14 H42C H 0.5322 1.1292 0.4554 0.077 Uiso 0.1792(19) 1 calc PR A -14 H42D H 0.5421 1.0351 0.4758 0.077 Uiso 0.1792(19) 1 calc PR A -14 C43K C 0.6160(4) 1.1184(7) 0.50714(18) 0.0777(15) Uani 0.1792(19) 1 d PD A -14 H43C H 0.6354 1.1707 0.4994 0.093 Uiso 0.1792(19) 1 calc PR A -14 H43D H 0.6506 1.0754 0.5175 0.093 Uiso 0.1792(19) 1 calc PR A -14 C44K C 0.5866(4) 1.1388(7) 0.5427(2) 0.1008(19) Uani 0.1792(19) 1 d PD A -14 H44C H 0.5772 1.0853 0.5556 0.121 Uiso 0.1792(19) 1 calc PR A -14 H44D H 0.5457 1.1706 0.5308 0.121 Uiso 0.1792(19) 1 calc PR A -14 C45K C 0.6347(7) 1.1928(8) 0.5766(3) 0.1057(17) Uani 0.1792(19) 1 d PDU A -14 H45D H 0.6690 1.1560 0.5944 0.127 Uiso 0.1792(19) 1 calc PR A -14 H45E H 0.6123 1.2208 0.5947 0.127 Uiso 0.1792(19) 1 calc PR A -14 H45F H 0.6537 1.2362 0.5626 0.127 Uiso 0.1792(19) 1 calc PR A -14 O8A O 0.2945(3) 1.2006(3) 0.09697(17) 0.0597(8) Uani 0.33 1 d PD A -31 C53A C 0.3437(2) 1.2327(4) 0.12151(16) 0.0393(9) Uani 0.33 1 d PD A -31 C54A C 0.3401(2) 1.2813(4) 0.16090(17) 0.0597(14) Uani 0.33 1 d PD A -31 H54A H 0.3718 1.3286 0.1670 0.072 Uiso 0.33 1 calc PR A -31 H54B H 0.3516 1.2425 0.1859 0.072 Uiso 0.33 1 calc PR A -31 C55A C 0.2727(3) 1.3175(4) 0.1545(2) 0.076(2) Uani 0.33 1 d PD A -31 H55A H 0.2545 1.3375 0.1246 0.091 Uiso 0.33 1 calc PR A -31 H55B H 0.2443 1.2717 0.1592 0.091 Uiso 0.33 1 calc PR A -31 C56A C 0.2731(4) 1.3909(4) 0.18458(15) 0.085(2) Uani 0.33 1 d PD A -31 H56A H 0.2303 1.4189 0.1753 0.102 Uiso 0.33 1 calc PR A -31 H56B H 0.3054 1.4335 0.1820 0.102 Uiso 0.33 1 calc PR A -31 C57A C 0.2886(5) 1.3656(4) 0.23139(14) 0.0714(16) Uani 0.33 1 d PD A -31 H57A H 0.3326 1.3411 0.2419 0.086 Uiso 0.33 1 calc PR A -31 H57B H 0.2574 1.3220 0.2347 0.086 Uiso 0.33 1 calc PR A -31 C58A C 0.2840(6) 1.4459(4) 0.25713(14) 0.096(2) Uani 0.33 1 d PD A -31 H58A H 0.3102 1.4919 0.2499 0.115 Uiso 0.33 1 calc PR A -31 H58B H 0.2386 1.4655 0.2486 0.115 Uiso 0.33 1 calc PR A -31 C59A C 0.3073(5) 1.4314(4) 0.30519(16) 0.101(3) Uani 0.33 1 d PDU A -31 H59A H 0.3526 1.4111 0.3145 0.121 Uiso 0.33 1 calc PR A -31 H59B H 0.2800 1.3883 0.3134 0.121 Uiso 0.33 1 calc PR A -31 C60A C 0.3020(5) 1.5192(4) 0.3262(2) 0.0744(18) Uani 0.33 1 d PDU A -31 H60A H 0.3311 1.5603 0.3191 0.089 Uiso 0.33 1 calc PR A -31 H60B H 0.3141 1.5124 0.3574 0.089 Uiso 0.33 1 calc PR A -31 H60C H 0.2575 1.5401 0.3154 0.089 Uiso 0.33 1 calc PR A -31 O8K O 0.2933(2) 1.1999(3) 0.09640(15) 0.0597(8) Uani 0.41 1 d PD A -32 C53K C 0.3426(2) 1.2125(3) 0.12652(14) 0.0393(9) Uani 0.41 1 d PD A -32 C54K C 0.33876(19) 1.2580(4) 0.16660(14) 0.0597(14) Uani 0.41 1 d PD A -32 H54C H 0.3560 1.3165 0.1671 0.072 Uiso 0.41 1 calc PR A -32 H54D H 0.3662 1.2274 0.1921 0.072 Uiso 0.41 1 calc PR A -32 C55K C 0.2699(2) 1.2628(5) 0.16908(15) 0.076(2) Uani 0.41 1 d PD A -32 H55C H 0.2452 1.3049 0.1478 0.091 Uiso 0.41 1 calc PR A -32 H55D H 0.2489 1.2065 0.1613 0.091 Uiso 0.41 1 calc PR A -32 C56K C 0.2662(3) 1.2880(3) 0.21283(16) 0.085(2) Uani 0.41 1 d PD A -32 H56C H 0.2925 1.2474 0.2342 0.102 Uiso 0.41 1 calc PR A -32 H56D H 0.2209 1.2824 0.2128 0.102 Uiso 0.41 1 calc PR A -32 C57K C 0.2893(4) 1.3784(3) 0.22676(15) 0.0714(16) Uani 0.41 1 d PD A -32 H57C H 0.2602 1.4206 0.2079 0.086 Uiso 0.41 1 calc PR A -32 H57D H 0.3334 1.3870 0.2249 0.086 Uiso 0.41 1 calc PR A -32 C58K C 0.2891(4) 1.3901(3) 0.27329(15) 0.096(2) Uani 0.41 1 d PD A -32 H58C H 0.2468 1.3710 0.2754 0.115 Uiso 0.41 1 calc PR A -32 H58D H 0.3227 1.3528 0.2921 0.115 Uiso 0.41 1 calc PR A -32 C59K C 0.3009(4) 1.4803(4) 0.28949(15) 0.101(3) Uani 0.41 1 d PDU A -32 H59C H 0.2644 1.5167 0.2732 0.121 Uiso 0.41 1 calc PR A -32 H59D H 0.3406 1.5021 0.2844 0.121 Uiso 0.41 1 calc PR A -32 C60K C 0.3084(4) 1.4870(6) 0.33739(16) 0.0744(18) Uani 0.41 1 d PDU A -32 H60D H 0.2667 1.4757 0.3420 0.089 Uiso 0.41 1 calc PR A -32 H60E H 0.3230 1.5446 0.3476 0.089 Uiso 0.41 1 calc PR A -32 H60F H 0.3402 1.4451 0.3533 0.089 Uiso 0.41 1 calc PR A -32 O8L O 0.2944(5) 1.2365(9) 0.0959(2) 0.0597(8) Uani 0.14 1 d PD A -33 C53L C 0.3426(3) 1.2162(8) 0.12593(17) 0.0393(9) Uani 0.14 1 d PD A -33 C54L C 0.3376(4) 1.2234(4) 0.17135(17) 0.0597(14) Uani 0.14 1 d PD A -33 H54Q H 0.3011 1.1882 0.1738 0.072 Uiso 0.14 1 calc PR A -33 H54R H 0.3778 1.2016 0.1922 0.072 Uiso 0.14 1 calc PR A -33 C55L C 0.3273(5) 1.3158(4) 0.1814(2) 0.076(2) Uani 0.14 1 d PD A -33 H55Q H 0.2874 1.3377 0.1604 0.091 Uiso 0.14 1 calc PR A -33 H55R H 0.3640 1.3508 0.1792 0.091 Uiso 0.14 1 calc PR A -33 C56L C 0.3217(5) 1.3236(4) 0.2267(2) 0.085(2) Uani 0.14 1 d PD A -33 H56Q H 0.2872 1.2852 0.2298 0.102 Uiso 0.14 1 calc PR A -33 H56R H 0.3629 1.3065 0.2480 0.102 Uiso 0.14 1 calc PR A -33 C57L C 0.3058(5) 1.4160(4) 0.2346(2) 0.0714(16) Uani 0.14 1 d PD A -33 H57Q H 0.2646 1.4330 0.2132 0.086 Uiso 0.14 1 calc PR A -33 H57R H 0.3402 1.4543 0.2315 0.086 Uiso 0.14 1 calc PR A -33 C58L C 0.2999(7) 1.4250(4) 0.2798(2) 0.096(2) Uani 0.14 1 d PD A -33 H58Q H 0.2595 1.3979 0.2811 0.115 Uiso 0.14 1 calc PR A -33 H58R H 0.3367 1.3962 0.3008 0.115 Uiso 0.14 1 calc PR A -33 C59L C 0.2997(8) 1.5201(4) 0.2905(2) 0.101(3) Uani 0.14 1 d PDU A -33 H59Q H 0.3387 1.5476 0.2870 0.121 Uiso 0.14 1 calc PR A -33 H59R H 0.2614 1.5477 0.2705 0.121 Uiso 0.14 1 calc PR A -33 C60L C 0.2986(9) 1.5327(10) 0.3364(3) 0.0744(18) Uani 0.14 1 d PDU A -33 H60Q H 0.2583 1.5609 0.3361 0.089 Uiso 0.14 1 calc PR A -33 H60R H 0.3354 1.5681 0.3521 0.089 Uiso 0.14 1 calc PR A -33 H60W H 0.3015 1.4770 0.3505 0.089 Uiso 0.14 1 calc PR A -33 O8M O 0.2944(6) 1.1681(10) 0.0946(3) 0.0597(8) Uani 0.12 1 d PD A -34 C53M C 0.3418(3) 1.1867(11) 0.12576(17) 0.0393(9) Uani 0.12 1 d PD A -34 C54M C 0.3357(3) 1.1717(7) 0.17040(16) 0.0597(14) Uani 0.12 1 d PD A -34 H54X H 0.3290 1.1101 0.1744 0.072 Uiso 0.12 1 calc PR A -34 H54Y H 0.3760 1.1896 0.1924 0.072 Uiso 0.12 1 calc PR A -34 C55M C 0.2787(4) 1.2227(8) 0.17564(18) 0.076(2) Uani 0.12 1 d PD A -34 H55X H 0.2376 1.1946 0.1597 0.091 Uiso 0.12 1 calc PR A -34 H55Y H 0.2788 1.2810 0.1640 0.091 Uiso 0.12 1 calc PR A -34 C56M C 0.2845(7) 1.2274(4) 0.2232(2) 0.085(2) Uani 0.12 1 d PD A -34 H56X H 0.2457 1.2021 0.2282 0.102 Uiso 0.12 1 calc PR A -34 H56Y H 0.3228 1.1949 0.2402 0.102 Uiso 0.12 1 calc PR A -34 C57M C 0.2910(10) 1.3207(4) 0.23709(19) 0.0714(16) Uani 0.12 1 d PD A -34 H57X H 0.2523 1.3529 0.2203 0.086 Uiso 0.12 1 calc PR A -34 H57Y H 0.3293 1.3462 0.2317 0.086 Uiso 0.12 1 calc PR A -34 C58M C 0.2979(9) 1.3264(4) 0.2848(2) 0.096(2) Uani 0.12 1 d PD A -34 H58X H 0.2557 1.3153 0.2894 0.115 Uiso 0.12 1 calc PR A -34 H58Y H 0.3292 1.2832 0.3009 0.115 Uiso 0.12 1 calc PR A -34 C59M C 0.3216(7) 1.4160(5) 0.3002(2) 0.101(3) Uani 0.12 1 d PDU A -34 H59X H 0.3667 1.4233 0.3001 0.121 Uiso 0.12 1 calc PR A -34 H59Y H 0.2944 1.4591 0.2808 0.121 Uiso 0.12 1 calc PR A -34 C60M C 0.3177(8) 1.4285(11) 0.3455(3) 0.0744(18) Uani 0.12 1 d PDU A -34 H60X H 0.3334 1.3770 0.3625 0.089 Uiso 0.12 1 calc PR A -34 H60Y H 0.2728 1.4393 0.3442 0.089 Uiso 0.12 1 calc PR A -34 H60Z H 0.3445 1.4774 0.3589 0.089 Uiso 0.12 1 calc PR A -34 O1A O 0.56185(7) 0.96671(10) 0.07671(4) 0.0349(4) Uani 1 1 d . . . H1A H 0.5647 1.0202 0.0774 0.092(11) Uiso 1 1 calc R . . O2A O 0.63649(7) 0.88408(10) 0.14448(4) 0.0355(4) Uani 1 1 d . . . H2A H 0.6262 0.8787 0.1178 0.043 Uiso 1 1 calc R . . O3A O 0.64180(7) 1.04276(11) 0.17738(4) 0.0389(5) Uani 1 1 d . . . H3A H 0.6474 0.9909 0.1729 0.086(11) Uiso 1 1 calc R . . O4A O 0.58316(7) 1.12676(10) 0.10555(5) 0.0385(5) Uani 1 1 d . . . H4A H 0.6137 1.1362 0.1280 0.046 Uiso 1 1 calc R . . C1A C 0.49930(10) 0.94331(15) 0.05566(6) 0.0305(6) Uani 1 1 d . B . C2A C 0.45453(11) 1.00444(14) 0.03327(6) 0.0311(6) Uani 1 1 d . . . C3A C 0.39342(11) 0.97664(15) 0.01023(6) 0.0344(6) Uani 1 1 d . B . H3A1 H 0.3621 1.0171 -0.0048 0.041 Uiso 1 1 calc R . . C4A C 0.37673(11) 0.89009(15) 0.00860(6) 0.0336(6) Uani 1 1 d D . . C5A C 0.42189(11) 0.83164(15) 0.03224(6) 0.0334(6) Uani 1 1 d . B . H5A H 0.4103 0.7731 0.0317 0.040 Uiso 1 1 calc R . . C6A C 0.48338(10) 0.85658(14) 0.05655(6) 0.0298(6) Uani 1 1 d . . . C7A C 0.53112(11) 0.79321(14) 0.08352(6) 0.0340(6) Uani 1 1 d . B . H7A1 H 0.5734 0.8025 0.0788 0.041 Uiso 1 1 calc R . . H7A2 H 0.5165 0.7349 0.0734 0.041 Uiso 1 1 calc R . . C16A C 0.59248(10) 0.84183(14) 0.15944(6) 0.0306(6) Uani 1 1 d . A . C17A C 0.54062(10) 0.79772(14) 0.13163(6) 0.0297(6) Uani 1 1 d . . . C18A C 0.49777(11) 0.75717(14) 0.14902(6) 0.0307(6) Uani 1 1 d . A . H18A H 0.4616 0.7280 0.1305 0.037 Uiso 1 1 calc R . . C19A C 0.50637(11) 0.75799(14) 0.19319(7) 0.0328(6) Uani 1 1 d D . . C20A C 0.55940(11) 0.80227(14) 0.21980(6) 0.0328(6) Uani 1 1 d . A . H20A H 0.5661 0.8029 0.2498 0.039 Uiso 1 1 calc R . . C21A C 0.60195(10) 0.84473(14) 0.20385(6) 0.0308(6) Uani 1 1 d . . . C22A C 0.65606(11) 0.89690(15) 0.23377(7) 0.0351(6) Uani 1 1 d . A . H22A H 0.6739 0.8656 0.2610 0.042 Uiso 1 1 calc R . . H22B H 0.6911 0.9042 0.2207 0.042 Uiso 1 1 calc R . . C31A C 0.62342(10) 1.05079(15) 0.21413(6) 0.0319(6) Uani 1 1 d . A . C32A C 0.63301(10) 0.98373(15) 0.24289(7) 0.0325(6) Uani 1 1 d . . . C33A C 0.61727(11) 0.99708(16) 0.28046(7) 0.0364(7) Uani 1 1 d . A . H33A H 0.6233 0.9521 0.3007 0.044 Uiso 1 1 calc R . . C34A C 0.59293(11) 1.07503(16) 0.28895(7) 0.0375(7) Uani 1 1 d D . . C35A C 0.58183(11) 1.13953(16) 0.25867(7) 0.0375(7) Uani 1 1 d . A . H35A H 0.5632 1.1917 0.2638 0.045 Uiso 1 1 calc R . . C36A C 0.59747(11) 1.12924(15) 0.22081(6) 0.0344(6) Uani 1 1 d . . . C37A C 0.58539(11) 1.20009(15) 0.18771(7) 0.0362(6) Uani 1 1 d . A . H37A H 0.6228 1.2039 0.1767 0.043 Uiso 1 1 calc R . . H37B H 0.5820 1.2551 0.2017 0.043 Uiso 1 1 calc R . . C46A C 0.52581(11) 1.15117(14) 0.11147(6) 0.0328(6) Uani 1 1 d . A . C47A C 0.52407(11) 1.18661(14) 0.15006(6) 0.0336(6) Uani 1 1 d . . . C48A C 0.46516(11) 1.20914(15) 0.15407(7) 0.0383(7) Uani 1 1 d . A . H48A H 0.4633 1.2332 0.1802 0.046 Uiso 1 1 calc R . . C49A C 0.40791(12) 1.19744(16) 0.12062(7) 0.0420(7) Uani 1 1 d D . . C50A C 0.41069(11) 1.16290(15) 0.08232(7) 0.0378(7) Uani 1 1 d . A . H50A H 0.3719 1.1552 0.0594 0.045 Uiso 1 1 calc R . . C51A C 0.46903(11) 1.13940(14) 0.07686(6) 0.0339(6) Uani 1 1 d . . . C52A C 0.47096(11) 1.09856(14) 0.03542(6) 0.0336(6) Uani 1 1 d . A . H52A H 0.4400 1.1282 0.0110 0.040 Uiso 1 1 calc R . . H52B H 0.5147 1.1058 0.0326 0.040 Uiso 1 1 calc R . . O1 O 0.07306(7) 0.95330(11) 0.00480(4) 0.0377(5) Uani 1 1 d . . . H1 H 0.0665 1.0058 0.0068 0.045 Uiso 1 1 calc R . . O2 O 0.03713(7) 1.11511(10) -0.01922(4) 0.0361(4) Uani 1 1 d . . . H2 H 0.0085 1.0959 -0.0407 0.155(18) Uiso 1 1 calc R . . O3 O -0.02219(7) 1.02230(10) -0.08881(4) 0.0359(4) Uani 1 1 d . . . H3 H -0.0315 0.9710 -0.0861 0.043 Uiso 1 1 calc R . . O4 O -0.01041(7) 0.86185(10) -0.05963(4) 0.0366(4) Uani 1 1 d . . . H4 H 0.0012 0.8577 -0.0328 0.044 Uiso 1 1 calc R . . O5 O 0.34296(8) 0.78546(11) 0.09432(5) 0.0481(5) Uani 1 1 d . . . O7 O 0.00149(10) 1.16907(12) -0.26137(5) 0.0594(6) Uani 1 1 d . . . C1 C 0.13712(10) 0.93536(16) 0.02502(6) 0.0335(6) Uani 1 1 d . . . C2 C 0.15478(11) 0.84957(16) 0.02450(6) 0.0347(6) Uani 1 1 d . . . C3 C 0.21833(11) 0.82870(16) 0.04676(6) 0.0364(6) Uani 1 1 d . . . H3B H 0.2318 0.7709 0.0472 0.044 Uiso 1 1 calc R . . C4 C 0.26285(11) 0.88957(17) 0.06842(6) 0.0383(7) Uani 1 1 d . . . C5 C 0.24393(10) 0.97537(17) 0.06654(6) 0.0360(6) Uani 1 1 d . . . H5 H 0.2747 1.0175 0.0803 0.043 Uiso 1 1 calc R . . C6 C 0.18085(10) 1.00013(16) 0.04481(6) 0.0347(6) Uani 1 1 d . . . C7 C 0.16018(11) 1.09255(16) 0.04273(7) 0.0380(7) Uani 1 1 d . . . H7A H 0.1932 1.1255 0.0646 0.046 Uiso 1 1 calc R . . H7B H 0.1191 1.0965 0.0497 0.046 Uiso 1 1 calc R . . C8 C 0.32983(11) 0.86116(17) 0.09317(7) 0.0387(7) Uani 1 1 d . . . C9 C 0.37832(11) 0.92556(17) 0.11797(7) 0.0412(7) Uani 1 1 d . . . H9A H 0.3718 0.9803 0.1021 0.049 Uiso 1 1 calc R . . H9B H 0.4225 0.9050 0.1209 0.049 Uiso 1 1 calc R . . C10 C 0.37154(12) 0.94009(18) 0.16242(7) 0.0466(8) Uani 1 1 d . . . H10E H 0.3301 0.9694 0.1594 0.056 Uiso 1 1 calc R . . H10F H 0.3705 0.8841 0.1762 0.056 Uiso 1 1 calc R . . C11 C 0.42663(13) 0.99339(18) 0.19112(7) 0.0486(8) Uani 1 1 d . . . H11E H 0.4307 1.0466 0.1759 0.058 Uiso 1 1 calc R . . H11F H 0.4675 0.9612 0.1965 0.058 Uiso 1 1 calc R . . C12 C 0.41732(14) 1.0167(2) 0.23419(8) 0.0578(9) Uani 1 1 d . . . H12E H 0.4493 1.0610 0.2482 0.069 Uiso 1 1 calc R . . H12F H 0.3738 1.0416 0.2289 0.069 Uiso 1 1 calc R . . C13 C 0.42462(16) 0.9410(2) 0.26452(8) 0.0690(10) Uani 1 1 d . . . H13E H 0.4681 0.9157 0.2698 0.083 Uiso 1 1 calc R . . H13F H 0.3923 0.8969 0.2507 0.083 Uiso 1 1 calc R . . C14 C 0.41567(18) 0.9661(3) 0.30759(9) 0.0830(12) Uani 1 1 d . . . H14E H 0.4469 1.0116 0.3210 0.100 Uiso 1 1 calc R . . H14F H 0.3716 0.9894 0.3025 0.100 Uiso 1 1 calc R . . C15 C 0.4255(2) 0.8904(3) 0.33833(11) 0.1173(17) Uani 1 1 d . . . H15G H 0.3938 0.8458 0.3256 0.141 Uiso 1 1 calc R . . H15H H 0.4197 0.9093 0.3654 0.141 Uiso 1 1 calc R . . H15I H 0.4692 0.8676 0.3438 0.141 Uiso 1 1 calc R . . C16 C 0.08955(10) 1.14214(14) -0.03136(6) 0.0307(6) Uani 1 1 d . C . C17 C 0.15082(11) 1.13260(15) -0.00147(7) 0.0346(6) Uani 1 1 d . . . C18 C 0.20340(11) 1.15848(16) -0.01323(7) 0.0407(7) Uani 1 1 d . C . H18 H 0.2455 1.1517 0.0064 0.049 Uiso 1 1 calc R . . C19 C 0.19624(11) 1.19471(16) -0.05359(7) 0.0399(7) Uani 1 1 d D . . C20 C 0.13429(11) 1.20463(15) -0.08184(7) 0.0379(7) Uani 1 1 d . C . H20 H 0.1290 1.2304 -0.1089 0.045 Uiso 1 1 calc R . . C21 C 0.08021(11) 1.17809(14) -0.07170(6) 0.0318(6) Uani 1 1 d . . . C22 C 0.01320(11) 1.18739(15) -0.10433(6) 0.0335(6) Uani 1 1 d . C . H22C H -0.0197 1.1856 -0.0892 0.040 Uiso 1 1 calc R . . H22D H 0.0101 1.2437 -0.1185 0.040 Uiso 1 1 calc R . . C31 C -0.01528(10) 1.03454(14) -0.12894(6) 0.0292(6) Uani 1 1 d . C . C32 C -0.00135(10) 1.11824(15) -0.13798(6) 0.0307(6) Uani 1 1 d . . . C33 C 0.00090(11) 1.13537(15) -0.17883(6) 0.0339(6) Uani 1 1 d . C . H33 H 0.0090 1.1920 -0.1861 0.041 Uiso 1 1 calc R . . C34 C -0.00860(11) 1.07065(15) -0.20964(6) 0.0345(6) Uani 1 1 d . . . C35 C -0.01964(10) 0.98764(15) -0.19878(6) 0.0323(6) Uani 1 1 d . C . H35 H -0.0242 0.9434 -0.2193 0.039 Uiso 1 1 calc R . . C36 C -0.02418(10) 0.96776(14) -0.15820(6) 0.0304(6) Uani 1 1 d . . . C37 C -0.03676(11) 0.87633(15) -0.14794(6) 0.0329(6) Uani 1 1 d . C . H37C H -0.0540 0.8445 -0.1751 0.039 Uiso 1 1 calc R . . H37D H -0.0704 0.8762 -0.1334 0.039 Uiso 1 1 calc R . . C38 C -0.00548(12) 1.09412(16) -0.25299(7) 0.0395(7) Uani 1 1 d . C . C39 C -0.01208(13) 1.02610(16) -0.28648(7) 0.0432(7) Uani 1 1 d . . . H39E H -0.0575 1.0066 -0.2965 0.052 Uiso 1 1 calc R C . H39F H 0.0150 0.9766 -0.2732 0.052 Uiso 1 1 calc R . . C40 C 0.00748(13) 1.05527(18) -0.32531(7) 0.0490(8) Uani 1 1 d . C . H40E H -0.0085 1.1141 -0.3330 0.059 Uiso 1 1 calc R . . H40F H 0.0552 1.0567 -0.3173 0.059 Uiso 1 1 calc R . . C41 C -0.01843(13) 0.99827(18) -0.36411(7) 0.0502(8) Uani 1 1 d . . . H41E H -0.0112 0.9378 -0.3551 0.060 Uiso 1 1 calc R C . H41F H 0.0058 1.0096 -0.3846 0.060 Uiso 1 1 calc R . . C42 C -0.09021(15) 1.0123(2) -0.38648(8) 0.0632(10) Uani 1 1 d . C . H42E H -0.1138 1.0037 -0.3654 0.076 Uiso 1 1 calc R . . H42F H -0.0968 1.0723 -0.3963 0.076 Uiso 1 1 calc R . . C43 C -0.11937(16) 0.9542(2) -0.42461(9) 0.0680(10) Uani 1 1 d . . . H43E H -0.1103 0.8941 -0.4154 0.082 Uiso 1 1 calc R C . H43F H -0.0983 0.9659 -0.4468 0.082 Uiso 1 1 calc R . . C44 C -0.19290(19) 0.9661(3) -0.44427(11) 0.0974(14) Uani 1 1 d . C . H44E H -0.2142 0.9524 -0.4224 0.117 Uiso 1 1 calc R . . H44F H -0.2021 1.0267 -0.4525 0.117 Uiso 1 1 calc R . . C45 C -0.22082(19) 0.9113(3) -0.48259(12) 0.0994(15) Uani 1 1 d . . . H45G H -0.2044 0.9298 -0.5058 0.119 Uiso 1 1 calc R C . H45H H -0.2680 0.9162 -0.4919 0.119 Uiso 1 1 calc R . . H45I H -0.2085 0.8517 -0.4753 0.119 Uiso 1 1 calc R . . C46 C 0.03575(10) 0.82620(14) -0.07490(6) 0.0308(6) Uani 1 1 d . C . C47 C 0.02215(10) 0.82963(14) -0.11993(6) 0.0309(6) Uani 1 1 d . . . C48 C 0.06492(11) 0.78988(14) -0.13759(6) 0.0326(6) Uani 1 1 d . C . H48 H 0.0558 0.7898 -0.1678 0.039 Uiso 1 1 calc R . . C49 C 0.12075(11) 0.75010(14) -0.11228(7) 0.0340(6) Uani 1 1 d D . . C50 C 0.13385(11) 0.75076(14) -0.06774(6) 0.0324(6) Uani 1 1 d . C . H50 H 0.1727 0.7256 -0.0502 0.039 Uiso 1 1 calc R . . C51 C 0.09178(11) 0.78700(14) -0.04856(6) 0.0313(6) Uani 1 1 d . . . C52 C 0.10696(11) 0.78364(15) 0.00031(6) 0.0345(6) Uani 1 1 d . C . H52C H 0.0662 0.7912 0.0073 0.041 Uiso 1 1 calc R . . H52D H 0.1240 0.7263 0.0104 0.041 Uiso 1 1 calc R . . O8 O 0.14047(12) 0.68572(16) -0.17260(7) 0.0509(7) Uani 0.719(2) 1 d PD C -11 C53 C 0.16093(13) 0.70223(19) -0.13434(9) 0.0331(7) Uani 0.719(2) 1 d PD C -11 C54 C 0.23130(13) 0.6872(2) -0.11009(10) 0.0456(8) Uani 0.719(2) 1 d PD C -11 H54E H 0.2343 0.6464 -0.0865 0.055 Uiso 0.719(2) 1 calc PR C -11 H54F H 0.2509 0.7417 -0.0971 0.055 Uiso 0.719(2) 1 calc PR C -11 C55 C 0.26999(14) 0.6523(3) -0.13809(10) 0.0553(9) Uani 0.719(2) 1 d PD C -11 H55E H 0.2637 0.5897 -0.1412 0.066 Uiso 0.719(2) 1 calc PR C -11 H55F H 0.2540 0.6782 -0.1669 0.066 Uiso 0.719(2) 1 calc PR C -11 C56 C 0.34157(16) 0.6716(3) -0.11870(11) 0.0619(12) Uani 0.719(2) 1 d PD C -11 H56E H 0.3637 0.6537 -0.1395 0.074 Uiso 0.719(2) 1 calc PR C -11 H56F H 0.3466 0.7343 -0.1154 0.074 Uiso 0.719(2) 1 calc PR C -11 C57 C 0.37619(16) 0.6311(2) -0.07620(11) 0.0564(12) Uani 0.719(2) 1 d PD C -11 H57E H 0.3727 0.5682 -0.0791 0.068 Uiso 0.719(2) 1 calc PR C -11 H57F H 0.3549 0.6487 -0.0549 0.068 Uiso 0.719(2) 1 calc PR C -11 C58 C 0.44741(16) 0.6560(3) -0.06007(11) 0.0651(14) Uani 0.719(2) 1 d PD C -11 H58E H 0.4671 0.6438 -0.0829 0.078 Uiso 0.719(2) 1 calc PR C -11 H58F H 0.4504 0.7183 -0.0548 0.078 Uiso 0.719(2) 1 calc PR C -11 C59 C 0.48576(18) 0.6117(3) -0.02028(14) 0.0876(18) Uani 0.719(2) 1 d PD C -11 H59E H 0.4837 0.5493 -0.0251 0.105 Uiso 0.719(2) 1 calc PR C -11 H59F H 0.4672 0.6243 0.0031 0.105 Uiso 0.719(2) 1 calc PR C -11 C60 C 0.55676(18) 0.6414(3) -0.00707(15) 0.0771(14) Uani 0.719(2) 1 d PD C -11 H60G H 0.5742 0.6325 -0.0309 0.092 Uiso 0.719(2) 1 calc PR C -11 H60H H 0.5821 0.6085 0.0178 0.092 Uiso 0.719(2) 1 calc PR C -11 H60I H 0.5591 0.7022 0.0003 0.092 Uiso 0.719(2) 1 calc PR C -11 O8F O 0.1507(3) 0.7116(5) -0.17103(17) 0.0509(7) Uani 0.281(2) 1 d PD C -12 C53F C 0.1698(3) 0.7194(5) -0.13218(19) 0.0331(7) Uani 0.281(2) 1 d PD C -12 C54F C 0.2294(2) 0.6702(5) -0.10640(18) 0.0456(8) Uani 0.281(2) 1 d PD C -12 H54G H 0.2165 0.6123 -0.1000 0.055 Uiso 0.281(2) 1 calc PR C -12 H54H H 0.2495 0.6998 -0.0789 0.055 Uiso 0.281(2) 1 calc PR C -12 C55F C 0.2787(2) 0.6630(6) -0.1310(2) 0.0553(9) Uani 0.281(2) 1 d PD C -12 H55G H 0.2932 0.7209 -0.1357 0.066 Uiso 0.281(2) 1 calc PR C -12 H55H H 0.2574 0.6372 -0.1594 0.066 Uiso 0.281(2) 1 calc PR C -12 C56F C 0.3378(3) 0.6090(4) -0.1076(2) 0.0619(12) Uani 0.281(2) 1 d PD C -12 H56G H 0.3594 0.5882 -0.1282 0.074 Uiso 0.281(2) 1 calc PR C -12 H56H H 0.3242 0.5588 -0.0942 0.074 Uiso 0.281(2) 1 calc PR C -12 C57F C 0.3847(3) 0.6643(4) -0.0731(2) 0.0564(12) Uani 0.281(2) 1 d PD C -12 H57G H 0.3967 0.7157 -0.0866 0.068 Uiso 0.281(2) 1 calc PR C -12 H57H H 0.3634 0.6834 -0.0521 0.068 Uiso 0.281(2) 1 calc PR C -12 C58F C 0.4453(3) 0.6136(4) -0.0504(3) 0.0651(14) Uani 0.281(2) 1 d PD C -12 H58G H 0.4340 0.5669 -0.0336 0.078 Uiso 0.281(2) 1 calc PR C -12 H58H H 0.4630 0.5876 -0.0719 0.078 Uiso 0.281(2) 1 calc PR C -12 C59F C 0.4963(3) 0.6705(5) -0.0206(3) 0.0876(18) Uani 0.281(2) 1 d PD C -12 H59G H 0.4794 0.6942 0.0019 0.105 Uiso 0.281(2) 1 calc PR C -12 H59H H 0.5060 0.7189 -0.0370 0.105 Uiso 0.281(2) 1 calc PR C -12 C60F C 0.5584(3) 0.6205(7) 0.0006(4) 0.0771(14) Uani 0.281(2) 1 d PD C -12 H60J H 0.5584 0.6010 0.0289 0.092 Uiso 0.281(2) 1 calc PR C -12 H60K H 0.5958 0.6575 0.0035 0.092 Uiso 0.281(2) 1 calc PR C -12 H60L H 0.5606 0.5711 -0.0172 0.092 Uiso 0.281(2) 1 calc PR C -12 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 O6A 0.0592(10) 0.0626(12) 0.0286(8) 0.0121(8) 0.0046(8) -0.0106(9) C23A 0.0426(13) 0.0326(13) 0.0292(11) 0.0042(10) 0.0081(10) 0.0081(11) C24A 0.0385(13) 0.0521(15) 0.0361(11) 0.0132(11) 0.0067(10) 0.0018(12) C25A 0.0440(15) 0.115(3) 0.0470(14) 0.0229(17) 0.0094(13) -0.0031(17) C26A 0.0351(17) 0.137(4) 0.068(2) 0.036(2) 0.0118(16) 0.003(2) C27A 0.051(2) 0.094(3) 0.075(2) 0.006(2) 0.0045(18) 0.007(2) C28A 0.060(2) 0.099(3) 0.089(3) 0.008(3) 0.019(2) -0.004(2) C29A 0.076(2) 0.116(3) 0.080(2) -0.015(2) 0.032(2) -0.022(2) C30A 0.059(2) 0.093(3) 0.078(2) 0.002(2) 0.0167(19) -0.010(2) O6K 0.0592(10) 0.0626(12) 0.0286(8) 0.0121(8) 0.0046(8) -0.0106(9) C23K 0.0426(13) 0.0326(13) 0.0292(11) 0.0042(10) 0.0081(10) 0.0081(11) C24K 0.0385(13) 0.0521(15) 0.0361(11) 0.0132(11) 0.0067(10) 0.0018(12) C25K 0.0440(15) 0.115(3) 0.0470(14) 0.0229(17) 0.0094(13) -0.0031(17) C26K 0.0351(17) 0.137(4) 0.068(2) 0.036(2) 0.0118(16) 0.003(2) C27K 0.051(2) 0.094(3) 0.075(2) 0.006(2) 0.0045(18) 0.007(2) C28K 0.060(2) 0.099(3) 0.089(3) 0.008(3) 0.019(2) -0.004(2) C29K 0.076(2) 0.116(3) 0.080(2) -0.015(2) 0.032(2) -0.022(2) C30K 0.059(2) 0.093(3) 0.078(2) 0.002(2) 0.0167(19) -0.010(2) O5A 0.0458(10) 0.0465(10) 0.0343(8) -0.0017(8) -0.0056(8) -0.0022(9) C8A 0.0383(12) 0.0496(15) 0.0220(10) -0.0011(10) 0.0050(9) -0.0025(12) C9A 0.0371(13) 0.0483(16) 0.0278(11) -0.0088(11) 0.0045(10) -0.0041(12) C10A 0.0386(17) 0.0522(16) 0.0289(11) -0.0052(11) 0.0051(12) 0.0014(14) C11A 0.0342(17) 0.0596(18) 0.0336(14) -0.0069(14) 0.0006(13) 0.0033(15) C12A 0.0373(15) 0.064(2) 0.0364(14) 0.0070(14) 0.0036(13) 0.0073(15) C13A 0.0456(19) 0.087(2) 0.0465(18) 0.0068(18) 0.0029(15) 0.0101(19) C14A 0.0407(18) 0.086(3) 0.055(2) 0.0122(19) 0.0016(15) 0.0162(18) C15A 0.0660(19) 0.075(2) 0.076(2) 0.0227(18) 0.0176(17) 0.0203(18) O5K 0.0458(10) 0.0465(10) 0.0343(8) -0.0017(8) -0.0056(8) -0.0022(9) C8K 0.0383(12) 0.0496(15) 0.0220(10) -0.0011(10) 0.0050(9) -0.0025(12) C9K 0.0371(13) 0.0483(16) 0.0278(11) -0.0088(11) 0.0045(10) -0.0041(12) C10K 0.0386(17) 0.0522(16) 0.0289(11) -0.0052(11) 0.0051(12) 0.0014(14) C11K 0.0342(17) 0.0596(18) 0.0336(14) -0.0069(14) 0.0006(13) 0.0033(15) C12K 0.0373(15) 0.064(2) 0.0364(14) 0.0070(14) 0.0036(13) 0.0073(15) C13K 0.0456(19) 0.087(2) 0.0465(18) 0.0068(18) 0.0029(15) 0.0101(19) C14K 0.0407(18) 0.086(3) 0.055(2) 0.0122(19) 0.0016(15) 0.0162(18) C15K 0.0660(19) 0.075(2) 0.076(2) 0.0227(18) 0.0176(17) 0.0203(18) O6 0.0435(10) 0.0767(15) 0.0625(13) 0.0146(12) 0.0192(10) -0.0007(10) C23 0.0443(15) 0.0570(17) 0.0440(14) -0.0123(13) 0.0086(12) -0.0069(13) C24 0.0515(17) 0.045(2) 0.075(2) 0.0003(17) 0.0303(15) -0.0053(16) C25 0.0434(17) 0.0515(19) 0.075(2) 0.0014(17) 0.0249(15) 0.0001(15) C26 0.062(2) 0.058(2) 0.136(3) 0.019(2) 0.061(2) 0.0046(19) C27 0.097(3) 0.057(2) 0.122(3) -0.005(2) 0.064(2) -0.004(2) C28 0.063(2) 0.056(2) 0.118(3) 0.011(2) 0.037(2) 0.0108(18) C29 0.077(3) 0.066(3) 0.149(4) 0.016(3) 0.027(3) 0.006(2) C30 0.104(3) 0.078(3) 0.091(3) 0.035(2) -0.021(3) 0.026(2) O6F 0.0435(10) 0.0767(15) 0.0625(13) 0.0146(12) 0.0192(10) -0.0007(10) C23F 0.0443(15) 0.0570(17) 0.0440(14) -0.0123(13) 0.0086(12) -0.0069(13) C24F 0.0515(17) 0.045(2) 0.075(2) 0.0003(17) 0.0303(15) -0.0053(16) C25F 0.0434(17) 0.0515(19) 0.075(2) 0.0014(17) 0.0249(15) 0.0001(15) C26F 0.062(2) 0.058(2) 0.136(3) 0.019(2) 0.061(2) 0.0046(19) C27F 0.097(3) 0.057(2) 0.122(3) -0.005(2) 0.064(2) -0.004(2) C28F 0.063(2) 0.056(2) 0.118(3) 0.011(2) 0.037(2) 0.0108(18) C29F 0.077(3) 0.066(3) 0.149(4) 0.016(3) 0.027(3) 0.006(2) C30F 0.104(3) 0.078(3) 0.091(3) 0.035(2) -0.021(3) 0.026(2) O7A 0.0969(13) 0.0613(12) 0.0315(8) -0.0009(8) 0.0183(9) 0.0317(11) C38A 0.0516(15) 0.0491(16) 0.0258(11) -0.0047(11) 0.0052(11) 0.0089(13) C39A 0.0536(17) 0.0443(17) 0.0257(11) -0.0022(12) 0.0097(12) 0.0045(14) C40A 0.0540(18) 0.0485(18) 0.0284(13) -0.0013(13) 0.0096(13) 0.0023(14) C41A 0.092(2) 0.0514(19) 0.0352(13) 0.0099(14) 0.0276(14) 0.0199(18) C42A 0.095(2) 0.063(2) 0.0402(15) 0.0116(15) 0.0290(15) 0.0260(19) C43A 0.109(3) 0.077(2) 0.0365(16) 0.0016(17) 0.007(2) 0.016(2) C44A 0.143(4) 0.108(3) 0.0385(18) 0.001(2) 0.009(3) 0.033(3) C45A 0.175(4) 0.085(3) 0.068(2) 0.014(2) 0.054(2) 0.046(3) O7K 0.0969(13) 0.0613(12) 0.0315(8) -0.0009(8) 0.0183(9) 0.0317(11) C38K 0.0516(15) 0.0491(16) 0.0258(11) -0.0047(11) 0.0052(11) 0.0089(13) C39K 0.0536(17) 0.0443(17) 0.0257(11) -0.0022(12) 0.0097(12) 0.0045(14) C40K 0.0540(18) 0.0485(18) 0.0284(13) -0.0013(13) 0.0096(13) 0.0023(14) C41K 0.092(2) 0.0514(19) 0.0352(13) 0.0099(14) 0.0276(14) 0.0199(18) C42K 0.095(2) 0.063(2) 0.0402(15) 0.0116(15) 0.0290(15) 0.0260(19) C43K 0.109(3) 0.077(2) 0.0365(16) 0.0016(17) 0.007(2) 0.016(2) C44K 0.143(4) 0.108(3) 0.0385(18) 0.001(2) 0.009(3) 0.033(3) C45K 0.175(4) 0.085(3) 0.068(2) 0.014(2) 0.054(2) 0.046(3) O8A 0.0426(11) 0.0649(18) 0.0656(12) -0.0507(12) 0.0078(9) -0.0054(12) C53A 0.0496(16) 0.0256(19) 0.0362(13) -0.0103(13) 0.0037(12) 0.0023(15) C54A 0.0435(18) 0.075(4) 0.059(2) -0.026(2) 0.0133(16) 0.011(2) C55A 0.065(3) 0.086(5) 0.077(3) -0.043(3) 0.022(2) 0.006(4) C56A 0.066(3) 0.101(5) 0.100(4) -0.039(3) 0.043(3) 0.006(3) C57A 0.073(2) 0.076(4) 0.068(2) -0.017(3) 0.0256(19) -0.001(3) C58A 0.170(4) 0.072(5) 0.074(3) -0.031(3) 0.077(3) -0.018(5) C59A 0.075(3) 0.165(8) 0.060(3) 0.006(4) 0.017(3) -0.007(5) C60A 0.064(2) 0.098(4) 0.065(3) -0.012(3) 0.026(2) -0.008(3) O8K 0.0426(11) 0.0649(18) 0.0656(12) -0.0507(12) 0.0078(9) -0.0054(12) C53K 0.0496(16) 0.0256(19) 0.0362(13) -0.0103(13) 0.0037(12) 0.0023(15) C54K 0.0435(18) 0.075(4) 0.059(2) -0.026(2) 0.0133(16) 0.011(2) C55K 0.065(3) 0.086(5) 0.077(3) -0.043(3) 0.022(2) 0.006(4) C56K 0.066(3) 0.101(5) 0.100(4) -0.039(3) 0.043(3) 0.006(3) C57K 0.073(2) 0.076(4) 0.068(2) -0.017(3) 0.0256(19) -0.001(3) C58K 0.170(4) 0.072(5) 0.074(3) -0.031(3) 0.077(3) -0.018(5) C59K 0.075(3) 0.165(8) 0.060(3) 0.006(4) 0.017(3) -0.007(5) C60K 0.064(2) 0.098(4) 0.065(3) -0.012(3) 0.026(2) -0.008(3) O8L 0.0426(11) 0.0649(18) 0.0656(12) -0.0507(12) 0.0078(9) -0.0054(12) C53L 0.0496(16) 0.0256(19) 0.0362(13) -0.0103(13) 0.0037(12) 0.0023(15) C54L 0.0435(18) 0.075(4) 0.059(2) -0.026(2) 0.0133(16) 0.011(2) C55L 0.065(3) 0.086(5) 0.077(3) -0.043(3) 0.022(2) 0.006(4) C56L 0.066(3) 0.101(5) 0.100(4) -0.039(3) 0.043(3) 0.006(3) C57L 0.073(2) 0.076(4) 0.068(2) -0.017(3) 0.0256(19) -0.001(3) C58L 0.170(4) 0.072(5) 0.074(3) -0.031(3) 0.077(3) -0.018(5) C59L 0.075(3) 0.165(8) 0.060(3) 0.006(4) 0.017(3) -0.007(5) C60L 0.064(2) 0.098(4) 0.065(3) -0.012(3) 0.026(2) -0.008(3) O8M 0.0426(11) 0.0649(18) 0.0656(12) -0.0507(12) 0.0078(9) -0.0054(12) C53M 0.0496(16) 0.0256(19) 0.0362(13) -0.0103(13) 0.0037(12) 0.0023(15) C54M 0.0435(18) 0.075(4) 0.059(2) -0.026(2) 0.0133(16) 0.011(2) C55M 0.065(3) 0.086(5) 0.077(3) -0.043(3) 0.022(2) 0.006(4) C56M 0.066(3) 0.101(5) 0.100(4) -0.039(3) 0.043(3) 0.006(3) C57M 0.073(2) 0.076(4) 0.068(2) -0.017(3) 0.0256(19) -0.001(3) C58M 0.170(4) 0.072(5) 0.074(3) -0.031(3) 0.077(3) -0.018(5) C59M 0.075(3) 0.165(8) 0.060(3) 0.006(4) 0.017(3) -0.007(5) C60M 0.064(2) 0.098(4) 0.065(3) -0.012(3) 0.026(2) -0.008(3) O1A 0.0362(8) 0.0410(9) 0.0240(7) -0.0019(6) 0.0042(6) -0.0032(7) O2A 0.0367(8) 0.0447(9) 0.0244(7) -0.0027(7) 0.0085(6) 0.0000(7) O3A 0.0404(8) 0.0487(10) 0.0274(7) -0.0060(7) 0.0103(6) 0.0008(8) O4A 0.0383(8) 0.0455(9) 0.0290(7) -0.0024(7) 0.0066(6) -0.0026(7) C1A 0.0338(11) 0.0424(13) 0.0155(8) -0.0011(9) 0.0076(8) -0.0002(10) C2A 0.0408(12) 0.0385(12) 0.0141(8) -0.0010(8) 0.0084(8) 0.0011(10) C3A 0.0375(12) 0.0448(13) 0.0189(9) -0.0019(9) 0.0055(9) 0.0054(11) C4A 0.0391(12) 0.0426(13) 0.0191(9) -0.0024(9) 0.0091(9) 0.0000(11) C5A 0.0415(12) 0.0362(12) 0.0212(9) -0.0025(9) 0.0077(9) -0.0025(10) C6A 0.0360(11) 0.0361(12) 0.0158(8) -0.0036(8) 0.0059(8) -0.0006(10) C7A 0.0403(12) 0.0330(12) 0.0245(10) -0.0033(9) 0.0039(9) 0.0004(10) C16A 0.0272(10) 0.0364(12) 0.0262(10) 0.0001(9) 0.0052(9) 0.0073(10) C17A 0.0316(11) 0.0326(11) 0.0220(9) -0.0005(9) 0.0042(8) 0.0062(10) C18A 0.0332(11) 0.0284(11) 0.0237(10) 0.0016(9) -0.0012(9) 0.0046(10) C19A 0.0362(12) 0.0329(12) 0.0256(10) 0.0038(9) 0.0042(9) 0.0036(10) C20A 0.0373(12) 0.0379(12) 0.0196(9) 0.0029(9) 0.0034(9) 0.0081(10) C21A 0.0297(11) 0.0356(12) 0.0230(9) 0.0004(9) 0.0018(9) 0.0071(10) C22A 0.0329(11) 0.0433(13) 0.0243(10) 0.0023(10) 0.0018(9) 0.0018(10) C31A 0.0312(11) 0.0403(12) 0.0210(9) -0.0082(9) 0.0031(9) -0.0036(10) C32A 0.0266(11) 0.0418(13) 0.0254(10) -0.0049(9) 0.0024(9) 0.0012(10) C33A 0.0339(12) 0.0482(14) 0.0199(9) 0.0014(10) -0.0022(9) 0.0038(11) C34A 0.0385(12) 0.0473(14) 0.0212(9) -0.0064(10) 0.0011(9) 0.0049(11) C35A 0.0376(12) 0.0420(13) 0.0260(10) -0.0105(10) -0.0006(10) 0.0006(11) C36A 0.0325(11) 0.0417(13) 0.0228(10) -0.0068(9) -0.0005(9) -0.0053(10) C37A 0.0399(12) 0.0401(13) 0.0258(10) -0.0092(9) 0.0059(9) -0.0039(11) C46A 0.0367(12) 0.0352(12) 0.0254(10) -0.0008(9) 0.0080(9) -0.0017(10) C47A 0.0420(12) 0.0320(12) 0.0224(9) -0.0046(9) 0.0032(9) 0.0005(10) C48A 0.0451(13) 0.0433(13) 0.0226(10) -0.0062(10) 0.0048(10) 0.0012(11) C49A 0.0427(13) 0.0472(14) 0.0319(11) -0.0105(10) 0.0053(10) 0.0025(12) C50A 0.0391(13) 0.0394(13) 0.0259(10) -0.0047(10) -0.0031(10) -0.0016(11) C51A 0.0430(12) 0.0345(12) 0.0203(9) 0.0000(9) 0.0040(9) -0.0016(11) C52A 0.0436(12) 0.0366(12) 0.0181(9) 0.0013(9) 0.0057(9) 0.0005(10) O1 0.0308(8) 0.0512(10) 0.0262(7) -0.0025(7) 0.0014(6) -0.0001(7) O2 0.0320(8) 0.0519(9) 0.0231(7) -0.0030(7) 0.0065(6) -0.0021(7) O3 0.0426(8) 0.0415(9) 0.0222(7) -0.0018(6) 0.0079(6) -0.0028(7) O4 0.0373(8) 0.0538(10) 0.0176(6) 0.0021(7) 0.0068(6) 0.0022(8) O5 0.0459(9) 0.0573(11) 0.0330(8) 0.0076(8) 0.0002(7) 0.0065(9) O7 0.1010(14) 0.0475(10) 0.0267(8) 0.0016(8) 0.0151(9) -0.0100(10) C1 0.0307(11) 0.0515(14) 0.0161(9) 0.0019(9) 0.0038(8) -0.0007(11) C2 0.0368(12) 0.0517(14) 0.0145(9) 0.0017(9) 0.0066(8) 0.0003(11) C3 0.0386(12) 0.0505(14) 0.0178(9) 0.0064(10) 0.0050(9) 0.0039(11) C4 0.0367(12) 0.0568(15) 0.0193(9) 0.0047(10) 0.0054(9) 0.0055(11) C5 0.0302(11) 0.0590(15) 0.0183(9) -0.0007(10) 0.0069(8) -0.0060(11) C6 0.0322(11) 0.0536(14) 0.0178(9) -0.0006(10) 0.0071(8) -0.0008(11) C7 0.0289(11) 0.0576(15) 0.0228(10) -0.0028(10) 0.0012(9) -0.0026(11) C8 0.0349(12) 0.0564(15) 0.0224(10) 0.0042(10) 0.0052(9) 0.0014(12) C9 0.0321(12) 0.0613(16) 0.0274(10) 0.0075(11) 0.0053(9) 0.0052(12) C10 0.0459(14) 0.0625(17) 0.0277(11) -0.0013(11) 0.0056(10) 0.0007(13) C11 0.0450(14) 0.0611(16) 0.0327(12) 0.0035(12) 0.0017(11) -0.0043(13) C12 0.0520(16) 0.0745(19) 0.0369(13) -0.0045(14) -0.0011(12) 0.0012(15) C13 0.0689(19) 0.094(2) 0.0366(14) 0.0016(15) 0.0047(14) 0.0100(18) C14 0.088(2) 0.117(3) 0.0456(15) 0.0028(18) 0.0214(15) 0.015(2) C15 0.161(4) 0.138(4) 0.0549(18) 0.031(2) 0.037(2) 0.012(3) C16 0.0324(11) 0.0384(12) 0.0207(9) -0.0069(9) 0.0074(8) -0.0026(10) C17 0.0347(12) 0.0399(13) 0.0270(10) -0.0047(10) 0.0061(9) 0.0003(10) C18 0.0335(12) 0.0478(14) 0.0374(11) -0.0043(11) 0.0062(10) -0.0017(11) C19 0.0405(12) 0.0416(14) 0.0386(11) -0.0042(10) 0.0136(10) -0.0055(11) C20 0.0466(13) 0.0389(13) 0.0295(10) -0.0041(10) 0.0136(10) -0.0006(11) C21 0.0353(11) 0.0336(12) 0.0242(9) -0.0052(9) 0.0056(9) -0.0013(10) C22 0.0380(12) 0.0388(12) 0.0226(9) -0.0029(9) 0.0076(9) 0.0034(10) C31 0.0257(10) 0.0411(12) 0.0170(9) 0.0041(9) 0.0008(8) 0.0035(10) C32 0.0282(11) 0.0392(12) 0.0222(9) -0.0013(9) 0.0041(8) 0.0032(10) C33 0.0369(12) 0.0378(12) 0.0249(10) 0.0033(9) 0.0062(9) 0.0000(10) C34 0.0393(12) 0.0405(13) 0.0205(9) 0.0021(9) 0.0044(9) 0.0009(11) C35 0.0344(11) 0.0375(12) 0.0208(9) -0.0037(9) 0.0023(9) 0.0003(10) C36 0.0287(11) 0.0367(12) 0.0214(9) 0.0024(9) 0.0014(8) 0.0036(10) C37 0.0356(11) 0.0427(13) 0.0170(9) -0.0033(9) 0.0031(9) -0.0037(10) C38 0.0474(13) 0.0411(13) 0.0249(10) 0.0021(10) 0.0039(10) -0.0035(11) C39 0.0603(14) 0.0432(14) 0.0264(10) -0.0007(10) 0.0137(10) -0.0091(12) C40 0.0648(16) 0.0519(15) 0.0317(11) -0.0015(11) 0.0170(11) -0.0057(13) C41 0.0680(16) 0.0548(16) 0.0299(11) -0.0033(11) 0.0180(11) -0.0037(14) C42 0.0761(19) 0.075(2) 0.0343(13) 0.0028(14) 0.0109(13) 0.0068(17) C43 0.085(2) 0.070(2) 0.0396(14) -0.0016(14) 0.0046(15) 0.0087(17) C44 0.087(2) 0.119(3) 0.062(2) -0.019(2) -0.0131(19) 0.027(2) C45 0.089(3) 0.118(3) 0.075(2) -0.020(2) 0.001(2) 0.006(2) C46 0.0354(11) 0.0376(12) 0.0196(9) 0.0006(9) 0.0086(8) -0.0059(10) C47 0.0353(11) 0.0358(12) 0.0194(9) 0.0007(9) 0.0051(9) -0.0048(10) C48 0.0419(12) 0.0329(12) 0.0214(9) -0.0021(9) 0.0074(9) -0.0043(10) C49 0.0409(12) 0.0334(12) 0.0244(10) -0.0022(9) 0.0053(9) -0.0019(10) C50 0.0389(12) 0.0304(12) 0.0241(10) 0.0002(9) 0.0041(9) 0.0023(10) C51 0.0369(12) 0.0330(12) 0.0204(9) 0.0019(9) 0.0034(9) -0.0039(10) C52 0.0363(12) 0.0434(13) 0.0219(9) 0.0062(9) 0.0063(9) 0.0010(11) O8 0.0635(12) 0.0525(14) 0.0291(8) -0.0187(9) 0.0030(8) 0.0111(11) C53 0.0427(14) 0.0220(13) 0.0299(11) -0.0035(10) 0.0044(10) -0.0120(12) C54 0.0455(14) 0.0535(18) 0.0373(12) -0.0078(13) 0.0120(11) -0.0025(14) C55 0.0481(16) 0.076(2) 0.0380(14) -0.0180(15) 0.0068(13) 0.0067(15) C56 0.061(2) 0.067(3) 0.059(2) -0.012(2) 0.0192(17) -0.009(2) C57 0.0631(19) 0.047(3) 0.0528(17) -0.0062(18) 0.0089(15) 0.0054(19) C58 0.075(2) 0.077(3) 0.0421(19) 0.007(2) 0.0150(17) -0.022(2) C59 0.078(3) 0.081(4) 0.082(3) 0.002(3) -0.007(2) 0.017(3) C60 0.086(2) 0.061(2) 0.066(2) -0.003(2) -0.005(2) 0.000(2) O8F 0.0635(12) 0.0525(14) 0.0291(8) -0.0187(9) 0.0030(8) 0.0111(11) C53F 0.0427(14) 0.0220(13) 0.0299(11) -0.0035(10) 0.0044(10) -0.0120(12) C54F 0.0455(14) 0.0535(18) 0.0373(12) -0.0078(13) 0.0120(11) -0.0025(14) C55F 0.0481(16) 0.076(2) 0.0380(14) -0.0180(15) 0.0068(13) 0.0067(15) C56F 0.061(2) 0.067(3) 0.059(2) -0.012(2) 0.0192(17) -0.009(2) C57F 0.0631(19) 0.047(3) 0.0528(17) -0.0062(18) 0.0089(15) 0.0054(19) C58F 0.075(2) 0.077(3) 0.0421(19) 0.007(2) 0.0150(17) -0.022(2) C59F 0.078(3) 0.081(4) 0.082(3) 0.002(3) -0.007(2) 0.017(3) C60F 0.086(2) 0.061(2) 0.066(2) -0.003(2) -0.005(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O6A C23A 1.222(3) . ? C23A C19A 1.485(4) . ? C23A C24A 1.510(3) . ? C24A C25A 1.522(4) . ? C25A C26A 1.521(4) . ? C26A C27A 1.508(5) . ? C27A C28A 1.523(4) . ? C28A C29A 1.481(5) . ? C29A C30A 1.509(4) . ? O6K C23K 1.228(9) . ? C23K C19A 1.491(9) . ? C23K C24K 1.527(6) . ? C24K C25K 1.528(8) . ? C25K C26K 1.529(8) . ? C26K C27K 1.525(8) . ? C27K C28K 1.516(7) . ? C28K C29K 1.510(8) . ? C29K C30K 1.522(8) . ? O5A C8A 1.223(3) . ? C8A C4A 1.501(3) . ? C8A C9A 1.512(3) . ? C9A C10A 1.530(4) . ? C10A C11A 1.534(3) . ? C11A C12A 1.523(4) . ? C12A C13A 1.525(4) . ? C13A C14A 1.526(4) . ? C14A C15A 1.521(4) . ? O5K C8K 1.220(9) . ? C8K C4A 1.498(7) . ? C8K C9K 1.526(7) . ? C9K C10K 1.530(7) . ? C10K C11K 1.529(7) . ? C11K C12K 1.533(7) . ? C12K C13K 1.528(8) . ? C13K C14K 1.528(7) . ? C14K C15K 1.525(8) . ? O6 C23 1.216(4) . ? C23 C19 1.490(4) . ? C23 C24 1.510(4) . ? C24 C25 1.520(4) . ? C25 C26 1.527(4) . ? C26 C27 1.514(5) . ? C27 C28 1.513(5) . ? C28 C29 1.499(4) . ? C29 C30 1.535(5) . ? O6F C23F 1.227(10) . ? C23F C19 1.494(8) . ? C23F C24F 1.531(7) . ? C24F C25F 1.524(7) . ? C25F C26F 1.527(7) . ? C26F C27F 1.523(8) . ? C27F C28F 1.532(8) . ? C28F C29F 1.534(8) . ? C29F C30F 1.532(8) . ? O7A C38A 1.205(4) . ? C38A C34A 1.491(4) . ? C38A C39A 1.511(4) . ? C39A C40A 1.510(4) . ? C40A C41A 1.519(4) . ? C41A C42A 1.536(4) . ? C42A C43A 1.519(4) . ? C43A C44A 1.527(5) . ? C44A C45A 1.504(5) . ? O7K C38K 1.207(10) . ? C38K C39K 1.518(7) . ? C38K C34A 1.528(8) . ? C39K C40K 1.532(7) . ? C40K C41K 1.524(7) . ? C41K C42K 1.532(8) . ? C42K C43K 1.525(7) . ? C43K C44K 1.526(8) . ? C44K C45K 1.528(9) . ? O8A C53A 1.233(6) . ? C53A C49A 1.510(6) . ? C53A C54A 1.524(6) . ? C54A C55A 1.526(6) . ? C55A C56A 1.514(7) . ? C56A C57A 1.522(6) . ? C57A C58A 1.536(7) . ? C58A C59A 1.519(6) . ? C59A C60A 1.559(7) . ? O8K C53K 1.231(6) . ? C53K C49A 1.510(6) . ? C53K C54K 1.521(6) . ? C54K C55K 1.528(6) . ? C55K C56K 1.515(6) . ? C56K C57K 1.525(6) . ? C57K C58K 1.540(6) . ? C58K C59K 1.503(6) . ? C59K C60K 1.534(6) . ? O8L C53L 1.241(10) . ? C53L C49A 1.512(8) . ? C53L C54L 1.532(7) . ? C54L C55L 1.517(7) . ? C55L C56L 1.532(8) . ? C56L C57L 1.530(7) . ? C57L C58L 1.535(8) . ? C58L C59L 1.532(7) . ? C59L C60L 1.526(8) . ? O8M C53M 1.243(10) . ? C53M C49A 1.510(7) . ? C53M C54M 1.530(7) . ? C54M C55M 1.529(8) . ? C55M C56M 1.530(7) . ? C56M C57M 1.524(7) . ? C57M C58M 1.529(8) . ? C58M C59M 1.527(8) . ? C59M C60M 1.527(9) . ? O1A C1A 1.373(2) . ? O2A C16A 1.373(3) . ? O3A C31A 1.389(3) . ? O4A C46A 1.375(3) . ? C1A C2A 1.402(3) . ? C1A C6A 1.405(3) . ? C2A C3A 1.383(3) . ? C2A C52A 1.514(3) . ? C3A C4A 1.400(3) . ? C4A C5A 1.392(3) . ? C5A C6A 1.387(3) . ? C6A C7A 1.511(3) . ? C7A C17A 1.530(3) . ? C16A C17A 1.397(3) . ? C16A C21A 1.409(3) . ? C17A C18A 1.388(3) . ? C18A C19A 1.404(3) . ? C19A C20A 1.399(3) . ? C20A C21A 1.368(3) . ? C21A C22A 1.519(3) . ? C22A C32A 1.511(3) . ? C31A C32A 1.385(3) . ? C31A C36A 1.398(3) . ? C32A C33A 1.394(3) . ? C33A C34A 1.393(3) . ? C34A C35A 1.386(3) . ? C35A C36A 1.395(3) . ? C36A C37A 1.519(3) . ? C37A C47A 1.529(3) . ? C46A C47A 1.394(3) . ? C46A C51A 1.410(3) . ? C47A C48A 1.375(3) . ? C48A C49A 1.397(3) . ? C49A C50A 1.387(3) . ? C50A C51A 1.385(4) . ? C51A C52A 1.516(3) . ? O1 C1 1.376(3) . ? O2 C16 1.385(3) . ? O3 C31 1.385(3) . ? O4 C46 1.372(3) . ? O5 C8 1.218(3) . ? O7 C38 1.226(3) . ? C1 C2 1.399(3) . ? C1 C6 1.406(3) . ? C2 C3 1.390(3) . ? C2 C52 1.507(3) . ? C3 C4 1.389(3) . ? C4 C5 1.401(4) . ? C4 C8 1.502(3) . ? C5 C6 1.393(3) . ? C6 C7 1.511(4) . ? C7 C17 1.536(3) . ? C8 C9 1.505(3) . ? C9 C10 1.528(3) . ? C10 C11 1.526(3) . ? C11 C12 1.533(4) . ? C12 C13 1.525(4) . ? C13 C14 1.537(4) . ? C14 C15 1.529(5) . ? C16 C21 1.395(3) . ? C16 C17 1.399(3) . ? C17 C18 1.376(4) . ? C18 C19 1.406(3) . ? C19 C20 1.390(3) . ? C20 C21 1.382(3) . ? C21 C22 1.528(3) . ? C22 C32 1.510(3) . ? C31 C36 1.393(3) . ? C31 C32 1.398(3) . ? C32 C33 1.383(3) . ? C33 C34 1.402(3) . ? C34 C35 1.389(3) . ? C34 C38 1.491(3) . ? C35 C36 1.401(3) . ? C36 C37 1.515(3) . ? C37 C47 1.516(3) . ? C38 C39 1.506(3) . ? C39 C40 1.533(4) . ? C40 C41 1.515(3) . ? C41 C42 1.524(4) . ? C42 C43 1.519(4) . ? C43 C44 1.542(5) . ? C44 C45 1.490(5) . ? C46 C51 1.401(3) . ? C46 C47 1.417(3) . ? C47 C48 1.387(3) . ? C48 C49 1.391(3) . ? C49 C50 1.401(3) . ? C49 C53F 1.492(7) . ? C49 C53 1.497(4) . ? C50 C51 1.383(3) . ? C51 C52 1.536(3) . ? O8 C53 1.224(3) . ? C53 C54 1.512(4) . ? C54 C55 1.526(4) . ? C55 C56 1.521(4) . ? C56 C57 1.507(4) . ? C57 C58 1.527(4) . ? C58 C59 1.488(5) . ? C59 C60 1.543(5) . ? O8F C53F 1.220(8) . ? C53F C54F 1.522(6) . ? C54F C55F 1.531(7) . ? C55F C56F 1.534(7) . ? C56F C57F 1.538(7) . ? C57F C58F 1.524(7) . ? C58F C59F 1.522(7) . ? C59F C60F 1.531(8) . ? 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 O6A C23A C19A 120.1(2) . . ? O6A C23A C24A 120.1(3) . . ? C19A C23A C24A 119.7(2) . . ? C23A C24A C25A 113.6(2) . . ? C26A C25A C24A 114.3(3) . . ? C27A C26A C25A 115.6(3) . . ? C26A C27A C28A 116.0(3) . . ? C29A C28A C27A 116.5(3) . . ? C28A C29A C30A 114.2(3) . . ? O6K C23K C19A 118.9(7) . . ? O6K C23K C24K 118.1(7) . . ? C19A C23K C24K 118.5(6) . . ? C23K C24K C25K 110.4(5) . . ? C24K C25K C26K 111.0(7) . . ? C27K C26K C25K 110.5(6) . . ? C28K C27K C26K 111.4(7) . . ? C29K C28K C27K 114.5(7) . . ? C28K C29K C30K 114.4(7) . . ? O5A C8A C4A 119.3(2) . . ? O5A C8A C9A 120.4(2) . . ? C4A C8A C9A 120.4(2) . . ? C8A C9A C10A 112.2(2) . . ? C9A C10A C11A 111.8(2) . . ? C12A C11A C10A 112.0(2) . . ? C11A C12A C13A 112.5(2) . . ? C12A C13A C14A 113.5(3) . . ? C15A C14A C13A 114.3(3) . . ? O5K C8K C4A 119.7(6) . . ? O5K C8K C9K 119.8(7) . . ? C4A C8K C9K 120.1(5) . . ? C8K C9K C10K 109.6(7) . . ? C11K C10K C9K 110.2(5) . . ? C10K C11K C12K 108.8(6) . . ? C13K C12K C11K 110.1(6) . . ? C12K C13K C14K 109.3(5) . . ? C15K C14K C13K 111.0(7) . . ? O6 C23 C19 121.2(3) . . ? O6 C23 C24 120.9(3) . . ? C19 C23 C24 117.5(2) . . ? C23 C24 C25 116.4(3) . . ? C24 C25 C26 111.1(2) . . ? C27 C26 C25 114.8(3) . . ? C28 C27 C26 114.3(3) . . ? C29 C28 C27 115.7(3) . . ? C28 C29 C30 113.2(3) . . ? O6F C23F C19 120.8(7) . . ? O6F C23F C24F 116.8(8) . . ? C19 C23F C24F 116.9(6) . . ? C25F C24F C23F 109.8(6) . . ? C24F C25F C26F 112.5(5) . . ? C27F C26F C25F 113.5(6) . . ? C26F C27F C28F 112.1(6) . . ? C27F C28F C29F 112.5(6) . . ? C30F C29F C28F 109.8(8) . . ? O7A C38A C34A 121.5(2) . . ? O7A C38A C39A 120.9(3) . . ? C34A C38A C39A 117.6(2) . . ? C40A C39A C38A 113.1(2) . . ? C39A C40A C41A 112.4(2) . . ? C40A C41A C42A 112.5(3) . . ? C43A C42A C41A 113.9(3) . . ? C42A C43A C44A 114.9(3) . . ? C45A C44A C43A 111.5(3) . . ? O7K C38K C39K 120.1(8) . . ? O7K C38K C34A 118.1(6) . . ? C39K C38K C34A 121.7(6) . . ? C38K C39K C40K 114.7(6) . . ? C41K C40K C39K 112.1(6) . . ? C40K C41K C42K 111.7(6) . . ? C43K C42K C41K 109.3(6) . . ? C42K C43K C44K 110.7(6) . . ? C43K C44K C45K 108.7(8) . . ? O8A C53A C49A 117.5(5) . . ? O8A C53A C54A 119.8(5) . . ? C49A C53A C54A 119.3(4) . . ? C53A C54A C55A 111.5(4) . . ? C56A C55A C54A 112.2(5) . . ? C55A C56A C57A 114.6(5) . . ? C56A C57A C58A 108.1(5) . . ? C59A C58A C57A 113.1(5) . . ? C58A C59A C60A 106.4(5) . . ? O8K C53K C49A 119.6(4) . . ? O8K C53K C54K 120.2(5) . . ? C49A C53K C54K 119.2(3) . . ? C53K C54K C55K 112.7(4) . . ? C56K C55K C54K 113.7(4) . . ? C55K C56K C57K 114.7(5) . . ? C56K C57K C58K 107.9(5) . . ? C59K C58K C57K 114.2(5) . . ? C58K C59K C60K 112.3(5) . . ? O8L C53L C49A 123.5(7) . . ? O8L C53L C54L 117.4(8) . . ? C49A C53L C54L 118.5(5) . . ? C55L C54L C53L 110.0(7) . . ? C54L C55L C56L 110.4(5) . . ? C57L C56L C55L 109.2(6) . . ? C56L C57L C58L 110.0(6) . . ? C59L C58L C57L 108.5(6) . . ? C60L C59L C58L 110.7(8) . . ? O8M C53M C49A 120.7(8) . . ? O8M C53M C54M 117.3(8) . . ? C49A C53M C54M 119.4(4) . . ? C55M C54M C53M 109.8(7) . . ? C54M C55M C56M 108.9(6) . . ? C57M C56M C55M 108.8(7) . . ? C56M C57M C58M 109.4(6) . . ? C59M C58M C57M 108.1(6) . . ? C60M C59M C58M 109.1(9) . . ? O1A C1A C2A 120.2(2) . . ? O1A C1A C6A 117.41(18) . . ? C2A C1A C6A 122.37(19) . . ? C3A C2A C1A 117.9(2) . . ? C3A C2A C52A 120.39(19) . . ? C1A C2A C52A 121.64(19) . . ? C2A C3A C4A 121.3(2) . . ? C5A C4A C3A 119.03(19) . . ? C5A C4A C8K 123.9(3) . . ? C3A C4A C8K 117.1(3) . . ? C5A C4A C8A 117.8(2) . . ? C3A C4A C8A 123.2(2) . . ? C8K C4A C8A 6.1(3) . . ? C6A C5A C4A 121.8(2) . . ? C5A C6A C1A 117.45(19) . . ? C5A C6A C7A 121.3(2) . . ? C1A C6A C7A 121.21(18) . . ? C6A C7A C17A 115.14(19) . . ? O2A C16A C17A 121.11(19) . . ? O2A C16A C21A 117.28(18) . . ? C17A C16A C21A 121.6(2) . . ? C18A C17A C16A 117.86(19) . . ? C18A C17A C7A 120.60(18) . . ? C16A C17A C7A 121.5(2) . . ? C17A C18A C19A 121.86(19) . . ? C20A C19A C18A 118.2(2) . . ? C20A C19A C23A 117.7(2) . . ? C18A C19A C23A 124.1(2) . . ? C20A C19A C23K 121.4(3) . . ? C18A C19A C23K 120.0(4) . . ? C23A C19A C23K 8.7(5) . . ? C21A C20A C19A 121.8(2) . . ? C20A C21A C16A 118.65(19) . . ? C20A C21A C22A 119.68(19) . . ? C16A C21A C22A 121.6(2) . . ? C32A C22A C21A 111.96(18) . . ? C32A C31A O3A 120.0(2) . . ? C32A C31A C36A 122.9(2) . . ? O3A C31A C36A 117.02(19) . . ? C31A C32A C33A 117.6(2) . . ? C31A C32A C22A 122.5(2) . . ? C33A C32A C22A 119.8(2) . . ? C34A C33A C32A 121.4(2) . . ? C35A C34A C33A 119.3(2) . . ? C35A C34A C38A 117.6(2) . . ? C33A C34A C38A 123.1(2) . . ? C35A C34A C38K 123.7(3) . . ? C33A C34A C38K 116.7(3) . . ? C38A C34A C38K 9.2(3) . . ? C34A C35A C36A 121.2(2) . . ? C35A C36A C31A 117.5(2) . . ? C35A C36A C37A 121.1(2) . . ? C31A C36A C37A 121.3(2) . . ? C36A C37A C47A 113.18(19) . . ? O4A C46A C47A 121.22(18) . . ? O4A C46A C51A 117.29(19) . . ? C47A C46A C51A 121.5(2) . . ? C48A C47A C46A 118.43(19) . . ? C48A C47A C37A 119.6(2) . . ? C46A C47A C37A 121.9(2) . . ? C47A C48A C49A 121.6(2) . . ? C50A C49A C48A 119.1(2) . . ? C50A C49A C53M 111.5(4) . . ? C48A C49A C53M 125.3(3) . . ? C50A C49A C53A 117.3(2) . . ? C48A C49A C53A 122.9(3) . . ? C53M C49A C53A 28.3(7) . . ? C50A C49A C53K 118.8(2) . . ? C48A C49A C53K 121.7(3) . . ? C53M C49A C53K 15.4(7) . . ? C53A C49A C53K 13.7(3) . . ? C50A C49A C53L 119.0(3) . . ? C48A C49A C53L 121.7(3) . . ? C53M C49A C53L 17.6(8) . . ? C53A C49A C53L 11.4(5) . . ? C53K C49A C53L 2.3(6) . . ? C51A C50A C49A 121.2(2) . . ? C50A C51A C46A 118.2(2) . . ? C50A C51A C52A 120.51(19) . . ? C46A C51A C52A 121.3(2) . . ? C2A C52A C51A 112.44(18) . . ? O1 C1 C2 115.56(19) . . ? O1 C1 C6 121.1(2) . . ? C2 C1 C6 123.3(2) . . ? C3 C2 C1 116.9(2) . . ? C3 C2 C52 122.0(2) . . ? C1 C2 C52 121.12(19) . . ? C4 C3 C2 122.2(2) . . ? C3 C4 C5 119.1(2) . . ? C3 C4 C8 118.8(2) . . ? C5 C4 C8 122.1(2) . . ? C6 C5 C4 121.3(2) . . ? C5 C6 C1 117.1(2) . . ? C5 C6 C7 121.5(2) . . ? C1 C6 C7 121.38(19) . . ? C6 C7 C17 112.66(19) . . ? O5 C8 C4 119.0(2) . . ? O5 C8 C9 121.1(2) . . ? C4 C8 C9 119.8(2) . . ? C8 C9 C10 111.0(2) . . ? C11 C10 C9 112.5(2) . . ? C10 C11 C12 113.5(2) . . ? C13 C12 C11 113.6(3) . . ? C12 C13 C14 112.6(3) . . ? C15 C14 C13 112.2(3) . . ? O2 C16 C21 120.26(18) . . ? O2 C16 C17 117.19(18) . . ? C21 C16 C17 122.5(2) . . ? C18 C17 C16 117.8(2) . . ? C18 C17 C7 120.34(19) . . ? C16 C17 C7 121.8(2) . . ? C17 C18 C19 121.5(2) . . ? C20 C19 C18 118.5(2) . . ? C20 C19 C23 120.5(2) . . ? C18 C19 C23 121.0(2) . . ? C20 C19 C23F 131.1(3) . . ? C18 C19 C23F 110.3(3) . . ? C23 C19 C23F 10.8(3) . . ? C21 C20 C19 121.9(2) . . ? C20 C21 C16 117.63(19) . . ? C20 C21 C22 120.15(19) . . ? C16 C21 C22 122.2(2) . . ? C32 C22 C21 112.64(19) . . ? O3 C31 C36 121.3(2) . . ? O3 C31 C32 115.21(18) . . ? C36 C31 C32 123.4(2) . . ? C33 C32 C31 117.5(2) . . ? C33 C32 C22 120.6(2) . . ? C31 C32 C22 121.86(19) . . ? C32 C33 C34 121.2(2) . . ? C35 C34 C33 119.4(2) . . ? C35 C34 C38 122.6(2) . . ? C33 C34 C38 118.1(2) . . ? C34 C35 C36 121.4(2) . . ? C31 C36 C35 117.0(2) . . ? C31 C36 C37 123.56(19) . . ? C35 C36 C37 119.46(19) . . ? C36 C37 C47 114.46(18) . . ? O7 C38 C34 119.7(2) . . ? O7 C38 C39 120.3(2) . . ? C34 C38 C39 120.0(2) . . ? C38 C39 C40 114.1(2) . . ? C41 C40 C39 113.4(2) . . ? C40 C41 C42 112.4(2) . . ? C43 C42 C41 114.7(3) . . ? C42 C43 C44 112.9(3) . . ? C45 C44 C43 112.7(3) . . ? O4 C46 C51 123.29(18) . . ? O4 C46 C47 115.11(18) . . ? C51 C46 C47 121.6(2) . . ? C48 C47 C46 117.88(19) . . ? C48 C47 C37 120.93(18) . . ? C46 C47 C37 121.2(2) . . ? C47 C48 C49 121.78(19) . . ? C48 C49 C50 118.7(2) . . ? C48 C49 C53F 119.6(3) . . ? C50 C49 C53F 121.1(3) . . ? C48 C49 C53 117.9(2) . . ? C50 C49 C53 123.2(2) . . ? C53F C49 C53 12.5(3) . . ? C51 C50 C49 121.8(2) . . ? C50 C51 C46 118.12(19) . . ? C50 C51 C52 120.11(19) . . ? C46 C51 C52 121.8(2) . . ? C2 C52 C51 114.75(19) . . ? O8 C53 C49 121.3(2) . . ? O8 C53 C54 119.8(3) . . ? C49 C53 C54 118.1(2) . . ? C53 C54 C55 113.3(2) . . ? C56 C55 C54 111.1(3) . . ? C57 C56 C55 117.4(3) . . ? C56 C57 C58 112.2(3) . . ? C59 C58 C57 114.9(3) . . ? C58 C59 C60 110.4(4) . . ? O8F C53F C49 115.5(5) . . ? O8F C53F C54F 119.3(6) . . ? C49 C53F C54F 121.5(5) . . ? C53F C54F C55F 111.1(5) . . ? C54F C55F C56F 113.1(6) . . ? C55F C56F C57F 108.8(5) . . ? C58F C57F C56F 110.2(5) . . ? C59F C58F C57F 111.1(5) . . ? C58F C59F C60F 111.1(6) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.34 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.546 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.083