Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Brouwer, E.' 'Enright, Gary D.' 'Halchuk, Peter A.' 'Ooms, Kristopher J.' 'Ripmeester, John' 'Udachin, Kostantin A.' _publ_contact_author_name 'Prof John Ripmeester' _publ_contact_author_address ; Prof John Ripmeester Steacie Institute for Molecular Sciences National Reserch Council Ottawa Ontario K1A OR6 CANADA ; data_kp4 _database_code_CSD 158144 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety C44H56O4·C14H30 _chemical_formula_sum 'C58 H86 O4' _chemical_formula_weight 847.27 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 12.647(3) _cell_length_b 12.659(3) _cell_length_c 17.565(4) _cell_angle_alpha 96.233(5) _cell_angle_beta 100.407(5) _cell_angle_gamma 90.120(5) _cell_volume 2748.8(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.024 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 932 _exptl_absorpt_coefficient_mu 0.062 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17876 _diffrn_reflns_av_R_equivalents 0.1249 _diffrn_reflns_av_sigmaI/netI 0.1753 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 22.30 _reflns_number_total 6465 _reflns_number_gt 2630 _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 w==1/[\s^2^(Fo^2^)+(0.0852P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6465 _refine_ls_number_parameters 927 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1838 _refine_ls_R_factor_gt 0.0889 _refine_ls_wR_factor_ref 0.2178 _refine_ls_wR_factor_gt 0.1975 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.608 _refine_ls_shift/su_mean 0.054 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.672040(11) 0.112260(11) -0.036319(8) 0.04415(5) Uani 1 d . A 1 H1 H 0.7303 0.0921 -0.0491 0.066 Uiso 1 calc R A 1 O2 O 0.609750(11) 0.314190(11) -0.037049(8) 0.04486(5) Uani 1 d . A 1 H2 H 0.5885 0.2508 -0.0502 0.067 Uiso 1 calc R A 1 O3 O 0.810529(11) 0.377631(11) -0.036081(8) 0.04488(5) Uani 1 d . A 1 H30 H 0.7459 0.3940 -0.0491 0.067 Uiso 1 calc R A 1 O4 O 0.873470(11) 0.178639(11) -0.036069(8) 0.04425(5) Uani 1 d . A 1 H4 H 0.8299 0.1274 -0.0516 0.066 Uiso 1 calc R A 1 C1 C 0.661131(17) 0.072651(16) 0.032439(11) 0.03549(7) Uani 1 d . A 1 C2 C 0.571581(16) 0.095582(16) 0.064180(12) 0.03489(7) Uani 1 d . A 1 C3 C 0.560421(17) 0.050571(17) 0.131669(12) 0.03890(8) Uani 1 d . A 1 H3 H 0.4982 0.0657 0.1538 0.047 Uiso 1 calc R A 1 C5 C 0.725641(17) -0.035260(17) 0.131910(12) 0.03916(8) Uani 1 d . A 1 H5 H 0.7791 -0.0804 0.1551 0.047 Uiso 1 calc R A 1 C6 C 0.741409(17) 0.006348(17) 0.064840(12) 0.03714(8) Uani 1 d . A 1 C8 C 0.486081(16) 0.170311(16) 0.030489(13) 0.03995(8) Uani 1 d . A 1 H8A H 0.4155 0.1479 0.0410 0.048 Uiso 1 calc R A 1 H8B H 0.4812 0.1649 -0.0267 0.048 Uiso 1 calc R A 1 C21 C 0.940320(16) 0.158340(17) 0.031678(12) 0.03716(8) Uani 1 d . A 1 C22 C 0.930730(16) 0.064140(17) 0.064530(12) 0.03820(8) Uani 1 d . A 1 C23 C 1.002939(16) 0.046710(17) 0.130651(12) 0.03718(8) Uani 1 d . A 1 H23 H 0.9966 -0.0170 0.1537 0.045 Uiso 1 calc R A 1 C25 C 1.091238(16) 0.212030(17) 0.131249(12) 0.03851(8) Uani 1 d . A 1 H25 H 1.1458 0.2633 0.1545 0.046 Uiso 1 calc R A 1 C26 C 1.020801(17) 0.233292(17) 0.064641(12) 0.03979(8) Uani 1 d . A 1 C28 C 0.842771(16) -0.015309(16) 0.032090(12) 0.03786(8) Uani 1 d . A 1 H28A H 0.8681 -0.0869 0.0433 0.045 Uiso 1 calc R A 1 H28B H 0.8259 -0.0155 -0.0252 0.045 Uiso 1 calc R A 1 C41 C 0.854800(17) 0.437051(16) 0.031650(11) 0.03606(7) Uani 1 d . A 1 C42 C 0.962599(16) 0.423780(16) 0.064969(11) 0.03374(7) Uani 1 d . A 1 C43 C 1.004739(17) 0.490431(16) 0.131523(12) 0.03860(8) Uani 1 d . A 1 H43 H 1.0776 0.4814 0.1547 0.046 Uiso 1 calc R A 1 C45 C 0.839729(17) 0.578778(17) 0.131240(12) 0.03919(8) Uani 1 d . A 1 H45 H 0.7977 0.6312 0.1539 0.047 Uiso 1 calc R A 1 C46 C 0.791762(17) 0.514560(17) 0.064550(12) 0.03608(7) Uani 1 d . A 1 C48 C 1.030530(17) 0.340250(16) 0.031700(12) 0.04005(8) Uani 1 d . A 1 H48A H 1.1067 0.3649 0.0437 0.048 Uiso 1 calc R A 1 H48B H 1.0082 0.3298 -0.0256 0.048 Uiso 1 calc R A 1 C61 C 0.575460(16) 0.351809(17) 0.031218(12) 0.03483(7) Uani 1 d . A 1 C62 C 0.601691(16) 0.455253(16) 0.064179(12) 0.03748(8) Uani 1 d . A 1 C63 C 0.563660(16) 0.492602(17) 0.130898(12) 0.03817(8) Uani 1 d . A 1 H63 H 0.5827 0.5629 0.1542 0.046 Uiso 1 calc R A 1 C65 C 0.475512(17) 0.327580(17) 0.130390(12) 0.03837(8) Uani 1 d . A 1 H65 H 0.4333 0.2830 0.1539 0.046 Uiso 1 calc R A 1 C66 C 0.509780(16) 0.285648(17) 0.064438(12) 0.03638(8) Uani 1 d . A 1 C68 C 0.673378(16) 0.525750(17) 0.030292(13) 0.04152(8) Uani 1 d . A 1 H68A H 0.6530 0.6007 0.0405 0.050 Uiso 1 calc R A 1 H68B H 0.6622 0.5072 -0.0269 0.050 Uiso 1 calc R A 1 C4 C 0.636880(17) -0.015315(17) 0.167420(12) 0.03958(8) Uani 1 d . A 1 C7A C 0.63085(4) -0.06549(4) 0.24082(3) 0.05251(18) Uani 0.4908(2) d P A 1 C9A C 0.72826(5) -0.03428(5) 0.30523(3) 0.0890(3) Uani 0.4908(2) d P A 1 H9A1 H 0.7216 -0.0687 0.3515 0.133 Uiso 0.4908(2) calc PR A 1 H9A2 H 0.7312 0.0431 0.3183 0.133 Uiso 0.4908(2) calc PR A 1 H9A3 H 0.7942 -0.0572 0.2870 0.133 Uiso 0.4908(2) calc PR A 1 C10A C 0.62224(5) -0.18737(4) 0.21983(3) 0.0778(2) Uani 0.4908(2) d P A 1 H10A H 0.6169 -0.2216 0.2665 0.117 Uiso 0.4908(2) calc PR A 1 H10B H 0.6863 -0.2122 0.1997 0.117 Uiso 0.4908(2) calc PR A 1 H10C H 0.5580 -0.2056 0.1800 0.117 Uiso 0.4908(2) calc PR A 1 C11A C 0.53193(5) -0.03009(5) 0.27516(3) 0.1490(2) Uani 0.4908(2) d P A 1 H11A H 0.5299 -0.0656 0.3218 0.224 Uiso 0.4908(2) calc PR A 1 H11B H 0.4667 -0.0491 0.2365 0.224 Uiso 0.4908(2) calc PR A 1 H11C H 0.5359 0.0471 0.2892 0.224 Uiso 0.4908(2) calc PR A 1 C24 C 1.085041(18) 0.120099(17) 0.164561(12) 0.04092(8) Uani 1 d . A 1 C27A C 1.16799(5) 0.10370(4) 0.23662(3) 0.0595(2) Uani 0.4197(2) d P A 1 C29A C 1.16767(6) 0.19752(6) 0.30020(4) 0.0875(3) Uani 0.4197(2) d P A 1 H29A H 1.2217 0.1864 0.3460 0.131 Uiso 0.4197(2) calc PR A 1 H29B H 1.0964 0.2022 0.3147 0.131 Uiso 0.4197(2) calc PR A 1 H29C H 1.1847 0.2637 0.2803 0.131 Uiso 0.4197(2) calc PR A 1 C30A C 1.27864(5) 0.09978(5) 0.21246(4) 0.0672(2) Uani 0.4197(2) d P A 1 H30A H 1.3339 0.0882 0.2575 0.101 Uiso 0.4197(2) calc PR A 1 H30B H 1.2938 0.1672 0.1935 0.101 Uiso 0.4197(2) calc PR A 1 H30C H 1.2790 0.0414 0.1710 0.101 Uiso 0.4197(2) calc PR A 1 C31A C 1.14623(6) -0.00170(6) 0.26717(4) 0.0957(3) Uani 0.4197(2) d P A 1 H31A H 1.2012 -0.0115 0.3127 0.144 Uiso 0.4197(2) calc PR A 1 H31B H 1.1485 -0.0605 0.2263 0.144 Uiso 0.4197(2) calc PR A 1 H31C H 1.0751 -0.0005 0.2820 0.144 Uiso 0.4197(2) calc PR A 1 C44 C 0.947981(17) 0.569390(17) 0.166539(12) 0.03911(8) Uani 1 d . A 1 C47A C 0.98887(4) 0.64415(4) 0.23897(3) 0.04559(17) Uani 0.4803(2) d P A 1 C49A C 0.92082(5) 0.63451(4) 0.30101(3) 0.0758(2) Uani 0.4803(2) d P A 1 H49A H 0.9496 0.6831 0.3475 0.114 Uiso 0.4803(2) calc PR A 1 H49B H 0.9225 0.5614 0.3145 0.114 Uiso 0.4803(2) calc PR A 1 H49C H 0.8465 0.6528 0.2810 0.114 Uiso 0.4803(2) calc PR A 1 C50A C 0.98650(5) 0.75768(4) 0.21495(3) 0.0696(2) Uani 0.4803(2) d P A 1 H50A H 1.0141 0.8081 0.2606 0.104 Uiso 0.4803(2) calc PR A 1 H50B H 0.9124 0.7752 0.1935 0.104 Uiso 0.4803(2) calc PR A 1 H50C H 1.0315 0.7620 0.1754 0.104 Uiso 0.4803(2) calc PR A 1 C51A C 1.10674(4) 0.61862(5) 0.26625(4) 0.0843(3) Uani 0.4803(2) d P A 1 H51A H 1.1364 0.6663 0.3130 0.126 Uiso 0.4803(2) calc PR A 1 H51B H 1.1475 0.6284 0.2250 0.126 Uiso 0.4803(2) calc PR A 1 H51C H 1.1120 0.5448 0.2782 0.126 Uiso 0.4803(2) calc PR A 1 C64 C 0.497749(17) 0.430001(18) 0.165352(12) 0.04320(8) Uani 1 d . A 1 C67A C 0.45472(3) 0.46708(3) 0.23905(2) 0.04915(13) Uani 0.6637(2) d P A 1 C69A C 0.48925(4) 0.39346(4) 0.30283(2) 0.08445(18) Uani 0.6637(2) d P A 1 H69A H 0.4600 0.4191 0.3493 0.127 Uiso 0.6637(2) calc PR A 1 H69B H 0.5679 0.3932 0.3160 0.127 Uiso 0.6637(2) calc PR A 1 H69C H 0.4618 0.3211 0.2838 0.127 Uiso 0.6637(2) calc PR A 1 C70A C 0.33081(3) 0.46552(3) 0.21846(2) 0.07987(17) Uani 0.6637(2) d P A 1 H70A H 0.3014 0.4900 0.2651 0.120 Uiso 0.6637(2) calc PR A 1 H70B H 0.3045 0.3929 0.1991 0.120 Uiso 0.6637(2) calc PR A 1 H70C H 0.3078 0.5126 0.1781 0.120 Uiso 0.6637(2) calc PR A 1 C71A C 0.49038(4) 0.58350(3) 0.26826(3) 0.09146(18) Uani 0.6637(2) d P A 1 H71A H 0.4609 0.6066 0.3151 0.137 Uiso 0.6637(2) calc PR A 1 H71B H 0.4638 0.6291 0.2276 0.137 Uiso 0.6637(2) calc PR A 1 H71C H 0.5691 0.5886 0.2806 0.137 Uiso 0.6637(2) calc PR A 1 C7B C 0.61175(4) -0.06283(4) 0.23895(3) 0.05251(18) Uani 0.5092(2) d P A -2 C9B C 0.70623(5) -0.12988(5) 0.27399(3) 0.1355(3) Uani 0.5092(2) d P A -2 H9B1 H 0.6901 -0.1575 0.3207 0.203 Uiso 0.5092(2) calc PR A -2 H9B2 H 0.7719 -0.0854 0.2878 0.203 Uiso 0.5092(2) calc PR A -2 H9B3 H 0.7167 -0.1893 0.2356 0.203 Uiso 0.5092(2) calc PR A -2 C10B C 0.51159(4) -0.13442(4) 0.21954(3) 0.0749(2) Uani 0.5092(2) d P A -2 H10D H 0.4984 -0.1625 0.2669 0.112 Uiso 0.5092(2) calc PR A -2 H10E H 0.5221 -0.1935 0.1809 0.112 Uiso 0.5092(2) calc PR A -2 H10F H 0.4497 -0.0934 0.1983 0.112 Uiso 0.5092(2) calc PR A -2 C11B C 0.59281(5) 0.02998(5) 0.29779(3) 0.1040(3) Uani 0.5092(2) d P A -2 H11D H 0.5793 0.0027 0.3453 0.156 Uiso 0.5092(2) calc PR A -2 H11E H 0.5305 0.0696 0.2754 0.156 Uiso 0.5092(2) calc PR A -2 H11F H 0.6565 0.0772 0.3103 0.156 Uiso 0.5092(2) calc PR A -2 C27B C 1.16574(4) 0.09187(3) 0.23601(2) 0.05955(16) Uani 0.5803(2) d P A -2 C29B C 1.25228(4) 0.17870(4) 0.26759(3) 0.0926(2) Uani 0.5803(2) d P A -2 H29D H 1.3003 0.1565 0.3131 0.139 Uiso 0.5803(2) calc PR A -2 H29E H 1.2178 0.2450 0.2827 0.139 Uiso 0.5803(2) calc PR A -2 H29F H 1.2939 0.1900 0.2271 0.139 Uiso 0.5803(2) calc PR A -2 C30B C 1.22299(4) -0.01185(4) 0.21794(3) 0.07373(19) Uani 0.5803(2) d P A -2 H30D H 1.2732 -0.0274 0.2645 0.111 Uiso 0.5803(2) calc PR A -2 H30E H 1.2627 -0.0045 0.1757 0.111 Uiso 0.5803(2) calc PR A -2 H30F H 1.1697 -0.0701 0.2020 0.111 Uiso 0.5803(2) calc PR A -2 C31B C 1.10323(4) 0.07459(4) 0.30199(3) 0.0957(2) Uani 0.5803(2) d P A -2 H31D H 1.1537 0.0568 0.3478 0.144 Uiso 0.5803(2) calc PR A -2 H31E H 1.0505 0.0162 0.2842 0.144 Uiso 0.5803(2) calc PR A -2 H31F H 1.0660 0.1398 0.3157 0.144 Uiso 0.5803(2) calc PR A -2 C47B C 1.00655(3) 0.63861(4) 0.23892(3) 0.05450(18) Uani 0.5197(2) d P A -2 C49B C 0.93060(5) 0.72028(5) 0.26948(4) 0.1232(3) Uani 0.5197(2) d P A -2 H49D H 0.9696 0.7638 0.3156 0.185 Uiso 0.5197(2) calc PR A -2 H49E H 0.8699 0.6832 0.2834 0.185 Uiso 0.5197(2) calc PR A -2 H49F H 0.9038 0.7661 0.2290 0.185 Uiso 0.5197(2) calc PR A -2 C50B C 1.09829(4) 0.70450(4) 0.21891(3) 0.0858(2) Uani 0.5197(2) d P A -2 H50D H 1.1338 0.7490 0.2657 0.129 Uiso 0.5197(2) calc PR A -2 H50E H 1.0688 0.7498 0.1787 0.129 Uiso 0.5197(2) calc PR A -2 H50F H 1.1507 0.6566 0.1996 0.129 Uiso 0.5197(2) calc PR A -2 C51B C 1.05453(5) 0.57590(4) 0.30519(3) 0.0835(2) Uani 0.5197(2) d P A -2 H51D H 1.0892 0.6250 0.3498 0.125 Uiso 0.5197(2) calc PR A -2 H51E H 1.1079 0.5272 0.2882 0.125 Uiso 0.5197(2) calc PR A -2 H51F H 0.9974 0.5350 0.3205 0.125 Uiso 0.5197(2) calc PR A -2 C67B C 0.45793(6) 0.48484(6) 0.23666(4) 0.0620(3) Uani 0.3363(2) d P A -2 C69B C 0.39323(8) 0.40318(7) 0.26955(5) 0.1267(4) Uani 0.3363(2) d P A -2 H69D H 0.3670 0.4373 0.3152 0.190 Uiso 0.3363(2) calc PR A -2 H69E H 0.4395 0.3442 0.2848 0.190 Uiso 0.3363(2) calc PR A -2 H69F H 0.3320 0.3760 0.2296 0.190 Uiso 0.3363(2) calc PR A -2 C70B C 0.38624(6) 0.57842(6) 0.21264(5) 0.0774(3) Uani 0.3363(2) d P A -2 H70D H 0.3598 0.6127 0.2581 0.116 Uiso 0.3363(2) calc PR A -2 H70E H 0.3251 0.5519 0.1724 0.116 Uiso 0.3363(2) calc PR A -2 H70F H 0.4283 0.6301 0.1921 0.116 Uiso 0.3363(2) calc PR A -2 C71B C 0.55211(7) 0.52787(8) 0.30076(5) 0.0940(4) Uani 0.3363(2) d P A -2 H71D H 0.5241 0.5613 0.3458 0.141 Uiso 0.3363(2) calc PR A -2 H71E H 0.5937 0.5806 0.2809 0.141 Uiso 0.3363(2) calc PR A -2 H71F H 0.5985 0.4692 0.3165 0.141 Uiso 0.3363(2) calc PR A -2 C1D C -0.2021 0.2788 0.1952 0.2069(9) Uani 0.33 d P B -1 H1D1 H -0.2651 0.3237 0.1956 0.310 Uiso 0.33 calc PR B -1 H1D2 H -0.2147 0.2269 0.1487 0.310 Uiso 0.33 calc PR B -1 H1D3 H -0.1388 0.3233 0.1946 0.310 Uiso 0.33 calc PR B -1 C2D C -0.1829 0.2202 0.2684 0.3272(14) Uani 0.33 d P B -1 H2D1 H -0.2487 0.1794 0.2711 0.393 Uiso 0.33 calc PR B -1 H2D2 H -0.1240 0.1694 0.2654 0.393 Uiso 0.33 calc PR B -1 C3D C -0.1533 0.2991 0.3420 0.1926(8) Uani 0.33 d P B -1 H3D1 H -0.2197 0.3279 0.3578 0.231 Uiso 0.33 calc PR B -1 H3D2 H -0.1105 0.3592 0.3307 0.231 Uiso 0.33 calc PR B -1 C4D C -0.0880 0.2447 0.4087 0.1681(7) Uani 0.33 d P B -1 H4D1 H -0.0220 0.2151 0.3927 0.202 Uiso 0.33 calc PR B -1 H4D2 H -0.0664 0.2976 0.4548 0.202 Uiso 0.33 calc PR B -1 C5D C -0.1556 0.1552 0.4298 0.3604(19) Uani 0.33 d P B -1 H5D1 H -0.2320 0.1756 0.4229 0.432 Uiso 0.33 calc PR B -1 H5D2 H -0.1505 0.0898 0.3944 0.432 Uiso 0.33 calc PR B -1 C6D C -0.1163 0.1333 0.5143 0.3116(12) Uani 0.33 d P B -1 H6D1 H -0.1132 0.2005 0.5492 0.374 Uiso 0.33 calc PR B -1 H6D2 H -0.1675 0.0838 0.5296 0.374 Uiso 0.33 calc PR B -1 C7D C -0.0045 0.0844 0.5231 0.2215(10) Uani 0.33 d P B -1 H7D1 H 0.0406 0.1157 0.5724 0.266 Uiso 0.33 calc PR B -1 H7D2 H 0.0306 0.1008 0.4796 0.266 Uiso 0.33 calc PR B -1 C8D C -0.0138 -0.0364 0.5230 0.2049(9) Uani 0.33 d P B -1 H8D1 H -0.0465 -0.0692 0.4702 0.246 Uiso 0.33 calc PR B -1 H8D2 H -0.0611 -0.0530 0.5595 0.246 Uiso 0.33 calc PR B -1 C9D C 0.0977 -0.0826 0.5475 0.2643(13) Uani 0.33 d P B -1 H9D1 H 0.1179 -0.1270 0.5026 0.317 Uiso 0.33 calc PR B -1 H9D2 H 0.1517 -0.0239 0.5639 0.317 Uiso 0.33 calc PR B -1 C10D C 0.0976 -0.1501 0.6150 0.2759(13) Uani 0.33 d P B -1 H10G H 0.1404 -0.1132 0.6633 0.331 Uiso 0.33 calc PR B -1 H10H H 0.0230 -0.1597 0.6234 0.331 Uiso 0.33 calc PR B -1 C11D C 0.1456 -0.2590 0.5964 0.2733(13) Uani 0.33 d P B -1 H11G H 0.0906 -0.3054 0.5608 0.328 Uiso 0.33 calc PR B -1 H11H H 0.2069 -0.2502 0.5695 0.328 Uiso 0.33 calc PR B -1 C12D C 0.1839 -0.3116 0.6705 0.1324(6) Uani 0.33 d P B -1 H12A H 0.2632 -0.3052 0.6845 0.159 Uiso 0.33 calc PR B -1 H12B H 0.1639 -0.3882 0.6608 0.159 Uiso 0.33 calc PR B -1 C13D C 0.1341 -0.2603 0.7385 0.1083(5) Uani 0.33 d P B -1 H13A H 0.0624 -0.2931 0.7367 0.130 Uiso 0.33 calc PR B -1 H13B H 0.1247 -0.1835 0.7340 0.130 Uiso 0.33 calc PR B -1 C14D C 0.2072 -0.2756 0.8162 0.1220(5) Uani 0.33 d P B -1 H14A H 0.2105 -0.3514 0.8229 0.183 Uiso 0.33 calc PR B -1 H14B H 0.1782 -0.2371 0.8591 0.183 Uiso 0.33 calc PR B -1 H14C H 0.2796 -0.2480 0.8162 0.183 Uiso 0.33 calc PR B -1 C1E C -0.19960(6) 0.27515(6) 0.18811(4) 0.0551(3) Uani 0.33 d P C -2 H1E1 H -0.1305 0.2705 0.1703 0.083 Uiso 0.33 calc PR C -2 H1E2 H -0.2540 0.3013 0.1478 0.083 Uiso 0.33 calc PR C -2 H1E3 H -0.2217 0.2046 0.1984 0.083 Uiso 0.33 calc PR C -2 C2E C -0.18820(11) 0.35084(9) 0.26194(6) 0.1312(6) Uani 0.33 d P C -2 H2E1 H -0.2604 0.3757 0.2689 0.157 Uiso 0.33 calc PR C -2 H2E2 H -0.1447 0.4137 0.2563 0.157 Uiso 0.33 calc PR C -2 C3E C -0.13548(15) 0.30141(13) 0.33473(9) 0.2191(9) Uani 0.33 d P C -2 H3E1 H -0.0596 0.2854 0.3320 0.263 Uiso 0.33 calc PR C -2 H3E2 H -0.1736 0.2342 0.3382 0.263 Uiso 0.33 calc PR C -2 C4E C -0.14103(14) 0.38059(13) 0.40662(8) 0.2180(8) Uani 0.33 d P C -2 H4E1 H -0.1003 0.4465 0.4039 0.262 Uiso 0.33 calc PR C -2 H4E2 H -0.2168 0.3993 0.4076 0.262 Uiso 0.33 calc PR C -2 C5E C -0.0935(3) 0.33153(19) 0.48111(11) 0.390(2) Uani 0.33 d P C -2 H5E1 H -0.1512 0.2945 0.5000 0.468 Uiso 0.33 calc PR C -2 H5E2 H -0.0619 0.3883 0.5222 0.468 Uiso 0.33 calc PR C -2 C6E C -0.0065(2) 0.25240(17) 0.46453(11) 0.3546(18) Uani 0.33 d P C -2 H6E1 H 0.0654 0.2850 0.4860 0.426 Uiso 0.33 calc PR C -2 H6E2 H -0.0119 0.2358 0.4076 0.426 Uiso 0.33 calc PR C -2 C7E C -0.01900(16) 0.14901(19) 0.50126(13) 0.2887(14) Uani 0.33 d P C -2 H7E1 H -0.0573 0.1634 0.5456 0.346 Uiso 0.33 calc PR C -2 H7E2 H -0.0619 0.0959 0.4623 0.346 Uiso 0.33 calc PR C -2 C8E C 0.0924(2) 0.10530(16) 0.52964(10) 0.3107(14) Uani 0.33 d P C -2 H8E1 H 0.1056 0.1093 0.5872 0.373 Uiso 0.33 calc PR C -2 H8E2 H 0.1478 0.1503 0.5147 0.373 Uiso 0.33 calc PR C -2 C9E C 0.10370(17) -0.01095(16) 0.49538(9) 0.2591(12) Uani 0.33 d P C -2 H9E1 H 0.0594 -0.0590 0.5183 0.311 Uiso 0.33 calc PR C -2 H9E2 H 0.0788 -0.0186 0.4382 0.311 Uiso 0.33 calc PR C -2 C10E C 0.2230(3) -0.0398(2) 0.51465(12) 0.464(3) Uani 0.33 d P C -2 H10I H 0.2679 0.0210 0.5071 0.556 Uiso 0.33 calc PR C -2 H10J H 0.2410 -0.0523 0.5701 0.556 Uiso 0.33 calc PR C -2 C11E C 0.25039(14) -0.13846(13) 0.46436(8) 0.2044(9) Uani 0.33 d P C -2 H11I H 0.2007 -0.1459 0.4135 0.245 Uiso 0.33 calc PR C -2 H11J H 0.2421 -0.2027 0.4905 0.245 Uiso 0.33 calc PR C -2 C12E C 0.36693(13) -0.12786(13) 0.45172(9) 0.2392(9) Uani 0.33 d P C -2 H12C H 0.3684 -0.1389 0.3953 0.287 Uiso 0.33 calc PR C -2 H12D H 0.3951 -0.0552 0.4717 0.287 Uiso 0.33 calc PR C -2 C13E C 0.43883(17) -0.20878(15) 0.49323(9) 0.2703(11) Uani 0.33 d P C -2 H13C H 0.4224 -0.2807 0.4651 0.324 Uiso 0.33 calc PR C -2 H13D H 0.4247 -0.2097 0.5468 0.324 Uiso 0.33 calc PR C -2 C14E C 0.55783(18) -0.17926(16) 0.49632(10) 0.3464(12) Uani 0.33 d P C -2 H14D H 0.5712 -0.1771 0.4433 0.520 Uiso 0.33 calc PR C -2 H14E H 0.6035 -0.2326 0.5216 0.520 Uiso 0.33 calc PR C -2 H14F H 0.5745 -0.1093 0.5261 0.520 Uiso 0.33 calc PR C -2 C1F C 0.38197(11) 0.78886(11) 0.44370(7) 0.1695(7) Uani 0.33 d P D -1 H1F1 H 0.4070 0.7882 0.3940 0.254 Uiso 0.33 calc PR D -1 H1F2 H 0.3653 0.8618 0.4620 0.254 Uiso 0.33 calc PR D -1 H1F3 H 0.3172 0.7435 0.4365 0.254 Uiso 0.33 calc PR D -1 C2F C 0.46998(11) 0.74694(11) 0.50390(7) 0.1866(6) Uani 0.33 d P D -1 H2F1 H 0.4545 0.6713 0.5080 0.224 Uiso 0.33 calc PR D -1 H2F2 H 0.4707 0.7874 0.5555 0.224 Uiso 0.33 calc PR D -1 C3F C 0.58041(10) 0.75778(10) 0.48069(7) 0.1551(6) Uani 0.33 d P D -1 H3F1 H 0.5722 0.7539 0.4233 0.186 Uiso 0.33 calc PR D -1 H3F2 H 0.6145 0.8272 0.5036 0.186 Uiso 0.33 calc PR D -1 C4F C 0.65064(10) 0.66728(10) 0.51074(7) 0.1432(6) Uani 0.33 d P D -1 H4F1 H 0.6652 0.6761 0.5684 0.172 Uiso 0.33 calc PR D -1 H4F2 H 0.6122 0.5983 0.4928 0.172 Uiso 0.33 calc PR D -1 C5F C 0.75679(7) 0.66790(10) 0.48064(5) 0.1142(5) Uani 0.33 d P D -1 H5F1 H 0.7995 0.7331 0.5034 0.137 Uiso 0.33 calc PR D -1 H5F2 H 0.7426 0.6667 0.4232 0.137 Uiso 0.33 calc PR D -1 C6F C 0.81900(11) 0.56917(12) 0.50434(7) 0.1650(7) Uani 0.33 d P D -1 H6F1 H 0.8285 0.5681 0.5614 0.198 Uiso 0.33 calc PR D -1 H6F2 H 0.7781 0.5041 0.4788 0.198 Uiso 0.33 calc PR D -1 C7F C 0.9291(3) 0.5717(2) 0.47971(16) 0.372(2) Uani 0.33 d P D -1 H7F1 H 0.9264 0.5266 0.4296 0.446 Uiso 0.33 calc PR D -1 H7F2 H 0.9479 0.6453 0.4722 0.446 Uiso 0.33 calc PR D -1 C8F C 1.01447(18) 0.53089(14) 0.54230(7) 0.2642(13) Uani 0.33 d P D -1 H8F1 H 0.9953 0.4575 0.5501 0.317 Uiso 0.33 calc PR D -1 H8F2 H 1.0176 0.5763 0.5923 0.317 Uiso 0.33 calc PR D -1 C9F C 1.12425(17) 0.53258(14) 0.51723(10) 0.2595(11) Uani 0.33 d P D -1 H9F1 H 1.1143 0.5292 0.4598 0.311 Uiso 0.33 calc PR D -1 H9F2 H 1.1637 0.5996 0.5399 0.311 Uiso 0.33 calc PR D -1 C10F C 1.18924(17) 0.43774(14) 0.54488(9) 0.2514(11) Uani 0.33 d P D -1 H10K H 1.1401 0.3771 0.5458 0.302 Uiso 0.33 calc PR D -1 H10L H 1.2297 0.4569 0.5984 0.302 Uiso 0.33 calc PR D -1 C11F C 1.26741(9) 0.40599(11) 0.48976(5) 0.1544(6) Uani 0.33 d P D -1 H11K H 1.3233 0.4624 0.4946 0.185 Uiso 0.33 calc PR D -1 H11L H 1.2283 0.3969 0.4352 0.185 Uiso 0.33 calc PR D -1 C12F C 1.32021(10) 0.30108(11) 0.51083(5) 0.1592(6) Uani 0.33 d P D -1 H12E H 1.3212 0.2937 0.5665 0.191 Uiso 0.33 calc PR D -1 H12F H 1.2788 0.2401 0.4791 0.191 Uiso 0.33 calc PR D -1 C13F C 1.43509(18) 0.30237(17) 0.49482(10) 0.2734(13) Uani 0.33 d P D -1 H13E H 1.4336 0.2880 0.4381 0.328 Uiso 0.33 calc PR D -1 H13F H 1.4687 0.3735 0.5128 0.328 Uiso 0.33 calc PR D -1 C14F C 1.50182(10) 0.21838(10) 0.53697(6) 0.1457(6) Uani 0.33 d P D -1 H14G H 1.4850 0.1483 0.5074 0.218 Uiso 0.33 calc PR D -1 H14H H 1.4847 0.2177 0.5892 0.218 Uiso 0.33 calc PR D -1 H14I H 1.5785 0.2353 0.5413 0.218 Uiso 0.33 calc PR D -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 0.03399(8) 0.03796(9) 0.06113(9) 0.00510(7) 0.01061(7) -0.00393(8) O2 0.04828(9) 0.03630(9) 0.04987(8) 0.01207(7) 0.00425(7) -0.00297(8) O3 0.03489(8) 0.04366(9) 0.05743(9) 0.01847(7) 0.00424(7) 0.00308(8) O4 0.04532(9) 0.03696(9) 0.04874(8) 0.01015(7) 0.00079(7) -0.00482(8) C1 0.03645(12) 0.03121(13) 0.03979(12) 0.01069(10) 0.00571(10) -0.01612(11) C2 0.02840(12) 0.02094(12) 0.05683(13) 0.01321(10) 0.00648(10) -0.00030(10) C3 0.02858(12) 0.02911(13) 0.05927(14) 0.00113(11) 0.01095(11) -0.00048(11) C5 0.02948(12) 0.02693(13) 0.05959(14) 0.01228(11) -0.00025(11) -0.00018(11) C6 0.03025(12) 0.02464(12) 0.05565(13) 0.00949(11) 0.00241(11) 0.00400(11) C8 0.02505(12) 0.02785(13) 0.06713(14) 0.01122(11) 0.00529(11) 0.00008(11) C21 0.03114(12) 0.03295(13) 0.04996(13) 0.00448(11) 0.01438(10) -0.00527(11) C22 0.02888(12) 0.02740(13) 0.06173(14) 0.00876(11) 0.01507(10) -0.00025(11) C23 0.03657(12) 0.02641(12) 0.05296(13) 0.01690(10) 0.01238(10) 0.00099(11) C25 0.02826(12) 0.02881(13) 0.05973(14) 0.01080(11) 0.00790(10) 0.00222(11) C26 0.03332(12) 0.03160(13) 0.06091(13) 0.01301(11) 0.02099(10) 0.00523(11) C28 0.04349(13) 0.01723(12) 0.05560(13) 0.00735(10) 0.01429(11) 0.00530(11) C41 0.03726(12) 0.03171(12) 0.04136(12) 0.01582(10) 0.00597(10) -0.01051(11) C42 0.03107(12) 0.02161(12) 0.05362(13) 0.01547(10) 0.01447(10) -0.00137(10) C43 0.02628(12) 0.03164(13) 0.05964(14) 0.01985(11) 0.00364(11) 0.00382(11) C45 0.03394(12) 0.02686(12) 0.06335(13) 0.01450(10) 0.02067(10) 0.00540(11) C46 0.03156(12) 0.02818(12) 0.05046(13) 0.01464(10) 0.00656(10) 0.00055(11) C48 0.03202(12) 0.02908(13) 0.06538(14) 0.02299(11) 0.01513(11) 0.00008(11) C61 0.02668(12) 0.03272(13) 0.04444(12) 0.01384(10) -0.00098(10) 0.00506(11) C62 0.02646(12) 0.02628(12) 0.05851(14) 0.01446(10) -0.00127(11) 0.00327(11) C63 0.03115(12) 0.02293(12) 0.05918(14) 0.00917(11) 0.00211(11) 0.00226(11) C65 0.03400(12) 0.02371(12) 0.05920(13) 0.01193(10) 0.00899(11) -0.00264(11) C66 0.02276(11) 0.02525(12) 0.06038(14) 0.01227(10) 0.00111(10) -0.00026(10) C68 0.03272(13) 0.02862(13) 0.06563(14) 0.01927(11) 0.00697(11) 0.00544(11) C4 0.03367(12) 0.03180(13) 0.05678(13) 0.01730(10) 0.01013(10) 0.00166(11) C7A 0.0373(3) 0.0479(3) 0.0774(3) 0.0155(3) 0.0188(2) 0.0025(3) C9A 0.0942(4) 0.0777(4) 0.1038(4) 0.0426(3) 0.0223(3) -0.0106(4) C10A 0.1186(5) 0.0382(3) 0.0841(3) 0.0324(2) 0.0233(3) -0.0185(3) C11A 0.1303(4) 0.1654(4) 0.2226(4) 0.1742(3) 0.1295(3) 0.0974(4) C24 0.04285(13) 0.03277(13) 0.04623(13) 0.01386(10) 0.00002(11) 0.00227(12) C27A 0.0790(4) 0.0245(3) 0.0861(4) 0.0125(3) 0.0405(3) -0.0052(3) C29A 0.0830(5) 0.1102(6) 0.0716(4) 0.0253(4) 0.0112(4) 0.0313(5) C30A 0.0475(4) 0.0713(4) 0.0794(4) 0.0156(3) -0.0024(3) 0.0264(3) C31A 0.0775(5) 0.1077(5) 0.0972(5) 0.0532(4) -0.0215(4) 0.0051(5) C44 0.03642(12) 0.02743(13) 0.05652(13) 0.01116(11) 0.01264(11) 0.00125(11) C47A 0.0472(3) 0.0307(3) 0.0618(3) 0.0223(2) 0.0075(2) 0.0219(2) C49A 0.0995(5) 0.0530(4) 0.0681(4) -0.0002(3) 0.0017(3) -0.0169(4) C50A 0.0720(4) 0.0387(3) 0.0894(4) -0.0060(3) -0.0001(3) -0.0162(3) C51A 0.0573(4) 0.0736(4) 0.1028(4) -0.0334(4) -0.0107(3) -0.0082(3) C64 0.03205(12) 0.04307(14) 0.05757(14) 0.01847(11) 0.00863(11) 0.00343(12) C67A 0.0418(2) 0.0269(2) 0.0787(2) -0.00589(18) 0.01814(18) -0.02193(17) C69A 0.0803(3) 0.0984(3) 0.0817(3) 0.0366(2) 0.0176(2) 0.0078(3) C70A 0.0561(2) 0.0732(3) 0.1235(3) 0.0231(2) 0.0441(2) 0.0150(2) C71A 0.1157(3) 0.0411(3) 0.1306(3) -0.0026(2) 0.0647(2) -0.0236(2) C7B 0.0373(3) 0.0479(3) 0.0774(3) 0.0155(2) 0.0188(2) 0.0025(2) C9B 0.0864(4) 0.2328(5) 0.1289(4) 0.1424(3) 0.0568(3) 0.0881(4) C10B 0.0867(4) 0.0484(3) 0.1050(4) 0.0249(3) 0.0490(3) -0.0042(3) C11B 0.1725(5) 0.0815(4) 0.0818(3) 0.0384(3) 0.0694(3) -0.0174(4) C27B 0.0790(3) 0.0245(2) 0.0861(3) 0.0125(2) 0.0405(2) -0.0052(2) C29B 0.1023(4) 0.0578(3) 0.1002(4) 0.0265(3) -0.0382(3) -0.0237(3) C30B 0.0707(3) 0.0680(3) 0.0796(3) 0.0293(2) -0.0065(3) 0.0058(3) C31B 0.0774(4) 0.1078(4) 0.0972(3) 0.0531(3) -0.0214(3) 0.0052(3) C47B 0.0338(3) 0.0501(3) 0.0780(3) -0.0025(3) 0.0117(2) -0.0081(2) C49B 0.1050(5) 0.1146(5) 0.1128(5) -0.0634(4) -0.0344(4) 0.0403(4) C50B 0.0745(4) 0.0606(4) 0.1138(4) 0.0044(3) -0.0021(3) -0.0265(3) C51B 0.1200(5) 0.0720(4) 0.0555(3) 0.0233(3) -0.0015(3) -0.0062(4) C67B 0.0678(5) 0.0868(5) 0.0427(4) 0.0550(3) 0.0120(3) 0.0048(4) C69B 0.2285(9) 0.0648(6) 0.1050(5) -0.0509(5) 0.1149(5) -0.0484(6) C70B 0.0646(4) 0.0512(5) 0.1259(6) -0.0134(5) 0.0565(4) 0.0192(4) C71B 0.0750(6) 0.1229(8) 0.0702(5) -0.0271(5) -0.0017(5) 0.0226(6) C1D 0.2268(17) 0.1070(11) 0.2648(17) 0.0063(11) -0.0058(14) -0.0027(12) C2D 0.2809(19) 0.2555(18) 0.400(3) -0.022(2) -0.020(2) -0.1659(14) C3D 0.2367(16) 0.2271(15) 0.1120(9) 0.0611(9) 0.0010(10) 0.0010(13) C4D 0.1644(12) 0.2276(14) 0.1126(8) 0.0605(8) 0.0010(8) 0.0013(11) C5D 0.724(5) 0.2267(18) 0.1120(11) 0.0614(11) 0.0012(19) 0.001(3) C6D 0.395(2) 0.276(2) 0.1918(13) 0.0248(13) -0.1387(13) 0.1288(17) C7D 0.2112(16) 0.293(2) 0.1273(11) -0.0239(12) -0.0293(11) 0.0261(17) C8D 0.2715(19) 0.2274(17) 0.1123(11) 0.0610(9) 0.0008(12) 0.0012(16) C9D 0.444(3) 0.2275(17) 0.1123(10) 0.0609(10) 0.0009(14) 0.001(2) C10D 0.477(3) 0.2272(17) 0.1126(10) 0.0608(10) 0.0012(15) 0.001(2) C11D 0.343(3) 0.291(2) 0.1981(14) 0.0938(13) 0.0407(15) 0.043(2) C12D 0.0887(7) 0.2124(13) 0.0871(7) 0.0152(8) -0.0064(6) -0.0351(8) C13D 0.1234(8) 0.0914(7) 0.1086(7) 0.0175(6) 0.0127(6) 0.0315(7) C14D 0.1033(8) 0.0931(8) 0.1681(10) 0.0307(7) 0.0111(7) -0.0073(7) C1E 0.0635(5) 0.0551(5) 0.0490(4) 0.0080(4) 0.0152(4) -0.0094(4) C2E 0.1688(11) 0.1178(9) 0.1066(7) 0.0297(6) 0.0141(7) -0.0072(9) C3E 0.2812(17) 0.1841(14) 0.2007(13) 0.0009(11) 0.0785(11) 0.0859(12) C4E 0.2262(14) 0.2604(15) 0.1767(11) 0.0673(10) 0.0367(10) -0.1107(11) C5E 0.724(5) 0.261(2) 0.1773(15) 0.0668(14) 0.037(2) -0.110(3) C6E 0.621(4) 0.261(2) 0.1768(15) 0.0669(13) 0.036(2) -0.110(2) C7E 0.1966(18) 0.372(3) 0.277(2) 0.032(2) -0.0082(16) 0.0724(19) C8E 0.494(3) 0.261(2) 0.1770(14) 0.0668(13) 0.0363(17) -0.110(2) C9E 0.363(3) 0.2791(19) 0.1257(11) 0.0703(11) -0.0077(15) -0.004(2) C10E 0.938(7) 0.261(2) 0.1768(16) 0.0674(15) 0.038(3) -0.111(3) C11E 0.3078(18) 0.1811(14) 0.1295(10) -0.0044(9) 0.0672(10) -0.0554(13) C12E 0.2694(14) 0.2459(16) 0.2423(14) 0.0708(12) 0.1254(10) 0.1496(12) C13E 0.377(2) 0.2609(18) 0.1768(13) 0.0672(12) 0.0369(14) -0.1103(17) C14E 0.500(3) 0.3362(17) 0.1820(14) 0.0750(12) -0.0189(16) -0.2727(15) C1F 0.2059(12) 0.1731(12) 0.1211(9) -0.0005(8) 0.0163(9) 0.0887(9) C2F 0.2209(11) 0.2249(12) 0.1556(8) 0.1024(8) 0.0952(8) 0.1199(10) C3F 0.2146(12) 0.1291(10) 0.1354(8) -0.0095(8) 0.0831(7) 0.0019(10) C4F 0.1586(11) 0.1438(11) 0.1051(8) -0.0071(8) -0.0220(8) -0.0340(9) C5F 0.0604(5) 0.1966(12) 0.0929(6) 0.0009(7) 0.0420(4) 0.0116(7) C6F 0.2076(13) 0.1967(14) 0.0928(7) 0.0008(8) 0.0420(8) 0.0118(12) C7F 0.461(4) 0.246(3) 0.366(3) -0.049(2) 0.014(3) -0.003(3) C8F 0.496(3) 0.1964(17) 0.0930(9) 0.0010(10) 0.0422(16) 0.011(2) C9F 0.306(2) 0.2259(15) 0.2627(16) 0.1155(11) 0.0438(15) -0.0569(15) C10F 0.313(2) 0.2426(17) 0.1883(12) 0.1052(10) -0.0316(14) 0.0056(17) C11F 0.1463(9) 0.2387(14) 0.0778(6) -0.0369(7) 0.0516(5) 0.0319(9) C12F 0.1863(11) 0.2223(13) 0.0401(6) -0.0249(7) -0.0334(7) 0.0717(10) C13F 0.376(3) 0.256(2) 0.1882(14) 0.0020(14) 0.0648(16) 0.066(2) C14F 0.1679(11) 0.1426(11) 0.1117(8) -0.0093(8) 0.0007(8) -0.0488(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.3858(4) . ? O2 C61 1.3847(4) . ? O3 C41 1.3631(3) . ? O4 C21 1.3787(3) . ? C1 C2 1.3682(4) . ? C1 C6 1.3992(4) . ? C2 C3 1.3988(4) . ? C2 C8 1.5196(4) . ? C3 C4 1.3866(4) . ? C5 C6 1.3872(4) . ? C5 C4 1.3903(4) . ? C6 C28 1.5110(4) . ? C8 C66 1.5237(4) . ? C21 C26 1.3911(4) . ? C21 C22 1.3942(4) . ? C22 C23 1.3802(4) . ? C22 C28 1.4885(4) . ? C23 C24 1.3958(4) . ? C25 C24 1.3663(4) . ? C25 C26 1.3884(4) . ? C26 C48 1.5422(4) . ? C41 C42 1.4012(4) . ? C41 C46 1.4067(4) . ? C42 C43 1.3861(3) . ? C42 C48 1.4996(4) . ? C43 C44 1.3863(4) . ? C45 C46 1.3912(3) . ? C45 C44 1.4082(4) . ? C46 C68 1.5224(4) . ? C61 C62 1.3872(4) . ? C61 C66 1.4178(4) . ? C62 C63 1.3830(4) . ? C62 C68 1.5098(4) . ? C63 C64 1.4045(4) . ? C65 C66 1.3640(4) . ? C65 C64 1.3786(4) . ? C4 C7A 1.5115(6) . ? C7A C11A 1.5317(9) . ? C7A C9A 1.5333(7) . ? C7A C10A 1.5458(8) . ? C24 C27A 1.5245(6) . ? C27A C30A 1.5333(10) . ? C27A C31A 1.5334(10) . ? C27A C29A 1.5400(9) . ? C44 C47A 1.5101(5) . ? C47A C49A 1.5201(8) . ? C47A C51A 1.5277(8) . ? C47A C50A 1.5400(8) . ? C64 C67A 1.5218(5) . ? C67A C69A 1.5382(6) . ? C67A C70A 1.5428(6) . ? C67A C71A 1.5453(6) . ? C7B C10B 1.5213(7) . ? C7B C11B 1.5273(8) . ? C7B C9B 1.5424(8) . ? C27B C30B 1.5314(7) . ? C27B C29B 1.5352(7) . ? C27B C31B 1.5496(8) . ? C47B C51B 1.5169(7) . ? C47B C49B 1.5329(8) . ? C47B C50B 1.5403(8) . ? C67B C71B 1.5371(10) . ? C67B C69B 1.5391(13) . ? C67B C70B 1.5421(11) . ? C1D C2D 1.5351(3) . ? C2D C3D 1.5334(3) . ? C3D C4D 1.5349(2) . ? C4D C5D 1.5347(3) . ? C5D C6D 1.5334(3) . ? C6D C7D 1.5334(3) . ? C7D C8D 1.5334(4) . ? C8D C9D 1.5346(3) . ? C9D C10D 1.5344(3) . ? C10D C11D 1.5336(3) . ? C11D C12D 1.5290(3) . ? C12D C13D 1.5329(3) . ? C13D C14D 1.5350(3) . ? C1E C2E 1.5110(12) . ? C2E C3E 1.5291(19) . ? C3E C4E 1.537(2) . ? C4E C5E 1.534(3) . ? C5E C6E 1.536(4) . ? C6E C7E 1.541(3) . ? C7E C8E 1.533(3) . ? C8E C9E 1.545(3) . ? C9E C10E 1.539(5) . ? C10E C11E 1.527(3) . ? C11E C12E 1.537(2) . ? C12E C13E 1.528(3) . ? C13E C14E 1.540(3) . ? C1F C2F 1.5290(18) . ? C2F C3F 1.534(2) . ? C3F C4F 1.5317(18) . ? C4F C5F 1.5294(16) . ? C5F C6F 1.5339(19) . ? C6F C7F 1.532(4) . ? C7F C8F 1.529(3) . ? C8F C9F 1.531(3) . ? C9F C10F 1.530(3) . ? C10F C11F 1.530(2) . ? C11F C12F 1.539(2) . ? C12F C13F 1.529(3) . ? C13F C14F 1.530(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 C2 C1 O1 119.587(19) . . ? C2 C1 C6 122.61(2) . . ? O1 C1 C6 117.74(2) . . ? C1 C2 C3 118.32(2) . . ? C1 C2 C8 122.64(2) . . ? C3 C2 C8 119.01(2) . . ? C4 C3 C2 122.40(2) . . ? C6 C5 C4 124.39(2) . . ? C5 C6 C1 116.14(2) . . ? C5 C6 C28 120.98(2) . . ? C1 C6 C28 122.80(2) . . ? C2 C8 C66 112.55(2) . . ? O4 C21 C26 117.68(2) . . ? O4 C21 C22 121.374(19) . . ? C26 C21 C22 120.90(2) . . ? C23 C22 C21 118.54(2) . . ? C23 C22 C28 119.57(2) . . ? C21 C22 C28 121.85(2) . . ? C22 C23 C24 121.79(2) . . ? C24 C25 C26 122.43(2) . . ? C25 C26 C21 118.30(2) . . ? C25 C26 C48 119.551(19) . . ? C21 C26 C48 122.09(2) . . ? C22 C28 C6 113.14(2) . . ? O3 C41 C42 119.93(2) . . ? O3 C41 C46 118.61(2) . . ? C42 C41 C46 121.38(2) . . ? C43 C42 C41 117.28(2) . . ? C43 C42 C48 120.51(2) . . ? C41 C42 C48 122.20(2) . . ? C42 C43 C44 124.53(2) . . ? C46 C45 C44 122.78(2) . . ? C45 C46 C41 118.06(2) . . ? C45 C46 C68 120.59(2) . . ? C41 C46 C68 121.31(2) . . ? C42 C48 C26 112.04(2) . . ? O2 C61 C62 119.57(2) . . ? O2 C61 C66 119.46(2) . . ? C62 C61 C66 120.90(2) . . ? C63 C62 C61 118.75(2) . . ? C63 C62 C68 119.82(2) . . ? C61 C62 C68 121.40(2) . . ? C62 C63 C64 122.17(2) . . ? C66 C65 C64 124.66(2) . . ? C65 C66 C61 117.16(2) . . ? C65 C66 C8 122.05(2) . . ? C61 C66 C8 120.64(2) . . ? C62 C68 C46 112.11(2) . . ? C3 C4 C5 116.14(2) . . ? C3 C4 C7A 125.27(3) . . ? C5 C4 C7A 118.59(3) . . ? C4 C7A C11A 111.95(4) . . ? C4 C7A C9A 111.96(4) . . ? C11A C7A C9A 105.85(5) . . ? C4 C7A C10A 108.03(4) . . ? C11A C7A C10A 108.06(5) . . ? C9A C7A C10A 110.94(4) . . ? C25 C24 C23 118.04(2) . . ? C25 C24 C27A 118.15(3) . . ? C23 C24 C27A 123.82(3) . . ? C24 C27A C30A 107.42(5) . . ? C24 C27A C31A 110.72(4) . . ? C30A C27A C31A 108.81(5) . . ? C24 C27A C29A 110.22(5) . . ? C30A C27A C29A 108.88(5) . . ? C31A C27A C29A 110.71(6) . . ? C43 C44 C45 115.95(2) . . ? C43 C44 C47A 127.14(3) . . ? C45 C44 C47A 116.89(3) . . ? C44 C47A C49A 111.16(4) . . ? C44 C47A C51A 107.14(4) . . ? C49A C47A C51A 112.69(5) . . ? C44 C47A C50A 107.46(4) . . ? C49A C47A C50A 111.08(4) . . ? C51A C47A C50A 107.03(4) . . ? C65 C64 C63 116.31(2) . . ? C65 C64 C67A 119.49(2) . . ? C63 C64 C67A 124.15(2) . . ? C64 C67A C69A 111.44(3) . . ? C64 C67A C70A 108.09(3) . . ? C69A C67A C70A 108.75(3) . . ? C64 C67A C71A 110.50(3) . . ? C69A C67A C71A 111.24(3) . . ? C70A C67A C71A 106.64(3) . . ? C10B C7B C11B 108.68(5) . . ? C10B C7B C9B 107.63(5) . . ? C11B C7B C9B 110.64(4) . . ? C30B C27B C29B 107.79(4) . . ? C30B C27B C31B 107.00(4) . . ? C29B C27B C31B 108.01(4) . . ? C51B C47B C49B 108.11(5) . . ? C51B C47B C50B 107.63(4) . . ? C49B C47B C50B 105.33(5) . . ? C71B C67B C69B 108.46(6) . . ? C71B C67B C70B 108.61(6) . . ? C69B C67B C70B 110.11(7) . . ? C3D C2D C1D 110.695(18) . . ? C2D C3D C4D 110.702(16) . . ? C5D C4D C3D 110.075(13) . . ? C6D C5D C4D 110.680(9) . . ? C7D C6D C5D 110.306(7) . . ? C6D C7D C8D 110.190(10) . . ? C7D C8D C9D 110.215(9) . . ? C10D C9D C8D 110.504(9) . . ? C11D C10D C9D 110.114(13) . . ? C12D C11D C10D 111.169(11) . . ? C11D C12D C13D 111.356(15) . . ? C12D C13D C14D 109.973(16) . . ? C1E C2E C3E 113.45(10) . . ? C2E C3E C4E 108.61(13) . . ? C5E C4E C3E 110.07(15) . . ? C4E C5E C6E 109.84(18) . . ? C5E C6E C7E 110.9(2) . . ? C8E C7E C6E 109.4(2) . . ? C7E C8E C9E 112.41(17) . . ? C10E C9E C8E 108.11(17) . . ? C11E C10E C9E 112.9(2) . . ? C10E C11E C12E 109.26(19) . . ? C13E C12E C11E 111.23(15) . . ? C12E C13E C14E 109.80(16) . . ? C1F C2F C3F 110.67(11) . . ? C4F C3F C2F 108.49(11) . . ? C5F C4F C3F 109.92(11) . . ? C4F C5F C6F 108.18(10) . . ? C7F C6F C5F 109.27(14) . . ? C8F C7F C6F 109.8(2) . . ? C7F C8F C9F 109.69(17) . . ? C10F C9F C8F 109.71(16) . . ? C9F C10F C11F 109.47(14) . . ? C10F C11F C12F 108.99(11) . . ? C13F C12F C11F 108.42(12) . . ? C14F C13F C12F 110.48(15) . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 22.30 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 0.295 _refine_diff_density_min -0.269 _refine_diff_density_rms 0.059 data_ku33 _database_code_CSD 158145 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _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 monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.5878(5) _cell_length_b 30.5003(17) _cell_length_c 13.5412(8) _cell_angle_alpha 90.00 _cell_angle_beta 109.8520(10) _cell_angle_gamma 90.00 _cell_volume 3724.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.157 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.072 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 43766 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 28.74 _reflns_number_total 9591 _reflns_number_gt 6368 _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 w==1/[\s^2^(Fo^2^)+(0.0607P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9591 _refine_ls_number_parameters 526 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0707 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1059 _refine_ls_wR_factor_gt 0.0984 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 0.185 _refine_ls_shift/su_mean 0.005 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.690560(4) 0.126030(1) 0.207630(3) 0.03175(1) Uani 1 d . . . O2 O 0.711870(3) 0.196250(1) 0.096290(3) 0.03227(1) Uani 1 d . . . O3 O 0.573570(4) 0.151550(1) -0.076130(3) 0.03143(1) Uani 1 d . . . O4 O 0.558070(3) 0.083280(1) 0.032300(2) 0.02855(1) Uani 1 d . . . H110 H 0.69887(10) 0.15389(3) 0.18383(7) 0.0505(3) Uiso 0.65 d P . . H120 H 0.65104(11) 0.18710(3) 0.02952(8) 0.0640(3) Uiso 0.65 d P . . H130 H 0.56707(9) 0.12554(3) -0.04544(6) 0.0442(2) Uiso 0.65 d P . . H140 H 0.59832(11) 0.09311(3) 0.10051(8) 0.0604(3) Uiso 0.65 d P . . H210 H 0.6552(2) 0.11724(6) 0.13411(14) 0.0650(6) Uiso 0.35 d P . . H220 H 0.7066(2) 0.16810(6) 0.12690(14) 0.0663(6) Uiso 0.35 d P . . H230 H 0.61688(19) 0.17120(6) -0.02129(13) 0.0569(5) Uiso 0.35 d P . . H240 H 0.5479(2) 0.10843(6) -0.01196(14) 0.0641(6) Uiso 0.35 d P . . C1 C 0.855940(5) 0.204990(2) 0.100880(4) 0.02674(1) Uani 1 d . . . C2 C 0.968980(5) 0.202170(2) 0.198140(4) 0.02790(1) Uani 1 d . . . C3 C 1.112260(5) 0.213010(2) 0.203430(4) 0.03127(2) Uani 1 d . . . H3 H 1.1895 0.2117 0.2696 0.038 Uiso 1 calc R . . C4 C 1.147350(5) 0.225780(2) 0.115550(4) 0.03106(2) Uani 1 d . . . C5 C 1.030490(5) 0.227110(2) 0.020020(4) 0.02988(1) Uani 1 d . . . H5 H 1.0513 0.2350 -0.0414 0.036 Uiso 1 calc R . . C6 C 0.884320(5) 0.217400(2) 0.010710(4) 0.02754(1) Uani 1 d . . . C7 C 0.760790(5) 0.220590(2) -0.095610(4) 0.02968(1) Uani 1 d . . . H7A H 0.6671 0.2282 -0.0841 0.036 Uiso 1 calc R . . H7B H 0.7843 0.2447 -0.1363 0.036 Uiso 1 calc R . . C8 C 1.306450(8) 0.238590(3) 0.120800(7) 0.03775(2) Uani 0.6921(1) d P A -1 C9 C 1.426090(9) 0.219890(4) 0.218800(7) 0.05224(3) Uani 0.6921(1) d P A -1 H9A H 1.4161 0.2332 0.2819 0.078 Uiso 0.6921(1) calc PR A -1 H9B H 1.5245 0.2265 0.2156 0.078 Uiso 0.6921(1) calc PR A -1 H9C H 1.4138 0.1881 0.2213 0.078 Uiso 0.6921(1) calc PR A -1 C10 C 1.316430(10) 0.289470(3) 0.125390(11) 0.07748(5) Uani 0.6921(1) d P A -1 H10A H 1.2429 0.3018 0.0623 0.116 Uiso 0.6921(1) calc PR A -1 H10B H 1.4160 0.2987 0.1290 0.116 Uiso 0.6921(1) calc PR A -1 H10C H 1.2967 0.3000 0.1878 0.116 Uiso 0.6921(1) calc PR A -1 C11 C 1.339940(9) 0.222320(4) 0.023320(7) 0.05826(3) Uani 0.6921(1) d P A -1 H11A H 1.3317 0.1903 0.0192 0.087 Uiso 0.6921(1) calc PR A -1 H11B H 1.4407 0.2311 0.0289 0.087 Uiso 0.6921(1) calc PR A -1 H11C H 1.2687 0.2353 -0.0400 0.087 Uiso 0.6921(1) calc PR A -1 C8A C 1.303660(18) 0.241440(6) 0.131060(15) 0.03775(2) Uani 0.3079(1) d P A -2 C9A C 1.41412(2) 0.207990(8) 0.195230(17) 0.05224(3) Uani 0.3079(1) d P A -2 H9A1 H 1.5151 0.2189 0.2090 0.078 Uiso 0.3079(1) calc PR A -2 H9A2 H 1.4010 0.1803 0.1562 0.078 Uiso 0.3079(1) calc PR A -2 H9A3 H 1.3978 0.2031 0.2620 0.078 Uiso 0.3079(1) calc PR A -2 C10A C 1.33887(2) 0.283650(7) 0.19299(2) 0.07748(5) Uani 0.3079(1) d P A -2 H10D H 1.3276 0.2792 0.2616 0.116 Uiso 0.3079(1) calc PR A -2 H10E H 1.2707 0.3067 0.1546 0.116 Uiso 0.3079(1) calc PR A -2 H10F H 1.4411 0.2924 0.2030 0.116 Uiso 0.3079(1) calc PR A -2 C11A C 1.33095(2) 0.245520(8) 0.028921(17) 0.05826(3) Uani 0.3079(1) d P A -2 H11D H 1.4367 0.2508 0.0426 0.087 Uiso 0.3079(1) calc PR A -2 H11E H 1.2730 0.2701 -0.0113 0.087 Uiso 0.3079(1) calc PR A -2 H11F H 1.3011 0.2183 -0.0113 0.087 Uiso 0.3079(1) calc PR A -2 C12 C 0.651740(5) 0.144240(2) -0.143550(3) 0.02601(1) Uani 1 d . . . C13 C 0.737510(5) 0.178750(2) -0.159990(4) 0.02750(1) Uani 1 d . . . C14 C 0.801070(5) 0.173870(2) -0.237160(4) 0.03146(1) Uani 1 d . . . H14 H 0.8566 0.1975 -0.2505 0.038 Uiso 1 calc R . . C15 C 0.786760(5) 0.135530(2) -0.296100(4) 0.03059(1) Uani 1 d . . . C16 C 0.709380(5) 0.100940(2) -0.271370(4) 0.02809(1) Uani 1 d . . . H16 H 0.7033 0.0739 -0.3074 0.034 Uiso 1 calc R . . C17 C 0.640320(5) 0.104340(2) -0.195860(3) 0.02556(1) Uani 1 d . . . C18 C 0.550360(5) 0.065920(2) -0.176520(3) 0.02634(1) Uani 1 d . . . H18A H 0.4603 0.0779 -0.1663 0.032 Uiso 1 calc R . . H18B H 0.5175 0.0476 -0.2407 0.032 Uiso 1 calc R . . C19 C 0.845990(6) 0.133750(2) -0.388230(4) 0.03905(2) Uani 0.9224(1) d P B -1 C20 C 1.004550(7) 0.151480(3) -0.354620(6) 0.06948(3) Uani 0.9224(1) d P B -1 H20A H 1.0690 0.1335 -0.2973 0.104 Uiso 0.9224(1) calc PR B -1 H20B H 1.0060 0.1819 -0.3307 0.104 Uiso 0.9224(1) calc PR B -1 H20C H 1.0402 0.1505 -0.4144 0.104 Uiso 0.9224(1) calc PR B -1 C21 C 0.747350(9) 0.163980(3) -0.476000(5) 0.06009(3) Uani 0.9224(1) d P B -1 H21A H 0.7833 0.1637 -0.5356 0.090 Uiso 0.9224(1) calc PR B -1 H21B H 0.7515 0.1940 -0.4491 0.090 Uiso 0.9224(1) calc PR B -1 H21C H 0.6447 0.1534 -0.4989 0.090 Uiso 0.9224(1) calc PR B -1 C22 C 0.842040(8) 0.088050(2) -0.432870(5) 0.05049(2) Uani 0.9224(1) d P B -1 H22A H 0.9014 0.0682 -0.3776 0.076 Uiso 0.9224(1) calc PR B -1 H22B H 0.8828 0.0887 -0.4901 0.076 Uiso 0.9224(1) calc PR B -1 H22C H 0.7393 0.0776 -0.4598 0.076 Uiso 0.9224(1) calc PR B -1 C19A C 0.87022(8) 0.13262(2) -0.37591(5) 0.03905(2) Uani 0.0776(1) d P B -2 C20A C 1.03345(9) 0.11891(4) -0.33002(7) 0.06948(3) Uani 0.0776(1) d P B -2 H20D H 1.0397 0.0874 -0.3151 0.104 Uiso 0.0776(1) calc PR B -2 H20E H 1.0819 0.1352 -0.2649 0.104 Uiso 0.0776(1) calc PR B -2 H20F H 1.0832 0.1254 -0.3807 0.104 Uiso 0.0776(1) calc PR B -2 C21A C 0.85922(11) 0.17603(3) -0.43425(6) 0.06009(3) Uani 0.0776(1) d P B -2 H21D H 0.9381 0.1958 -0.3929 0.090 Uiso 0.0776(1) calc PR B -2 H21E H 0.7625 0.1895 -0.4446 0.090 Uiso 0.0776(1) calc PR B -2 H21F H 0.8701 0.1707 -0.5026 0.090 Uiso 0.0776(1) calc PR B -2 C22A C 0.76405(9) 0.10582(3) -0.46815(6) 0.05049(2) Uani 0.0776(1) d P B -2 H22D H 0.8135 0.0991 -0.5189 0.076 Uiso 0.0776(1) calc PR B -2 H22E H 0.6742 0.1230 -0.5027 0.076 Uiso 0.0776(1) calc PR B -2 H22F H 0.7372 0.0784 -0.4412 0.076 Uiso 0.0776(1) calc PR B -2 C23 C 0.633050(5) 0.046380(2) 0.017980(3) 0.02304(1) Uani 1 d . . . C24 C 0.628980(5) 0.036200(2) -0.083290(3) 0.02362(1) Uani 1 d . . . C25 C 0.695710(5) -0.002700(2) -0.097220(3) 0.02617(1) Uani 1 d . . . H25 H 0.6932 -0.0102 -0.1659 0.031 Uiso 1 calc R . . C26 C 0.766410(5) -0.031360(2) -0.014700(4) 0.02581(1) Uani 1 d . . . C27 C 0.771300(5) -0.018620(2) 0.085280(4) 0.02594(1) Uani 1 d . . . H27 H 0.8209 -0.0370 0.1432 0.031 Uiso 1 calc R . . C28 C 0.706530(5) 0.019920(2) 0.103740(3) 0.02373(1) Uani 1 d . . . C29 C 0.716720(5) 0.032340(2) 0.214930(3) 0.02672(1) Uani 1 d . . . H29A H 0.7278 0.0052 0.2571 0.032 Uiso 1 calc R . . H29B H 0.6225 0.0465 0.2123 0.032 Uiso 1 calc R . . C30 C 0.837080(7) -0.073350(2) -0.038230(5) 0.02838(2) Uani 0.7803(1) d P C -1 C31 C 0.968040(8) -0.061720(3) -0.073450(7) 0.05108(2) Uani 0.7803(1) d P C -1 H31A H 1.0112 -0.0886 -0.0901 0.077 Uiso 0.7803(1) calc PR C -1 H31B H 1.0432 -0.0460 -0.0169 0.077 Uiso 0.7803(1) calc PR C -1 H31C H 0.9337 -0.0430 -0.1359 0.077 Uiso 0.7803(1) calc PR C -1 C32 C 0.725930(8) -0.099880(2) -0.126070(6) 0.03895(2) Uani 0.7803(1) d P C -1 H32A H 0.7752 -0.1258 -0.1414 0.058 Uiso 0.7803(1) calc PR C -1 H32B H 0.6881 -0.0817 -0.1893 0.058 Uiso 0.7803(1) calc PR C -1 H32C H 0.6433 -0.1091 -0.1037 0.058 Uiso 0.7803(1) calc PR C -1 C33 C 0.891220(10) -0.102680(3) 0.059220(6) 0.05426(3) Uani 0.7803(1) d P C -1 H33A H 0.8092 -0.1083 0.0853 0.081 Uiso 0.7803(1) calc PR C -1 H33B H 0.9721 -0.0880 0.1139 0.081 Uiso 0.7803(1) calc PR C -1 H33C H 0.9270 -0.1306 0.0408 0.081 Uiso 0.7803(1) calc PR C -1 C30A C 0.84278(2) -0.076480(7) -0.018039(17) 0.02838(2) Uani 0.2197(1) d P C -2 C31A C 1.01126(3) -0.069270(10) 0.01771(2) 0.05108(2) Uani 0.2197(1) d P C -2 H31D H 1.0326 -0.0431 -0.0168 0.077 Uiso 0.2197(1) calc PR C -2 H31E H 1.0585 -0.0949 -0.0013 0.077 Uiso 0.2197(1) calc PR C -2 H31F H 1.0502 -0.0652 0.0940 0.077 Uiso 0.2197(1) calc PR C -2 C32A C 0.79870(3) -0.090080(8) -0.13536(2) 0.03895(2) Uani 0.2197(1) d P C -2 H32D H 0.6904 -0.0917 -0.1664 0.058 Uiso 0.2197(1) calc PR C -2 H32E H 0.8417 -0.1188 -0.1403 0.058 Uiso 0.2197(1) calc PR C -2 H32F H 0.8362 -0.0683 -0.1733 0.058 Uiso 0.2197(1) calc PR C -2 C33A C 0.80460(3) -0.112820(9) 0.04340(2) 0.05426(3) Uani 0.2197(1) d P C -2 H33D H 0.8381 -0.1050 0.1180 0.081 Uiso 0.2197(1) calc PR C -2 H33E H 0.8538 -0.1399 0.0342 0.081 Uiso 0.2197(1) calc PR C -2 H33F H 0.6970 -0.1173 0.0180 0.081 Uiso 0.2197(1) calc PR C -2 C34 C 0.829590(5) 0.108670(2) 0.261790(3) 0.02514(1) Uani 1 d . . . C35 C 0.844550(5) 0.063180(2) 0.270340(3) 0.02485(1) Uani 1 d . . . C36 C 0.981620(5) 0.046460(2) 0.330630(3) 0.02693(1) Uani 1 d . . . H36 H 0.9931 0.0156 0.3379 0.032 Uiso 1 calc R . . C37 C 1.103860(5) 0.073210(2) 0.381220(3) 0.02681(1) Uani 1 d . . . C38 C 1.084270(5) 0.118090(2) 0.367020(3) 0.02753(1) Uani 1 d . . . H38 H 1.1662 0.1369 0.3990 0.033 Uiso 1 calc R . . C39 C 0.948870(5) 0.136640(2) 0.307600(3) 0.02630(1) Uani 1 d . . . C40 C 0.936790(6) 0.185960(2) 0.294300(4) 0.03025(1) Uani 1 d . . . H40A H 1.0072 0.2000 0.3576 0.036 Uiso 1 calc R . . H40B H 0.8354 0.1952 0.2889 0.036 Uiso 1 calc R . . C41 C 1.251120(5) 0.053000(2) 0.449910(4) 0.03140(1) Uani 1 d . . . C42 C 1.310180(6) 0.022480(2) 0.382880(4) 0.03972(2) Uani 1 d . . . H42A H 1.2325 0.0017 0.3451 0.060 Uiso 1 calc R . . H42B H 1.3964 0.0063 0.4285 0.060 Uiso 1 calc R . . H42C H 1.3393 0.0399 0.3323 0.060 Uiso 1 calc R . . C43 C 1.225980(6) 0.026490(2) 0.538750(4) 0.04251(2) Uani 1 d . . . H43A H 1.1928 0.0462 0.5836 0.064 Uiso 1 calc R . . H43B H 1.3189 0.0123 0.5807 0.064 Uiso 1 calc R . . H43C H 1.1501 0.0041 0.5087 0.064 Uiso 1 calc R . . C44 C 1.369460(7) 0.087650(2) 0.499220(5) 0.04906(2) Uani 1 d . . . H44A H 1.3863 0.1052 0.4437 0.074 Uiso 1 calc R . . H44B H 1.4621 0.0732 0.5408 0.074 Uiso 1 calc R . . H44C H 1.3359 0.1068 0.5448 0.074 Uiso 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 0.02609(1) 0.03406(2) 0.03382(2) -0.00349(1) 0.00850(1) 0.00543(1) O2 0.02375(1) 0.03255(2) 0.04005(2) -0.00129(1) 0.01025(1) 0.00219(1) O3 0.03129(2) 0.03021(2) 0.03475(2) 0.00092(1) 0.01378(1) -0.00048(1) O4 0.02663(1) 0.02845(2) 0.03217(1) -0.00084(1) 0.01205(1) 0.00056(1) C1 0.02403(2) 0.01995(2) 0.03504(2) -0.00263(2) 0.00846(2) 0.00225(2) C2 0.03070(2) 0.01920(2) 0.03216(2) -0.00388(2) 0.00854(2) 0.00226(2) C3 0.02835(2) 0.02382(2) 0.03544(2) -0.00246(2) 0.00277(2) 0.00139(2) C4 0.02497(2) 0.02187(2) 0.04387(2) -0.00081(2) 0.00846(2) 0.00121(2) C5 0.03057(2) 0.02202(2) 0.03735(2) 0.00123(2) 0.01191(2) 0.00043(2) C6 0.02782(2) 0.01788(2) 0.03348(2) -0.00104(2) 0.00594(2) 0.00131(2) C7 0.02941(2) 0.02323(2) 0.03325(2) 0.00461(2) 0.00654(2) -0.00176(2) C8 0.02531(2) 0.03164(3) 0.05524(3) 0.00006(2) 0.01230(2) 0.00040(2) C9 0.02444(3) 0.07162(6) 0.05144(4) -0.00521(4) 0.00089(3) -0.00569(3) C10 0.03909(3) 0.03352(4) 0.16497(11) 0.00938(6) 0.04136(5) -0.00407(3) C11 0.03060(3) 0.08719(9) 0.05856(4) 0.00233(5) 0.01717(3) 0.00580(5) C8A 0.02531(2) 0.03164(3) 0.05524(3) 0.00006(2) 0.01230(2) 0.00040(2) C9A 0.02444(3) 0.07162(6) 0.05144(4) -0.00521(4) 0.00089(3) -0.00569(3) C10A 0.03909(3) 0.03352(4) 0.16497(11) 0.00938(6) 0.04136(5) -0.00407(3) C11A 0.03060(3) 0.08719(9) 0.05856(4) 0.00233(5) 0.01717(3) 0.00580(5) C12 0.02256(2) 0.02874(2) 0.02468(2) 0.00376(2) 0.00536(2) -0.00008(2) C13 0.02467(2) 0.02629(2) 0.02751(2) 0.00481(2) 0.00360(2) -0.00156(2) C14 0.02986(2) 0.03086(2) 0.03179(2) 0.00519(2) 0.00805(2) -0.00808(2) C15 0.02871(2) 0.03591(3) 0.02721(2) 0.00349(2) 0.00956(2) -0.00493(2) C16 0.02825(2) 0.02937(2) 0.02493(2) 0.00145(2) 0.00679(2) -0.00399(2) C17 0.02279(2) 0.02787(2) 0.02293(2) 0.00371(2) 0.00374(2) -0.00324(2) C18 0.02506(2) 0.02827(2) 0.02400(2) 0.00015(2) 0.00611(2) -0.00630(2) C19 0.04361(3) 0.04250(3) 0.03597(2) -0.00024(2) 0.01993(2) -0.01195(2) C20 0.06082(3) 0.09492(6) 0.06879(3) -0.01721(4) 0.04298(2) -0.03514(4) C21 0.08805(5) 0.05956(4) 0.03839(3) 0.00917(3) 0.02894(3) -0.00590(4) C22 0.06798(3) 0.04392(4) 0.05702(3) -0.00225(3) 0.04397(2) -0.00503(3) C19A 0.04361(3) 0.04250(3) 0.03597(2) -0.00024(2) 0.01993(2) -0.01195(2) C20A 0.06082(3) 0.09492(6) 0.06879(3) -0.01721(4) 0.04298(2) -0.03514(4) C21A 0.08805(5) 0.05956(4) 0.03839(3) 0.00917(3) 0.02894(3) -0.00590(4) C22A 0.06798(3) 0.04392(4) 0.05702(3) -0.00225(3) 0.04397(2) -0.00503(3) C23 0.01933(2) 0.02308(2) 0.02800(2) -0.00158(2) 0.00970(1) -0.00463(2) C24 0.01992(2) 0.02685(2) 0.02378(2) -0.00009(2) 0.00701(1) -0.00753(2) C25 0.02550(2) 0.02884(2) 0.02591(2) -0.00452(2) 0.01099(1) -0.00739(2) C26 0.02171(2) 0.02563(2) 0.03115(2) -0.00299(2) 0.01035(2) -0.00595(2) C27 0.02278(2) 0.02600(2) 0.02761(2) 0.00170(2) 0.00669(2) -0.00415(2) C28 0.02134(2) 0.02634(2) 0.02409(2) -0.00098(2) 0.00846(1) -0.00710(2) C29 0.02756(2) 0.02977(2) 0.02395(2) 0.00091(2) 0.01022(2) -0.00345(2) C30 0.02679(2) 0.02721(2) 0.03277(2) -0.00083(2) 0.01222(2) -0.00180(2) C31 0.03822(3) 0.04570(4) 0.07987(4) -0.01922(4) 0.03379(3) -0.00870(3) C32 0.03469(3) 0.02827(3) 0.05153(3) -0.01044(3) 0.01155(3) -0.00252(3) C33 0.07126(5) 0.04177(4) 0.04707(3) 0.00408(3) 0.01659(4) 0.02483(4) C30A 0.02679(2) 0.02721(2) 0.03277(2) -0.00083(2) 0.01222(2) -0.00180(2) C31A 0.03822(3) 0.04570(4) 0.07987(4) -0.01922(4) 0.03379(3) -0.00870(3) C32A 0.03469(3) 0.02827(3) 0.05153(3) -0.01044(3) 0.01155(3) -0.00252(3) C33A 0.07126(5) 0.04177(4) 0.04707(3) 0.00408(3) 0.01659(4) 0.02483(4) C34 0.02467(2) 0.02992(2) 0.02217(2) -0.00225(2) 0.00968(1) 0.00281(2) C35 0.02736(2) 0.02888(2) 0.01983(2) -0.00248(2) 0.00999(1) -0.00209(2) C36 0.03119(2) 0.02729(2) 0.02297(2) 0.00026(2) 0.01006(2) 0.00017(2) C37 0.02720(2) 0.03299(2) 0.01989(2) -0.00002(2) 0.00753(2) 0.00014(2) C38 0.02767(2) 0.03177(2) 0.02244(2) -0.00419(2) 0.00757(2) -0.00383(2) C39 0.03043(2) 0.02715(2) 0.02267(2) -0.00507(2) 0.01079(2) -0.00026(2) C40 0.03281(2) 0.02767(2) 0.02815(2) -0.00759(2) 0.00757(2) 0.00078(2) C41 0.02851(2) 0.03778(3) 0.02454(2) 0.00197(2) 0.00463(2) 0.00242(2) C42 0.03531(2) 0.05115(3) 0.03159(2) 0.00394(2) 0.00993(2) 0.01119(2) C43 0.04315(3) 0.05461(3) 0.02871(2) 0.00978(2) 0.01082(2) 0.00946(3) C44 0.03322(3) 0.05027(3) 0.04878(3) -0.00001(3) -0.00551(3) -0.00079(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C34 1.3896 . ? O2 C1 1.3873 . ? O3 C12 1.3819 . ? O4 C23 1.3841 . ? C1 C6 1.39062(11) . ? C1 C2 1.3954 . ? C2 C3 1.39096(11) . ? C2 C40 1.51926(11) . ? C3 C4 1.39746(10) . ? C4 C5 1.3950 . ? C4 C8A 1.5181(2) . ? C4 C8 1.55273(12) . ? C5 C6 1.39559(11) . ? C6 C7 1.5254 . ? C7 C13 1.5186 . ? C8 C9 1.53892(12) . ? C8 C11 1.54260(16) . ? C8 C10 1.55475(15) . ? C8A C11A 1.4975(3) . ? C8A C10A 1.5108(3) . ? C8A C9A 1.5141(3) . ? C12 C17 1.3936 . ? C12 C13 1.3993 . ? C13 C14 1.3849 . ? C14 C15 1.3960 . ? C15 C16 1.3944 . ? C15 C19 1.53721(12) . ? C15 C19A 1.5504(8) . ? C16 C17 1.3980 . ? C17 C18 1.5294 . ? C18 C24 1.5288 . ? C19 C22 1.51464(12) . ? C19 C20 1.52996(12) . ? C19 C21 1.54716(10) . ? C19A C21A 1.5269(12) . ? C19A C20A 1.5329(11) . ? C19A C22A 1.5495(9) . ? C23 C28 1.3930 . ? C23 C24 1.39359(10) . ? C24 C25 1.3909 . ? C25 C26 1.3992 . ? C26 C27 1.39391(10) . ? C26 C30 1.53214(10) . ? C26 C30A 1.5667(2) . ? C27 C28 1.3912 . ? C28 C29 1.52319(11) . ? C29 C35 1.5249 . ? C30 C31 1.52859(14) . ? C30 C32 1.5311 . ? C30 C33 1.53160(12) . ? C30A C33A 1.5038(4) . ? C30A C31A 1.5365(3) . ? C30A C32A 1.5552(3) . ? C34 C39 1.3923 . ? C34 C35 1.39561(10) . ? C35 C36 1.3874 . ? C36 C37 1.4012 . ? C37 C38 1.38617(10) . ? C37 C41 1.5319 . ? C38 C39 1.3940 . ? C39 C40 1.51477(11) . ? C41 C44 1.5283 . ? C41 C43 1.53493(10) . ? C41 C42 1.5363 . ? 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 O2 C1 C6 120.112(4) . . ? O2 C1 C2 118.219(6) . . ? C6 C1 C2 121.644(6) . . ? C3 C2 C1 118.093(6) . . ? C3 C2 C40 121.181(4) . . ? C1 C2 C40 120.681(6) . . ? C2 C3 C4 122.789(4) . . ? C5 C4 C3 116.612(6) . . ? C5 C4 C8A 124.295(9) . . ? C3 C4 C8A 118.798(8) . . ? C5 C4 C8 120.155(6) . . ? C3 C4 C8 123.230(5) . . ? C8A C4 C8 6.347(8) . . ? C4 C5 C6 122.907(6) . . ? C1 C6 C5 117.928(4) . . ? C1 C6 C7 121.691(6) . . ? C5 C6 C7 120.381(5) . . ? C13 C7 C6 113.820(5) . . ? C9 C8 C11 107.930(8) . . ? C9 C8 C4 112.285(8) . . ? C11 C8 C4 111.507(6) . . ? C9 C8 C10 108.525(7) . . ? C11 C8 C10 109.113(9) . . ? C4 C8 C10 107.407(7) . . ? C11A C8A C10A 111.45(2) . . ? C11A C8A C9A 106.170(18) . . ? C10A C8A C9A 105.947(15) . . ? C11A C8A C4 111.856(13) . . ? C10A C8A C4 111.649(16) . . ? C9A C8A C4 109.430(15) . . ? O3 C12 C17 120.669(5) . . ? O3 C12 C13 117.621(5) . . ? C17 C12 C13 121.668(6) . . ? C14 C13 C12 118.174(5) . . ? C14 C13 C7 120.458(5) . . ? C12 C13 C7 121.367(6) . . ? C13 C14 C15 122.575(5) . . ? C16 C15 C14 116.967(6) . . ? C16 C15 C19 122.786(5) . . ? C14 C15 C19 120.125(5) . . ? C16 C15 C19A 124.53(3) . . ? C14 C15 C19A 118.21(3) . . ? C19 C15 C19A 8.83(2) . . ? C15 C16 C17 122.840(5) . . ? C12 C17 C16 117.487(5) . . ? C12 C17 C18 122.248(6) . . ? C16 C17 C18 120.206(5) . . ? C24 C18 C17 116.558(5) . . ? C22 C19 C20 109.368(6) . . ? C22 C19 C15 112.975(6) . . ? C20 C19 C15 110.470(5) . . ? C22 C19 C21 108.417(6) . . ? C20 C19 C21 107.716(7) . . ? C15 C19 C21 107.727(6) . . ? C21A C19A C20A 109.15(7) . . ? C21A C19A C22A 97.43(5) . . ? C20A C19A C22A 118.93(7) . . ? C21A C19A C15 110.47(6) . . ? C20A C19A C15 115.51(5) . . ? C22A C19A C15 103.82(6) . . ? O4 C23 C28 119.603(5) . . ? O4 C23 C24 118.471(4) . . ? C28 C23 C24 121.902(5) . . ? C25 C24 C23 117.584(4) . . ? C25 C24 C18 120.951(5) . . ? C23 C24 C18 121.443(5) . . ? C24 C25 C26 123.026(5) . . ? C27 C26 C25 116.672(6) . . ? C27 C26 C30 124.306(4) . . ? C25 C26 C30 118.990(6) . . ? C27 C26 C30A 114.268(9) . . ? C25 C26 C30A 129.060(9) . . ? C30 C26 C30A 10.175(9) . . ? C28 C27 C26 122.700(4) . . ? C27 C28 C23 118.032(5) . . ? C27 C28 C29 120.335(4) . . ? C23 C28 C29 121.633(5) . . ? C28 C29 C35 114.257(5) . . ? C31 C30 C32 108.000(7) . . ? C31 C30 C33 109.292(6) . . ? C32 C30 C33 107.667(7) . . ? C31 C30 C26 109.818(6) . . ? C32 C30 C26 111.286(5) . . ? C33 C30 C26 110.700(7) . . ? C33A C30A C31A 111.01(2) . . ? C33A C30A C32A 109.62(2) . . ? C31A C30A C32A 104.59(2) . . ? C33A C30A C26 115.31(2) . . ? C31A C30A C26 108.471(17) . . ? C32A C30A C26 107.231(15) . . ? O1 C34 C39 119.816(5) . . ? O1 C34 C35 118.406(4) . . ? C39 C34 C35 121.765(5) . . ? C36 C35 C34 117.668(4) . . ? C36 C35 C29 120.347(5) . . ? C34 C35 C29 121.981(4) . . ? C35 C36 C37 122.789(6) . . ? C38 C37 C36 117.113(5) . . ? C38 C37 C41 122.352(4) . . ? C36 C37 C41 120.531(6) . . ? C37 C38 C39 122.453(4) . . ? C34 C39 C38 118.131(5) . . ? C34 C39 C40 122.508(5) . . ? C38 C39 C40 119.359(4) . . ? C39 C40 C2 113.296(4) . . ? C44 C41 C37 112.425(6) . . ? C44 C41 C43 108.224(5) . . ? C37 C41 C43 109.280(5) . . ? C44 C41 C42 108.013(6) . . ? C37 C41 C42 109.495(5) . . ? C43 C41 C42 109.351(6) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 28.74 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.225 _refine_diff_density_min -0.243 _refine_diff_density_rms 0.037