# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2009 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'George Gokel' _publ_contact_author_email GOKELG@UMSL.EDU _publ_section_title ; Guest Molecule Entrapment by both Capsule and Hydrocarbon-sidechains in Self-assembled Pyrogallol[4]arenes ; loop_ _publ_author_name 'George Gokel' 'Oleg Kulikov' 'Nigam P. Rath' 'Dan Zhou.' # Attachment 'g10808.cif' data_g10808 _database_code_depnum_ccdc_archive 'CCDC 701456' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H102 O17' _chemical_formula_weight 1143.46 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 Rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'z, x, y' 'y, z, x' '-x, -y, -z' '-z, -x, -y' '-y, -z, -x' _cell_length_a 21.5048(9) _cell_length_b 21.5048(9) _cell_length_c 21.5048(9) _cell_angle_alpha 91.042(11) _cell_angle_beta 91.042(11) _cell_angle_gamma 91.042(11) _cell_volume 9940.0(7) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9936 _cell_measurement_theta_min 2.10 _cell_measurement_theta_max 24.89 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas no _exptl_crystal_density_diffrn 1.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3732 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9665 _exptl_absorpt_correction_T_max 0.9783 _exptl_absorpt_process_details 'sadabs v2008/1' _exptl_special_details ; All H atoms were added in their calculated positions and were treated using appropriate riding models. Solvent water H were not included in refinement. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 98900 _diffrn_reflns_av_R_equivalents 0.2336 _diffrn_reflns_av_sigmaI/netI 0.2896 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11656 _reflns_number_gt 3244 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Apex II (Bruker, 2006)' _computing_cell_refinement 'Bruker-Apex II (Bruker, 2006)' _computing_data_reduction 'Bruker-SAINT (Bruker, 2006)' _computing_structure_solution 'Bruker-SHELXTL (Sheldrick, G.M., 2008)' _computing_structure_refinement 'Bruker-SHELXTL (Sheldrick, G.M., 2008)' _computing_molecular_graphics 'Bruker-SHELXTL (Sheldrick, G.M., 2008)' _computing_publication_material 'Bruker-SHELXTL (Sheldrick, G.M., 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0067(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11656 _refine_ls_number_parameters 758 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.4117 _refine_ls_R_factor_gt 0.1649 _refine_ls_wR_factor_ref 0.5605 _refine_ls_wR_factor_gt 0.4189 _refine_ls_goodness_of_fit_ref 1.458 _refine_ls_restrained_S_all 1.459 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.003 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 0.8485(4) 0.3993(5) 0.4003(4) 0.080(3) Uani 1 1 d . . . H1 H 0.8444 0.4226 0.3697 0.119 Uiso 1 1 calc R . . O2 O 0.8258(5) 0.5228(5) 0.4032(4) 0.106(4) Uani 1 1 d . . . H2 H 0.8021 0.5501 0.4171 0.160 Uiso 1 1 calc R . . O3 O 0.8673(4) 0.5980(4) 0.5014(5) 0.091(3) Uani 1 1 d . . . H3 H 0.8291 0.6029 0.4943 0.136 Uiso 1 1 calc R . . O4 O 0.8361(4) 0.6430(4) 0.6118(5) 0.082(3) Uani 1 1 d . . . H4 H 0.8725 0.6563 0.6063 0.123 Uiso 1 1 calc R . . O5 O 0.7445(4) 0.6428(4) 0.6979(6) 0.103(4) Uani 1 1 d . . . H5 H 0.7542 0.6720 0.7228 0.154 Uiso 1 1 calc R . . O6 O 0.7387(4) 0.5554(4) 0.7867(5) 0.085(3) Uani 1 1 d . . . H6 H 0.7263 0.5921 0.7899 0.127 Uiso 1 1 calc R . . O7 O 0.6971(4) 0.4448(4) 0.8199(4) 0.074(3) Uani 1 1 d . . . H7 H 0.6599 0.4467 0.8076 0.111 Uiso 1 1 calc R . . O8 O 0.6281(4) 0.3455(5) 0.7749(5) 0.099(3) Uani 1 1 d . . . H8 H 0.6209 0.3414 0.8128 0.148 Uiso 1 1 calc R . . O9 O 0.6807(4) 0.2498(4) 0.7167(4) 0.076(3) Uani 1 1 d . . . H9 H 0.7009 0.2238 0.6960 0.115 Uiso 1 1 calc R . . O10 O 0.7153(4) 0.2019(4) 0.6072(4) 0.066(2) Uani 1 1 d . . . H10 H 0.6868 0.1977 0.5801 0.100 Uiso 1 1 calc R . . O11 O 0.7169(5) 0.2197(5) 0.4810(5) 0.096(3) Uani 1 1 d . . . H11 H 0.6829 0.2275 0.4978 0.145 Uiso 1 1 calc R . . O12 O 0.8114(5) 0.2838(5) 0.4275(4) 0.091(3) Uani 1 1 d . . . H12 H 0.8476 0.2882 0.4142 0.136 Uiso 1 1 calc R . . C1 C 0.9023(5) 0.4067(6) 0.5000(5) 0.047(3) Uani 1 1 d . . . C2 C 0.8695(5) 0.4346(7) 0.4523(6) 0.058(3) Uani 1 1 d . . . C3 C 0.8590(6) 0.4960(8) 0.4530(7) 0.067(4) Uani 1 1 d . . . C4 C 0.8796(6) 0.5351(7) 0.5031(7) 0.065(4) Uani 1 1 d . . . C5 C 0.9110(5) 0.5087(7) 0.5528(6) 0.059(4) Uani 1 1 d . . . C6 C 0.9204(5) 0.4444(6) 0.5495(6) 0.048(3) Uani 1 1 d . . . H6A H 0.9407 0.4257 0.5839 0.058 Uiso 1 1 calc R . . C7 C 0.9305(5) 0.5499(5) 0.6094(6) 0.056(3) Uani 1 1 d . . . H7A H 0.9344 0.5934 0.5939 0.067 Uiso 1 1 calc R . . C8 C 0.8801(5) 0.5505(5) 0.6562(5) 0.047(3) Uani 1 1 d . . . C9 C 0.8370(5) 0.5972(5) 0.6573(6) 0.061(4) Uani 1 1 d . . . C10 C 0.7902(6) 0.5982(5) 0.6995(7) 0.062(4) Uani 1 1 d . . . C11 C 0.7864(5) 0.5528(5) 0.7446(6) 0.057(3) Uani 1 1 d . . . C12 C 0.8297(5) 0.5065(5) 0.7473(5) 0.046(3) Uani 1 1 d . . . C13 C 0.8753(5) 0.5076(5) 0.7023(5) 0.047(3) Uani 1 1 d . . . H13 H 0.9056 0.4761 0.7037 0.057 Uiso 1 1 calc R . . C14 C 0.8275(4) 0.4584(5) 0.7981(5) 0.039(3) Uani 1 1 d . . . H14A H 0.8046 0.4779 0.8333 0.047 Uiso 1 1 calc R . . C15 C 0.7886(5) 0.4018(5) 0.7766(5) 0.044(3) Uani 1 1 d . . . C16 C 0.7267(5) 0.3981(5) 0.7866(5) 0.042(3) Uani 1 1 d . . . C17 C 0.6921(5) 0.3480(6) 0.7660(6) 0.054(3) Uani 1 1 d . . . C18 C 0.7191(5) 0.2984(5) 0.7344(5) 0.045(3) Uani 1 1 d . . . C19 C 0.7815(5) 0.3009(5) 0.7239(4) 0.035(3) Uani 1 1 d . . . C20 C 0.8161(5) 0.3516(5) 0.7447(4) 0.038(3) Uani 1 1 d . . . H20 H 0.8595 0.3530 0.7374 0.046 Uiso 1 1 calc R . . C21 C 0.8136(4) 0.2472(5) 0.6885(5) 0.040(3) Uani 1 1 d . . . H21A H 0.7866 0.2095 0.6944 0.048 Uiso 1 1 calc R . . C22 C 0.8135(5) 0.2576(5) 0.6194(5) 0.037(3) Uani 1 1 d . . . C23 C 0.7648(6) 0.2346(5) 0.5827(5) 0.049(3) Uani 1 1 d . . . C24 C 0.7657(6) 0.2436(5) 0.5182(6) 0.057(3) Uani 1 1 d . . . C25 C 0.8138(6) 0.2767(5) 0.4919(5) 0.051(3) Uani 1 1 d . . . C26 C 0.8623(5) 0.3004(5) 0.5278(5) 0.046(3) Uani 1 1 d . . . C27 C 0.8608(5) 0.2900(5) 0.5920(5) 0.039(3) Uani 1 1 d . . . H27 H 0.8940 0.3061 0.6176 0.047 Uiso 1 1 calc R . . C28 C 0.9157(5) 0.3380(6) 0.4988(5) 0.052(3) Uani 1 1 d . . . H28A H 0.9161 0.3251 0.4539 0.063 Uiso 1 1 calc R . . C29 C 0.9952(5) 0.5334(6) 0.6361(7) 0.071(4) Uani 1 1 d . . . H29A H 0.9948 0.4886 0.6458 0.085 Uiso 1 1 calc R . . H29B H 1.0263 0.5400 0.6033 0.085 Uiso 1 1 calc R . . C30 C 1.0163(6) 0.5695(6) 0.6935(7) 0.076(4) Uani 1 1 d . . . H30A H 1.0590 0.5565 0.7047 0.091 Uiso 1 1 calc R . . H30B H 0.9890 0.5577 0.7281 0.091 Uiso 1 1 calc R . . C31 C 1.0167(6) 0.6418(7) 0.6887(8) 0.092(5) Uani 1 1 d . . . H31A H 0.9743 0.6560 0.6787 0.110 Uiso 1 1 calc R . . H31B H 1.0445 0.6548 0.6550 0.110 Uiso 1 1 calc R . . C32 C 1.0400(7) 0.6724(8) 0.7522(8) 0.099(5) Uani 1 1 d . . . H32A H 1.0128 0.6574 0.7856 0.119 Uiso 1 1 calc R . . H32B H 1.0825 0.6576 0.7614 0.119 Uiso 1 1 calc R . . C33 C 1.0416(7) 0.7420(7) 0.7549(8) 0.098(5) Uani 1 1 d . . . H33A H 1.0514 0.7562 0.7980 0.118 Uiso 1 1 calc R . . H33B H 0.9998 0.7574 0.7436 0.118 Uiso 1 1 calc R . . C34 C 1.0896(7) 0.7705(7) 0.7110(8) 0.101(5) Uani 1 1 d . . . H34A H 1.0773 0.7598 0.6675 0.121 Uiso 1 1 calc R . . H34B H 1.1306 0.7518 0.7194 0.121 Uiso 1 1 calc R . . C35 C 1.0963(7) 0.8432(7) 0.7183(8) 0.105(5) Uani 1 1 d . . . H35A H 1.0555 0.8624 0.7101 0.126 Uiso 1 1 calc R . . H35B H 1.1098 0.8544 0.7614 0.126 Uiso 1 1 calc R . . C36 C 1.1420(12) 0.8669(9) 0.6745(11) 0.179(10) Uani 1 1 d . . . H36A H 1.1818 0.8464 0.6815 0.268 Uiso 1 1 calc R . . H36B H 1.1476 0.9119 0.6810 0.268 Uiso 1 1 calc R . . H36C H 1.1272 0.8583 0.6318 0.268 Uiso 1 1 calc R . . C37 C 0.8916(5) 0.4430(5) 0.8241(5) 0.055(3) Uani 1 1 d . . . H37A H 0.9156 0.4232 0.7905 0.066 Uiso 1 1 calc R . . H37B H 0.9134 0.4824 0.8362 0.066 Uiso 1 1 calc R . . C38 C 0.8919(6) 0.4011(6) 0.8788(6) 0.073(4) Uani 1 1 d . . . H38A H 0.8774 0.3590 0.8651 0.087 Uiso 1 1 calc R . . H38B H 0.8622 0.4168 0.9098 0.087 Uiso 1 1 calc R . . C39 C 0.9566(7) 0.3965(9) 0.9100(8) 0.112(6) Uani 1 1 d . . . H39A H 0.9866 0.3829 0.8783 0.135 Uiso 1 1 calc R . . H39B H 0.9700 0.4384 0.9253 0.135 Uiso 1 1 calc R . . C40 C 0.9591(10) 0.3524(9) 0.9633(11) 0.141(8) Uani 1 1 d . . . H40A H 0.9471 0.3104 0.9470 0.169 Uiso 1 1 calc R . . H40B H 1.0029 0.3505 0.9780 0.169 Uiso 1 1 calc R . . C41 C 0.9200(11) 0.3660(13) 1.0181(12) 0.155(9) Uani 1 1 d . . . H41A H 0.8760 0.3672 1.0041 0.186 Uiso 1 1 calc R . . H41B H 0.9239 0.3314 1.0476 0.186 Uiso 1 1 calc R . . C42 C 0.9359(11) 0.4251(13) 1.0517(11) 0.166(9) Uani 1 1 d D . . H42A H 0.9269 0.4614 1.0256 0.199 Uiso 1 1 calc R . . H42B H 0.9802 0.4267 1.0650 0.199 Uiso 1 1 calc R . . C43 C 0.8938(14) 0.4224(16) 1.1066(12) 0.231(17) Uani 1 1 d D . . H43A H 0.8497 0.4188 1.0928 0.277 Uiso 1 1 calc R . . H43B H 0.9038 0.3865 1.1329 0.277 Uiso 1 1 calc R . . C44 C 0.9059(11) 0.4825(13) 1.1415(12) 0.227(17) Uani 1 1 d D . . H44A H 0.9432 0.4788 1.1679 0.340 Uiso 1 1 calc R . . H44B H 0.8701 0.4919 1.1674 0.340 Uiso 1 1 calc R . . H44C H 0.9122 0.5160 1.1119 0.340 Uiso 1 1 calc R . . C45 C 0.8760(5) 0.2312(5) 0.7143(5) 0.050(3) Uani 1 1 d . . . H45A H 0.9037 0.2684 0.7123 0.060 Uiso 1 1 calc R . . H45B H 0.8938 0.1983 0.6877 0.060 Uiso 1 1 calc R . . C46 C 0.8754(6) 0.2088(7) 0.7817(6) 0.080(4) Uani 1 1 d . . . H46A H 0.8501 0.2375 0.8069 0.096 Uiso 1 1 calc R . . H46B H 0.8551 0.1672 0.7825 0.096 Uiso 1 1 calc R . . C47 C 0.9396(6) 0.2052(7) 0.8113(6) 0.079(4) Uani 1 1 d . . . H47A H 0.9658 0.1780 0.7855 0.095 Uiso 1 1 calc R . . H47B H 0.9593 0.2472 0.8130 0.095 Uiso 1 1 calc R . . C48 C 0.9366(8) 0.1801(8) 0.8762(7) 0.118(6) Uani 1 1 d . . . H48A H 0.9227 0.1359 0.8741 0.142 Uiso 1 1 calc R . . H48B H 0.9057 0.2036 0.9004 0.142 Uiso 1 1 calc R . . C49 C 1.0019(8) 0.1854(11) 0.9101(8) 0.155(9) Uani 1 1 d . . . H49A H 1.0203 0.2274 0.9046 0.186 Uiso 1 1 calc R . . H49B H 1.0304 0.1544 0.8924 0.186 Uiso 1 1 calc R . . C50 C 0.9912(18) 0.1721(17) 0.9871(17) 0.35(2) Uani 1 1 d . . . H50A H 0.9573 0.1983 1.0027 0.423 Uiso 1 1 calc R . . H50B H 0.9791 0.1279 0.9929 0.423 Uiso 1 1 calc R . . C51 C 1.054(2) 0.1880(18) 1.0254(18) 0.35(2) Uani 1 1 d . . . H51A H 1.0672 0.2324 1.0254 0.423 Uiso 1 1 calc R . . H51B H 1.0893 0.1604 1.0157 0.423 Uiso 1 1 calc R . . C52 C 1.013(3) 0.1671(19) 1.0863(13) 0.40(3) Uani 1 1 d . . . H52A H 0.9784 0.1399 1.0724 0.607 Uiso 1 1 calc R . . H52B H 0.9971 0.2043 1.1070 0.607 Uiso 1 1 calc R . . H52C H 1.0399 0.1447 1.1154 0.607 Uiso 1 1 calc R . . C53 C 0.9805(5) 0.3228(6) 0.5257(5) 0.067(4) Uani 1 1 d . . . H53A H 1.0114 0.3522 0.5085 0.080 Uiso 1 1 calc R . . H53B H 0.9803 0.3297 0.5714 0.080 Uiso 1 1 calc R . . C54 C 1.0011(7) 0.2567(7) 0.5122(7) 0.088(5) Uani 1 1 d . . . H54A H 1.0332 0.2459 0.5435 0.106 Uiso 1 1 calc R . . H54B H 0.9651 0.2282 0.5175 0.106 Uiso 1 1 calc R . . C55 C 1.0263(7) 0.2456(7) 0.4502(6) 0.087(4) Uani 1 1 d . . . H55A H 1.0638 0.2723 0.4456 0.104 Uiso 1 1 calc R . . H55B H 0.9952 0.2583 0.4187 0.104 Uiso 1 1 calc R . . C56 C 1.0433(7) 0.1792(7) 0.4368(8) 0.098(5) Uani 1 1 d . . . H56A H 1.0048 0.1534 0.4334 0.118 Uiso 1 1 calc R . . H56B H 1.0685 0.1638 0.4721 0.118 Uiso 1 1 calc R . . C57 C 1.0812(11) 0.1712(10) 0.3750(9) 0.154(9) Uani 1 1 d . . . H57A H 1.0552 0.1864 0.3402 0.185 Uiso 1 1 calc R . . H57B H 1.1184 0.1990 0.3784 0.185 Uiso 1 1 calc R . . C58 C 1.1004(11) 0.1140(12) 0.3592(10) 0.158(9) Uani 1 1 d . . . H58A H 1.0632 0.0863 0.3551 0.189 Uiso 1 1 calc R . . H58B H 1.1261 0.0985 0.3942 0.189 Uiso 1 1 calc R . . C59 C 1.1374(13) 0.1074(13) 0.3003(12) 0.187(10) Uani 1 1 d . . . H59A H 1.1405 0.0623 0.2912 0.224 Uiso 1 1 calc R . . H59B H 1.1119 0.1249 0.2663 0.224 Uiso 1 1 calc R . . C60 C 1.2001(13) 0.1342(12) 0.2952(12) 0.214(14) Uani 1 1 d . . . H60A H 1.2006 0.1643 0.2615 0.321 Uiso 1 1 calc R . . H60B H 1.2294 0.1011 0.2862 0.321 Uiso 1 1 calc R . . H60C H 1.2122 0.1553 0.3344 0.321 Uiso 1 1 calc R . . O1S O 0.7014(5) -0.0146(5) 0.3640(5) 0.094(3) Uani 1 1 d . . . O2S O 0.6992(9) 0.0790(7) 0.3261(9) 0.186(7) Uani 1 1 d . . . C1S C 0.7027(7) 0.0352(7) 0.3673(8) 0.080(5) Uani 1 1 d . . . C2S C 0.7260(18) 0.0727(12) 0.4207(16) 0.35(3) Uani 1 1 d . . . H2SA H 0.7327 0.0457 0.4564 0.526 Uiso 1 1 calc R . . H2SB H 0.6956 0.1043 0.4314 0.526 Uiso 1 1 calc R . . H2SC H 0.7655 0.0931 0.4101 0.526 Uiso 1 1 calc R . . C3S C 0.6816(13) 0.0545(13) 0.2631(17) 0.206(12) Uani 1 1 d . . . H3SA H 0.6375 0.0636 0.2533 0.248 Uiso 1 1 calc R . . H3SB H 0.6870 0.0089 0.2608 0.248 Uiso 1 1 calc R . . C4S C 0.7251(12) 0.0875(12) 0.2168(10) 0.185(10) Uani 1 1 d . . . H4SA H 0.7160 0.0717 0.1745 0.277 Uiso 1 1 calc R . . H4SB H 0.7685 0.0792 0.2279 0.277 Uiso 1 1 calc R . . H4SC H 0.7183 0.1324 0.2187 0.277 Uiso 1 1 calc R . . O3S O 0.7497(9) 0.4283(9) 0.6001(8) 0.212(7) Uani 1 1 d . . . O4S O 0.635(5) 0.448(4) 0.411(5) 0.55(5) Uani 0.50 1 d PU A 1 O5S O 0.695(2) 0.585(2) 0.500(3) 0.34(3) Uani 0.50 1 d PU B 1 O6S O 0.7228(15) 0.508(2) 0.560(2) 0.25(2) Uani 0.50 1 d PU C 1 O7S O 0.6876(14) 0.3994(17) 0.420(2) 0.25(2) Uani 0.50 1 d PU D 2 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 0.060(6) 0.135(8) 0.045(6) 0.020(6) -0.002(5) 0.030(6) O2 0.089(8) 0.146(10) 0.087(7) 0.076(7) -0.004(6) 0.037(6) O3 0.059(6) 0.073(7) 0.144(9) 0.064(6) 0.005(6) 0.024(5) O4 0.062(6) 0.049(6) 0.134(8) 0.038(6) -0.024(6) -0.002(5) O5 0.080(7) 0.063(7) 0.167(11) 0.006(6) 0.005(6) 0.045(6) O6 0.050(6) 0.077(6) 0.129(8) -0.017(6) 0.029(6) 0.018(5) O7 0.050(5) 0.080(6) 0.093(7) -0.009(5) 0.024(5) 0.014(5) O8 0.050(6) 0.112(8) 0.135(9) -0.005(8) 0.036(6) -0.014(5) O9 0.066(6) 0.069(6) 0.094(8) 0.005(5) -0.009(5) -0.017(5) O10 0.047(5) 0.052(5) 0.099(7) 0.002(5) -0.017(5) -0.005(4) O11 0.106(8) 0.092(7) 0.090(7) -0.017(6) -0.063(7) 0.014(7) O12 0.123(8) 0.117(8) 0.034(5) 0.003(5) -0.010(5) 0.057(7) C1 0.036(7) 0.074(9) 0.032(7) 0.013(7) 0.012(6) 0.017(6) C2 0.047(8) 0.079(11) 0.049(9) 0.031(8) 0.015(7) 0.008(7) C3 0.050(9) 0.086(12) 0.068(10) 0.045(9) -0.004(7) 0.021(8) C4 0.038(8) 0.067(10) 0.093(12) 0.046(9) 0.031(8) 0.018(7) C5 0.024(7) 0.086(11) 0.069(9) 0.044(9) 0.015(6) 0.012(7) C6 0.035(7) 0.055(9) 0.057(9) 0.036(7) 0.020(6) 0.013(6) C7 0.029(7) 0.052(8) 0.087(10) 0.035(7) 0.001(7) 0.004(6) C8 0.025(7) 0.043(7) 0.072(8) 0.014(6) -0.003(6) -0.003(6) C9 0.038(8) 0.044(8) 0.100(11) 0.018(7) 0.003(7) -0.008(6) C10 0.051(9) 0.038(8) 0.098(11) 0.004(7) -0.010(8) 0.017(7) C11 0.039(8) 0.045(8) 0.087(10) 0.003(7) -0.002(7) 0.003(6) C12 0.032(7) 0.050(7) 0.056(8) -0.008(6) 0.000(6) 0.007(6) C13 0.030(7) 0.040(7) 0.072(9) -0.001(6) -0.004(6) 0.005(5) C14 0.032(6) 0.047(7) 0.039(7) -0.005(6) 0.010(5) 0.005(5) C15 0.035(7) 0.047(7) 0.049(7) 0.004(6) 0.000(6) 0.001(6) C16 0.024(7) 0.047(8) 0.055(7) 0.004(6) 0.018(6) 0.009(6) C17 0.027(7) 0.045(8) 0.091(10) -0.006(7) 0.018(6) -0.009(6) C18 0.034(7) 0.046(8) 0.055(8) 0.005(6) 0.004(6) -0.018(6) C19 0.033(7) 0.046(7) 0.028(6) 0.013(5) -0.001(5) -0.002(6) C20 0.032(6) 0.048(7) 0.036(6) 0.008(5) 0.003(5) 0.003(6) C21 0.033(6) 0.033(6) 0.052(7) -0.002(5) -0.013(5) 0.003(5) C22 0.029(6) 0.041(7) 0.042(7) -0.001(6) -0.013(6) 0.013(5) C23 0.056(9) 0.046(7) 0.046(8) 0.002(6) 0.000(7) 0.019(7) C24 0.070(9) 0.045(8) 0.055(9) -0.007(7) -0.036(8) 0.005(7) C25 0.071(9) 0.047(8) 0.036(8) -0.003(6) -0.008(7) 0.022(7) C26 0.046(8) 0.062(8) 0.031(7) -0.011(6) -0.007(6) 0.025(6) C27 0.032(7) 0.053(7) 0.033(7) 0.010(5) -0.003(5) 0.014(6) C28 0.041(7) 0.086(10) 0.032(7) 0.022(6) 0.017(5) 0.021(7) C29 0.032(7) 0.063(9) 0.119(12) 0.042(9) 0.003(8) 0.000(6) C30 0.044(8) 0.062(10) 0.121(13) 0.033(9) -0.016(8) 0.000(7) C31 0.046(9) 0.098(12) 0.135(15) 0.043(11) 0.015(9) 0.025(8) C32 0.067(10) 0.103(14) 0.128(15) 0.012(11) -0.002(10) -0.001(9) C33 0.072(11) 0.080(12) 0.143(15) 0.021(10) 0.012(10) 0.020(9) C34 0.091(12) 0.071(11) 0.143(14) 0.035(10) 0.021(11) 0.031(9) C35 0.094(12) 0.096(14) 0.126(14) 0.022(11) 0.006(11) -0.004(10) C36 0.25(3) 0.099(15) 0.19(2) 0.049(15) 0.05(2) -0.019(16) C37 0.053(8) 0.055(8) 0.057(8) 0.004(6) 0.000(6) 0.016(6) C38 0.056(9) 0.097(11) 0.064(9) -0.007(8) -0.009(7) 0.015(7) C39 0.102(13) 0.138(15) 0.096(13) -0.029(12) -0.033(10) 0.045(11) C40 0.16(2) 0.124(16) 0.131(18) 0.001(15) -0.073(17) 0.023(14) C41 0.17(2) 0.19(2) 0.114(19) 0.064(17) 0.025(17) 0.04(2) C42 0.14(2) 0.21(3) 0.14(2) 0.01(2) 0.014(17) 0.06(2) C43 0.16(2) 0.42(6) 0.12(2) 0.03(3) 0.01(2) -0.03(3) C44 0.12(2) 0.45(5) 0.12(2) 0.12(3) 0.064(18) 0.07(3) C45 0.052(8) 0.056(8) 0.042(7) 0.007(6) 0.000(6) 0.003(6) C46 0.062(9) 0.107(11) 0.071(10) 0.028(8) -0.017(7) -0.006(8) C47 0.079(10) 0.099(11) 0.060(9) 0.028(8) 0.009(8) 0.019(8) C48 0.146(17) 0.137(15) 0.074(11) 0.031(10) -0.004(11) 0.031(12) C49 0.103(14) 0.27(3) 0.094(14) 0.039(15) -0.022(11) 0.051(15) C50 0.41(4) 0.34(3) 0.30(3) 0.18(3) -0.24(3) -0.12(3) C51 0.41(4) 0.34(3) 0.30(3) 0.18(3) -0.24(3) -0.12(3) C52 0.74(10) 0.37(5) 0.11(2) 0.08(3) -0.06(4) 0.09(6) C53 0.047(8) 0.102(11) 0.053(8) 0.007(7) 0.007(6) 0.035(7) C54 0.084(10) 0.103(12) 0.080(11) 0.029(9) 0.012(8) 0.042(9) C55 0.102(12) 0.091(12) 0.066(10) -0.008(8) -0.006(9) 0.002(9) C56 0.102(12) 0.095(13) 0.097(13) -0.018(10) -0.014(10) 0.037(9) C57 0.21(2) 0.127(17) 0.121(18) -0.036(14) -0.059(17) 0.078(17) C58 0.17(2) 0.20(3) 0.108(17) 0.017(16) 0.007(15) 0.083(18) C59 0.18(3) 0.24(3) 0.13(2) 0.00(2) -0.01(2) 0.06(2) C60 0.18(2) 0.22(3) 0.24(3) -0.11(2) 0.11(2) -0.07(2) O1S 0.106(8) 0.075(8) 0.103(8) 0.003(7) 0.002(6) 0.011(7) O2S 0.28(2) 0.121(13) 0.148(14) -0.009(12) -0.054(14) -0.034(12) C1S 0.124(13) 0.018(8) 0.098(12) 0.007(9) 0.010(9) 0.016(9) C2S 0.49(6) 0.19(3) 0.37(5) -0.19(3) 0.29(5) -0.23(4) C3S 0.19(3) 0.19(3) 0.24(3) 0.05(3) 0.03(2) -0.07(2) C4S 0.21(3) 0.19(2) 0.16(2) 0.034(18) -0.006(19) 0.09(2) O3S 0.207(17) 0.225(18) 0.206(17) 0.046(14) 0.009(13) 0.000(14) O4S 0.61(9) 0.46(7) 0.56(8) -0.36(7) -0.07(7) 0.04(7) O5S 0.24(4) 0.24(4) 0.53(7) 0.20(4) -0.08(4) -0.07(3) O6S 0.13(2) 0.34(5) 0.28(4) -0.12(4) 0.03(3) -0.09(3) O7S 0.12(2) 0.20(3) 0.42(5) -0.04(3) 0.12(3) 0.02(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 O1 C2 1.403(15) . ? O1 H1 0.8400 . ? O2 C3 1.413(14) . ? O2 H2 0.8400 . ? O3 C4 1.386(14) . ? O3 H3 0.8400 . ? O4 C9 1.401(13) . ? O4 H4 0.8400 . ? O5 C10 1.386(13) . ? O5 H5 0.8400 . ? O6 C11 1.381(13) . ? O6 H6 0.8400 . ? O7 C16 1.392(12) . ? O7 H7 0.8400 . ? O8 C17 1.395(12) . ? O8 H8 0.8400 . ? O9 C18 1.363(12) . ? O9 H9 0.8400 . ? O10 C23 1.382(13) . ? O10 H10 0.8400 . ? O11 C24 1.393(13) . ? O11 H11 0.8400 . ? O12 C25 1.395(12) . ? O12 H12 0.8400 . ? C1 C6 1.373(15) . ? C1 C2 1.386(15) . ? C1 C28 1.510(16) . ? C2 C3 1.344(17) . ? C3 C4 1.414(18) . ? C4 C5 1.389(16) . ? C5 C6 1.402(16) . ? C5 C7 1.540(17) . ? C6 H6A 0.9500 . ? C7 C8 1.492(15) . ? C7 C29 1.545(15) . ? C7 H7A 1.0000 . ? C8 C13 1.371(14) . ? C8 C9 1.378(15) . ? C9 C10 1.366(16) . ? C10 C11 1.391(16) . ? C11 C12 1.377(14) . ? C12 C13 1.390(14) . ? C12 C14 1.519(14) . ? C13 H13 0.9500 . ? C14 C37 1.520(14) . ? C14 C15 1.523(14) . ? C14 H14A 1.0000 . ? C15 C16 1.354(13) . ? C15 C20 1.413(14) . ? C16 C17 1.360(14) . ? C17 C18 1.396(15) . ? C18 C19 1.366(13) . ? C19 C20 1.372(13) . ? C19 C21 1.551(14) . ? C20 H20 0.9500 . ? C21 C45 1.492(13) . ? C21 C22 1.507(14) . ? C21 H21A 1.0000 . ? C22 C27 1.369(13) . ? C22 C23 1.380(14) . ? C23 C24 1.406(15) . ? C24 C25 1.381(16) . ? C25 C26 1.371(15) . ? C26 C27 1.403(13) . ? C26 C28 1.541(15) . ? C27 H27 0.9500 . ? C28 C53 1.542(14) . ? C28 H28A 1.0000 . ? C29 C30 1.506(18) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.558(18) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.57(2) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.496(19) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.538(19) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.57(2) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.46(2) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.495(15) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.540(18) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.50(2) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.49(3) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.48(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.502(5) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.498(5) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.536(15) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.514(16) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.508(18) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.57(2) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.70(4) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.60(4) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.66(5) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.522(17) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.465(17) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.503(18) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.58(3) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.34(2) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.51(3) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.46(3) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? O1S C1S 1.072(14) . ? O2S C1S 1.306(19) . ? O2S C3S 1.49(3) . ? C1S C2S 1.47(3) . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? C3S C4S 1.55(3) . ? C3S H3SA 0.9900 . ? C3S H3SB 0.9900 . ? C4S H4SA 0.9800 . ? C4S H4SB 0.9800 . ? C4S H4SC 0.9800 . ? 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 O1 H1 109.5 . . ? C3 O2 H2 109.5 . . ? C4 O3 H3 109.5 . . ? C9 O4 H4 109.5 . . ? C10 O5 H5 109.5 . . ? C11 O6 H6 109.5 . . ? C16 O7 H7 109.5 . . ? C17 O8 H8 109.5 . . ? C18 O9 H9 109.5 . . ? C23 O10 H10 109.5 . . ? C24 O11 H11 109.5 . . ? C25 O12 H12 109.5 . . ? C6 C1 C2 116.5(12) . . ? C6 C1 C28 121.5(10) . . ? C2 C1 C28 121.9(12) . . ? C3 C2 C1 121.6(14) . . ? C3 C2 O1 118.0(12) . . ? C1 C2 O1 120.4(13) . . ? C2 C3 C4 121.6(12) . . ? C2 C3 O2 119.9(16) . . ? C4 C3 O2 118.5(14) . . ? O3 C4 C5 122.2(16) . . ? O3 C4 C3 119.2(13) . . ? C5 C4 C3 118.7(13) . . ? C4 C5 C6 117.1(14) . . ? C4 C5 C7 119.4(13) . . ? C6 C5 C7 123.5(11) . . ? C1 C6 C5 124.4(11) . . ? C1 C6 H6A 117.8 . . ? C5 C6 H6A 117.8 . . ? C8 C7 C5 110.3(9) . . ? C8 C7 C29 114.4(10) . . ? C5 C7 C29 112.5(10) . . ? C8 C7 H7A 106.4 . . ? C5 C7 H7A 106.4 . . ? C29 C7 H7A 106.4 . . ? C13 C8 C9 115.7(11) . . ? C13 C8 C7 123.1(10) . . ? C9 C8 C7 121.1(10) . . ? C10 C9 C8 121.9(11) . . ? C10 C9 O4 116.8(11) . . ? C8 C9 O4 121.2(12) . . ? C9 C10 O5 121.8(12) . . ? C9 C10 C11 120.2(11) . . ? O5 C10 C11 118.0(13) . . ? O6 C11 C12 120.8(11) . . ? O6 C11 C10 118.8(11) . . ? C12 C11 C10 120.4(12) . . ? C11 C12 C13 116.3(11) . . ? C11 C12 C14 120.8(10) . . ? C13 C12 C14 122.9(9) . . ? C8 C13 C12 125.4(10) . . ? C8 C13 H13 117.3 . . ? C12 C13 H13 117.3 . . ? C12 C14 C37 113.1(8) . . ? C12 C14 C15 110.4(8) . . ? C37 C14 C15 114.3(9) . . ? C12 C14 H14A 106.2 . . ? C37 C14 H14A 106.2 . . ? C15 C14 H14A 106.2 . . ? C16 C15 C20 117.7(10) . . ? C16 C15 C14 121.5(10) . . ? C20 C15 C14 120.8(9) . . ? C15 C16 C17 121.0(10) . . ? C15 C16 O7 120.7(11) . . ? C17 C16 O7 118.2(9) . . ? C16 C17 C18 121.5(10) . . ? C16 C17 O8 120.6(11) . . ? C18 C17 O8 117.9(11) . . ? O9 C18 C19 124.3(11) . . ? O9 C18 C17 117.1(10) . . ? C19 C18 C17 118.6(10) . . ? C20 C19 C18 119.6(10) . . ? C20 C19 C21 119.8(9) . . ? C18 C19 C21 120.6(10) . . ? C19 C20 C15 121.6(10) . . ? C19 C20 H20 119.2 . . ? C15 C20 H20 119.2 . . ? C45 C21 C22 113.1(8) . . ? C45 C21 C19 114.2(8) . . ? C22 C21 C19 111.6(7) . . ? C45 C21 H21A 105.7 . . ? C22 C21 H21A 105.7 . . ? C19 C21 H21A 105.7 . . ? C27 C22 C23 119.0(10) . . ? C27 C22 C21 121.4(10) . . ? C23 C22 C21 119.6(10) . . ? C22 C23 O10 122.1(10) . . ? C22 C23 C24 119.2(12) . . ? O10 C23 C24 118.7(12) . . ? C25 C24 O11 120.2(12) . . ? C25 C24 C23 120.5(11) . . ? O11 C24 C23 119.3(13) . . ? C26 C25 C24 120.9(11) . . ? C26 C25 O12 121.9(12) . . ? C24 C25 O12 117.2(12) . . ? C25 C26 C27 117.6(11) . . ? C25 C26 C28 121.1(10) . . ? C27 C26 C28 121.3(10) . . ? C22 C27 C26 122.8(10) . . ? C22 C27 H27 118.6 . . ? C26 C27 H27 118.6 . . ? C1 C28 C26 111.0(8) . . ? C1 C28 C53 113.3(10) . . ? C26 C28 C53 113.7(9) . . ? C1 C28 H28A 106.0 . . ? C26 C28 H28A 106.0 . . ? C53 C28 H28A 106.0 . . ? C30 C29 C7 115.8(11) . . ? C30 C29 H29A 108.3 . . ? C7 C29 H29A 108.3 . . ? C30 C29 H29B 108.3 . . ? C7 C29 H29B 108.3 . . ? H29A C29 H29B 107.4 . . ? C29 C30 C31 116.3(12) . . ? C29 C30 H30A 108.2 . . ? C31 C30 H30A 108.2 . . ? C29 C30 H30B 108.2 . . ? C31 C30 H30B 108.2 . . ? H30A C30 H30B 107.4 . . ? C30 C31 C32 110.0(12) . . ? C30 C31 H31A 109.7 . . ? C32 C31 H31A 109.7 . . ? C30 C31 H31B 109.7 . . ? C32 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? C33 C32 C31 115.9(14) . . ? C33 C32 H32A 108.3 . . ? C31 C32 H32A 108.3 . . ? C33 C32 H32B 108.3 . . ? C31 C32 H32B 108.3 . . ? H32A C32 H32B 107.4 . . ? C32 C33 C34 112.8(13) . . ? C32 C33 H33A 109.0 . . ? C34 C33 H33A 109.0 . . ? C32 C33 H33B 109.0 . . ? C34 C33 H33B 109.0 . . ? H33A C33 H33B 107.8 . . ? C33 C34 C35 113.2(13) . . ? C33 C34 H34A 108.9 . . ? C35 C34 H34A 108.9 . . ? C33 C34 H34B 108.9 . . ? C35 C34 H34B 108.9 . . ? H34A C34 H34B 107.8 . . ? C36 C35 C34 110.0(14) . . ? C36 C35 H35A 109.7 . . ? C34 C35 H35A 109.7 . . ? C36 C35 H35B 109.7 . . ? C34 C35 H35B 109.7 . . ? H35A C35 H35B 108.2 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C14 115.4(9) . . ? C38 C37 H37A 108.4 . . ? C14 C37 H37A 108.4 . . ? C38 C37 H37B 108.4 . . ? C14 C37 H37B 108.4 . . ? H37A C37 H37B 107.5 . . ? C37 C38 C39 112.8(12) . . ? C37 C38 H38A 109.0 . . ? C39 C38 H38A 109.0 . . ? C37 C38 H38B 109.0 . . ? C39 C38 H38B 109.0 . . ? H38A C38 H38B 107.8 . . ? C40 C39 C38 114.1(16) . . ? C40 C39 H39A 108.7 . . ? C38 C39 H39A 108.7 . . ? C40 C39 H39B 108.7 . . ? C38 C39 H39B 108.7 . . ? H39A C39 H39B 107.6 . . ? C41 C40 C39 117.9(17) . . ? C41 C40 H40A 107.8 . . ? C39 C40 H40A 107.8 . . ? C41 C40 H40B 107.8 . . ? C39 C40 H40B 107.8 . . ? H40A C40 H40B 107.2 . . ? C42 C41 C40 115(2) . . ? C42 C41 H41A 108.6 . . ? C40 C41 H41A 108.6 . . ? C42 C41 H41B 108.6 . . ? C40 C41 H41B 108.6 . . ? H41A C41 H41B 107.5 . . ? C41 C42 C43 102(2) . . ? C41 C42 H42A 111.3 . . ? C43 C42 H42A 111.3 . . ? C41 C42 H42B 111.3 . . ? C43 C42 H42B 111.3 . . ? H42A C42 H42B 109.2 . . ? C44 C43 C42 105(2) . . ? C44 C43 H43A 110.8 . . ? C42 C43 H43A 110.8 . . ? C44 C43 H43B 110.8 . . ? C42 C43 H43B 110.8 . . ? H43A C43 H43B 108.8 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C21 C45 C46 114.3(9) . . ? C21 C45 H45A 108.7 . . ? C46 C45 H45A 108.7 . . ? C21 C45 H45B 108.7 . . ? C46 C45 H45B 108.7 . . ? H45A C45 H45B 107.6 . . ? C47 C46 C45 113.5(10) . . ? C47 C46 H46A 108.9 . . ? C45 C46 H46A 108.9 . . ? C47 C46 H46B 108.9 . . ? C45 C46 H46B 108.9 . . ? H46A C46 H46B 107.7 . . ? C48 C47 C46 111.2(12) . . ? C48 C47 H47A 109.4 . . ? C46 C47 H47A 109.4 . . ? C48 C47 H47B 109.4 . . ? C46 C47 H47B 109.4 . . ? H47A C47 H47B 108.0 . . ? C47 C48 C49 110.9(15) . . ? C47 C48 H48A 109.5 . . ? C49 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? C49 C48 H48B 109.5 . . ? H48A C48 H48B 108.0 . . ? C48 C49 C50 107.8(18) . . ? C48 C49 H49A 110.1 . . ? C50 C49 H49A 110.1 . . ? C48 C49 H49B 110.1 . . ? C50 C49 H49B 110.1 . . ? H49A C49 H49B 108.5 . . ? C51 C50 C49 110(3) . . ? C51 C50 H50A 109.7 . . ? C49 C50 H50A 109.7 . . ? C51 C50 H50B 109.7 . . ? C49 C50 H50B 109.7 . . ? H50A C50 H50B 108.2 . . ? C50 C51 C52 84(3) . . ? C50 C51 H51A 114.6 . . ? C52 C51 H51A 114.6 . . ? C50 C51 H51B 114.6 . . ? C52 C51 H51B 114.7 . . ? H51A C51 H51B 111.7 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.4 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 C28 114.4(11) . . ? C54 C53 H53A 108.7 . . ? C28 C53 H53A 108.7 . . ? C54 C53 H53B 108.7 . . ? C28 C53 H53B 108.7 . . ? H53A C53 H53B 107.6 . . ? C55 C54 C53 115.7(11) . . ? C55 C54 H54A 108.4 . . ? C53 C54 H54A 108.4 . . ? C55 C54 H54B 108.4 . . ? C53 C54 H54B 108.4 . . ? H54A C54 H54B 107.4 . . ? C54 C55 C56 114.6(13) . . ? C54 C55 H55A 108.6 . . ? C56 C55 H55A 108.6 . . ? C54 C55 H55B 108.6 . . ? C56 C55 H55B 108.6 . . ? H55A C55 H55B 107.6 . . ? C55 C56 C57 113.0(14) . . ? C55 C56 H56A 109.0 . . ? C57 C56 H56A 109.0 . . ? C55 C56 H56B 109.0 . . ? C57 C56 H56B 109.0 . . ? H56A C56 H56B 107.8 . . ? C58 C57 C56 118(2) . . ? C58 C57 H57A 107.8 . . ? C56 C57 H57A 107.8 . . ? C58 C57 H57B 107.8 . . ? C56 C57 H57B 107.8 . . ? H57A C57 H57B 107.1 . . ? C57 C58 C59 117(2) . . ? C57 C58 H58A 108.0 . . ? C59 C58 H58A 108.0 . . ? C57 C58 H58B 108.0 . . ? C59 C58 H58B 108.0 . . ? H58A C58 H58B 107.2 . . ? C60 C59 C58 122(2) . . ? C60 C59 H59A 106.9 . . ? C58 C59 H59A 106.9 . . ? C60 C59 H59B 106.8 . . ? C58 C59 H59B 106.8 . . ? H59A C59 H59B 106.7 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C1S O2S C3S 112.5(17) . . ? O1S C1S O2S 133.4(18) . . ? O1S C1S C2S 126(2) . . ? O2S C1S C2S 99.0(19) . . ? C1S C2S H2SA 109.5 . . ? C1S C2S H2SB 109.5 . . ? H2SA C2S H2SB 109.5 . . ? C1S C2S H2SC 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? O2S C3S C4S 107(2) . . ? O2S C3S H3SA 110.4 . . ? C4S C3S H3SA 110.4 . . ? O2S C3S H3SB 110.4 . . ? C4S C3S H3SB 110.4 . . ? H3SA C3S H3SB 108.6 . . ? C3S C4S H4SA 109.5 . . ? C3S C4S H4SB 109.5 . . ? H4SA C4S H4SB 109.5 . . ? C3S C4S H4SC 109.5 . . ? H4SA C4S H4SC 109.5 . . ? H4SB C4S H4SC 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 3.5(16) . . . . ? C28 C1 C2 C3 -178.6(10) . . . . ? C6 C1 C2 O1 -179.1(9) . . . . ? C28 C1 C2 O1 -1.1(15) . . . . ? C1 C2 C3 C4 -1.3(18) . . . . ? O1 C2 C3 C4 -178.8(10) . . . . ? C1 C2 C3 O2 179.4(10) . . . . ? O1 C2 C3 O2 1.8(16) . . . . ? C2 C3 C4 O3 -179.8(10) . . . . ? O2 C3 C4 O3 -0.5(16) . . . . ? C2 C3 C4 C5 -0.7(18) . . . . ? O2 C3 C4 C5 178.6(9) . . . . ? O3 C4 C5 C6 179.5(9) . . . . ? C3 C4 C5 C6 0.5(15) . . . . ? O3 C4 C5 C7 2.6(15) . . . . ? C3 C4 C5 C7 -176.5(10) . . . . ? C2 C1 C6 C5 -3.9(15) . . . . ? C28 C1 C6 C5 178.2(9) . . . . ? C4 C5 C6 C1 1.9(15) . . . . ? C7 C5 C6 C1 178.7(9) . . . . ? C4 C5 C7 C8 89.7(11) . . . . ? C6 C5 C7 C8 -87.0(12) . . . . ? C4 C5 C7 C29 -141.3(10) . . . . ? C6 C5 C7 C29 42.0(14) . . . . ? C5 C7 C8 C13 88.4(13) . . . . ? C29 C7 C8 C13 -39.6(16) . . . . ? C5 C7 C8 C9 -95.2(13) . . . . ? C29 C7 C8 C9 136.8(12) . . . . ? C13 C8 C9 C10 -3.9(17) . . . . ? C7 C8 C9 C10 179.5(12) . . . . ? C13 C8 C9 O4 -178.5(10) . . . . ? C7 C8 C9 O4 4.9(17) . . . . ? C8 C9 C10 O5 -175.5(11) . . . . ? O4 C9 C10 O5 -0.7(18) . . . . ? C8 C9 C10 C11 2.7(19) . . . . ? O4 C9 C10 C11 177.5(11) . . . . ? C9 C10 C11 O6 179.7(11) . . . . ? O5 C10 C11 O6 -2.0(17) . . . . ? C9 C10 C11 C12 0.0(18) . . . . ? O5 C10 C11 C12 178.2(11) . . . . ? O6 C11 C12 C13 179.2(10) . . . . ? C10 C11 C12 C13 -1.1(16) . . . . ? O6 C11 C12 C14 -2.5(16) . . . . ? C10 C11 C12 C14 177.3(10) . . . . ? C9 C8 C13 C12 2.8(16) . . . . ? C7 C8 C13 C12 179.3(11) . . . . ? C11 C12 C13 C8 -0.4(16) . . . . ? C14 C12 C13 C8 -178.7(10) . . . . ? C11 C12 C14 C37 -139.2(10) . . . . ? C13 C12 C14 C37 39.1(14) . . . . ? C11 C12 C14 C15 91.4(12) . . . . ? C13 C12 C14 C15 -90.3(12) . . . . ? C12 C14 C15 C16 -90.4(11) . . . . ? C37 C14 C15 C16 140.8(10) . . . . ? C12 C14 C15 C20 88.8(11) . . . . ? C37 C14 C15 C20 -40.0(13) . . . . ? C20 C15 C16 C17 -0.7(15) . . . . ? C14 C15 C16 C17 178.5(10) . . . . ? C20 C15 C16 O7 177.5(9) . . . . ? C14 C15 C16 O7 -3.3(15) . . . . ? C15 C16 C17 C18 0.6(17) . . . . ? O7 C16 C17 C18 -177.6(10) . . . . ? C15 C16 C17 O8 -178.0(10) . . . . ? O7 C16 C17 O8 3.8(16) . . . . ? C16 C17 C18 O9 178.8(10) . . . . ? O8 C17 C18 O9 -2.6(16) . . . . ? C16 C17 C18 C19 -0.3(17) . . . . ? O8 C17 C18 C19 178.3(10) . . . . ? O9 C18 C19 C20 -178.9(9) . . . . ? C17 C18 C19 C20 0.1(15) . . . . ? O9 C18 C19 C21 1.5(15) . . . . ? C17 C18 C19 C21 -179.4(9) . . . . ? C18 C19 C20 C15 -0.3(14) . . . . ? C21 C19 C20 C15 179.3(8) . . . . ? C16 C15 C20 C19 0.5(14) . . . . ? C14 C15 C20 C19 -178.7(9) . . . . ? C20 C19 C21 C45 40.1(12) . . . . ? C18 C19 C21 C45 -140.4(10) . . . . ? C20 C19 C21 C22 -89.8(11) . . . . ? C18 C19 C21 C22 89.7(11) . . . . ? C45 C21 C22 C27 -41.5(13) . . . . ? C19 C21 C22 C27 88.9(11) . . . . ? C45 C21 C22 C23 138.9(10) . . . . ? C19 C21 C22 C23 -90.6(11) . . . . ? C27 C22 C23 O10 -179.5(9) . . . . ? C21 C22 C23 O10 0.1(14) . . . . ? C27 C22 C23 C24 1.5(14) . . . . ? C21 C22 C23 C24 -178.9(9) . . . . ? C22 C23 C24 C25 -1.9(16) . . . . ? O10 C23 C24 C25 179.1(9) . . . . ? C22 C23 C24 O11 179.2(9) . . . . ? O10 C23 C24 O11 0.1(15) . . . . ? O11 C24 C25 C26 -179.7(9) . . . . ? C23 C24 C25 C26 1.3(16) . . . . ? O11 C24 C25 O12 -1.0(15) . . . . ? C23 C24 C25 O12 -179.9(9) . . . . ? C24 C25 C26 C27 -0.4(15) . . . . ? O12 C25 C26 C27 -179.1(9) . . . . ? C24 C25 C26 C28 -179.3(10) . . . . ? O12 C25 C26 C28 2.0(15) . . . . ? C23 C22 C27 C26 -0.7(14) . . . . ? C21 C22 C27 C26 179.8(9) . . . . ? C25 C26 C27 C22 0.1(14) . . . . ? C28 C26 C27 C22 179.0(9) . . . . ? C6 C1 C28 C26 89.8(12) . . . . ? C2 C1 C28 C26 -88.0(12) . . . . ? C6 C1 C28 C53 -39.5(13) . . . . ? C2 C1 C28 C53 142.6(10) . . . . ? C25 C26 C28 C1 91.6(12) . . . . ? C27 C26 C28 C1 -87.3(12) . . . . ? C25 C26 C28 C53 -139.3(10) . . . . ? C27 C26 C28 C53 41.8(14) . . . . ? C8 C7 C29 C30 -50.3(14) . . . . ? C5 C7 C29 C30 -177.1(10) . . . . ? C7 C29 C30 C31 -55.0(14) . . . . ? C29 C30 C31 C32 -179.8(11) . . . . ? C30 C31 C32 C33 -178.8(11) . . . . ? C31 C32 C33 C34 -66.1(17) . . . . ? C32 C33 C34 C35 -174.3(14) . . . . ? C33 C34 C35 C36 -179.1(16) . . . . ? C12 C14 C37 C38 173.7(10) . . . . ? C15 C14 C37 C38 -58.9(13) . . . . ? C14 C37 C38 C39 -169.9(11) . . . . ? C37 C38 C39 C40 -177.3(13) . . . . ? C38 C39 C40 C41 -62(2) . . . . ? C39 C40 C41 C42 -63(3) . . . . ? C40 C41 C42 C43 -175(2) . . . . ? C41 C42 C43 C44 -178(3) . . . . ? C22 C21 C45 C46 -169.5(10) . . . . ? C19 C21 C45 C46 61.4(13) . . . . ? C21 C45 C46 C47 -168.5(11) . . . . ? C45 C46 C47 C48 -177.2(12) . . . . ? C46 C47 C48 C49 -171.9(15) . . . . ? C47 C48 C49 C50 167.2(19) . . . . ? C48 C49 C50 C51 -171(3) . . . . ? C49 C50 C51 C52 180(3) . . . . ? C1 C28 C53 C54 -166.9(10) . . . . ? C26 C28 C53 C54 65.1(13) . . . . ? C28 C53 C54 C55 80.4(15) . . . . ? C53 C54 C55 C56 -177.0(12) . . . . ? C54 C55 C56 C57 -169.6(14) . . . . ? C55 C56 C57 C58 178.2(18) . . . . ? C56 C57 C58 C59 -179.2(18) . . . . ? C57 C58 C59 C60 68(3) . . . . ? C3S O2S C1S O1S 10(3) . . . . ? C3S O2S C1S C2S 175(2) . . . . ? C1S O2S C3S C4S -136(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.830 _refine_diff_density_min -0.623 _refine_diff_density_rms 0.132 # Attachment 'C10-Pg(g6508).cif' data_g6508 _database_code_depnum_ccdc_archive 'CCDC 701457' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C146 H227 N O28' _chemical_formula_weight 2444.29 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 37.210(2) _cell_length_b 37.210(2) _cell_length_c 25.915(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 31075(5) _cell_formula_units_Z 9 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8076 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 19.76 _exptl_crystal_description rectangular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.176 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12006 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9752 _exptl_absorpt_correction_T_max 0.9910 _exptl_absorpt_process_details 'sadabs v2008/1' _exptl_special_details ; All H atoms were added in their calculated positions and were treated using appropriate riding models. ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 186526 _diffrn_reflns_av_R_equivalents 0.2395 _diffrn_reflns_av_sigmaI/netI 0.1302 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 24.00 _reflns_number_total 10865 _reflns_number_gt 4254 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Apex II (Bruker, 2006)' _computing_cell_refinement 'Bruker-Apex II (Bruker, 2006)' _computing_data_reduction 'Bruker-SAINT (Bruker, 2006)' _computing_structure_solution 'Bruker-SHELXTL (Sheldrick, G.M., 2008)' _computing_structure_refinement 'Bruker-SHELXTL (Sheldrick, G.M., 2008)' _computing_molecular_graphics 'Bruker-SHELXTL (Sheldrick, G.M., 2008)' _computing_publication_material 'Bruker-SHELXTL (Sheldrick, G.M., 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00093(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10865 _refine_ls_number_parameters 717 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.3292 _refine_ls_R_factor_gt 0.1898 _refine_ls_wR_factor_ref 0.5360 _refine_ls_wR_factor_gt 0.4486 _refine_ls_goodness_of_fit_ref 1.601 _refine_ls_restrained_S_all 1.601 _refine_ls_shift/su_max 0.214 _refine_ls_shift/su_mean 0.015 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 0.7183(2) 0.1501(2) -0.1533(3) 0.079(2) Uani 1 1 d . . . H1 H 0.7359 0.1693 -0.1346 0.119 Uiso 1 1 calc R . . O2 O 0.6468(3) 0.1333(3) -0.1989(3) 0.124(4) Uani 1 1 d . . . H2 H 0.6511 0.1577 -0.1982 0.186 Uiso 1 1 calc R . . O3 O 0.5723(2) 0.0881(2) -0.1510(3) 0.094(3) Uani 1 1 d . . . H3 H 0.5759 0.1095 -0.1663 0.140 Uiso 1 1 calc R . . O4 O 0.5112(2) 0.0834(2) -0.0912(3) 0.071(2) Uani 1 1 d . . . H4 H 0.5294 0.0967 -0.1135 0.106 Uiso 1 1 calc R . . O5 O 0.4926(2) 0.1352(2) -0.0392(3) 0.083(2) Uani 1 1 d . . . H5 H 0.5050 0.1506 -0.0644 0.124 Uiso 1 1 calc R . . O6 O 0.5203(2) 0.16122(19) 0.0570(3) 0.062(2) Uani 1 1 d . . . H6 H 0.5404 0.1857 0.0563 0.093 Uiso 1 1 calc R . . O7 O 0.5861(2) 0.2209(2) 0.1078(3) 0.087(3) Uani 1 1 d . . . H7 H 0.5898 0.2404 0.1276 0.130 Uiso 1 1 calc R . . O8 O 0.6635(3) 0.2896(2) 0.1094(4) 0.118(4) Uani 1 1 d . . . H8 H 0.6534 0.2928 0.0820 0.177 Uiso 1 1 calc R . . O9 O 0.7322(2) 0.28262(19) 0.1118(4) 0.097(3) Uani 1 1 d . . . H9 H 0.7447 0.2845 0.0841 0.146 Uiso 1 1 calc R . . O10 O 0.7903(2) 0.2763(2) 0.0565(4) 0.092(3) Uani 1 1 d . . . H10 H 0.7911 0.2730 0.0885 0.138 Uiso 1 1 calc R . . O11 O 0.8138(2) 0.2728(2) -0.0426(4) 0.115(4) Uani 1 1 d . . . H11 H 0.8065 0.2908 -0.0423 0.173 Uiso 1 1 calc R . . O12 O 0.7825(2) 0.2024(3) -0.0932(3) 0.089(3) Uani 1 1 d . . . H12 H 0.7816 0.1800 -0.1004 0.133 Uiso 1 1 calc R . . C1 C 0.6816(3) 0.1127(2) -0.0771(4) 0.041(2) Uani 1 1 d . . . C2 C 0.6820(3) 0.1274(3) -0.1260(4) 0.055(3) Uani 1 1 d . . . C3 C 0.6452(3) 0.1196(3) -0.1500(4) 0.064(3) Uani 1 1 d . . . C4 C 0.6079(3) 0.0966(3) -0.1258(4) 0.062(3) Uani 1 1 d . . . C5 C 0.6065(3) 0.0806(2) -0.0751(4) 0.044(2) Uani 1 1 d . . . C6 C 0.6438(3) 0.0902(2) -0.0530(4) 0.040(2) Uani 1 1 d . . . H6A H 0.6435 0.0806 -0.0189 0.048 Uiso 1 1 calc R . . C7 C 0.5645(3) 0.0548(2) -0.0488(3) 0.040(2) Uani 1 1 d . . . H7A H 0.5433 0.0404 -0.0765 0.048 Uiso 1 1 calc R . . C8 C 0.5524(2) 0.0828(2) -0.0191(4) 0.040(2) Uani 1 1 d . . . C9 C 0.5276(3) 0.0964(3) -0.0434(4) 0.043(2) Uani 1 1 d . . . C10 C 0.5174(3) 0.1226(3) -0.0166(4) 0.054(3) Uani 1 1 d . . . C11 C 0.5312(3) 0.1354(3) 0.0323(4) 0.047(2) Uani 1 1 d . . . C12 C 0.5567(2) 0.1228(3) 0.0575(4) 0.041(2) Uani 1 1 d . . . C13 C 0.5664(3) 0.0969(3) 0.0304(4) 0.041(2) Uani 1 1 d . . . H13A H 0.5836 0.0882 0.0467 0.049 Uiso 1 1 calc R . . C14 C 0.5723(3) 0.1377(3) 0.1115(3) 0.042(2) Uani 1 1 d . . . H14A H 0.5533 0.1464 0.1272 0.050 Uiso 1 1 calc R . . C15 C 0.6156(3) 0.1763(3) 0.1100(3) 0.042(2) Uani 1 1 d . . . C16 C 0.6199(3) 0.2153(3) 0.1104(4) 0.059(3) Uani 1 1 d . . . C17 C 0.6592(4) 0.2500(3) 0.1100(5) 0.072(3) Uani 1 1 d . . . C18 C 0.6939(3) 0.2463(3) 0.1116(4) 0.061(3) Uani 1 1 d . . . C19 C 0.6910(3) 0.2076(3) 0.1118(4) 0.051(3) Uani 1 1 d . . . C20 C 0.6512(3) 0.1740(3) 0.1117(3) 0.043(2) Uani 1 1 d . . . H20A H 0.6483 0.1471 0.1128 0.052 Uiso 1 1 calc R . . C21 C 0.7287(3) 0.2026(3) 0.1116(4) 0.057(3) Uani 1 1 d . . . H21A H 0.7513 0.2279 0.1289 0.069 Uiso 1 1 calc R . . C22 C 0.7438(3) 0.2029(3) 0.0563(4) 0.050(3) Uani 1 1 d . . . C23 C 0.7724(3) 0.2384(3) 0.0324(6) 0.059(3) Uani 1 1 d . . . C24 C 0.7846(3) 0.2379(3) -0.0179(6) 0.069(3) Uani 1 1 d . . . C25 C 0.7688(3) 0.2006(3) -0.0449(5) 0.059(3) Uani 1 1 d . . . C26 C 0.7391(3) 0.1637(3) -0.0214(4) 0.049(3) Uani 1 1 d . . . C27 C 0.7273(3) 0.1660(3) 0.0289(4) 0.046(3) Uani 1 1 d . . . H27A H 0.7072 0.1411 0.0452 0.056 Uiso 1 1 calc R . . C28 C 0.7219(3) 0.1226(3) -0.0507(4) 0.051(3) Uani 1 1 d . . . H28A H 0.7423 0.1268 -0.0785 0.061 Uiso 1 1 calc R . . C29 C 0.5643(3) 0.0213(3) -0.0142(4) 0.044(2) Uani 1 1 d . . . H29A H 0.5867 0.0348 0.0117 0.053 Uiso 1 1 calc R . . H29B H 0.5376 0.0069 0.0047 0.053 Uiso 1 1 calc R . . C30 C 0.5702(3) -0.0108(3) -0.0438(4) 0.050(3) Uani 1 1 d . . . H30A H 0.5434 -0.0312 -0.0596 0.060 Uiso 1 1 calc R . . H30B H 0.5903 0.0033 -0.0720 0.060 Uiso 1 1 calc R . . C31 C 0.5855(3) -0.0340(3) -0.0101(4) 0.052(3) Uani 1 1 d . . . H31A H 0.6114 -0.0136 0.0074 0.063 Uiso 1 1 calc R . . H31B H 0.5646 -0.0496 0.0168 0.063 Uiso 1 1 calc R . . C32 C 0.5938(3) -0.0639(3) -0.0404(4) 0.057(3) Uani 1 1 d . . . H32A H 0.6121 -0.0492 -0.0701 0.069 Uiso 1 1 calc R . . H32B H 0.5673 -0.0866 -0.0542 0.069 Uiso 1 1 calc R . . C33 C 0.6142(3) -0.0821(3) -0.0067(4) 0.061(3) Uani 1 1 d . . . H33A H 0.6392 -0.0590 0.0095 0.074 Uiso 1 1 calc R . . H33B H 0.5948 -0.0983 0.0214 0.074 Uiso 1 1 calc R . . C34 C 0.6265(3) -0.1092(3) -0.0339(4) 0.062(3) Uani 1 1 d . . . H34A H 0.6430 -0.0943 -0.0647 0.075 Uiso 1 1 calc R . . H34B H 0.6012 -0.1343 -0.0461 0.075 Uiso 1 1 calc R . . C35 C 0.6524(4) -0.1231(3) -0.0007(5) 0.076(3) Uani 1 1 d . . . H35A H 0.6777 -0.0980 0.0115 0.092 Uiso 1 1 calc R . . H35B H 0.6359 -0.1379 0.0302 0.092 Uiso 1 1 calc R . . C36 C 0.6652(4) -0.1509(4) -0.0280(5) 0.089(4) Uani 1 1 d . . . H36A H 0.6399 -0.1771 -0.0378 0.106 Uiso 1 1 calc R . . H36B H 0.6801 -0.1371 -0.0601 0.106 Uiso 1 1 calc R . . C37 C 0.6921(4) -0.1611(3) 0.0038(6) 0.100(5) Uani 1 1 d . . . H37A H 0.6937 -0.1843 -0.0127 0.120 Uiso 1 1 calc R . . H37B H 0.6792 -0.1707 0.0382 0.120 Uiso 1 1 calc R . . C38 C 0.7353(4) -0.1253(4) 0.0108(8) 0.146(8) Uani 1 1 d . . . H38A H 0.7513 -0.1339 0.0323 0.219 Uiso 1 1 calc R . . H38B H 0.7341 -0.1023 0.0276 0.219 Uiso 1 1 calc R . . H38C H 0.7487 -0.1161 -0.0230 0.219 Uiso 1 1 calc R . . C39 C 0.5711(2) 0.1033(2) 0.1471(4) 0.055(3) Uani 1 1 d D . . H39A H 0.5909 0.0952 0.1337 0.066 Uiso 1 1 calc R . . H39B H 0.5805 0.1151 0.1821 0.066 Uiso 1 1 calc R . . C40 C 0.5291(2) 0.0651(3) 0.1515(4) 0.073(3) Uani 1 1 d D . . H40A H 0.5215 0.0537 0.1161 0.087 Uiso 1 1 calc R . . H40B H 0.5332 0.0449 0.1716 0.087 Uiso 1 1 calc R . . C41 C 0.4912(4) 0.0635(4) 0.1733(8) 0.45(3) Uani 1 1 d D . . H41A H 0.4770 0.0716 0.1474 0.539 Uiso 1 1 calc R . . H41B H 0.4979 0.0815 0.2041 0.539 Uiso 1 1 calc R . . C42 C 0.4656(7) 0.0183(5) 0.1874(8) 0.45(3) Uani 1 1 d D . . H42A H 0.4627 -0.0007 0.1588 0.539 Uiso 1 1 calc R . . H42B H 0.4750 0.0109 0.2193 0.539 Uiso 1 1 calc R . . C43 C 0.4280(5) 0.0225(5) 0.1949(6) 0.305(17) Uani 1 1 d D . . H43A H 0.4294 0.0418 0.1677 0.366 Uiso 1 1 calc R . . H43B H 0.4324 0.0374 0.2280 0.366 Uiso 1 1 calc R . . C44 C 0.3838(5) -0.0121(5) 0.1959(7) 0.305(17) Uani 1 1 d D . . H44A H 0.3837 -0.0308 0.2230 0.366 Uiso 1 1 calc R . . H44B H 0.3808 -0.0267 0.1629 0.366 Uiso 1 1 calc R . . C45 C 0.3424(4) -0.0147(5) 0.2024(6) 0.278(15) Uani 1 1 d D . . H45A H 0.3430 0.0037 0.1745 0.333 Uiso 1 1 calc R . . H45B H 0.3466 0.0013 0.2345 0.333 Uiso 1 1 calc R . . C46 C 0.2969(4) -0.0463(6) 0.2054(6) 0.278(15) Uani 1 1 d D . . H46A H 0.2982 -0.0614 0.2362 0.333 Uiso 1 1 calc R . . H46B H 0.2960 -0.0640 0.1762 0.333 Uiso 1 1 calc R . . C47 C 0.2512(4) -0.0610(7) 0.2075(6) 0.158(9) Uani 1 1 d D . . H47A H 0.2339 -0.0911 0.2007 0.189 Uiso 1 1 calc R . . H47B H 0.2429 -0.0539 0.2406 0.189 Uiso 1 1 calc R . . C48 C 0.2505(15) -0.0352(11) 0.1635(11) 1.12(15) Uani 1 1 d D . . H48A H 0.2224 -0.0395 0.1595 1.673 Uiso 1 1 calc R . . H48B H 0.2587 -0.0434 0.1316 1.673 Uiso 1 1 calc R . . H48C H 0.2699 -0.0058 0.1705 1.673 Uiso 1 1 calc R . . C49 C 0.7227(3) 0.1656(3) 0.1438(4) 0.057(3) Uani 1 1 d . . . H49A H 0.7000 0.1399 0.1285 0.068 Uiso 1 1 calc R . . H49B H 0.7140 0.1683 0.1790 0.068 Uiso 1 1 calc R . . C50 C 0.7614(3) 0.1611(3) 0.1480(5) 0.078(4) Uani 1 1 d . . . H50A H 0.7787 0.1733 0.1169 0.093 Uiso 1 1 calc R . . H50B H 0.7779 0.1772 0.1782 0.093 Uiso 1 1 calc R . . C51 C 0.7520(4) 0.1160(3) 0.1537(5) 0.080(4) Uani 1 1 d . . . H51A H 0.7378 0.1053 0.1872 0.096 Uiso 1 1 calc R . . H51B H 0.7322 0.0993 0.1263 0.096 Uiso 1 1 calc R . . C52 C 0.7870(4) 0.1084(4) 0.1515(5) 0.087(4) Uani 1 1 d . . . H52A H 0.8048 0.1215 0.1821 0.104 Uiso 1 1 calc R . . H52B H 0.8037 0.1225 0.1205 0.104 Uiso 1 1 calc R . . C53 C 0.7760(4) 0.0644(4) 0.1499(5) 0.086(4) Uani 1 1 d . . . H53A H 0.7580 0.0515 0.1193 0.104 Uiso 1 1 calc R . . H53B H 0.7590 0.0505 0.1808 0.104 Uiso 1 1 calc R . . C54 C 0.8102(5) 0.0546(5) 0.1477(8) 0.126(6) Uani 1 1 d . . . H54A H 0.8352 0.0808 0.1374 0.151 Uiso 1 1 calc R . . H54B H 0.8149 0.0494 0.1838 0.151 Uiso 1 1 calc R . . C55 C 0.8109(9) 0.0300(13) 0.1245(11) 0.38(3) Uani 1 1 d . . . H55A H 0.8042 0.0348 0.0891 0.451 Uiso 1 1 calc R . . H55B H 0.7862 0.0042 0.1364 0.451 Uiso 1 1 calc R . . C56 C 0.8442(11) 0.0171(12) 0.1163(13) 0.34(3) Uani 1 1 d . . . H56A H 0.8644 0.0360 0.0905 0.407 Uiso 1 1 calc R . . H56B H 0.8593 0.0212 0.1491 0.407 Uiso 1 1 calc R . . C57 C 0.8317(11) -0.0176(14) 0.1023(9) 0.29(2) Uani 1 1 d . . . H57A H 0.8152 -0.0216 0.0707 0.344 Uiso 1 1 calc R . . H57B H 0.8120 -0.0360 0.1290 0.344 Uiso 1 1 calc R . . C58 C 0.8597(9) -0.0337(8) 0.0910(8) 0.185(10) Uani 1 1 d . . . H58A H 0.8434 -0.0636 0.0843 0.277 Uiso 1 1 calc R . . H58B H 0.8780 -0.0287 0.1207 0.277 Uiso 1 1 calc R . . H58C H 0.8765 -0.0196 0.0606 0.277 Uiso 1 1 calc R . . C59 C 0.7180(3) 0.0873(3) -0.0164(5) 0.080(4) Uani 1 1 d . . . H59A H 0.7441 0.0969 0.0031 0.096 Uiso 1 1 calc R . . H59B H 0.6953 0.0794 0.0088 0.096 Uiso 1 1 calc R . . C60 C 0.7094(6) 0.0503(5) -0.0485(7) 0.173(10) Uani 1 1 d . . . H60A H 0.7269 0.0598 -0.0799 0.208 Uiso 1 1 calc R . . H60B H 0.6800 0.0359 -0.0595 0.208 Uiso 1 1 calc R . . C61 C 0.7183(6) 0.0192(6) -0.0184(11) 0.246(16) Uani 1 1 d . . . H61A H 0.7254 0.0284 0.0179 0.296 Uiso 1 1 calc R . . H61B H 0.6932 -0.0087 -0.0185 0.296 Uiso 1 1 calc R . . C62 C 0.7504(7) 0.0171(8) -0.0410(11) 0.280(19) Uani 1 1 d . . . H62A H 0.7379 0.0050 -0.0748 0.336 Uiso 1 1 calc R . . H62B H 0.7694 0.0469 -0.0485 0.336 Uiso 1 1 calc R . . C63 C 0.7757(5) 0.0047(7) -0.0367(6) 0.164(9) Uani 1 1 d . . . H63A H 0.7552 -0.0239 -0.0260 0.197 Uiso 1 1 calc R . . H63B H 0.7878 0.0189 -0.0035 0.197 Uiso 1 1 calc R . . C64 C 0.8045(6) -0.0028(7) -0.0478(7) 0.161(9) Uani 1 1 d . . . H64A H 0.7892 -0.0197 -0.0782 0.193 Uiso 1 1 calc R . . H64B H 0.8220 0.0252 -0.0627 0.193 Uiso 1 1 calc R . . C65 C 0.8328(5) -0.0117(7) -0.0531(6) 0.153(8) Uani 1 1 d . . . H65A H 0.8151 -0.0380 -0.0717 0.184 Uiso 1 1 calc R . . H65B H 0.8315 -0.0208 -0.0169 0.184 Uiso 1 1 calc R . . C66 C 0.8672(6) -0.0107(8) -0.0635(7) 0.181(10) Uani 1 1 d . . . H66A H 0.8710 0.0010 -0.0987 0.218 Uiso 1 1 calc R . . H66B H 0.8855 0.0137 -0.0420 0.218 Uiso 1 1 calc R . . C67 C 0.8924(7) -0.0258(9) -0.0681(9) 0.231(14) Uani 1 1 d . . . H67A H 0.8758 -0.0487 -0.0925 0.278 Uiso 1 1 calc R . . H67B H 0.8872 -0.0399 -0.0342 0.278 Uiso 1 1 calc R . . C68 C 0.9299(7) -0.0213(10) -0.0778(9) 0.277(18) Uani 1 1 d . . . H68A H 0.9287 -0.0480 -0.0733 0.416 Uiso 1 1 calc R . . H68B H 0.9503 -0.0009 -0.0539 0.416 Uiso 1 1 calc R . . H68C H 0.9380 -0.0116 -0.1133 0.416 Uiso 1 1 calc R . . C1S C 0.7335(7) 0.2550(7) -0.1870(9) 0.427(9) Uiso 1 1 d G . . C2S C 0.7308(10) 0.2626(10) -0.1361(8) 0.427(9) Uiso 1 1 d G . . H2SA H 0.7145 0.2362 -0.1178 0.640 Uiso 1 1 calc R . . H2SB H 0.7171 0.2792 -0.1327 0.640 Uiso 1 1 calc R . . H2SC H 0.7587 0.2778 -0.1212 0.640 Uiso 1 1 calc R . . C3S C 0.7677(7) 0.2962(7) -0.2805(8) 0.427(9) Uiso 1 1 d G . . H3SA H 0.7763 0.2753 -0.2868 0.512 Uiso 1 1 calc R . . H3SB H 0.7407 0.2860 -0.2980 0.512 Uiso 1 1 calc R . . C4S C 0.7929(8) 0.3280(9) -0.3036(9) 0.427(9) Uiso 1 1 d G . . H4SA H 0.7934 0.3216 -0.3402 0.640 Uiso 1 1 calc R . . H4SB H 0.8206 0.3384 -0.2888 0.640 Uiso 1 1 calc R . . H4SC H 0.7847 0.3492 -0.3001 0.640 Uiso 1 1 calc R . . O1S O 0.7094(8) 0.2282(6) -0.2148(11) 0.427(9) Uiso 1 1 d G . . O2S O 0.7602(6) 0.2953(6) -0.2289(8) 0.427(9) Uiso 1 1 d G . . N1S N 0.755(2) 0.329(2) -0.030(3) 0.427(9) Uiso 0.50 1 d PG A -1 C5S C 0.704(3) 0.323(3) -0.027(3) 0.427(9) Uiso 0.50 1 d PG A -1 C6S C 0.675(3) 0.310(3) -0.043(2) 0.427(9) Uiso 0.50 1 d PG A -1 H6SA H 0.6577 0.3183 -0.0241 0.640 Uiso 0.50 1 d PR A -1 H6SB H 0.6765 0.3182 -0.0782 0.640 Uiso 0.50 1 d PR A -1 H6SC H 0.6621 0.2802 -0.0410 0.640 Uiso 0.50 1 d PR 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 0.059(5) 0.061(5) 0.077(5) 0.005(4) 0.028(4) -0.001(4) O2 0.100(7) 0.116(7) 0.056(6) 0.028(5) -0.008(5) -0.021(5) O3 0.064(5) 0.100(6) 0.074(6) 0.022(5) -0.038(4) 0.009(4) O4 0.082(5) 0.054(4) 0.058(5) 0.006(4) -0.021(4) 0.021(4) O5 0.077(5) 0.086(5) 0.098(6) 0.024(5) -0.030(4) 0.050(5) O6 0.057(4) 0.049(4) 0.096(6) -0.003(4) -0.010(4) 0.038(4) O7 0.099(6) 0.082(5) 0.125(7) -0.035(5) -0.037(5) 0.079(5) O8 0.136(8) 0.048(5) 0.187(10) -0.034(5) -0.069(7) 0.060(5) O9 0.085(6) 0.030(4) 0.140(8) 0.007(4) -0.054(5) 0.002(4) O10 0.072(5) 0.038(4) 0.148(8) 0.017(5) -0.050(5) 0.012(4) O11 0.046(5) 0.084(6) 0.151(8) 0.080(6) -0.023(5) -0.016(4) O12 0.048(5) 0.117(7) 0.080(6) 0.051(5) 0.009(4) 0.025(5) C1 0.052(6) 0.023(5) 0.051(6) 0.000(4) 0.005(5) 0.022(5) C2 0.050(7) 0.042(6) 0.051(7) -0.001(5) 0.015(6) 0.007(5) C3 0.054(7) 0.070(7) 0.026(6) 0.010(5) -0.006(5) 0.000(6) C4 0.057(7) 0.061(7) 0.053(7) 0.005(6) -0.007(6) 0.018(6) C5 0.046(6) 0.026(5) 0.051(7) -0.006(4) -0.005(5) 0.012(4) C6 0.045(6) 0.030(5) 0.050(6) 0.003(4) 0.005(5) 0.024(5) C7 0.035(5) 0.027(5) 0.043(6) -0.004(4) -0.006(4) 0.005(4) C8 0.026(5) 0.026(5) 0.058(7) 0.000(5) -0.003(5) 0.005(4) C9 0.034(5) 0.034(5) 0.056(7) -0.002(5) -0.010(5) 0.012(4) C10 0.048(6) 0.054(6) 0.067(8) 0.000(6) -0.027(6) 0.031(5) C11 0.044(6) 0.040(6) 0.062(7) 0.002(5) -0.009(5) 0.024(5) C12 0.030(5) 0.033(5) 0.060(7) 0.002(5) -0.007(5) 0.016(4) C13 0.034(5) 0.043(5) 0.048(6) 0.001(5) -0.006(5) 0.021(4) C14 0.046(6) 0.047(6) 0.049(6) -0.001(5) -0.001(5) 0.036(5) C15 0.055(6) 0.032(5) 0.050(6) -0.008(4) -0.013(5) 0.030(5) C16 0.061(7) 0.060(7) 0.075(8) -0.019(6) -0.032(6) 0.044(6) C17 0.079(8) 0.037(6) 0.108(10) -0.019(6) -0.039(7) 0.035(6) C18 0.055(7) 0.042(6) 0.088(8) -0.004(6) -0.034(6) 0.025(5) C19 0.055(6) 0.032(5) 0.075(7) -0.007(5) -0.017(5) 0.028(5) C20 0.048(6) 0.030(5) 0.054(6) -0.002(4) -0.008(5) 0.021(5) C21 0.047(6) 0.019(5) 0.097(9) -0.005(5) -0.028(6) 0.010(4) C22 0.030(5) 0.041(6) 0.074(8) 0.016(6) -0.009(5) 0.015(5) C23 0.028(5) 0.026(6) 0.115(11) 0.012(7) -0.024(6) 0.007(5) C24 0.033(6) 0.048(7) 0.097(10) 0.033(7) -0.014(7) -0.001(5) C25 0.041(6) 0.060(8) 0.067(8) 0.030(7) -0.004(6) 0.019(6) C26 0.021(5) 0.043(6) 0.079(8) 0.022(6) -0.001(5) 0.013(5) C27 0.028(5) 0.036(6) 0.069(8) 0.019(5) -0.002(5) 0.012(4) C28 0.044(6) 0.045(6) 0.081(7) 0.024(5) 0.019(5) 0.035(5) C29 0.033(5) 0.036(5) 0.064(7) 0.002(5) -0.001(5) 0.018(4) C30 0.048(6) 0.031(5) 0.059(7) 0.006(5) 0.001(5) 0.010(5) C31 0.058(6) 0.030(5) 0.060(7) 0.013(5) 0.007(5) 0.016(5) C32 0.086(8) 0.028(5) 0.054(7) 0.001(5) 0.002(6) 0.026(5) C33 0.060(7) 0.055(6) 0.072(8) 0.007(6) 0.009(6) 0.032(6) C34 0.056(6) 0.055(7) 0.076(8) 0.015(6) 0.001(6) 0.028(6) C35 0.086(8) 0.056(7) 0.093(9) 0.012(6) 0.010(7) 0.040(7) C36 0.084(9) 0.073(8) 0.119(11) 0.040(8) 0.023(8) 0.047(7) C37 0.063(8) 0.051(7) 0.182(15) 0.014(8) -0.017(9) 0.026(7) C38 0.070(9) 0.074(10) 0.30(2) -0.015(12) -0.020(12) 0.038(8) C39 0.053(6) 0.054(6) 0.062(7) -0.008(5) -0.006(5) 0.030(5) C40 0.040(6) 0.075(8) 0.072(8) 0.005(6) 0.011(6) 0.005(6) C41 0.38(3) 0.24(2) 0.208(18) -0.137(16) 0.21(2) -0.24(2) C42 0.38(3) 0.24(2) 0.208(18) -0.137(16) 0.21(2) -0.24(2) C43 0.40(3) 0.097(10) 0.080(9) -0.010(7) 0.107(13) -0.125(13) C44 0.40(3) 0.097(10) 0.080(9) -0.010(7) 0.107(13) -0.125(13) C45 0.50(4) 0.091(11) 0.031(6) 0.027(8) 0.001(14) -0.006(15) C46 0.50(4) 0.091(11) 0.031(6) 0.027(8) 0.001(14) -0.006(15) C47 0.061(9) 0.31(3) 0.106(13) 0.037(15) 0.027(9) 0.099(14) C48 1.6(2) 0.34(6) 0.31(6) -0.12(5) 0.58(11) -0.33(10) C49 0.051(6) 0.040(6) 0.077(8) 0.007(5) -0.015(5) 0.021(5) C50 0.041(6) 0.075(8) 0.114(10) 0.015(7) -0.024(6) 0.026(6) C51 0.080(8) 0.066(8) 0.106(10) 0.021(7) -0.007(7) 0.047(7) C52 0.078(9) 0.093(10) 0.101(10) -0.003(8) 0.001(7) 0.051(8) C53 0.092(9) 0.089(9) 0.099(10) -0.006(8) -0.021(8) 0.061(8) C54 0.115(12) 0.140(14) 0.160(16) -0.058(12) -0.032(12) 0.093(11) C55 0.31(4) 0.71(8) 0.32(4) -0.38(5) -0.22(3) 0.42(5) C56 0.27(4) 0.49(6) 0.35(5) -0.35(5) -0.15(3) 0.26(4) C57 0.30(4) 0.53(7) 0.072(15) 0.06(3) 0.06(2) 0.24(5) C58 0.26(3) 0.26(3) 0.107(16) -0.007(16) 0.011(16) 0.18(2) C59 0.055(7) 0.066(7) 0.134(11) 0.050(8) 0.034(7) 0.042(6) C60 0.31(2) 0.122(12) 0.188(17) 0.099(12) 0.185(17) 0.185(16) C61 0.168(17) 0.153(16) 0.50(4) 0.21(2) 0.19(2) 0.139(16) C62 0.23(2) 0.36(3) 0.40(4) -0.30(3) -0.20(3) 0.25(3) C63 0.146(15) 0.32(3) 0.127(14) 0.101(15) 0.056(12) 0.195(19) C64 0.21(2) 0.27(2) 0.131(15) -0.071(15) -0.052(14) 0.22(2) C65 0.111(12) 0.31(3) 0.085(11) -0.073(13) -0.034(9) 0.137(16) C66 0.187(19) 0.36(3) 0.120(14) 0.084(17) 0.037(13) 0.23(2) C67 0.156(19) 0.38(4) 0.22(3) -0.13(3) -0.027(18) 0.18(2) C68 0.23(2) 0.51(5) 0.26(3) 0.23(3) 0.15(2) 0.31(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 C2 1.377(11) . ? O1 H1 0.8400 . ? O2 C3 1.358(12) . ? O2 H2 0.8400 . ? O3 C4 1.362(11) . ? O3 H3 0.8400 . ? O4 C9 1.358(11) . ? O4 H4 0.8400 . ? O5 C10 1.360(10) . ? O5 H5 0.8400 . ? O6 C11 1.375(10) . ? O6 H6 0.8400 . ? O7 C16 1.373(11) . ? O7 H7 0.8400 . ? O8 C17 1.400(11) . ? O8 H8 0.8400 . ? O9 C18 1.390(11) . ? O9 H9 0.8400 . ? O10 C23 1.373(12) . ? O10 H10 0.8400 . ? O11 C24 1.366(12) . ? O11 H11 0.8400 . ? O12 C25 1.341(12) . ? O12 H12 0.8400 . ? C1 C6 1.376(12) . ? C1 C2 1.378(13) . ? C1 C28 1.514(12) . ? C2 C3 1.397(14) . ? C3 C4 1.366(13) . ? C4 C5 1.432(13) . ? C5 C6 1.375(12) . ? C5 C7 1.525(12) . ? C6 H6A 0.9500 . ? C7 C8 1.532(12) . ? C7 C29 1.534(11) . ? C7 H7A 1.0000 . ? C8 C13 1.387(12) . ? C8 C9 1.403(12) . ? C9 C10 1.395(13) . ? C10 C11 1.361(13) . ? C11 C12 1.412(12) . ? C12 C13 1.377(12) . ? C12 C14 1.510(12) . ? C13 H13A 0.9500 . ? C14 C15 1.531(12) . ? C14 C39 1.557(12) . ? C14 H14A 1.0000 . ? C15 C20 1.368(11) . ? C15 C16 1.381(12) . ? C16 C17 1.385(14) . ? C17 C18 1.368(14) . ? C18 C19 1.387(12) . ? C19 C20 1.381(12) . ? C19 C21 1.505(12) . ? C20 H20A 0.9500 . ? C21 C49 1.530(12) . ? C21 C22 1.536(14) . ? C21 H21A 1.0000 . ? C22 C23 1.363(13) . ? C22 C27 1.389(13) . ? C23 C24 1.384(16) . ? C24 C25 1.394(16) . ? C25 C26 1.401(13) . ? C26 C27 1.390(13) . ? C26 C28 1.533(13) . ? C27 H27A 0.9500 . ? C28 C59 1.532(12) . ? C28 H28A 1.0000 . ? C29 C30 1.525(12) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.525(12) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.514(12) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.521(13) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.480(13) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.558(14) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.515(15) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.487(16) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.499(16) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.501(5) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.489(5) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.506(5) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.498(5) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.498(5) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.502(5) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.504(5) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.507(5) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.500(5) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.535(13) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.538(14) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.464(14) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.479(16) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.489(17) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.11(2) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.55(4) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.19(5) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.47(4) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 C60 1.498(19) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.56(2) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.36(2) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.244(19) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.271(18) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.256(18) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.291(19) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C67 1.32(2) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C68 1.34(2) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C1S O1S 1.1931 . ? C1S C2S 1.3639 . ? C1S O2S 1.7100 . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? C3S C4S 1.2356 . ? C3S O2S 1.3635 . ? C3S H3SA 0.9900 . ? C3S H3SB 0.9900 . ? C4S H4SA 0.9800 . ? C4S H4SB 0.9800 . ? C4S H4SC 0.9800 . ? N1S C5S 1.8185 . ? C5S C6S 1.0239 . ? C6S H6SA 0.9596 . ? C6S H6SB 0.9601 . ? C6S H6SC 0.9601 . ? 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 O1 H1 109.5 . . ? C3 O2 H2 109.5 . . ? C4 O3 H3 109.5 . . ? C9 O4 H4 109.5 . . ? C10 O5 H5 109.5 . . ? C11 O6 H6 109.5 . . ? C16 O7 H7 109.5 . . ? C17 O8 H8 109.5 . . ? C18 O9 H9 109.5 . . ? C23 O10 H10 109.5 . . ? C24 O11 H11 109.5 . . ? C25 O12 H12 109.5 . . ? C6 C1 C2 117.6(9) . . ? C6 C1 C28 121.9(8) . . ? C2 C1 C28 120.4(9) . . ? O1 C2 C1 121.9(10) . . ? O1 C2 C3 117.3(9) . . ? C1 C2 C3 120.8(9) . . ? C4 C3 O2 120.4(10) . . ? C4 C3 C2 120.7(9) . . ? O2 C3 C2 118.8(9) . . ? C3 C4 O3 119.3(9) . . ? C3 C4 C5 119.8(10) . . ? O3 C4 C5 121.0(9) . . ? C6 C5 C4 116.9(9) . . ? C6 C5 C7 124.2(8) . . ? C4 C5 C7 119.0(8) . . ? C1 C6 C5 124.2(9) . . ? C1 C6 H6A 117.9 . . ? C5 C6 H6A 117.9 . . ? C5 C7 C8 110.6(6) . . ? C5 C7 C29 111.2(7) . . ? C8 C7 C29 112.1(7) . . ? C5 C7 H7A 107.6 . . ? C8 C7 H7A 107.6 . . ? C29 C7 H7A 107.6 . . ? C13 C8 C9 118.0(8) . . ? C13 C8 C7 122.6(8) . . ? C9 C8 C7 119.3(8) . . ? O4 C9 C10 118.1(8) . . ? O4 C9 C8 122.8(9) . . ? C10 C9 C8 119.1(9) . . ? C11 C10 O5 118.9(9) . . ? C11 C10 C9 121.4(8) . . ? O5 C10 C9 119.7(9) . . ? C10 C11 O6 119.2(8) . . ? C10 C11 C12 120.9(9) . . ? O6 C11 C12 119.9(9) . . ? C13 C12 C11 116.7(9) . . ? C13 C12 C14 122.8(8) . . ? C11 C12 C14 120.5(8) . . ? C12 C13 C8 123.9(8) . . ? C12 C13 H13A 118.1 . . ? C8 C13 H13A 118.1 . . ? C12 C14 C15 110.6(7) . . ? C12 C14 C39 113.6(7) . . ? C15 C14 C39 111.8(7) . . ? C12 C14 H14A 106.8 . . ? C15 C14 H14A 106.8 . . ? C39 C14 H14A 106.8 . . ? C20 C15 C16 117.4(8) . . ? C20 C15 C14 122.5(7) . . ? C16 C15 C14 120.0(8) . . ? O7 C16 C17 118.6(9) . . ? O7 C16 C15 121.8(9) . . ? C17 C16 C15 119.5(9) . . ? C18 C17 C16 121.2(9) . . ? C18 C17 O8 119.3(10) . . ? C16 C17 O8 119.5(10) . . ? C17 C18 C19 121.0(9) . . ? C17 C18 O9 117.6(9) . . ? C19 C18 O9 121.3(9) . . ? C20 C19 C18 115.7(8) . . ? C20 C19 C21 122.1(8) . . ? C18 C19 C21 122.2(8) . . ? C15 C20 C19 125.1(8) . . ? C15 C20 H20A 117.4 . . ? C19 C20 H20A 117.4 . . ? C19 C21 C49 112.6(8) . . ? C19 C21 C22 111.2(8) . . ? C49 C21 C22 113.8(8) . . ? C19 C21 H21A 106.2 . . ? C49 C21 H21A 106.2 . . ? C22 C21 H21A 106.2 . . ? C23 C22 C27 118.0(11) . . ? C23 C22 C21 122.5(10) . . ? C27 C22 C21 119.5(8) . . ? C22 C23 O10 122.0(13) . . ? C22 C23 C24 121.3(10) . . ? O10 C23 C24 116.7(10) . . ? O11 C24 C23 122.7(12) . . ? O11 C24 C25 116.8(13) . . ? C23 C24 C25 120.4(10) . . ? O12 C25 C24 117.3(10) . . ? O12 C25 C26 123.2(11) . . ? C24 C25 C26 119.5(11) . . ? C27 C26 C25 117.8(10) . . ? C27 C26 C28 122.6(8) . . ? C25 C26 C28 119.6(10) . . ? C22 C27 C26 123.0(9) . . ? C22 C27 H27A 118.5 . . ? C26 C27 H27A 118.5 . . ? C1 C28 C59 113.5(8) . . ? C1 C28 C26 109.6(6) . . ? C59 C28 C26 112.3(9) . . ? C1 C28 H28A 107.0 . . ? C59 C28 H28A 107.0 . . ? C26 C28 H28A 107.0 . . ? C30 C29 C7 113.5(8) . . ? C30 C29 H29A 108.9 . . ? C7 C29 H29A 108.9 . . ? C30 C29 H29B 108.9 . . ? C7 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? C31 C30 C29 113.3(8) . . ? C31 C30 H30A 108.9 . . ? C29 C30 H30A 108.9 . . ? C31 C30 H30B 108.9 . . ? C29 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? C32 C31 C30 112.9(8) . . ? C32 C31 H31A 109.0 . . ? C30 C31 H31A 109.0 . . ? C32 C31 H31B 109.0 . . ? C30 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? C31 C32 C33 111.0(8) . . ? C31 C32 H32A 109.4 . . ? C33 C32 H32A 109.4 . . ? C31 C32 H32B 109.4 . . ? C33 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? C34 C33 C32 115.0(9) . . ? C34 C33 H33A 108.5 . . ? C32 C33 H33A 108.5 . . ? C34 C33 H33B 108.5 . . ? C32 C33 H33B 108.5 . . ? H33A C33 H33B 107.5 . . ? C33 C34 C35 114.5(9) . . ? C33 C34 H34A 108.6 . . ? C35 C34 H34A 108.6 . . ? C33 C34 H34B 108.6 . . ? C35 C34 H34B 108.6 . . ? H34A C34 H34B 107.6 . . ? C36 C35 C34 115.2(10) . . ? C36 C35 H35A 108.5 . . ? C34 C35 H35A 108.5 . . ? C36 C35 H35B 108.5 . . ? C34 C35 H35B 108.5 . . ? H35A C35 H35B 107.5 . . ? C37 C36 C35 113.5(12) . . ? C37 C36 H36A 108.9 . . ? C35 C36 H36A 108.9 . . ? C37 C36 H36B 108.9 . . ? C35 C36 H36B 108.9 . . ? H36A C36 H36B 107.7 . . ? C36 C37 C38 113.5(11) . . ? C36 C37 H37A 108.9 . . ? C38 C37 H37A 108.8 . . ? C36 C37 H37B 108.9 . . ? C38 C37 H37B 108.9 . . ? H37A C37 H37B 107.7 . . ? C37 C38 H38A 109.4 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 C14 114.3(8) . . ? C40 C39 H39A 108.7 . . ? C14 C39 H39A 108.7 . . ? C40 C39 H39B 108.7 . . ? C14 C39 H39B 108.7 . . ? H39A C39 H39B 107.6 . . ? C41 C40 C39 125.6(10) . . ? C41 C40 H40A 105.9 . . ? C39 C40 H40A 105.9 . . ? C41 C40 H40B 105.9 . . ? C39 C40 H40B 105.9 . . ? H40A C40 H40B 106.2 . . ? C40 C41 C42 101.3(12) . . ? C40 C41 H41A 111.6 . . ? C42 C41 H41A 111.5 . . ? C40 C41 H41B 111.5 . . ? C42 C41 H41B 111.5 . . ? H41A C41 H41B 109.3 . . ? C43 C42 C41 91.0(11) . . ? C43 C42 H42A 113.5 . . ? C41 C42 H42A 113.4 . . ? C43 C42 H42B 113.5 . . ? C41 C42 H42B 113.5 . . ? H42A C42 H42B 110.8 . . ? C42 C43 C44 126.4(17) . . ? C42 C43 H43A 105.7 . . ? C44 C43 H43A 105.7 . . ? C42 C43 H43B 105.7 . . ? C44 C43 H43B 105.7 . . ? H43A C43 H43B 106.1 . . ? C43 C44 C45 135.1(18) . . ? C43 C44 H44A 103.4 . . ? C45 C44 H44A 103.4 . . ? C43 C44 H44B 103.4 . . ? C45 C44 H44B 103.4 . . ? H44A C44 H44B 105.2 . . ? C44 C45 C46 140.7(16) . . ? C44 C45 H45A 101.8 . . ? C46 C45 H45A 101.8 . . ? C44 C45 H45B 101.9 . . ? C46 C45 H45B 101.9 . . ? H45A C45 H45B 104.7 . . ? C45 C46 C47 156(2) . . ? C45 C46 H46A 97.5 . . ? C47 C46 H46A 97.5 . . ? C45 C46 H46B 97.5 . . ? C47 C46 H46B 97.5 . . ? H46A C46 H46B 103.6 . . ? C48 C47 C46 97(2) . . ? C48 C47 H47A 112.4 . . ? C46 C47 H47A 112.4 . . ? C48 C47 H47B 112.4 . . ? C46 C47 H47B 112.4 . . ? H47A C47 H47B 109.9 . . ? C47 C48 H48A 109.3 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C21 C49 C50 114.6(8) . . ? C21 C49 H49A 108.6 . . ? C50 C49 H49A 108.6 . . ? C21 C49 H49B 108.6 . . ? C50 C49 H49B 108.6 . . ? H49A C49 H49B 107.6 . . ? C51 C50 C49 114.4(9) . . ? C51 C50 H50A 108.7 . . ? C49 C50 H50A 108.7 . . ? C51 C50 H50B 108.7 . . ? C49 C50 H50B 108.7 . . ? H50A C50 H50B 107.6 . . ? C52 C51 C50 117.8(10) . . ? C52 C51 H51A 107.9 . . ? C50 C51 H51A 107.8 . . ? C52 C51 H51B 107.8 . . ? C50 C51 H51B 107.8 . . ? H51A C51 H51B 107.2 . . ? C51 C52 C53 115.8(11) . . ? C51 C52 H52A 108.3 . . ? C53 C52 H52A 108.3 . . ? C51 C52 H52B 108.4 . . ? C53 C52 H52B 108.3 . . ? H52A C52 H52B 107.4 . . ? C52 C53 C54 118.3(12) . . ? C52 C53 H53A 107.7 . . ? C54 C53 H53A 107.7 . . ? C52 C53 H53B 107.7 . . ? C54 C53 H53B 107.8 . . ? H53A C53 H53B 107.1 . . ? C55 C54 C53 126.9(19) . . ? C55 C54 H54A 105.6 . . ? C53 C54 H54A 105.6 . . ? C55 C54 H54B 105.6 . . ? C53 C54 H54B 105.6 . . ? H54A C54 H54B 106.1 . . ? C54 C55 C56 133(2) . . ? C54 C55 H55A 103.9 . . ? C56 C55 H55A 103.9 . . ? C54 C55 H55B 103.8 . . ? C56 C55 H55B 103.9 . . ? H55A C55 H55B 105.4 . . ? C57 C56 C55 116(4) . . ? C57 C56 H56A 108.3 . . ? C55 C56 H56A 108.2 . . ? C57 C56 H56B 108.3 . . ? C55 C56 H56B 108.2 . . ? H56A C56 H56B 107.4 . . ? C56 C57 C58 122(4) . . ? C56 C57 H57A 106.9 . . ? C58 C57 H57A 106.8 . . ? C56 C57 H57B 106.8 . . ? C58 C57 H57B 106.7 . . ? H57A C57 H57B 106.6 . . ? C57 C58 H58A 109.6 . . ? C57 C58 H58B 109.4 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.4 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C60 C59 C28 110.4(11) . . ? C60 C59 H59A 109.6 . . ? C28 C59 H59A 109.6 . . ? C60 C59 H59B 109.6 . . ? C28 C59 H59B 109.6 . . ? H59A C59 H59B 108.1 . . ? C59 C60 C61 112.1(18) . . ? C59 C60 H60A 109.2 . . ? C61 C60 H60A 109.2 . . ? C59 C60 H60B 109.2 . . ? C61 C60 H60B 109.2 . . ? H60A C60 H60B 107.9 . . ? C62 C61 C60 110.1(19) . . ? C62 C61 H61A 109.7 . . ? C60 C61 H61A 109.6 . . ? C62 C61 H61B 109.7 . . ? C60 C61 H61B 109.6 . . ? H61A C61 H61B 108.1 . . ? C63 C62 C61 146(3) . . ? C63 C62 H62A 100.4 . . ? C61 C62 H62A 100.4 . . ? C63 C62 H62B 100.4 . . ? C61 C62 H62B 100.4 . . ? H62A C62 H62B 104.3 . . ? C62 C63 C64 160(2) . . ? C62 C63 H63A 96.2 . . ? C64 C63 H63A 96.1 . . ? C62 C63 H63B 96.1 . . ? C64 C63 H63B 96.1 . . ? H63A C63 H63B 103.4 . . ? C65 C64 C63 173(2) . . ? C65 C64 H64A 92.2 . . ? C63 C64 H64A 92.2 . . ? C65 C64 H64B 92.2 . . ? C63 C64 H64B 92.2 . . ? H64A C64 H64B 103.0 . . ? C64 C65 C66 164(3) . . ? C64 C65 H65A 94.9 . . ? C66 C65 H65A 94.8 . . ? C64 C65 H65B 94.8 . . ? C66 C65 H65B 94.9 . . ? H65A C65 H65B 103.2 . . ? C67 C66 C65 156(3) . . ? C67 C66 H66A 97.4 . . ? C65 C66 H66A 97.4 . . ? C67 C66 H66B 97.4 . . ? C65 C66 H66B 97.4 . . ? H66A C66 H66B 103.6 . . ? C66 C67 C68 152(3) . . ? C66 C67 H67A 98.7 . . ? C68 C67 H67A 98.7 . . ? C66 C67 H67B 98.7 . . ? C68 C67 H67B 98.7 . . ? H67A C67 H67B 103.9 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? O1S C1S C2S 130.8 . . ? O1S C1S O2S 102.3 . . ? C2S C1S O2S 120.2 . . ? C1S C2S H2SA 109.5 . . ? C1S C2S H2SB 109.5 . . ? H2SA C2S H2SB 109.5 . . ? C1S C2S H2SC 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? C4S C3S O2S 123.2 . . ? C4S C3S H3SA 106.5 . . ? O2S C3S H3SA 106.5 . . ? C4S C3S H3SB 106.5 . . ? O2S C3S H3SB 106.5 . . ? H3SA C3S H3SB 106.5 . . ? C3S C4S H4SA 109.5 . . ? C3S C4S H4SB 109.5 . . ? H4SA C4S H4SB 109.5 . . ? C3S C4S H4SC 109.5 . . ? H4SA C4S H4SC 109.5 . . ? H4SB C4S H4SC 109.5 . . ? C3S O2S C1S 131.8 . . ? C6S C5S N1S 146.2 . . ? C5S C6S H6SA 109.5 . . ? C5S C6S H6SB 109.4 . . ? H6SA C6S H6SB 109.5 . . ? C5S C6S H6SC 109.5 . . ? H6SA C6S H6SC 109.5 . . ? H6SB C6S H6SC 109.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 O1 -179.8(8) . . . . ? C28 C1 C2 O1 2.1(13) . . . . ? C6 C1 C2 C3 0.2(13) . . . . ? C28 C1 C2 C3 -177.9(9) . . . . ? O1 C2 C3 C4 178.7(10) . . . . ? C1 C2 C3 C4 -1.3(16) . . . . ? O1 C2 C3 O2 2.4(15) . . . . ? C1 C2 C3 O2 -177.6(10) . . . . ? O2 C3 C4 O3 -1.1(17) . . . . ? C2 C3 C4 O3 -177.3(10) . . . . ? O2 C3 C4 C5 177.1(10) . . . . ? C2 C3 C4 C5 0.8(17) . . . . ? C3 C4 C5 C6 0.8(14) . . . . ? O3 C4 C5 C6 178.9(9) . . . . ? C3 C4 C5 C7 -179.7(9) . . . . ? O3 C4 C5 C7 -1.6(14) . . . . ? C2 C1 C6 C5 1.5(12) . . . . ? C28 C1 C6 C5 179.5(8) . . . . ? C4 C5 C6 C1 -2.0(13) . . . . ? C7 C5 C6 C1 178.5(8) . . . . ? C6 C5 C7 C8 91.6(10) . . . . ? C4 C5 C7 C8 -88.0(10) . . . . ? C6 C5 C7 C29 -33.6(11) . . . . ? C4 C5 C7 C29 146.9(8) . . . . ? C5 C7 C8 C13 -83.6(10) . . . . ? C29 C7 C8 C13 41.1(10) . . . . ? C5 C7 C8 C9 93.6(9) . . . . ? C29 C7 C8 C9 -141.8(8) . . . . ? C13 C8 C9 O4 -177.8(8) . . . . ? C7 C8 C9 O4 4.9(12) . . . . ? C13 C8 C9 C10 -1.2(12) . . . . ? C7 C8 C9 C10 -178.5(8) . . . . ? O4 C9 C10 C11 177.1(8) . . . . ? C8 C9 C10 C11 0.4(14) . . . . ? O4 C9 C10 O5 -1.6(13) . . . . ? C8 C9 C10 O5 -178.3(8) . . . . ? O5 C10 C11 O6 -1.2(14) . . . . ? C9 C10 C11 O6 -179.9(8) . . . . ? O5 C10 C11 C12 179.2(8) . . . . ? C9 C10 C11 C12 0.5(14) . . . . ? C10 C11 C12 C13 -0.5(13) . . . . ? O6 C11 C12 C13 179.9(8) . . . . ? C10 C11 C12 C14 179.1(8) . . . . ? O6 C11 C12 C14 -0.4(12) . . . . ? C11 C12 C13 C8 -0.4(13) . . . . ? C14 C12 C13 C8 179.9(8) . . . . ? C9 C8 C13 C12 1.3(13) . . . . ? C7 C8 C13 C12 178.5(8) . . . . ? C13 C12 C14 C15 85.1(10) . . . . ? C11 C12 C14 C15 -94.5(9) . . . . ? C13 C12 C14 C39 -41.6(11) . . . . ? C11 C12 C14 C39 138.8(8) . . . . ? C12 C14 C15 C20 -91.8(10) . . . . ? C39 C14 C15 C20 35.9(12) . . . . ? C12 C14 C15 C16 92.6(10) . . . . ? C39 C14 C15 C16 -139.8(9) . . . . ? C20 C15 C16 O7 178.7(9) . . . . ? C14 C15 C16 O7 -5.4(15) . . . . ? C20 C15 C16 C17 2.9(15) . . . . ? C14 C15 C16 C17 178.8(9) . . . . ? O7 C16 C17 C18 -179.0(10) . . . . ? C15 C16 C17 C18 -3.1(18) . . . . ? O7 C16 C17 O8 3.0(17) . . . . ? C15 C16 C17 O8 178.9(10) . . . . ? C16 C17 C18 C19 2.5(19) . . . . ? O8 C17 C18 C19 -179.5(10) . . . . ? C16 C17 C18 O9 -179.1(10) . . . . ? O8 C17 C18 O9 -1.1(18) . . . . ? C17 C18 C19 C20 -1.7(16) . . . . ? O9 C18 C19 C20 180.0(9) . . . . ? C17 C18 C19 C21 177.6(11) . . . . ? O9 C18 C19 C21 -0.7(17) . . . . ? C16 C15 C20 C19 -2.4(15) . . . . ? C14 C15 C20 C19 -178.2(9) . . . . ? C18 C19 C20 C15 1.8(15) . . . . ? C21 C19 C20 C15 -177.6(9) . . . . ? C20 C19 C21 C49 -36.7(14) . . . . ? C18 C19 C21 C49 144.0(10) . . . . ? C20 C19 C21 C22 92.4(11) . . . . ? C18 C19 C21 C22 -86.9(12) . . . . ? C19 C21 C22 C23 91.0(10) . . . . ? C49 C21 C22 C23 -140.5(8) . . . . ? C19 C21 C22 C27 -87.9(9) . . . . ? C49 C21 C22 C27 40.6(11) . . . . ? C27 C22 C23 O10 179.9(8) . . . . ? C21 C22 C23 O10 1.0(13) . . . . ? C27 C22 C23 C24 0.6(13) . . . . ? C21 C22 C23 C24 -178.3(9) . . . . ? C22 C23 C24 O11 -178.8(8) . . . . ? O10 C23 C24 O11 1.9(14) . . . . ? C22 C23 C24 C25 -2.2(15) . . . . ? O10 C23 C24 C25 178.5(8) . . . . ? O11 C24 C25 O12 -2.3(13) . . . . ? C23 C24 C25 O12 -179.1(9) . . . . ? O11 C24 C25 C26 179.3(8) . . . . ? C23 C24 C25 C26 2.5(14) . . . . ? O12 C25 C26 C27 -179.6(8) . . . . ? C24 C25 C26 C27 -1.3(13) . . . . ? O12 C25 C26 C28 2.1(13) . . . . ? C24 C25 C26 C28 -179.6(8) . . . . ? C23 C22 C27 C26 0.6(13) . . . . ? C21 C22 C27 C26 179.5(8) . . . . ? C25 C26 C27 C22 -0.2(13) . . . . ? C28 C26 C27 C22 178.0(8) . . . . ? C6 C1 C28 C59 36.7(12) . . . . ? C2 C1 C28 C59 -145.3(9) . . . . ? C6 C1 C28 C26 -89.7(9) . . . . ? C2 C1 C28 C26 88.2(10) . . . . ? C27 C26 C28 C1 86.7(10) . . . . ? C25 C26 C28 C1 -95.2(9) . . . . ? C27 C26 C28 C59 -40.4(11) . . . . ? C25 C26 C28 C59 137.7(8) . . . . ? C5 C7 C29 C30 -63.8(9) . . . . ? C8 C7 C29 C30 171.8(7) . . . . ? C7 C29 C30 C31 159.0(7) . . . . ? C29 C30 C31 C32 -176.5(8) . . . . ? C30 C31 C32 C33 172.7(8) . . . . ? C31 C32 C33 C34 -175.4(8) . . . . ? C32 C33 C34 C35 172.6(9) . . . . ? C33 C34 C35 C36 179.9(9) . . . . ? C34 C35 C36 C37 176.0(9) . . . . ? C35 C36 C37 C38 -71.9(16) . . . . ? C12 C14 C39 C40 -55.8(11) . . . . ? C15 C14 C39 C40 178.2(8) . . . . ? C14 C39 C40 C41 -62.7(17) . . . . ? C39 C40 C41 C42 -158.2(14) . . . . ? C40 C41 C42 C43 -167.1(16) . . . . ? C41 C42 C43 C44 161.6(17) . . . . ? C42 C43 C44 C45 -180(2) . . . . ? C43 C44 C45 C46 -178.1(18) . . . . ? C44 C45 C46 C47 -172(3) . . . . ? C45 C46 C47 C48 48(4) . . . . ? C19 C21 C49 C50 -175.8(9) . . . . ? C22 C21 C49 C50 56.4(11) . . . . ? C21 C49 C50 C51 -149.5(10) . . . . ? C49 C50 C51 C52 172.5(11) . . . . ? C50 C51 C52 C53 -171.8(11) . . . . ? C51 C52 C53 C54 -179.9(13) . . . . ? C52 C53 C54 C55 -140(4) . . . . ? C53 C54 C55 C56 177(4) . . . . ? C54 C55 C56 C57 158(5) . . . . ? C55 C56 C57 C58 178(3) . . . . ? C1 C28 C59 C60 66.4(12) . . . . ? C26 C28 C59 C60 -168.6(10) . . . . ? C28 C59 C60 C61 162.9(11) . . . . ? C59 C60 C61 C62 -115(2) . . . . ? C60 C61 C62 C63 168(3) . . . . ? C61 C62 C63 C64 176(6) . . . . ? C62 C63 C64 C65 173(16) . . . . ? C63 C64 C65 C66 -128(19) . . . . ? C64 C65 C66 C67 -174(5) . . . . ? C65 C66 C67 C68 -175(4) . . . . ? C4S C3S O2S C1S -168.8 . . . . ? O1S C1S O2S C3S -26.1 . . . . ? C2S C1S O2S C3S 179.6 . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.899 _refine_diff_density_min -0.767 _refine_diff_density_rms 0.201 # Attachment 'Decenyl-Pg(g9708).cif' data_g9708 _database_code_depnum_ccdc_archive 'CCDC 701458' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C71 H110 O15' _chemical_formula_weight 1203.59 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 Rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 37.052(2) _cell_length_b 37.052(2) _cell_length_c 25.8772(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 30767(4) _cell_formula_units_Z 18 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7468 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 19.84 _exptl_crystal_description rectangular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.169 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11808 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9779 _exptl_absorpt_correction_T_max 0.9904 _exptl_absorpt_process_details 'sadabs v2008/1' _exptl_special_details ; All H atoms were added in their calculated positions and were treated using appropriate riding models. Solvents: 50% occupancy EtOAc (1), EtOH (1) and H2O (3) Restraints used: AFIX 6, DFIX for solvents Solvents refined isotropic only. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 138722 _diffrn_reflns_av_R_equivalents 0.1651 _diffrn_reflns_av_sigmaI/netI 0.1185 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12047 _reflns_number_gt 5534 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Apex II (Bruker, 2006)' _computing_cell_refinement 'Bruker-Apex II (Bruker, 2006)' _computing_data_reduction 'Bruker-SAINT (Bruker, 2006)' _computing_structure_solution 'Bruker-SHELXTL (Sheldrick, G.M., 2008)' _computing_structure_refinement 'Bruker-SHELXTL (Sheldrick, G.M., 2008)' _computing_molecular_graphics 'Bruker-SHELXTL (Sheldrick, G.M., 2008)' _computing_publication_material 'Bruker-SHELXTL (Sheldrick, G.M., 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12047 _refine_ls_number_parameters 653 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.2448 _refine_ls_R_factor_gt 0.1301 _refine_ls_wR_factor_ref 0.4327 _refine_ls_wR_factor_gt 0.3501 _refine_ls_goodness_of_fit_ref 1.335 _refine_ls_restrained_S_all 1.716 _refine_ls_shift/su_max 0.016 _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 0.7175(2) 0.1512(2) -0.1534(3) 0.0570(19) Uani 1 1 d . . . H1 H 0.7345 0.1430 -0.1476 0.085 Uiso 1 1 calc R . . O2 O 0.6452(3) 0.1321(2) -0.1993(2) 0.077(3) Uani 1 1 d . . . H2 H 0.6504 0.1570 -0.1984 0.116 Uiso 1 1 calc R . . O3 O 0.5710(2) 0.0851(2) -0.1508(2) 0.0510(18) Uani 1 1 d . . . H3 H 0.5755 0.0870 -0.1828 0.077 Uiso 1 1 calc R . . O4 O 0.5111(2) 0.08134(19) -0.0904(2) 0.0507(19) Uani 1 1 d . . . H4 H 0.5046 0.0983 -0.1029 0.076 Uiso 1 1 calc R . . O5 O 0.49226(19) 0.1335(2) -0.0388(3) 0.059(2) Uani 1 1 d . . . H5 H 0.4685 0.1131 -0.0445 0.088 Uiso 1 1 calc R . . O6 O 0.51905(19) 0.15811(18) 0.0589(3) 0.0480(18) Uani 1 1 d . . . H6 H 0.5384 0.1749 0.0781 0.072 Uiso 1 1 calc R . . O7 O 0.5852(2) 0.2185(2) 0.1084(3) 0.0514(18) Uani 1 1 d . . . H7 H 0.5769 0.2188 0.1385 0.077 Uiso 1 1 calc R . . O8 O 0.6621(3) 0.2873(2) 0.1073(4) 0.082(3) Uani 1 1 d . . . H8 H 0.6588 0.2928 0.0767 0.123 Uiso 1 1 calc R . . O9 O 0.7324(2) 0.28238(17) 0.1104(3) 0.0526(19) Uani 1 1 d . . . H9 H 0.7428 0.2869 0.0806 0.079 Uiso 1 1 calc R . . O10 O 0.79159(19) 0.27706(17) 0.0563(3) 0.0502(18) Uani 1 1 d . . . H10 H 0.7774 0.2756 0.0823 0.075 Uiso 1 1 calc R . . O11 O 0.81444(19) 0.2751(2) -0.0421(3) 0.063(2) Uani 1 1 d . . . H11 H 0.8120 0.2720 -0.0743 0.094 Uiso 1 1 calc R . . O12 O 0.78216(18) 0.2015(2) -0.0949(2) 0.0525(19) Uani 1 1 d . . . H12 H 0.8079 0.2180 -0.0971 0.079 Uiso 1 1 calc R . . C1 C 0.6822(2) 0.1124(2) -0.0766(3) 0.0244(19) Uani 1 1 d . . . C2 C 0.6815(3) 0.1271(3) -0.1263(3) 0.033(2) Uani 1 1 d . . . C3 C 0.6447(3) 0.1183(3) -0.1496(3) 0.039(2) Uani 1 1 d . . . C4 C 0.6069(3) 0.0937(3) -0.1247(3) 0.034(2) Uani 1 1 d . . . C5 C 0.6059(2) 0.0786(2) -0.0759(3) 0.0203(17) Uani 1 1 d . . . C6 C 0.6435(2) 0.0885(2) -0.0527(3) 0.0186(17) Uani 1 1 d . . . H6A H 0.6429 0.0785 -0.0188 0.022 Uiso 1 1 calc R . . C7 C 0.5637(2) 0.0519(2) -0.0482(3) 0.0219(18) Uani 1 1 d . . . H7A H 0.5421 0.0372 -0.0754 0.026 Uiso 1 1 calc R . . C8 C 0.5518(2) 0.0800(2) -0.0183(3) 0.0214(18) Uani 1 1 d . . . C9 C 0.5265(2) 0.0936(2) -0.0411(3) 0.028(2) Uani 1 1 d . . . C10 C 0.5165(2) 0.1200(3) -0.0147(4) 0.033(2) Uani 1 1 d . . . C11 C 0.5309(2) 0.1326(2) 0.0345(3) 0.030(2) Uani 1 1 d . . . C12 C 0.5562(2) 0.1200(2) 0.0594(3) 0.0201(18) Uani 1 1 d . . . C13 C 0.5660(2) 0.0940(2) 0.0310(3) 0.0190(17) Uani 1 1 d . . . H13A H 0.5836 0.0853 0.0468 0.023 Uiso 1 1 calc R . . C14 C 0.5723(2) 0.1345(2) 0.1134(3) 0.0224(18) Uani 1 1 d . . . H14A H 0.5529 0.1425 0.1299 0.027 Uiso 1 1 calc R . . C15 C 0.6157(2) 0.1741(2) 0.1128(3) 0.0206(17) Uani 1 1 d . . . C16 C 0.6197(3) 0.2135(2) 0.1103(3) 0.033(2) Uani 1 1 d . . . C17 C 0.6589(3) 0.2492(2) 0.1090(4) 0.041(2) Uani 1 1 d . . . C18 C 0.6941(3) 0.2456(2) 0.1101(3) 0.033(2) Uani 1 1 d . . . C19 C 0.6918(2) 0.2072(2) 0.1120(3) 0.0222(18) Uani 1 1 d . . . C20 C 0.6521(2) 0.1721(2) 0.1125(3) 0.0213(17) Uani 1 1 d . . . H20A H 0.6498 0.1454 0.1127 0.026 Uiso 1 1 calc R . . C21 C 0.7308(2) 0.2035(2) 0.1121(3) 0.0251(19) Uani 1 1 d . . . H21A H 0.7533 0.2296 0.1284 0.030 Uiso 1 1 calc R . . C22 C 0.7449(2) 0.2029(2) 0.0566(3) 0.0218(18) Uani 1 1 d . . . C23 C 0.7737(2) 0.2397(2) 0.0322(3) 0.031(2) Uani 1 1 d . . . C24 C 0.7856(2) 0.2386(2) -0.0182(4) 0.035(2) Uani 1 1 d . . . C25 C 0.7692(2) 0.2012(3) -0.0447(3) 0.033(2) Uani 1 1 d . . . C26 C 0.7402(2) 0.1642(2) -0.0218(3) 0.0256(19) Uani 1 1 d . . . C27 C 0.7284(2) 0.1658(2) 0.0284(3) 0.0219(18) Uani 1 1 d . . . H27A H 0.7083 0.1407 0.0445 0.026 Uiso 1 1 calc R . . C28 C 0.7225(2) 0.1232(2) -0.0506(3) 0.0263(19) Uani 1 1 d . . . H28A H 0.7426 0.1284 -0.0794 0.032 Uiso 1 1 calc R . . C29 C 0.56374(16) 0.01874(13) -0.0132(2) 0.0256(19) Uani 1 1 d G . . H29A H 0.5370 0.0042 0.0058 0.031 Uiso 1 1 calc R . . H29B H 0.5864 0.0324 0.0126 0.031 Uiso 1 1 calc R . . C30 C 0.56986(14) -0.01368(13) -0.04422(16) 0.033(2) Uani 1 1 d G . . H30A H 0.5429 -0.0348 -0.0593 0.039 Uiso 1 1 calc R . . H30B H 0.5897 0.0004 -0.0729 0.039 Uiso 1 1 calc R . . C31 C 0.58677(11) -0.03527(10) -0.00857(13) 0.030(2) Uani 1 1 d G . . H31A H 0.5664 -0.0501 0.0194 0.036 Uiso 1 1 calc R . . H31B H 0.6130 -0.0139 0.0076 0.036 Uiso 1 1 calc R . . C32 C 0.59510(12) -0.06698(11) -0.03844(13) 0.034(2) Uani 1 1 d G . . H32A H 0.5686 -0.0902 -0.0517 0.040 Uiso 1 1 calc R . . H32B H 0.6138 -0.0530 -0.0682 0.040 Uiso 1 1 calc R . . C33 C 0.61535(10) -0.08368(9) -0.00134(11) 0.033(2) Uani 1 1 d G . . H33A H 0.5958 -0.0985 0.0274 0.040 Uiso 1 1 calc R . . H33B H 0.6407 -0.0599 0.0136 0.040 Uiso 1 1 calc R . . C34 C 0.62737(13) -0.11374(11) -0.02765(14) 0.034(2) Uani 1 1 d G . . H34A H 0.6020 -0.1391 -0.0396 0.041 Uiso 1 1 calc R . . H34B H 0.6453 -0.1000 -0.0580 0.041 Uiso 1 1 calc R . . C35 C 0.65075(12) -0.12556(11) 0.01155(14) 0.037(2) Uani 1 1 d G . . H35A H 0.6319 -0.1410 0.0406 0.045 Uiso 1 1 calc R . . H35B H 0.6747 -0.0999 0.0256 0.045 Uiso 1 1 calc R . . C36 C 0.66700(15) -0.15327(13) -0.01379(17) 0.041(2) Uani 1 1 d G . . H36A H 0.6433 -0.1794 -0.0273 0.050 Uiso 1 1 calc R . . H36B H 0.6859 -0.1382 -0.0429 0.050 Uiso 1 1 calc R . . C37 C 0.69067(17) -0.16335(15) 0.0281(2) 0.050(3) Uani 1 1 d G . . H37A H 0.6751 -0.1804 0.0564 0.060 Uiso 1 1 calc R . . C38 C 0.73138(17) -0.14957(17) 0.0269(3) 0.076(4) Uani 1 1 d G . . H38A H 0.7478 -0.1324 -0.0008 0.092 Uiso 1 1 calc R . . H38B H 0.7440 -0.1569 0.0538 0.092 Uiso 1 1 calc R . . C39 C 0.57264(8) 0.10067(14) 0.1485(2) 0.029(2) Uani 1 1 d G . . H39A H 0.5940 0.0944 0.1354 0.035 Uiso 1 1 calc R . . H39B H 0.5810 0.1122 0.1838 0.035 Uiso 1 1 calc R . . C40 C 0.53100(9) 0.06010(12) 0.15169(18) 0.031(2) Uani 1 1 d G . . H40A H 0.5239 0.0472 0.1169 0.038 Uiso 1 1 calc R . . H40B H 0.5341 0.0406 0.1750 0.038 Uiso 1 1 calc R . . C41 C 0.49509(8) 0.06532(10) 0.17106(16) 0.034(2) Uani 1 1 d G . . H41A H 0.4889 0.0814 0.1455 0.040 Uiso 1 1 calc R . . H41B H 0.5030 0.0810 0.2040 0.040 Uiso 1 1 calc R . . C42 C 0.45600(8) 0.02215(9) 0.17940(15) 0.032(2) Uani 1 1 d G . . H42A H 0.4608 0.0080 0.2088 0.039 Uiso 1 1 calc R . . H42B H 0.4509 0.0048 0.1481 0.039 Uiso 1 1 calc R . . C43 C 0.41715(8) 0.02634(9) 0.19060(12) 0.034(2) Uani 1 1 d G . . H43A H 0.4144 0.0437 0.1636 0.041 Uiso 1 1 calc R . . H43B H 0.4205 0.0403 0.2243 0.041 Uiso 1 1 calc R . . C44 C 0.37724(8) -0.01727(9) 0.19154(15) 0.036(2) Uani 1 1 d G . . H44A H 0.3737 -0.0309 0.1575 0.043 Uiso 1 1 calc R . . H44B H 0.3803 -0.0348 0.2180 0.043 Uiso 1 1 calc R . . C45 C 0.33869(8) -0.01395(10) 0.20364(12) 0.036(2) Uani 1 1 d G . . H45A H 0.3416 -0.0016 0.2384 0.043 Uiso 1 1 calc R . . H45B H 0.3362 0.0046 0.1781 0.043 Uiso 1 1 calc R . . C46 C 0.29961(8) -0.05672(11) 0.2019(2) 0.035(2) Uani 1 1 d G . . H46A H 0.3032 -0.0753 0.2264 0.042 Uiso 1 1 calc R . . H46B H 0.2970 -0.0684 0.1668 0.042 Uiso 1 1 calc R . . C47 C 0.25898(8) -0.05731(14) 0.21520(18) 0.038(2) Uani 1 1 d G . . H47A H 0.2339 -0.0835 0.2143 0.046 Uiso 1 1 calc R . . C48 C 0.25606(9) -0.02339(16) 0.2281(3) 0.043(2) Uani 1 1 d G . . H48A H 0.2804 0.0033 0.2294 0.051 Uiso 1 1 calc R . . H48B H 0.2297 -0.0263 0.2358 0.051 Uiso 1 1 calc R . . C49 C 0.72718(19) 0.16761(18) 0.1439(3) 0.035(2) Uani 1 1 d G . . H49A H 0.7093 0.1412 0.1253 0.042 Uiso 1 1 calc R . . H49B H 0.7135 0.1665 0.1772 0.042 Uiso 1 1 calc R . . C50 C 0.76979(16) 0.17162(15) 0.1545(3) 0.062(3) Uani 1 1 d G . . H50A H 0.7856 0.1797 0.1217 0.075 Uiso 1 1 calc R . . H50B H 0.7849 0.1951 0.1788 0.075 Uiso 1 1 calc R . . C51 C 0.7719(2) 0.1347(2) 0.1761(2) 0.093(5) Uani 1 1 d G . . H51A H 0.7960 0.1449 0.1999 0.111 Uiso 1 1 calc R . . H51B H 0.7463 0.1170 0.1962 0.111 Uiso 1 1 calc R . . C52 C 0.77627(14) 0.10932(14) 0.13512(18) 0.099(5) Uani 1 1 d G . . H52A H 0.8015 0.1277 0.1146 0.119 Uiso 1 1 calc R . . H52B H 0.7520 0.0993 0.1117 0.119 Uiso 1 1 calc R . . C53 C 0.77957(17) 0.07091(16) 0.1531(2) 0.077(4) Uani 1 1 d G . . H53A H 0.7983 0.0791 0.1835 0.092 Uiso 1 1 calc R . . H53B H 0.7517 0.0487 0.1643 0.092 Uiso 1 1 calc R . . C54 C 0.7945(2) 0.05492(18) 0.1152(2) 0.148(8) Uani 1 1 d G . . H54A H 0.8172 0.0783 0.0960 0.177 Uiso 1 1 calc R . . H54B H 0.7718 0.0383 0.0904 0.177 Uiso 1 1 calc R . . C55 C 0.8116(2) 0.02611(19) 0.1387(3) 0.109(5) Uani 1 1 d G . . H55A H 0.8345 0.0423 0.1633 0.131 Uiso 1 1 calc R . . H55B H 0.7890 0.0021 0.1573 0.131 Uiso 1 1 calc R . . C56 C 0.8272(3) 0.0109(3) 0.0940(3) 0.28(2) Uani 1 1 d G . . H56A H 0.8444 0.0348 0.0711 0.337 Uiso 1 1 calc R . . H56B H 0.8028 -0.0095 0.0737 0.337 Uiso 1 1 calc R . . C57 C 0.8533(3) -0.0098(3) 0.1094(4) 0.291(19) Uani 1 1 d G . . H57A H 0.8776 0.0063 0.1295 0.349 Uiso 1 1 calc R . . C58 C 0.8426(4) -0.0552(3) 0.0943(4) 0.291(19) Uani 1 1 d G . . H58A H 0.8186 -0.0723 0.0742 0.349 Uiso 1 1 calc R . . H58B H 0.8603 -0.0655 0.1053 0.349 Uiso 1 1 calc R . . C59 C 0.7222(2) 0.08801(17) -0.0177(3) 0.035(2) Uani 1 1 d G . . H59A H 0.7491 0.0990 0.0005 0.042 Uiso 1 1 calc R . . H59B H 0.6998 0.0783 0.0085 0.042 Uiso 1 1 calc R . . C60 C 0.71496(17) 0.05104(17) -0.0523(2) 0.054(3) Uani 1 1 d G . . H60A H 0.7299 0.0616 -0.0855 0.065 Uiso 1 1 calc R . . H60B H 0.6849 0.0334 -0.0598 0.065 Uiso 1 1 calc R . . C61 C 0.73104(15) 0.02462(14) -0.02438(19) 0.071(3) Uani 1 1 d G . . H61A H 0.7604 0.0428 -0.0137 0.085 Uiso 1 1 calc R . . H61B H 0.7142 0.0117 0.0070 0.085 Uiso 1 1 calc R . . C62 C 0.72796(15) -0.00873(15) -0.0602(3) 0.083(4) Uani 1 1 d G . . H62A H 0.7390 0.0037 -0.0945 0.100 Uiso 1 1 calc R . . H62B H 0.6983 -0.0302 -0.0645 0.100 Uiso 1 1 calc R . . C63 C 0.75174(17) -0.02912(13) -0.0405(3) 0.095(4) Uani 1 1 d G . . H63A H 0.7407 -0.0567 -0.0572 0.114 Uiso 1 1 calc R . . H63B H 0.7471 -0.0338 -0.0028 0.114 Uiso 1 1 calc R . . C64 C 0.79972(16) -0.00262(16) -0.0510(2) 0.092(4) Uani 1 1 d G . . H64A H 0.8046 0.0086 -0.0866 0.111 Uiso 1 1 calc R . . H64B H 0.8125 0.0212 -0.0267 0.111 Uiso 1 1 calc R . . C65 C 0.8196(2) -0.0290(2) -0.0443(3) 0.113(5) Uani 1 1 d G . . H65A H 0.8047 -0.0545 -0.0657 0.136 Uiso 1 1 calc R . . H65B H 0.8174 -0.0377 -0.0077 0.136 Uiso 1 1 calc R . . C66 C 0.87094(19) -0.0020(2) -0.0620(4) 0.278(18) Uani 1 1 d G . . H66A H 0.8723 0.0048 -0.0992 0.334 Uiso 1 1 calc R . . H66B H 0.8844 0.0248 -0.0429 0.334 Uiso 1 1 calc R . . C67 C 0.8968(2) -0.0232(3) -0.0534(5) 0.200 Uiso 1 1 d G . . H67A H 0.8900 -0.0405 -0.0236 0.240 Uiso 1 1 calc R . . C68 C 0.9229(3) -0.0207(3) -0.0783(5) 0.200 Uiso 1 1 d G . . H68A H 0.9310 -0.0039 -0.1086 0.240 Uiso 1 1 calc R A 1 H68B H 0.9368 -0.0355 -0.0691 0.240 Uiso 1 1 calc R A 1 O1S O 0.7760(7) 0.4799(12) 0.7953(12) 0.33(3) Uiso 0.50 1 d PG B 1 O2S O 0.7128(5) 0.4667(5) 0.7708(7) 0.118(7) Uiso 0.50 1 d PG B 1 C1S C 0.7119(11) 0.4393(10) 0.6958(8) 0.186(18) Uiso 0.50 1 d PG B 1 H1SA H 0.7098 0.4409 0.6582 0.279 Uiso 0.50 1 calc PR B 1 H1SB H 0.6889 0.4127 0.7082 0.279 Uiso 0.50 1 calc PR B 1 H1SC H 0.7385 0.4412 0.7045 0.279 Uiso 0.50 1 calc PR B 1 C2S C 0.7095(6) 0.4745(6) 0.7208(7) 0.084(8) Uiso 0.50 1 d PG B 1 H2SA H 0.7327 0.5020 0.7098 0.101 Uiso 0.50 1 calc PR B 1 H2SB H 0.6826 0.4732 0.7135 0.101 Uiso 0.50 1 calc PR B 1 C3S C 0.7464(8) 0.4754(7) 0.8140(8) 0.20(2) Uiso 0.50 1 d PG B 1 C4S C 0.7376(11) 0.4678(10) 0.8522(7) 0.24(3) Uiso 0.50 1 d PG B 1 H4SA H 0.7622 0.4752 0.8734 0.357 Uiso 0.50 1 calc PR B 1 H4SB H 0.7181 0.4377 0.8550 0.357 Uiso 0.50 1 calc PR B 1 H4SC H 0.7240 0.4831 0.8643 0.357 Uiso 0.50 1 calc PR B 1 O4S O 0.5926(12) 0.3412(12) 0.6880(16) 0.231(16) Uiso 0.50 1 d P C 2 O5S O 0.979(3) -0.031(2) -0.060(2) 0.46(5) Uiso 0.50 1 d P . 2 O6S O 0.6300(19) 0.335(2) 0.720(2) 0.37(3) Uiso 0.50 1 d P D 1 C5S C 0.6583(11) 0.4469(6) 0.7154(10) 0.163(16) Uiso 0.50 1 d PGD E 2 H5SA H 0.6351 0.4519 0.7240 0.195 Uiso 0.50 1 calc PR E 2 H5SB H 0.6717 0.4474 0.7487 0.195 Uiso 0.50 1 calc PR E 2 C6S C 0.6394(14) 0.4054(5) 0.6980(18) 0.23(2) Uiso 0.50 1 d PGD E 2 H6SA H 0.6202 0.3868 0.7245 0.339 Uiso 0.50 1 calc PR E 2 H6SB H 0.6609 0.3980 0.6912 0.339 Uiso 0.50 1 calc PR E 2 H6SC H 0.6239 0.4025 0.6661 0.339 Uiso 0.50 1 calc PR E 2 O3S O 0.6805(4) 0.4739(4) 0.6949(5) 0.056(4) Uiso 0.50 1 d PGD E 2 H3S H 0.6764 0.4698 0.6630 0.085 Uiso 0.50 1 calc PR E 2 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 0.059(5) 0.056(4) 0.046(4) 0.029(3) 0.030(4) 0.021(4) O2 0.112(7) 0.066(5) 0.027(4) 0.026(4) -0.009(4) 0.025(5) O3 0.064(4) 0.055(4) 0.036(4) -0.003(3) -0.031(3) 0.032(4) O4 0.057(4) 0.044(4) 0.045(4) 0.007(3) -0.031(3) 0.021(3) O5 0.037(4) 0.059(4) 0.092(6) 0.030(4) -0.012(4) 0.033(3) O6 0.041(4) 0.031(4) 0.087(6) 0.005(3) 0.010(3) 0.029(3) O7 0.060(4) 0.056(4) 0.069(5) 0.001(4) 0.006(4) 0.052(4) O8 0.113(7) 0.027(4) 0.124(7) 0.002(4) -0.006(6) 0.048(4) O9 0.049(4) 0.019(3) 0.064(5) 0.003(3) -0.003(4) -0.003(3) O10 0.036(4) 0.015(3) 0.086(6) 0.002(3) -0.011(3) 0.003(3) O11 0.031(4) 0.048(4) 0.082(5) 0.047(4) 0.012(4) 0.000(3) O12 0.030(3) 0.083(5) 0.040(4) 0.032(4) 0.018(3) 0.024(4) C1 0.038(5) 0.018(4) 0.023(5) 0.005(3) 0.008(4) 0.018(4) C2 0.040(5) 0.028(5) 0.025(5) 0.008(4) 0.007(4) 0.012(4) C3 0.053(6) 0.035(5) 0.019(5) 0.007(4) -0.005(5) 0.014(5) C4 0.051(6) 0.030(5) 0.023(5) -0.005(4) -0.014(4) 0.022(5) C5 0.033(5) 0.013(4) 0.017(4) -0.003(3) -0.004(4) 0.014(4) C6 0.027(4) 0.015(4) 0.017(4) 0.002(3) 0.001(3) 0.013(3) C7 0.023(4) 0.015(4) 0.024(5) -0.001(3) -0.010(3) 0.007(3) C8 0.019(4) 0.011(4) 0.031(5) 0.007(3) -0.002(4) 0.004(3) C9 0.019(4) 0.030(5) 0.029(5) 0.010(4) -0.005(4) 0.008(4) C10 0.025(5) 0.032(5) 0.049(6) 0.014(4) -0.002(4) 0.020(4) C11 0.029(5) 0.020(4) 0.047(6) 0.008(4) 0.004(4) 0.017(4) C12 0.012(4) 0.013(4) 0.036(5) 0.009(3) 0.009(3) 0.007(3) C13 0.015(4) 0.018(4) 0.025(5) 0.009(3) 0.000(3) 0.009(3) C14 0.025(4) 0.025(4) 0.024(5) 0.009(4) 0.009(4) 0.017(4) C15 0.024(4) 0.019(4) 0.020(4) 0.005(3) 0.008(3) 0.012(3) C16 0.038(5) 0.028(5) 0.042(6) -0.003(4) 0.000(4) 0.024(4) C17 0.046(6) 0.020(5) 0.064(7) -0.001(4) 0.002(5) 0.022(4) C18 0.036(5) 0.014(4) 0.041(6) 0.001(4) -0.001(4) 0.007(4) C19 0.026(4) 0.014(4) 0.023(5) -0.001(3) -0.003(3) 0.008(3) C20 0.026(4) 0.022(4) 0.021(4) -0.002(3) -0.003(3) 0.016(4) C21 0.023(4) 0.015(4) 0.033(5) 0.004(3) -0.007(4) 0.006(3) C22 0.015(4) 0.022(4) 0.030(5) 0.012(4) -0.002(3) 0.010(3) C23 0.025(5) 0.024(5) 0.041(6) 0.010(4) -0.002(4) 0.009(4) C24 0.016(4) 0.020(5) 0.054(7) 0.019(4) 0.002(4) -0.003(4) C25 0.023(4) 0.039(5) 0.034(5) 0.018(4) 0.004(4) 0.014(4) C26 0.017(4) 0.032(5) 0.033(5) 0.015(4) 0.011(4) 0.016(4) C27 0.012(4) 0.018(4) 0.034(5) 0.013(4) 0.002(3) 0.007(3) C28 0.028(4) 0.025(4) 0.032(5) 0.009(4) 0.012(4) 0.018(4) C29 0.028(4) 0.016(4) 0.033(5) 0.007(4) -0.005(4) 0.011(4) C30 0.043(5) 0.015(4) 0.035(5) -0.003(4) -0.012(4) 0.010(4) C31 0.034(5) 0.021(4) 0.037(5) 0.000(4) -0.008(4) 0.015(4) C32 0.050(5) 0.018(4) 0.033(5) -0.001(4) -0.008(4) 0.018(4) C33 0.051(6) 0.024(4) 0.029(5) -0.003(4) -0.005(4) 0.023(4) C34 0.045(5) 0.026(5) 0.032(5) 0.005(4) -0.003(4) 0.018(4) C35 0.046(6) 0.028(5) 0.040(6) -0.003(4) -0.008(4) 0.019(4) C36 0.049(6) 0.028(5) 0.052(6) -0.007(4) -0.001(5) 0.023(5) C37 0.061(7) 0.037(5) 0.065(7) -0.008(5) -0.005(6) 0.033(5) C38 0.066(8) 0.079(9) 0.095(10) -0.029(7) -0.022(7) 0.045(7) C39 0.026(4) 0.032(5) 0.033(5) 0.009(4) 0.007(4) 0.017(4) C40 0.030(5) 0.032(5) 0.035(5) 0.013(4) 0.011(4) 0.018(4) C41 0.028(5) 0.038(5) 0.039(5) 0.002(4) 0.006(4) 0.019(4) C42 0.027(5) 0.038(5) 0.034(5) -0.001(4) 0.004(4) 0.018(4) C43 0.023(4) 0.042(5) 0.033(5) -0.001(4) 0.004(4) 0.013(4) C44 0.028(5) 0.036(5) 0.038(5) 0.004(4) 0.010(4) 0.012(4) C45 0.026(5) 0.043(5) 0.038(5) 0.007(4) 0.009(4) 0.017(4) C46 0.027(5) 0.042(5) 0.030(5) -0.004(4) 0.002(4) 0.013(4) C47 0.019(4) 0.045(6) 0.038(6) 0.002(4) 0.003(4) 0.007(4) C48 0.030(5) 0.047(6) 0.051(6) 0.006(5) -0.003(4) 0.019(5) C49 0.037(5) 0.029(5) 0.035(5) 0.013(4) -0.003(4) 0.014(4) C50 0.042(6) 0.083(8) 0.066(7) 0.039(6) 0.003(5) 0.034(6) C51 0.111(11) 0.092(10) 0.104(11) 0.057(9) 0.036(9) 0.072(9) C52 0.140(13) 0.037(7) 0.094(11) 0.023(7) 0.036(9) 0.025(8) C53 0.049(7) 0.088(9) 0.078(9) 0.014(7) -0.007(6) 0.024(7) C54 0.22(2) 0.089(12) 0.156(17) 0.031(11) 0.064(16) 0.098(14) C55 0.073(10) 0.114(13) 0.127(14) -0.002(11) -0.016(9) 0.038(9) C56 0.64(7) 0.28(3) 0.091(16) 0.040(18) 0.03(3) 0.36(4) C57 0.159(15) 0.31(3) 0.182(18) 0.17(2) -0.003(12) -0.047(19) C58 0.159(15) 0.31(3) 0.182(18) 0.17(2) -0.003(12) -0.047(19) C59 0.040(5) 0.039(5) 0.037(5) 0.017(4) 0.008(4) 0.028(4) C60 0.088(8) 0.046(6) 0.053(7) 0.005(5) 0.008(6) 0.052(6) C61 0.085(9) 0.050(7) 0.080(9) 0.004(6) -0.006(7) 0.036(7) C62 0.104(10) 0.063(8) 0.104(11) 0.002(7) 0.010(8) 0.058(8) C63 0.082(10) 0.078(9) 0.134(13) 0.007(9) 0.004(9) 0.047(8) C64 0.114(12) 0.080(10) 0.093(11) -0.012(8) -0.013(9) 0.056(9) C65 0.135(14) 0.132(14) 0.115(13) -0.013(10) -0.022(10) 0.099(13) C66 0.15(2) 0.38(4) 0.39(5) 0.04(4) -0.06(2) 0.19(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 C2 1.370(10) . ? O1 H1 0.8400 . ? O2 C3 1.381(10) . ? O2 H2 0.8400 . ? O3 C4 1.380(10) . ? O3 H3 0.8400 . ? O4 C9 1.380(9) . ? O4 H4 0.8400 . ? O5 C10 1.379(9) . ? O5 H5 0.8400 . ? O6 C11 1.377(9) . ? O6 H6 0.8400 . ? O7 C16 1.383(10) . ? O7 H7 0.8400 . ? O8 C17 1.357(10) . ? O8 H8 0.8400 . ? O9 C18 1.391(10) . ? O9 H9 0.8400 . ? O10 C23 1.351(10) . ? O10 H10 0.8400 . ? O11 C24 1.381(9) . ? O11 H11 0.8400 . ? O12 C25 1.383(10) . ? O12 H12 0.8400 . ? C1 C6 1.397(10) . ? C1 C2 1.402(11) . ? C1 C28 1.499(11) . ? C2 C3 1.371(12) . ? C3 C4 1.390(12) . ? C4 C5 1.373(11) . ? C5 C6 1.387(10) . ? C5 C7 1.547(10) . ? C6 H6A 0.9500 . ? C7 C8 1.527(11) . ? C7 C29 1.527(8) . ? C7 H7A 1.0000 . ? C8 C13 1.380(10) . ? C8 C9 1.399(10) . ? C9 C10 1.384(12) . ? C10 C11 1.368(12) . ? C11 C12 1.400(10) . ? C12 C13 1.394(10) . ? C12 C14 1.508(11) . ? C13 H13A 0.9500 . ? C14 C15 1.543(10) . ? C14 C39 1.555(8) . ? C14 H14A 1.0000 . ? C15 C20 1.387(10) . ? C15 C16 1.394(10) . ? C16 C17 1.393(12) . ? C17 C18 1.378(12) . ? C18 C19 1.382(10) . ? C19 C20 1.396(10) . ? C19 C21 1.517(10) . ? C20 H20A 0.9500 . ? C21 C49 1.513(9) . ? C21 C22 1.532(11) . ? C21 H21A 1.0000 . ? C22 C23 1.393(11) . ? C22 C27 1.398(10) . ? C23 C24 1.384(12) . ? C24 C25 1.385(12) . ? C25 C26 1.381(11) . ? C26 C27 1.382(11) . ? C26 C28 1.517(11) . ? C27 H27A 0.9500 . ? C28 C59 1.552(9) . ? C28 H28A 1.0000 . ? C29 C30 1.5525 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.5445 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.5606 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.5272 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.5483 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.5333 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.5699 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.5530 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.3294 . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C38 H38B 0.9500 . ? C39 C40 1.5255 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.5220 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.5448 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.5501 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.5520 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.5261 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.5216 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.5337 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.3559 . ? C47 H47A 0.9500 . ? C48 H48A 0.9500 . ? C48 H48B 0.9500 . ? C49 C50 1.5347 . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.5150 . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.4781 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.5591 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.3948 . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.6080 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.5224 . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.5540 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.5729 . ? C57 H57A 0.9500 . ? C58 H58A 0.9500 . ? C58 H58B 0.9500 . ? C59 C60 1.5428 . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.5547 . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.5027 . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.5076 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.5661 . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.5014 . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.7103 . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C67 1.5289 . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C68 1.1296 . ? C67 H67A 0.9500 . ? C68 H68A 0.9500 . ? C68 H68B 0.9500 . ? O1S C3S 1.1311 . ? O2S C2S 1.3474 . ? O2S C3S 1.5807 . ? C1S C2S 1.5008 . ? C1S H1SA 0.9800 . ? C1S H1SB 0.9800 . ? C1S H1SC 0.9800 . ? C2S H2SA 0.9900 . ? C2S H2SB 0.9900 . ? C3S C4S 1.0346 . ? C4S H4SA 0.9800 . ? C4S H4SB 0.9800 . ? C4S H4SC 0.9800 . ? O5S O5S 1.76(11) 3_765 ? O5S O5S 1.76(11) 2_645 ? C5S O3S 1.0662 . ? C5S C6S 1.4086 . ? C5S H5SA 0.9900 . ? C5S H5SB 0.9900 . ? C6S H6SA 0.9800 . ? C6S H6SB 0.9800 . ? C6S H6SC 0.9800 . ? O3S H3S 0.8400 . ? 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 O1 H1 109.5 . . ? C3 O2 H2 109.5 . . ? C4 O3 H3 109.5 . . ? C9 O4 H4 109.5 . . ? C10 O5 H5 109.5 . . ? C11 O6 H6 109.5 . . ? C16 O7 H7 109.5 . . ? C17 O8 H8 109.5 . . ? C18 O9 H9 109.5 . . ? C23 O10 H10 109.5 . . ? C24 O11 H11 109.5 . . ? C25 O12 H12 109.5 . . ? C6 C1 C2 116.1(7) . . ? C6 C1 C28 122.7(7) . . ? C2 C1 C28 121.2(7) . . ? C3 C2 O1 117.2(8) . . ? C3 C2 C1 121.3(8) . . ? O1 C2 C1 121.5(8) . . ? C2 C3 O2 119.6(9) . . ? C2 C3 C4 120.5(8) . . ? O2 C3 C4 119.8(9) . . ? C5 C4 O3 122.0(8) . . ? C5 C4 C3 120.4(8) . . ? O3 C4 C3 117.6(8) . . ? C4 C5 C6 118.1(7) . . ? C4 C5 C7 120.0(7) . . ? C6 C5 C7 121.9(7) . . ? C5 C6 C1 123.5(7) . . ? C5 C6 H6A 118.2 . . ? C1 C6 H6A 118.2 . . ? C8 C7 C29 111.5(6) . . ? C8 C7 C5 110.1(6) . . ? C29 C7 C5 112.5(6) . . ? C8 C7 H7A 107.5 . . ? C29 C7 H7A 107.5 . . ? C5 C7 H7A 107.5 . . ? C13 C8 C9 116.9(7) . . ? C13 C8 C7 122.6(6) . . ? C9 C8 C7 120.5(7) . . ? O4 C9 C10 118.6(7) . . ? O4 C9 C8 120.8(8) . . ? C10 C9 C8 120.7(7) . . ? C11 C10 O5 120.6(8) . . ? C11 C10 C9 120.4(7) . . ? O5 C10 C9 119.0(8) . . ? C10 C11 O6 117.3(7) . . ? C10 C11 C12 121.7(7) . . ? O6 C11 C12 121.0(8) . . ? C13 C12 C11 115.9(7) . . ? C13 C12 C14 122.9(6) . . ? C11 C12 C14 121.2(7) . . ? C8 C13 C12 124.5(7) . . ? C8 C13 H13A 117.8 . . ? C12 C13 H13A 117.8 . . ? C12 C14 C15 111.6(6) . . ? C12 C14 C39 114.4(6) . . ? C15 C14 C39 110.4(5) . . ? C12 C14 H14A 106.7 . . ? C15 C14 H14A 106.7 . . ? C39 C14 H14A 106.7 . . ? C20 C15 C16 117.4(7) . . ? C20 C15 C14 121.9(6) . . ? C16 C15 C14 120.7(7) . . ? O7 C16 C15 121.4(7) . . ? O7 C16 C17 117.9(7) . . ? C15 C16 C17 120.7(7) . . ? O8 C17 C18 120.6(8) . . ? O8 C17 C16 119.7(8) . . ? C18 C17 C16 119.7(7) . . ? C17 C18 C19 121.9(7) . . ? C17 C18 O9 116.9(7) . . ? C19 C18 O9 121.2(8) . . ? C18 C19 C20 117.0(7) . . ? C18 C19 C21 121.4(7) . . ? C20 C19 C21 121.7(6) . . ? C15 C20 C19 123.4(7) . . ? C15 C20 H20A 118.3 . . ? C19 C20 H20A 118.3 . . ? C19 C21 C49 114.1(6) . . ? C19 C21 C22 110.3(6) . . ? C49 C21 C22 112.2(6) . . ? C19 C21 H21A 106.6 . . ? C49 C21 H21A 106.6 . . ? C22 C21 H21A 106.6 . . ? C23 C22 C27 118.0(7) . . ? C23 C22 C21 120.7(7) . . ? C27 C22 C21 121.3(6) . . ? O10 C23 C24 117.7(7) . . ? O10 C23 C22 122.5(8) . . ? C24 C23 C22 119.9(8) . . ? O11 C24 C23 119.7(8) . . ? O11 C24 C25 119.7(9) . . ? C23 C24 C25 120.6(7) . . ? O12 C25 C26 120.4(8) . . ? O12 C25 C24 118.6(7) . . ? C26 C25 C24 121.0(8) . . ? C27 C26 C25 117.8(8) . . ? C27 C26 C28 121.2(7) . . ? C25 C26 C28 121.0(7) . . ? C26 C27 C22 122.7(7) . . ? C26 C27 H27A 118.6 . . ? C22 C27 H27A 118.6 . . ? C1 C28 C26 111.2(6) . . ? C1 C28 C59 115.8(6) . . ? C26 C28 C59 112.9(6) . . ? C1 C28 H28A 105.3 . . ? C26 C28 H28A 105.3 . . ? C59 C28 H28A 105.3 . . ? C7 C29 C30 112.1(4) . . ? C7 C29 H29A 109.2 . . ? C30 C29 H29A 109.2 . . ? C7 C29 H29B 109.2 . . ? C30 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? C31 C30 C29 110.2 . . ? C31 C30 H30A 109.6 . . ? C29 C30 H30A 109.6 . . ? C31 C30 H30B 109.6 . . ? C29 C30 H30B 109.6 . . ? H30A C30 H30B 108.1 . . ? C30 C31 C32 112.2 . . ? C30 C31 H31A 109.2 . . ? C32 C31 H31A 109.2 . . ? C30 C31 H31B 109.2 . . ? C32 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? C33 C32 C31 108.4 . . ? C33 C32 H32A 110.0 . . ? C31 C32 H32A 110.0 . . ? C33 C32 H32B 110.0 . . ? C31 C32 H32B 110.0 . . ? H32A C32 H32B 108.4 . . ? C32 C33 C34 113.0 . . ? C32 C33 H33A 109.0 . . ? C34 C33 H33A 109.0 . . ? C32 C33 H33B 109.0 . . ? C34 C33 H33B 109.0 . . ? H33A C33 H33B 107.8 . . ? C35 C34 C33 108.7 . . ? C35 C34 H34A 109.9 . . ? C33 C34 H34A 109.9 . . ? C35 C34 H34B 109.9 . . ? C33 C34 H34B 109.9 . . ? H34A C34 H34B 108.3 . . ? C34 C35 C36 111.5 . . ? C34 C35 H35A 109.3 . . ? C36 C35 H35A 109.3 . . ? C34 C35 H35B 109.3 . . ? C36 C35 H35B 109.3 . . ? H35A C35 H35B 108.0 . . ? C37 C36 C35 108.2 . . ? C37 C36 H36A 110.0 . . ? C35 C36 H36A 110.0 . . ? C37 C36 H36B 110.0 . . ? C35 C36 H36B 110.0 . . ? H36A C36 H36B 108.4 . . ? C38 C37 C36 124.1 . . ? C38 C37 H37A 118.0 . . ? C36 C37 H37A 118.0 . . ? C37 C38 H38A 120.0 . . ? C37 C38 H38B 120.0 . . ? H38A C38 H38B 120.0 . . ? C40 C39 C14 114.5(3) . . ? C40 C39 H39A 108.6 . . ? C14 C39 H39A 108.6 . . ? C40 C39 H39B 108.6 . . ? C14 C39 H39B 108.6 . . ? H39A C39 H39B 107.6 . . ? C41 C40 C39 114.2 . . ? C41 C40 H40A 108.7 . . ? C39 C40 H40A 108.7 . . ? C41 C40 H40B 108.7 . . ? C39 C40 H40B 108.7 . . ? H40A C40 H40B 107.6 . . ? C40 C41 C42 109.9 . . ? C40 C41 H41A 109.7 . . ? C42 C41 H41A 109.7 . . ? C40 C41 H41B 109.7 . . ? C42 C41 H41B 109.7 . . ? H41A C41 H41B 108.2 . . ? C41 C42 C43 111.1 . . ? C41 C42 H42A 109.4 . . ? C43 C42 H42A 109.4 . . ? C41 C42 H42B 109.4 . . ? C43 C42 H42B 109.4 . . ? H42A C42 H42B 108.0 . . ? C42 C43 C44 110.4 . . ? C42 C43 H43A 109.6 . . ? C44 C43 H43A 109.6 . . ? C42 C43 H43B 109.6 . . ? C44 C43 H43B 109.6 . . ? H43A C43 H43B 108.1 . . ? C45 C44 C43 111.2 . . ? C45 C44 H44A 109.4 . . ? C43 C44 H44A 109.4 . . ? C45 C44 H44B 109.4 . . ? C43 C44 H44B 109.4 . . ? H44A C44 H44B 108.0 . . ? C46 C45 C44 110.6 . . ? C46 C45 H45A 109.5 . . ? C44 C45 H45A 109.5 . . ? C46 C45 H45B 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 108.1 . . ? C45 C46 C47 115.1 . . ? C45 C46 H46A 108.5 . . ? C47 C46 H46A 108.5 . . ? C45 C46 H46B 108.5 . . ? C47 C46 H46B 108.5 . . ? H46A C46 H46B 107.5 . . ? C48 C47 C46 125.1 . . ? C48 C47 H47A 117.5 . . ? C46 C47 H47A 117.5 . . ? C47 C48 H48A 120.0 . . ? C47 C48 H48B 120.0 . . ? H48A C48 H48B 120.0 . . ? C21 C49 C50 112.2(5) . . ? C21 C49 H49A 109.2 . . ? C50 C49 H49A 109.2 . . ? C21 C49 H49B 109.2 . . ? C50 C49 H49B 109.2 . . ? H49A C49 H49B 107.9 . . ? C51 C50 C49 119.6 . . ? C51 C50 H50A 107.4 . . ? C49 C50 H50A 107.4 . . ? C51 C50 H50B 107.4 . . ? C49 C50 H50B 107.4 . . ? H50A C50 H50B 107.0 . . ? C52 C51 C50 112.5 . . ? C52 C51 H51A 109.1 . . ? C50 C51 H51A 109.1 . . ? C52 C51 H51B 109.1 . . ? C50 C51 H51B 109.1 . . ? H51A C51 H51B 107.8 . . ? C51 C52 C53 116.8 . . ? C51 C52 H52A 108.1 . . ? C53 C52 H52A 108.1 . . ? C51 C52 H52B 108.1 . . ? C53 C52 H52B 108.1 . . ? H52A C52 H52B 107.3 . . ? C54 C53 C52 114.0 . . ? C54 C53 H53A 108.8 . . ? C52 C53 H53A 108.8 . . ? C54 C53 H53B 108.8 . . ? C52 C53 H53B 108.8 . . ? H53A C53 H53B 107.7 . . ? C53 C54 C55 112.8 . . ? C53 C54 H54A 109.0 . . ? C55 C54 H54A 109.0 . . ? C53 C54 H54B 109.0 . . ? C55 C54 H54B 109.0 . . ? H54A C54 H54B 107.8 . . ? C56 C55 C54 108.0 . . ? C56 C55 H55A 110.1 . . ? C54 C55 H55A 110.1 . . ? C56 C55 H55B 110.1 . . ? C54 C55 H55B 110.1 . . ? H55A C55 H55B 108.4 . . ? C55 C56 C57 115.7 . . ? C55 C56 H56A 108.4 . . ? C57 C56 H56A 108.4 . . ? C55 C56 H56B 108.4 . . ? C57 C56 H56B 108.4 . . ? H56A C56 H56B 107.4 . . ? C56 C57 C58 125.2 . . ? C56 C57 H57A 117.4 . . ? C58 C57 H57A 117.4 . . ? C57 C58 H58A 120.0 . . ? C57 C58 H58B 120.0 . . ? H58A C58 H58B 120.0 . . ? C60 C59 C28 110.7(5) . . ? C60 C59 H59A 109.5 . . ? C28 C59 H59A 109.5 . . ? C60 C59 H59B 109.5 . . ? C28 C59 H59B 109.5 . . ? H59A C59 H59B 108.1 . . ? C59 C60 C61 109.8 . . ? C59 C60 H60A 109.7 . . ? C61 C60 H60A 109.7 . . ? C59 C60 H60B 109.7 . . ? C61 C60 H60B 109.7 . . ? H60A C60 H60B 108.2 . . ? C62 C61 C60 109.6 . . ? C62 C61 H61A 109.7 . . ? C60 C61 H61A 109.7 . . ? C62 C61 H61B 109.7 . . ? C60 C61 H61B 109.7 . . ? H61A C61 H61B 108.2 . . ? C61 C62 C63 112.3 . . ? C61 C62 H62A 109.1 . . ? C63 C62 H62A 109.1 . . ? C61 C62 H62B 109.1 . . ? C63 C62 H62B 109.1 . . ? H62A C62 H62B 107.9 . . ? C62 C63 C64 113.1 . . ? C62 C63 H63A 109.0 . . ? C64 C63 H63A 109.0 . . ? C62 C63 H63B 109.0 . . ? C64 C63 H63B 109.0 . . ? H63A C63 H63B 107.8 . . ? C65 C64 C63 110.2 . . ? C65 C64 H64A 109.6 . . ? C63 C64 H64A 109.6 . . ? C65 C64 H64B 109.6 . . ? C63 C64 H64B 109.6 . . ? H64A C64 H64B 108.1 . . ? C64 C65 C66 110.6 . . ? C64 C65 H65A 109.5 . . ? C66 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? C66 C65 H65B 109.5 . . ? H65A C65 H65B 108.1 . . ? C67 C66 C65 117.2 . . ? C67 C66 H66A 108.0 . . ? C65 C66 H66A 108.0 . . ? C67 C66 H66B 108.0 . . ? C65 C66 H66B 108.0 . . ? H66A C66 H66B 107.2 . . ? C68 C67 C66 127.3 . . ? C68 C67 H67A 116.3 . . ? C66 C67 H67A 116.3 . . ? C67 C68 H68A 120.0 . . ? C67 C68 H68B 120.0 . . ? H68A C68 H68B 120.0 . . ? C2S O2S C3S 141.6 . . ? C2S C1S H1SA 109.5 . . ? C2S C1S H1SB 109.5 . . ? H1SA C1S H1SB 109.5 . . ? C2S C1S H1SC 109.5 . . ? H1SA C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? O2S C2S C1S 100.1 . . ? O2S C2S H2SA 111.8 . . ? C1S C2S H2SA 111.8 . . ? O2S C2S H2SB 111.8 . . ? C1S C2S H2SB 111.8 . . ? H2SA C2S H2SB 109.5 . . ? C4S C3S O1S 126.9 . . ? C4S C3S O2S 120.6 . . ? O1S C3S O2S 109.6 . . ? C3S C4S H4SA 109.5 . . ? C3S C4S H4SB 109.5 . . ? H4SA C4S H4SB 109.5 . . ? C3S C4S H4SC 109.5 . . ? H4SA C4S H4SC 109.5 . . ? H4SB C4S H4SC 109.5 . . ? O5S O5S O5S 59.999(13) 3_765 2_645 ? O3S C5S C6S 126.4 . . ? O3S C5S H5SA 105.7 . . ? C6S C5S H5SA 105.7 . . ? O3S C5S H5SB 105.7 . . ? C6S C5S H5SB 105.7 . . ? H5SA C5S H5SB 106.2 . . ? C5S C6S H6SA 109.5 . . ? C5S C6S H6SB 109.5 . . ? H6SA C6S H6SB 109.5 . . ? C5S C6S H6SC 109.5 . . ? H6SA C6S H6SC 109.5 . . ? H6SB C6S H6SC 109.5 . . ? C5S O3S H3S 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.0(12) . . . . ? C28 C1 C2 C3 -178.1(8) . . . . ? C6 C1 C2 O1 179.3(7) . . . . ? C28 C1 C2 O1 1.2(12) . . . . ? O1 C2 C3 O2 3.0(13) . . . . ? C1 C2 C3 O2 -177.7(8) . . . . ? O1 C2 C3 C4 179.4(8) . . . . ? C1 C2 C3 C4 -1.3(13) . . . . ? C2 C3 C4 C5 1.5(13) . . . . ? O2 C3 C4 C5 177.9(8) . . . . ? C2 C3 C4 O3 -178.2(8) . . . . ? O2 C3 C4 O3 -1.9(13) . . . . ? O3 C4 C5 C6 179.4(7) . . . . ? C3 C4 C5 C6 -0.3(11) . . . . ? O3 C4 C5 C7 -1.5(11) . . . . ? C3 C4 C5 C7 178.8(7) . . . . ? C4 C5 C6 C1 -1.1(11) . . . . ? C7 C5 C6 C1 179.8(6) . . . . ? C2 C1 C6 C5 1.2(11) . . . . ? C28 C1 C6 C5 179.3(7) . . . . ? C4 C5 C7 C8 -88.1(8) . . . . ? C6 C5 C7 C8 91.0(8) . . . . ? C4 C5 C7 C29 146.9(7) . . . . ? C6 C5 C7 C29 -34.0(9) . . . . ? C29 C7 C8 C13 40.5(9) . . . . ? C5 C7 C8 C13 -85.1(8) . . . . ? C29 C7 C8 C9 -141.1(6) . . . . ? C5 C7 C8 C9 93.3(8) . . . . ? C13 C8 C9 O4 179.6(7) . . . . ? C7 C8 C9 O4 1.1(11) . . . . ? C13 C8 C9 C10 0.3(11) . . . . ? C7 C8 C9 C10 -178.3(7) . . . . ? O4 C9 C10 C11 179.5(7) . . . . ? C8 C9 C10 C11 -1.1(12) . . . . ? O4 C9 C10 O5 -1.0(11) . . . . ? C8 C9 C10 O5 178.4(7) . . . . ? O5 C10 C11 O6 1.8(11) . . . . ? C9 C10 C11 O6 -178.7(7) . . . . ? O5 C10 C11 C12 -178.7(7) . . . . ? C9 C10 C11 C12 0.8(12) . . . . ? C10 C11 C12 C13 0.2(11) . . . . ? O6 C11 C12 C13 179.7(6) . . . . ? C10 C11 C12 C14 179.2(7) . . . . ? O6 C11 C12 C14 -1.3(11) . . . . ? C9 C8 C13 C12 0.9(11) . . . . ? C7 C8 C13 C12 179.4(6) . . . . ? C11 C12 C13 C8 -1.1(11) . . . . ? C14 C12 C13 C8 179.9(7) . . . . ? C13 C12 C14 C15 85.9(8) . . . . ? C11 C12 C14 C15 -93.1(8) . . . . ? C13 C12 C14 C39 -40.3(9) . . . . ? C11 C12 C14 C39 140.7(6) . . . . ? C12 C14 C15 C20 -90.2(8) . . . . ? C39 C14 C15 C20 38.2(9) . . . . ? C12 C14 C15 C16 87.3(8) . . . . ? C39 C14 C15 C16 -144.3(7) . . . . ? C20 C15 C16 O7 177.5(7) . . . . ? C14 C15 C16 O7 -0.1(12) . . . . ? C20 C15 C16 C17 -1.5(12) . . . . ? C14 C15 C16 C17 -179.1(8) . . . . ? O7 C16 C17 O8 1.7(14) . . . . ? C15 C16 C17 O8 -179.2(8) . . . . ? O7 C16 C17 C18 -179.0(8) . . . . ? C15 C16 C17 C18 0.0(14) . . . . ? O8 C17 C18 C19 179.9(8) . . . . ? C16 C17 C18 C19 0.6(14) . . . . ? O8 C17 C18 O9 1.2(14) . . . . ? C16 C17 C18 O9 -178.1(8) . . . . ? C17 C18 C19 C20 0.3(13) . . . . ? O9 C18 C19 C20 178.9(7) . . . . ? C17 C18 C19 C21 178.7(8) . . . . ? O9 C18 C19 C21 -2.6(12) . . . . ? C16 C15 C20 C19 2.5(11) . . . . ? C14 C15 C20 C19 -179.9(7) . . . . ? C18 C19 C20 C15 -1.9(11) . . . . ? C21 C19 C20 C15 179.6(7) . . . . ? C18 C19 C21 C49 145.7(7) . . . . ? C20 C19 C21 C49 -35.9(10) . . . . ? C18 C19 C21 C22 -86.9(9) . . . . ? C20 C19 C21 C22 91.5(8) . . . . ? C19 C21 C22 C23 92.4(8) . . . . ? C49 C21 C22 C23 -139.2(7) . . . . ? C19 C21 C22 C27 -85.7(8) . . . . ? C49 C21 C22 C27 42.8(9) . . . . ? C27 C22 C23 O10 -179.6(7) . . . . ? C21 C22 C23 O10 2.3(11) . . . . ? C27 C22 C23 C24 -0.9(11) . . . . ? C21 C22 C23 C24 -179.0(7) . . . . ? O10 C23 C24 O11 -0.6(12) . . . . ? C22 C23 C24 O11 -179.4(7) . . . . ? O10 C23 C24 C25 178.5(7) . . . . ? C22 C23 C24 C25 -0.3(12) . . . . ? O11 C24 C25 O12 -0.4(12) . . . . ? C23 C24 C25 O12 -179.5(7) . . . . ? O11 C24 C25 C26 -179.9(7) . . . . ? C23 C24 C25 C26 1.0(12) . . . . ? O12 C25 C26 C27 180.0(7) . . . . ? C24 C25 C26 C27 -0.5(11) . . . . ? O12 C25 C26 C28 0.9(11) . . . . ? C24 C25 C26 C28 -179.5(7) . . . . ? C25 C26 C27 C22 -0.7(11) . . . . ? C28 C26 C27 C22 178.3(7) . . . . ? C23 C22 C27 C26 1.4(11) . . . . ? C21 C22 C27 C26 179.5(6) . . . . ? C6 C1 C28 C26 -91.1(8) . . . . ? C2 C1 C28 C26 86.9(9) . . . . ? C6 C1 C28 C59 39.6(10) . . . . ? C2 C1 C28 C59 -142.4(7) . . . . ? C27 C26 C28 C1 86.5(9) . . . . ? C25 C26 C28 C1 -94.4(8) . . . . ? C27 C26 C28 C59 -45.6(9) . . . . ? C25 C26 C28 C59 133.4(7) . . . . ? C8 C7 C29 C30 172.3(4) . . . . ? C5 C7 C29 C30 -63.5(6) . . . . ? C7 C29 C30 C31 157.8(4) . . . . ? C29 C30 C31 C32 -177.8 . . . . ? C30 C31 C32 C33 174.9 . . . . ? C31 C32 C33 C34 -176.8 . . . . ? C32 C33 C34 C35 175.1 . . . . ? C33 C34 C35 C36 -175.5 . . . . ? C34 C35 C36 C37 179.3 . . . . ? C35 C36 C37 C38 -113.7 . . . . ? C12 C14 C39 C40 -53.0(6) . . . . ? C15 C14 C39 C40 -179.9(4) . . . . ? C14 C39 C40 C41 -58.0(5) . . . . ? C39 C40 C41 C42 -172.8 . . . . ? C40 C41 C42 C43 -170.9 . . . . ? C41 C42 C43 C44 172.4 . . . . ? C42 C43 C44 C45 178.8 . . . . ? C43 C44 C45 C46 177.3 . . . . ? C44 C45 C46 C47 178.2 . . . . ? C45 C46 C47 C48 -0.4 . . . . ? C19 C21 C49 C50 -165.1(5) . . . . ? C22 C21 C49 C50 68.5(6) . . . . ? C21 C49 C50 C51 -167.5(5) . . . . ? C49 C50 C51 C52 93.9 . . . . ? C50 C51 C52 C53 178.9 . . . . ? C51 C52 C53 C54 -163.9 . . . . ? C52 C53 C54 C55 161.3 . . . . ? C53 C54 C55 C56 -179.6 . . . . ? C54 C55 C56 C57 167.7 . . . . ? C55 C56 C57 C58 122.6 . . . . ? C1 C28 C59 C60 64.9(7) . . . . ? C26 C28 C59 C60 -165.3(5) . . . . ? C28 C59 C60 C61 158.6(4) . . . . ? C59 C60 C61 C62 -174.3 . . . . ? C60 C61 C62 C63 167.0 . . . . ? C61 C62 C63 C64 -79.6 . . . . ? C62 C63 C64 C65 -164.3 . . . . ? C63 C64 C65 C66 173.8 . . . . ? C64 C65 C66 C67 175.1 . . . . ? C65 C66 C67 C68 145.3 . . . . ? C3S O2S C2S C1S 86.2 . . . . ? C2S O2S C3S C4S 170.6 . . . . ? C2S O2S C3S O1S -27.5 . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.126 _refine_diff_density_min -1.078 _refine_diff_density_rms 0.157