#------------------------------------------------------------------------------ #$Date: 2024-07-09 01:21:09 +0300 (Tue, 09 Jul 2024) $ #$Revision: 293308 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572104.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1572104 loop_ _publ_author_name 'Jenek, Niko A.' 'Helbig, Andreas' 'Boyt, Stuart M.' 'Kaur, M.' 'Sanderson, Hugh J.' 'Reeksting, Shaun Bernard' 'Kociok-K\"ohn, Gabriele' 'Helten, Holger' 'Hintermair, Ulrich' _publ_section_title ; Understanding and tuning the electronic structure of pentalenides ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D3SC04622B _journal_year 2024 _chemical_formula_moiety 'C60 H78 Na2 O6' _chemical_formula_sum 'C60 H78 Na2 O6' _chemical_formula_weight 941.20 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2023-07-12 deposited with the CCDC. 2024-07-02 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 93.4414(5) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 11.56222(7) _cell_length_b 12.72345(7) _cell_length_c 18.05699(10) _cell_measurement_reflns_used 37614 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 72.8670 _cell_measurement_theta_min 5.1710 _cell_volume 2651.60(3) _computing_cell_refinement 'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)' _computing_data_collection 'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)' _computing_data_reduction 'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)' _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _computing_structure_refinement ; SHELXL-2018/3 (Sheldrick, 2018) Sheldrick GM (2008) Acta Crystallogr A64:112--122 and C. B. H\"ubschle, G. M. Sheldrick and B. Dittrich ShelXle: a Qt graphical user interface for SHELXL J. Appl. Cryst., 44, (2011) 1281-1284. ; _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 150.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.1150 _diffrn_detector_type EosS2 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, EosS2' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_unetI/netI 0.0111 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 57489 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 72.894 _diffrn_reflns_theta_min 4.253 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.720 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.70894 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.179 _exptl_crystal_description block _exptl_crystal_F_000 1016 _exptl_crystal_size_max 0.613 _exptl_crystal_size_mid 0.582 _exptl_crystal_size_min 0.344 _refine_diff_density_max 0.267 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.038 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 346 _refine_ls_number_reflns 5290 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0437 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+1.0282P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1145 _refine_ls_wR_factor_ref 0.1154 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5091 _reflns_number_total 5290 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3sc04622b2.cif _cod_data_source_block s22uh31 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1572104 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.667 _shelx_estimated_absorpt_t_max 0.790 _oxdiff_exptl_absorpt_empirical_full_min 0.662 _oxdiff_exptl_absorpt_empirical_full_max 1.483 _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _shelx_res_file ; TITL shelxt_a.res in P2(1)/n s22uh31.res created by SHELXL-2018/3 at 13:37:10 on 28-Nov-2022 CELL 1.54184 11.56222 12.72345 18.05699 90.000 93.4414 90.000 ZERR 2 0.00007 0.00007 0.00010 0.000 0.0005 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H O NA UNIT 120 156 12 4 ACTA FMAP 2 PLAN 10 BOND $H CONF LIST 4 L.S. 10 TEMP -123.00 SIZE 0.344 0.582 0.613 WGHT 0.056400 1.028200 FVAR 6.30417 0.43032 NA 4 0.529488 0.697371 0.477664 11.00000 0.04854 0.03125 = 0.03144 0.00056 -0.00293 0.00353 C1 1 0.530733 0.505729 0.535704 11.00000 0.02139 0.02553 = 0.02090 0.00217 -0.00073 -0.00101 C2 1 0.447540 0.499302 0.592294 11.00000 0.02191 0.02717 = 0.02165 0.00291 0.00091 -0.00022 C3 1 0.459447 0.531070 0.670175 11.00000 0.02279 0.02626 = 0.02190 0.00376 0.00074 0.00259 C4 1 0.549811 0.596233 0.698390 11.00000 0.02472 0.03059 = 0.02663 0.00155 0.00265 -0.00114 AFIX 43 H4 2 0.610448 0.614073 0.667437 11.00000 -1.20000 AFIX 0 C5 1 0.552852 0.635218 0.770244 11.00000 0.02979 0.03765 = 0.03017 -0.00344 -0.00080 -0.00264 AFIX 43 H5 2 0.615507 0.679075 0.787116 11.00000 -1.20000 AFIX 0 C6 1 0.466714 0.611889 0.818292 11.00000 0.03334 0.04283 = 0.02327 -0.00107 0.00024 0.00571 C7 1 0.468149 0.657772 0.895508 11.00000 0.04904 0.07008 = 0.02800 -0.00973 0.00270 0.00037 AFIX 137 H7A 2 0.517904 0.720177 0.898234 11.00000 -1.50000 H7B 2 0.498259 0.605416 0.931511 11.00000 -1.50000 H7C 2 0.389216 0.677488 0.906869 11.00000 -1.50000 AFIX 0 C8 1 0.378526 0.545037 0.791766 11.00000 0.02872 0.04458 = 0.02441 0.00471 0.00559 0.00204 AFIX 43 H8 2 0.319265 0.526112 0.823479 11.00000 -1.20000 AFIX 0 C9 1 0.374991 0.505333 0.720155 11.00000 0.02458 0.03681 = 0.02523 0.00314 0.00142 -0.00263 AFIX 43 H9 2 0.313668 0.459336 0.704336 11.00000 -1.20000 AFIX 0 C10 1 0.339069 0.479994 0.554184 11.00000 0.02137 0.03010 = 0.02356 0.00302 0.00226 -0.00103 AFIX 43 H10 2 0.269008 0.468677 0.577930 11.00000 -1.20000 AFIX 0 C11 1 0.347840 0.479623 0.476244 11.00000 0.02093 0.02637 = 0.02339 0.00220 0.00009 -0.00073 C12 1 0.247552 0.494574 0.424345 11.00000 0.02078 0.02549 = 0.02275 -0.00254 0.00003 -0.00046 C13 1 0.255326 0.552210 0.358483 11.00000 0.02158 0.02858 = 0.02662 0.00103 0.00121 -0.00097 AFIX 43 H13 2 0.329313 0.573744 0.343966 11.00000 -1.20000 AFIX 0 C14 1 0.157490 0.578382 0.314184 11.00000 0.02756 0.03472 = 0.02605 0.00293 -0.00229 0.00022 AFIX 43 H14 2 0.166065 0.617425 0.270005 11.00000 -1.20000 AFIX 0 C15 1 0.046961 0.548877 0.332820 11.00000 0.02291 0.03888 = 0.03058 -0.00425 -0.00474 0.00197 C16 1 -0.059061 0.581858 0.285891 11.00000 0.02672 0.06444 = 0.04616 0.00412 -0.01018 0.00246 AFIX 137 H16A 2 -0.035759 0.625872 0.244812 11.00000 -1.50000 H16B 2 -0.110916 0.621847 0.316348 11.00000 -1.50000 H16C 2 -0.099437 0.519297 0.266002 11.00000 -1.50000 AFIX 0 C17 1 0.038618 0.489336 0.396905 11.00000 0.02013 0.04070 = 0.03004 -0.00686 0.00285 -0.00415 AFIX 43 H17 2 -0.035532 0.466998 0.410608 11.00000 -1.20000 AFIX 0 C18 1 0.135776 0.461892 0.441147 11.00000 0.02420 0.03374 = 0.02385 -0.00168 0.00278 -0.00407 AFIX 43 H18 2 0.126839 0.419934 0.483946 11.00000 -1.20000 AFIX 0 O1 3 0.367117 0.782409 0.524482 11.00000 0.05390 0.05600 = 0.03227 -0.00324 0.00094 0.01233 C21 1 0.378503 0.813863 0.601015 11.00000 0.05063 0.05792 = 0.03161 -0.00115 -0.00398 0.00852 AFIX 23 H21A 2 0.383723 0.891338 0.605037 11.00000 -1.20000 H21B 2 0.449118 0.782766 0.625835 11.00000 -1.20000 AFIX 0 C22 1 0.271658 0.774244 0.636214 11.00000 0.06113 0.04714 = 0.03517 0.00232 0.00243 0.00702 AFIX 23 H22A 2 0.250226 0.820643 0.677216 11.00000 -1.20000 H22B 2 0.282903 0.701775 0.655270 11.00000 -1.20000 AFIX 0 C23 1 0.180903 0.777737 0.571624 11.00000 0.05613 0.05042 = 0.04326 -0.00020 0.00097 -0.00748 AFIX 23 H23A 2 0.117285 0.727347 0.578762 11.00000 -1.20000 H23B 2 0.148157 0.849198 0.564674 11.00000 -1.20000 AFIX 0 C24 1 0.250780 0.746254 0.507311 11.00000 0.06502 0.04116 = 0.03934 -0.00566 -0.00616 0.00136 AFIX 23 H24A 2 0.249640 0.668963 0.500995 11.00000 -1.20000 H24B 2 0.218474 0.779038 0.460837 11.00000 -1.20000 AFIX 0 O2 3 0.659264 0.816196 0.535171 11.00000 0.06683 0.03581 = 0.05846 0.00254 -0.01640 -0.00373 PART 1 C25 1 0.640714 0.923875 0.525847 21.00000 0.06712 0.03282 = 0.07240 -0.00354 -0.01536 0.00048 AFIX 23 H25A 2 0.588399 0.951746 0.562594 21.00000 -1.20000 H25B 2 0.608320 0.940367 0.475183 21.00000 -1.20000 AFIX 0 C26 1 0.767812 0.968228 0.539621 21.00000 0.07933 0.01934 = 0.04717 0.00691 0.03225 0.00123 AFIX 23 H26A 2 0.815040 0.956364 0.496438 21.00000 -1.20000 H26B 2 0.768031 1.043951 0.552238 21.00000 -1.20000 AFIX 0 C27 1 0.806892 0.902873 0.603486 21.00000 0.06945 0.04730 = 0.11678 0.02010 -0.02616 -0.01642 AFIX 23 H27A 2 0.892514 0.899505 0.609080 21.00000 -1.20000 H27B 2 0.776819 0.929835 0.650033 21.00000 -1.20000 AFIX 0 C28 1 0.757161 0.800346 0.583808 21.00000 0.08081 0.05661 = 0.10317 0.03647 -0.02932 -0.01178 AFIX 23 H28A 2 0.814841 0.756726 0.559529 21.00000 -1.20000 H28B 2 0.734737 0.763372 0.629009 21.00000 -1.20000 AFIX 0 PART 2 C25A 1 0.674832 0.925429 0.511367 -21.00000 0.06586 0.04022 = 0.08133 0.01962 -0.00631 0.00132 AFIX 23 H25C 2 0.685490 0.928193 0.457410 -21.00000 -1.20000 H25D 2 0.605944 0.967888 0.521840 -21.00000 -1.20000 AFIX 0 C26A 1 0.777871 0.966464 0.552961 -21.00000 0.08157 0.06018 = 0.11892 -0.00286 -0.00229 -0.01832 AFIX 23 H26C 2 0.755731 1.019372 0.589738 -21.00000 -1.20000 H26D 2 0.831102 0.999725 0.518964 -21.00000 -1.20000 AFIX 0 C27A 1 0.834157 0.874342 0.590847 -21.00000 0.04761 0.05758 = 0.06007 0.01470 -0.00255 -0.00810 AFIX 23 H27C 2 0.871628 0.894253 0.639568 -21.00000 -1.20000 H27D 2 0.892591 0.842043 0.560031 -21.00000 -1.20000 AFIX 0 C28A 1 0.731913 0.800433 0.599865 -21.00000 0.05212 0.03780 = 0.02882 0.00156 0.00374 -0.01289 AFIX 23 H28C 2 0.758214 0.726470 0.603561 -21.00000 -1.20000 H28D 2 0.691045 0.818391 0.644807 -21.00000 -1.20000 AFIX 0 PART 0 O3 3 0.515334 0.797362 0.370245 11.00000 0.08015 0.05884 = 0.03272 0.00617 0.00190 0.01828 C29 1 0.589773 0.780698 0.311535 11.00000 0.04780 0.06819 = 0.05865 0.01500 0.00970 0.00265 AFIX 23 H29A 2 0.637946 0.717312 0.321329 11.00000 -1.20000 H29B 2 0.641691 0.841849 0.306589 11.00000 -1.20000 AFIX 0 C30 1 0.514208 0.766689 0.242666 11.00000 0.09825 0.07401 = 0.03850 0.00121 0.00409 0.03483 AFIX 23 H30A 2 0.514301 0.692366 0.226444 11.00000 -1.20000 H30B 2 0.541552 0.811083 0.202221 11.00000 -1.20000 AFIX 0 C31 1 0.394873 0.799452 0.261923 11.00000 0.05651 0.05806 = 0.05918 0.02307 -0.00257 -0.00681 AFIX 23 H31A 2 0.361006 0.850532 0.225380 11.00000 -1.20000 H31B 2 0.342689 0.737972 0.264014 11.00000 -1.20000 AFIX 0 C32 1 0.414881 0.848524 0.336212 11.00000 0.08463 0.07795 = 0.05160 0.02536 0.02601 0.04169 AFIX 23 H32A 2 0.428766 0.924933 0.331416 11.00000 -1.20000 H32B 2 0.346955 0.837846 0.366227 11.00000 -1.20000 AFIX 0 HKLF 4 REM shelxt_a.res in P2(1)/n REM wR2 = 0.1154, GooF = S = 1.043, Restrained GooF = 1.043 for all data REM R1 = 0.0437 for 5091 Fo > 4sig(Fo) and 0.0448 for all 5290 data REM 346 parameters refined using 0 restraints END WGHT 0.0564 1.0283 REM Highest difference peak 0.267, deepest hole -0.284, 1-sigma level 0.038 Q1 1 0.5000 0.5000 0.5000 10.50000 0.05 0.27 Q2 1 0.4821 0.8658 0.3600 11.00000 0.05 0.25 Q3 1 0.2983 0.4865 0.4486 11.00000 0.05 0.25 Q4 1 0.2609 0.5107 0.5810 11.00000 0.05 0.23 Q5 1 -0.0566 0.5537 0.2354 11.00000 0.05 0.23 Q6 1 0.2123 0.7173 0.5852 11.00000 0.05 0.22 Q7 1 0.4531 0.5114 0.6314 11.00000 0.05 0.22 Q8 1 0.3950 0.4862 0.5780 11.00000 0.05 0.21 Q9 1 -0.0635 0.6649 0.2773 11.00000 0.05 0.21 Q10 1 0.5852 0.8104 0.3823 11.00000 0.05 0.21 ; _shelx_res_checksum 40806 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Na Na 0.52949(5) 0.69737(4) 0.47766(3) 0.03729(15) Uani 1 1 d . . . . . C1 C 0.53073(10) 0.50573(9) 0.53570(6) 0.0227(2) Uani 1 1 d . . . . . C2 C 0.44754(10) 0.49930(9) 0.59229(6) 0.0236(2) Uani 1 1 d . . . . . C3 C 0.45945(10) 0.53107(9) 0.67017(6) 0.0237(2) Uani 1 1 d . . . . . C4 C 0.54981(10) 0.59623(10) 0.69839(7) 0.0273(3) Uani 1 1 d . . . . . H4 H 0.610448 0.614073 0.667437 0.033 Uiso 1 1 calc R U . . . C5 C 0.55285(11) 0.63522(11) 0.77024(7) 0.0326(3) Uani 1 1 d . . . . . H5 H 0.615507 0.679075 0.787116 0.039 Uiso 1 1 calc R U . . . C6 C 0.46671(11) 0.61189(11) 0.81829(7) 0.0332(3) Uani 1 1 d . . . . . C7 C 0.46815(15) 0.65777(15) 0.89551(8) 0.0490(4) Uani 1 1 d . . . . . H7A H 0.517904 0.720177 0.898234 0.074 Uiso 1 1 calc R U . . . H7B H 0.498259 0.605416 0.931511 0.074 Uiso 1 1 calc R U . . . H7C H 0.389216 0.677488 0.906869 0.074 Uiso 1 1 calc R U . . . C8 C 0.37853(11) 0.54504(11) 0.79177(7) 0.0324(3) Uani 1 1 d . . . . . H8 H 0.319265 0.526112 0.823479 0.039 Uiso 1 1 calc R U . . . C9 C 0.37499(11) 0.50533(10) 0.72016(7) 0.0289(3) Uani 1 1 d . . . . . H9 H 0.313668 0.459336 0.704336 0.035 Uiso 1 1 calc R U . . . C10 C 0.33907(10) 0.47999(9) 0.55418(6) 0.0250(2) Uani 1 1 d . . . . . H10 H 0.269008 0.468677 0.577930 0.030 Uiso 1 1 calc R U . . . C11 C 0.34784(10) 0.47962(9) 0.47624(6) 0.0236(2) Uani 1 1 d . . . . . C12 C 0.24755(10) 0.49457(9) 0.42434(6) 0.0231(2) Uani 1 1 d . . . . . C13 C 0.25533(10) 0.55221(9) 0.35848(6) 0.0256(2) Uani 1 1 d . . . . . H13 H 0.329313 0.573744 0.343966 0.031 Uiso 1 1 calc R U . . . C14 C 0.15749(10) 0.57838(10) 0.31418(7) 0.0296(3) Uani 1 1 d . . . . . H14 H 0.166065 0.617425 0.270005 0.036 Uiso 1 1 calc R U . . . C15 C 0.04696(10) 0.54888(11) 0.33282(7) 0.0310(3) Uani 1 1 d . . . . . C16 C -0.05906(12) 0.58186(14) 0.28589(9) 0.0463(4) Uani 1 1 d . . . . . H16A H -0.035759 0.625872 0.244812 0.069 Uiso 1 1 calc R U . . . H16B H -0.110916 0.621847 0.316348 0.069 Uiso 1 1 calc R U . . . H16C H -0.099437 0.519297 0.266002 0.069 Uiso 1 1 calc R U . . . C17 C 0.03862(10) 0.48934(11) 0.39691(7) 0.0302(3) Uani 1 1 d . . . . . H17 H -0.035532 0.466998 0.410608 0.036 Uiso 1 1 calc R U . . . C18 C 0.13578(10) 0.46189(10) 0.44115(7) 0.0272(3) Uani 1 1 d . . . . . H18 H 0.126839 0.419934 0.483946 0.033 Uiso 1 1 calc R U . . . O1 O 0.36712(10) 0.78241(9) 0.52448(6) 0.0475(3) Uani 1 1 d . . . . . C21 C 0.37850(14) 0.81386(14) 0.60102(8) 0.0470(4) Uani 1 1 d . . . . . H21A H 0.383723 0.891338 0.605037 0.056 Uiso 1 1 calc R U . . . H21B H 0.449118 0.782766 0.625835 0.056 Uiso 1 1 calc R U . . . C22 C 0.27166(15) 0.77424(14) 0.63621(8) 0.0478(4) Uani 1 1 d . . . . . H22A H 0.250226 0.820643 0.677216 0.057 Uiso 1 1 calc R U . . . H22B H 0.282903 0.701775 0.655270 0.057 Uiso 1 1 calc R U . . . C23 C 0.18090(15) 0.77774(14) 0.57162(9) 0.0500(4) Uani 1 1 d . . . . . H23A H 0.117285 0.727347 0.578762 0.060 Uiso 1 1 calc R U . . . H23B H 0.148157 0.849198 0.564674 0.060 Uiso 1 1 calc R U . . . C24 C 0.25078(15) 0.74625(13) 0.50731(9) 0.0489(4) Uani 1 1 d . . . . . H24A H 0.249640 0.668963 0.500995 0.059 Uiso 1 1 calc R U . . . H24B H 0.218474 0.779038 0.460837 0.059 Uiso 1 1 calc R U . . . O2 O 0.65926(11) 0.81620(9) 0.53517(7) 0.0545(3) Uani 1 1 d . . . . . C25 C 0.6407(11) 0.9239(10) 0.5258(7) 0.058(2) Uani 0.430(13) 1 d . . P A 1 H25A H 0.588399 0.951746 0.562594 0.070 Uiso 0.430(13) 1 calc R U P A 1 H25B H 0.608320 0.940367 0.475183 0.070 Uiso 0.430(13) 1 calc R U P A 1 C26 C 0.7678(12) 0.9682(7) 0.5396(6) 0.047(3) Uani 0.430(13) 1 d . . P A 1 H26A H 0.815040 0.956364 0.496438 0.057 Uiso 0.430(13) 1 calc R U P A 1 H26B H 0.768031 1.043951 0.552238 0.057 Uiso 0.430(13) 1 calc R U P A 1 C27 C 0.8069(13) 0.9029(10) 0.6035(9) 0.079(3) Uani 0.430(13) 1 d . . P A 1 H27A H 0.892514 0.899505 0.609080 0.095 Uiso 0.430(13) 1 calc R U P A 1 H27B H 0.776819 0.929835 0.650033 0.095 Uiso 0.430(13) 1 calc R U P A 1 C28 C 0.7572(13) 0.8003(10) 0.5838(8) 0.082(3) Uani 0.430(13) 1 d . . P A 1 H28A H 0.814841 0.756726 0.559529 0.098 Uiso 0.430(13) 1 calc R U P A 1 H28B H 0.734737 0.763372 0.629009 0.098 Uiso 0.430(13) 1 calc R U P A 1 C25A C 0.6748(8) 0.9254(8) 0.5114(6) 0.063(2) Uani 0.570(13) 1 d . . P A 2 H25C H 0.685490 0.928193 0.457410 0.075 Uiso 0.570(13) 1 calc R U P A 2 H25D H 0.605944 0.967888 0.521840 0.075 Uiso 0.570(13) 1 calc R U P A 2 C26A C 0.7779(13) 0.9665(9) 0.5530(7) 0.087(3) Uani 0.570(13) 1 d . . P A 2 H26C H 0.755731 1.019372 0.589738 0.105 Uiso 0.570(13) 1 calc R U P A 2 H26D H 0.831102 0.999725 0.518964 0.105 Uiso 0.570(13) 1 calc R U P A 2 C27A C 0.8342(7) 0.8743(7) 0.5908(5) 0.0553(16) Uani 0.570(13) 1 d . . P A 2 H27C H 0.871628 0.894253 0.639568 0.066 Uiso 0.570(13) 1 calc R U P A 2 H27D H 0.892591 0.842043 0.560031 0.066 Uiso 0.570(13) 1 calc R U P A 2 C28A C 0.7319(7) 0.8004(6) 0.5999(3) 0.0395(11) Uani 0.570(13) 1 d . . P A 2 H28C H 0.758214 0.726470 0.603561 0.047 Uiso 0.570(13) 1 calc R U P A 2 H28D H 0.691045 0.818391 0.644807 0.047 Uiso 0.570(13) 1 calc R U P A 2 O3 O 0.51533(12) 0.79736(10) 0.37025(6) 0.0573(3) Uani 1 1 d . . . . . C29 C 0.58977(16) 0.78070(17) 0.31154(10) 0.0580(4) Uani 1 1 d . . . . . H29A H 0.637946 0.717312 0.321329 0.070 Uiso 1 1 calc R U . . . H29B H 0.641691 0.841849 0.306589 0.070 Uiso 1 1 calc R U . . . C30 C 0.5142(2) 0.76669(18) 0.24267(10) 0.0703(6) Uani 1 1 d . . . . . H30A H 0.514301 0.692366 0.226444 0.084 Uiso 1 1 calc R U . . . H30B H 0.541552 0.811083 0.202221 0.084 Uiso 1 1 calc R U . . . C31 C 0.39487(16) 0.79945(15) 0.26192(11) 0.0582(5) Uani 1 1 d . . . . . H31A H 0.361006 0.850532 0.225380 0.070 Uiso 1 1 calc R U . . . H31B H 0.342689 0.737972 0.264014 0.070 Uiso 1 1 calc R U . . . C32 C 0.4149(2) 0.84852(18) 0.33621(11) 0.0705(6) Uani 1 1 d . . . . . H32A H 0.428766 0.924933 0.331416 0.085 Uiso 1 1 calc R U . . . H32B H 0.346955 0.837846 0.366227 0.085 Uiso 1 1 calc R U . . . 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 Na 0.0485(3) 0.0313(3) 0.0314(3) 0.0006(2) -0.0029(2) 0.0035(2) C1 0.0214(5) 0.0255(5) 0.0209(5) 0.0022(4) -0.0007(4) -0.0010(4) C2 0.0219(5) 0.0272(6) 0.0216(5) 0.0029(4) 0.0009(4) -0.0002(4) C3 0.0228(5) 0.0263(6) 0.0219(5) 0.0038(4) 0.0007(4) 0.0026(4) C4 0.0247(6) 0.0306(6) 0.0266(6) 0.0016(5) 0.0026(4) -0.0011(5) C5 0.0298(6) 0.0377(7) 0.0302(6) -0.0034(5) -0.0008(5) -0.0026(5) C6 0.0333(6) 0.0428(7) 0.0233(6) -0.0011(5) 0.0002(5) 0.0057(5) C7 0.0490(9) 0.0701(11) 0.0280(7) -0.0097(7) 0.0027(6) 0.0004(8) C8 0.0287(6) 0.0446(7) 0.0244(6) 0.0047(5) 0.0056(5) 0.0020(5) C9 0.0246(6) 0.0368(7) 0.0252(6) 0.0031(5) 0.0014(5) -0.0026(5) C10 0.0214(5) 0.0301(6) 0.0236(6) 0.0030(4) 0.0023(4) -0.0010(4) C11 0.0209(5) 0.0264(6) 0.0234(5) 0.0022(4) 0.0001(4) -0.0007(4) C12 0.0208(5) 0.0255(5) 0.0227(5) -0.0025(4) 0.0000(4) -0.0005(4) C13 0.0216(5) 0.0286(6) 0.0266(6) 0.0010(5) 0.0012(4) -0.0010(4) C14 0.0276(6) 0.0347(6) 0.0260(6) 0.0029(5) -0.0023(5) 0.0002(5) C15 0.0229(6) 0.0389(7) 0.0306(6) -0.0043(5) -0.0047(5) 0.0020(5) C16 0.0267(7) 0.0644(10) 0.0462(8) 0.0041(7) -0.0102(6) 0.0025(6) C17 0.0201(5) 0.0407(7) 0.0300(6) -0.0069(5) 0.0028(5) -0.0041(5) C18 0.0242(6) 0.0337(6) 0.0238(6) -0.0017(5) 0.0028(4) -0.0041(5) O1 0.0539(6) 0.0560(7) 0.0323(5) -0.0032(5) 0.0009(5) 0.0123(5) C21 0.0506(9) 0.0579(10) 0.0316(7) -0.0012(6) -0.0040(6) 0.0085(7) C22 0.0611(10) 0.0471(9) 0.0352(8) 0.0023(6) 0.0024(7) 0.0070(7) C23 0.0561(10) 0.0504(9) 0.0433(8) -0.0002(7) 0.0010(7) -0.0075(7) C24 0.0650(10) 0.0412(8) 0.0393(8) -0.0057(6) -0.0062(7) 0.0014(7) O2 0.0668(8) 0.0358(6) 0.0585(7) 0.0025(5) -0.0164(6) -0.0037(5) C25 0.067(6) 0.033(3) 0.072(5) -0.004(3) -0.015(4) 0.000(4) C26 0.079(7) 0.019(3) 0.047(3) 0.007(2) 0.032(4) 0.001(3) C27 0.069(7) 0.047(5) 0.117(9) 0.020(5) -0.026(5) -0.016(4) C28 0.081(7) 0.057(4) 0.103(9) 0.036(5) -0.029(5) -0.012(4) C25A 0.066(5) 0.040(2) 0.081(4) 0.020(3) -0.006(3) 0.001(3) C26A 0.082(5) 0.060(5) 0.119(8) -0.003(4) -0.002(5) -0.018(4) C27A 0.048(3) 0.058(5) 0.060(2) 0.015(3) -0.0026(18) -0.008(2) C28A 0.052(2) 0.038(2) 0.0288(16) 0.0016(14) 0.0037(14) -0.0129(16) O3 0.0801(9) 0.0588(7) 0.0327(6) 0.0062(5) 0.0019(5) 0.0183(6) C29 0.0478(9) 0.0682(11) 0.0586(10) 0.0150(9) 0.0097(8) 0.0027(8) C30 0.0982(16) 0.0740(13) 0.0385(9) 0.0012(9) 0.0041(9) 0.0348(12) C31 0.0565(10) 0.0581(11) 0.0592(11) 0.0231(8) -0.0026(8) -0.0068(8) C32 0.0846(14) 0.0779(13) 0.0516(10) 0.0254(10) 0.0260(10) 0.0417(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O3 Na O2 91.61(5) . . ? O3 Na O1 91.74(5) . . ? O2 Na O1 92.73(5) . . ? O3 Na C1 146.46(5) . . ? O2 Na C1 115.60(4) . . ? O1 Na C1 105.34(4) . . ? O3 Na C1 116.65(5) . 3_666 ? O2 Na C1 145.25(4) . 3_666 ? O1 Na C1 105.39(4) . 3_666 ? C1 Na C1 31.34(4) . 3_666 ? O3 Na C11 135.14(4) . 3_666 ? O2 Na C11 95.13(4) . 3_666 ? O1 Na C11 131.98(4) . 3_666 ? C1 Na C11 30.87(3) . 3_666 ? C1 Na C11 50.80(3) 3_666 3_666 ? O3 Na C10 106.41(4) . 3_666 ? O2 Na C10 105.76(4) . 3_666 ? O1 Na C10 153.38(4) . 3_666 ? C1 Na C10 49.48(3) . 3_666 ? C1 Na C10 49.19(3) 3_666 3_666 ? C11 Na C10 29.51(3) 3_666 3_666 ? O3 Na C2 96.66(4) . 3_666 ? O2 Na C2 134.37(5) . 3_666 ? O1 Na C2 131.54(4) . 3_666 ? C1 Na C2 50.49(3) . 3_666 ? C1 Na C2 30.34(3) 3_666 3_666 ? C11 Na C2 49.60(3) 3_666 3_666 ? C10 Na C2 29.16(3) 3_666 3_666 ? C1 C1 C11 108.10(12) 3_666 3_666 ? C1 C1 C2 108.24(12) 3_666 . ? C11 C1 C2 143.66(10) 3_666 . ? C1 C1 Na 75.47(9) 3_666 . ? C11 C1 Na 78.75(7) 3_666 . ? C2 C1 Na 110.04(8) . . ? C1 C1 Na 73.20(9) 3_666 3_666 ? C11 C1 Na 111.10(8) 3_666 3_666 ? C2 C1 Na 80.17(7) . 3_666 ? Na C1 Na 148.66(4) . 3_666 ? C10 C2 C1 105.88(10) . . ? C10 C2 C3 123.04(10) . . ? C1 C2 C3 129.46(10) . . ? C10 C2 Na 74.51(7) . 3_666 ? C1 C2 Na 69.50(6) . 3_666 ? C3 C2 Na 132.04(8) . 3_666 ? C4 C3 C9 115.73(11) . . ? C4 C3 C2 122.48(10) . . ? C9 C3 C2 121.58(11) . . ? C5 C4 C3 121.77(11) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C4 C5 C6 121.86(12) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C8 C6 C5 116.94(11) . . ? C8 C6 C7 121.43(12) . . ? C5 C6 C7 121.62(13) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C6 121.60(11) . . ? C9 C8 H8 119.2 . . ? C6 C8 H8 119.2 . . ? C8 C9 C3 122.04(12) . . ? C8 C9 H9 119.0 . . ? C3 C9 H9 119.0 . . ? C2 C10 C11 111.67(10) . . ? C2 C10 Na 76.33(7) . 3_666 ? C11 C10 Na 73.81(7) . 3_666 ? C2 C10 H10 124.2 . . ? C11 C10 H10 124.2 . . ? Na C10 H10 117.3 3_666 . ? C10 C11 C1 106.02(10) . 3_666 ? C10 C11 C12 122.41(10) . . ? C1 C11 C12 128.98(10) 3_666 . ? C10 C11 Na 76.68(7) . 3_666 ? C1 C11 Na 70.39(6) 3_666 3_666 ? C12 C11 Na 132.35(8) . 3_666 ? C13 C12 C18 116.29(10) . . ? C13 C12 C11 121.54(10) . . ? C18 C12 C11 121.84(10) . . ? C14 C13 C12 121.50(11) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C13 C14 C15 121.65(11) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C17 C15 C14 117.27(11) . . ? C17 C15 C16 121.64(12) . . ? C14 C15 C16 121.08(12) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C15 121.55(11) . . ? C18 C17 H17 119.2 . . ? C15 C17 H17 119.2 . . ? C17 C18 C12 121.67(11) . . ? C17 C18 H18 119.2 . . ? C12 C18 H18 119.2 . . ? C21 O1 C24 109.09(12) . . ? C21 O1 Na 116.23(9) . . ? C24 O1 Na 121.92(9) . . ? O1 C21 C22 106.37(13) . . ? O1 C21 H21A 110.5 . . ? C22 C21 H21A 110.5 . . ? O1 C21 H21B 110.5 . . ? C22 C21 H21B 110.5 . . ? H21A C21 H21B 108.6 . . ? C21 C22 C23 102.22(12) . . ? C21 C22 H22A 111.3 . . ? C23 C22 H22A 111.3 . . ? C21 C22 H22B 111.3 . . ? C23 C22 H22B 111.3 . . ? H22A C22 H22B 109.2 . . ? C24 C23 C22 101.87(14) . . ? C24 C23 H23A 111.4 . . ? C22 C23 H23A 111.4 . . ? C24 C23 H23B 111.4 . . ? C22 C23 H23B 111.4 . . ? H23A C23 H23B 109.3 . . ? O1 C24 C23 106.65(13) . . ? O1 C24 H24A 110.4 . . ? C23 C24 H24A 110.4 . . ? O1 C24 H24B 110.4 . . ? C23 C24 H24B 110.4 . . ? H24A C24 H24B 108.6 . . ? C25 O2 C28 109.2(8) . . ? C28A O2 C25A 107.4(5) . . ? C25 O2 Na 119.5(5) . . ? C28 O2 Na 131.2(5) . . ? C28A O2 Na 127.7(3) . . ? C25A O2 Na 124.8(4) . . ? O2 C25 C26 101.4(9) . . ? O2 C25 H25A 111.5 . . ? C26 C25 H25A 111.5 . . ? O2 C25 H25B 111.5 . . ? C26 C25 H25B 111.5 . . ? H25A C25 H25B 109.3 . . ? C27 C26 C25 99.2(10) . . ? C27 C26 H26A 111.9 . . ? C25 C26 H26A 111.9 . . ? C27 C26 H26B 111.9 . . ? C25 C26 H26B 111.9 . . ? H26A C26 H26B 109.6 . . ? C28 C27 C26 102.5(11) . . ? C28 C27 H27A 111.3 . . ? C26 C27 H27A 111.3 . . ? C28 C27 H27B 111.3 . . ? C26 C27 H27B 111.3 . . ? H27A C27 H27B 109.2 . . ? O2 C28 C27 108.3(10) . . ? O2 C28 H28A 110.0 . . ? C27 C28 H28A 110.0 . . ? O2 C28 H28B 110.0 . . ? C27 C28 H28B 110.0 . . ? H28A C28 H28B 108.4 . . ? C26A C25A O2 107.3(8) . . ? C26A C25A H25C 110.3 . . ? O2 C25A H25C 110.3 . . ? C26A C25A H25D 110.3 . . ? O2 C25A H25D 110.3 . . ? H25C C25A H25D 108.5 . . ? C25A C26A C27A 105.9(9) . . ? C25A C26A H26C 110.5 . . ? C27A C26A H26C 110.5 . . ? C25A C26A H26D 110.5 . . ? C27A C26A H26D 110.5 . . ? H26C C26A H26D 108.7 . . ? C26A C27A C28A 102.4(8) . . ? C26A C27A H27C 111.3 . . ? C28A C27A H27C 111.3 . . ? C26A C27A H27D 111.3 . . ? C28A C27A H27D 111.3 . . ? H27C C27A H27D 109.2 . . ? O2 C28A C27A 104.5(5) . . ? O2 C28A H28C 110.9 . . ? C27A C28A H28C 110.9 . . ? O2 C28A H28D 110.9 . . ? C27A C28A H28D 110.9 . . ? H28C C28A H28D 108.9 . . ? C29 O3 C32 105.00(13) . . ? C29 O3 Na 121.81(10) . . ? C32 O3 Na 128.42(11) . . ? O3 C29 C30 106.86(15) . . ? O3 C29 H29A 110.4 . . ? C30 C29 H29A 110.4 . . ? O3 C29 H29B 110.4 . . ? C30 C29 H29B 110.4 . . ? H29A C29 H29B 108.6 . . ? C29 C30 C31 105.96(15) . . ? C29 C30 H30A 110.5 . . ? C31 C30 H30A 110.5 . . ? C29 C30 H30B 110.5 . . ? C31 C30 H30B 110.5 . . ? H30A C30 H30B 108.7 . . ? C32 C31 C30 103.32(16) . . ? C32 C31 H31A 111.1 . . ? C30 C31 H31A 111.1 . . ? C32 C31 H31B 111.1 . . ? C30 C31 H31B 111.1 . . ? H31A C31 H31B 109.1 . . ? O3 C32 C31 105.90(15) . . ? O3 C32 H32A 110.6 . . ? C31 C32 H32A 110.6 . . ? O3 C32 H32B 110.6 . . ? C31 C32 H32B 110.6 . . ? H32A C32 H32B 108.7 . . ? 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 Na O3 2.3172(12) . ? Na O2 2.3299(13) . ? Na O1 2.3665(12) . ? Na C1 2.6537(12) . ? Na C1 2.6834(13) 3_666 ? Na C11 2.7630(13) 3_666 ? Na C10 2.7997(13) 3_666 ? Na C2 2.8228(13) 3_666 ? C1 C1 1.442(2) 3_666 ? C1 C11 1.4453(16) 3_666 ? C1 C2 1.4471(16) . ? C2 C10 1.4153(16) . ? C2 C3 1.4618(16) . ? C3 C4 1.4052(17) . ? C3 C9 1.4075(16) . ? C4 C5 1.3875(17) . ? C4 H4 0.9500 . ? C5 C6 1.3916(18) . ? C5 H5 0.9500 . ? C6 C8 1.3907(19) . ? C6 C7 1.5107(18) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.3866(18) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.4171(16) . ? C10 H10 0.9500 . ? C11 C12 1.4589(16) . ? C12 C13 1.4046(16) . ? C12 C18 1.4079(16) . ? C13 C14 1.3863(16) . ? C13 H13 0.9500 . ? C14 C15 1.3925(18) . ? C14 H14 0.9500 . ? C15 C17 1.3913(19) . ? C15 C16 1.5074(17) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.3836(17) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? O1 C21 1.4372(18) . ? O1 C24 1.438(2) . ? C21 C22 1.509(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.522(2) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.508(2) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? O2 C25 1.395(13) . ? O2 C28 1.405(13) . ? O2 C28A 1.412(8) . ? O2 C25A 1.469(11) . ? C25 C26 1.580(18) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.471(19) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.461(18) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C25A C26A 1.466(17) . ? C25A H25C 0.9900 . ? C25A H25D 0.9900 . ? C26A C27A 1.487(15) . ? C26A H26C 0.9900 . ? C26A H26D 0.9900 . ? C27A C28A 1.527(11) . ? C27A H27C 0.9900 . ? C27A H27D 0.9900 . ? C28A H28C 0.9900 . ? C28A H28D 0.9900 . ? O3 C29 1.421(2) . ? O3 C32 1.437(2) . ? C29 C30 1.487(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.502(3) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.485(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? 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 C1 C1 C2 C10 2.28(15) 3_666 . . . ? C11 C1 C2 C10 -178.63(15) 3_666 . . . ? Na C1 C2 C10 83.01(10) . . . . ? Na C1 C2 C10 -66.25(8) 3_666 . . . ? C1 C1 C2 C3 -163.29(12) 3_666 . . . ? C11 C1 C2 C3 15.8(3) 3_666 . . . ? Na C1 C2 C3 -82.56(13) . . . . ? Na C1 C2 C3 128.18(12) 3_666 . . . ? C1 C1 C2 Na 68.53(11) 3_666 . . 3_666 ? C11 C1 C2 Na -112.38(18) 3_666 . . 3_666 ? Na C1 C2 Na 149.26(6) . . . 3_666 ? C10 C2 C3 C4 -148.62(12) . . . . ? C1 C2 C3 C4 14.76(19) . . . . ? Na C2 C3 C4 112.30(12) 3_666 . . . ? C10 C2 C3 C9 25.83(18) . . . . ? C1 C2 C3 C9 -170.79(12) . . . . ? Na C2 C3 C9 -73.24(14) 3_666 . . . ? C9 C3 C4 C5 -2.06(18) . . . . ? C2 C3 C4 C5 172.69(11) . . . . ? C3 C4 C5 C6 0.1(2) . . . . ? C4 C5 C6 C8 1.7(2) . . . . ? C4 C5 C6 C7 -177.71(13) . . . . ? C5 C6 C8 C9 -1.5(2) . . . . ? C7 C6 C8 C9 177.99(14) . . . . ? C6 C8 C9 C3 -0.6(2) . . . . ? C4 C3 C9 C8 2.34(18) . . . . ? C2 C3 C9 C8 -172.46(12) . . . . ? C1 C2 C10 C11 -3.26(14) . . . . ? C3 C2 C10 C11 163.47(11) . . . . ? Na C2 C10 C11 -66.09(9) 3_666 . . . ? C1 C2 C10 Na 62.82(8) . . . 3_666 ? C3 C2 C10 Na -130.45(11) . . . 3_666 ? C2 C10 C11 C1 2.92(14) . . . 3_666 ? Na C10 C11 C1 -64.73(8) 3_666 . . 3_666 ? C2 C10 C11 C12 -160.30(11) . . . . ? Na C10 C11 C12 132.04(11) 3_666 . . . ? C2 C10 C11 Na 67.66(9) . . . 3_666 ? C10 C11 C12 C13 142.49(12) . . . . ? C1 C11 C12 C13 -16.60(19) 3_666 . . . ? Na C11 C12 C13 -115.42(11) 3_666 . . . ? C10 C11 C12 C18 -30.63(18) . . . . ? C1 C11 C12 C18 170.27(12) 3_666 . . . ? Na C11 C12 C18 71.45(15) 3_666 . . . ? C18 C12 C13 C14 2.25(17) . . . . ? C11 C12 C13 C14 -171.24(11) . . . . ? C12 C13 C14 C15 0.0(2) . . . . ? C13 C14 C15 C17 -1.71(19) . . . . ? C13 C14 C15 C16 177.33(13) . . . . ? C14 C15 C17 C18 1.07(19) . . . . ? C16 C15 C17 C18 -177.97(13) . . . . ? C15 C17 C18 C12 1.29(19) . . . . ? C13 C12 C18 C17 -2.89(18) . . . . ? C11 C12 C18 C17 170.58(11) . . . . ? C24 O1 C21 C22 11.98(17) . . . . ? Na O1 C21 C22 -130.59(11) . . . . ? O1 C21 C22 C23 -30.55(17) . . . . ? C21 C22 C23 C24 36.50(16) . . . . ? C21 O1 C24 C23 11.98(17) . . . . ? Na O1 C24 C23 152.02(10) . . . . ? C22 C23 C24 O1 -30.49(16) . . . . ? C28 O2 C25 C26 27.8(9) . . . . ? Na O2 C25 C26 -155.0(5) . . . . ? O2 C25 C26 C27 -42.0(11) . . . . ? C25 C26 C27 C28 39.8(16) . . . . ? C25 O2 C28 C27 -3.0(15) . . . . ? Na O2 C28 C27 -179.7(9) . . . . ? C26 C27 C28 O2 -25.4(19) . . . . ? C28A O2 C25A C26A 13.1(9) . . . . ? Na O2 C25A C26A -169.8(6) . . . . ? O2 C25A C26A C27A 10.1(12) . . . . ? C25A C26A C27A C28A -27.3(11) . . . . ? C25A O2 C28A C27A -30.2(6) . . . . ? Na O2 C28A C27A 152.8(4) . . . . ? C26A C27A C28A O2 35.6(8) . . . . ? C32 O3 C29 C30 -30.4(2) . . . . ? Na O3 C29 C30 127.03(14) . . . . ? O3 C29 C30 C31 12.1(2) . . . . ? C29 C30 C31 C32 10.2(2) . . . . ? C29 O3 C32 C31 37.3(2) . . . . ? Na O3 C32 C31 -118.05(13) . . . . ? C30 C31 C32 O3 -28.8(2) . . . . ?