#------------------------------------------------------------------------------ #$Date: 2017-02-15 06:48:02 +0200 (Wed, 15 Feb 2017) $ #$Revision: 192109 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/20/7042060.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_7042060 loop_ _publ_author_name 'Kyri, A. W.' 'Brehm, P.' 'Schnakenburg, G.' 'Streubel, R.' _publ_section_title ; Ring opening of a sterically crowded 1,2-oxaphosphetane complex ; _journal_name_full 'Dalton Trans.' _journal_paper_doi 10.1039/C7DT00136C _journal_year 2017 _chemical_formula_moiety '2(C36 H34 F6 Li O11 P W), C4 H10 O' _chemical_formula_sum 'C76 H78 F12 Li2 O23 P2 W2' _chemical_formula_weight 2030.90 _chemical_name_systematic AKY-488-2 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_date 2017-01-10 _audit_creation_method ; Olex2 1.2 (compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289) ; _audit_update_record ; 2017-01-10 deposited with the CCDC. 2017-02-03 downloaded from the CCDC. ; _cell_angle_alpha 86.722(3) _cell_angle_beta 74.872(2) _cell_angle_gamma 73.209(3) _cell_formula_units_Z 2 _cell_length_a 11.7408(5) _cell_length_b 18.5934(8) _cell_length_c 20.0735(8) _cell_measurement_reflns_used 9524 _cell_measurement_temperature 100 _cell_measurement_theta_max 29.31 _cell_measurement_theta_min 2.29 _cell_volume 4049.1(3) _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XS (Sheldrick, 2008)' _diffrn_ambient_temperature 100.0 _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0818 _diffrn_reflns_av_unetI/netI 0.0858 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 105146 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 28.000 _diffrn_reflns_theta_min 2.468 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.979 _exptl_absorpt_correction_T_max 0.5865 _exptl_absorpt_correction_T_min 0.4057 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1147 before and 0.0646 after correction. The Ratio of minimum to maximum transmission is 0.6917. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.666 _exptl_crystal_description plate _exptl_crystal_F_000 2020 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _refine_diff_density_max 4.023 _refine_diff_density_min -1.908 _refine_diff_density_rms 0.185 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1058 _refine_ls_number_reflns 19509 _refine_ls_number_restraints 27 _refine_ls_restrained_S_all 1.012 _refine_ls_R_factor_all 0.0959 _refine_ls_R_factor_gt 0.0470 _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^)+(0.0674P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1073 _refine_ls_wR_factor_ref 0.1261 _reflns_Friedel_coverage 0.000 _reflns_number_gt 12783 _reflns_number_total 19509 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; 4012f.res created by SHELXL-2014/7 TITL 4012f in P-1 #2 REM reset to P-1 #2 CELL 0.71073 11.7408 18.5934 20.0735 86.7216 74.8723 73.209 ZERR 2 0.0005 0.0008 0.0008 0.0026 0.0024 0.0026 LATT 1 SFAC C H F Li O P W UNIT 152 156 24 4 46 4 4 DFIX 1.49 0.01 O12 C39 DELU 0.005 0.005 F5 C4 DELU 0.005 0.005 F1' C3' ISOR 0.01 0.02 C40 C39 ISOR 0.005 0.01 C18 C3' L.S. 10 0 0 PLAN 10 SIZE 0.04 0.08 0.1 TEMP -173.15 BOND MORE -1 BOND $H CONF fmap 2 53 acta 52 OMIT -2 56 OMIT 0 2 0 OMIT 0 0 1 OMIT 1 1 1 OMIT 0 1 0 OMIT 0 1 1 OMIT 1 0 1 OMIT 0 -1 1 OMIT 0 1 2 OMIT 1 1 0 OMIT 0 -2 1 OMIT -1 1 1 OMIT 0 2 2 REM REM REM WGHT 0.067400 FVAR 0.06497 W 7 0.460390 0.274153 0.285889 11.00000 0.01992 0.01948 = 0.01767 0.00176 -0.00548 -0.00577 W' 7 -0.112505 0.369122 -0.289798 11.00000 0.02052 0.01873 = 0.01675 0.00101 -0.00453 -0.00657 P' 6 -0.140388 0.292271 -0.179667 11.00000 0.01719 0.01809 = 0.01447 -0.00139 -0.00234 -0.00270 P 6 0.603112 0.232987 0.367627 11.00000 0.01659 0.01301 = 0.01442 -0.00102 -0.00278 -0.00447 O10' 5 0.016248 0.248841 -0.412658 11.00000 0.02899 0.03017 = 0.01891 -0.00677 -0.00292 -0.00748 F5 3 0.428783 0.306438 0.628184 11.00000 0.03400 0.03073 = 0.01601 -0.00972 0.00060 -0.00772 F2 3 0.286017 0.224475 0.562564 11.00000 0.02364 0.02998 = 0.03705 0.00903 -0.00283 -0.01022 F4 3 0.503266 0.188973 0.599855 11.00000 0.03330 0.02429 = 0.02216 0.00598 -0.00744 -0.00945 F2' 3 -0.124949 0.398053 0.052832 11.00000 0.06182 0.04310 = 0.01871 -0.00929 -0.01117 -0.00842 O11 5 0.571482 0.149350 0.165890 11.00000 0.03418 0.03621 = 0.02474 -0.00655 -0.00360 -0.00958 C35' 1 -0.029006 0.288539 -0.365518 11.00000 0.01532 0.02436 = 0.01772 0.00497 -0.00587 -0.00761 F1 3 0.271103 0.290431 0.472148 11.00000 0.02478 0.04061 = 0.02582 -0.00059 -0.00527 -0.00345 O1 5 0.465696 0.345347 0.488266 11.00000 0.03003 0.01246 = 0.02043 -0.00256 0.00528 -0.00651 AFIX 147 H1 2 0.528657 0.340321 0.455264 11.00000 -1.50000 AFIX 0 C1 1 0.522454 0.208298 0.456673 11.00000 0.01769 0.01347 = 0.01544 -0.00103 -0.00471 -0.00335 AFIX 23 H1A 2 0.462609 0.182181 0.451591 11.00000 -1.20000 H1B 2 0.584472 0.172154 0.476587 11.00000 -1.20000 AFIX 0 C36 1 0.537259 0.191660 0.210938 11.00000 0.02293 0.02225 = 0.02493 0.00642 -0.00656 -0.00513 C18 1 0.692498 0.075901 0.369451 11.00000 0.02168 0.01711 = 0.01201 -0.00684 -0.00447 0.00058 F3 3 0.247884 0.344766 0.567985 11.00000 0.02304 0.02862 = 0.03145 -0.00672 0.00197 0.00040 O1' 5 -0.231136 0.407170 -0.056802 11.00000 0.01935 0.02784 = 0.02705 -0.01003 -0.00343 -0.00435 AFIX 147 H1' 2 -0.259229 0.385876 -0.081950 11.00000 -1.50000 AFIX 0 O2' 5 -0.273985 0.316737 -0.134914 11.00000 0.01791 0.01597 = 0.01799 -0.00284 -0.00102 -0.00048 O8 5 0.294260 0.174175 0.368879 11.00000 0.03290 0.04408 = 0.03797 0.00566 -0.00399 -0.02205 F6 3 0.612376 0.265327 0.563878 11.00000 0.02402 0.04166 = 0.02336 -0.00485 -0.00490 -0.01513 O2 5 0.652644 0.297264 0.381988 11.00000 0.01913 0.01287 = 0.01764 -0.00207 -0.00115 -0.00730 O10 5 0.629934 0.367640 0.192927 11.00000 0.03695 0.03599 = 0.03396 0.01067 -0.00961 -0.02070 C1' 1 -0.047954 0.305259 -0.118701 11.00000 0.01877 0.01854 = 0.01763 -0.00230 -0.00522 -0.00089 AFIX 23 H1'A 2 -0.030748 0.258837 -0.091810 11.00000 -1.20000 H1'B 2 0.032188 0.310084 -0.147004 11.00000 -1.20000 AFIX 0 F4' 3 -0.092645 0.495062 -0.044623 11.00000 0.03380 0.03021 = 0.03283 -0.01257 -0.00658 -0.00981 C2 1 0.452936 0.274791 0.509385 11.00000 0.01730 0.01681 = 0.01671 -0.00397 -0.00113 -0.00401 O7' 5 -0.062726 0.485287 -0.406011 11.00000 0.04809 0.03851 = 0.03711 0.01424 -0.01749 -0.02488 F6' 3 -0.049744 0.460513 -0.149817 11.00000 0.07298 0.04183 = 0.02357 0.00037 -0.00626 -0.03490 C2' 1 -0.105871 0.372818 -0.067042 11.00000 0.01920 0.02193 = 0.01924 -0.00181 -0.00526 -0.00131 C32' 1 -0.085729 0.442807 -0.364063 11.00000 0.02872 0.02355 = 0.03126 0.00075 -0.01165 -0.01031 C33 1 0.353092 0.210740 0.340845 11.00000 0.02564 0.02838 = 0.01706 -0.00078 -0.00335 -0.00623 C5' 1 -0.085753 0.182851 -0.187695 11.00000 0.02105 0.02108 = 0.01269 -0.00197 0.00014 -0.00389 O9' 5 -0.367247 0.361738 -0.314697 11.00000 0.02896 0.04423 = 0.03576 0.00029 -0.00976 -0.01316 C4 1 0.497294 0.257636 0.575544 11.00000 0.01463 0.02912 = 0.02984 0.00567 0.00620 -0.00630 O11' 5 0.145932 0.369618 -0.268747 11.00000 0.02674 0.04916 = 0.03001 0.00028 -0.00656 -0.02330 C6' 1 -0.146485 0.142377 -0.124765 11.00000 0.01122 0.02460 = 0.02127 0.00613 -0.00788 -0.00291 C33' 1 -0.219517 0.456959 -0.225483 11.00000 0.03382 0.02247 = 0.02773 0.00519 -0.00548 -0.00860 C18' 1 -0.125923 0.162484 -0.249397 11.00000 0.02629 0.01366 = 0.01714 -0.00075 -0.00599 -0.00541 C20 1 0.682270 -0.029815 0.445142 11.00000 0.03295 0.02162 = 0.03559 0.01551 -0.01189 -0.01130 AFIX 43 H20 2 0.711362 -0.061778 0.479440 11.00000 -1.20000 AFIX 0 C3' 1 -0.086486 0.343617 0.000404 11.00000 0.02790 0.01219 = 0.03054 -0.00320 -0.01105 0.00588 O9 5 0.332791 0.424475 0.375334 11.00000 0.05688 0.03323 = 0.03532 -0.00899 -0.02105 0.00318 O7 5 0.259593 0.341133 0.204329 11.00000 0.02831 0.04804 = 0.03743 0.01493 -0.01813 -0.01028 C34 1 0.378550 0.367768 0.347138 11.00000 0.02352 0.01647 = 0.02866 0.00467 -0.01275 -0.00142 C7 1 0.820977 0.205568 0.235283 11.00000 0.03154 0.01892 = 0.02049 0.00101 -0.00391 -0.00580 AFIX 43 H7 2 0.807974 0.248108 0.263342 11.00000 -1.20000 AFIX 0 C14 1 0.927736 0.168566 0.470137 11.00000 0.02936 0.02837 = 0.02182 0.00859 -0.01306 -0.01288 AFIX 43 H14 2 0.913026 0.192386 0.513425 11.00000 -1.20000 AFIX 0 C32 1 0.335056 0.316693 0.233629 11.00000 0.03068 0.02348 = 0.02132 0.00665 0.00020 -0.01098 C36' 1 0.052724 0.369684 -0.275429 11.00000 0.03042 0.02250 = 0.01513 -0.00403 -0.00213 -0.01159 C3 1 0.313080 0.284215 0.528264 11.00000 0.02534 0.02732 = 0.01480 -0.00239 -0.00052 -0.00267 F1' 3 -0.154506 0.295899 0.026706 11.00000 0.12257 0.03997 = 0.02443 0.00872 -0.01809 -0.03541 C6 1 0.790752 0.142483 0.265857 11.00000 0.01948 0.01286 = 0.01667 -0.00354 -0.00200 0.00222 F3' 3 0.029176 0.307547 0.002657 11.00000 0.08539 0.05921 = 0.05169 -0.01890 -0.05006 0.02890 C11 1 0.816875 0.079862 0.223696 11.00000 0.02567 0.01694 = 0.02909 -0.00210 -0.00662 -0.00202 AFIX 43 H11 2 0.800016 0.035231 0.243547 11.00000 -1.20000 AFIX 0 F5' 3 0.077370 0.412585 -0.089608 11.00000 0.02161 0.05700 = 0.08127 -0.02944 -0.00797 -0.01111 C23 1 0.601085 0.061697 0.345517 11.00000 0.03127 0.01427 = 0.02551 0.00238 -0.00965 -0.00663 AFIX 43 H23 2 0.572846 0.092147 0.310164 11.00000 -1.20000 AFIX 0 C11' 1 -0.135619 0.066772 -0.133653 11.00000 0.02988 0.02865 = 0.02255 0.00579 -0.00692 -0.01108 AFIX 43 H11' 2 -0.097784 0.044001 -0.178169 11.00000 -1.20000 AFIX 0 C12 1 0.848256 0.143184 0.376141 11.00000 0.02239 0.01414 = 0.01990 0.00481 -0.00561 -0.00604 C5 1 0.742348 0.143009 0.344439 11.00000 0.02295 0.01265 = 0.01548 -0.00099 -0.00364 -0.00465 C17 1 0.968072 0.100412 0.344975 11.00000 0.02726 0.02113 = 0.02818 -0.00102 -0.00844 -0.00875 AFIX 43 H17 2 0.984043 0.075928 0.301859 11.00000 -1.20000 AFIX 0 C16' 1 0.257711 0.161925 -0.262632 11.00000 0.02231 0.02784 = 0.03146 -0.00126 0.00138 -0.00479 AFIX 43 H16' 2 0.308705 0.176278 -0.303071 11.00000 -1.20000 AFIX 0 C23' 1 -0.250339 0.186445 -0.247857 11.00000 0.02683 0.02288 = 0.02049 -0.00244 -0.00555 -0.00278 AFIX 43 H23' 2 -0.306692 0.216858 -0.210123 11.00000 -1.20000 AFIX 0 C20' 1 -0.090013 0.097110 -0.357095 11.00000 0.03877 0.02165 = 0.02052 -0.00623 -0.00604 -0.00361 AFIX 43 H20' 2 -0.034384 0.066373 -0.394826 11.00000 -1.20000 AFIX 0 C7' 1 -0.202677 0.173396 -0.059540 11.00000 0.01940 0.02812 = 0.02489 0.00623 -0.00461 -0.00274 AFIX 43 H7' 2 -0.212620 0.225032 -0.051780 11.00000 -1.20000 AFIX 0 C34' 1 -0.275873 0.363717 -0.304856 11.00000 0.02879 0.01985 = 0.02145 0.00023 -0.00722 -0.00423 C15 1 1.044037 0.125838 0.437923 11.00000 0.02272 0.03058 = 0.04450 0.01550 -0.01654 -0.01047 AFIX 43 H15 2 1.109847 0.119357 0.459039 11.00000 -1.20000 AFIX 0 C10 1 0.867125 0.081577 0.153167 11.00000 0.03496 0.02281 = 0.02457 -0.00473 -0.00442 0.00200 AFIX 43 H10 2 0.883238 0.038524 0.125099 11.00000 -1.20000 AFIX 0 C9' 1 -0.231219 0.056144 -0.014696 11.00000 0.03522 0.04188 = 0.03670 0.02625 -0.00415 -0.01476 AFIX 43 H9' 2 -0.257989 0.026651 0.023093 11.00000 -1.20000 AFIX 0 C8' 1 -0.245090 0.130502 -0.004874 11.00000 0.02550 0.04867 = 0.02061 0.01137 -0.00332 -0.00461 AFIX 43 H8' 2 -0.283999 0.153120 0.039627 11.00000 -1.20000 AFIX 0 C35 1 0.571080 0.333795 0.227713 11.00000 0.02143 0.02637 = 0.02392 -0.00103 -0.00861 -0.00263 C17' 1 0.132750 0.180193 -0.254925 11.00000 0.02276 0.02851 = 0.01812 0.00205 -0.00059 0.00035 AFIX 43 H17' 2 0.098829 0.207276 -0.290148 11.00000 -1.20000 AFIX 0 C22 1 0.549372 0.004938 0.371079 11.00000 0.02841 0.02278 = 0.03419 -0.00375 -0.00790 -0.00896 AFIX 43 H22 2 0.484986 -0.002085 0.354044 11.00000 -1.20000 AFIX 0 C13 1 0.831656 0.176953 0.439443 11.00000 0.02328 0.02303 = 0.02192 0.00501 -0.00668 -0.00800 AFIX 43 H13 2 0.751798 0.206771 0.462430 11.00000 -1.20000 AFIX 0 C14' 1 0.233605 0.103431 -0.153327 11.00000 0.02501 0.02814 = 0.03106 0.00587 -0.01232 -0.00589 AFIX 43 H14' 2 0.268181 0.077303 -0.117940 11.00000 -1.20000 AFIX 0 C21 1 0.589613 -0.041796 0.420975 11.00000 0.03780 0.02179 = 0.03633 0.00368 -0.00363 -0.01499 AFIX 43 H21 2 0.554412 -0.081300 0.438310 11.00000 -1.20000 AFIX 0 C19 1 0.733921 0.027690 0.420613 11.00000 0.02647 0.01979 = 0.02651 0.00404 -0.00709 -0.00629 AFIX 43 H19 2 0.797592 0.034838 0.438239 11.00000 -1.20000 AFIX 0 C16 1 1.064288 0.092775 0.375352 11.00000 0.02279 0.02944 = 0.04350 0.00064 -0.00800 -0.00685 AFIX 43 H16 2 1.145042 0.064243 0.352348 11.00000 -1.20000 AFIX 0 C8 1 0.869529 0.207936 0.165001 11.00000 0.04057 0.02347 = 0.02273 0.00416 0.00114 -0.00299 AFIX 43 H8 2 0.886391 0.252471 0.144900 11.00000 -1.20000 AFIX 0 C15' 1 0.309856 0.122959 -0.212245 11.00000 0.02035 0.02530 = 0.03753 0.00058 -0.00299 -0.00176 AFIX 43 H15' 2 0.396298 0.109805 -0.217872 11.00000 -1.20000 AFIX 0 C22' 1 -0.294056 0.167094 -0.299896 11.00000 0.03184 0.02921 = 0.03417 -0.00415 -0.01684 -0.00480 AFIX 43 H22' 2 -0.379386 0.184833 -0.297748 11.00000 -1.20000 AFIX 0 C9 1 0.893653 0.145200 0.123780 11.00000 0.03787 0.03568 = 0.02014 -0.00297 -0.00459 0.00035 AFIX 43 H9 2 0.928339 0.146276 0.075485 11.00000 -1.20000 AFIX 0 C19' 1 -0.046013 0.116303 -0.305064 11.00000 0.03103 0.02090 = 0.02222 -0.00122 -0.00427 -0.00392 AFIX 43 H19' 2 0.039230 0.097979 -0.307115 11.00000 -1.20000 AFIX 0 C21' 1 -0.214703 0.122271 -0.354828 11.00000 0.04905 0.02168 = 0.02436 -0.00146 -0.01825 -0.00993 AFIX 43 H21' 2 -0.244605 0.108782 -0.390529 11.00000 -1.20000 AFIX 0 C10' 1 -0.178024 0.023990 -0.079906 11.00000 0.03125 0.03392 = 0.04167 0.01139 -0.01235 -0.01339 AFIX 43 H10' 2 -0.170759 -0.027269 -0.087606 11.00000 -1.20000 AFIX 0 C4' 1 -0.042851 0.435739 -0.087521 11.00000 0.02566 0.03253 = 0.02888 -0.01341 -0.00583 -0.00500 O5 5 0.930704 0.343332 0.310517 11.00000 0.02423 0.02427 = 0.02770 0.00806 -0.00434 -0.00739 O4 5 0.842674 0.349604 0.449108 11.00000 0.03179 0.02726 = 0.03183 0.00177 -0.01126 -0.01733 O6 5 0.724158 0.446998 0.295530 11.00000 0.02049 0.02258 = 0.02402 -0.00185 -0.00111 -0.00633 O3 5 0.635335 0.451707 0.434782 11.00000 0.03241 0.02316 = 0.02286 -0.00467 -0.00102 -0.01142 C29 1 0.838973 0.440214 0.244990 11.00000 0.02402 0.02557 = 0.01842 0.00221 0.00178 -0.00876 AFIX 23 H29A 2 0.839888 0.489655 0.224112 11.00000 -1.20000 H29B 2 0.848506 0.404508 0.207822 11.00000 -1.20000 AFIX 0 C28 1 0.943613 0.412582 0.278817 11.00000 0.02160 0.02714 = 0.03172 0.01154 -0.00512 -0.01090 AFIX 23 H28A 2 1.023700 0.404223 0.244090 11.00000 -1.20000 H28B 2 0.938460 0.449522 0.313888 11.00000 -1.20000 AFIX 0 C31 1 0.577621 0.510593 0.393382 11.00000 0.02967 0.01425 = 0.03430 -0.00387 -0.00097 -0.00292 AFIX 23 H31A 2 0.543405 0.558504 0.420208 11.00000 -1.20000 H31B 2 0.508969 0.497615 0.381716 11.00000 -1.20000 AFIX 0 C26 1 0.967574 0.351270 0.422553 11.00000 0.03971 0.03512 = 0.04006 0.01472 -0.02169 -0.02135 AFIX 23 H26A 2 1.018134 0.325125 0.453973 11.00000 -1.20000 H26B 2 0.971730 0.403809 0.417925 11.00000 -1.20000 AFIX 0 C30 1 0.669318 0.519892 0.328501 11.00000 0.03287 0.02200 = 0.02701 0.00004 -0.00515 -0.00448 AFIX 23 H30A 2 0.628130 0.555874 0.297893 11.00000 -1.20000 H30B 2 0.732967 0.539089 0.339287 11.00000 -1.20000 AFIX 0 C24 1 0.705828 0.474121 0.473861 11.00000 0.04853 0.02789 = 0.02454 -0.00658 -0.00317 -0.01763 AFIX 23 H24A 2 0.651335 0.510400 0.511031 11.00000 -1.20000 H24B 2 0.765706 0.497793 0.443734 11.00000 -1.20000 AFIX 0 C25 1 0.771750 0.402678 0.503969 11.00000 0.05586 0.03972 = 0.02348 0.00170 -0.01466 -0.02417 AFIX 23 H25A 2 0.826509 0.413684 0.529581 11.00000 -1.20000 H25B 2 0.711058 0.381495 0.536552 11.00000 -1.20000 AFIX 0 C27 1 1.013630 0.312233 0.353394 11.00000 0.01884 0.04475 = 0.04649 0.01959 -0.00749 -0.00750 AFIX 23 H27A 2 1.096138 0.317777 0.330504 11.00000 -1.20000 H27B 2 1.021425 0.257956 0.359471 11.00000 -1.20000 AFIX 0 C12' 1 0.053755 0.159582 -0.195817 11.00000 0.01695 0.01110 = 0.02023 -0.00493 0.00049 -0.00019 O8' 5 -0.289366 0.507449 -0.192623 11.00000 0.04861 0.02500 = 0.03592 -0.00192 -0.00245 0.00205 C13' 1 0.107205 0.121488 -0.145181 11.00000 0.01964 0.01334 = 0.02361 0.00389 -0.00196 0.00317 AFIX 43 H13' 2 0.056723 0.107516 -0.104316 11.00000 -1.20000 AFIX 0 O12 5 0.294043 0.119411 0.140372 11.00000 0.09379 0.12537 = 0.09116 0.01473 -0.05132 -0.05954 C38 1 0.185252 0.170819 0.186896 11.00000 0.05096 0.06656 = 0.05511 -0.01580 0.00341 -0.01952 AFIX 23 H38A 2 0.207837 0.187783 0.226253 11.00000 -1.20000 H38B 2 0.120027 0.145645 0.205021 11.00000 -1.20000 AFIX 0 C37 1 0.141408 0.237627 0.141863 11.00000 0.06587 0.09169 = 0.07968 0.01512 -0.01051 -0.03147 AFIX 137 H37A 2 0.131357 0.218939 0.099701 11.00000 -1.50000 H37B 2 0.202498 0.265830 0.129623 11.00000 -1.50000 H37C 2 0.062460 0.270637 0.167598 11.00000 -1.50000 AFIX 0 LI' 4 -0.439408 0.324750 -0.102199 11.00000 0.02003 0.03029 = 0.02613 -0.00535 -0.00457 -0.00645 LI 4 0.750989 0.360933 0.371754 11.00000 0.02791 0.02508 = 0.02039 0.00313 -0.00619 -0.01365 C39 1 0.332836 0.058625 0.182223 11.00000 0.11308 0.10700 = 0.12491 0.00958 -0.07292 -0.03979 AFIX 23 H39A 2 0.269764 0.031836 0.200261 11.00000 -1.20000 H39B 2 0.360470 0.073445 0.220573 11.00000 -1.20000 AFIX 0 C40 1 0.451658 0.009540 0.118216 11.00000 0.09083 0.07599 = 0.18045 -0.02501 -0.06598 0.00359 AFIX 137 H40A 2 0.429146 0.018310 0.074127 11.00000 -1.50000 H40B 2 0.469643 -0.044197 0.128206 11.00000 -1.50000 H40C 2 0.524647 0.026227 0.115436 11.00000 -1.50000 AFIX 0 O3' 5 -0.562445 0.386286 -0.160372 11.00000 0.02379 0.02861 = 0.02723 -0.00689 -0.00812 -0.00737 O5' 5 -0.476946 0.283053 -0.001107 11.00000 0.02858 0.02957 = 0.02803 -0.00022 -0.00161 -0.00755 O6' 5 -0.511449 0.425711 -0.045895 11.00000 0.02183 0.02776 = 0.02160 -0.00305 -0.00270 -0.00308 O4' 5 -0.527499 0.242835 -0.115099 11.00000 0.02584 0.02472 = 0.03987 -0.00342 -0.00859 -0.00138 C24' 1 -0.622525 0.337609 -0.182022 11.00000 0.02817 0.03722 = 0.02928 -0.00683 -0.01198 -0.00533 AFIX 23 H24C 2 -0.570297 0.311120 -0.225650 11.00000 -1.20000 H24D 2 -0.701927 0.367780 -0.190344 11.00000 -1.20000 AFIX 0 C30' 1 -0.574870 0.482347 -0.084881 11.00000 0.02893 0.02188 = 0.03281 -0.00366 -0.00612 -0.00408 AFIX 23 H30C 2 -0.514732 0.502298 -0.119259 11.00000 -1.20000 H30D 2 -0.631211 0.524325 -0.053696 11.00000 -1.20000 AFIX 0 C29' 1 -0.584313 0.413835 0.021241 11.00000 0.02854 0.03367 = 0.02361 -0.00441 -0.00285 -0.00670 AFIX 23 H29C 2 -0.663562 0.407492 0.017973 11.00000 -1.20000 H29D 2 -0.601414 0.456984 0.052646 11.00000 -1.20000 AFIX 0 C25' 1 -0.644471 0.281468 -0.127000 11.00000 0.01811 0.03116 = 0.04777 -0.00808 -0.01077 -0.00643 AFIX 23 H25C 2 -0.701554 0.307257 -0.084132 11.00000 -1.20000 H25D 2 -0.680904 0.245623 -0.142404 11.00000 -1.20000 AFIX 0 C31' 1 -0.646436 0.451312 -0.120841 11.00000 0.02363 0.03519 = 0.03542 -0.00396 -0.01188 -0.00433 AFIX 23 H31C 2 -0.713710 0.436974 -0.086848 11.00000 -1.20000 H31D 2 -0.683016 0.489275 -0.151700 11.00000 -1.20000 AFIX 0 C26' 1 -0.533835 0.195702 -0.056889 11.00000 0.03779 0.02801 = 0.05807 0.00320 -0.01539 -0.01292 AFIX 23 H26C 2 -0.454017 0.156728 -0.061935 11.00000 -1.20000 H26D 2 -0.597995 0.170119 -0.054288 11.00000 -1.20000 AFIX 0 C27' 1 -0.563850 0.241210 0.008912 11.00000 0.03263 0.03121 = 0.04316 0.01510 -0.00610 -0.01329 AFIX 23 H27C 2 -0.648536 0.275463 0.018092 11.00000 -1.20000 H27D 2 -0.557597 0.207527 0.048627 11.00000 -1.20000 AFIX 0 C28' 1 -0.509176 0.343887 0.046933 11.00000 0.03600 0.03878 = 0.01909 -0.00254 -0.00252 -0.00749 AFIX 23 H28C 2 -0.433437 0.352520 0.053511 11.00000 -1.20000 H28D 2 -0.556695 0.330970 0.092121 11.00000 -1.20000 AFIX 0 HKLF 4 REM 4012f in P-1 #2 REM R1 = 0.0470 for 12783 Fo > 4sig(Fo) and 0.0959 for all 19509 data REM 1058 parameters refined using 27 restraints END WGHT 0.0674 0.0000 REM Highest difference peak 4.023, deepest hole -1.908, 1-sigma level 0.185 Q1 1 0.1916 0.0798 -0.2821 11.00000 0.05 4.02 Q2 1 0.7638 -0.0153 0.2963 11.00000 0.05 3.71 Q3 1 -0.2815 0.0150 0.0216 11.00000 0.05 3.14 Q4 1 0.0351 0.1788 -0.1391 11.00000 0.05 2.95 Q5 1 -0.3140 0.5378 -0.1338 11.00000 0.05 2.75 Q6 1 1.1405 0.1203 0.4587 11.00000 0.05 2.29 Q7 1 0.4986 0.2380 0.5423 11.00000 0.05 1.54 Q8 1 -0.0791 0.3412 -0.0240 11.00000 0.05 1.34 Q9 1 0.5045 0.0010 0.0195 11.00000 0.05 1.32 Q10 1 0.3606 0.0778 0.1097 11.00000 0.05 1.25 REM The information below was added by Olex2. REM REM R1 = 0.0470 for 12783 Fo > 4sig(Fo) and 0.0959 for all 114197 data REM n/a parameters refined using n/a restraints REM Highest difference peak 4.02, deepest hole -1.91 REM Mean Shift 0, Max Shift 0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0959 REM R1_gt = 0.0470 REM wR_ref = 0.1261 REM GOOF = 1.009 REM Shift_max = 0.001 REM Shift_mean = 0 REM Reflections_all = 114197 REM Reflections_gt = 12783 REM Parameters = n/a REM Hole = -1.91 REM Peak = 4.02 REM Flack = n/a ; _cod_data_source_file c7dt00136c1.cif _cod_data_source_block 4012f _cod_database_code 7042060 _shelx_shelxl_version_number 2014/7 _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_max 0.890 _shelx_estimated_absorpt_t_min 0.755 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2. Restrained distances O12-C39 1.49 with sigma of 0.01 3. Rigid bond restraints F5, C4 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005 F1', C3' with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005 4. Uiso/Uaniso restraints and constraints Uanis(C40) \\sim Ueq, Uanis(C39) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C18) \\sim Ueq, Uanis(C3') \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 5.a Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C1'(H1'A,H1'B), C29(H29A,H29B), C28(H28A,H28B), C31(H31A,H31B), C26(H26A,H26B), C30(H30A,H30B), C24(H24A,H24B), C25(H25A,H25B), C27(H27A,H27B), C38(H38A,H38B), C39(H39A,H39B), C24'(H24C,H24D), C30'(H30C,H30D), C29'(H29C, H29D), C25'(H25C,H25D), C31'(H31C,H31D), C26'(H26C,H26D), C27'(H27C,H27D), C28'(H28C,H28D) 5.b Aromatic/amide H refined with riding coordinates: C20(H20), C7(H7), C14(H14), C11(H11), C23(H23), C11'(H11'), C17(H17), C16'(H16'), C23'(H23'), C20'(H20'), C7'(H7'), C15(H15), C10(H10), C9'(H9'), C8'(H8'), C17'(H17'), C22(H22), C13(H13), C14'(H14'), C21(H21), C19(H19), C16(H16), C8(H8), C15'(H15'), C22'(H22'), C9(H9), C19'(H19'), C21'(H21'), C10'(H10'), C13'(H13') 5.c Idealised Me refined as rotating group: C37(H37A,H37B,H37C), C40(H40A,H40B,H40C) 5.d Idealised tetrahedral OH refined as rotating group: O1(H1), O1'(H1') ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 W W 0.46039(2) 0.27415(2) 0.28589(2) 0.01891(7) Uani 1 1 d . . W' W -0.11250(2) 0.36912(2) -0.28980(2) 0.01853(7) Uani 1 1 d . . P' P -0.14039(13) 0.29227(8) -0.17967(7) 0.0173(3) Uani 1 1 d . . P P 0.60311(12) 0.23299(7) 0.36763(7) 0.0148(3) Uani 1 1 d . . O10' O 0.0162(4) 0.2488(2) -0.41266(19) 0.0265(9) Uani 1 1 d . . F5 F 0.4288(3) 0.30644(17) 0.62818(15) 0.0282(8) Uani 1 1 d . U F2 F 0.2860(3) 0.22447(18) 0.56256(17) 0.0310(8) Uani 1 1 d . . F4 F 0.5033(3) 0.18897(17) 0.59986(15) 0.0265(7) Uani 1 1 d . . F2' F -0.1249(4) 0.3981(2) 0.05283(17) 0.0420(10) Uani 1 1 d . . O11 O 0.5715(4) 0.1493(2) 0.1659(2) 0.0323(10) Uani 1 1 d . . C35' C -0.0290(5) 0.2885(3) -0.3655(3) 0.0186(12) Uani 1 1 d . . F1 F 0.2711(3) 0.29043(19) 0.47215(16) 0.0319(8) Uani 1 1 d . . O1 O 0.4657(3) 0.34535(19) 0.48827(18) 0.0230(9) Uani 1 1 d . . H1 H 0.5287 0.3403 0.4553 0.035 Uiso 1 1 calc GR . C1 C 0.5225(5) 0.2083(3) 0.4567(2) 0.0156(11) Uani 1 1 d . . H1A H 0.4626 0.1822 0.4516 0.019 Uiso 1 1 calc R . H1B H 0.5845 0.1722 0.4766 0.019 Uiso 1 1 calc R . C36 C 0.5373(5) 0.1917(3) 0.2109(3) 0.0238(13) Uani 1 1 d . . C18 C 0.6925(5) 0.0759(3) 0.3695(3) 0.0179(12) Uani 1 1 d . U F3 F 0.2479(3) 0.34477(18) 0.56798(16) 0.0308(8) Uani 1 1 d . . O1' O -0.2311(3) 0.4072(2) -0.05680(19) 0.0253(9) Uani 1 1 d . . H1' H -0.2592 0.3859 -0.0819 0.038 Uiso 1 1 calc GR . O2' O -0.2740(3) 0.31674(19) -0.13491(17) 0.0188(8) Uani 1 1 d . . O8 O 0.2943(4) 0.1742(2) 0.3689(2) 0.0371(11) Uani 1 1 d . . F6 F 0.6124(3) 0.26533(19) 0.56388(16) 0.0284(8) Uani 1 1 d . . O2 O 0.6526(3) 0.29726(18) 0.38199(17) 0.0165(8) Uani 1 1 d . . O10 O 0.6299(4) 0.3676(2) 0.1929(2) 0.0337(10) Uani 1 1 d . . C1' C -0.0480(5) 0.3053(3) -0.1187(3) 0.0191(12) Uani 1 1 d . . H1'A H -0.0307 0.2588 -0.0918 0.023 Uiso 1 1 calc R . H1'B H 0.0322 0.3101 -0.1470 0.023 Uiso 1 1 calc R . F4' F -0.0926(3) 0.49506(18) -0.04462(16) 0.0320(8) Uani 1 1 d . . C2 C 0.4529(5) 0.2748(3) 0.5094(3) 0.0176(11) Uani 1 1 d . . O7' O -0.0627(4) 0.4853(2) -0.4060(2) 0.0378(11) Uani 1 1 d . . F6' F -0.0497(4) 0.4605(2) -0.14982(17) 0.0433(10) Uani 1 1 d . . C2' C -0.1059(5) 0.3728(3) -0.0670(3) 0.0210(12) Uani 1 1 d . . C32' C -0.0857(5) 0.4428(3) -0.3641(3) 0.0264(13) Uani 1 1 d . . C33 C 0.3531(5) 0.2107(3) 0.3408(3) 0.0244(13) Uani 1 1 d . . C5' C -0.0858(5) 0.1829(3) -0.1877(3) 0.0195(12) Uani 1 1 d . . O9' O -0.3672(4) 0.3617(2) -0.3147(2) 0.0354(10) Uani 1 1 d . . C4 C 0.4973(5) 0.2576(3) 0.5755(3) 0.0270(14) Uani 1 1 d . U O11' O 0.1459(4) 0.3696(2) -0.2687(2) 0.0327(10) Uani 1 1 d . . C6' C -0.1465(5) 0.1424(3) -0.1248(3) 0.0190(12) Uani 1 1 d . . C33' C -0.2195(6) 0.4570(3) -0.2255(3) 0.0285(14) Uani 1 1 d . . C18' C -0.1259(5) 0.1625(3) -0.2494(3) 0.0190(12) Uani 1 1 d . . C20 C 0.6823(5) -0.0298(3) 0.4451(3) 0.0293(14) Uani 1 1 d . . H20 H 0.7114 -0.0618 0.4794 0.035 Uiso 1 1 calc R . C3' C -0.0865(5) 0.3436(3) 0.0004(3) 0.0252(13) Uani 1 1 d . U O9 O 0.3328(4) 0.4245(3) 0.3753(2) 0.0431(12) Uani 1 1 d . . O7 O 0.2596(4) 0.3411(2) 0.2043(2) 0.0367(11) Uani 1 1 d . . C34 C 0.3786(5) 0.3678(3) 0.3471(3) 0.0228(13) Uani 1 1 d . . C7 C 0.8210(5) 0.2056(3) 0.2353(3) 0.0245(13) Uani 1 1 d . . H7 H 0.8080 0.2481 0.2633 0.029 Uiso 1 1 calc R . C14 C 0.9277(5) 0.1686(3) 0.4701(3) 0.0246(13) Uani 1 1 d . . H14 H 0.9130 0.1924 0.5134 0.029 Uiso 1 1 calc R . C32 C 0.3351(6) 0.3167(3) 0.2336(3) 0.0260(13) Uani 1 1 d . . C36' C 0.0527(5) 0.3697(3) -0.2754(3) 0.0223(12) Uani 1 1 d . . C3 C 0.3131(5) 0.2842(3) 0.5283(3) 0.0243(13) Uani 1 1 d . . F1' F -0.1545(5) 0.2959(2) 0.02671(18) 0.0601(13) Uani 1 1 d . U C6 C 0.7908(5) 0.1425(3) 0.2659(3) 0.0182(12) Uani 1 1 d . . F3' F 0.0292(4) 0.3075(2) 0.0027(2) 0.0690(15) Uani 1 1 d . . C11 C 0.8169(5) 0.0799(3) 0.2237(3) 0.0247(13) Uani 1 1 d . . H11 H 0.8000 0.0352 0.2435 0.030 Uiso 1 1 calc R . F5' F 0.0774(3) 0.4126(2) -0.0896(2) 0.0530(11) Uani 1 1 d . . C23 C 0.6011(5) 0.0617(3) 0.3455(3) 0.0233(13) Uani 1 1 d . . H23 H 0.5728 0.0921 0.3102 0.028 Uiso 1 1 calc R . C11' C -0.1356(5) 0.0668(3) -0.1337(3) 0.0266(13) Uani 1 1 d . . H11' H -0.0978 0.0440 -0.1782 0.032 Uiso 1 1 calc R . C12 C 0.8483(5) 0.1432(3) 0.3761(3) 0.0188(12) Uani 1 1 d . . C5 C 0.7423(5) 0.1430(3) 0.3444(3) 0.0173(11) Uani 1 1 d . . C17 C 0.9681(5) 0.1004(3) 0.3450(3) 0.0248(13) Uani 1 1 d . . H17 H 0.9840 0.0759 0.3019 0.030 Uiso 1 1 calc R . C16' C 0.2577(5) 0.1619(3) -0.2626(3) 0.0292(14) Uani 1 1 d . . H16' H 0.3087 0.1763 -0.3031 0.035 Uiso 1 1 calc R . C23' C -0.2503(5) 0.1864(3) -0.2479(3) 0.0243(13) Uani 1 1 d . . H23' H -0.3067 0.2169 -0.2101 0.029 Uiso 1 1 calc R . C20' C -0.0900(6) 0.0971(3) -0.3571(3) 0.0281(14) Uani 1 1 d . . H20' H -0.0344 0.0664 -0.3948 0.034 Uiso 1 1 calc R . C7' C -0.2027(5) 0.1734(3) -0.0595(3) 0.0254(13) Uani 1 1 d . . H7' H -0.2126 0.2250 -0.0518 0.031 Uiso 1 1 calc R . C34' C -0.2759(6) 0.3637(3) -0.3049(3) 0.0238(13) Uani 1 1 d . . C15 C 1.0440(5) 0.1258(3) 0.4379(3) 0.0310(15) Uani 1 1 d . . H15 H 1.1098 0.1194 0.4590 0.037 Uiso 1 1 calc R . C10 C 0.8671(5) 0.0816(3) 0.1532(3) 0.0301(14) Uani 1 1 d . . H10 H 0.8832 0.0385 0.1251 0.036 Uiso 1 1 calc R . C9' C -0.2312(6) 0.0561(4) -0.0147(3) 0.0391(17) Uani 1 1 d . . H9' H -0.2580 0.0267 0.0231 0.047 Uiso 1 1 calc R . C8' C -0.2451(5) 0.1305(4) -0.0049(3) 0.0338(16) Uani 1 1 d . . H8' H -0.2840 0.1531 0.0396 0.041 Uiso 1 1 calc R . C35 C 0.5711(5) 0.3338(3) 0.2277(3) 0.0242(13) Uani 1 1 d . . C17' C 0.1328(5) 0.1802(3) -0.2549(3) 0.0258(13) Uani 1 1 d . . H17' H 0.0988 0.2073 -0.2901 0.031 Uiso 1 1 calc R . C22 C 0.5494(5) 0.0049(3) 0.3711(3) 0.0279(14) Uani 1 1 d . . H22 H 0.4850 -0.0021 0.3540 0.034 Uiso 1 1 calc R . C13 C 0.8317(5) 0.1770(3) 0.4394(3) 0.0225(12) Uani 1 1 d . . H13 H 0.7518 0.2068 0.4624 0.027 Uiso 1 1 calc R . C14' C 0.2336(5) 0.1034(3) -0.1533(3) 0.0276(14) Uani 1 1 d . . H14' H 0.2682 0.0773 -0.1179 0.033 Uiso 1 1 calc R . C21 C 0.5896(6) -0.0418(3) 0.4210(3) 0.0318(15) Uani 1 1 d . . H21 H 0.5544 -0.0813 0.4383 0.038 Uiso 1 1 calc R . C19 C 0.7339(5) 0.0277(3) 0.4206(3) 0.0244(13) Uani 1 1 d . . H19 H 0.7976 0.0348 0.4382 0.029 Uiso 1 1 calc R . C16 C 1.0643(6) 0.0928(3) 0.3754(3) 0.0321(15) Uani 1 1 d . . H16 H 1.1450 0.0642 0.3523 0.039 Uiso 1 1 calc R . C8 C 0.8695(6) 0.2079(3) 0.1650(3) 0.0322(15) Uani 1 1 d . . H8 H 0.8864 0.2525 0.1449 0.039 Uiso 1 1 calc R . C15' C 0.3099(5) 0.1230(3) -0.2122(3) 0.0296(14) Uani 1 1 d . . H15' H 0.3963 0.1098 -0.2179 0.036 Uiso 1 1 calc R . C22' C -0.2941(6) 0.1671(3) -0.2999(3) 0.0307(14) Uani 1 1 d . . H22' H -0.3794 0.1848 -0.2977 0.037 Uiso 1 1 calc R . C9 C 0.8937(6) 0.1452(3) 0.1238(3) 0.0340(16) Uani 1 1 d . . H9 H 0.9283 0.1463 0.0755 0.041 Uiso 1 1 calc R . C19' C -0.0460(6) 0.1163(3) -0.3051(3) 0.0259(13) Uani 1 1 d . . H19' H 0.0392 0.0980 -0.3071 0.031 Uiso 1 1 calc R . C21' C -0.2147(6) 0.1223(3) -0.3548(3) 0.0299(14) Uani 1 1 d . . H21' H -0.2446 0.1088 -0.3905 0.036 Uiso 1 1 calc R . C10' C -0.1780(6) 0.0240(4) -0.0799(3) 0.0346(15) Uani 1 1 d . . H10' H -0.1708 -0.0273 -0.0876 0.041 Uiso 1 1 calc R . C4' C -0.0429(5) 0.4357(3) -0.0875(3) 0.0294(14) Uani 1 1 d . . O5 O 0.9307(3) 0.3433(2) 0.31052(19) 0.0260(9) Uani 1 1 d . . O4 O 0.8427(4) 0.3496(2) 0.4491(2) 0.0278(9) Uani 1 1 d . . O6 O 0.7242(3) 0.4470(2) 0.29553(18) 0.0231(9) Uani 1 1 d . . O3 O 0.6353(4) 0.4517(2) 0.43478(19) 0.0263(9) Uani 1 1 d . . C29 C 0.8390(5) 0.4402(3) 0.2450(3) 0.0238(13) Uani 1 1 d . . H29A H 0.8399 0.4897 0.2241 0.029 Uiso 1 1 calc R . H29B H 0.8485 0.4045 0.2078 0.029 Uiso 1 1 calc R . C28 C 0.9436(5) 0.4126(3) 0.2788(3) 0.0267(14) Uani 1 1 d . . H28A H 1.0237 0.4042 0.2441 0.032 Uiso 1 1 calc R . H28B H 0.9385 0.4495 0.3139 0.032 Uiso 1 1 calc R . C31 C 0.5776(5) 0.5106(3) 0.3934(3) 0.0280(14) Uani 1 1 d . . H31A H 0.5434 0.5585 0.4202 0.034 Uiso 1 1 calc R . H31B H 0.5090 0.4976 0.3817 0.034 Uiso 1 1 calc R . C26 C 0.9676(6) 0.3513(4) 0.4226(3) 0.0343(15) Uani 1 1 d . . H26A H 1.0181 0.3251 0.4540 0.041 Uiso 1 1 calc R . H26B H 0.9717 0.4038 0.4179 0.041 Uiso 1 1 calc R . C30 C 0.6693(6) 0.5199(3) 0.3285(3) 0.0285(14) Uani 1 1 d . . H30A H 0.6281 0.5559 0.2979 0.034 Uiso 1 1 calc R . H30B H 0.7330 0.5391 0.3393 0.034 Uiso 1 1 calc R . C24 C 0.7058(6) 0.4741(3) 0.4739(3) 0.0331(15) Uani 1 1 d . . H24A H 0.6513 0.5104 0.5110 0.040 Uiso 1 1 calc R . H24B H 0.7657 0.4978 0.4437 0.040 Uiso 1 1 calc R . C25 C 0.7718(6) 0.4027(3) 0.5040(3) 0.0366(16) Uani 1 1 d . . H25A H 0.8265 0.4137 0.5296 0.044 Uiso 1 1 calc R . H25B H 0.7111 0.3815 0.5366 0.044 Uiso 1 1 calc R . C27 C 1.0136(5) 0.3122(4) 0.3534(3) 0.0380(17) Uani 1 1 d . . H27A H 1.0961 0.3178 0.3305 0.046 Uiso 1 1 calc R . H27B H 1.0214 0.2580 0.3595 0.046 Uiso 1 1 calc R . C12' C 0.0538(5) 0.1596(3) -0.1958(3) 0.0177(12) Uani 1 1 d . . O8' O -0.2894(4) 0.5074(2) -0.1926(2) 0.0408(12) Uani 1 1 d . . C13' C 0.1072(5) 0.1215(3) -0.1452(3) 0.0214(12) Uani 1 1 d . . H13' H 0.0567 0.1075 -0.1043 0.026 Uiso 1 1 calc R . O12 O 0.2940(7) 0.1194(4) 0.1404(4) 0.092(2) Uani 1 1 d D . C38 C 0.1853(7) 0.1708(5) 0.1869(4) 0.060(2) Uani 1 1 d . . H38A H 0.2078 0.1878 0.2263 0.071 Uiso 1 1 calc R . H38B H 0.1200 0.1456 0.2050 0.071 Uiso 1 1 calc R . C37 C 0.1414(8) 0.2376(5) 0.1419(5) 0.079(3) Uani 1 1 d . . H37A H 0.1314 0.2189 0.0997 0.119 Uiso 1 1 calc GR . H37B H 0.2025 0.2658 0.1296 0.119 Uiso 1 1 calc GR . H37C H 0.0625 0.2706 0.1676 0.119 Uiso 1 1 calc GR . Li' Li -0.4394(8) 0.3248(5) -0.1022(5) 0.026(2) Uani 1 1 d . . Li Li 0.7510(9) 0.3609(5) 0.3718(5) 0.023(2) Uani 1 1 d . . C39 C 0.3328(11) 0.0586(6) 0.1822(6) 0.105(4) Uani 1 1 d D U H39A H 0.2698 0.0318 0.2003 0.126 Uiso 1 1 calc R . H39B H 0.3605 0.0734 0.2206 0.126 Uiso 1 1 calc R . C40 C 0.4517(10) 0.0095(6) 0.1182(7) 0.114(4) Uani 1 1 d . U H40A H 0.4291 0.0183 0.0741 0.172 Uiso 1 1 calc GR . H40B H 0.4696 -0.0442 0.1282 0.172 Uiso 1 1 calc GR . H40C H 0.5246 0.0262 0.1154 0.172 Uiso 1 1 calc GR . O3' O -0.5624(3) 0.3863(2) -0.16037(19) 0.0259(9) Uani 1 1 d . . O5' O -0.4769(4) 0.2831(2) -0.0011(2) 0.0299(10) Uani 1 1 d . . O6' O -0.5114(3) 0.4257(2) -0.04590(18) 0.0250(9) Uani 1 1 d . . O4' O -0.5275(4) 0.2428(2) -0.1151(2) 0.0312(10) Uani 1 1 d . . C24' C -0.6225(6) 0.3376(3) -0.1820(3) 0.0312(14) Uani 1 1 d . . H24C H -0.5703 0.3111 -0.2256 0.037 Uiso 1 1 calc R . H24D H -0.7019 0.3678 -0.1903 0.037 Uiso 1 1 calc R . C30' C -0.5749(5) 0.4823(3) -0.0849(3) 0.0287(14) Uani 1 1 d . . H30C H -0.5147 0.5023 -0.1193 0.034 Uiso 1 1 calc R . H30D H -0.6312 0.5243 -0.0537 0.034 Uiso 1 1 calc R . C29' C -0.5843(5) 0.4138(3) 0.0212(3) 0.0296(14) Uani 1 1 d . . H29C H -0.6636 0.4075 0.0180 0.036 Uiso 1 1 calc R . H29D H -0.6014 0.4570 0.0526 0.036 Uiso 1 1 calc R . C25' C -0.6445(5) 0.2815(3) -0.1270(3) 0.0316(15) Uani 1 1 d . . H25C H -0.7016 0.3073 -0.0841 0.038 Uiso 1 1 calc R . H25D H -0.6809 0.2456 -0.1424 0.038 Uiso 1 1 calc R . C31' C -0.6464(5) 0.4513(3) -0.1208(3) 0.0313(14) Uani 1 1 d . . H31C H -0.7137 0.4370 -0.0868 0.038 Uiso 1 1 calc R . H31D H -0.6830 0.4893 -0.1517 0.038 Uiso 1 1 calc R . C26' C -0.5338(6) 0.1957(4) -0.0569(4) 0.0400(17) Uani 1 1 d . . H26C H -0.4540 0.1567 -0.0619 0.048 Uiso 1 1 calc R . H26D H -0.5980 0.1701 -0.0543 0.048 Uiso 1 1 calc R . C27' C -0.5639(6) 0.2412(4) 0.0089(3) 0.0360(16) Uani 1 1 d . . H27C H -0.6485 0.2755 0.0181 0.043 Uiso 1 1 calc R . H27D H -0.5576 0.2075 0.0486 0.043 Uiso 1 1 calc R . C28' C -0.5092(6) 0.3439(3) 0.0469(3) 0.0327(15) Uani 1 1 d . . H28C H -0.4334 0.3525 0.0535 0.039 Uiso 1 1 calc R . H28D H -0.5567 0.3310 0.0921 0.039 Uiso 1 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W 0.01992(13) 0.01948(13) 0.01767(12) 0.00176(9) -0.00548(9) -0.00577(10) W' 0.02052(13) 0.01873(13) 0.01675(12) 0.00101(9) -0.00453(9) -0.00657(10) P' 0.0172(7) 0.0181(7) 0.0145(7) -0.0014(5) -0.0023(5) -0.0027(6) P 0.0166(7) 0.0130(7) 0.0144(6) -0.0010(5) -0.0028(5) -0.0045(6) O10' 0.029(2) 0.030(2) 0.019(2) -0.0068(18) -0.0029(17) -0.0075(19) F5 0.0340(19) 0.0307(18) 0.0160(16) -0.0097(13) 0.0006(14) -0.0077(15) F2 0.0236(18) 0.0300(19) 0.0370(19) 0.0090(16) -0.0028(15) -0.0102(15) F4 0.0333(19) 0.0243(18) 0.0222(16) 0.0060(14) -0.0074(14) -0.0095(15) F2' 0.062(3) 0.043(2) 0.0187(17) -0.0093(16) -0.0112(17) -0.0084(19) O11 0.034(3) 0.036(3) 0.025(2) -0.0066(19) -0.0036(19) -0.010(2) C35' 0.015(3) 0.024(3) 0.018(3) 0.005(2) -0.006(2) -0.008(2) F1 0.0248(18) 0.041(2) 0.0258(18) -0.0006(15) -0.0053(15) -0.0035(16) O1 0.030(2) 0.0125(19) 0.020(2) -0.0026(15) 0.0053(16) -0.0065(17) C1 0.018(3) 0.013(3) 0.015(3) -0.001(2) -0.005(2) -0.003(2) C36 0.023(3) 0.022(3) 0.025(3) 0.006(3) -0.007(2) -0.005(2) C18 0.022(3) 0.017(2) 0.012(2) -0.0068(19) -0.004(2) 0.001(2) F3 0.0230(18) 0.0286(19) 0.0314(18) -0.0067(15) 0.0020(14) 0.0004(15) O1' 0.019(2) 0.028(2) 0.027(2) -0.0100(17) -0.0034(17) -0.0044(17) O2' 0.0179(19) 0.0160(19) 0.0180(19) -0.0028(15) -0.0010(15) -0.0005(16) O8 0.033(2) 0.044(3) 0.038(3) 0.006(2) -0.004(2) -0.022(2) F6 0.0240(18) 0.042(2) 0.0234(17) -0.0049(15) -0.0049(14) -0.0151(16) O2 0.0191(19) 0.0129(18) 0.0176(18) -0.0021(14) -0.0012(15) -0.0073(15) O10 0.037(3) 0.036(2) 0.034(2) 0.011(2) -0.010(2) -0.021(2) C1' 0.019(3) 0.019(3) 0.018(3) -0.002(2) -0.005(2) -0.001(2) F4' 0.034(2) 0.0302(19) 0.0328(19) -0.0126(15) -0.0066(15) -0.0098(16) C2 0.017(3) 0.017(3) 0.017(3) -0.004(2) -0.001(2) -0.004(2) O7' 0.048(3) 0.039(3) 0.037(2) 0.014(2) -0.017(2) -0.025(2) F6' 0.073(3) 0.042(2) 0.0236(19) 0.0004(16) -0.0063(18) -0.035(2) C2' 0.019(3) 0.022(3) 0.019(3) -0.002(2) -0.005(2) -0.001(2) C32' 0.029(3) 0.024(3) 0.031(3) 0.001(3) -0.012(3) -0.010(3) C33 0.026(3) 0.028(3) 0.017(3) -0.001(2) -0.003(2) -0.006(3) C5' 0.021(3) 0.021(3) 0.013(3) -0.002(2) 0.000(2) -0.004(2) O9' 0.029(2) 0.044(3) 0.036(2) 0.000(2) -0.010(2) -0.013(2) C4 0.015(3) 0.029(3) 0.030(3) 0.006(2) 0.006(2) -0.006(2) O11' 0.027(2) 0.049(3) 0.030(2) 0.000(2) -0.0066(19) -0.023(2) C6' 0.011(3) 0.025(3) 0.021(3) 0.006(2) -0.008(2) -0.003(2) C33' 0.034(4) 0.022(3) 0.028(3) 0.005(3) -0.005(3) -0.009(3) C18' 0.026(3) 0.014(3) 0.017(3) -0.001(2) -0.006(2) -0.005(2) C20 0.033(4) 0.022(3) 0.036(3) 0.016(3) -0.012(3) -0.011(3) C3' 0.028(3) 0.012(2) 0.031(3) -0.003(2) -0.011(2) 0.006(2) O9 0.057(3) 0.033(3) 0.035(3) -0.009(2) -0.021(2) 0.003(2) O7 0.028(2) 0.048(3) 0.037(3) 0.015(2) -0.018(2) -0.010(2) C34 0.024(3) 0.016(3) 0.029(3) 0.005(2) -0.013(2) -0.001(2) C7 0.032(3) 0.019(3) 0.020(3) 0.001(2) -0.004(2) -0.006(3) C14 0.029(3) 0.028(3) 0.022(3) 0.009(2) -0.013(3) -0.013(3) C32 0.031(3) 0.023(3) 0.021(3) 0.007(2) 0.000(3) -0.011(3) C36' 0.030(3) 0.022(3) 0.015(3) -0.004(2) -0.002(2) -0.012(3) C3 0.025(3) 0.027(3) 0.015(3) -0.002(2) -0.001(2) -0.003(3) F1' 0.123(4) 0.040(2) 0.024(2) 0.0087(17) -0.018(2) -0.035(2) C6 0.019(3) 0.013(3) 0.017(3) -0.004(2) -0.002(2) 0.002(2) F3' 0.085(3) 0.059(3) 0.052(3) -0.019(2) -0.050(3) 0.029(3) C11 0.026(3) 0.017(3) 0.029(3) -0.002(2) -0.007(3) -0.002(2) F5' 0.022(2) 0.057(3) 0.081(3) -0.029(2) -0.0080(19) -0.0111(19) C23 0.031(3) 0.014(3) 0.026(3) 0.002(2) -0.010(3) -0.007(2) C11' 0.030(3) 0.029(3) 0.023(3) 0.006(3) -0.007(3) -0.011(3) C12 0.022(3) 0.014(3) 0.020(3) 0.005(2) -0.006(2) -0.006(2) C5 0.023(3) 0.013(3) 0.015(3) -0.001(2) -0.004(2) -0.005(2) C17 0.027(3) 0.021(3) 0.028(3) -0.001(2) -0.008(3) -0.009(3) C16' 0.022(3) 0.028(3) 0.031(3) -0.001(3) 0.001(3) -0.005(3) C23' 0.027(3) 0.023(3) 0.020(3) -0.002(2) -0.006(2) -0.003(3) C20' 0.039(4) 0.022(3) 0.021(3) -0.006(2) -0.006(3) -0.004(3) C7' 0.019(3) 0.028(3) 0.025(3) 0.006(3) -0.005(2) -0.003(3) C34' 0.029(3) 0.020(3) 0.021(3) 0.000(2) -0.007(3) -0.004(3) C15 0.023(3) 0.031(3) 0.044(4) 0.016(3) -0.017(3) -0.010(3) C10 0.035(4) 0.023(3) 0.025(3) -0.005(3) -0.004(3) 0.002(3) C9' 0.035(4) 0.042(4) 0.037(4) 0.026(3) -0.004(3) -0.015(3) C8' 0.025(3) 0.049(4) 0.021(3) 0.011(3) -0.003(3) -0.005(3) C35 0.021(3) 0.026(3) 0.024(3) -0.001(3) -0.009(2) -0.003(3) C17' 0.023(3) 0.029(3) 0.018(3) 0.002(2) -0.001(2) 0.000(3) C22 0.028(3) 0.023(3) 0.034(3) -0.004(3) -0.008(3) -0.009(3) C13 0.023(3) 0.023(3) 0.022(3) 0.005(2) -0.007(2) -0.008(2) C14' 0.025(3) 0.028(3) 0.031(3) 0.006(3) -0.012(3) -0.006(3) C21 0.038(4) 0.022(3) 0.036(4) 0.004(3) -0.004(3) -0.015(3) C19 0.026(3) 0.020(3) 0.027(3) 0.004(2) -0.007(3) -0.006(3) C16 0.023(3) 0.029(3) 0.043(4) 0.001(3) -0.008(3) -0.007(3) C8 0.041(4) 0.023(3) 0.023(3) 0.004(3) 0.001(3) -0.003(3) C15' 0.020(3) 0.025(3) 0.038(4) 0.001(3) -0.003(3) -0.002(3) C22' 0.032(4) 0.029(3) 0.034(3) -0.004(3) -0.017(3) -0.005(3) C9 0.038(4) 0.036(4) 0.020(3) -0.003(3) -0.005(3) 0.000(3) C19' 0.031(3) 0.021(3) 0.022(3) -0.001(2) -0.004(3) -0.004(3) C21' 0.049(4) 0.022(3) 0.024(3) -0.001(2) -0.018(3) -0.010(3) C10' 0.031(4) 0.034(4) 0.042(4) 0.011(3) -0.012(3) -0.013(3) C4' 0.026(3) 0.033(3) 0.029(3) -0.013(3) -0.006(3) -0.005(3) O5 0.024(2) 0.024(2) 0.028(2) 0.0081(17) -0.0043(17) -0.0074(17) O4 0.032(2) 0.027(2) 0.032(2) 0.0018(18) -0.0113(19) -0.0173(19) O6 0.020(2) 0.023(2) 0.024(2) -0.0018(16) -0.0011(16) -0.0063(17) O3 0.032(2) 0.023(2) 0.023(2) -0.0047(17) -0.0010(17) -0.0114(18) C29 0.024(3) 0.026(3) 0.018(3) 0.002(2) 0.002(2) -0.009(3) C28 0.022(3) 0.027(3) 0.032(3) 0.012(3) -0.005(3) -0.011(3) C31 0.030(3) 0.014(3) 0.034(3) -0.004(2) -0.001(3) -0.003(3) C26 0.040(4) 0.035(4) 0.040(4) 0.015(3) -0.022(3) -0.021(3) C30 0.033(3) 0.022(3) 0.027(3) 0.000(2) -0.005(3) -0.004(3) C24 0.049(4) 0.028(3) 0.025(3) -0.007(3) -0.003(3) -0.018(3) C25 0.056(4) 0.040(4) 0.023(3) 0.002(3) -0.015(3) -0.024(3) C27 0.019(3) 0.045(4) 0.046(4) 0.020(3) -0.007(3) -0.008(3) C12' 0.017(3) 0.011(3) 0.020(3) -0.005(2) 0.000(2) 0.000(2) O8' 0.049(3) 0.025(2) 0.036(3) -0.002(2) -0.002(2) 0.002(2) C13' 0.020(3) 0.013(3) 0.024(3) 0.004(2) -0.002(2) 0.003(2) O12 0.094(5) 0.125(6) 0.091(5) 0.015(5) -0.051(4) -0.060(5) C38 0.051(5) 0.067(6) 0.055(5) -0.016(4) 0.003(4) -0.020(4) C37 0.066(6) 0.092(7) 0.080(7) 0.015(6) -0.011(5) -0.031(6) Li' 0.020(5) 0.030(5) 0.026(5) -0.005(4) -0.005(4) -0.006(4) Li 0.028(5) 0.025(5) 0.020(5) 0.003(4) -0.006(4) -0.014(4) C39 0.113(7) 0.107(7) 0.125(7) 0.010(6) -0.073(6) -0.040(6) C40 0.091(8) 0.076(7) 0.180(11) -0.025(7) -0.066(8) 0.004(6) O3' 0.024(2) 0.029(2) 0.027(2) -0.0069(17) -0.0081(17) -0.0074(18) O5' 0.029(2) 0.030(2) 0.028(2) -0.0002(18) -0.0016(18) -0.0075(19) O6' 0.022(2) 0.028(2) 0.022(2) -0.0031(17) -0.0027(16) -0.0031(18) O4' 0.026(2) 0.025(2) 0.040(2) -0.0034(19) -0.0086(19) -0.0014(18) C24' 0.028(3) 0.037(4) 0.029(3) -0.007(3) -0.012(3) -0.005(3) C30' 0.029(3) 0.022(3) 0.033(3) -0.004(3) -0.006(3) -0.004(3) C29' 0.029(3) 0.034(3) 0.024(3) -0.004(3) -0.003(3) -0.007(3) C25' 0.018(3) 0.031(3) 0.048(4) -0.008(3) -0.011(3) -0.006(3) C31' 0.024(3) 0.035(4) 0.035(4) -0.004(3) -0.012(3) -0.004(3) C26' 0.038(4) 0.028(4) 0.058(5) 0.003(3) -0.015(3) -0.013(3) C27' 0.033(4) 0.031(4) 0.043(4) 0.015(3) -0.006(3) -0.013(3) C28' 0.036(4) 0.039(4) 0.019(3) -0.003(3) -0.003(3) -0.007(3) 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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 C36 W P 101.76(16) C33 W P 88.98(16) C33 W C36 89.7(2) C34 W P 85.99(16) C34 W C36 170.4(2) C34 W C33 96.2(2) C34 W C35 86.4(2) C32 W P 171.67(16) C32 W C36 86.5(2) C32 W C33 89.7(2) C32 W C34 86.0(2) C32 W C35 90.2(2) C35 W P 91.49(16) C35 W C36 87.8(2) C35 W C33 177.5(2) C35' W' P' 102.98(15) C35' W' C36' 91.5(2) C35' W' C34' 86.6(2) C32' W' P' 169.01(17) C32' W' C35' 86.1(2) C32' W' C33' 88.2(2) C32' W' C36' 86.4(2) C32' W' C34' 94.9(2) C33' W' P' 83.80(16) C33' W' C35' 168.9(2) C33' W' C36' 97.6(2) C33' W' C34' 84.4(2) C36' W' P' 87.17(15) C36' W' C34' 177.6(2) C34' W' P' 91.79(15) O2' P' W' 111.65(14) O2' P' C1' 103.1(2) O2' P' C5' 108.7(2) C1' P' W' 114.07(17) C1' P' C5' 98.9(2) C5' P' W' 118.80(15) C1 P W 113.46(17) C1 P C5 100.2(2) O2 P W 111.52(14) O2 P C1 103.4(2) O2 P C5 107.6(2) C5 P W 119.13(17) O10' C35' W' 173.2(4) C2 O1 H1 109.5 P C1 H1A 108.1 P C1 H1B 108.1 H1A C1 H1B 107.3 C2 C1 P 116.7(3) C2 C1 H1A 108.1 C2 C1 H1B 108.1 O11 C36 W 173.2(5) C23 C18 C5 121.6(5) C23 C18 C19 116.8(5) C19 C18 C5 121.6(5) C2' O1' H1' 109.5 P' O2' Li' 160.7(4) P O2 Li 160.5(4) P' C1' H1'A 107.9 P' C1' H1'B 107.9 H1'A C1' H1'B 107.2 C2' C1' P' 117.5(4) C2' C1' H1'A 107.9 C2' C1' H1'B 107.9 O1 C2 C1 116.7(4) O1 C2 C4 106.8(4) O1 C2 C3 105.4(4) C4 C2 C1 109.1(4) C4 C2 C3 108.2(4) C3 C2 C1 110.2(4) O1' C2' C1' 116.9(5) O1' C2' C3' 106.9(4) O1' C2' C4' 106.0(4) C3' C2' C1' 106.3(4) C3' C2' C4' 108.5(5) C4' C2' C1' 111.9(4) O7' C32' W' 175.3(5) O8 C33 W 177.2(5) C6' C5' P' 114.4(3) C18' C5' P' 106.2(3) C18' C5' C6' 106.1(4) C12' C5' P' 106.3(4) C12' C5' C6' 108.9(4) C12' C5' C18' 115.1(4) F5 C4 F6 104.7(5) F5 C4 C2 113.3(4) F4 C4 F5 106.8(4) F4 C4 F6 106.4(4) F4 C4 C2 115.5(5) F6 C4 C2 109.5(4) C11' C6' C5' 117.2(5) C7' C6' C5' 125.5(5) C7' C6' C11' 117.2(5) O8' C33' W' 172.9(6) C23' C18' C5' 118.4(5) C23' C18' C19' 117.5(5) C19' C18' C5' 123.9(5) C21 C20 H20 119.3 C21 C20 C19 121.5(5) C19 C20 H20 119.3 F2' C3' C2' 114.6(4) F1' C3' F2' 102.3(4) F1' C3' C2' 111.8(5) F3' C3' F2' 103.3(5) F3' C3' C2' 117.2(5) F3' C3' F1' 106.1(5) O9 C34 W 172.8(5) C6 C7 H7 119.3 C8 C7 H7 119.3 C8 C7 C6 121.5(5) C15 C14 H14 120.0 C15 C14 C13 120.0(6) C13 C14 H14 120.0 O7 C32 W 178.4(5) O11' C36' W' 178.7(5) F2 C3 C2 111.3(4) F1 C3 F2 106.9(5) F1 C3 F3 107.1(4) F1 C3 C2 111.4(4) F3 C3 F2 107.1(4) F3 C3 C2 112.8(5) C7 C6 C11 117.7(5) C7 C6 C5 118.3(5) C11 C6 C5 123.7(5) C6 C11 H11 119.5 C10 C11 C6 121.0(5) C10 C11 H11 119.5 C18 C23 H23 118.9 C22 C23 C18 122.2(5) C22 C23 H23 118.9 C6' C11' H11' 119.0 C10' C11' C6' 122.0(6) C10' C11' H11' 119.0 C17 C12 C5 119.7(5) C13 C12 C5 124.0(5) C13 C12 C17 115.9(5) C18 C5 P 106.8(3) C18 C5 C12 110.9(4) C6 C5 P 105.7(3) C6 C5 C18 112.2(4) C6 C5 C12 107.8(4) C12 C5 P 113.4(3) C12 C17 H17 119.1 C16 C17 C12 121.7(5) C16 C17 H17 119.1 C17' C16' H16' 119.6 C17' C16' C15' 120.7(5) C15' C16' H16' 119.6 C18' C23' H23' 119.2 C22' C23' C18' 121.6(5) C22' C23' H23' 119.2 C19' C20' H20' 119.6 C19' C20' C21' 120.8(5) C21' C20' H20' 119.6 C6' C7' H7' 119.4 C6' C7' C8' 121.2(6) C8' C7' H7' 119.4 O9' C34' W' 178.3(5) C14 C15 H15 120.3 C16 C15 C14 119.4(6) C16 C15 H15 120.3 C11 C10 H10 119.9 C9 C10 C11 120.3(6) C9 C10 H10 119.9 C8' C9' H9' 120.2 C8' C9' C10' 119.6(5) C10' C9' H9' 120.2 C7' C8' H8' 119.8 C9' C8' C7' 120.4(6) C9' C8' H8' 119.8 O10 C35 W 176.8(5) C16' C17' H17' 119.3 C16' C17' C12' 121.5(5) C12' C17' H17' 119.3 C23 C22 H22 119.6 C23 C22 C21 120.9(6) C21 C22 H22 119.6 C14 C13 C12 122.3(5) C14 C13 H13 118.9 C12 C13 H13 118.9 C15' C14' H14' 119.5 C15' C14' C13' 121.0(5) C13' C14' H14' 119.5 C20 C21 H21 120.9 C22 C21 C20 118.2(5) C22 C21 H21 120.9 C18 C19 H19 119.8 C20 C19 C18 120.4(6) C20 C19 H19 119.8 C17 C16 H16 119.7 C15 C16 C17 120.6(6) C15 C16 H16 119.7 C7 C8 H8 120.1 C7 C8 C9 119.9(6) C9 C8 H8 120.1 C16' C15' C14' 118.7(5) C16' C15' H15' 120.7 C14' C15' H15' 120.7 C23' C22' H22' 119.8 C21' C22' C23' 120.5(6) C21' C22' H22' 119.8 C10 C9 C8 119.6(5) C10 C9 H9 120.2 C8 C9 H9 120.2 C18' C19' H19' 119.7 C20' C19' C18' 120.7(6) C20' C19' H19' 119.7 C20' C21' H21' 120.6 C22' C21' C20' 118.8(6) C22' C21' H21' 120.6 C11' C10' C9' 119.5(6) C11' C10' H10' 120.2 C9' C10' H10' 120.2 F4' C4' C2' 113.0(5) F4' C4' F5' 106.7(5) F6' C4' F4' 106.8(5) F6' C4' C2' 111.2(5) F6' C4' F5' 106.1(5) F5' C4' C2' 112.5(5) C28 O5 C27 114.3(4) C28 O5 Li 109.0(4) C27 O5 Li 107.9(4) C26 O4 Li 112.1(4) C25 O4 C26 114.7(5) C25 O4 Li 109.8(4) C29 O6 C30 114.0(4) C29 O6 Li 109.2(4) C30 O6 Li 110.4(4) C31 O3 Li 109.9(4) C24 O3 C31 114.6(4) C24 O3 Li 107.9(4) O6 C29 H29A 109.7 O6 C29 H29B 109.7 O6 C29 C28 109.6(4) H29A C29 H29B 108.2 C28 C29 H29A 109.7 C28 C29 H29B 109.7 O5 C28 C29 105.6(4) O5 C28 H28A 110.6 O5 C28 H28B 110.6 C29 C28 H28A 110.6 C29 C28 H28B 110.6 H28A C28 H28B 108.7 O3 C31 H31A 109.6 O3 C31 H31B 109.6 O3 C31 C30 110.4(5) H31A C31 H31B 108.1 C30 C31 H31A 109.6 C30 C31 H31B 109.6 O4 C26 H26A 110.4 O4 C26 H26B 110.4 O4 C26 C27 106.8(5) H26A C26 H26B 108.6 C27 C26 H26A 110.4 C27 C26 H26B 110.4 O6 C30 C31 106.8(4) O6 C30 H30A 110.4 O6 C30 H30B 110.4 C31 C30 H30A 110.4 C31 C30 H30B 110.4 H30A C30 H30B 108.6 O3 C24 H24A 110.6 O3 C24 H24B 110.6 O3 C24 C25 105.6(5) H24A C24 H24B 108.8 C25 C24 H24A 110.6 C25 C24 H24B 110.6 O4 C25 C24 109.1(5) O4 C25 H25A 109.9 O4 C25 H25B 109.9 C24 C25 H25A 109.9 C24 C25 H25B 109.9 H25A C25 H25B 108.3 O5 C27 C26 110.7(5) O5 C27 H27A 109.5 O5 C27 H27B 109.5 C26 C27 H27A 109.5 C26 C27 H27B 109.5 H27A C27 H27B 108.1 C17' C12' C5' 120.2(5) C13' C12' C5' 122.5(5) C13' C12' C17' 117.2(5) C14' C13' H13' 119.5 C12' C13' C14' 121.0(5) C12' C13' H13' 119.5 C39 O12 C38 104.4(8) O12 C38 H38A 110.7 O12 C38 H38B 110.7 O12 C38 C37 105.1(7) H38A C38 H38B 108.8 C37 C38 H38A 110.7 C37 C38 H38B 110.7 C38 C37 H37A 109.5 C38 C37 H37B 109.5 C38 C37 H37C 109.5 H37A C37 H37B 109.5 H37A C37 H37C 109.5 H37B C37 H37C 109.5 O2' Li' O3' 118.6(5) O2' Li' O5' 110.6(5) O2' Li' O6' 104.1(5) O2' Li' O4' 126.0(5) O3' Li' O4' 79.3(4) O5' Li' O3' 130.0(5) O5' Li' O4' 79.1(4) O6' Li' O3' 80.0(4) O6' Li' O5' 80.2(4) O6' Li' O4' 129.7(5) O2 Li O5 127.5(5) O2 Li O4 112.8(5) O2 Li O6 115.2(5) O2 Li O3 101.9(4) O5 Li O6 78.9(3) O4 Li O5 80.8(4) O4 Li O6 130.7(5) O3 Li O5 130.6(5) O3 Li O4 80.7(4) O3 Li O6 79.5(3) O12 C39 H39A 112.8 O12 C39 H39B 112.8 O12 C39 C40 94.9(8) H39A C39 H39B 110.2 C40 C39 H39A 112.8 C40 C39 H39B 112.8 C39 C40 H40A 109.5 C39 C40 H40B 109.5 C39 C40 H40C 109.5 H40A C40 H40B 109.5 H40A C40 H40C 109.5 H40B C40 H40C 109.5 C24' O3' Li' 109.9(4) C31' O3' Li' 109.5(4) C31' O3' C24' 113.8(4) C27' O5' Li' 112.0(4) C27' O5' C28' 114.9(5) C28' O5' Li' 108.6(4) C30' O6' Li' 109.6(4) C30' O6' C29' 114.8(4) C29' O6' Li' 109.5(4) C25' O4' Li' 108.1(4) C26' O4' Li' 109.4(4) C26' O4' C25' 114.1(5) O3' C24' H24C 109.8 O3' C24' H24D 109.8 O3' C24' C25' 109.5(5) H24C C24' H24D 108.2 C25' C24' H24C 109.8 C25' C24' H24D 109.8 O6' C30' H30C 109.5 O6' C30' H30D 109.5 O6' C30' C31' 110.6(5) H30C C30' H30D 108.1 C31' C30' H30C 109.5 C31' C30' H30D 109.5 O6' C29' H29C 110.6 O6' C29' H29D 110.6 O6' C29' C28' 105.7(4) H29C C29' H29D 108.7 C28' C29' H29C 110.6 C28' C29' H29D 110.6 O4' C25' C24' 106.8(5) O4' C25' H25C 110.4 O4' C25' H25D 110.4 C24' C25' H25C 110.4 C24' C25' H25D 110.4 H25C C25' H25D 108.6 O3' C31' C30' 107.3(5) O3' C31' H31C 110.3 O3' C31' H31D 110.3 C30' C31' H31C 110.3 C30' C31' H31D 110.3 H31C C31' H31D 108.5 O4' C26' H26C 109.5 O4' C26' H26D 109.5 O4' C26' C27' 110.6(5) H26C C26' H26D 108.1 C27' C26' H26C 109.5 C27' C26' H26D 109.5 O5' C27' C26' 106.8(5) O5' C27' H27C 110.4 O5' C27' H27D 110.4 C26' C27' H27C 110.4 C26' C27' H27D 110.4 H27C C27' H27D 108.6 O5' C28' C29' 110.4(5) O5' C28' H28C 109.6 O5' C28' H28D 109.6 C29' C28' H28C 109.6 C29' C28' H28D 109.6 H28C C28' H28D 108.1 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance W P 2.5761(14) W C36 2.046(6) W C33 2.044(6) W C34 2.031(6) W C32 1.982(7) W C35 2.043(6) W' P' 2.5627(13) W' C35' 2.037(6) W' C32' 1.992(6) W' C33' 2.030(6) W' C36' 2.037(6) W' C34' 2.049(6) P' O2' 1.541(3) P' C1' 1.901(5) P' C5' 1.951(5) P C1 1.891(5) P O2 1.542(4) P C5 1.949(5) O10' C35' 1.146(6) F5 C4 1.353(6) F2 C3 1.346(6) F4 C4 1.330(6) F2' C3' 1.395(6) O11 C36 1.143(7) F1 C3 1.329(6) O1 H1 0.8400 O1 C2 1.393(6) C1 H1A 0.9900 C1 H1B 0.9900 C1 C2 1.559(7) C18 C23 1.378(8) C18 C5 1.532(7) C18 C19 1.414(7) F3 C3 1.332(6) O1' H1' 0.8400 O1' C2' 1.388(6) O2' Li' 1.845(10) O8 C33 1.132(6) F6 C4 1.358(6) O2 Li 1.848(10) O10 C35 1.145(6) C1' H1'A 0.9900 C1' H1'B 0.9900 C1' C2' 1.550(7) F4' C4' 1.332(6) C2 C4 1.534(8) C2 C3 1.545(8) O7' C32' 1.155(6) F6' C4' 1.322(7) C2' C3' 1.478(8) C2' C4' 1.540(8) C5' C6' 1.550(7) C5' C18' 1.537(7) C5' C12' 1.535(7) O9' C34' 1.151(7) O11' C36' 1.136(7) C6' C11' 1.392(8) C6' C7' 1.378(7) C33' O8' 1.154(6) C18' C23' 1.391(8) C18' C19' 1.401(7) C20 H20 0.9500 C20 C21 1.377(9) C20 C19 1.383(8) C3' F1' 1.356(7) C3' F3' 1.341(7) O9 C34 1.141(7) O7 C32 1.160(7) C7 H7 0.9500 C7 C6 1.387(7) C7 C8 1.380(7) C14 H14 0.9500 C14 C15 1.373(8) C14 C13 1.388(8) C6 C11 1.392(7) C6 C5 1.530(7) C11 H11 0.9500 C11 C10 1.387(8) F5' C4' 1.341(7) C23 H23 0.9500 C23 C22 1.375(8) C11' H11' 0.9500 C11' C10' 1.377(8) C12 C5 1.538(8) C12 C17 1.398(7) C12 C13 1.392(7) C17 H17 0.9500 C17 C16 1.387(8) C16' H16' 0.9500 C16' C17' 1.375(8) C16' C15' 1.381(8) C23' H23' 0.9500 C23' C22' 1.383(8) C20' H20' 0.9500 C20' C19' 1.384(8) C20' C21' 1.391(8) C7' H7' 0.9500 C7' C8' 1.390(8) C15 H15 0.9500 C15 C16 1.364(9) C10 H10 0.9500 C10 C9 1.372(8) C9' H9' 0.9500 C9' C8' 1.364(9) C9' C10' 1.381(9) C8' H8' 0.9500 C17' H17' 0.9500 C17' C12' 1.412(7) C22 H22 0.9500 C22 C21 1.375(8) C13 H13 0.9500 C14' H14' 0.9500 C14' C15' 1.385(8) C14' C13' 1.391(8) C21 H21 0.9500 C19 H19 0.9500 C16 H16 0.9500 C8 H8 0.9500 C8 C9 1.387(8) C15' H15' 0.9500 C22' H22' 0.9500 C22' C21' 1.378(8) C9 H9 0.9500 C19' H19' 0.9500 C21' H21' 0.9500 C10' H10' 0.9500 O5 C28 1.433(6) O5 C27 1.442(7) O5 Li 2.089(10) O4 C26 1.432(7) O4 C25 1.432(7) O4 Li 2.078(10) O6 C29 1.437(6) O6 C30 1.437(6) O6 Li 2.164(10) O3 C31 1.453(7) O3 C24 1.432(7) O3 Li 2.078(10) C29 H29A 0.9900 C29 H29B 0.9900 C29 C28 1.505(8) C28 H28A 0.9900 C28 H28B 0.9900 C31 H31A 0.9900 C31 H31B 0.9900 C31 C30 1.495(7) C26 H26A 0.9900 C26 H26B 0.9900 C26 C27 1.498(9) C30 H30A 0.9900 C30 H30B 0.9900 C24 H24A 0.9900 C24 H24B 0.9900 C24 C25 1.512(8) C25 H25A 0.9900 C25 H25B 0.9900 C27 H27A 0.9900 C27 H27B 0.9900 C12' C13' 1.387(7) C13' H13' 0.9500 O12 C38 1.480(10) O12 C39 1.409(8) C38 H38A 0.9900 C38 H38B 0.9900 C38 C37 1.540(11) C37 H37A 0.9800 C37 H37B 0.9800 C37 H37C 0.9800 Li' O3' 2.129(10) Li' O5' 2.113(10) Li' O6' 2.084(10) Li' O4' 2.133(10) C39 H39A 0.9900 C39 H39B 0.9900 C39 C40 1.701(15) C40 H40A 0.9800 C40 H40B 0.9800 C40 H40C 0.9800 O3' C24' 1.442(7) O3' C31' 1.441(7) O5' C27' 1.421(7) O5' C28' 1.428(7) O6' C30' 1.426(7) O6' C29' 1.439(6) O4' C25' 1.429(7) O4' C26' 1.419(7) C24' H24C 0.9900 C24' H24D 0.9900 C24' C25' 1.500(8) C30' H30C 0.9900 C30' H30D 0.9900 C30' C31' 1.485(8) C29' H29C 0.9900 C29' H29D 0.9900 C29' C28' 1.495(8) C25' H25C 0.9900 C25' H25D 0.9900 C31' H31C 0.9900 C31' H31D 0.9900 C26' H26C 0.9900 C26' H26D 0.9900 C26' C27' 1.516(9) C27' H27C 0.9900 C27' H27D 0.9900 C28' H28C 0.9900 C28' H28D 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 W P C1 C2 -84.2(4) W P O2 Li -85.7(11) W' P' O2' Li' 82.3(12) P' O2' Li' O3' -72.5(13) P' O2' Li' O5' 116.6(10) P' O2' Li' O6' -158.7(9) P' O2' Li' O4' 25.3(16) P' C1' C2' O1' 15.8(6) P' C1' C2' C3' 135.0(4) P' C1' C2' C4' -106.7(5) P' C5' C6' C11' 164.6(4) P' C5' C6' C7' -20.3(7) P' C5' C18' C23' -58.2(5) P' C5' C18' C19' 126.8(5) P' C5' C12' C17' -65.1(5) P' C5' C12' C13' 111.5(5) P C1 C2 O1 -5.6(6) P C1 C2 C4 -126.8(4) P C1 C2 C3 114.5(4) P O2 Li O5 -18.3(16) P O2 Li O4 -114.2(10) P O2 Li O6 77.0(12) P O2 Li O3 160.9(9) O1 C2 C4 F5 62.7(5) O1 C2 C4 F4 -173.7(4) O1 C2 C4 F6 -53.7(5) O1 C2 C3 F2 -167.5(4) O1 C2 C3 F1 73.4(5) O1 C2 C3 F3 -47.1(6) C1 P O2 Li 152.1(11) C1 C2 C4 F5 -170.3(4) C1 C2 C4 F4 -46.7(6) C1 C2 C4 F6 73.3(5) C1 C2 C3 F2 65.7(5) C1 C2 C3 F1 -53.4(6) C1 C2 C3 F3 -173.9(4) C18 C23 C22 C21 -1.7(9) O1' C2' C3' F2' -58.9(6) O1' C2' C3' F1' 56.9(6) O1' C2' C3' F3' 179.7(5) O1' C2' C4' F4' 50.2(6) O1' C2' C4' F6' -69.9(5) O1' C2' C4' F5' 171.2(4) O2 P C1 C2 36.7(4) C1' P' O2' Li' -154.8(11) C1' C2' C3' F2' 175.5(5) C1' C2' C3' F1' -68.6(6) C1' C2' C3' F3' 54.2(7) C1' C2' C4' F4' 178.8(4) C1' C2' C4' F6' 58.6(6) C1' C2' C4' F5' -60.3(6) C5' P' O2' Li' -50.6(12) C5' C6' C11' C10' 175.1(5) C5' C6' C7' C8' -174.3(5) C5' C18' C23' C22' -176.7(5) C5' C18' C19' C20' 176.5(5) C5' C12' C13' C14' -177.9(5) C4 C2 C3 F2 -53.5(6) C4 C2 C3 F1 -172.6(4) C4 C2 C3 F3 66.9(6) C6' C5' C18' C23' 64.0(6) C6' C5' C18' C19' -111.0(5) C6' C5' C12' C17' 171.1(5) C6' C5' C12' C13' -12.2(7) C6' C11' C10' C9' -1.1(9) C6' C7' C8' C9' 0.4(9) C18' C5' C6' C11' 47.9(6) C18' C5' C6' C7' -137.0(5) C18' C5' C12' C17' 52.1(7) C18' C5' C12' C13' -131.2(5) C18' C23' C22' C21' 0.8(9) C3' C2' C4' F4' -64.3(6) C3' C2' C4' F6' 175.6(4) C3' C2' C4' F5' 56.7(6) C7 C6 C11 C10 -2.4(8) C7 C6 C5 P 54.2(6) C7 C6 C5 C18 170.2(5) C7 C6 C5 C12 -67.4(6) C7 C8 C9 C10 1.0(10) C14 C15 C16 C17 -1.6(9) C3 C2 C4 F5 -50.3(6) C3 C2 C4 F4 73.3(5) C3 C2 C4 F6 -166.7(4) C6 C7 C8 C9 -2.6(9) C6 C11 C10 C9 0.9(9) C11 C6 C5 P -131.9(5) C11 C6 C5 C18 -15.9(7) C11 C6 C5 C12 106.5(6) C11 C10 C9 C8 -0.2(10) C23 C18 C5 P 59.2(5) C23 C18 C5 C6 -56.3(6) C23 C18 C5 C12 -176.8(5) C23 C18 C19 C20 -0.9(8) C23 C22 C21 C20 0.6(9) C11' C6' C7' C8' 0.8(8) C12 C17 C16 C15 1.4(9) C5 P C1 C2 147.7(4) C5 P O2 Li 46.7(12) C5 C18 C23 C22 -175.3(5) C5 C18 C19 C20 176.2(5) C5 C6 C11 C10 -176.3(5) C5 C12 C17 C16 -173.4(5) C5 C12 C13 C14 172.3(5) C17 C12 C5 P -155.3(4) C17 C12 C5 C18 84.6(6) C17 C12 C5 C6 -38.6(6) C17 C12 C13 C14 -0.3(8) C16' C17' C12' C5' 178.1(5) C16' C17' C12' C13' 1.3(8) C23' C18' C19' C20' 1.5(8) C23' C22' C21' C20' -0.2(9) C7' C6' C11' C10' -0.4(9) C15 C14 C13 C12 0.1(8) C8' C9' C10' C11' 2.4(10) C17' C16' C15' C14' -0.8(9) C17' C12' C13' C14' -1.1(8) C13 C14 C15 C16 0.9(8) C13 C12 C5 P 32.4(6) C13 C12 C5 C18 -87.7(6) C13 C12 C5 C6 149.1(5) C13 C12 C17 C16 -0.4(8) C21 C20 C19 C18 -0.2(9) C19 C18 C23 C22 1.8(8) C19 C18 C5 P -117.8(5) C19 C18 C5 C6 126.8(5) C19 C18 C5 C12 6.2(7) C19 C20 C21 C22 0.3(9) C8 C7 C6 C11 3.2(9) C8 C7 C6 C5 177.5(5) C15' C16' C17' C12' -0.4(9) C15' C14' C13' C12' 0.0(9) C19' C18' C23' C22' -1.4(8) C19' C20' C21' C22' 0.3(9) C21' C20' C19' C18' -1.0(8) C10' C9' C8' C7' -2.0(10) C4' C2' C3' F2' 55.0(6) C4' C2' C3' F1' 170.9(4) C4' C2' C3' F3' -66.4(6) O4 C26 C27 O5 51.9(6) O6 C29 C28 O5 56.3(6) O3 C31 C30 O6 53.6(6) O3 C24 C25 O4 56.2(6) C29 O6 C30 C31 -161.6(5) C28 O5 C27 C26 79.5(6) C31 O3 C24 C25 -171.9(4) C26 O4 C25 C24 92.6(6) C30 O6 C29 C28 91.1(6) C24 O3 C31 C30 79.3(6) C25 O4 C26 C27 -162.0(5) C27 O5 C28 C29 -172.5(4) C12' C5' C6' C11' -76.6(6) C12' C5' C6' C7' 98.5(6) C12' C5' C18' C23' -175.5(5) C12' C5' C18' C19' 9.5(7) C13' C14' C15' C16' 1.0(9) C38 O12 C39 C40 178.9(7) Li' O3' C24' C25' 35.0(6) Li' O3' C31' C30' 39.6(6) Li' O5' C27' C26' 39.3(6) Li' O5' C28' C29' 37.6(6) Li' O6' C30' C31' 40.6(6) Li' O6' C29' C28' 45.7(6) Li' O4' C25' C24' 48.7(6) Li' O4' C26' C27' 39.6(6) Li O5 C28 C29 -51.7(5) Li O5 C27 C26 -41.9(6) Li O4 C26 C27 -35.9(6) Li O4 C25 C24 -34.7(6) Li O6 C29 C28 -32.9(6) Li O6 C30 C31 -38.2(6) Li O3 C31 C30 -42.3(6) Li O3 C24 C25 -49.1(5) C39 O12 C38 C37 -179.9(8) O3' C24' C25' O4' -56.4(6) O6' C30' C31' O3' -53.9(6) O6' C29' C28' O5' -55.9(6) O4' C26' C27' O5' -52.7(7) C24' O3' C31' C30' 163.0(5) C30' O6' C29' C28' 169.5(5) C29' O6' C30' C31' -83.2(6) C25' O4' C26' C27' -81.6(6) C31' O3' C24' C25' -88.2(6) C26' O4' C25' C24' 170.6(5) C27' O5' C28' C29' -88.7(6) C28' O5' C27' C26' 163.9(5)