#------------------------------------------------------------------------------ #$Date: 2021-10-14 01:24:52 +0300 (Thu, 14 Oct 2021) $ #$Revision: 269924 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/49/1564906.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_1564906 loop_ _publ_author_name 'Xu, Hui' 'Tian, Yuee' 'Wang, Huiqin' 'Man, Yi' 'Zhang, Jing' 'Zhang, Nan' 'Li, Ying' 'Han, Chunmiao' _publ_section_title ; Weaving host matrixes with intermolecular hydrogen bonds for high-efficiency white thermally activated delayed fluorescence ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D1SC04188F _journal_year 2021 _chemical_formula_moiety 'C60 H46 O4 P4 S, H2 O' _chemical_formula_sum 'C60 H48 O5 P4 S' _chemical_formula_weight 1004.92 _chemical_name_common DPSQPO _chemical_name_systematic DPSQPO _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_date 2017-10-17 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _audit_update_record ; 2021-07-30 deposited with the CCDC. 2021-10-07 downloaded from the CCDC. ; _cell_angle_alpha 100.306(5) _cell_angle_beta 97.237(5) _cell_angle_gamma 97.345(5) _cell_formula_units_Z 2 _cell_length_a 9.412(5) _cell_length_b 15.749(5) _cell_length_c 18.441(5) _cell_measurement_reflns_used 9988 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.251 _cell_measurement_theta_min 2.394 _cell_volume 2636.1(18) _computing_cell_refinement 'SAINT V8.18C (?, 2016)' _computing_data_reduction 'SAINT V8.18C (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.956 _diffrn_measured_fraction_theta_max 0.956 _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0185 _diffrn_reflns_av_unetI/netI 0.0272 _diffrn_reflns_Laue_measured_fraction_full 0.956 _diffrn_reflns_Laue_measured_fraction_max 0.956 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 17702 _diffrn_reflns_point_group_measured_fraction_full 0.956 _diffrn_reflns_point_group_measured_fraction_max 0.956 _diffrn_reflns_theta_full 24.999 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_min 2.271 _exptl_absorpt_coefficient_mu 0.232 _exptl_absorpt_correction_T_max 0.942 _exptl_absorpt_correction_T_min 0.938 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.266 _exptl_crystal_description block _exptl_crystal_F_000 1048 _exptl_crystal_preparation Luminescent _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.23 _refine_diff_density_max 0.345 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.055 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 634 _refine_ls_number_reflns 8892 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.046 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0407 _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^)+(0.0694P)^2^+1.1640P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1166 _refine_ls_wR_factor_ref 0.1254 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7644 _reflns_number_total 8892 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc04188f2.cif _cod_data_source_block 123 _cod_database_code 1564906 _shelx_shelxl_version_number 2016/6 _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 0.949 _shelx_estimated_absorpt_t_min 0.942 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All O(H,H) groups 2.a Free rotating group: O1(H1A,H1B) 2.b Aromatic/amide H refined with riding coordinates: C12(H12), C14(H14), C16(H16), C17(H17), C19(H19), C21(H21), C24(H24), C26(H26), C30(H30), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C67(H67), C68(H68), C69(H69), C70(H70) ; _shelx_res_file ; TITL 123 in P-1 123.res created by SHELXL-2016/6 at 09:49:17 on 17-Oct-2017 CELL 0.71069 9.412 15.749 18.441 100.306 97.237 97.345 ZERR 2 0.005 0.005 0.005 0.005 0.005 0.005 LATT 1 SFAC C H O P S UNIT 120 96 10 8 2 L.S. 4 PLAN 25 SIZE 0.26 0.24 0.23 LIST 1 fmap 2 ACTA MERG 2 OMIT -3 50 REM REM REM WGHT 0.069400 1.164000 FVAR 0.16367 P1 4 -0.055314 -0.204805 0.150384 11.00000 0.04682 0.03036 = 0.03346 0.00559 0.01136 0.00783 P2 4 -0.194913 -0.180699 0.436725 11.00000 0.04563 0.03484 = 0.03071 0.00593 0.01079 0.00230 S3 5 0.190803 -0.035800 0.212686 11.00000 0.04460 0.02965 = 0.04770 0.00979 0.02064 0.00802 P4 4 0.485311 0.099280 0.215253 11.00000 0.03134 0.03683 = 0.05499 0.00643 0.01525 0.00907 P5 4 0.183066 0.375481 0.271486 11.00000 0.04246 0.03057 = 0.04689 0.00458 0.00870 0.00838 O6 3 0.066627 0.400771 0.314192 11.00000 0.06199 0.04575 = 0.06400 0.00562 0.02280 0.01978 O7 3 0.081802 -0.237837 0.137008 11.00000 0.05735 0.04580 = 0.05888 0.00653 0.02038 0.01851 O8 3 0.477158 0.013841 0.164748 11.00000 0.04943 0.04074 = 0.07111 0.00236 0.02496 0.00878 O9 3 -0.179716 -0.119873 0.509306 11.00000 0.07145 0.04825 = 0.03755 -0.00181 0.01711 0.00076 C10 1 -0.039786 -0.142694 0.244701 11.00000 0.04099 0.02836 = 0.03296 0.00796 0.00843 0.00968 C11 1 0.070440 -0.070476 0.272452 11.00000 0.03727 0.02942 = 0.03823 0.01140 0.01039 0.00862 C12 1 0.010584 -0.063911 0.395936 11.00000 0.04651 0.03453 = 0.03376 0.00387 0.00681 0.00566 AFIX 43 H12 2 0.029120 -0.038412 0.446390 11.00000 -1.20000 AFIX 0 C13 1 0.185816 0.078126 0.227742 11.00000 0.03276 0.03052 = 0.03523 0.00987 0.00679 0.00502 C14 1 0.303958 0.224180 0.233318 11.00000 0.03174 0.03173 = 0.05829 0.00699 0.01174 0.00214 AFIX 43 H14 2 0.385349 0.262134 0.229084 11.00000 -1.20000 AFIX 0 C15 1 -0.110348 -0.276555 0.444559 11.00000 0.03970 0.04139 = 0.04139 0.01630 0.00730 -0.00054 C16 1 -0.125796 -0.171866 0.294349 11.00000 0.04093 0.02984 = 0.03532 0.00753 0.00659 0.00130 AFIX 43 H16 2 -0.201757 -0.217734 0.276498 11.00000 -1.20000 AFIX 0 C17 1 0.093549 -0.031999 0.347434 11.00000 0.04341 0.03154 = 0.04207 0.00423 0.00871 0.00096 AFIX 43 H17 2 0.165893 0.015930 0.365267 11.00000 -1.20000 AFIX 0 C18 1 -0.115190 -0.137602 0.087220 11.00000 0.04974 0.03495 = 0.03196 0.00640 0.00712 0.00116 C19 1 0.058176 0.200964 0.252969 11.00000 0.03226 0.03986 = 0.05927 0.01494 0.01488 0.01277 AFIX 43 H19 2 -0.026057 0.222430 0.263562 11.00000 -1.20000 AFIX 0 C20 1 -0.100751 -0.134045 0.369900 11.00000 0.04276 0.02893 = 0.03372 0.00779 0.00810 0.00712 C21 1 -0.091148 -0.336504 0.383191 11.00000 0.06265 0.04594 = 0.04901 0.01285 0.01013 0.01318 AFIX 43 H21 2 -0.131597 -0.331377 0.335788 11.00000 -1.20000 AFIX 0 C22 1 0.591057 0.184872 0.182539 11.00000 0.03052 0.04103 = 0.06611 0.01084 0.01595 0.00954 C23 1 0.310713 0.135180 0.223374 11.00000 0.02935 0.03443 = 0.04254 0.00665 0.00803 0.00716 C24 1 0.165376 0.502124 0.187487 11.00000 0.08258 0.05227 = 0.07031 0.02122 0.02474 0.03068 AFIX 43 H24 2 0.157509 0.537533 0.232463 11.00000 -1.20000 AFIX 0 C25 1 0.177983 0.415315 0.185478 11.00000 0.04031 0.04054 = 0.05055 0.00903 0.00151 0.00278 C26 1 0.060772 0.112172 0.240991 11.00000 0.03018 0.03699 = 0.06051 0.01569 0.01245 0.00369 AFIX 43 H26 2 -0.023190 0.074393 0.241831 11.00000 -1.20000 AFIX 0 C27 1 -0.202886 -0.293545 0.142190 11.00000 0.06244 0.03239 = 0.03613 0.00227 0.01354 0.00275 C28 1 -0.379382 -0.216310 0.391506 11.00000 0.04328 0.04536 = 0.04266 0.00877 0.01293 0.00857 C29 1 0.180348 0.258250 0.249294 11.00000 0.03601 0.03137 = 0.04681 0.00689 0.00809 0.00905 C30 1 -0.063967 -0.145420 0.019538 11.00000 0.06038 0.05870 = 0.03760 0.00994 0.01224 0.00311 AFIX 43 H30 2 0.003853 -0.182121 0.008969 11.00000 -1.20000 AFIX 0 C31 1 0.363967 0.414199 0.321921 11.00000 0.05367 0.03635 = 0.05281 0.00511 -0.00077 0.00091 C32 1 0.563536 0.103416 0.310596 11.00000 0.03538 0.04840 = 0.06130 0.01220 0.01046 0.01285 C33 1 -0.456514 -0.293890 0.398892 11.00000 0.05185 0.05771 = 0.10369 0.02383 0.00397 0.00216 AFIX 43 H33 2 -0.410187 -0.332005 0.423176 11.00000 -1.20000 AFIX 0 C34 1 -0.013255 -0.403671 0.390935 11.00000 0.06474 0.04778 = 0.08077 0.02240 0.02555 0.01655 AFIX 43 H34 2 -0.001484 -0.443507 0.349191 11.00000 -1.20000 AFIX 0 C35 1 -0.215724 -0.081983 0.102441 11.00000 0.06650 0.05023 = 0.04340 0.01200 0.01081 0.01564 AFIX 43 H35 2 -0.249788 -0.075972 0.148004 11.00000 -1.20000 AFIX 0 C36 1 0.678180 0.256350 0.229552 11.00000 0.03833 0.04969 = 0.08386 0.01433 0.00481 0.00626 AFIX 43 H36 2 0.683265 0.262686 0.280972 11.00000 -1.20000 AFIX 0 C37 1 0.703024 0.085738 0.325084 11.00000 0.05260 0.07347 = 0.08638 0.02131 0.01432 0.03153 AFIX 43 H37 2 0.753462 0.070819 0.285609 11.00000 -1.20000 AFIX 0 C38 1 -0.265138 -0.035649 0.050120 11.00000 0.07779 0.05789 = 0.07054 0.02292 0.00102 0.02171 AFIX 43 H38 2 -0.333333 0.000950 0.060172 11.00000 -1.20000 AFIX 0 C39 1 -0.052604 -0.286275 0.514847 11.00000 0.08327 0.07031 = 0.04496 0.02208 0.00451 0.01548 AFIX 43 H39 2 -0.065711 -0.247648 0.557047 11.00000 -1.20000 AFIX 0 C40 1 -0.167856 -0.371542 0.157898 11.00000 0.08577 0.04150 = 0.07303 0.01619 0.02352 0.01156 AFIX 43 H40 2 -0.071950 -0.376619 0.173450 11.00000 -1.20000 AFIX 0 C41 1 -0.346115 -0.287218 0.121295 11.00000 0.05823 0.06378 = 0.08863 0.02642 0.00419 -0.00580 AFIX 43 H41 2 -0.371082 -0.234736 0.111365 11.00000 -1.20000 AFIX 0 C42 1 0.472747 0.456226 0.293163 11.00000 0.05557 0.07011 = 0.06701 0.01674 -0.00176 -0.00680 AFIX 43 H42 2 0.453470 0.468810 0.245842 11.00000 -1.20000 AFIX 0 C43 1 0.583572 0.177431 0.106584 11.00000 0.07461 0.05555 = 0.07086 0.01272 0.02693 0.00635 AFIX 43 H43 2 0.524143 0.130300 0.074662 11.00000 -1.20000 AFIX 0 C45 1 0.164216 0.537506 0.123815 11.00000 0.07284 0.07057 = 0.09890 0.04556 0.02218 0.02714 AFIX 43 H45 2 0.158509 0.596457 0.126350 11.00000 -1.20000 AFIX 0 C46 1 0.610688 0.480473 0.332704 11.00000 0.05730 0.07821 = 0.09700 0.01673 -0.00476 -0.00746 AFIX 43 H46 2 0.683159 0.509367 0.312080 11.00000 -1.20000 AFIX 0 C47 1 -0.213485 -0.043656 -0.016801 11.00000 0.08427 0.07603 = 0.06146 0.03747 -0.01103 0.00209 AFIX 43 H47 2 -0.245990 -0.011849 -0.051748 11.00000 -1.20000 AFIX 0 C48 1 0.768824 0.089777 0.396831 11.00000 0.06471 0.08912 = 0.10578 0.02322 -0.00821 0.04142 AFIX 43 H48 2 0.864105 0.079673 0.405621 11.00000 -1.20000 AFIX 0 C49 1 -0.450038 -0.161765 0.354118 11.00000 0.05734 0.08034 = 0.10000 0.04513 0.01180 0.01650 AFIX 43 H49 2 -0.400069 -0.108720 0.349183 11.00000 -1.20000 AFIX 0 C50 1 0.046383 -0.411055 0.460530 11.00000 0.06748 0.07147 = 0.10201 0.04233 0.01570 0.02652 AFIX 43 H50 2 0.101685 -0.455038 0.466008 11.00000 -1.20000 AFIX 0 C51 1 0.025659 -0.354833 0.521678 11.00000 0.10118 0.09715 = 0.07552 0.04509 -0.00870 0.03202 AFIX 43 H51 2 0.064027 -0.361963 0.568817 11.00000 -1.20000 AFIX 0 C52 1 0.490234 0.120681 0.369802 11.00000 0.05802 0.15231 = 0.05829 0.00787 0.00672 0.04988 AFIX 43 H52 2 0.394750 0.130589 0.361620 11.00000 -1.20000 AFIX 0 C53 1 -0.114187 -0.098332 -0.032362 11.00000 0.07808 0.09394 = 0.03786 0.02706 0.00706 -0.00225 AFIX 43 H53 2 -0.080416 -0.103812 -0.077990 11.00000 -1.20000 AFIX 0 C54 1 0.757603 0.318277 0.199706 11.00000 0.04711 0.04710 = 0.12713 0.02277 0.00620 0.00075 AFIX 43 H54 2 0.815689 0.366244 0.231244 11.00000 -1.20000 AFIX 0 C55 1 0.663988 0.239686 0.077094 11.00000 0.11454 0.08073 = 0.09262 0.03687 0.04864 0.01586 AFIX 43 H55 2 0.658636 0.234081 0.025717 11.00000 -1.20000 AFIX 0 C56 1 -0.670369 -0.262166 0.333033 11.00000 0.04923 0.11285 = 0.14813 0.01859 -0.01094 0.00917 AFIX 43 H56 2 -0.768253 -0.277589 0.313565 11.00000 -1.20000 AFIX 0 C57 1 0.751006 0.309215 0.124040 11.00000 0.08020 0.06306 = 0.13673 0.04261 0.04774 0.00738 AFIX 43 H57 2 0.805915 0.350502 0.104483 11.00000 -1.20000 AFIX 0 C58 1 -0.277464 -0.442791 0.150272 11.00000 0.14227 0.03913 = 0.10212 0.02367 0.03773 0.00230 AFIX 43 H58 2 -0.254089 -0.495550 0.160336 11.00000 -1.20000 AFIX 0 C59 1 0.640468 0.462609 0.400428 11.00000 0.07973 0.10849 = 0.11980 0.04392 -0.04153 -0.02266 AFIX 43 H59 2 0.733118 0.479844 0.427521 11.00000 -1.20000 AFIX 0 C60 1 -0.602195 -0.315452 0.370473 11.00000 0.05395 0.08070 = 0.17188 0.02428 -0.00178 -0.01027 AFIX 43 H60 2 -0.653912 -0.367154 0.377163 11.00000 -1.20000 AFIX 0 C61 1 -0.453116 -0.357904 0.114914 11.00000 0.07477 0.08858 = 0.13489 0.04088 0.00006 -0.02522 AFIX 43 H61 2 -0.549686 -0.352582 0.101445 11.00000 -1.20000 AFIX 0 C62 1 0.694901 0.108483 0.454801 11.00000 0.09152 0.15230 = 0.07427 0.02058 -0.01192 0.05602 AFIX 43 H62 2 0.739131 0.110926 0.503314 11.00000 -1.20000 AFIX 0 C63 1 0.186924 0.364780 0.118397 11.00000 0.17407 0.04918 = 0.05037 0.00266 0.01569 0.00829 AFIX 43 H63 2 0.195072 0.306040 0.115197 11.00000 -1.20000 AFIX 0 C64 1 0.395514 0.396603 0.390713 11.00000 0.10996 0.18492 = 0.08620 0.07732 -0.03746 -0.07225 AFIX 43 H64 2 0.323134 0.369058 0.412280 11.00000 -1.20000 AFIX 0 C65 1 0.171458 0.485525 0.058021 11.00000 0.10859 0.10216 = 0.06757 0.04274 0.00616 0.01382 AFIX 43 H65 2 0.167831 0.508392 0.014807 11.00000 -1.20000 AFIX 0 C66 1 -0.595321 -0.185549 0.323794 11.00000 0.06320 0.12817 = 0.13302 0.06033 0.00079 0.03431 AFIX 43 H66 2 -0.641675 -0.149394 0.297186 11.00000 -1.20000 AFIX 0 C67 1 0.556809 0.123541 0.441746 11.00000 0.09953 0.24548 = 0.05719 0.01125 0.00952 0.08536 AFIX 43 H67 2 0.505946 0.135951 0.481465 11.00000 -1.20000 AFIX 0 C68 1 -0.417638 -0.435495 0.128299 11.00000 0.11074 0.07721 = 0.12004 0.02481 0.01630 -0.03527 AFIX 43 H68 2 -0.489705 -0.483536 0.122352 11.00000 -1.20000 AFIX 0 C69 1 0.535933 0.419587 0.429314 11.00000 0.14363 0.25262 = 0.12698 0.12169 -0.08019 -0.09363 AFIX 43 H69 2 0.557692 0.404979 0.475699 11.00000 -1.20000 AFIX 0 C70 1 0.183885 0.400887 0.054812 11.00000 0.23361 0.08369 = 0.04869 0.00948 0.01665 0.01472 AFIX 43 H70 2 0.190546 0.365975 0.009398 11.00000 -1.20000 AFIX 6 O1 3 0.374840 -0.174470 0.109621 11.00000 0.10480 0.09102 = 0.13337 -0.00654 0.05529 0.02844 H1A 2 0.404636 -0.155712 0.155881 11.00000 -1.50000 H1B 2 0.348949 -0.132920 0.089952 11.00000 -1.50000 AFIX 0 HKLF 4 REM 123 in P-1 REM R1 = 0.0407 for 7644 Fo > 4sig(Fo) and 0.0479 for all 8892 data REM 634 parameters refined using 0 restraints END WGHT 0.0694 1.1640 REM Highest difference peak 0.345, deepest hole -0.320, 1-sigma level 0.055 Q1 1 0.2702 -0.1860 0.1275 11.00000 0.05 0.35 Q2 1 0.3932 0.1229 0.2205 11.00000 0.05 0.34 Q3 1 0.5388 0.1489 0.1968 11.00000 0.05 0.29 Q4 1 0.5471 0.1860 0.3612 11.00000 0.05 0.29 Q5 1 -0.1382 -0.1554 0.3985 11.00000 0.05 0.27 Q6 1 0.3669 0.4186 0.4120 11.00000 0.05 0.26 Q7 1 0.3032 0.4030 0.4206 11.00000 0.05 0.25 Q8 1 0.5199 0.4580 0.4493 11.00000 0.05 0.24 Q9 1 0.3761 0.3401 0.3902 11.00000 0.05 0.24 Q10 1 0.5075 0.4453 0.4803 11.00000 0.05 0.23 Q11 1 0.0135 -0.1199 0.2533 11.00000 0.05 0.23 Q12 1 0.6180 0.2019 0.4399 11.00000 0.05 0.22 Q13 1 0.5293 0.0985 0.2670 11.00000 0.05 0.22 Q14 1 -0.0489 -0.1726 0.2063 11.00000 0.05 0.21 Q15 1 0.6542 0.2010 0.2084 11.00000 0.05 0.21 Q16 1 -0.0763 -0.1617 0.1163 11.00000 0.05 0.21 Q17 1 -0.2177 -0.0806 0.5044 11.00000 0.05 0.21 Q18 1 -0.0733 -0.1467 0.2594 11.00000 0.05 0.21 Q19 1 0.2745 0.3981 0.3074 11.00000 0.05 0.21 Q20 1 0.6212 0.1676 0.1537 11.00000 0.05 0.20 Q21 1 0.1883 0.3117 0.2611 11.00000 0.05 0.20 Q22 1 0.0815 -0.0736 0.3751 11.00000 0.05 0.20 Q23 1 0.1369 -0.2045 0.1300 11.00000 0.05 0.19 Q24 1 -0.0826 -0.1598 0.3441 11.00000 0.05 0.19 Q25 1 0.1882 0.4020 0.2240 11.00000 0.05 0.19 ; _shelx_res_checksum 22163 _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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group P1 P -0.05531(6) -0.20480(3) 0.15038(3) 0.03634(14) Uani 1 1 d . . . . . P2 P -0.19491(6) -0.18070(3) 0.43672(3) 0.03704(14) Uani 1 1 d . . . . . S3 S 0.19080(6) -0.03580(3) 0.21269(3) 0.03898(14) Uani 1 1 d . . . . . P4 P 0.48531(6) 0.09928(4) 0.21525(3) 0.04029(15) Uani 1 1 d . . . . . P5 P 0.18307(6) 0.37548(3) 0.27149(3) 0.03995(15) Uani 1 1 d . . . . . O6 O 0.06663(19) 0.40077(11) 0.31419(10) 0.0557(4) Uani 1 1 d . . . . . O7 O 0.08180(18) -0.23784(10) 0.13701(9) 0.0525(4) Uani 1 1 d . . . . . O8 O 0.47716(18) 0.01384(10) 0.16475(10) 0.0533(4) Uani 1 1 d . . . . . O9 O -0.17972(19) -0.11987(10) 0.50931(8) 0.0537(4) Uani 1 1 d . . . . . C10 C -0.0398(2) -0.14269(12) 0.24470(11) 0.0332(4) Uani 1 1 d . . . . . C11 C 0.0704(2) -0.07048(12) 0.27245(11) 0.0337(4) Uani 1 1 d . . . . . C12 C 0.0106(2) -0.06391(13) 0.39594(11) 0.0386(5) Uani 1 1 d . . . . . H12 H 0.029120 -0.038412 0.446390 0.046 Uiso 1 1 calc R . . . . C13 C 0.1858(2) 0.07813(12) 0.22774(11) 0.0323(4) Uani 1 1 d . . . . . C14 C 0.3040(2) 0.22418(13) 0.23332(13) 0.0406(5) Uani 1 1 d . . . . . H14 H 0.385349 0.262134 0.229084 0.049 Uiso 1 1 calc R . . . . C15 C -0.1103(2) -0.27656(14) 0.44456(12) 0.0403(5) Uani 1 1 d . . . . . C16 C -0.1258(2) -0.17187(13) 0.29435(11) 0.0355(4) Uani 1 1 d . . . . . H16 H -0.201757 -0.217734 0.276498 0.043 Uiso 1 1 calc R . . . . C17 C 0.0935(2) -0.03200(13) 0.34743(12) 0.0396(5) Uani 1 1 d . . . . . H17 H 0.165893 0.015930 0.365267 0.048 Uiso 1 1 calc R . . . . C18 C -0.1152(2) -0.13760(13) 0.08722(11) 0.0393(5) Uani 1 1 d . . . . . C19 C 0.0582(2) 0.20096(14) 0.25297(13) 0.0418(5) Uani 1 1 d . . . . . H19 H -0.026057 0.222430 0.263562 0.050 Uiso 1 1 calc R . . . . C20 C -0.1008(2) -0.13404(12) 0.36990(11) 0.0346(4) Uani 1 1 d . . . . . C21 C -0.0911(3) -0.33650(15) 0.38319(14) 0.0515(6) Uani 1 1 d . . . . . H21 H -0.131597 -0.331377 0.335788 0.062 Uiso 1 1 calc R . . . . C22 C 0.5911(2) 0.18487(14) 0.18254(14) 0.0447(5) Uani 1 1 d . . . . . C23 C 0.3107(2) 0.13518(13) 0.22337(11) 0.0351(4) Uani 1 1 d . . . . . C24 C 0.1654(3) 0.50212(17) 0.18749(17) 0.0643(7) Uani 1 1 d . . . . . H24 H 0.157509 0.537533 0.232463 0.077 Uiso 1 1 calc R . . . . C25 C 0.1780(2) 0.41531(14) 0.18548(13) 0.0446(5) Uani 1 1 d . . . . . C26 C 0.0608(2) 0.11217(14) 0.24099(13) 0.0414(5) Uani 1 1 d . . . . . H26 H -0.023190 0.074393 0.241831 0.050 Uiso 1 1 calc R . . . . C27 C -0.2029(3) -0.29355(13) 0.14219(12) 0.0441(5) Uani 1 1 d . . . . . C28 C -0.3794(2) -0.21631(14) 0.39151(12) 0.0430(5) Uani 1 1 d . . . . . C29 C 0.1803(2) 0.25825(13) 0.24929(12) 0.0377(5) Uani 1 1 d . . . . . C30 C -0.0640(3) -0.14542(17) 0.01954(12) 0.0523(6) Uani 1 1 d . . . . . H30 H 0.003853 -0.182121 0.008969 0.063 Uiso 1 1 calc R . . . . C31 C 0.3640(3) 0.41420(14) 0.32192(13) 0.0494(6) Uani 1 1 d . . . . . C32 C 0.5635(2) 0.10342(15) 0.31060(14) 0.0473(5) Uani 1 1 d . . . . . C33 C -0.4565(3) -0.29389(19) 0.39889(19) 0.0714(8) Uani 1 1 d . . . . . H33 H -0.410187 -0.332005 0.423176 0.086 Uiso 1 1 calc R . . . . C34 C -0.0133(3) -0.40367(17) 0.39093(17) 0.0612(7) Uani 1 1 d . . . . . H34 H -0.001484 -0.443507 0.349191 0.073 Uiso 1 1 calc R . . . . C35 C -0.2157(3) -0.08198(16) 0.10244(13) 0.0522(6) Uani 1 1 d . . . . . H35 H -0.249788 -0.075972 0.148004 0.063 Uiso 1 1 calc R . . . . C36 C 0.6782(3) 0.25635(16) 0.22955(17) 0.0576(6) Uani 1 1 d . . . . . H36 H 0.683265 0.262686 0.280972 0.069 Uiso 1 1 calc R . . . . C37 C 0.7030(3) 0.08574(19) 0.32508(18) 0.0678(8) Uani 1 1 d . . . . . H37 H 0.753462 0.070819 0.285609 0.081 Uiso 1 1 calc R . . . . C38 C -0.2651(3) -0.03565(18) 0.05012(16) 0.0674(7) Uani 1 1 d . . . . . H38 H -0.333333 0.000950 0.060172 0.081 Uiso 1 1 calc R . . . . C39 C -0.0526(3) -0.28628(19) 0.51485(15) 0.0650(7) Uani 1 1 d . . . . . H39 H -0.065711 -0.247648 0.557047 0.078 Uiso 1 1 calc R . . . . C40 C -0.1679(4) -0.37154(16) 0.15790(16) 0.0650(7) Uani 1 1 d . . . . . H40 H -0.071950 -0.376619 0.173450 0.078 Uiso 1 1 calc R . . . . C41 C -0.3461(3) -0.2872(2) 0.12130(18) 0.0708(8) Uani 1 1 d . . . . . H41 H -0.371082 -0.234736 0.111365 0.085 Uiso 1 1 calc R . . . . C42 C 0.4727(3) 0.45623(19) 0.29316(17) 0.0663(7) Uani 1 1 d . . . . . H42 H 0.453470 0.468810 0.245842 0.080 Uiso 1 1 calc R . . . . C43 C 0.5836(3) 0.17743(18) 0.10658(17) 0.0659(7) Uani 1 1 d . . . . . H43 H 0.524143 0.130300 0.074662 0.079 Uiso 1 1 calc R . . . . C45 C 0.1642(3) 0.5375(2) 0.1238(2) 0.0749(9) Uani 1 1 d . . . . . H45 H 0.158509 0.596457 0.126350 0.090 Uiso 1 1 calc R . . . . C46 C 0.6107(3) 0.4805(2) 0.3327(2) 0.0806(9) Uani 1 1 d . . . . . H46 H 0.683159 0.509367 0.312080 0.097 Uiso 1 1 calc R . . . . C47 C -0.2135(4) -0.0437(2) -0.01680(16) 0.0738(9) Uani 1 1 d . . . . . H47 H -0.245990 -0.011849 -0.051748 0.089 Uiso 1 1 calc R . . . . C48 C 0.7688(4) 0.0898(2) 0.3968(2) 0.0853(10) Uani 1 1 d . . . . . H48 H 0.864105 0.079673 0.405621 0.102 Uiso 1 1 calc R . . . . C49 C -0.4500(3) -0.1618(2) 0.35412(19) 0.0753(9) Uani 1 1 d . . . . . H49 H -0.400069 -0.108720 0.349183 0.090 Uiso 1 1 calc R . . . . C50 C 0.0464(3) -0.4111(2) 0.4605(2) 0.0755(9) Uani 1 1 d . . . . . H50 H 0.101685 -0.455038 0.466008 0.091 Uiso 1 1 calc R . . . . C51 C 0.0257(4) -0.3548(2) 0.5217(2) 0.0882(10) Uani 1 1 d . . . . . H51 H 0.064027 -0.361963 0.568817 0.106 Uiso 1 1 calc R . . . . C52 C 0.4902(3) 0.1207(3) 0.36980(17) 0.0884(11) Uani 1 1 d . . . . . H52 H 0.394750 0.130589 0.361620 0.106 Uiso 1 1 calc R . . . . C53 C -0.1142(3) -0.0983(2) -0.03236(14) 0.0697(8) Uani 1 1 d . . . . . H53 H -0.080416 -0.103812 -0.077990 0.084 Uiso 1 1 calc R . . . . C54 C 0.7576(3) 0.31828(18) 0.1997(2) 0.0743(9) Uani 1 1 d . . . . . H54 H 0.815689 0.366244 0.231244 0.089 Uiso 1 1 calc R . . . . C55 C 0.6640(4) 0.2397(2) 0.0771(2) 0.0905(11) Uani 1 1 d . . . . . H55 H 0.658636 0.234081 0.025717 0.109 Uiso 1 1 calc R . . . . C56 C -0.6704(4) -0.2622(3) 0.3330(3) 0.1069(14) Uani 1 1 d . . . . . H56 H -0.768253 -0.277589 0.313565 0.128 Uiso 1 1 calc R . . . . C57 C 0.7510(4) 0.3092(2) 0.1240(3) 0.0880(11) Uani 1 1 d . . . . . H57 H 0.805915 0.350502 0.104483 0.106 Uiso 1 1 calc R . . . . C58 C -0.2775(5) -0.44279(19) 0.1503(2) 0.0926(12) Uani 1 1 d . . . . . H58 H -0.254089 -0.495550 0.160336 0.111 Uiso 1 1 calc R . . . . C59 C 0.6405(4) 0.4626(3) 0.4004(2) 0.1083(14) Uani 1 1 d . . . . . H59 H 0.733118 0.479844 0.427521 0.130 Uiso 1 1 calc R . . . . C60 C -0.6022(4) -0.3155(3) 0.3705(3) 0.1058(14) Uani 1 1 d . . . . . H60 H -0.653912 -0.367154 0.377163 0.127 Uiso 1 1 calc R . . . . C61 C -0.4531(4) -0.3579(3) 0.1149(2) 0.1018(13) Uani 1 1 d . . . . . H61 H -0.549686 -0.352582 0.101445 0.122 Uiso 1 1 calc R . . . . C62 C 0.6949(4) 0.1085(3) 0.4548(2) 0.1051(13) Uani 1 1 d . . . . . H62 H 0.739131 0.110926 0.503314 0.126 Uiso 1 1 calc R . . . . C63 C 0.1869(5) 0.3648(2) 0.11840(16) 0.0930(12) Uani 1 1 d . . . . . H63 H 0.195072 0.306040 0.115197 0.112 Uiso 1 1 calc R . . . . C64 C 0.3955(5) 0.3966(3) 0.3907(2) 0.134(2) Uani 1 1 d . . . . . H64 H 0.323134 0.369058 0.412280 0.161 Uiso 1 1 calc R . . . . C65 C 0.1715(4) 0.4855(3) 0.0580(2) 0.0904(11) Uani 1 1 d . . . . . H65 H 0.167831 0.508392 0.014807 0.108 Uiso 1 1 calc R . . . . C66 C -0.5953(4) -0.1855(3) 0.3238(2) 0.1033(13) Uani 1 1 d . . . . . H66 H -0.641675 -0.149394 0.297186 0.124 Uiso 1 1 calc R . . . . C67 C 0.5568(5) 0.1235(4) 0.4417(2) 0.131(2) Uani 1 1 d . . . . . H67 H 0.505946 0.135951 0.481465 0.158 Uiso 1 1 calc R . . . . C68 C -0.4176(5) -0.4355(3) 0.1283(2) 0.1066(13) Uani 1 1 d . . . . . H68 H -0.489705 -0.483536 0.122352 0.128 Uiso 1 1 calc R . . . . C69 C 0.5359(6) 0.4196(5) 0.4293(3) 0.184(3) Uani 1 1 d . . . . . H69 H 0.557692 0.404979 0.475699 0.221 Uiso 1 1 calc R . . . . C70 C 0.1839(6) 0.4009(3) 0.05481(19) 0.1238(18) Uani 1 1 d . . . . . H70 H 0.190546 0.365975 0.009398 0.149 Uiso 1 1 calc R . . . . O1 O 0.3748(3) -0.17447(18) 0.10962(19) 0.1089(9) Uani 1 1 d . . . . . H1A H 0.404636 -0.155712 0.155881 0.163 Uiso 1 1 d G . . . . H1B H 0.348949 -0.132920 0.089952 0.163 Uiso 1 1 d G . . . . 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 P1 0.0468(3) 0.0304(3) 0.0335(3) 0.0056(2) 0.0114(2) 0.0078(2) P2 0.0456(3) 0.0348(3) 0.0307(3) 0.0059(2) 0.0108(2) 0.0023(2) S3 0.0446(3) 0.0297(3) 0.0477(3) 0.0098(2) 0.0206(2) 0.0080(2) P4 0.0313(3) 0.0368(3) 0.0550(3) 0.0064(2) 0.0152(2) 0.0091(2) P5 0.0425(3) 0.0306(3) 0.0469(3) 0.0046(2) 0.0087(2) 0.0084(2) O6 0.0620(10) 0.0458(9) 0.0640(11) 0.0056(8) 0.0228(8) 0.0198(8) O7 0.0573(10) 0.0458(9) 0.0589(10) 0.0065(7) 0.0204(8) 0.0185(8) O8 0.0494(9) 0.0407(8) 0.0711(11) 0.0024(8) 0.0250(8) 0.0088(7) O9 0.0715(11) 0.0482(9) 0.0376(8) -0.0018(7) 0.0171(8) 0.0008(8) C10 0.0410(11) 0.0284(9) 0.0330(10) 0.0080(8) 0.0084(8) 0.0097(8) C11 0.0373(10) 0.0294(9) 0.0382(10) 0.0114(8) 0.0104(8) 0.0086(8) C12 0.0465(12) 0.0345(10) 0.0338(10) 0.0039(8) 0.0068(9) 0.0057(9) C13 0.0328(10) 0.0305(10) 0.0352(10) 0.0099(8) 0.0068(8) 0.0050(8) C14 0.0317(10) 0.0317(10) 0.0583(13) 0.0070(9) 0.0117(9) 0.0021(8) C15 0.0397(11) 0.0414(11) 0.0414(11) 0.0163(9) 0.0073(9) -0.0005(9) C16 0.0409(11) 0.0298(10) 0.0353(10) 0.0075(8) 0.0066(9) 0.0013(8) C17 0.0434(12) 0.0315(10) 0.0421(11) 0.0042(8) 0.0087(9) 0.0010(9) C18 0.0497(12) 0.0350(10) 0.0320(10) 0.0064(8) 0.0071(9) 0.0012(9) C19 0.0323(10) 0.0399(11) 0.0593(13) 0.0149(10) 0.0149(10) 0.0128(9) C20 0.0428(11) 0.0289(9) 0.0337(10) 0.0078(8) 0.0081(8) 0.0071(8) C21 0.0627(15) 0.0459(13) 0.0490(13) 0.0128(10) 0.0101(11) 0.0132(11) C22 0.0305(10) 0.0410(12) 0.0661(15) 0.0108(10) 0.0159(10) 0.0095(9) C23 0.0293(10) 0.0344(10) 0.0425(11) 0.0066(8) 0.0080(8) 0.0072(8) C24 0.0826(19) 0.0523(15) 0.0703(17) 0.0212(13) 0.0247(15) 0.0307(14) C25 0.0403(12) 0.0405(11) 0.0506(13) 0.0090(10) 0.0015(10) 0.0028(9) C26 0.0302(10) 0.0370(11) 0.0605(14) 0.0157(10) 0.0125(9) 0.0037(8) C27 0.0624(14) 0.0324(11) 0.0361(11) 0.0023(8) 0.0135(10) 0.0028(10) C28 0.0433(12) 0.0454(12) 0.0427(12) 0.0088(9) 0.0129(10) 0.0086(10) C29 0.0360(11) 0.0314(10) 0.0468(12) 0.0069(9) 0.0081(9) 0.0091(8) C30 0.0604(15) 0.0587(14) 0.0376(12) 0.0099(10) 0.0122(11) 0.0031(12) C31 0.0537(14) 0.0364(11) 0.0528(13) 0.0051(10) -0.0008(11) 0.0009(10) C32 0.0354(11) 0.0484(13) 0.0613(14) 0.0122(11) 0.0105(10) 0.0128(10) C33 0.0519(16) 0.0577(16) 0.104(2) 0.0238(16) 0.0040(15) 0.0022(13) C34 0.0647(16) 0.0478(14) 0.0808(19) 0.0224(13) 0.0256(14) 0.0165(12) C35 0.0665(16) 0.0502(13) 0.0434(12) 0.0120(10) 0.0108(11) 0.0156(12) C36 0.0383(12) 0.0497(14) 0.0839(18) 0.0143(13) 0.0048(12) 0.0063(11) C37 0.0526(15) 0.0735(18) 0.086(2) 0.0213(15) 0.0143(14) 0.0315(14) C38 0.0778(19) 0.0579(16) 0.0705(18) 0.0229(14) 0.0010(15) 0.0217(14) C39 0.0833(19) 0.0703(17) 0.0450(14) 0.0221(12) 0.0045(13) 0.0155(15) C40 0.086(2) 0.0415(13) 0.0730(18) 0.0162(12) 0.0235(15) 0.0116(13) C41 0.0582(17) 0.0638(17) 0.089(2) 0.0264(15) 0.0042(15) -0.0058(13) C42 0.0556(16) 0.0701(18) 0.0670(17) 0.0167(14) -0.0018(13) -0.0068(13) C43 0.0746(19) 0.0556(15) 0.0709(18) 0.0127(13) 0.0269(15) 0.0063(14) C45 0.0728(19) 0.0706(19) 0.099(2) 0.0456(18) 0.0222(17) 0.0271(15) C46 0.0573(17) 0.078(2) 0.097(2) 0.0167(18) -0.0048(16) -0.0075(15) C47 0.084(2) 0.0760(19) 0.0615(18) 0.0375(15) -0.0110(15) 0.0021(17) C48 0.0647(19) 0.089(2) 0.106(3) 0.023(2) -0.0082(19) 0.0414(17) C49 0.0573(17) 0.080(2) 0.100(2) 0.0451(18) 0.0118(16) 0.0165(15) C50 0.0675(19) 0.0715(19) 0.102(3) 0.0423(19) 0.0157(17) 0.0265(15) C51 0.101(3) 0.097(2) 0.076(2) 0.045(2) -0.0087(19) 0.032(2) C52 0.0580(17) 0.152(3) 0.0583(17) 0.0079(19) 0.0067(14) 0.050(2) C53 0.078(2) 0.094(2) 0.0379(13) 0.0271(14) 0.0071(13) -0.0022(17) C54 0.0471(15) 0.0471(15) 0.127(3) 0.0228(17) 0.0062(17) 0.0007(12) C55 0.115(3) 0.081(2) 0.093(2) 0.037(2) 0.049(2) 0.016(2) C56 0.0492(19) 0.113(3) 0.148(4) 0.019(3) -0.011(2) 0.009(2) C57 0.080(2) 0.063(2) 0.137(3) 0.043(2) 0.048(2) 0.0074(17) C58 0.142(4) 0.0391(15) 0.102(3) 0.0237(16) 0.038(3) 0.0023(19) C59 0.080(2) 0.108(3) 0.120(3) 0.044(2) -0.042(2) -0.023(2) C60 0.0540(19) 0.081(2) 0.172(4) 0.024(3) -0.002(2) -0.0103(17) C61 0.075(2) 0.089(3) 0.135(3) 0.041(2) 0.000(2) -0.0252(19) C62 0.092(3) 0.152(4) 0.074(2) 0.021(2) -0.012(2) 0.056(3) C63 0.174(4) 0.0492(16) 0.0504(16) 0.0027(13) 0.016(2) 0.008(2) C64 0.110(3) 0.185(5) 0.086(3) 0.077(3) -0.037(2) -0.072(3) C65 0.109(3) 0.102(3) 0.068(2) 0.043(2) 0.0062(19) 0.014(2) C66 0.063(2) 0.128(3) 0.133(3) 0.060(3) 0.001(2) 0.034(2) C67 0.100(3) 0.245(6) 0.057(2) 0.011(3) 0.0095(19) 0.085(4) C68 0.111(3) 0.077(2) 0.120(3) 0.025(2) 0.016(3) -0.035(2) C69 0.144(4) 0.253(7) 0.127(4) 0.122(5) -0.080(3) -0.094(5) C70 0.234(6) 0.084(3) 0.0487(18) 0.0095(17) 0.017(3) 0.015(3) O1 0.105(2) 0.0910(18) 0.133(2) -0.0065(16) 0.0553(19) 0.0284(15) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 O7 P1 C10 111.20(9) . . ? O7 P1 C18 114.21(10) . . ? O7 P1 C27 111.48(11) . . ? C18 P1 C10 107.93(9) . . ? C18 P1 C27 106.26(10) . . ? C27 P1 C10 105.25(9) . . ? O9 P2 C15 112.09(10) . . ? O9 P2 C20 112.69(10) . . ? O9 P2 C28 114.25(10) . . ? C20 P2 C15 102.85(10) . . ? C28 P2 C15 108.37(10) . . ? C28 P2 C20 105.79(10) . . ? C13 S3 C11 101.78(9) . . ? O8 P4 C22 110.87(11) . . ? O8 P4 C23 114.39(9) . . ? O8 P4 C32 114.71(11) . . ? C22 P4 C23 105.35(10) . . ? C32 P4 C22 107.04(11) . . ? C32 P4 C23 103.71(10) . . ? O6 P5 C25 113.02(11) . . ? O6 P5 C29 113.02(10) . . ? O6 P5 C31 113.88(12) . . ? C25 P5 C29 107.84(10) . . ? C25 P5 C31 105.88(11) . . ? C31 P5 C29 102.38(10) . . ? C11 C10 P1 121.13(15) . . ? C16 C10 P1 120.30(15) . . ? C16 C10 C11 118.11(18) . . ? C10 C11 S3 119.62(15) . . ? C17 C11 S3 120.00(15) . . ? C17 C11 C10 120.09(18) . . ? C17 C12 C20 120.42(19) . . ? C23 C13 S3 119.04(15) . . ? C26 C13 S3 121.83(15) . . ? C26 C13 C23 119.08(18) . . ? C29 C14 C23 122.34(19) . . ? C21 C15 P2 122.93(16) . . ? C39 C15 P2 118.20(19) . . ? C39 C15 C21 118.7(2) . . ? C20 C16 C10 121.64(19) . . ? C12 C17 C11 120.76(19) . . ? C30 C18 P1 118.09(18) . . ? C30 C18 C35 119.5(2) . . ? C35 C18 P1 122.34(16) . . ? C26 C19 C29 120.33(19) . . ? C12 C20 P2 118.83(15) . . ? C16 C20 P2 121.90(15) . . ? C16 C20 C12 118.92(18) . . ? C34 C21 C15 121.3(2) . . ? C36 C22 P4 123.7(2) . . ? C43 C22 P4 117.24(19) . . ? C43 C22 C36 119.1(2) . . ? C13 C23 P4 122.83(15) . . ? C14 C23 P4 118.46(15) . . ? C14 C23 C13 118.38(18) . . ? C25 C24 C45 121.3(3) . . ? C24 C25 P5 118.32(19) . . ? C63 C25 P5 123.8(2) . . ? C63 C25 C24 117.9(2) . . ? C19 C26 C13 121.39(19) . . ? C40 C27 P1 117.4(2) . . ? C41 C27 P1 123.67(19) . . ? C41 C27 C40 118.9(2) . . ? C33 C28 P2 121.45(19) . . ? C33 C28 C49 118.6(2) . . ? C49 C28 P2 119.69(19) . . ? C14 C29 P5 120.54(15) . . ? C19 C29 P5 120.91(16) . . ? C19 C29 C14 118.40(18) . . ? C18 C30 C53 119.7(3) . . ? C42 C31 P5 123.8(2) . . ? C64 C31 P5 118.2(2) . . ? C64 C31 C42 117.9(3) . . ? C37 C32 P4 118.9(2) . . ? C52 C32 P4 123.48(19) . . ? C52 C32 C37 117.6(3) . . ? C28 C33 C60 120.4(3) . . ? C50 C34 C21 119.3(3) . . ? C38 C35 C18 120.2(2) . . ? C54 C36 C22 119.9(3) . . ? C48 C37 C32 121.2(3) . . ? C47 C38 C35 119.9(3) . . ? C15 C39 C51 119.2(3) . . ? C27 C40 C58 119.6(3) . . ? C27 C41 C61 120.7(3) . . ? C31 C42 C46 121.4(3) . . ? C22 C43 C55 120.7(3) . . ? C65 C45 C24 119.4(3) . . ? C59 C46 C42 120.1(3) . . ? C53 C47 C38 120.3(2) . . ? C62 C48 C37 120.1(3) . . ? C28 C49 C66 120.3(3) . . ? C51 C50 C34 120.5(3) . . ? C50 C51 C39 120.9(3) . . ? C32 C52 C67 120.7(3) . . ? C47 C53 C30 120.3(3) . . ? C57 C54 C36 120.4(3) . . ? C57 C55 C43 119.7(3) . . ? C60 C56 C66 119.9(3) . . ? C55 C57 C54 120.3(3) . . ? C68 C58 C40 120.4(3) . . ? C46 C59 C69 119.6(3) . . ? C56 C60 C33 120.6(3) . . ? C68 C61 C41 120.2(4) . . ? C67 C62 C48 119.7(3) . . ? C25 C63 C70 120.2(3) . . ? C31 C64 C69 120.1(4) . . ? C70 C65 C45 120.2(3) . . ? C56 C66 C49 120.0(3) . . ? C62 C67 C52 120.6(4) . . ? C58 C68 C61 120.1(3) . . ? C59 C69 C64 120.8(4) . . ? C65 C70 C63 121.0(3) . . ? 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 P1 O7 1.4842(18) . ? P1 C10 1.815(2) . ? P1 C18 1.795(2) . ? P1 C27 1.811(2) . ? P2 O9 1.4791(16) . ? P2 C15 1.814(2) . ? P2 C20 1.810(2) . ? P2 C28 1.801(2) . ? S3 C11 1.780(2) . ? S3 C13 1.773(2) . ? P4 O8 1.4802(17) . ? P4 C22 1.809(2) . ? P4 C23 1.820(2) . ? P4 C32 1.805(3) . ? P5 O6 1.4821(18) . ? P5 C25 1.804(2) . ? P5 C29 1.814(2) . ? P5 C31 1.808(3) . ? C10 C11 1.410(3) . ? C10 C16 1.395(3) . ? C11 C17 1.385(3) . ? C12 C17 1.378(3) . ? C12 C20 1.391(3) . ? C13 C23 1.405(3) . ? C13 C26 1.385(3) . ? C14 C23 1.391(3) . ? C14 C29 1.385(3) . ? C15 C21 1.385(3) . ? C15 C39 1.383(3) . ? C16 C20 1.391(3) . ? C18 C30 1.385(3) . ? C18 C35 1.390(3) . ? C19 C26 1.380(3) . ? C19 C29 1.385(3) . ? C21 C34 1.379(3) . ? C22 C36 1.388(3) . ? C22 C43 1.377(4) . ? C24 C25 1.382(3) . ? C24 C45 1.386(4) . ? C25 C63 1.364(4) . ? C27 C40 1.381(3) . ? C27 C41 1.376(4) . ? C28 C33 1.377(4) . ? C28 C49 1.378(4) . ? C30 C53 1.385(4) . ? C31 C42 1.363(4) . ? C31 C64 1.351(4) . ? C32 C37 1.380(3) . ? C32 C52 1.369(4) . ? C33 C60 1.381(4) . ? C34 C50 1.365(4) . ? C35 C38 1.380(3) . ? C36 C54 1.386(4) . ? C37 C48 1.375(4) . ? C38 C47 1.373(4) . ? C39 C51 1.397(4) . ? C40 C58 1.398(5) . ? C41 C61 1.380(4) . ? C42 C46 1.378(4) . ? C43 C55 1.391(4) . ? C45 C65 1.352(5) . ? C46 C59 1.332(5) . ? C47 C53 1.372(5) . ? C48 C62 1.357(5) . ? C49 C66 1.387(5) . ? C50 C51 1.355(5) . ? C52 C67 1.384(5) . ? C54 C57 1.370(5) . ? C55 C57 1.368(5) . ? C56 C60 1.351(5) . ? C56 C66 1.367(5) . ? C58 C68 1.356(6) . ? C59 C69 1.342(6) . ? C61 C68 1.363(6) . ? C62 C67 1.351(5) . ? C63 C70 1.390(5) . ? C64 C69 1.390(6) . ? C65 C70 1.344(5) . ?