#------------------------------------------------------------------------------ #$Date: 2019-12-14 04:48:16 +0200 (Sat, 14 Dec 2019) $ #$Revision: 245179 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/56/7125653.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_7125653 loop_ _publ_author_name 'Fink, Daniel' 'Orth, Nicole' 'Linseis, Michael' 'Ivanovi\'c-Burmazovi\'c, Ivana' 'Winter, Rainer' _publ_section_title ; Ring Size Matters: Supramolecular Isomerism in Self-Assembled Redox-Active Tetra- and Hexaruthenium Macrocycles ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/C9CC09307A _journal_year 2020 _chemical_formula_moiety 'C104 H184 O14 P8 Ru4 S2, 5(C6 H6)' _chemical_formula_sum 'C134 H214 O14 P8 Ru4 S2' _chemical_formula_weight 2765.20 _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 geom _audit_creation_date 2018-04-20 _audit_creation_method ; Olex2 1.2-alpha (compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488) ; _audit_update_record ; 2019-10-27 deposited with the CCDC. 2019-12-13 downloaded from the CCDC. ; _cell_angle_alpha 102.732(6) _cell_angle_beta 98.198(6) _cell_angle_gamma 101.465(6) _cell_formula_units_Z 1 _cell_length_a 11.9389(9) _cell_length_b 17.3830(15) _cell_length_c 18.6230(15) _cell_measurement_reflns_used 22812 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.05 _cell_measurement_theta_min 1.80 _cell_volume 3623.7(5) _computing_cell_refinement 'STOE X-AREA' _computing_data_collection 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015a)' _diffrn_ambient_temperature 100.15 _diffrn_detector_area_resol_mean 6.67 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1519 _diffrn_reflns_av_unetI/netI 0.1730 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 52347 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.858 _diffrn_reflns_theta_min 1.774 _exptl_absorpt_coefficient_mu 0.580 _exptl_absorpt_correction_T_max 0.9553 _exptl_absorpt_correction_T_min 0.8579 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details 'STOE X-RED32' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.267 _exptl_crystal_description block _exptl_crystal_F_000 1458 _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _refine_diff_density_max 0.848 _refine_diff_density_min -0.623 _refine_diff_density_rms 0.095 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.866 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 754 _refine_ls_number_reflns 15420 _refine_ls_number_restraints 8 _refine_ls_restrained_S_all 0.868 _refine_ls_R_factor_all 0.1321 _refine_ls_R_factor_gt 0.0595 _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^)+(0.0094P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0787 _refine_ls_wR_factor_ref 0.0926 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8546 _reflns_number_total 15420 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc09307a2.cif _cod_data_source_block pdf33 _cod_database_code 7125653 _shelx_shelxl_version_number 2017/1 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H,H) groups 2. Restrained distances C57-C58 = C58-C53 = C53-C54 = C54-C55 = C55-C56 = C56-C57 1.39 with sigma of 0.005 C59-C60 = C60-C61 1.39 with sigma of 0.005 3.a Ternary CH refined with riding coordinates: C17(H17), C20(H20), C23(H23), C29(H29), C26(H26), C32(H32), C41(H41), C35(H35), C38(H38), C44(H44), C47(H47), C50(H50) 3.b Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C4(H4), C11(H11), C12(H12), C5(H5), C6(H6), C8(H8), C56(H56), C57(H57), C58(H58), C53(H53), C54(H54), C55(H55), C61(H61), C60(H60), C59(H59), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C67(H67) 3.c Idealised Me refined as rotating group: C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B, H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C30(H30A,H30B,H30C), C31(H31A, H31B,H31C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C37(H37A,H37B, H37C), C36(H36A,H36B,H36C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C45(H45A, H45B,H45C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C52(H52A,H52B,H52C), C51(H51A,H51B,H51C) ; _shelx_res_file ; TITL PDF33 pdf33.res created by SHELXL-2017/1 at 13:44:54 on 20-Apr-2018 CELL 0.71073 11.9389 17.383 18.623 102.732 98.198 101.465 ZERR 1 0.0009 0.0015 0.0015 0.006 0.006 0.006 LATT 1 SFAC C H O P Ru S UNIT 134 214 14 8 4 2 DFIX 1.39 0.005 C57 C58 C58 C53 C53 C54 C54 C55 C55 C56 C56 C57 DFIX 1.39 0.005 C59 C60 C60 C61 L.S. 20 PLAN 30 TEMP -173 BOND CONF fmap 2 acta REM REM REM WGHT 0.009400 FVAR 0.21519 RU1 5 0.725652 0.795903 0.850433 11.00000 0.02493 0.01993 = 0.01414 0.00384 0.00270 0.00411 RU2 5 0.432086 0.229609 0.720646 11.00000 0.01850 0.01967 = 0.01604 0.00571 0.00339 0.00371 O1 3 0.678389 0.662260 0.814202 11.00000 0.03412 0.02473 = 0.01801 0.00432 0.00399 0.00825 O2 3 0.722430 0.718839 0.935522 11.00000 0.03137 0.02261 = 0.02163 0.00325 0.00278 0.00543 O3 3 0.620033 0.510533 0.838351 11.00000 0.02717 0.01775 = 0.01460 0.00283 0.00345 0.00227 O4 3 0.519675 0.359645 0.744224 11.00000 0.02471 0.02590 = 0.01914 0.00649 0.00426 0.01010 O5 3 0.511752 0.304888 0.840031 11.00000 0.02711 0.01867 = 0.02117 0.00692 0.00310 0.00186 O6 3 0.779307 0.971666 0.926157 11.00000 0.03781 0.02912 = 0.02612 0.00346 0.00591 0.00166 O7 3 0.334491 0.064012 0.734926 11.00000 0.03158 0.03404 = 0.03094 0.01454 0.00636 0.00413 P1 4 0.522060 0.791784 0.847636 11.00000 0.02732 0.02431 = 0.02393 0.00713 0.00657 0.00574 P2 4 0.927520 0.791558 0.853292 11.00000 0.02628 0.03061 = 0.02275 0.00240 0.00334 0.00476 P3 4 0.253458 0.271358 0.734184 11.00000 0.02357 0.03312 = 0.02229 0.00509 0.00396 0.00734 P4 4 0.614485 0.197681 0.707451 11.00000 0.02184 0.01968 = 0.01854 0.00291 0.00185 0.00326 S1 6 0.672889 0.834254 0.574600 11.00000 0.02714 0.02178 = 0.01685 0.00530 0.00191 0.00144 C1 1 0.716716 0.823467 0.750605 11.00000 0.02700 0.03031 = 0.01492 0.00282 0.00253 0.00446 AFIX 43 H1 2 0.679610 0.778738 0.708914 11.00000 -1.20000 AFIX 0 C2 1 0.753585 0.893585 0.731889 11.00000 0.02474 0.02092 = 0.02094 0.00642 0.00451 0.00733 AFIX 43 H2 2 0.783708 0.940916 0.772176 11.00000 -1.20000 AFIX 0 C3 1 0.752101 0.904369 0.656716 11.00000 0.01786 0.02641 = 0.01596 0.00199 -0.00018 0.00605 C4 1 0.812696 0.972318 0.640136 11.00000 0.02384 0.02176 = 0.01843 0.00138 -0.00109 0.00260 AFIX 43 H4 2 0.860936 1.018037 0.677193 11.00000 -1.20000 AFIX 0 C11 1 0.652918 0.554722 0.963400 11.00000 0.05725 0.02558 = 0.01981 0.00394 0.00698 0.00541 AFIX 43 H11 2 0.675131 0.589567 1.012728 11.00000 -1.20000 AFIX 0 C10 1 0.656920 0.576756 0.897599 11.00000 0.03055 0.01937 = 0.02207 0.00108 0.00352 0.00587 C9 1 0.688810 0.655716 0.881369 11.00000 0.01590 0.03392 = 0.02032 0.00286 0.00134 0.00742 C12 1 0.609158 0.469829 0.943233 11.00000 0.05086 0.02492 = 0.02004 0.01065 0.00643 0.00642 AFIX 43 H12 2 0.594972 0.436272 0.976493 11.00000 -1.20000 AFIX 0 C13 1 0.591325 0.445390 0.868075 11.00000 0.02297 0.01946 = 0.02384 0.00624 0.00476 0.00378 C14 1 0.539202 0.366135 0.815076 11.00000 0.01328 0.02854 = 0.02644 0.00543 0.00405 0.00851 C15 1 0.760283 0.902963 0.896303 11.00000 0.02990 0.02723 = 0.01489 0.01024 0.00720 0.00342 C17 1 0.473203 0.877824 0.816382 11.00000 0.04202 0.05537 = 0.04258 0.02009 0.00920 0.02483 AFIX 13 H17 2 0.544907 0.923222 0.830993 11.00000 -1.20000 AFIX 0 C18 1 0.441431 0.860887 0.730988 11.00000 0.03737 0.05289 = 0.04386 0.02783 0.00349 0.00706 AFIX 137 H18A 2 0.372042 0.815893 0.711854 11.00000 -1.20000 H18B 2 0.506511 0.846352 0.708885 11.00000 -1.20000 H18C 2 0.425371 0.909559 0.717481 11.00000 -1.20000 AFIX 0 C19 1 0.386514 0.912650 0.851749 11.00000 0.09890 0.07535 = 0.08901 0.04186 0.03420 0.04948 AFIX 137 H19A 2 0.375810 0.959927 0.833461 11.00000 -1.20000 H19B 2 0.413382 0.929458 0.906333 11.00000 -1.20000 H19C 2 0.312267 0.871900 0.839151 11.00000 -1.20000 AFIX 0 C20 1 0.422054 0.694440 0.790800 11.00000 0.02818 0.03262 = 0.03095 0.00677 0.00661 0.00130 AFIX 13 H20 2 0.439421 0.653159 0.817834 11.00000 -1.20000 AFIX 0 C21 1 0.444667 0.663507 0.711678 11.00000 0.03600 0.03817 = 0.03005 0.00057 -0.00139 -0.00406 AFIX 137 H21A 2 0.526893 0.662252 0.714789 11.00000 -1.20000 H21B 2 0.425873 0.699863 0.680792 11.00000 -1.20000 H21C 2 0.395675 0.608652 0.688928 11.00000 -1.20000 AFIX 0 C22 1 0.292774 0.689833 0.788591 11.00000 0.02528 0.04823 = 0.05276 0.00741 0.00099 -0.00215 AFIX 137 H22A 2 0.247923 0.634129 0.764350 11.00000 -1.20000 H22B 2 0.267950 0.726695 0.760102 11.00000 -1.20000 H22C 2 0.279299 0.705713 0.839902 11.00000 -1.20000 AFIX 0 C23 1 0.480232 0.801755 0.941624 11.00000 0.03819 0.02917 = 0.03282 0.00945 0.02099 0.01008 AFIX 13 H23 2 0.403321 0.816693 0.937188 11.00000 -1.20000 AFIX 0 C24 1 0.464287 0.724021 0.968656 11.00000 0.05225 0.05054 = 0.02899 0.02123 0.01931 0.01321 AFIX 137 H24A 2 0.535012 0.703557 0.967855 11.00000 -1.20000 H24B 2 0.397922 0.682953 0.935468 11.00000 -1.20000 H24C 2 0.449712 0.735757 1.019961 11.00000 -1.20000 AFIX 0 C25 1 0.566392 0.871197 0.999348 11.00000 0.05842 0.05639 = 0.02884 0.00376 0.02135 0.00918 AFIX 137 H25A 2 0.574027 0.920583 0.981434 11.00000 -1.20000 H25B 2 0.642394 0.857776 1.007162 11.00000 -1.20000 H25C 2 0.538554 0.880203 1.046831 11.00000 -1.20000 AFIX 0 C29 1 0.993399 0.780447 0.947109 11.00000 0.02724 0.04671 = 0.02694 0.00708 -0.00035 0.00960 AFIX 13 H29 2 0.949961 0.726633 0.951226 11.00000 -1.20000 AFIX 0 C30 1 0.973831 0.843339 1.011840 11.00000 0.02778 0.05823 = 0.02819 0.00824 -0.00540 0.00706 AFIX 137 H30A 2 0.996368 0.829225 1.059079 11.00000 -1.20000 H30B 2 0.891295 0.844455 1.004584 11.00000 -1.20000 H30C 2 1.021195 0.896943 1.013650 11.00000 -1.20000 AFIX 0 C31 1 1.121054 0.778031 0.957592 11.00000 0.03039 0.09139 = 0.05212 0.01621 -0.00167 0.01977 AFIX 137 H31A 2 1.169294 0.832712 0.964282 11.00000 -1.20000 H31B 2 1.134289 0.741286 0.913224 11.00000 -1.20000 H31C 2 1.141948 0.758537 1.002034 11.00000 -1.20000 AFIX 0 C26 1 1.034589 0.876301 0.836773 11.00000 0.04269 0.04856 = 0.05022 0.00413 0.02585 0.00116 AFIX 13 H26 2 1.110104 0.867584 0.860403 11.00000 -1.20000 AFIX 0 C27 1 1.037106 0.959126 0.881866 11.00000 0.04023 0.03775 = 0.04878 0.01126 0.00724 -0.00274 AFIX 137 H27A 2 1.106805 0.997618 0.878152 11.00000 -1.20000 H27B 2 1.038773 0.958503 0.934497 11.00000 -1.20000 H27C 2 0.967395 0.975712 0.862597 11.00000 -1.20000 AFIX 0 C28 1 1.052047 0.874254 0.760481 11.00000 0.09158 0.06972 = 0.04737 0.01394 0.02389 -0.01084 AFIX 137 H28A 2 0.978003 0.871896 0.728625 11.00000 -1.20000 H28B 2 1.080359 0.826193 0.740660 11.00000 -1.20000 H28C 2 1.109506 0.923298 0.760910 11.00000 -1.20000 AFIX 0 C32 1 0.950871 0.702140 0.786345 11.00000 0.03645 0.04261 = 0.03263 0.00327 0.01049 0.01863 AFIX 13 H32 2 1.033922 0.716797 0.780719 11.00000 -1.20000 AFIX 0 C33 1 0.877004 0.686420 0.708184 11.00000 0.04268 0.05014 = 0.02876 -0.00680 0.01308 0.01318 AFIX 137 H33A 2 0.902872 0.646495 0.672437 11.00000 -1.20000 H33B 2 0.885797 0.737269 0.692654 11.00000 -1.20000 H33C 2 0.794959 0.665413 0.709321 11.00000 -1.20000 AFIX 0 C34 1 0.935551 0.623234 0.810966 11.00000 0.06275 0.05027 = 0.04705 0.00744 0.01695 0.03089 AFIX 137 H34A 2 0.852985 0.602188 0.810747 11.00000 -1.20000 H34B 2 0.980986 0.633605 0.861735 11.00000 -1.20000 H34C 2 0.962840 0.583211 0.776234 11.00000 -1.20000 AFIX 0 C5 1 0.377115 0.194157 0.608135 11.00000 0.01513 0.02413 = 0.02076 0.00899 0.00260 0.00529 AFIX 43 H5 2 0.404064 0.234088 0.582973 11.00000 -1.20000 AFIX 0 C6 1 0.310679 0.125773 0.563115 11.00000 0.01835 0.02741 = 0.01904 0.00863 0.00342 0.00396 AFIX 43 H6 2 0.281132 0.085645 0.587409 11.00000 -1.20000 AFIX 0 C7 1 0.276090 0.102855 0.481812 11.00000 0.01885 0.02585 = 0.02147 0.01049 0.00460 0.00541 C8 1 0.204291 0.032964 0.437830 11.00000 0.02446 0.02349 = 0.02148 0.00800 0.00183 0.00625 AFIX 43 H8 2 0.168055 -0.009309 0.457668 11.00000 -1.20000 AFIX 0 C16 1 0.372224 0.129439 0.727219 11.00000 0.01850 0.03314 = 0.01234 0.00432 0.00229 0.00587 C41 1 0.245959 0.370723 0.715502 11.00000 0.02906 0.05047 = 0.04257 0.01445 0.00679 0.02017 AFIX 13 H41 2 0.161996 0.372341 0.710469 11.00000 -1.20000 AFIX 0 C42 1 0.312523 0.447682 0.774204 11.00000 0.04873 0.03914 = 0.07447 0.01454 0.01310 0.02164 AFIX 137 H42A 2 0.396381 0.451531 0.778857 11.00000 -1.20000 H42B 2 0.290205 0.446282 0.822626 11.00000 -1.20000 H42C 2 0.293985 0.494948 0.759050 11.00000 -1.20000 AFIX 0 C43 1 0.276948 0.373589 0.638624 11.00000 0.06047 0.07413 = 0.05905 0.04751 0.02278 0.04146 AFIX 137 H43A 2 0.228005 0.326319 0.600140 11.00000 -1.20000 H43B 2 0.359139 0.372845 0.640333 11.00000 -1.20000 H43C 2 0.263451 0.423432 0.626402 11.00000 -1.20000 AFIX 0 C35 1 0.124372 0.202933 0.667232 11.00000 0.01638 0.06053 = 0.03167 0.00230 -0.00166 0.00568 AFIX 13 H35 2 0.150622 0.188210 0.618439 11.00000 -1.20000 AFIX 0 C37 1 0.015613 0.236869 0.649702 11.00000 0.02401 0.08067 = 0.03605 0.00843 0.00721 0.01524 AFIX 137 H37A 2 0.036826 0.283712 0.628984 11.00000 -1.20000 H37B 2 -0.013232 0.253711 0.695974 11.00000 -1.20000 H37C 2 -0.045424 0.194612 0.613078 11.00000 -1.20000 AFIX 0 C36 1 0.086004 0.122188 0.688455 11.00000 0.02612 0.05109 = 0.05454 -0.00914 0.00647 -0.00503 AFIX 137 H36A 2 0.042439 0.130516 0.729169 11.00000 -1.20000 H36B 2 0.154948 0.103299 0.705042 11.00000 -1.20000 H36C 2 0.036234 0.081422 0.644645 11.00000 -1.20000 AFIX 0 C38 1 0.230434 0.285967 0.832785 11.00000 0.02252 0.04506 = 0.02814 -0.00134 0.00915 0.00836 AFIX 13 H38 2 0.294288 0.333384 0.862940 11.00000 -1.20000 AFIX 0 C39 1 0.117252 0.309608 0.846555 11.00000 0.03663 0.07917 = 0.03613 0.00298 0.01410 0.01550 AFIX 137 H39A 2 0.051122 0.263131 0.822917 11.00000 -1.20000 H39B 2 0.108674 0.355135 0.824907 11.00000 -1.20000 H39C 2 0.119354 0.325724 0.900673 11.00000 -1.20000 AFIX 0 C40 1 0.247654 0.215192 0.865393 11.00000 0.04567 0.06077 = 0.03030 0.01264 0.01779 0.00236 AFIX 137 H40A 2 0.326220 0.207305 0.863106 11.00000 -1.20000 H40B 2 0.189927 0.165730 0.836301 11.00000 -1.20000 H40C 2 0.237895 0.226995 0.917759 11.00000 -1.20000 AFIX 0 C44 1 0.691923 0.190342 0.799068 11.00000 0.02239 0.03786 = 0.01576 0.00337 0.00248 0.00858 AFIX 13 H44 2 0.718738 0.247285 0.831307 11.00000 -1.20000 AFIX 0 C45 1 0.614200 0.143398 0.841475 11.00000 0.03834 0.04217 = 0.02280 0.01568 0.00432 0.01504 AFIX 137 H45A 2 0.659344 0.145732 0.890502 11.00000 -1.20000 H45B 2 0.585518 0.086649 0.812455 11.00000 -1.20000 H45C 2 0.547974 0.167755 0.848620 11.00000 -1.20000 AFIX 0 C46 1 0.802988 0.157956 0.795228 11.00000 0.03033 0.05862 = 0.02385 0.00978 -0.00423 0.01659 AFIX 137 H46A 2 0.847249 0.182422 0.762087 11.00000 -1.20000 H46B 2 0.781041 0.098783 0.775520 11.00000 -1.20000 H46C 2 0.851134 0.172116 0.845641 11.00000 -1.20000 AFIX 0 C47 1 0.624194 0.104879 0.639176 11.00000 0.02772 0.02783 = 0.01698 0.00109 -0.00052 0.01463 AFIX 13 H47 2 0.705015 0.097936 0.652801 11.00000 -1.20000 AFIX 0 C48 1 0.541604 0.027723 0.644438 11.00000 0.03963 0.02655 = 0.02692 0.00500 0.00273 0.01250 AFIX 137 H48A 2 0.555936 -0.019645 0.610715 11.00000 -1.20000 H48B 2 0.460771 0.030818 0.629838 11.00000 -1.20000 H48C 2 0.555197 0.022570 0.696133 11.00000 -1.20000 AFIX 0 C49 1 0.607566 0.108744 0.556943 11.00000 0.03663 0.04279 = 0.01847 0.00458 0.00504 0.01837 AFIX 137 H49A 2 0.613980 0.057364 0.525200 11.00000 -1.20000 H49B 2 0.667691 0.153371 0.551570 11.00000 -1.20000 H49C 2 0.530404 0.117968 0.541523 11.00000 -1.20000 AFIX 0 C50 1 0.723481 0.275289 0.682070 11.00000 0.02657 0.02900 = 0.03634 0.00561 0.01004 0.00713 AFIX 13 H50 2 0.778747 0.245763 0.659107 11.00000 -1.20000 AFIX 0 C52 1 0.797862 0.344648 0.746834 11.00000 0.02592 0.03079 = 0.04541 0.00356 0.00721 0.00007 AFIX 137 H52A 2 0.843423 0.322620 0.781889 11.00000 -1.20000 H52B 2 0.747219 0.373958 0.773043 11.00000 -1.20000 H52C 2 0.850749 0.381944 0.727196 11.00000 -1.20000 AFIX 0 C51 1 0.667428 0.310950 0.621339 11.00000 0.02853 0.03019 = 0.04087 0.01837 0.01776 0.00394 AFIX 137 H51A 2 0.621604 0.347585 0.643358 11.00000 -1.20000 H51B 2 0.616380 0.266782 0.580678 11.00000 -1.20000 H51C 2 0.728614 0.341186 0.601314 11.00000 -1.20000 AFIX 0 C56 1 1.015867 0.183986 0.444476 11.00000 0.04818 0.12622 = 0.04141 0.03273 0.01533 0.03810 AFIX 43 H56 2 1.092799 0.176160 0.448279 11.00000 -1.20000 AFIX 0 C57 1 0.997682 0.261073 0.456323 11.00000 0.09370 0.08845 = 0.03486 0.01661 0.00219 -0.03684 AFIX 43 H57 2 1.062033 0.306739 0.467616 11.00000 -1.20000 AFIX 0 C58 1 0.885466 0.271988 0.451761 11.00000 0.13307 0.04100 = 0.03916 0.00995 0.01173 0.02683 AFIX 43 H58 2 0.872053 0.325025 0.460010 11.00000 -1.20000 AFIX 0 C53 1 0.793560 0.204973 0.435114 11.00000 0.05823 0.13120 = 0.03762 0.03099 0.01418 0.05983 AFIX 43 H53 2 0.716466 0.212406 0.431947 11.00000 -1.20000 AFIX 0 C54 1 0.810365 0.127641 0.422961 11.00000 0.07426 0.07505 = 0.04524 0.01480 0.01839 -0.01482 AFIX 43 H54 2 0.746288 0.081836 0.411980 11.00000 -1.20000 AFIX 0 C55 1 0.922193 0.118479 0.427132 11.00000 0.10155 0.06376 = 0.04390 0.02055 0.03195 0.04033 AFIX 43 H55 2 0.935243 0.065321 0.417761 11.00000 -1.20000 AFIX 0 C61 1 0.954653 0.498243 0.429789 11.00000 0.26707 0.07971 = 0.06248 0.00716 -0.02494 0.07540 AFIX 43 H61 2 0.920445 0.497306 0.380217 11.00000 -1.20000 AFIX 0 C60 1 0.883295 0.495782 0.482277 11.00000 0.21992 0.06355 = 0.12572 0.00293 -0.03131 0.06332 AFIX 43 H60 2 0.802427 0.492518 0.468461 11.00000 -1.20000 AFIX 0 C59 1 0.931736 0.498158 0.555176 11.00000 0.24816 0.06300 = 0.09817 0.00860 0.00567 0.07479 AFIX 43 H59 2 0.885830 0.497254 0.592799 11.00000 -1.20000 AFIX 0 C62 1 -0.014412 0.481509 0.922932 11.00000 0.11618 0.07258 = 0.05712 0.00152 -0.02443 0.03767 AFIX 43 H62 2 -0.025770 0.469312 0.869734 11.00000 -1.20000 AFIX 0 C63 1 -0.093296 0.443000 0.956834 11.00000 0.11862 0.07836 = 0.04853 -0.00629 -0.02759 0.01273 AFIX 43 H63 2 -0.158066 0.401996 0.926631 11.00000 -1.20000 AFIX 0 C64 1 -0.082439 0.461453 1.033503 11.00000 0.11501 0.10491 = 0.05508 -0.00212 -0.01958 0.01895 AFIX 43 H64 2 -0.140471 0.435445 1.056034 11.00000 -1.20000 AFIX 0 C65 1 0.512492 0.572946 0.482226 11.00000 0.12719 0.06304 = 0.06119 0.02907 0.02326 0.04316 AFIX 43 H65 2 0.519369 0.623533 0.469644 11.00000 -1.20000 AFIX 0 C66 1 0.567145 0.570321 0.550533 11.00000 0.09249 0.07610 = 0.07183 0.01889 0.02196 0.01870 AFIX 43 H66 2 0.614627 0.618146 0.585307 11.00000 -1.20000 AFIX 0 C67 1 0.551686 0.495918 0.568059 11.00000 0.12919 0.09891 = 0.04276 0.02889 0.00559 0.05109 AFIX 43 H67 2 0.586771 0.493192 0.616248 11.00000 -1.20000 AFIX 0 HKLF 4 REM PDF33 REM R1 = 0.0595 for 8546 Fo > 4sig(Fo) and 0.1321 for all 15420 data REM 754 parameters refined using 8 restraints END WGHT 0.0094 0.0000 REM Highest difference peak 0.848, deepest hole -0.623, 1-sigma level 0.095 Q1 1 0.3870 0.1790 0.6887 11.00000 0.05 0.85 Q2 1 0.5086 0.9494 0.8601 11.00000 0.05 0.71 Q3 1 0.7877 0.8298 0.8300 11.00000 0.05 0.69 Q4 1 0.7675 0.8510 0.8880 11.00000 0.05 0.67 Q5 1 1.1337 0.8681 0.7857 11.00000 0.05 0.63 Q6 1 0.3564 0.2414 0.7528 11.00000 0.05 0.61 Q7 1 0.6771 0.7334 0.8162 11.00000 0.05 0.52 Q8 1 0.4168 0.1763 0.7393 11.00000 0.05 0.48 Q9 1 0.1982 0.2292 0.6984 11.00000 0.05 0.47 Q10 1 0.9739 0.8757 0.7996 11.00000 0.05 0.46 Q11 1 0.5103 0.2173 0.6938 11.00000 0.05 0.45 Q12 1 0.4817 0.2916 0.7588 11.00000 0.05 0.45 Q13 1 0.5934 0.1469 0.6762 11.00000 0.05 0.44 Q14 1 0.6758 0.2427 0.7001 11.00000 0.05 0.44 Q15 1 0.7178 0.7272 0.8639 11.00000 0.05 0.42 Q16 1 0.8213 0.2582 0.4196 11.00000 0.05 0.42 Q17 1 0.4551 0.3201 0.7119 11.00000 0.05 0.41 Q18 1 0.9641 0.8370 0.8418 11.00000 0.05 0.40 Q19 1 0.5317 0.2327 0.7568 11.00000 0.05 0.40 Q20 1 0.9786 0.8238 0.8321 11.00000 0.05 0.40 Q21 1 0.4637 0.1771 0.6522 11.00000 0.05 0.38 Q22 1 0.6595 0.7578 0.8697 11.00000 0.05 0.38 Q23 1 0.8045 0.1643 0.4292 11.00000 0.05 0.38 Q24 1 0.8735 0.3842 0.4405 11.00000 0.05 0.37 Q25 1 -0.0618 0.5134 1.0082 11.00000 0.05 0.37 Q26 1 0.6297 0.8064 0.8772 11.00000 0.05 0.37 Q27 1 0.4726 0.1917 0.6678 11.00000 0.05 0.37 Q28 1 0.3684 0.1382 0.7578 11.00000 0.05 0.37 Q29 1 0.8575 0.1226 0.4199 11.00000 0.05 0.36 Q30 1 0.5245 0.4086 0.8405 11.00000 0.05 0.36 ; _shelx_res_checksum 8147 _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 Ru1 Ru 0.72565(4) 0.79590(2) 0.85043(2) 0.02005(11) Uani 1 1 d . Ru2 Ru 0.43209(4) 0.22961(2) 0.72065(2) 0.01801(11) Uani 1 1 d . O1 O 0.6784(3) 0.6623(2) 0.81420(17) 0.0257(9) Uani 1 1 d . O2 O 0.7224(3) 0.71884(19) 0.93552(17) 0.0260(8) Uani 1 1 d . O3 O 0.6200(3) 0.51053(18) 0.83835(16) 0.0206(7) Uani 1 1 d . O4 O 0.5197(3) 0.35965(19) 0.74422(17) 0.0225(8) Uani 1 1 d . O5 O 0.5118(3) 0.30489(19) 0.84003(17) 0.0227(8) Uani 1 1 d . O6 O 0.7793(3) 0.9717(2) 0.92616(19) 0.0326(9) Uani 1 1 d . O7 O 0.3345(3) 0.0640(2) 0.73493(19) 0.0317(9) Uani 1 1 d . P1 P 0.52206(13) 0.79178(8) 0.84764(7) 0.0249(3) Uani 1 1 d . P2 P 0.92752(14) 0.79156(9) 0.85329(7) 0.0277(3) Uani 1 1 d . P3 P 0.25346(13) 0.27136(9) 0.73418(7) 0.0266(3) Uani 1 1 d . P4 P 0.61448(13) 0.19768(8) 0.70745(7) 0.0208(3) Uani 1 1 d . S1 S 0.67289(12) 0.83425(7) 0.57460(6) 0.0228(3) Uani 1 1 d . C1 C 0.7167(5) 0.8235(3) 0.7506(3) 0.0251(12) Uani 1 1 d . H1 H 0.679610 0.778738 0.708914 0.030 Uiso 1 1 calc R C2 C 0.7536(4) 0.8936(3) 0.7319(3) 0.0217(11) Uani 1 1 d . H2 H 0.783708 0.940916 0.772176 0.026 Uiso 1 1 calc R C3 C 0.7521(4) 0.9044(3) 0.6567(2) 0.0209(11) Uani 1 1 d . C4 C 0.8127(4) 0.9723(3) 0.6401(3) 0.0229(11) Uani 1 1 d . H4 H 0.860936 1.018037 0.677193 0.027 Uiso 1 1 calc R C11 C 0.6529(5) 0.5547(3) 0.9634(3) 0.0352(14) Uani 1 1 d . H11 H 0.675131 0.589567 1.012728 0.042 Uiso 1 1 calc R C10 C 0.6569(5) 0.5768(3) 0.8976(3) 0.0249(12) Uani 1 1 d . C9 C 0.6888(5) 0.6557(3) 0.8814(3) 0.0241(12) Uani 1 1 d . C12 C 0.6092(5) 0.4698(3) 0.9432(3) 0.0316(13) Uani 1 1 d . H12 H 0.594972 0.436272 0.976493 0.038 Uiso 1 1 calc R C13 C 0.5913(4) 0.4454(3) 0.8681(3) 0.0221(11) Uani 1 1 d . C14 C 0.5392(4) 0.3661(3) 0.8151(3) 0.0225(11) Uani 1 1 d . C15 C 0.7603(5) 0.9030(3) 0.8963(2) 0.0234(12) Uani 1 1 d . C17 C 0.4732(6) 0.8778(4) 0.8164(3) 0.0434(16) Uani 1 1 d . H17 H 0.544907 0.923222 0.830993 0.052 Uiso 1 1 calc R C18 C 0.4414(6) 0.8609(4) 0.7310(3) 0.0432(16) Uani 1 1 d . H18A H 0.372042 0.815893 0.711854 0.052 Uiso 1 1 calc GR H18B H 0.506511 0.846352 0.708885 0.052 Uiso 1 1 calc GR H18C H 0.425371 0.909559 0.717481 0.052 Uiso 1 1 calc GR C19 C 0.3865(8) 0.9127(5) 0.8517(4) 0.079(3) Uani 1 1 d . H19A H 0.375810 0.959927 0.833461 0.094 Uiso 1 1 calc GR H19B H 0.413382 0.929458 0.906333 0.094 Uiso 1 1 calc GR H19C H 0.312267 0.871900 0.839151 0.094 Uiso 1 1 calc GR C20 C 0.4221(5) 0.6944(3) 0.7908(3) 0.0316(13) Uani 1 1 d . H20 H 0.439421 0.653159 0.817834 0.038 Uiso 1 1 calc R C21 C 0.4447(5) 0.6635(3) 0.7117(3) 0.0388(14) Uani 1 1 d . H21A H 0.526893 0.662252 0.714789 0.047 Uiso 1 1 calc GR H21B H 0.425873 0.699863 0.680792 0.047 Uiso 1 1 calc GR H21C H 0.395675 0.608652 0.688928 0.047 Uiso 1 1 calc GR C22 C 0.2928(5) 0.6898(4) 0.7886(3) 0.0453(15) Uani 1 1 d . H22A H 0.247923 0.634129 0.764350 0.054 Uiso 1 1 calc GR H22B H 0.267950 0.726695 0.760102 0.054 Uiso 1 1 calc GR H22C H 0.279299 0.705713 0.839902 0.054 Uiso 1 1 calc GR C23 C 0.4802(5) 0.8018(3) 0.9416(3) 0.0314(13) Uani 1 1 d . H23 H 0.403321 0.816693 0.937188 0.038 Uiso 1 1 calc R C24 C 0.4643(6) 0.7240(4) 0.9687(3) 0.0408(16) Uani 1 1 d . H24A H 0.535012 0.703557 0.967855 0.049 Uiso 1 1 calc GR H24B H 0.397922 0.682953 0.935468 0.049 Uiso 1 1 calc GR H24C H 0.449712 0.735757 1.019961 0.049 Uiso 1 1 calc GR C25 C 0.5664(6) 0.8712(4) 0.9993(3) 0.0484(18) Uani 1 1 d . H25A H 0.574027 0.920583 0.981434 0.058 Uiso 1 1 calc GR H25B H 0.642394 0.857776 1.007162 0.058 Uiso 1 1 calc GR H25C H 0.538554 0.880203 1.046831 0.058 Uiso 1 1 calc GR C29 C 0.9934(5) 0.7804(4) 0.9471(3) 0.0345(14) Uani 1 1 d . H29 H 0.949961 0.726633 0.951226 0.041 Uiso 1 1 calc R C30 C 0.9738(5) 0.8433(4) 1.0118(3) 0.0401(15) Uani 1 1 d . H30A H 0.996368 0.829225 1.059079 0.048 Uiso 1 1 calc GR H30B H 0.891295 0.844455 1.004584 0.048 Uiso 1 1 calc GR H30C H 1.021195 0.896943 1.013650 0.048 Uiso 1 1 calc GR C31 C 1.1211(6) 0.7780(5) 0.9576(4) 0.0586(19) Uani 1 1 d . H31A H 1.169294 0.832712 0.964282 0.070 Uiso 1 1 calc GR H31B H 1.134289 0.741286 0.913224 0.070 Uiso 1 1 calc GR H31C H 1.141948 0.758537 1.002034 0.070 Uiso 1 1 calc GR C26 C 1.0346(6) 0.8763(4) 0.8368(3) 0.0482(17) Uani 1 1 d . H26 H 1.110104 0.867584 0.860403 0.058 Uiso 1 1 calc R C27 C 1.0371(6) 0.9591(3) 0.8819(3) 0.0441(16) Uani 1 1 d . H27A H 1.106805 0.997618 0.878152 0.053 Uiso 1 1 calc GR H27B H 1.038773 0.958503 0.934497 0.053 Uiso 1 1 calc GR H27C H 0.967395 0.975712 0.862597 0.053 Uiso 1 1 calc GR C28 C 1.0520(7) 0.8743(5) 0.7605(4) 0.073(2) Uani 1 1 d . H28A H 0.978003 0.871896 0.728625 0.088 Uiso 1 1 calc GR H28B H 1.080359 0.826193 0.740660 0.088 Uiso 1 1 calc GR H28C H 1.109506 0.923298 0.760910 0.088 Uiso 1 1 calc GR C32 C 0.9509(5) 0.7021(3) 0.7863(3) 0.0365(14) Uani 1 1 d . H32 H 1.033922 0.716797 0.780719 0.044 Uiso 1 1 calc R C33 C 0.8770(6) 0.6864(4) 0.7082(3) 0.0423(16) Uani 1 1 d . H33A H 0.902872 0.646495 0.672437 0.051 Uiso 1 1 calc GR H33B H 0.885797 0.737269 0.692654 0.051 Uiso 1 1 calc GR H33C H 0.794959 0.665413 0.709321 0.051 Uiso 1 1 calc GR C34 C 0.9356(6) 0.6232(4) 0.8110(3) 0.0510(18) Uani 1 1 d . H34A H 0.852985 0.602188 0.810747 0.061 Uiso 1 1 calc GR H34B H 0.980986 0.633605 0.861735 0.061 Uiso 1 1 calc GR H34C H 0.962840 0.583211 0.776234 0.061 Uiso 1 1 calc GR C5 C 0.3771(4) 0.1942(3) 0.6081(2) 0.0195(11) Uani 1 1 d . H5 H 0.404064 0.234088 0.582973 0.023 Uiso 1 1 calc R C6 C 0.3107(4) 0.1258(3) 0.5631(2) 0.0214(11) Uani 1 1 d . H6 H 0.281132 0.085645 0.587409 0.026 Uiso 1 1 calc R C7 C 0.2761(4) 0.1029(3) 0.4818(2) 0.0213(11) Uani 1 1 d . C8 C 0.2043(4) 0.0330(3) 0.4378(2) 0.0230(11) Uani 1 1 d . H8 H 0.168055 -0.009309 0.457668 0.028 Uiso 1 1 calc R C16 C 0.3722(4) 0.1294(3) 0.7272(2) 0.0217(11) Uani 1 1 d . C41 C 0.2460(5) 0.3707(4) 0.7155(3) 0.0388(15) Uani 1 1 d . H41 H 0.161996 0.372341 0.710469 0.047 Uiso 1 1 calc R C42 C 0.3125(6) 0.4477(4) 0.7742(4) 0.0524(18) Uani 1 1 d . H42A H 0.396381 0.451531 0.778857 0.063 Uiso 1 1 calc GR H42B H 0.290205 0.446282 0.822626 0.063 Uiso 1 1 calc GR H42C H 0.293985 0.494948 0.759050 0.063 Uiso 1 1 calc GR C43 C 0.2769(6) 0.3736(4) 0.6386(3) 0.0548(19) Uani 1 1 d . H43A H 0.228005 0.326319 0.600140 0.066 Uiso 1 1 calc GR H43B H 0.359139 0.372845 0.640333 0.066 Uiso 1 1 calc GR H43C H 0.263451 0.423432 0.626402 0.066 Uiso 1 1 calc GR C35 C 0.1244(5) 0.2029(4) 0.6672(3) 0.0389(15) Uani 1 1 d . H35 H 0.150622 0.188210 0.618439 0.047 Uiso 1 1 calc R C37 C 0.0156(5) 0.2369(4) 0.6497(3) 0.0474(17) Uani 1 1 d . H37A H 0.036826 0.283712 0.628984 0.057 Uiso 1 1 calc GR H37B H -0.013232 0.253711 0.695974 0.057 Uiso 1 1 calc GR H37C H -0.045424 0.194612 0.613078 0.057 Uiso 1 1 calc GR C36 C 0.0860(6) 0.1222(4) 0.6885(4) 0.0498(18) Uani 1 1 d . H36A H 0.042439 0.130516 0.729169 0.060 Uiso 1 1 calc GR H36B H 0.154948 0.103299 0.705042 0.060 Uiso 1 1 calc GR H36C H 0.036234 0.081422 0.644645 0.060 Uiso 1 1 calc GR C38 C 0.2304(5) 0.2860(4) 0.8328(3) 0.0332(14) Uani 1 1 d . H38 H 0.294288 0.333384 0.862940 0.040 Uiso 1 1 calc R C39 C 0.1173(6) 0.3096(4) 0.8466(3) 0.0516(18) Uani 1 1 d . H39A H 0.051122 0.263131 0.822917 0.062 Uiso 1 1 calc GR H39B H 0.108674 0.355135 0.824907 0.062 Uiso 1 1 calc GR H39C H 0.119354 0.325724 0.900673 0.062 Uiso 1 1 calc GR C40 C 0.2477(6) 0.2152(4) 0.8654(3) 0.0459(16) Uani 1 1 d . H40A H 0.326220 0.207305 0.863106 0.055 Uiso 1 1 calc GR H40B H 0.189927 0.165730 0.836301 0.055 Uiso 1 1 calc GR H40C H 0.237895 0.226995 0.917759 0.055 Uiso 1 1 calc GR C44 C 0.6919(5) 0.1903(3) 0.7991(3) 0.0258(12) Uani 1 1 d . H44 H 0.718738 0.247285 0.831307 0.031 Uiso 1 1 calc R C45 C 0.6142(5) 0.1434(3) 0.8415(3) 0.0326(14) Uani 1 1 d . H45A H 0.659344 0.145732 0.890502 0.039 Uiso 1 1 calc GR H45B H 0.585518 0.086649 0.812455 0.039 Uiso 1 1 calc GR H45C H 0.547974 0.167755 0.848620 0.039 Uiso 1 1 calc GR C46 C 0.8030(5) 0.1580(4) 0.7952(3) 0.0378(14) Uani 1 1 d . H46A H 0.847249 0.182422 0.762087 0.045 Uiso 1 1 calc GR H46B H 0.781041 0.098783 0.775520 0.045 Uiso 1 1 calc GR H46C H 0.851134 0.172116 0.845641 0.045 Uiso 1 1 calc GR C47 C 0.6242(5) 0.1049(3) 0.6392(2) 0.0243(12) Uani 1 1 d . H47 H 0.705015 0.097936 0.652801 0.029 Uiso 1 1 calc R C48 C 0.5416(5) 0.0277(3) 0.6444(3) 0.0310(13) Uani 1 1 d . H48A H 0.555936 -0.019645 0.610715 0.037 Uiso 1 1 calc GR H48B H 0.460771 0.030818 0.629838 0.037 Uiso 1 1 calc GR H48C H 0.555197 0.022570 0.696133 0.037 Uiso 1 1 calc GR C49 C 0.6076(5) 0.1087(3) 0.5569(3) 0.0319(14) Uani 1 1 d . H49A H 0.613980 0.057364 0.525200 0.038 Uiso 1 1 calc GR H49B H 0.667691 0.153371 0.551570 0.038 Uiso 1 1 calc GR H49C H 0.530404 0.117968 0.541523 0.038 Uiso 1 1 calc GR C50 C 0.7235(5) 0.2753(3) 0.6821(3) 0.0306(13) Uani 1 1 d . H50 H 0.778747 0.245763 0.659107 0.037 Uiso 1 1 calc R C52 C 0.7979(5) 0.3446(3) 0.7468(3) 0.0360(14) Uani 1 1 d . H52A H 0.843423 0.322620 0.781889 0.043 Uiso 1 1 calc GR H52B H 0.747219 0.373958 0.773043 0.043 Uiso 1 1 calc GR H52C H 0.850749 0.381944 0.727196 0.043 Uiso 1 1 calc GR C51 C 0.6674(5) 0.3109(3) 0.6213(3) 0.0310(13) Uani 1 1 d . H51A H 0.621604 0.347585 0.643358 0.037 Uiso 1 1 calc GR H51B H 0.616380 0.266782 0.580678 0.037 Uiso 1 1 calc GR H51C H 0.728614 0.341186 0.601314 0.037 Uiso 1 1 calc GR C56 C 1.0159(6) 0.1840(5) 0.4445(4) 0.067(2) Uani 1 1 d D H56 H 1.092799 0.176160 0.448279 0.080 Uiso 1 1 calc R C57 C 0.9977(8) 0.2611(5) 0.4563(4) 0.082(3) Uani 1 1 d D H57 H 1.062033 0.306739 0.467616 0.098 Uiso 1 1 calc R C58 C 0.8855(8) 0.2720(4) 0.4518(4) 0.071(3) Uani 1 1 d D H58 H 0.872053 0.325025 0.460010 0.085 Uiso 1 1 calc R C53 C 0.7936(7) 0.2050(5) 0.4351(4) 0.068(3) Uani 1 1 d D H53 H 0.716466 0.212406 0.431947 0.082 Uiso 1 1 calc R C54 C 0.8104(7) 0.1276(4) 0.4230(4) 0.069(2) Uani 1 1 d D H54 H 0.746288 0.081836 0.411980 0.083 Uiso 1 1 calc R C55 C 0.9222(7) 0.1185(4) 0.4271(4) 0.064(2) Uani 1 1 d D H55 H 0.935243 0.065321 0.417761 0.077 Uiso 1 1 calc R C61 C 0.9547(17) 0.4982(7) 0.4298(6) 0.139(7) Uani 1 1 d D H61 H 0.920445 0.497306 0.380217 0.167 Uiso 1 1 calc R C60 C 0.8833(11) 0.4958(6) 0.4823(9) 0.142(5) Uani 1 1 d D H60 H 0.802427 0.492518 0.468461 0.171 Uiso 1 1 calc R C59 C 0.9317(18) 0.4982(6) 0.5552(7) 0.136(6) Uani 1 1 d D H59 H 0.885830 0.497254 0.592799 0.163 Uiso 1 1 calc R C62 C -0.0144(10) 0.4815(5) 0.9229(5) 0.086(3) Uani 1 1 d . H62 H -0.025770 0.469312 0.869734 0.104 Uiso 1 1 calc R C63 C -0.0933(10) 0.4430(6) 0.9568(5) 0.092(3) Uani 1 1 d . H63 H -0.158066 0.401996 0.926631 0.110 Uiso 1 1 calc R C64 C -0.0824(9) 0.4615(6) 1.0335(5) 0.100(3) Uani 1 1 d . H64 H -0.140471 0.435445 1.056034 0.120 Uiso 1 1 calc R C65 C 0.5125(8) 0.5729(5) 0.4822(5) 0.078(3) Uani 1 1 d . H65 H 0.519369 0.623533 0.469644 0.094 Uiso 1 1 calc R C66 C 0.5671(8) 0.5703(5) 0.5505(5) 0.080(3) Uani 1 1 d . H66 H 0.614627 0.618146 0.585307 0.096 Uiso 1 1 calc R C67 C 0.5517(9) 0.4959(6) 0.5681(4) 0.086(3) Uani 1 1 d . H67 H 0.586771 0.493192 0.616248 0.103 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 Ru1 0.0249(3) 0.0199(2) 0.0141(2) 0.00384(17) 0.00270(19) 0.00411(19) Ru2 0.0185(3) 0.0197(2) 0.0160(2) 0.00571(17) 0.00339(19) 0.00371(19) O1 0.034(2) 0.0247(19) 0.0180(17) 0.0043(14) 0.0040(16) 0.0082(17) O2 0.031(2) 0.0226(19) 0.0216(17) 0.0032(15) 0.0028(16) 0.0054(17) O3 0.027(2) 0.0177(17) 0.0146(15) 0.0028(13) 0.0035(15) 0.0023(15) O4 0.025(2) 0.0259(19) 0.0191(17) 0.0065(14) 0.0043(16) 0.0101(16) O5 0.027(2) 0.0187(18) 0.0212(17) 0.0069(14) 0.0031(16) 0.0019(16) O6 0.038(3) 0.029(2) 0.0261(19) 0.0035(16) 0.0059(18) 0.0017(18) O7 0.032(2) 0.034(2) 0.031(2) 0.0145(17) 0.0064(18) 0.0041(19) P1 0.0273(9) 0.0243(7) 0.0239(7) 0.0071(6) 0.0066(6) 0.0057(6) P2 0.0263(9) 0.0306(8) 0.0228(7) 0.0024(6) 0.0033(6) 0.0048(7) P3 0.0236(9) 0.0331(8) 0.0223(7) 0.0051(6) 0.0040(6) 0.0073(7) P4 0.0218(9) 0.0197(7) 0.0185(6) 0.0029(5) 0.0019(6) 0.0033(6) S1 0.0271(8) 0.0218(6) 0.0168(6) 0.0053(5) 0.0019(6) 0.0014(6) C1 0.027(3) 0.030(3) 0.015(2) 0.003(2) 0.003(2) 0.004(2) C2 0.025(3) 0.021(3) 0.021(2) 0.006(2) 0.005(2) 0.007(2) C3 0.018(3) 0.026(3) 0.016(2) 0.002(2) 0.000(2) 0.006(2) C4 0.024(3) 0.022(3) 0.018(2) 0.001(2) -0.001(2) 0.003(2) C11 0.057(4) 0.026(3) 0.020(3) 0.004(2) 0.007(3) 0.005(3) C10 0.031(3) 0.019(3) 0.022(2) 0.001(2) 0.004(2) 0.006(2) C9 0.016(3) 0.034(3) 0.020(3) 0.003(2) 0.001(2) 0.007(2) C12 0.051(4) 0.025(3) 0.020(3) 0.011(2) 0.006(3) 0.006(3) C13 0.023(3) 0.019(2) 0.024(2) 0.006(2) 0.005(2) 0.004(2) C14 0.013(3) 0.029(3) 0.026(3) 0.005(2) 0.004(2) 0.009(2) C15 0.030(3) 0.027(3) 0.015(2) 0.010(2) 0.007(2) 0.003(2) C17 0.042(4) 0.055(4) 0.043(3) 0.020(3) 0.009(3) 0.025(3) C18 0.037(4) 0.053(4) 0.044(4) 0.028(3) 0.003(3) 0.007(3) C19 0.099(7) 0.075(6) 0.089(6) 0.042(5) 0.034(5) 0.049(5) C20 0.028(4) 0.033(3) 0.031(3) 0.007(2) 0.007(3) 0.001(3) C21 0.036(4) 0.038(3) 0.030(3) 0.001(2) -0.001(3) -0.004(3) C22 0.025(4) 0.048(4) 0.053(4) 0.007(3) 0.001(3) -0.002(3) C23 0.038(4) 0.029(3) 0.033(3) 0.009(2) 0.021(3) 0.010(3) C24 0.052(5) 0.051(4) 0.029(3) 0.021(3) 0.019(3) 0.013(3) C25 0.058(5) 0.056(4) 0.029(3) 0.004(3) 0.021(3) 0.009(4) C29 0.027(4) 0.047(4) 0.027(3) 0.007(3) 0.000(3) 0.010(3) C30 0.028(4) 0.058(4) 0.028(3) 0.008(3) -0.005(3) 0.007(3) C31 0.030(4) 0.091(6) 0.052(4) 0.016(4) -0.002(3) 0.020(4) C26 0.043(5) 0.049(4) 0.050(4) 0.004(3) 0.026(3) 0.001(3) C27 0.040(4) 0.038(4) 0.049(4) 0.011(3) 0.007(3) -0.003(3) C28 0.092(7) 0.070(5) 0.047(4) 0.014(4) 0.024(4) -0.011(5) C32 0.036(4) 0.043(3) 0.033(3) 0.003(3) 0.010(3) 0.019(3) C33 0.043(4) 0.050(4) 0.029(3) -0.007(3) 0.013(3) 0.013(3) C34 0.063(5) 0.050(4) 0.047(4) 0.007(3) 0.017(4) 0.031(4) C5 0.015(3) 0.024(3) 0.021(2) 0.009(2) 0.003(2) 0.005(2) C6 0.018(3) 0.027(3) 0.019(2) 0.009(2) 0.003(2) 0.004(2) C7 0.019(3) 0.026(3) 0.021(2) 0.010(2) 0.005(2) 0.005(2) C8 0.024(3) 0.023(3) 0.021(2) 0.008(2) 0.002(2) 0.006(2) C16 0.019(3) 0.033(3) 0.012(2) 0.004(2) 0.002(2) 0.006(2) C41 0.029(4) 0.050(4) 0.043(3) 0.014(3) 0.007(3) 0.020(3) C42 0.049(5) 0.039(4) 0.074(5) 0.015(3) 0.013(4) 0.022(3) C43 0.060(5) 0.074(5) 0.059(4) 0.048(4) 0.023(4) 0.041(4) C35 0.016(3) 0.061(4) 0.032(3) 0.002(3) -0.002(3) 0.006(3) C37 0.024(4) 0.081(5) 0.036(3) 0.008(3) 0.007(3) 0.015(3) C36 0.026(4) 0.051(4) 0.055(4) -0.009(3) 0.006(3) -0.005(3) C38 0.023(3) 0.045(4) 0.028(3) -0.001(3) 0.009(3) 0.008(3) C39 0.037(4) 0.079(5) 0.036(3) 0.003(3) 0.014(3) 0.016(4) C40 0.046(4) 0.061(4) 0.030(3) 0.013(3) 0.018(3) 0.002(3) C44 0.022(3) 0.038(3) 0.016(2) 0.003(2) 0.002(2) 0.009(3) C45 0.038(4) 0.042(3) 0.023(3) 0.016(2) 0.004(3) 0.015(3) C46 0.030(4) 0.059(4) 0.024(3) 0.010(3) -0.004(3) 0.017(3) C47 0.028(3) 0.028(3) 0.017(2) 0.001(2) -0.001(2) 0.015(2) C48 0.040(4) 0.027(3) 0.027(3) 0.005(2) 0.003(3) 0.013(3) C49 0.037(4) 0.043(3) 0.018(3) 0.005(2) 0.005(2) 0.018(3) C50 0.027(3) 0.029(3) 0.036(3) 0.006(2) 0.010(3) 0.007(3) C52 0.026(4) 0.031(3) 0.045(3) 0.004(3) 0.007(3) 0.000(3) C51 0.029(4) 0.030(3) 0.041(3) 0.018(2) 0.018(3) 0.004(3) C56 0.048(6) 0.126(8) 0.041(4) 0.033(5) 0.015(4) 0.038(6) C57 0.094(8) 0.088(7) 0.035(4) 0.017(4) 0.002(5) -0.037(6) C58 0.133(9) 0.041(4) 0.039(4) 0.010(3) 0.012(5) 0.027(5) C53 0.058(6) 0.131(8) 0.038(4) 0.031(5) 0.014(4) 0.060(6) C54 0.074(7) 0.075(6) 0.045(4) 0.015(4) 0.018(4) -0.015(5) C55 0.102(7) 0.064(5) 0.044(4) 0.021(4) 0.032(5) 0.040(5) C61 0.27(2) 0.080(8) 0.062(7) 0.007(6) -0.025(10) 0.075(11) C60 0.220(16) 0.064(7) 0.126(11) 0.003(7) -0.031(12) 0.063(9) C59 0.248(19) 0.063(6) 0.098(10) 0.009(6) 0.006(10) 0.075(10) C62 0.116(9) 0.073(6) 0.057(5) 0.002(5) -0.024(6) 0.038(6) C63 0.119(9) 0.078(6) 0.049(5) -0.006(4) -0.028(5) 0.013(6) C64 0.115(9) 0.105(7) 0.055(5) -0.002(5) -0.020(5) 0.019(7) C65 0.127(9) 0.063(5) 0.061(5) 0.029(4) 0.023(5) 0.043(6) C66 0.092(7) 0.076(6) 0.072(6) 0.019(5) 0.022(5) 0.019(5) C67 0.129(9) 0.099(7) 0.043(4) 0.029(5) 0.006(5) 0.051(7) 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' Ru Ru -1.2594 0.8363 '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 O1 Ru1 O2 58.52(11) . . O1 Ru1 P1 88.19(10) . . O1 Ru1 P2 88.54(10) . . O1 Ru1 C9 29.32(13) . . O2 Ru1 P1 89.82(10) . . O2 Ru1 P2 87.60(10) . . O2 Ru1 C9 29.22(13) . . P1 Ru1 P2 176.57(5) . . P1 Ru1 C9 88.10(12) . . P2 Ru1 C9 88.55(12) . . C1 Ru1 O1 100.85(17) . . C1 Ru1 O2 159.29(16) . . C1 Ru1 P1 91.38(15) . . C1 Ru1 P2 90.24(15) . . C1 Ru1 C9 130.17(18) . . C15 Ru1 O1 169.75(16) . . C15 Ru1 O2 111.55(16) . . C15 Ru1 P1 89.26(17) . . C15 Ru1 P2 93.79(18) . . C15 Ru1 C1 89.1(2) . . C15 Ru1 C9 140.65(17) . . O4 Ru2 O5 58.83(11) . . O4 Ru2 P3 87.55(9) . . O4 Ru2 P4 88.61(9) . . O4 Ru2 C14 29.75(12) . . O5 Ru2 P3 88.82(9) . . O5 Ru2 P4 89.76(9) . . O5 Ru2 C14 29.11(12) . . P3 Ru2 C14 86.92(11) . . P4 Ru2 P3 176.10(5) . . P4 Ru2 C14 90.08(11) . . C5 Ru2 O4 104.52(16) . . C5 Ru2 O5 163.34(15) . . C5 Ru2 P3 89.84(14) . . C5 Ru2 P4 90.48(14) . . C5 Ru2 C14 134.23(17) . . C16 Ru2 O4 165.18(16) . . C16 Ru2 O5 106.35(16) . . C16 Ru2 P3 92.71(17) . . C16 Ru2 P4 91.18(17) . . C16 Ru2 C14 135.45(18) . . C16 Ru2 C5 90.3(2) . . C9 O1 Ru1 92.7(3) . . C9 O2 Ru1 88.9(3) . . C10 O3 C13 106.0(3) . . C14 O4 Ru2 91.4(3) . . C14 O5 Ru2 89.1(3) . . C17 P1 Ru1 114.1(2) . . C20 P1 Ru1 114.13(19) . . C20 P1 C17 108.6(3) . . C20 P1 C23 102.6(2) . . C23 P1 Ru1 113.8(2) . . C23 P1 C17 102.3(2) . . C29 P2 Ru1 109.71(19) . . C26 P2 Ru1 121.3(2) . . C26 P2 C29 104.3(3) . . C26 P2 C32 101.6(3) . . C32 P2 Ru1 114.9(2) . . C32 P2 C29 103.1(2) . . C41 P3 Ru2 116.0(2) . . C41 P3 C38 102.5(3) . . C35 P3 Ru2 113.37(19) . . C35 P3 C41 101.5(3) . . C35 P3 C38 111.3(3) . . C38 P3 Ru2 111.38(19) . . C44 P4 Ru2 110.09(17) . . C44 P4 C50 102.7(2) . . C47 P4 Ru2 121.73(18) . . C47 P4 C44 104.2(2) . . C47 P4 C50 99.7(2) . . C50 P4 Ru2 116.21(18) . . C3 S1 C7 92.4(2) . 2_666 C2 C1 Ru1 132.0(4) . . C1 C2 C3 126.9(5) . . C2 C3 S1 125.2(4) . . C4 C3 S1 110.1(3) . . C4 C3 C2 124.7(4) . . C3 C4 C8 113.1(4) . 2_666 C10 C11 C12 106.0(4) . . O3 C10 C11 110.5(4) . . O3 C10 C9 117.4(4) . . C11 C10 C9 132.1(4) . . O1 C9 Ru1 58.0(2) . . O1 C9 C10 121.2(4) . . O2 C9 Ru1 61.9(3) . . O2 C9 O1 119.9(5) . . O2 C9 C10 118.9(4) . . C10 C9 Ru1 174.8(4) . . C13 C12 C11 106.9(4) . . O3 C13 C14 117.1(4) . . C12 C13 O3 110.6(4) . . C12 C13 C14 132.1(4) . . O4 C14 Ru2 58.8(2) . . O4 C14 C13 120.4(4) . . O5 C14 Ru2 61.8(2) . . O5 C14 O4 120.5(4) . . O5 C14 C13 119.1(4) . . C13 C14 Ru2 175.6(4) . . O6 C15 Ru1 178.0(5) . . C18 C17 P1 112.6(4) . . C19 C17 P1 118.9(4) . . C19 C17 C18 110.8(5) . . C21 C20 P1 115.4(4) . . C22 C20 P1 115.3(4) . . C22 C20 C21 110.7(5) . . C24 C23 P1 114.8(4) . . C25 C23 P1 110.2(4) . . C25 C23 C24 110.8(5) . . C30 C29 P2 112.4(4) . . C30 C29 C31 110.1(5) . . C31 C29 P2 115.7(4) . . C27 C26 P2 115.6(4) . . C28 C26 P2 119.2(5) . . C28 C26 C27 113.3(6) . . C33 C32 P2 112.0(4) . . C34 C32 P2 116.3(4) . . C34 C32 C33 109.4(5) . . C6 C5 Ru2 131.9(4) . . C5 C6 C7 129.5(4) . . C6 C7 S1 122.8(4) . 2_666 C8 C7 S1 109.6(3) . 2_666 C8 C7 C6 127.6(4) . . C7 C8 C4 114.8(4) . 2_666 O7 C16 Ru2 177.1(4) . . C42 C41 P3 118.7(4) . . C42 C41 C43 110.0(5) . . C43 C41 P3 110.0(4) . . C37 C35 P3 118.2(4) . . C36 C35 P3 112.0(4) . . C36 C35 C37 108.8(5) . . C39 C38 P3 115.4(4) . . C40 C38 P3 112.8(4) . . C40 C38 C39 111.5(5) . . C45 C44 P4 114.2(4) . . C45 C44 C46 109.5(4) . . C46 C44 P4 114.8(3) . . C48 C47 P4 113.2(3) . . C48 C47 C49 108.7(4) . . C49 C47 P4 115.2(3) . . C52 C50 P4 116.3(4) . . C52 C50 C51 109.0(4) . . C51 C50 P4 112.1(4) . . C55 C56 C57 119.5(7) . . C56 C57 C58 119.9(7) . . C53 C58 C57 119.1(7) . . C54 C53 C58 121.7(7) . . C55 C54 C53 118.0(7) . . C54 C55 C56 121.8(7) . . C59 C61 C60 123.8(11) 2_766 . C59 C60 C61 119.0(11) . . C61 C59 C60 117.1(12) 2_766 . C63 C62 C64 119.3(9) . 2_567 C62 C63 C64 122.0(10) . . C63 C64 C62 118.6(10) . 2_567 C67 C65 C66 120.6(7) 2_666 . C65 C66 C67 118.2(8) . . C65 C67 C66 121.2(7) 2_666 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ru1 O1 2.202(3) . Ru1 O2 2.289(3) . Ru1 P1 2.4102(16) . Ru1 P2 2.4196(17) . Ru1 C1 2.013(4) . Ru1 C9 2.594(5) . Ru1 C15 1.805(5) . Ru2 O4 2.211(3) . Ru2 O5 2.276(3) . Ru2 P3 2.4138(16) . Ru2 P4 2.3840(16) . Ru2 C14 2.583(5) . Ru2 C5 2.020(5) . Ru2 C16 1.784(5) . O1 C9 1.272(5) . O2 C9 1.266(6) . O3 C10 1.355(5) . O3 C13 1.372(5) . O4 C14 1.282(5) . O5 C14 1.257(5) . O6 C15 1.162(6) . O7 C16 1.185(6) . P1 C17 1.884(6) . P1 C20 1.859(6) . P1 C23 1.869(5) . P2 C29 1.878(5) . P2 C26 1.861(6) . P2 C32 1.862(5) . P3 C41 1.852(6) . P3 C35 1.848(6) . P3 C38 1.865(5) . P4 C44 1.864(5) . P4 C47 1.856(5) . P4 C50 1.870(5) . S1 C3 1.740(5) . S1 C7 1.759(5) 2_666 C1 C2 1.349(6) . C2 C3 1.451(6) . C3 C4 1.378(7) . C4 C8 1.417(6) 2_666 C11 C10 1.366(6) . C11 C12 1.409(7) . C10 C9 1.459(7) . C12 C13 1.342(6) . C13 C14 1.464(7) . C17 C18 1.529(7) . C17 C19 1.463(8) . C20 C21 1.535(7) . C20 C22 1.524(8) . C23 C24 1.530(7) . C23 C25 1.513(8) . C29 C30 1.518(8) . C29 C31 1.519(8) . C26 C27 1.491(8) . C26 C28 1.459(8) . C32 C33 1.528(7) . C32 C34 1.525(8) . C5 C6 1.320(7) . C6 C7 1.453(6) . C7 C8 1.352(7) . C41 C42 1.517(8) . C41 C43 1.538(7) . C35 C37 1.552(8) . C35 C36 1.542(8) . C38 C39 1.528(7) . C38 C40 1.523(8) . C44 C45 1.531(7) . C44 C46 1.545(7) . C47 C48 1.530(7) . C47 C49 1.534(6) . C50 C52 1.525(7) . C50 C51 1.539(7) . C56 C57 1.375(5) . C56 C55 1.371(5) . C57 C58 1.383(5) . C58 C53 1.376(5) . C53 C54 1.373(5) . C54 C55 1.369(5) . C61 C60 1.387(5) . C61 C59 1.331(16) 2_766 C60 C59 1.386(5) . C62 C63 1.356(12) . C62 C64 1.379(12) 2_567 C63 C64 1.374(11) . C65 C66 1.359(10) . C65 C67 1.354(11) 2_666 C66 C67 1.386(10) . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 Ru1 O1 C9 O2 -2.8(5) . . Ru1 O1 C9 C10 174.0(4) . . Ru1 O2 C9 O1 2.7(5) . . Ru1 O2 C9 C10 -174.2(4) . . Ru1 P1 C17 C18 84.8(5) . . Ru1 P1 C17 C19 -143.3(5) . . Ru1 P1 C20 C21 -49.4(5) . . Ru1 P1 C20 C22 179.5(3) . . Ru1 P1 C23 C24 -79.0(5) . . Ru1 P1 C23 C25 46.9(4) . . Ru1 P2 C29 C30 -51.6(5) . . Ru1 P2 C29 C31 -179.2(4) . . Ru1 P2 C26 C27 50.1(6) . . Ru1 P2 C26 C28 -90.4(6) . . Ru1 P2 C32 C33 46.0(5) . . Ru1 P2 C32 C34 -80.8(5) . . Ru1 C1 C2 C3 173.6(4) . . Ru2 O4 C14 O5 3.7(5) . . Ru2 O4 C14 C13 -174.9(4) . . Ru2 O5 C14 O4 -3.5(5) . . Ru2 O5 C14 C13 175.0(4) . . Ru2 P3 C41 C42 -75.7(5) . . Ru2 P3 C41 C43 52.1(5) . . Ru2 P3 C35 C37 -158.3(4) . . Ru2 P3 C35 C36 74.0(4) . . Ru2 P3 C38 C39 -177.9(4) . . Ru2 P3 C38 C40 -48.2(5) . . Ru2 P4 C44 C45 43.9(4) . . Ru2 P4 C44 C46 171.7(3) . . Ru2 P4 C47 C48 -49.9(4) . . Ru2 P4 C47 C49 76.0(4) . . Ru2 P4 C50 C52 84.1(4) . . Ru2 P4 C50 C51 -42.4(4) . . Ru2 C5 C6 C7 -178.3(4) . . O3 C10 C9 O1 2.4(7) . . O3 C10 C9 O2 179.3(5) . . O3 C13 C14 O4 -1.5(7) . . O3 C13 C14 O5 179.9(4) . . S1 C3 C4 C8 -0.5(6) . 2_666 S1 C7 C8 C4 -0.5(6) 2_666 2_666 C1 C2 C3 S1 15.5(8) . . C1 C2 C3 C4 -165.2(5) . . C2 C3 C4 C8 -179.9(4) . 2_666 C11 C10 C9 O1 -175.1(6) . . C11 C10 C9 O2 1.7(9) . . C11 C12 C13 O3 -0.8(7) . . C11 C12 C13 C14 -174.6(6) . . C10 O3 C13 C12 0.2(6) . . C10 O3 C13 C14 175.0(4) . . C10 C11 C12 C13 1.0(7) . . C12 C11 C10 O3 -0.9(7) . . C12 C11 C10 C9 176.8(6) . . C12 C13 C14 O4 172.0(6) . . C12 C13 C14 O5 -6.6(9) . . C13 O3 C10 C11 0.5(6) . . C13 O3 C10 C9 -177.6(4) . . C17 P1 C20 C21 79.2(5) . . C17 P1 C20 C22 -52.0(5) . . C17 P1 C23 C24 157.3(5) . . C17 P1 C23 C25 -76.8(5) . . C20 P1 C17 C18 -43.8(5) . . C20 P1 C17 C19 88.2(6) . . C20 P1 C23 C24 44.8(5) . . C20 P1 C23 C25 170.7(4) . . C23 P1 C17 C18 -151.8(5) . . C23 P1 C17 C19 -19.8(7) . . C23 P1 C20 C21 -173.0(4) . . C23 P1 C20 C22 55.8(5) . . C29 P2 C26 C27 -74.2(6) . . C29 P2 C26 C28 145.4(6) . . C29 P2 C32 C33 165.3(4) . . C29 P2 C32 C34 38.5(5) . . C26 P2 C29 C30 79.8(5) . . C26 P2 C29 C31 -47.8(5) . . C26 P2 C32 C33 -86.9(5) . . C26 P2 C32 C34 146.3(5) . . C32 P2 C29 C30 -174.4(4) . . C32 P2 C29 C31 58.0(5) . . C32 P2 C26 C27 179.0(5) . . C32 P2 C26 C28 38.5(7) . . C5 C6 C7 S1 3.5(8) . 2_666 C5 C6 C7 C8 -177.5(5) . . C6 C7 C8 C4 -179.6(5) . 2_666 C7 S1 C3 C2 -179.9(4) 2_666 . C7 S1 C3 C4 0.7(4) 2_666 . C41 P3 C35 C37 -33.2(5) . . C41 P3 C35 C36 -160.9(4) . . C41 P3 C38 C39 57.4(5) . . C41 P3 C38 C40 -172.9(4) . . C35 P3 C41 C42 160.9(5) . . C35 P3 C41 C43 -71.2(5) . . C35 P3 C38 C39 -50.4(5) . . C35 P3 C38 C40 79.3(5) . . C38 P3 C41 C42 45.8(5) . . C38 P3 C41 C43 173.7(4) . . C38 P3 C35 C37 75.2(5) . . C38 P3 C35 C36 -52.5(5) . . C44 P4 C47 C48 75.0(4) . . C44 P4 C47 C49 -159.0(4) . . C44 P4 C50 C52 -36.1(5) . . C44 P4 C50 C51 -162.6(4) . . C47 P4 C44 C45 -88.1(4) . . C47 P4 C44 C46 39.6(5) . . C47 P4 C50 C52 -143.1(4) . . C47 P4 C50 C51 90.4(4) . . C50 P4 C44 C45 168.3(4) . . C50 P4 C44 C46 -64.0(4) . . C50 P4 C47 C48 -179.1(4) . . C50 P4 C47 C49 -53.2(4) . . C56 C57 C58 C53 -0.2(11) . . C57 C56 C55 C54 -1.6(10) . . C57 C58 C53 C54 0.0(11) . . C58 C53 C54 C55 -0.6(10) . . C53 C54 C55 C56 1.4(10) . . C55 C56 C57 C58 1.0(10) . . C61 C60 C59 C61 -0.8(19) . 2_766 C59 C61 C60 C59 1(2) 2_766 . C62 C63 C64 C62 -2.8(17) . 2_567 C64 C62 C63 C64 2.8(17) 2_567 . C65 C66 C67 C65 2.4(15) . 2_666 C67 C65 C66 C67 -2.4(15) 2_666 .