#------------------------------------------------------------------------------ #$Date: 2021-04-28 04:53:10 +0300 (Wed, 28 Apr 2021) $ #$Revision: 264609 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/72/7707205.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_7707205 loop_ _publ_author_name 'Tatarin, Sergei V.' 'Kalle, Paulina' 'Taydakov, Ilya V.' 'Varaksina, Evgenia' 'Korshunov, Vladislav M.' 'Bezzubov, Stanislav' _publ_section_title ; Sterically hindered phenanthroimidazole ligands drive structural flexibility and facile ligand exchange in cyclometalated iridium(III) complexes ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT00820J _journal_year 2021 _chemical_formula_moiety 'C71 H49 Ir N4 O6 S, 3(C H2 Cl2), 0.27(H2 O)' _chemical_formula_sum 'C74 H55.54 Cl6 Ir N4 O6.27 S' _chemical_formula_weight 1538.04 _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 _atom_sites_solution_primary dual _audit_creation_date 2020-12-22 _audit_creation_method ; Olex2 1.3 (compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003) ; _audit_update_record ; 2020-12-23 deposited with the CCDC. 2021-04-27 downloaded from the CCDC. ; _cell_angle_alpha 87.1280(10) _cell_angle_beta 82.5430(10) _cell_angle_gamma 82.4970(10) _cell_formula_units_Z 2 _cell_length_a 11.3617(4) _cell_length_b 11.4387(4) _cell_length_c 25.1626(9) _cell_measurement_reflns_used 9495 _cell_measurement_temperature 150 _cell_measurement_theta_max 30.51 _cell_measurement_theta_min 2.39 _cell_volume 3213.0(2) _computing_cell_refinement 'APEX3 v.2017.3_0 (Bruker AXS, 2017)' _computing_data_collection 'APEX3 v.2017.3_0 (Bruker AXS, 2017)' _computing_data_reduction 'SAINT v8.38A (Bruker AXS, 2016)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 150 _diffrn_detector 'CCD area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'Bruker SMART CCD area detector' _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.983 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART APEX-II' _diffrn_measurement_method \w-scan _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_unetI/netI 0.0547 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.983 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_number 38911 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.983 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.540 _diffrn_reflns_theta_min 2.291 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 30.0 _diffrn_source_power 1.5 _diffrn_source_target Mo _diffrn_source_type 'fine-focus sealed X-ray tube' _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.419 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8285 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0708 before and 0.0402 after correction. The Ratio of minimum to maximum transmission is 0.8285. The \l/2 correction factor is Not present.' _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.590 _exptl_crystal_description plate _exptl_crystal_F_000 1545 _exptl_crystal_preparation Luminescent _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: CH2Cl2, CH3OH' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _refine_diff_density_max 1.909 _refine_diff_density_min -1.509 _refine_diff_density_rms 0.149 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 836 _refine_ls_number_reflns 19375 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0427 _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^)+(0.0412P)^2^+9.7386P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0986 _refine_ls_wR_factor_ref 0.1028 _reflns_Friedel_coverage 0.000 _reflns_number_gt 16922 _reflns_number_total 19375 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt00820j2.cif _cod_data_source_block st38_p-1 _cod_database_code 7707205 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.830 _shelx_estimated_absorpt_t_min 0.684 _computing.bruker_data_scaling 'SADABS V2012/1 (Bruker AXS Inc.)' _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,H) groups 2. Others Fixed Sof: O0AA(0.27) H0AA(0.27) H0AB(0.27) 3.a Riding coordinates: O0AA(H0AA,H0AB) 3.b Secondary CH2 refined with riding coordinates: C02I(H02A,H02B), C02J(H02E,H02F), C02K(H02C,H02D) 3.c Aromatic/amide H refined with riding coordinates: C65(H65), C52(H52), C2(H2), C9(H9), C29(H29), C32(H32), C43(H43), C4(H4), C5(H5), C18(H18), C36(H36), C51(H51), C62(H62), C16(H16), C19(H19), C25(H25), C59(H59), C10(H10), C37(H37), C22(H22), C40(H40), C50(H50), C17(H17), C24(H24), C49(H49), C58(H58), C23(H23), C13(H13), C31(H31), C39(H39), C69(H69), C38(H38), C44(H44), C45(H45), C11(H11), C12(H12), C46(H46), C57(H57), C67(H67), C66(H66) 3.d Idealised Me refined as rotating group: C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C71(H71A,H71B,H71C) ; _shelx_res_file ; TITL st38_p-1_a.res in P-1 st38_p-1.res created by SHELXL-2018/3 at 17:22:51 on 22-Dec-2020 REM Old TITL st38_p-1 in P-1 REM SHELXT solution in P-1 REM R1 0.072, Rweak 0.015, Alpha 0.047, Orientation as input REM Formula found by SHELXT: C74 N5 O2 S7 Ir rem RIGU C68 Ir1 C28 C1 N1 N3 O4 O3 C33 C29 C2 C6 C34 C54 C7 C27 C63 C61 C32 = CELL 0.71073 11.3617 11.4387 25.1626 87.128 82.543 82.497 ZERR 2 0.0004 0.0004 0.0009 0.001 0.001 0.001 LATT 1 SFAC C H Cl Ir N O S UNIT 148 111.08 12 2 8 12.54 2 L.S. 8 PLAN 5 SIZE 0.17 0.14 0.08 TEMP -123.15 CONF list 4 fmap 2 acta MORE -1 BOND $H OMIT 1 0 0 OMIT -1 0 1 OMIT -2 0 6 OMIT -3 -7 13 OMIT -1 -4 19 OMIT -1 0 3 OMIT -3 1 5 OMIT 1 -3 5 OMIT 1 3 2 OMIT -2 0 1 REM REM REM WGHT 0.041200 9.738600 FVAR 0.26162 IR1 4 0.362183 0.438578 0.237712 11.00000 0.00883 0.01372 = 0.00938 -0.00019 0.00050 -0.00189 S1 7 0.694607 0.122287 0.222557 11.00000 0.02958 0.03235 = 0.03334 -0.00741 -0.00504 0.00056 CL00 3 0.627996 0.956085 0.542002 11.00000 0.04527 0.04349 = 0.04420 -0.00362 0.00166 -0.00298 CL1 3 0.398337 1.009746 0.607501 11.00000 0.05116 0.05096 = 0.05286 0.00906 0.00957 0.00758 CL2 3 0.054214 0.163516 0.001687 11.00000 0.05679 0.07511 = 0.03975 -0.01490 -0.00399 -0.02136 CL3 3 0.142421 0.056598 -0.101527 11.00000 0.04825 0.07202 = 0.04479 -0.01196 -0.00236 -0.00453 CL4 3 0.590995 0.780026 0.076710 11.00000 0.06951 0.05685 = 0.05944 -0.00748 -0.02155 0.00387 CL5 3 0.505146 1.016767 0.118450 11.00000 0.05601 0.03845 = 0.07963 0.01486 -0.00520 -0.00926 O3 6 0.496230 0.292776 0.254864 11.00000 0.01445 0.01605 = 0.01434 -0.00199 -0.00340 -0.00145 O4 6 0.399299 0.506961 0.310472 11.00000 0.01474 0.01871 = 0.01193 -0.00149 -0.00194 -0.00007 O5 6 0.090481 0.237045 0.112740 11.00000 0.01406 0.02162 = 0.02238 -0.00223 -0.00403 -0.00673 N1 5 0.211489 0.401891 0.286685 11.00000 0.01096 0.01414 = 0.01135 0.00026 -0.00049 -0.00207 O6 6 0.242966 0.873607 0.159012 11.00000 0.03056 0.01432 = 0.01905 0.00231 0.00446 -0.00092 N3 5 0.504133 0.478450 0.182318 11.00000 0.01176 0.01448 = 0.01310 -0.00083 0.00017 -0.00396 N2 5 0.050971 0.475716 0.341022 11.00000 0.01145 0.01536 = 0.01305 0.00020 0.00238 -0.00217 C34 1 0.138931 0.500349 0.301045 11.00000 0.01103 0.01250 = 0.01246 -0.00023 -0.00068 -0.00140 O2 6 0.725233 0.495724 0.500261 11.00000 0.02830 0.03094 = 0.02615 -0.00197 -0.00445 0.00128 N4 5 0.621892 0.420549 0.108197 11.00000 0.01135 0.01818 = 0.01153 -0.00191 0.00089 -0.00478 C1 1 0.320500 0.369077 0.172599 11.00000 0.01323 0.01094 = 0.01336 0.00272 -0.00239 -0.00047 C33 1 0.157899 0.608350 0.270146 11.00000 0.01244 0.01488 = 0.01154 0.00125 -0.00060 -0.00155 C28 1 0.257114 0.588720 0.228946 11.00000 0.01113 0.01235 = 0.01329 -0.00185 -0.00189 -0.00165 C53 1 0.204493 0.184647 0.313721 11.00000 0.01300 0.01468 = 0.01363 0.00031 -0.00354 -0.00454 C42 1 -0.000100 0.280315 0.388389 11.00000 0.01344 0.01991 = 0.01525 0.00262 -0.00159 -0.00629 C41 1 0.066593 0.353681 0.350839 11.00000 0.01114 0.01819 = 0.01321 -0.00084 -0.00105 -0.00499 C48 1 0.142788 0.108964 0.350843 11.00000 0.01290 0.02106 = 0.01571 0.00225 -0.00225 -0.00536 O1 6 0.644362 0.667627 0.536598 11.00000 0.03569 0.03393 = 0.02517 -0.00788 -0.01169 0.00144 C65 1 0.405581 0.659698 0.390259 11.00000 0.00917 0.01295 = 0.01213 0.00988 0.00453 0.00487 AFIX 43 H65 2 0.349814 0.676789 0.365024 11.00000 -1.20000 AFIX 0 C3 1 0.194564 0.278073 0.120536 11.00000 0.01247 0.01466 = 0.01975 0.00258 -0.00670 -0.00208 C52 1 0.298791 0.136888 0.275790 11.00000 0.01587 0.01832 = 0.01633 -0.00199 -0.00038 -0.00364 AFIX 43 H52 2 0.338678 0.187859 0.250672 11.00000 -1.20000 AFIX 0 C54 1 0.164921 0.309070 0.316272 11.00000 0.01112 0.01462 = 0.01127 0.00060 -0.00171 -0.00382 C2 1 0.211640 0.328464 0.167540 11.00000 0.01367 0.01407 = 0.01552 0.00089 0.00009 -0.00207 AFIX 43 H2 2 0.148904 0.335450 0.196528 11.00000 -1.20000 AFIX 0 C7 1 0.513614 0.414929 0.137943 11.00000 0.01188 0.01668 = 0.01207 -0.00141 -0.00015 -0.00157 C14 1 0.684798 0.492447 0.134789 11.00000 0.01190 0.01649 = 0.01199 -0.00067 -0.00075 -0.00285 C30 1 0.208757 0.789852 0.196795 11.00000 0.02352 0.01527 = 0.01368 0.00035 -0.00240 -0.00551 C9 1 0.646220 0.431757 0.010689 11.00000 0.01173 0.02303 = 0.01324 -0.00267 0.00129 -0.00251 AFIX 43 H9 2 0.620759 0.514180 0.011714 11.00000 -1.20000 AFIX 0 C27 1 0.609043 0.529410 0.179968 11.00000 0.01100 0.01581 = 0.01238 0.00219 -0.00009 -0.00235 C35 1 -0.024727 0.566104 0.371844 11.00000 0.01299 0.01629 = 0.01535 -0.00038 0.00447 -0.00119 C29 1 0.278816 0.680537 0.192439 11.00000 0.01461 0.01759 = 0.01303 -0.00103 0.00129 -0.00366 AFIX 43 H29 2 0.342440 0.668758 0.164008 11.00000 -1.20000 AFIX 0 C32 1 0.088551 0.718771 0.274552 11.00000 0.01515 0.01802 = 0.01472 -0.00057 0.00055 -0.00072 AFIX 43 H32 2 0.024281 0.731496 0.302639 11.00000 -1.20000 AFIX 0 C43 1 -0.101220 0.323932 0.424025 11.00000 0.01840 0.02361 = 0.01823 -0.00035 0.00353 -0.00431 AFIX 43 H43 2 -0.128008 0.406157 0.424031 11.00000 -1.20000 AFIX 0 C15 1 0.804124 0.521487 0.122391 11.00000 0.01150 0.01728 = 0.01322 0.00157 -0.00112 -0.00156 C60 1 0.681318 0.207528 0.276857 11.00000 0.01503 0.01775 = 0.01738 -0.00314 0.00186 -0.00165 C61 1 0.575569 0.296733 0.286061 11.00000 0.01173 0.01769 = 0.01544 0.00135 0.00136 -0.00277 C6 1 0.412088 0.357673 0.128473 11.00000 0.01194 0.01518 = 0.01286 -0.00133 0.00054 -0.00151 C8 1 0.657304 0.365002 0.057869 11.00000 0.01013 0.02052 = 0.01229 -0.00480 0.00209 -0.00382 C26 1 0.638514 0.617822 0.212693 11.00000 0.01347 0.01354 = 0.01310 0.00145 -0.00206 -0.00314 C4 1 0.285729 0.265597 0.077611 11.00000 0.01803 0.01727 = 0.01530 -0.00266 -0.00322 -0.00247 AFIX 43 H4 2 0.273336 0.230029 0.045810 11.00000 -1.20000 AFIX 0 C5 1 0.393942 0.305028 0.081439 11.00000 0.01548 0.01679 = 0.01598 -0.00136 -0.00080 -0.00387 AFIX 43 H5 2 0.456161 0.296568 0.052267 11.00000 -1.20000 AFIX 0 C47 1 0.041080 0.156996 0.388375 11.00000 0.01643 0.01960 = 0.01750 0.00305 -0.00161 -0.00510 C18 1 1.042772 0.566161 0.110613 11.00000 0.01112 0.02601 = 0.02599 0.00279 0.00076 -0.00403 AFIX 43 H18 2 1.124457 0.578640 0.107521 11.00000 -1.20000 AFIX 0 C36 1 -0.137743 0.606301 0.358367 11.00000 0.01545 0.02216 = 0.01506 0.00225 0.00227 0.00047 AFIX 43 H36 2 -0.168146 0.571718 0.330276 11.00000 -1.20000 AFIX 0 C51 1 0.333431 0.017092 0.274891 11.00000 0.01816 0.01727 = 0.02133 -0.00183 -0.00212 -0.00135 AFIX 43 H51 2 0.396981 -0.014312 0.249206 11.00000 -1.20000 AFIX 0 C62 1 0.571893 0.377392 0.327074 11.00000 0.01478 0.02351 = 0.01764 -0.00222 -0.00666 0.00105 AFIX 43 H62 2 0.634555 0.365334 0.349110 11.00000 -1.20000 AFIX 0 C63 1 0.484132 0.473345 0.338048 11.00000 0.01582 0.01820 = 0.01015 0.00111 0.00070 -0.00311 C16 1 0.886705 0.477452 0.078460 11.00000 0.01174 0.02240 = 0.01575 0.00029 -0.00053 -0.00473 AFIX 43 H16 2 0.860954 0.431737 0.052696 11.00000 -1.20000 AFIX 0 C20 1 0.841667 0.595343 0.159020 11.00000 0.01367 0.01757 = 0.01476 0.00128 -0.00127 -0.00212 C68 1 0.561576 0.609553 0.462549 11.00000 0.01703 0.02306 = 0.01176 -0.00231 -0.00010 -0.00456 C19 1 0.963112 0.613220 0.152470 11.00000 0.01410 0.02229 = 0.02400 -0.00244 -0.00017 -0.00530 AFIX 43 H19 2 0.990910 0.659006 0.177610 11.00000 -1.20000 AFIX 0 C25 1 0.554350 0.679374 0.250722 11.00000 0.01529 0.01846 = 0.01361 -0.00074 -0.00115 -0.00270 AFIX 43 H25 2 0.475329 0.658688 0.257334 11.00000 -1.20000 AFIX 0 C59 1 0.780878 0.184630 0.307151 11.00000 0.01941 0.02983 = 0.02927 0.00572 0.00717 0.01811 AFIX 43 H59 2 0.790439 0.224625 0.338205 11.00000 -1.20000 AFIX 0 C10 1 0.672848 0.376293 -0.037805 11.00000 0.01640 0.04358 = 0.01179 0.00196 -0.00076 -0.00301 AFIX 43 H10 2 0.665882 0.420892 -0.070373 11.00000 -1.20000 AFIX 0 C37 1 -0.205701 0.698020 0.386666 11.00000 0.01689 0.02536 = 0.02127 0.00493 0.00601 0.00590 AFIX 43 H37 2 -0.283273 0.726680 0.377785 11.00000 -1.20000 AFIX 0 C55 1 -0.006407 0.250312 0.155004 11.00000 0.01523 0.02775 = 0.02636 0.00269 -0.00216 -0.00913 AFIX 137 H55A 2 -0.076712 0.222233 0.143546 11.00000 -1.50000 H55B 2 -0.025389 0.333734 0.163741 11.00000 -1.50000 H55C 2 0.016311 0.204084 0.186763 11.00000 -1.50000 AFIX 0 C64 1 0.486373 0.551086 0.384016 11.00000 0.01805 0.01849 = 0.01209 -0.00311 0.00148 -0.00369 C22 1 0.784100 0.743043 0.230848 11.00000 0.01541 0.02246 = 0.01972 0.00008 -0.00331 -0.00641 AFIX 43 H22 2 0.862308 0.765798 0.224331 11.00000 -1.20000 AFIX 0 C21 1 0.755408 0.650640 0.201774 11.00000 0.01402 0.01788 = 0.01243 0.00116 -0.00312 -0.00334 C40 1 0.021512 0.614510 0.413068 11.00000 0.02205 0.02207 = 0.01760 -0.00301 -0.00213 -0.00037 AFIX 43 H40 2 0.099166 0.586062 0.421909 11.00000 -1.20000 AFIX 0 C50 1 0.274744 -0.059018 0.312023 11.00000 0.02123 0.01622 = 0.02751 0.00197 -0.00495 -0.00368 AFIX 43 H50 2 0.299297 -0.141645 0.311716 11.00000 -1.20000 AFIX 0 C17 1 1.003473 0.500412 0.072919 11.00000 0.01305 0.02550 = 0.01931 0.00167 0.00184 -0.00229 AFIX 43 H17 2 1.057657 0.471210 0.043175 11.00000 -1.20000 AFIX 0 C24 1 0.585163 0.769190 0.278450 11.00000 0.02083 0.01728 = 0.01705 -0.00262 -0.00015 -0.00383 AFIX 43 H24 2 0.527752 0.809491 0.304301 11.00000 -1.20000 AFIX 0 C49 1 0.181714 -0.013357 0.348759 11.00000 0.01888 0.01909 = 0.02407 0.00439 -0.00112 -0.00405 AFIX 43 H49 2 0.142525 -0.065658 0.373443 11.00000 -1.20000 AFIX 0 C58 1 0.864735 0.089958 0.282381 11.00000 0.01689 0.02411 = 0.03218 -0.00508 -0.00684 0.00342 AFIX 43 H58 2 0.936484 0.058480 0.296337 11.00000 -1.20000 AFIX 0 C23 1 0.700635 0.801154 0.268646 11.00000 0.02222 0.01738 = 0.01990 -0.00121 -0.00461 -0.00789 AFIX 43 H23 2 0.721875 0.862887 0.287963 11.00000 -1.20000 AFIX 0 C13 1 0.695881 0.244737 0.057610 11.00000 0.02134 0.02129 = 0.01943 -0.00332 0.00093 -0.00124 AFIX 43 H13 2 0.704620 0.200817 0.090223 11.00000 -1.20000 AFIX 0 C31 1 0.113778 0.809993 0.237753 11.00000 0.02238 0.01303 = 0.01628 -0.00114 -0.00066 0.00085 AFIX 43 H31 2 0.066899 0.885048 0.240493 11.00000 -1.20000 AFIX 0 C39 1 -0.049329 0.706068 0.441105 11.00000 0.03328 0.02795 = 0.02134 -0.00899 -0.00032 -0.00127 AFIX 43 H39 2 -0.020049 0.739849 0.469731 11.00000 -1.20000 AFIX 0 C69 1 0.564810 0.527795 0.422646 11.00000 0.01902 0.02433 = 0.01319 -0.00436 0.00174 -0.00333 AFIX 43 H69 2 0.619606 0.457484 0.421879 11.00000 -1.20000 AFIX 0 C38 1 -0.161715 0.748069 0.427613 11.00000 0.03137 0.02180 = 0.02316 -0.00320 0.00838 0.00558 AFIX 43 H38 2 -0.208652 0.811354 0.446516 11.00000 -1.20000 AFIX 0 C44 1 -0.161530 0.248066 0.458881 11.00000 0.02023 0.02814 = 0.02295 0.00274 0.00591 -0.00593 AFIX 43 H44 2 -0.229637 0.278075 0.482538 11.00000 -1.20000 AFIX 0 C45 1 -0.121891 0.127125 0.459161 11.00000 0.02569 0.03013 = 0.02736 0.00744 0.00871 -0.00961 AFIX 43 H45 2 -0.163673 0.075032 0.482927 11.00000 -1.20000 AFIX 0 C56 1 0.173503 0.986224 0.158722 11.00000 0.03213 0.01370 = 0.02570 0.00197 -0.00248 -0.00038 AFIX 137 H56A 2 0.207037 1.035456 0.129032 11.00000 -1.50000 H56B 2 0.174671 1.023924 0.192742 11.00000 -1.50000 H56C 2 0.090873 0.976996 0.154190 11.00000 -1.50000 AFIX 0 C11 1 0.709893 0.255122 -0.039088 11.00000 0.02683 0.03997 = 0.01773 -0.01218 0.00048 0.00157 AFIX 43 H11 2 0.727217 0.217086 -0.072412 11.00000 -1.20000 AFIX 0 C12 1 0.721384 0.190053 0.008800 11.00000 0.03146 0.02676 = 0.02576 -0.00908 0.00044 0.00207 AFIX 43 H12 2 0.746889 0.107627 0.007927 11.00000 -1.20000 AFIX 0 C46 1 -0.022997 0.082944 0.425352 11.00000 0.02579 0.02274 = 0.02504 0.00538 0.00123 -0.00698 AFIX 43 H46 2 0.003254 0.000643 0.426736 11.00000 -1.20000 AFIX 0 C57 1 0.830453 0.050723 0.237189 11.00000 0.02869 0.02293 = 0.03417 -0.00401 0.00095 -0.00692 AFIX 43 H57 2 0.876436 -0.009559 0.216026 11.00000 -1.20000 AFIX 0 C70 1 0.651701 0.582576 0.500972 11.00000 0.02490 0.02771 = 0.02209 -0.00243 -0.00166 -0.00554 C67 1 0.482614 0.711350 0.463880 11.00000 0.02176 0.02447 = 0.02124 -0.00014 0.00165 -0.00289 AFIX 43 H67 2 0.483403 0.766331 0.490864 11.00000 -1.20000 AFIX 0 C71 1 0.734866 0.651603 0.572255 11.00000 0.03505 0.03698 = 0.03016 -0.00401 -0.01418 -0.00272 AFIX 137 H71A 2 0.813940 0.636235 0.551336 11.00000 -1.50000 H71B 2 0.721389 0.584537 0.597094 11.00000 -1.50000 H71C 2 0.730920 0.723120 0.592623 11.00000 -1.50000 AFIX 0 C66 1 0.402213 0.735713 0.427007 11.00000 0.02838 0.02591 = 0.02386 -0.00189 -0.00040 0.00062 AFIX 43 H66 2 0.346593 0.805464 0.428510 11.00000 -1.20000 AFIX 0 C02I 1 0.535854 0.919226 0.601042 11.00000 0.04492 0.04141 = 0.02975 -0.00276 -0.00364 -0.00399 AFIX 23 H02A 2 0.521624 0.835821 0.600175 11.00000 -1.20000 H02B 2 0.577410 0.927638 0.632612 11.00000 -1.20000 AFIX 0 C02J 1 0.546517 0.866754 0.133807 11.00000 0.04355 0.04025 = 0.05621 0.01369 -0.01060 -0.00539 AFIX 23 H02E 2 0.478042 0.835066 0.155587 11.00000 -1.20000 H02F 2 0.613284 0.859548 0.155908 11.00000 -1.20000 AFIX 0 C02K 1 0.019442 0.128454 -0.060877 11.00000 0.07953 0.06667 = 0.04055 -0.00730 -0.01588 0.01017 AFIX 23 H02C 2 -0.011254 0.201927 -0.079757 11.00000 -1.20000 H02D 2 -0.045091 0.077081 -0.055375 11.00000 -1.20000 AFIX 0 PART -1 O0AA 6 0.503562 0.967891 0.019839 10.27000 0.02931 AFIX 3 H0AA 2 0.461152 0.980631 0.049839 10.27000 -1.50000 H0AB 2 0.530012 0.894971 0.021489 10.27000 -1.50000 AFIX 0 HKLF 4 REM st38_p-1_a.res in P-1 REM wR2 = 0.1028, GooF = S = 1.043, Restrained GooF = 1.043 for all data REM R1 = 0.0427 for 16922 Fo > 4sig(Fo) and 0.0531 for all 19375 data REM 836 parameters refined using 0 restraints END WGHT 0.0412 9.7269 REM Highest difference peak 1.909, deepest hole -1.509, 1-sigma level 0.149 Q1 1 0.3423 0.4943 0.2492 11.00000 0.05 1.91 Q2 1 0.1123 0.0613 -0.1403 11.00000 0.05 1.83 Q3 1 0.6270 0.8679 0.5496 11.00000 0.05 1.74 Q4 1 0.7736 0.0629 0.2062 11.00000 0.05 1.64 Q5 1 0.2952 -0.0124 -0.1285 11.00000 0.05 1.64 ; _shelx_res_checksum 97495 _shelx_hkl_file ; -1 0 0 0.20 0.40 1 0 0 -0.20 0.10 -2 0 0 1.50 1.60 -2 0 0 3.00 2.40 2 0 0 3.90 1.90 -3 0 0 1101.29 28.30 -3 0 0 1070.99 27.90 3 0 0 1093.49 28.00 -4 0 0 1344.27 35.10 -4 0 0 1356.76 34.70 4 0 0 1318.37 34.70 -5 0 0 361.26 13.30 -5 0 0 368.96 12.40 5 0 0 359.46 12.70 -6 0 0 719.33 20.50 -6 0 0 718.03 21.40 6 0 0 720.43 21.00 6 0 0 577.44 20.50 -7 0 0 492.75 16.90 -7 0 0 470.25 15.70 7 0 0 491.15 16.40 7 0 0 433.66 16.30 -8 0 0 609.64 19.90 -8 0 0 647.94 21.10 8 0 0 580.74 20.70 8 0 0 637.24 23.90 -9 0 0 173.78 10.00 9 0 0 175.98 11.00 9 0 0 163.58 10.90 -10 0 0 39.30 7.70 10 0 0 36.50 7.20 10 0 0 40.30 7.30 -11 0 0 102.19 11.10 11 0 0 88.29 10.00 -12 0 0 126.29 12.80 12 0 0 125.49 12.30 -13 0 0 47.00 9.60 -14 0 0 378.56 20.00 14 0 0 362.36 20.20 -15 0 0 200.58 16.70 15 0 0 200.88 17.10 15 -1 0 182.68 16.40 -15 1 0 162.58 17.10 14 -1 0 164.58 15.20 -14 1 0 162.68 16.30 13 -1 0 -6.70 7.00 -13 1 0 2.20 7.90 12 -1 0 142.99 12.60 -12 1 0 139.49 14.10 11 -1 0 452.25 19.00 -11 1 0 462.75 20.90 10 -1 0 76.99 8.80 -10 1 0 89.19 10.40 -10 1 0 84.49 9.70 9 -1 0 56.79 7.50 9 -1 0 34.80 7.20 -9 1 0 54.19 8.70 -9 1 0 51.19 6.30 8 -1 0 513.75 17.70 8 -1 0 493.05 18.80 -8 1 0 504.35 17.00 7 -1 0 879.01 25.50 7 -1 0 854.91 26.90 -7 1 0 895.51 27.30 -7 1 0 852.71 24.90 6 -1 0 224.18 9.60 6 -1 0 200.78 10.70 -6 1 0 210.68 11.30 -6 1 0 212.38 9.00 5 -1 0 454.45 14.50 5 -1 0 447.06 16.00 -5 1 0 448.96 14.10 -5 1 0 443.66 16.30 4 -1 0 238.08 9.70 4 -1 0 226.58 8.20 -4 1 0 222.28 7.90 -4 1 0 232.78 9.90 3 -1 0 214.48 8.20 3 -1 0 200.58 6.80 -3 1 0 214.78 8.40 -3 1 0 194.18 6.70 2 -1 0 254.97 8.90 2 -1 0 266.77 8.10 -2 1 0 258.07 9.10 -2 1 0 254.67 7.50 1 -1 0 2846.62 68.39 1 -1 0 2817.22 69.39 -1 1 0 2895.61 69.59 -1 1 0 2840.22 68.39 -1 -1 0 47.70 2.30 1 1 0 57.59 2.80 -2 -1 0 10.80 2.40 2 1 0 11.20 2.30 -3 -1 0 4355.56 103.59 -3 -1 0 4192.78 104.19 3 1 0 4280.27 103.49 3 1 0 4300.07 104.39 -4 -1 0 1281.57 33.50 -4 -1 0 1289.37 32.70 4 1 0 1295.67 33.00 4 1 0 1259.67 33.60 -5 -1 0 173.08 8.70 -5 -1 0 197.68 8.50 5 1 0 197.88 8.70 5 1 0 189.98 9.20 -6 -1 0 1461.85 37.90 -6 -1 0 1403.86 38.40 6 1 0 1437.76 38.80 6 1 0 1416.56 38.10 -7 -1 0 746.33 22.00 -7 -1 0 715.53 22.20 7 1 0 718.33 22.10 7 1 0 745.73 22.90 -8 -1 0 261.27 11.60 8 1 0 245.38 11.40 8 1 0 253.37 12.10 -9 -1 0 117.39 8.70 -9 -1 0 115.89 9.30 9 1 0 91.39 8.60 9 1 0 120.59 9.80 -10 -1 0 691.43 30.30 10 1 0 539.35 20.70 10 1 0 589.74 22.10 -11 -1 0 245.08 13.80 11 1 0 287.37 15.40 11 1 0 237.78 13.30 -12 -1 0 9.10 6.70 12 1 0 5.20 6.60 -13 -1 0 441.26 19.40 13 1 0 410.26 20.80 -14 -1 0 257.17 16.20 14 1 0 253.47 17.70 -15 -1 0 93.39 11.50 15 1 0 85.09 12.70 -16 -1 0 16.70 8.60 16 1 0 11.00 10.50 15 -2 0 103.99 13.40 -15 2 0 127.99 15.60 14 -2 0 6.80 8.20 -14 2 0 -5.70 8.90 13 -2 0 94.69 11.10 -13 2 0 73.39 12.90 12 -2 0 308.87 16.40 -12 2 0 313.77 19.50 11 -2 0 136.49 11.40 -11 2 0 164.48 14.70 10 -2 0 89.49 9.40 -10 2 0 87.79 8.10 -10 2 0 87.99 11.20 9 -2 0 460.05 17.30 9 -2 0 436.36 21.50 -9 2 0 468.75 20.30 8 -2 0 1602.34 43.30 8 -2 0 1587.64 45.90 -8 2 0 1553.34 42.70 -8 2 0 1647.74 46.60 7 -2 0 347.27 15.20 7 -2 0 376.76 13.40 -7 2 0 369.56 12.80 6 -2 0 28.80 5.50 6 -2 0 30.70 4.40 -6 2 0 29.50 4.20 -6 2 0 43.00 7.40 5 -2 0 639.84 18.60 5 -2 0 626.24 21.00 -5 2 0 668.13 21.80 -5 2 0 625.84 18.20 4 -2 0 1399.66 35.50 4 -2 0 1354.46 37.90 -4 2 0 1396.36 38.20 -4 2 0 1391.66 35.30 3 -2 0 648.94 19.20 3 -2 0 621.14 16.90 -3 2 0 650.83 19.40 -3 2 0 626.44 16.80 2 -2 0 621.94 16.00 2 -2 0 620.84 18.00 -2 2 0 606.04 15.90 1 -2 0 4656.43 115.39 1 -2 0 4899.11 114.09 1 -2 0 4646.73 113.89 -1 2 0 4782.82 115.59 0 -2 0 895.21 23.70 0 2 0 944.91 23.80 -1 -2 0 19.50 2.20 -1 -2 0 19.80 2.60 1 2 0 23.00 2.80 1 2 0 22.90 2.40 -2 -2 0 10.20 2.50 2 2 0 21.90 3.30 -3 -2 0 22.50 3.50 3 2 0 24.80 3.50 -4 -2 0 1017.10 27.70 4 2 0 1020.40 28.00 -5 -2 0 139.99 8.10 -5 -2 0 137.09 6.60 5 2 0 135.79 8.40 5 2 0 135.09 6.70 -6 -2 0 2074.49 53.79 -6 -2 0 2072.99 51.79 6 2 0 2039.90 52.19 6 2 0 2042.40 54.09 -7 -2 0 595.94 19.70 -7 -2 0 606.04 18.20 7 2 0 623.94 18.60 7 2 0 624.04 22.20 -8 -2 0 279.27 11.10 -8 -2 0 262.37 12.20 8 2 0 255.87 11.00 8 2 0 278.17 13.00 -9 -2 0 13.60 4.70 9 2 0 11.70 5.70 9 2 0 19.70 5.10 -10 -2 0 543.15 18.90 10 2 0 517.95 18.90 10 2 0 559.44 21.50 -11 -2 0 135.39 16.30 11 2 0 127.19 11.90 11 2 0 118.09 9.40 -12 -2 0 12.70 6.20 12 2 0 4.70 7.00 12 2 0 -0.80 5.20 -13 -2 0 374.46 16.50 13 2 0 305.27 17.50 13 2 0 351.76 19.40 -14 -2 0 202.18 13.60 14 2 0 207.08 16.80 -15 -2 0 50.99 8.80 15 2 0 41.80 11.20 -16 -2 0 20.90 10.20 16 2 0 2.90 16.20 15 -3 0 103.49 12.80 14 -3 0 9.70 8.10 -14 3 0 8.20 9.50 13 -3 0 314.87 17.30 -13 3 0 316.27 21.40 12 -3 0 576.84 22.40 -12 3 0 593.94 31.00 11 -3 0 38.10 7.40 -11 3 0 46.30 10.80 10 -3 0 75.99 8.20 -10 3 0 65.99 10.70 -10 3 0 71.19 7.80 9 -3 0 456.95 16.60 -9 3 0 410.16 20.30 -9 3 0 429.96 15.60 8 -3 0 299.27 12.50 8 -3 0 283.27 15.10 -8 3 0 300.87 11.80 -8 3 0 301.57 16.30 7 -3 0 9.80 4.10 7 -3 0 5.80 5.40 -7 3 0 5.90 3.30 -7 3 0 1.50 5.60 6 -3 0 432.46 17.40 6 -3 0 452.25 14.70 -6 3 0 483.85 14.50 5 -3 0 459.35 17.60 5 -3 0 484.15 14.70 -5 3 0 492.65 14.50 -5 3 0 482.75 18.60 4 -3 0 73.69 5.50 4 -3 0 75.89 8.10 -4 3 0 99.19 9.60 -4 3 0 88.59 5.40 3 -3 0 2.90 3.70 3 -3 0 2.80 2.30 -3 3 0 4.60 4.50 -3 3 0 2.60 2.10 2 -3 0 788.62 22.60 2 -3 0 765.32 20.00 -2 3 0 783.22 22.90 1 -3 0 115.89 6.20 1 -3 0 130.39 5.10 -1 3 0 123.99 6.50 0 -3 0 4.00 1.80 0 -3 0 9.00 2.70 0 3 0 9.00 2.40 0 3 0 8.10 2.70 -1 -3 0 907.81 24.50 -1 -3 0 924.51 23.80 1 3 0 946.01 23.90 1 3 0 923.51 24.60 -2 -3 0 1266.67 32.90 2 3 0 1251.67 32.90 -3 -3 0 1940.31 49.90 3 3 0 1966.00 50.09 -4 -3 0 78.69 6.30 4 3 0 77.09 6.80 -5 -3 0 1392.16 38.50 5 3 0 1443.26 39.00 -6 -3 0 470.75 16.50 6 3 0 479.65 17.10 7 3 0 77.59 7.80 -8 -3 0 143.09 7.40 -8 -3 0 129.39 9.20 8 3 0 139.89 10.30 -9 -3 0 720.53 21.20 9 3 0 695.63 24.80 -10 -3 0 273.77 11.80 10 3 0 302.77 15.50 10 3 0 246.08 11.40 -11 -3 0 8.00 5.00 11 3 0 -3.10 4.00 11 3 0 -1.50 6.40 -12 -3 0 10.30 5.40 12 3 0 5.50 5.10 -13 -3 0 320.17 14.70 13 3 0 365.16 19.80 -14 -3 0 174.88 11.60 14 3 0 158.08 15.70 15 3 0 19.10 10.20 16 3 0 25.90 11.10 14 -4 0 64.09 17.30 -14 4 0 25.70 11.80 13 -4 0 155.48 13.50 -13 4 0 163.98 19.60 12 -4 0 158.98 12.30 -12 4 0 131.09 15.30 11 -4 0 26.70 6.90 -11 4 0 29.00 18.20 10 -4 0 681.83 22.40 -10 4 0 667.33 27.90 -10 4 0 601.94 20.90 -9 4 0 497.65 22.80 -9 4 0 460.25 16.40 8 -4 0 150.88 9.00 -8 4 0 139.69 13.40 -8 4 0 140.19 8.10 7 -4 0 1.00 5.00 7 -4 0 1.40 3.70 -7 4 0 3.40 3.30 -7 4 0 10.10 6.20 6 -4 0 406.86 13.30 6 -4 0 390.56 16.80 -6 4 0 409.86 13.10 -6 4 0 420.06 18.10 5 -4 0 437.76 13.60 5 -4 0 445.26 17.30 -5 4 0 449.76 13.60 4 -4 0 196.58 11.10 4 -4 0 207.28 7.90 -4 4 0 210.68 12.30 -4 4 0 205.48 7.80 3 -4 0 1202.28 30.70 3 -4 0 1179.38 34.20 -3 4 0 1202.38 34.80 2 -4 0 1509.95 40.60 2 -4 0 1442.76 37.50 2 -4 0 1525.75 37.90 -2 4 0 1515.85 41.10 1 -4 0 860.11 22.20 1 -4 0 811.92 23.70 -1 4 0 827.12 24.00 -1 4 0 795.42 21.90 0 -4 0 406.16 13.30 0 -4 0 405.66 12.70 0 4 0 430.56 12.90 0 4 0 428.46 13.60 -1 -4 0 8.30 2.80 -1 -4 0 12.40 2.70 1 4 0 11.30 3.00 1 4 0 15.10 3.40 -2 -4 0 326.07 9.70 -2 -4 0 331.67 11.60 2 4 0 340.07 10.10 2 4 0 323.07 11.60 -3 -4 0 106.19 7.10 3 4 0 115.59 7.60 -4 -4 0 206.88 10.00 4 4 0 201.78 10.40 -5 -4 0 95.19 7.70 5 4 0 73.89 7.70 -6 -4 0 712.63 22.70 -7 -4 0 24.40 5.30 7 4 0 16.90 5.00 8 4 0 8.50 5.10 9 4 0 42.90 7.50 10 4 0 21.30 7.70 11 4 0 3.80 7.10 12 4 0 483.25 22.50 13 4 0 234.38 17.20 14 4 0 73.39 11.60 15 4 0 85.49 13.90 14 -5 0 95.19 11.70 -14 5 0 84.79 18.70 13 -5 0 280.67 15.90 -13 5 0 254.97 21.60 12 -5 0 109.39 10.70 -12 5 0 123.69 16.80 11 -5 0 19.00 6.60 -11 5 0 16.40 6.10 -11 5 0 24.50 9.80 10 -5 0 300.77 13.70 -10 5 0 272.27 19.40 -10 5 0 268.27 12.30 9 -5 0 238.48 11.90 -9 5 0 219.88 10.70 -9 5 0 232.38 17.30 8 -5 0 71.19 7.00 -8 5 0 70.39 6.60 -8 5 0 75.49 11.50 7 -5 0 664.23 19.90 -7 5 0 649.74 19.60 -7 5 0 644.24 25.80 6 -5 0 558.64 21.80 6 -5 0 603.14 17.60 -6 5 0 590.04 17.40 -6 5 0 554.44 22.80 5 -5 0 305.47 14.50 5 -5 0 322.87 10.80 -5 5 0 314.37 15.50 -5 5 0 314.57 10.60 4 -5 0 210.38 8.00 4 -5 0 203.38 11.40 3 -5 0 911.31 24.80 3 -5 0 958.90 25.20 3 -5 0 903.61 28.50 -3 5 0 979.60 29.70 2 -5 0 1513.25 42.20 2 -5 0 1558.94 39.50 2 -5 0 1492.85 38.90 -2 5 0 1570.14 43.00 1 -5 0 127.09 8.80 1 -5 0 118.89 7.30 -1 5 0 121.59 9.30 -1 5 0 109.49 6.70 0 -5 0 184.48 9.40 0 -5 0 178.88 10.10 0 5 0 195.68 8.90 0 5 0 205.78 10.00 -1 -5 0 1344.17 36.30 1 5 0 1394.76 36.90 1 5 0 1396.56 36.70 -2 -5 0 716.73 19.80 -2 -5 0 694.53 21.60 2 5 0 743.13 20.30 2 5 0 713.33 21.80 -3 -5 0 24.80 5.20 3 5 0 19.90 5.10 -4 -5 0 393.96 14.80 4 5 0 391.26 15.10 -5 -5 0 1895.31 51.19 5 5 0 1915.21 51.49 -6 -5 0 167.08 9.80 6 5 0 173.18 10.20 -7 -5 0 10.20 4.90 7 5 0 16.20 5.30 8 5 0 324.87 15.70 9 5 0 329.77 16.50 10 5 0 -5.40 6.10 11 5 0 29.10 9.60 12 5 0 243.28 16.60 13 5 0 115.09 13.50 14 5 0 27.80 9.80 15 5 0 209.98 25.50 14 -6 0 184.28 15.20 -14 6 0 184.78 23.00 13 -6 0 114.19 11.90 -13 6 0 64.79 14.20 12 -6 0 37.50 7.90 -12 6 0 60.09 13.30 11 -6 0 175.58 11.50 -11 6 0 167.68 18.30 -11 6 0 142.39 9.80 10 -6 0 544.35 18.80 -10 6 0 485.15 25.50 -10 6 0 489.55 20.30 9 -6 0 221.18 11.30 -9 6 0 214.98 17.60 -9 6 0 220.98 10.50 8 -6 0 25.10 5.20 -8 6 0 23.20 9.70 -8 6 0 19.90 4.50 7 -6 0 9.50 4.20 -7 6 0 5.30 7.40 -7 6 0 14.00 4.00 6 -6 0 957.00 26.60 -6 6 0 983.30 33.60 5 -6 0 57.79 7.70 5 -6 0 63.69 5.50 5 -6 0 56.29 5.40 -5 6 0 59.39 9.70 4 -6 0 304.57 10.40 4 -6 0 303.97 11.40 4 -6 0 295.47 14.20 -4 6 0 313.87 15.40 3 -6 0 228.88 8.70 3 -6 0 214.48 11.70 -3 6 0 261.07 15.20 2 -6 0 270.77 9.90 2 -6 0 268.27 12.70 -2 6 0 276.17 13.50 1 -6 0 64.79 6.20 1 -6 0 73.29 7.40 -1 6 0 60.39 5.80 -1 6 0 72.39 8.10 0 -6 0 88.29 7.10 0 -6 0 75.49 7.40 0 6 0 89.39 6.80 0 6 0 84.59 8.10 -1 -6 0 176.38 8.90 1 6 0 172.88 9.30 1 6 0 178.78 9.40 -2 -6 0 46.10 4.90 -2 -6 0 44.90 5.70 2 6 0 45.20 5.40 2 6 0 38.10 5.90 -3 -6 0 163.78 9.50 -3 -6 0 180.98 7.10 3 6 0 178.98 9.80 -4 -6 0 492.55 17.60 4 6 0 508.85 18.00 5 6 0 513.85 18.80 -6 -6 0 56.79 7.10 6 6 0 42.40 6.80 7 6 0 261.57 13.90 8 6 0 636.84 23.90 9 6 0 146.89 12.60 10 6 0 7.90 6.80 11 6 0 317.67 18.30 12 6 0 403.06 21.40 13 6 0 149.99 15.80 14 6 0 62.59 12.20 15 6 0 189.88 18.80 13 -7 0 102.69 11.30 -13 7 0 97.79 18.20 12 -7 0 49.20 7.80 -12 7 0 38.20 13.70 11 -7 0 234.98 12.60 -11 7 0 181.78 19.30 10 -7 0 207.58 11.50 -10 7 0 181.68 18.30 -10 7 0 186.78 11.80 9 -7 0 27.60 5.50 -9 7 0 5.90 8.40 8 -7 0 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132.59 19.40 0 -3 -32 109.39 14.80 0 3 32 115.79 15.50 -1 -3 -32 45.30 11.40 1 3 32 39.60 10.60 -2 -3 -32 22.80 9.30 2 3 32 20.20 10.20 -3 -3 -32 85.99 12.70 3 3 32 89.69 14.40 -4 -3 -32 176.08 16.10 -5 -3 -32 26.80 9.20 -5 -3 -32 30.90 10.10 -6 -3 -32 184.78 16.40 -6 -3 -32 227.98 18.10 -7 -3 -32 149.99 16.70 -7 -3 -32 152.98 15.20 -8 -3 -32 67.09 12.20 -8 -3 -32 74.69 12.80 -9 -3 -32 39.90 10.90 -9 -3 -32 47.10 11.40 3 -4 -32 53.59 13.10 -3 4 32 18.90 12.60 2 -4 -32 108.19 14.60 -2 4 32 115.49 15.40 -1 4 32 106.19 21.70 0 -4 -32 60.29 12.10 0 4 32 50.49 12.70 -1 -4 -32 20.30 9.80 1 4 32 22.60 10.20 -2 -4 -32 163.38 16.90 2 4 32 146.59 17.20 -3 -4 -32 90.29 13.80 3 4 32 95.49 14.80 -4 -4 -32 22.10 9.80 4 4 32 55.59 12.10 -5 -4 -32 114.59 14.60 -6 -4 -32 47.00 12.00 -6 -4 -32 49.10 11.00 -7 -4 -32 77.19 12.10 -7 -4 -32 60.49 12.80 -8 -4 -32 7.70 8.40 -8 -4 -32 -11.40 9.70 3 -5 -32 55.19 13.70 -3 5 32 38.00 12.90 2 -5 -32 117.99 15.70 -2 5 32 107.39 15.60 1 -5 -32 29.30 11.50 -1 5 32 26.70 10.80 0 -5 -32 17.00 12.10 -1 -5 -32 52.29 14.60 1 5 32 72.49 13.30 -2 -5 -32 125.09 15.50 2 5 32 141.89 17.30 -3 -5 -32 103.69 15.80 3 5 32 145.79 17.10 -4 -5 -32 2.40 9.50 4 5 32 -8.80 8.80 -5 -5 -32 89.69 14.00 -6 -5 -32 171.28 16.00 -6 -5 -32 184.08 18.30 -7 -5 -32 132.99 18.60 -7 -5 -32 178.68 16.80 -8 -5 -32 14.60 8.70 2 -6 -32 177.88 23.30 -2 6 32 194.88 20.20 1 -6 -32 56.69 14.10 -1 6 32 76.69 15.80 0 -6 -32 56.59 13.80 0 6 32 41.10 12.70 -1 -6 -32 106.09 15.50 -2 -6 -32 130.79 16.20 2 6 32 135.69 16.80 -3 -6 -32 21.10 12.00 3 6 32 48.60 12.40 -4 -6 -32 2.20 13.40 4 6 32 -0.50 9.70 -5 -6 -32 138.19 18.00 5 6 32 162.78 17.30 -6 -6 -32 63.79 14.40 -7 -6 -32 15.60 8.90 -7 -6 -32 4.70 11.90 -1 7 32 47.50 14.30 0 -7 -32 17.20 11.40 0 7 32 25.40 11.30 -1 -7 -32 136.39 17.80 1 7 32 167.18 18.60 -2 -7 -32 204.08 20.90 2 7 32 264.57 31.60 -3 -7 -32 -2.30 10.30 3 7 32 4.10 9.60 -4 -7 -32 42.60 14.30 4 7 32 42.50 12.20 -5 -7 -32 187.98 20.40 5 7 32 225.68 18.90 -6 -7 -32 162.18 20.60 2 8 32 29.30 11.70 -3 -8 -32 27.00 21.20 3 8 32 36.50 17.20 -4 -8 -32 157.18 23.80 4 8 32 238.98 20.00 1 5 -33 71.69 16.80 1 5 -33 65.29 10.60 0 5 -33 73.59 10.50 0 5 -33 75.09 13.50 -1 5 -33 166.88 13.50 -1 5 -33 145.29 17.10 -2 5 -33 64.19 9.10 -2 5 -33 65.69 12.90 -3 5 -33 20.20 6.60 2 4 -33 41.00 10.00 2 4 -33 22.80 10.30 1 4 -33 -6.50 7.10 1 4 -33 3.60 8.90 0 4 -33 136.49 16.10 0 4 -33 125.39 13.20 -1 4 -33 325.67 18.20 -1 4 -33 352.96 22.80 -2 4 -33 26.80 8.20 -2 4 -33 14.20 10.10 -3 4 -33 18.60 9.80 -4 4 -33 243.28 14.30 -4 4 -33 230.78 20.00 -5 4 -33 125.19 17.10 -3 -3 33 124.39 16.60 2 3 -33 83.19 12.00 1 3 -33 24.80 10.30 1 3 -33 32.50 9.50 0 3 -33 218.38 16.30 0 3 -33 171.28 18.00 -1 3 -33 86.69 10.80 -1 3 -33 53.39 11.70 -2 3 -33 6.60 7.50 -2 3 -33 17.70 8.80 -3 3 -33 8.10 7.30 -3 3 -33 8.70 9.60 -4 3 -33 145.49 15.00 -4 3 -33 152.58 17.40 -5 3 -33 37.40 8.00 -5 3 -33 27.20 10.90 -6 3 -33 18.20 10.30 4 2 -33 269.67 19.80 -4 -2 33 239.68 33.20 3 2 -33 170.58 24.80 -3 -2 33 190.08 20.00 2 2 -33 13.40 8.90 -2 -2 33 2.30 8.70 1 2 -33 287.67 18.30 0 2 -33 272.17 17.40 -1 2 -33 148.69 16.50 -1 2 -33 130.59 13.90 -2 2 -33 19.10 7.60 -2 2 -33 44.90 12.50 -3 2 -33 91.49 11.40 -3 2 -33 115.49 15.10 -4 2 -33 89.69 10.70 -4 2 -33 93.39 14.80 -5 2 -33 7.00 9.70 -6 2 -33 104.39 11.10 -6 2 -33 100.29 15.70 -7 2 -33 121.99 16.70 -7 2 -33 117.99 13.30 4 1 -33 183.68 18.10 -4 -1 33 178.88 22.50 3 1 -33 13.00 10.10 -3 -1 33 17.60 10.80 2 1 -33 49.80 11.00 -2 -1 33 31.60 12.30 1 1 -33 203.38 16.90 -1 -1 33 227.98 20.10 0 1 -33 80.29 11.90 0 -1 33 79.49 13.80 -1 1 -33 24.20 8.80 -2 1 -33 62.09 10.70 -2 1 -33 44.50 18.30 -3 1 -33 117.99 12.80 -4 1 -33 227.78 32.60 -4 1 -33 189.48 14.90 -5 1 -33 10.60 7.60 -5 1 -33 12.80 12.50 -6 1 -33 150.98 18.10 -6 1 -33 150.68 13.40 -7 1 -33 112.49 16.60 -7 1 -33 61.89 9.90 4 0 -33 228.38 19.10 -4 0 33 190.18 24.80 3 0 -33 -6.70 8.70 -3 0 33 0.80 10.00 2 0 -33 132.79 15.40 -2 0 33 134.59 18.20 1 0 -33 144.49 15.50 -1 0 33 126.89 16.20 0 0 -33 74.89 11.50 -1 0 -33 23.00 8.60 1 0 33 28.10 12.70 -2 0 -33 34.10 9.60 -3 0 -33 272.07 19.80 -3 0 -33 252.87 17.20 -4 0 -33 41.40 9.90 -4 0 -33 37.80 10.70 -5 0 -33 71.79 16.80 -5 0 -33 66.39 11.00 -6 0 -33 105.99 12.30 -6 0 -33 116.79 25.90 -7 0 -33 41.80 9.70 -7 0 -33 57.69 12.90 -8 0 -33 1.00 7.10 -8 0 -33 4.90 10.10 4 -1 -33 72.99 14.50 3 -1 -33 80.49 12.60 -3 1 33 77.19 13.80 -2 1 33 162.38 18.50 1 -1 -33 112.89 14.70 -1 1 33 112.59 17.50 0 -1 -33 9.30 8.60 -1 -1 -33 69.19 11.60 1 1 33 65.79 14.20 -2 -1 -33 322.27 19.60 2 1 33 343.27 22.70 -3 -1 -33 4.30 8.30 -4 -1 -33 6.80 8.50 -4 -1 -33 -7.90 8.10 -5 -1 -33 69.79 11.20 -5 -1 -33 75.59 12.90 -6 -1 -33 257.57 20.60 -6 -1 -33 253.27 17.00 -7 -1 -33 2.30 7.90 -7 -1 -33 -3.50 14.40 -8 -1 -33 18.10 10.80 -8 -1 -33 10.50 8.60 4 -2 -33 5.00 12.40 3 -2 -33 99.79 15.10 -3 2 33 124.79 17.90 2 -2 -33 188.18 17.90 -2 2 33 207.78 19.50 1 -2 -33 74.89 13.00 -1 2 33 87.19 15.30 0 -2 -33 29.20 10.20 -1 -2 -33 98.69 14.40 1 2 33 83.09 14.80 -2 -2 -33 100.29 13.20 2 2 33 120.39 16.50 -3 -2 -33 19.90 9.10 -4 -2 -33 43.60 10.30 -4 -2 -33 56.89 11.90 -5 -2 -33 83.19 12.30 -5 -2 -33 126.69 16.30 -6 -2 -33 62.69 12.20 -6 -2 -33 45.10 10.40 -7 -2 -33 14.50 9.00 -7 -2 -33 17.90 9.80 -8 -2 -33 18.10 9.30 -8 -2 -33 20.70 16.70 3 -3 -33 179.48 19.30 -3 3 33 151.38 19.20 2 -3 -33 384.86 23.70 -2 3 33 362.56 24.70 1 -3 -33 77.99 13.20 -1 3 33 97.39 15.10 0 -3 -33 11.50 9.90 0 3 33 37.00 12.00 -1 -3 -33 330.27 21.40 1 3 33 376.76 28.40 -2 -3 -33 163.98 16.60 2 3 33 129.69 17.90 -3 -3 -33 7.70 9.30 3 3 33 9.00 9.90 -4 -3 -33 293.07 19.60 -5 -3 -33 230.88 17.80 -5 -3 -33 228.48 18.70 -6 -3 -33 30.90 11.30 -6 -3 -33 16.00 10.20 -7 -3 -33 22.70 10.40 -7 -3 -33 -7.20 8.30 -8 -3 -33 147.59 15.50 -8 -3 -33 139.59 16.90 2 -4 -33 22.30 11.20 -2 4 33 39.00 11.80 1 -4 -33 -6.00 10.20 -1 4 33 16.70 10.80 0 -4 -33 36.20 12.30 0 4 33 54.09 12.30 -1 -4 -33 202.48 23.80 -2 -4 -33 27.20 10.50 2 4 33 23.00 11.10 -3 -4 -33 32.80 11.30 3 4 33 59.19 13.00 -4 -4 -33 174.18 17.60 4 4 33 213.08 19.40 -5 -4 -33 122.19 15.40 -6 -4 -33 28.80 11.30 -6 -4 -33 -2.20 8.50 -7 -4 -33 62.39 12.70 -7 -4 -33 64.79 12.00 -2 5 33 114.49 24.10 1 -5 -33 3.10 10.80 -1 5 33 32.20 10.90 0 -5 -33 268.47 21.70 0 5 33 283.27 22.20 -1 -5 -33 67.79 13.40 1 5 33 106.89 15.80 -2 -5 -33 5.90 10.30 -3 -5 -33 117.19 21.10 3 5 33 131.39 16.80 4 5 33 121.29 16.10 -5 -5 -33 37.80 15.60 -6 -5 -33 12.60 12.60 -6 -5 -33 6.40 8.10 -7 -5 -33 30.50 10.30 -7 -5 -33 25.40 11.70 -1 6 33 57.69 14.20 0 -6 -33 70.59 14.50 0 6 33 92.69 15.10 -1 -6 -33 40.90 12.20 1 6 33 18.00 10.80 -2 -6 -33 12.60 11.00 2 6 33 39.60 12.30 -3 -6 -33 232.68 20.80 3 6 33 265.87 32.30 -4 -6 -33 78.99 14.50 4 6 33 113.49 16.20 -5 -6 -33 42.10 12.60 -6 -6 -33 76.59 13.00 -6 -6 -33 111.29 16.70 1 7 33 35.70 12.20 -2 -7 -33 97.29 20.70 2 7 33 162.88 19.30 -3 -7 -33 94.19 16.00 3 7 33 130.89 18.40 -4 -7 -33 65.49 15.50 4 7 33 62.79 21.30 0 4 -34 128.09 13.30 -1 4 -34 40.60 9.70 -1 4 -34 33.30 16.10 -2 4 -34 108.69 11.80 -3 4 -34 174.28 13.80 2 3 -34 195.78 25.30 1 3 -34 158.08 18.50 1 3 -34 167.98 16.00 0 3 -34 13.20 8.40 0 3 -34 -1.00 9.40 -1 3 -34 90.29 14.30 -1 3 -34 125.99 13.50 -2 3 -34 144.39 16.80 -2 3 -34 182.58 14.30 -3 3 -34 88.59 11.20 -3 3 -34 88.79 14.50 -4 3 -34 93.19 10.90 -4 3 -34 92.19 14.10 -5 3 -34 207.38 16.50 -2 -2 34 242.98 25.00 1 2 -34 41.70 9.60 0 2 -34 41.40 11.00 -1 2 -34 186.98 15.40 -1 2 -34 183.18 18.40 -2 2 -34 97.59 12.30 -2 2 -34 90.99 14.40 -3 2 -34 8.00 7.30 -3 2 -34 16.80 10.20 -4 2 -34 83.29 13.90 -4 2 -34 77.09 10.50 -5 2 -34 254.07 15.70 -5 2 -34 272.47 21.80 -6 2 -34 54.19 9.20 -6 2 -34 54.19 13.70 3 1 -34 151.48 16.80 2 1 -34 200.68 19.90 -2 -1 34 240.38 21.40 1 1 -34 12.40 9.40 -1 -1 34 16.40 10.30 0 1 -34 225.48 17.30 -1 1 -34 260.67 17.40 -2 1 -34 14.30 8.10 -2 1 -34 -0.40 8.80 -3 1 -34 12.50 7.90 -3 1 -34 0.40 8.40 -4 1 -34 336.87 18.50 -4 1 -34 305.07 21.90 -5 1 -34 136.49 17.20 -5 1 -34 128.99 13.40 -6 1 -34 5.00 7.30 -6 1 -34 11.00 10.00 3 0 -34 165.88 18.10 2 0 -34 63.29 12.50 -2 0 34 73.29 15.40 1 0 -34 3.30 8.60 -1 0 34 19.30 10.70 0 0 -34 51.79 11.10 0 0 34 33.40 10.90 -1 0 -34 44.60 10.80 -2 0 -34 38.70 10.00 -3 0 -34 31.80 8.90 -3 0 -34 16.30 10.10 -4 0 -34 157.48 14.60 -4 0 -34 136.79 16.10 -5 0 -34 90.99 12.30 -5 0 -34 106.99 15.90 -6 0 -34 32.80 9.20 -6 0 -34 12.00 9.90 -7 0 -34 181.48 15.10 -7 0 -34 187.18 19.60 3 -1 -34 252.27 20.80 2 -1 -34 55.49 12.50 -2 1 34 63.49 13.60 1 -1 -34 128.29 20.20 -1 1 34 129.99 17.10 0 -1 -34 138.69 15.60 0 1 34 121.49 16.20 -1 -1 -34 44.70 11.00 1 1 34 59.79 14.10 -2 -1 -34 4.40 8.30 -3 -1 -34 114.89 14.80 -3 -1 -34 122.59 14.70 -4 -1 -34 23.60 10.60 -4 -1 -34 41.10 10.10 -5 -1 -34 88.49 14.80 -5 -1 -34 80.79 12.20 -6 -1 -34 64.99 10.50 -6 -1 -34 63.09 13.40 -7 -1 -34 78.69 14.60 -7 -1 -34 90.49 12.00 2 -2 -34 1.80 9.50 -2 2 34 17.50 10.50 1 -2 -34 147.19 16.30 -1 2 34 161.08 18.40 0 2 34 64.49 13.70 -1 -2 -34 82.19 13.10 1 2 34 68.59 14.30 -2 -2 -34 78.09 13.10 2 2 34 87.39 14.90 -3 -2 -34 144.79 15.00 -4 -2 -34 104.59 22.10 -4 -2 -34 151.18 15.80 -5 -2 -34 14.40 16.50 -5 -2 -34 19.60 9.10 -6 -2 -34 68.59 14.40 -6 -2 -34 36.30 10.10 -7 -2 -34 147.39 17.50 -7 -2 -34 136.89 15.10 2 -3 -34 92.29 14.90 -2 3 34 119.59 25.60 1 -3 -34 143.39 17.00 -1 3 34 122.99 16.40 0 -3 -34 67.49 13.90 0 3 34 43.40 12.70 1 3 34 21.10 11.50 -2 -3 -34 138.59 17.10 2 3 34 135.69 19.00 -3 -3 -34 113.29 14.70 3 3 34 127.99 18.70 -4 -3 -34 52.09 12.00 -5 -3 -34 57.99 12.30 -6 -3 -34 39.40 19.70 -6 -3 -34 43.10 11.40 -7 -3 -34 106.69 18.10 1 -4 -34 240.28 20.70 -1 4 34 261.27 23.10 0 -4 -34 53.79 13.20 0 4 34 42.60 12.50 -1 -4 -34 25.30 12.70 1 4 34 27.60 11.60 -2 -4 -34 410.36 24.50 2 4 34 460.65 26.70 -3 -4 -34 199.28 23.70 3 4 34 171.08 20.20 -6 -4 -34 143.49 24.90 0 -5 -34 4.50 11.70 0 5 34 24.40 11.90 -1 -5 -34 48.10 13.30 1 5 34 58.49 13.00 -2 -5 -34 369.96 24.10 2 5 34 364.46 24.50 -3 -5 -34 81.49 15.10 3 5 34 53.09 13.20 -4 -5 -34 -1.20 11.40 4 5 34 10.30 11.90 -5 -5 -34 28.00 12.20 -2 -6 -34 119.09 19.10 2 6 34 140.99 18.10 -3 -6 -34 31.50 13.90 0 2 -35 221.48 17.20 -1 2 -35 21.80 9.10 -1 2 -35 11.90 13.40 -2 2 -35 68.09 14.50 -2 2 -35 91.69 11.70 -3 2 -35 71.19 16.50 -3 2 -35 100.29 12.10 -4 2 -35 124.09 13.20 1 1 -35 156.78 16.30 0 1 -35 99.29 13.50 -1 1 -35 22.30 10.30 -1 1 -35 20.40 9.50 -2 1 -35 37.70 10.10 -2 1 -35 30.70 11.40 -3 1 -35 89.09 11.50 -3 1 -35 91.39 14.60 -4 1 -35 82.99 14.70 -4 1 -35 94.59 12.10 -5 1 -35 -14.90 10.30 -5 1 -35 9.40 7.90 1 0 -35 178.78 17.60 0 0 -35 73.99 20.80 0 0 35 37.60 12.80 -1 0 -35 59.39 11.30 -2 0 -35 136.99 16.90 -2 0 -35 128.39 14.40 -3 0 -35 190.58 16.10 -3 0 -35 182.28 18.90 -4 0 -35 16.60 10.30 -4 0 -35 15.40 8.30 -5 0 -35 144.79 18.00 -5 0 -35 172.28 14.80 1 -1 -35 103.69 14.40 0 -1 -35 10.50 9.30 0 1 35 5.60 10.90 -1 -1 -35 68.39 13.90 1 1 35 72.59 15.80 -2 -1 -35 192.38 17.40 -3 -1 -35 89.39 14.70 -3 -1 -35 81.99 12.80 -4 -1 -35 46.30 11.40 -4 -1 -35 43.50 12.50 -5 -1 -35 282.27 18.80 -5 -1 -35 331.27 22.80 1 -2 -35 49.30 12.80 0 -2 -35 10.80 9.50 0 2 35 11.20 10.10 -1 -2 -35 135.89 15.70 1 2 35 115.49 17.70 2 2 35 149.99 18.40 -3 -2 -35 -5.30 9.40 -4 -2 -35 92.79 13.60 -4 -2 -35 102.29 16.30 -5 -2 -35 117.59 13.90 -5 -2 -35 122.19 15.50 0 -3 -35 54.79 12.50 0 3 35 37.10 14.70 -1 -3 -35 93.89 15.10 1 3 35 91.89 15.80 -2 -3 -35 64.99 13.50 2 3 35 87.09 16.70 -3 -3 -35 -0.30 10.60 3 3 35 15.50 10.80 -4 -3 -35 206.78 29.00 -5 -3 -35 201.78 19.20 -1 -4 -35 104.49 15.40 1 4 35 182.38 20.00 -2 -4 -35 69.39 14.10 2 4 35 43.60 13.00 -3 -4 -35 56.29 13.30 3 4 35 58.49 13.60 -4 -4 -35 116.99 15.60 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 23747 _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 Ir1 Ir 0.36218(2) 0.43858(2) 0.23771(2) 0.01075(4) Uani 1 1 d . . . . . S1 S 0.69461(11) 0.12229(11) 0.22256(5) 0.0318(2) Uani 1 1 d . . . . . Cl00 Cl 0.62800(13) 0.95608(12) 0.54200(6) 0.0451(3) Uani 1 1 d . . . . . Cl1 Cl 0.39834(14) 1.00975(14) 0.60750(6) 0.0547(4) Uani 1 1 d . . . . . Cl2 Cl 0.05421(15) 0.16352(16) 0.00169(6) 0.0558(4) Uani 1 1 d . . . . . Cl3 Cl 0.14242(14) 0.05660(16) -0.10153(6) 0.0553(4) Uani 1 1 d . . . . . Cl4 Cl 0.59100(17) 0.78003(15) 0.07671(7) 0.0616(4) Uani 1 1 d . . . . . Cl5 Cl 0.50515(15) 1.01677(13) 0.11845(7) 0.0586(4) Uani 1 1 d . . . . . O3 O 0.4962(2) 0.2928(2) 0.25486(10) 0.0148(5) Uani 1 1 d . . . . . O4 O 0.3993(2) 0.5070(2) 0.31047(9) 0.0152(5) Uani 1 1 d . . . . . O5 O 0.0905(2) 0.2370(2) 0.11274(11) 0.0187(5) Uani 1 1 d . . . . . N1 N 0.2115(2) 0.4019(3) 0.28669(11) 0.0122(5) Uani 1 1 d . . . . . O6 O 0.2430(3) 0.8736(2) 0.15901(11) 0.0222(6) Uani 1 1 d . . . . . N3 N 0.5041(3) 0.4785(3) 0.18232(11) 0.0130(5) Uani 1 1 d . . . . . N2 N 0.0510(3) 0.4757(3) 0.34102(11) 0.0136(5) Uani 1 1 d . . . . . C34 C 0.1389(3) 0.5003(3) 0.30105(13) 0.0121(6) Uani 1 1 d . . . . . O2 O 0.7252(3) 0.4957(3) 0.50026(12) 0.0288(6) Uani 1 1 d . . . . . N4 N 0.6219(3) 0.4205(3) 0.10820(11) 0.0136(5) Uani 1 1 d . . . . . C1 C 0.3205(3) 0.3691(3) 0.17260(13) 0.0126(6) Uani 1 1 d . . . . . C33 C 0.1579(3) 0.6084(3) 0.27015(13) 0.0131(6) Uani 1 1 d . . . . . C28 C 0.2571(3) 0.5887(3) 0.22895(13) 0.0122(6) Uani 1 1 d . . . . . C53 C 0.2045(3) 0.1846(3) 0.31372(13) 0.0134(6) Uani 1 1 d . . . . . C42 C -0.0001(3) 0.2803(3) 0.38839(14) 0.0160(7) Uani 1 1 d . . . . . C41 C 0.0666(3) 0.3537(3) 0.35084(13) 0.0139(6) Uani 1 1 d . . . . . C48 C 0.1428(3) 0.1090(3) 0.35084(14) 0.0163(7) Uani 1 1 d . . . . . O1 O 0.6444(3) 0.6676(3) 0.53660(12) 0.0312(7) Uani 1 1 d . . . . . C65 C 0.4056(3) 0.6597(3) 0.39026(13) 0.0128(6) Uani 1 1 d . . . . . H65 H 0.349814 0.676789 0.365024 0.015 Uiso 1 1 calc R U . . . C3 C 0.1946(3) 0.2781(3) 0.12054(14) 0.0153(6) Uani 1 1 d . . . . . C52 C 0.2988(3) 0.1369(3) 0.27579(14) 0.0168(7) Uani 1 1 d . . . . . H52 H 0.338678 0.187859 0.250672 0.020 Uiso 1 1 calc R U . . . C54 C 0.1649(3) 0.3091(3) 0.31627(13) 0.0121(6) Uani 1 1 d . . . . . C2 C 0.2116(3) 0.3285(3) 0.16754(14) 0.0146(6) Uani 1 1 d . . . . . H2 H 0.148904 0.335450 0.196528 0.018 Uiso 1 1 calc R U . . . C7 C 0.5136(3) 0.4149(3) 0.13794(13) 0.0137(6) Uani 1 1 d . . . . . C14 C 0.6848(3) 0.4924(3) 0.13479(13) 0.0134(6) Uani 1 1 d . . . . . C30 C 0.2088(3) 0.7899(3) 0.19679(14) 0.0172(7) Uani 1 1 d . . . . . C9 C 0.6462(3) 0.4318(3) 0.01069(13) 0.0161(7) Uani 1 1 d . . . . . H9 H 0.620759 0.514180 0.011714 0.019 Uiso 1 1 calc R U . . . C27 C 0.6090(3) 0.5294(3) 0.17997(13) 0.0132(6) Uani 1 1 d . . . . . C35 C -0.0247(3) 0.5661(3) 0.37184(14) 0.0155(6) Uani 1 1 d . . . . . C29 C 0.2788(3) 0.6805(3) 0.19244(13) 0.0152(6) Uani 1 1 d . . . . . H29 H 0.342440 0.668758 0.164008 0.018 Uiso 1 1 calc R U . . . C32 C 0.0886(3) 0.7188(3) 0.27455(14) 0.0163(7) Uani 1 1 d . . . . . H32 H 0.024281 0.731496 0.302639 0.020 Uiso 1 1 calc R U . . . C43 C -0.1012(3) 0.3239(4) 0.42403(15) 0.0205(7) Uani 1 1 d . . . . . H43 H -0.128008 0.406157 0.424031 0.025 Uiso 1 1 calc R U . . . C15 C 0.8041(3) 0.5215(3) 0.12239(13) 0.0141(6) Uani 1 1 d . . . . . C60 C 0.6813(3) 0.2075(3) 0.27686(14) 0.0170(7) Uani 1 1 d . . . . . C61 C 0.5756(3) 0.2967(3) 0.28606(14) 0.0152(6) Uani 1 1 d . . . . . C6 C 0.4121(3) 0.3577(3) 0.12847(13) 0.0135(6) Uani 1 1 d . . . . . C8 C 0.6573(3) 0.3650(3) 0.05787(13) 0.0143(6) Uani 1 1 d . . . . . C26 C 0.6385(3) 0.6178(3) 0.21269(13) 0.0133(6) Uani 1 1 d . . . . . C4 C 0.2857(3) 0.2656(3) 0.07761(14) 0.0167(7) Uani 1 1 d . . . . . H4 H 0.273336 0.230029 0.045810 0.020 Uiso 1 1 calc R U . . . C5 C 0.3939(3) 0.3050(3) 0.08144(14) 0.0160(6) Uani 1 1 d . . . . . H5 H 0.456161 0.296568 0.052267 0.019 Uiso 1 1 calc R U . . . C47 C 0.0411(3) 0.1570(3) 0.38838(14) 0.0178(7) Uani 1 1 d . . . . . C18 C 1.0428(3) 0.5662(4) 0.11061(16) 0.0213(7) Uani 1 1 d . . . . . H18 H 1.124457 0.578640 0.107521 0.026 Uiso 1 1 calc R U . . . C36 C -0.1377(3) 0.6063(3) 0.35837(14) 0.0183(7) Uani 1 1 d . . . . . H36 H -0.168146 0.571718 0.330276 0.022 Uiso 1 1 calc R U . . . C51 C 0.3334(3) 0.0171(3) 0.27489(15) 0.0190(7) Uani 1 1 d . . . . . H51 H 0.396981 -0.014312 0.249206 0.023 Uiso 1 1 calc R U . . . C62 C 0.5719(3) 0.3774(3) 0.32707(14) 0.0185(7) Uani 1 1 d . . . . . H62 H 0.634555 0.365334 0.349110 0.022 Uiso 1 1 calc R U . . . C63 C 0.4841(3) 0.4733(3) 0.33805(13) 0.0149(6) Uani 1 1 d . . . . . C16 C 0.8867(3) 0.4775(3) 0.07846(14) 0.0165(7) Uani 1 1 d . . . . . H16 H 0.860954 0.431737 0.052696 0.020 Uiso 1 1 calc R U . . . C20 C 0.8417(3) 0.5953(3) 0.15902(14) 0.0154(6) Uani 1 1 d . . . . . C68 C 0.5616(3) 0.6096(3) 0.46255(14) 0.0172(7) Uani 1 1 d . . . . . C19 C 0.9631(3) 0.6132(3) 0.15247(15) 0.0200(7) Uani 1 1 d . . . . . H19 H 0.990910 0.659006 0.177610 0.024 Uiso 1 1 calc R U . . . C25 C 0.5544(3) 0.6794(3) 0.25072(13) 0.0158(6) Uani 1 1 d . . . . . H25 H 0.475329 0.658688 0.257334 0.019 Uiso 1 1 calc R U . . . C59 C 0.7809(4) 0.1846(4) 0.30715(18) 0.0292(10) Uani 1 1 d . . . . . H59 H 0.790439 0.224625 0.338205 0.035 Uiso 1 1 calc R U . . . C10 C 0.6728(3) 0.3763(4) -0.03780(15) 0.0242(8) Uani 1 1 d . . . . . H10 H 0.665882 0.420892 -0.070373 0.029 Uiso 1 1 calc R U . . . C37 C -0.2057(3) 0.6980(4) 0.38667(15) 0.0229(8) Uani 1 1 d . . . . . H37 H -0.283273 0.726680 0.377785 0.027 Uiso 1 1 calc R U . . . C55 C -0.0064(3) 0.2503(4) 0.15500(16) 0.0227(8) Uani 1 1 d . . . . . H55A H -0.076712 0.222233 0.143546 0.034 Uiso 1 1 calc R U . . . H55B H -0.025389 0.333734 0.163741 0.034 Uiso 1 1 calc R U . . . H55C H 0.016311 0.204084 0.186763 0.034 Uiso 1 1 calc R U . . . C64 C 0.4864(3) 0.5511(3) 0.38402(13) 0.0163(7) Uani 1 1 d . . . . . C22 C 0.7841(3) 0.7430(3) 0.23085(15) 0.0188(7) Uani 1 1 d . . . . . H22 H 0.862308 0.765798 0.224331 0.023 Uiso 1 1 calc R U . . . C21 C 0.7554(3) 0.6506(3) 0.20177(13) 0.0146(6) Uani 1 1 d . . . . . C40 C 0.0215(4) 0.6145(3) 0.41307(15) 0.0207(7) Uani 1 1 d . . . . . H40 H 0.099166 0.586062 0.421909 0.025 Uiso 1 1 calc R U . . . C50 C 0.2747(4) -0.0590(3) 0.31202(16) 0.0215(7) Uani 1 1 d . . . . . H50 H 0.299297 -0.141645 0.311716 0.026 Uiso 1 1 calc R U . . . C17 C 1.0035(3) 0.5004(4) 0.07292(15) 0.0197(7) Uani 1 1 d . . . . . H17 H 1.057657 0.471210 0.043175 0.024 Uiso 1 1 calc R U . . . C24 C 0.5852(3) 0.7692(3) 0.27845(14) 0.0184(7) Uani 1 1 d . . . . . H24 H 0.527752 0.809491 0.304301 0.022 Uiso 1 1 calc R U . . . C49 C 0.1817(3) -0.0134(3) 0.34876(16) 0.0208(7) Uani 1 1 d . . . . . H49 H 0.142525 -0.065658 0.373443 0.025 Uiso 1 1 calc R U . . . C58 C 0.8647(4) 0.0900(4) 0.28238(17) 0.0245(8) Uani 1 1 d . . . . . H58 H 0.936484 0.058480 0.296337 0.029 Uiso 1 1 calc R U . . . C23 C 0.7006(3) 0.8012(3) 0.26865(15) 0.0192(7) Uani 1 1 d . . . . . H23 H 0.721875 0.862887 0.287963 0.023 Uiso 1 1 calc R U . . . C13 C 0.6959(3) 0.2447(3) 0.05761(15) 0.0210(7) Uani 1 1 d . . . . . H13 H 0.704620 0.200817 0.090223 0.025 Uiso 1 1 calc R U . . . C31 C 0.1138(3) 0.8100(3) 0.23775(14) 0.0176(7) Uani 1 1 d . . . . . H31 H 0.066899 0.885048 0.240493 0.021 Uiso 1 1 calc R U . . . C39 C -0.0493(4) 0.7061(4) 0.44110(17) 0.0277(9) Uani 1 1 d . . . . . H39 H -0.020049 0.739849 0.469731 0.033 Uiso 1 1 calc R U . . . C69 C 0.5648(3) 0.5278(4) 0.42265(14) 0.0190(7) Uani 1 1 d . . . . . H69 H 0.619606 0.457484 0.421879 0.023 Uiso 1 1 calc R U . . . C38 C -0.1617(4) 0.7481(4) 0.42761(16) 0.0272(9) Uani 1 1 d . . . . . H38 H -0.208652 0.811354 0.446516 0.033 Uiso 1 1 calc R U . . . C44 C -0.1615(4) 0.2481(4) 0.45888(16) 0.0244(8) Uani 1 1 d . . . . . H44 H -0.229637 0.278075 0.482538 0.029 Uiso 1 1 calc R U . . . C45 C -0.1219(4) 0.1271(4) 0.45916(17) 0.0285(9) Uani 1 1 d . . . . . H45 H -0.163673 0.075032 0.482927 0.034 Uiso 1 1 calc R U . . . C56 C 0.1735(4) 0.9862(3) 0.15872(16) 0.0243(8) Uani 1 1 d . . . . . H56A H 0.207037 1.035456 0.129032 0.036 Uiso 1 1 calc R U . . . H56B H 0.174671 1.023924 0.192742 0.036 Uiso 1 1 calc R U . . . H56C H 0.090873 0.976996 0.154190 0.036 Uiso 1 1 calc R U . . . C11 C 0.7099(4) 0.2551(4) -0.03909(16) 0.0286(9) Uani 1 1 d . . . . . H11 H 0.727217 0.217086 -0.072412 0.034 Uiso 1 1 calc R U . . . C12 C 0.7214(4) 0.1901(4) 0.00880(17) 0.0286(9) Uani 1 1 d . . . . . H12 H 0.746889 0.107627 0.007927 0.034 Uiso 1 1 calc R U . . . C46 C -0.0230(4) 0.0829(4) 0.42535(16) 0.0248(8) Uani 1 1 d . . . . . H46 H 0.003254 0.000643 0.426736 0.030 Uiso 1 1 calc R U . . . C57 C 0.8305(4) 0.0507(4) 0.23719(18) 0.0286(9) Uani 1 1 d . . . . . H57 H 0.876436 -0.009559 0.216026 0.034 Uiso 1 1 calc R U . . . C70 C 0.6517(4) 0.5826(4) 0.50097(16) 0.0248(8) Uani 1 1 d . . . . . C67 C 0.4826(4) 0.7114(4) 0.46388(16) 0.0229(8) Uani 1 1 d . . . . . H67 H 0.483403 0.766331 0.490864 0.027 Uiso 1 1 calc R U . . . C71 C 0.7349(4) 0.6516(4) 0.57225(19) 0.0332(10) Uani 1 1 d . . . . . H71A H 0.813940 0.636235 0.551336 0.050 Uiso 1 1 calc R U . . . H71B H 0.721389 0.584537 0.597094 0.050 Uiso 1 1 calc R U . . . H71C H 0.730920 0.723120 0.592623 0.050 Uiso 1 1 calc R U . . . C66 C 0.4022(4) 0.7357(4) 0.42701(16) 0.0266(8) Uani 1 1 d . . . . . H66 H 0.346593 0.805464 0.428510 0.032 Uiso 1 1 calc R U . . . C02I C 0.5359(5) 0.9192(5) 0.6010(2) 0.0389(11) Uani 1 1 d . . . . . H02A H 0.521624 0.835821 0.600175 0.047 Uiso 1 1 calc R U . . . H02B H 0.577410 0.927638 0.632612 0.047 Uiso 1 1 calc R U . . . C02J C 0.5465(5) 0.8668(5) 0.1338(2) 0.0468(13) Uani 1 1 d . . . . . H02E H 0.478042 0.835066 0.155587 0.056 Uiso 1 1 calc R U . . . H02F H 0.613284 0.859548 0.155908 0.056 Uiso 1 1 calc R U . . . C02K C 0.0194(7) 0.1285(7) -0.0609(2) 0.0630(18) Uani 1 1 d . . . . . H02C H -0.011254 0.201927 -0.079757 0.076 Uiso 1 1 calc R U . . . H02D H -0.045091 0.077081 -0.055375 0.076 Uiso 1 1 calc R U . . . O0AA O 0.5036(10) 0.9679(10) 0.0198(4) 0.029(2) Uiso 0.27 1 d . . P A -1 H0AA H 0.461152 0.980631 0.049839 0.044 Uiso 0.27 1 d R U P A -1 H0AB H 0.530012 0.894971 0.021489 0.044 Uiso 0.27 1 d R U P A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.00883(6) 0.01372(6) 0.00938(6) -0.00019(4) 0.00050(4) -0.00189(4) S1 0.0296(5) 0.0324(6) 0.0333(6) -0.0074(5) -0.0050(4) 0.0006(5) Cl00 0.0453(7) 0.0435(7) 0.0442(7) -0.0036(6) 0.0017(6) -0.0030(6) Cl1 0.0512(8) 0.0510(8) 0.0529(8) 0.0091(7) 0.0096(7) 0.0076(7) Cl2 0.0568(9) 0.0751(11) 0.0398(7) -0.0149(7) -0.0040(6) -0.0214(8) Cl3 0.0482(8) 0.0720(10) 0.0448(8) -0.0120(7) -0.0024(6) -0.0045(7) Cl4 0.0695(10) 0.0569(9) 0.0594(9) -0.0075(7) -0.0216(8) 0.0039(8) Cl5 0.0560(9) 0.0384(7) 0.0796(11) 0.0149(7) -0.0052(8) -0.0093(7) O3 0.0145(11) 0.0161(12) 0.0143(11) -0.0020(9) -0.0034(9) -0.0015(10) O4 0.0147(11) 0.0187(12) 0.0119(11) -0.0015(9) -0.0019(9) -0.0001(10) O5 0.0141(12) 0.0216(13) 0.0224(13) -0.0022(10) -0.0040(10) -0.0067(10) N1 0.0110(12) 0.0141(13) 0.0114(12) 0.0003(10) -0.0005(10) -0.0021(11) O6 0.0306(15) 0.0143(12) 0.0190(13) 0.0023(10) 0.0045(11) -0.0009(11) N3 0.0118(13) 0.0145(13) 0.0131(13) -0.0008(10) 0.0002(10) -0.0040(11) N2 0.0115(12) 0.0154(13) 0.0130(13) 0.0002(10) 0.0024(10) -0.0022(11) C34 0.0110(14) 0.0125(15) 0.0125(14) -0.0002(11) -0.0007(11) -0.0014(12) O2 0.0283(15) 0.0309(16) 0.0261(15) -0.0020(12) -0.0044(12) 0.0013(13) N4 0.0113(12) 0.0182(14) 0.0115(12) -0.0019(10) 0.0009(10) -0.0048(11) C1 0.0132(14) 0.0109(14) 0.0134(14) 0.0027(11) -0.0024(12) -0.0005(12) C33 0.0124(14) 0.0149(15) 0.0115(14) 0.0013(12) -0.0006(11) -0.0016(12) C28 0.0111(14) 0.0124(14) 0.0133(14) -0.0019(11) -0.0019(11) -0.0017(12) C53 0.0130(14) 0.0147(15) 0.0136(14) 0.0003(12) -0.0035(12) -0.0045(13) C42 0.0134(15) 0.0199(17) 0.0152(15) 0.0026(13) -0.0016(12) -0.0063(13) C41 0.0111(14) 0.0182(16) 0.0132(14) -0.0008(12) -0.0011(11) -0.0050(13) C48 0.0129(15) 0.0211(17) 0.0157(15) 0.0022(13) -0.0022(12) -0.0054(14) O1 0.0357(17) 0.0339(17) 0.0252(15) -0.0079(13) -0.0117(13) 0.0014(14) C65 0.0092(13) 0.0130(15) 0.0121(14) 0.0099(11) 0.0045(11) 0.0049(12) C3 0.0125(15) 0.0147(15) 0.0197(16) 0.0026(12) -0.0067(12) -0.0021(13) C52 0.0159(16) 0.0183(17) 0.0163(15) -0.0020(13) -0.0004(12) -0.0036(14) C54 0.0111(14) 0.0146(15) 0.0113(14) 0.0006(11) -0.0017(11) -0.0038(12) C2 0.0137(15) 0.0141(15) 0.0155(15) 0.0009(12) 0.0001(12) -0.0021(13) C7 0.0119(14) 0.0167(16) 0.0121(14) -0.0014(12) -0.0002(11) -0.0016(13) C14 0.0119(14) 0.0165(16) 0.0120(14) -0.0007(12) -0.0007(11) -0.0028(13) C30 0.0235(18) 0.0153(16) 0.0137(15) 0.0004(12) -0.0024(13) -0.0055(14) C9 0.0117(15) 0.0230(18) 0.0132(15) -0.0027(13) 0.0013(12) -0.0025(13) C27 0.0110(14) 0.0158(15) 0.0124(14) 0.0022(12) -0.0001(11) -0.0023(12) C35 0.0130(15) 0.0163(16) 0.0154(15) -0.0004(12) 0.0045(12) -0.0012(13) C29 0.0146(15) 0.0176(16) 0.0130(14) -0.0010(12) 0.0013(12) -0.0037(13) C32 0.0152(15) 0.0180(16) 0.0147(15) -0.0006(13) 0.0005(12) -0.0007(13) C43 0.0184(17) 0.0236(18) 0.0182(17) -0.0004(14) 0.0035(13) -0.0043(15) C15 0.0115(14) 0.0173(16) 0.0132(14) 0.0016(12) -0.0011(12) -0.0016(13) C60 0.0150(15) 0.0177(16) 0.0174(16) -0.0031(13) 0.0019(12) -0.0016(13) C61 0.0117(14) 0.0177(16) 0.0154(15) 0.0013(12) 0.0014(12) -0.0028(13) C6 0.0119(14) 0.0152(15) 0.0129(14) -0.0013(12) 0.0005(11) -0.0015(12) C8 0.0101(14) 0.0205(17) 0.0123(14) -0.0048(12) 0.0021(11) -0.0038(13) C26 0.0135(15) 0.0135(15) 0.0131(14) 0.0015(12) -0.0021(12) -0.0031(12) C4 0.0180(16) 0.0173(16) 0.0153(15) -0.0027(13) -0.0032(13) -0.0025(14) C5 0.0155(15) 0.0168(16) 0.0160(15) -0.0014(12) -0.0008(12) -0.0039(13) C47 0.0164(16) 0.0196(17) 0.0175(16) 0.0031(13) -0.0016(13) -0.0051(14) C18 0.0111(15) 0.0260(19) 0.0260(19) 0.0028(15) 0.0008(13) -0.0040(14) C36 0.0154(16) 0.0222(18) 0.0151(15) 0.0023(13) 0.0023(12) 0.0005(14) C51 0.0182(16) 0.0173(17) 0.0213(17) -0.0018(13) -0.0021(13) -0.0014(14) C62 0.0148(16) 0.0235(18) 0.0176(16) -0.0022(14) -0.0067(13) 0.0010(14) C63 0.0158(15) 0.0182(16) 0.0102(14) 0.0011(12) 0.0007(12) -0.0031(13) C16 0.0117(15) 0.0224(17) 0.0157(15) 0.0003(13) -0.0005(12) -0.0047(13) C20 0.0137(15) 0.0176(16) 0.0148(15) 0.0013(12) -0.0013(12) -0.0021(13) C68 0.0170(16) 0.0231(18) 0.0118(15) -0.0023(13) -0.0001(12) -0.0046(14) C19 0.0141(16) 0.0223(18) 0.0240(18) -0.0024(14) -0.0002(13) -0.0053(14) C25 0.0153(15) 0.0185(16) 0.0136(15) -0.0007(12) -0.0011(12) -0.0027(13) C59 0.0194(18) 0.030(2) 0.029(2) 0.0057(17) 0.0072(16) 0.0181(17) C10 0.0164(17) 0.044(2) 0.0118(15) 0.0020(15) -0.0008(13) -0.0030(17) C37 0.0169(17) 0.0254(19) 0.0213(18) 0.0049(15) 0.0060(14) 0.0059(15) C55 0.0152(16) 0.028(2) 0.0264(19) 0.0027(15) -0.0022(14) -0.0091(15) C64 0.0180(16) 0.0185(17) 0.0121(14) -0.0031(12) 0.0015(12) -0.0037(14) C22 0.0154(16) 0.0225(18) 0.0197(17) 0.0001(14) -0.0033(13) -0.0064(14) C21 0.0140(15) 0.0179(16) 0.0124(14) 0.0012(12) -0.0031(12) -0.0033(13) C40 0.0220(18) 0.0221(18) 0.0176(16) -0.0030(14) -0.0021(14) -0.0004(15) C50 0.0212(18) 0.0162(17) 0.0275(19) 0.0020(14) -0.0049(15) -0.0037(15) C17 0.0131(15) 0.0255(19) 0.0193(17) 0.0017(14) 0.0018(13) -0.0023(14) C24 0.0208(17) 0.0173(16) 0.0170(16) -0.0026(13) -0.0001(13) -0.0038(14) C49 0.0189(17) 0.0191(17) 0.0241(18) 0.0044(14) -0.0011(14) -0.0040(15) C58 0.0169(17) 0.0241(19) 0.032(2) -0.0051(16) -0.0068(15) 0.0034(15) C23 0.0222(18) 0.0174(17) 0.0199(17) -0.0012(13) -0.0046(14) -0.0079(15) C13 0.0213(18) 0.0213(18) 0.0194(17) -0.0033(14) 0.0009(14) -0.0012(15) C31 0.0224(17) 0.0130(15) 0.0163(16) -0.0011(12) -0.0007(13) 0.0008(14) C39 0.033(2) 0.028(2) 0.0213(19) -0.0090(16) -0.0003(16) -0.0013(18) C69 0.0190(17) 0.0243(18) 0.0132(15) -0.0044(13) 0.0017(13) -0.0033(15) C38 0.031(2) 0.0218(19) 0.0232(19) -0.0032(15) 0.0084(16) 0.0056(17) C44 0.0202(18) 0.028(2) 0.0230(18) 0.0027(15) 0.0059(15) -0.0059(16) C45 0.026(2) 0.030(2) 0.027(2) 0.0074(17) 0.0087(16) -0.0096(18) C56 0.032(2) 0.0137(17) 0.0257(19) 0.0020(14) -0.0025(16) -0.0004(16) C11 0.027(2) 0.040(2) 0.0177(18) -0.0122(17) 0.0005(15) 0.0016(19) C12 0.031(2) 0.027(2) 0.026(2) -0.0091(16) 0.0004(17) 0.0021(18) C46 0.026(2) 0.0227(19) 0.0250(19) 0.0054(15) 0.0012(15) -0.0070(16) C57 0.029(2) 0.023(2) 0.034(2) -0.0040(17) 0.0009(17) -0.0069(17) C70 0.0249(19) 0.028(2) 0.0221(18) -0.0024(15) -0.0017(15) -0.0055(17) C67 0.0218(18) 0.0245(19) 0.0212(18) -0.0001(15) 0.0016(14) -0.0029(16) C71 0.035(2) 0.037(3) 0.030(2) -0.0040(19) -0.0142(19) -0.003(2) C66 0.028(2) 0.026(2) 0.0239(19) -0.0019(16) -0.0004(16) 0.0006(17) C02I 0.045(3) 0.041(3) 0.030(2) -0.003(2) -0.004(2) -0.004(2) C02J 0.044(3) 0.040(3) 0.056(3) 0.014(3) -0.011(3) -0.005(2) C02K 0.080(5) 0.067(4) 0.041(3) -0.007(3) -0.016(3) 0.010(4) 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 O4 Ir1 O3 84.55(9) . . ? N1 Ir1 O3 103.62(10) . . ? N1 Ir1 O4 81.11(10) . . ? N1 Ir1 N3 174.48(11) . . ? N3 Ir1 O3 80.10(10) . . ? N3 Ir1 O4 103.45(10) . . ? C1 Ir1 O3 95.14(11) . . ? C1 Ir1 O4 176.48(12) . . ? C1 Ir1 N1 95.57(12) . . ? C1 Ir1 N3 79.93(12) . . ? C28 Ir1 O3 169.60(11) . . ? C28 Ir1 O4 86.45(12) . . ? C28 Ir1 N1 80.06(12) . . ? C28 Ir1 N3 96.99(12) . . ? C28 Ir1 C1 94.15(13) . . ? C60 S1 C57 91.7(2) . . ? C61 O3 Ir1 125.0(2) . . ? C63 O4 Ir1 129.2(2) . . ? C3 O5 C55 117.6(3) . . ? C34 N1 Ir1 111.9(2) . . ? C34 N1 C54 106.7(3) . . ? C54 N1 Ir1 140.7(2) . . ? C30 O6 C56 118.7(3) . . ? C7 N3 Ir1 111.5(2) . . ? C7 N3 C27 106.7(3) . . ? C27 N3 Ir1 139.8(2) . . ? C34 N2 C41 106.9(3) . . ? C34 N2 C35 122.9(3) . . ? C41 N2 C35 129.2(3) . . ? N1 C34 N2 110.7(3) . . ? N1 C34 C33 117.6(3) . . ? N2 C34 C33 131.3(3) . . ? C7 N4 C14 107.6(3) . . ? C7 N4 C8 123.7(3) . . ? C14 N4 C8 128.6(3) . . ? C2 C1 Ir1 125.9(2) . . ? C2 C1 C6 118.2(3) . . ? C6 C1 Ir1 115.8(2) . . ? C28 C33 C34 111.1(3) . . ? C32 C33 C34 128.1(3) . . ? C32 C33 C28 120.7(3) . . ? C33 C28 Ir1 114.5(2) . . ? C29 C28 Ir1 126.9(3) . . ? C29 C28 C33 118.0(3) . . ? C48 C53 C54 117.2(3) . . ? C52 C53 C48 120.2(3) . . ? C52 C53 C54 122.7(3) . . ? C43 C42 C41 123.8(3) . . ? C43 C42 C47 120.0(3) . . ? C47 C42 C41 116.2(3) . . ? N2 C41 C42 130.6(3) . . ? C54 C41 N2 106.6(3) . . ? C54 C41 C42 122.8(3) . . ? C53 C48 C47 120.6(3) . . ? C49 C48 C53 117.4(3) . . ? C49 C48 C47 122.0(3) . . ? C70 O1 C71 115.1(4) . . ? C64 C65 H65 117.0 . . ? C66 C65 H65 117.0 . . ? C66 C65 C64 126.1(4) . . ? O5 C3 C2 123.7(3) . . ? O5 C3 C4 115.5(3) . . ? C2 C3 C4 120.8(3) . . ? C53 C52 H52 119.7 . . ? C51 C52 C53 120.5(3) . . ? C51 C52 H52 119.7 . . ? N1 C54 C53 129.1(3) . . ? C41 C54 N1 108.9(3) . . ? C41 C54 C53 121.9(3) . . ? C1 C2 H2 119.7 . . ? C3 C2 C1 120.6(3) . . ? C3 C2 H2 119.7 . . ? N3 C7 N4 110.4(3) . . ? N3 C7 C6 118.3(3) . . ? N4 C7 C6 131.2(3) . . ? N4 C14 C15 130.3(3) . . ? C27 C14 N4 105.9(3) . . ? C27 C14 C15 123.7(3) . . ? O6 C30 C29 114.7(3) . . ? O6 C30 C31 124.2(3) . . ? C29 C30 C31 121.1(3) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? C10 C9 C8 119.0(4) . . ? N3 C27 C26 129.6(3) . . ? C14 C27 N3 109.2(3) . . ? C14 C27 C26 120.7(3) . . ? C36 C35 N2 120.0(3) . . ? C36 C35 C40 121.8(3) . . ? C40 C35 N2 118.1(3) . . ? C28 C29 C30 121.0(3) . . ? C28 C29 H29 119.5 . . ? C30 C29 H29 119.5 . . ? C33 C32 H32 120.0 . . ? C31 C32 C33 120.0(3) . . ? C31 C32 H32 120.0 . . ? C42 C43 H43 119.7 . . ? C44 C43 C42 120.7(4) . . ? C44 C43 H43 119.7 . . ? C16 C15 C14 124.8(3) . . ? C16 C15 C20 119.3(3) . . ? C20 C15 C14 115.9(3) . . ? C61 C60 S1 118.2(3) . . ? C59 C60 S1 113.5(3) . . ? C59 C60 C61 128.2(3) . . ? O3 C61 C60 115.1(3) . . ? O3 C61 C62 126.7(3) . . ? C62 C61 C60 118.2(3) . . ? C1 C6 C7 111.3(3) . . ? C5 C6 C1 120.5(3) . . ? C5 C6 C7 128.0(3) . . ? C9 C8 N4 119.0(3) . . ? C13 C8 N4 119.0(3) . . ? C13 C8 C9 121.8(3) . . ? C25 C26 C27 123.1(3) . . ? C25 C26 C21 119.7(3) . . ? C21 C26 C27 117.0(3) . . ? C3 C4 H4 120.1 . . ? C5 C4 C3 119.9(3) . . ? C5 C4 H4 120.1 . . ? C6 C5 H5 120.0 . . ? C4 C5 C6 120.0(3) . . ? C4 C5 H5 120.0 . . ? C42 C47 C48 121.2(3) . . ? C46 C47 C42 117.2(3) . . ? C46 C47 C48 121.6(3) . . ? C19 C18 H18 120.0 . . ? C19 C18 C17 120.0(3) . . ? C17 C18 H18 120.0 . . ? C35 C36 H36 120.6 . . ? C35 C36 C37 118.7(4) . . ? C37 C36 H36 120.6 . . ? C52 C51 H51 120.0 . . ? C52 C51 C50 120.1(3) . . ? C50 C51 H51 120.0 . . ? C61 C62 H62 117.2 . . ? C63 C62 C61 125.6(3) . . ? C63 C62 H62 117.2 . . ? O4 C63 C62 125.4(3) . . ? O4 C63 C64 113.3(3) . . ? C62 C63 C64 121.2(3) . . ? C15 C16 H16 119.7 . . ? C17 C16 C15 120.6(3) . . ? C17 C16 H16 119.7 . . ? C15 C20 C21 120.3(3) . . ? C19 C20 C15 117.7(3) . . ? C19 C20 C21 121.9(3) . . ? C69 C68 C70 116.5(3) . . ? C67 C68 C69 120.8(4) . . ? C67 C68 C70 122.7(3) . . ? C18 C19 C20 121.9(4) . . ? C18 C19 H19 119.1 . . ? C20 C19 H19 119.1 . . ? C26 C25 H25 119.6 . . ? C24 C25 C26 120.8(3) . . ? C24 C25 H25 119.6 . . ? C60 C59 H59 125.7 . . ? C60 C59 C58 108.6(4) . . ? C58 C59 H59 125.7 . . ? C9 C10 H10 119.9 . . ? C9 C10 C11 120.3(4) . . ? C11 C10 H10 119.9 . . ? C36 C37 H37 119.7 . . ? C38 C37 C36 120.7(4) . . ? C38 C37 H37 119.7 . . ? O5 C55 H55A 109.5 . . ? O5 C55 H55B 109.5 . . ? O5 C55 H55C 109.5 . . ? H55A C55 H55B 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C65 C64 C63 120.5(3) . . ? C69 C64 C65 115.2(3) . . ? C69 C64 C63 124.3(3) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C23 C22 C21 121.3(3) . . ? C26 C21 C20 120.9(3) . . ? C22 C21 C26 118.1(3) . . ? C22 C21 C20 120.9(3) . . ? C35 C40 H40 120.9 . . ? C35 C40 C39 118.2(4) . . ? C39 C40 H40 120.9 . . ? C51 C50 H50 120.1 . . ? C49 C50 C51 119.8(4) . . ? C49 C50 H50 120.1 . . ? C18 C17 H17 119.8 . . ? C16 C17 C18 120.4(3) . . ? C16 C17 H17 119.8 . . ? C25 C24 H24 120.0 . . ? C25 C24 C23 120.1(3) . . ? C23 C24 H24 120.0 . . ? C48 C49 H49 119.0 . . ? C50 C49 C48 122.0(3) . . ? C50 C49 H49 119.0 . . ? C59 C58 H58 123.3 . . ? C57 C58 C59 113.5(4) . . ? C57 C58 H58 123.3 . . ? C22 C23 C24 120.0(3) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C8 C13 H13 120.7 . . ? C12 C13 C8 118.6(4) . . ? C12 C13 H13 120.7 . . ? C30 C31 H31 120.4 . . ? C32 C31 C30 119.2(3) . . ? C32 C31 H31 120.4 . . ? C40 C39 H39 119.7 . . ? C38 C39 C40 120.6(4) . . ? C38 C39 H39 119.7 . . ? C68 C69 H69 120.5 . . ? C64 C69 C68 119.0(4) . . ? C64 C69 H69 120.5 . . ? C37 C38 C39 120.0(4) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C43 C44 H44 120.1 . . ? C43 C44 C45 119.8(4) . . ? C45 C44 H44 120.1 . . ? C44 C45 H45 119.7 . . ? C46 C45 C44 120.6(4) . . ? C46 C45 H45 119.7 . . ? O6 C56 H56A 109.5 . . ? O6 C56 H56B 109.5 . . ? O6 C56 H56C 109.5 . . ? H56A C56 H56B 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C10 C11 H11 120.1 . . ? C10 C11 C12 119.7(4) . . ? C12 C11 H11 120.1 . . ? C13 C12 C11 120.5(4) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C47 C46 H46 119.1 . . ? C45 C46 C47 121.8(4) . . ? C45 C46 H46 119.1 . . ? S1 C57 H57 123.6 . . ? C58 C57 S1 112.8(3) . . ? C58 C57 H57 123.6 . . ? O2 C70 O1 122.9(4) . . ? O2 C70 C68 124.9(4) . . ? O1 C70 C68 112.2(4) . . ? C68 C67 H67 119.2 . . ? C68 C67 C66 121.6(4) . . ? C66 C67 H67 119.2 . . ? O1 C71 H71A 109.5 . . ? O1 C71 H71B 109.5 . . ? O1 C71 H71C 109.5 . . ? H71A C71 H71B 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C65 C66 C67 117.3(4) . . ? C65 C66 H66 121.4 . . ? C67 C66 H66 121.4 . . ? Cl00 C02I H02A 109.3 . . ? Cl00 C02I H02B 109.3 . . ? Cl1 C02I Cl00 111.5(3) . . ? Cl1 C02I H02A 109.3 . . ? Cl1 C02I H02B 109.3 . . ? H02A C02I H02B 108.0 . . ? Cl4 C02J H02E 108.8 . . ? Cl4 C02J H02F 108.8 . . ? Cl5 C02J Cl4 113.8(3) . . ? Cl5 C02J H02E 108.8 . . ? Cl5 C02J H02F 108.8 . . ? H02E C02J H02F 107.7 . . ? Cl2 C02K Cl3 113.2(4) . . ? Cl2 C02K H02C 108.9 . . ? Cl2 C02K H02D 108.9 . . ? Cl3 C02K H02C 108.9 . . ? Cl3 C02K H02D 108.9 . . ? H02C C02K H02D 107.8 . . ? H0AA O0AA H0AB 104.5 . . ? 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 Ir1 O3 2.173(2) . ? Ir1 O4 2.138(2) . ? Ir1 N1 2.053(3) . ? Ir1 N3 2.073(3) . ? Ir1 C1 1.993(3) . ? Ir1 C28 1.979(3) . ? S1 C60 1.698(4) . ? S1 C57 1.725(5) . ? Cl00 C02I 1.769(5) . ? Cl1 C02I 1.752(6) . ? Cl2 C02K 1.750(6) . ? Cl3 C02K 1.757(7) . ? Cl4 C02J 1.768(6) . ? Cl5 C02J 1.756(6) . ? O3 C61 1.276(4) . ? O4 C63 1.268(4) . ? O5 C3 1.368(4) . ? O5 C55 1.426(4) . ? N1 C34 1.341(4) . ? N1 C54 1.388(4) . ? O6 C30 1.372(4) . ? O6 C56 1.420(5) . ? N3 C7 1.348(4) . ? N3 C27 1.387(4) . ? N2 C34 1.369(4) . ? N2 C41 1.398(5) . ? N2 C35 1.444(4) . ? C34 C33 1.452(5) . ? O2 C70 1.211(5) . ? N4 C7 1.362(4) . ? N4 C14 1.403(4) . ? N4 C8 1.432(4) . ? C1 C2 1.400(5) . ? C1 C6 1.418(4) . ? C33 C28 1.432(4) . ? C33 C32 1.400(5) . ? C28 C29 1.386(5) . ? C53 C48 1.422(5) . ? C53 C52 1.411(5) . ? C53 C54 1.438(5) . ? C42 C41 1.439(5) . ? C42 C43 1.414(5) . ? C42 C47 1.427(5) . ? C41 C54 1.381(5) . ? C48 C47 1.460(5) . ? C48 C49 1.413(5) . ? O1 C70 1.343(5) . ? O1 C71 1.439(5) . ? C65 H65 0.9500 . ? C65 C64 1.447(5) . ? C65 C66 1.294(5) . ? C3 C2 1.388(5) . ? C3 C4 1.395(5) . ? C52 H52 0.9500 . ? C52 C51 1.376(5) . ? C2 H2 0.9500 . ? C7 C6 1.449(5) . ? C14 C27 1.382(4) . ? C14 C15 1.429(5) . ? C30 C29 1.393(5) . ? C30 C31 1.396(5) . ? C9 H9 0.9500 . ? C9 C8 1.390(5) . ? C9 C10 1.384(5) . ? C27 C26 1.434(5) . ? C35 C36 1.385(5) . ? C35 C40 1.391(5) . ? C29 H29 0.9500 . ? C32 H32 0.9500 . ? C32 C31 1.393(5) . ? C43 H43 0.9500 . ? C43 C44 1.384(5) . ? C15 C16 1.421(5) . ? C15 C20 1.421(5) . ? C60 C61 1.473(5) . ? C60 C59 1.434(6) . ? C61 C62 1.411(5) . ? C6 C5 1.405(5) . ? C8 C13 1.388(5) . ? C26 C25 1.407(5) . ? C26 C21 1.416(5) . ? C4 H4 0.9500 . ? C4 C5 1.380(5) . ? C5 H5 0.9500 . ? C47 C46 1.421(5) . ? C18 H18 0.9500 . ? C18 C19 1.379(5) . ? C18 C17 1.391(6) . ? C36 H36 0.9500 . ? C36 C37 1.387(5) . ? C51 H51 0.9500 . ? C51 C50 1.409(5) . ? C62 H62 0.9500 . ? C62 C63 1.396(5) . ? C63 C64 1.499(5) . ? C16 H16 0.9500 . ? C16 C17 1.374(5) . ? C20 C19 1.409(5) . ? C20 C21 1.466(5) . ? C68 C69 1.400(5) . ? C68 C70 1.491(5) . ? C68 C67 1.373(5) . ? C19 H19 0.9500 . ? C25 H25 0.9500 . ? C25 C24 1.376(5) . ? C59 H59 0.9500 . ? C59 C58 1.454(5) . ? C10 H10 0.9500 . ? C10 C11 1.396(6) . ? C37 H37 0.9500 . ? C37 C38 1.381(6) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C64 C69 1.395(5) . ? C22 H22 0.9500 . ? C22 C21 1.410(5) . ? C22 C23 1.382(5) . ? C40 H40 0.9500 . ? C40 C39 1.396(5) . ? C50 H50 0.9500 . ? C50 C49 1.377(5) . ? C17 H17 0.9500 . ? C24 H24 0.9500 . ? C24 C23 1.396(5) . ? C49 H49 0.9500 . ? C58 H58 0.9500 . ? C58 C57 1.363(6) . ? C23 H23 0.9500 . ? C13 H13 0.9500 . ? C13 C12 1.386(5) . ? C31 H31 0.9500 . ? C39 H39 0.9500 . ? C39 C38 1.383(6) . ? C69 H69 0.9500 . ? C38 H38 0.9500 . ? C44 H44 0.9500 . ? C44 C45 1.398(6) . ? C45 H45 0.9500 . ? C45 C46 1.374(6) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C11 H11 0.9500 . ? C11 C12 1.396(6) . ? C12 H12 0.9500 . ? C46 H46 0.9500 . ? C57 H57 0.9500 . ? C67 H67 0.9500 . ? C67 C66 1.379(6) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C66 H66 0.9500 . ? C02I H02A 0.9900 . ? C02I H02B 0.9900 . ? C02J H02E 0.9900 . ? C02J H02F 0.9900 . ? C02K H02C 0.9900 . ? C02K H02D 0.9900 . ? O0AA H0AA 0.8494 . ? O0AA H0AB 0.8498 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ir1 O3 C61 C60 -158.4(2) . . . . ? Ir1 O3 C61 C62 20.9(5) . . . . ? Ir1 O4 C63 C62 -2.8(5) . . . . ? Ir1 O4 C63 C64 174.5(2) . . . . ? Ir1 N1 C34 N2 -169.0(2) . . . . ? Ir1 N1 C34 C33 16.4(4) . . . . ? Ir1 N1 C54 C53 -15.3(6) . . . . ? Ir1 N1 C54 C41 165.7(3) . . . . ? Ir1 N3 C7 N4 -165.4(2) . . . . ? Ir1 N3 C7 C6 16.6(4) . . . . ? Ir1 N3 C27 C14 158.9(3) . . . . ? Ir1 N3 C27 C26 -28.4(6) . . . . ? Ir1 C1 C2 C3 -177.9(3) . . . . ? Ir1 C1 C6 C7 -7.8(4) . . . . ? Ir1 C1 C6 C5 177.2(3) . . . . ? Ir1 C28 C29 C30 -168.0(3) . . . . ? S1 C60 C61 O3 7.3(4) . . . . ? S1 C60 C61 C62 -172.1(3) . . . . ? S1 C60 C59 C58 -1.6(4) . . . . ? O3 C61 C62 C63 -5.2(6) . . . . ? O4 C63 C64 C65 -6.5(5) . . . . ? O4 C63 C64 C69 174.7(3) . . . . ? O5 C3 C2 C1 -179.7(3) . . . . ? O5 C3 C4 C5 179.6(3) . . . . ? N1 C34 C33 C28 -1.4(4) . . . . ? N1 C34 C33 C32 174.3(3) . . . . ? O6 C30 C29 C28 177.9(3) . . . . ? O6 C30 C31 C32 -178.8(4) . . . . ? N3 C7 C6 C1 -6.4(5) . . . . ? N3 C7 C6 C5 168.1(3) . . . . ? N3 C27 C26 C25 -8.0(6) . . . . ? N3 C27 C26 C21 178.2(3) . . . . ? N2 C34 C33 C28 -174.7(3) . . . . ? N2 C34 C33 C32 1.1(6) . . . . ? N2 C41 C54 N1 1.7(4) . . . . ? N2 C41 C54 C53 -177.4(3) . . . . ? N2 C35 C36 C37 -176.2(3) . . . . ? N2 C35 C40 C39 176.8(3) . . . . ? C34 N1 C54 C53 175.9(3) . . . . ? C34 N1 C54 C41 -3.1(4) . . . . ? C34 N2 C41 C42 -179.9(4) . . . . ? C34 N2 C41 C54 0.4(4) . . . . ? C34 N2 C35 C36 97.9(4) . . . . ? C34 N2 C35 C40 -79.0(4) . . . . ? C34 C33 C28 Ir1 -15.2(4) . . . . ? C34 C33 C28 C29 173.4(3) . . . . ? C34 C33 C32 C31 -173.6(4) . . . . ? N4 C7 C6 C1 176.1(4) . . . . ? N4 C7 C6 C5 -9.4(6) . . . . ? N4 C14 C27 N3 2.1(4) . . . . ? N4 C14 C27 C26 -171.3(3) . . . . ? N4 C14 C15 C16 -1.5(6) . . . . ? N4 C14 C15 C20 -178.3(3) . . . . ? N4 C8 C13 C12 175.2(3) . . . . ? C1 C6 C5 C4 1.0(5) . . . . ? C33 C28 C29 C30 2.2(5) . . . . ? C33 C32 C31 C30 -0.2(6) . . . . ? C28 C33 C32 C31 1.7(5) . . . . ? C53 C48 C47 C42 0.9(5) . . . . ? C53 C48 C47 C46 179.1(4) . . . . ? C53 C48 C49 C50 -0.8(6) . . . . ? C53 C52 C51 C50 0.0(6) . . . . ? C42 C41 C54 N1 -178.0(3) . . . . ? C42 C41 C54 C53 2.9(5) . . . . ? C42 C43 C44 C45 0.4(6) . . . . ? C42 C47 C46 C45 1.2(6) . . . . ? C41 N2 C34 N1 -2.4(4) . . . . ? C41 N2 C34 C33 171.2(3) . . . . ? C41 N2 C35 C36 -95.1(4) . . . . ? C41 N2 C35 C40 88.0(5) . . . . ? C41 C42 C43 C44 179.6(4) . . . . ? C41 C42 C47 C48 -2.0(5) . . . . ? C41 C42 C47 C46 179.6(3) . . . . ? C48 C53 C52 C51 -1.1(5) . . . . ? C48 C53 C54 N1 177.2(3) . . . . ? C48 C53 C54 C41 -4.0(5) . . . . ? C48 C47 C46 C45 -177.2(4) . . . . ? C65 C64 C69 C68 -1.3(5) . . . . ? C3 C4 C5 C6 0.0(5) . . . . ? C52 C53 C48 C47 -176.8(3) . . . . ? C52 C53 C48 C49 1.5(5) . . . . ? C52 C53 C54 N1 -4.0(6) . . . . ? C52 C53 C54 C41 174.9(3) . . . . ? C52 C51 C50 C49 0.8(6) . . . . ? C54 N1 C34 N2 3.4(4) . . . . ? C54 N1 C34 C33 -171.2(3) . . . . ? C54 C53 C48 C47 2.1(5) . . . . ? C54 C53 C48 C49 -179.6(3) . . . . ? C54 C53 C52 C51 -179.9(3) . . . . ? C2 C1 C6 C7 173.9(3) . . . . ? C2 C1 C6 C5 -1.1(5) . . . . ? C2 C3 C4 C5 -0.8(5) . . . . ? C7 N3 C27 C14 -2.4(4) . . . . ? C7 N3 C27 C26 170.2(3) . . . . ? C7 N4 C14 C27 -1.0(4) . . . . ? C7 N4 C14 C15 176.0(4) . . . . ? C7 N4 C8 C9 97.7(4) . . . . ? C7 N4 C8 C13 -79.0(4) . . . . ? C7 C6 C5 C4 -173.0(4) . . . . ? C14 N4 C7 N3 -0.5(4) . . . . ? C14 N4 C7 C6 177.2(4) . . . . ? C14 N4 C8 C9 -79.3(5) . . . . ? C14 N4 C8 C13 104.0(4) . . . . ? C14 C27 C26 C25 164.0(3) . . . . ? C14 C27 C26 C21 -9.9(5) . . . . ? C14 C15 C16 C17 -173.1(3) . . . . ? C14 C15 C20 C19 171.6(3) . . . . ? C14 C15 C20 C21 -8.6(5) . . . . ? C9 C8 C13 C12 -1.4(6) . . . . ? C9 C10 C11 C12 -0.7(6) . . . . ? C27 N3 C7 N4 1.8(4) . . . . ? C27 N3 C7 C6 -176.2(3) . . . . ? C27 C14 C15 C16 175.0(3) . . . . ? C27 C14 C15 C20 -1.8(5) . . . . ? C27 C26 C25 C24 -175.4(3) . . . . ? C27 C26 C21 C20 -0.4(5) . . . . ? C27 C26 C21 C22 175.7(3) . . . . ? C35 N2 C34 N1 167.0(3) . . . . ? C35 N2 C34 C33 -19.3(6) . . . . ? C35 N2 C41 C42 11.5(6) . . . . ? C35 N2 C41 C54 -168.2(3) . . . . ? C35 C36 C37 C38 -0.2(6) . . . . ? C35 C40 C39 C38 -0.8(6) . . . . ? C29 C30 C31 C32 -0.4(6) . . . . ? C32 C33 C28 Ir1 168.7(3) . . . . ? C32 C33 C28 C29 -2.7(5) . . . . ? C43 C42 C41 N2 0.6(6) . . . . ? C43 C42 C41 C54 -179.8(3) . . . . ? C43 C42 C47 C48 178.0(3) . . . . ? C43 C42 C47 C46 -0.4(5) . . . . ? C43 C44 C45 C46 0.4(7) . . . . ? C15 C14 C27 N3 -175.1(3) . . . . ? C15 C14 C27 C26 11.4(5) . . . . ? C15 C16 C17 C18 0.7(6) . . . . ? C15 C20 C19 C18 3.2(6) . . . . ? C15 C20 C21 C26 9.8(5) . . . . ? C15 C20 C21 C22 -166.2(3) . . . . ? C60 S1 C57 C58 0.4(4) . . . . ? C60 C61 C62 C63 174.1(3) . . . . ? C60 C59 C58 C57 1.9(5) . . . . ? C61 C60 C59 C58 -178.9(4) . . . . ? C61 C62 C63 O4 -5.2(6) . . . . ? C61 C62 C63 C64 177.7(3) . . . . ? C6 C1 C2 C3 0.2(5) . . . . ? C8 N4 C7 N3 -178.0(3) . . . . ? C8 N4 C7 C6 -0.4(6) . . . . ? C8 N4 C14 C27 176.4(3) . . . . ? C8 N4 C14 C15 -6.6(6) . . . . ? C8 C9 C10 C11 0.2(6) . . . . ? C8 C13 C12 C11 0.8(6) . . . . ? C26 C25 C24 C23 0.7(5) . . . . ? C4 C3 C2 C1 0.7(5) . . . . ? C47 C42 C41 N2 -179.4(3) . . . . ? C47 C42 C41 C54 0.2(5) . . . . ? C47 C42 C43 C44 -0.4(6) . . . . ? C47 C48 C49 C50 177.5(4) . . . . ? C36 C35 C40 C39 0.0(6) . . . . ? C36 C37 C38 C39 -0.6(6) . . . . ? C51 C50 C49 C48 -0.4(6) . . . . ? C62 C63 C64 C65 170.9(3) . . . . ? C62 C63 C64 C69 -7.8(5) . . . . ? C63 C64 C69 C68 177.5(3) . . . . ? C16 C15 C20 C19 -5.4(5) . . . . ? C16 C15 C20 C21 174.4(3) . . . . ? C20 C15 C16 C17 3.6(5) . . . . ? C68 C67 C66 C65 -1.3(6) . . . . ? C19 C18 C17 C16 -3.0(6) . . . . ? C19 C20 C21 C26 -170.4(3) . . . . ? C19 C20 C21 C22 13.6(5) . . . . ? C25 C26 C21 C20 -174.5(3) . . . . ? C25 C26 C21 C22 1.6(5) . . . . ? C25 C24 C23 C22 0.3(6) . . . . ? C59 C60 C61 O3 -175.6(4) . . . . ? C59 C60 C61 C62 5.1(6) . . . . ? C59 C58 C57 S1 -1.4(5) . . . . ? C10 C9 C8 N4 -175.7(3) . . . . ? C10 C9 C8 C13 0.9(5) . . . . ? C10 C11 C12 C13 0.2(7) . . . . ? C55 O5 C3 C2 1.8(5) . . . . ? C55 O5 C3 C4 -178.6(3) . . . . ? C64 C65 C66 C67 -0.2(6) . . . . ? C21 C26 C25 C24 -1.7(5) . . . . ? C21 C20 C19 C18 -176.6(4) . . . . ? C21 C22 C23 C24 -0.4(6) . . . . ? C40 C35 C36 C37 0.5(5) . . . . ? C40 C39 C38 C37 1.1(7) . . . . ? C17 C18 C19 C20 1.0(6) . . . . ? C49 C48 C47 C42 -177.3(4) . . . . ? C49 C48 C47 C46 0.9(6) . . . . ? C23 C22 C21 C26 -0.6(5) . . . . ? C23 C22 C21 C20 175.5(3) . . . . ? C31 C30 C29 C28 -0.6(6) . . . . ? C69 C68 C70 O2 -0.8(6) . . . . ? C69 C68 C70 O1 177.9(3) . . . . ? C69 C68 C67 C66 1.5(6) . . . . ? C44 C45 C46 C47 -1.2(7) . . . . ? C56 O6 C30 C29 177.1(3) . . . . ? C56 O6 C30 C31 -4.4(6) . . . . ? C57 S1 C60 C61 178.3(3) . . . . ? C57 S1 C60 C59 0.8(3) . . . . ? C70 C68 C69 C64 -177.0(3) . . . . ? C70 C68 C67 C66 178.3(4) . . . . ? C67 C68 C69 C64 0.0(5) . . . . ? C67 C68 C70 O2 -177.7(4) . . . . ? C67 C68 C70 O1 1.0(5) . . . . ? C71 O1 C70 O2 3.4(6) . . . . ? C71 O1 C70 C68 -175.4(4) . . . . ? C66 C65 C64 C63 -177.3(4) . . . . ? C66 C65 C64 C69 1.5(5) . . . . ?