#------------------------------------------------------------------------------ #$Date: 2026-06-01 23:55:06 +0100 (Mon, 01 Jun 2026) $ #$Revision: 306155 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/10/7721061.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_7721061 loop_ _publ_author_name 'Wang, Yue' 'Wu, Yifan' 'Wang, Longxiang' 'Sang, Linxue' 'Cao, Jianfang' 'Furuta, Hiroyuki' 'Xue, Songlin' 'Feng, Ru' _publ_section_title ; Iridium(I)-Corrorin Complexes as Green-Light Photosensitizers for Singlet Oxygen ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D6DT00801A _journal_year 2026 _chemical_formula_moiety 'C66 H28 Cl2 F20 Ir N7' _chemical_formula_sum 'C66 H28 Cl2 F20 Ir N7' _chemical_formula_weight 1562.05 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_block_doi 10.5517/ccdc.csd.cc2pwpr1 _audit_creation_date 2025-01-13 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _audit_update_record ; 2025-10-31 deposited with the CCDC. 2026-06-01 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 108.886(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 17.1169(16) _cell_length_b 21.148(2) _cell_length_c 20.1177(19) _cell_measurement_reflns_used 9975 _cell_measurement_temperature 193.00 _cell_measurement_theta_max 24.15 _cell_measurement_theta_min 2.30 _cell_volume 6890.3(11) _computing_cell_refinement 'SAINT V8.41 (Bruker, 2024)' _computing_data_collection 'APEX6 V2024.9-0 (Bruker, 2024)' _computing_data_reduction 'SAINT V8.41 (Bruker, 2024)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2019/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 193.00 _diffrn_detector CPAD _diffrn_detector_area_resol_mean 7.41 _diffrn_detector_type 'Bruker PHOTON II' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker D8 VENTURE TXS PHOTON II' _diffrn_measurement_method '\w and \f shutterless scans' _diffrn_measurement_specimen_support 'nylon loop' _diffrn_radiation_monochromator 'Helios Multi-layer Optic' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0940 _diffrn_reflns_av_unetI/netI 0.0910 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 50857 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.350 _diffrn_reflns_theta_min 1.896 _diffrn_source TXS _diffrn_source_current 40.0 _diffrn_source_power 1.8 _diffrn_source_type 'Rotaing Anode' _diffrn_source_voltage 45.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.113 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.5923 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1290 before and 0.0714 after correction. The Ratio of minimum to maximum transmission is 0.7944. The \l/2 correction factor is Not present. ; _exptl_crystal_density_diffrn 1.506 _exptl_crystal_description block _exptl_crystal_F_000 3056 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _refine_diff_density_max 0.839 _refine_diff_density_min -0.829 _refine_diff_density_rms 0.118 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 865 _refine_ls_number_reflns 12630 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.022 _refine_ls_R_factor_all 0.0970 _refine_ls_R_factor_gt 0.0559 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0389P)^2^+18.0059P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1079 _refine_ls_wR_factor_ref 0.1249 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8413 _reflns_number_total 12630 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00801a2.cif _cod_data_source_block 250110lu_lgpz0687657_0m _cod_depositor_comments ; The following automatic conversions were performed: data item '_diffrn_radiation_probe' value 'X-ray' was changed to 'x-ray' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas ; _cod_original_cell_volume 6890.4(12) _cod_database_code 7721061 _shelx_shelxl_version_number 2019/3 _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 0.833 _shelx_estimated_absorpt_t_min 0.771 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups 2.a Ternary CH refined with riding coordinates: C1(H1), C4(H4), C5(H5A), C8(H8) 2.b Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B), C7(H7A,H7B) 2.c Aromatic/amide H refined with riding coordinates: N2(H2), N5(H5), C17(H17), C18(H18), C19(H19), C21(H21), C31(H31), C32(H32), C37(H37), C39(H39), C41(H41), C42(H42), C54(H54), C58(H58), C59(H59), C60(H60) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL 250110lu_lgpz0687657_0m_a.res in P2(1)/n 250110lu_lgpz0687657_0m.res created by SHELXL-2019/3 at 19:41:05 on 13-Jan-2025 REM Old TITL 250110lu_lgpz0687657_0m_a.res in Pn REM SHELXT solution in P2(1)/n: R1 0.168, Rweak 0.027, Alpha 0.067 REM 0.788 for 411 systematic absences, Orientation as input REM Formula found by SHELXT: C73 N12 O12 Cl2 Ir CELL 0.71073 17.1169 21.1481 20.1177 90 108.886 90 ZERR 4 0.0016 0.0023 0.0019 0 0.003 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Cl F Ir N UNIT 264 112 8 80 4 28 L.S. 10 0 0 PLAN 8 SIZE 0.09 0.12 0.13 TEMP -80.15 CONF list 4 MORE -1 ABIN BOND $H fmap 2 53 acta SIZE 0.09 0.12 0.13 SHEL 999 0.83 OMIT 0 0 2 REM REM REM WGHT 0.038900 18.005899 FVAR 0.18833 IR1 5 0.688873 0.872341 0.858875 11.00000 0.03287 0.03286 = 0.03096 -0.00201 0.00974 0.00350 CL1 3 0.240666 0.611241 0.638524 11.00000 0.04205 0.08169 = 0.05346 0.01021 0.02302 0.00488 CL2 3 0.512832 0.482202 0.626404 11.00000 0.06461 0.05940 = 0.09094 0.00147 0.03962 0.01175 F1 4 0.956124 0.827675 0.864429 11.00000 0.04459 0.04399 = 0.06188 -0.01112 0.00906 -0.01102 F2 4 1.097661 0.777490 0.860081 11.00000 0.03741 0.08044 = 0.11335 0.00525 0.02193 -0.00448 F3 4 1.103262 0.655942 0.820424 11.00000 0.05621 0.08727 = 0.13201 0.00204 0.04708 0.02724 F4 4 0.965832 0.583275 0.788181 11.00000 0.07742 0.04737 = 0.07214 -0.00331 0.02350 0.02385 F5 4 0.824311 0.631938 0.795399 11.00000 0.04645 0.04158 = 0.06619 -0.00874 0.00403 0.00160 F6 4 0.727924 0.647457 0.565787 11.00000 0.07135 0.04019 = 0.17982 -0.00517 0.07411 0.00438 F7 4 0.830321 0.671520 0.493320 11.00000 0.09501 0.11818 = 0.23291 -0.09310 0.12062 -0.02901 F8 4 0.836281 0.788732 0.440927 11.00000 0.09429 0.23860 = 0.10141 -0.02315 0.07807 -0.04774 F9 4 0.739585 0.883050 0.465091 11.00000 0.10828 0.13707 = 0.13535 0.07295 0.05715 -0.01383 F10 4 0.638832 0.858220 0.537971 11.00000 0.06752 0.06796 = 0.15353 0.05092 0.06041 0.02220 F11 4 0.221474 0.865468 0.506014 11.00000 0.04131 0.10592 = 0.12094 -0.06219 0.00393 -0.00630 F12 4 0.079117 0.914695 0.512683 11.00000 0.02574 0.16014 = 0.16382 -0.05140 0.00205 0.00366 F13 4 0.082424 1.015629 0.595644 11.00000 0.05881 0.13768 = 0.12332 -0.00595 0.03644 0.04232 F14 4 0.228322 1.067010 0.672432 11.00000 0.08801 0.10606 = 0.14245 -0.05385 0.05962 0.01426 F15 4 0.370029 1.017700 0.666230 11.00000 0.05070 0.07699 = 0.11329 -0.05749 0.02643 -0.01604 F16 4 0.411764 0.897604 0.838420 11.00000 0.06837 0.07154 = 0.05399 -0.01163 0.02546 0.02075 F17 4 0.440246 0.932501 0.970746 11.00000 0.07414 0.10986 = 0.08438 -0.05424 0.04069 -0.00102 F18 4 0.536648 0.860754 1.078441 11.00000 0.07745 0.17564 = 0.04297 -0.04244 0.02837 -0.02740 F19 4 0.609273 0.754928 1.049359 11.00000 0.07166 0.14035 = 0.03626 0.01582 0.01242 -0.00683 F20 4 0.585799 0.720390 0.917423 11.00000 0.05791 0.06684 = 0.04274 0.01397 0.01100 0.01086 N1 6 0.284207 0.434168 0.602979 11.00000 0.09065 0.07852 = 0.09620 -0.02822 0.03995 -0.03801 N2 6 0.519172 0.682684 0.624031 11.00000 0.03153 0.05289 = 0.03775 -0.00551 0.01638 -0.00699 AFIX 43 H2 2 0.522308 0.704774 0.661878 11.00000 -1.20000 AFIX 0 N3 6 0.450411 0.703896 0.713459 11.00000 0.03474 0.04770 = 0.02834 -0.00083 0.01427 -0.00448 N4 6 0.505524 0.856576 0.636005 11.00000 0.02667 0.02656 = 0.03438 -0.00353 0.00641 0.00130 N5 6 0.469162 0.913010 0.508389 11.00000 0.03771 0.03800 = 0.03821 -0.00488 0.01001 -0.00193 AFIX 43 H5 2 0.507249 0.888576 0.536586 11.00000 -1.20000 AFIX 0 N6 6 0.670736 0.802940 0.780214 11.00000 0.03187 0.03421 = 0.02788 0.00782 0.01070 0.01024 N7 6 0.751455 0.802451 0.927441 11.00000 0.04004 0.03747 = 0.02796 -0.00172 0.01032 0.00370 C1 1 0.689926 0.943453 0.785675 11.00000 0.04866 0.03926 = 0.04000 0.00017 0.01553 0.00205 AFIX 13 H1 2 0.685098 0.926885 0.737952 11.00000 -1.20000 AFIX 0 C2 1 0.761284 0.986168 0.815508 11.00000 0.06312 0.05604 = 0.09867 0.01048 0.03665 -0.00304 AFIX 23 H2A 2 0.749041 1.027453 0.791136 11.00000 -1.20000 H2B 2 0.810055 0.968053 0.806192 11.00000 -1.20000 AFIX 0 C3 1 0.782473 0.997002 0.893816 11.00000 0.04909 0.05153 = 0.08091 -0.02235 0.02032 -0.00462 AFIX 23 H3A 2 0.842329 1.005601 0.914543 11.00000 -1.20000 H3B 2 0.752164 1.034481 0.902025 11.00000 -1.20000 AFIX 0 C4 1 0.760315 0.940443 0.929151 11.00000 0.04582 0.03709 = 0.04990 -0.00305 0.00240 0.00776 AFIX 13 H4 2 0.808105 0.922124 0.967210 11.00000 -1.20000 AFIX 0 C5 1 0.684647 0.933346 0.940926 11.00000 0.05956 0.03566 = 0.04190 -0.00816 0.02261 -0.00084 AFIX 13 H5A 2 0.688664 0.911041 0.985743 11.00000 -1.20000 AFIX 0 C6 1 0.618922 0.983712 0.920542 11.00000 0.05978 0.04164 = 0.06684 -0.01925 0.03543 0.00803 AFIX 23 H6A 2 0.639906 1.022585 0.947918 11.00000 -1.20000 H6B 2 0.569928 0.969176 0.932199 11.00000 -1.20000 AFIX 0 C7 1 0.593724 0.998780 0.842282 11.00000 0.04449 0.03794 = 0.07795 -0.00243 0.01670 0.01485 AFIX 23 H7A 2 0.533457 1.006533 0.824527 11.00000 -1.20000 H7B 2 0.621569 1.038295 0.836034 11.00000 -1.20000 AFIX 0 C8 1 0.614206 0.947500 0.798523 11.00000 0.04369 0.03862 = 0.04456 -0.00288 0.01235 0.00172 AFIX 13 H8 2 0.565813 0.932604 0.758588 11.00000 -1.20000 AFIX 0 C9 1 0.886476 0.730801 0.832263 11.00000 0.03270 0.03943 = 0.02958 -0.00048 0.00401 -0.00280 C10 1 0.957422 0.766717 0.846907 11.00000 0.03951 0.03203 = 0.04394 -0.00318 0.01245 0.01021 C11 1 1.030104 0.741755 0.844315 11.00000 0.03219 0.04864 = 0.06225 0.00280 0.00250 -0.00330 C12 1 1.033148 0.681443 0.823871 11.00000 0.04394 0.04438 = 0.06069 -0.00119 0.01868 0.01781 C13 1 0.962106 0.644254 0.805999 11.00000 0.05683 0.03242 = 0.04439 0.00181 0.01832 0.01452 C14 1 0.890957 0.669718 0.811104 11.00000 0.03674 0.04323 = 0.04775 -0.00376 0.00470 -0.00219 C15 1 0.810861 0.760536 0.841234 11.00000 0.03031 0.02028 = 0.03947 -0.00016 0.01095 -0.00029 C16 1 0.810217 0.767007 0.909087 11.00000 0.03352 0.03459 = 0.02492 0.00194 0.00566 -0.00140 C17 1 0.865465 0.739039 0.971923 11.00000 0.02902 0.04813 = 0.03893 -0.00015 0.00904 0.00327 AFIX 43 H17 2 0.912540 0.713802 0.975403 11.00000 -1.20000 AFIX 0 C18 1 0.837493 0.755585 1.025042 11.00000 0.05860 0.03958 = 0.03772 0.01131 0.00802 -0.00712 AFIX 43 H18 2 0.860473 0.743071 1.072779 11.00000 -1.20000 AFIX 0 C19 1 0.767840 0.794889 0.996710 11.00000 0.05065 0.03677 = 0.02921 0.00088 0.00950 0.00175 AFIX 43 H19 2 0.736848 0.813429 1.023212 11.00000 -1.20000 AFIX 0 C20 1 0.744794 0.776039 0.780084 11.00000 0.03003 0.02817 = 0.03677 0.00072 0.00548 0.00243 C21 1 0.737502 0.756232 0.711919 11.00000 0.02115 0.03722 = 0.04009 -0.00079 0.01519 0.00037 AFIX 43 H21 2 0.780020 0.738230 0.697167 11.00000 -1.20000 AFIX 0 C22 1 0.656420 0.767761 0.669643 11.00000 0.03044 0.03017 = 0.02604 -0.00136 0.01144 -0.00101 C23 1 0.625066 0.740464 0.598170 11.00000 0.02261 0.03058 = 0.03939 0.00112 0.00993 0.00045 C24 1 0.677237 0.751287 0.552477 11.00000 0.02947 0.04711 = 0.02350 -0.00764 0.01137 -0.00295 C25 1 0.683050 0.810221 0.525247 11.00000 0.04549 0.06092 = 0.04960 0.01816 0.02802 0.00637 C26 1 0.735908 0.822888 0.487641 11.00000 0.05448 0.09142 = 0.06253 0.03199 0.02827 -0.01418 C27 1 0.784290 0.775911 0.477221 11.00000 0.05203 0.12592 = 0.07934 -0.02754 0.05049 -0.02407 C28 1 0.780348 0.717094 0.502351 11.00000 0.04981 0.10371 = 0.10058 -0.06525 0.04439 -0.02414 C29 1 0.727096 0.705014 0.540314 11.00000 0.04376 0.05961 = 0.06535 -0.01406 0.02956 -0.00731 C30 1 0.563591 0.696911 0.580324 11.00000 0.03214 0.03862 = 0.03081 0.00169 0.01868 -0.00162 C31 1 0.536453 0.650459 0.524687 11.00000 0.02799 0.05457 = 0.03115 -0.00767 0.01542 -0.00428 AFIX 43 H31 2 0.554477 0.648130 0.484780 11.00000 -1.20000 AFIX 0 C32 1 0.481528 0.610954 0.538350 11.00000 0.03479 0.04766 = 0.03924 -0.00866 0.01185 -0.00072 AFIX 43 H32 2 0.455190 0.576029 0.510301 11.00000 -1.20000 AFIX 0 C33 1 0.469816 0.631218 0.603374 11.00000 0.03133 0.04564 = 0.03639 -0.00064 0.00932 -0.01400 C34 1 0.423647 0.608566 0.643904 11.00000 0.03332 0.03765 = 0.03424 -0.00305 0.01213 -0.01055 C35 1 0.377205 0.548676 0.628862 11.00000 0.03990 0.03405 = 0.03396 -0.00227 0.01182 -0.00435 C36 1 0.409814 0.490658 0.618899 11.00000 0.06228 0.03780 = 0.04947 -0.00713 0.02837 -0.00463 C37 1 0.362348 0.436583 0.605369 11.00000 0.10205 0.05357 = 0.09366 -0.02258 0.05254 -0.00671 AFIX 43 H37 2 0.387341 0.398542 0.597222 11.00000 -1.20000 AFIX 0 C38 1 0.294115 0.544393 0.626196 11.00000 0.03920 0.06091 = 0.03954 -0.00237 0.01536 -0.00412 C39 1 0.251714 0.487732 0.614400 11.00000 0.04979 0.08608 = 0.06739 -0.01066 0.01808 -0.02676 AFIX 43 H39 2 0.196270 0.487453 0.614545 11.00000 -1.20000 AFIX 0 C40 1 0.425523 0.644422 0.705715 11.00000 0.03243 0.04268 = 0.03515 0.00263 0.01279 -0.00031 C41 1 0.412664 0.621666 0.771739 11.00000 0.03981 0.04204 = 0.03219 0.00366 0.01618 -0.01029 AFIX 43 H41 2 0.393318 0.581203 0.779756 11.00000 -1.20000 AFIX 0 C42 1 0.434014 0.670049 0.817562 11.00000 0.05043 0.04232 = 0.03659 0.00914 0.01858 0.00090 AFIX 43 H42 2 0.433670 0.669900 0.864689 11.00000 -1.20000 AFIX 0 C43 1 0.457630 0.722423 0.781636 11.00000 0.04260 0.04127 = 0.02875 -0.00035 0.01597 0.00368 C44 1 0.478546 0.783983 0.797794 11.00000 0.02436 0.04457 = 0.03206 0.00120 0.01683 0.00915 C45 1 0.496322 0.806443 0.871733 11.00000 0.02812 0.04710 = 0.03475 -0.00825 0.01670 -0.00314 C46 1 0.546927 0.772025 0.927066 11.00000 0.03952 0.06659 = 0.03519 -0.00215 0.01241 0.00413 C47 1 0.560859 0.790143 0.997170 11.00000 0.04681 0.09243 = 0.03069 0.01096 0.00525 -0.01061 C48 1 0.524259 0.843761 1.010811 11.00000 0.05069 0.11672 = 0.05229 -0.02724 0.02888 -0.02297 C49 1 0.474732 0.879290 0.957463 11.00000 0.05399 0.07998 = 0.05876 -0.03586 0.03476 -0.02330 C50 1 0.462928 0.861007 0.888944 11.00000 0.03964 0.05864 = 0.04497 -0.00544 0.02404 0.00091 C51 1 0.618247 0.798049 0.714244 11.00000 0.02420 0.02324 = 0.02724 0.00229 0.00409 0.00270 C52 1 0.535715 0.824803 0.696055 11.00000 0.03468 0.02880 = 0.03778 -0.00307 0.01366 0.00179 C53 1 0.479034 0.826821 0.737961 11.00000 0.02916 0.03691 = 0.03166 -0.00208 0.01723 -0.00793 C54 1 0.413269 0.860261 0.699036 11.00000 0.02696 0.04699 = 0.03860 0.00070 0.01026 0.00203 AFIX 43 H54 2 0.365212 0.869448 0.711099 11.00000 -1.20000 AFIX 0 C55 1 0.428788 0.879702 0.635617 11.00000 0.02604 0.02656 = 0.03426 0.00208 0.01031 0.00436 C56 1 0.379708 0.914954 0.581288 11.00000 0.02405 0.02864 = 0.03770 -0.00691 0.00372 0.00448 C57 1 0.397855 0.931220 0.519672 11.00000 0.02931 0.03482 = 0.03329 0.00140 0.00824 0.01193 C58 1 0.355227 0.967456 0.462427 11.00000 0.04976 0.04496 = 0.04736 0.00736 0.01279 0.00730 AFIX 43 H58 2 0.302856 0.986490 0.455224 11.00000 -1.20000 AFIX 0 C59 1 0.401882 0.971679 0.416385 11.00000 0.06846 0.03780 = 0.04523 0.00420 0.01731 0.00177 AFIX 43 H59 2 0.387132 0.993418 0.372741 11.00000 -1.20000 AFIX 0 C60 1 0.472606 0.938216 0.447141 11.00000 0.05941 0.04459 = 0.03609 -0.00263 0.02323 -0.00542 AFIX 43 H60 2 0.516907 0.933330 0.428818 11.00000 -1.20000 AFIX 0 C61 1 0.300082 0.940304 0.586365 11.00000 0.02778 0.03391 = 0.04310 -0.00022 0.00504 0.00589 C62 1 0.225995 0.915608 0.548077 11.00000 0.04045 0.06664 = 0.06281 -0.02354 0.00388 0.01898 C63 1 0.151639 0.940323 0.550899 11.00000 0.03145 0.07978 = 0.08885 -0.01109 0.00450 0.01106 C64 1 0.152712 0.991114 0.592245 11.00000 0.04512 0.07856 = 0.07522 -0.00078 0.02602 0.02331 C65 1 0.226849 1.016961 0.631772 11.00000 0.06276 0.05123 = 0.07536 -0.00809 0.03794 0.01091 C66 1 0.298900 0.991029 0.627717 11.00000 0.04428 0.05633 = 0.04583 0.00032 0.02108 0.01224 HKLF 4 REM 250110lu_lgpz0687657_0m_a.res in P2(1)/n REM wR2 = 0.1249, GooF = S = 1.022, Restrained GooF = 1.022 for all data REM R1 = 0.0559 for 8413 Fo > 4sig(Fo) and 0.0970 for all 12630 data REM 865 parameters refined using 0 restraints END WGHT 0.0389 18.0058 REM Highest difference peak 0.839, deepest hole -0.829, 1-sigma level 0.118 Q1 1 0.6261 0.8740 0.8786 11.00000 0.05 0.84 Q2 1 0.7532 0.8774 0.8432 11.00000 0.05 0.81 Q3 1 0.7155 0.9213 0.8354 11.00000 0.05 0.64 Q4 1 0.6576 0.8160 0.8858 11.00000 0.05 0.57 Q5 1 0.6599 0.8632 0.7775 11.00000 0.05 0.53 Q6 1 0.6642 0.8132 0.8212 11.00000 0.05 0.49 Q7 1 0.7567 0.8608 0.3797 11.00000 0.05 0.49 Q8 1 0.8619 1.0614 0.8362 11.00000 0.05 0.48 ; _shelx_res_checksum 55533 _shelx_fab_file ; -22 0 6 -2.0734 -4.3337 -22 0 8 3.2852 -1.3757 -22 0 10 0.8914 5.2633 -22 0 12 -5.6923 -1.5835 -22 1 5 0.8746 1.8032 -22 1 6 2.1920 0.5328 -22 1 7 -1.4175 -1.0120 -22 1 8 -6.0642 0.0337 -22 1 9 0.4702 -1.1568 -22 1 10 9.4071 -1.1083 -22 1 11 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10 2 14 7.6940 1.3043 10 2 15 3.7753 -2.0211 10 2 16 10.2616 -1.6103 10 2 17 -1.4626 0.8618 10 2 18 -5.0265 -0.2467 10 3 10 -0.8151 -0.2409 10 3 11 1.7411 1.2391 10 3 12 -0.8271 1.0662 10 3 13 5.7816 0.8839 10 3 14 -8.1204 -0.4098 10 3 15 -8.6060 -0.9172 10 3 16 6.3924 0.0366 10 3 17 -8.9441 0.0193 10 3 18 -4.8172 0.3260 10 4 10 -0.6490 0.5826 10 4 11 8.8115 -1.1523 10 4 12 -5.5213 0.4265 10 4 13 -0.0366 0.2673 10 4 14 2.8680 -0.9019 10 4 15 6.0714 1.3221 10 4 16 3.1376 0.1204 10 4 17 -6.6958 -0.6663 10 4 18 6.4581 -1.0382 10 5 10 -5.4194 -0.3104 10 5 11 7.1834 -0.6000 10 5 12 -2.9950 -0.5442 10 5 13 3.0676 0.1961 10 5 14 -1.7184 0.5965 10 5 15 -2.8519 0.3082 10 5 16 -2.8068 1.2938 10 5 17 0.2038 -0.0800 10 6 10 1.4301 -0.2760 10 6 11 2.1213 0.3081 10 6 12 -3.1979 -0.1035 10 6 13 -0.0593 0.3795 10 6 14 -1.5821 0.0392 10 6 15 1.4871 -1.0532 10 6 16 -3.3539 0.1505 10 6 17 4.4117 -0.4001 10 7 10 -6.4962 0.0000 10 7 11 3.3547 0.5635 10 7 12 -3.5930 0.2601 10 7 13 -5.3806 -0.6708 10 7 14 4.9202 -0.2756 10 7 15 3.4824 -0.5002 10 7 16 -5.9568 0.3350 10 7 17 2.4095 0.7153 10 8 10 -0.9146 -0.0587 10 8 11 2.5781 -0.1330 10 8 12 0.8116 -0.2576 10 8 13 4.6181 -0.0358 10 8 14 2.4232 0.0914 10 8 15 -4.1151 0.3169 10 8 16 -6.7194 -0.0570 10 8 17 1.8459 -0.0783 10 9 10 -7.1474 0.0017 10 9 11 -7.2349 -0.6035 10 9 12 1.6431 0.4145 10 9 13 6.5262 0.5206 10 9 14 0.9771 -0.2267 10 9 15 6.9037 0.5574 10 9 16 0.8621 0.0084 10 10 10 1.8903 -0.0539 10 10 11 -1.1051 0.4043 10 10 12 -2.0815 0.1544 10 10 13 -5.5233 -0.2184 10 10 14 -10.4539 -0.3656 10 10 15 3.6433 -0.3073 10 10 16 6.4781 0.4294 10 11 10 6.7119 0.2405 10 11 11 6.5772 0.4117 10 11 12 2.8636 -0.3800 10 11 13 -1.0294 -0.2706 10 11 14 -7.5127 -0.2694 10 11 15 -0.1961 -0.0281 10 12 10 3.1695 -0.1106 10 12 11 -0.9423 -0.2569 10 12 12 3.4055 0.2593 10 12 13 10.2278 -0.2450 10 12 14 -4.8759 0.2410 10 12 15 -1.7365 0.6748 10 13 10 -4.3361 -0.2932 10 13 11 -11.2332 0.1823 10 13 12 -0.4971 0.4370 10 13 13 7.0868 -0.2125 10 13 14 0.0231 0.1020 10 14 10 -7.0479 0.3616 10 14 11 -0.6191 0.2602 10 14 12 2.5449 -0.3902 10 14 13 -6.8032 -0.1661 10 14 14 0.4706 0.1058 10 15 10 -2.6173 0.1919 10 15 11 10.2622 -0.0214 10 15 12 1.5920 -0.4343 10 15 13 -0.5016 0.0096 10 16 10 3.9717 -0.1284 10 16 11 8.9721 0.0196 10 16 12 -13.3609 -0.0836 10 17 10 -5.2125 0.6092 10 17 11 1.1290 0.1065 10 17 12 5.1084 -0.6583 10 18 10 2.5291 0.3905 10 18 11 -7.9791 -0.6246 10 19 10 1.7267 0.1219 11 0 11 -2.0417 -6.4617 11 0 13 9.1619 3.3108 11 0 15 -11.8985 6.1815 11 0 17 3.1968 -3.5245 11 1 11 1.2471 -2.9187 11 1 12 -9.2004 0.4723 11 1 13 -4.4854 0.2047 11 1 14 5.0036 0.2181 11 1 15 1.3440 0.3511 11 1 16 0.3076 -1.9059 11 1 17 -3.0488 -0.9844 11 2 11 4.5291 2.0872 11 2 12 -3.3132 -1.5083 11 2 13 7.5952 -0.7086 11 2 14 2.2332 1.4300 11 2 15 -4.9281 -1.0833 11 2 16 1.6528 1.6288 11 2 17 -0.8916 0.8417 11 3 11 -3.2492 0.9553 11 3 12 -6.1332 -1.0052 11 3 13 1.0631 -0.9528 11 3 14 -3.8451 -0.9565 11 3 15 5.7421 0.5275 11 3 16 7.6844 0.1640 11 3 17 -4.0023 -0.5324 11 4 11 1.4049 -0.6043 11 4 12 -1.5615 0.9896 11 4 13 2.9650 -0.6421 11 4 14 -5.1965 -0.1253 11 4 15 5.6401 0.7575 11 4 16 1.2505 -0.6024 11 4 17 -11.4254 0.8943 11 5 11 2.7718 0.0994 11 5 12 -3.3654 0.8391 11 5 13 4.9740 0.5813 11 5 14 -5.2995 -0.1141 11 5 15 1.5418 -0.6515 11 5 16 -0.0319 -0.3167 11 6 11 3.0054 0.1848 11 6 12 -0.2433 0.1416 11 6 13 3.0621 0.0981 11 6 14 -2.8399 -0.9776 11 6 15 -1.2274 -0.0432 11 6 16 -1.0904 1.5872 11 7 11 3.7280 0.2641 11 7 12 3.2510 -0.6496 11 7 13 1.9289 -0.0954 11 7 14 -4.8142 0.5980 11 7 15 -4.0712 0.1537 11 7 16 2.5346 0.5377 11 8 11 1.9016 0.0144 11 8 12 -6.5414 0.2441 11 8 13 -7.3490 0.4031 11 8 14 5.7831 -0.4439 11 8 15 4.8132 -0.3377 11 8 16 -9.1628 0.1088 11 9 11 4.5837 -0.1476 11 9 12 -1.8735 0.9316 11 9 13 -4.2187 -0.2077 11 9 14 2.8697 -0.5551 11 9 15 3.2733 -0.0574 11 10 11 -6.5978 0.0466 11 10 12 1.5322 -0.1173 11 10 13 5.6675 -0.4234 11 10 14 4.1155 0.0145 11 10 15 -0.4750 0.4596 11 11 11 -3.1491 -0.1091 11 11 12 4.1558 -0.1456 11 11 13 -0.4805 0.0764 11 11 14 -2.2798 0.1650 11 12 11 -4.1383 0.0159 11 12 12 -0.9929 0.0948 11 12 13 -0.6292 -0.2326 11 12 14 -8.7365 0.3117 11 13 11 -2.3801 0.2458 11 13 12 2.7159 0.0005 11 13 13 0.4271 -0.4442 11 14 11 -6.5649 -0.1183 11 14 12 6.5096 0.1605 11 14 13 10.0922 0.0526 11 15 11 3.7505 -0.3359 11 15 12 -7.5524 -0.1925 11 16 11 1.9481 0.1777 12 0 12 -3.3391 5.5302 12 0 14 0.1123 -1.3371 12 0 16 4.9709 -4.8053 12 1 12 0.8620 3.0485 12 1 13 10.4750 -0.1333 12 1 14 -1.1709 0.0179 12 1 15 -8.3143 -1.1032 12 1 16 2.9914 -0.6602 12 2 12 -5.2047 -2.0082 12 2 13 -1.7536 1.4621 12 2 14 -1.8250 0.7135 12 2 15 0.9517 -0.4498 12 2 16 -4.8647 0.7080 12 3 12 0.7852 -1.2683 12 3 13 -0.2086 0.2565 12 3 14 1.1738 0.4690 12 3 15 6.2286 1.4355 12 3 16 -3.4965 -0.3264 12 4 12 -0.0886 0.6226 12 4 13 5.3197 -0.9238 12 4 14 -6.9756 1.3239 12 4 15 1.0975 0.0866 12 5 12 -0.9130 0.0550 12 5 13 0.9638 -0.9484 12 5 14 -1.0556 -0.9462 12 5 15 10.9146 -0.1315 12 6 12 5.6270 -0.1714 12 6 13 3.0743 -0.0582 12 6 14 -7.8273 -0.1731 12 6 15 -2.9965 0.9647 12 7 12 0.5951 0.1167 12 7 13 3.2110 0.6872 12 7 14 1.6966 -0.1185 12 7 15 -1.2706 -0.5014 12 8 12 6.5131 0.2110 12 8 13 -9.7815 -0.1943 12 8 14 -4.7549 -0.4180 12 8 15 7.1103 0.3545 12 9 12 -4.1428 -0.0424 12 9 13 -9.2718 -0.9675 12 9 14 4.5361 0.0061 12 10 12 -9.5512 0.1646 12 10 13 -11.1069 0.1801 12 10 14 12.5747 0.1895 12 11 12 -2.9014 0.5949 12 11 13 7.1582 -0.2207 12 12 12 1.8190 0.1191 12 12 13 7.6111 -0.1257 12 13 12 6.3942 -0.3652 12 14 12 -4.8392 0.1676 13 0 13 15.0651 -4.2947 13 0 15 -14.5449 0.8934 13 1 13 8.2500 -2.8413 13 1 14 -2.8642 0.2550 13 1 15 -4.3946 0.3812 13 2 13 1.8566 1.6237 13 2 14 -8.0775 -1.4684 13 2 15 4.3254 -0.7885 13 3 13 2.9259 1.4185 13 3 14 -0.8136 0.3738 13 4 13 -7.0957 -1.0175 13 4 14 4.2894 0.3873 13 5 13 -3.7938 -0.3290 13 5 14 -8.1646 0.9595 13 6 13 1.4184 0.1308 13 6 14 6.1167 0.3333 13 7 13 -4.5983 -0.3059 13 7 14 -1.6897 -0.8445 13 8 13 2.2776 -0.0446 13 9 13 -6.0512 -0.2374 13 10 13 -6.8431 -0.2115 0 0 0 0.0 0.0 ; _shelx_fab_checksum 62909 _olex2_submission_special_instructions 'No special instructions were received' _site XU loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.68887(2) 0.87234(2) 0.85887(2) 0.03237(9) Uani 1 1 d . . . . . Cl1 Cl 0.24067(12) 0.61124(11) 0.63852(11) 0.0572(6) Uani 1 1 d . . . . . Cl2 Cl 0.51283(14) 0.48220(12) 0.62640(13) 0.0682(7) Uani 1 1 d . . . . . F1 F 0.9561(2) 0.8277(2) 0.8644(2) 0.0521(12) Uani 1 1 d . . . . . F2 F 1.0977(3) 0.7775(3) 0.8601(3) 0.0777(17) Uani 1 1 d . . . . . F3 F 1.1033(3) 0.6559(3) 0.8204(3) 0.0878(18) Uani 1 1 d . . . . . F4 F 0.9658(3) 0.5833(2) 0.7882(3) 0.0658(14) Uani 1 1 d . . . . . F5 F 0.8243(2) 0.6319(2) 0.7954(2) 0.0548(12) Uani 1 1 d . . . . . F6 F 0.7279(3) 0.6475(2) 0.5658(4) 0.089(2) Uani 1 1 d . . . . . F7 F 0.8303(4) 0.6715(3) 0.4933(4) 0.132(3) Uani 1 1 d . . . . . F8 F 0.8363(4) 0.7887(4) 0.4409(3) 0.134(3) Uani 1 1 d . . . . . F9 F 0.7396(4) 0.8831(4) 0.4651(4) 0.123(3) Uani 1 1 d . . . . . F10 F 0.6388(3) 0.8582(3) 0.5380(3) 0.090(2) Uani 1 1 d . . . . . F11 F 0.2215(3) 0.8655(3) 0.5060(3) 0.095(2) Uani 1 1 d . . . . . F12 F 0.0791(3) 0.9147(4) 0.5127(4) 0.123(3) Uani 1 1 d . . . . . F13 F 0.0824(3) 1.0156(3) 0.5956(3) 0.105(2) Uani 1 1 d . . . . . F14 F 0.2283(3) 1.0670(3) 0.6724(4) 0.107(2) Uani 1 1 d . . . . . F15 F 0.3700(3) 1.0177(3) 0.6662(3) 0.0804(18) Uani 1 1 d . . . . . F16 F 0.4118(3) 0.8976(2) 0.8384(2) 0.0633(14) Uani 1 1 d . . . . . F17 F 0.4402(3) 0.9325(3) 0.9707(3) 0.0858(19) Uani 1 1 d . . . . . F18 F 0.5366(3) 0.8608(3) 1.0784(2) 0.097(2) Uani 1 1 d . . . . . F19 F 0.6093(3) 0.7549(3) 1.0494(2) 0.0840(18) Uani 1 1 d . . . . . F20 F 0.5858(3) 0.7204(2) 0.9174(2) 0.0571(13) Uani 1 1 d . . . . . N1 N 0.2842(6) 0.4342(5) 0.6030(5) 0.086(3) Uani 1 1 d . . . . . N2 N 0.5192(3) 0.6827(3) 0.6240(3) 0.0395(15) Uani 1 1 d . . . . . H2 H 0.522308 0.704774 0.661878 0.047 Uiso 1 1 calc R U . . . N3 N 0.4504(3) 0.7039(3) 0.7135(3) 0.0359(15) Uani 1 1 d . . . . . N4 N 0.5055(3) 0.8566(3) 0.6360(3) 0.0300(13) Uani 1 1 d . . . . . N5 N 0.4692(3) 0.9130(3) 0.5084(3) 0.0385(15) Uani 1 1 d . . . . . H5 H 0.507249 0.888576 0.536586 0.046 Uiso 1 1 calc R U . . . N6 N 0.6707(3) 0.8029(3) 0.7802(3) 0.0311(13) Uani 1 1 d . . . . . N7 N 0.7515(3) 0.8025(3) 0.9274(3) 0.0353(14) Uani 1 1 d . . . . . C1 C 0.6899(4) 0.9435(4) 0.7857(4) 0.0424(19) Uani 1 1 d . . . . . H1 H 0.685098 0.926885 0.737952 0.051 Uiso 1 1 calc R U . . . C2 C 0.7613(5) 0.9862(5) 0.8155(5) 0.070(3) Uani 1 1 d . . . . . H2A H 0.749041 1.027453 0.791136 0.084 Uiso 1 1 calc R U . . . H2B H 0.810055 0.968053 0.806192 0.084 Uiso 1 1 calc R U . . . C3 C 0.7825(5) 0.9970(4) 0.8938(5) 0.061(3) Uani 1 1 d . . . . . H3A H 0.842329 1.005601 0.914543 0.073 Uiso 1 1 calc R U . . . H3B H 0.752164 1.034481 0.902025 0.073 Uiso 1 1 calc R U . . . C4 C 0.7603(5) 0.9404(4) 0.9292(4) 0.047(2) Uani 1 1 d . . . . . H4 H 0.808105 0.922124 0.967210 0.057 Uiso 1 1 calc R U . . . C5 C 0.6846(5) 0.9333(4) 0.9409(4) 0.044(2) Uani 1 1 d . . . . . H5A H 0.688664 0.911041 0.985743 0.053 Uiso 1 1 calc R U . . . C6 C 0.6189(5) 0.9837(4) 0.9205(4) 0.052(2) Uani 1 1 d . . . . . H6A H 0.639906 1.022585 0.947918 0.063 Uiso 1 1 calc R U . . . H6B H 0.569928 0.969176 0.932199 0.063 Uiso 1 1 calc R U . . . C7 C 0.5937(5) 0.9988(4) 0.8423(5) 0.054(2) Uani 1 1 d . . . . . H7A H 0.533457 1.006533 0.824527 0.065 Uiso 1 1 calc R U . . . H7B H 0.621569 1.038295 0.836034 0.065 Uiso 1 1 calc R U . . . C8 C 0.6142(5) 0.9475(4) 0.7985(4) 0.0428(19) Uani 1 1 d . . . . . H8 H 0.565813 0.932604 0.758588 0.051 Uiso 1 1 calc R U . . . C9 C 0.8865(4) 0.7308(4) 0.8323(3) 0.0354(17) Uani 1 1 d . . . . . C10 C 0.9574(4) 0.7667(4) 0.8469(4) 0.0387(18) Uani 1 1 d . . . . . C11 C 1.0301(5) 0.7418(4) 0.8443(4) 0.051(2) Uani 1 1 d . . . . . C12 C 1.0331(5) 0.6814(4) 0.8239(4) 0.049(2) Uani 1 1 d . . . . . C13 C 0.9621(5) 0.6443(4) 0.8060(4) 0.044(2) Uani 1 1 d . . . . . C14 C 0.8910(4) 0.6697(4) 0.8111(4) 0.045(2) Uani 1 1 d . . . . . C15 C 0.8109(4) 0.7605(3) 0.8412(4) 0.0301(16) Uani 1 1 d . . . . . C16 C 0.8102(4) 0.7670(3) 0.9091(3) 0.0319(16) Uani 1 1 d . . . . . C17 C 0.8655(4) 0.7390(4) 0.9719(4) 0.0392(18) Uani 1 1 d . . . . . H17 H 0.912540 0.713802 0.975403 0.047 Uiso 1 1 calc R U . . . C18 C 0.8375(5) 0.7556(4) 1.0250(4) 0.047(2) Uani 1 1 d . . . . . H18 H 0.860473 0.743071 1.072779 0.057 Uiso 1 1 calc R U . . . C19 C 0.7678(4) 0.7949(4) 0.9967(4) 0.0397(18) Uani 1 1 d . . . . . H19 H 0.736848 0.813429 1.023212 0.048 Uiso 1 1 calc R U . . . C20 C 0.7448(4) 0.7760(3) 0.7801(4) 0.0329(17) Uani 1 1 d . . . . . C21 C 0.7375(4) 0.7562(3) 0.7119(3) 0.0315(16) Uani 1 1 d . . . . . H21 H 0.780020 0.738230 0.697167 0.038 Uiso 1 1 calc R U . . . C22 C 0.6564(4) 0.7678(3) 0.6696(3) 0.0283(15) Uani 1 1 d . . . . . C23 C 0.6251(4) 0.7405(3) 0.5982(4) 0.0309(16) Uani 1 1 d . . . . . C24 C 0.6772(4) 0.7513(4) 0.5525(3) 0.0327(17) Uani 1 1 d . . . . . C25 C 0.6830(5) 0.8102(4) 0.5252(4) 0.049(2) Uani 1 1 d . . . . . C26 C 0.7359(5) 0.8229(5) 0.4876(5) 0.067(3) Uani 1 1 d . . . . . C27 C 0.7843(6) 0.7759(7) 0.4772(5) 0.079(4) Uani 1 1 d . . . . . C28 C 0.7803(6) 0.7171(6) 0.5024(6) 0.080(4) Uani 1 1 d . . . . . C29 C 0.7271(5) 0.7050(5) 0.5403(5) 0.053(2) Uani 1 1 d . . . . . C30 C 0.5636(4) 0.6969(3) 0.5803(3) 0.0318(16) Uani 1 1 d . . . . . C31 C 0.5365(4) 0.6505(4) 0.5247(4) 0.0365(18) Uani 1 1 d . . . . . H31 H 0.554477 0.648130 0.484780 0.044 Uiso 1 1 calc R U . . . C32 C 0.4815(4) 0.6110(4) 0.5384(4) 0.0406(19) Uani 1 1 d . . . . . H32 H 0.455190 0.576029 0.510301 0.049 Uiso 1 1 calc R U . . . C33 C 0.4698(4) 0.6312(4) 0.6034(4) 0.0382(17) Uani 1 1 d . . . . . C34 C 0.4236(4) 0.6086(3) 0.6439(4) 0.0348(17) Uani 1 1 d . . . . . C35 C 0.3772(4) 0.5487(4) 0.6289(4) 0.0360(17) Uani 1 1 d . . . . . C36 C 0.4098(5) 0.4907(4) 0.6189(4) 0.047(2) Uani 1 1 d . . . . . C37 C 0.3623(7) 0.4366(5) 0.6054(5) 0.078(3) Uani 1 1 d . . . . . H37 H 0.387341 0.398542 0.597222 0.094 Uiso 1 1 calc R U . . . C38 C 0.2941(4) 0.5444(4) 0.6262(4) 0.046(2) Uani 1 1 d . . . . . C39 C 0.2517(6) 0.4877(5) 0.6144(5) 0.068(3) Uani 1 1 d . . . . . H39 H 0.196270 0.487453 0.614545 0.082 Uiso 1 1 calc R U . . . C40 C 0.4255(4) 0.6444(4) 0.7057(4) 0.0363(18) Uani 1 1 d . . . . . C41 C 0.4127(4) 0.6217(4) 0.7717(3) 0.0369(17) Uani 1 1 d . . . . . H41 H 0.393318 0.581203 0.779756 0.044 Uiso 1 1 calc R U . . . C42 C 0.4340(4) 0.6700(4) 0.8176(4) 0.0420(19) Uani 1 1 d . . . . . H42 H 0.433670 0.669900 0.864689 0.050 Uiso 1 1 calc R U . . . C43 C 0.4576(4) 0.7224(4) 0.7816(3) 0.0365(17) Uani 1 1 d . . . . . C44 C 0.4785(4) 0.7840(4) 0.7978(3) 0.0318(17) Uani 1 1 d . . . . . C45 C 0.4963(4) 0.8064(4) 0.8717(4) 0.0351(17) Uani 1 1 d . . . . . C46 C 0.5469(5) 0.7720(4) 0.9271(4) 0.047(2) Uani 1 1 d . . . . . C47 C 0.5609(5) 0.7901(5) 0.9972(4) 0.058(3) Uani 1 1 d . . . . . C48 C 0.5243(6) 0.8438(6) 1.0108(5) 0.070(3) Uani 1 1 d . . . . . C49 C 0.4747(5) 0.8793(5) 0.9575(5) 0.060(3) Uani 1 1 d . . . . . C50 C 0.4629(4) 0.8610(4) 0.8889(4) 0.045(2) Uani 1 1 d . . . . . C51 C 0.6182(4) 0.7980(3) 0.7142(3) 0.0259(15) Uani 1 1 d . . . . . C52 C 0.5357(4) 0.8248(3) 0.6961(4) 0.0333(16) Uani 1 1 d . . . . . C53 C 0.4790(4) 0.8268(3) 0.7380(3) 0.0308(16) Uani 1 1 d . . . . . C54 C 0.4133(4) 0.8603(3) 0.6990(4) 0.0376(18) Uani 1 1 d . . . . . H54 H 0.365212 0.869448 0.711099 0.045 Uiso 1 1 calc R U . . . C55 C 0.4288(4) 0.8797(3) 0.6356(3) 0.0288(15) Uani 1 1 d . . . . . C56 C 0.3797(4) 0.9150(3) 0.5813(4) 0.0316(16) Uani 1 1 d . . . . . C57 C 0.3979(4) 0.9312(3) 0.5197(3) 0.0329(17) Uani 1 1 d . . . . . C58 C 0.3552(5) 0.9675(4) 0.4624(4) 0.048(2) Uani 1 1 d . . . . . H58 H 0.302856 0.986490 0.455224 0.058 Uiso 1 1 calc R U . . . C59 C 0.4019(5) 0.9717(4) 0.4164(4) 0.051(2) Uani 1 1 d . . . . . H59 H 0.387132 0.993418 0.372741 0.061 Uiso 1 1 calc R U . . . C60 C 0.4726(5) 0.9382(4) 0.4471(4) 0.045(2) Uani 1 1 d . . . . . H60 H 0.516907 0.933330 0.428818 0.054 Uiso 1 1 calc R U . . . C61 C 0.3001(4) 0.9403(4) 0.5864(4) 0.0365(17) Uani 1 1 d . . . . . C62 C 0.2260(5) 0.9156(4) 0.5481(5) 0.060(3) Uani 1 1 d . . . . . C63 C 0.1516(5) 0.9403(5) 0.5509(5) 0.070(3) Uani 1 1 d . . . . . C64 C 0.1527(5) 0.9911(5) 0.5922(5) 0.065(3) Uani 1 1 d . . . . . C65 C 0.2268(6) 1.0170(4) 0.6318(5) 0.059(2) Uani 1 1 d . . . . . C66 C 0.2989(5) 0.9910(4) 0.6277(4) 0.047(2) Uani 1 1 d . . . . . 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 0.03287(14) 0.03286(16) 0.03096(14) -0.00201(15) 0.00974(10) 0.00350(15) Cl1 0.0421(11) 0.0817(18) 0.0535(12) 0.0102(11) 0.0230(9) 0.0049(11) Cl2 0.0646(14) 0.0594(16) 0.0909(18) 0.0015(13) 0.0396(13) 0.0118(12) F1 0.045(3) 0.044(3) 0.062(3) -0.011(2) 0.009(2) -0.011(2) F2 0.037(3) 0.080(4) 0.113(5) 0.005(3) 0.022(3) -0.004(3) F3 0.056(3) 0.087(4) 0.132(5) 0.002(4) 0.047(3) 0.027(3) F4 0.077(3) 0.047(3) 0.072(3) -0.003(3) 0.023(3) 0.024(3) F5 0.046(2) 0.042(3) 0.066(3) -0.009(2) 0.004(2) 0.002(2) F6 0.071(4) 0.040(3) 0.180(6) -0.005(4) 0.074(4) 0.004(3) F7 0.095(4) 0.118(6) 0.233(8) -0.093(6) 0.121(5) -0.029(4) F8 0.094(4) 0.239(9) 0.101(5) -0.023(5) 0.078(4) -0.048(5) F9 0.108(5) 0.137(7) 0.135(6) 0.073(5) 0.057(4) -0.014(5) F10 0.068(3) 0.068(4) 0.154(6) 0.051(4) 0.060(4) 0.022(3) F11 0.041(3) 0.106(5) 0.121(5) -0.062(4) 0.004(3) -0.006(3) F12 0.026(3) 0.160(7) 0.164(6) -0.051(5) 0.002(3) 0.004(3) F13 0.059(3) 0.138(6) 0.123(5) -0.006(4) 0.036(3) 0.042(4) F14 0.088(4) 0.106(5) 0.142(6) -0.054(5) 0.060(4) 0.014(4) F15 0.051(3) 0.077(4) 0.113(4) -0.057(3) 0.026(3) -0.016(3) F16 0.068(3) 0.072(4) 0.054(3) -0.012(3) 0.025(3) 0.021(3) F17 0.074(3) 0.110(5) 0.084(4) -0.054(4) 0.041(3) -0.001(3) F18 0.077(4) 0.176(7) 0.043(3) -0.042(4) 0.028(3) -0.027(4) F19 0.072(3) 0.140(6) 0.036(3) 0.016(3) 0.012(3) -0.007(4) F20 0.058(3) 0.067(4) 0.043(3) 0.014(2) 0.011(2) 0.011(3) N1 0.091(7) 0.079(7) 0.096(7) -0.028(6) 0.040(6) -0.038(6) N2 0.032(3) 0.053(4) 0.038(3) -0.006(3) 0.016(3) -0.007(3) N3 0.035(3) 0.048(4) 0.028(3) -0.001(3) 0.014(3) -0.004(3) N4 0.027(3) 0.027(4) 0.034(3) -0.004(2) 0.006(2) 0.001(2) N5 0.038(3) 0.038(4) 0.038(4) -0.005(3) 0.010(3) -0.002(3) N6 0.032(3) 0.034(4) 0.028(3) 0.008(3) 0.011(3) 0.010(3) N7 0.040(3) 0.037(4) 0.028(3) -0.002(3) 0.010(3) 0.004(3) C1 0.049(5) 0.039(5) 0.040(4) 0.000(4) 0.016(4) 0.002(4) C2 0.063(6) 0.056(7) 0.099(8) 0.010(6) 0.037(6) -0.003(5) C3 0.049(5) 0.052(6) 0.081(7) -0.022(5) 0.020(5) -0.005(4) C4 0.046(5) 0.037(5) 0.050(5) -0.003(4) 0.002(4) 0.008(4) C5 0.060(5) 0.036(5) 0.042(4) -0.008(4) 0.023(4) -0.001(4) C6 0.060(5) 0.042(5) 0.067(6) -0.019(4) 0.035(5) 0.008(4) C7 0.044(5) 0.038(5) 0.078(6) -0.002(5) 0.017(4) 0.015(4) C8 0.044(4) 0.039(5) 0.045(5) -0.003(4) 0.012(4) 0.002(4) C9 0.033(4) 0.039(5) 0.030(4) 0.000(3) 0.004(3) -0.003(3) C10 0.040(4) 0.032(5) 0.044(4) -0.003(4) 0.012(3) 0.010(4) C11 0.032(4) 0.049(6) 0.062(6) 0.003(4) 0.002(4) -0.003(4) C12 0.044(5) 0.044(6) 0.061(5) -0.001(4) 0.019(4) 0.018(4) C13 0.057(5) 0.032(5) 0.044(5) 0.002(3) 0.018(4) 0.015(4) C14 0.037(4) 0.043(5) 0.048(5) -0.004(4) 0.005(4) -0.002(4) C15 0.030(4) 0.020(4) 0.039(4) 0.000(3) 0.011(3) 0.000(3) C16 0.034(4) 0.035(4) 0.025(4) 0.002(3) 0.006(3) -0.001(3) C17 0.029(4) 0.048(5) 0.039(4) 0.000(4) 0.009(3) 0.003(4) C18 0.059(5) 0.040(5) 0.038(4) 0.011(4) 0.008(4) -0.007(4) C19 0.051(5) 0.037(5) 0.029(4) 0.001(3) 0.009(3) 0.002(4) C20 0.030(4) 0.028(4) 0.037(4) 0.001(3) 0.005(3) 0.002(3) C21 0.021(3) 0.037(5) 0.040(4) -0.001(3) 0.015(3) 0.000(3) C22 0.030(4) 0.030(4) 0.026(4) -0.001(3) 0.011(3) -0.001(3) C23 0.023(3) 0.031(4) 0.039(4) 0.001(3) 0.010(3) 0.000(3) C24 0.029(4) 0.047(5) 0.023(4) -0.008(3) 0.011(3) -0.003(3) C25 0.045(5) 0.061(6) 0.050(5) 0.018(4) 0.028(4) 0.006(4) C26 0.054(5) 0.091(8) 0.063(6) 0.032(6) 0.028(5) -0.014(6) C27 0.052(6) 0.126(11) 0.079(7) -0.028(7) 0.050(5) -0.024(7) C28 0.050(6) 0.104(10) 0.101(8) -0.065(8) 0.044(6) -0.024(6) C29 0.044(5) 0.060(6) 0.065(6) -0.014(5) 0.030(4) -0.007(5) C30 0.032(4) 0.039(5) 0.031(4) 0.002(3) 0.019(3) -0.002(3) C31 0.028(4) 0.055(5) 0.031(4) -0.008(3) 0.015(3) -0.004(3) C32 0.035(4) 0.048(5) 0.039(4) -0.009(4) 0.012(3) -0.001(4) C33 0.031(4) 0.046(5) 0.036(4) -0.001(4) 0.009(3) -0.014(4) C34 0.033(4) 0.038(5) 0.034(4) -0.003(3) 0.012(3) -0.011(3) C35 0.040(4) 0.034(5) 0.034(4) -0.002(3) 0.012(3) -0.004(3) C36 0.062(5) 0.038(5) 0.049(5) -0.007(4) 0.028(4) -0.005(4) C37 0.102(8) 0.054(7) 0.094(8) -0.023(6) 0.053(7) -0.007(6) C38 0.039(4) 0.061(6) 0.040(5) -0.002(4) 0.015(4) -0.004(4) C39 0.050(5) 0.086(9) 0.067(6) -0.011(6) 0.018(5) -0.027(6) C40 0.032(4) 0.043(5) 0.035(4) 0.003(3) 0.013(3) 0.000(3) C41 0.040(4) 0.042(5) 0.032(4) 0.004(4) 0.016(3) -0.010(4) C42 0.050(5) 0.042(5) 0.037(4) 0.009(4) 0.019(4) 0.001(4) C43 0.043(4) 0.041(5) 0.029(4) 0.000(3) 0.016(3) 0.004(4) C44 0.024(3) 0.045(5) 0.032(4) 0.001(3) 0.017(3) 0.009(3) C45 0.028(4) 0.047(5) 0.035(4) -0.008(3) 0.017(3) -0.003(3) C46 0.040(4) 0.067(6) 0.035(5) -0.002(4) 0.012(4) 0.004(4) C47 0.047(5) 0.092(8) 0.031(5) 0.011(5) 0.005(4) -0.011(5) C48 0.051(6) 0.117(10) 0.052(6) -0.027(6) 0.029(5) -0.023(6) C49 0.054(5) 0.080(8) 0.059(6) -0.036(6) 0.035(5) -0.023(5) C50 0.040(4) 0.059(6) 0.045(5) -0.005(4) 0.024(4) 0.001(4) C51 0.024(3) 0.023(4) 0.027(4) 0.002(3) 0.004(3) 0.003(3) C52 0.035(4) 0.029(4) 0.038(4) -0.003(3) 0.014(3) 0.002(3) C53 0.029(4) 0.037(4) 0.032(4) -0.002(3) 0.017(3) -0.008(3) C54 0.027(3) 0.047(5) 0.039(4) 0.001(3) 0.010(3) 0.002(3) C55 0.026(3) 0.027(4) 0.034(4) 0.002(3) 0.010(3) 0.004(3) C56 0.024(3) 0.029(4) 0.038(4) -0.007(3) 0.004(3) 0.004(3) C57 0.029(4) 0.035(5) 0.033(4) 0.001(3) 0.008(3) 0.012(3) C58 0.050(5) 0.045(5) 0.047(5) 0.007(4) 0.013(4) 0.007(4) C59 0.068(6) 0.038(5) 0.045(5) 0.004(4) 0.017(4) 0.002(4) C60 0.059(5) 0.045(5) 0.036(4) -0.003(4) 0.023(4) -0.005(4) C61 0.028(4) 0.034(5) 0.043(4) 0.000(3) 0.005(3) 0.006(3) C62 0.040(5) 0.067(7) 0.063(6) -0.024(5) 0.004(4) 0.019(5) C63 0.031(5) 0.080(8) 0.089(7) -0.011(6) 0.004(5) 0.011(5) C64 0.045(5) 0.079(8) 0.075(7) -0.001(6) 0.026(5) 0.023(5) C65 0.063(6) 0.051(6) 0.075(6) -0.008(5) 0.038(5) 0.011(5) C66 0.044(5) 0.056(6) 0.046(5) 0.000(4) 0.021(4) 0.012(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' F F 0.0171 0.0103 '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' 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 N6 Ir1 C1 90.3(3) . . ? N6 Ir1 C4 153.1(3) . . ? N6 Ir1 C5 167.9(3) . . ? N6 Ir1 C8 100.1(2) . . ? N7 Ir1 N6 85.5(2) . . ? N7 Ir1 C1 148.8(3) . . ? N7 Ir1 C4 88.7(3) . . ? N7 Ir1 C5 93.2(3) . . ? N7 Ir1 C8 171.5(2) . . ? C1 Ir1 C4 81.2(3) . . ? C1 Ir1 C5 96.9(3) . . ? C1 Ir1 C8 38.5(3) . . ? C4 Ir1 C5 38.7(3) . . ? C4 Ir1 C8 89.1(3) . . ? C5 Ir1 C8 80.0(3) . . ? C39 N1 C37 116.1(9) . . ? C30 N2 H2 123.2 . . ? C33 N2 H2 123.2 . . ? C33 N2 C30 113.5(6) . . ? C40 N3 C43 107.8(6) . . ? C52 N4 C55 105.6(5) . . ? C57 N5 H5 125.0 . . ? C60 N5 H5 125.0 . . ? C60 N5 C57 110.0(6) . . ? C20 N6 Ir1 112.0(4) . . ? C51 N6 Ir1 133.2(4) . . ? C51 N6 C20 106.6(5) . . ? C16 N7 Ir1 118.0(4) . . ? C19 N7 Ir1 131.9(5) . . ? C19 N7 C16 106.6(6) . . ? Ir1 C1 H1 113.8 . . ? C2 C1 Ir1 110.1(6) . . ? C2 C1 H1 113.8 . . ? C8 C1 Ir1 72.4(4) . . ? C8 C1 H1 113.8 . . ? C8 C1 C2 125.3(7) . . ? C1 C2 H2A 108.8 . . ? C1 C2 H2B 108.8 . . ? C1 C2 C3 113.7(7) . . ? H2A C2 H2B 107.7 . . ? C3 C2 H2A 108.8 . . ? C3 C2 H2B 108.8 . . ? C2 C3 H3A 109.4 . . ? C2 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C4 C3 C2 111.1(7) . . ? C4 C3 H3A 109.4 . . ? C4 C3 H3B 109.4 . . ? Ir1 C4 H4 113.7 . . ? C3 C4 Ir1 114.0(6) . . ? C3 C4 H4 113.7 . . ? C5 C4 Ir1 70.9(4) . . ? C5 C4 C3 123.7(7) . . ? C5 C4 H4 113.7 . . ? Ir1 C5 H5A 114.0 . . ? C4 C5 Ir1 70.5(4) . . ? C4 C5 H5A 114.0 . . ? C4 C5 C6 121.9(7) . . ? C6 C5 Ir1 115.5(5) . . ? C6 C5 H5A 114.0 . . ? C5 C6 H6A 109.3 . . ? C5 C6 H6B 109.3 . . ? C5 C6 C7 111.4(6) . . ? H6A C6 H6B 108.0 . . ? C7 C6 H6A 109.3 . . ? C7 C6 H6B 109.3 . . ? C6 C7 H7A 108.7 . . ? C6 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C8 C7 C6 114.3(7) . . ? C8 C7 H7A 108.7 . . ? C8 C7 H7B 108.7 . . ? Ir1 C8 H8 114.0 . . ? C1 C8 Ir1 69.1(4) . . ? C1 C8 C7 123.7(7) . . ? C1 C8 H8 114.0 . . ? C7 C8 Ir1 114.2(5) . . ? C7 C8 H8 114.0 . . ? C10 C9 C15 118.5(7) . . ? C14 C9 C10 116.8(7) . . ? C14 C9 C15 124.7(6) . . ? F1 C10 C9 119.8(6) . . ? F1 C10 C11 118.3(7) . . ? C11 C10 C9 121.8(7) . . ? F2 C11 C10 120.2(8) . . ? F2 C11 C12 119.6(8) . . ? C12 C11 C10 120.2(8) . . ? F3 C12 C11 121.5(8) . . ? F3 C12 C13 118.8(8) . . ? C11 C12 C13 119.8(7) . . ? F4 C13 C12 119.8(7) . . ? F4 C13 C14 121.2(8) . . ? C14 C13 C12 118.9(7) . . ? F5 C14 C9 120.3(7) . . ? F5 C14 C13 117.2(7) . . ? C13 C14 C9 122.4(7) . . ? C16 C15 C9 116.4(6) . . ? C16 C15 C20 125.4(6) . . ? C20 C15 C9 118.1(6) . . ? N7 C16 C17 108.3(6) . . ? C15 C16 N7 123.6(6) . . ? C15 C16 C17 128.1(7) . . ? C16 C17 H17 126.6 . . ? C18 C17 C16 106.8(7) . . ? C18 C17 H17 126.6 . . ? C17 C18 H18 126.2 . . ? C17 C18 C19 107.6(7) . . ? C19 C18 H18 126.2 . . ? N7 C19 C18 110.8(7) . . ? N7 C19 H19 124.6 . . ? C18 C19 H19 124.6 . . ? N6 C20 C15 124.5(6) . . ? N6 C20 C21 109.4(6) . . ? C21 C20 C15 125.1(6) . . ? C20 C21 H21 126.3 . . ? C22 C21 C20 107.5(6) . . ? C22 C21 H21 126.3 . . ? C21 C22 C23 120.1(6) . . ? C21 C22 C51 105.3(5) . . ? C51 C22 C23 133.9(6) . . ? C22 C23 C24 116.0(5) . . ? C30 C23 C22 121.9(6) . . ? C30 C23 C24 120.6(6) . . ? C25 C24 C23 121.2(7) . . ? C29 C24 C23 122.1(7) . . ? C29 C24 C25 116.4(7) . . ? F10 C25 C24 119.4(6) . . ? F10 C25 C26 118.0(8) . . ? C24 C25 C26 122.5(8) . . ? F9 C26 C25 118.3(10) . . ? C27 C26 F9 122.6(9) . . ? C27 C26 C25 119.0(9) . . ? F8 C27 C26 118.7(12) . . ? F8 C27 C28 120.6(11) . . ? C26 C27 C28 120.7(9) . . ? F7 C28 C27 120.0(10) . . ? F7 C28 C29 120.2(12) . . ? C27 C28 C29 119.7(9) . . ? F6 C29 C24 121.2(7) . . ? F6 C29 C28 117.2(9) . . ? C24 C29 C28 121.6(9) . . ? N2 C30 C31 104.0(6) . . ? C23 C30 N2 121.6(6) . . ? C23 C30 C31 133.8(6) . . ? C30 C31 H31 125.3 . . ? C32 C31 C30 109.4(6) . . ? C32 C31 H31 125.3 . . ? C31 C32 H32 126.0 . . ? C31 C32 C33 108.0(7) . . ? C33 C32 H32 126.0 . . ? N2 C33 C32 105.0(6) . . ? N2 C33 C34 120.8(6) . . ? C34 C33 C32 134.2(7) . . ? C33 C34 C35 123.1(6) . . ? C33 C34 C40 117.6(6) . . ? C40 C34 C35 119.1(6) . . ? C36 C35 C34 125.0(7) . . ? C36 C35 C38 112.7(7) . . ? C38 C35 C34 122.3(7) . . ? C35 C36 Cl2 121.6(6) . . ? C37 C36 Cl2 116.8(7) . . ? C37 C36 C35 121.5(8) . . ? N1 C37 C36 124.3(9) . . ? N1 C37 H37 117.9 . . ? C36 C37 H37 117.9 . . ? C35 C38 Cl1 120.8(6) . . ? C39 C38 Cl1 117.2(7) . . ? C39 C38 C35 122.0(8) . . ? N1 C39 C38 123.3(9) . . ? N1 C39 H39 118.3 . . ? C38 C39 H39 118.3 . . ? N3 C40 C34 121.1(6) . . ? N3 C40 C41 109.7(6) . . ? C34 C40 C41 128.8(7) . . ? C40 C41 H41 126.9 . . ? C42 C41 C40 106.2(7) . . ? C42 C41 H41 126.9 . . ? C41 C42 H42 126.4 . . ? C41 C42 C43 107.3(6) . . ? C43 C42 H42 126.4 . . ? N3 C43 C42 109.0(7) . . ? C44 C43 N3 115.9(6) . . ? C44 C43 C42 134.9(7) . . ? C43 C44 C45 119.6(6) . . ? C43 C44 C53 116.9(6) . . ? C45 C44 C53 123.4(7) . . ? C46 C45 C44 120.6(7) . . ? C46 C45 C50 116.3(7) . . ? C50 C45 C44 123.2(7) . . ? F20 C46 C45 122.1(7) . . ? F20 C46 C47 116.2(7) . . ? C45 C46 C47 121.7(8) . . ? F19 C47 C46 119.9(9) . . ? F19 C47 C48 120.9(9) . . ? C48 C47 C46 119.2(8) . . ? F18 C48 C47 119.3(10) . . ? F18 C48 C49 120.1(10) . . ? C49 C48 C47 120.7(8) . . ? F17 C49 C48 120.7(8) . . ? F17 C49 C50 120.2(9) . . ? C48 C49 C50 119.0(9) . . ? F16 C50 C45 120.7(7) . . ? F16 C50 C49 116.1(8) . . ? C45 C50 C49 123.0(8) . . ? N6 C51 C22 111.2(5) . . ? N6 C51 C52 120.2(6) . . ? C22 C51 C52 128.6(6) . . ? N4 C52 C51 119.0(6) . . ? N4 C52 C53 111.7(6) . . ? C51 C52 C53 129.2(6) . . ? C52 C53 C44 127.7(6) . . ? C54 C53 C44 124.1(6) . . ? C54 C53 C52 105.3(6) . . ? C53 C54 H54 126.1 . . ? C53 C54 C55 107.8(6) . . ? C55 C54 H54 126.1 . . ? N4 C55 C54 109.6(6) . . ? C56 C55 N4 121.9(6) . . ? C56 C55 C54 128.4(6) . . ? C55 C56 C57 125.6(6) . . ? C55 C56 C61 118.6(6) . . ? C57 C56 C61 115.8(6) . . ? N5 C57 C56 122.6(6) . . ? N5 C57 C58 106.1(6) . . ? C58 C57 C56 131.3(6) . . ? C57 C58 H58 125.5 . . ? C57 C58 C59 109.0(7) . . ? C59 C58 H58 125.5 . . ? C58 C59 H59 126.9 . . ? C60 C59 C58 106.1(7) . . ? C60 C59 H59 126.9 . . ? N5 C60 C59 108.7(7) . . ? N5 C60 H60 125.6 . . ? C59 C60 H60 125.6 . . ? C62 C61 C56 121.8(7) . . ? C62 C61 C66 117.0(7) . . ? C66 C61 C56 121.1(6) . . ? F11 C62 C61 120.9(7) . . ? F11 C62 C63 117.0(8) . . ? C61 C62 C63 122.0(8) . . ? F12 C63 C62 120.8(9) . . ? F12 C63 C64 119.8(8) . . ? C64 C63 C62 119.4(8) . . ? F13 C64 C63 120.5(9) . . ? F13 C64 C65 119.7(9) . . ? C63 C64 C65 119.8(8) . . ? F14 C65 C64 120.1(8) . . ? F14 C65 C66 120.9(9) . . ? C64 C65 C66 119.0(8) . . ? F15 C66 C61 119.7(7) . . ? F15 C66 C65 117.6(8) . . ? C61 C66 C65 122.8(8) . . ? 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 N6 2.106(6) . ? Ir1 N7 2.068(6) . ? Ir1 C1 2.109(7) . ? Ir1 C4 2.109(8) . ? Ir1 C5 2.115(7) . ? Ir1 C8 2.152(7) . ? Cl1 C38 1.745(8) . ? Cl2 C36 1.730(8) . ? F1 C10 1.339(8) . ? F2 C11 1.331(9) . ? F3 C12 1.338(8) . ? F4 C13 1.346(8) . ? F5 C14 1.344(8) . ? F6 C29 1.319(10) . ? F7 C28 1.339(11) . ? F8 C27 1.349(9) . ? F9 C26 1.359(11) . ? F10 C25 1.339(9) . ? F11 C62 1.343(9) . ? F12 C63 1.345(10) . ? F13 C64 1.332(9) . ? F14 C65 1.333(10) . ? F15 C66 1.338(9) . ? F16 C50 1.350(9) . ? F17 C49 1.337(10) . ? F18 C48 1.356(9) . ? F19 C47 1.334(9) . ? F20 C46 1.325(9) . ? N1 C37 1.324(12) . ? N1 C39 1.315(12) . ? N2 H2 0.8800 . ? N2 C30 1.369(8) . ? N2 C33 1.358(9) . ? N3 C40 1.321(9) . ? N3 C43 1.393(8) . ? N4 C52 1.332(8) . ? N4 C55 1.399(8) . ? N5 H5 0.8800 . ? N5 C57 1.367(8) . ? N5 C60 1.361(9) . ? N6 C20 1.390(8) . ? N6 C51 1.344(8) . ? N7 C16 1.397(8) . ? N7 C19 1.339(8) . ? C1 H1 1.0000 . ? C1 C2 1.481(11) . ? C1 C8 1.404(10) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 C3 1.515(12) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.501(11) . ? C4 H4 1.0000 . ? C4 C5 1.398(10) . ? C5 H5A 1.0000 . ? C5 C6 1.507(10) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C6 C7 1.525(11) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.508(10) . ? C8 H8 1.0000 . ? C9 C10 1.381(10) . ? C9 C14 1.370(10) . ? C9 C15 1.501(9) . ? C10 C11 1.368(10) . ? C11 C12 1.346(11) . ? C12 C13 1.394(11) . ? C13 C14 1.366(10) . ? C15 C16 1.375(9) . ? C15 C20 1.414(9) . ? C16 C17 1.438(9) . ? C17 H17 0.9500 . ? C17 C18 1.351(10) . ? C18 H18 0.9500 . ? C18 C19 1.413(10) . ? C19 H19 0.9500 . ? C20 C21 1.400(9) . ? C21 H21 0.9500 . ? C21 C22 1.395(8) . ? C22 C23 1.480(9) . ? C22 C51 1.422(9) . ? C23 C24 1.492(9) . ? C23 C30 1.356(9) . ? C24 C25 1.378(10) . ? C24 C29 1.372(10) . ? C25 C26 1.381(10) . ? C26 C27 1.352(14) . ? C27 C28 1.353(15) . ? C28 C29 1.389(12) . ? C30 C31 1.448(9) . ? C31 H31 0.9500 . ? C31 C32 1.351(9) . ? C32 H32 0.9500 . ? C32 C33 1.451(10) . ? C33 C34 1.391(9) . ? C34 C35 1.474(9) . ? C34 C40 1.448(9) . ? C35 C36 1.389(10) . ? C35 C38 1.409(9) . ? C36 C37 1.378(12) . ? C37 H37 0.9500 . ? C38 C39 1.381(12) . ? C39 H39 0.9500 . ? C40 C41 1.495(9) . ? C41 H41 0.9500 . ? C41 C42 1.346(10) . ? C42 H42 0.9500 . ? C42 C43 1.450(10) . ? C43 C44 1.361(10) . ? C44 C45 1.496(9) . ? C44 C53 1.509(9) . ? C45 C46 1.377(10) . ? C45 C50 1.381(10) . ? C46 C47 1.405(11) . ? C47 C48 1.366(13) . ? C48 C49 1.359(13) . ? C49 C50 1.382(10) . ? C51 C52 1.454(9) . ? C52 C53 1.478(9) . ? C53 C54 1.345(9) . ? C54 H54 0.9500 . ? C54 C55 1.445(9) . ? C55 C56 1.364(9) . ? C56 C57 1.414(9) . ? C56 C61 1.499(9) . ? C57 C58 1.379(9) . ? C58 H58 0.9500 . ? C58 C59 1.408(10) . ? C59 H59 0.9500 . ? C59 C60 1.365(10) . ? C60 H60 0.9500 . ? C61 C62 1.357(10) . ? C61 C66 1.362(10) . ? C62 C63 1.394(11) . ? C63 C64 1.355(12) . ? C64 C65 1.374(12) . ? C65 C66 1.376(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_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ir1 N6 C20 C15 40.0(8) . . . . ? Ir1 N6 C20 C21 -151.0(5) . . . . ? Ir1 N6 C51 C22 144.7(5) . . . . ? Ir1 N6 C51 C52 -32.6(10) . . . . ? Ir1 N7 C16 C15 -22.1(9) . . . . ? Ir1 N7 C16 C17 159.3(5) . . . . ? Ir1 N7 C19 C18 -156.8(5) . . . . ? Ir1 C1 C2 C3 -35.1(9) . . . . ? Ir1 C1 C8 C7 105.8(7) . . . . ? Ir1 C4 C5 C6 -108.5(7) . . . . ? Ir1 C5 C6 C7 -24.3(9) . . . . ? Cl1 C38 C39 N1 178.6(8) . . . . ? Cl2 C36 C37 N1 175.1(8) . . . . ? F1 C10 C11 F2 1.1(12) . . . . ? F1 C10 C11 C12 -177.0(7) . . . . ? F2 C11 C12 F3 1.5(13) . . . . ? F2 C11 C12 C13 -178.8(7) . . . . ? F3 C12 C13 F4 2.4(12) . . . . ? F3 C12 C13 C14 178.4(7) . . . . ? F4 C13 C14 F5 -2.1(11) . . . . ? F4 C13 C14 C9 176.9(7) . . . . ? F7 C28 C29 F6 -0.6(13) . . . . ? F7 C28 C29 C24 177.8(8) . . . . ? F8 C27 C28 F7 2.3(16) . . . . ? F8 C27 C28 C29 179.3(8) . . . . ? F9 C26 C27 F8 -2.3(15) . . . . ? F9 C26 C27 C28 178.0(10) . . . . ? F10 C25 C26 F9 -0.6(13) . . . . ? F10 C25 C26 C27 176.7(9) . . . . ? F11 C62 C63 F12 -0.2(15) . . . . ? F11 C62 C63 C64 -179.7(9) . . . . ? F12 C63 C64 F13 0.4(16) . . . . ? F12 C63 C64 C65 179.4(9) . . . . ? F13 C64 C65 F14 -1.1(15) . . . . ? F13 C64 C65 C66 179.9(9) . . . . ? F14 C65 C66 F15 0.3(13) . . . . ? F14 C65 C66 C61 -179.4(8) . . . . ? F17 C49 C50 F16 -3.7(11) . . . . ? F17 C49 C50 C45 -179.5(7) . . . . ? F18 C48 C49 F17 2.6(13) . . . . ? F18 C48 C49 C50 -179.9(7) . . . . ? F19 C47 C48 F18 -0.9(13) . . . . ? F19 C47 C48 C49 -179.7(8) . . . . ? F20 C46 C47 F19 -1.7(12) . . . . ? F20 C46 C47 C48 178.5(8) . . . . ? N2 C30 C31 C32 -2.0(8) . . . . ? N2 C33 C34 C35 -172.2(7) . . . . ? N2 C33 C34 C40 4.4(11) . . . . ? N3 C40 C41 C42 -2.0(8) . . . . ? N3 C43 C44 C45 -173.6(6) . . . . ? N3 C43 C44 C53 8.8(9) . . . . ? N4 C52 C53 C44 162.2(6) . . . . ? N4 C52 C53 C54 1.2(8) . . . . ? N4 C55 C56 C57 1.4(11) . . . . ? N4 C55 C56 C61 -177.4(6) . . . . ? N5 C57 C58 C59 -0.6(9) . . . . ? N6 C20 C21 C22 -3.2(8) . . . . ? N6 C51 C52 N4 136.9(7) . . . . ? N6 C51 C52 C53 -37.7(11) . . . . ? N7 C16 C17 C18 2.5(8) . . . . ? C1 C2 C3 C4 30.0(11) . . . . ? C2 C1 C8 Ir1 -102.6(8) . . . . ? C2 C1 C8 C7 3.2(13) . . . . ? C2 C3 C4 Ir1 -10.4(9) . . . . ? C2 C3 C4 C5 -92.7(10) . . . . ? C3 C4 C5 Ir1 106.6(8) . . . . ? C3 C4 C5 C6 -1.8(12) . . . . ? C4 C5 C6 C7 57.6(10) . . . . ? C5 C6 C7 C8 20.7(10) . . . . ? C6 C7 C8 Ir1 -8.3(9) . . . . ? C6 C7 C8 C1 -88.5(10) . . . . ? C8 C1 C2 C3 47.2(12) . . . . ? C9 C10 C11 F2 -178.7(7) . . . . ? C9 C10 C11 C12 3.2(13) . . . . ? C9 C15 C16 N7 169.3(6) . . . . ? C9 C15 C16 C17 -12.3(11) . . . . ? C9 C15 C20 N6 179.1(6) . . . . ? C9 C15 C20 C21 11.8(11) . . . . ? C10 C9 C14 F5 -179.5(7) . . . . ? C10 C9 C14 C13 1.5(11) . . . . ? C10 C9 C15 C16 -76.1(9) . . . . ? C10 C9 C15 C20 107.6(8) . . . . ? C10 C11 C12 F3 179.6(8) . . . . ? C10 C11 C12 C13 -0.6(13) . . . . ? C11 C12 C13 F4 -177.4(7) . . . . ? C11 C12 C13 C14 -1.4(12) . . . . ? C12 C13 C14 F5 -178.1(7) . . . . ? C12 C13 C14 C9 0.9(12) . . . . ? C14 C9 C10 F1 176.7(6) . . . . ? C14 C9 C10 C11 -3.6(11) . . . . ? C14 C9 C15 C16 103.2(8) . . . . ? C14 C9 C15 C20 -73.2(10) . . . . ? C15 C9 C10 F1 -4.0(10) . . . . ? C15 C9 C10 C11 175.7(7) . . . . ? C15 C9 C14 F5 1.2(11) . . . . ? C15 C9 C14 C13 -177.8(7) . . . . ? C15 C16 C17 C18 -176.1(7) . . . . ? C15 C20 C21 C22 165.7(7) . . . . ? C16 N7 C19 C18 0.8(8) . . . . ? C16 C15 C20 N6 3.1(12) . . . . ? C16 C15 C20 C21 -164.2(7) . . . . ? C16 C17 C18 C19 -1.9(9) . . . . ? C17 C18 C19 N7 0.7(9) . . . . ? C19 N7 C16 C15 176.7(7) . . . . ? C19 N7 C16 C17 -2.0(8) . . . . ? C20 N6 C51 C22 0.2(8) . . . . ? C20 N6 C51 C52 -177.1(6) . . . . ? C20 C15 C16 N7 -14.6(12) . . . . ? C20 C15 C16 C17 163.8(7) . . . . ? C20 C21 C22 C23 -167.9(6) . . . . ? C20 C21 C22 C51 3.2(8) . . . . ? C21 C22 C23 C24 -50.7(9) . . . . ? C21 C22 C23 C30 115.1(8) . . . . ? C21 C22 C51 N6 -2.2(8) . . . . ? C21 C22 C51 C52 174.8(7) . . . . ? C22 C23 C24 C25 -71.5(9) . . . . ? C22 C23 C24 C29 102.8(8) . . . . ? C22 C23 C30 N2 9.7(11) . . . . ? C22 C23 C30 C31 -159.7(7) . . . . ? C22 C51 C52 N4 -39.9(11) . . . . ? C22 C51 C52 C53 145.6(7) . . . . ? C23 C22 C51 N6 167.1(7) . . . . ? C23 C22 C51 C52 -15.9(13) . . . . ? C23 C24 C25 F10 -2.4(11) . . . . ? C23 C24 C25 C26 174.6(7) . . . . ? C23 C24 C29 F6 3.5(12) . . . . ? C23 C24 C29 C28 -174.7(7) . . . . ? C23 C30 C31 C32 168.7(8) . . . . ? C24 C23 C30 N2 174.9(6) . . . . ? C24 C23 C30 C31 5.4(12) . . . . ? C24 C25 C26 F9 -177.6(8) . . . . ? C24 C25 C26 C27 -0.3(14) . . . . ? C25 C24 C29 F6 178.1(8) . . . . ? C25 C24 C29 C28 -0.2(12) . . . . ? C25 C26 C27 F8 -179.5(8) . . . . ? C25 C26 C27 C28 0.9(16) . . . . ? C26 C27 C28 F7 -178.1(9) . . . . ? C26 C27 C28 C29 -1.1(16) . . . . ? C27 C28 C29 F6 -177.6(9) . . . . ? C27 C28 C29 C24 0.8(14) . . . . ? C29 C24 C25 F10 -177.0(7) . . . . ? C29 C24 C25 C26 0.0(12) . . . . ? C30 N2 C33 C32 -1.8(8) . . . . ? C30 N2 C33 C34 176.8(7) . . . . ? C30 C23 C24 C25 122.4(8) . . . . ? C30 C23 C24 C29 -63.3(10) . . . . ? C30 C31 C32 C33 1.0(8) . . . . ? C31 C32 C33 N2 0.4(8) . . . . ? C31 C32 C33 C34 -177.9(8) . . . . ? C32 C33 C34 C35 5.9(13) . . . . ? C32 C33 C34 C40 -177.4(8) . . . . ? C33 N2 C30 C23 -169.8(7) . . . . ? C33 N2 C30 C31 2.4(8) . . . . ? C33 C34 C35 C36 51.7(11) . . . . ? C33 C34 C35 C38 -131.2(8) . . . . ? C33 C34 C40 N3 18.0(10) . . . . ? C33 C34 C40 C41 -153.1(7) . . . . ? C34 C35 C36 Cl2 2.3(11) . . . . ? C34 C35 C36 C37 179.6(8) . . . . ? C34 C35 C38 Cl1 1.7(10) . . . . ? C34 C35 C38 C39 -177.8(7) . . . . ? C34 C40 C41 C42 169.9(7) . . . . ? C35 C34 C40 N3 -165.2(6) . . . . ? C35 C34 C40 C41 23.7(11) . . . . ? C35 C36 C37 N1 -2.4(15) . . . . ? C35 C38 C39 N1 -1.9(14) . . . . ? C36 C35 C38 Cl1 179.1(6) . . . . ? C36 C35 C38 C39 -0.4(11) . . . . ? C37 N1 C39 C38 2.0(15) . . . . ? C38 C35 C36 Cl2 -175.0(6) . . . . ? C38 C35 C36 C37 2.3(11) . . . . ? C39 N1 C37 C36 0.1(16) . . . . ? C40 N3 C43 C42 -0.9(8) . . . . ? C40 N3 C43 C44 -176.6(6) . . . . ? C40 C34 C35 C36 -124.9(8) . . . . ? C40 C34 C35 C38 52.2(10) . . . . ? C40 C41 C42 C43 1.4(8) . . . . ? C41 C42 C43 N3 -0.4(8) . . . . ? C41 C42 C43 C44 174.1(8) . . . . ? C42 C43 C44 C45 12.1(12) . . . . ? C42 C43 C44 C53 -165.5(7) . . . . ? C43 N3 C40 C34 -171.0(6) . . . . ? C43 N3 C40 C41 1.7(8) . . . . ? C43 C44 C45 C46 46.4(9) . . . . ? C43 C44 C45 C50 -132.4(8) . . . . ? C43 C44 C53 C52 -67.4(9) . . . . ? C43 C44 C53 C54 90.3(9) . . . . ? C44 C45 C46 F20 4.3(11) . . . . ? C44 C45 C46 C47 -176.3(7) . . . . ? C44 C45 C50 F16 -0.4(11) . . . . ? C44 C45 C50 C49 175.3(7) . . . . ? C44 C53 C54 C55 -163.1(6) . . . . ? C45 C44 C53 C52 115.1(8) . . . . ? C45 C44 C53 C54 -87.2(9) . . . . ? C45 C46 C47 F19 178.9(7) . . . . ? C45 C46 C47 C48 -1.0(13) . . . . ? C46 C45 C50 F16 -179.2(7) . . . . ? C46 C45 C50 C49 -3.6(11) . . . . ? C46 C47 C48 F18 179.0(7) . . . . ? C46 C47 C48 C49 0.2(14) . . . . ? C47 C48 C49 F17 -178.6(8) . . . . ? C47 C48 C49 C50 -1.1(13) . . . . ? C48 C49 C50 F16 178.7(7) . . . . ? C48 C49 C50 C45 2.9(12) . . . . ? C50 C45 C46 F20 -176.8(7) . . . . ? C50 C45 C46 C47 2.6(11) . . . . ? C51 N6 C20 C15 -167.2(7) . . . . ? C51 N6 C20 C21 1.9(8) . . . . ? C51 C22 C23 C24 141.2(8) . . . . ? C51 C22 C23 C30 -53.0(11) . . . . ? C51 C52 C53 C44 -22.9(12) . . . . ? C51 C52 C53 C54 176.1(7) . . . . ? C52 N4 C55 C54 -0.1(7) . . . . ? C52 N4 C55 C56 -180.0(6) . . . . ? C52 C53 C54 C55 -1.1(8) . . . . ? C53 C44 C45 C46 -136.1(7) . . . . ? C53 C44 C45 C50 45.0(10) . . . . ? C53 C54 C55 N4 0.8(8) . . . . ? C53 C54 C55 C56 -179.3(7) . . . . ? C54 C55 C56 C57 -178.5(7) . . . . ? C54 C55 C56 C61 2.7(11) . . . . ? C55 N4 C52 C51 -176.1(6) . . . . ? C55 N4 C52 C53 -0.7(7) . . . . ? C55 C56 C57 N5 -0.6(11) . . . . ? C55 C56 C57 C58 -178.0(8) . . . . ? C55 C56 C61 C62 -106.5(9) . . . . ? C55 C56 C61 C66 76.2(10) . . . . ? C56 C57 C58 C59 177.2(8) . . . . ? C56 C61 C62 F11 2.7(13) . . . . ? C56 C61 C62 C63 -177.9(9) . . . . ? C56 C61 C66 F15 -2.0(12) . . . . ? C56 C61 C66 C65 177.7(8) . . . . ? C57 N5 C60 C59 -2.0(9) . . . . ? C57 C56 C61 C62 74.6(10) . . . . ? C57 C56 C61 C66 -102.7(8) . . . . ? C57 C58 C59 C60 -0.6(9) . . . . ? C58 C59 C60 N5 1.5(9) . . . . ? C60 N5 C57 C56 -176.4(7) . . . . ? C60 N5 C57 C58 1.6(8) . . . . ? C61 C56 C57 N5 178.2(6) . . . . ? C61 C56 C57 C58 0.8(12) . . . . ? C61 C62 C63 F12 -179.6(9) . . . . ? C61 C62 C63 C64 0.9(16) . . . . ? C62 C61 C66 F15 -179.5(8) . . . . ? C62 C61 C66 C65 0.2(13) . . . . ? C62 C63 C64 F13 179.8(9) . . . . ? C62 C63 C64 C65 -1.1(16) . . . . ? C63 C64 C65 F14 179.9(9) . . . . ? C63 C64 C65 C66 0.9(15) . . . . ? C64 C65 C66 F15 179.3(8) . . . . ? C64 C65 C66 C61 -0.4(14) . . . . ? C66 C61 C62 F11 -179.8(8) . . . . ? C66 C61 C62 C63 -0.5(14) . . . . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.002 0.109 0.315 403.5 81.8 ? 2 -0.002 -0.109 0.685 403.5 88.7 ? 3 -0.099 0.454 0.316 26.5 0.0 ? 4 0.099 0.546 0.684 26.5 0.0 ? 5 0.502 0.391 0.815 403.5 85.5 ? 6 0.498 0.609 0.185 403.5 85.0 ? 7 0.401 0.046 0.816 26.5 0.0 ? 8 0.599 0.954 0.184 26.5 0.0 ?