#------------------------------------------------------------------------------ #$Date: 2018-01-23 05:16:25 +0200 (Tue, 23 Jan 2018) $ #$Revision: 205481 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/53/7045338.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_7045338 loop_ _publ_author_name 'Congrave, Daniel G.' 'Hsu, Yu-Ting' 'Batsanov, Andrei S.' 'Beeby, Andrew' 'Bryce, Martin R.' _publ_section_title ; Sky-blue emitting bridged diiridium complexes: beneficial effects of intramolecular \p--\p stacking ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/C7DT04201A _journal_year 2018 _chemical_formula_moiety 'C84 H72 F6 Ir2 N6 O2, 5(C H2 Cl2)' _chemical_formula_sum 'C89 H82 Cl10 F6 Ir2 N6 O2' _chemical_formula_weight 2120.50 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _audit_creation_date 2016-12-27 _audit_creation_method ; Olex2 1.2-beta (compiled 2016.12.12 svn.r3370 for OlexSys, GUI svn.r5282) ; _audit_update_record ; 2017-09-22 deposited with the CCDC. 2017-12-14 downloaded from the CCDC. ; _cell_angle_alpha 66.269(3) _cell_angle_beta 77.005(3) _cell_angle_gamma 64.469(3) _cell_formula_units_Z 2 _cell_length_a 16.3594(14) _cell_length_b 17.7516(14) _cell_length_c 18.4512(15) _cell_measurement_reflns_used 9938 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 34.63 _cell_measurement_theta_min 2.55 _cell_volume 4417.7(6) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_collection 'APEX3 v.2016.1-0 (Bruker, 2016)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _diffrn_ambient_temperature 120 _diffrn_detector_area_resol_mean 10.4 _diffrn_detector_type 'Bruker PHOTON 100 CMOS' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device '3-circle area detector diffractometer' _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'focusing mirrors' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_unetI/netI 0.0462 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 115844 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 32.500 _diffrn_reflns_theta_max 33.142 _diffrn_reflns_theta_min 2.106 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\mS microsource' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.375 _exptl_absorpt_correction_T_max 0.3856 _exptl_absorpt_correction_T_min 0.2093 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details 'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1107 before and 0.0548 after correction. The Ratio of minimum to maximum transmission is 0.5428. The \l/2 correction factor is Not present.' _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2104 _exptl_crystal_preparation Luminescent _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.284 _exptl_crystal_size_min 0.214 _refine_diff_density_max 4.886 _refine_diff_density_min -1.519 _refine_diff_density_rms 0.153 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1129 _refine_ls_number_reflns 33660 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.027 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0387 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+10.4500P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0854 _refine_ls_wR_factor_ref 0.0972 _reflns_Friedel_coverage 0.000 _reflns_number_gt 25210 _reflns_number_total 33660 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt04201a2.cif _cod_data_source_block 12_16srv475 _cod_depositor_comments ; The following automatic conversions were performed: '_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according to /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas ; _cod_database_code 7045338 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.532 _shelx_estimated_absorpt_t_min 0.360 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups 2. Others Uiso(H31A)=Uiso(H31B)=Uiso(H31C)=FVAR(1) Uiso(H32A)=Uiso(H32B)=Uiso(H32C)=FVAR(2) Uiso(H33A)=Uiso(H33B)=Uiso(H33C)=FVAR(3) Uiso(H40A)=Uiso(H40B)=Uiso(H40C)=FVAR(4) Uiso(H41A)=Uiso(H41B)=Uiso(H41C)=FVAR(5) Uiso(H42A)=Uiso(H42B)=Uiso(H42C)=FVAR(6) Uiso(H40D)=Uiso(H40E)=Uiso(H40F)=FVAR(7) Uiso(H41D)=Uiso(H41E)=Uiso(H41F)=FVAR(8) Uiso(H31D)=Uiso(H31E)=Uiso(H31F)=Uiso(H42D)=Uiso(H42E)=Uiso(H42F)=FVAR(9) Uiso(H32D)=Uiso(H32E)=Uiso(H32F)=FVAR(10) Uiso(H33D)=Uiso(H33E)=Uiso(H33F)=FVAR(11) Fixed Sof: Cl5A(0.5) Cl6A(0.5) Cl5B(0.5) Cl6B(0.5) H3SA(0.5) H3SB(0.5) H3SC(0.5) H3SD(0.5) Cl1B(0.5) Cl2B(0.5) Cl1A(0.5) Cl2A(0.5) H1SC(0.5) H1SD(0.5) H1SA(0.5) H1SB(0.5) Cl3A(0.85) Cl4A(0.85) C2SA(0.85) H2SA(0.85) H2SB(0.85) Cl7A(0.75) Cl8A(0.75) C4SA(0.75) H4SA(0.75) H4SB(0.75) Cl3B(0.15) Cl4B(0.15) C2SB(0.15) H2SC(0.15) H2SD(0.15) Cl7B(0.25) Cl8B(0.25) C4SB(0.25) H4SC(0.25) H4SD(0.25) 3.a Secondary CH2 refined with riding coordinates: C3S(H3SA,H3SB), C3S(H3SC,H3SD), C1S(H1SC,H1SD), C1S(H1SA,H1SB), C2SA(H2SA, H2SB), C4SA(H4SA,H4SB), C2SB(H2SC,H2SD), C5S(H5SA,H5SB), C4SB(H4SC,H4SD) 3.b Aromatic/amide H refined with riding coordinates: C3A(H3A), C4A(H4A), C5A(H5A), C6A(H6A), C9A(H9A), C11A(H11A), C12A(H12A), C14A(H14A), C15A(H15A), C16A(H16A), C17A(H17A), C20A(H20A), C22A(H22A), C23A(H23A), C27A(H27A), C29A(H29A), C36A(H36A), C38A(H38A), C3B(H3B), C4B(H4B), C5B(H5B), C6B(H6B), C9B(H9B), C11B(H11B), C12B(H12B), C14B(H14B), C15B(H15B), C16B(H16B), C17B(H17B), C20B(H20B), C22B(H22B), C23B(H23B), C27B(H27B), C29B(H29B), C36B(H36B), C38B(H38B) 3.c Idealised Me refined as rotating group: C31A(H31A,H31B,H31C), C32A(H32A,H32B,H32C), C33A(H33A,H33B,H33C), C40A(H40A, H40B,H40C), C41A(H41A,H41B,H41C), C42A(H42A,H42B,H42C), C31B(H31D,H31E,H31F), C32B(H32D,H32E,H32F), C33B(H33D,H33E,H33F), C40B(H40D,H40E,H40F), C41B(H41D, H41E,H41F), C42B(H42D,H42E,H42F) ; _shelx_res_file ; 16srv475.res created by SHELXL-2014/7 TITL 16srv475 in P-1 #2 REM reset to P-1 #2 CELL 0.71073 16.3594 17.7516 18.4512 66.2688 77.0054 64.469 ZERR 2 0.0014 0.0014 0.0015 0.0029 0.0031 0.0028 LATT 1 SFAC C H Cl F Ir N O UNIT 178 164 20 12 4 12 4 L.S. 7 PLAN 10 SIZE 0.214 0.284 0.38 TEMP -153.15 BOND fmap 2 acta 65 REM REM REM WGHT 0.039000 10.450000 FVAR 0.07369 0.09173 0.11006 0.05221 0.04778 0.05369 0.04407 FVAR 0.08523 0.10569 0.04828 0.06956 0.04270 IRA 5 0.432366 0.379929 0.071740 11.00000 0.01830 0.01615 = 0.01587 -0.00506 -0.00245 -0.00820 F1A 4 0.699160 0.443486 0.080646 11.00000 0.03021 0.03111 = 0.03500 -0.00867 -0.01313 -0.01399 F2A 4 0.749353 0.396387 -0.017425 11.00000 0.02315 0.04393 = 0.04084 -0.01660 0.00617 -0.01313 F3A 4 0.730654 0.307276 0.098918 11.00000 0.02810 0.02095 = 0.05746 0.00615 -0.02244 -0.00923 O1A 7 0.577536 0.343968 0.056743 11.00000 0.01884 0.01786 = 0.02147 -0.00609 -0.00392 -0.00707 N1A 6 0.454455 0.504394 -0.001683 11.00000 0.01740 0.02060 = 0.01554 -0.00426 -0.00370 -0.00927 N2A 6 0.447928 0.389791 0.173899 11.00000 0.02093 0.01722 = 0.01728 -0.00537 -0.00225 -0.00877 N3A 6 0.418847 0.356132 -0.022665 11.00000 0.01972 0.02029 = 0.01882 -0.00634 -0.00314 -0.01084 C1A 1 0.597786 0.411798 0.033588 11.00000 0.01685 0.02154 = 0.01572 -0.00576 -0.00222 -0.00832 C2A 1 0.443420 0.258469 0.146469 11.00000 0.01936 0.01716 = 0.01996 -0.00646 -0.00034 -0.00819 C3A 1 0.430387 0.192020 0.132825 11.00000 0.02912 0.01922 = 0.02426 -0.00681 -0.00540 -0.01070 AFIX 43 H3A 2 0.410323 0.204523 0.083250 11.00000 -1.20000 AFIX 0 C4A 1 0.446537 0.107939 0.191152 11.00000 0.03000 0.01930 = 0.03394 -0.00842 -0.00629 -0.01135 AFIX 43 H4A 2 0.437939 0.063757 0.180633 11.00000 -1.20000 AFIX 0 C5A 1 0.475047 0.088304 0.264384 11.00000 0.03436 0.01989 = 0.02817 -0.00224 -0.00784 -0.01206 AFIX 43 H5A 2 0.486316 0.030796 0.303567 11.00000 -1.20000 AFIX 0 C6A 1 0.487001 0.152670 0.280152 11.00000 0.03042 0.02059 = 0.02278 -0.00392 -0.00693 -0.01111 AFIX 43 H6A 2 0.506225 0.139652 0.330237 11.00000 -1.20000 AFIX 0 C7A 1 0.470588 0.237199 0.221812 11.00000 0.01901 0.01802 = 0.02187 -0.00625 -0.00329 -0.00756 C8A 1 0.475672 0.310635 0.235913 11.00000 0.01784 0.01789 = 0.01941 -0.00669 -0.00056 -0.00746 C9A 1 0.503315 0.305875 0.304037 11.00000 0.02408 0.01862 = 0.01865 -0.00419 -0.00446 -0.00867 AFIX 43 H9A 2 0.523526 0.250347 0.346129 11.00000 -1.20000 AFIX 0 C10A 1 0.501746 0.381277 0.311311 11.00000 0.02446 0.02356 = 0.01793 -0.00627 -0.00293 -0.01187 C11A 1 0.468585 0.462252 0.249104 11.00000 0.03226 0.02101 = 0.02186 -0.00800 -0.00381 -0.01116 AFIX 43 H11A 2 0.463364 0.515871 0.253115 11.00000 -1.20000 AFIX 0 C12A 1 0.443486 0.463568 0.181763 11.00000 0.02762 0.01738 = 0.02121 -0.00634 -0.00544 -0.00880 AFIX 43 H12A 2 0.422287 0.518710 0.139421 11.00000 -1.20000 AFIX 0 C13A 1 0.299452 0.406964 0.085253 11.00000 0.02035 0.01536 = 0.01882 -0.00391 -0.00390 -0.00752 C14A 1 0.237712 0.431741 0.145580 11.00000 0.02700 0.02340 = 0.02071 -0.00873 -0.00122 -0.01092 AFIX 43 H14A 2 0.257782 0.441040 0.184614 11.00000 -1.20000 AFIX 0 C15A 1 0.147243 0.443022 0.149403 11.00000 0.02540 0.02563 = 0.02797 -0.01129 0.00491 -0.01061 AFIX 43 H15A 2 0.106470 0.459827 0.190889 11.00000 -1.20000 AFIX 0 C16A 1 0.116293 0.429832 0.092875 11.00000 0.01979 0.02663 = 0.03520 -0.01233 0.00079 -0.00917 AFIX 43 H16A 2 0.054354 0.438558 0.095330 11.00000 -1.20000 AFIX 0 C17A 1 0.175873 0.403954 0.032975 11.00000 0.02319 0.02209 = 0.02929 -0.00743 -0.00343 -0.01240 AFIX 43 H17A 2 0.155156 0.394325 -0.005456 11.00000 -1.20000 AFIX 0 C18A 1 0.266531 0.392145 0.029526 11.00000 0.02032 0.01709 = 0.02284 -0.00566 -0.00213 -0.00822 C19A 1 0.335086 0.361985 -0.029816 11.00000 0.02281 0.01763 = 0.01838 -0.00482 -0.00371 -0.00953 C20A 1 0.323302 0.334140 -0.085912 11.00000 0.02529 0.02084 = 0.02242 -0.00607 -0.00635 -0.00997 AFIX 43 H20A 2 0.264403 0.339905 -0.091671 11.00000 -1.20000 AFIX 0 C21A 1 0.396153 0.298058 -0.133645 11.00000 0.02926 0.02175 = 0.01779 -0.00502 -0.00598 -0.01086 C22A 1 0.480412 0.296192 -0.127103 11.00000 0.02485 0.03243 = 0.02477 -0.01442 0.00102 -0.01239 AFIX 43 H22A 2 0.531313 0.274867 -0.160538 11.00000 -1.20000 AFIX 0 C23A 1 0.488993 0.325778 -0.071321 11.00000 0.02230 0.03044 = 0.02046 -0.01030 0.00065 -0.01337 AFIX 43 H23A 2 0.546464 0.324572 -0.067316 11.00000 -1.20000 AFIX 0 C24A 1 0.695010 0.390192 0.048738 11.00000 0.02101 0.01873 = 0.02741 -0.00437 -0.00618 -0.00822 C25A 1 0.533534 0.378074 0.382473 11.00000 0.02855 0.02100 = 0.01854 -0.00650 -0.00600 -0.00957 C26A 1 0.478246 0.374988 0.452454 11.00000 0.03451 0.03948 = 0.02387 -0.01355 -0.00179 -0.01723 C27A 1 0.509390 0.375023 0.517006 11.00000 0.05053 0.04580 = 0.02333 -0.01582 -0.00310 -0.01926 AFIX 43 H27A 2 0.472145 0.372559 0.564851 11.00000 -1.20000 AFIX 0 C28A 1 0.593258 0.378565 0.512845 11.00000 0.04859 0.02748 = 0.03223 -0.01135 -0.01926 -0.00923 C29A 1 0.647583 0.380811 0.442963 11.00000 0.03471 0.02349 = 0.03412 -0.00812 -0.01503 -0.01041 AFIX 43 H29A 2 0.705415 0.382810 0.439847 11.00000 -1.20000 AFIX 0 C30A 1 0.619732 0.380219 0.377470 11.00000 0.02836 0.01669 = 0.02657 -0.00393 -0.00901 -0.00826 C31A 1 0.386116 0.372163 0.458811 11.00000 0.04745 0.08690 = 0.03462 -0.03003 0.01050 -0.04003 AFIX 137 H31A 2 0.354225 0.415790 0.410944 11.00000 21.00000 H31B 2 0.350929 0.386416 0.505370 11.00000 21.00000 H31C 2 0.393254 0.312445 0.464254 11.00000 21.00000 AFIX 0 C32A 1 0.625027 0.381061 0.583024 11.00000 0.07349 0.05237 = 0.04156 -0.01992 -0.02700 -0.02001 AFIX 137 H32A 2 0.681824 0.329861 0.599840 11.00000 31.00000 H32B 2 0.578619 0.378672 0.627035 11.00000 31.00000 H32C 2 0.635088 0.436256 0.567374 11.00000 31.00000 AFIX 0 C33A 1 0.681359 0.380178 0.303465 11.00000 0.02975 0.03361 = 0.03286 -0.01153 -0.00358 -0.01198 AFIX 137 H33A 2 0.695032 0.325986 0.292845 11.00000 41.00000 H33B 2 0.737895 0.382038 0.310749 11.00000 41.00000 H33C 2 0.651304 0.432484 0.258581 11.00000 41.00000 AFIX 0 C34A 1 0.383727 0.259346 -0.187030 11.00000 0.02679 0.02395 = 0.01887 -0.00823 -0.00516 -0.01029 C35A 1 0.347687 0.315060 -0.260943 11.00000 0.02911 0.02497 = 0.01943 -0.00603 -0.00492 -0.00735 C36A 1 0.330360 0.278186 -0.306840 11.00000 0.02907 0.03604 = 0.01730 -0.00816 -0.00659 -0.00790 AFIX 43 H36A 2 0.305526 0.315986 -0.356868 11.00000 -1.20000 AFIX 0 C37A 1 0.348200 0.188178 -0.281829 11.00000 0.02666 0.04056 = 0.02293 -0.01836 -0.00074 -0.01311 C38A 1 0.386119 0.133875 -0.209248 11.00000 0.03182 0.02756 = 0.02604 -0.01187 -0.00317 -0.01348 AFIX 43 H38A 2 0.399654 0.071804 -0.191602 11.00000 -1.20000 AFIX 0 C39A 1 0.404910 0.167902 -0.161486 11.00000 0.02950 0.02556 = 0.01881 -0.00670 -0.00515 -0.01153 C40A 1 0.328929 0.413006 -0.290787 11.00000 0.05320 0.02360 = 0.02975 -0.00282 -0.01293 -0.00623 AFIX 137 H40A 2 0.284155 0.440310 -0.254265 11.00000 51.00000 H40B 2 0.305115 0.441231 -0.343553 11.00000 51.00000 H40C 2 0.385305 0.421244 -0.293971 11.00000 51.00000 AFIX 0 C41A 1 0.328216 0.150159 -0.332585 11.00000 0.03870 0.05968 = 0.03268 -0.03029 0.00057 -0.02083 AFIX 137 H41A 2 0.376134 0.143642 -0.375051 11.00000 61.00000 H41B 2 0.269658 0.190357 -0.355857 11.00000 61.00000 H41C 2 0.325875 0.091782 -0.299818 11.00000 61.00000 AFIX 0 C42A 1 0.447784 0.105548 -0.083617 11.00000 0.05259 0.02720 = 0.02462 -0.00165 -0.01489 -0.01613 AFIX 137 H42A 2 0.511867 0.097033 -0.089006 11.00000 71.00000 H42B 2 0.443086 0.047997 -0.069247 11.00000 71.00000 H42C 2 0.416193 0.131193 -0.042119 11.00000 71.00000 AFIX 0 IRB 5 0.053967 0.128320 0.462406 11.00000 0.02060 0.01538 = 0.01957 -0.00661 -0.00216 -0.00800 F1B 4 0.165920 -0.210822 0.590534 11.00000 0.03124 0.01928 = 0.04052 0.00276 -0.01020 -0.00859 F2B 4 0.184241 -0.189389 0.465186 11.00000 0.03252 0.02811 = 0.05096 -0.02537 -0.00300 -0.00519 F3B 4 0.266671 -0.160704 0.518081 11.00000 0.01830 0.02326 = 0.05483 -0.01010 -0.00607 -0.00537 O1B 7 0.150010 -0.004853 0.485232 11.00000 0.02116 0.02040 = 0.02270 -0.00833 -0.00177 -0.00901 N1B 6 -0.027875 0.046833 0.491227 11.00000 0.02177 0.01472 = 0.01796 -0.00487 -0.00274 -0.00734 N2B 6 0.072876 0.147017 0.344186 11.00000 0.02309 0.01789 = 0.01927 -0.00362 -0.00404 -0.01079 N3B 6 0.033700 0.120474 0.577454 11.00000 0.02299 0.02151 = 0.02242 -0.01027 -0.00117 -0.00959 C1B 1 0.114209 -0.061147 0.502609 11.00000 0.02017 0.01746 = 0.01625 -0.00718 -0.00332 -0.00559 C2B 1 0.150199 0.177820 0.432638 11.00000 0.02147 0.01837 = 0.02323 -0.00827 -0.00211 -0.00851 C3B 1 0.192166 0.190666 0.482209 11.00000 0.02853 0.03482 = 0.02601 -0.01513 0.00016 -0.01643 AFIX 43 H3B 2 0.173966 0.176229 0.537137 11.00000 -1.20000 AFIX 0 C4B 1 0.260147 0.224243 0.452444 11.00000 0.03014 0.04329 = 0.03309 -0.02056 -0.00079 -0.02025 AFIX 43 H4B 2 0.287944 0.232236 0.487346 11.00000 -1.20000 AFIX 0 C5B 1 0.288066 0.246273 0.372601 11.00000 0.02959 0.04028 = 0.03532 -0.01783 0.00078 -0.02135 AFIX 43 H5B 2 0.333959 0.270122 0.352818 11.00000 -1.20000 AFIX 0 C6B 1 0.248686 0.233334 0.321720 11.00000 0.02508 0.02913 = 0.02511 -0.00885 -0.00069 -0.01427 AFIX 43 H6B 2 0.268273 0.247153 0.267086 11.00000 -1.20000 AFIX 0 C7B 1 0.180006 0.199841 0.351301 11.00000 0.02073 0.01651 = 0.02631 -0.00636 -0.00512 -0.00779 C8B 1 0.133736 0.184667 0.302189 11.00000 0.02077 0.01684 = 0.02443 -0.00675 -0.00496 -0.00660 C9B 1 0.144251 0.208252 0.219942 11.00000 0.02316 0.01945 = 0.02207 -0.00447 -0.00352 -0.00983 AFIX 43 H9B 2 0.186648 0.234847 0.190907 11.00000 -1.20000 AFIX 0 C10B 1 0.093405 0.193314 0.179862 11.00000 0.02476 0.02109 = 0.02084 -0.00634 -0.00254 -0.01043 C11B 1 0.035057 0.150096 0.225547 11.00000 0.03235 0.03102 = 0.02475 -0.00926 -0.00354 -0.01922 AFIX 43 H11B 2 0.001213 0.136078 0.200736 11.00000 -1.20000 AFIX 0 C12B 1 0.027087 0.128177 0.306147 11.00000 0.02870 0.02386 = 0.02445 -0.00677 -0.00297 -0.01656 AFIX 43 H12B 2 -0.012397 0.098442 0.336464 11.00000 -1.20000 AFIX 0 C13B 1 -0.030327 0.253518 0.449419 11.00000 0.02427 0.02100 = 0.03120 -0.00998 -0.00386 -0.01083 C14B 1 -0.059232 0.325483 0.379029 11.00000 0.02573 0.02086 = 0.03606 -0.00752 -0.00264 -0.00891 AFIX 43 H14B 2 -0.040867 0.315755 0.329844 11.00000 -1.20000 AFIX 0 C15B 1 -0.113931 0.410476 0.379383 11.00000 0.03200 0.02164 = 0.05207 -0.00757 -0.00755 -0.01052 AFIX 43 H15B 2 -0.131860 0.458118 0.330650 11.00000 -1.20000 AFIX 0 C16B 1 -0.142783 0.426630 0.450384 11.00000 0.03129 0.02350 = 0.06459 -0.01999 -0.01314 -0.00587 AFIX 43 H16B 2 -0.181290 0.484875 0.450191 11.00000 -1.20000 AFIX 0 C17B 1 -0.115463 0.358012 0.521167 11.00000 0.02971 0.03084 = 0.05268 -0.02697 -0.00938 -0.00409 AFIX 43 H17B 2 -0.134860 0.368627 0.569938 11.00000 -1.20000 AFIX 0 C18B 1 -0.058960 0.272720 0.520397 11.00000 0.02410 0.02403 = 0.03934 -0.01727 -0.00577 -0.00760 C19B 1 -0.023588 0.196375 0.592054 11.00000 0.02202 0.02484 = 0.03405 -0.01749 -0.00220 -0.00702 C20B 1 -0.042201 0.196040 0.670095 11.00000 0.02871 0.03517 = 0.03980 -0.02592 -0.00124 -0.00878 AFIX 43 H20B 2 -0.082484 0.248996 0.680065 11.00000 -1.20000 AFIX 0 C21B 1 -0.003008 0.120217 0.732338 11.00000 0.03001 0.03951 = 0.02965 -0.01964 0.00153 -0.01624 C22B 1 0.056123 0.043100 0.715567 11.00000 0.03273 0.03344 = 0.02434 -0.01378 -0.00002 -0.01368 AFIX 43 H22B 2 0.084509 -0.010612 0.757112 11.00000 -1.20000 AFIX 0 C23B 1 0.072334 0.046447 0.638206 11.00000 0.02691 0.02234 = 0.02526 -0.01035 -0.00078 -0.00892 AFIX 43 H23B 2 0.112638 -0.005908 0.627245 11.00000 -1.20000 AFIX 0 C24B 1 0.182661 -0.156832 0.519220 11.00000 0.02031 0.01814 = 0.03649 -0.00973 -0.00482 -0.00534 C25B 1 0.096391 0.227114 0.091269 11.00000 0.02751 0.02450 = 0.01969 -0.00448 -0.00383 -0.01566 C26B 1 0.020572 0.299368 0.053260 11.00000 0.02626 0.02707 = 0.02396 -0.00438 -0.00532 -0.01498 C27B 1 0.025550 0.334258 -0.029001 11.00000 0.03305 0.03168 = 0.02613 -0.00278 -0.00878 -0.01786 AFIX 43 H27B 2 -0.025396 0.383246 -0.055189 11.00000 -1.20000 AFIX 0 C28B 1 0.102412 0.300058 -0.074380 11.00000 0.04571 0.03363 = 0.02298 -0.00538 -0.00459 -0.02608 C29B 1 0.174524 0.226733 -0.035700 11.00000 0.03467 0.03326 = 0.02653 -0.01208 0.00177 -0.02055 AFIX 43 H29B 2 0.226428 0.200934 -0.066089 11.00000 -1.20000 AFIX 0 C30B 1 0.173221 0.189425 0.046990 11.00000 0.02849 0.02821 = 0.02442 -0.00884 -0.00217 -0.01667 C31B 1 -0.064111 0.340953 0.098939 11.00000 0.02612 0.03597 = 0.03423 -0.00628 -0.00475 -0.01354 AFIX 137 H31D 2 -0.100195 0.303889 0.117908 11.00000 101.00000 H31E 2 -0.099891 0.400532 0.064285 11.00000 101.00000 H31F 2 -0.047345 0.345496 0.144345 11.00000 101.00000 AFIX 0 C32B 1 0.106491 0.343520 -0.163565 11.00000 0.06709 0.04935 = 0.02567 -0.00782 -0.00515 -0.02839 AFIX 137 H32D 2 0.100451 0.405068 -0.177746 11.00000 111.00000 H32E 2 0.056900 0.343229 -0.184822 11.00000 111.00000 H32F 2 0.164769 0.310468 -0.186000 11.00000 111.00000 AFIX 0 C33B 1 0.254934 0.110305 0.086776 11.00000 0.02998 0.03619 = 0.03467 -0.01403 -0.00278 -0.01173 AFIX 137 H33D 2 0.294977 0.131237 0.098927 11.00000 121.00000 H33E 2 0.287957 0.076601 0.051141 11.00000 121.00000 H33F 2 0.234766 0.071855 0.136019 11.00000 121.00000 AFIX 0 C34B 1 -0.019073 0.120396 0.815598 11.00000 0.02980 0.04209 = 0.03105 -0.02325 0.00149 -0.01489 C35B 1 -0.088997 0.098355 0.865720 11.00000 0.02904 0.05565 = 0.04118 -0.03077 0.00367 -0.01988 C36B 1 -0.101649 0.099922 0.941948 11.00000 0.03618 0.05666 = 0.03994 -0.02996 0.00945 -0.02489 AFIX 43 H36B 2 -0.148877 0.084201 0.976507 11.00000 -1.20000 AFIX 0 C37B 1 -0.047124 0.123876 0.969287 11.00000 0.04246 0.04651 = 0.02969 -0.02155 -0.00102 -0.01829 C38B 1 0.022691 0.143420 0.919253 11.00000 0.04015 0.05479 = 0.03836 -0.02754 -0.00238 -0.02425 AFIX 43 H38B 2 0.061660 0.157962 0.937858 11.00000 -1.20000 AFIX 0 C39B 1 0.038242 0.142617 0.842074 11.00000 0.03791 0.04993 = 0.03446 -0.02462 0.00449 -0.02505 C40B 1 -0.150022 0.071827 0.838783 11.00000 0.04526 0.10984 = 0.06945 -0.06457 0.01816 -0.04781 AFIX 137 H40D 2 -0.175408 0.117464 0.788791 11.00000 81.00000 H40E 2 -0.199471 0.066117 0.879255 11.00000 81.00000 H40F 2 -0.114774 0.014690 0.830828 11.00000 81.00000 AFIX 0 C41B 1 -0.064028 0.127408 1.052040 11.00000 0.05908 0.06819 = 0.03078 -0.02949 0.00340 -0.02804 AFIX 137 H41D 2 -0.115934 0.182019 1.053219 11.00000 91.00000 H41E 2 -0.010040 0.126937 1.067153 11.00000 91.00000 H41F 2 -0.077070 0.075559 1.089408 11.00000 91.00000 AFIX 0 C42B 1 0.115293 0.164600 0.788525 11.00000 0.05533 0.08652 = 0.05252 -0.04393 0.01960 -0.05186 AFIX 137 H42D 2 0.148669 0.119958 0.762973 11.00000 101.00000 H42E 2 0.156327 0.164556 0.819926 11.00000 101.00000 H42F 2 0.090990 0.223581 0.747854 11.00000 101.00000 AFIX 0 PART 1 CL5A 3 0.148275 0.610298 0.249603 10.50000 0.11921 0.05359 = 0.06732 -0.03441 0.01484 -0.04083 CL6A 3 0.282283 0.692361 0.191626 10.50000 0.05817 0.06714 = 0.18653 -0.03621 -0.02979 -0.00285 PART 0 PART 2 CL5B 3 0.227450 0.599939 0.277608 10.50000 0.10734 0.18977 = 0.06563 -0.04419 0.01668 0.04412 CL6B 3 0.285455 0.700547 0.125578 10.50000 0.03829 0.05620 = 0.16345 -0.03933 0.01456 -0.01340 PART 0 C3S 1 0.200523 0.665932 0.173258 11.00000 0.08939 0.07721 = 0.06923 -0.04364 0.03087 -0.03394 PART 1 AFIX 23 H3SA 2 0.153440 0.722260 0.143404 10.50000 -1.20000 H3SB 2 0.229405 0.630670 0.137755 10.50000 -1.20000 AFIX 23 PART 0 PART 2 H3SC 2 0.193943 0.629117 0.148149 10.50000 -1.20000 H3SD 2 0.142623 0.717862 0.170314 10.50000 -1.20000 AFIX 0 PART 0 PART 1 CL1B 3 0.723843 0.087596 0.187376 10.50000 0.05871 0.07923 = 0.09073 -0.00416 0.01334 -0.02565 CL2B 3 0.682237 0.059883 0.055976 10.50000 0.08429 0.06902 = 0.11878 -0.05768 0.05743 -0.05314 PART 0 PART 2 CL1A 3 0.744420 0.049637 0.164562 10.50000 0.06442 0.09756 = 0.12136 0.02837 -0.01900 -0.02739 CL2A 3 0.653843 0.093371 0.024107 10.50000 0.06462 0.07875 = 0.10057 -0.04103 0.01598 -0.03421 PART 0 C1S 1 0.669518 0.133488 0.096902 11.00000 0.04053 0.04863 = 0.13017 -0.04001 -0.00766 -0.00359 PART 2 AFIX 23 H1SC 2 0.692123 0.182104 0.068502 10.50000 -1.20000 H1SD 2 0.610329 0.157699 0.124663 10.50000 -1.20000 AFIX 23 PART 0 PART 1 H1SA 2 0.603820 0.165265 0.107013 10.50000 -1.20000 H1SB 2 0.693510 0.178092 0.057987 10.50000 -1.20000 AFIX 0 CL3A 3 0.303333 -0.023894 0.319420 10.85000 0.08628 0.04046 = 0.04138 -0.01475 -0.00426 -0.01969 CL4A 3 0.364064 -0.161087 0.251671 10.85000 0.07677 0.09078 = 0.08464 -0.06756 -0.00974 -0.00830 C2SA 1 0.381854 -0.131725 0.325113 10.85000 0.04023 0.05789 = 0.04729 -0.02688 -0.00442 -0.01054 AFIX 23 H2SA 2 0.444413 -0.133516 0.317858 10.85000 -1.20000 H2SB 2 0.374711 -0.174940 0.378095 10.85000 -1.20000 AFIX 0 CL7A 3 0.096574 0.358594 0.578804 10.75000 0.08779 0.05655 = 0.11232 -0.03582 -0.02922 -0.00949 CL8A 3 0.142798 0.452742 0.419892 10.75000 0.06607 0.06000 = 0.18493 -0.06985 0.02616 -0.03478 C4SA 1 0.072958 0.400077 0.477459 10.75000 0.04434 0.04151 = 0.12315 -0.02979 -0.01223 -0.01668 AFIX 23 H4SA 2 0.081843 0.350220 0.461095 10.75000 -1.20000 H4SB 2 0.008954 0.442160 0.470413 10.75000 -1.20000 AFIX 0 PART 0 PART 2 CL3B 3 0.254659 -0.035077 0.316589 10.15000 0.06553 CL4B 3 0.417520 -0.163841 0.270035 10.15000 0.06961 C2SB 1 0.323244 -0.142078 0.335101 10.15000 0.04540 AFIX 23 H2SC 2 0.287145 -0.174765 0.335155 10.15000 -1.20000 H2SD 2 0.344383 -0.166568 0.389163 10.15000 -1.20000 AFIX 0 PART 0 CL9 3 0.541834 0.099519 0.515121 11.00000 0.04514 0.06936 = 0.05327 -0.00946 0.00539 0.01020 CL10 3 0.678113 0.030797 0.401466 11.00000 0.04189 0.08431 = 0.04356 -0.02799 -0.01183 -0.00462 C5S 1 0.646893 0.015779 0.503241 11.00000 0.03128 0.03998 = 0.04150 -0.01053 -0.00557 -0.00711 AFIX 23 H5SA 2 0.642677 -0.043255 0.531149 11.00000 -1.20000 H5SB 2 0.694197 0.017389 0.527282 11.00000 -1.20000 AFIX 0 PART 2 CL7B 3 0.117104 0.432094 0.479035 10.25000 0.07195 0.10682 = 0.12174 -0.08953 -0.03788 -0.00043 CL8B 3 0.019961 0.540314 0.330842 10.25000 0.09902 0.04119 = 0.05269 0.01124 -0.03230 -0.02560 C4SB 1 0.077245 0.434823 0.398806 10.25000 0.03219 AFIX 23 H4SC 2 0.035708 0.402494 0.419080 10.25000 -1.20000 H4SD 2 0.129423 0.401555 0.369713 10.25000 -1.20000 AFIX 0 HKLF 4 REM 16srv475 in P-1 #2 REM R1 = 0.0387 for 25210 Fo > 4sig(Fo) and 0.0647 for all 33660 data REM 1129 parameters refined using 0 restraints END WGHT 0.0382 10.5771 REM Highest difference peak 4.886, deepest hole -1.519, 1-sigma level 0.153 Q1 1 0.0005 0.1577 0.4593 11.00000 0.05 4.89 Q2 1 0.0804 0.1123 0.3965 11.00000 0.05 3.48 Q3 1 0.3207 0.1264 0.1440 11.00000 0.05 3.44 Q4 1 0.4585 0.3667 0.0028 11.00000 0.05 3.44 Q5 1 0.1910 0.3666 0.3173 11.00000 0.05 2.71 Q6 1 0.3921 0.4209 0.0756 11.00000 0.05 2.21 Q7 1 0.4795 0.3544 0.0910 11.00000 0.05 1.99 Q8 1 0.1914 -0.1747 0.7447 11.00000 0.05 1.58 Q9 1 0.4762 0.3343 0.0658 11.00000 0.05 1.57 Q10 1 0.4176 0.3386 0.0990 11.00000 0.05 1.36 ; _shelx_res_checksum 51079 _olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems' _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_occupancy _atom_site_disorder_assembly _atom_site_disorder_group IrA Ir 0.43237(2) 0.37993(2) 0.07174(2) 0.01608(3) Uani 1 1 d . . . . F1A F 0.69916(14) 0.44349(14) 0.08065(13) 0.0302(4) Uani 1 1 d . . . . F2A F 0.74935(14) 0.39639(16) -0.01742(14) 0.0367(5) Uani 1 1 d . . . . F3A F 0.73065(15) 0.30728(14) 0.09892(15) 0.0388(6) Uani 1 1 d . . . . O1A O 0.57754(14) 0.34397(14) 0.05674(13) 0.0191(4) Uani 1 1 d . . . . N1A N 0.45446(16) 0.50439(17) -0.00168(15) 0.0173(5) Uani 1 1 d . . . . N2A N 0.44793(17) 0.38979(16) 0.17390(15) 0.0179(5) Uani 1 1 d . . . . N3A N 0.41885(17) 0.35613(17) -0.02266(15) 0.0182(5) Uani 1 1 d . . . . C1A C 0.5978(2) 0.4118(2) 0.03359(17) 0.0177(5) Uani 1 1 d . . . . C2A C 0.4434(2) 0.25847(19) 0.14647(18) 0.0185(5) Uani 1 1 d . . . . C3A C 0.4304(2) 0.1920(2) 0.1328(2) 0.0232(6) Uani 1 1 d . . . . H3A H 0.4103 0.2045 0.0833 0.028 Uiso 1 1 calc R . . . C4A C 0.4465(2) 0.1079(2) 0.1912(2) 0.0265(7) Uani 1 1 d . . . . H4A H 0.4379 0.0638 0.1806 0.032 Uiso 1 1 calc R . . . C5A C 0.4750(2) 0.0883(2) 0.2644(2) 0.0279(7) Uani 1 1 d . . . . H5A H 0.4863 0.0308 0.3036 0.033 Uiso 1 1 calc R . . . C6A C 0.4870(2) 0.1527(2) 0.2802(2) 0.0244(6) Uani 1 1 d . . . . H6A H 0.5062 0.1397 0.3302 0.029 Uiso 1 1 calc R . . . C7A C 0.4706(2) 0.2372(2) 0.22181(18) 0.0193(5) Uani 1 1 d . . . . C8A C 0.4757(2) 0.31063(19) 0.23591(18) 0.0182(5) Uani 1 1 d . . . . C9A C 0.5033(2) 0.3059(2) 0.30404(18) 0.0205(6) Uani 1 1 d . . . . H9A H 0.5235 0.2503 0.3461 0.025 Uiso 1 1 calc R . . . C10A C 0.5017(2) 0.3813(2) 0.31131(18) 0.0210(6) Uani 1 1 d . . . . C11A C 0.4686(2) 0.4623(2) 0.24910(19) 0.0241(6) Uani 1 1 d . . . . H11A H 0.4634 0.5159 0.2531 0.029 Uiso 1 1 calc R . . . C12A C 0.4435(2) 0.4636(2) 0.18176(19) 0.0214(6) Uani 1 1 d . . . . H12A H 0.4223 0.5187 0.1394 0.026 Uiso 1 1 calc R . . . C13A C 0.2995(2) 0.40696(19) 0.08525(18) 0.0181(5) Uani 1 1 d . . . . C14A C 0.2377(2) 0.4317(2) 0.14558(19) 0.0229(6) Uani 1 1 d . . . . H14A H 0.2578 0.4410 0.1846 0.027 Uiso 1 1 calc R . . . C15A C 0.1472(2) 0.4430(2) 0.1494(2) 0.0265(7) Uani 1 1 d . . . . H15A H 0.1065 0.4598 0.1909 0.032 Uiso 1 1 calc R . . . C16A C 0.1163(2) 0.4298(2) 0.0929(2) 0.0270(7) Uani 1 1 d . . . . H16A H 0.0544 0.4386 0.0953 0.032 Uiso 1 1 calc R . . . C17A C 0.1759(2) 0.4040(2) 0.0330(2) 0.0236(6) Uani 1 1 d . . . . H17A H 0.1552 0.3943 -0.0055 0.028 Uiso 1 1 calc R . . . C18A C 0.2665(2) 0.3921(2) 0.02953(19) 0.0200(6) Uani 1 1 d . . . . C19A C 0.3351(2) 0.3620(2) -0.02982(18) 0.0190(5) Uani 1 1 d . . . . C20A C 0.3233(2) 0.3341(2) -0.08591(19) 0.0220(6) Uani 1 1 d . . . . H20A H 0.2644 0.3399 -0.0917 0.026 Uiso 1 1 calc R . . . C21A C 0.3962(2) 0.2981(2) -0.13364(18) 0.0223(6) Uani 1 1 d . . . . C22A C 0.4804(2) 0.2962(2) -0.1271(2) 0.0257(6) Uani 1 1 d . . . . H22A H 0.5313 0.2749 -0.1605 0.031 Uiso 1 1 calc R . . . C23A C 0.4890(2) 0.3258(2) -0.07132(19) 0.0230(6) Uani 1 1 d . . . . H23A H 0.5465 0.3246 -0.0673 0.028 Uiso 1 1 calc R . . . C24A C 0.6950(2) 0.3902(2) 0.0487(2) 0.0226(6) Uani 1 1 d . . . . C25A C 0.5335(2) 0.3781(2) 0.38247(18) 0.0220(6) Uani 1 1 d . . . . C26A C 0.4782(3) 0.3750(3) 0.4525(2) 0.0306(7) Uani 1 1 d . . . . C27A C 0.5094(3) 0.3750(3) 0.5170(2) 0.0381(9) Uani 1 1 d . . . . H27A H 0.4721 0.3726 0.5649 0.046 Uiso 1 1 calc R . . . C28A C 0.5933(3) 0.3786(2) 0.5128(2) 0.0347(8) Uani 1 1 d . . . . C29A C 0.6476(3) 0.3808(2) 0.4430(2) 0.0293(7) Uani 1 1 d . . . . H29A H 0.7054 0.3828 0.4398 0.035 Uiso 1 1 calc R . . . C30A C 0.6197(2) 0.3802(2) 0.3775(2) 0.0239(6) Uani 1 1 d . . . . C31A C 0.3861(3) 0.3722(4) 0.4588(3) 0.0502(12) Uani 1 1 d . . . . H31A H 0.3542 0.4158 0.4109 0.092(13) Uiso 1 1 calc GR . . . H31B H 0.3509 0.3864 0.5054 0.092(13) Uiso 1 1 calc GR . . . H31C H 0.3933 0.3124 0.4643 0.092(13) Uiso 1 1 calc GR . . . C32A C 0.6250(4) 0.3811(3) 0.5830(3) 0.0518(13) Uani 1 1 d . . . . H32A H 0.6818 0.3299 0.5998 0.110(15) Uiso 1 1 calc GR . . . H32B H 0.5786 0.3787 0.6270 0.110(15) Uiso 1 1 calc GR . . . H32C H 0.6351 0.4363 0.5674 0.110(15) Uiso 1 1 calc GR . . . C33A C 0.6814(3) 0.3802(3) 0.3035(2) 0.0318(7) Uani 1 1 d . . . . H33A H 0.6950 0.3260 0.2928 0.052(8) Uiso 1 1 calc GR . . . H33B H 0.7379 0.3820 0.3107 0.052(8) Uiso 1 1 calc GR . . . H33C H 0.6513 0.4325 0.2586 0.052(8) Uiso 1 1 calc GR . . . C34A C 0.3837(2) 0.2593(2) -0.18703(18) 0.0220(6) Uani 1 1 d . . . . C35A C 0.3477(2) 0.3151(2) -0.26094(19) 0.0256(6) Uani 1 1 d . . . . C36A C 0.3304(2) 0.2782(2) -0.3068(2) 0.0286(7) Uani 1 1 d . . . . H36A H 0.3055 0.3160 -0.3569 0.034 Uiso 1 1 calc R . . . C37A C 0.3482(2) 0.1882(3) -0.2818(2) 0.0275(7) Uani 1 1 d . . . . C38A C 0.3861(2) 0.1339(2) -0.2092(2) 0.0265(7) Uani 1 1 d . . . . H38A H 0.3997 0.0718 -0.1916 0.032 Uiso 1 1 calc R . . . C39A C 0.4049(2) 0.1679(2) -0.16149(19) 0.0239(6) Uani 1 1 d . . . . C40A C 0.3289(3) 0.4130(2) -0.2908(2) 0.0390(9) Uani 1 1 d . . . . H40A H 0.2842 0.4403 -0.2543 0.048(8) Uiso 1 1 calc GR . . . H40B H 0.3051 0.4412 -0.3436 0.048(8) Uiso 1 1 calc GR . . . H40C H 0.3853 0.4212 -0.2940 0.048(8) Uiso 1 1 calc GR . . . C41A C 0.3282(3) 0.1502(3) -0.3326(2) 0.0385(9) Uani 1 1 d . . . . H41A H 0.3761 0.1436 -0.3751 0.054(8) Uiso 1 1 calc GR . . . H41B H 0.2697 0.1904 -0.3559 0.054(8) Uiso 1 1 calc GR . . . H41C H 0.3259 0.0918 -0.2998 0.054(8) Uiso 1 1 calc GR . . . C42A C 0.4478(3) 0.1055(2) -0.0836(2) 0.0347(8) Uani 1 1 d . . . . H42A H 0.5119 0.0970 -0.0890 0.044(8) Uiso 1 1 calc GR . . . H42B H 0.4431 0.0480 -0.0692 0.044(8) Uiso 1 1 calc GR . . . H42C H 0.4162 0.1312 -0.0421 0.044(8) Uiso 1 1 calc GR . . . IrB Ir 0.05397(2) 0.12832(2) 0.46241(2) 0.01774(3) Uani 1 1 d . . . . F1B F 0.16592(14) -0.21082(13) 0.59053(14) 0.0339(5) Uani 1 1 d . . . . F2B F 0.18424(15) -0.18939(14) 0.46519(15) 0.0355(5) Uani 1 1 d . . . . F3B F 0.26667(13) -0.16070(14) 0.51808(15) 0.0336(5) Uani 1 1 d . . . . O1B O 0.15001(15) -0.00485(14) 0.48523(13) 0.0207(4) Uani 1 1 d . . . . N1B N -0.02788(17) 0.04683(16) 0.49123(15) 0.0180(5) Uani 1 1 d . . . . N2B N 0.07288(18) 0.14702(17) 0.34419(15) 0.0195(5) Uani 1 1 d . . . . N3B N 0.03370(18) 0.12047(18) 0.57745(16) 0.0210(5) Uani 1 1 d . . . . C1B C 0.1142(2) -0.06115(19) 0.50261(17) 0.0177(5) Uani 1 1 d . . . . C2B C 0.1502(2) 0.1778(2) 0.43264(19) 0.0202(6) Uani 1 1 d . . . . C3B C 0.1922(2) 0.1907(2) 0.4822(2) 0.0269(7) Uani 1 1 d . . . . H3B H 0.1740 0.1762 0.5371 0.032 Uiso 1 1 calc R . . . C4B C 0.2601(2) 0.2242(3) 0.4524(2) 0.0308(7) Uani 1 1 d . . . . H4B H 0.2879 0.2322 0.4873 0.037 Uiso 1 1 calc R . . . C5B C 0.2881(2) 0.2463(3) 0.3726(2) 0.0309(7) Uani 1 1 d . . . . H5B H 0.3340 0.2701 0.3528 0.037 Uiso 1 1 calc R . . . C6B C 0.2487(2) 0.2333(2) 0.3217(2) 0.0253(6) Uani 1 1 d . . . . H6B H 0.2683 0.2472 0.2671 0.030 Uiso 1 1 calc R . . . C7B C 0.1800(2) 0.1998(2) 0.35130(19) 0.0206(6) Uani 1 1 d . . . . C8B C 0.1337(2) 0.1847(2) 0.30219(19) 0.0204(6) Uani 1 1 d . . . . C9B C 0.1443(2) 0.2083(2) 0.21994(19) 0.0215(6) Uani 1 1 d . . . . H9B H 0.1866 0.2348 0.1909 0.026 Uiso 1 1 calc R . . . C10B C 0.0934(2) 0.1933(2) 0.17986(19) 0.0217(6) Uani 1 1 d . . . . C11B C 0.0351(2) 0.1501(2) 0.2255(2) 0.0265(7) Uani 1 1 d . . . . H11B H 0.0012 0.1361 0.2007 0.032 Uiso 1 1 calc R . . . C12B C 0.0271(2) 0.1282(2) 0.3061(2) 0.0235(6) Uani 1 1 d . . . . H12B H -0.0124 0.0984 0.3365 0.028 Uiso 1 1 calc R . . . C13B C -0.0303(2) 0.2535(2) 0.4494(2) 0.0240(6) Uani 1 1 d . . . . C14B C -0.0592(2) 0.3255(2) 0.3790(2) 0.0282(7) Uani 1 1 d . . . . H14B H -0.0409 0.3158 0.3298 0.034 Uiso 1 1 calc R . . . C15B C -0.1139(3) 0.4105(2) 0.3794(3) 0.0361(9) Uani 1 1 d . . . . H15B H -0.1319 0.4581 0.3307 0.043 Uiso 1 1 calc R . . . C16B C -0.1428(3) 0.4266(3) 0.4504(3) 0.0380(9) Uani 1 1 d . . . . H16B H -0.1813 0.4849 0.4502 0.046 Uiso 1 1 calc R . . . C17B C -0.1155(3) 0.3580(3) 0.5212(3) 0.0350(8) Uani 1 1 d . . . . H17B H -0.1349 0.3686 0.5699 0.042 Uiso 1 1 calc R . . . C18B C -0.0590(2) 0.2727(2) 0.5204(2) 0.0269(7) Uani 1 1 d . . . . C19B C -0.0236(2) 0.1964(2) 0.5921(2) 0.0251(6) Uani 1 1 d . . . . C20B C -0.0422(2) 0.1960(3) 0.6701(2) 0.0315(8) Uani 1 1 d . . . . H20B H -0.0825 0.2490 0.6801 0.038 Uiso 1 1 calc R . . . C21B C -0.0030(2) 0.1202(3) 0.7323(2) 0.0299(7) Uani 1 1 d . . . . C22B C 0.0561(2) 0.0431(3) 0.7156(2) 0.0288(7) Uani 1 1 d . . . . H22B H 0.0845 -0.0106 0.7571 0.035 Uiso 1 1 calc R . . . C23B C 0.0723(2) 0.0464(2) 0.6382(2) 0.0244(6) Uani 1 1 d . . . . H23B H 0.1126 -0.0059 0.6272 0.029 Uiso 1 1 calc R . . . C24B C 0.1827(2) -0.1568(2) 0.5192(2) 0.0251(6) Uani 1 1 d . . . . C25B C 0.0964(2) 0.2271(2) 0.09127(19) 0.0224(6) Uani 1 1 d . . . . C26B C 0.0206(2) 0.2994(2) 0.0533(2) 0.0248(6) Uani 1 1 d . . . . C27B C 0.0256(3) 0.3343(2) -0.0290(2) 0.0295(7) Uani 1 1 d . . . . H27B H -0.0254 0.3832 -0.0552 0.035 Uiso 1 1 calc R . . . C28B C 0.1024(3) 0.3001(3) -0.0744(2) 0.0311(8) Uani 1 1 d . . . . C29B C 0.1745(3) 0.2267(2) -0.0357(2) 0.0287(7) Uani 1 1 d . . . . H29B H 0.2264 0.2009 -0.0661 0.034 Uiso 1 1 calc R . . . C30B C 0.1732(2) 0.1894(2) 0.0470(2) 0.0248(6) Uani 1 1 d . . . . C31B C -0.0641(2) 0.3410(3) 0.0989(2) 0.0330(8) Uani 1 1 d . . . . H31D H -0.1002 0.3039 0.1179 0.048(6) Uiso 1 1 calc GR . . . H31E H -0.0999 0.4005 0.0643 0.048(6) Uiso 1 1 calc GR . . . H31F H -0.0473 0.3455 0.1443 0.048(6) Uiso 1 1 calc GR . . . C32B C 0.1065(4) 0.3435(3) -0.1636(2) 0.0464(11) Uani 1 1 d . . . . H32D H 0.1005 0.4051 -0.1777 0.070(10) Uiso 1 1 calc GR . . . H32E H 0.0569 0.3432 -0.1848 0.070(10) Uiso 1 1 calc GR . . . H32F H 0.1648 0.3105 -0.1860 0.070(10) Uiso 1 1 calc GR . . . C33B C 0.2549(3) 0.1103(3) 0.0868(2) 0.0332(8) Uani 1 1 d . . . . H33D H 0.2950 0.1312 0.0989 0.043(7) Uiso 1 1 calc GR . . . H33E H 0.2880 0.0766 0.0511 0.043(7) Uiso 1 1 calc GR . . . H33F H 0.2348 0.0719 0.1360 0.043(7) Uiso 1 1 calc GR . . . C34B C -0.0191(2) 0.1204(3) 0.8156(2) 0.0308(7) Uani 1 1 d . . . . C35B C -0.0890(3) 0.0984(3) 0.8657(3) 0.0368(9) Uani 1 1 d . . . . C36B C -0.1016(3) 0.0999(3) 0.9419(3) 0.0391(9) Uani 1 1 d . . . . H36B H -0.1489 0.0842 0.9765 0.047 Uiso 1 1 calc R . . . C37B C -0.0471(3) 0.1239(3) 0.9693(2) 0.0364(8) Uani 1 1 d . . . . C38B C 0.0227(3) 0.1434(3) 0.9193(2) 0.0382(9) Uani 1 1 d . . . . H38B H 0.0617 0.1580 0.9379 0.046 Uiso 1 1 calc R . . . C39B C 0.0382(3) 0.1426(3) 0.8421(2) 0.0354(8) Uani 1 1 d . . . . C40B C -0.1500(3) 0.0718(4) 0.8388(3) 0.0603(16) Uani 1 1 d . . . . H40D H -0.1754 0.1175 0.7888 0.085(12) Uiso 1 1 calc GR . . . H40E H -0.1995 0.0661 0.8793 0.085(12) Uiso 1 1 calc GR . . . H40F H -0.1148 0.0147 0.8308 0.085(12) Uiso 1 1 calc GR . . . C41B C -0.0640(3) 0.1274(4) 1.0520(3) 0.0481(11) Uani 1 1 d . . . . H41D H -0.1159 0.1820 1.0532 0.106(15) Uiso 1 1 calc GR . . . H41E H -0.0100 0.1269 1.0672 0.106(15) Uiso 1 1 calc GR . . . H41F H -0.0771 0.0756 1.0894 0.106(15) Uiso 1 1 calc GR . . . C42B C 0.1153(3) 0.1646(4) 0.7885(3) 0.0528(13) Uani 1 1 d . . . . H42D H 0.1487 0.1200 0.7630 0.048(6) Uiso 1 1 calc GR . . . H42E H 0.1563 0.1646 0.8199 0.048(6) Uiso 1 1 calc GR . . . H42F H 0.0910 0.2236 0.7479 0.048(6) Uiso 1 1 calc GR . . . Cl5A Cl 0.1483(3) 0.6103(2) 0.2496(2) 0.0762(9) Uani 0.5 1 d . P A 1 Cl6A Cl 0.2823(3) 0.6924(3) 0.1916(4) 0.1106(17) Uani 0.5 1 d . P A 1 Cl5B Cl 0.2274(4) 0.5999(4) 0.2776(3) 0.163(3) Uani 0.5 1 d . P A 2 Cl6B Cl 0.2855(2) 0.7005(2) 0.1256(3) 0.0911(14) Uani 0.5 1 d . P A 2 C3S C 0.2005(5) 0.6659(5) 0.1733(4) 0.0780(19) Uani 1 1 d . . . . H3SA H 0.1534 0.7223 0.1434 0.094 Uiso 0.5 1 calc R P A 1 H3SB H 0.2294 0.6307 0.1378 0.094 Uiso 0.5 1 calc R P A 1 H3SC H 0.1939 0.6291 0.1481 0.094 Uiso 0.5 1 calc R P A 2 H3SD H 0.1426 0.7179 0.1703 0.094 Uiso 0.5 1 calc R P A 2 Cl1B Cl 0.7238(4) 0.0876(3) 0.1874(4) 0.0886(16) Uani 0.5 1 d . P B 1 Cl2B Cl 0.6822(4) 0.0599(3) 0.0560(4) 0.0846(18) Uani 0.5 1 d . P B 1 Cl1A Cl 0.7444(4) 0.0496(4) 0.1646(4) 0.116(2) Uani 0.5 1 d . P B 2 Cl2A Cl 0.6538(4) 0.0934(4) 0.0241(4) 0.0792(14) Uani 0.5 1 d . P B 2 C1S C 0.6695(4) 0.1335(4) 0.0969(5) 0.0746(19) Uani 1 1 d . . . . H1SC H 0.6921 0.1821 0.0685 0.090 Uiso 0.5 1 calc R P B 2 H1SD H 0.6103 0.1577 0.1247 0.090 Uiso 0.5 1 calc R P B 2 H1SA H 0.6038 0.1653 0.1070 0.090 Uiso 0.5 1 calc R P B 1 H1SB H 0.6935 0.1781 0.0580 0.090 Uiso 0.5 1 calc R P B 1 Cl3A Cl 0.30333(13) -0.02389(10) 0.31942(9) 0.0575(4) Uani 0.85 1 d . P C 1 Cl4A Cl 0.36406(14) -0.16109(14) 0.25167(13) 0.0793(6) Uani 0.85 1 d . P C 1 C2SA C 0.3819(4) -0.1317(4) 0.3251(4) 0.0483(13) Uani 0.85 1 d . P C 1 H2SA H 0.4444 -0.1335 0.3179 0.058 Uiso 0.85 1 calc R P C 1 H2SB H 0.3747 -0.1749 0.3781 0.058 Uiso 0.85 1 calc R P C 1 Cl7A Cl 0.09657(17) 0.35859(15) 0.57880(17) 0.0859(7) Uani 0.75 1 d . P D 1 Cl8A Cl 0.14280(16) 0.45274(16) 0.4199(2) 0.0963(10) Uani 0.75 1 d . P D 1 C4SA C 0.0730(5) 0.4001(5) 0.4775(6) 0.068(2) Uani 0.75 1 d . P D 1 H4SA H 0.0818 0.3502 0.4611 0.081 Uiso 0.75 1 calc R P D 1 H4SB H 0.0090 0.4422 0.4704 0.081 Uiso 0.75 1 calc R P D 1 Cl3B Cl 0.2547(8) -0.0351(7) 0.3166(6) 0.066(2) Uiso 0.15 1 d . P E 2 Cl4B Cl 0.4175(8) -0.1638(7) 0.2700(7) 0.070(3) Uiso 0.15 1 d . P E 2 C2SB C 0.323(2) -0.142(2) 0.3351(19) 0.045(7) Uiso 0.15 1 d . P E 2 H2SC H 0.2871 -0.1748 0.3352 0.054 Uiso 0.15 1 calc R P E 2 H2SD H 0.3444 -0.1666 0.3892 0.054 Uiso 0.15 1 calc R P E 2 Cl9 Cl 0.54183(9) 0.09952(10) 0.51512(9) 0.0737(5) Uani 1 1 d . . . . Cl10 Cl 0.67811(8) 0.03080(10) 0.40147(7) 0.0603(3) Uani 1 1 d . . . . C5S C 0.6469(3) 0.0158(3) 0.5032(3) 0.0407(9) Uani 1 1 d . . . . H5SA H 0.6427 -0.0433 0.5311 0.049 Uiso 1 1 calc R . . . H5SB H 0.6942 0.0174 0.5273 0.049 Uiso 1 1 calc R . . . Cl7B Cl 0.1171(5) 0.4321(6) 0.4790(6) 0.090(3) Uani 0.25 1 d . P F 2 Cl8B Cl 0.0200(5) 0.5403(3) 0.3308(3) 0.0693(16) Uani 0.25 1 d . P F 2 C4SB C 0.0772(11) 0.4348(10) 0.3988(9) 0.032(3) Uiso 0.25 1 d . P F 2 H4SC H 0.0357 0.4025 0.4191 0.039 Uiso 0.25 1 calc R P F 2 H4SD H 0.1294 0.4016 0.3697 0.039 Uiso 0.25 1 calc R P F 2 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 IrA 0.01830(5) 0.01615(5) 0.01587(5) -0.00506(4) -0.00245(4) -0.00820(4) F1A 0.0302(10) 0.0311(10) 0.0350(11) -0.0087(9) -0.0131(9) -0.0140(9) F2A 0.0231(10) 0.0439(13) 0.0408(13) -0.0166(10) 0.0062(9) -0.0131(9) F3A 0.0281(11) 0.0210(10) 0.0575(15) 0.0062(9) -0.0224(10) -0.0092(8) O1A 0.0188(10) 0.0179(10) 0.0215(10) -0.0061(8) -0.0039(8) -0.0071(8) N1A 0.0174(11) 0.0206(12) 0.0155(11) -0.0043(9) -0.0037(9) -0.0093(9) N2A 0.0209(12) 0.0172(11) 0.0173(11) -0.0054(9) -0.0022(9) -0.0088(9) N3A 0.0197(12) 0.0203(12) 0.0188(12) -0.0063(9) -0.0031(9) -0.0108(10) C1A 0.0169(13) 0.0215(13) 0.0157(12) -0.0058(10) -0.0022(10) -0.0083(11) C2A 0.0194(13) 0.0172(13) 0.0200(13) -0.0065(11) -0.0003(10) -0.0082(11) C3A 0.0291(16) 0.0192(14) 0.0243(15) -0.0068(12) -0.0054(12) -0.0107(12) C4A 0.0300(17) 0.0193(14) 0.0339(18) -0.0084(13) -0.0063(14) -0.0113(13) C5A 0.0344(18) 0.0199(15) 0.0282(17) -0.0022(12) -0.0078(14) -0.0121(13) C6A 0.0304(16) 0.0206(14) 0.0228(15) -0.0039(12) -0.0069(12) -0.0111(13) C7A 0.0190(13) 0.0180(13) 0.0219(14) -0.0063(11) -0.0033(11) -0.0076(11) C8A 0.0178(13) 0.0179(13) 0.0194(13) -0.0067(11) -0.0006(10) -0.0075(11) C9A 0.0241(15) 0.0186(13) 0.0186(13) -0.0042(11) -0.0045(11) -0.0087(11) C10A 0.0245(15) 0.0236(14) 0.0179(13) -0.0063(11) -0.0029(11) -0.0119(12) C11A 0.0323(17) 0.0210(14) 0.0219(15) -0.0080(12) -0.0038(12) -0.0112(13) C12A 0.0276(15) 0.0174(13) 0.0212(14) -0.0063(11) -0.0054(12) -0.0088(12) C13A 0.0204(13) 0.0154(12) 0.0188(13) -0.0039(10) -0.0039(10) -0.0075(11) C14A 0.0270(16) 0.0234(15) 0.0207(14) -0.0087(12) -0.0012(12) -0.0109(12) C15A 0.0254(16) 0.0256(16) 0.0280(16) -0.0113(13) 0.0049(13) -0.0106(13) C16A 0.0198(15) 0.0266(16) 0.0352(18) -0.0123(14) 0.0008(13) -0.0092(13) C17A 0.0232(15) 0.0221(14) 0.0293(16) -0.0074(12) -0.0034(12) -0.0124(12) C18A 0.0203(14) 0.0171(13) 0.0228(14) -0.0057(11) -0.0021(11) -0.0082(11) C19A 0.0228(14) 0.0176(13) 0.0184(13) -0.0048(10) -0.0037(11) -0.0095(11) C20A 0.0253(15) 0.0208(14) 0.0224(14) -0.0061(11) -0.0063(12) -0.0100(12) C21A 0.0293(16) 0.0218(14) 0.0178(13) -0.0050(11) -0.0060(12) -0.0109(12) C22A 0.0248(16) 0.0324(17) 0.0248(16) -0.0144(13) 0.0010(12) -0.0124(13) C23A 0.0223(15) 0.0304(16) 0.0205(14) -0.0103(12) 0.0006(11) -0.0134(13) C24A 0.0210(14) 0.0187(14) 0.0274(16) -0.0044(12) -0.0062(12) -0.0082(11) C25A 0.0285(16) 0.0210(14) 0.0185(14) -0.0065(11) -0.0060(12) -0.0096(12) C26A 0.0345(19) 0.039(2) 0.0239(16) -0.0135(15) -0.0018(14) -0.0172(16) C27A 0.051(2) 0.046(2) 0.0233(17) -0.0158(16) -0.0031(16) -0.0193(19) C28A 0.049(2) 0.0275(17) 0.0322(19) -0.0114(15) -0.0193(17) -0.0092(16) C29A 0.0347(18) 0.0235(15) 0.0341(18) -0.0081(14) -0.0150(15) -0.0104(14) C30A 0.0284(16) 0.0167(13) 0.0266(16) -0.0039(12) -0.0090(13) -0.0083(12) C31A 0.047(3) 0.087(4) 0.035(2) -0.030(2) 0.0105(19) -0.040(3) C32A 0.073(3) 0.052(3) 0.042(2) -0.020(2) -0.027(2) -0.020(2) C33A 0.0297(18) 0.0336(19) 0.0329(19) -0.0115(15) -0.0036(14) -0.0120(15) C34A 0.0268(15) 0.0239(15) 0.0189(14) -0.0082(11) -0.0052(11) -0.0103(12) C35A 0.0291(16) 0.0250(15) 0.0194(14) -0.0060(12) -0.0049(12) -0.0074(13) C36A 0.0291(17) 0.0360(18) 0.0173(14) -0.0082(13) -0.0066(12) -0.0079(14) C37A 0.0267(16) 0.0406(19) 0.0229(15) -0.0184(14) -0.0007(12) -0.0131(14) C38A 0.0318(17) 0.0276(16) 0.0260(16) -0.0119(13) -0.0032(13) -0.0135(14) C39A 0.0295(16) 0.0256(15) 0.0188(14) -0.0067(12) -0.0052(12) -0.0115(13) C40A 0.053(3) 0.0236(17) 0.0298(19) -0.0028(14) -0.0129(17) -0.0062(17) C41A 0.039(2) 0.060(3) 0.033(2) -0.0303(19) 0.0006(16) -0.0208(19) C42A 0.053(2) 0.0272(17) 0.0246(17) -0.0017(14) -0.0149(16) -0.0161(17) IrB 0.02060(6) 0.01538(5) 0.01957(6) -0.00661(4) -0.00216(4) -0.00800(4) F1B 0.0312(11) 0.0193(9) 0.0405(12) 0.0028(8) -0.0102(9) -0.0086(8) F2B 0.0325(11) 0.0281(11) 0.0510(14) -0.0254(10) -0.0030(10) -0.0052(9) F3B 0.0183(9) 0.0233(10) 0.0548(14) -0.0101(9) -0.0061(9) -0.0054(8) O1B 0.0212(10) 0.0204(10) 0.0227(11) -0.0083(8) -0.0018(8) -0.0090(8) N1B 0.0218(12) 0.0147(11) 0.0180(11) -0.0049(9) -0.0027(9) -0.0073(9) N2B 0.0231(12) 0.0179(11) 0.0193(12) -0.0036(9) -0.0040(10) -0.0108(10) N3B 0.0230(13) 0.0215(12) 0.0224(13) -0.0103(10) -0.0012(10) -0.0096(10) C1B 0.0202(13) 0.0175(13) 0.0163(13) -0.0072(10) -0.0033(10) -0.0056(11) C2B 0.0215(14) 0.0184(13) 0.0232(14) -0.0083(11) -0.0021(11) -0.0085(11) C3B 0.0285(17) 0.0348(18) 0.0260(16) -0.0151(14) 0.0002(13) -0.0164(14) C4B 0.0301(17) 0.043(2) 0.0331(18) -0.0206(16) -0.0008(14) -0.0202(16) C5B 0.0296(17) 0.040(2) 0.0353(19) -0.0178(16) 0.0008(14) -0.0213(16) C6B 0.0251(16) 0.0291(16) 0.0251(16) -0.0088(13) -0.0007(12) -0.0143(13) C7B 0.0207(14) 0.0165(13) 0.0263(15) -0.0064(11) -0.0051(11) -0.0078(11) C8B 0.0208(14) 0.0168(13) 0.0244(15) -0.0067(11) -0.0050(11) -0.0066(11) C9B 0.0232(14) 0.0194(14) 0.0221(14) -0.0045(11) -0.0035(11) -0.0098(12) C10B 0.0248(15) 0.0211(14) 0.0208(14) -0.0063(11) -0.0025(11) -0.0104(12) C11B 0.0323(17) 0.0310(17) 0.0248(16) -0.0093(13) -0.0035(13) -0.0192(14) C12B 0.0287(16) 0.0239(15) 0.0244(15) -0.0068(12) -0.0030(12) -0.0166(13) C13B 0.0243(15) 0.0210(14) 0.0312(17) -0.0100(12) -0.0039(13) -0.0108(12) C14B 0.0257(16) 0.0209(15) 0.0361(19) -0.0075(13) -0.0026(14) -0.0089(13) C15B 0.0320(19) 0.0216(16) 0.052(2) -0.0076(16) -0.0075(17) -0.0105(14) C16B 0.0313(19) 0.0235(17) 0.065(3) -0.0200(18) -0.0131(18) -0.0059(14) C17B 0.0297(18) 0.0308(18) 0.053(2) -0.0270(18) -0.0094(17) -0.0041(15) C18B 0.0241(15) 0.0240(15) 0.0393(19) -0.0173(14) -0.0058(14) -0.0076(13) C19B 0.0220(15) 0.0248(15) 0.0341(18) -0.0175(14) -0.0022(13) -0.0070(12) C20B 0.0287(17) 0.0352(19) 0.040(2) -0.0259(16) -0.0012(15) -0.0088(15) C21B 0.0300(17) 0.040(2) 0.0296(17) -0.0196(15) 0.0015(14) -0.0162(15) C22B 0.0327(18) 0.0334(18) 0.0243(16) -0.0138(14) 0.0000(13) -0.0137(15) C23B 0.0269(16) 0.0223(15) 0.0253(16) -0.0104(12) -0.0008(12) -0.0089(12) C24B 0.0203(14) 0.0181(14) 0.0365(18) -0.0097(13) -0.0048(13) -0.0053(12) C25B 0.0275(15) 0.0245(15) 0.0197(14) -0.0045(11) -0.0038(12) -0.0157(13) C26B 0.0263(16) 0.0271(16) 0.0240(15) -0.0044(12) -0.0053(12) -0.0150(13) C27B 0.0330(18) 0.0317(17) 0.0261(16) -0.0028(14) -0.0088(14) -0.0179(15) C28B 0.046(2) 0.0336(18) 0.0230(16) -0.0054(14) -0.0046(15) -0.0261(17) C29B 0.0347(18) 0.0333(18) 0.0265(16) -0.0121(14) 0.0018(14) -0.0206(15) C30B 0.0285(16) 0.0282(16) 0.0244(15) -0.0088(13) -0.0022(12) -0.0167(13) C31B 0.0261(17) 0.0360(19) 0.0342(19) -0.0063(15) -0.0047(14) -0.0135(15) C32B 0.067(3) 0.049(3) 0.0257(19) -0.0078(18) -0.0052(19) -0.028(2) C33B 0.0300(18) 0.0362(19) 0.0347(19) -0.0140(16) -0.0028(15) -0.0117(15) C34B 0.0298(17) 0.042(2) 0.0310(18) -0.0233(16) 0.0015(14) -0.0149(16) C35B 0.0290(18) 0.056(2) 0.041(2) -0.0308(19) 0.0037(16) -0.0199(18) C36B 0.036(2) 0.057(3) 0.040(2) -0.030(2) 0.0095(17) -0.0249(19) C37B 0.042(2) 0.047(2) 0.0297(19) -0.0215(17) -0.0010(16) -0.0183(18) C38B 0.040(2) 0.055(3) 0.038(2) -0.0275(19) -0.0024(17) -0.0242(19) C39B 0.038(2) 0.050(2) 0.034(2) -0.0246(18) 0.0045(16) -0.0250(18) C40B 0.045(3) 0.110(5) 0.069(3) -0.065(3) 0.018(2) -0.048(3) C41B 0.059(3) 0.068(3) 0.031(2) -0.029(2) 0.0034(19) -0.028(2) C42B 0.055(3) 0.087(4) 0.053(3) -0.044(3) 0.020(2) -0.052(3) Cl5A 0.119(3) 0.0536(16) 0.0673(19) -0.0344(14) 0.0148(19) -0.0408(18) Cl6A 0.058(2) 0.067(2) 0.187(5) -0.036(3) -0.030(3) -0.0029(17) Cl5B 0.107(4) 0.190(6) 0.066(2) -0.044(3) 0.017(2) 0.044(4) Cl6B 0.0383(15) 0.0562(18) 0.163(4) -0.039(3) 0.015(2) -0.0134(13) C3S 0.089(5) 0.077(4) 0.069(4) -0.044(3) 0.031(4) -0.034(4) Cl1B 0.059(2) 0.079(3) 0.091(3) -0.004(2) 0.013(2) -0.026(2) Cl2B 0.084(4) 0.069(3) 0.119(5) -0.058(3) 0.057(3) -0.053(3) Cl1A 0.064(3) 0.098(4) 0.121(5) 0.028(3) -0.019(3) -0.027(3) Cl2A 0.065(3) 0.079(4) 0.101(4) -0.041(3) 0.016(2) -0.034(2) C1S 0.041(3) 0.049(3) 0.130(6) -0.040(4) -0.008(3) -0.004(2) Cl3A 0.0863(12) 0.0405(7) 0.0414(7) -0.0148(6) -0.0043(7) -0.0197(7) Cl4A 0.0768(12) 0.0908(13) 0.0846(13) -0.0676(12) -0.0097(10) -0.0083(10) C2SA 0.040(3) 0.058(3) 0.047(3) -0.027(3) -0.004(2) -0.011(3) Cl7A 0.0878(16) 0.0566(12) 0.112(2) -0.0358(12) -0.0292(14) -0.0095(11) Cl8A 0.0661(14) 0.0600(13) 0.185(3) -0.0699(18) 0.0262(17) -0.0348(11) C4SA 0.044(4) 0.042(4) 0.123(8) -0.030(4) -0.012(4) -0.017(3) Cl9 0.0451(7) 0.0694(9) 0.0533(7) -0.0095(6) 0.0054(6) 0.0102(6) Cl10 0.0419(6) 0.0843(9) 0.0436(6) -0.0280(6) -0.0118(5) -0.0046(6) C5S 0.031(2) 0.040(2) 0.042(2) -0.0105(18) -0.0056(17) -0.0071(17) Cl7B 0.072(4) 0.107(6) 0.122(6) -0.090(6) -0.038(4) 0.000(4) Cl8B 0.099(5) 0.041(3) 0.053(3) 0.011(2) -0.032(3) -0.026(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 -1.00 -1.00 0.0920 0.00 1.00 1.00 0.1070 1.00 -1.00 0.00 0.1100 -1.00 1.00 0.00 0.1030 1.00 1.00 0.00 0.1460 -1.00 -1.00 0.00 0.1410 -1.00 0.00 1.00 0.1290 1.00 0.00 1.00 0.1420 -1.00 0.00 -1.00 0.0990 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 O1A IrA N1A 73.72(8) . . N2A IrA O1A 82.61(9) . . N2A IrA N1A 91.89(9) . . N3A IrA O1A 97.44(9) . . N3A IrA N1A 94.12(9) . . N3A IrA N2A 173.76(10) . . C2A IrA O1A 92.95(10) . . C2A IrA N1A 165.55(10) . . C2A IrA N2A 80.63(11) . . C2A IrA N3A 93.13(11) . . C2A IrA C13A 84.80(12) . . C13A IrA O1A 176.97(10) . . C13A IrA N1A 108.71(10) . . C13A IrA N2A 99.00(11) . . C13A IrA N3A 80.68(11) . . C1A O1A IrA 111.52(18) . . N1A N1A IrA 112.0(2) 2_665 . C1A N1A IrA 135.6(2) 2_665 . C1A N1A N1A 110.6(3) 2_665 2_665 C8A N2A IrA 114.91(19) . . C12A N2A IrA 125.7(2) . . C12A N2A C8A 118.9(3) . . C19A N3A IrA 116.3(2) . . C23A N3A IrA 123.6(2) . . C23A N3A C19A 119.7(3) . . O1A C1A N1A 128.1(3) . 2_665 O1A C1A C24A 113.9(3) . . N1A C1A C24A 117.9(3) 2_665 . C3A C2A IrA 128.7(2) . . C3A C2A C7A 117.1(3) . . C7A C2A IrA 114.1(2) . . C4A C3A C2A 120.9(3) . . C5A C4A C3A 120.6(3) . . C6A C5A C4A 119.9(3) . . C5A C6A C7A 119.6(3) . . C2A C7A C8A 115.4(3) . . C6A C7A C2A 121.8(3) . . C6A C7A C8A 122.8(3) . . N2A C8A C7A 113.2(3) . . N2A C8A C9A 120.5(3) . . C9A C8A C7A 126.3(3) . . C10A C9A C8A 120.7(3) . . C9A C10A C11A 117.8(3) . . C9A C10A C25A 122.2(3) . . C11A C10A C25A 120.1(3) . . C12A C11A C10A 119.4(3) . . N2A C12A C11A 122.5(3) . . C14A C13A IrA 128.1(2) . . C14A C13A C18A 117.2(3) . . C18A C13A IrA 114.5(2) . . C15A C14A C13A 121.2(3) . . C16A C15A C14A 120.4(3) . . C17A C16A C15A 120.0(3) . . C16A C17A C18A 119.5(3) . . C13A C18A C19A 114.8(3) . . C17A C18A C13A 121.7(3) . . C17A C18A C19A 123.4(3) . . N3A C19A C18A 113.5(3) . . N3A C19A C20A 119.8(3) . . C20A C19A C18A 126.6(3) . . C21A C20A C19A 121.2(3) . . C20A C21A C22A 117.7(3) . . C20A C21A C34A 120.1(3) . . C22A C21A C34A 122.2(3) . . C23A C22A C21A 119.3(3) . . N3A C23A C22A 122.3(3) . . F1A C24A F2A 107.3(3) . . F1A C24A F3A 107.0(3) . . F1A C24A C1A 112.5(3) . . F2A C24A C1A 112.4(3) . . F3A C24A F2A 107.1(3) . . F3A C24A C1A 110.2(2) . . C26A C25A C10A 120.8(3) . . C26A C25A C30A 120.4(3) . . C30A C25A C10A 118.8(3) . . C25A C26A C27A 119.0(3) . . C25A C26A C31A 121.0(3) . . C27A C26A C31A 120.1(4) . . C28A C27A C26A 121.5(4) . . C27A C28A C29A 118.7(3) . . C27A C28A C32A 120.8(4) . . C29A C28A C32A 120.5(4) . . C28A C29A C30A 121.8(3) . . C25A C30A C33A 120.9(3) . . C29A C30A C25A 118.6(3) . . C29A C30A C33A 120.4(3) . . C35A C34A C21A 120.1(3) . . C39A C34A C21A 119.7(3) . . C39A C34A C35A 120.2(3) . . C34A C35A C40A 120.6(3) . . C36A C35A C34A 118.9(3) . . C36A C35A C40A 120.5(3) . . C37A C36A C35A 122.1(3) . . C36A C37A C38A 118.0(3) . . C36A C37A C41A 120.9(3) . . C38A C37A C41A 121.1(3) . . C37A C38A C39A 121.8(3) . . C34A C39A C42A 121.4(3) . . C38A C39A C34A 119.0(3) . . C38A C39A C42A 119.7(3) . . O1B IrB N1B 74.80(9) . . N2B IrB O1B 88.91(9) . . N2B IrB N1B 95.13(10) . . N3B IrB O1B 95.03(10) . . N3B IrB N1B 88.51(10) . . N3B IrB N2B 175.23(10) . . C2B IrB O1B 92.94(10) . . C2B IrB N1B 167.17(11) . . C2B IrB N2B 80.60(11) . . C2B IrB N3B 96.48(12) . . C2B IrB C13B 84.09(13) . . C13B IrB O1B 174.20(11) . . C13B IrB N1B 108.44(11) . . C13B IrB N2B 95.51(12) . . C13B IrB N3B 80.39(13) . . C1B O1B IrB 113.62(19) . . N1B N1B IrB 112.3(2) 2_556 . C1B N1B IrB 136.5(2) 2_556 . C1B N1B N1B 111.2(3) 2_556 2_556 C8B N2B IrB 116.1(2) . . C12B N2B IrB 124.5(2) . . C12B N2B C8B 119.4(3) . . C19B N3B IrB 116.3(2) . . C23B N3B IrB 124.3(2) . . C23B N3B C19B 119.3(3) . . O1B C1B N1B 128.1(3) . 2_556 O1B C1B C24B 113.9(3) . . N1B C1B C24B 118.0(3) 2_556 . C3B C2B IrB 127.9(2) . . C3B C2B C7B 117.4(3) . . C7B C2B IrB 114.7(2) . . C4B C3B C2B 121.0(3) . . C5B C4B C3B 121.0(3) . . C4B C5B C6B 119.7(3) . . C5B C6B C7B 119.6(3) . . C2B C7B C8B 115.0(3) . . C6B C7B C2B 121.4(3) . . C6B C7B C8B 123.6(3) . . N2B C8B C7B 113.5(3) . . N2B C8B C9B 120.0(3) . . C9B C8B C7B 126.4(3) . . C10B C9B C8B 120.8(3) . . C9B C10B C11B 117.5(3) . . C9B C10B C25B 121.4(3) . . C11B C10B C25B 121.1(3) . . C12B C11B C10B 119.6(3) . . N2B C12B C11B 122.6(3) . . C14B C13B IrB 128.4(3) . . C14B C13B C18B 116.4(3) . . C18B C13B IrB 115.1(2) . . C15B C14B C13B 121.6(4) . . C14B C15B C16B 120.6(4) . . C17B C16B C15B 119.9(3) . . C16B C17B C18B 119.3(4) . . C13B C18B C19B 114.4(3) . . C17B C18B C13B 122.2(3) . . C17B C18B C19B 123.4(3) . . N3B C19B C18B 113.7(3) . . N3B C19B C20B 119.8(3) . . C20B C19B C18B 126.5(3) . . C21B C20B C19B 120.9(3) . . C20B C21B C22B 118.1(3) . . C20B C21B C34B 121.2(3) . . C22B C21B C34B 120.6(3) . . C23B C22B C21B 119.0(3) . . N3B C23B C22B 122.8(3) . . F1B C24B F3B 106.9(3) . . F1B C24B C1B 111.9(3) . . F2B C24B F1B 108.4(3) . . F2B C24B F3B 107.0(3) . . F2B C24B C1B 112.2(3) . . F3B C24B C1B 110.1(3) . . C26B C25B C10B 118.4(3) . . C30B C25B C10B 121.1(3) . . C30B C25B C26B 120.5(3) . . C25B C26B C31B 122.1(3) . . C27B C26B C25B 118.3(3) . . C27B C26B C31B 119.6(3) . . C26B C27B C28B 122.3(3) . . C27B C28B C32B 120.3(4) . . C29B C28B C27B 118.2(3) . . C29B C28B C32B 121.5(4) . . C28B C29B C30B 121.7(3) . . C25B C30B C29B 118.9(3) . . C25B C30B C33B 121.4(3) . . C29B C30B C33B 119.8(3) . . C35B C34B C21B 120.9(3) . . C35B C34B C39B 120.6(3) . . C39B C34B C21B 118.5(3) . . C34B C35B C40B 121.2(4) . . C36B C35B C34B 118.9(3) . . C36B C35B C40B 119.8(4) . . C35B C36B C37B 121.8(4) . . C36B C37B C41B 120.7(4) . . C38B C37B C36B 118.1(4) . . C38B C37B C41B 121.2(4) . . C37B C38B C39B 122.2(3) . . C34B C39B C42B 120.7(3) . . C38B C39B C34B 118.4(4) . . C38B C39B C42B 120.9(3) . . Cl5A C3S Cl6A 118.7(5) . . Cl6B C3S Cl5B 108.4(5) . . Cl2B C1S Cl1B 115.5(4) . . Cl1A C1S Cl2A 111.1(4) . . Cl4A C2SA Cl3A 110.0(3) . . Cl8A C4SA Cl7A 110.0(5) . . Cl3B C2SB Cl4B 116.4(19) . . Cl9 C5S Cl10 110.9(2) . . Cl7B C4SB Cl8B 116.9(9) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 IrA O1A 2.160(2) . IrA N1A 2.215(2) . IrA N2A 2.042(2) . IrA N3A 2.027(2) . IrA C2A 1.991(3) . IrA C13A 1.993(3) . F1A C24A 1.330(4) . F2A C24A 1.334(4) . F3A C24A 1.330(4) . O1A C1A 1.268(4) . N1A N1A 1.443(5) 2_665 N1A C1A 1.310(4) 2_665 N2A C8A 1.371(4) . N2A C12A 1.345(4) . N3A C19A 1.361(4) . N3A C23A 1.344(4) . C1A N1A 1.310(4) 2_665 C1A C24A 1.531(4) . C2A C3A 1.407(4) . C2A C7A 1.408(4) . C3A C4A 1.397(5) . C4A C5A 1.389(5) . C5A C6A 1.384(5) . C6A C7A 1.402(4) . C7A C8A 1.466(4) . C8A C9A 1.389(4) . C9A C10A 1.387(4) . C10A C11A 1.399(4) . C10A C25A 1.490(4) . C11A C12A 1.382(4) . C13A C14A 1.399(4) . C13A C18A 1.416(4) . C14A C15A 1.394(5) . C15A C16A 1.391(5) . C16A C17A 1.386(5) . C17A C18A 1.396(4) . C18A C19A 1.465(4) . C19A C20A 1.392(4) . C20A C21A 1.389(5) . C21A C22A 1.396(5) . C21A C34A 1.496(4) . C22A C23A 1.385(4) . C25A C26A 1.396(5) . C25A C30A 1.408(5) . C26A C27A 1.397(5) . C26A C31A 1.506(6) . C27A C28A 1.384(6) . C28A C29A 1.388(6) . C28A C32A 1.522(5) . C29A C30A 1.389(5) . C30A C33A 1.504(5) . C34A C35A 1.400(4) . C34A C39A 1.396(5) . C35A C36A 1.393(5) . C35A C40A 1.505(5) . C36A C37A 1.384(5) . C37A C38A 1.388(5) . C37A C41A 1.509(5) . C38A C39A 1.395(4) . C39A C42A 1.512(5) . IrB O1B 2.128(2) . IrB N1B 2.213(2) . IrB N2B 2.041(3) . IrB N3B 2.030(3) . IrB C2B 1.992(3) . IrB C13B 1.994(3) . F1B C24B 1.332(4) . F2B C24B 1.330(4) . F3B C24B 1.342(4) . O1B C1B 1.268(4) . N1B N1B 1.447(5) 2_556 N1B C1B 1.309(4) 2_556 N2B C8B 1.359(4) . N2B C12B 1.344(4) . N3B C19B 1.362(4) . N3B C23B 1.342(4) . C1B N1B 1.309(4) 2_556 C1B C24B 1.526(4) . C2B C3B 1.395(4) . C2B C7B 1.416(4) . C3B C4B 1.388(5) . C4B C5B 1.385(5) . C5B C6B 1.386(5) . C6B C7B 1.397(4) . C7B C8B 1.465(4) . C8B C9B 1.393(4) . C9B C10B 1.391(4) . C10B C11B 1.400(4) . C10B C25B 1.495(4) . C11B C12B 1.368(5) . C13B C14B 1.401(5) . C13B C18B 1.413(5) . C14B C15B 1.385(5) . C15B C16B 1.389(6) . C16B C17B 1.379(6) . C17B C18B 1.397(5) . C18B C19B 1.465(5) . C19B C20B 1.401(5) . C20B C21B 1.373(6) . C21B C22B 1.404(5) . C21B C34B 1.500(5) . C22B C23B 1.373(5) . C25B C26B 1.404(5) . C25B C30B 1.396(5) . C26B C27B 1.388(5) . C26B C31B 1.506(5) . C27B C28B 1.389(6) . C28B C29B 1.379(5) . C28B C32B 1.510(5) . C29B C30B 1.397(5) . C30B C33B 1.514(5) . C34B C35B 1.391(5) . C34B C39B 1.398(5) . C35B C36B 1.385(5) . C35B C40B 1.511(5) . C36B C37B 1.390(5) . C37B C38B 1.374(6) . C37B C41B 1.511(5) . C38B C39B 1.394(5) . C39B C42B 1.507(6) . Cl5A C3S 1.660(7) . Cl6A C3S 1.731(9) . Cl5B C3S 1.842(8) . Cl6B C3S 1.683(7) . Cl1B C1S 1.786(10) . Cl2B C1S 1.676(8) . Cl1A C1S 1.702(8) . Cl2A C1S 1.860(10) . Cl3A C2SA 1.762(6) . Cl4A C2SA 1.752(6) . Cl7A C4SA 1.777(10) . Cl8A C4SA 1.698(8) . Cl3B C2SB 1.67(3) . Cl4B C2SB 1.73(3) . Cl9 C5S 1.761(4) . Cl10 C5S 1.772(5) . Cl7B C4SB 1.723(16) . Cl8B C4SB 1.756(16) .