#------------------------------------------------------------------------------ #$Date: 2021-04-28 04:53:10 +0300 (Wed, 28 Apr 2021) $ #$Revision: 264609 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/72/7707207.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_7707207 loop_ _publ_author_name 'Tatarin, Sergei V.' 'Kalle, Paulina' 'Taydakov, Ilya V.' 'Varaksina, Evgenia' 'Korshunov, Vladislav M.' 'Bezzubov, Stanislav' _publ_section_title ; Sterically hindered phenanthroimidazole ligands drive structural flexibility and facile ligand exchange in cyclometalated iridium(III) complexes ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT00820J _journal_year 2021 _chemical_formula_moiety 'C116 H84 Cl2 Ir2 N8 O8' _chemical_formula_sum 'C116 H84 Cl2 Ir2 N8 O8' _chemical_formula_weight 2173.21 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _audit_creation_date 2020-12-22 _audit_creation_method ; Olex2 1.3 (compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003) ; _audit_update_record ; 2020-12-23 deposited with the CCDC. 2021-04-27 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 115.060(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 24.510(3) _cell_length_b 22.242(3) _cell_length_c 22.805(3) _cell_measurement_reflns_used 9947 _cell_measurement_temperature 150.15 _cell_measurement_theta_max 29.97 _cell_measurement_theta_min 2.48 _cell_volume 11262(3) _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_collection 'APEX3 v.2017.3_0 (Bruker AXS, 2017)' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve 1.3 (Bourhis et al., 2015)' _diffrn_ambient_temperature 150 _diffrn_detector 'CCD area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'Bruker SMART CCD area detector' _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART APEX II' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0634 _diffrn_reflns_av_unetI/netI 0.0632 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 48294 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.000 _diffrn_reflns_theta_min 1.972 _diffrn_source_current 30.0 _diffrn_source_power 1.5 _diffrn_source_target Mo _diffrn_source_voltage 50.0 _exptl_absorpt_coefficient_mu 2.463 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.4979 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1225 before and 0.0547 after correction. The Ratio of minimum to maximum transmission is 0.6673. The \l/2 correction factor is 0.00150. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.282 _exptl_crystal_description plate _exptl_crystal_F_000 4352 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: CH2Cl2' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.04 _refine_diff_density_max 1.957 _refine_diff_density_min -2.436 _refine_diff_density_rms 0.138 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 627 _refine_ls_number_reflns 12241 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.070 _refine_ls_R_factor_all 0.0751 _refine_ls_R_factor_gt 0.0502 _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^)+(0.0369P)^2^+118.8870P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1117 _refine_ls_wR_factor_ref 0.1197 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8889 _reflns_number_total 12241 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt00820j2.cif _cod_data_source_block z _cod_original_cell_volume 11262(2) _cod_database_code 7707207 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.908 _shelx_estimated_absorpt_t_min 0.525 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints C47 \\sim C46: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.005 within 2A 3. Others Fixed Sof: C58(0.6) H58A(0.6) H58B(0.6) H58C(0.6) C60(0.4) H60A(0.4) H60B(0.4) H60C(0.4) 4.a Aromatic/amide H refined with riding coordinates: C2(H2), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24), C25(H25), C29(H29), C32(H32), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C43(H43), C44(H44), C45(H45), C46(H46), C49(H49), C50(H50), C51(H51), C52(H52) 4.b Idealised Me refined as rotating group: C56(H56A,H56B,H56C), C55(H55A,H55B,H55C), C57(H57A,H57B,H57C), C58(H58A,H58B, H58C), C60(H60A,H60B,H60C) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL z_a.res in C2/c z.res created by SHELXL-2018/3 at 17:02:40 on 22-Dec-2020 REM Old TITL z in C2/c REM SHELXT solution in C2/c REM R1 0.161, Rweak 0.006, Alpha 0.067, Orientation as input REM Formula found by SHELXT: C57 N6 O9 Cl Ir REM ABIN CELL 0.71073 24.5102 22.2424 22.8052 90 115.06 90 ZERR 4 0.0028 0.0025 0.0026 0 0.002 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Cl Ir N O UNIT 464 336 8 8 32 32 SIMU 0.005 0.005 2 C47 C46 L.S. 8 PLAN 5 SIZE 0.3 0.27 0.04 TEMP -123 CONF LIST 6 MORE -1 BOND $H ABIN fmap 2 acta OMIT -2 54 OMIT -1 1 1 OMIT 1 1 0 OMIT 1 1 1 OMIT 1 1 2 OMIT -2 2 1 OMIT -1 1 2 OMIT 0 2 1 OMIT 2 2 0 OMIT 3 1 2 OMIT -4 2 6 REM REM REM WGHT 0.036900 118.887009 FVAR 0.02102 IR1 4 0.584889 0.593146 0.315970 11.00000 0.01863 0.03562 = 0.01373 0.00265 0.00733 0.00105 CL1 3 0.478180 0.592005 0.305787 11.00000 0.02011 0.04208 = 0.01300 -0.00139 0.00804 -0.00231 N1 5 0.597700 0.683032 0.301672 11.00000 0.01914 0.03111 = 0.01316 -0.00273 0.00645 0.00287 N2 5 0.643483 0.747892 0.263177 11.00000 0.02197 0.03542 = 0.01901 0.00222 0.00919 -0.00078 N3 5 0.587539 0.503545 0.343383 11.00000 0.02517 0.04169 = 0.00699 -0.00306 0.00621 0.00344 N4 5 0.594668 0.441362 0.423301 11.00000 0.03082 0.03898 = 0.02335 0.00337 0.01642 0.00065 O1 6 0.791504 0.492516 0.320676 11.00000 0.04824 0.04618 = 0.06218 0.01134 0.03435 0.02044 O2 6 0.813243 0.583835 0.265306 11.00000 0.03424 0.05856 = 0.07216 0.00578 0.03785 0.00843 O3 6 0.705635 0.702520 0.550417 11.00000 0.07203 0.05421 = 0.03184 0.00576 -0.01195 -0.02481 O4 6 0.700488 0.606220 0.615840 11.00000 0.04982 0.06612 = 0.01861 -0.00135 0.00688 -0.01473 C1 1 0.662166 0.588064 0.307393 11.00000 0.02033 0.03602 = 0.01706 -0.00111 0.01061 0.00088 C2 1 0.701356 0.537994 0.321937 11.00000 0.03468 0.03917 = 0.02675 0.00533 0.01555 0.00136 AFIX 43 H2 2 0.693273 0.503354 0.341322 11.00000 -1.20000 AFIX 0 C3 1 0.751082 0.538749 0.308390 11.00000 0.03007 0.04147 = 0.03346 0.00382 0.01435 0.01407 C4 1 0.763270 0.589526 0.278069 11.00000 0.02214 0.04771 = 0.03720 0.00125 0.01596 0.00021 C5 1 0.726633 0.638768 0.264965 11.00000 0.02640 0.04222 = 0.02362 -0.00246 0.01158 -0.00213 AFIX 43 H5 2 0.734960 0.673270 0.245577 11.00000 -1.20000 AFIX 0 C6 1 0.676647 0.638531 0.280086 11.00000 0.01479 0.04826 = 0.01598 -0.00244 0.00450 -0.00071 C7 1 0.639108 0.689297 0.277635 11.00000 0.01983 0.03238 = 0.01540 0.00083 0.00537 -0.00347 C8 1 0.683111 0.768364 0.236243 11.00000 0.02231 0.03225 = 0.02595 0.00351 0.00784 -0.00077 C9 1 0.666683 0.759735 0.170439 11.00000 0.03265 0.04512 = 0.02561 -0.00031 0.01124 -0.00330 AFIX 43 H9 2 0.628021 0.744306 0.143244 11.00000 -1.20000 AFIX 0 C10 1 0.707569 0.773984 0.145071 11.00000 0.06678 0.05974 = 0.04122 0.00298 0.03502 -0.00157 AFIX 43 H10 2 0.696968 0.768336 0.100264 11.00000 -1.20000 AFIX 0 C11 1 0.763158 0.796176 0.184749 11.00000 0.05350 0.07218 = 0.07780 -0.00476 0.05146 -0.01183 AFIX 43 H11 2 0.791641 0.804318 0.167661 11.00000 -1.20000 AFIX 0 C12 1 0.778123 0.806802 0.249325 11.00000 0.03141 0.06875 = 0.06628 -0.02150 0.02550 -0.02117 AFIX 43 H12 2 0.815930 0.824526 0.275574 11.00000 -1.20000 AFIX 0 C13 1 0.739552 0.792295 0.276193 11.00000 0.02866 0.04850 = 0.03703 -0.01000 0.01067 -0.00555 AFIX 43 H13 2 0.750786 0.798317 0.321072 11.00000 -1.20000 AFIX 0 C14 1 0.607085 0.781577 0.283538 11.00000 0.01953 0.03953 = 0.02625 -0.00062 0.00674 -0.00041 C15 1 0.599254 0.845864 0.283235 11.00000 0.02645 0.03597 = 0.04754 0.00352 0.01738 -0.00170 C16 1 0.622157 0.886571 0.253335 11.00000 0.03665 0.04498 = 0.06077 0.01306 0.02295 0.00571 AFIX 43 H16 2 0.642356 0.872281 0.228555 11.00000 -1.20000 AFIX 0 C17 1 0.615814 0.948185 0.259306 11.00000 0.04987 0.03973 = 0.09170 0.01188 0.03291 -0.00394 AFIX 43 H17 2 0.631696 0.975717 0.238695 11.00000 -1.20000 AFIX 0 C18 1 0.585553 0.969911 0.296268 11.00000 0.04889 0.03780 = 0.14805 -0.00294 0.05492 -0.00034 AFIX 43 H18 2 0.583470 1.011749 0.303452 11.00000 -1.20000 AFIX 0 C19 1 0.561035 0.931169 0.319734 11.00000 0.07546 0.03404 = 0.11695 0.01017 0.05470 0.02111 AFIX 43 H19 2 0.537479 0.946815 0.340260 11.00000 -1.20000 AFIX 0 C20 1 0.565490 0.867943 0.318155 11.00000 0.02897 0.05475 = 0.09796 0.00710 0.04006 0.00894 C21 1 0.541172 0.825269 0.349540 11.00000 0.01691 0.04634 = 0.04551 0.00292 0.01438 0.00023 C22 1 0.511277 0.846983 0.386374 11.00000 0.03946 0.04236 = 0.07724 0.00059 0.03288 0.00614 AFIX 43 H22 2 0.506471 0.889037 0.389760 11.00000 -1.20000 AFIX 0 C23 1 0.489039 0.807322 0.417443 11.00000 0.03843 0.05334 = 0.06492 -0.00863 0.03294 0.00090 AFIX 43 H23 2 0.468457 0.822398 0.441503 11.00000 -1.20000 AFIX 0 C24 1 0.496253 0.746186 0.414073 11.00000 0.02850 0.04367 = 0.04534 -0.00419 0.02022 -0.00499 AFIX 43 H24 2 0.482146 0.719558 0.437183 11.00000 -1.20000 AFIX 0 C25 1 0.523782 0.723668 0.377396 11.00000 0.01783 0.04570 = 0.02798 -0.00585 0.00661 -0.00659 AFIX 43 H25 2 0.527749 0.681409 0.374546 11.00000 -1.20000 AFIX 0 C26 1 0.546186 0.762366 0.343985 11.00000 0.01817 0.04144 = 0.02713 0.00210 0.00697 0.00564 C27 1 0.579641 0.741075 0.308790 11.00000 0.01309 0.03621 = 0.02233 0.00152 0.00158 -0.00243 C56 1 0.779779 0.440007 0.348039 11.00000 0.12362 0.05243 = 0.12921 0.04231 0.09839 0.05001 AFIX 137 H56A 2 0.740727 0.423323 0.318587 11.00000 -1.50000 H56B 2 0.778973 0.449871 0.389547 11.00000 -1.50000 H56C 2 0.811488 0.410330 0.355003 11.00000 -1.50000 AFIX 0 C55 1 0.829786 0.633155 0.239069 11.00000 0.04716 0.08291 = 0.08924 0.02819 0.04988 0.01419 AFIX 137 H55A 2 0.798128 0.641626 0.195875 11.00000 -1.50000 H55B 2 0.867585 0.624390 0.235801 11.00000 -1.50000 H55C 2 0.835310 0.668229 0.267029 11.00000 -1.50000 AFIX 0 C28 1 0.624389 0.601900 0.412447 11.00000 0.02055 0.05202 = 0.01866 -0.00060 0.00886 -0.00169 C29 1 0.653602 0.652921 0.447942 11.00000 0.02659 0.04922 = 0.02149 0.00207 0.00301 -0.00827 AFIX 43 H29 2 0.656970 0.687848 0.425725 11.00000 -1.20000 AFIX 0 C30 1 0.677599 0.653167 0.514845 11.00000 0.03083 0.05285 = 0.01978 0.00313 0.00045 -0.00681 C31 1 0.673787 0.601749 0.549094 11.00000 0.03001 0.05442 = 0.01269 0.00516 0.00461 0.00268 C32 1 0.645166 0.552209 0.516285 11.00000 0.03721 0.04987 = 0.01740 0.00621 0.01448 -0.00046 AFIX 43 H32 2 0.641578 0.517903 0.539220 11.00000 -1.20000 AFIX 0 C33 1 0.620103 0.551163 0.446804 11.00000 0.02623 0.03299 = 0.01910 0.00549 0.01106 0.00586 C34 1 0.597849 0.498606 0.406180 11.00000 0.02914 0.04355 = 0.01759 0.01063 0.01324 0.00428 C35 1 0.599143 0.422682 0.485452 11.00000 0.04226 0.03069 = 0.02194 0.00763 0.01894 0.00627 C36 1 0.550256 0.431290 0.499591 11.00000 0.02740 0.03997 = 0.02407 0.00548 0.01009 0.00194 AFIX 43 H36 2 0.513456 0.446239 0.467376 11.00000 -1.20000 AFIX 0 C37 1 0.555018 0.418107 0.560681 11.00000 0.04372 0.04375 = 0.02904 0.00523 0.02350 0.00460 AFIX 43 H37 2 0.522120 0.425868 0.571242 11.00000 -1.20000 AFIX 0 C38 1 0.607212 0.393803 0.606186 11.00000 0.05906 0.05278 = 0.02122 0.01273 0.02403 0.01426 AFIX 43 H38 2 0.609830 0.382949 0.647587 11.00000 -1.20000 AFIX 0 C39 1 0.656504 0.385039 0.591557 11.00000 0.06182 0.07546 = 0.03274 0.02697 0.02530 0.03484 AFIX 43 H39 2 0.692936 0.368993 0.623383 11.00000 -1.20000 AFIX 0 C40 1 0.652453 0.399684 0.530708 11.00000 0.04172 0.05757 = 0.03621 0.01068 0.02336 0.01353 AFIX 43 H40 2 0.685859 0.393936 0.520497 11.00000 -1.20000 AFIX 0 C41 1 0.584063 0.404633 0.368831 11.00000 0.02693 0.04343 = 0.02473 -0.00112 0.01625 0.00317 C42 1 0.579314 0.340889 0.362778 11.00000 0.03423 0.03730 = 0.03103 -0.00104 0.01777 0.00405 C43 1 0.577386 0.299798 0.410022 11.00000 0.05366 0.05285 = 0.04434 -0.00119 0.02849 0.00825 AFIX 43 H43 2 0.578266 0.315323 0.449221 11.00000 -1.20000 AFIX 0 C44 1 0.574363 0.239775 0.400948 11.00000 0.08012 0.04571 = 0.05943 0.00546 0.04187 0.00637 AFIX 43 H44 2 0.573641 0.214029 0.433850 11.00000 -1.20000 AFIX 0 C45 1 0.572258 0.214717 0.343157 11.00000 0.08810 0.04530 = 0.06342 -0.00295 0.04873 0.00700 AFIX 43 H45 2 0.572106 0.172329 0.337973 11.00000 -1.20000 AFIX 0 C46 1 0.570325 0.254378 0.291658 11.00000 0.04791 0.05653 = 0.03406 0.00764 0.00388 0.01487 AFIX 43 H46 2 0.565504 0.238882 0.250930 11.00000 -1.20000 AFIX 0 C47 1 0.575950 0.317694 0.304507 11.00000 0.02943 0.03923 = 0.03071 -0.00106 0.01159 0.01034 C48 1 0.573043 0.357701 0.251067 11.00000 0.02420 0.03844 = 0.03953 -0.00895 0.01488 -0.00147 C49 1 0.568620 0.335111 0.191035 11.00000 0.02616 0.05140 = 0.03064 -0.01042 0.00953 0.00532 AFIX 43 H49 2 0.564566 0.292995 0.183492 11.00000 -1.20000 AFIX 0 C50 1 0.569977 0.371370 0.144401 11.00000 0.03317 0.04922 = 0.02841 -0.01151 0.01306 0.00092 AFIX 43 H50 2 0.565487 0.354703 0.104252 11.00000 -1.20000 AFIX 0 C51 1 0.577974 0.433612 0.154629 11.00000 0.02379 0.04736 = 0.02067 -0.00052 0.00630 0.00211 AFIX 43 H51 2 0.581043 0.458852 0.122555 11.00000 -1.20000 AFIX 0 C52 1 0.581332 0.457760 0.211957 11.00000 0.03115 0.04689 = 0.01685 -0.00122 0.01023 0.00583 AFIX 43 H52 2 0.586173 0.499915 0.218924 11.00000 -1.20000 AFIX 0 C53 1 0.577639 0.420407 0.260276 11.00000 0.02570 0.04260 = 0.02338 0.00001 0.01317 0.00474 C54 1 0.580951 0.443799 0.320473 11.00000 0.02373 0.03056 = 0.02142 0.00308 0.01074 0.00171 C57 1 0.719894 0.552216 0.650879 11.00000 0.03244 0.07411 = 0.01763 0.01044 0.00121 -0.00843 AFIX 137 H57A 2 0.745763 0.530249 0.635209 11.00000 -1.50000 H57B 2 0.684814 0.527484 0.644826 11.00000 -1.50000 H57C 2 0.742602 0.561356 0.696971 11.00000 -1.50000 AFIX 0 PART 1 C58 1 0.683743 0.765730 0.524067 10.60000 0.11723 0.05367 = 0.03176 -0.01147 0.01471 -0.02977 AFIX 137 H58A 2 0.702816 0.778318 0.495993 10.60000 -1.50000 H58B 2 0.694523 0.793989 0.560229 10.60000 -1.50000 H58C 2 0.639903 0.765269 0.499144 10.60000 -1.50000 AFIX 0 PART 0 PART 2 C60 1 0.777366 0.690918 0.569908 10.40000 0.02684 0.10038 = 0.02691 -0.02027 0.00042 -0.03273 AFIX 137 H60A 2 0.791872 0.657713 0.600974 10.40000 -1.50000 H60B 2 0.800221 0.727429 0.589447 10.40000 -1.50000 H60C 2 0.782839 0.680683 0.530944 10.40000 -1.50000 AFIX 0 HKLF 4 REM z_a.res in C2/c REM wR2 = 0.1197, GooF = S = 1.069, Restrained GooF = 1.070 for all data REM R1 = 0.0502 for 8889 Fo > 4sig(Fo) and 0.0751 for all 12241 data REM 627 parameters refined using 6 restraints END WGHT 0.0369 118.9036 REM Highest difference peak 1.957, deepest hole -2.436, 1-sigma level 0.138 Q1 1 0.6924 0.8284 0.5821 11.00000 0.05 1.96 Q2 1 0.5634 0.5686 0.3006 11.00000 0.05 1.69 Q3 1 0.5652 0.6252 0.3196 11.00000 0.05 1.46 Q4 1 0.6303 0.7825 0.5388 11.00000 0.05 1.07 Q5 1 0.6031 0.5900 0.2831 11.00000 0.05 1.04 ; _shelx_res_checksum 7657 _shelx_hkl_file ; -4 0 0 87.19 2.32 4 0 0 85.54 2.33 6 0 0 447.54 11.45 -6 0 0 451.13 11.73 8 0 0 153.97 4.27 -8 0 0 161.80 4.26 10 0 0 82.23 2.53 -10 0 0 81.53 2.46 12 0 0 230.18 6.32 -12 0 0 230.87 6.25 -14 0 0 49.83 1.83 14 0 0 52.03 2.01 -16 0 0 32.86 1.48 16 0 0 33.21 1.74 -18 0 0 59.53 2.30 18 0 0 61.55 2.58 -20 0 0 14.21 1.26 20 0 0 15.01 1.77 -22 0 0 5.98 0.98 22 0 0 3.97 1.30 -24 0 0 18.88 1.70 24 0 0 17.29 2.19 26 0 0 -0.16 1.33 -26 0 0 0.92 0.98 28 0 0 6.56 1.80 -28 0 0 7.69 1.45 30 0 0 12.54 2.11 -30 0 0 14.13 1.83 -1 -1 0 0.03 0.02 -1 1 0 -0.02 0.01 1 1 0 -0.03 0.02 -1 1 0 0.01 0.02 -1 1 0 -0.01 0.02 -3 -1 0 4.64 0.26 3 -1 0 4.34 0.23 -3 1 0 4.35 0.24 3 1 0 4.52 0.32 -3 1 0 3.88 0.18 5 -1 0 325.30 8.30 -5 -1 0 332.61 8.38 -5 1 0 320.89 8.34 -5 1 0 312.36 8.12 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7.7474 -0.5584 18 12 11 -3.5434 -0.0518 18 14 0 16.1126 -0.2173 18 14 1 -4.8358 -0.1407 18 14 2 18.3604 0.1712 18 14 3 4.7691 0.2065 18 14 4 8.6783 0.7555 18 14 5 -4.8438 0.1664 18 14 6 -3.3703 -0.1981 18 14 7 -9.0379 -0.3469 18 14 8 -17.3387 -0.4920 18 14 9 -5.7413 0.2090 18 14 10 -20.7056 -0.5449 18 16 0 4.4813 -0.0866 18 16 1 -14.9677 -0.2931 18 16 2 1.9519 0.4795 18 16 3 -4.7502 0.2417 18 16 4 14.2540 0.3885 18 16 5 21.9032 0.3924 18 16 6 13.6663 -0.1223 18 16 7 9.2305 0.4882 18 16 8 -3.2338 -0.0844 18 18 0 -0.9516 0.1331 18 18 1 -18.3184 -0.0911 18 18 2 -0.4242 0.3269 18 18 3 -0.1839 0.2816 18 18 4 18.7691 0.0516 18 18 5 14.1057 0.0462 18 18 6 -5.4542 0.1391 18 20 0 -4.7840 -0.3321 18 20 1 1.0384 -0.0898 18 20 2 -7.0162 0.5787 18 20 3 12.8350 0.0445 19 1 0 -28.3806 -9.6581 19 1 1 14.2658 3.9842 19 1 2 0.1686 0.7503 19 1 3 1.8361 0.2447 19 1 4 -1.9023 1.2525 19 1 5 4.5321 -0.8707 19 1 6 -4.4315 -1.5739 19 1 7 11.5161 0.9478 19 1 8 -9.8677 1.3998 19 1 9 10.3933 -0.4103 19 1 10 -27.6835 0.3108 19 1 11 11.0443 -0.9798 19 1 12 -9.9900 -1.9038 19 1 13 9.6000 1.2776 19 3 0 -19.4965 -0.2944 19 3 1 2.6693 2.1611 19 3 2 -13.1066 0.2943 19 3 3 -5.6196 -0.0606 19 3 4 -3.1365 0.6563 19 3 5 1.7065 -2.5550 19 3 6 5.7125 0.1476 19 3 7 9.7756 1.3802 19 3 8 1.0405 -0.1350 19 3 9 4.0574 -0.2772 19 3 10 -14.4419 0.2264 19 3 11 12.8203 -1.2530 19 3 12 -8.0949 0.1076 19 3 13 7.0130 1.8201 19 5 0 -0.8672 2.0839 19 5 1 -2.4685 1.4529 19 5 2 1.6328 -0.0795 19 5 3 -4.9916 0.0772 19 5 4 7.2648 -2.0395 19 5 5 3.9321 -0.9924 19 5 6 9.4564 1.8089 19 5 7 19.0320 0.5029 19 5 8 9.1390 -0.9342 19 5 9 16.4460 0.6403 19 5 10 11.4288 0.2985 19 5 11 16.2840 -0.6080 19 5 12 6.6546 1.3745 19 7 0 7.3178 0.3265 19 7 1 5.4805 -0.5631 19 7 2 -1.8576 -0.8171 19 7 3 0.6013 -1.3887 19 7 4 4.0721 -0.5100 19 7 5 1.6601 1.2837 19 7 6 6.1514 0.9253 19 7 7 1.8461 -0.6283 19 7 8 0.8693 -0.7066 19 7 9 -10.6544 1.5843 19 7 10 0.3090 0.0116 19 7 11 -21.2932 -0.3607 19 7 12 11.2814 1.1111 19 9 0 8.1230 -0.3833 19 9 1 -5.6271 -0.2771 19 9 2 4.8142 -0.4664 19 9 3 4.8426 -0.2122 19 9 4 -4.5581 1.1408 19 9 5 4.7934 0.8774 19 9 6 -15.6691 -0.5291 19 9 7 5.8998 -0.7714 19 9 8 -8.1522 0.4844 19 9 9 -9.9702 0.8549 19 9 10 -4.5093 -0.2469 19 9 11 -12.2372 -0.0522 19 11 0 -4.4743 -0.5867 19 11 1 -0.0633 -0.1672 19 11 2 -5.8171 -0.2672 19 11 3 -1.6847 0.5295 19 11 4 -16.6716 0.4811 19 11 5 -6.8009 -0.5844 19 11 6 -8.8977 -0.6800 19 11 7 8.2211 0.0008 19 11 8 -6.9267 1.2116 19 11 9 11.4237 0.1516 19 11 10 2.9707 -0.3042 19 13 0 -11.5837 -0.2317 19 13 1 -13.8589 -0.8685 19 13 2 -14.2414 -0.2480 19 13 3 -16.7852 0.0541 19 13 4 -17.0842 -0.6184 19 13 5 5.7990 0.2459 19 13 6 -5.8694 0.5089 19 13 7 12.8202 1.4536 19 13 8 -5.4978 0.6730 19 13 9 15.1938 -0.1119 19 15 0 -13.0766 0.0543 19 15 1 -0.3028 0.2185 19 15 2 -6.2340 -0.0068 19 15 3 -0.4406 -0.2015 19 15 4 9.3305 -0.0975 19 15 5 -4.9482 0.2101 19 15 6 1.8663 1.0419 19 15 7 10.2359 0.5514 19 15 8 -5.1919 0.5102 19 17 0 14.6048 -0.1519 19 17 1 17.8054 0.0864 19 17 2 15.5611 -0.0232 19 17 3 14.7646 -0.2572 19 17 4 -21.5749 0.0384 19 17 5 -1.9483 -0.2994 19 17 6 -11.4084 -0.0267 19 19 0 17.4297 -0.0666 19 19 1 17.3127 0.0789 19 19 2 18.2722 -0.0244 19 19 3 -4.4118 -0.1583 19 21 0 20.1714 0.1588 20 0 0 -0.4509 7.0312 20 0 2 -4.4565 0.5819 20 0 4 11.6024 -2.0777 20 0 6 8.5563 1.1809 20 0 8 1.9508 -0.6303 20 0 10 5.1714 -0.6556 20 0 12 -10.2131 1.9825 20 2 0 0.0471 3.2354 20 2 1 -16.4094 -1.1280 20 2 2 -5.7778 1.6877 20 2 3 -5.0884 -1.3793 20 2 4 2.0561 -1.0346 20 2 5 -9.1609 2.6090 20 2 6 -6.3237 0.7608 20 2 7 -12.5171 -0.6945 20 2 8 -12.1160 0.2484 20 2 9 -3.3315 -1.2909 20 2 10 -3.0103 0.1893 20 2 11 2.3040 1.1378 20 2 12 -10.9733 0.7753 20 4 0 4.6722 -0.0801 20 4 1 -19.7349 -0.8948 20 4 2 4.1059 -1.2570 20 4 3 -12.8841 -1.8211 20 4 4 1.4287 1.0249 20 4 5 -14.3709 3.0807 20 4 6 4.7926 -2.0577 20 4 7 -16.0661 -0.5381 20 4 8 18.1746 -0.6640 20 4 9 -4.0332 -1.3089 20 4 10 24.9858 0.3181 20 4 11 1.0335 0.4265 20 4 12 15.9320 -0.5478 20 6 0 -20.3388 -0.3257 20 6 1 -8.0266 -0.3265 20 6 2 -3.4372 0.0779 20 6 3 4.2378 1.0266 20 6 4 5.4446 2.1601 20 6 5 0.3224 -0.3653 20 6 6 5.3035 -2.1790 20 6 7 -8.9159 0.2848 20 6 8 7.6639 0.5263 20 6 9 -0.8688 -0.8017 20 6 10 8.2206 0.7372 20 6 11 5.1456 0.2300 20 8 0 -12.8150 -0.0736 20 8 1 23.1430 -0.0446 20 8 2 -8.9972 0.4983 20 8 3 13.2509 1.0036 20 8 4 -6.8412 -0.2493 20 8 5 2.6530 -1.7388 20 8 6 4.1316 -0.1521 20 8 7 0.6071 0.6413 20 8 8 12.4210 0.0343 20 8 9 11.7157 -0.0890 20 8 10 16.6152 0.5523 20 8 11 11.3687 1.1523 20 10 0 3.2972 0.1103 20 10 1 5.5456 0.1741 20 10 2 -1.0671 0.0829 20 10 3 7.3088 -0.4729 20 10 4 -2.6942 -1.3303 20 10 5 20.0359 -0.7441 20 10 6 -9.3174 0.9299 20 10 7 14.2320 0.5273 20 10 8 -11.9712 0.2346 20 10 9 13.9180 0.4826 20 10 10 -13.9541 0.7098 20 12 0 9.0071 0.0986 20 12 1 18.9237 0.3673 20 12 2 13.2610 -0.2311 20 12 3 10.4983 -0.9089 20 12 4 17.1028 -0.6516 20 12 5 -1.5363 0.7282 20 12 6 -12.4990 0.2590 20 12 7 -12.4936 0.4908 20 12 8 -21.4075 0.4538 20 12 9 -20.3735 0.4976 20 14 0 -5.0202 0.5893 20 14 1 7.9070 0.0520 20 14 2 -12.7540 -0.5997 20 14 3 3.6539 -0.5132 20 14 4 -11.6818 -0.0749 20 14 5 -8.4811 -0.2808 20 14 6 5.3301 -0.3465 20 14 7 -3.0590 -0.3458 20 16 0 -10.3759 -0.0617 20 16 1 -6.8822 -0.3323 20 16 2 -6.0841 -0.4839 20 16 3 -15.2066 -0.4110 20 16 4 10.0600 -0.5606 20 16 5 2.6572 -0.5344 20 18 0 -17.7996 -0.1769 20 18 1 -20.5957 0.0114 20 18 2 -29.5318 -0.1278 20 18 3 -0.6383 0.0409 20 20 0 -31.6855 0.2169 21 1 0 25.7616 -0.0938 21 1 1 -0.6890 -0.2394 21 1 2 23.7273 -2.4873 21 1 3 0.0292 1.2051 21 1 4 3.0745 1.7268 21 1 5 -2.7371 -1.1847 21 1 6 4.9532 -0.9741 21 1 7 -10.5777 0.1909 21 1 8 8.6879 -0.7744 21 1 9 -12.7841 1.0506 21 1 10 3.9882 1.3860 21 1 11 -10.9220 -1.2991 21 3 0 3.2048 -1.3370 21 3 1 21.1284 -2.4318 21 3 2 10.6123 -0.0384 21 3 3 11.3384 4.1609 21 3 4 1.9687 -0.1290 21 3 5 11.8117 -1.9685 21 3 6 -5.3327 0.5911 21 3 7 8.3354 0.2903 21 3 8 -6.3068 0.2395 21 3 9 -10.1857 1.6916 21 3 10 -1.7908 -0.7382 21 3 11 -26.3539 -1.9709 21 5 0 5.2211 -0.1943 21 5 1 20.0772 0.5844 21 5 2 -2.5065 2.3074 21 5 3 12.1172 0.7910 21 5 4 -11.2897 -1.9016 21 5 5 6.6120 -1.3287 21 5 6 -10.9217 2.0723 21 5 7 -2.0037 0.0606 21 5 8 -13.3029 -0.0768 21 5 9 -17.5726 0.6663 21 5 10 -11.1789 -2.0981 21 7 0 -0.3482 0.0502 21 7 1 -17.3442 0.6921 21 7 2 -13.7201 0.5738 21 7 3 -15.3802 -1.3914 21 7 4 -13.5746 -1.1404 21 7 5 6.3247 0.5099 21 7 6 -10.2707 0.6462 21 7 7 21.4583 -1.0949 21 7 8 -7.7669 -0.5383 21 7 9 12.3057 0.0151 21 7 10 -8.1001 -1.4517 21 9 0 -12.2534 0.7841 21 9 1 -18.8698 0.5135 21 9 2 1.1030 -0.6147 21 9 3 -10.9474 -0.3615 21 9 4 17.2726 0.3036 21 9 5 -6.8031 1.0450 21 9 6 28.7413 -0.2219 21 9 7 4.4333 -0.5869 21 9 8 19.4785 0.3013 21 9 9 -0.7791 -0.4570 21 11 0 -1.4317 0.7762 21 11 1 -10.7970 -0.1095 21 11 2 3.4337 0.2499 21 11 3 -5.7884 0.2848 21 11 4 3.6917 0.7983 21 11 5 -8.4251 -0.4258 21 11 6 21.9849 -0.9978 21 11 7 -10.6897 -0.6187 21 11 8 19.8636 -0.6358 21 13 0 -0.0708 -0.0444 21 13 1 -9.8744 -0.0269 21 13 2 4.2227 0.3976 21 13 3 -1.2600 0.4008 21 13 4 4.0819 -0.3595 21 13 5 2.8842 -1.5349 21 13 6 17.6419 -0.5672 21 13 7 -11.2273 -0.8518 21 15 0 6.2041 -0.5960 21 15 1 22.5180 0.2647 21 15 2 6.2917 0.2407 21 15 3 9.2854 0.2209 21 15 4 -12.4982 -0.1385 21 15 5 -6.8199 0.0824 21 17 0 0.8835 -0.2221 21 17 1 14.9654 0.1397 21 17 2 2.0904 -0.1423 21 17 3 -3.1399 -0.0409 21 19 0 11.7944 -0.0824 22 0 0 -25.8952 -7.5869 22 0 2 -30.3151 2.7793 22 0 4 -12.8722 -1.5129 22 0 6 -1.6639 -0.2906 22 0 8 19.2752 0.8734 22 0 10 27.6406 -2.7325 22 2 0 -17.2458 -0.5261 22 2 1 1.1464 3.6162 22 2 2 -22.7175 2.9766 22 2 3 6.0027 -4.2116 22 2 4 -3.9835 -0.0785 22 2 5 3.7376 0.8201 22 2 6 9.3829 0.0608 22 2 7 7.6089 1.1599 22 2 8 10.7265 0.4988 22 2 9 6.8334 -0.8206 22 2 10 3.1767 -0.2901 22 4 0 2.4389 0.7114 22 4 1 -8.2175 1.3686 22 4 2 -2.5344 -2.5189 22 4 3 0.9789 -3.8810 22 4 4 2.7233 1.5609 22 4 5 7.6988 0.6718 22 4 6 -0.4044 -0.5287 22 4 7 10.6550 0.6778 22 4 8 -10.2193 -0.6630 22 4 9 16.8184 -0.2632 22 6 0 15.7070 0.5718 22 6 1 -3.2599 -0.9048 22 6 2 10.5135 -2.0145 22 6 3 -3.1540 0.4017 22 6 4 3.8845 1.8789 22 6 5 -15.2414 0.7387 22 6 6 -4.2819 -0.1597 22 6 7 -11.2355 0.5408 22 6 8 -10.2882 -0.1793 22 6 9 4.2467 -0.2183 22 8 0 24.5721 -0.4090 22 8 1 -2.5433 -0.7946 22 8 2 19.0242 0.0780 22 8 3 -8.2136 1.9648 22 8 4 -0.0022 0.8301 22 8 5 -14.5663 0.0161 22 8 6 -15.9962 -0.1308 22 8 7 -25.5874 -0.3617 22 8 8 -16.1089 -0.1542 22 10 0 1.7420 -0.8565 22 10 1 9.4952 0.0428 22 10 2 -2.1553 0.9215 22 10 3 -3.0158 -0.1043 22 10 4 0.3767 -0.2245 22 10 5 -9.4262 -0.7038 22 10 6 -13.4806 -0.3634 22 10 7 -11.7010 -0.0091 22 12 0 -7.6655 0.1911 22 12 1 8.4713 0.5402 22 12 2 -8.9161 0.4222 22 12 3 8.3864 -0.0508 22 12 4 -3.2415 0.1842 22 12 5 12.8556 0.6042 22 12 6 -4.9161 0.3210 22 14 0 9.0792 0.2483 22 14 1 -4.2616 0.4014 22 14 2 1.5555 0.3976 22 14 3 -2.9532 -0.1550 22 14 4 15.7124 0.2830 22 16 0 8.5579 0.5305 22 16 1 -19.9583 0.1782 22 16 2 1.1593 -0.4282 23 1 0 8.7346 8.1695 23 1 1 -3.4059 -3.4325 23 1 2 11.9739 -3.1034 23 1 3 -9.7480 1.6833 23 1 4 -2.5674 0.5667 23 1 5 -2.2222 -0.4195 23 1 6 -12.7700 1.0118 23 1 7 3.6120 -1.6728 23 1 8 -23.2546 -2.3905 23 3 0 7.5747 -1.1471 23 3 1 -12.3421 -3.1225 23 3 2 13.5698 -0.5677 23 3 3 -17.4003 3.8290 23 3 4 8.1782 -1.0230 23 3 5 -7.7707 -0.3285 23 3 6 3.2231 0.2292 23 3 7 1.4596 -1.7586 23 3 8 8.4022 0.4744 23 5 0 0.2006 -1.9357 23 5 1 -9.4627 -0.4267 23 5 2 12.9741 1.8192 23 5 3 -13.7912 1.0851 23 5 4 13.7794 -1.3990 23 5 5 -2.1124 -0.4408 23 5 6 14.7190 -0.0891 23 5 7 7.2543 -0.8740 23 5 8 16.9686 2.3589 23 7 0 -23.9514 -0.0108 23 7 1 21.7256 0.8244 23 7 2 -5.2675 1.1858 23 7 3 18.4768 -0.9405 23 7 4 10.4652 -1.4972 23 7 5 13.4388 -0.3007 23 7 6 15.8653 -0.3583 23 7 7 3.9158 1.1645 23 9 0 4.3784 -0.0401 23 9 1 14.8878 0.0557 23 9 2 -6.5163 -0.7979 23 9 3 17.6693 -0.7119 23 9 4 -14.0980 0.0153 23 9 5 11.4675 0.7780 23 9 6 -5.6808 0.8584 23 11 0 -7.0211 0.2797 23 11 1 -8.8134 -0.6473 23 11 2 -15.3203 -0.1439 23 11 3 -9.2464 0.8415 23 11 4 -22.3606 0.0018 23 11 5 -4.8581 0.6579 23 13 0 0.6986 -0.5553 23 13 1 -7.4612 -0.3456 23 13 2 6.2673 -0.2899 23 13 3 1.2855 0.3242 23 13 4 -5.0880 0.8096 23 15 0 -9.0031 -0.1564 23 15 1 -8.7511 -0.2686 23 15 2 13.5865 0.6305 24 0 0 5.3505 -12.9394 24 0 2 4.9989 2.2538 24 0 4 14.4954 0.0586 24 0 6 1.4524 -1.7186 24 2 0 -4.3756 -3.0554 24 2 1 6.6951 4.7413 24 2 2 -0.3887 1.1887 24 2 3 12.0360 -1.1944 24 2 4 0.9746 0.6001 24 2 5 -2.4061 -1.0941 24 2 6 -4.6125 -0.6454 24 2 7 -9.0360 1.4055 24 4 0 -15.9357 2.0840 24 4 1 7.4890 2.0908 24 4 2 -27.7086 -0.3058 24 4 3 8.1104 -0.7576 24 4 4 -21.3172 0.0970 24 4 5 -8.8049 -0.9337 24 4 6 0.0866 0.0334 24 4 7 -20.6808 0.2589 24 6 0 -6.4574 1.7918 24 6 1 -3.4562 -0.3221 24 6 2 -15.9134 -1.3804 24 6 3 -0.3473 -0.3283 24 6 4 -10.5625 -0.2302 24 6 5 0.7540 0.3482 24 6 6 -1.8834 0.5090 24 8 0 -1.1007 -0.4395 24 8 1 -3.5930 -0.8103 24 8 2 0.6152 -0.4914 24 8 3 -1.5634 -0.2823 24 8 4 3.1752 0.7152 24 8 5 0.5887 0.0442 24 10 0 6.6337 -0.4963 24 10 1 -11.7391 0.0172 24 10 2 16.0243 -0.4457 24 10 3 2.7859 -0.5648 24 10 4 15.5959 -0.2865 24 12 0 17.1027 -0.1683 24 12 1 15.5687 -0.0643 24 12 2 17.4561 -0.4878 24 12 3 0.0281 0.3501 24 14 0 3.6714 0.3106 24 14 1 -0.4463 -0.0327 25 1 0 0.4079 8.4014 25 1 1 6.5572 -3.1122 25 1 2 -6.6437 -0.7064 25 1 3 -1.2063 -0.0422 25 1 4 -7.4065 -1.7307 25 1 5 0.9008 1.5398 25 1 6 17.3916 2.7857 25 3 0 4.5869 0.1823 25 3 1 7.5479 -1.8385 25 3 2 8.0995 -0.1133 25 3 3 -0.4366 -0.3079 25 3 4 3.1380 -0.3719 25 3 5 3.3107 3.2796 25 5 0 9.6063 -1.8169 25 5 1 16.2827 -0.6896 25 5 2 10.1566 0.6628 25 5 3 15.4489 0.1922 25 5 4 1.3690 1.6868 25 5 5 6.4909 1.0767 25 7 0 9.4473 0.1189 25 7 1 -18.0793 1.0542 25 7 2 3.8925 1.0328 25 7 3 -16.1801 0.4771 25 7 4 -6.5884 0.6341 25 9 0 -14.8981 0.5812 25 9 1 -13.0922 0.6514 25 9 2 -4.5170 0.5350 25 9 3 -13.6056 0.4520 25 11 0 -3.8019 -0.2146 25 11 1 1.1887 0.7064 25 11 2 -6.6886 0.3144 25 13 0 -20.1270 -0.2097 26 0 0 -8.7386 -4.7484 26 0 2 3.2752 -0.3795 26 0 4 10.7726 2.6943 26 2 0 -3.8168 -2.6637 26 2 1 -7.2209 0.0730 26 2 2 -2.1417 -1.1836 26 2 3 3.2893 1.7285 26 2 4 3.5067 1.0224 26 4 0 12.7253 0.5158 26 4 1 -17.5411 -0.0747 26 4 2 12.2112 1.1805 26 4 3 -6.1756 1.6149 26 6 0 -0.4893 0.2324 26 6 1 3.6985 0.1283 26 6 2 2.3035 -0.0237 26 6 3 5.2133 -0.3652 26 8 0 15.5603 -0.4812 26 8 1 12.7173 -0.2067 26 8 2 5.2724 -0.0430 26 10 0 -5.7842 0.6540 26 10 1 13.9614 0.1745 27 1 0 9.1302 -0.5815 27 1 1 -5.6655 1.0125 27 1 2 1.8641 3.9115 27 3 0 -5.5175 0.9632 27 3 1 -0.4866 1.6855 27 3 2 -7.3180 -0.0581 27 5 0 -8.8454 -0.6323 27 5 1 -4.3034 -0.7583 27 7 0 -19.4810 -0.1182 27 7 1 5.1314 -0.8507 28 0 0 -4.9665 6.8994 28 2 0 1.0826 0.9621 28 4 0 -1.2218 -0.9545 0 0 0 0.0 0.0 ; _shelx_fab_checksum 25708 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -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 0.58489(2) 0.59315(2) 0.31597(2) 0.02249(8) Uani 1 1 d . . . . . Cl1 Cl 0.47818(6) 0.59200(8) 0.30579(6) 0.0247(3) Uani 1 1 d . . . . . N1 N 0.5977(2) 0.6830(2) 0.3017(2) 0.0213(11) Uani 1 1 d . . . . . N2 N 0.6435(2) 0.7479(2) 0.2632(2) 0.0253(11) Uani 1 1 d . . . . . N3 N 0.5875(2) 0.5035(2) 0.3434(2) 0.0248(12) Uani 1 1 d . . . . . N4 N 0.5947(2) 0.4414(3) 0.4233(2) 0.0293(12) Uani 1 1 d . . . . . O1 O 0.7915(2) 0.4925(2) 0.3207(3) 0.0484(14) Uani 1 1 d . . . . . O2 O 0.8132(2) 0.5838(2) 0.2653(3) 0.0497(14) Uani 1 1 d . . . . . O3 O 0.7056(3) 0.7025(3) 0.5504(2) 0.0644(18) Uani 1 1 d . . . . . O4 O 0.7005(2) 0.6062(3) 0.6158(2) 0.0475(14) Uani 1 1 d . . . . . C1 C 0.6622(2) 0.5881(3) 0.3074(2) 0.0235(13) Uani 1 1 d . . . . . C2 C 0.7014(3) 0.5380(3) 0.3219(3) 0.0327(15) Uani 1 1 d . . . . . H2 H 0.693273 0.503354 0.341322 0.039 Uiso 1 1 calc R U . . . C3 C 0.7511(3) 0.5387(3) 0.3084(3) 0.0347(16) Uani 1 1 d . . . . . C4 C 0.7633(3) 0.5895(3) 0.2781(3) 0.0345(15) Uani 1 1 d . . . . . C5 C 0.7266(3) 0.6388(3) 0.2650(3) 0.0304(15) Uani 1 1 d . . . . . H5 H 0.734960 0.673270 0.245577 0.036 Uiso 1 1 calc R U . . . C6 C 0.6766(2) 0.6385(3) 0.2801(3) 0.0270(14) Uani 1 1 d . . . . . C7 C 0.6391(2) 0.6893(3) 0.2776(3) 0.0233(13) Uani 1 1 d . . . . . C8 C 0.6831(3) 0.7684(3) 0.2362(3) 0.0277(14) Uani 1 1 d . . . . . C9 C 0.6667(3) 0.7597(3) 0.1704(3) 0.0348(16) Uani 1 1 d . . . . . H9 H 0.628021 0.744306 0.143244 0.042 Uiso 1 1 calc R U . . . C10 C 0.7076(4) 0.7740(4) 0.1451(4) 0.052(2) Uani 1 1 d . . . . . H10 H 0.696968 0.768336 0.100264 0.062 Uiso 1 1 calc R U . . . C11 C 0.7632(4) 0.7962(4) 0.1847(4) 0.060(2) Uani 1 1 d . . . . . H11 H 0.791641 0.804318 0.167661 0.072 Uiso 1 1 calc R U . . . C12 C 0.7781(3) 0.8068(4) 0.2493(4) 0.054(2) Uani 1 1 d . . . . . H12 H 0.815930 0.824526 0.275574 0.065 Uiso 1 1 calc R U . . . C13 C 0.7396(3) 0.7923(3) 0.2762(3) 0.0392(17) Uani 1 1 d . . . . . H13 H 0.750786 0.798317 0.321072 0.047 Uiso 1 1 calc R U . . . C14 C 0.6071(3) 0.7816(3) 0.2835(3) 0.0295(14) Uani 1 1 d . . . . . C15 C 0.5993(3) 0.8459(3) 0.2832(3) 0.0361(16) Uani 1 1 d . . . . . C16 C 0.6222(3) 0.8866(4) 0.2533(4) 0.0467(19) Uani 1 1 d . . . . . H16 H 0.642356 0.872281 0.228555 0.056 Uiso 1 1 calc R U . . . C17 C 0.6158(4) 0.9482(4) 0.2593(5) 0.059(2) Uani 1 1 d . . . . . H17 H 0.631696 0.975717 0.238695 0.071 Uiso 1 1 calc R U . . . C18 C 0.5856(4) 0.9699(4) 0.2963(6) 0.074(3) Uani 1 1 d . . . . . H18 H 0.583470 1.011749 0.303452 0.088 Uiso 1 1 calc R U . . . C19 C 0.5610(5) 0.9312(4) 0.3197(5) 0.071(3) Uani 1 1 d . . . . . H19 H 0.537479 0.946815 0.340260 0.085 Uiso 1 1 calc R U . . . C20 C 0.5655(3) 0.8679(4) 0.3182(5) 0.056(2) Uani 1 1 d . . . . . C21 C 0.5412(3) 0.8253(3) 0.3495(3) 0.0359(16) Uani 1 1 d . . . . . C22 C 0.5113(3) 0.8470(4) 0.3864(4) 0.050(2) Uani 1 1 d . . . . . H22 H 0.506471 0.889037 0.389760 0.060 Uiso 1 1 calc R U . . . C23 C 0.4890(3) 0.8073(4) 0.4174(4) 0.048(2) Uani 1 1 d . . . . . H23 H 0.468457 0.822398 0.441503 0.058 Uiso 1 1 calc R U . . . C24 C 0.4963(3) 0.7462(3) 0.4141(3) 0.0376(17) Uani 1 1 d . . . . . H24 H 0.482146 0.719558 0.437183 0.045 Uiso 1 1 calc R U . . . C25 C 0.5238(3) 0.7237(3) 0.3774(3) 0.0316(15) Uani 1 1 d . . . . . H25 H 0.527749 0.681409 0.374546 0.038 Uiso 1 1 calc R U . . . C26 C 0.5462(3) 0.7624(3) 0.3440(3) 0.0298(15) Uani 1 1 d . . . . . C27 C 0.5796(2) 0.7411(3) 0.3088(3) 0.0259(13) Uani 1 1 d . . . . . C56 C 0.7798(5) 0.4400(4) 0.3480(6) 0.086(4) Uani 1 1 d . . . . . H56A H 0.740727 0.423323 0.318587 0.129 Uiso 1 1 calc R U . . . H56B H 0.778973 0.449871 0.389547 0.129 Uiso 1 1 calc R U . . . H56C H 0.811488 0.410330 0.355003 0.129 Uiso 1 1 calc R U . . . C55 C 0.8298(4) 0.6332(4) 0.2391(5) 0.066(3) Uani 1 1 d . . . . . H55A H 0.798128 0.641626 0.195875 0.099 Uiso 1 1 calc R U . . . H55B H 0.867585 0.624390 0.235801 0.099 Uiso 1 1 calc R U . . . H55C H 0.835310 0.668229 0.267029 0.099 Uiso 1 1 calc R U . . . C28 C 0.6244(3) 0.6019(3) 0.4124(3) 0.0302(15) Uani 1 1 d . . . . . C29 C 0.6536(3) 0.6529(3) 0.4479(3) 0.0349(16) Uani 1 1 d . . . . . H29 H 0.656970 0.687848 0.425725 0.042 Uiso 1 1 calc R U . . . C30 C 0.6776(3) 0.6532(4) 0.5148(3) 0.0380(17) Uani 1 1 d . . . . . C31 C 0.6738(3) 0.6017(3) 0.5491(3) 0.0339(16) Uani 1 1 d . . . . . C32 C 0.6452(3) 0.5522(3) 0.5163(3) 0.0338(16) Uani 1 1 d . . . . . H32 H 0.641578 0.517903 0.539220 0.041 Uiso 1 1 calc R U . . . C33 C 0.6201(3) 0.5512(3) 0.4468(3) 0.0256(14) Uani 1 1 d . . . . . C34 C 0.5978(3) 0.4986(3) 0.4062(3) 0.0289(15) Uani 1 1 d . . . . . C35 C 0.5991(3) 0.4227(3) 0.4855(3) 0.0298(15) Uani 1 1 d . . . . . C36 C 0.5503(3) 0.4313(3) 0.4996(3) 0.0308(15) Uani 1 1 d . . . . . H36 H 0.513456 0.446239 0.467376 0.037 Uiso 1 1 calc R U . . . C37 C 0.5550(3) 0.4181(3) 0.5607(3) 0.0361(17) Uani 1 1 d . . . . . H37 H 0.522120 0.425868 0.571242 0.043 Uiso 1 1 calc R U . . . C38 C 0.6072(3) 0.3938(3) 0.6062(3) 0.0419(19) Uani 1 1 d . . . . . H38 H 0.609830 0.382949 0.647587 0.050 Uiso 1 1 calc R U . . . C39 C 0.6565(4) 0.3850(4) 0.5916(4) 0.055(2) Uani 1 1 d . . . . . H39 H 0.692936 0.368993 0.623383 0.066 Uiso 1 1 calc R U . . . C40 C 0.6525(3) 0.3997(4) 0.5307(3) 0.0428(18) Uani 1 1 d . . . . . H40 H 0.685859 0.393936 0.520497 0.051 Uiso 1 1 calc R U . . . C41 C 0.5841(3) 0.4046(3) 0.3688(3) 0.0299(14) Uani 1 1 d . . . . . C42 C 0.5793(3) 0.3409(3) 0.3628(3) 0.0328(15) Uani 1 1 d . . . . . C43 C 0.5774(4) 0.2998(4) 0.4100(4) 0.048(2) Uani 1 1 d . . . . . H43 H 0.578266 0.315323 0.449221 0.057 Uiso 1 1 calc R U . . . C44 C 0.5744(4) 0.2398(4) 0.4009(4) 0.058(2) Uani 1 1 d . . . . . H44 H 0.573641 0.214029 0.433850 0.069 Uiso 1 1 calc R U . . . C45 C 0.5723(4) 0.2147(4) 0.3432(4) 0.060(2) Uani 1 1 d . . . . . H45 H 0.572106 0.172329 0.337973 0.072 Uiso 1 1 calc R U . . . C46 C 0.5703(3) 0.2544(4) 0.2917(4) 0.0508(18) Uani 1 1 d . U . . . H46 H 0.565504 0.238882 0.250930 0.061 Uiso 1 1 calc R U . . . C47 C 0.5759(3) 0.3177(3) 0.3045(3) 0.0335(14) Uani 1 1 d . U . . . C48 C 0.5730(3) 0.3577(3) 0.2511(3) 0.0336(15) Uani 1 1 d . . . . . C49 C 0.5686(3) 0.3351(4) 0.1910(3) 0.0369(17) Uani 1 1 d . . . . . H49 H 0.564566 0.292995 0.183492 0.044 Uiso 1 1 calc R U . . . C50 C 0.5700(3) 0.3714(3) 0.1444(3) 0.0369(17) Uani 1 1 d . . . . . H50 H 0.565487 0.354703 0.104252 0.044 Uiso 1 1 calc R U . . . C51 C 0.5780(3) 0.4336(3) 0.1546(3) 0.0317(15) Uani 1 1 d . . . . . H51 H 0.581043 0.458852 0.122555 0.038 Uiso 1 1 calc R U . . . C52 C 0.5813(3) 0.4578(3) 0.2120(3) 0.0316(15) Uani 1 1 d . . . . . H52 H 0.586173 0.499915 0.218924 0.038 Uiso 1 1 calc R U . . . C53 C 0.5776(3) 0.4204(3) 0.2603(3) 0.0296(15) Uani 1 1 d . . . . . C54 C 0.5810(3) 0.4438(3) 0.3205(3) 0.0248(13) Uani 1 1 d . . . . . C57 C 0.7199(3) 0.5522(4) 0.6509(3) 0.045(2) Uani 1 1 d . . . . . H57A H 0.745763 0.530249 0.635209 0.067 Uiso 1 1 calc R U . . . H57B H 0.684814 0.527484 0.644826 0.067 Uiso 1 1 calc R U . . . H57C H 0.742602 0.561356 0.696971 0.067 Uiso 1 1 calc R U . . . C58 C 0.6837(8) 0.7657(7) 0.5241(6) 0.073(5) Uani 0.6 1 d . . P A 1 H58A H 0.702816 0.778318 0.495993 0.110 Uiso 0.6 1 calc R U P A 1 H58B H 0.694523 0.793989 0.560229 0.110 Uiso 0.6 1 calc R U P A 1 H58C H 0.639903 0.765269 0.499144 0.110 Uiso 0.6 1 calc R U P A 1 C60 C 0.7774(7) 0.6909(11) 0.5699(8) 0.055(6) Uani 0.4 1 d . . P A 2 H60A H 0.791872 0.657713 0.600974 0.083 Uiso 0.4 1 calc R U P A 2 H60B H 0.800221 0.727429 0.589447 0.083 Uiso 0.4 1 calc R U P A 2 H60C H 0.782839 0.680683 0.530944 0.083 Uiso 0.4 1 calc R U P A 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 Ir1 0.01863(11) 0.03562(14) 0.01373(10) 0.00265(12) 0.00733(8) 0.00105(12) Cl1 0.0201(6) 0.0421(9) 0.0130(5) -0.0014(7) 0.0080(5) -0.0023(7) N1 0.019(2) 0.031(3) 0.013(2) -0.003(2) 0.0065(19) 0.003(2) N2 0.022(3) 0.035(3) 0.019(2) 0.002(2) 0.009(2) -0.001(2) N3 0.025(3) 0.042(3) 0.007(2) -0.003(2) 0.0062(19) 0.003(2) N4 0.031(3) 0.039(4) 0.023(3) 0.003(2) 0.016(2) 0.001(3) O1 0.048(3) 0.046(3) 0.062(3) 0.011(3) 0.034(3) 0.020(3) O2 0.034(3) 0.059(4) 0.072(4) 0.006(3) 0.038(3) 0.008(3) O3 0.072(4) 0.054(4) 0.032(3) 0.006(3) -0.012(3) -0.025(3) O4 0.050(3) 0.066(4) 0.019(2) -0.001(2) 0.007(2) -0.015(3) C1 0.020(3) 0.036(4) 0.017(2) -0.001(3) 0.011(2) 0.001(3) C2 0.035(4) 0.039(4) 0.027(3) 0.005(3) 0.016(3) 0.001(3) C3 0.030(3) 0.041(4) 0.033(3) 0.004(3) 0.014(3) 0.014(3) C4 0.022(3) 0.048(4) 0.037(3) 0.001(3) 0.016(3) 0.000(3) C5 0.026(3) 0.042(4) 0.024(3) -0.002(3) 0.012(3) -0.002(3) C6 0.015(3) 0.048(4) 0.016(3) -0.002(3) 0.005(2) -0.001(3) C7 0.020(3) 0.032(4) 0.015(3) 0.001(3) 0.005(2) -0.003(3) C8 0.022(3) 0.032(4) 0.026(3) 0.004(3) 0.008(3) -0.001(3) C9 0.033(4) 0.045(5) 0.026(3) 0.000(3) 0.011(3) -0.003(3) C10 0.067(5) 0.060(6) 0.041(4) 0.003(4) 0.035(4) -0.002(5) C11 0.053(5) 0.072(7) 0.078(6) -0.005(5) 0.051(5) -0.012(5) C12 0.031(4) 0.069(6) 0.066(5) -0.021(5) 0.026(4) -0.021(4) C13 0.029(3) 0.049(5) 0.037(4) -0.010(3) 0.011(3) -0.006(3) C14 0.020(3) 0.040(4) 0.026(3) -0.001(3) 0.007(3) 0.000(3) C15 0.026(3) 0.036(4) 0.048(4) 0.004(3) 0.017(3) -0.002(3) C16 0.037(4) 0.045(5) 0.061(5) 0.013(4) 0.023(4) 0.006(4) C17 0.050(5) 0.040(5) 0.092(7) 0.012(5) 0.033(5) -0.004(4) C18 0.049(5) 0.038(5) 0.148(10) -0.003(6) 0.055(6) 0.000(4) C19 0.075(7) 0.034(5) 0.117(9) 0.010(5) 0.055(7) 0.021(5) C20 0.029(4) 0.055(6) 0.098(7) 0.007(5) 0.040(5) 0.009(4) C21 0.017(3) 0.046(5) 0.046(4) 0.003(3) 0.014(3) 0.000(3) C22 0.039(4) 0.042(5) 0.077(6) 0.001(4) 0.033(4) 0.006(4) C23 0.038(4) 0.053(5) 0.065(5) -0.009(4) 0.033(4) 0.001(4) C24 0.029(3) 0.044(5) 0.045(4) -0.004(3) 0.020(3) -0.005(3) C25 0.018(3) 0.046(4) 0.028(3) -0.006(3) 0.007(3) -0.007(3) C26 0.018(3) 0.041(4) 0.027(3) 0.002(3) 0.007(3) 0.006(3) C27 0.013(3) 0.036(4) 0.022(3) 0.002(3) 0.002(2) -0.002(3) C56 0.124(9) 0.052(6) 0.129(9) 0.042(6) 0.098(8) 0.050(6) C55 0.047(5) 0.083(7) 0.089(7) 0.028(6) 0.050(5) 0.014(5) C28 0.021(3) 0.052(5) 0.019(3) -0.001(3) 0.009(2) -0.002(3) C29 0.027(3) 0.049(5) 0.021(3) 0.002(3) 0.003(3) -0.008(3) C30 0.031(4) 0.053(5) 0.020(3) 0.003(3) 0.000(3) -0.007(3) C31 0.030(3) 0.054(5) 0.013(3) 0.005(3) 0.005(2) 0.003(3) C32 0.037(4) 0.050(5) 0.017(3) 0.006(3) 0.014(3) 0.000(3) C33 0.026(3) 0.033(4) 0.019(3) 0.005(3) 0.011(2) 0.006(3) C34 0.029(3) 0.044(4) 0.018(3) 0.011(3) 0.013(3) 0.004(3) C35 0.042(4) 0.031(4) 0.022(3) 0.008(3) 0.019(3) 0.006(3) C36 0.027(3) 0.040(4) 0.024(3) 0.005(3) 0.010(3) 0.002(3) C37 0.044(4) 0.044(5) 0.029(3) 0.005(3) 0.024(3) 0.005(3) C38 0.059(5) 0.053(5) 0.021(3) 0.013(3) 0.024(3) 0.014(4) C39 0.062(5) 0.075(6) 0.033(4) 0.027(4) 0.025(4) 0.035(5) C40 0.042(4) 0.058(5) 0.036(4) 0.011(4) 0.023(3) 0.014(4) C41 0.027(3) 0.043(4) 0.025(3) -0.001(3) 0.016(3) 0.003(3) C42 0.034(4) 0.037(4) 0.031(3) -0.001(3) 0.018(3) 0.004(3) C43 0.054(5) 0.053(5) 0.044(4) -0.001(4) 0.028(4) 0.008(4) C44 0.080(6) 0.046(6) 0.059(5) 0.005(4) 0.042(5) 0.006(5) C45 0.088(7) 0.045(5) 0.063(5) -0.003(4) 0.049(5) 0.007(5) C46 0.048(4) 0.057(4) 0.034(3) 0.008(3) 0.004(3) 0.015(3) C47 0.029(3) 0.039(4) 0.031(3) -0.001(3) 0.012(3) 0.010(3) C48 0.024(3) 0.038(4) 0.040(4) -0.009(3) 0.015(3) -0.001(3) C49 0.026(3) 0.051(5) 0.031(3) -0.010(3) 0.010(3) 0.005(3) C50 0.033(4) 0.049(5) 0.028(3) -0.012(3) 0.013(3) 0.001(3) C51 0.024(3) 0.047(4) 0.021(3) -0.001(3) 0.006(3) 0.002(3) C52 0.031(3) 0.047(4) 0.017(3) -0.001(3) 0.010(3) 0.006(3) C53 0.026(3) 0.043(5) 0.023(3) 0.000(3) 0.013(3) 0.005(3) C54 0.024(3) 0.031(4) 0.021(3) 0.003(3) 0.011(2) 0.002(3) C57 0.032(4) 0.074(6) 0.018(3) 0.010(3) 0.001(3) -0.008(4) C58 0.117(14) 0.054(10) 0.032(7) -0.011(7) 0.015(8) -0.030(10) C60 0.027(9) 0.100(18) 0.027(9) -0.020(10) 0.000(7) -0.033(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Cl1 Ir1 Cl1 76.86(4) . 2_655 ? N1 Ir1 Cl1 102.44(13) . . ? N1 Ir1 Cl1 84.28(13) . 2_655 ? N1 Ir1 N3 169.77(18) . . ? N3 Ir1 Cl1 85.26(13) . . ? N3 Ir1 Cl1 104.22(13) . 2_655 ? C1 Ir1 Cl1 93.20(15) . 2_655 ? C1 Ir1 Cl1 169.39(16) . . ? C1 Ir1 N1 79.9(2) . . ? C1 Ir1 N3 93.7(2) . . ? C1 Ir1 C28 94.4(2) . . ? C28 Ir1 Cl1 95.85(16) . . ? C28 Ir1 Cl1 171.14(18) . 2_655 ? C28 Ir1 N1 92.5(2) . . ? C28 Ir1 N3 79.9(2) . . ? Ir1 Cl1 Ir1 103.13(4) . 2_655 ? C7 N1 Ir1 110.7(4) . . ? C7 N1 C27 106.4(5) . . ? C27 N1 Ir1 142.9(4) . . ? C7 N2 C8 123.3(5) . . ? C7 N2 C14 108.0(5) . . ? C14 N2 C8 128.6(6) . . ? C34 N3 Ir1 111.4(4) . . ? C34 N3 C54 104.9(5) . . ? C54 N3 Ir1 143.7(4) . . ? C34 N4 C35 124.9(5) . . ? C34 N4 C41 107.7(5) . . ? C41 N4 C35 127.4(6) . . ? C3 O1 C56 116.5(6) . . ? C4 O2 C55 117.7(6) . . ? C30 O3 C58 120.0(7) . . ? C30 O3 C60 104.3(9) . . ? C31 O4 C57 116.9(6) . . ? C2 C1 Ir1 127.0(5) . . ? C6 C1 Ir1 115.4(4) . . ? C6 C1 C2 117.4(5) . . ? C1 C2 H2 119.5 . . ? C3 C2 C1 121.0(6) . . ? C3 C2 H2 119.5 . . ? O1 C3 C2 125.1(7) . . ? O1 C3 C4 114.4(5) . . ? C2 C3 C4 120.5(6) . . ? O2 C4 C3 114.7(6) . . ? C5 C4 O2 126.0(6) . . ? C5 C4 C3 119.3(5) . . ? C4 C5 H5 119.9 . . ? C4 C5 C6 120.2(6) . . ? C6 C5 H5 119.9 . . ? C1 C6 C5 121.6(6) . . ? C1 C6 C7 111.5(5) . . ? C5 C6 C7 126.5(6) . . ? N1 C7 N2 110.3(5) . . ? N1 C7 C6 118.7(5) . . ? N2 C7 C6 130.2(5) . . ? C9 C8 N2 118.8(5) . . ? C9 C8 C13 120.6(6) . . ? C13 C8 N2 120.4(5) . . ? C8 C9 H9 120.4 . . ? C10 C9 C8 119.1(6) . . ? C10 C9 H9 120.4 . . ? C9 C10 H10 120.1 . . ? C11 C10 C9 119.9(7) . . ? C11 C10 H10 120.1 . . ? C10 C11 H11 119.7 . . ? C10 C11 C12 120.5(7) . . ? C12 C11 H11 119.7 . . ? C11 C12 H12 119.4 . . ? C13 C12 C11 121.1(7) . . ? C13 C12 H12 119.4 . . ? C8 C13 H13 120.7 . . ? C12 C13 C8 118.6(7) . . ? C12 C13 H13 120.7 . . ? N2 C14 C15 129.6(6) . . ? C27 C14 N2 106.4(6) . . ? C27 C14 C15 124.0(6) . . ? C14 C15 C20 115.9(6) . . ? C16 C15 C14 124.7(6) . . ? C16 C15 C20 119.4(7) . . ? C15 C16 H16 119.7 . . ? C15 C16 C17 120.6(7) . . ? C17 C16 H16 119.7 . . ? C16 C17 H17 120.0 . . ? C16 C17 C18 120.0(8) . . ? C18 C17 H17 120.0 . . ? C17 C18 H18 121.0 . . ? C19 C18 C17 118.1(9) . . ? C19 C18 H18 121.0 . . ? C18 C19 H19 116.6 . . ? C18 C19 C20 126.9(9) . . ? C20 C19 H19 116.6 . . ? C15 C20 C21 119.6(7) . . ? C19 C20 C15 114.7(7) . . ? C19 C20 C21 125.7(8) . . ? C22 C21 C20 119.4(7) . . ? C22 C21 C26 118.5(6) . . ? C26 C21 C20 122.0(6) . . ? C21 C22 H22 119.9 . . ? C23 C22 C21 120.2(7) . . ? C23 C22 H22 119.9 . . ? C22 C23 H23 119.5 . . ? C24 C23 C22 121.0(7) . . ? C24 C23 H23 119.5 . . ? C23 C24 H24 119.9 . . ? C25 C24 C23 120.1(7) . . ? C25 C24 H24 119.9 . . ? C24 C25 H25 119.6 . . ? C24 C25 C26 120.8(7) . . ? C26 C25 H25 119.6 . . ? C21 C26 C27 117.6(6) . . ? C25 C26 C21 119.2(6) . . ? C25 C26 C27 122.9(6) . . ? N1 C27 C26 130.4(6) . . ? C14 C27 N1 108.6(5) . . ? C14 C27 C26 120.4(6) . . ? O1 C56 H56A 109.5 . . ? O1 C56 H56B 109.5 . . ? O1 C56 H56C 109.5 . . ? H56A C56 H56B 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O2 C55 H55A 109.5 . . ? O2 C55 H55B 109.5 . . ? O2 C55 H55C 109.5 . . ? H55A C55 H55B 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C29 C28 Ir1 127.2(5) . . ? C29 C28 C33 118.0(5) . . ? C33 C28 Ir1 114.8(5) . . ? C28 C29 H29 119.5 . . ? C30 C29 C28 121.0(7) . . ? C30 C29 H29 119.5 . . ? O3 C30 C29 122.0(7) . . ? O3 C30 C31 117.2(6) . . ? C29 C30 C31 120.7(7) . . ? O4 C31 C30 116.1(6) . . ? C32 C31 O4 124.2(6) . . ? C32 C31 C30 119.7(5) . . ? C31 C32 H32 119.9 . . ? C31 C32 C33 120.2(6) . . ? C33 C32 H32 119.9 . . ? C28 C33 C32 120.3(6) . . ? C28 C33 C34 112.9(5) . . ? C32 C33 C34 126.0(6) . . ? N3 C34 C33 117.7(6) . . ? N4 C34 N3 112.2(6) . . ? N4 C34 C33 129.2(5) . . ? C36 C35 N4 118.7(6) . . ? C40 C35 N4 120.0(5) . . ? C40 C35 C36 121.3(5) . . ? C35 C36 H36 120.1 . . ? C37 C36 C35 119.7(6) . . ? C37 C36 H36 120.1 . . ? C36 C37 H37 120.0 . . ? C38 C37 C36 120.1(6) . . ? C38 C37 H37 120.0 . . ? C37 C38 H38 120.1 . . ? C37 C38 C39 119.9(6) . . ? C39 C38 H38 120.1 . . ? C38 C39 H39 119.9 . . ? C40 C39 C38 120.2(7) . . ? C40 C39 H39 119.9 . . ? C35 C40 C39 118.7(6) . . ? C35 C40 H40 120.6 . . ? C39 C40 H40 120.6 . . ? N4 C41 C42 129.5(6) . . ? C54 C41 N4 105.3(6) . . ? C54 C41 C42 125.1(6) . . ? C41 C42 C43 126.2(6) . . ? C47 C42 C41 115.5(6) . . ? C47 C42 C43 118.3(7) . . ? C42 C43 H43 118.8 . . ? C44 C43 C42 122.3(7) . . ? C44 C43 H43 118.8 . . ? C43 C44 H44 119.6 . . ? C43 C44 C45 120.8(8) . . ? C45 C44 H44 119.6 . . ? C44 C45 H45 120.3 . . ? C44 C45 C46 119.4(8) . . ? C46 C45 H45 120.3 . . ? C45 C46 H46 121.2 . . ? C47 C46 C45 117.6(7) . . ? C47 C46 H46 121.2 . . ? C42 C47 C46 121.3(7) . . ? C42 C47 C48 121.5(6) . . ? C46 C47 C48 117.0(6) . . ? C49 C48 C47 122.5(6) . . ? C53 C48 C47 119.9(6) . . ? C53 C48 C49 117.6(6) . . ? C48 C49 H49 118.9 . . ? C50 C49 C48 122.2(7) . . ? C50 C49 H49 118.9 . . ? C49 C50 H50 119.7 . . ? C49 C50 C51 120.5(6) . . ? C51 C50 H50 119.7 . . ? C50 C51 H51 120.4 . . ? C52 C51 C50 119.2(6) . . ? C52 C51 H51 120.4 . . ? C51 C52 H52 119.6 . . ? C51 C52 C53 120.7(7) . . ? C53 C52 H52 119.6 . . ? C48 C53 C52 119.6(6) . . ? C48 C53 C54 118.0(6) . . ? C52 C53 C54 122.4(6) . . ? N3 C54 C53 130.2(5) . . ? C41 C54 N3 109.8(5) . . ? C41 C54 C53 119.7(6) . . ? O4 C57 H57A 109.5 . . ? O4 C57 H57B 109.5 . . ? O4 C57 H57C 109.5 . . ? H57A C57 H57B 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? O3 C58 H58A 109.5 . . ? O3 C58 H58B 109.5 . . ? O3 C58 H58C 109.5 . . ? H58A C58 H58B 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? O3 C60 H60A 109.5 . . ? O3 C60 H60B 109.5 . . ? O3 C60 H60C 109.5 . . ? H60A C60 H60B 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 Cl1 2.5424(13) 2_655 ? Ir1 Cl1 2.5260(13) . ? Ir1 N1 2.071(5) . ? Ir1 N3 2.081(5) . ? Ir1 C1 1.988(5) . ? Ir1 C28 2.003(6) . ? N1 C7 1.350(7) . ? N1 C27 1.396(8) . ? N2 C7 1.360(8) . ? N2 C8 1.426(7) . ? N2 C14 1.387(8) . ? N3 C34 1.349(7) . ? N3 C54 1.412(8) . ? N4 C34 1.344(8) . ? N4 C35 1.436(7) . ? N4 C41 1.416(8) . ? O1 C3 1.372(8) . ? O1 C56 1.410(10) . ? O2 C4 1.380(7) . ? O2 C55 1.390(9) . ? O3 C30 1.365(9) . ? O3 C58 1.534(16) . ? O3 C60 1.641(19) . ? O4 C31 1.382(7) . ? O4 C57 1.409(9) . ? C1 C2 1.415(9) . ? C1 C6 1.400(9) . ? C2 H2 0.9500 . ? C2 C3 1.378(8) . ? C3 C4 1.421(10) . ? C4 C5 1.367(9) . ? C5 H5 0.9500 . ? C5 C6 1.406(8) . ? C6 C7 1.443(9) . ? C8 C9 1.393(8) . ? C8 C13 1.400(9) . ? C9 H9 0.9500 . ? C9 C10 1.389(9) . ? C10 H10 0.9500 . ? C10 C11 1.369(12) . ? C11 H11 0.9500 . ? C11 C12 1.379(11) . ? C12 H12 0.9500 . ? C12 C13 1.365(9) . ? C13 H13 0.9500 . ? C14 C15 1.442(10) . ? C14 C27 1.387(9) . ? C15 C16 1.387(10) . ? C15 C20 1.456(10) . ? C16 H16 0.9500 . ? C16 C17 1.392(12) . ? C17 H17 0.9500 . ? C17 C18 1.423(12) . ? C18 H18 0.9500 . ? C18 C19 1.289(12) . ? C19 H19 0.9500 . ? C19 C20 1.412(12) . ? C20 C21 1.459(10) . ? C21 C22 1.413(9) . ? C21 C26 1.415(10) . ? C22 H22 0.9500 . ? C22 C23 1.380(11) . ? C23 H23 0.9500 . ? C23 C24 1.378(10) . ? C24 H24 0.9500 . ? C24 C25 1.373(9) . ? C25 H25 0.9500 . ? C25 C26 1.406(9) . ? C26 C27 1.449(8) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C28 C29 1.402(9) . ? C28 C33 1.403(9) . ? C29 H29 0.9500 . ? C29 C30 1.383(8) . ? C30 C31 1.410(10) . ? C31 C32 1.350(10) . ? C32 H32 0.9500 . ? C32 C33 1.437(8) . ? C33 C34 1.447(9) . ? C35 C36 1.380(8) . ? C35 C40 1.375(9) . ? C36 H36 0.9500 . ? C36 C37 1.379(8) . ? C37 H37 0.9500 . ? C37 C38 1.372(10) . ? C38 H38 0.9500 . ? C38 C39 1.397(10) . ? C39 H39 0.9500 . ? C39 C40 1.387(9) . ? C40 H40 0.9500 . ? C41 C42 1.424(10) . ? C41 C54 1.382(8) . ? C42 C43 1.429(10) . ? C42 C47 1.395(8) . ? C43 H43 0.9500 . ? C43 C44 1.348(11) . ? C44 H44 0.9500 . ? C44 C45 1.412(11) . ? C45 H45 0.9500 . ? C45 C46 1.453(11) . ? C46 H46 0.9500 . ? C46 C47 1.433(11) . ? C47 C48 1.486(9) . ? C48 C49 1.419(9) . ? C48 C53 1.408(10) . ? C49 H49 0.9500 . ? C49 C50 1.346(10) . ? C50 H50 0.9500 . ? C50 C51 1.404(10) . ? C51 H51 0.9500 . ? C51 C52 1.383(8) . ? C52 H52 0.9500 . ? C52 C53 1.413(9) . ? C53 C54 1.438(8) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? 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 N1 C7 N2 174.8(4) . . . . ? Ir1 N1 C7 C6 -14.2(6) . . . . ? Ir1 N1 C27 C14 -176.4(5) . . . . ? Ir1 N1 C27 C26 12.7(10) . . . . ? Ir1 N3 C34 N4 174.8(4) . . . . ? Ir1 N3 C34 C33 -15.4(7) . . . . ? Ir1 N3 C54 C41 -174.3(5) . . . . ? Ir1 N3 C54 C53 12.1(11) . . . . ? Ir1 C1 C2 C3 174.3(5) . . . . ? Ir1 C1 C6 C5 -173.3(4) . . . . ? Ir1 C1 C6 C7 13.4(6) . . . . ? Ir1 C28 C29 C30 178.2(5) . . . . ? Ir1 C28 C33 C32 -178.3(5) . . . . ? Ir1 C28 C33 C34 10.9(7) . . . . ? N2 C8 C9 C10 -173.6(7) . . . . ? N2 C8 C13 C12 174.7(7) . . . . ? N2 C14 C15 C16 9.2(11) . . . . ? N2 C14 C15 C20 -169.8(7) . . . . ? N2 C14 C27 N1 -2.0(6) . . . . ? N2 C14 C27 C26 169.9(5) . . . . ? N4 C35 C36 C37 -174.9(6) . . . . ? N4 C35 C40 C39 176.5(7) . . . . ? N4 C41 C42 C43 7.9(11) . . . . ? N4 C41 C42 C47 -172.5(6) . . . . ? N4 C41 C54 N3 -1.8(6) . . . . ? N4 C41 C54 C53 172.6(5) . . . . ? O1 C3 C4 O2 0.7(9) . . . . ? O1 C3 C4 C5 -178.5(6) . . . . ? O2 C4 C5 C6 179.5(6) . . . . ? O3 C30 C31 O4 -1.6(9) . . . . ? O3 C30 C31 C32 178.3(6) . . . . ? O4 C31 C32 C33 -178.3(6) . . . . ? C1 C2 C3 O1 -180.0(6) . . . . ? C1 C2 C3 C4 -1.4(10) . . . . ? C1 C6 C7 N1 1.2(7) . . . . ? C1 C6 C7 N2 170.2(6) . . . . ? C2 C1 C6 C5 2.7(8) . . . . ? C2 C1 C6 C7 -170.5(5) . . . . ? C2 C3 C4 O2 -178.0(6) . . . . ? C2 C3 C4 C5 2.8(10) . . . . ? C3 C4 C5 C6 -1.4(10) . . . . ? C4 C5 C6 C1 -1.4(9) . . . . ? C4 C5 C6 C7 170.7(6) . . . . ? C5 C6 C7 N1 -171.6(5) . . . . ? C5 C6 C7 N2 -2.7(10) . . . . ? C6 C1 C2 C3 -1.3(9) . . . . ? C7 N1 C27 C14 5.0(6) . . . . ? C7 N1 C27 C26 -165.8(6) . . . . ? C7 N2 C8 C9 78.1(8) . . . . ? C7 N2 C8 C13 -96.9(8) . . . . ? C7 N2 C14 C15 175.4(6) . . . . ? C7 N2 C14 C27 -1.7(6) . . . . ? C8 N2 C7 N1 -179.3(5) . . . . ? C8 N2 C7 C6 11.1(9) . . . . ? C8 N2 C14 C15 -0.1(10) . . . . ? C8 N2 C14 C27 -177.1(5) . . . . ? C8 C9 C10 C11 0.0(12) . . . . ? C9 C8 C13 C12 -0.2(11) . . . . ? C9 C10 C11 C12 -2.6(14) . . . . ? C10 C11 C12 C13 3.9(14) . . . . ? C11 C12 C13 C8 -2.4(13) . . . . ? C13 C8 C9 C10 1.4(11) . . . . ? C14 N2 C7 N1 5.0(6) . . . . ? C14 N2 C7 C6 -164.7(6) . . . . ? C14 N2 C8 C9 -107.1(8) . . . . ? C14 N2 C8 C13 77.9(8) . . . . ? C14 C15 C16 C17 -175.6(7) . . . . ? C14 C15 C20 C19 177.1(8) . . . . ? C14 C15 C20 C21 -1.1(11) . . . . ? C15 C14 C27 N1 -179.3(6) . . . . ? C15 C14 C27 C26 -7.4(9) . . . . ? C15 C16 C17 C18 -0.1(13) . . . . ? C15 C20 C21 C22 176.5(7) . . . . ? C15 C20 C21 C26 -3.9(11) . . . . ? C16 C15 C20 C19 -2.0(12) . . . . ? C16 C15 C20 C21 179.8(7) . . . . ? C16 C17 C18 C19 -4.7(15) . . . . ? C17 C18 C19 C20 6.5(18) . . . . ? C18 C19 C20 C15 -3.2(16) . . . . ? C18 C19 C20 C21 174.9(10) . . . . ? C19 C20 C21 C22 -1.4(13) . . . . ? C19 C20 C21 C26 178.2(9) . . . . ? C20 C15 C16 C17 3.4(12) . . . . ? C20 C21 C22 C23 -178.7(8) . . . . ? C20 C21 C26 C25 177.6(6) . . . . ? C20 C21 C26 C27 3.5(10) . . . . ? C21 C22 C23 C24 1.0(12) . . . . ? C21 C26 C27 N1 171.9(6) . . . . ? C21 C26 C27 C14 2.0(9) . . . . ? C22 C21 C26 C25 -2.8(10) . . . . ? C22 C21 C26 C27 -176.9(6) . . . . ? C22 C23 C24 C25 -2.6(12) . . . . ? C23 C24 C25 C26 1.4(10) . . . . ? C24 C25 C26 C21 1.3(9) . . . . ? C24 C25 C26 C27 175.1(6) . . . . ? C25 C26 C27 N1 -2.0(10) . . . . ? C25 C26 C27 C14 -171.9(6) . . . . ? C26 C21 C22 C23 1.7(11) . . . . ? C27 N1 C7 N2 -6.1(6) . . . . ? C27 N1 C7 C6 164.8(5) . . . . ? C27 C14 C15 C16 -174.2(7) . . . . ? C27 C14 C15 C20 6.8(10) . . . . ? C56 O1 C3 C2 1.4(11) . . . . ? C56 O1 C3 C4 -177.2(8) . . . . ? C55 O2 C4 C3 -176.4(7) . . . . ? C55 O2 C4 C5 2.7(11) . . . . ? C28 C29 C30 O3 -179.2(6) . . . . ? C28 C29 C30 C31 0.6(10) . . . . ? C28 C33 C34 N3 3.5(8) . . . . ? C28 C33 C34 N4 171.4(6) . . . . ? C29 C28 C33 C32 0.0(9) . . . . ? C29 C28 C33 C34 -170.8(5) . . . . ? C29 C30 C31 O4 178.5(6) . . . . ? C29 C30 C31 C32 -1.6(10) . . . . ? C30 C31 C32 C33 1.7(10) . . . . ? C31 C32 C33 C28 -0.9(9) . . . . ? C31 C32 C33 C34 168.5(6) . . . . ? C32 C33 C34 N3 -166.6(6) . . . . ? C32 C33 C34 N4 1.3(10) . . . . ? C33 C28 C29 C30 0.1(9) . . . . ? C34 N3 C54 C41 3.3(6) . . . . ? C34 N3 C54 C53 -170.3(6) . . . . ? C34 N4 C35 C36 76.0(8) . . . . ? C34 N4 C35 C40 -100.7(8) . . . . ? C34 N4 C41 C42 177.5(6) . . . . ? C34 N4 C41 C54 -0.5(6) . . . . ? C35 N4 C34 N3 -175.1(5) . . . . ? C35 N4 C34 C33 16.5(10) . . . . ? C35 N4 C41 C42 -4.7(10) . . . . ? C35 N4 C41 C54 177.3(6) . . . . ? C35 C36 C37 C38 -3.2(11) . . . . ? C36 C35 C40 C39 0.0(12) . . . . ? C36 C37 C38 C39 3.0(12) . . . . ? C37 C38 C39 C40 -1.3(13) . . . . ? C38 C39 C40 C35 -0.2(13) . . . . ? C40 C35 C36 C37 1.6(11) . . . . ? C41 N4 C34 N3 2.7(7) . . . . ? C41 N4 C34 C33 -165.6(6) . . . . ? C41 N4 C35 C36 -101.5(8) . . . . ? C41 N4 C35 C40 81.9(9) . . . . ? C41 C42 C43 C44 -178.3(8) . . . . ? C41 C42 C47 C46 -179.3(6) . . . . ? C41 C42 C47 C48 -4.3(9) . . . . ? C42 C41 C54 N3 -179.9(6) . . . . ? C42 C41 C54 C53 -5.5(9) . . . . ? C42 C43 C44 C45 -0.7(14) . . . . ? C42 C47 C48 C49 -179.0(6) . . . . ? C42 C47 C48 C53 4.2(9) . . . . ? C43 C42 C47 C46 0.4(10) . . . . ? C43 C42 C47 C48 175.4(6) . . . . ? C43 C44 C45 C46 -3.1(14) . . . . ? C44 C45 C46 C47 5.3(12) . . . . ? C45 C46 C47 C42 -4.0(11) . . . . ? C45 C46 C47 C48 -179.2(7) . . . . ? C46 C47 C48 C49 -3.8(9) . . . . ? C46 C47 C48 C53 179.3(6) . . . . ? C47 C42 C43 C44 2.1(11) . . . . ? C47 C48 C49 C50 -175.5(6) . . . . ? C47 C48 C53 C52 173.3(6) . . . . ? C47 C48 C53 C54 -4.2(9) . . . . ? C48 C49 C50 C51 2.2(10) . . . . ? C48 C53 C54 N3 177.8(6) . . . . ? C48 C53 C54 C41 4.8(9) . . . . ? C49 C48 C53 C52 -3.8(9) . . . . ? C49 C48 C53 C54 178.8(6) . . . . ? C49 C50 C51 C52 -3.3(10) . . . . ? C50 C51 C52 C53 0.9(9) . . . . ? C51 C52 C53 C48 2.7(9) . . . . ? C51 C52 C53 C54 180.0(6) . . . . ? C52 C53 C54 N3 0.5(10) . . . . ? C52 C53 C54 C41 -172.6(6) . . . . ? C53 C48 C49 C50 1.4(9) . . . . ? C54 N3 C34 N4 -3.7(7) . . . . ? C54 N3 C34 C33 166.1(5) . . . . ? C54 C41 C42 C43 -174.5(7) . . . . ? C54 C41 C42 C47 5.1(9) . . . . ? C57 O4 C31 C30 -154.2(6) . . . . ? C57 O4 C31 C32 25.9(9) . . . . ? C58 O3 C30 C29 34.0(13) . . . . ? C58 O3 C30 C31 -145.9(10) . . . . ? C60 O3 C30 C29 -95.1(10) . . . . ? C60 O3 C30 C31 85.0(10) . . . . ? 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 -0.788 -0.109 -0.991 3159.8 1597.7 '40 CH2Cl2'