#------------------------------------------------------------------------------ #$Date: 2023-11-01 04:30:49 +0200 (Wed, 01 Nov 2023) $ #$Revision: 287190 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/76/7247611.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_7247611 loop_ _publ_author_name 'Chen, Yi-Sheng' 'Chiu, Siang-Yu' 'Li, Chia-Ying' 'Chen, Tsun-Ren' 'Chen, Jhy-Der' _publ_section_title ; Ligand effect of cyclometallated iridium(iii) complexes on N-alkylation of amines in hydrogen borrowing reactions ; _journal_issue 45 _journal_name_full 'RSC Advances' _journal_page_first 31948 _journal_page_last 31961 _journal_paper_doi 10.1039/D3RA07184G _journal_volume 13 _journal_year 2023 _chemical_formula_sum 'C49 H41 Cl5 Ir N2 O5 P' _chemical_formula_weight 1138.26 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2017/1 _audit_update_record ; 2023-09-30 deposited with the CCDC. 2023-10-24 downloaded from the CCDC. ; _cell_angle_alpha 86.17(5) _cell_angle_beta 69.00(5) _cell_angle_gamma 88.19(5) _cell_formula_units_Z 2 _cell_length_a 12.34(2) _cell_length_b 12.49(2) _cell_length_c 16.46(4) _cell_measurement_reflns_used 9338 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.16 _cell_measurement_theta_min 2.17 _cell_volume 2363(8) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0775 _diffrn_reflns_av_unetI/netI 0.0645 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 9296 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.998 _diffrn_reflns_theta_min 1.327 _exptl_absorpt_coefficient_mu 3.189 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.3092 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS, 2008)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.599 _exptl_crystal_description block _exptl_crystal_F_000 1132 _exptl_crystal_size_max 0.800 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _refine_diff_density_max 3.449 _refine_diff_density_min -1.869 _refine_diff_density_rms 0.166 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 563 _refine_ls_number_reflns 9296 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.060 _refine_ls_R_factor_all 0.0804 _refine_ls_R_factor_gt 0.0526 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0244P)^2^+8.1232P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1074 _refine_ls_wR_factor_ref 0.1246 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7178 _reflns_number_total 9296 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ra07184g2.cif _cod_data_source_block 12670_0m_tw _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'multi_scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas ; _cod_original_cell_volume 2364(8) _cod_database_code 7247611 _shelx_shelxl_version_number 2017/1 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.185 _shelx_estimated_absorpt_t_max 0.568 _shelx_res_file ; TITL 12670_0m_a.res in P-1 12670_0m_tw.res created by SHELXL-2017/1 at 14:44:34 on 06-Nov-2022 CELL 0.71073 12.3441 12.4886 16.4621 86.168 69.000 88.187 ZERR 2.00 0.0216 0.0220 0.0351 0.054 0.052 0.049 LATT 1 SFAC C H N O P CL IR UNIT 98 82 4 10 2 10 2 TEMP 20.000 SIZE 0.200 0.300 0.800 ACTA L.S. 8 FMAP 2 PLAN -5 0 0.00 BOND $H CONF eadp C1 C2 WGHT 0.024400 8.123203 BASF 0.49836 FVAR 4.46493 IR 7 0.511041 0.736264 0.720458 11.00000 0.03846 0.03521 = 0.03421 -0.00837 -0.00985 0.00169 CL1 6 0.560947 0.551278 0.756919 11.00000 0.04984 0.03114 = 0.05473 -0.01004 -0.02169 0.00673 P1 5 0.314974 0.703835 0.822025 11.00000 0.03319 0.03430 = 0.02818 -0.00662 -0.00956 0.00459 O1 4 0.565133 0.951891 0.882450 11.00000 0.07322 0.03517 = 0.04744 -0.01163 -0.03029 0.00402 O2 4 0.591529 0.650926 0.467256 11.00000 0.05967 0.05498 = 0.03024 -0.00968 -0.00365 0.00327 O3 4 -0.081658 0.972220 0.787762 11.00000 0.08422 0.17139 = 0.10062 -0.01327 -0.03872 0.08232 O4 4 0.125078 0.256726 0.857155 11.00000 0.06539 0.05228 = 0.06779 -0.01565 -0.00779 -0.01911 O5 4 0.327213 0.788937 1.175024 11.00000 0.10405 0.04227 = 0.04104 -0.00777 -0.03858 0.00982 N1 3 0.556067 0.802420 0.817585 11.00000 0.02084 0.03773 = 0.04143 -0.00767 -0.00881 0.00328 N2 3 0.495390 0.689698 0.605516 11.00000 0.02487 0.04617 = 0.03094 -0.00877 -0.00220 0.00784 C1 1 0.482030 0.894906 0.693587 11.00000 0.05126 0.03923 = 0.02926 -0.00889 -0.00626 -0.00982 C2 1 0.447812 0.942501 0.628189 11.00000 0.05126 0.03923 = 0.02926 -0.00889 -0.00626 -0.00982 AFIX 43 H2A 2 0.437896 0.900930 0.586598 11.00000 -1.20000 AFIX 0 C3 1 0.428311 1.052724 0.624895 11.00000 0.07959 0.04738 = 0.04998 0.00869 -0.02528 0.00734 AFIX 43 H3A 2 0.405701 1.084195 0.580592 11.00000 -1.20000 AFIX 0 C4 1 0.441924 1.117157 0.686617 11.00000 0.09260 0.03453 = 0.06259 0.00204 -0.02579 0.00465 AFIX 43 H4A 2 0.426029 1.190331 0.684000 11.00000 -1.20000 AFIX 0 C5 1 0.478452 1.073502 0.750898 11.00000 0.08935 0.03369 = 0.05245 -0.00056 -0.02871 0.00007 AFIX 43 H5A 2 0.488563 1.116498 0.791591 11.00000 -1.20000 AFIX 0 C6 1 0.500503 0.962228 0.754395 11.00000 0.05160 0.03496 = 0.03877 -0.00008 -0.01366 0.00319 C7 1 0.539344 0.905736 0.817845 11.00000 0.04463 0.03690 = 0.03213 -0.00310 -0.00873 0.00022 C8 1 0.598436 0.773729 0.883985 11.00000 0.03456 0.04292 = 0.03789 -0.00444 -0.01954 0.00243 C9 1 0.633504 0.677176 0.912226 11.00000 0.05564 0.04775 = 0.06761 -0.00748 -0.03530 0.00158 AFIX 43 H9A 2 0.632710 0.614114 0.885432 11.00000 -1.20000 AFIX 0 C10 1 0.670438 0.678485 0.983259 11.00000 0.07572 0.04806 = 0.08852 0.00618 -0.05474 -0.00050 AFIX 43 H10A 2 0.696998 0.614881 1.002643 11.00000 -1.20000 AFIX 0 C11 1 0.668931 0.771049 1.025841 11.00000 0.07830 0.06876 = 0.06785 0.00385 -0.05013 -0.00457 AFIX 43 H11A 2 0.691193 0.767524 1.074279 11.00000 -1.20000 AFIX 0 C12 1 0.634805 0.868406 0.997266 11.00000 0.08765 0.04995 = 0.05193 -0.01049 -0.04264 -0.00286 AFIX 43 H12A 2 0.633733 0.931548 1.024473 11.00000 -1.20000 AFIX 0 C13 1 0.602230 0.865168 0.925005 11.00000 0.04757 0.03684 = 0.05538 -0.00395 -0.02507 -0.00345 C14 1 0.682922 0.752091 0.636306 11.00000 0.05253 0.03445 = 0.04883 -0.02145 -0.02645 0.01984 C15 1 0.778992 0.784514 0.656504 11.00000 0.04186 0.08600 = 0.05844 -0.01386 -0.01340 -0.00987 AFIX 43 H15A 2 0.769224 0.805181 0.711949 11.00000 -1.20000 AFIX 0 C16 1 0.886769 0.784572 0.592033 11.00000 0.04088 0.11491 = 0.09595 -0.02339 -0.01112 -0.02463 AFIX 43 H16A 2 0.949146 0.811745 0.602994 11.00000 -1.20000 AFIX 0 C17 1 0.905643 0.745825 0.511798 11.00000 0.03969 0.14129 = 0.08964 -0.03319 0.01065 -0.01267 AFIX 43 H17A 2 0.980382 0.743156 0.470595 11.00000 -1.20000 AFIX 0 C18 1 0.811847 0.710546 0.492661 11.00000 0.05620 0.10044 = 0.05149 -0.02267 0.00984 -0.00882 AFIX 43 H18A 2 0.822958 0.685375 0.438317 11.00000 -1.20000 AFIX 0 C19 1 0.703156 0.713614 0.555256 11.00000 0.03192 0.06107 = 0.05358 -0.01190 -0.00233 -0.00604 C20 1 0.597607 0.682148 0.542693 11.00000 0.04456 0.04517 = 0.02712 -0.00514 -0.00362 0.00351 C21 1 0.413655 0.663637 0.567907 11.00000 0.04431 0.03682 = 0.02242 -0.00593 -0.01396 0.00407 C22 1 0.295027 0.660095 0.599471 11.00000 0.05298 0.07437 = 0.03444 -0.00665 -0.01612 -0.00324 AFIX 43 H22A 2 0.251869 0.679991 0.655441 11.00000 -1.20000 AFIX 0 C23 1 0.240899 0.625274 0.544146 11.00000 0.05636 0.09496 = 0.05308 -0.00508 -0.02985 -0.00347 AFIX 43 H23A 2 0.160358 0.621846 0.564120 11.00000 -1.20000 AFIX 0 C24 1 0.304948 0.595698 0.459970 11.00000 0.09268 0.07572 = 0.04958 -0.00697 -0.04187 -0.00679 AFIX 43 H24A 2 0.266628 0.572422 0.425040 11.00000 -1.20000 AFIX 0 C25 1 0.422720 0.600525 0.428449 11.00000 0.08327 0.04428 = 0.03623 -0.00909 -0.02144 -0.00130 AFIX 43 H25A 2 0.466234 0.580793 0.372501 11.00000 -1.20000 AFIX 0 C26 1 0.475293 0.636143 0.483285 11.00000 0.05500 0.03718 = 0.03641 -0.00638 -0.01683 0.00173 C27 1 0.192924 0.785770 0.811381 11.00000 0.04254 0.05267 = 0.02410 -0.00691 -0.01123 0.00890 C28 1 0.206362 0.896938 0.796368 11.00000 0.05513 0.06029 = 0.03825 -0.00187 -0.01090 0.01655 AFIX 43 H28A 2 0.275983 0.927845 0.791905 11.00000 -1.20000 AFIX 0 C29 1 0.117170 0.961568 0.788065 11.00000 0.06805 0.07830 = 0.05686 0.00252 -0.02041 0.03801 AFIX 43 H29A 2 0.127413 1.035342 0.777668 11.00000 -1.20000 AFIX 0 C30 1 0.011783 0.916149 0.795279 11.00000 0.06989 0.11202 = 0.05274 -0.01430 -0.02280 0.05244 C31 1 -0.063096 1.080972 0.753745 11.00000 0.15674 0.19591 = 0.09683 -0.00767 -0.05203 0.13029 AFIX 33 H31A 2 -0.134472 1.111498 0.751648 11.00000 -1.50000 H31B 2 -0.036757 1.121295 0.790666 11.00000 -1.50000 H31C 2 -0.005572 1.083279 0.696041 11.00000 -1.50000 AFIX 0 C32 1 -0.003742 0.806835 0.811257 11.00000 0.05030 0.12906 = 0.06564 -0.02221 -0.03110 0.02793 AFIX 43 H32A 2 -0.074182 0.776893 0.816611 11.00000 -1.20000 AFIX 0 C33 1 0.085411 0.741042 0.819420 11.00000 0.04584 0.08272 = 0.05322 -0.01941 -0.02185 0.01686 AFIX 43 H33A 2 0.074254 0.667403 0.830199 11.00000 -1.20000 AFIX 0 C34 1 0.257820 0.566548 0.835398 11.00000 0.03158 0.04336 = 0.03243 -0.00933 -0.00894 0.00233 C35 1 0.172616 0.528385 0.913140 11.00000 0.03492 0.04806 = 0.03157 -0.00911 -0.00800 0.00256 AFIX 43 H35A 2 0.146182 0.572539 0.959745 11.00000 -1.20000 AFIX 0 C36 1 0.125967 0.425346 0.922718 11.00000 0.03270 0.05673 = 0.03979 -0.00321 -0.00674 -0.00602 AFIX 43 H36A 2 0.070140 0.401466 0.975342 11.00000 -1.20000 AFIX 0 C37 1 0.163392 0.359418 0.853521 11.00000 0.04264 0.04830 = 0.04819 -0.00549 -0.01430 -0.00454 C38 1 0.036289 0.216647 0.935121 11.00000 0.10142 0.07318 = 0.09911 -0.01639 0.01742 -0.04510 AFIX 33 H38A 2 0.018221 0.144311 0.928434 11.00000 -1.50000 H38B 2 0.062911 0.217829 0.983156 11.00000 -1.50000 H38C 2 -0.031946 0.260861 0.946182 11.00000 -1.50000 AFIX 0 C39 1 0.247200 0.396282 0.775996 11.00000 0.04749 0.04622 = 0.04565 -0.01669 -0.01078 -0.00333 AFIX 43 H39A 2 0.272170 0.352726 0.728968 11.00000 -1.20000 AFIX 0 C40 1 0.294472 0.497994 0.767775 11.00000 0.03765 0.04803 = 0.03081 -0.00515 -0.00438 0.00077 AFIX 43 H40A 2 0.352077 0.520446 0.715588 11.00000 -1.20000 AFIX 0 C41 1 0.310642 0.726236 0.933119 11.00000 0.02566 0.03136 = 0.03610 -0.00761 -0.00628 0.01072 C42 1 0.276057 0.824618 0.971061 11.00000 0.05214 0.03412 = 0.03684 -0.00189 -0.01911 0.00451 AFIX 43 H42A 2 0.248479 0.878905 0.941905 11.00000 -1.20000 AFIX 0 C43 1 0.282347 0.842151 1.051275 11.00000 0.07158 0.02451 = 0.04563 -0.00480 -0.02500 0.00207 AFIX 43 H43A 2 0.258526 0.907986 1.075407 11.00000 -1.20000 AFIX 0 C44 1 0.323458 0.763457 1.096225 11.00000 0.06049 0.03613 = 0.03008 -0.00148 -0.01421 -0.00002 C45 1 0.359708 0.665982 1.059377 11.00000 0.05270 0.02856 = 0.04380 -0.00247 -0.02246 0.00390 AFIX 43 H45A 2 0.387942 0.612071 1.088418 11.00000 -1.20000 AFIX 0 C46 1 0.353376 0.649726 0.978503 11.00000 0.04496 0.03010 = 0.04138 -0.00744 -0.01567 0.00727 AFIX 43 H46A 2 0.379055 0.584448 0.953897 11.00000 -1.20000 AFIX 0 C47 1 0.360592 0.706434 1.225824 11.00000 0.12461 0.05604 = 0.05073 0.00016 -0.05208 0.00161 AFIX 33 H47A 2 0.359728 0.734463 1.278953 11.00000 -1.50000 H47B 2 0.307153 0.647962 1.239266 11.00000 -1.50000 H47C 2 0.437353 0.681365 1.193433 11.00000 -1.50000 AFIX 0 C48 1 0.249888 0.951990 0.460614 11.00000 0.21601 0.21984 = 0.08733 0.02454 -0.04837 -0.11458 AFIX 23 H48A 2 0.257396 1.026993 0.440086 11.00000 -1.20000 H48B 2 0.327662 0.924154 0.450214 11.00000 -1.20000 AFIX 0 CL2 6 0.196904 0.889997 0.400969 11.00000 0.18973 0.26581 = 0.14104 -0.08303 -0.05246 -0.05401 CL3 6 0.177907 0.946584 0.569714 11.00000 0.14487 0.18670 = 0.08862 -0.02147 -0.04060 -0.00928 C49 1 1.115485 0.465424 0.277050 11.00000 0.09319 0.15094 = 0.17404 -0.01629 -0.04697 0.02411 AFIX 23 H49A 2 1.198440 0.460076 0.264357 11.00000 -1.20000 H49B 2 1.083818 0.393963 0.295092 11.00000 -1.20000 AFIX 0 CL4 6 1.056738 0.545288 0.362401 11.00000 0.11622 0.34532 = 0.27183 -0.19214 -0.03353 0.01823 CL5 6 1.093630 0.506204 0.183963 11.00000 0.16764 0.20913 = 0.20572 0.01516 -0.10535 -0.02275 HKLF 5 REM 12670_0m_a.res in P-1 REM R1 = 0.0526 for 7178 Fo > 4sig(Fo) and 0.0804 for all 9296 data REM 563 parameters refined using 0 restraints END WGHT 0.0243 8.1223 REM Highest difference peak 3.449, deepest hole -1.869, 1-sigma level 0.166 Q1 1 0.4670 0.7864 0.8411 11.00000 0.05 3.45 Q2 1 0.4971 0.7338 0.6737 11.00000 0.05 2.42 Q3 1 0.5163 0.7417 0.7719 11.00000 0.05 2.31 Q4 1 0.4722 0.6760 0.7373 11.00000 0.05 1.44 Q5 1 0.4658 0.9187 0.6805 11.00000 0.05 1.31 ; _shelx_res_checksum 89896 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ir Ir 0.51104(3) 0.73626(2) 0.72046(2) 0.03656(10) Uani 1 1 d . . . . . Cl1 Cl 0.56095(17) 0.55128(14) 0.75692(12) 0.0442(4) Uani 1 1 d . . . . . P1 P 0.31497(15) 0.70383(14) 0.82203(11) 0.0322(4) Uani 1 1 d . . . . . O1 O 0.5651(5) 0.9519(4) 0.8824(3) 0.0492(13) Uani 1 1 d . . . . . O2 O 0.5915(5) 0.6509(4) 0.4673(3) 0.0514(14) Uani 1 1 d . . . . . O3 O -0.0817(7) 0.9722(9) 0.7878(6) 0.119(3) Uani 1 1 d . . . . . O4 O 0.1251(5) 0.2567(5) 0.8572(4) 0.0652(17) Uani 1 1 d . . . . . O5 O 0.3272(6) 0.7889(4) 1.1750(3) 0.0590(16) Uani 1 1 d . . . . . N1 N 0.5561(4) 0.8024(5) 0.8176(4) 0.0338(13) Uani 1 1 d . . . . . N2 N 0.4954(5) 0.6897(5) 0.6055(3) 0.0360(13) Uani 1 1 d . . . . . C1 C 0.4820(7) 0.8949(6) 0.6936(4) 0.0416(12) Uani 1 1 d . . . . . C2 C 0.4478(7) 0.9425(6) 0.6282(4) 0.0416(12) Uani 1 1 d . . . . . H2A H 0.437896 0.900930 0.586598 0.050 Uiso 1 1 calc R U . . . C3 C 0.4283(8) 1.0527(7) 0.6249(6) 0.059(2) Uani 1 1 d . . . . . H3A H 0.405701 1.084195 0.580592 0.071 Uiso 1 1 calc R U . . . C4 C 0.4419(9) 1.1172(7) 0.6866(6) 0.064(3) Uani 1 1 d . . . . . H4A H 0.426029 1.190331 0.684000 0.077 Uiso 1 1 calc R U . . . C5 C 0.4785(8) 1.0735(6) 0.7509(5) 0.058(2) Uani 1 1 d . . . . . H5A H 0.488563 1.116498 0.791591 0.069 Uiso 1 1 calc R U . . . C6 C 0.5005(7) 0.9622(6) 0.7544(5) 0.0426(18) Uani 1 1 d . . . . . C7 C 0.5393(6) 0.9057(6) 0.8178(4) 0.0392(17) Uani 1 1 d . . . . . C8 C 0.5984(6) 0.7737(6) 0.8840(4) 0.0366(16) Uani 1 1 d . . . . . C9 C 0.6335(7) 0.6772(7) 0.9122(6) 0.053(2) Uani 1 1 d . . . . . H9A H 0.632710 0.614114 0.885432 0.064 Uiso 1 1 calc R U . . . C10 C 0.6704(8) 0.6785(7) 0.9833(6) 0.064(3) Uani 1 1 d . . . . . H10A H 0.696998 0.614881 1.002643 0.077 Uiso 1 1 calc R U . . . C11 C 0.6689(8) 0.7710(8) 1.0258(6) 0.065(3) Uani 1 1 d . . . . . H11A H 0.691193 0.767524 1.074279 0.078 Uiso 1 1 calc R U . . . C12 C 0.6348(8) 0.8684(7) 0.9973(5) 0.058(2) Uani 1 1 d . . . . . H12A H 0.633733 0.931548 1.024473 0.069 Uiso 1 1 calc R U . . . C13 C 0.6022(7) 0.8652(6) 0.9250(5) 0.0446(18) Uani 1 1 d . . . . . C14 C 0.6829(7) 0.7521(6) 0.6363(5) 0.0425(18) Uani 1 1 d . . . . . C15 C 0.7790(7) 0.7845(8) 0.6565(6) 0.063(2) Uani 1 1 d . . . . . H15A H 0.769224 0.805181 0.711949 0.075 Uiso 1 1 calc R U . . . C16 C 0.8868(8) 0.7846(10) 0.5920(8) 0.086(4) Uani 1 1 d . . . . . H16A H 0.949146 0.811745 0.602994 0.103 Uiso 1 1 calc R U . . . C17 C 0.9056(9) 0.7458(11) 0.5118(8) 0.098(4) Uani 1 1 d . . . . . H17A H 0.980382 0.743156 0.470595 0.118 Uiso 1 1 calc R U . . . C18 C 0.8118(8) 0.7105(9) 0.4927(6) 0.076(3) Uani 1 1 d . . . . . H18A H 0.822958 0.685375 0.438317 0.092 Uiso 1 1 calc R U . . . C19 C 0.7032(7) 0.7136(7) 0.5553(5) 0.052(2) Uani 1 1 d . . . . . C20 C 0.5976(6) 0.6821(6) 0.5427(4) 0.0414(17) Uani 1 1 d . . . . . C21 C 0.4137(6) 0.6636(5) 0.5679(4) 0.0339(15) Uani 1 1 d . . . . . C22 C 0.2950(7) 0.6601(7) 0.5995(5) 0.054(2) Uani 1 1 d . . . . . H22A H 0.251869 0.679991 0.655441 0.064 Uiso 1 1 calc R U . . . C23 C 0.2409(8) 0.6253(8) 0.5441(6) 0.065(3) Uani 1 1 d . . . . . H23A H 0.160358 0.621846 0.564120 0.078 Uiso 1 1 calc R U . . . C24 C 0.3049(10) 0.5957(8) 0.4600(6) 0.068(3) Uani 1 1 d . . . . . H24A H 0.266628 0.572422 0.425040 0.081 Uiso 1 1 calc R U . . . C25 C 0.4227(9) 0.6005(6) 0.4284(5) 0.054(2) Uani 1 1 d . . . . . H25A H 0.466234 0.580793 0.372501 0.065 Uiso 1 1 calc R U . . . C26 C 0.4753(7) 0.6361(6) 0.4833(5) 0.0426(18) Uani 1 1 d . . . . . C27 C 0.1929(6) 0.7858(6) 0.8114(4) 0.0399(17) Uani 1 1 d . . . . . C28 C 0.2064(8) 0.8969(7) 0.7964(5) 0.053(2) Uani 1 1 d . . . . . H28A H 0.275983 0.927845 0.791905 0.064 Uiso 1 1 calc R U . . . C29 C 0.1172(9) 0.9616(8) 0.7881(6) 0.069(3) Uani 1 1 d . . . . . H29A H 0.127413 1.035342 0.777668 0.083 Uiso 1 1 calc R U . . . C30 C 0.0118(10) 0.9161(11) 0.7953(6) 0.079(3) Uani 1 1 d . . . . . C31 C -0.0631(13) 1.0810(14) 0.7537(9) 0.151(8) Uani 1 1 d . . . . . H31A H -0.134472 1.111498 0.751648 0.227 Uiso 1 1 calc R U . . . H31B H -0.036757 1.121295 0.790666 0.227 Uiso 1 1 calc R U . . . H31C H -0.005572 1.083279 0.696041 0.227 Uiso 1 1 calc R U . . . C32 C -0.0037(8) 0.8068(11) 0.8113(6) 0.079(3) Uani 1 1 d . . . . . H32A H -0.074182 0.776893 0.816611 0.094 Uiso 1 1 calc R U . . . C33 C 0.0854(7) 0.7410(8) 0.8194(5) 0.059(2) Uani 1 1 d . . . . . H33A H 0.074254 0.667403 0.830199 0.071 Uiso 1 1 calc R U . . . C34 C 0.2578(6) 0.5665(6) 0.8354(4) 0.0362(16) Uani 1 1 d . . . . . C35 C 0.1726(6) 0.5284(6) 0.9131(4) 0.0390(17) Uani 1 1 d . . . . . H35A H 0.146182 0.572539 0.959745 0.047 Uiso 1 1 calc R U . . . C36 C 0.1260(6) 0.4253(6) 0.9227(5) 0.0446(18) Uani 1 1 d . . . . . H36A H 0.070140 0.401466 0.975342 0.054 Uiso 1 1 calc R U . . . C37 C 0.1634(7) 0.3594(6) 0.8535(5) 0.0467(19) Uani 1 1 d . . . . . C38 C 0.0363(11) 0.2166(9) 0.9351(8) 0.104(5) Uani 1 1 d . . . . . H38A H 0.018221 0.144311 0.928434 0.156 Uiso 1 1 calc R U . . . H38B H 0.062911 0.217829 0.983156 0.156 Uiso 1 1 calc R U . . . H38C H -0.031946 0.260861 0.946182 0.156 Uiso 1 1 calc R U . . . C39 C 0.2472(7) 0.3963(6) 0.7760(5) 0.0473(19) Uani 1 1 d . . . . . H39A H 0.272170 0.352726 0.728968 0.057 Uiso 1 1 calc R U . . . C40 C 0.2945(6) 0.4980(6) 0.7678(4) 0.0409(17) Uani 1 1 d . . . . . H40A H 0.352077 0.520446 0.715588 0.049 Uiso 1 1 calc R U . . . C41 C 0.3106(5) 0.7262(5) 0.9331(4) 0.0323(15) Uani 1 1 d . . . . . C42 C 0.2761(7) 0.8246(6) 0.9711(4) 0.0403(17) Uani 1 1 d . . . . . H42A H 0.248479 0.878905 0.941905 0.048 Uiso 1 1 calc R U . . . C43 C 0.2823(7) 0.8422(6) 1.0513(5) 0.0461(19) Uani 1 1 d . . . . . H43A H 0.258526 0.907986 1.075407 0.055 Uiso 1 1 calc R U . . . C44 C 0.3235(7) 0.7635(6) 1.0962(4) 0.0428(18) Uani 1 1 d . . . . . C45 C 0.3597(7) 0.6660(5) 1.0594(5) 0.0403(17) Uani 1 1 d . . . . . H45A H 0.387942 0.612071 1.088418 0.048 Uiso 1 1 calc R U . . . C46 C 0.3534(6) 0.6497(6) 0.9785(5) 0.0387(16) Uani 1 1 d . . . . . H46A H 0.379055 0.584448 0.953897 0.046 Uiso 1 1 calc R U . . . C47 C 0.3606(10) 0.7064(7) 1.2258(6) 0.072(3) Uani 1 1 d . . . . . H47A H 0.359728 0.734463 1.278953 0.107 Uiso 1 1 calc R U . . . H47B H 0.307153 0.647962 1.239266 0.107 Uiso 1 1 calc R U . . . H47C H 0.437353 0.681365 1.193433 0.107 Uiso 1 1 calc R U . . . C48 C 0.2499(17) 0.9520(16) 0.4606(9) 0.175(9) Uani 1 1 d . . . . . H48A H 0.257396 1.026993 0.440086 0.210 Uiso 1 1 calc R U . . . H48B H 0.327662 0.924154 0.450214 0.210 Uiso 1 1 calc R U . . . Cl2 Cl 0.1969(5) 0.8900(5) 0.4010(3) 0.196(3) Uani 1 1 d . . . . . Cl3 Cl 0.1779(4) 0.9466(4) 0.5697(2) 0.1396(15) Uani 1 1 d . . . . . C49 C 1.1155(13) 0.4654(14) 0.2770(11) 0.140(6) Uani 1 1 d . . . . . H49A H 1.198440 0.460076 0.264357 0.168 Uiso 1 1 calc R U . . . H49B H 1.083818 0.393963 0.295092 0.168 Uiso 1 1 calc R U . . . Cl4 Cl 1.0567(5) 0.5453(7) 0.3624(5) 0.246(4) Uani 1 1 d . . . . . Cl5 Cl 1.0936(5) 0.5062(5) 0.1840(4) 0.184(2) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir 0.03846(17) 0.03521(16) 0.03421(15) -0.00837(11) -0.00985(12) 0.00169(11) Cl1 0.0498(11) 0.0311(9) 0.0547(11) -0.0100(8) -0.0217(9) 0.0067(8) P1 0.0332(10) 0.0343(10) 0.0282(9) -0.0066(7) -0.0096(7) 0.0046(8) O1 0.073(4) 0.035(3) 0.047(3) -0.012(2) -0.030(3) 0.004(3) O2 0.060(4) 0.055(3) 0.030(3) -0.010(2) -0.004(2) 0.003(3) O3 0.084(6) 0.171(9) 0.101(6) -0.013(6) -0.039(5) 0.082(6) O4 0.065(4) 0.052(4) 0.068(4) -0.016(3) -0.008(3) -0.019(3) O5 0.104(5) 0.042(3) 0.041(3) -0.008(2) -0.039(3) 0.010(3) N1 0.021(3) 0.038(3) 0.041(3) -0.008(3) -0.009(2) 0.003(2) N2 0.025(3) 0.046(4) 0.031(3) -0.009(3) -0.002(2) 0.008(3) C1 0.051(3) 0.039(3) 0.029(2) -0.009(2) -0.006(2) -0.010(2) C2 0.051(3) 0.039(3) 0.029(2) -0.009(2) -0.006(2) -0.010(2) C3 0.080(6) 0.047(5) 0.050(5) 0.009(4) -0.025(5) 0.007(5) C4 0.093(7) 0.035(5) 0.063(6) 0.002(4) -0.026(5) 0.005(5) C5 0.089(7) 0.034(4) 0.052(5) -0.001(4) -0.029(5) 0.000(4) C6 0.052(5) 0.035(4) 0.039(4) 0.000(3) -0.014(4) 0.003(3) C7 0.045(4) 0.037(4) 0.032(4) -0.003(3) -0.009(3) 0.000(3) C8 0.035(4) 0.043(4) 0.038(4) -0.004(3) -0.020(3) 0.002(3) C9 0.056(5) 0.048(5) 0.068(5) -0.007(4) -0.035(4) 0.002(4) C10 0.076(7) 0.048(5) 0.089(7) 0.006(5) -0.055(6) -0.001(5) C11 0.078(7) 0.069(6) 0.068(6) 0.004(5) -0.050(5) -0.005(5) C12 0.088(7) 0.050(5) 0.052(5) -0.010(4) -0.043(5) -0.003(5) C13 0.048(5) 0.037(4) 0.055(5) -0.004(3) -0.025(4) -0.003(3) C14 0.053(5) 0.034(4) 0.049(4) -0.021(3) -0.026(4) 0.020(3) C15 0.042(5) 0.086(7) 0.058(5) -0.014(5) -0.013(4) -0.010(5) C16 0.041(6) 0.115(10) 0.096(8) -0.023(7) -0.011(5) -0.025(6) C17 0.040(6) 0.141(12) 0.090(8) -0.033(8) 0.011(5) -0.013(6) C18 0.056(6) 0.100(8) 0.051(5) -0.023(5) 0.010(5) -0.009(6) C19 0.032(4) 0.061(5) 0.054(5) -0.012(4) -0.002(4) -0.006(4) C20 0.045(4) 0.045(4) 0.027(4) -0.005(3) -0.004(3) 0.004(3) C21 0.044(4) 0.037(4) 0.022(3) -0.006(3) -0.014(3) 0.004(3) C22 0.053(5) 0.074(6) 0.034(4) -0.007(4) -0.016(4) -0.003(4) C23 0.056(6) 0.095(7) 0.053(5) -0.005(5) -0.030(5) -0.003(5) C24 0.093(8) 0.076(7) 0.050(5) -0.007(5) -0.042(5) -0.007(6) C25 0.083(7) 0.044(5) 0.036(4) -0.009(3) -0.021(4) -0.001(4) C26 0.055(5) 0.037(4) 0.036(4) -0.006(3) -0.017(4) 0.002(4) C27 0.043(4) 0.053(5) 0.024(3) -0.007(3) -0.011(3) 0.009(4) C28 0.055(5) 0.060(5) 0.038(4) -0.002(4) -0.011(4) 0.017(4) C29 0.068(7) 0.078(7) 0.057(5) 0.003(5) -0.020(5) 0.038(5) C30 0.070(7) 0.112(9) 0.053(6) -0.014(6) -0.023(5) 0.052(7) C31 0.157(14) 0.196(17) 0.097(10) -0.008(10) -0.052(10) 0.130(13) C32 0.050(6) 0.129(11) 0.066(6) -0.022(7) -0.031(5) 0.028(6) C33 0.046(5) 0.083(7) 0.053(5) -0.019(5) -0.022(4) 0.017(5) C34 0.032(4) 0.043(4) 0.032(4) -0.009(3) -0.009(3) 0.002(3) C35 0.035(4) 0.048(4) 0.032(4) -0.009(3) -0.008(3) 0.003(3) C36 0.033(4) 0.057(5) 0.040(4) -0.003(4) -0.007(3) -0.006(4) C37 0.043(4) 0.048(5) 0.048(4) -0.005(4) -0.014(4) -0.005(4) C38 0.101(9) 0.073(8) 0.099(9) -0.016(6) 0.017(7) -0.045(7) C39 0.047(5) 0.046(5) 0.046(4) -0.017(4) -0.011(4) -0.003(4) C40 0.038(4) 0.048(4) 0.031(4) -0.005(3) -0.004(3) 0.001(3) C41 0.026(3) 0.031(4) 0.036(4) -0.008(3) -0.006(3) 0.011(3) C42 0.052(5) 0.034(4) 0.037(4) -0.002(3) -0.019(3) 0.005(3) C43 0.072(6) 0.025(4) 0.046(4) -0.005(3) -0.025(4) 0.002(4) C44 0.060(5) 0.036(4) 0.030(4) -0.001(3) -0.014(3) 0.000(4) C45 0.053(5) 0.029(4) 0.044(4) -0.002(3) -0.022(4) 0.004(3) C46 0.045(4) 0.030(4) 0.041(4) -0.007(3) -0.016(3) 0.007(3) C47 0.125(9) 0.056(6) 0.051(5) 0.000(4) -0.052(6) 0.002(6) C48 0.22(2) 0.22(2) 0.087(10) 0.025(12) -0.048(12) -0.115(17) Cl2 0.190(5) 0.266(7) 0.141(4) -0.083(4) -0.052(4) -0.054(5) Cl3 0.145(4) 0.187(4) 0.089(2) -0.021(3) -0.041(2) -0.009(3) C49 0.093(11) 0.151(15) 0.174(16) -0.016(13) -0.047(11) 0.024(10) Cl4 0.116(4) 0.345(10) 0.272(8) -0.192(7) -0.034(4) 0.018(5) Cl5 0.168(5) 0.209(6) 0.206(6) 0.015(5) -0.105(4) -0.023(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' P P 0.1023 0.0942 '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' 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 C1 Ir C14 89.6(3) . . ? C1 Ir N2 92.8(3) . . ? C14 Ir N2 80.2(3) . . ? C1 Ir N1 81.3(3) . . ? C14 Ir N1 89.1(3) . . ? N2 Ir N1 167.8(2) . . ? C1 Ir P1 94.8(2) . . ? C14 Ir P1 175.5(2) . . ? N2 Ir P1 100.2(2) . . ? N1 Ir P1 90.9(2) . . ? C1 Ir Cl1 174.6(2) . . ? C14 Ir Cl1 87.3(2) . . ? N2 Ir Cl1 91.10(19) . . ? N1 Ir Cl1 94.14(19) . . ? P1 Ir Cl1 88.17(11) . . ? C34 P1 C27 102.0(4) . . ? C34 P1 C41 102.1(3) . . ? C27 P1 C41 104.1(3) . . ? C34 P1 Ir 118.0(2) . . ? C27 P1 Ir 120.1(3) . . ? C41 P1 Ir 108.4(2) . . ? C7 O1 C13 104.0(6) . . ? C20 O2 C26 105.9(5) . . ? C30 O3 C31 117.3(11) . . ? C37 O4 C38 118.6(7) . . ? C44 O5 C47 117.8(6) . . ? C7 N1 C8 106.9(6) . . ? C7 N1 Ir 111.4(5) . . ? C8 N1 Ir 141.6(5) . . ? C20 N2 C21 105.3(6) . . ? C20 N2 Ir 111.6(5) . . ? C21 N2 Ir 143.2(4) . . ? C2 C1 C6 118.4(7) . . ? C2 C1 Ir 129.8(5) . . ? C6 C1 Ir 111.8(5) . . ? C1 C2 C3 119.8(7) . . ? C1 C2 H2A 120.1 . . ? C3 C2 H2A 120.1 . . ? C2 C3 C4 121.5(8) . . ? C2 C3 H3A 119.3 . . ? C4 C3 H3A 119.3 . . ? C5 C4 C3 120.5(8) . . ? C5 C4 H4A 119.8 . . ? C3 C4 H4A 119.8 . . ? C4 C5 C6 118.8(8) . . ? C4 C5 H5A 120.6 . . ? C6 C5 H5A 120.6 . . ? C5 C6 C1 121.0(7) . . ? C5 C6 C7 124.9(7) . . ? C1 C6 C7 114.1(7) . . ? N1 C7 O1 113.2(6) . . ? N1 C7 C6 121.2(7) . . ? O1 C7 C6 125.6(7) . . ? C13 C8 C9 119.6(7) . . ? C13 C8 N1 107.7(6) . . ? C9 C8 N1 132.6(7) . . ? C8 C9 C10 116.8(8) . . ? C8 C9 H9A 121.6 . . ? C10 C9 H9A 121.6 . . ? C11 C10 C9 122.5(8) . . ? C11 C10 H10A 118.7 . . ? C9 C10 H10A 118.7 . . ? C12 C11 C10 120.9(8) . . ? C12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C11 C12 C13 115.2(8) . . ? C11 C12 H12A 122.4 . . ? C13 C12 H12A 122.4 . . ? C8 C13 C12 124.9(7) . . ? C8 C13 O1 108.1(6) . . ? C12 C13 O1 127.0(7) . . ? C19 C14 C15 118.7(7) . . ? C19 C14 Ir 113.3(6) . . ? C15 C14 Ir 127.5(6) . . ? C16 C15 C14 118.2(9) . . ? C16 C15 H15A 120.9 . . ? C14 C15 H15A 120.9 . . ? C15 C16 C17 122.2(9) . . ? C15 C16 H16A 118.9 . . ? C17 C16 H16A 118.9 . . ? C16 C17 C18 119.5(9) . . ? C16 C17 H17A 120.2 . . ? C18 C17 H17A 120.2 . . ? C19 C18 C17 118.9(9) . . ? C19 C18 H18A 120.6 . . ? C17 C18 H18A 120.6 . . ? C18 C19 C14 122.3(8) . . ? C18 C19 C20 124.3(8) . . ? C14 C19 C20 113.4(7) . . ? N2 C20 O2 113.5(7) . . ? N2 C20 C19 120.8(7) . . ? O2 C20 C19 125.5(6) . . ? C22 C21 C26 119.8(7) . . ? C22 C21 N2 132.7(6) . . ? C26 C21 N2 107.5(6) . . ? C21 C22 C23 117.5(7) . . ? C21 C22 H22A 121.3 . . ? C23 C22 H22A 121.3 . . ? C24 C23 C22 121.6(9) . . ? C24 C23 H23A 119.2 . . ? C22 C23 H23A 119.2 . . ? C25 C24 C23 120.7(8) . . ? C25 C24 H24A 119.6 . . ? C23 C24 H24A 119.6 . . ? C24 C25 C26 117.2(8) . . ? C24 C25 H25A 121.4 . . ? C26 C25 H25A 121.4 . . ? O2 C26 C21 107.8(6) . . ? O2 C26 C25 129.0(7) . . ? C21 C26 C25 123.1(8) . . ? C28 C27 C33 118.5(8) . . ? C28 C27 P1 118.8(6) . . ? C33 C27 P1 122.8(6) . . ? C29 C28 C27 120.8(9) . . ? C29 C28 H28A 119.6 . . ? C27 C28 H28A 119.6 . . ? C28 C29 C30 120.2(10) . . ? C28 C29 H29A 119.9 . . ? C30 C29 H29A 119.9 . . ? O3 C30 C32 115.0(12) . . ? O3 C30 C29 125.0(12) . . ? C32 C30 C29 120.0(9) . . ? O3 C31 H31A 109.5 . . ? O3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 C33 120.4(10) . . ? C30 C32 H32A 119.8 . . ? C33 C32 H32A 119.8 . . ? C32 C33 C27 120.3(10) . . ? C32 C33 H33A 119.9 . . ? C27 C33 H33A 119.9 . . ? C40 C34 C35 117.1(7) . . ? C40 C34 P1 121.4(5) . . ? C35 C34 P1 121.5(5) . . ? C34 C35 C36 121.8(7) . . ? C34 C35 H35A 119.1 . . ? C36 C35 H35A 119.1 . . ? C37 C36 C35 119.7(7) . . ? C37 C36 H36A 120.2 . . ? C35 C36 H36A 120.2 . . ? O4 C37 C36 124.0(7) . . ? O4 C37 C39 116.8(7) . . ? C36 C37 C39 119.2(7) . . ? O4 C38 H38A 109.5 . . ? O4 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O4 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 C40 120.6(7) . . ? C37 C39 H39A 119.7 . . ? C40 C39 H39A 119.7 . . ? C34 C40 C39 121.6(7) . . ? C34 C40 H40A 119.2 . . ? C39 C40 H40A 119.2 . . ? C46 C41 C42 116.9(6) . . ? C46 C41 P1 120.8(5) . . ? C42 C41 P1 122.0(5) . . ? C43 C42 C41 120.9(7) . . ? C43 C42 H42A 119.6 . . ? C41 C42 H42A 119.6 . . ? C42 C43 C44 121.1(7) . . ? C42 C43 H43A 119.4 . . ? C44 C43 H43A 119.4 . . ? O5 C44 C43 116.7(7) . . ? O5 C44 C45 124.3(7) . . ? C43 C44 C45 119.0(7) . . ? C44 C45 C46 119.2(7) . . ? C44 C45 H45A 120.4 . . ? C46 C45 H45A 120.4 . . ? C41 C46 C45 122.9(7) . . ? C41 C46 H46A 118.6 . . ? C45 C46 H46A 118.6 . . ? O5 C47 H47A 109.5 . . ? O5 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? O5 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? Cl2 C48 Cl3 118.6(10) . . ? Cl2 C48 H48A 107.7 . . ? Cl3 C48 H48A 107.7 . . ? Cl2 C48 H48B 107.7 . . ? Cl3 C48 H48B 107.7 . . ? H48A C48 H48B 107.1 . . ? Cl5 C49 Cl4 115.9(10) . . ? Cl5 C49 H49A 108.3 . . ? Cl4 C49 H49A 108.3 . . ? Cl5 C49 H49B 108.3 . . ? Cl4 C49 H49B 108.3 . . ? H49A C49 H49B 107.4 . . ? 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 Ir C1 2.050(8) . ? Ir C14 2.084(9) . ? Ir N2 2.091(7) . ? Ir N1 2.095(6) . ? Ir P1 2.427(4) . ? Ir Cl1 2.463(4) . ? P1 C34 1.844(8) . ? P1 C27 1.848(8) . ? P1 C41 1.850(8) . ? O1 C7 1.379(9) . ? O1 C13 1.404(9) . ? O2 C20 1.354(9) . ? O2 C26 1.379(10) . ? O3 C30 1.370(11) . ? O3 C31 1.427(18) . ? O4 C37 1.371(10) . ? O4 C38 1.428(11) . ? O5 C44 1.373(9) . ? O5 C47 1.427(10) . ? N1 C7 1.300(9) . ? N1 C8 1.394(9) . ? N2 C20 1.319(9) . ? N2 C21 1.415(9) . ? C1 C2 1.384(11) . ? C1 C6 1.431(10) . ? C2 C3 1.391(11) . ? C2 H2A 0.9300 . ? C3 C4 1.396(12) . ? C3 H3A 0.9300 . ? C4 C5 1.367(12) . ? C4 H4A 0.9300 . ? C5 C6 1.409(11) . ? C5 H5A 0.9300 . ? C6 C7 1.434(10) . ? C8 C13 1.375(10) . ? C8 C9 1.376(11) . ? C9 C10 1.400(12) . ? C9 H9A 0.9300 . ? C10 C11 1.388(13) . ? C10 H10A 0.9300 . ? C11 C12 1.382(12) . ? C11 H11A 0.9300 . ? C12 C13 1.389(11) . ? C12 H12A 0.9300 . ? C14 C19 1.383(11) . ? C14 C15 1.418(11) . ? C15 C16 1.373(13) . ? C15 H15A 0.9300 . ? C16 C17 1.375(15) . ? C16 H16A 0.9300 . ? C17 C18 1.395(15) . ? C17 H17A 0.9300 . ? C18 C19 1.369(11) . ? C18 H18A 0.9300 . ? C19 C20 1.460(11) . ? C21 C22 1.368(11) . ? C21 C26 1.388(10) . ? C22 C23 1.404(11) . ? C22 H22A 0.9300 . ? C23 C24 1.395(13) . ? C23 H23A 0.9300 . ? C24 C25 1.359(13) . ? C24 H24A 0.9300 . ? C25 C26 1.388(11) . ? C25 H25A 0.9300 . ? C27 C28 1.398(11) . ? C27 C33 1.415(12) . ? C28 C29 1.385(11) . ? C28 H28A 0.9300 . ? C29 C30 1.398(16) . ? C29 H29A 0.9300 . ? C30 C32 1.379(16) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 C33 1.392(12) . ? C32 H32A 0.9300 . ? C33 H33A 0.9300 . ? C34 C40 1.385(10) . ? C34 C35 1.399(10) . ? C35 C36 1.403(11) . ? C35 H35A 0.9300 . ? C36 C37 1.383(11) . ? C36 H36A 0.9300 . ? C37 C39 1.384(11) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C40 1.393(11) . ? C39 H39A 0.9300 . ? C40 H40A 0.9300 . ? C41 C46 1.380(9) . ? C41 C42 1.400(9) . ? C42 C43 1.382(10) . ? C42 H42A 0.9300 . ? C43 C44 1.383(10) . ? C43 H43A 0.9300 . ? C44 C45 1.386(10) . ? C45 C46 1.390(10) . ? C45 H45A 0.9300 . ? C46 H46A 0.9300 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 Cl2 1.608(16) . ? C48 Cl3 1.692(15) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 Cl5 1.692(17) . ? C49 Cl4 1.705(17) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? 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 C6 C1 C2 C3 -2.3(11) . . . . ? Ir C1 C2 C3 177.1(6) . . . . ? C1 C2 C3 C4 -0.3(13) . . . . ? C2 C3 C4 C5 2.0(15) . . . . ? C3 C4 C5 C6 -0.9(14) . . . . ? C4 C5 C6 C1 -1.8(13) . . . . ? C4 C5 C6 C7 179.8(8) . . . . ? C2 C1 C6 C5 3.4(12) . . . . ? Ir C1 C6 C5 -176.1(6) . . . . ? C2 C1 C6 C7 -178.1(7) . . . . ? Ir C1 C6 C7 2.4(8) . . . . ? C8 N1 C7 O1 -1.4(8) . . . . ? Ir N1 C7 O1 178.4(4) . . . . ? C8 N1 C7 C6 177.2(7) . . . . ? Ir N1 C7 C6 -3.0(9) . . . . ? C13 O1 C7 N1 0.4(8) . . . . ? C13 O1 C7 C6 -178.1(7) . . . . ? C5 C6 C7 N1 178.9(8) . . . . ? C1 C6 C7 N1 0.4(11) . . . . ? C5 C6 C7 O1 -2.7(13) . . . . ? C1 C6 C7 O1 178.9(7) . . . . ? C7 N1 C8 C13 1.9(8) . . . . ? Ir N1 C8 C13 -177.8(6) . . . . ? C7 N1 C8 C9 -178.3(8) . . . . ? Ir N1 C8 C9 2.0(14) . . . . ? C13 C8 C9 C10 0.7(12) . . . . ? N1 C8 C9 C10 -179.2(8) . . . . ? C8 C9 C10 C11 2.0(14) . . . . ? C9 C10 C11 C12 -2.7(16) . . . . ? C10 C11 C12 C13 0.6(14) . . . . ? C9 C8 C13 C12 -2.9(13) . . . . ? N1 C8 C13 C12 176.9(8) . . . . ? C9 C8 C13 O1 178.5(7) . . . . ? N1 C8 C13 O1 -1.6(8) . . . . ? C11 C12 C13 C8 2.3(14) . . . . ? C11 C12 C13 O1 -179.4(8) . . . . ? C7 O1 C13 C8 0.8(8) . . . . ? C7 O1 C13 C12 -177.7(8) . . . . ? C19 C14 C15 C16 5.3(14) . . . . ? Ir C14 C15 C16 176.8(8) . . . . ? C14 C15 C16 C17 -5.7(18) . . . . ? C15 C16 C17 C18 4(2) . . . . ? C16 C17 C18 C19 -1.2(19) . . . . ? C17 C18 C19 C14 1.1(16) . . . . ? C17 C18 C19 C20 178.1(10) . . . . ? C15 C14 C19 C18 -3.1(14) . . . . ? Ir C14 C19 C18 -175.8(8) . . . . ? C15 C14 C19 C20 179.5(8) . . . . ? Ir C14 C19 C20 6.9(9) . . . . ? C21 N2 C20 O2 -1.5(8) . . . . ? Ir N2 C20 O2 179.3(5) . . . . ? C21 N2 C20 C19 174.1(7) . . . . ? Ir N2 C20 C19 -5.2(9) . . . . ? C26 O2 C20 N2 -0.6(8) . . . . ? C26 O2 C20 C19 -175.9(8) . . . . ? C18 C19 C20 N2 -178.4(9) . . . . ? C14 C19 C20 N2 -1.1(11) . . . . ? C18 C19 C20 O2 -3.4(14) . . . . ? C14 C19 C20 O2 173.9(7) . . . . ? C20 N2 C21 C22 -178.1(8) . . . . ? Ir N2 C21 C22 0.7(14) . . . . ? C20 N2 C21 C26 3.0(8) . . . . ? Ir N2 C21 C26 -178.2(6) . . . . ? C26 C21 C22 C23 1.7(12) . . . . ? N2 C21 C22 C23 -177.1(8) . . . . ? C21 C22 C23 C24 -0.3(14) . . . . ? C22 C23 C24 C25 -0.5(15) . . . . ? C23 C24 C25 C26 -0.2(14) . . . . ? C20 O2 C26 C21 2.5(8) . . . . ? C20 O2 C26 C25 -177.4(8) . . . . ? C22 C21 C26 O2 177.5(7) . . . . ? N2 C21 C26 O2 -3.4(8) . . . . ? C22 C21 C26 C25 -2.6(12) . . . . ? N2 C21 C26 C25 176.5(7) . . . . ? C24 C25 C26 O2 -178.4(8) . . . . ? C24 C25 C26 C21 1.7(12) . . . . ? C34 P1 C27 C28 -177.4(5) . . . . ? C41 P1 C27 C28 76.7(6) . . . . ? Ir P1 C27 C28 -44.7(6) . . . . ? C34 P1 C27 C33 3.8(7) . . . . ? C41 P1 C27 C33 -102.1(6) . . . . ? Ir P1 C27 C33 136.5(5) . . . . ? C33 C27 C28 C29 -1.1(11) . . . . ? P1 C27 C28 C29 -179.9(6) . . . . ? C27 C28 C29 C30 0.5(13) . . . . ? C31 O3 C30 C32 -167.4(10) . . . . ? C31 O3 C30 C29 12.7(15) . . . . ? C28 C29 C30 O3 -179.7(9) . . . . ? C28 C29 C30 C32 0.4(14) . . . . ? O3 C30 C32 C33 179.4(8) . . . . ? C29 C30 C32 C33 -0.6(15) . . . . ? C30 C32 C33 C27 0.0(14) . . . . ? C28 C27 C33 C32 0.9(11) . . . . ? P1 C27 C33 C32 179.6(6) . . . . ? C27 P1 C34 C40 104.2(6) . . . . ? C41 P1 C34 C40 -148.4(6) . . . . ? Ir P1 C34 C40 -29.8(7) . . . . ? C27 P1 C34 C35 -73.5(6) . . . . ? C41 P1 C34 C35 33.9(7) . . . . ? Ir P1 C34 C35 152.6(5) . . . . ? C40 C34 C35 C36 0.0(11) . . . . ? P1 C34 C35 C36 177.8(6) . . . . ? C34 C35 C36 C37 -0.9(11) . . . . ? C38 O4 C37 C36 3.8(13) . . . . ? C38 O4 C37 C39 -178.3(9) . . . . ? C35 C36 C37 O4 178.4(7) . . . . ? C35 C36 C37 C39 0.5(12) . . . . ? O4 C37 C39 C40 -177.3(7) . . . . ? C36 C37 C39 C40 0.7(12) . . . . ? C35 C34 C40 C39 1.2(11) . . . . ? P1 C34 C40 C39 -176.6(6) . . . . ? C37 C39 C40 C34 -1.6(12) . . . . ? C34 P1 C41 C46 47.3(7) . . . . ? C27 P1 C41 C46 153.2(6) . . . . ? Ir P1 C41 C46 -77.9(6) . . . . ? C34 P1 C41 C42 -139.6(6) . . . . ? C27 P1 C41 C42 -33.7(7) . . . . ? Ir P1 C41 C42 95.2(6) . . . . ? C46 C41 C42 C43 -1.5(11) . . . . ? P1 C41 C42 C43 -174.8(6) . . . . ? C41 C42 C43 C44 0.3(12) . . . . ? C47 O5 C44 C43 175.2(8) . . . . ? C47 O5 C44 C45 -6.0(12) . . . . ? C42 C43 C44 O5 179.5(7) . . . . ? C42 C43 C44 C45 0.6(12) . . . . ? O5 C44 C45 C46 -179.1(7) . . . . ? C43 C44 C45 C46 -0.3(12) . . . . ? C42 C41 C46 C45 1.9(11) . . . . ? P1 C41 C46 C45 175.2(6) . . . . ? C44 C45 C46 C41 -1.0(12) . . . . ?