#------------------------------------------------------------------------------ #$Date: 2021-07-05 20:29:19 +0300 (Mon, 05 Jul 2021) $ #$Revision: 267145 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/75/7707515.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_7707515 loop_ _publ_author_name 'Cheung, Wai-Man' 'Chong, Man-Chun' 'Sung, Herman H.-Y.' 'Cheng, Shun-Cheung' 'Williams, Ian D.' 'Ko, Chi-Chiu' 'Leung, Wa-Hung' _publ_section_title ; Synthesis, structure and reactivity of iridium complexes containing a bis-cyclometalated tridentate C^N^C ligand. ; _journal_issue 24 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 8512 _journal_page_last 8523 _journal_paper_doi 10.1039/d1dt01269j _journal_volume 50 _journal_year 2021 _chemical_formula_moiety 'C54 H43 Cl Ir P3, 0.5(C H2 Cl2)' _chemical_formula_sum 'C54.5 H44 Cl2 Ir P3' _chemical_formula_weight 1054.90 _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 _atom_sites_solution_primary iterative _audit_creation_date 2019-02-28 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _audit_update_record ; 2021-03-25 deposited with the CCDC. 2021-05-27 downloaded from the CCDC. ; _cell_angle_alpha 76.851(3) _cell_angle_beta 88.011(3) _cell_angle_gamma 69.189(4) _cell_formula_units_Z 2 _cell_length_a 10.7955(5) _cell_length_b 12.1139(4) _cell_length_c 18.5808(6) _cell_measurement_reflns_used 7939 _cell_measurement_temperature 118(20) _cell_measurement_theta_max 73.3220 _cell_measurement_theta_min 3.9970 _cell_volume 2208.99(16) _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve (Bourhis et al., 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 118(20) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.3577 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.942 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 32.00 138.00 1.00 3.00 -- 106.99 -30.00 150.00 106 2 \w -69.00 31.00 1.00 2.00 -- -40.57 57.00-120.00 100 3 \w -74.00 26.00 1.00 2.00 -- -40.57 77.00 0.00 100 4 \w -66.00 36.00 1.00 2.00 -- -40.57 37.00 150.00 102 5 \w 29.00 138.00 1.00 3.00 -- 106.99 -30.00 0.00 109 6 \w 28.00 139.00 1.00 3.00 -- 106.99 -77.00 150.00 111 7 \w 73.00 154.00 1.00 3.00 -- 106.99 77.00 -30.00 81 8 \w 94.00 177.00 1.00 3.00 -- 106.99 125.00 150.00 83 9 \w 32.00 117.00 1.00 3.00 -- 106.99-125.00 0.00 85 10 \w 46.00 109.00 1.00 3.00 -- 106.99 -94.00 90.00 63 ; _diffrn_measurement_device 'kappa diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.1404361000 _diffrn_orient_matrix_UB_12 0.0034120000 _diffrn_orient_matrix_UB_13 -0.0162797000 _diffrn_orient_matrix_UB_21 -0.0235246000 _diffrn_orient_matrix_UB_22 -0.0221913000 _diffrn_orient_matrix_UB_23 0.0834642000 _diffrn_orient_matrix_UB_31 -0.0555924000 _diffrn_orient_matrix_UB_32 0.1379934000 _diffrn_orient_matrix_UB_33 -0.0060686000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_unetI/netI 0.0430 _diffrn_reflns_Laue_measured_fraction_full 0.984 _diffrn_reflns_Laue_measured_fraction_max 0.942 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 12789 _diffrn_reflns_point_group_measured_fraction_full 0.984 _diffrn_reflns_point_group_measured_fraction_max 0.942 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.999 _diffrn_reflns_theta_min 4.012 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_current 0.80 _diffrn_source_power 0.040 _diffrn_source_target Cu _diffrn_source_type 'SuperNova (Cu) X-ray Source' _diffrn_source_voltage 50 _exptl_absorpt_coefficient_mu 8.280 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.64245 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.586 _exptl_crystal_description plate _exptl_crystal_F_000 1054 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _refine_diff_density_max 1.413 _refine_diff_density_min -1.434 _refine_diff_density_rms 0.112 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 559 _refine_ls_number_reflns 8465 _refine_ls_number_restraints 20 _refine_ls_restrained_S_all 1.042 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0299 _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^)+(0.0430P)^2^+1.9410P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0758 _refine_ls_wR_factor_ref 0.0775 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7901 _reflns_number_total 8465 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt01269j2.cif _cod_data_source_block wai228cult _cod_depositor_comments 'Adding full bibliography for 7707513--7707520.cif.' _cod_original_cell_volume 2208.99(15) _cod_original_formula_sum 'C54.50 H44 Cl2 Ir P3' _cod_database_code 7707515 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.852 _shelx_estimated_absorpt_t_min 0.491 _reflns_odcompleteness_completeness 98.61 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2. Restrained distances Cl2S-C1S = Cl1S-C1S 1.72 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(Cl2S) \\sim Ueq, Uanis(Cl1S) \\sim Ueq, Uanis(C1S) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.002 4. Others Fixed Sof: Cl1S(0.5) Cl2S(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5) 5.a Secondary CH2 refined with riding coordinates: C1S(H1SA,H1SB) 5.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C5(H5), C6(H6), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C33(H33), C34(H34), C35(H35), C36(H36), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C82(H82), C83(H83), C84(H84), C85(H85), C86(H86) ; _shelx_res_file ; wai228cult.res created by SHELXL-2014/7 TITL CELL 1.54184 10.795513 12.113874 18.580817 76.8505 88.0107 69.1892 ZERR 2 0.000493 0.000381 0.000627 0.0028 0.0032 0.0035 LATT 1 SFAC C H Cl Ir P UNIT 109 88 4 2 6 DFIX 1.72 Cl2S C1S Cl1S C1S ISOR 0.003 0.002 Cl2S Cl1S C1S L.S. 10 PLAN 20 SIZE 0.02 0.08 0.1 fmap 2 ACTA OMIT 0 5 17 OMIT -4 0 2 OMIT 5 2 21 OMIT 5 10 19 OMIT 3 1 21 OMIT 2 4 3 REM REM REM WGHT 0.043000 1.941000 FVAR 3.75441 IR1 4 0.441769 0.395822 0.259748 11.00000 0.01156 0.01090 = 0.01308 -0.00077 -0.00176 -0.00358 CL1 3 0.295436 0.410720 0.366570 11.00000 0.01935 0.02035 = 0.01756 -0.00459 0.00305 -0.00890 P1 5 0.388577 0.225041 0.247511 11.00000 0.01352 0.01128 = 0.01671 -0.00126 -0.00261 -0.00409 P2 5 0.654264 0.295353 0.324420 11.00000 0.01152 0.01240 = 0.01605 -0.00153 -0.00217 -0.00337 P3 5 0.437522 0.594017 0.240844 11.00000 0.01323 0.01084 = 0.01395 -0.00093 -0.00053 -0.00369 C1 1 0.258024 0.337372 0.184811 11.00000 0.01624 0.01410 = 0.01879 0.00000 -0.00232 -0.00290 C2 1 0.289090 0.442071 0.180786 11.00000 0.01593 0.01646 = 0.01454 -0.00108 -0.00303 -0.00520 C3 1 0.210498 0.546605 0.129212 11.00000 0.02518 0.01625 = 0.02075 0.00071 -0.00504 -0.00769 AFIX 43 H3 2 0.227539 0.618128 0.123232 11.00000 -1.20000 AFIX 0 C4 1 0.107408 0.544414 0.086947 11.00000 0.02287 0.02004 = 0.02346 0.00234 -0.01036 -0.00435 AFIX 43 H4 2 0.058829 0.613788 0.052013 11.00000 -1.20000 AFIX 0 C5 1 0.075874 0.440078 0.096133 11.00000 0.01795 0.02636 = 0.02274 -0.00116 -0.00909 -0.00703 AFIX 43 H5 2 0.004274 0.441033 0.069252 11.00000 -1.20000 AFIX 0 C6 1 0.152631 0.334369 0.145959 11.00000 0.01926 0.01941 = 0.02336 -0.00354 -0.00181 -0.00761 AFIX 43 H6 2 0.133527 0.263722 0.152904 11.00000 -1.20000 AFIX 0 C11 1 0.314009 0.133426 0.312661 11.00000 0.01652 0.01546 = 0.01746 -0.00170 -0.00334 -0.00767 C12 1 0.188993 0.190002 0.338653 11.00000 0.01528 0.01513 = 0.02224 -0.00086 -0.00504 -0.00362 AFIX 43 H12 2 0.146593 0.273668 0.323745 11.00000 -1.20000 AFIX 0 C13 1 0.129079 0.120978 0.386480 11.00000 0.01601 0.02196 = 0.02352 -0.00564 -0.00027 -0.00741 AFIX 43 H13 2 0.046747 0.158736 0.404063 11.00000 -1.20000 AFIX 0 C14 1 0.190710 -0.004129 0.408472 11.00000 0.02225 0.02120 = 0.02014 0.00233 -0.00263 -0.01316 AFIX 43 H14 2 0.149197 -0.049897 0.440176 11.00000 -1.20000 AFIX 0 C15 1 0.314113 -0.060805 0.383171 11.00000 0.02543 0.01532 = 0.02309 -0.00087 -0.00431 -0.00680 AFIX 43 H15 2 0.355252 -0.144667 0.397594 11.00000 -1.20000 AFIX 0 C16 1 0.376119 0.007830 0.336289 11.00000 0.01679 0.01845 = 0.01938 -0.00372 -0.00251 -0.00445 AFIX 43 H16 2 0.459936 -0.030210 0.320431 11.00000 -1.20000 AFIX 0 C21 1 0.487466 0.114981 0.195258 11.00000 0.02421 0.01372 = 0.01862 -0.00235 0.00005 -0.00819 C22 1 0.421718 0.076715 0.148561 11.00000 0.02414 0.02043 = 0.02356 -0.00573 -0.00018 -0.01055 AFIX 43 H22 2 0.329594 0.109423 0.143212 11.00000 -1.20000 AFIX 0 C23 1 0.491793 -0.009884 0.109673 11.00000 0.03741 0.02373 = 0.02348 -0.00809 0.00113 -0.01380 AFIX 43 H23 2 0.446744 -0.034560 0.078423 11.00000 -1.20000 AFIX 0 C24 1 0.628614 -0.058970 0.117753 11.00000 0.03813 0.01950 = 0.03693 -0.01589 0.00436 -0.00544 AFIX 43 H24 2 0.675977 -0.116825 0.091899 11.00000 -1.20000 AFIX 0 C25 1 0.694698 -0.022181 0.164073 11.00000 0.02140 0.02734 = 0.05763 -0.02184 -0.00476 0.00110 AFIX 43 H25 2 0.786763 -0.055867 0.169714 11.00000 -1.20000 AFIX 0 C26 1 0.624274 0.065847 0.202924 11.00000 0.02023 0.02433 = 0.03771 -0.01513 -0.00474 -0.00291 AFIX 43 H26 2 0.669640 0.090982 0.233729 11.00000 -1.20000 AFIX 0 C31 1 0.712481 0.302506 0.231617 11.00000 0.01815 0.01482 = 0.01859 -0.00436 0.00072 -0.00680 C32 1 0.592120 0.356075 0.189052 11.00000 0.01472 0.01301 = 0.02303 -0.00469 -0.00176 -0.00428 C33 1 0.595263 0.370418 0.112921 11.00000 0.02138 0.01803 = 0.01858 -0.00396 -0.00068 -0.00760 AFIX 43 H33 2 0.517007 0.405715 0.083472 11.00000 -1.20000 AFIX 0 C34 1 0.717770 0.331050 0.081090 11.00000 0.02966 0.03057 = 0.01778 -0.00952 0.00577 -0.01578 AFIX 43 H34 2 0.720261 0.339799 0.030079 11.00000 -1.20000 AFIX 0 C35 1 0.836112 0.279050 0.124022 11.00000 0.01944 0.02627 = 0.02919 -0.01240 0.00997 -0.01177 AFIX 43 H35 2 0.916363 0.254084 0.101411 11.00000 -1.20000 AFIX 0 C36 1 0.835372 0.264087 0.200561 11.00000 0.01595 0.01976 = 0.02704 -0.00647 0.00081 -0.00572 AFIX 43 H36 2 0.913858 0.229783 0.229805 11.00000 -1.20000 AFIX 0 C41 1 0.701099 0.135201 0.370796 11.00000 0.01777 0.01462 = 0.01713 -0.00261 -0.00328 -0.00633 C42 1 0.832711 0.057499 0.371481 11.00000 0.01670 0.01691 = 0.02641 -0.00396 -0.00231 -0.00482 AFIX 43 H42 2 0.895220 0.087185 0.347263 11.00000 -1.20000 AFIX 0 C43 1 0.870769 -0.063943 0.408159 11.00000 0.01848 0.01600 = 0.03210 -0.00531 -0.00653 -0.00105 AFIX 43 H43 2 0.958323 -0.115538 0.408002 11.00000 -1.20000 AFIX 0 C44 1 0.778258 -0.108001 0.444907 11.00000 0.02686 0.01507 = 0.02464 -0.00040 -0.00827 -0.00746 AFIX 43 H44 2 0.803846 -0.189089 0.469844 11.00000 -1.20000 AFIX 0 C45 1 0.647392 -0.031375 0.444601 11.00000 0.02525 0.02036 = 0.02294 -0.00211 -0.00470 -0.01180 AFIX 43 H45 2 0.585536 -0.061462 0.469299 11.00000 -1.20000 AFIX 0 C46 1 0.607987 0.090133 0.407628 11.00000 0.01629 0.01894 = 0.01841 -0.00269 -0.00200 -0.00682 AFIX 43 H46 2 0.520065 0.141089 0.407444 11.00000 -1.20000 AFIX 0 C51 1 0.755147 0.338338 0.382247 11.00000 0.01232 0.01158 = 0.01990 -0.00308 -0.00567 0.00023 C52 1 0.841381 0.398308 0.353901 11.00000 0.02017 0.01519 = 0.02791 -0.00462 -0.00276 -0.00520 AFIX 43 H52 2 0.847977 0.420536 0.303008 11.00000 -1.20000 AFIX 0 C53 1 0.917535 0.424947 0.401567 11.00000 0.02153 0.01903 = 0.04356 -0.00959 -0.00468 -0.00729 AFIX 43 H53 2 0.975970 0.463768 0.382406 11.00000 -1.20000 AFIX 0 C54 1 0.906917 0.394076 0.477265 11.00000 0.03079 0.01774 = 0.03811 -0.00924 -0.01888 -0.00423 AFIX 43 H54 2 0.957857 0.412421 0.508853 11.00000 -1.20000 AFIX 0 C55 1 0.820155 0.335659 0.506130 11.00000 0.03396 0.01692 = 0.02330 -0.00450 -0.00988 -0.00030 AFIX 43 H55 2 0.812436 0.315427 0.557025 11.00000 -1.20000 AFIX 0 C56 1 0.745053 0.307543 0.458948 11.00000 0.01950 0.01361 = 0.02145 -0.00166 -0.00450 -0.00111 AFIX 43 H56 2 0.687512 0.267899 0.478441 11.00000 -1.20000 AFIX 0 C61 1 0.508706 0.643720 0.154428 11.00000 0.02122 0.01183 = 0.01802 -0.00225 0.00208 -0.00727 C62 1 0.646843 0.598731 0.150072 11.00000 0.02194 0.01452 = 0.02599 -0.00110 0.00357 -0.00609 AFIX 43 H62 2 0.700294 0.550263 0.191916 11.00000 -1.20000 AFIX 0 C63 1 0.704394 0.626099 0.083632 11.00000 0.02897 0.01996 = 0.03416 -0.01001 0.01216 -0.01000 AFIX 43 H63 2 0.796199 0.596332 0.081137 11.00000 -1.20000 AFIX 0 C64 1 0.625293 0.697629 0.021112 11.00000 0.04590 0.02600 = 0.02176 -0.01000 0.01385 -0.01932 AFIX 43 H64 2 0.664100 0.714404 -0.023543 11.00000 -1.20000 AFIX 0 C65 1 0.489386 0.744120 0.024662 11.00000 0.04407 0.02260 = 0.01495 -0.00184 -0.00264 -0.01863 AFIX 43 H65 2 0.436802 0.793011 -0.017391 11.00000 -1.20000 AFIX 0 C66 1 0.430837 0.718070 0.090941 11.00000 0.02576 0.01568 = 0.01899 -0.00301 -0.00260 -0.00925 AFIX 43 H66 2 0.339088 0.750310 0.093160 11.00000 -1.20000 AFIX 0 C71 1 0.524257 0.628756 0.310489 11.00000 0.01458 0.01055 = 0.01707 -0.00210 -0.00241 -0.00080 C72 1 0.599684 0.703463 0.294157 11.00000 0.02125 0.01548 = 0.01840 -0.00266 -0.00056 -0.00673 AFIX 43 H72 2 0.611367 0.736112 0.245157 11.00000 -1.20000 AFIX 0 C73 1 0.657234 0.728953 0.351173 11.00000 0.02157 0.01719 = 0.02810 -0.00509 -0.00157 -0.00946 AFIX 43 H73 2 0.707937 0.778137 0.340197 11.00000 -1.20000 AFIX 0 C74 1 0.639279 0.681309 0.424285 11.00000 0.02284 0.01595 = 0.02322 -0.00676 -0.00664 -0.00377 AFIX 43 H74 2 0.678972 0.697378 0.462356 11.00000 -1.20000 AFIX 0 C75 1 0.562086 0.609761 0.440403 11.00000 0.02272 0.01597 = 0.01508 -0.00113 -0.00119 -0.00538 AFIX 43 H75 2 0.548504 0.579197 0.489450 11.00000 -1.20000 AFIX 0 C76 1 0.504669 0.583183 0.383903 11.00000 0.01971 0.01191 = 0.01875 -0.00139 -0.00130 -0.00573 AFIX 43 H76 2 0.453080 0.534844 0.395237 11.00000 -1.20000 AFIX 0 C81 1 0.275361 0.715776 0.238299 11.00000 0.01684 0.01807 = 0.01388 -0.00328 -0.00239 -0.00318 C82 1 0.270425 0.835859 0.223171 11.00000 0.02064 0.01797 = 0.02780 -0.00673 0.00052 -0.00394 AFIX 43 H82 2 0.347638 0.852486 0.212382 11.00000 -1.20000 AFIX 0 C83 1 0.151687 0.930076 0.224123 11.00000 0.02542 0.01910 = 0.03589 -0.01122 -0.00374 -0.00361 AFIX 43 H83 2 0.149121 1.009704 0.213413 11.00000 -1.20000 AFIX 0 C84 1 0.037058 0.905875 0.240967 11.00000 0.01896 0.02280 = 0.03445 -0.01220 -0.00141 0.00549 AFIX 43 H84 2 -0.042874 0.969306 0.241153 11.00000 -1.20000 AFIX 0 C85 1 0.040852 0.787403 0.257578 11.00000 0.01543 0.03336 = 0.03482 -0.00968 0.00528 -0.00339 AFIX 43 H85 2 -0.036297 0.771213 0.269537 11.00000 -1.20000 AFIX 0 C86 1 0.160440 0.692109 0.256401 11.00000 0.02003 0.01974 = 0.02474 -0.00172 -0.00066 -0.00414 AFIX 43 H86 2 0.162840 0.612515 0.267817 11.00000 -1.20000 AFIX 0 PART -1 CL1S 3 -0.003581 1.114153 -0.035147 10.50000 0.15015 0.12775 = 0.13190 -0.03793 0.01240 -0.04141 CL2S 3 -0.114037 0.921398 -0.016545 10.50000 0.13521 0.14507 = 0.13133 -0.03414 0.02383 -0.03625 C1S 1 -0.074752 1.025110 0.014189 10.50000 0.14696 0.14379 = 0.15096 -0.03035 0.01026 -0.05340 AFIX 23 H1SA 2 -0.156449 1.077965 0.030029 10.50000 -1.20000 H1SB 2 -0.017877 0.981646 0.058525 10.50000 -1.20000 AFIX 0 HKLF 4 REM REM R1 = 0.0299 for 7901 Fo > 4sig(Fo) and 0.0325 for all 8465 data REM 559 parameters refined using 20 restraints END WGHT 0.0431 1.5569 REM Highest difference peak 1.413, deepest hole -1.434, 1-sigma level 0.112 Q1 1 -0.0974 1.0019 -0.0234 11.00000 0.05 1.41 Q2 1 0.4224 0.4139 0.2029 11.00000 0.05 1.29 Q3 1 0.4621 0.3791 0.3183 11.00000 0.05 1.26 Q4 1 0.0630 1.1010 -0.0165 11.00000 0.05 1.26 Q5 1 -0.1371 0.8785 -0.0251 11.00000 0.05 1.06 Q6 1 0.4729 0.3528 0.2211 11.00000 0.05 1.01 Q7 1 0.4233 0.3202 0.2838 11.00000 0.05 0.94 Q8 1 -0.0631 1.1163 -0.0374 11.00000 0.05 0.94 Q9 1 0.4229 0.5008 0.2346 11.00000 0.05 0.86 Q10 1 0.5171 0.4368 0.2220 11.00000 0.05 0.80 Q11 1 0.4008 0.4410 0.3061 11.00000 0.05 0.79 Q12 1 0.4539 0.4945 0.2709 11.00000 0.05 0.71 Q13 1 0.5059 0.3071 0.3826 11.00000 0.05 0.63 Q14 1 0.4164 0.3028 0.2436 11.00000 0.05 0.57 Q15 1 0.3730 0.4818 0.1395 11.00000 0.05 0.55 Q16 1 0.2791 0.4169 0.3171 11.00000 0.05 0.50 Q17 1 0.4556 0.4256 0.1118 11.00000 0.05 0.50 Q18 1 0.4361 0.3593 0.4131 11.00000 0.05 0.49 Q19 1 0.2604 0.4850 0.1558 11.00000 0.05 0.48 Q20 1 0.3431 0.1792 0.2887 11.00000 0.05 0.46 ; _shelx_res_checksum 89373 _shelx_hkl_file ; -13 -8 -2 21635.5 1182.95 8 -13 -8 -1 3662.89 550.580 8 -13 -8 0 28426.2 1463.94 8 -13 -8 1 12903.8 913.650 8 -13 -7 -2 20286.3 1176.77 8 -13 -7 -1 19309.6 1209.71 8 -13 -7 0 49357.9 2176.59 8 -13 -7 1 8392.35 814.432 8 -13 -7 2 51258.8 2178.67 8 -13 -7 3-147.526 319.823 8 -13 -6 -3 28779.9 1369.13 8 -13 -6 -2 2911.55 519.901 8 -13 -6 -1 39590.8 1868.10 8 -13 -6 0 11521.8 961.653 8 -13 -6 1 49419.4 2213.27 8 -13 -6 2 38553.2 1858.72 8 -13 -6 3 18408.3 1158.14 8 -13 -6 4 18803.6 1097.40 8 -13 -5 -2 865.935 343.839 8 -13 -5 -1 34193.2 1682.09 8 -13 -5 0 624.883 421.700 8 -13 -5 1 42735.7 2025.54 8 -13 -5 2 1232.81 453.826 8 -13 -5 3 74604.3 2904.81 8 -13 -5 4 11588.5 874.967 8 -13 -4 -2 4817.18 565.044 8 -13 -4 -1 9032.73 790.590 8 -13 -4 0 5033.97 636.952 8 -13 -4 1 22074.8 1320.40 8 -13 -4 2 1228.61 433.093 8 -13 -4 3 51610.8 2226.48 8 -13 -4 4 569.805 365.737 8 -13 -4 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10 8 8 14426.0 1329.24 7 10 8 9 36350.7 1939.55 6 10 8 9 40607.0 2169.11 7 10 8 10 28454.9 1663.99 6 10 8 10 32733.1 1805.82 7 10 8 11 48671.6 2352.22 6 10 8 11 58395.7 2400.30 7 10 8 12 474.603 327.399 6 10 8 13 67051.1 2652.69 6 10 8 14 2832.84 444.239 6 10 9 -10 16183.2 963.350 1 10 9 -9 26293.5 1442.66 1 10 9 -8 21422.7 1404.93 1 10 9 -7 41903.8 2209.40 1 10 9 -6 80262.8 3493.79 1 10 9 -5 18869.2 1521.08 1 10 9 -4 79155.7 3564.08 1 10 9 -3 1632.11 663.795 1 10 9 -2 129944. 5124.87 1 10 9 -1 18411.3 1546.01 1 10 9 -1 19341.7 1545.48 7 10 9 0 106574. 4458.24 1 10 9 0 109334. 4466.82 7 10 9 1 16785.6 1459.08 7 10 9 2 49176.6 2669.40 7 10 9 3 3642.39 811.471 7 10 9 4 31151.9 2050.84 7 10 9 5 944.483 658.522 7 10 9 6 40875.0 2027.90 6 10 9 6 38430.8 2307.56 7 10 9 7 574.290 364.416 6 10 9 7 294.982 575.428 7 10 9 8 27832.7 1641.89 6 10 9 8 29806.5 1855.92 7 10 9 9 1327.19 464.603 6 10 9 9 1305.32 506.448 7 10 9 10 55465.4 2584.17 6 10 9 10 66741.5 2680.52 7 10 9 11 2994.97 551.814 6 10 9 12 56240.6 2393.41 6 10 9 13 9022.48 761.180 6 10 9 14 15005.0 898.291 6 10 10 -8 15.3692 283.430 1 10 10 -7 69123.2 2787.02 1 10 10 -6 6051.48 781.836 1 10 10 -5 137822. 5026.31 1 10 10 -4 10539.2 1096.51 1 10 10 -3 77101.0 3362.30 1 10 10 -2 16024.1 1358.67 1 10 10 -1 41063.6 2273.38 1 10 10 0 23909.1 1658.36 1 10 10 1 61627.9 2960.59 1 10 10 1 63975.8 3062.63 7 10 10 2 24922.2 1719.79 1 10 10 2 26303.3 1845.95 7 10 10 3 36359.5 2209.37 7 10 10 4 38516.3 1940.84 6 10 10 4 43845.6 2425.06 7 10 10 5 7457.89 798.859 6 10 10 5 7900.02 1028.09 7 10 10 6 16336.2 1179.67 6 10 10 6 15090.2 1364.57 7 10 10 7 9698.00 888.613 6 10 10 7 9603.82 1045.78 7 10 10 8 21200.1 1365.65 6 10 10 8 21970.8 1487.97 7 10 10 9 16914.3 1203.00 6 10 10 9 18484.6 1253.92 7 10 10 10 35397.3 1796.63 6 10 10 11 8746.69 820.497 6 10 10 12 58692.7 2383.33 6 10 10 13 7072.04 623.977 6 10 11 -6 2084.16 437.594 1 10 11 -5 30649.1 1547.11 1 10 11 -4 2688.54 560.210 1 10 11 -3 23520.1 1442.69 1 10 11 -2 3248.03 629.800 1 10 11 -1 34928.1 1898.27 1 10 11 0 5044.31 766.548 1 10 11 1 86531.6 3514.55 1 10 11 2 10585.9 1026.51 1 10 11 2 11056.5 891.115 6 10 11 3 60399.0 2725.06 1 10 11 3 58929.0 2466.45 6 10 11 4 23821.7 1368.98 6 10 11 4 22804.3 1507.06 1 10 11 5 23499.7 1374.68 6 10 11 6 9427.74 848.796 6 10 11 7 7214.25 761.793 6 10 11 8 183.928 306.363 6 10 11 9 16767.5 1120.85 6 10 11 10 2779.64 486.911 6 10 11 11 38972.4 1754.34 6 10 11 12 38517.0 1654.51 6 10 12 -2 4208.10 527.033 1 10 12 -1 3052.13 498.502 1 10 12 0 8515.52 761.194 1 10 12 1 34294.4 1541.85 6 10 12 1 33566.2 1671.95 1 10 12 2 804.984 349.175 6 10 12 2-43.8946 305.204 1 10 12 3 67797.3 2565.08 6 10 12 3 64422.5 2652.56 1 10 12 4 688.034 352.557 1 10 12 4 905.825 343.837 6 10 12 5 40782.3 1827.75 6 10 12 6 1835.95 433.323 6 10 12 7 14779.6 980.162 6 10 12 8 2856.70 474.353 6 10 12 9 16483.1 1007.28 6 10 12 10 2834.41 433.339 6 11 -2 3 851.597 296.006 7 11 -2 4 23252.4 1166.81 7 11 -1 1 2874.46 470.949 7 11 -1 2 8005.88 757.971 7 11 -1 3 18908.9 1190.78 7 11 -1 4 36956.0 1805.90 7 11 -1 5 6100.52 696.063 7 11 -1 6 50527.4 2153.51 7 11 -1 7 463.084 315.969 7 11 -1 8 28930.8 1330.20 7 11 0 0 25447.7 1435.92 7 11 0 1 8923.14 842.719 7 11 0 2 2445.67 560.824 7 11 0 3 37682.0 1960.43 7 11 0 4 31038.7 1754.01 7 11 0 5 27121.8 1606.12 7 11 0 6 43925.4 2131.55 7 11 0 7 30960.1 1652.98 7 11 0 8 45446.2 2015.50 7 11 0 9 6432.09 624.482 7 11 1 -1 73909.6 2991.23 7 11 1 0 39460.7 1995.40 7 11 1 1 34888.0 1885.23 7 11 1 2 11966.8 1091.83 7 11 1 3 58783.1 2732.04 7 11 1 4 23432.4 1577.97 7 11 1 5 67167.8 3011.72 7 11 1 6 22228.5 1514.08 7 11 1 7 53245.7 2483.33 7 11 1 8 13244.2 1068.53 7 11 1 9 34426.6 1713.08 7 11 1 10 19329.6 1111.48 7 11 1 11 38600.4 1569.78 7 11 2 -2 15216.5 1125.34 7 11 2 -1 79439.0 3253.81 7 11 2 0 3132.92 637.822 7 11 2 1 36794.9 2023.39 7 11 2 2 3729.23 714.213 7 11 2 3 37880.3 2127.63 7 11 2 4 6183.47 901.379 7 11 2 5 56378.8 2752.00 7 11 2 6 1704.24 632.854 7 11 2 7 44836.3 2325.98 7 11 2 8 117.452 450.596 7 11 2 9 38001.5 1915.40 7 11 2 10 258.944 320.425 7 11 2 11 30831.0 1447.42 7 11 3 -3 162.839 360.785 7 11 3 -2 108752. 4136.06 7 11 3 -1-11.5198 399.338 7 11 3 0 73416.4 3208.10 7 11 3 1 1142.96 484.351 7 11 3 2 7280.88 939.500 7 11 3 3 340.387 530.905 7 11 3 4 79901.1 3545.53 7 11 3 5 29697.4 1912.65 7 11 3 6 62883.7 3001.93 7 11 3 7 38702.9 2161.98 7 11 3 8 17617.1 1360.86 7 11 3 9 12682.3 1084.63 7 11 3 10 14806.4 1078.07 7 11 3 11 6996.21 672.097 7 11 3 12 25945.5 1228.87 7 11 4 -6 16743.8 1266.18 1 11 4 -5 88272.0 3602.21 1 11 4 -4 39988.2 2136.55 1 11 4 -3 38585.4 2125.60 1 11 4 -3 40353.0 2063.44 7 11 4 -2 31934.6 1897.78 1 11 4 -2 32557.9 1862.07 7 11 4 -1 30654.4 1831.31 7 11 4 0 28351.0 1779.13 7 11 4 1 50292.0 2557.66 7 11 4 2 26301.4 1767.48 7 11 4 3 17786.9 1448.23 7 11 4 4 79817.3 3576.23 7 11 4 5 1208.19 613.918 7 11 4 6 47341.4 2527.93 7 11 4 7 302.622 526.006 7 11 4 8 20624.7 1497.82 7 11 4 9 510.757 461.555 7 11 4 10 8994.23 872.535 7 11 4 11-118.728 315.871 7 11 4 12 15069.5 911.046 7 11 5 -10 544.282 287.690 1 11 5 -9 27828.0 1499.84 1 11 5 -8-387.965 388.975 1 11 5 -7 36521.7 1983.44 1 11 5 -6 1671.24 568.430 1 11 5 -5 71636.7 3170.84 1 11 5 -4 690.904 505.946 1 11 5 -4 488.725 387.628 7 11 5 -3 80140.2 3548.09 1 11 5 -3 86041.9 3531.44 7 11 5 -2 9279.33 1027.03 1 11 5 -2 7513.23 927.944 7 11 5 -1 30004.7 1844.47 7 11 5 0 13826.4 1230.29 7 11 5 1 10167.9 1071.93 7 11 5 2 2082.04 597.962 7 11 5 3 53466.4 2722.64 7 11 5 4 42413.3 2383.43 7 11 5 5 27854.0 1877.29 7 11 5 6 61879.6 3013.34 7 11 5 7 1.70115 522.917 7 11 5 8 13617.1 1230.92 7 11 5 9 6224.56 831.359 7 11 5 10 16439.4 1182.85 7 11 5 11 20684.7 1233.73 7 11 5 12 14104.2 877.491 7 11 6 -10 685.739 313.677 1 11 6 -9 15236.1 1067.91 1 11 6 -8 515.934 470.070 1 11 6 -7 25677.9 1631.96 1 11 6 -6 2032.03 581.332 1 11 6 -5 70295.8 3083.25 1 11 6 -5 61468.2 2747.93 7 11 6 -4 5816.31 925.386 1 11 6 -4 4810.45 737.994 7 11 6 -3 47315.3 2442.73 1 11 6 -3 41951.2 2239.59 7 11 6 -2 731.361 550.474 1 11 6 -2 150.650 455.038 7 11 6 -1 19105.0 1465.18 7 11 6 0 1288.37 547.875 7 11 6 1 62810.6 2995.26 7 11 6 2 7129.93 967.164 7 11 6 3 74939.0 3405.37 7 11 6 4 820.266 546.307 7 11 6 5 79636.4 3579.89 7 11 6 6 12417.6 1233.45 7 11 6 7 78751.8 3464.78 7 11 6 8 46186.6 2383.26 7 11 6 9 18852.4 1356.67 7 11 6 10 16671.8 1186.05 7 11 6 11 20005.0 1194.16 7 11 6 12 3655.05 459.621 7 11 7 -10 19410.2 1057.44 1 11 7 -9 7018.00 721.691 1 11 7 -8 19106.5 1302.58 1 11 7 -7 12171.5 1078.10 1 11 7 -6 11761.8 1132.90 1 11 7 -5 49705.0 2529.17 1 11 7 -4 22036.1 1470.71 7 11 7 -4 21178.0 1584.40 1 11 7 -3 24384.5 1699.80 1 11 7 -3 24924.8 1633.26 7 11 7 -2 5737.14 867.420 1 11 7 -2 5775.50 843.532 7 11 7 -1 2824.08 687.428 1 11 7 -1 3685.37 710.799 7 11 7 0 605.945 492.959 7 11 7 1 11840.5 1186.32 7 11 7 2 5014.24 854.600 7 11 7 3 97124.6 4087.58 7 11 7 4 19896.0 1570.79 7 11 7 5 187269. 6709.55 7 11 7 6 551.398 574.778 7 11 7 7 118476. 4619.65 7 11 7 8 920.348 506.746 7 11 7 9 104156. 3987.66 7 11 7 10 2394.41 553.731 7 11 7 11 56809.8 2293.78 7 11 8 -9 17708.3 1048.53 1 11 8 -8 41763.4 1944.18 1 11 8 -7 6052.03 785.782 1 11 8 -6 50346.4 2431.54 1 11 8 -5 10.6703 453.712 1 11 8 -4 72079.1 3230.11 1 11 8 -3 1869.46 684.455 1 11 8 -2 30218.0 1906.06 1 11 8 -2 28618.3 1803.00 7 11 8 -1-354.001 530.953 1 11 8 -1 257.771 483.874 7 11 8 0 4723.61 830.939 7 11 8 1 6333.66 943.348 7 11 8 2 48985.2 2562.34 7 11 8 3 2781.02 732.816 7 11 8 4 102436. 4219.06 7 11 8 5 7859.26 966.063 7 11 8 6 59955.0 2873.76 7 11 8 7 39893.4 2188.27 7 11 8 8 25558.9 1619.83 7 11 8 9 35758.0 1863.42 7 11 8 10 31551.9 1613.91 7 11 8 11 7133.54 629.792 7 11 9 -8 2743.55 436.583 1 11 9 -7 63926.6 2588.48 1 11 9 -6 21528.5 1380.12 1 11 9 -5 58495.8 2643.04 1 11 9 -4 55842.3 2618.92 1 11 9 -3 12349.7 1146.02 1 11 9 -2 95713.0 3889.00 1 11 9 -1 4524.11 789.541 7 11 9 -1 4145.60 779.359 1 11 9 0 21674.9 1583.22 1 11 9 0 22351.2 1581.04 7 11 9 1 22370.8 1590.35 1 11 9 1 22102.7 1594.96 7 11 9 2 25922.1 1744.07 7 11 9 3 60126.5 2895.42 7 11 9 4 59778.3 2877.00 7 11 9 5 24142.3 1659.12 7 11 9 6 48273.2 2459.79 7 11 9 7 3380.01 679.672 7 11 9 8 57075.1 2562.99 7 11 9 9 656.378 357.289 7 11 9 10 32122.6 1511.76 7 11 10 -6 583.048 328.972 1 11 10 -5 99115.1 3624.81 1 11 10 -4 1413.94 505.250 1 11 10 -3 67521.5 2862.22 1 11 10 -2 1793.62 578.849 1 11 10 -1 25140.7 1575.67 1 11 10 0 6416.64 837.307 1 11 10 1 40469.2 2113.21 1 11 10 2 2803.65 667.733 1 11 10 2 3418.55 723.787 7 11 10 3 57762.2 2653.63 1 11 10 3 55447.2 2686.43 7 11 10 4 4027.98 758.296 7 11 10 5 41784.3 2215.93 7 11 10 6 5768.44 804.066 7 11 10 7 22875.4 1457.08 7 11 10 8 20285.4 1271.33 7 11 10 9 28788.6 1419.26 7 11 11 -3 43620.3 1904.05 1 11 11 -2-314.806 365.330 1 11 11 -1 18570.2 1196.91 1 11 11 0 909.186 403.193 1 11 11 1 52860.0 2339.23 1 11 11 2 2895.73 606.862 1 11 11 3 81913.4 3215.44 1 11 11 4 408.560 413.200 1 11 11 5 22528.6 1358.24 1 11 11 6 766.685 381.728 1 11 11 7 15023.5 1040.35 1 11 11 8 456.399 303.826 1 12 0 3 22097.9 1115.30 7 12 1 1 49288.3 2044.96 7 12 1 2 458.175 302.458 7 12 1 3 57853.9 2365.34 7 12 1 4 4071.85 566.835 7 12 1 5 34677.3 1644.22 7 12 1 6 991.040 362.798 7 12 1 7 88565.5 3087.73 7 12 2 0 6263.43 661.291 7 12 2 1 20046.1 1238.29 7 12 2 2 12620.2 974.521 7 12 2 3 22617.0 1357.46 7 12 2 4 30158.3 1631.85 7 12 2 5 19184.7 1240.95 7 12 2 6 36940.1 1798.56 7 12 2 7 55785.7 2301.80 7 12 2 8 5099.34 564.731 7 12 3 -1 244.817 329.508 7 12 3 0 24581.9 1410.23 7 12 3 1-158.067 387.651 7 12 3 2 15130.8 1136.36 7 12 3 3-106.625 421.215 7 12 3 4 39557.1 2013.95 7 12 3 5-242.383 397.037 7 12 3 6 63028.3 2698.76 7 12 3 7 1166.08 456.844 7 12 3 8 37538.2 1764.98 7 12 3 9 5786.14 582.520 7 12 4 -2 15388.9 1066.87 7 12 4 -1 28489.8 1553.99 7 12 4 0 19739.8 1260.90 1 12 4 0 19997.2 1317.24 7 12 4 1 14601.4 1134.25 7 12 4 2 9873.47 954.621 7 12 4 3 20742.6 1491.49 7 12 4 4 19393.5 1366.95 7 12 4 5 13184.7 1119.17 7 12 4 6 14204.3 1136.03 7 12 4 7 14383.0 1105.62 7 12 4 8 9247.45 838.205 7 12 4 9 5947.78 631.190 7 12 4 10 14759.0 872.017 7 12 5 -5 34760.3 1698.84 1 12 5 -4 6395.13 720.308 1 12 5 -3 55755.5 2324.68 7 12 5 -3 54226.7 2413.54 1 12 5 -2 761.974 449.518 1 12 5 -2 377.977 345.257 7 12 5 -1 74171.6 3039.09 1 12 5 -1 73184.3 2997.70 7 12 5 0 7382.12 842.192 1 12 5 0 10161.7 944.762 7 12 5 1 49539.1 2348.51 7 12 5 2 11621.5 1051.73 7 12 5 3 34432.9 1911.11 7 12 5 4 12263.2 1110.18 7 12 5 5 13817.4 1159.26 7 12 5 6 558.857 508.132 7 12 5 7 31798.2 1740.61 7 12 5 8 8141.12 804.341 7 12 5 9 19041.3 1154.98 7 12 5 10 9228.74 699.799 7 12 6 -7 9129.33 721.266 1 12 6 -6 19877.7 1192.58 1 12 6 -5 15223.6 1093.71 1 12 6 -4 9694.82 897.709 1 12 6 -3 21685.9 1316.69 7 12 6 -3 25883.2 1507.75 1 12 6 -2 4430.46 686.577 1 12 6 -2 3838.94 615.059 7 12 6 -1 40603.5 2061.77 1 12 6 -1 39207.5 1979.65 7 12 6 0 12073.7 1050.62 1 12 6 0 12538.2 1076.27 7 12 6 1 40174.1 2073.27 7 12 6 2 1669.17 547.247 7 12 6 3 71019.6 3076.11 7 12 6 4 230.507 430.291 7 12 6 5 97740.5 3856.59 7 12 6 6 4940.82 751.295 7 12 6 7 40424.5 2018.36 7 12 6 8 7359.48 785.409 7 12 6 9 14203.6 977.995 7 12 6 10 334.898 284.242 7 12 7 -7 3480.05 461.574 1 12 7 -6 19512.6 1178.78 1 12 7 -5-130.750 368.858 1 12 7 -4 28971.4 1602.87 1 12 7 -3 1931.16 553.569 1 12 7 -2 34127.0 1782.89 7 12 7 -2 36074.6 1890.57 1 12 7 -1 20712.5 1378.78 1 12 7 -1 18748.1 1301.30 7 12 7 0 29696.6 1757.88 1 12 7 0 32612.5 1774.93 7 12 7 1 11781.3 1064.38 7 12 7 2 16393.3 1282.78 7 12 7 3 19150.0 1381.02 7 12 7 4 32372.7 1843.56 7 12 7 5 74282.7 3152.68 7 12 7 6 44448.7 2188.62 7 12 7 7 96102.9 3659.26 7 12 7 8 1117.55 429.624 7 12 7 9 51991.5 2150.86 7 12 7 10 316.907 257.309 7 12 8 -6 12996.1 894.623 1 12 8 -5 22892.5 1314.90 1 12 8 -4 21958.0 1346.86 1 12 8 -3 8253.83 855.191 1 12 8 -2 26566.8 1555.27 1 12 8 -1 6129.75 755.110 7 12 8 -1 6817.73 812.132 1 12 8 0 31604.9 1792.96 1 12 8 0 34715.9 1826.65 7 12 8 1-62.9324 455.709 1 12 8 1 257.137 430.954 7 12 8 2 23899.5 1514.87 7 12 8 3 373.080 429.306 7 12 8 4 40162.1 2075.93 7 12 8 5 761.615 514.283 7 12 8 6 65576.3 2796.84 7 12 8 7 8330.76 836.534 7 12 8 8 43922.5 1977.54 7 12 8 9 17053.9 1012.13 7 12 9 -5 39001.7 1714.31 1 12 9 -4 970.071 391.543 1 12 9 -3 38569.0 1847.57 1 12 9 -2 10679.9 937.132 1 12 9 -1 30345.4 1646.79 1 12 9 0 3173.87 611.146 1 12 9 1 38041.4 1947.47 1 12 9 1 39340.1 1971.50 7 12 9 2 4365.94 672.793 1 12 9 2 5432.28 728.890 7 12 9 3 51509.2 2344.61 1 12 9 3 49201.9 2347.13 7 12 9 4 27306.7 1599.11 7 12 9 5 35382.4 1845.67 7 12 9 6 44483.4 2095.05 7 12 9 7 8342.72 804.389 7 12 9 8 22840.4 1226.57 7 12 10 -3 47618.8 1968.87 1 12 10 -2 1062.40 376.710 1 12 10 -1 27109.8 1434.16 1 12 10 0 848.410 405.202 1 12 10 1 19570.0 1225.28 1 12 10 2-196.981 375.383 1 12 10 3 42026.6 1958.96 1 12 10 4 290.245 407.452 1 12 10 5 84441.7 3192.26 1 12 10 6 4313.09 580.585 1 13 4 1 9186.07 690.773 7 13 4 2 5126.61 547.128 7 13 4 3 5414.53 583.886 7 13 4 4 1031.79 351.060 7 13 4 5 9963.99 740.056 7 13 5 0 473.119 282.846 7 13 5 1 32871.8 1528.30 7 13 5 2 1421.76 387.745 7 13 5 3 24567.0 1311.91 7 13 5 4 1435.37 391.350 7 13 5 5 15739.8 988.274 7 13 5 6 3277.41 457.422 7 13 6 -1 47481.2 1893.51 7 13 6 0 12469.7 817.147 7 13 6 0 10044.4 785.972 1 13 6 1 39483.4 1739.24 7 13 6 1 36911.2 1679.85 1 13 6 2 2363.45 435.059 1 13 6 2 2597.82 470.617 7 13 6 3 31668.2 1539.04 1 13 6 3 37933.3 1699.13 7 13 6 4 4071.87 511.406 1 13 6 4 6197.72 660.046 7 13 6 5 45991.7 1961.23 7 13 6 6 5785.61 589.291 7 13 7 -1 7827.36 666.295 1 13 7 0 53255.1 2096.67 7 13 7 0 50164.9 2092.71 1 13 7 1 20264.5 1154.86 7 13 7 1 19293.4 1128.24 1 13 7 2 21224.2 1216.70 1 13 7 2 23361.6 1261.91 7 13 7 3 10231.4 813.552 1 13 7 3 11290.8 867.954 7 13 7 4 21333.3 1208.58 1 13 7 4 24258.8 1281.73 7 13 7 5 4165.08 511.553 1 13 7 5 3467.53 512.107 7 13 7 6 51287.2 2057.87 7 13 8 0 33788.1 1551.30 1 13 8 1 4758.21 553.580 1 13 8 1 4963.14 565.266 7 13 8 2 24865.4 1297.89 7 13 8 2 23798.7 1271.64 1 13 8 3 7648.28 692.013 1 13 8 3 7728.66 707.028 7 13 8 4 25804.0 1340.29 1 13 8 4 27782.8 1376.32 7 13 8 5 558.557 315.562 7 13 8 5 294.546 289.275 1 0 0 0 0.00 0.00 0 TITL wai228CuLT in P1 REM P1 (#1 in standard setting) CELL 1.54184 10.795513 12.113874 18.580817 76.8505 88.0107 69.1892 ZERR 9.00 0.000493 0.000381 0.000627 0.0028 0.0032 0.0035 LATT -1 SFAC C H N O UNIT 99.00 90.00 9.00 9.00 TREF HKLF 4 END ; _shelx_hkl_checksum 68362 _olex2_date_sample_data_collection 2019-02-22 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.434 _oxdiff_exptl_absorpt_empirical_full_min 0.787 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.44177(2) 0.39582(2) 0.25975(2) 0.01225(5) Uani 1 1 d . . . . . Cl1 Cl 0.29544(8) 0.41072(7) 0.36657(4) 0.01860(16) Uani 1 1 d . . . . . P1 P 0.38858(8) 0.22504(7) 0.24751(5) 0.01418(16) Uani 1 1 d . . . . . P2 P 0.65426(8) 0.29535(7) 0.32442(5) 0.01380(16) Uani 1 1 d . . . . . P3 P 0.43752(8) 0.59402(7) 0.24084(4) 0.01314(16) Uani 1 1 d . . . . . C1 C 0.2580(3) 0.3374(3) 0.18481(19) 0.0176(7) Uani 1 1 d . . . . . C2 C 0.2891(3) 0.4421(3) 0.18079(18) 0.0161(6) Uani 1 1 d . . . . . C3 C 0.2105(4) 0.5466(3) 0.1292(2) 0.0213(7) Uani 1 1 d . . . . . H3 H 0.2275 0.6181 0.1232 0.026 Uiso 1 1 calc R . . . . C4 C 0.1074(4) 0.5444(3) 0.0869(2) 0.0240(8) Uani 1 1 d . . . . . H4 H 0.0588 0.6138 0.0520 0.029 Uiso 1 1 calc R . . . . C5 C 0.0759(4) 0.4401(3) 0.0961(2) 0.0231(7) Uani 1 1 d . . . . . H5 H 0.0043 0.4410 0.0693 0.028 Uiso 1 1 calc R . . . . C6 C 0.1526(4) 0.3344(3) 0.1460(2) 0.0206(7) Uani 1 1 d . . . . . H6 H 0.1335 0.2637 0.1529 0.025 Uiso 1 1 calc R . . . . C11 C 0.3140(3) 0.1334(3) 0.31266(19) 0.0162(6) Uani 1 1 d . . . . . C12 C 0.1890(3) 0.1900(3) 0.3387(2) 0.0185(7) Uani 1 1 d . . . . . H12 H 0.1466 0.2737 0.3237 0.022 Uiso 1 1 calc R . . . . C13 C 0.1291(4) 0.1210(3) 0.3865(2) 0.0202(7) Uani 1 1 d . . . . . H13 H 0.0467 0.1587 0.4041 0.024 Uiso 1 1 calc R . . . . C14 C 0.1907(4) -0.0041(3) 0.4085(2) 0.0208(7) Uani 1 1 d . . . . . H14 H 0.1492 -0.0499 0.4402 0.025 Uiso 1 1 calc R . . . . C15 C 0.3141(4) -0.0608(3) 0.3832(2) 0.0219(7) Uani 1 1 d . . . . . H15 H 0.3553 -0.1447 0.3976 0.026 Uiso 1 1 calc R . . . . C16 C 0.3761(3) 0.0078(3) 0.33629(19) 0.0187(7) Uani 1 1 d . . . . . H16 H 0.4599 -0.0302 0.3204 0.022 Uiso 1 1 calc R . . . . C21 C 0.4875(4) 0.1150(3) 0.19526(19) 0.0187(7) Uani 1 1 d . . . . . C22 C 0.4217(4) 0.0767(3) 0.1486(2) 0.0218(7) Uani 1 1 d . . . . . H22 H 0.3296 0.1094 0.1432 0.026 Uiso 1 1 calc R . . . . C23 C 0.4918(4) -0.0099(3) 0.1097(2) 0.0269(8) Uani 1 1 d . . . . . H23 H 0.4467 -0.0346 0.0784 0.032 Uiso 1 1 calc R . . . . C24 C 0.6286(4) -0.0590(3) 0.1178(2) 0.0313(9) Uani 1 1 d . . . . . H24 H 0.6760 -0.1168 0.0919 0.038 Uiso 1 1 calc R . . . . C25 C 0.6947(4) -0.0222(4) 0.1641(3) 0.0360(10) Uani 1 1 d . . . . . H25 H 0.7868 -0.0559 0.1697 0.043 Uiso 1 1 calc R . . . . C26 C 0.6243(4) 0.0658(3) 0.2029(2) 0.0273(8) Uani 1 1 d . . . . . H26 H 0.6696 0.0910 0.2337 0.033 Uiso 1 1 calc R . . . . C31 C 0.7125(3) 0.3025(3) 0.23162(19) 0.0168(6) Uani 1 1 d . . . . . C32 C 0.5921(3) 0.3561(3) 0.1891(2) 0.0169(7) Uani 1 1 d . . . . . C33 C 0.5953(4) 0.3704(3) 0.11292(19) 0.0192(7) Uani 1 1 d . . . . . H33 H 0.5170 0.4057 0.0835 0.023 Uiso 1 1 calc R . . . . C34 C 0.7178(4) 0.3311(3) 0.0811(2) 0.0240(8) Uani 1 1 d . . . . . H34 H 0.7203 0.3398 0.0301 0.029 Uiso 1 1 calc R . . . . C35 C 0.8361(4) 0.2791(3) 0.1240(2) 0.0231(7) Uani 1 1 d . . . . . H35 H 0.9164 0.2541 0.1014 0.028 Uiso 1 1 calc R . . . . C36 C 0.8354(4) 0.2641(3) 0.2006(2) 0.0209(7) Uani 1 1 d . . . . . H36 H 0.9139 0.2298 0.2298 0.025 Uiso 1 1 calc R . . . . C41 C 0.7011(3) 0.1352(3) 0.37080(19) 0.0164(6) Uani 1 1 d . . . . . C42 C 0.8327(4) 0.0575(3) 0.3715(2) 0.0204(7) Uani 1 1 d . . . . . H42 H 0.8952 0.0872 0.3473 0.025 Uiso 1 1 calc R . . . . C43 C 0.8708(4) -0.0639(3) 0.4082(2) 0.0235(7) Uani 1 1 d . . . . . H43 H 0.9583 -0.1155 0.4080 0.028 Uiso 1 1 calc R . . . . C44 C 0.7783(4) -0.1080(3) 0.4449(2) 0.0227(7) Uani 1 1 d . . . . . H44 H 0.8038 -0.1891 0.4698 0.027 Uiso 1 1 calc R . . . . C45 C 0.6474(4) -0.0314(3) 0.4446(2) 0.0222(7) Uani 1 1 d . . . . . H45 H 0.5855 -0.0615 0.4693 0.027 Uiso 1 1 calc R . . . . C46 C 0.6080(3) 0.0901(3) 0.40763(19) 0.0179(7) Uani 1 1 d . . . . . H46 H 0.5201 0.1411 0.4074 0.022 Uiso 1 1 calc R . . . . C51 C 0.7551(3) 0.3383(3) 0.38225(19) 0.0158(6) Uani 1 1 d . . . . . C52 C 0.8414(4) 0.3983(3) 0.3539(2) 0.0214(7) Uani 1 1 d . . . . . H52 H 0.8480 0.4205 0.3030 0.026 Uiso 1 1 calc R . . . . C53 C 0.9175(4) 0.4249(3) 0.4016(2) 0.0275(8) Uani 1 1 d . . . . . H53 H 0.9760 0.4638 0.3824 0.033 Uiso 1 1 calc R . . . . C54 C 0.9069(4) 0.3941(3) 0.4773(2) 0.0291(9) Uani 1 1 d . . . . . H54 H 0.9579 0.4124 0.5089 0.035 Uiso 1 1 calc R . . . . C55 C 0.8202(4) 0.3357(3) 0.5061(2) 0.0269(8) Uani 1 1 d . . . . . H55 H 0.8124 0.3154 0.5570 0.032 Uiso 1 1 calc R . . . . C56 C 0.7451(4) 0.3075(3) 0.4589(2) 0.0198(7) Uani 1 1 d . . . . . H56 H 0.6875 0.2679 0.4784 0.024 Uiso 1 1 calc R . . . . C61 C 0.5087(4) 0.6437(3) 0.15443(19) 0.0169(7) Uani 1 1 d . . . . . C62 C 0.6468(4) 0.5987(3) 0.1501(2) 0.0216(7) Uani 1 1 d . . . . . H62 H 0.7003 0.5503 0.1919 0.026 Uiso 1 1 calc R . . . . C63 C 0.7044(4) 0.6261(3) 0.0836(2) 0.0270(8) Uani 1 1 d . . . . . H63 H 0.7962 0.5963 0.0811 0.032 Uiso 1 1 calc R . . . . C64 C 0.6253(4) 0.6976(4) 0.0211(2) 0.0289(9) Uani 1 1 d . . . . . H64 H 0.6641 0.7144 -0.0235 0.035 Uiso 1 1 calc R . . . . C65 C 0.4894(4) 0.7441(3) 0.0247(2) 0.0256(8) Uani 1 1 d . . . . . H65 H 0.4368 0.7930 -0.0174 0.031 Uiso 1 1 calc R . . . . C66 C 0.4308(4) 0.7181(3) 0.09094(19) 0.0197(7) Uani 1 1 d . . . . . H66 H 0.3391 0.7503 0.0932 0.024 Uiso 1 1 calc R . . . . C71 C 0.5243(3) 0.6288(3) 0.31049(18) 0.0152(6) Uani 1 1 d . . . . . C72 C 0.5997(4) 0.7035(3) 0.29416(19) 0.0185(7) Uani 1 1 d . . . . . H72 H 0.6114 0.7361 0.2452 0.022 Uiso 1 1 calc R . . . . C73 C 0.6572(4) 0.7290(3) 0.3512(2) 0.0215(7) Uani 1 1 d . . . . . H73 H 0.7079 0.7781 0.3402 0.026 Uiso 1 1 calc R . . . . C74 C 0.6393(4) 0.6813(3) 0.4243(2) 0.0210(7) Uani 1 1 d . . . . . H74 H 0.6790 0.6974 0.4624 0.025 Uiso 1 1 calc R . . . . C75 C 0.5621(4) 0.6098(3) 0.44040(19) 0.0187(7) Uani 1 1 d . . . . . H75 H 0.5485 0.5792 0.4895 0.022 Uiso 1 1 calc R . . . . C76 C 0.5047(3) 0.5832(3) 0.38390(19) 0.0171(7) Uani 1 1 d . . . . . H76 H 0.4531 0.5348 0.3952 0.020 Uiso 1 1 calc R . . . . C81 C 0.2754(3) 0.7158(3) 0.23830(18) 0.0171(7) Uani 1 1 d . . . . . C82 C 0.2704(4) 0.8359(3) 0.2232(2) 0.0227(7) Uani 1 1 d . . . . . H82 H 0.3476 0.8525 0.2124 0.027 Uiso 1 1 calc R . . . . C83 C 0.1517(4) 0.9301(3) 0.2241(2) 0.0270(8) Uani 1 1 d . . . . . H83 H 0.1491 1.0097 0.2134 0.032 Uiso 1 1 calc R . . . . C84 C 0.0371(4) 0.9059(3) 0.2410(2) 0.0280(8) Uani 1 1 d . . . . . H84 H -0.0429 0.9693 0.2412 0.034 Uiso 1 1 calc R . . . . C85 C 0.0409(4) 0.7874(4) 0.2576(2) 0.0291(8) Uani 1 1 d . . . . . H85 H -0.0363 0.7712 0.2695 0.035 Uiso 1 1 calc R . . . . C86 C 0.1604(4) 0.6921(3) 0.2564(2) 0.0229(7) Uani 1 1 d . . . . . H86 H 0.1628 0.6125 0.2678 0.027 Uiso 1 1 calc R . . . . Cl1S Cl -0.0036(7) 1.1142(6) -0.0351(4) 0.138(2) Uani 0.5 1 d D U P A -1 Cl2S Cl -0.1140(7) 0.9214(6) -0.0165(4) 0.141(2) Uani 0.5 1 d D U P A -1 C1S C -0.075(2) 1.025(2) 0.0142(13) 0.147(9) Uani 0.5 1 d D U P A -1 H1SA H -0.1564 1.0780 0.0300 0.177 Uiso 0.5 1 calc R . P A -1 H1SB H -0.0179 0.9816 0.0585 0.177 Uiso 0.5 1 calc R . P A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.01156(8) 0.01090(8) 0.01308(8) -0.00077(5) -0.00176(5) -0.00358(5) Cl1 0.0194(4) 0.0203(4) 0.0176(4) -0.0046(3) 0.0030(3) -0.0089(3) P1 0.0135(4) 0.0113(4) 0.0167(4) -0.0013(3) -0.0026(3) -0.0041(3) P2 0.0115(4) 0.0124(4) 0.0161(4) -0.0015(3) -0.0022(3) -0.0034(3) P3 0.0132(4) 0.0108(4) 0.0139(4) -0.0009(3) -0.0005(3) -0.0037(3) C1 0.0162(16) 0.0141(15) 0.0188(16) 0.0000(12) -0.0023(13) -0.0029(13) C2 0.0159(16) 0.0165(15) 0.0145(15) -0.0011(12) -0.0030(12) -0.0052(13) C3 0.0252(18) 0.0163(16) 0.0208(17) 0.0007(13) -0.0050(14) -0.0077(14) C4 0.0229(18) 0.0200(17) 0.0235(18) 0.0023(14) -0.0104(15) -0.0044(14) C5 0.0179(17) 0.0264(18) 0.0227(18) -0.0012(14) -0.0091(14) -0.0070(14) C6 0.0193(17) 0.0194(17) 0.0234(18) -0.0035(14) -0.0018(14) -0.0076(14) C11 0.0165(16) 0.0155(15) 0.0175(16) -0.0017(12) -0.0033(13) -0.0077(13) C12 0.0153(16) 0.0151(16) 0.0222(17) -0.0009(13) -0.0050(13) -0.0036(13) C13 0.0160(16) 0.0220(17) 0.0235(18) -0.0056(14) -0.0003(13) -0.0074(14) C14 0.0223(17) 0.0212(17) 0.0201(17) 0.0023(13) -0.0026(14) -0.0132(14) C15 0.0254(19) 0.0153(16) 0.0231(18) -0.0009(13) -0.0043(14) -0.0068(14) C16 0.0168(16) 0.0184(16) 0.0194(16) -0.0037(13) -0.0025(13) -0.0045(13) C21 0.0242(18) 0.0137(15) 0.0186(16) -0.0023(13) 0.0001(14) -0.0082(14) C22 0.0241(18) 0.0204(17) 0.0236(18) -0.0057(14) -0.0002(14) -0.0105(15) C23 0.037(2) 0.0237(18) 0.0235(19) -0.0081(15) 0.0011(16) -0.0138(17) C24 0.038(2) 0.0195(18) 0.037(2) -0.0159(16) 0.0044(18) -0.0054(16) C25 0.021(2) 0.027(2) 0.058(3) -0.022(2) -0.0048(19) 0.0011(16) C26 0.0202(19) 0.0243(19) 0.038(2) -0.0151(16) -0.0047(16) -0.0029(15) C31 0.0182(16) 0.0148(15) 0.0186(16) -0.0044(12) 0.0007(13) -0.0068(13) C32 0.0147(16) 0.0130(15) 0.0230(17) -0.0047(13) -0.0018(13) -0.0043(12) C33 0.0214(17) 0.0180(16) 0.0186(17) -0.0040(13) -0.0007(13) -0.0076(14) C34 0.030(2) 0.0306(19) 0.0178(17) -0.0095(15) 0.0058(15) -0.0158(16) C35 0.0194(17) 0.0263(18) 0.0292(19) -0.0124(15) 0.0100(15) -0.0118(15) C36 0.0160(16) 0.0198(17) 0.0270(19) -0.0065(14) 0.0008(14) -0.0057(13) C41 0.0178(16) 0.0146(15) 0.0171(16) -0.0026(12) -0.0033(13) -0.0063(13) C42 0.0167(17) 0.0169(16) 0.0264(18) -0.0040(14) -0.0023(14) -0.0048(13) C43 0.0185(17) 0.0160(16) 0.032(2) -0.0053(14) -0.0065(15) -0.0011(14) C44 0.0269(19) 0.0151(16) 0.0246(18) -0.0004(13) -0.0083(15) -0.0075(14) C45 0.0253(18) 0.0204(17) 0.0229(18) -0.0021(14) -0.0047(14) -0.0118(15) C46 0.0163(16) 0.0189(16) 0.0184(16) -0.0027(13) -0.0020(13) -0.0068(13) C51 0.0123(15) 0.0116(14) 0.0199(16) -0.0031(12) -0.0057(12) 0.0002(12) C52 0.0202(17) 0.0152(16) 0.0279(19) -0.0046(14) -0.0028(14) -0.0052(14) C53 0.0215(18) 0.0190(17) 0.044(2) -0.0096(16) -0.0047(17) -0.0073(15) C54 0.031(2) 0.0177(17) 0.038(2) -0.0092(16) -0.0189(17) -0.0042(15) C55 0.034(2) 0.0169(17) 0.0233(19) -0.0045(14) -0.0099(16) -0.0003(15) C56 0.0195(17) 0.0136(15) 0.0214(17) -0.0017(13) -0.0045(14) -0.0011(13) C61 0.0212(17) 0.0118(15) 0.0180(16) -0.0022(12) 0.0021(13) -0.0073(13) C62 0.0219(18) 0.0145(16) 0.0260(19) -0.0011(13) 0.0036(14) -0.0061(14) C63 0.029(2) 0.0200(18) 0.034(2) -0.0100(15) 0.0122(17) -0.0100(15) C64 0.046(2) 0.0260(19) 0.0218(19) -0.0100(15) 0.0139(17) -0.0193(18) C65 0.044(2) 0.0226(18) 0.0149(17) -0.0018(14) -0.0026(16) -0.0186(17) C66 0.0258(18) 0.0157(16) 0.0190(17) -0.0030(13) -0.0026(14) -0.0093(14) C71 0.0146(15) 0.0106(14) 0.0171(16) -0.0021(12) -0.0024(12) -0.0008(12) C72 0.0213(17) 0.0155(16) 0.0184(16) -0.0027(13) -0.0006(13) -0.0067(13) C73 0.0216(18) 0.0172(16) 0.0281(19) -0.0051(14) -0.0016(14) -0.0095(14) C74 0.0228(18) 0.0160(16) 0.0232(18) -0.0068(13) -0.0066(14) -0.0038(14) C75 0.0227(17) 0.0160(16) 0.0151(16) -0.0011(12) -0.0012(13) -0.0054(13) C76 0.0197(16) 0.0119(15) 0.0188(16) -0.0014(12) -0.0013(13) -0.0057(13) C81 0.0168(16) 0.0181(16) 0.0139(15) -0.0033(12) -0.0024(12) -0.0032(13) C82 0.0206(18) 0.0180(17) 0.0278(19) -0.0067(14) 0.0005(14) -0.0039(14) C83 0.0254(19) 0.0191(17) 0.036(2) -0.0112(16) -0.0037(16) -0.0036(15) C84 0.0190(18) 0.0228(18) 0.034(2) -0.0122(16) -0.0014(15) 0.0055(15) C85 0.0154(18) 0.033(2) 0.035(2) -0.0097(17) 0.0053(15) -0.0034(16) C86 0.0200(18) 0.0197(17) 0.0247(18) -0.0017(14) -0.0007(14) -0.0041(14) Cl1S 0.150(3) 0.128(3) 0.132(3) -0.0379(18) 0.0124(18) -0.0414(18) Cl2S 0.135(3) 0.145(3) 0.131(3) -0.0341(18) 0.0238(18) -0.0362(18) C1S 0.147(10) 0.144(10) 0.151(10) -0.030(4) 0.010(3) -0.053(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -4.7710 6.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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 P1 Ir1 Cl1 87.73(3) . . ? P1 Ir1 P2 100.61(3) . . ? P2 Ir1 Cl1 100.01(3) . . ? P3 Ir1 Cl1 94.51(3) . . ? P3 Ir1 P1 160.86(3) . . ? P3 Ir1 P2 97.72(3) . . ? C2 Ir1 Cl1 95.18(10) . . ? C2 Ir1 P1 67.28(9) . . ? C2 Ir1 P2 160.24(10) . . ? C2 Ir1 P3 93.58(9) . . ? C32 Ir1 Cl1 167.47(10) . . ? C32 Ir1 P1 90.88(9) . . ? C32 Ir1 P2 68.01(10) . . ? C32 Ir1 P3 90.88(9) . . ? C32 Ir1 C2 95.77(13) . . ? C1 P1 Ir1 83.72(11) . . ? C1 P1 C11 107.43(16) . . ? C1 P1 C21 106.70(16) . . ? C11 P1 Ir1 129.58(11) . . ? C11 P1 C21 101.15(16) . . ? C21 P1 Ir1 122.98(12) . . ? C31 P2 Ir1 82.74(11) . . ? C31 P2 C41 107.39(15) . . ? C31 P2 C51 111.22(16) . . ? C41 P2 Ir1 118.38(11) . . ? C41 P2 C51 98.80(15) . . ? C51 P2 Ir1 134.76(11) . . ? C61 P3 Ir1 113.38(11) . . ? C61 P3 C71 103.58(16) . . ? C61 P3 C81 103.82(16) . . ? C71 P3 Ir1 117.47(10) . . ? C71 P3 C81 98.58(15) . . ? C81 P3 Ir1 117.80(11) . . ? C2 C1 P1 101.4(2) . . ? C6 C1 P1 134.1(3) . . ? C6 C1 C2 124.5(3) . . ? C1 C2 Ir1 107.0(2) . . ? C3 C2 Ir1 137.5(3) . . ? C3 C2 C1 115.5(3) . . ? C4 C3 C2 120.9(3) . . ? C5 C4 C3 121.2(3) . . ? C6 C5 C4 119.4(3) . . ? C1 C6 C5 118.2(3) . . ? C12 C11 P1 119.2(3) . . ? C16 C11 P1 121.8(3) . . ? C16 C11 C12 119.0(3) . . ? C13 C12 C11 119.8(3) . . ? C12 C13 C14 120.6(3) . . ? C15 C14 C13 120.0(3) . . ? C14 C15 C16 119.8(3) . . ? C15 C16 C11 120.7(3) . . ? C22 C21 P1 118.6(3) . . ? C26 C21 P1 122.2(3) . . ? C26 C21 C22 119.1(3) . . ? C21 C22 C23 120.9(4) . . ? C24 C23 C22 119.6(4) . . ? C25 C24 C23 119.9(4) . . ? C24 C25 C26 120.5(4) . . ? C21 C26 C25 119.8(4) . . ? C32 C31 P2 101.3(2) . . ? C36 C31 P2 135.8(3) . . ? C36 C31 C32 122.8(3) . . ? C31 C32 Ir1 107.8(2) . . ? C33 C32 Ir1 133.4(3) . . ? C33 C32 C31 118.8(3) . . ? C32 C33 C34 119.0(3) . . ? C35 C34 C33 121.5(3) . . ? C34 C35 C36 120.5(3) . . ? C35 C36 C31 117.4(3) . . ? C42 C41 P2 119.6(3) . . ? C46 C41 P2 120.9(3) . . ? C46 C41 C42 119.5(3) . . ? C43 C42 C41 120.4(3) . . ? C44 C43 C42 119.9(3) . . ? C43 C44 C45 120.1(3) . . ? C44 C45 C46 120.5(3) . . ? C45 C46 C41 119.7(3) . . ? C52 C51 P2 123.5(3) . . ? C52 C51 C56 119.0(3) . . ? C56 C51 P2 117.5(3) . . ? C53 C52 C51 120.1(4) . . ? C54 C53 C52 120.4(4) . . ? C53 C54 C55 120.0(3) . . ? C56 C55 C54 119.9(4) . . ? C55 C56 C51 120.5(4) . . ? C62 C61 P3 118.5(3) . . ? C66 C61 P3 122.7(3) . . ? C66 C61 C62 118.6(3) . . ? C63 C62 C61 120.4(4) . . ? C64 C63 C62 120.1(4) . . ? C65 C64 C63 120.4(4) . . ? C64 C65 C66 120.1(4) . . ? C65 C66 C61 120.5(4) . . ? C72 C71 P3 124.2(3) . . ? C76 C71 P3 116.2(3) . . ? C76 C71 C72 119.4(3) . . ? C73 C72 C71 120.0(3) . . ? C74 C73 C72 120.2(3) . . ? C75 C74 C73 119.7(3) . . ? C74 C75 C76 120.5(3) . . ? C71 C76 C75 120.1(3) . . ? C82 C81 P3 118.5(3) . . ? C86 C81 P3 122.3(3) . . ? C86 C81 C82 119.1(3) . . ? C83 C82 C81 120.6(4) . . ? C84 C83 C82 120.0(4) . . ? C83 C84 C85 120.1(3) . . ? C84 C85 C86 120.1(4) . . ? C81 C86 C85 120.2(4) . . ? Cl1S C1S Cl2S 124.2(14) . . ? 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 2.4921(8) . ? Ir1 P1 2.3935(8) . ? Ir1 P2 2.3937(8) . ? Ir1 P3 2.3300(8) . ? Ir1 C2 2.079(3) . ? Ir1 C32 2.044(4) . ? P1 C1 1.796(3) . ? P1 C11 1.817(3) . ? P1 C21 1.835(4) . ? P2 C31 1.809(4) . ? P2 C41 1.826(3) . ? P2 C51 1.830(3) . ? P3 C61 1.826(3) . ? P3 C71 1.828(3) . ? P3 C81 1.839(3) . ? C1 C2 1.409(5) . ? C1 C6 1.384(5) . ? C2 C3 1.408(5) . ? C3 C4 1.395(5) . ? C4 C5 1.395(5) . ? C5 C6 1.394(5) . ? C11 C12 1.404(5) . ? C11 C16 1.396(5) . ? C12 C13 1.383(5) . ? C13 C14 1.388(5) . ? C14 C15 1.386(5) . ? C15 C16 1.387(5) . ? C21 C22 1.390(5) . ? C21 C26 1.381(5) . ? C22 C23 1.392(5) . ? C23 C24 1.381(6) . ? C24 C25 1.375(6) . ? C25 C26 1.404(5) . ? C31 C32 1.405(5) . ? C31 C36 1.393(5) . ? C32 C33 1.386(5) . ? C33 C34 1.397(5) . ? C34 C35 1.391(5) . ? C35 C36 1.392(5) . ? C41 C42 1.397(5) . ? C41 C46 1.396(5) . ? C42 C43 1.390(5) . ? C43 C44 1.383(5) . ? C44 C45 1.387(5) . ? C45 C46 1.391(5) . ? C51 C52 1.394(5) . ? C51 C56 1.399(5) . ? C52 C53 1.391(5) . ? C53 C54 1.382(6) . ? C54 C55 1.389(6) . ? C55 C56 1.387(5) . ? C61 C62 1.401(5) . ? C61 C66 1.399(5) . ? C62 C63 1.388(5) . ? C63 C64 1.384(6) . ? C64 C65 1.377(6) . ? C65 C66 1.388(5) . ? C71 C72 1.398(5) . ? C71 C76 1.389(5) . ? C72 C73 1.391(5) . ? C73 C74 1.386(5) . ? C74 C75 1.383(5) . ? C75 C76 1.390(5) . ? C81 C82 1.399(5) . ? C81 C86 1.384(5) . ? C82 C83 1.384(5) . ? C83 C84 1.380(6) . ? C84 C85 1.384(6) . ? C85 C86 1.397(5) . ? Cl1S C1S 1.638(15) . ? Cl2S C1S 1.675(16) . ?