#------------------------------------------------------------------------------ #$Date: 2019-11-10 15:29:03 +0200 (Sun, 10 Nov 2019) $ #$Revision: 225945 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/58/4515845.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_4515845 loop_ _publ_author_name 'Kim, Youyoung' 'Park, Yoonsu' 'Chang, Sukbok' _publ_section_title ; Delineating Physical Organic Parameters in Site-Selective C-H Functionalization of Indoles. ; _journal_issue 6 _journal_name_full 'ACS central science' _journal_page_first 768 _journal_page_last 775 _journal_paper_doi 10.1021/acscentsci.8b00264 _journal_volume 4 _journal_year 2018 _chemical_formula_sum 'C29 H30 F3 Ir N2 O5 S' _chemical_formula_weight 767.81 _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 direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 81.373(2) _cell_angle_beta 79.858(2) _cell_angle_gamma 67.962(2) _cell_formula_units_Z 2 _cell_length_a 9.6211(3) _cell_length_b 10.9933(4) _cell_length_c 14.5750(4) _cell_measurement_reflns_used 9740 _cell_measurement_temperature 426(2) _cell_measurement_theta_max 27.934 _cell_measurement_theta_min 2.864 _cell_volume 1400.64(8) _computing_cell_refinement 'Bruker SMART APEXll' _computing_data_collection 'Bruker SMART APEXll' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_publication_material 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution SHELXTL _diffrn_ambient_temperature 426(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega phi scan' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_unetI/netI 0.0159 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 128466 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.971 _diffrn_reflns_theta_min 2.852 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 4.904 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.5084 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.821 _exptl_crystal_description block _exptl_crystal_F_000 756 _exptl_crystal_size_max 0.210 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.110 _refine_diff_density_max 2.039 _refine_diff_density_min -1.022 _refine_diff_density_rms 0.126 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 380 _refine_ls_number_reflns 6734 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.122 _refine_ls_R_factor_all 0.0263 _refine_ls_R_factor_gt 0.0232 _refine_ls_shift/su_max 0.040 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+3.1962P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.0597 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6352 _reflns_number_total 6734 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file oc8b00264_si_003.cif _cod_data_source_block p1_a _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/current/ACS/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 6909 2019-04-08 15:41:33Z antanas ; _cod_database_code 4515845 _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_min 0.426 _shelx_estimated_absorpt_t_max 0.615 _shelx_res_file ; p1_a.res created by SHELXL-2014/7 TITL p1_a.res in P-1 CELL 0.71073 9.6211 10.9933 14.5750 81.373 79.858 67.962 ZERR 2.000 0.0003 0.0004 0.0004 0.002 0.002 0.002 LATT 1 SFAC C H N O Ir S F UNIT 58 60 4 10 2 2 6 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! L.S. 10 ACTA BOND $H FMAP 2 PLAN 10 HTAB C28 O2_$1 EQIV $1 -x+1, -y+1, -z+2 HTAB C28 O2 HTAB C12 O3 HTAB C12 F1 HTAB CONF SIZE 0.21 0.16 0.11 FREE F2 F5 FREE F3 F5 FREE F2 F4 TEMP 153 WGHT 0.030200 3.196200 FVAR 0.38515 IR1 5 0.306573 0.259977 0.762976 11.00000 0.01301 0.01367 = 0.01631 -0.00220 -0.00099 -0.00568 C1 1 0.311228 0.087851 0.853965 11.00000 0.02316 0.01625 = 0.02111 0.00195 -0.00204 -0.00939 C2 1 0.240750 0.089238 0.773437 11.00000 0.02233 0.02050 = 0.02282 -0.00055 -0.00084 -0.01443 C3 1 0.110937 0.207425 0.769822 11.00000 0.01624 0.02701 = 0.02433 -0.00173 -0.00029 -0.01376 C4 1 0.097383 0.279715 0.848132 11.00000 0.01676 0.02054 = 0.02198 0.00104 0.00234 -0.00764 C5 1 0.219407 0.204316 0.900628 11.00000 0.01935 0.01895 = 0.01861 0.00110 -0.00032 -0.00813 C6 1 0.441068 -0.022622 0.890415 11.00000 0.03040 0.01866 = 0.02927 0.00167 -0.00573 -0.00450 AFIX 137 H6A 2 0.404788 -0.067832 0.945313 11.00000 -1.50000 H6B 2 0.511237 0.011746 0.906029 11.00000 -1.50000 H6C 2 0.490850 -0.082969 0.843391 11.00000 -1.50000 AFIX 0 C7 1 0.293505 -0.015760 0.707215 11.00000 0.03027 0.02550 = 0.03069 -0.00837 -0.00153 -0.01692 AFIX 137 H7A 2 0.245798 -0.079203 0.729305 11.00000 -1.50000 H7B 2 0.401261 -0.058758 0.703663 11.00000 -1.50000 H7C 2 0.267269 0.023386 0.646235 11.00000 -1.50000 AFIX 0 C8 1 0.006864 0.248716 0.697940 11.00000 0.03262 0.04336 = 0.02797 -0.00220 -0.00082 -0.02169 AFIX 137 H8A 2 0.056685 0.203027 0.643280 11.00000 -1.50000 H8B 2 -0.021766 0.341979 0.681618 11.00000 -1.50000 H8C 2 -0.081809 0.227917 0.722312 11.00000 -1.50000 AFIX 0 C9 1 -0.028160 0.404823 0.872710 11.00000 0.01847 0.02881 = 0.02618 -0.00227 0.00343 -0.00231 AFIX 137 H9A 2 -0.113147 0.385067 0.906925 11.00000 -1.50000 H9B 2 -0.057398 0.459753 0.816440 11.00000 -1.50000 H9C 2 0.005314 0.450118 0.910573 11.00000 -1.50000 AFIX 0 C10 1 0.250558 0.242500 0.987265 11.00000 0.02950 0.02807 = 0.01777 -0.00151 -0.00303 -0.00958 AFIX 137 H10A 2 0.206574 0.336504 0.988337 11.00000 -1.50000 H10B 2 0.357832 0.214107 0.987443 11.00000 -1.50000 H10C 2 0.207217 0.201343 1.041497 11.00000 -1.50000 AFIX 0 C11 1 0.606898 0.486105 0.739197 11.00000 0.01321 0.01438 = 0.02360 -0.00253 -0.00211 -0.00510 C12 1 0.595888 0.484333 0.645332 11.00000 0.02632 0.02176 = 0.02315 -0.00573 -0.00144 -0.01119 AFIX 43 H12 2 0.571089 0.418568 0.626669 11.00000 -1.20000 AFIX 0 C13 1 0.622190 0.581330 0.580106 11.00000 0.03142 0.02400 = 0.02208 -0.00449 -0.00081 -0.01318 AFIX 43 H13 2 0.615337 0.580122 0.517416 11.00000 -1.20000 AFIX 0 C14 1 0.658839 0.680823 0.607304 11.00000 0.02056 0.01968 = 0.02999 -0.00256 -0.00010 -0.00893 C15 1 0.685446 0.785806 0.535586 11.00000 0.03899 0.02827 = 0.03271 0.00162 -0.00481 -0.01910 AFIX 137 H15A 2 0.597985 0.865306 0.539738 11.00000 -1.50000 H15B 2 0.703595 0.756863 0.474174 11.00000 -1.50000 H15C 2 0.771764 0.802353 0.547005 11.00000 -1.50000 AFIX 0 C16 1 0.666761 0.682134 0.701511 11.00000 0.02240 0.01828 = 0.03195 -0.00448 -0.00384 -0.01032 AFIX 43 H16 2 0.690474 0.748421 0.720317 11.00000 -1.20000 AFIX 0 C17 1 0.639711 0.585602 0.768334 11.00000 0.01921 0.01883 = 0.02681 -0.00524 -0.00571 -0.00649 AFIX 43 H17 2 0.643643 0.588020 0.831309 11.00000 -1.20000 AFIX 0 C18 1 0.600912 0.111227 0.650335 11.00000 0.01883 0.02268 = 0.02632 -0.01094 0.00157 -0.01147 C19 1 0.725244 0.119382 0.568092 11.00000 0.01988 0.02801 = 0.03371 -0.01300 0.00676 -0.01007 C20 1 0.176323 0.545563 0.679945 11.00000 0.01536 0.02013 = 0.01786 -0.00052 0.00075 -0.00743 C21 1 0.094653 0.642710 0.605883 11.00000 0.03704 0.02461 = 0.02155 0.00084 -0.00592 -0.00343 AFIX 137 H21A 2 0.131910 0.607723 0.546145 11.00000 -1.50000 H21B 2 0.111444 0.723825 0.604101 11.00000 -1.50000 H21C 2 -0.011706 0.658809 0.619965 11.00000 -1.50000 AFIX 0 C22 1 0.101659 0.713364 0.795748 11.00000 0.01859 0.01384 = 0.02501 -0.00449 0.00247 -0.00704 C23 1 -0.021127 0.818281 0.765998 11.00000 0.02038 0.01753 = 0.02878 -0.00191 -0.00097 -0.00525 AFIX 43 H23 2 -0.066690 0.813733 0.716028 11.00000 -1.20000 AFIX 0 C24 1 -0.073822 0.931473 0.814262 11.00000 0.02287 0.01528 = 0.03853 -0.00327 0.00347 -0.00174 AFIX 43 H24 2 -0.155264 1.003875 0.795442 11.00000 -1.20000 AFIX 0 C25 1 -0.007456 0.937807 0.889117 11.00000 0.03300 0.01736 = 0.03525 -0.01093 0.00549 -0.00607 AFIX 43 H25 2 -0.042212 1.015480 0.918193 11.00000 -1.20000 AFIX 0 C26 1 0.110400 0.830022 0.921699 11.00000 0.03134 0.02443 = 0.03105 -0.01319 0.00190 -0.00891 AFIX 43 H26 2 0.152430 0.833562 0.973569 11.00000 -1.20000 AFIX 0 C27 1 0.164273 0.716195 0.874692 11.00000 0.02095 0.01949 = 0.02480 -0.00574 0.00192 -0.00771 C28 1 0.279387 0.590536 0.892961 11.00000 0.02004 0.02230 = 0.02263 -0.00711 -0.00179 -0.00675 AFIX 43 H28 2 0.336307 0.566469 0.942520 11.00000 -1.20000 AFIX 0 C29 1 0.291526 0.512761 0.826198 11.00000 0.01298 0.01594 = 0.02016 -0.00222 -0.00076 -0.00502 F1 7 0.784572 0.204753 0.577574 11.00000 0.06922 0.07388 = 0.05454 -0.03124 0.02839 -0.05957 N1 3 0.394036 0.388354 0.807140 11.00000 0.01408 0.01569 = 0.02224 -0.00481 -0.00246 -0.00562 N2 3 0.183006 0.586475 0.762171 11.00000 0.01494 0.01168 = 0.02158 -0.00307 -0.00175 -0.00291 O1 4 0.657232 0.234586 0.791271 11.00000 0.01759 0.01484 = 0.03256 -0.00374 -0.00614 -0.00285 O2 4 0.580175 0.388100 0.912012 11.00000 0.02502 0.02650 = 0.02160 -0.00263 -0.00992 -0.00855 O3 4 0.488795 0.219864 0.653958 11.00000 0.01684 0.01857 = 0.02115 -0.00551 0.00195 -0.00731 O4 4 0.624870 0.007718 0.698397 11.00000 0.02591 0.01739 = 0.04110 -0.00572 0.00133 -0.00691 O5 4 0.234585 0.428243 0.662922 11.00000 0.02064 0.01567 = 0.01750 -0.00297 -0.00265 -0.00560 S1 6 0.566179 0.362900 0.820419 11.00000 0.01383 0.01473 = 0.02013 -0.00284 -0.00409 -0.00452 F3 7 0.852417 0.005969 0.576018 10.50000 0.03133 F2 7 0.681819 0.120984 0.490099 10.50000 0.03884 0.07614 = 0.01076 -0.01783 0.00860 -0.03330 F4 7 0.666134 0.185090 0.486275 10.50000 0.06082 F5 7 0.822667 0.008394 0.540301 10.50000 0.05260 HKLF 4 REM p1_a.res in P-1 REM R1 = 0.0232 for 6352 Fo > 4sig(Fo) and 0.0263 for all 6734 data REM 380 parameters refined using 0 restraints END WGHT 0.0302 3.1963 REM Instructions for potential hydrogen bonds HTAB C12 F1 HTAB C12 O3 HTAB C28 O2 HTAB C28 O2_$1 REM Highest difference peak 2.039, deepest hole -1.022, 1-sigma level 0.126 Q1 1 0.3838 0.2066 0.7936 11.00000 0.05 2.04 Q2 1 0.2320 0.3101 0.7322 11.00000 0.05 1.90 Q3 1 0.0919 0.2133 0.7105 11.00000 0.05 1.66 Q4 1 0.7696 0.0401 0.5035 11.00000 0.05 1.57 Q5 1 0.3162 0.2763 0.7071 11.00000 0.05 1.30 Q6 1 0.6611 0.2486 0.4936 11.00000 0.05 1.29 Q7 1 0.8692 0.0497 0.6008 11.00000 0.05 1.29 Q8 1 0.2864 0.2401 0.8232 11.00000 0.05 1.26 Q9 1 0.8361 -0.0231 0.5666 11.00000 0.05 1.04 Q10 1 0.3988 0.1988 0.7277 11.00000 0.05 0.85 ; _shelx_res_checksum 2818 _shelx_hkl_file ; 2 1 1 2909.51 133.89 2 1 1 3109.89 133.79 2 1 1 3160.58 133.89 2 1 1 3196.48 134.39 2 1 1 3110.49 134.39 2 1 1 3274.87 133.79 2 1 1 2535.25 133.99 2 1 1 2963.30 133.99 2 1 1 3196.38 134.09 2 1 1 3306.07 133.49 -2 -1 -1 2904.81 134.09 -2 -1 -1 2763.42 134.09 -2 -1 -1 3106.69 133.99 -2 -1 -1 3100.59 134.29 -2 -1 -1 3214.98 134.39 -2 -1 -1 3061.09 133.89 -2 -1 -1 2913.71 134.09 -2 -1 -1 2827.62 133.99 -2 -1 -1 2948.61 133.79 -2 -1 -1 2963.90 134.29 -2 -1 -1 3102.99 134.29 -2 -1 -1 2936.01 133.79 -2 -1 -1 3181.58 133.89 4 2 2 15.50 9.60 4 2 2 21.40 5.30 4 2 2 17.40 9.10 4 2 2 20.70 3.10 4 2 2 22.40 7.60 4 2 2 20.80 7.80 4 2 2 20.70 7.10 4 2 2 21.80 9.90 4 2 2 16.00 3.50 4 2 2 19.30 3.80 4 2 2 15.20 9.20 4 2 2 18.50 10.20 4 2 2 22.80 12.50 -4 -2 -2 16.60 9.70 -4 -2 -2 19.80 10.30 -4 -2 -2 23.60 2.80 -4 -2 -2 22.20 8.10 -4 -2 -2 16.00 3.30 -4 -2 -2 13.70 9.70 -4 -2 -2 23.90 10.20 -4 -2 -2 22.50 12.60 -4 -2 -2 10.70 11.00 -4 -2 -2 17.60 8.70 -4 -2 -2 14.90 12.00 -4 -2 -2 15.40 6.60 6 3 3 2907.41 132.89 6 3 3 3016.00 129.29 6 3 3 2826.52 130.79 6 3 3 3087.89 131.39 6 3 3 3032.30 132.09 6 3 3 2849.01 142.09 6 3 3 2791.72 130.89 6 3 3 2879.31 132.69 6 3 3 2966.60 129.99 6 3 3 3177.18 131.59 6 3 3 3027.50 129.89 6 3 3 2850.11 132.99 6 3 3 2983.50 130.09 -6 -3 -3 2757.22 134.09 -6 -3 -3 2970.20 132.89 -6 -3 -3 2856.11 129.79 -6 -3 -3 2893.61 133.19 -6 -3 -3 2916.81 132.59 -6 -3 -3 2878.11 133.69 -6 -3 -3 2856.51 131.09 -6 -3 -3 2857.01 130.89 -6 -3 -3 2939.51 134.99 -6 -3 -3 2982.50 132.19 -6 -3 -3 2919.81 130.29 -6 -3 -3 2717.33 140.19 -6 -3 -3 3012.40 130.39 8 4 4 726.03 36.10 8 4 4 612.64 57.89 8 4 4 726.03 49.50 8 4 4 759.62 36.50 8 4 4 781.72 36.20 8 4 4 756.22 56.09 8 4 4 747.43 37.90 8 4 4 751.72 55.49 8 4 4 796.22 36.40 8 4 4 733.63 37.60 8 4 4 645.64 57.79 8 4 4 683.83 36.50 -8 -4 -4 734.93 65.59 -8 -4 -4 774.82 35.80 -8 -4 -4 650.03 51.79 -8 -4 -4 784.72 55.69 -8 -4 -4 664.13 45.40 -8 -4 -4 722.13 66.19 -8 -4 -4 748.23 36.80 -8 -4 -4 751.92 51.79 -8 -4 -4 821.82 37.40 -8 -4 -4 794.22 59.89 -8 -4 -4 777.72 36.90 -8 -4 -4 782.92 38.50 -8 -4 -4 751.92 57.29 -8 -4 -4 805.42 54.89 10 5 5 48.30 37.40 10 5 5 27.90 14.70 10 5 5 39.40 10.60 10 5 5 53.39 10.30 10 5 5 75.19 10.50 10 5 5 59.09 46.50 10 5 5 54.79 10.30 10 5 5 60.59 11.00 10 5 5 76.39 9.80 10 5 5 52.39 39.40 10 5 5 61.59 47.70 10 5 5 58.89 34.00 -10 -5 -5 73.29 51.79 -10 -5 -5 68.99 42.70 -10 -5 -5 64.99 40.90 -10 -5 -5 95.39 12.30 -10 -5 -5 83.29 11.40 -10 -5 -5 62.19 36.80 -10 -5 -5 43.50 9.50 -10 -5 -5 44.10 32.50 -10 -5 -5 63.19 8.00 -10 -5 -5 72.59 8.60 -10 -5 -5 66.39 13.30 12 6 6 136.49 15.60 12 6 6 89.79 15.80 12 6 6 117.79 14.50 12 6 6 109.89 68.39 12 6 6 121.29 15.40 12 6 6 75.39 16.30 12 6 6 82.39 19.50 12 6 6 50.69 48.70 12 6 6 79.69 14.90 -12 -6 -6 68.09 66.99 -12 -6 -6 106.39 53.19 -12 -6 -6 52.39 67.49 -12 -6 -6 82.09 14.60 -12 -6 -6 97.59 10.60 -12 -6 -6 80.89 16.10 -12 -6 -6 93.39 14.40 -12 -6 -6 34.20 16.80 -12 -6 -6 53.79 77.49 -11 -5 -6 13.70 10.20 -11 -5 -6 20.60 10.90 -11 -5 -6 4.20 57.89 -11 -5 -6 6.50 11.70 -11 -5 -6 10.90 13.20 -11 -5 -6 6.70 44.00 -11 -5 -6 16.70 60.09 -11 -5 -6 14.30 7.90 -11 -5 -6 29.10 48.10 -11 -5 -6 1.40 48.30 11 5 6 14.70 11.20 11 5 6 17.50 41.10 11 5 6 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45.90 -4 6 13 -7.20 10.40 -4 6 13 1.20 8.00 -4 6 13 1.00 13.30 -4 6 13 -26.50 16.60 -4 6 13 7.90 14.40 6 -5 -12 213.98 16.20 6 -5 -12 206.28 18.60 6 -5 -12 209.68 25.20 6 -5 -12 205.38 18.60 6 -5 -12 231.68 16.40 -6 5 12 212.48 23.00 -6 5 12 190.08 15.50 -6 5 12 266.77 21.50 -1 -8 -16 510.35 29.30 -1 -8 -16 456.65 30.10 -1 -8 -16 419.46 30.30 -1 -8 -16 471.15 29.40 -1 -8 -16 402.56 59.79 -1 -8 -16 414.36 29.10 -1 -8 -16 476.35 57.59 1 8 16 486.25 25.50 1 8 16 420.86 39.50 1 8 16 404.56 26.90 1 8 16 420.26 24.90 1 8 16 437.66 23.80 1 8 16 386.96 35.20 1 8 16 393.16 46.50 1 8 16 456.35 32.20 1 -7 -15 453.55 63.29 1 -7 -15 454.65 28.10 1 -7 -15 509.05 53.79 1 -7 -15 458.85 28.70 1 -7 -15 452.65 29.60 1 -7 -15 493.55 28.70 1 -7 -15 412.96 28.50 -1 7 15 360.56 24.10 -1 7 15 508.35 24.80 -1 7 15 432.46 27.10 -1 7 15 419.76 45.00 -1 7 15 467.25 29.20 -1 7 15 247.08 103.59 -1 7 15 380.66 29.70 -1 7 15 463.55 24.10 -1 7 15 373.76 31.40 3 -6 -14 -8.70 112.09 3 -6 -14 15.30 10.80 3 -6 -14 21.80 10.40 3 -6 -14 21.60 9.80 3 -6 -14 6.60 48.60 3 -6 -14 10.00 9.90 3 -6 -14 32.40 10.40 -3 6 14 31.80 8.70 -3 6 14 40.20 16.00 -3 6 14 26.00 8.20 -3 6 14 35.00 39.70 -3 6 14 42.30 18.70 -3 6 14 47.60 10.70 -3 6 14 22.70 12.90 -3 6 14 12.40 85.29 5 -5 -13 97.79 12.80 5 -5 -13 64.09 19.00 5 -5 -13 40.40 12.30 5 -5 -13 93.29 14.80 5 -5 -13 44.40 12.00 5 -5 -13 72.49 11.80 -5 5 13 80.09 10.60 -5 5 13 129.69 83.19 -5 5 13 78.89 14.10 -5 5 13 83.19 15.50 -5 5 13 63.09 11.10 -5 5 13 8.20 49.40 -5 5 13 63.29 18.80 -2 -8 -17 13.90 12.50 -2 -8 -17 12.40 12.20 -2 -8 -17 16.30 13.10 -2 -8 -17 18.80 12.70 -2 -8 -17 -5.40 55.99 2 8 17 13.90 15.00 2 8 17 43.80 10.50 2 8 17 30.30 12.90 2 8 17 42.70 12.70 2 8 17 29.30 8.80 2 8 17 34.00 11.30 2 8 17 28.40 8.00 0 -7 -16 271.07 23.70 0 -7 -16 296.87 53.39 0 -7 -16 303.07 24.30 0 -7 -16 313.17 24.70 0 -7 -16 237.78 58.89 0 -7 -16 300.47 24.30 0 -7 -16 303.17 24.00 0 7 16 294.57 19.90 0 7 16 185.98 35.90 0 7 16 276.67 19.70 0 7 16 260.67 44.90 0 7 16 307.27 19.30 0 7 16 329.47 24.30 0 7 16 297.07 23.30 0 7 16 269.17 23.50 2 -6 -15 171.68 15.90 2 -6 -15 285.97 85.49 2 -6 -15 182.18 15.00 2 -6 -15 163.48 15.80 2 -6 -15 187.78 15.50 2 -6 -15 203.28 64.19 2 -6 -15 183.78 15.30 2 -6 -15 231.48 53.59 -2 6 15 227.68 21.30 -2 6 15 188.18 16.20 -2 6 15 187.48 14.80 -2 6 15 192.88 23.30 -2 6 15 210.18 13.70 -2 6 15 99.99 47.60 -2 6 15 112.49 91.99 -2 6 15 174.08 13.10 -2 6 15 187.38 16.10 4 -5 -14 -23.30 10.20 4 -5 -14 -6.10 9.70 4 -5 -14 -26.90 13.50 4 -5 -14 -24.30 70.99 4 -5 -14 -9.90 10.60 4 -5 -14 24.60 10.30 4 -5 -14 -15.90 10.50 -4 5 14 4.20 14.00 -4 5 14 -4.90 8.90 -4 5 14 1.90 13.00 -4 5 14 15.30 46.10 -4 5 14 12.10 17.10 -4 5 14 -8.80 8.30 -4 5 14 -26.70 86.09 6 -4 -13 113.79 24.50 6 -4 -13 148.99 17.60 6 -4 -13 132.99 16.50 6 -4 -13 138.09 14.90 6 -4 -13 169.08 18.90 -6 4 13 139.89 17.10 -6 4 13 161.88 20.50 -1 -7 -17 211.88 17.90 -1 -7 -17 239.08 23.30 -1 -7 -17 208.38 63.29 -1 -7 -17 182.28 16.90 -1 -7 -17 241.58 23.20 -1 -7 -17 216.28 59.59 -1 -7 -17 183.28 17.20 1 7 17 201.18 22.90 1 7 17 202.08 20.80 1 7 17 243.48 22.00 1 7 17 171.98 16.10 1 7 17 260.37 17.90 1 7 17 268.07 17.60 1 7 17 215.18 18.00 1 7 17 200.68 22.30 1 -6 -16 334.27 26.00 1 -6 -16 343.57 25.40 1 -6 -16 352.96 54.29 1 -6 -16 303.17 25.50 1 -6 -16 369.76 27.00 1 -6 -16 360.46 64.99 1 -6 -16 356.36 26.20 -1 6 16 330.37 26.20 -1 6 16 407.66 22.50 -1 6 16 396.06 26.90 -1 6 16 421.76 22.40 -1 6 16 306.77 29.80 -1 6 16 322.87 25.70 -1 6 16 342.37 21.60 3 -5 -15 47.30 11.30 3 -5 -15 48.50 11.10 3 -5 -15 28.30 57.59 3 -5 -15 33.00 10.50 3 -5 -15 45.80 12.10 3 -5 -15 18.30 14.70 3 -5 -15 7.40 12.10 -3 5 15 53.49 13.40 -3 5 15 -13.30 95.49 -3 5 15 55.19 9.20 -3 5 15 38.30 11.30 -3 5 15 42.00 16.30 -3 5 15 50.89 43.30 -3 5 15 43.60 18.30 -3 5 15 43.60 9.40 5 -4 -14 76.39 14.30 5 -4 -14 81.39 12.70 5 -4 -14 93.89 13.60 5 -4 -14 84.09 16.20 5 -4 -14 54.99 77.59 5 -4 -14 60.99 13.20 5 -4 -14 79.59 13.70 -5 4 14 110.59 88.99 -5 4 14 92.99 10.80 -5 4 14 65.89 14.50 -5 4 14 77.49 11.90 -5 4 14 89.39 15.60 -5 4 14 79.09 17.90 0 -6 -17 236.78 21.60 0 -6 -17 210.18 17.90 0 -6 -17 147.79 16.90 0 -6 -17 225.08 55.29 0 -6 -17 152.08 15.60 0 -6 -17 189.78 16.70 0 -6 -17 218.98 62.49 0 6 17 191.68 17.20 0 6 17 117.39 24.00 0 6 17 203.78 18.30 0 6 17 191.78 14.00 0 6 17 183.68 21.40 0 6 17 285.37 22.40 0 6 17 261.77 18.60 2 -5 -16 345.27 73.09 2 -5 -16 310.57 23.00 2 -5 -16 274.87 24.20 2 -5 -16 282.97 61.59 2 -5 -16 272.67 23.80 2 -5 -16 259.87 20.40 2 -5 -16 249.97 20.20 2 -5 -16 241.98 19.00 -2 5 16 311.27 20.30 -2 5 16 329.07 21.30 -2 5 16 260.87 19.90 -2 5 16 168.08 48.70 -2 5 16 260.37 18.60 -2 5 16 290.17 26.40 -2 5 16 276.57 22.70 4 -4 -15 22.30 11.90 4 -4 -15 1.80 12.40 4 -4 -15 17.00 11.10 4 -4 -15 12.90 10.10 4 -4 -15 17.10 61.89 4 -4 -15 12.40 10.30 4 -4 -15 -4.80 14.10 -4 4 15 -11.90 16.90 -4 4 15 -14.40 94.39 -4 4 15 20.10 9.10 -4 4 15 13.10 13.70 -4 4 15 1.80 9.60 -4 4 15 -4.80 14.30 -1 -6 -18 292.47 26.10 -1 -6 -18 332.87 29.20 -1 -6 -18 235.68 31.70 -1 -6 -18 339.77 27.80 -1 -6 -18 240.08 62.59 1 6 18 358.56 25.80 1 6 18 356.66 23.50 1 6 18 330.97 22.60 1 6 18 290.17 24.80 1 6 18 242.18 27.90 1 6 18 267.97 24.50 1 -5 -17 492.25 34.40 1 -5 -17 431.76 31.70 1 -5 -17 443.36 29.80 1 -5 -17 476.05 29.50 1 -5 -17 499.65 31.00 1 -5 -17 470.45 31.10 1 -5 -17 422.06 70.79 -1 5 17 403.86 36.90 -1 5 17 559.44 31.50 -1 5 17 485.95 30.70 -1 5 17 411.26 25.80 -1 5 17 424.16 40.90 -1 5 17 492.45 28.30 -1 5 17 474.25 27.70 3 -4 -16 48.30 11.70 3 -4 -16 58.89 11.90 3 -4 -16 38.30 13.20 3 -4 -16 52.09 15.80 3 -4 -16 12.40 56.69 3 -4 -16 35.50 12.40 3 -4 -16 48.50 11.50 -3 4 16 57.29 19.10 -3 4 16 56.69 12.40 -3 4 16 51.69 10.10 -3 4 16 67.29 12.10 -3 4 16 58.99 15.60 -3 4 16 56.29 14.20 5 -3 -15 59.19 13.00 5 -3 -15 30.70 17.90 5 -3 -15 16.80 14.60 5 -3 -15 72.99 14.10 5 -3 -15 51.49 61.29 5 -3 -15 66.99 14.60 -5 3 15 38.80 17.60 -5 3 15 45.30 24.30 -5 3 15 67.59 12.30 0 -5 -18 202.18 66.59 0 -5 -18 230.58 22.10 0 -5 -18 227.48 19.60 0 -5 -18 223.38 20.80 0 -5 -18 230.28 18.30 0 -5 -18 203.48 17.30 0 5 18 289.77 24.90 0 5 18 277.97 22.00 0 5 18 173.18 26.30 0 5 18 274.07 26.00 0 5 18 276.57 20.90 0 5 18 195.88 22.10 2 -4 -17 223.78 23.40 2 -4 -17 214.68 18.60 2 -4 -17 259.07 23.20 2 -4 -17 244.28 58.79 2 -4 -17 202.98 18.60 2 -4 -17 237.78 20.10 2 -4 -17 265.27 23.60 -2 4 17 247.48 24.90 -2 4 17 242.78 17.80 -2 4 17 283.57 20.40 -2 4 17 228.08 18.50 -2 4 17 227.18 22.40 -2 4 17 223.38 18.40 4 -3 -16 7.90 11.50 4 -3 -16 -8.50 60.09 4 -3 -16 -15.40 15.70 4 -3 -16 24.00 13.20 4 -3 -16 3.80 13.90 4 -3 -16 19.10 12.00 -4 3 16 3.00 13.00 -4 3 16 -5.60 9.90 -4 3 16 -14.30 16.60 -4 3 16 11.90 14.50 -4 3 16 -31.30 10.70 -4 3 16 14.10 11.50 1 -4 -18 466.95 33.30 1 -4 -18 451.55 37.30 1 -4 -18 525.85 32.20 1 -4 -18 391.26 75.59 -1 4 18 498.05 43.10 -1 4 18 545.15 37.70 -1 4 18 378.46 35.40 3 -3 -17 95.39 63.19 3 -3 -17 64.59 13.70 3 -3 -17 66.59 13.00 3 -3 -17 77.59 14.10 3 -3 -17 91.99 15.00 3 -3 -17 94.59 17.50 -3 3 17 98.59 15.90 -3 3 17 72.39 19.40 -3 3 17 65.99 13.40 2 -9 -13 132.49 13.90 2 -9 -13 125.69 14.00 2 -9 -13 126.59 14.70 2 -9 -13 129.19 13.80 -2 9 13 133.69 15.70 -2 9 13 113.09 10.40 -2 9 13 134.69 12.00 -2 9 13 131.09 18.10 -2 9 13 129.59 12.20 -2 9 13 79.99 20.80 -2 9 13 123.59 10.10 1 -9 -14 13.70 73.69 1 -9 -14 24.40 11.10 1 -9 -14 9.40 10.90 1 -9 -14 12.90 10.40 1 -9 -14 10.60 11.60 1 -9 -14 32.40 10.70 -1 9 14 29.60 15.30 -1 9 14 24.90 14.60 -1 9 14 -11.70 18.70 -1 9 14 29.90 7.30 -1 9 14 24.60 6.70 -1 9 14 -7.40 9.90 -1 9 14 24.60 9.60 3 -8 -13 312.17 23.30 3 -8 -13 270.87 25.50 3 -8 -13 294.87 24.10 3 -8 -13 377.16 25.00 -3 8 13 311.67 19.40 -3 8 13 292.37 18.70 -3 8 13 301.17 22.90 -3 8 13 308.17 25.20 -3 8 13 283.37 19.40 -3 8 13 89.79 47.40 -3 8 13 246.38 27.20 0 -9 -15 -24.90 12.20 0 -9 -15 30.10 10.70 0 -9 -15 19.20 10.20 0 -9 -15 11.10 11.40 0 -9 -15 -11.10 68.19 0 9 15 -9.20 17.80 0 9 15 -1.00 6.70 0 9 15 13.90 10.30 0 9 15 12.80 9.60 0 9 15 -15.80 10.40 0 9 15 -11.30 6.40 0 9 15 20.80 14.90 2 -8 -14 67.49 12.50 2 -8 -14 143.69 13.70 2 -8 -14 109.09 13.30 2 -8 -14 82.19 13.10 2 -8 -14 108.99 13.70 -2 8 14 74.59 43.30 -2 8 14 94.69 18.20 -2 8 14 109.99 14.90 -2 8 14 102.29 22.70 -2 8 14 120.19 10.90 -2 8 14 130.99 12.30 -2 8 14 124.29 99.19 -2 8 14 92.69 9.10 4 -7 -13 273.57 24.30 4 -7 -13 284.07 24.20 4 -7 -13 276.47 25.00 4 -7 -13 270.87 23.80 -4 7 13 292.37 24.80 -4 7 13 308.87 20.70 -4 7 13 307.97 27.50 1 -8 -15 11.60 11.60 1 -8 -15 9.30 70.69 1 -8 -15 7.00 10.80 1 -8 -15 41.40 12.20 1 -8 -15 23.40 10.50 1 -8 -15 22.50 11.10 -1 8 15 19.50 20.10 -1 8 15 35.80 129.49 -1 8 15 25.60 41.30 -1 8 15 13.60 16.80 -1 8 15 25.80 11.00 -1 8 15 21.30 10.60 -1 8 15 35.00 14.20 -1 8 15 6.30 6.90 -1 8 15 37.90 9.20 3 -7 -14 241.18 23.10 3 -7 -14 269.67 24.80 3 -7 -14 271.07 23.30 3 -7 -14 258.87 22.50 3 -7 -14 286.97 24.30 -3 7 14 229.58 17.80 -3 7 14 268.77 22.60 -3 7 14 239.08 17.60 -3 7 14 296.97 100.59 -3 7 14 249.28 27.20 -3 7 14 244.38 23.60 -3 7 14 242.18 18.30 0 -8 -16 15.20 10.70 0 -8 -16 9.50 11.40 0 -8 -16 -0.80 11.90 0 -8 -16 42.30 11.70 0 -8 -16 -26.50 64.99 0 8 16 -6.30 10.80 0 8 16 14.50 11.30 0 8 16 5.80 6.90 0 8 16 -5.70 54.19 0 8 16 2.30 19.40 0 8 16 18.70 16.00 0 8 16 4.80 7.30 2 -7 -15 151.18 15.20 2 -7 -15 140.99 13.70 2 -7 -15 119.99 14.00 2 -7 -15 132.59 74.09 2 -7 -15 135.29 14.60 2 -7 -15 135.89 21.90 -2 7 15 111.59 15.70 -2 7 15 137.99 14.10 -2 7 15 97.89 14.90 -2 7 15 136.89 11.20 -2 7 15 80.99 107.09 -2 7 15 105.79 23.50 -2 7 15 117.89 21.30 4 -6 -14 349.96 25.20 4 -6 -14 241.38 25.10 4 -6 -14 290.27 25.10 4 -6 -14 296.57 25.30 -4 6 14 278.97 24.10 -4 6 14 300.97 21.00 -4 6 14 275.37 27.60 -4 6 14 277.07 19.70 -4 6 14 323.17 25.10 1 -7 -16 33.20 12.00 1 -7 -16 19.30 16.90 1 -7 -16 17.10 11.60 1 -7 -16 8.40 10.10 1 -7 -16 4.90 11.40 1 -7 -16 -47.30 69.19 -1 7 16 -38.10 20.90 -1 7 16 -18.30 11.70 -1 7 16 23.20 14.40 -1 7 16 1.00 7.90 -1 7 16 -9.80 13.80 -1 7 16 10.80 18.20 -1 7 16 0.90 13.00 3 -6 -15 233.88 24.20 3 -6 -15 190.18 79.59 3 -6 -15 231.38 18.40 3 -6 -15 195.48 18.00 3 -6 -15 146.99 21.40 3 -6 -15 272.97 23.30 -3 6 15 256.87 19.20 -3 6 15 107.99 108.19 -3 6 15 264.17 20.50 -3 6 15 218.88 26.40 -3 6 15 257.57 22.50 -3 6 15 181.88 17.60 2 -6 -16 89.39 12.80 2 -6 -16 76.89 23.80 2 -6 -16 86.39 13.40 2 -6 -16 79.99 12.60 2 -6 -16 113.79 98.29 2 -6 -16 62.99 13.30 -2 6 16 80.39 19.40 -2 6 16 90.29 11.00 -2 6 16 71.49 10.90 -2 6 16 82.49 24.30 -2 6 16 87.09 15.40 -4 5 15 154.38 22.90 1 -6 -17 3.90 12.40 1 -6 -17 -5.20 75.09 1 -6 -17 9.10 10.80 -1 6 17 -22.10 23.60 -1 6 17 -2.00 12.00 -1 6 17 2.90 19.00 3 -5 -16 196.48 17.70 3 -5 -16 109.19 20.50 3 -5 -16 163.68 16.20 3 -5 -16 133.39 15.90 -3 5 16 180.08 21.50 -3 5 16 175.38 23.60 -3 5 16 151.38 18.90 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 23072 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 Ir1 Ir 0.30657(2) 0.25998(2) 0.76298(2) 0.01410(4) Uani 1 1 d . . . C1 C 0.3112(4) 0.0879(3) 0.8540(2) 0.0200(6) Uani 1 1 d . . . C2 C 0.2407(4) 0.0892(3) 0.7734(2) 0.0203(6) Uani 1 1 d . . . C3 C 0.1109(3) 0.2074(3) 0.7698(2) 0.0211(6) Uani 1 1 d . . . C4 C 0.0974(3) 0.2797(3) 0.8481(2) 0.0204(6) Uani 1 1 d . . . C5 C 0.2194(3) 0.2043(3) 0.9006(2) 0.0192(6) Uani 1 1 d . . . C6 C 0.4411(4) -0.0226(3) 0.8904(3) 0.0276(7) Uani 1 1 d . . . H6A H 0.4048 -0.0678 0.9453 0.041 Uiso 1 1 calc R U . H6B H 0.5112 0.0117 0.9060 0.041 Uiso 1 1 calc R U . H6C H 0.4908 -0.0830 0.8434 0.041 Uiso 1 1 calc R U . C7 C 0.2935(4) -0.0158(3) 0.7072(3) 0.0265(7) Uani 1 1 d . . . H7A H 0.2458 -0.0792 0.7293 0.040 Uiso 1 1 calc R U . H7B H 0.4013 -0.0588 0.7037 0.040 Uiso 1 1 calc R U . H7C H 0.2673 0.0234 0.6462 0.040 Uiso 1 1 calc R U . C8 C 0.0069(4) 0.2487(4) 0.6979(3) 0.0328(8) Uani 1 1 d . . . H8A H 0.0567 0.2030 0.6433 0.049 Uiso 1 1 calc R U . H8B H -0.0218 0.3420 0.6816 0.049 Uiso 1 1 calc R U . H8C H -0.0818 0.2279 0.7223 0.049 Uiso 1 1 calc R U . C9 C -0.0282(4) 0.4048(4) 0.8727(2) 0.0272(7) Uani 1 1 d . . . H9A H -0.1131 0.3851 0.9069 0.041 Uiso 1 1 calc R U . H9B H -0.0574 0.4598 0.8164 0.041 Uiso 1 1 calc R U . H9C H 0.0053 0.4501 0.9106 0.041 Uiso 1 1 calc R U . C10 C 0.2506(4) 0.2425(4) 0.9873(2) 0.0254(7) Uani 1 1 d . . . H10A H 0.2066 0.3365 0.9883 0.038 Uiso 1 1 calc R U . H10B H 0.3578 0.2141 0.9874 0.038 Uiso 1 1 calc R U . H10C H 0.2072 0.2013 1.0415 0.038 Uiso 1 1 calc R U . C11 C 0.6069(3) 0.4861(3) 0.7392(2) 0.0170(5) Uani 1 1 d . . . C12 C 0.5959(4) 0.4843(3) 0.6453(2) 0.0228(6) Uani 1 1 d . . . H12 H 0.5711 0.4186 0.6267 0.027 Uiso 1 1 calc R U . C13 C 0.6222(4) 0.5813(3) 0.5801(2) 0.0250(7) Uani 1 1 d . . . H13 H 0.6153 0.5801 0.5174 0.030 Uiso 1 1 calc R U . C14 C 0.6588(4) 0.6808(3) 0.6073(2) 0.0233(6) Uani 1 1 d . . . C15 C 0.6854(5) 0.7858(4) 0.5356(3) 0.0317(8) Uani 1 1 d . . . H15A H 0.5980 0.8653 0.5397 0.048 Uiso 1 1 calc R U . H15B H 0.7036 0.7569 0.4742 0.048 Uiso 1 1 calc R U . H15C H 0.7718 0.8024 0.5470 0.048 Uiso 1 1 calc R U . C16 C 0.6668(4) 0.6821(3) 0.7015(2) 0.0230(6) Uani 1 1 d . . . H16 H 0.6905 0.7484 0.7203 0.028 Uiso 1 1 calc R U . C17 C 0.6397(4) 0.5856(3) 0.7683(2) 0.0210(6) Uani 1 1 d . . . H17 H 0.6436 0.5880 0.8313 0.025 Uiso 1 1 calc R U . C18 C 0.6009(4) 0.1112(3) 0.6503(2) 0.0211(6) Uani 1 1 d . . . C19 C 0.7252(4) 0.1194(4) 0.5681(3) 0.0270(7) Uani 1 1 d . . . C20 C 0.1763(3) 0.5456(3) 0.6799(2) 0.0180(6) Uani 1 1 d . . . C21 C 0.0947(4) 0.6427(4) 0.6059(2) 0.0300(7) Uani 1 1 d . . . H21A H 0.1319 0.6077 0.5461 0.045 Uiso 1 1 calc R U . H21B H 0.1114 0.7238 0.6041 0.045 Uiso 1 1 calc R U . H21C H -0.0117 0.6588 0.6200 0.045 Uiso 1 1 calc R U . C22 C 0.1017(3) 0.7134(3) 0.7957(2) 0.0192(6) Uani 1 1 d . . . C23 C -0.0211(4) 0.8183(3) 0.7660(2) 0.0230(6) Uani 1 1 d . . . H23 H -0.0667 0.8137 0.7160 0.028 Uiso 1 1 calc R U . C24 C -0.0738(4) 0.9315(3) 0.8143(3) 0.0280(7) Uani 1 1 d . . . H24 H -0.1553 1.0039 0.7954 0.034 Uiso 1 1 calc R U . C25 C -0.0075(4) 0.9378(3) 0.8891(3) 0.0298(7) Uani 1 1 d . . . H25 H -0.0422 1.0155 0.9182 0.036 Uiso 1 1 calc R U . C26 C 0.1104(4) 0.8300(4) 0.9217(3) 0.0289(7) Uani 1 1 d . . . H26 H 0.1524 0.8336 0.9736 0.035 Uiso 1 1 calc R U . C27 C 0.1643(4) 0.7162(3) 0.8747(2) 0.0218(6) Uani 1 1 d . . . C28 C 0.2794(4) 0.5905(3) 0.8930(2) 0.0215(6) Uani 1 1 d . . . H28 H 0.3363 0.5665 0.9425 0.026 Uiso 1 1 calc R U . C29 C 0.2915(3) 0.5128(3) 0.8262(2) 0.0165(5) Uani 1 1 d . . . F1 F 0.7846(4) 0.2048(3) 0.5776(2) 0.0578(8) Uani 1 1 d . . . N1 N 0.3940(3) 0.3884(2) 0.80714(18) 0.0169(5) Uani 1 1 d . . . N2 N 0.1830(3) 0.5865(2) 0.76217(18) 0.0165(5) Uani 1 1 d . . . O1 O 0.6572(2) 0.2346(2) 0.79127(17) 0.0220(5) Uani 1 1 d . . . O2 O 0.5802(3) 0.3881(2) 0.91201(16) 0.0236(5) Uani 1 1 d . . . O3 O 0.4888(2) 0.2199(2) 0.65396(15) 0.0187(4) Uani 1 1 d . . . O4 O 0.6249(3) 0.0077(2) 0.69840(19) 0.0288(5) Uani 1 1 d . . . O5 O 0.2346(2) 0.4282(2) 0.66292(15) 0.0180(4) Uani 1 1 d . . . S1 S 0.56618(8) 0.36290(7) 0.82042(5) 0.01603(13) Uani 1 1 d . . . F3 F 0.8524(5) 0.0060(5) 0.5760(3) 0.0313(9) Uiso 0.5 1 d . . P F2 F 0.6818(6) 0.1210(7) 0.4901(3) 0.0382(13) Uani 0.5 1 d . . P F4 F 0.6661(9) 0.1851(8) 0.4863(6) 0.061(2) Uiso 0.5 1 d . . P F5 F 0.8227(7) 0.0084(6) 0.5403(5) 0.0526(14) Uiso 0.5 1 d . . P 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 0.01301(6) 0.01367(6) 0.01631(6) -0.00220(4) -0.00099(4) -0.00568(4) C1 0.0232(15) 0.0163(14) 0.0211(14) 0.0019(11) -0.0020(12) -0.0094(12) C2 0.0223(15) 0.0205(15) 0.0228(15) -0.0006(12) -0.0008(12) -0.0144(12) C3 0.0162(14) 0.0270(16) 0.0243(15) -0.0017(12) -0.0003(11) -0.0138(12) C4 0.0168(14) 0.0205(15) 0.0220(14) 0.0010(12) 0.0023(11) -0.0076(12) C5 0.0193(14) 0.0189(14) 0.0186(14) 0.0011(11) -0.0003(11) -0.0081(12) C6 0.0304(18) 0.0187(15) 0.0293(17) 0.0017(13) -0.0057(14) -0.0045(13) C7 0.0303(17) 0.0255(16) 0.0307(17) -0.0084(13) -0.0015(14) -0.0169(14) C8 0.0326(19) 0.043(2) 0.0280(17) -0.0022(15) -0.0008(14) -0.0217(17) C9 0.0185(15) 0.0288(18) 0.0262(16) -0.0023(13) 0.0034(12) -0.0023(13) C10 0.0295(17) 0.0281(17) 0.0178(14) -0.0015(12) -0.0030(12) -0.0096(14) C11 0.0132(13) 0.0144(13) 0.0236(14) -0.0025(11) -0.0021(11) -0.0051(10) C12 0.0263(16) 0.0218(15) 0.0231(15) -0.0057(12) -0.0014(12) -0.0112(13) C13 0.0314(17) 0.0240(16) 0.0221(15) -0.0045(12) -0.0008(13) -0.0132(14) C14 0.0206(15) 0.0197(15) 0.0300(16) -0.0026(12) -0.0001(12) -0.0089(12) C15 0.039(2) 0.0283(18) 0.0327(18) 0.0016(14) -0.0048(15) -0.0191(16) C16 0.0224(15) 0.0183(15) 0.0320(17) -0.0045(12) -0.0038(13) -0.0103(12) C17 0.0192(14) 0.0188(14) 0.0268(15) -0.0052(12) -0.0057(12) -0.0065(12) C18 0.0188(14) 0.0227(15) 0.0263(15) -0.0109(12) 0.0016(12) -0.0115(12) C19 0.0199(15) 0.0280(17) 0.0337(18) -0.0130(14) 0.0068(13) -0.0101(13) C20 0.0154(13) 0.0201(14) 0.0179(13) -0.0005(11) 0.0007(10) -0.0074(11) C21 0.0370(19) 0.0246(17) 0.0215(16) 0.0008(13) -0.0059(14) -0.0034(15) C22 0.0186(14) 0.0138(13) 0.0250(15) -0.0045(11) 0.0025(11) -0.0070(11) C23 0.0204(15) 0.0175(15) 0.0288(16) -0.0019(12) -0.0010(12) -0.0052(12) C24 0.0229(16) 0.0153(15) 0.0385(19) -0.0033(13) 0.0035(14) -0.0017(12) C25 0.0330(18) 0.0174(15) 0.0353(18) -0.0109(13) 0.0055(15) -0.0061(14) C26 0.0313(18) 0.0244(17) 0.0311(17) -0.0132(14) 0.0019(14) -0.0089(14) C27 0.0210(15) 0.0195(15) 0.0248(15) -0.0057(12) 0.0019(12) -0.0077(12) C28 0.0200(15) 0.0223(15) 0.0226(15) -0.0071(12) -0.0018(12) -0.0068(12) C29 0.0130(13) 0.0159(13) 0.0202(14) -0.0022(11) -0.0008(10) -0.0050(11) F1 0.0692(19) 0.074(2) 0.0545(16) -0.0312(15) 0.0284(14) -0.0596(17) N1 0.0141(11) 0.0157(12) 0.0222(12) -0.0048(9) -0.0025(9) -0.0056(9) N2 0.0149(11) 0.0117(11) 0.0216(12) -0.0031(9) -0.0018(9) -0.0029(9) O1 0.0176(10) 0.0148(10) 0.0326(12) -0.0037(9) -0.0061(9) -0.0028(8) O2 0.0250(12) 0.0265(12) 0.0216(11) -0.0026(9) -0.0099(9) -0.0085(10) O3 0.0168(10) 0.0186(10) 0.0211(10) -0.0055(8) 0.0020(8) -0.0073(8) O4 0.0259(12) 0.0174(11) 0.0411(14) -0.0057(10) 0.0013(10) -0.0069(9) O5 0.0206(10) 0.0157(10) 0.0175(10) -0.0030(8) -0.0026(8) -0.0056(8) S1 0.0138(3) 0.0147(3) 0.0201(3) -0.0028(3) -0.0041(3) -0.0045(3) F2 0.039(3) 0.076(4) 0.0108(18) -0.018(2) 0.0086(16) -0.033(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O3 Ir1 N1 87.38(9) O3 Ir1 C4 164.23(11) N1 Ir1 C4 107.45(11) O3 Ir1 C5 147.57(10) N1 Ir1 C5 94.43(11) C4 Ir1 C5 39.32(12) O3 Ir1 C1 112.04(10) N1 Ir1 C1 117.10(11) C4 Ir1 C1 66.46(12) C5 Ir1 C1 39.61(12) O3 Ir1 O5 77.01(8) N1 Ir1 O5 78.80(9) C4 Ir1 O5 100.17(10) C5 Ir1 O5 135.13(10) C1 Ir1 O5 161.15(11) O3 Ir1 C3 124.78(11) N1 Ir1 C3 145.57(11) C4 Ir1 C3 39.57(12) C5 Ir1 C3 65.68(12) C1 Ir1 C3 65.70(12) O5 Ir1 C3 95.49(11) O3 Ir1 C2 102.53(10) N1 Ir1 C2 156.45(11) C4 Ir1 C2 65.88(12) C5 Ir1 C2 65.78(12) C1 Ir1 C2 39.38(12) O5 Ir1 C2 124.02(10) C3 Ir1 C2 38.55(12) C5 C1 C2 107.6(3) C5 C1 C6 125.5(3) C2 C1 C6 126.3(3) C5 C1 Ir1 70.03(17) C2 C1 Ir1 71.81(17) C6 C1 Ir1 130.3(2) C3 C2 C1 107.6(3) C3 C2 C7 126.3(3) C1 C2 C7 126.1(3) C3 C2 Ir1 69.84(17) C1 C2 Ir1 68.81(17) C7 C2 Ir1 127.5(2) C2 C3 C4 108.8(3) C2 C3 C8 125.5(3) C4 C3 C8 125.7(3) C2 C3 Ir1 71.61(17) C4 C3 Ir1 69.28(17) C8 C3 Ir1 125.4(2) C5 C4 C3 107.4(3) C5 C4 C9 126.8(3) C3 C4 C9 125.7(3) C5 C4 Ir1 70.48(17) C3 C4 Ir1 71.15(17) C9 C4 Ir1 127.1(2) C4 C5 C1 108.5(3) C4 C5 C10 125.8(3) C1 C5 C10 125.7(3) C4 C5 Ir1 70.20(17) C1 C5 Ir1 70.36(17) C10 C5 Ir1 123.4(2) C1 C6 H6A 109.5 C1 C6 H6B 109.5 H6A C6 H6B 109.5 C1 C6 H6C 109.5 H6A C6 H6C 109.5 H6B C6 H6C 109.5 C2 C7 H7A 109.5 C2 C7 H7B 109.5 H7A C7 H7B 109.5 C2 C7 H7C 109.5 H7A C7 H7C 109.5 H7B C7 H7C 109.5 C3 C8 H8A 109.5 C3 C8 H8B 109.5 H8A C8 H8B 109.5 C3 C8 H8C 109.5 H8A C8 H8C 109.5 H8B C8 H8C 109.5 C4 C9 H9A 109.5 C4 C9 H9B 109.5 H9A C9 H9B 109.5 C4 C9 H9C 109.5 H9A C9 H9C 109.5 H9B C9 H9C 109.5 C5 C10 H10A 109.5 C5 C10 H10B 109.5 H10A C10 H10B 109.5 C5 C10 H10C 109.5 H10A C10 H10C 109.5 H10B C10 H10C 109.5 C17 C11 C12 120.9(3) C17 C11 S1 121.4(2) C12 C11 S1 117.7(2) C13 C12 C11 119.5(3) C13 C12 H12 120.3 C11 C12 H12 120.3 C12 C13 C14 120.8(3) C12 C13 H13 119.6 C14 C13 H13 119.6 C16 C14 C13 118.9(3) C16 C14 C15 121.2(3) C13 C14 C15 119.9(3) C14 C15 H15A 109.5 C14 C15 H15B 109.5 H15A C15 H15B 109.5 C14 C15 H15C 109.5 H15A C15 H15C 109.5 H15B C15 H15C 109.5 C14 C16 C17 121.1(3) C14 C16 H16 119.4 C17 C16 H16 119.4 C11 C17 C16 118.9(3) C11 C17 H17 120.6 C16 C17 H17 120.6 O4 C18 O3 131.5(3) O4 C18 C19 117.1(3) O3 C18 C19 111.4(3) F5 C19 F2 79.8(5) F5 C19 F1 114.4(4) F2 C19 F1 119.1(4) F5 C19 F3 26.8(3) F2 C19 F3 106.5(4) F1 C19 F3 98.3(3) F5 C19 F4 102.7(5) F2 C19 F4 28.2(4) F1 C19 F4 94.5(4) F3 C19 F4 127.2(5) F5 C19 C18 116.8(4) F2 C19 C18 110.3(3) F1 C19 C18 112.8(3) F3 C19 C18 108.5(3) F4 C19 C18 112.9(4) O5 C20 N2 122.6(3) O5 C20 C21 117.1(3) N2 C20 C21 120.3(3) C20 C21 H21A 109.5 C20 C21 H21B 109.5 H21A C21 H21B 109.5 C20 C21 H21C 109.5 H21A C21 H21C 109.5 H21B C21 H21C 109.5 C23 C22 C27 121.6(3) C23 C22 N2 131.6(3) C27 C22 N2 106.8(3) C22 C23 C24 117.3(3) C22 C23 H23 121.3 C24 C23 H23 121.3 C25 C24 C23 121.4(3) C25 C24 H24 119.3 C23 C24 H24 119.3 C24 C25 C26 121.0(3) C24 C25 H25 119.5 C26 C25 H25 119.5 C25 C26 C27 118.4(3) C25 C26 H26 120.8 C27 C26 H26 120.8 C26 C27 C22 120.1(3) C26 C27 C28 131.1(3) C22 C27 C28 108.8(3) C29 C28 C27 108.6(3) C29 C28 H28 125.7 C27 C28 H28 125.7 C28 C29 N1 131.4(3) C28 C29 N2 108.6(3) N1 C29 N2 119.7(3) C29 N1 S1 114.6(2) C29 N1 Ir1 116.50(19) S1 N1 Ir1 128.87(14) C20 N2 C22 127.6(3) C20 N2 C29 124.8(2) C22 N2 C29 107.1(2) C18 O3 Ir1 124.1(2) C20 O5 Ir1 126.5(2) O1 S1 O2 116.54(14) O1 S1 N1 107.00(13) O2 S1 N1 112.95(14) O1 S1 C11 110.10(14) O2 S1 C11 107.23(15) N1 S1 C11 102.07(14) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ir1 O3 2.108(2) Ir1 N1 2.114(2) Ir1 C4 2.124(3) Ir1 C5 2.128(3) Ir1 C1 2.132(3) Ir1 O5 2.148(2) Ir1 C3 2.149(3) Ir1 C2 2.172(3) C1 C5 1.443(4) C1 C2 1.451(4) C1 C6 1.490(4) C2 C3 1.427(5) C2 C7 1.498(4) C3 C4 1.447(5) C3 C8 1.481(5) C4 C5 1.431(4) C4 C9 1.493(4) C5 C10 1.499(4) C6 H6A 0.9600 C6 H6B 0.9600 C6 H6C 0.9600 C7 H7A 0.9600 C7 H7B 0.9600 C7 H7C 0.9600 C8 H8A 0.9600 C8 H8B 0.9600 C8 H8C 0.9600 C9 H9A 0.9600 C9 H9B 0.9600 C9 H9C 0.9600 C10 H10A 0.9600 C10 H10B 0.9600 C10 H10C 0.9600 C11 C17 1.386(4) C11 C12 1.394(4) C11 S1 1.773(3) C12 C13 1.385(5) C12 H12 0.9300 C13 C14 1.395(5) C13 H13 0.9300 C14 C16 1.391(5) C14 C15 1.502(5) C15 H15A 0.9600 C15 H15B 0.9600 C15 H15C 0.9600 C16 C17 1.397(5) C16 H16 0.9300 C17 H17 0.9300 C18 O4 1.208(4) C18 O3 1.275(4) C18 C19 1.555(4) C19 F5 1.299(7) C19 F2 1.274(6) C19 F1 1.302(4) C19 F3 1.388(6) C19 F4 1.393(9) C20 O5 1.242(4) C20 N2 1.361(4) C20 C21 1.499(4) C21 H21A 0.9600 C21 H21B 0.9600 C21 H21C 0.9600 C22 C23 1.386(4) C22 C27 1.399(5) C22 N2 1.431(4) C23 C24 1.401(5) C23 H23 0.9300 C24 C25 1.380(6) C24 H24 0.9300 C25 C26 1.388(5) C25 H25 0.9300 C26 C27 1.396(4) C26 H26 0.9300 C27 C28 1.432(4) C28 C29 1.351(4) C28 H28 0.9300 C29 N1 1.388(4) C29 N2 1.449(4) N1 S1 1.615(3) O1 S1 1.435(2) O2 S1 1.442(2) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C28 H28 O2 0.93 2.57 3.428(4) 153.5 2_667 C28 H28 O2 0.93 2.45 2.944(4) 113.5 . C12 H12 O3 0.93 2.55 3.409(4) 154.5 . C12 H12 F1 0.93 2.57 3.132(4) 119.1 . 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 C5 C1 C2 C3 1.9(3) C6 C1 C2 C3 173.6(3) Ir1 C1 C2 C3 -59.3(2) C5 C1 C2 C7 -177.1(3) C6 C1 C2 C7 -5.4(5) Ir1 C1 C2 C7 121.7(3) C5 C1 C2 Ir1 61.2(2) C6 C1 C2 Ir1 -127.1(3) C1 C2 C3 C4 -0.9(3) C7 C2 C3 C4 178.1(3) Ir1 C2 C3 C4 -59.5(2) C1 C2 C3 C8 179.4(3) C7 C2 C3 C8 -1.6(5) Ir1 C2 C3 C8 120.8(3) C1 C2 C3 Ir1 58.6(2) C7 C2 C3 Ir1 -122.4(3) C2 C3 C4 C5 -0.5(3) C8 C3 C4 C5 179.2(3) Ir1 C3 C4 C5 -61.5(2) C2 C3 C4 C9 -176.3(3) C8 C3 C4 C9 3.3(5) Ir1 C3 C4 C9 122.7(3) C2 C3 C4 Ir1 61.0(2) C8 C3 C4 Ir1 -119.3(3) C3 C4 C5 C1 1.7(3) C9 C4 C5 C1 177.5(3) Ir1 C4 C5 C1 -60.2(2) C3 C4 C5 C10 179.4(3) C9 C4 C5 C10 -4.9(5) Ir1 C4 C5 C10 117.5(3) C3 C4 C5 Ir1 61.9(2) C9 C4 C5 Ir1 -122.3(3) C2 C1 C5 C4 -2.3(3) C6 C1 C5 C4 -174.0(3) Ir1 C1 C5 C4 60.1(2) C2 C1 C5 C10 -179.9(3) C6 C1 C5 C10 8.3(5) Ir1 C1 C5 C10 -117.6(3) C2 C1 C5 Ir1 -62.4(2) C6 C1 C5 Ir1 125.9(3) C17 C11 C12 C13 1.8(5) S1 C11 C12 C13 178.0(3) C11 C12 C13 C14 -0.3(5) C12 C13 C14 C16 -0.8(5) C12 C13 C14 C15 -179.4(3) C13 C14 C16 C17 0.4(5) C15 C14 C16 C17 179.0(3) C12 C11 C17 C16 -2.1(5) S1 C11 C17 C16 -178.2(2) C14 C16 C17 C11 1.0(5) O4 C18 C19 F5 19.1(6) O3 C18 C19 F5 -160.9(4) O4 C18 C19 F2 107.7(5) O3 C18 C19 F2 -72.3(5) O4 C18 C19 F1 -116.4(4) O3 C18 C19 F1 63.6(4) O4 C18 C19 F3 -8.6(5) O3 C18 C19 F3 171.4(3) O4 C18 C19 F4 137.9(5) O3 C18 C19 F4 -42.1(5) C27 C22 C23 C24 4.4(5) N2 C22 C23 C24 -179.3(3) C22 C23 C24 C25 -0.8(5) C23 C24 C25 C26 -2.6(6) C24 C25 C26 C27 2.4(5) C25 C26 C27 C22 1.2(5) C25 C26 C27 C28 -178.0(3) C23 C22 C27 C26 -4.6(5) N2 C22 C27 C26 178.2(3) C23 C22 C27 C28 174.7(3) N2 C22 C27 C28 -2.4(3) C26 C27 C28 C29 -179.1(4) C22 C27 C28 C29 1.7(4) C27 C28 C29 N1 173.1(3) C27 C28 C29 N2 -0.2(3) C28 C29 N1 S1 -38.6(4) N2 C29 N1 S1 134.1(2) C28 C29 N1 Ir1 142.4(3) N2 C29 N1 Ir1 -44.9(3) O5 C20 N2 C22 -169.4(3) C21 C20 N2 C22 9.7(5) O5 C20 N2 C29 19.6(5) C21 C20 N2 C29 -161.2(3) C23 C22 N2 C20 13.3(5) C27 C22 N2 C20 -170.0(3) C23 C22 N2 C29 -174.5(3) C27 C22 N2 C29 2.3(3) C28 C29 N2 C20 171.2(3) N1 C29 N2 C20 -3.0(4) C28 C29 N2 C22 -1.3(3) N1 C29 N2 C22 -175.5(3) O4 C18 O3 Ir1 7.3(5) C19 C18 O3 Ir1 -172.74(19) N2 C20 O5 Ir1 16.5(4) C21 C20 O5 Ir1 -162.7(2) C29 N1 S1 O1 -175.8(2) Ir1 N1 S1 O1 3.1(2) C29 N1 S1 O2 54.7(3) Ir1 N1 S1 O2 -126.47(18) C29 N1 S1 C11 -60.1(2) Ir1 N1 S1 C11 118.74(19) C17 C11 S1 O1 -129.6(3) C12 C11 S1 O1 54.2(3) C17 C11 S1 O2 -1.9(3) C12 C11 S1 O2 -178.1(2) C17 C11 S1 N1 117.1(3) C12 C11 S1 N1 -59.1(3)