#------------------------------------------------------------------------------ #$Date: 2021-10-15 04:06:22 +0300 (Fri, 15 Oct 2021) $ #$Revision: 269966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/37/7243742.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_7243742 loop_ _publ_author_name 'Mart\'inez-Vollbert, Emiliano' 'Philouze, Christian' 'Gautier-Luneau, Isabelle' 'Moreau, Yohann' 'Lano\"e, Pierre-Henri' 'Loiseau, Frederique' _publ_section_title ; Study of a phosphorescent cationic iridium(III) complex displaying blue shift in crystals ; _journal_name_full 'Physical Chemistry Chemical Physics' _journal_paper_doi 10.1039/D1CP03341G _journal_year 2021 _chemical_formula_moiety 'C48 H50 Ir N6 O4, F6 P, 3(C2 H4 Cl2)' _chemical_formula_sum 'C54 H62 Cl6 F6 Ir N6 O4 P' _chemical_formula_weight 1408.96 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2021-03-24 _audit_creation_method ; Olex2 1.2 (compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862) ; _audit_update_record ; 2021-03-24 deposited with the CCDC. 2021-10-13 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 117.07(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 19.554(4) _cell_length_b 22.055(4) _cell_length_c 15.394(3) _cell_measurement_reflns_used 41641 _cell_measurement_temperature 200 _cell_measurement_theta_max 30.000 _cell_measurement_theta_min 2.809 _cell_volume 5912(3) _computing_cell_refinement EvalCCD _computing_data_collection Collect _computing_data_reduction EvalCCD _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'ShelXT-2016 (Sheldrick, 2008)' _diffrn_ambient_temperature 200 _diffrn_detector 'CCD area detector' _diffrn_detector_type 'APEX II' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device '\k-geometry 4 circles diffractometer' _diffrn_measurement_device_type 'Bruker-AXS-enraf-nonius KappaAPEXII' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_collimation 'Montel optic' _diffrn_radiation_detector CCD _diffrn_radiation_monochromator 'Multilayer mirrors' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_unetI/netI 0.0236 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 41641 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.998 _diffrn_reflns_theta_min 2.809 _diffrn_source 'Incoatec ISG250' _diffrn_source_target Mo _diffrn_source_type 'Microfocus sealed tube' _exptl_absorpt_coefficient_mu 2.625 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.576016 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2004/1 (Bruker,2004) was used for absorption correction. R(int) was 0.0922 before and 0.0353 after correction. The Ratio of minimum to maximum transmission is 0.5760. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.583 _exptl_crystal_description plate _exptl_crystal_F_000 2832 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _refine_diff_density_max 2.163 _refine_diff_density_min -1.139 _refine_diff_density_rms 0.090 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.167 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 424 _refine_ls_number_reflns 8603 _refine_ls_number_restraints 175 _refine_ls_restrained_S_all 1.803 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0265 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0278P)^2^+12.8958P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0645 _refine_ls_wR_factor_ref 0.0742 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7680 _reflns_number_total 8603 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1cp03341g2.cif _cod_data_source_block sad _cod_original_cell_volume 5911(2) _cod_database_code 7243742 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances Cl1B-C25B 1.7 with sigma of 0.02 C26B-Cl2B 1.7 with sigma of 0.02 C25B-C26B 1.5 with sigma of 0.02 C25B-Cl2B 2.6 with sigma of 0.02 Cl1B-C26B 2.6 with sigma of 0.02 C27A-Cl3 1.7 with sigma of 0.01 C27A-C27A_$1 1.6 with sigma of 0.01 C27A-Cl3_$1 2.6 with sigma of 0.01 C27B-Cl3 1.7 with sigma of 0.01 C27B-C27B_$1 1.6 with sigma of 0.01 C27B-Cl3_$1 2.6 with sigma of 0.01 C27B-Cl3 1.7 with sigma of 0.01 C19-C19_$2 1.38 with sigma of 0.005 N3-C19 1.45 with sigma of 0.005 C19-C20 1.45 with sigma of 0.005 3. Rigid bond restraints Cl1B, Cl2B, C26B, C25B, Cl1A, C25A, C26A, Cl2A with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C27A, Cl3 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 P1, F1, F2A, F3A, F3B, F2B with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 Cl3, C27A, C27B with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 4. Uiso/Uaniso restraints and constraints Cl1B \\sim Cl2B \\sim C26B \\sim C25B \\sim Cl1A \\sim C25A \\sim C26A \\sim Cl2A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 Cl3 \\sim C27A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 P1 \\sim F1 \\sim F2A \\sim F3A \\sim F3B \\sim F2B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 Cl3 \\sim C27A \\sim C27B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 5. Others Sof(Cl2B)=Sof(Cl1B)=Sof(C25B)=Sof(H25C)=Sof(H25D)=Sof(C26B)=Sof(H26C)= Sof(H26D)=1-FVAR(1) Sof(Cl1A)=Sof(Cl2A)=Sof(C25A)=Sof(H25A)=Sof(H25B)=Sof(C26A)=Sof(H26A)= Sof(H26B)=FVAR(1) Sof(F2A)=Sof(F3A)=1-FVAR(2) Sof(F3B)=Sof(F2B)=FVAR(2) Sof(C27B)=Sof(H27C)=Sof(H27D)=1-FVAR(3) Sof(C27A)=Sof(H27A)=Sof(H27B)=FVAR(3) 6.a Ternary CH refined with riding coordinates: C14(H14) 6.b Secondary CH2 refined with riding coordinates: C25A(H25A,H25B), C26A(H26A,H26B), C25B(H25C,H25D), C26B(H26C,H26D), C27A(H27A, H27B), C27B(H27C,H27D) 6.c Aromatic/amide H refined with riding coordinates: C20(H20), C23(H23), C12(H12), C9(H9), C5(H5), C2(H2), C22(H22), C10(H10), C4(H4) 6.d Idealised Me refined as rotating group: C24(H24A,H24B,H24C), C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C15(H15A,H15B, H15C), C16(H16A,H16B,H16C) ; _shelx_res_file ; sad.res created by SHELXL-2014/7 TITL sad_a.res in C2/c CELL 0.71073 19.5541 22.0549 15.3936 90 117.07 90 ZERR 4 0.0039 0.0044 0.0031 0 0.03 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Cl F Ir N O P UNIT 216 248 24 24 4 24 16 4 EQIV $1 1-X,+Y,0.5-Z EQIV $2 1-X,+Y,1.5-Z EQIV $3 -0.5+X,0.5+Y,+Z DFIX 1.7 Cl1B C25B DFIX 1.7 C26B Cl2B DFIX 1.5 C25B C26B DFIX 2.6 C25B Cl2B DFIX 2.6 Cl1B C26B DFIX 1.7 0.01 C27A Cl3 DFIX 1.6 0.01 C27A C27A_$1 DFIX 2.6 0.01 C27A Cl3_$1 DFIX 1.7 0.01 C27B Cl3 DFIX 1.6 0.01 C27B C27B_$1 DFIX 2.6 0.01 C27B Cl3_$1 DFIX 1.7 0.01 C27B Cl3 DFIX 1.38 0.005 C19 C19_$2 DFIX 1.45 0.005 N3 C19 DFIX 1.45 0.005 C19 C20 DELU Cl1B Cl2B C26B C25B Cl1A C25A C26A Cl2A DELU C27A Cl3 DELU P1 F1 F2A F3A F3B F2B DELU Cl3 C27A C27B SIMU 0.04 0.08 1.7 Cl1B Cl2B C26B C25B Cl1A C25A C26A Cl2A SIMU 0.04 0.08 1.7 Cl3 C27A SIMU 0.04 0.08 1.7 P1 F1 F2A F3A F3B F2B SIMU 0.04 0.08 1.7 Cl3 C27A C27B L.S. 20 0 0 PLAN 20 TEMP -73.15 HTAB C20 F1_$3 HTAB C9 N3 HTAB C2 N1 HTAB C18 F2A HTAB C18 F2B REM Old TITL sad in C2/c #15 BUMP BOND $H HTAB LIST 4 fmap 2 53 ACTA OMIT 0 2 1 OMIT 1 1 0 OMIT -2 2 1 REM /home/olex/SAUVEGARDE/Stock/CIRE/PH_Lanoe/PHLEMV2OMebpy191216/Sadabs/ REM sad.hkl WGHT 0.027800 12.895801 FVAR 0.11017 0.72380 0.49402 0.51344 IR1 5 0.500000 0.705902 0.750000 10.50000 0.03001 0.02099 = 0.02330 0.00000 0.01258 0.00000 P1 8 1.000000 0.575564 0.750000 10.50000 0.08454 0.03170 = 0.07947 0.00000 0.05484 0.00000 PART 1 CL1A 3 0.844015 0.425228 0.829810 21.00000 0.09798 0.05037 = 0.08537 0.00128 0.04188 -0.00615 CL2A 3 0.850693 0.277188 1.012589 21.00000 0.12777 0.06880 = 0.07847 0.00022 0.05210 -0.01284 PART 0 N3 6 0.532534 0.781098 0.847003 11.00000 0.03070 0.02620 = 0.02474 -0.00083 0.01318 0.00201 N1 6 0.595831 0.698959 0.730130 11.00000 0.03224 0.02335 = 0.02621 -0.00211 0.01291 -0.00177 CL3 3 0.383318 0.536717 0.220059 11.00000 0.24198 0.15683 = 0.06936 -0.00200 0.04977 0.06411 O2 7 0.884109 0.789579 0.836839 11.00000 0.03902 0.04889 = 0.06068 -0.01554 0.02758 -0.01397 N2 6 0.663359 0.651220 0.667341 11.00000 0.03288 0.02627 = 0.03092 -0.00692 0.01587 -0.00169 O1 7 0.304911 0.550001 0.467041 11.00000 0.03914 0.04751 = 0.05394 -0.01906 0.01446 -0.01177 C19 1 0.517082 0.837412 0.804187 11.00000 0.02771 0.02530 = 0.02778 -0.00048 0.01410 0.00045 C1 1 0.466596 0.641096 0.645610 11.00000 0.03375 0.02073 = 0.02510 0.00011 0.01287 -0.00035 C7 1 0.594423 0.655625 0.668775 11.00000 0.03348 0.02460 = 0.02608 -0.00207 0.01371 0.00016 C8 1 0.667823 0.725353 0.768194 11.00000 0.03206 0.02446 = 0.02821 -0.00125 0.01510 -0.00068 C6 1 0.521779 0.624315 0.614733 11.00000 0.03476 0.02364 = 0.02820 -0.00261 0.01380 -0.00190 C13 1 0.710494 0.696680 0.727706 11.00000 0.03354 0.02486 = 0.02761 -0.00098 0.01408 0.00091 C20 1 0.532881 0.890172 0.860648 11.00000 0.04071 0.02433 = 0.03678 -0.00133 0.01875 0.00270 AFIX 43 H20 2 0.522325 0.928749 0.829821 11.00000 -1.20000 AFIX 0 C23 1 0.562305 0.778688 0.943716 11.00000 0.04251 0.03107 = 0.02629 0.00108 0.01393 0.00499 AFIX 43 H23 2 0.572901 0.740055 0.974362 11.00000 -1.20000 AFIX 0 C21 1 0.563270 0.886436 0.959416 11.00000 0.03866 0.03291 = 0.03485 -0.00836 0.01653 0.00278 C12 1 0.783893 0.716093 0.746686 11.00000 0.03494 0.03376 = 0.03555 -0.00378 0.01926 -0.00047 AFIX 43 H12 2 0.812274 0.696891 0.718134 11.00000 -1.20000 AFIX 0 C9 1 0.699286 0.773662 0.832895 11.00000 0.03582 0.03394 = 0.03774 -0.01033 0.01792 -0.00216 AFIX 43 H9 2 0.671424 0.792685 0.862314 11.00000 -1.20000 AFIX 0 C5 1 0.501080 0.586852 0.533043 11.00000 0.04044 0.03351 = 0.03601 -0.00952 0.01786 -0.00155 AFIX 43 H5 2 0.537591 0.577826 0.510152 11.00000 -1.20000 AFIX 0 C11 1 0.813044 0.764931 0.809490 11.00000 0.03229 0.03346 = 0.03765 -0.00326 0.01568 -0.00472 C2 1 0.393320 0.615514 0.597799 11.00000 0.03459 0.02802 = 0.03289 -0.00233 0.01492 -0.00224 AFIX 43 H2 2 0.355857 0.624662 0.619051 11.00000 -1.20000 AFIX 0 C22 1 0.578497 0.829707 1.001540 11.00000 0.04759 0.03751 = 0.02616 -0.00302 0.01383 0.00478 AFIX 43 H22 2 0.600149 0.825739 1.070417 11.00000 -1.20000 AFIX 0 C3 1 0.375145 0.576618 0.519015 11.00000 0.03570 0.02822 = 0.03535 -0.00348 0.01067 -0.00408 C10 1 0.771691 0.792852 0.852730 11.00000 0.03668 0.03408 = 0.04200 -0.01416 0.01607 -0.00629 AFIX 43 H10 2 0.794211 0.825662 0.896570 11.00000 -1.20000 AFIX 0 C4 1 0.428210 0.563097 0.485865 11.00000 0.04213 0.03489 = 0.03386 -0.01051 0.01201 -0.00319 AFIX 43 H4 2 0.414428 0.537517 0.430755 11.00000 -1.20000 AFIX 0 F1 4 0.951328 0.525540 0.768412 11.00000 0.14409 0.06323 = 0.24904 0.02768 0.14849 0.01253 C14 1 0.688456 0.599110 0.627499 11.00000 0.04052 0.03109 = 0.04443 -0.01222 0.02212 -0.00081 AFIX 13 H14 2 0.646476 0.568224 0.605902 11.00000 -1.20000 AFIX 0 C24 1 0.578156 0.942835 1.019725 11.00000 0.06542 0.03918 = 0.04235 -0.01538 0.02151 0.00228 AFIX 137 H24A 2 0.572192 0.978424 0.978760 11.00000 -1.50000 H24B 2 0.630558 0.941717 1.073193 11.00000 -1.50000 H24C 2 0.541448 0.945229 1.046642 11.00000 -1.50000 AFIX 0 C18 1 0.925490 0.770564 0.786945 11.00000 0.05719 0.07518 = 0.09112 -0.02795 0.05199 -0.02649 AFIX 137 H18A 2 0.894479 0.777449 0.716814 11.00000 -1.50000 H18B 2 0.937400 0.727282 0.798939 11.00000 -1.50000 H18C 2 0.973366 0.793738 0.810386 11.00000 -1.50000 AFIX 0 C17 1 0.246036 0.562405 0.493818 11.00000 0.04110 0.06613 = 0.07020 -0.02233 0.02221 -0.01529 AFIX 137 H17A 2 0.198895 0.541443 0.449026 11.00000 -1.50000 H17B 2 0.236602 0.606188 0.490421 11.00000 -1.50000 H17C 2 0.261834 0.548177 0.560553 11.00000 -1.50000 AFIX 0 C15 1 0.696810 0.616921 0.538649 11.00000 0.10578 0.05401 = 0.06916 -0.01857 0.06548 -0.00972 AFIX 137 H15A 2 0.648968 0.635559 0.490710 11.00000 -1.50000 H15B 2 0.707886 0.580814 0.510125 11.00000 -1.50000 H15C 2 0.739029 0.646013 0.557128 11.00000 -1.50000 AFIX 0 C16 1 0.759463 0.569636 0.706550 11.00000 0.05074 0.04325 = 0.07736 -0.01528 0.01444 0.01261 AFIX 137 H16A 2 0.803852 0.596255 0.723411 11.00000 -1.50000 H16B 2 0.768632 0.530723 0.682917 11.00000 -1.50000 H16C 2 0.751855 0.562855 0.764478 11.00000 -1.50000 AFIX 0 PART 2 F2A 4 0.964590 0.621695 0.797670 -31.00000 0.18492 0.07115 = 0.23447 -0.05492 0.15679 -0.00214 PART 0 PART 1 C25A 1 0.814771 0.370778 0.895222 21.00000 0.07672 0.09362 = 0.09488 0.01109 0.04714 0.00153 AFIX 23 H25A 2 0.799864 0.392061 0.940660 21.00000 -1.20000 H25B 2 0.770239 0.346908 0.848761 21.00000 -1.20000 AFIX 0 C26A 1 0.878794 0.331772 0.948128 21.00000 0.09134 0.07617 = 0.08326 -0.00371 0.04940 0.00097 AFIX 23 H26A 2 0.923165 0.355706 0.994786 21.00000 -1.20000 H26B 2 0.893940 0.310863 0.902615 21.00000 -1.20000 AFIX 0 PART 0 PART 2 F3A 4 1.058876 0.553447 0.854483 -31.00000 0.19776 0.13382 = 0.11706 0.05805 0.03440 0.02680 CL2B 3 0.892099 0.267536 1.008233 -21.00000 0.25563 0.10571 = 0.08099 -0.01750 0.07029 -0.06033 CL1B 3 0.799146 0.423124 0.839624 -21.00000 0.21981 0.10892 = 0.18440 -0.02700 0.01967 0.05888 C25B 1 0.852902 0.357718 0.881860 -21.00000 0.11748 0.10176 = 0.10423 0.00975 0.06664 0.01064 AFIX 23 H25C 2 0.826163 0.323528 0.837734 -21.00000 -1.20000 H25D 2 0.903415 0.363116 0.882569 -21.00000 -1.20000 AFIX 0 C26B 1 0.864027 0.343986 0.980446 -21.00000 0.13121 0.15162 = 0.08771 -0.03614 0.07310 0.02414 AFIX 23 H26C 2 0.815633 0.351187 0.984616 -21.00000 -1.20000 H26D 2 0.904079 0.370867 1.028104 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C27A 1 0.463442 0.537936 0.200821 41.00000 0.38030 0.31571 = 0.16171 -0.17308 0.20849 -0.26170 AFIX 23 H27A 2 0.463364 0.501945 0.162343 41.00000 -1.20000 H27B 2 0.462505 0.574644 0.163279 41.00000 -1.20000 AFIX 0 F3B 4 1.052399 0.591008 0.849798 31.00000 0.25354 0.15450 = 0.09975 -0.05483 -0.00574 -0.01380 F2B 4 0.938779 0.624840 0.732235 31.00000 0.13168 0.04392 = 0.22277 0.00415 0.11290 0.02807 PART 0 PART 2 C27B 1 0.481243 0.537011 0.284449 -41.00000 0.24971 0.41604 = 0.14019 -0.03029 0.03986 -0.25692 AFIX 23 H27C 2 0.498000 0.573420 0.326627 -41.00000 -1.20000 H27D 2 0.498340 0.500779 0.327003 -41.00000 -1.20000 AFIX 0 HKLF 4 REM sad_a.res in C2/c REM R1 = 0.0265 for 7680 Fo > 4sig(Fo) and 0.0362 for all 8603 data REM 424 parameters refined using 175 restraints END WGHT 0.0278 12.8952 REM Instructions for potential hydrogen bonds HTAB C20 F1_$3 HTAB C9 N3 HTAB C2 N1_$2 HTAB C18 F2A HTAB C18 F2B EQIV $4 -x+2, -y+1, -z+2 HTAB C26A F3B_$4 HTAB C26B F3A_$4 REM Highest difference peak 2.163, deepest hole -1.139, 1-sigma level 0.090 Q1 1 0.5000 0.8805 0.7500 10.50000 0.05 2.16 Q2 1 0.5000 0.5083 0.2500 10.50000 0.05 0.97 Q3 1 0.9362 0.5374 0.7023 11.00000 0.05 0.65 Q4 1 0.9984 0.5610 0.8353 11.00000 0.05 0.61 Q5 1 0.4697 0.7164 0.7506 11.00000 0.05 0.54 Q6 1 0.5430 0.6749 0.7953 11.00000 0.05 0.47 Q7 1 0.5193 0.6568 0.7175 11.00000 0.05 0.47 Q8 1 0.4734 0.7215 0.7092 11.00000 0.05 0.44 Q9 1 0.5000 0.8366 0.7500 10.50000 0.05 0.44 Q10 1 0.4790 0.5625 0.2228 11.00000 0.05 0.42 Q11 1 0.5783 0.8596 0.9800 11.00000 0.05 0.40 Q12 1 0.7826 0.7421 0.7652 11.00000 0.05 0.39 Q13 1 0.4778 0.5787 0.2544 11.00000 0.05 0.38 Q14 1 0.5600 0.6392 0.6388 11.00000 0.05 0.36 Q15 1 0.4463 0.5786 0.2426 11.00000 0.05 0.36 Q16 1 0.5417 0.7792 0.9028 11.00000 0.05 0.32 Q17 1 0.8632 0.4026 0.8512 11.00000 0.05 0.31 Q18 1 0.6784 0.7571 0.7894 11.00000 0.05 0.31 Q19 1 0.4606 0.5819 0.4992 11.00000 0.05 0.31 Q20 1 0.6990 0.7029 0.7572 11.00000 0.05 0.30 ; _shelx_res_checksum 25602 _shelx_hkl_file ; 4 0 0 676.09 22.31 -4 0 0 632.94 21.92 -6 0 0 861.82 29.75 6 0 0 798.26 28.76 8 0 0 241.21 8.48 8 0 0 257.65 15.20 -8 0 0 263.02 7.64 8 0 0 265.12 7.62 -8 0 0 250.52 8.46 8 0 0 251.45 7.62 -8 0 0 278.09 15.83 10 0 0 607.69 21.20 -10 0 0 679.91 21.13 10 0 0 673.14 29.26 10 0 0 647.05 18.49 -10 0 0 639.75 18.48 10 0 0 711.85 18.80 -10 0 0 620.16 28.99 12 0 0 319.73 13.92 -12 0 0 374.23 22.44 -12 0 0 363.31 12.10 -12 0 0 369.67 10.90 12 0 0 374.94 22.06 12 0 0 376.71 10.91 12 0 0 384.61 10.90 -14 0 0 180.29 7.07 -14 0 0 206.16 6.62 14 0 0 226.01 6.62 14 0 0 205.98 6.62 14 0 0 181.74 8.26 -16 0 0 170.12 5.95 16 0 0 174.16 5.97 -18 0 0 55.84 3.03 18 0 0 72.55 3.16 -18 0 0 74.08 4.35 20 0 0 61.84 3.00 -20 0 0 55.39 4.15 22 0 0 21.47 1.72 -22 0 0 17.31 2.70 -24 0 0 29.50 3.30 -1 -1 0 -0.77 0.38 1 1 0 -0.45 0.20 -3 -1 0 116.73 7.41 3 1 0 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-19 18.75 2.34 -10 10 19 20.75 2.60 -8 10 19 11.61 1.75 -8 -10 19 11.87 1.99 8 -10 -19 12.10 1.81 -8 10 19 12.48 2.35 -6 -10 19 4.87 1.50 -6 10 19 7.67 1.45 6 -10 -19 9.12 2.24 -4 10 19 -2.58 1.26 -4 -10 19 -1.96 1.31 -17 -11 19 67.46 4.87 17 11 -19 64.01 4.79 -17 11 19 57.16 4.95 -17 11 19 65.31 4.30 -15 11 19 52.94 3.87 -15 11 19 48.24 4.39 -15 -11 19 53.61 4.21 -13 -11 19 32.27 3.28 -13 11 19 38.16 3.18 -13 11 19 34.68 3.53 11 -11 -19 49.91 3.66 -11 11 19 48.74 3.59 -11 -11 19 47.90 3.75 -11 11 19 51.19 4.39 -9 -11 19 49.38 3.84 9 -11 -19 50.14 3.72 -9 11 19 49.30 3.47 -9 11 19 48.22 4.21 7 -11 -19 78.17 4.64 -7 11 19 79.71 4.53 -7 -11 19 78.46 4.80 5 -11 -19 27.60 2.92 -5 11 19 32.84 2.76 -5 -11 19 35.49 2.90 16 12 -19 3.64 1.73 -16 -12 19 1.70 1.41 -16 12 19 -2.22 2.67 -16 12 19 -0.59 1.56 14 12 -19 -1.61 0.99 -14 12 19 -0.26 1.05 -14 -12 19 -0.50 0.88 -14 12 19 -2.67 1.15 -12 12 19 0.06 1.37 -12 -12 19 -0.14 1.37 10 -12 -19 0.31 1.38 -10 12 19 -2.22 1.07 -10 12 19 -0.40 1.37 -8 12 19 3.00 1.16 -8 -12 19 1.85 1.02 8 -12 -19 2.34 1.80 -6 12 19 2.92 2.01 -6 -12 19 1.46 1.17 6 -12 -19 2.19 1.16 -15 13 19 32.79 3.07 -15 -13 19 43.57 3.82 15 13 -19 43.15 3.80 -15 13 19 35.12 3.65 -13 13 19 39.27 3.30 -13 -13 19 33.88 3.24 -13 13 19 34.59 3.70 -11 13 19 27.12 2.77 11 -13 -19 31.13 2.86 -11 -13 19 28.37 2.99 -11 13 19 22.57 2.98 -9 -13 19 16.95 2.34 -9 13 19 16.33 2.09 9 -13 -19 15.40 2.25 -9 13 19 16.34 2.59 -7 13 19 40.94 3.23 -7 -13 19 41.11 3.42 7 -13 -19 42.78 3.46 -14 14 19 4.85 1.31 -14 14 19 6.31 1.89 -12 14 19 23.92 3.02 -12 14 19 24.13 2.67 -12 -14 19 29.94 2.98 -10 -14 19 25.53 2.78 -10 14 19 22.43 2.41 10 -14 -19 26.57 2.70 -10 14 19 20.95 2.77 -8 14 19 31.89 2.82 8 -14 -19 29.37 2.93 -8 -14 19 28.21 2.80 -20 0 20 37.65 3.86 -20 0 20 42.97 4.63 -18 0 20 50.27 4.95 -18 0 20 55.52 4.31 -16 0 20 43.43 4.35 -16 0 20 41.46 3.82 -14 0 20 95.82 6.82 -14 0 20 99.90 5.75 -12 0 20 46.97 3.62 -12 0 20 45.10 4.42 -10 0 20 38.38 3.21 10 0 -20 31.93 2.59 -8 0 20 85.18 4.99 8 0 -20 87.80 4.68 -6 0 20 55.44 3.83 6 0 -20 46.36 3.32 4 0 -20 125.06 5.99 -4 0 20 121.88 6.10 -19 -1 20 3.28 1.96 -19 1 20 2.12 1.28 -19 -1 20 1.23 1.65 -17 1 20 1.79 1.75 -17 -1 20 -2.79 1.29 -15 -1 20 0.80 1.65 -15 1 20 1.89 1.80 -15 1 20 0.30 1.19 -15 -1 20 3.40 3.50 -13 1 20 7.40 2.20 -13 1 20 7.42 3.50 -13 -1 20 7.53 1.90 -11 1 20 -2.58 1.78 -11 1 20 -0.74 1.57 -9 1 20 0.26 1.75 9 1 -20 1.58 0.81 -9 -1 20 0.27 2.94 9 -1 -20 0.45 1.25 -7 1 20 3.15 1.88 -7 -1 20 1.07 1.03 7 -1 -20 1.43 1.15 -5 -1 20 -3.67 1.75 5 1 -20 1.47 0.85 5 -1 -20 0.21 1.03 -3 1 20 1.74 1.24 3 1 -20 0.50 1.06 3 -1 -20 3.42 1.39 -20 2 20 16.89 2.50 -20 -2 20 19.02 3.07 -20 2 20 20.71 3.33 -20 -2 20 20.54 2.75 -18 -2 20 33.56 4.08 -18 2 20 34.78 4.07 -18 2 20 28.61 3.33 -18 -2 20 32.06 3.53 -16 -2 20 30.36 3.28 -16 -2 20 33.78 3.96 -16 2 20 37.84 3.60 -16 2 20 34.11 3.88 -14 2 20 50.41 4.02 -14 -2 20 54.00 4.05 -14 2 20 48.39 4.55 -12 2 20 33.97 3.17 -12 -2 20 38.22 3.31 -12 2 20 45.53 4.23 -10 2 20 42.60 4.23 10 -2 -20 40.05 3.01 -10 -2 20 40.99 3.34 -10 2 20 35.01 3.14 8 -2 -20 49.22 3.36 -8 -2 20 43.96 3.57 -8 2 20 44.37 3.53 8 2 -20 45.07 3.08 6 2 -20 21.40 2.17 -6 -2 20 22.60 2.52 -6 2 20 25.09 2.60 6 -2 -20 24.51 2.46 -4 -2 20 28.57 2.86 4 -2 -20 32.58 2.79 4 2 -20 29.50 2.50 -4 2 20 33.65 2.81 -19 -3 20 19.71 2.91 -19 3 20 25.46 3.50 -19 3 20 23.94 3.09 -17 3 20 30.64 3.31 -17 -3 20 31.29 3.23 -17 3 20 28.74 3.59 -15 3 20 34.07 3.31 -15 3 20 31.69 3.84 -15 -3 20 31.81 3.33 -13 -3 20 27.62 3.02 -13 3 20 26.68 2.73 -13 3 20 26.37 3.46 -11 -3 20 17.40 2.42 -11 3 20 18.24 2.99 -11 3 20 19.11 2.48 9 -3 -20 47.90 3.38 -9 3 20 47.42 4.43 -9 -3 20 45.08 3.63 9 3 -20 40.31 2.86 -9 3 20 45.98 3.62 7 3 -20 47.85 3.23 -7 3 20 47.21 3.58 7 -3 -20 51.75 3.54 -7 -3 20 52.97 3.81 -5 3 20 17.58 2.24 5 -3 -20 20.27 2.19 -5 -3 20 19.92 2.29 5 3 -20 18.70 2.02 3 -3 -20 29.73 2.70 3 3 -20 27.63 2.51 -3 3 20 27.17 2.66 -3 -3 20 32.82 2.87 -20 4 20 10.04 2.39 -20 -4 20 8.00 1.91 -18 4 20 7.04 1.96 -18 4 20 12.02 2.46 -18 -4 20 6.53 1.94 -16 -4 20 5.16 1.83 -16 4 20 8.90 2.37 -14 -4 20 6.10 1.63 -14 4 20 6.03 1.75 -14 4 20 5.16 1.84 -12 4 20 7.08 1.92 -12 -4 20 7.80 1.63 -10 4 20 2.45 1.70 -10 4 20 2.47 1.66 8 -4 -20 0.53 1.60 -8 4 20 -1.52 2.26 -8 4 20 5.81 1.74 -8 -4 20 2.92 2.18 -6 -4 20 3.37 1.51 -6 4 20 4.10 2.05 6 4 -20 2.89 1.11 6 -4 -20 5.66 1.33 -4 4 20 2.19 1.15 4 -4 -20 3.33 1.14 -4 -4 20 1.52 1.14 -19 5 20 27.82 3.03 -19 5 20 28.98 3.58 -19 -5 20 26.45 3.10 -17 -5 20 95.68 5.89 -17 5 20 78.57 6.09 -17 5 20 73.43 5.10 -15 5 20 48.56 4.69 -15 -5 20 60.58 4.44 -15 5 20 51.67 4.01 -13 -5 20 47.92 3.91 -13 5 20 44.26 3.70 -13 5 20 47.26 4.49 -11 -5 20 54.55 4.03 -11 5 20 48.29 3.61 -11 5 20 53.29 4.80 11 -5 -20 51.78 3.49 -9 5 20 59.08 4.93 -9 5 20 51.12 3.71 9 -5 -20 53.20 3.72 -9 -5 20 55.15 4.00 7 5 -20 87.24 4.42 -7 -5 20 88.20 5.17 -7 5 20 91.51 5.00 7 -5 -20 85.33 4.74 -5 5 20 50.08 3.71 5 -5 -20 56.43 3.78 -5 -5 20 64.04 4.12 -18 6 20 -3.69 2.50 -18 -6 20 -1.77 4.68 -18 6 20 -0.43 1.77 -16 6 20 3.10 1.80 -16 6 20 3.06 3.21 -16 -6 20 0.75 1.46 -14 -6 20 -2.40 1.48 -14 6 20 -2.84 2.04 -12 6 20 5.00 1.48 -12 -6 20 -0.48 1.79 -10 6 20 -1.41 1.66 -10 -6 20 -2.64 1.73 -10 6 20 -1.96 1.66 10 -6 -20 -0.98 1.90 -8 -6 20 -2.45 1.47 -8 6 20 0.60 1.48 8 -6 -20 -2.79 1.59 -8 6 20 0.94 1.29 6 -6 -20 0.28 0.90 -6 -6 20 1.99 1.02 -6 6 20 1.43 2.32 -4 6 20 0.65 1.20 -4 -6 20 -1.27 0.94 4 -6 -20 0.34 0.88 -19 -7 20 28.78 3.25 -19 7 20 30.24 3.92 -19 7 20 29.22 3.26 -17 -7 20 57.51 4.53 -17 7 20 48.94 4.70 -17 7 20 46.09 3.83 -15 -7 20 36.15 3.55 -15 7 20 32.85 3.68 -15 7 20 30.95 3.14 -13 7 20 51.72 3.84 -13 -7 20 44.51 3.72 -13 7 20 45.66 4.41 -11 7 20 44.23 3.55 -11 7 20 42.22 4.23 -11 -7 20 43.22 3.59 11 -7 -20 41.56 3.24 -9 -7 20 44.33 3.61 9 -7 -20 44.09 3.38 -9 7 20 44.97 4.35 -9 7 20 42.78 3.46 -7 -7 20 52.94 3.89 -7 7 20 54.37 3.82 7 -7 -20 49.17 3.51 5 -7 -20 39.68 3.20 -5 -7 20 45.65 3.46 -5 7 20 41.59 3.29 -18 -8 20 14.68 2.59 -18 8 20 20.06 3.14 -18 8 20 16.88 2.36 -16 8 20 30.50 3.13 -16 8 20 30.13 3.48 -16 -8 20 25.18 3.13 -14 8 20 17.50 2.27 -14 -8 20 17.75 2.56 -14 8 20 11.67 2.59 -12 -8 20 19.41 2.60 -12 8 20 16.44 2.88 -12 8 20 15.35 2.43 10 -8 -20 5.57 3.00 -10 -8 20 7.10 1.75 -10 8 20 4.54 2.67 -10 8 20 10.96 2.51 8 -8 -20 15.12 2.03 -8 8 20 16.82 2.27 -8 -8 20 14.25 2.18 -6 -8 20 23.11 2.53 -6 8 20 18.09 2.27 6 -8 -20 24.44 2.47 -17 -9 20 16.94 2.62 -17 9 20 18.49 2.79 -17 9 20 18.92 2.60 -15 9 20 24.87 2.61 -15 -9 20 25.04 2.88 -15 9 20 20.17 3.11 -13 9 20 13.25 2.19 -13 -9 20 14.68 2.30 -13 9 20 17.69 2.69 -11 9 20 35.43 3.72 -11 -9 20 37.40 3.43 11 -9 -20 32.57 2.94 -11 9 20 30.11 3.00 -9 9 20 45.75 4.43 -9 9 20 42.67 3.35 9 -9 -20 45.57 3.52 -9 -9 20 43.22 3.60 7 -9 -20 22.26 2.39 -7 9 20 21.96 2.35 -7 -9 20 22.87 2.55 -16 10 20 30.11 2.94 -16 10 20 24.87 3.31 -16 -10 20 26.63 3.18 -14 10 20 23.11 3.00 -14 10 20 21.48 2.59 -14 -10 20 22.68 2.82 -12 10 20 40.73 4.20 -12 10 20 41.36 3.44 -12 -10 20 45.95 3.75 -10 10 20 43.37 4.23 -10 -10 20 40.45 3.62 10 -10 -20 37.40 3.20 -10 10 20 42.96 3.33 -8 -10 20 45.47 3.63 8 -10 -20 42.93 3.46 -8 10 20 38.87 3.19 -15 -11 20 -0.05 1.10 -15 11 20 5.05 1.64 -15 11 20 0.43 1.64 -13 11 20 1.63 1.51 -13 11 20 -2.35 1.56 -11 11 20 -1.16 1.51 11 -11 -20 2.06 1.39 -11 11 20 0.39 0.97 -11 -11 20 -1.37 1.12 -9 11 20 5.45 1.83 -18 0 21 -1.21 1.18 -18 0 21 -1.28 1.62 -16 0 21 1.38 2.93 -14 0 21 0.27 1.56 -14 0 21 1.49 1.95 -10 0 21 2.01 2.76 8 0 -21 0.63 1.20 -8 0 21 -1.45 1.31 -17 1 21 37.10 3.65 -17 -1 21 37.41 3.61 -17 -1 21 28.89 4.01 -17 1 21 36.47 4.14 -15 -1 21 43.49 3.69 -15 1 21 35.12 4.12 -15 1 21 29.82 3.40 -13 1 21 51.25 3.96 -13 -1 21 57.01 4.16 -13 1 21 44.40 4.65 -11 1 21 29.32 2.92 -11 -1 21 28.82 2.89 -9 -1 21 45.31 3.80 9 1 -21 42.69 3.09 9 -1 -21 39.65 3.07 -9 1 21 41.06 3.57 7 -1 -21 76.43 4.46 -7 -1 21 81.32 5.05 -7 1 21 78.30 4.87 7 1 -21 74.17 4.30 -16 -2 21 2.82 2.20 -16 2 21 1.93 2.13 -16 2 21 2.82 1.47 -14 2 21 29.09 3.13 -14 2 21 24.07 3.33 -14 -2 21 20.67 2.79 -12 2 21 18.97 2.59 -12 2 21 16.09 2.84 -12 -2 21 15.21 2.37 -10 2 21 9.03 1.89 10 -2 -21 4.54 1.30 -10 -2 21 6.99 2.87 8 2 -21 13.14 1.75 8 -2 -21 13.20 1.90 -8 2 21 12.00 1.89 -8 -2 21 15.13 2.22 -17 -3 21 32.60 3.35 -17 3 21 28.46 3.67 -17 3 21 31.20 3.26 -15 3 21 28.97 3.30 -15 -3 21 28.18 3.03 -15 3 21 29.39 3.73 -13 -3 21 21.64 2.61 -13 3 21 19.45 3.15 -13 3 21 17.73 2.49 -11 3 21 14.60 2.56 -11 3 21 16.17 2.40 -11 -3 21 14.26 2.12 -9 3 21 2.36 1.67 -9 -3 21 2.40 1.62 -7 -3 21 17.59 2.22 -7 3 21 12.60 2.09 7 3 -21 12.34 1.69 -16 4 21 36.07 4.23 -16 -4 21 35.33 3.58 -16 4 21 33.45 3.51 -14 4 21 42.64 3.62 -14 4 21 35.77 4.08 -14 -4 21 40.43 3.77 -12 4 21 41.67 4.37 -12 -4 21 45.74 3.84 -12 4 21 42.22 3.46 -10 -4 21 33.37 3.21 10 -4 -21 26.83 2.56 -10 4 21 29.63 3.68 -10 4 21 34.02 3.05 -8 -4 21 44.87 3.70 -8 4 21 40.55 3.41 8 -4 -21 39.71 3.21 -13 5 21 -0.42 1.14 -13 -5 21 -0.34 1.17 -11 5 21 -2.87 2.10 -11 -5 21 -0.12 1.24 -9 5 21 3.47 1.67 -9 -5 21 -3.23 2.02 9 -5 -21 -1.68 1.26 -9 5 21 4.02 1.58 -14 6 21 41.76 4.35 -14 6 21 43.44 3.63 -14 -6 21 40.13 3.72 -12 -6 21 37.40 3.47 -12 6 21 31.72 3.84 -12 6 21 32.73 3.11 -10 6 21 51.24 4.72 -10 6 21 53.72 3.93 10 -6 -21 45.39 3.45 -10 -6 21 57.32 4.13 -13 7 21 0.59 1.45 -13 7 21 -0.04 1.40 -13 -7 21 1.09 1.17 11 -7 -21 2.94 1.11 -11 -7 21 0.57 2.16 -11 7 21 1.92 1.59 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 73193 _shelx_shelxl_version_number 2014/7 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.5000 0.70590(2) 0.7500 0.02459(4) Uani 1 2 d S T P . . P1 P 1.0000 0.57556(6) 0.7500 0.0585(3) Uani 1 2 d S TU P . . Cl1A Cl 0.84401(16) 0.42523(9) 0.82981(17) 0.0778(8) Uani 0.724(8) 1 d . U . A 1 Cl2A Cl 0.8507(2) 0.27719(13) 1.0126(2) 0.0897(8) Uani 0.724(8) 1 d . U . A 1 N3 N 0.53253(12) 0.78110(9) 0.84700(14) 0.0270(4) Uani 1 1 d D . . . . N1 N 0.59583(12) 0.69896(9) 0.73013(15) 0.0274(4) Uani 1 1 d . . . . . Cl3 Cl 0.38332(15) 0.53672(11) 0.22006(13) 0.1641(11) Uani 1 1 d D U . . . O2 O 0.88411(13) 0.78958(10) 0.83684(19) 0.0477(5) Uani 1 1 d . . . . . N2 N 0.66336(12) 0.65122(9) 0.66734(15) 0.0295(4) Uani 1 1 d . . . . . O1 O 0.30491(12) 0.55000(11) 0.46704(17) 0.0494(5) Uani 1 1 d . . . . . C19 C 0.51708(13) 0.83741(10) 0.80419(12) 0.0264(4) Uani 1 1 d D . . . . C1 C 0.46660(14) 0.64110(10) 0.64561(16) 0.0267(4) Uani 1 1 d . . . . . C7 C 0.59442(14) 0.65563(11) 0.66877(17) 0.0280(4) Uani 1 1 d . . . . . C8 C 0.66782(14) 0.72535(11) 0.76819(18) 0.0277(4) Uani 1 1 d . . . . . C6 C 0.52178(14) 0.62431(11) 0.61473(18) 0.0291(5) Uani 1 1 d . . . . . C13 C 0.71049(15) 0.69668(11) 0.72771(18) 0.0286(5) Uani 1 1 d . . . . . C20 C 0.53288(16) 0.89017(11) 0.86065(18) 0.0335(5) Uani 1 1 d D . . . . H20 H 0.5223 0.9287 0.8298 0.040 Uiso 1 1 calc R . . . . C23 C 0.56231(16) 0.77869(12) 0.94372(18) 0.0340(5) Uani 1 1 d . . . . . H23 H 0.5729 0.7401 0.9744 0.041 Uiso 1 1 calc R . . . . C21 C 0.56327(16) 0.88644(12) 0.9594(2) 0.0355(5) Uani 1 1 d . . . . . C12 C 0.78389(16) 0.71609(12) 0.7467(2) 0.0335(5) Uani 1 1 d . . . . . H12 H 0.8123 0.6969 0.7181 0.040 Uiso 1 1 calc R . . . . C9 C 0.69929(16) 0.77366(13) 0.8329(2) 0.0354(5) Uani 1 1 d . . . . . H9 H 0.6714 0.7927 0.8623 0.042 Uiso 1 1 calc R . . . . C5 C 0.50108(16) 0.58685(12) 0.5330(2) 0.0365(6) Uani 1 1 d . . . . . H5 H 0.5376 0.5778 0.5102 0.044 Uiso 1 1 calc R . . . . C11 C 0.81304(15) 0.76493(12) 0.8095(2) 0.0346(5) Uani 1 1 d . . . . . C2 C 0.39332(15) 0.61551(12) 0.59780(19) 0.0320(5) Uani 1 1 d . . . . . H2 H 0.3559 0.6247 0.6191 0.038 Uiso 1 1 calc R . . . . C22 C 0.57850(17) 0.82971(13) 1.00154(19) 0.0382(6) Uani 1 1 d . . . . . H22 H 0.6001 0.8257 1.0704 0.046 Uiso 1 1 calc R . . . . C3 C 0.37515(16) 0.57662(12) 0.5190(2) 0.0352(5) Uani 1 1 d . . . . . C10 C 0.77169(17) 0.79285(12) 0.8527(2) 0.0383(6) Uani 1 1 d . . . . . H10 H 0.7942 0.8257 0.8966 0.046 Uiso 1 1 calc R . . . . C4 C 0.42821(17) 0.56310(13) 0.4859(2) 0.0390(6) Uani 1 1 d . . . . . H4 H 0.4144 0.5375 0.4308 0.047 Uiso 1 1 calc R . . . . F1 F 0.9513(2) 0.52554(14) 0.7684(4) 0.1295(15) Uani 1 1 d . U . . . C14 C 0.68846(16) 0.59911(12) 0.6275(2) 0.0376(6) Uani 1 1 d . . . . . H14 H 0.6465 0.5682 0.6059 0.045 Uiso 1 1 calc R . . . . C24 C 0.5782(2) 0.94284(15) 1.0197(2) 0.0501(8) Uani 1 1 d . . . . . H24A H 0.5722 0.9784 0.9788 0.075 Uiso 1 1 calc GR . . . . H24B H 0.6306 0.9417 1.0732 0.075 Uiso 1 1 calc GR . . . . H24C H 0.5414 0.9452 1.0466 0.075 Uiso 1 1 calc GR . . . . C18 C 0.9255(2) 0.7706(2) 0.7869(4) 0.0675(11) Uani 1 1 d . . . . . H18A H 0.8945 0.7774 0.7168 0.101 Uiso 1 1 calc GR . . . . H18B H 0.9374 0.7273 0.7989 0.101 Uiso 1 1 calc GR . . . . H18C H 0.9734 0.7937 0.8104 0.101 Uiso 1 1 calc GR . . . . C17 C 0.2460(2) 0.56241(19) 0.4938(3) 0.0603(10) Uani 1 1 d . . . . . H17A H 0.1989 0.5414 0.4490 0.091 Uiso 1 1 calc GR . . . . H17B H 0.2366 0.6062 0.4904 0.091 Uiso 1 1 calc GR . . . . H17C H 0.2618 0.5482 0.5606 0.091 Uiso 1 1 calc GR . . . . C15 C 0.6968(3) 0.61692(18) 0.5386(3) 0.0665(11) Uani 1 1 d . . . . . H15A H 0.6490 0.6356 0.4907 0.100 Uiso 1 1 calc GR . . . . H15B H 0.7079 0.5808 0.5101 0.100 Uiso 1 1 calc GR . . . . H15C H 0.7390 0.6460 0.5571 0.100 Uiso 1 1 calc GR . . . . C16 C 0.7595(2) 0.56964(16) 0.7066(3) 0.0627(11) Uani 1 1 d . . . . . H16A H 0.8039 0.5963 0.7234 0.094 Uiso 1 1 calc GR . . . . H16B H 0.7686 0.5307 0.6829 0.094 Uiso 1 1 calc GR . . . . H16C H 0.7519 0.5629 0.7645 0.094 Uiso 1 1 calc GR . . . . F2A F 0.9646(14) 0.6217(7) 0.798(2) 0.140(6) Uani 0.51(3) 1 d . U . B 2 C25A C 0.8148(5) 0.3708(4) 0.8952(6) 0.085(2) Uani 0.724(8) 1 d . U . A 1 H25A H 0.7999 0.3921 0.9407 0.102 Uiso 0.724(8) 1 calc R . . A 1 H25B H 0.7702 0.3469 0.8488 0.102 Uiso 0.724(8) 1 calc R . . A 1 C26A C 0.8788(5) 0.3318(4) 0.9481(6) 0.0799(19) Uani 0.724(8) 1 d . U . A 1 H26A H 0.9232 0.3557 0.9948 0.096 Uiso 0.724(8) 1 calc R . . A 1 H26B H 0.8939 0.3109 0.9026 0.096 Uiso 0.724(8) 1 calc R . . A 1 F3A F 1.0589(8) 0.5534(10) 0.8545(12) 0.164(6) Uani 0.51(3) 1 d . U . B 2 Cl2B Cl 0.8921(11) 0.2675(5) 1.0082(7) 0.150(5) Uani 0.276(8) 1 d D U . A 2 Cl1B Cl 0.7991(12) 0.4231(5) 0.8396(10) 0.199(8) Uani 0.276(8) 1 d D U . A 2 C25B C 0.8529(16) 0.3577(9) 0.8819(15) 0.102(6) Uani 0.276(8) 1 d D U . A 2 H25C H 0.8262 0.3235 0.8377 0.122 Uiso 0.276(8) 1 calc R . . A 2 H25D H 0.9034 0.3631 0.8826 0.122 Uiso 0.276(8) 1 calc R . . A 2 C26B C 0.8640(16) 0.3440(9) 0.9804(13) 0.115(6) Uani 0.276(8) 1 d D U . A 2 H26C H 0.8156 0.3512 0.9846 0.138 Uiso 0.276(8) 1 calc R . . A 2 H26D H 0.9041 0.3709 1.0281 0.138 Uiso 0.276(8) 1 calc R . . A 2 C27A C 0.4634(3) 0.5379(9) 0.2008(5) 0.253(10) Uani 0.513(19) 1 d D U . C 1 H27A H 0.4634 0.5019 0.1623 0.304 Uiso 0.513(19) 1 calc R . . C 1 H27B H 0.4625 0.5746 0.1633 0.304 Uiso 0.513(19) 1 calc R . . C 1 F3B F 1.0524(12) 0.5910(12) 0.8498(13) 0.202(7) Uani 0.49(3) 1 d . U . B 1 F2B F 0.9388(9) 0.6248(5) 0.732(2) 0.120(5) Uani 0.49(3) 1 d . U . B 1 C27B C 0.4812(4) 0.5370(13) 0.2844(5) 0.287(13) Uani 0.487(19) 1 d D U . C 2 H27C H 0.4980 0.5734 0.3266 0.345 Uiso 0.487(19) 1 calc R . . C 2 H27D H 0.4983 0.5008 0.3270 0.345 Uiso 0.487(19) 1 calc R . . C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.03001(7) 0.02099(6) 0.02330(6) 0.000 0.01258(5) 0.000 P1 0.0845(10) 0.0317(5) 0.0795(9) 0.000 0.0548(8) 0.000 Cl1A 0.0980(15) 0.0504(9) 0.0854(12) 0.0013(7) 0.0419(11) -0.0062(9) Cl2A 0.128(2) 0.0688(12) 0.0785(13) 0.0002(9) 0.0521(13) -0.0128(12) N3 0.0307(10) 0.0262(9) 0.0247(9) -0.0008(7) 0.0132(8) 0.0020(7) N1 0.0322(10) 0.0234(9) 0.0262(9) -0.0021(7) 0.0129(8) -0.0018(7) Cl3 0.242(3) 0.1568(19) 0.0694(9) -0.0020(11) 0.0498(13) 0.0641(19) O2 0.0390(11) 0.0489(13) 0.0607(14) -0.0155(10) 0.0276(10) -0.0140(9) N2 0.0329(10) 0.0263(10) 0.0309(10) -0.0069(8) 0.0159(8) -0.0017(8) O1 0.0391(11) 0.0475(12) 0.0539(13) -0.0191(10) 0.0145(10) -0.0118(9) C19 0.0277(10) 0.0253(10) 0.0278(11) -0.0005(8) 0.0141(9) 0.0005(8) C1 0.0338(11) 0.0207(10) 0.0251(10) 0.0001(8) 0.0129(9) -0.0004(8) C7 0.0335(12) 0.0246(10) 0.0261(10) -0.0021(8) 0.0137(9) 0.0002(9) C8 0.0321(11) 0.0245(10) 0.0282(11) -0.0013(8) 0.0151(9) -0.0007(9) C6 0.0348(12) 0.0236(10) 0.0282(11) -0.0026(8) 0.0138(9) -0.0019(9) C13 0.0335(12) 0.0249(10) 0.0276(11) -0.0010(8) 0.0141(9) 0.0009(9) C20 0.0407(13) 0.0243(11) 0.0368(13) -0.0013(9) 0.0188(11) 0.0027(10) C23 0.0425(14) 0.0311(12) 0.0263(11) 0.0011(9) 0.0139(10) 0.0050(10) C21 0.0387(13) 0.0329(13) 0.0349(13) -0.0084(10) 0.0165(11) 0.0028(10) C12 0.0349(12) 0.0338(12) 0.0356(13) -0.0038(10) 0.0193(11) -0.0005(10) C9 0.0358(13) 0.0339(12) 0.0377(13) -0.0103(11) 0.0179(11) -0.0022(10) C5 0.0404(14) 0.0335(13) 0.0360(13) -0.0095(10) 0.0179(11) -0.0015(11) C11 0.0323(12) 0.0335(13) 0.0377(13) -0.0033(10) 0.0157(11) -0.0047(10) C2 0.0346(12) 0.0280(11) 0.0329(12) -0.0023(9) 0.0149(10) -0.0022(10) C22 0.0476(15) 0.0375(14) 0.0262(11) -0.0030(10) 0.0138(11) 0.0048(12) C3 0.0357(13) 0.0282(12) 0.0354(13) -0.0035(10) 0.0107(11) -0.0041(10) C10 0.0367(13) 0.0341(13) 0.0420(14) -0.0142(11) 0.0161(11) -0.0063(11) C4 0.0421(14) 0.0349(13) 0.0339(13) -0.0105(11) 0.0120(11) -0.0032(11) F1 0.144(3) 0.0632(17) 0.249(5) 0.028(2) 0.148(3) 0.0125(18) C14 0.0405(14) 0.0311(12) 0.0444(15) -0.0122(11) 0.0221(12) -0.0008(10) C24 0.065(2) 0.0392(15) 0.0423(16) -0.0154(13) 0.0215(15) 0.0023(14) C18 0.057(2) 0.075(3) 0.091(3) -0.028(2) 0.052(2) -0.026(2) C17 0.0411(17) 0.066(2) 0.070(2) -0.0223(19) 0.0222(17) -0.0153(16) C15 0.106(3) 0.054(2) 0.069(2) -0.0186(18) 0.065(3) -0.010(2) C16 0.0507(19) 0.0433(18) 0.077(3) -0.0153(17) 0.0144(18) 0.0126(15) F2A 0.185(12) 0.071(6) 0.234(16) -0.055(9) 0.157(12) -0.002(6) C25A 0.077(4) 0.094(5) 0.095(5) 0.011(4) 0.047(4) 0.002(4) C26A 0.091(5) 0.076(4) 0.083(5) -0.004(3) 0.049(4) 0.001(3) F3A 0.198(8) 0.134(11) 0.117(8) 0.058(8) 0.034(6) 0.027(7) Cl2B 0.256(16) 0.106(5) 0.081(4) -0.017(4) 0.070(7) -0.060(7) Cl1B 0.220(15) 0.109(6) 0.184(9) -0.027(6) 0.020(10) 0.059(8) C25B 0.117(14) 0.102(12) 0.104(11) 0.010(9) 0.067(12) 0.011(10) C26B 0.131(14) 0.152(12) 0.088(10) -0.036(8) 0.073(11) 0.024(12) C27A 0.380(19) 0.32(2) 0.162(14) -0.173(15) 0.208(17) -0.262(19) F3B 0.254(12) 0.155(15) 0.100(9) -0.055(10) -0.006(8) -0.014(10) F2B 0.132(8) 0.044(4) 0.223(15) 0.004(7) 0.113(10) 0.028(4) C27B 0.250(11) 0.42(3) 0.140(19) -0.03(2) 0.040(17) -0.257(17) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 N3 Ir1 N3 77.47(11) 2_656 . ? N1 Ir1 N3 99.35(8) 2_656 2_656 ? N1 Ir1 N3 99.35(8) . . ? N1 Ir1 N3 87.41(8) 2_656 . ? N1 Ir1 N3 87.41(8) . 2_656 ? N1 Ir1 N1 171.38(11) . 2_656 ? C1 Ir1 N3 96.19(9) . 2_656 ? C1 Ir1 N3 173.61(8) . . ? C1 Ir1 N3 96.20(9) 2_656 . ? C1 Ir1 N3 173.61(8) 2_656 2_656 ? C1 Ir1 N1 79.30(9) . . ? C1 Ir1 N1 94.56(9) 2_656 . ? C1 Ir1 N1 79.30(9) 2_656 2_656 ? C1 Ir1 N1 94.56(9) . 2_656 ? C1 Ir1 C1 90.15(13) . 2_656 ? F1 P1 F1 90.3(2) 2_756 . ? F1 P1 F2A 86.5(6) 2_756 2_756 ? F1 P1 F2A 86.5(6) . . ? F1 P1 F2A 164.9(12) . 2_756 ? F1 P1 F2A 164.9(12) 2_756 . ? F1 P1 F3A 75.1(9) . 2_756 ? F1 P1 F3A 79.5(7) 2_756 2_756 ? F1 P1 F3A 79.5(7) . . ? F1 P1 F3A 75.1(9) 2_756 . ? F2A P1 F2A 100.2(14) 2_756 . ? F3A P1 F2A 113.7(14) . 2_756 ? F3A P1 F2A 113.7(14) 2_756 . ? F3A P1 F2A 89.8(8) . . ? F3A P1 F2A 89.8(8) 2_756 2_756 ? F3A P1 F3A 143.8(18) 2_756 . ? F3B P1 F1 99.7(12) 2_756 2_756 ? F3B P1 F1 99.4(10) . 2_756 ? F3B P1 F1 99.4(10) 2_756 . ? F3B P1 F1 99.7(12) . . ? F3B P1 F3B 153(2) . 2_756 ? F3B P1 F2B 61.9(19) 2_756 . ? F3B P1 F2B 98.0(8) . . ? F3B P1 F2B 61.9(19) . 2_756 ? F3B P1 F2B 98.0(8) 2_756 2_756 ? F2B P1 F1 161.7(10) 2_756 . ? F2B P1 F1 92.4(5) . . ? F2B P1 F1 161.7(10) . 2_756 ? F2B P1 F1 92.4(5) 2_756 2_756 ? F2B P1 F2B 90.7(11) 2_756 . ? C19 N3 Ir1 115.98(14) . . ? C23 N3 Ir1 126.41(17) . . ? C23 N3 C19 117.5(2) . . ? C7 N1 Ir1 115.83(17) . . ? C7 N1 C8 106.9(2) . . ? C8 N1 Ir1 137.15(16) . . ? C11 O2 C18 118.0(3) . . ? C7 N2 C13 107.3(2) . . ? C7 N2 C14 125.2(2) . . ? C13 N2 C14 126.1(2) . . ? C3 O1 C17 118.7(2) . . ? N3 C19 C19 115.24(11) . 2_656 ? N3 C19 C20 121.02(18) . . ? C20 C19 C19 123.74(13) . 2_656 ? C6 C1 Ir1 115.62(17) . . ? C2 C1 Ir1 125.89(19) . . ? C2 C1 C6 118.3(2) . . ? N1 C7 N2 111.1(2) . . ? N1 C7 C6 116.4(2) . . ? N2 C7 C6 132.4(2) . . ? N1 C8 C13 108.6(2) . . ? N1 C8 C9 131.1(2) . . ? C9 C8 C13 120.3(2) . . ? C1 C6 C7 112.4(2) . . ? C5 C6 C1 120.2(2) . . ? C5 C6 C7 127.0(2) . . ? N2 C13 C8 106.0(2) . . ? N2 C13 C12 131.8(2) . . ? C12 C13 C8 122.2(2) . . ? C19 C20 H20 119.9 . . ? C21 C20 C19 120.3(2) . . ? C21 C20 H20 119.9 . . ? N3 C23 H23 118.5 . . ? N3 C23 C22 123.0(2) . . ? C22 C23 H23 118.5 . . ? C20 C21 C22 118.2(2) . . ? C20 C21 C24 120.3(3) . . ? C22 C21 C24 121.5(3) . . ? C13 C12 H12 121.9 . . ? C11 C12 C13 116.2(2) . . ? C11 C12 H12 121.9 . . ? C8 C9 H9 121.0 . . ? C10 C9 C8 118.0(2) . . ? C10 C9 H9 121.0 . . ? C6 C5 H5 119.8 . . ? C4 C5 C6 120.3(3) . . ? C4 C5 H5 119.8 . . ? O2 C11 C12 124.2(3) . . ? O2 C11 C10 113.8(2) . . ? C12 C11 C10 122.0(2) . . ? C1 C2 H2 120.0 . . ? C3 C2 C1 120.1(2) . . ? C3 C2 H2 120.0 . . ? C23 C22 H22 120.0 . . ? C21 C22 C23 120.0(2) . . ? C21 C22 H22 120.0 . . ? O1 C3 C2 124.3(3) . . ? O1 C3 C4 114.5(2) . . ? C4 C3 C2 121.2(2) . . ? C9 C10 C11 121.2(2) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C5 C4 C3 119.7(2) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? N2 C14 H14 106.8 . . ? N2 C14 C15 111.5(3) . . ? N2 C14 C16 110.7(2) . . ? C15 C14 H14 106.8 . . ? C15 C14 C16 113.8(3) . . ? C16 C14 H14 106.8 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O2 C18 H18A 109.5 . . ? O2 C18 H18B 109.5 . . ? O2 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O1 C17 H17A 109.5 . . ? O1 C17 H17B 109.5 . . ? O1 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Cl1A C25A H25A 110.2 . . ? Cl1A C25A H25B 110.2 . . ? H25A C25A H25B 108.5 . . ? C26A C25A Cl1A 107.4(6) . . ? C26A C25A H25A 110.2 . . ? C26A C25A H25B 110.2 . . ? Cl2A C26A H26A 110.1 . . ? Cl2A C26A H26B 110.1 . . ? C25A C26A Cl2A 108.0(6) . . ? C25A C26A H26A 110.1 . . ? C25A C26A H26B 110.1 . . ? H26A C26A H26B 108.4 . . ? Cl1B C25B H25C 109.7 . . ? Cl1B C25B H25D 109.7 . . ? H25C C25B H25D 108.2 . . ? C26B C25B Cl1B 109.9(14) . . ? C26B C25B H25C 109.7 . . ? C26B C25B H25D 109.7 . . ? Cl2B C26B H26C 109.8 . . ? Cl2B C26B H26D 109.8 . . ? C25B C26B Cl2B 109.4(12) . . ? C25B C26B H26C 109.8 . . ? C25B C26B H26D 109.8 . . ? H26C C26B H26D 108.2 . . ? Cl3 C27A H27A 109.7 . . ? Cl3 C27A H27B 109.7 . . ? C27A C27A Cl3 110.0(8) 2_655 . ? C27A C27A H27A 109.7 2_655 . ? C27A C27A H27B 109.7 2_655 . ? H27A C27A H27B 108.2 . . ? P1 F3B F2B 62.2(13) . 2_756 ? F3B F2B P1 55.9(8) 2_756 . ? Cl3 C27B H27C 109.4 . . ? Cl3 C27B H27D 109.4 . . ? C27B C27B Cl3 111.1(7) 2_655 . ? C27B C27B H27C 109.4 2_655 . ? C27B C27B H27D 109.4 2_655 . ? H27C C27B H27D 108.0 . . ? 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 N3 2.126(2) . ? Ir1 N3 2.126(2) 2_656 ? Ir1 N1 2.037(2) 2_656 ? Ir1 N1 2.037(2) . ? Ir1 C1 2.024(2) 2_656 ? Ir1 C1 2.024(2) . ? P1 F1 1.565(3) 2_756 ? P1 F1 1.565(3) . ? P1 F2A 1.586(10) . ? P1 F2A 1.586(10) 2_756 ? P1 F3A 1.570(11) 2_756 ? P1 F3A 1.570(11) . ? P1 F3B 1.447(13) 2_756 ? P1 F3B 1.447(13) . ? P1 F2B 1.546(9) 2_756 ? P1 F2B 1.546(9) . ? Cl1A C25A 1.819(8) . ? Cl2A C26A 1.798(8) . ? N3 C19 1.374(3) . ? N3 C23 1.330(3) . ? N1 C7 1.335(3) . ? N1 C8 1.383(3) . ? Cl3 C27A 1.722(8) . ? Cl3 C27B 1.709(7) . ? O2 C11 1.368(3) . ? O2 C18 1.409(4) . ? N2 C7 1.362(3) . ? N2 C13 1.392(3) . ? N2 C14 1.487(3) . ? O1 C3 1.368(3) . ? O1 C17 1.415(4) . ? C19 C19 1.488(3) 2_656 ? C19 C20 1.400(3) . ? C1 C6 1.412(3) . ? C1 C2 1.398(3) . ? C7 C6 1.453(3) . ? C8 C13 1.399(3) . ? C8 C9 1.396(3) . ? C6 C5 1.402(3) . ? C13 C12 1.395(4) . ? C20 H20 0.9500 . ? C20 C21 1.360(4) . ? C23 H23 0.9500 . ? C23 C22 1.379(4) . ? C21 C22 1.378(4) . ? C21 C24 1.499(4) . ? C12 H12 0.9500 . ? C12 C11 1.385(4) . ? C9 H9 0.9500 . ? C9 C10 1.372(4) . ? C5 H5 0.9500 . ? C5 C4 1.375(4) . ? C11 C10 1.402(4) . ? C2 H2 0.9500 . ? C2 C3 1.393(4) . ? C22 H22 0.9500 . ? C3 C4 1.381(4) . ? C10 H10 0.9500 . ? C4 H4 0.9500 . ? C14 H14 1.0000 . ? C14 C15 1.502(5) . ? C14 C16 1.514(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C25A H25A 0.9900 . ? C25A H25B 0.9900 . ? C25A C26A 1.429(11) . ? C26A H26A 0.9900 . ? C26A H26B 0.9900 . ? Cl2B C26B 1.765(16) . ? Cl1B C25B 1.728(16) . ? C25B H25C 0.9900 . ? C25B H25D 0.9900 . ? C25B C26B 1.463(17) . ? C26B H26C 0.9900 . ? C26B H26D 0.9900 . ? C27A C27A 1.538(9) 2_655 ? C27A H27A 0.9900 . ? C27A H27B 0.9900 . ? F3B F2B 1.54(5) 2_756 ? F2B F3B 1.54(5) 2_756 ? C27B C27B 1.540(10) 2_655 ? C27B H27C 0.9900 . ? C27B H27D 0.9900 . ? 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 C20 H20 F1 0.95 2.49 3.378(4) 156.3 3_455 C9 H9 N3 0.95 2.63 3.369(4) 135.0 . C18 H18B F2A 0.98 2.39 3.358(17) 169.1 . C18 H18B F2B 0.98 2.49 3.362(15) 148.6 .