#------------------------------------------------------------------------------ #$Date: 2018-01-23 05:16:25 +0200 (Tue, 23 Jan 2018) $ #$Revision: 205481 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/53/7045339.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_7045339 loop_ _publ_author_name 'Congrave, Daniel G.' 'Hsu, Yu-Ting' 'Batsanov, Andrei S.' 'Beeby, Andrew' 'Bryce, Martin R.' _publ_section_title ; Sky-blue emitting bridged diiridium complexes: beneficial effects of intramolecular \p--\p stacking ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/C7DT04201A _journal_year 2018 _chemical_formula_moiety 'C94 H72 F10 Ir2 N6 O2, 2(C H2 Cl2)' _chemical_formula_sum 'C96 H76 Cl4 F10 Ir2 N6 O2' _chemical_formula_weight 2061.82 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary heavy _audit_creation_date 2017-01-09 _audit_creation_method ; Olex2 1.2-beta (compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289) ; _audit_update_record ; 2017-09-22 deposited with the CCDC. 2017-12-14 downloaded from the CCDC. ; _cell_angle_alpha 101.8809(19) _cell_angle_beta 93.1589(19) _cell_angle_gamma 109.7449(19) _cell_formula_units_Z 2 _cell_length_a 12.8310(8) _cell_length_b 13.3678(8) _cell_length_c 27.8367(16) _cell_measurement_reflns_used 9915 _cell_measurement_temperature 120 _cell_measurement_theta_max 31.83 _cell_measurement_theta_min 2.33 _cell_volume 4357.2(5) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_collection 'APEX3 v.2016.1-0 (Bruker, 2016)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL 2014/7 multi-CPU (Sheldrick, 2015)' _computing_structure_solution 'ShelXS 2013/1 (Sheldrick, 2008)' _diffrn_ambient_temperature 120 _diffrn_detector_area_resol_mean 10.4 _diffrn_detector_type 'Bruker PHOTON 100 CMOS' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device '3-circle area detector diffractometer' _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'focusing mirrors' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_unetI/netI 0.0529 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_number 84964 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 29.999 _diffrn_reflns_theta_max 29.999 _diffrn_reflns_theta_min 2.114 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\mS microsource' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.248 _exptl_absorpt_correction_T_max 0.8595 _exptl_absorpt_correction_T_min 0.5267 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1284 before and 0.0562 after correction. The Ratio of minimum to maximum transmission is 0.6128. The \l/2 correction factor is Not present. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.572 _exptl_crystal_description needle _exptl_crystal_F_000 2044 _exptl_crystal_preparation Luminescent _exptl_crystal_size_max 0.295 _exptl_crystal_size_mid 0.117 _exptl_crystal_size_min 0.059 _refine_diff_density_max 3.223 _refine_diff_density_min -7.359 _refine_diff_density_rms 0.182 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.283 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1129 _refine_ls_number_reflns 25354 _refine_ls_number_restraints 1090 _refine_ls_restrained_S_all 1.261 _refine_ls_R_factor_all 0.0861 _refine_ls_R_factor_gt 0.0624 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+44.0740P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1269 _refine_ls_wR_factor_ref 0.1350 _reflns_Friedel_coverage 0.000 _reflns_number_gt 19773 _reflns_number_total 25354 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt04201a2.cif _cod_data_source_block 11_16srv477 _cod_depositor_comments ; The following automatic conversions were performed: '_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according to /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas ; _cod_database_code 7045339 _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 0.831 _shelx_estimated_absorpt_t_min 0.447 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2. Restrained distances Cl3-C96 \\sim Cl4-C96 \\sim Cl5-C96 \\sim Cl6-C97 \\sim Cl7-C97 with sigma of 0.02 3. Rigid body (RIGU) restrains All non-hydrogen atoms with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4. Others Uiso(H65A)=Uiso(H65B)=Uiso(H65C)=FVAR(1) Uiso(H66A)=Uiso(H66B)=Uiso(H66C)=FVAR(2) Uiso(H67A)=Uiso(H67B)=Uiso(H67C)=FVAR(3) Uiso(H74A)=Uiso(H74B)=Uiso(H74C)=FVAR(4) Uiso(H75A)=Uiso(H75B)=Uiso(H75C)=FVAR(5) Uiso(H76A)=Uiso(H76B)=Uiso(H76C)=FVAR(6) Uiso(H83A)=Uiso(H83B)=Uiso(H83C)=FVAR(7) Uiso(H84A)=Uiso(H84B)=Uiso(H84C)=FVAR(8) Uiso(H85A)=Uiso(H85B)=Uiso(H85C)=FVAR(9) Uiso(H92A)=Uiso(H92B)=Uiso(H92C)=FVAR(10) Uiso(H93A)=Uiso(H93B)=Uiso(H93C)=FVAR(11) Uiso(H94A)=Uiso(H94B)=Uiso(H94C)=FVAR(12) Fixed Sof: Cl6(0.5) Cl7(0.5) Cl3(0.4) Cl4(0.27) Cl5(0.13) Cl8(0.1) Cl9(0.1) C97(0.5) H97A(0.5) H97B(0.5) C96(0.4) H96A(0.4) H96B(0.4) 5.a Riding coordinates: C97(H97A,H97B), C96(H96A,H96B) 5.b Secondary CH2 refined with riding coordinates: C95(H95A,H95B) 5.c Aromatic/amide H refined with riding coordinates: C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C12(H12), C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C32(H32), C34(H34), C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C43(H43), C45(H45), C46(H46), C61(H61), C63(H63), C70(H70), C72(H72), C79(H79), C81(H81), C88(H88), C90(H90) 5.d Idealised Me refined as rotating group: C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C74(H74A,H74B, H74C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C83(H83A,H83B,H83C), C84(H84A, H84B,H84C), C85(H85A,H85B,H85C), C92(H92A,H92B,H92C), C93(H93A,H93B,H93C), C94(H94A,H94B,H94C) ; _shelx_res_file ; 16srv477.res created by SHELXL-2014/7 TITL 16srv477 in P-1 #2 REM reset to P-1 #2 CELL 0.71073 12.831 13.3678 27.8367 101.8809 93.1589 109.7449 ZERR 2 0.0008 0.0008 0.0016 0.0019 0.0019 0.0019 LATT 1 SFAC C H Cl F Ir N O UNIT 192 152 8 20 4 12 4 SADI Cl3 C96 Cl4 C96 Cl5 C96 Cl6 C97 Cl7 C97 RIGU L.S. 7 PLAN 40 SIZE 0.059 0.117 0.295 TEMP -153.15 FREE Cl5 H96A FREE Cl5 Cl4 BIND C96 Cl5 BOND fmap 2 acta 60 OMIT -3 60 OMIT 0 -1 2 OMIT -1 1 2 OMIT -1 1 0 REM REM REM WGHT 0.000000 44.074001 FVAR 0.05871 0.08462 0.11146 0.04853 0.05902 0.11584 0.05383 FVAR 0.12237 0.09584 0.16817 0.06486 0.07607 0.07207 IR1 5 0.064667 0.914506 0.296237 11.00000 0.01401 0.01461 = 0.01952 0.00617 0.00262 0.00482 IR2 5 0.076768 0.539993 0.219272 11.00000 0.01831 0.01712 = 0.02215 0.00492 -0.00016 0.00588 F1 4 0.095385 0.857346 0.144384 11.00000 0.02881 0.05138 = 0.04720 0.02835 0.00505 0.01380 F2 4 0.223421 1.043889 0.121751 11.00000 0.05447 0.06036 = 0.07405 0.04849 0.02125 0.02350 F3 4 0.435697 1.152532 0.168349 11.00000 0.06100 0.03647 = 0.06885 0.02491 0.03241 0.00134 F4 4 0.517399 1.076107 0.239670 11.00000 0.04382 0.06938 = 0.04302 0.01424 0.00639 -0.00863 F5 4 0.386618 0.892304 0.263735 11.00000 0.02709 0.05792 = 0.03507 0.01760 -0.00706 -0.00699 F6 4 -0.259539 0.588295 0.244359 11.00000 0.02478 0.03254 = 0.03688 0.01263 -0.00349 0.00930 F7 4 -0.414838 0.419977 0.269265 11.00000 0.01523 0.03132 = 0.07263 0.01396 -0.00424 -0.00323 F8 4 -0.357967 0.331982 0.341233 11.00000 0.03509 0.04166 = 0.09739 0.04383 0.01817 0.00136 F9 4 -0.144195 0.407284 0.386032 11.00000 0.04679 0.05350 = 0.06430 0.04616 0.01109 0.01487 F10 4 0.012640 0.573315 0.360076 11.00000 0.02341 0.03687 = 0.03728 0.01807 -0.00183 0.01030 O1 7 -0.057602 0.769918 0.306843 11.00000 0.02006 0.01594 = 0.03058 0.00974 0.01008 0.00634 O2 7 0.171209 0.680152 0.192785 11.00000 0.02440 0.02169 = 0.02534 0.00415 0.00680 0.00708 N1 6 0.105497 0.779709 0.253561 11.00000 0.01626 0.01472 = 0.02225 0.00727 0.00372 0.00579 N2 6 0.040139 0.674796 0.262264 11.00000 0.01604 0.01737 = 0.02090 0.00812 0.00146 0.00513 N3 6 -0.022444 0.924916 0.235327 11.00000 0.01637 0.01855 = 0.02232 0.00532 0.00108 0.00350 N4 6 0.153917 0.920554 0.360154 11.00000 0.01785 0.01645 = 0.02159 0.00677 0.00572 0.00742 N5 6 -0.068916 0.501910 0.174807 11.00000 0.02277 0.02163 = 0.02467 0.00806 -0.00203 0.00431 N6 6 0.221560 0.568292 0.263012 11.00000 0.01822 0.01503 = 0.02415 0.00484 0.00160 0.00385 C1 1 0.166515 0.769445 0.218339 11.00000 0.01986 0.02125 = 0.01871 0.00301 0.00058 0.00616 C2 1 -0.038463 0.682623 0.289185 11.00000 0.01328 0.01768 = 0.02107 0.00987 0.00059 0.00251 C3 1 0.170186 1.053513 0.284772 11.00000 0.01626 0.01721 = 0.02176 0.00539 0.00636 0.00980 C4 1 0.276499 1.118199 0.310566 11.00000 0.01624 0.02149 = 0.02455 0.00599 0.00100 0.00538 AFIX 43 H4 2 0.306996 1.094857 0.336187 11.00000 -1.20000 AFIX 0 C5 1 0.338119 1.216182 0.299208 11.00000 0.01964 0.01812 = 0.03007 0.00401 0.00076 0.00281 AFIX 43 H5 2 0.410643 1.258059 0.316714 11.00000 -1.20000 AFIX 0 C6 1 0.294930 1.253304 0.262696 11.00000 0.02202 0.01861 = 0.03300 0.00925 0.00361 0.00126 AFIX 43 H6 2 0.337867 1.320292 0.255316 11.00000 -1.20000 AFIX 0 C7 1 0.189872 1.193343 0.237051 11.00000 0.02096 0.01963 = 0.02681 0.00998 0.00380 0.00596 AFIX 43 H7 2 0.159340 1.219888 0.212702 11.00000 -1.20000 AFIX 0 C8 1 0.128343 1.093127 0.247046 11.00000 0.01604 0.01571 = 0.02225 0.00624 0.00091 0.00460 C9 1 0.020732 1.018172 0.219306 11.00000 0.01753 0.01807 = 0.02088 0.00615 0.00287 0.00522 C10 1 -0.034167 1.032776 0.178021 11.00000 0.02210 0.02485 = 0.02277 0.00922 -0.00041 0.00395 AFIX 43 H10 2 -0.004470 1.098884 0.167529 11.00000 -1.20000 AFIX 0 C11 1 -0.131687 0.951498 0.152240 11.00000 0.02182 0.03142 = 0.02540 0.00796 -0.00287 0.00591 C12 1 -0.174477 0.857089 0.169959 11.00000 0.02265 0.03047 = 0.02945 0.00809 -0.00693 -0.00043 AFIX 43 H12 2 -0.241999 0.800605 0.153497 11.00000 -1.20000 AFIX 0 C13 1 -0.119660 0.845600 0.210867 11.00000 0.02179 0.02099 = 0.02798 0.01280 -0.00072 -0.00229 AFIX 43 H13 2 -0.149953 0.781026 0.222471 11.00000 -1.20000 AFIX 0 C14 1 0.000128 1.002460 0.344379 11.00000 0.01472 0.01123 = 0.02297 0.00736 0.00544 0.00381 C15 1 -0.082716 1.044229 0.335586 11.00000 0.01879 0.02498 = 0.02762 0.01298 0.00539 0.00959 AFIX 43 H15 2 -0.109969 1.038800 0.302361 11.00000 -1.20000 AFIX 0 C16 1 -0.126660 1.093518 0.373856 11.00000 0.02213 0.03356 = 0.03368 0.01609 0.00983 0.01668 AFIX 43 H16 2 -0.182155 1.122598 0.366595 11.00000 -1.20000 AFIX 0 C17 1 -0.090423 1.100743 0.422532 11.00000 0.02804 0.03137 = 0.03023 0.01300 0.01241 0.01686 AFIX 43 H17 2 -0.120969 1.134464 0.448684 11.00000 -1.20000 AFIX 0 C18 1 -0.009310 1.058538 0.432976 11.00000 0.02305 0.02639 = 0.02457 0.01034 0.00823 0.01251 AFIX 43 H18 2 0.015831 1.063123 0.466379 11.00000 -1.20000 AFIX 0 C19 1 0.035270 1.009563 0.394697 11.00000 0.01691 0.01749 = 0.02314 0.01028 0.00627 0.00693 C20 1 0.123357 0.965185 0.402614 11.00000 0.01780 0.01849 = 0.02154 0.00829 0.00615 0.00712 C21 1 0.174766 0.967622 0.448197 11.00000 0.01805 0.02205 = 0.02181 0.00768 0.00578 0.00904 AFIX 43 H21 2 0.151135 0.997773 0.477698 11.00000 -1.20000 AFIX 0 C22 1 0.260171 0.926683 0.451338 11.00000 0.01638 0.01979 = 0.02498 0.00807 0.00269 0.00553 C23 1 0.293708 0.886174 0.407244 11.00000 0.02150 0.02637 = 0.02672 0.00865 0.00452 0.01328 AFIX 43 H23 2 0.353629 0.859635 0.407808 11.00000 -1.20000 AFIX 0 C24 1 0.240198 0.884477 0.362777 11.00000 0.02049 0.02058 = 0.02248 0.00590 0.00434 0.01055 AFIX 43 H24 2 0.264569 0.857102 0.332936 11.00000 -1.20000 AFIX 0 C25 1 -0.017369 0.409003 0.240636 11.00000 0.02180 0.01997 = 0.02387 0.00501 0.00100 0.00724 C26 1 0.013780 0.359736 0.275932 11.00000 0.02307 0.02382 = 0.03073 0.00674 -0.00185 0.00939 AFIX 43 H26 2 0.088062 0.389656 0.292684 11.00000 -1.20000 AFIX 0 C27 1 -0.061069 0.269140 0.286700 11.00000 0.03448 0.02317 = 0.03679 0.01089 -0.00369 0.00996 AFIX 43 H27 2 -0.037830 0.237874 0.311072 11.00000 -1.20000 AFIX 0 C28 1 -0.170934 0.221582 0.262647 11.00000 0.03508 0.01961 = 0.04686 0.01522 -0.00319 0.00239 AFIX 43 H28 2 -0.222047 0.158849 0.270569 11.00000 -1.20000 AFIX 0 C29 1 -0.203515 0.266995 0.227500 11.00000 0.02567 0.02155 = 0.04383 0.01192 -0.00366 0.00082 AFIX 43 H29 2 -0.277908 0.235769 0.210853 11.00000 -1.20000 AFIX 0 C30 1 -0.128176 0.358642 0.216063 11.00000 0.02625 0.01956 = 0.02991 0.00861 -0.00367 0.00747 C31 1 -0.156521 0.414178 0.179739 11.00000 0.02432 0.02203 = 0.02996 0.00963 -0.00300 0.00285 C32 1 -0.260488 0.385035 0.151670 11.00000 0.02415 0.03244 = 0.03230 0.01210 -0.00561 0.00267 AFIX 43 H32 2 -0.321076 0.323266 0.155116 11.00000 -1.20000 AFIX 0 C33 1 -0.276096 0.445782 0.118657 11.00000 0.03109 0.03844 = 0.03344 0.01342 -0.00615 0.00544 C34 1 -0.184817 0.535202 0.114859 11.00000 0.03161 0.04579 = 0.04263 0.02648 -0.00776 0.00637 AFIX 43 H34 2 -0.192449 0.577907 0.092445 11.00000 -1.20000 AFIX 0 C35 1 -0.082842 0.562729 0.143400 11.00000 0.02544 0.03709 = 0.03669 0.02033 -0.00184 0.00274 AFIX 43 H35 2 -0.021849 0.625157 0.140891 11.00000 -1.20000 AFIX 0 C36 1 0.136175 0.438330 0.176102 11.00000 0.02807 0.02339 = 0.02093 0.00474 -0.00019 0.00961 C37 1 0.083863 0.359624 0.132090 11.00000 0.03756 0.02961 = 0.03011 0.00173 -0.00149 0.00967 AFIX 43 H37 2 0.008831 0.347892 0.120200 11.00000 -1.20000 AFIX 0 C38 1 0.139123 0.298476 0.105497 11.00000 0.04609 0.03359 = 0.03067 -0.00054 0.00330 0.01235 AFIX 43 H38 2 0.101173 0.244970 0.075977 11.00000 -1.20000 AFIX 0 C39 1 0.248791 0.314310 0.121362 11.00000 0.04520 0.03044 = 0.02996 0.00657 0.01302 0.01481 AFIX 43 H39 2 0.286685 0.273422 0.102413 11.00000 -1.20000 AFIX 0 C40 1 0.302839 0.390164 0.165043 11.00000 0.03211 0.02745 = 0.03084 0.00925 0.01042 0.01269 AFIX 43 H40 2 0.377722 0.400350 0.176433 11.00000 -1.20000 AFIX 0 C41 1 0.248329 0.451688 0.192436 11.00000 0.02603 0.02385 = 0.02339 0.00672 0.00389 0.00948 C42 1 0.294715 0.526192 0.240874 11.00000 0.02006 0.01668 = 0.02464 0.00824 0.00662 0.00326 C43 1 0.401155 0.551725 0.266287 11.00000 0.02050 0.01285 = 0.02906 0.00763 0.00761 0.00592 AFIX 43 H43 2 0.453586 0.525769 0.250111 11.00000 -1.20000 AFIX 0 C44 1 0.431282 0.614249 0.314657 11.00000 0.01752 0.01501 = 0.02998 0.00619 0.00433 0.00520 C45 1 0.352183 0.650792 0.337040 11.00000 0.02119 0.02247 = 0.02610 0.00266 0.00142 0.00899 AFIX 43 H45 2 0.368409 0.691560 0.370537 11.00000 -1.20000 AFIX 0 C46 1 0.249562 0.626963 0.309858 11.00000 0.01882 0.02600 = 0.02436 0.00076 0.00115 0.01140 AFIX 43 H46 2 0.196671 0.653559 0.325233 11.00000 -1.20000 AFIX 0 C47 1 0.237452 0.872166 0.205542 11.00000 0.02027 0.02079 = 0.02635 0.00385 0.00785 0.00653 C48 1 0.198618 0.909979 0.168338 11.00000 0.02863 0.03509 = 0.03406 0.01438 0.01238 0.01570 C49 1 0.264598 1.005796 0.156126 11.00000 0.04163 0.03677 = 0.04355 0.01964 0.02020 0.01808 C50 1 0.371493 1.061937 0.179960 11.00000 0.03941 0.02899 = 0.04023 0.00861 0.02357 0.00854 C51 1 0.413242 1.024119 0.216337 11.00000 0.03530 0.03198 = 0.03074 0.00210 0.01314 0.00018 C52 1 0.345950 0.929117 0.228378 11.00000 0.02690 0.03195 = 0.02356 0.00469 0.00670 0.00164 C53 1 -0.119183 0.582260 0.300597 11.00000 0.01806 0.01631 = 0.02619 0.00638 0.00557 0.00546 C54 1 -0.228747 0.543777 0.279121 11.00000 0.01853 0.01927 = 0.03244 0.00874 0.00069 0.00613 C55 1 -0.309395 0.459145 0.292403 11.00000 0.01689 0.01640 = 0.04840 0.01026 0.00417 0.00077 C56 1 -0.279545 0.413176 0.328043 11.00000 0.02942 0.02508 = 0.05350 0.01909 0.01168 0.00612 C57 1 -0.171948 0.450559 0.350741 11.00000 0.03208 0.03111 = 0.04415 0.02380 0.01075 0.01263 C58 1 -0.092063 0.535164 0.336875 11.00000 0.02285 0.02036 = 0.02674 0.00868 0.00400 0.00885 C59 1 -0.190533 0.960443 0.106138 11.00000 0.02313 0.04166 = 0.02892 0.01192 -0.00562 0.00420 C60 1 -0.144608 0.950349 0.061991 11.00000 0.03019 0.07489 = 0.03320 0.02428 0.00437 0.01652 C61 1 -0.202327 0.954337 0.019141 11.00000 0.04065 0.08944 = 0.03435 0.02906 0.00685 0.02650 AFIX 43 H61 2 -0.171817 0.945534 -0.011102 11.00000 -1.20000 AFIX 0 C62 1 -0.301892 0.970604 0.019397 11.00000 0.04402 0.07555 = 0.03264 0.01615 -0.00238 0.02567 C63 1 -0.346480 0.980617 0.063097 11.00000 0.03749 0.07409 = 0.03327 0.00944 -0.00445 0.02619 AFIX 43 H63 2 -0.416259 0.990762 0.063411 11.00000 -1.20000 AFIX 0 C64 1 -0.292079 0.976303 0.107153 11.00000 0.02960 0.04334 = 0.03077 0.00159 -0.00543 0.01147 C65 1 -0.037520 0.927740 0.058969 11.00000 0.04605 0.15234 = 0.04471 0.04400 0.01549 0.04829 AFIX 137 H65A 2 0.025501 0.993486 0.076239 11.00000 21.00000 H65B 2 -0.027239 0.907557 0.024144 11.00000 21.00000 H65C 2 -0.041156 0.867471 0.074558 11.00000 21.00000 AFIX 0 C66 1 -0.364524 0.972537 -0.028520 11.00000 0.07089 0.13681 = 0.03572 0.02261 -0.00012 0.06326 AFIX 137 H66A 2 -0.322655 1.038147 -0.039466 11.00000 31.00000 H66B 2 -0.438807 0.973522 -0.022625 11.00000 31.00000 H66C 2 -0.372270 0.907180 -0.054196 11.00000 31.00000 AFIX 0 C67 1 -0.345922 0.985776 0.153500 11.00000 0.05001 0.07577 = 0.03256 0.00481 -0.00050 0.03365 AFIX 137 H67A 2 -0.377835 0.913346 0.160443 11.00000 41.00000 H67B 2 -0.405362 1.015003 0.149061 11.00000 41.00000 H67C 2 -0.289763 1.035172 0.181289 11.00000 41.00000 AFIX 0 C68 1 0.312967 0.925442 0.499990 11.00000 0.01691 0.02219 = 0.02251 0.00803 0.00398 0.00750 C69 1 0.297691 0.824042 0.511745 11.00000 0.02417 0.02563 = 0.02943 0.00958 0.00425 0.00934 C70 1 0.342040 0.825442 0.558704 11.00000 0.02814 0.02918 = 0.03236 0.01414 0.00215 0.01333 AFIX 43 H70 2 0.333303 0.757816 0.566960 11.00000 -1.20000 AFIX 0 C71 1 0.398226 0.921511 0.593688 11.00000 0.02348 0.03392 = 0.02917 0.01356 0.00207 0.01040 C72 1 0.411876 1.019817 0.581028 11.00000 0.02009 0.02694 = 0.02651 0.00598 -0.00011 0.00699 AFIX 43 H72 2 0.449943 1.086359 0.605050 11.00000 -1.20000 AFIX 0 C73 1 0.372005 1.024323 0.534661 11.00000 0.01753 0.02581 = 0.02766 0.00897 0.00388 0.00768 C74 1 0.231664 0.715827 0.476124 11.00000 0.05569 0.02304 = 0.03621 0.01003 0.00110 0.00738 AFIX 137 H74A 2 0.167640 0.722392 0.457923 11.00000 51.00000 H74B 2 0.204937 0.659260 0.494655 11.00000 51.00000 H74C 2 0.279582 0.695629 0.452687 11.00000 51.00000 AFIX 0 C75 1 0.443076 0.922345 0.645517 11.00000 0.04095 0.05788 = 0.03662 0.02081 -0.00861 0.01057 AFIX 137 H75A 2 0.516037 0.913991 0.645061 11.00000 61.00000 H75B 2 0.390933 0.861717 0.656650 11.00000 61.00000 H75C 2 0.451174 0.991863 0.668257 11.00000 61.00000 AFIX 0 C76 1 0.395533 1.134212 0.522481 11.00000 0.03493 0.02482 = 0.03577 0.00886 0.00071 0.00734 AFIX 137 H76A 2 0.431281 1.135287 0.492280 11.00000 71.00000 H76B 2 0.445388 1.191979 0.549981 11.00000 71.00000 H76C 2 0.325196 1.146678 0.517278 11.00000 71.00000 AFIX 0 C77 1 -0.384615 0.415839 0.086791 11.00000 0.03243 0.04426 = 0.04180 0.02228 -0.01120 0.00192 C78 1 -0.414775 0.328963 0.045848 11.00000 0.05307 0.05665 = 0.04625 0.01077 -0.02085 0.01142 C79 1 -0.512788 0.308729 0.014146 11.00000 0.05670 0.07575 = 0.04977 0.01132 -0.02715 0.01132 AFIX 43 H79 2 -0.534139 0.249020 -0.014160 11.00000 -1.20000 AFIX 0 C80 1 -0.577812 0.369722 0.021909 11.00000 0.03360 0.06057 = 0.05355 0.03406 -0.01430 -0.00490 C81 1 -0.546162 0.455459 0.063169 11.00000 0.03229 0.05986 = 0.06770 0.02683 -0.01600 0.00156 AFIX 43 H81 2 -0.591159 0.499207 0.069325 11.00000 -1.20000 AFIX 0 C82 1 -0.449244 0.480766 0.096684 11.00000 0.02839 0.05184 = 0.06147 0.02289 -0.01015 0.00092 C83 1 -0.345224 0.258410 0.035005 11.00000 0.10543 0.11725 = 0.08005 -0.03324 -0.04947 0.06649 AFIX 137 H83A 2 -0.266999 0.304944 0.036325 11.00000 81.00000 H83B 2 -0.372318 0.209499 0.001904 11.00000 81.00000 H83C 2 -0.350998 0.214776 0.059713 11.00000 81.00000 AFIX 0 C84 1 -0.681427 0.345609 -0.014171 11.00000 0.04593 0.10484 = 0.06670 0.04835 -0.02304 0.00082 AFIX 137 H84A 2 -0.748355 0.312970 0.000727 11.00000 91.00000 H84B 2 -0.680580 0.294466 -0.044797 11.00000 91.00000 H84C 2 -0.682153 0.413844 -0.021705 11.00000 91.00000 AFIX 0 C85 1 -0.421998 0.573894 0.142309 11.00000 0.04147 0.07315 = 0.09121 -0.00575 -0.02130 0.01561 AFIX 137 H85A 2 -0.419484 0.545843 0.172055 11.00000 101.00000 H85B 2 -0.479672 0.606810 0.142647 11.00000 101.00000 H85C 2 -0.349196 0.629325 0.141764 11.00000 101.00000 AFIX 0 C86 1 0.543849 0.643322 0.343285 11.00000 0.01580 0.01979 = 0.02748 0.00065 0.00297 0.00511 C87 1 0.555987 0.588809 0.379762 11.00000 0.02013 0.02103 = 0.03140 0.00263 0.00142 0.00548 C88 1 0.660797 0.620424 0.407362 11.00000 0.02130 0.03089 = 0.03119 0.00470 0.00078 0.00922 AFIX 43 H88 2 0.669919 0.582205 0.431575 11.00000 -1.20000 AFIX 0 C89 1 0.752460 0.706255 0.400529 11.00000 0.02137 0.03556 = 0.02822 -0.00112 0.00143 0.00837 C90 1 0.737408 0.760354 0.364658 11.00000 0.01634 0.03128 = 0.03437 0.00332 0.00522 0.00190 AFIX 43 H90 2 0.798861 0.819337 0.359529 11.00000 -1.20000 AFIX 0 C91 1 0.633861 0.729999 0.335913 11.00000 0.01824 0.02058 = 0.03308 0.00237 0.00429 0.00712 C92 1 0.459846 0.496985 0.390089 11.00000 0.02419 0.02624 = 0.04909 0.01448 -0.00171 0.00063 AFIX 137 H92A 2 0.414217 0.527596 0.411335 11.00000 111.00000 H92B 2 0.488913 0.452287 0.406862 11.00000 111.00000 H92C 2 0.413907 0.451377 0.358783 11.00000 111.00000 AFIX 0 C93 1 0.864389 0.740915 0.431545 11.00000 0.02563 0.04931 = 0.03919 -0.00123 -0.00432 0.00992 AFIX 137 H93A 2 0.921532 0.738759 0.409812 11.00000 121.00000 H93B 2 0.860806 0.690965 0.453225 11.00000 121.00000 H93C 2 0.883606 0.815555 0.451765 11.00000 121.00000 AFIX 0 C94 1 0.624903 0.790644 0.296178 11.00000 0.03141 0.03365 = 0.04206 0.01346 0.00468 0.00918 AFIX 137 H94A 2 0.614330 0.741726 0.263374 11.00000 131.00000 H94B 2 0.693588 0.854466 0.299961 11.00000 131.00000 H94C 2 0.561019 0.814826 0.299588 11.00000 131.00000 AFIX 0 CL1 3 0.147799 1.413732 0.412995 11.00000 0.06904 0.04667 = 0.09420 -0.00296 0.00033 0.03116 CL2 3 0.268972 1.280215 0.441535 11.00000 0.04533 0.05341 = 0.06322 0.02815 -0.00344 0.00621 PART 1 CL6 3 -0.624918 0.741266 0.109743 10.50000 0.11694 0.09666 = 0.09364 0.03497 0.05426 0.07083 CL7 3 -0.852932 0.679861 0.065103 10.50000 0.13676 0.27890 = 0.12633 0.11420 0.07400 0.13632 PART 0 PART 2 CL3 3 -0.548164 0.744654 0.184644 10.40000 0.09800 0.11176 = 0.08578 0.03335 0.01610 0.05021 CL4 3 -0.623187 0.793478 0.099428 10.27000 0.09456 CL5 3 -0.600585 0.723883 0.077104 10.13000 0.11085 PART 0 PART 3 CL8 3 -0.851923 0.535311 0.030442 10.10000 0.10560 CL9 3 -0.982522 0.634910 0.019229 10.10000 0.11710 PART 0 C95 1 0.175949 1.292919 0.396273 11.00000 0.03651 0.02771 = 0.04492 0.01011 0.00658 0.00606 AFIX 23 H95A 2 0.208205 1.290929 0.364745 11.00000 -1.20000 H95B 2 0.104907 1.229588 0.390565 11.00000 -1.20000 AFIX 0 PART 1 C97 1 -0.750572 0.631952 0.086267 10.50000 0.07918 AFIX 3 H97A 2 -0.738362 0.578692 0.058807 10.50000 -1.20000 H97B 2 -0.777342 0.595742 0.113207 10.50000 -1.20000 AFIX 0 PART 0 PART 2 C96 1 -0.646576 0.686882 0.130735 10.40000 0.09289 AFIX 3 H96A 2 -0.634536 0.622932 0.110195 10.40000 -1.20000 H96B 2 -0.723485 0.664052 0.139505 10.40000 -1.20000 AFIX 0 HKLF 4 REM 16srv477 in P-1 #2 REM R1 = 0.0624 for 19773 Fo > 4sig(Fo) and 0.0861 for all 25354 data REM 1129 parameters refined using 1090 restraints END WGHT 0.0000 44.0980 REM Highest difference peak 3.223, deepest hole -7.359, 1-sigma level 0.182 Q1 1 0.3474 0.8228 0.3253 11.00000 0.05 3.22 Q2 1 -0.2251 0.5823 0.1852 11.00000 0.05 3.07 Q3 1 -0.2352 0.9573 0.2634 11.00000 0.05 3.07 Q4 1 -0.1879 0.6800 0.1930 11.00000 0.05 2.98 Q5 1 0.3588 0.4486 0.2476 11.00000 0.05 2.93 Q6 1 0.0470 1.2829 0.3717 11.00000 0.05 2.82 Q7 1 -0.2000 0.0566 0.2721 11.00000 0.05 2.50 Q8 1 0.1218 0.5322 0.1975 11.00000 0.05 2.45 Q9 1 -0.1843 1.0442 0.2654 11.00000 0.05 2.16 Q10 1 0.0752 0.9241 0.3233 11.00000 0.05 2.14 Q11 1 0.0960 0.9805 0.2991 11.00000 0.05 1.90 Q12 1 0.0875 1.1648 0.1415 11.00000 0.05 1.89 Q13 1 0.1145 0.9193 0.2818 11.00000 0.05 1.76 Q14 1 0.0782 0.8606 0.2876 11.00000 0.05 1.40 Q15 1 -0.7959 0.5393 0.0295 11.00000 0.05 1.39 Q16 1 0.1044 0.6022 0.2230 11.00000 0.05 1.21 Q17 1 0.0472 0.5485 0.2484 11.00000 0.05 1.19 Q18 1 0.3357 1.1997 0.4042 11.00000 0.05 1.02 Q19 1 -0.9071 0.5087 0.0360 11.00000 0.05 0.96 Q20 1 -0.5161 0.6751 0.1633 11.00000 0.05 0.90 Q21 1 -1.0805 0.5598 -0.0020 11.00000 0.05 0.88 Q22 1 -0.8958 0.7802 -0.0159 11.00000 0.05 0.86 Q23 1 0.1810 1.4177 0.4434 11.00000 0.05 0.82 Q24 1 -0.0032 0.9030 0.3022 11.00000 0.05 0.82 Q25 1 0.0218 0.4884 0.2343 11.00000 0.05 0.80 Q26 1 -0.2067 0.2159 0.1145 11.00000 0.05 0.79 Q27 1 -0.2265 0.4247 0.3409 11.00000 0.05 0.77 Q28 1 -0.9210 0.7459 0.0024 11.00000 0.05 0.77 Q29 1 -0.3547 0.3603 0.2733 11.00000 0.05 0.77 Q30 1 -0.5980 0.8399 0.1012 11.00000 0.05 0.74 Q31 1 0.5005 1.1483 0.2346 11.00000 0.05 0.71 Q32 1 0.4459 0.5847 0.2171 11.00000 0.05 0.71 Q33 1 -1.0252 0.5421 -0.0197 11.00000 0.05 0.68 Q34 1 0.0215 0.8434 0.3115 11.00000 0.05 0.67 Q35 1 0.5397 1.1892 0.4737 11.00000 0.05 0.66 Q36 1 -0.9897 0.5371 -0.0117 11.00000 0.05 0.66 Q37 1 0.3370 0.5241 0.2498 11.00000 0.05 0.65 Q38 1 -0.0017 1.3767 0.4215 11.00000 0.05 0.64 Q39 1 0.0081 0.8998 0.2593 11.00000 0.05 0.63 Q40 1 -0.1772 0.9174 0.2310 11.00000 0.05 0.62 ; _shelx_res_checksum 3259 _olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems' _olex2_submission_special_instructions 'No special instructions were received' 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 0.06467(2) 0.91451(2) 0.29624(2) 0.01578(6) Uani 1 1 d . U . . . Ir2 Ir 0.07677(2) 0.53999(2) 0.21927(2) 0.01940(6) Uani 1 1 d . U . . . F1 F 0.0954(4) 0.8573(4) 0.14438(18) 0.0400(11) Uani 1 1 d . U . . . F2 F 0.2234(5) 1.0439(5) 0.1218(2) 0.0566(15) Uani 1 1 d . U . . . F3 F 0.4357(5) 1.1525(4) 0.1683(2) 0.0568(15) Uani 1 1 d . U . . . F4 F 0.5174(5) 1.0761(5) 0.2397(2) 0.0596(16) Uani 1 1 d . U . . . F5 F 0.3866(4) 0.8923(4) 0.26374(17) 0.0453(13) Uani 1 1 d . U . . . F6 F -0.2595(3) 0.5883(4) 0.24436(16) 0.0313(9) Uani 1 1 d . U . . . F7 F -0.4148(3) 0.4200(4) 0.2693(2) 0.0430(12) Uani 1 1 d . U . . . F8 F -0.3580(4) 0.3320(4) 0.3412(2) 0.0567(15) Uani 1 1 d . U . . . F9 F -0.1442(4) 0.4073(4) 0.3860(2) 0.0506(14) Uani 1 1 d . U . . . F10 F 0.0126(3) 0.5733(4) 0.36008(16) 0.0315(9) Uani 1 1 d . U . . . O1 O -0.0576(4) 0.7699(4) 0.30684(17) 0.0213(9) Uani 1 1 d . U . . . O2 O 0.1712(4) 0.6802(4) 0.19278(18) 0.0242(10) Uani 1 1 d . U . . . N1 N 0.1055(4) 0.7797(4) 0.2536(2) 0.0172(10) Uani 1 1 d . U . . . N2 N 0.0401(4) 0.6748(4) 0.2623(2) 0.0178(10) Uani 1 1 d . U . . . N3 N -0.0224(4) 0.9249(4) 0.2353(2) 0.0198(10) Uani 1 1 d . U . . . N4 N 0.1539(4) 0.9206(4) 0.3602(2) 0.0178(10) Uani 1 1 d . U . . . N5 N -0.0689(5) 0.5019(5) 0.1748(2) 0.0238(11) Uani 1 1 d . U . . . N6 N 0.2216(4) 0.5683(4) 0.2630(2) 0.0197(10) Uani 1 1 d . U . . . C1 C 0.1665(5) 0.7694(5) 0.2183(2) 0.0206(12) Uani 1 1 d . U . . . C2 C -0.0385(5) 0.6826(5) 0.2892(2) 0.0174(11) Uani 1 1 d . U . . . C3 C 0.1702(5) 1.0535(5) 0.2848(2) 0.0171(11) Uani 1 1 d . U . . . C4 C 0.2765(5) 1.1182(5) 0.3106(2) 0.0211(12) Uani 1 1 d . U . . . H4 H 0.3070 1.0949 0.3362 0.025 Uiso 1 1 calc R . . . . C5 C 0.3381(6) 1.2162(5) 0.2992(3) 0.0240(13) Uani 1 1 d . U . . . H5 H 0.4106 1.2581 0.3167 0.029 Uiso 1 1 calc R . . . . C6 C 0.2949(6) 1.2533(6) 0.2627(3) 0.0257(14) Uani 1 1 d . U . . . H6 H 0.3379 1.3203 0.2553 0.031 Uiso 1 1 calc R . . . . C7 C 0.1899(6) 1.1933(5) 0.2371(3) 0.0221(13) Uani 1 1 d . U . . . H7 H 0.1593 1.2199 0.2127 0.027 Uiso 1 1 calc R . . . . C8 C 0.1283(5) 1.0931(5) 0.2470(2) 0.0181(12) Uani 1 1 d . U . . . C9 C 0.0207(5) 1.0182(5) 0.2193(2) 0.0189(12) Uani 1 1 d . U . . . C10 C -0.0342(6) 1.0328(6) 0.1780(2) 0.0240(13) Uani 1 1 d . U . . . H10 H -0.0045 1.0989 0.1675 0.029 Uiso 1 1 calc R . . . . C11 C -0.1317(6) 0.9515(6) 0.1522(3) 0.0272(14) Uani 1 1 d . U . . . C12 C -0.1745(6) 0.8571(6) 0.1700(3) 0.0304(16) Uani 1 1 d . U . . . H12 H -0.2420 0.8006 0.1535 0.037 Uiso 1 1 calc R . . . . C13 C -0.1197(6) 0.8456(6) 0.2109(3) 0.0253(14) Uani 1 1 d . U . . . H13 H -0.1500 0.7810 0.2225 0.030 Uiso 1 1 calc R . . . . C14 C 0.0001(5) 1.0025(5) 0.3444(2) 0.0159(11) Uani 1 1 d . U . . . C15 C -0.0827(5) 1.0442(5) 0.3356(3) 0.0222(13) Uani 1 1 d . U . . . H15 H -0.1100 1.0388 0.3024 0.027 Uiso 1 1 calc R . . . . C16 C -0.1267(6) 1.0935(6) 0.3739(3) 0.0265(14) Uani 1 1 d . U . . . H16 H -0.1822 1.1226 0.3666 0.032 Uiso 1 1 calc R . . . . C17 C -0.0904(6) 1.1007(6) 0.4225(3) 0.0270(14) Uani 1 1 d . U . . . H17 H -0.1210 1.1345 0.4487 0.032 Uiso 1 1 calc R . . . . C18 C -0.0093(6) 1.0585(6) 0.4330(3) 0.0228(13) Uani 1 1 d . U . . . H18 H 0.0158 1.0631 0.4664 0.027 Uiso 1 1 calc R . . . . C19 C 0.0353(5) 1.0096(5) 0.3947(2) 0.0180(11) Uani 1 1 d . U . . . C20 C 0.1234(5) 0.9652(5) 0.4026(2) 0.0184(11) Uani 1 1 d . U . . . C21 C 0.1748(5) 0.9676(5) 0.4482(2) 0.0196(12) Uani 1 1 d . U . . . H21 H 0.1511 0.9978 0.4777 0.024 Uiso 1 1 calc R . . . . C22 C 0.2602(5) 0.9267(5) 0.4513(2) 0.0202(12) Uani 1 1 d . U . . . C23 C 0.2937(6) 0.8862(6) 0.4072(3) 0.0232(13) Uani 1 1 d . U . . . H23 H 0.3536 0.8596 0.4078 0.028 Uiso 1 1 calc R . . . . C24 C 0.2402(5) 0.8845(5) 0.3628(2) 0.0202(12) Uani 1 1 d . U . . . H24 H 0.2646 0.8571 0.3329 0.024 Uiso 1 1 calc R . . . . C25 C -0.0174(6) 0.4090(5) 0.2406(2) 0.0221(12) Uani 1 1 d . U . . . C26 C 0.0138(6) 0.3597(6) 0.2759(3) 0.0258(14) Uani 1 1 d . U . . . H26 H 0.0881 0.3897 0.2927 0.031 Uiso 1 1 calc R . . . . C27 C -0.0611(7) 0.2691(6) 0.2867(3) 0.0313(16) Uani 1 1 d . U . . . H27 H -0.0378 0.2379 0.3111 0.038 Uiso 1 1 calc R . . . . C28 C -0.1709(7) 0.2216(6) 0.2626(3) 0.0350(17) Uani 1 1 d . U . . . H28 H -0.2220 0.1588 0.2706 0.042 Uiso 1 1 calc R . . . . C29 C -0.2035(6) 0.2670(6) 0.2275(3) 0.0321(16) Uani 1 1 d . U . . . H29 H -0.2779 0.2358 0.2109 0.038 Uiso 1 1 calc R . . . . C30 C -0.1282(6) 0.3586(6) 0.2161(3) 0.0253(14) Uani 1 1 d . U . . . C31 C -0.1565(6) 0.4142(6) 0.1797(3) 0.0266(14) Uani 1 1 d . U . . . C32 C -0.2605(6) 0.3850(6) 0.1517(3) 0.0313(16) Uani 1 1 d . U . . . H32 H -0.3211 0.3233 0.1551 0.038 Uiso 1 1 calc R . . . . C33 C -0.2761(7) 0.4458(7) 0.1187(3) 0.0358(17) Uani 1 1 d . U . . . C34 C -0.1848(7) 0.5352(7) 0.1149(3) 0.040(2) Uani 1 1 d . U . . . H34 H -0.1924 0.5779 0.0924 0.048 Uiso 1 1 calc R . . . . C35 C -0.0828(6) 0.5627(7) 0.1434(3) 0.0338(17) Uani 1 1 d . U . . . H35 H -0.0218 0.6252 0.1409 0.041 Uiso 1 1 calc R . . . . C36 C 0.1362(6) 0.4383(6) 0.1761(3) 0.0242(13) Uani 1 1 d . U . . . C37 C 0.0839(7) 0.3596(6) 0.1321(3) 0.0341(16) Uani 1 1 d . U . . . H37 H 0.0088 0.3479 0.1202 0.041 Uiso 1 1 calc R . . . . C38 C 0.1391(7) 0.2985(7) 0.1055(3) 0.0386(18) Uani 1 1 d . U . . . H38 H 0.1012 0.2450 0.0760 0.046 Uiso 1 1 calc R . . . . C39 C 0.2488(7) 0.3143(6) 0.1214(3) 0.0346(16) Uani 1 1 d . U . . . H39 H 0.2867 0.2734 0.1024 0.042 Uiso 1 1 calc R . . . . C40 C 0.3028(6) 0.3902(6) 0.1650(3) 0.0290(14) Uani 1 1 d . U . . . H40 H 0.3777 0.4004 0.1764 0.035 Uiso 1 1 calc R . . . . C41 C 0.2483(6) 0.4517(6) 0.1924(3) 0.0241(13) Uani 1 1 d . U . . . C42 C 0.2947(5) 0.5262(5) 0.2409(2) 0.0207(12) Uani 1 1 d . U . . . C43 C 0.4012(5) 0.5517(5) 0.2663(2) 0.0202(12) Uani 1 1 d . U . . . H43 H 0.4536 0.5258 0.2501 0.024 Uiso 1 1 calc R . . . . C44 C 0.4313(5) 0.6142(5) 0.3147(3) 0.0208(12) Uani 1 1 d . U . . . C45 C 0.3522(6) 0.6508(6) 0.3370(3) 0.0235(13) Uani 1 1 d . U . . . H45 H 0.3684 0.6916 0.3705 0.028 Uiso 1 1 calc R . . . . C46 C 0.2496(6) 0.6270(6) 0.3099(3) 0.0231(13) Uani 1 1 d . U . . . H46 H 0.1967 0.6536 0.3252 0.028 Uiso 1 1 calc R . . . . C47 C 0.2375(6) 0.8722(5) 0.2055(3) 0.0228(12) Uani 1 1 d . U . . . C48 C 0.1986(6) 0.9100(6) 0.1683(3) 0.0302(14) Uani 1 1 d . U . . . C49 C 0.2646(7) 1.0058(7) 0.1561(3) 0.0374(16) Uani 1 1 d . U . . . C50 C 0.3715(7) 1.0619(6) 0.1800(3) 0.0364(16) Uani 1 1 d . U . . . C51 C 0.4132(7) 1.0241(7) 0.2163(3) 0.0363(16) Uani 1 1 d . U . . . C52 C 0.3459(6) 0.9291(6) 0.2284(3) 0.0300(15) Uani 1 1 d . U . . . C53 C -0.1192(5) 0.5823(5) 0.3006(2) 0.0201(12) Uani 1 1 d . U . . . C54 C -0.2287(5) 0.5438(5) 0.2791(3) 0.0233(13) Uani 1 1 d . U . . . C55 C -0.3094(6) 0.4591(6) 0.2924(3) 0.0282(14) Uani 1 1 d . U . . . C56 C -0.2795(7) 0.4132(6) 0.3280(3) 0.0352(16) Uani 1 1 d . U . . . C57 C -0.1719(7) 0.4506(6) 0.3507(3) 0.0329(16) Uani 1 1 d . U . . . C58 C -0.0921(6) 0.5352(5) 0.3369(3) 0.0225(13) Uani 1 1 d . U . . . C59 C -0.1905(6) 0.9604(7) 0.1061(3) 0.0330(16) Uani 1 1 d . U . . . C60 C -0.1446(7) 0.9503(9) 0.0620(3) 0.045(2) Uani 1 1 d . U . . . C61 C -0.2023(8) 0.9543(9) 0.0191(3) 0.052(2) Uani 1 1 d . U . . . H61 H -0.1718 0.9455 -0.0111 0.062 Uiso 1 1 calc R . . . . C62 C -0.3019(8) 0.9706(9) 0.0194(3) 0.049(2) Uani 1 1 d . U . . . C63 C -0.3465(8) 0.9806(9) 0.0631(3) 0.048(2) Uani 1 1 d . U . . . H63 H -0.4163 0.9908 0.0634 0.057 Uiso 1 1 calc R . . . . C64 C -0.2921(7) 0.9763(7) 0.1072(3) 0.0365(17) Uani 1 1 d . U . . . C65 C -0.0375(9) 0.9277(12) 0.0590(4) 0.074(4) Uani 1 1 d . U . . . H65A H 0.0255 0.9935 0.0762 0.08(2) Uiso 1 1 calc GR . . . . H65B H -0.0272 0.9076 0.0241 0.08(2) Uiso 1 1 calc GR . . . . H65C H -0.0412 0.8675 0.0746 0.08(2) Uiso 1 1 calc GR . . . . C66 C -0.3645(10) 0.9725(12) -0.0285(4) 0.074(4) Uani 1 1 d . U . . . H66A H -0.3227 1.0381 -0.0395 0.11(3) Uiso 1 1 calc GR . . . . H66B H -0.4388 0.9735 -0.0226 0.11(3) Uiso 1 1 calc GR . . . . H66C H -0.3723 0.9072 -0.0542 0.11(3) Uiso 1 1 calc GR . . . . C67 C -0.3459(8) 0.9858(9) 0.1535(3) 0.051(2) Uani 1 1 d . U . . . H67A H -0.3778 0.9133 0.1604 0.049(16) Uiso 1 1 calc GR . . . . H67B H -0.4054 1.0150 0.1491 0.049(16) Uiso 1 1 calc GR . . . . H67C H -0.2898 1.0352 0.1813 0.049(16) Uiso 1 1 calc GR . . . . C68 C 0.3130(5) 0.9254(5) 0.5000(2) 0.0199(12) Uani 1 1 d . U . . . C69 C 0.2977(6) 0.8240(6) 0.5117(3) 0.0258(13) Uani 1 1 d . U . . . C70 C 0.3420(6) 0.8254(6) 0.5587(3) 0.0281(14) Uani 1 1 d . U . . . H70 H 0.3333 0.7578 0.5670 0.034 Uiso 1 1 calc R . . . . C71 C 0.3982(6) 0.9215(6) 0.5937(3) 0.0279(14) Uani 1 1 d . U . . . C72 C 0.4119(6) 1.0198(6) 0.5810(3) 0.0251(13) Uani 1 1 d . U . . . H72 H 0.4499 1.0864 0.6051 0.030 Uiso 1 1 calc R . . . . C73 C 0.3720(5) 1.0243(6) 0.5347(3) 0.0233(13) Uani 1 1 d . U . . . C74 C 0.2317(8) 0.7158(6) 0.4761(3) 0.0398(19) Uani 1 1 d . U . . . H74A H 0.1676 0.7224 0.4579 0.059(18) Uiso 1 1 calc GR . . . . H74B H 0.2049 0.6593 0.4947 0.059(18) Uiso 1 1 calc GR . . . . H74C H 0.2796 0.6956 0.4527 0.059(18) Uiso 1 1 calc GR . . . . C75 C 0.4431(8) 0.9223(8) 0.6455(3) 0.046(2) Uani 1 1 d . U . . . H75A H 0.5160 0.9140 0.6451 0.12(3) Uiso 1 1 calc GR . . . . H75B H 0.3909 0.8617 0.6566 0.12(3) Uiso 1 1 calc GR . . . . H75C H 0.4512 0.9919 0.6683 0.12(3) Uiso 1 1 calc GR . . . . C76 C 0.3955(7) 1.1342(6) 0.5225(3) 0.0326(16) Uani 1 1 d . U . . . H76A H 0.4313 1.1353 0.4923 0.054(17) Uiso 1 1 calc GR . . . . H76B H 0.4454 1.1920 0.5500 0.054(17) Uiso 1 1 calc GR . . . . H76C H 0.3252 1.1467 0.5173 0.054(17) Uiso 1 1 calc GR . . . . C77 C -0.3846(7) 0.4158(7) 0.0868(3) 0.0414(18) Uani 1 1 d . U . . . C78 C -0.4148(9) 0.3290(9) 0.0458(4) 0.056(2) Uani 1 1 d . U . . . C79 C -0.5128(9) 0.3087(10) 0.0141(4) 0.066(3) Uani 1 1 d . U . . . H79 H -0.5341 0.2490 -0.0142 0.079 Uiso 1 1 calc R . . . . C80 C -0.5778(8) 0.3697(9) 0.0219(4) 0.053(2) Uani 1 1 d . U . . . C81 C -0.5462(8) 0.4555(9) 0.0632(4) 0.056(2) Uani 1 1 d . U . . . H81 H -0.5912 0.4992 0.0693 0.068 Uiso 1 1 calc R . . . . C82 C -0.4492(7) 0.4808(8) 0.0967(4) 0.050(2) Uani 1 1 d . U . . . C83 C -0.3452(13) 0.2584(13) 0.0350(5) 0.105(6) Uani 1 1 d . U . . . H83A H -0.2670 0.3049 0.0363 0.12(3) Uiso 1 1 calc GR . . . . H83B H -0.3723 0.2095 0.0019 0.12(3) Uiso 1 1 calc GR . . . . H83C H -0.3510 0.2148 0.0597 0.12(3) Uiso 1 1 calc GR . . . . C84 C -0.6814(9) 0.3456(11) -0.0142(4) 0.076(4) Uani 1 1 d . U . . . H84A H -0.7484 0.3130 0.0007 0.10(3) Uiso 1 1 calc GR . . . . H84B H -0.6806 0.2945 -0.0448 0.10(3) Uiso 1 1 calc GR . . . . H84C H -0.6822 0.4138 -0.0217 0.10(3) Uiso 1 1 calc GR . . . . C85 C -0.4220(9) 0.5739(10) 0.1423(5) 0.075(4) Uani 1 1 d . U . . . H85A H -0.4195 0.5458 0.1721 0.17(4) Uiso 1 1 calc GR . . . . H85B H -0.4797 0.6068 0.1426 0.17(4) Uiso 1 1 calc GR . . . . H85C H -0.3492 0.6293 0.1418 0.17(4) Uiso 1 1 calc GR . . . . C86 C 0.5438(5) 0.6433(5) 0.3433(3) 0.0221(12) Uani 1 1 d . U . . . C87 C 0.5560(6) 0.5888(6) 0.3798(3) 0.0253(13) Uani 1 1 d . U . . . C88 C 0.6608(6) 0.6204(6) 0.4074(3) 0.0284(14) Uani 1 1 d . U . . . H88 H 0.6699 0.5822 0.4316 0.034 Uiso 1 1 calc R . . . . C89 C 0.7525(6) 0.7063(6) 0.4005(3) 0.0303(15) Uani 1 1 d . U . . . C90 C 0.7374(6) 0.7604(6) 0.3647(3) 0.0297(15) Uani 1 1 d . U . . . H90 H 0.7989 0.8193 0.3595 0.036 Uiso 1 1 calc R . . . . C91 C 0.6339(6) 0.7300(6) 0.3359(3) 0.0245(13) Uani 1 1 d . U . . . C92 C 0.4598(6) 0.4970(6) 0.3901(3) 0.0348(17) Uani 1 1 d . U . . . H92A H 0.4142 0.5276 0.4113 0.065(19) Uiso 1 1 calc GR . . . . H92B H 0.4889 0.4523 0.4069 0.065(19) Uiso 1 1 calc GR . . . . H92C H 0.4139 0.4514 0.3588 0.065(19) Uiso 1 1 calc GR . . . . C93 C 0.8644(7) 0.7409(8) 0.4315(3) 0.041(2) Uani 1 1 d . U . . . H93A H 0.9215 0.7388 0.4098 0.08(2) Uiso 1 1 calc GR . . . . H93B H 0.8608 0.6910 0.4532 0.08(2) Uiso 1 1 calc GR . . . . H93C H 0.8836 0.8156 0.4518 0.08(2) Uiso 1 1 calc GR . . . . C94 C 0.6249(7) 0.7906(7) 0.2962(3) 0.0357(17) Uani 1 1 d . U . . . H94A H 0.6143 0.7417 0.2634 0.07(2) Uiso 1 1 calc GR . . . . H94B H 0.6936 0.8545 0.3000 0.07(2) Uiso 1 1 calc GR . . . . H94C H 0.5610 0.8148 0.2996 0.07(2) Uiso 1 1 calc GR . . . . Cl1 Cl 0.1478(3) 1.4137(2) 0.41300(13) 0.0707(8) Uani 1 1 d . U . . . Cl2 Cl 0.2690(2) 1.2802(2) 0.44154(10) 0.0552(6) Uani 1 1 d . U . . . Cl6 Cl -0.6249(7) 0.7413(7) 0.1097(3) 0.090(2) Uani 0.5 1 d D U P A 1 Cl7 Cl -0.8529(9) 0.6799(12) 0.0651(4) 0.152(5) Uani 0.5 1 d D U P A 1 Cl3 Cl -0.5482(9) 0.7447(9) 0.1846(4) 0.093(3) Uani 0.4 1 d D U P B 2 Cl4 Cl -0.6232(14) 0.7935(14) 0.0994(6) 0.095(5) Uiso 0.27 1 d D U P B 2 Cl5 Cl -0.601(3) 0.724(3) 0.0771(11) 0.111(11) Uiso 0.13 1 d D U P B 2 Cl8 Cl -0.852(4) 0.535(4) 0.0304(17) 0.106(13) Uiso 0.1 1 d . U P C 3 Cl9 Cl -0.983(4) 0.635(4) 0.0192(18) 0.117(14) Uiso 0.1 1 d . U P D 3 C95 C 0.1759(7) 1.2929(6) 0.3963(3) 0.0375(17) Uani 1 1 d . U . . . H95A H 0.2082 1.2909 0.3647 0.045 Uiso 1 1 calc R . . . . H95B H 0.1049 1.2296 0.3906 0.045 Uiso 1 1 calc R . . . . C97 C -0.7506(13) 0.6320(19) 0.0863(10) 0.079(7) Uiso 0.5 1 d D U P A 1 H97A H -0.7384 0.5787 0.0588 0.095 Uiso 0.5 1 d R . P A 1 H97B H -0.7773 0.5957 0.1132 0.095 Uiso 0.5 1 d R . P A 1 C96 C -0.647(3) 0.687(2) 0.1307(8) 0.093(11) Uiso 0.4 1 d D U P B 2 H96A H -0.6345 0.6229 0.1102 0.111 Uiso 0.4 1 d R . P B 2 H96B H -0.7235 0.6641 0.1395 0.111 Uiso 0.4 1 d R . P B 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 0.01401(11) 0.01461(11) 0.01952(12) 0.00617(9) 0.00262(9) 0.00482(9) Ir2 0.01831(12) 0.01712(12) 0.02215(13) 0.00492(10) -0.00016(10) 0.00588(10) F1 0.029(2) 0.051(3) 0.047(3) 0.028(2) 0.0051(19) 0.014(2) F2 0.054(3) 0.060(4) 0.074(4) 0.048(3) 0.021(3) 0.023(3) F3 0.061(3) 0.036(3) 0.069(4) 0.025(3) 0.032(3) 0.001(2) F4 0.044(3) 0.069(4) 0.043(3) 0.014(3) 0.006(2) -0.009(3) F5 0.027(2) 0.058(3) 0.035(2) 0.018(2) -0.0071(19) -0.007(2) F6 0.025(2) 0.033(2) 0.037(2) 0.0126(19) -0.0035(17) 0.0093(18) F7 0.0152(19) 0.031(2) 0.073(3) 0.014(2) -0.004(2) -0.0032(17) F8 0.035(3) 0.042(3) 0.097(4) 0.044(3) 0.018(3) 0.001(2) F9 0.047(3) 0.054(3) 0.064(3) 0.046(3) 0.011(2) 0.015(3) F10 0.023(2) 0.037(2) 0.037(2) 0.0181(19) -0.0018(17) 0.0103(18) O1 0.020(2) 0.0159(19) 0.031(2) 0.0097(17) 0.0101(18) 0.0063(17) O2 0.024(2) 0.022(2) 0.025(2) 0.0042(18) 0.0068(19) 0.0071(18) N1 0.016(2) 0.015(2) 0.022(2) 0.0073(18) 0.0037(19) 0.0058(18) N2 0.016(2) 0.017(2) 0.021(2) 0.0081(19) 0.0015(18) 0.0051(18) N3 0.016(2) 0.019(2) 0.022(2) 0.0053(19) 0.0011(18) 0.0035(18) N4 0.018(2) 0.016(2) 0.022(2) 0.0068(19) 0.0057(18) 0.0074(19) N5 0.023(2) 0.022(3) 0.025(3) 0.008(2) -0.002(2) 0.004(2) N6 0.018(2) 0.015(2) 0.024(2) 0.0048(19) 0.0016(18) 0.0039(19) C1 0.020(3) 0.021(3) 0.019(3) 0.003(2) 0.001(2) 0.006(2) C2 0.013(2) 0.018(2) 0.021(3) 0.010(2) 0.001(2) 0.003(2) C3 0.016(2) 0.017(3) 0.022(3) 0.005(2) 0.006(2) 0.010(2) C4 0.016(3) 0.021(3) 0.025(3) 0.006(2) 0.001(2) 0.005(2) C5 0.020(3) 0.018(3) 0.030(3) 0.004(2) 0.001(2) 0.003(2) C6 0.022(3) 0.019(3) 0.033(3) 0.009(3) 0.004(2) 0.001(2) C7 0.021(3) 0.020(3) 0.027(3) 0.010(2) 0.004(2) 0.006(2) C8 0.016(2) 0.016(2) 0.022(3) 0.006(2) 0.001(2) 0.005(2) C9 0.018(3) 0.018(3) 0.021(3) 0.006(2) 0.003(2) 0.005(2) C10 0.022(3) 0.025(3) 0.023(3) 0.009(2) 0.000(2) 0.004(2) C11 0.022(3) 0.031(3) 0.025(3) 0.008(2) -0.003(2) 0.006(3) C12 0.023(3) 0.030(3) 0.029(3) 0.008(3) -0.007(3) 0.000(3) C13 0.022(3) 0.021(3) 0.028(3) 0.013(2) -0.001(2) -0.002(2) C14 0.015(2) 0.011(2) 0.023(3) 0.007(2) 0.005(2) 0.004(2) C15 0.019(3) 0.025(3) 0.028(3) 0.013(3) 0.005(2) 0.010(2) C16 0.022(3) 0.034(4) 0.034(3) 0.016(3) 0.010(3) 0.017(3) C17 0.028(3) 0.031(4) 0.030(3) 0.013(3) 0.012(3) 0.017(3) C18 0.023(3) 0.026(3) 0.025(3) 0.010(2) 0.008(2) 0.013(3) C19 0.017(3) 0.017(3) 0.023(3) 0.010(2) 0.006(2) 0.007(2) C20 0.018(3) 0.018(3) 0.022(3) 0.008(2) 0.006(2) 0.007(2) C21 0.018(3) 0.022(3) 0.022(3) 0.008(2) 0.006(2) 0.009(2) C22 0.016(3) 0.020(3) 0.025(3) 0.008(2) 0.003(2) 0.006(2) C23 0.021(3) 0.026(3) 0.027(3) 0.009(2) 0.005(2) 0.013(3) C24 0.020(3) 0.021(3) 0.022(3) 0.006(2) 0.004(2) 0.011(2) C25 0.022(3) 0.020(3) 0.024(3) 0.005(2) 0.001(2) 0.007(2) C26 0.023(3) 0.024(3) 0.031(3) 0.007(3) -0.002(3) 0.009(3) C27 0.034(3) 0.023(3) 0.037(4) 0.011(3) -0.004(3) 0.010(3) C28 0.035(4) 0.020(3) 0.047(4) 0.015(3) -0.003(3) 0.002(3) C29 0.026(3) 0.022(3) 0.044(4) 0.012(3) -0.004(3) 0.001(3) C30 0.026(3) 0.020(3) 0.030(3) 0.009(2) -0.004(2) 0.007(2) C31 0.024(3) 0.022(3) 0.030(3) 0.010(3) -0.003(2) 0.003(2) C32 0.024(3) 0.032(4) 0.032(4) 0.012(3) -0.006(3) 0.003(3) C33 0.031(3) 0.038(4) 0.033(4) 0.013(3) -0.006(3) 0.005(3) C34 0.032(3) 0.046(4) 0.043(4) 0.026(4) -0.008(3) 0.006(3) C35 0.025(3) 0.037(4) 0.037(4) 0.020(3) -0.002(3) 0.003(3) C36 0.028(3) 0.023(3) 0.021(3) 0.005(2) 0.000(2) 0.010(2) C37 0.038(4) 0.030(4) 0.030(3) 0.002(3) -0.001(3) 0.010(3) C38 0.046(4) 0.034(4) 0.031(4) -0.001(3) 0.003(3) 0.012(3) C39 0.045(4) 0.030(4) 0.030(3) 0.007(3) 0.013(3) 0.015(3) C40 0.032(3) 0.027(3) 0.031(3) 0.009(3) 0.010(3) 0.013(3) C41 0.026(3) 0.024(3) 0.023(3) 0.007(2) 0.004(2) 0.009(2) C42 0.020(3) 0.017(3) 0.025(3) 0.008(2) 0.007(2) 0.003(2) C43 0.021(3) 0.013(3) 0.029(3) 0.008(2) 0.008(2) 0.006(2) C44 0.018(3) 0.015(3) 0.030(3) 0.006(2) 0.004(2) 0.005(2) C45 0.021(3) 0.022(3) 0.026(3) 0.003(2) 0.001(2) 0.009(2) C46 0.019(3) 0.026(3) 0.024(3) 0.001(2) 0.001(2) 0.011(2) C47 0.020(3) 0.021(3) 0.026(3) 0.004(2) 0.008(2) 0.007(2) C48 0.029(3) 0.035(3) 0.034(3) 0.014(3) 0.012(3) 0.016(3) C49 0.042(3) 0.037(4) 0.044(4) 0.020(3) 0.020(3) 0.018(3) C50 0.039(3) 0.029(3) 0.040(4) 0.009(3) 0.024(3) 0.009(3) C51 0.035(3) 0.032(3) 0.031(3) 0.002(3) 0.013(3) 0.000(3) C52 0.027(3) 0.032(3) 0.024(3) 0.005(3) 0.007(2) 0.002(2) C53 0.018(3) 0.016(3) 0.026(3) 0.006(2) 0.006(2) 0.005(2) C54 0.019(3) 0.019(3) 0.032(3) 0.009(2) 0.001(2) 0.006(2) C55 0.017(3) 0.016(3) 0.048(4) 0.010(3) 0.004(2) 0.001(2) C56 0.029(3) 0.025(3) 0.054(4) 0.019(3) 0.012(3) 0.006(3) C57 0.032(3) 0.031(3) 0.044(4) 0.024(3) 0.011(3) 0.013(3) C58 0.023(3) 0.020(3) 0.027(3) 0.009(2) 0.004(2) 0.009(2) C59 0.023(3) 0.042(4) 0.029(3) 0.012(3) -0.006(2) 0.004(3) C60 0.030(4) 0.075(6) 0.033(3) 0.024(4) 0.004(3) 0.017(4) C61 0.041(4) 0.089(8) 0.034(4) 0.029(4) 0.007(3) 0.026(5) C62 0.044(4) 0.076(7) 0.033(4) 0.016(4) -0.002(3) 0.026(4) C63 0.037(4) 0.074(7) 0.033(3) 0.009(4) -0.004(3) 0.026(4) C64 0.030(3) 0.043(5) 0.031(3) 0.002(3) -0.005(3) 0.011(3) C65 0.046(5) 0.152(12) 0.045(6) 0.044(7) 0.015(4) 0.048(7) C66 0.071(7) 0.137(12) 0.036(5) 0.023(6) 0.000(4) 0.063(8) C67 0.050(5) 0.076(7) 0.033(4) 0.005(4) 0.000(3) 0.034(5) C68 0.017(3) 0.022(3) 0.023(3) 0.008(2) 0.004(2) 0.007(2) C69 0.024(3) 0.026(3) 0.029(3) 0.010(2) 0.004(2) 0.009(2) C70 0.028(3) 0.029(3) 0.032(3) 0.014(2) 0.002(3) 0.013(3) C71 0.023(3) 0.034(3) 0.029(3) 0.014(2) 0.002(2) 0.010(3) C72 0.020(3) 0.027(3) 0.027(3) 0.006(2) 0.000(2) 0.007(3) C73 0.018(3) 0.026(3) 0.028(3) 0.009(2) 0.004(2) 0.008(2) C74 0.056(5) 0.023(3) 0.036(4) 0.010(3) 0.001(4) 0.007(3) C75 0.041(5) 0.058(6) 0.037(4) 0.021(4) -0.009(3) 0.011(4) C76 0.035(4) 0.025(3) 0.036(4) 0.009(3) 0.001(3) 0.007(3) C77 0.032(3) 0.044(4) 0.042(4) 0.022(3) -0.011(3) 0.002(3) C78 0.053(5) 0.057(5) 0.046(4) 0.011(4) -0.021(4) 0.011(4) C79 0.057(5) 0.076(6) 0.050(5) 0.011(5) -0.027(4) 0.011(5) C80 0.034(4) 0.061(5) 0.054(5) 0.034(4) -0.014(3) -0.005(3) C81 0.032(4) 0.060(5) 0.068(5) 0.027(4) -0.016(4) 0.002(4) C82 0.028(4) 0.052(5) 0.061(5) 0.023(4) -0.010(3) 0.001(3) C83 0.105(10) 0.117(11) 0.080(9) -0.033(8) -0.049(8) 0.066(9) C84 0.046(5) 0.105(9) 0.067(7) 0.048(6) -0.023(5) 0.001(5) C85 0.041(6) 0.073(7) 0.091(7) -0.006(6) -0.021(5) 0.016(5) C86 0.016(2) 0.020(3) 0.027(3) 0.001(2) 0.003(2) 0.005(2) C87 0.020(3) 0.021(3) 0.031(3) 0.003(2) 0.001(2) 0.005(2) C88 0.021(3) 0.031(3) 0.031(3) 0.005(3) 0.001(2) 0.009(2) C89 0.021(3) 0.036(4) 0.028(3) -0.001(3) 0.001(2) 0.008(3) C90 0.016(3) 0.031(4) 0.034(3) 0.003(3) 0.005(2) 0.002(2) C91 0.018(3) 0.021(3) 0.033(3) 0.002(2) 0.004(2) 0.007(2) C92 0.024(3) 0.026(3) 0.049(5) 0.014(3) -0.002(3) 0.001(3) C93 0.026(3) 0.049(5) 0.039(4) -0.001(4) -0.004(3) 0.010(3) C94 0.031(4) 0.034(4) 0.042(4) 0.013(3) 0.005(3) 0.009(3) Cl1 0.0690(18) 0.0467(14) 0.094(2) -0.0030(14) 0.0003(16) 0.0312(14) Cl2 0.0453(13) 0.0534(14) 0.0632(15) 0.0281(12) -0.0034(11) 0.0062(11) Cl6 0.117(6) 0.097(6) 0.094(5) 0.035(5) 0.054(5) 0.071(5) Cl7 0.137(8) 0.279(15) 0.126(8) 0.114(9) 0.074(7) 0.136(10) Cl3 0.098(7) 0.112(8) 0.086(6) 0.033(6) 0.016(5) 0.050(6) C95 0.037(4) 0.028(4) 0.045(4) 0.010(3) 0.007(3) 0.006(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' 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' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1.00 0.00 0.00 0.1190 -1.00 0.00 0.00 0.0940 0.00 1.00 0.00 0.0320 0.00 -1.00 0.00 0.0500 0.00 0.00 -1.00 0.0260 0.00 0.00 1.00 0.0290 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O1 Ir1 N1 74.71(18) N3 Ir1 O1 96.4(2) N3 Ir1 N1 91.9(2) N4 Ir1 O1 87.33(19) N4 Ir1 N1 93.5(2) N4 Ir1 N3 174.1(2) C3 Ir1 O1 175.8(2) C3 Ir1 N1 107.8(2) C3 Ir1 N3 80.2(2) C3 Ir1 N4 95.8(2) C3 Ir1 C14 89.0(2) C14 Ir1 O1 88.7(2) C14 Ir1 N1 162.8(2) C14 Ir1 N3 94.6(2) C14 Ir1 N4 80.9(2) N2 Ir2 O2 75.09(19) N5 Ir2 O2 96.7(2) N5 Ir2 N2 87.2(2) N5 Ir2 N6 176.5(2) N6 Ir2 O2 85.9(2) N6 Ir2 N2 95.8(2) C25 Ir2 O2 176.7(2) C25 Ir2 N2 105.0(2) C25 Ir2 N5 80.1(2) C25 Ir2 N6 97.3(2) C25 Ir2 C36 86.1(3) C36 Ir2 O2 93.9(2) C36 Ir2 N2 168.6(3) C36 Ir2 N5 97.3(3) C36 Ir2 N6 80.1(2) C2 O1 Ir1 113.8(4) C1 O2 Ir2 112.2(4) N2 N1 Ir1 112.8(3) C1 N1 Ir1 134.9(4) C1 N1 N2 111.9(5) N1 N2 Ir2 113.4(3) C2 N2 Ir2 134.4(4) C2 N2 N1 111.4(5) C9 N3 Ir1 116.3(4) C9 N3 C13 119.7(6) C13 N3 Ir1 124.0(4) C20 N4 Ir1 116.1(4) C20 N4 C24 118.9(6) C24 N4 Ir1 125.0(4) C31 N5 Ir2 116.8(4) C35 N5 Ir2 123.0(5) C35 N5 C31 120.0(6) C42 N6 Ir2 115.6(4) C46 N6 Ir2 124.9(4) C46 N6 C42 119.4(6) O2 C1 N1 126.9(6) O2 C1 C47 116.1(6) N1 C1 C47 117.0(6) O1 C2 N2 126.3(6) O1 C2 C53 113.6(5) N2 C2 C53 120.1(6) C4 C3 Ir1 128.1(5) C4 C3 C8 117.0(6) C8 C3 Ir1 114.8(4) C5 C4 C3 121.0(6) C6 C5 C4 120.8(6) C7 C6 C5 120.2(6) C6 C7 C8 119.7(6) C3 C8 C9 114.1(5) C7 C8 C3 121.3(6) C7 C8 C9 124.5(6) N3 C9 C8 113.9(5) N3 C9 C10 120.2(6) C10 C9 C8 125.8(6) C11 C10 C9 120.5(6) C10 C11 C12 117.8(6) C10 C11 C59 122.6(7) C12 C11 C59 119.5(6) C13 C12 C11 120.4(6) N3 C13 C12 121.4(6) C15 C14 Ir1 129.3(5) C15 C14 C19 116.7(6) C19 C14 Ir1 113.4(4) C16 C15 C14 121.9(6) C17 C16 C15 120.5(6) C16 C17 C18 119.6(6) C17 C18 C19 120.0(6) C14 C19 C20 115.2(5) C18 C19 C14 121.3(6) C18 C19 C20 123.5(6) N4 C20 C19 113.6(5) N4 C20 C21 120.6(6) C21 C20 C19 125.8(6) C22 C21 C20 120.9(6) C21 C22 C23 117.3(6) C21 C22 C68 121.3(6) C23 C22 C68 121.4(6) C24 C23 C22 120.0(6) N4 C24 C23 122.1(6) C26 C25 Ir2 127.9(5) C26 C25 C30 116.6(6) C30 C25 Ir2 115.5(5) C27 C26 C25 121.1(7) C26 C27 C28 121.5(7) C29 C28 C27 118.8(7) C28 C29 C30 120.2(7) C25 C30 C31 114.3(6) C29 C30 C25 121.7(6) C29 C30 C31 123.9(6) N5 C31 C30 113.2(6) N5 C31 C32 120.2(6) C32 C31 C30 126.5(6) C33 C32 C31 120.6(7) C32 C33 C77 122.5(7) C34 C33 C32 117.5(7) C34 C33 C77 120.0(7) C35 C34 C33 120.7(7) N5 C35 C34 120.9(7) C37 C36 Ir2 128.9(6) C37 C36 C41 116.9(7) C41 C36 Ir2 114.2(5) C38 C37 C36 121.4(8) C39 C38 C37 120.9(8) C38 C39 C40 119.4(7) C39 C40 C41 120.5(7) C36 C41 C42 114.6(6) C40 C41 C36 120.9(7) C40 C41 C42 124.3(7) N6 C42 C41 113.8(6) N6 C42 C43 119.5(6) C43 C42 C41 126.5(6) C44 C43 C42 121.1(6) C43 C44 C45 117.7(6) C43 C44 C86 123.0(6) C45 C44 C86 119.3(6) C46 C45 C44 119.1(6) N6 C46 C45 123.0(6) C48 C47 C1 120.8(6) C48 C47 C52 117.6(7) C52 C47 C1 121.5(6) F1 C48 C47 120.3(7) F1 C48 C49 118.5(7) C47 C48 C49 121.1(7) F2 C49 C48 120.1(8) F2 C49 C50 119.8(7) C50 C49 C48 120.1(8) F3 C50 C49 120.8(8) F3 C50 C51 119.4(8) C49 C50 C51 119.8(7) F4 C51 C50 121.2(7) F4 C51 C52 119.5(8) C50 C51 C52 119.3(8) F5 C52 C47 118.7(6) F5 C52 C51 119.3(7) C47 C52 C51 122.0(7) C54 C53 C2 119.0(6) C54 C53 C58 117.9(6) C58 C53 C2 122.6(6) F6 C54 C53 120.1(6) F6 C54 C55 118.4(6) C53 C54 C55 121.5(6) F7 C55 C54 120.2(7) F7 C55 C56 120.5(6) C56 C55 C54 119.2(7) F8 C56 C55 119.1(7) F8 C56 C57 120.0(7) C57 C56 C55 120.9(7) F9 C57 C56 120.5(7) F9 C57 C58 120.3(7) C56 C57 C58 119.2(7) F10 C58 C53 119.7(6) F10 C58 C57 119.0(6) C53 C58 C57 121.3(6) C60 C59 C11 119.9(7) C64 C59 C11 120.1(7) C64 C59 C60 120.0(7) C59 C60 C65 121.4(8) C61 C60 C59 119.3(8) C61 C60 C65 119.2(8) C62 C61 C60 121.7(9) C61 C62 C63 118.6(8) C61 C62 C66 120.5(9) C63 C62 C66 120.8(9) C62 C63 C64 121.9(8) C59 C64 C63 118.5(8) C59 C64 C67 122.0(7) C63 C64 C67 119.4(8) C69 C68 C22 119.2(6) C73 C68 C22 120.0(6) C73 C68 C69 120.7(6) C68 C69 C74 122.4(6) C70 C69 C68 117.9(7) C70 C69 C74 119.6(6) C71 C70 C69 122.3(7) C70 C71 C72 118.4(7) C70 C71 C75 122.0(7) C72 C71 C75 119.6(7) C73 C72 C71 122.3(7) C68 C73 C76 122.2(6) C72 C73 C68 118.3(6) C72 C73 C76 119.4(7) C78 C77 C33 119.2(9) C78 C77 C82 121.1(8) C82 C77 C33 119.5(8) C77 C78 C79 117.8(10) C77 C78 C83 121.3(9) C79 C78 C83 120.9(10) C80 C79 C78 123.3(11) C79 C80 C81 117.6(9) C79 C80 C84 121.1(11) C81 C80 C84 121.3(11) C80 C81 C82 122.3(11) C77 C82 C81 117.8(10) C77 C82 C85 122.9(8) C81 C82 C85 119.3(10) C87 C86 C44 119.7(6) C91 C86 C44 119.6(6) C91 C86 C87 120.4(6) C86 C87 C92 122.2(6) C88 C87 C86 118.7(6) C88 C87 C92 119.1(7) C89 C88 C87 122.0(7) C88 C89 C93 121.3(7) C90 C89 C88 118.0(7) C90 C89 C93 120.8(7) C89 C90 C91 121.5(7) C86 C91 C90 119.3(7) C86 C91 C94 122.2(6) C90 C91 C94 118.4(6) Cl1 C95 Cl2 112.9(5) Cl6 C97 Cl7 110.4(14) Cl3 C96 Cl4 104.5(16) Cl5 C96 Cl3 116(2) Cl5 C96 Cl4 37.9(14) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ir1 O1 2.126(4) Ir1 N1 2.181(5) Ir1 N3 2.034(5) Ir1 N4 2.034(5) Ir1 C3 1.995(6) Ir1 C14 1.999(6) Ir2 O2 2.158(5) Ir2 N2 2.156(5) Ir2 N5 2.032(6) Ir2 N6 2.040(5) Ir2 C25 1.989(7) Ir2 C36 2.000(7) F1 C48 1.332(9) F2 C49 1.334(10) F3 C50 1.329(9) F4 C51 1.335(10) F5 C52 1.341(9) F6 C54 1.342(8) F7 C55 1.344(8) F8 C56 1.339(8) F9 C57 1.327(8) F10 C58 1.337(8) O1 C2 1.278(8) O2 C1 1.280(8) N1 N2 1.448(6) N1 C1 1.302(8) N2 C2 1.308(8) N3 C9 1.360(8) N3 C13 1.364(8) N4 C20 1.351(8) N4 C24 1.353(8) N5 C31 1.360(9) N5 C35 1.353(9) N6 C42 1.362(8) N6 C46 1.335(8) C1 C47 1.495(9) C2 C53 1.499(8) C3 C4 1.401(9) C3 C8 1.425(8) C4 C5 1.392(9) C5 C6 1.385(10) C6 C7 1.377(9) C7 C8 1.399(9) C8 C9 1.461(9) C9 C10 1.397(9) C10 C11 1.387(9) C11 C12 1.398(10) C11 C59 1.500(10) C12 C13 1.368(9) C14 C15 1.389(8) C14 C19 1.422(9) C15 C16 1.384(10) C16 C17 1.381(10) C17 C18 1.385(9) C18 C19 1.387(9) C19 C20 1.469(8) C20 C21 1.387(9) C21 C22 1.386(9) C22 C23 1.388(9) C22 C68 1.486(9) C23 C24 1.374(9) C25 C26 1.400(9) C25 C30 1.414(9) C26 C27 1.369(10) C27 C28 1.398(11) C28 C29 1.368(10) C29 C30 1.390(10) C30 C31 1.469(9) C31 C32 1.397(9) C32 C33 1.393(10) C33 C34 1.390(11) C33 C77 1.492(11) C34 C35 1.385(10) C36 C37 1.400(10) C36 C41 1.425(10) C37 C38 1.385(11) C38 C39 1.383(12) C39 C40 1.383(11) C40 C41 1.391(10) C41 C42 1.457(9) C42 C43 1.400(9) C43 C44 1.386(9) C44 C45 1.392(9) C44 C86 1.496(9) C45 C46 1.384(9) C47 C48 1.380(10) C47 C52 1.382(10) C48 C49 1.397(11) C49 C50 1.373(12) C50 C51 1.379(12) C51 C52 1.392(10) C53 C54 1.375(9) C53 C58 1.381(9) C54 C55 1.382(9) C55 C56 1.370(11) C56 C57 1.365(11) C57 C58 1.385(10) C59 C60 1.393(11) C59 C64 1.390(11) C60 C61 1.389(11) C60 C65 1.506(13) C61 C62 1.367(13) C62 C63 1.373(13) C62 C66 1.528(12) C63 C64 1.399(11) C64 C67 1.499(12) C68 C69 1.412(9) C68 C73 1.404(9) C69 C70 1.391(10) C69 C74 1.511(10) C70 C71 1.378(11) C71 C72 1.387(10) C71 C75 1.520(10) C72 C73 1.383(9) C73 C76 1.510(10) C77 C78 1.378(14) C77 C82 1.389(14) C78 C79 1.408(13) C78 C83 1.503(17) C79 C80 1.347(16) C80 C81 1.375(15) C80 C84 1.520(12) C81 C82 1.410(12) C82 C85 1.514(15) C86 C87 1.397(10) C86 C91 1.392(9) C87 C88 1.395(9) C87 C92 1.507(10) C88 C89 1.392(10) C89 C90 1.388(11) C89 C93 1.507(10) C90 C91 1.398(10) C91 C94 1.521(10) Cl1 C95 1.749(8) Cl2 C95 1.761(9) Cl6 C97 1.749(17) Cl7 C97 1.767(17) Cl3 C96 1.760(19) Cl4 C96 1.770(19) Cl5 C96 1.74(2)