#------------------------------------------------------------------------------ #$Date: 2018-01-23 05:16:25 +0200 (Tue, 23 Jan 2018) $ #$Revision: 205481 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/53/7045341.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_7045341 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 'C60 H38 F8 Ir2 N6 O4' _chemical_formula_sum 'C60 H38 F8 Ir2 N6 O4' _chemical_formula_weight 1443.36 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_date 2017-09-22 _audit_creation_method ; Olex2 1.2-beta (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _audit_update_record ; 2017-09-22 deposited with the CCDC. 2017-12-14 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 101.1365(14) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.7982(5) _cell_length_b 23.4916(10) _cell_length_c 19.1919(8) _cell_measurement_reflns_used 9964 _cell_measurement_temperature 120 _cell_measurement_theta_max 31.24 _cell_measurement_theta_min 2.33 _cell_volume 5219.0(4) _computing_cell_refinement 'SAINT v8.38A (Bruker, 2017)' _computing_data_collection 'APEX3 v.2016.1-0 (Bruker, 2016)' _computing_data_reduction 'SAINT v8.38A (Bruker, 2017)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL 2016/6 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 0.0660 _diffrn_reflns_av_unetI/netI 0.0481 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 108935 _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 29.999 _diffrn_reflns_theta_min 2.163 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\mS microsource' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 5.179 _exptl_absorpt_correction_T_max 0.6963 _exptl_absorpt_correction_T_min 0.6318 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details 'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1033 before and 0.0617 after correction. The Ratio of minimum to maximum transmission is 0.9074. The \l/2 correction factor is Not present.' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.837 _exptl_crystal_description prism _exptl_crystal_F_000 2792 _exptl_crystal_preparation Luminescent _exptl_crystal_size_max 0.117 _exptl_crystal_size_mid 0.112 _exptl_crystal_size_min 0.093 _refine_diff_density_max 1.452 _refine_diff_density_min -1.041 _refine_diff_density_rms 0.152 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 735 _refine_ls_number_reflns 15211 _refine_ls_number_restraints 18 _refine_ls_restrained_S_all 1.044 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_gt 0.0360 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0230P)^2^+8.4630P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.0661 _reflns_Friedel_coverage 0.000 _reflns_number_gt 11519 _reflns_number_total 15211 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt04201a2.cif _cod_data_source_block beta-10_17srv057 _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 7045341 _shelx_shelxl_version_number 2016/6 _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 0.644 _shelx_estimated_absorpt_t_min 0.582 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(O4A) = Uanis(O4B) 3. Rigid body (RIGU) restrains C57, O4B, C60B with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C57, O4A, C60A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4. Others Sof(O4B)=Sof(C60B)=Sof(H60D)=Sof(H60E)=Sof(H60F)=1-FVAR(1) Sof(O4A)=Sof(C60A)=Sof(H60A)=Sof(H60B)=Sof(H60C)=FVAR(1) 5.a Riding coordinates: C60A(H60A,H60B,H60C), C60B(H60D,H60E,H60F) 5.b Aromatic/amide H refined with riding coordinates: C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C32(H32), C33(H33), C34(H34), C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C43(H43), C44(H44), C45(H45), C46(H46) 5.c Idealised Me refined as rotating group: C53(H53A,H53B,H53C) ; _shelx_res_file ; TITL 17asb004 in P2(1)/n 17srv057.res created by SHELXL-2016/6 at 14:05:32 on 22-Sep-2017 CELL 0.71073 11.7982 23.4916 19.1919 90 101.1365 90 ZERR 4 0.0005 0.001 0.0008 0 0.0014 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H F Ir N O UNIT 240 152 32 8 24 16 RIGU C57 O4B C60B RIGU C57 O4A C60A EADP O4A O4B L.S. 7 PLAN 10 SIZE 0.093 0.112 0.117 TEMP -153.15 BOND fmap 2 53 acta OMIT -3 60 OMIT 1 0 1 OMIT 1 1 0 OMIT 0 2 1 REM REM REM WGHT 0.023000 8.463000 FVAR 0.04273 0.51976 IR1 4 0.328223 0.146840 0.633564 11.00000 0.01304 0.01273 = 0.01983 0.00259 0.00146 -0.00104 IR2 4 0.329559 0.360909 0.603430 11.00000 0.01382 0.01255 = 0.01870 0.00136 0.00367 -0.00130 F1 3 0.611637 0.301070 0.735661 11.00000 0.02876 0.03744 = 0.02139 -0.00160 0.00462 -0.00772 F2 3 0.805342 0.354384 0.729118 11.00000 0.03057 0.05140 = 0.03465 -0.00281 -0.00613 -0.02231 F3 3 0.755096 0.308145 0.484583 11.00000 0.02942 0.04740 = 0.03435 0.00598 0.01825 -0.00489 F4 3 0.559597 0.253559 0.493462 11.00000 0.02607 0.03410 = 0.02340 -0.00483 0.00478 -0.00637 F5 3 0.097424 0.240133 0.728069 11.00000 0.02948 0.08070 = 0.01638 -0.00093 0.00120 -0.00129 F6 3 -0.109487 0.196265 0.729559 11.00000 0.03337 0.09040 = 0.03582 0.02451 0.01825 0.00173 F7 3 -0.174005 0.174888 0.481522 11.00000 0.02765 0.06438 = 0.04018 -0.01662 -0.00319 -0.01383 F8 3 0.030560 0.223163 0.479904 11.00000 0.02572 0.04607 = 0.01744 0.00029 0.00486 0.00140 O1 6 0.480150 0.189660 0.615665 11.00000 0.01506 0.01460 = 0.02994 0.00351 0.00407 -0.00050 O2 6 0.170384 0.313729 0.580003 11.00000 0.01464 0.01573 = 0.02735 0.00509 0.00139 -0.00147 O3 6 0.883967 0.358426 0.592897 11.00000 0.01849 0.05198 = 0.05260 0.01348 0.00592 -0.01500 N1 5 0.280231 0.235752 0.623934 11.00000 0.01152 0.01654 = 0.01808 0.00221 0.00292 -0.00383 N2 5 0.377741 0.272610 0.622426 11.00000 0.01228 0.01276 = 0.02155 0.00195 0.00484 -0.00461 N3 5 0.399542 0.152298 0.738302 11.00000 0.01848 0.01618 = 0.02631 0.00474 0.00151 -0.00464 N4 5 0.256751 0.134828 0.529551 11.00000 0.02058 0.01454 = 0.02004 0.00084 0.00512 0.00105 N5 5 0.299003 0.378131 0.701896 11.00000 0.01483 0.01768 = 0.02160 0.00254 0.00292 -0.00333 N6 5 0.371006 0.355283 0.505554 11.00000 0.01538 0.01800 = 0.01784 0.00036 -0.00049 0.00262 C1 1 0.470919 0.243894 0.618318 11.00000 0.01442 0.01813 = 0.01577 0.00197 0.00211 -0.00467 C2 1 0.182834 0.262653 0.601896 11.00000 0.01595 0.01660 = 0.01321 0.00084 0.00088 -0.00290 C3 1 0.415847 0.073370 0.645207 11.00000 0.01562 0.01657 = 0.03257 0.00535 0.00493 -0.00076 C4 1 0.417853 0.030179 0.594948 11.00000 0.02575 0.01969 = 0.03522 0.00578 0.00591 0.00143 AFIX 43 H4 2 0.366428 0.032079 0.550336 11.00000 -1.20000 AFIX 0 C5 1 0.494419 -0.015587 0.609590 11.00000 0.03636 0.02035 = 0.04646 0.00360 0.01120 0.00520 AFIX 43 H5 2 0.494567 -0.044590 0.575113 11.00000 -1.20000 AFIX 0 C6 1 0.570109 -0.018681 0.674365 11.00000 0.03474 0.02869 = 0.06103 0.00961 0.00986 0.01563 AFIX 43 H6 2 0.622545 -0.049664 0.684013 11.00000 -1.20000 AFIX 0 C7 1 0.569686 0.022850 0.724710 11.00000 0.02515 0.03788 = 0.04772 0.01077 -0.00434 0.00672 AFIX 43 H7 2 0.621593 0.020450 0.769101 11.00000 -1.20000 AFIX 0 C8 1 0.492765 0.068766 0.710670 11.00000 0.01274 0.02209 = 0.03613 0.00787 0.00156 -0.00246 C9 1 0.483798 0.113472 0.762151 11.00000 0.01794 0.02004 = 0.03113 0.00619 0.00079 -0.00759 C10 1 0.544890 0.117379 0.831847 11.00000 0.02239 0.03117 = 0.03949 0.01323 -0.01351 -0.00487 AFIX 43 H10 2 0.605813 0.091360 0.848331 11.00000 -1.20000 AFIX 0 C11 1 0.517945 0.158394 0.876854 11.00000 0.03897 0.03471 = 0.02617 0.00376 -0.00840 -0.01449 AFIX 43 H11 2 0.560403 0.161065 0.924129 11.00000 -1.20000 AFIX 0 C12 1 0.428339 0.195874 0.852800 11.00000 0.03733 0.02623 = 0.02676 -0.00230 -0.00078 -0.00942 AFIX 43 H12 2 0.406062 0.223672 0.883501 11.00000 -1.20000 AFIX 0 C13 1 0.372638 0.191641 0.783203 11.00000 0.02033 0.02387 = 0.02609 0.00383 0.00130 -0.00666 AFIX 43 H13 2 0.312246 0.217774 0.766027 11.00000 -1.20000 AFIX 0 C14 1 0.186123 0.104569 0.644446 11.00000 0.01369 0.01221 = 0.03063 0.00174 0.00259 0.00244 C15 1 0.149528 0.089230 0.707294 11.00000 0.01820 0.02065 = 0.03073 0.00255 0.00466 -0.00017 AFIX 43 H15 2 0.193505 0.101217 0.751649 11.00000 -1.20000 AFIX 0 C16 1 0.050874 0.057051 0.706134 11.00000 0.02582 0.02037 = 0.04288 0.00549 0.01352 -0.00025 AFIX 43 H16 2 0.029170 0.046669 0.749572 11.00000 -1.20000 AFIX 0 C17 1 -0.016307 0.039881 0.642579 11.00000 0.01960 0.01761 = 0.05379 0.00127 0.01274 -0.00431 AFIX 43 H17 2 -0.083948 0.017897 0.642396 11.00000 -1.20000 AFIX 0 C18 1 0.014784 0.054627 0.579592 11.00000 0.01947 0.01679 = 0.04167 -0.00178 -0.00175 0.00004 AFIX 43 H18 2 -0.031854 0.043373 0.535725 11.00000 -1.20000 AFIX 0 C19 1 0.116666 0.086681 0.580345 11.00000 0.01934 0.01288 = 0.02876 0.00067 0.00056 0.00127 C20 1 0.155689 0.104847 0.516266 11.00000 0.02152 0.01482 = 0.02753 -0.00135 -0.00116 0.00096 C21 1 0.101674 0.094965 0.446372 11.00000 0.03942 0.02362 = 0.03066 -0.00557 -0.00521 -0.00277 AFIX 43 H21 2 0.032260 0.073426 0.436654 11.00000 -1.20000 AFIX 0 C22 1 0.147748 0.116056 0.391263 11.00000 0.05592 0.03225 = 0.02446 -0.00340 -0.00657 -0.00150 AFIX 43 H22 2 0.109921 0.109578 0.343565 11.00000 -1.20000 AFIX 0 C23 1 0.249567 0.146801 0.405519 11.00000 0.04955 0.03236 = 0.01956 0.00202 0.00850 -0.00006 AFIX 43 H23 2 0.282877 0.161634 0.368038 11.00000 -1.20000 AFIX 0 C24 1 0.301370 0.155366 0.475236 11.00000 0.03404 0.02129 = 0.02612 0.00196 0.00589 -0.00003 AFIX 43 H24 2 0.371200 0.176554 0.485428 11.00000 -1.20000 AFIX 0 C25 1 0.246700 0.435175 0.584073 11.00000 0.01169 0.01557 = 0.02987 0.00190 0.00623 -0.00512 C26 1 0.210792 0.461125 0.518457 11.00000 0.01539 0.02219 = 0.03251 0.00385 0.00725 -0.00194 AFIX 43 H26 2 0.227824 0.443783 0.476958 11.00000 -1.20000 AFIX 0 C27 1 0.150139 0.512254 0.512902 11.00000 0.02120 0.03074 = 0.03901 0.01207 0.00497 0.00070 AFIX 43 H27 2 0.126067 0.529334 0.467589 11.00000 -1.20000 AFIX 0 C28 1 0.124690 0.538270 0.571805 11.00000 0.02640 0.02500 = 0.05270 0.00058 0.00835 0.00735 AFIX 43 H28 2 0.085210 0.573721 0.567495 11.00000 -1.20000 AFIX 0 C29 1 0.156665 0.512756 0.637683 11.00000 0.02692 0.02248 = 0.03953 -0.00498 0.00695 0.00206 AFIX 43 H29 2 0.138077 0.530309 0.678638 11.00000 -1.20000 AFIX 0 C30 1 0.216732 0.460787 0.643738 11.00000 0.01649 0.01685 = 0.02633 -0.00042 0.00297 -0.00184 C31 1 0.248019 0.429267 0.709988 11.00000 0.01296 0.02081 = 0.02824 -0.00336 0.00463 -0.00709 C32 1 0.230728 0.445790 0.776450 11.00000 0.02325 0.03170 = 0.03308 -0.00749 0.01119 -0.00001 AFIX 43 H32 2 0.193722 0.480950 0.782044 11.00000 -1.20000 AFIX 0 C33 1 0.267257 0.411174 0.834477 11.00000 0.04292 0.03993 = 0.02502 -0.00770 0.01269 -0.00034 AFIX 43 H33 2 0.255180 0.422252 0.880090 11.00000 -1.20000 AFIX 0 C34 1 0.321444 0.360361 0.825830 11.00000 0.04758 0.03591 = 0.02295 0.00328 0.00742 0.00197 AFIX 43 H34 2 0.348304 0.336378 0.865433 11.00000 -1.20000 AFIX 0 C35 1 0.335863 0.345086 0.759563 11.00000 0.03033 0.02561 = 0.02477 0.00248 0.01054 0.00009 AFIX 43 H35 2 0.373067 0.310037 0.753675 11.00000 -1.20000 AFIX 0 C36 1 0.473877 0.407388 0.620498 11.00000 0.01491 0.01245 = 0.02188 0.00265 0.00178 0.00321 C37 1 0.529691 0.433876 0.683616 11.00000 0.02016 0.02070 = 0.01929 0.00015 0.00470 -0.00098 AFIX 43 H37 2 0.500759 0.428274 0.725992 11.00000 -1.20000 AFIX 0 C38 1 0.625957 0.467950 0.685206 11.00000 0.02137 0.02160 = 0.02135 -0.00282 -0.00133 -0.00241 AFIX 43 H38 2 0.663081 0.484784 0.728655 11.00000 -1.20000 AFIX 0 C39 1 0.668274 0.477594 0.624040 11.00000 0.01759 0.02410 = 0.02809 0.00045 0.00165 -0.00766 AFIX 43 H39 2 0.734094 0.501146 0.625296 11.00000 -1.20000 AFIX 0 C40 1 0.614779 0.452976 0.561318 11.00000 0.02252 0.02481 = 0.02710 0.00455 0.00818 -0.00430 AFIX 43 H40 2 0.643200 0.459819 0.519018 11.00000 -1.20000 AFIX 0 C41 1 0.519706 0.418282 0.559671 11.00000 0.01777 0.01785 = 0.01840 0.00207 0.00136 -0.00182 C42 1 0.460600 0.388354 0.495304 11.00000 0.01715 0.01723 = 0.02281 0.00153 0.00560 -0.00094 C43 1 0.490544 0.391431 0.429058 11.00000 0.03369 0.03303 = 0.02594 -0.00115 0.01021 -0.00983 AFIX 43 H43 2 0.552199 0.415362 0.421913 11.00000 -1.20000 AFIX 0 C44 1 0.430976 0.359857 0.373870 11.00000 0.04691 0.04980 = 0.02210 -0.00368 0.01236 -0.01197 AFIX 43 H44 2 0.450769 0.361764 0.328238 11.00000 -1.20000 AFIX 0 C45 1 0.341928 0.325279 0.385410 11.00000 0.03249 0.03977 = 0.02734 -0.00877 0.00190 -0.00509 AFIX 43 H45 2 0.300128 0.302755 0.347974 11.00000 -1.20000 AFIX 0 C46 1 0.314858 0.323872 0.450927 11.00000 0.01973 0.02325 = 0.02524 -0.00019 0.00251 0.00032 AFIX 43 H46 2 0.253812 0.299751 0.458604 11.00000 -1.20000 AFIX 0 C47 1 0.577819 0.276683 0.614809 11.00000 0.01575 0.01219 = 0.02376 0.00323 0.00413 0.00034 C48 1 0.645023 0.302835 0.672304 11.00000 0.01844 0.01989 = 0.02250 0.00367 0.00415 0.00316 C49 1 0.747897 0.330006 0.669247 11.00000 0.01708 0.02479 = 0.03279 0.00250 -0.00439 -0.00364 C50 1 0.787485 0.333025 0.605776 11.00000 0.01501 0.02178 = 0.03825 0.00803 0.00400 -0.00313 C51 1 0.720146 0.306645 0.547008 11.00000 0.02195 0.02422 = 0.02864 0.00370 0.00866 0.00090 C52 1 0.619546 0.278793 0.551744 11.00000 0.01322 0.02014 = 0.02683 0.00043 -0.00015 0.00067 C53 1 0.967721 0.381071 0.648792 11.00000 0.01888 0.04157 = 0.07830 -0.01185 0.01228 -0.01427 AFIX 137 H53A 2 1.036703 0.391920 0.630527 11.00000 -1.50000 H53B 2 0.988417 0.352307 0.686064 11.00000 -1.50000 H53C 2 0.936071 0.414675 0.668510 11.00000 -1.50000 AFIX 0 C54 1 0.072582 0.231611 0.603779 11.00000 0.01439 0.01179 = 0.01920 0.00465 0.00320 0.00198 C55 1 0.032487 0.223483 0.666483 11.00000 0.02061 0.03134 = 0.01483 0.00635 0.00086 0.00119 C56 1 -0.073995 0.199984 0.667450 11.00000 0.02540 0.04118 = 0.02458 0.01964 0.01444 0.00921 C57 1 -0.145839 0.181786 0.606325 11.00000 0.01304 0.02195 = 0.04578 0.00859 0.00923 0.00050 C58 1 -0.107580 0.190575 0.543337 11.00000 0.01780 0.02372 = 0.02950 -0.00507 -0.00163 -0.00166 C59 1 -0.002133 0.215268 0.542847 11.00000 0.01917 0.01932 = 0.01522 0.00058 0.00453 0.00220 PART 1 O4A 6 -0.253581 0.158737 0.592440 21.00000 0.01786 0.05245 = 0.05023 0.01433 0.00599 -0.01199 C60A 1 -0.281711 0.123206 0.646551 21.00000 0.03730 0.04013 = 0.07748 0.02939 0.03108 0.01429 AFIX 3 H60A 2 -0.349741 0.100276 0.626811 21.00000 -1.50000 H60B 2 -0.298961 0.147196 0.684961 21.00000 -1.50000 H60C 2 -0.216761 0.097996 0.665241 21.00000 -1.50000 AFIX 0 PART 0 PART 2 O4B 6 -0.246609 0.159999 0.621641 -21.00000 0.01786 0.05245 = 0.05023 0.01433 0.00599 -0.01199 C60B 1 -0.308249 0.119763 0.571737 -21.00000 0.02641 0.03241 = 0.07578 -0.00222 0.02095 -0.01127 AFIX 3 H60D 2 -0.359409 0.139763 0.533187 -21.00000 -1.50000 H60E 2 -0.354289 0.095003 0.596567 -21.00000 -1.50000 H60F 2 -0.252809 0.096683 0.552027 -21.00000 -1.50000 AFIX 0 HKLF 4 REM 17asb004 in P2(1)/n REM R1 = 0.0360 for 11519 Fo > 4sig(Fo) and 0.0629 for all 15211 data REM 735 parameters refined using 18 restraints END WGHT 0.0232 8.4689 REM Highest difference peak 1.452, deepest hole -1.041, 1-sigma level 0.152 Q1 1 0.3351 0.3606 0.6418 11.00000 0.05 1.45 Q2 1 0.3332 0.1430 0.6807 11.00000 0.05 1.38 Q3 1 0.3599 0.1264 0.6037 11.00000 0.05 1.27 Q4 1 0.3591 0.3993 0.6023 11.00000 0.05 1.02 Q5 1 0.3767 0.1231 0.6505 11.00000 0.05 0.85 Q6 1 0.3556 0.1804 0.6419 11.00000 0.05 0.83 Q7 1 0.2765 0.3403 0.6242 11.00000 0.05 0.80 Q8 1 0.3855 0.3395 0.6058 11.00000 0.05 0.74 Q9 1 0.2967 0.4031 0.5962 11.00000 0.05 0.73 Q10 1 -0.3351 0.0604 0.5087 11.00000 0.05 0.71 ; _shelx_res_checksum 80416 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -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 0.32822(2) 0.14684(2) 0.63356(2) 0.01543(4) Uani 1 1 d . . . . . Ir2 Ir 0.32956(2) 0.36091(2) 0.60343(2) 0.01495(4) Uani 1 1 d . . . . . F1 F 0.6116(2) 0.30107(10) 0.73566(12) 0.0292(5) Uani 1 1 d . . . . . F2 F 0.8053(2) 0.35438(11) 0.72912(14) 0.0405(7) Uani 1 1 d . . . . . F3 F 0.7551(2) 0.30815(11) 0.48458(13) 0.0354(6) Uani 1 1 d . . . . . F4 F 0.5596(2) 0.25356(9) 0.49346(12) 0.0279(6) Uani 1 1 d . . . . . F5 F 0.0974(2) 0.24013(13) 0.72807(13) 0.0426(7) Uani 1 1 d . . . . . F6 F -0.1095(2) 0.19626(14) 0.72956(14) 0.0516(8) Uani 1 1 d . . . . . F7 F -0.1740(2) 0.17489(12) 0.48152(14) 0.0454(7) Uani 1 1 d . . . . . F8 F 0.0306(2) 0.22316(11) 0.47990(12) 0.0297(5) Uani 1 1 d . . . . . O1 O 0.4802(2) 0.18966(10) 0.61566(14) 0.0199(6) Uani 1 1 d . . . . . O2 O 0.1704(2) 0.31373(10) 0.58000(14) 0.0196(6) Uani 1 1 d . . . . . O3 O 0.8840(3) 0.35843(14) 0.59290(19) 0.0411(8) Uani 1 1 d . . . . . N1 N 0.2802(3) 0.23575(12) 0.62393(16) 0.0154(6) Uani 1 1 d . . . . . N2 N 0.3777(3) 0.27261(12) 0.62243(16) 0.0153(6) Uani 1 1 d . . . . . N3 N 0.3995(3) 0.15230(13) 0.73830(17) 0.0207(7) Uani 1 1 d . . . . . N4 N 0.2568(3) 0.13483(12) 0.52955(16) 0.0182(6) Uani 1 1 d . . . . . N5 N 0.2990(3) 0.37813(13) 0.70190(17) 0.0181(7) Uani 1 1 d . . . . . N6 N 0.3710(3) 0.35528(12) 0.50555(16) 0.0176(6) Uani 1 1 d . . . . . C1 C 0.4709(3) 0.24389(15) 0.6183(2) 0.0162(8) Uani 1 1 d . . . . . C2 C 0.1828(3) 0.26265(15) 0.60190(19) 0.0155(7) Uani 1 1 d . . . . . C3 C 0.4158(3) 0.07337(16) 0.6452(2) 0.0215(8) Uani 1 1 d . . . . . C4 C 0.4179(4) 0.03018(16) 0.5949(2) 0.0269(9) Uani 1 1 d . . . . . H4 H 0.366428 0.032079 0.550336 0.032 Uiso 1 1 calc R . . . . C5 C 0.4944(4) -0.01559(17) 0.6096(3) 0.0340(11) Uani 1 1 d . . . . . H5 H 0.494567 -0.044590 0.575113 0.041 Uiso 1 1 calc R . . . . C6 C 0.5701(4) -0.01868(19) 0.6744(3) 0.0414(12) Uani 1 1 d . . . . . H6 H 0.622545 -0.049664 0.684013 0.050 Uiso 1 1 calc R . . . . C7 C 0.5697(4) 0.02285(19) 0.7247(3) 0.0384(12) Uani 1 1 d . . . . . H7 H 0.621593 0.020450 0.769101 0.046 Uiso 1 1 calc R . . . . C8 C 0.4928(3) 0.06877(16) 0.7107(2) 0.0241(9) Uani 1 1 d . . . . . C9 C 0.4838(3) 0.11347(16) 0.7622(2) 0.0236(9) Uani 1 1 d . . . . . C10 C 0.5449(4) 0.11738(19) 0.8318(2) 0.0336(11) Uani 1 1 d . . . . . H10 H 0.605813 0.091360 0.848331 0.040 Uiso 1 1 calc R . . . . C11 C 0.5179(4) 0.15839(19) 0.8769(2) 0.0352(11) Uani 1 1 d . . . . . H11 H 0.560403 0.161065 0.924129 0.042 Uiso 1 1 calc R . . . . C12 C 0.4283(4) 0.19587(18) 0.8528(2) 0.0310(10) Uani 1 1 d . . . . . H12 H 0.406062 0.223672 0.883501 0.037 Uiso 1 1 calc R . . . . C13 C 0.3726(3) 0.19164(16) 0.7832(2) 0.0239(9) Uani 1 1 d . . . . . H13 H 0.312246 0.217774 0.766027 0.029 Uiso 1 1 calc R . . . . C14 C 0.1861(3) 0.10457(14) 0.6444(2) 0.0191(8) Uani 1 1 d . . . . . C15 C 0.1495(3) 0.08923(16) 0.7073(2) 0.0232(9) Uani 1 1 d . . . . . H15 H 0.193505 0.101217 0.751649 0.028 Uiso 1 1 calc R . . . . C16 C 0.0509(4) 0.05705(16) 0.7061(2) 0.0288(10) Uani 1 1 d . . . . . H16 H 0.029170 0.046669 0.749572 0.035 Uiso 1 1 calc R . . . . C17 C -0.0163(4) 0.03988(16) 0.6426(3) 0.0296(10) Uani 1 1 d . . . . . H17 H -0.083948 0.017897 0.642396 0.035 Uiso 1 1 calc R . . . . C18 C 0.0148(3) 0.05463(16) 0.5796(2) 0.0270(9) Uani 1 1 d . . . . . H18 H -0.031854 0.043373 0.535725 0.032 Uiso 1 1 calc R . . . . C19 C 0.1167(3) 0.08668(15) 0.5803(2) 0.0209(8) Uani 1 1 d . . . . . C20 C 0.1557(3) 0.10485(15) 0.5163(2) 0.0221(8) Uani 1 1 d . . . . . C21 C 0.1017(4) 0.09497(17) 0.4464(2) 0.0328(10) Uani 1 1 d . . . . . H21 H 0.032260 0.073426 0.436654 0.039 Uiso 1 1 calc R . . . . C22 C 0.1477(5) 0.11606(19) 0.3913(2) 0.0395(12) Uani 1 1 d . . . . . H22 H 0.109921 0.109578 0.343565 0.047 Uiso 1 1 calc R . . . . C23 C 0.2496(4) 0.14680(18) 0.4055(2) 0.0336(10) Uani 1 1 d . . . . . H23 H 0.282877 0.161634 0.368038 0.040 Uiso 1 1 calc R . . . . C24 C 0.3014(4) 0.15537(16) 0.4752(2) 0.0271(9) Uani 1 1 d . . . . . H24 H 0.371200 0.176554 0.485428 0.033 Uiso 1 1 calc R . . . . C25 C 0.2467(3) 0.43517(15) 0.5841(2) 0.0187(8) Uani 1 1 d . . . . . C26 C 0.2108(3) 0.46112(16) 0.5185(2) 0.0230(8) Uani 1 1 d . . . . . H26 H 0.227824 0.443783 0.476958 0.028 Uiso 1 1 calc R . . . . C27 C 0.1501(4) 0.51225(18) 0.5129(2) 0.0304(10) Uani 1 1 d . . . . . H27 H 0.126067 0.529334 0.467589 0.037 Uiso 1 1 calc R . . . . C28 C 0.1247(4) 0.53827(18) 0.5718(3) 0.0346(11) Uani 1 1 d . . . . . H28 H 0.085210 0.573721 0.567495 0.042 Uiso 1 1 calc R . . . . C29 C 0.1567(4) 0.51276(17) 0.6377(2) 0.0296(10) Uani 1 1 d . . . . . H29 H 0.138077 0.530309 0.678638 0.035 Uiso 1 1 calc R . . . . C30 C 0.2167(3) 0.46079(15) 0.6437(2) 0.0200(8) Uani 1 1 d . . . . . C31 C 0.2480(3) 0.42927(16) 0.7100(2) 0.0206(8) Uani 1 1 d . . . . . C32 C 0.2307(4) 0.44579(18) 0.7765(2) 0.0286(10) Uani 1 1 d . . . . . H32 H 0.193722 0.480950 0.782044 0.034 Uiso 1 1 calc R . . . . C33 C 0.2673(4) 0.41117(19) 0.8345(2) 0.0351(11) Uani 1 1 d . . . . . H33 H 0.255180 0.422252 0.880090 0.042 Uiso 1 1 calc R . . . . C34 C 0.3214(4) 0.36036(19) 0.8258(2) 0.0354(11) Uani 1 1 d . . . . . H34 H 0.348304 0.336378 0.865433 0.042 Uiso 1 1 calc R . . . . C35 C 0.3359(4) 0.34509(17) 0.7596(2) 0.0262(9) Uani 1 1 d . . . . . H35 H 0.373067 0.310037 0.753675 0.031 Uiso 1 1 calc R . . . . C36 C 0.4739(3) 0.40739(14) 0.6205(2) 0.0167(8) Uani 1 1 d . . . . . C37 C 0.5297(3) 0.43388(15) 0.6836(2) 0.0199(8) Uani 1 1 d . . . . . H37 H 0.500759 0.428274 0.725992 0.024 Uiso 1 1 calc R . . . . C38 C 0.6260(3) 0.46795(16) 0.6852(2) 0.0222(8) Uani 1 1 d . . . . . H38 H 0.663081 0.484784 0.728655 0.027 Uiso 1 1 calc R . . . . C39 C 0.6683(3) 0.47759(16) 0.6240(2) 0.0236(9) Uani 1 1 d . . . . . H39 H 0.734094 0.501146 0.625296 0.028 Uiso 1 1 calc R . . . . C40 C 0.6148(3) 0.45298(16) 0.5613(2) 0.0244(9) Uani 1 1 d . . . . . H40 H 0.643200 0.459819 0.519018 0.029 Uiso 1 1 calc R . . . . C41 C 0.5197(3) 0.41828(15) 0.5597(2) 0.0183(8) Uani 1 1 d . . . . . C42 C 0.4606(3) 0.38835(15) 0.4953(2) 0.0188(8) Uani 1 1 d . . . . . C43 C 0.4905(4) 0.39143(18) 0.4291(2) 0.0303(10) Uani 1 1 d . . . . . H43 H 0.552199 0.415362 0.421913 0.036 Uiso 1 1 calc R . . . . C44 C 0.4310(4) 0.3599(2) 0.3739(2) 0.0388(11) Uani 1 1 d . . . . . H44 H 0.450769 0.361764 0.328238 0.047 Uiso 1 1 calc R . . . . C45 C 0.3419(4) 0.32528(19) 0.3854(2) 0.0337(10) Uani 1 1 d . . . . . H45 H 0.300128 0.302755 0.347974 0.040 Uiso 1 1 calc R . . . . C46 C 0.3149(3) 0.32387(16) 0.4509(2) 0.0230(9) Uani 1 1 d . . . . . H46 H 0.253812 0.299751 0.458604 0.028 Uiso 1 1 calc R . . . . C47 C 0.5778(3) 0.27668(14) 0.6148(2) 0.0172(8) Uani 1 1 d . . . . . C48 C 0.6450(3) 0.30283(15) 0.6723(2) 0.0202(8) Uani 1 1 d . . . . . C49 C 0.7479(3) 0.33001(17) 0.6692(2) 0.0261(9) Uani 1 1 d . . . . . C50 C 0.7875(3) 0.33303(16) 0.6058(2) 0.0252(9) Uani 1 1 d . . . . . C51 C 0.7201(4) 0.30664(17) 0.5470(2) 0.0244(9) Uani 1 1 d . . . . . C52 C 0.6195(3) 0.27879(16) 0.5517(2) 0.0206(8) Uani 1 1 d . . . . . C53 C 0.9677(4) 0.3811(2) 0.6488(3) 0.0459(14) Uani 1 1 d . . . . . H53A H 1.036703 0.391920 0.630527 0.069 Uiso 1 1 calc GR . . . . H53B H 0.988417 0.352307 0.686064 0.069 Uiso 1 1 calc GR . . . . H53C H 0.936071 0.414675 0.668510 0.069 Uiso 1 1 calc GR . . . . C54 C 0.0726(3) 0.23161(14) 0.60378(19) 0.0151(7) Uani 1 1 d . . . . . C55 C 0.0325(3) 0.22348(17) 0.6665(2) 0.0226(8) Uani 1 1 d . . . . . C56 C -0.0740(4) 0.19998(19) 0.6674(2) 0.0291(10) Uani 1 1 d . . . . . C57 C -0.1458(3) 0.18179(16) 0.6063(2) 0.0264(9) Uani 1 1 d . U . . . C58 C -0.1076(3) 0.19058(16) 0.5433(2) 0.0245(9) Uani 1 1 d . . . . . C59 C -0.0021(3) 0.21527(15) 0.54285(19) 0.0177(8) Uani 1 1 d . . . . . O4A O -0.2536(12) 0.1587(7) 0.5924(5) 0.040(2) Uani 0.520(9) 1 d . U P A 1 C60A C -0.2817(9) 0.1232(4) 0.6466(6) 0.049(3) Uani 0.520(9) 1 d . U P A 1 H60A H -0.349741 0.100276 0.626811 0.073 Uiso 0.520(9) 1 d R . P A 1 H60B H -0.298961 0.147196 0.684961 0.073 Uiso 0.520(9) 1 d R . P A 1 H60C H -0.216761 0.097996 0.665241 0.073 Uiso 0.520(9) 1 d R . P A 1 O4B O -0.2466(14) 0.1600(8) 0.6216(6) 0.040(2) Uani 0.480(9) 1 d . U P A 2 C60B C -0.3082(9) 0.1198(4) 0.5717(7) 0.043(3) Uani 0.480(9) 1 d . U P A 2 H60D H -0.359409 0.139763 0.533187 0.065 Uiso 0.480(9) 1 d R . P A 2 H60E H -0.354289 0.095003 0.596567 0.065 Uiso 0.480(9) 1 d R . P A 2 H60F H -0.252809 0.096683 0.552027 0.065 Uiso 0.480(9) 1 d R . P A 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 0.01304(7) 0.01273(6) 0.01983(8) 0.00259(6) 0.00146(6) -0.00104(5) Ir2 0.01382(7) 0.01255(6) 0.01870(7) 0.00136(6) 0.00367(6) -0.00130(5) F1 0.0288(13) 0.0374(13) 0.0214(12) -0.0016(11) 0.0046(11) -0.0077(11) F2 0.0306(14) 0.0514(16) 0.0346(15) -0.0028(13) -0.0061(12) -0.0223(13) F3 0.0294(14) 0.0474(15) 0.0344(15) 0.0060(12) 0.0182(12) -0.0049(12) F4 0.0261(13) 0.0341(13) 0.0234(13) -0.0048(10) 0.0048(11) -0.0064(10) F5 0.0295(15) 0.081(2) 0.0164(13) -0.0009(13) 0.0012(12) -0.0013(14) F6 0.0334(16) 0.090(2) 0.0358(16) 0.0245(16) 0.0182(13) 0.0017(16) F7 0.0276(15) 0.0644(19) 0.0402(16) -0.0166(14) -0.0032(12) -0.0138(14) F8 0.0257(13) 0.0461(15) 0.0174(12) 0.0003(11) 0.0049(10) 0.0014(11) O1 0.0151(13) 0.0146(12) 0.0299(15) 0.0035(11) 0.0041(12) -0.0005(10) O2 0.0146(13) 0.0157(12) 0.0273(15) 0.0051(11) 0.0014(11) -0.0015(10) O3 0.0185(16) 0.052(2) 0.053(2) 0.0135(17) 0.0059(15) -0.0150(15) N1 0.0115(15) 0.0165(14) 0.0181(16) 0.0022(12) 0.0029(13) -0.0038(12) N2 0.0123(15) 0.0128(14) 0.0215(17) 0.0019(12) 0.0048(13) -0.0046(12) N3 0.0185(16) 0.0162(15) 0.0263(18) 0.0047(13) 0.0015(14) -0.0046(13) N4 0.0206(16) 0.0145(14) 0.0200(16) 0.0008(12) 0.0051(13) 0.0010(12) N5 0.0148(16) 0.0177(15) 0.0216(17) 0.0025(13) 0.0029(13) -0.0033(12) N6 0.0154(15) 0.0180(15) 0.0178(15) 0.0004(13) -0.0005(12) 0.0026(13) C1 0.0144(18) 0.0181(17) 0.016(2) 0.0020(14) 0.0021(16) -0.0047(14) C2 0.0160(18) 0.0166(17) 0.0132(18) 0.0008(14) 0.0009(15) -0.0029(14) C3 0.0156(19) 0.0166(17) 0.033(2) 0.0053(16) 0.0049(17) -0.0008(15) C4 0.026(2) 0.0197(19) 0.035(2) 0.0058(18) 0.0059(19) 0.0014(16) C5 0.036(3) 0.020(2) 0.046(3) 0.004(2) 0.011(2) 0.0052(19) C6 0.035(3) 0.029(2) 0.061(3) 0.010(2) 0.010(3) 0.016(2) C7 0.025(2) 0.038(3) 0.048(3) 0.011(2) -0.004(2) 0.007(2) C8 0.0127(19) 0.0221(19) 0.036(2) 0.0079(18) 0.0016(17) -0.0025(15) C9 0.018(2) 0.0200(18) 0.031(2) 0.0062(17) 0.0008(17) -0.0076(15) C10 0.022(2) 0.031(2) 0.039(3) 0.013(2) -0.014(2) -0.0049(18) C11 0.039(3) 0.035(2) 0.026(2) 0.004(2) -0.008(2) -0.014(2) C12 0.037(3) 0.026(2) 0.027(2) -0.0023(18) -0.001(2) -0.0094(19) C13 0.020(2) 0.0239(19) 0.026(2) 0.0038(17) 0.0013(17) -0.0067(16) C14 0.0137(18) 0.0122(16) 0.031(2) 0.0017(15) 0.0026(16) 0.0024(14) C15 0.018(2) 0.0206(19) 0.031(2) 0.0025(17) 0.0047(18) -0.0002(16) C16 0.026(2) 0.0204(19) 0.043(3) 0.0055(18) 0.014(2) -0.0003(17) C17 0.020(2) 0.0176(19) 0.054(3) 0.0013(19) 0.013(2) -0.0043(16) C18 0.019(2) 0.0168(18) 0.042(3) -0.0018(18) -0.0018(19) 0.0000(16) C19 0.019(2) 0.0129(16) 0.029(2) 0.0007(15) 0.0006(17) 0.0013(14) C20 0.022(2) 0.0148(17) 0.028(2) -0.0014(16) -0.0012(17) 0.0010(15) C21 0.039(3) 0.024(2) 0.031(2) -0.0056(18) -0.005(2) -0.0028(19) C22 0.056(3) 0.032(2) 0.024(2) -0.003(2) -0.007(2) -0.002(2) C23 0.050(3) 0.032(2) 0.020(2) 0.0020(19) 0.008(2) 0.000(2) C24 0.034(2) 0.0213(19) 0.026(2) 0.0020(17) 0.0059(19) 0.0000(18) C25 0.0117(18) 0.0156(17) 0.030(2) 0.0019(16) 0.0062(16) -0.0051(14) C26 0.015(2) 0.0222(19) 0.033(2) 0.0038(17) 0.0073(17) -0.0019(15) C27 0.021(2) 0.031(2) 0.039(3) 0.012(2) 0.005(2) 0.0007(18) C28 0.026(2) 0.025(2) 0.053(3) 0.001(2) 0.008(2) 0.0074(18) C29 0.027(2) 0.022(2) 0.040(3) -0.0050(19) 0.007(2) 0.0021(17) C30 0.016(2) 0.0168(17) 0.026(2) -0.0004(16) 0.0030(16) -0.0018(15) C31 0.0130(18) 0.0208(18) 0.028(2) -0.0034(16) 0.0046(16) -0.0071(15) C32 0.023(2) 0.032(2) 0.033(2) -0.0075(19) 0.0112(19) 0.0000(18) C33 0.043(3) 0.040(3) 0.025(2) -0.008(2) 0.013(2) 0.000(2) C34 0.048(3) 0.036(2) 0.023(2) 0.003(2) 0.007(2) 0.002(2) C35 0.030(2) 0.026(2) 0.025(2) 0.0025(17) 0.0105(18) 0.0001(18) C36 0.0149(18) 0.0125(16) 0.022(2) 0.0026(14) 0.0018(15) 0.0032(14) C37 0.020(2) 0.0207(18) 0.0193(19) 0.0001(15) 0.0047(16) -0.0010(15) C38 0.021(2) 0.0216(19) 0.021(2) -0.0028(16) -0.0013(17) -0.0024(16) C39 0.018(2) 0.0241(19) 0.028(2) 0.0004(17) 0.0016(17) -0.0077(16) C40 0.023(2) 0.025(2) 0.027(2) 0.0046(17) 0.0082(18) -0.0043(17) C41 0.0178(19) 0.0178(17) 0.0184(19) 0.0021(15) 0.0014(16) -0.0018(15) C42 0.0172(19) 0.0172(17) 0.023(2) 0.0015(15) 0.0056(16) -0.0009(15) C43 0.034(3) 0.033(2) 0.026(2) -0.0012(19) 0.010(2) -0.0098(19) C44 0.047(3) 0.050(3) 0.022(2) -0.004(2) 0.012(2) -0.012(2) C45 0.032(3) 0.040(3) 0.027(2) -0.009(2) 0.002(2) -0.005(2) C46 0.020(2) 0.0232(19) 0.025(2) -0.0002(17) 0.0025(17) 0.0003(16) C47 0.0157(18) 0.0122(16) 0.024(2) 0.0032(15) 0.0041(16) 0.0003(14) C48 0.018(2) 0.0199(18) 0.023(2) 0.0037(16) 0.0042(17) 0.0032(15) C49 0.017(2) 0.025(2) 0.033(2) 0.0025(18) -0.0044(18) -0.0036(16) C50 0.015(2) 0.0218(19) 0.038(3) 0.0080(18) 0.0040(18) -0.0031(16) C51 0.022(2) 0.024(2) 0.029(2) 0.0037(17) 0.0087(18) 0.0009(16) C52 0.0132(19) 0.0201(18) 0.027(2) 0.0004(16) -0.0001(16) 0.0007(15) C53 0.019(2) 0.042(3) 0.078(4) -0.012(3) 0.012(3) -0.014(2) C54 0.0144(18) 0.0118(15) 0.0192(19) 0.0047(14) 0.0032(15) 0.0020(14) C55 0.021(2) 0.031(2) 0.0148(19) 0.0063(17) 0.0009(16) 0.0012(17) C56 0.025(2) 0.041(2) 0.025(2) 0.0196(19) 0.0144(19) 0.0092(19) C57 0.0130(19) 0.0219(19) 0.046(3) 0.0086(19) 0.0092(19) 0.0005(15) C58 0.018(2) 0.0237(19) 0.030(2) -0.0051(17) -0.0016(18) -0.0017(16) C59 0.0192(19) 0.0193(18) 0.0152(18) 0.0006(15) 0.0045(16) 0.0022(15) O4A 0.018(2) 0.052(2) 0.050(6) 0.014(6) 0.006(5) -0.0120(18) C60A 0.037(6) 0.040(5) 0.077(9) 0.029(5) 0.031(6) 0.014(4) O4B 0.018(2) 0.052(2) 0.050(6) 0.014(6) 0.006(5) -0.0120(18) C60B 0.026(5) 0.032(5) 0.076(9) -0.002(5) 0.021(5) -0.011(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.00 1.00 0.00 0.0430 0.00 -1.00 0.00 0.0560 -1.00 0.00 0.00 0.0500 1.00 0.00 0.00 0.0180 0.00 0.00 1.00 0.0220 0.00 0.00 -1.00 0.0580 -1.00 0.00 1.00 0.0350 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O1 Ir1 N1 75.28(10) N3 Ir1 O1 85.95(11) N3 Ir1 N1 94.32(12) N3 Ir1 N4 175.63(12) N4 Ir1 O1 96.27(11) N4 Ir1 N1 89.89(11) C3 Ir1 O1 89.58(12) C3 Ir1 N1 164.40(13) C3 Ir1 N3 80.64(15) C3 Ir1 N4 95.59(14) C14 Ir1 O1 176.45(13) C14 Ir1 N1 106.16(13) C14 Ir1 N3 97.12(14) C14 Ir1 N4 80.55(14) C14 Ir1 C3 89.17(14) O2 Ir2 N2 74.43(10) N5 Ir2 O2 89.57(11) N5 Ir2 N2 97.02(12) N5 Ir2 N6 171.52(12) N6 Ir2 O2 97.43(11) N6 Ir2 N2 89.49(11) C25 Ir2 O2 92.00(12) C25 Ir2 N2 166.24(13) C25 Ir2 N5 80.26(14) C25 Ir2 N6 94.66(14) C36 Ir2 O2 176.82(12) C36 Ir2 N2 107.99(12) C36 Ir2 N5 92.14(14) C36 Ir2 N6 80.65(14) C36 Ir2 C25 85.65(14) C1 O1 Ir1 112.4(2) C2 O2 Ir2 112.1(2) C50 O3 C53 121.2(4) N2 N1 Ir1 112.6(2) C2 N1 Ir1 133.9(2) C2 N1 N2 110.9(3) N1 N2 Ir2 113.2(2) C1 N2 Ir2 133.0(2) C1 N2 N1 112.0(3) C9 N3 Ir1 115.3(3) C13 N3 Ir1 125.1(3) C13 N3 C9 119.5(3) C20 N4 Ir1 115.9(3) C24 N4 Ir1 124.2(3) C24 N4 C20 119.9(3) C31 N5 Ir2 116.2(3) C35 N5 Ir2 124.0(3) C35 N5 C31 119.4(3) C42 N6 Ir2 115.4(2) C46 N6 Ir2 125.8(3) C46 N6 C42 118.7(3) O1 C1 N2 126.6(3) O1 C1 C47 115.7(3) N2 C1 C47 117.8(3) O2 C2 N1 127.0(3) O2 C2 C54 115.0(3) N1 C2 C54 118.0(3) C4 C3 Ir1 128.6(3) C4 C3 C8 117.7(4) C8 C3 Ir1 113.4(3) C5 C4 C3 120.9(4) C6 C5 C4 120.0(4) C7 C6 C5 120.3(4) C6 C7 C8 120.1(4) C3 C8 C9 115.5(3) C7 C8 C3 120.9(4) C7 C8 C9 123.5(4) N3 C9 C8 113.5(3) N3 C9 C10 119.1(4) C10 C9 C8 127.2(4) C11 C10 C9 120.7(4) C10 C11 C12 119.4(4) C13 C12 C11 118.0(4) N3 C13 C12 123.1(4) C15 C14 Ir1 128.5(3) C19 C14 Ir1 114.7(3) C19 C14 C15 116.8(3) C16 C15 C14 121.6(4) C17 C16 C15 120.7(4) C18 C17 C16 119.9(4) C17 C18 C19 119.7(4) C14 C19 C18 121.2(4) C14 C19 C20 115.2(3) C18 C19 C20 123.6(4) N4 C20 C19 113.6(3) N4 C20 C21 119.2(4) C21 C20 C19 127.2(4) C22 C21 C20 120.5(4) C21 C22 C23 119.6(4) C24 C23 C22 118.4(4) N4 C24 C23 122.4(4) C26 C25 Ir2 127.1(3) C26 C25 C30 118.2(3) C30 C25 Ir2 114.5(3) C25 C26 C27 120.7(4) C28 C27 C26 120.9(4) C27 C28 C29 119.8(4) C28 C29 C30 119.7(4) C25 C30 C29 120.6(4) C25 C30 C31 115.8(3) C29 C30 C31 123.6(4) N5 C31 C30 113.0(3) N5 C31 C32 119.8(4) C32 C31 C30 127.1(4) C33 C32 C31 120.0(4) C32 C33 C34 119.5(4) C35 C34 C33 119.0(4) N5 C35 C34 122.3(4) C37 C36 Ir2 128.7(3) C41 C36 Ir2 114.7(3) C41 C36 C37 116.4(3) C38 C37 C36 121.3(4) C39 C38 C37 120.4(4) C40 C39 C38 119.7(4) C39 C40 C41 120.1(4) C36 C41 C42 114.5(3) C40 C41 C36 122.0(4) C40 C41 C42 123.4(4) N6 C42 C41 114.0(3) N6 C42 C43 120.5(4) C43 C42 C41 125.5(4) C44 C43 C42 119.8(4) C43 C44 C45 119.2(4) C46 C45 C44 119.1(4) N6 C46 C45 122.7(4) C48 C47 C1 123.9(3) C48 C47 C52 115.9(3) C52 C47 C1 120.1(3) F1 C48 C47 119.1(3) F1 C48 C49 117.6(4) C47 C48 C49 123.2(4) F2 C49 C48 117.5(4) F2 C49 C50 121.9(4) C48 C49 C50 120.5(4) O3 C50 C49 128.5(4) O3 C50 C51 114.7(4) C49 C50 C51 116.9(4) F3 C51 C50 119.1(4) F3 C51 C52 119.4(4) C52 C51 C50 121.5(4) F4 C52 C47 119.4(3) F4 C52 C51 118.6(4) C51 C52 C47 122.0(4) C55 C54 C2 122.1(3) C59 C54 C2 122.1(3) C59 C54 C55 115.4(3) F5 C55 C54 119.5(4) F5 C55 C56 118.3(4) C56 C55 C54 122.1(4) F6 C56 C55 118.8(4) F6 C56 C57 119.4(4) C55 C56 C57 121.8(4) C56 C57 C58 116.5(4) C56 C57 O4B 110.4(6) O4A C57 C56 133.6(6) O4A C57 C58 109.8(6) O4B C57 C58 133.0(6) F7 C58 C57 119.9(4) F7 C58 C59 119.0(4) C59 C58 C57 121.1(4) F8 C59 C54 118.4(3) F8 C59 C58 118.7(3) C58 C59 C54 123.0(4) C57 O4A C60A 115.6(10) C57 O4B C60B 116.6(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ir1 O1 2.140(3) Ir1 N1 2.163(3) Ir1 N3 2.028(3) Ir1 N4 2.031(3) Ir1 C3 2.002(4) Ir1 C14 1.994(4) Ir2 O2 2.152(2) Ir2 N2 2.163(3) Ir2 N5 2.032(3) Ir2 N6 2.035(3) Ir2 C25 1.999(4) Ir2 C36 1.996(4) F1 C48 1.349(4) F2 C49 1.344(5) F3 C51 1.341(5) F4 C52 1.341(4) F5 C55 1.337(5) F6 C56 1.340(5) F7 C58 1.341(5) F8 C59 1.350(4) O1 C1 1.281(4) O2 C2 1.270(4) O3 C50 1.350(5) O3 C53 1.414(6) N1 N2 1.445(4) N1 C2 1.308(5) N2 C1 1.305(5) N3 C9 1.362(5) N3 C13 1.343(5) N4 C20 1.366(5) N4 C24 1.345(5) N5 C31 1.366(5) N5 C35 1.353(5) N6 C42 1.356(5) N6 C46 1.347(5) C1 C47 1.490(5) C2 C54 1.498(5) C3 C4 1.403(6) C3 C8 1.405(5) C4 C5 1.397(5) C5 C6 1.385(7) C6 C7 1.374(7) C7 C8 1.402(6) C8 C9 1.460(6) C9 C10 1.395(6) C10 C11 1.372(7) C11 C12 1.385(6) C12 C13 1.374(6) C14 C15 1.404(5) C14 C19 1.404(5) C15 C16 1.384(5) C16 C17 1.380(6) C17 C18 1.374(6) C18 C19 1.416(5) C19 C20 1.458(6) C20 C21 1.389(6) C21 C22 1.372(7) C22 C23 1.383(7) C23 C24 1.374(6) C25 C26 1.390(5) C25 C30 1.398(5) C26 C27 1.392(5) C27 C28 1.368(6) C28 C29 1.384(6) C29 C30 1.405(5) C30 C31 1.456(5) C31 C32 1.386(5) C32 C33 1.379(6) C33 C34 1.379(6) C34 C35 1.363(6) C36 C37 1.407(5) C36 C41 1.402(5) C37 C38 1.385(5) C38 C39 1.380(5) C39 C40 1.374(6) C40 C41 1.382(5) C41 C42 1.474(5) C42 C43 1.386(5) C43 C44 1.371(6) C44 C45 1.379(6) C45 C46 1.356(6) C47 C48 1.373(5) C47 C52 1.393(5) C48 C49 1.383(5) C49 C50 1.388(6) C50 C51 1.393(6) C51 C52 1.374(5) C54 C55 1.389(5) C54 C59 1.376(5) C55 C56 1.376(6) C56 C57 1.376(6) C57 C58 1.385(6) C57 O4A 1.360(14) C57 O4B 1.377(15) C58 C59 1.374(5) O4A C60A 1.421(16) O4B C60B 1.439(19)