#------------------------------------------------------------------------------ #$Date: 2021-11-04 02:00:01 +0200 (Thu, 04 Nov 2021) $ #$Revision: 270277 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/86/7708697.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_7708697 loop_ _publ_author_name 'Li, Qiuxia' 'Shi, Chao' 'Huang, Manli' 'Zhang, Xinghua' 'Sun, Fangxiang' 'Zheng, Ying' 'Yan, Hong' 'Yang, Chuluo' 'Yuan, Aihua' _publ_section_title ; Three types of charged ligand-based neutral phosphorescent iridium(iii) complexes featuring nido-carborane: synthesis, structures, and solution processed organic light-emitting diode applications ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT02990H _journal_year 2021 _chemical_formula_moiety 'C42 H50 B9 Ir N4, 2(C H2 Cl2)' _chemical_formula_sum 'C44 H54 B9 Cl4 Ir N4' _chemical_formula_weight 1070.20 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2021-07-07 deposited with the CCDC. 2021-10-21 downloaded from the CCDC. ; _cell_angle_alpha 97.597(3) _cell_angle_beta 91.556(3) _cell_angle_gamma 116.084(3) _cell_formula_units_Z 2 _cell_length_a 12.292(3) _cell_length_b 13.345(3) _cell_length_c 16.243(4) _cell_measurement_reflns_used 2949 _cell_measurement_temperature 158(2) _cell_measurement_theta_max 17.58 _cell_measurement_theta_min 2.30 _cell_volume 2361.2(10) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 158(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.983 _diffrn_measurement_device_type 'APEX2 CCD detector' _diffrn_measurement_method 'omega scan' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0815 _diffrn_reflns_av_unetI/netI 0.0929 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.983 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 30929 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.983 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.600 _diffrn_reflns_theta_min 1.853 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 3.091 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_correction_T_min 0.6759 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker, 2012)' _exptl_crystal_density_diffrn 1.505 _exptl_crystal_description sheet _exptl_crystal_F_000 1072 _exptl_crystal_size_max 0.170 _exptl_crystal_size_mid 0.110 _exptl_crystal_size_min 0.040 _refine_diff_density_max 0.811 _refine_diff_density_min -1.066 _refine_diff_density_rms 0.175 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 705 _refine_ls_number_reflns 8747 _refine_ls_number_restraints 561 _refine_ls_restrained_S_all 1.038 _refine_ls_R_factor_all 0.0811 _refine_ls_R_factor_gt 0.0537 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0658P)^2^+2.7943P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1167 _refine_ls_wR_factor_ref 0.1321 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6891 _reflns_number_total 8747 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt02990h2.cif _cod_data_source_block Ir3 _cod_original_cell_volume 2361.3(9) _cod_database_code 7708697 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.622 _shelx_estimated_absorpt_t_max 0.886 _shelx_res_file ; 1.res created by SHELXL-2014/7 TITL 1 in P-1 CELL 0.71073 12.2925 13.3449 16.2432 97.597 91.556 116.084 ZERR 2.00 0.0026 0.0030 0.0035 0.003 0.003 0.003 LATT 1 SFAC C H B N Cl Ir UNIT 88 108 18 8 8 2 L.S. 20 BOND $h acta FMAP 2 PLAN 20 omit 0 1 0 omit 0 0 1 size 0.17 0.11 0.04 sump 1 .0001 1 3 1 5 1 6 sadi .02 c43a cl1a c43a cl2a c43b cl1b c43b cl2b c43 cl1 c43 cl2 sadi .02 c43a cl1a c43y cl1y c43y cl2y c43z cl1z c43z cl2z sadi cl1a cl2a cl1b cl2b cl1y cl2y cl1z cl2z cl1 cl2 dfix 1.5 c32 c39a c32 c39z dfix 1.53 c39a c40a c39a c41a c39a c42a c39z c40z c39z c41z c39z c42z sadi c32 c40a c32 c41a c32 c42a c32 c40z c32 c41z c32 c42z sadi c40a c41a c41a c42a c42a c40a c40z c41z c41z c42z c42z c40z simu .02 .03 3 c43a > c42z dfix 1.1 b1 h1 b2 h2 b3 h3 c24 h24a sadi .02 h23 b2 h23 b3 TEMP -115 WGHT 0.065840 2.794300 FVAR 0.09147 0.53155 0.47630 0.66999 0.41146 0.11223 B1 3 0.895556 0.314130 0.637297 11.00000 0.03357 0.03889 = 0.03270 -0.01626 -0.01868 0.01904 H1 2 0.839156 0.228462 0.603568 11.00000 -1.20000 B2 3 1.027779 0.415994 0.598352 11.00000 0.05708 0.05000 = 0.02868 -0.01573 -0.01182 0.03826 H2 2 1.062708 0.403261 0.538299 11.00000 -1.20000 H23 2 0.999869 0.475947 0.605229 11.00000 -1.20000 B3 3 1.036253 0.546881 0.646392 11.00000 0.03334 0.03040 = 0.01921 0.00187 0.00406 0.02074 H3 2 1.082239 0.628344 0.625079 11.00000 -1.20000 B4 3 0.937496 0.466942 0.788827 11.00000 0.02363 0.02819 = 0.02476 0.00547 0.00002 0.00451 AFIX 153 H4 2 0.906279 0.483925 0.850966 11.00000 -1.20000 AFIX 0 B5 3 0.919150 0.332197 0.747428 11.00000 0.02844 0.02960 = 0.05247 0.01290 0.00127 0.01543 AFIX 153 H5 2 0.876208 0.259518 0.782428 11.00000 -1.20000 AFIX 0 B6 3 1.040993 0.351097 0.684139 11.00000 0.04280 0.02978 = 0.04871 -0.00219 -0.00973 0.02125 AFIX 153 H6 2 1.081270 0.290073 0.677110 11.00000 -1.20000 AFIX 0 B7 3 1.132581 0.500641 0.688444 11.00000 0.02264 0.03993 = 0.02902 0.00197 -0.00168 0.01163 AFIX 153 H7 2 1.233116 0.540391 0.683646 11.00000 -1.20000 AFIX 0 B8 3 1.066825 0.570197 0.753902 11.00000 0.02058 0.03282 = 0.02160 -0.00556 0.00380 0.01240 AFIX 153 H8 2 1.121902 0.655229 0.792638 11.00000 -1.20000 AFIX 0 B9 3 1.067626 0.445496 0.779620 11.00000 0.02477 0.02665 = 0.04464 0.00492 -0.01539 0.01280 AFIX 153 H9 2 1.124902 0.446652 0.834891 11.00000 -1.20000 AFIX 0 C1 1 0.440146 0.770855 0.575722 11.00000 0.02678 0.02304 = 0.02462 -0.00273 0.00320 0.00892 C2 1 0.344890 0.703015 0.514855 11.00000 0.03801 0.03153 = 0.02783 -0.00085 -0.01718 0.01721 AFIX 43 H2A 2 0.300145 0.734560 0.488433 11.00000 -1.20000 AFIX 0 C3 1 0.315409 0.590181 0.492877 11.00000 0.03031 0.03567 = 0.02053 -0.00307 -0.01100 0.01152 AFIX 43 H3A 2 0.248632 0.542632 0.452880 11.00000 -1.20000 AFIX 0 C4 1 0.384969 0.547356 0.530196 11.00000 0.03279 0.01922 = 0.03929 0.00316 0.00517 0.00538 AFIX 43 H4A 2 0.366829 0.469916 0.515969 11.00000 -1.20000 AFIX 0 C5 1 0.479716 0.617751 0.587557 11.00000 0.02360 0.02770 = 0.02764 0.00131 -0.00054 0.01567 AFIX 43 H5A 2 0.528053 0.587830 0.611617 11.00000 -1.20000 AFIX 0 C6 1 0.572374 0.942075 0.670879 11.00000 0.01379 0.02325 = 0.02353 0.00105 -0.00296 0.00576 C7 1 0.473098 0.889636 0.608389 11.00000 0.03001 0.02692 = 0.02474 0.00674 0.00474 0.01838 C8 1 0.414382 0.949239 0.579959 11.00000 0.02922 0.04171 = 0.02778 0.00611 -0.00410 0.01677 AFIX 43 H8A 2 0.348437 0.912496 0.537570 11.00000 -1.20000 AFIX 0 C9 1 0.451590 1.061087 0.613065 11.00000 0.03179 0.03249 = 0.04971 0.00516 -0.00807 0.02094 AFIX 43 H9A 2 0.411509 1.101461 0.593643 11.00000 -1.20000 AFIX 0 C10 1 0.546847 1.113673 0.674221 11.00000 0.03283 0.02369 = 0.04981 0.00701 0.00685 0.01534 AFIX 43 H10A 2 0.572061 1.190610 0.697254 11.00000 -1.20000 AFIX 0 C11 1 0.607251 1.056046 0.703119 11.00000 0.02370 0.02532 = 0.03050 -0.00158 -0.00161 0.00741 AFIX 43 H11A 2 0.673201 1.094495 0.745377 11.00000 -1.20000 AFIX 0 C12 1 0.819196 0.804933 0.583889 11.00000 0.01843 0.01887 = 0.02387 -0.00036 -0.00200 0.00295 C13 1 0.882892 0.810550 0.513492 11.00000 0.02949 0.03819 = 0.03528 0.00832 0.00743 0.02032 AFIX 43 H13A 2 0.925281 0.766011 0.503521 11.00000 -1.20000 AFIX 0 C14 1 0.883882 0.881513 0.458259 11.00000 0.03342 0.03907 = 0.02733 0.00866 0.00734 0.01904 AFIX 43 H14A 2 0.924702 0.884011 0.409179 11.00000 -1.20000 AFIX 0 C15 1 0.825183 0.948799 0.474812 11.00000 0.03133 0.03099 = 0.02736 0.01568 0.01088 0.01327 AFIX 43 H15A 2 0.827595 1.000533 0.439115 11.00000 -1.20000 AFIX 0 C16 1 0.763410 0.937920 0.544717 11.00000 0.03638 0.03183 = 0.02916 0.01275 -0.00014 0.01958 AFIX 43 H16A 2 0.721920 0.983124 0.555594 11.00000 -1.20000 AFIX 0 C17 1 0.728489 0.728836 0.708522 11.00000 0.01576 0.01996 = 0.02193 0.00085 -0.00787 0.00651 C18 1 0.809604 0.731723 0.647488 11.00000 0.01778 0.02326 = 0.02060 0.01079 -0.00001 0.01028 C19 1 0.875495 0.668959 0.646902 11.00000 0.02176 0.02217 = 0.01937 0.00370 0.00391 0.00927 AFIX 43 H19A 2 0.930959 0.675161 0.606005 11.00000 -1.20000 AFIX 0 C20 1 0.861199 0.597085 0.705546 11.00000 0.02071 0.02534 = 0.02163 -0.00033 -0.00396 0.00986 C21 1 0.777954 0.591719 0.763767 11.00000 0.03054 0.02609 = 0.02237 0.00878 0.00279 0.01490 AFIX 43 H21A 2 0.763790 0.541936 0.803355 11.00000 -1.20000 AFIX 0 C22 1 0.715748 0.656112 0.765729 11.00000 0.02112 0.02999 = 0.03080 0.00770 0.00862 0.01253 AFIX 43 H22A 2 0.662029 0.650756 0.807732 11.00000 -1.20000 AFIX 0 C23 1 0.925728 0.523539 0.701397 11.00000 0.02715 0.02627 = 0.02317 0.00363 0.00224 0.01614 C24 1 0.843163 0.391314 0.698772 11.00000 0.05217 0.02602 = 0.05027 0.00262 -0.00862 0.01992 H24A 2 0.742999 0.356768 0.700882 11.00000 -1.20000 C25 1 0.744897 0.952570 0.866777 11.00000 0.02156 0.02618 = 0.02083 0.00035 0.00240 0.01369 C26 1 0.825377 1.029262 0.931303 11.00000 0.02656 0.03640 = 0.02124 -0.00163 -0.00256 0.00826 AFIX 43 H26A 2 0.800966 1.025075 0.986242 11.00000 -1.20000 AFIX 0 C27 1 0.939937 1.112331 0.921212 11.00000 0.02710 0.02235 = 0.02804 0.00294 -0.00070 0.00624 C28 1 0.968065 1.113008 0.838144 11.00000 0.01565 0.02394 = 0.03793 0.00002 0.00012 0.00002 AFIX 43 H28A 2 1.044334 1.168089 0.825814 11.00000 -1.20000 AFIX 0 C29 1 0.888019 1.036093 0.774685 11.00000 0.02151 0.02687 = 0.02216 0.00620 -0.00170 0.00427 AFIX 43 H29A 2 0.911114 1.039235 0.719386 11.00000 -1.20000 AFIX 0 C30 1 0.623926 0.862306 0.874525 11.00000 0.02147 0.02558 = 0.02222 -0.00290 -0.00144 0.00867 C31 1 0.575330 0.835840 0.948063 11.00000 0.02802 0.03823 = 0.02392 -0.00562 -0.00562 0.00527 AFIX 43 H31A 2 0.621181 0.879568 0.999082 11.00000 -1.20000 AFIX 0 C32 1 0.460357 0.746494 0.950468 11.00000 0.02909 0.04113 = 0.04135 0.00486 0.01162 0.01525 C33 1 0.397168 0.688572 0.872410 11.00000 0.01646 0.03560 = 0.03487 -0.00632 0.00303 -0.00315 AFIX 43 H33A 2 0.317783 0.627925 0.869542 11.00000 -1.20000 AFIX 0 C34 1 0.448377 0.718344 0.800825 11.00000 0.02159 0.03019 = 0.02551 0.00199 -0.00308 0.00840 AFIX 43 H34A 2 0.402299 0.677829 0.749153 11.00000 -1.20000 AFIX 0 C35 1 1.027845 1.199962 0.991453 11.00000 0.02530 0.03502 = 0.02486 -0.00932 -0.00889 0.00810 C36 1 1.001488 1.156257 1.074677 11.00000 0.04375 0.05094 = 0.03078 0.00499 -0.01855 -0.01096 AFIX 137 H36A 2 0.920494 1.146381 1.088127 11.00000 -1.50000 H36B 2 1.062718 1.210844 1.118752 11.00000 -1.50000 H36C 2 1.004362 1.083539 1.070483 11.00000 -1.50000 AFIX 0 C37 1 1.010767 1.306147 0.997299 11.00000 0.11092 0.03739 = 0.06398 -0.01256 -0.04121 0.02996 AFIX 137 H37A 2 0.930256 1.290757 1.015336 11.00000 -1.50000 H37B 2 1.017322 1.330395 0.942507 11.00000 -1.50000 H37C 2 1.073658 1.366084 1.037842 11.00000 -1.50000 AFIX 0 C38 1 1.158644 1.227121 0.975528 11.00000 0.02060 0.12386 = 0.07010 -0.00999 -0.00185 -0.00466 AFIX 137 H38A 2 1.181913 1.270778 0.929502 11.00000 -1.50000 H38B 2 1.165453 1.156607 0.960843 11.00000 -1.50000 H38C 2 1.212751 1.271459 1.025990 11.00000 -1.50000 AFIX 0 IR1 6 0.650933 0.838351 0.696996 11.00000 0.01871 0.02018 = 0.01939 0.00096 -0.00076 0.00936 N1 4 0.508319 0.727128 0.611841 11.00000 0.02956 0.02055 = 0.01428 0.00237 0.00330 0.01150 N2 4 0.757056 0.868169 0.599056 11.00000 0.02045 0.02066 = 0.02236 0.00045 0.00025 0.00991 N3 4 0.776665 0.955095 0.786868 11.00000 0.01775 0.02349 = 0.02580 0.00217 0.00108 0.01151 N4 4 0.560721 0.802033 0.799177 11.00000 0.01919 0.02358 = 0.02546 0.00347 -0.00107 0.01514 PART 1 C43A 1 0.257219 0.912472 0.759946 21.00000 0.09505 0.08798 = 0.07948 0.02128 0.03720 0.03431 AFIX 23 H43A 2 0.194652 0.833513 0.742151 21.00000 -1.20000 H43B 2 0.317577 0.930639 0.718267 21.00000 -1.20000 AFIX 0 CL1A 5 0.328523 0.922156 0.854540 21.00000 0.08752 0.08422 = 0.11061 0.00661 0.04097 0.02188 CL2A 5 0.188512 1.001462 0.760703 21.00000 0.11273 0.10103 = 0.07996 0.03513 0.03584 0.05241 PART 2 C43Z 1 0.281193 0.897884 0.762116 -21.00000 0.08152 0.06880 = 0.06760 0.01835 0.03878 0.03972 AFIX 23 H43C 2 0.265007 0.820543 0.736414 -21.00000 -1.20000 H43D 2 0.351950 0.951775 0.737402 -21.00000 -1.20000 AFIX 0 CL1Z 5 0.317933 0.914412 0.867084 -21.00000 0.05998 0.06205 = 0.05620 0.01084 0.01878 0.04011 CL2Z 5 0.155245 0.919189 0.737410 -21.00000 0.07972 0.11643 = 0.08442 0.04025 0.01757 0.01946 PART 3 C43B 1 0.339619 0.337845 0.700573 31.00000 0.05843 0.09403 = 0.07747 0.00489 0.01971 0.02723 AFIX 23 H43E 2 0.280321 0.354945 0.670397 31.00000 -1.20000 H43F 2 0.295958 0.258886 0.710835 31.00000 -1.20000 AFIX 0 CL1B 5 0.451412 0.345839 0.636156 31.00000 0.03037 0.03913 = 0.07309 0.01100 0.00699 0.02031 CL2B 5 0.386734 0.424926 0.795149 31.00000 0.08643 0.09035 = 0.08729 -0.00206 0.00047 0.05213 PART 4 C43Y 1 0.350621 0.348939 0.709288 51.00000 0.05667 0.09367 = 0.07532 0.00222 0.01943 0.02841 AFIX 23 H43G 2 0.377992 0.411383 0.757156 51.00000 -1.20000 H43H 2 0.291735 0.357601 0.671612 51.00000 -1.20000 AFIX 0 CL1Y 5 0.474487 0.360418 0.656426 51.00000 0.07096 0.08508 = 0.12032 0.03428 0.00973 0.03435 CL2Y 5 0.278054 0.222098 0.745543 51.00000 0.06140 0.11198 = 0.05998 0.03171 0.01010 0.03758 PART 5 C43 1 0.424289 0.404242 0.726783 61.00000 0.06486 0.09146 = 0.08126 0.01189 0.01307 0.02941 AFIX 23 H43I 2 0.418718 0.474292 0.719191 61.00000 -1.20000 H43J 2 0.506139 0.426554 0.754495 61.00000 -1.20000 AFIX 0 CL1 5 0.409322 0.326213 0.630009 61.00000 0.06657 0.09437 = 0.09977 0.00866 0.00285 0.03525 CL2 5 0.316585 0.333751 0.791230 61.00000 0.07210 0.10488 = 0.08805 0.03106 0.00744 0.03003 PART 6 C39A 1 0.404300 0.722001 1.032479 41.00000 0.04143 0.07645 = 0.03221 0.01196 0.01197 0.01077 C40A 1 0.498710 0.727727 1.098287 41.00000 0.05481 0.08621 = 0.05029 0.02721 0.00809 0.01562 AFIX 137 H40A 2 0.523108 0.667984 1.080944 41.00000 -1.50000 H40B 2 0.463564 0.717272 1.151775 41.00000 -1.50000 H40C 2 0.570094 0.801603 1.104405 41.00000 -1.50000 AFIX 0 C41A 1 0.294302 0.606783 1.020496 41.00000 0.05622 0.09069 = 0.03977 0.01972 0.03025 -0.00198 AFIX 137 H41A 2 0.320566 0.547677 1.006082 41.00000 -1.50000 H41B 2 0.236907 0.602183 0.975385 41.00000 -1.50000 H41C 2 0.254485 0.596175 1.072294 41.00000 -1.50000 AFIX 0 C42A 1 0.361514 0.812224 1.063684 41.00000 0.05680 0.09100 = 0.04646 0.00451 0.02283 0.01834 AFIX 137 H42A 2 0.298402 0.807563 1.023043 41.00000 -1.50000 H42B 2 0.430687 0.887576 1.070240 41.00000 -1.50000 H42C 2 0.328347 0.798688 1.117536 41.00000 -1.50000 PART 7 AFIX 0 C39Z 1 0.408022 0.703105 1.029227 -41.00000 0.04877 0.07803 = 0.03313 0.01499 0.01372 0.00423 C40Z 1 0.495050 0.773154 1.106624 -41.00000 0.06200 0.08076 = 0.04465 0.01758 0.01840 0.00035 AFIX 137 H40D 2 0.573758 0.772162 1.100986 -41.00000 -1.50000 H40E 2 0.460893 0.740986 1.156203 -41.00000 -1.50000 H40F 2 0.506307 0.851232 1.112314 -41.00000 -1.50000 AFIX 0 C41Z 1 0.382678 0.579682 1.026464 -41.00000 0.06064 0.07467 = 0.05198 0.01999 0.01434 0.00972 AFIX 137 H41D 2 0.459906 0.574831 1.029678 -41.00000 -1.50000 H41E 2 0.334072 0.534794 0.974174 -41.00000 -1.50000 H41F 2 0.337818 0.550358 1.073769 -41.00000 -1.50000 AFIX 0 C42Z 1 0.287671 0.710713 1.037401 -41.00000 0.05489 0.09045 = 0.04774 0.01825 0.02218 0.01096 AFIX 137 H42D 2 0.225058 0.652979 0.995514 -41.00000 -1.50000 H42E 2 0.298942 0.785792 1.028596 -41.00000 -1.50000 H42F 2 0.262168 0.698224 1.093313 -41.00000 -1.50000 PART 0 AFIX 0 HKLF 4 REM 1 in P-1 REM R1 = 0.0537 for 6891 Fo > 4sig(Fo) and 0.0811 for all 8747 data REM 705 parameters refined using 561 restraints END WGHT 0.0251 17.4289 REM Highest difference peak 0.811, deepest hole -1.066, 1-sigma level 0.175 Q1 1 1.2574 0.4752 0.8689 11.00000 0.05 0.81 Q2 1 0.6764 0.9128 0.6757 11.00000 0.05 0.77 Q3 1 0.5312 1.2219 0.6368 11.00000 0.05 0.76 Q4 1 0.9165 0.1899 0.7569 11.00000 0.05 0.74 Q5 1 0.4469 0.5431 0.9999 11.00000 0.05 0.73 Q6 1 0.1357 0.4871 0.9308 11.00000 0.05 0.71 Q7 1 0.9764 1.1472 0.7112 11.00000 0.05 0.69 Q8 1 0.4810 0.4073 0.7145 11.00000 0.05 0.67 Q9 1 0.8328 0.9603 0.9866 11.00000 0.05 0.66 Q10 1 0.9089 1.0286 0.4629 11.00000 0.05 0.65 Q11 1 1.1937 0.4387 0.5440 11.00000 0.05 0.64 Q12 1 0.8629 0.8237 0.7458 11.00000 0.05 0.63 Q13 1 0.0556 0.9900 0.7992 11.00000 0.05 0.63 Q14 1 1.1983 0.7789 0.5831 11.00000 0.05 0.63 Q15 1 0.5159 0.7775 0.6644 11.00000 0.05 0.63 Q16 1 0.4168 0.6759 0.7135 11.00000 0.05 0.63 Q17 1 0.4430 0.8603 0.7373 11.00000 0.05 0.63 Q18 1 0.9220 0.2456 0.6024 11.00000 0.05 0.63 Q19 1 1.2634 0.4517 0.6684 11.00000 0.05 0.62 Q20 1 0.7430 0.9564 0.7087 11.00000 0.05 0.62 ; _shelx_res_checksum 85233 _shelx_hkl_file ; -1 0 0 0.01 0.12 -1 0 0 0.01 0.11 1 0 0 122.29 2.30 1 0 0 122.87 2.00 -2 0 0 0.02 0.88 -2 0 0 1.22 0.41 -2 0 0 1.48 0.35 -2 0 0 1.22 0.36 -2 0 0 1.49 0.41 2 0 0 2.33 0.92 2 0 0 2.09 0.41 2 0 0 2.08 0.46 -3 0 0 69.86 1.60 -3 0 0 69.55 1.84 -3 0 0 67.18 3.51 3 0 0 69.60 2.12 3 0 0 68.45 1.86 3 0 0 69.83 3.12 -4 0 0 84.77 2.25 -4 0 0 84.62 1.96 -4 0 0 86.16 4.40 4 0 0 85.50 3.83 4 0 0 85.92 2.58 4 0 0 84.68 2.27 -5 0 0 -0.90 1.33 -5 0 0 -1.72 0.45 -5 0 0 -1.74 0.52 5 0 0 0.48 0.62 5 0 0 0.23 1.39 5 0 0 0.47 0.54 -6 0 0 45.17 4.40 -6 0 0 43.78 1.50 -6 0 0 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56.76 5.84 2 9 0 41.73 5.37 2 9 0 50.85 4.16 2 9 0 57.75 5.11 -3 -9 0 21.00 2.98 -3 -9 0 6.27 3.32 3 9 0 20.57 3.93 3 9 0 15.30 4.22 3 9 0 22.12 3.59 -4 -9 0 5.14 3.73 4 9 0 2.58 2.92 4 9 0 3.15 2.94 -5 -9 0 -5.94 2.73 5 9 0 0.52 2.99 5 9 0 3.68 3.54 -6 -9 0 29.52 5.67 6 9 0 20.13 5.03 -7 -9 0 3.13 4.14 7 9 0 7.55 4.33 -14 10 0 0.96 3.76 -13 10 0 16.08 5.01 -12 10 0 36.24 6.10 -11 10 0 0.18 2.97 -11 10 0 2.79 1.69 -11 10 0 2.16 2.01 -10 10 0 35.99 3.18 -10 10 0 33.24 5.51 -10 10 0 36.72 3.72 -9 10 0 31.42 3.06 -9 10 0 31.04 3.52 -9 10 0 25.76 3.95 -9 10 0 21.55 4.61 -8 10 0 13.15 2.58 -8 10 0 11.14 3.11 -8 10 0 12.57 2.19 7 -10 0 8.88 3.38 -7 10 0 12.44 2.14 -7 10 0 12.44 3.01 -7 10 0 12.43 2.51 6 -10 0 25.27 4.44 -6 10 0 13.92 2.53 -6 10 0 20.52 3.64 -6 10 0 19.53 3.20 5 -10 0 6.05 3.37 -5 10 0 11.19 2.36 -5 10 0 6.02 2.54 -5 10 0 5.33 2.16 4 -10 0 -3.16 2.06 -4 10 0 2.95 1.77 -4 10 0 0.04 2.07 -4 10 0 2.60 2.26 3 -10 0 62.28 6.44 -3 10 0 59.93 4.36 -3 10 0 63.28 5.95 -3 10 0 66.16 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54.05 2.01 2 4 -4 50.48 3.20 2 4 -4 53.54 3.80 2 4 -4 50.77 3.62 2 4 -4 54.14 2.30 -2 -4 4 49.77 3.88 1 4 -4 2.64 0.81 1 4 -4 3.98 1.67 1 4 -4 6.02 1.81 1 4 -4 3.99 1.45 1 4 -4 2.65 0.93 -1 -4 4 3.63 1.90 0 4 -4 92.93 4.16 0 4 -4 91.92 3.21 0 4 -4 94.11 4.52 0 4 -4 94.33 4.01 0 4 -4 92.30 2.80 0 -4 4 95.40 4.90 -1 4 -4 74.08 3.84 -1 4 -4 67.14 2.80 -1 4 -4 67.09 2.43 -1 4 -4 67.55 3.17 -1 4 -4 75.15 3.43 1 -4 4 75.58 4.19 -2 4 -4 -0.40 0.92 -2 4 -4 0.21 0.84 -2 4 -4 3.15 1.27 -2 4 -4 -0.37 1.06 -2 4 -4 3.12 1.44 2 -4 4 0.24 1.45 -3 4 -4 145.49 3.89 -3 4 -4 139.05 5.89 -3 4 -4 146.35 4.65 -3 4 -4 145.63 5.25 -3 4 -4 144.55 3.92 -3 4 -4 144.48 4.52 -4 4 -4 139.31 4.38 -4 4 -4 148.92 4.04 -4 4 -4 150.02 4.67 -4 4 -4 140.07 5.00 -4 4 -4 147.48 6.28 -5 4 -4 43.59 3.58 -5 4 -4 40.02 2.45 -5 4 -4 41.72 2.51 -5 4 -4 41.97 2.90 -5 4 -4 39.73 2.18 -6 4 -4 19.92 1.59 -6 4 -4 20.29 1.84 -6 4 -4 22.56 1.98 -6 4 -4 27.39 3.48 -6 4 -4 22.52 2.27 6 -4 4 23.77 1.08 -7 4 -4 118.35 4.49 -7 4 -4 119.68 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4.52 1 2 -7 198.62 7.39 1 2 -7 189.96 6.53 1 2 -7 189.29 7.38 1 2 -7 204.39 4.80 1 2 -7 203.63 5.51 -1 -2 7 188.40 6.38 0 2 -7 8.32 1.84 0 2 -7 10.31 1.64 0 2 -7 11.97 2.10 0 2 -7 10.26 1.42 0 2 -7 8.52 2.13 0 -2 7 9.91 1.64 -1 2 -7 5.02 1.54 -1 2 -7 5.16 1.77 -1 2 -7 1.44 1.33 -1 2 -7 1.45 1.14 1 -2 7 3.58 1.20 -2 2 -7 106.33 4.21 -2 2 -7 104.21 3.60 -2 2 -7 105.08 4.33 -2 2 -7 109.72 5.02 -2 2 -7 110.27 4.46 2 -2 7 99.51 4.19 -3 2 -7 17.54 2.38 -3 2 -7 14.62 2.10 -3 2 -7 17.30 2.06 -3 2 -7 17.72 2.31 -3 2 -7 17.82 2.02 3 -2 7 18.83 2.13 -4 2 -7 0.94 1.16 -4 2 -7 -0.03 1.36 -4 2 -7 5.72 1.44 -4 2 -7 1.06 1.34 -4 2 -7 6.99 1.84 4 -2 7 1.26 1.19 -5 2 -7 120.97 4.96 -5 2 -7 128.91 4.97 -5 2 -7 129.45 4.33 -5 2 -7 121.84 4.40 -5 2 -7 125.74 5.95 5 -2 7 135.47 5.23 -6 2 -7 28.85 3.60 -6 2 -7 38.45 2.98 -6 2 -7 30.11 2.70 -6 2 -7 38.71 3.45 -6 2 -7 30.01 2.34 6 -2 7 33.39 2.76 -7 2 -7 2.24 1.85 -7 2 -7 2.24 1.59 -7 2 -7 0.49 1.89 -8 2 -7 32.48 2.85 -8 2 -7 40.74 5.06 -8 2 -7 32.39 3.29 -9 2 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2.09 1 5 -9 68.68 2.99 1 5 -9 69.95 6.03 1 5 -9 69.23 5.26 1 5 -9 68.99 3.45 1 5 -9 66.65 4.70 -1 -5 9 74.29 5.19 0 5 -9 81.92 3.38 0 5 -9 73.27 4.71 0 5 -9 81.43 3.88 0 5 -9 72.40 5.28 0 5 -9 90.74 5.11 0 -5 9 84.27 5.26 -1 5 -9 1.04 1.21 -1 5 -9 0.81 1.88 -1 5 -9 1.06 1.40 -1 5 -9 0.76 1.63 -1 5 -9 0.32 1.59 1 -5 9 -0.60 1.69 -2 5 -9 14.75 2.40 -2 5 -9 16.93 2.43 -2 5 -9 14.38 2.96 -2 5 -9 14.37 1.96 -2 5 -9 14.39 2.59 2 -5 9 11.79 2.44 -3 5 -9 47.33 3.08 -3 5 -9 40.91 3.02 -3 5 -9 52.48 4.89 -3 5 -9 51.41 4.24 -3 5 -9 40.62 3.47 3 -5 9 43.99 4.22 -4 5 -9 23.39 2.84 -4 5 -9 28.97 3.72 -4 5 -9 23.25 2.45 -4 5 -9 29.03 3.26 -5 5 -9 13.49 2.10 -5 5 -9 13.64 2.46 -5 5 -9 24.19 3.45 -5 5 -9 20.09 3.01 -5 5 -9 19.86 2.64 -6 5 -9 67.11 5.25 -6 5 -9 75.52 4.61 -6 5 -9 57.86 3.83 -6 5 -9 76.19 4.10 -6 5 -9 57.78 4.40 -7 5 -9 61.55 4.05 -7 5 -9 62.18 4.71 -7 5 -9 51.24 5.52 -8 5 -9 3.17 2.66 -8 5 -9 1.72 1.57 -8 5 -9 3.61 2.15 -9 5 -9 18.49 2.67 -9 5 -9 18.68 3.08 -9 5 -9 28.26 4.49 -10 5 -9 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2.43 -1 4 -9 19.44 3.27 -1 4 -9 19.28 2.86 1 -4 9 20.92 2.83 -2 4 -9 0.84 1.22 -2 4 -9 1.59 1.54 -2 4 -9 0.88 1.41 -2 4 -9 0.86 1.48 -2 4 -9 1.58 1.75 2 -4 9 0.28 1.54 -3 4 -9 29.99 3.02 -3 4 -9 27.30 3.47 -3 4 -9 27.44 3.05 -3 4 -9 29.77 2.60 -3 4 -9 32.02 2.88 3 -4 9 28.34 3.20 -4 4 -9 47.02 4.35 -4 4 -9 40.37 3.61 -4 4 -9 46.04 3.77 -4 4 -9 40.21 3.12 -4 4 -9 44.49 2.69 -4 4 -9 39.35 3.85 -5 4 -9 25.85 2.85 -5 4 -9 26.22 3.27 -5 4 -9 23.53 2.65 -5 4 -9 19.90 3.20 -5 4 -9 21.76 3.10 -6 4 -9 44.77 4.73 -6 4 -9 40.05 3.27 -6 4 -9 41.00 3.74 -6 4 -9 40.69 3.76 -6 4 -9 40.55 3.25 -7 4 -9 44.70 4.09 -7 4 -9 49.75 5.11 -7 4 -9 44.17 3.50 -8 4 -9 28.22 4.37 -8 4 -9 27.33 3.46 -8 4 -9 26.91 2.86 -9 4 -9 -0.77 2.09 -9 4 -9 3.86 2.88 -9 4 -9 -0.75 1.78 -10 4 -9 37.93 3.59 -10 4 -9 43.74 5.80 -10 4 -9 38.19 4.19 -11 4 -9 20.89 4.62 -12 4 -9 4.11 3.56 11 3 -9 16.53 5.14 -11 -3 9 19.59 5.31 10 3 -9 -0.22 3.36 -10 -3 9 3.03 3.56 9 3 -9 7.37 3.63 -9 -3 9 21.64 4.76 8 3 -9 28.60 3.80 8 3 -9 28.66 4.35 8 3 -9 23.25 4.58 -8 -3 9 36.61 5.43 7 3 -9 7.42 2.57 7 3 -9 4.43 3.18 7 3 -9 7.54 2.94 -7 -3 9 9.26 3.23 6 3 -9 7.14 2.87 6 3 -9 4.84 2.85 6 3 -9 6.94 2.49 -6 -3 9 3.67 2.50 5 3 -9 34.46 3.86 5 3 -9 31.38 4.61 5 3 -9 35.20 4.48 -5 -3 9 26.92 4.05 4 3 -9 52.50 5.44 4 3 -9 43.84 2.47 4 3 -9 43.77 2.15 4 3 -9 50.66 5.24 4 3 -9 49.45 4.51 -4 -3 9 49.83 4.73 3 3 -9 26.53 3.83 3 3 -9 27.81 1.99 3 3 -9 25.82 3.30 3 3 -9 25.79 3.90 3 3 -9 28.13 2.34 -3 -3 9 27.96 3.40 2 3 -9 84.74 4.84 2 3 -9 84.20 3.10 2 3 -9 85.03 5.32 2 3 -9 84.47 3.58 2 3 -9 84.70 5.47 -2 -3 9 86.09 4.77 1 3 -9 51.21 3.05 1 3 -9 51.34 2.66 1 3 -9 47.97 4.60 1 3 -9 52.41 4.01 1 3 -9 47.20 4.01 -1 -3 9 56.52 3.60 0 3 -9 30.08 2.36 0 3 -9 30.42 2.74 0 3 -9 37.01 4.05 0 3 -9 35.80 3.47 0 3 -9 31.34 3.59 0 -3 9 36.56 3.05 -1 3 -9 50.92 3.62 -1 3 -9 52.24 4.68 -1 3 -9 51.09 4.06 -1 3 -9 50.69 3.13 -1 3 -9 51.46 3.56 1 -3 9 50.12 3.34 -2 3 -9 39.19 3.61 -2 3 -9 37.91 2.88 -2 3 -9 38.83 4.00 -2 3 -9 37.84 3.30 -2 3 -9 35.87 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-6 4 -10 103.60 4.67 -6 4 -10 121.04 6.70 -6 4 -10 103.23 5.37 -6 4 -10 119.31 5.86 -6 4 -10 120.19 5.21 -7 4 -10 14.79 3.36 -7 4 -10 27.01 3.45 -7 4 -10 27.50 3.03 -8 4 -10 4.00 2.11 -8 4 -10 1.63 2.38 -8 4 -10 4.11 2.46 -9 4 -10 45.39 3.83 -9 4 -10 45.19 4.41 -9 4 -10 40.70 5.28 -10 4 -10 12.52 3.73 -10 4 -10 9.77 2.89 -10 4 -10 10.06 2.49 -11 4 -10 2.37 3.16 -12 4 -10 12.48 4.47 10 3 -10 22.33 5.45 -10 -3 10 20.72 5.22 9 3 -10 5.09 3.41 -9 -3 10 19.89 4.56 8 3 -10 0.78 2.84 8 3 -10 -1.42 2.64 8 3 -10 0.73 2.49 -8 -3 10 -2.99 2.87 7 3 -10 10.46 3.16 7 3 -10 9.55 3.36 7 3 -10 10.58 3.64 -7 -3 10 13.82 3.60 6 3 -10 53.51 5.02 6 3 -10 54.85 5.82 6 3 -10 47.40 5.76 -6 -3 10 48.73 5.32 5 3 -10 11.86 3.49 5 3 -10 14.82 3.46 5 3 -10 14.37 2.98 -5 -3 10 9.95 2.98 4 3 -10 22.86 1.96 4 3 -10 23.69 3.40 4 3 -10 23.39 2.30 4 3 -10 24.30 3.95 4 3 -10 26.92 4.34 -4 -3 10 21.61 3.35 3 3 -10 29.86 4.26 3 3 -10 28.90 3.66 3 3 -10 33.75 4.45 3 3 -10 27.30 2.14 3 3 -10 28.23 2.54 -3 -3 10 30.73 3.55 2 3 -10 14.89 3.24 2 3 -10 11.38 1.99 2 3 -10 12.46 2.68 2 3 -10 11.32 1.71 2 3 -10 12.92 3.11 -2 -3 10 13.89 2.47 1 3 -10 4.30 2.17 1 3 -10 4.31 1.90 1 3 -10 2.26 1.30 1 3 -10 2.26 1.51 1 3 -10 0.36 1.99 -1 -3 10 -0.22 1.21 0 3 -10 69.13 5.71 0 3 -10 67.97 4.95 0 3 -10 54.90 3.35 0 3 -10 53.66 4.04 0 3 -10 54.86 2.90 0 -3 10 55.65 3.59 -1 3 -10 26.88 3.25 -1 3 -10 32.75 2.72 -1 3 -10 32.96 3.14 -1 3 -10 32.26 3.52 -1 3 -10 33.03 4.06 1 -3 10 32.39 3.03 -2 3 -10 -0.57 1.28 -2 3 -10 -2.94 1.34 -2 3 -10 -2.93 1.21 -2 3 -10 1.35 1.61 -2 3 -10 -0.53 1.48 2 -3 10 -0.03 1.21 -3 3 -10 27.09 3.61 -3 3 -10 26.70 3.25 -3 3 -10 28.27 2.80 -3 3 -10 28.53 3.24 -4 3 -10 85.15 4.64 -4 3 -10 89.86 4.68 -4 3 -10 83.10 4.76 -4 3 -10 85.67 4.05 -4 3 -10 89.13 5.26 4 -3 10 100.60 4.80 -5 3 -10 4.23 1.88 -5 3 -10 10.39 2.41 -5 3 -10 8.70 2.46 -5 3 -10 10.25 2.08 -5 3 -10 4.20 2.13 -6 3 -10 4.77 1.85 -6 3 -10 3.14 2.20 -6 3 -10 4.76 2.14 -7 3 -10 60.85 5.80 -7 3 -10 60.88 4.14 -7 3 -10 60.97 4.80 -8 3 -10 10.22 2.27 -8 3 -10 8.16 2.98 -8 3 -10 10.12 2.61 -9 3 -10 10.02 2.70 -9 3 -10 10.14 2.35 -9 3 -10 10.32 3.21 -10 3 -10 26.72 3.82 -10 3 -10 27.39 4.73 -10 3 -10 27.07 3.34 -11 3 -10 24.42 4.77 11 2 -10 6.08 3.96 -11 -2 10 3.92 4.20 10 2 -10 -1.84 3.04 -10 -2 10 2.75 3.35 9 2 -10 30.37 5.36 -9 -2 10 20.11 4.43 8 2 -10 25.31 4.34 8 2 -10 16.62 4.27 8 2 -10 24.90 3.76 -8 -2 10 19.41 4.06 7 2 -10 3.66 2.96 7 2 -10 8.38 2.57 7 2 -10 8.63 2.98 -7 -2 10 7.04 2.89 6 2 -10 26.34 3.66 6 2 -10 26.52 4.18 6 2 -10 28.57 4.72 -6 -2 10 30.67 4.37 5 2 -10 56.62 5.63 5 2 -10 54.97 4.83 5 2 -10 65.20 6.45 -5 -2 10 57.73 4.60 4 2 -10 23.03 4.39 4 2 -10 25.49 4.05 4 2 -10 30.68 2.55 4 2 -10 24.87 3.48 4 2 -10 30.80 2.22 -4 -2 10 29.13 3.47 3 2 -10 -0.26 1.26 3 2 -10 -0.28 1.08 3 2 -10 0.04 1.87 3 2 -10 0.03 1.62 3 2 -10 -0.99 2.04 -3 -2 10 0.29 1.40 2 2 -10 63.93 5.00 2 2 -10 64.70 3.34 2 2 -10 65.33 4.93 2 2 -10 64.54 2.90 2 2 -10 67.47 5.75 1 2 -10 52.17 4.80 1 2 -10 47.11 3.05 1 2 -10 33.03 4.16 1 2 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28.08 5.08 -1 5 -18 35.89 4.03 -1 5 -18 27.43 5.64 -2 5 -18 9.92 3.39 -2 5 -18 10.21 4.55 -2 5 -18 10.64 3.95 -2 5 -18 11.46 3.01 -3 5 -18 3.77 3.67 -3 5 -18 3.58 3.32 -3 5 -18 3.17 2.39 -3 5 -18 2.60 2.99 -4 5 -18 13.74 3.70 -4 5 -18 11.56 3.75 -4 5 -18 14.97 3.55 -4 5 -18 11.22 4.15 -5 5 -18 11.64 3.45 -5 5 -18 10.78 3.93 4 4 -18 5.56 3.67 4 4 -18 5.48 4.06 4 4 -18 15.00 4.90 3 4 -18 1.92 3.41 3 4 -18 2.07 3.73 3 4 -18 0.31 3.29 2 4 -18 19.51 4.67 2 4 -18 18.71 5.12 2 4 -18 11.27 4.47 1 4 -18 19.74 4.59 1 4 -18 18.50 5.05 1 4 -18 26.67 4.05 1 4 -18 27.32 3.54 0 4 -18 0.13 2.33 0 4 -18 6.70 3.87 0 4 -18 7.34 3.54 0 4 -18 -0.47 2.70 -1 4 -18 8.78 3.90 -1 4 -18 8.27 4.27 -1 4 -18 17.83 3.42 -1 4 -18 17.79 3.97 -2 4 -18 18.28 4.73 -2 4 -18 18.84 4.26 -2 4 -18 22.93 4.01 -2 4 -18 25.27 3.65 -3 4 -18 9.31 3.01 -3 4 -18 8.70 4.34 -3 4 -18 7.98 3.16 -3 4 -18 9.24 3.97 -4 4 -18 4.72 3.47 -4 4 -18 5.18 3.19 -4 4 -18 -0.95 2.65 -4 4 -18 -0.11 2.69 -5 4 -18 26.79 3.98 -5 4 -18 25.87 4.46 5 3 -18 -1.51 3.52 5 3 -18 -1.58 3.48 5 3 -18 -2.11 3.08 4 3 -18 17.81 5.14 4 3 -18 14.60 4.58 4 3 -18 14.35 5.10 3 3 -18 20.94 5.43 3 3 -18 21.76 4.89 2 3 -18 -0.74 2.74 2 3 -18 7.87 4.22 2 3 -18 -1.17 2.04 2 3 -18 -1.13 2.39 2 3 -18 8.50 3.89 1 3 -18 12.35 2.76 1 3 -18 12.44 3.19 1 3 -18 18.22 4.97 1 3 -18 16.99 4.41 1 3 -18 16.82 4.92 0 3 -18 19.81 4.60 0 3 -18 30.99 3.75 0 3 -18 30.31 4.47 0 3 -18 18.96 5.06 -1 3 -18 2.85 3.14 -1 3 -18 3.78 2.42 -1 3 -18 2.54 3.41 -1 3 -18 3.75 2.78 -2 3 -18 7.61 3.40 -2 3 -18 8.86 3.73 -2 3 -18 7.48 2.92 -2 3 -18 8.69 4.11 -3 3 -18 18.20 4.17 -3 3 -18 20.66 4.66 -3 3 -18 21.58 4.24 -3 3 -18 18.15 3.62 -4 3 -18 16.02 4.63 -4 3 -18 16.25 4.18 -4 3 -18 10.83 3.11 -4 3 -18 10.76 3.59 5 2 -18 2.35 3.68 5 2 -18 6.43 4.30 5 2 -18 2.54 3.31 4 2 -18 -6.20 2.95 4 2 -18 -6.64 2.66 4 2 -18 0.38 3.49 3 2 -18 25.54 5.84 3 2 -18 17.26 4.74 3 2 -18 26.83 4.95 2 2 -18 19.33 5.06 2 2 -18 21.83 3.92 2 2 -18 19.70 4.51 2 2 -18 20.46 4.93 2 2 -18 21.64 3.38 1 2 -18 0.25 2.45 1 2 -18 0.14 2.11 1 2 -18 1.96 3.54 1 2 -18 2.57 3.16 1 2 -18 1.71 3.23 0 2 -18 10.98 3.71 0 2 -18 0.34 2.50 0 2 -18 0.17 2.14 0 2 -18 10.52 4.03 -1 2 -18 25.94 3.57 -1 2 -18 21.95 5.24 -1 2 -18 27.03 4.38 -1 2 -18 23.10 4.74 -2 2 -18 -4.10 2.51 -2 2 -18 1.53 2.92 -2 2 -18 -3.58 2.37 -2 2 -18 1.92 2.54 -3 2 -18 1.75 2.43 -3 2 -18 1.79 2.79 -3 2 -18 1.84 3.01 -3 2 -18 2.10 3.28 -4 2 -18 17.50 3.88 -4 2 -18 16.96 3.32 6 1 -18 -0.20 3.66 6 1 -18 1.55 3.89 6 1 -18 1.35 3.38 5 1 -18 20.89 4.74 5 1 -18 22.99 5.75 5 1 -18 20.91 5.40 4 1 -18 0.42 3.20 4 1 -18 21.33 5.64 4 1 -18 0.47 3.52 3 1 -18 1.31 3.21 3 1 -18 0.32 1.95 3 1 -18 -0.80 2.49 3 1 -18 2.84 3.26 3 1 -18 2.83 3.56 2 1 -18 22.11 5.18 2 1 -18 1.16 2.65 2 1 -18 0.88 2.27 2 1 -18 14.40 4.42 2 1 -18 23.87 4.73 1 1 -18 25.21 5.51 1 1 -18 26.37 4.99 1 1 -18 24.42 3.41 1 1 -18 18.71 4.65 1 1 -18 25.00 3.99 0 1 -18 4.29 2.42 0 1 -18 4.01 2.76 0 1 -18 -1.52 2.73 0 1 -18 -1.94 2.89 0 1 -18 -1.13 2.51 -1 1 -18 9.68 3.62 -1 1 -18 8.94 3.96 -1 1 -18 7.24 3.38 -1 1 -18 7.13 2.90 -2 1 -18 16.66 4.84 -2 1 -18 17.33 4.40 -2 1 -18 15.57 3.20 -2 1 -18 15.67 3.70 -3 1 -18 2.94 3.03 -3 1 -18 2.95 2.62 -3 1 -18 -2.19 2.64 -3 1 -18 -1.82 2.91 -4 1 -18 0.07 2.31 -4 1 -18 0.14 2.68 6 0 -18 3.51 4.38 6 0 -18 5.43 4.43 6 0 -18 3.41 3.85 5 0 -18 2.24 3.75 5 0 -18 1.79 3.35 5 0 -18 2.90 3.89 4 0 -18 26.96 5.61 4 0 -18 20.11 4.73 4 0 -18 19.09 5.25 3 0 -18 17.47 3.03 3 0 -18 19.74 4.71 3 0 -18 19.43 4.86 3 0 -18 20.09 5.30 3 0 -18 18.33 3.69 2 0 -18 5.61 3.80 2 0 -18 0.46 3.32 2 0 -18 0.43 2.75 2 0 -18 0.14 3.63 2 0 -18 -0.21 2.03 1 0 -18 19.26 4.46 1 0 -18 23.87 5.18 1 0 -18 18.53 3.12 1 0 -18 18.72 3.62 1 0 -18 18.18 4.91 0 0 -18 52.88 6.49 0 0 -18 52.37 7.30 0 0 -18 33.88 3.92 0 0 -18 34.00 4.54 -1 0 -18 -5.42 2.16 -1 0 -18 4.54 3.61 -1 0 -18 4.58 3.28 -1 0 -18 -5.13 1.87 -2 0 -18 9.14 3.39 -2 0 -18 4.89 3.30 -2 0 -18 4.76 3.59 -2 0 -18 9.03 2.91 -3 0 -18 12.41 3.85 -3 0 -18 12.46 4.27 -3 0 -18 7.01 3.26 -3 0 -18 7.22 2.85 6 -1 -18 12.36 4.26 6 -1 -18 13.10 4.93 6 -1 -18 13.07 5.29 5 -1 -18 21.84 5.51 5 -1 -18 20.18 4.49 5 -1 -18 19.01 4.95 4 -1 -18 -6.25 3.35 4 -1 -18 -6.39 3.12 4 -1 -18 2.31 3.60 3 -1 -18 26.00 4.05 3 -1 -18 25.34 3.49 3 -1 -18 7.12 3.67 3 -1 -18 11.80 4.83 3 -1 -18 6.62 4.06 2 -1 -18 27.90 4.43 2 -1 -18 20.87 5.26 2 -1 -18 25.62 5.18 2 -1 -18 27.42 3.80 2 -1 -18 21.77 4.75 1 -1 -18 1.37 3.47 1 -1 -18 -4.21 1.77 1 -1 -18 -4.56 2.08 1 -1 -18 1.31 3.21 -1 1 18 1.22 3.55 0 -1 -18 5.48 3.75 0 -1 -18 11.20 2.78 0 -1 -18 11.62 3.28 0 -1 -18 5.83 3.47 0 1 18 14.87 4.71 -1 -1 -18 13.33 4.57 -1 -1 -18 16.13 3.93 -1 -1 -18 15.90 3.39 -1 -1 -18 13.87 4.07 1 1 18 24.99 5.21 -2 -1 -18 1.36 2.84 -2 -1 -18 2.44 2.41 -2 -1 -18 2.65 2.83 -2 -1 -18 1.30 3.06 -3 -1 -18 13.14 5.03 -3 -1 -18 12.47 4.43 6 -2 -18 2.63 4.47 6 -2 -18 0.21 3.64 6 -2 -18 0.53 3.32 5 -2 -18 19.35 5.46 5 -2 -18 19.12 4.84 5 -2 -18 11.26 4.54 4 -2 -18 17.29 4.59 4 -2 -18 19.15 3.62 4 -2 -18 16.45 5.04 4 -2 -18 19.59 3.17 4 -2 -18 19.98 5.18 3 -2 -18 4.12 2.85 3 -2 -18 2.42 3.47 3 -2 -18 4.35 2.47 3 -2 -18 2.27 3.24 2 -2 -18 9.87 2.73 2 -2 -18 12.82 3.54 2 -2 -18 10.31 3.94 2 -2 -18 8.75 4.29 -2 2 18 25.91 6.14 1 -2 -18 21.08 5.01 1 -2 -18 21.57 4.12 1 -2 -18 22.87 3.42 1 -2 -18 22.42 4.55 -1 2 18 19.04 5.04 0 -2 -18 -0.70 2.32 0 -2 -18 -0.85 2.64 0 -2 -18 5.75 3.63 0 -2 -18 5.25 3.33 0 2 18 6.93 3.87 -1 -2 -18 12.70 3.33 -1 -2 -18 12.22 4.33 -1 -2 -18 12.51 4.74 -1 -2 -18 12.51 3.60 1 2 18 14.65 4.66 -2 -2 -18 23.67 5.04 -2 -2 -18 22.69 5.57 5 -3 -18 4.99 4.19 5 -3 -18 6.77 4.50 5 -3 -18 5.63 3.87 4 -3 -18 23.42 5.64 4 -3 -18 23.27 3.81 4 -3 -18 23.74 5.09 4 -3 -18 23.28 3.33 3 -3 -18 15.50 3.81 3 -3 -18 12.75 4.37 3 -3 -18 15.71 3.28 3 -3 -18 13.06 4.80 -3 3 18 9.75 4.54 2 -3 -18 -2.73 3.17 2 -3 -18 -2.31 2.91 2 -3 -18 3.60 2.77 2 -3 -18 3.36 2.36 -2 3 18 -3.33 3.20 1 -3 -18 9.49 3.68 1 -3 -18 9.41 3.18 1 -3 -18 4.39 3.64 -1 3 18 6.23 4.23 0 -3 -18 6.20 3.09 0 -3 -18 6.55 2.70 0 -3 -18 9.20 4.54 0 3 18 10.03 4.74 -1 -3 -18 2.56 3.79 1 3 18 -0.53 3.61 4 -4 -18 -1.25 2.53 4 -4 -18 -1.05 3.00 -4 4 18 4.19 4.15 3 -4 -18 30.23 6.59 3 -4 -18 15.03 3.31 3 -4 -18 15.51 3.88 -3 4 18 15.92 5.01 2 -4 -18 23.67 3.79 2 -4 -18 3.12 4.33 2 -4 -18 23.86 4.41 -2 4 18 18.10 5.62 1 -4 -18 -2.22 2.10 1 -4 -18 -4.39 3.15 1 -4 -18 -2.13 2.46 -1 4 18 0.89 4.16 0 6 -19 3.06 2.96 -1 6 -19 13.70 4.16 -1 6 -19 16.21 3.11 -1 6 -19 15.06 3.56 -1 6 -19 12.54 4.48 -2 6 -19 9.75 3.07 -2 6 -19 9.26 3.47 -2 6 -19 17.55 4.94 -2 6 -19 18.60 4.48 1 5 -19 16.02 5.23 1 5 -19 16.99 4.65 0 5 -19 4.46 4.11 0 5 -19 4.59 3.74 0 5 -19 14.46 3.44 0 5 -19 14.32 2.96 -1 5 -19 16.25 5.04 -1 5 -19 17.12 4.59 -1 5 -19 9.46 3.51 -1 5 -19 9.32 3.01 -2 5 -19 0.86 2.98 -2 5 -19 5.85 3.69 -2 5 -19 2.25 2.63 -2 5 -19 5.29 4.02 -3 5 -19 15.34 3.40 -3 5 -19 22.93 5.36 -3 5 -19 14.18 3.82 -3 5 -19 23.64 4.84 2 4 -19 0.24 3.79 2 4 -19 -0.19 3.62 1 4 -19 5.98 3.98 1 4 -19 -3.25 2.14 1 4 -19 -3.35 2.52 1 4 -19 6.79 3.72 0 4 -19 22.03 3.48 0 4 -19 21.08 3.95 0 4 -19 23.35 5.72 0 4 -19 16.96 4.35 -1 4 -19 16.89 3.27 -1 4 -19 19.64 5.15 -1 4 -19 20.50 4.67 -1 4 -19 15.42 3.66 -2 4 -19 0.81 2.95 -2 4 -19 -0.72 2.51 -2 4 -19 -0.20 2.20 -2 4 -19 0.80 3.18 -3 4 -19 13.00 3.22 -3 4 -19 13.15 3.74 -3 4 -19 8.79 4.12 -3 4 -19 9.13 3.78 3 3 -19 -1.55 3.91 2 3 -19 9.33 4.35 2 3 -19 10.22 4.00 2 3 -19 12.39 4.70 1 3 -19 -1.01 3.31 1 3 -19 19.84 3.48 1 3 -19 20.74 4.07 1 3 -19 -0.97 3.08 0 3 -19 1.64 2.63 0 3 -19 1.96 3.08 0 3 -19 1.90 3.13 0 3 -19 1.22 3.33 -1 3 -19 4.51 2.96 -1 3 -19 4.58 3.34 -1 3 -19 4.27 2.52 -1 3 -19 4.15 3.64 -2 3 -19 25.15 5.37 -2 3 -19 19.49 4.06 -2 3 -19 19.18 3.47 -2 3 -19 27.15 4.96 -3 3 -19 1.53 3.43 -3 3 -19 8.80 3.39 -3 3 -19 8.40 2.91 -3 3 -19 1.11 3.16 3 2 -19 6.96 3.92 3 2 -19 6.79 4.36 3 2 -19 7.18 4.32 2 2 -19 3.27 2.55 2 2 -19 4.97 2.82 2 2 -19 -2.29 2.99 2 2 -19 -0.80 3.65 2 2 -19 -1.48 3.35 1 2 -19 30.61 6.04 1 2 -19 20.68 3.94 1 2 -19 20.58 3.41 1 2 -19 30.89 5.40 0 2 -19 21.25 4.59 0 2 -19 20.21 5.05 0 2 -19 17.28 3.25 0 2 -19 17.25 3.75 -1 2 -19 2.14 2.36 -1 2 -19 -0.24 3.10 -1 2 -19 1.36 2.97 -1 2 -19 -0.28 3.34 -2 2 -19 8.11 3.95 -2 2 -19 8.66 4.40 -2 2 -19 10.00 3.07 -2 2 -19 9.86 3.54 -3 2 -19 34.92 6.16 -3 2 -19 35.86 5.50 4 1 -19 5.37 4.07 3 1 -19 17.23 5.19 3 1 -19 17.23 4.68 3 1 -19 17.84 5.15 2 1 -19 26.97 4.40 2 1 -19 21.00 4.99 2 1 -19 20.89 5.59 2 1 -19 25.50 5.44 2 1 -19 26.27 3.77 1 1 -19 5.05 3.89 1 1 -19 1.09 3.22 1 1 -19 -2.01 2.87 1 1 -19 -2.00 2.46 1 1 -19 0.90 3.47 0 1 -19 11.13 3.58 0 1 -19 10.97 3.10 0 1 -19 17.22 4.46 0 1 -19 17.16 4.93 -1 1 -19 9.81 4.03 -1 1 -19 9.83 4.47 -1 1 -19 11.70 3.01 -1 1 -19 11.43 3.44 -2 1 -19 1.51 3.52 -2 1 -19 4.26 3.20 -2 1 -19 4.33 2.78 -2 1 -19 1.75 3.23 4 0 -19 5.81 4.19 3 0 -19 5.52 3.87 3 0 -19 5.75 3.53 3 0 -19 3.98 3.79 3 0 -19 -0.47 2.67 3 0 -19 -0.58 2.29 2 0 -19 26.53 5.16 2 0 -19 25.64 5.71 2 0 -19 23.65 4.06 2 0 -19 23.20 5.40 2 0 -19 22.95 3.48 1 0 -19 12.10 3.21 1 0 -19 17.33 4.76 1 0 -19 12.54 3.76 1 0 -19 10.63 4.02 1 0 -19 17.02 5.30 0 0 -19 -0.45 2.21 0 0 -19 -0.61 2.55 0 0 -19 -1.04 3.49 0 0 -19 -1.60 3.74 -1 0 -19 6.28 2.68 -1 0 -19 6.04 3.99 -1 0 -19 6.43 3.11 -1 0 -19 5.83 3.63 4 -1 -19 13.11 4.90 3 -1 -19 7.38 4.49 3 -1 -19 10.30 2.87 3 -1 -19 10.27 3.31 3 -1 -19 5.15 3.66 2 -1 -19 0.33 3.86 2 -1 -19 0.79 3.75 2 -1 -19 0.10 3.53 2 -1 -19 -0.95 2.21 2 -1 -19 -0.93 2.63 1 -1 -19 16.53 5.30 1 -1 -19 4.39 2.99 1 -1 -19 17.90 4.88 1 -1 -19 4.28 2.58 0 -1 -19 12.17 3.93 0 -1 -19 6.50 2.77 0 -1 -19 6.25 3.19 0 -1 -19 11.21 4.25 0 1 19 23.13 5.50 2 -2 -19 2.10 3.12 2 -2 -19 2.59 2.72 1 -2 -19 -0.98 3.08 -1 2 19 -6.32 2.88 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 66580 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 B1 B 0.8956(10) 0.3141(9) 0.6373(6) 0.037(3) Uani 1 1 d D . . . . H1 H 0.839(6) 0.228(3) 0.604(4) 0.044 Uiso 1 1 d D U . . . B2 B 1.0278(11) 0.4160(10) 0.5984(6) 0.043(3) Uani 1 1 d D . . . . H2 H 1.063(7) 0.403(7) 0.538(3) 0.051 Uiso 1 1 d D U . . . H23 H 1.000(8) 0.476(4) 0.605(5) 0.051 Uiso 1 1 d D U . . . B3 B 1.0363(9) 0.5469(8) 0.6464(5) 0.025(2) Uani 1 1 d D . . . . H3 H 1.082(6) 0.628(3) 0.625(4) 0.031 Uiso 1 1 d D U . . . B4 B 0.9375(9) 0.4669(8) 0.7888(6) 0.028(2) Uani 1 1 d . . . . . H4 H 0.9063 0.4839 0.8510 0.034 Uiso 1 1 calc R U . . . B5 B 0.9192(9) 0.3322(8) 0.7474(7) 0.035(2) Uani 1 1 d . . . . . H5 H 0.8762 0.2595 0.7824 0.042 Uiso 1 1 calc R U . . . B6 B 1.0410(10) 0.3511(9) 0.6841(7) 0.040(3) Uani 1 1 d . . . . . H6 H 1.0813 0.2901 0.6771 0.048 Uiso 1 1 calc R U . . . B7 B 1.1326(9) 0.5006(9) 0.6884(6) 0.032(2) Uani 1 1 d . . . . . H7 H 1.2331 0.5404 0.6836 0.038 Uiso 1 1 calc R U . . . B8 B 1.0668(8) 0.5702(8) 0.7539(5) 0.026(2) Uani 1 1 d . . . . . H8 H 1.1219 0.6552 0.7926 0.031 Uiso 1 1 calc R U . . . B9 B 1.0676(9) 0.4455(8) 0.7796(6) 0.032(2) Uani 1 1 d . . . . . H9 H 1.1249 0.4467 0.8349 0.038 Uiso 1 1 calc R U . . . C1 C 0.4401(7) 0.7709(6) 0.5757(5) 0.0263(18) Uani 1 1 d . . . . . C2 C 0.3449(8) 0.7030(7) 0.5149(5) 0.033(2) Uani 1 1 d . . . . . H2A H 0.3001 0.7346 0.4884 0.039 Uiso 1 1 calc R U . . . C3 C 0.3154(8) 0.5902(7) 0.4929(5) 0.031(2) Uani 1 1 d . . . . . H3A H 0.2486 0.5426 0.4529 0.037 Uiso 1 1 calc R U . . . C4 C 0.3850(8) 0.5474(7) 0.5302(5) 0.033(2) Uani 1 1 d . . . . . H4A H 0.3668 0.4699 0.5160 0.039 Uiso 1 1 calc R U . . . C5 C 0.4797(7) 0.6178(6) 0.5876(5) 0.0251(18) Uani 1 1 d . . . . . H5A H 0.5281 0.5878 0.6116 0.030 Uiso 1 1 calc R U . . . C6 C 0.5724(7) 0.9421(6) 0.6709(4) 0.0215(17) Uani 1 1 d . . . . . C7 C 0.4731(7) 0.8896(6) 0.6084(5) 0.0248(18) Uani 1 1 d . . . . . C8 C 0.4144(8) 0.9492(7) 0.5800(5) 0.033(2) Uani 1 1 d . . . . . H8A H 0.3484 0.9125 0.5376 0.039 Uiso 1 1 calc R U . . . C9 C 0.4516(8) 1.0611(7) 0.6131(5) 0.036(2) Uani 1 1 d . . . . . H9A H 0.4115 1.1015 0.5936 0.043 Uiso 1 1 calc R U . . . C10 C 0.5468(8) 1.1137(7) 0.6742(5) 0.034(2) Uani 1 1 d . . . . . H10A H 0.5721 1.1906 0.6973 0.041 Uiso 1 1 calc R U . . . C11 C 0.6073(7) 1.0560(6) 0.7031(5) 0.0285(19) Uani 1 1 d . . . . . H11A H 0.6732 1.0945 0.7454 0.034 Uiso 1 1 calc R U . . . C12 C 0.8192(7) 0.8049(6) 0.5839(4) 0.0228(17) Uani 1 1 d . . . . . C13 C 0.8829(8) 0.8105(7) 0.5135(5) 0.032(2) Uani 1 1 d . . . . . H13A H 0.9253 0.7660 0.5035 0.038 Uiso 1 1 calc R U . . . C14 C 0.8839(8) 0.8815(7) 0.4583(5) 0.032(2) Uani 1 1 d . . . . . H14A H 0.9247 0.8840 0.4092 0.038 Uiso 1 1 calc R U . . . C15 C 0.8252(7) 0.9488(7) 0.4748(5) 0.0289(19) Uani 1 1 d . . . . . H15A H 0.8276 1.0005 0.4391 0.035 Uiso 1 1 calc R U . . . C16 C 0.7634(8) 0.9379(7) 0.5447(5) 0.030(2) Uani 1 1 d . . . . . H16A H 0.7219 0.9831 0.5556 0.036 Uiso 1 1 calc R U . . . C17 C 0.7285(7) 0.7288(6) 0.7085(4) 0.0202(16) Uani 1 1 d . . . . . C18 C 0.8096(7) 0.7317(6) 0.6475(4) 0.0194(16) Uani 1 1 d . . . . . C19 C 0.8755(7) 0.6690(6) 0.6469(4) 0.0212(17) Uani 1 1 d . . . . . H19A H 0.9310 0.6752 0.6060 0.025 Uiso 1 1 calc R U . . . C20 C 0.8612(7) 0.5971(6) 0.7055(4) 0.0233(17) Uani 1 1 d . . . . . C21 C 0.7780(7) 0.5917(6) 0.7638(5) 0.0250(18) Uani 1 1 d . . . . . H21A H 0.7638 0.5419 0.8034 0.030 Uiso 1 1 calc R U . . . C22 C 0.7157(7) 0.6561(6) 0.7657(5) 0.0265(18) Uani 1 1 d . . . . . H22A H 0.6620 0.6508 0.8077 0.032 Uiso 1 1 calc R U . . . C23 C 0.9257(7) 0.5235(6) 0.7014(4) 0.0240(17) Uani 1 1 d . . . . . C24 C 0.8432(9) 0.3913(7) 0.6988(6) 0.043(2) Uani 1 1 d D . . . . H24A H 0.743(2) 0.357(7) 0.701(5) 0.051 Uiso 1 1 d D U . . . C25 C 0.7449(7) 0.9526(6) 0.8668(4) 0.0221(17) Uani 1 1 d . . . . . C26 C 0.8254(8) 1.0293(7) 0.9313(5) 0.031(2) Uani 1 1 d . . . . . H26A H 0.8010 1.0251 0.9862 0.037 Uiso 1 1 calc R U . . . C27 C 0.9399(7) 1.1123(6) 0.9212(5) 0.0278(19) Uani 1 1 d . . . . . C28 C 0.9681(7) 1.1130(7) 0.8381(5) 0.0297(19) Uani 1 1 d . . . . . H28A H 1.0443 1.1681 0.8258 0.036 Uiso 1 1 calc R U . . . C29 C 0.8880(7) 1.0361(6) 0.7747(5) 0.0258(18) Uani 1 1 d . . . . . H29A H 0.9111 1.0392 0.7194 0.031 Uiso 1 1 calc R U . . . C30 C 0.6239(7) 0.8623(6) 0.8745(5) 0.0245(18) Uani 1 1 d . . . . . C31 C 0.5753(8) 0.8358(7) 0.9481(5) 0.035(2) Uani 1 1 d . . . . . H31A H 0.6212 0.8796 0.9991 0.042 Uiso 1 1 calc R U . . . C32 C 0.4604(8) 0.7465(7) 0.9505(5) 0.037(2) Uani 1 1 d D . . . . C33 C 0.3972(8) 0.6886(7) 0.8724(5) 0.036(2) Uani 1 1 d . . . . . H33A H 0.3178 0.6279 0.8695 0.043 Uiso 1 1 calc R U . . . C34 C 0.4484(7) 0.7183(7) 0.8008(5) 0.0273(18) Uani 1 1 d . . . . . H34A H 0.4023 0.6778 0.7492 0.033 Uiso 1 1 calc R U . . . C35 C 1.0278(8) 1.2000(7) 0.9915(5) 0.032(2) Uani 1 1 d . . . . . C36 C 1.0015(9) 1.1563(8) 1.0747(5) 0.054(3) Uani 1 1 d . . . . . H36A H 0.9205 1.1464 1.0881 0.081 Uiso 1 1 calc R U . . . H36B H 1.0627 1.2108 1.1188 0.081 Uiso 1 1 calc R U . . . H36C H 1.0044 1.0835 1.0705 0.081 Uiso 1 1 calc R U . . . C37 C 1.0108(12) 1.3061(9) 0.9973(7) 0.075(4) Uani 1 1 d . . . . . H37A H 0.9303 1.2908 1.0153 0.113 Uiso 1 1 calc R U . . . H37B H 1.0173 1.3304 0.9425 0.113 Uiso 1 1 calc R U . . . H37C H 1.0737 1.3661 1.0378 0.113 Uiso 1 1 calc R U . . . C38 C 1.1586(9) 1.2271(12) 0.9755(8) 0.088(5) Uani 1 1 d . . . . . H38A H 1.1819 1.2708 0.9295 0.132 Uiso 1 1 calc R U . . . H38B H 1.1655 1.1566 0.9608 0.132 Uiso 1 1 calc R U . . . H38C H 1.2128 1.2715 1.0260 0.132 Uiso 1 1 calc R U . . . Ir1 Ir 0.65093(3) 0.83835(2) 0.69700(2) 0.01946(11) Uani 1 1 d . . . . . N1 N 0.5083(6) 0.7271(5) 0.6118(3) 0.0214(14) Uani 1 1 d . . . . . N2 N 0.7571(6) 0.8682(5) 0.5991(4) 0.0212(14) Uani 1 1 d . . . . . N3 N 0.7767(6) 0.9551(5) 0.7869(4) 0.0217(14) Uani 1 1 d . . . . . N4 N 0.5607(6) 0.8020(5) 0.7992(4) 0.0208(14) Uani 1 1 d . . . . . C43A C 0.257(4) 0.912(4) 0.7599(15) 0.089(7) Uani 0.532(17) 1 d D U P A 1 H43A H 0.1947 0.8335 0.7422 0.106 Uiso 0.532(17) 1 calc R U P A 1 H43B H 0.3176 0.9306 0.7183 0.106 Uiso 0.532(17) 1 calc R U P A 1 Cl1A Cl 0.329(2) 0.922(2) 0.8545(12) 0.100(5) Uani 0.532(17) 1 d D U P A 1 Cl2A Cl 0.1885(10) 1.0015(12) 0.7607(6) 0.094(3) Uani 0.532(17) 1 d D U P A 1 C43Z C 0.281(3) 0.898(4) 0.7621(13) 0.069(6) Uani 0.468(17) 1 d D U P A 2 H43C H 0.2650 0.8205 0.7364 0.083 Uiso 0.468(17) 1 calc R U P A 2 H43D H 0.3520 0.9518 0.7374 0.083 Uiso 0.468(17) 1 calc R U P A 2 Cl1Z Cl 0.3179(18) 0.9144(17) 0.8671(10) 0.054(3) Uani 0.468(17) 1 d D U P A 2 Cl2Z Cl 0.1552(9) 0.9192(15) 0.7374(7) 0.100(4) Uani 0.468(17) 1 d D U P A 2 C43B C 0.340(2) 0.338(3) 0.7006(13) 0.080(6) Uani 0.476(3) 1 d D U P B 3 H43E H 0.2803 0.3549 0.6704 0.096 Uiso 0.476(3) 1 calc R U P B 3 H43F H 0.2960 0.2589 0.7108 0.096 Uiso 0.476(3) 1 calc R U P B 3 Cl1B Cl 0.4514(10) 0.3458(9) 0.6362(6) 0.046(2) Uani 0.476(3) 1 d D U P B 3 Cl2B Cl 0.3867(8) 0.4249(7) 0.7951(5) 0.085(2) Uani 0.476(3) 1 d D U P B 3 C43Y C 0.351(3) 0.349(2) 0.709(2) 0.078(6) Uani 0.411(3) 1 d D U P C 4 H43G H 0.3780 0.4114 0.7572 0.094 Uiso 0.411(3) 1 calc R U P C 4 H43H H 0.2917 0.3576 0.6716 0.094 Uiso 0.411(3) 1 calc R U P C 4 Cl1Y Cl 0.4745(15) 0.3604(19) 0.6564(11) 0.091(5) Uani 0.411(3) 1 d D U P C 4 Cl2Y Cl 0.2781(7) 0.2221(8) 0.7455(5) 0.076(2) Uani 0.411(3) 1 d D U P C 4 C43 C 0.424(8) 0.404(5) 0.727(4) 0.081(8) Uani 0.112(3) 1 d D U P D 5 H43I H 0.4187 0.4743 0.7192 0.098 Uiso 0.112(3) 1 calc R U P D 5 H43J H 0.5061 0.4266 0.7545 0.098 Uiso 0.112(3) 1 calc R U P D 5 Cl1 Cl 0.409(4) 0.326(5) 0.630(2) 0.088(8) Uani 0.112(3) 1 d D U P D 5 Cl2 Cl 0.317(3) 0.334(4) 0.7912(19) 0.090(7) Uani 0.112(3) 1 d D U P D 5 C39A C 0.4043(13) 0.7220(13) 1.0325(8) 0.055(4) Uani 0.670(14) 1 d D U P E 6 C40A C 0.4987(14) 0.7277(16) 1.0983(8) 0.068(5) Uani 0.670(14) 1 d D U P E 6 H40A H 0.5231 0.6680 1.0809 0.102 Uiso 0.670(14) 1 calc R U P E 6 H40B H 0.4636 0.7173 1.1518 0.102 Uiso 0.670(14) 1 calc R U P E 6 H40C H 0.5701 0.8016 1.1044 0.102 Uiso 0.670(14) 1 calc R U P E 6 C41A C 0.2943(13) 0.6068(12) 1.0205(9) 0.074(5) Uani 0.670(14) 1 d D U P E 6 H41A H 0.3206 0.5477 1.0061 0.110 Uiso 0.670(14) 1 calc R U P E 6 H41B H 0.2369 0.6022 0.9754 0.110 Uiso 0.670(14) 1 calc R U P E 6 H41C H 0.2545 0.5962 1.0723 0.110 Uiso 0.670(14) 1 calc R U P E 6 C42A C 0.3615(15) 0.8122(13) 1.0637(9) 0.070(5) Uani 0.670(14) 1 d D U P E 6 H42A H 0.2984 0.8076 1.0230 0.106 Uiso 0.670(14) 1 calc R U P E 6 H42B H 0.4307 0.8876 1.0702 0.106 Uiso 0.670(14) 1 calc R U P E 6 H42C H 0.3283 0.7987 1.1175 0.106 Uiso 0.670(14) 1 calc R U P E 6 C39Z C 0.408(2) 0.7031(19) 1.0292(12) 0.061(7) Uani 0.330(14) 1 d D U P E 7 C40Z C 0.495(3) 0.773(3) 1.1066(10) 0.073(8) Uani 0.330(14) 1 d D U P E 7 H40D H 0.5738 0.7722 1.1010 0.110 Uiso 0.330(14) 1 calc R U P E 7 H40E H 0.4609 0.7410 1.1562 0.110 Uiso 0.330(14) 1 calc R U P E 7 H40F H 0.5063 0.8512 1.1123 0.110 Uiso 0.330(14) 1 calc R U P E 7 C41Z C 0.383(3) 0.5797(17) 1.0265(17) 0.069(8) Uani 0.330(14) 1 d D U P E 7 H41D H 0.4599 0.5748 1.0297 0.103 Uiso 0.330(14) 1 calc R U P E 7 H41E H 0.3341 0.5348 0.9742 0.103 Uiso 0.330(14) 1 calc R U P E 7 H41F H 0.3378 0.5504 1.0738 0.103 Uiso 0.330(14) 1 calc R U P E 7 C42Z C 0.288(2) 0.711(3) 1.0374(17) 0.071(7) Uani 0.330(14) 1 d D U P E 7 H42D H 0.2251 0.6530 0.9955 0.107 Uiso 0.330(14) 1 calc R U P E 7 H42E H 0.2989 0.7858 1.0286 0.107 Uiso 0.330(14) 1 calc R U P E 7 H42F H 0.2622 0.6982 1.0933 0.107 Uiso 0.330(14) 1 calc R U P E 7 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 B1 0.034(7) 0.039(6) 0.033(5) -0.016(4) -0.019(5) 0.019(5) B2 0.057(8) 0.050(7) 0.029(5) -0.016(5) -0.012(5) 0.038(6) B3 0.033(6) 0.030(5) 0.019(4) 0.002(4) 0.004(4) 0.021(5) B4 0.024(6) 0.028(5) 0.025(5) 0.005(4) 0.000(4) 0.005(4) B5 0.028(6) 0.030(5) 0.052(6) 0.013(5) 0.001(5) 0.015(5) B6 0.043(7) 0.030(5) 0.049(6) -0.002(5) -0.010(5) 0.021(5) B7 0.023(6) 0.040(6) 0.029(5) 0.002(4) -0.002(4) 0.012(5) B8 0.021(5) 0.033(5) 0.022(4) -0.006(4) 0.004(4) 0.012(4) B9 0.025(6) 0.027(5) 0.045(6) 0.005(4) -0.015(4) 0.013(4) C1 0.027(5) 0.023(4) 0.025(4) -0.003(3) 0.003(3) 0.009(4) C2 0.038(6) 0.032(5) 0.028(4) -0.001(4) -0.017(4) 0.017(4) C3 0.030(5) 0.036(5) 0.021(4) -0.003(3) -0.011(3) 0.012(4) C4 0.033(5) 0.019(4) 0.039(5) 0.003(4) 0.005(4) 0.005(4) C5 0.024(5) 0.028(4) 0.028(4) 0.001(3) -0.001(3) 0.016(4) C6 0.014(4) 0.023(4) 0.024(4) 0.001(3) -0.003(3) 0.006(3) C7 0.030(5) 0.027(4) 0.025(4) 0.007(3) 0.005(3) 0.018(4) C8 0.029(5) 0.042(5) 0.028(4) 0.006(4) -0.004(4) 0.017(4) C9 0.032(6) 0.032(5) 0.050(5) 0.005(4) -0.008(4) 0.021(4) C10 0.033(6) 0.024(4) 0.050(5) 0.007(4) 0.007(4) 0.015(4) C11 0.024(5) 0.025(4) 0.031(4) -0.002(3) -0.002(4) 0.007(4) C12 0.018(5) 0.019(4) 0.024(4) 0.000(3) -0.002(3) 0.003(3) C13 0.029(5) 0.038(5) 0.035(5) 0.008(4) 0.007(4) 0.020(4) C14 0.033(5) 0.039(5) 0.027(4) 0.009(4) 0.007(4) 0.019(4) C15 0.031(5) 0.031(5) 0.027(4) 0.016(4) 0.011(4) 0.013(4) C16 0.036(5) 0.032(5) 0.029(4) 0.013(4) 0.000(4) 0.020(4) C17 0.016(4) 0.020(4) 0.022(4) 0.001(3) -0.008(3) 0.007(3) C18 0.018(4) 0.023(4) 0.021(4) 0.011(3) 0.000(3) 0.010(3) C19 0.022(5) 0.022(4) 0.019(4) 0.004(3) 0.004(3) 0.009(3) C20 0.021(5) 0.025(4) 0.022(4) 0.000(3) -0.004(3) 0.010(4) C21 0.031(5) 0.026(4) 0.022(4) 0.009(3) 0.003(3) 0.015(4) C22 0.021(5) 0.030(4) 0.031(4) 0.008(3) 0.009(3) 0.013(4) C23 0.027(5) 0.026(4) 0.023(4) 0.004(3) 0.002(3) 0.016(4) C24 0.052(7) 0.026(5) 0.050(6) 0.003(4) -0.009(5) 0.020(5) C25 0.022(5) 0.026(4) 0.021(4) 0.000(3) 0.002(3) 0.014(4) C26 0.027(5) 0.036(5) 0.021(4) -0.002(3) -0.003(3) 0.008(4) C27 0.027(5) 0.022(4) 0.028(4) 0.003(3) -0.001(4) 0.006(4) C28 0.016(5) 0.024(4) 0.038(5) 0.000(4) 0.000(4) 0.000(4) C29 0.022(5) 0.027(4) 0.022(4) 0.006(3) -0.002(3) 0.004(4) C30 0.021(5) 0.026(4) 0.022(4) -0.003(3) -0.001(3) 0.009(4) C31 0.028(5) 0.038(5) 0.024(4) -0.006(4) -0.006(4) 0.005(4) C32 0.029(6) 0.041(5) 0.041(5) 0.005(4) 0.012(4) 0.015(5) C33 0.016(5) 0.036(5) 0.035(5) -0.006(4) 0.003(4) -0.003(4) C34 0.022(5) 0.030(4) 0.026(4) 0.002(3) -0.003(3) 0.008(4) C35 0.025(5) 0.035(5) 0.025(4) -0.009(3) -0.009(3) 0.008(4) C36 0.044(6) 0.051(6) 0.031(5) 0.005(4) -0.019(4) -0.011(5) C37 0.111(11) 0.037(6) 0.064(7) -0.013(5) -0.041(7) 0.030(7) C38 0.021(7) 0.124(12) 0.070(8) -0.010(8) -0.002(6) -0.005(7) Ir1 0.01871(19) 0.02018(16) 0.01939(15) 0.00096(10) -0.00076(11) 0.00936(13) N1 0.030(4) 0.021(3) 0.014(3) 0.002(2) 0.003(3) 0.011(3) N2 0.020(4) 0.021(3) 0.022(3) 0.000(3) 0.000(3) 0.010(3) N3 0.018(4) 0.023(3) 0.026(3) 0.002(3) 0.001(3) 0.012(3) N4 0.019(4) 0.024(3) 0.025(3) 0.003(3) -0.001(3) 0.015(3) C43A 0.095(12) 0.088(12) 0.079(10) 0.021(10) 0.037(10) 0.034(10) Cl1A 0.088(7) 0.084(7) 0.111(9) 0.007(7) 0.041(6) 0.022(6) Cl2A 0.113(6) 0.101(7) 0.080(5) 0.035(5) 0.036(4) 0.052(6) C43Z 0.082(12) 0.069(10) 0.068(10) 0.018(9) 0.039(9) 0.040(9) Cl1Z 0.060(6) 0.062(5) 0.056(5) 0.011(4) 0.019(4) 0.040(5) Cl2Z 0.080(6) 0.116(9) 0.084(6) 0.040(6) 0.018(4) 0.019(6) C43B 0.058(9) 0.094(9) 0.077(9) 0.005(9) 0.020(8) 0.027(8) Cl1B 0.030(5) 0.039(5) 0.073(5) 0.011(4) 0.007(4) 0.020(4) Cl2B 0.086(5) 0.090(5) 0.087(5) -0.002(4) 0.000(4) 0.052(4) C43Y 0.057(9) 0.094(10) 0.075(9) 0.002(9) 0.019(9) 0.028(9) Cl1Y 0.071(8) 0.085(8) 0.120(9) 0.034(7) 0.010(7) 0.034(6) Cl2Y 0.061(5) 0.112(6) 0.060(4) 0.032(4) 0.010(3) 0.038(4) C43 0.065(11) 0.091(11) 0.081(10) 0.012(10) 0.013(10) 0.029(10) Cl1 0.067(12) 0.094(11) 0.100(11) 0.009(10) 0.003(11) 0.035(11) Cl2 0.072(11) 0.105(11) 0.088(11) 0.031(10) 0.007(10) 0.030(10) C39A 0.041(8) 0.076(9) 0.032(7) 0.012(6) 0.012(6) 0.011(7) C40A 0.055(9) 0.086(10) 0.050(8) 0.027(7) 0.008(7) 0.016(8) C41A 0.056(9) 0.091(10) 0.040(7) 0.020(7) 0.030(7) -0.002(8) C42A 0.057(9) 0.091(10) 0.046(8) 0.005(8) 0.023(7) 0.018(8) C39Z 0.049(10) 0.078(11) 0.033(10) 0.015(10) 0.014(9) 0.004(10) C40Z 0.062(11) 0.081(13) 0.045(10) 0.018(11) 0.018(10) 0.000(11) C41Z 0.061(12) 0.075(12) 0.052(11) 0.020(11) 0.014(11) 0.010(11) C42Z 0.055(11) 0.090(12) 0.048(10) 0.018(11) 0.022(10) 0.011(11) 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' B B 0.0013 0.0007 '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' Cl Cl 0.1484 0.1585 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C24 B1 B6 104.9(7) . . ? C24 B1 B5 59.0(5) . . ? B6 B1 B5 60.8(6) . . ? C24 B1 B2 104.9(7) . . ? B6 B1 B2 60.0(6) . . ? B5 B1 B2 109.3(7) . . ? C24 B1 H1 125(5) . . ? B6 B1 H1 121(4) . . ? B5 B1 H1 118(4) . . ? B2 B1 H1 123(4) . . ? B3 B2 B6 103.5(7) . . ? B3 B2 B1 102.9(7) . . ? B6 B2 B1 58.7(6) . . ? B3 B2 B7 57.5(5) . . ? B6 B2 B7 60.4(6) . . ? B1 B2 B7 106.4(7) . . ? B3 B2 H2 124(5) . . ? B6 B2 H2 123(5) . . ? B1 B2 H2 126(5) . . ? B7 B2 H2 120(5) . . ? B3 B2 H23 27(5) . . ? B6 B2 H23 121(5) . . ? B1 B2 H23 94(5) . . ? B7 B2 H23 84(5) . . ? H2 B2 H23 116(7) . . ? C23 B3 B7 109.6(6) . . ? C23 B3 B8 62.2(5) . . ? B7 B3 B8 61.2(5) . . ? C23 B3 B2 109.1(7) . . ? B7 B3 B2 62.2(5) . . ? B8 B3 B2 112.9(7) . . ? C23 B3 H23 99(5) . . ? B7 B3 H23 89(5) . . ? B8 B3 H23 131(5) . . ? B2 B3 H23 27(5) . . ? C23 B3 H3 120(4) . . ? B7 B3 H3 114(4) . . ? B8 B3 H3 108(4) . . ? B2 B3 H3 127(4) . . ? H23 B3 H3 120(6) . . ? C23 B4 C24 55.0(5) . . ? C23 B4 B5 103.3(6) . . ? C24 B4 B5 58.6(5) . . ? C23 B4 B9 104.6(6) . . ? C24 B4 B9 105.3(7) . . ? B5 B4 B9 61.5(6) . . ? C23 B4 B8 59.2(5) . . ? C24 B4 B8 104.5(6) . . ? B5 B4 B8 110.0(7) . . ? B9 B4 B8 60.7(5) . . ? C23 B4 H4 125.9 . . ? C24 B4 H4 125.3 . . ? B5 B4 H4 121.5 . . ? B9 B4 H4 122.0 . . ? B8 B4 H4 121.0 . . ? C24 B5 B4 60.2(5) . . ? C24 B5 B1 57.8(6) . . ? B4 B5 B1 108.6(7) . . ? C24 B5 B6 102.6(7) . . ? B4 B5 B6 106.9(7) . . ? B1 B5 B6 59.0(6) . . ? C24 B5 B9 104.9(7) . . ? B4 B5 B9 59.4(6) . . ? B1 B5 B9 107.9(7) . . ? B6 B5 B9 60.0(6) . . ? C24 B5 H5 125.1 . . ? B4 B5 H5 121.1 . . ? B1 B5 H5 121.7 . . ? B6 B5 H5 123.8 . . ? B9 B5 H5 122.3 . . ? B1 B6 B2 61.3(6) . . ? B1 B6 B5 60.1(6) . . ? B2 B6 B5 109.8(7) . . ? B1 B6 B9 108.9(7) . . ? B2 B6 B9 110.0(7) . . ? B5 B6 B9 60.2(6) . . ? B1 B6 B7 108.6(7) . . ? B2 B6 B7 60.7(6) . . ? B5 B6 B7 107.7(7) . . ? B9 B6 B7 59.9(5) . . ? B1 B6 H6 121.1 . . ? B2 B6 H6 119.9 . . ? B5 B6 H6 121.6 . . ? B9 B6 H6 121.0 . . ? B7 B6 H6 122.0 . . ? B3 B7 B8 59.8(5) . . ? B3 B7 B9 105.8(7) . . ? B8 B7 B9 59.9(5) . . ? B3 B7 B6 104.6(7) . . ? B8 B7 B6 107.4(7) . . ? B9 B7 B6 59.7(6) . . ? B3 B7 B2 60.4(5) . . ? B8 B7 B2 110.2(7) . . ? B9 B7 B2 108.4(7) . . ? B6 B7 B2 59.0(6) . . ? B3 B7 H7 123.6 . . ? B8 B7 H7 120.8 . . ? B9 B7 H7 122.2 . . ? B6 B7 H7 123.5 . . ? B2 B7 H7 120.5 . . ? C23 B8 B3 54.6(5) . . ? C23 B8 B4 59.6(5) . . ? B3 B8 B4 104.7(7) . . ? C23 B8 B7 102.0(6) . . ? B3 B8 B7 59.0(5) . . ? B4 B8 B7 108.0(7) . . ? C23 B8 B9 104.0(6) . . ? B3 B8 B9 106.1(6) . . ? B4 B8 B9 59.5(6) . . ? B7 B8 B9 61.0(6) . . ? C23 B8 H8 126.4 . . ? B3 B8 H8 124.5 . . ? B4 B8 H8 121.7 . . ? B7 B8 H8 122.6 . . ? B9 B8 H8 122.3 . . ? B4 B9 B8 59.7(5) . . ? B4 B9 B6 106.6(7) . . ? B8 B9 B6 107.3(7) . . ? B4 B9 B5 59.1(5) . . ? B8 B9 B5 107.2(6) . . ? B6 B9 B5 59.9(6) . . ? B4 B9 B7 106.6(6) . . ? B8 B9 B7 59.1(5) . . ? B6 B9 B7 60.4(6) . . ? B5 B9 B7 107.8(7) . . ? B4 B9 H9 122.8 . . ? B8 B9 H9 122.3 . . ? B6 B9 H9 122.0 . . ? B5 B9 H9 122.0 . . ? B7 B9 H9 122.1 . . ? N1 C1 C2 120.4(7) . . ? N1 C1 C7 115.1(7) . . ? C2 C1 C7 124.5(7) . . ? C3 C2 C1 120.1(7) . . ? C3 C2 H2A 120.0 . . ? C1 C2 H2A 120.0 . . ? C2 C3 C4 118.7(7) . . ? C2 C3 H3A 120.6 . . ? C4 C3 H3A 120.6 . . ? C5 C4 C3 119.1(7) . . ? C5 C4 H4A 120.4 . . ? C3 C4 H4A 120.4 . . ? N1 C5 C4 123.4(7) . . ? N1 C5 H5A 118.3 . . ? C4 C5 H5A 118.3 . . ? C11 C6 C7 116.6(7) . . ? C11 C6 Ir1 129.5(6) . . ? C7 C6 Ir1 113.9(5) . . ? C8 C7 C6 121.3(7) . . ? C8 C7 C1 123.8(7) . . ? C6 C7 C1 114.9(7) . . ? C9 C8 C7 120.4(8) . . ? C9 C8 H8A 119.8 . . ? C7 C8 H8A 119.8 . . ? C10 C9 C8 119.6(7) . . ? C10 C9 H9A 120.2 . . ? C8 C9 H9A 120.2 . . ? C9 C10 C11 121.0(8) . . ? C9 C10 H10A 119.5 . . ? C11 C10 H10A 119.5 . . ? C10 C11 C6 121.2(7) . . ? C10 C11 H11A 119.4 . . ? C6 C11 H11A 119.4 . . ? N2 C12 C13 121.0(7) . . ? N2 C12 C18 113.9(6) . . ? C13 C12 C18 125.0(7) . . ? C14 C13 C12 119.5(8) . . ? C14 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? C15 C14 C13 119.8(8) . . ? C15 C14 H14A 120.1 . . ? C13 C14 H14A 120.1 . . ? C16 C15 C14 117.4(7) . . ? C16 C15 H15A 121.3 . . ? C14 C15 H15A 121.3 . . ? N2 C16 C15 125.0(8) . . ? N2 C16 H16A 117.5 . . ? C15 C16 H16A 117.5 . . ? C22 C17 C18 115.4(7) . . ? C22 C17 Ir1 131.5(6) . . ? C18 C17 Ir1 113.1(5) . . ? C19 C18 C17 122.0(6) . . ? C19 C18 C12 122.2(7) . . ? C17 C18 C12 115.7(6) . . ? C18 C19 C20 121.1(7) . . ? C18 C19 H19A 119.4 . . ? C20 C19 H19A 119.4 . . ? C21 C20 C19 116.5(7) . . ? C21 C20 C23 122.2(7) . . ? C19 C20 C23 121.2(7) . . ? C22 C21 C20 122.3(7) . . ? C22 C21 H21A 118.9 . . ? C20 C21 H21A 118.9 . . ? C21 C22 C17 122.6(7) . . ? C21 C22 H22A 118.7 . . ? C17 C22 H22A 118.7 . . ? C20 C23 B3 120.7(6) . . ? C20 C23 C24 116.8(7) . . ? B3 C23 C24 111.5(7) . . ? C20 C23 B8 121.2(6) . . ? B3 C23 B8 63.2(5) . . ? C24 C23 B8 112.4(6) . . ? C20 C23 B4 118.3(6) . . ? B3 C23 B4 113.1(6) . . ? C24 C23 B4 62.6(5) . . ? B8 C23 B4 61.2(5) . . ? C23 C24 B1 111.5(8) . . ? C23 C24 B5 111.3(7) . . ? B1 C24 B5 63.2(6) . . ? C23 C24 B4 62.3(5) . . ? B1 C24 B4 113.9(7) . . ? B5 C24 B4 61.2(6) . . ? C23 C24 H24A 121(5) . . ? B1 C24 H24A 118(5) . . ? B5 C24 H24A 119(5) . . ? B4 C24 H24A 119(5) . . ? N3 C25 C26 119.8(7) . . ? N3 C25 C30 114.0(6) . . ? C26 C25 C30 126.1(7) . . ? C25 C26 C27 124.2(8) . . ? C25 C26 H26A 117.9 . . ? C27 C26 H26A 117.9 . . ? C26 C27 C28 114.1(7) . . ? C26 C27 C35 124.7(7) . . ? C28 C27 C35 121.1(7) . . ? C29 C28 C27 121.3(8) . . ? C29 C28 H28A 119.4 . . ? C27 C28 H28A 119.4 . . ? N3 C29 C28 123.1(7) . . ? N3 C29 H29A 118.5 . . ? C28 C29 H29A 118.5 . . ? C31 C30 N4 121.1(7) . . ? C31 C30 C25 125.4(7) . . ? N4 C30 C25 113.5(6) . . ? C30 C31 C32 122.1(7) . . ? C30 C31 H31A 119.0 . . ? C32 C31 H31A 119.0 . . ? C31 C32 C33 115.3(7) . . ? C31 C32 C39Z 124.7(11) . . ? C33 C32 C39Z 119.7(11) . . ? C31 C32 C39A 121.5(9) . . ? C33 C32 C39A 122.9(9) . . ? C34 C33 C32 120.7(8) . . ? C34 C33 H33A 119.7 . . ? C32 C33 H33A 119.7 . . ? N4 C34 C33 123.6(7) . . ? N4 C34 H34A 118.2 . . ? C33 C34 H34A 118.2 . . ? C37 C35 C27 109.0(7) . . ? C37 C35 C38 109.8(10) . . ? C27 C35 C38 110.5(8) . . ? C37 C35 C36 108.1(8) . . ? C27 C35 C36 110.2(7) . . ? C38 C35 C36 109.2(8) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N4 Ir1 N3 79.1(2) . . ? N4 Ir1 N2 172.8(2) . . ? N3 Ir1 N2 98.1(2) . . ? N4 Ir1 N1 96.3(2) . . ? N3 Ir1 N1 172.8(2) . . ? N2 Ir1 N1 87.1(2) . . ? N4 Ir1 C6 91.8(3) . . ? N3 Ir1 C6 94.9(3) . . ? N2 Ir1 C6 95.0(3) . . ? N1 Ir1 C6 79.6(3) . . ? N4 Ir1 C17 93.4(3) . . ? N3 Ir1 C17 89.9(3) . . ? N2 Ir1 C17 79.9(3) . . ? N1 Ir1 C17 96.0(3) . . ? C6 Ir1 C17 173.5(3) . . ? C5 N1 C1 118.3(6) . . ? C5 N1 Ir1 125.4(5) . . ? C1 N1 Ir1 116.3(5) . . ? C16 N2 C12 117.2(7) . . ? C16 N2 Ir1 125.6(5) . . ? C12 N2 Ir1 117.1(5) . . ? C29 N3 C25 117.5(6) . . ? C29 N3 Ir1 126.1(5) . . ? C25 N3 Ir1 116.4(5) . . ? C34 N4 C30 117.2(6) . . ? C34 N4 Ir1 125.9(5) . . ? C30 N4 Ir1 116.7(5) . . ? Cl1A C43A Cl2A 113.6(13) . . ? Cl1A C43A H43A 108.9 . . ? Cl2A C43A H43A 108.9 . . ? Cl1A C43A H43B 108.9 . . ? Cl2A C43A H43B 108.9 . . ? H43A C43A H43B 107.7 . . ? Cl1Z C43Z Cl2Z 113.8(13) . . ? Cl1Z C43Z H43C 108.8 . . ? Cl2Z C43Z H43C 108.8 . . ? Cl1Z C43Z H43D 108.8 . . ? Cl2Z C43Z H43D 108.8 . . ? H43C C43Z H43D 107.7 . . ? Cl2B C43B Cl1B 116.5(14) . . ? Cl2B C43B H43E 108.2 . . ? Cl1B C43B H43E 108.2 . . ? Cl2B C43B H43F 108.2 . . ? Cl1B C43B H43F 108.2 . . ? H43E C43B H43F 107.3 . . ? Cl2Y C43Y Cl1Y 113.3(15) . . ? Cl2Y C43Y H43G 108.9 . . ? Cl1Y C43Y H43G 108.9 . . ? Cl2Y C43Y H43H 108.9 . . ? Cl1Y C43Y H43H 108.9 . . ? H43G C43Y H43H 107.7 . . ? Cl1 C43 Cl2 114.0(17) . . ? Cl1 C43 H43I 108.8 . . ? Cl2 C43 H43I 108.8 . . ? Cl1 C43 H43J 108.8 . . ? Cl2 C43 H43J 108.8 . . ? H43I C43 H43J 107.7 . . ? C41A C39A C32 110.8(10) . . ? C41A C39A C40A 110.2(11) . . ? C32 C39A C40A 110.1(10) . . ? C41A C39A C42A 108.1(11) . . ? C32 C39A C42A 109.1(10) . . ? C40A C39A C42A 108.5(11) . . ? C39A C40A H40A 109.5 . . ? C39A C40A H40B 109.5 . . ? H40A C40A H40B 109.5 . . ? C39A C40A H40C 109.5 . . ? H40A C40A H40C 109.5 . . ? H40B C40A H40C 109.5 . . ? C39A C41A H41A 109.5 . . ? C39A C41A H41B 109.5 . . ? H41A C41A H41B 109.5 . . ? C39A C41A H41C 109.5 . . ? H41A C41A H41C 109.5 . . ? H41B C41A H41C 109.5 . . ? C39A C42A H42A 109.5 . . ? C39A C42A H42B 109.5 . . ? H42A C42A H42B 109.5 . . ? C39A C42A H42C 109.5 . . ? H42A C42A H42C 109.5 . . ? H42B C42A H42C 109.5 . . ? C32 C39Z C40Z 111.2(14) . . ? C32 C39Z C41Z 111.1(14) . . ? C40Z C39Z C41Z 108.3(14) . . ? C32 C39Z C42Z 109.1(13) . . ? C40Z C39Z C42Z 108.6(14) . . ? C41Z C39Z C42Z 108.4(14) . . ? C39Z C40Z H40D 109.5 . . ? C39Z C40Z H40E 109.5 . . ? H40D C40Z H40E 109.5 . . ? C39Z C40Z H40F 109.5 . . ? H40D C40Z H40F 109.5 . . ? H40E C40Z H40F 109.5 . . ? C39Z C41Z H41D 109.5 . . ? C39Z C41Z H41E 109.5 . . ? H41D C41Z H41E 109.5 . . ? C39Z C41Z H41F 109.5 . . ? H41D C41Z H41F 109.5 . . ? H41E C41Z H41F 109.5 . . ? C39Z C42Z H42D 109.5 . . ? C39Z C42Z H42E 109.5 . . ? H42D C42Z H42E 109.5 . . ? C39Z C42Z H42F 109.5 . . ? H42D C42Z H42F 109.5 . . ? H42E C42Z H42F 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 C24 1.679(14) . ? B1 B6 1.752(14) . ? B1 B5 1.772(14) . ? B1 B2 1.797(17) . ? B1 H1 1.10(2) . ? B2 B3 1.774(14) . ? B2 B6 1.774(15) . ? B2 B7 1.805(13) . ? B2 H2 1.10(2) . ? B2 H23 1.00(4) . ? B3 C23 1.584(12) . ? B3 B7 1.720(13) . ? B3 B8 1.734(12) . ? B3 H23 0.99(4) . ? B3 H3 1.09(2) . ? B4 C23 1.725(11) . ? B4 C24 1.730(12) . ? B4 B5 1.747(14) . ? B4 B9 1.751(14) . ? B4 B8 1.754(13) . ? B4 H4 1.1200 . ? B5 C24 1.701(12) . ? B5 B6 1.784(16) . ? B5 B9 1.790(14) . ? B5 H5 1.1200 . ? B6 B9 1.787(14) . ? B6 B7 1.799(14) . ? B6 H6 1.1200 . ? B7 B8 1.758(13) . ? B7 B9 1.791(14) . ? B7 H7 1.1200 . ? B8 C23 1.718(12) . ? B8 B9 1.773(13) . ? B8 H8 1.1200 . ? B9 H9 1.1200 . ? C1 N1 1.371(10) . ? C1 C2 1.392(11) . ? C1 C7 1.470(10) . ? C2 C3 1.377(11) . ? C2 H2A 0.9500 . ? C3 C4 1.385(11) . ? C3 H3A 0.9500 . ? C4 C5 1.362(11) . ? C4 H4A 0.9500 . ? C5 N1 1.341(9) . ? C5 H5A 0.9500 . ? C6 C11 1.405(10) . ? C6 C7 1.415(10) . ? C6 Ir1 2.083(7) . ? C7 C8 1.397(10) . ? C8 C9 1.379(11) . ? C8 H8A 0.9500 . ? C9 C10 1.371(12) . ? C9 H9A 0.9500 . ? C10 C11 1.393(11) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 N2 1.371(9) . ? C12 C13 1.395(11) . ? C12 C18 1.486(9) . ? C13 C14 1.385(11) . ? C13 H13A 0.9500 . ? C14 C15 1.384(11) . ? C14 H14A 0.9500 . ? C15 C16 1.371(11) . ? C15 H15A 0.9500 . ? C16 N2 1.345(9) . ? C16 H16A 0.9500 . ? C17 C22 1.394(10) . ? C17 C18 1.417(10) . ? C17 Ir1 2.090(7) . ? C18 C19 1.397(10) . ? C19 C20 1.400(10) . ? C19 H19A 0.9500 . ? C20 C21 1.397(11) . ? C20 C23 1.506(10) . ? C21 C22 1.377(10) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C24 1.596(11) . ? C24 H24A 1.11(2) . ? C25 N3 1.366(9) . ? C25 C26 1.376(10) . ? C25 C30 1.467(11) . ? C26 C27 1.388(11) . ? C26 H26A 0.9500 . ? C27 C28 1.402(11) . ? C27 C35 1.519(10) . ? C28 C29 1.364(10) . ? C28 H28A 0.9500 . ? C29 N3 1.361(9) . ? C29 H29A 0.9500 . ? C30 C31 1.369(11) . ? C30 N4 1.374(9) . ? C31 C32 1.398(11) . ? C31 H31A 0.9500 . ? C32 C33 1.403(11) . ? C32 C39Z 1.516(18) . ? C32 C39A 1.524(14) . ? C33 C34 1.359(11) . ? C33 H33A 0.9500 . ? C34 N4 1.345(10) . ? C34 H34A 0.9500 . ? C35 C37 1.513(13) . ? C35 C38 1.523(14) . ? C35 C36 1.529(12) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? Ir1 N4 2.015(6) . ? Ir1 N3 2.026(6) . ? Ir1 N2 2.053(6) . ? Ir1 N1 2.056(6) . ? C43A Cl1A 1.709(15) . ? C43A Cl2A 1.733(15) . ? C43A H43A 0.9900 . ? C43A H43B 0.9900 . ? C43Z Cl1Z 1.712(15) . ? C43Z Cl2Z 1.738(16) . ? C43Z H43C 0.9900 . ? C43Z H43D 0.9900 . ? C43B Cl2B 1.713(17) . ? C43B Cl1B 1.724(14) . ? C43B H43E 0.9900 . ? C43B H43F 0.9900 . ? C43Y Cl2Y 1.724(18) . ? C43Y Cl1Y 1.726(15) . ? C43Y H43G 0.9900 . ? C43Y H43H 0.9900 . ? C43 Cl1 1.724(17) . ? C43 Cl2 1.725(18) . ? C43 H43I 0.9900 . ? C43 H43J 0.9900 . ? C39A C41A 1.519(15) . ? C39A C40A 1.526(15) . ? C39A C42A 1.547(16) . ? C40A H40A 0.9800 . ? C40A H40B 0.9800 . ? C40A H40C 0.9800 . ? C41A H41A 0.9800 . ? C41A H41B 0.9800 . ? C41A H41C 0.9800 . ? C42A H42A 0.9800 . ? C42A H42B 0.9800 . ? C42A H42C 0.9800 . ? C39Z C40Z 1.528(18) . ? C39Z C41Z 1.530(18) . ? C39Z C42Z 1.535(18) . ? C40Z H40D 0.9800 . ? C40Z H40E 0.9800 . ? C40Z H40F 0.9800 . ? C41Z H41D 0.9800 . ? C41Z H41E 0.9800 . ? C41Z H41F 0.9800 . ? C42Z H42D 0.9800 . ? C42Z H42E 0.9800 . ? C42Z H42F 0.9800 . ?