#------------------------------------------------------------------------------ #$Date: 2017-07-27 08:14:18 +0300 (Thu, 27 Jul 2017) $ #$Revision: 199367 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/87/7228791.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_7228791 loop_ _publ_author_name 'Jing, Yi-Ming' 'Zheng, You-Xuan' _publ_section_title ; Photoluminescence and electroluminescence of deep red iridium(iii) complexes with 2,3-diphenylquinoxaline derivatives and 1,3,4-oxadiazole derivatives ligands ; _journal_issue 59 _journal_name_full 'RSC Adv.' _journal_page_first 37021 _journal_paper_doi 10.1039/C7RA05530G _journal_volume 7 _journal_year 2017 _chemical_formula_moiety 'C54 H35 Ir N6 O2' _chemical_formula_sum 'C54 H35 Ir N6 O2' _chemical_formula_weight 992.08 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_date 2017-03-01 _audit_creation_method ; Olex2 1.2 (compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289) ; _audit_update_record ; 2017-03-01 deposited with the CCDC. 2017-07-19 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 110.451(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.3469(19) _cell_length_b 31.314(5) _cell_length_c 13.335(2) _cell_measurement_reflns_used 5855 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25.32 _cell_measurement_theta_min 2.32 _cell_volume 4439.5(12) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 293.15 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0657 _diffrn_reflns_av_unetI/netI 0.0713 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 24108 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.009 _diffrn_reflns_theta_max 25.009 _diffrn_reflns_theta_min 1.755 _exptl_absorpt_coefficient_mu 3.057 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.4451 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS 2014/5' _exptl_crystal_colour black _exptl_crystal_colour_primary black _exptl_crystal_density_diffrn 1.484 _exptl_crystal_description block _exptl_crystal_F_000 1976 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.19 _refine_diff_density_max 5.635 _refine_diff_density_min -6.532 _refine_diff_density_rms 0.256 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 562 _refine_ls_number_reflns 7779 _refine_ls_number_restraints 360 _refine_ls_restrained_S_all 1.113 _refine_ls_R_factor_all 0.1210 _refine_ls_R_factor_gt 0.1040 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+257.0153P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2567 _refine_ls_wR_factor_ref 0.2655 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6215 _reflns_number_total 7779 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; 1_sq.res created by SHELXL-2014/7 TITL 20161228ZYX_DP_0m in P2(1)/c CELL 0.71073 11.3469 31.3136 13.3349 90 110.451 90 ZERR 4 0.0019 0.0051 0.0022 0 0.003 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Ir N O UNIT 216 140 4 24 8 ISOR 0.01 0.02 $C N1 N2 N4 N5 N6 ISOR 0.001 0.002 C40 N3 C2 L.S. 10 PLAN 10 SIZE 0.27 0.24 0.19 TEMP 20 FREE O1 C51 FREE N5 C11 FREE C15 C8 BOND $H fmap 2 acta ABIN OMIT -3 50.02 OMIT -1 12 2 OMIT -1 2 3 OMIT 3 3 2 OMIT -1 14 1 OMIT -1 2 1 REM REM REM WGHT 0.030500 257.015320 FVAR 0.18182 PART 1 C1 1 0.617757 0.112736 0.322635 11.00000 0.03146 0.02409 = 0.03242 0.00160 0.00081 -0.00265 C2 1 0.678984 0.094571 0.427230 11.00000 0.04704 0.04732 = 0.04712 0.00041 0.01646 0.00011 AFIX 43 H2 2 0.764694 0.088684 0.450937 11.00000 -1.20000 AFIX 0 C3 1 0.610908 0.085993 0.491618 11.00000 0.04765 0.05200 = 0.04251 0.00789 0.01062 0.00390 AFIX 43 H3 2 0.649396 0.071819 0.556112 11.00000 -1.20000 AFIX 0 C4 1 0.483831 0.098137 0.462486 11.00000 0.05118 0.05096 = 0.05254 0.00451 0.02225 -0.00524 AFIX 43 H4 2 0.438563 0.092452 0.507192 11.00000 -1.20000 AFIX 0 C5 1 0.430222 0.117960 0.369319 11.00000 0.04416 0.04830 = 0.04886 0.00621 0.02190 0.00305 AFIX 43 H5 2 0.348039 0.127768 0.351224 11.00000 -1.20000 AFIX 0 C6 1 0.493884 0.124439 0.298023 11.00000 0.05535 0.06225 = 0.06550 -0.00108 0.02948 -0.00465 PART 0 C7 1 0.436017 0.139952 0.189908 11.00000 0.04235 0.04180 = 0.05047 0.00162 0.01038 0.00315 C8 1 0.314208 0.161659 0.141565 11.00000 0.04179 0.04697 = 0.04858 -0.00157 0.00581 -0.00413 C9 1 0.254878 0.187018 0.205148 11.00000 0.04293 0.03838 = 0.05456 0.01727 0.01040 0.00465 C10 1 0.331782 0.211999 0.289223 11.00000 0.05216 0.05687 = 0.06570 0.00683 0.01982 0.00445 AFIX 43 H10 2 0.418822 0.210794 0.308764 11.00000 -1.20000 AFIX 0 C11 1 0.275117 0.239346 0.344641 11.00000 0.06689 0.05600 = 0.06334 0.00603 0.02475 0.00223 AFIX 43 H11 2 0.324883 0.255803 0.401817 11.00000 -1.20000 AFIX 0 C12 1 0.140858 0.241317 0.311652 11.00000 0.07116 0.06869 = 0.07357 0.00664 0.03263 0.00883 AFIX 43 H12 2 0.102166 0.259884 0.344995 11.00000 -1.20000 AFIX 0 C13 1 0.068063 0.214449 0.227263 11.00000 0.05815 0.07177 = 0.07451 0.01088 0.02408 0.00345 AFIX 43 H13 2 -0.019070 0.214997 0.207381 11.00000 -1.20000 AFIX 0 C14 1 0.120233 0.188299 0.175116 11.00000 0.05653 0.06656 = 0.05792 0.00908 0.01705 0.00059 AFIX 43 H14 2 0.069818 0.171099 0.119916 11.00000 -1.20000 AFIX 0 C15 1 0.316617 0.146972 -0.025223 11.00000 0.05463 0.05448 = 0.04884 0.00073 0.00144 0.00218 C16 1 0.251492 0.144637 -0.140485 11.00000 0.06288 0.06205 = 0.06172 -0.00419 0.00635 0.00567 AFIX 43 H16 2 0.167290 0.152441 -0.170125 11.00000 -1.20000 AFIX 0 C17 1 0.309413 0.132072 -0.199476 11.00000 0.08420 0.07788 = 0.06864 0.00275 0.01477 -0.00096 AFIX 43 H17 2 0.267430 0.133308 -0.273074 11.00000 -1.20000 AFIX 0 C18 1 0.439575 0.115410 -0.160964 11.00000 0.07564 0.06346 = 0.05917 0.00244 0.01964 -0.00202 AFIX 43 H18 2 0.477941 0.104707 -0.206973 11.00000 -1.20000 AFIX 0 C19 1 0.499094 0.116965 -0.052491 11.00000 0.05432 0.05544 = 0.04844 0.00002 0.01358 -0.00883 AFIX 43 H19 2 0.582777 0.108318 -0.027251 11.00000 -1.20000 AFIX 0 C20 1 0.448449 0.130330 0.027754 11.00000 0.03811 0.02730 = 0.05759 -0.01134 0.00666 -0.00174 C21 1 0.713198 0.066004 0.186524 11.00000 0.04020 0.03380 = 0.03621 -0.00416 0.01324 -0.00075 C22 1 0.619605 0.035643 0.138751 11.00000 0.04714 0.04985 = 0.04847 -0.00620 0.01538 -0.00643 AFIX 43 H22 2 0.535969 0.044329 0.115084 11.00000 -1.20000 AFIX 0 C23 1 0.644838 -0.004863 0.125769 11.00000 0.06397 0.05939 = 0.06338 -0.00226 0.01756 -0.00156 AFIX 43 H23 2 0.579957 -0.024189 0.095141 11.00000 -1.20000 AFIX 0 C24 1 0.775875 -0.018787 0.160177 11.00000 0.07230 0.05632 = 0.07112 -0.00433 0.02397 0.00254 AFIX 43 H24 2 0.795632 -0.047231 0.153628 11.00000 -1.20000 AFIX 0 C25 1 0.869880 0.011011 0.202586 11.00000 0.04835 0.02957 = 0.05611 -0.00547 0.01453 0.00554 AFIX 43 H25 2 0.953579 0.002899 0.220550 11.00000 -1.20000 AFIX 0 C26 1 0.840985 0.052827 0.218679 11.00000 0.04633 0.04466 = 0.04711 -0.00042 0.01719 -0.00286 C27 1 0.931933 0.084334 0.275406 11.00000 0.03026 0.03869 = 0.03674 -0.00009 0.00770 -0.00208 C28 1 1.066759 0.082227 0.308288 11.00000 0.03819 0.04013 = 0.03975 0.00280 0.01149 0.00409 C29 1 1.128618 0.053963 0.249197 11.00000 0.04547 0.05425 = 0.05765 -0.00609 0.02080 0.00826 C30 1 1.091498 0.053946 0.138997 11.00000 0.07608 0.07535 = 0.07203 -0.00458 0.03074 0.00964 AFIX 43 H30 2 1.020580 0.069630 0.100290 11.00000 -1.20000 AFIX 0 C31 1 1.152069 0.032589 0.085019 11.00000 0.09248 0.09773 = 0.09281 -0.00308 0.03875 0.00501 AFIX 43 H31 2 1.122963 0.032795 0.010600 11.00000 -1.20000 AFIX 0 C32 1 1.252728 0.011528 0.139327 11.00000 0.08334 0.08268 = 0.08391 -0.01065 0.03737 0.00712 AFIX 43 H32 2 1.295784 -0.002552 0.101213 11.00000 -1.20000 AFIX 0 C33 1 1.301280 0.008467 0.251381 11.00000 0.07592 0.08044 = 0.09375 -0.00532 0.03207 0.00772 AFIX 43 H33 2 1.372564 -0.007630 0.286897 11.00000 -1.20000 AFIX 0 C34 1 1.235179 0.031444 0.307971 11.00000 0.05955 0.06390 = 0.07077 -0.00239 0.02427 0.00303 AFIX 43 H34 2 1.263147 0.031243 0.382366 11.00000 -1.20000 AFIX 0 C35 1 1.085254 0.137263 0.419055 11.00000 0.02683 0.02473 = 0.04109 -0.00103 0.00295 -0.00600 C36 1 1.166490 0.163752 0.506824 11.00000 0.04015 0.05216 = 0.04339 0.00003 0.00975 -0.00390 AFIX 43 H36 2 1.251693 0.157537 0.538179 11.00000 -1.20000 AFIX 0 C37 1 1.114518 0.198438 0.542860 11.00000 0.04745 0.04932 = 0.04005 -0.00989 0.01303 -0.00648 AFIX 43 H37 2 1.165760 0.215702 0.597482 11.00000 -1.20000 AFIX 0 C38 1 0.987665 0.207183 0.497828 11.00000 0.04531 0.04514 = 0.04160 -0.00677 0.01694 0.00110 AFIX 43 H38 2 0.955147 0.230325 0.523351 11.00000 -1.20000 AFIX 0 C39 1 0.907600 0.182881 0.416520 11.00000 0.04028 0.04320 = 0.03217 0.00457 0.01180 -0.00129 AFIX 43 H39 2 0.822581 0.189511 0.386066 11.00000 -1.20000 AFIX 0 C40 1 0.957824 0.148619 0.382222 11.00000 0.02019 0.01933 = 0.02026 -0.00087 0.00654 -0.00078 C41 1 0.642568 0.225613 0.171671 11.00000 0.03748 0.03324 = 0.03797 0.00032 0.01014 0.00115 C42 1 0.586830 0.263280 0.192533 11.00000 0.04429 0.04651 = 0.04562 0.00372 0.00899 0.00506 AFIX 43 H42 2 0.561041 0.264469 0.251449 11.00000 -1.20000 AFIX 0 C43 1 0.570130 0.298531 0.126085 11.00000 0.06675 0.05309 = 0.06680 0.00064 0.01773 0.00544 AFIX 43 H43 2 0.536022 0.323420 0.142560 11.00000 -1.20000 AFIX 0 C44 1 0.602885 0.297328 0.036924 11.00000 0.06442 0.05234 = 0.06665 0.00759 0.01688 0.00405 AFIX 43 H44 2 0.585639 0.320847 -0.008513 11.00000 -1.20000 AFIX 0 C45 1 0.657052 0.264497 0.013981 11.00000 0.05740 0.05364 = 0.05771 0.00205 0.01740 -0.00126 AFIX 43 H45 2 0.682012 0.265255 -0.045417 11.00000 -1.20000 AFIX 0 C46 1 0.679741 0.226028 0.080339 11.00000 0.04041 0.03797 = 0.04328 0.00365 0.01038 -0.00299 PART 1 C47 1 0.737201 0.189654 0.050497 11.00000 0.03283 0.03501 = 0.03158 0.00433 0.00613 -0.00522 C48 1 0.822092 0.151950 -0.040998 11.00000 0.04030 0.04204 = 0.03754 0.00412 0.01032 -0.00023 N5 4 0.754864 0.151880 0.089178 11.00000 0.04007 0.04080 = 0.03573 -0.00442 0.01520 -0.00687 N6 4 0.809934 0.127188 0.030272 11.00000 0.05064 0.05152 = 0.04366 0.00411 0.01973 0.00397 O2 5 0.776692 0.191924 -0.034738 11.00000 0.05340 0.04131 = 0.05042 0.00709 0.02238 -0.00005 PART 0 C49 1 0.861791 0.143253 -0.132690 11.00000 0.04406 0.04898 = 0.04923 0.00657 0.01608 -0.00297 C50 1 0.875694 0.176627 -0.194048 11.00000 0.05717 0.06288 = 0.05764 0.00752 0.02571 0.00227 AFIX 43 H50 2 0.866079 0.204713 -0.175562 11.00000 -1.20000 AFIX 0 C51 1 0.905733 0.166932 -0.288330 11.00000 0.06529 0.07293 = 0.06189 0.00409 0.02535 0.00093 AFIX 43 H51 2 0.909980 0.188782 -0.334183 11.00000 -1.20000 AFIX 0 C52 1 0.927196 0.127003 -0.309466 11.00000 0.07241 0.07778 = 0.06835 -0.00453 0.02844 -0.00288 AFIX 43 H52 2 0.947299 0.120980 -0.369874 11.00000 -1.20000 AFIX 0 C53 1 0.919822 0.093248 -0.240760 11.00000 0.08262 0.08056 = 0.08071 -0.00563 0.03040 0.00741 AFIX 43 H53 2 0.937293 0.065351 -0.255025 11.00000 -1.20000 AFIX 0 C54 1 0.886330 0.102109 -0.151986 11.00000 0.06233 0.05114 = 0.05425 -0.00087 0.01664 0.00171 AFIX 43 H54 2 0.880801 0.080271 -0.106567 11.00000 -1.20000 AFIX 0 IR1 3 0.690928 0.127143 0.212419 11.00000 0.02986 0.02996 = 0.02835 0.00161 0.00496 -0.00062 N1 4 0.500348 0.133971 0.121717 11.00000 0.04521 0.02865 = 0.05265 0.00291 0.01754 0.00260 N2 4 0.255067 0.163138 0.036392 11.00000 0.04997 0.05745 = 0.05555 0.00437 0.00769 0.00746 AFIX 2 N3 4 0.879241 0.119492 0.300499 11.00000 0.01058 0.01011 = 0.00959 -0.00048 0.00245 -0.00025 AFIX 0 N4 4 1.140628 0.105206 0.384841 11.00000 0.03647 0.04457 = 0.04897 0.00175 0.01254 0.00854 O1 5 0.661969 0.194400 0.239625 11.00000 0.04961 0.02547 = 0.03395 0.00064 0.01144 0.00127 HKLF 4 REM 20161228ZYX_DP_0m in P2(1)/c REM R1 = 0.1040 for 6215 Fo > 4sig(Fo) and 0.1210 for all 7779 data REM 562 parameters refined using 360 restraints END WGHT 0.0304 257.1681 REM Highest difference peak 5.635, deepest hole -6.532, 1-sigma level 0.256 Q1 1 0.7157 0.1232 0.4604 11.00000 0.05 5.63 Q2 1 0.9053 0.1240 0.1180 11.00000 0.05 5.34 Q3 1 0.3279 0.1389 0.2854 11.00000 0.05 2.26 Q4 1 0.9759 0.1312 0.4175 11.00000 0.05 1.41 Q5 1 0.8119 0.1262 0.2668 11.00000 0.05 1.20 Q6 1 0.4207 0.1270 0.0744 11.00000 0.05 1.17 Q7 1 0.6179 0.1203 0.2216 11.00000 0.05 1.15 Q8 1 0.9220 0.0966 0.3472 11.00000 0.05 1.14 Q9 1 0.5266 0.1255 0.3774 11.00000 0.05 1.11 Q10 1 0.9241 0.1198 0.2824 11.00000 0.05 1.10 REM The information below was added by Olex2. REM REM R1 = 0.1040 for 6215 Fo > 4sig(Fo) and 0.1210 for all 30007 data REM n/a parameters refined using n/a restraints REM Highest difference peak 5.63, deepest hole -6.53 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1210 REM R1_gt = 0.1040 REM wR_ref = 0.2655 REM GOOF = 1.133 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 30007 REM Reflections_gt = 6215 REM Parameters = n/a REM Hole = -6.53 REM Peak = 5.63 REM Flack = n/a ; _cod_data_source_file c7ra05530g2.cif _cod_data_source_block 1_sq _cod_original_cell_volume 4439.4(13) _cod_database_code 7228791 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.594 _shelx_estimated_absorpt_t_min 0.492 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2. Uiso/Uaniso restraints and constraints Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(N6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C40) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002 3.a Fixed occupancy and ADP/Uiso: N3 3.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24), C25(H25), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C42(H42), C43(H43), C44(H44), C45(H45), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54) ; _shelx_fab_file ; -13 0 2 3.1183 0.0000 -13 0 4 1.8391 0.0000 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26 0 -0.5420 0.0000 8 26 1 3.2526 0.0000 8 26 2 0.4942 0.0000 8 27 0 -4.7594 0.0000 8 27 1 0.2966 0.0000 8 28 0 -2.4693 0.0000 8 28 1 2.0691 0.0000 9 0 0 -1.0633 0.0000 9 0 2 0.6271 0.0000 9 0 4 -2.2727 0.0000 9 0 6 -3.3286 0.0000 9 1 0 -0.5230 0.0000 9 1 1 0.6932 0.0000 9 1 2 0.5791 0.0000 9 1 3 -0.5795 0.0000 9 1 4 -0.6480 0.0000 9 1 5 4.7726 0.0000 9 1 6 0.4364 0.0000 9 1 7 -0.8842 0.0000 9 2 0 -1.2365 0.0000 9 2 1 -0.2575 0.0000 9 2 2 0.9114 0.0000 9 2 3 -0.1205 0.0000 9 2 4 -2.1364 0.0000 9 2 5 0.7876 0.0000 9 2 6 -3.3429 0.0000 9 2 7 -0.4327 0.0000 9 3 0 -0.9477 0.0000 9 3 1 -0.0821 0.0000 9 3 2 1.4322 0.0000 9 3 3 -0.3697 0.0000 9 3 4 -1.8401 0.0000 9 3 5 3.7349 0.0000 9 3 6 0.9743 0.0000 9 3 7 0.9411 0.0000 9 4 0 -1.6706 0.0000 9 4 1 -0.7603 0.0000 9 4 2 1.4003 0.0000 9 4 3 0.0330 0.0000 9 4 4 -1.7698 0.0000 9 4 5 1.6396 0.0000 9 4 6 -2.7769 0.0000 9 4 7 -1.1677 0.0000 9 5 0 -0.2635 0.0000 9 5 1 -0.8907 0.0000 9 5 2 1.6280 0.0000 9 5 3 0.0699 0.0000 9 5 4 -2.4627 0.0000 9 5 5 1.7639 0.0000 9 5 6 0.6570 0.0000 9 5 7 2.5830 0.0000 9 6 0 -2.0073 0.0000 9 6 1 -1.3646 0.0000 9 6 2 1.6664 0.0000 9 6 3 0.2692 0.0000 9 6 4 -1.2870 0.0000 9 6 5 2.1726 0.0000 9 6 6 -1.0606 0.0000 9 6 7 -1.2978 0.0000 9 7 0 0.7934 0.0000 9 7 1 -1.3895 0.0000 9 7 2 1.2848 0.0000 9 7 3 0.3712 0.0000 9 7 4 -2.0939 0.0000 9 7 5 -0.2770 0.0000 9 7 6 -0.7244 0.0000 9 7 7 2.6459 0.0000 9 8 0 -1.5894 0.0000 9 8 1 -1.7727 0.0000 9 8 2 1.9839 0.0000 9 8 3 0.4283 0.0000 9 8 4 -0.8541 0.0000 9 8 5 2.2295 0.0000 9 8 6 0.7385 0.0000 9 9 0 1.3380 0.0000 9 9 1 -2.0666 0.0000 9 9 2 0.6989 0.0000 9 9 3 0.0211 0.0000 9 9 4 -1.3490 0.0000 9 9 5 -1.0108 0.0000 9 9 6 -3.0076 0.0000 9 10 0 0.0763 0.0000 9 10 1 -1.9079 0.0000 9 10 2 2.7186 0.0000 9 10 3 0.9115 0.0000 9 10 4 -0.6374 0.0000 9 10 5 2.4717 0.0000 9 10 6 0.8736 0.0000 9 11 0 1.2780 0.0000 9 11 1 -3.2465 0.0000 9 11 2 0.0248 0.0000 9 11 3 -0.8207 0.0000 9 11 4 -1.5403 0.0000 9 11 5 0.0547 0.0000 9 11 6 -5.4808 0.0000 9 12 0 2.5779 0.0000 9 12 1 -1.8013 0.0000 9 12 2 3.3492 0.0000 9 12 3 2.0230 0.0000 9 12 4 -0.6716 0.0000 9 12 5 3.4864 0.0000 9 12 6 -0.7897 0.0000 9 13 0 1.0015 0.0000 9 13 1 -4.2348 0.0000 9 13 2 -0.6015 0.0000 9 13 3 -1.3007 0.0000 9 13 4 -2.8796 0.0000 9 13 5 1.8324 0.0000 9 13 6 -6.9302 0.0000 9 14 0 4.4734 0.0000 9 14 1 -1.3951 0.0000 9 14 2 2.9362 0.0000 9 14 3 2.9984 0.0000 9 14 4 -0.7930 0.0000 9 14 5 4.6268 0.0000 9 15 0 0.7099 0.0000 9 15 1 -3.9853 0.0000 9 15 2 -0.7750 0.0000 9 15 3 -0.9067 0.0000 9 15 4 -3.8714 0.0000 9 15 5 2.8287 0.0000 9 16 0 4.3158 0.0000 9 16 1 -0.8011 0.0000 9 16 2 1.4711 0.0000 9 16 3 2.5289 0.0000 9 16 4 -0.8391 0.0000 9 16 5 4.6237 0.0000 9 17 0 0.4084 0.0000 9 17 1 -2.3825 0.0000 9 17 2 -0.0440 0.0000 9 17 3 -0.0447 0.0000 9 17 4 -3.1395 0.0000 9 17 5 2.6936 0.0000 9 18 0 2.0217 0.0000 9 18 1 -0.4803 0.0000 9 18 2 -0.0010 0.0000 9 18 3 0.4348 0.0000 9 18 4 -0.9108 0.0000 9 19 0 0.1221 0.0000 9 19 1 -0.4051 0.0000 9 19 2 1.4257 0.0000 9 19 3 0.6443 0.0000 9 19 4 -1.1950 0.0000 9 20 0 -0.9103 0.0000 9 20 1 -0.7192 0.0000 9 20 2 -0.6498 0.0000 9 20 3 -1.8490 0.0000 9 21 0 -0.2535 0.0000 9 21 1 0.8731 0.0000 9 21 2 2.7124 0.0000 9 21 3 1.0186 0.0000 9 22 0 -2.6962 0.0000 9 22 1 -1.1308 0.0000 9 22 2 -0.5764 0.0000 9 22 3 -2.8140 0.0000 9 23 0 -0.9243 0.0000 9 23 1 1.0696 0.0000 9 23 2 3.0027 0.0000 9 24 0 -2.7120 0.0000 9 24 1 -1.1827 0.0000 9 25 0 -1.6234 0.0000 9 25 1 0.4284 0.0000 9 26 0 -1.6356 0.0000 10 0 0 2.5055 0.0000 10 0 2 0.4959 0.0000 10 1 0 0.5940 0.0000 10 1 1 -3.1470 0.0000 10 1 2 -1.5905 0.0000 10 1 3 4.4010 0.0000 10 1 4 -0.4482 0.0000 10 1 5 1.3521 0.0000 10 2 0 2.2186 0.0000 10 2 1 0.1064 0.0000 10 2 2 -0.1369 0.0000 10 2 3 3.4435 0.0000 10 2 4 -4.2272 0.0000 10 2 5 -1.4949 0.0000 10 3 0 1.3355 0.0000 10 3 1 -1.2443 0.0000 10 3 2 -3.5838 0.0000 10 3 3 2.6856 0.0000 10 3 4 -0.7876 0.0000 10 3 5 -0.1541 0.0000 10 4 0 1.3441 0.0000 10 4 1 0.1508 0.0000 10 4 2 -1.4241 0.0000 10 4 3 4.2652 0.0000 10 4 4 -0.2859 0.0000 10 4 5 -2.3877 0.0000 10 5 0 1.1270 0.0000 10 5 1 1.1763 0.0000 10 5 2 -2.9897 0.0000 10 5 3 0.2988 0.0000 10 5 4 -0.3669 0.0000 10 5 5 -1.8172 0.0000 10 6 0 0.2343 0.0000 10 6 1 -0.0415 0.0000 10 6 2 -2.3132 0.0000 10 6 3 2.3766 0.0000 10 6 4 3.0368 0.0000 10 6 5 -1.7932 0.0000 10 7 0 0.2064 0.0000 10 7 1 2.4339 0.0000 10 7 2 -0.5801 0.0000 10 7 3 -1.0383 0.0000 10 7 4 -0.3018 0.0000 10 7 5 -2.3264 0.0000 10 8 0 -0.1384 0.0000 10 8 1 -0.3357 0.0000 10 8 2 -2.5140 0.0000 10 8 3 0.0298 0.0000 10 8 4 3.4960 0.0000 10 8 5 0.4857 0.0000 10 9 0 -0.8059 0.0000 10 9 1 1.8502 0.0000 10 9 2 1.3526 0.0000 10 9 3 -0.1853 0.0000 10 9 4 -1.3170 0.0000 10 9 5 -1.6412 0.0000 10 10 0 0.9071 0.0000 10 10 1 -0.1119 0.0000 10 10 2 -2.4380 0.0000 10 10 3 -0.7387 0.0000 10 10 4 1.2414 0.0000 10 10 5 3.0181 0.0000 10 11 0 -1.4073 0.0000 10 11 1 0.1391 0.0000 10 11 2 1.1592 0.0000 10 11 3 2.0690 0.0000 10 11 4 -2.4446 0.0000 10 12 0 2.7044 0.0000 10 12 1 0.9228 0.0000 10 12 2 -2.1652 0.0000 10 12 3 -0.0554 0.0000 10 12 4 -1.4665 0.0000 10 13 0 -1.3523 0.0000 10 13 1 -1.4257 0.0000 10 13 2 -0.5517 0.0000 10 13 3 3.4413 0.0000 10 13 4 -2.1719 0.0000 10 14 0 3.7368 0.0000 10 14 1 1.9454 0.0000 10 14 2 -1.1892 0.0000 10 14 3 0.5197 0.0000 10 14 4 -2.5257 0.0000 10 15 0 -0.6286 0.0000 10 15 1 -2.1338 0.0000 10 15 2 -1.7077 0.0000 10 15 3 2.4702 0.0000 10 16 0 3.2538 0.0000 10 16 1 1.7211 0.0000 10 16 2 0.5947 0.0000 10 16 3 0.1749 0.0000 10 17 0 0.4218 0.0000 10 17 1 -2.1040 0.0000 10 17 2 -1.1606 0.0000 10 17 3 0.1158 0.0000 10 18 0 1.9009 0.0000 10 18 1 0.1794 0.0000 10 18 2 2.2261 0.0000 10 19 0 1.1133 0.0000 10 19 1 -1.6953 0.0000 10 19 2 0.1755 0.0000 10 20 0 0.6956 0.0000 10 20 1 -1.3161 0.0000 10 21 0 0.9281 0.0000 10 21 1 -1.0501 0.0000 10 22 0 -0.0545 0.0000 11 0 0 1.8331 0.0000 11 0 2 -5.0682 0.0000 11 0 4 -4.6118 0.0000 11 1 0 -0.2380 0.0000 11 1 1 1.4891 0.0000 11 1 2 -0.9173 0.0000 11 1 3 4.9050 0.0000 11 1 4 0.7177 0.0000 11 2 0 1.1199 0.0000 11 2 1 2.1649 0.0000 11 2 2 -3.0965 0.0000 11 2 3 -0.6104 0.0000 11 2 4 -2.9885 0.0000 11 3 0 -0.0100 0.0000 11 3 1 0.6492 0.0000 11 3 2 -1.3668 0.0000 11 3 3 0.8934 0.0000 11 3 4 1.2943 0.0000 11 4 0 -0.2710 0.0000 11 4 1 1.5437 0.0000 11 4 2 0.9727 0.0000 11 4 3 -1.2593 0.0000 11 5 0 1.4128 0.0000 11 5 1 -0.5128 0.0000 11 5 2 0.3367 0.0000 11 5 3 -2.8352 0.0000 11 6 0 -1.0770 0.0000 11 6 1 -1.2211 0.0000 11 6 2 3.5180 0.0000 11 6 3 -1.1349 0.0000 11 7 0 2.9110 0.0000 11 7 1 -1.0665 0.0000 11 7 2 1.8523 0.0000 11 7 3 -2.8284 0.0000 11 8 0 -1.0191 0.0000 11 8 1 -3.0642 0.0000 11 8 2 2.7158 0.0000 11 8 3 0.4233 0.0000 11 9 0 3.0320 0.0000 11 9 1 -0.3489 0.0000 11 9 2 1.0793 0.0000 11 9 3 -0.1146 0.0000 11 10 0 -0.7129 0.0000 11 10 1 -2.3616 0.0000 11 10 2 -0.0826 0.0000 11 10 3 2.4330 0.0000 11 11 0 1.6275 0.0000 11 11 1 1.1562 0.0000 11 11 2 -0.8969 0.0000 11 12 0 -0.4184 0.0000 11 12 1 -0.5293 0.0000 11 12 2 -2.2029 0.0000 11 13 0 -0.0760 0.0000 11 13 1 1.9517 0.0000 11 13 2 -1.3550 0.0000 11 14 0 0.3084 0.0000 11 14 1 0.2586 0.0000 11 14 2 -2.2259 0.0000 11 15 0 -0.8712 0.0000 11 15 1 0.9149 0.0000 11 16 0 1.6560 0.0000 11 16 1 -0.2681 0.0000 11 17 0 -0.6756 0.0000 11 18 0 2.9591 0.0000 12 0 0 0.9745 0.0000 12 1 0 -0.1422 0.0000 12 1 1 -0.5963 0.0000 12 2 0 1.4121 0.0000 12 2 1 0.4264 0.0000 12 3 0 0.0933 0.0000 12 3 1 -2.0640 0.0000 12 4 0 2.0020 0.0000 12 4 1 0.5130 0.0000 12 5 0 0.7213 0.0000 12 5 1 -2.3878 0.0000 12 6 0 1.7020 0.0000 12 6 1 0.8893 0.0000 12 7 0 0.0992 0.0000 12 7 1 -0.2641 0.0000 12 8 0 0.7312 0.0000 12 8 1 2.5083 0.0000 12 9 0 -2.4961 0.0000 12 10 0 0.1346 0.0000 12 11 0 -5.3419 0.0000 0 0 0 0.0 0.0 ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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_disorder_assembly _atom_site_disorder_group C1 C 0.6178(16) 0.1127(5) 0.3226(14) 0.032(4) Uani 1 1 d . U A 1 C2 C 0.679(2) 0.0946(7) 0.4272(17) 0.047(5) Uani 1 1 d . U A 1 H2 H 0.7647 0.0887 0.4509 0.057 Uiso 1 1 calc R . A 1 C3 C 0.611(2) 0.0860(7) 0.4916(17) 0.049(5) Uani 1 1 d . U A 1 H3 H 0.6494 0.0718 0.5561 0.059 Uiso 1 1 calc R . A 1 C4 C 0.484(2) 0.0981(7) 0.4625(18) 0.050(5) Uani 1 1 d . U A 1 H4 H 0.4386 0.0925 0.5072 0.061 Uiso 1 1 calc R . A 1 C5 C 0.430(2) 0.1180(6) 0.3693(17) 0.046(5) Uani 1 1 d . U A 1 H5 H 0.3480 0.1278 0.3512 0.055 Uiso 1 1 calc R . A 1 C6 C 0.494(2) 0.1244(8) 0.298(2) 0.059(6) Uani 1 1 d . U A 1 C7 C 0.4360(19) 0.1400(6) 0.1899(17) 0.046(5) Uani 1 1 d . U . . C8 C 0.314(2) 0.1617(7) 0.1416(17) 0.048(5) Uani 1 1 d . U . . C9 C 0.2549(19) 0.1870(6) 0.2051(18) 0.047(5) Uani 1 1 d . U . . C10 C 0.332(2) 0.2120(7) 0.289(2) 0.058(6) Uani 1 1 d . U . . H10 H 0.4188 0.2108 0.3088 0.070 Uiso 1 1 calc R . . . C11 C 0.275(2) 0.2393(8) 0.345(2) 0.062(6) Uani 1 1 d . U . . H11 H 0.3249 0.2558 0.4018 0.074 Uiso 1 1 calc R . . . C12 C 0.141(3) 0.2413(9) 0.312(2) 0.069(7) Uani 1 1 d . U . . H12 H 0.1022 0.2599 0.3450 0.083 Uiso 1 1 calc R . . . C13 C 0.068(2) 0.2144(9) 0.227(2) 0.068(7) Uani 1 1 d . U . . H13 H -0.0191 0.2150 0.2074 0.081 Uiso 1 1 calc R . . . C14 C 0.120(2) 0.1883(8) 0.175(2) 0.061(6) Uani 1 1 d . U . . H14 H 0.0698 0.1711 0.1199 0.073 Uiso 1 1 calc R . . . C15 C 0.317(2) 0.1470(8) -0.0252(19) 0.057(6) Uani 1 1 d . U . . C16 C 0.251(3) 0.1446(8) -0.140(2) 0.066(7) Uani 1 1 d . U . . H16 H 0.1673 0.1524 -0.1701 0.080 Uiso 1 1 calc R . . . C17 C 0.309(3) 0.1321(9) -0.199(2) 0.080(8) Uani 1 1 d . U . . H17 H 0.2674 0.1333 -0.2731 0.096 Uiso 1 1 calc R . . . C18 C 0.440(3) 0.1154(8) -0.161(2) 0.067(7) Uani 1 1 d . U . . H18 H 0.4779 0.1047 -0.2070 0.081 Uiso 1 1 calc R . . . C19 C 0.499(2) 0.1170(7) -0.0525(18) 0.054(6) Uani 1 1 d . U . . H19 H 0.5828 0.1083 -0.0273 0.065 Uiso 1 1 calc R . . . C20 C 0.4484(18) 0.1303(6) 0.0278(17) 0.044(5) Uani 1 1 d . U . . C21 C 0.7132(18) 0.0660(6) 0.1865(15) 0.037(4) Uani 1 1 d . U . . C22 C 0.620(2) 0.0356(7) 0.1388(17) 0.049(5) Uani 1 1 d . U . . H22 H 0.5360 0.0443 0.1151 0.059 Uiso 1 1 calc R . . . C23 C 0.645(2) -0.0049(8) 0.126(2) 0.063(6) Uani 1 1 d . U . . H23 H 0.5800 -0.0242 0.0951 0.076 Uiso 1 1 calc R . . . C24 C 0.776(2) -0.0188(8) 0.160(2) 0.067(7) Uani 1 1 d . U . . H24 H 0.7956 -0.0472 0.1536 0.080 Uiso 1 1 calc R . . . C25 C 0.870(2) 0.0110(6) 0.2026(17) 0.046(5) Uani 1 1 d . U . . H25 H 0.9536 0.0029 0.2205 0.055 Uiso 1 1 calc R . . . C26 C 0.841(2) 0.0528(7) 0.2187(17) 0.046(5) Uani 1 1 d . U . . C27 C 0.9319(17) 0.0843(6) 0.2754(15) 0.036(4) Uani 1 1 d . U . . C28 C 1.0668(18) 0.0822(6) 0.3083(16) 0.040(4) Uani 1 1 d . U . . C29 C 1.129(2) 0.0540(7) 0.2492(19) 0.052(5) Uani 1 1 d . U . . C30 C 1.091(3) 0.0539(9) 0.139(2) 0.073(7) Uani 1 1 d . U . . H30 H 1.0206 0.0696 0.1003 0.088 Uiso 1 1 calc R . . . C31 C 1.152(3) 0.0326(11) 0.085(3) 0.093(9) Uani 1 1 d . U . . H31 H 1.1230 0.0328 0.0106 0.111 Uiso 1 1 calc R . . . C32 C 1.253(3) 0.0115(10) 0.139(2) 0.081(8) Uani 1 1 d . U . . H32 H 1.2958 -0.0026 0.1012 0.097 Uiso 1 1 calc R . . . C33 C 1.301(3) 0.0085(10) 0.251(3) 0.083(8) Uani 1 1 d . U . . H33 H 1.3726 -0.0076 0.2869 0.099 Uiso 1 1 calc R . . . C34 C 1.235(2) 0.0314(8) 0.308(2) 0.064(6) Uani 1 1 d . U . . H34 H 1.2631 0.0312 0.3824 0.077 Uiso 1 1 calc R . . . C35 C 1.0853(16) 0.1373(5) 0.4191(15) 0.033(4) Uani 1 1 d . U . . C36 C 1.166(2) 0.1638(7) 0.5068(16) 0.047(5) Uani 1 1 d . U . . H36 H 1.2517 0.1575 0.5382 0.056 Uiso 1 1 calc R . . . C37 C 1.115(2) 0.1984(7) 0.5429(16) 0.046(5) Uani 1 1 d . U . . H37 H 1.1658 0.2157 0.5975 0.055 Uiso 1 1 calc R . . . C38 C 0.9877(19) 0.2072(7) 0.4978(16) 0.044(5) Uani 1 1 d . U . . H38 H 0.9551 0.2303 0.5234 0.052 Uiso 1 1 calc R . . . C39 C 0.9076(19) 0.1829(6) 0.4165(15) 0.039(4) Uani 1 1 d . U . . H39 H 0.8226 0.1895 0.3861 0.047 Uiso 1 1 calc R . . . C40 C 0.9578(14) 0.1486(5) 0.3822(12) 0.020(3) Uani 1 1 d . U . . C41 C 0.6426(18) 0.2256(6) 0.1717(15) 0.037(4) Uani 1 1 d . U . . C42 C 0.5868(19) 0.2633(7) 0.1925(17) 0.047(5) Uani 1 1 d . U . . H42 H 0.5610 0.2645 0.2514 0.057 Uiso 1 1 calc R . . . C43 C 0.570(2) 0.2985(8) 0.126(2) 0.064(6) Uani 1 1 d . U . . H43 H 0.5360 0.3234 0.1426 0.076 Uiso 1 1 calc R . . . C44 C 0.603(2) 0.2973(8) 0.037(2) 0.063(6) Uani 1 1 d . U . . H44 H 0.5856 0.3208 -0.0085 0.075 Uiso 1 1 calc R . . . C45 C 0.657(2) 0.2645(7) 0.014(2) 0.057(6) Uani 1 1 d . U . . H45 H 0.6820 0.2653 -0.0454 0.068 Uiso 1 1 calc R . . . C46 C 0.6797(18) 0.2260(6) 0.0803(16) 0.042(5) Uani 1 1 d . U . . C47 C 0.7372(17) 0.1897(6) 0.0505(14) 0.035(4) Uani 1 1 d . U B 1 C48 C 0.8221(18) 0.1520(6) -0.0410(16) 0.041(4) Uani 1 1 d . U B 1 N5 N 0.7549(15) 0.1519(5) 0.0892(12) 0.038(4) Uani 1 1 d . U B 1 N6 N 0.8099(16) 0.1272(6) 0.0303(13) 0.048(4) Uani 1 1 d . U B 1 O2 O 0.7767(13) 0.1919(4) -0.0347(11) 0.047(3) Uani 1 1 d . . B 1 C49 C 0.862(2) 0.1433(7) -0.1327(17) 0.047(5) Uani 1 1 d . U . . C50 C 0.876(2) 0.1766(8) -0.1940(19) 0.058(6) Uani 1 1 d . U . . H50 H 0.8661 0.2047 -0.1756 0.069 Uiso 1 1 calc R . . . C51 C 0.906(2) 0.1669(9) -0.288(2) 0.066(7) Uani 1 1 d . U . . H51 H 0.9100 0.1888 -0.3342 0.079 Uiso 1 1 calc R . . . C52 C 0.927(3) 0.1270(9) -0.309(2) 0.072(7) Uani 1 1 d . U . . H52 H 0.9473 0.1210 -0.3699 0.086 Uiso 1 1 calc R . . . C53 C 0.920(3) 0.0932(10) -0.241(2) 0.081(8) Uani 1 1 d . U . . H53 H 0.9373 0.0654 -0.2550 0.097 Uiso 1 1 calc R . . . C54 C 0.886(2) 0.1021(8) -0.1520(19) 0.057(6) Uani 1 1 d . U . . H54 H 0.8808 0.0803 -0.1066 0.068 Uiso 1 1 calc R . . . Ir1 Ir 0.69093(7) 0.12714(2) 0.21242(6) 0.0308(2) Uani 1 1 d . . . . N1 N 0.5003(16) 0.1340(5) 0.1217(14) 0.042(4) Uani 1 1 d . U . . N2 N 0.2551(18) 0.1631(6) 0.0364(16) 0.057(5) Uani 1 1 d . U . . N3 N 0.8792(10) 0.1195(3) 0.3005(8) 0.010 Uani 1 1 d . U . . N4 N 1.1406(15) 0.1052(5) 0.3848(14) 0.044(4) Uani 1 1 d . U . . O1 O 0.6620(12) 0.1944(4) 0.2396(10) 0.037(3) Uani 1 1 d . . . . 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 C1 0.031(7) 0.024(7) 0.032(7) 0.002(6) 0.001(6) -0.003(6) C2 0.047(5) 0.047(5) 0.047(5) 0.0004(10) 0.0165(19) 0.0001(10) C3 0.048(8) 0.052(9) 0.043(8) 0.008(7) 0.011(7) 0.004(7) C4 0.051(9) 0.051(9) 0.053(9) 0.005(7) 0.022(7) -0.005(7) C5 0.044(8) 0.048(9) 0.049(8) 0.006(7) 0.022(7) 0.003(7) C6 0.055(9) 0.062(10) 0.066(9) -0.001(8) 0.029(8) -0.005(8) C7 0.042(8) 0.042(8) 0.050(9) 0.002(7) 0.010(7) 0.003(7) C8 0.042(8) 0.047(8) 0.049(9) -0.002(7) 0.006(7) -0.004(7) C9 0.043(8) 0.038(8) 0.055(9) 0.017(7) 0.010(7) 0.005(7) C10 0.052(9) 0.057(9) 0.066(10) 0.007(8) 0.020(8) 0.004(7) C11 0.067(10) 0.056(9) 0.063(10) 0.006(8) 0.025(8) 0.002(8) C12 0.071(10) 0.069(10) 0.074(10) 0.007(8) 0.033(8) 0.009(8) C13 0.058(10) 0.072(10) 0.075(10) 0.011(8) 0.024(8) 0.003(8) C14 0.057(9) 0.067(10) 0.058(10) 0.009(8) 0.017(8) 0.001(8) C15 0.055(9) 0.054(9) 0.049(9) 0.001(7) 0.001(7) 0.002(8) C16 0.063(10) 0.062(10) 0.062(10) -0.004(8) 0.006(8) 0.006(8) C17 0.084(11) 0.078(11) 0.069(11) 0.003(9) 0.015(8) -0.001(9) C18 0.076(10) 0.063(10) 0.059(10) 0.002(8) 0.020(8) -0.002(8) C19 0.054(9) 0.055(9) 0.048(9) 0.000(7) 0.014(7) -0.009(7) C20 0.038(8) 0.027(7) 0.058(9) -0.011(7) 0.007(7) -0.002(6) C21 0.040(8) 0.034(7) 0.036(8) -0.004(6) 0.013(6) -0.001(6) C22 0.047(8) 0.050(9) 0.048(9) -0.006(7) 0.015(7) -0.006(7) C23 0.064(10) 0.059(10) 0.063(10) -0.002(8) 0.018(8) -0.002(8) C24 0.072(10) 0.056(10) 0.071(10) -0.004(8) 0.024(8) 0.003(8) C25 0.048(8) 0.030(8) 0.056(9) -0.005(7) 0.015(7) 0.006(7) C26 0.046(8) 0.045(8) 0.047(8) 0.000(7) 0.017(7) -0.003(7) C27 0.030(7) 0.039(8) 0.037(8) 0.000(6) 0.008(6) -0.002(6) C28 0.038(8) 0.040(8) 0.040(8) 0.003(7) 0.011(6) 0.004(7) C29 0.045(8) 0.054(9) 0.058(9) -0.006(7) 0.021(7) 0.008(7) C30 0.076(11) 0.075(11) 0.072(11) -0.005(8) 0.031(8) 0.010(8) C31 0.092(12) 0.098(13) 0.093(12) -0.003(9) 0.039(9) 0.005(9) C32 0.083(11) 0.083(12) 0.084(11) -0.011(9) 0.037(9) 0.007(9) C33 0.076(11) 0.080(11) 0.094(12) -0.005(9) 0.032(9) 0.008(9) C34 0.060(10) 0.064(10) 0.071(10) -0.002(8) 0.024(8) 0.003(8) C35 0.027(7) 0.025(7) 0.041(8) -0.001(6) 0.003(6) -0.006(6) C36 0.040(8) 0.052(9) 0.043(8) 0.000(7) 0.010(7) -0.004(7) C37 0.047(8) 0.049(8) 0.040(8) -0.010(7) 0.013(7) -0.006(7) C38 0.045(8) 0.045(8) 0.042(8) -0.007(7) 0.017(7) 0.001(7) C39 0.040(8) 0.043(8) 0.032(8) 0.005(6) 0.012(6) -0.001(7) C40 0.020(3) 0.019(3) 0.020(3) -0.0009(10) 0.0065(14) -0.0008(10) C41 0.037(8) 0.033(7) 0.038(8) 0.000(6) 0.010(6) 0.001(6) C42 0.044(8) 0.047(8) 0.046(8) 0.004(7) 0.009(7) 0.005(7) C43 0.067(10) 0.053(9) 0.067(10) 0.001(8) 0.018(8) 0.005(8) C44 0.064(10) 0.052(9) 0.067(10) 0.008(8) 0.017(8) 0.004(8) C45 0.057(9) 0.054(9) 0.058(9) 0.002(8) 0.017(7) -0.001(8) C46 0.040(8) 0.038(8) 0.043(8) 0.004(7) 0.010(7) -0.003(7) C47 0.033(7) 0.035(7) 0.032(7) 0.004(6) 0.006(6) -0.005(6) C48 0.040(8) 0.042(8) 0.038(8) 0.004(7) 0.010(6) 0.000(7) N5 0.040(7) 0.041(7) 0.036(7) -0.004(6) 0.015(6) -0.007(6) N6 0.051(8) 0.052(8) 0.044(7) 0.004(7) 0.020(6) 0.004(7) O2 0.053(9) 0.041(8) 0.050(9) 0.007(7) 0.022(7) 0.000(7) C49 0.044(8) 0.049(8) 0.049(9) 0.007(7) 0.016(7) -0.003(7) C50 0.057(9) 0.063(10) 0.058(9) 0.008(8) 0.026(8) 0.002(8) C51 0.065(10) 0.073(10) 0.062(10) 0.004(8) 0.025(8) 0.001(8) C52 0.072(10) 0.078(11) 0.068(10) -0.005(8) 0.028(8) -0.003(8) C53 0.083(11) 0.081(11) 0.081(11) -0.006(9) 0.030(9) 0.007(9) C54 0.062(9) 0.051(9) 0.054(9) -0.001(7) 0.017(7) 0.002(7) Ir1 0.0299(4) 0.0300(4) 0.0284(4) 0.0016(3) 0.0050(3) -0.0006(3) N1 0.045(7) 0.029(7) 0.053(8) 0.003(6) 0.018(6) 0.003(6) N2 0.050(8) 0.057(8) 0.056(8) 0.004(7) 0.008(7) 0.007(7) N3 0.011 0.010 0.010 0.000 0.002 0.000 N4 0.036(7) 0.045(7) 0.049(8) 0.002(6) 0.013(6) 0.009(6) O1 0.050(8) 0.025(6) 0.034(7) 0.001(5) 0.011(6) 0.001(6) 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' 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_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C2 C1 Ir1 128.6(14) C6 C1 C2 116.3(19) C6 C1 Ir1 114.9(14) C1 C2 H2 120.0 C3 C2 C1 120(2) C3 C2 H2 120.0 C2 C3 H3 119.3 C2 C3 C4 121(2) C4 C3 H3 119.3 C3 C4 H4 120.9 C5 C4 C3 118(2) C5 C4 H4 120.9 C4 C5 H5 119.1 C4 C5 C6 122(2) C6 C5 H5 119.1 C1 C6 C5 122(2) C1 C6 C7 113.4(19) C5 C6 C7 124(2) C6 C7 C8 129(2) N1 C7 C6 117.2(19) N1 C7 C8 114.3(19) C7 C8 C9 122.8(19) N2 C8 C7 122(2) N2 C8 C9 115.0(19) C10 C9 C8 118.6(19) C10 C9 C14 121(2) C14 C9 C8 120(2) C9 C10 H10 120.5 C9 C10 C11 119(2) C11 C10 H10 120.5 C10 C11 H11 120.3 C10 C11 C12 119(2) C12 C11 H11 120.3 C11 C12 H12 120.6 C13 C12 C11 119(2) C13 C12 H12 120.6 C12 C13 H13 118.8 C14 C13 C12 122(3) C14 C13 H13 118.8 C9 C14 H14 120.3 C13 C14 C9 119(2) C13 C14 H14 120.3 C16 C15 C20 122(2) N2 C15 C16 119(2) N2 C15 C20 119(2) C15 C16 H16 120.2 C17 C16 C15 120(3) C17 C16 H16 120.2 C16 C17 H17 117.5 C16 C17 C18 125(3) C18 C17 H17 117.5 C17 C18 H18 122.6 C19 C18 C17 115(3) C19 C18 H18 122.6 C18 C19 H19 115.9 C18 C19 C20 128(2) C20 C19 H19 115.9 C19 C20 C15 109.9(19) N1 C20 C15 120(2) N1 C20 C19 129(2) C22 C21 C26 118.1(18) C22 C21 Ir1 127.8(15) C26 C21 Ir1 114.0(14) C21 C22 H22 118.5 C23 C22 C21 123(2) C23 C22 H22 118.5 C22 C23 H23 120.4 C22 C23 C24 119(2) C24 C23 H23 120.4 C23 C24 H24 120.6 C25 C24 C23 119(2) C25 C24 H24 120.6 C24 C25 H25 119.6 C24 C25 C26 121(2) C26 C25 H25 119.6 C21 C26 C27 115.4(18) C25 C26 C21 120.0(19) C25 C26 C27 124.4(19) C26 C27 C28 128.4(18) N3 C27 C26 113.1(16) N3 C27 C28 118.6(16) C27 C28 C29 120.4(18) N4 C28 C27 122.9(18) N4 C28 C29 116.6(18) C30 C29 C28 122(2) C30 C29 C34 119(2) C34 C29 C28 118(2) C29 C30 H30 118.3 C31 C30 C29 123(3) C31 C30 H30 118.3 C30 C31 H31 120.9 C32 C31 C30 118(3) C32 C31 H31 120.9 C31 C32 H32 117.6 C31 C32 C33 125(3) C33 C32 H32 117.6 C32 C33 H33 121.8 C32 C33 C34 116(3) C34 C33 H33 121.8 C29 C34 C33 118(3) C29 C34 H34 120.9 C33 C34 H34 120.9 C40 C35 C36 114.8(16) N4 C35 C36 117.0(16) N4 C35 C40 128.1(16) C35 C36 H36 120.3 C37 C36 C35 119.4(18) C37 C36 H36 120.3 C36 C37 H37 119.8 C38 C37 C36 120.4(19) C38 C37 H37 119.8 C37 C38 H38 118.8 C39 C38 C37 122.3(19) C39 C38 H38 118.8 C38 C39 H39 121.3 C40 C39 C38 117.4(18) C40 C39 H39 121.3 C35 C40 N3 112.9(13) C39 C40 C35 125.6(15) C39 C40 N3 121.5(14) C42 C41 C46 116.7(18) O1 C41 C42 118.0(18) O1 C41 C46 125.2(17) C41 C42 H42 119.7 C43 C42 C41 121(2) C43 C42 H42 119.7 C42 C43 H43 119.4 C44 C43 C42 121(2) C44 C43 H43 119.4 C43 C44 H44 119.1 C45 C44 C43 122(2) C45 C44 H44 119.1 C44 C45 H45 119.6 C44 C45 C46 121(2) C46 C45 H45 119.6 C41 C46 C45 118.9(19) C41 C46 C47 122.0(17) C47 C46 C45 119.1(19) N5 C47 C46 130.1(18) N5 C47 O2 109.5(17) O2 C47 C46 120.2(16) N6 C48 O2 111.8(18) N6 C48 C49 130.9(19) O2 C48 C49 116.9(17) C47 N5 N6 108.9(16) C47 N5 Ir1 126.3(13) N6 N5 Ir1 124.4(12) C48 N6 N5 105.7(17) C47 O2 C48 104.1(14) C50 C49 C48 119(2) C54 C49 C48 118(2) C54 C49 C50 122(2) C49 C50 H50 121.0 C49 C50 C51 118(2) C51 C50 H50 121.0 C50 C51 H51 120.0 C52 C51 C50 120(3) C52 C51 H51 120.0 C51 C52 H52 119.7 C51 C52 C53 121(3) C53 C52 H52 119.7 C52 C53 H53 120.2 C54 C53 C52 120(3) C54 C53 H53 120.2 C49 C54 C53 119(2) C49 C54 H54 120.5 C53 C54 H54 120.5 C1 Ir1 C21 91.2(7) C1 Ir1 N5 171.2(7) C1 Ir1 N1 80.5(7) C1 Ir1 N3 99.8(6) C1 Ir1 O1 88.3(6) C21 Ir1 N5 96.7(7) C21 Ir1 N1 99.7(7) C21 Ir1 N3 79.4(6) C21 Ir1 O1 178.8(7) N5 Ir1 O1 83.7(5) N1 Ir1 N5 94.5(6) N1 Ir1 O1 79.1(5) N3 Ir1 N5 85.3(5) N3 Ir1 N1 179.0(6) N3 Ir1 O1 101.8(4) C7 N1 Ir1 108.4(13) C20 N1 C7 122.2(19) C20 N1 Ir1 129.2(15) C8 N2 C15 116.9(19) C27 N3 C40 119.1(12) C27 N3 Ir1 114.5(10) C40 N3 Ir1 126.4(9) C28 N4 C35 115.7(16) C41 O1 Ir1 127.5(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C2 1.44(3) C1 C6 1.38(3) C1 Ir1 1.976(19) C2 H2 0.9300 C2 C3 1.37(3) C3 H3 0.9300 C3 C4 1.41(3) C4 H4 0.9300 C4 C5 1.33(3) C5 H5 0.9300 C5 C6 1.40(3) C6 C7 1.44(3) C7 C8 1.47(3) C7 N1 1.36(3) C8 C9 1.48(3) C8 N2 1.33(3) C9 C10 1.40(3) C9 C14 1.44(3) C10 H10 0.9300 C10 C11 1.42(3) C11 H11 0.9300 C11 C12 1.43(4) C12 H12 0.9300 C12 C13 1.42(4) C13 H13 0.9300 C13 C14 1.34(3) C14 H14 0.9300 C15 C16 1.46(3) C15 C20 1.51(3) C15 N2 1.35(3) C16 H16 0.9300 C16 C17 1.25(4) C17 H17 0.9300 C17 C18 1.48(4) C18 H18 0.9300 C18 C19 1.37(3) C19 H19 0.9300 C19 C20 1.44(3) C20 N1 1.19(3) C21 C22 1.40(3) C21 C26 1.42(3) C21 Ir1 1.977(18) C22 H22 0.9300 C22 C23 1.32(3) C23 H23 0.9300 C23 C24 1.46(3) C24 H24 0.9300 C24 C25 1.38(3) C25 H25 0.9300 C25 C26 1.38(3) C26 C27 1.44(3) C27 C28 1.44(3) C27 N3 1.35(2) C28 C29 1.51(3) C28 N4 1.29(2) C29 C30 1.38(3) C29 C34 1.38(3) C30 H30 0.9300 C30 C31 1.34(4) C31 H31 0.9300 C31 C32 1.30(4) C32 H32 0.9300 C32 C33 1.40(4) C33 H33 0.9300 C33 C34 1.43(4) C34 H34 0.9300 C35 C36 1.47(3) C35 C40 1.40(2) C35 N4 1.35(2) C36 H36 0.9300 C36 C37 1.40(3) C37 H37 0.9300 C37 C38 1.38(3) C38 H38 0.9300 C38 C39 1.38(3) C39 H39 0.9300 C39 C40 1.37(2) C40 N3 1.461(18) C41 C42 1.41(3) C41 C46 1.42(3) C41 O1 1.30(2) C42 H42 0.9300 C42 C43 1.39(3) C43 H43 0.9300 C43 C44 1.36(3) C44 H44 0.9300 C44 C45 1.29(3) C45 H45 0.9300 C45 C46 1.46(3) C46 C47 1.44(3) C47 N5 1.28(2) C47 O2 1.36(2) C48 N6 1.27(2) C48 O2 1.37(2) C48 C49 1.47(3) N5 N6 1.40(2) N5 Ir1 2.159(15) C49 C50 1.37(3) C49 C54 1.36(3) C50 H50 0.9300 C50 C51 1.45(3) C51 H51 0.9300 C51 C52 1.32(4) C52 H52 0.9300 C52 C53 1.42(4) C53 H53 0.9300 C53 C54 1.39(4) C54 H54 0.9300 Ir1 N1 2.087(17) Ir1 N3 2.061(11) Ir1 O1 2.181(12) loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons 1 -0.725 0.000 0.500 209.2 21.1 2 -0.605 0.500 0.000 209.2 21.1