#------------------------------------------------------------------------------ #$Date: 2019-12-14 01:09:06 +0200 (Sat, 14 Dec 2019) $ #$Revision: 245085 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/65/1556566.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_1556566 loop_ _publ_author_name 'Gao, Tai-Bao' 'Zhang, Jing-JIng' 'Wen, Jing' 'Yang, Xue-Xiao' 'Ma, Haibo' 'Cao, Deng-Ke' 'Jiang, Dechen' _publ_section_title ; Single-molecule MicroRNA Electrochemiluminescence Detection Using Cyclometalated Dinuclear Ir(III) Complex with Synergistic Effect. ; _journal_name_full 'Analytical chemistry' _journal_paper_doi 10.1021/acs.analchem.9b04431 _journal_year 2019 _chemical_formula_moiety 'C38 H21 F4 Ir N8, H2 O' _chemical_formula_sum 'C38 H23 F4 Ir N8 O' _chemical_formula_weight 875.84 _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' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2014/6 _cell_angle_alpha 90 _cell_angle_beta 96.413(7) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.273(2) _cell_length_b 10.772(2) _cell_length_c 29.566(6) _cell_measurement_reflns_used 4854 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 24.717 _cell_measurement_theta_min 2.3 _cell_volume 3251.3(11) _computing_cell_refinement SMART _computing_data_collection 'SMART (Bruker, 2000)' _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2014)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.976 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker Smart Aepex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0901 _diffrn_reflns_av_unetI/netI 0.0853 _diffrn_reflns_Laue_measured_fraction_full 0.976 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_number 21906 _diffrn_reflns_point_group_measured_fraction_full 0.976 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_min 2.014 _exptl_absorpt_coefficient_mu 4.176 _exptl_absorpt_correction_T_max 0.659 _exptl_absorpt_correction_T_min 0.582 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.789 _exptl_crystal_density_method 'not measured' _exptl_crystal_description blocky _exptl_crystal_F_000 1712 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.995 _refine_diff_density_min -1.621 _refine_diff_density_rms 0.188 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 469 _refine_ls_number_reflns 5738 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.013 _refine_ls_R_factor_all 0.0964 _refine_ls_R_factor_gt 0.0599 _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^)+(0.0900P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1314 _refine_ls_wR_factor_ref 0.1457 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4231 _reflns_number_total 5738 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ac9b04431_si_002.cif _cod_data_source_block 1 _cod_original_cell_volume 3251.4(11) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 1556566 _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. ; _shelxl_version_number 2014/6 _shelx_res_file ; TITL 1 in P2(1)/c CELL 0.71073 10.2729 10.7722 29.5663 90.000 96.413 90.000 ZERR 4.00 0.0022 0.0021 0.0059 0.000 0.007 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O F Ir UNIT 152 92 32 4 16 4 L.S. 50 ACTA omit 0 50 BOND $h FMAP 2 PLAN 10 dfix 1.4 C25 N4 htab TEMP 23.000 WGHT 0.090000 FVAR 0.06163 IR1 6 0.740607 0.901391 0.141401 11.00000 0.01947 0.01949 = 0.01709 -0.00058 0.00338 0.00146 F1 5 1.077615 1.284453 0.173171 11.00000 0.07074 0.04818 = 0.07188 -0.01151 0.00688 -0.03201 F2 5 1.232852 0.886827 0.213211 11.00000 0.03434 0.08087 = 0.05852 -0.00507 -0.00180 -0.00038 F3 5 0.683924 0.929692 0.320646 11.00000 0.05273 0.05154 = 0.02220 -0.00448 0.00793 0.00372 F4 5 0.466469 1.222184 0.224283 11.00000 0.07154 0.05400 = 0.05280 -0.01147 0.01275 0.03190 N1 3 0.845603 0.755589 0.169940 11.00000 0.02899 0.02380 = 0.02409 -0.00117 0.00603 -0.00037 N2 3 0.638394 1.051462 0.115145 11.00000 0.02151 0.02199 = 0.02070 -0.00447 0.00742 -0.00536 N3 3 0.565813 0.801384 0.120946 11.00000 0.02718 0.02226 = 0.01671 -0.00142 0.00032 -0.00322 N4 3 0.449594 0.684252 0.069741 11.00000 0.02222 0.03080 = 0.02773 -0.00488 0.00528 -0.00586 AFIX 43 H4A 2 0.427700 0.638989 0.046155 11.00000 -1.20000 AFIX 0 N5 3 0.778798 0.821744 0.074569 11.00000 0.01542 0.02264 = 0.02239 0.00088 0.00461 -0.00395 N6 3 0.704275 0.671812 0.022412 11.00000 0.01528 0.02413 = 0.01914 0.00226 0.00012 0.00324 N7 3 1.119674 0.658938 -0.044516 11.00000 0.02168 0.03604 = 0.02424 -0.00470 0.01290 0.00634 N8 3 1.203495 0.850586 0.010126 11.00000 0.02643 0.04028 = 0.02339 -0.00290 0.00033 -0.01035 C1 1 0.910152 0.987822 0.161960 11.00000 0.03600 0.02347 = 0.01404 -0.01001 0.00280 -0.00945 C2 1 0.933062 1.116705 0.160273 11.00000 0.03673 0.04991 = 0.03163 -0.00630 0.00540 -0.01223 AFIX 43 H2A 2 0.866691 1.171554 0.149642 11.00000 -1.20000 AFIX 0 C3 1 1.056588 1.158088 0.174858 11.00000 0.05843 0.02477 = 0.04818 0.00126 -0.00723 -0.01136 C4 1 1.156406 1.085380 0.191350 11.00000 0.03815 0.07103 = 0.04564 0.00082 0.00221 -0.03229 AFIX 43 H4B 2 1.238817 1.118564 0.200340 11.00000 -1.20000 AFIX 0 C5 1 1.134124 0.963982 0.194497 11.00000 0.02621 0.05822 = 0.01958 -0.00928 -0.00405 -0.00208 C6 1 1.010870 0.907924 0.181704 11.00000 0.01275 0.04099 = 0.02390 -0.00188 -0.00029 -0.00003 C7 1 0.973741 0.779324 0.185494 11.00000 0.02532 0.03634 = 0.01734 -0.00441 0.00076 0.00204 C8 1 1.053837 0.680024 0.204389 11.00000 0.03338 0.05315 = 0.03579 -0.00343 0.00007 0.02526 AFIX 43 H8B 2 1.141097 0.693785 0.215292 11.00000 -1.20000 AFIX 0 C9 1 1.000317 0.564248 0.206222 11.00000 0.05665 0.03244 = 0.03530 0.01343 -0.00392 0.02351 AFIX 43 H9A 2 1.052490 0.499580 0.218723 11.00000 -1.20000 AFIX 0 C10 1 0.875026 0.540654 0.190599 11.00000 0.07393 0.02727 = 0.02174 0.00498 0.00016 0.01598 AFIX 43 H10A 2 0.841181 0.460691 0.191303 11.00000 -1.20000 AFIX 0 C11 1 0.796242 0.640474 0.173103 11.00000 0.03512 0.03700 = 0.01011 0.00642 -0.00234 0.00782 AFIX 43 H11A 2 0.708125 0.626554 0.163518 11.00000 -1.20000 AFIX 0 C12 1 0.675961 0.966014 0.197700 11.00000 0.02756 0.02024 = 0.02439 -0.00319 0.00026 -0.00648 C13 1 0.705114 0.918435 0.241959 11.00000 0.02622 0.03034 = 0.01708 -0.00612 0.00225 -0.00279 AFIX 43 H13A 2 0.757984 0.848624 0.247050 11.00000 -1.20000 AFIX 0 C14 1 0.654492 0.976365 0.277740 11.00000 0.03773 0.04386 = 0.01401 -0.00681 0.00498 -0.01822 C15 1 0.572202 1.075077 0.272991 11.00000 0.03132 0.04210 = 0.03013 -0.01300 0.01352 0.00860 AFIX 43 H15A 2 0.535704 1.109185 0.297578 11.00000 -1.20000 AFIX 0 C16 1 0.545979 1.121682 0.229680 11.00000 0.02785 0.02877 = 0.04113 0.00509 -0.00657 0.00984 C17 1 0.593778 1.071312 0.191181 11.00000 0.02578 0.03476 = 0.03253 -0.00061 0.01684 0.00592 C18 1 0.568718 1.117246 0.144850 11.00000 0.03937 0.01760 = 0.02734 -0.00358 0.00016 0.00078 C19 1 0.486778 1.211992 0.127724 11.00000 0.04957 0.03376 = 0.04969 -0.00108 0.00509 0.02213 AFIX 43 H19A 2 0.438012 1.255283 0.147212 11.00000 -1.20000 AFIX 0 C20 1 0.476096 1.243444 0.082206 11.00000 0.04609 0.05036 = 0.03297 0.00806 0.00128 0.02160 AFIX 43 H20A 2 0.422774 1.308895 0.071093 11.00000 -1.20000 AFIX 0 C21 1 0.545291 1.176628 0.053869 11.00000 0.04018 0.02825 = 0.04918 0.01151 0.00472 -0.00139 AFIX 43 H21A 2 0.538664 1.194683 0.022938 11.00000 -1.20000 AFIX 0 C22 1 0.624474 1.082779 0.071626 11.00000 0.03297 0.03595 = 0.02603 0.00817 0.01295 -0.00136 AFIX 43 H22A 2 0.671436 1.038206 0.051937 11.00000 -1.20000 AFIX 0 C23 1 0.444286 0.787241 0.133673 11.00000 0.02168 0.03438 = 0.02723 -0.00360 0.00703 -0.01439 AFIX 43 H23A 2 0.415723 0.821831 0.159645 11.00000 -1.20000 AFIX 0 C24 1 0.370898 0.716369 0.103582 11.00000 0.01475 0.04401 = 0.03312 0.00688 0.01445 -0.00643 AFIX 43 H24A 2 0.284265 0.693007 0.104931 11.00000 -1.20000 AFIX 0 C25 1 0.567334 0.738831 0.081603 11.00000 0.01011 0.01819 = 0.01555 0.00256 -0.00361 0.00352 C26 1 0.682370 0.741764 0.057813 11.00000 0.02218 0.02393 = 0.02460 0.00337 0.01406 0.00745 C27 1 0.873808 0.800386 0.045742 11.00000 0.02034 0.02649 = 0.01476 0.00272 0.00395 -0.00585 C28 1 0.829137 0.708958 0.014742 11.00000 0.02411 0.01646 = 0.02172 -0.00269 0.00489 0.00613 C29 1 1.074197 0.570950 -0.074627 11.00000 0.03302 0.02749 = 0.02728 -0.00944 0.00540 0.00581 AFIX 43 H29A 2 1.131876 0.538333 -0.093638 11.00000 -1.20000 AFIX 0 C30 1 0.946797 0.525856 -0.079098 11.00000 0.03462 0.04450 = 0.01876 -0.01450 0.00789 -0.00692 AFIX 43 H30A 2 0.919028 0.467542 -0.101296 11.00000 -1.20000 AFIX 0 C31 1 0.864026 0.569436 -0.050103 11.00000 0.03058 0.02473 = 0.02787 -0.00669 0.01042 -0.00049 AFIX 43 H31A 2 0.779153 0.538523 -0.051453 11.00000 -1.20000 AFIX 0 C32 1 0.906243 0.660783 -0.018196 11.00000 0.01454 0.01820 = 0.01769 -0.00141 -0.00208 0.00539 C33 1 1.037202 0.705688 -0.017282 11.00000 0.02491 0.02457 = 0.01596 0.00232 -0.00243 0.00202 C34 1 1.079613 0.805547 0.013159 11.00000 0.01690 0.02737 = 0.02433 0.00704 0.01334 0.00189 C35 1 0.999565 0.857798 0.044579 11.00000 0.02524 0.02368 = 0.02252 0.00678 0.00562 0.01197 C36 1 1.042722 0.965345 0.067766 11.00000 0.02273 0.02811 = 0.02880 -0.00591 -0.00543 0.00721 AFIX 43 H36A 2 0.988276 1.005762 0.086126 11.00000 -1.20000 AFIX 0 C37 1 1.166499 1.012454 0.063607 11.00000 0.02911 0.03890 = 0.02349 -0.00401 0.00804 -0.01466 AFIX 43 H37A 2 1.196186 1.084201 0.078937 11.00000 -1.20000 AFIX 0 C38 1 1.244684 0.949391 0.035909 11.00000 0.02414 0.04839 = 0.02704 0.01447 0.00549 -0.00990 AFIX 43 H38A 2 1.330249 0.976727 0.035061 11.00000 -1.20000 AFIX 0 O1W 4 0.374156 0.576560 0.990211 11.00000 0.03036 0.01612 = 0.04197 -0.00651 0.00211 -0.00603 AFIX 3 H1WB 2 0.340536 0.506220 0.994821 11.00000 -1.20000 H1WC 2 0.317496 0.622200 0.975081 11.00000 -1.20000 AFIX 0 HKLF 4 REM 1 in P2(1)/c REM R1 = 0.0599 for 4231 Fo > 4sig(Fo) and 0.0964 for all 5738 data REM 469 parameters refined using 1 restraints END WGHT 0.0323 24.6414 REM Instructions for potential hydrogen bonds EQIV $1 x, y, z-1 HTAB N4 O1W_$1 EQIV $2 x+1, y, z HTAB C4 F4_$2 HTAB C8 F2 HTAB C11 N3 EQIV $3 -x+1, y+1/2, -z+1/2 HTAB C19 F3_$3 HTAB C19 F4 HTAB C22 N5 EQIV $4 -x+2, -y+2, -z HTAB C22 N8_$4 EQIV $5 -x+1, -y+1, -z+1 HTAB O1W N6_$5 EQIV $6 x-1, y, z+1 HTAB O1W N7_$6 REM Highest difference peak 0.995, deepest hole -1.621, 1-sigma level 0.188 Q1 1 0.7927 0.9791 0.1316 11.00000 0.05 1.00 Q2 1 0.6773 0.8431 0.1375 11.00000 0.05 0.99 Q3 1 0.7441 0.9015 0.1118 11.00000 0.05 0.87 Q4 1 0.7371 0.9231 0.1705 11.00000 0.05 0.87 Q5 1 0.8015 0.8383 0.1354 11.00000 0.05 0.87 Q6 1 1.2545 1.1142 0.2270 11.00000 0.05 0.77 Q7 1 0.7257 0.6246 0.0485 11.00000 0.05 0.77 Q8 1 0.6788 0.8092 0.0099 11.00000 0.05 0.76 Q9 1 0.7318 0.5204 0.1283 11.00000 0.05 0.75 Q10 1 1.0681 1.2142 0.0832 11.00000 0.05 0.72 ; _shelx_res_checksum 62979 _shelx_hkl_file ; 2 0 0 59.39 2.55 2 0 0 55.53 2.59 -2 0 0 59.92 2.58 -3 0 0 3.77 0.86 -3 0 0 2.80 1.06 3 0 0 4.27 0.96 -4 0 0 139.89 6.34 -4 0 0 141.65 6.05 4 0 0 143.79 6.11 5 0 0 18.03 2.13 -5 0 0 18.32 1.95 -5 0 0 13.56 2.17 -6 0 0 165.22 7.15 -6 0 0 147.56 7.49 -7 0 0 22.07 2.67 -8 0 0 38.72 3.95 -8 0 0 46.75 5.07 -9 0 0 5.88 4.34 -9 0 0 5.08 2.64 -10 0 0 62.33 7.07 -10 0 0 63.61 5.62 -11 0 0 19.13 4.02 -11 0 0 19.60 5.87 -12 0 0 10.57 4.50 -12 0 0 12.33 6.92 -13 0 0 20.39 8.68 1 -1 0 234.27 8.87 1 -1 0 238.42 8.42 -1 -1 0 221.09 8.51 1 -1 0 209.38 8.38 -1 1 0 225.76 8.38 -1 1 0 244.62 8.42 1 1 0 220.39 8.48 -1 1 0 224.56 8.87 2 -1 0 13.25 1.44 -2 -1 0 12.91 0.87 -2 -1 0 12.98 1.06 -2 1 0 13.23 0.91 2 1 0 11.63 0.80 -2 1 0 13.15 1.53 -3 -1 0 164.71 6.87 -3 -1 0 168.20 6.75 3 -1 0 184.18 6.73 3 -1 0 170.17 7.15 -3 1 0 160.92 7.26 -3 1 0 162.93 6.70 3 1 0 172.76 6.63 -4 -1 0 13.29 1.64 4 -1 0 10.05 1.83 -4 -1 0 9.31 1.35 4 1 0 10.88 1.27 -4 1 0 12.21 2.00 -4 1 0 9.82 1.31 -5 -1 0 26.96 2.36 -5 -1 0 26.21 2.40 -5 1 0 25.49 2.93 5 1 0 27.72 2.13 -5 1 0 27.14 2.20 -6 -1 0 43.53 3.44 -6 -1 0 35.06 3.04 -6 1 0 43.37 3.99 -6 1 0 43.35 2.99 -7 -1 0 11.30 2.40 -7 -1 0 16.47 2.88 -7 1 0 8.57 1.94 -7 1 0 12.96 3.20 -8 -1 0 9.54 3.09 -8 -1 0 11.18 2.52 -8 1 0 11.60 2.35 -8 1 0 13.94 3.80 -9 -1 0 7.35 3.47 -9 1 0 9.41 4.12 -9 1 0 5.92 2.51 -10 -1 0 11.89 4.87 -10 -1 0 4.69 3.00 -10 1 0 7.02 3.17 -10 1 0 3.24 4.73 -11 -1 0 5.12 5.39 -11 -1 0 9.14 3.78 -11 1 0 13.62 4.25 -11 1 0 15.77 6.25 -12 -1 0 0.10 6.77 -12 -1 0 3.00 4.29 -12 1 0 7.59 7.32 -12 1 0 -6.58 3.99 -13 -1 0 13.07 8.76 -13 -1 0 1.04 4.91 -13 1 0 14.69 9.41 -13 1 0 9.72 5.62 0 -2 0 1.00 0.82 0 -2 0 2.14 0.32 0 2 0 2.53 0.32 0 2 0 2.50 0.90 1 -2 0 21.48 1.01 1 -2 0 20.43 1.91 -1 -2 0 23.47 1.57 1 -2 0 21.21 0.94 -1 2 0 21.54 0.98 1 2 0 20.25 1.45 -1 2 0 24.07 1.96 2 -2 0 177.91 7.54 2 -2 0 163.29 6.59 -2 -2 0 177.38 6.87 -2 -2 0 170.93 6.87 -2 2 0 173.15 6.61 -2 2 0 179.59 6.56 -3 -2 0 80.47 3.47 3 -2 0 85.71 3.42 -3 -2 0 75.72 3.32 -3 -2 0 75.12 3.69 3 -2 0 79.07 4.32 -3 2 0 78.58 3.27 -3 2 0 79.29 3.42 -3 2 0 73.58 4.43 -4 -2 0 -0.03 1.04 -4 -2 0 0.27 0.74 -4 2 0 2.63 1.77 4 2 0 -0.19 0.65 -4 2 0 -1.30 0.78 -5 -2 0 -1.90 1.08 -5 -2 0 0.10 1.15 -5 2 0 1.18 1.08 -5 2 0 -1.57 1.88 5 2 0 0.15 0.92 -6 -2 0 8.98 1.91 6 2 0 7.32 1.52 -6 2 0 6.99 1.55 -6 2 0 5.58 2.62 -7 -2 0 -0.34 1.98 -7 -2 0 0.17 1.68 -7 2 0 1.13 2.86 -7 2 0 -0.52 1.56 -8 -2 0 32.67 3.80 -8 -2 0 22.98 3.33 -8 2 0 23.75 3.11 -8 2 0 24.37 4.95 -9 -2 0 5.77 3.52 -9 -2 0 5.83 2.74 -9 2 0 4.35 4.08 -9 2 0 3.97 2.55 -10 -2 0 5.02 4.35 -10 2 0 4.53 3.17 -10 2 0 0.43 5.15 -11 -2 0 5.90 3.69 -11 -2 0 11.75 5.62 -11 2 0 10.30 6.22 -12 -2 0 6.64 6.74 -12 -2 0 12.51 4.65 -12 2 0 23.21 7.91 -13 -2 0 3.53 4.92 -13 2 0 -4.25 5.40 -13 2 0 8.87 9.46 0 -3 0 1.74 1.22 0 -3 0 -0.03 0.31 0 3 0 0.09 1.02 0 3 0 -0.10 0.34 1 -3 0 88.22 3.51 1 -3 0 91.94 3.65 -1 -3 0 101.20 4.52 1 -3 0 96.20 4.85 -1 3 0 96.04 3.63 -1 3 0 91.34 4.85 1 3 0 90.78 4.34 2 -3 0 0.69 0.40 -2 -3 0 -0.75 1.10 2 -3 0 2.34 1.52 2 -3 0 0.83 0.45 -2 -3 0 1.78 0.68 -2 3 0 0.64 0.41 2 3 0 0.84 0.79 -2 3 0 1.37 0.43 -2 3 0 2.17 1.29 -3 -3 0 433.58 16.47 -3 -3 0 440.45 16.46 -3 -3 0 430.37 16.06 -3 3 0 427.34 17.52 -3 3 0 405.56 15.92 -3 3 0 436.85 16.03 -4 -3 0 46.64 3.05 4 -3 0 57.50 2.72 -4 -3 0 55.27 3.00 -4 -3 0 56.35 2.66 -4 3 0 49.68 4.29 -4 3 0 49.27 2.69 -5 -3 0 62.05 3.41 -5 -3 0 63.95 3.27 -5 3 0 58.71 3.26 -5 3 0 57.74 4.83 -6 -3 0 27.56 2.96 -6 -3 0 29.37 2.75 -6 -3 0 25.53 2.54 -6 3 0 22.78 3.95 -6 3 0 31.30 2.58 -7 -3 0 73.97 4.72 -7 -3 0 68.30 4.41 -7 3 0 74.44 6.49 -7 3 0 70.15 4.27 -8 -3 0 18.38 2.91 -8 -3 0 24.62 3.45 -8 3 0 14.68 4.35 -8 3 0 16.87 2.95 -9 -3 0 38.27 4.32 -9 -3 0 34.78 4.50 -9 3 0 39.66 6.40 -9 3 0 33.09 3.85 -10 -3 0 8.83 3.83 -10 -3 0 17.64 4.30 -10 3 0 16.64 3.55 -10 3 0 14.72 5.91 -11 -3 0 27.96 6.25 -11 -3 0 22.56 4.78 -11 3 0 11.11 7.07 -11 3 0 29.42 4.64 -12 -3 0 11.71 7.03 -12 3 0 0.22 7.82 -12 3 0 4.48 4.67 0 -4 0 86.39 3.54 0 -4 0 93.23 5.01 0 4 0 86.77 4.85 1 -4 0 0.33 0.33 1 -4 0 0.37 0.46 1 -4 0 1.42 1.90 -1 -4 0 0.41 0.43 -1 -4 0 1.97 1.59 1 4 0 -0.41 1.18 -1 4 0 -0.11 0.49 -1 4 0 0.00 1.56 2 -4 0 217.75 7.86 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6.02 2 -5 -34 -2.27 3.79 -2 -5 34 -0.46 2.01 2 5 -34 -3.38 5.84 -2 5 34 12.07 7.00 1 -5 -34 6.75 4.16 -1 -5 34 -0.21 6.63 -1 -5 34 -3.56 2.03 1 5 -34 4.39 6.08 -1 5 34 -4.28 7.17 0 -5 34 3.37 7.24 0 -5 -34 5.39 4.36 0 5 -34 -4.92 5.66 -1 -5 -34 10.70 4.70 -1 5 -34 3.94 6.49 -2 -5 -34 -2.25 4.30 -2 5 -34 4.58 6.74 -3 -6 34 8.03 6.22 3 -6 -34 16.44 4.39 -3 6 34 22.70 8.15 -2 -6 34 4.76 6.53 2 -6 -34 6.06 4.19 -2 -6 34 1.29 2.26 2 6 -34 16.17 7.05 -2 6 34 -1.64 7.60 1 -6 -34 21.23 4.75 -1 -6 34 30.62 7.59 -1 -6 34 23.91 2.80 1 6 -34 20.63 7.56 0 -6 -34 9.82 4.57 0 -6 34 8.73 2.73 0 -6 34 26.00 8.24 0 6 -34 -0.52 6.89 6 0 -35 7.14 4.09 -6 0 35 -2.08 5.19 -5 0 35 4.16 4.69 5 0 -35 7.60 4.04 -4 0 35 7.76 5.24 -3 0 35 -8.03 5.24 3 0 -35 -7.51 3.60 2 0 -35 2.14 4.06 -2 0 35 -0.69 5.68 -1 0 35 -5.61 5.47 1 0 -35 3.27 3.81 0 0 35 9.30 6.60 0 0 -35 4.87 4.04 -1 0 -35 6.71 4.58 -2 0 -35 7.47 4.75 -3 0 -35 -0.86 5.05 6 -1 -35 14.98 4.12 -6 -1 35 11.34 5.16 -6 1 35 6.48 5.51 -5 -1 35 -8.58 4.99 5 -1 -35 -3.71 3.69 5 1 -35 -0.02 3.89 -5 1 35 4.47 4.62 4 -1 -35 20.92 4.12 -4 -1 35 15.69 5.13 4 1 -35 12.59 4.16 -4 1 35 24.99 6.09 -3 -1 35 -1.03 5.43 3 -1 -35 2.55 3.72 -3 1 35 1.52 5.72 3 1 -35 -2.47 3.78 2 -1 -35 21.91 4.49 -2 -1 35 35.44 6.92 2 1 -35 18.55 4.77 -2 1 35 9.40 6.09 -1 -1 35 14.32 6.55 1 -1 -35 2.21 3.66 1 1 -35 3.88 4.06 -1 1 35 2.24 6.53 0 -1 -35 14.65 5.09 0 -1 35 21.97 7.88 0 1 -35 17.37 4.97 0 1 35 22.04 7.65 -1 -1 -35 15.78 4.88 1 -1 35 13.59 7.75 -2 1 -35 13.90 5.55 -3 -1 -35 -1.74 4.98 -3 1 -35 4.33 5.58 6 -2 -35 7.39 4.16 -6 -2 35 1.95 4.70 -6 2 35 -2.10 4.86 -5 -2 35 22.99 2.69 -5 -2 35 35.93 6.52 5 2 -35 31.04 5.28 -5 2 35 30.22 6.46 4 -2 -35 1.88 3.62 -4 -2 35 3.96 1.92 -4 -2 35 -0.68 4.93 4 2 -35 -1.17 4.37 -4 2 35 12.84 5.63 -3 -2 35 24.50 2.49 -3 -2 35 24.26 5.84 3 -2 -35 19.33 4.59 -3 2 35 31.39 6.78 3 2 -35 30.11 5.40 -2 -2 35 -0.78 5.90 2 -2 -35 2.18 3.56 -2 -2 35 5.30 1.93 2 2 -35 7.47 4.80 -2 2 35 -8.39 5.80 1 -2 -35 21.69 4.59 -1 2 35 22.41 6.93 1 2 -35 25.08 5.50 0 -2 -35 -1.33 3.92 0 -2 35 -7.82 6.49 0 2 -35 9.23 5.16 0 2 35 -3.43 7.48 1 -2 35 30.08 8.46 -1 -2 -35 30.88 5.85 -2 -2 -35 0.17 4.63 -2 2 -35 -6.05 5.12 -3 -2 -35 19.75 5.86 -3 2 -35 21.09 6.39 5 -3 -35 -4.42 3.72 -5 -3 35 7.54 5.13 -5 -3 35 2.35 1.98 -5 3 35 9.84 6.38 4 -3 -35 1.06 3.84 -4 -3 35 -9.48 4.94 -4 -3 35 1.88 1.99 -4 3 35 4.34 6.26 4 3 -35 10.62 5.06 -3 -3 35 3.47 1.99 3 -3 -35 -3.45 3.75 -3 -3 35 -4.80 5.12 3 3 -35 2.90 5.04 -3 3 35 17.36 6.55 -2 -3 35 1.48 1.98 2 -3 -35 6.99 4.15 -2 3 35 -2.23 6.59 -1 -3 35 3.64 2.03 1 -3 -35 -0.22 4.10 -1 -3 35 -10.51 5.90 -1 3 35 7.86 7.38 1 3 -35 -4.88 5.02 0 -3 35 0.72 7.14 0 3 -35 5.22 5.27 0 3 35 2.57 7.23 -1 -3 -35 -2.75 3.96 -1 3 -35 -0.67 5.27 -2 -3 -35 7.91 4.65 -2 3 -35 -2.30 5.27 -3 -3 -35 11.76 5.37 -3 3 -35 -2.43 6.12 -5 -4 35 7.93 5.52 -5 -4 35 6.16 2.36 -5 4 35 18.59 6.67 -4 -4 35 -0.41 2.17 -4 -4 35 2.76 5.33 4 -4 -35 -8.37 3.86 -4 4 35 11.52 6.21 3 -4 -35 15.50 4.32 -3 -4 35 6.27 5.86 -3 -4 35 9.03 2.34 3 4 -35 15.69 5.86 -3 4 35 7.19 6.86 2 -4 -35 5.84 4.13 -2 -4 35 1.31 6.27 2 4 -35 3.46 5.62 -2 4 35 3.69 7.21 -1 -4 35 17.32 6.88 1 -4 -35 12.61 4.54 -1 -4 35 11.84 2.49 1 4 -35 16.03 5.85 -1 4 35 14.71 7.10 0 -4 35 18.79 7.88 0 -4 -35 8.61 4.45 0 4 -35 2.73 5.87 -1 -4 -35 9.35 4.86 -1 4 -35 5.88 5.88 -2 -4 -35 4.75 4.91 -2 4 -35 8.59 6.69 -3 -5 35 -7.56 5.65 3 -5 -35 2.74 4.01 -3 -5 35 -0.32 2.13 3 5 -35 -6.69 5.93 -3 5 35 17.70 7.94 -2 -5 35 32.66 3.11 2 -5 -35 33.31 5.48 -2 -5 35 32.66 7.32 -2 5 35 35.27 8.23 2 5 -35 26.33 6.92 1 -5 -35 5.76 4.65 -1 -5 35 -0.43 2.30 -1 -5 35 0.55 6.82 -1 5 35 -2.44 7.58 1 5 -35 8.53 6.24 0 -5 35 14.74 2.78 0 -5 -35 19.57 4.94 0 -5 35 22.33 8.32 0 5 -35 21.90 6.92 -1 -5 -35 0.80 4.36 -1 5 -35 -8.72 6.42 -5 0 36 21.41 5.95 5 0 -36 11.48 4.26 -4 0 36 14.25 5.96 4 0 -36 11.72 4.51 3 0 -36 10.40 4.38 -3 0 36 8.06 6.35 2 0 -36 11.02 4.32 -2 0 36 16.61 7.03 -1 0 36 20.59 7.22 1 0 -36 17.81 4.86 0 0 -36 21.10 5.30 0 0 36 36.79 8.81 -1 0 -36 9.69 5.07 -2 0 -36 48.15 7.40 -3 0 -36 12.37 5.73 5 -1 -36 3.37 4.24 -5 -1 36 -1.08 5.21 5 1 -36 6.60 4.53 -5 1 36 14.60 5.94 -4 -1 36 6.04 5.41 4 -1 -36 -1.82 3.69 -4 1 36 19.85 6.00 -3 -1 36 22.30 6.44 3 -1 -36 9.29 3.90 -3 1 36 -0.29 6.05 3 1 -36 9.72 4.64 -2 -1 36 17.28 6.58 2 -1 -36 9.71 3.97 2 1 -36 6.33 4.53 -2 1 36 1.64 6.14 -1 -1 36 8.29 6.60 1 -1 -36 13.23 4.91 -1 1 36 25.42 7.61 1 1 -36 17.08 5.16 0 -1 36 10.74 7.31 0 -1 -36 8.94 4.88 0 1 -36 4.09 5.06 0 1 36 7.72 7.57 -1 -1 -36 8.53 5.08 -1 1 -36 12.54 5.49 -2 -1 -36 5.51 4.87 -2 1 -36 -0.79 5.36 -5 -2 36 6.54 5.49 -5 2 36 8.06 5.62 -4 -2 36 10.41 5.35 4 2 -36 4.78 4.74 -4 2 36 2.98 6.00 3 -2 -36 7.04 4.18 -3 -2 36 -0.90 5.92 -3 -2 36 0.10 2.03 3 2 -36 2.86 4.78 -3 2 36 7.24 6.25 -2 -2 36 1.78 1.99 2 -2 -36 5.80 4.38 2 2 -36 5.74 4.75 -2 2 36 15.96 6.48 -1 -2 36 8.82 6.92 -1 2 36 12.50 7.19 1 2 -36 7.60 4.83 0 -2 36 2.29 7.39 0 -2 -36 -4.35 4.39 0 2 36 9.63 7.30 0 2 -36 2.56 4.85 -1 -2 -36 9.56 5.00 -1 2 -36 4.07 5.74 -2 -2 -36 -1.80 4.68 -2 2 -36 -1.99 5.83 -4 -3 36 12.10 2.39 -4 -3 36 16.19 5.88 4 -3 -36 24.35 4.81 -4 3 36 22.00 7.12 4 3 -36 15.99 5.47 3 -3 -36 28.00 5.09 -3 -3 36 20.24 6.68 3 3 -36 26.25 5.87 -3 3 36 24.59 7.34 2 -3 -36 1.69 4.23 -2 -3 36 15.00 6.45 -2 -3 36 6.86 2.17 2 3 -36 6.73 5.33 1 -3 -36 30.33 5.60 -1 -3 36 22.23 2.75 -1 -3 36 16.69 7.20 1 3 -36 16.31 5.53 -1 3 36 11.72 7.22 0 -3 36 -1.93 7.21 0 3 36 10.98 7.73 0 3 -36 8.19 5.41 -1 -3 -36 20.86 5.27 -1 3 -36 19.65 6.32 -2 3 -36 12.44 6.44 -3 -4 36 10.08 6.57 3 -4 -36 0.05 4.35 -3 -4 36 4.22 2.23 -3 4 36 2.00 7.24 3 4 -36 -1.86 6.03 -2 -4 36 19.93 2.78 2 -4 -36 13.14 4.92 -2 4 36 35.19 8.44 2 4 -36 13.32 6.21 -1 -4 36 11.60 7.32 1 -4 -36 10.95 4.77 -1 4 36 0.05 7.64 1 4 -36 22.46 6.34 0 -4 -36 -1.63 4.38 0 -4 36 10.17 8.22 0 4 -36 3.66 6.29 4 0 -37 4.38 4.65 -4 0 37 2.49 5.93 -3 0 37 7.88 6.42 3 0 -37 5.23 4.47 -2 0 37 3.70 6.94 2 0 -37 0.86 4.38 -1 0 37 0.92 6.94 1 0 -37 1.79 4.57 0 0 -37 0.49 4.68 0 0 37 9.03 7.72 -1 0 -37 5.81 5.20 -4 -1 37 -7.75 5.36 4 -1 -37 1.08 4.21 -4 1 37 16.77 6.52 3 -1 -37 16.09 4.73 -3 -1 37 23.63 7.28 -3 1 37 14.36 6.70 3 1 -37 21.46 5.23 2 -1 -37 0.93 4.48 -2 -1 37 -0.48 6.38 -2 1 37 -3.06 5.97 2 1 -37 5.51 4.28 1 -1 -37 21.67 5.59 -1 -1 37 26.67 7.25 -1 1 37 9.81 7.45 1 1 -37 24.80 5.66 0 -1 -37 2.79 4.85 0 -1 37 13.98 7.80 0 1 37 6.99 7.36 -1 1 -37 16.62 6.10 4 -2 -37 16.18 4.88 -4 2 37 9.49 6.66 3 -2 -37 -0.36 3.83 3 2 -37 -6.29 5.26 -3 2 37 4.08 6.27 -2 -2 37 21.76 7.43 2 -2 -37 33.31 5.59 -2 2 37 31.67 7.54 2 2 -37 24.86 6.07 1 -2 -37 -0.68 4.31 -1 -2 37 0.87 7.01 -1 2 37 -2.37 7.42 1 2 -37 4.09 5.14 0 -2 37 28.93 8.53 0 -2 -37 9.93 5.13 0 2 37 27.38 8.83 0 2 -37 15.40 5.99 -1 -2 -37 0.91 5.02 -1 2 -37 -3.33 5.61 -3 -3 37 19.91 6.84 -3 -3 37 1.81 2.37 3 3 -37 5.87 5.54 -3 3 37 12.75 6.97 -2 -3 37 0.09 6.43 2 -3 -37 8.62 4.59 -2 -3 37 2.40 2.36 -2 3 37 8.33 7.10 2 3 -37 7.20 5.50 -1 -3 37 0.19 7.26 1 -3 -37 4.69 4.57 1 3 -37 6.48 5.44 -1 3 37 -7.98 7.43 0 -3 -37 -4.78 4.53 0 -3 37 14.15 8.25 0 3 -37 1.74 5.78 3 0 -38 15.88 5.16 2 0 -38 32.16 5.92 -1 0 38 15.45 7.74 1 0 -38 6.56 4.95 0 0 -38 19.40 6.11 -2 -1 38 1.23 6.60 2 -1 -38 11.98 5.36 2 1 -38 7.52 5.25 -2 1 38 -10.60 6.70 -1 -1 38 16.37 7.53 1 -1 -38 5.14 5.16 -1 1 38 14.10 7.81 1 1 -38 13.75 5.93 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 2771 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 Ir1 Ir 0.74061(4) 0.90139(3) 0.14140(2) 0.01858(15) Uani 1 1 d . . F1 F 1.0776(8) 1.2845(6) 0.1732(3) 0.064(2) Uani 1 1 d . . F2 F 1.2329(7) 0.8868(7) 0.2132(3) 0.058(2) Uani 1 1 d . . F3 F 0.6839(7) 0.9297(6) 0.32065(19) 0.0419(17) Uani 1 1 d . . F4 F 0.4665(8) 1.2222(6) 0.2243(2) 0.059(2) Uani 1 1 d . . N1 N 0.8456(9) 0.7556(7) 0.1699(3) 0.025(2) Uani 1 1 d . . N2 N 0.6384(8) 1.0515(7) 0.1151(3) 0.0210(19) Uani 1 1 d . . N3 N 0.5658(8) 0.8014(7) 0.1209(2) 0.0222(18) Uani 1 1 d . . N4 N 0.4496(8) 0.6843(7) 0.0697(3) 0.027(2) Uani 1 1 d D . H4A H 0.4277 0.6390 0.0462 0.032 Uiso 1 1 calc R U N5 N 0.7788(8) 0.8217(7) 0.0746(3) 0.0200(18) Uani 1 1 d . . N6 N 0.7043(7) 0.6718(7) 0.0224(2) 0.0197(18) Uani 1 1 d . . N7 N 1.1197(8) 0.6589(8) -0.0445(3) 0.027(2) Uani 1 1 d . . N8 N 1.2035(9) 0.8506(8) 0.0101(3) 0.030(2) Uani 1 1 d . . C1 C 0.9102(10) 0.9878(9) 0.1620(3) 0.025(2) Uani 1 1 d . . C2 C 0.9331(12) 1.1167(10) 0.1603(4) 0.039(3) Uani 1 1 d . . H2A H 0.8667 1.1716 0.1496 0.047 Uiso 1 1 calc R U C3 C 1.0566(14) 1.1581(10) 0.1749(4) 0.045(3) Uani 1 1 d . . C4 C 1.1564(13) 1.0854(12) 0.1913(4) 0.052(4) Uani 1 1 d . . H4B H 1.2388 1.1186 0.2003 0.062 Uiso 1 1 calc R U C5 C 1.1341(11) 0.9640(11) 0.1945(4) 0.035(3) Uani 1 1 d . . C6 C 1.0109(9) 0.9079(9) 0.1817(3) 0.026(2) Uani 1 1 d . . C7 C 0.9737(10) 0.7793(9) 0.1855(3) 0.026(2) Uani 1 1 d . . C8 C 1.0538(12) 0.6800(11) 0.2044(4) 0.041(3) Uani 1 1 d . . H8B H 1.1411 0.6938 0.2153 0.049 Uiso 1 1 calc R U C9 C 1.0003(13) 0.5642(10) 0.2062(4) 0.042(3) Uani 1 1 d . . H9A H 1.0525 0.4996 0.2187 0.051 Uiso 1 1 calc R U C10 C 0.8750(14) 0.5407(10) 0.1906(3) 0.041(3) Uani 1 1 d . . H10A H 0.8412 0.4607 0.1913 0.050 Uiso 1 1 calc R U C11 C 0.7962(11) 0.6405(9) 0.1731(3) 0.028(2) Uani 1 1 d . . H11A H 0.7081 0.6266 0.1635 0.033 Uiso 1 1 calc R U C12 C 0.6760(10) 0.9660(8) 0.1977(3) 0.024(2) Uani 1 1 d . . C13 C 0.7051(10) 0.9184(8) 0.2420(3) 0.025(2) Uani 1 1 d . . H13A H 0.7580 0.8486 0.2470 0.029 Uiso 1 1 calc R U C14 C 0.6545(11) 0.9764(10) 0.2777(3) 0.032(3) Uani 1 1 d . . C15 C 0.5722(11) 1.0751(9) 0.2730(4) 0.034(3) Uani 1 1 d . . H15A H 0.5357 1.1092 0.2976 0.041 Uiso 1 1 calc R U C16 C 0.5460(11) 1.1217(9) 0.2297(4) 0.033(3) Uani 1 1 d . . C17 C 0.5938(11) 1.0713(9) 0.1912(4) 0.030(3) Uani 1 1 d . . C18 C 0.5687(11) 1.1172(8) 0.1449(3) 0.028(3) Uani 1 1 d . . C19 C 0.4868(12) 1.2120(10) 0.1277(4) 0.044(3) Uani 1 1 d . . H19A H 0.4380 1.2553 0.1472 0.053 Uiso 1 1 calc R U C20 C 0.4761(12) 1.2434(11) 0.0822(4) 0.043(3) Uani 1 1 d . . H20A H 0.4228 1.3089 0.0711 0.052 Uiso 1 1 calc R U C21 C 0.5453(11) 1.1766(10) 0.0539(4) 0.039(3) Uani 1 1 d . . H21A H 0.5387 1.1947 0.0229 0.047 Uiso 1 1 calc R U C22 C 0.6245(11) 1.0828(9) 0.0716(3) 0.031(3) Uani 1 1 d . . H22A H 0.6714 1.0382 0.0519 0.037 Uiso 1 1 calc R U C23 C 0.4443(10) 0.7872(9) 0.1337(3) 0.027(2) Uani 1 1 d . . H23A H 0.4157 0.8218 0.1596 0.033 Uiso 1 1 calc R U C24 C 0.3709(10) 0.7164(9) 0.1036(3) 0.030(3) Uani 1 1 d . . H24A H 0.2843 0.6930 0.1049 0.036 Uiso 1 1 calc R U C25 C 0.5673(8) 0.7388(8) 0.0816(3) 0.015(2) Uani 1 1 d D . C26 C 0.6824(10) 0.7418(8) 0.0578(3) 0.023(2) Uani 1 1 d . . C27 C 0.8738(9) 0.8004(9) 0.0457(3) 0.020(2) Uani 1 1 d . . C28 C 0.8291(10) 0.7090(8) 0.0147(3) 0.021(2) Uani 1 1 d . . C29 C 1.0742(11) 0.5710(9) -0.0746(3) 0.029(3) Uani 1 1 d . . H29A H 1.1319 0.5383 -0.0936 0.035 Uiso 1 1 calc R U C30 C 0.9468(11) 0.5259(10) -0.0791(3) 0.032(3) Uani 1 1 d . . H30A H 0.9190 0.4675 -0.1013 0.039 Uiso 1 1 calc R U C31 C 0.8640(11) 0.5694(8) -0.0501(3) 0.027(2) Uani 1 1 d . . H31A H 0.7792 0.5385 -0.0515 0.033 Uiso 1 1 calc R U C32 C 0.9062(9) 0.6608(8) -0.0182(3) 0.017(2) Uani 1 1 d . . C33 C 1.0372(10) 0.7057(9) -0.0173(3) 0.022(2) Uani 1 1 d . . C34 C 1.0796(9) 0.8055(9) 0.0132(3) 0.022(2) Uani 1 1 d . . C35 C 0.9996(10) 0.8578(9) 0.0446(3) 0.024(2) Uani 1 1 d . . C36 C 1.0427(10) 0.9653(9) 0.0678(3) 0.027(2) Uani 1 1 d . . H36A H 0.9883 1.0058 0.0861 0.033 Uiso 1 1 calc R U C37 C 1.1665(10) 1.0125(10) 0.0636(3) 0.030(3) Uani 1 1 d . . H37A H 1.1962 1.0842 0.0789 0.036 Uiso 1 1 calc R U C38 C 1.2447(11) 0.9494(10) 0.0359(3) 0.033(3) Uani 1 1 d . . H38A H 1.3302 0.9767 0.0351 0.040 Uiso 1 1 calc R U O1W O 0.3742(7) 0.5766(5) 0.9902(2) 0.0296(17) Uani 1 1 d . . H1WB H 0.3405 0.5062 0.9948 0.036 Uiso 1 1 d R U H1WC H 0.3175 0.6222 0.9751 0.036 Uiso 1 1 d R U loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.0195(2) 0.0195(2) 0.0171(2) -0.00058(17) 0.00338(15) 0.00146(19) F1 0.071(6) 0.048(4) 0.072(5) -0.012(4) 0.007(5) -0.032(4) F2 0.034(4) 0.081(5) 0.059(5) -0.005(4) -0.002(4) 0.000(4) F3 0.053(5) 0.052(4) 0.022(3) -0.004(3) 0.008(3) 0.004(3) F4 0.072(6) 0.054(4) 0.053(4) -0.011(4) 0.013(4) 0.032(4) N1 0.029(5) 0.024(4) 0.024(5) -0.001(4) 0.006(4) 0.000(4) N2 0.022(5) 0.022(4) 0.021(4) -0.004(3) 0.007(4) -0.005(4) N3 0.027(5) 0.022(4) 0.017(4) -0.001(3) 0.000(4) -0.003(4) N4 0.022(5) 0.031(5) 0.028(5) -0.005(4) 0.005(4) -0.006(4) N5 0.015(4) 0.023(4) 0.022(4) 0.001(4) 0.005(4) -0.004(4) N6 0.015(4) 0.024(4) 0.019(4) 0.002(3) 0.000(4) 0.003(4) N7 0.022(5) 0.036(5) 0.024(5) -0.005(4) 0.013(4) 0.006(4) N8 0.026(5) 0.040(5) 0.023(5) -0.003(4) 0.000(4) -0.010(4) C1 0.036(7) 0.023(5) 0.014(5) -0.010(4) 0.003(5) -0.009(5) C2 0.037(7) 0.050(8) 0.032(6) -0.006(5) 0.005(6) -0.012(6) C3 0.058(9) 0.025(6) 0.048(8) 0.001(5) -0.007(7) -0.011(6) C4 0.038(8) 0.071(10) 0.046(8) 0.001(7) 0.002(7) -0.032(7) C5 0.026(6) 0.058(8) 0.020(6) -0.009(5) -0.004(5) -0.002(6) C6 0.013(5) 0.041(6) 0.024(5) -0.002(5) 0.000(4) 0.000(5) C7 0.025(6) 0.036(6) 0.017(5) -0.004(4) 0.001(5) 0.002(5) C8 0.033(7) 0.053(8) 0.036(7) -0.003(6) 0.000(6) 0.025(6) C9 0.057(9) 0.032(6) 0.035(7) 0.013(5) -0.004(7) 0.024(6) C10 0.074(10) 0.027(6) 0.022(6) 0.005(5) 0.000(7) 0.016(6) C11 0.035(7) 0.037(6) 0.010(5) 0.006(4) -0.002(5) 0.008(5) C12 0.028(6) 0.020(5) 0.024(5) -0.003(4) 0.000(5) -0.006(5) C13 0.026(6) 0.030(6) 0.017(5) -0.006(4) 0.002(5) -0.003(5) C14 0.038(7) 0.044(7) 0.014(5) -0.007(5) 0.005(5) -0.018(6) C15 0.031(7) 0.042(7) 0.030(6) -0.013(5) 0.014(5) 0.009(5) C16 0.028(6) 0.029(6) 0.041(7) 0.005(5) -0.007(6) 0.010(5) C17 0.026(6) 0.035(6) 0.033(6) -0.001(5) 0.017(5) 0.006(5) C18 0.039(7) 0.018(5) 0.027(6) -0.004(4) 0.000(5) 0.001(5) C19 0.050(8) 0.034(6) 0.050(8) -0.001(6) 0.005(7) 0.022(6) C20 0.046(8) 0.050(7) 0.033(7) 0.008(6) 0.001(6) 0.022(6) C21 0.040(7) 0.028(6) 0.049(7) 0.012(5) 0.005(6) -0.001(5) C22 0.033(6) 0.036(6) 0.026(6) 0.008(5) 0.013(5) -0.001(5) C23 0.022(6) 0.034(6) 0.027(6) -0.004(5) 0.007(5) -0.014(5) C24 0.015(6) 0.044(6) 0.033(6) 0.007(5) 0.014(5) -0.006(5) C25 0.010(5) 0.018(4) 0.016(5) 0.003(4) -0.004(4) 0.004(4) C26 0.022(6) 0.024(5) 0.025(5) 0.003(4) 0.014(5) 0.007(4) C27 0.020(6) 0.026(5) 0.015(5) 0.003(4) 0.004(4) -0.006(5) C28 0.024(6) 0.016(5) 0.022(5) -0.003(4) 0.005(5) 0.006(4) C29 0.033(7) 0.027(6) 0.027(6) -0.009(4) 0.005(5) 0.006(5) C30 0.035(7) 0.044(7) 0.019(5) -0.014(5) 0.008(5) -0.007(6) C31 0.031(6) 0.025(5) 0.028(6) -0.007(4) 0.010(5) 0.000(5) C32 0.015(5) 0.018(5) 0.018(5) -0.001(4) -0.002(4) 0.005(4) C33 0.025(6) 0.025(5) 0.016(5) 0.002(4) -0.002(4) 0.002(5) C34 0.017(5) 0.027(5) 0.024(5) 0.007(4) 0.013(5) 0.002(4) C35 0.025(6) 0.024(5) 0.023(5) 0.007(4) 0.006(5) 0.012(5) C36 0.023(6) 0.028(5) 0.029(6) -0.006(5) -0.005(5) 0.007(5) C37 0.029(6) 0.039(6) 0.023(5) -0.004(5) 0.008(5) -0.015(5) C38 0.024(6) 0.048(6) 0.027(6) 0.014(5) 0.005(5) -0.010(5) O1W 0.030(4) 0.016(3) 0.042(4) -0.007(3) 0.002(4) -0.006(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C12 Ir1 C1 86.8(4) C12 Ir1 N2 80.5(3) C1 Ir1 N2 98.1(4) C12 Ir1 N1 97.7(4) C1 Ir1 N1 80.3(4) N2 Ir1 N1 177.6(3) C12 Ir1 N3 93.7(3) C1 Ir1 N3 177.1(4) N2 Ir1 N3 84.9(3) N1 Ir1 N3 96.8(3) C12 Ir1 N5 170.6(4) C1 Ir1 N5 102.4(3) N2 Ir1 N5 95.9(3) N1 Ir1 N5 86.2(3) N3 Ir1 N5 77.2(3) C11 N1 C7 120.3(9) C11 N1 Ir1 123.6(7) C7 N1 Ir1 116.1(7) C22 N2 C18 118.6(9) C22 N2 Ir1 124.7(7) C18 N2 Ir1 116.4(6) C25 N3 C23 106.5(8) C25 N3 Ir1 114.1(6) C23 N3 Ir1 139.1(6) C25 N4 C24 106.1(8) C25 N4 H4A 126.9 C24 N4 H4A 126.9 C26 N5 C27 101.8(7) C26 N5 Ir1 111.9(5) C27 N5 Ir1 144.6(6) C26 N6 C28 101.9(8) C33 N7 C29 117.9(9) C38 N8 C34 118.4(8) C2 C1 C6 119.6(10) C2 C1 Ir1 126.0(9) C6 C1 Ir1 114.3(7) C3 C2 C1 117.5(11) C3 C2 H2A 121.2 C1 C2 H2A 121.2 C4 C3 C2 124.7(11) C4 C3 F1 118.3(12) C2 C3 F1 117.0(12) C5 C4 C3 118.0(12) C5 C4 H4B 121.0 C3 C4 H4B 121.0 C4 C5 F2 119.7(11) C4 C5 C6 123.7(12) F2 C5 C6 116.5(10) C5 C6 C1 116.1(10) C5 C6 C7 128.6(10) C1 C6 C7 115.2(9) N1 C7 C8 118.9(10) N1 C7 C6 113.9(9) C8 C7 C6 127.2(10) C9 C8 C7 118.9(11) C9 C8 H8B 120.5 C7 C8 H8B 120.5 C10 C9 C8 122.3(11) C10 C9 H9A 118.9 C8 C9 H9A 118.9 C9 C10 C11 118.1(11) C9 C10 H10A 120.9 C11 C10 H10A 120.9 N1 C11 C10 121.5(11) N1 C11 H11A 119.2 C10 C11 H11A 119.2 C13 C12 C17 118.8(9) C13 C12 Ir1 126.6(7) C17 C12 Ir1 114.7(7) C14 C13 C12 119.3(9) C14 C13 H13A 120.3 C12 C13 H13A 120.3 C15 C14 F3 117.1(9) C15 C14 C13 124.0(10) F3 C14 C13 118.8(10) C14 C15 C16 116.0(9) C14 C15 H15A 122.0 C16 C15 H15A 122.0 F4 C16 C15 117.0(10) F4 C16 C17 118.4(10) C15 C16 C17 124.5(9) C16 C17 C12 117.3(10) C16 C17 C18 126.5(9) C12 C17 C18 116.2(9) C19 C18 N2 118.8(9) C19 C18 C17 129.3(10) N2 C18 C17 111.9(9) C18 C19 C20 121.1(11) C18 C19 H19A 119.4 C20 C19 H19A 119.4 C21 C20 C19 118.7(11) C21 C20 H20A 120.7 C19 C20 H20A 120.7 C20 C21 C22 118.9(11) C20 C21 H21A 120.5 C22 C21 H21A 120.5 N2 C22 C21 123.9(10) N2 C22 H22A 118.0 C21 C22 H22A 118.0 C24 C23 N3 110.4(8) C24 C23 H23A 124.8 N3 C23 H23A 124.8 C23 C24 N4 106.8(8) C23 C24 H24A 126.6 N4 C24 H24A 126.6 N4 C25 N3 110.2(8) N4 C25 C26 129.8(8) N3 C25 C26 120.0(8) N6 C26 N5 117.7(8) N6 C26 C25 126.3(9) N5 C26 C25 116.0(8) C28 C27 N5 108.7(8) C28 C27 C35 121.4(8) N5 C27 C35 129.9(8) C27 C28 N6 109.9(7) C27 C28 C32 122.9(9) N6 C28 C32 127.1(9) N7 C29 C30 124.2(9) N7 C29 H29A 117.9 C30 C29 H29A 117.9 C31 C30 C29 118.0(10) C31 C30 H30A 121.0 C29 C30 H30A 121.0 C30 C31 C32 120.0(10) C30 C31 H31A 120.0 C32 C31 H31A 120.0 C31 C32 C33 118.2(8) C31 C32 C28 124.4(9) C33 C32 C28 117.4(8) N7 C33 C32 121.5(9) N7 C33 C34 119.5(9) C32 C33 C34 119.0(8) N8 C34 C35 120.6(9) N8 C34 C33 116.2(8) C35 C34 C33 123.2(9) C36 C35 C34 118.3(9) C36 C35 C27 125.7(9) C34 C35 C27 115.6(9) C37 C36 C35 120.3(9) C37 C36 H36A 119.8 C35 C36 H36A 119.8 C36 C37 C38 118.0(10) C36 C37 H37A 121.0 C38 C37 H37A 121.0 N8 C38 C37 123.6(10) N8 C38 H38A 118.2 C37 C38 H38A 118.2 H1WB O1W H1WC 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ir1 C12 1.986(9) Ir1 C1 2.008(10) Ir1 N2 2.034(8) Ir1 N1 2.034(8) Ir1 N3 2.123(8) Ir1 N5 2.229(7) F1 C3 1.380(12) F2 C5 1.378(13) F3 C14 1.367(11) F4 C16 1.355(11) N1 C11 1.347(12) N1 C7 1.369(13) N2 C22 1.322(12) N2 C18 1.388(12) N3 C25 1.346(11) N3 C23 1.352(12) N4 C25 1.355(10) N4 C24 1.398(11) N4 H4A 0.8600 N5 C26 1.364(12) N5 C27 1.385(11) N6 C26 1.329(11) N6 C28 1.386(12) N7 C33 1.331(11) N7 C29 1.348(13) N8 C38 1.349(13) N8 C34 1.374(12) C1 C2 1.410(14) C1 C6 1.420(14) C2 C3 1.368(17) C2 H2A 0.9300 C3 C4 1.338(17) C4 C5 1.333(15) C4 H4B 0.9300 C5 C6 1.416(14) C6 C7 1.445(14) C7 C8 1.425(14) C8 C9 1.366(16) C8 H8B 0.9300 C9 C10 1.342(17) C9 H9A 0.9300 C10 C11 1.409(14) C10 H10A 0.9300 C11 H11A 0.9300 C12 C13 1.406(13) C12 C17 1.414(13) C13 C14 1.379(13) C13 H13A 0.9300 C14 C15 1.356(14) C15 C16 1.374(15) C15 H15A 0.9300 C16 C17 1.399(14) C17 C18 1.452(14) C18 C19 1.383(14) C19 C20 1.380(15) C19 H19A 0.9300 C20 C21 1.363(15) C20 H20A 0.9300 C21 C22 1.365(14) C21 H21A 0.9300 C22 H22A 0.9300 C23 C24 1.339(13) C23 H23A 0.9300 C24 H24A 0.9300 C25 C26 1.442(12) C27 C28 1.388(13) C27 C35 1.436(13) C28 C32 1.420(12) C29 C30 1.388(15) C29 H29A 0.9300 C30 C31 1.357(13) C30 H30A 0.9300 C31 C32 1.398(13) C31 H31A 0.9300 C32 C33 1.427(13) C33 C34 1.439(13) C34 C35 1.424(12) C35 C36 1.393(14) C36 C37 1.387(14) C36 H36A 0.9300 C37 C38 1.387(14) C37 H37A 0.9300 C38 H38A 0.9300 O1W H1WB 0.8500 O1W H1WC 0.8500