#------------------------------------------------------------------------------ #$Date: 2019-11-26 03:35:14 +0200 (Tue, 26 Nov 2019) $ #$Revision: 242518 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/25/4132557.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_4132557 loop_ _publ_author_name 'Lai, Po-Ni' 'Brysacz, Caroline H.' 'Alam, Md Kamrul' 'Ayoub, Nicholas A.' 'Gray, Thomas G.' 'Bao, Jiming' 'Teets, Thomas S.' _publ_section_title ; Highly Efficient Red-Emitting Bis-Cyclometalated Iridium Complexes. ; _journal_issue 32 _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 10198 _journal_page_last 10207 _journal_paper_doi 10.1021/jacs.8b04841 _journal_volume 140 _journal_year 2018 _chemical_formula_sum 'C39 H32 Cl4 Ir N3 O S2' _chemical_formula_weight 956.79 _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 geom _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 116.2263(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.9276(5) _cell_length_b 24.1615(10) _cell_length_c 13.3586(5) _cell_measurement_reflns_used 9980 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 27.51 _cell_measurement_theta_min 2.39 _cell_volume 3743.0(3) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 123(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.997 _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 0.0242 _diffrn_reflns_av_unetI/netI 0.0293 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 22840 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.548 _diffrn_reflns_theta_min 1.756 _exptl_absorpt_coefficient_mu 4.001 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.5701 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.698 _exptl_crystal_description block _exptl_crystal_F_000 1888 _exptl_crystal_size_max 0.360 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _refine_diff_density_max 2.394 _refine_diff_density_min -2.509 _refine_diff_density_rms 0.162 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 527 _refine_ls_number_reflns 8612 _refine_ls_number_restraints 405 _refine_ls_restrained_S_all 1.036 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0387 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+22.3510P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1050 _refine_ls_wR_factor_ref 0.1095 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7428 _reflns_number_total 8612 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja8b04841_si_002.cif _cod_data_source_block 4 _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 4132557 _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 0.327 _shelx_estimated_absorpt_t_max 0.690 _shelx_res_file ; bl9.res created by SHELXL-2014/7 TITL BL9 in P2(1)/c CELL 0.71073 12.92760 24.16150 13.35860 90.0000 116.2263 90.0000 ZERR 4.00 0.00050 0.00100 0.00050 0.0000 0.0004 0.0000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O S IR CL UNIT 156 128 12 4 8 4 16 TEMP -150.010 SIZE 0.10 0.20 0.36 L.S. 16 BOND FMAP 2 PLAN 70 sadi n3 c51 n3 c51a sadi c51 c52 c52 c53 c53 c54 c54 c55 c55 c56 c56 c51 = C51 C52A C52A C53A C53A C54A C54A C55A C55A C56A C56A C51 sadi 0.04 c51 c53 c52 c54 c53 c55 c54 c56 c55 c51 c56 c52 = C51 C53A C52A C54A C53A C55A C54A C56A C55A C51 C56A C52A simu c51 c52 c53 c54 c55 c56 c51a c52a c53a c54a c55a c56a n3 = C1S C2S CL1S CL2S CL3S CL4S C1SA CL1A CL2A delu c51 c52 c53 c54 c55 c56 c51a c52a c53a c54a c55a c56a n3 = C1S C2S CL1S CL2S CL3S CL4S C1SA CL1A CL2A sadi c1s cl1s c1s cl2s c1sa cl1a c1sa cl2a sadi 0.04 cl1s cl2s cl1a cl2a acta WGHT 0.052300 22.350998 FVAR 0.06585 0.65066 0.51045 O1 4 0.048378 1.052922 -0.256386 11.00000 0.02597 0.02624 = 0.02628 -0.00477 0.01103 -0.00315 IR1 6 0.181994 1.104745 -0.141530 11.00000 0.01851 0.01903 = 0.01937 -0.00039 0.00926 0.00063 S1 5 -0.057977 1.153711 0.005861 11.00000 0.02942 0.03114 = 0.03303 0.00269 0.02179 0.00252 S2 5 0.430030 1.247688 -0.028524 11.00000 0.02386 0.03043 = 0.02632 0.00076 0.00913 -0.00702 CL3S 7 0.209167 1.140783 0.322700 11.00000 0.12960 0.10438 = 0.12274 -0.00566 0.05751 -0.01764 CL4S 7 0.364581 1.048354 0.436534 11.00000 0.12620 0.11619 = 0.19357 0.01878 0.07494 -0.00491 N1 3 0.177958 1.054799 -0.018281 11.00000 0.02305 0.02065 = 0.02182 -0.00124 0.00874 -0.00099 N2 3 0.181896 1.156862 -0.262856 11.00000 0.01911 0.02299 = 0.01928 0.00127 0.00960 0.00209 N3 3 0.303576 1.055298 -0.171307 11.00000 0.02683 0.02827 = 0.02316 0.00231 0.01320 0.00920 C1 1 -0.043134 0.974984 -0.367328 11.00000 0.04723 0.04150 = 0.04591 -0.01598 0.01826 -0.01184 AFIX 137 H1A 2 -0.026281 0.935244 -0.361342 11.00000 -1.50000 H1B 2 -0.069786 0.986802 -0.444980 11.00000 -1.50000 H1C 2 -0.103347 0.982435 -0.343400 11.00000 -1.50000 AFIX 0 C2 1 0.064921 1.006580 -0.293650 11.00000 0.04031 0.03183 = 0.03181 -0.00552 0.01372 -0.00191 C2S 1 0.307438 1.107703 0.443649 11.00000 0.12247 0.10202 = 0.14247 0.04525 0.05767 0.00918 AFIX 23 H2S1 2 0.371769 1.133852 0.482851 11.00000 -1.20000 H2S2 2 0.268542 1.102254 0.492245 11.00000 -1.20000 AFIX 0 C3 1 0.169925 0.983807 -0.276216 11.00000 0.04996 0.03777 = 0.05185 -0.01904 0.01663 0.00456 AFIX 43 H3 2 0.167888 0.946485 -0.299390 11.00000 -1.20000 AFIX 0 C4 1 0.279889 1.009282 -0.228134 11.00000 0.04244 0.04291 = 0.03321 -0.00659 0.01303 0.00875 C5 1 0.371286 0.978756 -0.249022 11.00000 0.05213 0.05755 = 0.05382 -0.02050 0.01927 0.01844 AFIX 137 H5A 2 0.361865 0.987212 -0.324332 11.00000 -1.50000 H5B 2 0.362910 0.938815 -0.242102 11.00000 -1.50000 H5C 2 0.448024 0.990555 -0.194101 11.00000 -1.50000 AFIX 0 C11 1 0.042003 1.120581 -0.028010 11.00000 0.02035 0.02324 = 0.02479 -0.00241 0.01118 -0.00333 C12 1 0.240289 1.008290 0.022284 11.00000 0.03027 0.02383 = 0.03156 0.00023 0.01284 0.00093 AFIX 43 H12 2 0.292415 0.996892 -0.006264 11.00000 -1.20000 AFIX 0 C13 1 0.230693 0.976523 0.104488 11.00000 0.04668 0.02196 = 0.03404 0.00544 0.01518 0.00500 AFIX 43 H13 2 0.276326 0.944189 0.132252 11.00000 -1.20000 AFIX 0 C14 1 0.154012 0.992512 0.145365 11.00000 0.05448 0.02358 = 0.02962 0.00424 0.02023 -0.00502 AFIX 43 H14 2 0.146107 0.971163 0.201308 11.00000 -1.20000 AFIX 0 C15 1 0.088966 1.039803 0.104175 11.00000 0.03754 0.02864 = 0.02708 -0.00001 0.01644 -0.00225 AFIX 43 H15 2 0.035715 1.051153 0.131390 11.00000 -1.20000 AFIX 0 C16 1 0.101907 1.070772 0.022459 11.00000 0.02344 0.02133 = 0.02284 -0.00135 0.01065 -0.00308 C20 1 0.064838 1.146264 -0.108530 11.00000 0.01470 0.02404 = 0.01939 -0.00155 0.00645 -0.00122 C21 1 -0.003191 1.196879 -0.144415 11.00000 0.01627 0.02359 = 0.02297 -0.00083 0.00878 0.00005 C22 1 -0.073775 1.205593 -0.089584 11.00000 0.01965 0.02885 = 0.02719 -0.00240 0.01139 -0.00327 C23 1 -0.148252 1.251234 -0.113826 11.00000 0.02467 0.03490 = 0.04058 -0.00172 0.02030 0.00346 AFIX 43 H23 2 -0.195866 1.255817 -0.076916 11.00000 -1.20000 AFIX 0 C24 1 -0.151236 1.288943 -0.191251 11.00000 0.02303 0.03422 = 0.04076 0.00208 0.01308 0.00798 AFIX 43 H24 2 -0.201510 1.319900 -0.208554 11.00000 -1.20000 AFIX 0 C25 1 -0.080500 1.282250 -0.245414 11.00000 0.02748 0.02982 = 0.03233 0.00735 0.01252 0.00391 AFIX 43 H25 2 -0.082913 1.308981 -0.298556 11.00000 -1.20000 AFIX 0 C26 1 -0.007241 1.237215 -0.222446 11.00000 0.02480 0.03022 = 0.02720 0.00302 0.01295 0.00256 AFIX 43 H26 2 0.040511 1.233464 -0.259408 11.00000 -1.20000 AFIX 0 C31 1 0.319374 1.201422 -0.105759 11.00000 0.01770 0.02238 = 0.02388 -0.00066 0.00789 -0.00065 C32 1 0.118575 1.148962 -0.372815 11.00000 0.01809 0.03405 = 0.02303 -0.00058 0.00794 -0.00138 AFIX 43 H32 2 0.068508 1.117894 -0.397482 11.00000 -1.20000 AFIX 0 C33 1 0.123916 1.184380 -0.450727 11.00000 0.02404 0.04094 = 0.02076 0.00460 0.00614 -0.00081 AFIX 43 H33 2 0.077510 1.178141 -0.528081 11.00000 -1.20000 AFIX 0 C34 1 0.198296 1.229602 -0.414858 11.00000 0.02730 0.04140 = 0.02792 0.00827 0.01111 -0.00009 AFIX 43 H34 2 0.203288 1.254587 -0.467464 11.00000 -1.20000 AFIX 0 C35 1 0.264873 1.237686 -0.301570 11.00000 0.01871 0.03025 = 0.02956 0.00519 0.01124 -0.00022 AFIX 43 H35 2 0.316081 1.268303 -0.275835 11.00000 -1.20000 AFIX 0 C36 1 0.256402 1.200782 -0.225695 11.00000 0.01608 0.02315 = 0.02529 0.00136 0.01027 0.00192 C40 1 0.300716 1.159803 -0.046135 11.00000 0.01392 0.02277 = 0.02319 -0.00176 0.01102 0.00165 C41 1 0.379074 1.165719 0.071534 11.00000 0.01855 0.02360 = 0.02258 -0.00192 0.00967 0.00227 C42 1 0.455567 1.211281 0.092141 11.00000 0.01928 0.02626 = 0.02593 0.00108 0.00951 0.00097 C43 1 0.541045 1.223488 0.198625 11.00000 0.02324 0.03315 = 0.03134 -0.00570 0.00927 -0.00339 AFIX 43 H43 2 0.591422 1.254039 0.210605 11.00000 -1.20000 AFIX 0 C44 1 0.550844 1.189997 0.286683 11.00000 0.01846 0.04009 = 0.02349 -0.00272 0.00413 0.00020 AFIX 43 H44 2 0.608597 1.197681 0.359864 11.00000 -1.20000 AFIX 0 C45 1 0.476583 1.145001 0.268925 11.00000 0.02201 0.03524 = 0.02178 0.00446 0.00700 0.00799 AFIX 43 H45 2 0.484092 1.122583 0.330194 11.00000 -1.20000 AFIX 0 C46 1 0.392216 1.132867 0.162777 11.00000 0.02237 0.02586 = 0.02427 0.00219 0.00965 0.00331 AFIX 43 H46 2 0.342846 1.101993 0.151784 11.00000 -1.20000 AFIX 0 C51 1 0.412628 1.080716 -0.144301 11.00000 0.03176 0.02768 = 0.05533 0.00153 0.02784 0.00914 PART 1 C52 1 0.419801 1.103382 -0.238509 21.00000 0.03362 0.02478 = 0.05983 -0.00613 0.03090 -0.00439 AFIX 43 H52 2 0.360022 1.097618 -0.311568 21.00000 -1.20000 AFIX 0 C53 1 0.517814 1.134666 -0.221033 21.00000 0.02829 0.03846 = 0.07025 0.00551 0.03380 0.00344 AFIX 43 H53 2 0.524772 1.151266 -0.282241 21.00000 -1.20000 AFIX 0 C54 1 0.605402 1.141124 -0.112052 21.00000 0.02464 0.03959 = 0.07903 0.00017 0.02531 -0.00179 AFIX 43 H54 2 0.670719 1.163230 -0.099723 21.00000 -1.20000 AFIX 0 C55 1 0.598467 1.115851 -0.021943 21.00000 0.03028 0.03372 = 0.06914 -0.00283 0.02790 0.00153 AFIX 43 H55 2 0.660605 1.119313 0.050548 21.00000 -1.20000 AFIX 0 C56 1 0.500948 1.085383 -0.036922 21.00000 0.02132 0.03359 = 0.06188 -0.00855 0.01847 0.00251 AFIX 43 H56 2 0.495202 1.068354 0.024526 21.00000 -1.20000 AFIX 0 PART 2 C52A 1 0.488210 1.076496 -0.028753 -21.00000 0.02419 0.02338 = 0.06443 -0.01696 0.01911 -0.00680 AFIX 43 H52A 2 0.465893 1.053670 0.016272 -21.00000 -1.20000 AFIX 0 C53A 1 0.594372 1.104361 0.022443 -21.00000 0.03358 0.02832 = 0.07870 -0.00699 0.04032 -0.00808 AFIX 43 H53A 2 0.642319 1.099834 0.100025 -21.00000 -1.20000 AFIX 0 C54A 1 0.629014 1.138612 -0.040923 -21.00000 0.04101 0.04020 = 0.08293 0.00884 0.04236 0.00402 AFIX 43 H54A 2 0.699409 1.158634 -0.007435 -21.00000 -1.20000 AFIX 0 C55A 1 0.556796 1.142677 -0.155798 -21.00000 0.03709 0.04485 = 0.08577 0.01094 0.03552 0.00155 AFIX 43 H55A 2 0.581702 1.163687 -0.201236 -21.00000 -1.20000 AFIX 0 C56A 1 0.449413 1.116696 -0.205069 -21.00000 0.03911 0.02570 = 0.08920 0.01096 0.03964 0.00492 AFIX 43 H56A 2 0.399869 1.123456 -0.281557 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C1S 1 -0.171185 1.134481 -0.382550 31.00000 0.03848 0.03836 = 0.03395 -0.01837 0.01545 -0.00581 AFIX 23 H1S1 2 -0.146340 1.172461 -0.389480 31.00000 -1.20000 H1S2 2 -0.104447 1.115088 -0.323921 31.00000 -1.20000 AFIX 0 CL1S 7 -0.281403 1.137980 -0.342864 31.00000 0.04871 0.10899 = 0.10280 -0.06241 0.04398 -0.01636 CL2S 7 -0.212713 1.100236 -0.507700 31.00000 0.07234 0.04870 = 0.02303 -0.01511 0.01160 -0.01601 PART 2 CL1A 7 -0.313537 1.118540 -0.358879 -31.00000 0.14145 0.17567 = 0.15438 0.11801 0.11073 0.09478 C1SA 1 -0.191328 1.127737 -0.376403 -31.00000 0.06751 0.07976 = 0.04122 0.01376 0.00147 0.01235 AFIX 23 H1S3 2 -0.166218 1.166677 -0.358138 -31.00000 -1.20000 H1S4 2 -0.129860 1.104076 -0.321595 -31.00000 -1.20000 AFIX 0 CL2A 7 -0.201967 1.113515 -0.505800 -31.00000 0.05663 0.15342 = 0.04906 0.04237 0.01998 0.03478 HKLF 4 REM BL9 in P2(1)/c REM R1 = 0.0387 for 7428 Fo > 4sig(Fo) and 0.0466 for all 8612 data REM 527 parameters refined using 405 restraints END WGHT 0.0523 22.3509 REM Highest difference peak 2.394, deepest hole -2.509, 1-sigma level 0.162 Q1 1 0.4735 1.0287 0.5002 11.00000 0.05 2.39 Q2 1 0.1981 1.1057 -0.0804 11.00000 0.05 1.76 Q3 1 0.1130 1.1050 -0.1520 11.00000 0.05 1.51 Q4 1 0.2184 1.1389 -0.1078 11.00000 0.05 1.34 Q5 1 -0.2943 1.1758 -0.3916 11.00000 0.05 1.28 Q6 1 0.1853 1.0704 -0.1342 11.00000 0.05 1.24 Q7 1 0.2528 1.1069 -0.1384 11.00000 0.05 1.20 Q8 1 0.1866 1.1016 -0.2066 11.00000 0.05 0.79 Q9 1 0.2265 1.0741 -0.1925 11.00000 0.05 0.62 Q10 1 0.2046 1.1391 -0.2132 11.00000 0.05 0.61 Q11 1 -0.2268 1.1421 -0.3724 11.00000 0.05 0.54 Q12 1 -0.3261 1.1341 -0.4076 11.00000 0.05 0.53 Q13 1 0.4278 1.1397 -0.0328 11.00000 0.05 0.52 Q14 1 -0.0678 1.2523 -0.2545 11.00000 0.05 0.49 Q15 1 -0.1426 1.2776 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4 311.70 6.47 4 3 -4 326.28 6.45 -4 3 4 316.40 6.43 -3 3 4 104.55 2.27 -3 3 4 104.19 2.19 3 3 -4 106.56 2.24 2 3 -4 56.05 1.25 -2 3 4 55.72 1.29 -1 -3 4 240.05 4.96 -1 3 4 241.36 4.95 1 3 -4 247.66 4.93 0 -3 4 30.40 0.82 0 3 -4 31.98 0.78 0 3 4 30.01 0.78 1 -3 4 193.16 4.10 -1 -3 -4 204.24 3.96 1 3 4 189.92 4.05 -1 3 -4 195.76 4.03 1 3 4 192.08 4.02 -2 -3 -4 135.32 2.78 2 -3 4 127.72 2.89 2 3 4 130.73 2.84 2 3 4 128.76 2.80 -2 3 -4 132.04 2.82 -3 -3 -4 14.17 0.54 3 -3 4 13.05 0.62 3 3 4 13.09 0.56 -3 3 -4 13.74 0.56 3 3 4 13.39 0.52 -4 -3 -4 153.66 3.34 4 -3 4 153.05 3.47 4 3 4 151.19 3.32 -4 3 -4 152.38 3.38 4 3 4 153.72 3.38 -5 -3 -4 52.85 1.44 5 -3 4 51.29 1.54 5 3 4 52.08 1.47 -5 3 -4 54.53 1.48 5 3 4 52.79 1.42 -6 -3 -4 25.51 0.94 6 -3 4 23.19 1.02 -6 3 -4 23.58 0.95 6 3 4 25.19 0.99 6 3 4 24.45 0.92 -7 -3 -4 38.39 1.29 7 -3 4 38.39 1.39 -7 3 -4 39.25 1.33 7 3 4 38.39 1.29 7 3 4 37.62 1.33 -8 -3 -4 54.65 1.66 8 -3 4 52.07 1.74 8 3 4 53.63 1.65 8 3 4 52.70 1.69 -8 3 -4 53.26 1.70 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4 -4 73.08 1.66 -2 -4 -4 30.35 0.79 2 -4 4 28.88 0.90 2 4 4 30.07 0.84 -2 4 -4 28.30 0.83 2 4 4 28.78 0.82 -3 -4 -4 76.42 1.76 3 -4 4 72.88 1.87 3 4 4 74.68 1.77 3 4 4 75.96 1.79 -3 4 -4 76.40 1.80 -4 -4 -4 81.55 1.97 4 -4 4 82.27 2.11 -4 4 -4 85.76 2.03 4 4 4 85.68 2.02 4 4 4 81.82 1.98 -5 -4 -4 28.66 0.95 5 -4 4 27.72 1.05 -5 4 -4 28.23 0.98 5 4 4 28.82 0.95 5 4 4 27.97 0.97 -6 -4 -4 54.73 1.52 6 -4 4 52.61 1.64 6 4 4 52.40 1.55 6 4 4 51.54 1.51 -6 4 -4 56.02 1.59 -7 -4 -4 21.11 0.93 7 -4 4 21.62 1.04 7 4 4 20.88 0.95 7 4 4 20.10 0.95 -7 4 -4 21.04 0.97 8 -4 4 21.38 1.09 -8 -4 -4 22.25 1.00 -8 4 -4 21.33 1.05 8 4 4 21.82 1.04 8 4 4 21.25 1.04 9 -4 4 39.83 1.56 -9 -4 -4 39.42 1.43 -9 4 -4 38.84 1.49 9 4 4 38.01 1.47 9 4 4 40.42 1.47 -10 -4 -4 0.15 0.45 -10 4 -4 0.28 0.46 10 4 4 0.30 0.47 -11 -4 -4 29.92 1.40 -11 4 -4 32.05 1.47 -12 -4 -4 27.93 1.41 -12 4 -4 29.15 1.48 -16 -5 4 0.79 0.69 -16 5 4 0.00 0.66 -15 -5 4 3.70 0.79 -15 5 4 3.69 0.76 -14 -5 4 1.71 0.62 -14 5 4 2.99 0.68 -13 -5 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17.84 1.32 -13 -2 15 0.95 0.53 -13 2 15 1.87 0.58 -12 -2 15 52.37 1.84 -12 2 15 52.67 1.86 -11 -2 15 35.70 1.43 -11 2 15 36.85 1.48 -10 -2 15 2.52 0.52 -10 2 15 3.37 0.55 -9 -2 15 40.01 1.45 -9 2 15 39.89 1.47 -8 2 15 13.20 0.86 -7 -2 15 25.70 1.24 -7 2 15 21.81 1.05 -6 -2 15 61.72 2.02 -6 2 15 59.50 2.02 -5 -2 15 2.43 0.59 -5 2 15 1.38 0.54 -4 -2 15 61.04 2.04 -4 2 15 54.22 1.99 -3 -2 15 47.17 1.82 -3 2 15 47.08 1.82 -2 -2 15 0.43 0.55 -2 2 15 0.76 0.53 -1 -2 15 27.48 1.51 -1 2 15 29.44 1.50 0 -2 15 7.70 0.93 0 2 15 7.59 0.94 1 -2 15 3.43 0.79 1 2 15 3.12 0.77 -13 -3 15 2.33 0.59 -13 3 15 2.95 0.65 -12 -3 15 1.05 0.49 -12 3 15 1.86 0.55 -11 -3 15 8.06 0.75 -11 3 15 8.32 0.82 -10 -3 15 3.77 0.56 -10 3 15 3.02 0.55 -9 3 15 2.04 0.47 -8 3 15 7.53 0.70 -7 -3 15 14.67 1.01 -7 3 15 12.30 0.85 -6 -3 15 1.53 0.51 -5 -3 15 3.34 0.65 -5 3 15 2.39 0.60 -4 -3 15 8.32 0.89 -4 3 15 8.13 0.85 -3 -3 15 0.93 0.53 -3 3 15 0.63 0.51 -2 -3 15 3.96 0.72 -2 3 15 5.45 0.79 -1 -3 15 -0.42 0.56 -1 3 15 0.17 0.53 0 -3 15 5.19 0.86 0 3 15 4.36 0.82 1 -3 15 3.67 0.78 1 3 15 3.44 0.77 -13 -4 15 0.60 0.51 -13 4 15 -0.08 0.48 -12 -4 15 2.99 0.58 -12 4 15 2.62 0.58 -11 -4 15 2.28 0.55 -11 4 15 1.59 0.49 -10 -4 15 0.93 0.41 -10 4 15 1.16 0.45 -9 4 15 13.71 0.90 -8 -4 15 4.80 0.68 -8 4 15 5.35 0.64 -7 -4 15 7.74 0.80 -7 4 15 5.82 0.63 -6 -4 15 17.05 1.06 -6 4 15 14.94 0.90 -5 -4 15 2.88 0.62 -5 4 15 2.95 0.64 -4 -4 15 11.97 0.99 -4 4 15 9.92 0.94 -3 -4 15 9.02 0.92 -3 4 15 10.51 1.00 -2 -4 15 0.01 0.52 -2 4 15 1.04 0.58 -1 -4 15 5.07 0.81 -1 4 15 6.85 0.88 0 -4 15 4.30 0.81 0 4 15 4.91 0.80 -13 -5 15 30.19 1.42 -13 5 15 28.41 1.42 -12 -5 15 2.29 0.58 -12 5 15 2.72 0.60 -11 -5 15 20.55 1.10 -11 5 15 21.95 1.15 -10 5 15 23.99 1.16 -9 5 15 0.79 0.42 -8 -5 15 35.83 1.43 -8 5 15 31.45 1.31 -7 -5 15 26.83 1.28 -7 5 15 29.62 1.23 -6 -5 15 0.23 0.46 -6 5 15 0.27 0.37 -5 -5 15 37.48 1.55 -5 5 15 38.80 1.57 -4 -5 15 24.98 1.31 -4 5 15 24.34 1.31 -3 -5 15 7.32 0.85 -3 5 15 6.12 0.78 -2 -5 15 47.29 1.89 -2 5 15 50.14 1.92 -1 -5 15 11.30 1.05 -1 5 15 11.18 1.06 0 -5 15 16.84 1.33 0 5 15 15.34 1.25 -13 -6 15 0.20 0.49 -13 6 15 0.75 0.52 -12 -6 15 13.26 0.96 -12 6 15 11.36 0.96 -11 -6 15 8.17 0.78 -11 6 15 7.77 0.78 -10 6 15 4.38 0.61 -9 -6 15 19.99 1.09 -9 6 15 20.07 1.06 -8 -6 15 13.73 0.97 -8 6 15 14.70 0.93 -7 -6 15 17.59 1.07 -7 6 15 15.44 0.95 -6 -6 15 14.62 1.03 -6 6 15 13.06 0.87 -5 -6 15 0.30 0.46 -5 6 15 0.48 0.51 -5 6 15 -0.12 0.44 -4 -6 15 20.81 1.22 -4 6 15 21.64 1.23 -3 -6 15 19.36 1.25 -3 6 15 23.28 1.30 -2 -6 15 0.43 0.56 -2 6 15 -0.49 0.48 -1 -6 15 15.81 1.25 -1 6 15 17.93 1.25 0 -6 15 4.68 0.84 0 6 15 5.13 0.84 -13 -7 15 0.66 0.52 -13 7 15 0.71 0.50 -12 -7 15 0.01 0.43 -12 7 15 -0.05 0.45 -11 7 15 -0.45 0.37 -10 7 15 0.69 0.42 -9 -7 15 0.12 0.42 -9 7 15 -0.29 0.35 -8 -7 15 -0.24 0.39 -8 7 15 0.04 0.37 -7 -7 15 0.06 0.44 -7 7 15 -0.42 0.36 -6 -7 15 0.69 0.48 -6 7 15 0.27 0.40 -5 -7 15 5.01 0.69 -5 7 15 2.99 0.55 -5 7 15 2.27 0.58 -4 -7 15 1.12 0.54 -4 7 15 2.03 0.58 -3 -7 15 0.26 0.51 -3 7 15 -0.26 0.46 -2 -7 15 -0.43 0.53 -2 7 15 -0.07 0.49 -1 -7 15 0.45 0.57 -1 7 15 0.41 0.54 0 -7 15 0.09 0.62 0 7 15 -0.48 0.55 -12 -8 15 13.61 1.01 -12 8 15 13.80 1.03 -11 8 15 7.15 0.79 -10 8 15 5.08 0.67 -9 8 15 52.91 1.81 -8 -8 15 7.08 0.74 -8 8 15 6.31 0.69 -7 -8 15 12.94 0.96 -7 8 15 11.91 0.89 -6 -8 15 36.63 1.49 -6 8 15 34.72 1.39 -5 -8 15 1.79 0.54 -5 8 15 0.78 0.43 -4 -8 15 10.45 0.97 -4 8 15 10.30 0.95 -3 -8 15 10.57 1.00 -3 8 15 13.36 1.07 -2 -8 15 4.46 0.74 -2 8 15 5.87 0.81 -1 -8 15 32.72 1.65 -1 8 15 33.40 1.60 0 -8 15 18.29 1.40 0 8 15 19.13 1.35 -12 9 15 4.93 0.71 -11 9 15 9.62 0.88 -10 9 15 30.31 1.37 -9 9 15 4.84 0.65 -8 9 15 20.10 1.11 -7 -9 15 16.12 1.04 -7 9 15 18.05 1.03 -6 -9 15 2.95 0.58 -6 9 15 1.81 0.51 -5 -9 15 22.29 1.22 -5 9 15 21.70 1.13 -4 -9 15 6.74 0.81 -4 9 15 8.62 0.78 -4 9 15 9.03 0.91 -3 -9 15 4.82 0.75 -3 9 15 5.09 0.77 -2 -9 15 33.35 1.63 -2 9 15 36.26 1.63 -1 -9 15 8.91 1.01 -1 9 15 8.16 0.94 -12 10 15 -0.26 0.43 -11 10 15 1.83 0.56 -10 10 15 -0.43 0.40 -9 10 15 4.87 0.67 -8 10 15 4.10 0.62 -7 -10 15 0.34 0.55 -7 10 15 0.56 0.42 -6 -10 15 3.04 0.60 -6 10 15 1.88 0.50 -5 -10 15 1.33 0.53 -5 10 15 0.41 0.41 -4 -10 15 1.91 0.60 -4 10 15 2.33 0.55 -4 10 15 2.82 0.63 -3 -10 15 4.21 0.70 -3 10 15 5.89 0.81 -2 -10 15 1.17 0.62 -2 10 15 0.24 0.56 -1 -10 15 3.04 0.75 -1 10 15 3.24 0.74 -11 11 15 6.83 0.77 -10 11 15 14.78 1.03 -9 11 15 0.14 0.45 -8 11 15 7.24 0.77 -7 11 15 4.69 0.64 -6 -11 15 1.12 0.55 -6 11 15 1.24 0.50 -5 -11 15 7.96 0.83 -5 11 15 7.53 0.78 -4 -11 15 0.12 0.49 -4 11 15 1.11 0.49 -4 11 15 0.53 0.51 -3 -11 15 2.24 0.64 -3 11 15 1.46 0.60 -3 11 15 2.16 0.68 -2 -11 15 7.56 0.93 -2 11 15 8.02 0.95 -1 -11 15 1.15 0.64 -1 11 15 0.61 0.60 -11 12 15 11.24 0.97 -10 12 15 6.78 0.78 -9 12 15 55.46 1.91 -8 12 15 10.04 0.88 -7 12 15 10.32 0.91 -6 12 15 29.82 1.35 -5 -12 15 0.05 0.50 -5 12 15 0.95 0.50 -4 -12 15 21.91 1.28 -4 12 15 23.09 1.31 -4 12 15 21.90 1.18 -3 -12 15 11.84 1.05 -3 12 15 12.06 0.96 -3 12 15 11.91 1.05 -2 12 15 1.52 0.63 -10 13 15 18.18 1.15 -9 13 15 1.63 0.56 -8 13 15 2.86 0.62 -7 13 15 1.97 0.53 -6 13 15 1.77 0.56 -5 13 15 10.64 0.91 -4 -13 15 6.91 0.92 -4 13 15 6.63 0.83 -4 13 15 6.06 0.75 -3 -13 15 1.49 0.64 -3 13 15 1.38 0.54 -3 13 15 1.73 0.59 -10 14 15 0.14 0.46 -9 14 15 0.38 0.47 -8 14 15 -0.42 0.45 -7 14 15 0.76 0.52 -6 14 15 1.62 0.55 -5 14 15 0.06 0.46 -4 14 15 2.58 0.64 -4 14 15 3.35 0.65 -3 -14 15 3.16 0.91 -3 14 15 1.83 0.59 -3 14 15 4.08 0.74 -8 15 15 16.21 1.12 -7 15 15 20.26 1.20 -6 15 15 1.29 0.56 -5 15 15 18.59 1.17 -4 15 15 5.99 0.82 -12 0 16 50.64 1.84 -11 0 16 0.75 0.47 -10 0 16 21.12 1.11 -7 0 16 75.30 2.38 -6 0 16 16.31 1.18 -5 0 16 9.73 0.94 -4 0 16 38.60 1.71 -3 0 16 1.59 0.63 -2 0 16 27.49 1.53 -1 0 16 7.42 0.98 -12 -1 16 4.79 0.71 -12 1 16 3.36 0.64 -11 -1 16 31.57 1.37 -11 1 16 29.75 1.37 -10 -1 16 3.25 0.59 -10 1 16 4.57 0.65 -9 1 16 0.97 0.42 -7 -1 16 1.72 0.56 -7 1 16 0.35 0.51 -6 -1 16 8.72 0.92 -6 1 16 11.11 1.00 -5 -1 16 13.19 1.13 -5 1 16 13.13 1.11 -4 -1 16 -0.22 0.50 -4 1 16 0.25 0.51 -3 -1 16 23.55 1.42 -3 1 16 22.99 1.39 -2 -1 16 5.97 0.88 -2 1 16 5.71 0.85 -1 -1 16 -0.79 0.57 -1 1 16 -0.48 0.57 -12 -2 16 2.41 0.56 -12 2 16 3.56 0.66 -11 -2 16 -0.24 0.41 -11 2 16 -0.74 0.39 -10 2 16 2.24 0.52 -9 2 16 7.63 0.78 -8 -2 16 0.88 0.53 -7 -2 16 1.06 0.52 -7 2 16 0.63 0.52 -6 -2 16 3.22 0.67 -6 2 16 2.95 0.67 -5 -2 16 3.06 0.69 -5 2 16 2.76 0.67 -4 -2 16 4.80 0.78 -4 2 16 3.84 0.75 -3 -2 16 1.55 0.62 -3 2 16 2.01 0.67 -2 -2 16 0.27 0.59 -2 2 16 -0.25 0.53 -12 -3 16 4.13 0.64 -12 3 16 3.45 0.63 -11 -3 16 26.62 1.27 -11 3 16 26.40 1.27 -10 3 16 10.34 0.87 -9 3 16 14.70 0.97 -8 -3 16 31.44 1.45 -8 3 16 30.30 1.37 -7 -3 16 3.25 0.67 -6 -3 16 16.52 1.15 -6 3 16 15.49 1.14 -5 -3 16 44.12 1.79 -5 3 16 44.00 1.81 -4 -3 16 0.85 0.58 -4 3 16 0.50 0.54 -3 -3 16 24.42 1.41 -3 3 16 24.27 1.42 -2 -3 16 30.13 1.60 -2 3 16 28.77 1.56 -12 -4 16 16.81 1.08 -12 4 16 16.80 1.10 -11 4 16 -0.11 0.41 -10 4 16 21.89 1.16 -9 -4 16 30.35 1.40 -9 4 16 26.51 1.26 -8 -4 16 10.24 0.94 -8 4 16 10.21 0.83 -7 -4 16 26.47 1.35 -6 -4 16 19.53 1.23 -6 4 16 19.86 1.24 -5 -4 16 11.17 1.03 -5 4 16 15.23 1.15 -4 -4 16 22.10 1.35 -4 4 16 23.27 1.37 -3 -4 16 2.20 0.68 -3 4 16 2.36 0.67 -2 -4 16 13.79 1.19 -2 4 16 12.02 1.12 -12 -5 16 3.74 0.66 -12 5 16 2.27 0.59 -11 5 16 3.25 0.61 -10 5 16 3.28 0.58 -9 -5 16 0.01 0.47 -9 5 16 -0.11 0.40 -8 -5 16 -0.69 0.43 -8 5 16 0.01 0.40 -7 -5 16 -0.35 0.46 -7 5 16 0.07 0.50 -6 -5 16 0.20 0.48 -6 5 16 -0.22 0.48 -5 -5 16 -0.12 0.50 -5 5 16 -0.41 0.46 -4 -5 16 2.64 0.69 -4 5 16 1.65 0.61 -3 -5 16 0.23 0.54 -3 5 16 1.83 0.64 -2 -5 16 6.37 0.89 -2 5 16 5.33 0.88 -11 6 16 -0.26 0.40 -10 -6 16 13.32 1.03 -10 6 16 10.32 0.87 -9 -6 16 9.06 0.89 -9 6 16 9.37 0.85 -8 -6 16 -0.12 0.45 -8 6 16 -0.12 0.39 -7 -6 16 20.94 1.24 -7 6 16 22.72 1.14 -6 -6 16 2.05 0.61 -6 6 16 2.29 0.65 -5 -6 16 2.41 0.63 -5 6 16 1.81 0.61 -4 -6 16 23.31 1.37 -4 6 16 25.47 1.41 -3 -6 16 1.88 0.68 -3 6 16 1.47 0.63 -2 -6 16 8.80 1.00 -2 6 16 9.03 1.00 -11 7 16 23.39 1.23 -10 7 16 3.92 0.63 -9 -7 16 9.22 0.86 -9 7 16 9.24 0.82 -8 -7 16 47.03 1.71 -8 7 16 40.82 1.61 -7 -7 16 6.41 0.78 -7 7 16 6.09 0.70 -6 -7 16 14.44 1.12 -5 -7 16 24.64 1.36 -5 7 16 26.43 1.42 -4 -7 16 2.93 0.68 -4 7 16 2.83 0.66 -3 -7 16 29.52 1.57 -3 7 16 29.22 1.56 -2 -7 16 17.83 1.38 -2 7 16 21.02 1.39 -11 8 16 -0.05 0.43 -10 8 16 4.89 0.70 -9 8 16 8.77 0.86 -8 -8 16 0.16 0.47 -8 8 16 0.29 0.43 -7 -8 16 14.71 1.07 -7 8 16 13.73 0.99 -6 -8 16 1.14 0.58 -6 8 16 1.15 0.49 -5 -8 16 1.15 0.57 -5 8 16 0.37 0.51 -4 -8 16 8.92 0.93 -4 8 16 7.48 0.92 -3 -8 16 0.21 0.60 -3 8 16 -0.11 0.57 -10 9 16 0.80 0.46 -9 9 16 5.91 0.74 -8 9 16 2.15 0.56 -7 -9 16 0.01 0.46 -7 9 16 -0.21 0.40 -6 -9 16 3.68 0.68 -6 9 16 4.76 0.67 -5 -9 16 9.16 0.96 -5 9 16 8.22 0.92 -4 -9 16 0.64 0.58 -4 9 16 -0.50 0.50 -3 -9 16 0.97 0.61 -3 9 16 -0.48 0.53 -10 10 16 32.35 1.47 -9 10 16 30.88 1.41 -8 10 16 0.58 0.48 -7 10 16 15.12 1.05 -6 -10 16 6.42 0.80 -6 10 16 7.32 0.80 -5 -10 16 14.14 1.13 -5 10 16 15.02 1.17 -5 10 16 13.08 1.04 -4 -10 16 20.29 1.31 -4 10 16 20.12 1.32 -9 11 16 14.41 1.06 -8 11 16 13.60 1.05 -7 11 16 1.69 0.55 -6 11 16 9.04 0.90 -5 -11 16 20.00 1.28 -5 11 16 20.76 1.20 -5 11 16 20.14 1.30 -8 12 16 0.01 0.47 -7 12 16 1.49 0.53 -6 12 16 0.25 0.48 -8 0 17 -0.23 0.48 -7 0 17 -0.38 0.49 -6 0 17 0.00 0.54 -5 0 17 0.15 0.57 -9 -1 17 17.00 1.20 -8 -1 17 9.08 0.97 -8 1 17 8.87 0.94 -7 -1 17 4.62 0.77 -7 1 17 6.04 0.83 -6 -1 17 36.24 1.69 -6 1 17 36.32 1.69 -5 -1 17 9.89 1.05 -5 1 17 9.49 1.03 -9 -2 17 2.88 0.68 -8 -2 17 13.83 1.13 -8 2 17 15.83 1.18 -7 -2 17 27.20 1.44 -7 2 17 24.87 1.45 -6 -2 17 0.32 0.56 -6 2 17 0.37 0.57 -5 -2 17 25.25 1.50 -5 2 17 26.58 1.53 -10 3 17 -0.03 0.43 -9 -3 17 0.99 0.57 -8 -3 17 0.92 0.58 -7 -3 17 2.23 0.63 -7 3 17 1.83 0.64 -6 -3 17 9.00 0.96 -6 3 17 8.39 0.95 -5 -3 17 2.46 0.72 -5 3 17 2.51 0.71 -8 -4 17 6.69 0.84 -7 -4 17 3.54 0.73 -7 4 17 4.56 0.76 -6 -4 17 -0.30 0.52 -6 4 17 0.86 0.58 -5 -4 17 4.41 0.82 -5 4 17 6.13 0.86 -9 -5 17 31.05 1.49 -9 5 17 30.61 1.39 -7 -5 17 1.28 0.60 -7 5 17 2.60 0.68 -6 -5 17 28.73 1.52 -6 5 17 29.62 1.57 -8 -6 17 5.78 0.82 -7 6 17 12.15 1.09 -6 -6 17 0.31 0.56 -6 6 17 -0.07 0.52 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 81181 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_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.0484(3) 1.05292(15) -0.2564(3) 0.0264(8) Uani 1 1 d . . . . . Ir1 Ir 0.18199(2) 1.10475(2) -0.14153(2) 0.01865(7) Uani 1 1 d . . . . . S1 S -0.05798(12) 1.15371(6) 0.00586(12) 0.0283(3) Uani 1 1 d . . . . . S2 S 0.43003(12) 1.24769(6) -0.02852(11) 0.0276(3) Uani 1 1 d . . . . . Cl3S Cl 0.2092(4) 1.14078(16) 0.3227(3) 0.1183(11) Uani 1 1 d . U . . . Cl4S Cl 0.3646(4) 1.04835(19) 0.4365(5) 0.1438(16) Uani 1 1 d . U . . . N1 N 0.1780(4) 1.05480(17) -0.0183(4) 0.0223(9) Uani 1 1 d . . . . . N2 N 0.1819(4) 1.15686(17) -0.2629(3) 0.0201(8) Uani 1 1 d . . . . . N3 N 0.3036(4) 1.05530(19) -0.1713(4) 0.0253(9) Uani 1 1 d . U . . . C1 C -0.0431(6) 0.9750(3) -0.3673(6) 0.0457(16) Uani 1 1 d . . . . . H1A H -0.0263 0.9352 -0.3613 0.069 Uiso 1 1 calc R U . . . H1B H -0.0698 0.9868 -0.4450 0.069 Uiso 1 1 calc R U . . . H1C H -0.1033 0.9824 -0.3434 0.069 Uiso 1 1 calc R U . . . C2 C 0.0649(6) 1.0066(3) -0.2937(5) 0.0355(13) Uani 1 1 d . . . . . C2S C 0.3074(14) 1.1077(6) 0.4436(14) 0.123(5) Uani 1 1 d . U . . . H2S1 H 0.3718 1.1339 0.4829 0.147 Uiso 1 1 calc R U . . . H2S2 H 0.2685 1.1023 0.4922 0.147 Uiso 1 1 calc R U . . . C3 C 0.1699(6) 0.9838(3) -0.2762(6) 0.0487(18) Uani 1 1 d . . . . . H3 H 0.1679 0.9465 -0.2994 0.058 Uiso 1 1 calc R U . . . C4 C 0.2799(6) 1.0093(3) -0.2281(5) 0.0409(15) Uani 1 1 d . . . . . C5 C 0.3713(7) 0.9788(3) -0.2490(7) 0.056(2) Uani 1 1 d . . . . . H5A H 0.3619 0.9872 -0.3243 0.084 Uiso 1 1 calc R U . . . H5B H 0.3629 0.9388 -0.2421 0.084 Uiso 1 1 calc R U . . . H5C H 0.4480 0.9906 -0.1941 0.084 Uiso 1 1 calc R U . . . C11 C 0.0420(4) 1.1206(2) -0.0280(4) 0.0224(10) Uani 1 1 d . . . . . C12 C 0.2403(5) 1.0083(2) 0.0223(5) 0.0289(11) Uani 1 1 d . . . . . H12 H 0.2924 0.9969 -0.0063 0.035 Uiso 1 1 calc R U . . . C13 C 0.2307(6) 0.9765(2) 0.1045(5) 0.0352(13) Uani 1 1 d . . . . . H13 H 0.2763 0.9442 0.1323 0.042 Uiso 1 1 calc R U . . . C14 C 0.1540(6) 0.9925(2) 0.1454(5) 0.0353(13) Uani 1 1 d . . . . . H14 H 0.1461 0.9712 0.2013 0.042 Uiso 1 1 calc R U . . . C15 C 0.0890(5) 1.0398(2) 0.1042(5) 0.0303(12) Uani 1 1 d . . . . . H15 H 0.0357 1.0512 0.1314 0.036 Uiso 1 1 calc R U . . . C16 C 0.1019(4) 1.0708(2) 0.0225(4) 0.0224(10) Uani 1 1 d . . . . . C20 C 0.0648(4) 1.1463(2) -0.1085(4) 0.0198(9) Uani 1 1 d . . . . . C21 C -0.0032(4) 1.1969(2) -0.1444(4) 0.0209(10) Uani 1 1 d . . . . . C22 C -0.0738(4) 1.2056(2) -0.0896(4) 0.0248(11) Uani 1 1 d . . . . . C23 C -0.1483(5) 1.2512(2) -0.1138(5) 0.0312(12) Uani 1 1 d . . . . . H23 H -0.1959 1.2558 -0.0769 0.037 Uiso 1 1 calc R U . . . C24 C -0.1512(5) 1.2889(3) -0.1913(5) 0.0330(13) Uani 1 1 d . . . . . H24 H -0.2015 1.3199 -0.2086 0.040 Uiso 1 1 calc R U . . . C25 C -0.0805(5) 1.2823(2) -0.2454(5) 0.0301(12) Uani 1 1 d . . . . . H25 H -0.0829 1.3090 -0.2986 0.036 Uiso 1 1 calc R U . . . C26 C -0.0072(5) 1.2372(2) -0.2224(5) 0.0269(11) Uani 1 1 d . . . . . H26 H 0.0405 1.2335 -0.2594 0.032 Uiso 1 1 calc R U . . . C31 C 0.3194(4) 1.2014(2) -0.1058(4) 0.0218(10) Uani 1 1 d . . . . . C32 C 0.1186(4) 1.1490(2) -0.3728(4) 0.0255(11) Uani 1 1 d . . . . . H32 H 0.0685 1.1179 -0.3975 0.031 Uiso 1 1 calc R U . . . C33 C 0.1239(5) 1.1844(3) -0.4507(4) 0.0300(12) Uani 1 1 d . . . . . H33 H 0.0775 1.1781 -0.5281 0.036 Uiso 1 1 calc R U . . . C34 C 0.1983(5) 1.2296(3) -0.4149(5) 0.0326(12) Uani 1 1 d . . . . . H34 H 0.2033 1.2546 -0.4675 0.039 Uiso 1 1 calc R U . . . C35 C 0.2649(4) 1.2377(2) -0.3016(5) 0.0260(11) Uani 1 1 d . . . . . H35 H 0.3161 1.2683 -0.2758 0.031 Uiso 1 1 calc R U . . . C36 C 0.2564(4) 1.2008(2) -0.2257(4) 0.0211(10) Uani 1 1 d . . . . . C40 C 0.3007(4) 1.1598(2) -0.0461(4) 0.0189(9) Uani 1 1 d . . . . . C41 C 0.3791(4) 1.1657(2) 0.0715(4) 0.0214(10) Uani 1 1 d . . . . . C42 C 0.4556(4) 1.2113(2) 0.0921(4) 0.0240(10) Uani 1 1 d . . . . . C43 C 0.5410(5) 1.2235(2) 0.1986(5) 0.0303(12) Uani 1 1 d . . . . . H43 H 0.5914 1.2540 0.2106 0.036 Uiso 1 1 calc R U . . . C44 C 0.5508(5) 1.1900(2) 0.2867(5) 0.0292(12) Uani 1 1 d . . . . . H44 H 0.6086 1.1977 0.3599 0.035 Uiso 1 1 calc R U . . . C45 C 0.4766(5) 1.1450(2) 0.2689(4) 0.0273(11) Uani 1 1 d . . . . . H45 H 0.4841 1.1226 0.3302 0.033 Uiso 1 1 calc R U . . . C46 C 0.3922(5) 1.1329(2) 0.1628(4) 0.0244(10) Uani 1 1 d . . . . . H46 H 0.3428 1.1020 0.1518 0.029 Uiso 1 1 calc R U . . . C51 C 0.4126(5) 1.0807(2) -0.1443(5) 0.0351(12) Uani 1 1 d D U . . . C52 C 0.4198(11) 1.1034(5) -0.2385(9) 0.036(3) Uani 0.65(2) 1 d D U P A 1 H52 H 0.3600 1.0976 -0.3116 0.043 Uiso 0.65(2) 1 calc R U P A 1 C53 C 0.5178(10) 1.1347(5) -0.2210(12) 0.041(3) Uani 0.65(2) 1 d D U P A 1 H53 H 0.5248 1.1513 -0.2822 0.050 Uiso 0.65(2) 1 calc R U P A 1 C54 C 0.6054(10) 1.1411(5) -0.1121(13) 0.047(4) Uani 0.65(2) 1 d D U P A 1 H54 H 0.6707 1.1632 -0.0997 0.056 Uiso 0.65(2) 1 calc R U P A 1 C55 C 0.5985(9) 1.1159(5) -0.0219(12) 0.042(3) Uani 0.65(2) 1 d D U P A 1 H55 H 0.6606 1.1193 0.0505 0.051 Uiso 0.65(2) 1 calc R U P A 1 C56 C 0.5009(18) 1.0854(14) -0.0369(12) 0.039(3) Uani 0.65(2) 1 d D U P A 1 H56 H 0.4952 1.0684 0.0245 0.047 Uiso 0.65(2) 1 calc R U P A 1 C52A C 0.488(3) 1.076(3) -0.0288(16) 0.038(5) Uani 0.35(2) 1 d D U P A 2 H52A H 0.4659 1.0537 0.0163 0.045 Uiso 0.35(2) 1 calc R U P A 2 C53A C 0.5944(16) 1.1044(10) 0.0224(19) 0.041(4) Uani 0.35(2) 1 d D U P A 2 H53A H 0.6423 1.0998 0.1000 0.049 Uiso 0.35(2) 1 calc R U P A 2 C54A C 0.6290(18) 1.1386(9) -0.041(3) 0.049(5) Uani 0.35(2) 1 d D U P A 2 H54A H 0.6994 1.1586 -0.0074 0.059 Uiso 0.35(2) 1 calc R U P A 2 C55A C 0.557(2) 1.1427(11) -0.156(3) 0.053(5) Uani 0.35(2) 1 d D U P A 2 H55A H 0.5817 1.1637 -0.2012 0.063 Uiso 0.35(2) 1 calc R U P A 2 C56A C 0.449(2) 1.1167(11) -0.205(2) 0.047(5) Uani 0.35(2) 1 d D U P A 2 H56A H 0.3999 1.1235 -0.2816 0.057 Uiso 0.35(2) 1 calc R U P A 2 C1S C -0.1712(16) 1.1345(12) -0.3825(17) 0.037(4) Uani 0.51(2) 1 d D U P B 1 H1S1 H -0.1463 1.1725 -0.3895 0.045 Uiso 0.51(2) 1 calc R U P B 1 H1S2 H -0.1044 1.1151 -0.3239 0.045 Uiso 0.51(2) 1 calc R U P B 1 Cl1S Cl -0.2814(6) 1.1380(4) -0.3429(7) 0.083(3) Uani 0.51(2) 1 d D U P B 1 Cl2S Cl -0.2127(9) 1.1002(3) -0.5077(7) 0.0515(19) Uani 0.51(2) 1 d D U P B 1 Cl1A Cl -0.3135(17) 1.1185(9) -0.3589(15) 0.141(6) Uani 0.49(2) 1 d D U P B 2 C1SA C -0.191(2) 1.1277(18) -0.3764(17) 0.071(7) Uani 0.49(2) 1 d D U P B 2 H1S3 H -0.1662 1.1667 -0.3581 0.085 Uiso 0.49(2) 1 calc R U P B 2 H1S4 H -0.1299 1.1041 -0.3216 0.085 Uiso 0.49(2) 1 calc R U P B 2 Cl2A Cl -0.2020(10) 1.1135(8) -0.5058(9) 0.088(4) Uani 0.49(2) 1 d D U P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0260(19) 0.0262(19) 0.0263(19) -0.0048(15) 0.0110(16) -0.0031(15) Ir1 0.01851(10) 0.01903(11) 0.01937(11) -0.00039(7) 0.00926(8) 0.00063(7) S1 0.0294(7) 0.0311(7) 0.0330(7) 0.0027(5) 0.0218(6) 0.0025(5) S2 0.0239(6) 0.0304(7) 0.0263(6) 0.0008(5) 0.0091(5) -0.0070(5) Cl3S 0.130(3) 0.104(3) 0.123(3) -0.006(2) 0.058(2) -0.018(2) Cl4S 0.126(3) 0.116(3) 0.194(5) 0.019(3) 0.075(3) -0.005(2) N1 0.023(2) 0.021(2) 0.022(2) -0.0012(16) 0.0087(17) -0.0010(17) N2 0.019(2) 0.023(2) 0.019(2) 0.0013(16) 0.0096(17) 0.0021(16) N3 0.027(2) 0.028(2) 0.023(2) 0.0023(18) 0.0132(18) 0.0092(18) C1 0.047(4) 0.041(4) 0.046(4) -0.016(3) 0.018(3) -0.012(3) C2 0.040(3) 0.032(3) 0.032(3) -0.006(2) 0.014(3) -0.002(3) C2S 0.122(12) 0.102(9) 0.142(12) 0.045(9) 0.058(9) 0.009(8) C3 0.050(4) 0.038(4) 0.052(4) -0.019(3) 0.017(3) 0.005(3) C4 0.042(4) 0.043(4) 0.033(3) -0.007(3) 0.013(3) 0.009(3) C5 0.052(4) 0.058(5) 0.054(4) -0.021(4) 0.019(4) 0.018(4) C11 0.020(2) 0.023(2) 0.025(2) -0.002(2) 0.011(2) -0.0033(19) C12 0.030(3) 0.024(3) 0.032(3) 0.000(2) 0.013(2) 0.001(2) C13 0.047(4) 0.022(3) 0.034(3) 0.005(2) 0.015(3) 0.005(2) C14 0.054(4) 0.024(3) 0.030(3) 0.004(2) 0.020(3) -0.005(3) C15 0.038(3) 0.029(3) 0.027(3) 0.000(2) 0.016(2) -0.002(2) C16 0.023(2) 0.021(2) 0.023(2) -0.0013(19) 0.011(2) -0.0031(19) C20 0.015(2) 0.024(2) 0.019(2) -0.0016(19) 0.0065(18) -0.0012(18) C21 0.016(2) 0.024(2) 0.023(2) -0.0008(19) 0.0088(19) 0.0000(18) C22 0.020(2) 0.029(3) 0.027(3) -0.002(2) 0.011(2) -0.003(2) C23 0.025(3) 0.035(3) 0.041(3) -0.002(2) 0.020(2) 0.003(2) C24 0.023(3) 0.034(3) 0.041(3) 0.002(2) 0.013(2) 0.008(2) C25 0.027(3) 0.030(3) 0.032(3) 0.007(2) 0.013(2) 0.004(2) C26 0.025(3) 0.030(3) 0.027(3) 0.003(2) 0.013(2) 0.003(2) C31 0.018(2) 0.022(2) 0.024(2) -0.0007(19) 0.008(2) -0.0007(18) C32 0.018(2) 0.034(3) 0.023(2) -0.001(2) 0.008(2) -0.001(2) C33 0.024(3) 0.041(3) 0.021(2) 0.005(2) 0.006(2) -0.001(2) C34 0.027(3) 0.041(3) 0.028(3) 0.008(2) 0.011(2) 0.000(2) C35 0.019(2) 0.030(3) 0.030(3) 0.005(2) 0.011(2) 0.000(2) C36 0.016(2) 0.023(2) 0.025(2) 0.0014(19) 0.010(2) 0.0019(18) C40 0.014(2) 0.023(2) 0.023(2) -0.0018(19) 0.0110(19) 0.0016(18) C41 0.019(2) 0.024(2) 0.023(2) -0.0019(19) 0.010(2) 0.0023(19) C42 0.019(2) 0.026(3) 0.026(3) 0.001(2) 0.010(2) 0.001(2) C43 0.023(3) 0.033(3) 0.031(3) -0.006(2) 0.009(2) -0.003(2) C44 0.018(2) 0.040(3) 0.023(3) -0.003(2) 0.004(2) 0.000(2) C45 0.022(3) 0.035(3) 0.022(2) 0.004(2) 0.007(2) 0.008(2) C46 0.022(3) 0.026(3) 0.024(2) 0.002(2) 0.010(2) 0.003(2) C51 0.032(3) 0.028(3) 0.055(3) 0.002(3) 0.028(3) 0.009(2) C52 0.034(6) 0.025(6) 0.060(6) -0.006(5) 0.031(5) -0.004(4) C53 0.028(6) 0.038(5) 0.070(7) 0.006(5) 0.034(6) 0.003(4) C54 0.025(6) 0.040(6) 0.079(10) 0.000(7) 0.025(6) -0.002(5) C55 0.030(5) 0.034(7) 0.069(7) -0.003(6) 0.028(5) 0.002(4) C56 0.021(6) 0.034(12) 0.062(6) -0.009(5) 0.018(4) 0.003(4) C52A 0.024(10) 0.023(14) 0.064(8) -0.017(9) 0.019(7) -0.007(7) C53A 0.034(8) 0.028(10) 0.079(10) -0.007(9) 0.040(8) -0.008(7) C54A 0.041(10) 0.040(11) 0.083(12) 0.009(11) 0.042(9) 0.004(8) C55A 0.037(11) 0.045(10) 0.086(12) 0.011(11) 0.036(10) 0.002(9) C56A 0.039(10) 0.026(11) 0.089(11) 0.011(10) 0.040(8) 0.005(7) C1S 0.038(7) 0.038(9) 0.034(7) -0.018(7) 0.015(6) -0.006(6) Cl1S 0.049(3) 0.109(5) 0.103(5) -0.062(5) 0.044(3) -0.016(3) Cl2S 0.072(4) 0.049(3) 0.023(2) -0.015(2) 0.012(2) -0.016(2) Cl1A 0.141(10) 0.176(11) 0.154(9) 0.118(8) 0.111(8) 0.095(8) C1SA 0.068(12) 0.080(17) 0.041(9) 0.014(10) 0.001(9) 0.012(13) Cl2A 0.057(5) 0.153(10) 0.049(4) 0.042(5) 0.020(4) 0.035(5) 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' S S 0.1246 0.1234 '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' Cl Cl 0.1484 0.1585 '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 O1 Ir1 124.8(4) C40 Ir1 C20 88.22(19) C40 Ir1 N2 80.09(18) C20 Ir1 N2 97.40(18) C40 Ir1 N1 99.40(18) C20 Ir1 N1 80.23(19) N2 Ir1 N1 177.60(16) C40 Ir1 O1 173.85(17) C20 Ir1 O1 90.09(17) N2 Ir1 O1 94.26(15) N1 Ir1 O1 86.14(16) C40 Ir1 N3 93.99(18) C20 Ir1 N3 175.75(18) N2 Ir1 N3 86.57(17) N1 Ir1 N3 95.81(17) O1 Ir1 N3 88.08(16) C22 S1 C11 90.1(3) C42 S2 C31 89.7(2) C12 N1 C16 118.7(5) C12 N1 Ir1 126.0(4) C16 N1 Ir1 115.3(3) C32 N2 C36 119.8(4) C32 N2 Ir1 124.4(4) C36 N2 Ir1 115.7(3) C4 N3 C51 117.7(5) C4 N3 Ir1 125.4(4) C51 N3 Ir1 115.8(3) O1 C2 C3 126.9(6) O1 C2 C1 115.4(6) C3 C2 C1 117.6(6) Cl4S C2S Cl3S 120.7(11) C2 C3 C4 128.0(6) N3 C4 C3 124.4(6) N3 C4 C5 121.3(6) C3 C4 C5 114.3(6) C20 C11 C16 119.2(5) C20 C11 S1 115.7(4) C16 C11 S1 125.1(4) N1 C12 C13 122.1(5) C14 C13 C12 119.2(5) C15 C14 C13 119.4(5) C14 C15 C16 119.6(5) N1 C16 C15 121.0(5) N1 C16 C11 112.6(4) C15 C16 C11 126.5(5) C11 C20 C21 109.1(4) C11 C20 Ir1 112.7(4) C21 C20 Ir1 138.2(4) C26 C21 C22 117.2(5) C26 C21 C20 130.0(5) C22 C21 C20 112.8(4) C23 C22 C21 122.0(5) C23 C22 S1 125.7(4) C21 C22 S1 112.3(4) C24 C23 C22 119.0(5) C23 C24 C25 120.4(5) C26 C25 C24 120.9(5) C25 C26 C21 120.3(5) C40 C31 C36 118.7(5) C40 C31 S2 115.8(4) C36 C31 S2 125.2(4) N2 C32 C33 122.0(5) C32 C33 C34 119.1(5) C35 C34 C33 119.2(5) C34 C35 C36 119.7(5) N2 C36 C35 120.1(5) N2 C36 C31 111.9(4) C35 C36 C31 128.0(5) C31 C40 C41 109.8(4) C31 C40 Ir1 113.6(4) C41 C40 Ir1 136.5(4) C46 C41 C42 117.6(5) C46 C41 C40 130.1(5) C42 C41 C40 112.2(4) C43 C42 C41 122.1(5) C43 C42 S2 125.5(4) C41 C42 S2 112.4(4) C44 C43 C42 118.4(5) C43 C44 C45 120.7(5) C46 C45 C44 120.6(5) C45 C46 C41 120.6(5) C56 C51 C52 122.8(8) C56A C51 C52A 115.2(12) C56 C51 N3 124.4(8) C56A C51 N3 131.8(11) C52 C51 N3 112.8(6) C52A C51 N3 111.8(10) C53 C52 C51 118.1(9) C54 C53 C52 119.2(9) C55 C54 C53 121.3(9) C54 C55 C56 120.5(10) C51 C56 C55 118.0(10) C53A C52A C51 123.3(15) C54A C53A C52A 119.8(15) C53A C54A C55A 118.0(14) C56A C55A C54A 121.8(15) C55A C56A C51 121.7(14) Cl2S C1S Cl1S 112.0(9) Cl2A C1SA Cl1A 116.5(13) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C2 1.281(7) O1 Ir1 2.136(4) Ir1 C40 2.005(5) Ir1 C20 2.021(5) Ir1 N2 2.052(4) Ir1 N1 2.061(4) Ir1 N3 2.147(4) S1 C22 1.735(6) S1 C11 1.742(5) S2 C42 1.735(5) S2 C31 1.748(5) Cl3S C2S 1.746(15) Cl4S C2S 1.635(15) N1 C12 1.349(7) N1 C16 1.373(7) N2 C32 1.342(7) N2 C36 1.370(6) N3 C4 1.304(8) N3 C51 1.430(7) C1 C2 1.512(9) C2 C3 1.386(10) C3 C4 1.416(10) C4 C5 1.520(9) C11 C20 1.382(7) C11 C16 1.429(7) C12 C13 1.390(8) C13 C14 1.382(9) C14 C15 1.381(8) C15 C16 1.393(7) C20 C21 1.458(7) C21 C26 1.411(7) C21 C22 1.416(7) C22 C23 1.404(8) C23 C24 1.366(8) C24 C25 1.404(8) C25 C26 1.385(8) C31 C40 1.369(7) C31 C36 1.441(7) C32 C33 1.373(8) C33 C34 1.393(8) C34 C35 1.385(8) C35 C36 1.390(7) C40 C41 1.453(7) C41 C46 1.401(7) C41 C42 1.423(7) C42 C43 1.394(8) C43 C44 1.387(8) C44 C45 1.399(8) C45 C46 1.385(7) C51 C56 1.388(11) C51 C56A 1.408(13) C51 C52 1.413(10) C51 C52A 1.419(13) C52 C53 1.404(10) C53 C54 1.403(11) C54 C55 1.388(11) C55 C56 1.396(11) C52A C53A 1.405(13) C53A C54A 1.392(13) C54A C55A 1.404(14) C55A C56A 1.395(14) C1S Cl2S 1.725(11) C1S Cl1S 1.728(12) Cl1A C1SA 1.711(14) C1SA Cl2A 1.707(13)