# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_cmpnd_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C23 H30 Cl N3 Rh), C4 H10 O, 2(F6 Sb)' _chemical_formula_sum 'C50 H70 Cl2 F12 N6 O Rh2 Sb2' _chemical_formula_weight 1519.34 _chemical_absolute_configuration rmad 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' F F 0.0171 0.0103 '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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21 _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.8002(5) _cell_length_b 28.1813(15) _cell_length_c 12.2161(7) _cell_angle_alpha 90.00 _cell_angle_beta 97.6030(10) _cell_angle_gamma 90.00 _cell_volume 3003.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11669 _cell_measurement_theta_min 2.217 _cell_measurement_theta_max 28.208 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.379 _exptl_crystal_size_mid 0.099 _exptl_crystal_size_min 0.094 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.680 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1508 _exptl_absorpt_coefficient_mu 1.596 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.471 _exptl_absorpt_correction_T_max 0.799 _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS within SAINT+ package, v. 6.45. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX DUO system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 32158 _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_sigmaI/netI 0.0657 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 29.50 _reflns_number_total 14491 _reflns_number_gt 12308 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_cell_refinement 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_data_reduction 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP program, SHELXTL v6.12, Bruker2000' _computing_publication_material ENCIFER _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Asymmetric untit is composed by two independent Rh-complexes molecules with different metal configuration and a diethylether solvent molecule. Most of the hydrogen atoms of methyl and phenyl groups have been included in the model in calculated positions and refined with a riding model. Hydrogen atoms bonded to chiral carbon atoms (C16 and C46) have been included in observed positions and refined with an isotropic thermal parameter equal to 1.2 times those of the carbon atoms they are bounded to. A geometrical restrain has been included in C16-H16 distance. Diethylether solvent molecule has been found to be disordered. Atoms have been included in two sets of positions with complementary occupancy factors (0.627/0.373(9)). Geometrical restraints in C-O and C-C bond lengths have been included in the refinement. A common isotropic thermal parameter has been defined for all the carbon atoms. Equivalent thermal parameters of four fluorine atoms of both counterions have been found to be too large. Therefore, fluorine atoms have been modelled in two sets of positions. Geometrical restraints in Sb-F bond length have been used. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+6.1480P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(3) _refine_ls_number_reflns 14491 _refine_ls_number_parameters 679 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0614 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1179 _refine_ls_wR_factor_gt 0.1113 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.036 _refine_ls_shift/su_mean 0.001 _iucr_refine_instructions_details ; TITL fjl202ds in P2(1) CELL 0.71073 8.8002 28.1813 12.2161 90.000 97.603 90.000 ZERR 2.00 0.0005 0.0015 0.0007 0.000 0.001 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N F CL RH SB O UNIT 100 140 12 24 4 4 4 2 MERG 2 OMIT 0 -2 0 DFIX 0.96 0.02 C16 H16 dfix 41.00 0.01 O1A C60A O1A C62A O1B C60B O1B C62B dfix 51.00 0.01 C62A C63 C62B C63 C60A C61A C60B C61B dfix 61.0 0.01 SB1 F3A SB1 F3B SB1 F4A SB1 F4B dfix 61.0 0.01 SB1 F5A SB1 F5B SB1 F6A SB1 F6B dfix 61.0 0.01 SB2 F9A SB2 F9B SB2 F10A SB2 F10B dfix 61.0 0.01 SB2 F11A SB2 F11B SB2 F12A SB2 F12B FMAP 2 PLAN 20 ACTA 55.00 BOND $H CONF L.S. 6 TEMP -173.00 WGHT 0.039900 6.148000 FVAR 0.22459 0.62697 0.06284 1.32153 1.65409 1.87790 0.60983 FVAR 0.52471 MOLE 1 RH1 6 0.041889 0.430137 0.061562 11.00000 0.02061 0.02273 = 0.03058 -0.00433 0.00192 -0.00072 CL1 5 0.291078 0.450089 0.019074 11.00000 0.02754 0.04129 = 0.04894 -0.01903 0.01555 -0.00985 N1 3 0.052445 0.487665 0.171373 11.00000 0.01927 0.03154 = 0.03404 0.00237 0.00418 0.00255 N2 3 0.167957 0.402008 0.207408 11.00000 0.02811 0.02683 = 0.03221 0.00409 0.00111 -0.00339 N3 3 0.137743 0.515842 0.336829 11.00000 0.04232 0.02850 = 0.03523 -0.01188 0.00656 -0.01182 C1 1 -0.060422 0.369233 -0.027582 11.00000 0.04384 0.03488 = 0.04221 -0.00821 -0.01040 -0.00596 C2 1 -0.164883 0.388694 0.042060 11.00000 0.02891 0.05625 = 0.04375 -0.00064 -0.00431 -0.02075 C3 1 -0.199424 0.436644 0.006544 11.00000 0.01568 0.05114 = 0.04817 -0.01290 -0.00104 -0.00221 C4 1 -0.111529 0.447761 -0.083369 11.00000 0.02311 0.03695 = 0.03855 -0.00612 0.00310 0.00268 C5 1 -0.031385 0.404088 -0.105365 11.00000 0.02539 0.04010 = 0.02570 -0.01098 -0.00202 -0.00512 C6 1 0.001167 0.319205 -0.023995 11.00000 0.11947 0.03282 = 0.08886 -0.02333 -0.05818 0.00032 AFIX 137 H6A 2 -0.050950 0.301145 -0.086539 11.00000 -1.50000 H6B 2 -0.017085 0.304037 0.045267 11.00000 -1.50000 H6C 2 0.111532 0.319943 -0.028385 11.00000 -1.50000 AFIX 0 C7 1 -0.229266 0.362148 0.131405 11.00000 0.05175 0.09625 = 0.05930 0.01760 -0.00622 -0.04287 AFIX 137 H7A 2 -0.266127 0.384735 0.182917 11.00000 -1.50000 H7B 2 -0.149243 0.342104 0.171165 11.00000 -1.50000 H7C 2 -0.314627 0.342205 0.098693 11.00000 -1.50000 AFIX 0 C8 1 -0.305755 0.469198 0.053089 11.00000 0.02494 0.10418 = 0.05324 -0.02116 0.00820 0.00709 AFIX 137 H8A 2 -0.410145 0.464099 0.015914 11.00000 -1.50000 H8B 2 -0.275014 0.502084 0.041943 11.00000 -1.50000 H8C 2 -0.302660 0.463010 0.132295 11.00000 -1.50000 AFIX 0 C9 1 -0.113153 0.491795 -0.147975 11.00000 0.05998 0.04082 = 0.05016 0.01133 -0.01178 -0.00540 AFIX 137 H9A 2 -0.009819 0.498264 -0.165850 11.00000 -1.50000 H9B 2 -0.146666 0.518181 -0.104717 11.00000 -1.50000 H9C 2 -0.184057 0.488303 -0.216437 11.00000 -1.50000 AFIX 0 C10 1 0.066448 0.399829 -0.197161 11.00000 0.04674 0.09589 = 0.03807 -0.02271 -0.00175 0.01242 AFIX 137 H10A 2 0.152705 0.378482 -0.174211 11.00000 -1.50000 H10B 2 0.105556 0.431213 -0.213781 11.00000 -1.50000 H10C 2 0.004738 0.387021 -0.263217 11.00000 -1.50000 AFIX 0 C11 1 0.007343 0.533409 0.176142 11.00000 0.02973 0.02126 = 0.04387 -0.00225 0.01379 -0.00168 AFIX 43 H11 2 -0.050817 0.550606 0.118167 11.00000 -1.20000 AFIX 0 C12 1 0.060636 0.550864 0.280230 11.00000 0.03595 0.02444 = 0.04759 -0.01135 0.01548 -0.00365 AFIX 43 H12 2 0.045222 0.581988 0.306535 11.00000 -1.20000 AFIX 0 C13 1 0.203471 0.517867 0.453182 11.00000 0.06759 0.04568 = 0.03759 -0.00740 0.00239 -0.01777 AFIX 137 H13A 2 0.242310 0.549918 0.471016 11.00000 -1.50000 H13B 2 0.287825 0.495029 0.466871 11.00000 -1.50000 H13C 2 0.124304 0.510011 0.499596 11.00000 -1.50000 AFIX 0 C14 1 0.130363 0.477310 0.270061 11.00000 0.02418 0.02673 = 0.03036 -0.00437 0.00208 -0.00417 C15 1 0.199029 0.431663 0.288045 11.00000 0.02644 0.02866 = 0.03397 0.00347 -0.00305 0.00127 AFIX 43 H15 2 0.262871 0.423631 0.354348 11.00000 -1.20000 AFIX 0 C16 1 0.242599 0.354989 0.213908 11.00000 0.02288 0.02999 = 0.04297 0.00535 0.00346 0.00723 AFIX 2 H16 2 0.223024 0.354103 0.135859 11.00000 -1.20000 AFIX 0 C17 1 0.413815 0.357905 0.265974 11.00000 0.02782 0.02925 = 0.09834 0.01788 0.00370 0.00461 AFIX 137 H17A 2 0.469242 0.379337 0.222014 11.00000 -1.50000 H17B 2 0.459898 0.326224 0.266999 11.00000 -1.50000 H17C 2 0.419989 0.369989 0.341656 11.00000 -1.50000 AFIX 0 C18 1 0.155076 0.319189 0.272310 11.00000 0.02440 0.02533 = 0.04205 0.00203 -0.00285 0.00099 C19 1 0.063726 0.329960 0.352076 11.00000 0.04247 0.03402 = 0.04255 0.00287 0.01057 0.00348 AFIX 43 H19 2 0.050370 0.362146 0.371863 11.00000 -1.20000 AFIX 0 C20 1 -0.008858 0.294463 0.403761 11.00000 0.03315 0.04728 = 0.04951 0.00898 0.00947 0.00037 AFIX 43 H20 2 -0.069062 0.302820 0.459893 11.00000 -1.20000 AFIX 0 C21 1 0.003485 0.247887 0.376515 11.00000 0.04462 0.04066 = 0.06510 0.02211 -0.00622 -0.00359 AFIX 43 H21 2 -0.048611 0.224029 0.411980 11.00000 -1.20000 AFIX 0 C22 1 0.093422 0.236166 0.296200 11.00000 0.04558 0.02769 = 0.05511 0.00518 -0.00458 -0.00094 AFIX 43 H22 2 0.103798 0.203794 0.276800 11.00000 -1.20000 AFIX 0 C23 1 0.169428 0.270949 0.242924 11.00000 0.03459 0.02433 = 0.04733 -0.00002 -0.00144 0.00568 AFIX 43 H23 2 0.230312 0.262335 0.187385 11.00000 -1.20000 AFIX 0 RH31 6 0.457490 0.672627 0.412801 11.00000 0.01847 0.03074 = 0.03367 -0.00610 0.00353 -0.00191 CL31 5 0.216154 0.648195 0.464828 11.00000 0.02545 0.04015 = 0.04033 -0.00832 0.01066 -0.00633 N31 3 0.448161 0.613729 0.308183 11.00000 0.02909 0.02196 = 0.03270 -0.00537 0.00619 -0.00146 N32 3 0.324316 0.698126 0.259107 11.00000 0.02279 0.02350 = 0.03326 0.00111 0.00083 -0.00115 N33 3 0.366658 0.581441 0.146524 11.00000 0.03755 0.02899 = 0.03988 -0.00283 0.01439 -0.00465 C31 1 0.606488 0.659289 0.560613 11.00000 0.02658 0.04593 = 0.04327 -0.00445 -0.00814 -0.00626 C32 1 0.696321 0.663075 0.471629 11.00000 0.01925 0.05070 = 0.05262 -0.01195 -0.00364 -0.00240 C33 1 0.672916 0.709449 0.428106 11.00000 0.02713 0.05421 = 0.04291 -0.01075 -0.00743 -0.01347 C34 1 0.574704 0.734353 0.493542 11.00000 0.03478 0.03933 = 0.04124 -0.00763 -0.00419 -0.00815 C35 1 0.533913 0.703434 0.572187 11.00000 0.03792 0.06377 = 0.03254 -0.01377 0.00329 0.00444 C36 1 0.596143 0.615154 0.633101 11.00000 0.05255 0.06175 = 0.06016 0.00719 -0.00603 -0.00094 AFIX 137 H36A 2 0.621063 0.586826 0.592485 11.00000 -1.50000 H36B 2 0.491872 0.612289 0.652292 11.00000 -1.50000 H36C 2 0.668894 0.618198 0.700762 11.00000 -1.50000 AFIX 0 C37 1 0.800277 0.627001 0.432792 11.00000 0.01756 0.07310 = 0.07579 -0.02572 0.00263 0.00521 AFIX 137 H37A 2 0.777901 0.623741 0.352405 11.00000 -1.50000 H37B 2 0.784481 0.596421 0.467782 11.00000 -1.50000 H37C 2 0.906973 0.637062 0.452589 11.00000 -1.50000 AFIX 0 C38 1 0.752684 0.730441 0.340132 11.00000 0.04038 0.07798 = 0.05776 -0.01642 0.00924 -0.02830 AFIX 137 H38A 2 0.681467 0.750857 0.292953 11.00000 -1.50000 H38B 2 0.789217 0.705018 0.295496 11.00000 -1.50000 H38C 2 0.840103 0.749326 0.373787 11.00000 -1.50000 AFIX 0 C39 1 0.541481 0.786043 0.484078 11.00000 0.06558 0.03522 = 0.07757 -0.01181 -0.02259 -0.00629 AFIX 137 H39A 2 0.452038 0.793411 0.521026 11.00000 -1.50000 H39B 2 0.520170 0.794823 0.405930 11.00000 -1.50000 H39C 2 0.630342 0.803956 0.519042 11.00000 -1.50000 AFIX 0 C40 1 0.436355 0.713650 0.662350 11.00000 0.03544 0.08119 = 0.03899 -0.02093 0.00751 0.00264 AFIX 137 H40A 2 0.500553 0.712834 0.734277 11.00000 -1.50000 H40B 2 0.355578 0.689621 0.660645 11.00000 -1.50000 H40C 2 0.389663 0.745121 0.650603 11.00000 -1.50000 AFIX 0 C41 1 0.496761 0.567296 0.309574 11.00000 0.03103 0.03646 = 0.04929 -0.00060 0.01080 0.00574 AFIX 43 H41 2 0.554681 0.551666 0.370204 11.00000 -1.20000 AFIX 0 C42 1 0.447708 0.547484 0.209144 11.00000 0.03589 0.03295 = 0.05844 -0.00872 0.01714 0.00028 AFIX 43 H42 2 0.466454 0.515947 0.186939 11.00000 -1.20000 AFIX 0 C43 1 0.299404 0.577695 0.030203 11.00000 0.06377 0.04476 = 0.03534 -0.01185 0.00330 -0.01535 AFIX 137 H43A 2 0.194723 0.590312 0.021339 11.00000 -1.50000 H43B 2 0.297144 0.544323 0.007488 11.00000 -1.50000 H43C 2 0.361481 0.595950 -0.015816 11.00000 -1.50000 AFIX 0 C44 1 0.368702 0.620717 0.208936 11.00000 0.02899 0.03145 = 0.03115 -0.00435 0.00807 -0.01008 C45 1 0.298478 0.666416 0.186355 11.00000 0.02844 0.03340 = 0.03839 -0.00282 0.00641 -0.01169 AFIX 43 H45 2 0.234726 0.672467 0.118793 11.00000 -1.20000 AFIX 0 C46 1 0.241008 0.743993 0.237000 11.00000 0.02316 0.03506 = 0.06062 0.00080 -0.00931 -0.00422 AFIX 2 H46 2 0.163136 0.741167 0.179115 11.00000 -1.20000 AFIX 0 C47 1 0.165667 0.758309 0.335826 11.00000 0.03402 0.03392 = 0.09170 -0.00651 0.02030 0.01031 AFIX 137 H47A 2 0.112361 0.730912 0.362242 11.00000 -1.50000 H47B 2 0.091737 0.783784 0.314804 11.00000 -1.50000 H47C 2 0.243915 0.769541 0.394689 11.00000 -1.50000 AFIX 0 C48 1 0.352060 0.781379 0.197854 11.00000 0.02589 0.02962 = 0.06276 0.01742 -0.00960 -0.00393 C49 1 0.446599 0.768079 0.119673 11.00000 0.03162 0.03560 = 0.07555 0.02148 0.00110 -0.00247 AFIX 43 H49 2 0.448309 0.735952 0.096317 11.00000 -1.20000 AFIX 0 C50 1 0.539492 0.801912 0.075125 11.00000 0.04306 0.05681 = 0.07813 0.03280 0.00398 -0.00065 AFIX 43 H50 2 0.605369 0.792530 0.023382 11.00000 -1.20000 AFIX 0 C51 1 0.533913 0.848114 0.106923 11.00000 0.05202 0.05429 = 0.11863 0.05353 -0.02914 -0.02918 AFIX 43 H51 2 0.594197 0.871306 0.076170 11.00000 -1.20000 AFIX 0 C52 1 0.436749 0.861616 0.186960 11.00000 0.06170 0.03399 = 0.11468 0.01851 -0.04035 -0.01711 AFIX 43 H52 2 0.433622 0.893686 0.210525 11.00000 -1.20000 AFIX 0 C53 1 0.347350 0.827586 0.229776 11.00000 0.04177 0.03865 = 0.07185 -0.00215 -0.01145 -0.00247 AFIX 43 H53 2 0.281910 0.836623 0.282100 11.00000 -1.20000 AFIX 0 SB1 7 0.205955 0.159055 0.977979 11.00000 0.07956 0.03777 = 0.04007 -0.00803 0.01220 -0.01732 F1 4 0.236369 0.096425 1.016977 11.00000 0.21008 0.04229 = 0.07311 0.01118 -0.00218 -0.02617 F2 4 0.180838 0.221675 0.938551 11.00000 0.11324 0.03644 = 0.09256 -0.00197 0.01539 -0.00599 F3A 4 0.306272 0.177977 1.111502 71.00000 0.06809 F4A 4 0.083677 0.143789 0.841266 71.00000 0.05535 F5A 4 0.009694 0.166862 1.029412 71.00000 0.07830 F6A 4 0.373343 0.156975 0.903964 71.00000 0.06971 F3B 4 0.255951 0.170290 1.130124 -71.00000 0.05454 F4B 4 0.191727 0.134001 0.834467 -71.00000 0.10059 F5B 4 0.009946 0.144711 1.008929 -71.00000 0.10564 F6B 4 0.418554 0.161598 0.963121 -71.00000 0.07853 SB2 7 0.735873 0.441170 0.477606 11.00000 0.06742 0.04198 = 0.03967 0.00245 -0.00189 0.00793 F7 4 0.720955 0.376538 0.439254 11.00000 0.05880 0.06219 = 0.12187 -0.02652 -0.00091 0.00020 F8 4 0.744630 0.505783 0.516173 11.00000 0.20446 0.03721 = 0.11718 -0.00236 -0.02900 0.01018 F9A 4 0.728727 0.430355 0.629205 81.00000 0.08978 F10A 4 0.769190 0.458498 0.334512 81.00000 0.08798 F11A 4 0.941742 0.438963 0.468383 81.00000 0.08004 F12A 4 0.531979 0.454565 0.448707 81.00000 0.06478 F9B 4 0.758821 0.421031 0.624440 -81.00000 0.04553 F10B 4 0.658452 0.456133 0.330455 -81.00000 0.08032 F11B 4 0.953430 0.434438 0.515083 -81.00000 0.06295 F12B 4 0.517732 0.436004 0.488009 -81.00000 0.07019 PART 1 O1A 8 0.246591 0.536490 0.734967 21.00000 0.02793 C60A 1 0.386728 0.528288 0.785511 21.00000 31.00000 AFIX 23 H60A 2 0.382935 0.515045 0.860163 21.00000 -1.20000 H60B 2 0.447524 0.557947 0.792578 21.00000 -1.20000 AFIX 0 C61A 1 0.462553 0.489662 0.707008 21.00000 31.00000 AFIX 33 H61A 2 0.566093 0.481346 0.741403 21.00000 -1.50000 H61B 2 0.467728 0.503663 0.634161 21.00000 -1.50000 H61C 2 0.398901 0.461022 0.698804 21.00000 -1.50000 AFIX 0 C62A 1 0.203037 0.579963 0.749395 21.00000 31.00000 AFIX 23 H62A 2 0.238255 0.596886 0.686335 21.00000 -1.20000 H62B 2 0.273884 0.590259 0.814835 21.00000 -1.20000 AFIX 0 PART 2 O1B 8 0.252492 0.557761 0.744693 -21.00000 0.02980 C60B 1 0.336137 0.523941 0.710093 -21.00000 31.00000 AFIX 23 H60C 2 0.369337 0.534116 0.639402 -21.00000 -1.20000 H60D 2 0.270844 0.495486 0.694662 -21.00000 -1.20000 AFIX 0 C61B 1 0.489235 0.508674 0.795060 -21.00000 31.00000 AFIX 33 H61D 2 0.536790 0.480776 0.765818 -21.00000 -1.50000 H61E 2 0.459556 0.501126 0.867619 -21.00000 -1.50000 H61F 2 0.562539 0.535026 0.802346 -21.00000 -1.50000 AFIX 0 C62B 1 0.112981 0.567864 0.689405 -21.00000 31.00000 AFIX 23 H62C 2 0.047329 0.539213 0.681893 -21.00000 -1.20000 H62D 2 0.122236 0.580380 0.614854 -21.00000 -1.20000 AFIX 0 PART 0 C63 1 0.041142 0.608474 0.765509 11.00000 31.00000 PART 1 AFIX 33 H63A 2 0.061670 0.642579 0.773014 21.00000 -1.50000 H63B 2 0.002154 0.596756 0.832006 21.00000 -1.50000 H63C 2 -0.035412 0.602819 0.700964 21.00000 -1.50000 PART 2 H63D 2 -0.061497 0.618792 0.733418 -21.00000 -1.50000 H63E 2 0.110473 0.635834 0.772993 -21.00000 -1.50000 H63F 2 0.036191 0.594501 0.838415 -21.00000 -1.50000 HKLF 4 REM fjl202ds in P2(1) REM R1 = 0.0480 for 12308 Fo > 4sig(Fo) and 0.0614 for all 14491 data REM 679 parameters refined using 26 restraints END ; 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.04189(5) 0.430137(16) 0.06156(4) 0.02477(10) Uani 1 1 d . . . Cl1 Cl 0.29108(17) 0.45009(7) 0.01907(14) 0.0383(4) Uani 1 1 d . . . N1 N 0.0524(5) 0.4877(2) 0.1714(4) 0.0282(11) Uani 1 1 d . . . N2 N 0.1680(6) 0.4020(2) 0.2074(4) 0.0293(11) Uani 1 1 d . . . N3 N 0.1377(7) 0.5158(2) 0.3368(4) 0.0352(13) Uani 1 1 d . . . C1 C -0.0604(8) 0.3692(3) -0.0276(6) 0.0418(16) Uani 1 1 d . . . C2 C -0.1649(8) 0.3887(3) 0.0421(6) 0.0438(18) Uani 1 1 d . . . C3 C -0.1994(6) 0.4366(3) 0.0065(5) 0.0388(16) Uani 1 1 d . . . C4 C -0.1115(7) 0.4478(3) -0.0834(5) 0.0330(14) Uani 1 1 d . . . C5 C -0.0314(7) 0.4041(3) -0.1054(5) 0.0309(14) Uani 1 1 d . . . C6 C 0.0012(14) 0.3192(3) -0.0240(9) 0.087(4) Uani 1 1 d . . . H6A H -0.0509 0.3011 -0.0865 0.130 Uiso 1 1 calc R . . H6B H -0.0171 0.3040 0.0453 0.130 Uiso 1 1 calc R . . H6C H 0.1115 0.3199 -0.0284 0.130 Uiso 1 1 calc R . . C7 C -0.2293(10) 0.3621(4) 0.1314(7) 0.070(3) Uani 1 1 d . . . H7A H -0.2661 0.3847 0.1829 0.105 Uiso 1 1 calc R . . H7B H -0.1492 0.3421 0.1712 0.105 Uiso 1 1 calc R . . H7C H -0.3146 0.3422 0.0987 0.105 Uiso 1 1 calc R . . C8 C -0.3058(8) 0.4692(4) 0.0531(7) 0.061(3) Uani 1 1 d . . . H8A H -0.4101 0.4641 0.0159 0.091 Uiso 1 1 calc R . . H8B H -0.2750 0.5021 0.0419 0.091 Uiso 1 1 calc R . . H8C H -0.3027 0.4630 0.1323 0.091 Uiso 1 1 calc R . . C9 C -0.1132(10) 0.4918(3) -0.1480(7) 0.052(2) Uani 1 1 d . . . H9A H -0.0098 0.4983 -0.1659 0.078 Uiso 1 1 calc R . . H9B H -0.1467 0.5182 -0.1047 0.078 Uiso 1 1 calc R . . H9C H -0.1841 0.4883 -0.2164 0.078 Uiso 1 1 calc R . . C10 C 0.0664(10) 0.3998(4) -0.1972(6) 0.061(3) Uani 1 1 d . . . H10A H 0.1527 0.3785 -0.1742 0.091 Uiso 1 1 calc R . . H10B H 0.1056 0.4312 -0.2138 0.091 Uiso 1 1 calc R . . H10C H 0.0047 0.3870 -0.2632 0.091 Uiso 1 1 calc R . . C11 C 0.0073(7) 0.5334(2) 0.1761(5) 0.0308(13) Uani 1 1 d . . . H11 H -0.0508 0.5506 0.1182 0.037 Uiso 1 1 calc R . . C12 C 0.0606(8) 0.5509(2) 0.2802(6) 0.0351(14) Uani 1 1 d . . . H12 H 0.0452 0.5820 0.3065 0.042 Uiso 1 1 calc R . . C13 C 0.2035(10) 0.5179(3) 0.4532(6) 0.051(2) Uani 1 1 d . . . H13A H 0.2423 0.5499 0.4710 0.076 Uiso 1 1 calc R . . H13B H 0.2878 0.4950 0.4669 0.076 Uiso 1 1 calc R . . H13C H 0.1243 0.5100 0.4996 0.076 Uiso 1 1 calc R . . C14 C 0.1304(7) 0.4773(2) 0.2701(5) 0.0272(12) Uani 1 1 d . . . C15 C 0.1990(6) 0.4317(3) 0.2880(5) 0.0303(12) Uani 1 1 d . . . H15 H 0.2629 0.4236 0.3543 0.036 Uiso 1 1 calc R . . C16 C 0.2426(7) 0.3550(2) 0.2139(6) 0.0320(13) Uani 1 1 d D . . H16 H 0.223(8) 0.354(3) 0.1359(18) 0.038 Uiso 1 1 d D . . C17 C 0.4138(8) 0.3579(3) 0.2660(8) 0.052(2) Uani 1 1 d . . . H17A H 0.4692 0.3793 0.2220 0.078 Uiso 1 1 calc R . . H17B H 0.4599 0.3262 0.2670 0.078 Uiso 1 1 calc R . . H17C H 0.4200 0.3700 0.3417 0.078 Uiso 1 1 calc R . . C18 C 0.1551(7) 0.3192(2) 0.2723(5) 0.0312(13) Uani 1 1 d . . . C19 C 0.0637(8) 0.3300(3) 0.3521(6) 0.0392(15) Uani 1 1 d . . . H19 H 0.0504 0.3621 0.3719 0.047 Uiso 1 1 calc R . . C20 C -0.0089(8) 0.2945(3) 0.4038(6) 0.0430(17) Uani 1 1 d . . . H20 H -0.0691 0.3028 0.4599 0.052 Uiso 1 1 calc R . . C21 C 0.0035(9) 0.2479(3) 0.3765(7) 0.051(2) Uani 1 1 d . . . H21 H -0.0486 0.2240 0.4120 0.062 Uiso 1 1 calc R . . C22 C 0.0934(9) 0.2362(3) 0.2962(6) 0.0438(17) Uani 1 1 d . . . H22 H 0.1038 0.2038 0.2768 0.053 Uiso 1 1 calc R . . C23 C 0.1694(8) 0.2709(2) 0.2429(6) 0.0360(14) Uani 1 1 d . . . H23 H 0.2303 0.2623 0.1874 0.043 Uiso 1 1 calc R . . Rh31 Rh 0.45749(5) 0.672627(18) 0.41280(4) 0.02762(11) Uani 1 1 d . . . Cl31 Cl 0.21615(16) 0.64820(7) 0.46483(13) 0.0347(4) Uani 1 1 d . . . N31 N 0.4482(6) 0.61373(19) 0.3082(4) 0.0277(11) Uani 1 1 d . . . N32 N 0.3243(6) 0.69813(19) 0.2591(4) 0.0268(10) Uani 1 1 d . . . N33 N 0.3667(7) 0.5814(2) 0.1465(5) 0.0346(12) Uani 1 1 d . . . C31 C 0.6065(7) 0.6593(3) 0.5606(6) 0.0397(15) Uani 1 1 d . . . C32 C 0.6963(7) 0.6631(3) 0.4716(6) 0.0416(17) Uani 1 1 d . . . C33 C 0.6729(8) 0.7094(3) 0.4281(6) 0.0425(17) Uani 1 1 d . . . C34 C 0.5747(8) 0.7344(3) 0.4935(6) 0.0393(15) Uani 1 1 d . . . C35 C 0.5339(9) 0.7034(4) 0.5722(6) 0.045(2) Uani 1 1 d . . . C36 C 0.5961(10) 0.6152(4) 0.6331(7) 0.059(2) Uani 1 1 d . . . H36A H 0.6211 0.5868 0.5925 0.089 Uiso 1 1 calc R . . H36B H 0.4919 0.6123 0.6523 0.089 Uiso 1 1 calc R . . H36C H 0.6689 0.6182 0.7008 0.089 Uiso 1 1 calc R . . C37 C 0.8003(8) 0.6270(4) 0.4328(8) 0.056(2) Uani 1 1 d . . . H37A H 0.7779 0.6237 0.3524 0.084 Uiso 1 1 calc R . . H37B H 0.7845 0.5964 0.4678 0.084 Uiso 1 1 calc R . . H37C H 0.9070 0.6371 0.4526 0.084 Uiso 1 1 calc R . . C38 C 0.7527(9) 0.7304(4) 0.3401(7) 0.058(2) Uani 1 1 d . . . H38A H 0.6815 0.7509 0.2930 0.088 Uiso 1 1 calc R . . H38B H 0.7892 0.7050 0.2955 0.088 Uiso 1 1 calc R . . H38C H 0.8401 0.7493 0.3738 0.088 Uiso 1 1 calc R . . C39 C 0.5415(11) 0.7860(3) 0.4841(8) 0.062(2) Uani 1 1 d . . . H39A H 0.4520 0.7934 0.5210 0.094 Uiso 1 1 calc R . . H39B H 0.5202 0.7948 0.4059 0.094 Uiso 1 1 calc R . . H39C H 0.6303 0.8040 0.5190 0.094 Uiso 1 1 calc R . . C40 C 0.4364(9) 0.7137(4) 0.6624(6) 0.052(2) Uani 1 1 d . . . H40A H 0.5006 0.7128 0.7343 0.077 Uiso 1 1 calc R . . H40B H 0.3556 0.6896 0.6606 0.077 Uiso 1 1 calc R . . H40C H 0.3897 0.7451 0.6506 0.077 Uiso 1 1 calc R . . C41 C 0.4968(8) 0.5673(3) 0.3096(6) 0.0384(15) Uani 1 1 d . . . H41 H 0.5547 0.5517 0.3702 0.046 Uiso 1 1 calc R . . C42 C 0.4477(8) 0.5475(3) 0.2091(6) 0.0414(16) Uani 1 1 d . . . H42 H 0.4665 0.5159 0.1869 0.050 Uiso 1 1 calc R . . C43 C 0.2994(10) 0.5777(3) 0.0302(6) 0.048(2) Uani 1 1 d . . . H43A H 0.1947 0.5903 0.0213 0.072 Uiso 1 1 calc R . . H43B H 0.2971 0.5443 0.0075 0.072 Uiso 1 1 calc R . . H43C H 0.3615 0.5960 -0.0158 0.072 Uiso 1 1 calc R . . C44 C 0.3687(7) 0.6207(2) 0.2089(5) 0.0302(13) Uani 1 1 d . . . C45 C 0.2985(7) 0.6664(3) 0.1864(5) 0.0332(13) Uani 1 1 d . . . H45 H 0.2347 0.6725 0.1188 0.040 Uiso 1 1 calc R . . C46 C 0.2410(7) 0.7440(3) 0.2370(7) 0.0409(16) Uani 1 1 d . . . H46 H 0.163(9) 0.741(3) 0.179(7) 0.049 Uiso 1 1 d . . . C47 C 0.1657(8) 0.7583(3) 0.3358(7) 0.052(2) Uani 1 1 d . . . H47A H 0.1124 0.7309 0.3622 0.078 Uiso 1 1 calc R . . H47B H 0.0917 0.7838 0.3148 0.078 Uiso 1 1 calc R . . H47C H 0.2439 0.7695 0.3947 0.078 Uiso 1 1 calc R . . C48 C 0.3521(8) 0.7814(3) 0.1979(7) 0.0408(17) Uani 1 1 d . . . C49 C 0.4466(8) 0.7681(3) 0.1197(7) 0.0481(19) Uani 1 1 d . . . H49 H 0.4483 0.7360 0.0963 0.058 Uiso 1 1 calc R . . C50 C 0.5395(9) 0.8019(4) 0.0751(8) 0.060(3) Uani 1 1 d . . . H50 H 0.6054 0.7925 0.0234 0.072 Uiso 1 1 calc R . . C51 C 0.5339(11) 0.8481(4) 0.1069(10) 0.079(4) Uani 1 1 d . . . H51 H 0.5942 0.8713 0.0762 0.094 Uiso 1 1 calc R . . C52 C 0.4367(12) 0.8616(3) 0.1870(10) 0.075(3) Uani 1 1 d . . . H52 H 0.4336 0.8937 0.2105 0.090 Uiso 1 1 calc R . . C53 C 0.3474(9) 0.8276(3) 0.2298(7) 0.052(2) Uani 1 1 d . . . H53 H 0.2819 0.8366 0.2821 0.063 Uiso 1 1 calc R . . Sb1 Sb 0.20595(7) 0.159055(19) 0.97798(4) 0.05208(15) Uani 1 1 d D . . F1 F 0.2364(11) 0.0964(3) 1.0170(5) 0.110(3) Uani 1 1 d . . . F2 F 0.1808(8) 0.2217(2) 0.9386(5) 0.0806(17) Uani 1 1 d . . . F3A F 0.3063(12) 0.1780(4) 1.1115(7) 0.068(3) Uiso 0.610(14) 1 d PD . . F4A F 0.0837(9) 0.1438(3) 0.8413(5) 0.055(3) Uiso 0.610(14) 1 d PD . . F5A F 0.0097(9) 0.1669(5) 1.0294(9) 0.078(3) Uiso 0.610(14) 1 d PD . . F6A F 0.3733(10) 0.1570(3) 0.9040(8) 0.070(3) Uiso 0.610(14) 1 d PD . . F3B F 0.2560(17) 0.1703(6) 1.1301(7) 0.055(4) Uiso 0.390(14) 1 d PD . . F4B F 0.192(3) 0.1340(7) 0.8345(9) 0.101(7) Uiso 0.390(14) 1 d PD . . F5B F 0.0099(14) 0.1447(9) 1.0089(19) 0.106(7) Uiso 0.390(14) 1 d PD . . F6B F 0.4186(11) 0.1616(7) 0.9631(16) 0.079(5) Uiso 0.390(14) 1 d PD . . Sb2 Sb 0.73587(7) 0.441170(19) 0.47761(4) 0.05049(15) Uani 1 1 d D . . F7 F 0.7210(6) 0.3765(2) 0.4393(6) 0.0821(18) Uani 1 1 d . . . F8 F 0.7446(12) 0.5058(3) 0.5162(7) 0.124(3) Uani 1 1 d . . . F9A F 0.7287(19) 0.4304(7) 0.6292(8) 0.090(6) Uiso 0.525(16) 1 d PD . . F10A F 0.7692(17) 0.4585(5) 0.3345(7) 0.088(5) Uiso 0.525(16) 1 d PD . . F11A F 0.9417(10) 0.4390(6) 0.4684(13) 0.080(4) Uiso 0.525(16) 1 d PD . . F12A F 0.5320(9) 0.4546(4) 0.4487(9) 0.065(3) Uiso 0.525(16) 1 d PD . . F9B F 0.7588(15) 0.4210(5) 0.6244(6) 0.046(3) Uiso 0.475(16) 1 d PD . . F10B F 0.6585(17) 0.4561(5) 0.3305(7) 0.080(5) Uiso 0.475(16) 1 d PD . . F11B F 0.9534(9) 0.4344(5) 0.5151(11) 0.063(3) Uiso 0.475(16) 1 d PD . . F12B F 0.5177(9) 0.4360(6) 0.4880(11) 0.070(4) Uiso 0.475(16) 1 d PD . . O1A O 0.2466(7) 0.5365(3) 0.7350(5) 0.0279(16) Uiso 0.627(9) 1 d PD A 1 C60A C 0.3867(14) 0.5283(6) 0.7855(11) 0.0628(13) Uiso 0.627(9) 1 d PD A 1 H60A H 0.3829 0.5150 0.8602 0.075 Uiso 0.627(9) 1 calc PR A 1 H60B H 0.4475 0.5579 0.7926 0.075 Uiso 0.627(9) 1 calc PR A 1 C61A C 0.4626(17) 0.4897(5) 0.7070(12) 0.0628(13) Uiso 0.627(9) 1 d PD A 1 H61A H 0.5661 0.4813 0.7414 0.094 Uiso 0.627(9) 1 calc PR A 1 H61B H 0.4677 0.5037 0.6342 0.094 Uiso 0.627(9) 1 calc PR A 1 H61C H 0.3989 0.4610 0.6988 0.094 Uiso 0.627(9) 1 calc PR A 1 C62A C 0.2030(15) 0.5800(4) 0.7494(13) 0.0628(13) Uiso 0.627(9) 1 d PD A 1 H62A H 0.2383 0.5969 0.6863 0.075 Uiso 0.627(9) 1 calc PR A 1 H62B H 0.2739 0.5903 0.8148 0.075 Uiso 0.627(9) 1 calc PR A 1 O1B O 0.2525(13) 0.5578(5) 0.7447(9) 0.030(3) Uiso 0.373(9) 1 d PD A 2 C60B C 0.336(2) 0.5239(8) 0.7101(18) 0.0628(13) Uiso 0.373(9) 1 d PD A 2 H60C H 0.3693 0.5341 0.6394 0.075 Uiso 0.373(9) 1 calc PR A 2 H60D H 0.2708 0.4955 0.6947 0.075 Uiso 0.373(9) 1 calc PR A 2 C61B C 0.489(2) 0.5087(9) 0.7951(19) 0.0628(13) Uiso 0.373(9) 1 d PD A 2 H61D H 0.5368 0.4808 0.7658 0.094 Uiso 0.373(9) 1 calc PR A 2 H61E H 0.4596 0.5011 0.8676 0.094 Uiso 0.373(9) 1 calc PR A 2 H61F H 0.5625 0.5350 0.8023 0.094 Uiso 0.373(9) 1 calc PR A 2 C62B C 0.113(2) 0.5679(8) 0.6894(16) 0.0628(13) Uiso 0.373(9) 1 d PD A 2 H62C H 0.0473 0.5392 0.6819 0.075 Uiso 0.373(9) 1 calc PR A 2 H62D H 0.1222 0.5804 0.6149 0.075 Uiso 0.373(9) 1 calc PR A 2 C63 C 0.0411(10) 0.6085(4) 0.7655(8) 0.0628(13) Uiso 1 1 d D . . H63A H 0.0617 0.6426 0.7730 0.094 Uiso 0.627(9) 1 calc PR A 1 H63B H 0.0022 0.5968 0.8320 0.094 Uiso 0.627(9) 1 calc PR A 1 H63C H -0.0354 0.6028 0.7010 0.094 Uiso 0.627(9) 1 calc PR A 1 H63D H -0.0615 0.6188 0.7334 0.094 Uiso 0.373(9) 1 d PR A 2 H63E H 0.1105 0.6358 0.7730 0.094 Uiso 0.373(9) 1 d PR A 2 H63F H 0.0362 0.5945 0.8384 0.094 Uiso 0.373(9) 1 d PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0206(2) 0.0227(2) 0.0306(2) -0.00433(18) 0.00192(15) -0.00072(17) Cl1 0.0275(7) 0.0413(10) 0.0489(8) -0.0190(7) 0.0156(6) -0.0099(6) N1 0.019(2) 0.032(3) 0.034(3) 0.002(2) 0.0042(19) 0.003(2) N2 0.028(3) 0.027(3) 0.032(3) 0.004(2) 0.001(2) -0.003(2) N3 0.042(3) 0.028(3) 0.035(3) -0.012(2) 0.007(2) -0.012(2) C1 0.044(4) 0.035(4) 0.042(4) -0.008(3) -0.010(3) -0.006(3) C2 0.029(3) 0.056(5) 0.044(4) -0.001(3) -0.004(3) -0.021(3) C3 0.016(2) 0.051(5) 0.048(3) -0.013(3) -0.001(2) -0.002(3) C4 0.023(3) 0.037(4) 0.039(3) -0.006(3) 0.003(2) 0.003(2) C5 0.025(3) 0.040(4) 0.026(3) -0.011(3) -0.002(2) -0.005(3) C6 0.119(9) 0.033(5) 0.089(7) -0.023(5) -0.058(7) 0.000(5) C7 0.052(5) 0.096(8) 0.059(5) 0.018(5) -0.006(4) -0.043(5) C8 0.025(3) 0.104(8) 0.053(5) -0.021(5) 0.008(3) 0.007(4) C9 0.060(5) 0.041(4) 0.050(4) 0.011(3) -0.012(4) -0.005(4) C10 0.047(4) 0.096(7) 0.038(4) -0.023(4) -0.002(3) 0.012(5) C11 0.030(3) 0.021(3) 0.044(3) -0.002(2) 0.014(3) -0.002(2) C12 0.036(3) 0.024(3) 0.048(4) -0.011(3) 0.015(3) -0.004(3) C13 0.068(5) 0.046(5) 0.038(4) -0.007(3) 0.002(4) -0.018(4) C14 0.024(3) 0.027(3) 0.030(3) -0.004(2) 0.002(2) -0.004(2) C15 0.026(3) 0.029(3) 0.034(3) 0.003(3) -0.003(2) 0.001(3) C16 0.023(3) 0.030(3) 0.043(3) 0.005(3) 0.003(3) 0.007(2) C17 0.028(3) 0.029(3) 0.098(6) 0.018(4) 0.004(4) 0.005(3) C18 0.024(3) 0.025(3) 0.042(3) 0.002(3) -0.003(2) 0.001(2) C19 0.042(4) 0.034(4) 0.043(4) 0.003(3) 0.011(3) 0.003(3) C20 0.033(3) 0.047(4) 0.050(4) 0.009(3) 0.009(3) 0.000(3) C21 0.045(4) 0.041(4) 0.065(5) 0.022(4) -0.006(4) -0.004(3) C22 0.046(4) 0.028(4) 0.055(4) 0.005(3) -0.005(3) -0.001(3) C23 0.035(3) 0.024(3) 0.047(4) 0.000(3) -0.001(3) 0.006(3) Rh31 0.01847(19) 0.0307(3) 0.0337(2) -0.0061(2) 0.00353(16) -0.00191(18) Cl31 0.0255(7) 0.0402(10) 0.0403(8) -0.0083(6) 0.0107(6) -0.0063(6) N31 0.029(3) 0.022(3) 0.033(2) -0.0054(19) 0.006(2) -0.001(2) N32 0.023(2) 0.023(3) 0.033(3) 0.001(2) 0.0008(19) -0.001(2) N33 0.038(3) 0.029(3) 0.040(3) -0.003(2) 0.014(2) -0.005(2) C31 0.027(3) 0.046(4) 0.043(3) -0.004(3) -0.008(3) -0.006(3) C32 0.019(3) 0.051(5) 0.053(4) -0.012(3) -0.004(2) -0.002(3) C33 0.027(3) 0.054(5) 0.043(4) -0.011(3) -0.007(3) -0.013(3) C34 0.035(3) 0.039(4) 0.041(3) -0.008(3) -0.004(3) -0.008(3) C35 0.038(4) 0.064(6) 0.033(4) -0.014(3) 0.003(3) 0.004(3) C36 0.053(5) 0.062(6) 0.060(5) 0.007(4) -0.006(4) -0.001(4) C37 0.018(3) 0.073(6) 0.076(6) -0.026(5) 0.003(3) 0.005(3) C38 0.040(4) 0.078(6) 0.058(5) -0.016(4) 0.009(4) -0.028(4) C39 0.066(5) 0.035(4) 0.078(6) -0.012(4) -0.023(5) -0.006(4) C40 0.035(4) 0.081(6) 0.039(4) -0.021(4) 0.008(3) 0.003(4) C41 0.031(3) 0.036(4) 0.049(4) -0.001(3) 0.011(3) 0.006(3) C42 0.036(4) 0.033(4) 0.058(4) -0.009(3) 0.017(3) 0.000(3) C43 0.064(5) 0.045(5) 0.035(4) -0.012(3) 0.003(3) -0.015(4) C44 0.029(3) 0.031(3) 0.031(3) -0.004(2) 0.008(2) -0.010(3) C45 0.028(3) 0.033(4) 0.038(3) -0.003(3) 0.006(2) -0.012(3) C46 0.023(3) 0.035(4) 0.061(4) 0.001(3) -0.009(3) -0.004(3) C47 0.034(4) 0.034(4) 0.092(6) -0.007(4) 0.020(4) 0.010(3) C48 0.026(3) 0.030(4) 0.063(5) 0.017(3) -0.010(3) -0.004(3) C49 0.032(4) 0.036(4) 0.076(5) 0.021(4) 0.001(3) -0.002(3) C50 0.043(4) 0.057(6) 0.078(6) 0.033(5) 0.004(4) -0.001(4) C51 0.052(5) 0.054(6) 0.119(9) 0.054(6) -0.029(5) -0.029(5) C52 0.062(6) 0.034(5) 0.115(9) 0.019(5) -0.040(6) -0.017(4) C53 0.042(4) 0.039(4) 0.072(5) -0.002(4) -0.011(4) -0.002(3) Sb1 0.0796(4) 0.0378(3) 0.0401(2) -0.0080(2) 0.0122(2) -0.0173(3) F1 0.210(9) 0.042(4) 0.073(4) 0.011(3) -0.002(5) -0.026(5) F2 0.113(5) 0.036(3) 0.093(4) -0.002(3) 0.015(4) -0.006(3) Sb2 0.0674(3) 0.0420(3) 0.0397(2) 0.0025(2) -0.0019(2) 0.0079(3) F7 0.059(3) 0.062(4) 0.122(5) -0.027(4) -0.001(3) 0.000(3) F8 0.204(9) 0.037(4) 0.117(6) -0.002(4) -0.029(6) 0.010(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N1 2.098(6) . ? Rh1 N2 2.124(5) . ? Rh1 C4 2.138(6) . ? Rh1 C2 2.149(7) . ? Rh1 C3 2.149(5) . ? Rh1 C1 2.164(7) . ? Rh1 C5 2.183(6) . ? Rh1 Cl1 2.3865(15) . ? N1 C14 1.338(8) . ? N1 C11 1.352(8) . ? N2 C15 1.293(8) . ? N2 C16 1.476(8) . ? N3 C12 1.337(10) . ? N3 C14 1.354(8) . ? N3 C13 1.463(9) . ? C1 C5 1.413(10) . ? C1 C2 1.441(11) . ? C1 C6 1.509(12) . ? C2 C3 1.439(12) . ? C2 C7 1.495(11) . ? C3 C4 1.459(9) . ? C3 C8 1.477(10) . ? C4 C5 1.461(10) . ? C4 C9 1.470(10) . ? C5 C10 1.506(10) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.386(9) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.426(9) . ? C15 H15 0.9500 . ? C16 C18 1.505(9) . ? C16 C17 1.558(9) . ? C16 H16 0.95(2) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.377(9) . ? C18 C23 1.416(9) . ? C19 C20 1.383(10) . ? C19 H19 0.9500 . ? C20 C21 1.362(12) . ? C20 H20 0.9500 . ? C21 C22 1.380(12) . ? C21 H21 0.9500 . ? C22 C23 1.395(10) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? Rh31 N31 2.090(5) . ? Rh31 C31 2.120(6) . ? Rh31 C32 2.146(6) . ? Rh31 C33 2.148(7) . ? Rh31 C35 2.157(7) . ? Rh31 C34 2.189(7) . ? Rh31 N32 2.198(5) . ? Rh31 Cl31 2.3970(15) . ? N31 C44 1.332(8) . ? N31 C41 1.376(9) . ? N32 C45 1.260(8) . ? N32 C46 1.493(9) . ? N33 C44 1.343(9) . ? N33 C42 1.366(10) . ? N33 C43 1.469(9) . ? C31 C35 1.414(12) . ? C31 C32 1.430(10) . ? C31 C36 1.536(12) . ? C32 C33 1.416(12) . ? C32 C37 1.487(11) . ? C33 C34 1.436(10) . ? C33 C38 1.482(11) . ? C34 C35 1.379(11) . ? C34 C39 1.487(11) . ? C35 C40 1.511(9) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.365(11) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.439(10) . ? C45 H45 0.9500 . ? C46 C47 1.507(11) . ? C46 C48 1.555(10) . ? C46 H46 0.92(8) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C53 1.361(12) . ? C48 C49 1.398(12) . ? C49 C50 1.411(11) . ? C49 H49 0.9500 . ? C50 C51 1.361(16) . ? C50 H50 0.9500 . ? C51 C52 1.433(17) . ? C51 H51 0.9500 . ? C52 C53 1.386(13) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? Sb1 F3A 1.828(7) . ? Sb1 F6A 1.828(7) . ? Sb1 F2 1.835(6) . ? Sb1 F1 1.839(7) . ? Sb1 F5B 1.859(10) . ? Sb1 F4B 1.879(9) . ? Sb1 F3B 1.879(8) . ? Sb1 F6B 1.905(9) . ? Sb1 F4A 1.912(6) . ? Sb1 F5A 1.927(7) . ? F3A F3B 0.567(15) . ? F4A F4B 1.00(2) . ? F5A F5B 0.67(2) . ? F6A F6B 0.788(16) . ? Sb2 F12A 1.822(7) . ? Sb2 F11A 1.831(8) . ? Sb2 F9B 1.867(7) . ? Sb2 F10A 1.875(8) . ? Sb2 F8 1.880(7) . ? Sb2 F7 1.881(7) . ? Sb2 F10B 1.884(8) . ? Sb2 F9A 1.886(8) . ? Sb2 F11B 1.918(8) . ? Sb2 F12B 1.946(8) . ? F10A F10B 0.971(15) . ? F11A F11B 0.580(15) . ? F12A F12B 0.732(14) . ? O1A C62A 1.303(11) . ? O1A C60A 1.324(11) . ? C60A C61A 1.649(12) . ? C60A H60A 0.9900 . ? C60A H60B 0.9900 . ? C61A H61A 0.9800 . ? C61A H61B 0.9800 . ? C61A H61C 0.9800 . ? C62A C63 1.670(12) . ? C62A H62A 0.9900 . ? C62A H62B 0.9900 . ? O1B C60B 1.308(13) . ? O1B C62B 1.351(13) . ? C60B C61B 1.645(14) . ? C60B H60C 0.9900 . ? C60B H60D 0.9900 . ? C61B H61D 0.9800 . ? C61B H61E 0.9800 . ? C61B H61F 0.9800 . ? C62B C63 1.652(13) . ? C62B H62C 0.9900 . ? C62B H62D 0.9900 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C63 H63D 0.9800 . ? C63 H63E 0.9800 . ? C63 H63F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Rh1 N2 77.2(2) . . ? N1 Rh1 C4 108.6(2) . . ? N2 Rh1 C4 169.7(2) . . ? N1 Rh1 C2 117.1(3) . . ? N2 Rh1 C2 103.3(3) . . ? C4 Rh1 C2 66.5(3) . . ? N1 Rh1 C3 95.3(2) . . ? N2 Rh1 C3 132.8(2) . . ? C4 Rh1 C3 39.8(2) . . ? C2 Rh1 C3 39.1(3) . . ? N1 Rh1 C1 156.2(2) . . ? N2 Rh1 C1 105.2(3) . . ? C4 Rh1 C1 65.9(3) . . ? C2 Rh1 C1 39.0(3) . . ? C3 Rh1 C1 65.3(3) . . ? N1 Rh1 C5 147.1(2) . . ? N2 Rh1 C5 135.7(2) . . ? C4 Rh1 C5 39.5(3) . . ? C2 Rh1 C5 64.7(3) . . ? C3 Rh1 C5 65.1(2) . . ? C1 Rh1 C5 37.9(3) . . ? N1 Rh1 Cl1 89.59(14) . . ? N2 Rh1 Cl1 82.96(14) . . ? C4 Rh1 Cl1 105.24(18) . . ? C2 Rh1 Cl1 153.2(2) . . ? C3 Rh1 Cl1 144.1(2) . . ? C1 Rh1 Cl1 114.2(2) . . ? C5 Rh1 Cl1 92.43(17) . . ? C14 N1 C11 106.7(5) . . ? C14 N1 Rh1 112.4(4) . . ? C11 N1 Rh1 140.9(4) . . ? C15 N2 C16 119.4(5) . . ? C15 N2 Rh1 115.6(4) . . ? C16 N2 Rh1 124.0(4) . . ? C12 N3 C14 107.4(5) . . ? C12 N3 C13 125.6(6) . . ? C14 N3 C13 126.7(7) . . ? C5 C1 C2 108.6(7) . . ? C5 C1 C6 124.9(8) . . ? C2 C1 C6 126.4(9) . . ? C5 C1 Rh1 71.8(4) . . ? C2 C1 Rh1 69.9(4) . . ? C6 C1 Rh1 127.0(5) . . ? C3 C2 C1 107.8(6) . . ? C3 C2 C7 127.2(8) . . ? C1 C2 C7 125.0(9) . . ? C3 C2 Rh1 70.4(4) . . ? C1 C2 Rh1 71.1(4) . . ? C7 C2 Rh1 126.0(5) . . ? C2 C3 C4 108.5(6) . . ? C2 C3 C8 125.9(7) . . ? C4 C3 C8 125.6(8) . . ? C2 C3 Rh1 70.4(4) . . ? C4 C3 Rh1 69.7(3) . . ? C8 C3 Rh1 125.7(5) . . ? C3 C4 C5 105.9(6) . . ? C3 C4 C9 128.1(7) . . ? C5 C4 C9 125.7(6) . . ? C3 C4 Rh1 70.5(3) . . ? C5 C4 Rh1 71.9(4) . . ? C9 C4 Rh1 126.9(5) . . ? C1 C5 C4 109.1(6) . . ? C1 C5 C10 128.1(7) . . ? C4 C5 C10 122.8(7) . . ? C1 C5 Rh1 70.3(4) . . ? C4 C5 Rh1 68.6(3) . . ? C10 C5 Rh1 126.5(5) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C12 108.2(6) . . ? N1 C11 H11 125.9 . . ? C12 C11 H11 125.9 . . ? N3 C12 C11 107.4(6) . . ? N3 C12 H12 126.3 . . ? C11 C12 H12 126.3 . . ? N3 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 N3 110.2(6) . . ? N1 C14 C15 119.5(5) . . ? N3 C14 C15 130.2(6) . . ? N2 C15 C14 115.0(5) . . ? N2 C15 H15 122.5 . . ? C14 C15 H15 122.5 . . ? N2 C16 C18 112.0(5) . . ? N2 C16 C17 112.0(5) . . ? C18 C16 C17 111.7(5) . . ? N2 C16 H16 87(4) . . ? C18 C16 H16 115(4) . . ? C17 C16 H16 117(4) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 118.1(7) . . ? C19 C18 C16 124.8(6) . . ? C23 C18 C16 117.1(6) . . ? C18 C19 C20 120.8(7) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C21 C20 C19 121.9(7) . . ? C21 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? C20 C21 C22 118.4(8) . . ? C20 C21 H21 120.8 . . ? C22 C21 H21 120.8 . . ? C21 C22 C23 121.3(8) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C22 C23 C18 119.5(7) . . ? C22 C23 H23 120.3 . . ? C18 C23 H23 120.3 . . ? N31 Rh31 C31 110.5(3) . . ? N31 Rh31 C32 93.6(3) . . ? C31 Rh31 C32 39.2(3) . . ? N31 Rh31 C33 113.6(3) . . ? C31 Rh31 C33 64.7(3) . . ? C32 Rh31 C33 38.5(3) . . ? N31 Rh31 C35 148.7(3) . . ? C31 Rh31 C35 38.6(3) . . ? C32 Rh31 C35 64.8(3) . . ? C33 Rh31 C35 63.9(3) . . ? N31 Rh31 C34 152.2(2) . . ? C31 Rh31 C34 63.6(3) . . ? C32 Rh31 C34 64.3(3) . . ? C33 Rh31 C34 38.6(3) . . ? C35 Rh31 C34 37.0(3) . . ? N31 Rh31 N32 76.3(2) . . ? C31 Rh31 N32 170.1(3) . . ? C32 Rh31 N32 135.6(2) . . ? C33 Rh31 N32 106.3(2) . . ? C35 Rh31 N32 135.0(3) . . ? C34 Rh31 N32 106.9(2) . . ? N31 Rh31 Cl31 88.25(14) . . ? C31 Rh31 Cl31 101.13(19) . . ? C32 Rh31 Cl31 137.6(2) . . ? C33 Rh31 Cl31 156.7(2) . . ? C35 Rh31 Cl31 93.3(2) . . ? C34 Rh31 Cl31 119.3(2) . . ? N32 Rh31 Cl31 85.95(14) . . ? C44 N31 C41 106.1(6) . . ? C44 N31 Rh31 114.4(4) . . ? C41 N31 Rh31 139.5(5) . . ? C45 N32 C46 116.6(6) . . ? C45 N32 Rh31 113.4(5) . . ? C46 N32 Rh31 129.1(4) . . ? C44 N33 C42 107.0(6) . . ? C44 N33 C43 125.6(6) . . ? C42 N33 C43 127.2(6) . . ? C35 C31 C32 108.2(7) . . ? C35 C31 C36 126.3(7) . . ? C32 C31 C36 125.4(8) . . ? C35 C31 Rh31 72.1(4) . . ? C32 C31 Rh31 71.4(4) . . ? C36 C31 Rh31 123.9(5) . . ? C33 C32 C31 106.7(7) . . ? C33 C32 C37 125.2(7) . . ? C31 C32 C37 128.1(8) . . ? C33 C32 Rh31 70.8(4) . . ? C31 C32 Rh31 69.4(4) . . ? C37 C32 Rh31 126.6(5) . . ? C32 C33 C34 108.1(7) . . ? C32 C33 C38 125.5(8) . . ? C34 C33 C38 125.9(8) . . ? C32 C33 Rh31 70.7(4) . . ? C34 C33 Rh31 72.3(4) . . ? C38 C33 Rh31 128.8(5) . . ? C35 C34 C33 108.1(7) . . ? C35 C34 C39 127.3(8) . . ? C33 C34 C39 124.2(8) . . ? C35 C34 Rh31 70.2(4) . . ? C33 C34 Rh31 69.1(4) . . ? C39 C34 Rh31 131.8(5) . . ? C34 C35 C31 108.9(6) . . ? C34 C35 C40 127.8(8) . . ? C31 C35 C40 123.2(8) . . ? C34 C35 Rh31 72.8(4) . . ? C31 C35 Rh31 69.3(4) . . ? C40 C35 Rh31 126.5(5) . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C35 C40 H40A 109.5 . . ? C35 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C35 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 N31 108.5(7) . . ? C42 C41 H41 125.8 . . ? N31 C41 H41 125.8 . . ? C41 C42 N33 107.2(7) . . ? C41 C42 H42 126.4 . . ? N33 C42 H42 126.4 . . ? N33 C43 H43A 109.5 . . ? N33 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N33 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N31 C44 N33 111.2(6) . . ? N31 C44 C45 117.9(6) . . ? N33 C44 C45 131.0(6) . . ? N32 C45 C44 117.8(6) . . ? N32 C45 H45 121.1 . . ? C44 C45 H45 121.1 . . ? N32 C46 C47 110.1(6) . . ? N32 C46 C48 109.2(5) . . ? C47 C46 C48 115.2(7) . . ? N32 C46 H46 111(5) . . ? C47 C46 H46 106(5) . . ? C48 C46 H46 105(5) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C53 C48 C49 119.7(7) . . ? C53 C48 C46 121.1(8) . . ? C49 C48 C46 118.9(7) . . ? C48 C49 C50 120.6(9) . . ? C48 C49 H49 119.7 . . ? C50 C49 H49 119.7 . . ? C51 C50 C49 119.4(10) . . ? C51 C50 H50 120.3 . . ? C49 C50 H50 120.3 . . ? C50 C51 C52 119.7(8) . . ? C50 C51 H51 120.1 . . ? C52 C51 H51 120.1 . . ? C53 C52 C51 119.6(10) . . ? C53 C52 H52 120.2 . . ? C51 C52 H52 120.2 . . ? C48 C53 C52 120.9(10) . . ? C48 C53 H53 119.6 . . ? C52 C53 H53 119.6 . . ? F3A Sb1 F6A 97.2(5) . . ? F3A Sb1 F2 88.9(4) . . ? F6A Sb1 F2 88.7(4) . . ? F3A Sb1 F1 90.7(4) . . ? F6A Sb1 F1 89.9(4) . . ? F2 Sb1 F1 178.5(4) . . ? F3A Sb1 F5B 103.5(8) . . ? F6A Sb1 F5B 157.5(8) . . ? F2 Sb1 F5B 100.4(8) . . ? F1 Sb1 F5B 81.1(9) . . ? F3A Sb1 F4B 155.1(7) . . ? F6A Sb1 F4B 59.0(7) . . ? F2 Sb1 F4B 97.2(7) . . ? F1 Sb1 F4B 82.6(7) . . ? F5B Sb1 F4B 99.2(9) . . ? F3A Sb1 F3B 17.5(5) . . ? F6A Sb1 F3B 113.3(5) . . ? F2 Sb1 F3B 95.8(5) . . ? F1 Sb1 F3B 84.2(5) . . ? F5B Sb1 F3B 86.4(8) . . ? F4B Sb1 F3B 164.6(8) . . ? F3A Sb1 F6B 73.1(6) . . ? F6A Sb1 F6B 24.3(5) . . ? F2 Sb1 F6B 91.4(6) . . ? F1 Sb1 F6B 87.1(7) . . ? F5B Sb1 F6B 167.8(10) . . ? F4B Sb1 F6B 82.5(8) . . ? F3B Sb1 F6B 89.1(7) . . ? F3A Sb1 F4A 173.8(4) . . ? F6A Sb1 F4A 87.6(4) . . ? F2 Sb1 F4A 87.3(3) . . ? F1 Sb1 F4A 93.2(3) . . ? F5B Sb1 F4A 72.5(8) . . ? F4B Sb1 F4A 30.7(6) . . ? F3B Sb1 F4A 158.9(5) . . ? F6B Sb1 F4A 111.8(6) . . ? F3A Sb1 F5A 91.4(5) . . ? F6A Sb1 F5A 168.6(5) . . ? F2 Sb1 F5A 83.9(4) . . ? F1 Sb1 F5A 97.5(5) . . ? F5B Sb1 F5A 20.4(8) . . ? F4B Sb1 F5A 113.3(7) . . ? F3B Sb1 F5A 76.2(5) . . ? F6B Sb1 F5A 163.9(6) . . ? F4A Sb1 F5A 83.4(4) . . ? F3B F3A Sb1 86.3(12) . . ? F4B F4A Sb1 72.8(7) . . ? F5B F5A Sb1 74.1(11) . . ? F6B F6A Sb1 83.3(9) . . ? F3A F3B Sb1 76.2(11) . . ? F4A F4B Sb1 76.5(7) . . ? F5A F5B Sb1 85.6(12) . . ? F6A F6B Sb1 72.4(8) . . ? F12A Sb2 F11A 162.2(7) . . ? F12A Sb2 F9B 103.2(5) . . ? F11A Sb2 F9B 93.8(7) . . ? F12A Sb2 F10A 92.1(5) . . ? F11A Sb2 F10A 70.9(8) . . ? F9B Sb2 F10A 164.7(6) . . ? F12A Sb2 F8 81.6(5) . . ? F11A Sb2 F8 92.3(6) . . ? F9B Sb2 F8 93.3(5) . . ? F10A Sb2 F8 88.6(5) . . ? F12A Sb2 F7 96.8(4) . . ? F11A Sb2 F7 89.4(5) . . ? F9B Sb2 F7 86.6(5) . . ? F10A Sb2 F7 92.0(5) . . ? F8 Sb2 F7 178.3(4) . . ? F12A Sb2 F10B 63.0(5) . . ? F11A Sb2 F10B 100.6(8) . . ? F9B Sb2 F10B 164.7(6) . . ? F10A Sb2 F10B 30.0(5) . . ? F8 Sb2 F10B 91.1(5) . . ? F7 Sb2 F10B 88.5(5) . . ? F12A Sb2 F9A 93.7(6) . . ? F11A Sb2 F9A 102.5(8) . . ? F9B Sb2 F9A 11.7(7) . . ? F10A Sb2 F9A 170.8(7) . . ? F8 Sb2 F9A 85.2(7) . . ? F7 Sb2 F9A 94.5(6) . . ? F10B Sb2 F9A 156.7(6) . . ? F12A Sb2 F11B 173.3(5) . . ? F11A Sb2 F11B 17.6(5) . . ? F9B Sb2 F11B 76.3(6) . . ? F10A Sb2 F11B 88.5(7) . . ? F8 Sb2 F11B 91.7(5) . . ? F7 Sb2 F11B 89.9(4) . . ? F10B Sb2 F11B 118.3(7) . . ? F9A Sb2 F11B 84.9(7) . . ? F12A Sb2 F12B 22.1(4) . . ? F11A Sb2 F12B 173.8(7) . . ? F9B Sb2 F12B 84.1(6) . . ? F10A Sb2 F12B 111.0(6) . . ? F8 Sb2 F12B 93.7(6) . . ? F7 Sb2 F12B 84.7(5) . . ? F10B Sb2 F12B 81.0(6) . . ? F9A Sb2 F12B 76.3(6) . . ? F11B Sb2 F12B 159.9(7) . . ? F10B F10A Sb2 75.5(7) . . ? F11B F11A Sb2 89.7(13) . . ? F12B F12A Sb2 88.5(10) . . ? F10A F10B Sb2 74.5(7) . . ? F11A F11B Sb2 72.7(12) . . ? F12A F12B Sb2 69.4(9) . . ? C62A O1A C60A 111.9(10) . . ? O1A C60A C61A 105.5(10) . . ? O1A C60A H60A 110.6 . . ? C61A C60A H60A 110.6 . . ? O1A C60A H60B 110.6 . . ? C61A C60A H60B 110.6 . . ? H60A C60A H60B 108.8 . . ? C60A C61A H61A 109.5 . . ? C60A C61A H61B 109.5 . . ? H61A C61A H61B 109.5 . . ? C60A C61A H61C 109.5 . . ? H61A C61A H61C 109.5 . . ? H61B C61A H61C 109.5 . . ? O1A C62A C63 137.7(11) . . ? O1A C62A H62A 102.7 . . ? C63 C62A H62A 102.7 . . ? O1A C62A H62B 102.7 . . ? C63 C62A H62B 102.7 . . ? H62A C62A H62B 105.0 . . ? C60B O1B C62B 120.3(14) . . ? O1B C60B C61B 115.8(17) . . ? O1B C60B H60C 108.3 . . ? C61B C60B H60C 108.3 . . ? O1B C60B H60D 108.3 . . ? C61B C60B H60D 108.3 . . ? H60C C60B H60D 107.4 . . ? C60B C61B H61D 109.5 . . ? C60B C61B H61E 109.5 . . ? H61D C61B H61E 109.5 . . ? C60B C61B H61F 109.5 . . ? H61D C61B H61F 109.5 . . ? H61E C61B H61F 109.5 . . ? O1B C62B C63 104.8(11) . . ? O1B C62B H62C 110.8 . . ? C63 C62B H62C 110.8 . . ? O1B C62B H62D 110.8 . . ? C63 C62B H62D 110.8 . . ? H62C C62B H62D 108.9 . . ? C62B C63 H63A 130.7 . . ? C62A C63 H63A 109.5 . . ? C62B C63 H63B 115.8 . . ? C62A C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62B C63 H63C 73.0 . . ? C62A C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C62B C63 H63D 112.4 . . ? C62A C63 H63D 148.3 . . ? H63A C63 H63D 84.0 . . ? H63B C63 H63D 91.5 . . ? C62B C63 H63E 108.5 . . ? C62A C63 H63E 81.9 . . ? H63B C63 H63E 118.0 . . ? H63C C63 H63E 123.8 . . ? H63D C63 H63E 109.5 . . ? C62B C63 H63F 107.4 . . ? C62A C63 H63F 93.2 . . ? H63A C63 H63F 109.8 . . ? H63C C63 H63F 123.9 . . ? H63D C63 H63F 109.5 . . ? H63E C63 H63F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Rh1 N1 C14 0.7(4) . . . . ? C4 Rh1 N1 C14 171.9(4) . . . . ? C2 Rh1 N1 C14 99.3(5) . . . . ? C3 Rh1 N1 C14 133.4(4) . . . . ? C1 Rh1 N1 C14 99.4(7) . . . . ? C5 Rh1 N1 C14 -176.0(4) . . . . ? Cl1 Rh1 N1 C14 -82.2(4) . . . . ? N2 Rh1 N1 C11 179.6(7) . . . . ? C4 Rh1 N1 C11 -9.3(7) . . . . ? C2 Rh1 N1 C11 -81.8(7) . . . . ? C3 Rh1 N1 C11 -47.7(7) . . . . ? C1 Rh1 N1 C11 -81.7(9) . . . . ? C5 Rh1 N1 C11 2.9(9) . . . . ? Cl1 Rh1 N1 C11 96.7(6) . . . . ? N1 Rh1 N2 C15 -3.8(4) . . . . ? C4 Rh1 N2 C15 -129.3(12) . . . . ? C2 Rh1 N2 C15 -119.1(5) . . . . ? C3 Rh1 N2 C15 -89.2(5) . . . . ? C1 Rh1 N2 C15 -159.4(5) . . . . ? C5 Rh1 N2 C15 173.6(4) . . . . ? Cl1 Rh1 N2 C15 87.4(4) . . . . ? N1 Rh1 N2 C16 -172.6(5) . . . . ? C4 Rh1 N2 C16 61.9(14) . . . . ? C2 Rh1 N2 C16 72.2(5) . . . . ? C3 Rh1 N2 C16 102.1(5) . . . . ? C1 Rh1 N2 C16 31.9(5) . . . . ? C5 Rh1 N2 C16 4.9(6) . . . . ? Cl1 Rh1 N2 C16 -81.4(4) . . . . ? N1 Rh1 C1 C5 118.4(6) . . . . ? N2 Rh1 C1 C5 -148.9(4) . . . . ? C4 Rh1 C1 C5 36.7(4) . . . . ? C2 Rh1 C1 C5 118.5(6) . . . . ? C3 Rh1 C1 C5 80.6(4) . . . . ? Cl1 Rh1 C1 C5 -59.9(4) . . . . ? N1 Rh1 C1 C2 -0.1(9) . . . . ? N2 Rh1 C1 C2 92.5(4) . . . . ? C4 Rh1 C1 C2 -81.8(5) . . . . ? C3 Rh1 C1 C2 -38.0(4) . . . . ? C5 Rh1 C1 C2 -118.5(6) . . . . ? Cl1 Rh1 C1 C2 -178.4(4) . . . . ? N1 Rh1 C1 C6 -121.1(9) . . . . ? N2 Rh1 C1 C6 -28.5(9) . . . . ? C4 Rh1 C1 C6 157.2(9) . . . . ? C2 Rh1 C1 C6 -121.0(10) . . . . ? C3 Rh1 C1 C6 -159.0(10) . . . . ? C5 Rh1 C1 C6 120.4(10) . . . . ? Cl1 Rh1 C1 C6 60.6(9) . . . . ? C5 C1 C2 C3 -0.5(7) . . . . ? C6 C1 C2 C3 -177.0(7) . . . . ? Rh1 C1 C2 C3 61.2(4) . . . . ? C5 C1 C2 C7 177.1(6) . . . . ? C6 C1 C2 C7 0.6(11) . . . . ? Rh1 C1 C2 C7 -121.2(7) . . . . ? C5 C1 C2 Rh1 -61.7(5) . . . . ? C6 C1 C2 Rh1 121.8(7) . . . . ? N1 Rh1 C2 C3 62.3(4) . . . . ? N2 Rh1 C2 C3 144.5(4) . . . . ? C4 Rh1 C2 C3 -37.5(4) . . . . ? C1 Rh1 C2 C3 -117.7(6) . . . . ? C5 Rh1 C2 C3 -81.0(4) . . . . ? Cl1 Rh1 C2 C3 -114.5(5) . . . . ? N1 Rh1 C2 C1 179.9(4) . . . . ? N2 Rh1 C2 C1 -97.8(4) . . . . ? C4 Rh1 C2 C1 80.2(4) . . . . ? C3 Rh1 C2 C1 117.7(6) . . . . ? C5 Rh1 C2 C1 36.7(4) . . . . ? Cl1 Rh1 C2 C1 3.2(8) . . . . ? N1 Rh1 C2 C7 -60.1(9) . . . . ? N2 Rh1 C2 C7 22.2(9) . . . . ? C4 Rh1 C2 C7 -159.8(10) . . . . ? C3 Rh1 C2 C7 -122.3(10) . . . . ? C1 Rh1 C2 C7 120.0(11) . . . . ? C5 Rh1 C2 C7 156.7(10) . . . . ? Cl1 Rh1 C2 C7 123.2(8) . . . . ? C1 C2 C3 C4 -2.0(7) . . . . ? C7 C2 C3 C4 -179.5(7) . . . . ? Rh1 C2 C3 C4 59.6(4) . . . . ? C1 C2 C3 C8 178.0(6) . . . . ? C7 C2 C3 C8 0.5(11) . . . . ? Rh1 C2 C3 C8 -120.4(7) . . . . ? C1 C2 C3 Rh1 -61.6(4) . . . . ? C7 C2 C3 Rh1 120.9(7) . . . . ? N1 Rh1 C3 C2 -127.7(4) . . . . ? N2 Rh1 C3 C2 -50.3(5) . . . . ? C4 Rh1 C3 C2 119.3(6) . . . . ? C1 Rh1 C3 C2 37.9(4) . . . . ? C5 Rh1 C3 C2 79.8(4) . . . . ? Cl1 Rh1 C3 C2 135.6(4) . . . . ? N1 Rh1 C3 C4 113.0(4) . . . . ? N2 Rh1 C3 C4 -169.6(4) . . . . ? C2 Rh1 C3 C4 -119.3(6) . . . . ? C1 Rh1 C3 C4 -81.4(5) . . . . ? C5 Rh1 C3 C4 -39.5(4) . . . . ? Cl1 Rh1 C3 C4 16.3(6) . . . . ? N1 Rh1 C3 C8 -7.0(8) . . . . ? N2 Rh1 C3 C8 70.4(9) . . . . ? C4 Rh1 C3 C8 -119.9(10) . . . . ? C2 Rh1 C3 C8 120.7(9) . . . . ? C1 Rh1 C3 C8 158.6(9) . . . . ? C5 Rh1 C3 C8 -159.4(9) . . . . ? Cl1 Rh1 C3 C8 -103.6(7) . . . . ? C2 C3 C4 C5 3.6(7) . . . . ? C8 C3 C4 C5 -176.4(6) . . . . ? Rh1 C3 C4 C5 63.7(4) . . . . ? C2 C3 C4 C9 177.8(7) . . . . ? C8 C3 C4 C9 -2.2(11) . . . . ? Rh1 C3 C4 C9 -122.2(7) . . . . ? C2 C3 C4 Rh1 -60.0(4) . . . . ? C8 C3 C4 Rh1 120.0(7) . . . . ? N1 Rh1 C4 C3 -75.4(5) . . . . ? N2 Rh1 C4 C3 47.7(14) . . . . ? C2 Rh1 C4 C3 36.9(5) . . . . ? C1 Rh1 C4 C3 79.7(5) . . . . ? C5 Rh1 C4 C3 115.0(6) . . . . ? Cl1 Rh1 C4 C3 -170.2(4) . . . . ? N1 Rh1 C4 C5 169.7(4) . . . . ? N2 Rh1 C4 C5 -67.2(13) . . . . ? C2 Rh1 C4 C5 -78.1(4) . . . . ? C3 Rh1 C4 C5 -115.0(6) . . . . ? C1 Rh1 C4 C5 -35.3(4) . . . . ? Cl1 Rh1 C4 C5 74.9(4) . . . . ? N1 Rh1 C4 C9 48.2(7) . . . . ? N2 Rh1 C4 C9 171.3(11) . . . . ? C2 Rh1 C4 C9 160.4(7) . . . . ? C3 Rh1 C4 C9 123.6(8) . . . . ? C1 Rh1 C4 C9 -156.7(7) . . . . ? C5 Rh1 C4 C9 -121.5(8) . . . . ? Cl1 Rh1 C4 C9 -46.6(7) . . . . ? C2 C1 C5 C4 2.8(7) . . . . ? C6 C1 C5 C4 179.4(7) . . . . ? Rh1 C1 C5 C4 -57.7(4) . . . . ? C2 C1 C5 C10 -178.0(6) . . . . ? C6 C1 C5 C10 -1.4(11) . . . . ? Rh1 C1 C5 C10 121.5(7) . . . . ? C2 C1 C5 Rh1 60.5(5) . . . . ? C6 C1 C5 Rh1 -122.9(7) . . . . ? C3 C4 C5 C1 -4.0(7) . . . . ? C9 C4 C5 C1 -178.3(7) . . . . ? Rh1 C4 C5 C1 58.7(4) . . . . ? C3 C4 C5 C10 176.8(6) . . . . ? C9 C4 C5 C10 2.4(10) . . . . ? Rh1 C4 C5 C10 -120.5(6) . . . . ? C3 C4 C5 Rh1 -62.7(4) . . . . ? C9 C4 C5 Rh1 122.9(7) . . . . ? N1 Rh1 C5 C1 -139.1(5) . . . . ? N2 Rh1 C5 C1 45.5(5) . . . . ? C4 Rh1 C5 C1 -120.9(6) . . . . ? C2 Rh1 C5 C1 -37.7(5) . . . . ? C3 Rh1 C5 C1 -81.1(5) . . . . ? Cl1 Rh1 C5 C1 127.9(4) . . . . ? N1 Rh1 C5 C4 -18.2(6) . . . . ? N2 Rh1 C5 C4 166.4(3) . . . . ? C2 Rh1 C5 C4 83.2(4) . . . . ? C3 Rh1 C5 C4 39.8(4) . . . . ? C1 Rh1 C5 C4 120.9(6) . . . . ? Cl1 Rh1 C5 C4 -111.2(3) . . . . ? N1 Rh1 C5 C10 97.5(8) . . . . ? N2 Rh1 C5 C10 -78.0(8) . . . . ? C4 Rh1 C5 C10 115.7(9) . . . . ? C2 Rh1 C5 C10 -161.1(8) . . . . ? C3 Rh1 C5 C10 155.4(8) . . . . ? C1 Rh1 C5 C10 -123.4(9) . . . . ? Cl1 Rh1 C5 C10 4.5(7) . . . . ? C14 N1 C11 C12 0.4(7) . . . . ? Rh1 N1 C11 C12 -178.5(5) . . . . ? C14 N3 C12 C11 -1.0(7) . . . . ? C13 N3 C12 C11 -175.2(6) . . . . ? N1 C11 C12 N3 0.4(7) . . . . ? C11 N1 C14 N3 -1.0(7) . . . . ? Rh1 N1 C14 N3 178.3(4) . . . . ? C11 N1 C14 C15 -177.0(5) . . . . ? Rh1 N1 C14 C15 2.3(7) . . . . ? C12 N3 C14 N1 1.2(7) . . . . ? C13 N3 C14 N1 175.4(6) . . . . ? C12 N3 C14 C15 176.7(6) . . . . ? C13 N3 C14 C15 -9.2(11) . . . . ? C16 N2 C15 C14 175.3(5) . . . . ? Rh1 N2 C15 C14 6.1(7) . . . . ? N1 C14 C15 N2 -5.7(8) . . . . ? N3 C14 C15 N2 179.2(6) . . . . ? C15 N2 C16 C18 87.0(7) . . . . ? Rh1 N2 C16 C18 -104.7(5) . . . . ? C15 N2 C16 C17 -39.4(8) . . . . ? Rh1 N2 C16 C17 128.9(5) . . . . ? N2 C16 C18 C19 -28.1(9) . . . . ? C17 C16 C18 C19 98.4(8) . . . . ? N2 C16 C18 C23 152.4(6) . . . . ? C17 C16 C18 C23 -81.1(8) . . . . ? C23 C18 C19 C20 1.5(11) . . . . ? C16 C18 C19 C20 -178.0(6) . . . . ? C18 C19 C20 C21 -1.6(12) . . . . ? C19 C20 C21 C22 1.1(12) . . . . ? C20 C21 C22 C23 -0.5(12) . . . . ? C21 C22 C23 C18 0.5(11) . . . . ? C19 C18 C23 C22 -1.0(10) . . . . ? C16 C18 C23 C22 178.6(6) . . . . ? C31 Rh31 N31 C44 -173.8(4) . . . . ? C32 Rh31 N31 C44 -137.5(5) . . . . ? C33 Rh31 N31 C44 -103.4(5) . . . . ? C35 Rh31 N31 C44 178.4(5) . . . . ? C34 Rh31 N31 C44 -101.8(6) . . . . ? N32 Rh31 N31 C44 -1.3(4) . . . . ? Cl31 Rh31 N31 C44 84.9(4) . . . . ? C31 Rh31 N31 C41 8.4(7) . . . . ? C32 Rh31 N31 C41 44.8(7) . . . . ? C33 Rh31 N31 C41 78.8(7) . . . . ? C35 Rh31 N31 C41 0.7(9) . . . . ? C34 Rh31 N31 C41 80.5(9) . . . . ? N32 Rh31 N31 C41 -179.1(7) . . . . ? Cl31 Rh31 N31 C41 -92.8(7) . . . . ? N31 Rh31 N32 C45 3.7(4) . . . . ? C32 Rh31 N32 C45 84.7(6) . . . . ? C33 Rh31 N32 C45 114.7(5) . . . . ? C35 Rh31 N32 C45 -176.1(5) . . . . ? C34 Rh31 N32 C45 155.1(4) . . . . ? Cl31 Rh31 N32 C45 -85.5(4) . . . . ? N31 Rh31 N32 C46 172.5(5) . . . . ? C32 Rh31 N32 C46 -106.5(6) . . . . ? C33 Rh31 N32 C46 -76.5(6) . . . . ? C35 Rh31 N32 C46 -7.3(7) . . . . ? C34 Rh31 N32 C46 -36.1(6) . . . . ? Cl31 Rh31 N32 C46 83.3(5) . . . . ? N31 Rh31 C31 C35 -173.6(4) . . . . ? C32 Rh31 C31 C35 117.1(7) . . . . ? C33 Rh31 C31 C35 79.3(5) . . . . ? C34 Rh31 C31 C35 36.1(5) . . . . ? Cl31 Rh31 C31 C35 -81.2(4) . . . . ? N31 Rh31 C31 C32 69.4(5) . . . . ? C33 Rh31 C31 C32 -37.8(5) . . . . ? C35 Rh31 C31 C32 -117.1(7) . . . . ? C34 Rh31 C31 C32 -81.0(5) . . . . ? Cl31 Rh31 C31 C32 161.7(4) . . . . ? N31 Rh31 C31 C36 -51.3(7) . . . . ? C32 Rh31 C31 C36 -120.7(9) . . . . ? C33 Rh31 C31 C36 -158.5(8) . . . . ? C35 Rh31 C31 C36 122.2(8) . . . . ? C34 Rh31 C31 C36 158.3(8) . . . . ? Cl31 Rh31 C31 C36 41.0(7) . . . . ? C35 C31 C32 C33 -1.7(7) . . . . ? C36 C31 C32 C33 -179.8(6) . . . . ? Rh31 C31 C32 C33 61.4(4) . . . . ? C35 C31 C32 C37 176.0(7) . . . . ? C36 C31 C32 C37 -2.1(11) . . . . ? Rh31 C31 C32 C37 -120.9(7) . . . . ? C35 C31 C32 Rh31 -63.1(5) . . . . ? C36 C31 C32 Rh31 118.8(7) . . . . ? N31 Rh31 C32 C33 124.4(4) . . . . ? C31 Rh31 C32 C33 -117.1(7) . . . . ? C35 Rh31 C32 C33 -79.2(5) . . . . ? C34 Rh31 C32 C33 -38.0(4) . . . . ? N32 Rh31 C32 C33 50.3(6) . . . . ? Cl31 Rh31 C32 C33 -144.3(4) . . . . ? N31 Rh31 C32 C31 -118.6(5) . . . . ? C33 Rh31 C32 C31 117.1(7) . . . . ? C35 Rh31 C32 C31 37.9(5) . . . . ? C34 Rh31 C32 C31 79.0(5) . . . . ? N32 Rh31 C32 C31 167.3(4) . . . . ? Cl31 Rh31 C32 C31 -27.2(6) . . . . ? N31 Rh31 C32 C37 4.3(8) . . . . ? C31 Rh31 C32 C37 122.8(10) . . . . ? C33 Rh31 C32 C37 -120.1(9) . . . . ? C35 Rh31 C32 C37 160.7(9) . . . . ? C34 Rh31 C32 C37 -158.2(9) . . . . ? N32 Rh31 C32 C37 -69.8(9) . . . . ? Cl31 Rh31 C32 C37 95.6(7) . . . . ? C31 C32 C33 C34 2.5(7) . . . . ? C37 C32 C33 C34 -175.3(6) . . . . ? Rh31 C32 C33 C34 63.0(4) . . . . ? C31 C32 C33 C38 175.0(6) . . . . ? C37 C32 C33 C38 -2.7(11) . . . . ? Rh31 C32 C33 C38 -124.5(7) . . . . ? C31 C32 C33 Rh31 -60.5(4) . . . . ? C37 C32 C33 Rh31 121.7(7) . . . . ? N31 Rh31 C33 C32 -64.0(4) . . . . ? C31 Rh31 C33 C32 38.5(4) . . . . ? C35 Rh31 C33 C32 81.5(5) . . . . ? C34 Rh31 C33 C32 117.2(6) . . . . ? N32 Rh31 C33 C32 -145.9(4) . . . . ? Cl31 Rh31 C33 C32 94.4(7) . . . . ? N31 Rh31 C33 C34 178.8(4) . . . . ? C31 Rh31 C33 C34 -78.8(5) . . . . ? C32 Rh31 C33 C34 -117.2(6) . . . . ? C35 Rh31 C33 C34 -35.7(5) . . . . ? N32 Rh31 C33 C34 96.9(4) . . . . ? Cl31 Rh31 C33 C34 -22.8(8) . . . . ? N31 Rh31 C33 C38 56.6(9) . . . . ? C31 Rh31 C33 C38 159.1(9) . . . . ? C32 Rh31 C33 C38 120.6(10) . . . . ? C35 Rh31 C33 C38 -157.9(10) . . . . ? C34 Rh31 C33 C38 -122.2(10) . . . . ? N32 Rh31 C33 C38 -25.3(9) . . . . ? Cl31 Rh31 C33 C38 -145.0(6) . . . . ? C32 C33 C34 C35 -2.4(8) . . . . ? C38 C33 C34 C35 -174.9(7) . . . . ? Rh31 C33 C34 C35 59.6(5) . . . . ? C32 C33 C34 C39 170.9(7) . . . . ? C38 C33 C34 C39 -1.6(11) . . . . ? Rh31 C33 C34 C39 -127.1(7) . . . . ? C32 C33 C34 Rh31 -62.0(5) . . . . ? C38 C33 C34 Rh31 125.5(7) . . . . ? N31 Rh31 C34 C35 -121.8(6) . . . . ? C31 Rh31 C34 C35 -37.7(4) . . . . ? C32 Rh31 C34 C35 -81.5(5) . . . . ? C33 Rh31 C34 C35 -119.4(7) . . . . ? N32 Rh31 C34 C35 145.5(4) . . . . ? Cl31 Rh31 C34 C35 50.5(5) . . . . ? N31 Rh31 C34 C33 -2.4(8) . . . . ? C31 Rh31 C34 C33 81.7(5) . . . . ? C32 Rh31 C34 C33 37.9(4) . . . . ? C35 Rh31 C34 C33 119.4(7) . . . . ? N32 Rh31 C34 C33 -95.2(4) . . . . ? Cl31 Rh31 C34 C33 169.9(4) . . . . ? N31 Rh31 C34 C39 115.4(8) . . . . ? C31 Rh31 C34 C39 -160.6(9) . . . . ? C32 Rh31 C34 C39 155.7(9) . . . . ? C33 Rh31 C34 C39 117.8(10) . . . . ? C35 Rh31 C34 C39 -122.9(10) . . . . ? N32 Rh31 C34 C39 22.6(8) . . . . ? Cl31 Rh31 C34 C39 -72.4(8) . . . . ? C33 C34 C35 C31 1.3(8) . . . . ? C39 C34 C35 C31 -171.7(7) . . . . ? Rh31 C34 C35 C31 60.2(5) . . . . ? C33 C34 C35 C40 177.8(7) . . . . ? C39 C34 C35 C40 4.8(13) . . . . ? Rh31 C34 C35 C40 -123.3(8) . . . . ? C33 C34 C35 Rh31 -58.9(5) . . . . ? C39 C34 C35 Rh31 128.1(8) . . . . ? C32 C31 C35 C34 0.3(8) . . . . ? C36 C31 C35 C34 178.3(7) . . . . ? Rh31 C31 C35 C34 -62.4(5) . . . . ? C32 C31 C35 C40 -176.4(6) . . . . ? C36 C31 C35 C40 1.6(11) . . . . ? Rh31 C31 C35 C40 120.9(7) . . . . ? C32 C31 C35 Rh31 62.7(4) . . . . ? C36 C31 C35 Rh31 -119.3(7) . . . . ? N31 Rh31 C35 C34 130.3(5) . . . . ? C31 Rh31 C35 C34 118.6(6) . . . . ? C32 Rh31 C35 C34 80.2(5) . . . . ? C33 Rh31 C35 C34 37.3(5) . . . . ? N32 Rh31 C35 C34 -50.1(6) . . . . ? Cl31 Rh31 C35 C34 -137.6(4) . . . . ? N31 Rh31 C35 C31 11.7(7) . . . . ? C32 Rh31 C35 C31 -38.4(4) . . . . ? C33 Rh31 C35 C31 -81.3(5) . . . . ? C34 Rh31 C35 C31 -118.6(6) . . . . ? N32 Rh31 C35 C31 -168.7(4) . . . . ? Cl31 Rh31 C35 C31 103.7(4) . . . . ? N31 Rh31 C35 C40 -105.0(8) . . . . ? C31 Rh31 C35 C40 -116.7(10) . . . . ? C32 Rh31 C35 C40 -155.1(9) . . . . ? C33 Rh31 C35 C40 162.0(9) . . . . ? C34 Rh31 C35 C40 124.7(10) . . . . ? N32 Rh31 C35 C40 74.6(9) . . . . ? Cl31 Rh31 C35 C40 -13.0(8) . . . . ? C44 N31 C41 C42 1.3(7) . . . . ? Rh31 N31 C41 C42 179.2(5) . . . . ? N31 C41 C42 N33 -1.0(8) . . . . ? C44 N33 C42 C41 0.3(8) . . . . ? C43 N33 C42 C41 176.0(6) . . . . ? C41 N31 C44 N33 -1.1(7) . . . . ? Rh31 N31 C44 N33 -179.6(4) . . . . ? C41 N31 C44 C45 177.5(5) . . . . ? Rh31 N31 C44 C45 -0.9(7) . . . . ? C42 N33 C44 N31 0.5(7) . . . . ? C43 N33 C44 N31 -175.2(6) . . . . ? C42 N33 C44 C45 -177.9(6) . . . . ? C43 N33 C44 C45 6.3(11) . . . . ? C46 N32 C45 C44 -175.7(5) . . . . ? Rh31 N32 C45 C44 -5.4(7) . . . . ? N31 C44 C45 N32 4.4(8) . . . . ? N33 C44 C45 N32 -177.2(6) . . . . ? C45 N32 C46 C47 130.3(6) . . . . ? Rh31 N32 C46 C47 -38.2(8) . . . . ? C45 N32 C46 C48 -102.2(7) . . . . ? Rh31 N32 C46 C48 89.3(7) . . . . ? N32 C46 C48 C53 -142.2(7) . . . . ? C47 C46 C48 C53 -17.7(10) . . . . ? N32 C46 C48 C49 44.5(9) . . . . ? C47 C46 C48 C49 169.0(6) . . . . ? C53 C48 C49 C50 1.3(11) . . . . ? C46 C48 C49 C50 174.6(7) . . . . ? C48 C49 C50 C51 -1.5(12) . . . . ? C49 C50 C51 C52 1.5(13) . . . . ? C50 C51 C52 C53 -1.1(14) . . . . ? C49 C48 C53 C52 -0.9(12) . . . . ? C46 C48 C53 C52 -174.2(7) . . . . ? C51 C52 C53 C48 0.8(13) . . . . ? F6A Sb1 F3A F3B -158(2) . . . . ? F2 Sb1 F3A F3B 114(2) . . . . ? F1 Sb1 F3A F3B -68(2) . . . . ? F5B Sb1 F3A F3B 13(2) . . . . ? F4B Sb1 F3A F3B -142(2) . . . . ? F6B Sb1 F3A F3B -155(2) . . . . ? F5A Sb1 F3A F3B 30(2) . . . . ? F6A Sb1 F4A F4B 20.2(13) . . . . ? F2 Sb1 F4A F4B 109.0(13) . . . . ? F1 Sb1 F4A F4B -69.6(14) . . . . ? F5B Sb1 F4A F4B -149.2(16) . . . . ? F3B Sb1 F4A F4B -151.7(18) . . . . ? F6B Sb1 F4A F4B 18.6(15) . . . . ? F5A Sb1 F4A F4B -166.8(14) . . . . ? F3A Sb1 F5A F5B -127(3) . . . . ? F6A Sb1 F5A F5B 94(4) . . . . ? F2 Sb1 F5A F5B 144(3) . . . . ? F1 Sb1 F5A F5B -37(3) . . . . ? F4B Sb1 F5A F5B 49(3) . . . . ? F3B Sb1 F5A F5B -119(3) . . . . ? F6B Sb1 F5A F5B -142(3) . . . . ? F4A Sb1 F5A F5B 56(2) . . . . ? F3A Sb1 F6A F6B 7.5(18) . . . . ? F2 Sb1 F6A F6B 96.2(17) . . . . ? F1 Sb1 F6A F6B -83.2(17) . . . . ? F5B Sb1 F6A F6B -149(2) . . . . ? F4B Sb1 F6A F6B -164.6(19) . . . . ? F3B Sb1 F6A F6B 0.4(19) . . . . ? F4A Sb1 F6A F6B -176.4(17) . . . . ? F5A Sb1 F6A F6B 146(3) . . . . ? F6A Sb1 F3B F3A 24(2) . . . . ? F2 Sb1 F3B F3A -67(2) . . . . ? F1 Sb1 F3B F3A 111(2) . . . . ? F5B Sb1 F3B F3A -167(2) . . . . ? F4B Sb1 F3B F3A 81(4) . . . . ? F6B Sb1 F3B F3A 24(2) . . . . ? F4A Sb1 F3B F3A -164.8(14) . . . . ? F5A Sb1 F3B F3A -149(2) . . . . ? F3A Sb1 F4B F4A -175.2(10) . . . . ? F6A Sb1 F4B F4A -156.3(15) . . . . ? F2 Sb1 F4B F4A -72.1(12) . . . . ? F1 Sb1 F4B F4A 109.3(12) . . . . ? F5B Sb1 F4B F4A 29.6(15) . . . . ? F3B Sb1 F4B F4A 140(2) . . . . ? F6B Sb1 F4B F4A -162.6(14) . . . . ? F5A Sb1 F4B F4A 14.3(15) . . . . ? F3A Sb1 F5B F5A 55(3) . . . . ? F6A Sb1 F5B F5A -149.1(18) . . . . ? F2 Sb1 F5B F5A -37(3) . . . . ? F1 Sb1 F5B F5A 143(3) . . . . ? F4B Sb1 F5B F5A -136(2) . . . . ? F3B Sb1 F5B F5A 59(2) . . . . ? F6B Sb1 F5B F5A 127(4) . . . . ? F4A Sb1 F5B F5A -120(3) . . . . ? F3A Sb1 F6B F6A -172.2(18) . . . . ? F2 Sb1 F6B F6A -83.8(16) . . . . ? F1 Sb1 F6B F6A 96.2(16) . . . . ? F5B Sb1 F6B F6A 112(4) . . . . ? F4B Sb1 F6B F6A 13.3(17) . . . . ? F3B Sb1 F6B F6A -179.6(17) . . . . ? F4A Sb1 F6B F6A 3.8(18) . . . . ? F5A Sb1 F6B F6A -156.4(18) . . . . ? F12A Sb2 F10A F10B -13.2(12) . . . . ? F11A Sb2 F10A F10B 172.3(14) . . . . ? F9B Sb2 F10A F10B 167.8(19) . . . . ? F8 Sb2 F10A F10B -94.8(12) . . . . ? F7 Sb2 F10A F10B 83.6(12) . . . . ? F11B Sb2 F10A F10B 173.5(12) . . . . ? F12B Sb2 F10A F10B -1.4(14) . . . . ? F12A Sb2 F11A F11B 157.8(19) . . . . ? F9B Sb2 F11A F11B -5(2) . . . . ? F10A Sb2 F11A F11B 176(3) . . . . ? F8 Sb2 F11A F11B 88(2) . . . . ? F7 Sb2 F11A F11B -92(2) . . . . ? F10B Sb2 F11A F11B 180(2) . . . . ? F11A Sb2 F12A F12B 166.7(19) . . . . ? F9B Sb2 F12A F12B -30.9(16) . . . . ? F10A Sb2 F12A F12B 149.4(15) . . . . ? F8 Sb2 F12A F12B -122.3(15) . . . . ? F7 Sb2 F12A F12B 57.2(15) . . . . ? F10B Sb2 F12A F12B 142.1(17) . . . . ? F9A Sb2 F12A F12B -37.8(16) . . . . ? F12A Sb2 F10B F10A 165.2(14) . . . . ? F11A Sb2 F10B F10A -7.4(13) . . . . ? F9B Sb2 F10B F10A -167.8(19) . . . . ? F8 Sb2 F10B F10A 85.1(12) . . . . ? F7 Sb2 F10B F10A -96.5(12) . . . . ? F9A Sb2 F10B F10A 165.6(18) . . . . ? F11B Sb2 F10B F10A -7.4(14) . . . . ? F12B Sb2 F10B F10A 178.7(13) . . . . ? F9B Sb2 F11B F11A 175(3) . . . . ? F10A Sb2 F11B F11A -4(2) . . . . ? F8 Sb2 F11B F11A -92(2) . . . . ? F7 Sb2 F11B F11A 88(2) . . . . ? F10B Sb2 F11B F11A 0(3) . . . . ? F9A Sb2 F11B F11A -177(3) . . . . ? F12B Sb2 F11B F11A 162(2) . . . . ? F9B Sb2 F12B F12A 149.9(15) . . . . ? F10A Sb2 F12B F12A -33.0(16) . . . . ? F8 Sb2 F12B F12A 56.9(15) . . . . ? F7 Sb2 F12B F12A -123.1(15) . . . . ? F10B Sb2 F12B F12A -33.7(15) . . . . ? F9A Sb2 F12B F12A 141.0(16) . . . . ? F11B Sb2 F12B F12A 162.1(14) . . . . ? C62A O1A C60A C61A -146.9(11) . . . . ? C60A O1A C62A C63 -144.6(16) . . . . ? C62B O1B C60B C61B -170(2) . . . . ? C60B O1B C62B C63 175.0(17) . . . . ? O1B C62B C63 C62A 12.0(11) . . . . ? O1A C62A C63 C62B -47(2) . . . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.315 _refine_diff_density_min -2.050 _refine_diff_density_rms 0.111 _database_code_depnum_ccdc_archive 'CCDC 937402' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_cmpnd_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H30 Cl Ir N3, F6 Sb' _chemical_formula_sum 'C23 H30 Cl F6 Ir N3 Sb' _chemical_formula_weight 811.90 _chemical_absolute_configuration rmad 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21 _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.7614(5) _cell_length_b 19.2349(8) _cell_length_c 12.7525(5) _cell_angle_alpha 90.00 _cell_angle_beta 112.6350(10) _cell_angle_gamma 90.00 _cell_volume 2662.77(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16102 _cell_measurement_theta_min 2.266 _cell_measurement_theta_max 30.137 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.293 _exptl_crystal_size_mid 0.181 _exptl_crystal_size_min 0.103 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.025 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 6.166 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.269 _exptl_absorpt_correction_T_max 0.437 _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS within SAINT+ package, v. 6.45. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX DUO system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 24028 _diffrn_reflns_av_R_equivalents 0.0179 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 30.46 _reflns_number_total 13916 _reflns_number_gt 13362 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_cell_refinement 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_data_reduction 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP program, SHELXTL v6.12, Bruker2000' _computing_publication_material ENCIFER _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Asymmetric untit is composed by two independent Ir-complexes molecules with different metal configuration. Hydrogen atoms of methyl and phenyl groups have been included in the model in calculated positions and refined with a riding model. The rest of the hydrogen atoms have been included in observed positions and refined with an isotropic thermal parameter equal to 1.2 times those of the carbon atoms thay are bounded to. Geometrical restrains have been included in three C-H distances. Higher residual density peaks are located close to the metal atoms. They have no chemical sense. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0355P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.003(3) _refine_ls_number_reflns 13916 _refine_ls_number_parameters 673 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0262 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_ref 0.0583 _refine_ls_wR_factor_gt 0.0578 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL fjl203ds in P2(1) CELL 0.71073 11.7614 19.2349 12.7525 90.000 112.635 90.000 ZERR 4.00 0.0005 0.0008 0.0005 0.000 0.001 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H CL F IR N SB UNIT 92 120 4 24 4 12 4 MERG 2 DFIX 0.96 0.02 C15 H15 C12 H12 C41 H41 FMAP 2 PLAN 25 ACTA 55.00 BOND $H CONF WPDB -2 L.S. 4 TEMP -173.00 WGHT 0.035500 FVAR 0.22337 IR1 5 0.164462 0.737631 0.951077 11.00000 0.01753 0.01745 = 0.02672 -0.00361 0.00998 -0.00153 CL1 3 0.339876 0.771461 0.912755 11.00000 0.02052 0.03217 = 0.04112 0.00086 0.01631 -0.00094 N1 6 0.062570 0.757866 0.781024 11.00000 0.02002 0.02908 = 0.03043 -0.01001 0.01111 -0.00366 N2 6 0.136250 0.848301 0.945411 11.00000 0.01900 0.01885 = 0.02344 -0.00312 0.00935 -0.00152 N3 6 -0.029964 0.832571 0.643737 11.00000 0.02299 0.03852 = 0.02277 -0.00372 0.00657 -0.00853 C1 1 0.194155 0.629071 0.978972 11.00000 0.03546 0.01935 = 0.04901 -0.00111 0.02518 -0.00006 C2 1 0.068248 0.644220 0.962003 11.00000 0.03026 0.01998 = 0.03688 0.00065 0.01815 -0.00265 C3 1 0.068739 0.690650 1.049106 11.00000 0.02253 0.01912 = 0.03320 0.00248 0.01265 -0.00217 C4 1 0.195608 0.702967 1.122782 11.00000 0.02671 0.02262 = 0.03318 0.00106 0.01073 -0.00179 C5 1 0.271194 0.663553 1.081501 11.00000 0.02363 0.02831 = 0.04275 0.00786 0.01581 0.00300 C6 1 0.237692 0.580155 0.908976 11.00000 0.05434 0.02396 = 0.06946 -0.00787 0.03980 0.00232 AFIX 137 H6A 2 0.315907 0.597030 0.908019 11.00000 -1.50000 H6B 2 0.175899 0.578248 0.831093 11.00000 -1.50000 H6C 2 0.249427 0.533552 0.942548 11.00000 -1.50000 AFIX 0 C7 1 -0.045510 0.615398 0.870030 11.00000 0.04180 0.03311 = 0.05132 -0.00918 0.01825 -0.01862 AFIX 137 H7A 2 -0.081251 0.579136 0.901935 11.00000 -1.50000 H7B 2 -0.023639 0.595501 0.809540 11.00000 -1.50000 H7C 2 -0.105711 0.652789 0.838727 11.00000 -1.50000 AFIX 0 C8 1 -0.044440 0.713420 1.067499 11.00000 0.02990 0.03859 = 0.04490 0.00241 0.02462 0.00429 AFIX 137 H8A 2 -0.109664 0.725108 0.994226 11.00000 -1.50000 H8B 2 -0.024955 0.754363 1.117038 11.00000 -1.50000 H8C 2 -0.072497 0.675635 1.103225 11.00000 -1.50000 AFIX 0 C9 1 0.239206 0.743205 1.232649 11.00000 0.04391 0.03328 = 0.02718 -0.00289 0.00916 -0.00268 AFIX 137 H9A 2 0.251472 0.711262 1.295953 11.00000 -1.50000 H9B 2 0.177306 0.778098 1.229632 11.00000 -1.50000 H9C 2 0.317187 0.766417 1.243793 11.00000 -1.50000 AFIX 0 C10 1 0.409306 0.658588 1.136750 11.00000 0.02285 0.04404 = 0.06312 0.01267 0.01583 0.00730 AFIX 137 H10A 2 0.443495 0.704131 1.167318 11.00000 -1.50000 H10B 2 0.442075 0.643865 1.080305 11.00000 -1.50000 H10C 2 0.432317 0.624534 1.198616 11.00000 -1.50000 AFIX 0 C11 1 0.017328 0.722334 0.680519 11.00000 0.02648 0.03489 = 0.03271 -0.01487 0.01289 -0.00782 C12 1 -0.040443 0.767414 0.595770 11.00000 0.02650 0.04684 = 0.02774 -0.01267 0.01120 -0.01501 C13 1 -0.087139 0.896606 0.587387 11.00000 0.04572 0.04733 = 0.02573 0.00271 -0.00549 -0.00538 AFIX 137 H13A 2 -0.172057 0.898902 0.583098 11.00000 -1.50000 H13B 2 -0.087345 0.897578 0.510481 11.00000 -1.50000 H13C 2 -0.040553 0.936503 0.630601 11.00000 -1.50000 AFIX 0 C14 1 0.033372 0.824174 0.756375 11.00000 0.01986 0.02736 = 0.02283 -0.00378 0.00614 -0.00498 C15 1 0.076719 0.873876 0.845755 11.00000 0.02346 0.02095 = 0.02614 -0.00385 0.00975 -0.00215 C16 1 0.205335 0.895026 1.041235 11.00000 0.02048 0.02161 = 0.02619 -0.00703 0.00533 0.00124 C17 1 0.239561 0.964674 1.002348 11.00000 0.03544 0.02582 = 0.03285 -0.00755 0.01414 -0.00917 AFIX 137 H17A 2 0.278408 0.956102 0.947983 11.00000 -1.50000 H17B 2 0.297152 0.989771 1.068279 11.00000 -1.50000 H17C 2 0.164973 0.992614 0.965955 11.00000 -1.50000 AFIX 0 C18 1 0.136540 0.906838 1.119111 11.00000 0.02494 0.02103 = 0.02476 0.00010 0.00842 0.00633 C19 1 0.012166 0.891505 1.089008 11.00000 0.02771 0.02827 = 0.03414 0.00290 0.01357 0.00511 AFIX 43 H19 2 -0.033262 0.870757 1.017432 11.00000 -1.20000 AFIX 0 C20 1 -0.045388 0.906196 1.162215 11.00000 0.03224 0.04401 = 0.04650 0.00154 0.02210 0.00613 AFIX 43 H20 2 -0.130272 0.895622 1.140696 11.00000 -1.20000 AFIX 0 C21 1 0.019954 0.936451 1.267596 11.00000 0.05450 0.04327 = 0.04022 0.00684 0.03045 0.02003 AFIX 43 H21 2 -0.020191 0.946790 1.317678 11.00000 -1.20000 AFIX 0 C22 1 0.142887 0.951230 1.298580 11.00000 0.04854 0.04285 = 0.02666 -0.00081 0.01190 0.01527 AFIX 43 H22 2 0.188260 0.971014 1.370964 11.00000 -1.20000 AFIX 0 C23 1 0.201097 0.937382 1.224581 11.00000 0.03371 0.03010 = 0.02302 -0.00285 0.00519 0.00857 AFIX 43 H23 2 0.285632 0.948811 1.245980 11.00000 -1.20000 AFIX 0 IR31 5 0.551884 0.761323 0.696442 11.00000 0.01725 0.01979 = 0.02038 0.00126 0.00667 -0.00086 CL31 3 0.767318 0.783623 0.755511 11.00000 0.01820 0.03614 = 0.03219 -0.00180 0.01058 -0.00247 N31 6 0.601025 0.712061 0.852139 11.00000 0.01982 0.01771 = 0.02746 0.00026 0.00843 -0.00111 N32 6 0.555980 0.843126 0.808091 11.00000 0.01726 0.02050 = 0.02312 0.00308 0.00736 0.00092 N33 6 0.654317 0.719304 1.037407 11.00000 0.02102 0.02306 = 0.02472 0.00405 0.01147 0.00158 C31 1 0.446991 0.795418 0.523034 11.00000 0.02793 0.03259 = 0.02199 0.00345 0.00480 -0.00589 C32 1 0.365862 0.768303 0.573649 11.00000 0.02214 0.03131 = 0.02613 0.00247 0.00475 -0.00381 C33 1 0.395600 0.697466 0.603503 11.00000 0.02152 0.02967 = 0.02853 0.00136 0.00773 -0.00411 C34 1 0.500216 0.679590 0.573750 11.00000 0.02687 0.03303 = 0.02307 -0.00738 0.00650 -0.00328 C35 1 0.528173 0.739196 0.522081 11.00000 0.02609 0.04176 = 0.02498 -0.00303 0.00799 -0.00513 C36 1 0.440790 0.864558 0.470642 11.00000 0.05295 0.04213 = 0.02570 0.01180 0.00713 -0.00847 AFIX 137 H36A 2 0.412356 0.859469 0.388018 11.00000 -1.50000 H36B 2 0.522755 0.885909 0.500184 11.00000 -1.50000 H36C 2 0.383146 0.894156 0.488972 11.00000 -1.50000 AFIX 0 C37 1 0.259124 0.806323 0.584245 11.00000 0.02359 0.03864 = 0.04146 0.00310 0.00580 0.00322 AFIX 137 H37A 2 0.182868 0.793305 0.521033 11.00000 -1.50000 H37B 2 0.272132 0.856551 0.582282 11.00000 -1.50000 H37C 2 0.252785 0.793899 0.656327 11.00000 -1.50000 AFIX 0 C38 1 0.328787 0.650264 0.652973 11.00000 0.03014 0.02941 = 0.04032 0.00221 0.01095 -0.00620 AFIX 137 H38A 2 0.297115 0.677168 0.701162 11.00000 -1.50000 H38B 2 0.385340 0.614382 0.698716 11.00000 -1.50000 H38C 2 0.259974 0.628207 0.591569 11.00000 -1.50000 AFIX 0 C39 1 0.560415 0.609915 0.583619 11.00000 0.04113 0.03824 = 0.05001 -0.01468 0.01302 0.00731 AFIX 137 H39A 2 0.539834 0.590248 0.507621 11.00000 -1.50000 H39B 2 0.530832 0.578772 0.628481 11.00000 -1.50000 H39C 2 0.649955 0.615148 0.621210 11.00000 -1.50000 AFIX 0 C40 1 0.625844 0.743685 0.474661 11.00000 0.03600 0.06787 = 0.02948 -0.00669 0.01674 -0.00779 AFIX 137 H40A 2 0.693062 0.711703 0.515974 11.00000 -1.50000 H40B 2 0.657697 0.791312 0.482834 11.00000 -1.50000 H40C 2 0.590907 0.730987 0.394038 11.00000 -1.50000 AFIX 0 C41 1 0.627143 0.646706 0.896927 11.00000 0.02270 0.02021 = 0.03412 0.00154 0.00909 0.00081 H41 2 0.613060 0.605592 0.853038 11.00000 -1.20000 C42 1 0.659215 0.650225 1.011103 11.00000 0.02535 0.01702 = 0.03274 0.00509 0.00831 0.00047 H42 2 0.676158 0.616837 1.063323 11.00000 -1.20000 C43 1 0.680881 0.749078 1.148719 11.00000 0.03875 0.02639 = 0.02203 0.00286 0.00887 0.00147 AFIX 137 H43A 2 0.747504 0.783172 1.165677 11.00000 -1.50000 H43B 2 0.706159 0.712137 1.206042 11.00000 -1.50000 H43C 2 0.606948 0.772065 1.149727 11.00000 -1.50000 AFIX 0 C44 1 0.618229 0.754860 0.938305 11.00000 0.01726 0.02064 = 0.02287 0.00196 0.00925 -0.00235 C45 1 0.591352 0.827467 0.914053 11.00000 0.01762 0.02074 = 0.02887 0.00247 0.00956 0.00035 H45 2 0.589160 0.860315 0.979620 11.00000 -1.20000 C46 1 0.523995 0.916448 0.771052 11.00000 0.02088 0.01868 = 0.02741 0.00472 0.00427 0.00321 H46 2 0.460183 0.903426 0.689503 11.00000 -1.20000 C47 1 0.464700 0.954456 0.841898 11.00000 0.03265 0.02254 = 0.04757 0.00644 0.01860 0.01013 AFIX 137 H47A 2 0.398013 0.925971 0.847160 11.00000 -1.50000 H47B 2 0.431241 0.998969 0.805800 11.00000 -1.50000 H47C 2 0.526714 0.962873 0.918295 11.00000 -1.50000 AFIX 0 C48 1 0.633988 0.955953 0.766754 11.00000 0.03190 0.01400 = 0.03268 0.00121 0.01304 0.00067 C49 1 0.620229 0.993937 0.670345 11.00000 0.05604 0.03566 = 0.03163 0.00695 0.00639 -0.01443 AFIX 43 H49 2 0.543894 0.993074 0.606843 11.00000 -1.20000 AFIX 0 C50 1 0.717347 1.033299 0.665891 11.00000 0.06680 0.04375 = 0.04433 -0.00031 0.02509 -0.02819 AFIX 43 H50 2 0.706997 1.058740 0.598976 11.00000 -1.20000 AFIX 0 C51 1 0.828023 1.035849 0.757024 11.00000 0.04725 0.02941 = 0.06681 -0.00457 0.03503 -0.01081 AFIX 43 H51 2 0.893802 1.063174 0.753623 11.00000 -1.20000 AFIX 0 C52 1 0.842879 0.998245 0.853891 11.00000 0.02842 0.03063 = 0.05408 -0.00397 0.01617 -0.00142 AFIX 43 H52 2 0.919071 0.999723 0.917513 11.00000 -1.20000 AFIX 0 C53 1 0.745800 0.958119 0.858068 11.00000 0.02844 0.02396 = 0.03986 0.00274 0.01143 -0.00154 AFIX 43 H53 2 0.756759 0.931997 0.924488 11.00000 -1.20000 AFIX 0 SB1 7 0.633417 0.937165 0.266424 11.00000 0.02596 0.02425 = 0.02348 -0.00319 0.00949 -0.00086 F1 4 0.501834 0.874466 0.228231 11.00000 0.03985 0.04926 = 0.07090 -0.02503 0.02604 -0.01856 F2 4 0.765770 0.997678 0.304920 11.00000 0.04110 0.03454 = 0.04938 -0.00872 0.01913 -0.00960 F3 4 0.647654 0.918662 0.128039 11.00000 0.07246 0.03840 = 0.02876 -0.00582 0.02535 -0.00747 F4 4 0.623770 0.956623 0.405975 11.00000 0.08592 0.06200 = 0.05381 -0.03031 0.05225 -0.03132 F5 4 0.741108 0.862918 0.331988 11.00000 0.05691 0.02924 = 0.04036 0.00049 -0.00968 0.00472 F6 4 0.523390 1.008245 0.197781 11.00000 0.04240 0.03679 = 0.08899 -0.01722 -0.01428 0.01812 SB2 7 0.856580 0.575170 0.385950 11.00000 0.04267 0.03076 = 0.03126 -0.00337 0.00216 0.00783 F7 4 0.692624 0.599096 0.304481 11.00000 0.03992 0.04770 = 0.12686 -0.00012 -0.00940 0.00003 F8 4 1.023699 0.555920 0.459364 11.00000 0.05900 0.08395 = 0.10871 -0.02939 -0.01876 0.03221 F9 4 0.864300 0.551082 0.248373 11.00000 0.13030 0.15736 = 0.05514 -0.04152 0.03175 -0.00674 F10 4 0.849554 0.601474 0.522797 11.00000 0.11431 0.09130 = 0.06807 -0.03508 0.04137 -0.02802 F11 4 0.813611 0.485210 0.402644 11.00000 0.12416 0.03277 = 0.08587 0.00954 0.00203 -0.01455 F12 4 0.897206 0.667681 0.369200 11.00000 0.08043 0.04872 = 0.08229 0.01046 -0.00359 -0.01712 H11 2 0.014012 0.677238 0.678242 11.00000 0.04775 H12 2 -0.091776 0.776627 0.521429 11.00000 0.04686 H15 2 0.073293 0.921661 0.830405 11.00000 0.04822 H16 2 0.281111 0.872489 1.074915 11.00000 0.04127 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 REM fjl203dm in P2(1) REM R1 = 0.0248 for 13362 Fo > 4sig(Fo) and 0.0262 for all 13916 data REM 673 parameters refined using 4 restraints END ; 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.164462(12) 0.737631(8) 0.951077(13) 0.02013(4) Uani 1 1 d . . . Cl1 Cl 0.33988(9) 0.77146(6) 0.91275(10) 0.0299(2) Uani 1 1 d . . . N1 N 0.0626(3) 0.7579(2) 0.7810(3) 0.0261(7) Uani 1 1 d . . . N2 N 0.1363(3) 0.84830(19) 0.9454(3) 0.0201(7) Uani 1 1 d . . . N3 N -0.0300(3) 0.8326(2) 0.6437(3) 0.0288(8) Uani 1 1 d . . . C1 C 0.1942(4) 0.6291(3) 0.9790(5) 0.0319(10) Uani 1 1 d . . . C2 C 0.0682(4) 0.6442(2) 0.9620(4) 0.0275(9) Uani 1 1 d . . . C3 C 0.0687(4) 0.6906(2) 1.0491(4) 0.0244(8) Uani 1 1 d . . . C4 C 0.1956(4) 0.7030(2) 1.1228(4) 0.0277(9) Uani 1 1 d . . . C5 C 0.2712(4) 0.6636(3) 1.0815(4) 0.0306(10) Uani 1 1 d . . . C6 C 0.2377(5) 0.5802(3) 0.9090(6) 0.0444(13) Uani 1 1 d . . . H6A H 0.3159 0.5970 0.9080 0.067 Uiso 1 1 calc R . . H6B H 0.1759 0.5782 0.8311 0.067 Uiso 1 1 calc R . . H6C H 0.2494 0.5336 0.9425 0.067 Uiso 1 1 calc R . . C7 C -0.0455(5) 0.6154(3) 0.8700(5) 0.0420(12) Uani 1 1 d . . . H7A H -0.0813 0.5791 0.9019 0.063 Uiso 1 1 calc R . . H7B H -0.0236 0.5955 0.8095 0.063 Uiso 1 1 calc R . . H7C H -0.1057 0.6528 0.8387 0.063 Uiso 1 1 calc R . . C8 C -0.0444(4) 0.7134(3) 1.0675(5) 0.0347(10) Uani 1 1 d . . . H8A H -0.1097 0.7251 0.9942 0.052 Uiso 1 1 calc R . . H8B H -0.0250 0.7544 1.1170 0.052 Uiso 1 1 calc R . . H8C H -0.0725 0.6756 1.1032 0.052 Uiso 1 1 calc R . . C9 C 0.2392(5) 0.7432(3) 1.2326(4) 0.0362(10) Uani 1 1 d . . . H9A H 0.2515 0.7113 1.2960 0.054 Uiso 1 1 calc R . . H9B H 0.1773 0.7781 1.2296 0.054 Uiso 1 1 calc R . . H9C H 0.3172 0.7664 1.2438 0.054 Uiso 1 1 calc R . . C10 C 0.4093(4) 0.6586(3) 1.1367(6) 0.0436(13) Uani 1 1 d . . . H10A H 0.4435 0.7041 1.1673 0.065 Uiso 1 1 calc R . . H10B H 0.4421 0.6439 1.0803 0.065 Uiso 1 1 calc R . . H10C H 0.4323 0.6245 1.1986 0.065 Uiso 1 1 calc R . . C11 C 0.0173(4) 0.7223(3) 0.6805(4) 0.0309(11) Uani 1 1 d . . . C12 C -0.0404(4) 0.7674(3) 0.5958(4) 0.0335(11) Uani 1 1 d D . . C13 C -0.0871(5) 0.8966(3) 0.5874(4) 0.0454(14) Uani 1 1 d . . . H13A H -0.1721 0.8989 0.5831 0.068 Uiso 1 1 calc R . . H13B H -0.0873 0.8976 0.5105 0.068 Uiso 1 1 calc R . . H13C H -0.0406 0.9365 0.6306 0.068 Uiso 1 1 calc R . . C14 C 0.0334(4) 0.8242(2) 0.7564(4) 0.0240(8) Uani 1 1 d . . . C15 C 0.0767(4) 0.8739(2) 0.8458(4) 0.0235(8) Uani 1 1 d D . . C16 C 0.2053(4) 0.8950(2) 1.0412(4) 0.0239(8) Uani 1 1 d . . . C17 C 0.2396(4) 0.9647(3) 1.0023(4) 0.0311(10) Uani 1 1 d . . . H17A H 0.2784 0.9561 0.9480 0.047 Uiso 1 1 calc R . . H17B H 0.2972 0.9898 1.0683 0.047 Uiso 1 1 calc R . . H17C H 0.1650 0.9926 0.9660 0.047 Uiso 1 1 calc R . . C18 C 0.1365(4) 0.9068(2) 1.1191(4) 0.0239(8) Uani 1 1 d . . . C19 C 0.0122(4) 0.8915(3) 1.0890(4) 0.0295(9) Uani 1 1 d . . . H19 H -0.0333 0.8708 1.0174 0.035 Uiso 1 1 calc R . . C20 C -0.0454(5) 0.9062(3) 1.1622(5) 0.0388(11) Uani 1 1 d . . . H20 H -0.1303 0.8956 1.1407 0.047 Uiso 1 1 calc R . . C21 C 0.0200(5) 0.9365(3) 1.2676(5) 0.0423(13) Uani 1 1 d . . . H21 H -0.0202 0.9468 1.3177 0.051 Uiso 1 1 calc R . . C22 C 0.1429(5) 0.9512(3) 1.2986(4) 0.0401(12) Uani 1 1 d . . . H22 H 0.1883 0.9710 1.3710 0.048 Uiso 1 1 calc R . . C23 C 0.2011(4) 0.9374(3) 1.2246(4) 0.0307(10) Uani 1 1 d . . . H23 H 0.2856 0.9488 1.2460 0.037 Uiso 1 1 calc R . . Ir31 Ir 0.551884(12) 0.761323(8) 0.696442(12) 0.01932(4) Uani 1 1 d . . . Cl31 Cl 0.76732(9) 0.78362(6) 0.75551(10) 0.0286(2) Uani 1 1 d . . . N31 N 0.6010(3) 0.71206(19) 0.8521(3) 0.0219(7) Uani 1 1 d . . . N32 N 0.5560(3) 0.84313(19) 0.8081(3) 0.0204(7) Uani 1 1 d . . . N33 N 0.6543(3) 0.71930(19) 1.0374(3) 0.0221(7) Uani 1 1 d . . . C31 C 0.4470(4) 0.7954(3) 0.5230(4) 0.0289(9) Uani 1 1 d . . . C32 C 0.3659(4) 0.7683(3) 0.5736(4) 0.0279(9) Uani 1 1 d . . . C33 C 0.3956(4) 0.6975(2) 0.6035(4) 0.0271(9) Uani 1 1 d . . . C34 C 0.5002(4) 0.6796(3) 0.5737(4) 0.0286(9) Uani 1 1 d . . . C35 C 0.5282(4) 0.7392(3) 0.5221(4) 0.0315(9) Uani 1 1 d . . . C36 C 0.4408(5) 0.8646(3) 0.4706(4) 0.0427(13) Uani 1 1 d . . . H36A H 0.4124 0.8595 0.3880 0.064 Uiso 1 1 calc R . . H36B H 0.5228 0.8859 0.5002 0.064 Uiso 1 1 calc R . . H36C H 0.3831 0.8942 0.4890 0.064 Uiso 1 1 calc R . . C37 C 0.2591(4) 0.8063(3) 0.5842(5) 0.0366(11) Uani 1 1 d . . . H37A H 0.1829 0.7933 0.5210 0.055 Uiso 1 1 calc R . . H37B H 0.2721 0.8566 0.5823 0.055 Uiso 1 1 calc R . . H37C H 0.2528 0.7939 0.6563 0.055 Uiso 1 1 calc R . . C38 C 0.3288(4) 0.6503(3) 0.6530(5) 0.0341(10) Uani 1 1 d . . . H38A H 0.2971 0.6772 0.7012 0.051 Uiso 1 1 calc R . . H38B H 0.3853 0.6144 0.6987 0.051 Uiso 1 1 calc R . . H38C H 0.2600 0.6282 0.5916 0.051 Uiso 1 1 calc R . . C39 C 0.5604(5) 0.6099(3) 0.5836(5) 0.0445(13) Uani 1 1 d . . . H39A H 0.5398 0.5902 0.5076 0.067 Uiso 1 1 calc R . . H39B H 0.5308 0.5788 0.6285 0.067 Uiso 1 1 calc R . . H39C H 0.6500 0.6151 0.6212 0.067 Uiso 1 1 calc R . . C40 C 0.6258(4) 0.7437(4) 0.4747(4) 0.0432(13) Uani 1 1 d . . . H40A H 0.6931 0.7117 0.5160 0.065 Uiso 1 1 calc R . . H40B H 0.6577 0.7913 0.4828 0.065 Uiso 1 1 calc R . . H40C H 0.5909 0.7310 0.3940 0.065 Uiso 1 1 calc R . . C41 C 0.6271(4) 0.6467(2) 0.8969(4) 0.0262(9) Uani 1 1 d D . . H41 H 0.613(5) 0.6056(18) 0.853(4) 0.031 Uiso 1 1 d D . . C42 C 0.6592(4) 0.6502(2) 1.0111(4) 0.0259(9) Uani 1 1 d . . . H42 H 0.676(5) 0.617(3) 1.063(5) 0.031 Uiso 1 1 d . . . C43 C 0.6809(4) 0.7491(2) 1.1487(3) 0.0299(10) Uani 1 1 d . . . H43A H 0.7475 0.7832 1.1657 0.045 Uiso 1 1 calc R . . H43B H 0.7062 0.7121 1.2060 0.045 Uiso 1 1 calc R . . H43C H 0.6069 0.7721 1.1497 0.045 Uiso 1 1 calc R . . C44 C 0.6182(3) 0.7549(2) 0.9383(3) 0.0198(7) Uani 1 1 d . . . C45 C 0.5914(4) 0.8275(2) 0.9141(4) 0.0222(8) Uani 1 1 d . . . H45 H 0.589(5) 0.860(3) 0.980(5) 0.027 Uiso 1 1 d . . . C46 C 0.5240(4) 0.9164(2) 0.7711(4) 0.0238(8) Uani 1 1 d . . . H46 H 0.460(5) 0.903(3) 0.690(5) 0.029 Uiso 1 1 d . . . C47 C 0.4647(4) 0.9545(3) 0.8419(5) 0.0333(10) Uani 1 1 d . . . H47A H 0.3980 0.9260 0.8472 0.050 Uiso 1 1 calc R . . H47B H 0.4312 0.9990 0.8058 0.050 Uiso 1 1 calc R . . H47C H 0.5267 0.9629 0.9183 0.050 Uiso 1 1 calc R . . C48 C 0.6340(4) 0.9560(2) 0.7668(4) 0.0260(8) Uani 1 1 d . . . C49 C 0.6202(6) 0.9939(3) 0.6703(5) 0.0443(13) Uani 1 1 d . . . H49 H 0.5439 0.9931 0.6068 0.053 Uiso 1 1 calc R . . C50 C 0.7173(6) 1.0333(3) 0.6659(5) 0.0505(16) Uani 1 1 d . . . H50 H 0.7070 1.0587 0.5990 0.061 Uiso 1 1 calc R . . C51 C 0.8280(5) 1.0358(3) 0.7570(6) 0.0439(13) Uani 1 1 d . . . H51 H 0.8938 1.0632 0.7536 0.053 Uiso 1 1 calc R . . C52 C 0.8429(4) 0.9982(3) 0.8539(5) 0.0376(11) Uani 1 1 d . . . H52 H 0.9191 0.9997 0.9175 0.045 Uiso 1 1 calc R . . C53 C 0.7458(4) 0.9581(3) 0.8581(4) 0.0313(10) Uani 1 1 d . . . H53 H 0.7568 0.9320 0.9245 0.038 Uiso 1 1 calc R . . Sb1 Sb 0.63342(3) 0.937165(15) 0.26642(2) 0.02457(6) Uani 1 1 d . . . F1 F 0.5018(3) 0.87447(19) 0.2282(3) 0.0519(9) Uani 1 1 d . . . F2 F 0.7658(3) 0.99768(17) 0.3049(3) 0.0412(7) Uani 1 1 d . . . F3 F 0.6477(3) 0.91866(17) 0.1280(2) 0.0448(8) Uani 1 1 d . . . F4 F 0.6238(4) 0.9566(2) 0.4060(3) 0.0596(11) Uani 1 1 d . . . F5 F 0.7411(3) 0.86292(17) 0.3320(3) 0.0507(9) Uani 1 1 d . . . F6 F 0.5234(3) 1.0082(2) 0.1978(4) 0.0680(13) Uani 1 1 d . . . Sb2 Sb 0.85658(3) 0.575170(19) 0.38595(3) 0.03853(8) Uani 1 1 d . . . F7 F 0.6926(3) 0.5991(2) 0.3045(5) 0.0840(16) Uani 1 1 d . . . F8 F 1.0237(4) 0.5559(3) 0.4594(5) 0.0993(19) Uani 1 1 d . . . F9 F 0.8643(6) 0.5511(4) 0.2484(4) 0.115(2) Uani 1 1 d . . . F10 F 0.8496(5) 0.6015(3) 0.5228(4) 0.0893(16) Uani 1 1 d . . . F11 F 0.8136(5) 0.4852(2) 0.4026(4) 0.0925(17) Uani 1 1 d . . . F12 F 0.8972(4) 0.6677(2) 0.3692(4) 0.0810(15) Uani 1 1 d . . . H11 H 0.014(6) 0.677(4) 0.678(5) 0.048(19) Uiso 1 1 d . . . H12 H -0.092(4) 0.777(3) 0.521(2) 0.047(17) Uiso 1 1 d D . . H15 H 0.073(5) 0.9217(12) 0.830(5) 0.048(17) Uiso 1 1 d D . . H16 H 0.281(5) 0.872(3) 1.075(5) 0.041(16) Uiso 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 Ir1 0.01753(6) 0.01745(7) 0.02672(7) -0.00361(6) 0.00998(6) -0.00153(5) Cl1 0.0205(4) 0.0322(6) 0.0411(6) 0.0009(4) 0.0163(4) -0.0009(4) N1 0.0200(13) 0.0291(19) 0.0304(17) -0.0100(16) 0.0111(14) -0.0037(14) N2 0.0190(14) 0.0188(17) 0.0234(16) -0.0031(13) 0.0093(13) -0.0015(12) N3 0.0230(16) 0.039(2) 0.0228(18) -0.0037(16) 0.0066(15) -0.0085(15) C1 0.035(2) 0.019(2) 0.049(3) -0.001(2) 0.025(2) -0.0001(18) C2 0.030(2) 0.020(2) 0.037(2) 0.0007(17) 0.0181(19) -0.0026(16) C3 0.0225(17) 0.019(2) 0.033(2) 0.0025(16) 0.0127(18) -0.0022(15) C4 0.0267(19) 0.023(2) 0.033(2) 0.0011(18) 0.0107(19) -0.0018(16) C5 0.0236(19) 0.028(2) 0.043(3) 0.008(2) 0.016(2) 0.0030(17) C6 0.054(3) 0.024(3) 0.069(4) -0.008(3) 0.040(3) 0.002(2) C7 0.042(3) 0.033(3) 0.051(3) -0.009(2) 0.018(3) -0.019(2) C8 0.030(2) 0.039(3) 0.045(3) 0.002(2) 0.025(2) 0.0043(19) C9 0.044(2) 0.033(3) 0.027(2) -0.003(2) 0.009(2) -0.003(2) C10 0.023(2) 0.044(3) 0.063(4) 0.013(3) 0.016(2) 0.007(2) C11 0.0265(19) 0.035(3) 0.033(2) -0.0149(19) 0.0129(19) -0.0078(18) C12 0.0265(19) 0.047(3) 0.028(2) -0.013(2) 0.0112(18) -0.015(2) C13 0.046(3) 0.047(3) 0.026(2) 0.003(2) -0.005(2) -0.005(2) C14 0.0199(17) 0.027(2) 0.0228(19) -0.0038(16) 0.0061(16) -0.0050(15) C15 0.0235(17) 0.021(2) 0.026(2) -0.0039(16) 0.0098(17) -0.0021(15) C16 0.0205(17) 0.022(2) 0.026(2) -0.0070(16) 0.0053(16) 0.0012(15) C17 0.035(2) 0.026(2) 0.033(2) -0.0075(18) 0.014(2) -0.0092(18) C18 0.0249(18) 0.021(2) 0.0248(19) 0.0001(16) 0.0084(17) 0.0063(15) C19 0.028(2) 0.028(2) 0.034(2) 0.0029(18) 0.0136(19) 0.0051(17) C20 0.032(2) 0.044(3) 0.046(3) 0.002(2) 0.022(2) 0.006(2) C21 0.054(3) 0.043(3) 0.040(3) 0.007(2) 0.030(3) 0.020(3) C22 0.049(3) 0.043(3) 0.027(2) -0.001(2) 0.012(2) 0.015(2) C23 0.034(2) 0.030(2) 0.023(2) -0.0028(18) 0.0052(18) 0.0086(18) Ir31 0.01725(6) 0.01979(7) 0.02038(7) 0.00126(6) 0.00667(5) -0.00086(5) Cl31 0.0182(4) 0.0361(6) 0.0322(5) -0.0018(4) 0.0106(4) -0.0025(4) N31 0.0198(14) 0.0177(16) 0.0275(17) 0.0003(14) 0.0084(14) -0.0011(12) N32 0.0173(14) 0.0205(17) 0.0231(16) 0.0031(13) 0.0074(13) 0.0009(12) N33 0.0210(14) 0.0231(19) 0.0247(17) 0.0040(13) 0.0115(14) 0.0016(12) C31 0.028(2) 0.033(3) 0.022(2) 0.0035(18) 0.0048(17) -0.0059(18) C32 0.0221(16) 0.031(3) 0.0261(19) 0.0025(18) 0.0048(16) -0.0038(17) C33 0.0215(18) 0.030(2) 0.029(2) 0.0014(18) 0.0077(17) -0.0041(16) C34 0.027(2) 0.033(3) 0.023(2) -0.0074(18) 0.0065(18) -0.0033(17) C35 0.0261(18) 0.042(3) 0.0250(19) -0.003(2) 0.0080(16) -0.0051(19) C36 0.053(3) 0.042(3) 0.026(2) 0.012(2) 0.007(2) -0.008(3) C37 0.0236(19) 0.039(3) 0.041(3) 0.003(2) 0.006(2) 0.0032(19) C38 0.030(2) 0.029(3) 0.040(3) 0.002(2) 0.011(2) -0.0062(18) C39 0.041(3) 0.038(3) 0.050(3) -0.015(3) 0.013(3) 0.007(2) C40 0.036(2) 0.068(4) 0.029(2) -0.007(2) 0.017(2) -0.008(3) C41 0.0227(18) 0.020(2) 0.034(2) 0.0015(17) 0.0091(18) 0.0008(16) C42 0.0254(19) 0.017(2) 0.033(2) 0.0051(17) 0.0083(18) 0.0005(15) C43 0.039(2) 0.026(3) 0.0220(18) 0.0029(16) 0.0089(17) 0.0015(18) C44 0.0173(14) 0.021(2) 0.0229(17) 0.0020(15) 0.0092(14) -0.0024(14) C45 0.0176(16) 0.021(2) 0.029(2) 0.0025(16) 0.0096(16) 0.0004(14) C46 0.0209(16) 0.019(2) 0.027(2) 0.0047(16) 0.0043(16) 0.0032(15) C47 0.033(2) 0.023(2) 0.048(3) 0.006(2) 0.019(2) 0.0101(18) C48 0.032(2) 0.0140(19) 0.033(2) 0.0012(16) 0.0130(19) 0.0007(16) C49 0.056(3) 0.036(3) 0.032(3) 0.007(2) 0.006(2) -0.014(2) C50 0.067(4) 0.044(3) 0.044(3) 0.000(3) 0.025(3) -0.028(3) C51 0.047(3) 0.029(3) 0.067(4) -0.005(3) 0.035(3) -0.011(2) C52 0.028(2) 0.031(3) 0.054(3) -0.004(2) 0.016(2) -0.0014(19) C53 0.028(2) 0.024(2) 0.040(3) 0.0027(19) 0.011(2) -0.0015(17) Sb1 0.02596(12) 0.02425(14) 0.02348(13) -0.00319(11) 0.00949(11) -0.00086(10) F1 0.0399(16) 0.049(2) 0.071(2) -0.0250(18) 0.0260(17) -0.0186(14) F2 0.0411(15) 0.0345(17) 0.0494(18) -0.0087(14) 0.0191(15) -0.0096(13) F3 0.072(2) 0.0384(18) 0.0288(14) -0.0058(13) 0.0254(15) -0.0075(16) F4 0.086(3) 0.062(2) 0.054(2) -0.0303(18) 0.052(2) -0.031(2) F5 0.0569(19) 0.0292(17) 0.0404(17) 0.0005(13) -0.0097(16) 0.0047(14) F6 0.0424(17) 0.037(2) 0.089(3) -0.0172(19) -0.0143(19) 0.0181(15) Sb2 0.04267(17) 0.03076(18) 0.03126(16) -0.00337(13) 0.00216(14) 0.00783(14) F7 0.0399(19) 0.048(3) 0.127(4) 0.000(3) -0.009(2) 0.0000(17) F8 0.059(2) 0.084(4) 0.109(4) -0.029(3) -0.019(3) 0.032(2) F9 0.130(5) 0.157(6) 0.055(3) -0.042(3) 0.032(3) -0.007(4) F10 0.114(4) 0.091(4) 0.068(3) -0.035(3) 0.041(3) -0.028(3) F11 0.124(4) 0.033(2) 0.086(3) 0.010(2) 0.002(3) -0.015(2) F12 0.080(3) 0.049(3) 0.082(3) 0.010(2) -0.004(3) -0.017(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 N1 2.071(4) . ? Ir1 C1 2.124(5) . ? Ir1 N2 2.151(4) . ? Ir1 C2 2.156(4) . ? Ir1 C3 2.175(4) . ? Ir1 C4 2.181(5) . ? Ir1 C5 2.183(5) . ? Ir1 Cl1 2.3864(10) . ? N1 C14 1.327(6) . ? N1 C11 1.367(6) . ? N2 C15 1.289(6) . ? N2 C16 1.482(5) . ? N3 C14 1.349(6) . ? N3 C12 1.379(7) . ? N3 C13 1.454(7) . ? C1 C5 1.435(7) . ? C1 C2 1.442(6) . ? C1 C6 1.515(7) . ? C2 C3 1.424(6) . ? C2 C7 1.505(7) . ? C3 C4 1.444(6) . ? C3 C8 1.503(6) . ? C4 C5 1.415(7) . ? C4 C9 1.507(7) . ? C5 C10 1.504(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.348(8) . ? C11 H11 0.87(7) . ? C12 H12 0.92(2) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.423(6) . ? C15 H15 0.94(2) . ? C16 C18 1.520(6) . ? C16 C17 1.535(7) . ? C16 H16 0.93(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.394(6) . ? C18 C23 1.394(6) . ? C19 C20 1.377(7) . ? C19 H19 0.9500 . ? C20 C21 1.393(8) . ? C20 H20 0.9500 . ? C21 C22 1.374(8) . ? C21 H21 0.9500 . ? C22 C23 1.388(7) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? Ir31 N31 2.071(4) . ? Ir31 N32 2.110(4) . ? Ir31 C34 2.135(5) . ? Ir31 C33 2.148(4) . ? Ir31 C32 2.149(4) . ? Ir31 C35 2.174(4) . ? Ir31 C31 2.178(4) . ? Ir31 Cl31 2.3880(10) . ? N31 C44 1.325(5) . ? N31 C41 1.366(6) . ? N32 C45 1.287(6) . ? N32 C46 1.489(5) . ? N33 C44 1.354(5) . ? N33 C42 1.377(6) . ? N33 C43 1.449(5) . ? C31 C32 1.440(6) . ? C31 C35 1.446(7) . ? C31 C36 1.477(7) . ? C32 C33 1.422(7) . ? C32 C37 1.503(7) . ? C33 C34 1.461(6) . ? C33 C38 1.490(6) . ? C34 C35 1.423(7) . ? C34 C39 1.498(7) . ? C35 C40 1.492(6) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.358(7) . ? C41 H41 0.946(19) . ? C42 H42 0.89(6) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.439(6) . ? C45 H45 1.06(5) . ? C46 C48 1.519(6) . ? C46 C47 1.524(7) . ? C46 H46 1.05(5) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C53 1.381(6) . ? C48 C49 1.385(7) . ? C49 C50 1.390(8) . ? C49 H49 0.9500 . ? C50 C51 1.372(9) . ? C50 H50 0.9500 . ? C51 C52 1.383(8) . ? C51 H51 0.9500 . ? C52 C53 1.396(7) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? Sb1 F2 1.852(3) . ? Sb1 F6 1.854(3) . ? Sb1 F4 1.864(3) . ? Sb1 F3 1.870(3) . ? Sb1 F1 1.873(3) . ? Sb1 F5 1.878(3) . ? Sb2 F11 1.838(4) . ? Sb2 F10 1.849(5) . ? Sb2 F9 1.850(5) . ? Sb2 F8 1.860(4) . ? Sb2 F7 1.862(4) . ? Sb2 F12 1.876(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ir1 C1 110.59(19) . . ? N1 Ir1 N2 76.07(14) . . ? C1 Ir1 N2 172.52(17) . . ? N1 Ir1 C2 96.76(17) . . ? C1 Ir1 C2 39.35(17) . . ? N2 Ir1 C2 138.48(15) . . ? N1 Ir1 C3 117.45(15) . . ? C1 Ir1 C3 65.38(17) . . ? N2 Ir1 C3 108.85(15) . . ? C2 Ir1 C3 38.37(17) . . ? N1 Ir1 C4 156.15(15) . . ? C1 Ir1 C4 65.05(19) . . ? N2 Ir1 C4 107.48(15) . . ? C2 Ir1 C4 64.53(17) . . ? C3 Ir1 C4 38.73(16) . . ? N1 Ir1 C5 148.40(18) . . ? C1 Ir1 C5 38.9(2) . . ? N2 Ir1 C5 135.03(17) . . ? C2 Ir1 C5 64.47(17) . . ? C3 Ir1 C5 64.15(16) . . ? C4 Ir1 C5 37.84(18) . . ? N1 Ir1 Cl1 86.09(10) . . ? C1 Ir1 Cl1 101.71(13) . . ? N2 Ir1 Cl1 81.82(9) . . ? C2 Ir1 Cl1 139.20(12) . . ? C3 Ir1 Cl1 155.59(12) . . ? C4 Ir1 Cl1 117.68(12) . . ? C5 Ir1 Cl1 92.58(12) . . ? C14 N1 C11 106.7(4) . . ? C14 N1 Ir1 114.9(3) . . ? C11 N1 Ir1 138.4(4) . . ? C15 N2 C16 119.9(4) . . ? C15 N2 Ir1 115.4(3) . . ? C16 N2 Ir1 122.9(3) . . ? C14 N3 C12 106.4(4) . . ? C14 N3 C13 126.0(4) . . ? C12 N3 C13 127.2(4) . . ? C5 C1 C2 107.2(4) . . ? C5 C1 C6 125.9(4) . . ? C2 C1 C6 126.7(5) . . ? C5 C1 Ir1 72.8(3) . . ? C2 C1 Ir1 71.5(3) . . ? C6 C1 Ir1 125.6(4) . . ? C3 C2 C1 108.3(4) . . ? C3 C2 C7 125.1(4) . . ? C1 C2 C7 126.6(5) . . ? C3 C2 Ir1 71.5(2) . . ? C1 C2 Ir1 69.1(3) . . ? C7 C2 Ir1 126.0(4) . . ? C2 C3 C4 107.7(4) . . ? C2 C3 C8 124.5(4) . . ? C4 C3 C8 127.3(4) . . ? C2 C3 Ir1 70.1(2) . . ? C4 C3 Ir1 70.9(2) . . ? C8 C3 Ir1 130.8(3) . . ? C5 C4 C3 108.0(4) . . ? C5 C4 C9 125.7(4) . . ? C3 C4 C9 125.8(4) . . ? C5 C4 Ir1 71.2(3) . . ? C3 C4 Ir1 70.4(3) . . ? C9 C4 Ir1 129.9(3) . . ? C4 C5 C1 108.7(4) . . ? C4 C5 C10 125.4(5) . . ? C1 C5 C10 125.9(5) . . ? C4 C5 Ir1 71.0(3) . . ? C1 C5 Ir1 68.4(3) . . ? C10 C5 Ir1 126.8(3) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 N1 108.9(4) . . ? C12 C11 H11 128(4) . . ? N1 C11 H11 122(4) . . ? C11 C12 N3 107.3(4) . . ? C11 C12 H12 151(4) . . ? N3 C12 H12 101(4) . . ? N3 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 N3 110.7(4) . . ? N1 C14 C15 118.4(4) . . ? N3 C14 C15 130.8(4) . . ? N2 C15 C14 115.1(4) . . ? N2 C15 H15 123(4) . . ? C14 C15 H15 121(4) . . ? N2 C16 C18 111.6(3) . . ? N2 C16 C17 113.1(4) . . ? C18 C16 C17 110.6(4) . . ? N2 C16 H16 103(4) . . ? C18 C16 H16 115(4) . . ? C17 C16 H16 103(4) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 118.6(4) . . ? C19 C18 C16 123.7(4) . . ? C23 C18 C16 117.6(4) . . ? C20 C19 C18 120.5(5) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 120.5(5) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C22 C21 C20 119.5(5) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C21 C22 C23 120.3(5) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C18 120.6(5) . . ? C22 C23 H23 119.7 . . ? C18 C23 H23 119.7 . . ? N31 Ir31 N32 76.63(14) . . ? N31 Ir31 C34 105.15(17) . . ? N32 Ir31 C34 165.89(15) . . ? N31 Ir31 C33 97.53(16) . . ? N32 Ir31 C33 126.23(15) . . ? C34 Ir31 C33 39.90(17) . . ? N31 Ir31 C32 123.86(15) . . ? N32 Ir31 C32 101.39(16) . . ? C34 Ir31 C32 65.75(18) . . ? C33 Ir31 C32 38.64(18) . . ? N31 Ir31 C35 140.31(19) . . ? N32 Ir31 C35 142.82(18) . . ? C34 Ir31 C35 38.54(19) . . ? C33 Ir31 C35 65.04(17) . . ? C32 Ir31 C35 64.73(17) . . ? N31 Ir31 C31 162.02(15) . . ? N32 Ir31 C31 108.51(16) . . ? C34 Ir31 C31 65.62(18) . . ? C33 Ir31 C31 65.29(17) . . ? C32 Ir31 C31 38.87(17) . . ? C35 Ir31 C31 38.81(19) . . ? N31 Ir31 Cl31 84.78(10) . . ? N32 Ir31 Cl31 84.68(9) . . ? C34 Ir31 Cl31 109.37(13) . . ? C33 Ir31 Cl31 148.81(13) . . ? C32 Ir31 Cl31 151.35(12) . . ? C35 Ir31 Cl31 93.48(11) . . ? C31 Ir31 Cl31 112.57(12) . . ? C44 N31 C41 106.7(4) . . ? C44 N31 Ir31 114.1(3) . . ? C41 N31 Ir31 139.2(3) . . ? C45 N32 C46 119.7(4) . . ? C45 N32 Ir31 116.6(3) . . ? C46 N32 Ir31 123.7(3) . . ? C44 N33 C42 106.7(4) . . ? C44 N33 C43 125.9(4) . . ? C42 N33 C43 127.3(4) . . ? C32 C31 C35 106.7(4) . . ? C32 C31 C36 127.1(5) . . ? C35 C31 C36 126.0(5) . . ? C32 C31 Ir31 69.5(2) . . ? C35 C31 Ir31 70.5(3) . . ? C36 C31 Ir31 129.8(3) . . ? C33 C32 C31 109.3(4) . . ? C33 C32 C37 124.8(4) . . ? C31 C32 C37 125.8(5) . . ? C33 C32 Ir31 70.6(2) . . ? C31 C32 Ir31 71.6(2) . . ? C37 C32 Ir31 128.0(3) . . ? C32 C33 C34 107.5(4) . . ? C32 C33 C38 125.6(4) . . ? C34 C33 C38 126.9(4) . . ? C32 C33 Ir31 70.7(2) . . ? C34 C33 Ir31 69.6(2) . . ? C38 C33 Ir31 126.4(3) . . ? C35 C34 C33 107.4(4) . . ? C35 C34 C39 125.0(5) . . ? C33 C34 C39 127.3(5) . . ? C35 C34 Ir31 72.2(3) . . ? C33 C34 Ir31 70.6(3) . . ? C39 C34 Ir31 127.2(3) . . ? C34 C35 C31 109.1(4) . . ? C34 C35 C40 125.8(5) . . ? C31 C35 C40 125.0(5) . . ? C34 C35 Ir31 69.2(3) . . ? C31 C35 Ir31 70.7(3) . . ? C40 C35 Ir31 126.0(3) . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C35 C40 H40A 109.5 . . ? C35 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C35 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 N31 109.1(4) . . ? C42 C41 H41 126(3) . . ? N31 C41 H41 124(3) . . ? C41 C42 N33 106.8(4) . . ? C41 C42 H42 131(4) . . ? N33 C42 H42 122(4) . . ? N33 C43 H43A 109.5 . . ? N33 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N33 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N31 C44 N33 110.7(4) . . ? N31 C44 C45 118.3(4) . . ? N33 C44 C45 130.9(4) . . ? N32 C45 C44 114.1(4) . . ? N32 C45 H45 126(3) . . ? C44 C45 H45 119(3) . . ? N32 C46 C48 111.7(3) . . ? N32 C46 C47 112.6(4) . . ? C48 C46 C47 111.8(4) . . ? N32 C46 H46 95(3) . . ? C48 C46 H46 112(3) . . ? C47 C46 H46 113(3) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C53 C48 C49 118.7(5) . . ? C53 C48 C46 122.2(4) . . ? C49 C48 C46 119.1(4) . . ? C48 C49 C50 120.4(5) . . ? C48 C49 H49 119.8 . . ? C50 C49 H49 119.8 . . ? C51 C50 C49 120.8(5) . . ? C51 C50 H50 119.6 . . ? C49 C50 H50 119.6 . . ? C50 C51 C52 119.4(5) . . ? C50 C51 H51 120.3 . . ? C52 C51 H51 120.3 . . ? C51 C52 C53 119.9(5) . . ? C51 C52 H52 120.0 . . ? C53 C52 H52 120.0 . . ? C48 C53 C52 120.8(5) . . ? C48 C53 H53 119.6 . . ? C52 C53 H53 119.6 . . ? F2 Sb1 F6 91.40(17) . . ? F2 Sb1 F4 88.54(15) . . ? F6 Sb1 F4 90.8(2) . . ? F2 Sb1 F3 89.91(14) . . ? F6 Sb1 F3 89.69(19) . . ? F4 Sb1 F3 178.37(16) . . ? F2 Sb1 F1 178.84(15) . . ? F6 Sb1 F1 89.73(18) . . ? F4 Sb1 F1 91.70(16) . . ? F3 Sb1 F1 89.84(15) . . ? F2 Sb1 F5 90.34(15) . . ? F6 Sb1 F5 177.92(15) . . ? F4 Sb1 F5 90.35(18) . . ? F3 Sb1 F5 89.16(16) . . ? F1 Sb1 F5 88.53(16) . . ? F11 Sb2 F10 92.0(3) . . ? F11 Sb2 F9 89.4(3) . . ? F10 Sb2 F9 178.6(3) . . ? F11 Sb2 F8 92.2(3) . . ? F10 Sb2 F8 90.1(3) . . ? F9 Sb2 F8 90.0(3) . . ? F11 Sb2 F7 91.5(2) . . ? F10 Sb2 F7 92.6(3) . . ? F9 Sb2 F7 87.2(3) . . ? F8 Sb2 F7 175.3(3) . . ? F11 Sb2 F12 178.7(3) . . ? F10 Sb2 F12 87.4(3) . . ? F9 Sb2 F12 91.3(3) . . ? F8 Sb2 F12 88.9(2) . . ? F7 Sb2 F12 87.5(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ir1 N1 C14 176.4(3) . . . . ? N2 Ir1 N1 C14 -0.1(3) . . . . ? C2 Ir1 N1 C14 138.3(3) . . . . ? C3 Ir1 N1 C14 104.2(3) . . . . ? C4 Ir1 N1 C14 101.7(5) . . . . ? C5 Ir1 N1 C14 -171.2(3) . . . . ? Cl1 Ir1 N1 C14 -82.6(3) . . . . ? C1 Ir1 N1 C11 -6.7(5) . . . . ? N2 Ir1 N1 C11 176.9(5) . . . . ? C2 Ir1 N1 C11 -44.7(4) . . . . ? C3 Ir1 N1 C11 -78.8(5) . . . . ? C4 Ir1 N1 C11 -81.3(6) . . . . ? C5 Ir1 N1 C11 5.8(6) . . . . ? Cl1 Ir1 N1 C11 94.4(4) . . . . ? N1 Ir1 N2 C15 -1.9(3) . . . . ? C2 Ir1 N2 C15 -86.3(4) . . . . ? C3 Ir1 N2 C15 -116.5(3) . . . . ? C4 Ir1 N2 C15 -157.3(3) . . . . ? C5 Ir1 N2 C15 171.6(3) . . . . ? Cl1 Ir1 N2 C15 86.1(3) . . . . ? N1 Ir1 N2 C16 -166.7(3) . . . . ? C2 Ir1 N2 C16 108.8(3) . . . . ? C3 Ir1 N2 C16 78.6(3) . . . . ? C4 Ir1 N2 C16 37.8(3) . . . . ? C5 Ir1 N2 C16 6.7(4) . . . . ? Cl1 Ir1 N2 C16 -78.8(3) . . . . ? N1 Ir1 C1 C5 169.6(2) . . . . ? C2 Ir1 C1 C5 -115.5(4) . . . . ? C3 Ir1 C1 C5 -78.7(3) . . . . ? C4 Ir1 C1 C5 -35.9(3) . . . . ? Cl1 Ir1 C1 C5 79.4(3) . . . . ? N1 Ir1 C1 C2 -74.9(3) . . . . ? C3 Ir1 C1 C2 36.7(3) . . . . ? C4 Ir1 C1 C2 79.6(3) . . . . ? C5 Ir1 C1 C2 115.5(4) . . . . ? Cl1 Ir1 C1 C2 -165.1(3) . . . . ? N1 Ir1 C1 C6 47.5(5) . . . . ? C2 Ir1 C1 C6 122.4(6) . . . . ? C3 Ir1 C1 C6 159.1(5) . . . . ? C4 Ir1 C1 C6 -158.0(5) . . . . ? C5 Ir1 C1 C6 -122.2(5) . . . . ? Cl1 Ir1 C1 C6 -42.7(5) . . . . ? C5 C1 C2 C3 3.4(5) . . . . ? C6 C1 C2 C3 177.8(5) . . . . ? Ir1 C1 C2 C3 -61.1(3) . . . . ? C5 C1 C2 C7 -175.5(5) . . . . ? C6 C1 C2 C7 -1.1(8) . . . . ? Ir1 C1 C2 C7 120.0(5) . . . . ? C5 C1 C2 Ir1 64.5(3) . . . . ? C6 C1 C2 Ir1 -121.1(5) . . . . ? N1 Ir1 C2 C3 -126.7(3) . . . . ? C1 Ir1 C2 C3 118.8(4) . . . . ? N2 Ir1 C2 C3 -50.1(4) . . . . ? C4 Ir1 C2 C3 37.8(3) . . . . ? C5 Ir1 C2 C3 79.9(3) . . . . ? Cl1 Ir1 C2 C3 141.4(2) . . . . ? N1 Ir1 C2 C1 114.5(3) . . . . ? N2 Ir1 C2 C1 -169.0(3) . . . . ? C3 Ir1 C2 C1 -118.8(4) . . . . ? C4 Ir1 C2 C1 -81.0(3) . . . . ? C5 Ir1 C2 C1 -38.9(3) . . . . ? Cl1 Ir1 C2 C1 22.6(4) . . . . ? N1 Ir1 C2 C7 -6.3(4) . . . . ? C1 Ir1 C2 C7 -120.8(5) . . . . ? N2 Ir1 C2 C7 70.3(5) . . . . ? C3 Ir1 C2 C7 120.4(5) . . . . ? C4 Ir1 C2 C7 158.2(5) . . . . ? C5 Ir1 C2 C7 -159.7(5) . . . . ? Cl1 Ir1 C2 C7 -98.2(4) . . . . ? C1 C2 C3 C4 -1.6(5) . . . . ? C7 C2 C3 C4 177.3(5) . . . . ? Ir1 C2 C3 C4 -61.2(3) . . . . ? C1 C2 C3 C8 -173.9(4) . . . . ? C7 C2 C3 C8 5.0(8) . . . . ? Ir1 C2 C3 C8 126.5(5) . . . . ? C1 C2 C3 Ir1 59.6(3) . . . . ? C7 C2 C3 Ir1 -121.5(5) . . . . ? N1 Ir1 C3 C2 63.7(3) . . . . ? C1 Ir1 C3 C2 -37.7(3) . . . . ? N2 Ir1 C3 C2 147.5(2) . . . . ? C4 Ir1 C3 C2 -117.9(4) . . . . ? C5 Ir1 C3 C2 -80.8(3) . . . . ? Cl1 Ir1 C3 C2 -99.7(3) . . . . ? N1 Ir1 C3 C4 -178.4(2) . . . . ? C1 Ir1 C3 C4 80.2(3) . . . . ? N2 Ir1 C3 C4 -94.7(3) . . . . ? C2 Ir1 C3 C4 117.9(4) . . . . ? C5 Ir1 C3 C4 37.0(3) . . . . ? Cl1 Ir1 C3 C4 18.2(5) . . . . ? N1 Ir1 C3 C8 -55.2(5) . . . . ? C1 Ir1 C3 C8 -156.6(5) . . . . ? N2 Ir1 C3 C8 28.5(5) . . . . ? C2 Ir1 C3 C8 -118.9(5) . . . . ? C4 Ir1 C3 C8 123.2(6) . . . . ? C5 Ir1 C3 C8 160.2(5) . . . . ? Cl1 Ir1 C3 C8 141.4(4) . . . . ? C2 C3 C4 C5 -0.8(5) . . . . ? C8 C3 C4 C5 171.2(5) . . . . ? Ir1 C3 C4 C5 -61.5(3) . . . . ? C2 C3 C4 C9 -173.6(4) . . . . ? C8 C3 C4 C9 -1.6(8) . . . . ? Ir1 C3 C4 C9 125.7(5) . . . . ? C2 C3 C4 Ir1 60.8(3) . . . . ? C8 C3 C4 Ir1 -127.3(5) . . . . ? N1 Ir1 C4 C5 121.5(4) . . . . ? C1 Ir1 C4 C5 36.8(3) . . . . ? N2 Ir1 C4 C5 -143.5(3) . . . . ? C2 Ir1 C4 C5 80.5(3) . . . . ? C3 Ir1 C4 C5 118.0(4) . . . . ? Cl1 Ir1 C4 C5 -53.7(3) . . . . ? N1 Ir1 C4 C3 3.5(5) . . . . ? C1 Ir1 C4 C3 -81.1(3) . . . . ? N2 Ir1 C4 C3 98.6(3) . . . . ? C2 Ir1 C4 C3 -37.4(3) . . . . ? C5 Ir1 C4 C3 -118.0(4) . . . . ? Cl1 Ir1 C4 C3 -171.6(2) . . . . ? N1 Ir1 C4 C9 -117.3(5) . . . . ? C1 Ir1 C4 C9 158.0(5) . . . . ? N2 Ir1 C4 C9 -22.3(5) . . . . ? C2 Ir1 C4 C9 -158.3(5) . . . . ? C3 Ir1 C4 C9 -120.8(5) . . . . ? C5 Ir1 C4 C9 121.2(5) . . . . ? Cl1 Ir1 C4 C9 67.5(4) . . . . ? C3 C4 C5 C1 2.9(5) . . . . ? C9 C4 C5 C1 175.7(5) . . . . ? Ir1 C4 C5 C1 -58.1(3) . . . . ? C3 C4 C5 C10 -176.8(4) . . . . ? C9 C4 C5 C10 -4.0(8) . . . . ? Ir1 C4 C5 C10 122.2(5) . . . . ? C3 C4 C5 Ir1 61.1(3) . . . . ? C9 C4 C5 Ir1 -126.2(5) . . . . ? C2 C1 C5 C4 -3.9(6) . . . . ? C6 C1 C5 C4 -178.3(5) . . . . ? Ir1 C1 C5 C4 59.8(3) . . . . ? C2 C1 C5 C10 175.8(5) . . . . ? C6 C1 C5 C10 1.4(8) . . . . ? Ir1 C1 C5 C10 -120.5(5) . . . . ? C2 C1 C5 Ir1 -63.7(3) . . . . ? C6 C1 C5 Ir1 121.9(5) . . . . ? N1 Ir1 C5 C4 -138.8(3) . . . . ? C1 Ir1 C5 C4 -120.0(4) . . . . ? N2 Ir1 C5 C4 53.4(3) . . . . ? C2 Ir1 C5 C4 -80.7(3) . . . . ? C3 Ir1 C5 C4 -37.9(3) . . . . ? Cl1 Ir1 C5 C4 134.4(3) . . . . ? N1 Ir1 C5 C1 -18.8(4) . . . . ? N2 Ir1 C5 C1 173.5(2) . . . . ? C2 Ir1 C5 C1 39.4(3) . . . . ? C3 Ir1 C5 C1 82.2(3) . . . . ? C4 Ir1 C5 C1 120.0(4) . . . . ? Cl1 Ir1 C5 C1 -105.5(2) . . . . ? N1 Ir1 C5 C10 100.6(5) . . . . ? C1 Ir1 C5 C10 119.4(6) . . . . ? N2 Ir1 C5 C10 -67.1(5) . . . . ? C2 Ir1 C5 C10 158.8(5) . . . . ? C3 Ir1 C5 C10 -158.4(5) . . . . ? C4 Ir1 C5 C10 -120.5(6) . . . . ? Cl1 Ir1 C5 C10 13.9(5) . . . . ? C14 N1 C11 C12 -0.8(5) . . . . ? Ir1 N1 C11 C12 -177.9(3) . . . . ? N1 C11 C12 N3 0.7(5) . . . . ? C14 N3 C12 C11 -0.4(5) . . . . ? C13 N3 C12 C11 -174.0(5) . . . . ? C11 N1 C14 N3 0.5(5) . . . . ? Ir1 N1 C14 N3 178.4(3) . . . . ? C11 N1 C14 C15 -176.0(4) . . . . ? Ir1 N1 C14 C15 1.9(5) . . . . ? C12 N3 C14 N1 -0.1(5) . . . . ? C13 N3 C14 N1 173.7(4) . . . . ? C12 N3 C14 C15 175.9(4) . . . . ? C13 N3 C14 C15 -10.3(8) . . . . ? C16 N2 C15 C14 168.7(4) . . . . ? Ir1 N2 C15 C14 3.3(5) . . . . ? N1 C14 C15 N2 -3.5(6) . . . . ? N3 C14 C15 N2 -179.3(4) . . . . ? C15 N2 C16 C18 102.9(4) . . . . ? Ir1 N2 C16 C18 -92.9(4) . . . . ? C15 N2 C16 C17 -22.6(5) . . . . ? Ir1 N2 C16 C17 141.6(3) . . . . ? N2 C16 C18 C19 -15.9(6) . . . . ? C17 C16 C18 C19 110.9(5) . . . . ? N2 C16 C18 C23 166.8(4) . . . . ? C17 C16 C18 C23 -66.3(5) . . . . ? C23 C18 C19 C20 -0.1(7) . . . . ? C16 C18 C19 C20 -177.4(5) . . . . ? C18 C19 C20 C21 -0.2(8) . . . . ? C19 C20 C21 C22 -0.4(9) . . . . ? C20 C21 C22 C23 1.2(9) . . . . ? C21 C22 C23 C18 -1.5(8) . . . . ? C19 C18 C23 C22 0.9(7) . . . . ? C16 C18 C23 C22 178.4(5) . . . . ? N32 Ir31 N31 C44 -4.7(3) . . . . ? C34 Ir31 N31 C44 -170.2(3) . . . . ? C33 Ir31 N31 C44 -130.2(3) . . . . ? C32 Ir31 N31 C44 -99.6(3) . . . . ? C35 Ir31 N31 C44 170.2(3) . . . . ? C31 Ir31 N31 C44 -113.6(6) . . . . ? Cl31 Ir31 N31 C44 81.1(3) . . . . ? N32 Ir31 N31 C41 178.8(4) . . . . ? C34 Ir31 N31 C41 13.2(5) . . . . ? C33 Ir31 N31 C41 53.3(5) . . . . ? C32 Ir31 N31 C41 83.9(5) . . . . ? C35 Ir31 N31 C41 -6.3(5) . . . . ? C31 Ir31 N31 C41 69.8(7) . . . . ? Cl31 Ir31 N31 C41 -95.4(4) . . . . ? N31 Ir31 N32 C45 3.8(3) . . . . ? C34 Ir31 N32 C45 102.8(7) . . . . ? C33 Ir31 N32 C45 93.4(3) . . . . ? C32 Ir31 N32 C45 126.2(3) . . . . ? C35 Ir31 N32 C45 -170.8(3) . . . . ? C31 Ir31 N32 C45 165.9(3) . . . . ? Cl31 Ir31 N32 C45 -82.1(3) . . . . ? N31 Ir31 N32 C46 -177.9(3) . . . . ? C34 Ir31 N32 C46 -78.9(8) . . . . ? C33 Ir31 N32 C46 -88.3(3) . . . . ? C32 Ir31 N32 C46 -55.5(3) . . . . ? C35 Ir31 N32 C46 7.4(4) . . . . ? C31 Ir31 N32 C46 -15.9(3) . . . . ? Cl31 Ir31 N32 C46 96.2(3) . . . . ? N31 Ir31 C31 C32 18.8(7) . . . . ? N32 Ir31 C31 C32 -85.2(3) . . . . ? C34 Ir31 C31 C32 81.0(3) . . . . ? C33 Ir31 C31 C32 36.9(3) . . . . ? C35 Ir31 C31 C32 117.2(4) . . . . ? Cl31 Ir31 C31 C32 -177.1(2) . . . . ? N31 Ir31 C31 C35 -98.4(6) . . . . ? N32 Ir31 C31 C35 157.6(3) . . . . ? C34 Ir31 C31 C35 -36.2(3) . . . . ? C33 Ir31 C31 C35 -80.3(3) . . . . ? C32 Ir31 C31 C35 -117.2(4) . . . . ? Cl31 Ir31 C31 C35 65.7(3) . . . . ? N31 Ir31 C31 C36 140.6(5) . . . . ? N32 Ir31 C31 C36 36.6(5) . . . . ? C34 Ir31 C31 C36 -157.2(5) . . . . ? C33 Ir31 C31 C36 158.7(5) . . . . ? C32 Ir31 C31 C36 121.8(6) . . . . ? C35 Ir31 C31 C36 -121.0(6) . . . . ? Cl31 Ir31 C31 C36 -55.4(5) . . . . ? C35 C31 C32 C33 0.1(5) . . . . ? C36 C31 C32 C33 174.0(5) . . . . ? Ir31 C31 C32 C33 -60.9(3) . . . . ? C35 C31 C32 C37 -174.9(4) . . . . ? C36 C31 C32 C37 -0.9(8) . . . . ? Ir31 C31 C32 C37 124.1(5) . . . . ? C35 C31 C32 Ir31 61.0(3) . . . . ? C36 C31 C32 Ir31 -125.1(5) . . . . ? N31 Ir31 C32 C33 -54.1(3) . . . . ? N32 Ir31 C32 C33 -135.5(3) . . . . ? C34 Ir31 C32 C33 38.4(3) . . . . ? C35 Ir31 C32 C33 81.0(3) . . . . ? C31 Ir31 C32 C33 119.0(4) . . . . ? Cl31 Ir31 C32 C33 124.6(3) . . . . ? N31 Ir31 C32 C31 -173.1(3) . . . . ? N32 Ir31 C32 C31 105.4(3) . . . . ? C34 Ir31 C32 C31 -80.7(3) . . . . ? C33 Ir31 C32 C31 -119.0(4) . . . . ? C35 Ir31 C32 C31 -38.0(3) . . . . ? Cl31 Ir31 C32 C31 5.6(5) . . . . ? N31 Ir31 C32 C37 65.4(5) . . . . ? N32 Ir31 C32 C37 -16.0(5) . . . . ? C34 Ir31 C32 C37 157.9(5) . . . . ? C33 Ir31 C32 C37 119.5(5) . . . . ? C35 Ir31 C32 C37 -159.5(5) . . . . ? C31 Ir31 C32 C37 -121.5(6) . . . . ? Cl31 Ir31 C32 C37 -115.9(4) . . . . ? C31 C32 C33 C34 1.4(5) . . . . ? C37 C32 C33 C34 176.5(4) . . . . ? Ir31 C32 C33 C34 -60.1(3) . . . . ? C31 C32 C33 C38 -177.0(4) . . . . ? C37 C32 C33 C38 -1.9(7) . . . . ? Ir31 C32 C33 C38 121.5(5) . . . . ? C31 C32 C33 Ir31 61.5(3) . . . . ? C37 C32 C33 Ir31 -123.4(4) . . . . ? N31 Ir31 C33 C32 137.3(3) . . . . ? N32 Ir31 C33 C32 58.4(3) . . . . ? C34 Ir31 C33 C32 -118.1(4) . . . . ? C35 Ir31 C33 C32 -80.1(3) . . . . ? C31 Ir31 C33 C32 -37.2(3) . . . . ? Cl31 Ir31 C33 C32 -130.4(3) . . . . ? N31 Ir31 C33 C34 -104.6(3) . . . . ? N32 Ir31 C33 C34 176.4(2) . . . . ? C32 Ir31 C33 C34 118.1(4) . . . . ? C35 Ir31 C33 C34 38.0(3) . . . . ? C31 Ir31 C33 C34 80.9(3) . . . . ? Cl31 Ir31 C33 C34 -12.3(4) . . . . ? N31 Ir31 C33 C38 16.8(4) . . . . ? N32 Ir31 C33 C38 -62.2(5) . . . . ? C34 Ir31 C33 C38 121.4(5) . . . . ? C32 Ir31 C33 C38 -120.5(5) . . . . ? C35 Ir31 C33 C38 159.4(5) . . . . ? C31 Ir31 C33 C38 -157.7(5) . . . . ? Cl31 Ir31 C33 C38 109.1(4) . . . . ? C32 C33 C34 C35 -2.4(5) . . . . ? C38 C33 C34 C35 175.9(4) . . . . ? Ir31 C33 C34 C35 -63.3(3) . . . . ? C32 C33 C34 C39 -176.6(5) . . . . ? C38 C33 C34 C39 1.7(8) . . . . ? Ir31 C33 C34 C39 122.5(5) . . . . ? C32 C33 C34 Ir31 60.8(3) . . . . ? C38 C33 C34 Ir31 -120.8(5) . . . . ? N31 Ir31 C34 C35 -160.0(2) . . . . ? N32 Ir31 C34 C35 104.6(7) . . . . ? C33 Ir31 C34 C35 116.5(4) . . . . ? C32 Ir31 C34 C35 79.3(3) . . . . ? C31 Ir31 C34 C35 36.5(3) . . . . ? Cl31 Ir31 C34 C35 -70.2(3) . . . . ? N31 Ir31 C34 C33 83.6(3) . . . . ? N32 Ir31 C34 C33 -11.9(8) . . . . ? C32 Ir31 C34 C33 -37.2(3) . . . . ? C35 Ir31 C34 C33 -116.5(4) . . . . ? C31 Ir31 C34 C33 -80.0(3) . . . . ? Cl31 Ir31 C34 C33 173.3(2) . . . . ? N31 Ir31 C34 C39 -39.1(5) . . . . ? N32 Ir31 C34 C39 -134.5(6) . . . . ? C33 Ir31 C34 C39 -122.7(6) . . . . ? C32 Ir31 C34 C39 -159.8(5) . . . . ? C35 Ir31 C34 C39 120.9(6) . . . . ? C31 Ir31 C34 C39 157.3(5) . . . . ? Cl31 Ir31 C34 C39 50.6(5) . . . . ? C33 C34 C35 C31 2.5(5) . . . . ? C39 C34 C35 C31 176.9(4) . . . . ? Ir31 C34 C35 C31 -59.7(3) . . . . ? C33 C34 C35 C40 -177.7(4) . . . . ? C39 C34 C35 C40 -3.4(7) . . . . ? Ir31 C34 C35 C40 120.1(4) . . . . ? C33 C34 C35 Ir31 62.2(3) . . . . ? C39 C34 C35 Ir31 -123.5(5) . . . . ? C32 C31 C35 C34 -1.6(5) . . . . ? C36 C31 C35 C34 -175.7(4) . . . . ? Ir31 C31 C35 C34 58.8(3) . . . . ? C32 C31 C35 C40 178.6(4) . . . . ? C36 C31 C35 C40 4.6(7) . . . . ? Ir31 C31 C35 C40 -121.0(4) . . . . ? C32 C31 C35 Ir31 -60.4(3) . . . . ? C36 C31 C35 Ir31 125.6(5) . . . . ? N31 Ir31 C35 C34 31.2(4) . . . . ? N32 Ir31 C35 C34 -157.0(2) . . . . ? C33 Ir31 C35 C34 -39.3(3) . . . . ? C32 Ir31 C35 C34 -82.2(3) . . . . ? C31 Ir31 C35 C34 -120.3(4) . . . . ? Cl31 Ir31 C35 C34 117.2(2) . . . . ? N31 Ir31 C35 C31 151.4(3) . . . . ? N32 Ir31 C35 C31 -36.8(4) . . . . ? C34 Ir31 C35 C31 120.3(4) . . . . ? C33 Ir31 C35 C31 81.0(3) . . . . ? C32 Ir31 C35 C31 38.1(3) . . . . ? Cl31 Ir31 C35 C31 -122.6(2) . . . . ? N31 Ir31 C35 C40 -88.7(6) . . . . ? N32 Ir31 C35 C40 83.1(6) . . . . ? C34 Ir31 C35 C40 -119.9(6) . . . . ? C33 Ir31 C35 C40 -159.2(6) . . . . ? C32 Ir31 C35 C40 157.9(6) . . . . ? C31 Ir31 C35 C40 119.8(6) . . . . ? Cl31 Ir31 C35 C40 -2.7(5) . . . . ? C44 N31 C41 C42 0.6(5) . . . . ? Ir31 N31 C41 C42 177.3(3) . . . . ? N31 C41 C42 N33 -0.8(5) . . . . ? C44 N33 C42 C41 0.7(5) . . . . ? C43 N33 C42 C41 -180.0(4) . . . . ? C41 N31 C44 N33 -0.2(4) . . . . ? Ir31 N31 C44 N33 -177.8(2) . . . . ? C41 N31 C44 C45 -177.1(3) . . . . ? Ir31 N31 C44 C45 5.2(4) . . . . ? C42 N33 C44 N31 -0.3(4) . . . . ? C43 N33 C44 N31 -179.7(4) . . . . ? C42 N33 C44 C45 176.2(4) . . . . ? C43 N33 C44 C45 -3.2(7) . . . . ? C46 N32 C45 C44 179.4(3) . . . . ? Ir31 N32 C45 C44 -2.2(4) . . . . ? N31 C44 C45 N32 -2.0(5) . . . . ? N33 C44 C45 N32 -178.3(4) . . . . ? C45 N32 C46 C48 92.5(5) . . . . ? Ir31 N32 C46 C48 -85.7(4) . . . . ? C45 N32 C46 C47 -34.3(5) . . . . ? Ir31 N32 C46 C47 147.5(3) . . . . ? N32 C46 C48 C53 -52.5(6) . . . . ? C47 C46 C48 C53 74.7(5) . . . . ? N32 C46 C48 C49 130.8(5) . . . . ? C47 C46 C48 C49 -102.0(5) . . . . ? C53 C48 C49 C50 0.1(9) . . . . ? C46 C48 C49 C50 176.9(5) . . . . ? C48 C49 C50 C51 -0.6(10) . . . . ? C49 C50 C51 C52 0.5(10) . . . . ? C50 C51 C52 C53 0.1(9) . . . . ? C49 C48 C53 C52 0.6(8) . . . . ? C46 C48 C53 C52 -176.2(5) . . . . ? C51 C52 C53 C48 -0.7(8) . . . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.907 _refine_diff_density_min -0.535 _refine_diff_density_rms 0.113 _database_code_depnum_ccdc_archive 'CCDC 937403' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_cmpnd_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H32 Cl Ir N3, F6 Sb' _chemical_formula_sum 'C27 H32 Cl F6 Ir N3 Sb' _chemical_formula_weight 861.96 _chemical_absolute_configuration rmad 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' F F 0.0171 0.0103 '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' Sb Sb -0.5866 1.5461 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.8788(15) _cell_length_b 22.480(3) _cell_length_c 12.2248(17) _cell_angle_alpha 90.00 _cell_angle_beta 100.898(2) _cell_angle_gamma 90.00 _cell_volume 2935.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11281 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 28.78 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.135 _exptl_crystal_size_mid 0.106 _exptl_crystal_size_min 0.094 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.950 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 5.599 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.481 _exptl_absorpt_correction_T_max 0.637 _exptl_absorpt_process_details ; Multi-scan absorption included in APEX2 package (Bruker AXS, 2008). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX DUO system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_standards_decay_% 0 _diffrn_reflns_number 32638 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0526 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 29.63 _reflns_number_total 14641 _reflns_number_gt 13218 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_cell_refinement 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_data_reduction 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP program, SHELXTL v6.12, Bruker2000' _computing_publication_material ENCIFER _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Maximal residual density peaks are found in the proximity the metal atoms. They have no chemical sense. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.014(4) _refine_ls_number_reflns 14641 _refine_ls_number_parameters 717 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0784 _refine_ls_wR_factor_gt 0.0751 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL fjl127ds in P2(1) CELL 0.71073 10.8788 22.4801 12.2248 90.000 100.898 90.000 ZERR 4.00 0.0015 0.0032 0.0017 0.000 0.002 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N F CL SB IR UNIT 108 128 12 24 4 4 4 MERG 2 FMAP 2 PLAN 10 ACTA 55 BOND $H CONF L.S. 4 TEMP -173.00 WGHT 0.042500 FVAR 0.19284 IR1 7 0.185054 0.805845 0.150707 11.00000 0.01684 0.01873 = 0.02293 -0.00273 0.00607 -0.00199 CL1 5 0.102376 0.781867 -0.040004 11.00000 0.02538 0.03102 = 0.02135 -0.00416 0.00589 -0.00022 N1 3 0.210797 0.715554 0.182908 11.00000 0.01777 0.02760 = 0.02815 -0.00133 0.00396 0.00279 N2 3 0.004129 0.775534 0.165635 11.00000 0.01389 0.02152 = 0.02349 -0.00182 0.00526 0.00007 N3 3 0.134578 0.629628 0.223771 11.00000 0.02606 0.01667 = 0.03290 0.00065 -0.00298 0.00408 C1 1 0.195129 0.901483 0.159930 11.00000 0.02777 0.01655 = 0.04174 -0.00257 0.00417 -0.00899 C2 1 0.291084 0.880654 0.103187 11.00000 0.03065 0.01987 = 0.03374 -0.00779 0.01367 -0.01145 C3 1 0.371468 0.841481 0.177162 11.00000 0.02381 0.02257 = 0.03827 -0.00573 0.00736 -0.00629 C4 1 0.328751 0.839904 0.280953 11.00000 0.02169 0.02735 = 0.03257 -0.00751 0.00529 -0.01223 C5 1 0.221011 0.876623 0.270680 11.00000 0.02874 0.02181 = 0.03576 -0.01430 0.01081 -0.01498 C6 1 0.092486 0.945147 0.113705 11.00000 0.03739 0.02470 = 0.05707 -0.00326 0.01366 -0.00511 AFIX 137 H6A 2 0.125231 0.985799 0.123611 11.00000 -1.50000 H6B 2 0.022735 0.940607 0.153367 11.00000 -1.50000 H6C 2 0.063036 0.937304 0.034211 11.00000 -1.50000 AFIX 0 C7 1 0.305657 0.894442 -0.013055 11.00000 0.04504 0.03054 = 0.03448 0.00067 0.01442 -0.01487 AFIX 137 H7A 2 0.228916 0.913146 -0.053288 11.00000 -1.50000 H7B 2 0.321289 0.857561 -0.050922 11.00000 -1.50000 H7C 2 0.376339 0.921679 -0.011311 11.00000 -1.50000 AFIX 0 C8 1 0.486008 0.812392 0.150601 11.00000 0.01873 0.04268 = 0.06999 -0.01219 0.01472 -0.00646 AFIX 137 H8A 2 0.465709 0.793891 0.076799 11.00000 -1.50000 H8B 2 0.515806 0.781880 0.206607 11.00000 -1.50000 H8C 2 0.551529 0.842353 0.151000 11.00000 -1.50000 AFIX 0 C9 1 0.390574 0.807293 0.383401 11.00000 0.03865 0.05119 = 0.03743 -0.00498 -0.00402 -0.01160 AFIX 137 H9A 2 0.453339 0.833069 0.428189 11.00000 -1.50000 H9B 2 0.431368 0.771421 0.361905 11.00000 -1.50000 H9C 2 0.327498 0.796036 0.427192 11.00000 -1.50000 AFIX 0 C10 1 0.153056 0.890649 0.364434 11.00000 0.03736 0.03517 = 0.03584 -0.01703 0.01365 -0.01615 AFIX 137 H10A 2 0.145714 0.854410 0.407295 11.00000 -1.50000 H10B 2 0.069306 0.905909 0.333525 11.00000 -1.50000 H10C 2 0.200044 0.920731 0.413333 11.00000 -1.50000 AFIX 0 C11 1 0.305570 0.674420 0.195359 11.00000 0.02571 0.03270 = 0.03551 -0.00350 0.00148 0.01488 AFIX 43 H11 2 0.389392 0.681840 0.187381 11.00000 -1.20000 AFIX 0 C12 1 0.258807 0.621125 0.221124 11.00000 0.03144 0.03251 = 0.03664 -0.00112 -0.00267 0.01159 AFIX 43 H12 2 0.303831 0.584830 0.234726 11.00000 -1.20000 AFIX 0 C13 1 0.049380 0.583923 0.251841 11.00000 0.03588 0.01895 = 0.06897 0.01173 -0.00510 -0.00248 AFIX 137 H13A 2 -0.000519 0.600603 0.303315 11.00000 -1.50000 H13B 2 0.098165 0.550085 0.287197 11.00000 -1.50000 H13C 2 -0.006413 0.570554 0.183760 11.00000 -1.50000 AFIX 0 C14 1 0.108837 0.687246 0.200603 11.00000 0.02611 0.02035 = 0.01924 -0.00344 0.00210 -0.00223 C15 1 -0.006048 0.719765 0.185795 11.00000 0.02021 0.01585 = 0.02975 -0.00028 0.00618 -0.00029 AFIX 43 H15 2 -0.083759 0.701628 0.190473 11.00000 -1.20000 AFIX 0 C16 1 -0.108900 0.813326 0.128116 11.00000 0.01824 0.01916 = 0.02211 -0.00049 0.00489 0.00206 AFIX 13 H16 2 -0.085572 0.844226 0.076840 11.00000 -1.20000 AFIX 0 C17 1 -0.217604 0.777535 0.061857 11.00000 0.02493 0.02534 = 0.02565 -0.00262 0.00125 0.00096 AFIX 137 H17A 2 -0.186409 0.751737 0.008514 11.00000 -1.50000 H17B 2 -0.280542 0.804838 0.021589 11.00000 -1.50000 H17C 2 -0.255505 0.753099 0.113015 11.00000 -1.50000 AFIX 0 C18 1 -0.150433 0.845916 0.223967 11.00000 0.01462 0.02257 = 0.02098 -0.00055 0.00373 -0.00200 C19 1 -0.125952 0.824386 0.330282 11.00000 0.02913 0.01822 = 0.02180 0.00165 0.00727 0.00210 AFIX 43 H19 2 -0.075181 0.789948 0.346593 11.00000 -1.20000 AFIX 0 C20 1 -0.174451 0.852200 0.416324 11.00000 0.04407 0.03146 = 0.02107 0.00264 0.00678 0.00410 AFIX 43 H20 2 -0.153991 0.836989 0.490030 11.00000 -1.20000 AFIX 0 C21 1 -0.249334 0.900011 0.395241 11.00000 0.03057 0.03327 = 0.02375 -0.00105 0.01082 -0.00059 AFIX 43 H21 2 -0.282104 0.917719 0.454215 11.00000 -1.20000 AFIX 0 C22 1 -0.279958 0.924210 0.288094 11.00000 0.01982 0.02298 = 0.02832 -0.00507 0.00785 -0.00363 C23 1 -0.360466 0.974018 0.261801 11.00000 0.02371 0.02209 = 0.03846 -0.01036 0.00710 0.00478 AFIX 43 H23 2 -0.397415 0.991266 0.318755 11.00000 -1.20000 AFIX 0 C24 1 -0.385698 0.997215 0.160247 11.00000 0.02824 0.02434 = 0.03869 -0.00760 0.00178 -0.00011 AFIX 43 H24 2 -0.440329 1.030440 0.145841 11.00000 -1.20000 AFIX 0 C25 1 -0.332177 0.973046 0.073072 11.00000 0.02947 0.02966 = 0.02544 0.00338 -0.00406 0.00340 AFIX 43 H25 2 -0.349590 0.990459 0.000990 11.00000 -1.20000 AFIX 0 C26 1 -0.255072 0.924386 0.093073 11.00000 0.02105 0.02007 = 0.02693 -0.00229 0.00513 0.00027 AFIX 43 H26 2 -0.220127 0.908081 0.034087 11.00000 -1.20000 AFIX 0 C27 1 -0.226756 0.898125 0.199765 11.00000 0.01678 0.01126 = 0.02437 -0.00132 0.00241 -0.00310 IR31 7 0.829759 0.192065 0.336115 11.00000 0.01501 0.01937 = 0.02174 0.00044 0.00416 -0.00328 CL31 5 0.884729 0.215681 0.530608 11.00000 0.02562 0.03064 = 0.02367 -0.00286 0.00627 -0.00620 N31 3 0.796917 0.282869 0.319268 11.00000 0.02208 0.01429 = 0.02061 0.00218 0.00345 0.00005 N32 3 1.003806 0.226448 0.312437 11.00000 0.01775 0.01477 = 0.01720 0.00222 0.00288 -0.00106 N33 3 0.868961 0.373256 0.303644 11.00000 0.02026 0.01751 = 0.03779 0.00223 0.00721 0.00050 C31 1 0.826375 0.096975 0.310686 11.00000 0.02818 0.01673 = 0.04042 -0.00257 0.00499 -0.00458 C32 1 0.729249 0.112457 0.369910 11.00000 0.02565 0.02641 = 0.02868 -0.00028 0.00054 -0.00630 C33 1 0.645686 0.153125 0.304378 11.00000 0.01504 0.03073 = 0.02932 -0.00325 0.00566 -0.00970 C34 1 0.689428 0.161285 0.200329 11.00000 0.02498 0.03083 = 0.02648 -0.00068 0.00759 -0.01304 C35 1 0.798281 0.126505 0.203701 11.00000 0.02868 0.02729 = 0.02593 -0.00675 0.00523 -0.01461 C36 1 0.928092 0.052352 0.347812 11.00000 0.03202 0.01848 = 0.08098 0.00412 0.01261 -0.00515 AFIX 137 H36A 2 0.898439 0.012645 0.322242 11.00000 -1.50000 H36B 2 0.950708 0.052583 0.429307 11.00000 -1.50000 H36C 2 1.001630 0.062652 0.316161 11.00000 -1.50000 AFIX 0 C37 1 0.716648 0.089993 0.482127 11.00000 0.03996 0.03955 = 0.03369 0.00738 0.00683 -0.01829 AFIX 137 H37A 2 0.703181 0.123588 0.529576 11.00000 -1.50000 H37B 2 0.793263 0.068899 0.515978 11.00000 -1.50000 H37C 2 0.645223 0.062741 0.474521 11.00000 -1.50000 AFIX 0 C38 1 0.530294 0.178263 0.335356 11.00000 0.01982 0.03906 = 0.05968 -0.00403 0.01575 -0.00469 AFIX 137 H38A 2 0.460503 0.150576 0.312887 11.00000 -1.50000 H38B 2 0.510391 0.216436 0.297418 11.00000 -1.50000 H38C 2 0.544062 0.184315 0.416144 11.00000 -1.50000 AFIX 0 C39 1 0.627086 0.197696 0.104000 11.00000 0.03008 0.05898 = 0.03105 0.01018 -0.00945 -0.02066 AFIX 137 H39A 2 0.689989 0.221424 0.075837 11.00000 -1.50000 H39B 2 0.565737 0.224241 0.127879 11.00000 -1.50000 H39C 2 0.584480 0.171402 0.044848 11.00000 -1.50000 AFIX 0 C40 1 0.864869 0.118704 0.108174 11.00000 0.04107 0.03982 = 0.04505 -0.01860 0.01985 -0.01363 AFIX 137 H40A 2 0.809832 0.098123 0.047135 11.00000 -1.50000 H40B 2 0.940882 0.095099 0.132365 11.00000 -1.50000 H40C 2 0.887501 0.157781 0.082460 11.00000 -1.50000 AFIX 0 C41 1 0.701270 0.322417 0.321014 11.00000 0.01833 0.03058 = 0.03775 0.00001 0.00914 0.00719 AFIX 43 H41 2 0.618315 0.312309 0.328001 11.00000 -1.20000 AFIX 0 C42 1 0.744666 0.378280 0.311126 11.00000 0.02247 0.02566 = 0.03165 -0.00130 0.00292 0.00911 AFIX 43 H42 2 0.698142 0.414129 0.309637 11.00000 -1.20000 AFIX 0 C43 1 0.952705 0.422681 0.290407 11.00000 0.03221 0.01859 = 0.07193 0.00413 0.01834 -0.00542 AFIX 137 H43A 2 1.009890 0.429973 0.361260 11.00000 -1.50000 H43B 2 0.903068 0.458540 0.268028 11.00000 -1.50000 H43C 2 1.001173 0.412589 0.233077 11.00000 -1.50000 AFIX 0 C44 1 0.896572 0.315489 0.308991 11.00000 0.01908 0.01663 = 0.02286 0.00196 0.00485 0.00162 C45 1 1.009885 0.283311 0.302860 11.00000 0.01694 0.01898 = 0.01971 0.00288 0.00193 0.00043 AFIX 43 H45 2 1.084209 0.302875 0.292419 11.00000 -1.20000 AFIX 0 C46 1 1.111390 0.188771 0.298441 11.00000 0.01906 0.01561 = 0.02219 -0.00240 0.00200 0.00024 AFIX 13 H46 2 1.076684 0.153244 0.253827 11.00000 -1.20000 AFIX 0 C47 1 1.200351 0.220284 0.233202 11.00000 0.02096 0.03027 = 0.03759 0.00489 0.01345 0.00776 AFIX 137 H47A 2 1.151293 0.240408 0.168211 11.00000 -1.50000 H47B 2 1.255736 0.190884 0.208445 11.00000 -1.50000 H47C 2 1.250700 0.249636 0.281390 11.00000 -1.50000 AFIX 0 C48 1 1.182929 0.166031 0.409194 11.00000 0.01619 0.02062 = 0.02204 0.00238 0.00776 0.00090 C49 1 1.187924 0.197905 0.505079 11.00000 0.02360 0.03027 = 0.02652 -0.00477 0.00058 0.00928 AFIX 43 H49 2 1.143732 0.234510 0.501738 11.00000 -1.20000 AFIX 0 C50 1 1.255596 0.178794 0.608173 11.00000 0.03993 0.04709 = 0.02056 -0.00541 0.00464 0.01385 AFIX 43 H50 2 1.255291 0.202143 0.672894 11.00000 -1.20000 AFIX 0 C51 1 1.321116 0.127571 0.616302 11.00000 0.03078 0.04819 = 0.02633 0.00930 0.00341 0.02031 AFIX 43 H51 2 1.368289 0.115305 0.686134 11.00000 -1.20000 AFIX 0 C52 1 1.319266 0.091811 0.519361 11.00000 0.02317 0.02751 = 0.02378 0.00537 0.00701 0.00430 C53 1 1.388465 0.037441 0.526281 11.00000 0.02902 0.02315 = 0.04119 0.01422 0.01311 0.00902 AFIX 43 H53 2 1.431132 0.023693 0.596782 11.00000 -1.20000 AFIX 0 C54 1 1.393945 0.005641 0.434738 11.00000 0.01961 0.02049 = 0.04962 0.00717 0.00659 0.00186 AFIX 43 H54 2 1.442063 -0.029880 0.440758 11.00000 -1.20000 AFIX 0 C55 1 1.329065 0.024329 0.329571 11.00000 0.02504 0.01530 = 0.04708 -0.00365 0.01143 0.00314 AFIX 43 H55 2 1.333062 0.001157 0.265351 11.00000 -1.20000 AFIX 0 C56 1 1.259910 0.075985 0.319371 11.00000 0.01904 0.01940 = 0.02922 0.00081 0.00525 -0.00307 AFIX 43 H56 2 1.217281 0.088411 0.247939 11.00000 -1.20000 AFIX 0 C57 1 1.251645 0.110806 0.414263 11.00000 0.01646 0.02137 = 0.02747 0.00200 0.00707 -0.00446 SB1 6 0.297867 0.085398 -0.037515 11.00000 0.02958 0.02693 = 0.02570 0.00090 0.00272 0.00361 F1 4 0.321726 0.025247 0.067857 11.00000 0.05986 0.05083 = 0.04737 0.02190 -0.00194 -0.01216 F2 4 0.267599 0.145597 -0.143511 11.00000 0.10605 0.04376 = 0.04284 0.02014 0.02934 0.03687 F3 4 0.458123 0.074786 -0.067705 11.00000 0.04427 0.04337 = 0.05913 -0.00291 0.02546 0.01256 F4 4 0.137174 0.098090 -0.006626 11.00000 0.02998 0.09168 = 0.06095 -0.01217 0.00952 0.00409 F5 4 0.360827 0.140086 0.073724 11.00000 0.04702 0.05150 = 0.05396 -0.02203 0.01958 -0.01838 F6 4 0.231926 0.030750 -0.148496 11.00000 0.06018 0.04619 = 0.04633 -0.01644 -0.01367 0.01203 SB2 6 0.342866 0.418241 0.270829 11.00000 0.02452 0.03018 = 0.02209 -0.00359 0.00607 -0.00547 F7 4 0.397034 0.359161 0.185096 11.00000 0.05624 0.09099 = 0.06113 -0.04738 0.02395 0.00255 F8 4 0.287513 0.477296 0.357748 11.00000 0.08877 0.03279 = 0.04717 -0.00517 0.01775 0.02465 F9 4 0.248862 0.363131 0.333674 11.00000 0.04544 0.05172 = 0.05152 -0.00454 0.01381 -0.03282 F10 4 0.435468 0.474890 0.211659 11.00000 0.09494 0.10437 = 0.04926 0.02117 0.02249 -0.05555 F11 4 0.478637 0.403204 0.385397 11.00000 0.03026 0.06481 = 0.03782 -0.00185 -0.00272 -0.00079 F12 4 0.204172 0.433444 0.159242 11.00000 0.04309 0.12500 = 0.02880 0.00921 0.00129 0.01344 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 REM fjl127ds in P2(1) REM R1 = 0.0362 for 13218 Fo > 4sig(Fo) and 0.0436 for all 14641 data REM 717 parameters refined using 1 restraints END ; 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.185054(19) 0.805845(10) 0.150707(18) 0.01920(5) Uani 1 1 d . . . Cl1 Cl 0.10238(14) 0.78187(8) -0.04000(13) 0.0257(3) Uani 1 1 d . . . N1 N 0.2108(5) 0.7156(3) 0.1829(5) 0.0246(12) Uani 1 1 d . . . N2 N 0.0041(4) 0.7755(2) 0.1656(4) 0.0194(11) Uani 1 1 d . . . N3 N 0.1346(5) 0.6296(3) 0.2238(5) 0.0263(12) Uani 1 1 d . . . C1 C 0.1951(6) 0.9015(3) 0.1599(6) 0.0290(17) Uani 1 1 d . . . C2 C 0.2911(6) 0.8807(3) 0.1032(6) 0.0271(15) Uani 1 1 d . . . C3 C 0.3715(6) 0.8415(3) 0.1772(6) 0.0280(15) Uani 1 1 d . . . C4 C 0.3288(6) 0.8399(3) 0.2810(6) 0.0272(15) Uani 1 1 d . . . C5 C 0.2210(6) 0.8766(3) 0.2707(6) 0.0282(15) Uani 1 1 d . . . C6 C 0.0925(7) 0.9451(3) 0.1137(7) 0.0391(18) Uani 1 1 d . . . H6A H 0.1252 0.9858 0.1236 0.059 Uiso 1 1 calc R . . H6B H 0.0227 0.9406 0.1534 0.059 Uiso 1 1 calc R . . H6C H 0.0630 0.9373 0.0342 0.059 Uiso 1 1 calc R . . C7 C 0.3057(7) 0.8944(3) -0.0131(6) 0.0358(17) Uani 1 1 d . . . H7A H 0.2289 0.9131 -0.0533 0.054 Uiso 1 1 calc R . . H7B H 0.3213 0.8576 -0.0509 0.054 Uiso 1 1 calc R . . H7C H 0.3763 0.9217 -0.0113 0.054 Uiso 1 1 calc R . . C8 C 0.4860(6) 0.8124(4) 0.1506(7) 0.043(2) Uani 1 1 d . . . H8A H 0.4657 0.7939 0.0768 0.064 Uiso 1 1 calc R . . H8B H 0.5158 0.7819 0.2066 0.064 Uiso 1 1 calc R . . H8C H 0.5515 0.8424 0.1510 0.064 Uiso 1 1 calc R . . C9 C 0.3906(7) 0.8073(5) 0.3834(6) 0.0439(18) Uani 1 1 d . . . H9A H 0.4533 0.8331 0.4282 0.066 Uiso 1 1 calc R . . H9B H 0.4314 0.7714 0.3619 0.066 Uiso 1 1 calc R . . H9C H 0.3275 0.7960 0.4272 0.066 Uiso 1 1 calc R . . C10 C 0.1531(7) 0.8906(3) 0.3644(6) 0.0352(17) Uani 1 1 d . . . H10A H 0.1457 0.8544 0.4073 0.053 Uiso 1 1 calc R . . H10B H 0.0693 0.9059 0.3335 0.053 Uiso 1 1 calc R . . H10C H 0.2000 0.9207 0.4133 0.053 Uiso 1 1 calc R . . C11 C 0.3056(6) 0.6744(3) 0.1954(6) 0.0319(17) Uani 1 1 d . . . H11 H 0.3894 0.6818 0.1874 0.038 Uiso 1 1 calc R . . C12 C 0.2588(7) 0.6211(4) 0.2211(6) 0.0347(17) Uani 1 1 d . . . H12 H 0.3038 0.5848 0.2347 0.042 Uiso 1 1 calc R . . C13 C 0.0494(7) 0.5839(4) 0.2518(7) 0.043(2) Uani 1 1 d . . . H13A H -0.0005 0.6006 0.3033 0.065 Uiso 1 1 calc R . . H13B H 0.0982 0.5501 0.2872 0.065 Uiso 1 1 calc R . . H13C H -0.0064 0.5706 0.1838 0.065 Uiso 1 1 calc R . . C14 C 0.1088(5) 0.6872(3) 0.2006(5) 0.0222(12) Uani 1 1 d . . . C15 C -0.0060(6) 0.7198(3) 0.1858(5) 0.0217(13) Uani 1 1 d . . . H15 H -0.0838 0.7016 0.1905 0.026 Uiso 1 1 calc R . . C16 C -0.1089(5) 0.8133(3) 0.1281(5) 0.0197(12) Uani 1 1 d . . . H16 H -0.0856 0.8442 0.0768 0.024 Uiso 1 1 calc R . . C17 C -0.2176(6) 0.7775(3) 0.0619(5) 0.0258(14) Uani 1 1 d . . . H17A H -0.1864 0.7517 0.0085 0.039 Uiso 1 1 calc R . . H17B H -0.2805 0.8048 0.0216 0.039 Uiso 1 1 calc R . . H17C H -0.2555 0.7531 0.1130 0.039 Uiso 1 1 calc R . . C18 C -0.1504(5) 0.8459(3) 0.2240(5) 0.0193(12) Uani 1 1 d . . . C19 C -0.1260(6) 0.8244(3) 0.3303(5) 0.0227(13) Uani 1 1 d . . . H19 H -0.0752 0.7899 0.3466 0.027 Uiso 1 1 calc R . . C20 C -0.1745(7) 0.8522(3) 0.4163(6) 0.0321(15) Uani 1 1 d . . . H20 H -0.1540 0.8370 0.4900 0.039 Uiso 1 1 calc R . . C21 C -0.2493(6) 0.9000(3) 0.3952(5) 0.0285(15) Uani 1 1 d . . . H21 H -0.2821 0.9177 0.4542 0.034 Uiso 1 1 calc R . . C22 C -0.2800(5) 0.9242(3) 0.2881(5) 0.0233(13) Uani 1 1 d . . . C23 C -0.3605(6) 0.9740(3) 0.2618(6) 0.0279(15) Uani 1 1 d . . . H23 H -0.3974 0.9913 0.3188 0.034 Uiso 1 1 calc R . . C24 C -0.3857(6) 0.9972(3) 0.1602(6) 0.0310(15) Uani 1 1 d . . . H24 H -0.4403 1.0304 0.1458 0.037 Uiso 1 1 calc R . . C25 C -0.3322(6) 0.9730(3) 0.0731(6) 0.0294(15) Uani 1 1 d . . . H25 H -0.3496 0.9905 0.0010 0.035 Uiso 1 1 calc R . . C26 C -0.2551(5) 0.9244(3) 0.0931(5) 0.0226(13) Uani 1 1 d . . . H26 H -0.2201 0.9081 0.0341 0.027 Uiso 1 1 calc R . . C27 C -0.2268(5) 0.8981(3) 0.1998(5) 0.0177(12) Uani 1 1 d . . . Ir31 Ir 0.829759(19) 0.192065(9) 0.336115(18) 0.01862(5) Uani 1 1 d . . . Cl31 Cl 0.88473(14) 0.21568(8) 0.53061(13) 0.0264(3) Uani 1 1 d . . . N31 N 0.7969(5) 0.2829(2) 0.3193(4) 0.0191(11) Uani 1 1 d . . . N32 N 1.0038(4) 0.2264(2) 0.3124(4) 0.0166(10) Uani 1 1 d . . . N33 N 0.8690(5) 0.3733(2) 0.3036(5) 0.0250(12) Uani 1 1 d . . . C31 C 0.8264(6) 0.0970(3) 0.3107(7) 0.0286(15) Uani 1 1 d . . . C32 C 0.7292(6) 0.1125(3) 0.3699(6) 0.0275(14) Uani 1 1 d . . . C33 C 0.6457(5) 0.1531(3) 0.3044(5) 0.0248(14) Uani 1 1 d . . . C34 C 0.6894(6) 0.1613(3) 0.2003(6) 0.0271(15) Uani 1 1 d . . . C35 C 0.7983(6) 0.1265(3) 0.2037(6) 0.0273(14) Uani 1 1 d . . . C36 C 0.9281(7) 0.0524(3) 0.3478(8) 0.044(2) Uani 1 1 d . . . H36A H 0.8984 0.0126 0.3222 0.065 Uiso 1 1 calc R . . H36B H 0.9507 0.0526 0.4293 0.065 Uiso 1 1 calc R . . H36C H 1.0016 0.0627 0.3162 0.065 Uiso 1 1 calc R . . C37 C 0.7166(7) 0.0900(4) 0.4821(6) 0.0377(18) Uani 1 1 d . . . H37A H 0.7032 0.1236 0.5296 0.057 Uiso 1 1 calc R . . H37B H 0.7933 0.0689 0.5160 0.057 Uiso 1 1 calc R . . H37C H 0.6452 0.0627 0.4745 0.057 Uiso 1 1 calc R . . C38 C 0.5303(6) 0.1783(4) 0.3354(7) 0.038(2) Uani 1 1 d . . . H38A H 0.4605 0.1506 0.3129 0.058 Uiso 1 1 calc R . . H38B H 0.5104 0.2164 0.2974 0.058 Uiso 1 1 calc R . . H38C H 0.5441 0.1843 0.4161 0.058 Uiso 1 1 calc R . . C39 C 0.6271(6) 0.1977(4) 0.1040(6) 0.042(2) Uani 1 1 d . . . H39A H 0.6900 0.2214 0.0758 0.063 Uiso 1 1 calc R . . H39B H 0.5657 0.2242 0.1279 0.063 Uiso 1 1 calc R . . H39C H 0.5845 0.1714 0.0448 0.063 Uiso 1 1 calc R . . C40 C 0.8649(7) 0.1187(4) 0.1082(7) 0.0405(19) Uani 1 1 d . . . H40A H 0.8098 0.0981 0.0471 0.061 Uiso 1 1 calc R . . H40B H 0.9409 0.0951 0.1324 0.061 Uiso 1 1 calc R . . H40C H 0.8875 0.1578 0.0825 0.061 Uiso 1 1 calc R . . C41 C 0.7013(6) 0.3224(3) 0.3210(6) 0.0284(16) Uani 1 1 d . . . H41 H 0.6183 0.3123 0.3280 0.034 Uiso 1 1 calc R . . C42 C 0.7447(6) 0.3783(3) 0.3111(6) 0.0269(14) Uani 1 1 d . . . H42 H 0.6981 0.4141 0.3096 0.032 Uiso 1 1 calc R . . C43 C 0.9527(7) 0.4227(3) 0.2904(7) 0.0398(18) Uani 1 1 d . . . H43A H 1.0099 0.4300 0.3613 0.060 Uiso 1 1 calc R . . H43B H 0.9031 0.4585 0.2680 0.060 Uiso 1 1 calc R . . H43C H 1.0012 0.4126 0.2331 0.060 Uiso 1 1 calc R . . C44 C 0.8966(5) 0.3155(3) 0.3090(5) 0.0194(13) Uani 1 1 d . . . C45 C 1.0099(5) 0.2833(3) 0.3029(5) 0.0187(12) Uani 1 1 d . . . H45 H 1.0842 0.3029 0.2924 0.022 Uiso 1 1 calc R . . C46 C 1.1114(5) 0.1888(3) 0.2984(5) 0.0192(11) Uani 1 1 d . . . H46 H 1.0767 0.1532 0.2538 0.023 Uiso 1 1 calc R . . C47 C 1.2004(6) 0.2203(3) 0.2332(6) 0.0286(15) Uani 1 1 d . . . H47A H 1.1513 0.2404 0.1682 0.043 Uiso 1 1 calc R . . H47B H 1.2557 0.1909 0.2084 0.043 Uiso 1 1 calc R . . H47C H 1.2507 0.2496 0.2814 0.043 Uiso 1 1 calc R . . C48 C 1.1829(5) 0.1660(3) 0.4092(5) 0.0191(12) Uani 1 1 d . . . C49 C 1.1879(5) 0.1979(3) 0.5051(5) 0.0273(13) Uani 1 1 d . . . H49 H 1.1437 0.2345 0.5017 0.033 Uiso 1 1 calc R . . C50 C 1.2556(7) 0.1788(4) 0.6082(6) 0.0360(17) Uani 1 1 d . . . H50 H 1.2553 0.2021 0.6729 0.043 Uiso 1 1 calc R . . C51 C 1.3211(6) 0.1276(4) 0.6163(6) 0.0354(17) Uani 1 1 d . . . H51 H 1.3683 0.1153 0.6861 0.042 Uiso 1 1 calc R . . C52 C 1.3193(6) 0.0918(3) 0.5194(5) 0.0245(13) Uani 1 1 d . . . C53 C 1.3885(6) 0.0374(3) 0.5263(6) 0.0303(15) Uani 1 1 d . . . H53 H 1.4311 0.0237 0.5968 0.036 Uiso 1 1 calc R . . C54 C 1.3939(6) 0.0056(3) 0.4347(6) 0.0299(15) Uani 1 1 d . . . H54 H 1.4421 -0.0299 0.4408 0.036 Uiso 1 1 calc R . . C55 C 1.3291(6) 0.0243(3) 0.3296(6) 0.0285(15) Uani 1 1 d . . . H55 H 1.3331 0.0012 0.2654 0.034 Uiso 1 1 calc R . . C56 C 1.2599(5) 0.0760(3) 0.3194(5) 0.0225(13) Uani 1 1 d . . . H56 H 1.2173 0.0884 0.2479 0.027 Uiso 1 1 calc R . . C57 C 1.2516(5) 0.1108(3) 0.4143(5) 0.0214(12) Uani 1 1 d . . . Sb1 Sb 0.29787(4) 0.08540(2) -0.03752(4) 0.02773(10) Uani 1 1 d . . . F1 F 0.3217(5) 0.0252(2) 0.0679(4) 0.0543(13) Uani 1 1 d . . . F2 F 0.2676(6) 0.1456(2) -0.1435(4) 0.0622(16) Uani 1 1 d . . . F3 F 0.4581(4) 0.0748(2) -0.0677(4) 0.0469(12) Uani 1 1 d . . . F4 F 0.1372(4) 0.0981(3) -0.0066(4) 0.0607(16) Uani 1 1 d . . . F5 F 0.3608(4) 0.1401(2) 0.0737(4) 0.0495(12) Uani 1 1 d . . . F6 F 0.2319(5) 0.0307(2) -0.1485(4) 0.0540(13) Uani 1 1 d . . . Sb2 Sb 0.34287(4) 0.41824(2) 0.27083(3) 0.02538(10) Uani 1 1 d . . . F7 F 0.3970(5) 0.3592(3) 0.1851(5) 0.0678(17) Uani 1 1 d . . . F8 F 0.2875(5) 0.4773(2) 0.3577(4) 0.0556(14) Uani 1 1 d . . . F9 F 0.2489(4) 0.3631(2) 0.3337(4) 0.0490(13) Uani 1 1 d . . . F10 F 0.4355(6) 0.4749(3) 0.2117(5) 0.082(2) Uani 1 1 d . . . F11 F 0.4786(4) 0.4032(2) 0.3854(4) 0.0455(12) Uani 1 1 d . . . F12 F 0.2042(4) 0.4334(3) 0.1592(4) 0.0664(18) 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 Ir1 0.01684(10) 0.01873(12) 0.02293(11) -0.00273(10) 0.00607(8) -0.00199(10) Cl1 0.0254(7) 0.0310(9) 0.0213(7) -0.0042(6) 0.0059(6) -0.0002(6) N1 0.018(2) 0.028(3) 0.028(3) -0.001(2) 0.004(2) 0.003(2) N2 0.014(2) 0.022(3) 0.023(3) -0.002(2) 0.005(2) 0.000(2) N3 0.026(3) 0.017(3) 0.033(3) 0.001(2) -0.003(2) 0.004(2) C1 0.028(3) 0.017(4) 0.042(4) -0.003(3) 0.004(3) -0.009(3) C2 0.031(3) 0.020(3) 0.034(4) -0.008(3) 0.014(3) -0.011(3) C3 0.024(3) 0.023(4) 0.038(4) -0.006(3) 0.007(3) -0.006(3) C4 0.022(3) 0.027(4) 0.033(4) -0.008(3) 0.005(3) -0.012(3) C5 0.029(3) 0.022(3) 0.036(4) -0.014(3) 0.011(3) -0.015(3) C6 0.037(4) 0.025(4) 0.057(5) -0.003(4) 0.014(4) -0.005(3) C7 0.045(4) 0.031(4) 0.034(4) 0.001(3) 0.014(3) -0.015(3) C8 0.019(3) 0.043(5) 0.070(5) -0.012(5) 0.015(3) -0.006(3) C9 0.039(4) 0.051(5) 0.037(4) -0.005(4) -0.004(3) -0.012(4) C10 0.037(4) 0.035(4) 0.036(4) -0.017(3) 0.014(3) -0.016(3) C11 0.026(3) 0.033(4) 0.036(4) -0.003(3) 0.001(3) 0.015(3) C12 0.031(4) 0.033(4) 0.037(4) -0.001(3) -0.003(3) 0.012(3) C13 0.036(4) 0.019(4) 0.069(6) 0.012(4) -0.005(4) -0.002(3) C14 0.026(3) 0.020(3) 0.019(3) -0.003(3) 0.002(2) -0.002(3) C15 0.020(3) 0.016(3) 0.030(3) 0.000(3) 0.006(3) 0.000(2) C16 0.018(3) 0.019(3) 0.022(3) 0.000(3) 0.005(2) 0.002(2) C17 0.025(3) 0.025(3) 0.026(3) -0.003(3) 0.001(3) 0.001(3) C18 0.015(2) 0.023(3) 0.021(3) -0.001(2) 0.004(2) -0.002(2) C19 0.029(3) 0.018(3) 0.022(3) 0.002(2) 0.007(2) 0.002(2) C20 0.044(4) 0.031(4) 0.021(3) 0.003(3) 0.007(3) 0.004(3) C21 0.031(3) 0.033(4) 0.024(3) -0.001(3) 0.011(3) -0.001(3) C22 0.020(3) 0.023(3) 0.028(3) -0.005(3) 0.008(2) -0.004(3) C23 0.024(3) 0.022(3) 0.038(4) -0.010(3) 0.007(3) 0.005(3) C24 0.028(3) 0.024(4) 0.039(4) -0.008(3) 0.002(3) 0.000(3) C25 0.029(3) 0.030(4) 0.025(3) 0.003(3) -0.004(3) 0.003(3) C26 0.021(3) 0.020(3) 0.027(3) -0.002(3) 0.005(2) 0.000(3) C27 0.017(3) 0.011(3) 0.024(3) -0.001(2) 0.002(2) -0.003(2) Ir31 0.01501(9) 0.01937(12) 0.02174(11) 0.00044(10) 0.00416(8) -0.00328(9) Cl31 0.0256(7) 0.0306(9) 0.0237(8) -0.0029(6) 0.0063(6) -0.0062(6) N31 0.022(2) 0.014(3) 0.021(3) 0.002(2) 0.003(2) 0.000(2) N32 0.018(2) 0.015(3) 0.017(2) 0.0022(19) 0.0029(19) -0.001(2) N33 0.020(2) 0.018(3) 0.038(3) 0.002(2) 0.007(2) 0.001(2) C31 0.028(4) 0.017(4) 0.040(4) -0.003(3) 0.005(3) -0.005(3) C32 0.026(3) 0.026(4) 0.029(3) 0.000(3) 0.001(3) -0.006(3) C33 0.015(3) 0.031(4) 0.029(3) -0.003(3) 0.006(2) -0.010(3) C34 0.025(3) 0.031(4) 0.026(3) -0.001(3) 0.008(3) -0.013(3) C35 0.029(3) 0.027(4) 0.026(3) -0.007(3) 0.005(3) -0.015(3) C36 0.032(4) 0.018(4) 0.081(6) 0.004(4) 0.013(4) -0.005(3) C37 0.040(4) 0.040(4) 0.034(4) 0.007(3) 0.007(3) -0.018(4) C38 0.020(3) 0.039(5) 0.060(5) -0.004(4) 0.016(3) -0.005(3) C39 0.030(3) 0.059(6) 0.031(4) 0.010(4) -0.009(3) -0.021(4) C40 0.041(4) 0.040(5) 0.045(5) -0.019(4) 0.020(4) -0.014(4) C41 0.018(3) 0.031(4) 0.038(4) 0.000(3) 0.009(3) 0.007(3) C42 0.022(3) 0.026(4) 0.032(4) -0.001(3) 0.003(3) 0.009(3) C43 0.032(4) 0.019(4) 0.072(5) 0.004(4) 0.018(4) -0.005(3) C44 0.019(3) 0.017(3) 0.023(3) 0.002(2) 0.005(2) 0.002(2) C45 0.017(3) 0.019(3) 0.020(3) 0.003(2) 0.002(2) 0.000(2) C46 0.019(2) 0.016(3) 0.022(3) -0.002(3) 0.002(2) 0.000(3) C47 0.021(3) 0.030(4) 0.038(4) 0.005(3) 0.013(3) 0.008(3) C48 0.016(3) 0.021(3) 0.022(3) 0.002(2) 0.008(2) 0.001(2) C49 0.024(3) 0.030(4) 0.027(3) -0.005(3) 0.001(2) 0.009(3) C50 0.040(4) 0.047(5) 0.021(3) -0.005(3) 0.005(3) 0.014(3) C51 0.031(3) 0.048(5) 0.026(3) 0.009(3) 0.003(3) 0.020(3) C52 0.023(3) 0.028(4) 0.024(3) 0.005(3) 0.007(2) 0.004(3) C53 0.029(3) 0.023(4) 0.041(4) 0.014(3) 0.013(3) 0.009(3) C54 0.020(3) 0.020(3) 0.050(4) 0.007(3) 0.007(3) 0.002(3) C55 0.025(3) 0.015(3) 0.047(4) -0.004(3) 0.011(3) 0.003(3) C56 0.019(3) 0.019(3) 0.029(3) 0.001(3) 0.005(2) -0.003(2) C57 0.016(3) 0.021(3) 0.027(3) 0.002(3) 0.007(2) -0.004(2) Sb1 0.0296(2) 0.0269(2) 0.0257(2) 0.00090(19) 0.00272(17) 0.00361(19) F1 0.060(3) 0.051(3) 0.047(3) 0.022(2) -0.002(2) -0.012(3) F2 0.106(4) 0.044(3) 0.043(3) 0.020(2) 0.029(3) 0.037(3) F3 0.044(3) 0.043(3) 0.059(3) -0.003(2) 0.025(2) 0.013(2) F4 0.030(2) 0.092(5) 0.061(3) -0.012(3) 0.010(2) 0.004(3) F5 0.047(3) 0.051(3) 0.054(3) -0.022(2) 0.020(2) -0.018(2) F6 0.060(3) 0.046(3) 0.046(3) -0.016(2) -0.014(2) 0.012(2) Sb2 0.0245(2) 0.0302(2) 0.0221(2) -0.00359(18) 0.00607(16) -0.00547(18) F7 0.056(3) 0.091(4) 0.061(3) -0.047(3) 0.024(3) 0.003(3) F8 0.089(4) 0.033(3) 0.047(3) -0.005(2) 0.018(3) 0.025(3) F9 0.045(3) 0.052(3) 0.052(3) -0.005(2) 0.014(2) -0.033(2) F10 0.095(4) 0.104(5) 0.049(3) 0.021(3) 0.022(3) -0.056(4) F11 0.030(2) 0.065(3) 0.038(2) -0.002(2) -0.0027(18) -0.001(2) F12 0.043(3) 0.125(6) 0.029(3) 0.009(3) 0.001(2) 0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 N1 2.076(6) . ? Ir1 N2 2.123(5) . ? Ir1 C3 2.147(6) . ? Ir1 C5 2.149(6) . ? Ir1 C4 2.150(6) . ? Ir1 C1 2.155(8) . ? Ir1 C2 2.179(6) . ? Ir1 Cl1 2.3963(16) . ? N1 C14 1.331(8) . ? N1 C11 1.372(8) . ? N2 C15 1.286(8) . ? N2 C16 1.494(7) . ? N3 C14 1.344(9) . ? N3 C12 1.371(9) . ? N3 C13 1.467(9) . ? C1 C2 1.437(10) . ? C1 C5 1.442(10) . ? C1 C6 1.514(11) . ? C2 C3 1.435(10) . ? C2 C7 1.492(10) . ? C3 C4 1.432(9) . ? C3 C8 1.496(9) . ? C4 C5 1.420(10) . ? C4 C9 1.497(11) . ? C5 C10 1.510(9) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.362(11) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.430(9) . ? C15 H15 0.9500 . ? C16 C18 1.521(8) . ? C16 C17 1.530(8) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.365(8) . ? C18 C27 1.436(8) . ? C19 C20 1.409(9) . ? C19 H19 0.9500 . ? C20 C21 1.344(10) . ? C20 H20 0.9500 . ? C21 C22 1.399(9) . ? C21 H21 0.9500 . ? C22 C23 1.420(9) . ? C22 C27 1.443(8) . ? C23 C24 1.327(10) . ? C23 H23 0.9500 . ? C24 C25 1.416(10) . ? C24 H24 0.9500 . ? C25 C26 1.372(9) . ? C25 H25 0.9500 . ? C26 C27 1.412(9) . ? C26 H26 0.9500 . ? Ir31 N31 2.076(5) . ? Ir31 N32 2.115(5) . ? Ir31 C34 2.146(7) . ? Ir31 C33 2.152(6) . ? Ir31 C31 2.159(7) . ? Ir31 C35 2.168(7) . ? Ir31 C32 2.177(7) . ? Ir31 Cl31 2.3990(16) . ? N31 C44 1.334(8) . ? N31 C41 1.372(8) . ? N32 C45 1.286(8) . ? N32 C46 1.481(7) . ? N33 C44 1.332(8) . ? N33 C42 1.377(8) . ? N33 C43 1.465(9) . ? C31 C32 1.432(10) . ? C31 C35 1.447(10) . ? C31 C36 1.499(10) . ? C32 C33 1.424(10) . ? C32 C37 1.492(9) . ? C33 C34 1.452(9) . ? C33 C38 1.489(9) . ? C34 C35 1.413(10) . ? C34 C39 1.488(10) . ? C35 C40 1.496(10) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.355(10) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.443(8) . ? C45 H45 0.9500 . ? C46 C48 1.517(8) . ? C46 C47 1.538(8) . ? C46 H46 1.0000 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.366(9) . ? C48 C57 1.444(9) . ? C49 C50 1.401(9) . ? C49 H49 0.9500 . ? C50 C51 1.348(10) . ? C50 H50 0.9500 . ? C51 C52 1.429(10) . ? C51 H51 0.9500 . ? C52 C57 1.420(9) . ? C52 C53 1.430(9) . ? C53 C54 1.339(10) . ? C53 H53 0.9500 . ? C54 C55 1.409(10) . ? C54 H54 0.9500 . ? C55 C56 1.376(9) . ? C55 H55 0.9500 . ? C56 C57 1.416(9) . ? C56 H56 0.9500 . ? Sb1 F1 1.852(5) . ? Sb1 F2 1.859(5) . ? Sb1 F3 1.864(4) . ? Sb1 F5 1.865(4) . ? Sb1 F6 1.870(5) . ? Sb1 F4 1.879(5) . ? Sb2 F10 1.853(5) . ? Sb2 F7 1.856(5) . ? Sb2 F9 1.862(4) . ? Sb2 F11 1.864(4) . ? Sb2 F12 1.864(4) . ? Sb2 F8 1.870(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ir1 N2 76.3(2) . . ? N1 Ir1 C3 104.3(2) . . ? N2 Ir1 C3 166.2(2) . . ? N1 Ir1 C5 126.4(3) . . ? N2 Ir1 C5 103.4(2) . . ? C3 Ir1 C5 64.9(2) . . ? N1 Ir1 C4 98.9(3) . . ? N2 Ir1 C4 127.3(2) . . ? C3 Ir1 C4 38.9(3) . . ? C5 Ir1 C4 38.6(3) . . ? N1 Ir1 C1 164.1(2) . . ? N2 Ir1 C1 110.8(2) . . ? C3 Ir1 C1 65.3(3) . . ? C5 Ir1 C1 39.2(3) . . ? C4 Ir1 C1 65.4(3) . . ? N1 Ir1 C2 138.2(2) . . ? N2 Ir1 C2 144.7(2) . . ? C3 Ir1 C2 38.7(3) . . ? C5 Ir1 C2 64.7(2) . . ? C4 Ir1 C2 64.9(3) . . ? C1 Ir1 C2 38.7(3) . . ? N1 Ir1 Cl1 88.68(17) . . ? N2 Ir1 Cl1 80.09(14) . . ? C3 Ir1 Cl1 113.6(2) . . ? C5 Ir1 Cl1 144.8(2) . . ? C4 Ir1 Cl1 152.51(18) . . ? C1 Ir1 Cl1 106.3(2) . . ? C2 Ir1 Cl1 91.97(19) . . ? C14 N1 C11 106.9(6) . . ? C14 N1 Ir1 114.3(5) . . ? C11 N1 Ir1 138.7(5) . . ? C15 N2 C16 121.2(5) . . ? C15 N2 Ir1 116.4(4) . . ? C16 N2 Ir1 120.9(4) . . ? C14 N3 C12 107.2(6) . . ? C14 N3 C13 127.5(6) . . ? C12 N3 C13 125.2(6) . . ? C2 C1 C5 107.2(6) . . ? C2 C1 C6 125.7(7) . . ? C5 C1 C6 126.9(7) . . ? C2 C1 Ir1 71.6(4) . . ? C5 C1 Ir1 70.2(4) . . ? C6 C1 Ir1 126.9(5) . . ? C3 C2 C1 107.9(6) . . ? C3 C2 C7 124.5(6) . . ? C1 C2 C7 127.6(7) . . ? C3 C2 Ir1 69.4(4) . . ? C1 C2 Ir1 69.7(4) . . ? C7 C2 Ir1 124.8(5) . . ? C4 C3 C2 108.2(6) . . ? C4 C3 C8 127.2(7) . . ? C2 C3 C8 124.4(7) . . ? C4 C3 Ir1 70.7(4) . . ? C2 C3 Ir1 71.8(4) . . ? C8 C3 Ir1 127.3(5) . . ? C5 C4 C3 107.9(6) . . ? C5 C4 C9 126.3(6) . . ? C3 C4 C9 125.7(7) . . ? C5 C4 Ir1 70.7(4) . . ? C3 C4 Ir1 70.4(4) . . ? C9 C4 Ir1 126.4(5) . . ? C4 C5 C1 108.6(6) . . ? C4 C5 C10 124.7(7) . . ? C1 C5 C10 126.5(7) . . ? C4 C5 Ir1 70.8(4) . . ? C1 C5 Ir1 70.6(4) . . ? C10 C5 Ir1 128.4(5) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 N1 108.2(6) . . ? C12 C11 H11 125.9 . . ? N1 C11 H11 125.9 . . ? C11 C12 N3 107.2(6) . . ? C11 C12 H12 126.4 . . ? N3 C12 H12 126.4 . . ? N3 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 N3 110.4(6) . . ? N1 C14 C15 118.1(6) . . ? N3 C14 C15 131.4(6) . . ? N2 C15 C14 114.7(6) . . ? N2 C15 H15 122.7 . . ? C14 C15 H15 122.7 . . ? N2 C16 C18 112.6(5) . . ? N2 C16 C17 111.9(5) . . ? C18 C16 C17 110.4(5) . . ? N2 C16 H16 107.2 . . ? C18 C16 H16 107.2 . . ? C17 C16 H16 107.2 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C27 119.2(6) . . ? C19 C18 C16 122.0(6) . . ? C27 C18 C16 118.6(5) . . ? C18 C19 C20 121.3(6) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C21 C20 C19 120.7(6) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C20 C21 C22 121.3(6) . . ? C20 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C21 C22 C23 123.1(6) . . ? C21 C22 C27 119.0(6) . . ? C23 C22 C27 117.9(6) . . ? C24 C23 C22 122.1(6) . . ? C24 C23 H23 119.0 . . ? C22 C23 H23 119.0 . . ? C23 C24 C25 120.8(7) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C26 C25 C24 119.8(6) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C27 121.2(6) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C26 C27 C18 123.3(5) . . ? C26 C27 C22 118.2(6) . . ? C18 C27 C22 118.4(6) . . ? N31 Ir31 N32 76.6(2) . . ? N31 Ir31 C34 99.0(3) . . ? N32 Ir31 C34 122.4(2) . . ? N31 Ir31 C33 104.2(2) . . ? N32 Ir31 C33 161.9(2) . . ? C34 Ir31 C33 39.5(2) . . ? N31 Ir31 C31 164.0(2) . . ? N32 Ir31 C31 109.5(2) . . ? C34 Ir31 C31 65.1(3) . . ? C33 Ir31 C31 65.3(3) . . ? N31 Ir31 C35 126.5(2) . . ? N32 Ir31 C35 99.5(2) . . ? C34 Ir31 C35 38.2(3) . . ? C33 Ir31 C35 65.1(2) . . ? C31 Ir31 C35 39.1(3) . . ? N31 Ir31 C32 138.1(2) . . ? N32 Ir31 C32 145.2(2) . . ? C34 Ir31 C32 64.7(3) . . ? C33 Ir31 C32 38.4(3) . . ? C31 Ir31 C32 38.6(3) . . ? C35 Ir31 C32 64.5(3) . . ? N31 Ir31 Cl31 83.49(15) . . ? N32 Ir31 Cl31 89.59(14) . . ? C34 Ir31 Cl31 147.72(17) . . ? C33 Ir31 Cl31 108.53(18) . . ? C31 Ir31 Cl31 110.9(2) . . ? C35 Ir31 Cl31 149.9(2) . . ? C32 Ir31 Cl31 91.94(19) . . ? C44 N31 C41 106.1(5) . . ? C44 N31 Ir31 115.0(4) . . ? C41 N31 Ir31 138.8(4) . . ? C45 N32 C46 120.2(5) . . ? C45 N32 Ir31 116.0(4) . . ? C46 N32 Ir31 123.7(4) . . ? C44 N33 C42 107.0(5) . . ? C44 N33 C43 127.3(5) . . ? C42 N33 C43 125.7(6) . . ? C32 C31 C35 107.2(6) . . ? C32 C31 C36 125.6(7) . . ? C35 C31 C36 126.8(7) . . ? C32 C31 Ir31 71.4(4) . . ? C35 C31 Ir31 70.8(4) . . ? C36 C31 Ir31 128.9(5) . . ? C33 C32 C31 109.0(6) . . ? C33 C32 C37 125.1(6) . . ? C31 C32 C37 126.0(7) . . ? C33 C32 Ir31 69.9(4) . . ? C31 C32 Ir31 70.1(4) . . ? C37 C32 Ir31 126.1(5) . . ? C32 C33 C34 107.1(6) . . ? C32 C33 C38 125.4(6) . . ? C34 C33 C38 127.3(7) . . ? C32 C33 Ir31 71.7(4) . . ? C34 C33 Ir31 70.0(3) . . ? C38 C33 Ir31 126.9(5) . . ? C35 C34 C33 108.4(6) . . ? C35 C34 C39 125.6(6) . . ? C33 C34 C39 125.9(6) . . ? C35 C34 Ir31 71.7(4) . . ? C33 C34 Ir31 70.5(4) . . ? C39 C34 Ir31 125.9(5) . . ? C34 C35 C31 108.2(6) . . ? C34 C35 C40 124.7(7) . . ? C31 C35 C40 126.9(7) . . ? C34 C35 Ir31 70.1(4) . . ? C31 C35 Ir31 70.1(4) . . ? C40 C35 Ir31 129.1(5) . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C35 C40 H40A 109.5 . . ? C35 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C35 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 N31 108.7(6) . . ? C42 C41 H41 125.6 . . ? N31 C41 H41 125.6 . . ? C41 C42 N33 107.0(6) . . ? C41 C42 H42 126.5 . . ? N33 C42 H42 126.5 . . ? N33 C43 H43A 109.5 . . ? N33 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N33 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N33 C44 N31 111.1(5) . . ? N33 C44 C45 132.3(6) . . ? N31 C44 C45 116.5(6) . . ? N32 C45 C44 115.7(5) . . ? N32 C45 H45 122.1 . . ? C44 C45 H45 122.1 . . ? N32 C46 C48 111.9(4) . . ? N32 C46 C47 112.6(5) . . ? C48 C46 C47 110.5(5) . . ? N32 C46 H46 107.1 . . ? C48 C46 H46 107.1 . . ? C47 C46 H46 107.1 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C49 C48 C57 118.5(6) . . ? C49 C48 C46 121.3(6) . . ? C57 C48 C46 120.1(5) . . ? C48 C49 C50 122.7(6) . . ? C48 C49 H49 118.7 . . ? C50 C49 H49 118.7 . . ? C51 C50 C49 120.6(7) . . ? C51 C50 H50 119.7 . . ? C49 C50 H50 119.7 . . ? C50 C51 C52 119.7(6) . . ? C50 C51 H51 120.2 . . ? C52 C51 H51 120.2 . . ? C57 C52 C51 120.3(6) . . ? C57 C52 C53 119.2(6) . . ? C51 C52 C53 120.5(6) . . ? C54 C53 C52 120.9(6) . . ? C54 C53 H53 119.6 . . ? C52 C53 H53 119.6 . . ? C53 C54 C55 120.7(6) . . ? C53 C54 H54 119.7 . . ? C55 C54 H54 119.7 . . ? C56 C55 C54 120.3(6) . . ? C56 C55 H55 119.8 . . ? C54 C55 H55 119.8 . . ? C55 C56 C57 120.7(6) . . ? C55 C56 H56 119.7 . . ? C57 C56 H56 119.7 . . ? C56 C57 C52 118.2(6) . . ? C56 C57 C48 123.5(6) . . ? C52 C57 C48 118.2(6) . . ? F1 Sb1 F2 177.9(2) . . ? F1 Sb1 F3 91.8(2) . . ? F2 Sb1 F3 90.2(2) . . ? F1 Sb1 F5 89.4(2) . . ? F2 Sb1 F5 91.2(3) . . ? F3 Sb1 F5 90.0(2) . . ? F1 Sb1 F6 90.5(2) . . ? F2 Sb1 F6 88.8(2) . . ? F3 Sb1 F6 91.0(2) . . ? F5 Sb1 F6 179.0(2) . . ? F1 Sb1 F4 89.1(3) . . ? F2 Sb1 F4 88.9(3) . . ? F3 Sb1 F4 178.6(2) . . ? F5 Sb1 F4 88.9(2) . . ? F6 Sb1 F4 90.1(2) . . ? F10 Sb2 F7 91.0(3) . . ? F10 Sb2 F9 178.1(3) . . ? F7 Sb2 F9 90.8(3) . . ? F10 Sb2 F11 90.3(2) . . ? F7 Sb2 F11 90.2(2) . . ? F9 Sb2 F11 89.3(2) . . ? F10 Sb2 F12 90.7(3) . . ? F7 Sb2 F12 91.0(3) . . ? F9 Sb2 F12 89.6(2) . . ? F11 Sb2 F12 178.4(2) . . ? F10 Sb2 F8 89.5(3) . . ? F7 Sb2 F8 179.5(3) . . ? F9 Sb2 F8 88.7(2) . . ? F11 Sb2 F8 89.8(2) . . ? F12 Sb2 F8 89.0(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ir1 N1 C14 -2.9(4) . . . . ? C3 Ir1 N1 C14 162.9(5) . . . . ? C5 Ir1 N1 C14 93.8(5) . . . . ? C4 Ir1 N1 C14 123.5(5) . . . . ? C1 Ir1 N1 C14 115.8(8) . . . . ? C2 Ir1 N1 C14 -174.5(4) . . . . ? Cl1 Ir1 N1 C14 -83.0(5) . . . . ? N2 Ir1 N1 C11 179.7(8) . . . . ? C3 Ir1 N1 C11 -14.5(8) . . . . ? C5 Ir1 N1 C11 -83.6(8) . . . . ? C4 Ir1 N1 C11 -53.9(8) . . . . ? C1 Ir1 N1 C11 -61.7(12) . . . . ? C2 Ir1 N1 C11 8.1(9) . . . . ? Cl1 Ir1 N1 C11 99.6(7) . . . . ? N1 Ir1 N2 C15 -0.2(5) . . . . ? C3 Ir1 N2 C15 -94.4(11) . . . . ? C5 Ir1 N2 C15 -124.9(5) . . . . ? C4 Ir1 N2 C15 -91.0(5) . . . . ? C1 Ir1 N2 C15 -165.3(5) . . . . ? C2 Ir1 N2 C15 170.1(5) . . . . ? Cl1 Ir1 N2 C15 90.9(5) . . . . ? N1 Ir1 N2 C16 -166.1(5) . . . . ? C3 Ir1 N2 C16 99.6(10) . . . . ? C5 Ir1 N2 C16 69.1(5) . . . . ? C4 Ir1 N2 C16 103.1(5) . . . . ? C1 Ir1 N2 C16 28.8(5) . . . . ? C2 Ir1 N2 C16 4.2(6) . . . . ? Cl1 Ir1 N2 C16 -75.0(4) . . . . ? N1 Ir1 C1 C2 88.4(9) . . . . ? N2 Ir1 C1 C2 -157.4(4) . . . . ? C3 Ir1 C1 C2 36.9(4) . . . . ? C5 Ir1 C1 C2 116.9(6) . . . . ? C4 Ir1 C1 C2 79.9(4) . . . . ? Cl1 Ir1 C1 C2 -72.0(4) . . . . ? N1 Ir1 C1 C5 -28.5(10) . . . . ? N2 Ir1 C1 C5 85.7(4) . . . . ? C3 Ir1 C1 C5 -79.9(4) . . . . ? C4 Ir1 C1 C5 -36.9(4) . . . . ? C2 Ir1 C1 C5 -116.9(6) . . . . ? Cl1 Ir1 C1 C5 171.1(3) . . . . ? N1 Ir1 C1 C6 -150.4(7) . . . . ? N2 Ir1 C1 C6 -36.2(7) . . . . ? C3 Ir1 C1 C6 158.1(7) . . . . ? C5 Ir1 C1 C6 -121.9(8) . . . . ? C4 Ir1 C1 C6 -158.8(7) . . . . ? C2 Ir1 C1 C6 121.2(8) . . . . ? Cl1 Ir1 C1 C6 49.2(7) . . . . ? C5 C1 C2 C3 2.4(7) . . . . ? C6 C1 C2 C3 178.2(7) . . . . ? Ir1 C1 C2 C3 -59.1(5) . . . . ? C5 C1 C2 C7 -179.5(7) . . . . ? C6 C1 C2 C7 -3.8(12) . . . . ? Ir1 C1 C2 C7 118.9(7) . . . . ? C5 C1 C2 Ir1 61.5(5) . . . . ? C6 C1 C2 Ir1 -122.7(7) . . . . ? N1 Ir1 C2 C3 -36.5(6) . . . . ? N2 Ir1 C2 C3 157.8(4) . . . . ? C5 Ir1 C2 C3 80.7(4) . . . . ? C4 Ir1 C2 C3 37.9(4) . . . . ? C1 Ir1 C2 C3 119.3(6) . . . . ? Cl1 Ir1 C2 C3 -126.7(4) . . . . ? N1 Ir1 C2 C1 -155.7(4) . . . . ? N2 Ir1 C2 C1 38.5(6) . . . . ? C3 Ir1 C2 C1 -119.3(6) . . . . ? C5 Ir1 C2 C1 -38.5(4) . . . . ? C4 Ir1 C2 C1 -81.3(4) . . . . ? Cl1 Ir1 C2 C1 114.0(4) . . . . ? N1 Ir1 C2 C7 81.9(7) . . . . ? N2 Ir1 C2 C7 -83.9(7) . . . . ? C3 Ir1 C2 C7 118.4(8) . . . . ? C5 Ir1 C2 C7 -160.9(7) . . . . ? C4 Ir1 C2 C7 156.3(7) . . . . ? C1 Ir1 C2 C7 -122.3(8) . . . . ? Cl1 Ir1 C2 C7 -8.3(6) . . . . ? C1 C2 C3 C4 -2.3(8) . . . . ? C7 C2 C3 C4 179.5(6) . . . . ? Ir1 C2 C3 C4 -61.6(5) . . . . ? C1 C2 C3 C8 -177.5(7) . . . . ? C7 C2 C3 C8 4.4(11) . . . . ? Ir1 C2 C3 C8 123.2(7) . . . . ? C1 C2 C3 Ir1 59.3(5) . . . . ? C7 C2 C3 Ir1 -118.8(7) . . . . ? N1 Ir1 C3 C4 -86.5(4) . . . . ? N2 Ir1 C3 C4 4.3(12) . . . . ? C5 Ir1 C3 C4 37.4(4) . . . . ? C1 Ir1 C3 C4 80.7(4) . . . . ? C2 Ir1 C3 C4 117.6(6) . . . . ? Cl1 Ir1 C3 C4 178.6(4) . . . . ? N1 Ir1 C3 C2 155.9(4) . . . . ? N2 Ir1 C3 C2 -113.3(10) . . . . ? C5 Ir1 C3 C2 -80.3(4) . . . . ? C4 Ir1 C3 C2 -117.6(6) . . . . ? C1 Ir1 C3 C2 -36.9(4) . . . . ? Cl1 Ir1 C3 C2 61.0(4) . . . . ? N1 Ir1 C3 C8 36.1(7) . . . . ? N2 Ir1 C3 C8 126.9(10) . . . . ? C5 Ir1 C3 C8 159.9(8) . . . . ? C4 Ir1 C3 C8 122.6(9) . . . . ? C1 Ir1 C3 C8 -156.7(8) . . . . ? C2 Ir1 C3 C8 -119.8(8) . . . . ? Cl1 Ir1 C3 C8 -58.8(7) . . . . ? C2 C3 C4 C5 1.4(7) . . . . ? C8 C3 C4 C5 176.3(7) . . . . ? Ir1 C3 C4 C5 -61.0(4) . . . . ? C2 C3 C4 C9 -176.2(7) . . . . ? C8 C3 C4 C9 -1.3(12) . . . . ? Ir1 C3 C4 C9 121.4(7) . . . . ? C2 C3 C4 Ir1 62.4(5) . . . . ? C8 C3 C4 Ir1 -122.7(7) . . . . ? N1 Ir1 C4 C5 -140.2(4) . . . . ? N2 Ir1 C4 C5 -60.6(5) . . . . ? C3 Ir1 C4 C5 118.1(6) . . . . ? C1 Ir1 C4 C5 37.5(4) . . . . ? C2 Ir1 C4 C5 80.4(4) . . . . ? Cl1 Ir1 C4 C5 115.4(5) . . . . ? N1 Ir1 C4 C3 101.7(4) . . . . ? N2 Ir1 C4 C3 -178.7(4) . . . . ? C5 Ir1 C4 C3 -118.1(6) . . . . ? C1 Ir1 C4 C3 -80.6(4) . . . . ? C2 Ir1 C4 C3 -37.8(4) . . . . ? Cl1 Ir1 C4 C3 -2.8(7) . . . . ? N1 Ir1 C4 C9 -18.8(6) . . . . ? N2 Ir1 C4 C9 60.8(7) . . . . ? C3 Ir1 C4 C9 -120.5(8) . . . . ? C5 Ir1 C4 C9 121.4(8) . . . . ? C1 Ir1 C4 C9 158.9(7) . . . . ? C2 Ir1 C4 C9 -158.3(7) . . . . ? Cl1 Ir1 C4 C9 -123.3(6) . . . . ? C3 C4 C5 C1 0.1(7) . . . . ? C9 C4 C5 C1 177.7(7) . . . . ? Ir1 C4 C5 C1 -60.8(5) . . . . ? C3 C4 C5 C10 -175.2(6) . . . . ? C9 C4 C5 C10 2.3(11) . . . . ? Ir1 C4 C5 C10 123.9(6) . . . . ? C3 C4 C5 Ir1 60.9(5) . . . . ? C9 C4 C5 Ir1 -121.6(7) . . . . ? C2 C1 C5 C4 -1.6(7) . . . . ? C6 C1 C5 C4 -177.3(7) . . . . ? Ir1 C1 C5 C4 60.8(5) . . . . ? C2 C1 C5 C10 173.7(6) . . . . ? C6 C1 C5 C10 -2.0(11) . . . . ? Ir1 C1 C5 C10 -123.9(7) . . . . ? C2 C1 C5 Ir1 -62.4(5) . . . . ? C6 C1 C5 Ir1 121.9(7) . . . . ? N1 Ir1 C5 C4 51.9(5) . . . . ? N2 Ir1 C5 C4 134.6(4) . . . . ? C3 Ir1 C5 C4 -37.7(4) . . . . ? C1 Ir1 C5 C4 -118.8(6) . . . . ? C2 Ir1 C5 C4 -80.7(4) . . . . ? Cl1 Ir1 C5 C4 -133.7(4) . . . . ? N1 Ir1 C5 C1 170.7(3) . . . . ? N2 Ir1 C5 C1 -106.6(4) . . . . ? C3 Ir1 C5 C1 81.1(4) . . . . ? C4 Ir1 C5 C1 118.8(6) . . . . ? C2 Ir1 C5 C1 38.1(4) . . . . ? Cl1 Ir1 C5 C1 -14.9(5) . . . . ? N1 Ir1 C5 C10 -67.6(8) . . . . ? N2 Ir1 C5 C10 15.1(7) . . . . ? C3 Ir1 C5 C10 -157.2(8) . . . . ? C4 Ir1 C5 C10 -119.5(9) . . . . ? C1 Ir1 C5 C10 121.7(9) . . . . ? C2 Ir1 C5 C10 159.8(8) . . . . ? Cl1 Ir1 C5 C10 106.8(7) . . . . ? C14 N1 C11 C12 -0.2(8) . . . . ? Ir1 N1 C11 C12 177.4(6) . . . . ? N1 C11 C12 N3 0.4(8) . . . . ? C14 N3 C12 C11 -0.4(8) . . . . ? C13 N3 C12 C11 -178.0(7) . . . . ? C11 N1 C14 N3 -0.1(7) . . . . ? Ir1 N1 C14 N3 -178.3(4) . . . . ? C11 N1 C14 C15 -176.2(6) . . . . ? Ir1 N1 C14 C15 5.5(7) . . . . ? C12 N3 C14 N1 0.3(7) . . . . ? C13 N3 C14 N1 177.8(6) . . . . ? C12 N3 C14 C15 175.8(7) . . . . ? C13 N3 C14 C15 -6.7(11) . . . . ? C16 N2 C15 C14 168.9(5) . . . . ? Ir1 N2 C15 C14 3.0(7) . . . . ? N1 C14 C15 N2 -5.7(9) . . . . ? N3 C14 C15 N2 179.0(6) . . . . ? C15 N2 C16 C18 95.4(7) . . . . ? Ir1 N2 C16 C18 -99.4(5) . . . . ? C15 N2 C16 C17 -29.7(8) . . . . ? Ir1 N2 C16 C17 135.6(4) . . . . ? N2 C16 C18 C19 -26.8(8) . . . . ? C17 C16 C18 C19 99.1(7) . . . . ? N2 C16 C18 C27 158.6(5) . . . . ? C17 C16 C18 C27 -75.5(7) . . . . ? C27 C18 C19 C20 0.3(9) . . . . ? C16 C18 C19 C20 -174.3(6) . . . . ? C18 C19 C20 C21 1.8(11) . . . . ? C19 C20 C21 C22 -1.0(11) . . . . ? C20 C21 C22 C23 178.9(7) . . . . ? C20 C21 C22 C27 -1.8(10) . . . . ? C21 C22 C23 C24 178.2(7) . . . . ? C27 C22 C23 C24 -1.1(10) . . . . ? C22 C23 C24 C25 -0.3(11) . . . . ? C23 C24 C25 C26 1.2(10) . . . . ? C24 C25 C26 C27 -0.7(10) . . . . ? C25 C26 C27 C18 177.6(6) . . . . ? C25 C26 C27 C22 -0.7(9) . . . . ? C19 C18 C27 C26 178.7(6) . . . . ? C16 C18 C27 C26 -6.6(9) . . . . ? C19 C18 C27 C22 -3.0(8) . . . . ? C16 C18 C27 C22 171.7(5) . . . . ? C21 C22 C27 C26 -177.8(6) . . . . ? C23 C22 C27 C26 1.6(8) . . . . ? C21 C22 C27 C18 3.8(9) . . . . ? C23 C22 C27 C18 -176.8(5) . . . . ? N32 Ir31 N31 C44 -3.4(4) . . . . ? C34 Ir31 N31 C44 -124.7(5) . . . . ? C33 Ir31 N31 C44 -164.7(4) . . . . ? C31 Ir31 N31 C44 -117.8(9) . . . . ? C35 Ir31 N31 C44 -95.4(5) . . . . ? C32 Ir31 N31 C44 173.4(4) . . . . ? Cl31 Ir31 N31 C44 87.8(4) . . . . ? N32 Ir31 N31 C41 -178.9(7) . . . . ? C34 Ir31 N31 C41 59.8(7) . . . . ? C33 Ir31 N31 C41 19.8(7) . . . . ? C31 Ir31 N31 C41 66.7(11) . . . . ? C35 Ir31 N31 C41 89.1(7) . . . . ? C32 Ir31 N31 C41 -2.1(9) . . . . ? Cl31 Ir31 N31 C41 -87.7(7) . . . . ? N31 Ir31 N32 C45 2.0(4) . . . . ? C34 Ir31 N32 C45 94.2(5) . . . . ? C33 Ir31 N32 C45 96.8(8) . . . . ? C31 Ir31 N32 C45 166.5(5) . . . . ? C35 Ir31 N32 C45 127.4(5) . . . . ? C32 Ir31 N32 C45 -174.2(4) . . . . ? Cl31 Ir31 N32 C45 -81.4(4) . . . . ? N31 Ir31 N32 C46 -173.3(5) . . . . ? C34 Ir31 N32 C46 -81.1(5) . . . . ? C33 Ir31 N32 C46 -78.5(9) . . . . ? C31 Ir31 N32 C46 -8.8(5) . . . . ? C35 Ir31 N32 C46 -47.9(5) . . . . ? C32 Ir31 N32 C46 10.4(6) . . . . ? Cl31 Ir31 N32 C46 103.2(4) . . . . ? N31 Ir31 C31 C32 -87.5(10) . . . . ? N32 Ir31 C31 C32 162.5(4) . . . . ? C34 Ir31 C31 C32 -80.0(4) . . . . ? C33 Ir31 C31 C32 -36.3(4) . . . . ? C35 Ir31 C31 C32 -116.6(5) . . . . ? Cl31 Ir31 C31 C32 65.2(4) . . . . ? N31 Ir31 C31 C35 29.1(10) . . . . ? N32 Ir31 C31 C35 -80.9(4) . . . . ? C34 Ir31 C31 C35 36.6(4) . . . . ? C33 Ir31 C31 C35 80.3(4) . . . . ? C32 Ir31 C31 C35 116.6(5) . . . . ? Cl31 Ir31 C31 C35 -178.2(3) . . . . ? N31 Ir31 C31 C36 151.3(8) . . . . ? N32 Ir31 C31 C36 41.3(8) . . . . ? C34 Ir31 C31 C36 158.8(8) . . . . ? C33 Ir31 C31 C36 -157.5(8) . . . . ? C35 Ir31 C31 C36 122.2(9) . . . . ? C32 Ir31 C31 C36 -121.2(9) . . . . ? Cl31 Ir31 C31 C36 -56.0(8) . . . . ? C35 C31 C32 C33 -2.9(8) . . . . ? C36 C31 C32 C33 -175.8(7) . . . . ? Ir31 C31 C32 C33 59.2(5) . . . . ? C35 C31 C32 C37 177.1(7) . . . . ? C36 C31 C32 C37 4.2(12) . . . . ? Ir31 C31 C32 C37 -120.7(7) . . . . ? C35 C31 C32 Ir31 -62.1(5) . . . . ? C36 C31 C32 Ir31 125.0(7) . . . . ? N31 Ir31 C32 C33 35.6(6) . . . . ? N32 Ir31 C32 C33 -149.9(4) . . . . ? C34 Ir31 C32 C33 -38.9(4) . . . . ? C31 Ir31 C32 C33 -120.1(6) . . . . ? C35 Ir31 C32 C33 -81.4(4) . . . . ? Cl31 Ir31 C32 C33 118.0(4) . . . . ? N31 Ir31 C32 C31 155.6(4) . . . . ? N32 Ir31 C32 C31 -29.9(6) . . . . ? C34 Ir31 C32 C31 81.2(4) . . . . ? C33 Ir31 C32 C31 120.1(6) . . . . ? C35 Ir31 C32 C31 38.7(4) . . . . ? Cl31 Ir31 C32 C31 -121.9(4) . . . . ? N31 Ir31 C32 C37 -83.8(7) . . . . ? N32 Ir31 C32 C37 90.7(7) . . . . ? C34 Ir31 C32 C37 -158.3(7) . . . . ? C33 Ir31 C32 C37 -119.3(8) . . . . ? C31 Ir31 C32 C37 120.6(8) . . . . ? C35 Ir31 C32 C37 159.2(7) . . . . ? Cl31 Ir31 C32 C37 -1.4(6) . . . . ? C31 C32 C33 C34 2.2(8) . . . . ? C37 C32 C33 C34 -177.9(7) . . . . ? Ir31 C32 C33 C34 61.5(4) . . . . ? C31 C32 C33 C38 178.0(7) . . . . ? C37 C32 C33 C38 -2.1(11) . . . . ? Ir31 C32 C33 C38 -122.7(7) . . . . ? C31 C32 C33 Ir31 -59.3(5) . . . . ? C37 C32 C33 Ir31 120.6(7) . . . . ? N31 Ir31 C33 C32 -156.4(4) . . . . ? N32 Ir31 C33 C32 113.3(8) . . . . ? C34 Ir31 C33 C32 116.7(6) . . . . ? C31 Ir31 C33 C32 36.4(4) . . . . ? C35 Ir31 C33 C32 79.7(4) . . . . ? Cl31 Ir31 C33 C32 -68.6(4) . . . . ? N31 Ir31 C33 C34 86.9(4) . . . . ? N32 Ir31 C33 C34 -3.4(10) . . . . ? C31 Ir31 C33 C34 -80.3(5) . . . . ? C35 Ir31 C33 C34 -37.0(4) . . . . ? C32 Ir31 C33 C34 -116.7(6) . . . . ? Cl31 Ir31 C33 C34 174.7(4) . . . . ? N31 Ir31 C33 C38 -35.4(7) . . . . ? N32 Ir31 C33 C38 -125.7(8) . . . . ? C34 Ir31 C33 C38 -122.3(8) . . . . ? C31 Ir31 C33 C38 157.4(7) . . . . ? C35 Ir31 C33 C38 -159.3(7) . . . . ? C32 Ir31 C33 C38 121.0(8) . . . . ? Cl31 Ir31 C33 C38 52.4(7) . . . . ? C32 C33 C34 C35 -0.5(8) . . . . ? C38 C33 C34 C35 -176.2(6) . . . . ? Ir31 C33 C34 C35 62.0(5) . . . . ? C32 C33 C34 C39 176.7(7) . . . . ? C38 C33 C34 C39 1.0(12) . . . . ? Ir31 C33 C34 C39 -120.7(8) . . . . ? C32 C33 C34 Ir31 -62.6(4) . . . . ? C38 C33 C34 Ir31 121.7(7) . . . . ? N31 Ir31 C34 C35 140.5(4) . . . . ? N32 Ir31 C34 C35 60.7(5) . . . . ? C33 Ir31 C34 C35 -118.1(6) . . . . ? C31 Ir31 C34 C35 -37.4(4) . . . . ? C32 Ir31 C34 C35 -80.2(4) . . . . ? Cl31 Ir31 C34 C35 -127.5(4) . . . . ? N31 Ir31 C34 C33 -101.4(4) . . . . ? N32 Ir31 C34 C33 178.7(4) . . . . ? C31 Ir31 C34 C33 80.7(4) . . . . ? C35 Ir31 C34 C33 118.1(6) . . . . ? C32 Ir31 C34 C33 37.9(4) . . . . ? Cl31 Ir31 C34 C33 -9.4(6) . . . . ? N31 Ir31 C34 C39 19.4(6) . . . . ? N32 Ir31 C34 C39 -60.4(7) . . . . ? C33 Ir31 C34 C39 120.8(8) . . . . ? C31 Ir31 C34 C39 -158.5(7) . . . . ? C35 Ir31 C34 C39 -121.1(7) . . . . ? C32 Ir31 C34 C39 158.7(7) . . . . ? Cl31 Ir31 C34 C39 111.4(6) . . . . ? C33 C34 C35 C31 -1.3(8) . . . . ? C39 C34 C35 C31 -178.5(7) . . . . ? Ir31 C34 C35 C31 60.0(5) . . . . ? C33 C34 C35 C40 174.3(6) . . . . ? C39 C34 C35 C40 -2.9(11) . . . . ? Ir31 C34 C35 C40 -124.4(7) . . . . ? C33 C34 C35 Ir31 -61.3(5) . . . . ? C39 C34 C35 Ir31 121.5(7) . . . . ? C32 C31 C35 C34 2.6(8) . . . . ? C36 C31 C35 C34 175.4(7) . . . . ? Ir31 C31 C35 C34 -59.9(5) . . . . ? C32 C31 C35 C40 -172.9(7) . . . . ? C36 C31 C35 C40 -0.1(11) . . . . ? Ir31 C31 C35 C40 124.6(7) . . . . ? C32 C31 C35 Ir31 62.5(5) . . . . ? C36 C31 C35 Ir31 -124.7(7) . . . . ? N31 Ir31 C35 C34 -51.4(5) . . . . ? N32 Ir31 C35 C34 -131.7(4) . . . . ? C33 Ir31 C35 C34 38.2(4) . . . . ? C31 Ir31 C35 C34 119.0(5) . . . . ? C32 Ir31 C35 C34 80.8(4) . . . . ? Cl31 Ir31 C35 C34 122.3(4) . . . . ? N31 Ir31 C35 C31 -170.4(3) . . . . ? N32 Ir31 C35 C31 109.3(4) . . . . ? C34 Ir31 C35 C31 -119.0(5) . . . . ? C33 Ir31 C35 C31 -80.8(4) . . . . ? C32 Ir31 C35 C31 -38.2(4) . . . . ? Cl31 Ir31 C35 C31 3.3(6) . . . . ? N31 Ir31 C35 C40 67.6(8) . . . . ? N32 Ir31 C35 C40 -12.7(8) . . . . ? C34 Ir31 C35 C40 119.0(9) . . . . ? C33 Ir31 C35 C40 157.2(8) . . . . ? C31 Ir31 C35 C40 -122.0(9) . . . . ? C32 Ir31 C35 C40 -160.2(8) . . . . ? Cl31 Ir31 C35 C40 -118.7(7) . . . . ? C44 N31 C41 C42 0.3(8) . . . . ? Ir31 N31 C41 C42 176.1(5) . . . . ? N31 C41 C42 N33 -0.3(8) . . . . ? C44 N33 C42 C41 0.1(8) . . . . ? C43 N33 C42 C41 179.1(7) . . . . ? C42 N33 C44 N31 0.1(7) . . . . ? C43 N33 C44 N31 -178.9(7) . . . . ? C42 N33 C44 C45 178.3(6) . . . . ? C43 N33 C44 C45 -0.8(12) . . . . ? C41 N31 C44 N33 -0.3(7) . . . . ? Ir31 N31 C44 N33 -177.2(4) . . . . ? C41 N31 C44 C45 -178.8(5) . . . . ? Ir31 N31 C44 C45 4.3(7) . . . . ? C46 N32 C45 C44 175.1(5) . . . . ? Ir31 N32 C45 C44 -0.4(7) . . . . ? N33 C44 C45 N32 179.3(6) . . . . ? N31 C44 C45 N32 -2.6(8) . . . . ? C45 N32 C46 C48 104.6(6) . . . . ? Ir31 N32 C46 C48 -80.3(5) . . . . ? C45 N32 C46 C47 -20.7(7) . . . . ? Ir31 N32 C46 C47 154.5(4) . . . . ? N32 C46 C48 C49 -29.7(8) . . . . ? C47 C46 C48 C49 96.8(7) . . . . ? N32 C46 C48 C57 152.8(5) . . . . ? C47 C46 C48 C57 -80.8(7) . . . . ? C57 C48 C49 C50 -0.9(10) . . . . ? C46 C48 C49 C50 -178.5(6) . . . . ? C48 C49 C50 C51 1.0(11) . . . . ? C49 C50 C51 C52 -1.4(11) . . . . ? C50 C51 C52 C57 1.7(11) . . . . ? C50 C51 C52 C53 179.8(7) . . . . ? C57 C52 C53 C54 2.5(10) . . . . ? C51 C52 C53 C54 -175.6(7) . . . . ? C52 C53 C54 C55 -1.5(10) . . . . ? C53 C54 C55 C56 0.6(10) . . . . ? C54 C55 C56 C57 -0.7(9) . . . . ? C55 C56 C57 C52 1.7(9) . . . . ? C55 C56 C57 C48 178.7(6) . . . . ? C51 C52 C57 C56 175.6(6) . . . . ? C53 C52 C57 C56 -2.5(9) . . . . ? C51 C52 C57 C48 -1.6(9) . . . . ? C53 C52 C57 C48 -179.7(6) . . . . ? C49 C48 C57 C56 -175.8(6) . . . . ? C46 C48 C57 C56 1.8(8) . . . . ? C49 C48 C57 C52 1.2(8) . . . . ? C46 C48 C57 C52 178.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.719 _refine_diff_density_min -0.810 _refine_diff_density_rms 0.139 _database_code_depnum_ccdc_archive 'CCDC 937404' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_cmpnd_7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H32 N3 O Rh, 2(F6 Sb),0.5(H2 O)' _chemical_formula_sum 'C23 H33 F12 N3 O1.5 Rh Sb2' _chemical_formula_weight 949.91 _chemical_absolute_configuration rmad 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.1017(9) _cell_length_b 10.9590(13) _cell_length_c 17.954(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.0550(10) _cell_angle_gamma 90.00 _cell_volume 1574.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9893 _cell_measurement_theta_min 2.184 _cell_measurement_theta_max 29.35 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.169 _exptl_crystal_size_mid 0.114 _exptl_crystal_size_min 0.055 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.023 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 918 _exptl_absorpt_coefficient_mu 2.320 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.836 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ; Absorption corrections based on face indexing, including in APEX2 package (Bruker AXS, 2008). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX DUO system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 17290 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 29.52 _reflns_number_total 6417 _reflns_number_gt 5965 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_cell_refinement 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_data_reduction 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP program, SHELXTL v6.12, Bruker2000' _computing_publication_material ENCIFER _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. All non-hydrogen atoms of the coordination complex were refined with anisotropic displacement parameters. Hydrogen atoms have been included in the model in calculated positions and refined with positional and thermal riding parameters.Hydrogen atoms of the hydration water molecule have not been included in the model. Both SbF6- anion molecules exhibit fluorine disorder, modelized in the base of two fluorine positions with complementary occupancy factors (0.70 / 0.30). Maximal residual density peaks are found in the proximity of the disordered fragment. They have no chemical sense. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0574P)^2^+0.7067P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(3) _refine_ls_number_reflns 6417 _refine_ls_number_parameters 385 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0410 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.0992 _refine_ls_wR_factor_gt 0.0973 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL fjl91ds in P2(1) CELL 0.71073 8.1017 10.9590 17.9540 90.000 99.055 90.000 ZERR 2.00 0.0009 0.0013 0.0021 0.000 0.001 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O F RH SB UNIT 46 66 6 3 24 2 4 MERG 2 FMAP 2 PLAN 10 ACTA 55.00 WPDB -2 OMIT 0 0 1 BOND $H CONF L.S. 4 TEMP -173.00 WGHT 0.057400 0.706700 FVAR 0.33349 0.64452 0.09195 RH1 6 0.439585 0.245405 0.224231 11.00000 0.02334 0.02976 = 0.03220 0.00096 0.01017 0.00398 N1 3 0.330832 0.234780 0.321512 11.00000 0.04744 0.04371 = 0.04398 0.01080 0.03052 0.01841 N2 3 0.388666 0.433452 0.247335 11.00000 0.02349 0.03350 = 0.03051 0.00165 0.00972 0.00304 N3 3 0.205850 0.327728 0.406671 11.00000 0.03197 0.04838 = 0.03540 0.00416 0.01297 0.00503 O1 4 0.177664 0.253901 0.170541 11.00000 0.02603 0.06652 = 0.09139 -0.02547 0.01282 -0.00033 AFIX 1 H1A 2 0.135965 0.171194 0.159429 11.00000 31.00000 H1B 2 0.169736 0.300864 0.123696 11.00000 31.00000 AFIX 0 C1 1 0.624745 0.244560 0.149214 11.00000 0.02797 0.03847 = 0.03643 0.00079 0.01290 0.01092 C2 1 0.520400 0.140071 0.134674 11.00000 0.02696 0.04470 = 0.04069 -0.00544 0.01074 0.00812 C3 1 0.534144 0.069002 0.202067 11.00000 0.03397 0.03505 = 0.04921 -0.00323 0.01715 0.00341 C4 1 0.650267 0.129735 0.258425 11.00000 0.03197 0.03873 = 0.04518 0.00293 0.00912 0.01259 C5 1 0.704206 0.239213 0.227280 11.00000 0.02156 0.03844 = 0.04393 -0.00197 0.00985 0.01010 C6 1 0.652294 0.337288 0.091660 11.00000 0.04458 0.05328 = 0.04725 0.01087 0.02878 0.00949 AFIX 137 H6A 2 0.724378 0.302798 0.057993 11.00000 -1.50000 H6B 2 0.706003 0.409535 0.116965 11.00000 -1.50000 H6C 2 0.544609 0.360483 0.062190 11.00000 -1.50000 AFIX 0 C7 1 0.416580 0.106654 0.062933 11.00000 0.03850 0.06908 = 0.05284 -0.01575 0.00203 0.00442 AFIX 137 H7A 2 0.373204 0.180818 0.036264 11.00000 -1.50000 H7B 2 0.323043 0.055779 0.072954 11.00000 -1.50000 H7C 2 0.484260 0.061079 0.031741 11.00000 -1.50000 AFIX 0 C8 1 0.454811 -0.054143 0.211909 11.00000 0.05014 0.03419 = 0.07378 -0.00238 0.02243 0.00836 AFIX 137 H8A 2 0.533471 -0.119142 0.204206 11.00000 -1.50000 H8B 2 0.352758 -0.062640 0.174924 11.00000 -1.50000 H8C 2 0.426955 -0.060199 0.262956 11.00000 -1.50000 AFIX 0 C9 1 0.712130 0.082159 0.337146 11.00000 0.05135 0.06864 = 0.04390 0.01769 0.00896 0.02490 AFIX 137 H9A 2 0.624667 0.032518 0.354219 11.00000 -1.50000 H9B 2 0.739582 0.151072 0.371660 11.00000 -1.50000 H9C 2 0.812138 0.032130 0.336454 11.00000 -1.50000 AFIX 0 C10 1 0.830843 0.327811 0.265869 11.00000 0.02510 0.06008 = 0.05763 -0.00900 0.00897 0.00731 AFIX 137 H10A 2 0.814834 0.337869 0.318498 11.00000 -1.50000 H10B 2 0.816813 0.406806 0.240066 11.00000 -1.50000 H10C 2 0.943587 0.296623 0.264244 11.00000 -1.50000 AFIX 0 C11 1 0.279389 0.149859 0.366960 11.00000 0.08834 0.05266 = 0.08718 0.03007 0.06585 0.03063 AFIX 43 H11 2 0.294140 0.064276 0.362749 11.00000 -1.20000 AFIX 0 C12 1 0.201959 0.206779 0.420544 11.00000 0.05729 0.05147 = 0.06252 0.02291 0.03976 0.01307 AFIX 43 H12 2 0.154880 0.168309 0.459723 11.00000 -1.20000 AFIX 0 C13 1 0.148263 0.423802 0.450915 11.00000 0.04261 0.04889 = 0.04614 -0.00971 0.02273 -0.00439 AFIX 137 H13A 2 0.244447 0.469338 0.476974 11.00000 -1.50000 H13B 2 0.085807 0.388351 0.488151 11.00000 -1.50000 H13C 2 0.075347 0.479097 0.417729 11.00000 -1.50000 AFIX 0 C14 1 0.283906 0.341961 0.345752 11.00000 0.03225 0.03379 = 0.03341 0.00557 0.01173 0.00527 C15 1 0.313289 0.449117 0.304383 11.00000 0.03076 0.03341 = 0.03372 -0.00072 0.01227 -0.00028 AFIX 43 H15 2 0.278926 0.527628 0.318335 11.00000 -1.20000 AFIX 0 C16 1 0.414542 0.538755 0.199741 11.00000 0.03709 0.03087 = 0.03191 0.00215 0.01207 0.00570 AFIX 13 H16 2 0.420846 0.505991 0.148281 11.00000 -1.20000 AFIX 0 C17 1 0.273741 0.633001 0.190468 11.00000 0.04104 0.03785 = 0.04442 0.00432 0.00704 0.00723 AFIX 137 H17A 2 0.167058 0.592373 0.172677 11.00000 -1.50000 H17B 2 0.294944 0.694788 0.153662 11.00000 -1.50000 H17C 2 0.268938 0.672272 0.239119 11.00000 -1.50000 AFIX 0 C18 1 0.583899 0.600558 0.227840 11.00000 0.03284 0.03195 = 0.03913 0.00475 0.00824 0.00856 C19 1 0.676880 0.643861 0.174249 11.00000 0.03753 0.04347 = 0.04526 0.01329 0.01803 0.00975 AFIX 43 H19 2 0.639315 0.630670 0.122036 11.00000 -1.20000 AFIX 0 C20 1 0.824952 0.706465 0.197988 11.00000 0.04197 0.05259 = 0.08834 0.01942 0.02453 -0.00133 AFIX 43 H20 2 0.887694 0.737111 0.161601 11.00000 -1.20000 AFIX 0 C21 1 0.882788 0.724945 0.274594 11.00000 0.02951 0.06406 = 0.10699 0.00464 0.00497 -0.00413 AFIX 43 H21 2 0.984695 0.767239 0.290260 11.00000 -1.20000 AFIX 0 C22 1 0.791932 0.681845 0.326748 11.00000 0.04850 0.06187 = 0.06835 -0.00381 -0.00175 -0.00584 AFIX 43 H22 2 0.830422 0.694647 0.378924 11.00000 -1.20000 AFIX 0 C23 1 0.642924 0.619119 0.303955 11.00000 0.03756 0.04641 = 0.04170 -0.00100 0.00735 -0.00331 AFIX 43 H23 2 0.581124 0.588767 0.340774 11.00000 -1.20000 AFIX 0 SB1 7 0.704094 0.303967 0.537941 11.00000 0.04266 0.04980 = 0.03997 0.00898 0.01824 0.00605 F1 5 0.878073 0.209305 0.505532 21.00000 0.04714 F2 5 0.531995 0.387398 0.570823 21.00000 0.04775 F3 5 0.737422 0.214901 0.628733 21.00000 0.05261 F4 5 0.674066 0.371994 0.442617 21.00000 0.08786 F5 5 0.559733 0.173351 0.498571 21.00000 0.06868 F6 5 0.856732 0.417777 0.572364 21.00000 0.06787 F1B 5 0.906943 0.232691 0.531463 -21.00000 0.04237 F2B 5 0.503871 0.396724 0.544028 -21.00000 0.04493 F3B 5 0.752927 0.323053 0.643893 -21.00000 0.09943 F4B 5 0.626285 0.311175 0.435085 -21.00000 0.07183 F5B 5 0.589434 0.158779 0.545080 -21.00000 0.08311 F6B 5 0.810892 0.457037 0.530976 -21.00000 0.07842 SB2 7 0.095951 0.479331 -0.028095 11.00000 0.03067 0.04686 = 0.04063 0.00798 0.00472 0.00261 F7A 5 0.260002 0.420445 -0.083025 21.00000 0.06415 F8A 5 -0.060817 0.528471 0.027507 21.00000 0.06890 F9A 5 0.008850 0.564586 -0.114275 21.00000 0.11074 F10A 5 0.200551 0.386599 0.055311 21.00000 0.08586 F11A 5 0.270841 0.578176 0.019455 21.00000 0.06131 F12A 5 -0.080734 0.391787 -0.074997 21.00000 0.08093 F7B 5 0.196420 0.473061 -0.113323 -21.00000 0.05715 F9B 5 -0.003233 0.635141 -0.059574 -21.00000 0.08706 F12B 5 -0.025842 0.333928 -0.058470 -21.00000 0.04814 F11B 5 0.219846 0.616912 -0.003989 -21.00000 0.05005 F8B 5 -0.000608 0.490653 0.063310 -21.00000 0.10185 F10B 5 0.176332 0.327715 0.011329 -21.00000 0.11707 O2 4 0.039378 0.038580 0.246417 10.50000 0.07441 0.10589 = 0.08014 -0.00680 0.00540 -0.03386 HKLF 4 REM fjl91ds in P2(1) REM R1 = 0.0379 for 5965 Fo > 4sig(Fo) and 0.0410 for all 6417 data REM 385 parameters refined using 1 restraints END ; 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.43958(5) 0.24541(4) 0.22423(2) 0.02781(9) Uani 1 1 d . . . N1 N 0.3308(7) 0.2348(6) 0.3215(3) 0.0425(13) Uani 1 1 d . . . N2 N 0.3887(5) 0.4335(5) 0.2473(2) 0.0286(9) Uani 1 1 d . . . N3 N 0.2058(6) 0.3277(5) 0.4067(3) 0.0378(12) Uani 1 1 d . . . O1 O 0.1777(5) 0.2539(6) 0.1705(3) 0.0609(15) Uani 1 1 d . . . H1A H 0.1360 0.1712 0.1594 0.092 Uiso 1 1 d . . . H1B H 0.1697 0.3009 0.1237 0.092 Uiso 1 1 d . . . C1 C 0.6247(6) 0.2446(7) 0.1492(3) 0.0334(11) Uani 1 1 d . . . C2 C 0.5204(7) 0.1401(6) 0.1347(4) 0.0369(13) Uani 1 1 d . . . C3 C 0.5341(8) 0.0690(6) 0.2021(4) 0.0383(13) Uani 1 1 d . . . C4 C 0.6503(8) 0.1297(6) 0.2584(4) 0.0383(13) Uani 1 1 d . . . C5 C 0.7042(6) 0.2392(6) 0.2273(3) 0.0341(11) Uani 1 1 d . . . C6 C 0.6523(9) 0.3373(7) 0.0917(4) 0.0461(16) Uani 1 1 d . . . H6A H 0.7244 0.3028 0.0580 0.069 Uiso 1 1 calc R . . H6B H 0.7060 0.4095 0.1170 0.069 Uiso 1 1 calc R . . H6C H 0.5446 0.3605 0.0622 0.069 Uiso 1 1 calc R . . C7 C 0.4166(9) 0.1067(9) 0.0629(4) 0.0540(19) Uani 1 1 d . . . H7A H 0.3732 0.1808 0.0363 0.081 Uiso 1 1 calc R . . H7B H 0.3230 0.0558 0.0730 0.081 Uiso 1 1 calc R . . H7C H 0.4843 0.0611 0.0317 0.081 Uiso 1 1 calc R . . C8 C 0.4548(9) -0.0541(7) 0.2119(5) 0.0513(18) Uani 1 1 d . . . H8A H 0.5335 -0.1191 0.2042 0.077 Uiso 1 1 calc R . . H8B H 0.3528 -0.0626 0.1749 0.077 Uiso 1 1 calc R . . H8C H 0.4270 -0.0602 0.2630 0.077 Uiso 1 1 calc R . . C9 C 0.7121(10) 0.0822(9) 0.3371(4) 0.0545(19) Uani 1 1 d . . . H9A H 0.6247 0.0325 0.3542 0.082 Uiso 1 1 calc R . . H9B H 0.7396 0.1511 0.3717 0.082 Uiso 1 1 calc R . . H9C H 0.8121 0.0321 0.3365 0.082 Uiso 1 1 calc R . . C10 C 0.8308(7) 0.3278(8) 0.2659(4) 0.0473(16) Uani 1 1 d . . . H10A H 0.8148 0.3379 0.3185 0.071 Uiso 1 1 calc R . . H10B H 0.8168 0.4068 0.2401 0.071 Uiso 1 1 calc R . . H10C H 0.9436 0.2966 0.2642 0.071 Uiso 1 1 calc R . . C11 C 0.2794(13) 0.1499(9) 0.3670(6) 0.070(3) Uani 1 1 d . . . H11 H 0.2941 0.0643 0.3627 0.085 Uiso 1 1 calc R . . C12 C 0.2020(10) 0.2068(8) 0.4205(5) 0.054(2) Uani 1 1 d . . . H12 H 0.1549 0.1683 0.4597 0.065 Uiso 1 1 calc R . . C13 C 0.1483(9) 0.4238(7) 0.4509(4) 0.0442(15) Uani 1 1 d . . . H13A H 0.2444 0.4693 0.4770 0.066 Uiso 1 1 calc R . . H13B H 0.0858 0.3884 0.4882 0.066 Uiso 1 1 calc R . . H13C H 0.0753 0.4791 0.4177 0.066 Uiso 1 1 calc R . . C14 C 0.2839(7) 0.3420(6) 0.3458(3) 0.0324(12) Uani 1 1 d . . . C15 C 0.3133(7) 0.4491(6) 0.3044(3) 0.0319(11) Uani 1 1 d . . . H15 H 0.2789 0.5276 0.3183 0.038 Uiso 1 1 calc R . . C16 C 0.4145(7) 0.5388(6) 0.1997(3) 0.0326(11) Uani 1 1 d . . . H16 H 0.4208 0.5060 0.1483 0.039 Uiso 1 1 calc R . . C17 C 0.2737(8) 0.6330(7) 0.1905(4) 0.0411(14) Uani 1 1 d . . . H17A H 0.1671 0.5924 0.1727 0.062 Uiso 1 1 calc R . . H17B H 0.2949 0.6948 0.1537 0.062 Uiso 1 1 calc R . . H17C H 0.2689 0.6723 0.2391 0.062 Uiso 1 1 calc R . . C18 C 0.5839(7) 0.6006(6) 0.2278(3) 0.0344(12) Uani 1 1 d . . . C19 C 0.6769(8) 0.6439(7) 0.1742(4) 0.0409(14) Uani 1 1 d . . . H19 H 0.6393 0.6307 0.1220 0.049 Uiso 1 1 calc R . . C20 C 0.8250(10) 0.7065(8) 0.1980(6) 0.059(2) Uani 1 1 d . . . H20 H 0.8877 0.7371 0.1616 0.071 Uiso 1 1 calc R . . C21 C 0.8828(9) 0.7249(9) 0.2746(6) 0.067(2) Uani 1 1 d . . . H21 H 0.9847 0.7672 0.2903 0.081 Uiso 1 1 calc R . . C22 C 0.7919(10) 0.6818(9) 0.3267(5) 0.061(2) Uani 1 1 d . . . H22 H 0.8304 0.6946 0.3789 0.073 Uiso 1 1 calc R . . C23 C 0.6429(8) 0.6191(7) 0.3040(4) 0.0418(14) Uani 1 1 d . . . H23 H 0.5811 0.5888 0.3408 0.050 Uiso 1 1 calc R . . Sb1 Sb 0.70409(5) 0.30397(4) 0.53794(2) 0.04288(12) Uani 1 1 d . . . F1 F 0.8781(9) 0.2093(7) 0.5055(4) 0.0471(17) Uiso 0.645(7) 1 d P . . F2 F 0.5320(9) 0.3874(7) 0.5708(5) 0.0477(17) Uiso 0.645(7) 1 d P . . F3 F 0.7374(9) 0.2149(7) 0.6287(4) 0.0526(17) Uiso 0.645(7) 1 d P . . F4 F 0.6741(14) 0.3720(12) 0.4426(6) 0.088(3) Uiso 0.645(7) 1 d P . . F5 F 0.5597(10) 0.1734(9) 0.4986(6) 0.069(2) Uiso 0.645(7) 1 d P . . F6 F 0.8567(11) 0.4178(9) 0.5724(5) 0.068(2) Uiso 0.645(7) 1 d P . . F1B F 0.9069(14) 0.2327(12) 0.5315(7) 0.042(3) Uiso 0.355(7) 1 d P . . F2B F 0.5039(16) 0.3967(12) 0.5440(8) 0.045(3) Uiso 0.355(7) 1 d P . . F3B F 0.753(3) 0.323(2) 0.6439(12) 0.099(6) Uiso 0.355(7) 1 d P . . F4B F 0.626(2) 0.3112(18) 0.4351(9) 0.072(4) Uiso 0.355(7) 1 d P . . F5B F 0.589(2) 0.1588(18) 0.5451(12) 0.083(5) Uiso 0.355(7) 1 d P . . F6B F 0.811(2) 0.4570(18) 0.5310(11) 0.078(5) Uiso 0.355(7) 1 d P . . Sb2 Sb 0.09595(5) 0.47933(4) -0.02810(2) 0.03949(11) Uani 1 1 d . . . F7A F 0.2600(10) 0.4204(8) -0.0830(4) 0.064(2) Uiso 0.645(7) 1 d P . . F8A F -0.0608(11) 0.5285(9) 0.0275(5) 0.069(2) Uiso 0.645(7) 1 d P . . F9A F 0.0089(16) 0.5646(14) -0.1143(7) 0.111(4) Uiso 0.645(7) 1 d P . . F10A F 0.2006(12) 0.3866(11) 0.0553(6) 0.086(3) Uiso 0.645(7) 1 d P . . F11A F 0.2708(10) 0.5782(9) 0.0195(5) 0.061(2) Uiso 0.645(7) 1 d P . . F12A F -0.0807(13) 0.3918(11) -0.0750(5) 0.081(3) Uiso 0.645(7) 1 d P . . F7B F 0.1964(16) 0.4731(15) -0.1133(7) 0.057(3) Uiso 0.355(7) 1 d P . . F9B F -0.003(2) 0.635(2) -0.0596(11) 0.087(5) Uiso 0.355(7) 1 d P . . F12B F -0.0258(15) 0.3339(13) -0.0585(7) 0.048(3) Uiso 0.355(7) 1 d P . . F11B F 0.2198(17) 0.6169(13) -0.0040(7) 0.050(3) Uiso 0.355(7) 1 d P . . F8B F -0.001(3) 0.491(2) 0.0633(13) 0.102(6) Uiso 0.355(7) 1 d P . . F10B F 0.176(3) 0.328(3) 0.0113(15) 0.117(8) Uiso 0.355(7) 1 d P . . O2 O 0.0394(18) 0.0386(18) 0.2464(8) 0.088(5) Uani 0.50 1 d P . . 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 Rh1 0.02334(18) 0.02976(19) 0.03220(19) 0.00096(17) 0.01017(13) 0.00398(16) N1 0.047(3) 0.044(3) 0.044(3) 0.011(3) 0.031(2) 0.018(3) N2 0.023(2) 0.033(2) 0.031(2) 0.0016(18) 0.0097(16) 0.0030(18) N3 0.032(2) 0.048(3) 0.035(2) 0.004(2) 0.0130(18) 0.005(2) O1 0.026(2) 0.067(4) 0.091(4) -0.025(3) 0.013(2) 0.000(2) C1 0.028(2) 0.038(3) 0.036(3) 0.001(3) 0.0129(19) 0.011(3) C2 0.027(3) 0.045(3) 0.041(3) -0.005(3) 0.011(2) 0.008(2) C3 0.034(3) 0.035(3) 0.049(3) -0.003(3) 0.017(2) 0.003(3) C4 0.032(3) 0.039(3) 0.045(3) 0.003(3) 0.009(2) 0.013(3) C5 0.022(2) 0.038(3) 0.044(3) -0.002(3) 0.0098(19) 0.010(2) C6 0.045(3) 0.053(4) 0.047(3) 0.011(3) 0.029(3) 0.009(3) C7 0.038(4) 0.069(5) 0.053(4) -0.016(4) 0.002(3) 0.004(3) C8 0.050(4) 0.034(4) 0.074(5) -0.002(3) 0.022(3) 0.008(3) C9 0.051(4) 0.069(5) 0.044(3) 0.018(3) 0.009(3) 0.025(4) C10 0.025(3) 0.060(5) 0.058(4) -0.009(3) 0.009(2) 0.007(3) C11 0.088(6) 0.053(5) 0.087(6) 0.030(5) 0.066(5) 0.031(4) C12 0.057(4) 0.051(4) 0.063(4) 0.023(4) 0.040(4) 0.013(3) C13 0.043(3) 0.049(4) 0.046(3) -0.010(3) 0.023(3) -0.004(3) C14 0.032(3) 0.034(3) 0.033(3) 0.006(2) 0.012(2) 0.005(2) C15 0.031(3) 0.033(3) 0.034(3) -0.001(2) 0.0123(19) 0.000(2) C16 0.037(3) 0.031(3) 0.032(3) 0.002(2) 0.012(2) 0.006(2) C17 0.041(3) 0.038(3) 0.044(3) 0.004(3) 0.007(2) 0.007(3) C18 0.033(3) 0.032(3) 0.039(3) 0.005(2) 0.008(2) 0.009(2) C19 0.038(3) 0.043(4) 0.045(3) 0.013(3) 0.018(2) 0.010(3) C20 0.042(4) 0.053(5) 0.088(6) 0.019(4) 0.025(4) -0.001(3) C21 0.030(3) 0.064(6) 0.107(7) 0.005(5) 0.005(4) -0.004(4) C22 0.048(4) 0.062(5) 0.068(5) -0.004(4) -0.002(3) -0.006(4) C23 0.038(3) 0.046(4) 0.042(3) -0.001(3) 0.007(2) -0.003(3) Sb1 0.0427(2) 0.0498(3) 0.0400(2) 0.00898(19) 0.01824(16) 0.00605(19) Sb2 0.03067(19) 0.0469(2) 0.0406(2) 0.00798(18) 0.00472(14) 0.00261(18) O2 0.074(9) 0.106(13) 0.080(9) -0.007(9) 0.005(7) -0.034(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N1 2.080(4) . ? Rh1 C5 2.137(5) . ? Rh1 C4 2.137(6) . ? Rh1 C3 2.140(6) . ? Rh1 N2 2.155(5) . ? Rh1 C2 2.163(6) . ? Rh1 C1 2.168(5) . ? Rh1 O1 2.190(5) . ? N1 C14 1.329(8) . ? N1 C11 1.346(9) . ? N2 C15 1.284(7) . ? N2 C16 1.470(7) . ? N3 C12 1.350(10) . ? N3 C14 1.356(7) . ? N3 C13 1.440(9) . ? O1 H1A 0.9769 . ? O1 H1B 0.9795 . ? C1 C2 1.423(10) . ? C1 C5 1.449(8) . ? C1 C6 1.491(9) . ? C2 C3 1.429(9) . ? C2 C7 1.470(9) . ? C3 C4 1.433(9) . ? C3 C8 1.517(10) . ? C4 C5 1.421(9) . ? C4 C9 1.516(9) . ? C5 C10 1.501(10) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.378(11) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.429(8) . ? C15 H15 0.9500 . ? C16 C17 1.528(8) . ? C16 C18 1.542(9) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.390(9) . ? C18 C19 1.395(8) . ? C19 C20 1.389(11) . ? C19 H19 0.9500 . ? C20 C21 1.396(13) . ? C20 H20 0.9500 . ? C21 C22 1.363(13) . ? C21 H21 0.9500 . ? C22 C23 1.394(10) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? Sb1 F6 1.796(9) . ? Sb1 F1B 1.840(11) . ? Sb1 F2 1.841(7) . ? Sb1 F4 1.847(11) . ? Sb1 F4B 1.857(16) . ? Sb1 F5B 1.86(2) . ? Sb1 F3 1.883(7) . ? Sb1 F3B 1.89(2) . ? Sb1 F6B 1.901(19) . ? Sb1 F5 1.912(9) . ? Sb1 F1 1.913(7) . ? Sb1 F2B 1.932(13) . ? F1 F1B 0.550(12) . ? F2 F2B 0.509(13) . ? F3 F3B 1.22(2) . ? F4 F4B 0.772(18) . ? F5 F5B 0.847(18) . ? F6 F6B 0.888(17) . ? Sb2 F8A 1.816(8) . ? Sb2 F12A 1.816(10) . ? Sb2 F11B 1.825(13) . ? Sb2 F7B 1.844(13) . ? Sb2 F9A 1.850(13) . ? Sb2 F11A 1.879(8) . ? Sb2 F10B 1.88(3) . ? Sb2 F7A 1.889(8) . ? Sb2 F10A 1.896(10) . ? Sb2 F12B 1.908(13) . ? Sb2 F8B 1.93(2) . ? Sb2 F9B 1.93(2) . ? F7A F7B 0.898(14) . ? F8A F8B 0.85(2) . ? F9A F9B 1.27(2) . ? F10A F10B 1.01(3) . ? F11A F11B 0.688(13) . ? F12A F12B 0.804(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Rh1 C5 122.2(2) . . ? N1 Rh1 C4 98.6(2) . . ? C5 Rh1 C4 38.8(3) . . ? N1 Rh1 C3 108.5(2) . . ? C5 Rh1 C3 65.7(2) . . ? C4 Rh1 C3 39.1(3) . . ? N1 Rh1 N2 76.9(2) . . ? C5 Rh1 N2 104.3(2) . . ? C4 Rh1 N2 132.9(2) . . ? C3 Rh1 N2 170.0(2) . . ? N1 Rh1 C2 144.3(3) . . ? C5 Rh1 C2 65.3(2) . . ? C4 Rh1 C2 64.9(2) . . ? C3 Rh1 C2 38.8(3) . . ? N2 Rh1 C2 138.0(2) . . ? N1 Rh1 C1 161.4(2) . . ? C5 Rh1 C1 39.3(2) . . ? C4 Rh1 C1 64.9(2) . . ? C3 Rh1 C1 65.0(3) . . ? N2 Rh1 C1 107.2(2) . . ? C2 Rh1 C1 38.4(3) . . ? N1 Rh1 O1 82.1(2) . . ? C5 Rh1 O1 155.7(2) . . ? C4 Rh1 O1 145.7(3) . . ? C3 Rh1 O1 107.9(2) . . ? N2 Rh1 O1 80.9(2) . . ? C2 Rh1 O1 94.7(2) . . ? C1 Rh1 O1 116.4(2) . . ? C14 N1 C11 106.3(5) . . ? C14 N1 Rh1 114.0(4) . . ? C11 N1 Rh1 139.5(6) . . ? C15 N2 C16 119.2(5) . . ? C15 N2 Rh1 114.3(4) . . ? C16 N2 Rh1 126.1(3) . . ? C12 N3 C14 106.8(5) . . ? C12 N3 C13 126.7(5) . . ? C14 N3 C13 126.4(6) . . ? Rh1 O1 H1A 109.3 . . ? Rh1 O1 H1B 109.2 . . ? H1A O1 H1B 109.8 . . ? C2 C1 C5 107.8(6) . . ? C2 C1 C6 124.8(6) . . ? C5 C1 C6 127.3(6) . . ? C2 C1 Rh1 70.6(3) . . ? C5 C1 Rh1 69.2(3) . . ? C6 C1 Rh1 128.4(4) . . ? C1 C2 C3 108.6(5) . . ? C1 C2 C7 127.1(7) . . ? C3 C2 C7 124.3(7) . . ? C1 C2 Rh1 71.0(3) . . ? C3 C2 Rh1 69.7(3) . . ? C7 C2 Rh1 125.9(4) . . ? C2 C3 C4 107.5(6) . . ? C2 C3 C8 127.3(6) . . ? C4 C3 C8 125.0(6) . . ? C2 C3 Rh1 71.5(4) . . ? C4 C3 Rh1 70.3(3) . . ? C8 C3 Rh1 127.7(4) . . ? C5 C4 C3 108.8(5) . . ? C5 C4 C9 125.5(7) . . ? C3 C4 C9 125.6(7) . . ? C5 C4 Rh1 70.6(3) . . ? C3 C4 Rh1 70.5(3) . . ? C9 C4 Rh1 127.1(5) . . ? C4 C5 C1 107.3(6) . . ? C4 C5 C10 126.5(6) . . ? C1 C5 C10 126.0(6) . . ? C4 C5 Rh1 70.6(3) . . ? C1 C5 Rh1 71.5(3) . . ? C10 C5 Rh1 127.0(4) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C12 109.2(7) . . ? N1 C11 H11 125.4 . . ? C12 C11 H11 125.4 . . ? N3 C12 C11 106.8(6) . . ? N3 C12 H12 126.6 . . ? C11 C12 H12 126.6 . . ? N3 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 N3 110.9(5) . . ? N1 C14 C15 118.5(5) . . ? N3 C14 C15 130.6(6) . . ? N2 C15 C14 116.3(5) . . ? N2 C15 H15 121.8 . . ? C14 C15 H15 121.8 . . ? N2 C16 C17 114.9(5) . . ? N2 C16 C18 110.8(5) . . ? C17 C16 C18 110.4(5) . . ? N2 C16 H16 106.7 . . ? C17 C16 H16 106.7 . . ? C18 C16 H16 106.7 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 119.3(6) . . ? C23 C18 C16 122.5(5) . . ? C19 C18 C16 118.2(6) . . ? C20 C19 C18 119.4(7) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C19 C20 C21 120.9(7) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C22 C21 C20 119.5(7) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C21 C22 C23 120.4(8) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C18 C23 C22 120.6(7) . . ? C18 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? F6 Sb1 F1B 75.1(5) . . ? F6 Sb1 F2 93.4(4) . . ? F1B Sb1 F2 163.8(5) . . ? F6 Sb1 F4 91.2(5) . . ? F1B Sb1 F4 95.8(5) . . ? F2 Sb1 F4 95.8(4) . . ? F6 Sb1 F4B 114.9(7) . . ? F1B Sb1 F4B 97.0(6) . . ? F2 Sb1 F4B 98.2(6) . . ? F4 Sb1 F4B 24.1(6) . . ? F6 Sb1 F5B 153.6(7) . . ? F1B Sb1 F5B 95.9(7) . . ? F2 Sb1 F5B 89.5(6) . . ? F4 Sb1 F5B 114.5(7) . . ? F4B Sb1 F5B 90.6(9) . . ? F6 Sb1 F3 93.7(4) . . ? F1B Sb1 F3 80.0(4) . . ? F2 Sb1 F3 89.6(3) . . ? F4 Sb1 F3 172.5(5) . . ? F4B Sb1 F3 149.7(6) . . ? F5B Sb1 F3 60.1(7) . . ? F6 Sb1 F3B 63.5(8) . . ? F1B Sb1 F3B 93.6(8) . . ? F2 Sb1 F3B 70.8(7) . . ? F4 Sb1 F3B 149.6(8) . . ? F4B Sb1 F3B 168.4(9) . . ? F5B Sb1 F3B 93.0(9) . . ? F3 Sb1 F3B 37.6(7) . . ? F6 Sb1 F6B 27.6(5) . . ? F1B Sb1 F6B 87.1(7) . . ? F2 Sb1 F6B 87.6(6) . . ? F4 Sb1 F6B 65.0(7) . . ? F4B Sb1 F6B 89.1(8) . . ? F5B Sb1 F6B 177.0(8) . . ? F3 Sb1 F6B 120.7(6) . . ? F3B Sb1 F6B 86.7(9) . . ? F6 Sb1 F5 174.2(4) . . ? F1B Sb1 F5 99.2(5) . . ? F2 Sb1 F5 92.3(3) . . ? F4 Sb1 F5 88.6(5) . . ? F4B Sb1 F5 64.7(7) . . ? F5B Sb1 F5 25.9(6) . . ? F3 Sb1 F5 85.9(4) . . ? F3B Sb1 F5 118.2(8) . . ? F6B Sb1 F5 153.5(6) . . ? F6 Sb1 F1 88.9(4) . . ? F1B Sb1 F1 16.7(4) . . ? F2 Sb1 F1 176.9(3) . . ? F4 Sb1 F1 86.2(4) . . ? F4B Sb1 F1 82.6(6) . . ? F5B Sb1 F1 87.5(6) . . ? F3 Sb1 F1 88.3(3) . . ? F3B Sb1 F1 108.6(7) . . ? F6B Sb1 F1 95.4(6) . . ? F5 Sb1 F1 85.3(4) . . ? F6 Sb1 F2B 98.9(5) . . ? F1B Sb1 F2B 173.4(6) . . ? F2 Sb1 F2B 15.3(4) . . ? F4 Sb1 F2B 81.4(6) . . ? F4B Sb1 F2B 82.9(7) . . ? F5B Sb1 F2B 90.8(7) . . ? F3 Sb1 F2B 103.4(5) . . ? F3B Sb1 F2B 86.0(8) . . ? F6B Sb1 F2B 86.2(6) . . ? F5 Sb1 F2B 86.8(5) . . ? F1 Sb1 F2B 165.5(5) . . ? F1B F1 Sb1 74.1(15) . . ? F2B F2 Sb1 93(2) . . ? F3B F3 Sb1 71.6(11) . . ? F4B F4 Sb1 78.6(16) . . ? F5B F5 Sb1 73.4(15) . . ? F6B F6 Sb1 82.8(13) . . ? F1 F1B Sb1 89.2(16) . . ? F2 F2B Sb1 72.1(19) . . ? F3 F3B Sb1 70.7(11) . . ? F4 F4B Sb1 77.3(16) . . ? F5 F5B Sb1 80.7(16) . . ? F6 F6B Sb1 69.6(13) . . ? F8A Sb2 F12A 81.0(4) . . ? F8A Sb2 F11B 91.8(5) . . ? F12A Sb2 F11B 155.5(6) . . ? F8A Sb2 F7B 154.9(6) . . ? F12A Sb2 F7B 90.8(5) . . ? F11B Sb2 F7B 86.0(6) . . ? F8A Sb2 F9A 95.9(5) . . ? F12A Sb2 F9A 73.1(6) . . ? F11B Sb2 F9A 84.5(6) . . ? F7B Sb2 F9A 59.0(6) . . ? F8A Sb2 F11A 97.0(4) . . ? F12A Sb2 F11A 176.6(5) . . ? F11B Sb2 F11A 21.3(4) . . ? F7B Sb2 F11A 89.9(5) . . ? F9A Sb2 F11A 104.5(5) . . ? F8A Sb2 F10B 106.6(9) . . ? F12A Sb2 F10B 84.8(9) . . ? F11B Sb2 F10B 119.7(9) . . ? F7B Sb2 F10B 96.2(9) . . ? F9A Sb2 F10B 145.5(10) . . ? F11A Sb2 F10B 98.4(9) . . ? F8A Sb2 F7A 177.0(4) . . ? F12A Sb2 F7A 98.4(4) . . ? F11B Sb2 F7A 90.0(5) . . ? F7B Sb2 F7A 27.8(4) . . ? F9A Sb2 F7A 86.7(5) . . ? F11A Sb2 F7A 83.8(4) . . ? F10B Sb2 F7A 70.4(8) . . ? F8A Sb2 F10A 89.4(4) . . ? F12A Sb2 F10A 107.7(5) . . ? F11B Sb2 F10A 95.4(6) . . ? F7B Sb2 F10A 115.8(6) . . ? F9A Sb2 F10A 174.8(5) . . ? F11A Sb2 F10A 74.9(4) . . ? F10B Sb2 F10A 31.2(8) . . ? F7A Sb2 F10A 88.0(4) . . ? F8A Sb2 F12B 91.7(5) . . ? F12A Sb2 F12B 24.8(4) . . ? F11B Sb2 F12B 176.4(6) . . ? F7B Sb2 F12B 90.4(6) . . ? F9A Sb2 F12B 94.1(6) . . ? F11A Sb2 F12B 158.5(5) . . ? F10B Sb2 F12B 60.2(10) . . ? F7A Sb2 F12B 86.6(5) . . ? F10A Sb2 F12B 85.7(5) . . ? F8A Sb2 F8B 26.0(7) . . ? F12A Sb2 F8B 91.9(7) . . ? F11B Sb2 F8B 91.5(8) . . ? F7B Sb2 F8B 177.3(8) . . ? F9A Sb2 F8B 121.8(9) . . ? F11A Sb2 F8B 87.4(7) . . ? F10B Sb2 F8B 84.2(11) . . ? F7A Sb2 F8B 151.5(8) . . ? F10A Sb2 F8B 63.5(8) . . ? F12B Sb2 F8B 92.1(8) . . ? F8A Sb2 F9B 66.7(6) . . ? F12A Sb2 F9B 94.0(7) . . ? F11B Sb2 F9B 61.8(8) . . ? F7B Sb2 F9B 90.4(7) . . ? F9A Sb2 F9B 39.0(6) . . ? F11A Sb2 F9B 82.7(7) . . ? F10B Sb2 F9B 173.3(10) . . ? F7A Sb2 F9B 116.3(6) . . ? F10A Sb2 F9B 144.9(7) . . ? F12B Sb2 F9B 118.8(7) . . ? F8B Sb2 F9B 89.2(10) . . ? F7B F7A Sb2 73.3(10) . . ? F8B F8A Sb2 84.5(17) . . ? F9B F9A Sb2 74.1(10) . . ? F10B F10A Sb2 73.7(17) . . ? F11B F11A Sb2 75.0(13) . . ? F12B F12A Sb2 84.0(12) . . ? F7A F7B Sb2 78.9(10) . . ? F9A F9B Sb2 66.9(11) . . ? F12A F12B Sb2 71.2(12) . . ? F11A F11B Sb2 83.7(14) . . ? F8A F8B Sb2 69.5(16) . . ? F10A F10B Sb2 75.2(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 Rh1 N1 C14 100.5(5) . . . . ? C4 Rh1 N1 C14 133.9(5) . . . . ? C3 Rh1 N1 C14 172.9(5) . . . . ? N2 Rh1 N1 C14 1.7(5) . . . . ? C2 Rh1 N1 C14 -167.8(4) . . . . ? C1 Rh1 N1 C14 106.7(8) . . . . ? O1 Rh1 N1 C14 -80.8(5) . . . . ? C5 Rh1 N1 C11 -86.1(10) . . . . ? C4 Rh1 N1 C11 -52.7(10) . . . . ? C3 Rh1 N1 C11 -13.7(10) . . . . ? N2 Rh1 N1 C11 175.1(10) . . . . ? C2 Rh1 N1 C11 5.6(12) . . . . ? C1 Rh1 N1 C11 -79.9(14) . . . . ? O1 Rh1 N1 C11 92.6(10) . . . . ? N1 Rh1 N2 C15 -2.9(4) . . . . ? C5 Rh1 N2 C15 -123.2(4) . . . . ? C4 Rh1 N2 C15 -92.5(5) . . . . ? C2 Rh1 N2 C15 168.0(4) . . . . ? C1 Rh1 N2 C15 -164.0(4) . . . . ? O1 Rh1 N2 C15 81.1(4) . . . . ? N1 Rh1 N2 C16 -175.4(5) . . . . ? C5 Rh1 N2 C16 64.2(5) . . . . ? C4 Rh1 N2 C16 94.9(5) . . . . ? C2 Rh1 N2 C16 -4.6(6) . . . . ? C1 Rh1 N2 C16 23.4(5) . . . . ? O1 Rh1 N2 C16 -91.5(5) . . . . ? N1 Rh1 C1 C2 110.5(8) . . . . ? C5 Rh1 C1 C2 118.7(6) . . . . ? C4 Rh1 C1 C2 80.5(4) . . . . ? C3 Rh1 C1 C2 37.1(4) . . . . ? N2 Rh1 C1 C2 -149.6(3) . . . . ? O1 Rh1 C1 C2 -61.3(4) . . . . ? N1 Rh1 C1 C5 -8.3(10) . . . . ? C4 Rh1 C1 C5 -38.2(4) . . . . ? C3 Rh1 C1 C5 -81.6(4) . . . . ? N2 Rh1 C1 C5 91.7(4) . . . . ? C2 Rh1 C1 C5 -118.7(6) . . . . ? O1 Rh1 C1 C5 180.0(4) . . . . ? N1 Rh1 C1 C6 -130.0(8) . . . . ? C5 Rh1 C1 C6 -121.7(8) . . . . ? C4 Rh1 C1 C6 -159.9(7) . . . . ? C3 Rh1 C1 C6 156.7(7) . . . . ? N2 Rh1 C1 C6 -30.0(6) . . . . ? C2 Rh1 C1 C6 119.6(7) . . . . ? O1 Rh1 C1 C6 58.2(7) . . . . ? C5 C1 C2 C3 -0.4(6) . . . . ? C6 C1 C2 C3 176.2(5) . . . . ? Rh1 C1 C2 C3 -59.9(4) . . . . ? C5 C1 C2 C7 -179.4(6) . . . . ? C6 C1 C2 C7 -2.8(9) . . . . ? Rh1 C1 C2 C7 121.1(6) . . . . ? C5 C1 C2 Rh1 59.4(3) . . . . ? C6 C1 C2 Rh1 -123.9(6) . . . . ? N1 Rh1 C2 C1 -149.1(4) . . . . ? C5 Rh1 C2 C1 -37.7(3) . . . . ? C4 Rh1 C2 C1 -80.7(4) . . . . ? C3 Rh1 C2 C1 -119.1(5) . . . . ? N2 Rh1 C2 C1 46.3(5) . . . . ? O1 Rh1 C2 C1 127.9(4) . . . . ? N1 Rh1 C2 C3 -30.0(6) . . . . ? C5 Rh1 C2 C3 81.4(4) . . . . ? C4 Rh1 C2 C3 38.4(4) . . . . ? N2 Rh1 C2 C3 165.4(3) . . . . ? C1 Rh1 C2 C3 119.1(5) . . . . ? O1 Rh1 C2 C3 -113.0(4) . . . . ? N1 Rh1 C2 C7 88.3(8) . . . . ? C5 Rh1 C2 C7 -160.3(8) . . . . ? C4 Rh1 C2 C7 156.7(8) . . . . ? C3 Rh1 C2 C7 118.4(8) . . . . ? N2 Rh1 C2 C7 -76.2(7) . . . . ? C1 Rh1 C2 C7 -122.6(8) . . . . ? O1 Rh1 C2 C7 5.4(7) . . . . ? C1 C2 C3 C4 -0.8(6) . . . . ? C7 C2 C3 C4 178.2(6) . . . . ? Rh1 C2 C3 C4 -61.5(4) . . . . ? C1 C2 C3 C8 -175.6(6) . . . . ? C7 C2 C3 C8 3.4(10) . . . . ? Rh1 C2 C3 C8 123.7(6) . . . . ? C1 C2 C3 Rh1 60.7(4) . . . . ? C7 C2 C3 Rh1 -120.3(6) . . . . ? N1 Rh1 C3 C2 162.1(4) . . . . ? C5 Rh1 C3 C2 -80.2(4) . . . . ? C4 Rh1 C3 C2 -117.1(5) . . . . ? C1 Rh1 C3 C2 -36.8(3) . . . . ? O1 Rh1 C3 C2 74.6(4) . . . . ? N1 Rh1 C3 C4 -80.8(4) . . . . ? C5 Rh1 C3 C4 36.9(3) . . . . ? C2 Rh1 C3 C4 117.1(5) . . . . ? C1 Rh1 C3 C4 80.4(4) . . . . ? O1 Rh1 C3 C4 -168.3(4) . . . . ? N1 Rh1 C3 C8 38.8(7) . . . . ? C5 Rh1 C3 C8 156.6(7) . . . . ? C4 Rh1 C3 C8 119.6(8) . . . . ? C2 Rh1 C3 C8 -123.3(8) . . . . ? C1 Rh1 C3 C8 -160.0(7) . . . . ? O1 Rh1 C3 C8 -48.7(7) . . . . ? C2 C3 C4 C5 1.8(6) . . . . ? C8 C3 C4 C5 176.7(5) . . . . ? Rh1 C3 C4 C5 -60.4(4) . . . . ? C2 C3 C4 C9 -175.5(6) . . . . ? C8 C3 C4 C9 -0.5(10) . . . . ? Rh1 C3 C4 C9 122.3(6) . . . . ? C2 C3 C4 Rh1 62.2(4) . . . . ? C8 C3 C4 Rh1 -122.8(6) . . . . ? N1 Rh1 C4 C5 -132.1(4) . . . . ? C3 Rh1 C4 C5 119.2(5) . . . . ? N2 Rh1 C4 C5 -52.0(4) . . . . ? C2 Rh1 C4 C5 81.2(4) . . . . ? C1 Rh1 C4 C5 38.6(4) . . . . ? O1 Rh1 C4 C5 139.3(4) . . . . ? N1 Rh1 C4 C3 108.7(4) . . . . ? C5 Rh1 C4 C3 -119.2(5) . . . . ? N2 Rh1 C4 C3 -171.2(3) . . . . ? C2 Rh1 C4 C3 -38.0(4) . . . . ? C1 Rh1 C4 C3 -80.5(4) . . . . ? O1 Rh1 C4 C3 20.1(6) . . . . ? N1 Rh1 C4 C9 -11.8(7) . . . . ? C5 Rh1 C4 C9 120.3(8) . . . . ? C3 Rh1 C4 C9 -120.5(8) . . . . ? N2 Rh1 C4 C9 68.3(8) . . . . ? C2 Rh1 C4 C9 -158.5(8) . . . . ? C1 Rh1 C4 C9 158.9(8) . . . . ? O1 Rh1 C4 C9 -100.4(7) . . . . ? C3 C4 C5 C1 -2.0(6) . . . . ? C9 C4 C5 C1 175.2(6) . . . . ? Rh1 C4 C5 C1 -62.5(4) . . . . ? C3 C4 C5 C10 -177.4(5) . . . . ? C9 C4 C5 C10 -0.2(9) . . . . ? Rh1 C4 C5 C10 122.2(6) . . . . ? C3 C4 C5 Rh1 60.4(4) . . . . ? C9 C4 C5 Rh1 -122.3(6) . . . . ? C2 C1 C5 C4 1.5(6) . . . . ? C6 C1 C5 C4 -175.0(5) . . . . ? Rh1 C1 C5 C4 61.9(4) . . . . ? C2 C1 C5 C10 176.9(5) . . . . ? C6 C1 C5 C10 0.3(9) . . . . ? Rh1 C1 C5 C10 -122.7(6) . . . . ? C2 C1 C5 Rh1 -60.3(4) . . . . ? C6 C1 C5 Rh1 123.1(6) . . . . ? N1 Rh1 C5 C4 60.1(5) . . . . ? C3 Rh1 C5 C4 -37.2(4) . . . . ? N2 Rh1 C5 C4 143.4(4) . . . . ? C2 Rh1 C5 C4 -80.0(4) . . . . ? C1 Rh1 C5 C4 -116.8(6) . . . . ? O1 Rh1 C5 C4 -116.8(6) . . . . ? N1 Rh1 C5 C1 176.9(4) . . . . ? C4 Rh1 C5 C1 116.8(6) . . . . ? C3 Rh1 C5 C1 79.6(4) . . . . ? N2 Rh1 C5 C1 -99.8(4) . . . . ? C2 Rh1 C5 C1 36.8(4) . . . . ? O1 Rh1 C5 C1 -0.1(8) . . . . ? N1 Rh1 C5 C10 -61.5(7) . . . . ? C4 Rh1 C5 C10 -121.6(7) . . . . ? C3 Rh1 C5 C10 -158.8(6) . . . . ? N2 Rh1 C5 C10 21.8(6) . . . . ? C2 Rh1 C5 C10 158.4(7) . . . . ? C1 Rh1 C5 C10 121.6(8) . . . . ? O1 Rh1 C5 C10 121.6(7) . . . . ? C14 N1 C11 C12 -0.9(11) . . . . ? Rh1 N1 C11 C12 -174.6(6) . . . . ? C14 N3 C12 C11 0.2(10) . . . . ? C13 N3 C12 C11 -176.1(8) . . . . ? N1 C11 C12 N3 0.5(12) . . . . ? C11 N1 C14 N3 1.0(9) . . . . ? Rh1 N1 C14 N3 176.6(4) . . . . ? C11 N1 C14 C15 -176.0(7) . . . . ? Rh1 N1 C14 C15 -0.5(7) . . . . ? C12 N3 C14 N1 -0.8(8) . . . . ? C13 N3 C14 N1 175.5(6) . . . . ? C12 N3 C14 C15 175.9(7) . . . . ? C13 N3 C14 C15 -7.8(10) . . . . ? C16 N2 C15 C14 176.6(5) . . . . ? Rh1 N2 C15 C14 3.5(6) . . . . ? N1 C14 C15 N2 -2.1(8) . . . . ? N3 C14 C15 N2 -178.5(6) . . . . ? C15 N2 C16 C17 -34.9(8) . . . . ? Rh1 N2 C16 C17 137.4(4) . . . . ? C15 N2 C16 C18 91.2(6) . . . . ? Rh1 N2 C16 C18 -96.5(5) . . . . ? N2 C16 C18 C23 -41.7(8) . . . . ? C17 C16 C18 C23 86.8(7) . . . . ? N2 C16 C18 C19 141.2(5) . . . . ? C17 C16 C18 C19 -90.3(7) . . . . ? C23 C18 C19 C20 -1.1(10) . . . . ? C16 C18 C19 C20 176.1(6) . . . . ? C18 C19 C20 C21 0.9(12) . . . . ? C19 C20 C21 C22 -0.6(14) . . . . ? C20 C21 C22 C23 0.4(14) . . . . ? C19 C18 C23 C22 1.0(11) . . . . ? C16 C18 C23 C22 -176.1(7) . . . . ? C21 C22 C23 C18 -0.6(13) . . . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.107 _refine_diff_density_min -0.614 _refine_diff_density_rms 0.114 _database_code_depnum_ccdc_archive 'CCDC 937405' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_cmpnd_10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H32 Ir N3 O, 2(F6 Sb), 1/2(H2O)' _chemical_formula_sum 'C23 H33 F12 Ir N3 O1.50 Sb2' _chemical_formula_weight 1039.22 _chemical_absolute_configuration rmad 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' Sb Sb -0.5866 1.5461 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.1389(5) _cell_length_b 10.9750(6) _cell_length_c 17.8510(10) _cell_angle_alpha 90.00 _cell_angle_beta 99.1760(10) _cell_angle_gamma 90.00 _cell_volume 1574.13(16) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 601 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 29.55 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.193 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 982 _exptl_absorpt_coefficient_mu 6.016 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.823 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ; Absorption corrections based on face indexing, including in APEX2 package (Bruker AXS, 2008). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX DUO system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 17157 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 29.55 _reflns_number_total 7912 _reflns_number_gt 7607 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_cell_refinement 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_data_reduction 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP program, SHELXTL v6.12, Bruker2000' _computing_publication_material ENCIFER _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. All non-hydrogen atoms of the coordination complex were refined with anisotropic displacement parameters. Hydrogen atoms have been included in the model in calculated positions and refined with positional and thermal riding parameters.Hydrogen atoms of the hydration water molecule have not been included in the model. The SbF6- counteranion exhibit fluorine disorder, modelized in the base of two fluorine positions with complementary occupancy factors (0.61/0.39 and 0.58/0.42).Geometrical restrains in Sb-F bond lengths have been included in the refinement. Maximal residual density peaks are found in the proximity of the disordered fragment, or close to the metal atom. They have no chemical sense. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0491P)^2^+2.5501P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.004(4) _refine_ls_number_reflns 7912 _refine_ls_number_parameters 390 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0302 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0739 _refine_ls_wR_factor_gt 0.0729 _refine_ls_goodness_of_fit_ref 0.942 _refine_ls_restrained_S_all 0.949 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL fjl76ds in P2(1) CELL 0.71073 8.1389 10.9750 17.8510 90.000 99.176 90.000 ZERR 2.00 0.0005 0.0006 0.0010 0.000 0.001 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O F SB IR UNIT 46 66 6 3 24 4 2 MERG 2 OMIT 0 0 1 OMIT 0 0 2 DFIX 3.74 0.020 F3A F4A DFIX 3.74 0.020 F5A F6A DFIX 3.74 0.020 F3B F4B DFIX 3.74 0.020 F5B F6B dfix 31.00 0.01 SB1 F1 SB1 F2 SB1 F3A SB1 F3B SB1 F4A dfix 31.00 0.01 SB1 F4B SB1 F5A SB1 F5B SB1 F6A SB1 F6B dfix 31.00 0.01 SB2 F7A SB2 F7B SB2 F8A SB2 F8B SB2 F9A SB2 F9B dfix 31.00 0.01 SB2 F10A SB2 F10B SB2 F11 SB2 F12 FMAP 2 PLAN 5 ACTA 55.00 BOND $H CONF L.S. 4 TEMP -173.00 WGHT 0.049100 2.550100 FVAR 0.28252 0.61008 1.86898 0.57998 IR1 7 0.443494 0.244269 0.225486 11.00000 0.02025 0.03344 = 0.03135 0.00459 0.00847 0.00639 N1 3 0.333036 0.237612 0.322211 11.00000 0.04605 0.05467 = 0.05290 0.02480 0.03088 0.02486 N2 3 0.391955 0.431070 0.248240 11.00000 0.02065 0.03746 = 0.02874 -0.00257 0.00381 -0.00085 N3 3 0.209442 0.326634 0.407654 11.00000 0.03210 0.06238 = 0.03338 0.00682 0.01210 0.00990 O1 4 0.183006 0.255477 0.173510 11.00000 0.01937 0.04310 = 0.09555 -0.01808 0.00829 -0.00061 AFIX 1 H1A 2 0.136961 0.172869 0.166009 11.00000 0.09928 H1B 2 0.174828 0.296209 0.124083 11.00000 0.13246 AFIX 0 C1 1 0.625086 0.243654 0.148850 11.00000 0.02059 0.04220 = 0.03270 -0.00068 0.00729 0.00984 C2 1 0.522387 0.137115 0.134434 11.00000 0.01919 0.04370 = 0.03927 -0.00252 0.00916 0.00425 C3 1 0.537162 0.065188 0.203701 11.00000 0.02504 0.04076 = 0.04429 0.00357 0.01348 0.00679 C4 1 0.654617 0.128828 0.259773 11.00000 0.02783 0.04673 = 0.03745 0.00595 0.00724 0.01121 C5 1 0.706218 0.236642 0.227033 11.00000 0.02298 0.04310 = 0.03718 -0.00406 0.00688 0.00813 C6 1 0.654688 0.334233 0.089626 11.00000 0.04018 0.05862 = 0.03551 0.00215 0.01984 0.00552 AFIX 137 H6A 2 0.749643 0.307925 0.066106 11.00000 -1.50000 H6B 2 0.678483 0.414225 0.113277 11.00000 -1.50000 H6C 2 0.555299 0.339790 0.050762 11.00000 -1.50000 AFIX 0 C7 1 0.413327 0.104475 0.061901 11.00000 0.02903 0.07377 = 0.04790 -0.02548 0.00145 0.00597 AFIX 137 H7A 2 0.367353 0.178909 0.036391 11.00000 -1.50000 H7B 2 0.322198 0.052347 0.072721 11.00000 -1.50000 H7C 2 0.478796 0.060728 0.028950 11.00000 -1.50000 AFIX 0 C8 1 0.461595 -0.054777 0.213524 11.00000 0.04235 0.04080 = 0.06779 0.00166 0.02443 0.00567 AFIX 137 H8A 2 0.529339 -0.118810 0.195335 11.00000 -1.50000 H8B 2 0.348903 -0.057163 0.184380 11.00000 -1.50000 H8C 2 0.456351 -0.068041 0.267381 11.00000 -1.50000 AFIX 0 C9 1 0.718081 0.081133 0.338604 11.00000 0.05174 0.06420 = 0.04165 0.01749 0.00156 0.02747 AFIX 137 H9A 2 0.623856 0.054252 0.362446 11.00000 -1.50000 H9B 2 0.778335 0.146008 0.369204 11.00000 -1.50000 H9C 2 0.793161 0.012246 0.335221 11.00000 -1.50000 AFIX 0 C10 1 0.834714 0.323703 0.264970 11.00000 0.02530 0.05804 = 0.04997 -0.01662 0.00109 0.00240 AFIX 137 H10A 2 0.821739 0.333438 0.318285 11.00000 -1.50000 H10B 2 0.820546 0.402877 0.239368 11.00000 -1.50000 H10C 2 0.946004 0.291808 0.262100 11.00000 -1.50000 AFIX 0 C11 1 0.282291 0.150459 0.367835 11.00000 0.09206 0.05663 = 0.10037 0.04389 0.07367 0.04145 AFIX 43 H11 2 0.296200 0.065026 0.363006 11.00000 -1.20000 AFIX 0 C12 1 0.208239 0.207022 0.421511 11.00000 0.05707 0.07849 = 0.05976 0.03715 0.03925 0.03086 AFIX 43 H12 2 0.163790 0.168508 0.461537 11.00000 -1.20000 AFIX 0 C13 1 0.148617 0.423676 0.452569 11.00000 0.04251 0.06931 = 0.04181 -0.01296 0.02093 -0.00500 AFIX 137 H13A 2 0.091770 0.387477 0.491609 11.00000 -1.50000 H13B 2 0.070629 0.475593 0.419279 11.00000 -1.50000 H13C 2 0.242789 0.472834 0.476846 11.00000 -1.50000 AFIX 0 C14 1 0.286485 0.342342 0.347038 11.00000 0.02637 0.05130 = 0.02928 0.00714 0.00923 0.00688 C15 1 0.314975 0.448301 0.305197 11.00000 0.02673 0.03718 = 0.03530 -0.00217 0.00953 -0.00056 AFIX 43 H15 2 0.279593 0.526848 0.318324 11.00000 -1.20000 AFIX 0 C16 1 0.418976 0.534910 0.198171 11.00000 0.03361 0.03142 = 0.03079 0.00308 0.00793 0.00631 AFIX 13 H16 2 0.423303 0.501182 0.146482 11.00000 -1.20000 AFIX 0 C17 1 0.279597 0.629486 0.190285 11.00000 0.03162 0.03887 = 0.04697 0.00017 0.00394 0.00579 AFIX 137 H17A 2 0.171926 0.588606 0.176662 11.00000 -1.50000 H17B 2 0.295026 0.688043 0.150546 11.00000 -1.50000 H17C 2 0.282413 0.672488 0.238586 11.00000 -1.50000 AFIX 0 C18 1 0.587903 0.594154 0.226652 11.00000 0.03101 0.03463 = 0.03290 0.00069 0.00708 0.00224 C19 1 0.681688 0.636500 0.172189 11.00000 0.04063 0.03937 = 0.04815 0.00721 0.01680 0.00427 AFIX 43 H19 2 0.643546 0.623686 0.119662 11.00000 -1.20000 AFIX 0 C20 1 0.831013 0.697395 0.196085 11.00000 0.03972 0.04792 = 0.08243 0.01101 0.02726 0.00072 AFIX 43 H20 2 0.894212 0.726586 0.159438 11.00000 -1.20000 AFIX 0 C21 1 0.887082 0.715486 0.270355 11.00000 0.02789 0.06353 = 0.08554 0.00208 0.00186 -0.00962 AFIX 43 H21 2 0.988607 0.757847 0.285845 11.00000 -1.20000 AFIX 0 C22 1 0.798131 0.673021 0.323076 11.00000 0.03964 0.06811 = 0.06027 -0.01543 -0.00519 -0.00672 AFIX 43 H22 2 0.839923 0.685258 0.375326 11.00000 -1.20000 AFIX 0 C23 1 0.647787 0.612193 0.302897 11.00000 0.03513 0.05944 = 0.04224 -0.00568 0.00824 -0.00506 AFIX 43 H23 2 0.587275 0.583545 0.340689 11.00000 -1.20000 AFIX 0 SB1 6 0.707356 0.305351 0.538913 11.00000 0.04163 0.06256 = 0.04189 0.01640 0.01781 0.01114 F1 5 0.892061 0.219829 0.516677 11.00000 0.05785 0.08455 = 0.11881 0.03122 0.04653 0.02921 F2 5 0.525106 0.391383 0.562857 11.00000 0.05281 0.07179 = 0.10111 -0.02005 0.03191 0.00847 F3A 5 0.735366 0.211606 0.628153 21.00000 0.05367 F4A 5 0.677078 0.374380 0.442577 21.00000 0.09536 F5A 5 0.562198 0.177715 0.496172 21.00000 0.08236 F6A 5 0.860451 0.420242 0.576239 21.00000 0.08145 F3B 5 0.778595 0.344755 0.642135 -21.00000 0.12534 F4B 5 0.631533 0.307704 0.435702 -21.00000 0.07340 F5B 5 0.594208 0.163734 0.556554 -21.00000 0.12072 F6B 5 0.796471 0.458849 0.520867 -21.00000 0.10121 SB2 6 0.094085 0.479534 -0.027454 11.00000 0.02422 0.05147 = 0.04073 0.00725 0.00083 0.00208 F7A 5 0.254606 0.414552 -0.083610 41.00000 0.05829 F8A 5 -0.059455 0.541961 0.026511 41.00000 0.06950 F9A 5 0.006964 0.569208 -0.113226 41.00000 0.07701 F10A 5 0.188158 0.377909 0.054364 41.00000 0.06324 F7B 5 0.203842 0.462283 -0.109732 -41.00000 0.04438 F8B 5 -0.022406 0.507688 0.055546 -41.00000 0.05898 F9B 5 -0.001336 0.627903 -0.068512 -41.00000 0.05795 F10B 5 0.190047 0.343521 0.022379 -41.00000 0.05950 F11 5 0.259111 0.587602 0.014462 11.00000 0.05613 0.09373 = 0.07445 -0.03065 0.02861 -0.02973 F12 5 -0.065240 0.369768 -0.069468 11.00000 0.07539 0.15999 = 0.07609 -0.03328 0.01489 -0.07414 O2 4 0.048637 0.042677 0.238480 10.50000 0.05237 0.06778 = 0.04935 -0.00622 -0.00168 -0.00988 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 REM fjl76ds in P2(1) REM R1 = 0.0288 for 7607 Fo > 4sig(Fo) and 0.0302 for all 7912 data REM 390 parameters refined using 25 restraints END ; 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.44349(2) 0.244269(19) 0.225486(10) 0.02787(5) Uani 1 1 d . . . N1 N 0.3330(7) 0.2376(7) 0.3222(3) 0.0487(13) Uani 1 1 d . . . N2 N 0.3920(5) 0.4311(4) 0.2482(2) 0.0290(9) Uani 1 1 d . . . N3 N 0.2094(7) 0.3266(6) 0.4077(3) 0.0419(12) Uani 1 1 d . . . O1 O 0.1830(5) 0.2555(5) 0.1735(3) 0.0528(12) Uani 1 1 d . . . H1A H 0.1370 0.1729 0.1660 0.099 Uiso 1 1 d . . . H1B H 0.1748 0.2962 0.1241 0.132 Uiso 1 1 d . . . C1 C 0.6251(5) 0.2437(7) 0.1488(3) 0.0315(9) Uani 1 1 d . . . C2 C 0.5224(6) 0.1371(5) 0.1344(3) 0.0336(11) Uani 1 1 d . . . C3 C 0.5372(7) 0.0652(6) 0.2037(3) 0.0358(12) Uani 1 1 d . . . C4 C 0.6546(7) 0.1288(6) 0.2598(3) 0.0371(12) Uani 1 1 d . . . C5 C 0.7062(6) 0.2366(7) 0.2270(3) 0.0342(10) Uani 1 1 d . . . C6 C 0.6547(8) 0.3342(7) 0.0896(3) 0.0433(14) Uani 1 1 d . . . H6A H 0.7496 0.3079 0.0661 0.065 Uiso 1 1 calc R . . H6B H 0.6785 0.4142 0.1133 0.065 Uiso 1 1 calc R . . H6C H 0.5553 0.3398 0.0508 0.065 Uiso 1 1 calc R . . C7 C 0.4133(8) 0.1045(8) 0.0619(4) 0.0507(17) Uani 1 1 d . . . H7A H 0.3674 0.1789 0.0364 0.076 Uiso 1 1 calc R . . H7B H 0.3222 0.0523 0.0727 0.076 Uiso 1 1 calc R . . H7C H 0.4788 0.0607 0.0289 0.076 Uiso 1 1 calc R . . C8 C 0.4616(9) -0.0548(7) 0.2135(5) 0.0486(17) Uani 1 1 d . . . H8A H 0.5293 -0.1188 0.1953 0.073 Uiso 1 1 calc R . . H8B H 0.3489 -0.0572 0.1844 0.073 Uiso 1 1 calc R . . H8C H 0.4564 -0.0680 0.2674 0.073 Uiso 1 1 calc R . . C9 C 0.7181(9) 0.0811(7) 0.3386(4) 0.0532(18) Uani 1 1 d . . . H9A H 0.6239 0.0543 0.3624 0.080 Uiso 1 1 calc R . . H9B H 0.7783 0.1460 0.3692 0.080 Uiso 1 1 calc R . . H9C H 0.7932 0.0122 0.3352 0.080 Uiso 1 1 calc R . . C10 C 0.8347(7) 0.3237(7) 0.2650(4) 0.0450(14) Uani 1 1 d . . . H10A H 0.8217 0.3334 0.3183 0.067 Uiso 1 1 calc R . . H10B H 0.8205 0.4029 0.2394 0.067 Uiso 1 1 calc R . . H10C H 0.9460 0.2918 0.2621 0.067 Uiso 1 1 calc R . . C11 C 0.2823(13) 0.1505(8) 0.3678(6) 0.077(3) Uani 1 1 d . . . H11 H 0.2962 0.0650 0.3630 0.092 Uiso 1 1 calc R . . C12 C 0.2082(10) 0.2070(8) 0.4215(5) 0.062(2) Uani 1 1 d . . . H12 H 0.1638 0.1685 0.4615 0.074 Uiso 1 1 calc R . . C13 C 0.1486(9) 0.4237(8) 0.4526(4) 0.0497(16) Uani 1 1 d . . . H13A H 0.0918 0.3875 0.4916 0.074 Uiso 1 1 calc R . . H13B H 0.0706 0.4756 0.4193 0.074 Uiso 1 1 calc R . . H13C H 0.2428 0.4728 0.4768 0.074 Uiso 1 1 calc R . . C14 C 0.2865(7) 0.3423(6) 0.3470(3) 0.0351(12) Uani 1 1 d . . . C15 C 0.3150(7) 0.4483(5) 0.3052(3) 0.0326(11) Uani 1 1 d . . . H15 H 0.2796 0.5268 0.3183 0.039 Uiso 1 1 calc R . . C16 C 0.4190(7) 0.5349(5) 0.1982(3) 0.0316(11) Uani 1 1 d . . . H16 H 0.4233 0.5012 0.1465 0.038 Uiso 1 1 calc R . . C17 C 0.2796(8) 0.6295(6) 0.1903(4) 0.0394(12) Uani 1 1 d . . . H17A H 0.1719 0.5886 0.1767 0.059 Uiso 1 1 calc R . . H17B H 0.2950 0.6880 0.1505 0.059 Uiso 1 1 calc R . . H17C H 0.2824 0.6725 0.2386 0.059 Uiso 1 1 calc R . . C18 C 0.5879(7) 0.5942(5) 0.2267(3) 0.0326(11) Uani 1 1 d . . . C19 C 0.6817(8) 0.6365(6) 0.1722(4) 0.0417(13) Uani 1 1 d . . . H19 H 0.6435 0.6237 0.1197 0.050 Uiso 1 1 calc R . . C20 C 0.8310(9) 0.6974(7) 0.1961(5) 0.0548(18) Uani 1 1 d . . . H20 H 0.8942 0.7266 0.1594 0.066 Uiso 1 1 calc R . . C21 C 0.8871(8) 0.7155(7) 0.2704(5) 0.060(2) Uani 1 1 d . . . H21 H 0.9886 0.7578 0.2858 0.072 Uiso 1 1 calc R . . C22 C 0.7981(9) 0.6730(8) 0.3231(5) 0.0574(18) Uani 1 1 d . . . H22 H 0.8399 0.6853 0.3753 0.069 Uiso 1 1 calc R . . C23 C 0.6478(8) 0.6122(7) 0.3029(4) 0.0454(14) Uani 1 1 d . . . H23 H 0.5873 0.5835 0.3407 0.054 Uiso 1 1 calc R . . Sb1 Sb 0.70736(6) 0.30535(5) 0.53891(2) 0.04747(11) Uani 1 1 d D . . F1 F 0.8921(6) 0.2198(5) 0.5167(4) 0.0835(18) Uani 1 1 d D . . F2 F 0.5251(6) 0.3914(5) 0.5629(3) 0.0731(14) Uani 1 1 d D . . F3A F 0.7354(9) 0.2116(6) 0.6282(3) 0.054(2) Uiso 0.610(10) 1 d PD . . F4A F 0.6771(15) 0.3744(12) 0.4426(5) 0.095(3) Uiso 0.610(10) 1 d PD . . F5A F 0.5622(11) 0.1777(8) 0.4962(6) 0.082(3) Uiso 0.610(10) 1 d PD . . F6A F 0.8605(11) 0.4202(8) 0.5762(6) 0.081(3) Uiso 0.610(10) 1 d PD . . F3B F 0.779(3) 0.345(2) 0.6421(6) 0.125(8) Uiso 0.390(10) 1 d PD . . F4B F 0.6315(18) 0.3077(15) 0.4357(5) 0.073(4) Uiso 0.390(10) 1 d PD . . F5B F 0.594(3) 0.1637(13) 0.5566(14) 0.121(7) Uiso 0.390(10) 1 d PD . . F6B F 0.796(2) 0.4588(11) 0.5209(11) 0.101(6) Uiso 0.390(10) 1 d PD . . Sb2 Sb 0.09408(5) 0.47953(4) -0.02745(2) 0.03928(10) Uani 1 1 d D . . F7A F 0.2546(10) 0.4146(8) -0.0836(5) 0.058(2) Uiso 0.580(11) 1 d PD . . F8A F -0.0595(11) 0.5420(9) 0.0265(6) 0.069(3) Uiso 0.580(11) 1 d PD . . F9A F 0.0070(12) 0.5692(9) -0.1132(5) 0.077(3) Uiso 0.580(11) 1 d PD . . F10A F 0.1882(11) 0.3779(8) 0.0544(5) 0.063(2) Uiso 0.580(11) 1 d PD . . F7B F 0.2038(12) 0.4623(9) -0.1097(5) 0.044(2) Uiso 0.420(11) 1 d PD . . F8B F -0.0224(15) 0.5077(11) 0.0555(6) 0.059(3) Uiso 0.420(11) 1 d PD . . F9B F -0.0013(13) 0.6279(8) -0.0685(6) 0.058(3) Uiso 0.420(11) 1 d PD . . F10B F 0.1900(14) 0.3435(9) 0.0224(7) 0.059(3) Uiso 0.420(11) 1 d PD . . F11 F 0.2591(6) 0.5876(5) 0.0145(3) 0.0728(14) Uani 1 1 d D . . F12 F -0.0652(7) 0.3698(7) -0.0695(3) 0.104(2) Uani 1 1 d D . . O2 O 0.0486(13) 0.0427(11) 0.2385(6) 0.058(3) Uani 0.50 1 d P . . 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 0.02025(8) 0.03344(9) 0.03135(9) 0.00459(9) 0.00847(6) 0.00639(8) N1 0.046(3) 0.055(3) 0.053(3) 0.025(3) 0.031(2) 0.025(3) N2 0.0206(19) 0.037(2) 0.029(2) -0.0026(18) 0.0038(16) -0.0008(16) N3 0.032(3) 0.062(4) 0.033(2) 0.007(2) 0.0121(19) 0.010(2) O1 0.0194(16) 0.043(2) 0.096(3) -0.018(3) 0.0083(18) -0.0006(19) C1 0.0206(19) 0.042(2) 0.033(2) -0.001(3) 0.0073(16) 0.010(3) C2 0.019(2) 0.044(3) 0.039(3) -0.003(2) 0.009(2) 0.0042(19) C3 0.025(2) 0.041(3) 0.044(3) 0.004(2) 0.013(2) 0.007(2) C4 0.028(3) 0.047(3) 0.037(3) 0.006(2) 0.007(2) 0.011(2) C5 0.023(2) 0.043(3) 0.037(2) -0.004(3) 0.0069(17) 0.008(3) C6 0.040(3) 0.059(4) 0.036(3) 0.002(3) 0.020(2) 0.006(3) C7 0.029(3) 0.074(5) 0.048(4) -0.025(3) 0.001(2) 0.006(3) C8 0.042(4) 0.041(4) 0.068(5) 0.002(3) 0.024(3) 0.006(3) C9 0.052(4) 0.064(4) 0.042(3) 0.017(3) 0.002(3) 0.027(3) C10 0.025(3) 0.058(4) 0.050(3) -0.017(3) 0.001(2) 0.002(2) C11 0.092(7) 0.057(5) 0.100(7) 0.044(5) 0.074(6) 0.041(4) C12 0.057(4) 0.078(6) 0.060(4) 0.037(4) 0.039(4) 0.031(4) C13 0.043(3) 0.069(4) 0.042(3) -0.013(3) 0.021(3) -0.005(3) C14 0.026(3) 0.051(3) 0.029(3) 0.007(2) 0.009(2) 0.007(2) C15 0.027(2) 0.037(3) 0.035(3) -0.002(2) 0.010(2) -0.001(2) C16 0.034(3) 0.031(3) 0.031(3) 0.003(2) 0.008(2) 0.006(2) C17 0.032(3) 0.039(3) 0.047(3) 0.000(2) 0.004(2) 0.006(2) C18 0.031(3) 0.035(3) 0.033(3) 0.001(2) 0.007(2) 0.002(2) C19 0.041(3) 0.039(3) 0.048(3) 0.007(3) 0.017(3) 0.004(2) C20 0.040(3) 0.048(3) 0.082(5) 0.011(4) 0.027(4) 0.001(3) C21 0.028(3) 0.064(5) 0.086(5) 0.002(4) 0.002(3) -0.010(3) C22 0.040(4) 0.068(5) 0.060(4) -0.015(4) -0.005(3) -0.007(3) C23 0.035(3) 0.059(4) 0.042(3) -0.006(3) 0.008(2) -0.005(3) Sb1 0.0416(2) 0.0626(3) 0.0419(2) 0.01640(19) 0.01781(17) 0.01114(19) F1 0.058(3) 0.085(4) 0.119(4) 0.031(3) 0.047(3) 0.029(3) F2 0.053(3) 0.072(3) 0.101(4) -0.020(3) 0.032(3) 0.008(2) Sb2 0.02422(17) 0.0515(2) 0.0407(2) 0.00725(17) 0.00083(14) 0.00208(15) F11 0.056(3) 0.094(4) 0.074(3) -0.031(3) 0.029(2) -0.030(3) F12 0.075(4) 0.160(6) 0.076(4) -0.033(4) 0.015(3) -0.074(4) O2 0.052(6) 0.068(7) 0.049(6) -0.006(5) -0.002(4) -0.010(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 N1 2.071(4) . ? Ir1 C5 2.136(5) . ? Ir1 C4 2.144(5) . ? Ir1 N2 2.144(5) . ? Ir1 C3 2.166(6) . ? Ir1 C1 2.168(4) . ? Ir1 O1 2.178(4) . ? Ir1 C2 2.184(5) . ? N1 C14 1.309(10) . ? N1 C11 1.362(9) . ? N2 C15 1.290(7) . ? N2 C16 1.486(7) . ? N3 C12 1.336(10) . ? N3 C14 1.345(7) . ? N3 C13 1.466(9) . ? O1 H1A 0.9820 . ? O1 H1B 0.9818 . ? C1 C2 1.436(9) . ? C1 C5 1.448(7) . ? C1 C6 1.498(9) . ? C2 C3 1.456(8) . ? C2 C7 1.492(8) . ? C3 C4 1.449(9) . ? C3 C8 1.475(10) . ? C4 C5 1.413(10) . ? C4 C9 1.513(8) . ? C5 C10 1.496(9) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.360(11) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.421(8) . ? C15 H15 0.9500 . ? C16 C17 1.527(8) . ? C16 C18 1.533(8) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.385(9) . ? C18 C19 1.407(8) . ? C19 C20 1.393(10) . ? C19 H19 0.9500 . ? C20 C21 1.346(12) . ? C20 H20 0.9500 . ? C21 C22 1.358(12) . ? C21 H21 0.9500 . ? C22 C23 1.390(9) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? Sb1 F6A 1.823(7) . ? Sb1 F4B 1.848(8) . ? Sb1 F5B 1.859(9) . ? Sb1 F4A 1.859(7) . ? Sb1 F2 1.865(4) . ? Sb1 F1 1.868(4) . ? Sb1 F3A 1.879(6) . ? Sb1 F6B 1.882(9) . ? Sb1 F3B 1.891(9) . ? Sb1 F5A 1.911(7) . ? F3A F3B 1.51(2) . ? F3A F5B 1.66(2) . ? F4A F4B 0.821(16) . ? F5A F5B 1.08(2) . ? F6A F6B 1.124(18) . ? F6A F3B 1.66(2) . ? Sb2 F8A 1.828(7) . ? Sb2 F12 1.840(5) . ? Sb2 F10B 1.846(8) . ? Sb2 F7B 1.846(7) . ? Sb2 F11 1.857(4) . ? Sb2 F9A 1.863(7) . ? Sb2 F10A 1.899(7) . ? Sb2 F9B 1.900(8) . ? Sb2 F8B 1.907(8) . ? Sb2 F7A 1.907(7) . ? F7A F7B 0.775(10) . ? F8A F8B 0.672(13) . ? F9A F9B 1.036(13) . ? F10A F10B 0.687(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ir1 C5 123.7(2) . . ? N1 Ir1 C4 100.1(2) . . ? C5 Ir1 C4 38.6(3) . . ? N1 Ir1 N2 75.6(2) . . ? C5 Ir1 N2 105.1(2) . . ? C4 Ir1 N2 133.1(2) . . ? N1 Ir1 C3 109.3(2) . . ? C5 Ir1 C3 65.6(2) . . ? C4 Ir1 C3 39.3(2) . . ? N2 Ir1 C3 170.68(19) . . ? N1 Ir1 C1 162.95(19) . . ? C5 Ir1 C1 39.30(18) . . ? C4 Ir1 C1 65.3(2) . . ? N2 Ir1 C1 107.2(2) . . ? C3 Ir1 C1 65.7(2) . . ? N1 Ir1 O1 80.5(2) . . ? C5 Ir1 O1 155.8(2) . . ? C4 Ir1 O1 146.8(2) . . ? N2 Ir1 O1 79.64(18) . . ? C3 Ir1 O1 108.7(2) . . ? C1 Ir1 O1 116.52(18) . . ? N1 Ir1 C2 145.0(3) . . ? C5 Ir1 C2 64.9(2) . . ? C4 Ir1 C2 65.0(2) . . ? N2 Ir1 C2 138.2(2) . . ? C3 Ir1 C2 39.1(2) . . ? C1 Ir1 C2 38.5(2) . . ? O1 Ir1 C2 95.5(2) . . ? C14 N1 C11 106.4(5) . . ? C14 N1 Ir1 116.0(5) . . ? C11 N1 Ir1 137.4(6) . . ? C15 N2 C16 119.9(5) . . ? C15 N2 Ir1 115.1(4) . . ? C16 N2 Ir1 124.5(3) . . ? C12 N3 C14 107.0(6) . . ? C12 N3 C13 126.8(6) . . ? C14 N3 C13 126.0(6) . . ? Ir1 O1 H1A 109.3 . . ? Ir1 O1 H1B 109.3 . . ? H1A O1 H1B 109.2 . . ? C2 C1 C5 107.0(6) . . ? C2 C1 C6 124.6(5) . . ? C5 C1 C6 128.0(6) . . ? C2 C1 Ir1 71.3(3) . . ? C5 C1 Ir1 69.1(3) . . ? C6 C1 Ir1 130.2(4) . . ? C1 C2 C3 108.8(5) . . ? C1 C2 C7 126.8(6) . . ? C3 C2 C7 124.3(6) . . ? C1 C2 Ir1 70.1(3) . . ? C3 C2 Ir1 69.8(3) . . ? C7 C2 Ir1 124.8(4) . . ? C4 C3 C2 106.3(5) . . ? C4 C3 C8 126.1(6) . . ? C2 C3 C8 127.3(6) . . ? C4 C3 Ir1 69.6(3) . . ? C2 C3 Ir1 71.1(3) . . ? C8 C3 Ir1 128.5(4) . . ? C5 C4 C3 109.0(5) . . ? C5 C4 C9 126.5(6) . . ? C3 C4 C9 124.4(6) . . ? C5 C4 Ir1 70.4(3) . . ? C3 C4 Ir1 71.2(3) . . ? C9 C4 Ir1 127.5(4) . . ? C4 C5 C1 108.9(6) . . ? C4 C5 C10 125.4(5) . . ? C1 C5 C10 125.5(6) . . ? C4 C5 Ir1 71.0(3) . . ? C1 C5 Ir1 71.6(3) . . ? C10 C5 Ir1 127.4(4) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 N1 108.1(7) . . ? C12 C11 H11 125.9 . . ? N1 C11 H11 125.9 . . ? N3 C12 C11 107.5(6) . . ? N3 C12 H12 126.2 . . ? C11 C12 H12 126.2 . . ? N3 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 N3 110.9(6) . . ? N1 C14 C15 117.4(5) . . ? N3 C14 C15 131.6(6) . . ? N2 C15 C14 115.8(5) . . ? N2 C15 H15 122.1 . . ? C14 C15 H15 122.1 . . ? N2 C16 C17 113.4(5) . . ? N2 C16 C18 109.7(4) . . ? C17 C16 C18 110.9(5) . . ? N2 C16 H16 107.5 . . ? C17 C16 H16 107.5 . . ? C18 C16 H16 107.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 119.2(6) . . ? C23 C18 C16 122.9(5) . . ? C19 C18 C16 117.9(5) . . ? C20 C19 C18 119.3(7) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C21 C20 C19 121.0(7) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C20 C21 C22 119.8(7) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C21 C22 C23 122.0(7) . . ? C21 C22 H22 119.0 . . ? C23 C22 H22 119.0 . . ? C18 C23 C22 118.7(7) . . ? C18 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? F6A Sb1 F4B 117.1(6) . . ? F6A Sb1 F5B 147.7(8) . . ? F4B Sb1 F5B 94.9(9) . . ? F6A Sb1 F4A 92.2(5) . . ? F4B Sb1 F4A 25.6(5) . . ? F5B Sb1 F4A 120.1(8) . . ? F6A Sb1 F2 95.1(4) . . ? F4B Sb1 F2 94.0(5) . . ? F5B Sb1 F2 87.2(7) . . ? F4A Sb1 F2 90.7(4) . . ? F6A Sb1 F1 84.2(4) . . ? F4B Sb1 F1 87.0(5) . . ? F5B Sb1 F1 93.0(7) . . ? F4A Sb1 F1 90.0(4) . . ? F2 Sb1 F1 179.0(3) . . ? F6A Sb1 F3A 94.9(4) . . ? F4B Sb1 F3A 146.0(6) . . ? F5B Sb1 F3A 52.8(8) . . ? F4A Sb1 F3A 170.9(5) . . ? F2 Sb1 F3A 94.4(3) . . ? F1 Sb1 F3A 85.0(3) . . ? F6A Sb1 F6B 35.3(6) . . ? F4B Sb1 F6B 83.9(8) . . ? F5B Sb1 F6B 172.9(9) . . ? F4A Sb1 F6B 58.3(7) . . ? F2 Sb1 F6B 85.9(6) . . ? F1 Sb1 F6B 93.9(6) . . ? F3A Sb1 F6B 129.6(6) . . ? F6A Sb1 F3B 53.1(8) . . ? F4B Sb1 F3B 165.9(9) . . ? F5B Sb1 F3B 96.3(10) . . ? F4A Sb1 F3B 141.5(9) . . ? F2 Sb1 F3B 78.0(7) . . ? F1 Sb1 F3B 100.9(8) . . ? F3A Sb1 F3B 47.4(8) . . ? F6B Sb1 F3B 84.0(9) . . ? F6A Sb1 F5A 174.9(5) . . ? F4B Sb1 F5A 61.7(6) . . ? F5B Sb1 F5A 33.2(7) . . ? F4A Sb1 F5A 87.0(5) . . ? F2 Sb1 F5A 89.9(3) . . ? F1 Sb1 F5A 90.8(4) . . ? F3A Sb1 F5A 85.5(4) . . ? F6B Sb1 F5A 144.9(7) . . ? F3B Sb1 F5A 129.1(8) . . ? F3B F3A F5B 123.1(9) . . ? F3B F3A Sb1 66.7(5) . . ? F5B F3A Sb1 63.0(5) . . ? F4B F4A Sb1 76.4(8) . . ? F5B F5A Sb1 70.7(6) . . ? F6B F6A F3B 128.9(12) . . ? F6B F6A Sb1 75.3(6) . . ? F3B F6A Sb1 65.6(6) . . ? F3A F3B F6A 118.2(10) . . ? F3A F3B Sb1 65.9(5) . . ? F6A F3B Sb1 61.3(5) . . ? F4A F4B Sb1 78.0(8) . . ? F5A F5B F3A 138.7(10) . . ? F5A F5B Sb1 76.1(7) . . ? F3A F5B Sb1 64.2(5) . . ? F6A F6B Sb1 69.5(6) . . ? F8A Sb2 F12 87.9(4) . . ? F8A Sb2 F10B 108.7(5) . . ? F12 Sb2 F10B 83.3(5) . . ? F8A Sb2 F7B 156.3(5) . . ? F12 Sb2 F7B 90.4(3) . . ? F10B Sb2 F7B 94.5(5) . . ? F8A Sb2 F11 93.4(3) . . ? F12 Sb2 F11 178.5(3) . . ? F10B Sb2 F11 95.7(4) . . ? F7B Sb2 F11 88.6(3) . . ? F8A Sb2 F9A 91.9(5) . . ? F12 Sb2 F9A 81.9(4) . . ? F10B Sb2 F9A 154.1(5) . . ? F7B Sb2 F9A 64.5(4) . . ? F11 Sb2 F9A 98.6(4) . . ? F8A Sb2 F10A 92.3(5) . . ? F12 Sb2 F10A 95.8(4) . . ? F10B Sb2 F10A 21.1(4) . . ? F7B Sb2 F10A 111.4(4) . . ? F11 Sb2 F10A 83.6(3) . . ? F9A Sb2 F10A 175.1(4) . . ? F8A Sb2 F9B 67.1(5) . . ? F12 Sb2 F9B 100.7(4) . . ? F10B Sb2 F9B 173.9(5) . . ? F7B Sb2 F9B 90.0(5) . . ? F11 Sb2 F9B 80.4(4) . . ? F9A Sb2 F9B 32.0(4) . . ? F10A Sb2 F9B 152.8(5) . . ? F8A Sb2 F8B 20.6(4) . . ? F12 Sb2 F8B 91.0(4) . . ? F10B Sb2 F8B 88.9(6) . . ? F7B Sb2 F8B 176.4(5) . . ? F11 Sb2 F8B 90.0(4) . . ? F9A Sb2 F8B 112.4(5) . . ? F10A Sb2 F8B 71.8(5) . . ? F9B Sb2 F8B 86.4(5) . . ? F8A Sb2 F7A 179.9(5) . . ? F12 Sb2 F7A 92.2(3) . . ? F10B Sb2 F7A 71.2(5) . . ? F7B Sb2 F7A 23.8(3) . . ? F11 Sb2 F7A 86.5(3) . . ? F9A Sb2 F7A 88.2(4) . . ? F10A Sb2 F7A 87.6(4) . . ? F9B Sb2 F7A 112.9(4) . . ? F8B Sb2 F7A 159.4(5) . . ? F7B F7A Sb2 73.7(7) . . ? F8B F8A Sb2 86.3(10) . . ? F9B F9A Sb2 76.0(6) . . ? F10B F10A Sb2 75.1(9) . . ? F7A F7B Sb2 82.5(8) . . ? F8A F8B Sb2 73.1(9) . . ? F9A F9B Sb2 72.0(6) . . ? F10A F10B Sb2 83.8(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 Ir1 N1 C14 100.0(5) . . . . ? C4 Ir1 N1 C14 133.3(5) . . . . ? N2 Ir1 N1 C14 1.2(5) . . . . ? C3 Ir1 N1 C14 172.9(5) . . . . ? C1 Ir1 N1 C14 103.2(10) . . . . ? O1 Ir1 N1 C14 -80.4(5) . . . . ? C2 Ir1 N1 C14 -166.3(4) . . . . ? C5 Ir1 N1 C11 -85.4(10) . . . . ? C4 Ir1 N1 C11 -52.1(10) . . . . ? N2 Ir1 N1 C11 175.8(10) . . . . ? C3 Ir1 N1 C11 -12.5(10) . . . . ? C1 Ir1 N1 C11 -82.2(16) . . . . ? O1 Ir1 N1 C11 94.2(10) . . . . ? C2 Ir1 N1 C11 8.3(11) . . . . ? N1 Ir1 N2 C15 -3.0(4) . . . . ? C5 Ir1 N2 C15 -124.6(4) . . . . ? C4 Ir1 N2 C15 -93.5(4) . . . . ? C1 Ir1 N2 C15 -165.5(4) . . . . ? O1 Ir1 N2 C15 79.8(4) . . . . ? C2 Ir1 N2 C15 166.4(4) . . . . ? N1 Ir1 N2 C16 -174.8(4) . . . . ? C5 Ir1 N2 C16 63.6(4) . . . . ? C4 Ir1 N2 C16 94.7(4) . . . . ? C1 Ir1 N2 C16 22.6(4) . . . . ? O1 Ir1 N2 C16 -92.1(4) . . . . ? C2 Ir1 N2 C16 -5.5(5) . . . . ? N1 Ir1 C1 C2 113.2(10) . . . . ? C5 Ir1 C1 C2 117.3(6) . . . . ? C4 Ir1 C1 C2 80.2(4) . . . . ? N2 Ir1 C1 C2 -149.7(3) . . . . ? C3 Ir1 C1 C2 36.9(3) . . . . ? O1 Ir1 C1 C2 -62.9(4) . . . . ? N1 Ir1 C1 C5 -4.2(12) . . . . ? C4 Ir1 C1 C5 -37.1(4) . . . . ? N2 Ir1 C1 C5 93.0(4) . . . . ? C3 Ir1 C1 C5 -80.5(4) . . . . ? O1 Ir1 C1 C5 179.8(4) . . . . ? C2 Ir1 C1 C5 -117.3(6) . . . . ? N1 Ir1 C1 C6 -126.9(9) . . . . ? C5 Ir1 C1 C6 -122.7(8) . . . . ? C4 Ir1 C1 C6 -159.8(6) . . . . ? N2 Ir1 C1 C6 -29.7(6) . . . . ? C3 Ir1 C1 C6 156.8(6) . . . . ? O1 Ir1 C1 C6 57.1(6) . . . . ? C2 Ir1 C1 C6 120.0(6) . . . . ? C5 C1 C2 C3 1.0(6) . . . . ? C6 C1 C2 C3 174.3(5) . . . . ? Ir1 C1 C2 C3 -59.2(4) . . . . ? C5 C1 C2 C7 179.4(5) . . . . ? C6 C1 C2 C7 -7.4(8) . . . . ? Ir1 C1 C2 C7 119.1(5) . . . . ? C5 C1 C2 Ir1 60.2(3) . . . . ? C6 C1 C2 Ir1 -126.5(5) . . . . ? N1 Ir1 C2 C1 -151.9(3) . . . . ? C5 Ir1 C2 C1 -38.4(3) . . . . ? C4 Ir1 C2 C1 -81.2(3) . . . . ? N2 Ir1 C2 C1 46.3(4) . . . . ? C3 Ir1 C2 C1 -119.9(4) . . . . ? O1 Ir1 C2 C1 126.9(3) . . . . ? N1 Ir1 C2 C3 -32.0(5) . . . . ? C5 Ir1 C2 C3 81.5(4) . . . . ? C4 Ir1 C2 C3 38.7(3) . . . . ? N2 Ir1 C2 C3 166.2(3) . . . . ? C1 Ir1 C2 C3 119.9(4) . . . . ? O1 Ir1 C2 C3 -113.2(3) . . . . ? N1 Ir1 C2 C7 86.4(7) . . . . ? C5 Ir1 C2 C7 -160.1(7) . . . . ? C4 Ir1 C2 C7 157.2(6) . . . . ? N2 Ir1 C2 C7 -75.4(6) . . . . ? C3 Ir1 C2 C7 118.4(7) . . . . ? C1 Ir1 C2 C7 -121.7(7) . . . . ? O1 Ir1 C2 C7 5.2(6) . . . . ? C1 C2 C3 C4 -1.5(6) . . . . ? C7 C2 C3 C4 -180.0(5) . . . . ? Ir1 C2 C3 C4 -61.0(4) . . . . ? C1 C2 C3 C8 -176.0(5) . . . . ? C7 C2 C3 C8 5.6(9) . . . . ? Ir1 C2 C3 C8 124.6(6) . . . . ? C1 C2 C3 Ir1 59.5(4) . . . . ? C7 C2 C3 Ir1 -119.0(5) . . . . ? N1 Ir1 C3 C4 -82.4(4) . . . . ? C5 Ir1 C3 C4 36.8(3) . . . . ? C1 Ir1 C3 C4 80.1(3) . . . . ? O1 Ir1 C3 C4 -168.6(3) . . . . ? C2 Ir1 C3 C4 116.4(5) . . . . ? N1 Ir1 C3 C2 161.2(3) . . . . ? C5 Ir1 C3 C2 -79.7(3) . . . . ? C4 Ir1 C3 C2 -116.4(5) . . . . ? C1 Ir1 C3 C2 -36.3(3) . . . . ? O1 Ir1 C3 C2 75.0(3) . . . . ? N1 Ir1 C3 C8 38.2(7) . . . . ? C5 Ir1 C3 C8 157.3(7) . . . . ? C4 Ir1 C3 C8 120.5(7) . . . . ? C1 Ir1 C3 C8 -159.4(7) . . . . ? O1 Ir1 C3 C8 -48.0(7) . . . . ? C2 Ir1 C3 C8 -123.1(7) . . . . ? C2 C3 C4 C5 1.5(6) . . . . ? C8 C3 C4 C5 176.0(5) . . . . ? Ir1 C3 C4 C5 -60.5(4) . . . . ? C2 C3 C4 C9 -174.8(5) . . . . ? C8 C3 C4 C9 -0.3(9) . . . . ? Ir1 C3 C4 C9 123.1(6) . . . . ? C2 C3 C4 Ir1 62.0(4) . . . . ? C8 C3 C4 Ir1 -123.5(6) . . . . ? N1 Ir1 C4 C5 -132.8(4) . . . . ? N2 Ir1 C4 C5 -53.1(4) . . . . ? C3 Ir1 C4 C5 119.1(5) . . . . ? C1 Ir1 C4 C5 37.8(3) . . . . ? O1 Ir1 C4 C5 139.1(4) . . . . ? C2 Ir1 C4 C5 80.5(4) . . . . ? N1 Ir1 C4 C3 108.1(4) . . . . ? C5 Ir1 C4 C3 -119.1(5) . . . . ? N2 Ir1 C4 C3 -172.2(3) . . . . ? C1 Ir1 C4 C3 -81.2(4) . . . . ? O1 Ir1 C4 C3 20.0(6) . . . . ? C2 Ir1 C4 C3 -38.6(3) . . . . ? N1 Ir1 C4 C9 -11.3(7) . . . . ? C5 Ir1 C4 C9 121.5(8) . . . . ? N2 Ir1 C4 C9 68.4(7) . . . . ? C3 Ir1 C4 C9 -119.4(8) . . . . ? C1 Ir1 C4 C9 159.3(7) . . . . ? O1 Ir1 C4 C9 -99.4(7) . . . . ? C2 Ir1 C4 C9 -158.0(7) . . . . ? C3 C4 C5 C1 -0.9(6) . . . . ? C9 C4 C5 C1 175.3(5) . . . . ? Ir1 C4 C5 C1 -61.9(4) . . . . ? C3 C4 C5 C10 -176.1(5) . . . . ? C9 C4 C5 C10 0.1(9) . . . . ? Ir1 C4 C5 C10 122.9(6) . . . . ? C3 C4 C5 Ir1 61.0(4) . . . . ? C9 C4 C5 Ir1 -122.7(6) . . . . ? C2 C1 C5 C4 -0.1(6) . . . . ? C6 C1 C5 C4 -173.0(5) . . . . ? Ir1 C1 C5 C4 61.6(4) . . . . ? C2 C1 C5 C10 175.1(5) . . . . ? C6 C1 C5 C10 2.2(9) . . . . ? Ir1 C1 C5 C10 -123.2(6) . . . . ? C2 C1 C5 Ir1 -61.7(3) . . . . ? C6 C1 C5 Ir1 125.4(6) . . . . ? N1 Ir1 C5 C4 60.2(5) . . . . ? N2 Ir1 C5 C4 142.8(3) . . . . ? C3 Ir1 C5 C4 -37.4(4) . . . . ? C1 Ir1 C5 C4 -118.4(6) . . . . ? O1 Ir1 C5 C4 -118.8(6) . . . . ? C2 Ir1 C5 C4 -80.7(4) . . . . ? N1 Ir1 C5 C1 178.5(4) . . . . ? C4 Ir1 C5 C1 118.4(6) . . . . ? N2 Ir1 C5 C1 -98.9(4) . . . . ? C3 Ir1 C5 C1 80.9(4) . . . . ? O1 Ir1 C5 C1 -0.4(9) . . . . ? C2 Ir1 C5 C1 37.7(4) . . . . ? N1 Ir1 C5 C10 -60.4(7) . . . . ? C4 Ir1 C5 C10 -120.6(7) . . . . ? N2 Ir1 C5 C10 22.2(6) . . . . ? C3 Ir1 C5 C10 -158.0(6) . . . . ? C1 Ir1 C5 C10 121.0(8) . . . . ? O1 Ir1 C5 C10 120.6(6) . . . . ? C2 Ir1 C5 C10 158.7(7) . . . . ? C14 N1 C11 C12 -1.5(11) . . . . ? Ir1 N1 C11 C12 -176.5(6) . . . . ? C14 N3 C12 C11 -1.2(11) . . . . ? C13 N3 C12 C11 -177.5(8) . . . . ? N1 C11 C12 N3 1.7(12) . . . . ? C11 N1 C14 N3 0.8(9) . . . . ? Ir1 N1 C14 N3 177.0(4) . . . . ? C11 N1 C14 C15 -175.7(8) . . . . ? Ir1 N1 C14 C15 0.5(7) . . . . ? C12 N3 C14 N1 0.2(8) . . . . ? C13 N3 C14 N1 176.6(6) . . . . ? C12 N3 C14 C15 176.1(7) . . . . ? C13 N3 C14 C15 -7.5(11) . . . . ? C16 N2 C15 C14 176.4(5) . . . . ? Ir1 N2 C15 C14 4.1(6) . . . . ? N1 C14 C15 N2 -3.2(8) . . . . ? N3 C14 C15 N2 -178.8(6) . . . . ? C15 N2 C16 C17 -32.4(7) . . . . ? Ir1 N2 C16 C17 139.1(4) . . . . ? C15 N2 C16 C18 92.2(6) . . . . ? Ir1 N2 C16 C18 -96.3(5) . . . . ? N2 C16 C18 C23 -40.4(8) . . . . ? C17 C16 C18 C23 85.6(7) . . . . ? N2 C16 C18 C19 142.4(5) . . . . ? C17 C16 C18 C19 -91.5(6) . . . . ? C23 C18 C19 C20 -1.1(9) . . . . ? C16 C18 C19 C20 176.1(6) . . . . ? C18 C19 C20 C21 0.4(10) . . . . ? C19 C20 C21 C22 0.6(12) . . . . ? C20 C21 C22 C23 -1.0(13) . . . . ? C19 C18 C23 C22 0.7(10) . . . . ? C16 C18 C23 C22 -176.3(6) . . . . ? C21 C22 C23 C18 0.3(12) . . . . ? F6A Sb1 F3A F3B 26.2(10) . . . . ? F4B Sb1 F3A F3B -173.1(13) . . . . ? F5B Sb1 F3A F3B -152.4(14) . . . . ? F2 Sb1 F3A F3B -69.3(10) . . . . ? F1 Sb1 F3A F3B 109.9(10) . . . . ? F6B Sb1 F3A F3B 19.0(13) . . . . ? F5A Sb1 F3A F3B -158.9(10) . . . . ? F6A Sb1 F3A F5B 178.6(10) . . . . ? F4B Sb1 F3A F5B -20.7(13) . . . . ? F2 Sb1 F3A F5B 83.1(9) . . . . ? F1 Sb1 F3A F5B -97.7(9) . . . . ? F6B Sb1 F3A F5B 171.4(12) . . . . ? F3B Sb1 F3A F5B 152.4(14) . . . . ? F5A Sb1 F3A F5B -6.5(10) . . . . ? F6A Sb1 F4A F4B 167.1(15) . . . . ? F5B Sb1 F4A F4B -10.6(18) . . . . ? F2 Sb1 F4A F4B -97.8(15) . . . . ? F1 Sb1 F4A F4B 82.9(15) . . . . ? F6B Sb1 F4A F4B 177.5(18) . . . . ? F3B Sb1 F4A F4B -169.3(17) . . . . ? F5A Sb1 F4A F4B -7.9(15) . . . . ? F4B Sb1 F5A F5B -179.5(16) . . . . ? F4A Sb1 F5A F5B -175.7(15) . . . . ? F2 Sb1 F5A F5B -84.9(14) . . . . ? F1 Sb1 F5A F5B 94.3(14) . . . . ? F3A Sb1 F5A F5B 9.4(14) . . . . ? F6B Sb1 F5A F5B -167.7(17) . . . . ? F3B Sb1 F5A F5B -10.5(17) . . . . ? F4B Sb1 F6A F6B 21.6(13) . . . . ? F5B Sb1 F6A F6B -168.3(17) . . . . ? F4A Sb1 F6A F6B 15.4(12) . . . . ? F2 Sb1 F6A F6B -75.5(12) . . . . ? F1 Sb1 F6A F6B 105.2(12) . . . . ? F3A Sb1 F6A F6B -170.4(12) . . . . ? F3B Sb1 F6A F6B -146.4(15) . . . . ? F4B Sb1 F6A F3B 168.1(11) . . . . ? F5B Sb1 F6A F3B -21.8(17) . . . . ? F4A Sb1 F6A F3B 161.8(10) . . . . ? F2 Sb1 F6A F3B 70.9(9) . . . . ? F1 Sb1 F6A F3B -108.3(9) . . . . ? F3A Sb1 F6A F3B -23.9(10) . . . . ? F6B Sb1 F6A F3B 146.4(15) . . . . ? F5B F3A F3B F6A -63(2) . . . . ? Sb1 F3A F3B F6A -33.2(10) . . . . ? F5B F3A F3B Sb1 -29.5(13) . . . . ? F6B F6A F3B F3A 78(2) . . . . ? Sb1 F6A F3B F3A 34.7(11) . . . . ? F6B F6A F3B Sb1 43.4(16) . . . . ? F6A Sb1 F3B F3A -146.7(13) . . . . ? F4B Sb1 F3B F3A 164(3) . . . . ? F5B Sb1 F3B F3A 21.8(11) . . . . ? F4A Sb1 F3B F3A -176.7(7) . . . . ? F2 Sb1 F3B F3A 107.5(8) . . . . ? F1 Sb1 F3B F3A -72.6(8) . . . . ? F6B Sb1 F3B F3A -165.4(10) . . . . ? F5A Sb1 F3B F3A 27.6(13) . . . . ? F4B Sb1 F3B F6A -49(4) . . . . ? F5B Sb1 F3B F6A 168.5(9) . . . . ? F4A Sb1 F3B F6A -30.0(16) . . . . ? F2 Sb1 F3B F6A -105.8(7) . . . . ? F1 Sb1 F3B F6A 74.1(7) . . . . ? F3A Sb1 F3B F6A 146.7(13) . . . . ? F6B Sb1 F3B F6A -18.7(8) . . . . ? F5A Sb1 F3B F6A 174.2(6) . . . . ? F6A Sb1 F4B F4A -14.5(17) . . . . ? F5B Sb1 F4B F4A 170.8(16) . . . . ? F2 Sb1 F4B F4A 83.3(14) . . . . ? F1 Sb1 F4B F4A -96.4(15) . . . . ? F3A Sb1 F4B F4A -172.8(10) . . . . ? F6B Sb1 F4B F4A -2.2(15) . . . . ? F3B Sb1 F4B F4A 28(4) . . . . ? F5A Sb1 F4B F4A 171.0(17) . . . . ? Sb1 F5A F5B F3A -16(2) . . . . ? F3B F3A F5B F5A 48(4) . . . . ? Sb1 F3A F5B F5A 18(2) . . . . ? F3B F3A F5B Sb1 30.5(14) . . . . ? F6A Sb1 F5B F5A -170.8(8) . . . . ? F4B Sb1 F5B F5A 0.4(14) . . . . ? F4A Sb1 F5B F5A 5.0(17) . . . . ? F2 Sb1 F5B F5A 94.2(13) . . . . ? F1 Sb1 F5B F5A -86.8(13) . . . . ? F3A Sb1 F5B F5A -168.1(18) . . . . ? F3B Sb1 F5B F5A 171.8(14) . . . . ? F6A Sb1 F5B F3A -2.6(18) . . . . ? F4B Sb1 F5B F3A 168.5(7) . . . . ? F4A Sb1 F5B F3A 173.1(5) . . . . ? F2 Sb1 F5B F3A -97.7(6) . . . . ? F1 Sb1 F5B F3A 81.3(6) . . . . ? F3B Sb1 F5B F3A -20.0(10) . . . . ? F5A Sb1 F5B F3A 168.1(18) . . . . ? F3B F6A F6B Sb1 -40.3(15) . . . . ? F4B Sb1 F6B F6A -160.7(12) . . . . ? F4A Sb1 F6B F6A -161.8(14) . . . . ? F2 Sb1 F6B F6A 104.8(11) . . . . ? F1 Sb1 F6B F6A -74.2(11) . . . . ? F3A Sb1 F6B F6A 12.5(15) . . . . ? F3B Sb1 F6B F6A 26.4(12) . . . . ? F5A Sb1 F6B F6A -171.2(8) . . . . ? F12 Sb2 F7A F7B 86.1(10) . . . . ? F10B Sb2 F7A F7B 168.3(11) . . . . ? F11 Sb2 F7A F7B -94.5(10) . . . . ? F9A Sb2 F7A F7B 4.2(10) . . . . ? F10A Sb2 F7A F7B -178.2(10) . . . . ? F9B Sb2 F7A F7B -16.5(11) . . . . ? F8B Sb2 F7A F7B -175.2(12) . . . . ? F12 Sb2 F8A F8B 98.4(15) . . . . ? F10B Sb2 F8A F8B 16.2(16) . . . . ? F7B Sb2 F8A F8B -175.3(13) . . . . ? F11 Sb2 F8A F8B -81.0(15) . . . . ? F9A Sb2 F8A F8B -179.7(15) . . . . ? F10A Sb2 F8A F8B 2.7(15) . . . . ? F9B Sb2 F8A F8B -159.0(16) . . . . ? F8A Sb2 F9A F9B 37.9(9) . . . . ? F12 Sb2 F9A F9B 125.6(9) . . . . ? F10B Sb2 F9A F9B -178.6(10) . . . . ? F7B Sb2 F9A F9B -140.1(10) . . . . ? F11 Sb2 F9A F9B -55.8(9) . . . . ? F8B Sb2 F9A F9B 37.8(10) . . . . ? F7A Sb2 F9A F9B -142.0(9) . . . . ? F8A Sb2 F10A F10B 142.1(14) . . . . ? F12 Sb2 F10A F10B 54.0(14) . . . . ? F7B Sb2 F10A F10B -38.7(15) . . . . ? F11 Sb2 F10A F10B -124.7(14) . . . . ? F9B Sb2 F10A F10B -178.7(13) . . . . ? F8B Sb2 F10A F10B 143.1(15) . . . . ? F7A Sb2 F10A F10B -38.0(14) . . . . ? F8A Sb2 F7B F7A 179.7(10) . . . . ? F12 Sb2 F7B F7A -94.5(10) . . . . ? F10B Sb2 F7B F7A -11.1(10) . . . . ? F11 Sb2 F7B F7A 84.5(10) . . . . ? F9A Sb2 F7B F7A -175.3(11) . . . . ? F10A Sb2 F7B F7A 1.9(11) . . . . ? F9B Sb2 F7B F7A 164.8(10) . . . . ? F12 Sb2 F8B F8A -81.4(15) . . . . ? F10B Sb2 F8B F8A -164.7(15) . . . . ? F11 Sb2 F8B F8A 99.6(15) . . . . ? F9A Sb2 F8B F8A 0.3(16) . . . . ? F10A Sb2 F8B F8A -177.1(16) . . . . ? F9B Sb2 F8B F8A 19.3(15) . . . . ? F7A Sb2 F8B F8A 179.7(11) . . . . ? F8A Sb2 F9B F9A -138.1(10) . . . . ? F12 Sb2 F9B F9A -55.0(9) . . . . ? F7B Sb2 F9B F9A 35.4(9) . . . . ? F11 Sb2 F9B F9A 124.0(9) . . . . ? F10A Sb2 F9B F9A 178.6(8) . . . . ? F8B Sb2 F9B F9A -145.4(9) . . . . ? F7A Sb2 F9B F9A 42.0(10) . . . . ? F8A Sb2 F10B F10A -40.4(15) . . . . ? F12 Sb2 F10B F10A -125.9(14) . . . . ? F7B Sb2 F10B F10A 144.2(14) . . . . ? F11 Sb2 F10B F10A 55.2(14) . . . . ? F9A Sb2 F10B F10A 178.6(11) . . . . ? F8B Sb2 F10B F10A -34.7(14) . . . . ? F7A Sb2 F10B F10A 139.5(15) . . . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.224 _refine_diff_density_min -0.672 _refine_diff_density_rms 0.119 _database_code_depnum_ccdc_archive 'CCDC 937406'