#------------------------------------------------------------------------------ #$Date: 2018-01-23 05:16:25 +0200 (Tue, 23 Jan 2018) $ #$Revision: 205481 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/53/7045340.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7045340 loop_ _publ_author_name 'Congrave, Daniel G.' 'Hsu, Yu-Ting' 'Batsanov, Andrei S.' 'Beeby, Andrew' 'Bryce, Martin R.' _publ_section_title ; Sky-blue emitting bridged diiridium complexes: beneficial effects of intramolecular \p--\p stacking ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/C7DT04201A _journal_year 2018 _chemical_formula_moiety 'C60 H38 F8 Ir2 N6 O4' _chemical_formula_sum 'C60 H38 F8 Ir2 N6 O4' _chemical_formula_weight 1443.36 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_date 2017-06-11 _audit_creation_method ; Olex2 1.2-beta (compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337) ; _audit_update_record ; 2017-09-22 deposited with the CCDC. 2017-12-14 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 94.6047(15) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 24.6611(12) _cell_length_b 13.3724(6) _cell_length_c 15.0140(7) _cell_measurement_reflns_used 9650 _cell_measurement_temperature 120 _cell_measurement_theta_max 35.24 _cell_measurement_theta_min 2.24 _cell_volume 4935.3(4) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2016)' _computing_data_collection 'APEX3 v.2016.1-0 (Bruker, 2016)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL 2014/7 multi-CPU (Sheldrick, 2015)' _computing_structure_solution 'ShelXS 2013/1 (Sheldrick, 2008)' _diffrn_ambient_temperature 120 _diffrn_detector_area_resol_mean 10.4 _diffrn_detector_type 'Bruker PHOTON 100 CMOS' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.935 _diffrn_measurement_device '3-circle area detector diffractometer' _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'focusing mirrors' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_unetI/netI 0.0233 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.935 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 66493 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.935 _diffrn_reflns_theta_full 32.500 _diffrn_reflns_theta_max 35.637 _diffrn_reflns_theta_min 2.245 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\mS microsource' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 5.477 _exptl_absorpt_correction_T_max 0.6709 _exptl_absorpt_correction_T_min 0.4400 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details 'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0702 before and 0.0515 after correction. The Ratio of minimum to maximum transmission is 0.6558. The \l/2 correction factor is Not present.' _exptl_crystal_colour 'clear yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.943 _exptl_crystal_description block _exptl_crystal_F_000 2792 _exptl_crystal_preparation Luminescent _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.196 _exptl_crystal_size_min 0.136 _refine_diff_density_max 1.098 _refine_diff_density_min -0.656 _refine_diff_density_rms 0.118 _refine_ls_extinction_coef 0.000061(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 365 _refine_ls_number_reflns 10647 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.025 _refine_ls_R_factor_all 0.0276 _refine_ls_R_factor_gt 0.0200 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0150P)^2^+10.4440P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.0424 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9317 _reflns_number_total 10647 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt04201a2.cif _cod_data_source_block alpha-10_17srv056 _cod_depositor_comments ; The following automatic conversions were performed: '_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according to /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas ; _cod_database_code 7045340 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.523 _shelx_estimated_absorpt_t_min 0.379 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(C30A) = Uanis(C30B) 3. Others Fixed Sof: C30A(0.43) H30A(0.43) H30B(0.43) H30C(0.43) C30B(0.57) H30D(0.57) H30E(0.57) H30F(0.57) 4.a Riding coordinates: C30A(H30A,H30B,H30C), C30B(H30D,H30E,H30F) 4.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C23(H23) ; _shelx_res_file ; 17srv056.res created by SHELXL-2014/7 TITL 17srv056 in C2/c CELL 0.71073 24.6611 13.3724 15.014 90 94.6047 90 ZERR 4 0.0012 0.0006 0.0007 0 0.0015 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H F Ir N O UNIT 240 152 32 8 24 16 EADP C30A C30B L.S. 7 PLAN 8 SIZE 0.136 0.196 0.22 TEMP -153.15 BOND fmap 2 acta 65 REM REM REM WGHT 0.015000 10.443995 EXTI 0.000061 FVAR 0.03815 IR 4 0.565898 0.257934 0.390597 11.00000 0.00874 0.00882 = 0.01083 0.00005 0.00008 -0.00034 F1 3 0.596579 0.442604 0.139120 11.00000 0.01988 0.01188 = 0.05383 0.00829 0.00389 0.00147 F2 3 0.698755 0.468724 0.105916 11.00000 0.02778 0.02734 = 0.09719 0.02059 0.01640 -0.01042 F3 3 0.733106 0.126625 0.169587 11.00000 0.01706 0.02993 = 0.05330 0.00064 0.00721 0.01184 F4 3 0.629563 0.102758 0.203617 11.00000 0.01954 0.01127 = 0.03188 0.00167 0.00058 0.00057 O1 6 0.520740 0.264786 0.099067 11.00000 0.01087 0.01520 = 0.01266 0.00023 0.00069 0.00008 O2 6 0.772985 0.298502 0.118566 11.00000 0.01404 0.05142 = 0.06750 0.01309 0.01535 -0.00122 N1 5 0.529260 0.254485 0.253564 11.00000 0.00799 0.01027 = 0.01242 0.00015 0.00086 0.00012 N2 5 0.561456 0.107019 0.410468 11.00000 0.01180 0.01060 = 0.01450 -0.00027 0.00058 -0.00040 N3 5 0.576351 0.409040 0.385043 11.00000 0.01361 0.01104 = 0.01430 0.00012 -0.00040 -0.00091 C1 1 0.548662 0.261477 0.174846 11.00000 0.00873 0.00822 = 0.01308 0.00022 0.00145 0.00060 C2 1 0.584911 0.252976 0.522347 11.00000 0.01134 0.01188 = 0.01309 -0.00080 0.00033 0.00007 C3 1 0.598382 0.332770 0.580811 11.00000 0.02085 0.01269 = 0.01573 -0.00117 0.00003 -0.00082 AFIX 43 H3 2 0.600411 0.398542 0.557394 11.00000 -1.20000 AFIX 0 C4 1 0.608779 0.317685 0.671891 11.00000 0.02709 0.01842 = 0.01407 -0.00340 -0.00057 -0.00294 AFIX 43 H4 2 0.617448 0.373161 0.709923 11.00000 -1.20000 AFIX 0 C5 1 0.606662 0.222001 0.708346 11.00000 0.02946 0.02186 = 0.01272 0.00056 -0.00038 -0.00458 AFIX 43 H5 2 0.613657 0.212306 0.770896 11.00000 -1.20000 AFIX 0 C6 1 0.594269 0.141092 0.652617 11.00000 0.02249 0.01597 = 0.01459 0.00270 -0.00074 -0.00190 AFIX 43 H6 2 0.592847 0.075586 0.676807 11.00000 -1.20000 AFIX 0 C7 1 0.583846 0.156318 0.560454 11.00000 0.01307 0.01199 = 0.01497 0.00021 0.00013 -0.00133 C8 1 0.570967 0.075366 0.496710 11.00000 0.01126 0.01269 = 0.01398 0.00053 0.00068 0.00012 C9 1 0.567222 -0.025863 0.517611 11.00000 0.01762 0.01223 = 0.01687 0.00289 0.00123 0.00052 AFIX 43 H9 2 0.574208 -0.047268 0.577772 11.00000 -1.20000 AFIX 0 C10 1 0.553452 -0.095136 0.451609 11.00000 0.01831 0.01166 = 0.02149 0.00103 0.00359 -0.00025 AFIX 43 H10 2 0.550131 -0.163973 0.465835 11.00000 -1.20000 AFIX 0 C11 1 0.544513 -0.062150 0.363674 11.00000 0.01750 0.01174 = 0.01916 -0.00270 0.00262 -0.00080 AFIX 43 H11 2 0.535286 -0.108220 0.316721 11.00000 -1.20000 AFIX 0 C12 1 0.549281 0.038567 0.345882 11.00000 0.01607 0.01333 = 0.01411 -0.00161 0.00092 -0.00132 AFIX 43 H12 2 0.543767 0.060633 0.285692 11.00000 -1.20000 AFIX 0 C13 1 0.646459 0.262982 0.382635 11.00000 0.01045 0.01359 = 0.01341 -0.00059 -0.00058 -0.00015 C14 1 0.683593 0.183606 0.386118 11.00000 0.01382 0.01637 = 0.02317 -0.00101 -0.00071 0.00257 AFIX 43 H14 2 0.670535 0.117045 0.390060 11.00000 -1.20000 AFIX 0 C15 1 0.738945 0.199931 0.383947 11.00000 0.01373 0.02384 = 0.03049 -0.00035 -0.00067 0.00459 AFIX 43 H15 2 0.763121 0.144527 0.385757 11.00000 -1.20000 AFIX 0 C16 1 0.759561 0.296406 0.379151 11.00000 0.01159 0.02948 = 0.03229 -0.00281 0.00098 -0.00124 AFIX 43 H16 2 0.797554 0.306827 0.377213 11.00000 -1.20000 AFIX 0 C17 1 0.724440 0.376983 0.377224 11.00000 0.01304 0.02055 = 0.02806 -0.00088 0.00119 -0.00525 AFIX 43 H17 2 0.738201 0.443155 0.374307 11.00000 -1.20000 AFIX 0 C18 1 0.668385 0.360744 0.379589 11.00000 0.01266 0.01431 = 0.01604 -0.00047 -0.00021 -0.00139 C19 1 0.628769 0.441314 0.383609 11.00000 0.01473 0.01318 = 0.01313 0.00112 0.00039 -0.00214 C20 1 0.640465 0.543346 0.391017 11.00000 0.02056 0.01441 = 0.02247 0.00082 0.00230 -0.00549 AFIX 43 H20 2 0.676828 0.565925 0.388412 11.00000 -1.20000 AFIX 0 C21 1 0.599669 0.611353 0.402061 11.00000 0.02912 0.01049 = 0.02856 0.00109 0.00605 -0.00133 AFIX 43 H21 2 0.607846 0.680407 0.409595 11.00000 -1.20000 AFIX 0 C22 1 0.546018 0.577496 0.402049 11.00000 0.02391 0.01255 = 0.03163 0.00006 0.00485 0.00290 AFIX 43 H22 2 0.517041 0.623234 0.407894 11.00000 -1.20000 AFIX 0 C23 1 0.536020 0.476199 0.393366 11.00000 0.01438 0.01160 = 0.02382 0.00000 0.00200 0.00161 AFIX 43 H23 2 0.499623 0.452895 0.393232 11.00000 -1.20000 AFIX 0 C24 1 0.608694 0.271661 0.169971 11.00000 0.00957 0.01271 = 0.01303 0.00040 0.00207 -0.00018 C25 1 0.629685 0.362573 0.146133 11.00000 0.01346 0.01280 = 0.02585 0.00358 0.00250 0.00033 C26 1 0.683303 0.376284 0.128806 11.00000 0.01690 0.02143 = 0.03880 0.00801 0.00485 -0.00612 C27 1 0.719848 0.296954 0.134987 11.00000 0.01223 0.03259 = 0.03324 0.00499 0.00566 -0.00307 C28 1 0.699418 0.205713 0.161061 11.00000 0.01342 0.02230 = 0.02908 -0.00025 0.00427 0.00548 C29 1 0.645856 0.193689 0.178255 11.00000 0.01325 0.01324 = 0.02059 -0.00049 0.00177 0.00024 PART 1 C30A 1 0.799284 0.400558 0.118593 10.43000 0.02231 0.05757 = 0.07153 0.02580 0.02192 -0.00200 AFIX 3 H30A 2 0.783264 0.437038 0.066303 10.43000 -1.50000 H30B 2 0.838384 0.391908 0.113603 10.43000 -1.50000 H30C 2 0.793544 0.438458 0.172903 10.43000 -1.50000 AFIX 0 PART 0 PART 2 C30B 1 0.796756 0.375029 0.077302 10.57000 0.02231 0.05757 = 0.07153 0.02580 0.02192 -0.00200 AFIX 3 H30D 2 0.835396 0.360079 0.073482 10.57000 -1.50000 H30E 2 0.778696 0.380679 0.016952 10.57000 -1.50000 H30F 2 0.793076 0.438249 0.109272 10.57000 -1.50000 AFIX 0 HKLF 4 REM 17srv056 in C2/c REM R1 = 0.0200 for 9317 Fo > 4sig(Fo) and 0.0276 for all 10647 data REM 365 parameters refined using 0 restraints END WGHT 0.0148 10.4437 REM Highest difference peak 1.098, deepest hole -0.656, 1-sigma level 0.118 Q1 1 0.8026 0.2408 0.3270 11.00000 0.05 1.10 Q2 1 0.5613 0.2628 0.3326 11.00000 0.05 0.80 Q3 1 0.5495 -0.0840 0.4104 11.00000 0.05 0.78 Q4 1 0.5743 0.2587 0.4588 11.00000 0.05 0.74 Q5 1 0.7079 0.1930 0.3982 11.00000 0.05 0.74 Q6 1 0.5748 0.2316 0.3517 11.00000 0.05 0.73 Q7 1 0.5779 0.1166 0.5254 11.00000 0.05 0.71 Q8 1 0.5992 0.1823 0.6762 11.00000 0.05 0.68 ; _shelx_res_checksum 78937 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ir Ir 0.56590(2) 0.25793(2) 0.39060(2) 0.00950(2) Uani 1 1 d . . . . F1 F 0.59658(5) 0.44260(8) 0.13912(9) 0.0285(3) Uani 1 1 d . . . . F2 F 0.69876(6) 0.46872(10) 0.10592(13) 0.0502(4) Uani 1 1 d . . . . F3 F 0.73311(5) 0.12663(9) 0.16959(10) 0.0332(3) Uani 1 1 d . . . . F4 F 0.62956(4) 0.10276(7) 0.20362(8) 0.0210(2) Uani 1 1 d . . . . O1 O 0.52074(5) 0.26479(8) 0.09907(8) 0.0129(2) Uani 1 1 d . . . . O2 O 0.77299(6) 0.29850(15) 0.11857(14) 0.0437(4) Uani 1 1 d . . . . N1 N 0.52926(5) 0.25448(9) 0.25356(9) 0.0102(2) Uani 1 1 d . . . . N2 N 0.56146(5) 0.10702(10) 0.41047(9) 0.0123(2) Uani 1 1 d . . . . N3 N 0.57635(5) 0.40904(10) 0.38504(9) 0.0131(2) Uani 1 1 d . . . . C1 C 0.54866(6) 0.26148(10) 0.17485(10) 0.0100(2) Uani 1 1 d . . . . C2 C 0.58491(6) 0.25298(11) 0.52235(11) 0.0121(2) Uani 1 1 d . . . . C3 C 0.59838(7) 0.33277(12) 0.58081(11) 0.0165(3) Uani 1 1 d . . . . H3 H 0.6004 0.3985 0.5574 0.020 Uiso 1 1 calc R . . . C4 C 0.60878(8) 0.31769(13) 0.67189(12) 0.0200(3) Uani 1 1 d . . . . H4 H 0.6174 0.3732 0.7099 0.024 Uiso 1 1 calc R . . . C5 C 0.60666(8) 0.22200(14) 0.70835(12) 0.0215(3) Uani 1 1 d . . . . H5 H 0.6137 0.2123 0.7709 0.026 Uiso 1 1 calc R . . . C6 C 0.59427(7) 0.14109(12) 0.65262(11) 0.0178(3) Uani 1 1 d . . . . H6 H 0.5928 0.0756 0.6768 0.021 Uiso 1 1 calc R . . . C7 C 0.58385(6) 0.15632(11) 0.56045(11) 0.0134(3) Uani 1 1 d . . . . C8 C 0.57097(6) 0.07537(11) 0.49671(11) 0.0127(3) Uani 1 1 d . . . . C9 C 0.56722(7) -0.02586(11) 0.51761(11) 0.0156(3) Uani 1 1 d . . . . H9 H 0.5742 -0.0473 0.5778 0.019 Uiso 1 1 calc R . . . C10 C 0.55345(7) -0.09514(12) 0.45161(12) 0.0170(3) Uani 1 1 d . . . . H10 H 0.5501 -0.1640 0.4658 0.020 Uiso 1 1 calc R . . . C11 C 0.54451(7) -0.06215(12) 0.36367(12) 0.0161(3) Uani 1 1 d . . . . H11 H 0.5353 -0.1082 0.3167 0.019 Uiso 1 1 calc R . . . C12 C 0.54928(7) 0.03857(11) 0.34588(11) 0.0145(3) Uani 1 1 d . . . . H12 H 0.5438 0.0606 0.2857 0.017 Uiso 1 1 calc R . . . C13 C 0.64646(6) 0.26298(11) 0.38264(11) 0.0126(3) Uani 1 1 d . . . . C14 C 0.68359(7) 0.18361(13) 0.38612(12) 0.0179(3) Uani 1 1 d . . . . H14 H 0.6705 0.1170 0.3901 0.021 Uiso 1 1 calc R . . . C15 C 0.73895(7) 0.19993(14) 0.38395(14) 0.0228(4) Uani 1 1 d . . . . H15 H 0.7631 0.1445 0.3858 0.027 Uiso 1 1 calc R . . . C16 C 0.75956(7) 0.29641(15) 0.37915(14) 0.0245(4) Uani 1 1 d . . . . H16 H 0.7976 0.3068 0.3772 0.029 Uiso 1 1 calc R . . . C17 C 0.72444(7) 0.37698(13) 0.37722(13) 0.0206(3) Uani 1 1 d . . . . H17 H 0.7382 0.4432 0.3743 0.025 Uiso 1 1 calc R . . . C18 C 0.66839(6) 0.36074(12) 0.37959(11) 0.0144(3) Uani 1 1 d . . . . C19 C 0.62877(6) 0.44131(11) 0.38361(11) 0.0137(3) Uani 1 1 d . . . . C20 C 0.64047(7) 0.54335(12) 0.39102(12) 0.0191(3) Uani 1 1 d . . . . H20 H 0.6768 0.5659 0.3884 0.023 Uiso 1 1 calc R . . . C21 C 0.59967(8) 0.61135(12) 0.40206(13) 0.0225(4) Uani 1 1 d . . . . H21 H 0.6078 0.6804 0.4096 0.027 Uiso 1 1 calc R . . . C22 C 0.54602(8) 0.57750(13) 0.40205(14) 0.0226(4) Uani 1 1 d . . . . H22 H 0.5170 0.6232 0.4079 0.027 Uiso 1 1 calc R . . . C23 C 0.53602(7) 0.47620(12) 0.39337(12) 0.0166(3) Uani 1 1 d . . . . H23 H 0.4996 0.4529 0.3932 0.020 Uiso 1 1 calc R . . . C24 C 0.60869(6) 0.27166(11) 0.16997(10) 0.0117(2) Uani 1 1 d . . . . C25 C 0.62969(7) 0.36257(12) 0.14613(12) 0.0173(3) Uani 1 1 d . . . . C26 C 0.68330(8) 0.37628(14) 0.12881(15) 0.0256(4) Uani 1 1 d . . . . C27 C 0.71985(7) 0.29695(16) 0.13499(15) 0.0258(4) Uani 1 1 d . . . . C28 C 0.69942(7) 0.20571(14) 0.16106(13) 0.0215(3) Uani 1 1 d . . . . C29 C 0.64586(7) 0.19369(12) 0.17826(12) 0.0157(3) Uani 1 1 d . . . . C30A C 0.7993(4) 0.4006(8) 0.1186(6) 0.0495(17) Uani 0.43 1 d . P A 1 H30A H 0.7833 0.4370 0.0663 0.074 Uiso 0.43 1 d R P A 1 H30B H 0.8384 0.3919 0.1136 0.074 Uiso 0.43 1 d R P A 1 H30C H 0.7935 0.4385 0.1729 0.074 Uiso 0.43 1 d R P A 1 C30B C 0.7968(3) 0.3750(5) 0.0773(4) 0.0495(17) Uani 0.57 1 d . P A 2 H30D H 0.8354 0.3601 0.0735 0.074 Uiso 0.57 1 d R P A 2 H30E H 0.7787 0.3807 0.0170 0.074 Uiso 0.57 1 d R P A 2 H30F H 0.7931 0.4382 0.1093 0.074 Uiso 0.57 1 d R P 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 Ir 0.00874(3) 0.00882(3) 0.01083(3) 0.00005(2) 0.00008(2) -0.00034(2) F1 0.0199(5) 0.0119(4) 0.0538(8) 0.0083(5) 0.0039(5) 0.0015(4) F2 0.0278(7) 0.0273(6) 0.0972(13) 0.0206(7) 0.0164(8) -0.0104(5) F3 0.0171(5) 0.0299(6) 0.0533(8) 0.0006(6) 0.0072(5) 0.0118(5) F4 0.0195(5) 0.0113(4) 0.0319(6) 0.0017(4) 0.0006(4) 0.0006(4) O1 0.0109(5) 0.0152(5) 0.0127(5) 0.0002(4) 0.0007(4) 0.0001(4) O2 0.0140(6) 0.0514(10) 0.0675(13) 0.0131(9) 0.0153(7) -0.0012(7) N1 0.0080(5) 0.0103(5) 0.0124(5) 0.0001(4) 0.0009(4) 0.0001(4) N2 0.0118(6) 0.0106(5) 0.0145(6) -0.0003(4) 0.0006(5) -0.0004(4) N3 0.0136(6) 0.0110(5) 0.0143(6) 0.0001(4) -0.0004(5) -0.0009(4) C1 0.0087(5) 0.0082(5) 0.0131(6) 0.0002(5) 0.0015(5) 0.0006(4) C2 0.0113(6) 0.0119(6) 0.0131(6) -0.0008(5) 0.0003(5) 0.0001(5) C3 0.0208(8) 0.0127(6) 0.0157(7) -0.0012(5) 0.0000(6) -0.0008(5) C4 0.0271(9) 0.0184(7) 0.0141(7) -0.0034(6) -0.0006(6) -0.0029(6) C5 0.0295(9) 0.0219(8) 0.0127(7) 0.0006(6) -0.0004(7) -0.0046(7) C6 0.0225(8) 0.0160(7) 0.0146(7) 0.0027(5) -0.0007(6) -0.0019(6) C7 0.0131(6) 0.0120(6) 0.0150(7) 0.0002(5) 0.0001(5) -0.0013(5) C8 0.0113(6) 0.0127(6) 0.0140(7) 0.0005(5) 0.0007(5) 0.0001(5) C9 0.0176(7) 0.0122(6) 0.0169(7) 0.0029(5) 0.0012(6) 0.0005(5) C10 0.0183(7) 0.0117(6) 0.0215(8) 0.0010(5) 0.0036(6) -0.0003(5) C11 0.0175(7) 0.0117(6) 0.0192(8) -0.0027(5) 0.0026(6) -0.0008(5) C12 0.0161(7) 0.0133(6) 0.0141(7) -0.0016(5) 0.0009(6) -0.0013(5) C13 0.0104(6) 0.0136(6) 0.0134(6) -0.0006(5) -0.0006(5) -0.0002(5) C14 0.0138(7) 0.0164(7) 0.0232(8) -0.0010(6) -0.0007(6) 0.0026(5) C15 0.0137(7) 0.0238(8) 0.0305(10) -0.0003(7) -0.0007(7) 0.0046(6) C16 0.0116(7) 0.0295(9) 0.0323(10) -0.0028(8) 0.0010(7) -0.0012(6) C17 0.0130(7) 0.0206(7) 0.0281(9) -0.0009(6) 0.0012(6) -0.0053(6) C18 0.0127(7) 0.0143(6) 0.0160(7) -0.0005(5) -0.0002(5) -0.0014(5) C19 0.0147(7) 0.0132(6) 0.0131(7) 0.0011(5) 0.0004(5) -0.0021(5) C20 0.0206(8) 0.0144(7) 0.0225(8) 0.0008(6) 0.0023(6) -0.0055(6) C21 0.0291(9) 0.0105(6) 0.0286(9) 0.0011(6) 0.0060(7) -0.0013(6) C22 0.0239(8) 0.0125(7) 0.0316(10) 0.0001(6) 0.0049(7) 0.0029(6) C23 0.0144(7) 0.0116(6) 0.0238(8) 0.0000(6) 0.0020(6) 0.0016(5) C24 0.0096(6) 0.0127(6) 0.0130(6) 0.0004(5) 0.0021(5) -0.0002(5) C25 0.0135(7) 0.0128(6) 0.0259(9) 0.0036(6) 0.0025(6) 0.0003(5) C26 0.0169(8) 0.0214(8) 0.0388(11) 0.0080(7) 0.0049(7) -0.0061(6) C27 0.0122(7) 0.0326(10) 0.0332(10) 0.0050(8) 0.0057(7) -0.0031(7) C28 0.0134(7) 0.0223(8) 0.0291(9) -0.0002(7) 0.0043(7) 0.0055(6) C29 0.0133(7) 0.0132(6) 0.0206(8) -0.0005(5) 0.0018(6) 0.0002(5) C30A 0.0223(14) 0.058(4) 0.072(5) 0.026(3) 0.022(3) -0.002(2) C30B 0.0223(14) 0.058(4) 0.072(5) 0.026(3) 0.022(3) -0.002(2) 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1.00 1.00 1.00 0.0390 1.00 -1.00 -1.00 0.0840 1.00 -1.00 0.00 0.0720 -1.00 1.00 -1.00 0.0870 0.00 0.00 -1.00 0.0940 1.00 0.00 0.00 0.0090 -1.00 0.00 0.00 0.0840 -1.00 -1.00 1.00 0.0920 -1.00 -1.00 0.00 0.0920 1.00 1.00 -1.00 0.0780 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 O1 Ir N1 74.39(5) 2_655 . N2 Ir O1 88.08(5) . 2_655 N2 Ir N1 95.38(5) . . N3 Ir O1 95.17(5) . 2_655 N3 Ir N1 91.52(5) . . N3 Ir N2 172.95(5) . . C2 Ir O1 94.89(5) . 2_655 C2 Ir N1 168.70(5) . . C2 Ir N2 80.43(6) . . C2 Ir N3 93.04(6) . . C2 Ir C13 84.55(6) . . C13 Ir O1 175.57(5) . 2_655 C13 Ir N1 106.41(6) . . C13 Ir N2 96.15(6) . . C13 Ir N3 80.49(6) . . C1 O1 Ir 113.53(10) . 2_655 C27 O2 C30A 115.8(4) . . C27 O2 C30B 123.8(3) . . N1 N1 Ir 114.05(12) 2_655 . C1 N1 Ir 133.97(10) . . C1 N1 N1 111.64(15) . 2_655 C8 N2 Ir 115.95(10) . . C12 N2 Ir 125.18(11) . . C12 N2 C8 118.87(13) . . C19 N3 Ir 115.91(10) . . C23 N3 Ir 123.88(11) . . C23 N3 C19 119.72(14) . . O1 C1 N1 126.32(14) . . O1 C1 C24 114.64(13) . . N1 C1 C24 118.98(13) . . C3 C2 Ir 128.23(12) . . C3 C2 C7 116.91(15) . . C7 C2 Ir 114.86(11) . . C4 C3 C2 121.46(15) . . C3 C4 C5 120.74(16) . . C6 C5 C4 119.51(16) . . C5 C6 C7 119.76(15) . . C2 C7 C8 114.94(14) . . C6 C7 C2 121.60(14) . . C6 C7 C8 123.46(14) . . N2 C8 C7 113.77(13) . . N2 C8 C9 120.35(14) . . C9 C8 C7 125.88(15) . . C10 C9 C8 120.49(15) . . C9 C10 C11 118.66(15) . . C12 C11 C10 118.89(15) . . N2 C12 C11 122.71(15) . . C14 C13 Ir 128.44(12) . . C14 C13 C18 116.78(14) . . C18 C13 Ir 114.61(11) . . C15 C14 C13 121.49(16) . . C14 C15 C16 120.82(17) . . C17 C16 C15 119.57(16) . . C16 C17 C18 119.76(16) . . C13 C18 C19 114.93(14) . . C17 C18 C13 121.54(15) . . C17 C18 C19 123.46(14) . . N3 C19 C18 113.92(13) . . N3 C19 C20 119.82(15) . . C20 C19 C18 126.15(15) . . C21 C20 C19 120.45(16) . . C20 C21 C22 119.14(16) . . C23 C22 C21 118.64(16) . . N3 C23 C22 122.18(16) . . C25 C24 C1 119.13(13) . . C25 C24 C29 115.25(14) . . C29 C24 C1 125.25(13) . . F1 C25 C24 118.90(14) . . F1 C25 C26 117.66(15) . . C24 C25 C26 123.44(15) . . F2 C26 C25 117.72(17) . . F2 C26 C27 121.49(17) . . C25 C26 C27 120.78(16) . . O2 C27 C26 127.47(18) . . O2 C27 C28 116.33(18) . . C28 C27 C26 116.20(16) . . F3 C28 C27 118.86(16) . . F3 C28 C29 119.04(16) . . C29 C28 C27 122.10(16) . . F4 C29 C24 119.64(14) . . F4 C29 C28 118.16(15) . . C28 C29 C24 122.19(15) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ir O1 2.1565(11) 2_655 Ir N1 2.1801(13) . Ir N2 2.0443(13) . Ir N3 2.0396(13) . Ir C2 1.9971(16) . Ir C13 2.0010(15) . F1 C25 1.3451(19) . F2 C26 1.346(2) . F3 C28 1.345(2) . F4 C29 1.3452(18) . O1 Ir 2.1566(11) 2_655 O1 C1 1.2825(19) . O2 C27 1.353(2) . O2 C30A 1.511(10) . O2 C30B 1.354(7) . N1 N1 1.439(2) 2_655 N1 C1 1.3135(19) . N2 C8 1.365(2) . N2 C12 1.350(2) . N3 C19 1.365(2) . N3 C23 1.353(2) . C1 C24 1.494(2) . C2 C3 1.404(2) . C2 C7 1.415(2) . C3 C4 1.386(2) . C4 C5 1.394(2) . C5 C6 1.387(2) . C6 C7 1.402(2) . C7 C8 1.463(2) . C8 C9 1.394(2) . C9 C10 1.379(2) . C10 C11 1.393(2) . C11 C12 1.380(2) . C13 C14 1.400(2) . C13 C18 1.417(2) . C14 C15 1.385(2) . C15 C16 1.391(3) . C16 C17 1.381(3) . C17 C18 1.403(2) . C18 C19 1.459(2) . C19 C20 1.397(2) . C20 C21 1.376(3) . C21 C22 1.398(3) . C22 C23 1.381(2) . C24 C25 1.380(2) . C24 C29 1.387(2) . C25 C26 1.380(2) . C26 C27 1.390(3) . C27 C28 1.388(3) . C28 C29 1.376(2) .