#------------------------------------------------------------------------------ #$Date: 2018-01-12 03:58:53 +0200 (Fri, 12 Jan 2018) $ #$Revision: 205098 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/11/7121129.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_7121129 loop_ _publ_author_name 'Kubanik, Mario' 'Lam, Nelson Y. S.' 'Holtkamp, Hannah U.' 'S\"ohnel, Tilo' 'Anderson, Robert F.' 'Jamieson, Stephen M. F.' 'Hartinger, Christian G.' _publ_section_title ; Quinoline-para-quinones and metals: coordination-assisted formation of quinoline-ortho-quinones ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/C7CC09478G _journal_year 2018 _chemical_formula_moiety 'C19 H18 Cl2 Ir N O3' _chemical_formula_sum 'C19 H18 Cl2 Ir N O3' _chemical_formula_weight 571.44 _chemical_name_systematic ; Chlorido(7-chloro-8-hydroxyquinolinolato-5,6-dione-?N1,?O8)(?5-pentamethylcyclopentadienyl)iridium(III) ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2017-08-31 deposited with the CCDC. 2018-01-02 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 92.400(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.4492(8) _cell_length_b 7.3746(4) _cell_length_c 17.1873(9) _cell_measurement_reflns_used 9975 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25.226 _cell_measurement_theta_min 3.125 _cell_volume 1829.82(17) _computing_cell_refinement 'SAINT (Bruker, 2008)' _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_data_reduction 'SAINT (Bruker, 2008)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXS-2016/6 (Sheldrick, 2016)' _diffrn_ambient_temperature 100(2) _diffrn_detector 'Bruker APEX2 area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART APEX2 area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0650 _diffrn_reflns_av_unetI/netI 0.0502 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 19988 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.498 _diffrn_reflns_theta_min 2.709 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\ms' _exptl_absorpt_coefficient_mu 7.608 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.4269 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1333 before and 0.0919 after correction. The Ratio of minimum to maximum transmission is 0.5726. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour black _exptl_crystal_density_diffrn 2.074 _exptl_crystal_description fragment _exptl_crystal_F_000 1096 _exptl_crystal_size_max 0.280 _exptl_crystal_size_mid 0.220 _exptl_crystal_size_min 0.140 _refine_diff_density_max 1.146 _refine_diff_density_min -1.719 _refine_diff_density_rms 0.197 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 240 _refine_ls_number_reflns 4198 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.089 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_gt 0.0287 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+0.7876P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0730 _refine_ls_wR_factor_ref 0.0745 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3845 _reflns_number_total 4198 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7cc09478g2.cif _cod_data_source_block maku213_0m _cod_database_code 7121129 _shelx_shelxl_version_number 2016/6 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.225 _shelx_estimated_absorpt_t_max 0.416 _shelx_res_file ; TITL MaKu213_0m in P2(1)/c maku213_0m.res created by SHELXL-2016/6 at 12:56:26 on 31-Aug-2017 CELL 0.71073 14.4492 7.3746 17.1873 90.000 92.400 90.000 ZERR 4.00 0.0008 0.0004 0.0009 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H CL IR N O UNIT 76 72 8 4 4 12 MERG 2 OMIT -2.00 55.00 OMIT -3 1 5 OMIT -3 3 4 OMIT -2 1 6 OMIT -3 1 4 OMIT -2 1 7 OMIT 1 0 4 OMIT -4 2 5 OMIT 3 3 0 OMIT -6 6 10 OMIT 1 4 5 OMIT -3 3 6 FMAP 2 PLAN 25 SIZE 0.140 0.220 0.280 ACTA L.S. 10 TEMP -173.00 WGHT 0.033700 0.787600 FVAR 0.08209 C1 1 0.881937 0.034678 0.190868 11.00000 0.01810 0.02710 = 0.01513 0.00553 -0.00083 -0.00591 AFIX 43 H1 2 0.857009 -0.013523 0.236777 11.00000 -1.20000 AFIX 0 C2 1 0.972147 0.100231 0.193783 11.00000 0.01586 0.03899 = 0.01769 0.00133 -0.00546 -0.00541 AFIX 43 H2 2 1.008960 0.093283 0.240797 11.00000 -1.20000 AFIX 0 C3 1 1.007608 0.174754 0.128630 11.00000 0.01198 0.03387 = 0.02111 -0.00066 0.00030 -0.00466 AFIX 43 H3 2 1.069316 0.219409 0.129600 11.00000 -1.20000 AFIX 0 C4 1 0.951567 0.184094 0.060648 11.00000 0.01292 0.02362 = 0.01626 0.00105 0.00421 -0.00387 C5 1 0.983743 0.268362 -0.012221 11.00000 0.01943 0.02338 = 0.01830 -0.00114 0.00522 -0.00756 C6 1 0.912281 0.296140 -0.080239 11.00000 0.02460 0.02340 = 0.01540 -0.00263 0.00768 -0.00506 C7 1 0.825663 0.204090 -0.075072 11.00000 0.01586 0.01939 = 0.01096 -0.00012 0.00111 -0.00275 C8 1 0.797532 0.116284 -0.008691 11.00000 0.01247 0.01270 = 0.01324 -0.00345 0.00113 0.00293 C9 1 0.862887 0.113836 0.060796 11.00000 0.01151 0.01388 = 0.01306 -0.00175 0.00335 -0.00291 C18 1 0.718863 -0.337663 0.153706 11.00000 0.01254 0.01124 = 0.02114 0.00544 0.00456 -0.00047 C19 1 0.811726 -0.416833 0.176490 11.00000 0.01560 0.02088 = 0.02789 0.00511 -0.00386 0.00082 AFIX 137 H19A 2 0.804230 -0.544138 0.191320 11.00000 -1.50000 H19B 2 0.839270 -0.348974 0.220682 11.00000 -1.50000 H19C 2 0.852340 -0.409103 0.132353 11.00000 -1.50000 AFIX 0 C10 1 0.674075 -0.344934 0.078293 11.00000 0.01407 0.00706 = 0.01977 0.00333 0.00416 -0.00104 C11 1 0.709811 -0.429595 0.006495 11.00000 0.02457 0.02400 = 0.01938 -0.00313 0.00363 -0.00422 AFIX 137 H11A 2 0.777640 -0.433356 0.010476 11.00000 -1.50000 H11B 2 0.689700 -0.357732 -0.039102 11.00000 -1.50000 H1C 2 0.685530 -0.553224 0.001019 11.00000 -1.50000 AFIX 0 C12 1 0.584120 -0.257112 0.083701 11.00000 0.01101 0.01221 = 0.02944 0.00302 -0.00023 -0.00381 C13 1 0.513721 -0.242041 0.017219 11.00000 0.02434 0.02050 = 0.04788 0.00210 -0.01826 -0.00368 AFIX 137 H13A 2 0.481906 -0.358507 0.009792 11.00000 -1.50000 H13B 2 0.544881 -0.209783 -0.030413 11.00000 -1.50000 H13C 2 0.468437 -0.147998 0.028896 11.00000 -1.50000 AFIX 0 C14 1 0.574729 -0.196880 0.162094 11.00000 0.01366 0.01691 = 0.03202 0.00394 0.00922 -0.00367 C15 1 0.493700 -0.099820 0.192797 11.00000 0.02348 0.02368 = 0.05552 -0.00040 0.01868 0.00002 AFIX 137 H15A 2 0.454986 -0.052392 0.149249 11.00000 -1.50000 H15B 2 0.515430 0.000825 0.226015 11.00000 -1.50000 H15C 2 0.457310 -0.183958 0.223352 11.00000 -1.50000 AFIX 0 C16 1 0.659724 -0.240171 0.205632 11.00000 0.02190 0.01503 = 0.01682 0.00317 0.00718 -0.00592 C17 1 0.677183 -0.211904 0.291598 11.00000 0.04768 0.02896 = 0.01723 0.00352 0.00770 -0.00789 AFIX 137 H17A 2 0.643143 -0.104722 0.308250 11.00000 -1.50000 H17B 2 0.743623 -0.193910 0.302724 11.00000 -1.50000 H17C 2 0.656168 -0.318648 0.319872 11.00000 -1.50000 AFIX 0 N1 5 0.828879 0.037836 0.124388 11.00000 0.01097 0.01687 = 0.01304 0.00085 -0.00005 -0.00429 O1 6 0.719234 0.042997 -0.000748 11.00000 0.01369 0.01870 = 0.01409 0.00215 -0.00037 -0.00401 O3 6 0.935016 0.392218 -0.134530 11.00000 0.03337 0.04032 = 0.02022 0.00969 0.00587 -0.01720 O2 6 1.062981 0.314717 -0.018572 11.00000 0.01949 0.06486 = 0.02742 0.00693 0.00622 -0.01546 CL1 3 0.645502 0.231940 0.145768 11.00000 0.01784 0.01497 = 0.02139 -0.00184 0.00459 -0.00036 CL2 3 0.748737 0.221539 -0.154569 11.00000 0.02400 0.02820 = 0.01466 0.00340 -0.00197 -0.00188 IR 4 0.693414 -0.065900 0.112101 11.00000 0.00860 0.01295 = 0.01214 0.00045 0.00209 -0.00243 HKLF 4 REM MaKu213_0m in P2(1)/c REM R1 = 0.0287 for 3845 Fo > 4sig(Fo) and 0.0315 for all 4198 data REM 240 parameters refined using 0 restraints END WGHT 0.0337 0.7876 REM Highest difference peak 1.146, deepest hole -1.719, 1-sigma level 0.197 Q1 1 0.7140 -0.0613 0.1755 11.00000 0.05 1.15 Q2 1 0.6372 -0.0318 0.1656 11.00000 0.05 1.13 Q3 1 0.7198 -0.1543 0.1441 11.00000 0.05 0.95 Q4 1 0.7388 -0.0841 0.0547 11.00000 0.05 0.92 Q5 1 0.6774 -0.0616 0.0468 11.00000 0.05 0.91 Q6 1 0.6972 -0.2844 0.1063 11.00000 0.05 0.89 Q7 1 0.6735 0.0876 0.1387 11.00000 0.05 0.89 Q8 1 0.6225 0.1524 0.0939 11.00000 0.05 0.78 Q9 1 0.4793 -0.4382 0.0337 11.00000 0.05 0.76 Q10 1 0.6743 -0.2231 0.1410 11.00000 0.05 0.75 Q11 1 0.8755 -0.3495 0.1823 11.00000 0.05 0.73 Q12 1 0.6890 0.3279 0.1150 11.00000 0.05 0.71 Q13 1 0.7216 0.0867 0.0935 11.00000 0.05 0.68 Q14 1 1.1124 0.1532 -0.0509 11.00000 0.05 0.68 Q15 1 0.6821 0.1613 0.1753 11.00000 0.05 0.63 Q16 1 0.7058 -0.2003 -0.0399 11.00000 0.05 0.60 Q17 1 0.8207 0.0648 0.2385 11.00000 0.05 0.60 Q18 1 0.8777 0.2636 0.2088 11.00000 0.05 0.60 Q19 1 0.6418 -0.1477 0.1746 11.00000 0.05 0.59 Q20 1 0.6641 -0.0660 0.3478 11.00000 0.05 0.58 Q21 1 0.7577 0.1310 0.1290 11.00000 0.05 0.57 Q22 1 0.9258 -0.4499 0.0957 11.00000 0.05 0.57 Q23 1 0.4026 -0.1690 0.2908 11.00000 0.05 0.55 Q24 1 0.5843 0.2220 0.0755 11.00000 0.05 0.55 Q25 1 0.9588 0.3104 -0.0419 11.00000 0.05 0.55 ; _shelx_res_checksum 11214 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp C1 C 0.8819(3) 0.0347(6) 0.1909(3) 0.0202(9) Uani 1 1 d . . H1 H 0.857009 -0.013523 0.236777 0.024 Uiso 1 1 calc R U C2 C 0.9721(3) 0.1002(7) 0.1938(3) 0.0244(10) Uani 1 1 d . . H2 H 1.008960 0.093283 0.240797 0.029 Uiso 1 1 calc R U C3 C 1.0076(3) 0.1748(7) 0.1286(2) 0.0223(9) Uani 1 1 d . . H3 H 1.069316 0.219409 0.129600 0.027 Uiso 1 1 calc R U C4 C 0.9516(2) 0.1841(6) 0.0606(2) 0.0175(8) Uani 1 1 d . . C5 C 0.9837(3) 0.2684(6) -0.0122(2) 0.0202(9) Uani 1 1 d . . C6 C 0.9123(3) 0.2961(6) -0.0802(2) 0.0209(9) Uani 1 1 d . . C7 C 0.8257(3) 0.2041(6) -0.0751(2) 0.0154(8) Uani 1 1 d . . C8 C 0.7975(2) 0.1163(6) -0.0087(2) 0.0128(7) Uani 1 1 d . . C9 C 0.8629(2) 0.1138(6) 0.0608(2) 0.0127(7) Uani 1 1 d . . C18 C 0.7189(2) -0.3377(6) 0.1537(2) 0.0149(8) Uani 1 1 d . . C19 C 0.8117(3) -0.4168(6) 0.1765(3) 0.0216(10) Uani 1 1 d . . H19A H 0.804230 -0.544138 0.191320 0.032 Uiso 1 1 calc R U H19B H 0.839270 -0.348974 0.220682 0.032 Uiso 1 1 calc R U H19C H 0.852340 -0.409103 0.132353 0.032 Uiso 1 1 calc R U C10 C 0.6741(2) -0.3449(5) 0.0783(2) 0.0135(8) Uani 1 1 d . . C11 C 0.7098(3) -0.4296(6) 0.0065(3) 0.0226(10) Uani 1 1 d . . H11A H 0.777640 -0.433356 0.010476 0.034 Uiso 1 1 calc R U H11B H 0.689700 -0.357732 -0.039102 0.034 Uiso 1 1 calc R U H1C H 0.685530 -0.553224 0.001019 0.034 Uiso 1 1 calc R U C12 C 0.5841(2) -0.2571(6) 0.0837(3) 0.0176(8) Uani 1 1 d . . C13 C 0.5137(3) -0.2420(7) 0.0172(3) 0.0315(12) Uani 1 1 d . . H13A H 0.481906 -0.358507 0.009792 0.047 Uiso 1 1 calc R U H13B H 0.544881 -0.209783 -0.030413 0.047 Uiso 1 1 calc R U H13C H 0.468437 -0.147998 0.028896 0.047 Uiso 1 1 calc R U C14 C 0.5747(3) -0.1969(6) 0.1621(3) 0.0206(9) Uani 1 1 d . . C15 C 0.4937(3) -0.0998(7) 0.1928(4) 0.0338(12) Uani 1 1 d . . H15A H 0.454986 -0.052392 0.149249 0.051 Uiso 1 1 calc R U H15B H 0.515430 0.000825 0.226015 0.051 Uiso 1 1 calc R U H15C H 0.457310 -0.183958 0.223352 0.051 Uiso 1 1 calc R U C16 C 0.6597(3) -0.2402(6) 0.2056(2) 0.0177(8) Uani 1 1 d . . C17 C 0.6772(4) -0.2119(7) 0.2916(3) 0.0311(11) Uani 1 1 d . . H17A H 0.643143 -0.104722 0.308250 0.047 Uiso 1 1 calc R U H17B H 0.743623 -0.193910 0.302724 0.047 Uiso 1 1 calc R U H17C H 0.656168 -0.318648 0.319872 0.047 Uiso 1 1 calc R U N1 N 0.8289(2) 0.0378(5) 0.12439(19) 0.0136(7) Uani 1 1 d . . O1 O 0.71923(19) 0.0430(4) -0.00075(17) 0.0155(6) Uani 1 1 d . . O3 O 0.9350(2) 0.3922(5) -0.13453(19) 0.0312(8) Uani 1 1 d . . O2 O 1.0630(2) 0.3147(6) -0.0186(2) 0.0371(9) Uani 1 1 d . . Cl1 Cl 0.64550(6) 0.23194(14) 0.14577(6) 0.0180(2) Uani 1 1 d . . Cl2 Cl 0.74874(7) 0.22154(15) -0.15457(6) 0.0224(2) Uani 1 1 d . . Ir Ir 0.69341(2) -0.06590(2) 0.11210(2) 0.01118(7) Uani 1 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0181(19) 0.027(2) 0.015(2) 0.0055(18) -0.0008(16) -0.0059(17) C2 0.0159(19) 0.039(3) 0.018(2) 0.001(2) -0.0055(17) -0.0054(19) C3 0.0120(16) 0.034(3) 0.021(2) -0.001(2) 0.0003(15) -0.0047(17) C4 0.0129(16) 0.024(2) 0.0163(19) 0.0011(17) 0.0042(15) -0.0039(16) C5 0.0194(18) 0.023(2) 0.018(2) -0.0011(17) 0.0052(15) -0.0076(17) C6 0.025(2) 0.023(2) 0.0154(19) -0.0026(18) 0.0077(16) -0.0051(18) C7 0.0159(17) 0.019(2) 0.0110(17) -0.0001(16) 0.0011(14) -0.0028(16) C8 0.0125(16) 0.0127(19) 0.0132(18) -0.0034(16) 0.0011(14) 0.0029(15) C9 0.0115(16) 0.0139(19) 0.0131(18) -0.0018(16) 0.0033(14) -0.0029(15) C18 0.0125(16) 0.0112(19) 0.021(2) 0.0054(16) 0.0046(15) -0.0005(15) C19 0.0156(19) 0.021(2) 0.028(2) 0.0051(18) -0.0039(18) 0.0008(16) C10 0.0141(16) 0.0071(19) 0.0198(19) 0.0033(16) 0.0042(15) -0.0010(15) C11 0.025(2) 0.024(3) 0.019(2) -0.0031(17) 0.0036(18) -0.0042(17) C12 0.0110(16) 0.012(2) 0.029(2) 0.0030(17) -0.0002(15) -0.0038(15) C13 0.024(2) 0.021(2) 0.048(3) 0.002(2) -0.018(2) -0.0037(19) C14 0.0137(17) 0.017(2) 0.032(2) 0.0039(19) 0.0092(16) -0.0037(16) C15 0.023(2) 0.024(3) 0.056(3) 0.000(2) 0.019(2) 0.0000(19) C16 0.0219(18) 0.015(2) 0.0168(19) 0.0032(16) 0.0072(15) -0.0059(16) C17 0.048(3) 0.029(3) 0.017(2) 0.004(2) 0.008(2) -0.008(2) N1 0.0110(14) 0.0169(18) 0.0130(16) 0.0009(13) -0.0001(13) -0.0043(12) O1 0.0137(13) 0.0187(16) 0.0141(14) 0.0021(11) -0.0004(11) -0.0040(11) O3 0.0334(17) 0.040(2) 0.0202(16) 0.0097(15) 0.0059(14) -0.0172(16) O2 0.0195(15) 0.065(3) 0.0274(17) 0.0069(18) 0.0062(13) -0.0155(16) Cl1 0.0178(4) 0.0150(5) 0.0214(5) -0.0018(4) 0.0046(4) -0.0004(4) Cl2 0.0240(5) 0.0282(6) 0.0147(4) 0.0034(4) -0.0020(4) -0.0019(4) Ir 0.00860(9) 0.01295(11) 0.01214(10) 0.00045(5) 0.00209(6) -0.00243(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N1 C1 C2 121.6(4) C3 C2 C1 119.6(4) C2 C3 C4 118.8(4) C9 C4 C3 119.0(4) C9 C4 C5 118.7(3) C3 C4 C5 122.3(3) O2 C5 C4 121.7(4) O2 C5 C6 120.2(4) C4 C5 C6 118.1(3) O3 C6 C7 125.7(4) O3 C6 C5 117.5(4) C7 C6 C5 116.8(4) C8 C7 C6 124.1(3) C8 C7 Cl2 118.9(3) C6 C7 Cl2 116.8(3) O1 C8 C7 125.6(3) O1 C8 C9 116.6(3) C7 C8 C9 117.8(3) N1 C9 C4 122.0(3) N1 C9 C8 114.6(3) C4 C9 C8 123.4(4) C10 C18 C16 108.7(3) C10 C18 C19 126.1(4) C16 C18 C19 125.1(4) C10 C18 Ir 70.6(2) C16 C18 Ir 69.3(2) C19 C18 Ir 125.9(3) C18 C10 C12 107.3(4) C18 C10 C11 127.4(4) C12 C10 C11 125.3(4) C18 C10 Ir 70.7(2) C12 C10 Ir 70.4(2) C11 C10 Ir 125.2(3) C14 C12 C10 108.5(3) C14 C12 C13 127.3(4) C10 C12 C13 124.1(4) C14 C12 Ir 71.4(2) C10 C12 Ir 70.1(2) C13 C12 Ir 126.1(3) C12 C14 C16 107.9(4) C12 C14 C15 126.2(4) C16 C14 C15 125.9(4) C12 C14 Ir 70.0(2) C16 C14 Ir 68.7(2) C15 C14 Ir 124.8(3) C14 C16 C18 107.5(3) C14 C16 C17 125.6(4) C18 C16 C17 126.5(4) C14 C16 Ir 72.1(2) C18 C16 Ir 71.1(2) C17 C16 Ir 128.6(3) C9 N1 C1 118.9(3) C9 N1 Ir 116.2(2) C1 N1 Ir 124.9(3) C8 O1 Ir 116.6(2) N1 Ir C16 112.62(14) N1 Ir O1 76.02(11) C16 Ir O1 164.05(14) N1 Ir C10 118.96(14) C16 Ir C10 66.17(16) O1 Ir C10 98.00(13) N1 Ir C18 99.20(13) C16 Ir C18 39.60(16) O1 Ir C18 127.90(13) C10 Ir C18 38.64(15) N1 Ir C12 158.33(15) C16 Ir C12 65.69(15) O1 Ir C12 101.15(14) C10 Ir C12 39.55(14) C18 Ir C12 65.18(14) N1 Ir C14 150.11(15) C16 Ir C14 39.24(15) O1 Ir C14 133.83(13) C10 Ir C14 65.60(16) C18 Ir C14 65.32(15) C12 Ir C14 38.54(17) N1 Ir Cl1 85.35(10) C16 Ir Cl1 107.16(12) O1 Ir Cl1 86.43(8) C10 Ir Cl1 155.67(10) C18 Ir Cl1 145.55(11) C12 Ir Cl1 116.12(11) C14 Ir Cl1 94.10(12) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 N1 1.349(5) C1 C2 1.389(6) C2 C3 1.366(6) C3 C4 1.395(5) C4 C9 1.382(5) C4 C5 1.490(6) C5 O2 1.204(5) C5 C6 1.541(6) C6 O3 1.227(5) C6 C7 1.430(6) C7 C8 1.387(6) C7 Cl2 1.730(4) C8 O1 1.266(5) C8 C9 1.491(5) C9 N1 1.340(5) C18 C10 1.425(6) C18 C16 1.452(6) C18 C19 1.500(5) C18 Ir 2.154(4) C10 C12 1.459(5) C10 C11 1.494(6) C10 Ir 2.153(4) C12 C14 1.431(6) C12 C13 1.502(5) C12 Ir 2.158(4) C14 C16 1.447(5) C14 C15 1.488(6) C14 Ir 2.176(4) C16 C17 1.503(6) C16 Ir 2.130(4) N1 Ir 2.104(3) O1 Ir 2.146(3) Cl1 Ir 2.3816(10)