#------------------------------------------------------------------------------ #$Date: 2017-11-02 04:52:44 +0200 (Thu, 02 Nov 2017) $ #$Revision: 202505 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/78/1547865.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_1547865 loop_ _publ_author_name 'Islamova, Regina M. M' 'Dobrynin, Mikhail V.' 'Vlasov, Andrey V.' 'Eremina, Anzhelika A.' 'Kinzhalov, Mikhail A.' 'Kolesnikov, Ilya E.' 'Zolotarev, Andrei' 'Masloborodova, Eleonora A.' 'Luzyanin, Konstantin' _publ_section_title ; Iridium(III)-catalysed cross-linking of polysiloxanes leading to the thermally resistant luminescent silicone rubbers ; _journal_name_full 'Catalysis Science & Technology' _journal_paper_doi 10.1039/C7CY02013A _journal_year 2017 _chemical_formula_moiety 'C31 H25 Cl Ir N3, C H2 Cl2' _chemical_formula_sum 'C32 H27 Cl3 Ir N3' _chemical_formula_weight 752.12 _chemical_name_systematic ; ? ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_date 2015-01-27 _audit_creation_method ; Olex2 1.2-ac2 (compiled 2012.03.27 svn.r2268, GUI svn.r4156) ; _audit_update_record ; 2016-10-06 deposited with the CCDC. 2017-11-01 downloaded from the CCDC. ; _cell_angle_alpha 90.00 _cell_angle_beta 112.277(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 16.7446(4) _cell_length_b 8.57762(18) _cell_length_c 21.5557(5) _cell_measurement_reflns_used 13222 _cell_measurement_temperature 100.01(10) _cell_measurement_theta_max 75.9890 _cell_measurement_theta_min 2.8840 _cell_volume 2864.94(13) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100.01(10) _diffrn_detector_area_resol_mean 10.3829 _diffrn_measured_fraction_theta_full 0.9907 _diffrn_measured_fraction_theta_max 0.9907 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -40.00 30.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -40.3787 38.0000 -120.0000 70 #__ type_ start__ end____ width___ exp.time_ 2 omega -36.00 25.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -40.3787 38.0000 120.0000 61 #__ type_ start__ end____ width___ exp.time_ 3 omega -130.00 -88.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -40.3787 -178.0000 0.0000 42 #__ type_ start__ end____ width___ exp.time_ 4 omega -41.00 30.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -40.3787 38.0000 -180.0000 71 #__ type_ start__ end____ width___ exp.time_ 5 omega 105.00 130.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 40.3787 178.0000 90.0000 25 #__ type_ start__ end____ width___ exp.time_ 6 omega 88.00 169.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 30.0000 -60.0000 81 #__ type_ start__ end____ width___ exp.time_ 7 omega 29.00 54.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -95.0000 -120.0000 25 #__ type_ start__ end____ width___ exp.time_ 8 omega 59.00 89.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -30.0000 -60.0000 30 #__ type_ start__ end____ width___ exp.time_ 9 omega 113.00 146.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 60.0000 33 #__ type_ start__ end____ width___ exp.time_ 10 omega 73.00 103.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -112.0000 150.0000 30 #__ type_ start__ end____ width___ exp.time_ 11 omega 54.00 135.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 15.0000 120.0000 81 #__ type_ start__ end____ width___ exp.time_ 12 omega 35.00 61.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -30.0000 120.0000 26 #__ type_ start__ end____ width___ exp.time_ 13 omega 38.00 96.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -45.0000 -180.0000 58 #__ type_ start__ end____ width___ exp.time_ 14 omega 35.00 74.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -95.0000 -150.0000 39 #__ type_ start__ end____ width___ exp.time_ 15 omega 57.00 90.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -30.0000 0.0000 33 #__ type_ start__ end____ width___ exp.time_ 16 omega 50.00 94.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -45.0000 150.0000 44 #__ type_ start__ end____ width___ exp.time_ 17 omega 86.00 131.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 120.0000 45 #__ type_ start__ end____ width___ exp.time_ 18 omega 39.00 86.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -45.0000 120.0000 47 #__ type_ start__ end____ width___ exp.time_ 19 omega 122.00 177.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 45.0000 -30.0000 55 #__ type_ start__ end____ width___ exp.time_ 20 omega 116.00 144.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -77.0000 120.0000 28 #__ type_ start__ end____ width___ exp.time_ 21 omega 90.00 115.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -112.0000 -150.0000 25 #__ type_ start__ end____ width___ exp.time_ 22 omega 85.00 111.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -112.0000 -180.0000 26 #__ type_ start__ end____ width___ exp.time_ 23 omega 37.00 83.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -95.0000 -90.0000 46 #__ type_ start__ end____ width___ exp.time_ 24 omega 84.00 114.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -112.0000 30.0000 30 #__ type_ start__ end____ width___ exp.time_ 25 omega 99.00 126.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 45.0000 -60.0000 27 #__ type_ start__ end____ width___ exp.time_ 26 omega 83.00 134.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 30.0000 -180.0000 51 #__ type_ start__ end____ width___ exp.time_ 27 omega 89.00 114.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 -180.0000 25 #__ type_ start__ end____ width___ exp.time_ 28 omega 132.00 177.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 -180.0000 45 #__ type_ start__ end____ width___ exp.time_ 29 omega 83.00 115.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 120.0000 32 #__ type_ start__ end____ width___ exp.time_ 30 omega 35.00 60.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -30.0000 -90.0000 25 #__ type_ start__ end____ width___ exp.time_ 31 omega 66.00 92.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -45.0000 90.0000 26 #__ type_ start__ end____ width___ exp.time_ 32 omega 54.00 82.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -112.0000 -150.0000 28 #__ type_ start__ end____ width___ exp.time_ 33 omega 90.00 115.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -112.0000 -120.0000 25 #__ type_ start__ end____ width___ exp.time_ 34 omega 60.00 104.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -112.0000 -30.0000 44 #__ type_ start__ end____ width___ exp.time_ 35 omega 112.00 146.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -77.0000 150.0000 34 #__ type_ start__ end____ width___ exp.time_ 36 omega 82.00 108.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 178.0000 -30.0000 26 #__ type_ start__ end____ width___ exp.time_ 37 omega 57.00 82.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -77.0000 150.0000 25 #__ type_ start__ end____ width___ exp.time_ 38 omega -60.00 -14.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -40.3787 -77.0000 120.0000 46 #__ type_ start__ end____ width___ exp.time_ 39 omega -51.00 -25.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -40.3787 -38.0000 60.0000 26 #__ type_ start__ end____ width___ exp.time_ 40 omega -81.00 -33.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -40.3787 -38.0000 -90.0000 48 #__ type_ start__ end____ width___ exp.time_ 41 omega -51.00 -25.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -40.3787 -57.0000 60.0000 26 #__ type_ start__ end____ width___ exp.time_ 42 omega -70.00 -6.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -40.3787 -26.0000 150.7207 64 #__ type_ start__ end____ width___ exp.time_ 43 omega -65.00 -8.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -40.3787 -77.0000 -180.0000 57 #__ type_ start__ end____ width___ exp.time_ 44 omega -54.00 -24.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -40.3787 -77.0000 90.0000 30 #__ type_ start__ end____ width___ exp.time_ 45 omega -79.00 -54.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -40.3787 -57.0000 120.0000 25 #__ type_ start__ end____ width___ exp.time_ 46 omega -51.00 -26.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -40.3787 -57.0000 0.0000 25 #__ type_ start__ end____ width___ exp.time_ 47 omega -43.00 -14.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -40.3787 -57.0000 -90.0000 29 #__ type_ start__ end____ width___ exp.time_ 48 omega -37.00 -11.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -40.3787 57.0000 -30.0000 26 #__ type_ start__ end____ width___ exp.time_ 49 omega -71.00 -11.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -40.3787 -57.0000 -60.0000 60 #__ type_ start__ end____ width___ exp.time_ 50 omega -52.00 -26.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -40.3787 -77.0000 -150.0000 26 #__ type_ start__ end____ width___ exp.time_ 51 omega -57.00 -18.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -40.3787 -57.0000 -150.0000 39 #__ type_ start__ end____ width___ exp.time_ 52 omega 80.00 106.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 72.0000 147.4109 26 #__ type_ start__ end____ width___ exp.time_ 53 omega 140.00 165.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 66.0000 -100.0253 25 #__ type_ start__ end____ width___ exp.time_ 54 omega 142.00 168.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 51.0000 -158.4443 26 #__ type_ start__ end____ width___ exp.time_ 55 omega 82.00 108.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 66.0000 -100.0253 26 #__ type_ start__ end____ width___ exp.time_ 56 omega 81.00 107.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 68.0000 -147.2346 26 #__ type_ start__ end____ width___ exp.time_ 57 omega 84.00 109.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 51.0000 -158.4443 25 #__ type_ start__ end____ width___ exp.time_ 58 omega 82.00 108.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 63.0000 -146.8273 26 #__ type_ start__ end____ width___ exp.time_ 59 omega 83.00 109.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 -120.0000 26 #__ type_ start__ end____ width___ exp.time_ 60 omega 79.00 108.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 -150.0000 29 #__ type_ start__ end____ width___ exp.time_ 61 omega 79.00 104.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 -120.0000 25 #__ type_ start__ end____ width___ exp.time_ 62 omega 83.00 134.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 -150.0000 51 #__ type_ start__ end____ width___ exp.time_ 63 omega 83.00 109.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 150.0000 26 #__ type_ start__ end____ width___ exp.time_ 64 omega 123.00 149.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 150.0000 26 #__ type_ start__ end____ width___ exp.time_ 65 omega 78.00 104.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -15.0000 -60.0000 26 #__ type_ start__ end____ width___ exp.time_ 66 omega 79.00 104.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 -180.0000 25 #__ type_ start__ end____ width___ exp.time_ 67 omega 83.00 110.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 -90.0000 27 #__ type_ start__ end____ width___ exp.time_ 68 omega 84.00 110.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 -180.0000 26 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0080618000 _diffrn_orient_matrix_UB_12 -0.1782357000 _diffrn_orient_matrix_UB_13 0.0094406000 _diffrn_orient_matrix_UB_21 -0.0900877000 _diffrn_orient_matrix_UB_22 -0.0057535000 _diffrn_orient_matrix_UB_23 0.0036052000 _diffrn_orient_matrix_UB_31 -0.0413225000 _diffrn_orient_matrix_UB_32 -0.0223638000 _diffrn_orient_matrix_UB_33 -0.0765492000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_reflns_av_R_equivalents 0.0750 _diffrn_reflns_av_unetI/netI 0.0459 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 37122 _diffrn_reflns_theta_full 72.48 _diffrn_reflns_theta_max 72.48 _diffrn_reflns_theta_min 2.87 _diffrn_source 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 11.802 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.61703 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.744 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1472 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _refine_diff_density_max 2.312 _refine_diff_density_min -1.420 _refine_diff_density_rms 0.175 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 354 _refine_ls_number_reflns 5634 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.096 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0385 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+8.2494P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1049 _refine_ls_wR_factor_ref 0.1114 _reflns_number_gt 4867 _reflns_number_total 5634 _reflns_threshold_expression >2sigma(I) _cod_data_source_file c7cy02013a2.cif _cod_data_source_block km857 _cod_original_cell_volume 2864.94(12) _cod_database_code 1547865 _chemical_oxdiff_formula 'Ir1 N3 Cl1 C15 h20' _reflns_odcompleteness_completeness 93.70 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 80.95 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 '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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags Ir1 Ir 0.881692(14) 0.41206(3) 0.613652(11) 0.01661(10) Uani 1 1 d . Cl1 Cl 0.84072(8) 0.26826(16) 0.50583(6) 0.0222(3) Uani 1 1 d . Cl2 Cl 0.60598(11) 0.13387(19) 0.46284(9) 0.0371(3) Uani 1 1 d . Cl3 Cl 0.57229(13) 0.3308(3) 0.34455(9) 0.0487(5) Uani 1 1 d . N2 N 0.8906(3) 0.6077(5) 0.5619(2) 0.0186(9) Uani 1 1 d . C15 C 0.7584(3) 0.4958(6) 0.5859(3) 0.0185(10) Uani 1 1 d . C21 C 0.9106(3) 0.5196(7) 0.7033(3) 0.0187(10) Uani 1 1 d . N3 N 0.8548(3) 0.2336(5) 0.6664(2) 0.0174(9) Uani 1 1 d . C1 C 1.0030(4) 0.3378(7) 0.6384(3) 0.0207(11) Uani 1 1 d . N1 N 1.0718(3) 0.2918(6) 0.6522(2) 0.0225(10) Uani 1 1 d . C22 C 0.9437(4) 0.6697(7) 0.7218(3) 0.0243(12) Uani 1 1 d . H22 H 0.9544 0.7329 0.6907 0.029 Uiso 1 1 calc R C26 C 0.8961(4) 0.4261(7) 0.7520(3) 0.0200(11) Uani 1 1 d . C19 C 0.6083(4) 0.5054(7) 0.5755(3) 0.0239(12) Uani 1 1 d . H19 H 0.5630 0.4605 0.5841 0.029 Uiso 1 1 calc R C23 C 0.9606(4) 0.7251(7) 0.7859(3) 0.0278(12) Uani 1 1 d . H23 H 0.9816 0.8259 0.7971 0.033 Uiso 1 1 calc R C28 C 0.8377(4) 0.1610(7) 0.7670(3) 0.0232(11) Uani 1 1 d . H28 H 0.8416 0.1854 0.8101 0.028 Uiso 1 1 calc R C10 C 0.9601(4) 0.6485(7) 0.5487(3) 0.0224(11) Uani 1 1 d . H10 H 1.0084 0.5843 0.5639 0.027 Uiso 1 1 calc R C32 C 0.6238(4) 0.3166(8) 0.4321(3) 0.0326(13) Uani 1 1 d . H32A H 0.6026 0.3988 0.4528 0.039 Uiso 1 1 calc R H32B H 0.6853 0.3321 0.4447 0.039 Uiso 1 1 calc R C29 C 0.8071(4) 0.0166(7) 0.7398(3) 0.0260(12) Uani 1 1 d . H29 H 0.7902 -0.0563 0.7644 0.031 Uiso 1 1 calc R C24 C 0.9466(4) 0.6319(8) 0.8341(3) 0.0274(12) Uani 1 1 d . H24 H 0.9589 0.6698 0.8771 0.033 Uiso 1 1 calc R C25 C 0.9141(4) 0.4824(7) 0.8169(3) 0.0245(12) Uani 1 1 d . H25 H 0.9042 0.4197 0.8485 0.029 Uiso 1 1 calc R C16 C 0.7436(4) 0.6373(6) 0.5500(3) 0.0190(10) Uani 1 1 d . C14 C 0.8175(4) 0.6991(7) 0.5370(3) 0.0204(11) Uani 1 1 d . C27 C 0.8627(3) 0.2692(7) 0.7303(3) 0.0203(11) Uani 1 1 d . C30 C 0.8016(4) -0.0185(7) 0.6753(3) 0.0236(11) Uani 1 1 d . H30 H 0.7807 -0.1143 0.6556 0.028 Uiso 1 1 calc R C12 C 0.8911(4) 0.8773(7) 0.4911(3) 0.0246(12) Uani 1 1 d . H12 H 0.8917 0.9686 0.4680 0.030 Uiso 1 1 calc R C18 C 0.5958(4) 0.6464(7) 0.5409(3) 0.0265(12) Uani 1 1 d . H18 H 0.5427 0.6968 0.5270 0.032 Uiso 1 1 calc R C2 C 1.1521(4) 0.2221(7) 0.6636(3) 0.0201(11) Uani 1 1 d . C9 C 1.0859(5) -0.0334(8) 0.6783(3) 0.0343(14) Uani 1 1 d . H9A H 1.0725 0.0007 0.7156 0.051 Uiso 1 1 calc R H9B H 1.1015 -0.1418 0.6837 0.051 Uiso 1 1 calc R H9C H 1.0365 -0.0193 0.6375 0.051 Uiso 1 1 calc R C31 C 0.8282(4) 0.0934(6) 0.6419(3) 0.0246(13) Uani 1 1 d . H31 H 0.8274 0.0692 0.5996 0.030 Uiso 1 1 calc R C17 C 0.6638(4) 0.7106(7) 0.5275(3) 0.0235(11) Uani 1 1 d . H17 H 0.6558 0.8029 0.5033 0.028 Uiso 1 1 calc R C11 C 0.9629(4) 0.7806(7) 0.5138(3) 0.0254(12) Uani 1 1 d . H11 H 1.0120 0.8050 0.5055 0.030 Uiso 1 1 calc R C3 C 1.1598(4) 0.0601(8) 0.6753(3) 0.0267(12) Uani 1 1 d . C5 C 1.3058(5) 0.0815(9) 0.6786(3) 0.0362(16) Uani 1 1 d . H5 H 1.3579 0.0338 0.6839 0.043 Uiso 1 1 calc R C13 C 0.8188(4) 0.8361(7) 0.5033(3) 0.0225(11) Uani 1 1 d . H13 H 0.7706 0.9007 0.4889 0.027 Uiso 1 1 calc R C6 C 1.2965(4) 0.2404(9) 0.6683(3) 0.0345(15) Uani 1 1 d . H6 H 1.3425 0.2988 0.6668 0.041 Uiso 1 1 calc R C7 C 1.2191(4) 0.3146(8) 0.6600(3) 0.0271(13) Uani 1 1 d . C4 C 1.2380(4) -0.0075(9) 0.6812(3) 0.0344(14) Uani 1 1 d . H4 H 1.2449 -0.1148 0.6870 0.041 Uiso 1 1 calc R C8 C 1.2066(4) 0.4861(9) 0.6457(4) 0.0351(15) Uani 1 1 d . H8A H 1.1769 0.5020 0.5984 0.053 Uiso 1 1 calc R H8B H 1.2618 0.5367 0.6604 0.053 Uiso 1 1 calc R H8C H 1.1731 0.5293 0.6691 0.053 Uiso 1 1 calc R C20 C 0.6883(4) 0.4312(7) 0.5974(3) 0.0208(11) Uani 1 1 d . H20 H 0.6954 0.3369 0.6201 0.025 Uiso 1 1 calc R 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 0.01548(15) 0.01897(14) 0.01935(14) 0.00119(8) 0.01109(11) 0.00153(8) Cl1 0.0223(6) 0.0258(6) 0.0226(6) -0.0008(5) 0.0130(5) 0.0027(5) Cl2 0.0337(8) 0.0314(8) 0.0472(9) 0.0048(7) 0.0167(7) 0.0039(6) Cl3 0.0402(10) 0.0606(12) 0.0359(9) 0.0081(8) 0.0037(8) -0.0167(9) N2 0.019(2) 0.019(2) 0.021(2) 0.0002(17) 0.011(2) 0.0004(17) C15 0.015(3) 0.021(3) 0.024(3) 0.001(2) 0.011(2) 0.003(2) C21 0.014(2) 0.023(3) 0.022(3) -0.002(2) 0.009(2) 0.002(2) N3 0.018(2) 0.017(2) 0.018(2) 0.0019(17) 0.0087(18) 0.0042(17) C1 0.020(3) 0.023(3) 0.026(3) 0.003(2) 0.015(2) 0.000(2) N1 0.019(2) 0.032(3) 0.020(2) 0.0009(19) 0.011(2) -0.001(2) C22 0.020(3) 0.023(3) 0.030(3) -0.002(2) 0.011(2) 0.001(2) C26 0.014(3) 0.026(3) 0.018(3) -0.001(2) 0.004(2) 0.003(2) C19 0.018(3) 0.031(3) 0.026(3) -0.002(2) 0.012(2) 0.000(2) C23 0.024(3) 0.027(3) 0.031(3) -0.003(2) 0.010(3) 0.000(2) C28 0.023(3) 0.028(3) 0.020(3) 0.004(2) 0.009(2) 0.003(2) C10 0.017(3) 0.029(3) 0.025(3) -0.003(2) 0.013(2) -0.001(2) C32 0.027(3) 0.029(3) 0.040(4) 0.003(3) 0.010(3) -0.002(3) C29 0.026(3) 0.025(3) 0.033(3) 0.005(2) 0.017(3) -0.001(2) C24 0.025(3) 0.034(3) 0.020(3) -0.006(2) 0.005(2) 0.005(2) C25 0.021(3) 0.031(3) 0.022(3) 0.001(2) 0.008(2) 0.002(2) C16 0.021(3) 0.019(3) 0.018(2) -0.002(2) 0.008(2) 0.002(2) C14 0.021(3) 0.021(3) 0.023(3) -0.001(2) 0.013(2) 0.002(2) C27 0.014(2) 0.027(3) 0.020(3) 0.003(2) 0.007(2) 0.003(2) C30 0.025(3) 0.020(3) 0.027(3) -0.002(2) 0.011(3) 0.000(2) C12 0.039(4) 0.021(3) 0.022(3) -0.001(2) 0.020(3) -0.003(2) C18 0.020(3) 0.031(3) 0.031(3) -0.001(2) 0.012(3) 0.003(2) C2 0.015(3) 0.030(3) 0.017(2) -0.001(2) 0.007(2) 0.003(2) C9 0.038(4) 0.034(3) 0.030(3) 0.001(3) 0.012(3) -0.003(3) C31 0.034(3) 0.018(3) 0.035(3) -0.001(2) 0.028(3) 0.001(2) C17 0.024(3) 0.023(3) 0.025(3) 0.000(2) 0.010(2) 0.002(2) C11 0.030(3) 0.025(3) 0.030(3) -0.005(2) 0.021(3) -0.005(2) C3 0.028(3) 0.035(3) 0.019(3) -0.001(2) 0.010(3) 0.006(3) C5 0.025(3) 0.053(4) 0.031(3) -0.001(3) 0.011(3) 0.013(3) C13 0.025(3) 0.024(3) 0.021(3) 0.001(2) 0.012(2) 0.004(2) C6 0.024(3) 0.053(4) 0.033(3) 0.001(3) 0.018(3) 0.002(3) C7 0.020(3) 0.042(4) 0.020(3) -0.001(2) 0.007(2) -0.002(3) C4 0.030(4) 0.041(4) 0.029(3) -0.001(3) 0.008(3) 0.012(3) C8 0.028(3) 0.042(4) 0.037(4) 0.009(3) 0.014(3) -0.006(3) C20 0.019(3) 0.025(3) 0.020(3) 0.000(2) 0.010(2) 0.001(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -4.7710 6.5667 '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 N2 Ir1 Cl1 87.08(13) N2 Ir1 N3 170.41(17) C15 Ir1 Cl1 90.61(16) C15 Ir1 N2 80.1(2) C15 Ir1 N3 90.85(19) C21 Ir1 Cl1 176.42(15) C21 Ir1 N2 96.1(2) C21 Ir1 C15 88.2(2) C21 Ir1 N3 80.5(2) N3 Ir1 Cl1 96.14(13) C1 Ir1 Cl1 89.09(17) C1 Ir1 N2 97.5(2) C1 Ir1 C15 177.5(2) C1 Ir1 C21 92.2(2) C1 Ir1 N3 91.62(19) C10 N2 Ir1 125.1(4) C10 N2 C14 118.7(5) C14 N2 Ir1 116.1(4) C16 C15 Ir1 114.2(4) C20 C15 Ir1 128.9(4) C20 C15 C16 116.9(5) C22 C21 Ir1 128.0(4) C22 C21 C26 118.2(5) C26 C21 Ir1 113.8(4) C27 N3 Ir1 115.7(4) C31 N3 Ir1 124.6(4) C31 N3 C27 119.7(5) N1 C1 Ir1 178.4(5) C1 N1 C2 173.5(6) C23 C22 C21 120.6(6) C21 C26 C27 115.8(5) C25 C26 C21 120.9(5) C25 C26 C27 123.2(5) C20 C19 C18 120.5(5) C22 C23 C24 121.1(6) C27 C28 C29 120.2(5) N2 C10 C11 123.0(5) Cl3 C32 Cl2 112.3(4) C28 C29 C30 119.4(5) C25 C24 C23 119.4(5) C24 C25 C26 119.9(5) C15 C16 C14 115.4(5) C17 C16 C15 121.9(5) C17 C16 C14 122.6(5) N2 C14 C16 114.1(5) N2 C14 C13 119.9(5) C13 C14 C16 126.0(5) N3 C27 C26 114.0(5) N3 C27 C28 119.5(5) C28 C27 C26 126.5(5) C31 C30 C29 117.5(6) C13 C12 C11 119.0(5) C17 C18 C19 119.0(5) N1 C2 C3 117.9(5) C7 C2 N1 118.9(5) C7 C2 C3 123.2(5) N3 C31 C30 123.7(5) C16 C17 C18 120.2(6) C10 C11 C12 118.8(5) C2 C3 C9 121.0(6) C4 C3 C2 116.5(6) C4 C3 C9 122.5(6) C6 C5 C4 120.4(6) C12 C13 C14 120.5(5) C5 C6 C7 120.9(6) C2 C7 C8 121.0(5) C6 C7 C2 117.4(6) C6 C7 C8 121.6(6) C5 C4 C3 121.5(7) C19 C20 C15 121.4(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ir1 Cl1 2.4869(13) Ir1 N2 2.051(5) Ir1 C15 2.049(5) Ir1 C21 2.027(5) Ir1 N3 2.056(4) Ir1 C1 1.999(6) Cl2 C32 1.771(7) Cl3 C32 1.756(7) N2 C10 1.345(7) N2 C14 1.379(7) C15 C16 1.410(8) C15 C20 1.402(7) C21 C22 1.398(8) C21 C26 1.414(8) N3 C27 1.367(7) N3 C31 1.321(7) C1 N1 1.146(8) N1 C2 1.406(7) C22 C23 1.386(8) C26 C25 1.401(8) C26 C27 1.465(8) C19 C18 1.395(9) C19 C20 1.394(8) C23 C24 1.399(9) C28 C29 1.383(9) C28 C27 1.383(8) C10 C11 1.371(8) C29 C30 1.391(8) C24 C25 1.387(9) C16 C14 1.469(7) C16 C17 1.386(8) C14 C13 1.386(8) C30 C31 1.372(8) C12 C11 1.388(9) C12 C13 1.378(8) C18 C17 1.391(8) C2 C3 1.409(9) C2 C7 1.400(8) C9 C3 1.496(9) C3 C4 1.393(9) C5 C6 1.381(11) C5 C4 1.385(11) C6 C7 1.393(9) C7 C8 1.502(10)