# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_publication _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Dr Warren B. Cross' _publ_contact_author_address ;Department of Chemistry, University of Leicester, University Road, Leicester, LE1 7RH, UK ; _publ_contact_author_email wbc2@le.ac.uk _publ_contact_author_phone '+44(0)116 252 2126' _publ_contact_author_fax '44 (0)116 252 3789' loop_ _publ_author_name _publ_author_address W.B.Cross ;Department of Chemistry, University of Leicester, University Road, Leicester, LE1 7RH, UK ; C.G.Daly ;Department of Chemistry, University of Leicester, University Road, Leicester, LE1 7RH, UK ; Y.Boutadla ;Department of Chemistry, University of Leicester, University Road, Leicester, LE1 7RH, UK ; K.Singh ;Department of Chemistry, University of Leicester, University Road, Leicester, LE1 7RH, UK ; _publ_section_title ;'Variable coordination of amine functionalised N-heterocyclic carbene ligands to Ru, Rh and Ir: C-H and N-H activation' ; data_11019 _database_code_depnum_ccdc_archive 'CCDC 823381' #TrackingRef '- Paper#2 cif files.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Cp*Rh(C,C)I (3)' _chemical_melting_point ? _chemical_formula_moiety 'C34 H45 I N3 Rh' _chemical_formula_sum 'C34 H45 I N3 Rh' _chemical_formula_weight 725.54 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.277(5) _cell_length_b 8.466(3) _cell_length_c 28.869(11) _cell_angle_alpha 90.00 _cell_angle_beta 95.710(8) _cell_angle_gamma 90.00 _cell_volume 3229(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 887 _cell_measurement_theta_min 2.793 _cell_measurement_theta_max 28.286 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 1.511 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.521 _exptl_absorpt_correction_T_max 0.831 _exptl_absorpt_process_details ; absorption correction based on 6595 reflections(SADABS);Rint 0.0819 before correction and 0.0696 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24670 _diffrn_reflns_av_R_equivalents 0.1738 _diffrn_reflns_av_sigmaI/netI 0.1267 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6361 _reflns_number_gt 4328 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. ; _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^)+(0.0408P)^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_number_reflns 6361 _refine_ls_number_parameters 363 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0907 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1242 _refine_ls_wR_factor_gt 0.1103 _refine_ls_goodness_of_fit_ref 0.922 _refine_ls_restrained_S_all 0.922 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 0.82231(3) 0.26063(5) 0.078322(16) 0.02200(14) Uani 1 1 d . . . I1 I 0.94385(3) 0.48419(5) 0.118497(15) 0.03323(14) Uani 1 1 d . . . N1 N 0.8049(4) 0.1608(6) 0.18080(17) 0.0281(12) Uani 1 1 d . . . N2 N 0.6936(4) 0.3251(6) 0.15051(17) 0.0247(11) Uani 1 1 d . . . N3 N 0.5050(4) 0.4943(6) 0.15494(17) 0.0312(13) Uani 1 1 d . . . H3 H 0.4995 0.4044 0.1622 0.037 Uiso 1 1 d R . . C1 C 0.7725(4) 0.2332(7) 0.1407(2) 0.0249(13) Uani 1 1 d . . . C2 C 0.7492(5) 0.2100(8) 0.2161(2) 0.0356(16) Uani 1 1 d . . . H2 H 0.7583 0.1764 0.2476 0.043 Uiso 1 1 calc R . . C3 C 0.6805(5) 0.3133(8) 0.1979(2) 0.0347(16) Uani 1 1 d . . . H3A H 0.6321 0.3682 0.2139 0.042 Uiso 1 1 calc R . . C4 C 0.6502(5) 0.4205(7) 0.1142(2) 0.0261(14) Uani 1 1 d . . . C5 C 0.7037(4) 0.4162(6) 0.07489(19) 0.0212(13) Uani 1 1 d . . . C6 C 0.6686(5) 0.5097(7) 0.0376(2) 0.0286(14) Uani 1 1 d . . . H6 H 0.7045 0.5120 0.0108 0.034 Uiso 1 1 calc R . . C7 C 0.5814(5) 0.6010(7) 0.0386(2) 0.0319(15) Uani 1 1 d . . . H7 H 0.5593 0.6659 0.0127 0.038 Uiso 1 1 calc R . . C8 C 0.5272(5) 0.5977(7) 0.0768(2) 0.0319(15) Uani 1 1 d . . . H8 H 0.4671 0.6585 0.0768 0.038 Uiso 1 1 calc R . . C9 C 0.5597(5) 0.5066(7) 0.1153(2) 0.0293(15) Uani 1 1 d . . . C10 C 0.8920(5) 0.0514(8) 0.1876(2) 0.0362(16) Uani 1 1 d . . . H10 H 0.9175 0.0341 0.1565 0.043 Uiso 1 1 calc R . . C11 C 0.8576(6) -0.1076(9) 0.2048(3) 0.058(2) Uani 1 1 d . . . H11A H 0.8369 -0.0957 0.2363 0.088 Uiso 1 1 calc R . . H11B H 0.9135 -0.1834 0.2054 0.088 Uiso 1 1 calc R . . H11C H 0.8002 -0.1461 0.1839 0.088 Uiso 1 1 calc R . . C12 C 0.9764(6) 0.1225(10) 0.2191(3) 0.061(2) Uani 1 1 d . . . H12A H 0.9917 0.2282 0.2079 0.092 Uiso 1 1 calc R . . H12B H 1.0367 0.0557 0.2194 0.092 Uiso 1 1 calc R . . H12C H 0.9560 0.1301 0.2508 0.092 Uiso 1 1 calc R . . C13 C 0.7648(5) 0.1080(7) 0.0217(2) 0.0291(15) Uani 1 1 d . . . C14 C 0.8251(5) 0.0143(7) 0.0556(2) 0.0296(15) Uani 1 1 d . . . C15 C 0.9268(5) 0.0648(7) 0.0585(2) 0.0288(15) Uani 1 1 d . . . C16 C 0.9314(5) 0.1920(7) 0.0257(2) 0.0307(15) Uani 1 1 d . . . C17 C 0.8343(5) 0.2168(7) 0.0029(2) 0.0290(15) Uani 1 1 d . . . C18 C 0.6564(5) 0.0836(9) 0.0049(3) 0.0475(19) Uani 1 1 d . . . H18A H 0.6513 0.0093 -0.0213 0.071 Uiso 1 1 calc R . . H18B H 0.6260 0.1848 -0.0054 0.071 Uiso 1 1 calc R . . H18C H 0.6206 0.0405 0.0301 0.071 Uiso 1 1 calc R . . C19 C 0.7845(5) -0.1287(8) 0.0786(2) 0.0424(18) Uani 1 1 d . . . H19A H 0.7822 -0.2185 0.0571 0.064 Uiso 1 1 calc R . . H19B H 0.7161 -0.1064 0.0868 0.064 Uiso 1 1 calc R . . H19C H 0.8287 -0.1544 0.1068 0.064 Uiso 1 1 calc R . . C20 C 1.0177(5) -0.0066(8) 0.0844(2) 0.0365(16) Uani 1 1 d . . . H20A H 0.9986 -0.1050 0.0992 0.055 Uiso 1 1 calc R . . H20B H 1.0462 0.0672 0.1084 0.055 Uiso 1 1 calc R . . H20C H 1.0682 -0.0293 0.0628 0.055 Uiso 1 1 calc R . . C21 C 1.0263(5) 0.2720(8) 0.0157(2) 0.0416(18) Uani 1 1 d . . . H21A H 1.0680 0.1986 -0.0004 0.062 Uiso 1 1 calc R . . H21B H 1.0637 0.3058 0.0450 0.062 Uiso 1 1 calc R . . H21C H 1.0099 0.3644 -0.0040 0.062 Uiso 1 1 calc R . . C22 C 0.8078(6) 0.3200(9) -0.0388(2) 0.053(2) Uani 1 1 d . . . H22A H 0.8346 0.4265 -0.0325 0.080 Uiso 1 1 calc R . . H22B H 0.7340 0.3252 -0.0455 0.080 Uiso 1 1 calc R . . H22C H 0.8374 0.2758 -0.0658 0.080 Uiso 1 1 calc R . . C23 C 0.4152(4) 0.5847(7) 0.1576(2) 0.0280(14) Uani 1 1 d . . . C24 C 0.4248(5) 0.7460(7) 0.1654(2) 0.0325(15) Uani 1 1 d . . . C25 C 0.3370(5) 0.8349(8) 0.1681(2) 0.0368(17) Uani 1 1 d . . . H25 H 0.3418 0.9458 0.1728 0.044 Uiso 1 1 calc R . . C26 C 0.2440(5) 0.7635(7) 0.1642(2) 0.0300(15) Uani 1 1 d . . . H26 H 0.1847 0.8253 0.1659 0.036 Uiso 1 1 calc R . . C27 C 0.2357(5) 0.6010(8) 0.1576(2) 0.0281(14) Uani 1 1 d . . . H27 H 0.1707 0.5531 0.1553 0.034 Uiso 1 1 calc R . . C28 C 0.3201(5) 0.5084(7) 0.1545(2) 0.0292(14) Uani 1 1 d . . . C29 C 0.5262(5) 0.8276(8) 0.1728(2) 0.0389(17) Uani 1 1 d . . . H29 H 0.5787 0.7503 0.1647 0.047 Uiso 1 1 calc R . . C30 C 0.5345(6) 0.9720(8) 0.1423(3) 0.055(2) Uani 1 1 d . . . H30A H 0.5174 0.9428 0.1096 0.082 Uiso 1 1 calc R . . H30B H 0.6038 1.0129 0.1465 0.082 Uiso 1 1 calc R . . H30C H 0.4875 1.0535 0.1510 0.082 Uiso 1 1 calc R . . C31 C 0.5493(6) 0.8687(10) 0.2240(3) 0.059(2) Uani 1 1 d . . . H31A H 0.5027 0.9511 0.2324 0.089 Uiso 1 1 calc R . . H31B H 0.6191 0.9071 0.2296 0.089 Uiso 1 1 calc R . . H31C H 0.5411 0.7744 0.2430 0.089 Uiso 1 1 calc R . . C32 C 0.3108(5) 0.3312(7) 0.1463(2) 0.0346(16) Uani 1 1 d . . . H32 H 0.3712 0.2810 0.1639 0.041 Uiso 1 1 calc R . . C33 C 0.3149(6) 0.2904(9) 0.0954(2) 0.051(2) Uani 1 1 d . . . H33A H 0.2538 0.3302 0.0772 0.077 Uiso 1 1 calc R . . H33B H 0.3187 0.1755 0.0918 0.077 Uiso 1 1 calc R . . H33C H 0.3748 0.3393 0.0841 0.077 Uiso 1 1 calc R . . C34 C 0.2185(6) 0.2588(8) 0.1642(3) 0.056(2) Uani 1 1 d . . . H34A H 0.2187 0.2818 0.1975 0.084 Uiso 1 1 calc R . . H34B H 0.2195 0.1442 0.1595 0.084 Uiso 1 1 calc R . . H34C H 0.1574 0.3033 0.1473 0.084 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 Rh1 0.0230(3) 0.0202(3) 0.0230(3) -0.0013(2) 0.0035(2) 0.0026(2) I1 0.0314(2) 0.0278(2) 0.0403(3) -0.00525(19) 0.0023(2) -0.00313(19) N1 0.031(3) 0.034(3) 0.020(3) 0.005(2) 0.003(2) 0.006(2) N2 0.029(3) 0.025(3) 0.021(3) 0.000(2) 0.004(2) 0.003(2) N3 0.033(3) 0.029(3) 0.033(3) 0.004(2) 0.009(3) 0.006(2) C1 0.027(3) 0.022(3) 0.025(3) 0.000(3) 0.004(3) -0.003(3) C2 0.047(4) 0.039(4) 0.023(3) 0.003(3) 0.009(3) 0.004(3) C3 0.033(4) 0.043(4) 0.029(4) 0.001(3) 0.009(3) 0.005(3) C4 0.033(4) 0.019(3) 0.027(3) -0.003(3) 0.005(3) 0.001(3) C5 0.026(3) 0.017(3) 0.021(3) -0.001(2) 0.002(3) 0.002(2) C6 0.030(3) 0.027(3) 0.030(4) -0.006(3) 0.008(3) 0.002(3) C7 0.038(4) 0.026(3) 0.032(4) 0.002(3) 0.004(3) 0.013(3) C8 0.022(3) 0.028(3) 0.046(4) -0.005(3) 0.006(3) 0.008(3) C9 0.026(3) 0.021(3) 0.041(4) -0.001(3) 0.004(3) -0.001(3) C10 0.036(4) 0.038(4) 0.034(4) 0.007(3) 0.000(3) 0.013(3) C11 0.067(6) 0.050(5) 0.059(5) 0.019(4) 0.015(5) 0.017(4) C12 0.041(5) 0.083(7) 0.058(5) 0.012(5) -0.002(4) 0.010(5) C13 0.029(3) 0.028(3) 0.030(4) -0.010(3) 0.000(3) 0.005(3) C14 0.027(3) 0.031(3) 0.031(4) -0.013(3) 0.005(3) -0.001(3) C15 0.031(4) 0.021(3) 0.035(4) -0.005(3) 0.008(3) 0.005(3) C16 0.038(4) 0.025(3) 0.031(4) -0.007(3) 0.016(3) 0.006(3) C17 0.038(4) 0.029(3) 0.021(3) -0.003(3) 0.006(3) 0.013(3) C18 0.036(4) 0.054(5) 0.050(5) -0.022(4) -0.009(4) 0.000(4) C19 0.042(4) 0.032(4) 0.053(5) -0.003(3) 0.004(4) -0.003(3) C20 0.033(4) 0.038(4) 0.038(4) -0.001(3) 0.001(3) 0.013(3) C21 0.042(4) 0.042(4) 0.044(4) -0.009(3) 0.018(4) -0.002(3) C22 0.076(6) 0.059(5) 0.028(4) 0.005(4) 0.016(4) 0.034(4) C23 0.025(3) 0.032(3) 0.028(4) 0.004(3) 0.010(3) 0.009(3) C24 0.031(4) 0.035(4) 0.034(4) 0.000(3) 0.011(3) -0.001(3) C25 0.042(4) 0.028(4) 0.041(4) 0.001(3) 0.011(3) 0.011(3) C26 0.024(3) 0.038(4) 0.029(4) -0.003(3) 0.007(3) 0.004(3) C27 0.023(3) 0.040(4) 0.020(3) -0.002(3) -0.003(3) -0.004(3) C28 0.035(4) 0.033(4) 0.019(3) 0.002(3) 0.003(3) 0.001(3) C29 0.032(4) 0.032(4) 0.054(5) -0.007(3) 0.010(3) -0.001(3) C30 0.046(5) 0.052(5) 0.069(6) 0.001(4) 0.019(4) -0.015(4) C31 0.044(5) 0.073(6) 0.062(6) -0.016(5) 0.013(4) -0.023(4) C32 0.031(4) 0.032(4) 0.041(4) -0.008(3) 0.004(3) -0.004(3) C33 0.067(5) 0.039(4) 0.047(5) -0.008(4) 0.004(4) -0.001(4) C34 0.044(4) 0.040(4) 0.087(6) -0.005(4) 0.018(4) 0.003(4) _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 C1 1.993(6) . ? Rh1 C5 2.048(6) . ? Rh1 C13 2.161(6) . ? Rh1 C14 2.188(6) . ? Rh1 C17 2.231(6) . ? Rh1 C15 2.271(6) . ? Rh1 C16 2.276(5) . ? Rh1 I1 2.6756(9) . ? N1 C1 1.342(7) . ? N1 C2 1.381(7) . ? N1 C10 1.479(8) . ? N2 C1 1.357(7) . ? N2 C3 1.399(7) . ? N2 C4 1.401(7) . ? N3 C9 1.419(7) . ? N3 C23 1.425(7) . ? N3 H3 0.7946 . ? C2 C3 1.334(9) . ? C2 H2 0.9500 . ? C3 H3A 0.9500 . ? C4 C5 1.398(7) . ? C4 C9 1.408(8) . ? C5 C6 1.379(8) . ? C6 C7 1.394(8) . ? C6 H6 0.9500 . ? C7 C8 1.377(8) . ? C7 H7 0.9500 . ? C8 C9 1.386(9) . ? C8 H8 0.9500 . ? C10 C12 1.498(10) . ? C10 C11 1.521(9) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.438(9) . ? C13 C17 1.448(8) . ? C13 C18 1.487(8) . ? C14 C15 1.411(8) . ? C14 C19 1.506(8) . ? C15 C16 1.440(8) . ? C15 C20 1.483(9) . ? C16 C17 1.404(9) . ? C16 C21 1.484(8) . ? C17 C22 1.501(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.388(8) . ? C23 C28 1.414(8) . ? C24 C25 1.397(8) . ? C24 C29 1.510(9) . ? C25 C26 1.370(9) . ? C25 H25 0.9500 . ? C26 C27 1.392(8) . ? C26 H26 0.9500 . ? C27 C28 1.378(8) . ? C27 H27 0.9500 . ? C28 C32 1.522(8) . ? C29 C30 1.518(9) . ? C29 C31 1.519(10) . ? C29 H29 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C34 1.507(9) . ? C32 C33 1.516(9) . ? C32 H32 1.0000 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 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 C1 Rh1 C5 78.2(2) . . ? C1 Rh1 C13 119.3(2) . . ? C5 Rh1 C13 97.8(2) . . ? C1 Rh1 C14 100.2(2) . . ? C5 Rh1 C14 129.4(2) . . ? C13 Rh1 C14 38.6(2) . . ? C1 Rh1 C17 157.7(2) . . ? C5 Rh1 C17 100.9(2) . . ? C13 Rh1 C17 38.5(2) . . ? C14 Rh1 C17 62.8(2) . . ? C1 Rh1 C15 114.1(2) . . ? C5 Rh1 C15 160.6(2) . . ? C13 Rh1 C15 63.4(2) . . ? C14 Rh1 C15 36.8(2) . . ? C17 Rh1 C15 61.9(2) . . ? C1 Rh1 C16 149.8(2) . . ? C5 Rh1 C16 132.0(2) . . ? C13 Rh1 C16 62.8(2) . . ? C14 Rh1 C16 61.7(2) . . ? C17 Rh1 C16 36.3(2) . . ? C15 Rh1 C16 36.9(2) . . ? C1 Rh1 I1 86.03(17) . . ? C5 Rh1 I1 89.64(16) . . ? C13 Rh1 I1 154.53(16) . . ? C14 Rh1 I1 140.99(17) . . ? C17 Rh1 I1 116.26(17) . . ? C15 Rh1 I1 105.57(16) . . ? C16 Rh1 I1 94.24(17) . . ? C1 N1 C2 110.5(5) . . ? C1 N1 C10 125.4(5) . . ? C2 N1 C10 124.0(5) . . ? C1 N2 C3 109.7(5) . . ? C1 N2 C4 116.3(5) . . ? C3 N2 C4 133.7(5) . . ? C9 N3 C23 120.2(5) . . ? C9 N3 H3 110.5 . . ? C23 N3 H3 113.6 . . ? N1 C1 N2 105.6(5) . . ? N1 C1 Rh1 136.6(4) . . ? N2 C1 Rh1 117.0(4) . . ? C3 C2 N1 107.6(5) . . ? C3 C2 H2 126.2 . . ? N1 C2 H2 126.2 . . ? C2 C3 N2 106.6(5) . . ? C2 C3 H3A 126.7 . . ? N2 C3 H3A 126.7 . . ? C5 C4 N2 112.8(5) . . ? C5 C4 C9 122.4(6) . . ? N2 C4 C9 124.7(5) . . ? C6 C5 C4 117.3(5) . . ? C6 C5 Rh1 127.2(4) . . ? C4 C5 Rh1 115.3(4) . . ? C5 C6 C7 121.3(5) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C8 C7 C6 120.4(6) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C7 C8 C9 120.6(5) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C8 C9 C4 117.9(5) . . ? C8 C9 N3 123.0(5) . . ? C4 C9 N3 119.1(5) . . ? N1 C10 C12 110.9(6) . . ? N1 C10 C11 109.9(5) . . ? C12 C10 C11 112.8(6) . . ? N1 C10 H10 107.7 . . ? C12 C10 H10 107.7 . . ? C11 C10 H10 107.7 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C17 106.0(5) . . ? C14 C13 C18 126.9(6) . . ? C17 C13 C18 126.6(6) . . ? C14 C13 Rh1 71.7(3) . . ? C17 C13 Rh1 73.4(4) . . ? C18 C13 Rh1 126.0(4) . . ? C15 C14 C13 109.8(5) . . ? C15 C14 C19 126.8(6) . . ? C13 C14 C19 122.9(6) . . ? C15 C14 Rh1 74.8(3) . . ? C13 C14 Rh1 69.7(3) . . ? C19 C14 Rh1 128.1(4) . . ? C14 C15 C16 106.8(6) . . ? C14 C15 C20 129.3(6) . . ? C16 C15 C20 123.4(6) . . ? C14 C15 Rh1 68.4(3) . . ? C16 C15 Rh1 71.7(3) . . ? C20 C15 Rh1 131.1(4) . . ? C17 C16 C15 108.9(5) . . ? C17 C16 C21 126.8(6) . . ? C15 C16 C21 124.1(6) . . ? C17 C16 Rh1 70.1(3) . . ? C15 C16 Rh1 71.3(3) . . ? C21 C16 Rh1 128.4(4) . . ? C16 C17 C13 108.5(5) . . ? C16 C17 C22 126.5(6) . . ? C13 C17 C22 124.4(6) . . ? C16 C17 Rh1 73.6(3) . . ? C13 C17 Rh1 68.2(3) . . ? C22 C17 Rh1 130.7(4) . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C28 121.8(6) . . ? C24 C23 N3 118.2(6) . . ? C28 C23 N3 119.9(6) . . ? C23 C24 C25 118.4(6) . . ? C23 C24 C29 122.7(6) . . ? C25 C24 C29 118.9(6) . . ? C26 C25 C24 120.6(6) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C27 120.4(6) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C28 C27 C26 121.2(6) . . ? C28 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C27 C28 C23 117.6(6) . . ? C27 C28 C32 121.2(6) . . ? C23 C28 C32 121.2(5) . . ? C24 C29 C30 113.6(6) . . ? C24 C29 C31 109.6(5) . . ? C30 C29 C31 111.2(6) . . ? C24 C29 H29 107.4 . . ? C30 C29 H29 107.4 . . ? C31 C29 H29 107.4 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C34 C32 C33 110.4(6) . . ? C34 C32 C28 113.8(5) . . ? C33 C32 C28 111.4(5) . . ? C34 C32 H32 106.9 . . ? C33 C32 H32 106.9 . . ? C28 C32 H32 106.9 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 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 C2 N1 C1 N2 -1.9(7) . . . . ? C10 N1 C1 N2 -178.2(5) . . . . ? C2 N1 C1 Rh1 167.0(5) . . . . ? C10 N1 C1 Rh1 -9.4(10) . . . . ? C3 N2 C1 N1 2.5(7) . . . . ? C4 N2 C1 N1 176.5(5) . . . . ? C3 N2 C1 Rh1 -169.0(4) . . . . ? C4 N2 C1 Rh1 5.0(7) . . . . ? C5 Rh1 C1 N1 -169.7(7) . . . . ? C13 Rh1 C1 N1 97.9(6) . . . . ? C14 Rh1 C1 N1 61.9(7) . . . . ? C17 Rh1 C1 N1 100.3(8) . . . . ? C15 Rh1 C1 N1 26.1(7) . . . . ? C16 Rh1 C1 N1 12.4(9) . . . . ? I1 Rh1 C1 N1 -79.2(6) . . . . ? C5 Rh1 C1 N2 -1.7(4) . . . . ? C13 Rh1 C1 N2 -94.2(5) . . . . ? C14 Rh1 C1 N2 -130.1(4) . . . . ? C17 Rh1 C1 N2 -91.7(7) . . . . ? C15 Rh1 C1 N2 -166.0(4) . . . . ? C16 Rh1 C1 N2 -179.7(4) . . . . ? I1 Rh1 C1 N2 88.7(4) . . . . ? C1 N1 C2 C3 0.6(7) . . . . ? C10 N1 C2 C3 177.0(6) . . . . ? N1 C2 C3 N2 1.0(7) . . . . ? C1 N2 C3 C2 -2.2(7) . . . . ? C4 N2 C3 C2 -174.7(6) . . . . ? C1 N2 C4 C5 -6.4(7) . . . . ? C3 N2 C4 C5 165.8(6) . . . . ? C1 N2 C4 C9 170.7(6) . . . . ? C3 N2 C4 C9 -17.1(10) . . . . ? N2 C4 C5 C6 -178.2(5) . . . . ? C9 C4 C5 C6 4.6(9) . . . . ? N2 C4 C5 Rh1 4.9(6) . . . . ? C9 C4 C5 Rh1 -172.3(5) . . . . ? C1 Rh1 C5 C6 -178.4(6) . . . . ? C13 Rh1 C5 C6 -59.9(6) . . . . ? C14 Rh1 C5 C6 -84.7(6) . . . . ? C17 Rh1 C5 C6 -21.1(6) . . . . ? C15 Rh1 C5 C6 -46.7(10) . . . . ? C16 Rh1 C5 C6 0.3(7) . . . . ? I1 Rh1 C5 C6 95.6(5) . . . . ? C1 Rh1 C5 C4 -1.8(4) . . . . ? C13 Rh1 C5 C4 116.6(4) . . . . ? C14 Rh1 C5 C4 91.8(5) . . . . ? C17 Rh1 C5 C4 155.5(4) . . . . ? C15 Rh1 C5 C4 129.8(6) . . . . ? C16 Rh1 C5 C4 176.8(4) . . . . ? I1 Rh1 C5 C4 -87.8(4) . . . . ? C4 C5 C6 C7 -1.9(9) . . . . ? Rh1 C5 C6 C7 174.5(5) . . . . ? C5 C6 C7 C8 -1.0(9) . . . . ? C6 C7 C8 C9 1.5(9) . . . . ? C7 C8 C9 C4 1.1(9) . . . . ? C7 C8 C9 N3 -177.7(5) . . . . ? C5 C4 C9 C8 -4.2(9) . . . . ? N2 C4 C9 C8 179.0(5) . . . . ? C5 C4 C9 N3 174.6(5) . . . . ? N2 C4 C9 N3 -2.2(9) . . . . ? C23 N3 C9 C8 -3.6(9) . . . . ? C23 N3 C9 C4 177.7(6) . . . . ? C1 N1 C10 C12 112.4(7) . . . . ? C2 N1 C10 C12 -63.4(8) . . . . ? C1 N1 C10 C11 -122.2(7) . . . . ? C2 N1 C10 C11 62.0(8) . . . . ? C1 Rh1 C13 C14 -67.8(4) . . . . ? C5 Rh1 C13 C14 -148.7(3) . . . . ? C17 Rh1 C13 C14 113.6(5) . . . . ? C15 Rh1 C13 C14 36.2(3) . . . . ? C16 Rh1 C13 C14 77.8(4) . . . . ? I1 Rh1 C13 C14 105.4(4) . . . . ? C1 Rh1 C13 C17 178.5(3) . . . . ? C5 Rh1 C13 C17 97.7(4) . . . . ? C14 Rh1 C13 C17 -113.6(5) . . . . ? C15 Rh1 C13 C17 -77.5(4) . . . . ? C16 Rh1 C13 C17 -35.9(3) . . . . ? I1 Rh1 C13 C17 -8.2(6) . . . . ? C1 Rh1 C13 C18 55.0(6) . . . . ? C5 Rh1 C13 C18 -25.9(6) . . . . ? C14 Rh1 C13 C18 122.8(7) . . . . ? C17 Rh1 C13 C18 -123.6(7) . . . . ? C15 Rh1 C13 C18 159.0(7) . . . . ? C16 Rh1 C13 C18 -159.4(7) . . . . ? I1 Rh1 C13 C18 -131.8(5) . . . . ? C17 C13 C14 C15 1.4(6) . . . . ? C18 C13 C14 C15 173.7(6) . . . . ? Rh1 C13 C14 C15 -64.5(4) . . . . ? C17 C13 C14 C19 -171.2(5) . . . . ? C18 C13 C14 C19 1.2(9) . . . . ? Rh1 C13 C14 C19 122.9(6) . . . . ? C17 C13 C14 Rh1 65.9(4) . . . . ? C18 C13 C14 Rh1 -121.8(6) . . . . ? C1 Rh1 C14 C15 -116.8(4) . . . . ? C5 Rh1 C14 C15 160.1(3) . . . . ? C13 Rh1 C14 C15 118.3(5) . . . . ? C17 Rh1 C14 C15 78.5(4) . . . . ? C16 Rh1 C14 C15 37.3(4) . . . . ? I1 Rh1 C14 C15 -20.5(5) . . . . ? C1 Rh1 C14 C13 124.8(4) . . . . ? C5 Rh1 C14 C13 41.8(4) . . . . ? C17 Rh1 C14 C13 -39.8(3) . . . . ? C15 Rh1 C14 C13 -118.3(5) . . . . ? C16 Rh1 C14 C13 -81.0(4) . . . . ? I1 Rh1 C14 C13 -138.8(3) . . . . ? C1 Rh1 C14 C19 8.3(6) . . . . ? C5 Rh1 C14 C19 -74.8(7) . . . . ? C13 Rh1 C14 C19 -116.5(7) . . . . ? C17 Rh1 C14 C19 -156.3(7) . . . . ? C15 Rh1 C14 C19 125.2(8) . . . . ? C16 Rh1 C14 C19 162.5(7) . . . . ? I1 Rh1 C14 C19 104.7(6) . . . . ? C13 C14 C15 C16 -0.5(7) . . . . ? C19 C14 C15 C16 171.7(6) . . . . ? Rh1 C14 C15 C16 -61.8(4) . . . . ? C13 C14 C15 C20 -172.6(6) . . . . ? C19 C14 C15 C20 -0.4(10) . . . . ? Rh1 C14 C15 C20 126.1(6) . . . . ? C13 C14 C15 Rh1 61.3(4) . . . . ? C19 C14 C15 Rh1 -126.5(6) . . . . ? C1 Rh1 C15 C14 74.1(4) . . . . ? C5 Rh1 C15 C14 -52.6(8) . . . . ? C13 Rh1 C15 C14 -37.9(4) . . . . ? C17 Rh1 C15 C14 -81.4(4) . . . . ? C16 Rh1 C15 C14 -117.3(5) . . . . ? I1 Rh1 C15 C14 166.8(3) . . . . ? C1 Rh1 C15 C16 -168.6(4) . . . . ? C5 Rh1 C15 C16 64.7(8) . . . . ? C13 Rh1 C15 C16 79.4(4) . . . . ? C14 Rh1 C15 C16 117.3(5) . . . . ? C17 Rh1 C15 C16 35.9(4) . . . . ? I1 Rh1 C15 C16 -75.9(4) . . . . ? C1 Rh1 C15 C20 -49.7(6) . . . . ? C5 Rh1 C15 C20 -176.5(6) . . . . ? C13 Rh1 C15 C20 -161.8(7) . . . . ? C14 Rh1 C15 C20 -123.9(7) . . . . ? C17 Rh1 C15 C20 154.7(6) . . . . ? C16 Rh1 C15 C20 118.8(7) . . . . ? I1 Rh1 C15 C20 42.9(6) . . . . ? C14 C15 C16 C17 -0.6(7) . . . . ? C20 C15 C16 C17 172.0(5) . . . . ? Rh1 C15 C16 C17 -60.3(4) . . . . ? C14 C15 C16 C21 -176.0(5) . . . . ? C20 C15 C16 C21 -3.4(9) . . . . ? Rh1 C15 C16 C21 124.3(6) . . . . ? C14 C15 C16 Rh1 59.7(4) . . . . ? C20 C15 C16 Rh1 -127.7(6) . . . . ? C1 Rh1 C16 C17 140.2(5) . . . . ? C5 Rh1 C16 C17 -37.1(5) . . . . ? C13 Rh1 C16 C17 38.0(4) . . . . ? C14 Rh1 C16 C17 81.8(4) . . . . ? C15 Rh1 C16 C17 119.1(5) . . . . ? I1 Rh1 C16 C17 -130.5(3) . . . . ? C1 Rh1 C16 C15 21.1(7) . . . . ? C5 Rh1 C16 C15 -156.2(4) . . . . ? C13 Rh1 C16 C15 -81.1(4) . . . . ? C14 Rh1 C16 C15 -37.3(4) . . . . ? C17 Rh1 C16 C15 -119.1(5) . . . . ? I1 Rh1 C16 C15 110.4(4) . . . . ? C1 Rh1 C16 C21 -98.1(7) . . . . ? C5 Rh1 C16 C21 84.6(7) . . . . ? C13 Rh1 C16 C21 159.7(7) . . . . ? C14 Rh1 C16 C21 -156.4(7) . . . . ? C17 Rh1 C16 C21 121.7(8) . . . . ? C15 Rh1 C16 C21 -119.2(8) . . . . ? I1 Rh1 C16 C21 -8.7(6) . . . . ? C15 C16 C17 C13 1.5(7) . . . . ? C21 C16 C17 C13 176.8(6) . . . . ? Rh1 C16 C17 C13 -59.5(4) . . . . ? C15 C16 C17 C22 -170.0(6) . . . . ? C21 C16 C17 C22 5.3(10) . . . . ? Rh1 C16 C17 C22 129.0(6) . . . . ? C15 C16 C17 Rh1 61.1(4) . . . . ? C21 C16 C17 Rh1 -123.7(6) . . . . ? C14 C13 C17 C16 -1.8(6) . . . . ? C18 C13 C17 C16 -174.1(6) . . . . ? Rh1 C13 C17 C16 63.0(4) . . . . ? C14 C13 C17 C22 169.9(5) . . . . ? C18 C13 C17 C22 -2.4(10) . . . . ? Rh1 C13 C17 C22 -125.3(6) . . . . ? C14 C13 C17 Rh1 -64.8(4) . . . . ? C18 C13 C17 Rh1 122.9(6) . . . . ? C1 Rh1 C17 C16 -121.7(6) . . . . ? C5 Rh1 C17 C16 152.8(4) . . . . ? C13 Rh1 C17 C16 -118.3(5) . . . . ? C14 Rh1 C17 C16 -78.3(4) . . . . ? C15 Rh1 C17 C16 -36.5(4) . . . . ? I1 Rh1 C17 C16 57.8(4) . . . . ? C1 Rh1 C17 C13 -3.4(8) . . . . ? C5 Rh1 C17 C13 -88.9(4) . . . . ? C14 Rh1 C17 C13 40.0(3) . . . . ? C15 Rh1 C17 C13 81.7(4) . . . . ? C16 Rh1 C17 C13 118.3(5) . . . . ? I1 Rh1 C17 C13 176.1(3) . . . . ? C1 Rh1 C17 C22 113.9(8) . . . . ? C5 Rh1 C17 C22 28.4(7) . . . . ? C13 Rh1 C17 C22 117.3(8) . . . . ? C14 Rh1 C17 C22 157.3(7) . . . . ? C15 Rh1 C17 C22 -160.9(7) . . . . ? C16 Rh1 C17 C22 -124.4(8) . . . . ? I1 Rh1 C17 C22 -66.6(7) . . . . ? C9 N3 C23 C24 -72.7(8) . . . . ? C9 N3 C23 C28 110.0(6) . . . . ? C28 C23 C24 C25 -2.6(9) . . . . ? N3 C23 C24 C25 -179.9(6) . . . . ? C28 C23 C24 C29 174.8(6) . . . . ? N3 C23 C24 C29 -2.5(9) . . . . ? C23 C24 C25 C26 1.2(10) . . . . ? C29 C24 C25 C26 -176.3(6) . . . . ? C24 C25 C26 C27 0.4(10) . . . . ? C25 C26 C27 C28 -0.7(9) . . . . ? C26 C27 C28 C23 -0.7(9) . . . . ? C26 C27 C28 C32 -178.7(5) . . . . ? C24 C23 C28 C27 2.3(9) . . . . ? N3 C23 C28 C27 179.5(5) . . . . ? C24 C23 C28 C32 -179.7(6) . . . . ? N3 C23 C28 C32 -2.5(9) . . . . ? C23 C24 C29 C30 129.8(7) . . . . ? C25 C24 C29 C30 -52.8(8) . . . . ? C23 C24 C29 C31 -105.1(7) . . . . ? C25 C24 C29 C31 72.2(8) . . . . ? C27 C28 C32 C34 -27.5(9) . . . . ? C23 C28 C32 C34 154.5(6) . . . . ? C27 C28 C32 C33 98.1(7) . . . . ? C23 C28 C32 C33 -79.8(8) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.034 _refine_diff_density_min -1.294 _refine_diff_density_rms 0.186 #===END data_10110 _database_code_depnum_ccdc_archive 'CCDC 823382' #TrackingRef '- Paper#2 cif files.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Cp*Ir(C,C)I (4)' _chemical_melting_point ? _chemical_formula_moiety 'C34 H45 I Ir N3' _chemical_formula_sum 'C34 H45 I Ir N3' _chemical_formula_weight 814.83 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' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.219(4) _cell_length_b 8.444(3) _cell_length_c 29.021(9) _cell_angle_alpha 90.00 _cell_angle_beta 95.654(5) _cell_angle_gamma 90.00 _cell_volume 3223.7(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 972 _cell_measurement_theta_min 2.513 _cell_measurement_theta_max 24.662 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 5.126 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.587 _exptl_absorpt_correction_T_max 0.831 _exptl_absorpt_process_details ; absorption correction based on 12443 reflections(SADABS);Rint 0.1247 before correction and 0.0411 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24406 _diffrn_reflns_av_R_equivalents 0.0652 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6341 _reflns_number_gt 5231 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. ; _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^)+(0.0777P)^2^+4.6714P] 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_number_reflns 6341 _refine_ls_number_parameters 363 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1370 _refine_ls_wR_factor_gt 0.1305 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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 0.32155(2) 0.26045(3) 0.077853(10) 0.01817(12) Uani 1 1 d . . . I1 I 0.44298(5) 0.48574(7) 0.11697(2) 0.04121(19) Uani 1 1 d . . . N1 N 0.0050(5) 0.5019(8) 0.1555(2) 0.0281(15) Uani 1 1 d . . . H1 H 0.0006 0.4242 0.1647 0.034 Uiso 1 1 d R . . N2 N 0.1941(5) 0.3321(7) 0.1510(2) 0.0204(13) Uani 1 1 d . . . N3 N 0.3056(5) 0.1669(8) 0.1806(2) 0.0263(15) Uani 1 1 d . . . C1 C 0.2745(6) 0.2394(8) 0.1402(3) 0.0220(17) Uani 1 1 d . . . C2 C 0.1815(6) 0.3212(10) 0.1979(3) 0.0283(18) Uani 1 1 d . . . H2 H 0.1335 0.3771 0.2140 0.034 Uiso 1 1 calc R . . C3 C 0.2501(7) 0.2172(11) 0.2158(3) 0.033(2) Uani 1 1 d . . . H3 H 0.2592 0.1836 0.2472 0.040 Uiso 1 1 calc R . . C4 C 0.1505(6) 0.4261(8) 0.1143(3) 0.0201(16) Uani 1 1 d . . . C5 C 0.2035(5) 0.4183(8) 0.0746(3) 0.0194(16) Uani 1 1 d . . . C6 C 0.1691(6) 0.5126(8) 0.0382(2) 0.0211(16) Uani 1 1 d . . . H6 H 0.2060 0.5166 0.0118 0.025 Uiso 1 1 calc R . . C7 C 0.0791(6) 0.6053(9) 0.0390(3) 0.0266(18) Uani 1 1 d . . . H7 H 0.0560 0.6684 0.0130 0.032 Uiso 1 1 calc R . . C8 C 0.0261(6) 0.6034(9) 0.0771(3) 0.0252(17) Uani 1 1 d . . . H8 H -0.0342 0.6646 0.0771 0.030 Uiso 1 1 calc R . . C9 C 0.0592(5) 0.5131(9) 0.1158(3) 0.0227(16) Uani 1 1 d . . . C10 C 0.3931(7) 0.0567(11) 0.1872(3) 0.036(2) Uani 1 1 d . . . H10 H 0.4179 0.0388 0.1562 0.043 Uiso 1 1 calc R . . C11 C 0.4791(8) 0.1307(15) 0.2179(4) 0.059(3) Uani 1 1 d . . . H11A H 0.4941 0.2359 0.2061 0.089 Uiso 1 1 calc R . . H11B H 0.5397 0.0637 0.2182 0.089 Uiso 1 1 calc R . . H11C H 0.4594 0.1406 0.2495 0.089 Uiso 1 1 calc R . . C12 C 0.3584(9) -0.1032(12) 0.2046(4) 0.058(3) Uani 1 1 d . . . H12A H 0.3433 -0.0929 0.2369 0.087 Uiso 1 1 calc R . . H12B H 0.4125 -0.1816 0.2027 0.087 Uiso 1 1 calc R . . H12C H 0.2971 -0.1377 0.1855 0.087 Uiso 1 1 calc R . . C13 C -0.0853(6) 0.5909(9) 0.1578(3) 0.0229(17) Uani 1 1 d . . . C14 C -0.1816(6) 0.5154(9) 0.1550(3) 0.0238(17) Uani 1 1 d . . . C15 C -0.2659(6) 0.6089(9) 0.1583(3) 0.0256(17) Uani 1 1 d . . . H15 H -0.3310 0.5602 0.1564 0.031 Uiso 1 1 calc R . . C16 C -0.2593(7) 0.7714(9) 0.1644(3) 0.031(2) Uani 1 1 d . . . H16 H -0.3187 0.8337 0.1659 0.037 Uiso 1 1 calc R . . C17 C -0.1655(6) 0.8395(10) 0.1681(3) 0.0282(18) Uani 1 1 d . . . H17 H -0.1604 0.9508 0.1727 0.034 Uiso 1 1 calc R . . C18 C -0.0778(7) 0.7536(9) 0.1656(3) 0.0282(19) Uani 1 1 d . . . C19 C 0.0269(6) 0.8349(10) 0.1736(3) 0.032(2) Uani 1 1 d . . . H19 H 0.0796 0.7579 0.1652 0.038 Uiso 1 1 calc R . . C20 C 0.0490(8) 0.8747(13) 0.2246(3) 0.049(3) Uani 1 1 d . . . H20A H -0.0095 0.9299 0.2354 0.074 Uiso 1 1 calc R . . H20B H 0.1091 0.9431 0.2290 0.074 Uiso 1 1 calc R . . H20C H 0.0617 0.7769 0.2424 0.074 Uiso 1 1 calc R . . C21 C 0.0322(8) 0.9813(12) 0.1428(4) 0.049(3) Uani 1 1 d . . . H21A H 0.0150 0.9514 0.1103 0.074 Uiso 1 1 calc R . . H21B H 0.1012 1.0252 0.1467 0.074 Uiso 1 1 calc R . . H21C H -0.0162 1.0610 0.1516 0.074 Uiso 1 1 calc R . . C22 C -0.1905(6) 0.3381(10) 0.1467(3) 0.0298(19) Uani 1 1 d . . . H22 H -0.1302 0.2877 0.1644 0.036 Uiso 1 1 calc R . . C23 C -0.1853(9) 0.2983(12) 0.0963(4) 0.048(3) Uani 1 1 d . . . H23A H -0.1828 0.1831 0.0926 0.073 Uiso 1 1 calc R . . H23B H -0.1240 0.3457 0.0856 0.073 Uiso 1 1 calc R . . H23C H -0.2455 0.3404 0.0780 0.073 Uiso 1 1 calc R . . C24 C -0.2834(8) 0.2657(10) 0.1640(4) 0.046(3) Uani 1 1 d . . . H24A H -0.2831 0.2860 0.1973 0.070 Uiso 1 1 calc R . . H24B H -0.2833 0.1512 0.1585 0.070 Uiso 1 1 calc R . . H24C H -0.3444 0.3127 0.1475 0.070 Uiso 1 1 calc R . . C25 C 0.4317(6) 0.1901(9) 0.0257(3) 0.0257(17) Uani 1 1 d . . . C26 C 0.3322(7) 0.2147(10) 0.0020(3) 0.0292(19) Uani 1 1 d . . . C27 C 0.2638(6) 0.1063(9) 0.0215(3) 0.0272(18) Uani 1 1 d . . . C28 C 0.3231(6) 0.0114(8) 0.0559(3) 0.0242(17) Uani 1 1 d . . . C29 C 0.4269(6) 0.0658(9) 0.0582(3) 0.0238(17) Uani 1 1 d . . . C30 C 0.5266(7) 0.2760(10) 0.0160(3) 0.036(2) Uani 1 1 d . . . H30A H 0.5608 0.3173 0.0450 0.055 Uiso 1 1 calc R . . H30B H 0.5089 0.3641 -0.0053 0.055 Uiso 1 1 calc R . . H30C H 0.5721 0.2029 0.0019 0.055 Uiso 1 1 calc R . . C31 C 0.3084(8) 0.3190(12) -0.0392(3) 0.046(3) Uani 1 1 d . . . H31A H 0.3178 0.2594 -0.0675 0.069 Uiso 1 1 calc R . . H31B H 0.3539 0.4108 -0.0370 0.069 Uiso 1 1 calc R . . H31C H 0.2377 0.3551 -0.0403 0.069 Uiso 1 1 calc R . . C32 C 0.1561(7) 0.0829(12) 0.0043(4) 0.047(3) Uani 1 1 d . . . H32A H 0.1282 0.1820 -0.0092 0.070 Uiso 1 1 calc R . . H32B H 0.1177 0.0512 0.0300 0.070 Uiso 1 1 calc R . . H32C H 0.1508 -0.0001 -0.0194 0.070 Uiso 1 1 calc R . . C33 C 0.2867(7) -0.1310(10) 0.0802(3) 0.040(2) Uani 1 1 d . . . H33A H 0.3148 -0.2269 0.0673 0.060 Uiso 1 1 calc R . . H33B H 0.2123 -0.1352 0.0758 0.060 Uiso 1 1 calc R . . H33C H 0.3092 -0.1240 0.1133 0.060 Uiso 1 1 calc R . . C34 C 0.5192(6) -0.0085(10) 0.0843(3) 0.0320(19) Uani 1 1 d . . . H34A H 0.5703 -0.0304 0.0629 0.048 Uiso 1 1 calc R . . H34B H 0.4996 -0.1078 0.0985 0.048 Uiso 1 1 calc R . . H34C H 0.5476 0.0643 0.1085 0.048 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 0.01804(17) 0.01778(17) 0.01883(18) -0.00172(11) 0.00253(12) 0.00238(11) I1 0.0364(3) 0.0381(4) 0.0488(4) -0.0035(3) 0.0028(3) -0.0033(3) N1 0.029(4) 0.026(4) 0.032(4) 0.005(3) 0.012(3) 0.003(3) N2 0.018(3) 0.024(3) 0.020(3) -0.003(3) 0.005(3) 0.001(3) N3 0.027(4) 0.032(4) 0.021(4) -0.001(3) 0.004(3) 0.006(3) C1 0.018(4) 0.023(4) 0.025(4) -0.006(3) 0.000(3) 0.001(3) C2 0.025(4) 0.040(5) 0.021(4) -0.002(4) 0.008(3) 0.005(4) C3 0.030(5) 0.045(5) 0.024(4) 0.002(4) 0.004(4) -0.001(4) C4 0.021(4) 0.020(4) 0.019(4) -0.002(3) 0.001(3) -0.001(3) C5 0.015(4) 0.018(4) 0.025(4) -0.005(3) -0.001(3) 0.001(3) C6 0.029(4) 0.021(4) 0.014(4) 0.000(3) 0.006(3) 0.009(3) C7 0.023(4) 0.024(4) 0.031(5) 0.002(3) -0.008(4) 0.005(3) C8 0.020(4) 0.027(4) 0.029(4) -0.002(3) -0.001(3) 0.004(3) C9 0.012(3) 0.027(4) 0.028(4) -0.008(3) 0.001(3) -0.001(3) C10 0.034(5) 0.045(5) 0.029(5) 0.011(4) 0.005(4) 0.010(4) C11 0.035(6) 0.097(9) 0.045(7) 0.016(6) 0.001(5) 0.017(6) C12 0.074(8) 0.053(7) 0.050(7) 0.024(5) 0.024(6) 0.027(6) C13 0.024(4) 0.023(4) 0.024(4) -0.002(3) 0.012(3) 0.003(3) C14 0.025(4) 0.026(4) 0.021(4) 0.002(3) 0.003(3) 0.004(3) C15 0.021(4) 0.032(4) 0.024(4) -0.007(3) 0.002(3) -0.004(3) C16 0.033(5) 0.028(4) 0.033(5) 0.002(4) 0.013(4) 0.010(4) C17 0.029(4) 0.025(4) 0.031(5) -0.004(3) 0.005(4) 0.007(3) C18 0.029(5) 0.028(4) 0.029(5) -0.003(3) 0.012(4) -0.006(3) C19 0.025(4) 0.025(4) 0.046(5) -0.007(4) 0.007(4) 0.000(4) C20 0.047(6) 0.057(7) 0.045(6) -0.006(5) 0.010(5) -0.022(5) C21 0.044(6) 0.049(6) 0.058(7) 0.004(5) 0.021(5) -0.007(5) C22 0.026(4) 0.029(4) 0.036(5) -0.004(4) 0.009(4) -0.001(4) C23 0.063(7) 0.035(5) 0.046(6) -0.008(5) -0.003(5) 0.001(5) C24 0.039(6) 0.034(5) 0.069(8) -0.003(5) 0.015(5) -0.011(4) C25 0.031(4) 0.022(4) 0.026(4) -0.005(3) 0.011(4) 0.008(3) C26 0.037(5) 0.032(4) 0.019(4) -0.005(3) 0.004(4) 0.010(4) C27 0.027(4) 0.028(4) 0.026(4) -0.015(3) -0.003(4) 0.002(3) C28 0.026(4) 0.012(3) 0.034(4) -0.014(3) -0.001(3) 0.003(3) C29 0.025(4) 0.026(4) 0.021(4) -0.007(3) 0.003(3) 0.005(3) C30 0.032(5) 0.039(5) 0.041(5) -0.008(4) 0.018(4) 0.008(4) C31 0.066(7) 0.051(6) 0.023(5) 0.003(4) 0.013(5) 0.029(5) C32 0.027(5) 0.053(6) 0.058(7) -0.024(5) -0.005(5) 0.001(4) C33 0.044(5) 0.028(5) 0.050(6) -0.011(4) 0.009(5) -0.014(4) C34 0.029(4) 0.030(4) 0.036(5) 0.000(4) -0.003(4) 0.012(4) _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 C1 1.978(8) . ? Ir1 C5 2.048(7) . ? Ir1 C27 2.169(7) . ? Ir1 C28 2.198(7) . ? Ir1 C26 2.253(8) . ? Ir1 C29 2.264(7) . ? Ir1 C25 2.280(7) . ? Ir1 I1 2.6693(8) . ? N1 C13 1.417(9) . ? N1 C9 1.418(10) . ? N1 H1 0.7123 . ? N2 C1 1.380(9) . ? N2 C2 1.391(10) . ? N2 C4 1.404(9) . ? N3 C1 1.351(10) . ? N3 C3 1.382(10) . ? N3 C10 1.482(10) . ? C2 C3 1.331(12) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C5 1.408(10) . ? C4 C9 1.418(10) . ? C5 C6 1.365(10) . ? C6 C7 1.426(10) . ? C6 H6 0.9500 . ? C7 C8 1.366(11) . ? C7 H7 0.9500 . ? C8 C9 1.394(11) . ? C8 H8 0.9500 . ? C10 C11 1.509(14) . ? C10 C12 1.529(13) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C18 1.395(10) . ? C13 C14 1.419(11) . ? C14 C15 1.377(10) . ? C14 C22 1.519(11) . ? C15 C16 1.385(11) . ? C15 H15 0.9500 . ? C16 C17 1.361(12) . ? C16 H16 0.9500 . ? C17 C18 1.376(11) . ? C17 H17 0.9500 . ? C18 C19 1.542(11) . ? C19 C20 1.520(13) . ? C19 C21 1.531(13) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.501(12) . ? C22 C23 1.510(13) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C29 1.417(11) . ? C25 C26 1.438(12) . ? C25 C30 1.499(12) . ? C26 C27 1.441(12) . ? C26 C31 1.494(12) . ? C27 C28 1.450(11) . ? C27 C32 1.475(11) . ? C28 C29 1.443(11) . ? C28 C33 1.496(11) . ? C29 C34 1.508(11) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 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 C1 Ir1 C5 78.1(3) . . ? C1 Ir1 C27 121.1(3) . . ? C5 Ir1 C27 98.4(3) . . ? C1 Ir1 C28 101.0(3) . . ? C5 Ir1 C28 129.7(3) . . ? C27 Ir1 C28 38.8(3) . . ? C1 Ir1 C26 159.0(3) . . ? C5 Ir1 C26 100.8(3) . . ? C27 Ir1 C26 38.0(3) . . ? C28 Ir1 C26 63.2(3) . . ? C1 Ir1 C29 115.0(3) . . ? C5 Ir1 C29 161.2(3) . . ? C27 Ir1 C29 63.5(3) . . ? C28 Ir1 C29 37.7(3) . . ? C26 Ir1 C29 62.0(3) . . ? C1 Ir1 C25 149.6(3) . . ? C5 Ir1 C25 132.3(3) . . ? C27 Ir1 C25 62.8(3) . . ? C28 Ir1 C25 62.2(3) . . ? C26 Ir1 C25 37.0(3) . . ? C29 Ir1 C25 36.3(3) . . ? C1 Ir1 I1 84.6(2) . . ? C5 Ir1 I1 88.8(2) . . ? C27 Ir1 I1 154.2(2) . . ? C28 Ir1 I1 141.5(2) . . ? C26 Ir1 I1 116.4(2) . . ? C29 Ir1 I1 105.4(2) . . ? C25 Ir1 I1 94.1(2) . . ? C13 N1 C9 119.8(6) . . ? C13 N1 H1 111.8 . . ? C9 N1 H1 115.5 . . ? C1 N2 C2 110.7(6) . . ? C1 N2 C4 114.7(6) . . ? C2 N2 C4 134.3(6) . . ? C1 N3 C3 111.3(7) . . ? C1 N3 C10 124.3(7) . . ? C3 N3 C10 124.2(7) . . ? N3 C1 N2 103.6(7) . . ? N3 C1 Ir1 137.6(6) . . ? N2 C1 Ir1 118.3(6) . . ? C3 C2 N2 106.5(7) . . ? C3 C2 H2 126.7 . . ? N2 C2 H2 126.7 . . ? C2 C3 N3 107.7(8) . . ? C2 C3 H3 126.1 . . ? N3 C3 H3 126.1 . . ? N2 C4 C5 113.2(6) . . ? N2 C4 C9 123.8(7) . . ? C5 C4 C9 122.9(7) . . ? C6 C5 C4 116.9(6) . . ? C6 C5 Ir1 127.5(6) . . ? C4 C5 Ir1 115.6(5) . . ? C5 C6 C7 121.5(7) . . ? C5 C6 H6 119.2 . . ? C7 C6 H6 119.2 . . ? C8 C7 C6 120.1(7) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C7 C8 C9 121.0(7) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C8 C9 N1 123.3(7) . . ? C8 C9 C4 117.3(7) . . ? N1 C9 C4 119.4(7) . . ? N3 C10 C11 110.5(8) . . ? N3 C10 C12 109.9(7) . . ? C11 C10 C12 113.8(8) . . ? N3 C10 H10 107.5 . . ? C11 C10 H10 107.5 . . ? C12 C10 H10 107.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 N1 118.9(7) . . ? C18 C13 C14 120.1(7) . . ? N1 C13 C14 120.9(7) . . ? C15 C14 C13 117.8(7) . . ? C15 C14 C22 121.7(7) . . ? C13 C14 C22 120.5(7) . . ? C14 C15 C16 122.4(8) . . ? C14 C15 H15 118.8 . . ? C16 C15 H15 118.8 . . ? C17 C16 C15 118.3(8) . . ? C17 C16 H16 120.8 . . ? C15 C16 H16 120.8 . . ? C16 C17 C18 122.6(8) . . ? C16 C17 H17 118.7 . . ? C18 C17 H17 118.7 . . ? C17 C18 C13 118.8(8) . . ? C17 C18 C19 120.4(7) . . ? C13 C18 C19 120.7(7) . . ? C20 C19 C21 112.0(8) . . ? C20 C19 C18 109.1(7) . . ? C21 C19 C18 111.4(8) . . ? C20 C19 H19 108.1 . . ? C21 C19 H19 108.1 . . ? C18 C19 H19 108.1 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 C22 C23 110.5(8) . . ? C24 C22 C14 113.7(7) . . ? C23 C22 C14 111.2(7) . . ? C24 C22 H22 107.0 . . ? C23 C22 H22 107.0 . . ? C14 C22 H22 107.0 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C29 C25 C26 109.0(7) . . ? C29 C25 C30 125.2(8) . . ? C26 C25 C30 125.7(8) . . ? C29 C25 Ir1 71.2(4) . . ? C26 C25 Ir1 70.5(4) . . ? C30 C25 Ir1 126.9(6) . . ? C25 C26 C27 107.5(7) . . ? C25 C26 C31 125.4(8) . . ? C27 C26 C31 126.7(9) . . ? C25 C26 Ir1 72.5(5) . . ? C27 C26 Ir1 67.9(4) . . ? C31 C26 Ir1 130.8(6) . . ? C26 C27 C28 107.7(7) . . ? C26 C27 C32 125.1(8) . . ? C28 C27 C32 126.7(8) . . ? C26 C27 Ir1 74.2(5) . . ? C28 C27 Ir1 71.7(4) . . ? C32 C27 Ir1 126.3(6) . . ? C29 C28 C27 107.6(7) . . ? C29 C28 C33 125.7(7) . . ? C27 C28 C33 126.3(7) . . ? C29 C28 Ir1 73.6(4) . . ? C27 C28 Ir1 69.5(4) . . ? C33 C28 Ir1 128.3(6) . . ? C25 C29 C28 108.1(7) . . ? C25 C29 C34 123.8(7) . . ? C28 C29 C34 127.5(7) . . ? C25 C29 Ir1 72.4(4) . . ? C28 C29 Ir1 68.7(4) . . ? C34 C29 Ir1 131.5(5) . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 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 C3 N3 C1 N2 -2.6(9) . . . . ? C10 N3 C1 N2 -178.2(7) . . . . ? C3 N3 C1 Ir1 169.4(7) . . . . ? C10 N3 C1 Ir1 -6.3(13) . . . . ? C2 N2 C1 N3 3.3(8) . . . . ? C4 N2 C1 N3 177.5(6) . . . . ? C2 N2 C1 Ir1 -170.5(5) . . . . ? C4 N2 C1 Ir1 3.6(8) . . . . ? C5 Ir1 C1 N3 -171.8(9) . . . . ? C27 Ir1 C1 N3 95.5(9) . . . . ? C28 Ir1 C1 N3 59.6(9) . . . . ? C26 Ir1 C1 N3 99.1(11) . . . . ? C29 Ir1 C1 N3 22.6(9) . . . . ? C25 Ir1 C1 N3 7.0(12) . . . . ? I1 Ir1 C1 N3 -81.8(8) . . . . ? C5 Ir1 C1 N2 -0.7(6) . . . . ? C27 Ir1 C1 N2 -93.4(6) . . . . ? C28 Ir1 C1 N2 -129.3(6) . . . . ? C26 Ir1 C1 N2 -89.9(10) . . . . ? C29 Ir1 C1 N2 -166.3(5) . . . . ? C25 Ir1 C1 N2 178.0(5) . . . . ? I1 Ir1 C1 N2 89.2(5) . . . . ? C1 N2 C2 C3 -2.8(9) . . . . ? C4 N2 C2 C3 -175.4(8) . . . . ? N2 C2 C3 N3 1.2(10) . . . . ? C1 N3 C3 C2 0.9(10) . . . . ? C10 N3 C3 C2 176.6(8) . . . . ? C1 N2 C4 C5 -5.5(9) . . . . ? C2 N2 C4 C5 166.9(8) . . . . ? C1 N2 C4 C9 171.0(7) . . . . ? C2 N2 C4 C9 -16.6(13) . . . . ? N2 C4 C5 C6 -176.7(6) . . . . ? C9 C4 C5 C6 6.8(11) . . . . ? N2 C4 C5 Ir1 5.0(8) . . . . ? C9 C4 C5 Ir1 -171.5(6) . . . . ? C1 Ir1 C5 C6 179.5(7) . . . . ? C27 Ir1 C5 C6 -60.3(7) . . . . ? C28 Ir1 C5 C6 -86.0(7) . . . . ? C26 Ir1 C5 C6 -21.9(7) . . . . ? C29 Ir1 C5 C6 -44.8(13) . . . . ? C25 Ir1 C5 C6 0.4(9) . . . . ? I1 Ir1 C5 C6 94.8(7) . . . . ? C1 Ir1 C5 C4 -2.4(5) . . . . ? C27 Ir1 C5 C4 117.8(6) . . . . ? C28 Ir1 C5 C4 92.1(6) . . . . ? C26 Ir1 C5 C4 156.2(6) . . . . ? C29 Ir1 C5 C4 133.3(8) . . . . ? C25 Ir1 C5 C4 178.5(5) . . . . ? I1 Ir1 C5 C4 -87.1(5) . . . . ? C4 C5 C6 C7 -4.8(11) . . . . ? Ir1 C5 C6 C7 173.3(6) . . . . ? C5 C6 C7 C8 1.2(12) . . . . ? C6 C7 C8 C9 0.7(12) . . . . ? C7 C8 C9 N1 -177.4(7) . . . . ? C7 C8 C9 C4 1.1(11) . . . . ? C13 N1 C9 C8 -2.9(11) . . . . ? C13 N1 C9 C4 178.7(7) . . . . ? N2 C4 C9 C8 178.9(7) . . . . ? C5 C4 C9 C8 -4.9(11) . . . . ? N2 C4 C9 N1 -2.6(11) . . . . ? C5 C4 C9 N1 173.6(7) . . . . ? C1 N3 C10 C11 110.9(9) . . . . ? C3 N3 C10 C11 -64.3(11) . . . . ? C1 N3 C10 C12 -122.7(9) . . . . ? C3 N3 C10 C12 62.2(11) . . . . ? C9 N1 C13 C18 -74.1(10) . . . . ? C9 N1 C13 C14 109.6(8) . . . . ? C18 C13 C14 C15 2.5(12) . . . . ? N1 C13 C14 C15 178.9(7) . . . . ? C18 C13 C14 C22 -179.7(8) . . . . ? N1 C13 C14 C22 -3.4(11) . . . . ? C13 C14 C15 C16 -0.2(12) . . . . ? C22 C14 C15 C16 -177.9(8) . . . . ? C14 C15 C16 C17 -1.4(13) . . . . ? C15 C16 C17 C18 0.8(13) . . . . ? C16 C17 C18 C13 1.5(13) . . . . ? C16 C17 C18 C19 -175.7(8) . . . . ? N1 C13 C18 C17 -179.6(7) . . . . ? C14 C13 C18 C17 -3.2(12) . . . . ? N1 C13 C18 C19 -2.4(12) . . . . ? C14 C13 C18 C19 174.0(8) . . . . ? C17 C18 C19 C20 71.9(11) . . . . ? C13 C18 C19 C20 -105.2(9) . . . . ? C17 C18 C19 C21 -52.2(11) . . . . ? C13 C18 C19 C21 130.7(9) . . . . ? C15 C14 C22 C24 -26.8(12) . . . . ? C13 C14 C22 C24 155.5(8) . . . . ? C15 C14 C22 C23 98.7(9) . . . . ? C13 C14 C22 C23 -78.9(10) . . . . ? C1 Ir1 C25 C29 24.4(8) . . . . ? C5 Ir1 C25 C29 -157.3(4) . . . . ? C27 Ir1 C25 C29 -81.4(5) . . . . ? C28 Ir1 C25 C29 -37.5(5) . . . . ? C26 Ir1 C25 C29 -119.1(7) . . . . ? I1 Ir1 C25 C29 110.6(4) . . . . ? C1 Ir1 C25 C26 143.5(6) . . . . ? C5 Ir1 C25 C26 -38.2(6) . . . . ? C27 Ir1 C25 C26 37.7(5) . . . . ? C28 Ir1 C25 C26 81.6(5) . . . . ? C29 Ir1 C25 C26 119.1(7) . . . . ? I1 Ir1 C25 C26 -130.3(5) . . . . ? C1 Ir1 C25 C30 -96.0(9) . . . . ? C5 Ir1 C25 C30 82.3(8) . . . . ? C27 Ir1 C25 C30 158.1(8) . . . . ? C28 Ir1 C25 C30 -157.9(8) . . . . ? C26 Ir1 C25 C30 120.5(9) . . . . ? C29 Ir1 C25 C30 -120.4(10) . . . . ? I1 Ir1 C25 C30 -9.8(7) . . . . ? C29 C25 C26 C27 2.0(9) . . . . ? C30 C25 C26 C27 178.9(7) . . . . ? Ir1 C25 C26 C27 -59.1(5) . . . . ? C29 C25 C26 C31 -170.9(8) . . . . ? C30 C25 C26 C31 6.1(13) . . . . ? Ir1 C25 C26 C31 128.0(8) . . . . ? C29 C25 C26 Ir1 61.1(5) . . . . ? C30 C25 C26 Ir1 -121.9(8) . . . . ? C1 Ir1 C26 C25 -122.8(9) . . . . ? C5 Ir1 C26 C25 152.3(5) . . . . ? C27 Ir1 C26 C25 -117.9(7) . . . . ? C28 Ir1 C26 C25 -78.6(5) . . . . ? C29 Ir1 C26 C25 -35.9(5) . . . . ? I1 Ir1 C26 C25 58.2(5) . . . . ? C1 Ir1 C26 C27 -4.9(11) . . . . ? C5 Ir1 C26 C27 -89.8(5) . . . . ? C28 Ir1 C26 C27 39.4(5) . . . . ? C29 Ir1 C26 C27 82.0(5) . . . . ? C25 Ir1 C26 C27 117.9(7) . . . . ? I1 Ir1 C26 C27 176.1(4) . . . . ? C1 Ir1 C26 C31 115.2(11) . . . . ? C5 Ir1 C26 C31 30.3(10) . . . . ? C27 Ir1 C26 C31 120.1(11) . . . . ? C28 Ir1 C26 C31 159.4(10) . . . . ? C29 Ir1 C26 C31 -157.9(10) . . . . ? C25 Ir1 C26 C31 -122.0(11) . . . . ? I1 Ir1 C26 C31 -63.8(10) . . . . ? C25 C26 C27 C28 -2.2(8) . . . . ? C31 C26 C27 C28 170.5(8) . . . . ? Ir1 C26 C27 C28 -64.3(5) . . . . ? C25 C26 C27 C32 -174.3(7) . . . . ? C31 C26 C27 C32 -1.6(13) . . . . ? Ir1 C26 C27 C32 123.6(8) . . . . ? C25 C26 C27 Ir1 62.1(5) . . . . ? C31 C26 C27 Ir1 -125.2(8) . . . . ? C1 Ir1 C27 C26 177.9(5) . . . . ? C5 Ir1 C27 C26 96.9(5) . . . . ? C28 Ir1 C27 C26 -115.3(7) . . . . ? C29 Ir1 C27 C26 -77.6(5) . . . . ? C25 Ir1 C27 C26 -36.7(5) . . . . ? I1 Ir1 C27 C26 -8.1(8) . . . . ? C1 Ir1 C27 C28 -66.8(5) . . . . ? C5 Ir1 C27 C28 -147.9(5) . . . . ? C26 Ir1 C27 C28 115.3(7) . . . . ? C29 Ir1 C27 C28 37.7(4) . . . . ? C25 Ir1 C27 C28 78.6(5) . . . . ? I1 Ir1 C27 C28 107.2(6) . . . . ? C1 Ir1 C27 C32 55.8(9) . . . . ? C5 Ir1 C27 C32 -25.3(9) . . . . ? C28 Ir1 C27 C32 122.5(10) . . . . ? C26 Ir1 C27 C32 -122.2(10) . . . . ? C29 Ir1 C27 C32 160.2(9) . . . . ? C25 Ir1 C27 C32 -158.9(9) . . . . ? I1 Ir1 C27 C32 -130.2(7) . . . . ? C26 C27 C28 C29 1.7(8) . . . . ? C32 C27 C28 C29 173.6(8) . . . . ? Ir1 C27 C28 C29 -64.3(5) . . . . ? C26 C27 C28 C33 -170.9(7) . . . . ? C32 C27 C28 C33 1.1(13) . . . . ? Ir1 C27 C28 C33 123.1(8) . . . . ? C26 C27 C28 Ir1 66.0(5) . . . . ? C32 C27 C28 Ir1 -122.1(8) . . . . ? C1 Ir1 C28 C29 -116.8(5) . . . . ? C5 Ir1 C28 C29 159.6(4) . . . . ? C27 Ir1 C28 C29 116.5(7) . . . . ? C26 Ir1 C28 C29 78.0(5) . . . . ? C25 Ir1 C28 C29 36.2(4) . . . . ? I1 Ir1 C28 C29 -21.6(6) . . . . ? C1 Ir1 C28 C27 126.7(5) . . . . ? C5 Ir1 C28 C27 43.1(6) . . . . ? C26 Ir1 C28 C27 -38.5(5) . . . . ? C29 Ir1 C28 C27 -116.5(7) . . . . ? C25 Ir1 C28 C27 -80.3(5) . . . . ? I1 Ir1 C28 C27 -138.1(4) . . . . ? C1 Ir1 C28 C33 6.0(8) . . . . ? C5 Ir1 C28 C33 -77.5(8) . . . . ? C27 Ir1 C28 C33 -120.7(9) . . . . ? C26 Ir1 C28 C33 -159.2(8) . . . . ? C29 Ir1 C28 C33 122.8(9) . . . . ? C25 Ir1 C28 C33 159.0(8) . . . . ? I1 Ir1 C28 C33 101.2(7) . . . . ? C26 C25 C29 C28 -0.9(9) . . . . ? C30 C25 C29 C28 -177.9(7) . . . . ? Ir1 C25 C29 C28 59.7(5) . . . . ? C26 C25 C29 C34 170.7(7) . . . . ? C30 C25 C29 C34 -6.3(12) . . . . ? Ir1 C25 C29 C34 -128.7(7) . . . . ? C26 C25 C29 Ir1 -60.6(5) . . . . ? C30 C25 C29 Ir1 122.4(8) . . . . ? C27 C28 C29 C25 -0.5(8) . . . . ? C33 C28 C29 C25 172.2(7) . . . . ? Ir1 C28 C29 C25 -62.1(5) . . . . ? C27 C28 C29 C34 -171.7(7) . . . . ? C33 C28 C29 C34 0.9(13) . . . . ? Ir1 C28 C29 C34 126.7(8) . . . . ? C27 C28 C29 Ir1 61.6(5) . . . . ? C33 C28 C29 Ir1 -125.7(8) . . . . ? C1 Ir1 C29 C25 -166.7(5) . . . . ? C5 Ir1 C29 C25 62.2(10) . . . . ? C27 Ir1 C29 C25 79.5(5) . . . . ? C28 Ir1 C29 C25 118.2(7) . . . . ? C26 Ir1 C29 C25 36.6(5) . . . . ? I1 Ir1 C29 C25 -75.5(5) . . . . ? C1 Ir1 C29 C28 75.1(5) . . . . ? C5 Ir1 C29 C28 -56.0(11) . . . . ? C27 Ir1 C29 C28 -38.8(5) . . . . ? C26 Ir1 C29 C28 -81.7(5) . . . . ? C25 Ir1 C29 C28 -118.2(7) . . . . ? I1 Ir1 C29 C28 166.2(4) . . . . ? C1 Ir1 C29 C34 -46.8(8) . . . . ? C5 Ir1 C29 C34 -177.9(8) . . . . ? C27 Ir1 C29 C34 -160.6(9) . . . . ? C28 Ir1 C29 C34 -121.9(10) . . . . ? C26 Ir1 C29 C34 156.5(9) . . . . ? C25 Ir1 C29 C34 119.9(10) . . . . ? I1 Ir1 C29 C34 44.4(8) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.542 _refine_diff_density_min -2.850 _refine_diff_density_rms 0.218 #===END data_11012 _database_code_depnum_ccdc_archive 'CCDC 823383' #TrackingRef '- Paper#2 cif files.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[(p-cymene)Ru(C,NH2)I]I (5)' _chemical_melting_point ? _chemical_formula_moiety 'C22 H29 N3 Ru I,0.5 C H Cl3,(C2 H5)2 O' _chemical_formula_sum 'C26.50 H39.50 Cl1.50 I2 N3 O Ru' _chemical_formula_weight 824.16 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.772(6) _cell_length_b 14.552(7) _cell_length_c 16.056(8) _cell_angle_alpha 77.716(9) _cell_angle_beta 88.809(9) _cell_angle_gamma 85.046(10) _cell_volume 2678(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 734 _cell_measurement_theta_min 2.674 _cell_measurement_theta_max 28.140 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.044 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1612 _exptl_absorpt_coefficient_mu 3.068 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.574 _exptl_absorpt_correction_T_max 0.831 _exptl_absorpt_process_details ; absorption correction based on 5196 reflections(SADABS);Rint 0.0696 before correction and 0.0466 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21113 _diffrn_reflns_av_R_equivalents 0.1013 _diffrn_reflns_av_sigmaI/netI 0.1733 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10398 _reflns_number_gt 5255 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Atom C22A is disordered and attempt to split this atom failed but is still refined as anisotropic. Disordered CHCl3 and (C2H5)2O was omitted using the SQUEEZE option of PLATON. The solvent accessible voids are 482.7 A3 with an estimated 253e/cell to be added. Two solvent CHCl3 and four (C2H5)2O molecules/unit cell accounting for 284e were included in the formula, FWt, (000) and density calculations. PLATON Reference: Spek, A.L. (1990), Acta Cryst. A46, C-34. 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. ; _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^)+(0.0630P)^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_number_reflns 10398 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1308 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.1635 _refine_ls_wR_factor_gt 0.1444 _refine_ls_goodness_of_fit_ref 0.869 _refine_ls_restrained_S_all 0.869 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 I2A I 0.67812(7) 0.82855(6) 0.44252(6) 0.0448(2) Uani 1 1 d . . . I2 I 0.72250(9) 0.20887(7) 1.01873(6) 0.0666(3) Uani 1 1 d . . . Ru Ru 0.52186(8) 0.32301(7) 0.24579(6) 0.0304(2) Uani 1 1 d . . . I1 I 0.33146(7) 0.24547(6) 0.21152(5) 0.0409(2) Uani 1 1 d . . . N1 N 0.5291(8) 0.3760(6) 0.1100(5) 0.032(2) Uani 1 1 d . . . H1A H 0.5733 0.3335 0.0856 0.039 Uiso 1 1 calc R . . H1B H 0.4568 0.3813 0.0879 0.039 Uiso 1 1 calc R . . N2 N 0.4249(8) 0.5209(6) 0.1742(6) 0.033(2) Uani 1 1 d . . . N3 N 0.3287(7) 0.4679(6) 0.2841(5) 0.028(2) Uani 1 1 d . . . C1 C 0.4165(10) 0.4449(7) 0.2361(7) 0.029(3) Uani 1 1 d . . . C2 C 0.3360(11) 0.5908(8) 0.1817(8) 0.043(3) Uani 1 1 d . . . H2 H 0.3209 0.6505 0.1444 0.052 Uiso 1 1 calc R . . C3 C 0.2781(10) 0.5562(7) 0.2512(8) 0.033(3) Uani 1 1 d . . . H3 H 0.2137 0.5867 0.2739 0.040 Uiso 1 1 calc R . . C4 C 0.5194(10) 0.5377(8) 0.1185(7) 0.031(3) Uani 1 1 d . . . C5 C 0.5737(9) 0.4630(8) 0.0892(7) 0.032(3) Uani 1 1 d . . . C6 C 0.6730(10) 0.4786(9) 0.0393(7) 0.040(3) Uani 1 1 d . . . H6 H 0.7126 0.4271 0.0203 0.048 Uiso 1 1 calc R . . C7 C 0.7133(10) 0.5644(9) 0.0178(7) 0.040(3) Uani 1 1 d . . . H7 H 0.7806 0.5720 -0.0159 0.048 Uiso 1 1 calc R . . C8 C 0.6586(11) 0.6422(10) 0.0439(7) 0.048(4) Uani 1 1 d . . . H8 H 0.6860 0.7030 0.0271 0.058 Uiso 1 1 calc R . . C9 C 0.5592(11) 0.6278(9) 0.0973(7) 0.042(3) Uani 1 1 d . . . H9 H 0.5211 0.6788 0.1179 0.051 Uiso 1 1 calc R . . C10 C 0.2838(10) 0.4089(8) 0.3635(7) 0.034(3) Uani 1 1 d . . . H10 H 0.3257 0.3449 0.3710 0.041 Uiso 1 1 calc R . . C11 C 0.1598(10) 0.3957(10) 0.3591(8) 0.051(4) Uani 1 1 d . . . H11A H 0.1160 0.4574 0.3484 0.077 Uiso 1 1 calc R . . H11B H 0.1353 0.3575 0.4133 0.077 Uiso 1 1 calc R . . H11C H 0.1467 0.3635 0.3129 0.077 Uiso 1 1 calc R . . C12 C 0.3175(12) 0.4512(9) 0.4384(7) 0.054(4) Uani 1 1 d . . . H12A H 0.3963 0.4686 0.4306 0.081 Uiso 1 1 calc R . . H12B H 0.3114 0.4046 0.4918 0.081 Uiso 1 1 calc R . . H12C H 0.2664 0.5076 0.4404 0.081 Uiso 1 1 calc R . . C13 C 0.6684(11) 0.3671(8) 0.3094(7) 0.040(3) Uani 1 1 d . . . C14 C 0.5860(9) 0.3232(9) 0.3710(8) 0.039(3) Uani 1 1 d . . . H14 H 0.5422 0.3636 0.4058 0.047 Uiso 1 1 calc R . . C15 C 0.5500(10) 0.2323(10) 0.3727(8) 0.049(4) Uani 1 1 d . . . H15 H 0.4831 0.2106 0.4086 0.059 Uiso 1 1 calc R . . C16 C 0.5970(12) 0.1788(9) 0.3161(10) 0.053(4) Uani 1 1 d . . . C17 C 0.6785(10) 0.2206(8) 0.2540(8) 0.042(3) Uani 1 1 d . . . H17 H 0.6988 0.1906 0.2045 0.051 Uiso 1 1 calc R . . C18 C 0.7084(8) 0.3123(8) 0.2516(7) 0.032(3) Uani 1 1 d . . . H18 H 0.7503 0.3441 0.2001 0.038 Uiso 1 1 calc R . . C19 C 0.7102(9) 0.4606(9) 0.3089(8) 0.040(3) Uani 1 1 d . . . H19 H 0.7289 0.4902 0.2486 0.048 Uiso 1 1 calc R . . C20 C 0.5588(13) 0.0814(9) 0.3119(11) 0.081(5) Uani 1 1 d . . . H20A H 0.5895 0.0342 0.3609 0.121 Uiso 1 1 calc R . . H20B H 0.5873 0.0639 0.2590 0.121 Uiso 1 1 calc R . . H20C H 0.4753 0.0839 0.3129 0.121 Uiso 1 1 calc R . . C21 C 0.6259(11) 0.5270(9) 0.3417(9) 0.052(4) Uani 1 1 d . . . H21A H 0.5528 0.5301 0.3128 0.078 Uiso 1 1 calc R . . H21B H 0.6540 0.5899 0.3308 0.078 Uiso 1 1 calc R . . H21C H 0.6156 0.5045 0.4032 0.078 Uiso 1 1 calc R . . C22 C 0.8209(10) 0.4413(9) 0.3595(9) 0.052(4) Uani 1 1 d . . . H22A H 0.8049 0.4118 0.4189 0.078 Uiso 1 1 calc R . . H22B H 0.8549 0.5008 0.3575 0.078 Uiso 1 1 calc R . . H22C H 0.8741 0.3988 0.3347 0.078 Uiso 1 1 calc R . . Ru1A Ru 0.02944(9) 0.86178(7) 0.28687(6) 0.0369(3) Uani 1 1 d . . . I1A I 0.05632(7) 0.69014(6) 0.39479(6) 0.0451(2) Uani 1 1 d . . . N1A N -0.0426(8) 0.9030(6) 0.3964(6) 0.034(2) Uani 1 1 d . . . H1A1 H -0.1182 0.8910 0.4002 0.041 Uiso 1 1 calc R . . H1A2 H -0.0063 0.8671 0.4440 0.041 Uiso 1 1 calc R . . N2A N 0.1690(8) 0.9783(6) 0.3753(6) 0.032(2) Uani 1 1 d . . . N3A N 0.2836(8) 0.8664(6) 0.3430(6) 0.032(2) Uani 1 1 d . . . C1A C 0.1735(10) 0.9026(9) 0.3379(8) 0.038(3) Uani 1 1 d . . . C2A C 0.2782(10) 0.9871(8) 0.4041(8) 0.038(3) Uani 1 1 d . . . H2A H 0.2993 1.0330 0.4336 0.045 Uiso 1 1 calc R . . C3A C 0.3465(9) 0.9189(8) 0.3822(8) 0.036(3) Uani 1 1 d . . . H3A H 0.4263 0.9084 0.3922 0.043 Uiso 1 1 calc R . . C4A C 0.0711(9) 1.0393(8) 0.3852(6) 0.028(3) Uani 1 1 d . . . C5A C -0.0341(9) 1.0027(8) 0.3956(7) 0.031(3) Uani 1 1 d . . . C6A C -0.1297(10) 1.0614(8) 0.4065(7) 0.035(3) Uani 1 1 d . . . H6A H -0.2024 1.0368 0.4137 0.042 Uiso 1 1 calc R . . C7A C -0.1204(10) 1.1568(8) 0.4071(7) 0.038(3) Uani 1 1 d . . . H7A H -0.1856 1.1975 0.4146 0.045 Uiso 1 1 calc R . . C8A C -0.0122(11) 1.1896(8) 0.3962(7) 0.038(3) Uani 1 1 d . . . H8A H -0.0038 1.2539 0.3963 0.045 Uiso 1 1 calc R . . C9A C 0.0812(10) 1.1323(8) 0.3854(7) 0.032(3) Uani 1 1 d . . . H9A H 0.1540 1.1566 0.3780 0.039 Uiso 1 1 calc R . . C10A C 0.3317(12) 0.7841(9) 0.3114(8) 0.049(4) Uani 1 1 d . . . H10A H 0.2685 0.7564 0.2871 0.059 Uiso 1 1 calc R . . C11A C 0.3822(11) 0.7126(9) 0.3850(8) 0.053(4) Uani 1 1 d . . . H11D H 0.4458 0.7381 0.4084 0.079 Uiso 1 1 calc R . . H11E H 0.4100 0.6552 0.3656 0.079 Uiso 1 1 calc R . . H11F H 0.3239 0.6974 0.4291 0.079 Uiso 1 1 calc R . . C12A C 0.4166(12) 0.8153(11) 0.2409(10) 0.075(5) Uani 1 1 d . . . H12D H 0.3797 0.8654 0.1968 0.112 Uiso 1 1 calc R . . H12E H 0.4436 0.7615 0.2159 0.112 Uiso 1 1 calc R . . H12F H 0.4815 0.8392 0.2645 0.112 Uiso 1 1 calc R . . C13A C 0.020(2) 0.7936(12) 0.1767(9) 0.088(7) Uani 1 1 d . . . H13A H 0.0587 0.7288 0.1820 0.106 Uiso 1 1 calc R . . C14A C 0.0910(13) 0.8737(13) 0.1566(8) 0.065(5) Uani 1 1 d . . . H14A H 0.1743 0.8636 0.1443 0.078 Uiso 1 1 calc R . . C15A C 0.0395(13) 0.9668(11) 0.1657(8) 0.058(4) Uani 1 1 d . . . C16A C -0.0743(12) 0.9667(10) 0.1957(8) 0.048(4) Uani 1 1 d . . . H16A H -0.1083 1.0241 0.2149 0.058 Uiso 1 1 calc R . . C17A C -0.1370(14) 0.8858(13) 0.2115(9) 0.063(4) Uani 1 1 d . . . H17A H -0.2103 0.8886 0.2439 0.076 Uiso 1 1 calc R . . C18A C -0.092(2) 0.8010(17) 0.2020(13) 0.097(7) Uani 1 1 d . . . C19A C 0.123(3) 1.0483(16) 0.1322(16) 0.146(11) Uani 1 1 d . . . H19A H 0.2029 1.0348 0.1551 0.176 Uiso 1 1 calc R . . C20A C -0.155(2) 0.7164(14) 0.2210(12) 0.162(12) Uani 1 1 d . . . H20D H -0.1497 0.6885 0.2821 0.243 Uiso 1 1 calc R . . H20E H -0.1215 0.6705 0.1887 0.243 Uiso 1 1 calc R . . H20F H -0.2347 0.7336 0.2049 0.243 Uiso 1 1 calc R . . C21A C 0.114(2) 1.0854(18) 0.0316(14) 0.162(10) Uani 1 1 d . . . H21D H 0.1604 1.0419 0.0030 0.243 Uiso 1 1 calc R . . H21E H 0.1424 1.1483 0.0159 0.243 Uiso 1 1 calc R . . H21F H 0.0345 1.0889 0.0142 0.243 Uiso 1 1 calc R . . C22A C 0.046(3) 1.144(3) 0.1599(14) 0.31(3) Uani 1 1 d . . . H22D H -0.0344 1.1432 0.1469 0.460 Uiso 1 1 calc R . . H22E H 0.0747 1.2028 0.1275 0.460 Uiso 1 1 calc R . . H22F H 0.0551 1.1412 0.2210 0.460 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 I2A 0.0345(5) 0.0402(5) 0.0560(6) -0.0015(4) -0.0007(4) -0.0037(4) I2 0.0834(8) 0.0566(6) 0.0535(6) -0.0072(5) 0.0124(5) 0.0156(6) Ru 0.0285(5) 0.0319(5) 0.0282(5) -0.0020(4) -0.0030(4) 0.0016(4) I1 0.0369(5) 0.0399(5) 0.0463(5) -0.0090(4) -0.0044(4) -0.0042(4) N1 0.029(5) 0.041(6) 0.024(5) -0.003(5) -0.001(4) 0.008(5) N2 0.034(6) 0.029(5) 0.038(6) -0.007(5) -0.002(5) -0.003(4) N3 0.032(6) 0.027(5) 0.022(5) -0.002(4) 0.004(4) 0.000(4) C1 0.041(7) 0.027(6) 0.017(6) -0.001(5) -0.002(5) -0.008(5) C2 0.060(9) 0.024(7) 0.043(8) -0.006(6) -0.010(7) 0.008(6) C3 0.036(7) 0.022(6) 0.041(8) -0.009(6) 0.004(6) 0.003(5) C4 0.046(8) 0.030(7) 0.017(6) 0.000(5) -0.003(5) -0.015(6) C5 0.030(7) 0.031(7) 0.033(7) -0.003(6) -0.016(5) 0.005(5) C6 0.034(7) 0.042(8) 0.034(7) 0.011(6) 0.000(6) 0.004(6) C7 0.024(7) 0.055(9) 0.034(7) 0.004(7) -0.005(5) -0.003(6) C8 0.051(9) 0.063(10) 0.028(7) 0.008(7) -0.007(6) -0.031(8) C9 0.060(9) 0.042(8) 0.024(7) -0.009(6) -0.016(6) 0.008(7) C10 0.033(7) 0.027(6) 0.038(7) 0.001(6) 0.005(6) 0.003(5) C11 0.037(8) 0.066(10) 0.052(9) -0.016(8) 0.003(7) -0.008(7) C12 0.100(12) 0.045(8) 0.019(7) -0.010(6) 0.015(7) -0.014(8) C13 0.054(9) 0.036(7) 0.030(7) -0.010(6) -0.005(6) 0.009(6) C14 0.026(7) 0.050(8) 0.038(8) -0.008(7) -0.003(6) 0.006(6) C15 0.025(7) 0.054(9) 0.049(9) 0.028(7) 0.006(6) 0.004(6) C16 0.043(8) 0.029(7) 0.072(10) 0.023(7) -0.014(8) 0.009(6) C17 0.047(8) 0.039(7) 0.040(8) -0.017(6) -0.023(6) 0.031(6) C18 0.014(6) 0.044(7) 0.032(7) 0.008(6) -0.012(5) -0.007(5) C19 0.025(7) 0.045(8) 0.048(8) -0.007(6) -0.014(6) -0.002(6) C20 0.075(12) 0.037(9) 0.124(15) -0.001(9) -0.024(10) -0.005(8) C21 0.047(8) 0.048(8) 0.070(10) -0.037(8) -0.017(7) 0.011(7) C22 0.041(8) 0.034(7) 0.085(11) -0.015(7) -0.001(7) -0.013(6) Ru1A 0.0398(6) 0.0382(6) 0.0344(6) -0.0105(5) 0.0001(5) -0.0059(5) I1A 0.0469(5) 0.0337(5) 0.0537(6) -0.0091(4) 0.0064(4) 0.0000(4) N1A 0.039(6) 0.030(5) 0.031(6) -0.002(5) 0.004(5) -0.004(5) N2A 0.036(6) 0.024(5) 0.037(6) -0.012(5) 0.010(5) -0.006(4) N3A 0.033(6) 0.027(5) 0.038(6) -0.010(5) 0.008(5) -0.006(4) C1A 0.025(7) 0.044(8) 0.040(7) 0.000(6) 0.009(5) 0.002(6) C2A 0.033(7) 0.037(7) 0.045(8) -0.008(6) -0.006(6) -0.015(6) C3A 0.018(6) 0.035(7) 0.056(8) -0.016(6) 0.008(6) 0.009(5) C4A 0.025(6) 0.034(7) 0.020(6) 0.000(5) 0.004(5) 0.006(5) C5A 0.029(7) 0.036(7) 0.026(6) 0.003(5) -0.010(5) -0.013(5) C6A 0.042(7) 0.025(6) 0.028(7) 0.009(5) -0.010(5) 0.015(5) C7A 0.038(7) 0.040(7) 0.036(7) -0.010(6) -0.010(6) 0.005(6) C8A 0.054(8) 0.018(6) 0.042(8) -0.005(6) -0.016(6) 0.001(6) C9A 0.044(8) 0.026(6) 0.027(7) -0.005(5) -0.004(5) -0.005(6) C10A 0.059(9) 0.047(8) 0.051(9) -0.029(7) -0.006(7) -0.006(7) C11A 0.051(9) 0.054(9) 0.056(9) -0.024(8) -0.005(7) 0.009(7) C12A 0.055(10) 0.097(13) 0.091(13) -0.057(11) 0.037(9) -0.031(9) C13A 0.18(2) 0.055(11) 0.025(9) -0.011(8) -0.020(12) 0.000(14) C14A 0.053(10) 0.105(14) 0.032(8) -0.018(9) 0.003(7) 0.023(10) C15A 0.070(11) 0.067(11) 0.032(8) 0.009(7) -0.006(7) -0.031(9) C16A 0.055(9) 0.056(9) 0.030(8) -0.009(7) -0.005(7) 0.018(7) C17A 0.070(11) 0.083(12) 0.042(9) -0.013(9) -0.014(8) -0.029(10) C18A 0.103(17) 0.109(19) 0.084(15) -0.014(13) -0.033(13) -0.033(15) C19A 0.26(4) 0.100(18) 0.09(2) -0.013(14) -0.02(2) -0.05(2) C20A 0.28(3) 0.119(18) 0.096(16) 0.022(14) -0.093(18) -0.14(2) C21A 0.21(3) 0.17(3) 0.11(2) -0.039(18) -0.037(19) 0.01(2) C22A 0.20(3) 0.68(9) 0.057(16) 0.00(3) -0.016(18) -0.31(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 Ru C1 2.054(11) . ? Ru N1 2.154(8) . ? Ru C14 2.163(12) . ? Ru C18 2.190(10) . ? Ru C15 2.194(11) . ? Ru C13 2.230(13) . ? Ru C17 2.256(11) . ? Ru C16 2.275(11) . ? Ru I1 2.7116(16) . ? N1 C5 1.385(14) . ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? N2 C1 1.328(13) . ? N2 C2 1.417(14) . ? N2 C4 1.418(14) . ? N3 C1 1.338(13) . ? N3 C3 1.370(13) . ? N3 C10 1.492(13) . ? C2 C3 1.323(15) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C5 1.378(15) . ? C4 C9 1.402(15) . ? C5 C6 1.410(15) . ? C6 C7 1.348(16) . ? C6 H6 0.9500 . ? C7 C8 1.392(17) . ? C7 H7 0.9500 . ? C8 C9 1.439(17) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.494(15) . ? C10 C12 1.536(16) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C18 1.398(15) . ? C13 C14 1.457(16) . ? C13 C19 1.485(16) . ? C14 C15 1.418(17) . ? C14 H14 1.0000 . ? C15 C16 1.394(19) . ? C15 H15 1.0000 . ? C16 C17 1.445(17) . ? C16 C20 1.540(18) . ? C17 C18 1.402(15) . ? C17 H17 1.0000 . ? C18 H18 1.0000 . ? C19 C21 1.492(15) . ? C19 C22 1.523(15) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? Ru1A C1A 2.082(13) . ? Ru1A N1A 2.114(9) . ? Ru1A C14A 2.175(13) . ? Ru1A C16A 2.183(12) . ? Ru1A C15A 2.212(13) . ? Ru1A C13A 2.213(15) . ? Ru1A C17A 2.286(15) . ? Ru1A C18A 2.342(19) . ? Ru1A I1A 2.7177(17) . ? N1A C5A 1.460(13) . ? N1A H1A1 0.9200 . ? N1A H1A2 0.9200 . ? N2A C1A 1.361(14) . ? N2A C2A 1.401(14) . ? N2A C4A 1.419(13) . ? N3A C1A 1.354(13) . ? N3A C3A 1.361(14) . ? N3A C10A 1.462(14) . ? C2A C3A 1.323(15) . ? C2A H2A 0.9500 . ? C3A H3A 0.9500 . ? C4A C9A 1.370(14) . ? C4A C5A 1.383(14) . ? C5A C6A 1.385(15) . ? C6A C7A 1.404(15) . ? C6A H6A 0.9500 . ? C7A C8A 1.393(16) . ? C7A H7A 0.9500 . ? C8A C9A 1.353(15) . ? C8A H8A 0.9500 . ? C9A H9A 0.9500 . ? C10A C11A 1.494(17) . ? C10A C12A 1.517(17) . ? C10A H10A 1.0000 . ? C11A H11D 0.9800 . ? C11A H11E 0.9800 . ? C11A H11F 0.9800 . ? C12A H12D 0.9800 . ? C12A H12E 0.9800 . ? C12A H12F 0.9800 . ? C13A C18A 1.37(3) . ? C13A C14A 1.47(2) . ? C13A H13A 1.0000 . ? C14A C15A 1.47(2) . ? C14A H14A 1.0000 . ? C15A C16A 1.414(18) . ? C15A C19A 1.61(3) . ? C16A C17A 1.418(19) . ? C16A H16A 1.0000 . ? C17A C18A 1.34(2) . ? C17A H17A 1.0000 . ? C18A C20A 1.46(2) . ? C19A C21A 1.59(3) . ? C19A C22A 1.73(5) . ? C19A H19A 1.0000 . ? C20A H20D 0.9800 . ? C20A H20E 0.9800 . ? C20A H20F 0.9800 . ? C21A H21D 0.9800 . ? C21A H21E 0.9800 . ? C21A H21F 0.9800 . ? C22A H22D 0.9800 . ? C22A H22E 0.9800 . ? C22A H22F 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 C1 Ru N1 80.4(4) . . ? C1 Ru C14 95.5(4) . . ? N1 Ru C14 148.4(4) . . ? C1 Ru C18 125.8(4) . . ? N1 Ru C18 90.0(4) . . ? C14 Ru C18 66.9(4) . . ? C1 Ru C15 118.0(5) . . ? N1 Ru C15 161.6(5) . . ? C14 Ru C15 38.0(5) . . ? C18 Ru C15 79.6(4) . . ? C1 Ru C13 97.9(4) . . ? N1 Ru C13 110.4(4) . . ? C14 Ru C13 38.7(4) . . ? C18 Ru C13 36.9(4) . . ? C15 Ru C13 69.7(5) . . ? C1 Ru C17 162.5(5) . . ? N1 Ru C17 96.4(4) . . ? C14 Ru C17 78.2(4) . . ? C18 Ru C17 36.7(4) . . ? C15 Ru C17 66.3(5) . . ? C13 Ru C17 66.9(4) . . ? C1 Ru C16 153.2(5) . . ? N1 Ru C16 125.4(5) . . ? C14 Ru C16 66.6(5) . . ? C18 Ru C16 67.1(4) . . ? C15 Ru C16 36.3(5) . . ? C13 Ru C16 80.6(5) . . ? C17 Ru C16 37.2(4) . . ? C1 Ru I1 84.9(3) . . ? N1 Ru I1 84.9(3) . . ? C14 Ru I1 126.2(3) . . ? C18 Ru I1 147.6(3) . . ? C15 Ru I1 95.6(4) . . ? C13 Ru I1 164.7(3) . . ? C17 Ru I1 112.1(3) . . ? C16 Ru I1 90.1(4) . . ? C5 N1 Ru 112.2(7) . . ? C5 N1 H1A 109.2 . . ? Ru N1 H1A 109.2 . . ? C5 N1 H1B 109.2 . . ? Ru N1 H1B 109.2 . . ? H1A N1 H1B 107.9 . . ? C1 N2 C2 110.1(10) . . ? C1 N2 C4 125.3(10) . . ? C2 N2 C4 123.6(10) . . ? C1 N3 C3 111.8(9) . . ? C1 N3 C10 127.6(9) . . ? C3 N3 C10 120.6(9) . . ? N2 C1 N3 105.0(9) . . ? N2 C1 Ru 123.5(8) . . ? N3 C1 Ru 131.6(8) . . ? C3 C2 N2 106.2(10) . . ? C3 C2 H2 126.9 . . ? N2 C2 H2 126.9 . . ? C2 C3 N3 106.8(10) . . ? C2 C3 H3 126.6 . . ? N3 C3 H3 126.6 . . ? C5 C4 C9 121.2(11) . . ? C5 C4 N2 118.6(10) . . ? C9 C4 N2 120.2(11) . . ? C4 C5 N1 118.9(11) . . ? C4 C5 C6 118.3(11) . . ? N1 C5 C6 122.8(11) . . ? C7 C6 C5 121.9(12) . . ? C7 C6 H6 119.0 . . ? C5 C6 H6 119.0 . . ? C6 C7 C8 121.4(12) . . ? C6 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? C7 C8 C9 117.9(12) . . ? C7 C8 H8 121.0 . . ? C9 C8 H8 121.0 . . ? C4 C9 C8 119.3(12) . . ? C4 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? N3 C10 C11 113.5(10) . . ? N3 C10 C12 107.3(9) . . ? C11 C10 C12 114.7(10) . . ? N3 C10 H10 107.0 . . ? C11 C10 H10 107.0 . . ? C12 C10 H10 107.0 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 114.3(11) . . ? C18 C13 C19 122.0(12) . . ? C14 C13 C19 123.7(11) . . ? C18 C13 Ru 70.0(6) . . ? C14 C13 Ru 68.2(7) . . ? C19 C13 Ru 132.8(8) . . ? C15 C14 C13 123.0(11) . . ? C15 C14 Ru 72.2(7) . . ? C13 C14 Ru 73.2(7) . . ? C15 C14 H14 117.9 . . ? C13 C14 H14 117.9 . . ? Ru C14 H14 117.9 . . ? C16 C15 C14 120.2(12) . . ? C16 C15 Ru 75.0(7) . . ? C14 C15 Ru 69.8(7) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? Ru C15 H15 119.6 . . ? C15 C16 C17 118.0(12) . . ? C15 C16 C20 123.1(14) . . ? C17 C16 C20 118.6(14) . . ? C15 C16 Ru 68.7(7) . . ? C17 C16 Ru 70.7(6) . . ? C20 C16 Ru 127.9(9) . . ? C18 C17 C16 120.3(11) . . ? C18 C17 Ru 69.1(6) . . ? C16 C17 Ru 72.1(7) . . ? C18 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? Ru C17 H17 119.1 . . ? C13 C18 C17 124.0(11) . . ? C13 C18 Ru 73.1(7) . . ? C17 C18 Ru 74.2(6) . . ? C13 C18 H18 117.6 . . ? C17 C18 H18 117.6 . . ? Ru C18 H18 117.6 . . ? C13 C19 C21 114.0(10) . . ? C13 C19 C22 106.4(10) . . ? C21 C19 C22 112.5(11) . . ? C13 C19 H19 107.9 . . ? C21 C19 H19 107.9 . . ? C22 C19 H19 107.9 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C1A Ru1A N1A 79.9(4) . . ? C1A Ru1A C14A 97.8(6) . . ? N1A Ru1A C14A 159.3(5) . . ? C1A Ru1A C16A 118.8(5) . . ? N1A Ru1A C16A 95.4(4) . . ? C14A Ru1A C16A 67.5(5) . . ? C1A Ru1A C15A 93.8(5) . . ? N1A Ru1A C15A 120.1(5) . . ? C14A Ru1A C15A 39.2(5) . . ? C16A Ru1A C15A 37.5(5) . . ? C1A Ru1A C13A 128.0(8) . . ? N1A Ru1A C13A 151.5(7) . . ? C14A Ru1A C13A 39.1(6) . . ? C16A Ru1A C13A 77.0(6) . . ? C15A Ru1A C13A 69.4(6) . . ? C1A Ru1A C17A 155.3(6) . . ? N1A Ru1A C17A 95.4(5) . . ? C14A Ru1A C17A 78.1(6) . . ? C16A Ru1A C17A 36.9(5) . . ? C15A Ru1A C17A 67.5(5) . . ? C13A Ru1A C17A 62.0(7) . . ? C1A Ru1A C18A 162.8(7) . . ? N1A Ru1A C18A 117.2(7) . . ? C14A Ru1A C18A 67.2(7) . . ? C16A Ru1A C18A 64.5(7) . . ? C15A Ru1A C18A 79.9(6) . . ? C13A Ru1A C18A 34.8(7) . . ? C17A Ru1A C18A 33.6(6) . . ? C1A Ru1A I1A 90.3(3) . . ? N1A Ru1A I1A 82.5(2) . . ? C14A Ru1A I1A 118.2(5) . . ? C16A Ru1A I1A 150.1(4) . . ? C15A Ru1A I1A 157.3(4) . . ? C13A Ru1A I1A 90.6(4) . . ? C17A Ru1A I1A 113.4(4) . . ? C18A Ru1A I1A 89.8(5) . . ? C5A N1A Ru1A 113.0(7) . . ? C5A N1A H1A1 109.0 . . ? Ru1A N1A H1A1 109.0 . . ? C5A N1A H1A2 109.0 . . ? Ru1A N1A H1A2 109.0 . . ? H1A1 N1A H1A2 107.8 . . ? C1A N2A C2A 108.7(9) . . ? C1A N2A C4A 126.8(10) . . ? C2A N2A C4A 124.5(10) . . ? C1A N3A C3A 109.7(10) . . ? C1A N3A C10A 126.8(10) . . ? C3A N3A C10A 123.5(10) . . ? N3A C1A N2A 106.0(10) . . ? N3A C1A Ru1A 132.0(9) . . ? N2A C1A Ru1A 122.1(8) . . ? C3A C2A N2A 106.8(11) . . ? C3A C2A H2A 126.6 . . ? N2A C2A H2A 126.6 . . ? C2A C3A N3A 108.8(10) . . ? C2A C3A H3A 125.6 . . ? N3A C3A H3A 125.6 . . ? C9A C4A C5A 120.8(10) . . ? C9A C4A N2A 120.4(10) . . ? C5A C4A N2A 118.7(10) . . ? C4A C5A C6A 119.1(11) . . ? C4A C5A N1A 119.9(10) . . ? C6A C5A N1A 121.0(10) . . ? C5A C6A C7A 120.6(11) . . ? C5A C6A H6A 119.7 . . ? C7A C6A H6A 119.7 . . ? C8A C7A C6A 117.7(11) . . ? C8A C7A H7A 121.2 . . ? C6A C7A H7A 121.2 . . ? C9A C8A C7A 121.7(11) . . ? C9A C8A H8A 119.1 . . ? C7A C8A H8A 119.1 . . ? C8A C9A C4A 120.1(11) . . ? C8A C9A H9A 119.9 . . ? C4A C9A H9A 119.9 . . ? N3A C10A C11A 108.4(10) . . ? N3A C10A C12A 109.3(11) . . ? C11A C10A C12A 113.6(13) . . ? N3A C10A H10A 108.5 . . ? C11A C10A H10A 108.5 . . ? C12A C10A H10A 108.5 . . ? C10A C11A H11D 109.5 . . ? C10A C11A H11E 109.5 . . ? H11D C11A H11E 109.5 . . ? C10A C11A H11F 109.5 . . ? H11D C11A H11F 109.5 . . ? H11E C11A H11F 109.5 . . ? C10A C12A H12D 109.5 . . ? C10A C12A H12E 109.5 . . ? H12D C12A H12E 109.5 . . ? C10A C12A H12F 109.5 . . ? H12D C12A H12F 109.5 . . ? H12E C12A H12F 109.5 . . ? C18A C13A C14A 123.9(18) . . ? C18A C13A Ru1A 77.8(11) . . ? C14A C13A Ru1A 69.1(8) . . ? C18A C13A H13A 117.6 . . ? C14A C13A H13A 117.6 . . ? Ru1A C13A H13A 117.6 . . ? C13A C14A C15A 117.9(14) . . ? C13A C14A Ru1A 71.8(8) . . ? C15A C14A Ru1A 71.8(7) . . ? C13A C14A H14A 120.9 . . ? C15A C14A H14A 120.9 . . ? Ru1A C14A H14A 120.9 . . ? C16A C15A C14A 114.2(13) . . ? C16A C15A C19A 133.9(17) . . ? C14A C15A C19A 111.7(16) . . ? C16A C15A Ru1A 70.1(7) . . ? C14A C15A Ru1A 69.1(7) . . ? C19A C15A Ru1A 132.7(13) . . ? C15A C16A C17A 123.8(14) . . ? C15A C16A Ru1A 72.4(7) . . ? C17A C16A Ru1A 75.5(8) . . ? C15A C16A H16A 117.8 . . ? C17A C16A H16A 117.8 . . ? Ru1A C16A H16A 117.8 . . ? C18A C17A C16A 122.5(17) . . ? C18A C17A Ru1A 75.5(11) . . ? C16A C17A Ru1A 67.6(8) . . ? C18A C17A H17A 117.9 . . ? C16A C17A H17A 117.9 . . ? Ru1A C17A H17A 117.9 . . ? C17A C18A C13A 118(2) . . ? C17A C18A C20A 123(2) . . ? C13A C18A C20A 119(2) . . ? C17A C18A Ru1A 70.9(11) . . ? C13A C18A Ru1A 67.4(10) . . ? C20A C18A Ru1A 130.9(14) . . ? C21A C19A C15A 111.5(19) . . ? C21A C19A C22A 96.7(19) . . ? C15A C19A C22A 101(2) . . ? C21A C19A H19A 115.2 . . ? C15A C19A H19A 115.2 . . ? C22A C19A H19A 115.2 . . ? C18A C20A H20D 109.5 . . ? C18A C20A H20E 109.5 . . ? H20D C20A H20E 109.5 . . ? C18A C20A H20F 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? C19A C21A H21D 109.5 . . ? C19A C21A H21E 109.5 . . ? H21D C21A H21E 109.5 . . ? C19A C21A H21F 109.5 . . ? H21D C21A H21F 109.5 . . ? H21E C21A H21F 109.5 . . ? C19A C22A H22D 109.5 . . ? C19A C22A H22E 109.5 . . ? H22D C22A H22E 109.5 . . ? C19A C22A H22F 109.5 . . ? H22D C22A H22F 109.5 . . ? H22E C22A H22F 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 C1 Ru N1 C5 61.2(7) . . . . ? C14 Ru N1 C5 -23.6(12) . . . . ? C18 Ru N1 C5 -65.1(8) . . . . ? C15 Ru N1 C5 -120.4(14) . . . . ? C13 Ru N1 C5 -33.7(8) . . . . ? C17 Ru N1 C5 -101.4(8) . . . . ? C16 Ru N1 C5 -126.6(8) . . . . ? I1 Ru N1 C5 146.9(7) . . . . ? C2 N2 C1 N3 -3.2(12) . . . . ? C4 N2 C1 N3 165.8(10) . . . . ? C2 N2 C1 Ru 176.1(8) . . . . ? C4 N2 C1 Ru -14.9(15) . . . . ? C3 N3 C1 N2 2.7(12) . . . . ? C10 N3 C1 N2 -178.5(10) . . . . ? C3 N3 C1 Ru -176.5(8) . . . . ? C10 N3 C1 Ru 2.3(17) . . . . ? N1 Ru C1 N2 -27.2(9) . . . . ? C14 Ru C1 N2 121.2(9) . . . . ? C18 Ru C1 N2 55.8(11) . . . . ? C15 Ru C1 N2 153.4(9) . . . . ? C13 Ru C1 N2 82.3(9) . . . . ? C17 Ru C1 N2 53.4(19) . . . . ? C16 Ru C1 N2 167.1(10) . . . . ? I1 Ru C1 N2 -112.9(9) . . . . ? N1 Ru C1 N3 151.9(11) . . . . ? C14 Ru C1 N3 -59.7(11) . . . . ? C18 Ru C1 N3 -125.1(10) . . . . ? C15 Ru C1 N3 -27.5(12) . . . . ? C13 Ru C1 N3 -98.6(11) . . . . ? C17 Ru C1 N3 -127.5(14) . . . . ? C16 Ru C1 N3 -13.8(17) . . . . ? I1 Ru C1 N3 66.2(10) . . . . ? C1 N2 C2 C3 2.6(13) . . . . ? C4 N2 C2 C3 -166.6(10) . . . . ? N2 C2 C3 N3 -0.8(13) . . . . ? C1 N3 C3 C2 -1.1(13) . . . . ? C10 N3 C3 C2 180.0(10) . . . . ? C1 N2 C4 C5 38.9(16) . . . . ? C2 N2 C4 C5 -153.6(11) . . . . ? C1 N2 C4 C9 -138.3(11) . . . . ? C2 N2 C4 C9 29.3(16) . . . . ? C9 C4 C5 N1 -178.2(10) . . . . ? N2 C4 C5 N1 4.6(15) . . . . ? C9 C4 C5 C6 2.1(16) . . . . ? N2 C4 C5 C6 -175.1(10) . . . . ? Ru N1 C5 C4 -59.6(11) . . . . ? Ru N1 C5 C6 120.1(10) . . . . ? C4 C5 C6 C7 -2.1(17) . . . . ? N1 C5 C6 C7 178.2(11) . . . . ? C5 C6 C7 C8 0.0(18) . . . . ? C6 C7 C8 C9 2.1(17) . . . . ? C5 C4 C9 C8 0.0(17) . . . . ? N2 C4 C9 C8 177.1(10) . . . . ? C7 C8 C9 C4 -2.0(17) . . . . ? C1 N3 C10 C11 -124.5(12) . . . . ? C3 N3 C10 C11 54.3(14) . . . . ? C1 N3 C10 C12 107.7(12) . . . . ? C3 N3 C10 C12 -73.5(13) . . . . ? C1 Ru C13 C18 -143.0(7) . . . . ? N1 Ru C13 C18 -60.3(7) . . . . ? C14 Ru C13 C18 128.2(10) . . . . ? C15 Ru C13 C18 100.0(8) . . . . ? C17 Ru C13 C18 27.9(7) . . . . ? C16 Ru C13 C18 64.1(7) . . . . ? I1 Ru C13 C18 117.2(11) . . . . ? C1 Ru C13 C14 88.9(7) . . . . ? N1 Ru C13 C14 171.5(6) . . . . ? C18 Ru C13 C14 -128.2(10) . . . . ? C15 Ru C13 C14 -28.1(7) . . . . ? C17 Ru C13 C14 -100.2(8) . . . . ? C16 Ru C13 C14 -64.1(7) . . . . ? I1 Ru C13 C14 -10.9(16) . . . . ? C1 Ru C13 C19 -27.4(12) . . . . ? N1 Ru C13 C19 55.2(12) . . . . ? C14 Ru C13 C19 -116.3(14) . . . . ? C18 Ru C13 C19 115.6(15) . . . . ? C15 Ru C13 C19 -144.4(13) . . . . ? C17 Ru C13 C19 143.5(13) . . . . ? C16 Ru C13 C19 179.7(13) . . . . ? I1 Ru C13 C19 -127.2(12) . . . . ? C18 C13 C14 C15 0.5(16) . . . . ? C19 C13 C14 C15 -177.6(11) . . . . ? Ru C13 C14 C15 54.7(10) . . . . ? C18 C13 C14 Ru -54.2(9) . . . . ? C19 C13 C14 Ru 127.7(11) . . . . ? C1 Ru C14 C15 130.1(7) . . . . ? N1 Ru C14 C15 -149.3(8) . . . . ? C18 Ru C14 C15 -103.2(8) . . . . ? C13 Ru C14 C15 -134.1(10) . . . . ? C17 Ru C14 C15 -66.5(7) . . . . ? C16 Ru C14 C15 -29.2(7) . . . . ? I1 Ru C14 C15 42.4(8) . . . . ? C1 Ru C14 C13 -95.8(7) . . . . ? N1 Ru C14 C13 -15.3(11) . . . . ? C18 Ru C14 C13 30.8(6) . . . . ? C15 Ru C14 C13 134.1(10) . . . . ? C17 Ru C14 C13 67.6(7) . . . . ? C16 Ru C14 C13 104.8(8) . . . . ? I1 Ru C14 C13 176.4(5) . . . . ? C13 C14 C15 C16 2.7(18) . . . . ? Ru C14 C15 C16 57.8(11) . . . . ? C13 C14 C15 Ru -55.1(10) . . . . ? C1 Ru C15 C16 169.6(7) . . . . ? N1 Ru C15 C16 -8.6(18) . . . . ? C14 Ru C15 C16 -130.8(11) . . . . ? C18 Ru C15 C16 -65.3(8) . . . . ? C13 Ru C15 C16 -102.2(8) . . . . ? C17 Ru C15 C16 -29.3(8) . . . . ? I1 Ru C15 C16 82.4(8) . . . . ? C1 Ru C15 C14 -59.6(8) . . . . ? N1 Ru C15 C14 122.2(14) . . . . ? C18 Ru C15 C14 65.5(7) . . . . ? C13 Ru C15 C14 28.6(7) . . . . ? C17 Ru C15 C14 101.5(8) . . . . ? C16 Ru C15 C14 130.8(11) . . . . ? I1 Ru C15 C14 -146.9(6) . . . . ? C14 C15 C16 C17 -2.9(17) . . . . ? Ru C15 C16 C17 52.4(10) . . . . ? C14 C15 C16 C20 -177.5(11) . . . . ? Ru C15 C16 C20 -122.2(12) . . . . ? C14 C15 C16 Ru -55.3(10) . . . . ? C1 Ru C16 C15 -20.7(15) . . . . ? N1 Ru C16 C15 176.7(7) . . . . ? C14 Ru C16 C15 30.5(8) . . . . ? C18 Ru C16 C15 104.1(9) . . . . ? C13 Ru C16 C15 68.3(8) . . . . ? C17 Ru C16 C15 132.1(12) . . . . ? I1 Ru C16 C15 -99.5(8) . . . . ? C1 Ru C16 C17 -152.8(9) . . . . ? N1 Ru C16 C17 44.5(9) . . . . ? C14 Ru C16 C17 -101.6(8) . . . . ? C18 Ru C16 C17 -28.0(7) . . . . ? C15 Ru C16 C17 -132.1(12) . . . . ? C13 Ru C16 C17 -63.9(8) . . . . ? I1 Ru C16 C17 128.4(7) . . . . ? C1 Ru C16 C20 95.4(17) . . . . ? N1 Ru C16 C20 -67.2(15) . . . . ? C14 Ru C16 C20 146.6(15) . . . . ? C18 Ru C16 C20 -139.8(15) . . . . ? C15 Ru C16 C20 116.1(17) . . . . ? C13 Ru C16 C20 -175.6(15) . . . . ? C17 Ru C16 C20 -111.8(18) . . . . ? I1 Ru C16 C20 16.6(14) . . . . ? C15 C16 C17 C18 0.0(17) . . . . ? C20 C16 C17 C18 174.9(11) . . . . ? Ru C16 C17 C18 51.5(9) . . . . ? C15 C16 C17 Ru -51.5(10) . . . . ? C20 C16 C17 Ru 123.4(11) . . . . ? C1 Ru C17 C18 3.3(18) . . . . ? N1 Ru C17 C18 81.5(7) . . . . ? C14 Ru C17 C18 -67.0(7) . . . . ? C15 Ru C17 C18 -105.0(8) . . . . ? C13 Ru C17 C18 -28.0(7) . . . . ? C16 Ru C17 C18 -133.7(11) . . . . ? I1 Ru C17 C18 168.6(6) . . . . ? C1 Ru C17 C16 137.0(14) . . . . ? N1 Ru C17 C16 -144.9(8) . . . . ? C14 Ru C17 C16 66.7(8) . . . . ? C18 Ru C17 C16 133.7(11) . . . . ? C15 Ru C17 C16 28.6(8) . . . . ? C13 Ru C17 C16 105.6(9) . . . . ? I1 Ru C17 C16 -57.8(8) . . . . ? C14 C13 C18 C17 -3.5(16) . . . . ? C19 C13 C18 C17 174.6(10) . . . . ? Ru C13 C18 C17 -56.8(9) . . . . ? C14 C13 C18 Ru 53.2(9) . . . . ? C19 C13 C18 Ru -128.7(11) . . . . ? C16 C17 C18 C13 3.4(16) . . . . ? Ru C17 C18 C13 56.3(10) . . . . ? C16 C17 C18 Ru -52.9(9) . . . . ? C1 Ru C18 C13 47.3(8) . . . . ? N1 Ru C18 C13 125.5(7) . . . . ? C14 Ru C18 C13 -32.3(7) . . . . ? C15 Ru C18 C13 -69.8(7) . . . . ? C17 Ru C18 C13 -133.9(10) . . . . ? C16 Ru C18 C13 -105.6(8) . . . . ? I1 Ru C18 C13 -154.0(6) . . . . ? C1 Ru C18 C17 -178.8(7) . . . . ? N1 Ru C18 C17 -100.6(7) . . . . ? C14 Ru C18 C17 101.6(8) . . . . ? C15 Ru C18 C17 64.1(8) . . . . ? C13 Ru C18 C17 133.9(10) . . . . ? C16 Ru C18 C17 28.3(7) . . . . ? I1 Ru C18 C17 -20.1(10) . . . . ? C18 C13 C19 C21 152.0(11) . . . . ? C14 C13 C19 C21 -30.0(16) . . . . ? Ru C13 C19 C21 60.4(16) . . . . ? C18 C13 C19 C22 -83.4(14) . . . . ? C14 C13 C19 C22 94.5(13) . . . . ? Ru C13 C19 C22 -175.1(9) . . . . ? C1A Ru1A N1A C5A 62.3(7) . . . . ? C14A Ru1A N1A C5A -22.9(17) . . . . ? C16A Ru1A N1A C5A -56.1(8) . . . . ? C15A Ru1A N1A C5A -26.2(9) . . . . ? C13A Ru1A N1A C5A -128.7(11) . . . . ? C17A Ru1A N1A C5A -93.2(8) . . . . ? C18A Ru1A N1A C5A -120.2(9) . . . . ? I1A Ru1A N1A C5A 153.9(7) . . . . ? C3A N3A C1A N2A -0.5(12) . . . . ? C10A N3A C1A N2A -179.9(10) . . . . ? C3A N3A C1A Ru1A 179.7(9) . . . . ? C10A N3A C1A Ru1A 0.2(17) . . . . ? C2A N2A C1A N3A -0.6(12) . . . . ? C4A N2A C1A N3A 179.9(9) . . . . ? C2A N2A C1A Ru1A 179.3(8) . . . . ? C4A N2A C1A Ru1A -0.2(15) . . . . ? N1A Ru1A C1A N3A 141.7(11) . . . . ? C14A Ru1A C1A N3A -59.1(12) . . . . ? C16A Ru1A C1A N3A -127.7(11) . . . . ? C15A Ru1A C1A N3A -98.3(11) . . . . ? C13A Ru1A C1A N3A -31.7(14) . . . . ? C17A Ru1A C1A N3A -137.5(13) . . . . ? C18A Ru1A C1A N3A -31(3) . . . . ? I1A Ru1A C1A N3A 59.3(11) . . . . ? N1A Ru1A C1A N2A -38.1(9) . . . . ? C14A Ru1A C1A N2A 121.0(10) . . . . ? C16A Ru1A C1A N2A 52.4(10) . . . . ? C15A Ru1A C1A N2A 81.9(10) . . . . ? C13A Ru1A C1A N2A 148.5(9) . . . . ? C17A Ru1A C1A N2A 42.7(17) . . . . ? C18A Ru1A C1A N2A 149(2) . . . . ? I1A Ru1A C1A N2A -120.5(9) . . . . ? C1A N2A C2A C3A 1.4(13) . . . . ? C4A N2A C2A C3A -179.1(10) . . . . ? N2A C2A C3A N3A -1.7(13) . . . . ? C1A N3A C3A C2A 1.4(14) . . . . ? C10A N3A C3A C2A -179.1(10) . . . . ? C1A N2A C4A C9A -149.0(11) . . . . ? C2A N2A C4A C9A 31.5(15) . . . . ? C1A N2A C4A C5A 31.6(16) . . . . ? C2A N2A C4A C5A -147.8(11) . . . . ? C9A C4A C5A C6A -0.3(16) . . . . ? N2A C4A C5A C6A 179.1(9) . . . . ? C9A C4A C5A N1A -179.1(9) . . . . ? N2A C4A C5A N1A 0.2(15) . . . . ? Ru1A N1A C5A C4A -55.0(11) . . . . ? Ru1A N1A C5A C6A 126.2(9) . . . . ? C4A C5A C6A C7A 0.1(16) . . . . ? N1A C5A C6A C7A 178.9(10) . . . . ? C5A C6A C7A C8A 0.0(16) . . . . ? C6A C7A C8A C9A 0.0(17) . . . . ? C7A C8A C9A C4A -0.2(17) . . . . ? C5A C4A C9A C8A 0.3(17) . . . . ? N2A C4A C9A C8A -179.0(10) . . . . ? C1A N3A C10A C11A -120.2(13) . . . . ? C3A N3A C10A C11A 60.5(15) . . . . ? C1A N3A C10A C12A 115.6(13) . . . . ? C3A N3A C10A C12A -63.8(15) . . . . ? C1A Ru1A C13A C18A 179.6(11) . . . . ? N1A Ru1A C13A C18A 13.4(19) . . . . ? C14A Ru1A C13A C18A -134.0(17) . . . . ? C16A Ru1A C13A C18A -63.7(12) . . . . ? C15A Ru1A C13A C18A -102.2(13) . . . . ? C17A Ru1A C13A C18A -27.5(12) . . . . ? I1A Ru1A C13A C18A 88.8(12) . . . . ? C1A Ru1A C13A C14A -46.4(12) . . . . ? N1A Ru1A C13A C14A 147.3(10) . . . . ? C16A Ru1A C13A C14A 70.2(9) . . . . ? C15A Ru1A C13A C14A 31.8(9) . . . . ? C17A Ru1A C13A C14A 106.5(10) . . . . ? C18A Ru1A C13A C14A 134.0(17) . . . . ? I1A Ru1A C13A C14A -137.2(9) . . . . ? C18A C13A C14A C15A 1(2) . . . . ? Ru1A C13A C14A C15A -56.9(11) . . . . ? C18A C13A C14A Ru1A 58.0(16) . . . . ? C1A Ru1A C14A C13A 144.9(11) . . . . ? N1A Ru1A C14A C13A -133.3(16) . . . . ? C16A Ru1A C14A C13A -97.1(11) . . . . ? C15A Ru1A C14A C13A -128.8(14) . . . . ? C17A Ru1A C14A C13A -59.9(10) . . . . ? C18A Ru1A C14A C13A -26.4(11) . . . . ? I1A Ru1A C14A C13A 50.4(11) . . . . ? C1A Ru1A C14A C15A -86.4(9) . . . . ? N1A Ru1A C14A C15A -4.5(19) . . . . ? C16A Ru1A C14A C15A 31.7(8) . . . . ? C13A Ru1A C14A C15A 128.8(14) . . . . ? C17A Ru1A C14A C15A 68.8(9) . . . . ? C18A Ru1A C14A C15A 102.3(10) . . . . ? I1A Ru1A C14A C15A 179.1(7) . . . . ? C13A C14A C15A C16A 1.7(18) . . . . ? Ru1A C14A C15A C16A -55.2(10) . . . . ? C13A C14A C15A C19A -174.0(15) . . . . ? Ru1A C14A C15A C19A 129.0(13) . . . . ? C13A C14A C15A Ru1A 56.9(11) . . . . ? C1A Ru1A C15A C16A -135.1(9) . . . . ? N1A Ru1A C15A C16A -54.7(9) . . . . ? C14A Ru1A C15A C16A 127.2(12) . . . . ? C13A Ru1A C15A C16A 95.5(11) . . . . ? C17A Ru1A C15A C16A 28.3(8) . . . . ? C18A Ru1A C15A C16A 61.0(10) . . . . ? I1A Ru1A C15A C16A 125.2(11) . . . . ? C1A Ru1A C15A C14A 97.7(9) . . . . ? N1A Ru1A C15A C14A 178.2(8) . . . . ? C16A Ru1A C15A C14A -127.2(12) . . . . ? C13A Ru1A C15A C14A -31.7(10) . . . . ? C17A Ru1A C15A C14A -98.9(10) . . . . ? C18A Ru1A C15A C14A -66.2(10) . . . . ? I1A Ru1A C15A C14A -2.0(16) . . . . ? C1A Ru1A C15A C19A -3.0(19) . . . . ? N1A Ru1A C15A C19A 77(2) . . . . ? C14A Ru1A C15A C19A -101(2) . . . . ? C16A Ru1A C15A C19A 132(2) . . . . ? C13A Ru1A C15A C19A -132(2) . . . . ? C17A Ru1A C15A C19A 160(2) . . . . ? C18A Ru1A C15A C19A -167(2) . . . . ? I1A Ru1A C15A C19A -102.7(19) . . . . ? C14A C15A C16A C17A -3.4(19) . . . . ? C19A C15A C16A C17A 171.1(17) . . . . ? Ru1A C15A C16A C17A -58.1(12) . . . . ? C14A C15A C16A Ru1A 54.6(10) . . . . ? C19A C15A C16A Ru1A -130.8(19) . . . . ? C1A Ru1A C16A C15A 53.5(10) . . . . ? N1A Ru1A C16A C15A 134.9(8) . . . . ? C14A Ru1A C16A C15A -33.0(9) . . . . ? C13A Ru1A C16A C15A -73.0(10) . . . . ? C17A Ru1A C16A C15A -133.2(13) . . . . ? C18A Ru1A C16A C15A -107.5(11) . . . . ? I1A Ru1A C16A C15A -140.8(8) . . . . ? C1A Ru1A C16A C17A -173.2(9) . . . . ? N1A Ru1A C16A C17A -91.9(9) . . . . ? C14A Ru1A C16A C17A 100.2(10) . . . . ? C15A Ru1A C16A C17A 133.2(13) . . . . ? C13A Ru1A C16A C17A 60.3(10) . . . . ? C18A Ru1A C16A C17A 25.7(10) . . . . ? I1A Ru1A C16A C17A -7.6(13) . . . . ? C15A C16A C17A C18A 2(2) . . . . ? Ru1A C16A C17A C18A -54.3(15) . . . . ? C15A C16A C17A Ru1A 56.7(12) . . . . ? C1A Ru1A C17A C18A 149.3(14) . . . . ? N1A Ru1A C17A C18A -133.3(12) . . . . ? C14A Ru1A C17A C18A 66.6(12) . . . . ? C16A Ru1A C17A C18A 135.0(16) . . . . ? C15A Ru1A C17A C18A 106.3(13) . . . . ? C13A Ru1A C17A C18A 28.4(12) . . . . ? I1A Ru1A C17A C18A -49.1(13) . . . . ? C1A Ru1A C17A C16A 14.3(18) . . . . ? N1A Ru1A C17A C16A 91.7(9) . . . . ? C14A Ru1A C17A C16A -68.4(9) . . . . ? C15A Ru1A C17A C16A -28.7(8) . . . . ? C13A Ru1A C17A C16A -106.6(10) . . . . ? C18A Ru1A C17A C16A -135.0(16) . . . . ? I1A Ru1A C17A C16A 175.9(7) . . . . ? C16A C17A C18A C13A 1(3) . . . . ? Ru1A C17A C18A C13A -50.2(16) . . . . ? C16A C17A C18A C20A 177.8(15) . . . . ? Ru1A C17A C18A C20A 127.0(19) . . . . ? C16A C17A C18A Ru1A 50.8(13) . . . . ? C14A C13A C18A C17A -2(3) . . . . ? Ru1A C13A C18A C17A 51.8(16) . . . . ? C14A C13A C18A C20A -179.6(15) . . . . ? Ru1A C13A C18A C20A -125.5(17) . . . . ? C14A C13A C18A Ru1A -54.1(14) . . . . ? C1A Ru1A C18A C17A -134(2) . . . . ? N1A Ru1A C18A C17A 54.5(13) . . . . ? C14A Ru1A C18A C17A -103.1(12) . . . . ? C16A Ru1A C18A C17A -28.1(10) . . . . ? C15A Ru1A C18A C17A -64.3(12) . . . . ? C13A Ru1A C18A C17A -132.6(19) . . . . ? I1A Ru1A C18A C17A 136.0(12) . . . . ? C1A Ru1A C18A C13A -1(3) . . . . ? N1A Ru1A C18A C13A -172.9(10) . . . . ? C14A Ru1A C18A C13A 29.5(11) . . . . ? C16A Ru1A C18A C13A 104.5(13) . . . . ? C15A Ru1A C18A C13A 68.3(12) . . . . ? C17A Ru1A C18A C13A 132.6(19) . . . . ? I1A Ru1A C18A C13A -91.4(12) . . . . ? C1A Ru1A C18A C20A 109(3) . . . . ? N1A Ru1A C18A C20A -63(3) . . . . ? C14A Ru1A C18A C20A 140(3) . . . . ? C16A Ru1A C18A C20A -145(3) . . . . ? C15A Ru1A C18A C20A 178(3) . . . . ? C13A Ru1A C18A C20A 110(3) . . . . ? C17A Ru1A C18A C20A -117(3) . . . . ? I1A Ru1A C18A C20A 19(2) . . . . ? C16A C15A C19A C21A -91(2) . . . . ? C14A C15A C19A C21A 84(2) . . . . ? Ru1A C15A C19A C21A 164.7(15) . . . . ? C16A C15A C19A C22A 11(3) . . . . ? C14A C15A C19A C22A -174.7(14) . . . . ? Ru1A C15A C19A C22A -94(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A I2 0.92 2.78 3.697(9) 175.2 1_554 N1A H1A1 I2A 0.92 2.66 3.564(9) 167.2 1_455 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.183 _refine_diff_density_min -1.139 _refine_diff_density_rms 0.206 #===END data_11014 _database_code_depnum_ccdc_archive 'CCDC 823384' #TrackingRef '- Paper#2 cif files.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Cp*Rh(C,NH2)I]I (6)' _chemical_melting_point ? _chemical_formula_moiety 'C22 H30 N3 I Rh,I,5.5(C H2 Cl2)' _chemical_formula_sum 'C27.50 H41 Cl11 I2 N3 Rh' _chemical_formula_weight 1160.29 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.430(3) _cell_length_b 11.745(4) _cell_length_c 29.671(10) _cell_angle_alpha 89.104(8) _cell_angle_beta 86.111(8) _cell_angle_gamma 75.463(7) _cell_volume 3173.7(19) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 989 _cell_measurement_theta_min 2.261 _cell_measurement_theta_max 28.382 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.428 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2260 _exptl_absorpt_coefficient_mu 3.442 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.535 _exptl_absorpt_correction_T_max 0.831 _exptl_absorpt_process_details ; absorption correction based on 6950 reflections(SADABS);Rint 0.1175 before correction and 0.0619 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25014 _diffrn_reflns_av_R_equivalents 0.1037 _diffrn_reflns_av_sigmaI/netI 0.1606 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12332 _reflns_number_gt 6843 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Disordered CH2Cl2 was omitted using the SQUEEZE option of PLATON.The solvent accessible voids are 1005.4 A3 with an estimated 935e/cell to be added. Twenty two solvent CH2Cl2 molecules/unit cell accounting for 924e were included in the formula, FWt, (000) and density calculations. PLATON Reference: Spek, A.L. (1990), Acta Cryst. A46,C-34. 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. ; _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^)+(0.1135P)^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_number_reflns 12332 _refine_ls_number_parameters 519 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1193 _refine_ls_R_factor_gt 0.0840 _refine_ls_wR_factor_ref 0.2301 _refine_ls_wR_factor_gt 0.2165 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.937 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 I2A I 0.90227(12) 0.86609(8) 0.08058(3) 0.0425(3) Uani 1 1 d . . . Rh1 Rh 0.52910(11) 0.47805(9) 0.35438(3) 0.0270(2) Uani 1 1 d . . . I1 I 0.23530(9) 0.54607(8) 0.34916(3) 0.0370(2) Uani 1 1 d . . . N1 N 0.4891(12) 0.5608(9) 0.4187(3) 0.033(3) Uani 1 1 d . . . H1A H 0.4796 0.6401 0.4146 0.040 Uiso 1 1 calc R . . H1B H 0.4009 0.5515 0.4313 0.040 Uiso 1 1 calc R . . N2 N 0.5706(13) 0.3243(9) 0.4361(3) 0.033(3) Uani 1 1 d . . . N3 N 0.4660(11) 0.2428(9) 0.3883(4) 0.031(2) Uani 1 1 d . . . C1 C 0.5231(13) 0.3357(10) 0.3941(4) 0.026(3) Uani 1 1 d . . . C2 C 0.5497(15) 0.2212(13) 0.4566(5) 0.041(3) Uani 1 1 d . . . H2 H 0.5781 0.1920 0.4856 0.049 Uiso 1 1 calc R . . C3 C 0.4789(17) 0.1702(12) 0.4261(5) 0.043(4) Uani 1 1 d . . . H3 H 0.4461 0.1003 0.4301 0.052 Uiso 1 1 calc R . . C4 C 0.6405(15) 0.4018(12) 0.4580(4) 0.035(3) Uani 1 1 d . . . C5 C 0.5955(16) 0.5195(13) 0.4487(4) 0.037(3) Uani 1 1 d . . . C6 C 0.6736(14) 0.5964(12) 0.4673(5) 0.039(3) Uani 1 1 d . . . H6 H 0.6526 0.6772 0.4593 0.047 Uiso 1 1 calc R . . C7 C 0.7788(14) 0.5511(13) 0.4968(5) 0.040(4) Uani 1 1 d . . . H7 H 0.8261 0.6029 0.5105 0.048 Uiso 1 1 calc R . . C8 C 0.8182(16) 0.4358(14) 0.5072(5) 0.044(4) Uani 1 1 d . . . H8 H 0.8914 0.4079 0.5280 0.053 Uiso 1 1 calc R . . C9 C 0.7490(16) 0.3545(14) 0.4867(5) 0.046(4) Uani 1 1 d . . . H9 H 0.7770 0.2725 0.4927 0.055 Uiso 1 1 calc R . . C10 C 0.3975(16) 0.2165(12) 0.3489(5) 0.041(4) Uani 1 1 d . . . H10 H 0.3959 0.2800 0.3259 0.049 Uiso 1 1 calc R . . C11 C 0.2413(15) 0.2098(13) 0.3615(5) 0.045(4) Uani 1 1 d . . . H11A H 0.2425 0.1438 0.3823 0.068 Uiso 1 1 calc R . . H11B H 0.1938 0.1979 0.3342 0.068 Uiso 1 1 calc R . . H11C H 0.1866 0.2832 0.3763 0.068 Uiso 1 1 calc R . . C12 C 0.4816(18) 0.0964(14) 0.3275(5) 0.055(4) Uani 1 1 d . . . H12A H 0.5834 0.0769 0.3361 0.082 Uiso 1 1 calc R . . H12B H 0.4802 0.1015 0.2946 0.082 Uiso 1 1 calc R . . H12C H 0.4342 0.0350 0.3385 0.082 Uiso 1 1 calc R . . C13 C 0.7079(16) 0.3829(12) 0.3083(4) 0.037(3) Uani 1 1 d . . . C14 C 0.7610(14) 0.4593(15) 0.3348(5) 0.045(4) Uani 1 1 d . . . C15 C 0.6798(17) 0.5795(12) 0.3223(5) 0.042(4) Uani 1 1 d . . . C16 C 0.5836(18) 0.5696(13) 0.2918(5) 0.049(4) Uani 1 1 d . . . C17 C 0.5877(16) 0.4520(12) 0.2836(4) 0.036(3) Uani 1 1 d . . . C18 C 0.7773(19) 0.2543(17) 0.3067(7) 0.076(6) Uani 1 1 d . . . H18A H 0.8710 0.2397 0.2886 0.114 Uiso 1 1 calc R . . H18B H 0.7120 0.2137 0.2929 0.114 Uiso 1 1 calc R . . H18C H 0.7947 0.2247 0.3374 0.114 Uiso 1 1 calc R . . C19 C 0.8813(18) 0.434(2) 0.3636(6) 0.081(7) Uani 1 1 d . . . H19A H 0.9173 0.3483 0.3668 0.121 Uiso 1 1 calc R . . H19B H 0.8481 0.4691 0.3934 0.121 Uiso 1 1 calc R . . H19C H 0.9607 0.4662 0.3503 0.121 Uiso 1 1 calc R . . C20 C 0.706(2) 0.6946(15) 0.3424(8) 0.089(7) Uani 1 1 d . . . H20A H 0.7765 0.7229 0.3223 0.133 Uiso 1 1 calc R . . H20B H 0.7451 0.6778 0.3722 0.133 Uiso 1 1 calc R . . H20C H 0.6129 0.7549 0.3453 0.133 Uiso 1 1 calc R . . C21 C 0.482(2) 0.6774(17) 0.2693(7) 0.086(7) Uani 1 1 d . . . H21A H 0.4519 0.7424 0.2910 0.129 Uiso 1 1 calc R . . H21B H 0.3944 0.6557 0.2598 0.129 Uiso 1 1 calc R . . H21C H 0.5347 0.7019 0.2428 0.129 Uiso 1 1 calc R . . C22 C 0.5067(18) 0.408(2) 0.2498(5) 0.097(9) Uani 1 1 d . . . H22A H 0.4059 0.4136 0.2620 0.145 Uiso 1 1 calc R . . H22B H 0.5555 0.3257 0.2427 0.145 Uiso 1 1 calc R . . H22C H 0.5048 0.4554 0.2222 0.145 Uiso 1 1 calc R . . I2 I 0.35296(13) 0.87561(8) 0.42241(4) 0.0512(3) Uani 1 1 d . . . Rh1A Rh 0.06690(11) 0.46831(8) 0.14170(3) 0.0256(2) Uani 1 1 d . . . I1A I -0.22466(10) 0.53458(8) 0.16433(3) 0.0367(2) Uani 1 1 d . . . N1A N 0.0102(12) 0.5522(9) 0.0794(3) 0.031(2) Uani 1 1 d . . . H1A1 H -0.0802 0.5429 0.0729 0.038 Uiso 1 1 calc R . . H1A2 H 0.0017 0.6315 0.0826 0.038 Uiso 1 1 calc R . . N2A N 0.0909(11) 0.3153(8) 0.0612(3) 0.027(2) Uani 1 1 d . . . N3A N -0.0029(12) 0.2315(9) 0.1172(3) 0.032(2) Uani 1 1 d . . . C1A C 0.0482(14) 0.3252(10) 0.1055(4) 0.027(3) Uani 1 1 d . . . C2A C 0.067(2) 0.2077(14) 0.0448(5) 0.056(4) Uani 1 1 d . . . H2A H 0.0876 0.1769 0.0150 0.067 Uiso 1 1 calc R . . C3A C 0.0084(17) 0.1596(12) 0.0811(4) 0.040(3) Uani 1 1 d . . . H3A H -0.0200 0.0875 0.0812 0.048 Uiso 1 1 calc R . . C4A C 0.1574(13) 0.3908(11) 0.0338(4) 0.029(3) Uani 1 1 d . . . C5A C 0.1130(14) 0.5091(11) 0.0421(4) 0.033(3) Uani 1 1 d . . . C6A C 0.1852(16) 0.5854(12) 0.0165(4) 0.037(3) Uani 1 1 d . . . H6A H 0.1672 0.6660 0.0245 0.044 Uiso 1 1 calc R . . C7A C 0.2788(16) 0.5412(14) -0.0189(5) 0.044(4) Uani 1 1 d . . . H7A H 0.3138 0.5934 -0.0390 0.053 Uiso 1 1 calc R . . C8A C 0.3246(18) 0.4223(19) -0.0267(5) 0.062(5) Uani 1 1 d . . . H8A H 0.3985 0.3942 -0.0501 0.074 Uiso 1 1 calc R . . C9A C 0.2641(15) 0.3377(13) -0.0004(4) 0.038(3) Uani 1 1 d . . . H9A H 0.2934 0.2553 -0.0057 0.046 Uiso 1 1 calc R . . C10A C -0.0641(14) 0.2031(10) 0.1610(4) 0.029(3) Uani 1 1 d . . . H10A H -0.0598 0.2665 0.1826 0.034 Uiso 1 1 calc R . . C11A C -0.2330(16) 0.2054(14) 0.1574(5) 0.050(4) Uani 1 1 d . . . H11D H -0.2844 0.2807 0.1447 0.075 Uiso 1 1 calc R . . H11E H -0.2777 0.1958 0.1876 0.075 Uiso 1 1 calc R . . H11F H -0.2407 0.1411 0.1378 0.075 Uiso 1 1 calc R . . C12A C 0.0178(18) 0.0881(13) 0.1802(5) 0.054(4) Uani 1 1 d . . . H12D H 0.0194 0.0243 0.1591 0.080 Uiso 1 1 calc R . . H12E H -0.0312 0.0737 0.2091 0.080 Uiso 1 1 calc R . . H12F H 0.1186 0.0912 0.1849 0.080 Uiso 1 1 calc R . . C13A C 0.2548(16) 0.3718(11) 0.1756(4) 0.037(3) Uani 1 1 d . . . C14A C 0.2949(16) 0.4603(15) 0.1454(5) 0.046(4) Uani 1 1 d . . . C15A C 0.2227(17) 0.5687(13) 0.1628(5) 0.044(4) Uani 1 1 d . . . C16A C 0.1284(18) 0.5598(14) 0.1991(6) 0.053(4) Uani 1 1 d . . . C17A C 0.1432(16) 0.4318(12) 0.2078(4) 0.037(3) Uani 1 1 d . . . C18A C 0.3252(18) 0.2483(15) 0.1724(6) 0.062(5) Uani 1 1 d . . . H18D H 0.2696 0.2042 0.1918 0.093 Uiso 1 1 calc R . . H18E H 0.4254 0.2341 0.1821 0.093 Uiso 1 1 calc R . . H18F H 0.3286 0.2224 0.1410 0.093 Uiso 1 1 calc R . . C19A C 0.4180(15) 0.4322(16) 0.1102(5) 0.055(4) Uani 1 1 d . . . H19D H 0.3832 0.4645 0.0812 0.082 Uiso 1 1 calc R . . H19E H 0.4553 0.3466 0.1076 0.082 Uiso 1 1 calc R . . H19F H 0.4969 0.4668 0.1186 0.082 Uiso 1 1 calc R . . C20A C 0.233(2) 0.6835(15) 0.1446(7) 0.075(6) Uani 1 1 d . . . H20D H 0.3187 0.7041 0.1559 0.113 Uiso 1 1 calc R . . H20E H 0.1440 0.7435 0.1541 0.113 Uiso 1 1 calc R . . H20F H 0.2436 0.6796 0.1115 0.113 Uiso 1 1 calc R . . C21A C 0.031(2) 0.6592(17) 0.2288(7) 0.087(7) Uani 1 1 d . . . H21D H 0.0830 0.6707 0.2551 0.131 Uiso 1 1 calc R . . H21E H -0.0603 0.6379 0.2390 0.131 Uiso 1 1 calc R . . H21F H 0.0073 0.7321 0.2113 0.131 Uiso 1 1 calc R . . C22A C 0.0867(19) 0.3741(18) 0.2460(5) 0.068(5) Uani 1 1 d . . . H22D H 0.1056 0.2897 0.2397 0.102 Uiso 1 1 calc R . . H22E H -0.0192 0.4077 0.2510 0.102 Uiso 1 1 calc R . . H22F H 0.1356 0.3857 0.2730 0.102 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 I2A 0.0643(7) 0.0251(5) 0.0384(6) -0.0058(4) 0.0013(4) -0.0125(4) Rh1 0.0244(5) 0.0262(5) 0.0309(6) -0.0009(4) 0.0029(4) -0.0084(4) I1 0.0262(5) 0.0375(5) 0.0465(6) -0.0006(4) -0.0021(4) -0.0067(4) N1 0.038(7) 0.035(6) 0.025(6) -0.011(5) 0.010(5) -0.010(5) N2 0.052(7) 0.021(6) 0.028(6) 0.005(5) 0.004(5) -0.014(5) N3 0.018(5) 0.027(6) 0.044(7) -0.009(5) 0.001(5) 0.000(4) C1 0.032(7) 0.022(6) 0.027(7) 0.001(5) 0.004(5) -0.014(5) C2 0.036(8) 0.042(9) 0.045(9) -0.006(7) -0.005(6) -0.008(7) C3 0.060(10) 0.028(8) 0.044(9) 0.009(6) 0.000(7) -0.016(7) C4 0.036(8) 0.041(8) 0.028(7) 0.002(6) 0.010(6) -0.010(6) C5 0.059(10) 0.045(9) 0.012(7) -0.005(6) 0.007(6) -0.020(7) C6 0.022(7) 0.035(8) 0.060(10) 0.004(7) -0.001(6) -0.010(6) C7 0.026(8) 0.055(10) 0.048(9) -0.016(7) 0.008(6) -0.030(7) C8 0.044(9) 0.063(11) 0.028(8) 0.001(7) -0.004(6) -0.016(8) C9 0.047(9) 0.053(10) 0.033(8) -0.013(7) 0.004(7) -0.005(8) C10 0.049(9) 0.032(8) 0.047(9) -0.009(6) -0.016(7) -0.017(7) C11 0.033(8) 0.051(10) 0.055(10) -0.002(7) 0.000(7) -0.018(7) C12 0.062(11) 0.051(10) 0.058(11) -0.008(8) -0.001(8) -0.026(9) C13 0.048(9) 0.035(8) 0.026(7) 0.002(6) 0.009(6) -0.011(7) C14 0.014(7) 0.085(12) 0.037(8) -0.013(8) 0.008(6) -0.014(7) C15 0.058(10) 0.032(8) 0.042(9) -0.003(6) 0.016(7) -0.026(7) C16 0.054(10) 0.043(9) 0.047(10) 0.021(7) 0.013(8) -0.014(8) C17 0.062(10) 0.032(8) 0.028(7) 0.000(6) 0.015(6) -0.039(7) C18 0.037(10) 0.081(14) 0.092(15) 0.007(11) 0.008(9) 0.014(9) C19 0.038(10) 0.15(2) 0.061(12) 0.000(12) 0.012(8) -0.044(12) C20 0.085(15) 0.044(11) 0.144(19) -0.033(11) 0.056(13) -0.044(11) C21 0.074(14) 0.085(15) 0.083(14) 0.050(12) 0.032(11) -0.006(11) C22 0.039(10) 0.22(3) 0.033(10) -0.046(13) 0.000(8) -0.025(13) I2 0.0762(8) 0.0284(5) 0.0510(6) 0.0078(4) -0.0159(5) -0.0144(5) Rh1A 0.0279(5) 0.0229(5) 0.0269(6) -0.0028(4) -0.0013(4) -0.0079(4) I1A 0.0308(5) 0.0341(5) 0.0431(6) -0.0060(4) 0.0068(4) -0.0065(4) N1A 0.038(6) 0.020(5) 0.040(7) 0.000(5) -0.010(5) -0.012(5) N2A 0.036(6) 0.013(5) 0.028(6) -0.009(4) -0.002(4) 0.001(4) N3A 0.041(7) 0.024(6) 0.027(6) -0.008(5) -0.001(5) -0.004(5) C1A 0.036(7) 0.010(6) 0.030(7) -0.005(5) -0.006(5) 0.006(5) C2A 0.085(13) 0.046(10) 0.032(9) 0.000(7) -0.014(8) -0.007(9) C3A 0.068(10) 0.025(7) 0.034(8) -0.004(6) -0.006(7) -0.026(7) C4A 0.025(7) 0.035(8) 0.025(7) -0.009(6) 0.007(5) -0.004(6) C5A 0.035(8) 0.030(7) 0.027(7) 0.006(6) -0.003(6) 0.004(6) C6A 0.049(9) 0.033(8) 0.034(8) -0.002(6) 0.001(6) -0.021(7) C7A 0.046(9) 0.044(9) 0.040(9) 0.008(7) 0.004(7) -0.010(7) C8A 0.046(10) 0.114(17) 0.036(9) 0.005(10) 0.004(7) -0.043(11) C9A 0.036(8) 0.039(8) 0.032(8) -0.011(6) -0.005(6) 0.007(6) C10A 0.038(8) 0.020(6) 0.034(8) 0.001(5) -0.009(6) -0.015(6) C11A 0.045(9) 0.055(10) 0.056(10) -0.009(8) 0.007(7) -0.026(8) C12A 0.059(11) 0.047(10) 0.057(11) 0.021(8) 0.000(8) -0.020(8) C13A 0.049(9) 0.025(7) 0.034(8) -0.005(6) -0.009(6) -0.004(6) C14A 0.035(8) 0.069(11) 0.044(9) 0.011(8) -0.015(7) -0.030(8) C15A 0.060(10) 0.038(9) 0.053(10) -0.007(7) -0.008(8) -0.043(8) C16A 0.049(10) 0.044(9) 0.061(11) -0.026(8) -0.019(8) 0.006(8) C17A 0.059(10) 0.043(8) 0.018(7) -0.002(6) 0.008(6) -0.034(7) C18A 0.060(11) 0.067(12) 0.062(11) -0.004(9) -0.035(9) -0.015(9) C19A 0.025(8) 0.095(14) 0.049(10) -0.008(9) -0.002(7) -0.025(8) C20A 0.095(15) 0.051(11) 0.099(15) 0.013(10) -0.051(12) -0.044(11) C21A 0.060(12) 0.079(14) 0.107(16) -0.054(12) -0.042(11) 0.026(11) C22A 0.066(12) 0.111(16) 0.030(9) 0.003(9) -0.016(8) -0.024(11) _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 C1 2.041(12) . ? Rh1 N1 2.121(9) . ? Rh1 C17 2.143(12) . ? Rh1 C13 2.179(13) . ? Rh1 C14 2.182(12) . ? Rh1 C16 2.226(13) . ? Rh1 C15 2.231(13) . ? Rh1 I1 2.6985(16) . ? N1 C5 1.379(17) . ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? N2 C1 1.347(15) . ? N2 C2 1.398(17) . ? N2 C4 1.435(17) . ? N3 C1 1.350(14) . ? N3 C3 1.390(17) . ? N3 C10 1.449(16) . ? C2 C3 1.388(19) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C5 1.370(19) . ? C4 C9 1.378(19) . ? C5 C6 1.438(18) . ? C6 C7 1.367(19) . ? C6 H6 0.9500 . ? C7 C8 1.35(2) . ? C7 H7 0.9500 . ? C8 C9 1.45(2) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.516(19) . ? C10 C12 1.55(2) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.404(19) . ? C13 C17 1.45(2) . ? C13 C18 1.49(2) . ? C14 C19 1.44(2) . ? C14 C15 1.48(2) . ? C15 C16 1.35(2) . ? C15 C20 1.57(2) . ? C16 C17 1.397(19) . ? C16 C21 1.56(2) . ? C17 C22 1.47(2) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? Rh1A C1A 2.060(11) . ? Rh1A N1A 2.118(10) . ? Rh1A C17A 2.136(13) . ? Rh1A C14A 2.139(13) . ? Rh1A C13A 2.153(14) . ? Rh1A C16A 2.212(14) . ? Rh1A C15A 2.227(12) . ? Rh1A I1A 2.7034(16) . ? N1A C5A 1.431(16) . ? N1A H1A1 0.9200 . ? N1A H1A2 0.9200 . ? N2A C1A 1.346(15) . ? N2A C4A 1.423(16) . ? N2A C2A 1.435(18) . ? N3A C1A 1.340(15) . ? N3A C3A 1.357(15) . ? N3A C10A 1.456(16) . ? C2A C3A 1.36(2) . ? C2A H2A 0.9500 . ? C3A H3A 0.9500 . ? C4A C5A 1.369(17) . ? C4A C9A 1.413(16) . ? C5A C6A 1.434(18) . ? C6A C7A 1.348(19) . ? C6A H6A 0.9500 . ? C7A C8A 1.37(2) . ? C7A H7A 0.9500 . ? C8A C9A 1.46(2) . ? C8A H8A 0.9500 . ? C9A H9A 0.9500 . ? C10A C12A 1.502(18) . ? C10A C11A 1.597(18) . ? C10A H10A 1.0000 . ? C11A H11D 0.9800 . ? C11A H11E 0.9800 . ? C11A H11F 0.9800 . ? C12A H12D 0.9800 . ? C12A H12E 0.9800 . ? C12A H12F 0.9800 . ? C13A C17A 1.425(18) . ? C13A C18A 1.44(2) . ? C13A C14A 1.466(19) . ? C14A C15A 1.37(2) . ? C14A C19A 1.48(2) . ? C15A C16A 1.37(2) . ? C15A C20A 1.47(2) . ? C16A C17A 1.50(2) . ? C16A C21A 1.54(2) . ? C17A C22A 1.45(2) . ? C18A H18D 0.9800 . ? C18A H18E 0.9800 . ? C18A H18F 0.9800 . ? C19A H19D 0.9800 . ? C19A H19E 0.9800 . ? C19A H19F 0.9800 . ? C20A H20D 0.9800 . ? C20A H20E 0.9800 . ? C20A H20F 0.9800 . ? C21A H21D 0.9800 . ? C21A H21E 0.9800 . ? C21A H21F 0.9800 . ? C22A H22D 0.9800 . ? C22A H22E 0.9800 . ? C22A H22F 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 C1 Rh1 N1 80.4(5) . . ? C1 Rh1 C17 119.0(5) . . ? N1 Rh1 C17 159.8(4) . . ? C1 Rh1 C13 94.8(5) . . ? N1 Rh1 C13 141.4(5) . . ? C17 Rh1 C13 39.3(5) . . ? C1 Rh1 C14 105.2(6) . . ? N1 Rh1 C14 106.5(5) . . ? C17 Rh1 C14 65.0(5) . . ? C13 Rh1 C14 37.6(5) . . ? C1 Rh1 C16 155.4(5) . . ? N1 Rh1 C16 122.7(5) . . ? C17 Rh1 C16 37.2(5) . . ? C13 Rh1 C16 62.2(5) . . ? C14 Rh1 C16 62.7(6) . . ? C1 Rh1 C15 143.2(6) . . ? N1 Rh1 C15 98.9(5) . . ? C17 Rh1 C15 62.5(5) . . ? C13 Rh1 C15 62.8(5) . . ? C14 Rh1 C15 39.2(6) . . ? C16 Rh1 C15 35.3(6) . . ? C1 Rh1 I1 94.3(3) . . ? N1 Rh1 I1 85.6(3) . . ? C17 Rh1 I1 97.6(4) . . ? C13 Rh1 I1 133.0(4) . . ? C14 Rh1 I1 158.4(4) . . ? C16 Rh1 I1 95.8(4) . . ? C15 Rh1 I1 122.5(4) . . ? C5 N1 Rh1 115.3(8) . . ? C5 N1 H1A 108.5 . . ? Rh1 N1 H1A 108.5 . . ? C5 N1 H1B 108.5 . . ? Rh1 N1 H1B 108.5 . . ? H1A N1 H1B 107.5 . . ? C1 N2 C2 111.1(11) . . ? C1 N2 C4 126.7(10) . . ? C2 N2 C4 122.2(11) . . ? C1 N3 C3 111.7(11) . . ? C1 N3 C10 127.0(11) . . ? C3 N3 C10 121.2(12) . . ? N2 C1 N3 105.5(10) . . ? N2 C1 Rh1 122.5(8) . . ? N3 C1 Rh1 131.8(9) . . ? C3 C2 N2 106.0(13) . . ? C3 C2 H2 127.0 . . ? N2 C2 H2 127.0 . . ? C2 C3 N3 105.5(12) . . ? C2 C3 H3 127.2 . . ? N3 C3 H3 127.2 . . ? C5 C4 C9 123.6(14) . . ? C5 C4 N2 117.6(12) . . ? C9 C4 N2 118.8(13) . . ? C4 C5 N1 120.7(13) . . ? C4 C5 C6 117.9(14) . . ? N1 C5 C6 121.1(13) . . ? C7 C6 C5 118.8(13) . . ? C7 C6 H6 120.6 . . ? C5 C6 H6 120.6 . . ? C8 C7 C6 122.6(13) . . ? C8 C7 H7 118.7 . . ? C6 C7 H7 118.7 . . ? C7 C8 C9 120.0(14) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C4 C9 C8 116.7(14) . . ? C4 C9 H9 121.6 . . ? C8 C9 H9 121.6 . . ? N3 C10 C11 110.3(12) . . ? N3 C10 C12 111.5(12) . . ? C11 C10 C12 107.6(11) . . ? N3 C10 H10 109.1 . . ? C11 C10 H10 109.1 . . ? C12 C10 H10 109.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C17 108.7(12) . . ? C14 C13 C18 121.6(15) . . ? C17 C13 C18 129.6(14) . . ? C14 C13 Rh1 71.3(7) . . ? C17 C13 Rh1 69.0(7) . . ? C18 C13 Rh1 128.2(11) . . ? C13 C14 C19 129.6(17) . . ? C13 C14 C15 105.5(12) . . ? C19 C14 C15 124.4(16) . . ? C13 C14 Rh1 71.1(8) . . ? C19 C14 Rh1 127.4(11) . . ? C15 C14 Rh1 72.2(7) . . ? C16 C15 C14 108.0(12) . . ? C16 C15 C20 128.2(16) . . ? C14 C15 C20 123.8(15) . . ? C16 C15 Rh1 72.2(8) . . ? C14 C15 Rh1 68.6(7) . . ? C20 C15 Rh1 124.5(10) . . ? C15 C16 C17 111.5(14) . . ? C15 C16 C21 123.3(16) . . ? C17 C16 C21 125.2(17) . . ? C15 C16 Rh1 72.5(8) . . ? C17 C16 Rh1 68.1(7) . . ? C21 C16 Rh1 126.5(10) . . ? C16 C17 C13 105.9(12) . . ? C16 C17 C22 126.4(17) . . ? C13 C17 C22 126.8(15) . . ? C16 C17 Rh1 74.6(8) . . ? C13 C17 Rh1 71.7(7) . . ? C22 C17 Rh1 127.5(10) . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C1A Rh1A N1A 80.7(4) . . ? C1A Rh1A C17A 115.9(5) . . ? N1A Rh1A C17A 162.6(4) . . ? C1A Rh1A C14A 108.6(6) . . ? N1A Rh1A C14A 105.0(5) . . ? C17A Rh1A C14A 66.2(5) . . ? C1A Rh1A C13A 94.4(5) . . ? N1A Rh1A C13A 141.0(5) . . ? C17A Rh1A C13A 38.8(5) . . ? C14A Rh1A C13A 39.9(5) . . ? C1A Rh1A C16A 155.8(5) . . ? N1A Rh1A C16A 122.8(5) . . ? C17A Rh1A C16A 40.2(5) . . ? C14A Rh1A C16A 62.9(6) . . ? C13A Rh1A C16A 64.3(5) . . ? C1A Rh1A C15A 144.5(6) . . ? N1A Rh1A C15A 99.8(5) . . ? C17A Rh1A C15A 63.9(5) . . ? C14A Rh1A C15A 36.6(6) . . ? C13A Rh1A C15A 62.9(5) . . ? C16A Rh1A C15A 35.9(6) . . ? C1A Rh1A I1A 92.7(4) . . ? N1A Rh1A I1A 84.8(3) . . ? C17A Rh1A I1A 98.7(4) . . ? C14A Rh1A I1A 157.7(4) . . ? C13A Rh1A I1A 134.2(4) . . ? C16A Rh1A I1A 94.8(4) . . ? C15A Rh1A I1A 122.8(4) . . ? C5A N1A Rh1A 114.4(8) . . ? C5A N1A H1A1 108.6 . . ? Rh1A N1A H1A1 108.6 . . ? C5A N1A H1A2 108.6 . . ? Rh1A N1A H1A2 108.6 . . ? H1A1 N1A H1A2 107.6 . . ? C1A N2A C4A 128.5(10) . . ? C1A N2A C2A 108.3(11) . . ? C4A N2A C2A 123.1(11) . . ? C1A N3A C3A 110.3(11) . . ? C1A N3A C10A 128.6(10) . . ? C3A N3A C10A 121.1(11) . . ? N3A C1A N2A 107.6(10) . . ? N3A C1A Rh1A 132.2(9) . . ? N2A C1A Rh1A 120.2(8) . . ? C3A C2A N2A 105.1(12) . . ? C3A C2A H2A 127.4 . . ? N2A C2A H2A 127.4 . . ? C2A C3A N3A 108.6(12) . . ? C2A C3A H3A 125.7 . . ? N3A C3A H3A 125.7 . . ? C5A C4A C9A 124.6(13) . . ? C5A C4A N2A 118.1(11) . . ? C9A C4A N2A 117.3(11) . . ? C4A C5A N1A 119.6(11) . . ? C4A C5A C6A 118.6(12) . . ? N1A C5A C6A 121.4(11) . . ? C7A C6A C5A 119.1(13) . . ? C7A C6A H6A 120.4 . . ? C5A C6A H6A 120.4 . . ? C6A C7A C8A 121.4(14) . . ? C6A C7A H7A 119.3 . . ? C8A C7A H7A 119.3 . . ? C7A C8A C9A 122.5(15) . . ? C7A C8A H8A 118.8 . . ? C9A C8A H8A 118.8 . . ? C4A C9A C8A 113.1(13) . . ? C4A C9A H9A 123.5 . . ? C8A C9A H9A 123.5 . . ? N3A C10A C12A 114.1(11) . . ? N3A C10A C11A 109.2(10) . . ? C12A C10A C11A 110.7(11) . . ? N3A C10A H10A 107.5 . . ? C12A C10A H10A 107.5 . . ? C11A C10A H10A 107.5 . . ? C10A C11A H11D 109.5 . . ? C10A C11A H11E 109.5 . . ? H11D C11A H11E 109.5 . . ? C10A C11A H11F 109.5 . . ? H11D C11A H11F 109.5 . . ? H11E C11A H11F 109.5 . . ? C10A C12A H12D 109.5 . . ? C10A C12A H12E 109.5 . . ? H12D C12A H12E 109.5 . . ? C10A C12A H12F 109.5 . . ? H12D C12A H12F 109.5 . . ? H12E C12A H12F 109.5 . . ? C17A C13A C18A 128.9(14) . . ? C17A C13A C14A 107.7(12) . . ? C18A C13A C14A 123.4(14) . . ? C17A C13A Rh1A 70.0(8) . . ? C18A C13A Rh1A 127.9(10) . . ? C14A C13A Rh1A 69.5(7) . . ? C15A C14A C13A 107.1(13) . . ? C15A C14A C19A 128.0(14) . . ? C13A C14A C19A 123.3(15) . . ? C15A C14A Rh1A 75.2(9) . . ? C13A C14A Rh1A 70.6(8) . . ? C19A C14A Rh1A 130.5(10) . . ? C16A C15A C14A 111.8(13) . . ? C16A C15A C20A 121.5(16) . . ? C14A C15A C20A 126.6(16) . . ? C16A C15A Rh1A 71.4(8) . . ? C14A C15A Rh1A 68.2(7) . . ? C20A C15A Rh1A 125.0(11) . . ? C15A C16A C17A 107.5(12) . . ? C15A C16A C21A 128.4(17) . . ? C17A C16A C21A 124.0(17) . . ? C15A C16A Rh1A 72.6(8) . . ? C17A C16A Rh1A 67.2(7) . . ? C21A C16A Rh1A 128.4(11) . . ? C13A C17A C22A 123.4(14) . . ? C13A C17A C16A 105.4(11) . . ? C22A C17A C16A 129.9(14) . . ? C13A C17A Rh1A 71.2(7) . . ? C22A C17A Rh1A 130.7(10) . . ? C16A C17A Rh1A 72.6(8) . . ? C13A C18A H18D 109.5 . . ? C13A C18A H18E 109.5 . . ? H18D C18A H18E 109.5 . . ? C13A C18A H18F 109.5 . . ? H18D C18A H18F 109.5 . . ? H18E C18A H18F 109.5 . . ? C14A C19A H19D 109.5 . . ? C14A C19A H19E 109.5 . . ? H19D C19A H19E 109.5 . . ? C14A C19A H19F 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? C15A C20A H20D 109.5 . . ? C15A C20A H20E 109.5 . . ? H20D C20A H20E 109.5 . . ? C15A C20A H20F 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? C16A C21A H21D 109.5 . . ? C16A C21A H21E 109.5 . . ? H21D C21A H21E 109.5 . . ? C16A C21A H21F 109.5 . . ? H21D C21A H21F 109.5 . . ? H21E C21A H21F 109.5 . . ? C17A C22A H22D 109.5 . . ? C17A C22A H22E 109.5 . . ? H22D C22A H22E 109.5 . . ? C17A C22A H22F 109.5 . . ? H22D C22A H22F 109.5 . . ? H22E C22A H22F 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 C1 Rh1 N1 C5 60.5(10) . . . . ? C17 Rh1 N1 C5 -104.4(16) . . . . ? C13 Rh1 N1 C5 -25.2(13) . . . . ? C14 Rh1 N1 C5 -42.6(11) . . . . ? C16 Rh1 N1 C5 -110.4(10) . . . . ? C15 Rh1 N1 C5 -82.2(10) . . . . ? I1 Rh1 N1 C5 155.6(9) . . . . ? C2 N2 C1 N3 2.5(14) . . . . ? C4 N2 C1 N3 179.8(11) . . . . ? C2 N2 C1 Rh1 177.9(9) . . . . ? C4 N2 C1 Rh1 -4.8(18) . . . . ? C3 N3 C1 N2 -1.1(14) . . . . ? C10 N3 C1 N2 178.5(11) . . . . ? C3 N3 C1 Rh1 -175.9(10) . . . . ? C10 N3 C1 Rh1 3.8(19) . . . . ? N1 Rh1 C1 N2 -33.3(10) . . . . ? C17 Rh1 C1 N2 140.8(10) . . . . ? C13 Rh1 C1 N2 108.1(11) . . . . ? C14 Rh1 C1 N2 71.3(11) . . . . ? C16 Rh1 C1 N2 128.0(14) . . . . ? C15 Rh1 C1 N2 58.8(14) . . . . ? I1 Rh1 C1 N2 -118.1(10) . . . . ? N1 Rh1 C1 N3 140.7(12) . . . . ? C17 Rh1 C1 N3 -45.2(13) . . . . ? C13 Rh1 C1 N3 -77.9(12) . . . . ? C14 Rh1 C1 N3 -114.7(12) . . . . ? C16 Rh1 C1 N3 -58(2) . . . . ? C15 Rh1 C1 N3 -127.2(12) . . . . ? I1 Rh1 C1 N3 56.0(11) . . . . ? C1 N2 C2 C3 -3.0(15) . . . . ? C4 N2 C2 C3 179.6(12) . . . . ? N2 C2 C3 N3 2.1(15) . . . . ? C1 N3 C3 C2 -0.7(15) . . . . ? C10 N3 C3 C2 179.6(12) . . . . ? C1 N2 C4 C5 34.9(18) . . . . ? C2 N2 C4 C5 -148.1(12) . . . . ? C1 N2 C4 C9 -144.6(13) . . . . ? C2 N2 C4 C9 32.4(18) . . . . ? C9 C4 C5 N1 178.1(12) . . . . ? N2 C4 C5 N1 -1.4(18) . . . . ? C9 C4 C5 C6 5(2) . . . . ? N2 C4 C5 C6 -174.6(11) . . . . ? Rh1 N1 C5 C4 -52.8(15) . . . . ? Rh1 N1 C5 C6 120.2(11) . . . . ? C4 C5 C6 C7 -6.4(19) . . . . ? N1 C5 C6 C7 -179.6(12) . . . . ? C5 C6 C7 C8 4(2) . . . . ? C6 C7 C8 C9 0(2) . . . . ? C5 C4 C9 C8 -1(2) . . . . ? N2 C4 C9 C8 178.8(11) . . . . ? C7 C8 C9 C4 -2(2) . . . . ? C1 N3 C10 C11 -121.3(14) . . . . ? C3 N3 C10 C11 58.3(16) . . . . ? C1 N3 C10 C12 119.1(14) . . . . ? C3 N3 C10 C12 -61.2(16) . . . . ? C1 Rh1 C13 C14 -108.8(9) . . . . ? N1 Rh1 C13 C14 -28.1(12) . . . . ? C17 Rh1 C13 C14 119.5(12) . . . . ? C16 Rh1 C13 C14 80.5(10) . . . . ? C15 Rh1 C13 C14 40.5(9) . . . . ? I1 Rh1 C13 C14 150.8(8) . . . . ? C1 Rh1 C13 C17 131.7(7) . . . . ? N1 Rh1 C13 C17 -147.6(7) . . . . ? C14 Rh1 C13 C17 -119.5(12) . . . . ? C16 Rh1 C13 C17 -39.1(8) . . . . ? C15 Rh1 C13 C17 -79.0(8) . . . . ? I1 Rh1 C13 C17 31.2(9) . . . . ? C1 Rh1 C13 C18 7.2(15) . . . . ? N1 Rh1 C13 C18 87.9(16) . . . . ? C17 Rh1 C13 C18 -124.5(18) . . . . ? C14 Rh1 C13 C18 115.9(18) . . . . ? C16 Rh1 C13 C18 -163.6(17) . . . . ? C15 Rh1 C13 C18 156.5(16) . . . . ? I1 Rh1 C13 C18 -93.3(15) . . . . ? C17 C13 C14 C19 -177.5(14) . . . . ? C18 C13 C14 C19 -1(2) . . . . ? Rh1 C13 C14 C19 123.4(16) . . . . ? C17 C13 C14 C15 -5.4(14) . . . . ? C18 C13 C14 C15 171.6(13) . . . . ? Rh1 C13 C14 C15 -64.5(9) . . . . ? C17 C13 C14 Rh1 59.1(9) . . . . ? C18 C13 C14 Rh1 -123.9(14) . . . . ? C1 Rh1 C14 C13 77.9(9) . . . . ? N1 Rh1 C14 C13 162.2(8) . . . . ? C17 Rh1 C14 C13 -37.5(8) . . . . ? C16 Rh1 C14 C13 -79.1(9) . . . . ? C15 Rh1 C14 C13 -114.0(12) . . . . ? I1 Rh1 C14 C13 -75.9(15) . . . . ? C1 Rh1 C14 C19 -48.1(18) . . . . ? N1 Rh1 C14 C19 36.2(18) . . . . ? C17 Rh1 C14 C19 -163.4(19) . . . . ? C13 Rh1 C14 C19 -126(2) . . . . ? C16 Rh1 C14 C19 155.0(19) . . . . ? C15 Rh1 C14 C19 120(2) . . . . ? I1 Rh1 C14 C19 158.1(13) . . . . ? C1 Rh1 C14 C15 -168.2(8) . . . . ? N1 Rh1 C14 C15 -83.9(8) . . . . ? C17 Rh1 C14 C15 76.5(8) . . . . ? C13 Rh1 C14 C15 114.0(12) . . . . ? C16 Rh1 C14 C15 34.9(8) . . . . ? I1 Rh1 C14 C15 38.1(16) . . . . ? C13 C14 C15 C16 2.0(16) . . . . ? C19 C14 C15 C16 174.6(14) . . . . ? Rh1 C14 C15 C16 -61.8(11) . . . . ? C13 C14 C15 C20 -178.2(13) . . . . ? C19 C14 C15 C20 -6(2) . . . . ? Rh1 C14 C15 C20 118.0(13) . . . . ? C13 C14 C15 Rh1 63.8(9) . . . . ? C19 C14 C15 Rh1 -123.6(14) . . . . ? C1 Rh1 C15 C16 137.6(10) . . . . ? N1 Rh1 C15 C16 -136.5(9) . . . . ? C17 Rh1 C15 C16 35.0(9) . . . . ? C13 Rh1 C15 C16 79.5(10) . . . . ? C14 Rh1 C15 C16 118.3(12) . . . . ? I1 Rh1 C15 C16 -46.1(10) . . . . ? C1 Rh1 C15 C14 19.3(12) . . . . ? N1 Rh1 C15 C14 105.2(8) . . . . ? C17 Rh1 C15 C14 -83.3(9) . . . . ? C13 Rh1 C15 C14 -38.8(8) . . . . ? C16 Rh1 C15 C14 -118.3(12) . . . . ? I1 Rh1 C15 C14 -164.4(6) . . . . ? C1 Rh1 C15 C20 -97.8(16) . . . . ? N1 Rh1 C15 C20 -11.9(16) . . . . ? C17 Rh1 C15 C20 159.6(17) . . . . ? C13 Rh1 C15 C20 -155.9(17) . . . . ? C14 Rh1 C15 C20 -117.1(18) . . . . ? C16 Rh1 C15 C20 125(2) . . . . ? I1 Rh1 C15 C20 78.5(16) . . . . ? C14 C15 C16 C17 2.4(17) . . . . ? C20 C15 C16 C17 -177.4(13) . . . . ? Rh1 C15 C16 C17 -57.1(10) . . . . ? C14 C15 C16 C21 -177.8(12) . . . . ? C20 C15 C16 C21 2(2) . . . . ? Rh1 C15 C16 C21 122.7(14) . . . . ? C14 C15 C16 Rh1 59.5(9) . . . . ? C20 C15 C16 Rh1 -120.3(15) . . . . ? C1 Rh1 C16 C15 -104.0(15) . . . . ? N1 Rh1 C16 C15 53.9(11) . . . . ? C17 Rh1 C16 C15 -122.7(14) . . . . ? C13 Rh1 C16 C15 -81.4(10) . . . . ? C14 Rh1 C16 C15 -38.8(9) . . . . ? I1 Rh1 C16 C15 142.4(9) . . . . ? C1 Rh1 C16 C17 18.7(19) . . . . ? N1 Rh1 C16 C17 176.6(8) . . . . ? C13 Rh1 C16 C17 41.3(9) . . . . ? C14 Rh1 C16 C17 83.9(10) . . . . ? C15 Rh1 C16 C17 122.7(14) . . . . ? I1 Rh1 C16 C17 -95.0(9) . . . . ? C1 Rh1 C16 C21 137.1(16) . . . . ? N1 Rh1 C16 C21 -64.9(17) . . . . ? C17 Rh1 C16 C21 118(2) . . . . ? C13 Rh1 C16 C21 159.7(18) . . . . ? C14 Rh1 C16 C21 -157.7(18) . . . . ? C15 Rh1 C16 C21 -119(2) . . . . ? I1 Rh1 C16 C21 23.5(16) . . . . ? C15 C16 C17 C13 -5.7(16) . . . . ? C21 C16 C17 C13 174.5(13) . . . . ? Rh1 C16 C17 C13 -65.3(8) . . . . ? C15 C16 C17 C22 -174.8(14) . . . . ? C21 C16 C17 C22 5(2) . . . . ? Rh1 C16 C17 C22 125.6(15) . . . . ? C15 C16 C17 Rh1 59.6(11) . . . . ? C21 C16 C17 Rh1 -120.1(14) . . . . ? C14 C13 C17 C16 6.9(15) . . . . ? C18 C13 C17 C16 -169.8(15) . . . . ? Rh1 C13 C17 C16 67.4(9) . . . . ? C14 C13 C17 C22 175.9(14) . . . . ? C18 C13 C17 C22 -1(2) . . . . ? Rh1 C13 C17 C22 -123.6(14) . . . . ? C14 C13 C17 Rh1 -60.5(9) . . . . ? C18 C13 C17 Rh1 122.8(16) . . . . ? C1 Rh1 C17 C16 -171.2(9) . . . . ? N1 Rh1 C17 C16 -8(2) . . . . ? C13 Rh1 C17 C16 -112.9(12) . . . . ? C14 Rh1 C17 C16 -77.1(10) . . . . ? C15 Rh1 C17 C16 -33.2(9) . . . . ? I1 Rh1 C17 C16 89.6(9) . . . . ? C1 Rh1 C17 C13 -58.3(9) . . . . ? N1 Rh1 C17 C13 104.7(15) . . . . ? C14 Rh1 C17 C13 35.8(8) . . . . ? C16 Rh1 C17 C13 112.9(12) . . . . ? C15 Rh1 C17 C13 79.7(9) . . . . ? I1 Rh1 C17 C13 -157.5(7) . . . . ? C1 Rh1 C17 C22 64.4(18) . . . . ? N1 Rh1 C17 C22 -132.6(17) . . . . ? C13 Rh1 C17 C22 122.7(18) . . . . ? C14 Rh1 C17 C22 158.5(18) . . . . ? C16 Rh1 C17 C22 -124(2) . . . . ? C15 Rh1 C17 C22 -157.6(18) . . . . ? I1 Rh1 C17 C22 -34.8(16) . . . . ? C1A Rh1A N1A C5A -61.4(9) . . . . ? C17A Rh1A N1A C5A 102.5(17) . . . . ? C14A Rh1A N1A C5A 45.5(10) . . . . ? C13A Rh1A N1A C5A 24.1(12) . . . . ? C16A Rh1A N1A C5A 112.6(9) . . . . ? C15A Rh1A N1A C5A 82.6(9) . . . . ? I1A Rh1A N1A C5A -155.0(8) . . . . ? C3A N3A C1A N2A 1.0(14) . . . . ? C10A N3A C1A N2A -178.8(11) . . . . ? C3A N3A C1A Rh1A -179.6(10) . . . . ? C10A N3A C1A Rh1A 1(2) . . . . ? C4A N2A C1A N3A -177.5(11) . . . . ? C2A N2A C1A N3A -1.0(14) . . . . ? C4A N2A C1A Rh1A 3.1(17) . . . . ? C2A N2A C1A Rh1A 179.5(9) . . . . ? N1A Rh1A C1A N3A -143.2(12) . . . . ? C17A Rh1A C1A N3A 42.1(13) . . . . ? C14A Rh1A C1A N3A 114.0(12) . . . . ? C13A Rh1A C1A N3A 75.8(12) . . . . ? C16A Rh1A C1A N3A 49(2) . . . . ? C15A Rh1A C1A N3A 122.8(13) . . . . ? I1A Rh1A C1A N3A -58.9(12) . . . . ? N1A Rh1A C1A N2A 36.2(9) . . . . ? C17A Rh1A C1A N2A -138.6(9) . . . . ? C14A Rh1A C1A N2A -66.6(10) . . . . ? C13A Rh1A C1A N2A -104.9(10) . . . . ? C16A Rh1A C1A N2A -131.6(14) . . . . ? C15A Rh1A C1A N2A -57.8(13) . . . . ? I1A Rh1A C1A N2A 120.4(9) . . . . ? C1A N2A C2A C3A 0.7(16) . . . . ? C4A N2A C2A C3A 177.4(12) . . . . ? N2A C2A C3A N3A -0.1(17) . . . . ? C1A N3A C3A C2A -0.6(17) . . . . ? C10A N3A C3A C2A 179.3(12) . . . . ? C1A N2A C4A C5A -36.3(19) . . . . ? C2A N2A C4A C5A 147.7(13) . . . . ? C1A N2A C4A C9A 144.2(12) . . . . ? C2A N2A C4A C9A -31.8(18) . . . . ? C9A C4A C5A N1A -176.3(12) . . . . ? N2A C4A C5A N1A 4.2(18) . . . . ? C9A C4A C5A C6A -4(2) . . . . ? N2A C4A C5A C6A 176.4(11) . . . . ? Rh1A N1A C5A C4A 50.8(14) . . . . ? Rh1A N1A C5A C6A -121.1(11) . . . . ? C4A C5A C6A C7A 9(2) . . . . ? N1A C5A C6A C7A -178.6(12) . . . . ? C5A C6A C7A C8A -11(2) . . . . ? C6A C7A C8A C9A 7(2) . . . . ? C5A C4A C9A C8A 0.1(19) . . . . ? N2A C4A C9A C8A 179.6(12) . . . . ? C7A C8A C9A C4A -1(2) . . . . ? C1A N3A C10A C12A -120.6(14) . . . . ? C3A N3A C10A C12A 59.6(16) . . . . ? C1A N3A C10A C11A 114.9(14) . . . . ? C3A N3A C10A C11A -64.9(15) . . . . ? C1A Rh1A C13A C17A -127.2(8) . . . . ? N1A Rh1A C13A C17A 152.2(7) . . . . ? C14A Rh1A C13A C17A 118.8(11) . . . . ? C16A Rh1A C13A C17A 41.0(8) . . . . ? C15A Rh1A C13A C17A 81.3(8) . . . . ? I1A Rh1A C13A C17A -29.2(9) . . . . ? C1A Rh1A C13A C18A -2.9(15) . . . . ? N1A Rh1A C13A C18A -83.6(16) . . . . ? C17A Rh1A C13A C18A 124.2(18) . . . . ? C14A Rh1A C13A C18A -116.9(18) . . . . ? C16A Rh1A C13A C18A 165.3(17) . . . . ? C15A Rh1A C13A C18A -154.5(17) . . . . ? I1A Rh1A C13A C18A 95.0(14) . . . . ? C1A Rh1A C13A C14A 114.0(9) . . . . ? N1A Rh1A C13A C14A 33.3(11) . . . . ? C17A Rh1A C13A C14A -118.8(11) . . . . ? C16A Rh1A C13A C14A -77.8(10) . . . . ? C15A Rh1A C13A C14A -37.5(9) . . . . ? I1A Rh1A C13A C14A -148.0(7) . . . . ? C17A C13A C14A C15A 7.1(15) . . . . ? C18A C13A C14A C15A -170.5(13) . . . . ? Rh1A C13A C14A C15A 66.9(10) . . . . ? C17A C13A C14A C19A 173.9(12) . . . . ? C18A C13A C14A C19A -4(2) . . . . ? Rh1A C13A C14A C19A -126.4(13) . . . . ? C17A C13A C14A Rh1A -59.8(10) . . . . ? C18A C13A C14A Rh1A 122.6(13) . . . . ? C1A Rh1A C14A C15A 171.4(9) . . . . ? N1A Rh1A C14A C15A 86.3(9) . . . . ? C17A Rh1A C14A C15A -77.8(9) . . . . ? C13A Rh1A C14A C15A -114.6(12) . . . . ? C16A Rh1A C14A C15A -33.2(9) . . . . ? I1A Rh1A C14A C15A -27.5(16) . . . . ? C1A Rh1A C14A C13A -73.9(9) . . . . ? N1A Rh1A C14A C13A -159.0(7) . . . . ? C17A Rh1A C14A C13A 36.9(8) . . . . ? C16A Rh1A C14A C13A 81.4(9) . . . . ? C15A Rh1A C14A C13A 114.6(12) . . . . ? I1A Rh1A C14A C13A 87.1(13) . . . . ? C1A Rh1A C14A C19A 43.7(16) . . . . ? N1A Rh1A C14A C19A -41.4(16) . . . . ? C17A Rh1A C14A C19A 154.5(17) . . . . ? C13A Rh1A C14A C19A 117.6(19) . . . . ? C16A Rh1A C14A C19A -161.0(18) . . . . ? C15A Rh1A C14A C19A -128(2) . . . . ? I1A Rh1A C14A C19A -155.3(11) . . . . ? C13A C14A C15A C16A -5.7(17) . . . . ? C19A C14A C15A C16A -171.7(13) . . . . ? Rh1A C14A C15A C16A 58.0(11) . . . . ? C13A C14A C15A C20A 178.0(14) . . . . ? C19A C14A C15A C20A 12(3) . . . . ? Rh1A C14A C15A C20A -118.2(16) . . . . ? C13A C14A C15A Rh1A -63.8(9) . . . . ? C19A C14A C15A Rh1A 130.3(15) . . . . ? C1A Rh1A C15A C16A -137.9(10) . . . . ? N1A Rh1A C15A C16A 134.2(9) . . . . ? C17A Rh1A C15A C16A -39.3(9) . . . . ? C14A Rh1A C15A C16A -123.8(14) . . . . ? C13A Rh1A C15A C16A -82.9(10) . . . . ? I1A Rh1A C15A C16A 44.1(11) . . . . ? C1A Rh1A C15A C14A -14.1(14) . . . . ? N1A Rh1A C15A C14A -101.9(9) . . . . ? C17A Rh1A C15A C14A 84.6(10) . . . . ? C13A Rh1A C15A C14A 41.0(9) . . . . ? C16A Rh1A C15A C14A 123.8(14) . . . . ? I1A Rh1A C15A C14A 167.9(7) . . . . ? C1A Rh1A C15A C20A 106.1(17) . . . . ? N1A Rh1A C15A C20A 18.3(16) . . . . ? C17A Rh1A C15A C20A -155.2(18) . . . . ? C14A Rh1A C15A C20A 120.2(19) . . . . ? C13A Rh1A C15A C20A 161.2(17) . . . . ? C16A Rh1A C15A C20A -116(2) . . . . ? I1A Rh1A C15A C20A -71.9(16) . . . . ? C14A C15A C16A C17A 2.2(17) . . . . ? C20A C15A C16A C17A 178.7(13) . . . . ? Rh1A C15A C16A C17A 58.4(10) . . . . ? C14A C15A C16A C21A 178.1(14) . . . . ? C20A C15A C16A C21A -5(2) . . . . ? Rh1A C15A C16A C21A -125.7(16) . . . . ? C14A C15A C16A Rh1A -56.2(11) . . . . ? C20A C15A C16A Rh1A 120.3(15) . . . . ? C1A Rh1A C16A C15A 108.4(16) . . . . ? N1A Rh1A C16A C15A -57.1(11) . . . . ? C17A Rh1A C16A C15A 118.2(13) . . . . ? C14A Rh1A C16A C15A 33.8(9) . . . . ? C13A Rh1A C16A C15A 78.6(10) . . . . ? I1A Rh1A C16A C15A -144.0(9) . . . . ? C1A Rh1A C16A C17A -9.8(19) . . . . ? N1A Rh1A C16A C17A -175.3(7) . . . . ? C14A Rh1A C16A C17A -84.4(9) . . . . ? C13A Rh1A C16A C17A -39.6(8) . . . . ? C15A Rh1A C16A C17A -118.2(13) . . . . ? I1A Rh1A C16A C17A 97.7(8) . . . . ? C1A Rh1A C16A C21A -126.0(17) . . . . ? N1A Rh1A C16A C21A 68(2) . . . . ? C17A Rh1A C16A C21A -116(2) . . . . ? C14A Rh1A C16A C21A 159(2) . . . . ? C13A Rh1A C16A C21A -156(2) . . . . ? C15A Rh1A C16A C21A 126(2) . . . . ? I1A Rh1A C16A C21A -18.4(18) . . . . ? C18A C13A C17A C22A 4(2) . . . . ? C14A C13A C17A C22A -173.5(13) . . . . ? Rh1A C13A C17A C22A 127.0(14) . . . . ? C18A C13A C17A C16A 171.8(14) . . . . ? C14A C13A C17A C16A -5.7(15) . . . . ? Rh1A C13A C17A C16A -65.2(9) . . . . ? C18A C13A C17A Rh1A -123.1(15) . . . . ? C14A C13A C17A Rh1A 59.5(9) . . . . ? C15A C16A C17A C13A 2.4(16) . . . . ? C21A C16A C17A C13A -173.8(13) . . . . ? Rh1A C16A C17A C13A 64.2(9) . . . . ? C15A C16A C17A C22A 169.1(15) . . . . ? C21A C16A C17A C22A -7(2) . . . . ? Rh1A C16A C17A C22A -129.0(17) . . . . ? C15A C16A C17A Rh1A -61.8(11) . . . . ? C21A C16A C17A Rh1A 122.0(14) . . . . ? C1A Rh1A C17A C13A 62.0(9) . . . . ? N1A Rh1A C17A C13A -100.3(17) . . . . ? C14A Rh1A C17A C13A -37.9(8) . . . . ? C16A Rh1A C17A C13A -113.5(11) . . . . ? C15A Rh1A C17A C13A -78.4(9) . . . . ? I1A Rh1A C17A C13A 159.3(7) . . . . ? C1A Rh1A C17A C22A -56.3(17) . . . . ? N1A Rh1A C17A C22A 141.3(16) . . . . ? C14A Rh1A C17A C22A -156.3(17) . . . . ? C13A Rh1A C17A C22A -118.4(18) . . . . ? C16A Rh1A C17A C22A 128(2) . . . . ? C15A Rh1A C17A C22A 163.3(17) . . . . ? I1A Rh1A C17A C22A 40.9(16) . . . . ? C1A Rh1A C17A C16A 175.6(8) . . . . ? N1A Rh1A C17A C16A 13(2) . . . . ? C14A Rh1A C17A C16A 75.6(9) . . . . ? C13A Rh1A C17A C16A 113.5(11) . . . . ? C15A Rh1A C17A C16A 35.1(8) . . . . ? I1A Rh1A C17A C16A -87.2(8) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1A H1A2 I2A 0.92 2.68 3.570(10) 163.1 1_455 N1 H1A I2 0.92 2.73 3.598(11) 157.5 . _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 2.920 _refine_diff_density_min -1.356 _refine_diff_density_rms 0.299 #===END data_11005 _database_code_depnum_ccdc_archive 'CCDC 823385' #TrackingRef '- Paper#2 cif files.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Cp*Ir(C,NH)I (7)' _chemical_melting_point ? _chemical_formula_moiety 'C22 H29 I Ir N3' _chemical_formula_sum 'C22 H29 I Ir N3' _chemical_formula_weight 654.58 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' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.218(3) _cell_length_b 10.812(3) _cell_length_c 11.389(4) _cell_angle_alpha 75.863(5) _cell_angle_beta 78.648(5) _cell_angle_gamma 86.600(5) _cell_volume 1079.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 812 _cell_measurement_theta_min 2.254 _cell_measurement_theta_max 25.297 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.015 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 7.628 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.586 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details ; absorption correction based on 4642 reflections(SADABS);Rint 0.0819 before correction and 0.0365 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8383 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0815 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4177 _reflns_number_gt 3460 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. ; _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^)+(0.0421P)^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_number_reflns 4177 _refine_ls_number_parameters 251 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1008 _refine_ls_wR_factor_gt 0.0963 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 0.30326(4) 0.15555(3) 0.70143(3) 0.02139(12) Uani 1 1 d . . . I1 I 0.58516(7) 0.13841(6) 0.73359(7) 0.0420(2) Uani 1 1 d . . . N1 N 0.3868(8) 0.1800(7) 0.5118(7) 0.0312(18) Uani 1 1 d . . . H1 H 0.4722 0.1465 0.4844 0.037 Uiso 1 1 calc R . . N2 N 0.2881(8) 0.4189(7) 0.5432(6) 0.0241(16) Uani 1 1 d . . . N3 N 0.3499(8) 0.4326(7) 0.7117(7) 0.0283(17) Uani 1 1 d . . . C1 C 0.3136(9) 0.3439(8) 0.6538(8) 0.026(2) Uani 1 1 d . . . C2 C 0.3142(10) 0.5462(8) 0.5312(8) 0.028(2) Uani 1 1 d . . . H2 H 0.3076 0.6140 0.4614 0.034 Uiso 1 1 calc R . . C3 C 0.3502(11) 0.5556(8) 0.6350(8) 0.032(2) Uani 1 1 d . . . H3 H 0.3723 0.6322 0.6545 0.038 Uiso 1 1 calc R . . C4 C 0.2443(10) 0.3680(9) 0.4510(8) 0.027(2) Uani 1 1 d . . . C5 C 0.3043(10) 0.2487(8) 0.4354(8) 0.026(2) Uani 1 1 d . . . C6 C 0.2649(11) 0.2108(10) 0.3357(8) 0.040(3) Uani 1 1 d . . . H6 H 0.3022 0.1322 0.3181 0.048 Uiso 1 1 calc R . . C7 C 0.1731(13) 0.2853(11) 0.2630(9) 0.049(3) Uani 1 1 d . . . H7 H 0.1534 0.2585 0.1943 0.058 Uiso 1 1 calc R . . C8 C 0.1108(12) 0.3955(11) 0.2870(9) 0.046(3) Uani 1 1 d . . . H8 H 0.0412 0.4412 0.2407 0.055 Uiso 1 1 calc R . . C9 C 0.1502(10) 0.4395(9) 0.3795(8) 0.033(2) Uani 1 1 d . . . H9 H 0.1127 0.5192 0.3943 0.040 Uiso 1 1 calc R . . C10 C 0.3751(10) 0.4060(9) 0.8379(8) 0.033(2) Uani 1 1 d . . . H10 H 0.3690 0.3116 0.8717 0.040 Uiso 1 1 calc R . . C11 C 0.5264(12) 0.4465(11) 0.8447(10) 0.048(3) Uani 1 1 d . . . H11A H 0.6021 0.4049 0.7934 0.073 Uiso 1 1 calc R . . H11B H 0.5408 0.4215 0.9303 0.073 Uiso 1 1 calc R . . H11C H 0.5346 0.5393 0.8147 0.073 Uiso 1 1 calc R . . C12 C 0.2532(11) 0.4674(10) 0.9173(9) 0.042(3) Uani 1 1 d . . . H12A H 0.2623 0.5604 0.8916 0.063 Uiso 1 1 calc R . . H12B H 0.2625 0.4382 1.0040 0.063 Uiso 1 1 calc R . . H12C H 0.1563 0.4431 0.9074 0.063 Uiso 1 1 calc R . . C13 C 0.0847(10) 0.1386(8) 0.8135(8) 0.026(2) Uani 1 1 d . . . C14 C 0.1840(10) 0.0689(8) 0.8879(8) 0.030(2) Uani 1 1 d . . . C15 C 0.2455(10) -0.0319(8) 0.8329(9) 0.031(2) Uani 1 1 d . . . C16 C 0.1890(10) -0.0253(8) 0.7248(9) 0.029(2) Uani 1 1 d . . . C17 C 0.0911(9) 0.0827(9) 0.7093(8) 0.027(2) Uani 1 1 d . . . C18 C -0.0204(10) 0.2468(9) 0.8377(9) 0.038(2) Uani 1 1 d . . . H18A H -0.0050 0.3189 0.7654 0.056 Uiso 1 1 calc R . . H18B H -0.0013 0.2735 0.9094 0.056 Uiso 1 1 calc R . . H18C H -0.1227 0.2177 0.8539 0.056 Uiso 1 1 calc R . . C19 C 0.2038(12) 0.0875(10) 1.0090(8) 0.043(3) Uani 1 1 d . . . H19A H 0.1365 0.0314 1.0755 0.065 Uiso 1 1 calc R . . H19B H 0.1817 0.1765 1.0122 0.065 Uiso 1 1 calc R . . H19C H 0.3062 0.0667 1.0192 0.065 Uiso 1 1 calc R . . C20 C 0.3507(11) -0.1317(10) 0.8847(11) 0.048(3) Uani 1 1 d . . . H20A H 0.2947 -0.2042 0.9404 0.073 Uiso 1 1 calc R . . H20B H 0.4104 -0.0957 0.9303 0.073 Uiso 1 1 calc R . . H20C H 0.4159 -0.1604 0.8172 0.073 Uiso 1 1 calc R . . C21 C 0.2259(12) -0.1142(9) 0.6421(10) 0.046(3) Uani 1 1 d . . . H21A H 0.3267 -0.1476 0.6443 0.069 Uiso 1 1 calc R . . H21B H 0.2192 -0.0686 0.5576 0.069 Uiso 1 1 calc R . . H21C H 0.1561 -0.1850 0.6696 0.069 Uiso 1 1 calc R . . C22 C -0.0044(11) 0.1176(10) 0.6136(9) 0.040(3) Uani 1 1 d . . . H22A H -0.0919 0.0633 0.6391 0.061 Uiso 1 1 calc R . . H22B H 0.0518 0.1053 0.5347 0.061 Uiso 1 1 calc R . . H22C H -0.0355 0.2072 0.6042 0.061 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 0.01827(18) 0.01797(18) 0.02652(19) -0.00261(13) -0.00409(13) -0.00074(13) I1 0.0254(3) 0.0366(4) 0.0582(5) 0.0025(3) -0.0115(3) 0.0009(3) N1 0.021(4) 0.033(5) 0.032(4) -0.004(4) 0.010(3) 0.000(3) N2 0.026(4) 0.023(4) 0.024(4) -0.002(3) -0.009(3) -0.001(3) N3 0.032(4) 0.026(4) 0.029(4) -0.005(3) -0.011(3) -0.002(3) C1 0.022(5) 0.028(5) 0.026(5) -0.003(4) 0.000(4) -0.008(4) C2 0.031(5) 0.017(5) 0.033(5) -0.002(4) -0.005(4) 0.004(4) C3 0.044(6) 0.013(4) 0.035(5) -0.005(4) 0.005(5) -0.009(4) C4 0.027(5) 0.032(5) 0.021(4) -0.006(4) -0.004(4) -0.007(4) C5 0.026(5) 0.024(5) 0.024(5) -0.006(4) 0.004(4) -0.010(4) C6 0.041(6) 0.052(7) 0.023(5) -0.010(5) 0.004(5) -0.010(5) C7 0.067(8) 0.050(7) 0.029(6) -0.004(5) -0.009(6) -0.031(6) C8 0.050(7) 0.051(7) 0.032(6) 0.005(5) -0.014(5) -0.009(6) C9 0.031(5) 0.037(6) 0.030(5) -0.003(4) -0.008(4) -0.001(4) C10 0.032(5) 0.037(6) 0.029(5) -0.001(4) -0.010(4) -0.014(4) C11 0.052(7) 0.058(8) 0.040(6) -0.014(6) -0.013(5) -0.019(6) C12 0.045(6) 0.045(7) 0.035(6) -0.008(5) -0.003(5) -0.009(5) C13 0.025(5) 0.016(4) 0.034(5) -0.002(4) 0.002(4) -0.007(4) C14 0.029(5) 0.023(5) 0.034(5) -0.002(4) -0.002(4) -0.010(4) C15 0.022(5) 0.021(5) 0.044(6) 0.003(4) -0.003(4) -0.003(4) C16 0.023(5) 0.021(5) 0.042(6) -0.014(4) 0.003(4) -0.008(4) C17 0.020(4) 0.033(5) 0.022(5) -0.003(4) 0.007(4) -0.016(4) C18 0.026(5) 0.035(6) 0.049(6) -0.017(5) 0.011(5) 0.001(4) C19 0.050(7) 0.053(7) 0.026(5) -0.002(5) -0.011(5) -0.015(5) C20 0.034(6) 0.030(6) 0.077(8) -0.006(5) -0.007(6) 0.005(5) C21 0.047(7) 0.031(6) 0.059(7) -0.021(5) 0.009(6) -0.007(5) C22 0.030(5) 0.054(7) 0.042(6) -0.013(5) -0.015(5) -0.004(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 C1 1.978(9) . ? Ir1 N1 2.101(7) . ? Ir1 C17 2.129(8) . ? Ir1 C13 2.154(8) . ? Ir1 C14 2.197(9) . ? Ir1 C16 2.210(8) . ? Ir1 C15 2.228(9) . ? Ir1 I1 2.6843(11) . ? N1 C5 1.328(11) . ? N1 H1 0.8800 . ? N2 C1 1.376(11) . ? N2 C2 1.380(10) . ? N2 C4 1.430(10) . ? N3 C1 1.379(11) . ? N3 C3 1.401(11) . ? N3 C10 1.457(11) . ? C2 C3 1.318(12) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C9 1.380(13) . ? C4 C5 1.411(12) . ? C5 C6 1.413(12) . ? C6 C7 1.385(15) . ? C6 H6 0.9500 . ? C7 C8 1.356(15) . ? C7 H7 0.9500 . ? C8 C9 1.373(13) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.508(13) . ? C10 C12 1.525(13) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.427(13) . ? C13 C17 1.447(12) . ? C13 C18 1.516(12) . ? C14 C15 1.422(13) . ? C14 C19 1.488(12) . ? C15 C16 1.413(13) . ? C15 C20 1.498(13) . ? C16 C17 1.430(12) . ? C16 C21 1.485(12) . ? C17 C22 1.498(12) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 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 C1 Ir1 N1 81.1(3) . . ? C1 Ir1 C17 114.1(4) . . ? N1 Ir1 C17 99.1(3) . . ? C1 Ir1 C13 98.1(3) . . ? N1 Ir1 C13 134.4(3) . . ? C17 Ir1 C13 39.5(3) . . ? C1 Ir1 C14 116.9(3) . . ? N1 Ir1 C14 159.3(3) . . ? C17 Ir1 C14 65.1(3) . . ? C13 Ir1 C14 38.3(3) . . ? C1 Ir1 C16 151.9(4) . . ? N1 Ir1 C16 95.8(3) . . ? C17 Ir1 C16 38.4(3) . . ? C13 Ir1 C16 64.2(3) . . ? C14 Ir1 C16 63.5(3) . . ? C1 Ir1 C15 154.2(4) . . ? N1 Ir1 C15 124.6(3) . . ? C17 Ir1 C15 63.5(3) . . ? C13 Ir1 C15 63.0(3) . . ? C14 Ir1 C15 37.5(3) . . ? C16 Ir1 C15 37.1(3) . . ? C1 Ir1 I1 90.9(3) . . ? N1 Ir1 I1 87.3(2) . . ? C17 Ir1 I1 154.8(3) . . ? C13 Ir1 I1 138.2(2) . . ? C14 Ir1 I1 101.8(2) . . ? C16 Ir1 I1 117.0(2) . . ? C15 Ir1 I1 92.7(2) . . ? C5 N1 Ir1 116.8(6) . . ? C5 N1 H1 121.6 . . ? Ir1 N1 H1 121.6 . . ? C1 N2 C2 112.3(7) . . ? C1 N2 C4 122.9(7) . . ? C2 N2 C4 124.8(7) . . ? C1 N3 C3 110.6(7) . . ? C1 N3 C10 125.7(7) . . ? C3 N3 C10 123.6(7) . . ? N2 C1 N3 102.4(7) . . ? N2 C1 Ir1 124.9(6) . . ? N3 C1 Ir1 132.7(7) . . ? C3 C2 N2 106.9(8) . . ? C3 C2 H2 126.5 . . ? N2 C2 H2 126.5 . . ? C2 C3 N3 107.8(8) . . ? C2 C3 H3 126.1 . . ? N3 C3 H3 126.1 . . ? C9 C4 C5 123.6(8) . . ? C9 C4 N2 118.6(8) . . ? C5 C4 N2 117.8(8) . . ? N1 C5 C4 121.0(8) . . ? N1 C5 C6 125.0(9) . . ? C4 C5 C6 113.9(9) . . ? C7 C6 C5 121.7(10) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C8 C7 C6 121.9(10) . . ? C8 C7 H7 119.0 . . ? C6 C7 H7 119.0 . . ? C7 C8 C9 118.7(10) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? C8 C9 C4 120.0(10) . . ? C8 C9 H9 120.0 . . ? C4 C9 H9 120.0 . . ? N3 C10 C11 112.4(8) . . ? N3 C10 C12 110.3(8) . . ? C11 C10 C12 111.4(8) . . ? N3 C10 H10 107.5 . . ? C11 C10 H10 107.5 . . ? C12 C10 H10 107.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C17 108.1(8) . . ? C14 C13 C18 128.5(8) . . ? C17 C13 C18 123.2(8) . . ? C14 C13 Ir1 72.5(5) . . ? C17 C13 Ir1 69.3(5) . . ? C18 C13 Ir1 126.9(6) . . ? C15 C14 C13 107.1(8) . . ? C15 C14 C19 126.2(9) . . ? C13 C14 C19 126.2(9) . . ? C15 C14 Ir1 72.4(5) . . ? C13 C14 Ir1 69.2(5) . . ? C19 C14 Ir1 129.6(6) . . ? C16 C15 C14 109.7(8) . . ? C16 C15 C20 125.6(9) . . ? C14 C15 C20 124.7(9) . . ? C16 C15 Ir1 70.7(5) . . ? C14 C15 Ir1 70.1(5) . . ? C20 C15 Ir1 127.0(7) . . ? C15 C16 C17 107.6(7) . . ? C15 C16 C21 126.0(9) . . ? C17 C16 C21 126.4(9) . . ? C15 C16 Ir1 72.1(5) . . ? C17 C16 Ir1 67.7(5) . . ? C21 C16 Ir1 125.2(6) . . ? C16 C17 C13 107.4(8) . . ? C16 C17 C22 125.5(8) . . ? C13 C17 C22 126.5(9) . . ? C16 C17 Ir1 73.8(5) . . ? C13 C17 Ir1 71.2(5) . . ? C22 C17 Ir1 127.6(6) . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 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 C1 Ir1 N1 C5 -59.6(7) . . . . ? C17 Ir1 N1 C5 53.6(7) . . . . ? C13 Ir1 N1 C5 33.1(8) . . . . ? C14 Ir1 N1 C5 91.9(11) . . . . ? C16 Ir1 N1 C5 92.2(7) . . . . ? C15 Ir1 N1 C5 117.6(7) . . . . ? I1 Ir1 N1 C5 -150.9(6) . . . . ? C2 N2 C1 N3 2.8(9) . . . . ? C4 N2 C1 N3 -179.2(7) . . . . ? C2 N2 C1 Ir1 -175.3(6) . . . . ? C4 N2 C1 Ir1 2.8(11) . . . . ? C3 N3 C1 N2 -1.9(9) . . . . ? C10 N3 C1 N2 174.2(8) . . . . ? C3 N3 C1 Ir1 175.9(7) . . . . ? C10 N3 C1 Ir1 -8.0(13) . . . . ? N1 Ir1 C1 N2 34.6(7) . . . . ? C17 Ir1 C1 N2 -61.5(8) . . . . ? C13 Ir1 C1 N2 -99.3(7) . . . . ? C14 Ir1 C1 N2 -134.5(7) . . . . ? C16 Ir1 C1 N2 -51.0(11) . . . . ? C15 Ir1 C1 N2 -140.1(8) . . . . ? I1 Ir1 C1 N2 121.7(7) . . . . ? N1 Ir1 C1 N3 -142.8(9) . . . . ? C17 Ir1 C1 N3 121.2(8) . . . . ? C13 Ir1 C1 N3 83.4(9) . . . . ? C14 Ir1 C1 N3 48.1(9) . . . . ? C16 Ir1 C1 N3 131.6(8) . . . . ? C15 Ir1 C1 N3 42.5(13) . . . . ? I1 Ir1 C1 N3 -55.6(8) . . . . ? C1 N2 C2 C3 -2.7(10) . . . . ? C4 N2 C2 C3 179.3(8) . . . . ? N2 C2 C3 N3 1.4(10) . . . . ? C1 N3 C3 C2 0.3(10) . . . . ? C10 N3 C3 C2 -175.8(8) . . . . ? C1 N2 C4 C9 146.2(9) . . . . ? C2 N2 C4 C9 -36.0(12) . . . . ? C1 N2 C4 C5 -35.9(11) . . . . ? C2 N2 C4 C5 141.9(8) . . . . ? Ir1 N1 C5 C4 48.2(10) . . . . ? Ir1 N1 C5 C6 -130.0(8) . . . . ? C9 C4 C5 N1 -175.6(8) . . . . ? N2 C4 C5 N1 6.6(12) . . . . ? C9 C4 C5 C6 2.8(13) . . . . ? N2 C4 C5 C6 -175.0(7) . . . . ? N1 C5 C6 C7 177.2(9) . . . . ? C4 C5 C6 C7 -1.1(13) . . . . ? C5 C6 C7 C8 -3.2(15) . . . . ? C6 C7 C8 C9 5.8(16) . . . . ? C7 C8 C9 C4 -4.1(15) . . . . ? C5 C4 C9 C8 -0.3(14) . . . . ? N2 C4 C9 C8 177.5(8) . . . . ? C1 N3 C10 C11 122.5(10) . . . . ? C3 N3 C10 C11 -62.0(12) . . . . ? C1 N3 C10 C12 -112.5(10) . . . . ? C3 N3 C10 C12 63.0(11) . . . . ? C1 Ir1 C13 C14 -123.8(5) . . . . ? N1 Ir1 C13 C14 150.8(5) . . . . ? C17 Ir1 C13 C14 117.9(7) . . . . ? C16 Ir1 C13 C14 79.2(5) . . . . ? C15 Ir1 C13 C14 37.6(5) . . . . ? I1 Ir1 C13 C14 -23.3(6) . . . . ? C1 Ir1 C13 C17 118.4(5) . . . . ? N1 Ir1 C13 C17 33.0(7) . . . . ? C14 Ir1 C13 C17 -117.9(7) . . . . ? C16 Ir1 C13 C17 -38.6(5) . . . . ? C15 Ir1 C13 C17 -80.3(6) . . . . ? I1 Ir1 C13 C17 -141.1(4) . . . . ? C1 Ir1 C13 C18 1.7(9) . . . . ? N1 Ir1 C13 C18 -83.7(9) . . . . ? C17 Ir1 C13 C18 -116.7(10) . . . . ? C14 Ir1 C13 C18 125.5(10) . . . . ? C16 Ir1 C13 C18 -155.3(9) . . . . ? C15 Ir1 C13 C18 163.0(9) . . . . ? I1 Ir1 C13 C18 102.2(8) . . . . ? C17 C13 C14 C15 -2.5(10) . . . . ? C18 C13 C14 C15 173.4(8) . . . . ? Ir1 C13 C14 C15 -63.0(6) . . . . ? C17 C13 C14 C19 -175.0(8) . . . . ? C18 C13 C14 C19 1.0(15) . . . . ? Ir1 C13 C14 C19 124.5(9) . . . . ? C17 C13 C14 Ir1 60.5(6) . . . . ? C18 C13 C14 Ir1 -123.6(9) . . . . ? C1 Ir1 C14 C15 -176.0(5) . . . . ? N1 Ir1 C14 C15 36.0(12) . . . . ? C17 Ir1 C14 C15 78.4(6) . . . . ? C13 Ir1 C14 C15 116.7(8) . . . . ? C16 Ir1 C14 C15 35.6(5) . . . . ? I1 Ir1 C14 C15 -78.9(5) . . . . ? C1 Ir1 C14 C13 67.3(6) . . . . ? N1 Ir1 C14 C13 -80.8(10) . . . . ? C17 Ir1 C14 C13 -38.3(5) . . . . ? C16 Ir1 C14 C13 -81.2(5) . . . . ? C15 Ir1 C14 C13 -116.7(8) . . . . ? I1 Ir1 C14 C13 164.4(4) . . . . ? C1 Ir1 C14 C19 -53.1(10) . . . . ? N1 Ir1 C14 C19 158.8(9) . . . . ? C17 Ir1 C14 C19 -158.8(10) . . . . ? C13 Ir1 C14 C19 -120.4(11) . . . . ? C16 Ir1 C14 C19 158.4(10) . . . . ? C15 Ir1 C14 C19 122.8(11) . . . . ? I1 Ir1 C14 C19 44.0(9) . . . . ? C13 C14 C15 C16 1.1(10) . . . . ? C19 C14 C15 C16 173.5(8) . . . . ? Ir1 C14 C15 C16 -59.8(6) . . . . ? C13 C14 C15 C20 -177.2(8) . . . . ? C19 C14 C15 C20 -4.8(15) . . . . ? Ir1 C14 C15 C20 121.9(9) . . . . ? C13 C14 C15 Ir1 60.9(6) . . . . ? C19 C14 C15 Ir1 -126.6(9) . . . . ? C1 Ir1 C15 C16 128.7(8) . . . . ? N1 Ir1 C15 C16 -45.0(6) . . . . ? C17 Ir1 C15 C16 37.6(5) . . . . ? C13 Ir1 C15 C16 82.1(5) . . . . ? C14 Ir1 C15 C16 120.4(8) . . . . ? I1 Ir1 C15 C16 -133.6(5) . . . . ? C1 Ir1 C15 C14 8.3(11) . . . . ? N1 Ir1 C15 C14 -165.4(5) . . . . ? C17 Ir1 C15 C14 -82.8(6) . . . . ? C13 Ir1 C15 C14 -38.4(5) . . . . ? C16 Ir1 C15 C14 -120.4(8) . . . . ? I1 Ir1 C15 C14 106.0(5) . . . . ? C1 Ir1 C15 C20 -110.8(10) . . . . ? N1 Ir1 C15 C20 75.6(10) . . . . ? C17 Ir1 C15 C20 158.2(10) . . . . ? C13 Ir1 C15 C20 -157.4(10) . . . . ? C14 Ir1 C15 C20 -119.0(11) . . . . ? C16 Ir1 C15 C20 120.5(11) . . . . ? I1 Ir1 C15 C20 -13.1(9) . . . . ? C14 C15 C16 C17 0.8(10) . . . . ? C20 C15 C16 C17 179.1(8) . . . . ? Ir1 C15 C16 C17 -58.6(6) . . . . ? C14 C15 C16 C21 -179.6(8) . . . . ? C20 C15 C16 C21 -1.3(14) . . . . ? Ir1 C15 C16 C21 121.0(9) . . . . ? C14 C15 C16 Ir1 59.4(6) . . . . ? C20 C15 C16 Ir1 -122.3(9) . . . . ? C1 Ir1 C16 C15 -133.8(7) . . . . ? N1 Ir1 C16 C15 144.2(5) . . . . ? C17 Ir1 C16 C15 -118.4(7) . . . . ? C13 Ir1 C16 C15 -78.7(5) . . . . ? C14 Ir1 C16 C15 -35.9(5) . . . . ? I1 Ir1 C16 C15 54.3(5) . . . . ? C1 Ir1 C16 C17 -15.4(10) . . . . ? N1 Ir1 C16 C17 -97.3(5) . . . . ? C13 Ir1 C16 C17 39.7(5) . . . . ? C14 Ir1 C16 C17 82.5(5) . . . . ? C15 Ir1 C16 C17 118.4(7) . . . . ? I1 Ir1 C16 C17 172.7(4) . . . . ? C1 Ir1 C16 C21 104.3(10) . . . . ? N1 Ir1 C16 C21 22.4(9) . . . . ? C17 Ir1 C16 C21 119.7(11) . . . . ? C13 Ir1 C16 C21 159.4(10) . . . . ? C14 Ir1 C16 C21 -157.7(10) . . . . ? C15 Ir1 C16 C21 -121.8(11) . . . . ? I1 Ir1 C16 C21 -67.6(9) . . . . ? C15 C16 C17 C13 -2.3(9) . . . . ? C21 C16 C17 C13 178.1(8) . . . . ? Ir1 C16 C17 C13 -63.8(6) . . . . ? C15 C16 C17 C22 -173.6(8) . . . . ? C21 C16 C17 C22 6.8(14) . . . . ? Ir1 C16 C17 C22 125.0(8) . . . . ? C15 C16 C17 Ir1 61.4(6) . . . . ? C21 C16 C17 Ir1 -118.2(9) . . . . ? C14 C13 C17 C16 3.0(9) . . . . ? C18 C13 C17 C16 -173.2(8) . . . . ? Ir1 C13 C17 C16 65.5(6) . . . . ? C14 C13 C17 C22 174.1(8) . . . . ? C18 C13 C17 C22 -2.1(13) . . . . ? Ir1 C13 C17 C22 -123.3(9) . . . . ? C14 C13 C17 Ir1 -62.5(6) . . . . ? C18 C13 C17 Ir1 121.3(8) . . . . ? C1 Ir1 C17 C16 172.1(5) . . . . ? N1 Ir1 C17 C16 87.9(5) . . . . ? C13 Ir1 C17 C16 -115.3(7) . . . . ? C14 Ir1 C17 C16 -78.1(5) . . . . ? C15 Ir1 C17 C16 -36.4(5) . . . . ? I1 Ir1 C17 C16 -15.4(9) . . . . ? C1 Ir1 C17 C13 -72.6(6) . . . . ? N1 Ir1 C17 C13 -156.8(5) . . . . ? C14 Ir1 C17 C13 37.2(5) . . . . ? C16 Ir1 C17 C13 115.3(7) . . . . ? C15 Ir1 C17 C13 78.9(5) . . . . ? I1 Ir1 C17 C13 99.9(7) . . . . ? C1 Ir1 C17 C22 49.5(9) . . . . ? N1 Ir1 C17 C22 -34.7(9) . . . . ? C13 Ir1 C17 C22 122.1(11) . . . . ? C14 Ir1 C17 C22 159.2(9) . . . . ? C16 Ir1 C17 C22 -122.6(10) . . . . ? C15 Ir1 C17 C22 -159.0(9) . . . . ? I1 Ir1 C17 C22 -138.0(7) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 2.294 _refine_diff_density_min -1.647 _refine_diff_density_rms 0.228 #===END data_11026 _database_code_depnum_ccdc_archive 'CCDC 823386' #TrackingRef '- Paper#2 cif files.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Cp*Ir(C,NH2)I][CF3CO2] (8)' _chemical_melting_point ? _chemical_formula_moiety 'C22 H30 I Ir N3, C2 F3 O2,5C5H12' _chemical_formula_sum 'C49 H90 F3 I Ir N3 O2' _chemical_formula_weight 1129.34 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' I I -0.4742 1.8119 '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.957(3) _cell_length_b 10.360(2) _cell_length_c 21.186(4) _cell_angle_alpha 90.00 _cell_angle_beta 110.741(4) _cell_angle_gamma 90.00 _cell_volume 3480.6(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 657 _cell_measurement_theta_min 2.349 _cell_measurement_theta_max 28.402 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2312 _exptl_absorpt_coefficient_mu 4.795 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.539 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details ; absorption correction based on 4559 reflections(SADABS);Rint 0.1338 before correction and 0.0635 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26753 _diffrn_reflns_av_R_equivalents 0.1501 _diffrn_reflns_av_sigmaI/netI 0.1704 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6829 _reflns_number_gt 3745 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Disordered C5H12 was omitted using the SQUEEZE option of PLATON.The solvent accessible voids are 1211 A3 with an estimated 840e/cell to be added. Twenty solvent C5H12 molecules/unit cell accounting for 840e were included in the formula, FWt, (000) and density calculations. PLATON Reference: Spek, A.L. (1990), Acta Cryst. A46,C-34. 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. ; _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^)+(0.0315P)^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_number_reflns 6829 _refine_ls_number_parameters 314 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0949 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1136 _refine_ls_wR_factor_gt 0.1052 _refine_ls_goodness_of_fit_ref 0.795 _refine_ls_restrained_S_all 0.795 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.60383(2) 0.13720(4) 0.77758(2) 0.03325(13) Uani 1 1 d . . . I1 I 0.74213(4) 0.07442(7) 0.74838(4) 0.0460(2) Uani 1 1 d . . . N1 N 0.5980(5) 0.2984(7) 0.7119(4) 0.039(2) Uani 1 1 d . . . H1A H 0.6514 0.3304 0.7205 0.047 Uiso 1 1 calc R . . H1B H 0.5770 0.2713 0.6677 0.047 Uiso 1 1 calc R . . N2 N 0.6349(5) 0.3976(7) 0.8415(4) 0.034(2) Uani 1 1 d . . . N3 N 0.7293(5) 0.2728(8) 0.9047(4) 0.040(2) Uani 1 1 d . . . C1 C 0.6646(5) 0.2726(9) 0.8467(5) 0.029(2) Uani 1 1 d . . . C2 C 0.6850(7) 0.4717(10) 0.8965(5) 0.050(3) Uani 1 1 d . . . H2 H 0.6799 0.5612 0.9041 0.061 Uiso 1 1 calc R . . C3 C 0.7390(7) 0.3926(9) 0.9341(5) 0.046(3) Uani 1 1 d . . . H3 H 0.7803 0.4137 0.9766 0.055 Uiso 1 1 calc R . . C4 C 0.5620(6) 0.4475(9) 0.7864(5) 0.034(2) Uani 1 1 d . . . C5 C 0.5452(6) 0.3980(9) 0.7220(5) 0.029(2) Uani 1 1 d . . . C6 C 0.4752(6) 0.4445(10) 0.6686(5) 0.045(3) Uani 1 1 d . . . H6 H 0.4623 0.4115 0.6242 0.054 Uiso 1 1 calc R . . C7 C 0.4256(7) 0.5379(10) 0.6812(5) 0.044(3) Uani 1 1 d . . . H7 H 0.3797 0.5717 0.6445 0.052 Uiso 1 1 calc R . . C8 C 0.4403(7) 0.5855(11) 0.7463(6) 0.053(3) Uani 1 1 d . . . H8 H 0.4040 0.6487 0.7538 0.063 Uiso 1 1 calc R . . C9 C 0.5077(7) 0.5398(11) 0.7988(6) 0.059(3) Uani 1 1 d . . . H9 H 0.5180 0.5697 0.8434 0.071 Uiso 1 1 calc R . . C10 C 0.7846(6) 0.1593(10) 0.9331(5) 0.043(3) Uani 1 1 d . . . H10 H 0.7595 0.0823 0.9046 0.052 Uiso 1 1 calc R . . C11 C 0.7891(7) 0.1323(11) 1.0030(5) 0.061(4) Uani 1 1 d . . . H11A H 0.8241 0.1980 1.0335 0.092 Uiso 1 1 calc R . . H11B H 0.8140 0.0469 1.0169 0.092 Uiso 1 1 calc R . . H11C H 0.7322 0.1344 1.0049 0.092 Uiso 1 1 calc R . . C12 C 0.8732(6) 0.1813(10) 0.9308(5) 0.055(3) Uani 1 1 d . . . H12A H 0.8708 0.1767 0.8840 0.082 Uiso 1 1 calc R . . H12B H 0.9116 0.1146 0.9576 0.082 Uiso 1 1 calc R . . H12C H 0.8938 0.2666 0.9494 0.082 Uiso 1 1 calc R . . C13 C 0.5446(6) 0.0417(10) 0.8417(6) 0.048(3) Uani 1 1 d . . . C14 C 0.5784(6) -0.0523(9) 0.8103(5) 0.039(3) Uani 1 1 d . . . C15 C 0.5345(6) -0.0464(10) 0.7343(5) 0.039(3) Uani 1 1 d . . . C16 C 0.4754(6) 0.0515(10) 0.7228(5) 0.040(3) Uani 1 1 d . . . C17 C 0.4807(6) 0.1156(10) 0.7863(6) 0.047(3) Uani 1 1 d . . . C18 C 0.5603(7) 0.0622(12) 0.9171(5) 0.070(4) Uani 1 1 d . . . H18A H 0.6041 0.0025 0.9440 0.105 Uiso 1 1 calc R . . H18B H 0.5080 0.0459 0.9256 0.105 Uiso 1 1 calc R . . H18C H 0.5787 0.1512 0.9296 0.105 Uiso 1 1 calc R . . C19 C 0.6414(6) -0.1559(10) 0.8460(6) 0.063(4) Uani 1 1 d . . . H19A H 0.6786 -0.1233 0.8899 0.095 Uiso 1 1 calc R . . H19B H 0.6751 -0.1791 0.8185 0.095 Uiso 1 1 calc R . . H19C H 0.6113 -0.2323 0.8528 0.095 Uiso 1 1 calc R . . C20 C 0.5459(8) -0.1364(10) 0.6845(6) 0.061(3) Uani 1 1 d . . . H20A H 0.5171 -0.2178 0.6858 0.091 Uiso 1 1 calc R . . H20B H 0.6062 -0.1527 0.6953 0.091 Uiso 1 1 calc R . . H20C H 0.5220 -0.0985 0.6393 0.091 Uiso 1 1 calc R . . C21 C 0.4122(6) 0.0955(11) 0.6579(5) 0.068(4) Uani 1 1 d . . . H21A H 0.4249 0.0570 0.6203 0.101 Uiso 1 1 calc R . . H21B H 0.4142 0.1898 0.6551 0.101 Uiso 1 1 calc R . . H21C H 0.3558 0.0686 0.6555 0.101 Uiso 1 1 calc R . . C22 C 0.4223(6) 0.2153(11) 0.7938(6) 0.071(4) Uani 1 1 d . . . H22A H 0.4102 0.2777 0.7569 0.106 Uiso 1 1 calc R . . H22B H 0.4483 0.2599 0.8371 0.106 Uiso 1 1 calc R . . H22C H 0.3696 0.1743 0.7926 0.106 Uiso 1 1 calc R . . C23 C 0.6275(8) 0.2651(13) 0.5276(6) 0.063(4) Uani 1 1 d . . . C24 C 0.5650(6) 0.1659(10) 0.5368(5) 0.039(3) Uani 1 1 d . . . F1 F 0.5954(5) 0.3252(7) 0.4685(4) 0.092(3) Uani 1 1 d . . . F2 F 0.6462(4) 0.3581(6) 0.5761(4) 0.079(2) Uani 1 1 d . . . F3 F 0.7006(4) 0.2152(7) 0.5306(4) 0.084(2) Uani 1 1 d . . . O1 O 0.5554(4) 0.0727(7) 0.4987(3) 0.049(2) Uani 1 1 d . . . O2 O 0.5313(5) 0.1918(7) 0.5764(3) 0.051(2) 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 0.0242(2) 0.0373(2) 0.0296(2) -0.0019(2) -0.00118(16) -0.0009(2) I1 0.0349(4) 0.0494(5) 0.0517(5) -0.0011(4) 0.0130(4) 0.0048(4) N1 0.029(5) 0.052(6) 0.022(5) -0.003(4) -0.008(4) 0.000(4) N2 0.030(5) 0.040(6) 0.021(5) -0.001(4) -0.006(4) -0.006(4) N3 0.030(5) 0.033(5) 0.047(6) -0.007(4) 0.003(4) -0.004(4) C1 0.011(5) 0.037(6) 0.030(6) 0.001(5) -0.002(4) 0.000(4) C2 0.049(7) 0.039(7) 0.037(7) -0.012(5) -0.016(6) 0.006(6) C3 0.044(7) 0.040(7) 0.035(6) -0.005(5) -0.011(5) 0.002(5) C4 0.030(6) 0.035(6) 0.031(6) -0.004(5) 0.004(5) 0.001(5) C5 0.026(5) 0.032(6) 0.027(6) -0.003(4) 0.006(5) 0.002(4) C6 0.025(6) 0.040(7) 0.052(7) 0.004(6) -0.009(5) 0.003(5) C7 0.045(7) 0.040(7) 0.028(6) -0.001(5) -0.008(5) -0.001(6) C8 0.044(7) 0.050(7) 0.055(8) 0.006(6) 0.006(6) 0.014(6) C9 0.054(8) 0.067(9) 0.071(9) 0.005(7) 0.040(7) -0.014(7) C10 0.030(6) 0.043(7) 0.046(7) 0.006(6) -0.001(5) 0.000(5) C11 0.055(8) 0.059(8) 0.041(7) 0.009(6) -0.019(6) 0.000(7) C12 0.038(7) 0.062(8) 0.056(8) 0.003(6) 0.008(6) -0.006(6) C13 0.022(6) 0.047(7) 0.065(8) -0.004(6) 0.001(6) -0.007(5) C14 0.032(6) 0.031(6) 0.042(7) 0.003(5) 0.000(5) -0.003(5) C15 0.037(6) 0.030(6) 0.042(7) 0.001(5) 0.002(5) -0.015(5) C16 0.026(6) 0.042(7) 0.040(7) -0.008(5) -0.004(5) -0.015(5) C17 0.022(6) 0.044(7) 0.078(9) 0.000(6) 0.021(6) 0.000(5) C18 0.050(8) 0.114(11) 0.046(8) -0.020(8) 0.018(6) -0.024(8) C19 0.039(7) 0.041(7) 0.078(9) 0.014(7) -0.019(6) -0.007(6) C20 0.084(9) 0.029(6) 0.071(9) -0.009(7) 0.030(7) -0.010(7) C21 0.031(7) 0.091(10) 0.056(8) 0.026(7) -0.015(6) -0.017(6) C22 0.031(7) 0.071(9) 0.101(11) -0.018(8) 0.013(7) -0.009(7) C23 0.055(9) 0.060(9) 0.045(8) -0.015(7) -0.018(7) -0.004(7) C24 0.035(6) 0.044(8) 0.031(6) -0.005(5) 0.002(5) -0.011(5) F1 0.081(6) 0.099(6) 0.080(6) 0.033(5) 0.008(5) -0.026(5) F2 0.085(5) 0.059(4) 0.081(5) -0.021(4) 0.018(4) -0.021(4) F3 0.050(5) 0.091(6) 0.100(6) -0.002(5) 0.012(4) -0.001(4) O1 0.049(5) 0.044(5) 0.046(5) -0.006(4) 0.005(4) -0.002(4) O2 0.060(5) 0.066(5) 0.022(4) -0.012(4) 0.008(4) -0.009(4) _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 C1 2.026(9) . ? Ir1 N1 2.153(7) . ? Ir1 C17 2.172(10) . ? Ir1 C14 2.176(10) . ? Ir1 C13 2.192(11) . ? Ir1 C15 2.253(9) . ? Ir1 C16 2.256(9) . ? Ir1 I1 2.7082(9) . ? N1 C5 1.431(11) . ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? N2 C1 1.380(11) . ? N2 C2 1.403(11) . ? N2 C4 1.462(11) . ? N3 C1 1.326(10) . ? N3 C3 1.372(11) . ? N3 C10 1.492(11) . ? C2 C3 1.276(12) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C5 1.391(12) . ? C4 C9 1.415(14) . ? C5 C6 1.404(12) . ? C6 C7 1.368(13) . ? C6 H6 0.9500 . ? C7 C8 1.402(13) . ? C7 H7 0.9500 . ? C8 C9 1.366(14) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.484(13) . ? C10 C12 1.537(13) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.411(14) . ? C13 C17 1.496(14) . ? C13 C18 1.537(14) . ? C14 C19 1.514(12) . ? C14 C15 1.517(13) . ? C15 C16 1.386(13) . ? C15 C20 1.471(13) . ? C16 C17 1.475(14) . ? C16 C21 1.483(13) . ? C17 C22 1.479(13) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 F3 1.323(13) . ? C23 F1 1.330(13) . ? C23 F2 1.362(12) . ? C23 C24 1.537(15) . ? C24 O2 1.202(11) . ? C24 O1 1.232(11) . ? 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 C1 Ir1 N1 80.0(3) . . ? C1 Ir1 C17 105.5(4) . . ? N1 Ir1 C17 108.0(4) . . ? C1 Ir1 C14 120.1(4) . . ? N1 Ir1 C14 159.5(3) . . ? C17 Ir1 C14 64.8(4) . . ? C1 Ir1 C13 95.2(4) . . ? N1 Ir1 C13 145.6(4) . . ? C17 Ir1 C13 40.1(4) . . ? C14 Ir1 C13 37.7(4) . . ? C1 Ir1 C15 159.6(4) . . ? N1 Ir1 C15 119.6(3) . . ? C17 Ir1 C15 64.5(4) . . ? C14 Ir1 C15 40.0(3) . . ? C13 Ir1 C15 65.4(4) . . ? C1 Ir1 C16 142.7(4) . . ? N1 Ir1 C16 99.0(3) . . ? C17 Ir1 C16 38.9(4) . . ? C14 Ir1 C16 62.9(4) . . ? C13 Ir1 C16 64.6(4) . . ? C15 Ir1 C16 35.8(3) . . ? C1 Ir1 I1 94.1(3) . . ? N1 Ir1 I1 83.3(2) . . ? C17 Ir1 I1 158.6(3) . . ? C14 Ir1 I1 98.1(3) . . ? C13 Ir1 I1 131.1(3) . . ? C15 Ir1 I1 94.2(3) . . ? C16 Ir1 I1 123.0(3) . . ? C5 N1 Ir1 110.5(6) . . ? C5 N1 H1A 109.5 . . ? Ir1 N1 H1A 109.5 . . ? C5 N1 H1B 109.5 . . ? Ir1 N1 H1B 109.5 . . ? H1A N1 H1B 108.1 . . ? C1 N2 C2 110.6(8) . . ? C1 N2 C4 125.2(8) . . ? C2 N2 C4 124.2(8) . . ? C1 N3 C3 110.4(8) . . ? C1 N3 C10 124.6(8) . . ? C3 N3 C10 124.9(8) . . ? N3 C1 N2 103.4(8) . . ? N3 C1 Ir1 135.5(7) . . ? N2 C1 Ir1 121.0(6) . . ? C3 C2 N2 104.9(9) . . ? C3 C2 H2 127.6 . . ? N2 C2 H2 127.6 . . ? C2 C3 N3 110.7(9) . . ? C2 C3 H3 124.6 . . ? N3 C3 H3 124.6 . . ? C5 C4 C9 120.8(9) . . ? C5 C4 N2 118.3(8) . . ? C9 C4 N2 120.8(9) . . ? C4 C5 C6 119.0(9) . . ? C4 C5 N1 119.4(8) . . ? C6 C5 N1 121.5(9) . . ? C7 C6 C5 119.2(10) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C6 C7 C8 122.2(10) . . ? C6 C7 H7 118.9 . . ? C8 C7 H7 118.9 . . ? C9 C8 C7 119.1(11) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 120.5 . . ? C8 C9 C4 119.6(11) . . ? C8 C9 H9 120.2 . . ? C4 C9 H9 120.2 . . ? C11 C10 N3 110.7(9) . . ? C11 C10 C12 110.7(9) . . ? N3 C10 C12 110.7(8) . . ? C11 C10 H10 108.2 . . ? N3 C10 H10 108.2 . . ? C12 C10 H10 108.2 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C17 106.6(10) . . ? C14 C13 C18 129.5(10) . . ? C17 C13 C18 123.7(10) . . ? C14 C13 Ir1 70.5(6) . . ? C17 C13 Ir1 69.2(6) . . ? C18 C13 Ir1 129.3(7) . . ? C13 C14 C19 125.9(10) . . ? C13 C14 C15 110.1(9) . . ? C19 C14 C15 123.6(10) . . ? C13 C14 Ir1 71.8(6) . . ? C19 C14 Ir1 127.9(7) . . ? C15 C14 Ir1 72.7(5) . . ? C16 C15 C20 127.4(10) . . ? C16 C15 C14 105.6(9) . . ? C20 C15 C14 126.6(10) . . ? C16 C15 Ir1 72.2(6) . . ? C20 C15 Ir1 130.2(7) . . ? C14 C15 Ir1 67.2(5) . . ? C15 C16 C17 111.2(9) . . ? C15 C16 C21 128.9(11) . . ? C17 C16 C21 119.9(10) . . ? C15 C16 Ir1 72.0(6) . . ? C17 C16 Ir1 67.5(5) . . ? C21 C16 Ir1 127.3(7) . . ? C16 C17 C22 125.9(10) . . ? C16 C17 C13 106.2(9) . . ? C22 C17 C13 126.8(11) . . ? C16 C17 Ir1 73.7(6) . . ? C22 C17 Ir1 129.7(7) . . ? C13 C17 Ir1 70.7(6) . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? F3 C23 F1 107.0(12) . . ? F3 C23 F2 106.1(9) . . ? F1 C23 F2 106.7(10) . . ? F3 C23 C24 114.2(11) . . ? F1 C23 C24 111.1(9) . . ? F2 C23 C24 111.4(11) . . ? O2 C24 O1 130.3(11) . . ? O2 C24 C23 117.3(11) . . ? O1 C24 C23 112.3(11) . . ? 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 C5 -66.9(6) . . . . ? C17 Ir1 N1 C5 36.3(7) . . . . ? C14 Ir1 N1 C5 102.3(11) . . . . ? C13 Ir1 N1 C5 17.7(9) . . . . ? C15 Ir1 N1 C5 106.6(6) . . . . ? C16 Ir1 N1 C5 75.2(6) . . . . ? I1 Ir1 N1 C5 -162.3(6) . . . . ? C3 N3 C1 N2 0.2(11) . . . . ? C10 N3 C1 N2 -178.6(8) . . . . ? C3 N3 C1 Ir1 -174.5(8) . . . . ? C10 N3 C1 Ir1 6.7(16) . . . . ? C2 N2 C1 N3 1.7(11) . . . . ? C4 N2 C1 N3 -178.6(8) . . . . ? C2 N2 C1 Ir1 177.3(7) . . . . ? C4 N2 C1 Ir1 -3.0(13) . . . . ? N1 Ir1 C1 N3 -143.5(11) . . . . ? C17 Ir1 C1 N3 110.4(10) . . . . ? C14 Ir1 C1 N3 40.8(11) . . . . ? C13 Ir1 C1 N3 70.9(10) . . . . ? C15 Ir1 C1 N3 52.7(17) . . . . ? C16 Ir1 C1 N3 124.7(10) . . . . ? I1 Ir1 C1 N3 -61.1(10) . . . . ? N1 Ir1 C1 N2 42.5(7) . . . . ? C17 Ir1 C1 N2 -63.6(8) . . . . ? C14 Ir1 C1 N2 -133.1(7) . . . . ? C13 Ir1 C1 N2 -103.0(8) . . . . ? C15 Ir1 C1 N2 -121.2(11) . . . . ? C16 Ir1 C1 N2 -49.3(11) . . . . ? I1 Ir1 C1 N2 125.0(7) . . . . ? C1 N2 C2 C3 -3.0(12) . . . . ? C4 N2 C2 C3 177.3(10) . . . . ? N2 C2 C3 N3 3.0(13) . . . . ? C1 N3 C3 C2 -2.2(14) . . . . ? C10 N3 C3 C2 176.6(10) . . . . ? C1 N2 C4 C5 -33.5(14) . . . . ? C2 N2 C4 C5 146.1(10) . . . . ? C1 N2 C4 C9 143.8(10) . . . . ? C2 N2 C4 C9 -36.6(14) . . . . ? C9 C4 C5 C6 2.4(15) . . . . ? N2 C4 C5 C6 179.8(8) . . . . ? C9 C4 C5 N1 -175.7(9) . . . . ? N2 C4 C5 N1 1.6(13) . . . . ? Ir1 N1 C5 C4 55.0(10) . . . . ? Ir1 N1 C5 C6 -123.1(8) . . . . ? C4 C5 C6 C7 0.5(15) . . . . ? N1 C5 C6 C7 178.6(9) . . . . ? C5 C6 C7 C8 -2.7(16) . . . . ? C6 C7 C8 C9 1.8(17) . . . . ? C7 C8 C9 C4 1.2(16) . . . . ? C5 C4 C9 C8 -3.3(16) . . . . ? N2 C4 C9 C8 179.4(9) . . . . ? C1 N3 C10 C11 -126.5(10) . . . . ? C3 N3 C10 C11 54.9(13) . . . . ? C1 N3 C10 C12 110.4(11) . . . . ? C3 N3 C10 C12 -68.2(13) . . . . ? C1 Ir1 C13 C14 -134.8(6) . . . . ? N1 Ir1 C13 C14 145.3(6) . . . . ? C17 Ir1 C13 C14 117.2(9) . . . . ? C15 Ir1 C13 C14 38.3(6) . . . . ? C16 Ir1 C13 C14 77.9(6) . . . . ? I1 Ir1 C13 C14 -34.7(7) . . . . ? C1 Ir1 C13 C17 108.0(6) . . . . ? N1 Ir1 C13 C17 28.1(9) . . . . ? C14 Ir1 C13 C17 -117.2(9) . . . . ? C15 Ir1 C13 C17 -78.9(6) . . . . ? C16 Ir1 C13 C17 -39.3(6) . . . . ? I1 Ir1 C13 C17 -151.9(5) . . . . ? C1 Ir1 C13 C18 -9.2(10) . . . . ? N1 Ir1 C13 C18 -89.2(11) . . . . ? C17 Ir1 C13 C18 -117.2(13) . . . . ? C14 Ir1 C13 C18 125.6(13) . . . . ? C15 Ir1 C13 C18 163.9(11) . . . . ? C16 Ir1 C13 C18 -156.5(11) . . . . ? I1 Ir1 C13 C18 90.9(10) . . . . ? C17 C13 C14 C19 -175.8(9) . . . . ? C18 C13 C14 C19 -1.3(17) . . . . ? Ir1 C13 C14 C19 124.1(10) . . . . ? C17 C13 C14 C15 -2.9(11) . . . . ? C18 C13 C14 C15 171.6(10) . . . . ? Ir1 C13 C14 C15 -63.0(7) . . . . ? C17 C13 C14 Ir1 60.2(7) . . . . ? C18 C13 C14 Ir1 -125.3(11) . . . . ? C1 Ir1 C14 C13 54.7(7) . . . . ? N1 Ir1 C14 C13 -113.0(10) . . . . ? C17 Ir1 C14 C13 -39.3(6) . . . . ? C15 Ir1 C14 C13 -118.8(8) . . . . ? C16 Ir1 C14 C13 -82.7(6) . . . . ? I1 Ir1 C14 C13 154.3(5) . . . . ? C1 Ir1 C14 C19 -67.0(10) . . . . ? N1 Ir1 C14 C19 125.3(10) . . . . ? C17 Ir1 C14 C19 -161.0(11) . . . . ? C13 Ir1 C14 C19 -121.7(12) . . . . ? C15 Ir1 C14 C19 119.5(12) . . . . ? C16 Ir1 C14 C19 155.6(11) . . . . ? I1 Ir1 C14 C19 32.6(10) . . . . ? C1 Ir1 C14 C15 173.6(6) . . . . ? N1 Ir1 C14 C15 5.9(13) . . . . ? C17 Ir1 C14 C15 79.6(6) . . . . ? C13 Ir1 C14 C15 118.8(8) . . . . ? C16 Ir1 C14 C15 36.1(6) . . . . ? I1 Ir1 C14 C15 -86.8(6) . . . . ? C13 C14 C15 C16 -0.1(11) . . . . ? C19 C14 C15 C16 173.0(9) . . . . ? Ir1 C14 C15 C16 -62.5(7) . . . . ? C13 C14 C15 C20 -173.5(10) . . . . ? C19 C14 C15 C20 -0.4(16) . . . . ? Ir1 C14 C15 C20 124.0(10) . . . . ? C13 C14 C15 Ir1 62.4(7) . . . . ? C19 C14 C15 Ir1 -124.5(10) . . . . ? C1 Ir1 C15 C16 100.0(11) . . . . ? N1 Ir1 C15 C16 -61.5(7) . . . . ? C17 Ir1 C15 C16 35.6(6) . . . . ? C14 Ir1 C15 C16 116.2(9) . . . . ? C13 Ir1 C15 C16 80.1(7) . . . . ? I1 Ir1 C15 C16 -146.2(6) . . . . ? C1 Ir1 C15 C20 -135.6(11) . . . . ? N1 Ir1 C15 C20 62.9(10) . . . . ? C17 Ir1 C15 C20 160.0(11) . . . . ? C14 Ir1 C15 C20 -119.5(12) . . . . ? C13 Ir1 C15 C20 -155.6(11) . . . . ? C16 Ir1 C15 C20 124.4(12) . . . . ? I1 Ir1 C15 C20 -21.8(10) . . . . ? C1 Ir1 C15 C14 -16.1(14) . . . . ? N1 Ir1 C15 C14 -177.6(5) . . . . ? C17 Ir1 C15 C14 -80.6(6) . . . . ? C13 Ir1 C15 C14 -36.1(6) . . . . ? C16 Ir1 C15 C14 -116.2(9) . . . . ? I1 Ir1 C15 C14 97.6(6) . . . . ? C20 C15 C16 C17 176.5(9) . . . . ? C14 C15 C16 C17 3.1(11) . . . . ? Ir1 C15 C16 C17 -56.1(7) . . . . ? C20 C15 C16 C21 -3.6(18) . . . . ? C14 C15 C16 C21 -177.0(10) . . . . ? Ir1 C15 C16 C21 123.8(11) . . . . ? C20 C15 C16 Ir1 -127.4(11) . . . . ? C14 C15 C16 Ir1 59.2(6) . . . . ? C1 Ir1 C16 C15 -145.4(7) . . . . ? N1 Ir1 C16 C15 129.3(6) . . . . ? C17 Ir1 C16 C15 -123.1(9) . . . . ? C14 Ir1 C16 C15 -40.4(6) . . . . ? C13 Ir1 C16 C15 -82.6(7) . . . . ? I1 Ir1 C16 C15 41.4(7) . . . . ? C1 Ir1 C16 C17 -22.3(9) . . . . ? N1 Ir1 C16 C17 -107.6(6) . . . . ? C14 Ir1 C16 C17 82.7(6) . . . . ? C13 Ir1 C16 C17 40.5(6) . . . . ? C15 Ir1 C16 C17 123.1(9) . . . . ? I1 Ir1 C16 C17 164.5(5) . . . . ? C1 Ir1 C16 C21 89.0(12) . . . . ? N1 Ir1 C16 C21 3.7(11) . . . . ? C17 Ir1 C16 C21 111.2(13) . . . . ? C14 Ir1 C16 C21 -166.0(12) . . . . ? C13 Ir1 C16 C21 151.8(12) . . . . ? C15 Ir1 C16 C21 -125.6(13) . . . . ? I1 Ir1 C16 C21 -84.2(10) . . . . ? C15 C16 C17 C22 -173.8(10) . . . . ? C21 C16 C17 C22 6.3(16) . . . . ? Ir1 C16 C17 C22 127.5(11) . . . . ? C15 C16 C17 C13 -4.9(11) . . . . ? C21 C16 C17 C13 175.2(9) . . . . ? Ir1 C16 C17 C13 -63.6(6) . . . . ? C15 C16 C17 Ir1 58.7(7) . . . . ? C21 C16 C17 Ir1 -121.2(9) . . . . ? C14 C13 C17 C16 4.6(11) . . . . ? C18 C13 C17 C16 -170.3(9) . . . . ? Ir1 C13 C17 C16 65.6(7) . . . . ? C14 C13 C17 C22 173.4(10) . . . . ? C18 C13 C17 C22 -1.5(16) . . . . ? Ir1 C13 C17 C22 -125.6(11) . . . . ? C14 C13 C17 Ir1 -61.0(7) . . . . ? C18 C13 C17 Ir1 124.1(10) . . . . ? C1 Ir1 C17 C16 166.2(6) . . . . ? N1 Ir1 C17 C16 81.9(6) . . . . ? C14 Ir1 C17 C16 -77.4(6) . . . . ? C13 Ir1 C17 C16 -114.3(8) . . . . ? C15 Ir1 C17 C16 -32.9(5) . . . . ? I1 Ir1 C17 C16 -37.8(12) . . . . ? C1 Ir1 C17 C22 42.8(12) . . . . ? N1 Ir1 C17 C22 -41.5(12) . . . . ? C14 Ir1 C17 C22 159.2(12) . . . . ? C13 Ir1 C17 C22 122.3(14) . . . . ? C15 Ir1 C17 C22 -156.3(12) . . . . ? C16 Ir1 C17 C22 -123.4(14) . . . . ? I1 Ir1 C17 C22 -161.2(7) . . . . ? C1 Ir1 C17 C13 -79.5(7) . . . . ? N1 Ir1 C17 C13 -163.8(6) . . . . ? C14 Ir1 C17 C13 36.9(6) . . . . ? C15 Ir1 C17 C13 81.4(6) . . . . ? C16 Ir1 C17 C13 114.3(8) . . . . ? I1 Ir1 C17 C13 76.5(11) . . . . ? F3 C23 C24 O2 131.2(11) . . . . ? F1 C23 C24 O2 -107.7(12) . . . . ? F2 C23 C24 O2 11.2(15) . . . . ? F3 C23 C24 O1 -51.5(13) . . . . ? F1 C23 C24 O1 69.6(13) . . . . ? F2 C23 C24 O1 -171.6(9) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A I1 0.92 3.04 3.824(8) 144.1 2_656 N1 H1B O2 0.92 1.99 2.904(10) 173.1 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.991 _refine_diff_density_min -1.925 _refine_diff_density_rms 0.200