# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_ns97 _database_code_depnum_ccdc_archive 'CCDC 876632' #TrackingRef '- ns97.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H34 Ir N6, F6 P, 0.5(H2 O)' _chemical_formula_sum 'C48 H35 F6 Ir N6 O0.50 P' _chemical_formula_weight 1040.99 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' P P 0.1023 0.0942 '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 Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 10.7181(13) _cell_length_b 17.865(3) _cell_length_c 41.906(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8024.3(19) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 187 _cell_measurement_theta_min 3 _cell_measurement_theta_max 22 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4120 _exptl_absorpt_coefficient_mu 3.442 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5998 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'SADABS 2008, Bruker AXS, 2008' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II CCD' _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 123459 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -54 _diffrn_reflns_limit_l_max 54 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9194 _reflns_number_gt 7799 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs, 1990-2000)' _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^)+(0.0186P)^2^+28.7626P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9194 _refine_ls_number_parameters 574 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.0814 _refine_ls_wR_factor_gt 0.0777 _refine_ls_goodness_of_fit_ref 1.174 _refine_ls_restrained_S_all 1.174 _refine_ls_shift/su_max 0.004 _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 0.569282(15) 0.200837(10) 0.329547(4) 0.02337(6) Uani 1 1 d . . . N1 N 0.4075(3) 0.1583(2) 0.34783(8) 0.0270(8) Uani 1 1 d . . . N2 N 0.7164(3) 0.2509(2) 0.30669(8) 0.0237(8) Uani 1 1 d . . . N3 N 0.6874(3) 0.1097(2) 0.34190(8) 0.0257(8) Uani 1 1 d . . . N4 N 0.6292(3) 0.2285(2) 0.37689(8) 0.0257(8) Uani 1 1 d . . . N5 N 0.9881(4) 0.0383(2) 0.42512(9) 0.0345(10) Uani 1 1 d . . . N6 N 0.9365(4) 0.1350(2) 0.45647(9) 0.0325(9) Uani 1 1 d . . . C1 C 0.3941(4) 0.0886(3) 0.35864(11) 0.0325(11) Uani 1 1 d . . . H1 H 0.4648 0.0565 0.3590 0.039 Uiso 1 1 calc R . . C2 C 0.2811(5) 0.0615(3) 0.36934(11) 0.0394(12) Uani 1 1 d . . . H2 H 0.2734 0.0113 0.3766 0.047 Uiso 1 1 calc R . . C3 C 0.1803(5) 0.1084(3) 0.36931(12) 0.0433(13) Uani 1 1 d . . . H3 H 0.1016 0.0905 0.3764 0.052 Uiso 1 1 calc R . . C4 C 0.1917(5) 0.1796(3) 0.35930(12) 0.0399(13) Uani 1 1 d . . . H4 H 0.1219 0.2123 0.3600 0.048 Uiso 1 1 calc R . . C5 C 0.3076(4) 0.2054(3) 0.34777(10) 0.0297(10) Uani 1 1 d . . . C6 C 0.3329(4) 0.2793(3) 0.33441(10) 0.0303(10) Uani 1 1 d . . . C7 C 0.2439(5) 0.3360(3) 0.33215(12) 0.0387(12) Uani 1 1 d . . . H7 H 0.1625 0.3284 0.3405 0.046 Uiso 1 1 calc R . . C8 C 0.2739(5) 0.4032(3) 0.31780(12) 0.0399(12) Uani 1 1 d . . . H8 H 0.2133 0.4418 0.3162 0.048 Uiso 1 1 calc R . . C9 C 0.3920(5) 0.4139(3) 0.30578(12) 0.0369(12) Uani 1 1 d . . . H9 H 0.4129 0.4601 0.2959 0.044 Uiso 1 1 calc R . . C10 C 0.4813(5) 0.3572(3) 0.30811(11) 0.0320(11) Uani 1 1 d . . . H10 H 0.5621 0.3656 0.2995 0.038 Uiso 1 1 calc R . . C11 C 0.4559(4) 0.2891(3) 0.32256(10) 0.0265(10) Uani 1 1 d . . . C12 C 0.5346(4) 0.1668(3) 0.28462(10) 0.0246(9) Uani 1 1 d . . . C13 C 0.4423(4) 0.1188(3) 0.27368(11) 0.0290(10) Uani 1 1 d . . . H13 H 0.3834 0.0990 0.2884 0.035 Uiso 1 1 calc R . . C14 C 0.4339(4) 0.0988(3) 0.24165(11) 0.0324(10) Uani 1 1 d . . . H14 H 0.3701 0.0655 0.2349 0.039 Uiso 1 1 calc R . . C15 C 0.5183(4) 0.1274(3) 0.21936(10) 0.0297(10) Uani 1 1 d . . . H15 H 0.5119 0.1141 0.1975 0.036 Uiso 1 1 calc R . . C16 C 0.6098(4) 0.1746(3) 0.22943(11) 0.0295(10) Uani 1 1 d . . . H16 H 0.6677 0.1942 0.2144 0.035 Uiso 1 1 calc R . . C17 C 0.6198(4) 0.1947(3) 0.26180(10) 0.0252(9) Uani 1 1 d . . . C18 C 0.7178(4) 0.2437(3) 0.27446(10) 0.0258(10) Uani 1 1 d . . . C19 C 0.8086(4) 0.2815(3) 0.25671(10) 0.0289(10) Uani 1 1 d . . . H19 H 0.8095 0.2772 0.2341 0.035 Uiso 1 1 calc R . . C20 C 0.8966(4) 0.3248(3) 0.27180(11) 0.0337(11) Uani 1 1 d . . . H20 H 0.9581 0.3506 0.2597 0.040 Uiso 1 1 calc R . . C21 C 0.8946(4) 0.3305(3) 0.30450(11) 0.0296(10) Uani 1 1 d . . . H21 H 0.9551 0.3599 0.3154 0.035 Uiso 1 1 calc R . . C22 C 0.8031(4) 0.2929(3) 0.32122(10) 0.0277(10) Uani 1 1 d . . . H22 H 0.8016 0.2969 0.3438 0.033 Uiso 1 1 calc R . . C23 C 0.7137(4) 0.0501(3) 0.32396(10) 0.0296(10) Uani 1 1 d . . . H23 H 0.6709 0.0438 0.3043 0.035 Uiso 1 1 calc R . . C24 C 0.8011(4) -0.0030(3) 0.33293(10) 0.0297(10) Uani 1 1 d . . . H24 H 0.8181 -0.0441 0.3192 0.036 Uiso 1 1 calc R . . C25 C 0.8620(4) 0.0031(3) 0.36087(11) 0.0291(10) Uani 1 1 d . . . H25 H 0.9222 -0.0333 0.3669 0.035 Uiso 1 1 calc R . . C26 C 0.8354(4) 0.0640(3) 0.38095(10) 0.0281(10) Uani 1 1 d . . . C27 C 0.7468(4) 0.1161(3) 0.37059(10) 0.0262(10) Uani 1 1 d . . . C28 C 0.7134(4) 0.1800(3) 0.38983(10) 0.0253(9) Uani 1 1 d . . . C29 C 0.5931(4) 0.2877(3) 0.39372(10) 0.0285(10) Uani 1 1 d . . . H29 H 0.5341 0.3212 0.3847 0.034 Uiso 1 1 calc R . . C30 C 0.6389(4) 0.3024(3) 0.42413(10) 0.0326(11) Uani 1 1 d . . . H30 H 0.6100 0.3447 0.4357 0.039 Uiso 1 1 calc R . . C31 C 0.7260(4) 0.2553(3) 0.43731(10) 0.0313(11) Uani 1 1 d . . . H31 H 0.7587 0.2656 0.4579 0.038 Uiso 1 1 calc R . . C32 C 0.7668(4) 0.1923(3) 0.42059(10) 0.0276(10) Uani 1 1 d . . . C33 C 0.8587(4) 0.1385(3) 0.42982(10) 0.0302(11) Uani 1 1 d . . . C34 C 0.8921(4) 0.0781(3) 0.41132(11) 0.0319(11) Uani 1 1 d . . . C35 C 1.0132(4) 0.0735(3) 0.45209(11) 0.0345(11) Uani 1 1 d . . . C36 C 1.1184(4) 0.0519(3) 0.47305(11) 0.0357(12) Uani 1 1 d . . . C37 C 1.2188(5) 0.0163(4) 0.45881(12) 0.0477(15) Uani 1 1 d . . . H37 H 1.2176 0.0072 0.4365 0.057 Uiso 1 1 calc R . . C38 C 1.3212(5) -0.0065(4) 0.47671(14) 0.0516(15) Uani 1 1 d . . . H38 H 1.3887 -0.0317 0.4667 0.062 Uiso 1 1 calc R . . C39 C 1.3248(5) 0.0076(3) 0.50898(13) 0.0446(13) Uani 1 1 d . . . H39 H 1.3953 -0.0070 0.5212 0.054 Uiso 1 1 calc R . . C40 C 1.2260(5) 0.0428(3) 0.52335(12) 0.0393(12) Uani 1 1 d . . . H40 H 1.2278 0.0518 0.5457 0.047 Uiso 1 1 calc R . . C41 C 1.1240(5) 0.0652(3) 0.50574(11) 0.0355(11) Uani 1 1 d . . . H41 H 1.0567 0.0899 0.5160 0.043 Uiso 1 1 calc R . . C42 C 0.9334(4) 0.1867(3) 0.48313(10) 0.0331(11) Uani 1 1 d . . . C43 C 1.0064(5) 0.2493(3) 0.48308(12) 0.0382(12) Uani 1 1 d . . . H43 H 1.0624 0.2590 0.4660 0.046 Uiso 1 1 calc R . . C44 C 0.9967(5) 0.2984(3) 0.50858(13) 0.0483(14) Uani 1 1 d . . . H44 H 1.0464 0.3424 0.5086 0.058 Uiso 1 1 calc R . . C45 C 0.9179(6) 0.2855(4) 0.53381(14) 0.0507(15) Uani 1 1 d . . . C46 C 0.8467(5) 0.2218(4) 0.53348(12) 0.0511(16) Uani 1 1 d . . . H46 H 0.7927 0.2116 0.5509 0.061 Uiso 1 1 calc R . . C47 C 0.8521(5) 0.1716(4) 0.50795(12) 0.0432(13) Uani 1 1 d . . . H47 H 0.8011 0.1282 0.5076 0.052 Uiso 1 1 calc R . . C48 C 0.9108(7) 0.3375(4) 0.56178(15) 0.073(2) Uani 1 1 d . . . H48A H 0.8408 0.3229 0.5755 0.110 Uiso 1 1 calc R . . H48B H 0.8982 0.3888 0.5542 0.110 Uiso 1 1 calc R . . H48C H 0.9887 0.3347 0.5740 0.110 Uiso 1 1 calc R . . P1 P 0.97772(12) 0.39854(8) 0.40013(3) 0.0313(3) Uani 1 1 d . . . F1 F 0.9496(3) 0.37227(18) 0.43568(7) 0.0453(8) Uani 1 1 d . . . F2 F 1.1239(3) 0.3949(2) 0.40715(8) 0.0564(9) Uani 1 1 d . . . F3 F 0.9740(3) 0.48395(18) 0.41123(7) 0.0506(8) Uani 1 1 d . . . F4 F 1.0070(3) 0.42537(17) 0.36433(6) 0.0433(7) Uani 1 1 d . . . F5 F 0.8327(3) 0.40142(19) 0.39266(7) 0.0499(8) Uani 1 1 d . . . F6 F 0.9811(3) 0.31352(17) 0.38853(7) 0.0500(8) Uani 1 1 d . . . O1 O 1.0973(7) -0.0912(5) 0.4001(2) 0.056(2) Uani 0.50 1 d PD . . H1A H 1.058(9) -0.049(5) 0.412(3) 0.084 Uiso 0.50 1 d PD . . H1B H 1.180(5) -0.094(7) 0.410(3) 0.084 Uiso 0.50 1 d PD . . 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 0.01889(8) 0.03583(10) 0.01538(8) -0.00226(7) -0.00078(6) -0.00240(7) N1 0.0230(19) 0.039(2) 0.0188(19) -0.0036(16) -0.0023(15) -0.0026(16) N2 0.0173(17) 0.033(2) 0.0205(18) -0.0008(15) 0.0007(14) -0.0009(15) N3 0.0200(18) 0.038(2) 0.0190(18) -0.0048(16) 0.0010(14) -0.0067(16) N4 0.0205(18) 0.040(2) 0.0164(18) -0.0003(16) 0.0013(14) -0.0027(16) N5 0.030(2) 0.055(3) 0.019(2) 0.0063(18) 0.0037(16) 0.0057(19) N6 0.026(2) 0.055(3) 0.0160(18) 0.0010(17) -0.0034(16) 0.0023(19) C1 0.028(2) 0.047(3) 0.022(2) -0.008(2) -0.0018(19) -0.005(2) C2 0.037(3) 0.055(3) 0.027(3) -0.003(2) 0.001(2) -0.014(3) C3 0.026(3) 0.071(4) 0.033(3) -0.001(3) 0.004(2) -0.012(3) C4 0.027(3) 0.062(4) 0.030(3) -0.003(2) 0.002(2) 0.004(2) C5 0.023(2) 0.051(3) 0.015(2) -0.004(2) -0.0020(17) 0.001(2) C6 0.031(2) 0.044(3) 0.016(2) -0.0077(19) -0.0011(18) 0.003(2) C7 0.029(2) 0.055(3) 0.033(3) -0.012(2) 0.002(2) 0.010(2) C8 0.041(3) 0.046(3) 0.033(3) -0.013(2) -0.005(2) 0.012(2) C9 0.041(3) 0.034(3) 0.036(3) -0.004(2) -0.008(2) -0.002(2) C10 0.031(2) 0.040(3) 0.025(2) -0.007(2) -0.004(2) -0.006(2) C11 0.023(2) 0.039(3) 0.018(2) -0.0081(18) -0.0042(16) 0.0001(19) C12 0.022(2) 0.032(2) 0.020(2) -0.0003(18) -0.0028(17) 0.0011(18) C13 0.026(2) 0.035(3) 0.026(2) -0.0001(19) 0.0018(19) -0.001(2) C14 0.032(2) 0.038(3) 0.027(2) -0.003(2) -0.009(2) -0.004(2) C15 0.038(3) 0.036(3) 0.015(2) -0.0069(19) -0.0051(19) 0.000(2) C16 0.027(2) 0.041(3) 0.021(2) 0.001(2) 0.0006(19) 0.000(2) C17 0.023(2) 0.032(2) 0.021(2) -0.0015(19) -0.0002(17) 0.0044(19) C18 0.025(2) 0.036(3) 0.017(2) 0.0003(18) -0.0043(17) 0.0028(19) C19 0.028(2) 0.039(3) 0.020(2) 0.0015(18) 0.0044(19) -0.001(2) C20 0.027(2) 0.046(3) 0.028(3) 0.006(2) 0.007(2) 0.000(2) C21 0.020(2) 0.039(3) 0.029(2) -0.008(2) -0.0020(18) -0.0026(19) C22 0.021(2) 0.040(3) 0.022(2) -0.0044(19) -0.0016(17) 0.001(2) C23 0.026(2) 0.043(3) 0.020(2) -0.0003(19) 0.0022(18) -0.010(2) C24 0.029(2) 0.038(3) 0.023(2) 0.000(2) 0.0072(19) -0.001(2) C25 0.024(2) 0.035(3) 0.029(2) 0.004(2) 0.0037(19) -0.001(2) C26 0.024(2) 0.041(3) 0.020(2) 0.0033(19) 0.0032(18) -0.006(2) C27 0.016(2) 0.042(3) 0.020(2) 0.0004(19) 0.0013(17) -0.0045(19) C28 0.020(2) 0.038(3) 0.018(2) 0.0005(18) 0.0016(17) -0.0056(19) C29 0.022(2) 0.041(3) 0.023(2) -0.002(2) 0.0005(17) -0.0043(19) C30 0.027(2) 0.047(3) 0.023(2) -0.008(2) 0.0037(19) -0.001(2) C31 0.027(2) 0.053(3) 0.015(2) -0.001(2) 0.0004(18) -0.008(2) C32 0.022(2) 0.045(3) 0.016(2) -0.0013(19) 0.0023(17) -0.004(2) C33 0.025(2) 0.050(3) 0.015(2) 0.002(2) -0.0007(18) -0.002(2) C34 0.025(2) 0.051(3) 0.020(2) 0.006(2) 0.0021(18) -0.001(2) C35 0.027(2) 0.057(3) 0.019(2) 0.005(2) 0.0017(19) 0.001(2) C36 0.025(2) 0.056(3) 0.026(3) 0.006(2) -0.002(2) 0.003(2) C37 0.036(3) 0.081(4) 0.026(3) 0.011(3) 0.002(2) 0.009(3) C38 0.032(3) 0.079(4) 0.043(3) 0.006(3) 0.002(2) 0.011(3) C39 0.029(3) 0.068(4) 0.037(3) 0.003(3) -0.010(2) -0.002(3) C40 0.034(3) 0.054(3) 0.030(3) -0.005(2) -0.010(2) -0.001(2) C41 0.030(2) 0.049(3) 0.028(3) -0.004(2) -0.009(2) 0.000(2) C42 0.025(2) 0.057(3) 0.018(2) 0.001(2) -0.0030(18) 0.006(2) C43 0.035(3) 0.050(3) 0.030(3) 0.004(2) -0.007(2) 0.003(2) C44 0.045(3) 0.054(3) 0.046(3) -0.003(3) -0.018(3) 0.006(3) C45 0.045(3) 0.066(4) 0.042(3) -0.010(3) -0.015(3) 0.019(3) C46 0.034(3) 0.097(5) 0.022(3) -0.004(3) 0.000(2) 0.017(3) C47 0.027(3) 0.074(4) 0.028(3) -0.001(3) -0.003(2) -0.001(3) C48 0.084(5) 0.089(5) 0.046(4) -0.029(4) -0.025(4) 0.042(4) P1 0.0267(6) 0.0446(7) 0.0227(6) -0.0013(5) 0.0023(5) 0.0021(6) F1 0.0433(18) 0.067(2) 0.0255(15) 0.0075(14) 0.0047(13) 0.0007(15) F2 0.0257(15) 0.095(3) 0.0490(19) 0.0013(19) 0.0016(14) -0.0001(17) F3 0.069(2) 0.051(2) 0.0317(16) -0.0090(14) 0.0116(15) -0.0023(17) F4 0.0570(19) 0.0505(18) 0.0224(14) -0.0026(13) 0.0072(13) -0.0068(15) F5 0.0295(15) 0.071(2) 0.0486(19) 0.0118(17) -0.0054(14) 0.0016(15) F6 0.061(2) 0.0435(19) 0.0451(18) -0.0012(14) 0.0067(16) 0.0034(16) O1 0.027(4) 0.071(6) 0.070(6) -0.015(5) -0.017(4) 0.001(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 C11 2.012(5) . ? Ir1 C12 2.013(4) . ? Ir1 N1 2.042(4) . ? Ir1 N2 2.050(3) . ? Ir1 N3 2.126(4) . ? Ir1 N4 2.143(3) . ? N1 C1 1.333(6) . ? N1 C5 1.361(6) . ? N2 C22 1.342(5) . ? N2 C18 1.357(5) . ? N3 C23 1.334(6) . ? N3 C27 1.365(5) . ? N4 C29 1.328(6) . ? N4 C28 1.364(6) . ? N5 C35 1.321(6) . ? N5 C34 1.378(6) . ? N6 C35 1.384(6) . ? N6 C33 1.395(5) . ? N6 C42 1.449(6) . ? C1 C2 1.380(7) . ? C1 H1 0.9500 . ? C2 C3 1.367(7) . ? C2 H2 0.9500 . ? C3 C4 1.345(8) . ? C3 H3 0.9500 . ? C4 C5 1.411(7) . ? C4 H4 0.9500 . ? C5 C6 1.459(7) . ? C6 C7 1.395(7) . ? C6 C11 1.420(6) . ? C7 C8 1.380(8) . ? C7 H7 0.9500 . ? C8 C9 1.376(7) . ? C8 H8 0.9500 . ? C9 C10 1.398(7) . ? C9 H9 0.9500 . ? C10 C11 1.386(7) . ? C10 H10 0.9500 . ? C12 C13 1.388(6) . ? C12 C17 1.413(6) . ? C13 C14 1.391(6) . ? C13 H13 0.9500 . ? C14 C15 1.397(7) . ? C14 H14 0.9500 . ? C15 C16 1.361(6) . ? C15 H15 0.9500 . ? C16 C17 1.407(6) . ? C16 H16 0.9500 . ? C17 C18 1.467(6) . ? C18 C19 1.399(6) . ? C19 C20 1.373(7) . ? C19 H19 0.9500 . ? C20 C21 1.374(6) . ? C20 H20 0.9500 . ? C21 C22 1.380(6) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.385(6) . ? C23 H23 0.9500 . ? C24 C25 1.345(6) . ? C24 H24 0.9500 . ? C25 C26 1.404(6) . ? C25 H25 0.9500 . ? C26 C27 1.399(6) . ? C26 C34 1.433(6) . ? C27 C28 1.443(6) . ? C28 C32 1.427(6) . ? C29 C30 1.391(6) . ? C29 H29 0.9500 . ? C30 C31 1.373(7) . ? C30 H30 0.9500 . ? C31 C32 1.395(7) . ? C31 H31 0.9500 . ? C32 C33 1.430(6) . ? C33 C34 1.376(7) . ? C35 C36 1.481(6) . ? C36 C37 1.385(7) . ? C36 C41 1.392(7) . ? C37 C38 1.391(7) . ? C37 H37 0.9500 . ? C38 C39 1.376(8) . ? C38 H38 0.9500 . ? C39 C40 1.371(7) . ? C39 H39 0.9500 . ? C40 C41 1.378(6) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C43 1.366(7) . ? C42 C47 1.383(7) . ? C43 C44 1.386(7) . ? C43 H43 0.9500 . ? C44 C45 1.373(8) . ? C44 H44 0.9500 . ? C45 C46 1.369(9) . ? C45 C48 1.498(8) . ? C46 C47 1.397(8) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? P1 F5 1.586(3) . ? P1 F1 1.591(3) . ? P1 F2 1.595(3) . ? P1 F6 1.595(3) . ? P1 F3 1.596(3) . ? P1 F4 1.606(3) . ? O1 H1A 0.99(2) . ? O1 H1B 0.98(2) . ? 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 C11 Ir1 C12 89.39(17) . . ? C11 Ir1 N1 80.41(17) . . ? C12 Ir1 N1 94.70(16) . . ? C11 Ir1 N2 93.13(16) . . ? C12 Ir1 N2 80.59(16) . . ? N1 Ir1 N2 172.09(14) . . ? C11 Ir1 N3 174.26(15) . . ? C12 Ir1 N3 96.10(16) . . ? N1 Ir1 N3 97.42(14) . . ? N2 Ir1 N3 89.43(14) . . ? C11 Ir1 N4 97.73(15) . . ? C12 Ir1 N4 172.22(16) . . ? N1 Ir1 N4 89.59(14) . . ? N2 Ir1 N4 95.83(14) . . ? N3 Ir1 N4 76.89(14) . . ? C1 N1 C5 119.5(4) . . ? C1 N1 Ir1 124.5(3) . . ? C5 N1 Ir1 115.9(3) . . ? C22 N2 C18 119.8(4) . . ? C22 N2 Ir1 124.4(3) . . ? C18 N2 Ir1 115.7(3) . . ? C23 N3 C27 117.7(4) . . ? C23 N3 Ir1 126.9(3) . . ? C27 N3 Ir1 115.3(3) . . ? C29 N4 C28 119.2(4) . . ? C29 N4 Ir1 126.0(3) . . ? C28 N4 Ir1 114.8(3) . . ? C35 N5 C34 105.4(4) . . ? C35 N6 C33 106.5(4) . . ? C35 N6 C42 128.4(4) . . ? C33 N6 C42 125.1(4) . . ? N1 C1 C2 122.2(5) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 118.6(5) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C4 C3 C2 120.5(5) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 119.8(5) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? N1 C5 C4 119.3(5) . . ? N1 C5 C6 114.4(4) . . ? C4 C5 C6 126.2(4) . . ? C7 C6 C11 121.4(5) . . ? C7 C6 C5 123.8(5) . . ? C11 C6 C5 114.7(4) . . ? C8 C7 C6 120.1(5) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C9 C8 C7 119.7(5) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 120.2(5) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C11 C10 C9 122.2(5) . . ? C11 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? C10 C11 C6 116.4(4) . . ? C10 C11 Ir1 129.3(3) . . ? C6 C11 Ir1 114.4(3) . . ? C13 C12 C17 117.1(4) . . ? C13 C12 Ir1 128.8(3) . . ? C17 C12 Ir1 114.0(3) . . ? C12 C13 C14 121.5(4) . . ? C12 C13 H13 119.2 . . ? C14 C13 H13 119.2 . . ? C13 C14 C15 120.6(4) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C16 C15 C14 119.1(4) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? C15 C16 C17 120.8(4) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C16 C17 C12 120.9(4) . . ? C16 C17 C18 123.7(4) . . ? C12 C17 C18 115.4(4) . . ? N2 C18 C19 119.5(4) . . ? N2 C18 C17 114.1(4) . . ? C19 C18 C17 126.5(4) . . ? C20 C19 C18 120.3(4) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C21 119.4(4) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? C20 C21 C22 118.7(4) . . ? C20 C21 H21 120.6 . . ? C22 C21 H21 120.6 . . ? N2 C22 C21 122.4(4) . . ? N2 C22 H22 118.8 . . ? C21 C22 H22 118.8 . . ? N3 C23 C24 122.5(4) . . ? N3 C23 H23 118.8 . . ? C24 C23 H23 118.8 . . ? C25 C24 C23 120.6(4) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 119.0(4) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? C27 C26 C25 117.9(4) . . ? C27 C26 C34 116.5(4) . . ? C25 C26 C34 125.6(4) . . ? N3 C27 C26 122.3(4) . . ? N3 C27 C28 116.3(4) . . ? C26 C27 C28 121.4(4) . . ? N4 C28 C32 121.8(4) . . ? N4 C28 C27 116.4(4) . . ? C32 C28 C27 121.8(4) . . ? N4 C29 C30 122.3(4) . . ? N4 C29 H29 118.9 . . ? C30 C29 H29 118.9 . . ? C31 C30 C29 119.5(5) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C30 C31 C32 120.3(4) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C31 C32 C28 116.9(4) . . ? C31 C32 C33 128.5(4) . . ? C28 C32 C33 114.6(4) . . ? C34 C33 N6 105.1(4) . . ? C34 C33 C32 123.7(4) . . ? N6 C33 C32 131.1(4) . . ? C33 C34 N5 111.2(4) . . ? C33 C34 C26 121.9(4) . . ? N5 C34 C26 126.8(5) . . ? N5 C35 N6 111.8(4) . . ? N5 C35 C36 122.5(5) . . ? N6 C35 C36 125.5(4) . . ? C37 C36 C41 118.0(5) . . ? C37 C36 C35 117.1(4) . . ? C41 C36 C35 124.9(5) . . ? C36 C37 C38 121.0(5) . . ? C36 C37 H37 119.5 . . ? C38 C37 H37 119.5 . . ? C39 C38 C37 119.9(5) . . ? C39 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? C40 C39 C38 119.6(5) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C39 C40 C41 120.7(5) . . ? C39 C40 H40 119.6 . . ? C41 C40 H40 119.6 . . ? C40 C41 C36 120.8(5) . . ? C40 C41 H41 119.6 . . ? C36 C41 H41 119.6 . . ? C43 C42 C47 121.4(5) . . ? C43 C42 N6 120.5(4) . . ? C47 C42 N6 118.1(5) . . ? C42 C43 C44 118.3(5) . . ? C42 C43 H43 120.9 . . ? C44 C43 H43 120.9 . . ? C45 C44 C43 122.3(6) . . ? C45 C44 H44 118.9 . . ? C43 C44 H44 118.9 . . ? C46 C45 C44 118.3(5) . . ? C46 C45 C48 119.7(6) . . ? C44 C45 C48 122.0(6) . . ? C45 C46 C47 121.2(5) . . ? C45 C46 H46 119.4 . . ? C47 C46 H46 119.4 . . ? C42 C47 C46 118.5(5) . . ? C42 C47 H47 120.8 . . ? C46 C47 H47 120.8 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? F5 P1 F1 90.51(17) . . ? F5 P1 F2 179.1(2) . . ? F1 P1 F2 90.05(17) . . ? F5 P1 F6 89.59(19) . . ? F1 P1 F6 90.50(18) . . ? F2 P1 F6 89.7(2) . . ? F5 P1 F3 90.12(19) . . ? F1 P1 F3 90.24(17) . . ? F2 P1 F3 90.6(2) . . ? F6 P1 F3 179.21(19) . . ? F5 P1 F4 89.87(17) . . ? F1 P1 F4 179.6(2) . . ? F2 P1 F4 89.58(18) . . ? F6 P1 F4 89.72(17) . . ? F3 P1 F4 89.54(16) . . ? H1A O1 H1B 102(3) . . ? 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 C11 Ir1 N1 C1 176.4(4) . . . . ? C12 Ir1 N1 C1 87.9(4) . . . . ? N3 Ir1 N1 C1 -8.9(4) . . . . ? N4 Ir1 N1 C1 -85.6(4) . . . . ? C11 Ir1 N1 C5 -1.7(3) . . . . ? C12 Ir1 N1 C5 -90.3(3) . . . . ? N3 Ir1 N1 C5 173.0(3) . . . . ? N4 Ir1 N1 C5 96.2(3) . . . . ? C11 Ir1 N2 C22 91.0(4) . . . . ? C12 Ir1 N2 C22 179.9(4) . . . . ? N3 Ir1 N2 C22 -83.8(4) . . . . ? N4 Ir1 N2 C22 -7.1(4) . . . . ? C11 Ir1 N2 C18 -84.4(3) . . . . ? C12 Ir1 N2 C18 4.5(3) . . . . ? N3 Ir1 N2 C18 100.7(3) . . . . ? N4 Ir1 N2 C18 177.5(3) . . . . ? C12 Ir1 N3 C23 -4.4(4) . . . . ? N1 Ir1 N3 C23 91.2(4) . . . . ? N2 Ir1 N3 C23 -84.8(4) . . . . ? N4 Ir1 N3 C23 179.0(4) . . . . ? C12 Ir1 N3 C27 171.7(3) . . . . ? N1 Ir1 N3 C27 -92.7(3) . . . . ? N2 Ir1 N3 C27 91.3(3) . . . . ? N4 Ir1 N3 C27 -4.9(3) . . . . ? C11 Ir1 N4 C29 0.6(4) . . . . ? N1 Ir1 N4 C29 -79.6(4) . . . . ? N2 Ir1 N4 C29 94.6(4) . . . . ? N3 Ir1 N4 C29 -177.3(4) . . . . ? C11 Ir1 N4 C28 -178.3(3) . . . . ? N1 Ir1 N4 C28 101.4(3) . . . . ? N2 Ir1 N4 C28 -84.4(3) . . . . ? N3 Ir1 N4 C28 3.7(3) . . . . ? C5 N1 C1 C2 1.3(7) . . . . ? Ir1 N1 C1 C2 -176.8(3) . . . . ? N1 C1 C2 C3 -1.2(7) . . . . ? C1 C2 C3 C4 -0.5(8) . . . . ? C2 C3 C4 C5 2.0(8) . . . . ? C1 N1 C5 C4 0.2(6) . . . . ? Ir1 N1 C5 C4 178.5(3) . . . . ? C1 N1 C5 C6 -178.1(4) . . . . ? Ir1 N1 C5 C6 0.2(5) . . . . ? C3 C4 C5 N1 -1.9(7) . . . . ? C3 C4 C5 C6 176.2(5) . . . . ? N1 C5 C6 C7 -179.8(4) . . . . ? C4 C5 C6 C7 2.0(7) . . . . ? N1 C5 C6 C11 2.3(5) . . . . ? C4 C5 C6 C11 -175.9(4) . . . . ? C11 C6 C7 C8 0.8(7) . . . . ? C5 C6 C7 C8 -176.9(4) . . . . ? C6 C7 C8 C9 -0.1(7) . . . . ? C7 C8 C9 C10 -0.1(7) . . . . ? C8 C9 C10 C11 -0.5(7) . . . . ? C9 C10 C11 C6 1.2(6) . . . . ? C9 C10 C11 Ir1 -178.5(3) . . . . ? C7 C6 C11 C10 -1.4(6) . . . . ? C5 C6 C11 C10 176.6(4) . . . . ? C7 C6 C11 Ir1 178.4(3) . . . . ? C5 C6 C11 Ir1 -3.7(5) . . . . ? C12 Ir1 C11 C10 -82.5(4) . . . . ? N1 Ir1 C11 C10 -177.4(4) . . . . ? N2 Ir1 C11 C10 -2.0(4) . . . . ? N4 Ir1 C11 C10 94.3(4) . . . . ? C12 Ir1 C11 C6 97.7(3) . . . . ? N1 Ir1 C11 C6 2.9(3) . . . . ? N2 Ir1 C11 C6 178.3(3) . . . . ? N4 Ir1 C11 C6 -85.4(3) . . . . ? C11 Ir1 C12 C13 -90.9(4) . . . . ? N1 Ir1 C12 C13 -10.6(4) . . . . ? N2 Ir1 C12 C13 175.8(4) . . . . ? N3 Ir1 C12 C13 87.4(4) . . . . ? C11 Ir1 C12 C17 91.3(3) . . . . ? N1 Ir1 C12 C17 171.6(3) . . . . ? N2 Ir1 C12 C17 -2.0(3) . . . . ? N3 Ir1 C12 C17 -90.4(3) . . . . ? C17 C12 C13 C14 0.0(7) . . . . ? Ir1 C12 C13 C14 -177.7(4) . . . . ? C12 C13 C14 C15 -0.6(7) . . . . ? C13 C14 C15 C16 0.6(7) . . . . ? C14 C15 C16 C17 -0.1(7) . . . . ? C15 C16 C17 C12 -0.5(7) . . . . ? C15 C16 C17 C18 178.5(4) . . . . ? C13 C12 C17 C16 0.5(7) . . . . ? Ir1 C12 C17 C16 178.6(3) . . . . ? C13 C12 C17 C18 -178.5(4) . . . . ? Ir1 C12 C17 C18 -0.5(5) . . . . ? C22 N2 C18 C19 -1.1(6) . . . . ? Ir1 N2 C18 C19 174.5(3) . . . . ? C22 N2 C18 C17 178.5(4) . . . . ? Ir1 N2 C18 C17 -5.9(5) . . . . ? C16 C17 C18 N2 -174.8(4) . . . . ? C12 C17 C18 N2 4.2(6) . . . . ? C16 C17 C18 C19 4.7(7) . . . . ? C12 C17 C18 C19 -176.3(4) . . . . ? N2 C18 C19 C20 0.7(7) . . . . ? C17 C18 C19 C20 -178.8(4) . . . . ? C18 C19 C20 C21 0.1(7) . . . . ? C19 C20 C21 C22 -0.6(7) . . . . ? C18 N2 C22 C21 0.7(7) . . . . ? Ir1 N2 C22 C21 -174.5(3) . . . . ? C20 C21 C22 N2 0.2(7) . . . . ? C27 N3 C23 C24 -2.3(6) . . . . ? Ir1 N3 C23 C24 173.8(3) . . . . ? N3 C23 C24 C25 1.2(7) . . . . ? C23 C24 C25 C26 0.3(7) . . . . ? C24 C25 C26 C27 -0.6(6) . . . . ? C24 C25 C26 C34 179.9(4) . . . . ? C23 N3 C27 C26 1.9(6) . . . . ? Ir1 N3 C27 C26 -174.6(3) . . . . ? C23 N3 C27 C28 -178.2(4) . . . . ? Ir1 N3 C27 C28 5.3(5) . . . . ? C25 C26 C27 N3 -0.4(6) . . . . ? C34 C26 C27 N3 179.0(4) . . . . ? C25 C26 C27 C28 179.6(4) . . . . ? C34 C26 C27 C28 -0.9(6) . . . . ? C29 N4 C28 C32 -1.9(6) . . . . ? Ir1 N4 C28 C32 177.1(3) . . . . ? C29 N4 C28 C27 178.8(4) . . . . ? Ir1 N4 C28 C27 -2.1(5) . . . . ? N3 C27 C28 N4 -2.1(6) . . . . ? C26 C27 C28 N4 177.8(4) . . . . ? N3 C27 C28 C32 178.6(4) . . . . ? C26 C27 C28 C32 -1.4(6) . . . . ? C28 N4 C29 C30 0.4(6) . . . . ? Ir1 N4 C29 C30 -178.5(3) . . . . ? N4 C29 C30 C31 1.2(7) . . . . ? C29 C30 C31 C32 -1.2(7) . . . . ? C30 C31 C32 C28 -0.3(6) . . . . ? C30 C31 C32 C33 177.9(5) . . . . ? N4 C28 C32 C31 1.9(6) . . . . ? C27 C28 C32 C31 -178.9(4) . . . . ? N4 C28 C32 C33 -176.6(4) . . . . ? C27 C28 C32 C33 2.6(6) . . . . ? C35 N6 C33 C34 1.0(5) . . . . ? C42 N6 C33 C34 -178.5(4) . . . . ? C35 N6 C33 C32 -175.8(5) . . . . ? C42 N6 C33 C32 4.7(8) . . . . ? C31 C32 C33 C34 -179.9(5) . . . . ? C28 C32 C33 C34 -1.7(7) . . . . ? C31 C32 C33 N6 -3.6(8) . . . . ? C28 C32 C33 N6 174.6(5) . . . . ? N6 C33 C34 N5 -0.9(5) . . . . ? C32 C33 C34 N5 176.2(4) . . . . ? N6 C33 C34 C26 -177.7(4) . . . . ? C32 C33 C34 C26 -0.6(7) . . . . ? C35 N5 C34 C33 0.5(5) . . . . ? C35 N5 C34 C26 177.0(5) . . . . ? C27 C26 C34 C33 1.9(7) . . . . ? C25 C26 C34 C33 -178.7(4) . . . . ? C27 C26 C34 N5 -174.3(4) . . . . ? C25 C26 C34 N5 5.1(8) . . . . ? C34 N5 C35 N6 0.2(5) . . . . ? C34 N5 C35 C36 -175.0(4) . . . . ? C33 N6 C35 N5 -0.7(5) . . . . ? C42 N6 C35 N5 178.7(4) . . . . ? C33 N6 C35 C36 174.3(5) . . . . ? C42 N6 C35 C36 -6.2(8) . . . . ? N5 C35 C36 C37 26.0(8) . . . . ? N6 C35 C36 C37 -148.6(5) . . . . ? N5 C35 C36 C41 -154.5(5) . . . . ? N6 C35 C36 C41 30.9(8) . . . . ? C41 C36 C37 C38 0.9(9) . . . . ? C35 C36 C37 C38 -179.6(5) . . . . ? C36 C37 C38 C39 -1.2(10) . . . . ? C37 C38 C39 C40 1.2(9) . . . . ? C38 C39 C40 C41 -0.9(9) . . . . ? C39 C40 C41 C36 0.7(8) . . . . ? C37 C36 C41 C40 -0.6(8) . . . . ? C35 C36 C41 C40 179.9(5) . . . . ? C35 N6 C42 C43 89.6(6) . . . . ? C33 N6 C42 C43 -91.1(6) . . . . ? C35 N6 C42 C47 -92.3(6) . . . . ? C33 N6 C42 C47 87.1(6) . . . . ? C47 C42 C43 C44 -0.4(7) . . . . ? N6 C42 C43 C44 177.7(4) . . . . ? C42 C43 C44 C45 0.8(8) . . . . ? C43 C44 C45 C46 -0.1(8) . . . . ? C43 C44 C45 C48 178.1(5) . . . . ? C44 C45 C46 C47 -1.1(8) . . . . ? C48 C45 C46 C47 -179.2(5) . . . . ? C43 C42 C47 C46 -0.7(8) . . . . ? N6 C42 C47 C46 -178.8(4) . . . . ? C45 C46 C47 C42 1.4(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 O1 H1A N5 0.99(2) 1.82(3) 2.797(9) 169(12) . O1 H1B F2 0.98(2) 2.11(6) 3.013(8) 152(10) 8_855 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.442 _refine_diff_density_min -1.121 _refine_diff_density_rms 0.109 _iucr_refine_instructions_details ; TITL NS97 in Pbca CELL 0.71073 10.7181 17.8655 41.9058 90.0000 90.0000 90.0000 ZERR 8.00 0.0013 0.0032 0.0036 0.0000 0.0000 0.0000 LATT 1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O F P IR UNIT 384 280 48 4 48 8 8 REM ---------------------------------------------------------- REM Data collection: Bruker APEX II CCD REM Absorption correction: SADABS REM Crystal habit: prismatic; Crystal colour: yellow REM Mole 1 is the Ir(III) cationic complex REM Mole 2 is the PF6 anion (disordered) REM Mole 3 is 0.5 water molecule REM ---------------------------------------------------------- L.S. 10 ACTA CONF SIZE 0.211 0.181 0.115 BOND $H WPDB -2 FMAP 2 PLAN 10 TEMP -173 EQIV $1 2.5-X, -0.5+Y, Z HTAB O1 N5 HTAB O1 F2_$1 DFIX 0.98 O1 H1A O1 H1B DFIX 1.54 H1A H1B WGHT 0.018600 28.762602 FVAR 0.15074 MOLE 1 IR1 7 0.569282 0.200837 0.329547 11.00000 0.01889 0.03583 = 0.01538 -0.00226 -0.00078 -0.00240 N1 3 0.407502 0.158330 0.347830 11.00000 0.02297 0.03915 = 0.01882 -0.00364 -0.00233 -0.00255 N2 3 0.716355 0.250871 0.306694 11.00000 0.01726 0.03337 = 0.02053 -0.00082 0.00073 -0.00089 N3 3 0.687351 0.109691 0.341903 11.00000 0.01996 0.03816 = 0.01902 -0.00482 0.00104 -0.00672 N4 3 0.629155 0.228526 0.376891 11.00000 0.02048 0.04027 = 0.01637 -0.00033 0.00131 -0.00270 N5 3 0.988089 0.038298 0.425125 11.00000 0.02970 0.05468 = 0.01910 0.00626 0.00371 0.00569 N6 3 0.936481 0.135031 0.456470 11.00000 0.02617 0.05544 = 0.01601 0.00099 -0.00338 0.00233 C1 1 0.394099 0.088616 0.358639 11.00000 0.02818 0.04718 = 0.02202 -0.00796 -0.00185 -0.00484 AFIX 43 H1 2 0.464762 0.056526 0.358987 11.00000 -1.20000 AFIX 0 C2 1 0.281070 0.061496 0.369340 11.00000 0.03669 0.05476 = 0.02689 -0.00278 0.00071 -0.01405 AFIX 43 H2 2 0.273447 0.011310 0.376575 11.00000 -1.20000 AFIX 0 C3 1 0.180283 0.108383 0.369308 11.00000 0.02587 0.07073 = 0.03332 -0.00101 0.00432 -0.01223 AFIX 43 H3 2 0.101555 0.090534 0.376419 11.00000 -1.20000 AFIX 0 C4 1 0.191666 0.179557 0.359296 11.00000 0.02719 0.06240 = 0.03006 -0.00322 0.00228 0.00434 AFIX 43 H4 2 0.121902 0.212318 0.359977 11.00000 -1.20000 AFIX 0 C5 1 0.307623 0.205412 0.347771 11.00000 0.02346 0.05058 = 0.01492 -0.00361 -0.00202 0.00077 C6 1 0.332890 0.279280 0.334415 11.00000 0.03098 0.04409 = 0.01591 -0.00765 -0.00106 0.00310 C7 1 0.243892 0.335986 0.332154 11.00000 0.02863 0.05468 = 0.03294 -0.01193 0.00189 0.01049 AFIX 43 H7 2 0.162476 0.328367 0.340506 11.00000 -1.20000 AFIX 0 C8 1 0.273902 0.403161 0.317803 11.00000 0.04072 0.04570 = 0.03334 -0.01267 -0.00472 0.01157 AFIX 43 H8 2 0.213278 0.441778 0.316234 11.00000 -1.20000 AFIX 0 C9 1 0.391987 0.413947 0.305781 11.00000 0.04070 0.03425 = 0.03583 -0.00430 -0.00781 -0.00172 AFIX 43 H9 2 0.412875 0.460094 0.295865 11.00000 -1.20000 AFIX 0 C10 1 0.481322 0.357208 0.308113 11.00000 0.03148 0.03957 = 0.02508 -0.00715 -0.00353 -0.00567 AFIX 43 H10 2 0.562120 0.365598 0.299507 11.00000 -1.20000 AFIX 0 C11 1 0.455922 0.289121 0.322565 11.00000 0.02289 0.03891 = 0.01781 -0.00806 -0.00421 0.00015 C12 1 0.534645 0.166802 0.284618 11.00000 0.02162 0.03209 = 0.02006 -0.00033 -0.00276 0.00107 C13 1 0.442268 0.118750 0.273683 11.00000 0.02648 0.03483 = 0.02584 -0.00012 0.00181 -0.00110 AFIX 43 H13 2 0.383431 0.099019 0.288404 11.00000 -1.20000 AFIX 0 C14 1 0.433879 0.098825 0.241655 11.00000 0.03221 0.03840 = 0.02651 -0.00347 -0.00926 -0.00390 AFIX 43 H14 2 0.370127 0.065474 0.234881 11.00000 -1.20000 AFIX 0 C15 1 0.518311 0.127395 0.219360 11.00000 0.03778 0.03642 = 0.01498 -0.00695 -0.00511 0.00029 AFIX 43 H15 2 0.511910 0.114054 0.197476 11.00000 -1.20000 AFIX 0 C16 1 0.609819 0.174589 0.229432 11.00000 0.02702 0.04071 = 0.02086 0.00075 0.00059 0.00014 AFIX 43 H16 2 0.667651 0.194227 0.214431 11.00000 -1.20000 AFIX 0 C17 1 0.619843 0.194667 0.261802 11.00000 0.02288 0.03219 = 0.02057 -0.00153 -0.00023 0.00439 C18 1 0.717791 0.243740 0.274455 11.00000 0.02504 0.03569 = 0.01662 0.00034 -0.00429 0.00278 C19 1 0.808648 0.281523 0.256713 11.00000 0.02784 0.03880 = 0.02017 0.00150 0.00441 -0.00057 AFIX 43 H19 2 0.809541 0.277213 0.234119 11.00000 -1.20000 AFIX 0 C20 1 0.896559 0.324816 0.271802 11.00000 0.02722 0.04557 = 0.02831 0.00593 0.00725 0.00030 AFIX 43 H20 2 0.958147 0.350564 0.259748 11.00000 -1.20000 AFIX 0 C21 1 0.894609 0.330545 0.304497 11.00000 0.02020 0.03918 = 0.02937 -0.00750 -0.00200 -0.00262 AFIX 43 H21 2 0.955089 0.359854 0.315383 11.00000 -1.20000 AFIX 0 C22 1 0.803144 0.292922 0.321215 11.00000 0.02091 0.04030 = 0.02184 -0.00443 -0.00164 0.00102 AFIX 43 H22 2 0.801565 0.296937 0.343817 11.00000 -1.20000 AFIX 0 C23 1 0.713697 0.050083 0.323960 11.00000 0.02613 0.04284 = 0.01976 -0.00031 0.00221 -0.01042 AFIX 43 H23 2 0.670909 0.043805 0.304288 11.00000 -1.20000 AFIX 0 C24 1 0.801079 -0.002990 0.332931 11.00000 0.02877 0.03750 = 0.02294 0.00018 0.00724 -0.00059 AFIX 43 H24 2 0.818140 -0.044081 0.319220 11.00000 -1.20000 AFIX 0 C25 1 0.862044 0.003071 0.360873 11.00000 0.02379 0.03450 = 0.02896 0.00409 0.00366 -0.00058 AFIX 43 H25 2 0.922222 -0.033287 0.366936 11.00000 -1.20000 AFIX 0 C26 1 0.835383 0.063960 0.380946 11.00000 0.02383 0.04052 = 0.02006 0.00331 0.00322 -0.00556 C27 1 0.746822 0.116098 0.370588 11.00000 0.01633 0.04239 = 0.02000 0.00040 0.00128 -0.00451 C28 1 0.713424 0.179997 0.389834 11.00000 0.01988 0.03806 = 0.01809 0.00054 0.00157 -0.00564 C29 1 0.593135 0.287711 0.393718 11.00000 0.02163 0.04068 = 0.02317 -0.00247 0.00051 -0.00430 AFIX 43 H29 2 0.534067 0.321179 0.384657 11.00000 -1.20000 AFIX 0 C30 1 0.638865 0.302393 0.424134 11.00000 0.02698 0.04744 = 0.02326 -0.00800 0.00373 -0.00100 AFIX 43 H30 2 0.610033 0.344712 0.435711 11.00000 -1.20000 AFIX 0 C31 1 0.725995 0.255286 0.437314 11.00000 0.02663 0.05267 = 0.01463 -0.00053 0.00037 -0.00842 AFIX 43 H31 2 0.758675 0.265611 0.457922 11.00000 -1.20000 AFIX 0 C32 1 0.766787 0.192324 0.420594 11.00000 0.02233 0.04481 = 0.01554 -0.00133 0.00232 -0.00434 C33 1 0.858715 0.138460 0.429820 11.00000 0.02525 0.05048 = 0.01496 0.00218 -0.00070 -0.00174 C34 1 0.892115 0.078069 0.411317 11.00000 0.02495 0.05050 = 0.02015 0.00595 0.00209 -0.00063 C35 1 1.013168 0.073548 0.452088 11.00000 0.02712 0.05738 = 0.01897 0.00489 0.00174 0.00083 C36 1 1.118369 0.051896 0.473048 11.00000 0.02521 0.05551 = 0.02647 0.00605 -0.00196 0.00260 C37 1 1.218760 0.016270 0.458812 11.00000 0.03630 0.08097 = 0.02591 0.01148 0.00198 0.00947 AFIX 43 H37 2 1.217585 0.007231 0.436474 11.00000 -1.20000 AFIX 0 C38 1 1.321239 -0.006474 0.476708 11.00000 0.03245 0.07932 = 0.04301 0.00623 0.00196 0.01100 AFIX 43 H38 2 1.388705 -0.031668 0.466668 11.00000 -1.20000 AFIX 0 C39 1 1.324765 0.007573 0.508983 11.00000 0.02898 0.06775 = 0.03716 0.00328 -0.00951 -0.00204 AFIX 43 H39 2 1.395257 -0.007025 0.521236 11.00000 -1.20000 AFIX 0 C40 1 1.225954 0.042754 0.523345 11.00000 0.03409 0.05409 = 0.02967 -0.00498 -0.00965 -0.00102 AFIX 43 H40 2 1.227799 0.051795 0.545680 11.00000 -1.20000 AFIX 0 C41 1 1.123960 0.065155 0.505743 11.00000 0.02991 0.04855 = 0.02817 -0.00376 -0.00904 -0.00001 AFIX 43 H41 2 1.056681 0.089938 0.516048 11.00000 -1.20000 AFIX 0 C42 1 0.933386 0.186684 0.483132 11.00000 0.02506 0.05665 = 0.01760 0.00074 -0.00295 0.00594 C43 1 1.006402 0.249325 0.483077 11.00000 0.03518 0.04953 = 0.02979 0.00449 -0.00735 0.00278 AFIX 43 H43 2 1.062387 0.259036 0.465997 11.00000 -1.20000 AFIX 0 C44 1 0.996723 0.298356 0.508577 11.00000 0.04520 0.05406 = 0.04564 -0.00287 -0.01770 0.00579 AFIX 43 H44 2 1.046363 0.342409 0.508604 11.00000 -1.20000 AFIX 0 C45 1 0.917856 0.285469 0.533810 11.00000 0.04462 0.06595 = 0.04160 -0.01001 -0.01524 0.01941 C46 1 0.846729 0.221840 0.533482 11.00000 0.03387 0.09729 = 0.02220 -0.00406 0.00039 0.01724 AFIX 43 H46 2 0.792734 0.211627 0.550925 11.00000 -1.20000 AFIX 0 C47 1 0.852119 0.171638 0.507950 11.00000 0.02694 0.07422 = 0.02830 -0.00077 -0.00261 -0.00093 AFIX 43 H47 2 0.801113 0.128155 0.507646 11.00000 -1.20000 AFIX 0 C48 1 0.910765 0.337487 0.561777 11.00000 0.08447 0.08940 = 0.04567 -0.02907 -0.02492 0.04153 AFIX 33 H48A 2 0.840793 0.322943 0.575494 11.00000 -1.50000 H48B 2 0.898180 0.388812 0.554178 11.00000 -1.50000 H48C 2 0.988681 0.334743 0.573958 11.00000 -1.50000 AFIX 0 MOLE 2 P1 6 0.977717 0.398542 0.400127 11.00000 0.02666 0.04464 = 0.02273 -0.00128 0.00232 0.00210 F1 5 0.949628 0.372268 0.435683 11.00000 0.04333 0.06710 = 0.02549 0.00752 0.00474 0.00069 F2 5 1.123868 0.394863 0.407151 11.00000 0.02571 0.09452 = 0.04898 0.00135 0.00156 -0.00012 F3 5 0.973999 0.483948 0.411234 11.00000 0.06891 0.05109 = 0.03166 -0.00904 0.01164 -0.00231 F4 5 1.007020 0.425373 0.364326 11.00000 0.05703 0.05054 = 0.02238 -0.00257 0.00716 -0.00681 F5 5 0.832683 0.401422 0.392661 11.00000 0.02951 0.07147 = 0.04865 0.01179 -0.00540 0.00161 F6 5 0.981081 0.313515 0.388527 11.00000 0.06141 0.04348 = 0.04509 -0.00122 0.00666 0.00344 MOLE 3 O1 4 1.097314 -0.091196 0.400118 10.50000 0.02726 0.07087 = 0.07047 -0.01496 -0.01676 0.00149 H1A 2 1.058189 -0.048795 0.411576 10.50000 -1.50000 H1B 2 1.180352 -0.093684 0.410011 10.50000 -1.50000 MOLE 0 HKLF 4 REM NS97 in Pbca REM R1 = 0.0441 for 7799 Fo > 4sig(Fo) and 0.0552 for all 9194 data REM 574 parameters refined using 3 restraints END WGHT 0.0186 28.7819 REM Highest difference peak 2.442, deepest hole -1.121, 1-sigma level 0.109 Q1 1 0.5892 0.1519 0.3298 11.00000 0.05 2.44 Q2 1 0.5607 0.2582 0.3292 11.00000 0.05 0.96 Q3 1 0.5960 0.2503 0.3324 11.00000 0.05 0.90 Q4 1 0.4981 0.2287 0.3186 11.00000 0.05 0.68 Q5 1 0.6797 0.2980 0.2831 11.00000 0.05 0.66 Q6 1 0.5707 0.3925 0.3183 11.00000 0.05 0.61 Q7 1 0.8437 0.2016 0.3301 11.00000 0.05 0.61 Q8 1 0.8188 0.2663 0.5700 11.00000 0.05 0.59 Q9 1 0.5455 0.2045 0.3120 11.00000 0.05 0.58 Q10 1 0.5580 0.1930 0.3066 11.00000 0.05 0.55 ;