# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_ns-50 _database_code_depnum_ccdc_archive 'CCDC 914724' #TrackingRef 'total.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H22 F6 Ir N4, F6 P' _chemical_formula_sum 'C36 H22 F12 Ir N4 P' _chemical_formula_weight 961.75 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' 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 10.557(5) _cell_length_b 33.014(10) _cell_length_c 10.957(3) _cell_angle_alpha 90.00 _cell_angle_beta 118.22(2) _cell_angle_gamma 90.00 _cell_volume 3365.0(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 3 _cell_measurement_theta_max 22 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.898 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1864 _exptl_absorpt_coefficient_mu 4.117 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3552 _exptl_absorpt_correction_T_max 0.7454 _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 46698 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 26.54 _reflns_number_total 6509 _reflns_number_gt 5927 _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^)+(0.0316P)^2^+8.5829P] 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 6509 _refine_ls_number_parameters 524 _refine_ls_number_restraints 119 _refine_ls_R_factor_all 0.0323 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0703 _refine_ls_wR_factor_gt 0.0671 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.128 _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 0.538762(15) 0.363829(4) 0.553161(14) 0.01048(6) Uani 1 1 d . . . F1 F 0.0690(3) 0.31392(8) 0.8096(2) 0.0272(6) Uani 1 1 d . . . F2 F 0.1324(3) 0.25517(8) 0.7733(3) 0.0339(6) Uani 1 1 d . . . F3 F -0.0458(2) 0.28609(7) 0.6090(2) 0.0203(5) Uani 1 1 d . . . F4 F 0.8904(3) 0.17848(8) 0.8138(3) 0.0506(9) Uani 1 1 d . . . F5 F 0.6721(3) 0.16099(8) 0.6934(3) 0.0400(7) Uani 1 1 d . . . F6 F 0.8017(4) 0.16880(8) 0.5948(3) 0.0419(7) Uani 1 1 d . . . N1 N 0.6036(3) 0.38614(9) 0.7488(3) 0.0129(6) Uani 1 1 d . . . N2 N 0.4613(3) 0.33621(9) 0.3634(3) 0.0144(7) Uani 1 1 d . . . N3 N 0.6956(3) 0.39409(9) 0.5131(3) 0.0140(7) Uani 1 1 d . . . N4 N 0.4343(3) 0.42015(9) 0.4646(3) 0.0149(7) Uani 1 1 d . . . C1 C 0.7251(4) 0.40709(11) 0.8241(4) 0.0154(8) Uani 1 1 d . . . H1 H 0.7922 0.4098 0.7898 0.019 Uiso 1 1 calc R . . C2 C 0.7568(4) 0.42493(11) 0.9505(4) 0.0169(8) Uani 1 1 d . . . H2 H 0.8437 0.4396 1.0016 0.020 Uiso 1 1 calc R . . C3 C 0.6591(4) 0.42084(11) 0.9994(4) 0.0177(8) Uani 1 1 d . . . H3 H 0.6763 0.4335 1.0837 0.021 Uiso 1 1 calc R . . C4 C 0.5346(4) 0.39805(11) 0.9247(4) 0.0156(8) Uani 1 1 d . . . H4 H 0.4670 0.3948 0.9581 0.019 Uiso 1 1 calc R . . C5 C 0.5105(4) 0.38016(11) 0.8008(4) 0.0125(7) Uani 1 1 d . . . C6 C 0.3886(4) 0.35313(11) 0.7145(4) 0.0124(7) Uani 1 1 d . . . C7 C 0.2912(4) 0.33868(11) 0.7556(4) 0.0140(8) Uani 1 1 d . . . H7 H 0.2960 0.3475 0.8402 0.017 Uiso 1 1 calc R . . C8 C 0.1861(4) 0.31109(11) 0.6715(4) 0.0136(8) Uani 1 1 d . . . C9 C 0.1763(4) 0.29930(11) 0.5449(4) 0.0141(8) Uani 1 1 d . . . H9 H 0.1036 0.2809 0.4869 0.017 Uiso 1 1 calc R . . C10 C 0.2727(4) 0.31451(11) 0.5040(4) 0.0147(8) Uani 1 1 d . . . H10 H 0.2636 0.3067 0.4168 0.018 Uiso 1 1 calc R . . C11 C 0.3834(4) 0.34117(11) 0.5882(4) 0.0126(7) Uani 1 1 d . . . C12 C 0.0861(4) 0.29187(12) 0.7153(4) 0.0165(8) Uani 1 1 d . . . C13 C 0.6347(4) 0.30953(11) 0.6141(4) 0.0124(7) Uani 1 1 d . . . C14 C 0.7272(4) 0.29590(11) 0.7494(4) 0.0140(8) Uani 1 1 d . . . H14 H 0.7578 0.3144 0.8245 0.017 Uiso 1 1 calc R . . C15 C 0.7749(4) 0.25586(12) 0.7756(4) 0.0153(8) Uani 1 1 d . . . H15 H 0.8368 0.2473 0.8678 0.018 Uiso 1 1 calc R . . C16 C 0.7316(4) 0.22841(11) 0.6666(4) 0.0154(8) Uani 1 1 d . . . C17 C 0.6409(4) 0.24068(11) 0.5312(4) 0.0148(8) Uani 1 1 d . . . H17 H 0.6114 0.2220 0.4569 0.018 Uiso 1 1 calc R . . C18 C 0.5939(4) 0.28079(11) 0.5058(4) 0.0127(7) Uani 1 1 d . . . C19 C 0.4991(4) 0.29640(11) 0.3656(4) 0.0130(7) Uani 1 1 d . . . C20 C 0.4451(4) 0.27419(12) 0.2433(4) 0.0159(8) Uani 1 1 d . . . H20 H 0.4714 0.2466 0.2454 0.019 Uiso 1 1 calc R . . C21 C 0.3532(4) 0.29224(12) 0.1189(4) 0.0187(8) Uani 1 1 d . . . H21 H 0.3161 0.2772 0.0350 0.022 Uiso 1 1 calc R . . C22 C 0.3155(4) 0.33275(12) 0.1178(4) 0.0175(8) Uani 1 1 d . . . H22 H 0.2522 0.3459 0.0335 0.021 Uiso 1 1 calc R . . C23 C 0.3719(4) 0.35320(12) 0.2411(4) 0.0157(8) Uani 1 1 d . . . H23 H 0.3464 0.3808 0.2401 0.019 Uiso 1 1 calc R . . C24 C 0.7752(4) 0.18478(12) 0.6924(4) 0.0214(9) Uani 1 1 d . . . C25 C 0.8260(4) 0.38154(12) 0.5417(4) 0.0187(8) Uani 1 1 d . . . H25 H 0.8620 0.3574 0.5944 0.022 Uiso 1 1 calc R . . C26 C 0.9130(5) 0.40234(13) 0.4976(4) 0.0230(9) Uani 1 1 d . . . H26 H 1.0061 0.3925 0.5204 0.028 Uiso 1 1 calc R . . C27 C 0.8621(5) 0.43718(13) 0.4209(4) 0.0244(9) Uani 1 1 d . . . H27 H 0.9195 0.4514 0.3896 0.029 Uiso 1 1 calc R . . C28 C 0.7249(4) 0.45156(12) 0.3890(4) 0.0192(8) Uani 1 1 d . . . C29 C 0.6453(4) 0.42944(11) 0.4392(4) 0.0160(8) Uani 1 1 d . . . C30 C 0.5056(4) 0.44308(11) 0.4118(4) 0.0168(8) Uani 1 1 d . . . C31 C 0.4455(5) 0.47787(11) 0.3313(4) 0.0202(9) Uani 1 1 d . . . C32 C 0.5285(5) 0.49951(13) 0.2802(4) 0.0263(10) Uani 1 1 d . . . H32 H 0.4887 0.5230 0.2253 0.032 Uiso 1 1 calc R . . C33 C 0.6607(5) 0.48751(12) 0.3076(4) 0.0249(9) Uani 1 1 d . . . H33 H 0.7130 0.5029 0.2731 0.030 Uiso 1 1 calc R . . C34 C 0.3051(4) 0.43205(12) 0.4415(4) 0.0192(8) Uani 1 1 d . . . H34 H 0.2564 0.4167 0.4800 0.023 Uiso 1 1 calc R . . C35 C 0.2377(5) 0.46645(13) 0.3623(4) 0.0243(9) Uani 1 1 d . . . H35 H 0.1452 0.4743 0.3483 0.029 Uiso 1 1 calc R . . C36 C 0.3065(5) 0.48868(12) 0.3052(4) 0.0246(9) Uani 1 1 d . . . H36 H 0.2599 0.5113 0.2480 0.029 Uiso 1 1 calc R . . P1 P 1.13465(12) 0.44585(3) 0.88843(12) 0.0242(2) Uani 1 1 d DU . . F8 F 1.1917(3) 0.43485(8) 0.7805(3) 0.0338(6) Uani 1 1 d U A . F12 F 1.0728(4) 0.40037(9) 0.8714(4) 0.0505(8) Uani 1 1 d U A . F7A F 0.9844(6) 0.46006(16) 0.7652(6) 0.0456(14) Uani 0.847(9) 1 d PDU A 1 F9A F 1.2015(6) 0.48928(13) 0.9106(6) 0.0524(14) Uani 0.847(9) 1 d PDU A 1 F10A F 1.2816(4) 0.42837(14) 1.0138(3) 0.0411(12) Uani 0.847(9) 1 d PDU A 1 F11A F 1.0756(7) 0.45476(19) 0.9957(7) 0.0420(14) Uani 0.847(9) 1 d PDU A 1 F7B F 0.9694(16) 0.4459(8) 0.766(3) 0.037(6) Uani 0.153(9) 1 d PDU A 2 F9B F 1.131(3) 0.4946(4) 0.833(3) 0.047(6) Uani 0.153(9) 1 d PDU A 2 F10B F 1.3004(14) 0.4557(9) 0.992(2) 0.066(6) Uani 0.153(9) 1 d PDU A 2 F11B F 1.093(4) 0.4696(9) 0.994(4) 0.036(6) Uani 0.153(9) 1 d PDU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.01474(9) 0.00757(9) 0.00855(9) -0.00010(5) 0.00503(6) -0.00049(5) F1 0.0254(13) 0.0417(16) 0.0198(12) -0.0131(11) 0.0151(11) -0.0139(11) F2 0.0324(14) 0.0270(14) 0.0449(16) 0.0234(12) 0.0204(13) 0.0056(11) F3 0.0144(11) 0.0277(13) 0.0150(11) -0.0025(9) 0.0038(9) -0.0073(9) F4 0.0512(18) 0.0191(14) 0.0351(16) 0.0006(12) -0.0178(14) 0.0100(13) F5 0.0437(17) 0.0143(13) 0.065(2) 0.0029(13) 0.0285(15) -0.0038(12) F6 0.072(2) 0.0211(14) 0.0447(17) 0.0051(12) 0.0377(16) 0.0170(14) N1 0.0210(17) 0.0063(15) 0.0124(15) 0.0004(12) 0.0089(13) 0.0027(12) N2 0.0227(17) 0.0115(16) 0.0113(15) -0.0007(12) 0.0102(14) -0.0043(13) N3 0.0208(17) 0.0102(15) 0.0107(15) -0.0027(12) 0.0072(13) -0.0017(13) N4 0.0207(17) 0.0113(15) 0.0114(15) -0.0014(12) 0.0067(13) -0.0001(13) C1 0.0174(19) 0.0116(18) 0.0154(19) 0.0002(15) 0.0062(16) -0.0008(15) C2 0.020(2) 0.0098(18) 0.0172(19) -0.0016(15) 0.0056(16) -0.0024(15) C3 0.025(2) 0.0122(19) 0.0129(19) -0.0014(15) 0.0062(16) -0.0021(16) C4 0.022(2) 0.0116(18) 0.0129(18) 0.0002(14) 0.0077(16) -0.0003(15) C5 0.0153(18) 0.0082(18) 0.0114(18) 0.0026(14) 0.0042(15) 0.0007(14) C6 0.0125(18) 0.0091(17) 0.0118(18) 0.0009(14) 0.0027(15) 0.0030(14) C7 0.0177(19) 0.0147(19) 0.0096(17) 0.0009(14) 0.0065(15) 0.0007(15) C8 0.0142(18) 0.0124(18) 0.0126(18) 0.0048(14) 0.0049(15) 0.0025(14) C9 0.0129(18) 0.0119(18) 0.0133(18) -0.0007(14) 0.0027(15) -0.0020(14) C10 0.0161(19) 0.0143(19) 0.0106(18) -0.0023(14) 0.0038(15) 0.0002(15) C11 0.0153(18) 0.0075(17) 0.0129(18) 0.0043(14) 0.0049(15) 0.0042(14) C12 0.0174(19) 0.016(2) 0.0129(19) 0.0016(15) 0.0049(16) 0.0009(15) C13 0.0133(18) 0.0129(18) 0.0117(18) -0.0008(14) 0.0064(15) -0.0025(14) C14 0.0157(19) 0.0133(18) 0.0120(18) -0.0029(14) 0.0058(15) -0.0030(15) C15 0.0133(18) 0.0163(19) 0.0130(18) 0.0032(15) 0.0034(15) 0.0014(15) C16 0.0169(19) 0.0114(19) 0.0161(19) 0.0027(15) 0.0064(16) 0.0016(15) C17 0.0158(19) 0.0120(18) 0.0140(19) -0.0015(14) 0.0047(15) -0.0020(15) C18 0.0128(18) 0.0127(18) 0.0114(18) -0.0001(14) 0.0047(15) -0.0018(14) C19 0.0148(18) 0.0117(18) 0.0147(19) -0.0001(14) 0.0087(15) -0.0004(14) C20 0.021(2) 0.0126(19) 0.0141(19) -0.0019(15) 0.0081(16) -0.0011(15) C21 0.021(2) 0.019(2) 0.0129(19) -0.0022(15) 0.0055(16) -0.0026(16) C22 0.021(2) 0.016(2) 0.0135(19) 0.0034(15) 0.0060(16) 0.0020(16) C23 0.020(2) 0.0138(18) 0.0107(18) 0.0007(15) 0.0055(16) 0.0010(16) C24 0.023(2) 0.016(2) 0.018(2) -0.0007(16) 0.0032(17) 0.0022(16) C25 0.021(2) 0.016(2) 0.019(2) -0.0015(16) 0.0089(17) 0.0014(16) C26 0.023(2) 0.024(2) 0.027(2) -0.0017(18) 0.0158(18) -0.0026(17) C27 0.031(2) 0.026(2) 0.022(2) -0.0042(17) 0.0177(19) -0.0101(18) C28 0.029(2) 0.015(2) 0.0151(19) -0.0032(15) 0.0122(17) -0.0054(17) C29 0.025(2) 0.0133(19) 0.0105(18) -0.0022(14) 0.0088(16) -0.0021(16) C30 0.024(2) 0.0117(19) 0.0146(19) -0.0036(15) 0.0090(17) -0.0003(16) C31 0.033(2) 0.0103(19) 0.0144(19) 0.0000(15) 0.0091(18) -0.0001(17) C32 0.042(3) 0.015(2) 0.020(2) 0.0064(17) 0.013(2) 0.0015(19) C33 0.039(3) 0.016(2) 0.022(2) 0.0021(17) 0.017(2) -0.0079(18) C34 0.019(2) 0.017(2) 0.019(2) 0.0002(16) 0.0067(17) 0.0015(16) C35 0.028(2) 0.017(2) 0.026(2) 0.0033(17) 0.0117(19) 0.0055(17) C36 0.032(2) 0.012(2) 0.023(2) 0.0040(16) 0.0074(19) 0.0059(17) P1 0.0233(6) 0.0236(6) 0.0258(6) -0.0051(5) 0.0116(5) 0.0001(5) F8 0.0461(16) 0.0260(14) 0.0402(16) -0.0071(12) 0.0294(14) -0.0041(12) F12 0.055(2) 0.0291(16) 0.074(2) 0.0038(15) 0.0358(18) -0.0059(14) F7A 0.047(3) 0.034(3) 0.039(2) 0.004(2) 0.007(2) 0.022(2) F9A 0.082(4) 0.023(2) 0.071(4) -0.021(2) 0.053(3) -0.024(2) F10A 0.0306(19) 0.055(3) 0.0290(18) -0.0006(17) 0.0064(15) 0.0087(17) F11A 0.038(2) 0.056(4) 0.043(2) -0.013(3) 0.0287(18) -0.007(3) F7B 0.027(8) 0.045(13) 0.053(10) -0.020(10) 0.031(7) -0.015(9) F9B 0.080(15) 0.027(10) 0.079(14) -0.029(10) 0.073(11) -0.022(10) F10B 0.044(9) 0.073(11) 0.059(9) -0.022(9) 0.006(8) 0.018(9) F11B 0.043(11) 0.044(13) 0.035(9) -0.008(10) 0.030(8) -0.004(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 Ir1 C11 1.999(4) . ? Ir1 C13 2.012(4) . ? Ir1 N2 2.053(3) . ? Ir1 N1 2.054(3) . ? Ir1 N4 2.146(3) . ? Ir1 N3 2.149(3) . ? F1 C12 1.345(4) . ? F2 C12 1.348(5) . ? F3 C12 1.342(4) . ? F4 C24 1.327(5) . ? F5 C24 1.346(5) . ? F6 C24 1.336(5) . ? N1 C1 1.343(5) . ? N1 C5 1.363(5) . ? N2 C23 1.344(5) . ? N2 C19 1.371(5) . ? N3 C25 1.325(5) . ? N3 C29 1.375(5) . ? N4 C34 1.324(5) . ? N4 C30 1.373(5) . ? C1 C2 1.392(5) . ? C1 H1 0.9500 . ? C2 C3 1.375(6) . ? C2 H2 0.9500 . ? C3 C4 1.395(5) . ? C3 H3 0.9500 . ? C4 C5 1.390(5) . ? C4 H4 0.9500 . ? C5 C6 1.482(5) . ? C6 C7 1.388(5) . ? C6 C11 1.414(5) . ? C7 C8 1.394(5) . ? C7 H7 0.9500 . ? C8 C9 1.396(5) . ? C8 C12 1.492(5) . ? C9 C10 1.385(5) . ? C9 H9 0.9500 . ? C10 C11 1.404(5) . ? C10 H10 0.9500 . ? C13 C14 1.409(5) . ? C13 C18 1.418(5) . ? C14 C15 1.395(5) . ? C14 H14 0.9500 . ? C15 C16 1.393(5) . ? C15 H15 0.9500 . ? C16 C17 1.392(5) . ? C16 C24 1.498(5) . ? C17 C18 1.395(5) . ? C17 H17 0.9500 . ? C18 C19 1.475(5) . ? C19 C20 1.391(5) . ? C20 C21 1.380(5) . ? C20 H20 0.9500 . ? C21 C22 1.394(6) . ? C21 H21 0.9500 . ? C22 C23 1.369(5) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C25 C26 1.404(6) . ? C25 H25 0.9500 . ? C26 C27 1.375(6) . ? C26 H26 0.9500 . ? C27 C28 1.403(6) . ? C27 H27 0.9500 . ? C28 C29 1.407(5) . ? C28 C33 1.446(6) . ? C29 C30 1.432(6) . ? C30 C31 1.404(5) . ? C31 C36 1.402(6) . ? C31 C32 1.434(6) . ? C32 C33 1.342(7) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.402(6) . ? C34 H34 0.9500 . ? C35 C36 1.374(6) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? P1 F9A 1.565(4) . ? P1 F7A 1.592(4) . ? P1 F11A 1.596(5) . ? P1 F8 1.602(3) . ? P1 F10B 1.606(12) . ? P1 F12 1.612(3) . ? P1 F10A 1.616(3) . ? P1 F11B 1.617(15) . ? P1 F7B 1.623(12) . ? P1 F9B 1.713(13) . ? 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 C13 86.15(14) . . ? C11 Ir1 N2 93.35(14) . . ? C13 Ir1 N2 80.64(14) . . ? C11 Ir1 N1 80.34(14) . . ? C13 Ir1 N1 96.09(13) . . ? N2 Ir1 N1 173.12(12) . . ? C11 Ir1 N4 96.80(13) . . ? C13 Ir1 N4 173.21(13) . . ? N2 Ir1 N4 93.05(12) . . ? N1 Ir1 N4 90.45(12) . . ? C11 Ir1 N3 174.18(13) . . ? C13 Ir1 N3 99.58(13) . . ? N2 Ir1 N3 88.61(12) . . ? N1 Ir1 N3 97.93(12) . . ? N4 Ir1 N3 77.62(12) . . ? C1 N1 C5 119.1(3) . . ? C1 N1 Ir1 125.1(3) . . ? C5 N1 Ir1 115.7(2) . . ? C23 N2 C19 118.6(3) . . ? C23 N2 Ir1 125.5(3) . . ? C19 N2 Ir1 115.8(2) . . ? C25 N3 C29 118.3(3) . . ? C25 N3 Ir1 128.3(3) . . ? C29 N3 Ir1 113.2(2) . . ? C34 N4 C30 118.5(3) . . ? C34 N4 Ir1 127.3(3) . . ? C30 N4 Ir1 113.7(3) . . ? N1 C1 C2 122.6(4) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C3 C2 C1 118.3(4) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C2 C3 C4 119.8(4) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 119.3(4) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N1 C5 C4 120.8(3) . . ? N1 C5 C6 113.6(3) . . ? C4 C5 C6 125.6(3) . . ? C7 C6 C11 122.0(3) . . ? C7 C6 C5 123.6(3) . . ? C11 C6 C5 114.4(3) . . ? C6 C7 C8 119.3(3) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C7 C8 C9 120.1(3) . . ? C7 C8 C12 121.9(3) . . ? C9 C8 C12 118.0(3) . . ? C10 C9 C8 119.9(3) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 121.7(3) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C10 C11 C6 116.9(3) . . ? C10 C11 Ir1 127.7(3) . . ? C6 C11 Ir1 115.3(3) . . ? F3 C12 F1 106.4(3) . . ? F3 C12 F2 106.1(3) . . ? F1 C12 F2 105.9(3) . . ? F3 C12 C8 112.6(3) . . ? F1 C12 C8 113.0(3) . . ? F2 C12 C8 112.4(3) . . ? C14 C13 C18 116.9(3) . . ? C14 C13 Ir1 128.6(3) . . ? C18 C13 Ir1 114.4(3) . . ? C15 C14 C13 121.5(3) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C16 C15 C14 120.0(3) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C17 C16 C15 120.4(3) . . ? C17 C16 C24 118.4(3) . . ? C15 C16 C24 121.1(3) . . ? C16 C17 C18 119.3(3) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C17 C18 C13 122.0(3) . . ? C17 C18 C19 122.8(3) . . ? C13 C18 C19 115.2(3) . . ? N2 C19 C20 120.3(3) . . ? N2 C19 C18 113.7(3) . . ? C20 C19 C18 125.9(3) . . ? C21 C20 C19 120.0(4) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 119.2(4) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? C23 C22 C21 118.4(4) . . ? C23 C22 H22 120.8 . . ? C21 C22 H22 120.8 . . ? N2 C23 C22 123.4(4) . . ? N2 C23 H23 118.3 . . ? C22 C23 H23 118.3 . . ? F4 C24 F6 107.5(4) . . ? F4 C24 F5 105.2(3) . . ? F6 C24 F5 104.6(3) . . ? F4 C24 C16 113.2(3) . . ? F6 C24 C16 113.0(3) . . ? F5 C24 C16 112.7(3) . . ? N3 C25 C26 122.8(4) . . ? N3 C25 H25 118.6 . . ? C26 C25 H25 118.6 . . ? C27 C26 C25 119.3(4) . . ? C27 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? C26 C27 C28 119.6(4) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? C27 C28 C29 117.7(4) . . ? C27 C28 C33 124.0(4) . . ? C29 C28 C33 118.4(4) . . ? N3 C29 C28 122.3(4) . . ? N3 C29 C30 117.6(3) . . ? C28 C29 C30 120.1(4) . . ? N4 C30 C31 122.7(4) . . ? N4 C30 C29 117.0(3) . . ? C31 C30 C29 120.3(4) . . ? C36 C31 C30 117.1(4) . . ? C36 C31 C32 124.6(4) . . ? C30 C31 C32 118.4(4) . . ? C33 C32 C31 121.9(4) . . ? C33 C32 H32 119.0 . . ? C31 C32 H32 119.0 . . ? C32 C33 C28 121.0(4) . . ? C32 C33 H33 119.5 . . ? C28 C33 H33 119.5 . . ? N4 C34 C35 122.3(4) . . ? N4 C34 H34 118.9 . . ? C35 C34 H34 118.9 . . ? C36 C35 C34 119.5(4) . . ? C36 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? C35 C36 C31 119.9(4) . . ? C35 C36 H36 120.0 . . ? C31 C36 H36 120.0 . . ? F9A P1 F7A 93.2(3) . . ? F9A P1 F11A 91.2(3) . . ? F7A P1 F11A 89.5(4) . . ? F9A P1 F8 91.3(2) . . ? F7A P1 F8 90.7(3) . . ? F11A P1 F8 177.4(2) . . ? F9A P1 F10B 56.2(10) . . ? F7A P1 F10B 148.9(11) . . ? F11A P1 F10B 96.6(10) . . ? F8 P1 F10B 84.5(10) . . ? F9A P1 F12 177.3(3) . . ? F7A P1 F12 89.4(2) . . ? F11A P1 F12 88.8(3) . . ? F8 P1 F12 88.66(16) . . ? F10B P1 F12 121.1(11) . . ? F9A P1 F10A 90.8(2) . . ? F7A P1 F10A 175.8(3) . . ? F11A P1 F10A 89.5(3) . . ? F8 P1 F10A 90.10(18) . . ? F12 P1 F10A 86.5(2) . . ? F9A P1 F11B 72.4(11) . . ? F7A P1 F11B 88.0(15) . . ? F8 P1 F11B 163.6(11) . . ? F10B P1 F11B 88.2(17) . . ? F12 P1 F11B 107.7(11) . . ? F10A P1 F11B 92.4(15) . . ? F9A P1 F7B 110.8(9) . . ? F11A P1 F7B 88.2(13) . . ? F8 P1 F7B 91.2(13) . . ? F10B P1 F7B 166.2(13) . . ? F12 P1 F7B 71.8(10) . . ? F10A P1 F7B 158.3(9) . . ? F11B P1 F7B 92(2) . . ? F7A P1 F9B 65.0(8) . . ? F11A P1 F9B 97.8(7) . . ? F8 P1 F9B 84.6(7) . . ? F10B P1 F9B 83.9(8) . . ? F12 P1 F9B 153.4(9) . . ? F10A P1 F9B 119.1(8) . . ? F11B P1 F9B 80.1(13) . . ? F7B P1 F9B 82.6(8) . . ? 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 175.7(3) . . . . ? C13 Ir1 N1 C1 90.6(3) . . . . ? N4 Ir1 N1 C1 -87.5(3) . . . . ? N3 Ir1 N1 C1 -10.0(3) . . . . ? C11 Ir1 N1 C5 -7.2(3) . . . . ? C13 Ir1 N1 C5 -92.3(3) . . . . ? N4 Ir1 N1 C5 89.6(3) . . . . ? N3 Ir1 N1 C5 167.1(2) . . . . ? C11 Ir1 N2 C23 94.3(3) . . . . ? C13 Ir1 N2 C23 179.8(3) . . . . ? N4 Ir1 N2 C23 -2.7(3) . . . . ? N3 Ir1 N2 C23 -80.2(3) . . . . ? C11 Ir1 N2 C19 -81.7(3) . . . . ? C13 Ir1 N2 C19 3.8(3) . . . . ? N4 Ir1 N2 C19 -178.7(3) . . . . ? N3 Ir1 N2 C19 103.7(3) . . . . ? C13 Ir1 N3 C25 -8.8(3) . . . . ? N2 Ir1 N3 C25 -89.1(3) . . . . ? N1 Ir1 N3 C25 88.8(3) . . . . ? N4 Ir1 N3 C25 177.5(3) . . . . ? C13 Ir1 N3 C29 166.1(2) . . . . ? N2 Ir1 N3 C29 85.8(3) . . . . ? N1 Ir1 N3 C29 -96.3(2) . . . . ? N4 Ir1 N3 C29 -7.6(2) . . . . ? C11 Ir1 N4 C34 -1.9(3) . . . . ? N2 Ir1 N4 C34 91.8(3) . . . . ? N1 Ir1 N4 C34 -82.2(3) . . . . ? N3 Ir1 N4 C34 179.7(3) . . . . ? C11 Ir1 N4 C30 -173.2(3) . . . . ? N2 Ir1 N4 C30 -79.4(3) . . . . ? N1 Ir1 N4 C30 106.5(3) . . . . ? N3 Ir1 N4 C30 8.5(2) . . . . ? C5 N1 C1 C2 -3.6(5) . . . . ? Ir1 N1 C1 C2 173.5(3) . . . . ? N1 C1 C2 C3 -0.1(6) . . . . ? C1 C2 C3 C4 2.2(6) . . . . ? C2 C3 C4 C5 -0.7(6) . . . . ? C1 N1 C5 C4 5.0(5) . . . . ? Ir1 N1 C5 C4 -172.2(3) . . . . ? C1 N1 C5 C6 -174.0(3) . . . . ? Ir1 N1 C5 C6 8.7(4) . . . . ? C3 C4 C5 N1 -3.0(5) . . . . ? C3 C4 C5 C6 176.0(3) . . . . ? N1 C5 C6 C7 171.5(3) . . . . ? C4 C5 C6 C7 -7.5(6) . . . . ? N1 C5 C6 C11 -5.2(5) . . . . ? C4 C5 C6 C11 175.8(3) . . . . ? C11 C6 C7 C8 1.0(5) . . . . ? C5 C6 C7 C8 -175.4(3) . . . . ? C6 C7 C8 C9 -2.3(5) . . . . ? C6 C7 C8 C12 174.9(3) . . . . ? C7 C8 C9 C10 1.1(5) . . . . ? C12 C8 C9 C10 -176.1(3) . . . . ? C8 C9 C10 C11 1.3(6) . . . . ? C9 C10 C11 C6 -2.5(5) . . . . ? C9 C10 C11 Ir1 176.2(3) . . . . ? C7 C6 C11 C10 1.3(5) . . . . ? C5 C6 C11 C10 178.1(3) . . . . ? C7 C6 C11 Ir1 -177.6(3) . . . . ? C5 C6 C11 Ir1 -0.8(4) . . . . ? C13 Ir1 C11 C10 -77.8(3) . . . . ? N2 Ir1 C11 C10 2.6(3) . . . . ? N1 Ir1 C11 C10 -174.6(3) . . . . ? N4 Ir1 C11 C10 96.1(3) . . . . ? C13 Ir1 C11 C6 101.0(3) . . . . ? N2 Ir1 C11 C6 -178.6(3) . . . . ? N1 Ir1 C11 C6 4.2(3) . . . . ? N4 Ir1 C11 C6 -85.1(3) . . . . ? C7 C8 C12 F3 144.6(3) . . . . ? C9 C8 C12 F3 -38.2(5) . . . . ? C7 C8 C12 F1 24.1(5) . . . . ? C9 C8 C12 F1 -158.7(3) . . . . ? C7 C8 C12 F2 -95.6(4) . . . . ? C9 C8 C12 F2 81.5(4) . . . . ? C11 Ir1 C13 C14 -85.8(3) . . . . ? N2 Ir1 C13 C14 -179.9(4) . . . . ? N1 Ir1 C13 C14 -6.0(3) . . . . ? N3 Ir1 C13 C14 93.1(3) . . . . ? C11 Ir1 C13 C18 89.1(3) . . . . ? N2 Ir1 C13 C18 -4.9(3) . . . . ? N1 Ir1 C13 C18 169.0(3) . . . . ? N3 Ir1 C13 C18 -91.9(3) . . . . ? C18 C13 C14 C15 -0.8(5) . . . . ? Ir1 C13 C14 C15 174.1(3) . . . . ? C13 C14 C15 C16 0.4(6) . . . . ? C14 C15 C16 C17 0.1(6) . . . . ? C14 C15 C16 C24 -177.0(4) . . . . ? C15 C16 C17 C18 0.0(6) . . . . ? C24 C16 C17 C18 177.1(4) . . . . ? C16 C17 C18 C13 -0.5(6) . . . . ? C16 C17 C18 C19 179.4(3) . . . . ? C14 C13 C18 C17 0.9(5) . . . . ? Ir1 C13 C18 C17 -174.7(3) . . . . ? C14 C13 C18 C19 -179.0(3) . . . . ? Ir1 C13 C18 C19 5.4(4) . . . . ? C23 N2 C19 C20 -0.3(5) . . . . ? Ir1 N2 C19 C20 176.0(3) . . . . ? C23 N2 C19 C18 -178.2(3) . . . . ? Ir1 N2 C19 C18 -1.9(4) . . . . ? C17 C18 C19 N2 177.8(3) . . . . ? C13 C18 C19 N2 -2.3(5) . . . . ? C17 C18 C19 C20 0.0(6) . . . . ? C13 C18 C19 C20 179.9(4) . . . . ? N2 C19 C20 C21 0.2(6) . . . . ? C18 C19 C20 C21 177.9(4) . . . . ? C19 C20 C21 C22 -0.1(6) . . . . ? C20 C21 C22 C23 0.2(6) . . . . ? C19 N2 C23 C22 0.3(6) . . . . ? Ir1 N2 C23 C22 -175.6(3) . . . . ? C21 C22 C23 N2 -0.3(6) . . . . ? C17 C16 C24 F4 161.9(4) . . . . ? C15 C16 C24 F4 -21.1(6) . . . . ? C17 C16 C24 F6 39.4(5) . . . . ? C15 C16 C24 F6 -143.5(4) . . . . ? C17 C16 C24 F5 -78.9(5) . . . . ? C15 C16 C24 F5 98.2(4) . . . . ? C29 N3 C25 C26 -1.3(6) . . . . ? Ir1 N3 C25 C26 173.4(3) . . . . ? N3 C25 C26 C27 -0.2(6) . . . . ? C25 C26 C27 C28 0.6(6) . . . . ? C26 C27 C28 C29 0.6(6) . . . . ? C26 C27 C28 C33 -179.1(4) . . . . ? C25 N3 C29 C28 2.6(5) . . . . ? Ir1 N3 C29 C28 -172.9(3) . . . . ? C25 N3 C29 C30 -178.6(3) . . . . ? Ir1 N3 C29 C30 5.9(4) . . . . ? C27 C28 C29 N3 -2.3(6) . . . . ? C33 C28 C29 N3 177.5(3) . . . . ? C27 C28 C29 C30 179.0(4) . . . . ? C33 C28 C29 C30 -1.2(5) . . . . ? C34 N4 C30 C31 -1.9(5) . . . . ? Ir1 N4 C30 C31 170.2(3) . . . . ? C34 N4 C30 C29 179.7(3) . . . . ? Ir1 N4 C30 C29 -8.2(4) . . . . ? N3 C29 C30 N4 1.5(5) . . . . ? C28 C29 C30 N4 -179.7(3) . . . . ? N3 C29 C30 C31 -176.9(3) . . . . ? C28 C29 C30 C31 1.9(5) . . . . ? N4 C30 C31 C36 -0.3(6) . . . . ? C29 C30 C31 C36 178.0(4) . . . . ? N4 C30 C31 C32 -179.5(4) . . . . ? C29 C30 C31 C32 -1.2(6) . . . . ? C36 C31 C32 C33 -179.4(4) . . . . ? C30 C31 C32 C33 -0.2(6) . . . . ? C31 C32 C33 C28 0.9(6) . . . . ? C27 C28 C33 C32 179.6(4) . . . . ? C29 C28 C33 C32 -0.2(6) . . . . ? C30 N4 C34 C35 1.8(6) . . . . ? Ir1 N4 C34 C35 -169.1(3) . . . . ? N4 C34 C35 C36 0.5(6) . . . . ? C34 C35 C36 C31 -2.8(6) . . . . ? C30 C31 C36 C35 2.6(6) . . . . ? C32 C31 C36 C35 -178.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.876 _refine_diff_density_min -1.411 _refine_diff_density_rms 0.125 _iucr_refine_instructions_details ; TITL NS-50 in P2(1)/c CELL 0.71073 10.5567 33.0144 10.9574 90.0000 118.2188 90.0000 ZERR 4.00 0.0045 0.0098 0.0026 0.0000 0.0217 0.0000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N F P IR UNIT 144 88 16 48 4 4 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 ---------------------------------------------------------- L.S. 10 ACTA 50 FMAP 2 PLAN 10 TEMP -173 CONF WPDB -2 SIZE 0.492 0.416 0.182 BOND $H SADI F7A F9A F9A F10A F7B F9B F9B F10B SADI F7A F10A F7B F10B SADI P1 F7A P1 F9A P1 F10A P1 F11A P1 F7B P1 F9B P1 F10B P1 F11B SIMU 0.01 P1 > F11B WGHT 0.031600 8.582900 FVAR 0.23443 0.84684 MOLE 1 IR1 6 0.538762 0.363829 0.553161 11.00000 0.01474 0.00757 = 0.00855 -0.00010 0.00503 -0.00049 F1 4 0.068968 0.313924 0.809605 11.00000 0.02540 0.04175 = 0.01979 -0.01313 0.01512 -0.01395 F2 4 0.132394 0.255172 0.773329 11.00000 0.03243 0.02698 = 0.04491 0.02339 0.02042 0.00564 F3 4 -0.045848 0.286087 0.608974 11.00000 0.01440 0.02771 = 0.01505 -0.00248 0.00381 -0.00726 F4 4 0.890438 0.178479 0.813758 11.00000 0.05118 0.01906 = 0.03511 0.00065 -0.01779 0.01004 F5 4 0.672071 0.160989 0.693366 11.00000 0.04372 0.01432 = 0.06529 0.00292 0.02854 -0.00378 F6 4 0.801726 0.168797 0.594767 11.00000 0.07220 0.02109 = 0.04473 0.00508 0.03765 0.01703 N1 3 0.603583 0.386138 0.748819 11.00000 0.02096 0.00634 = 0.01244 0.00039 0.00885 0.00273 N2 3 0.461293 0.336215 0.363389 11.00000 0.02275 0.01151 = 0.01135 -0.00069 0.01015 -0.00425 N3 3 0.695587 0.394091 0.513062 11.00000 0.02084 0.01019 = 0.01074 -0.00266 0.00723 -0.00171 N4 3 0.434280 0.420149 0.464552 11.00000 0.02074 0.01131 = 0.01144 -0.00141 0.00671 -0.00012 C1 1 0.725149 0.407089 0.824124 11.00000 0.01742 0.01156 = 0.01539 0.00015 0.00617 -0.00083 AFIX 43 H1 2 0.792192 0.409839 0.789789 11.00000 -1.20000 AFIX 0 C2 1 0.756783 0.424934 0.950493 11.00000 0.01979 0.00981 = 0.01718 -0.00158 0.00562 -0.00236 AFIX 43 H2 2 0.843652 0.439569 1.001649 11.00000 -1.20000 AFIX 0 C3 1 0.659082 0.420837 0.999381 11.00000 0.02472 0.01218 = 0.01289 -0.00140 0.00619 -0.00211 AFIX 43 H3 2 0.676320 0.433481 1.083729 11.00000 -1.20000 AFIX 0 C4 1 0.534574 0.398049 0.924669 11.00000 0.02185 0.01158 = 0.01290 0.00020 0.00774 -0.00033 AFIX 43 H4 2 0.466989 0.394800 0.958139 11.00000 -1.20000 AFIX 0 C5 1 0.510512 0.380157 0.800755 11.00000 0.01532 0.00817 = 0.01136 0.00263 0.00416 0.00074 C6 1 0.388586 0.353126 0.714475 11.00000 0.01248 0.00911 = 0.01182 0.00091 0.00270 0.00295 C7 1 0.291165 0.338685 0.755563 11.00000 0.01767 0.01470 = 0.00955 0.00088 0.00647 0.00072 AFIX 43 H7 2 0.296013 0.347521 0.840179 11.00000 -1.20000 AFIX 0 C8 1 0.186130 0.311086 0.671455 11.00000 0.01416 0.01235 = 0.01257 0.00485 0.00494 0.00254 C9 1 0.176279 0.299297 0.544935 11.00000 0.01289 0.01186 = 0.01326 -0.00066 0.00274 -0.00203 AFIX 43 H9 2 0.103555 0.280861 0.486912 11.00000 -1.20000 AFIX 0 C10 1 0.272669 0.314509 0.504042 11.00000 0.01606 0.01434 = 0.01060 -0.00225 0.00377 0.00018 AFIX 43 H10 2 0.263641 0.306706 0.416831 11.00000 -1.20000 AFIX 0 C11 1 0.383380 0.341172 0.588243 11.00000 0.01532 0.00747 = 0.01293 0.00428 0.00492 0.00419 C12 1 0.086143 0.291873 0.715255 11.00000 0.01742 0.01644 = 0.01291 0.00162 0.00488 0.00086 C13 1 0.634720 0.309528 0.614110 11.00000 0.01328 0.01287 = 0.01169 -0.00077 0.00636 -0.00247 C14 1 0.727213 0.295904 0.749387 11.00000 0.01569 0.01334 = 0.01203 -0.00286 0.00580 -0.00302 AFIX 43 H14 2 0.757843 0.314397 0.824462 11.00000 -1.20000 AFIX 0 C15 1 0.774850 0.255863 0.775593 11.00000 0.01326 0.01626 = 0.01297 0.00318 0.00340 0.00138 AFIX 43 H15 2 0.836779 0.247318 0.867757 11.00000 -1.20000 AFIX 0 C16 1 0.731583 0.228412 0.666574 11.00000 0.01687 0.01141 = 0.01612 0.00270 0.00638 0.00160 C17 1 0.640929 0.240683 0.531168 11.00000 0.01576 0.01195 = 0.01401 -0.00154 0.00474 -0.00197 AFIX 43 H17 2 0.611402 0.221954 0.456857 11.00000 -1.20000 AFIX 0 C18 1 0.593948 0.280785 0.505846 11.00000 0.01280 0.01267 = 0.01136 -0.00007 0.00472 -0.00182 C19 1 0.499113 0.296397 0.365592 11.00000 0.01482 0.01169 = 0.01473 -0.00013 0.00872 -0.00043 C20 1 0.445060 0.274186 0.243285 11.00000 0.02092 0.01260 = 0.01410 -0.00189 0.00812 -0.00112 AFIX 43 H20 2 0.471424 0.246579 0.245440 11.00000 -1.20000 AFIX 0 C21 1 0.353203 0.292235 0.118892 11.00000 0.02132 0.01880 = 0.01288 -0.00221 0.00554 -0.00260 AFIX 43 H21 2 0.316126 0.277239 0.035033 11.00000 -1.20000 AFIX 0 C22 1 0.315461 0.332752 0.117772 11.00000 0.02068 0.01579 = 0.01348 0.00339 0.00601 0.00199 AFIX 43 H22 2 0.252157 0.345853 0.033521 11.00000 -1.20000 AFIX 0 C23 1 0.371851 0.353201 0.241054 11.00000 0.02041 0.01377 = 0.01066 0.00074 0.00550 0.00103 AFIX 43 H23 2 0.346419 0.380848 0.240065 11.00000 -1.20000 AFIX 0 C24 1 0.775175 0.184776 0.692393 11.00000 0.02293 0.01573 = 0.01775 -0.00071 0.00318 0.00219 C25 1 0.825965 0.381536 0.541726 11.00000 0.02080 0.01624 = 0.01866 -0.00149 0.00893 0.00145 AFIX 43 H25 2 0.862042 0.357448 0.594370 11.00000 -1.20000 AFIX 0 C26 1 0.913006 0.402339 0.497565 11.00000 0.02298 0.02403 = 0.02703 -0.00169 0.01585 -0.00259 AFIX 43 H26 2 1.006112 0.392451 0.520439 11.00000 -1.20000 AFIX 0 C27 1 0.862108 0.437179 0.420850 11.00000 0.03098 0.02622 = 0.02213 -0.00415 0.01767 -0.01014 AFIX 43 H27 2 0.919549 0.451424 0.389600 11.00000 -1.20000 AFIX 0 C28 1 0.724875 0.451563 0.389005 11.00000 0.02933 0.01520 = 0.01511 -0.00318 0.01217 -0.00535 C29 1 0.645318 0.429440 0.439248 11.00000 0.02469 0.01329 = 0.01053 -0.00224 0.00876 -0.00207 C30 1 0.505581 0.443077 0.411838 11.00000 0.02403 0.01168 = 0.01462 -0.00359 0.00903 -0.00034 C31 1 0.445464 0.477873 0.331321 11.00000 0.03313 0.01033 = 0.01440 0.00004 0.00910 -0.00011 C32 1 0.528484 0.499514 0.280208 11.00000 0.04180 0.01536 = 0.02007 0.00639 0.01319 0.00150 AFIX 43 H32 2 0.488664 0.523038 0.225318 11.00000 -1.20000 AFIX 0 C33 1 0.660736 0.487513 0.307636 11.00000 0.03914 0.01617 = 0.02212 0.00214 0.01677 -0.00788 AFIX 43 H33 2 0.713034 0.502861 0.273089 11.00000 -1.20000 AFIX 0 C34 1 0.305110 0.432052 0.441503 11.00000 0.01931 0.01659 = 0.01889 0.00015 0.00674 0.00148 AFIX 43 H34 2 0.256386 0.416748 0.479968 11.00000 -1.20000 AFIX 0 C35 1 0.237693 0.466450 0.362316 11.00000 0.02821 0.01695 = 0.02615 0.00328 0.01166 0.00554 AFIX 43 H35 2 0.145212 0.474328 0.348285 11.00000 -1.20000 AFIX 0 C36 1 0.306470 0.488679 0.305156 11.00000 0.03182 0.01227 = 0.02290 0.00401 0.00742 0.00586 AFIX 43 H36 2 0.259884 0.511337 0.247988 11.00000 -1.20000 AFIX 0 MOLE 2 P1 5 1.134647 0.445851 0.888433 11.00000 0.02332 0.02362 = 0.02580 -0.00505 0.01164 0.00006 F8 4 1.191711 0.434851 0.780499 11.00000 0.04614 0.02604 = 0.04024 -0.00709 0.02943 -0.00406 F12 4 1.072812 0.400374 0.871424 11.00000 0.05485 0.02912 = 0.07398 0.00378 0.03580 -0.00590 PART 1 F7A 4 0.984422 0.460065 0.765159 21.00000 0.04701 0.03387 = 0.03939 0.00399 0.00695 0.02234 F9A 4 1.201452 0.489276 0.910589 21.00000 0.08228 0.02336 = 0.07146 -0.02141 0.05263 -0.02384 F10A 4 1.281629 0.428366 1.013839 21.00000 0.03057 0.05450 = 0.02902 -0.00062 0.00643 0.00869 F11A 4 1.075613 0.454762 0.995674 21.00000 0.03837 0.05632 = 0.04299 -0.01326 0.02873 -0.00740 PART 2 F7B 4 0.969350 0.445950 0.765791 -21.00000 0.02740 0.04453 = 0.05309 -0.01986 0.03082 -0.01523 F9B 4 1.131326 0.494596 0.833368 -21.00000 0.08023 0.02652 = 0.07886 -0.02905 0.07343 -0.02236 F10B 4 1.300358 0.455712 0.992225 -21.00000 0.04410 0.07291 = 0.05868 -0.02183 0.00605 0.01754 F11B 4 1.093225 0.469644 0.993615 -21.00000 0.04287 0.04376 = 0.03525 -0.00821 0.03039 -0.00375 PART 0 MOLE 0 HKLF 4 1 1 0 0 0 0 -1 0 1 0 REM NS-50 in P2(1)/c REM R1 = 0.0277 for 5927 Fo > 4sig(Fo) and 0.0323 for all 6509 data REM 524 parameters refined using 119 restraints END WGHT 0.0316 8.5827 REM Highest difference peak 1.876, deepest hole -1.411, 1-sigma level 0.125 Q1 1 0.6603 0.3625 0.5957 11.00000 0.05 1.88 Q2 1 0.4308 0.3639 0.5230 11.00000 0.05 1.85 Q3 1 0.0645 0.3888 0.1996 11.00000 0.05 1.05 Q4 1 0.0424 0.1955 0.5977 11.00000 0.05 0.96 Q5 1 0.6458 0.3642 0.6967 11.00000 0.05 0.86 Q6 1 1.1810 0.4091 0.9467 11.00000 0.05 0.74 Q7 1 1.0391 0.4814 0.7607 11.00000 0.05 0.71 Q8 1 1.3110 0.4774 0.9667 11.00000 0.05 0.67 Q9 1 0.7947 0.1749 0.8290 11.00000 0.05 0.67 Q10 1 0.9054 0.1809 0.6993 11.00000 0.05 0.66 ; data_ns-51 _database_code_depnum_ccdc_archive 'CCDC 914725' #TrackingRef 'total.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H26 F6 Ir N4, F6 P' _chemical_formula_sum 'C38 H26 F12 Ir N4 P' _chemical_formula_weight 989.80 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' 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 'F d d 2' _symmetry_space_group_name_Hall 'F 2 -2d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 19.198(3) _cell_length_b 68.958(10) _cell_length_c 11.0075(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 14572(4) _cell_formula_units_Z 16 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 159 _cell_measurement_theta_min 3 _cell_measurement_theta_max 22 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.805 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7712 _exptl_absorpt_coefficient_mu 3.806 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4778 _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 62389 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -89 _diffrn_reflns_limit_k_max 89 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8011 _reflns_number_gt 7780 _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^)+(0.0056P)^2^+38.3473P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.021(4) _refine_ls_number_reflns 8011 _refine_ls_number_parameters 506 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0181 _refine_ls_R_factor_gt 0.0168 _refine_ls_wR_factor_ref 0.0364 _refine_ls_wR_factor_gt 0.0359 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.124 _refine_ls_shift/su_max 0.005 _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 0.466792(5) 0.428608(1) 0.539773(17) 0.01188(3) Uani 1 1 d . . . F1 F 0.34212(9) 0.40615(3) 1.11687(16) 0.0293(4) Uani 1 1 d . . . F2 F 0.44360(8) 0.39326(3) 1.13313(15) 0.0224(4) Uani 1 1 d . . . F3 F 0.36106(9) 0.37784(2) 1.0437(2) 0.0351(4) Uani 1 1 d . . . F4 F 0.33887(9) 0.34073(2) 0.3070(2) 0.0440(6) Uani 1 1 d . . . F5 F 0.39557(11) 0.33191(2) 0.46522(19) 0.0371(5) Uani 1 1 d . . . F6 F 0.44963(10) 0.33595(2) 0.2959(2) 0.0364(4) Uani 1 1 d . . . N1 N 0.36858(11) 0.43938(3) 0.5709(2) 0.0146(5) Uani 1 1 d . . . N2 N 0.56244(11) 0.41579(3) 0.52064(19) 0.0130(5) Uani 1 1 d . . . N3 N 0.48484(12) 0.44285(3) 0.3699(2) 0.0148(5) Uani 1 1 d . . . N4 N 0.51038(12) 0.45581(3) 0.5938(2) 0.0153(5) Uani 1 1 d . . . C1 C 0.33089(15) 0.44965(4) 0.4908(3) 0.0178(6) Uani 1 1 d . . . H1 H 0.3479 0.4511 0.4103 0.021 Uiso 1 1 calc R . . C2 C 0.26791(14) 0.45830(4) 0.5214(3) 0.0209(6) Uani 1 1 d . . . H2 H 0.2415 0.4651 0.4623 0.025 Uiso 1 1 calc R . . C3 C 0.24461(15) 0.45673(4) 0.6402(3) 0.0214(6) Uani 1 1 d . . . H3 H 0.2033 0.4632 0.6649 0.026 Uiso 1 1 calc R . . C4 C 0.28191(15) 0.44570(4) 0.7226(3) 0.0199(6) Uani 1 1 d . . . H4 H 0.2656 0.4443 0.8036 0.024 Uiso 1 1 calc R . . C5 C 0.34362(14) 0.43667(4) 0.6865(3) 0.0155(6) Uani 1 1 d . . . C6 C 0.38709(13) 0.42382(4) 0.7612(2) 0.0138(6) Uani 1 1 d . . . C7 C 0.36772(14) 0.41709(4) 0.8769(3) 0.0160(6) Uani 1 1 d . . . H7 H 0.3254 0.4213 0.9130 0.019 Uiso 1 1 calc R . . C8 C 0.41086(15) 0.40424(4) 0.9376(2) 0.0152(6) Uani 1 1 d . . . C9 C 0.47346(14) 0.39822(4) 0.8858(3) 0.0151(5) Uani 1 1 d . . . H9 H 0.5027 0.3894 0.9280 0.018 Uiso 1 1 calc R . . C10 C 0.49311(13) 0.40514(3) 0.7723(3) 0.0159(6) Uani 1 1 d . . . H10 H 0.5364 0.4012 0.7386 0.019 Uiso 1 1 calc R . . C11 C 0.45036(14) 0.41783(4) 0.7068(2) 0.0134(5) Uani 1 1 d . . . C12 C 0.38963(13) 0.39565(4) 1.0570(3) 0.0181(6) Uani 1 1 d . . . C13 C 0.43652(14) 0.40269(4) 0.4750(2) 0.0128(5) Uani 1 1 d . . . C14 C 0.36916(14) 0.39607(4) 0.4484(2) 0.0158(6) Uani 1 1 d . . . H14 H 0.3310 0.4048 0.4562 0.019 Uiso 1 1 calc R . . C15 C 0.35668(15) 0.37715(4) 0.4109(3) 0.0180(6) Uani 1 1 d . . . H15 H 0.3105 0.3730 0.3938 0.022 Uiso 1 1 calc R . . C16 C 0.41171(15) 0.36425(4) 0.3983(3) 0.0163(6) Uani 1 1 d . . . C17 C 0.47954(14) 0.37033(4) 0.4214(3) 0.0160(6) Uani 1 1 d . . . H17 H 0.5173 0.3615 0.4119 0.019 Uiso 1 1 calc R . . C18 C 0.49191(14) 0.38928(4) 0.4583(2) 0.0140(5) Uani 1 1 d . . . C19 C 0.56196(14) 0.39694(4) 0.4826(2) 0.0135(5) Uani 1 1 d . . . C20 C 0.62416(14) 0.38667(4) 0.4697(3) 0.0165(6) Uani 1 1 d . . . H20 H 0.6236 0.3736 0.4431 0.020 Uiso 1 1 calc R . . C21 C 0.68668(15) 0.39577(4) 0.4960(3) 0.0207(6) Uani 1 1 d . . . H21 H 0.7294 0.3889 0.4875 0.025 Uiso 1 1 calc R . . C22 C 0.68673(14) 0.41479(4) 0.5347(3) 0.0192(6) Uani 1 1 d . . . H22 H 0.7292 0.4212 0.5531 0.023 Uiso 1 1 calc R . . C23 C 0.62393(13) 0.42421(3) 0.5459(3) 0.0181(5) Uani 1 1 d . . . H23 H 0.6240 0.4373 0.5728 0.022 Uiso 1 1 calc R . . C24 C 0.39920(16) 0.34351(4) 0.3665(3) 0.0237(7) Uani 1 1 d . . . C25 C 0.46996(15) 0.43618(4) 0.2596(3) 0.0203(6) Uani 1 1 d . . . H25 H 0.4449 0.4244 0.2525 0.024 Uiso 1 1 calc R . . C26 C 0.48970(17) 0.44582(5) 0.1542(3) 0.0252(7) Uani 1 1 d . . . H26 H 0.4773 0.4406 0.0772 0.030 Uiso 1 1 calc R . . C27 C 0.52700(17) 0.46282(5) 0.1605(3) 0.0231(7) Uani 1 1 d . . . C28 C 0.54332(14) 0.47040(4) 0.2773(3) 0.0197(6) Uani 1 1 d . . . C29 C 0.52060(15) 0.45989(4) 0.3789(3) 0.0155(6) Uani 1 1 d . . . C30 C 0.53436(14) 0.46689(4) 0.4996(2) 0.0147(5) Uani 1 1 d . . . C31 C 0.57294(14) 0.48413(4) 0.5174(2) 0.0165(6) Uani 1 1 d . . . C32 C 0.59622(16) 0.49423(4) 0.4117(3) 0.0201(6) Uani 1 1 d . . . H32 H 0.6222 0.5058 0.4215 0.024 Uiso 1 1 calc R . . C33 C 0.58252(14) 0.48784(4) 0.2980(3) 0.0227(6) Uani 1 1 d . . . H33 H 0.5992 0.4950 0.2304 0.027 Uiso 1 1 calc R . . C34 C 0.58625(16) 0.49007(4) 0.6379(3) 0.0202(6) Uani 1 1 d . . . C35 C 0.55955(17) 0.47891(4) 0.7311(3) 0.0231(6) Uani 1 1 d . . . H35 H 0.5666 0.4828 0.8130 0.028 Uiso 1 1 calc R . . C36 C 0.52234(17) 0.46196(5) 0.7064(3) 0.0202(7) Uani 1 1 d . . . H36 H 0.5049 0.4546 0.7725 0.024 Uiso 1 1 calc R . . C37 C 0.54848(18) 0.47305(5) 0.0456(4) 0.0357(8) Uani 1 1 d . . . H37A H 0.5448 0.4641 -0.0232 0.054 Uiso 1 1 calc R . . H37B H 0.5967 0.4775 0.0533 0.054 Uiso 1 1 calc R . . H37C H 0.5179 0.4842 0.0319 0.054 Uiso 1 1 calc R . . C38 C 0.62873(17) 0.50779(4) 0.6655(3) 0.0273(7) Uani 1 1 d . . . H38A H 0.6298 0.5099 0.7536 0.041 Uiso 1 1 calc R . . H38B H 0.6078 0.5191 0.6257 0.041 Uiso 1 1 calc R . . H38C H 0.6763 0.5060 0.6354 0.041 Uiso 1 1 calc R . . P1 P 0.80319(5) 0.470892(15) 0.59292(10) 0.0419(3) Uani 1 1 d . . . F7 F 0.81355(15) 0.44837(4) 0.5877(5) 0.1266(19) Uani 1 1 d . . . F8 F 0.87131(17) 0.47333(7) 0.5136(3) 0.1248(16) Uani 1 1 d . . . F9 F 0.85110(14) 0.47150(3) 0.7099(2) 0.0602(7) Uani 1 1 d . . . F10 F 0.79483(13) 0.49375(3) 0.5938(3) 0.0637(7) Uani 1 1 d . . . F11 F 0.73705(16) 0.46908(5) 0.6738(4) 0.1210(16) Uani 1 1 d . . . F12 F 0.7553(2) 0.47010(7) 0.4779(4) 0.170(3) 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 0.01130(4) 0.00981(4) 0.01451(4) 0.00085(4) 0.00063(4) -0.00015(4) F1 0.0211(9) 0.0463(11) 0.0206(9) 0.0083(8) 0.0085(7) 0.0118(8) F2 0.0162(9) 0.0323(10) 0.0187(9) 0.0042(7) -0.0023(7) 0.0009(7) F3 0.0487(11) 0.0294(9) 0.0270(9) 0.0041(10) 0.0014(11) -0.0236(8) F4 0.0322(10) 0.0209(8) 0.0791(17) -0.0121(11) -0.0306(12) 0.0016(7) F5 0.0511(13) 0.0163(9) 0.0440(12) 0.0056(8) 0.0001(10) -0.0042(8) F6 0.0352(10) 0.0200(8) 0.0540(12) -0.0144(11) 0.0093(12) -0.0015(7) N1 0.0136(11) 0.0110(10) 0.0192(13) -0.0022(8) -0.0008(9) -0.0016(8) N2 0.0123(10) 0.0157(10) 0.0109(12) 0.0021(9) 0.0012(9) -0.0007(8) N3 0.0154(12) 0.0126(11) 0.0165(12) -0.0003(9) 0.0007(10) 0.0007(9) N4 0.0149(11) 0.0136(11) 0.0175(11) 0.0026(9) 0.0011(10) 0.0006(9) C1 0.0149(14) 0.0156(13) 0.0229(14) 0.0004(11) -0.0043(12) -0.0006(11) C2 0.0185(13) 0.0155(12) 0.0288(18) 0.0000(12) -0.0054(13) 0.0018(11) C3 0.0146(14) 0.0142(13) 0.0354(18) -0.0013(12) -0.0003(13) 0.0033(11) C4 0.0178(14) 0.0168(13) 0.0252(16) -0.0007(12) 0.0013(12) 0.0035(11) C5 0.0146(14) 0.0129(12) 0.0190(14) -0.0030(11) -0.0009(11) -0.0015(10) C6 0.0126(13) 0.0092(11) 0.0197(15) -0.0005(10) -0.0020(10) -0.0013(10) C7 0.0130(13) 0.0147(13) 0.0203(14) -0.0036(11) 0.0014(11) 0.0001(10) C8 0.0160(14) 0.0148(13) 0.0148(14) 0.0002(10) 0.0013(11) -0.0033(11) C9 0.0119(13) 0.0148(13) 0.0186(14) 0.0008(11) -0.0026(11) -0.0008(10) C10 0.0111(12) 0.0148(11) 0.0218(16) 0.0003(11) 0.0024(11) 0.0014(9) C11 0.0128(13) 0.0110(12) 0.0166(13) -0.0004(10) 0.0002(11) -0.0026(10) C12 0.0137(13) 0.0194(12) 0.0213(16) 0.0029(12) 0.0003(12) -0.0006(10) C13 0.0151(13) 0.0109(12) 0.0123(13) 0.0016(10) 0.0026(11) 0.0002(10) C14 0.0133(13) 0.0150(13) 0.0193(14) -0.0014(11) -0.0006(11) 0.0032(10) C15 0.0141(13) 0.0185(14) 0.0214(15) 0.0007(11) -0.0033(11) -0.0041(11) C16 0.0177(14) 0.0129(12) 0.0185(14) -0.0008(11) -0.0014(11) -0.0005(11) C17 0.0140(14) 0.0156(13) 0.0184(14) 0.0006(11) 0.0010(11) 0.0044(10) C18 0.0126(13) 0.0166(13) 0.0128(12) 0.0021(10) -0.0008(11) 0.0011(10) C19 0.0147(13) 0.0136(12) 0.0122(13) 0.0020(10) 0.0001(11) -0.0006(10) C20 0.0149(14) 0.0171(13) 0.0174(14) -0.0024(11) 0.0005(11) 0.0018(11) C21 0.0134(14) 0.0243(15) 0.0245(15) -0.0009(12) 0.0002(12) 0.0040(11) C22 0.0126(12) 0.0232(13) 0.0218(14) 0.0025(15) -0.0007(15) -0.0029(10) C23 0.0163(12) 0.0170(12) 0.0209(13) 0.0011(14) 0.0027(15) -0.0006(9) C24 0.0182(15) 0.0191(14) 0.0337(18) -0.0015(13) -0.0059(13) 0.0003(12) C25 0.0198(15) 0.0205(14) 0.0207(15) -0.0033(11) -0.0035(11) 0.0018(11) C26 0.0308(18) 0.0285(16) 0.0164(15) 0.0000(12) -0.0040(13) 0.0017(13) C27 0.0263(17) 0.0267(16) 0.0162(15) 0.0040(12) 0.0014(13) 0.0030(13) C28 0.0206(13) 0.0184(13) 0.0201(15) 0.0031(12) 0.0045(13) 0.0027(10) C29 0.0131(14) 0.0129(14) 0.0206(16) 0.0015(12) -0.0003(12) 0.0031(11) C30 0.0143(13) 0.0120(12) 0.0179(13) 0.0021(10) 0.0014(11) 0.0018(10) C31 0.0185(13) 0.0118(11) 0.0194(16) 0.0006(10) 0.0003(11) -0.0002(10) C32 0.0194(16) 0.0145(14) 0.0263(16) 0.0032(12) 0.0018(13) -0.0018(11) C33 0.0260(14) 0.0208(13) 0.0213(14) 0.0070(15) 0.0040(15) -0.0011(11) C34 0.0223(16) 0.0135(13) 0.0248(16) 0.0008(12) -0.0003(13) -0.0026(11) C35 0.0348(18) 0.0184(14) 0.0163(15) -0.0019(12) -0.0013(13) -0.0069(13) C36 0.0272(17) 0.0154(15) 0.0180(15) 0.0014(12) 0.0003(13) -0.0038(12) C37 0.047(2) 0.0416(17) 0.0186(14) 0.0101(19) 0.005(2) -0.0061(14) C38 0.0331(18) 0.0183(15) 0.0305(17) -0.0004(13) -0.0035(14) -0.0083(13) P1 0.0268(5) 0.0423(5) 0.0567(6) -0.0283(5) -0.0120(4) 0.0060(4) F7 0.0638(19) 0.0468(15) 0.269(6) -0.082(2) -0.053(3) 0.0145(14) F8 0.073(2) 0.211(4) 0.090(3) 0.049(3) 0.031(2) 0.075(2) F9 0.093(2) 0.0371(12) 0.0501(14) -0.0074(11) -0.0264(14) 0.0112(13) F10 0.0581(15) 0.0500(14) 0.0830(19) 0.0161(13) -0.0138(14) 0.0054(12) F11 0.0566(19) 0.075(2) 0.232(5) 0.045(3) 0.063(2) 0.0230(16) F12 0.127(3) 0.216(5) 0.167(4) -0.143(4) -0.122(3) 0.102(3) _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 2.008(3) . ? Ir1 C13 2.011(3) . ? Ir1 N2 2.049(2) . ? Ir1 N1 2.055(2) . ? Ir1 N4 2.138(2) . ? Ir1 N3 2.140(2) . ? F1 C12 1.338(3) . ? F2 C12 1.343(3) . ? F3 C12 1.353(3) . ? F4 C24 1.344(3) . ? F5 C24 1.352(4) . ? F6 C24 1.346(4) . ? N1 C1 1.342(3) . ? N1 C5 1.373(3) . ? N2 C23 1.345(3) . ? N2 C19 1.366(3) . ? N3 C25 1.330(4) . ? N3 C29 1.364(4) . ? N4 C36 1.330(4) . ? N4 C30 1.368(3) . ? C1 C2 1.389(4) . ? C1 H1 0.9500 . ? C2 C3 1.387(4) . ? C2 H2 0.9500 . ? C3 C4 1.383(4) . ? C3 H3 0.9500 . ? C4 C5 1.396(4) . ? C4 H4 0.9500 . ? C5 C6 1.468(4) . ? C6 C7 1.405(4) . ? C6 C11 1.416(4) . ? C7 C8 1.385(4) . ? C7 H7 0.9500 . ? C8 C9 1.394(4) . ? C8 C12 1.498(4) . ? C9 C10 1.389(4) . ? C9 H9 0.9500 . ? C10 C11 1.400(4) . ? C10 H10 0.9500 . ? C13 C14 1.402(4) . ? C13 C18 1.421(4) . ? C14 C15 1.389(4) . ? C14 H14 0.9500 . ? C15 C16 1.388(4) . ? C15 H15 0.9500 . ? C16 C17 1.391(4) . ? C16 C24 1.491(4) . ? C17 C18 1.389(4) . ? C17 H17 0.9500 . ? C18 C19 1.469(4) . ? C19 C20 1.396(4) . ? C20 C21 1.385(4) . ? C20 H20 0.9500 . ? C21 C22 1.379(4) . ? C21 H21 0.9500 . ? C22 C23 1.375(4) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C25 C26 1.390(4) . ? C25 H25 0.9500 . ? C26 C27 1.375(4) . ? C26 H26 0.9500 . ? C27 C28 1.423(4) . ? C27 C37 1.506(5) . ? C28 C29 1.402(4) . ? C28 C33 1.437(4) . ? C29 C30 1.439(4) . ? C30 C31 1.415(4) . ? C31 C34 1.411(4) . ? C31 C32 1.428(4) . ? C32 C33 1.352(5) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.381(4) . ? C34 C38 1.500(4) . ? C35 C36 1.396(4) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? P1 F11 1.556(3) . ? P1 F12 1.566(3) . ? P1 F7 1.567(3) . ? P1 F8 1.581(3) . ? P1 F9 1.583(2) . ? P1 F10 1.584(3) . ? 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 C13 87.16(11) . . ? C11 Ir1 N2 94.32(10) . . ? C13 Ir1 N2 80.73(10) . . ? C11 Ir1 N1 80.61(10) . . ? C13 Ir1 N1 96.62(10) . . ? N2 Ir1 N1 174.43(9) . . ? C11 Ir1 N4 97.55(10) . . ? C13 Ir1 N4 172.64(10) . . ? N2 Ir1 N4 93.23(9) . . ? N1 Ir1 N4 89.75(8) . . ? C11 Ir1 N3 174.36(10) . . ? C13 Ir1 N3 98.33(10) . . ? N2 Ir1 N3 87.89(8) . . ? N1 Ir1 N3 97.37(9) . . ? N4 Ir1 N3 77.12(9) . . ? C1 N1 C5 119.5(2) . . ? C1 N1 Ir1 125.15(19) . . ? C5 N1 Ir1 115.19(18) . . ? C23 N2 C19 118.7(2) . . ? C23 N2 Ir1 125.37(17) . . ? C19 N2 Ir1 115.87(17) . . ? C25 N3 C29 118.2(3) . . ? C25 N3 Ir1 127.18(18) . . ? C29 N3 Ir1 114.4(2) . . ? C36 N4 C30 118.0(2) . . ? C36 N4 Ir1 127.4(2) . . ? C30 N4 Ir1 114.25(18) . . ? N1 C1 C2 122.5(3) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C3 C2 C1 118.4(3) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C4 C3 C2 119.6(3) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 119.9(3) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? N1 C5 C4 119.9(3) . . ? N1 C5 C6 113.8(2) . . ? C4 C5 C6 126.3(3) . . ? C7 C6 C11 120.9(2) . . ? C7 C6 C5 123.8(2) . . ? C11 C6 C5 115.3(2) . . ? C8 C7 C6 119.4(3) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C7 C8 C9 120.6(3) . . ? C7 C8 C12 120.9(2) . . ? C9 C8 C12 118.4(2) . . ? C10 C9 C8 120.0(3) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 121.3(2) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C10 C11 C6 117.9(2) . . ? C10 C11 Ir1 127.7(2) . . ? C6 C11 Ir1 114.47(19) . . ? F1 C12 F2 106.6(2) . . ? F1 C12 F3 105.5(2) . . ? F2 C12 F3 105.6(2) . . ? F1 C12 C8 113.8(2) . . ? F2 C12 C8 112.7(2) . . ? F3 C12 C8 112.0(2) . . ? C14 C13 C18 116.8(2) . . ? C14 C13 Ir1 129.0(2) . . ? C18 C13 Ir1 114.07(19) . . ? C15 C14 C13 121.8(3) . . ? C15 C14 H14 119.1 . . ? C13 C14 H14 119.1 . . ? C16 C15 C14 120.0(3) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 120.1(2) . . ? C15 C16 C24 121.0(3) . . ? C17 C16 C24 118.8(3) . . ? C18 C17 C16 119.8(2) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C17 C18 C13 121.5(3) . . ? C17 C18 C19 123.2(2) . . ? C13 C18 C19 115.3(2) . . ? N2 C19 C20 120.6(2) . . ? N2 C19 C18 113.8(2) . . ? C20 C19 C18 125.6(2) . . ? C21 C20 C19 119.3(3) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C22 C21 C20 119.8(3) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C23 C22 C21 118.5(3) . . ? C23 C22 H22 120.8 . . ? C21 C22 H22 120.8 . . ? N2 C23 C22 123.1(2) . . ? N2 C23 H23 118.4 . . ? C22 C23 H23 118.4 . . ? F4 C24 F6 106.5(3) . . ? F4 C24 F5 105.2(3) . . ? F6 C24 F5 105.8(2) . . ? F4 C24 C16 113.0(2) . . ? F6 C24 C16 113.0(3) . . ? F5 C24 C16 112.8(3) . . ? N3 C25 C26 122.5(3) . . ? N3 C25 H25 118.7 . . ? C26 C25 H25 118.7 . . ? C27 C26 C25 120.5(3) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C26 C27 C28 118.3(3) . . ? C26 C27 C37 120.0(3) . . ? C28 C27 C37 121.8(3) . . ? C29 C28 C27 117.5(3) . . ? C29 C28 C33 118.0(3) . . ? C27 C28 C33 124.5(3) . . ? N3 C29 C28 123.0(3) . . ? N3 C29 C30 116.6(3) . . ? C28 C29 C30 120.4(3) . . ? N4 C30 C31 122.7(2) . . ? N4 C30 C29 116.8(2) . . ? C31 C30 C29 120.4(2) . . ? C34 C31 C30 118.0(2) . . ? C34 C31 C32 124.6(2) . . ? C30 C31 C32 117.4(2) . . ? C33 C32 C31 122.3(3) . . ? C33 C32 H32 118.8 . . ? C31 C32 H32 118.8 . . ? C32 C33 C28 121.4(3) . . ? C32 C33 H33 119.3 . . ? C28 C33 H33 119.3 . . ? C35 C34 C31 118.0(3) . . ? C35 C34 C38 120.3(3) . . ? C31 C34 C38 121.7(3) . . ? C34 C35 C36 120.8(3) . . ? C34 C35 H35 119.6 . . ? C36 C35 H35 119.6 . . ? N4 C36 C35 122.5(3) . . ? N4 C36 H36 118.8 . . ? C35 C36 H36 118.8 . . ? C27 C37 H37A 109.5 . . ? C27 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C27 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34 C38 H38A 109.5 . . ? C34 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C34 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? F11 P1 F12 88.9(3) . . ? F11 P1 F7 92.6(2) . . ? F12 P1 F7 90.6(2) . . ? F11 P1 F8 178.0(3) . . ? F12 P1 F8 92.5(3) . . ? F7 P1 F8 88.9(2) . . ? F11 P1 F9 90.6(2) . . ? F12 P1 F9 179.4(3) . . ? F7 P1 F9 88.99(18) . . ? F8 P1 F9 88.04(18) . . ? F11 P1 F10 89.63(16) . . ? F12 P1 F10 88.9(2) . . ? F7 P1 F10 177.7(2) . . ? F8 P1 F10 88.9(2) . . ? F9 P1 F10 91.57(13) . . ? 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 -177.0(2) . . . . ? C13 Ir1 N1 C1 -91.0(2) . . . . ? N4 Ir1 N1 C1 85.3(2) . . . . ? N3 Ir1 N1 C1 8.4(2) . . . . ? C11 Ir1 N1 C5 7.68(18) . . . . ? C13 Ir1 N1 C5 93.68(19) . . . . ? N4 Ir1 N1 C5 -90.01(19) . . . . ? N3 Ir1 N1 C5 -166.99(18) . . . . ? C11 Ir1 N2 C23 -94.6(2) . . . . ? C13 Ir1 N2 C23 179.0(3) . . . . ? N4 Ir1 N2 C23 3.3(2) . . . . ? N3 Ir1 N2 C23 80.2(2) . . . . ? C11 Ir1 N2 C19 83.28(19) . . . . ? C13 Ir1 N2 C19 -3.12(19) . . . . ? N4 Ir1 N2 C19 -178.89(18) . . . . ? N3 Ir1 N2 C19 -101.92(19) . . . . ? C13 Ir1 N3 C25 7.6(3) . . . . ? N2 Ir1 N3 C25 88.0(2) . . . . ? N1 Ir1 N3 C25 -90.2(2) . . . . ? N4 Ir1 N3 C25 -178.2(3) . . . . ? C13 Ir1 N3 C29 -166.7(2) . . . . ? N2 Ir1 N3 C29 -86.4(2) . . . . ? N1 Ir1 N3 C29 95.4(2) . . . . ? N4 Ir1 N3 C29 7.38(19) . . . . ? C11 Ir1 N4 C36 1.6(3) . . . . ? N2 Ir1 N4 C36 -93.2(3) . . . . ? N1 Ir1 N4 C36 82.1(3) . . . . ? N3 Ir1 N4 C36 179.7(3) . . . . ? C11 Ir1 N4 C30 174.56(19) . . . . ? N2 Ir1 N4 C30 79.77(19) . . . . ? N1 Ir1 N4 C30 -104.94(19) . . . . ? N3 Ir1 N4 C30 -7.32(18) . . . . ? C5 N1 C1 C2 2.2(4) . . . . ? Ir1 N1 C1 C2 -173.0(2) . . . . ? N1 C1 C2 C3 2.1(4) . . . . ? C1 C2 C3 C4 -4.0(4) . . . . ? C2 C3 C4 C5 1.7(4) . . . . ? C1 N1 C5 C4 -4.5(4) . . . . ? Ir1 N1 C5 C4 171.1(2) . . . . ? C1 N1 C5 C6 175.1(2) . . . . ? Ir1 N1 C5 C6 -9.3(3) . . . . ? C3 C4 C5 N1 2.6(4) . . . . ? C3 C4 C5 C6 -176.9(3) . . . . ? N1 C5 C6 C7 -172.0(2) . . . . ? C4 C5 C6 C7 7.5(4) . . . . ? N1 C5 C6 C11 5.7(3) . . . . ? C4 C5 C6 C11 -174.8(3) . . . . ? C11 C6 C7 C8 -0.7(4) . . . . ? C5 C6 C7 C8 176.8(3) . . . . ? C6 C7 C8 C9 0.9(4) . . . . ? C6 C7 C8 C12 -175.6(2) . . . . ? C7 C8 C9 C10 0.1(4) . . . . ? C12 C8 C9 C10 176.8(2) . . . . ? C8 C9 C10 C11 -1.4(4) . . . . ? C9 C10 C11 C6 1.6(4) . . . . ? C9 C10 C11 Ir1 -177.2(2) . . . . ? C7 C6 C11 C10 -0.5(4) . . . . ? C5 C6 C11 C10 -178.3(2) . . . . ? C7 C6 C11 Ir1 178.49(19) . . . . ? C5 C6 C11 Ir1 0.7(3) . . . . ? C13 Ir1 C11 C10 77.3(2) . . . . ? N2 Ir1 C11 C10 -3.1(2) . . . . ? N1 Ir1 C11 C10 174.5(3) . . . . ? N4 Ir1 C11 C10 -97.0(2) . . . . ? C13 Ir1 C11 C6 -101.6(2) . . . . ? N2 Ir1 C11 C6 177.97(19) . . . . ? N1 Ir1 C11 C6 -4.36(18) . . . . ? N4 Ir1 C11 C6 84.1(2) . . . . ? C7 C8 C12 F1 -22.9(4) . . . . ? C9 C8 C12 F1 160.5(2) . . . . ? C7 C8 C12 F2 -144.4(2) . . . . ? C9 C8 C12 F2 39.0(3) . . . . ? C7 C8 C12 F3 96.8(3) . . . . ? C9 C8 C12 F3 -79.9(3) . . . . ? C11 Ir1 C13 C14 86.8(3) . . . . ? N2 Ir1 C13 C14 -178.3(3) . . . . ? N1 Ir1 C13 C14 6.6(3) . . . . ? N3 Ir1 C13 C14 -91.9(3) . . . . ? C11 Ir1 C13 C18 -91.0(2) . . . . ? N2 Ir1 C13 C18 3.88(19) . . . . ? N1 Ir1 C13 C18 -171.17(19) . . . . ? N3 Ir1 C13 C18 90.3(2) . . . . ? C18 C13 C14 C15 1.8(4) . . . . ? Ir1 C13 C14 C15 -175.9(2) . . . . ? C13 C14 C15 C16 -0.3(4) . . . . ? C14 C15 C16 C17 -1.0(4) . . . . ? C14 C15 C16 C24 175.8(3) . . . . ? C15 C16 C17 C18 0.7(4) . . . . ? C24 C16 C17 C18 -176.1(3) . . . . ? C16 C17 C18 C13 0.9(4) . . . . ? C16 C17 C18 C19 -179.0(3) . . . . ? C14 C13 C18 C17 -2.1(4) . . . . ? Ir1 C13 C18 C17 175.9(2) . . . . ? C14 C13 C18 C19 177.8(2) . . . . ? Ir1 C13 C18 C19 -4.2(3) . . . . ? C23 N2 C19 C20 -0.3(4) . . . . ? Ir1 N2 C19 C20 -178.26(19) . . . . ? C23 N2 C19 C18 179.7(3) . . . . ? Ir1 N2 C19 C18 1.7(3) . . . . ? C17 C18 C19 N2 -178.5(2) . . . . ? C13 C18 C19 N2 1.6(3) . . . . ? C17 C18 C19 C20 1.5(4) . . . . ? C13 C18 C19 C20 -178.4(3) . . . . ? N2 C19 C20 C21 0.0(4) . . . . ? C18 C19 C20 C21 -179.9(3) . . . . ? C19 C20 C21 C22 0.1(4) . . . . ? C20 C21 C22 C23 0.0(5) . . . . ? C19 N2 C23 C22 0.4(5) . . . . ? Ir1 N2 C23 C22 178.2(3) . . . . ? C21 C22 C23 N2 -0.2(5) . . . . ? C15 C16 C24 F4 24.8(4) . . . . ? C17 C16 C24 F4 -158.4(3) . . . . ? C15 C16 C24 F6 145.7(3) . . . . ? C17 C16 C24 F6 -37.5(4) . . . . ? C15 C16 C24 F5 -94.4(3) . . . . ? C17 C16 C24 F5 82.4(3) . . . . ? C29 N3 C25 C26 0.3(4) . . . . ? Ir1 N3 C25 C26 -173.9(2) . . . . ? N3 C25 C26 C27 1.0(5) . . . . ? C25 C26 C27 C28 -1.4(5) . . . . ? C25 C26 C27 C37 179.6(3) . . . . ? C26 C27 C28 C29 0.5(4) . . . . ? C37 C27 C28 C29 179.5(3) . . . . ? C26 C27 C28 C33 179.2(3) . . . . ? C37 C27 C28 C33 -1.7(5) . . . . ? C25 N3 C29 C28 -1.2(4) . . . . ? Ir1 N3 C29 C28 173.7(2) . . . . ? C25 N3 C29 C30 178.6(3) . . . . ? Ir1 N3 C29 C30 -6.5(3) . . . . ? C27 C28 C29 N3 0.8(4) . . . . ? C33 C28 C29 N3 -178.0(3) . . . . ? C27 C28 C29 C30 -179.0(3) . . . . ? C33 C28 C29 C30 2.2(4) . . . . ? C36 N4 C30 C31 2.1(4) . . . . ? Ir1 N4 C30 C31 -171.6(2) . . . . ? C36 N4 C30 C29 -179.9(2) . . . . ? Ir1 N4 C30 C29 6.4(3) . . . . ? N3 C29 C30 N4 0.1(4) . . . . ? C28 C29 C30 N4 179.9(3) . . . . ? N3 C29 C30 C31 178.1(2) . . . . ? C28 C29 C30 C31 -2.1(4) . . . . ? N4 C30 C31 C34 -0.6(4) . . . . ? C29 C30 C31 C34 -178.5(3) . . . . ? N4 C30 C31 C32 178.8(3) . . . . ? C29 C30 C31 C32 0.9(4) . . . . ? C34 C31 C32 C33 179.5(3) . . . . ? C30 C31 C32 C33 0.0(4) . . . . ? C31 C32 C33 C28 0.1(4) . . . . ? C29 C28 C33 C32 -1.2(4) . . . . ? C27 C28 C33 C32 -180.0(3) . . . . ? C30 C31 C34 C35 -1.3(4) . . . . ? C32 C31 C34 C35 179.2(3) . . . . ? C30 C31 C34 C38 177.9(3) . . . . ? C32 C31 C34 C38 -1.5(5) . . . . ? C31 C34 C35 C36 1.9(5) . . . . ? C38 C34 C35 C36 -177.4(3) . . . . ? C30 N4 C36 C35 -1.6(4) . . . . ? Ir1 N4 C36 C35 171.2(2) . . . . ? C34 C35 C36 N4 -0.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.576 _refine_diff_density_min -0.583 _refine_diff_density_rms 0.069 _iucr_refine_instructions_details ; TITL NS-51 in Fdd2 CELL 0.71073 19.1978 68.9579 11.0075 90.0000 90.0000 90.0000 ZERR 16.00 0.0034 0.0101 0.0012 0.0000 0.0000 0.0000 LATT -4 SYMM -X, -Y, Z SYMM 0.25+X, 0.25-Y, 0.25+Z SYMM 0.25-X, 0.25+Y, 0.25+Z SFAC C H N F P IR UNIT 608 416 64 192 16 16 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 (slightly disordered) REM ---------------------------------------------------------- L.S. 10 ACTA CONF SIZE 0.34 0.22 0.18 WPDB -2 BOND $H FMAP 2 PLAN 10 TWIN TEMP -173 WGHT 0.005600 38.347301 BASF 0.02079 FVAR 0.05800 IR1 6 0.466792 0.428608 0.539773 11.00000 0.01130 0.00981 = 0.01451 0.00085 0.00063 -0.00015 F1 4 0.342123 0.406153 1.116868 11.00000 0.02105 0.04628 = 0.02055 0.00830 0.00855 0.01180 F2 4 0.443600 0.393256 1.133129 11.00000 0.01621 0.03226 = 0.01867 0.00421 -0.00229 0.00088 F3 4 0.361058 0.377840 1.043740 11.00000 0.04871 0.02943 = 0.02703 0.00411 0.00141 -0.02360 F4 4 0.338874 0.340732 0.306989 11.00000 0.03217 0.02089 = 0.07908 -0.01211 -0.03058 0.00163 F5 4 0.395572 0.331907 0.465223 11.00000 0.05109 0.01630 = 0.04404 0.00558 0.00006 -0.00416 F6 4 0.449633 0.335950 0.295928 11.00000 0.03523 0.02004 = 0.05397 -0.01438 0.00928 -0.00147 N1 3 0.368578 0.439381 0.570912 11.00000 0.01363 0.01104 = 0.01920 -0.00218 -0.00078 -0.00160 N2 3 0.562438 0.415786 0.520641 11.00000 0.01234 0.01573 = 0.01093 0.00206 0.00124 -0.00066 N3 3 0.484839 0.442851 0.369944 11.00000 0.01538 0.01257 = 0.01651 -0.00029 0.00070 0.00070 N4 3 0.510382 0.455808 0.593822 11.00000 0.01486 0.01355 = 0.01745 0.00257 0.00106 0.00064 C1 1 0.330887 0.449650 0.490845 11.00000 0.01489 0.01557 = 0.02293 0.00042 -0.00433 -0.00057 AFIX 43 H1 2 0.347908 0.451054 0.410285 11.00000 -1.20000 AFIX 0 C2 1 0.267912 0.458302 0.521368 11.00000 0.01848 0.01554 = 0.02877 0.00004 -0.00537 0.00178 AFIX 43 H2 2 0.241465 0.465128 0.462275 11.00000 -1.20000 AFIX 0 C3 1 0.244607 0.456728 0.640233 11.00000 0.01461 0.01416 = 0.03540 -0.00126 -0.00032 0.00333 AFIX 43 H3 2 0.203260 0.463189 0.664937 11.00000 -1.20000 AFIX 0 C4 1 0.281913 0.445698 0.722601 11.00000 0.01781 0.01676 = 0.02524 -0.00067 0.00128 0.00351 AFIX 43 H4 2 0.265570 0.444272 0.803571 11.00000 -1.20000 AFIX 0 C5 1 0.343617 0.436666 0.686535 11.00000 0.01460 0.01288 = 0.01902 -0.00299 -0.00093 -0.00146 C6 1 0.387091 0.423824 0.761210 11.00000 0.01257 0.00925 = 0.01966 -0.00053 -0.00203 -0.00128 C7 1 0.367720 0.417091 0.876850 11.00000 0.01300 0.01469 = 0.02030 -0.00359 0.00139 0.00014 AFIX 43 H7 2 0.325427 0.421312 0.913021 11.00000 -1.20000 AFIX 0 C8 1 0.410863 0.404240 0.937628 11.00000 0.01597 0.01478 = 0.01484 0.00018 0.00132 -0.00331 C9 1 0.473457 0.398215 0.885792 11.00000 0.01193 0.01479 = 0.01863 0.00080 -0.00264 -0.00078 AFIX 43 H9 2 0.502682 0.389377 0.928040 11.00000 -1.20000 AFIX 0 C10 1 0.493111 0.405136 0.772334 11.00000 0.01108 0.01481 = 0.02183 0.00031 0.00242 0.00141 AFIX 43 H10 2 0.536377 0.401179 0.738571 11.00000 -1.20000 AFIX 0 C11 1 0.450358 0.417834 0.706786 11.00000 0.01279 0.01097 = 0.01655 -0.00037 0.00023 -0.00259 C12 1 0.389632 0.395652 1.056989 11.00000 0.01367 0.01944 = 0.02127 0.00287 0.00033 -0.00056 C13 1 0.436515 0.402685 0.474965 11.00000 0.01509 0.01093 = 0.01232 0.00160 0.00260 0.00015 C14 1 0.369161 0.396071 0.448372 11.00000 0.01326 0.01500 = 0.01925 -0.00141 -0.00060 0.00320 AFIX 43 H14 2 0.331028 0.404761 0.456203 11.00000 -1.20000 AFIX 0 C15 1 0.356684 0.377147 0.410871 11.00000 0.01410 0.01847 = 0.02143 0.00065 -0.00333 -0.00415 AFIX 43 H15 2 0.310474 0.373037 0.393821 11.00000 -1.20000 AFIX 0 C16 1 0.411708 0.364245 0.398313 11.00000 0.01768 0.01286 = 0.01848 -0.00076 -0.00139 -0.00045 C17 1 0.479540 0.370326 0.421373 11.00000 0.01400 0.01562 = 0.01838 0.00058 0.00098 0.00436 AFIX 43 H17 2 0.517277 0.361543 0.411904 11.00000 -1.20000 AFIX 0 C18 1 0.491906 0.389283 0.458292 11.00000 0.01257 0.01660 = 0.01281 0.00214 -0.00081 0.00111 C19 1 0.561964 0.396939 0.482550 11.00000 0.01473 0.01357 = 0.01217 0.00201 0.00013 -0.00057 C20 1 0.624158 0.386666 0.469689 11.00000 0.01489 0.01713 = 0.01744 -0.00236 0.00053 0.00178 AFIX 43 H20 2 0.623629 0.373559 0.443126 11.00000 -1.20000 AFIX 0 C21 1 0.686684 0.395774 0.496048 11.00000 0.01338 0.02432 = 0.02449 -0.00093 0.00018 0.00403 AFIX 43 H21 2 0.729370 0.388939 0.487530 11.00000 -1.20000 AFIX 0 C22 1 0.686735 0.414790 0.534682 11.00000 0.01264 0.02315 = 0.02179 0.00252 -0.00073 -0.00293 AFIX 43 H22 2 0.729173 0.421236 0.553115 11.00000 -1.20000 AFIX 0 C23 1 0.623927 0.424215 0.545921 11.00000 0.01629 0.01704 = 0.02090 0.00108 0.00272 -0.00062 AFIX 43 H23 2 0.623980 0.437305 0.572828 11.00000 -1.20000 AFIX 0 C24 1 0.399197 0.343514 0.366484 11.00000 0.01817 0.01914 = 0.03370 -0.00149 -0.00592 0.00032 C25 1 0.469957 0.436176 0.259578 11.00000 0.01977 0.02051 = 0.02067 -0.00333 -0.00355 0.00175 AFIX 43 H25 2 0.444859 0.424357 0.252508 11.00000 -1.20000 AFIX 0 C26 1 0.489701 0.445823 0.154203 11.00000 0.03080 0.02845 = 0.01645 0.00002 -0.00396 0.00169 AFIX 43 H26 2 0.477331 0.440635 0.077219 11.00000 -1.20000 AFIX 0 C27 1 0.526999 0.462818 0.160488 11.00000 0.02628 0.02670 = 0.01621 0.00399 0.00138 0.00304 C28 1 0.543316 0.470403 0.277295 11.00000 0.02062 0.01842 = 0.02007 0.00313 0.00447 0.00271 C29 1 0.520602 0.459885 0.378877 11.00000 0.01310 0.01294 = 0.02057 0.00147 -0.00025 0.00309 C30 1 0.534359 0.466888 0.499625 11.00000 0.01430 0.01202 = 0.01785 0.00207 0.00141 0.00184 C31 1 0.572937 0.484133 0.517442 11.00000 0.01845 0.01177 = 0.01936 0.00062 0.00028 -0.00017 C32 1 0.596219 0.494228 0.411656 11.00000 0.01940 0.01450 = 0.02635 0.00317 0.00182 -0.00182 AFIX 43 H32 2 0.622246 0.505840 0.421497 11.00000 -1.20000 AFIX 0 C33 1 0.582524 0.487842 0.298045 11.00000 0.02600 0.02081 = 0.02132 0.00697 0.00401 -0.00111 AFIX 43 H33 2 0.599183 0.495040 0.230436 11.00000 -1.20000 AFIX 0 C34 1 0.586249 0.490071 0.637875 11.00000 0.02229 0.01349 = 0.02476 0.00076 -0.00028 -0.00256 C35 1 0.559552 0.478905 0.731095 11.00000 0.03478 0.01836 = 0.01628 -0.00190 -0.00130 -0.00689 AFIX 43 H35 2 0.566596 0.482800 0.812962 11.00000 -1.20000 AFIX 0 C36 1 0.522342 0.461965 0.706394 11.00000 0.02723 0.01542 = 0.01795 0.00144 0.00034 -0.00384 AFIX 43 H36 2 0.504907 0.454556 0.772496 11.00000 -1.20000 AFIX 0 C37 1 0.548484 0.473053 0.045603 11.00000 0.04694 0.04164 = 0.01863 0.01005 0.00505 -0.00611 AFIX 33 H37A 2 0.544836 0.464085 -0.023167 11.00000 -1.50000 H37B 2 0.596735 0.477525 0.053349 11.00000 -1.50000 H37C 2 0.517865 0.484211 0.031859 11.00000 -1.50000 AFIX 0 C38 1 0.628726 0.507790 0.665550 11.00000 0.03312 0.01825 = 0.03052 -0.00037 -0.00348 -0.00831 AFIX 33 H38A 2 0.629825 0.509899 0.753573 11.00000 -1.50000 H38B 2 0.607784 0.519083 0.625709 11.00000 -1.50000 H38C 2 0.676315 0.505962 0.635444 11.00000 -1.50000 AFIX 0 P1 5 0.803190 0.470892 0.592919 11.00000 0.02676 0.04225 = 0.05669 -0.02828 -0.01197 0.00601 F7 4 0.813547 0.448368 0.587732 11.00000 0.06383 0.04678 = 0.26928 -0.08249 -0.05306 0.01445 F8 4 0.871308 0.473335 0.513596 11.00000 0.07316 0.21087 = 0.09043 0.04894 0.03139 0.07528 F9 4 0.851103 0.471504 0.709897 11.00000 0.09347 0.03714 = 0.05005 -0.00743 -0.02642 0.01123 F10 4 0.794826 0.493748 0.593800 11.00000 0.05808 0.05004 = 0.08296 0.01615 -0.01375 0.00544 F11 4 0.737050 0.469082 0.673778 11.00000 0.05664 0.07463 = 0.23161 0.04491 0.06322 0.02303 F12 4 0.755291 0.470104 0.477890 11.00000 0.12670 0.21594 = 0.16683 -0.14266 -0.12214 0.10184 HKLF 4 1 0 1 0 0 0 1 1 0 0 REM NS-51 in Fdd2 REM R1 = 0.0168 for 7780 Fo > 4sig(Fo) and 0.0181 for all 8011 data REM 506 parameters refined using 1 restraints END WGHT 0.0055 38.3555 REM Highest difference peak 0.576, deepest hole -0.583, 1-sigma level 0.069 Q1 1 0.8518 0.4618 0.5222 11.00000 0.05 0.58 Q2 1 0.4445 0.3481 1.0470 11.00000 0.05 0.54 Q3 1 0.1470 0.4406 0.3381 11.00000 0.05 0.53 Q4 1 0.8759 0.4786 0.5342 11.00000 0.05 0.52 Q5 1 0.7409 0.4623 0.5198 11.00000 0.05 0.44 Q6 1 0.7753 0.4745 0.4473 11.00000 0.05 0.44 Q7 1 0.3287 0.4285 0.5387 11.00000 0.05 0.43 Q8 1 0.7894 0.4479 0.6683 11.00000 0.05 0.37 Q9 1 0.7578 0.4748 0.7087 11.00000 0.05 0.37 Q10 1 0.4619 0.4406 0.5564 11.00000 0.05 0.36 ; data_ns-52 _database_code_depnum_ccdc_archive 'CCDC 914726' #TrackingRef 'total.cif' _audit_update_record ; 2012-07-20 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H38 F6 Ir N4, F6 P' _chemical_formula_sum 'C42 H38 F12 Ir N4 P' _chemical_formula_weight 1049.93 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' 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 13.440(3) _cell_length_b 13.5222(13) _cell_length_c 26.448(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.526(16) _cell_angle_gamma 90.00 _cell_volume 4804.9(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 115 _cell_measurement_theta_min 3 _cell_measurement_theta_max 22 _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2072 _exptl_absorpt_coefficient_mu 2.890 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3690 _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 52312 _diffrn_reflns_av_R_equivalents 0.0900 _diffrn_reflns_av_sigmaI/netI 0.0695 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10899 _reflns_number_gt 8408 _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^)+(0.0882P)^2^+20.6754P] 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 10899 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0829 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.1679 _refine_ls_wR_factor_gt 0.1552 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _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 0.543717(19) 0.671134(19) 0.337772(9) 0.01782(10) Uani 1 1 d . . . F1 F 0.9149(4) 0.3767(4) 0.2411(2) 0.0520(15) Uani 1 1 d . . . F2 F 0.9007(6) 0.3047(5) 0.3113(2) 0.082(3) Uani 1 1 d . . . F3 F 0.8080(5) 0.2641(5) 0.2480(3) 0.080(2) Uani 1 1 d . . . F4 F 0.2309(4) 0.2771(4) 0.2879(2) 0.0453(13) Uani 1 1 d . . . F5 F 0.1423(4) 0.3416(4) 0.34589(19) 0.0526(15) Uani 1 1 d . . . F6 F 0.1267(4) 0.3929(4) 0.26799(19) 0.0415(12) Uani 1 1 d . . . N1 N 0.6011(5) 0.6184(4) 0.4054(2) 0.0209(12) Uani 1 1 d . . . N2 N 0.4837(5) 0.7073(4) 0.2681(2) 0.0205(12) Uani 1 1 d . . . N3 N 0.4695(4) 0.7987(4) 0.3665(2) 0.0187(11) Uani 1 1 d . . . N4 N 0.6590(4) 0.7804(4) 0.3434(2) 0.0203(12) Uani 1 1 d . . . C1 C 0.5725(5) 0.6514(5) 0.4517(3) 0.0237(15) Uani 1 1 d . . . H1 H 0.5221 0.7004 0.4536 0.028 Uiso 1 1 calc R . . C2 C 0.6160(6) 0.6144(5) 0.4958(3) 0.0299(17) Uani 1 1 d . . . H2 H 0.5956 0.6381 0.5277 0.036 Uiso 1 1 calc R . . C3 C 0.6888(6) 0.5432(6) 0.4933(3) 0.0296(17) Uani 1 1 d . . . H3 H 0.7188 0.5175 0.5235 0.036 Uiso 1 1 calc R . . C4 C 0.7185(6) 0.5087(5) 0.4463(3) 0.0257(15) Uani 1 1 d . . . H4 H 0.7695 0.4603 0.4441 0.031 Uiso 1 1 calc R . . C5 C 0.6722(5) 0.5463(5) 0.4026(3) 0.0203(14) Uani 1 1 d . . . C6 C 0.6902(5) 0.5136(5) 0.3498(2) 0.0227(14) Uani 1 1 d . . . C7 C 0.7623(5) 0.4420(5) 0.3377(3) 0.0228(14) Uani 1 1 d . . . H7 H 0.8021 0.4116 0.3635 0.027 Uiso 1 1 calc R . . C8 C 0.7734(5) 0.4175(5) 0.2879(3) 0.0238(15) Uani 1 1 d . . . C9 C 0.7170(6) 0.4623(5) 0.2496(3) 0.0284(17) Uani 1 1 d . . . H9 H 0.7267 0.4447 0.2153 0.034 Uiso 1 1 calc R . . C10 C 0.6453(6) 0.5337(5) 0.2617(3) 0.0262(16) Uani 1 1 d . . . H10 H 0.6057 0.5630 0.2355 0.031 Uiso 1 1 calc R . . C11 C 0.6317(5) 0.5620(5) 0.3122(3) 0.0216(14) Uani 1 1 d . . . C12 C 0.4302(5) 0.5743(5) 0.3344(2) 0.0199(14) Uani 1 1 d . . . C13 C 0.3966(5) 0.5104(5) 0.3718(2) 0.0229(14) Uani 1 1 d . . . H13 H 0.4278 0.5125 0.4045 0.027 Uiso 1 1 calc R . . C14 C 0.3190(6) 0.4439(6) 0.3629(3) 0.0267(16) Uani 1 1 d . . . H14 H 0.2979 0.4012 0.3891 0.032 Uiso 1 1 calc R . . C15 C 0.2722(6) 0.4407(5) 0.3147(3) 0.0253(15) Uani 1 1 d . . . C16 C 0.3007(5) 0.5033(5) 0.2766(2) 0.0203(13) Uani 1 1 d . . . H16 H 0.2684 0.5010 0.2442 0.024 Uiso 1 1 calc R . . C17 C 0.3780(5) 0.5703(5) 0.2865(2) 0.0210(14) Uani 1 1 d . . . C18 C 0.4108(6) 0.6466(5) 0.2501(3) 0.0246(15) Uani 1 1 d . . . C19 C 0.3673(6) 0.6629(6) 0.2017(3) 0.0289(16) Uani 1 1 d . . . H19 H 0.3176 0.6191 0.1887 0.035 Uiso 1 1 calc R . . C20 C 0.3972(5) 0.7428(6) 0.1731(3) 0.0251(15) Uani 1 1 d . . . H20 H 0.3673 0.7561 0.1408 0.030 Uiso 1 1 calc R . . C21 C 0.4728(6) 0.8033(6) 0.1932(3) 0.0287(16) Uani 1 1 d . . . H21 H 0.4949 0.8583 0.1742 0.034 Uiso 1 1 calc R . . C22 C 0.5157(6) 0.7846(5) 0.2399(3) 0.0270(16) Uani 1 1 d . . . H22 H 0.5679 0.8257 0.2525 0.032 Uiso 1 1 calc R . . C23 C 0.8478(6) 0.3406(6) 0.2727(3) 0.0325(18) Uani 1 1 d . . . C24 C 0.1926(6) 0.3651(6) 0.3041(3) 0.0264(16) Uani 1 1 d . . . C25 C 0.3708(5) 0.8070(5) 0.3708(2) 0.0190(13) Uani 1 1 d . . . H25 H 0.3297 0.7521 0.3621 0.023 Uiso 1 1 calc R . . C26 C 0.3265(5) 0.8935(5) 0.3877(3) 0.0237(15) Uani 1 1 d . . . H26 H 0.2562 0.8966 0.3905 0.028 Uiso 1 1 calc R . . C27 C 0.3850(5) 0.9759(5) 0.4005(2) 0.0195(13) Uani 1 1 d . . . C28 C 0.4878(5) 0.9673(5) 0.3945(3) 0.0241(15) Uani 1 1 d . . . H28 H 0.5301 1.0219 0.4020 0.029 Uiso 1 1 calc R . . C29 C 0.5280(5) 0.8784(5) 0.3776(2) 0.0222(14) Uani 1 1 d . . . C30 C 0.6359(5) 0.8651(5) 0.3678(2) 0.0209(14) Uani 1 1 d . . . C31 C 0.7079(5) 0.9327(5) 0.3828(2) 0.0200(14) Uani 1 1 d . . . H31 H 0.6897 0.9905 0.4007 0.024 Uiso 1 1 calc R . . C32 C 0.8085(5) 0.9160(5) 0.3714(2) 0.0228(15) Uani 1 1 d . . . C33 C 0.8304(6) 0.8292(6) 0.3449(3) 0.0280(16) Uani 1 1 d . . . H33 H 0.8970 0.8147 0.3362 0.034 Uiso 1 1 calc R . . C34 C 0.7548(5) 0.7652(6) 0.3316(3) 0.0245(15) Uani 1 1 d . . . H34 H 0.7708 0.7074 0.3131 0.029 Uiso 1 1 calc R . . C35 C 0.3406(5) 1.0726(5) 0.4219(3) 0.0237(15) Uani 1 1 d . . . C36 C 0.2264(6) 1.0756(6) 0.4160(3) 0.0362(19) Uani 1 1 d . . . H36A H 0.1972 1.0302 0.4404 0.054 Uiso 1 1 calc R . . H36B H 0.2065 1.0555 0.3816 0.054 Uiso 1 1 calc R . . H36C H 0.2029 1.1430 0.4223 0.054 Uiso 1 1 calc R . . C37 C 0.3811(6) 1.1617(5) 0.3933(3) 0.0320(17) Uani 1 1 d . . . H37A H 0.3486 1.2222 0.4050 0.048 Uiso 1 1 calc R . . H37B H 0.3677 1.1533 0.3570 0.048 Uiso 1 1 calc R . . H37C H 0.4531 1.1668 0.3997 0.048 Uiso 1 1 calc R . . C38 C 0.3696(6) 1.0788(6) 0.4783(3) 0.0333(18) Uani 1 1 d . . . H38A H 0.3405 1.0229 0.4963 0.050 Uiso 1 1 calc R . . H38B H 0.3447 1.1409 0.4923 0.050 Uiso 1 1 calc R . . H38C H 0.4423 1.0767 0.4825 0.050 Uiso 1 1 calc R . . C39 C 0.8924(5) 0.9869(6) 0.3893(3) 0.0264(15) Uani 1 1 d . . . C40 C 0.8678(7) 1.0907(7) 0.3679(3) 0.041(2) Uani 1 1 d . . . H40A H 0.8547 1.0860 0.3313 0.061 Uiso 1 1 calc R . . H40B H 0.9243 1.1351 0.3745 0.061 Uiso 1 1 calc R . . H40C H 0.8088 1.1168 0.3843 0.061 Uiso 1 1 calc R . . C41 C 0.8924(7) 0.9910(7) 0.4475(3) 0.042(2) Uani 1 1 d . . . H41A H 0.8286 1.0174 0.4585 0.063 Uiso 1 1 calc R . . H41B H 0.9466 1.0339 0.4598 0.063 Uiso 1 1 calc R . . H41C H 0.9020 0.9242 0.4612 0.063 Uiso 1 1 calc R . . C42 C 0.9942(6) 0.9555(8) 0.3714(5) 0.056(3) Uani 1 1 d . . . H42A H 1.0106 0.8900 0.3852 0.083 Uiso 1 1 calc R . . H42B H 1.0443 1.0034 0.3832 0.083 Uiso 1 1 calc R . . H42C H 0.9932 0.9527 0.3344 0.083 Uiso 1 1 calc R . . P1 P 0.67204(17) 0.23207(15) 0.47865(7) 0.0295(4) Uani 1 1 d . . . F7 F 0.7561(4) 0.2761(3) 0.44254(19) 0.0448(13) Uani 1 1 d . . . F8 F 0.6504(4) 0.1443(3) 0.43777(17) 0.0346(11) Uani 1 1 d . . . F9 F 0.7538(4) 0.1635(3) 0.50611(18) 0.0358(11) Uani 1 1 d . . . F10 F 0.5889(4) 0.1869(3) 0.51371(17) 0.0338(10) Uani 1 1 d . . . F11 F 0.6937(4) 0.3188(3) 0.51896(18) 0.0427(12) Uani 1 1 d . . . F12 F 0.5887(4) 0.2995(4) 0.44992(18) 0.0419(12) 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 0.02205(16) 0.01632(15) 0.01503(14) -0.00061(10) -0.00040(9) 0.00027(10) F1 0.039(3) 0.044(3) 0.075(4) 0.007(3) 0.034(3) 0.005(2) F2 0.112(6) 0.090(5) 0.047(3) 0.015(3) 0.018(4) 0.080(5) F3 0.050(4) 0.049(4) 0.142(7) -0.056(4) 0.038(4) -0.012(3) F4 0.044(3) 0.030(3) 0.061(3) -0.007(2) -0.005(2) -0.008(2) F5 0.054(4) 0.072(4) 0.032(3) -0.007(3) 0.010(2) -0.034(3) F6 0.025(3) 0.053(3) 0.046(3) -0.001(2) -0.009(2) -0.010(2) N1 0.035(4) 0.011(3) 0.016(3) 0.000(2) -0.005(2) -0.002(2) N2 0.032(3) 0.014(3) 0.015(3) 0.001(2) -0.001(2) 0.008(2) N3 0.020(3) 0.017(3) 0.019(3) 0.001(2) 0.001(2) 0.001(2) N4 0.019(3) 0.020(3) 0.021(3) 0.002(2) 0.003(2) 0.000(2) C1 0.023(4) 0.020(4) 0.028(4) -0.002(3) 0.002(3) 0.002(3) C2 0.053(5) 0.021(4) 0.015(3) -0.002(3) -0.006(3) -0.002(3) C3 0.037(5) 0.026(4) 0.025(4) 0.002(3) -0.013(3) 0.004(3) C4 0.032(4) 0.020(4) 0.026(3) 0.000(3) -0.004(3) 0.006(3) C5 0.024(4) 0.014(3) 0.023(3) -0.001(3) 0.004(3) -0.007(3) C6 0.024(4) 0.023(4) 0.021(3) 0.002(3) 0.001(3) -0.007(3) C7 0.020(4) 0.021(4) 0.027(4) -0.002(3) 0.003(3) -0.005(3) C8 0.026(4) 0.013(3) 0.033(4) 0.000(3) 0.008(3) 0.001(3) C9 0.043(5) 0.020(4) 0.023(3) -0.007(3) 0.007(3) -0.007(3) C10 0.038(5) 0.022(4) 0.018(3) 0.001(3) -0.003(3) 0.002(3) C11 0.024(4) 0.018(3) 0.023(3) -0.004(3) 0.003(3) 0.001(3) C12 0.027(4) 0.013(3) 0.020(3) -0.005(2) 0.005(3) 0.002(3) C13 0.028(4) 0.022(4) 0.018(3) 0.006(3) -0.001(3) 0.002(3) C14 0.031(4) 0.023(4) 0.026(4) 0.001(3) 0.004(3) -0.002(3) C15 0.031(4) 0.023(4) 0.023(3) -0.007(3) 0.008(3) 0.001(3) C16 0.022(4) 0.023(4) 0.016(3) -0.003(3) -0.004(2) -0.004(3) C17 0.025(4) 0.022(4) 0.015(3) -0.002(3) 0.001(3) 0.003(3) C18 0.027(4) 0.024(4) 0.023(3) 0.001(3) -0.002(3) 0.005(3) C19 0.038(4) 0.030(4) 0.018(3) -0.005(3) 0.000(3) 0.005(3) C20 0.026(4) 0.033(4) 0.016(3) -0.001(3) -0.001(3) 0.007(3) C21 0.035(4) 0.031(4) 0.020(3) 0.002(3) 0.007(3) 0.005(3) C22 0.029(4) 0.019(4) 0.032(4) 0.002(3) 0.001(3) -0.001(3) C23 0.036(5) 0.023(4) 0.039(4) 0.000(3) 0.011(3) 0.002(3) C24 0.022(4) 0.036(4) 0.021(3) -0.006(3) -0.004(3) -0.005(3) C25 0.012(3) 0.024(4) 0.021(3) 0.000(3) -0.003(2) 0.001(3) C26 0.019(4) 0.027(4) 0.025(3) 0.000(3) 0.000(3) -0.007(3) C27 0.020(3) 0.019(3) 0.019(3) 0.002(3) -0.003(2) 0.009(3) C28 0.026(4) 0.016(3) 0.031(4) 0.000(3) 0.000(3) -0.002(3) C29 0.022(4) 0.027(4) 0.018(3) 0.000(3) 0.001(2) -0.001(3) C30 0.024(4) 0.020(3) 0.019(3) 0.003(3) 0.000(3) 0.001(3) C31 0.023(4) 0.017(3) 0.020(3) -0.001(3) -0.002(3) 0.001(3) C32 0.024(4) 0.028(4) 0.016(3) 0.000(3) -0.007(3) -0.005(3) C33 0.023(4) 0.032(4) 0.029(4) 0.005(3) 0.002(3) 0.000(3) C34 0.022(4) 0.027(4) 0.025(3) -0.007(3) 0.000(3) 0.001(3) C35 0.015(4) 0.018(3) 0.038(4) -0.003(3) 0.002(3) 0.006(3) C36 0.035(5) 0.027(4) 0.047(5) -0.009(4) 0.006(4) -0.001(3) C37 0.034(5) 0.020(4) 0.041(4) 0.006(3) 0.003(3) 0.005(3) C38 0.041(5) 0.027(4) 0.032(4) -0.006(3) 0.007(3) -0.001(3) C39 0.018(4) 0.032(4) 0.029(4) 0.000(3) -0.004(3) -0.004(3) C40 0.044(5) 0.044(5) 0.033(4) 0.002(4) -0.006(4) -0.008(4) C41 0.039(5) 0.049(5) 0.036(4) -0.004(4) -0.019(4) -0.014(4) C42 0.013(4) 0.063(7) 0.090(8) -0.030(6) 0.006(4) -0.002(4) P1 0.0454(13) 0.0215(10) 0.0218(9) -0.0022(7) 0.0044(8) -0.0018(8) F7 0.065(4) 0.027(3) 0.043(3) 0.002(2) 0.020(2) -0.008(2) F8 0.052(3) 0.023(2) 0.029(2) -0.0078(18) 0.005(2) 0.003(2) F9 0.032(3) 0.037(3) 0.038(3) 0.002(2) 0.001(2) 0.002(2) F10 0.043(3) 0.028(2) 0.031(2) -0.0001(18) 0.002(2) -0.003(2) F11 0.065(4) 0.033(3) 0.031(2) -0.012(2) 0.001(2) -0.011(2) F12 0.067(4) 0.027(2) 0.031(2) 0.004(2) 0.006(2) 0.008(2) _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 C12 2.011(7) . ? Ir1 C11 2.019(7) . ? Ir1 N2 2.050(5) . ? Ir1 N1 2.056(5) . ? Ir1 N3 2.142(6) . ? Ir1 N4 2.143(6) . ? F1 C23 1.337(9) . ? F2 C23 1.321(11) . ? F3 C23 1.328(10) . ? F4 C24 1.369(9) . ? F5 C24 1.348(9) . ? F6 C24 1.340(9) . ? N1 C1 1.367(9) . ? N1 C5 1.369(9) . ? N2 C18 1.355(10) . ? N2 C22 1.361(9) . ? N3 C25 1.340(9) . ? N3 C29 1.361(9) . ? N4 C34 1.349(9) . ? N4 C30 1.354(9) . ? C1 C2 1.385(10) . ? C1 H1 0.9500 . ? C2 C3 1.376(11) . ? C2 H2 0.9500 . ? C3 C4 1.397(10) . ? C3 H3 0.9500 . ? C4 C5 1.393(10) . ? C4 H4 0.9500 . ? C5 C6 1.491(9) . ? C6 C7 1.411(10) . ? C6 C11 1.413(10) . ? C7 C8 1.373(10) . ? C7 H7 0.9500 . ? C8 C9 1.387(11) . ? C8 C23 1.505(10) . ? C9 C10 1.406(11) . ? C9 H9 0.9500 . ? C10 C11 1.405(9) . ? C10 H10 0.9500 . ? C12 C13 1.398(9) . ? C12 C17 1.432(9) . ? C13 C14 1.392(10) . ? C13 H13 0.9500 . ? C14 C15 1.409(10) . ? C14 H14 0.9500 . ? C15 C16 1.377(10) . ? C15 C24 1.501(10) . ? C16 C17 1.398(10) . ? C16 H16 0.9500 . ? C17 C18 1.486(10) . ? C18 C19 1.411(10) . ? C19 C20 1.385(11) . ? C19 H19 0.9500 . ? C20 C21 1.398(11) . ? C20 H20 0.9500 . ? C21 C22 1.373(10) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C25 C26 1.391(10) . ? C25 H25 0.9500 . ? C26 C27 1.400(10) . ? C26 H26 0.9500 . ? C27 C28 1.400(10) . ? C27 C35 1.551(9) . ? C28 C29 1.396(10) . ? C28 H28 0.9500 . ? C29 C30 1.492(10) . ? C30 C31 1.381(10) . ? C31 C32 1.411(10) . ? C31 H31 0.9500 . ? C32 C33 1.403(10) . ? C32 C39 1.544(10) . ? C33 C34 1.374(10) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C37 1.531(10) . ? C35 C38 1.535(11) . ? C35 C36 1.538(11) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C42 1.519(11) . ? C39 C41 1.541(11) . ? C39 C40 1.546(12) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? P1 F10 1.592(5) . ? P1 F9 1.598(5) . ? P1 F11 1.607(5) . ? P1 F7 1.613(5) . ? P1 F12 1.619(6) . ? P1 F8 1.626(5) . ? 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 C12 Ir1 C11 87.7(3) . . ? C12 Ir1 N2 80.5(3) . . ? C11 Ir1 N2 95.3(3) . . ? C12 Ir1 N1 94.6(3) . . ? C11 Ir1 N1 80.2(3) . . ? N2 Ir1 N1 173.5(2) . . ? C12 Ir1 N3 100.4(2) . . ? C11 Ir1 N3 171.9(3) . . ? N2 Ir1 N3 87.2(2) . . ? N1 Ir1 N3 97.9(2) . . ? C12 Ir1 N4 176.6(2) . . ? C11 Ir1 N4 95.7(3) . . ? N2 Ir1 N4 99.4(2) . . ? N1 Ir1 N4 85.7(2) . . ? N3 Ir1 N4 76.3(2) . . ? C1 N1 C5 119.6(6) . . ? C1 N1 Ir1 123.9(5) . . ? C5 N1 Ir1 116.5(4) . . ? C18 N2 C22 120.5(6) . . ? C18 N2 Ir1 115.8(5) . . ? C22 N2 Ir1 123.7(5) . . ? C25 N3 C29 118.9(6) . . ? C25 N3 Ir1 124.7(5) . . ? C29 N3 Ir1 116.3(5) . . ? C34 N4 C30 118.1(6) . . ? C34 N4 Ir1 124.9(5) . . ? C30 N4 Ir1 116.2(4) . . ? N1 C1 C2 120.9(7) . . ? N1 C1 H1 119.6 . . ? C2 C1 H1 119.6 . . ? C3 C2 C1 119.9(7) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 119.7(7) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 119.0(7) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? N1 C5 C4 120.8(6) . . ? N1 C5 C6 113.1(6) . . ? C4 C5 C6 126.0(7) . . ? C7 C6 C11 122.1(6) . . ? C7 C6 C5 123.0(6) . . ? C11 C6 C5 114.9(6) . . ? C8 C7 C6 118.4(7) . . ? C8 C7 H7 120.8 . . ? C6 C7 H7 120.8 . . ? C7 C8 C9 121.5(7) . . ? C7 C8 C23 120.9(7) . . ? C9 C8 C23 117.5(7) . . ? C8 C9 C10 120.0(6) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C11 C10 C9 120.6(7) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C6 117.3(6) . . ? C10 C11 Ir1 127.6(5) . . ? C6 C11 Ir1 115.0(5) . . ? C13 C12 C17 116.3(6) . . ? C13 C12 Ir1 129.0(5) . . ? C17 C12 Ir1 114.7(5) . . ? C14 C13 C12 122.3(6) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? C13 C14 C15 119.2(7) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C16 C15 C14 121.2(7) . . ? C16 C15 C24 119.6(6) . . ? C14 C15 C24 119.2(6) . . ? C15 C16 C17 118.7(6) . . ? C15 C16 H16 120.6 . . ? C17 C16 H16 120.6 . . ? C16 C17 C12 122.3(6) . . ? C16 C17 C18 124.1(6) . . ? C12 C17 C18 113.5(6) . . ? N2 C18 C19 120.2(7) . . ? N2 C18 C17 114.7(6) . . ? C19 C18 C17 125.0(7) . . ? C20 C19 C18 119.9(7) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 117.8(7) . . ? C19 C20 H20 121.1 . . ? C21 C20 H20 121.1 . . ? C22 C21 C20 121.2(7) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? N2 C22 C21 120.3(7) . . ? N2 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? F2 C23 F3 107.2(8) . . ? F2 C23 F1 105.0(8) . . ? F3 C23 F1 104.3(7) . . ? F2 C23 C8 113.3(7) . . ? F3 C23 C8 114.0(7) . . ? F1 C23 C8 112.2(6) . . ? F6 C24 F5 108.3(6) . . ? F6 C24 F4 105.5(6) . . ? F5 C24 F4 104.7(7) . . ? F6 C24 C15 113.3(7) . . ? F5 C24 C15 112.3(6) . . ? F4 C24 C15 112.1(6) . . ? N3 C25 C26 122.1(6) . . ? N3 C25 H25 119.0 . . ? C26 C25 H25 119.0 . . ? C25 C26 C27 120.3(7) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C28 C27 C26 117.1(6) . . ? C28 C27 C35 120.1(6) . . ? C26 C27 C35 122.7(6) . . ? C29 C28 C27 120.0(7) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? N3 C29 C28 121.6(7) . . ? N3 C29 C30 115.2(6) . . ? C28 C29 C30 123.1(7) . . ? N4 C30 C31 121.9(6) . . ? N4 C30 C29 114.9(6) . . ? C31 C30 C29 123.2(6) . . ? C30 C31 C32 120.1(6) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C33 C32 C31 117.1(6) . . ? C33 C32 C39 120.7(7) . . ? C31 C32 C39 122.1(6) . . ? C34 C33 C32 119.4(7) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? N4 C34 C33 123.3(7) . . ? N4 C34 H34 118.3 . . ? C33 C34 H34 118.3 . . ? C37 C35 C38 110.6(6) . . ? C37 C35 C36 107.3(6) . . ? C38 C35 C36 108.9(6) . . ? C37 C35 C27 109.8(6) . . ? C38 C35 C27 108.1(6) . . ? C36 C35 C27 112.2(6) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C42 C39 C41 110.2(7) . . ? C42 C39 C32 112.8(7) . . ? C41 C39 C32 107.9(6) . . ? C42 C39 C40 109.0(7) . . ? C41 C39 C40 109.1(7) . . ? C32 C39 C40 107.7(6) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? F10 P1 F9 89.9(3) . . ? F10 P1 F11 90.6(3) . . ? F9 P1 F11 90.7(3) . . ? F10 P1 F7 179.0(3) . . ? F9 P1 F7 90.0(3) . . ? F11 P1 F7 90.3(3) . . ? F10 P1 F12 90.1(3) . . ? F9 P1 F12 178.7(3) . . ? F11 P1 F12 90.6(3) . . ? F7 P1 F12 90.0(3) . . ? F10 P1 F8 89.5(3) . . ? F9 P1 F8 89.3(3) . . ? F11 P1 F8 179.8(3) . . ? F7 P1 F8 89.5(3) . . ? F12 P1 F8 89.4(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 C12 Ir1 N1 C1 -88.4(6) . . . . ? C11 Ir1 N1 C1 -175.2(6) . . . . ? N3 Ir1 N1 C1 12.8(6) . . . . ? N4 Ir1 N1 C1 88.3(6) . . . . ? C12 Ir1 N1 C5 91.8(5) . . . . ? C11 Ir1 N1 C5 5.0(5) . . . . ? N3 Ir1 N1 C5 -167.0(5) . . . . ? N4 Ir1 N1 C5 -91.5(5) . . . . ? C12 Ir1 N2 C18 -8.1(5) . . . . ? C11 Ir1 N2 C18 78.7(5) . . . . ? N3 Ir1 N2 C18 -109.1(5) . . . . ? N4 Ir1 N2 C18 175.3(5) . . . . ? C12 Ir1 N2 C22 174.3(6) . . . . ? C11 Ir1 N2 C22 -99.0(6) . . . . ? N3 Ir1 N2 C22 73.2(6) . . . . ? N4 Ir1 N2 C22 -2.3(6) . . . . ? C12 Ir1 N3 C25 -9.9(6) . . . . ? N2 Ir1 N3 C25 69.9(5) . . . . ? N1 Ir1 N3 C25 -106.1(5) . . . . ? N4 Ir1 N3 C25 170.3(6) . . . . ? C12 Ir1 N3 C29 174.8(5) . . . . ? N2 Ir1 N3 C29 -105.3(5) . . . . ? N1 Ir1 N3 C29 78.7(5) . . . . ? N4 Ir1 N3 C29 -4.9(5) . . . . ? C11 Ir1 N4 C34 0.0(6) . . . . ? N2 Ir1 N4 C34 -96.3(6) . . . . ? N1 Ir1 N4 C34 79.7(6) . . . . ? N3 Ir1 N4 C34 178.9(6) . . . . ? C11 Ir1 N4 C30 -169.4(5) . . . . ? N2 Ir1 N4 C30 94.2(5) . . . . ? N1 Ir1 N4 C30 -89.8(5) . . . . ? N3 Ir1 N4 C30 9.5(5) . . . . ? C5 N1 C1 C2 1.4(10) . . . . ? Ir1 N1 C1 C2 -178.4(5) . . . . ? N1 C1 C2 C3 -0.2(12) . . . . ? C1 C2 C3 C4 0.1(12) . . . . ? C2 C3 C4 C5 -1.1(12) . . . . ? C1 N1 C5 C4 -2.4(10) . . . . ? Ir1 N1 C5 C4 177.4(5) . . . . ? C1 N1 C5 C6 176.1(6) . . . . ? Ir1 N1 C5 C6 -4.1(7) . . . . ? C3 C4 C5 N1 2.3(11) . . . . ? C3 C4 C5 C6 -176.0(7) . . . . ? N1 C5 C6 C7 178.1(6) . . . . ? C4 C5 C6 C7 -3.5(11) . . . . ? N1 C5 C6 C11 0.1(9) . . . . ? C4 C5 C6 C11 178.5(7) . . . . ? C11 C6 C7 C8 -1.7(10) . . . . ? C5 C6 C7 C8 -179.6(6) . . . . ? C6 C7 C8 C9 1.0(11) . . . . ? C6 C7 C8 C23 -179.0(7) . . . . ? C7 C8 C9 C10 -0.9(11) . . . . ? C23 C8 C9 C10 179.1(7) . . . . ? C8 C9 C10 C11 1.5(11) . . . . ? C9 C10 C11 C6 -2.1(11) . . . . ? C9 C10 C11 Ir1 173.6(6) . . . . ? C7 C6 C11 C10 2.2(10) . . . . ? C5 C6 C11 C10 -179.7(6) . . . . ? C7 C6 C11 Ir1 -174.0(5) . . . . ? C5 C6 C11 Ir1 4.0(8) . . . . ? C12 Ir1 C11 C10 84.4(7) . . . . ? N2 Ir1 C11 C10 4.1(7) . . . . ? N1 Ir1 C11 C10 179.5(7) . . . . ? N4 Ir1 C11 C10 -95.9(7) . . . . ? C12 Ir1 C11 C6 -99.8(6) . . . . ? N2 Ir1 C11 C6 179.9(5) . . . . ? N1 Ir1 C11 C6 -4.8(5) . . . . ? N4 Ir1 C11 C6 79.9(5) . . . . ? C11 Ir1 C12 C13 91.1(6) . . . . ? N2 Ir1 C12 C13 -173.1(7) . . . . ? N1 Ir1 C12 C13 11.2(6) . . . . ? N3 Ir1 C12 C13 -87.8(6) . . . . ? C11 Ir1 C12 C17 -88.1(5) . . . . ? N2 Ir1 C12 C17 7.7(5) . . . . ? N1 Ir1 C12 C17 -168.0(5) . . . . ? N3 Ir1 C12 C17 93.1(5) . . . . ? C17 C12 C13 C14 2.1(10) . . . . ? Ir1 C12 C13 C14 -177.0(5) . . . . ? C12 C13 C14 C15 -0.2(11) . . . . ? C13 C14 C15 C16 -1.2(11) . . . . ? C13 C14 C15 C24 176.5(7) . . . . ? C14 C15 C16 C17 0.5(11) . . . . ? C24 C15 C16 C17 -177.2(7) . . . . ? C15 C16 C17 C12 1.6(10) . . . . ? C15 C16 C17 C18 -175.3(6) . . . . ? C13 C12 C17 C16 -2.8(10) . . . . ? Ir1 C12 C17 C16 176.4(5) . . . . ? C13 C12 C17 C18 174.3(6) . . . . ? Ir1 C12 C17 C18 -6.4(8) . . . . ? C22 N2 C18 C19 0.2(10) . . . . ? Ir1 N2 C18 C19 -177.6(5) . . . . ? C22 N2 C18 C17 -175.5(6) . . . . ? Ir1 N2 C18 C17 6.8(8) . . . . ? C16 C17 C18 N2 176.8(6) . . . . ? C12 C17 C18 N2 -0.3(9) . . . . ? C16 C17 C18 C19 1.4(11) . . . . ? C12 C17 C18 C19 -175.7(7) . . . . ? N2 C18 C19 C20 -1.9(11) . . . . ? C17 C18 C19 C20 173.3(7) . . . . ? C18 C19 C20 C21 2.0(11) . . . . ? C19 C20 C21 C22 -0.4(11) . . . . ? C18 N2 C22 C21 1.5(10) . . . . ? Ir1 N2 C22 C21 179.0(5) . . . . ? C20 C21 C22 N2 -1.3(11) . . . . ? C7 C8 C23 F2 -2.4(11) . . . . ? C9 C8 C23 F2 177.6(8) . . . . ? C7 C8 C23 F3 120.5(9) . . . . ? C9 C8 C23 F3 -59.4(10) . . . . ? C7 C8 C23 F1 -121.1(8) . . . . ? C9 C8 C23 F1 58.9(10) . . . . ? C16 C15 C24 F6 -29.0(10) . . . . ? C14 C15 C24 F6 153.2(7) . . . . ? C16 C15 C24 F5 -152.1(7) . . . . ? C14 C15 C24 F5 30.1(10) . . . . ? C16 C15 C24 F4 90.3(8) . . . . ? C14 C15 C24 F4 -87.5(8) . . . . ? C29 N3 C25 C26 -1.9(10) . . . . ? Ir1 N3 C25 C26 -177.1(5) . . . . ? N3 C25 C26 C27 0.4(10) . . . . ? C25 C26 C27 C28 1.4(10) . . . . ? C25 C26 C27 C35 -177.1(6) . . . . ? C26 C27 C28 C29 -1.6(10) . . . . ? C35 C27 C28 C29 176.9(6) . . . . ? C25 N3 C29 C28 1.7(10) . . . . ? Ir1 N3 C29 C28 177.2(5) . . . . ? C25 N3 C29 C30 -175.3(6) . . . . ? Ir1 N3 C29 C30 0.2(7) . . . . ? C27 C28 C29 N3 0.1(10) . . . . ? C27 C28 C29 C30 176.9(6) . . . . ? C34 N4 C30 C31 -3.2(10) . . . . ? Ir1 N4 C30 C31 167.0(5) . . . . ? C34 N4 C30 C29 177.6(6) . . . . ? Ir1 N4 C30 C29 -12.3(7) . . . . ? N3 C29 C30 N4 7.9(9) . . . . ? C28 C29 C30 N4 -169.0(6) . . . . ? N3 C29 C30 C31 -171.3(6) . . . . ? C28 C29 C30 C31 11.7(10) . . . . ? N4 C30 C31 C32 1.9(10) . . . . ? C29 C30 C31 C32 -178.9(6) . . . . ? C30 C31 C32 C33 -0.1(10) . . . . ? C30 C31 C32 C39 -177.3(6) . . . . ? C31 C32 C33 C34 -0.3(10) . . . . ? C39 C32 C33 C34 177.0(7) . . . . ? C30 N4 C34 C33 2.8(10) . . . . ? Ir1 N4 C34 C33 -166.4(6) . . . . ? C32 C33 C34 N4 -1.1(11) . . . . ? C28 C27 C35 C37 49.7(9) . . . . ? C26 C27 C35 C37 -131.9(7) . . . . ? C28 C27 C35 C38 -71.1(8) . . . . ? C26 C27 C35 C38 107.4(7) . . . . ? C28 C27 C35 C36 168.9(6) . . . . ? C26 C27 C35 C36 -12.7(10) . . . . ? C33 C32 C39 C42 4.4(10) . . . . ? C31 C32 C39 C42 -178.5(8) . . . . ? C33 C32 C39 C41 -117.5(8) . . . . ? C31 C32 C39 C41 59.6(9) . . . . ? C33 C32 C39 C40 124.8(7) . . . . ? C31 C32 C39 C40 -58.1(9) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 4.247 _refine_diff_density_min -2.262 _refine_diff_density_rms 0.210 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 550 153 ' ' 2 0.000 0.500 0.500 550 155 ' ' _platon_squeeze_details ; ; _iucr_refine_instructions_details ; TITL NS-52 in P2(1)/c CELL 0.71073 13.4399 13.5222 26.4480 90.0000 91.5258 90.0000 ZERR 4.00 0.0027 0.0013 0.0058 0.0000 0.0160 0.0000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N F P IR UNIT 168 152 16 48 4 4 REM ---------------------------------------------------------- REM Data collection: Bruker APEX II CCD REM Absorption correction: SADABS REM Crystal habit: platelet; Crystal colour: yellow REM Mole 1 is the Ir(III) cationic complex REM Mole 2 is the PF6 anion REM About 2 DCM molecules were highly disordered and squeezed REM ---------------------------------------------------------- L.S. 10 ACTA CONF SIZE 0.452 0.398 0.066 BOND $H WPDB -2 FMAP 2 PLAN 10 TEMP -173 WGHT 0.088200 20.675400 FVAR 2.06903 IR1 6 0.543717 0.671134 0.337772 11.00000 0.02205 0.01632 = 0.01503 -0.00061 -0.00040 0.00027 F1 4 0.914871 0.376707 0.241100 11.00000 0.03917 0.04383 = 0.07480 0.00665 0.03415 0.00502 F2 4 0.900731 0.304688 0.311289 11.00000 0.11170 0.08970 = 0.04659 0.01496 0.01800 0.08026 F3 4 0.807969 0.264134 0.247992 11.00000 0.04960 0.04894 = 0.14185 -0.05560 0.03767 -0.01194 F4 4 0.230939 0.277145 0.287930 11.00000 0.04408 0.03004 = 0.06136 -0.00748 -0.00468 -0.00846 F5 4 0.142251 0.341574 0.345886 11.00000 0.05435 0.07158 = 0.03232 -0.00697 0.01038 -0.03413 F6 4 0.126662 0.392856 0.267987 11.00000 0.02510 0.05289 = 0.04614 -0.00142 -0.00856 -0.00968 N1 3 0.601118 0.618421 0.405397 11.00000 0.03497 0.01104 = 0.01625 -0.00013 -0.00522 -0.00179 N2 3 0.483749 0.707281 0.268132 11.00000 0.03178 0.01430 = 0.01547 0.00140 -0.00098 0.00817 N3 3 0.469522 0.798683 0.366514 11.00000 0.02044 0.01679 = 0.01898 0.00126 0.00100 0.00096 N4 3 0.658979 0.780440 0.343376 11.00000 0.01938 0.02029 = 0.02142 0.00220 0.00276 -0.00041 C1 1 0.572481 0.651413 0.451662 11.00000 0.02314 0.02022 = 0.02790 -0.00181 0.00157 0.00166 AFIX 43 H1 2 0.522056 0.700403 0.453568 11.00000 -1.20000 AFIX 0 C2 1 0.616008 0.614363 0.495800 11.00000 0.05331 0.02062 = 0.01545 -0.00198 -0.00630 -0.00246 AFIX 43 H2 2 0.595601 0.638084 0.527705 11.00000 -1.20000 AFIX 0 C3 1 0.688829 0.543165 0.493339 11.00000 0.03732 0.02615 = 0.02464 0.00193 -0.01336 0.00375 AFIX 43 H3 2 0.718809 0.517537 0.523520 11.00000 -1.20000 AFIX 0 C4 1 0.718530 0.508687 0.446276 11.00000 0.03158 0.01957 = 0.02564 -0.00008 -0.00423 0.00627 AFIX 43 H4 2 0.769518 0.460338 0.444083 11.00000 -1.20000 AFIX 0 C5 1 0.672231 0.546293 0.402620 11.00000 0.02414 0.01414 = 0.02279 -0.00138 0.00408 -0.00676 C6 1 0.690219 0.513556 0.349801 11.00000 0.02407 0.02324 = 0.02074 0.00183 0.00094 -0.00695 C7 1 0.762265 0.442035 0.337736 11.00000 0.01971 0.02119 = 0.02749 -0.00189 0.00279 -0.00459 AFIX 43 H7 2 0.802104 0.411579 0.363538 11.00000 -1.20000 AFIX 0 C8 1 0.773436 0.417499 0.287851 11.00000 0.02612 0.01279 = 0.03296 0.00039 0.00786 0.00131 C9 1 0.716961 0.462266 0.249642 11.00000 0.04290 0.01952 = 0.02319 -0.00651 0.00684 -0.00748 AFIX 43 H9 2 0.726681 0.444710 0.215346 11.00000 -1.20000 AFIX 0 C10 1 0.645290 0.533667 0.261684 11.00000 0.03801 0.02193 = 0.01837 0.00089 -0.00287 0.00213 AFIX 43 H10 2 0.605700 0.563034 0.235452 11.00000 -1.20000 AFIX 0 C11 1 0.631679 0.561988 0.312159 11.00000 0.02389 0.01782 = 0.02325 -0.00358 0.00337 0.00087 C12 1 0.430184 0.574318 0.334361 11.00000 0.02705 0.01326 = 0.01959 -0.00486 0.00470 0.00212 C13 1 0.396608 0.510445 0.371815 11.00000 0.02805 0.02242 = 0.01810 0.00598 -0.00111 0.00204 AFIX 43 H13 2 0.427803 0.512509 0.404455 11.00000 -1.20000 AFIX 0 C14 1 0.319029 0.443915 0.362930 11.00000 0.03113 0.02336 = 0.02575 0.00078 0.00351 -0.00192 AFIX 43 H14 2 0.297919 0.401242 0.389087 11.00000 -1.20000 AFIX 0 C15 1 0.272236 0.440688 0.314655 11.00000 0.03094 0.02269 = 0.02263 -0.00678 0.00803 0.00076 C16 1 0.300690 0.503286 0.276580 11.00000 0.02179 0.02264 = 0.01620 -0.00317 -0.00381 -0.00427 AFIX 43 H16 2 0.268382 0.501000 0.244213 11.00000 -1.20000 AFIX 0 C17 1 0.378032 0.570252 0.286486 11.00000 0.02532 0.02212 = 0.01546 -0.00218 0.00082 0.00271 C18 1 0.410830 0.646614 0.250114 11.00000 0.02704 0.02361 = 0.02293 0.00129 -0.00246 0.00534 C19 1 0.367330 0.662885 0.201674 11.00000 0.03795 0.03032 = 0.01844 -0.00530 -0.00007 0.00480 AFIX 43 H19 2 0.317638 0.619064 0.188710 11.00000 -1.20000 AFIX 0 C20 1 0.397180 0.742827 0.173057 11.00000 0.02567 0.03340 = 0.01601 -0.00095 -0.00103 0.00694 AFIX 43 H20 2 0.367271 0.756147 0.140825 11.00000 -1.20000 AFIX 0 C21 1 0.472799 0.803285 0.193179 11.00000 0.03476 0.03150 = 0.02011 0.00186 0.00715 0.00525 AFIX 43 H21 2 0.494885 0.858323 0.174177 11.00000 -1.20000 AFIX 0 C22 1 0.515702 0.784561 0.239884 11.00000 0.02919 0.01924 = 0.03243 0.00217 0.00063 -0.00140 AFIX 43 H22 2 0.567936 0.825743 0.252541 11.00000 -1.20000 AFIX 0 C23 1 0.847841 0.340584 0.272654 11.00000 0.03613 0.02298 = 0.03905 -0.00015 0.01136 0.00212 C24 1 0.192558 0.365075 0.304142 11.00000 0.02151 0.03604 = 0.02149 -0.00553 -0.00351 -0.00483 C25 1 0.370779 0.806986 0.370850 11.00000 0.01189 0.02358 = 0.02145 0.00024 -0.00313 0.00073 AFIX 43 H25 2 0.329713 0.752061 0.362143 11.00000 -1.20000 AFIX 0 C26 1 0.326485 0.893475 0.387696 11.00000 0.01929 0.02679 = 0.02483 -0.00034 -0.00045 -0.00713 AFIX 43 H26 2 0.256234 0.896649 0.390496 11.00000 -1.20000 AFIX 0 C27 1 0.384958 0.975882 0.400546 11.00000 0.02009 0.01919 = 0.01895 0.00192 -0.00315 0.00929 C28 1 0.487755 0.967285 0.394524 11.00000 0.02578 0.01611 = 0.03051 0.00028 0.00039 -0.00167 AFIX 43 H28 2 0.530142 1.021897 0.401952 11.00000 -1.20000 AFIX 0 C29 1 0.527981 0.878407 0.377595 11.00000 0.02187 0.02699 = 0.01762 -0.00009 0.00089 -0.00110 C30 1 0.635929 0.865075 0.367788 11.00000 0.02377 0.01991 = 0.01914 0.00299 0.00038 0.00070 C31 1 0.707914 0.932684 0.382766 11.00000 0.02319 0.01675 = 0.01995 -0.00106 -0.00192 0.00100 AFIX 43 H31 2 0.689654 0.990465 0.400725 11.00000 -1.20000 AFIX 0 C32 1 0.808527 0.916022 0.371425 11.00000 0.02400 0.02807 = 0.01607 -0.00007 -0.00664 -0.00481 C33 1 0.830449 0.829188 0.344899 11.00000 0.02323 0.03199 = 0.02879 0.00512 0.00184 0.00029 AFIX 43 H33 2 0.897042 0.814749 0.336241 11.00000 -1.20000 AFIX 0 C34 1 0.754813 0.765235 0.331556 11.00000 0.02163 0.02720 = 0.02461 -0.00697 0.00022 0.00098 AFIX 43 H34 2 0.770781 0.707386 0.313074 11.00000 -1.20000 AFIX 0 C35 1 0.340553 1.072618 0.421902 11.00000 0.01544 0.01780 = 0.03807 -0.00335 0.00184 0.00607 C36 1 0.226436 1.075592 0.416050 11.00000 0.03535 0.02651 = 0.04686 -0.00929 0.00570 -0.00052 AFIX 33 H36A 2 0.197222 1.030214 0.440443 11.00000 -1.50000 H36B 2 0.206510 1.055508 0.381647 11.00000 -1.50000 H36C 2 0.202859 1.142950 0.422330 11.00000 -1.50000 AFIX 0 C37 1 0.381137 1.161733 0.393317 11.00000 0.03440 0.02039 = 0.04128 0.00552 0.00336 0.00458 AFIX 33 H37A 2 0.348632 1.222152 0.404964 11.00000 -1.50000 H37B 2 0.367650 1.153264 0.356978 11.00000 -1.50000 H37C 2 0.453114 1.166836 0.399708 11.00000 -1.50000 AFIX 0 C38 1 0.369633 1.078848 0.478346 11.00000 0.04084 0.02721 = 0.03222 -0.00587 0.00666 -0.00110 AFIX 33 H38A 2 0.340473 1.022911 0.496273 11.00000 -1.50000 H38B 2 0.344705 1.140927 0.492335 11.00000 -1.50000 H38C 2 0.442283 1.076681 0.482458 11.00000 -1.50000 AFIX 0 C39 1 0.892428 0.986910 0.389277 11.00000 0.01794 0.03209 = 0.02895 -0.00023 -0.00369 -0.00405 C40 1 0.867815 1.090695 0.367874 11.00000 0.04355 0.04436 = 0.03341 0.00176 -0.00637 -0.00781 AFIX 33 H40A 2 0.854699 1.085986 0.331326 11.00000 -1.50000 H40B 2 0.924345 1.135059 0.374461 11.00000 -1.50000 H40C 2 0.808797 1.116837 0.384266 11.00000 -1.50000 AFIX 0 C41 1 0.892405 0.990982 0.447517 11.00000 0.03889 0.04891 = 0.03628 -0.00421 -0.01945 -0.01357 AFIX 33 H41A 2 0.828623 1.017392 0.458524 11.00000 -1.50000 H41B 2 0.946571 1.033913 0.459830 11.00000 -1.50000 H41C 2 0.902006 0.924230 0.461227 11.00000 -1.50000 AFIX 0 C42 1 0.994153 0.955468 0.371434 11.00000 0.01334 0.06329 = 0.09035 -0.02974 0.00581 -0.00239 AFIX 33 H42A 2 1.010567 0.889987 0.385171 11.00000 -1.50000 H42B 2 1.044314 1.003389 0.383222 11.00000 -1.50000 H42C 2 0.993213 0.952739 0.334397 11.00000 -1.50000 AFIX 0 P1 5 0.672045 0.232068 0.478648 11.00000 0.04542 0.02145 = 0.02185 -0.00218 0.00438 -0.00180 F7 4 0.756087 0.276140 0.442542 11.00000 0.06527 0.02707 = 0.04314 0.00166 0.02039 -0.00818 F8 4 0.650418 0.144345 0.437770 11.00000 0.05229 0.02281 = 0.02890 -0.00782 0.00459 0.00267 F9 4 0.753850 0.163476 0.506109 11.00000 0.03232 0.03651 = 0.03844 0.00206 0.00120 0.00247 F10 4 0.588939 0.186911 0.513708 11.00000 0.04307 0.02778 = 0.03066 -0.00006 0.00198 -0.00257 F11 4 0.693708 0.318820 0.518964 11.00000 0.06475 0.03274 = 0.03072 -0.01232 0.00146 -0.01068 F12 4 0.588681 0.299550 0.449920 11.00000 0.06734 0.02725 = 0.03127 0.00409 0.00559 0.00840 HKLF 4 REM NS-52 in P2(1)/c REM R1 = 0.0629 for 8408 Fo > 4sig(Fo) and 0.0829 for all 10899 data REM 541 parameters refined using 0 restraints END WGHT 0.0881 20.6300 REM Highest difference peak 4.247, deepest hole -2.262, 1-sigma level 0.210 Q1 1 0.6112 0.6704 0.3378 11.00000 0.05 4.25 Q2 1 0.4763 0.6720 0.3361 11.00000 0.05 3.73 Q3 1 0.5380 0.6431 0.3075 11.00000 0.05 1.49 Q4 1 0.5492 0.6582 0.3701 11.00000 0.05 1.11 Q5 1 0.5108 0.9887 0.3415 11.00000 0.05 1.07 Q6 1 0.5503 0.6993 0.3639 11.00000 0.05 1.00 Q7 1 0.4783 0.6172 0.3591 11.00000 0.05 0.97 Q8 1 0.5805 0.9851 0.3338 11.00000 0.05 0.97 Q9 1 0.5608 0.1762 0.5097 11.00000 0.05 0.96 Q10 1 0.6250 0.6815 0.3868 11.00000 0.05 0.94 ;