# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Dr Paul Newman' _publ_contact_author_email newmanp1@cardiff.ac.uk loop_ _publ_author_name P.Newman K.Cavell data_cmpd2_DT_ART_04_2011_010582 _database_code_depnum_ccdc_archive 'CCDC 820461' #TrackingRef 'cmpd2_kjc1105.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H38 N4 Rh, P F6' _chemical_formula_sum 'C29 H38 F6 N4 P Rh' _chemical_formula_weight 690.51 _chemical_absolute_configuration ad 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 11.9244(5) _cell_length_b 14.2882(3) _cell_length_c 16.8801(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2876.00(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6039 _cell_measurement_theta_min 2.09 _cell_measurement_theta_max 28.30 _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 0.716 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.7878 _exptl_absorpt_correction_T_max 0.9319 _exptl_absorpt_process_details Denzo/Scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6979 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 28.30 _reflns_number_total 6979 _reflns_number_gt 6039 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'cOLLECT,Nonius BV, 1997-2001' _computing_cell_refinement DENZO/SCALEPACK _computing_data_reduction DENZO/SCALEPACK _computing_structure_solution SHELXs-97 _computing_structure_refinement SHELXL-97 _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^)+(0.0672P)^2^+18.4844P] 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 SHELXL _refine_ls_extinction_coef 0.0200(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(6) _refine_ls_number_reflns 6979 _refine_ls_number_parameters 374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0925 _refine_ls_R_factor_gt 0.0790 _refine_ls_wR_factor_ref 0.1884 _refine_ls_wR_factor_gt 0.1765 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 C1 C 0.0001(7) 0.9772(6) 0.9737(5) 0.0386(16) Uani 1 1 d . . . H1 H -0.0228 0.9584 0.9222 0.046 Uiso 1 1 calc R . . C2 C -0.0820(7) 1.0110(6) 1.0252(5) 0.047(2) Uani 1 1 d . . . H2 H -0.1577 1.0174 1.0085 0.056 Uiso 1 1 calc R . . C3 C -0.0496(7) 1.0347(6) 1.1011(5) 0.046(2) Uani 1 1 d . . . H3 H -0.1025 1.0581 1.1382 0.056 Uiso 1 1 calc R . . C4 C 0.0609(8) 1.0237(7) 1.1216(5) 0.047(2) Uani 1 1 d . . . H4 H 0.0847 1.0385 1.1738 0.056 Uiso 1 1 calc R . . C5 C 0.1383(7) 0.9910(5) 1.0667(5) 0.0379(17) Uani 1 1 d . . . C6 C 0.2577(7) 0.9724(5) 1.0896(4) 0.0419(15) Uani 1 1 d . . . H6A H 0.2686 0.9895 1.1459 0.050 Uiso 1 1 calc R . . H6B H 0.2734 0.9047 1.0840 0.050 Uiso 1 1 calc R . . C7 C 0.3415(6) 1.0128(5) 0.9626(5) 0.0335(15) Uani 1 1 d . . . C8 C 0.4096(6) 1.0950(6) 1.0810(5) 0.0431(17) Uani 1 1 d . . . H8 H 0.3806 1.1109 1.1349 0.052 Uiso 1 1 calc R . . C9 C 0.4213(8) 1.1798(6) 1.0293(6) 0.048(2) Uani 1 1 d . . . C10 C 0.4859(7) 1.1375(6) 0.9598(5) 0.0428(18) Uani 1 1 d . . . C11 C 0.5809(6) 1.0801(6) 1.0038(5) 0.0430(17) Uani 1 1 d . . . H11A H 0.6013 1.0235 0.9732 0.052 Uiso 1 1 calc R . . H11B H 0.6489 1.1189 1.0113 0.052 Uiso 1 1 calc R . . C12 C 0.5294(8) 1.0535(8) 1.0836(7) 0.061(3) Uani 1 1 d . . . H12A H 0.5730 1.0808 1.1278 0.074 Uiso 1 1 calc R . . H12B H 0.5269 0.9847 1.0900 0.074 Uiso 1 1 calc R . . C13 C 0.3102(8) 1.2220(7) 1.0051(8) 0.061(3) Uani 1 1 d . . . H13A H 0.2570 1.1718 0.9927 0.091 Uiso 1 1 calc R . . H13B H 0.3209 1.2615 0.9583 0.091 Uiso 1 1 calc R . . H13C H 0.2806 1.2599 1.0488 0.091 Uiso 1 1 calc R . . C14 C 0.4901(9) 1.2570(7) 1.0713(6) 0.062(3) Uani 1 1 d . . . H14A H 0.4579 1.2693 1.1236 0.093 Uiso 1 1 calc R . . H14B H 0.4881 1.3144 1.0395 0.093 Uiso 1 1 calc R . . H14C H 0.5680 1.2362 1.0772 0.093 Uiso 1 1 calc R . . C15 C 0.5313(7) 1.2063(7) 0.9004(5) 0.048(2) Uani 1 1 d . . . H15A H 0.4689 1.2377 0.8735 0.073 Uiso 1 1 calc R . . H15B H 0.5771 1.1731 0.8612 0.073 Uiso 1 1 calc R . . H15C H 0.5776 1.2530 0.9276 0.073 Uiso 1 1 calc R . . C16 C 0.3988(7) 1.0601(7) 0.8323(5) 0.047(2) Uani 1 1 d . . . H16A H 0.4573 1.0998 0.8077 0.056 Uiso 1 1 calc R . . H16B H 0.4133 0.9946 0.8163 0.056 Uiso 1 1 calc R . . C17 C 0.2872(6) 1.0891(6) 0.8013(5) 0.0409(17) Uani 1 1 d . . . C18 C 0.2729(8) 1.1694(6) 0.7588(5) 0.051(2) Uani 1 1 d . . . H18 H 0.3345 1.2095 0.7479 0.062 Uiso 1 1 calc R . . C19 C 0.1638(9) 1.1914(6) 0.7315(5) 0.053(2) Uani 1 1 d . . . H19 H 0.1507 1.2467 0.7016 0.064 Uiso 1 1 calc R . . C20 C 0.0786(7) 1.1324(6) 0.7486(5) 0.0412(18) Uani 1 1 d . . . H20 H 0.0050 1.1452 0.7299 0.049 Uiso 1 1 calc R . . C21 C 0.0992(7) 1.0523(6) 0.7941(5) 0.0386(17) Uani 1 1 d . . . H21 H 0.0388 1.0113 0.8057 0.046 Uiso 1 1 calc R . . C22 C 0.3455(9) 0.8116(6) 0.9630(6) 0.056(3) Uani 1 1 d . . . H22 H 0.3613 0.8579 1.0019 0.067 Uiso 1 1 calc R . . C23 C 0.3836(8) 0.8313(7) 0.8851(6) 0.051(2) Uani 1 1 d . . . H23 H 0.4220 0.8886 0.8761 0.061 Uiso 1 1 calc R . . C24 C 0.3664(9) 0.7660(7) 0.8158(7) 0.066(3) Uani 1 1 d . . . H24A H 0.4286 0.7753 0.7778 0.080 Uiso 1 1 calc R . . H24B H 0.3710 0.7008 0.8353 0.080 Uiso 1 1 calc R . . C25 C 0.2568(9) 0.7782(6) 0.7723(5) 0.054(2) Uani 1 1 d . . . H25A H 0.2333 0.7168 0.7507 0.065 Uiso 1 1 calc R . . H25B H 0.2687 0.8211 0.7271 0.065 Uiso 1 1 calc R . . C26 C 0.1637(7) 0.8165(5) 0.8236(5) 0.0430(19) Uani 1 1 d . . . H26 H 0.1215 0.8674 0.8031 0.052 Uiso 1 1 calc R . . C27 C 0.1350(9) 0.7844(6) 0.8963(6) 0.055(2) Uani 1 1 d . . . H27 H 0.0783 0.8173 0.9243 0.067 Uiso 1 1 calc R . . C28 C 0.1871(12) 0.6990(7) 0.9370(8) 0.079(4) Uani 1 1 d . . . H28A H 0.1287 0.6662 0.9681 0.095 Uiso 1 1 calc R . . H28B H 0.2153 0.6552 0.8962 0.095 Uiso 1 1 calc R . . C29 C 0.2830(11) 0.7265(7) 0.9916(8) 0.078(4) Uani 1 1 d . . . H29A H 0.2528 0.7390 1.0452 0.094 Uiso 1 1 calc R . . H29B H 0.3360 0.6734 0.9958 0.094 Uiso 1 1 calc R . . N1 N 0.1099(5) 0.9694(4) 0.9922(4) 0.0343(13) Uani 1 1 d . . . N2 N 0.3384(5) 1.0259(5) 1.0402(4) 0.0385(14) Uani 1 1 d . . . N3 N 0.4084(5) 1.0674(5) 0.9204(4) 0.0389(14) Uani 1 1 d . . . N4 N 0.2018(5) 1.0318(5) 0.8216(3) 0.0331(13) Uani 1 1 d . . . F1 F -0.1304(4) 0.9164(4) 0.8074(4) 0.0681(16) Uani 1 1 d . . . F2 F -0.1961(7) 1.0543(5) 0.8492(5) 0.097(3) Uani 1 1 d . . . F3 F -0.3536(5) 1.0325(5) 0.7830(5) 0.089(2) Uani 1 1 d . . . F4 F -0.2881(7) 0.8928(5) 0.7420(6) 0.119(4) Uani 1 1 d . . . F5 F -0.1937(8) 1.0244(6) 0.7225(5) 0.119(4) Uani 1 1 d . . . F6 F -0.2892(9) 0.9245(7) 0.8700(7) 0.148(5) Uani 1 1 d . . . P1 P -0.2432(2) 0.97408(13) 0.79520(11) 0.0386(4) Uani 1 1 d . . . Rh1 Rh 0.24454(5) 0.91482(3) 0.91176(3) 0.03511(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.042(4) 0.034(4) 0.040(4) 0.002(3) 0.009(3) -0.005(3) C2 0.042(4) 0.051(5) 0.046(5) 0.009(4) 0.011(4) -0.001(4) C3 0.048(5) 0.048(5) 0.043(5) -0.003(4) 0.020(4) 0.002(4) C4 0.061(5) 0.051(5) 0.028(4) 0.000(3) 0.011(4) -0.011(4) C5 0.041(4) 0.035(4) 0.037(4) 0.006(3) 0.008(3) -0.003(3) C6 0.048(4) 0.043(4) 0.034(3) -0.002(3) -0.012(4) 0.003(4) C7 0.029(3) 0.031(4) 0.041(4) -0.009(3) -0.002(3) 0.003(3) C8 0.043(4) 0.054(5) 0.033(4) -0.014(4) 0.000(3) -0.010(4) C9 0.050(5) 0.043(5) 0.051(5) -0.009(4) -0.003(4) -0.002(4) C10 0.034(4) 0.051(5) 0.043(4) -0.002(4) 0.000(3) -0.006(3) C11 0.036(4) 0.045(4) 0.048(4) -0.012(4) -0.001(3) 0.002(4) C12 0.053(5) 0.073(7) 0.058(6) 0.006(5) -0.029(5) -0.004(4) C13 0.041(5) 0.038(5) 0.104(8) -0.009(5) -0.003(5) 0.008(4) C14 0.068(6) 0.054(6) 0.064(7) -0.027(5) -0.016(5) 0.004(5) C15 0.045(4) 0.056(5) 0.045(5) -0.005(4) 0.000(4) -0.014(4) C16 0.037(4) 0.066(6) 0.038(4) -0.020(4) 0.015(3) -0.019(4) C17 0.040(4) 0.041(4) 0.042(4) -0.002(4) 0.012(3) -0.008(3) C18 0.061(6) 0.044(4) 0.049(5) -0.007(4) 0.006(4) -0.016(4) C19 0.085(7) 0.039(5) 0.035(4) -0.001(4) -0.006(4) 0.002(5) C20 0.048(4) 0.043(4) 0.033(4) 0.007(3) 0.000(3) 0.009(4) C21 0.045(4) 0.039(4) 0.032(4) -0.008(3) 0.000(3) 0.004(3) C22 0.067(6) 0.037(5) 0.064(6) 0.005(4) -0.025(5) 0.019(4) C23 0.043(5) 0.044(5) 0.065(6) -0.011(4) -0.006(4) 0.005(4) C24 0.066(7) 0.046(6) 0.087(8) -0.029(5) 0.003(6) 0.019(5) C25 0.058(5) 0.057(5) 0.047(4) -0.018(3) -0.004(5) 0.015(6) C26 0.051(5) 0.023(4) 0.055(5) -0.012(3) -0.006(4) -0.010(3) C27 0.063(6) 0.036(5) 0.068(7) -0.017(4) -0.001(5) -0.013(4) C28 0.114(10) 0.038(5) 0.086(8) -0.003(5) -0.006(7) -0.018(6) C29 0.109(11) 0.044(5) 0.081(8) 0.007(5) -0.015(7) 0.025(6) N1 0.040(3) 0.030(3) 0.033(3) -0.002(2) 0.003(3) 0.002(3) N2 0.037(3) 0.045(4) 0.034(3) -0.005(3) -0.004(3) -0.003(3) N3 0.028(3) 0.044(4) 0.044(3) -0.014(3) 0.005(3) -0.007(2) N4 0.037(3) 0.036(3) 0.026(3) -0.009(3) 0.005(2) -0.003(3) F1 0.051(3) 0.044(3) 0.109(5) -0.003(3) -0.027(3) 0.011(3) F2 0.121(6) 0.064(4) 0.105(5) -0.040(4) -0.074(5) 0.038(4) F3 0.052(3) 0.075(4) 0.141(7) -0.015(5) -0.028(4) 0.030(3) F4 0.126(6) 0.059(4) 0.171(8) -0.041(4) -0.114(6) 0.030(4) F5 0.180(9) 0.077(5) 0.101(6) 0.035(5) 0.077(6) 0.045(5) F6 0.169(9) 0.118(7) 0.158(8) 0.079(7) 0.102(7) 0.039(7) P1 0.0337(9) 0.0415(9) 0.0404(9) -0.0003(7) -0.0039(9) 0.0017(10) Rh1 0.0355(3) 0.0282(3) 0.0416(3) -0.0054(2) -0.0030(3) 0.0012(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 C1 N1 1.351(10) . ? C1 C2 1.395(11) . ? C1 H1 0.9500 . ? C2 C3 1.380(13) . ? C2 H2 0.9500 . ? C3 C4 1.371(13) . ? C3 H3 0.9500 . ? C4 C5 1.388(11) . ? C4 H4 0.9500 . ? C5 N1 1.339(10) . ? C5 C6 1.499(11) . ? C6 N2 1.484(10) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N2 1.324(10) . ? C7 N3 1.324(10) . ? C7 Rh1 2.008(7) . ? C8 N2 1.474(10) . ? C8 C9 1.499(13) . ? C8 C12 1.548(12) . ? C8 H8 1.0000 . ? C9 C13 1.512(12) . ? C9 C10 1.527(12) . ? C9 C14 1.546(12) . ? C10 C15 1.506(12) . ? C10 N3 1.516(10) . ? C10 C11 1.583(12) . ? C11 C12 1.529(14) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.488(12) . ? C16 N3 1.495(10) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 N4 1.351(9) . ? C17 C18 1.364(13) . ? C18 C19 1.416(14) . ? C18 H18 0.9500 . ? C19 C20 1.352(13) . ? C19 H19 0.9500 . ? C20 C21 1.399(11) . ? C20 H20 0.9500 . ? C21 N4 1.342(10) . ? C21 H21 0.9500 . ? C22 C23 1.419(15) . ? C22 C29 1.506(16) . ? C22 Rh1 2.090(8) . ? C22 H22 0.9500 . ? C23 C24 1.510(13) . ? C23 Rh1 2.092(9) . ? C23 H23 0.9500 . ? C24 C25 1.509(15) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.511(13) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.354(14) . ? C26 Rh1 2.263(8) . ? C26 H26 0.9500 . ? C27 C28 1.531(16) . ? C27 Rh1 2.291(8) . ? C27 H27 0.9500 . ? C28 C29 1.520(17) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? N1 Rh1 2.242(6) . ? N4 Rh1 2.316(7) . ? F1 P1 1.591(5) . ? F2 P1 1.568(6) . ? F3 P1 1.572(6) . ? F4 P1 1.562(6) . ? F5 P1 1.540(7) . ? F6 P1 1.548(8) . ? 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 N1 C1 C2 124.5(8) . . ? N1 C1 H1 117.8 . . ? C2 C1 H1 117.8 . . ? C3 C2 C1 117.8(8) . . ? C3 C2 H2 121.1 . . ? C1 C2 H2 121.1 . . ? C4 C3 C2 118.4(8) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C3 C4 C5 120.6(8) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? N1 C5 C4 122.4(8) . . ? N1 C5 C6 116.1(7) . . ? C4 C5 C6 121.3(7) . . ? N2 C6 C5 112.3(6) . . ? N2 C6 H6A 109.1 . . ? C5 C6 H6A 109.1 . . ? N2 C6 H6B 109.1 . . ? C5 C6 H6B 109.1 . . ? H6A C6 H6B 107.9 . . ? N2 C7 N3 117.7(7) . . ? N2 C7 Rh1 120.3(6) . . ? N3 C7 Rh1 121.9(6) . . ? N2 C8 C9 108.9(7) . . ? N2 C8 C12 106.7(7) . . ? C9 C8 C12 103.9(7) . . ? N2 C8 H8 112.3 . . ? C9 C8 H8 112.3 . . ? C12 C8 H8 112.3 . . ? C8 C9 C13 113.4(8) . . ? C8 C9 C10 100.0(7) . . ? C13 C9 C10 113.1(8) . . ? C8 C9 C14 111.0(8) . . ? C13 C9 C14 107.7(8) . . ? C10 C9 C14 111.5(8) . . ? C15 C10 N3 110.9(7) . . ? C15 C10 C9 115.8(8) . . ? N3 C10 C9 106.9(6) . . ? C15 C10 C11 113.1(7) . . ? N3 C10 C11 107.4(7) . . ? C9 C10 C11 101.9(7) . . ? C12 C11 C10 104.7(6) . . ? C12 C11 H11A 110.8 . . ? C10 C11 H11A 110.8 . . ? C12 C11 H11B 110.8 . . ? C10 C11 H11B 110.8 . . ? H11A C11 H11B 108.9 . . ? C11 C12 C8 104.5(7) . . ? C11 C12 H12A 110.8 . . ? C8 C12 H12A 110.8 . . ? C11 C12 H12B 110.8 . . ? C8 C12 H12B 110.8 . . ? H12A C12 H12B 108.9 . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 N3 113.5(6) . . ? C17 C16 H16A 108.9 . . ? N3 C16 H16A 108.9 . . ? C17 C16 H16B 108.9 . . ? N3 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? N4 C17 C18 123.3(8) . . ? N4 C17 C16 114.6(7) . . ? C18 C17 C16 122.0(8) . . ? C17 C18 C19 118.3(8) . . ? C17 C18 H18 120.9 . . ? C19 C18 H18 120.9 . . ? C20 C19 C18 118.8(8) . . ? C20 C19 H19 120.6 . . ? C18 C19 H19 120.6 . . ? C19 C20 C21 119.7(8) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? N4 C21 C20 122.0(8) . . ? N4 C21 H21 119.0 . . ? C20 C21 H21 119.0 . . ? C23 C22 C29 128.0(10) . . ? C23 C22 Rh1 70.2(5) . . ? C29 C22 Rh1 114.7(7) . . ? C23 C22 H22 116.0 . . ? C29 C22 H22 116.0 . . ? Rh1 C22 H22 84.8 . . ? C22 C23 C24 123.5(10) . . ? C22 C23 Rh1 70.1(5) . . ? C24 C23 Rh1 114.3(6) . . ? C22 C23 H23 118.3 . . ? C24 C23 H23 118.3 . . ? Rh1 C23 H23 85.7 . . ? C25 C24 C23 115.0(7) . . ? C25 C24 H24A 108.5 . . ? C23 C24 H24A 108.5 . . ? C25 C24 H24B 108.5 . . ? C23 C24 H24B 108.5 . . ? H24A C24 H24B 107.5 . . ? C24 C25 C26 113.6(7) . . ? C24 C25 H25A 108.8 . . ? C26 C25 H25A 108.8 . . ? C24 C25 H25B 108.8 . . ? C26 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? C27 C26 C25 125.6(9) . . ? C27 C26 Rh1 73.8(5) . . ? C25 C26 Rh1 106.7(6) . . ? C27 C26 H26 117.2 . . ? C25 C26 H26 117.2 . . ? Rh1 C26 H26 89.4 . . ? C26 C27 C28 125.0(10) . . ? C26 C27 Rh1 71.6(5) . . ? C28 C27 Rh1 111.5(7) . . ? C26 C27 H27 117.5 . . ? C28 C27 H27 117.5 . . ? Rh1 C27 H27 86.9 . . ? C29 C28 C27 111.8(8) . . ? C29 C28 H28A 109.3 . . ? C27 C28 H28A 109.3 . . ? C29 C28 H28B 109.3 . . ? C27 C28 H28B 109.3 . . ? H28A C28 H28B 107.9 . . ? C22 C29 C28 112.7(9) . . ? C22 C29 H29A 109.1 . . ? C28 C29 H29A 109.1 . . ? C22 C29 H29B 109.1 . . ? C28 C29 H29B 109.1 . . ? H29A C29 H29B 107.8 . . ? C5 N1 C1 116.3(7) . . ? C5 N1 Rh1 117.9(5) . . ? C1 N1 Rh1 125.7(5) . . ? C7 N2 C8 122.8(7) . . ? C7 N2 C6 120.1(6) . . ? C8 N2 C6 117.1(6) . . ? C7 N3 C16 116.6(6) . . ? C7 N3 C10 121.4(6) . . ? C16 N3 C10 122.0(6) . . ? C21 N4 C17 117.8(7) . . ? C21 N4 Rh1 125.9(5) . . ? C17 N4 Rh1 116.0(5) . . ? F5 P1 F6 177.9(7) . . ? F5 P1 F4 91.2(6) . . ? F6 P1 F4 90.4(6) . . ? F5 P1 F2 89.2(5) . . ? F6 P1 F2 89.2(6) . . ? F4 P1 F2 178.8(4) . . ? F5 P1 F3 88.2(5) . . ? F6 P1 F3 93.1(5) . . ? F4 P1 F3 91.9(4) . . ? F2 P1 F3 89.3(4) . . ? F5 P1 F1 91.2(4) . . ? F6 P1 F1 87.5(5) . . ? F4 P1 F1 88.8(3) . . ? F2 P1 F1 90.0(3) . . ? F3 P1 F1 179.1(4) . . ? C7 Rh1 C22 89.0(3) . . ? C7 Rh1 C23 91.9(3) . . ? C22 Rh1 C23 39.7(4) . . ? C7 Rh1 N1 84.9(3) . . ? C22 Rh1 N1 114.0(4) . . ? C23 Rh1 N1 153.6(3) . . ? C7 Rh1 C26 163.6(3) . . ? C22 Rh1 C26 94.6(4) . . ? C23 Rh1 C26 80.9(3) . . ? N1 Rh1 C26 108.0(3) . . ? C7 Rh1 C27 160.7(4) . . ? C22 Rh1 C27 78.5(4) . . ? C23 Rh1 C27 87.9(4) . . ? N1 Rh1 C27 86.8(3) . . ? C26 Rh1 C27 34.6(3) . . ? C7 Rh1 N4 84.5(3) . . ? C22 Rh1 N4 155.1(4) . . ? C23 Rh1 N4 116.4(3) . . ? N1 Rh1 N4 89.4(2) . . ? C26 Rh1 N4 85.6(3) . . ? C27 Rh1 N4 112.8(3) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.001 _refine_diff_density_min -1.118 _refine_diff_density_rms 0.129 # Attachment 'cmpd3_kjc1006.cif' data_cmpd3_DT_ART_04_2011_010582 _database_code_depnum_ccdc_archive 'CCDC 820462' #TrackingRef 'cmpd3_kjc1006.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H38 Ir N4, P F6' _chemical_formula_sum 'C29 H38 F6 Ir N4 P' _chemical_formula_weight 779.80 _chemical_absolute_configuration ad 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 P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 11.9370(6) _cell_length_b 14.3375(5) _cell_length_c 16.8348(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2881.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5794 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 27.42 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.798 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 4.756 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.3296 _exptl_absorpt_correction_T_max 0.3827 _exptl_absorpt_process_details Denzo/Scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9643 _diffrn_reflns_av_R_equivalents 0.0597 _diffrn_reflns_av_sigmaI/netI 0.0997 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 27.42 _reflns_number_total 6304 _reflns_number_gt 5794 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'cOLLECT,Nonius BV, 1997-2001' _computing_cell_refinement DENZO/SCALEPACK _computing_data_reduction DENZO/SCALEPACK _computing_structure_solution SHELXs-97 _computing_structure_refinement SHELXL-97 _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^)+(0.0000P)^2^+36.8469P] 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 SHELXL _refine_ls_extinction_coef 0.0053(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.103(18) _refine_ls_number_reflns 6304 _refine_ls_number_parameters 374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0687 _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.1489 _refine_ls_wR_factor_gt 0.1441 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 C1 C 0.4016(10) 0.5529(8) 0.7077(8) 0.030(3) Uani 1 1 d . . . H1 H 0.4613 0.5113 0.6963 0.036 Uiso 1 1 calc R . . C2 C 0.4246(11) 0.6301(9) 0.7534(8) 0.037(3) Uani 1 1 d . . . H2 H 0.4988 0.6415 0.7714 0.045 Uiso 1 1 calc R . . C3 C 0.3399(13) 0.6902(9) 0.7729(8) 0.040(3) Uani 1 1 d . . . H3 H 0.3533 0.7431 0.8055 0.048 Uiso 1 1 calc R . . C4 C 0.2333(12) 0.6711(8) 0.7433(6) 0.034(3) Uani 1 1 d . . . H4 H 0.1727 0.7126 0.7529 0.040 Uiso 1 1 calc R . . C5 C 0.2175(9) 0.5901(8) 0.6994(6) 0.027(2) Uani 1 1 d . . . C6 C 0.1004(10) 0.5624(10) 0.6679(7) 0.035(3) Uani 1 1 d . . . H6A H 0.0841 0.4972 0.6836 0.042 Uiso 1 1 calc R . . H6B H 0.0431 0.6030 0.6927 0.042 Uiso 1 1 calc R . . C7 C 0.1613(10) 0.5142(10) 0.5391(8) 0.033(3) Uani 1 1 d . . . C8 C 0.0115(10) 0.6387(9) 0.5419(7) 0.031(3) Uani 1 1 d . . . C9 C 0.0771(10) 0.6815(8) 0.4700(7) 0.030(3) Uani 1 1 d . . . C10 C 0.0888(9) 0.5930(8) 0.4196(7) 0.032(2) Uani 1 1 d . . . H10 H 0.1171 0.6075 0.3651 0.038 Uiso 1 1 calc R . . C11 C -0.0797(9) 0.5778(9) 0.4991(7) 0.031(2) Uani 1 1 d . . . H11A H -0.0946 0.5202 0.5296 0.037 Uiso 1 1 calc R . . H11B H -0.1505 0.6131 0.4937 0.037 Uiso 1 1 calc R . . C12 C -0.0316(11) 0.5543(10) 0.4172(9) 0.041(3) Uani 1 1 d . . . H12A H -0.0756 0.5845 0.3745 0.049 Uiso 1 1 calc R . . H12B H -0.0312 0.4860 0.4082 0.049 Uiso 1 1 calc R . . C13 C -0.0325(11) 0.7106(9) 0.6021(8) 0.039(3) Uani 1 1 d . . . H13A H -0.0674 0.6781 0.6469 0.058 Uiso 1 1 calc R . . H13B H -0.0880 0.7508 0.5763 0.058 Uiso 1 1 calc R . . H13C H 0.0299 0.7488 0.6214 0.058 Uiso 1 1 calc R . . C14 C 0.0066(11) 0.7548(10) 0.4268(8) 0.044(3) Uani 1 1 d . . . H14A H 0.0156 0.8154 0.4531 0.066 Uiso 1 1 calc R . . H14B H -0.0725 0.7364 0.4282 0.066 Uiso 1 1 calc R . . H14C H 0.0314 0.7596 0.3715 0.066 Uiso 1 1 calc R . . C15 C 0.1884(11) 0.7264(11) 0.4948(11) 0.056(4) Uani 1 1 d . . . H15A H 0.2287 0.7477 0.4474 0.084 Uiso 1 1 calc R . . H15B H 0.2342 0.6805 0.5233 0.084 Uiso 1 1 calc R . . H15C H 0.1736 0.7798 0.5296 0.084 Uiso 1 1 calc R . . C16 C 0.2442(10) 0.4757(7) 0.4125(7) 0.034(2) Uani 1 1 d . . . H16A H 0.2348 0.4936 0.3561 0.041 Uiso 1 1 calc R . . H16B H 0.2274 0.4083 0.4170 0.041 Uiso 1 1 calc R . . C17 C 0.3628(10) 0.4915(8) 0.4358(7) 0.031(3) Uani 1 1 d . . . C18 C 0.4404(12) 0.5227(10) 0.3811(7) 0.037(3) Uani 1 1 d . . . H18 H 0.4168 0.5380 0.3288 0.044 Uiso 1 1 calc R . . C19 C 0.5532(11) 0.5321(10) 0.4018(9) 0.042(3) Uani 1 1 d . . . H19 H 0.6072 0.5537 0.3647 0.050 Uiso 1 1 calc R . . C20 C 0.5824(11) 0.5087(8) 0.4778(8) 0.032(3) Uani 1 1 d . . . H20 H 0.6582 0.5124 0.4946 0.039 Uiso 1 1 calc R . . C21 C 0.5001(9) 0.4797(8) 0.5296(7) 0.029(2) Uani 1 1 d . . . H21 H 0.5223 0.4642 0.5822 0.035 Uiso 1 1 calc R . . C22 C 0.1587(13) 0.3159(9) 0.5404(8) 0.038(3) Uani 1 1 d . . . H22 H 0.1472 0.3628 0.5014 0.046 Uiso 1 1 calc R . . C23 C 0.1186(11) 0.3365(10) 0.6204(8) 0.040(3) Uani 1 1 d . . . H23 H 0.0829 0.3945 0.6302 0.048 Uiso 1 1 calc R . . C24 C 0.1324(13) 0.2675(10) 0.6888(9) 0.050(4) Uani 1 1 d . . . H24A H 0.1259 0.2032 0.6680 0.060 Uiso 1 1 calc R . . H24B H 0.0712 0.2772 0.7277 0.060 Uiso 1 1 calc R . . C25 C 0.2461(12) 0.2785(10) 0.7313(7) 0.044(3) Uani 1 1 d . . . H25A H 0.2357 0.3185 0.7787 0.053 Uiso 1 1 calc R . . H25B H 0.2712 0.2164 0.7500 0.053 Uiso 1 1 calc R . . C26 C 0.3361(11) 0.3201(10) 0.6800(9) 0.040(3) Uani 1 1 d . . . H26 H 0.3758 0.3717 0.7013 0.048 Uiso 1 1 calc R . . C27 C 0.3659(11) 0.2921(8) 0.6078(9) 0.038(3) Uani 1 1 d . . . H27 H 0.4213 0.3270 0.5803 0.046 Uiso 1 1 calc R . . C28 C 0.3155(17) 0.2061(9) 0.5665(10) 0.063(5) Uani 1 1 d . . . H28A H 0.3742 0.1759 0.5339 0.075 Uiso 1 1 calc R . . H28B H 0.2915 0.1608 0.6075 0.075 Uiso 1 1 calc R . . C29 C 0.2156(16) 0.2291(12) 0.5135(12) 0.071(5) Uani 1 1 d . . . H29A H 0.2416 0.2371 0.4581 0.085 Uiso 1 1 calc R . . H29B H 0.1617 0.1767 0.5146 0.085 Uiso 1 1 calc R . . N1 N 0.2977(8) 0.5322(6) 0.6773(5) 0.0234(19) Uani 1 1 d . . . N2 N 0.3911(8) 0.4717(7) 0.5115(6) 0.026(2) Uani 1 1 d . . . N3 N 0.0927(7) 0.5706(7) 0.5813(5) 0.0275(19) Uani 1 1 d . . . N4 N 0.1625(8) 0.5282(8) 0.4609(6) 0.030(2) Uani 1 1 d . . . F1 F 0.6958(9) 0.5530(6) 0.6526(7) 0.085(4) Uani 1 1 d . . . F2 F 0.7849(11) 0.4199(9) 0.6309(7) 0.106(4) Uani 1 1 d . . . F3 F 0.8582(7) 0.5275(8) 0.7156(8) 0.075(3) Uani 1 1 d . . . F4 F 0.7903(9) 0.3906(6) 0.7585(8) 0.091(4) Uani 1 1 d . . . F5 F 0.7013(11) 0.5222(7) 0.7827(6) 0.096(5) Uani 1 1 d . . . F6 F 0.6280(6) 0.4148(6) 0.6997(6) 0.060(2) Uani 1 1 d . . . P1 P 0.7434(3) 0.47264(19) 0.70666(17) 0.0300(6) Uani 1 1 d . . . Ir1 Ir 0.25872(4) 0.41802(3) 0.59159(2) 0.02496(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.023(5) 0.029(6) 0.039(7) -0.003(5) -0.003(5) -0.001(4) C2 0.037(7) 0.034(7) 0.041(8) 0.001(6) 0.004(6) -0.014(5) C3 0.061(9) 0.030(6) 0.028(6) 0.003(5) 0.006(7) -0.002(6) C4 0.040(7) 0.038(6) 0.024(5) 0.003(4) 0.006(5) 0.017(6) C5 0.037(6) 0.022(5) 0.021(5) -0.002(4) 0.019(4) 0.007(5) C6 0.024(5) 0.060(9) 0.022(6) 0.005(6) 0.010(4) 0.012(6) C7 0.019(6) 0.050(7) 0.030(6) 0.007(6) -0.001(5) -0.011(5) C8 0.031(6) 0.042(7) 0.021(6) 0.004(5) 0.000(5) 0.000(5) C9 0.031(6) 0.028(6) 0.032(6) 0.012(5) -0.007(5) 0.006(5) C10 0.031(5) 0.035(6) 0.029(6) 0.003(5) -0.003(5) 0.000(5) C11 0.023(5) 0.030(6) 0.040(6) 0.010(6) -0.006(4) -0.003(5) C12 0.043(7) 0.044(7) 0.034(7) 0.002(6) -0.011(6) -0.002(5) C13 0.042(7) 0.035(6) 0.039(8) 0.001(6) 0.002(6) 0.014(5) C14 0.039(7) 0.047(8) 0.046(8) 0.021(7) 0.001(6) -0.001(6) C15 0.029(7) 0.058(9) 0.081(12) 0.020(8) 0.013(7) -0.013(7) C16 0.035(6) 0.035(5) 0.033(6) 0.002(5) -0.003(7) 0.000(5) C17 0.035(7) 0.031(6) 0.026(6) -0.001(5) -0.008(5) 0.004(5) C18 0.044(7) 0.046(7) 0.020(6) 0.003(5) 0.002(5) -0.001(6) C19 0.044(7) 0.047(7) 0.034(7) -0.020(7) 0.013(6) -0.003(6) C20 0.035(7) 0.021(5) 0.041(7) 0.002(5) 0.004(5) 0.000(5) C21 0.022(5) 0.035(6) 0.031(6) -0.003(5) 0.000(5) 0.011(5) C22 0.054(9) 0.027(6) 0.033(7) -0.004(5) -0.006(6) -0.019(6) C23 0.035(7) 0.036(7) 0.048(8) 0.012(6) -0.007(6) -0.017(5) C24 0.057(9) 0.040(8) 0.053(9) 0.023(7) -0.009(7) -0.017(7) C25 0.043(7) 0.064(8) 0.025(5) 0.016(5) -0.015(7) -0.018(7) C26 0.028(7) 0.035(7) 0.056(9) 0.015(6) 0.005(6) 0.009(5) C27 0.038(7) 0.024(6) 0.052(9) 0.017(6) -0.006(6) 0.012(5) C28 0.116(15) 0.025(6) 0.047(9) 0.018(6) -0.001(9) 0.014(8) C29 0.075(12) 0.056(10) 0.082(12) -0.031(9) -0.003(10) -0.024(9) N1 0.026(5) 0.021(4) 0.023(5) -0.007(4) 0.006(4) -0.001(4) N2 0.026(5) 0.024(5) 0.029(5) -0.008(4) 0.006(4) 0.000(4) N3 0.018(4) 0.040(5) 0.025(5) 0.004(4) 0.001(3) 0.000(4) N4 0.028(5) 0.040(6) 0.022(5) 0.009(4) -0.005(4) 0.001(4) F1 0.099(8) 0.044(5) 0.112(9) 0.038(5) -0.067(7) -0.029(5) F2 0.124(10) 0.096(8) 0.096(8) -0.058(7) 0.046(8) -0.018(8) F3 0.036(5) 0.076(7) 0.114(9) 0.004(7) -0.014(6) -0.021(5) F4 0.095(8) 0.045(5) 0.134(10) 0.025(6) -0.078(8) -0.028(5) F5 0.149(12) 0.068(7) 0.072(7) -0.034(6) 0.069(8) -0.044(7) F6 0.038(4) 0.041(4) 0.099(7) 0.017(5) -0.026(4) -0.008(4) P1 0.0256(14) 0.0326(14) 0.0317(14) -0.0007(11) -0.0015(14) -0.0010(14) Ir1 0.0239(2) 0.0215(2) 0.0295(2) 0.00331(16) -0.00088(18) 0.00001(18) _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 C1 N1 1.373(14) . ? C1 C2 1.376(17) . ? C2 C3 1.368(19) . ? C3 C4 1.394(19) . ? C4 C5 1.389(15) . ? C5 N1 1.320(13) . ? C5 C6 1.548(17) . ? C6 N3 1.466(14) . ? C7 N4 1.332(16) . ? C7 N3 1.352(16) . ? C7 Ir1 2.008(13) . ? C8 N3 1.527(15) . ? C8 C13 1.539(17) . ? C8 C9 1.567(17) . ? C8 C11 1.570(16) . ? C9 C14 1.530(16) . ? C9 C10 1.533(17) . ? C9 C15 1.535(19) . ? C10 N4 1.456(14) . ? C10 C12 1.541(17) . ? C11 C12 1.531(18) . ? C16 N4 1.477(15) . ? C16 C17 1.486(16) . ? C17 N2 1.348(15) . ? C17 C18 1.381(17) . ? C18 C19 1.397(18) . ? C19 C20 1.37(2) . ? C20 C21 1.377(17) . ? C21 N2 1.341(14) . ? C22 C23 1.46(2) . ? C22 C29 1.49(2) . ? C22 Ir1 2.077(12) . ? C23 C24 1.526(18) . ? C23 Ir1 2.097(12) . ? C24 C25 1.542(19) . ? C25 C26 1.503(18) . ? C26 C27 1.33(2) . ? C26 Ir1 2.245(13) . ? C27 C28 1.54(2) . ? C27 Ir1 2.230(11) . ? C28 C29 1.52(2) . ? N1 Ir1 2.232(9) . ? N2 Ir1 2.216(10) . ? F1 P1 1.574(9) . ? F2 P1 1.563(10) . ? F3 P1 1.587(9) . ? F4 P1 1.569(10) . ? F5 P1 1.548(9) . ? F6 P1 1.612(8) . ? 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 N1 C1 C2 124.2(11) . . ? C3 C2 C1 119.5(13) . . ? C2 C3 C4 117.7(12) . . ? C5 C4 C3 118.6(11) . . ? N1 C5 C4 125.2(11) . . ? N1 C5 C6 113.4(10) . . ? C4 C5 C6 121.3(11) . . ? N3 C6 C5 112.1(9) . . ? N4 C7 N3 115.8(11) . . ? N4 C7 Ir1 122.1(10) . . ? N3 C7 Ir1 122.0(9) . . ? N3 C8 C13 111.1(9) . . ? N3 C8 C9 105.6(9) . . ? C13 C8 C9 114.6(11) . . ? N3 C8 C11 106.6(10) . . ? C13 C8 C11 116.0(10) . . ? C9 C8 C11 102.1(9) . . ? C14 C9 C10 110.8(10) . . ? C14 C9 C15 108.5(11) . . ? C10 C9 C15 114.8(11) . . ? C14 C9 C8 111.2(10) . . ? C10 C9 C8 98.5(9) . . ? C15 C9 C8 112.8(11) . . ? N4 C10 C9 108.6(9) . . ? N4 C10 C12 110.3(10) . . ? C9 C10 C12 103.2(10) . . ? C12 C11 C8 106.0(9) . . ? C11 C12 C10 104.2(10) . . ? N4 C16 C17 113.9(10) . . ? N2 C17 C18 122.0(11) . . ? N2 C17 C16 117.1(11) . . ? C18 C17 C16 120.8(11) . . ? C17 C18 C19 120.7(12) . . ? C20 C19 C18 117.2(13) . . ? C19 C20 C21 118.9(12) . . ? N2 C21 C20 125.0(12) . . ? C23 C22 C29 126.8(14) . . ? C23 C22 Ir1 70.3(7) . . ? C29 C22 Ir1 116.9(11) . . ? C22 C23 C24 122.0(13) . . ? C22 C23 Ir1 68.8(7) . . ? C24 C23 Ir1 116.7(9) . . ? C23 C24 C25 112.3(11) . . ? C26 C25 C24 113.8(10) . . ? C27 C26 C25 126.8(14) . . ? C27 C26 Ir1 72.1(8) . . ? C25 C26 Ir1 109.6(8) . . ? C26 C27 C28 123.4(14) . . ? C26 C27 Ir1 73.4(8) . . ? C28 C27 Ir1 111.6(9) . . ? C29 C28 C27 113.4(11) . . ? C22 C29 C28 111.1(13) . . ? C5 N1 C1 114.4(9) . . ? C5 N1 Ir1 119.5(8) . . ? C1 N1 Ir1 126.0(7) . . ? C21 N2 C17 116.1(11) . . ? C21 N2 Ir1 125.7(8) . . ? C17 N2 Ir1 118.0(8) . . ? C7 N3 C6 115.9(10) . . ? C7 N3 C8 122.6(9) . . ? C6 N3 C8 121.5(9) . . ? C7 N4 C10 124.2(11) . . ? C7 N4 C16 118.4(10) . . ? C10 N4 C16 117.5(9) . . ? F5 P1 F2 178.4(7) . . ? F5 P1 F4 90.0(7) . . ? F2 P1 F4 88.7(8) . . ? F5 P1 F1 91.4(7) . . ? F2 P1 F1 89.8(7) . . ? F4 P1 F1 178.4(6) . . ? F5 P1 F3 88.5(7) . . ? F2 P1 F3 92.5(7) . . ? F4 P1 F3 90.6(6) . . ? F1 P1 F3 90.2(6) . . ? F5 P1 F6 91.1(6) . . ? F2 P1 F6 87.9(6) . . ? F4 P1 F6 87.7(5) . . ? F1 P1 F6 91.6(5) . . ? F3 P1 F6 178.2(6) . . ? C7 Ir1 C22 88.2(5) . . ? C7 Ir1 C23 91.3(5) . . ? C22 Ir1 C23 40.9(6) . . ? C7 Ir1 N2 84.7(4) . . ? C22 Ir1 N2 113.7(5) . . ? C23 Ir1 N2 154.6(5) . . ? C7 Ir1 C27 160.4(5) . . ? C22 Ir1 C27 79.1(6) . . ? C23 Ir1 C27 88.7(6) . . ? N2 Ir1 C27 86.9(4) . . ? C7 Ir1 N1 84.4(5) . . ? C22 Ir1 N1 154.9(5) . . ? C23 Ir1 N1 115.2(5) . . ? N2 Ir1 N1 89.4(3) . . ? C27 Ir1 N1 113.3(4) . . ? C7 Ir1 C26 163.6(5) . . ? C22 Ir1 C26 94.1(6) . . ? C23 Ir1 C26 80.0(5) . . ? N2 Ir1 C26 109.1(4) . . ? C27 Ir1 C26 34.5(5) . . ? N1 Ir1 C26 86.8(5) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 2.205 _refine_diff_density_min -2.132 _refine_diff_density_rms 0.201