# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Munetaka Akita' _publ_contact_author_address ; Chemical Resources Laboratory Tokyo Institute of Technology R1-27 nagatsuta Midori-ku Yokohama 226-8503 JAPAN ; _publ_contact_author_email MAKITA@RES.TITECH.AC.JP _publ_section_title ; Selective synthesis of isomeric heterodinuclear complexes with switched metal arrangements: Proton-induced reversible metal migration on an iridium complex with a novel dinucleating PNNN ligand (3-diphenylphosphinomethyl-5-pyridylpyrazolate) ; loop_ _publ_author_name 'Munetaka Akita' 'Christian Dubs' 'Akiko Inagaki' data_compound_3a _database_code_depnum_ccdc_archive 'CCDC 243413' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'compound 3a BF4' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H34 B F4 Ir N3 P Pd' _chemical_formula_weight 877.00 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' B B 0.0013 0.0007 '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' Pd Pd -0.9988 1.0072 '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 triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.898(6) _cell_length_b 11.791(8) _cell_length_c 12.960(8) _cell_angle_alpha 96.74(2) _cell_angle_beta 111.63(2) _cell_angle_gamma 95.51(2) _cell_volume 1519.8(16) _cell_formula_units_Z 2 _cell_measurement_temperature 213 _cell_measurement_reflns_used 11566 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.6 _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.916 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 5.071 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.455 _exptl_absorpt_correction_T_max 0.602 _exptl_special_details ; ? ; _diffrn_ambient_temperature 213 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 11628 _diffrn_reflns_av_R_equivalents 0.0644 _diffrn_reflns_av_sigmaI/netI 0.0709 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6288 _reflns_number_gt 4764 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'teXsan Ver. 1.11' _computing_publication_material 'teXsan Ver. 1.11' _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6288 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0862 _refine_ls_R_factor_gt 0.0732 _refine_ls_wR_factor_ref 0.2569 _refine_ls_wR_factor_gt 0.2532 _refine_ls_goodness_of_fit_ref 1.635 _refine_ls_restrained_S_all 1.635 _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 0.28510(5) -0.17469(5) -0.12458(5) 0.0520(2) Uani 1 1 d . . . Pd1 Pd 0.37167(10) -0.41864(9) 0.14164(9) 0.0487(3) Uani 1 1 d . . . P1 P 0.5835(4) -0.4004(3) 0.2753(3) 0.0503(8) Uani 1 1 d . . . F1 F 0.8071(9) 0.2201(10) 0.7227(10) 0.081(3) Uani 1 1 d . . . F2 F 0.9938(11) 0.3488(10) 0.7590(11) 0.092(3) Uani 1 1 d . . . F3 F 0.9798(15) 0.1618(12) 0.6888(15) 0.122(5) Uani 1 1 d . . . F4 F 0.9991(12) 0.2136(14) 0.8680(11) 0.109(4) Uani 1 1 d . . . N1 N 0.4724(10) -0.3226(10) 0.0547(9) 0.047(2) Uani 1 1 d . . . N2 N 0.4481(10) -0.2441(10) -0.0152(9) 0.045(2) Uani 1 1 d . . . N3 N 0.4480(13) -0.0710(10) -0.1380(10) 0.055(3) Uani 1 1 d . . . C1 C 0.1517(14) -0.4838(16) 0.0387(16) 0.073(5) Uani 1 1 d . . . C01 C 0.1532(16) -0.3300(14) -0.1573(14) 0.062(4) Uani 1 1 d . . . C2 C 0.2073(18) -0.5496(18) 0.1213(19) 0.080(6) Uani 1 1 d . . . C02 C 0.1246(16) -0.2480(14) -0.0829(16) 0.063(4) Uani 1 1 d . . . C3 C 0.2722(16) -0.494(2) 0.2322(14) 0.080(6) Uani 1 1 d . . . C03 C 0.0025(18) -0.1864(18) -0.1150(17) 0.074(5) Uani 1 1 d . . . C04 C 0.0305(19) -0.0717(16) -0.1557(18) 0.081(5) Uani 1 1 d . . . C05 C 0.1368(14) -0.0682(14) -0.1966(15) 0.063(4) Uani 1 1 d . . . C06 C 0.1461(15) -0.1516(16) -0.2812(13) 0.066(4) Uani 1 1 d . . . C07 C 0.0338(17) -0.2557(15) -0.3422(14) 0.066(4) Uani 1 1 d . . . C08 C 0.0668(17) -0.3593(17) -0.2818(17) 0.077(5) Uani 1 1 d . . . C11 C 0.6074(15) -0.3260(14) 0.0943(12) 0.056(3) Uani 1 1 d . . . C12 C 0.6706(12) -0.2474(13) 0.0504(12) 0.050(3) Uani 1 1 d . . . C13 C 0.5642(12) -0.1966(12) -0.0212(11) 0.047(3) Uani 1 1 d . . . C14 C 0.6680(14) -0.4027(15) 0.1776(13) 0.058(4) Uani 1 1 d . . . C21 C 0.5687(13) -0.1072(13) -0.0852(12) 0.053(3) Uani 1 1 d . . . C22 C 0.6819(19) -0.0569(16) -0.0999(15) 0.068(4) Uani 1 1 d . . . C23 C 0.6766(16) 0.0268(15) -0.1636(15) 0.065(4) Uani 1 1 d . . . C24 C 0.5516(18) 0.0668(14) -0.2127(15) 0.065(4) Uani 1 1 d . . . C25 C 0.4440(15) 0.0145(14) -0.2000(12) 0.058(4) Uani 1 1 d . . . C31 C 0.6366(15) -0.5162(13) 0.3535(12) 0.055(3) Uani 1 1 d . . . C32 C 0.5675(16) -0.6282(14) 0.3067(14) 0.059(4) Uani 1 1 d . . . C33 C 0.6062(19) -0.7207(13) 0.3654(15) 0.067(4) Uani 1 1 d . . . C34 C 0.715(2) -0.7019(17) 0.4678(16) 0.077(5) Uani 1 1 d . . . C35 C 0.7854(19) -0.5919(17) 0.5133(16) 0.073(5) Uani 1 1 d . . . C36 C 0.7410(17) -0.4978(15) 0.4565(13) 0.064(4) Uani 1 1 d . . . C41 C 0.6507(15) -0.2671(14) 0.3782(12) 0.057(4) Uani 1 1 d . . . C42 C 0.7636(16) -0.1918(16) 0.3898(15) 0.073(5) Uani 1 1 d . . . C43 C 0.809(2) -0.0911(17) 0.4634(17) 0.081(6) Uani 1 1 d . . . C44 C 0.740(2) -0.0671(15) 0.522(2) 0.090(7) Uani 1 1 d . . . C45 C 0.624(3) -0.1346(19) 0.5224(18) 0.104(8) Uani 1 1 d . . . C46 C 0.5796(19) -0.2335(16) 0.4436(17) 0.076(5) Uani 1 1 d . . . B1 B 0.946(2) 0.233(2) 0.7597(19) 0.073(5) Uani 1 1 d . . . H1 H 0.0865 -0.4367 0.0454 0.089 Uiso 1 1 d . . . H2 H 0.1239 -0.5166 -0.0389 0.089 Uiso 1 1 d . . . H3 H 0.2120 -0.6296 0.1022 0.097 Uiso 1 1 d . . . H4 H 0.3204 -0.5403 0.2857 0.095 Uiso 1 1 d . . . H5 H 0.2239 -0.4493 0.2633 0.095 Uiso 1 1 d . . . H6 H 0.1950 -0.3926 -0.1234 0.076 Uiso 1 1 d . . . H7 H 0.1542 -0.2645 -0.0066 0.079 Uiso 1 1 d . . . H8 H -0.0713 -0.2358 -0.1751 0.088 Uiso 1 1 d . . . H9 H -0.0240 -0.1717 -0.0523 0.088 Uiso 1 1 d . . . H10 H -0.0488 -0.0586 -0.2134 0.093 Uiso 1 1 d . . . H11 H 0.0535 -0.0094 -0.0926 0.093 Uiso 1 1 d . . . H12 H 0.1754 0.0096 -0.1953 0.076 Uiso 1 1 d . . . H13 H 0.1860 -0.1204 -0.3292 0.077 Uiso 1 1 d . . . H14 H -0.0491 -0.2350 -0.3411 0.080 Uiso 1 1 d . . . H15 H 0.0230 -0.2742 -0.4193 0.080 Uiso 1 1 d . . . H16 H 0.1135 -0.4054 -0.3182 0.092 Uiso 1 1 d . . . H17 H -0.0143 -0.4067 -0.2917 0.092 Uiso 1 1 d . . . H18 H 0.7643 -0.2301 0.0656 0.060 Uiso 1 1 d . . . H19 H 0.7616 -0.3764 0.2164 0.072 Uiso 1 1 d . . . H20 H 0.6572 -0.4802 0.1387 0.072 Uiso 1 1 d . . . H21 H 0.7667 -0.0827 -0.0618 0.082 Uiso 1 1 d . . . H22 H 0.7533 0.0592 -0.1747 0.079 Uiso 1 1 d . . . H23 H 0.5445 0.1323 -0.2523 0.078 Uiso 1 1 d . . . H24 H 0.3591 0.0377 -0.2381 0.070 Uiso 1 1 d . . . H25 H 0.4944 -0.6415 0.2351 0.072 Uiso 1 1 d . . . H26 H 0.5567 -0.7973 0.3348 0.079 Uiso 1 1 d . . . H27 H 0.7418 -0.7655 0.5071 0.094 Uiso 1 1 d . . . H28 H 0.8639 -0.5780 0.5831 0.086 Uiso 1 1 d . . . H29 H 0.7831 -0.4201 0.4912 0.077 Uiso 1 1 d . . . H30 H 0.8136 -0.2126 0.3418 0.091 Uiso 1 1 d . . . H31 H 0.8875 -0.0405 0.4712 0.097 Uiso 1 1 d . . . H32 H 0.7678 0.0072 0.5695 0.104 Uiso 1 1 d . . . H33 H 0.5788 -0.1128 0.5744 0.126 Uiso 1 1 d . . . H34 H 0.4937 -0.2813 0.4303 0.091 Uiso 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 0.0479(4) 0.0564(4) 0.0487(3) 0.0096(2) 0.0141(2) 0.0103(2) Pd1 0.0410(6) 0.0558(6) 0.0467(6) 0.0081(4) 0.0149(4) 0.0039(4) P1 0.0446(19) 0.057(2) 0.0441(17) 0.0112(15) 0.0115(14) 0.0049(14) F1 0.052(6) 0.096(8) 0.088(7) 0.026(6) 0.020(5) -0.007(5) F2 0.070(7) 0.080(7) 0.113(9) 0.025(6) 0.022(6) -0.001(5) F3 0.131(12) 0.105(10) 0.149(13) -0.012(9) 0.086(11) 0.014(8) F4 0.078(8) 0.161(13) 0.095(9) 0.064(9) 0.030(7) 0.015(7) N1 0.038(6) 0.059(7) 0.042(5) 0.011(5) 0.012(4) 0.002(4) N2 0.034(5) 0.056(6) 0.040(5) 0.012(5) 0.006(4) 0.011(4) N3 0.056(7) 0.049(7) 0.051(6) 0.009(5) 0.013(5) 0.000(5) C1 0.022(7) 0.090(12) 0.084(11) 0.020(9) -0.004(7) -0.010(6) C01 0.058(9) 0.061(9) 0.058(9) 0.008(7) 0.017(7) -0.009(7) C2 0.055(11) 0.089(13) 0.103(15) 0.026(11) 0.040(10) -0.009(8) C02 0.053(9) 0.055(9) 0.085(11) 0.013(8) 0.032(8) -0.002(6) C3 0.039(9) 0.150(19) 0.052(9) 0.025(10) 0.014(7) 0.017(9) C03 0.064(10) 0.092(13) 0.083(12) 0.025(10) 0.040(9) 0.027(9) C04 0.068(11) 0.063(11) 0.093(13) 0.008(9) 0.009(10) 0.021(8) C05 0.042(8) 0.061(9) 0.072(10) 0.020(8) 0.001(7) 0.016(6) C06 0.047(9) 0.078(11) 0.051(8) 0.017(8) -0.004(6) 0.000(7) C07 0.062(10) 0.068(10) 0.054(8) 0.003(7) 0.012(7) -0.001(7) C08 0.047(10) 0.078(12) 0.084(12) 0.010(9) 0.009(8) -0.013(7) C11 0.049(8) 0.071(10) 0.047(7) 0.012(7) 0.015(6) 0.010(6) C12 0.028(6) 0.062(8) 0.054(7) 0.007(6) 0.009(5) 0.004(5) C13 0.032(6) 0.064(8) 0.044(7) 0.013(6) 0.013(5) 0.002(5) C14 0.042(8) 0.077(10) 0.050(8) 0.011(7) 0.012(6) 0.004(6) C21 0.042(7) 0.063(9) 0.048(7) 0.011(6) 0.010(6) 0.011(6) C22 0.089(12) 0.071(11) 0.066(10) 0.029(8) 0.047(9) 0.020(8) C23 0.058(9) 0.065(10) 0.073(10) 0.012(8) 0.028(8) 0.008(7) C24 0.077(11) 0.055(9) 0.064(9) 0.011(7) 0.030(8) -0.003(7) C25 0.050(8) 0.070(10) 0.045(7) 0.012(7) 0.007(6) 0.013(7) C31 0.065(9) 0.052(8) 0.048(7) 0.007(6) 0.024(7) 0.002(6) C32 0.058(9) 0.060(9) 0.057(8) 0.011(7) 0.018(7) 0.010(7) C33 0.100(13) 0.045(8) 0.064(10) 0.010(7) 0.042(9) 0.010(8) C34 0.113(15) 0.070(11) 0.063(10) 0.023(9) 0.042(10) 0.040(10) C35 0.079(12) 0.072(11) 0.067(10) 0.016(9) 0.023(9) 0.021(9) C36 0.069(10) 0.065(10) 0.051(8) 0.012(7) 0.016(7) 0.002(7) C41 0.058(9) 0.062(9) 0.042(7) 0.009(6) 0.013(6) -0.011(6) C42 0.046(9) 0.083(12) 0.065(10) 0.020(9) -0.007(7) -0.001(7) C43 0.073(12) 0.069(12) 0.075(12) 0.022(9) 0.005(10) -0.028(9) C44 0.084(13) 0.043(9) 0.123(18) 0.027(10) 0.017(13) -0.006(8) C45 0.15(2) 0.070(13) 0.067(12) -0.005(10) 0.033(13) -0.025(13) C46 0.078(12) 0.067(11) 0.079(12) -0.006(9) 0.037(10) -0.008(8) B1 0.078(14) 0.077(13) 0.078(13) 0.035(11) 0.042(11) 0.005(10) _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 C06 2.105(14) . ? Ir1 C01 2.112(15) . ? Ir1 N2 2.128(10) . ? Ir1 N3 2.130(12) . ? Ir1 C05 2.148(14) . ? Ir1 C02 2.149(15) . ? Pd1 C3 2.086(18) . ? Pd1 C2 2.165(16) . ? Pd1 N1 2.174(11) . ? Pd1 C1 2.273(13) . ? Pd1 P1 2.290(4) . ? P1 C31 1.808(16) . ? P1 C14 1.819(16) . ? P1 C41 1.832(16) . ? F1 B1 1.40(2) . ? F2 B1 1.41(2) . ? F3 B1 1.35(3) . ? F4 B1 1.36(2) . ? N1 N2 1.348(15) . ? N1 C11 1.375(18) . ? N2 C13 1.366(16) . ? N3 C25 1.355(19) . ? N3 C21 1.376(18) . ? C1 C2 1.39(3) . ? C01 C02 1.42(2) . ? C01 C08 1.52(2) . ? C2 C3 1.39(3) . ? C02 C03 1.52(2) . ? C03 C04 1.55(3) . ? C04 C05 1.44(3) . ? C05 C06 1.42(3) . ? C06 C07 1.55(2) . ? C07 C08 1.53(3) . ? C11 C12 1.40(2) . ? C11 C14 1.50(2) . ? C12 C13 1.427(18) . ? C13 C21 1.42(2) . ? C21 C22 1.40(2) . ? C22 C23 1.35(2) . ? C23 C24 1.43(2) . ? C24 C25 1.34(2) . ? C31 C36 1.37(2) . ? C31 C32 1.40(2) . ? C32 C33 1.41(2) . ? C33 C34 1.39(3) . ? C34 C35 1.38(3) . ? C35 C36 1.43(2) . ? C41 C46 1.39(2) . ? C41 C42 1.39(2) . ? C42 C43 1.36(3) . ? C43 C44 1.28(3) . ? C44 C45 1.43(3) . ? C45 C46 1.37(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 C06 Ir1 C01 82.6(7) . . ? C06 Ir1 N2 155.5(6) . . ? C01 Ir1 N2 92.1(6) . . ? C06 Ir1 N3 94.4(6) . . ? C01 Ir1 N3 153.5(6) . . ? N2 Ir1 N3 79.8(5) . . ? C06 Ir1 C05 39.1(7) . . ? C01 Ir1 C05 97.3(7) . . ? N2 Ir1 C05 164.5(6) . . ? N3 Ir1 C05 96.6(6) . . ? C06 Ir1 C02 89.9(7) . . ? C01 Ir1 C02 39.0(7) . . ? N2 Ir1 C02 100.9(6) . . ? N3 Ir1 C02 167.3(6) . . ? C05 Ir1 C02 79.3(7) . . ? C3 Pd1 C2 38.1(8) . . ? C3 Pd1 N1 174.1(7) . . ? C2 Pd1 N1 145.2(7) . . ? C3 Pd1 C1 66.3(7) . . ? C2 Pd1 C1 36.3(7) . . ? N1 Pd1 C1 114.3(6) . . ? C3 Pd1 P1 97.2(5) . . ? C2 Pd1 P1 125.2(6) . . ? N1 Pd1 P1 83.0(3) . . ? C1 Pd1 P1 161.5(5) . . ? C31 P1 C14 105.2(7) . . ? C31 P1 C41 105.6(7) . . ? C14 P1 C41 108.6(7) . . ? C31 P1 Pd1 120.6(5) . . ? C14 P1 Pd1 96.1(5) . . ? C41 P1 Pd1 118.8(6) . . ? N2 N1 C11 107.0(11) . . ? N2 N1 Pd1 139.0(8) . . ? C11 N1 Pd1 113.0(9) . . ? N1 N2 C13 110.3(10) . . ? N1 N2 Ir1 140.1(8) . . ? C13 N2 Ir1 109.5(8) . . ? C25 N3 C21 118.4(12) . . ? C25 N3 Ir1 128.2(10) . . ? C21 N3 Ir1 113.0(10) . . ? C2 C1 Pd1 67.6(9) . . ? C02 C01 C08 122.2(17) . . ? C02 C01 Ir1 71.9(9) . . ? C08 C01 Ir1 109.9(11) . . ? C1 C2 C3 119(2) . . ? C1 C2 Pd1 76.1(10) . . ? C3 C2 Pd1 67.8(11) . . ? C01 C02 C03 125.3(17) . . ? C01 C02 Ir1 69.1(9) . . ? C03 C02 Ir1 115.2(12) . . ? C2 C3 Pd1 74.0(10) . . ? C02 C03 C04 111.0(14) . . ? C05 C04 C03 114.0(15) . . ? C06 C05 C04 125.8(15) . . ? C06 C05 Ir1 68.8(8) . . ? C04 C05 Ir1 114.7(12) . . ? C05 C06 C07 120.9(15) . . ? C05 C06 Ir1 72.1(8) . . ? C07 C06 Ir1 114.5(11) . . ? C08 C07 C06 109.7(13) . . ? C01 C08 C07 115.3(15) . . ? N1 C11 C12 110.6(13) . . ? N1 C11 C14 120.4(13) . . ? C12 C11 C14 128.9(14) . . ? C11 C12 C13 104.0(11) . . ? N2 C13 C21 122.3(11) . . ? N2 C13 C12 108.0(11) . . ? C21 C13 C12 129.6(11) . . ? C11 C14 P1 108.0(11) . . ? N3 C21 C22 119.1(14) . . ? N3 C21 C13 114.7(12) . . ? C22 C21 C13 126.1(13) . . ? C23 C22 C21 122.1(16) . . ? C22 C23 C24 117.6(15) . . ? C25 C24 C23 118.8(15) . . ? C24 C25 N3 123.8(14) . . ? C36 C31 C32 119.4(15) . . ? C36 C31 P1 122.4(12) . . ? C32 C31 P1 118.2(11) . . ? C31 C32 C33 119.7(15) . . ? C34 C33 C32 120.4(15) . . ? C35 C34 C33 120.0(16) . . ? C34 C35 C36 119.2(17) . . ? C31 C36 C35 121.0(16) . . ? C46 C41 C42 117.3(16) . . ? C46 C41 P1 118.3(12) . . ? C42 C41 P1 124.3(14) . . ? C43 C42 C41 123(2) . . ? C44 C43 C42 115.7(18) . . ? C43 C44 C45 128(2) . . ? C46 C45 C44 114(2) . . ? C45 C46 C41 121.4(18) . . ? F3 B1 F4 113(2) . . ? F3 B1 F1 109.1(19) . . ? F4 B1 F1 109.4(15) . . ? F3 B1 F2 109.5(16) . . ? F4 B1 F2 107.6(19) . . ? F1 B1 F2 108.4(17) . . ? _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.902 _refine_diff_density_max 1.694 _refine_diff_density_min -2.326 _refine_diff_density_rms 0.221 #===END data_compound_4a _database_code_depnum_ccdc_archive 'CCDC 243414' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'compound 4a BF4' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32.50 H35 B Cl F4 Ir N3 P Pd' _chemical_formula_weight 919.47 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' B B 0.0013 0.0007 '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' Pd Pd -0.9988 1.0072 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.877(9) _cell_length_b 14.786(13) _cell_length_c 16.189(14) _cell_angle_alpha 83.74(4) _cell_angle_beta 79.66(3) _cell_angle_gamma 88.57(3) _cell_volume 3248(5) _cell_formula_units_Z 4 _cell_measurement_temperature 213 _cell_measurement_reflns_used 12471 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.880 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1788 _exptl_absorpt_coefficient_mu 4.829 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.348 _exptl_absorpt_correction_T_max 0.616 _exptl_special_details ; ? ; _diffrn_ambient_temperature 213 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 18654 _diffrn_reflns_av_R_equivalents 0.1828 _diffrn_reflns_av_sigmaI/netI 0.3832 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.49 _reflns_number_total 11925 _reflns_number_gt 3480 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'teXsan Ver. 1.11' _computing_publication_material 'teXsan Ver. 1.11' _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11925 _refine_ls_number_parameters 737 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2412 _refine_ls_R_factor_gt 0.0633 _refine_ls_wR_factor_ref 0.2056 _refine_ls_wR_factor_gt 0.1307 _refine_ls_goodness_of_fit_ref 0.662 _refine_ls_restrained_S_all 0.662 _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 0.69306(7) 0.18396(5) 0.51893(6) 0.0440(3) Uani 1 1 d . . . Ir2 Ir 0.82849(7) 0.16838(6) 0.90621(7) 0.0486(3) Uani 1 1 d . . . Pd1 Pd 0.76411(13) 0.46099(10) 0.53999(13) 0.0510(5) Uani 1 1 d . . . Pd2 Pd 0.79804(15) 0.45737(11) 0.85289(15) 0.0647(6) Uani 1 1 d . . . Cl1 Cl 0.6317(10) 0.4378(8) 0.0879(9) 0.168(5) Uiso 1 1 d . . . Cl2 Cl 0.4537(10) 0.3684(8) 0.0585(9) 0.178(5) Uiso 1 1 d . . . P1 P 0.8145(4) 0.1234(3) 0.4253(4) 0.0476(16) Uani 1 1 d . . . P2 P 0.6916(4) 0.0927(3) 0.9784(4) 0.0482(15) Uani 1 1 d . . . F1 F 0.7831(13) 0.6257(11) 0.2783(12) 0.108(6) Uiso 1 1 d . . . F2 F 0.6977(11) 0.5040(9) 0.2614(10) 0.080(4) Uiso 1 1 d . . . F3 F 0.7959(19) 0.5724(15) 0.1528(18) 0.164(9) Uiso 1 1 d . . . F4 F 0.6595(14) 0.6433(11) 0.2122(12) 0.114(6) Uiso 1 1 d . . . F5 F 0.1545(15) 0.2090(12) 0.3797(14) 0.124(6) Uiso 1 1 d . . . F6 F 0.2945(16) 0.1500(12) 0.3459(14) 0.126(7) Uiso 1 1 d . . . F7 F 0.1549(14) 0.0774(11) 0.3429(12) 0.113(6) Uiso 1 1 d . . . F8 F 0.1989(16) 0.2024(14) 0.2536(15) 0.139(7) Uiso 1 1 d . . . N1A N 0.8157(12) 0.2496(10) 0.5352(13) 0.050(5) Uani 1 1 d . . . N1B N 0.7192(14) 0.2520(11) 0.8684(13) 0.060(6) Uani 1 1 d . . . N2A N 0.8225(13) 0.3312(10) 0.5665(11) 0.045(4) Uani 1 1 d . . . N2B N 0.7236(16) 0.3421(11) 0.8313(13) 0.066(6) Uani 1 1 d . . . N3A N 0.8818(10) 0.4932(10) 0.5921(13) 0.048(5) Uani 1 1 d . . . N3B N 0.7003(15) 0.5126(12) 0.7760(13) 0.064(6) Uani 1 1 d . . . C1A C 0.709(2) 0.5877(16) 0.4960(18) 0.074(8) Uani 1 1 d . . . C1B C 0.885(2) 0.4193(17) 0.946(2) 0.088(10) Uani 1 1 d . . . C2A C 0.640(2) 0.5188(18) 0.498(2) 0.088(11) Uani 1 1 d . . . C2B C 0.911(3) 0.501(2) 0.909(3) 0.139(17) Uani 1 1 d . . . C3A C 0.657(2) 0.4441(17) 0.4654(19) 0.076(9) Uani 1 1 d . . . C3B C 0.857(2) 0.5708(19) 0.892(3) 0.121(15) Uani 1 1 d . . . C01A C 0.6285(17) 0.1810(13) 0.6485(17) 0.057(7) Uani 1 1 d . . . C01B C 0.9166(17) 0.1817(14) 0.7824(16) 0.054(6) Uani 1 1 d . . . C02A C 0.5820(18) 0.2527(14) 0.6074(17) 0.060(7) Uani 1 1 d . . . C02B C 0.9525(16) 0.2459(15) 0.8255(17) 0.064(8) Uani 1 1 d . . . C03A C 0.4796(18) 0.2551(15) 0.584(2) 0.076(9) Uani 1 1 d . . . C03B C 1.0466(17) 0.2324(15) 0.8644(16) 0.057(6) Uani 1 1 d . . . C04A C 0.4837(17) 0.2224(15) 0.5006(17) 0.058(7) Uani 1 1 d . . . C04B C 1.024(2) 0.1834(14) 0.9538(18) 0.071(8) Uani 1 1 d . . . C05A C 0.5650(18) 0.1565(15) 0.4739(16) 0.061(7) Uani 1 1 d . . . C05B C 0.9416(18) 0.1213(15) 0.9699(17) 0.063(7) Uani 1 1 d . . . C06A C 0.5883(19) 0.0797(14) 0.5247(16) 0.063(8) Uani 1 1 d . . . C06B C 0.9293(16) 0.0556(14) 0.9232(18) 0.061(7) Uani 1 1 d . . . C07A C 0.5346(18) 0.0510(13) 0.6100(18) 0.062(7) Uani 1 1 d . . . C07B C 0.9978(18) 0.0394(15) 0.840(2) 0.077(9) Uani 1 1 d . . . C08A C 0.576(2) 0.0913(17) 0.6771(19) 0.077(8) Uani 1 1 d . . . C08B C 0.965(2) 0.0900(17) 0.7641(19) 0.075(9) Uani 1 1 d . . . C11A C 0.9042(17) 0.2095(14) 0.5265(15) 0.053(6) Uani 1 1 d . . . C11B C 0.6287(19) 0.2204(14) 0.8644(16) 0.058(7) Uani 1 1 d . . . C12A C 0.9686(14) 0.2593(12) 0.5571(13) 0.040(5) Uani 1 1 d . . . C12B C 0.5730(16) 0.2895(13) 0.8304(14) 0.046(6) Uani 1 1 d . . . C13A C 0.9161(14) 0.3344(12) 0.5803(13) 0.038(5) Uani 1 1 d . . . C13B C 0.6362(15) 0.3626(14) 0.8090(18) 0.060(7) Uani 1 1 d . . . C14A C 0.9125(16) 0.1186(12) 0.4906(15) 0.051(6) Uani 1 1 d . . . C14B C 0.6094(16) 0.1204(14) 0.9011(16) 0.056(7) Uani 1 1 d . . . C21A C 0.9513(17) 0.4218(13) 0.6047(15) 0.052(6) Uani 1 1 d . . . C21B C 0.6225(17) 0.4564(14) 0.7768(18) 0.066(8) Uani 1 1 d . . . C22A C 1.0325(16) 0.4309(14) 0.6378(16) 0.057(7) Uani 1 1 d . . . C22B C 0.540(2) 0.4879(15) 0.7421(17) 0.073(8) Uani 1 1 d . . . C23A C 1.0537(17) 0.5141(17) 0.6605(16) 0.061(7) Uani 1 1 d . . . C23B C 0.537(3) 0.580(2) 0.711(2) 0.103(12) Uani 1 1 d . . . C24A C 0.988(2) 0.5879(16) 0.6452(19) 0.076(9) Uani 1 1 d . . . C24B C 0.610(3) 0.6350(18) 0.712(2) 0.102(13) Uani 1 1 d . . . C25A C 0.905(2) 0.5746(14) 0.6139(17) 0.070(8) Uani 1 1 d . . . C25B C 0.692(2) 0.6013(15) 0.749(2) 0.090(10) Uani 1 1 d . . . C31A C 0.8017(14) 0.0117(12) 0.3949(14) 0.042(5) Uani 1 1 d . . . C31B C 0.6918(17) -0.0295(12) 0.9991(16) 0.051(6) Uani 1 1 d . . . C32A C 0.7775(16) 0.0000(13) 0.3146(15) 0.050(6) Uani 1 1 d . . . C32B C 0.7227(17) -0.0823(14) 0.9315(17) 0.059(7) Uani 1 1 d . . . C33A C 0.7624(19) -0.0836(15) 0.2922(17) 0.064(7) Uani 1 1 d . . . C33B C 0.7297(16) -0.1818(15) 0.9473(18) 0.061(7) Uani 1 1 d . . . C34A C 0.7635(16) -0.1611(14) 0.3499(19) 0.060(7) Uani 1 1 d . . . C34B C 0.708(2) -0.2241(15) 1.025(2) 0.078(9) Uani 1 1 d . . . C35A C 0.782(2) -0.1539(14) 0.4293(19) 0.069(8) Uani 1 1 d . . . C35B C 0.6796(16) -0.1686(14) 1.0906(15) 0.047(5) Uani 1 1 d . . . C36A C 0.805(2) -0.0658(14) 0.4523(15) 0.062(7) Uani 1 1 d . . . C36B C 0.6702(16) -0.0726(13) 1.0809(18) 0.060(7) Uani 1 1 d . . . C41A C 0.8604(14) 0.1926(14) 0.3270(14) 0.044(6) Uani 1 1 d . . . C41B C 0.6244(16) 0.1260(12) 1.0731(16) 0.052(6) Uani 1 1 d . . . C42A C 0.9457(16) 0.1743(12) 0.2745(16) 0.047(6) Uani 1 1 d . . . C42B C 0.5266(13) 0.1116(13) 1.1012(15) 0.043(5) Uani 1 1 d . . . C43A C 0.9746(13) 0.2230(14) 0.2003(15) 0.047(6) Uani 1 1 d . . . C43B C 0.4748(17) 0.1310(16) 1.1803(15) 0.056(6) Uani 1 1 d . . . C44A C 0.920(2) 0.2986(14) 0.1763(18) 0.070(9) Uani 1 1 d . . . C44B C 0.525(2) 0.1676(15) 1.2320(15) 0.060(7) Uani 1 1 d . . . C45A C 0.836(2) 0.3221(15) 0.230(2) 0.073(9) Uani 1 1 d . . . C45B C 0.6191(19) 0.1883(19) 1.2096(19) 0.077(9) Uani 1 1 d . . . C46A C 0.8075(15) 0.2699(13) 0.3054(16) 0.047(6) Uani 1 1 d . . . C46B C 0.6742(19) 0.1662(15) 1.1290(19) 0.067(7) Uani 1 1 d . . . C51 C 0.572(3) 0.388(2) 0.019(3) 0.131(13) Uiso 1 1 d . . . B1 B 0.738(3) 0.589(3) 0.218(3) 0.093(12) Uiso 1 1 d . . . B2 B 0.214(4) 0.152(3) 0.317(4) 0.130(16) Uiso 1 1 d . . . H1 H 0.6977 0.6349 0.5338 0.085 Uiso 1 1 d . . . H2 H 0.7412 0.6176 0.4417 0.085 Uiso 1 1 d . . . H3 H 0.5784 0.5193 0.5402 0.108 Uiso 1 1 d . . . H4 H 0.6799 0.4466 0.4024 0.094 Uiso 1 1 d . . . H5 H 0.6152 0.3910 0.4781 0.094 Uiso 1 1 d . . . H6 H 0.6711 0.1994 0.6852 0.070 Uiso 1 1 d . . . H7 H 0.6031 0.3125 0.6165 0.071 Uiso 1 1 d . . . H8 H 0.4378 0.2147 0.6255 0.085 Uiso 1 1 d . . . H9 H 0.4524 0.3145 0.5848 0.085 Uiso 1 1 d . . . H10 H 0.4219 0.1944 0.4986 0.068 Uiso 1 1 d . . . H11 H 0.4888 0.2758 0.4584 0.068 Uiso 1 1 d . . . H12 H 0.5776 0.1492 0.4126 0.073 Uiso 1 1 d . . . H13 H 0.6153 0.0285 0.4949 0.077 Uiso 1 1 d . . . H14 H 0.4684 0.0714 0.6119 0.078 Uiso 1 1 d . . . H15 H 0.5354 -0.0135 0.6201 0.078 Uiso 1 1 d . . . H16 H 0.6207 0.0482 0.6999 0.089 Uiso 1 1 d . . . H17 H 0.5231 0.1003 0.7245 0.089 Uiso 1 1 d . . . H18 H 1.0376 0.2455 0.5606 0.049 Uiso 1 1 d . . . H19 H 0.9056 0.0665 0.5321 0.063 Uiso 1 1 d . . . H20 H 0.9775 0.1108 0.4545 0.063 Uiso 1 1 d . . . H21 H 1.0761 0.3779 0.6467 0.063 Uiso 1 1 d . . . H22 H 1.1108 0.5227 0.6842 0.071 Uiso 1 1 d . . . H23 H 1.0008 0.6487 0.6589 0.089 Uiso 1 1 d . . . H24 H 0.8623 0.6257 0.6048 0.083 Uiso 1 1 d . . . H25 H 0.7742 0.0544 0.2752 0.060 Uiso 1 1 d . . . H26 H 0.7508 -0.0894 0.2348 0.078 Uiso 1 1 d . . . H27 H 0.7498 -0.2200 0.3344 0.072 Uiso 1 1 d . . . H28 H 0.7819 -0.2096 0.4692 0.079 Uiso 1 1 d . . . H29 H 0.8198 -0.0602 0.5081 0.073 Uiso 1 1 d . . . H30 H 0.9856 0.1232 0.2919 0.055 Uiso 1 1 d . . . H31 H 1.0359 0.2079 0.1645 0.057 Uiso 1 1 d . . . H32 H 0.9384 0.3326 0.1209 0.067 Uiso 1 1 d . . . H33 H 0.7997 0.3750 0.2116 0.073 Uiso 1 1 d . . . H34 H 0.7502 0.2887 0.3440 0.052 Uiso 1 1 d . . . H35 H 0.8567 0.4141 1.0060 0.101 Uiso 1 1 d . . . H36 H 0.9309 0.3674 0.9401 0.101 Uiso 1 1 d . . . H37 H 0.9749 0.5015 0.8699 0.158 Uiso 1 1 d . . . H38 H 0.8793 0.6211 0.8538 0.136 Uiso 1 1 d . . . H39 H 0.8189 0.5962 0.9435 0.136 Uiso 1 1 d . . . H40 H 0.8803 0.2085 0.7388 0.061 Uiso 1 1 d . . . H41 H 0.9374 0.3096 0.8093 0.074 Uiso 1 1 d . . . H42 H 1.0922 0.1948 0.8301 0.067 Uiso 1 1 d . . . H43 H 1.0781 0.2886 0.8652 0.067 Uiso 1 1 d . . . H44 H 1.0810 0.1500 0.9655 0.083 Uiso 1 1 d . . . H45 H 1.0115 0.2296 0.9922 0.083 Uiso 1 1 d . . . H46 H 0.9193 0.1051 1.0308 0.076 Uiso 1 1 d . . . H47 H 0.8985 0.0015 0.9526 0.076 Uiso 1 1 d . . . H48 H 1.0627 0.0582 0.8425 0.089 Uiso 1 1 d . . . H49 H 1.0008 -0.0250 0.8338 0.089 Uiso 1 1 d . . . H50 H 0.9196 0.0537 0.7428 0.088 Uiso 1 1 d . . . H51 H 1.0204 0.1017 0.7179 0.088 Uiso 1 1 d . . . H52 H 0.5047 0.2864 0.8230 0.058 Uiso 1 1 d . . . H53 H 0.6204 0.0781 0.8573 0.068 Uiso 1 1 d . . . H54 H 0.5405 0.1103 0.9281 0.068 Uiso 1 1 d . . . H55 H 0.4880 0.4456 0.7379 0.095 Uiso 1 1 d . . . H56 H 0.4779 0.6044 0.6901 0.119 Uiso 1 1 d . . . H57 H 0.6096 0.6976 0.6870 0.111 Uiso 1 1 d . . . H58 H 0.7455 0.6431 0.7541 0.121 Uiso 1 1 d . . . H59 H 0.7399 -0.0539 0.8723 0.068 Uiso 1 1 d . . . H60 H 0.7490 -0.2190 0.8997 0.070 Uiso 1 1 d . . . H61 H 0.7130 -0.2890 1.0341 0.088 Uiso 1 1 d . . . H62 H 0.6630 -0.2005 1.1482 0.056 Uiso 1 1 d . . . H63 H 0.6522 -0.0379 1.1289 0.063 Uiso 1 1 d . . . H64 H 0.4906 0.0858 1.0619 0.053 Uiso 1 1 d . . . H65 H 0.4038 0.1174 1.1974 0.070 Uiso 1 1 d . . . H66 H 0.4912 0.1792 1.2891 0.076 Uiso 1 1 d . . . H67 H 0.6515 0.2190 1.2479 0.094 Uiso 1 1 d . . . H68 H 0.7454 0.1791 1.1158 0.081 Uiso 1 1 d . . . H69 H 0.5761 0.4282 -0.0353 0.152 Uiso 1 1 d . . . H70 H 0.6036 0.3319 0.0021 0.152 Uiso 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 0.0440(6) 0.0389(5) 0.0495(7) -0.0071(4) -0.0074(5) -0.0013(4) Ir2 0.0489(6) 0.0407(5) 0.0539(8) 0.0009(4) -0.0067(5) -0.0002(4) Pd1 0.0532(11) 0.0370(9) 0.0631(15) -0.0013(8) -0.0138(10) 0.0011(7) Pd2 0.0629(13) 0.0426(10) 0.0850(18) -0.0021(10) -0.0057(12) -0.0034(8) P1 0.050(4) 0.034(3) 0.058(5) -0.009(3) -0.006(3) -0.003(2) P2 0.047(4) 0.045(3) 0.051(5) -0.001(3) -0.005(3) -0.005(2) N1A 0.028(10) 0.039(9) 0.093(17) -0.033(9) -0.024(10) 0.014(7) N1B 0.056(13) 0.042(10) 0.070(16) 0.007(9) 0.010(11) -0.002(8) N2A 0.054(12) 0.042(9) 0.037(12) -0.003(8) -0.001(9) -0.009(8) N2B 0.090(17) 0.040(10) 0.055(15) 0.013(9) 0.008(12) 0.010(10) N3A 0.014(8) 0.042(9) 0.085(16) -0.016(9) 0.007(9) -0.001(6) N3B 0.069(14) 0.051(11) 0.060(16) 0.021(10) 0.008(12) 0.002(9) C1A 0.09(2) 0.064(16) 0.07(2) 0.008(14) -0.032(18) 0.006(14) C1B 0.13(3) 0.050(16) 0.08(3) -0.011(15) -0.01(2) 0.000(16) C2A 0.07(2) 0.067(17) 0.15(3) -0.009(17) -0.08(2) 0.013(14) C2B 0.16(4) 0.08(2) 0.21(5) -0.03(3) -0.09(4) 0.00(2) C3A 0.08(2) 0.059(15) 0.08(2) 0.025(15) -0.020(17) -0.011(14) C3B 0.09(2) 0.057(18) 0.22(5) -0.02(2) -0.03(3) -0.020(16) C01A 0.056(16) 0.039(12) 0.09(2) -0.027(12) -0.036(15) -0.004(10) C01B 0.051(15) 0.045(12) 0.062(19) -0.004(11) 0.000(13) 0.014(10) C02A 0.063(17) 0.052(14) 0.06(2) -0.024(12) 0.007(14) 0.008(11) C02B 0.038(13) 0.071(15) 0.07(2) 0.034(13) -0.013(13) -0.032(11) C03A 0.053(16) 0.061(15) 0.09(3) 0.019(15) 0.020(16) 0.002(11) C03B 0.054(16) 0.077(16) 0.044(17) -0.015(12) -0.011(13) -0.015(11) C04A 0.052(16) 0.066(15) 0.06(2) -0.032(13) -0.006(14) 0.005(11) C04B 0.10(2) 0.036(12) 0.08(2) -0.021(12) -0.015(18) 0.013(12) C05A 0.067(17) 0.062(15) 0.045(18) -0.007(12) 0.016(14) 0.004(12) C05B 0.056(16) 0.058(14) 0.07(2) -0.008(13) -0.006(15) -0.011(11) C06A 0.10(2) 0.050(12) 0.053(18) 0.011(11) -0.035(15) -0.051(12) C06B 0.036(13) 0.042(12) 0.10(2) -0.004(13) -0.010(15) 0.020(9) C07A 0.069(17) 0.037(12) 0.08(2) 0.006(12) -0.014(16) -0.005(10) C07B 0.041(15) 0.060(15) 0.14(3) -0.044(16) -0.033(18) 0.018(11) C08A 0.08(2) 0.073(17) 0.08(2) 0.007(15) -0.024(18) -0.001(14) C08B 0.060(19) 0.096(19) 0.09(2) -0.051(17) -0.046(17) 0.019(14) C11A 0.057(16) 0.057(14) 0.045(17) 0.005(11) -0.010(13) -0.001(11) C11B 0.074(18) 0.046(12) 0.053(18) 0.006(11) -0.018(14) -0.009(11) C12A 0.034(12) 0.046(11) 0.051(16) -0.021(9) -0.025(11) 0.001(8) C12B 0.049(14) 0.051(12) 0.043(16) 0.001(10) -0.021(12) -0.001(9) C13A 0.037(12) 0.042(11) 0.037(14) -0.001(9) -0.014(10) 0.003(8) C13B 0.030(12) 0.046(12) 0.10(2) -0.008(12) 0.004(14) 0.005(9) C14A 0.056(15) 0.040(11) 0.065(19) -0.006(10) -0.031(13) 0.001(9) C14B 0.046(14) 0.056(13) 0.07(2) -0.009(12) -0.031(14) 0.001(10) C21A 0.060(16) 0.048(12) 0.054(18) -0.021(11) -0.016(13) -0.001(10) C21B 0.051(15) 0.044(12) 0.09(2) 0.014(13) 0.000(15) 0.025(10) C22A 0.041(14) 0.062(14) 0.07(2) -0.030(12) -0.008(14) -0.011(10) C22B 0.09(2) 0.066(15) 0.06(2) 0.008(13) -0.027(16) 0.032(14) C23A 0.032(14) 0.096(19) 0.06(2) 0.001(14) -0.023(13) -0.019(12) C23B 0.12(3) 0.08(2) 0.09(3) 0.029(19) 0.00(2) 0.050(19) C24A 0.065(19) 0.075(18) 0.10(3) -0.016(15) -0.033(18) -0.010(14) C24B 0.10(3) 0.054(17) 0.13(3) 0.045(18) 0.00(2) 0.007(16) C25A 0.11(2) 0.048(13) 0.06(2) -0.002(12) -0.036(18) 0.001(13) C25B 0.12(3) 0.039(13) 0.10(3) -0.013(14) 0.02(2) 0.020(14) C31A 0.034(12) 0.041(11) 0.047(16) 0.001(10) 0.003(11) 0.007(8) C31B 0.068(16) 0.027(10) 0.057(18) -0.020(10) -0.001(13) 0.008(9) C32A 0.051(15) 0.052(12) 0.046(17) -0.001(11) -0.007(12) 0.014(10) C32B 0.055(15) 0.048(13) 0.08(2) -0.010(12) -0.025(15) 0.008(10) C33A 0.079(19) 0.055(14) 0.054(19) -0.024(12) 0.012(15) -0.011(12) C33B 0.037(13) 0.063(15) 0.08(2) -0.004(14) -0.012(14) 0.002(10) C34A 0.038(14) 0.049(13) 0.09(2) -0.023(13) 0.007(15) 0.002(9) C34B 0.09(2) 0.044(13) 0.11(3) 0.003(15) -0.05(2) -0.017(13) C35A 0.09(2) 0.039(12) 0.08(2) -0.021(13) -0.003(18) 0.009(11) C35B 0.057(15) 0.049(12) 0.037(15) -0.007(10) -0.011(12) -0.004(10) C36A 0.09(2) 0.054(14) 0.042(17) -0.011(11) -0.017(15) -0.011(12) C36B 0.056(15) 0.031(11) 0.09(2) -0.001(11) 0.002(14) -0.010(9) C41A 0.014(11) 0.073(14) 0.049(16) 0.000(11) -0.021(11) -0.014(9) C41B 0.048(14) 0.038(11) 0.070(19) 0.011(11) -0.025(14) 0.004(9) C42A 0.046(14) 0.040(11) 0.061(19) -0.004(11) -0.030(14) 0.003(9) C42B 0.013(10) 0.058(12) 0.063(18) -0.021(11) -0.009(11) 0.003(8) C43A 0.019(10) 0.060(13) 0.056(17) -0.016(12) 0.015(11) 0.006(8) C43B 0.046(15) 0.097(18) 0.027(15) -0.021(12) -0.006(12) 0.014(12) C44A 0.10(2) 0.038(12) 0.08(2) 0.000(12) -0.056(19) -0.012(13) C44B 0.09(2) 0.063(14) 0.033(16) -0.024(12) -0.019(15) 0.039(13) C45A 0.08(2) 0.042(13) 0.11(3) -0.025(15) -0.05(2) 0.006(13) C45B 0.028(15) 0.14(2) 0.08(2) -0.040(18) -0.032(16) -0.001(14) C46A 0.033(12) 0.048(12) 0.059(18) 0.000(11) -0.004(12) 0.001(9) C46B 0.069(19) 0.063(15) 0.06(2) -0.012(14) 0.001(16) -0.001(12) _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 N1A 2.052(15) . ? Ir1 C05A 2.10(3) . ? Ir1 C01A 2.12(3) . ? Ir1 C06A 2.128(17) . ? Ir1 C02A 2.21(2) . ? Ir1 P1 2.290(7) . ? Ir2 N1B 2.068(18) . ? Ir2 C05B 2.09(3) . ? Ir2 C01B 2.14(3) . ? Ir2 C06B 2.176(19) . ? Ir2 C02B 2.224(19) . ? Ir2 P2 2.292(6) . ? Pd1 N3A 2.056(17) . ? Pd1 C2A 2.09(2) . ? Pd1 N2A 2.096(16) . ? Pd1 C1A 2.11(2) . ? Pd1 C3A 2.12(3) . ? Pd2 N3B 2.09(2) . ? Pd2 C2B 2.10(4) . ? Pd2 C3B 2.10(3) . ? Pd2 N2B 2.11(2) . ? Pd2 C1B 2.12(3) . ? Cl1 C51 1.74(4) . ? Cl2 C51 1.67(4) . ? P1 C31A 1.80(2) . ? P1 C41A 1.82(2) . ? P1 C14A 1.86(2) . ? P2 C41B 1.76(3) . ? P2 C31B 1.801(19) . ? P2 C14B 1.85(2) . ? F1 B1 1.42(4) . ? F2 B1 1.44(4) . ? F3 B1 1.25(5) . ? F4 B1 1.35(4) . ? F5 B2 1.50(5) . ? F6 B2 1.28(5) . ? F7 B2 1.37(5) . ? F8 B2 1.25(5) . ? N1A C11A 1.34(3) . ? N1A N2A 1.37(2) . ? N1B C11B 1.37(3) . ? N1B N2B 1.40(2) . ? N2A C13A 1.36(2) . ? N2B C13B 1.35(3) . ? N3A C25A 1.35(3) . ? N3A C21A 1.43(2) . ? N3B C25B 1.35(3) . ? N3B C21B 1.38(3) . ? C1A C2A 1.41(3) . ? C01A C02A 1.40(3) . ? C01A C08A 1.52(3) . ? C01B C02B 1.39(3) . ? C01B C08B 1.53(3) . ? C1B C2B 1.31(4) . ? C2A C3A 1.28(3) . ? C02A C03A 1.53(3) . ? C2B C3B 1.30(4) . ? C02B C03B 1.55(3) . ? C03A C04A 1.47(4) . ? C03B C04B 1.53(3) . ? C04A C05A 1.51(3) . ? C04B C05B 1.45(3) . ? C05A C06A 1.39(3) . ? C05B C06B 1.33(3) . ? C06A C07A 1.47(3) . ? C06B C07B 1.54(4) . ? C07A C08A 1.50(3) . ? C07B C08B 1.51(4) . ? C11A C12A 1.36(3) . ? C11A C14A 1.51(3) . ? C11B C12B 1.39(3) . ? C11B C14B 1.54(3) . ? C12A C13A 1.36(3) . ? C12B C13B 1.38(3) . ? C13A C21A 1.51(3) . ? C13B C21B 1.45(3) . ? C21A C22A 1.35(3) . ? C21B C22B 1.41(3) . ? C22A C23A 1.37(3) . ? C22B C23B 1.40(3) . ? C23A C24A 1.44(3) . ? C23B C24B 1.32(4) . ? C24A C25A 1.36(3) . ? C24B C25B 1.42(4) . ? C31A C36A 1.40(3) . ? C31A C32A 1.43(3) . ? C31B C36B 1.39(3) . ? C31B C32B 1.41(3) . ? C32A C33A 1.36(3) . ? C32B C33B 1.47(3) . ? C33A C34A 1.40(3) . ? C33B C34B 1.32(4) . ? C34A C35A 1.37(3) . ? C34B C35B 1.41(4) . ? C35A C36A 1.45(3) . ? C35B C36B 1.42(3) . ? C41A C42A 1.37(3) . ? C41A C46A 1.39(3) . ? C41B C42B 1.37(3) . ? C41B C46B 1.42(3) . ? C42A C43A 1.33(3) . ? C42B C43B 1.41(3) . ? C43A C44A 1.40(3) . ? C43B C44B 1.34(3) . ? C44A C45A 1.39(4) . ? C44B C45B 1.33(3) . ? C45A C46A 1.37(3) . ? C45B C46B 1.45(4) . ? 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 N1A Ir1 C05A 160.6(8) . . ? N1A Ir1 C01A 92.9(8) . . ? C05A Ir1 C01A 97.1(9) . . ? N1A Ir1 C06A 160.7(8) . . ? C05A Ir1 C06A 38.5(8) . . ? C01A Ir1 C06A 81.3(9) . . ? N1A Ir1 C02A 99.0(8) . . ? C05A Ir1 C02A 79.5(9) . . ? C01A Ir1 C02A 37.5(8) . . ? C06A Ir1 C02A 87.6(10) . . ? N1A Ir1 P1 77.3(5) . . ? C05A Ir1 P1 103.2(7) . . ? C01A Ir1 P1 144.4(6) . . ? C06A Ir1 P1 96.8(8) . . ? C02A Ir1 P1 175.5(6) . . ? N1B Ir2 C05B 159.9(9) . . ? N1B Ir2 C01B 92.9(8) . . ? C05B Ir2 C01B 95.9(10) . . ? N1B Ir2 C06B 164.0(9) . . ? C05B Ir2 C06B 36.1(9) . . ? C01B Ir2 C06B 81.2(9) . . ? N1B Ir2 C02B 95.9(7) . . ? C05B Ir2 C02B 80.7(9) . . ? C01B Ir2 C02B 37.0(9) . . ? C06B Ir2 C02B 88.4(9) . . ? N1B Ir2 P2 79.2(5) . . ? C05B Ir2 P2 105.1(7) . . ? C01B Ir2 P2 139.2(7) . . ? C06B Ir2 P2 95.5(6) . . ? C02B Ir2 P2 174.0(6) . . ? N3A Pd1 C2A 141.8(9) . . ? N3A Pd1 N2A 79.3(6) . . ? C2A Pd1 N2A 138.4(9) . . ? N3A Pd1 C1A 104.5(8) . . ? C2A Pd1 C1A 39.2(9) . . ? N2A Pd1 C1A 172.2(9) . . ? N3A Pd1 C3A 168.8(8) . . ? C2A Pd1 C3A 35.3(9) . . ? N2A Pd1 C3A 106.1(8) . . ? C1A Pd1 C3A 68.9(9) . . ? N3B Pd2 C2B 138.9(11) . . ? N3B Pd2 C3B 104.5(12) . . ? C2B Pd2 C3B 36.0(11) . . ? N3B Pd2 N2B 77.0(7) . . ? C2B Pd2 N2B 144.0(11) . . ? C3B Pd2 N2B 171.1(13) . . ? N3B Pd2 C1B 169.2(10) . . ? C2B Pd2 C1B 36.4(11) . . ? C3B Pd2 C1B 68.1(12) . . ? N2B Pd2 C1B 109.1(9) . . ? C31A P1 C41A 104.7(11) . . ? C31A P1 C14A 108.1(9) . . ? C41A P1 C14A 107.1(9) . . ? C31A P1 Ir1 120.3(7) . . ? C41A P1 Ir1 117.7(8) . . ? C14A P1 Ir1 97.8(8) . . ? C41B P2 C31B 102.3(10) . . ? C41B P2 C14B 103.9(11) . . ? C31B P2 C14B 106.1(10) . . ? C41B P2 Ir2 122.6(7) . . ? C31B P2 Ir2 120.7(8) . . ? C14B P2 Ir2 98.8(8) . . ? C11A N1A N2A 108.3(17) . . ? C11A N1A Ir1 122.1(13) . . ? N2A N1A Ir1 128.9(12) . . ? C11B N1B N2B 106.6(17) . . ? C11B N1B Ir2 122.6(13) . . ? N2B N1B Ir2 130.0(14) . . ? C13A N2A N1A 105.2(15) . . ? C13A N2A Pd1 112.3(11) . . ? N1A N2A Pd1 133.3(13) . . ? C13B N2B N1B 107.3(18) . . ? C13B N2B Pd2 113.0(13) . . ? N1B N2B Pd2 132.5(16) . . ? C25A N3A C21A 114.7(19) . . ? C25A N3A Pd1 128.4(15) . . ? C21A N3A Pd1 116.8(13) . . ? C25B N3B C21B 118(2) . . ? C25B N3B Pd2 125.9(19) . . ? C21B N3B Pd2 113.0(13) . . ? C2A C1A Pd1 69.9(13) . . ? C02A C01A C08A 120(2) . . ? C02A C01A Ir1 74.8(16) . . ? C08A C01A Ir1 109.2(16) . . ? C02B C01B C08B 125(2) . . ? C02B C01B Ir2 74.6(15) . . ? C08B C01B Ir2 109.5(17) . . ? C2B C1B Pd2 71(2) . . ? C3A C2A C1A 126(3) . . ? C3A C2A Pd1 73.4(16) . . ? C1A C2A Pd1 71.0(14) . . ? C01A C02A C03A 129(2) . . ? C01A C02A Ir1 67.7(15) . . ? C03A C02A Ir1 113.4(18) . . ? C3B C2B C1B 129(4) . . ? C3B C2B Pd2 72(2) . . ? C1B C2B Pd2 73(2) . . ? C01B C02B C03B 124(2) . . ? C01B C02B Ir2 68.4(12) . . ? C03B C02B Ir2 110.8(14) . . ? C04A C03A C02A 110(2) . . ? C2A C3A Pd1 71.3(16) . . ? C2B C3B Pd2 72(2) . . ? C04B C03B C02B 111(2) . . ? C03A C04A C05A 117(2) . . ? C05B C04B C03B 115(2) . . ? C06A C05A C04A 124(2) . . ? C06A C05A Ir1 71.7(13) . . ? C04A C05A Ir1 111.7(16) . . ? C06B C05B C04B 125(3) . . ? C06B C05B Ir2 75.3(15) . . ? C04B C05B Ir2 112.5(17) . . ? C05A C06A C07A 124(2) . . ? C05A C06A Ir1 69.8(12) . . ? C07A C06A Ir1 114.6(15) . . ? C05B C06B C07B 124(2) . . ? C05B C06B Ir2 68.5(14) . . ? C07B C06B Ir2 112.2(16) . . ? C06A C07A C08A 112.5(19) . . ? C08B C07B C06B 113(2) . . ? C07A C08A C01A 115(2) . . ? C07B C08B C01B 113(2) . . ? N1A C11A C12A 111(2) . . ? N1A C11A C14A 116.5(19) . . ? C12A C11A C14A 133(2) . . ? N1B C11B C12B 110.3(18) . . ? N1B C11B C14B 114.9(18) . . ? C12B C11B C14B 135(2) . . ? C13A C12A C11A 104.0(18) . . ? C13B C12B C11B 104(2) . . ? N2A C13A C12A 111.8(16) . . ? N2A C13A C21A 118.3(17) . . ? C12A C13A C21A 129.1(19) . . ? N2B C13B C12B 111.2(19) . . ? N2B C13B C21B 115.9(18) . . ? C12B C13B C21B 133(2) . . ? C11A C14A P1 103.9(13) . . ? C11B C14B P2 107.1(14) . . ? C22A C21A N3A 124.7(18) . . ? C22A C21A C13A 125.6(19) . . ? N3A C21A C13A 109.5(18) . . ? N3B C21B C22B 121(2) . . ? N3B C21B C13B 114.8(19) . . ? C22B C21B C13B 124(2) . . ? C21A C22A C23A 119(2) . . ? C23B C22B C21B 118(3) . . ? C22A C23A C24A 117(2) . . ? C24B C23B C22B 121(3) . . ? C25A C24A C23A 121(2) . . ? C23B C24B C25B 120(2) . . ? N3A C25A C24A 123(2) . . ? N3B C25B C24B 122(3) . . ? C36A C31A C32A 117.9(18) . . ? C36A C31A P1 120.9(18) . . ? C32A C31A P1 120.8(14) . . ? C36B C31B C32B 119.2(19) . . ? C36B C31B P2 121.5(17) . . ? C32B C31B P2 119.1(18) . . ? C33A C32A C31A 122(2) . . ? C31B C32B C33B 120(2) . . ? C32A C33A C34A 121(2) . . ? C34B C33B C32B 121(3) . . ? C35A C34A C33A 120(2) . . ? C33B C34B C35B 117(2) . . ? C34A C35A C36A 120(2) . . ? C34B C35B C36B 126(2) . . ? C31A C36A C35A 120(2) . . ? C31B C36B C35B 117(2) . . ? C42A C41A C46A 118(2) . . ? C42A C41A P1 123.6(16) . . ? C46A C41A P1 118.1(18) . . ? C42B C41B C46B 115(2) . . ? C42B C41B P2 125.2(18) . . ? C46B C41B P2 119.2(19) . . ? C43A C42A C41A 122.3(19) . . ? C41B C42B C43B 125(2) . . ? C42A C43A C44A 120(2) . . ? C44B C43B C42B 118(2) . . ? C45A C44A C43A 119(2) . . ? C45B C44B C43B 122(3) . . ? C46A C45A C44A 119(2) . . ? C44B C45B C46B 121(2) . . ? C45A C46A C41A 121(2) . . ? C41B C46B C45B 119(2) . . ? Cl2 C51 Cl1 113(3) . . ? F3 B1 F4 120(4) . . ? F3 B1 F1 114(3) . . ? F4 B1 F1 104(3) . . ? F3 B1 F2 109(3) . . ? F4 B1 F2 105(3) . . ? F1 B1 F2 104(3) . . ? F8 B2 F6 124(5) . . ? F8 B2 F7 117(5) . . ? F6 B2 F7 116(4) . . ? F8 B2 F5 95(4) . . ? F6 B2 F5 99(4) . . ? F7 B2 F5 94(4) . . ? _diffrn_measured_fraction_theta_max 0.803 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.803 _refine_diff_density_max 0.809 _refine_diff_density_min -1.073 _refine_diff_density_rms 0.155 #===END data_compound_5 _database_code_depnum_ccdc_archive 'CCDC 243415' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'compound 5' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H29 Ir N3 P' _chemical_formula_weight 642.72 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' 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 triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.341(5) _cell_length_b 9.958(5) _cell_length_c 13.571(9) _cell_angle_alpha 92.45(5) _cell_angle_beta 102.39(4) _cell_angle_gamma 98.18(2) _cell_volume 1216.9(13) _cell_formula_units_Z 2 _cell_measurement_temperature 213 _cell_measurement_reflns_used 4059 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.754 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 5.575 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.344 _exptl_absorpt_correction_T_max 0.572 _exptl_special_details ; ? ; _diffrn_ambient_temperature 213 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 4773 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0601 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3595 _reflns_number_gt 2686 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'teXsan Ver. 1.11' _computing_publication_material 'teXsan Ver. 1.11' _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3595 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0799 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1468 _refine_ls_wR_factor_gt 0.1363 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _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 0.09785(5) 0.79731(4) 0.36593(4) 0.04135(18) Uani 1 1 d . . . P1 P -0.0728(3) 0.7090(3) 0.2222(2) 0.0402(7) Uani 1 1 d . . . N1 N 0.1407(10) 0.9409(10) 0.2662(8) 0.047(3) Uani 1 1 d . . . N2 N 0.2090(10) 1.0724(9) 0.2946(8) 0.044(2) Uani 1 1 d . . . N3 N 0.2665(11) 1.3182(10) 0.1099(8) 0.049(2) Uani 1 1 d . . . C01 C 0.3025(12) 0.8828(12) 0.4769(10) 0.047(3) Uani 1 1 d . . . C02 C 0.1834(15) 0.9223(11) 0.5069(9) 0.048(3) Uani 1 1 d . . . C03 C 0.1189(15) 0.8632(12) 0.5949(11) 0.051(3) Uani 1 1 d . . . C04 C -0.0057(15) 0.7426(14) 0.5607(12) 0.058(4) Uani 1 1 d . . . C05 C 0.0014(13) 0.6679(11) 0.4659(10) 0.045(3) Uani 1 1 d . . . C06 C 0.1324(15) 0.6209(12) 0.4466(11) 0.055(3) Uani 1 1 d . . . C07 C 0.2766(15) 0.6429(14) 0.5268(11) 0.057(3) Uani 1 1 d . . . C08 C 0.3834(15) 0.7739(15) 0.5192(11) 0.060(4) Uani 1 1 d . . . C11 C 0.0957(11) 0.9163(11) 0.1653(8) 0.037(2) Uani 1 1 d . . . C12 C 0.1396(13) 1.0334(12) 0.1215(10) 0.045(3) Uani 1 1 d . . . C13 C 0.2082(11) 1.1270(11) 0.2052(10) 0.042(3) Uani 1 1 d . . . C14 C 0.0191(12) 0.7772(11) 0.1220(9) 0.044(3) Uani 1 1 d . . . C21 C 0.2673(12) 1.2724(12) 0.2027(10) 0.044(3) Uani 1 1 d . . . C22 C 0.3190(14) 1.3579(12) 0.2916(11) 0.052(3) Uani 1 1 d . . . C23 C 0.3687(15) 1.4928(14) 0.2841(13) 0.063(4) Uani 1 1 d . . . C24 C 0.3623(14) 1.5411(12) 0.1892(13) 0.058(4) Uani 1 1 d . . . C25 C 0.3106(14) 1.4484(13) 0.1049(12) 0.058(4) Uani 1 1 d . . . C31 C -0.1393(11) 0.5288(11) 0.1872(9) 0.041(3) Uani 1 1 d . . . C32 C -0.2766(14) 0.4699(13) 0.1994(13) 0.059(4) Uani 1 1 d . . . C33 C -0.3237(14) 0.3319(13) 0.1756(13) 0.063(4) Uani 1 1 d . . . C34 C -0.2379(14) 0.2525(12) 0.1431(11) 0.054(3) Uani 1 1 d . . . C35 C -0.1009(15) 0.3091(13) 0.1314(12) 0.058(3) Uani 1 1 d . . . C36 C -0.0525(13) 0.4457(12) 0.1549(13) 0.059(4) Uani 1 1 d . . . C41 C -0.2413(13) 0.7843(11) 0.2076(11) 0.047(3) Uani 1 1 d . . . C42 C -0.3235(12) 0.8072(13) 0.1135(10) 0.048(3) Uani 1 1 d . . . C43 C -0.4497(13) 0.8706(13) 0.1069(12) 0.057(4) Uani 1 1 d . . . C44 C -0.4952(14) 0.9080(13) 0.1932(14) 0.061(4) Uani 1 1 d . . . C45 C -0.4160(14) 0.8858(14) 0.2846(12) 0.060(4) Uani 1 1 d . . . C46 C -0.2890(12) 0.8244(12) 0.2941(11) 0.050(3) Uani 1 1 d . . . H1 H 0.1153 0.5363 0.4036 0.065 Uiso 1 1 d . . . H2 H -0.0905 0.6118 0.4325 0.053 Uiso 1 1 d . . . H3 H -0.0995 0.7756 0.5518 0.069 Uiso 1 1 d . . . H4 H -0.0015 0.6809 0.6132 0.069 Uiso 1 1 d . . . H5 H 0.0821 0.9341 0.6272 0.062 Uiso 1 1 d . . . H6 H 0.1973 0.8347 0.6425 0.062 Uiso 1 1 d . . . H7 H 0.1764 1.0163 0.4997 0.056 Uiso 1 1 d . . . H8 H 0.3621 0.9545 0.4527 0.056 Uiso 1 1 d . . . H9 H 0.4505 0.7541 0.4772 0.071 Uiso 1 1 d . . . H10 H 0.4440 0.8060 0.5854 0.071 Uiso 1 1 d . . . H11 H 0.2514 0.6469 0.5914 0.072 Uiso 1 1 d . . . H12 H 0.3268 0.5655 0.5225 0.072 Uiso 1 1 d . . . H13 H 0.1267 1.0491 0.0513 0.055 Uiso 1 1 d . . . H14 H 0.0904 0.7227 0.1097 0.054 Uiso 1 1 d . . . H15 H -0.0507 0.7823 0.0613 0.054 Uiso 1 1 d . . . H16 H 0.3200 1.3219 0.3569 0.063 Uiso 1 1 d . . . H17 H 0.4093 1.5542 0.3438 0.076 Uiso 1 1 d . . . H18 H 0.3931 1.6345 0.1796 0.068 Uiso 1 1 d . . . H19 H 0.3053 1.4812 0.0392 0.068 Uiso 1 1 d . . . H20 H -0.3388 0.5251 0.2263 0.068 Uiso 1 1 d . . . H21 H -0.4214 0.2921 0.1769 0.078 Uiso 1 1 d . . . H22 H -0.2706 0.1575 0.1276 0.063 Uiso 1 1 d . . . H23 H -0.0393 0.2527 0.1074 0.072 Uiso 1 1 d . . . H24 H 0.0438 0.4839 0.1473 0.069 Uiso 1 1 d . . . H25 H -0.2923 0.7798 0.0532 0.062 Uiso 1 1 d . . . H26 H -0.5048 0.8880 0.0422 0.070 Uiso 1 1 d . . . H27 H -0.5825 0.9489 0.1894 0.072 Uiso 1 1 d . . . H28 H -0.4465 0.9131 0.3459 0.074 Uiso 1 1 d . . . H29 H -0.2347 0.8067 0.3599 0.061 Uiso 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 0.0443(3) 0.0376(2) 0.0403(3) 0.00620(18) 0.00759(17) 0.00171(15) P1 0.0391(14) 0.0380(13) 0.0404(19) 0.0034(12) 0.0047(11) 0.0024(11) N1 0.048(5) 0.046(5) 0.044(7) 0.018(5) 0.005(4) -0.002(4) N2 0.047(5) 0.038(5) 0.044(7) 0.007(4) 0.008(4) 0.002(4) N3 0.059(6) 0.046(5) 0.042(7) 0.004(5) 0.019(4) -0.002(4) C01 0.038(5) 0.051(6) 0.040(8) -0.008(5) -0.011(5) -0.003(5) C02 0.075(8) 0.035(5) 0.031(7) -0.001(5) 0.008(5) 0.005(5) C03 0.068(8) 0.040(6) 0.048(9) 0.003(6) 0.017(6) 0.010(5) C04 0.068(8) 0.054(7) 0.059(10) 0.015(7) 0.026(7) 0.010(6) C05 0.057(7) 0.040(5) 0.043(8) 0.008(5) 0.027(5) 0.001(5) C06 0.071(8) 0.036(6) 0.054(9) 0.010(6) 0.009(6) 0.002(5) C07 0.066(8) 0.054(7) 0.049(9) 0.017(6) 0.006(6) 0.014(6) C08 0.061(8) 0.068(8) 0.042(8) 0.006(7) -0.004(6) 0.004(6) C11 0.035(5) 0.044(5) 0.031(6) 0.008(5) 0.005(4) 0.000(4) C12 0.057(7) 0.042(6) 0.038(7) 0.010(5) 0.013(5) 0.008(5) C13 0.040(5) 0.040(5) 0.051(8) 0.004(5) 0.020(5) 0.008(4) C14 0.049(6) 0.041(5) 0.039(7) 0.011(5) 0.007(5) 0.001(5) C21 0.040(5) 0.045(6) 0.048(8) 0.007(5) 0.009(5) 0.007(4) C22 0.055(7) 0.041(6) 0.055(9) 0.004(6) 0.007(6) -0.001(5) C23 0.060(8) 0.051(7) 0.069(11) 0.000(7) 0.008(7) -0.008(6) C24 0.050(7) 0.036(6) 0.086(12) 0.003(6) 0.014(6) -0.003(5) C25 0.059(7) 0.044(6) 0.069(11) 0.014(7) 0.018(6) -0.001(5) C31 0.039(5) 0.045(6) 0.040(7) 0.008(5) 0.010(4) 0.013(4) C32 0.049(6) 0.047(6) 0.081(11) -0.005(7) 0.021(6) 0.002(5) C33 0.051(7) 0.046(7) 0.090(12) 0.002(7) 0.020(7) -0.008(5) C34 0.058(7) 0.038(6) 0.059(10) 0.002(6) 0.004(6) -0.001(5) C35 0.065(8) 0.047(7) 0.068(11) 0.003(7) 0.024(7) 0.015(6) C36 0.047(6) 0.043(6) 0.087(12) 0.002(7) 0.021(6) 0.004(5) C41 0.048(6) 0.034(5) 0.058(9) -0.005(5) 0.013(5) 0.000(4) C42 0.046(6) 0.052(6) 0.044(8) 0.014(6) 0.004(5) 0.010(5) C43 0.043(6) 0.052(7) 0.071(10) 0.016(7) -0.001(6) 0.006(5) C44 0.048(7) 0.045(6) 0.088(12) 0.008(7) 0.011(7) 0.007(5) C45 0.051(7) 0.066(8) 0.067(11) -0.008(7) 0.021(7) 0.009(6) C46 0.042(6) 0.048(6) 0.058(9) -0.005(6) 0.009(5) 0.006(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 N1 2.067(9) . ? Ir1 C06 2.136(11) . ? Ir1 C05 2.158(10) . ? Ir1 C02 2.170(13) . ? Ir1 C01 2.200(10) . ? Ir1 P1 2.289(3) . ? P1 C41 1.815(12) . ? P1 C31 1.821(12) . ? P1 C14 1.860(12) . ? N1 C11 1.345(15) . ? N1 N2 1.372(13) . ? N2 C13 1.350(15) . ? N3 C25 1.313(15) . ? N3 C21 1.357(15) . ? C01 C02 1.365(19) . ? C01 C08 1.475(18) . ? C02 C03 1.550(17) . ? C03 C04 1.528(19) . ? C04 C05 1.48(2) . ? C05 C06 1.440(19) . ? C06 C07 1.521(18) . ? C07 C08 1.547(18) . ? C11 C12 1.381(14) . ? C11 C14 1.498(15) . ? C12 C13 1.414(18) . ? C13 C21 1.479(15) . ? C21 C22 1.400(19) . ? C22 C23 1.373(17) . ? C23 C24 1.39(2) . ? C24 C25 1.39(2) . ? C31 C36 1.359(17) . ? C31 C32 1.379(16) . ? C32 C33 1.384(18) . ? C33 C34 1.33(2) . ? C34 C35 1.368(17) . ? C35 C36 1.372(17) . ? C41 C42 1.388(17) . ? C41 C46 1.404(19) . ? C42 C43 1.403(17) . ? C43 C44 1.38(2) . ? C44 C45 1.35(2) . ? C45 C46 1.395(17) . ? 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 Ir1 C06 155.0(5) . . ? N1 Ir1 C05 165.5(4) . . ? C06 Ir1 C05 39.2(5) . . ? N1 Ir1 C02 99.0(4) . . ? C06 Ir1 C02 89.1(5) . . ? C05 Ir1 C02 80.8(5) . . ? N1 Ir1 C01 91.4(4) . . ? C06 Ir1 C01 81.1(5) . . ? C05 Ir1 C01 96.6(5) . . ? C02 Ir1 C01 36.4(5) . . ? N1 Ir1 P1 79.1(3) . . ? C06 Ir1 P1 102.5(4) . . ? C05 Ir1 P1 95.3(4) . . ? C02 Ir1 P1 156.5(4) . . ? C01 Ir1 P1 164.8(4) . . ? C41 P1 C31 103.9(5) . . ? C41 P1 C14 105.2(6) . . ? C31 P1 C14 107.4(6) . . ? C41 P1 Ir1 111.7(4) . . ? C31 P1 Ir1 125.5(4) . . ? C14 P1 Ir1 101.5(4) . . ? C11 N1 N2 112.7(9) . . ? C11 N1 Ir1 122.7(7) . . ? N2 N1 Ir1 124.5(8) . . ? C13 N2 N1 103.0(10) . . ? C25 N3 C21 117.8(12) . . ? C02 C01 C08 125.4(12) . . ? C02 C01 Ir1 70.6(7) . . ? C08 C01 Ir1 110.9(8) . . ? C01 C02 C03 124.4(11) . . ? C01 C02 Ir1 73.0(7) . . ? C03 C02 Ir1 112.2(8) . . ? C04 C03 C02 113.5(12) . . ? C05 C04 C03 113.6(11) . . ? C06 C05 C04 124.6(12) . . ? C06 C05 Ir1 69.6(6) . . ? C04 C05 Ir1 112.6(8) . . ? C05 C06 C07 120.9(14) . . ? C05 C06 Ir1 71.2(6) . . ? C07 C06 Ir1 112.6(8) . . ? C06 C07 C08 114.4(10) . . ? C01 C08 C07 111.8(11) . . ? N1 C11 C12 107.8(10) . . ? N1 C11 C14 119.3(9) . . ? C12 C11 C14 132.8(11) . . ? C11 C12 C13 103.7(10) . . ? N2 C13 C12 112.6(9) . . ? N2 C13 C21 120.2(11) . . ? C12 C13 C21 127.1(11) . . ? C11 C14 P1 104.2(9) . . ? N3 C21 C22 122.2(11) . . ? N3 C21 C13 116.4(11) . . ? C22 C21 C13 121.4(11) . . ? C23 C22 C21 118.6(13) . . ? C22 C23 C24 119.4(14) . . ? C23 C24 C25 118.1(11) . . ? N3 C25 C24 123.9(13) . . ? C36 C31 C32 117.5(11) . . ? C36 C31 P1 121.6(8) . . ? C32 C31 P1 120.8(9) . . ? C31 C32 C33 120.1(13) . . ? C34 C33 C32 121.5(12) . . ? C33 C34 C35 119.1(11) . . ? C34 C35 C36 120.1(12) . . ? C31 C36 C35 121.7(11) . . ? C42 C41 C46 118.4(11) . . ? C42 C41 P1 122.2(11) . . ? C46 C41 P1 119.4(10) . . ? C41 C42 C43 119.8(13) . . ? C44 C43 C42 120.7(12) . . ? C45 C44 C43 119.7(13) . . ? C44 C45 C46 121.2(15) . . ? C45 C46 C41 120.2(13) . . ? _diffrn_measured_fraction_theta_max 0.646 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.646 _refine_diff_density_max 1.213 _refine_diff_density_min -2.076 _refine_diff_density_rms 0.181 #===END data_compound_8 _database_code_depnum_ccdc_archive 'CCDC 243416' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'compound 8' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H31 Cl2 Ir N3 P' _chemical_formula_weight 727.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.130(18) _cell_length_b 14.56(2) _cell_length_c 18.75(2) _cell_angle_alpha 78.51(6) _cell_angle_beta 85.37(6) _cell_angle_gamma 71.38(6) _cell_volume 2823(7) _cell_formula_units_Z 4 _cell_measurement_reflns_used 11494 _cell_measurement_temperature 213 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 #_cell_measurement_temperature 213 _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.712 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 5.001 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.604 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 213 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 14895 _diffrn_reflns_av_R_equivalents 0.1296 _diffrn_reflns_av_sigmaI/netI 0.3247 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9937 _reflns_number_gt 2858 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'teXsan Ver. 1.11' _computing_publication_material 'teXsan Ver. 1.11' _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9937 _refine_ls_number_parameters 627 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2282 _refine_ls_R_factor_gt 0.0727 _refine_ls_wR_factor_ref 0.2076 _refine_ls_wR_factor_gt 0.1586 _refine_ls_goodness_of_fit_ref 0.694 _refine_ls_restrained_S_all 0.694 _refine_ls_shift/su_max 0.006 _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 -0.19169(9) 0.18753(7) 0.52272(5) 0.0638(3) Uani 1 1 d . . . Ir2 Ir 0.23809(8) 0.16863(6) 0.09755(5) 0.0515(3) Uani 1 1 d . . . Cl1 Cl 0.5857(8) 0.2056(7) 0.3648(5) 0.127(3) Uiso 1 1 d . . . Cl2 Cl 0.5389(8) 0.4162(6) 0.3319(5) 0.113(3) Uiso 1 1 d . . . Cl3 Cl 0.0187(15) 0.4761(13) 0.3651(9) 0.241(6) Uiso 1 1 d . . . Cl4 Cl 0.250(2) 0.3566(15) 0.4059(12) 0.316(10) Uiso 1 1 d . . . P1 P 0.0733(5) 0.1605(4) 0.1871(3) 0.0525(14) Uani 1 1 d . . . P2 P 0.3252(6) 0.2803(4) 0.1284(3) 0.0545(15) Uani 1 1 d . . . N1A N 0.0014(16) 0.1719(11) 0.3898(9) 0.054(4) Uani 1 1 d . . . N1B N 0.3637(16) 0.0767(10) 0.1719(8) 0.054(4) Uani 1 1 d . . . N2A N -0.0826(16) 0.1338(15) 0.4380(9) 0.061(5) Uani 1 1 d . . . N2B N 0.3955(16) -0.0232(13) 0.1897(10) 0.055(4) Uani 1 1 d . . . N3A N -0.2390(18) 0.0602(13) 0.5189(10) 0.070(6) Uani 1 1 d . . . N3B N 0.640(2) -0.1789(15) 0.3241(11) 0.086(7) Uani 1 1 d . . . C1A C -0.184(2) 0.3357(17) 0.4946(12) 0.072(7) Uani 1 1 d . . . C1B C 0.183(2) 0.2765(16) -0.0097(12) 0.070(7) Uani 1 1 d . . . C2A C -0.086(3) 0.2759(18) 0.5468(18) 0.111(13) Uani 1 1 d . . . C2B C 0.0817(18) 0.2371(14) 0.0249(11) 0.053(5) Uiso 1 1 d . . . C3A C -0.091(3) 0.2783(16) 0.6257(15) 0.096(10) Uani 1 1 d . . . C3B C 0.049(3) 0.1555(18) -0.0056(11) 0.097(9) Uani 1 1 d . . . C4A C -0.213(3) 0.2683(17) 0.6576(13) 0.074(7) Uani 1 1 d . . . C4B C 0.156(3) 0.0658(18) -0.0124(14) 0.087(8) Uani 1 1 d . . . C5A C -0.277(2) 0.2209(19) 0.6239(14) 0.081(8) Uani 1 1 d . . . C5B C 0.274(2) 0.0489(13) 0.0396(11) 0.063(6) Uani 1 1 d . . . C6A C -0.370(2) 0.2546(19) 0.5726(14) 0.080(7) Uiso 1 1 d . . . C6B C 0.363(2) 0.0902(16) 0.0209(15) 0.075(7) Uani 1 1 d . . . C7A C -0.409(3) 0.366(2) 0.5396(14) 0.095(9) Uani 1 1 d . . . C7B C 0.374(2) 0.1604(16) -0.0491(14) 0.072(7) Uani 1 1 d . . . C8A C -0.305(3) 0.4109(17) 0.5172(19) 0.113(11) Uani 1 1 d . . . C8B C 0.2668(19) 0.2380(17) -0.0728(11) 0.063(6) Uani 1 1 d . . . C11A C -0.095(2) 0.0570(14) 0.4192(12) 0.054(5) Uani 1 1 d . . . C11B C 0.487(3) -0.0548(14) 0.2419(16) 0.080(8) Uani 1 1 d . . . C12A C -0.018(2) 0.0305(13) 0.3607(11) 0.058(6) Uani 1 1 d . . . C12B C 0.505(2) 0.0251(17) 0.2646(12) 0.065(7) Uani 1 1 d . . . C13A C 0.0390(18) 0.1102(15) 0.3443(12) 0.061(6) Uani 1 1 d . . . C13B C 0.426(2) 0.1105(15) 0.2236(11) 0.067(6) Uani 1 1 d . . . C14A C 0.1298(18) 0.1262(14) 0.2809(11) 0.057(6) Uani 1 1 d . . . C14B C 0.4002(19) 0.2131(14) 0.2159(10) 0.053(5) Uani 1 1 d . . . C21A C -0.185(2) 0.0116(14) 0.4653(12) 0.063(6) Uani 1 1 d . . . C21B C 0.553(3) -0.1628(15) 0.2741(18) 0.107(12) Uani 1 1 d . . . C22A C -0.217(2) -0.0676(15) 0.4475(13) 0.075(7) Uani 1 1 d . . . C22B C 0.520(3) -0.2311(17) 0.2458(16) 0.100(10) Uani 1 1 d . . . C23A C -0.304(2) -0.0997(16) 0.4920(16) 0.081(8) Uani 1 1 d . . . C23B C 0.580(3) -0.3265(19) 0.2692(18) 0.106(10) Uani 1 1 d . . . C24A C -0.357(2) -0.058(2) 0.5495(16) 0.080(8) Uani 1 1 d . . . C24B C 0.673(3) -0.3522(16) 0.3223(17) 0.096(10) Uani 1 1 d . . . C25A C -0.329(2) 0.0221(18) 0.5636(12) 0.076(8) Uani 1 1 d . . . C25B C 0.698(3) -0.276(3) 0.344(2) 0.126(12) Uani 1 1 d . . . C31A C 0.006(2) 0.0598(14) 0.1873(11) 0.053(5) Uani 1 1 d . . . C31B C 0.2462(19) 0.4054(14) 0.1447(12) 0.053(5) Uani 1 1 d . . . C32A C -0.126(2) 0.0681(15) 0.2036(12) 0.063(6) Uani 1 1 d . . . C32B C 0.310(2) 0.4552(18) 0.1775(17) 0.094(9) Uani 1 1 d . . . C33A C -0.170(3) -0.0126(19) 0.2086(13) 0.086(9) Uani 1 1 d . . . C33B C 0.241(3) 0.5432(17) 0.1967(14) 0.081(8) Uani 1 1 d . . . C34A C -0.085(2) -0.1016(16) 0.1992(14) 0.074(7) Uani 1 1 d . . . C34B C 0.127(3) 0.5943(15) 0.1758(15) 0.087(9) Uani 1 1 d . . . C35A C 0.044(2) -0.1116(13) 0.1838(11) 0.055(5) Uani 1 1 d . . . C35B C 0.064(2) 0.5485(19) 0.1368(12) 0.079(7) Uani 1 1 d . . . C36A C 0.088(2) -0.0279(17) 0.1788(14) 0.072(7) Uani 1 1 d . . . C36B C 0.121(2) 0.4553(17) 0.1225(13) 0.073(7) Uani 1 1 d . . . C41A C -0.064(2) 0.2705(16) 0.1881(13) 0.069(7) Uani 1 1 d . . . C41B C 0.455(2) 0.296(2) 0.0684(15) 0.098(11) Uani 1 1 d . . . C42A C -0.071(2) 0.3429(16) 0.2294(13) 0.063(6) Uani 1 1 d . . . C42B C 0.446(2) 0.3758(17) 0.0104(12) 0.067(6) Uani 1 1 d . . . C43A C -0.167(3) 0.430(2) 0.2218(18) 0.107(10) Uani 1 1 d . . . C43B C 0.544(2) 0.3771(17) -0.0390(15) 0.080(8) Uani 1 1 d . . . C44A C -0.250(4) 0.4515(16) 0.1649(19) 0.129(15) Uani 1 1 d . . . C44B C 0.654(2) 0.2987(17) -0.0362(12) 0.072(7) Uani 1 1 d . . . C45A C -0.258(2) 0.387(2) 0.1301(16) 0.093(9) Uani 1 1 d . . . C45B C 0.663(2) 0.2189(16) 0.0171(18) 0.101(10) Uani 1 1 d . . . C46A C -0.1583(19) 0.2971(15) 0.1369(11) 0.058(6) Uani 1 1 d . . . C46B C 0.5692(19) 0.2135(16) 0.0672(14) 0.071(7) Uani 1 1 d . . . C51 C 0.647(2) 0.304(2) 0.3497(15) 0.096(8) Uiso 1 1 d . . . C52 C 0.124(6) 0.370(4) 0.396(3) 0.22(2) Uiso 1 1 d . . . H1 H -0.1572 0.3547 0.4437 0.085 Uiso 1 1 d . . . H2 H 0.0027 0.2619 0.5242 0.140 Uiso 1 1 d . . . H3 H -0.0254 0.2244 0.6514 0.102 Uiso 1 1 d . . . H4 H -0.0820 0.3383 0.6349 0.102 Uiso 1 1 d . . . H5 H -0.1999 0.2378 0.7089 0.084 Uiso 1 1 d . . . H6 H -0.2699 0.3358 0.6586 0.084 Uiso 1 1 d . . . H7 H -0.2791 0.1610 0.6566 0.098 Uiso 1 1 d . . . H8 H -0.4334 0.2199 0.5768 0.107 Uiso 1 1 d . . . H9 H -0.4629 0.3807 0.5006 0.111 Uiso 1 1 d . . . H10 H -0.4584 0.4004 0.5785 0.111 Uiso 1 1 d . . . H11 H -0.2849 0.4352 0.5571 0.140 Uiso 1 1 d . . . H12 H -0.3344 0.4651 0.4781 0.140 Uiso 1 1 d . . . H13 H -0.0041 -0.0244 0.3368 0.066 Uiso 1 1 d . . . H14 H 0.2012 0.0643 0.2833 0.067 Uiso 1 1 d . . . H15 H 0.1666 0.1746 0.2887 0.067 Uiso 1 1 d . . . H16 H -0.1756 -0.0994 0.4054 0.092 Uiso 1 1 d . . . H17 H -0.3320 -0.1520 0.4801 0.098 Uiso 1 1 d . . . H18 H -0.4148 -0.0883 0.5828 0.097 Uiso 1 1 d . . . H19 H -0.3714 0.0527 0.6043 0.096 Uiso 1 1 d . . . H20 H -0.1844 0.1316 0.2112 0.075 Uiso 1 1 d . . . H21 H -0.2620 -0.0055 0.2171 0.101 Uiso 1 1 d . . . H22 H -0.1129 -0.1576 0.2023 0.082 Uiso 1 1 d . . . H23 H 0.0998 -0.1759 0.1760 0.065 Uiso 1 1 d . . . H24 H 0.1780 -0.0340 0.1680 0.083 Uiso 1 1 d . . . H25 H -0.0056 0.3295 0.2661 0.074 Uiso 1 1 d . . . H26 H -0.1737 0.4815 0.2470 0.115 Uiso 1 1 d . . . H27 H -0.3188 0.5128 0.1561 0.104 Uiso 1 1 d . . . H28 H -0.3331 0.4014 0.0970 0.111 Uiso 1 1 d . . . H29 H -0.1506 0.2499 0.1032 0.072 Uiso 1 1 d . . . H30 H 0.1712 0.3454 -0.0079 0.094 Uiso 1 1 d . . . H31 H 0.0087 0.2834 0.0447 0.071 Uiso 1 1 d . . . H32 H -0.0157 0.1340 0.0273 0.126 Uiso 1 1 d . . . H33 H 0.0081 0.1835 -0.0515 0.126 Uiso 1 1 d . . . H34 H 0.1245 0.0096 -0.0020 0.103 Uiso 1 1 d . . . H35 H 0.1825 0.0729 -0.0628 0.103 Uiso 1 1 d . . . H36 H 0.3009 -0.0152 0.0702 0.073 Uiso 1 1 d . . . H37 H 0.4457 0.0499 0.0420 0.089 Uiso 1 1 d . . . H38 H 0.4420 0.1880 -0.0457 0.081 Uiso 1 1 d . . . H39 H 0.4032 0.1214 -0.0884 0.081 Uiso 1 1 d . . . H40 H 0.2158 0.2156 -0.1013 0.079 Uiso 1 1 d . . . H41 H 0.2883 0.2914 -0.1043 0.079 Uiso 1 1 d . . . H42 H 0.5649 0.0225 0.3027 0.079 Uiso 1 1 d . . . H43 H 0.4802 0.2266 0.2195 0.064 Uiso 1 1 d . . . H44 H 0.3478 0.2362 0.2561 0.064 Uiso 1 1 d . . . H45 H 0.4483 -0.2104 0.2076 0.135 Uiso 1 1 d . . . H46 H 0.5580 -0.3795 0.2513 0.124 Uiso 1 1 d . . . H47 H 0.7231 -0.4208 0.3405 0.107 Uiso 1 1 d . . . H48 H 0.7694 -0.2950 0.3826 0.157 Uiso 1 1 d . . . H49 H 0.4033 0.4244 0.1850 0.104 Uiso 1 1 d . . . H50 H 0.2808 0.5729 0.2296 0.089 Uiso 1 1 d . . . H51 H 0.0823 0.6567 0.1866 0.089 Uiso 1 1 d . . . H52 H -0.0230 0.5886 0.1178 0.092 Uiso 1 1 d . . . H53 H 0.0721 0.4254 0.0976 0.075 Uiso 1 1 d . . . H54 H 0.3668 0.4326 0.0042 0.085 Uiso 1 1 d . . . H55 H 0.5400 0.4368 -0.0743 0.090 Uiso 1 1 d . . . H56 H 0.7250 0.2979 -0.0742 0.091 Uiso 1 1 d . . . H57 H 0.7449 0.1648 0.0222 0.107 Uiso 1 1 d . . . H58 H 0.5769 0.1511 0.1032 0.083 Uiso 1 1 d . . . H59 H 0.6959 0.3019 0.3916 0.114 Uiso 1 1 d . . . H60 H 0.7087 0.2985 0.3091 0.114 Uiso 1 1 d . . . H61 H 0.0865 0.3434 0.4514 0.213 Uiso 1 1 d . . . H62 H 0.1097 0.3135 0.3754 0.213 Uiso 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 0.0804(8) 0.0554(6) 0.0546(7) -0.0097(5) 0.0075(6) -0.0222(6) Ir2 0.0624(6) 0.0415(5) 0.0484(6) -0.0044(4) 0.0040(5) -0.0165(4) P1 0.061(4) 0.042(3) 0.052(4) -0.004(2) 0.013(3) -0.019(3) P2 0.071(4) 0.038(3) 0.052(4) -0.001(2) 0.002(3) -0.019(3) N1A 0.071(12) 0.052(10) 0.034(10) -0.020(8) -0.001(9) -0.008(9) N1B 0.093(13) 0.037(9) 0.029(9) -0.016(7) 0.024(9) -0.014(9) N2A 0.053(11) 0.094(14) 0.036(11) 0.007(9) -0.001(9) -0.033(10) N2B 0.043(10) 0.067(12) 0.055(12) -0.025(9) -0.002(9) -0.009(9) N3A 0.090(14) 0.065(12) 0.062(14) 0.008(10) -0.004(12) -0.046(11) N3B 0.087(16) 0.071(15) 0.070(15) 0.024(11) -0.009(12) -0.002(12) C1A 0.104(19) 0.080(16) 0.042(14) -0.030(11) 0.041(13) -0.040(15) C1B 0.084(17) 0.063(14) 0.055(15) 0.001(11) 0.016(13) -0.022(13) C2A 0.10(2) 0.067(17) 0.18(3) -0.068(18) -0.10(2) 0.015(14) C3A 0.18(3) 0.038(14) 0.08(2) -0.025(12) -0.01(2) -0.034(17) C3B 0.19(3) 0.070(17) 0.026(13) 0.000(11) 0.003(16) -0.044(19) C4A 0.085(19) 0.067(16) 0.055(16) 0.002(12) 0.001(14) -0.010(14) C4B 0.14(3) 0.061(16) 0.060(17) -0.023(12) 0.010(17) -0.029(16) C5A 0.069(17) 0.092(19) 0.09(2) 0.002(15) -0.013(15) -0.040(15) C5B 0.103(19) 0.034(11) 0.039(13) -0.015(9) 0.030(13) -0.004(12) C6B 0.049(14) 0.042(13) 0.10(2) 0.014(12) -0.016(13) 0.013(11) C7A 0.10(2) 0.12(2) 0.071(19) -0.004(16) 0.023(16) -0.051(18) C7B 0.048(14) 0.057(15) 0.10(2) 0.008(13) -0.013(13) -0.012(12) C8A 0.11(2) 0.040(14) 0.16(3) -0.025(16) -0.01(2) 0.026(14) C8B 0.048(13) 0.092(17) 0.039(13) -0.006(11) -0.002(11) -0.012(12) C11A 0.070(15) 0.043(12) 0.054(15) -0.019(10) 0.005(12) -0.020(11) C11B 0.10(2) 0.025(11) 0.11(2) -0.025(12) 0.028(17) -0.009(12) C12A 0.090(17) 0.033(11) 0.051(14) -0.018(9) 0.007(12) -0.013(11) C12B 0.061(14) 0.082(17) 0.048(14) 0.014(12) 0.001(11) -0.034(13) C13A 0.047(13) 0.058(14) 0.064(16) -0.008(11) -0.006(11) 0.000(11) C13B 0.104(19) 0.046(13) 0.042(14) 0.004(10) 0.006(13) -0.018(12) C14A 0.049(12) 0.047(12) 0.069(15) 0.012(10) 0.013(11) -0.022(10) C14B 0.068(14) 0.054(13) 0.042(13) -0.026(9) -0.002(11) -0.016(11) C21A 0.104(18) 0.036(12) 0.042(14) -0.020(9) 0.002(13) -0.005(12) C21B 0.15(3) 0.018(11) 0.12(3) -0.004(14) 0.05(2) -0.004(15) C22A 0.093(18) 0.037(12) 0.076(18) -0.002(11) 0.008(15) 0.001(12) C22B 0.13(2) 0.038(14) 0.11(2) -0.011(14) 0.031(19) -0.005(15) C23A 0.096(19) 0.044(13) 0.09(2) 0.013(13) 0.019(16) -0.031(13) C23B 0.15(3) 0.054(17) 0.11(3) -0.015(16) 0.05(2) -0.040(19) C24A 0.069(17) 0.076(18) 0.09(2) 0.008(15) -0.013(15) -0.033(14) C24B 0.15(3) 0.019(11) 0.10(2) 0.006(13) 0.04(2) -0.018(15) C25A 0.089(18) 0.072(16) 0.042(15) -0.002(12) 0.035(13) -0.005(14) C25B 0.12(3) 0.09(2) 0.15(3) 0.02(2) -0.02(2) -0.03(2) C31A 0.061(14) 0.053(13) 0.040(13) -0.011(9) 0.002(11) -0.009(11) C31B 0.043(12) 0.037(11) 0.068(15) 0.003(10) 0.007(11) -0.008(10) C32A 0.083(17) 0.063(14) 0.052(15) -0.027(11) 0.025(12) -0.032(13) C32B 0.09(2) 0.064(17) 0.12(3) -0.013(16) 0.034(18) -0.036(15) C33A 0.15(3) 0.08(2) 0.068(16) -0.017(14) -0.005(18) -0.09(2) C33B 0.12(2) 0.045(14) 0.09(2) -0.036(13) 0.043(17) -0.025(14) C34A 0.080(18) 0.049(14) 0.094(19) 0.010(12) -0.035(15) -0.028(13) C34B 0.13(3) 0.025(12) 0.080(19) 0.012(11) 0.031(18) -0.017(15) C35A 0.076(16) 0.039(11) 0.060(14) -0.018(9) -0.012(12) -0.023(11) C35B 0.10(2) 0.080(18) 0.040(15) -0.007(12) 0.043(14) -0.023(15) C36A 0.081(17) 0.057(15) 0.081(18) 0.005(12) -0.005(14) -0.036(13) C36B 0.10(2) 0.057(14) 0.071(18) -0.015(12) 0.014(15) -0.042(14) C41A 0.049(14) 0.070(15) 0.079(18) 0.008(13) 0.016(13) -0.025(12) C41B 0.055(15) 0.12(2) 0.11(2) 0.064(18) -0.033(15) -0.062(16) C42A 0.059(14) 0.057(14) 0.080(17) -0.033(12) 0.017(12) -0.022(12) C42B 0.074(16) 0.080(16) 0.056(15) -0.015(12) 0.005(13) -0.035(13) C43A 0.14(3) 0.08(2) 0.09(2) -0.008(17) -0.01(2) -0.013(19) C43B 0.057(15) 0.064(15) 0.11(2) -0.015(14) 0.035(14) -0.013(12) C44A 0.23(4) 0.015(12) 0.11(3) -0.027(13) 0.03(3) 0.008(17) C44B 0.078(17) 0.070(16) 0.056(15) 0.011(12) 0.015(13) -0.027(13) C45A 0.060(16) 0.09(2) 0.10(2) 0.028(17) 0.014(14) -0.008(15) C45B 0.073(18) 0.042(14) 0.16(3) -0.010(16) 0.021(18) 0.004(12) C46A 0.039(12) 0.075(15) 0.048(14) -0.017(11) 0.009(10) -0.001(11) C46B 0.038(13) 0.068(15) 0.10(2) -0.020(13) 0.010(13) 0.000(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 N2A 2.046(19) . ? Ir1 N3A 2.099(18) . ? Ir1 C5A 2.12(3) . ? Ir1 C2A 2.13(2) . ? Ir1 C6A 2.14(3) . ? Ir1 C1A 2.15(2) . ? Ir2 N1B 2.017(16) . ? Ir2 C2B 2.148(19) . ? Ir2 C5B 2.15(2) . ? Ir2 C6B 2.15(3) . ? Ir2 C1B 2.28(2) . ? Ir2 P2 2.322(6) . ? Ir2 P1 2.400(6) . ? Cl1 C51 1.73(3) . ? Cl2 C51 1.68(3) . ? Cl3 C52 1.64(5) . ? Cl4 C52 1.37(5) . ? P1 C41A 1.83(2) . ? P1 C14A 1.83(2) . ? P1 C31A 1.85(2) . ? P2 C41B 1.80(2) . ? P2 C31B 1.83(2) . ? P2 C14B 1.85(2) . ? N1A C13A 1.31(2) . ? N1A N2A 1.41(2) . ? N1B N2B 1.36(2) . ? N1B C13B 1.47(3) . ? N2A C11A 1.29(2) . ? N2B C11B 1.37(3) . ? N3A C21A 1.34(3) . ? N3A C25A 1.43(3) . ? N3B C21B 1.34(4) . ? N3B C25B 1.34(3) . ? C1A C2A 1.46(3) . ? C1A C8A 1.53(3) . ? C1B C2B 1.47(3) . ? C1B C8B 1.53(3) . ? C2A C3A 1.48(4) . ? C2B C3B 1.57(3) . ? C3A C4A 1.47(4) . ? C3B C4B 1.48(3) . ? C4A C5A 1.39(3) . ? C4B C5B 1.62(3) . ? C5A C6A 1.38(3) . ? C5B C6B 1.31(3) . ? C6A C7A 1.55(3) . ? C6B C7B 1.52(3) . ? C7A C8A 1.49(4) . ? C7B C8B 1.39(3) . ? C11A C12A 1.38(3) . ? C11A C21A 1.49(3) . ? C11B C12B 1.39(3) . ? C11B C21B 1.53(3) . ? C12A C13A 1.46(3) . ? C12B C13B 1.39(3) . ? C13A C14A 1.53(3) . ? C13B C14B 1.41(3) . ? C21A C22A 1.41(3) . ? C21B C22B 1.37(4) . ? C22A C23A 1.37(3) . ? C22B C23B 1.33(3) . ? C23A C24A 1.34(3) . ? C23B C24B 1.41(4) . ? C24A C25A 1.38(3) . ? C24B C25B 1.36(4) . ? C31A C36A 1.34(3) . ? C31A C32A 1.45(3) . ? C31B C36B 1.40(3) . ? C31B C32B 1.41(3) . ? C32A C33A 1.40(3) . ? C32B C33B 1.37(3) . ? C33A C34A 1.38(3) . ? C33B C34B 1.30(3) . ? C34A C35A 1.41(3) . ? C34B C35B 1.42(4) . ? C35A C36A 1.44(3) . ? C35B C36B 1.37(3) . ? C41A C46A 1.38(3) . ? C41A C42A 1.41(3) . ? C41B C42B 1.41(3) . ? C41B C46B 1.44(3) . ? C42A C43A 1.37(3) . ? C42B C43B 1.38(3) . ? C43A C44A 1.39(4) . ? C43B C44B 1.37(3) . ? C44A C45A 1.28(4) . ? C44B C45B 1.36(3) . ? C45A C46A 1.41(3) . ? C45B C46B 1.36(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 N2A Ir1 N3A 76.6(8) . . ? N2A Ir1 C5A 168.5(8) . . ? N3A Ir1 C5A 101.0(9) . . ? N2A Ir1 C2A 98.9(11) . . ? N3A Ir1 C2A 158.7(8) . . ? C5A Ir1 C2A 79.3(11) . . ? N2A Ir1 C6A 152.6(9) . . ? N3A Ir1 C6A 92.7(9) . . ? C5A Ir1 C6A 37.6(8) . . ? C2A Ir1 C6A 99.6(11) . . ? N2A Ir1 C1A 97.8(8) . . ? N3A Ir1 C1A 160.3(8) . . ? C5A Ir1 C1A 88.2(9) . . ? C2A Ir1 C1A 40.0(9) . . ? C6A Ir1 C1A 83.9(9) . . ? N1B Ir2 C2B 165.3(7) . . ? N1B Ir2 C5B 87.9(7) . . ? C2B Ir2 C5B 83.7(8) . . ? N1B Ir2 C6B 84.3(7) . . ? C2B Ir2 C6B 95.7(8) . . ? C5B Ir2 C6B 35.5(8) . . ? N1B Ir2 C1B 153.7(7) . . ? C2B Ir2 C1B 38.5(7) . . ? C5B Ir2 C1B 88.9(8) . . ? C6B Ir2 C1B 78.1(8) . . ? N1B Ir2 P2 80.5(5) . . ? C2B Ir2 P2 113.2(6) . . ? C5B Ir2 P2 143.8(7) . . ? C6B Ir2 P2 108.8(7) . . ? C1B Ir2 P2 86.8(6) . . ? N1B Ir2 P1 88.0(5) . . ? C2B Ir2 P1 83.3(6) . . ? C5B Ir2 P1 109.1(7) . . ? C6B Ir2 P1 143.8(7) . . ? C1B Ir2 P1 117.6(6) . . ? P2 Ir2 P1 104.7(2) . . ? C41A P1 C14A 104.2(11) . . ? C41A P1 C31A 104.9(10) . . ? C14A P1 C31A 99.0(9) . . ? C41A P1 Ir2 118.5(7) . . ? C14A P1 Ir2 113.3(6) . . ? C31A P1 Ir2 114.6(7) . . ? C41B P2 C31B 102.4(12) . . ? C41B P2 C14B 104.7(10) . . ? C31B P2 C14B 104.0(10) . . ? C41B P2 Ir2 112.1(11) . . ? C31B P2 Ir2 129.3(8) . . ? C14B P2 Ir2 101.9(6) . . ? C13A N1A N2A 103.8(18) . . ? N2B N1B C13B 107.9(15) . . ? N2B N1B Ir2 128.0(13) . . ? C13B N1B Ir2 123.7(12) . . ? C11A N2A N1A 110.8(19) . . ? C11A N2A Ir1 118.5(15) . . ? N1A N2A Ir1 130.5(15) . . ? N1B N2B C11B 107.8(16) . . ? C21A N3A C25A 115(2) . . ? C21A N3A Ir1 116.4(15) . . ? C25A N3A Ir1 128.0(18) . . ? C21B N3B C25B 110(3) . . ? C2A C1A C8A 122(2) . . ? C2A C1A Ir1 69.5(13) . . ? C8A C1A Ir1 112.3(17) . . ? C2B C1B C8B 124(2) . . ? C2B C1B Ir2 65.7(11) . . ? C8B C1B Ir2 111.2(14) . . ? C1A C2A C3A 125(2) . . ? C1A C2A Ir1 70.5(12) . . ? C3A C2A Ir1 111(2) . . ? C1B C2B C3B 120(2) . . ? C1B C2B Ir2 75.8(12) . . ? C3B C2B Ir2 109.1(14) . . ? C4A C3A C2A 110(3) . . ? C4B C3B C2B 116(2) . . ? C5A C4A C3A 119(2) . . ? C3B C4B C5B 113(2) . . ? C6A C5A C4A 133(2) . . ? C6A C5A Ir1 72.0(16) . . ? C4A C5A Ir1 112.8(18) . . ? C6B C5B C4B 123(2) . . ? C6B C5B Ir2 72.3(15) . . ? C4B C5B Ir2 110.8(13) . . ? C5A C6A C7A 116(2) . . ? C5A C6A Ir1 70.4(16) . . ? C7A C6A Ir1 106.6(16) . . ? C5B C6B C7B 127(2) . . ? C5B C6B Ir2 72.2(15) . . ? C7B C6B Ir2 110.5(15) . . ? C8A C7A C6A 118(2) . . ? C8B C7B C6B 118.0(19) . . ? C7A C8A C1A 112(2) . . ? C7B C8B C1B 112.5(18) . . ? N2A C11A C12A 112(2) . . ? N2A C11A C21A 116(2) . . ? C12A C11A C21A 132.2(19) . . ? N2B C11B C12B 110.6(19) . . ? N2B C11B C21B 125(2) . . ? C12B C11B C21B 125(3) . . ? C11A C12A C13A 100.5(17) . . ? C11B C12B C13B 107(2) . . ? N1A C13A C12A 112.6(19) . . ? N1A C13A C14A 121(2) . . ? C12A C13A C14A 126.4(19) . . ? C12B C13B C14B 138(2) . . ? C12B C13B N1B 105.6(18) . . ? C14B C13B N1B 116.6(17) . . ? C13A C14A P1 120.0(14) . . ? C13B C14B P2 112.1(14) . . ? N3A C21A C22A 125(2) . . ? N3A C21A C11A 112.7(19) . . ? C22A C21A C11A 122(2) . . ? N3B C21B C22B 128(2) . . ? N3B C21B C11B 116(3) . . ? C22B C21B C11B 116(3) . . ? C23A C22A C21A 116(2) . . ? C23B C22B C21B 119(3) . . ? C24A C23A C22A 122(2) . . ? C22B C23B C24B 118(3) . . ? C23A C24A C25A 120(2) . . ? C25B C24B C23B 117(2) . . ? C24A C25A N3A 121(2) . . ? N3B C25B C24B 129(3) . . ? C36A C31A C32A 119(2) . . ? C36A C31A P1 117.0(17) . . ? C32A C31A P1 123.5(15) . . ? C36B C31B C32B 118(2) . . ? C36B C31B P2 120.4(18) . . ? C32B C31B P2 121.3(17) . . ? C33A C32A C31A 121(2) . . ? C33B C32B C31B 118(2) . . ? C34A C33A C32A 119(2) . . ? C34B C33B C32B 125(3) . . ? C33A C34A C35A 121(2) . . ? C33B C34B C35B 116(2) . . ? C34A C35A C36A 119.6(19) . . ? C36B C35B C34B 122(2) . . ? C31A C36A C35A 120(2) . . ? C35B C36B C31B 119(2) . . ? C46A C41A C42A 115(2) . . ? C46A C41A P1 120.6(19) . . ? C42A C41A P1 123.3(18) . . ? C42B C41B C46B 114(2) . . ? C42B C41B P2 125(2) . . ? C46B C41B P2 119.4(17) . . ? C43A C42A C41A 122(2) . . ? C43B C42B C41B 122(2) . . ? C42A C43A C44A 117(3) . . ? C44B C43B C42B 122(2) . . ? C45A C44A C43A 123(3) . . ? C45B C44B C43B 118(2) . . ? C44A C45A C46A 118(3) . . ? C46B C45B C44B 123(2) . . ? C41A C46A C45A 123(2) . . ? C45B C46B C41B 121(2) . . ? Cl2 C51 Cl1 115.4(16) . . ? Cl4 C52 Cl3 125(4) . . ? _diffrn_measured_fraction_theta_max 0.767 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.767 _refine_diff_density_max 1.934 _refine_diff_density_min -1.521 _refine_diff_density_rms 0.163 #===END