# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1552 # Disorder of a central carbon in a sigma-allyl group (C2') observed data_ccd130 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; (triphenylphosphine)(sigma-allyl)bis(pi-allyl)iridium ; _publ_contact_author ; R. Thomas Baker CST-18 MS J514 Los Alamos National Laboratory Los Alamos, NM 87545 USA ; _publ_contact_author_email 'weg@lanl.gov' loop_ _publ_author_name 'Kevin D. John' 'Kenneth V. Salazar' 'Brian L. Scott' 'R. Thomas Baker' 'Alfred P. Sattelberger' _publ_requested_journal 'Chemical Communications' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H60 Ir2 P2' _chemical_formula_weight 1155.36 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' '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2972(4) _cell_length_b 15.7287(7) _cell_length_c 16.6995(8) _cell_angle_alpha 73.249(1) _cell_angle_beta 82.344(1) _cell_angle_gamma 79.303(1) _cell_volume 2289.49(18) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'multifaceted block' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_crystal_preparation 'crystallized from toluene' _exptl_absorpt_coefficient_mu 11.824 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8678 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0350 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 26.56 _reflns_number_total 8678 _reflns_number_gt 7576 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0408P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8678 _refine_ls_number_parameters 518 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0670 _refine_ls_wR_factor_gt 0.0645 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.002 _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 Ir Ir 0.885082(16) 0.401548(9) 0.734858(9) 0.02346(5) Uani 1 1 d . . . P P 1.12996(11) 0.41696(6) 0.70404(6) 0.02148(19) Uani 1 1 d . . . C1 C 0.8276(5) 0.5316(3) 0.7609(3) 0.0336(9) Uani 1 1 d . . . H1A H 0.9166 0.5569 0.7572 0.040 Uiso 1 1 calc R . . H1B H 0.7664 0.5717 0.7184 0.040 Uiso 1 1 calc R . . C2 C 0.7482(5) 0.5264(3) 0.8452(3) 0.0428(11) Uani 1 1 d . . . H2A H 0.8043 0.4994 0.8906 0.051 Uiso 1 1 calc R . . C3 C 0.6093(6) 0.5550(4) 0.8639(4) 0.0588(15) Uani 1 1 d . . . H3A H 0.5472 0.5826 0.8214 0.071 Uiso 1 1 calc R . . H3B H 0.5730 0.5476 0.9198 0.071 Uiso 1 1 calc R . . C4 C 0.8309(5) 0.4687(3) 0.6048(3) 0.0390(10) Uani 1 1 d . . . H4A H 0.7894 0.5319 0.5925 0.047 Uiso 1 1 calc R . . H4B H 0.9002 0.4532 0.5605 0.047 Uiso 1 1 calc R . . C5 C 0.7347(6) 0.4066(3) 0.6462(3) 0.0463(12) Uani 1 1 d . . . H5A H 0.7315 0.3539 0.6267 0.056 Uiso 1 1 calc R . . C6 C 0.6502(5) 0.4200(3) 0.7201(3) 0.0459(12) Uani 1 1 d . . . H6A H 0.5974 0.3719 0.7529 0.055 Uiso 1 1 calc R . . H6B H 0.5954 0.4796 0.7165 0.055 Uiso 1 1 calc R . . C8 C 0.8616(5) 0.2714(3) 0.8179(3) 0.0392(11) Uani 1 1 d . . . H8A H 0.7652 0.2516 0.8292 0.047 Uiso 1 1 calc R . . C9 C 0.9001(6) 0.3224(3) 0.8669(3) 0.0424(11) Uani 1 1 d . . . H9A H 0.9974 0.3050 0.8868 0.051 Uiso 1 1 calc R . . H9B H 0.8245 0.3400 0.9076 0.051 Uiso 1 1 calc R . . C10 C 1.2520(4) 0.3547(2) 0.7856(2) 0.0263(8) Uani 1 1 d . . . C11 C 1.2422(5) 0.3802(3) 0.8601(2) 0.0346(10) Uani 1 1 d . . . H11B H 1.1766 0.4307 0.8665 0.041 Uiso 1 1 calc R . . C12 C 1.3287(5) 0.3315(3) 0.9242(3) 0.0431(11) Uani 1 1 d . . . H12B H 1.3212 0.3497 0.9730 0.052 Uiso 1 1 calc R . . C13 C 1.4260(5) 0.2561(3) 0.9167(3) 0.0412(11) Uani 1 1 d . . . H13B H 1.4851 0.2243 0.9597 0.049 Uiso 1 1 calc R . . C14 C 1.4354(5) 0.2278(3) 0.8446(3) 0.0352(10) Uani 1 1 d . . . H14B H 1.4989 0.1760 0.8398 0.042 Uiso 1 1 calc R . . C15 C 1.3494(4) 0.2772(3) 0.7791(2) 0.0277(8) Uani 1 1 d . . . H15B H 1.3570 0.2583 0.7306 0.033 Uiso 1 1 calc R . . C16 C 1.2252(4) 0.3791(2) 0.6138(2) 0.0226(8) Uani 1 1 d . . . C17 C 1.3637(5) 0.4012(3) 0.5818(2) 0.0296(9) Uani 1 1 d . . . H17B H 1.4042 0.4384 0.6039 0.036 Uiso 1 1 calc R . . C18 C 1.4418(5) 0.3683(3) 0.5175(3) 0.0337(9) Uani 1 1 d . . . H18B H 1.5342 0.3835 0.4967 0.040 Uiso 1 1 calc R . . C19 C 1.3826(5) 0.3128(3) 0.4844(3) 0.0363(10) Uani 1 1 d . . . H19B H 1.4354 0.2903 0.4416 0.044 Uiso 1 1 calc R . . C20 C 1.2456(5) 0.2911(3) 0.5146(3) 0.0348(10) Uani 1 1 d . . . H20B H 1.2059 0.2539 0.4919 0.042 Uiso 1 1 calc R . . C21 C 1.1649(5) 0.3244(3) 0.5791(2) 0.0292(9) Uani 1 1 d . . . H21B H 1.0716 0.3101 0.5987 0.035 Uiso 1 1 calc R . . C22 C 1.1735(4) 0.5326(2) 0.6732(2) 0.0223(8) Uani 1 1 d . . . C23 C 1.2715(5) 0.5619(3) 0.7108(3) 0.0333(9) Uani 1 1 d . . . H23B H 1.3171 0.5231 0.7569 0.040 Uiso 1 1 calc R . . C24 C 1.3021(5) 0.6497(3) 0.6797(3) 0.0404(11) Uani 1 1 d . . . H24B H 1.3666 0.6695 0.7059 0.049 Uiso 1 1 calc R . . C25 C 1.2374(5) 0.7071(3) 0.6106(3) 0.0375(10) Uani 1 1 d . . . H25B H 1.2592 0.7653 0.5896 0.045 Uiso 1 1 calc R . . C26 C 1.1403(5) 0.6781(3) 0.5726(3) 0.0361(10) Uani 1 1 d . . . H26B H 1.0975 0.7165 0.5254 0.043 Uiso 1 1 calc R . . C7 C 0.9573(5) 0.2524(3) 0.7514(3) 0.0373(10) Uani 1 1 d . . . H7A H 0.9195 0.2256 0.7145 0.045 Uiso 1 1 calc R . . H7B H 1.0588 0.2287 0.7626 0.045 Uiso 1 1 calc R . . Ir' Ir 0.697422(17) 0.887788(9) 0.736423(9) 0.02516(5) Uani 1 1 d . A . P' P 0.89980(11) 0.89288(6) 0.80091(6) 0.0224(2) Uani 1 1 d . . . C1' C 0.7368(6) 1.0009(3) 0.6304(3) 0.0426(11) Uani 1 1 d . . . C2A' C 0.7355(13) 1.0902(6) 0.6501(6) 0.048(3) Uiso 0.608(18) 1 d P A 1 H2AA H 0.8174 1.0920 0.6757 0.057 Uiso 0.608(18) 1 calc PR A 1 C2B' C 0.655(2) 1.0852(9) 0.6326(9) 0.050(5) Uiso 0.392(18) 1 d P A 2 H2BA H 0.5599 1.0798 0.6264 0.061 Uiso 0.392(18) 1 calc PR A 2 C3' C 0.6453(10) 1.1611(6) 0.6384(6) 0.103(3) Uiso 1 1 d . . . C4' C 0.8256(5) 0.8026(3) 0.6591(3) 0.0387(11) Uani 1 1 d . . . H4'A H 0.8500 0.8322 0.6006 0.046 Uiso 1 1 calc R A . H4'B H 0.9039 0.7572 0.6851 0.046 Uiso 1 1 calc R . . C5' C 0.6805(6) 0.7831(3) 0.6815(3) 0.0435(12) Uani 1 1 d . A . H5'A H 0.6618 0.7238 0.7166 0.052 Uiso 1 1 calc R . . C6' C 0.5623(6) 0.8537(4) 0.6545(3) 0.0517(13) Uani 1 1 d . . . H6'A H 0.4640 0.8423 0.6774 0.062 Uiso 1 1 calc R A . H6'B H 0.5683 0.8869 0.5957 0.062 Uiso 1 1 calc R . . C7' C 0.6118(5) 0.8056(3) 0.8635(3) 0.0399(11) Uani 1 1 d . . . H7'A H 0.5931 0.7459 0.8669 0.048 Uiso 1 1 calc R A . H7'B H 0.6533 0.8094 0.9124 0.048 Uiso 1 1 calc R . . C8' C 0.5088(5) 0.8783(3) 0.8261(3) 0.0443(11) Uani 1 1 d . A . H8'A H 0.4172 0.8672 0.8108 0.053 Uiso 1 1 calc R . . C9' C 0.5392(5) 0.9673(3) 0.8061(3) 0.0398(11) Uani 1 1 d . . . H9'A H 0.5762 0.9845 0.8499 0.048 Uiso 1 1 calc R A . H9'B H 0.4694 1.0140 0.7738 0.048 Uiso 1 1 calc R . . C10' C 1.0409(5) 0.9527(3) 0.7336(2) 0.0293(9) Uani 1 1 d . . . C11' C 1.0956(5) 1.0239(3) 0.7477(3) 0.0307(9) Uani 1 1 d . . . H11A H 1.0625 1.0423 0.7960 0.037 Uiso 1 1 calc R . . C12' C 1.1992(5) 1.0673(3) 0.6900(3) 0.0408(11) Uani 1 1 d . . . H12A H 1.2323 1.1156 0.6992 0.049 Uiso 1 1 calc R . . C13' C 1.2529(5) 1.0393(3) 0.6196(3) 0.0436(12) Uani 1 1 d . . . H13A H 1.3232 1.0680 0.5818 0.052 Uiso 1 1 calc R . . C14' C 1.2025(5) 0.9687(3) 0.6051(3) 0.0435(11) Uani 1 1 d . . . H14A H 1.2381 0.9499 0.5572 0.052 Uiso 1 1 calc R . . C15' C 1.0990(5) 0.9258(3) 0.6616(3) 0.0364(10) Uani 1 1 d . . . H15A H 1.0671 0.8775 0.6515 0.044 Uiso 1 1 calc R . . C16' C 1.0133(4) 0.7835(2) 0.8440(2) 0.0245(8) Uani 1 1 d . . . C17' C 1.1530(5) 0.7811(3) 0.8663(3) 0.0328(9) Uani 1 1 d . . . H17A H 1.1890 0.8347 0.8573 0.039 Uiso 1 1 calc R . . C18' C 1.2395(5) 0.7011(3) 0.9015(3) 0.0374(10) Uani 1 1 d . . . H18A H 1.3327 0.7010 0.9160 0.045 Uiso 1 1 calc R . . C19' C 1.1869(5) 0.6207(3) 0.9152(3) 0.0386(10) Uani 1 1 d . . . H19A H 1.2447 0.5665 0.9389 0.046 Uiso 1 1 calc R . . C20' C 1.0490(5) 0.6216(3) 0.8935(3) 0.0383(10) Uani 1 1 d . . . H20A H 1.0134 0.5678 0.9027 0.046 Uiso 1 1 calc R . . C21' C 0.9622(5) 0.7026(3) 0.8577(3) 0.0323(9) Uani 1 1 d . . . H21A H 0.8693 0.7024 0.8429 0.039 Uiso 1 1 calc R . . C22' C 0.8655(4) 0.9374(2) 0.8929(2) 0.0225(8) Uani 1 1 d . . . C23' C 0.8797(5) 0.8823(3) 0.9734(2) 0.0295(9) Uani 1 1 d . . . H23A H 0.9154 0.8214 0.9815 0.035 Uiso 1 1 calc R . . C24' C 0.8414(5) 0.9169(3) 1.0418(2) 0.0338(9) Uani 1 1 d . . . H24A H 0.8520 0.8788 1.0955 0.041 Uiso 1 1 calc R . . C25' C 0.7878(5) 1.0067(3) 1.0320(3) 0.0351(10) Uani 1 1 d . . . H25A H 0.7615 1.0290 1.0787 0.042 Uiso 1 1 calc R . . C26' C 0.7737(5) 1.0630(3) 0.9521(3) 0.0337(9) Uani 1 1 d . . . H26A H 0.7400 1.1241 0.9446 0.040 Uiso 1 1 calc R . . C27' C 0.8097(4) 1.0289(3) 0.8830(2) 0.0280(8) Uani 1 1 d . . . H27A H 0.7969 1.0669 0.8295 0.034 Uiso 1 1 calc R . . C27 C 1.1066(5) 0.5926(2) 0.6043(2) 0.0299(9) Uani 1 1 d . . . H27B H 1.0381 0.5744 0.5794 0.036 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir 0.02185(9) 0.02046(8) 0.02586(8) -0.00309(6) -0.00045(6) -0.00397(6) P 0.0228(5) 0.0219(4) 0.0191(4) -0.0051(3) -0.0016(4) -0.0026(4) C1 0.030(2) 0.027(2) 0.043(2) -0.0113(17) 0.0065(19) -0.0054(17) C2 0.044(3) 0.038(2) 0.048(3) -0.020(2) 0.008(2) -0.006(2) C3 0.054(3) 0.059(3) 0.061(3) -0.025(3) 0.020(3) -0.008(3) C4 0.039(3) 0.037(2) 0.037(2) -0.0001(18) -0.015(2) -0.003(2) C5 0.045(3) 0.040(3) 0.057(3) -0.006(2) -0.027(2) -0.010(2) C6 0.026(3) 0.037(2) 0.068(3) 0.003(2) -0.013(2) -0.010(2) C8 0.040(3) 0.027(2) 0.041(2) 0.0066(18) 0.001(2) -0.0087(19) C9 0.046(3) 0.039(2) 0.030(2) 0.0037(18) 0.005(2) -0.004(2) C10 0.025(2) 0.0285(19) 0.0249(18) -0.0044(15) -0.0025(16) -0.0068(16) C11 0.036(3) 0.039(2) 0.025(2) -0.0084(17) -0.0012(18) 0.0026(19) C12 0.047(3) 0.059(3) 0.022(2) -0.0096(19) -0.0057(19) -0.006(2) C13 0.035(3) 0.051(3) 0.027(2) 0.0054(19) -0.0104(19) -0.001(2) C14 0.026(2) 0.033(2) 0.037(2) 0.0016(17) -0.0004(18) -0.0001(18) C15 0.023(2) 0.032(2) 0.0272(19) -0.0062(16) 0.0003(16) -0.0043(16) C16 0.023(2) 0.0248(18) 0.0185(17) -0.0042(14) -0.0041(14) -0.0009(15) C17 0.031(2) 0.033(2) 0.027(2) -0.0122(16) -0.0022(17) -0.0056(17) C18 0.029(2) 0.039(2) 0.031(2) -0.0109(17) 0.0039(18) -0.0032(18) C19 0.040(3) 0.038(2) 0.031(2) -0.0179(18) 0.0038(19) 0.0010(19) C20 0.047(3) 0.033(2) 0.029(2) -0.0166(17) -0.0039(19) -0.0047(19) C21 0.031(2) 0.031(2) 0.0263(19) -0.0083(16) -0.0016(17) -0.0075(17) C22 0.022(2) 0.0238(18) 0.0211(17) -0.0080(14) 0.0040(15) -0.0057(15) C23 0.033(2) 0.036(2) 0.032(2) -0.0101(17) -0.0017(18) -0.0079(18) C24 0.042(3) 0.043(3) 0.044(3) -0.020(2) 0.003(2) -0.019(2) C25 0.036(3) 0.027(2) 0.049(3) -0.0145(19) 0.013(2) -0.0092(18) C26 0.035(3) 0.030(2) 0.037(2) -0.0003(17) 0.0033(19) -0.0055(18) C7 0.039(3) 0.023(2) 0.045(3) -0.0043(17) -0.001(2) -0.0041(18) Ir' 0.02924(10) 0.02629(8) 0.02070(8) -0.00894(6) -0.00338(6) -0.00112(6) P' 0.0249(5) 0.0233(5) 0.0193(4) -0.0074(4) 0.0023(4) -0.0049(4) C1' 0.060(3) 0.035(2) 0.025(2) -0.0017(17) -0.001(2) -0.001(2) C4' 0.045(3) 0.040(2) 0.037(2) -0.027(2) -0.002(2) 0.003(2) C5' 0.058(3) 0.041(2) 0.043(3) -0.027(2) -0.010(2) -0.009(2) C6' 0.055(3) 0.063(3) 0.049(3) -0.033(3) -0.021(3) 0.000(3) C7' 0.046(3) 0.044(3) 0.028(2) -0.0061(18) 0.010(2) -0.017(2) C8' 0.029(3) 0.066(3) 0.043(3) -0.024(2) 0.008(2) -0.010(2) C9' 0.031(2) 0.050(3) 0.040(2) -0.023(2) -0.0039(19) 0.009(2) C10' 0.032(2) 0.0263(19) 0.029(2) -0.0076(16) 0.0010(17) -0.0055(17) C11' 0.031(2) 0.029(2) 0.032(2) -0.0086(16) 0.0023(17) -0.0056(17) C12' 0.038(3) 0.028(2) 0.054(3) -0.0099(19) 0.008(2) -0.0089(19) C13' 0.038(3) 0.039(2) 0.041(3) 0.0029(19) 0.016(2) -0.009(2) C14' 0.044(3) 0.049(3) 0.031(2) -0.010(2) 0.011(2) -0.004(2) C15' 0.039(3) 0.042(2) 0.028(2) -0.0119(18) 0.0112(19) -0.013(2) C16' 0.027(2) 0.0241(18) 0.0216(18) -0.0093(14) 0.0011(15) -0.0001(15) C17' 0.028(2) 0.031(2) 0.042(2) -0.0140(18) -0.0005(19) -0.0055(17) C18' 0.025(2) 0.046(3) 0.040(2) -0.014(2) -0.0062(19) 0.0008(19) C19' 0.041(3) 0.031(2) 0.039(2) -0.0078(18) -0.004(2) 0.0055(19) C20' 0.042(3) 0.026(2) 0.047(3) -0.0067(18) -0.011(2) -0.0025(19) C21' 0.030(2) 0.030(2) 0.038(2) -0.0104(17) -0.0064(18) -0.0039(17) C22' 0.021(2) 0.0278(18) 0.0206(17) -0.0083(14) -0.0004(14) -0.0057(15) C23' 0.035(2) 0.0271(19) 0.0257(19) -0.0056(15) -0.0017(17) -0.0064(17) C24' 0.039(3) 0.042(2) 0.0212(19) -0.0083(17) 0.0017(17) -0.0117(19) C25' 0.037(3) 0.045(2) 0.028(2) -0.0178(18) 0.0053(18) -0.011(2) C26' 0.035(2) 0.032(2) 0.036(2) -0.0160(18) 0.0032(19) -0.0038(18) C27' 0.030(2) 0.0277(19) 0.0241(19) -0.0063(15) 0.0014(16) -0.0040(16) C27 0.032(2) 0.0260(19) 0.031(2) -0.0038(16) -0.0032(17) -0.0089(17) _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 Ir C5 2.144(5) . ? Ir C8 2.147(4) . ? Ir C1 2.168(4) . ? Ir C6 2.187(5) . ? Ir C4 2.204(4) . ? Ir C9 2.205(4) . ? Ir C7 2.264(4) . ? Ir P 2.3082(10) . ? P C10 1.825(4) . ? P C16 1.837(4) . ? P C22 1.848(4) . ? C1 C2 1.488(6) . ? C2 C3 1.314(7) . ? C4 C5 1.415(7) . ? C5 C6 1.419(7) . ? C8 C7 1.395(6) . ? C8 C9 1.416(7) . ? C10 C15 1.400(5) . ? C10 C11 1.402(5) . ? C11 C12 1.381(6) . ? C12 C13 1.377(6) . ? C13 C14 1.386(6) . ? C14 C15 1.397(6) . ? C16 C17 1.393(6) . ? C16 C21 1.394(5) . ? C17 C18 1.386(5) . ? C18 C19 1.382(6) . ? C19 C20 1.372(6) . ? C20 C21 1.401(5) . ? C22 C23 1.383(5) . ? C22 C27 1.396(5) . ? C23 C24 1.396(6) . ? C24 C25 1.376(7) . ? C25 C26 1.378(6) . ? C26 C27 1.376(5) . ? Ir' C5' 2.141(4) . ? Ir' C8' 2.147(5) . ? Ir' C1' 2.165(4) . ? Ir' C9' 2.187(4) . ? Ir' C6' 2.206(5) . ? Ir' C4' 2.208(4) . ? Ir' C7' 2.272(4) . ? Ir' P' 2.3134(10) . ? P' C10' 1.823(4) . ? P' C22' 1.833(3) . ? P' C16' 1.846(4) . ? C1' C2B' 1.408(14) . ? C1' C2A' 1.531(10) . ? C2A' C3' 1.247(11) . ? C2B' C3' 1.210(15) . ? C4' C5' 1.417(7) . ? C5' C6' 1.427(7) . ? C7' C8' 1.399(7) . ? C8' C9' 1.415(7) . ? C10' C15' 1.398(5) . ? C10' C11' 1.401(5) . ? C11' C12' 1.393(6) . ? C12' C13' 1.373(6) . ? C13' C14' 1.374(7) . ? C14' C15' 1.380(6) . ? C16' C21' 1.387(5) . ? C16' C17' 1.390(6) . ? C17' C18' 1.378(6) . ? C18' C19' 1.386(6) . ? C19' C20' 1.375(7) . ? C20' C21' 1.392(6) . ? C22' C23' 1.380(5) . ? C22' C27' 1.406(5) . ? C23' C24' 1.381(5) . ? C24' C25' 1.377(6) . ? C25' C26' 1.381(6) . ? C26' C27' 1.385(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Ir C8 98.64(19) . . ? C5 Ir C1 103.82(18) . . ? C8 Ir C1 128.51(17) . . ? C5 Ir C6 38.24(19) . . ? C8 Ir C6 87.26(18) . . ? C1 Ir C6 83.02(18) . . ? C5 Ir C4 37.95(18) . . ? C8 Ir C4 133.22(18) . . ? C1 Ir C4 87.99(17) . . ? C6 Ir C4 67.05(18) . . ? C5 Ir C9 130.8(2) . . ? C8 Ir C9 37.94(17) . . ? C1 Ir C9 95.89(17) . . ? C6 Ir C9 102.82(19) . . ? C4 Ir C9 168.70(18) . . ? C5 Ir C7 91.07(18) . . ? C8 Ir C7 36.74(16) . . ? C1 Ir C7 161.79(17) . . ? C6 Ir C7 103.31(17) . . ? C4 Ir C7 110.21(17) . . ? C9 Ir C7 66.16(17) . . ? C5 Ir P 125.88(16) . . ? C8 Ir P 110.63(13) . . ? C1 Ir P 92.38(12) . . ? C6 Ir P 159.76(13) . . ? C4 Ir P 93.18(13) . . ? C9 Ir P 97.24(14) . . ? C7 Ir P 87.13(12) . . ? C10 P C16 100.77(17) . . ? C10 P C22 104.75(18) . . ? C16 P C22 99.13(16) . . ? C10 P Ir 116.17(13) . . ? C16 P Ir 116.62(13) . . ? C22 P Ir 116.82(12) . . ? C2 C1 Ir 112.7(3) . . ? C3 C2 C1 128.6(5) . . ? C5 C4 Ir 68.7(3) . . ? C4 C5 C6 117.7(4) . . ? C4 C5 Ir 73.3(3) . . ? C6 C5 Ir 72.5(3) . . ? C5 C6 Ir 69.2(3) . . ? C7 C8 C9 120.5(4) . . ? C7 C8 Ir 76.2(2) . . ? C9 C8 Ir 73.3(2) . . ? C8 C9 Ir 68.8(2) . . ? C15 C10 C11 117.8(4) . . ? C15 C10 P 122.0(3) . . ? C11 C10 P 120.0(3) . . ? C12 C11 C10 120.9(4) . . ? C13 C12 C11 120.8(4) . . ? C12 C13 C14 119.7(4) . . ? C13 C14 C15 119.9(4) . . ? C14 C15 C10 120.9(4) . . ? C17 C16 C21 118.8(3) . . ? C17 C16 P 119.8(3) . . ? C21 C16 P 121.2(3) . . ? C18 C17 C16 120.8(4) . . ? C19 C18 C17 120.0(4) . . ? C20 C19 C18 119.9(4) . . ? C19 C20 C21 120.7(4) . . ? C16 C21 C20 119.7(4) . . ? C23 C22 C27 118.5(4) . . ? C23 C22 P 124.8(3) . . ? C27 C22 P 116.6(3) . . ? C22 C23 C24 120.1(4) . . ? C25 C24 C23 120.4(4) . . ? C24 C25 C26 119.7(4) . . ? C27 C26 C25 120.2(4) . . ? C8 C7 Ir 67.1(2) . . ? C5' Ir' C8' 100.00(19) . . ? C5' Ir' C1' 104.56(18) . . ? C8' Ir' C1' 127.34(19) . . ? C5' Ir' C9' 133.26(19) . . ? C8' Ir' C9' 38.11(18) . . ? C1' Ir' C9' 95.03(18) . . ? C5' Ir' C6' 38.28(18) . . ? C8' Ir' C6' 85.9(2) . . ? C1' Ir' C6' 85.7(2) . . ? C9' Ir' C6' 103.89(18) . . ? C5' Ir' C4' 38.00(18) . . ? C8' Ir' C4' 135.88(19) . . ? C1' Ir' C4' 86.16(18) . . ? C9' Ir' C4' 170.70(17) . . ? C6' Ir' C4' 66.96(18) . . ? C5' Ir' C7' 90.26(18) . . ? C8' Ir' C7' 36.77(18) . . ? C1' Ir' C7' 161.41(17) . . ? C9' Ir' C7' 66.45(17) . . ? C6' Ir' C7' 99.9(2) . . ? C4' Ir' C7' 112.37(17) . . ? C5' Ir' P' 124.12(14) . . ? C8' Ir' P' 109.58(14) . . ? C1' Ir' P' 93.77(14) . . ? C9' Ir' P' 95.72(13) . . ? C6' Ir' P' 160.36(14) . . ? C4' Ir' P' 93.40(12) . . ? C7' Ir' P' 86.87(13) . . ? C10' P' C22' 105.02(17) . . ? C10' P' C16' 99.56(18) . . ? C22' P' C16' 100.67(16) . . ? C10' P' Ir' 116.07(14) . . ? C22' P' Ir' 117.26(13) . . ? C16' P' Ir' 115.70(13) . . ? C2B' C1' C2A' 33.7(7) . . ? C2B' C1' Ir' 116.9(6) . . ? C2A' C1' Ir' 116.4(4) . . ? C3' C2A' C1' 132.2(11) . . ? C3' C2B' C1' 152.2(18) . . ? C2B' C3' C2A' 40.9(8) . . ? C5' C4' Ir' 68.4(2) . . ? C4' C5' C6' 117.8(5) . . ? C4' C5' Ir' 73.6(2) . . ? C6' C5' Ir' 73.4(2) . . ? C5' C6' Ir' 68.4(2) . . ? C8' C7' Ir' 66.8(3) . . ? C7' C8' C9' 120.6(5) . . ? C7' C8' Ir' 76.5(3) . . ? C9' C8' Ir' 72.5(3) . . ? C8' C9' Ir' 69.4(2) . . ? C15' C10' C11' 117.1(4) . . ? C15' C10' P' 117.4(3) . . ? C11' C10' P' 125.5(3) . . ? C12' C11' C10' 120.5(4) . . ? C13' C12' C11' 120.6(4) . . ? C12' C13' C14' 119.9(4) . . ? C13' C14' C15' 119.9(4) . . ? C14' C15' C10' 122.0(4) . . ? C21' C16' C17' 118.2(4) . . ? C21' C16' P' 122.2(3) . . ? C17' C16' P' 119.6(3) . . ? C18' C17' C16' 121.5(4) . . ? C17' C18' C19' 119.7(4) . . ? C20' C19' C18' 119.6(4) . . ? C19' C20' C21' 120.5(4) . . ? C16' C21' C20' 120.4(4) . . ? C23' C22' C27' 118.2(3) . . ? C23' C22' P' 122.0(3) . . ? C27' C22' P' 119.5(3) . . ? C22' C23' C24' 120.6(4) . . ? C25' C24' C23' 121.2(4) . . ? C24' C25' C26' 119.1(4) . . ? C25' C26' C27' 120.2(4) . . ? C26' C27' C22' 120.7(4) . . ? C26 C27 C22 121.0(4) . . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 26.56 _diffrn_measured_fraction_theta_full 0.908 _refine_diff_density_max 1.940 _refine_diff_density_min -1.670 _refine_diff_density_rms 0.122 # Disorder of a terminal carbon in a sigma-allyl group (C9) observed # Severly disorderd toluene observed data_ccd140a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; (bis(2-diphenylphosphinoethyl)phenylphosphine)tris(sigma-allyl)iridium ; _publ_contact_author ; R. Thomas Baker CST-18 MS J514 Los Alamos National Laboratory Los Alamos, NM 87545 USA ; _publ_contact_author_email 'weg@lanl.gov' loop_ _publ_author_name 'Kevin D. John' 'Kenneth V. Salazar' 'Brian L. Scott' 'R. Thomas Baker' 'Alfred P. Sattelberger' _publ_requested_journal 'Chemical Communications' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H48 Ir P3 (C7 H8)' _chemical_formula_weight 942.06 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ir' 'Ir' -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.2226(5) _cell_length_b 25.4429(13) _cell_length_c 16.3141(8) _cell_angle_alpha 90.00 _cell_angle_beta 106.450(1) _cell_angle_gamma 90.00 _cell_volume 4467.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'multifaceted block' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_crystal_preparation 'crystallized from toluene' _exptl_absorpt_coefficient_mu 3.13 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22711 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 26.39 _reflns_number_total 8890 _reflns_number_gt 7159 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0413P)^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 8890 _refine_ls_number_parameters 434 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0761 _refine_ls_wR_factor_gt 0.0733 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 Ir Ir 0.844890(13) 0.212752(5) -0.000119(8) 0.02278(5) Uani 1 1 d . . . P1 P 0.90837(10) 0.15321(4) 0.11333(6) 0.0312(2) Uani 1 1 d . . . P2 P 0.93122(11) 0.27585(4) 0.09937(6) 0.0328(2) Uani 1 1 d . . . P3 P 1.03044(10) 0.22032(4) -0.03748(8) 0.0364(3) Uani 1 1 d . . . C1 C 0.6665(4) 0.21466(15) 0.0309(3) 0.0369(9) Uani 1 1 d . . . H1A H 0.6182 0.1846 0.0033 0.044 Uiso 1 1 calc R . . H1B H 0.6840 0.2094 0.0920 0.044 Uiso 1 1 calc R . . C2 C 0.5858(4) 0.26192(17) 0.0081(3) 0.0435(11) Uani 1 1 d . . . H2A H 0.6123 0.2922 0.0399 0.052 Uiso 1 1 calc R . . C3 C 0.4799(4) 0.2647(2) -0.0530(4) 0.0580(14) Uani 1 1 d . . . H3A H 0.4498 0.2353 -0.0864 0.070 Uiso 1 1 calc R . . H3B H 0.4354 0.2960 -0.0628 0.070 Uiso 1 1 calc R . . C4 C 0.7737(4) 0.15112(17) -0.0969(2) 0.0369(10) Uani 1 1 d . . . H4A H 0.8106 0.1571 -0.1431 0.044 Uiso 1 1 calc R . . H4B H 0.8057 0.1178 -0.0710 0.044 Uiso 1 1 calc R . . C5 C 0.6400(4) 0.14471(19) -0.1353(3) 0.0497(12) Uani 1 1 d . . . H5A H 0.5957 0.1753 -0.1551 0.060 Uiso 1 1 calc R . . C6 C 0.5750(5) 0.1015(2) -0.1451(3) 0.0608(15) Uani 1 1 d . . . H6A H 0.6140 0.0696 -0.1265 0.073 Uiso 1 1 calc R . . H6B H 0.4897 0.1025 -0.1707 0.073 Uiso 1 1 calc R . . C7 C 0.7594(4) 0.26608(16) -0.1054(2) 0.0322(9) Uani 1 1 d . . . H7A H 0.7952 0.2585 -0.1517 0.039 Uiso 1 1 calc R . . H7B H 0.6718 0.2574 -0.1257 0.039 Uiso 1 1 calc R . . C8 C 0.7691(6) 0.3231(2) -0.0899(3) 0.0639(16) Uani 1 1 d . . . C9 C 0.8086(8) 0.3610(3) -0.1237(5) 0.066(3) Uani 0.710(17) 1 d P . . C9A C 0.7191(17) 0.3623(7) -0.0971(10) 0.046(6) Uani 0.290(17) 1 d P . . C10 C 0.9518(6) 0.19201(18) 0.2131(3) 0.0606(16) Uani 1 1 d . . . H10A H 0.8782 0.1986 0.2315 0.073 Uiso 1 1 calc R . . H10B H 1.0096 0.1719 0.2575 0.073 Uiso 1 1 calc R . . C11 C 1.0111(6) 0.24397(17) 0.2015(3) 0.0654(17) Uani 1 1 d . . . H11A H 1.0974 0.2380 0.2037 0.078 Uiso 1 1 calc R . . H11B H 1.0094 0.2673 0.2482 0.078 Uiso 1 1 calc R . . C12 C 1.0615(4) 0.30740(18) 0.0705(3) 0.0491(12) Uani 1 1 d . . . H12A H 1.0305 0.3323 0.0244 0.059 Uiso 1 1 calc R . . H12B H 1.1143 0.3260 0.1193 0.059 Uiso 1 1 calc R . . C13 C 1.1346(4) 0.26375(19) 0.0423(4) 0.0598(15) Uani 1 1 d . . . H13A H 1.1785 0.2432 0.0917 0.072 Uiso 1 1 calc R . . H13B H 1.1958 0.2792 0.0178 0.072 Uiso 1 1 calc R . . C14 C 0.7999(4) 0.10663(16) 0.1401(3) 0.0400(10) Uani 1 1 d . . . C15 C 0.8273(5) 0.08529(19) 0.2224(3) 0.0547(13) Uani 1 1 d . . . H15A H 0.9004 0.0950 0.2630 0.066 Uiso 1 1 calc R . . C16 C 0.7479(6) 0.0502(2) 0.2446(4) 0.0671(17) Uani 1 1 d . . . H16A H 0.7676 0.0369 0.2999 0.080 Uiso 1 1 calc R . . C17 C 0.6419(7) 0.03485(19) 0.1866(4) 0.0700(18) Uani 1 1 d . . . H17A H 0.5883 0.0115 0.2021 0.084 Uiso 1 1 calc R . . C18 C 0.6132(5) 0.0544(2) 0.1029(4) 0.0655(15) Uani 1 1 d . . . H18A H 0.5411 0.0436 0.0625 0.079 Uiso 1 1 calc R . . C19 C 0.6928(5) 0.09011(17) 0.0803(3) 0.0495(12) Uani 1 1 d . . . H19A H 0.6737 0.1029 0.0246 0.059 Uiso 1 1 calc R . . C20 C 1.0406(4) 0.10911(15) 0.1245(3) 0.0373(10) Uani 1 1 d . . . C21 C 1.1612(5) 0.1250(2) 0.1576(4) 0.0755(19) Uani 1 1 d . . . H21A H 1.1774 0.1594 0.1768 0.091 Uiso 1 1 calc R . . C22 C 1.2601(5) 0.0908(2) 0.1630(5) 0.098(3) Uani 1 1 d . . . H22A H 1.3412 0.1027 0.1857 0.117 Uiso 1 1 calc R . . C23 C 1.2391(5) 0.0403(2) 0.1353(4) 0.0714(17) Uani 1 1 d . . . H23A H 1.3055 0.0176 0.1393 0.086 Uiso 1 1 calc R . . C24 C 1.1198(5) 0.02305(18) 0.1016(3) 0.0512(12) Uani 1 1 d . . . H24A H 1.1048 -0.0115 0.0828 0.061 Uiso 1 1 calc R . . C25 C 1.0209(4) 0.05728(16) 0.0955(3) 0.0399(10) Uani 1 1 d . . . H25A H 0.9402 0.0454 0.0716 0.048 Uiso 1 1 calc R . . C26 C 0.8522(4) 0.32949(15) 0.1360(2) 0.0374(10) Uani 1 1 d . . . C27 C 0.7821(5) 0.31902(18) 0.1923(3) 0.0548(13) Uani 1 1 d . . . H27A H 0.7770 0.2847 0.2106 0.066 Uiso 1 1 calc R . . C28 C 0.7201(6) 0.3583(2) 0.2215(4) 0.0685(16) Uani 1 1 d . . . H28A H 0.6761 0.3504 0.2604 0.082 Uiso 1 1 calc R . . C29 C 0.7227(5) 0.4090(2) 0.1938(4) 0.0656(16) Uani 1 1 d . . . H29A H 0.6798 0.4353 0.2130 0.079 Uiso 1 1 calc R . . C30 C 0.7891(5) 0.42051(18) 0.1375(3) 0.0594(14) Uani 1 1 d . . . H30A H 0.7908 0.4549 0.1183 0.071 Uiso 1 1 calc R . . C31 C 0.8546(5) 0.38128(16) 0.1084(3) 0.0450(11) Uani 1 1 d . . . H31A H 0.8998 0.3898 0.0704 0.054 Uiso 1 1 calc R . . C32 C 1.0261(5) 0.25076(18) -0.1416(4) 0.0548(14) Uani 1 1 d . . . C33 C 1.0749(6) 0.3008(2) -0.1471(5) 0.091(2) Uani 1 1 d . . . H33A H 1.1114 0.3198 -0.0976 0.109 Uiso 1 1 calc R . . C34 C 1.0686(9) 0.3224(3) -0.2280(7) 0.124(4) Uani 1 1 d . . . H34A H 1.1000 0.3559 -0.2319 0.149 Uiso 1 1 calc R . . C35 C 1.0179(9) 0.2950(3) -0.2986(7) 0.130(5) Uani 1 1 d . . . H35A H 1.0152 0.3094 -0.3515 0.156 Uiso 1 1 calc R . . C36 C 0.9682(7) 0.2445(3) -0.2950(4) 0.095(3) Uani 1 1 d . . . H36A H 0.9320 0.2259 -0.3449 0.115 Uiso 1 1 calc R . . C37 C 0.9740(6) 0.2232(2) -0.2165(4) 0.0677(17) Uani 1 1 d . . . H37A H 0.9423 0.1897 -0.2137 0.081 Uiso 1 1 calc R . . C38 C 1.1335(4) 0.16481(16) -0.0445(3) 0.0387(10) Uani 1 1 d . . . C39 C 1.2609(5) 0.1714(2) -0.0241(4) 0.0759(19) Uani 1 1 d . . . H39A H 1.2961 0.2032 -0.0018 0.091 Uiso 1 1 calc R . . C40 C 1.3359(5) 0.1313(2) -0.0364(5) 0.087(2) Uani 1 1 d . . . H40A H 1.4214 0.1364 -0.0226 0.104 Uiso 1 1 calc R . . C41 C 1.2865(5) 0.08378(19) -0.0688(4) 0.0604(15) Uani 1 1 d . . . H41A H 1.3380 0.0566 -0.0760 0.072 Uiso 1 1 calc R . . C42 C 1.1591(5) 0.07687(17) -0.0906(3) 0.0495(12) Uani 1 1 d . . . H42A H 1.1243 0.0451 -0.1139 0.059 Uiso 1 1 calc R . . C43 C 1.0831(4) 0.11730(16) -0.0776(3) 0.0408(10) Uani 1 1 d . . . H43A H 0.9976 0.1123 -0.0914 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir 0.02270(9) 0.02696(8) 0.01771(8) -0.00154(6) 0.00416(5) -0.00005(6) P1 0.0427(6) 0.0263(5) 0.0209(5) -0.0013(4) 0.0031(4) 0.0026(4) P2 0.0414(6) 0.0260(5) 0.0255(5) -0.0048(4) 0.0004(5) 0.0018(4) P3 0.0304(6) 0.0303(6) 0.0529(7) -0.0046(5) 0.0192(5) -0.0025(4) C1 0.033(2) 0.039(2) 0.045(2) 0.0010(19) 0.0217(19) -0.0005(18) C2 0.034(3) 0.039(2) 0.065(3) -0.002(2) 0.026(2) 0.006(2) C3 0.033(3) 0.057(3) 0.087(4) 0.004(3) 0.022(3) 0.012(2) C4 0.035(2) 0.049(3) 0.027(2) -0.0079(18) 0.0096(17) -0.0063(19) C5 0.049(3) 0.045(3) 0.042(3) -0.001(2) -0.007(2) -0.001(2) C6 0.038(3) 0.051(3) 0.078(4) -0.020(3) -0.007(3) -0.004(2) C7 0.026(2) 0.046(2) 0.0223(19) 0.0069(17) 0.0021(16) 0.0049(18) C8 0.084(4) 0.043(3) 0.039(3) 0.015(2) -0.023(3) -0.005(3) C9 0.062(6) 0.060(5) 0.064(5) 0.020(4) -0.003(4) -0.020(4) C9A 0.042(12) 0.049(11) 0.043(9) 0.006(8) 0.003(7) -0.002(8) C10 0.115(5) 0.034(2) 0.021(2) -0.0007(18) -0.001(3) 0.012(3) C11 0.106(4) 0.031(2) 0.034(2) -0.0119(19) -0.022(3) 0.009(3) C12 0.032(3) 0.037(2) 0.074(3) -0.019(2) 0.008(2) -0.007(2) C13 0.026(3) 0.043(3) 0.109(5) -0.032(3) 0.016(3) -0.008(2) C14 0.059(3) 0.029(2) 0.041(2) 0.0061(18) 0.029(2) 0.009(2) C15 0.070(3) 0.054(3) 0.048(3) 0.011(2) 0.029(3) 0.013(3) C16 0.103(5) 0.055(3) 0.062(4) 0.023(3) 0.054(4) 0.015(3) C17 0.106(5) 0.033(3) 0.096(5) 0.017(3) 0.070(4) 0.010(3) C18 0.073(4) 0.042(3) 0.084(4) 0.003(3) 0.027(3) -0.005(3) C19 0.067(3) 0.031(2) 0.054(3) 0.005(2) 0.022(3) -0.002(2) C20 0.044(3) 0.029(2) 0.031(2) 0.0035(17) -0.0020(19) 0.0043(18) C21 0.046(3) 0.041(3) 0.110(5) 0.002(3) -0.026(3) 0.001(2) C22 0.039(3) 0.055(4) 0.166(7) 0.015(4) -0.025(4) 0.004(3) C23 0.047(3) 0.054(3) 0.109(5) 0.018(3) 0.014(3) 0.016(3) C24 0.061(3) 0.033(2) 0.060(3) 0.001(2) 0.017(3) 0.010(2) C25 0.042(3) 0.039(2) 0.038(2) -0.0040(19) 0.0084(19) 0.0004(19) C26 0.055(3) 0.031(2) 0.027(2) -0.0070(16) 0.0127(19) 0.0013(19) C27 0.090(4) 0.036(3) 0.049(3) -0.016(2) 0.037(3) -0.017(3) C28 0.104(5) 0.052(3) 0.073(4) -0.024(3) 0.063(3) -0.024(3) C29 0.079(4) 0.053(3) 0.079(4) -0.026(3) 0.045(3) -0.002(3) C30 0.079(4) 0.029(2) 0.076(4) -0.005(2) 0.032(3) 0.008(2) C31 0.067(3) 0.030(2) 0.043(2) 0.0000(18) 0.025(2) 0.008(2) C32 0.061(3) 0.036(2) 0.088(4) 0.015(3) 0.056(3) 0.012(2) C33 0.107(5) 0.042(3) 0.164(7) 0.023(4) 0.104(5) 0.009(3) C34 0.171(9) 0.062(5) 0.206(10) 0.052(5) 0.162(9) 0.035(5) C35 0.170(9) 0.103(6) 0.184(10) 0.095(6) 0.159(9) 0.089(6) C36 0.132(6) 0.101(5) 0.085(5) 0.046(4) 0.082(5) 0.063(5) C37 0.097(5) 0.058(3) 0.073(4) 0.020(3) 0.065(4) 0.031(3) C38 0.031(2) 0.034(2) 0.057(3) -0.0032(19) 0.022(2) 0.0005(18) C39 0.034(3) 0.051(3) 0.151(6) -0.028(3) 0.040(3) -0.004(2) C40 0.036(3) 0.062(4) 0.169(7) -0.025(4) 0.041(4) 0.002(3) C41 0.049(3) 0.039(3) 0.103(4) -0.003(3) 0.039(3) 0.010(2) C42 0.059(3) 0.032(2) 0.068(3) -0.002(2) 0.035(3) 0.000(2) C43 0.036(2) 0.038(2) 0.056(3) -0.001(2) 0.023(2) -0.0031(19) _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 Ir C7 2.186(4) . ? Ir C1 2.200(4) . ? Ir C4 2.208(4) . ? Ir P2 2.2935(10) . ? Ir P3 2.3374(11) . ? Ir P1 2.3412(10) . ? P1 C20 1.828(4) . ? P1 C14 1.838(4) . ? P1 C10 1.848(4) . ? P2 C26 1.818(4) . ? P2 C11 1.841(4) . ? P2 C12 1.842(5) . ? P3 C13 1.849(5) . ? P3 C38 1.850(4) . ? P3 C32 1.854(5) . ? C1 C2 1.488(6) . ? C2 C3 1.319(6) . ? C4 C5 1.463(6) . ? C5 C6 1.304(6) . ? C7 C8 1.471(7) . ? C8 C9A 1.133(17) . ? C8 C9 1.253(9) . ? C9 C9A 1.202(18) . ? C10 C11 1.516(7) . ? C12 C13 1.527(6) . ? C14 C19 1.382(6) . ? C14 C15 1.400(6) . ? C15 C16 1.380(7) . ? C16 C17 1.350(8) . ? C17 C18 1.403(8) . ? C18 C19 1.394(7) . ? C20 C21 1.368(6) . ? C20 C25 1.397(6) . ? C21 C22 1.393(7) . ? C22 C23 1.362(8) . ? C23 C24 1.368(7) . ? C24 C25 1.392(6) . ? C26 C27 1.394(6) . ? C26 C31 1.396(6) . ? C27 C28 1.377(7) . ? C28 C29 1.370(7) . ? C29 C30 1.368(7) . ? C30 C31 1.400(6) . ? C32 C37 1.387(8) . ? C32 C33 1.400(7) . ? C33 C34 1.414(10) . ? C34 C35 1.329(14) . ? C35 C36 1.407(11) . ? C36 C37 1.375(7) . ? C38 C43 1.379(6) . ? C38 C39 1.383(6) . ? C39 C40 1.372(7) . ? C40 C41 1.372(7) . ? C41 C42 1.383(7) . ? C42 C43 1.391(6) . ? 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 C7 Ir C1 86.64(15) . . ? C7 Ir C4 83.67(16) . . ? C1 Ir C4 90.67(15) . . ? C7 Ir P2 97.18(11) . . ? C1 Ir P2 92.94(12) . . ? C4 Ir P2 176.33(11) . . ? C7 Ir P3 88.23(11) . . ? C1 Ir P3 173.75(11) . . ? C4 Ir P3 92.33(11) . . ? P2 Ir P3 84.14(4) . . ? C7 Ir P1 172.05(11) . . ? C1 Ir P1 85.73(11) . . ? C4 Ir P1 94.19(11) . . ? P2 Ir P1 85.44(4) . . ? P3 Ir P1 99.52(4) . . ? C20 P1 C14 98.87(19) . . ? C20 P1 C10 103.6(2) . . ? C14 P1 C10 99.3(2) . . ? C20 P1 Ir 122.19(14) . . ? C14 P1 Ir 122.09(15) . . ? C10 P1 Ir 107.23(14) . . ? C26 P2 C11 101.0(2) . . ? C26 P2 C12 104.7(2) . . ? C11 P2 C12 101.8(3) . . ? C26 P2 Ir 127.62(14) . . ? C11 P2 Ir 109.38(14) . . ? C12 P2 Ir 109.32(15) . . ? C13 P3 C38 102.6(2) . . ? C13 P3 C32 104.0(3) . . ? C38 P3 C32 96.7(2) . . ? C13 P3 Ir 107.35(17) . . ? C38 P3 Ir 124.90(14) . . ? C32 P3 Ir 118.60(16) . . ? C2 C1 Ir 119.3(3) . . ? C3 C2 C1 125.9(5) . . ? C5 C4 Ir 120.3(3) . . ? C6 C5 C4 128.1(5) . . ? C8 C7 Ir 118.8(3) . . ? C9A C8 C9 60.3(9) . . ? C9A C8 C7 147.0(10) . . ? C9 C8 C7 134.5(7) . . ? C9A C9 C8 54.9(9) . . ? C8 C9A C9 64.8(11) . . ? C11 C10 P1 111.8(3) . . ? C10 C11 P2 112.3(3) . . ? C13 C12 P2 107.1(3) . . ? C12 C13 P3 111.1(3) . . ? C19 C14 C15 118.0(4) . . ? C19 C14 P1 122.0(3) . . ? C15 C14 P1 119.9(4) . . ? C16 C15 C14 121.3(5) . . ? C17 C16 C15 120.6(5) . . ? C16 C17 C18 119.5(5) . . ? C19 C18 C17 120.1(6) . . ? C14 C19 C18 120.3(5) . . ? C21 C20 C25 117.1(4) . . ? C21 C20 P1 122.8(3) . . ? C25 C20 P1 120.0(3) . . ? C20 C21 C22 121.5(5) . . ? C23 C22 C21 120.5(5) . . ? C22 C23 C24 119.6(5) . . ? C23 C24 C25 119.9(4) . . ? C24 C25 C20 121.4(4) . . ? C27 C26 C31 117.4(4) . . ? C27 C26 P2 119.5(3) . . ? C31 C26 P2 123.1(3) . . ? C28 C27 C26 121.5(4) . . ? C29 C28 C27 120.7(5) . . ? C30 C29 C28 119.3(5) . . ? C29 C30 C31 120.9(5) . . ? C26 C31 C30 120.2(4) . . ? C37 C32 C33 118.6(5) . . ? C37 C32 P3 119.5(4) . . ? C33 C32 P3 122.0(5) . . ? C32 C33 C34 119.8(8) . . ? C35 C34 C33 120.1(7) . . ? C34 C35 C36 121.4(7) . . ? C37 C36 C35 118.9(8) . . ? C36 C37 C32 121.3(6) . . ? C43 C38 C39 118.8(4) . . ? C43 C38 P3 119.9(3) . . ? C39 C38 P3 121.0(3) . . ? C40 C39 C38 120.7(5) . . ? C39 C40 C41 120.9(5) . . ? C40 C41 C42 119.1(4) . . ? C41 C42 C43 120.1(4) . . ? C38 C43 C42 120.4(4) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.136 _refine_diff_density_min -1.018 _refine_diff_density_rms 0.143 # Severly disorderd toluene observed data_ccd163a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; (1,2-bis(diphenylphosphino)benzene)bis(sigma-allyl)(pi-allyl)iridium ; _publ_contact_author ; R. Thomas Baker CST-18 MS J514 Los Alamos National Laboratory Los Alamos, NM 87545 USA ; _publ_contact_author_email 'weg@lanl.gov' loop_ _publ_author_name 'Kevin D. John' 'Kenneth V. Salazar' 'Brian L. Scott' 'R. Thomas Baker' 'Alfred P. Sattelberger' _publ_requested_journal 'Chemical Communications' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H39 Ir P2 2(C7 H8)' _chemical_formula_weight 946.17 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' '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7816(5) _cell_length_b 13.5959(6) _cell_length_c 13.9441(6) _cell_angle_alpha 86.058(1) _cell_angle_beta 71.302(1) _cell_angle_gamma 83.341(1) _cell_volume 1921.98(15) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'multifaceted block' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_crystal_preparation 'crystallized from toluene' _exptl_absorpt_coefficient_mu 3.60 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10344 _diffrn_reflns_av_R_equivalents 0.0144 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 26.40 _reflns_number_total 7345 _reflns_number_gt 6790 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0173P)^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 7345 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0205 _refine_ls_R_factor_gt 0.0179 _refine_ls_wR_factor_ref 0.0421 _refine_ls_wR_factor_gt 0.0414 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.001 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 Ir Ir 0.225694(8) 0.214667(6) -0.248860(7) 0.02595(3) Uani 1 1 d . . . P1 P 0.02179(6) 0.23775(4) -0.13091(4) 0.02604(12) Uani 1 1 d . . . P2 P 0.12989(6) 0.31069(4) -0.35051(4) 0.02640(12) Uani 1 1 d . . . C1 C 0.2702(2) 0.34809(18) -0.19276(19) 0.0343(5) Uani 1 1 d . . . H1A H 0.3206 0.3872 -0.2497 0.041 Uiso 1 1 calc R . . H1B H 0.1885 0.3876 -0.1596 0.041 Uiso 1 1 calc R . . C2 C 0.3453(3) 0.3253(2) -0.1207(2) 0.0422(6) Uani 1 1 d . . . H2A H 0.3006 0.2981 -0.0577 0.051 Uiso 1 1 calc R . . C3 C 0.4690(3) 0.3395(3) -0.1365(3) 0.0630(9) Uani 1 1 d . . . H3A H 0.5180 0.3665 -0.1982 0.076 Uiso 1 1 calc R . . H3B H 0.5074 0.3226 -0.0859 0.076 Uiso 1 1 calc R . . C4 C 0.4237(2) 0.2281(2) -0.3556(2) 0.0394(6) Uani 1 1 d . . . H4A H 0.4196 0.2904 -0.3932 0.047 Uiso 1 1 calc R . . H4B H 0.4808 0.2344 -0.3154 0.047 Uiso 1 1 calc R . . C5 C 0.4900(3) 0.1532(3) -0.4292(2) 0.0548(8) Uani 1 1 d . . . H5A H 0.4583 0.1514 -0.4837 0.066 Uiso 1 1 calc R . . C6 C 0.5897(3) 0.0875(3) -0.4281(3) 0.0658(9) Uani 1 1 d . . . H6A H 0.6256 0.0858 -0.3755 0.079 Uiso 1 1 calc R . . H6B H 0.6242 0.0428 -0.4799 0.079 Uiso 1 1 calc R . . C9 C 0.3249(3) 0.1058(2) -0.1663(2) 0.0441(7) Uani 1 1 d . . . H9A H 0.4166 0.0844 -0.2008 0.053 Uiso 1 1 calc R . . H9B H 0.3059 0.1159 -0.0946 0.053 Uiso 1 1 calc R . . C8 C 0.2306(3) 0.06010(18) -0.1942(2) 0.0414(6) Uani 1 1 d . . . H8A H 0.1537 0.0377 -0.1411 0.050 Uiso 1 1 calc R . . C7 C 0.2372(3) 0.05648(18) -0.2960(2) 0.0427(6) Uani 1 1 d . . . H7A H 0.1605 0.0371 -0.3091 0.051 Uiso 1 1 calc R . . H7B H 0.3201 0.0296 -0.3427 0.051 Uiso 1 1 calc R . . C10 C -0.0659(2) 0.34870(16) -0.16995(17) 0.0269(5) Uani 1 1 d . . . C11 C -0.0160(2) 0.38309(17) -0.27041(17) 0.0277(5) Uani 1 1 d . . . C12 C -0.0826(2) 0.46555(18) -0.30449(19) 0.0340(5) Uani 1 1 d . . . H12A H -0.0498 0.4893 -0.3710 0.041 Uiso 1 1 calc R . . C13 C -0.1968(2) 0.5120(2) -0.2399(2) 0.0401(6) Uani 1 1 d . . . H13A H -0.2399 0.5674 -0.2627 0.048 Uiso 1 1 calc R . . C14 C -0.2470(2) 0.4760(2) -0.1414(2) 0.0414(6) Uani 1 1 d . . . H14A H -0.3242 0.5071 -0.0983 0.050 Uiso 1 1 calc R . . C15 C -0.1837(2) 0.39440(19) -0.10652(19) 0.0347(5) Uani 1 1 d . . . H15A H -0.2194 0.3697 -0.0407 0.042 Uiso 1 1 calc R . . C16 C 0.0186(2) 0.25837(18) -0.00205(18) 0.0303(5) Uani 1 1 d . . . C17 C 0.0451(3) 0.1775(2) 0.0577(2) 0.0398(6) Uani 1 1 d . . . H17A H 0.0566 0.1138 0.0338 0.048 Uiso 1 1 calc R . . C18 C 0.0545(3) 0.1912(2) 0.1530(2) 0.0489(7) Uani 1 1 d . . . H18A H 0.0713 0.1368 0.1928 0.059 Uiso 1 1 calc R . . C19 C 0.0388(3) 0.2856(2) 0.1884(2) 0.0501(7) Uani 1 1 d . . . H19A H 0.0447 0.2947 0.2523 0.060 Uiso 1 1 calc R . . C20 C 0.0148(3) 0.3659(2) 0.1302(2) 0.0427(6) Uani 1 1 d . . . H20A H 0.0052 0.4293 0.1543 0.051 Uiso 1 1 calc R . . C21 C 0.0046(2) 0.35330(19) 0.03498(19) 0.0354(6) Uani 1 1 d . . . H21A H -0.0116 0.4084 -0.0043 0.043 Uiso 1 1 calc R . . C22 C -0.1061(2) 0.15311(17) -0.11199(18) 0.0292(5) Uani 1 1 d . . . C23 C -0.1149(2) 0.11245(18) -0.19771(19) 0.0364(6) Uani 1 1 d . . . H23A H -0.0492 0.1193 -0.2594 0.044 Uiso 1 1 calc R . . C24 C -0.2217(3) 0.0616(2) -0.1917(2) 0.0466(7) Uani 1 1 d . . . H24A H -0.2275 0.0347 -0.2496 0.056 Uiso 1 1 calc R . . C25 C -0.3198(3) 0.0505(2) -0.1000(2) 0.0481(7) Uani 1 1 d . . . H25A H -0.3917 0.0170 -0.0962 0.058 Uiso 1 1 calc R . . C26 C -0.3100(2) 0.0897(2) -0.0144(2) 0.0425(6) Uani 1 1 d . . . H26A H -0.3749 0.0814 0.0475 0.051 Uiso 1 1 calc R . . C27 C -0.2045(2) 0.14126(19) -0.01981(19) 0.0358(6) Uani 1 1 d . . . H27A H -0.1992 0.1680 0.0382 0.043 Uiso 1 1 calc R . . C28 C 0.0657(2) 0.24599(17) -0.43336(18) 0.0312(5) Uani 1 1 d . . . C29 C -0.0587(3) 0.2696(2) -0.4428(2) 0.0456(7) Uani 1 1 d . . . H29A H -0.1124 0.3232 -0.4088 0.055 Uiso 1 1 calc R . . C30 C -0.1037(3) 0.2142(2) -0.5023(3) 0.0573(8) Uani 1 1 d . . . H30A H -0.1878 0.2302 -0.5069 0.069 Uiso 1 1 calc R . . C31 C -0.0251(3) 0.1360(2) -0.5543(2) 0.0567(8) Uani 1 1 d . . . H31A H -0.0554 0.0993 -0.5945 0.068 Uiso 1 1 calc R . . C32 C 0.0988(3) 0.1121(2) -0.5467(2) 0.0532(8) Uani 1 1 d . . . H32A H 0.1528 0.0596 -0.5826 0.064 Uiso 1 1 calc R . . C33 C 0.1437(3) 0.1657(2) -0.4860(2) 0.0429(6) Uani 1 1 d . . . H33A H 0.2270 0.1480 -0.4803 0.052 Uiso 1 1 calc R . . C34 C 0.2223(2) 0.40434(17) -0.43569(18) 0.0293(5) Uani 1 1 d . . . C35 C 0.2314(3) 0.49479(19) -0.3985(2) 0.0377(6) Uani 1 1 d . . . H35A H 0.1845 0.5097 -0.3317 0.045 Uiso 1 1 calc R . . C36 C 0.3103(3) 0.5631(2) -0.4607(2) 0.0465(7) Uani 1 1 d . . . H36A H 0.3151 0.6237 -0.4357 0.056 Uiso 1 1 calc R . . C37 C 0.3812(3) 0.5408(2) -0.5593(2) 0.0470(7) Uani 1 1 d . . . H37A H 0.4329 0.5867 -0.6012 0.056 Uiso 1 1 calc R . . C38 C 0.3755(3) 0.4504(2) -0.5958(2) 0.0454(7) Uani 1 1 d . . . H38A H 0.4254 0.4348 -0.6618 0.055 Uiso 1 1 calc R . . C39 C 0.2960(2) 0.3829(2) -0.53497(18) 0.0360(6) Uani 1 1 d . . . H39A H 0.2918 0.3225 -0.5607 0.043 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir 0.02585(5) 0.02500(5) 0.02500(5) -0.00081(3) -0.00533(3) -0.00238(3) P1 0.0283(3) 0.0256(3) 0.0228(3) -0.0023(2) -0.0052(2) -0.0042(2) P2 0.0294(3) 0.0264(3) 0.0224(3) -0.0038(2) -0.0061(2) -0.0026(2) C1 0.0332(12) 0.0370(14) 0.0333(14) -0.0033(11) -0.0086(10) -0.0099(10) C2 0.0476(15) 0.0479(16) 0.0374(15) 0.0003(12) -0.0186(12) -0.0153(13) C3 0.0627(19) 0.088(3) 0.052(2) 0.0044(18) -0.0317(16) -0.0296(18) C4 0.0281(12) 0.0424(15) 0.0412(15) 0.0026(12) -0.0029(11) -0.0034(11) C5 0.0391(15) 0.078(2) 0.0419(17) -0.0128(16) -0.0020(13) -0.0094(15) C6 0.0435(17) 0.073(2) 0.068(2) -0.0229(18) 0.0010(15) 0.0083(16) C9 0.0414(14) 0.0404(15) 0.0459(17) 0.0078(13) -0.0138(12) 0.0088(12) C8 0.0452(14) 0.0234(12) 0.0464(17) 0.0037(11) -0.0040(12) 0.0012(11) C7 0.0436(14) 0.0255(13) 0.0537(18) -0.0085(12) -0.0079(13) 0.0001(11) C10 0.0261(11) 0.0272(12) 0.0280(12) -0.0054(9) -0.0081(9) -0.0030(9) C11 0.0285(11) 0.0279(12) 0.0263(12) -0.0043(9) -0.0079(9) -0.0011(9) C12 0.0405(13) 0.0337(13) 0.0303(13) -0.0020(10) -0.0155(11) -0.0001(10) C13 0.0403(14) 0.0391(15) 0.0450(16) -0.0074(12) -0.0219(12) 0.0084(11) C14 0.0305(12) 0.0455(16) 0.0460(16) -0.0114(13) -0.0100(11) 0.0056(11) C15 0.0329(12) 0.0388(14) 0.0295(13) -0.0035(11) -0.0056(10) -0.0028(10) C16 0.0311(11) 0.0351(13) 0.0237(12) -0.0033(10) -0.0055(9) -0.0070(10) C17 0.0463(14) 0.0406(15) 0.0316(14) -0.0017(12) -0.0111(11) -0.0036(12) C18 0.0600(18) 0.0532(18) 0.0366(16) 0.0095(14) -0.0223(13) -0.0040(14) C19 0.0558(17) 0.066(2) 0.0326(15) -0.0064(14) -0.0187(13) -0.0084(15) C20 0.0515(16) 0.0454(16) 0.0326(15) -0.0071(12) -0.0121(12) -0.0111(13) C21 0.0393(13) 0.0370(14) 0.0313(14) -0.0027(11) -0.0117(11) -0.0067(11) C22 0.0301(11) 0.0258(12) 0.0301(13) 0.0005(10) -0.0069(9) -0.0051(9) C23 0.0404(13) 0.0376(14) 0.0297(13) -0.0053(11) -0.0063(11) -0.0094(11) C24 0.0542(16) 0.0496(17) 0.0409(16) -0.0088(13) -0.0164(13) -0.0167(13) C25 0.0396(14) 0.0471(17) 0.0582(19) -0.0028(14) -0.0120(13) -0.0163(12) C26 0.0371(13) 0.0400(15) 0.0434(16) 0.0013(12) -0.0018(12) -0.0094(11) C27 0.0360(13) 0.0373(14) 0.0314(14) -0.0014(11) -0.0048(10) -0.0095(11) C28 0.0397(13) 0.0295(12) 0.0255(12) 0.0005(10) -0.0108(10) -0.0074(10) C29 0.0529(16) 0.0438(16) 0.0481(17) -0.0111(13) -0.0268(14) -0.0001(13) C30 0.067(2) 0.0542(19) 0.068(2) -0.0058(16) -0.0437(18) -0.0085(16) C31 0.089(2) 0.0482(18) 0.0490(19) -0.0037(15) -0.0388(17) -0.0206(17) C32 0.071(2) 0.0466(17) 0.0440(17) -0.0186(14) -0.0169(15) -0.0064(15) C33 0.0460(15) 0.0423(15) 0.0411(16) -0.0142(12) -0.0122(12) -0.0037(12) C34 0.0314(11) 0.0316(12) 0.0248(12) 0.0022(10) -0.0098(9) -0.0023(10) C35 0.0454(14) 0.0346(14) 0.0312(14) -0.0021(11) -0.0087(11) -0.0050(11) C36 0.0543(16) 0.0332(14) 0.0554(19) 0.0059(13) -0.0214(14) -0.0109(12) C37 0.0456(15) 0.0557(18) 0.0430(17) 0.0181(14) -0.0163(13) -0.0231(13) C38 0.0394(14) 0.068(2) 0.0270(14) 0.0073(13) -0.0077(11) -0.0130(13) C39 0.0369(13) 0.0445(15) 0.0261(13) -0.0007(11) -0.0079(10) -0.0084(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 Ir C1 2.184(2) . ? Ir C8 2.186(2) . ? Ir C4 2.196(2) . ? Ir C9 2.202(3) . ? Ir P2 2.2698(6) . ? Ir C7 2.270(2) . ? Ir P1 2.2867(6) . ? P1 C16 1.827(2) . ? P1 C10 1.831(2) . ? P1 C22 1.840(2) . ? P2 C34 1.831(2) . ? P2 C11 1.832(2) . ? P2 C28 1.839(2) . ? C1 C2 1.477(3) . ? C2 C3 1.315(4) . ? C4 C5 1.451(4) . ? C5 C6 1.320(4) . ? C9 C8 1.416(4) . ? C8 C7 1.403(4) . ? C10 C15 1.398(3) . ? C10 C11 1.398(3) . ? C11 C12 1.399(3) . ? C12 C13 1.383(3) . ? C13 C14 1.383(4) . ? C14 C15 1.377(4) . ? C16 C17 1.392(4) . ? C16 C21 1.397(3) . ? C17 C18 1.391(4) . ? C18 C19 1.379(4) . ? C19 C20 1.365(4) . ? C20 C21 1.390(3) . ? C22 C23 1.386(3) . ? C22 C27 1.393(3) . ? C23 C24 1.388(4) . ? C24 C25 1.386(4) . ? C25 C26 1.378(4) . ? C26 C27 1.384(3) . ? C28 C29 1.387(4) . ? C28 C33 1.393(3) . ? C29 C30 1.385(4) . ? C30 C31 1.370(4) . ? C31 C32 1.373(4) . ? C32 C33 1.381(4) . ? C34 C39 1.389(3) . ? C34 C35 1.392(3) . ? C35 C36 1.392(4) . ? C36 C37 1.377(4) . ? C37 C38 1.377(4) . ? C38 C39 1.381(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 C1 Ir C8 131.82(10) . . ? C1 Ir C4 80.61(10) . . ? C8 Ir C4 104.52(10) . . ? C1 Ir C9 97.40(10) . . ? C8 Ir C9 37.65(10) . . ? C4 Ir C9 85.24(10) . . ? C1 Ir P2 89.59(7) . . ? C8 Ir P2 136.87(8) . . ? C4 Ir P2 92.13(7) . . ? C9 Ir P2 172.01(8) . . ? C1 Ir C7 162.08(10) . . ? C8 Ir C7 36.63(10) . . ? C4 Ir C7 89.74(10) . . ? C9 Ir C7 66.57(11) . . ? P2 Ir C7 105.94(8) . . ? C1 Ir P1 86.79(7) . . ? C8 Ir P1 86.73(7) . . ? C4 Ir P1 166.84(7) . . ? C9 Ir P1 100.26(8) . . ? P2 Ir P1 83.92(2) . . ? C7 Ir P1 103.42(7) . . ? C16 P1 C10 106.01(11) . . ? C16 P1 C22 103.34(11) . . ? C10 P1 C22 97.84(10) . . ? C16 P1 Ir 116.01(8) . . ? C10 P1 Ir 107.83(7) . . ? C22 P1 Ir 123.28(8) . . ? C34 P2 C11 103.54(11) . . ? C34 P2 C28 103.32(11) . . ? C11 P2 C28 103.67(11) . . ? C34 P2 Ir 119.17(8) . . ? C11 P2 Ir 108.51(8) . . ? C28 P2 Ir 116.83(8) . . ? C2 C1 Ir 112.44(17) . . ? C3 C2 C1 126.6(3) . . ? C5 C4 Ir 121.76(19) . . ? C6 C5 C4 127.8(3) . . ? C8 C9 Ir 70.57(15) . . ? C7 C8 C9 121.1(3) . . ? C7 C8 Ir 74.94(15) . . ? C9 C8 Ir 71.78(15) . . ? C8 C7 Ir 68.43(14) . . ? C15 C10 C11 119.8(2) . . ? C15 C10 P1 122.86(19) . . ? C11 C10 P1 117.18(16) . . ? C10 C11 C12 119.1(2) . . ? C10 C11 P2 116.29(17) . . ? C12 C11 P2 124.52(18) . . ? C13 C12 C11 120.4(2) . . ? C14 C13 C12 120.0(2) . . ? C15 C14 C13 120.5(2) . . ? C14 C15 C10 120.1(2) . . ? C17 C16 C21 118.5(2) . . ? C17 C16 P1 118.91(18) . . ? C21 C16 P1 122.2(2) . . ? C18 C17 C16 120.5(2) . . ? C19 C18 C17 119.9(3) . . ? C20 C19 C18 120.3(3) . . ? C19 C20 C21 120.4(3) . . ? C20 C21 C16 120.3(3) . . ? C23 C22 C27 119.3(2) . . ? C23 C22 P1 117.02(18) . . ? C27 C22 P1 122.89(18) . . ? C22 C23 C24 120.2(2) . . ? C25 C24 C23 120.3(3) . . ? C26 C25 C24 119.6(2) . . ? C25 C26 C27 120.5(2) . . ? C26 C27 C22 120.1(2) . . ? C29 C28 C33 118.0(2) . . ? C29 C28 P2 123.76(19) . . ? C33 C28 P2 118.22(19) . . ? C30 C29 C28 120.8(3) . . ? C31 C30 C29 120.5(3) . . ? C30 C31 C32 119.6(3) . . ? C31 C32 C33 120.3(3) . . ? C32 C33 C28 120.8(3) . . ? C39 C34 C35 118.6(2) . . ? C39 C34 P2 120.91(19) . . ? C35 C34 P2 120.07(18) . . ? C36 C35 C34 120.4(2) . . ? C37 C36 C35 119.9(3) . . ? C36 C37 C38 120.0(3) . . ? C37 C38 C39 120.3(3) . . ? C38 C39 C34 120.6(2) . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 0.574 _refine_diff_density_min -0.408 _refine_diff_density_rms 0.060