# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Langer, Jens' _publ_contact_author_email j.langer@uni-jena.de _publ_section_title ; An iridium-mediated C-H activation/CO2-carboxylation reaction of 1,1 bisdiphenylphosphinomethane ; loop_ _publ_author_name J.Langer M.J.Fabra 'Pilar Garca-Orduna' F.Lahoz H.Gorls L.Oro ; M.Westerhausen ; # Attachment '- dalton.cif' data_FO3581 _database_code_depnum_ccdc_archive 'CCDC 770462' #TrackingRef '- dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H49 Cl Ir O P4' _chemical_formula_weight 1041.44 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' O O 0.0106 0.0060 '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' Cl Cl 0.1484 0.1585 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.9857(3) _cell_length_b 21.0322(6) _cell_length_c 21.3775(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.868(2) _cell_angle_gamma 90.00 _cell_volume 4473.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.546 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2092 _exptl_absorpt_coefficient_mu 3.226 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30048 _diffrn_reflns_av_R_equivalents 0.1292 _diffrn_reflns_av_sigmaI/netI 0.1339 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 27.46 _reflns_number_total 10210 _reflns_number_gt 6285 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+0.6562P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10210 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1232 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.1268 _refine_ls_wR_factor_gt 0.1060 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 0.77825(3) 0.129623(12) 0.183051(13) 0.02327(9) Uani 1 1 d . . . H1IR H 0.7544 0.1274 0.2562 0.035 Uiso 1 1 d . . . Cl1 Cl 0.8170(2) 0.13172(10) 0.06845(8) 0.0376(4) Uani 1 1 d . . . P1 P 0.6205(2) 0.04758(9) 0.17421(9) 0.0258(4) Uani 1 1 d . . . P2 P 0.5600(2) 0.16973(9) 0.17194(9) 0.0261(4) Uani 1 1 d . . . P3 P 0.9949(2) 0.08984(9) 0.20508(9) 0.0256(4) Uani 1 1 d . . . P4 P 0.9277(2) 0.21392(9) 0.20058(9) 0.0268(4) Uani 1 1 d . . . C1 C 0.4819(8) 0.0968(4) 0.1694(4) 0.0335(18) Uani 1 1 d . . . H1A H 0.3889 0.0865 0.1662 0.040 Uiso 1 1 calc R . . C2 C 0.6195(8) -0.0107(3) 0.1106(3) 0.0322(18) Uani 1 1 d . . . C3 C 0.7384(9) -0.0357(4) 0.0917(4) 0.039(2) Uani 1 1 d . . . H3A H 0.8226 -0.0212 0.1104 0.047 Uiso 1 1 calc R . . C4 C 0.7333(11) -0.0817(4) 0.0457(4) 0.046(2) Uani 1 1 d . . . H4A H 0.8146 -0.1000 0.0340 0.055 Uiso 1 1 calc R . . C5 C 0.6147(11) -0.1013(4) 0.0169(4) 0.049(2) Uani 1 1 d . . . H5A H 0.6130 -0.1318 -0.0158 0.058 Uiso 1 1 calc R . . C6 C 0.4980(11) -0.0771(4) 0.0350(4) 0.051(2) Uani 1 1 d . . . H6A H 0.4147 -0.0917 0.0153 0.061 Uiso 1 1 calc R . . C7 C 0.4986(10) -0.0307(4) 0.0824(4) 0.043(2) Uani 1 1 d . . . H7A H 0.4167 -0.0136 0.0945 0.051 Uiso 1 1 calc R . . C8 C 0.6218(8) -0.0076(3) 0.2413(3) 0.0278(17) Uani 1 1 d . . . C9 C 0.7311(9) -0.0459(4) 0.2580(4) 0.041(2) Uani 1 1 d . . . H9A H 0.8071 -0.0442 0.2341 0.049 Uiso 1 1 calc R . . C10 C 0.7321(10) -0.0866(4) 0.3086(4) 0.048(2) Uani 1 1 d . . . H10A H 0.8094 -0.1118 0.3200 0.058 Uiso 1 1 calc R . . C11 C 0.6224(11) -0.0910(4) 0.3426(4) 0.051(3) Uani 1 1 d . . . H11A H 0.6226 -0.1194 0.3772 0.062 Uiso 1 1 calc R . . C12 C 0.5118(12) -0.0538(4) 0.3262(4) 0.059(3) Uani 1 1 d . . . H12A H 0.4348 -0.0569 0.3492 0.071 Uiso 1 1 calc R . . C13 C 0.5120(9) -0.0115(4) 0.2761(4) 0.041(2) Uani 1 1 d . . . H13A H 0.4359 0.0148 0.2658 0.049 Uiso 1 1 calc R . . C14 C 0.5024(8) 0.2229(3) 0.1076(3) 0.0296(17) Uani 1 1 d . . . C15 C 0.3664(9) 0.2318(4) 0.0938(4) 0.045(2) Uani 1 1 d . . . H15A H 0.3048 0.2092 0.1170 0.054 Uiso 1 1 calc R . . C16 C 0.3180(10) 0.2731(4) 0.0469(4) 0.046(2) Uani 1 1 d . . . H16A H 0.2239 0.2793 0.0386 0.055 Uiso 1 1 calc R . . C17 C 0.4062(10) 0.3049(4) 0.0124(4) 0.048(2) Uani 1 1 d . . . H17A H 0.3735 0.3324 -0.0207 0.057 Uiso 1 1 calc R . . C18 C 0.5397(11) 0.2969(5) 0.0257(4) 0.058(3) Uani 1 1 d . . . H18A H 0.6003 0.3205 0.0027 0.070 Uiso 1 1 calc R . . C19 C 0.5908(9) 0.2553(4) 0.0721(4) 0.047(2) Uani 1 1 d . . . H19A H 0.6850 0.2490 0.0796 0.057 Uiso 1 1 calc R . . C20 C 0.5193(7) 0.2181(3) 0.2390(3) 0.0258(16) Uani 1 1 d . . . C21 C 0.4843(9) 0.1885(4) 0.2925(4) 0.039(2) Uani 1 1 d . . . H21A H 0.4727 0.1437 0.2931 0.047 Uiso 1 1 calc R . . C22 C 0.4659(11) 0.2244(5) 0.3460(4) 0.055(3) Uani 1 1 d . . . H22A H 0.4411 0.2036 0.3827 0.065 Uiso 1 1 calc R . . C23 C 0.4827(10) 0.2885(5) 0.3469(5) 0.055(3) Uani 1 1 d . . . H23A H 0.4689 0.3124 0.3835 0.066 Uiso 1 1 calc R . . C24 C 0.5200(10) 0.3183(4) 0.2939(4) 0.047(2) Uani 1 1 d . . . H24A H 0.5334 0.3630 0.2942 0.056 Uiso 1 1 calc R . . C25 C 0.5382(9) 0.2840(4) 0.2404(4) 0.041(2) Uani 1 1 d . . . H25A H 0.5639 0.3053 0.2041 0.049 Uiso 1 1 calc R . . C26 C 1.0759(8) 0.1653(3) 0.1845(4) 0.0302(17) Uani 1 1 d . . . H26A H 1.1569 0.1755 0.2127 0.036 Uiso 1 1 calc R . . H26B H 1.0967 0.1671 0.1401 0.036 Uiso 1 1 calc R . . C27 C 1.0700(7) 0.0252(3) 0.1638(3) 0.0277(16) Uani 1 1 d . . . C28 C 1.0874(8) 0.0306(4) 0.0996(4) 0.0363(19) Uani 1 1 d . . . H28A H 1.0696 0.0700 0.0788 0.044 Uiso 1 1 calc R . . C29 C 1.1304(9) -0.0210(4) 0.0664(4) 0.039(2) Uani 1 1 d . . . H29A H 1.1406 -0.0171 0.0228 0.047 Uiso 1 1 calc R . . C30 C 1.1585(9) -0.0779(4) 0.0964(4) 0.042(2) Uani 1 1 d . . . H30A H 1.1875 -0.1134 0.0736 0.051 Uiso 1 1 calc R . . C31 C 1.1445(10) -0.0833(4) 0.1598(4) 0.049(2) Uani 1 1 d . . . H31A H 1.1654 -0.1224 0.1807 0.058 Uiso 1 1 calc R . . C32 C 1.0998(9) -0.0318(4) 0.1932(4) 0.0367(19) Uani 1 1 d . . . H32A H 1.0898 -0.0360 0.2368 0.044 Uiso 1 1 calc R . . C33 C 1.0530(8) 0.0777(3) 0.2865(3) 0.0279(16) Uani 1 1 d . . . C34 C 0.9671(8) 0.0690(4) 0.3331(4) 0.0341(19) Uani 1 1 d . . . H34A H 0.8730 0.0664 0.3220 0.041 Uiso 1 1 calc R . . C35 C 1.0152(8) 0.0639(4) 0.3956(4) 0.0377(19) Uani 1 1 d . . . H35A H 0.9543 0.0574 0.4268 0.045 Uiso 1 1 calc R . . C36 C 1.1531(9) 0.0683(4) 0.4128(4) 0.039(2) Uani 1 1 d . . . H36A H 1.1856 0.0664 0.4558 0.047 Uiso 1 1 calc R . . C37 C 1.2415(9) 0.0756(4) 0.3676(4) 0.039(2) Uani 1 1 d . . . H37A H 1.3355 0.0777 0.3788 0.046 Uiso 1 1 calc R . . C38 C 1.1913(8) 0.0798(4) 0.3052(4) 0.0351(19) Uani 1 1 d . . . H38A H 1.2528 0.0842 0.2739 0.042 Uiso 1 1 calc R . . C39 C 0.9619(8) 0.2410(3) 0.2809(3) 0.0292(17) Uani 1 1 d . . . C40 C 0.8623(9) 0.2354(3) 0.3239(4) 0.0351(19) Uani 1 1 d . . . H40A H 0.7760 0.2191 0.3103 0.042 Uiso 1 1 calc R . . C41 C 0.8905(10) 0.2538(4) 0.3859(4) 0.045(2) Uani 1 1 d . . . H41A H 0.8238 0.2497 0.4148 0.054 Uiso 1 1 calc R . . C42 C 1.0140(11) 0.2776(4) 0.4055(4) 0.053(3) Uani 1 1 d . . . H42A H 1.0329 0.2896 0.4482 0.064 Uiso 1 1 calc R . . C43 C 1.1120(10) 0.2846(5) 0.3640(4) 0.052(2) Uani 1 1 d . . . H43A H 1.1976 0.3013 0.3782 0.063 Uiso 1 1 calc R . . C44 C 1.0855(9) 0.2675(4) 0.3022(4) 0.041(2) Uani 1 1 d . . . H44A H 1.1522 0.2738 0.2736 0.049 Uiso 1 1 calc R . . C45 C 0.9294(7) 0.2859(4) 0.1526(3) 0.0286(17) Uani 1 1 d . . . C46 C 0.8875(9) 0.3429(4) 0.1743(4) 0.041(2) Uani 1 1 d . . . H46A H 0.8633 0.3459 0.2162 0.049 Uiso 1 1 calc R . . C47 C 0.8795(9) 0.3965(4) 0.1362(4) 0.044(2) Uani 1 1 d . . . H47A H 0.8490 0.4357 0.1520 0.053 Uiso 1 1 calc R . . C48 C 0.9155(9) 0.3929(4) 0.0761(4) 0.043(2) Uani 1 1 d . . . H48A H 0.9127 0.4299 0.0505 0.052 Uiso 1 1 calc R . . C49 C 0.9559(10) 0.3356(4) 0.0523(4) 0.046(2) Uani 1 1 d . . . H49A H 0.9791 0.3326 0.0103 0.056 Uiso 1 1 calc R . . C50 C 0.9621(9) 0.2820(4) 0.0911(4) 0.040(2) Uani 1 1 d . . . H50A H 0.9892 0.2423 0.0750 0.048 Uiso 1 1 calc R . . O1D O 0.5427(6) 0.0574(3) 0.4423(3) 0.0497(16) Uani 1 1 d . . . C1D C 0.5667(9) 0.0107(5) 0.4894(4) 0.050(2) Uani 1 1 d . . . H1DA H 0.6233 0.0286 0.5255 0.060 Uiso 1 1 calc R . . H1DB H 0.6146 -0.0259 0.4727 0.060 Uiso 1 1 calc R . . C2D C 0.6603(10) 0.0741(5) 0.4157(5) 0.059(3) Uani 1 1 d . . . H2DA H 0.6399 0.1064 0.3832 0.088 Uiso 1 1 calc R . . H2DB H 0.6982 0.0364 0.3968 0.088 Uiso 1 1 calc R . . H2DC H 0.7254 0.0912 0.4482 0.088 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 Ir1 0.02500(15) 0.02050(14) 0.02406(14) -0.00052(13) 0.00054(10) -0.00049(14) Cl1 0.0467(12) 0.0384(10) 0.0275(9) 0.0001(9) 0.0020(8) -0.0011(10) P1 0.0278(11) 0.0219(9) 0.0273(10) 0.0005(8) 0.0003(8) -0.0011(8) P2 0.0269(11) 0.0238(10) 0.0272(10) 0.0013(8) 0.0006(8) -0.0002(8) P3 0.0264(11) 0.0245(10) 0.0256(10) -0.0001(8) 0.0009(8) 0.0002(8) P4 0.0295(11) 0.0225(9) 0.0284(10) 0.0001(8) 0.0010(8) -0.0001(8) C1 0.029(5) 0.031(4) 0.040(5) 0.008(3) -0.003(3) -0.005(3) C2 0.045(5) 0.021(4) 0.029(4) 0.004(3) -0.003(4) -0.002(3) C3 0.039(5) 0.041(5) 0.038(5) -0.006(4) 0.006(4) 0.008(4) C4 0.077(7) 0.032(4) 0.029(4) -0.006(4) 0.010(4) -0.001(4) C5 0.082(8) 0.028(4) 0.034(5) -0.001(4) -0.005(5) -0.004(5) C6 0.062(7) 0.039(5) 0.049(6) 0.005(4) -0.014(5) -0.015(5) C7 0.052(6) 0.037(5) 0.036(5) -0.004(4) -0.011(4) -0.012(4) C8 0.041(5) 0.020(4) 0.021(4) -0.002(3) -0.004(3) -0.007(3) C9 0.037(5) 0.041(5) 0.045(5) 0.002(4) 0.000(4) -0.002(4) C10 0.058(6) 0.039(5) 0.045(6) 0.012(4) -0.015(5) -0.003(5) C11 0.083(8) 0.031(5) 0.040(5) 0.011(4) 0.002(5) -0.007(5) C12 0.098(9) 0.042(5) 0.042(6) 0.003(4) 0.036(6) -0.008(6) C13 0.049(6) 0.026(4) 0.049(5) 0.002(4) 0.016(4) 0.006(4) C14 0.036(5) 0.025(4) 0.027(4) -0.012(3) -0.002(3) 0.004(3) C15 0.029(5) 0.059(6) 0.044(5) 0.009(4) -0.004(4) 0.003(4) C16 0.042(6) 0.049(5) 0.044(5) 0.002(4) -0.009(4) 0.015(4) C17 0.064(7) 0.047(5) 0.031(5) 0.003(4) 0.002(4) 0.018(5) C18 0.076(8) 0.059(6) 0.043(6) 0.024(5) 0.020(5) 0.008(5) C19 0.030(5) 0.058(6) 0.054(6) 0.024(5) 0.001(4) 0.002(4) C20 0.027(4) 0.023(4) 0.027(4) -0.001(3) -0.003(3) 0.002(3) C21 0.048(5) 0.037(5) 0.034(5) -0.002(4) 0.012(4) -0.004(4) C22 0.071(7) 0.066(7) 0.029(5) 0.001(5) 0.016(5) -0.005(5) C23 0.056(6) 0.062(6) 0.047(6) -0.023(5) 0.002(5) 0.013(5) C24 0.058(6) 0.036(5) 0.044(5) -0.012(4) -0.002(4) 0.010(4) C25 0.048(6) 0.034(4) 0.043(5) 0.000(4) 0.015(4) 0.003(4) C26 0.035(5) 0.022(4) 0.034(4) 0.004(3) 0.004(3) 0.000(3) C27 0.025(4) 0.028(4) 0.030(4) -0.005(3) -0.002(3) -0.001(3) C28 0.040(5) 0.038(5) 0.031(4) 0.005(4) 0.003(4) 0.012(4) C29 0.045(5) 0.042(5) 0.032(4) -0.007(4) 0.007(4) 0.000(4) C30 0.052(6) 0.037(5) 0.039(5) -0.003(4) 0.008(4) 0.007(4) C31 0.080(7) 0.027(4) 0.041(5) 0.009(4) 0.014(5) 0.008(4) C32 0.050(5) 0.031(4) 0.030(4) -0.003(4) 0.008(4) 0.006(4) C33 0.029(4) 0.021(4) 0.033(4) 0.001(3) 0.000(3) 0.002(3) C34 0.036(5) 0.032(4) 0.033(4) -0.008(3) -0.004(4) 0.000(4) C35 0.038(5) 0.049(5) 0.027(4) 0.003(4) 0.003(3) 0.002(4) C36 0.049(6) 0.037(5) 0.028(4) -0.005(4) -0.012(4) 0.008(4) C37 0.040(5) 0.030(4) 0.044(5) 0.003(4) -0.004(4) 0.001(4) C38 0.030(5) 0.042(5) 0.034(5) 0.008(4) 0.003(3) 0.006(4) C39 0.032(5) 0.025(4) 0.031(4) 0.006(3) 0.002(3) 0.002(3) C40 0.047(5) 0.025(4) 0.033(4) 0.004(3) -0.002(4) -0.006(4) C41 0.063(7) 0.036(5) 0.037(5) 0.000(4) 0.006(4) 0.000(4) C42 0.074(8) 0.051(6) 0.031(5) -0.015(4) -0.013(5) 0.009(5) C43 0.040(6) 0.065(6) 0.048(6) -0.019(5) -0.013(4) 0.001(5) C44 0.037(5) 0.035(4) 0.050(5) -0.015(4) 0.001(4) -0.005(4) C45 0.026(4) 0.029(4) 0.030(4) 0.000(3) -0.003(3) -0.002(3) C46 0.057(6) 0.029(4) 0.038(5) -0.005(4) 0.003(4) 0.010(4) C47 0.052(6) 0.027(4) 0.052(6) -0.003(4) -0.007(4) 0.005(4) C48 0.056(6) 0.030(4) 0.040(5) 0.008(4) -0.010(4) -0.009(4) C49 0.056(6) 0.046(5) 0.038(5) 0.010(4) 0.007(4) -0.001(4) C50 0.048(6) 0.035(5) 0.040(5) 0.010(4) 0.015(4) 0.005(4) O1D 0.036(4) 0.065(4) 0.047(4) 0.004(3) -0.004(3) 0.008(3) C1D 0.034(5) 0.071(6) 0.043(5) 0.002(5) -0.012(4) 0.013(5) C2D 0.056(7) 0.063(7) 0.057(6) -0.004(5) -0.002(5) -0.003(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 P4 2.3273(19) . ? Ir1 P2 2.330(2) . ? Ir1 P3 2.3300(19) . ? Ir1 P1 2.3333(19) . ? Ir1 Cl1 2.5129(18) . ? P1 C1 1.724(8) . ? P1 C2 1.829(8) . ? P1 C8 1.845(7) . ? P1 P2 2.639(3) . ? P2 C1 1.720(8) . ? P2 C14 1.827(8) . ? P2 C20 1.832(7) . ? P3 C33 1.805(8) . ? P3 C27 1.817(7) . ? P3 C26 1.852(7) . ? P3 P4 2.694(3) . ? P4 C39 1.815(8) . ? P4 C45 1.829(8) . ? P4 C26 1.855(8) . ? C2 C7 1.369(11) . ? C2 C3 1.390(11) . ? C3 C4 1.378(11) . ? C4 C5 1.352(13) . ? C5 C6 1.358(14) . ? C6 C7 1.406(12) . ? C8 C13 1.379(11) . ? C8 C9 1.378(11) . ? C9 C10 1.380(11) . ? C10 C11 1.368(14) . ? C11 C12 1.374(14) . ? C12 C13 1.393(12) . ? C14 C15 1.378(11) . ? C14 C19 1.390(11) . ? C15 C16 1.382(12) . ? C16 C17 1.371(13) . ? C17 C18 1.350(14) . ? C18 C19 1.388(12) . ? C20 C21 1.374(10) . ? C20 C25 1.399(11) . ? C21 C22 1.396(12) . ? C22 C23 1.359(14) . ? C23 C24 1.373(13) . ? C24 C25 1.377(11) . ? C27 C32 1.373(10) . ? C27 C28 1.403(10) . ? C28 C29 1.386(11) . ? C29 C30 1.376(12) . ? C30 C31 1.378(11) . ? C31 C32 1.393(11) . ? C33 C34 1.382(11) . ? C33 C38 1.405(11) . ? C34 C35 1.385(10) . ? C35 C36 1.398(12) . ? C36 C37 1.371(12) . ? C37 C38 1.387(11) . ? C39 C44 1.395(11) . ? C39 C40 1.416(11) . ? C40 C41 1.385(11) . ? C41 C42 1.364(14) . ? C42 C43 1.384(14) . ? C43 C44 1.373(11) . ? C45 C46 1.363(11) . ? C45 C50 1.386(10) . ? C46 C47 1.389(11) . ? C47 C48 1.366(12) . ? C48 C49 1.381(12) . ? C49 C50 1.397(11) . ? O1D C2D 1.392(11) . ? O1D C1D 1.414(11) . ? C1D C1D 1.510(18) 3_656 ? 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 P4 Ir1 P2 108.78(7) . . ? P4 Ir1 P3 70.69(6) . . ? P2 Ir1 P3 174.21(7) . . ? P4 Ir1 P1 174.71(7) . . ? P2 Ir1 P1 68.92(6) . . ? P3 Ir1 P1 111.08(7) . . ? P4 Ir1 Cl1 89.65(7) . . ? P2 Ir1 Cl1 96.56(7) . . ? P3 Ir1 Cl1 89.21(7) . . ? P1 Ir1 Cl1 95.32(7) . . ? C1 P1 C2 113.8(4) . . ? C1 P1 C8 112.1(4) . . ? C2 P1 C8 99.0(3) . . ? C1 P1 Ir1 95.4(3) . . ? C2 P1 Ir1 121.1(3) . . ? C8 P1 Ir1 116.2(2) . . ? C1 P1 P2 39.9(3) . . ? C2 P1 P2 130.7(2) . . ? C8 P1 P2 127.8(2) . . ? Ir1 P1 P2 55.48(6) . . ? C1 P2 C14 114.2(4) . . ? C1 P2 C20 113.0(4) . . ? C14 P2 C20 99.9(3) . . ? C1 P2 Ir1 95.6(3) . . ? C14 P2 Ir1 122.0(3) . . ? C20 P2 Ir1 112.9(2) . . ? C1 P2 P1 40.1(3) . . ? C14 P2 P1 131.8(2) . . ? C20 P2 P1 126.3(2) . . ? Ir1 P2 P1 55.60(6) . . ? C33 P3 C27 104.5(3) . . ? C33 P3 C26 103.8(3) . . ? C27 P3 C26 108.7(3) . . ? C33 P3 Ir1 117.6(3) . . ? C27 P3 Ir1 125.8(2) . . ? C26 P3 Ir1 93.5(2) . . ? C33 P3 P4 103.3(2) . . ? C27 P3 P4 145.0(3) . . ? C26 P3 P4 43.4(2) . . ? Ir1 P3 P4 54.61(6) . . ? C39 P4 C45 105.1(3) . . ? C39 P4 C26 105.0(4) . . ? C45 P4 C26 107.9(3) . . ? C39 P4 Ir1 117.3(3) . . ? C45 P4 Ir1 125.2(2) . . ? C26 P4 Ir1 93.5(2) . . ? C39 P4 P3 104.1(2) . . ? C45 P4 P3 143.9(3) . . ? C26 P4 P3 43.3(2) . . ? Ir1 P4 P3 54.70(6) . . ? P1 C1 P2 100.0(4) . . ? C7 C2 C3 119.9(8) . . ? C7 C2 P1 118.9(7) . . ? C3 C2 P1 121.2(6) . . ? C4 C3 C2 119.5(8) . . ? C5 C4 C3 121.1(9) . . ? C4 C5 C6 119.8(9) . . ? C5 C6 C7 120.9(9) . . ? C2 C7 C6 118.8(9) . . ? C13 C8 C9 118.3(7) . . ? C13 C8 P1 120.2(6) . . ? C9 C8 P1 121.4(6) . . ? C8 C9 C10 121.2(8) . . ? C11 C10 C9 120.4(9) . . ? C10 C11 C12 119.3(8) . . ? C11 C12 C13 120.5(9) . . ? C8 C13 C12 120.3(8) . . ? C15 C14 C19 118.4(7) . . ? C15 C14 P2 119.1(6) . . ? C19 C14 P2 122.5(6) . . ? C16 C15 C14 121.3(8) . . ? C15 C16 C17 119.7(9) . . ? C18 C17 C16 119.6(8) . . ? C17 C18 C19 121.7(9) . . ? C14 C19 C18 119.2(9) . . ? C21 C20 C25 118.3(7) . . ? C21 C20 P2 119.3(6) . . ? C25 C20 P2 121.9(6) . . ? C20 C21 C22 119.9(8) . . ? C23 C22 C21 121.5(9) . . ? C22 C23 C24 118.9(9) . . ? C23 C24 C25 120.7(9) . . ? C24 C25 C20 120.6(8) . . ? P4 C26 P3 93.3(4) . . ? C32 C27 C28 118.6(7) . . ? C32 C27 P3 120.9(6) . . ? C28 C27 P3 120.3(6) . . ? C29 C28 C27 120.5(7) . . ? C30 C29 C28 120.1(8) . . ? C29 C30 C31 119.8(8) . . ? C30 C31 C32 120.3(8) . . ? C27 C32 C31 120.7(7) . . ? C34 C33 C38 117.0(7) . . ? C34 C33 P3 123.0(6) . . ? C38 C33 P3 119.9(6) . . ? C33 C34 C35 121.3(8) . . ? C34 C35 C36 120.1(8) . . ? C37 C36 C35 120.0(7) . . ? C36 C37 C38 118.9(8) . . ? C37 C38 C33 122.6(8) . . ? C44 C39 C40 118.2(7) . . ? C44 C39 P4 121.6(6) . . ? C40 C39 P4 120.1(6) . . ? C41 C40 C39 120.0(8) . . ? C42 C41 C40 120.1(9) . . ? C41 C42 C43 120.8(8) . . ? C44 C43 C42 120.0(9) . . ? C43 C44 C39 120.7(8) . . ? C46 C45 C50 118.6(7) . . ? C46 C45 P4 121.3(6) . . ? C50 C45 P4 119.8(6) . . ? C45 C46 C47 121.3(8) . . ? C48 C47 C46 119.9(8) . . ? C47 C48 C49 120.2(8) . . ? C48 C49 C50 119.1(8) . . ? C45 C50 C49 120.8(8) . . ? C2D O1D C1D 111.7(7) . . ? O1D C1D C1D 108.7(9) . 3_656 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.975 _refine_diff_density_min -1.039 _refine_diff_density_rms 0.173 #=== END data_FO3498 _database_code_depnum_ccdc_archive 'CCDC 770463' #TrackingRef '- dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H41 Li O4 P2' _chemical_formula_weight 570.54 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.2326(6) _cell_length_b 9.2525(2) _cell_length_c 21.7101(7) _cell_angle_alpha 90.00 _cell_angle_beta 106.354(2) _cell_angle_gamma 90.00 _cell_volume 3128.76(17) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.211 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 0.174 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10804 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3572 _reflns_number_gt 2844 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+0.3462P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3572 _refine_ls_number_parameters 264 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.1037 _refine_ls_wR_factor_gt 0.0942 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 Li Li 0.5000 0.4427(4) 0.7500 0.0302(7) Uani 1 2 d S . . P1 P 0.46818(2) 0.17213(3) 0.680272(15) 0.01962(12) Uani 1 1 d . . . O1 O 0.62977(7) 0.47867(11) 0.75248(5) 0.0347(3) Uani 1 1 d . . . O2 O 0.48184(7) 0.58643(11) 0.67160(5) 0.0345(3) Uani 1 1 d . . . C1 C 0.5000 0.0709(2) 0.7500 0.0247(4) Uani 1 2 d S . . H1 H 0.5000 -0.033(3) 0.7500 0.046(7) Uiso 1 2 d S . . C2 C 0.36495(9) 0.09477(14) 0.63151(6) 0.0219(3) Uani 1 1 d . . . C3 C 0.30026(10) 0.18306(17) 0.59510(7) 0.0308(3) Uani 1 1 d . . . H3 H 0.3114(12) 0.280(2) 0.5934(8) 0.042(5) Uiso 1 1 d . . . C4 C 0.22117(11) 0.12723(19) 0.56033(8) 0.0381(4) Uani 1 1 d . . . H4 H 0.1800(14) 0.190(2) 0.5369(10) 0.057(6) Uiso 1 1 d . . . C5 C 0.20564(10) -0.01859(18) 0.56135(7) 0.0332(4) Uani 1 1 d . . . H5 H 0.1535(12) -0.0605(19) 0.5377(8) 0.041(5) Uiso 1 1 d . . . C6 C 0.26898(11) -0.10854(17) 0.59705(8) 0.0376(4) Uani 1 1 d . . . H6 H 0.2590(13) -0.206(2) 0.5982(9) 0.051(5) Uiso 1 1 d . . . C7 C 0.34745(11) -0.05312(17) 0.63169(8) 0.0338(4) Uani 1 1 d . . . H7 H 0.3912(12) -0.1140(19) 0.6572(8) 0.038(5) Uiso 1 1 d . . . C8 C 0.53426(9) 0.11567(14) 0.62753(6) 0.0231(3) Uani 1 1 d . . . C9 C 0.60639(10) 0.03050(17) 0.65088(8) 0.0328(3) Uani 1 1 d . . . H9 H 0.6208(12) -0.0051(19) 0.6946(9) 0.043(5) Uiso 1 1 d . . . C10 C 0.65988(12) -0.0047(2) 0.61277(9) 0.0442(4) Uani 1 1 d . . . H10 H 0.7112(14) -0.060(2) 0.6327(10) 0.057(6) Uiso 1 1 d . . . C11 C 0.64179(12) 0.0450(2) 0.55086(9) 0.0451(5) Uani 1 1 d . . . H11 H 0.6764(14) 0.022(2) 0.5248(10) 0.058(6) Uiso 1 1 d . . . C12 C 0.57051(13) 0.1307(2) 0.52668(8) 0.0428(4) Uani 1 1 d . . . H12 H 0.5544(13) 0.164(2) 0.4847(10) 0.052(6) Uiso 1 1 d . . . C13 C 0.51690(11) 0.16646(17) 0.56438(7) 0.0321(3) Uani 1 1 d . . . H13 H 0.4680(12) 0.2245(18) 0.5467(8) 0.031(4) Uiso 1 1 d . . . C14 C 0.62998(13) 0.6104(2) 0.71800(10) 0.0484(5) Uani 1 1 d . . . H14B H 0.6858(14) 0.623(2) 0.7092(9) 0.053(6) Uiso 1 1 d . . . H14A H 0.6181(13) 0.686(2) 0.7457(9) 0.054(6) Uiso 1 1 d . . . C15 C 0.56058(13) 0.6106(2) 0.65627(10) 0.0476(5) Uani 1 1 d . . . H15B H 0.5649(13) 0.528(2) 0.6254(9) 0.055(6) Uiso 1 1 d . . . H15A H 0.5578(14) 0.699(2) 0.6345(10) 0.064(6) Uiso 1 1 d . . . C16 C 0.41193(13) 0.5684(2) 0.61531(9) 0.0424(4) Uani 1 1 d . . . H16C H 0.4058(13) 0.658(2) 0.5902(9) 0.048(5) Uiso 1 1 d . . . H16B H 0.3605(13) 0.550(2) 0.6290(9) 0.047(5) Uiso 1 1 d . . . H16A H 0.4224(14) 0.484(2) 0.5906(9) 0.055(6) Uiso 1 1 d . . . C17 C 0.67724(12) 0.3649(2) 0.73358(10) 0.0411(4) Uani 1 1 d . . . H17B H 0.6743(13) 0.277(2) 0.7593(9) 0.049(5) Uiso 1 1 d . . . H17A H 0.6543(12) 0.3467(18) 0.6890(9) 0.035(4) Uiso 1 1 d . . . H17C H 0.7357(15) 0.395(2) 0.7407(10) 0.058(6) 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 Li 0.0284(19) 0.0293(17) 0.0368(18) 0.000 0.0154(15) 0.000 P1 0.0202(2) 0.02053(19) 0.01845(18) -0.00045(12) 0.00595(13) 0.00083(13) O1 0.0313(6) 0.0360(6) 0.0405(6) -0.0032(5) 0.0161(5) -0.0042(5) O2 0.0359(6) 0.0323(6) 0.0364(6) 0.0034(4) 0.0123(5) -0.0049(5) C1 0.0320(11) 0.0210(9) 0.0201(9) 0.000 0.0058(8) 0.000 C2 0.0216(7) 0.0264(7) 0.0193(6) -0.0013(5) 0.0084(5) 0.0005(5) C3 0.0256(8) 0.0284(8) 0.0359(8) 0.0033(6) 0.0047(6) 0.0020(6) C4 0.0247(8) 0.0459(9) 0.0392(9) 0.0055(7) 0.0016(7) 0.0057(7) C5 0.0227(8) 0.0487(9) 0.0284(8) -0.0077(7) 0.0076(6) -0.0102(7) C6 0.0381(10) 0.0320(9) 0.0405(9) -0.0040(7) 0.0078(7) -0.0098(7) C7 0.0300(9) 0.0294(8) 0.0371(8) 0.0007(6) 0.0011(7) -0.0014(6) C8 0.0237(7) 0.0242(7) 0.0229(7) -0.0061(5) 0.0089(6) -0.0067(5) C9 0.0296(8) 0.0364(8) 0.0347(8) -0.0037(6) 0.0128(7) 0.0030(6) C10 0.0334(10) 0.0494(10) 0.0554(11) -0.0134(9) 0.0216(8) 0.0019(8) C11 0.0429(11) 0.0531(11) 0.0515(11) -0.0229(9) 0.0334(9) -0.0169(9) C12 0.0561(12) 0.0501(10) 0.0295(8) -0.0086(7) 0.0237(8) -0.0194(9) C13 0.0362(9) 0.0357(8) 0.0259(7) -0.0006(6) 0.0114(7) -0.0058(7) C14 0.0413(11) 0.0422(10) 0.0655(13) 0.0013(9) 0.0213(10) -0.0165(8) C15 0.0463(11) 0.0478(11) 0.0538(11) 0.0153(9) 0.0224(9) -0.0096(8) C16 0.0467(11) 0.0375(9) 0.0383(9) 0.0079(8) 0.0044(8) -0.0007(8) C17 0.0293(10) 0.0501(10) 0.0480(11) -0.0084(8) 0.0176(8) -0.0028(8) _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 Li O2 2.114(2) 2_656 ? Li O2 2.114(2) . ? Li O1 2.1184(12) . ? Li O1 2.1185(12) 2_656 ? Li P1 2.895(3) 2_656 ? Li P1 2.896(3) . ? P1 C1 1.7308(11) . ? P1 C8 1.8509(14) . ? P1 C2 1.8553(14) . ? O1 C14 1.431(2) . ? O1 C17 1.431(2) . ? O2 C16 1.424(2) . ? O2 C15 1.426(2) . ? C1 P1 1.7307(11) 2_656 ? C1 H1 0.96(3) . ? C2 C3 1.388(2) . ? C2 C7 1.398(2) . ? C3 C4 1.393(2) . ? C3 H3 0.92(2) . ? C4 C5 1.374(2) . ? C4 H4 0.92(2) . ? C5 C6 1.379(2) . ? C5 H5 0.942(19) . ? C6 C7 1.383(2) . ? C6 H6 0.91(2) . ? C7 H7 0.952(18) . ? C8 C9 1.384(2) . ? C8 C13 1.401(2) . ? C9 C10 1.396(2) . ? C9 H9 0.968(18) . ? C10 C11 1.372(3) . ? C10 H10 0.97(2) . ? C11 C12 1.379(3) . ? C11 H11 0.93(2) . ? C12 C13 1.392(2) . ? C12 H12 0.93(2) . ? C13 H13 0.946(18) . ? C14 C15 1.488(3) . ? C14 H14B 0.98(2) . ? C14 H14A 0.98(2) . ? C15 H15B 1.03(2) . ? C15 H15A 0.94(2) . ? C16 H16C 0.98(2) . ? C16 H16B 0.98(2) . ? C16 H16A 0.99(2) . ? C17 H17B 1.00(2) . ? C17 H17A 0.949(18) . ? C17 H17C 0.96(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Li O2 102.03(15) 2_656 . ? O2 Li O1 88.19(8) 2_656 . ? O2 Li O1 80.43(7) . . ? O2 Li O1 80.43(7) 2_656 2_656 ? O2 Li O1 88.19(8) . 2_656 ? O1 Li O1 161.91(19) . 2_656 ? O2 Li P1 99.15(5) 2_656 2_656 ? O2 Li P1 158.22(11) . 2_656 ? O1 Li P1 95.33(8) . 2_656 ? O1 Li P1 100.31(8) 2_656 2_656 ? O2 Li P1 158.22(11) 2_656 . ? O2 Li P1 99.15(5) . . ? O1 Li P1 100.31(8) . . ? O1 Li P1 95.33(8) 2_656 . ? P1 Li P1 60.35(7) 2_656 . ? C1 P1 C8 107.82(6) . . ? C1 P1 C2 106.82(6) . . ? C8 P1 C2 97.22(6) . . ? C1 P1 Li 92.59(7) . . ? C8 P1 Li 121.22(4) . . ? C2 P1 Li 129.15(4) . . ? C14 O1 C17 113.31(14) . . ? C14 O1 Li 105.63(13) . . ? C17 O1 Li 119.27(13) . . ? C16 O2 C15 111.59(14) . . ? C16 O2 Li 120.93(11) . . ? C15 O2 Li 110.82(10) . . ? P1 C1 P1 114.46(11) 2_656 . ? P1 C1 H1 122.77(6) 2_656 . ? P1 C1 H1 122.77(5) . . ? C3 C2 C7 117.12(13) . . ? C3 C2 P1 120.98(11) . . ? C7 C2 P1 121.85(11) . . ? C2 C3 C4 121.63(14) . . ? C2 C3 H3 118.2(12) . . ? C4 C3 H3 120.2(11) . . ? C5 C4 C3 120.06(15) . . ? C5 C4 H4 121.4(13) . . ? C3 C4 H4 118.6(13) . . ? C4 C5 C6 119.38(15) . . ? C4 C5 H5 122.4(11) . . ? C6 C5 H5 118.2(11) . . ? C5 C6 C7 120.58(15) . . ? C5 C6 H6 119.9(13) . . ? C7 C6 H6 119.5(13) . . ? C6 C7 C2 121.22(15) . . ? C6 C7 H7 121.3(11) . . ? C2 C7 H7 117.5(11) . . ? C9 C8 C13 117.76(13) . . ? C9 C8 P1 120.81(11) . . ? C13 C8 P1 121.26(12) . . ? C8 C9 C10 121.27(16) . . ? C8 C9 H9 119.9(11) . . ? C10 C9 H9 118.8(11) . . ? C11 C10 C9 120.35(18) . . ? C11 C10 H10 122.3(12) . . ? C9 C10 H10 117.2(12) . . ? C10 C11 C12 119.40(15) . . ? C10 C11 H11 121.3(13) . . ? C12 C11 H11 119.3(13) . . ? C11 C12 C13 120.62(16) . . ? C11 C12 H12 122.8(13) . . ? C13 C12 H12 116.5(13) . . ? C12 C13 C8 120.59(16) . . ? C12 C13 H13 119.2(10) . . ? C8 C13 H13 120.2(10) . . ? O1 C14 C15 111.05(14) . . ? O1 C14 H14B 109.9(11) . . ? C15 C14 H14B 109.2(12) . . ? O1 C14 H14A 104.9(11) . . ? C15 C14 H14A 108.9(12) . . ? H14B C14 H14A 112.8(17) . . ? O2 C15 C14 106.89(15) . . ? O2 C15 H15B 105.4(12) . . ? C14 C15 H15B 114.3(11) . . ? O2 C15 H15A 109.6(14) . . ? C14 C15 H15A 111.7(14) . . ? H15B C15 H15A 108.7(17) . . ? O2 C16 H16C 107.9(11) . . ? O2 C16 H16B 107.6(11) . . ? H16C C16 H16B 111.0(16) . . ? O2 C16 H16A 109.9(12) . . ? H16C C16 H16A 112.0(15) . . ? H16B C16 H16A 108.4(16) . . ? O1 C17 H17B 109.1(11) . . ? O1 C17 H17A 109.6(11) . . ? H17B C17 H17A 110.9(15) . . ? O1 C17 H17C 109.2(12) . . ? H17B C17 H17C 110.5(16) . . ? H17A C17 H17C 107.5(17) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.263 _refine_diff_density_min -0.239 _refine_diff_density_rms 0.041 #=== END data_FO3600 _database_code_depnum_ccdc_archive 'CCDC 770464' #TrackingRef '- dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C81 H90 Cl Ir O6 P6' _chemical_formula_weight 1573.00 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' O O 0.0106 0.0060 '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' Cl Cl 0.1484 0.1585 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.9095(3) _cell_length_b 13.8595(2) _cell_length_c 27.8469(5) _cell_angle_alpha 90.00 _cell_angle_beta 111.662(1) _cell_angle_gamma 90.00 _cell_volume 7500.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3232 _exptl_absorpt_coefficient_mu 1.996 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49853 _diffrn_reflns_av_R_equivalents 0.0942 _diffrn_reflns_av_sigmaI/netI 0.0984 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 27.48 _reflns_number_total 17055 _reflns_number_gt 11474 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0568P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17055 _refine_ls_number_parameters 855 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0983 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1232 _refine_ls_wR_factor_gt 0.1062 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.056 _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 Ir1 Ir 0.301615(9) -0.009352(12) 0.831769(7) 0.02080(7) Uani 1 1 d . . . P1 P 0.27404(6) -0.16879(9) 0.79774(5) 0.0237(3) Uani 1 1 d . . . P2 P 0.33349(6) -0.02522(9) 0.76088(5) 0.0238(3) Uani 1 1 d . . . P3 P 0.40875(6) 0.03392(9) 0.88906(5) 0.0232(3) Uani 1 1 d . . . P4 P 0.29838(6) -0.00417(9) 0.91457(5) 0.0233(3) Uani 1 1 d . . . P5 P 0.19598(6) 0.07095(9) 0.79025(5) 0.0244(3) Uani 1 1 d . . . P6 P 0.06075(7) 0.08147(10) 0.68851(5) 0.0274(3) Uani 1 1 d . . . C1 C 0.2907(2) -0.1422(4) 0.73840(19) 0.0254(11) Uani 1 1 d . . . H1A H 0.3216 -0.1901 0.7318 0.030 Uiso 1 1 calc R . . H1B H 0.2478 -0.1357 0.7076 0.030 Uiso 1 1 calc R . . C2 C 0.3277(2) -0.2737(3) 0.8283(2) 0.0248(11) Uani 1 1 d . . . C3 C 0.3436(3) -0.3458(4) 0.7995(2) 0.0364(13) Uani 1 1 d . . . H3A H 0.3314 -0.3383 0.7633 0.044 Uiso 1 1 calc R . . C4 C 0.3775(3) -0.4285(4) 0.8241(3) 0.0485(17) Uani 1 1 d . . . H4A H 0.3891 -0.4772 0.8047 0.058 Uiso 1 1 calc R . . C5 C 0.3944(3) -0.4406(4) 0.8767(3) 0.0430(15) Uani 1 1 d . . . H5A H 0.4179 -0.4972 0.8932 0.052 Uiso 1 1 calc R . . C6 C 0.3776(3) -0.3715(4) 0.9050(2) 0.0396(14) Uani 1 1 d . . . H6A H 0.3882 -0.3807 0.9409 0.048 Uiso 1 1 calc R . . C7 C 0.3450(3) -0.2877(4) 0.8808(2) 0.0325(12) Uani 1 1 d . . . H7A H 0.3345 -0.2390 0.9007 0.039 Uiso 1 1 calc R . . C8 C 0.1920(2) -0.2349(3) 0.7754(2) 0.0253(11) Uani 1 1 d . . . C9 C 0.1694(3) -0.2720(4) 0.8126(2) 0.0322(12) Uani 1 1 d . . . H9A H 0.1959 -0.2614 0.8482 0.039 Uiso 1 1 calc R . . C10 C 0.1086(3) -0.3244(4) 0.7990(2) 0.0365(13) Uani 1 1 d . . . H10A H 0.0934 -0.3488 0.8248 0.044 Uiso 1 1 calc R . . C11 C 0.0705(3) -0.3405(4) 0.7473(2) 0.0414(14) Uani 1 1 d . . . H11A H 0.0288 -0.3760 0.7376 0.050 Uiso 1 1 calc R . . C12 C 0.0924(3) -0.3059(4) 0.7102(2) 0.0436(15) Uani 1 1 d . . . H12A H 0.0662 -0.3179 0.6748 0.052 Uiso 1 1 calc R . . C13 C 0.1533(3) -0.2527(4) 0.7241(2) 0.0339(13) Uani 1 1 d . . . H13A H 0.1681 -0.2286 0.6980 0.041 Uiso 1 1 calc R . . C14 C 0.4238(3) -0.0478(4) 0.7706(2) 0.0278(11) Uani 1 1 d . . . C15 C 0.4636(3) 0.0233(4) 0.7594(2) 0.0370(13) Uani 1 1 d . . . H15A H 0.4438 0.0843 0.7467 0.044 Uiso 1 1 calc R . . C16 C 0.5317(3) 0.0056(5) 0.7666(3) 0.0458(15) Uani 1 1 d . . . H16A H 0.5580 0.0544 0.7585 0.055 Uiso 1 1 calc R . . C17 C 0.5618(3) -0.0821(5) 0.7854(2) 0.0471(16) Uani 1 1 d . . . H17A H 0.6089 -0.0934 0.7912 0.056 Uiso 1 1 calc R . . C18 C 0.5226(3) -0.1531(5) 0.7958(2) 0.0450(15) Uani 1 1 d . . . H18A H 0.5424 -0.2145 0.8077 0.054 Uiso 1 1 calc R . . C19 C 0.4544(3) -0.1357(4) 0.7890(2) 0.0352(13) Uani 1 1 d . . . H19A H 0.4283 -0.1848 0.7971 0.042 Uiso 1 1 calc R . . C20 C 0.3090(3) 0.0548(4) 0.7045(2) 0.0291(12) Uani 1 1 d . . . C21 C 0.3049(3) 0.1539(4) 0.7109(2) 0.0313(12) Uani 1 1 d . . . H21A H 0.3107 0.1792 0.7439 0.038 Uiso 1 1 calc R . . C22 C 0.2925(3) 0.2160(4) 0.6694(3) 0.0425(15) Uani 1 1 d . . . H22A H 0.2901 0.2837 0.6740 0.051 Uiso 1 1 calc R . . C23 C 0.2838(3) 0.1789(5) 0.6220(3) 0.0551(18) Uani 1 1 d . . . H23A H 0.2757 0.2211 0.5935 0.066 Uiso 1 1 calc R . . C24 C 0.2867(4) 0.0810(5) 0.6151(2) 0.0548(18) Uani 1 1 d . . . H24A H 0.2800 0.0560 0.5818 0.066 Uiso 1 1 calc R . . C25 C 0.2993(3) 0.0191(4) 0.6563(2) 0.0414(14) Uani 1 1 d . . . H25A H 0.3013 -0.0485 0.6513 0.050 Uiso 1 1 calc R . . C26 C 0.3911(3) 0.0146(4) 0.9485(2) 0.0290(11) Uani 1 1 d . . . H26A H 0.4147 -0.0430 0.9681 0.035 Uiso 1 1 calc R . . H26B H 0.4016 0.0720 0.9713 0.035 Uiso 1 1 calc R . . C27 C 0.4887(2) -0.0366(4) 0.9028(2) 0.0264(11) Uani 1 1 d . . . C28 C 0.5505(3) 0.0025(4) 0.9043(2) 0.0323(12) Uani 1 1 d . . . H28A H 0.5524 0.0685 0.8956 0.039 Uiso 1 1 calc R . . C29 C 0.6093(3) -0.0532(5) 0.9182(2) 0.0441(15) Uani 1 1 d . . . H29A H 0.6512 -0.0256 0.9187 0.053 Uiso 1 1 calc R . . C30 C 0.6074(3) -0.1477(5) 0.9312(2) 0.0462(16) Uani 1 1 d . . . H30A H 0.6482 -0.1854 0.9418 0.055 Uiso 1 1 calc R . . C31 C 0.5457(3) -0.1889(4) 0.9289(2) 0.0411(14) Uani 1 1 d . . . H31A H 0.5438 -0.2551 0.9371 0.049 Uiso 1 1 calc R . . C32 C 0.4878(3) -0.1327(4) 0.9147(2) 0.0332(13) Uani 1 1 d . . . H32A H 0.4457 -0.1610 0.9131 0.040 Uiso 1 1 calc R . . C33 C 0.4429(3) 0.1566(4) 0.8926(2) 0.0287(12) Uani 1 1 d . . . C34 C 0.4795(3) 0.2027(4) 0.9390(2) 0.0397(14) Uani 1 1 d . . . H34A H 0.4841 0.1722 0.9707 0.048 Uiso 1 1 calc R . . C35 C 0.5091(3) 0.2916(4) 0.9399(3) 0.0500(17) Uani 1 1 d . . . H35A H 0.5332 0.3224 0.9720 0.060 Uiso 1 1 calc R . . C36 C 0.5041(3) 0.3363(4) 0.8942(3) 0.0479(16) Uani 1 1 d . . . H36A H 0.5254 0.3970 0.8948 0.058 Uiso 1 1 calc R . . C37 C 0.4678(3) 0.2918(4) 0.8482(3) 0.0431(15) Uani 1 1 d . . . H37A H 0.4635 0.3223 0.8166 0.052 Uiso 1 1 calc R . . C38 C 0.4378(3) 0.2033(4) 0.8474(2) 0.0338(13) Uani 1 1 d . . . H38A H 0.4129 0.1736 0.8152 0.041 Uiso 1 1 calc R . . C39 C 0.2717(3) -0.1055(4) 0.9434(2) 0.0304(12) Uani 1 1 d . . . C40 C 0.3143(4) -0.1551(4) 0.9867(2) 0.0476(16) Uani 1 1 d . . . H40A H 0.3616 -0.1384 1.0023 0.057 Uiso 1 1 calc R . . C41 C 0.2872(5) -0.2295(5) 1.0068(3) 0.075(3) Uani 1 1 d . . . H41A H 0.3167 -0.2643 1.0360 0.091 Uiso 1 1 calc R . . C42 C 0.2205(5) -0.2532(5) 0.9859(3) 0.072(3) Uani 1 1 d . . . H42A H 0.2031 -0.3036 1.0007 0.086 Uiso 1 1 calc R . . C43 C 0.1767(4) -0.2041(4) 0.9426(3) 0.0541(19) Uani 1 1 d . . . H43A H 0.1292 -0.2203 0.9279 0.065 Uiso 1 1 calc R . . C44 C 0.2029(3) -0.1326(4) 0.9218(2) 0.0403(14) Uani 1 1 d . . . H44A H 0.1734 -0.1003 0.8917 0.048 Uiso 1 1 calc R . . C45 C 0.2637(2) 0.0974(3) 0.93975(19) 0.0245(11) Uani 1 1 d . . . C46 C 0.2246(3) 0.0864(4) 0.9703(2) 0.0310(12) Uani 1 1 d . . . H46A H 0.2133 0.0236 0.9783 0.037 Uiso 1 1 calc R . . C47 C 0.2021(3) 0.1666(4) 0.9893(2) 0.0374(13) Uani 1 1 d . . . H47A H 0.1749 0.1587 1.0098 0.045 Uiso 1 1 calc R . . C48 C 0.2194(3) 0.2587(4) 0.9782(2) 0.0390(14) Uani 1 1 d . . . H48A H 0.2034 0.3137 0.9907 0.047 Uiso 1 1 calc R . . C49 C 0.2595(3) 0.2698(4) 0.9491(2) 0.0395(14) Uani 1 1 d . . . H49A H 0.2720 0.3327 0.9421 0.047 Uiso 1 1 calc R . . C50 C 0.2818(3) 0.1902(4) 0.9302(2) 0.0308(12) Uani 1 1 d . . . H50A H 0.3097 0.1986 0.9103 0.037 Uiso 1 1 calc R . . C51 C 0.1535(2) 0.0469(4) 0.7198(2) 0.0273(11) Uani 1 1 d . . . H51A H 0.1575 -0.0230 0.7140 0.033 Uiso 1 1 calc R . . H51B H 0.1796 0.0815 0.7018 0.033 Uiso 1 1 calc R . . C52 C 0.1271(2) 0.0363(4) 0.8127(2) 0.0258(11) Uani 1 1 d . . . C53 C 0.0917(3) -0.0512(4) 0.7943(2) 0.0318(12) Uani 1 1 d . . . H53A H 0.1014 -0.0876 0.7690 0.038 Uiso 1 1 calc R . . C54 C 0.0430(3) -0.0839(4) 0.8131(2) 0.0374(14) Uani 1 1 d . . . H54A H 0.0195 -0.1427 0.8004 0.045 Uiso 1 1 calc R . . C55 C 0.0282(3) -0.0322(4) 0.8501(2) 0.0404(14) Uani 1 1 d . . . H55A H -0.0046 -0.0559 0.8634 0.048 Uiso 1 1 calc R . . C56 C 0.0615(3) 0.0541(4) 0.8675(2) 0.0357(13) Uani 1 1 d . . . H56A H 0.0508 0.0906 0.8925 0.043 Uiso 1 1 calc R . . C57 C 0.1101(3) 0.0879(4) 0.8491(2) 0.0298(12) Uani 1 1 d . . . H57A H 0.1325 0.1475 0.8616 0.036 Uiso 1 1 calc R . . C58 C 0.1957(3) 0.2042(3) 0.79262(19) 0.0252(11) Uani 1 1 d . . . C59 C 0.2584(3) 0.2510(4) 0.8108(2) 0.0312(12) Uani 1 1 d . . . H59A H 0.2996 0.2142 0.8231 0.037 Uiso 1 1 calc R . . C60 C 0.2621(3) 0.3515(4) 0.8114(2) 0.0406(14) Uani 1 1 d . . . H60A H 0.3055 0.3828 0.8248 0.049 Uiso 1 1 calc R . . C61 C 0.2026(3) 0.4051(4) 0.7926(2) 0.0425(15) Uani 1 1 d . . . H61A H 0.2050 0.4735 0.7922 0.051 Uiso 1 1 calc R . . C62 C 0.1401(3) 0.3601(4) 0.7746(2) 0.0383(14) Uani 1 1 d . . . H62A H 0.0993 0.3977 0.7620 0.046 Uiso 1 1 calc R . . C63 C 0.1354(3) 0.2595(4) 0.7745(2) 0.0323(12) Uani 1 1 d . . . H63A H 0.0916 0.2289 0.7622 0.039 Uiso 1 1 calc R . . C64 C 0.0245(3) -0.0300(4) 0.6534(2) 0.0284(11) Uani 1 1 d . . . C65 C -0.0381(3) -0.0615(4) 0.6535(2) 0.0359(13) Uani 1 1 d . . . H65A H -0.0589 -0.0275 0.6736 0.043 Uiso 1 1 calc R . . C66 C -0.0714(3) -0.1411(4) 0.6253(2) 0.0413(14) Uani 1 1 d . . . H66A H -0.1143 -0.1620 0.6261 0.050 Uiso 1 1 calc R . . C67 C -0.0408(3) -0.1893(4) 0.5960(2) 0.0436(15) Uani 1 1 d . . . H67A H -0.0637 -0.2429 0.5756 0.052 Uiso 1 1 calc R . . C68 C 0.0223(3) -0.1609(4) 0.5959(2) 0.0426(15) Uani 1 1 d . . . H68A H 0.0434 -0.1960 0.5764 0.051 Uiso 1 1 calc R . . C69 C 0.0551(3) -0.0804(4) 0.6246(2) 0.0339(13) Uani 1 1 d . . . H69A H 0.0984 -0.0601 0.6244 0.041 Uiso 1 1 calc R . . C70 C 0.0592(3) 0.1575(4) 0.6335(2) 0.0287(12) Uani 1 1 d . . . C71 C 0.0025(3) 0.1543(4) 0.5878(2) 0.0342(13) Uani 1 1 d . . . H71A H -0.0329 0.1085 0.5840 0.041 Uiso 1 1 calc R . . C72 C -0.0034(3) 0.2162(4) 0.5480(2) 0.0399(14) Uani 1 1 d . . . H72A H -0.0428 0.2126 0.5170 0.048 Uiso 1 1 calc R . . C73 C 0.0468(3) 0.2834(4) 0.5523(3) 0.0478(16) Uani 1 1 d . . . H73A H 0.0425 0.3256 0.5244 0.057 Uiso 1 1 calc R . . C74 C 0.1037(3) 0.2887(4) 0.5979(3) 0.0481(16) Uani 1 1 d . . . H74A H 0.1388 0.3349 0.6015 0.058 Uiso 1 1 calc R . . C75 C 0.1096(3) 0.2270(4) 0.6381(3) 0.0442(15) Uani 1 1 d . . . H75A H 0.1484 0.2318 0.6694 0.053 Uiso 1 1 calc R . . Cl1 Cl 0.19509(8) -0.20165(11) 0.60333(6) 0.0458(4) Uani 1 1 d . . . O1M O 0.3200(3) -0.3273(4) 0.6647(2) 0.0759(16) Uani 1 1 d . . . H1M H 0.2831 -0.3035 0.6442 0.114 Uiso 1 1 calc R . . C1M C 0.3754(4) -0.2841(6) 0.6567(3) 0.072(2) Uani 1 1 d . . . H1M1 H 0.3734 -0.2140 0.6607 0.108 Uiso 1 1 calc R . . H1M2 H 0.3733 -0.2989 0.6217 0.108 Uiso 1 1 calc R . . H1M3 H 0.4186 -0.3089 0.6820 0.108 Uiso 1 1 calc R . . O2M O 0.3795(3) -0.0319(3) 0.5199(2) 0.0674(14) Uani 1 1 d . . . H2M H 0.3369 -0.0292 0.5028 0.101 Uiso 1 1 calc R . . C2M C 0.4072(4) 0.0583(6) 0.5240(5) 0.106(4) Uani 1 1 d . . . H2M1 H 0.3744 0.1058 0.5274 0.159 Uiso 1 1 calc R . . H2M2 H 0.4171 0.0725 0.4930 0.159 Uiso 1 1 calc R . . H2M3 H 0.4499 0.0613 0.5545 0.159 Uiso 1 1 calc R . . O3M O 0.2419(2) -0.0024(3) 0.47167(17) 0.0465(10) Uani 1 1 d . . . H3M H 0.2133 -0.0157 0.4854 0.070 Uiso 1 1 calc R . . C3M C 0.2165(3) -0.0335(5) 0.4203(3) 0.0510(16) Uani 1 1 d . . . H3M1 H 0.2407 0.0003 0.4012 0.076 Uiso 1 1 calc R . . H3M2 H 0.1672 -0.0195 0.4047 0.076 Uiso 1 1 calc R . . H3M3 H 0.2239 -0.1031 0.4192 0.076 Uiso 1 1 calc R . . O5M O 0.0834(4) -0.3725(6) 0.5637(3) 0.082(3) Uiso 0.775(11) 1 d P A 1 H5M H 0.0966 -0.3164 0.5608 0.123 Uiso 0.775(11) 1 calc PR A 1 O5MA O 0.1849(12) -0.4205(16) 0.5578(9) 0.069(8) Uiso 0.225(11) 1 d P A 2 H5MA H 0.1933 -0.3619 0.5552 0.103 Uiso 0.225(11) 1 calc PR A 2 C5M C 0.1074(5) -0.4369(6) 0.5350(4) 0.090(3) Uani 1 1 d . . . H5M1 H 0.1271 -0.4003 0.5137 0.135 Uiso 0.775(11) 1 calc PR A 1 H5M2 H 0.0691 -0.4764 0.5127 0.135 Uiso 0.775(11) 1 calc PR A 1 H5M3 H 0.1428 -0.4789 0.5587 0.135 Uiso 0.775(11) 1 calc PR A 1 H5M4 H 0.0862 -0.3908 0.5070 0.135 Uiso 0.225(11) 1 calc PR A 2 H5M5 H 0.0883 -0.4278 0.5620 0.135 Uiso 0.225(11) 1 calc PR A 2 H5M6 H 0.0979 -0.5028 0.5214 0.135 Uiso 0.225(11) 1 calc PR A 2 O6M O 0.1510(2) -0.0462(3) 0.51803(18) 0.0536(12) Uani 1 1 d . . . H6M H 0.1904 -0.0223 0.5255 0.080 Uiso 1 1 calc R . . C6M C 0.1064(3) 0.0238(5) 0.5219(3) 0.061(2) Uani 1 1 d . . . H6M1 H 0.1269 0.0569 0.5552 0.091 Uiso 1 1 calc R . . H6M2 H 0.0629 -0.0062 0.5195 0.091 Uiso 1 1 calc R . . H6M3 H 0.0978 0.0705 0.4938 0.091 Uiso 1 1 calc R . . O4M O 0.2173(6) 0.4964(8) 0.6779(4) 0.163(4) Uiso 1 1 d . . . H4M H 0.2369 0.5138 0.7088 0.244 Uiso 1 1 calc R . . C4M C 0.2650(4) 0.4748(6) 0.6579(4) 0.078(2) Uiso 1 1 d . . . H4M1 H 0.2895 0.5336 0.6553 0.116 Uiso 1 1 calc R . . H4M2 H 0.2425 0.4467 0.6234 0.116 Uiso 1 1 calc R . . H4M3 H 0.2977 0.4282 0.6803 0.116 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 Ir1 0.01737(10) 0.02121(11) 0.02094(11) 0.00060(8) 0.00368(8) -0.00049(8) P1 0.0218(7) 0.0226(6) 0.0247(7) -0.0005(5) 0.0063(6) -0.0023(5) P2 0.0210(6) 0.0257(7) 0.0224(7) 0.0005(5) 0.0055(6) -0.0036(5) P3 0.0172(6) 0.0247(6) 0.0241(7) -0.0006(5) 0.0033(6) 0.0002(5) P4 0.0222(6) 0.0231(6) 0.0232(7) 0.0019(5) 0.0068(5) 0.0015(5) P5 0.0180(6) 0.0234(7) 0.0273(8) 0.0008(5) 0.0031(6) -0.0005(5) P6 0.0190(7) 0.0312(7) 0.0273(8) -0.0009(6) 0.0031(6) 0.0020(5) C1 0.017(2) 0.030(3) 0.022(3) -0.002(2) -0.001(2) -0.004(2) C2 0.017(2) 0.019(2) 0.034(3) 0.002(2) 0.004(2) -0.0001(19) C3 0.047(4) 0.028(3) 0.036(3) 0.001(2) 0.017(3) 0.000(2) C4 0.057(4) 0.029(3) 0.070(5) -0.001(3) 0.035(4) 0.007(3) C5 0.040(3) 0.029(3) 0.061(5) 0.012(3) 0.019(3) 0.011(3) C6 0.032(3) 0.041(3) 0.036(4) 0.005(3) 0.001(3) 0.001(3) C7 0.026(3) 0.030(3) 0.033(3) -0.001(2) 0.002(3) -0.001(2) C8 0.019(3) 0.027(3) 0.026(3) 0.000(2) 0.003(2) 0.000(2) C9 0.027(3) 0.033(3) 0.030(3) 0.000(2) 0.003(3) -0.007(2) C10 0.036(3) 0.036(3) 0.040(4) 0.004(3) 0.018(3) -0.008(2) C11 0.029(3) 0.042(3) 0.045(4) -0.001(3) 0.005(3) -0.012(3) C12 0.033(3) 0.057(4) 0.033(4) 0.001(3) 0.002(3) -0.015(3) C13 0.032(3) 0.039(3) 0.025(3) 0.003(2) 0.004(3) -0.009(2) C14 0.027(3) 0.033(3) 0.021(3) -0.002(2) 0.007(2) 0.000(2) C15 0.031(3) 0.040(3) 0.042(4) 0.002(3) 0.016(3) 0.000(2) C16 0.029(3) 0.064(4) 0.049(4) -0.002(3) 0.020(3) -0.006(3) C17 0.026(3) 0.072(5) 0.046(4) -0.009(3) 0.016(3) 0.004(3) C18 0.035(3) 0.051(4) 0.046(4) -0.005(3) 0.012(3) 0.014(3) C19 0.028(3) 0.041(3) 0.036(3) 0.001(3) 0.013(3) 0.001(2) C20 0.023(3) 0.032(3) 0.032(3) 0.008(2) 0.009(2) -0.002(2) C21 0.025(3) 0.036(3) 0.029(3) 0.001(2) 0.005(2) -0.004(2) C22 0.030(3) 0.037(3) 0.053(4) 0.018(3) 0.006(3) -0.004(2) C23 0.050(4) 0.064(5) 0.041(4) 0.028(4) 0.005(3) -0.010(3) C24 0.067(5) 0.068(5) 0.025(4) 0.002(3) 0.012(3) -0.022(4) C25 0.050(4) 0.044(3) 0.028(3) 0.002(3) 0.011(3) -0.010(3) C26 0.025(3) 0.032(3) 0.028(3) 0.002(2) 0.007(2) 0.004(2) C27 0.022(3) 0.030(3) 0.023(3) -0.003(2) 0.004(2) 0.000(2) C28 0.026(3) 0.036(3) 0.032(3) -0.001(2) 0.007(2) -0.003(2) C29 0.019(3) 0.068(4) 0.041(4) -0.011(3) 0.006(3) -0.003(3) C30 0.034(3) 0.059(4) 0.036(4) -0.006(3) 0.001(3) 0.022(3) C31 0.040(3) 0.034(3) 0.043(4) 0.002(3) 0.008(3) 0.011(3) C32 0.025(3) 0.031(3) 0.038(3) 0.004(2) 0.005(3) 0.003(2) C33 0.020(3) 0.025(3) 0.034(3) -0.002(2) 0.002(2) 0.002(2) C34 0.041(3) 0.035(3) 0.034(4) -0.007(3) 0.004(3) -0.010(3) C35 0.041(4) 0.044(4) 0.052(4) -0.022(3) 0.003(3) -0.010(3) C36 0.039(4) 0.029(3) 0.065(5) 0.000(3) 0.006(3) -0.007(3) C37 0.043(4) 0.031(3) 0.050(4) 0.012(3) 0.011(3) -0.002(3) C38 0.028(3) 0.033(3) 0.035(3) 0.001(2) 0.006(3) -0.003(2) C39 0.042(3) 0.023(3) 0.031(3) -0.004(2) 0.020(3) -0.004(2) C40 0.067(5) 0.041(4) 0.026(3) 0.004(3) 0.006(3) -0.002(3) C41 0.132(8) 0.044(4) 0.039(5) 0.009(3) 0.018(5) -0.017(5) C42 0.132(8) 0.042(4) 0.060(5) -0.010(4) 0.058(6) -0.037(5) C43 0.077(5) 0.039(4) 0.061(5) -0.015(3) 0.043(4) -0.023(3) C44 0.048(4) 0.031(3) 0.050(4) -0.002(3) 0.027(3) -0.009(3) C45 0.017(2) 0.029(3) 0.020(3) -0.006(2) -0.002(2) 0.000(2) C46 0.025(3) 0.031(3) 0.033(3) -0.001(2) 0.005(3) -0.001(2) C47 0.028(3) 0.048(4) 0.030(3) -0.006(3) 0.004(3) 0.003(3) C48 0.032(3) 0.044(3) 0.030(3) -0.008(3) -0.002(3) 0.012(3) C49 0.038(3) 0.032(3) 0.037(4) 0.001(3) 0.000(3) 0.004(2) C50 0.026(3) 0.031(3) 0.029(3) 0.001(2) 0.003(2) 0.005(2) C51 0.017(3) 0.034(3) 0.027(3) -0.002(2) 0.004(2) 0.003(2) C52 0.017(2) 0.028(3) 0.028(3) 0.004(2) 0.003(2) 0.004(2) C53 0.028(3) 0.029(3) 0.035(3) 0.006(2) 0.008(3) 0.006(2) C54 0.026(3) 0.034(3) 0.049(4) 0.005(3) 0.010(3) -0.004(2) C55 0.024(3) 0.049(4) 0.048(4) 0.008(3) 0.012(3) -0.001(3) C56 0.029(3) 0.042(3) 0.034(3) -0.002(3) 0.009(3) 0.006(2) C57 0.023(3) 0.031(3) 0.031(3) 0.003(2) 0.005(2) 0.002(2) C58 0.024(3) 0.025(3) 0.022(3) -0.001(2) 0.004(2) -0.001(2) C59 0.029(3) 0.026(3) 0.035(3) -0.001(2) 0.008(3) 0.001(2) C60 0.040(3) 0.032(3) 0.048(4) -0.001(3) 0.014(3) -0.008(3) C61 0.058(4) 0.024(3) 0.047(4) 0.002(3) 0.021(3) 0.003(3) C62 0.042(4) 0.029(3) 0.041(4) 0.004(3) 0.011(3) 0.011(3) C63 0.029(3) 0.029(3) 0.034(3) -0.002(2) 0.007(3) 0.001(2) C64 0.021(3) 0.035(3) 0.025(3) 0.000(2) 0.003(2) 0.000(2) C65 0.028(3) 0.037(3) 0.040(4) 0.007(3) 0.009(3) -0.001(2) C66 0.032(3) 0.040(3) 0.047(4) 0.005(3) 0.009(3) -0.008(3) C67 0.046(4) 0.029(3) 0.042(4) 0.003(3) 0.000(3) -0.008(3) C68 0.039(4) 0.038(3) 0.043(4) -0.002(3) 0.006(3) 0.004(3) C69 0.023(3) 0.037(3) 0.037(3) -0.001(3) 0.006(3) -0.001(2) C70 0.027(3) 0.030(3) 0.025(3) 0.002(2) 0.004(2) 0.002(2) C71 0.029(3) 0.033(3) 0.039(4) 0.002(3) 0.010(3) 0.004(2) C72 0.035(3) 0.045(4) 0.032(3) 0.005(3) 0.003(3) 0.007(3) C73 0.061(4) 0.034(3) 0.052(4) 0.013(3) 0.025(4) 0.007(3) C74 0.049(4) 0.045(4) 0.050(4) 0.004(3) 0.018(4) -0.009(3) C75 0.037(3) 0.043(3) 0.047(4) 0.005(3) 0.008(3) -0.001(3) Cl1 0.0460(9) 0.0510(9) 0.0393(9) 0.0013(7) 0.0144(7) 0.0067(7) O1M 0.067(4) 0.078(4) 0.084(4) 0.026(3) 0.030(3) 0.030(3) C1M 0.074(6) 0.088(6) 0.061(5) 0.012(4) 0.033(5) 0.027(5) O2M 0.054(3) 0.051(3) 0.072(4) -0.007(3) -0.005(3) 0.019(2) C2M 0.052(5) 0.056(5) 0.180(11) -0.003(6) 0.008(6) -0.003(4) O3M 0.046(3) 0.039(2) 0.052(3) -0.001(2) 0.015(2) -0.0056(19) C3M 0.049(4) 0.051(4) 0.049(4) 0.004(3) 0.013(3) 0.004(3) C5M 0.103(7) 0.057(5) 0.099(7) -0.001(5) 0.024(6) 0.000(5) O6M 0.050(3) 0.056(3) 0.060(3) 0.003(2) 0.026(2) 0.012(2) C6M 0.044(4) 0.073(5) 0.075(5) 0.038(4) 0.035(4) 0.025(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 P3 2.2989(13) . ? Ir1 P2 2.3153(13) . ? Ir1 P4 2.3327(13) . ? Ir1 P5 2.3598(13) . ? Ir1 P1 2.3896(13) . ? P1 C8 1.839(5) . ? P1 C2 1.842(5) . ? P1 C1 1.847(5) . ? P2 C20 1.833(5) . ? P2 C14 1.833(5) . ? P2 C1 1.846(5) . ? P3 C33 1.833(5) . ? P3 C26 1.845(5) . ? P3 C27 1.851(5) . ? P4 C39 1.806(5) . ? P4 C26 1.835(5) . ? P4 C45 1.837(5) . ? P5 C52 1.832(5) . ? P5 C58 1.848(5) . ? P5 C51 1.861(5) . ? P6 C64 1.836(5) . ? P6 C70 1.849(5) . ? P6 C51 1.872(5) . ? C2 C7 1.383(7) . ? C2 C3 1.398(7) . ? C3 C4 1.387(8) . ? C4 C5 1.384(9) . ? C5 C6 1.366(8) . ? C6 C7 1.388(7) . ? C8 C13 1.380(7) . ? C8 C9 1.387(7) . ? C9 C10 1.388(7) . ? C10 C11 1.381(8) . ? C11 C12 1.364(8) . ? C12 C13 1.395(7) . ? C14 C19 1.383(7) . ? C14 C15 1.398(7) . ? C15 C16 1.384(8) . ? C16 C17 1.381(9) . ? C17 C18 1.378(9) . ? C18 C19 1.389(7) . ? C20 C25 1.376(8) . ? C20 C21 1.391(7) . ? C21 C22 1.386(8) . ? C22 C23 1.365(9) . ? C23 C24 1.375(10) . ? C24 C25 1.377(8) . ? C27 C32 1.374(7) . ? C27 C28 1.388(7) . ? C28 C29 1.380(8) . ? C29 C30 1.364(9) . ? C30 C31 1.390(8) . ? C31 C32 1.370(7) . ? C33 C38 1.382(7) . ? C33 C34 1.392(8) . ? C34 C35 1.375(8) . ? C35 C36 1.383(9) . ? C36 C37 1.372(9) . ? C37 C38 1.374(7) . ? C39 C44 1.390(8) . ? C39 C40 1.387(8) . ? C40 C41 1.391(9) . ? C41 C42 1.338(11) . ? C42 C43 1.393(11) . ? C43 C44 1.361(8) . ? C45 C50 1.393(7) . ? C45 C46 1.390(7) . ? C46 C47 1.384(7) . ? C47 C48 1.392(8) . ? C48 C49 1.373(8) . ? C49 C50 1.377(7) . ? C52 C57 1.390(7) . ? C52 C53 1.415(7) . ? C53 C54 1.382(7) . ? C54 C55 1.379(8) . ? C55 C56 1.379(8) . ? C56 C57 1.379(7) . ? C58 C59 1.380(7) . ? C58 C63 1.401(7) . ? C59 C60 1.395(7) . ? C60 C61 1.376(8) . ? C61 C62 1.365(8) . ? C62 C63 1.398(7) . ? C64 C65 1.380(7) . ? C64 C69 1.384(7) . ? C65 C66 1.383(8) . ? C66 C67 1.381(8) . ? C67 C68 1.379(8) . ? C68 C69 1.397(8) . ? C70 C71 1.383(7) . ? C70 C75 1.398(7) . ? C71 C72 1.371(8) . ? C72 C73 1.375(8) . ? C73 C74 1.385(9) . ? C74 C75 1.377(8) . ? O1M C1M 1.393(9) . ? O2M C2M 1.365(9) . ? O3M C3M 1.396(8) . ? O5M C5M 1.409(10) . ? O5MA C5M 1.52(2) . ? O6M C6M 1.376(7) . ? O4M C4M 1.343(11) . ? 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 P3 Ir1 P2 95.91(5) . . ? P3 Ir1 P4 71.48(4) . . ? P2 Ir1 P4 165.51(5) . . ? P3 Ir1 P5 135.48(5) . . ? P2 Ir1 P5 97.99(5) . . ? P4 Ir1 P5 96.11(4) . . ? P3 Ir1 P1 123.17(4) . . ? P2 Ir1 P1 71.18(4) . . ? P4 Ir1 P1 109.25(4) . . ? P5 Ir1 P1 101.34(4) . . ? C8 P1 C2 95.5(2) . . ? C8 P1 C1 104.9(2) . . ? C2 P1 C1 106.7(2) . . ? C8 P1 Ir1 130.80(16) . . ? C2 P1 Ir1 122.01(17) . . ? C1 P1 Ir1 94.17(16) . . ? C20 P2 C14 100.2(2) . . ? C20 P2 C1 107.1(2) . . ? C14 P2 C1 104.1(2) . . ? C20 P2 Ir1 126.51(17) . . ? C14 P2 Ir1 119.67(17) . . ? C1 P2 Ir1 96.69(16) . . ? C33 P3 C26 106.9(2) . . ? C33 P3 C27 100.0(2) . . ? C26 P3 C27 101.7(2) . . ? C33 P3 Ir1 122.67(17) . . ? C26 P3 Ir1 96.80(17) . . ? C27 P3 Ir1 125.47(17) . . ? C39 P4 C26 108.8(3) . . ? C39 P4 C45 101.3(2) . . ? C26 P4 C45 100.7(2) . . ? C39 P4 Ir1 122.85(17) . . ? C26 P4 Ir1 95.93(16) . . ? C45 P4 Ir1 124.08(17) . . ? C52 P5 C58 103.7(2) . . ? C52 P5 C51 100.6(2) . . ? C58 P5 C51 102.1(2) . . ? C52 P5 Ir1 114.85(16) . . ? C58 P5 Ir1 117.94(17) . . ? C51 P5 Ir1 115.35(16) . . ? C64 P6 C70 99.3(2) . . ? C64 P6 C51 100.7(2) . . ? C70 P6 C51 103.2(2) . . ? P2 C1 P1 95.7(2) . . ? C7 C2 C3 118.7(5) . . ? C7 C2 P1 118.5(4) . . ? C3 C2 P1 122.2(4) . . ? C4 C3 C2 119.6(5) . . ? C5 C4 C3 120.4(6) . . ? C6 C5 C4 120.4(5) . . ? C5 C6 C7 119.4(6) . . ? C2 C7 C6 121.4(5) . . ? C13 C8 C9 118.4(5) . . ? C13 C8 P1 123.8(4) . . ? C9 C8 P1 117.7(4) . . ? C10 C9 C8 121.2(5) . . ? C11 C10 C9 119.2(5) . . ? C12 C11 C10 120.4(5) . . ? C11 C12 C13 120.2(6) . . ? C8 C13 C12 120.5(5) . . ? C19 C14 C15 118.2(5) . . ? C19 C14 P2 121.0(4) . . ? C15 C14 P2 120.8(4) . . ? C16 C15 C14 120.5(5) . . ? C17 C16 C15 120.8(6) . . ? C16 C17 C18 119.0(5) . . ? C17 C18 C19 120.5(6) . . ? C14 C19 C18 121.0(5) . . ? C25 C20 C21 119.0(5) . . ? C25 C20 P2 120.9(4) . . ? C21 C20 P2 120.0(4) . . ? C22 C21 C20 120.6(5) . . ? C23 C22 C21 119.3(6) . . ? C22 C23 C24 120.7(6) . . ? C23 C24 C25 120.2(6) . . ? C20 C25 C24 120.3(6) . . ? P4 C26 P3 94.7(2) . . ? C32 C27 C28 117.9(5) . . ? C32 C27 P3 118.0(4) . . ? C28 C27 P3 124.0(4) . . ? C29 C28 C27 120.8(5) . . ? C30 C29 C28 120.1(5) . . ? C29 C30 C31 120.0(5) . . ? C32 C31 C30 119.1(5) . . ? C31 C32 C27 122.1(5) . . ? C38 C33 C34 117.5(5) . . ? C38 C33 P3 119.2(4) . . ? C34 C33 P3 123.0(4) . . ? C35 C34 C33 121.2(6) . . ? C34 C35 C36 120.3(6) . . ? C37 C36 C35 119.1(6) . . ? C36 C37 C38 120.5(6) . . ? C37 C38 C33 121.5(6) . . ? C44 C39 C40 118.2(5) . . ? C44 C39 P4 117.3(4) . . ? C40 C39 P4 124.5(5) . . ? C39 C40 C41 119.3(7) . . ? C42 C41 C40 121.4(7) . . ? C41 C42 C43 120.3(6) . . ? C44 C43 C42 118.9(7) . . ? C43 C44 C39 121.8(6) . . ? C50 C45 C46 118.7(5) . . ? C50 C45 P4 117.5(4) . . ? C46 C45 P4 123.6(4) . . ? C47 C46 C45 120.3(5) . . ? C46 C47 C48 119.9(5) . . ? C49 C48 C47 119.9(5) . . ? C48 C49 C50 120.1(5) . . ? C49 C50 C45 120.9(5) . . ? P5 C51 P6 117.0(3) . . ? C57 C52 C53 117.6(5) . . ? C57 C52 P5 124.0(4) . . ? C53 C52 P5 118.3(4) . . ? C54 C53 C52 120.4(5) . . ? C53 C54 C55 120.8(5) . . ? C56 C55 C54 119.4(5) . . ? C55 C56 C57 120.6(5) . . ? C56 C57 C52 121.3(5) . . ? C59 C58 C63 118.8(5) . . ? C59 C58 P5 117.9(4) . . ? C63 C58 P5 123.2(4) . . ? C58 C59 C60 121.0(5) . . ? C61 C60 C59 119.7(6) . . ? C62 C61 C60 120.1(5) . . ? C61 C62 C63 120.9(5) . . ? C58 C63 C62 119.4(5) . . ? C65 C64 C69 118.9(5) . . ? C65 C64 P6 118.1(4) . . ? C69 C64 P6 122.9(4) . . ? C66 C65 C64 122.0(5) . . ? C65 C66 C67 118.4(5) . . ? C68 C67 C66 121.0(6) . . ? C67 C68 C69 119.7(6) . . ? C64 C69 C68 120.0(5) . . ? C71 C70 C75 117.8(5) . . ? C71 C70 P6 119.4(4) . . ? C75 C70 P6 122.3(4) . . ? C72 C71 C70 121.0(5) . . ? C73 C72 C71 121.0(6) . . ? C72 C73 C74 119.1(6) . . ? C75 C74 C73 120.0(6) . . ? C74 C75 C70 121.1(6) . . ? O5M C5M O5MA 102.5(11) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.762 _refine_diff_density_min -0.896 _refine_diff_density_rms 0.138 #=== END data_FOSpan _database_code_depnum_ccdc_archive 'CCDC 770465' #TrackingRef '- dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C51 H44 I Ir O2 P4, 3(C3 H6 O)' _chemical_formula_sum 'C60 H62 I Ir O5 P4' _chemical_formula_weight 1306.16 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' O O 0.0106 0.0060 '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' I I -0.4742 1.8119 '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_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3388(7) _cell_length_b 13.1005(7) _cell_length_c 17.6742(10) _cell_angle_alpha 84.285(2) _cell_angle_beta 79.868(2) _cell_angle_gamma 79.862(2) _cell_volume 2761.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7451 _cell_measurement_theta_min 2.2185 _cell_measurement_theta_max 25.0845 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.140 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.035 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 3.140 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.748 _exptl_absorpt_correction_T_max 0.960 _exptl_absorpt_process_details ; R. H. Blessing, Acta Crystallogr., Sect A 1995, 51, 33-38. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_reflns_number 25015 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_sigmaI/netI 0.0893 _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 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 25.09 _reflns_number_total 9747 _reflns_number_gt 8418 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v. 5.611 (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT+ v. 6.45 (Bruker AXS, 2003)' _computing_data_reduction 'SAINT+ v. 6.45 (Bruker AXS, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP program, SHELXTL v6.12, Bruker2000' _computing_publication_material 'XCIF program, SHELXTLv6.12, BrukerAXS' _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. Hydrogen atoms have been located and refined with a rigid model. A disorder has been oserved in a phenyl cycle, with three carbon atoms in two possible positions with refined occupancy factors of 0.588 and 0.412. The disordered carbon atoms have been refined with isotropic thermal parameters and the hydrogen atoms bounded to these carbon atoms have not been included in the model. The hydride ligand was included from electrostatic potential calculations (HYDEX program). The highest peak and the deepest hole are located around iridium and iodine atoms, respectively. Both of them can be artefacts, probably due to the absorption effects. Several attempts have been made to reduce this effect, with no success. ; _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^)+(0.0692P)^2^+51.9456P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9747 _refine_ls_number_parameters 645 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0696 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1739 _refine_ls_wR_factor_gt 0.1683 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.000 _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 0.33039(3) 0.29451(3) 0.232674(19) 0.01016(13) Uani 1 1 d . . . H H 0.3890 0.3906 0.1922 0.03(3) Uiso 1 1 d . . . I1 I 0.24146(8) 0.12423(7) 0.30076(5) 0.0485(3) Uani 1 1 d . . . P1 P 0.15798(19) 0.40034(18) 0.22524(14) 0.0133(5) Uani 1 1 d . . . P2 P 0.27960(19) 0.28416(18) 0.11119(13) 0.0128(5) Uani 1 1 d . . . P3 P 0.50824(19) 0.19772(18) 0.23736(14) 0.0131(5) Uani 1 1 d . . . P4 P 0.3869(2) 0.32735(18) 0.34591(14) 0.0131(5) Uani 1 1 d . . . O1 O 0.0072(5) 0.5011(5) 0.0985(4) 0.0177(14) Uani 1 1 d . . . H1 H -0.0290 0.5234 0.0626 0.027 Uiso 1 1 calc R . . O2 O 0.0952(6) 0.3924(5) 0.0082(4) 0.0213(15) Uani 1 1 d . . . C1 C 0.1546(8) 0.3751(7) 0.1291(5) 0.016(2) Uani 1 1 d . . . C2 C 0.0854(8) 0.4223(7) 0.0759(5) 0.015(2) Uani 1 1 d . . . C3 C 0.1537(8) 0.5399(7) 0.2323(6) 0.017(2) Uani 1 1 d . . . C4 C 0.1946(9) 0.5991(8) 0.1682(6) 0.024(2) Uani 1 1 d . . . H4 H 0.2186 0.5688 0.1202 0.036 Uiso 1 1 calc R . . C5 C 0.2009(9) 0.7035(8) 0.1738(7) 0.030(3) Uani 1 1 d . . . H5 H 0.2293 0.7441 0.1296 0.044 Uiso 1 1 calc R . . C6 C 0.1654(9) 0.7481(8) 0.2443(8) 0.033(3) Uani 1 1 d . . . H6 H 0.1702 0.8188 0.2484 0.049 Uiso 1 1 calc R . . C7 C 0.1237(9) 0.6894(9) 0.3075(8) 0.033(3) Uani 1 1 d . . . H7 H 0.0989 0.7199 0.3554 0.050 Uiso 1 1 calc R . . C8 C 0.1172(8) 0.5843(8) 0.3023(6) 0.022(2) Uani 1 1 d . . . H8 H 0.0880 0.5440 0.3463 0.033 Uiso 1 1 calc R . . C9 C 0.0329(8) 0.3757(7) 0.2931(6) 0.017(2) Uani 1 1 d . . . C10 C 0.0420(8) 0.3318(8) 0.3663(6) 0.024(2) Uani 1 1 d . . . H10 H 0.1136 0.3120 0.3810 0.035 Uiso 1 1 calc R . . C11 C -0.0532(9) 0.3158(9) 0.4195(6) 0.026(2) Uani 1 1 d . . . H11 H -0.0461 0.2862 0.4700 0.040 Uiso 1 1 calc R . . C12 C -0.1576(9) 0.3434(9) 0.3980(6) 0.026(2) Uani 1 1 d . . . H12 H -0.2225 0.3320 0.4334 0.039 Uiso 1 1 calc R . . C13 C -0.1670(9) 0.3881(9) 0.3241(6) 0.026(2) Uani 1 1 d . . . H13 H -0.2387 0.4081 0.3095 0.039 Uiso 1 1 calc R . . C14 C -0.0722(8) 0.4038(8) 0.2711(6) 0.021(2) Uani 1 1 d . . . H14 H -0.0792 0.4334 0.2206 0.032 Uiso 1 1 calc R . . C15 C 0.2516(8) 0.1621(7) 0.0844(5) 0.016(2) Uani 1 1 d . . . C16 C 0.1528(9) 0.1252(9) 0.1198(6) 0.027(2) Uani 1 1 d . . . H16 H 0.0990 0.1672 0.1539 0.041 Uiso 1 1 calc R . . C17 C 0.1336(10) 0.0289(9) 0.1055(7) 0.033(3) Uani 1 1 d . . . H17 H 0.0669 0.0048 0.1298 0.050 Uiso 1 1 calc R . . C18 C 0.2117(11) -0.0332(9) 0.0553(7) 0.034(3) Uani 1 1 d . . . H18 H 0.1985 -0.0997 0.0458 0.052 Uiso 1 1 calc R . . C19 C 0.3093(10) 0.0024(8) 0.0192(7) 0.032(3) Uani 1 1 d . . . H19 H 0.3630 -0.0397 -0.0148 0.048 Uiso 1 1 calc R . . C20 C 0.3272(9) 0.0993(8) 0.0333(6) 0.023(2) Uani 1 1 d . . . H20 H 0.3929 0.1239 0.0074 0.035 Uiso 1 1 calc R . . C21 C 0.3750(8) 0.3254(7) 0.0271(5) 0.0152(19) Uani 1 1 d . . . C22 C 0.3471(8) 0.3414(8) -0.0452(6) 0.021(2) Uani 1 1 d . . . H22 H 0.2767 0.3281 -0.0530 0.031 Uiso 1 1 calc R . . C23 C 0.4202(9) 0.3770(8) -0.1076(6) 0.022(2) Uani 1 1 d . . . H23 H 0.4026 0.3792 -0.1580 0.033 Uiso 1 1 calc R . . C24A C 0.5148(18) 0.408(2) -0.0985(12) 0.021(5) Uiso 0.59(5) 1 d P . . C25A C 0.5450(18) 0.400(2) -0.0247(11) 0.028(6) Uiso 0.59(5) 1 d P . . C26A C 0.4749(17) 0.361(2) 0.0380(11) 0.023(5) Uiso 0.59(5) 1 d P . . C24B C 0.529(2) 0.374(3) -0.1018(15) 0.014(7) Uiso 0.41(5) 1 d P . . C25B C 0.563(2) 0.351(3) -0.0294(14) 0.020(8) Uiso 0.41(5) 1 d P . . C26B C 0.487(2) 0.321(3) 0.0350(14) 0.016(7) Uiso 0.41(5) 1 d P . . C27 C 0.5083(8) 0.2220(7) 0.3389(5) 0.017(2) Uani 1 1 d . . . H27A H 0.4949 0.1610 0.3749 0.021 Uiso 1 1 calc R . . H27B H 0.5774 0.2457 0.3460 0.021 Uiso 1 1 calc R . . C28 C 0.6353(8) 0.2379(8) 0.1813(5) 0.017(2) Uani 1 1 d . . . C29 C 0.6492(8) 0.3432(8) 0.1795(6) 0.021(2) Uani 1 1 d . . . H29 H 0.5934 0.3916 0.2071 0.031 Uiso 1 1 calc R . . C30 C 0.7447(9) 0.3753(9) 0.1372(6) 0.027(2) Uani 1 1 d . . . H30 H 0.7543 0.4457 0.1368 0.040 Uiso 1 1 calc R . . C31 C 0.8263(9) 0.3066(8) 0.0956(6) 0.025(2) Uani 1 1 d . . . H31 H 0.8913 0.3295 0.0667 0.037 Uiso 1 1 calc R . . C32 C 0.8117(9) 0.2039(9) 0.0966(6) 0.028(2) Uani 1 1 d . . . H32 H 0.8671 0.1562 0.0682 0.042 Uiso 1 1 calc R . . C33 C 0.7167(8) 0.1698(8) 0.1390(6) 0.024(2) Uani 1 1 d . . . H33 H 0.7077 0.0993 0.1388 0.035 Uiso 1 1 calc R . . C34 C 0.5373(8) 0.0576(7) 0.2331(5) 0.0146(19) Uani 1 1 d . . . C35 C 0.6136(8) -0.0027(8) 0.2751(6) 0.021(2) Uani 1 1 d . . . H35 H 0.6491 0.0291 0.3078 0.031 Uiso 1 1 calc R . . C36 C 0.6382(9) -0.1105(8) 0.2692(6) 0.024(2) Uani 1 1 d . . . H36 H 0.6891 -0.1525 0.2985 0.036 Uiso 1 1 calc R . . C37 C 0.5871(9) -0.1546(8) 0.2201(6) 0.028(2) Uani 1 1 d . . . H37 H 0.6050 -0.2274 0.2149 0.042 Uiso 1 1 calc R . . C38 C 0.5110(9) -0.0958(8) 0.1783(7) 0.028(2) Uani 1 1 d . . . H38 H 0.4757 -0.1278 0.1455 0.042 Uiso 1 1 calc R . . C39 C 0.4867(8) 0.0098(8) 0.1847(6) 0.021(2) Uani 1 1 d . . . H39 H 0.4347 0.0508 0.1557 0.032 Uiso 1 1 calc R . . C40 C 0.4424(8) 0.4465(7) 0.3492(6) 0.017(2) Uani 1 1 d . . . C41 C 0.4076(8) 0.5363(7) 0.3056(5) 0.016(2) Uani 1 1 d . . . H41 H 0.3547 0.5359 0.2726 0.024 Uiso 1 1 calc R . . C42 C 0.4498(8) 0.6270(8) 0.3098(6) 0.021(2) Uani 1 1 d . . . H42 H 0.4256 0.6884 0.2798 0.031 Uiso 1 1 calc R . . C43 C 0.5269(9) 0.6275(8) 0.3576(6) 0.025(2) Uani 1 1 d . . . H43 H 0.5556 0.6894 0.3607 0.037 Uiso 1 1 calc R . . C44 C 0.5627(9) 0.5374(9) 0.4013(6) 0.024(2) Uani 1 1 d . . . H44 H 0.6171 0.5376 0.4332 0.036 Uiso 1 1 calc R . . C45 C 0.5196(9) 0.4477(8) 0.3986(6) 0.022(2) Uani 1 1 d . . . H45 H 0.5421 0.3872 0.4300 0.033 Uiso 1 1 calc R . . C46 C 0.3037(8) 0.3130(7) 0.4414(5) 0.0142(19) Uani 1 1 d . . . C47 C 0.2421(8) 0.4004(8) 0.4764(6) 0.021(2) Uani 1 1 d . . . H47 H 0.2483 0.4680 0.4528 0.031 Uiso 1 1 calc R . . C48 C 0.1716(9) 0.3880(9) 0.5460(6) 0.028(3) Uani 1 1 d . . . H48 H 0.1297 0.4479 0.5696 0.042 Uiso 1 1 calc R . . C49 C 0.1612(9) 0.2911(10) 0.5815(6) 0.032(3) Uani 1 1 d . . . H49 H 0.1131 0.2836 0.6293 0.049 Uiso 1 1 calc R . . C50 C 0.2225(10) 0.2042(10) 0.5459(7) 0.033(3) Uani 1 1 d . . . H50 H 0.2166 0.1368 0.5699 0.049 Uiso 1 1 calc R . . C51 C 0.2920(9) 0.2149(8) 0.4761(6) 0.023(2) Uani 1 1 d . . . H51 H 0.3319 0.1548 0.4518 0.035 Uiso 1 1 calc R . . O61 O 0.9113(8) 0.8729(8) 0.2115(6) 0.056(3) Uani 1 1 d . . . C61 C 0.9053(9) 0.8117(10) 0.1666(8) 0.037(3) Uani 1 1 d . . . C62 C 0.8742(10) 0.7067(10) 0.1919(7) 0.037(3) Uani 1 1 d . . . H62A H 0.9409 0.6534 0.1833 0.056 Uiso 1 1 calc R . . H62B H 0.8189 0.6934 0.1621 0.056 Uiso 1 1 calc R . . H62C H 0.8426 0.7045 0.2468 0.056 Uiso 1 1 calc R . . C63 C 0.9327(14) 0.8335(13) 0.0809(9) 0.060(4) Uani 1 1 d . . . H63A H 0.8648 0.8396 0.0580 0.090 Uiso 1 1 calc R . . H63B H 0.9881 0.7765 0.0589 0.090 Uiso 1 1 calc R . . H63C H 0.9630 0.8987 0.0698 0.090 Uiso 1 1 calc R . . O71 O 0.7835(7) 0.0602(7) 0.3946(5) 0.041(2) Uani 1 1 d . . . C71 C 0.8757(9) 0.0591(9) 0.3574(7) 0.030(3) Uani 1 1 d . . . C72 C 0.9777(13) -0.0066(14) 0.3824(12) 0.076(6) Uani 1 1 d . . . H72A H 0.9591 -0.0348 0.4357 0.114 Uiso 1 1 calc R . . H72B H 1.0363 0.0361 0.3792 0.114 Uiso 1 1 calc R . . H72C H 1.0043 -0.0640 0.3487 0.114 Uiso 1 1 calc R . . C73 C 0.8972(11) 0.1186(10) 0.2833(7) 0.036(3) Uani 1 1 d . . . H73A H 0.9238 0.0708 0.2423 0.054 Uiso 1 1 calc R . . H73B H 0.9540 0.1617 0.2850 0.054 Uiso 1 1 calc R . . H73C H 0.8281 0.1634 0.2730 0.054 Uiso 1 1 calc R . . O81 O 0.6195(7) 0.2464(6) 0.5044(5) 0.040(2) Uani 1 1 d . . . C81 C 0.6459(9) 0.1622(8) 0.5386(6) 0.024(2) Uani 1 1 d . . . C83 C 0.7499(12) 0.1395(13) 0.5740(9) 0.054(4) Uani 1 1 d . . . H83A H 0.7966 0.0764 0.5539 0.081 Uiso 1 1 calc R . . H83B H 0.7300 0.1291 0.6301 0.081 Uiso 1 1 calc R . . H83C H 0.7911 0.1981 0.5613 0.081 Uiso 1 1 calc R . . C82 C 0.5760(10) 0.0795(9) 0.5468(8) 0.037(3) Uani 1 1 d . . . H82A H 0.5012 0.1099 0.5364 0.055 Uiso 1 1 calc R . . H82B H 0.5706 0.0469 0.5994 0.055 Uiso 1 1 calc R . . H82C H 0.6098 0.0270 0.5101 0.055 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 Ir1 0.00807(19) 0.01310(19) 0.01053(19) -0.00137(13) -0.00326(13) -0.00297(13) I1 0.0459(5) 0.0522(6) 0.0481(5) -0.0043(4) -0.0105(4) -0.0067(4) P1 0.0107(12) 0.0151(12) 0.0153(12) -0.0012(9) -0.0044(9) -0.0025(9) P2 0.0106(11) 0.0167(12) 0.0121(12) -0.0013(9) -0.0022(9) -0.0042(9) P3 0.0111(12) 0.0152(12) 0.0141(12) -0.0022(9) -0.0040(9) -0.0027(9) P4 0.0125(12) 0.0153(12) 0.0129(12) -0.0004(9) -0.0040(9) -0.0040(9) O1 0.016(3) 0.018(3) 0.020(4) 0.000(3) -0.008(3) 0.001(3) O2 0.019(4) 0.027(4) 0.019(4) -0.001(3) -0.008(3) 0.001(3) C1 0.010(5) 0.020(5) 0.018(5) -0.006(4) -0.001(4) -0.004(4) C2 0.018(5) 0.014(5) 0.015(5) 0.000(4) -0.004(4) -0.005(4) C3 0.009(5) 0.018(5) 0.026(5) 0.000(4) -0.008(4) -0.003(4) C4 0.021(5) 0.025(6) 0.026(6) 0.003(4) -0.011(4) -0.003(4) C5 0.031(6) 0.016(5) 0.044(7) 0.008(5) -0.015(5) -0.009(5) C6 0.027(6) 0.016(5) 0.059(8) -0.008(5) -0.014(6) -0.003(4) C7 0.022(6) 0.026(6) 0.055(8) -0.021(6) -0.007(6) -0.002(5) C8 0.010(5) 0.029(6) 0.030(6) -0.007(5) -0.005(4) -0.004(4) C9 0.017(5) 0.017(5) 0.019(5) -0.005(4) -0.001(4) -0.007(4) C10 0.014(5) 0.033(6) 0.025(6) 0.001(5) -0.005(4) -0.005(4) C11 0.024(6) 0.035(6) 0.020(5) 0.005(5) -0.006(4) -0.005(5) C12 0.018(5) 0.034(6) 0.026(6) -0.003(5) 0.006(4) -0.011(5) C13 0.013(5) 0.038(6) 0.028(6) -0.004(5) -0.005(4) -0.007(4) C14 0.011(5) 0.030(6) 0.021(5) 0.005(4) -0.003(4) -0.004(4) C15 0.012(5) 0.021(5) 0.017(5) 0.000(4) -0.006(4) -0.003(4) C16 0.030(6) 0.031(6) 0.024(6) -0.011(5) -0.001(5) -0.012(5) C17 0.041(7) 0.031(6) 0.034(6) 0.002(5) -0.005(5) -0.025(5) C18 0.061(8) 0.021(6) 0.027(6) 0.002(5) -0.018(6) -0.013(6) C19 0.045(7) 0.022(6) 0.027(6) -0.006(5) -0.014(5) 0.008(5) C20 0.024(6) 0.027(6) 0.020(5) -0.002(4) -0.007(4) -0.006(4) C21 0.016(5) 0.019(5) 0.011(5) -0.003(4) -0.002(4) -0.001(4) C22 0.018(5) 0.028(6) 0.019(5) 0.003(4) -0.010(4) -0.006(4) C23 0.031(6) 0.024(5) 0.011(5) 0.003(4) -0.006(4) -0.005(4) C27 0.017(5) 0.019(5) 0.019(5) -0.004(4) -0.009(4) -0.003(4) C28 0.012(5) 0.024(5) 0.017(5) -0.002(4) -0.003(4) -0.006(4) C29 0.013(5) 0.025(5) 0.026(6) -0.004(4) -0.005(4) -0.007(4) C30 0.024(6) 0.031(6) 0.030(6) 0.000(5) -0.006(5) -0.016(5) C31 0.019(5) 0.035(6) 0.022(5) 0.001(5) -0.003(4) -0.012(5) C32 0.018(5) 0.041(7) 0.024(6) -0.011(5) 0.006(4) -0.005(5) C33 0.019(5) 0.027(6) 0.027(6) -0.008(4) -0.002(4) -0.007(4) C34 0.011(5) 0.015(5) 0.016(5) 0.000(4) 0.002(4) -0.004(4) C35 0.012(5) 0.024(5) 0.026(6) -0.005(4) -0.005(4) -0.001(4) C36 0.021(5) 0.023(5) 0.027(6) 0.002(4) -0.004(4) 0.001(4) C37 0.029(6) 0.019(5) 0.034(6) -0.003(5) -0.001(5) -0.001(4) C38 0.030(6) 0.025(6) 0.034(6) -0.007(5) -0.010(5) -0.008(5) C39 0.018(5) 0.024(5) 0.025(5) -0.006(4) -0.010(4) -0.005(4) C40 0.010(5) 0.021(5) 0.020(5) -0.005(4) -0.001(4) -0.007(4) C41 0.012(5) 0.019(5) 0.018(5) -0.005(4) -0.001(4) -0.005(4) C42 0.022(5) 0.023(5) 0.018(5) -0.004(4) -0.003(4) -0.005(4) C43 0.027(6) 0.023(5) 0.028(6) -0.007(4) -0.003(5) -0.012(5) C44 0.019(5) 0.038(6) 0.019(5) -0.011(5) -0.008(4) -0.009(5) C45 0.023(5) 0.026(5) 0.019(5) -0.005(4) -0.004(4) -0.006(4) C46 0.014(5) 0.024(5) 0.007(4) -0.004(4) -0.005(4) -0.005(4) C47 0.016(5) 0.030(6) 0.019(5) -0.004(4) -0.005(4) -0.007(4) C48 0.020(6) 0.042(7) 0.025(6) -0.020(5) -0.004(5) -0.006(5) C49 0.021(6) 0.058(8) 0.021(6) -0.009(5) -0.001(5) -0.011(5) C50 0.028(6) 0.044(7) 0.027(6) 0.012(5) -0.009(5) -0.012(5) C51 0.022(5) 0.027(6) 0.019(5) 0.002(4) -0.005(4) -0.002(4) O61 0.038(5) 0.060(6) 0.078(7) -0.044(6) -0.012(5) 0.000(5) C61 0.016(6) 0.048(8) 0.052(8) -0.020(6) -0.016(5) 0.003(5) C62 0.031(7) 0.049(8) 0.031(7) -0.017(6) -0.013(5) 0.011(6) C63 0.065(10) 0.075(11) 0.053(9) -0.001(8) -0.024(8) -0.032(9) O71 0.034(5) 0.051(5) 0.040(5) -0.006(4) -0.003(4) -0.011(4) C71 0.022(6) 0.028(6) 0.044(7) -0.007(5) -0.015(5) -0.003(5) C72 0.041(9) 0.077(12) 0.111(15) 0.035(11) -0.041(10) -0.006(8) C73 0.040(7) 0.047(7) 0.027(6) -0.008(5) -0.003(5) -0.019(6) O81 0.047(5) 0.026(4) 0.042(5) 0.003(4) 0.001(4) -0.001(4) C81 0.024(6) 0.025(6) 0.025(6) -0.005(4) -0.006(5) -0.003(4) C83 0.039(8) 0.079(11) 0.056(9) 0.006(8) -0.033(7) -0.021(7) C82 0.033(7) 0.034(7) 0.046(7) -0.001(6) -0.005(6) -0.015(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 P4 2.334(2) . ? Ir1 P1 2.343(2) . ? Ir1 P3 2.344(2) . ? Ir1 P2 2.363(2) . ? Ir1 I1 2.7369(10) . ? P1 C1 1.771(10) . ? P1 C3 1.836(10) . ? P1 C9 1.836(10) . ? P2 C1 1.776(9) . ? P2 C15 1.817(10) . ? P2 C21 1.826(9) . ? P3 C34 1.814(9) . ? P3 C28 1.832(9) . ? P3 C27 1.853(10) . ? P4 C40 1.821(9) . ? P4 C46 1.825(9) . ? P4 C27 1.844(10) . ? O1 C2 1.323(11) . ? O2 C2 1.274(11) . ? C1 C2 1.407(14) . ? C3 C4 1.378(14) . ? C3 C8 1.388(14) . ? C4 C5 1.398(15) . ? C5 C6 1.397(17) . ? C6 C7 1.366(18) . ? C7 C8 1.407(15) . ? C9 C10 1.378(14) . ? C9 C14 1.397(14) . ? C10 C11 1.401(14) . ? C11 C12 1.385(15) . ? C12 C13 1.392(16) . ? C13 C14 1.395(14) . ? C15 C20 1.395(14) . ? C15 C16 1.410(14) . ? C16 C17 1.379(15) . ? C17 C18 1.395(17) . ? C18 C19 1.393(18) . ? C19 C20 1.379(15) . ? C21 C22 1.367(14) . ? C21 C26B 1.40(3) . ? C21 C26A 1.44(2) . ? C22 C23 1.394(14) . ? C23 C24A 1.34(2) . ? C24A C25A 1.41(3) . ? C25A C26A 1.39(3) . ? C24B C25B 1.41(4) . ? C25B C26B 1.42(3) . ? C28 C33 1.384(14) . ? C28 C29 1.416(14) . ? C29 C30 1.389(14) . ? C30 C31 1.385(16) . ? C31 C32 1.386(15) . ? C32 C33 1.394(14) . ? C34 C35 1.389(14) . ? C34 C39 1.395(14) . ? C35 C36 1.402(14) . ? C36 C37 1.380(16) . ? C37 C38 1.378(16) . ? C38 C39 1.375(15) . ? C40 C41 1.386(14) . ? C40 C45 1.403(14) . ? C41 C42 1.392(13) . ? C42 C43 1.381(15) . ? C43 C44 1.393(15) . ? C44 C45 1.380(14) . ? C46 C51 1.388(14) . ? C46 C47 1.393(14) . ? C47 C48 1.389(14) . ? C48 C49 1.377(17) . ? C49 C50 1.391(17) . ? C50 C51 1.383(15) . ? O61 C61 1.203(14) . ? C61 C62 1.498(18) . ? C61 C63 1.50(2) . ? O71 C71 1.208(14) . ? C71 C73 1.463(17) . ? C71 C72 1.503(18) . ? O81 C81 1.224(13) . ? C81 C82 1.481(15) . ? C81 C83 1.495(16) . ? 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 P4 Ir1 P1 107.41(8) . . ? P4 Ir1 P3 71.94(8) . . ? P1 Ir1 P3 176.42(8) . . ? P4 Ir1 P2 172.00(8) . . ? P1 Ir1 P2 70.49(8) . . ? P3 Ir1 P2 109.64(8) . . ? P4 Ir1 I1 92.74(6) . . ? P1 Ir1 I1 95.18(6) . . ? P3 Ir1 I1 88.38(6) . . ? P2 Ir1 I1 95.14(6) . . ? C1 P1 C3 110.2(5) . . ? C1 P1 C9 113.7(4) . . ? C3 P1 C9 101.7(4) . . ? C1 P1 Ir1 95.1(3) . . ? C3 P1 Ir1 116.0(3) . . ? C9 P1 Ir1 120.4(3) . . ? C1 P2 C15 111.0(4) . . ? C1 P2 C21 112.4(4) . . ? C15 P2 C21 102.6(4) . . ? C1 P2 Ir1 94.3(3) . . ? C15 P2 Ir1 120.3(3) . . ? C21 P2 Ir1 116.4(3) . . ? C34 P3 C28 102.3(4) . . ? C34 P3 C27 105.8(4) . . ? C28 P3 C27 106.5(4) . . ? C34 P3 Ir1 122.6(3) . . ? C28 P3 Ir1 122.6(3) . . ? C27 P3 Ir1 94.4(3) . . ? C40 P4 C46 103.0(4) . . ? C40 P4 C27 105.9(4) . . ? C46 P4 C27 108.2(4) . . ? C40 P4 Ir1 119.2(3) . . ? C46 P4 Ir1 123.6(3) . . ? C27 P4 Ir1 95.0(3) . . ? C2 C1 P1 131.8(7) . . ? C2 C1 P2 127.6(7) . . ? P1 C1 P2 99.9(5) . . ? O2 C2 O1 119.8(9) . . ? O2 C2 C1 122.9(9) . . ? O1 C2 C1 117.3(8) . . ? C4 C3 C8 120.0(9) . . ? C4 C3 P1 119.1(8) . . ? C8 C3 P1 120.7(8) . . ? C3 C4 C5 120.2(10) . . ? C6 C5 C4 120.0(10) . . ? C7 C6 C5 119.7(10) . . ? C6 C7 C8 120.5(11) . . ? C3 C8 C7 119.6(10) . . ? C10 C9 C14 119.7(9) . . ? C10 C9 P1 120.3(8) . . ? C14 C9 P1 119.9(7) . . ? C9 C10 C11 120.9(10) . . ? C12 C11 C10 119.7(10) . . ? C11 C12 C13 119.6(9) . . ? C12 C13 C14 120.7(10) . . ? C13 C14 C9 119.5(9) . . ? C20 C15 C16 117.8(9) . . ? C20 C15 P2 122.7(7) . . ? C16 C15 P2 119.4(7) . . ? C17 C16 C15 120.7(10) . . ? C16 C17 C18 120.2(11) . . ? C19 C18 C17 119.9(10) . . ? C20 C19 C18 119.5(11) . . ? C19 C20 C15 121.9(10) . . ? C22 C21 C26B 118.6(13) . . ? C22 C21 C26A 117.1(11) . . ? C22 C21 P2 122.6(7) . . ? C26B C21 P2 117.7(12) . . ? C26A C21 P2 119.3(10) . . ? C21 C22 C23 121.1(9) . . ? C24A C23 C22 121.9(12) . . ? C23 C24A C25A 119.6(17) . . ? C26A C25A C24A 119.3(18) . . ? C25A C26A C21 120.4(17) . . ? C24B C25B C26B 120(2) . . ? C21 C26B C25B 119(2) . . ? P4 C27 P3 96.0(5) . . ? C33 C28 C29 118.9(9) . . ? C33 C28 P3 122.4(8) . . ? C29 C28 P3 118.7(7) . . ? C30 C29 C28 119.6(10) . . ? C31 C30 C29 121.3(10) . . ? C30 C31 C32 118.9(9) . . ? C31 C32 C33 120.8(10) . . ? C28 C33 C32 120.6(10) . . ? C35 C34 C39 119.2(9) . . ? C35 C34 P3 120.6(7) . . ? C39 C34 P3 120.1(8) . . ? C34 C35 C36 120.0(9) . . ? C37 C36 C35 118.9(10) . . ? C38 C37 C36 121.7(10) . . ? C39 C38 C37 119.1(10) . . ? C38 C39 C34 121.0(10) . . ? C41 C40 C45 119.6(9) . . ? C41 C40 P4 121.3(7) . . ? C45 C40 P4 119.1(8) . . ? C40 C41 C42 120.4(9) . . ? C43 C42 C41 119.8(10) . . ? C42 C43 C44 120.1(9) . . ? C45 C44 C43 120.5(10) . . ? C44 C45 C40 119.6(10) . . ? C51 C46 C47 119.2(9) . . ? C51 C46 P4 120.4(7) . . ? C47 C46 P4 120.0(7) . . ? C48 C47 C46 119.6(10) . . ? C49 C48 C47 121.5(10) . . ? C48 C49 C50 118.6(10) . . ? C51 C50 C49 120.8(11) . . ? C50 C51 C46 120.3(10) . . ? O61 C61 C62 122.5(13) . . ? O61 C61 C63 122.4(14) . . ? C62 C61 C63 115.0(11) . . ? O71 C71 C73 123.0(11) . . ? O71 C71 C72 122.6(13) . . ? C73 C71 C72 114.4(12) . . ? O81 C81 C82 121.3(11) . . ? O81 C81 C83 121.1(11) . . ? C82 C81 C83 117.6(11) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.263 _refine_diff_density_min -4.982 _refine_diff_density_rms 0.226 #=== END data_FO3479 _database_code_depnum_ccdc_archive 'CCDC 770466' #TrackingRef '- dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H62 Li2 O8 P4' _chemical_formula_weight 1048.86 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' O O 0.0106 0.0060 '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' Li Li -0.0003 0.0001 '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 11.5057(2) _cell_length_b 15.9886(4) _cell_length_c 32.4517(6) _cell_angle_alpha 92.3670(10) _cell_angle_beta 90.7410(10) _cell_angle_gamma 110.6140(10) _cell_volume 5580.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 0.189 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31591 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0726 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 27.43 _reflns_number_total 23791 _reflns_number_gt 15912 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+10.5381P] 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 23791 _refine_ls_number_parameters 1309 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1212 _refine_ls_R_factor_gt 0.0769 _refine_ls_wR_factor_ref 0.2019 _refine_ls_wR_factor_gt 0.1765 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1A P 0.21801(7) 0.15917(5) 0.50422(2) 0.02286(17) Uani 1 1 d . . . P2A P 0.48893(7) 0.25243(6) 0.49640(2) 0.02356(18) Uani 1 1 d . . . P3A P 0.32975(8) 0.37512(6) 0.22698(3) 0.0297(2) Uani 1 1 d . . . P4A P 0.50568(8) 0.28468(6) 0.24920(3) 0.02780(19) Uani 1 1 d . . . Li1A Li 0.3176(5) 0.3947(4) 0.37418(16) 0.0299(12) Uani 1 1 d . . . Li2A Li 0.1789(5) 0.1639(4) 0.36625(17) 0.0323(13) Uani 1 1 d . . . O1A O 0.3343(2) 0.33780(16) 0.42184(7) 0.0366(6) Uani 1 1 d . . . O2A O 0.2607(2) 0.18860(16) 0.41790(7) 0.0316(5) Uani 1 1 d . . . O3A O 0.3347(2) 0.36328(16) 0.31826(7) 0.0333(5) Uani 1 1 d . . . O4A O 0.2434(2) 0.21476(17) 0.31699(7) 0.0351(6) Uani 1 1 d . . . O5A O 0.3899(2) 0.52722(16) 0.39350(8) 0.0383(6) Uani 1 1 d . . . O6A O 0.1521(2) 0.41741(16) 0.37948(8) 0.0371(6) Uani 1 1 d . . . O7A O -0.0039(2) 0.14373(18) 0.36996(8) 0.0417(6) Uani 1 1 d . . . O8A O 0.1150(2) 0.02758(16) 0.36785(7) 0.0359(6) Uani 1 1 d . . . C1A C 0.3350(3) 0.2608(2) 0.48301(9) 0.0230(6) Uani 1 1 d . . . C2A C 0.3083(3) 0.2623(2) 0.43670(9) 0.0245(6) Uani 1 1 d . . . C3A C 0.0702(3) 0.1741(2) 0.49289(9) 0.0237(6) Uani 1 1 d . . . C4A C 0.0556(3) 0.2455(2) 0.47304(12) 0.0349(8) Uani 1 1 d . . . H4AA H 0.1267 0.2953 0.4668 0.042 Uiso 1 1 calc R . . C5A C -0.0617(3) 0.2447(3) 0.46227(13) 0.0424(9) Uani 1 1 d . . . H5AA H -0.0702 0.2934 0.4483 0.051 Uiso 1 1 calc R . . C6A C -0.1663(3) 0.1737(3) 0.47158(13) 0.0441(10) Uani 1 1 d . . . H6AA H -0.2464 0.1730 0.4637 0.053 Uiso 1 1 calc R . . C7A C -0.1538(3) 0.1040(3) 0.49236(12) 0.0407(9) Uani 1 1 d . . . H7AA H -0.2256 0.0558 0.4996 0.049 Uiso 1 1 calc R . . C8A C -0.0368(3) 0.1039(2) 0.50279(11) 0.0322(7) Uani 1 1 d . . . H8AA H -0.0292 0.0552 0.5170 0.039 Uiso 1 1 calc R . . C9A C 0.2347(3) 0.1871(2) 0.56007(10) 0.0251(7) Uani 1 1 d . . . C10A C 0.1754(3) 0.2382(2) 0.58093(11) 0.0330(8) Uani 1 1 d . . . H10A H 0.1289 0.2658 0.5657 0.040 Uiso 1 1 calc R . . C11A C 0.1836(4) 0.2490(3) 0.62347(12) 0.0439(9) Uani 1 1 d . . . H11A H 0.1416 0.2831 0.6372 0.053 Uiso 1 1 calc R . . C12A C 0.2523(4) 0.2108(3) 0.64608(11) 0.0446(10) Uani 1 1 d . . . H12A H 0.2572 0.2184 0.6753 0.054 Uiso 1 1 calc R . . C13A C 0.3135(3) 0.1621(3) 0.62640(11) 0.0427(9) Uani 1 1 d . . . H13A H 0.3629 0.1373 0.6419 0.051 Uiso 1 1 calc R . . C14A C 0.3034(3) 0.1488(2) 0.58363(11) 0.0341(8) Uani 1 1 d . . . H14A H 0.3439 0.1131 0.5703 0.041 Uiso 1 1 calc R . . C15A C 0.6051(3) 0.3583(2) 0.48155(9) 0.0261(7) Uani 1 1 d . . . C16A C 0.7287(3) 0.3639(2) 0.48614(11) 0.0340(8) Uani 1 1 d . . . H16A H 0.7461 0.3133 0.4946 0.041 Uiso 1 1 calc R . . C17A C 0.8261(3) 0.4417(3) 0.47854(12) 0.0419(9) Uani 1 1 d . . . H17A H 0.9093 0.4433 0.4808 0.050 Uiso 1 1 calc R . . C18A C 0.8026(4) 0.5168(3) 0.46771(12) 0.0449(10) Uani 1 1 d . . . H18A H 0.8694 0.5709 0.4633 0.054 Uiso 1 1 calc R . . C19A C 0.6815(4) 0.5129(3) 0.46328(12) 0.0422(9) Uani 1 1 d . . . H19A H 0.6652 0.5644 0.4554 0.051 Uiso 1 1 calc R . . C20A C 0.5827(3) 0.4343(2) 0.47018(11) 0.0337(8) Uani 1 1 d . . . H20A H 0.4997 0.4327 0.4671 0.040 Uiso 1 1 calc R . . C21A C 0.5048(3) 0.1735(2) 0.45617(10) 0.0242(6) Uani 1 1 d . . . C22A C 0.4749(3) 0.0851(2) 0.46669(11) 0.0320(7) Uani 1 1 d . . . H22A H 0.4451 0.0682 0.4934 0.038 Uiso 1 1 calc R . . C23A C 0.4880(4) 0.0210(3) 0.43869(12) 0.0407(9) Uani 1 1 d . . . H23A H 0.4660 -0.0393 0.4461 0.049 Uiso 1 1 calc R . . C24A C 0.5327(4) 0.0454(3) 0.40035(12) 0.0410(9) Uani 1 1 d . . . H24A H 0.5438 0.0021 0.3814 0.049 Uiso 1 1 calc R . . C25A C 0.5616(3) 0.1329(3) 0.38926(11) 0.0382(8) Uani 1 1 d . . . H25A H 0.5918 0.1495 0.3626 0.046 Uiso 1 1 calc R . . C26A C 0.5468(3) 0.1963(2) 0.41690(10) 0.0314(7) Uani 1 1 d . . . H26A H 0.5656 0.2560 0.4089 0.038 Uiso 1 1 calc R . . C27A C 0.3425(3) 0.2805(2) 0.25647(10) 0.0267(7) Uani 1 1 d . . . C28A C 0.3040(3) 0.2870(2) 0.30122(10) 0.0265(7) Uani 1 1 d . . . C29A C 0.1685(3) 0.3666(2) 0.23452(10) 0.0297(7) Uani 1 1 d . . . C30A C 0.1398(4) 0.4411(3) 0.22539(12) 0.0423(9) Uani 1 1 d . . . H30A H 0.2026 0.4920 0.2154 0.051 Uiso 1 1 calc R . . C31A C 0.0213(4) 0.4429(3) 0.23048(15) 0.0565(12) Uani 1 1 d . . . H31A H 0.0030 0.4944 0.2239 0.068 Uiso 1 1 calc R . . C32A C -0.0687(4) 0.3705(4) 0.24501(14) 0.0553(12) Uani 1 1 d . . . H32A H -0.1498 0.3719 0.2488 0.066 Uiso 1 1 calc R . . C33A C -0.0435(4) 0.2955(3) 0.25426(13) 0.0498(11) Uani 1 1 d . . . H33A H -0.1073 0.2452 0.2642 0.060 Uiso 1 1 calc R . . C34A C 0.0745(3) 0.2927(3) 0.24910(11) 0.0383(8) Uani 1 1 d . . . H34A H 0.0913 0.2406 0.2555 0.046 Uiso 1 1 calc R . . C35A C 0.3149(4) 0.3257(3) 0.17369(11) 0.0455(10) Uani 1 1 d . . . C36A C 0.4204(6) 0.3491(6) 0.15132(15) 0.101(3) Uani 1 1 d . . . H36A H 0.4969 0.3884 0.1633 0.121 Uiso 1 1 calc R . . C37A C 0.4153(9) 0.3150(8) 0.1105(2) 0.159(5) Uani 1 1 d . . . H37A H 0.4887 0.3311 0.0949 0.191 Uiso 1 1 calc R . . C38A C 0.3057(10) 0.2589(6) 0.09312(18) 0.127(4) Uani 1 1 d . . . H38A H 0.3039 0.2334 0.0661 0.152 Uiso 1 1 calc R . . C39A C 0.1980(8) 0.2391(4) 0.11445(16) 0.094(2) Uani 1 1 d . . . H39A H 0.1205 0.2035 0.1017 0.113 Uiso 1 1 calc R . . C40A C 0.2043(6) 0.2720(3) 0.15489(13) 0.0673(15) Uani 1 1 d . . . H40A H 0.1303 0.2572 0.1701 0.081 Uiso 1 1 calc R . . C41A C 0.5067(3) 0.1750(2) 0.26325(11) 0.0336(8) Uani 1 1 d . . . C42A C 0.4118(4) 0.1078(2) 0.28116(11) 0.0372(8) Uani 1 1 d . . . H42A H 0.3372 0.1172 0.2881 0.045 Uiso 1 1 calc R . . C43A C 0.4252(4) 0.0266(3) 0.28909(13) 0.0483(10) Uani 1 1 d . . . H43A H 0.3585 -0.0198 0.3003 0.058 Uiso 1 1 calc R . . C44A C 0.5342(5) 0.0135(3) 0.28076(15) 0.0561(12) Uani 1 1 d . . . H44A H 0.5441 -0.0411 0.2872 0.067 Uiso 1 1 calc R . . C45A C 0.6284(4) 0.0790(3) 0.26323(18) 0.0670(14) Uani 1 1 d . . . H45A H 0.7039 0.0699 0.2575 0.080 Uiso 1 1 calc R . . C46A C 0.6147(4) 0.1587(3) 0.25369(16) 0.0562(12) Uani 1 1 d . . . H46A H 0.6798 0.2028 0.2405 0.067 Uiso 1 1 calc R . . C47A C 0.5971(3) 0.3575(2) 0.29229(10) 0.0294(7) Uani 1 1 d . . . C48A C 0.6277(5) 0.4467(3) 0.29049(16) 0.0687(15) Uani 1 1 d . . . H48A H 0.5959 0.4693 0.2680 0.082 Uiso 1 1 calc R . . C49A C 0.7039(5) 0.5069(3) 0.32022(17) 0.0693(15) Uani 1 1 d . . . H49A H 0.7219 0.5693 0.3181 0.083 Uiso 1 1 calc R . . C50A C 0.7520(4) 0.4775(3) 0.35176(12) 0.0521(11) Uani 1 1 d . . . H50A H 0.8065 0.5182 0.3717 0.063 Uiso 1 1 calc R . . C51A C 0.7212(7) 0.3885(4) 0.35465(17) 0.118(3) Uani 1 1 d . . . H51A H 0.7514 0.3663 0.3776 0.142 Uiso 1 1 calc R . . C52A C 0.6464(7) 0.3290(4) 0.32472(16) 0.103(3) Uani 1 1 d . . . H52A H 0.6291 0.2668 0.3269 0.124 Uiso 1 1 calc R . . C53A C 0.2951(4) 0.5616(3) 0.40433(12) 0.0406(9) Uani 1 1 d . . . H53A H 0.2783 0.5952 0.3814 0.049 Uiso 1 1 calc R . . H53B H 0.3214 0.6025 0.4292 0.049 Uiso 1 1 calc R . . C54A C 0.1816(4) 0.4837(3) 0.41267(12) 0.0416(9) Uani 1 1 d . . . H54A H 0.1951 0.4569 0.4384 0.050 Uiso 1 1 calc R . . H54B H 0.1108 0.5044 0.4166 0.050 Uiso 1 1 calc R . . C55A C 0.1056(4) 0.4443(3) 0.34338(13) 0.0513(11) Uani 1 1 d . . . H55A H 0.0282 0.4542 0.3496 0.077 Uiso 1 1 calc R . . H55B H 0.0895 0.3973 0.3214 0.077 Uiso 1 1 calc R . . H55C H 0.1671 0.4998 0.3343 0.077 Uiso 1 1 calc R . . C56A C 0.5024(4) 0.5959(3) 0.38364(15) 0.0569(12) Uani 1 1 d . . . H56A H 0.5325 0.6382 0.4074 0.085 Uiso 1 1 calc R . . H56B H 0.4873 0.6274 0.3600 0.085 Uiso 1 1 calc R . . H56C H 0.5649 0.5693 0.3766 0.085 Uiso 1 1 calc R . . C57A C 0.0076(4) 0.0094(3) 0.39269(12) 0.0412(9) Uani 1 1 d . . . H57A H 0.0323 0.0346 0.4212 0.049 Uiso 1 1 calc R . . H57B H -0.0363 -0.0560 0.3938 0.049 Uiso 1 1 calc R . . C58A C -0.0751(3) 0.0518(3) 0.37338(13) 0.0445(10) Uani 1 1 d . . . H58A H -0.1054 0.0231 0.3458 0.053 Uiso 1 1 calc R . . H58B H -0.1477 0.0449 0.3907 0.053 Uiso 1 1 calc R . . C59A C -0.0728(5) 0.1919(3) 0.35274(17) 0.0673(14) Uani 1 1 d . . . H59A H -0.1424 0.1889 0.3705 0.101 Uiso 1 1 calc R . . H59B H -0.1049 0.1657 0.3252 0.101 Uiso 1 1 calc R . . H59C H -0.0191 0.2545 0.3506 0.101 Uiso 1 1 calc R . . C60A C 0.1988(4) -0.0107(3) 0.38465(15) 0.0588(12) Uani 1 1 d . . . H60A H 0.1581 -0.0758 0.3847 0.088 Uiso 1 1 calc R . . H60B H 0.2232 0.0135 0.4130 0.088 Uiso 1 1 calc R . . H60C H 0.2728 0.0040 0.3678 0.088 Uiso 1 1 calc R . . P1B P -0.00822(9) 0.74925(7) 0.25193(3) 0.0366(2) Uani 1 1 d . . . P2B P 0.19115(9) 0.67598(6) 0.26979(3) 0.0388(2) Uani 1 1 d . . . P3B P 0.01146(9) 0.75755(7) -0.00089(4) 0.0432(3) Uani 1 1 d . . . P4B P 0.27983(9) 0.84772(7) -0.01172(4) 0.0463(3) Uani 1 1 d . . . Li1B Li 0.2048(6) 0.6507(5) 0.1283(2) 0.0456(16) Uani 1 1 d . . . Li2B Li 0.2852(6) 0.8865(4) 0.1301(2) 0.0459(16) Uani 1 1 d . . . O1B O 0.1913(3) 0.6915(2) 0.18245(9) 0.0510(7) Uani 1 1 d . A . O2B O 0.2198(3) 0.8368(2) 0.17984(10) 0.0674(10) Uani 1 1 d . A . O3B O 0.1607(3) 0.6877(2) 0.07926(10) 0.0635(9) Uani 1 1 d . A . O4B O 0.2489(3) 0.8365(2) 0.07653(10) 0.0598(9) Uani 1 1 d . A . O5B O 0.3770(3) 0.6397(2) 0.11993(10) 0.0573(8) Uani 1 1 d . A . O6B O 0.1533(4) 0.5139(2) 0.11928(13) 0.0811(12) Uani 1 1 d . A . O7B O 0.4740(3) 0.9419(3) 0.13483(11) 0.0766(11) Uani 1 1 d . . . O8B O 0.2976(3) 1.0164(2) 0.14366(9) 0.0556(8) Uani 1 1 d . . . C1B C 0.1600(3) 0.7671(3) 0.24306(13) 0.0393(9) Uani 1 1 d . A . C2B C 0.1942(4) 0.7654(3) 0.19771(13) 0.0455(10) Uani 1 1 d . . . C3B C -0.0915(3) 0.6735(2) 0.20879(12) 0.0395(9) Uani 1 1 d . . . C4B C -0.0769(4) 0.6881(3) 0.16747(14) 0.0507(10) Uani 1 1 d . . . H4BA H -0.0190 0.7429 0.1589 0.061 Uiso 1 1 calc R . . C5B C -0.1456(5) 0.6238(3) 0.13807(15) 0.0658(14) Uani 1 1 d . . . H5BA H -0.1352 0.6348 0.1096 0.079 Uiso 1 1 calc R . . C6B C -0.2287(6) 0.5443(4) 0.15023(19) 0.0817(18) Uani 1 1 d . . . H6BA H -0.2784 0.5010 0.1302 0.098 Uiso 1 1 calc R . . C7B C -0.2400(6) 0.5274(4) 0.1913(2) 0.0838(18) Uani 1 1 d . . . H7BA H -0.2937 0.4707 0.1995 0.101 Uiso 1 1 calc R . . C8B C -0.1743(5) 0.5917(3) 0.22083(16) 0.0629(13) Uani 1 1 d . . . H8BA H -0.1855 0.5803 0.2493 0.076 Uiso 1 1 calc R . . C9B C -0.0189(3) 0.8575(3) 0.24096(12) 0.0386(9) Uani 1 1 d . . . C10B C 0.0466(4) 0.9308(3) 0.26716(13) 0.0449(9) Uani 1 1 d . . . H10B H 0.1011 0.9239 0.2879 0.054 Uiso 1 1 calc R . . C11B C 0.0343(4) 1.0130(3) 0.26363(14) 0.0492(10) Uani 1 1 d . . . H11B H 0.0821 1.0623 0.2813 0.059 Uiso 1 1 calc R . . C12B C -0.0473(4) 1.0242(3) 0.23452(14) 0.0502(10) Uani 1 1 d . . . H12B H -0.0549 1.0810 0.2318 0.060 Uiso 1 1 calc R . . C13B C -0.1176(4) 0.9517(3) 0.20943(14) 0.0473(10) Uani 1 1 d . . . H13B H -0.1761 0.9582 0.1901 0.057 Uiso 1 1 calc R . . C14B C -0.1034(4) 0.8692(3) 0.21222(13) 0.0427(9) Uani 1 1 d . . . H14B H -0.1516 0.8201 0.1945 0.051 Uiso 1 1 calc R . . C15B C 0.2025(4) 0.7162(3) 0.32429(13) 0.0426(9) Uani 1 1 d . . . C16B C 0.0971(4) 0.6788(3) 0.34793(15) 0.0567(12) Uani 1 1 d . . . H16B H 0.0224 0.6387 0.3351 0.068 Uiso 1 1 calc R . . C17B C 0.1015(6) 0.7004(5) 0.39017(17) 0.0792(19) Uani 1 1 d . . . H17B H 0.0298 0.6745 0.4060 0.095 Uiso 1 1 calc R . . C18B C 0.2094(7) 0.7592(4) 0.40935(16) 0.0769(18) Uani 1 1 d . . . H18B H 0.2116 0.7748 0.4380 0.092 Uiso 1 1 calc R . . C19B C 0.3127(6) 0.7943(3) 0.38635(16) 0.0752(17) Uani 1 1 d . . . H19B H 0.3878 0.8330 0.3994 0.090 Uiso 1 1 calc R . . C20B C 0.3096(5) 0.7743(3) 0.34456(15) 0.0615(13) Uani 1 1 d . . . H20B H 0.3821 0.8008 0.3292 0.074 Uiso 1 1 calc R . . C21B C 0.3564(3) 0.7006(3) 0.26077(12) 0.0377(8) Uani 1 1 d . . . C22B C 0.4024(4) 0.6335(3) 0.26834(12) 0.0440(9) Uani 1 1 d . . . H22B H 0.3483 0.5778 0.2774 0.053 Uiso 1 1 calc R . . C23B C 0.5277(4) 0.6468(3) 0.26287(13) 0.0512(11) Uani 1 1 d . . . H23B H 0.5580 0.6000 0.2682 0.061 Uiso 1 1 calc R . . C24B C 0.6074(4) 0.7265(3) 0.24990(14) 0.0530(11) Uani 1 1 d . . . H24B H 0.6925 0.7350 0.2461 0.064 Uiso 1 1 calc R . . C25B C 0.5635(4) 0.7938(3) 0.24248(15) 0.0562(12) Uani 1 1 d . . . H25B H 0.6187 0.8495 0.2339 0.067 Uiso 1 1 calc R . . C26B C 0.4385(4) 0.7813(3) 0.24744(14) 0.0507(11) Uani 1 1 d . . . H26B H 0.4089 0.8283 0.2417 0.061 Uiso 1 1 calc R . . C27B C 0.1660(3) 0.7529(3) 0.01430(13) 0.0403(9) Uani 1 1 d . A . C28B C 0.1945(4) 0.7594(3) 0.06090(14) 0.0487(11) Uani 1 1 d . . . C29B C -0.1018(3) 0.6501(2) 0.01168(11) 0.0350(8) Uani 1 1 d . B . C30B C -0.2233(4) 0.6393(3) 0.00192(15) 0.0528(11) Uani 1 1 d . . . H30B H -0.2415 0.6872 -0.0096 0.063 Uiso 1 1 calc R B . C31B C -0.3196(4) 0.5600(3) 0.00855(19) 0.0735(16) Uani 1 1 d . B . H31B H -0.4030 0.5549 0.0026 0.088 Uiso 1 1 calc R . . C32B C -0.2953(5) 0.4885(3) 0.02363(16) 0.0646(14) Uani 1 1 d . . . H32B H -0.3612 0.4340 0.0280 0.077 Uiso 1 1 calc R B . C33B C -0.1753(5) 0.4970(3) 0.03223(14) 0.0578(12) Uani 1 1 d . B . H33B H -0.1575 0.4476 0.0421 0.069 Uiso 1 1 calc R . . C34B C -0.0785(4) 0.5773(3) 0.02666(13) 0.0494(10) Uani 1 1 d . . . H34B H 0.0045 0.5823 0.0332 0.059 Uiso 1 1 calc R B . C41B C 0.2510(3) 0.8065(3) -0.06607(14) 0.0465(10) Uani 1 1 d . B . C42B C 0.2958(4) 0.7439(3) -0.08408(15) 0.0579(12) Uani 1 1 d . . . H42B H 0.3434 0.7189 -0.0678 0.069 Uiso 1 1 calc R B . C43B C 0.2719(5) 0.7179(4) -0.12503(17) 0.0760(16) Uani 1 1 d . B . H43B H 0.3045 0.6760 -0.1371 0.091 Uiso 1 1 calc R . . C44B C 0.2002(5) 0.7527(4) -0.14891(17) 0.0824(19) Uani 1 1 d . . . H44B H 0.1819 0.7336 -0.1771 0.099 Uiso 1 1 calc R B . C45B C 0.1562(5) 0.8148(5) -0.1316(2) 0.0830(18) Uani 1 1 d . B . H45B H 0.1073 0.8388 -0.1478 0.100 Uiso 1 1 calc R . . C46B C 0.1826(4) 0.8425(4) -0.09049(17) 0.0641(13) Uani 1 1 d . . . H46B H 0.1535 0.8868 -0.0789 0.077 Uiso 1 1 calc R B . C47B C 0.4278(4) 0.8325(3) -0.00139(16) 0.0603(14) Uani 1 1 d . B . C48B C 0.4424(5) 0.7615(4) 0.01907(17) 0.0709(16) Uani 1 1 d . . . H48B H 0.3718 0.7137 0.0274 0.085 Uiso 1 1 calc R B . C49B C 0.5619(6) 0.7616(5) 0.0272(2) 0.103(3) Uani 1 1 d . B . H49B H 0.5723 0.7141 0.0416 0.124 Uiso 1 1 calc R . . C50B C 0.6652(6) 0.8298(6) 0.0145(3) 0.127(4) Uani 1 1 d . . . H50B H 0.7461 0.8290 0.0200 0.153 Uiso 1 1 calc R B . C51B C 0.6505(5) 0.8976(5) -0.0056(3) 0.120(3) Uani 1 1 d . B . H51B H 0.7216 0.9443 -0.0145 0.144 Uiso 1 1 calc R . . C52B C 0.5326(4) 0.9004(4) -0.0135(2) 0.083(2) Uani 1 1 d . . . H52B H 0.5242 0.9492 -0.0274 0.099 Uiso 1 1 calc R B . C53B C 0.2476(5) 0.4945(3) 0.09918(16) 0.0657(14) Uani 1 1 d . . . H53C H 0.2456 0.5071 0.0696 0.079 Uiso 0.660(9) 1 calc PR A 1 H53D H 0.2352 0.4304 0.1012 0.079 Uiso 0.660(9) 1 calc PR A 1 H53E H 0.2840 0.4631 0.1183 0.079 Uiso 0.340(9) 1 d PR A 2 H53F H 0.2099 0.4526 0.0753 0.079 Uiso 0.340(9) 1 d PR A 2 C54B C 0.3745(7) 0.5526(5) 0.1192(3) 0.064(2) Uiso 0.660(9) 1 d P A 1 H54C H 0.3826 0.5342 0.1476 0.077 Uiso 0.660(9) 1 calc PR A 1 H54D H 0.4433 0.5465 0.1028 0.077 Uiso 0.660(9) 1 calc PR A 1 C55B C 0.4820(9) 0.6962(8) 0.1473(3) 0.089(3) Uiso 0.660(9) 1 d P A 1 H55D H 0.5575 0.6845 0.1401 0.133 Uiso 0.660(9) 1 calc PR A 1 H55E H 0.4627 0.6819 0.1761 0.133 Uiso 0.660(9) 1 calc PR A 1 H55F H 0.4951 0.7594 0.1438 0.133 Uiso 0.660(9) 1 calc PR A 1 C54C C 0.3404(14) 0.5643(10) 0.0855(5) 0.059(4) Uiso 0.340(9) 1 d P A 2 H54E H 0.3131 0.5854 0.0602 0.071 Uiso 0.340(9) 1 calc PR A 2 H54F H 0.4125 0.5466 0.0789 0.071 Uiso 0.340(9) 1 calc PR A 2 C55C C 0.4390(15) 0.6225(12) 0.1506(5) 0.069(5) Uiso 0.340(9) 1 d P A 2 H55G H 0.5175 0.6194 0.1407 0.104 Uiso 0.340(9) 1 calc PR A 2 H55H H 0.3896 0.5652 0.1618 0.104 Uiso 0.340(9) 1 calc PR A 2 H55I H 0.4562 0.6702 0.1723 0.104 Uiso 0.340(9) 1 calc PR A 2 C56B C 0.0366(5) 0.4520(4) 0.1140(2) 0.0815(17) Uani 1 1 d . . . H56D H 0.0414 0.3922 0.1104 0.122 Uiso 1 1 calc R A . H56E H -0.0036 0.4649 0.0895 0.122 Uiso 1 1 calc R . . H56F H -0.0120 0.4545 0.1383 0.122 Uiso 1 1 calc R . . C57B C 0.5074(9) 1.0335(6) 0.1413(3) 0.136(3) Uiso 1 1 d . . . H57C H 0.5845 1.0561 0.1587 0.163 Uiso 1 1 calc R . . H57D H 0.5259 1.0616 0.1144 0.163 Uiso 1 1 calc R . . C58B C 0.4183(8) 1.0594(6) 0.1599(3) 0.124(3) Uiso 1 1 d . . . H58C H 0.4408 1.1247 0.1575 0.149 Uiso 1 1 calc R . . H58D H 0.4191 1.0480 0.1896 0.149 Uiso 1 1 calc R . . C59B C 0.2142(5) 1.0316(4) 0.17305(19) 0.0794(17) Uani 1 1 d . . . H59D H 0.2117 1.0918 0.1704 0.119 Uiso 1 1 calc R . . H59E H 0.2432 1.0262 0.2010 0.119 Uiso 1 1 calc R . . H59F H 0.1308 0.9872 0.1678 0.119 Uiso 1 1 calc R . . C60B C 0.5556(7) 0.9230(5) 0.1081(2) 0.111(2) Uiso 1 1 d . . . H60D H 0.6408 0.9515 0.1191 0.167 Uiso 1 1 calc R . . H60E H 0.5482 0.9459 0.0810 0.167 Uiso 1 1 calc R . . H60F H 0.5354 0.8581 0.1053 0.167 Uiso 1 1 calc R . . C35B C -0.0063(5) 0.8384(3) 0.03007(14) 0.0315(15) Uiso 0.50 1 d PG B 1 C36B C 0.0078(5) 0.9220(3) 0.01569(12) 0.0406(17) Uiso 0.50 1 d PG B 1 H36B H 0.0272 0.9341 -0.0123 0.049 Uiso 0.50 1 calc PR B 1 C37B C -0.0063(5) 0.9879(3) 0.04228(15) 0.049(2) Uiso 0.50 1 d PG B 1 H37B H 0.0033 1.0451 0.0325 0.059 Uiso 0.50 1 calc PR B 1 C38B C -0.0347(6) 0.9702(3) 0.08326(14) 0.051(2) Uiso 0.50 1 d PG B 1 H38B H -0.0444 1.0153 0.1014 0.061 Uiso 0.50 1 calc PR B 1 C39B C -0.0488(6) 0.8866(4) 0.09765(12) 0.058(2) Uiso 0.50 1 d PG B 1 H39B H -0.0682 0.8745 0.1257 0.070 Uiso 0.50 1 calc PR B 1 C40B C -0.0347(5) 0.8207(3) 0.07105(15) 0.0441(19) Uiso 0.50 1 d PG B 1 H40B H -0.0443 0.7635 0.0809 0.053 Uiso 0.50 1 calc PR B 1 C35C C -0.0184(4) 0.8291(3) 0.04736(14) 0.0256(13) Uiso 0.50 1 d PG B 2 C36C C -0.1187(4) 0.7999(2) 0.07323(14) 0.0326(15) Uiso 0.50 1 d PG B 2 H36C H -0.1729 0.7392 0.0713 0.039 Uiso 0.50 1 calc PR B 2 C37C C -0.1398(4) 0.8595(3) 0.10195(14) 0.0420(18) Uiso 0.50 1 d PG B 2 H37C H -0.2084 0.8396 0.1196 0.050 Uiso 0.50 1 calc PR B 2 C38C C -0.0606(5) 0.9484(3) 0.10480(15) 0.050(2) Uiso 0.50 1 d PG B 2 H38C H -0.0750 0.9891 0.1244 0.060 Uiso 0.50 1 calc PR B 2 C39C C 0.0397(5) 0.9776(2) 0.07893(18) 0.060(2) Uiso 0.50 1 d PG B 2 H39C H 0.0938 1.0383 0.0809 0.072 Uiso 0.50 1 calc PR B 2 C40C C 0.0608(4) 0.9179(3) 0.05021(15) 0.049(2) Uiso 0.50 1 d PG B 2 H40C H 0.1293 0.9379 0.0325 0.059 Uiso 0.50 1 calc PR B 2 H1A H 0.333(3) 0.315(2) 0.4981(10) 0.024(8) Uiso 1 1 d . . . H1B H 0.206(4) 0.824(3) 0.2579(14) 0.062(14) Uiso 1 1 d . . . H27A H 0.283(4) 0.224(3) 0.2435(12) 0.041(11) Uiso 1 1 d . . . H27B H 0.167(4) 0.695(3) 0.0033(12) 0.047(11) 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 P1A 0.0182(4) 0.0223(4) 0.0284(4) 0.0026(3) 0.0006(3) 0.0074(3) P2A 0.0176(4) 0.0287(4) 0.0239(4) 0.0022(3) -0.0005(3) 0.0075(3) P3A 0.0307(4) 0.0295(5) 0.0294(4) 0.0042(4) 0.0010(3) 0.0108(4) P4A 0.0282(4) 0.0295(5) 0.0261(4) 0.0002(3) 0.0015(3) 0.0109(4) Li1A 0.041(3) 0.024(3) 0.024(3) 0.002(2) -0.002(2) 0.010(2) Li2A 0.030(3) 0.031(3) 0.028(3) 0.002(2) -0.001(2) 0.001(2) O1A 0.0456(15) 0.0312(14) 0.0326(13) 0.0080(10) -0.0051(11) 0.0124(12) O2A 0.0322(12) 0.0320(14) 0.0288(12) -0.0038(10) -0.0057(10) 0.0098(10) O3A 0.0379(13) 0.0329(14) 0.0284(12) -0.0034(10) 0.0020(10) 0.0123(11) O4A 0.0359(13) 0.0379(15) 0.0291(12) 0.0079(10) 0.0050(10) 0.0094(11) O5A 0.0385(14) 0.0255(13) 0.0475(15) 0.0008(11) 0.0048(11) 0.0069(11) O6A 0.0402(14) 0.0307(14) 0.0405(14) 0.0005(11) -0.0004(11) 0.0128(11) O7A 0.0293(13) 0.0381(15) 0.0535(16) 0.0103(12) 0.0000(11) 0.0058(11) O8A 0.0341(13) 0.0323(14) 0.0374(14) 0.0014(11) -0.0015(10) 0.0072(11) C1A 0.0196(15) 0.0247(17) 0.0240(15) 0.0005(12) 0.0020(12) 0.0070(13) C2A 0.0173(14) 0.0321(18) 0.0253(15) 0.0013(13) -0.0016(12) 0.0102(13) C3A 0.0186(14) 0.0248(16) 0.0273(16) -0.0024(12) -0.0002(12) 0.0076(12) C4A 0.0219(16) 0.035(2) 0.049(2) 0.0101(16) 0.0030(15) 0.0106(15) C5A 0.035(2) 0.049(2) 0.052(2) 0.0097(19) 0.0005(17) 0.0254(18) C6A 0.0232(18) 0.056(3) 0.057(2) -0.010(2) -0.0061(16) 0.0201(18) C7A 0.0199(16) 0.039(2) 0.057(2) -0.0058(18) 0.0017(16) 0.0039(15) C8A 0.0246(16) 0.0305(19) 0.0402(19) 0.0021(15) 0.0037(14) 0.0079(14) C9A 0.0174(14) 0.0236(16) 0.0304(16) 0.0067(13) 0.0026(12) 0.0018(12) C10A 0.0317(18) 0.0299(19) 0.0356(19) 0.0014(14) -0.0022(14) 0.0089(15) C11A 0.042(2) 0.045(2) 0.041(2) -0.0104(18) 0.0026(17) 0.0132(18) C12A 0.044(2) 0.053(3) 0.0257(18) -0.0013(17) -0.0051(16) 0.0033(19) C13A 0.0323(19) 0.055(3) 0.036(2) 0.0158(18) -0.0068(16) 0.0081(18) C14A 0.0256(17) 0.040(2) 0.0364(19) 0.0107(15) 0.0013(14) 0.0101(15) C15A 0.0218(15) 0.0289(18) 0.0245(15) -0.0018(13) 0.0018(12) 0.0052(13) C16A 0.0246(17) 0.034(2) 0.0396(19) -0.0047(15) -0.0018(14) 0.0067(15) C17A 0.0221(17) 0.047(2) 0.046(2) -0.0097(18) -0.0005(15) 0.0003(16) C18A 0.039(2) 0.035(2) 0.044(2) -0.0077(17) 0.0067(17) -0.0073(17) C19A 0.049(2) 0.029(2) 0.043(2) -0.0020(16) 0.0042(18) 0.0080(17) C20A 0.0336(18) 0.0295(19) 0.0350(19) -0.0023(14) 0.0009(15) 0.0078(15) C21A 0.0145(14) 0.0265(17) 0.0331(17) 0.0026(13) -0.0035(12) 0.0090(12) C22A 0.0312(18) 0.0302(19) 0.0346(18) 0.0045(14) -0.0036(14) 0.0106(15) C23A 0.051(2) 0.030(2) 0.044(2) 0.0000(16) -0.0079(18) 0.0186(18) C24A 0.045(2) 0.036(2) 0.047(2) -0.0117(17) -0.0053(17) 0.0223(18) C25A 0.041(2) 0.043(2) 0.0346(19) 0.0022(16) 0.0055(16) 0.0191(18) C26A 0.0319(18) 0.0314(19) 0.0334(18) 0.0034(14) 0.0055(14) 0.0139(15) C27A 0.0287(17) 0.0270(18) 0.0238(16) 0.0007(13) 0.0005(13) 0.0093(14) C28A 0.0234(15) 0.0325(19) 0.0260(16) 0.0024(13) -0.0014(12) 0.0127(14) C29A 0.0319(18) 0.0282(18) 0.0287(17) -0.0037(13) -0.0048(13) 0.0109(14) C30A 0.043(2) 0.035(2) 0.050(2) -0.0094(17) -0.0113(17) 0.0155(17) C31A 0.050(3) 0.048(3) 0.080(3) -0.022(2) -0.023(2) 0.030(2) C32A 0.040(2) 0.080(4) 0.052(3) -0.016(2) -0.0079(19) 0.030(2) C33A 0.0281(19) 0.064(3) 0.047(2) 0.007(2) -0.0077(17) 0.0037(19) C34A 0.0347(19) 0.039(2) 0.040(2) 0.0029(16) -0.0082(15) 0.0120(16) C35A 0.065(3) 0.061(3) 0.0281(19) 0.0131(18) 0.0072(18) 0.043(2) C36A 0.078(4) 0.225(8) 0.037(3) 0.023(4) 0.013(2) 0.098(5) C37A 0.154(7) 0.375(15) 0.040(3) 0.034(6) 0.030(4) 0.204(10) C38A 0.245(11) 0.188(8) 0.034(3) -0.006(4) -0.001(5) 0.186(9) C39A 0.180(7) 0.061(4) 0.042(3) -0.015(2) -0.011(4) 0.045(4) C40A 0.106(4) 0.049(3) 0.035(2) -0.006(2) 0.002(2) 0.014(3) C41A 0.0288(17) 0.0318(19) 0.0395(19) -0.0060(15) -0.0087(14) 0.0111(15) C42A 0.040(2) 0.032(2) 0.041(2) -0.0032(15) -0.0008(16) 0.0146(16) C43A 0.062(3) 0.032(2) 0.050(2) -0.0030(17) -0.003(2) 0.014(2) C44A 0.070(3) 0.034(2) 0.069(3) -0.008(2) -0.019(2) 0.026(2) C45A 0.045(3) 0.050(3) 0.113(4) -0.005(3) -0.011(3) 0.028(2) C46A 0.032(2) 0.040(2) 0.098(4) 0.000(2) 0.000(2) 0.0139(18) C47A 0.0260(16) 0.0275(18) 0.0307(17) 0.0011(14) 0.0048(13) 0.0042(14) C48A 0.079(4) 0.042(3) 0.076(3) -0.003(2) -0.037(3) 0.013(2) C49A 0.075(3) 0.038(3) 0.080(4) -0.009(2) -0.030(3) 0.005(2) C50A 0.048(2) 0.050(3) 0.037(2) -0.0063(18) -0.0001(18) -0.010(2) C51A 0.162(7) 0.070(4) 0.057(3) 0.026(3) -0.058(4) -0.041(4) C52A 0.159(6) 0.042(3) 0.061(3) 0.017(2) -0.059(4) -0.024(3) C53A 0.056(2) 0.032(2) 0.037(2) -0.0085(16) -0.0015(17) 0.0204(18) C54A 0.046(2) 0.047(2) 0.036(2) -0.0018(17) 0.0080(17) 0.0219(19) C55A 0.052(2) 0.052(3) 0.054(3) -0.007(2) -0.016(2) 0.024(2) C56A 0.044(2) 0.045(3) 0.069(3) 0.009(2) -0.003(2) 0.001(2) C57A 0.040(2) 0.031(2) 0.046(2) 0.0098(16) 0.0091(17) 0.0037(16) C58A 0.0295(19) 0.038(2) 0.056(2) 0.0062(18) 0.0052(17) -0.0011(16) C59A 0.055(3) 0.060(3) 0.088(4) 0.024(3) -0.014(3) 0.021(2) C60A 0.058(3) 0.054(3) 0.070(3) 0.008(2) -0.003(2) 0.027(2) P1B 0.0318(5) 0.0336(5) 0.0453(5) 0.0037(4) 0.0128(4) 0.0120(4) P2B 0.0328(5) 0.0269(5) 0.0567(6) -0.0021(4) 0.0100(4) 0.0106(4) P3B 0.0259(5) 0.0352(6) 0.0678(7) 0.0043(5) -0.0153(5) 0.0103(4) P4B 0.0247(5) 0.0375(6) 0.0749(8) -0.0204(5) -0.0088(5) 0.0117(4) Li1B 0.047(4) 0.038(4) 0.055(4) -0.008(3) -0.002(3) 0.020(3) Li2B 0.037(3) 0.035(4) 0.057(4) -0.004(3) 0.010(3) 0.001(3) O1B 0.0470(17) 0.0533(19) 0.0576(18) -0.0047(14) 0.0106(14) 0.0242(14) O2B 0.078(2) 0.047(2) 0.070(2) 0.0131(16) 0.0386(18) 0.0099(17) O3B 0.079(2) 0.063(2) 0.0564(19) -0.0141(16) -0.0274(17) 0.0375(19) O4B 0.0379(16) 0.065(2) 0.071(2) -0.0383(17) -0.0116(14) 0.0165(15) O5B 0.0569(19) 0.064(2) 0.0573(19) -0.0001(15) -0.0009(15) 0.0293(17) O6B 0.075(2) 0.042(2) 0.117(3) -0.0079(19) 0.041(2) 0.0093(18) O7B 0.0432(18) 0.107(3) 0.069(2) -0.038(2) 0.0050(16) 0.0175(19) O8B 0.067(2) 0.0446(18) 0.0486(17) -0.0063(13) -0.0040(15) 0.0124(15) C1B 0.0334(19) 0.032(2) 0.051(2) -0.0016(17) 0.0126(17) 0.0104(16) C2B 0.034(2) 0.042(2) 0.059(3) -0.001(2) 0.0177(18) 0.0123(18) C3B 0.0339(19) 0.029(2) 0.054(2) -0.0012(16) 0.0125(17) 0.0090(16) C4B 0.051(3) 0.035(2) 0.062(3) 0.0013(19) 0.010(2) 0.0108(19) C5B 0.088(4) 0.048(3) 0.055(3) -0.007(2) 0.013(3) 0.018(3) C6B 0.095(4) 0.044(3) 0.081(4) -0.024(3) 0.005(3) -0.003(3) C7B 0.085(4) 0.043(3) 0.097(5) -0.003(3) 0.007(3) -0.009(3) C8B 0.061(3) 0.042(3) 0.071(3) 0.000(2) 0.013(2) 0.000(2) C9B 0.0347(19) 0.038(2) 0.045(2) -0.0008(16) 0.0125(16) 0.0140(17) C10B 0.041(2) 0.046(2) 0.050(2) -0.0092(19) 0.0007(18) 0.0197(19) C11B 0.042(2) 0.038(2) 0.066(3) -0.017(2) 0.000(2) 0.0147(19) C12B 0.049(2) 0.040(2) 0.067(3) -0.005(2) 0.006(2) 0.023(2) C13B 0.043(2) 0.045(2) 0.058(3) -0.0033(19) 0.0007(19) 0.0218(19) C14B 0.037(2) 0.036(2) 0.052(2) -0.0053(18) 0.0056(17) 0.0101(17) C15B 0.053(2) 0.033(2) 0.051(2) 0.0076(17) 0.0154(19) 0.0246(19) C16B 0.050(3) 0.076(3) 0.063(3) 0.023(2) 0.019(2) 0.043(2) C17B 0.092(4) 0.129(5) 0.059(3) 0.036(3) 0.035(3) 0.087(4) C18B 0.139(6) 0.080(4) 0.047(3) 0.006(3) 0.013(3) 0.081(4) C19B 0.127(5) 0.036(3) 0.057(3) -0.010(2) 0.009(3) 0.024(3) C20B 0.085(4) 0.032(2) 0.057(3) -0.003(2) 0.013(2) 0.006(2) C21B 0.0307(18) 0.035(2) 0.048(2) -0.0079(16) 0.0048(16) 0.0124(16) C22B 0.042(2) 0.042(2) 0.047(2) -0.0062(18) -0.0039(18) 0.0146(18) C23B 0.049(2) 0.064(3) 0.053(3) -0.009(2) -0.012(2) 0.037(2) C24B 0.037(2) 0.062(3) 0.058(3) -0.009(2) 0.0003(19) 0.016(2) C25B 0.033(2) 0.050(3) 0.080(3) -0.006(2) 0.011(2) 0.008(2) C26B 0.037(2) 0.037(2) 0.077(3) -0.003(2) 0.014(2) 0.0107(18) C27B 0.0309(19) 0.039(2) 0.054(2) -0.0137(18) -0.0173(17) 0.0179(17) C28B 0.034(2) 0.061(3) 0.058(3) -0.027(2) -0.0187(18) 0.028(2) C29B 0.0382(19) 0.035(2) 0.0310(18) -0.0063(15) -0.0075(15) 0.0130(16) C30B 0.040(2) 0.042(3) 0.074(3) -0.005(2) -0.002(2) 0.0116(19) C31B 0.038(2) 0.051(3) 0.122(5) -0.003(3) 0.011(3) 0.004(2) C32B 0.065(3) 0.037(3) 0.075(3) -0.008(2) 0.020(3) -0.002(2) C33B 0.088(4) 0.033(2) 0.048(3) 0.0016(19) 0.004(2) 0.017(2) C34B 0.061(3) 0.040(2) 0.048(2) -0.0013(18) -0.010(2) 0.019(2) C41B 0.0252(18) 0.041(2) 0.066(3) -0.0048(19) -0.0049(18) 0.0029(16) C42B 0.052(3) 0.053(3) 0.063(3) -0.017(2) -0.012(2) 0.013(2) C43B 0.072(4) 0.071(4) 0.069(3) -0.024(3) -0.008(3) 0.008(3) C44B 0.062(3) 0.092(5) 0.053(3) -0.008(3) -0.013(3) -0.021(3) C45B 0.046(3) 0.108(5) 0.083(4) 0.014(4) -0.010(3) 0.011(3) C46B 0.037(2) 0.071(3) 0.081(4) 0.005(3) -0.006(2) 0.014(2) C47B 0.027(2) 0.064(3) 0.085(3) -0.050(3) -0.018(2) 0.017(2) C48B 0.053(3) 0.091(4) 0.083(4) -0.040(3) -0.028(3) 0.048(3) C49B 0.076(4) 0.146(6) 0.116(5) -0.078(5) -0.051(4) 0.085(5) C50B 0.051(4) 0.156(7) 0.186(8) -0.128(7) -0.054(4) 0.068(5) C51B 0.029(3) 0.103(5) 0.211(9) -0.108(6) -0.008(4) 0.014(3) C52B 0.033(2) 0.064(3) 0.140(5) -0.062(3) -0.006(3) 0.011(2) C53B 0.096(4) 0.050(3) 0.066(3) 0.002(2) 0.020(3) 0.043(3) C56B 0.072(4) 0.070(4) 0.100(4) -0.001(3) -0.025(3) 0.024(3) C59B 0.080(4) 0.070(4) 0.097(4) -0.020(3) 0.001(3) 0.040(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1A C3A 1.833(3) . ? P1A C9A 1.840(3) . ? P1A C1A 1.871(3) . ? P2A C21A 1.833(3) . ? P2A C15A 1.837(3) . ? P2A C1A 1.870(3) . ? P3A C29A 1.832(3) . ? P3A C35A 1.852(4) . ? P3A C27A 1.871(3) . ? P4A C41A 1.834(4) . ? P4A C47A 1.839(3) . ? P4A C27A 1.873(3) . ? Li1A O1A 1.867(6) . ? Li1A O3A 1.894(6) . ? Li1A O5A 2.052(6) . ? Li1A O6A 2.068(6) . ? Li1A C54A 2.740(7) . ? Li1A Li2A 3.463(8) . ? Li2A O2A 1.869(6) . ? Li2A O4A 1.865(6) . ? Li2A O7A 2.019(6) . ? Li2A O8A 2.043(6) . ? Li2A C57A 2.741(7) . ? O1A C2A 1.256(4) . ? O2A C2A 1.240(4) . ? O3A C28A 1.246(4) . ? O4A C28A 1.255(4) . ? O5A C56A 1.422(5) . ? O5A C53A 1.425(4) . ? O6A C55A 1.425(5) . ? O6A C54A 1.429(4) . ? O7A C59A 1.410(5) . ? O7A C58A 1.418(4) . ? O8A C60A 1.424(5) . ? O8A C57A 1.433(4) . ? C1A C2A 1.533(4) . ? C1A H1A 0.99(3) . ? C3A C4A 1.393(5) . ? C3A C8A 1.394(4) . ? C4A C5A 1.384(5) . ? C4A H4AA 0.9500 . ? C5A C6A 1.379(6) . ? C5A H5AA 0.9500 . ? C6A C7A 1.375(6) . ? C6A H6AA 0.9500 . ? C7A C8A 1.385(5) . ? C7A H7AA 0.9500 . ? C8A H8AA 0.9500 . ? C9A C14A 1.395(5) . ? C9A C10A 1.396(5) . ? C10A C11A 1.382(5) . ? C10A H10A 0.9500 . ? C11A C12A 1.378(6) . ? C11A H11A 0.9500 . ? C12A C13A 1.366(6) . ? C12A H12A 0.9500 . ? C13A C14A 1.392(5) . ? C13A H13A 0.9500 . ? C14A H14A 0.9500 . ? C15A C20A 1.392(5) . ? C15A C16A 1.398(4) . ? C16A C17A 1.383(5) . ? C16A H16A 0.9500 . ? C17A C18A 1.379(6) . ? C17A H17A 0.9500 . ? C18A C19A 1.378(6) . ? C18A H18A 0.9500 . ? C19A C20A 1.395(5) . ? C19A H19A 0.9500 . ? C20A H20A 0.9500 . ? C21A C26A 1.386(5) . ? C21A C22A 1.392(5) . ? C22A C23A 1.390(5) . ? C22A H22A 0.9500 . ? C23A C24A 1.371(5) . ? C23A H23A 0.9500 . ? C24A C25A 1.385(5) . ? C24A H24A 0.9500 . ? C25A C26A 1.383(5) . ? C25A H25A 0.9500 . ? C26A H26A 0.9500 . ? C27A C28A 1.534(4) . ? C27A H27A 0.99(4) . ? C29A C30A 1.387(5) . ? C29A C34A 1.396(5) . ? C30A C31A 1.386(6) . ? C30A H30A 0.9500 . ? C31A C32A 1.359(7) . ? C31A H31A 0.9500 . ? C32A C33A 1.373(6) . ? C32A H32A 0.9500 . ? C33A C34A 1.385(5) . ? C33A H33A 0.9500 . ? C34A H34A 0.9500 . ? C35A C36A 1.365(6) . ? C35A C40A 1.377(7) . ? C36A C37A 1.405(9) . ? C36A H36A 0.9500 . ? C37A C38A 1.362(13) . ? C37A H37A 0.9500 . ? C38A C39A 1.372(11) . ? C38A H38A 0.9500 . ? C39A C40A 1.385(6) . ? C39A H39A 0.9500 . ? C40A H40A 0.9500 . ? C41A C46A 1.392(5) . ? C41A C42A 1.388(5) . ? C42A C43A 1.393(5) . ? C42A H42A 0.9500 . ? C43A C44A 1.371(6) . ? C43A H43A 0.9500 . ? C44A C45A 1.364(7) . ? C44A H44A 0.9500 . ? C45A C46A 1.384(6) . ? C45A H45A 0.9500 . ? C46A H46A 0.9500 . ? C47A C48A 1.347(6) . ? C47A C52A 1.357(6) . ? C48A C49A 1.391(6) . ? C48A H48A 0.9500 . ? C49A C50A 1.335(7) . ? C49A H49A 0.9500 . ? C50A C51A 1.347(7) . ? C50A H50A 0.9500 . ? C51A C52A 1.384(7) . ? C51A H51A 0.9500 . ? C52A H52A 0.9500 . ? C53A C54A 1.491(5) . ? C53A H53A 0.9900 . ? C53A H53B 0.9900 . ? C54A H54A 0.9900 . ? C54A H54B 0.9900 . ? C55A H55A 0.9800 . ? C55A H55B 0.9800 . ? C55A H55C 0.9800 . ? C56A H56A 0.9800 . ? C56A H56B 0.9800 . ? C56A H56C 0.9800 . ? C57A C58A 1.494(6) . ? C57A H57A 0.9900 . ? C57A H57B 0.9900 . ? C58A H58A 0.9900 . ? C58A H58B 0.9900 . ? C59A H59A 0.9800 . ? C59A H59B 0.9800 . ? C59A H59C 0.9800 . ? C60A H60A 0.9800 . ? C60A H60B 0.9800 . ? C60A H60C 0.9800 . ? P1B C9B 1.827(4) . ? P1B C3B 1.831(4) . ? P1B C1B 1.882(4) . ? P2B C21B 1.831(4) . ? P2B C15B 1.843(4) . ? P2B C1B 1.862(4) . ? P3B C35B 1.675(4) . ? P3B C29B 1.820(4) . ? P3B C27B 1.866(4) . ? P3B C35C 2.005(4) . ? P4B C47B 1.831(4) . ? P4B C41B 1.841(4) . ? P4B C27B 1.861(4) . ? Li1B O3B 1.847(8) . ? Li1B O1B 1.875(7) . ? Li1B O6B 2.062(8) . ? Li1B O5B 2.071(7) . ? Li1B C54C 2.773(16) . ? Li2B O4B 1.862(8) . ? Li2B O2B 1.876(7) . ? Li2B O7B 2.038(7) . ? Li2B O8B 2.060(8) . ? Li2B C58B 2.772(11) . ? O1B C2B 1.251(5) . ? O2B C2B 1.244(5) . ? O3B C28B 1.253(6) . ? O4B C28B 1.252(5) . ? O5B C55C 1.310(16) . ? O5B C54B 1.382(8) . ? O5B C55B 1.484(10) . ? O5B C54C 1.548(15) . ? O6B C56B 1.363(6) . ? O6B C53B 1.392(6) . ? O7B C60B 1.387(8) . ? O7B C57B 1.382(9) . ? O8B C58B 1.400(9) . ? O8B C59B 1.434(6) . ? C1B C2B 1.530(6) . ? C1B H1B 0.98(5) . ? C3B C4B 1.373(6) . ? C3B C8B 1.395(6) . ? C4B C5B 1.385(6) . ? C4B H4BA 0.9500 . ? C5B C6B 1.372(7) . ? C5B H5BA 0.9500 . ? C6B C7B 1.368(8) . ? C6B H6BA 0.9500 . ? C7B C8B 1.379(7) . ? C7B H7BA 0.9500 . ? C8B H8BA 0.9500 . ? C9B C10B 1.394(5) . ? C9B C14B 1.403(6) . ? C10B C11B 1.381(6) . ? C10B H10B 0.9500 . ? C11B C12B 1.383(6) . ? C11B H11B 0.9500 . ? C12B C13B 1.380(6) . ? C12B H12B 0.9500 . ? C13B C14B 1.391(6) . ? C13B H13B 0.9500 . ? C14B H14B 0.9500 . ? C15B C20B 1.392(6) . ? C15B C16B 1.403(6) . ? C16B C17B 1.396(7) . ? C16B H16B 0.9500 . ? C17B C18B 1.386(9) . ? C17B H17B 0.9500 . ? C18B C19B 1.369(8) . ? C18B H18B 0.9500 . ? C19B C20B 1.377(7) . ? C19B H19B 0.9500 . ? C20B H20B 0.9500 . ? C21B C22B 1.382(5) . ? C21B C26B 1.395(5) . ? C22B C23B 1.396(6) . ? C22B H22B 0.9500 . ? C23B C24B 1.369(6) . ? C23B H23B 0.9500 . ? C24B C25B 1.368(6) . ? C24B H24B 0.9500 . ? C25B C26B 1.393(5) . ? C25B H25B 0.9500 . ? C26B H26B 0.9500 . ? C27B C28B 1.535(6) . ? C27B H27B 0.98(4) . ? C29B C30B 1.378(5) . ? C29B C34B 1.388(5) . ? C30B C31B 1.386(6) . ? C30B H30B 0.9500 . ? C31B C32B 1.375(7) . ? C31B H31B 0.9500 . ? C32B C33B 1.363(7) . ? C32B H32B 0.9500 . ? C33B C34B 1.392(6) . ? C33B H33B 0.9500 . ? C34B H34B 0.9500 . ? C41B C46B 1.386(6) . ? C41B C42B 1.389(6) . ? C42B C43B 1.370(7) . ? C42B H42B 0.9500 . ? C43B C44B 1.391(9) . ? C43B H43B 0.9500 . ? C44B C45B 1.368(9) . ? C44B H44B 0.9500 . ? C45B C46B 1.382(8) . ? C45B H45B 0.9500 . ? C46B H46B 0.9500 . ? C47B C48B 1.397(8) . ? C47B C52B 1.384(7) . ? C48B C49B 1.396(6) . ? C48B H48B 0.9500 . ? C49B C50B 1.381(11) . ? C49B H49B 0.9500 . ? C50B C51B 1.347(12) . ? C50B H50B 0.9500 . ? C51B C52B 1.394(8) . ? C51B H51B 0.9500 . ? C52B H52B 0.9500 . ? C53B C54C 1.340(15) . ? C53B C54B 1.545(9) . ? C53B H53C 0.9900 . ? C53B H53D 0.9900 . ? C53B H53E 0.9898 . ? C53B H53F 0.9902 . ? C54B H53E 1.4422 . ? C54B H54C 0.9900 . ? C54B H54D 0.9900 . ? C55B H55D 0.9800 . ? C55B H55E 0.9800 . ? C55B H55F 0.9800 . ? C54C H54E 0.9900 . ? C54C H54F 0.9900 . ? C55C H55G 0.9800 . ? C55C H55H 0.9800 . ? C55C H55I 0.9800 . ? C56B H56D 0.9800 . ? C56B H56E 0.9800 . ? C56B H56F 0.9800 . ? C57B C58B 1.372(10) . ? C57B H57C 0.9900 . ? C57B H57D 0.9900 . ? C58B H58C 0.9900 . ? C58B H58D 0.9900 . ? C59B H59D 0.9800 . ? C59B H59E 0.9800 . ? C59B H59F 0.9800 . ? C60B H60D 0.9800 . ? C60B H60E 0.9800 . ? C60B H60F 0.9800 . ? C35B C36B 1.3900 . ? C35B C40B 1.3900 . ? C36B C37B 1.3900 . ? C36B H36B 0.9500 . ? C37B C38B 1.3900 . ? C37B H37B 0.9500 . ? C38B C39B 1.3900 . ? C38B H38B 0.9500 . ? C39B C40B 1.3900 . ? C39B H39B 0.9500 . ? C40B H40B 0.9500 . ? C35C C36C 1.3900 . ? C35C C40C 1.3900 . ? C36C C37C 1.3900 . ? C36C H36C 0.9500 . ? C37C C38C 1.3900 . ? C37C H37C 0.9500 . ? C38C C39C 1.3900 . ? C38C H38C 0.9500 . ? C39C C40C 1.3900 . ? C39C H39C 0.9500 . ? C40C H40C 0.9500 . ? 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 C3A P1A C9A 100.34(14) . . ? C3A P1A C1A 102.89(14) . . ? C9A P1A C1A 102.13(14) . . ? C21A P2A C15A 101.77(14) . . ? C21A P2A C1A 102.91(14) . . ? C15A P2A C1A 105.36(15) . . ? C29A P3A C35A 99.60(17) . . ? C29A P3A C27A 102.98(15) . . ? C35A P3A C27A 100.06(16) . . ? C41A P4A C47A 101.53(16) . . ? C41A P4A C27A 105.65(16) . . ? C47A P4A C27A 105.23(15) . . ? O1A Li1A O3A 129.5(3) . . ? O1A Li1A O5A 102.1(3) . . ? O3A Li1A O5A 118.4(3) . . ? O1A Li1A O6A 105.7(3) . . ? O3A Li1A O6A 108.5(3) . . ? O5A Li1A O6A 81.9(2) . . ? O1A Li1A C54A 93.1(2) . . ? O3A Li1A C54A 133.5(3) . . ? O5A Li1A C54A 56.53(17) . . ? O6A Li1A C54A 30.72(13) . . ? O1A Li1A Li2A 65.8(2) . . ? O3A Li1A Li2A 75.3(2) . . ? O5A Li1A Li2A 166.2(3) . . ? O6A Li1A Li2A 94.7(2) . . ? C54A Li1A Li2A 115.5(2) . . ? O2A Li2A O4A 126.2(3) . . ? O2A Li2A O7A 112.4(3) . . ? O4A Li2A O7A 111.8(3) . . ? O2A Li2A O8A 97.2(3) . . ? O4A Li2A O8A 117.9(3) . . ? O7A Li2A O8A 82.0(2) . . ? O2A Li2A C57A 91.2(2) . . ? O4A Li2A C57A 139.2(3) . . ? O7A Li2A C57A 56.65(17) . . ? O8A Li2A C57A 30.67(13) . . ? O2A Li2A Li1A 75.2(2) . . ? O4A Li2A Li1A 66.1(2) . . ? O7A Li2A Li1A 103.3(3) . . ? O8A Li2A Li1A 171.9(3) . . ? C57A Li2A Li1A 149.8(2) . . ? C2A O1A Li1A 143.0(3) . . ? C2A O2A Li2A 128.0(3) . . ? C28A O3A Li1A 128.2(3) . . ? C28A O4A Li2A 143.7(3) . . ? C56A O5A C53A 112.3(3) . . ? C56A O5A Li1A 130.8(3) . . ? C53A O5A Li1A 111.9(3) . . ? C55A O6A C54A 113.0(3) . . ? C55A O6A Li1A 116.6(3) . . ? C54A O6A Li1A 101.6(3) . . ? C59A O7A C58A 112.8(3) . . ? C59A O7A Li2A 129.4(3) . . ? C58A O7A Li2A 111.3(3) . . ? C60A O8A C57A 110.5(3) . . ? C60A O8A Li2A 116.3(3) . . ? C57A O8A Li2A 102.7(3) . . ? C2A C1A P1A 109.3(2) . . ? C2A C1A P2A 114.8(2) . . ? P1A C1A P2A 104.77(16) . . ? C2A C1A H1A 111.7(19) . . ? P1A C1A H1A 110.2(19) . . ? P2A C1A H1A 105.8(19) . . ? O2A C2A O1A 126.6(3) . . ? O2A C2A C1A 116.5(3) . . ? O1A C2A C1A 116.8(3) . . ? C4A C3A C8A 117.8(3) . . ? C4A C3A P1A 126.0(2) . . ? C8A C3A P1A 116.0(2) . . ? C5A C4A C3A 120.6(3) . . ? C5A C4A H4AA 119.7 . . ? C3A C4A H4AA 119.7 . . ? C6A C5A C4A 120.6(4) . . ? C6A C5A H5AA 119.7 . . ? C4A C5A H5AA 119.7 . . ? C7A C6A C5A 119.6(3) . . ? C7A C6A H6AA 120.2 . . ? C5A C6A H6AA 120.2 . . ? C6A C7A C8A 120.1(3) . . ? C6A C7A H7AA 119.9 . . ? C8A C7A H7AA 119.9 . . ? C7A C8A C3A 121.2(3) . . ? C7A C8A H8AA 119.4 . . ? C3A C8A H8AA 119.4 . . ? C14A C9A C10A 117.6(3) . . ? C14A C9A P1A 117.7(3) . . ? C10A C9A P1A 124.5(3) . . ? C11A C10A C9A 120.7(3) . . ? C11A C10A H10A 119.6 . . ? C9A C10A H10A 119.6 . . ? C12A C11A C10A 120.6(4) . . ? C12A C11A H11A 119.7 . . ? C10A C11A H11A 119.7 . . ? C13A C12A C11A 119.9(3) . . ? C13A C12A H12A 120.0 . . ? C11A C12A H12A 120.0 . . ? C12A C13A C14A 120.1(4) . . ? C12A C13A H13A 120.0 . . ? C14A C13A H13A 120.0 . . ? C13A C14A C9A 121.0(4) . . ? C13A C14A H14A 119.5 . . ? C9A C14A H14A 119.5 . . ? C20A C15A C16A 117.9(3) . . ? C20A C15A P2A 126.7(3) . . ? C16A C15A P2A 115.1(3) . . ? C17A C16A C15A 121.4(4) . . ? C17A C16A H16A 119.3 . . ? C15A C16A H16A 119.3 . . ? C18A C17A C16A 120.1(4) . . ? C18A C17A H17A 120.0 . . ? C16A C17A H17A 120.0 . . ? C17A C18A C19A 119.5(3) . . ? C17A C18A H18A 120.3 . . ? C19A C18A H18A 120.3 . . ? C18A C19A C20A 120.8(4) . . ? C18A C19A H19A 119.6 . . ? C20A C19A H19A 119.6 . . ? C15A C20A C19A 120.3(3) . . ? C15A C20A H20A 119.9 . . ? C19A C20A H20A 119.9 . . ? C26A C21A C22A 118.5(3) . . ? C26A C21A P2A 124.7(3) . . ? C22A C21A P2A 116.8(2) . . ? C21A C22A C23A 120.9(3) . . ? C21A C22A H22A 119.6 . . ? C23A C22A H22A 119.6 . . ? C24A C23A C22A 119.8(4) . . ? C24A C23A H23A 120.1 . . ? C22A C23A H23A 120.1 . . ? C23A C24A C25A 120.0(3) . . ? C23A C24A H24A 120.0 . . ? C25A C24A H24A 120.0 . . ? C26A C25A C24A 120.2(3) . . ? C26A C25A H25A 119.9 . . ? C24A C25A H25A 119.9 . . ? C25A C26A C21A 120.6(3) . . ? C25A C26A H26A 119.7 . . ? C21A C26A H26A 119.7 . . ? C28A C27A P3A 110.7(2) . . ? C28A C27A P4A 116.1(2) . . ? P3A C27A P4A 104.97(16) . . ? C28A C27A H27A 107(2) . . ? P3A C27A H27A 107(2) . . ? P4A C27A H27A 110(2) . . ? O3A C28A O4A 126.3(3) . . ? O3A C28A C27A 117.2(3) . . ? O4A C28A C27A 116.5(3) . . ? C30A C29A C34A 118.1(3) . . ? C30A C29A P3A 116.2(3) . . ? C34A C29A P3A 125.7(3) . . ? C29A C30A C31A 121.4(4) . . ? C29A C30A H30A 119.3 . . ? C31A C30A H30A 119.3 . . ? C32A C31A C30A 119.5(4) . . ? C32A C31A H31A 120.2 . . ? C30A C31A H31A 120.2 . . ? C31A C32A C33A 120.6(4) . . ? C31A C32A H32A 119.7 . . ? C33A C32A H32A 119.7 . . ? C32A C33A C34A 120.3(4) . . ? C32A C33A H33A 119.8 . . ? C34A C33A H33A 119.8 . . ? C33A C34A C29A 120.0(4) . . ? C33A C34A H34A 120.0 . . ? C29A C34A H34A 120.0 . . ? C36A C35A C40A 118.9(5) . . ? C36A C35A P3A 116.8(4) . . ? C40A C35A P3A 124.2(3) . . ? C35A C36A C37A 119.8(7) . . ? C35A C36A H36A 120.1 . . ? C37A C36A H36A 120.1 . . ? C38A C37A C36A 120.3(7) . . ? C38A C37A H37A 119.9 . . ? C36A C37A H37A 119.9 . . ? C37A C38A C39A 120.4(6) . . ? C37A C38A H38A 119.8 . . ? C39A C38A H38A 119.8 . . ? C40A C39A C38A 118.7(7) . . ? C40A C39A H39A 120.7 . . ? C38A C39A H39A 120.7 . . ? C35A C40A C39A 121.8(6) . . ? C35A C40A H40A 119.1 . . ? C39A C40A H40A 119.1 . . ? C46A C41A C42A 118.0(4) . . ? C46A C41A P4A 114.8(3) . . ? C42A C41A P4A 127.1(3) . . ? C43A C42A C41A 120.5(4) . . ? C43A C42A H42A 119.8 . . ? C41A C42A H42A 119.8 . . ? C44A C43A C42A 120.3(4) . . ? C44A C43A H43A 119.8 . . ? C42A C43A H43A 119.8 . . ? C45A C44A C43A 119.8(4) . . ? C45A C44A H44A 120.1 . . ? C43A C44A H44A 120.1 . . ? C44A C45A C46A 120.5(4) . . ? C44A C45A H45A 119.7 . . ? C46A C45A H45A 119.7 . . ? C45A C46A C41A 120.7(4) . . ? C45A C46A H46A 119.6 . . ? C41A C46A H46A 119.6 . . ? C48A C47A C52A 116.2(4) . . ? C48A C47A P4A 118.7(3) . . ? C52A C47A P4A 124.8(3) . . ? C47A C48A C49A 122.5(5) . . ? C47A C48A H48A 118.7 . . ? C49A C48A H48A 118.7 . . ? C50A C49A C48A 120.3(5) . . ? C50A C49A H49A 119.9 . . ? C48A C49A H49A 119.9 . . ? C49A C50A C51A 118.4(4) . . ? C49A C50A H50A 120.8 . . ? C51A C50A H50A 120.8 . . ? C50A C51A C52A 121.0(5) . . ? C50A C51A H51A 119.5 . . ? C52A C51A H51A 119.5 . . ? C47A C52A C51A 121.6(5) . . ? C47A C52A H52A 119.2 . . ? C51A C52A H52A 119.2 . . ? O5A C53A C54A 107.3(3) . . ? O5A C53A H53A 110.3 . . ? C54A C53A H53A 110.3 . . ? O5A C53A H53B 110.3 . . ? C54A C53A H53B 110.3 . . ? H53A C53A H53B 108.5 . . ? O6A C54A C53A 111.3(3) . . ? O6A C54A Li1A 47.69(19) . . ? C53A C54A Li1A 80.8(2) . . ? O6A C54A H54A 109.4 . . ? C53A C54A H54A 109.4 . . ? Li1A C54A H54A 87.1 . . ? O6A C54A H54B 109.4 . . ? C53A C54A H54B 109.4 . . ? Li1A C54A H54B 156.7 . . ? H54A C54A H54B 108.0 . . ? O6A C55A H55A 109.5 . . ? O6A C55A H55B 109.5 . . ? H55A C55A H55B 109.5 . . ? O6A C55A H55C 109.5 . . ? H55A C55A H55C 109.5 . . ? H55B C55A H55C 109.5 . . ? O5A C56A H56A 109.5 . . ? O5A C56A H56B 109.5 . . ? H56A C56A H56B 109.5 . . ? O5A C56A H56C 109.5 . . ? H56A C56A H56C 109.5 . . ? H56B C56A H56C 109.5 . . ? O8A C57A C58A 107.4(3) . . ? O8A C57A Li2A 46.7(2) . . ? C58A C57A Li2A 78.9(2) . . ? O8A C57A H57A 110.2 . . ? C58A C57A H57A 110.2 . . ? Li2A C57A H57A 87.1 . . ? O8A C57A H57B 110.2 . . ? C58A C57A H57B 110.2 . . ? Li2A C57A H57B 156.5 . . ? H57A C57A H57B 108.5 . . ? O7A C58A C57A 107.3(3) . . ? O7A C58A H58A 110.3 . . ? C57A C58A H58A 110.3 . . ? O7A C58A H58B 110.3 . . ? C57A C58A H58B 110.3 . . ? H58A C58A H58B 108.5 . . ? O7A C59A H59A 109.5 . . ? O7A C59A H59B 109.5 . . ? H59A C59A H59B 109.5 . . ? O7A C59A H59C 109.5 . . ? H59A C59A H59C 109.5 . . ? H59B C59A H59C 109.5 . . ? O8A C60A H60A 109.5 . . ? O8A C60A H60B 109.5 . . ? H60A C60A H60B 109.5 . . ? O8A C60A H60C 109.5 . . ? H60A C60A H60C 109.5 . . ? H60B C60A H60C 109.5 . . ? C9B P1B C3B 105.13(18) . . ? C9B P1B C1B 103.06(17) . . ? C3B P1B C1B 104.13(17) . . ? C21B P2B C15B 99.02(18) . . ? C21B P2B C1B 102.34(18) . . ? C15B P2B C1B 101.86(17) . . ? C35B P3B C29B 109.3(2) . . ? C35B P3B C27B 105.3(2) . . ? C29B P3B C27B 105.57(18) . . ? C35B P3B C35C 15.42(19) . . ? C29B P3B C35C 96.95(18) . . ? C27B P3B C35C 100.82(19) . . ? C47B P4B C41B 100.20(19) . . ? C47B P4B C27B 103.0(2) . . ? C41B P4B C27B 100.93(18) . . ? O3B Li1B O1B 128.9(4) . . ? O3B Li1B O6B 104.3(4) . . ? O1B Li1B O6B 115.4(4) . . ? O3B Li1B O5B 106.5(4) . . ? O1B Li1B O5B 111.0(4) . . ? O6B Li1B O5B 79.7(3) . . ? O3B Li1B C54C 90.0(4) . . ? O1B Li1B C54C 138.9(5) . . ? O6B Li1B C54C 55.1(3) . . ? O5B Li1B C54C 33.5(3) . . ? O4B Li2B O2B 129.0(4) . . ? O4B Li2B O7B 105.6(3) . . ? O2B Li2B O7B 110.6(4) . . ? O4B Li2B O8B 120.9(4) . . ? O2B Li2B O8B 98.6(3) . . ? O7B Li2B O8B 82.6(3) . . ? O4B Li2B C58B 131.5(4) . . ? O2B Li2B C58B 98.9(3) . . ? O7B Li2B C58B 54.9(3) . . ? O8B Li2B C58B 29.2(2) . . ? C2B O1B Li1B 132.8(4) . . ? C2B O2B Li2B 140.0(4) . . ? C28B O3B Li1B 135.4(4) . . ? C28B O4B Li2B 135.0(4) . . ? C55C O5B C54B 65.8(8) . . ? C55C O5B C55B 46.6(8) . . ? C54B O5B C55B 108.8(6) . . ? C55C O5B C54C 112.3(10) . . ? C54B O5B C54C 48.1(6) . . ? C55B O5B C54C 143.1(7) . . ? C55C O5B Li1B 121.2(8) . . ? C54B O5B Li1B 113.7(4) . . ? C55B O5B Li1B 117.8(5) . . ? C54C O5B Li1B 99.0(6) . . ? C56B O6B C53B 116.5(4) . . ? C56B O6B Li1B 128.2(4) . . ? C53B O6B Li1B 109.0(3) . . ? C60B O7B C57B 109.8(6) . . ? C60B O7B Li2B 125.3(4) . . ? C57B O7B Li2B 108.7(5) . . ? C58B O8B C59B 107.2(5) . . ? C58B O8B Li2B 104.9(5) . . ? C59B O8B Li2B 118.2(3) . . ? C2B C1B P2B 110.1(3) . . ? C2B C1B P1B 114.9(3) . . ? P2B C1B P1B 105.52(19) . . ? C2B C1B H1B 113(3) . . ? P2B C1B H1B 108(3) . . ? P1B C1B H1B 105(3) . . ? O1B C2B O2B 127.1(4) . . ? O1B C2B C1B 116.0(4) . . ? O2B C2B C1B 116.9(4) . . ? C4B C3B C8B 119.0(4) . . ? C4B C3B P1B 127.1(3) . . ? C8B C3B P1B 113.9(3) . . ? C3B C4B C5B 120.8(4) . . ? C3B C4B H4BA 119.6 . . ? C5B C4B H4BA 119.6 . . ? C6B C5B C4B 119.8(5) . . ? C6B C5B H5BA 120.1 . . ? C4B C5B H5BA 120.1 . . ? C7B C6B C5B 119.9(5) . . ? C7B C6B H6BA 120.1 . . ? C5B C6B H6BA 120.1 . . ? C6B C7B C8B 120.7(5) . . ? C6B C7B H7BA 119.6 . . ? C8B C7B H7BA 119.6 . . ? C7B C8B C3B 119.7(5) . . ? C7B C8B H8BA 120.1 . . ? C3B C8B H8BA 120.1 . . ? C10B C9B C14B 117.4(4) . . ? C10B C9B P1B 117.7(3) . . ? C14B C9B P1B 124.1(3) . . ? C11B C10B C9B 121.5(4) . . ? C11B C10B H10B 119.2 . . ? C9B C10B H10B 119.2 . . ? C10B C11B C12B 120.5(4) . . ? C10B C11B H11B 119.8 . . ? C12B C11B H11B 119.8 . . ? C13B C12B C11B 119.2(4) . . ? C13B C12B H12B 120.4 . . ? C11B C12B H12B 120.4 . . ? C12B C13B C14B 120.6(4) . . ? C12B C13B H13B 119.7 . . ? C14B C13B H13B 119.7 . . ? C13B C14B C9B 120.8(4) . . ? C13B C14B H14B 119.6 . . ? C9B C14B H14B 119.6 . . ? C20B C15B C16B 117.6(4) . . ? C20B C15B P2B 125.4(3) . . ? C16B C15B P2B 116.8(4) . . ? C17B C16B C15B 120.2(5) . . ? C17B C16B H16B 119.9 . . ? C15B C16B H16B 119.9 . . ? C18B C17B C16B 120.7(5) . . ? C18B C17B H17B 119.6 . . ? C16B C17B H17B 119.6 . . ? C19B C18B C17B 118.9(5) . . ? C19B C18B H18B 120.6 . . ? C17B C18B H18B 120.6 . . ? C18B C19B C20B 121.1(6) . . ? C18B C19B H19B 119.5 . . ? C20B C19B H19B 119.5 . . ? C19B C20B C15B 121.5(5) . . ? C19B C20B H20B 119.3 . . ? C15B C20B H20B 119.3 . . ? C22B C21B C26B 118.1(4) . . ? C22B C21B P2B 116.7(3) . . ? C26B C21B P2B 125.2(3) . . ? C21B C22B C23B 120.6(4) . . ? C21B C22B H22B 119.7 . . ? C23B C22B H22B 119.7 . . ? C24B C23B C22B 120.7(4) . . ? C24B C23B H23B 119.6 . . ? C22B C23B H23B 119.6 . . ? C23B C24B C25B 119.4(4) . . ? C23B C24B H24B 120.3 . . ? C25B C24B H24B 120.3 . . ? C24B C25B C26B 120.7(4) . . ? C24B C25B H25B 119.7 . . ? C26B C25B H25B 119.7 . . ? C25B C26B C21B 120.5(4) . . ? C25B C26B H26B 119.7 . . ? C21B C26B H26B 119.7 . . ? C28B C27B P4B 111.0(3) . . ? C28B C27B P3B 115.4(3) . . ? P4B C27B P3B 104.4(2) . . ? C28B C27B H27B 108(2) . . ? P4B C27B H27B 111(2) . . ? P3B C27B H27B 107(2) . . ? O4B C28B O3B 126.9(4) . . ? O4B C28B C27B 116.0(5) . . ? O3B C28B C27B 117.1(4) . . ? C30B C29B C34B 117.6(4) . . ? C30B C29B P3B 114.7(3) . . ? C34B C29B P3B 127.5(3) . . ? C29B C30B C31B 121.3(4) . . ? C29B C30B H30B 119.4 . . ? C31B C30B H30B 119.4 . . ? C32B C31B C30B 120.4(5) . . ? C32B C31B H31B 119.8 . . ? C30B C31B H31B 119.8 . . ? C33B C32B C31B 119.0(4) . . ? C33B C32B H32B 120.5 . . ? C31B C32B H32B 120.5 . . ? C32B C33B C34B 120.8(4) . . ? C32B C33B H33B 119.6 . . ? C34B C33B H33B 119.6 . . ? C29B C34B C33B 120.7(4) . . ? C29B C34B H34B 119.6 . . ? C33B C34B H34B 119.6 . . ? C46B C41B C42B 118.5(4) . . ? C46B C41B P4B 117.1(4) . . ? C42B C41B P4B 124.3(4) . . ? C43B C42B C41B 120.7(5) . . ? C43B C42B H42B 119.7 . . ? C41B C42B H42B 119.7 . . ? C42B C43B C44B 120.2(6) . . ? C42B C43B H43B 119.9 . . ? C44B C43B H43B 119.9 . . ? C45B C44B C43B 119.6(5) . . ? C45B C44B H44B 120.2 . . ? C43B C44B H44B 120.2 . . ? C44B C45B C46B 120.2(6) . . ? C44B C45B H45B 119.9 . . ? C46B C45B H45B 119.9 . . ? C41B C46B C45B 120.7(5) . . ? C41B C46B H46B 119.6 . . ? C45B C46B H46B 119.6 . . ? C48B C47B C52B 118.8(5) . . ? C48B C47B P4B 125.5(4) . . ? C52B C47B P4B 115.6(4) . . ? C47B C48B C49B 119.3(6) . . ? C47B C48B H48B 120.3 . . ? C49B C48B H48B 120.3 . . ? C50B C49B C48B 120.9(7) . . ? C50B C49B H49B 119.6 . . ? C48B C49B H49B 119.6 . . ? C51B C50B C49B 119.6(5) . . ? C51B C50B H50B 120.2 . . ? C49B C50B H50B 120.2 . . ? C50B C51B C52B 121.0(7) . . ? C50B C51B H51B 119.5 . . ? C52B C51B H51B 119.5 . . ? C47B C52B C51B 120.4(7) . . ? C47B C52B H52B 119.8 . . ? C51B C52B H52B 119.8 . . ? C54C C53B O6B 116.5(7) . . ? C54C C53B C54B 48.6(7) . . ? O6B C53B C54B 109.4(5) . . ? C54C C53B H53C 62.2 . . ? O6B C53B H53C 109.8 . . ? C54B C53B H53C 109.8 . . ? C54C C53B H53D 133.2 . . ? O6B C53B H53D 109.8 . . ? C54B C53B H53D 109.8 . . ? H53C C53B H53D 108.2 . . ? C54C C53B H53E 108.0 . . ? O6B C53B H53E 108.3 . . ? C54B C53B H53E 65.1 . . ? H53C C53B H53E 140.7 . . ? H53D C53B H53E 48.3 . . ? C54C C53B H53F 108.1 . . ? O6B C53B H53F 108.2 . . ? C54B C53B H53F 142.1 . . ? H53C C53B H53F 50.9 . . ? H53D C53B H53F 61.0 . . ? H53E C53B H53F 107.4 . . ? O5B C54B C53B 105.9(6) . . ? O5B C54B H53E 138.6 . . ? C53B C54B H53E 38.5 . . ? O5B C54B H54C 110.6 . . ? C53B C54B H54C 110.6 . . ? H53E C54B H54C 77.9 . . ? O5B C54B H54D 110.6 . . ? C53B C54B H54D 110.6 . . ? H53E C54B H54D 104.0 . . ? H54C C54B H54D 108.7 . . ? O5B C55B H55D 109.5 . . ? O5B C55B H55E 109.5 . . ? H55D C55B H55E 109.5 . . ? O5B C55B H55F 109.5 . . ? H55D C55B H55F 109.5 . . ? H55E C55B H55F 109.5 . . ? C53B C54C O5B 107.9(10) . . ? C53B C54C Li1B 78.9(7) . . ? O5B C54C Li1B 47.5(4) . . ? C53B C54C H54E 110.1 . . ? O5B C54C H54E 110.1 . . ? Li1B C54C H54E 86.5 . . ? C53B C54C H54F 110.1 . . ? O5B C54C H54F 110.1 . . ? Li1B C54C H54F 157.3 . . ? H54E C54C H54F 108.4 . . ? O5B C55C H55G 109.5 . . ? O5B C55C H55H 109.5 . . ? H55G C55C H55H 109.5 . . ? O5B C55C H55I 109.5 . . ? H55G C55C H55I 109.5 . . ? H55H C55C H55I 109.5 . . ? O6B C56B H56D 109.5 . . ? O6B C56B H56E 109.5 . . ? H56D C56B H56E 109.5 . . ? O6B C56B H56F 109.5 . . ? H56D C56B H56F 109.5 . . ? H56E C56B H56F 109.5 . . ? C58B C57B O7B 114.0(8) . . ? C58B C57B H57C 108.8 . . ? O7B C57B H57C 108.8 . . ? C58B C57B H57D 108.7 . . ? O7B C57B H57D 108.8 . . ? H57C C57B H57D 107.6 . . ? C57B C58B O8B 114.8(8) . . ? C57B C58B Li2B 77.1(6) . . ? O8B C58B Li2B 45.9(3) . . ? C57B C58B H58C 108.6 . . ? O8B C58B H58C 108.6 . . ? Li2B C58B H58C 149.2 . . ? C57B C58B H58D 108.6 . . ? O8B C58B H58D 108.6 . . ? Li2B C58B H58D 98.6 . . ? H58C C58B H58D 107.5 . . ? O8B C59B H59D 109.5 . . ? O8B C59B H59E 109.5 . . ? H59D C59B H59E 109.5 . . ? O8B C59B H59F 109.5 . . ? H59D C59B H59F 109.5 . . ? H59E C59B H59F 109.5 . . ? O7B C60B H60D 109.5 . . ? O7B C60B H60E 109.5 . . ? H60D C60B H60E 109.5 . . ? O7B C60B H60F 109.5 . . ? H60D C60B H60F 109.5 . . ? H60E C60B H60F 109.5 . . ? C36B C35B C40B 120.0 . . ? C36B C35B P3B 121.4(3) . . ? C40B C35B P3B 118.6(3) . . ? C35B C36B C37B 120.0 . . ? C35B C36B H36B 120.0 . . ? C37B C36B H36B 120.0 . . ? C38B C37B C36B 120.0 . . ? C38B C37B H37B 120.0 . . ? C36B C37B H37B 120.0 . . ? C37B C38B C39B 120.0 . . ? C37B C38B H38B 120.0 . . ? C39B C38B H38B 120.0 . . ? C40B C39B C38B 120.0 . . ? C40B C39B H39B 120.0 . . ? C38B C39B H39B 120.0 . . ? C39B C40B C35B 120.0 . . ? C39B C40B H40B 120.0 . . ? C35B C40B H40B 120.0 . . ? C36C C35C C40C 120.0 . . ? C36C C35C P3B 125.1(2) . . ? C40C C35C P3B 114.3(2) . . ? C37C C36C C35C 120.0 . . ? C37C C36C H36C 120.0 . . ? C35C C36C H36C 120.0 . . ? C36C C37C C38C 120.0 . . ? C36C C37C H37C 120.0 . . ? C38C C37C H37C 120.0 . . ? C39C C38C C37C 120.0 . . ? C39C C38C H38C 120.0 . . ? C37C C38C H38C 120.0 . . ? C38C C39C C40C 120.0 . . ? C38C C39C H39C 120.0 . . ? C40C C39C H39C 120.0 . . ? C39C C40C C35C 120.0 . . ? C39C C40C H40C 120.0 . . ? C35C C40C H40C 120.0 . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.935 _refine_diff_density_max 0.881 _refine_diff_density_min -0.781 _refine_diff_density_rms 0.073 #=== END data_FO3494 _database_code_depnum_ccdc_archive 'CCDC 770467' #TrackingRef '- dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H45 Cl I Ir P4' _chemical_formula_weight 1124.29 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' P P 0.1023 0.0942 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.7210(5) _cell_length_b 16.1700(3) _cell_length_c 25.2040(7) _cell_angle_alpha 90.00 _cell_angle_beta 120.220(3) _cell_angle_gamma 90.00 _cell_volume 4479.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.667 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 3.906 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41253 _diffrn_reflns_av_R_equivalents 0.0910 _diffrn_reflns_av_sigmaI/netI 0.0778 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 27.47 _reflns_number_total 10225 _reflns_number_gt 7899 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1057P)^2^+148.1634P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10225 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1138 _refine_ls_R_factor_gt 0.0833 _refine_ls_wR_factor_ref 0.2321 _refine_ls_wR_factor_gt 0.2139 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.78777(4) 0.26060(2) 0.425427(19) 0.01658(15) Uani 1 1 d . . . I1 I 0.30184(16) 0.05672(10) 0.19227(8) 0.0842(5) Uani 1 1 d . . . Cl1 Cl 0.8237(3) 0.12832(16) 0.48072(13) 0.0243(6) Uani 1 1 d . . . P1 P 0.8437(3) 0.34866(18) 0.50926(13) 0.0204(6) Uani 1 1 d . . . P2 P 0.9875(3) 0.30079(17) 0.46357(13) 0.0182(6) Uani 1 1 d . . . P3 P 0.5825(3) 0.22026(18) 0.37532(14) 0.0197(6) Uani 1 1 d . . . P4 P 0.7413(3) 0.18896(17) 0.33668(13) 0.0177(6) Uani 1 1 d . . . C1 C 0.9792(11) 0.3879(7) 0.5072(5) 0.023(2) Uani 1 1 d . . . H1A H 0.9636 0.4411 0.4850 0.028 Uiso 1 1 calc R . . H1B H 1.0521 0.3925 0.5486 0.028 Uiso 1 1 calc R . . C2 C 0.7545(11) 0.4392(7) 0.5049(6) 0.026(3) Uani 1 1 d . . . C3 C 0.7208(12) 0.4948(7) 0.4562(6) 0.030(3) Uani 1 1 d . . . H3A H 0.7456 0.4856 0.4269 0.036 Uiso 1 1 calc R . . C4 C 0.6513(13) 0.5628(8) 0.4515(7) 0.038(3) Uani 1 1 d . . . H4A H 0.6271 0.6003 0.4183 0.046 Uiso 1 1 calc R . . C5 C 0.6163(14) 0.5769(9) 0.4950(8) 0.044(4) Uani 1 1 d . . . H5A H 0.5682 0.6239 0.4912 0.053 Uiso 1 1 calc R . . C6 C 0.6499(14) 0.5253(9) 0.5413(8) 0.042(4) Uani 1 1 d . . . H6A H 0.6265 0.5363 0.5710 0.051 Uiso 1 1 calc R . . C7 C 0.7195(12) 0.4540(8) 0.5479(6) 0.031(3) Uani 1 1 d . . . H7A H 0.7419 0.4170 0.5812 0.037 Uiso 1 1 calc R . . C8 C 0.8996(12) 0.3086(8) 0.5862(6) 0.027(3) Uani 1 1 d . . . C9 C 0.8361(14) 0.2435(8) 0.5938(7) 0.034(3) Uani 1 1 d . . . H9A H 0.7687 0.2184 0.5595 0.041 Uiso 1 1 calc R . . C10 C 0.8751(18) 0.2165(10) 0.6539(8) 0.051(5) Uani 1 1 d . . . H10A H 0.8347 0.1721 0.6610 0.062 Uiso 1 1 calc R . . C11 C 0.974(2) 0.2555(14) 0.7031(8) 0.071(7) Uani 1 1 d . . . H11A H 0.9977 0.2389 0.7438 0.086 Uiso 1 1 calc R . . C12 C 1.0376(16) 0.3186(12) 0.6937(8) 0.052(4) Uani 1 1 d . . . H12A H 1.1068 0.3429 0.7276 0.062 Uiso 1 1 calc R . . C13 C 1.0002(14) 0.3442(9) 0.6364(6) 0.038(3) Uani 1 1 d . . . H13A H 1.0430 0.3875 0.6299 0.045 Uiso 1 1 calc R . . C14 C 1.1100(10) 0.2331(7) 0.5169(5) 0.021(2) Uani 1 1 d . . . C15 C 1.2020(12) 0.2609(8) 0.5736(6) 0.032(3) Uani 1 1 d . . . H15A H 1.2016 0.3163 0.5861 0.038 Uiso 1 1 calc R . . C16 C 1.2942(12) 0.2075(9) 0.6115(6) 0.033(3) Uani 1 1 d . . . H16A H 1.3579 0.2262 0.6501 0.040 Uiso 1 1 calc R . . C17 C 1.2938(13) 0.1270(9) 0.5934(6) 0.034(3) Uani 1 1 d . . . H17A H 1.3581 0.0906 0.6191 0.041 Uiso 1 1 calc R . . C18 C 1.1995(11) 0.0996(7) 0.5378(6) 0.027(3) Uani 1 1 d . . . H18A H 1.1973 0.0436 0.5259 0.032 Uiso 1 1 calc R . . C19 C 1.1111(11) 0.1520(7) 0.5005(6) 0.023(2) Uani 1 1 d . . . H19A H 1.0478 0.1328 0.4619 0.028 Uiso 1 1 calc R . . C20 C 1.0353(11) 0.3395(7) 0.4102(5) 0.024(2) Uani 1 1 d . . . C21 C 1.1268(12) 0.3016(8) 0.4053(6) 0.029(3) Uani 1 1 d . . . H21A H 1.1705 0.2566 0.4314 0.035 Uiso 1 1 calc R . . C22 C 1.1545(13) 0.3302(10) 0.3613(7) 0.037(3) Uani 1 1 d . . . H22A H 1.2167 0.3040 0.3571 0.045 Uiso 1 1 calc R . . C23 C 1.0932(15) 0.3949(10) 0.3249(6) 0.041(4) Uani 1 1 d . . . H23A H 1.1141 0.4143 0.2959 0.049 Uiso 1 1 calc R . . C24 C 1.0010(15) 0.4331(9) 0.3292(7) 0.038(3) Uani 1 1 d . . . H24A H 0.9584 0.4784 0.3032 0.045 Uiso 1 1 calc R . . C25 C 0.9705(14) 0.4047(8) 0.3722(6) 0.034(3) Uani 1 1 d . . . H25A H 0.9063 0.4299 0.3753 0.041 Uiso 1 1 calc R . . C26 C 0.6008(11) 0.1422(7) 0.3278(6) 0.024(2) Uani 1 1 d . . . H26A H 0.5330 0.1422 0.2848 0.029 Uiso 1 1 calc R . . H26B H 0.6138 0.0859 0.3454 0.029 Uiso 1 1 calc R . . C27 C 0.5041(11) 0.1682(7) 0.4104(6) 0.026(3) Uani 1 1 d . . . C28 C 0.448(2) 0.0952(11) 0.3883(11) 0.074(7) Uani 1 1 d . . . H28A H 0.4521 0.0692 0.3556 0.089 Uiso 1 1 calc R . . C29 C 0.384(3) 0.0580(14) 0.4132(17) 0.129(14) Uani 1 1 d . . . H29A H 0.3491 0.0049 0.3995 0.155 Uiso 1 1 calc R . . C30 C 0.373(2) 0.0997(12) 0.4586(12) 0.075(7) Uani 1 1 d . . . H30A H 0.3286 0.0755 0.4756 0.090 Uiso 1 1 calc R . . C31 C 0.4253(14) 0.1743(11) 0.4781(7) 0.046(4) Uani 1 1 d . . . H31A H 0.4159 0.2032 0.5083 0.055 Uiso 1 1 calc R . . C32 C 0.4919(13) 0.2088(10) 0.4549(6) 0.036(3) Uani 1 1 d . . . H32A H 0.5299 0.2610 0.4697 0.043 Uiso 1 1 calc R . . C33 C 0.4687(11) 0.2962(7) 0.3250(6) 0.025(2) Uani 1 1 d . . . C34 C 0.3604(13) 0.2743(9) 0.2759(7) 0.038(3) Uani 1 1 d . . . H34A H 0.3436 0.2177 0.2645 0.046 Uiso 1 1 calc R . . C35 C 0.2738(13) 0.3341(10) 0.2422(7) 0.041(3) Uani 1 1 d . . . H35A H 0.1977 0.3188 0.2080 0.049 Uiso 1 1 calc R . . C36 C 0.3002(14) 0.4175(10) 0.2593(7) 0.042(4) Uani 1 1 d . . . H36A H 0.2423 0.4592 0.2363 0.050 Uiso 1 1 calc R . . C37 C 0.4053(17) 0.4377(10) 0.3073(10) 0.078(7) Uani 1 1 d . . . H37A H 0.4218 0.4940 0.3196 0.093 Uiso 1 1 calc R . . C38 C 0.4933(16) 0.3771(10) 0.3405(8) 0.057(5) Uani 1 1 d . . . H38A H 0.5702 0.3928 0.3740 0.068 Uiso 1 1 calc R . . C39 C 0.6902(11) 0.2444(8) 0.2646(5) 0.026(3) Uani 1 1 d . . . C40 C 0.6503(13) 0.1980(8) 0.2109(6) 0.032(3) Uani 1 1 d . . . H40A H 0.6532 0.1393 0.2126 0.038 Uiso 1 1 calc R . . C41 C 0.6068(16) 0.2382(11) 0.1556(7) 0.050(4) Uani 1 1 d . . . H41A H 0.5791 0.2068 0.1191 0.060 Uiso 1 1 calc R . . C42 C 0.6030(12) 0.3234(10) 0.1525(6) 0.039(3) Uani 1 1 d . . . H42A H 0.5746 0.3510 0.1144 0.046 Uiso 1 1 calc R . . C43 C 0.6412(14) 0.3677(9) 0.2059(7) 0.043(4) Uani 1 1 d . . . H43A H 0.6370 0.4263 0.2041 0.052 Uiso 1 1 calc R . . C44 C 0.6845(13) 0.3295(8) 0.2611(6) 0.030(3) Uani 1 1 d . . . H44A H 0.7108 0.3615 0.2972 0.036 Uiso 1 1 calc R . . C45 C 0.8471(10) 0.1115(7) 0.3395(5) 0.019(2) Uani 1 1 d . . . C46 C 0.8658(12) 0.0369(7) 0.3721(5) 0.026(3) Uani 1 1 d . . . H46A H 0.8134 0.0235 0.3875 0.031 Uiso 1 1 calc R . . C47 C 0.9562(12) -0.0160(8) 0.3821(6) 0.031(3) Uani 1 1 d . . . H47A H 0.9668 -0.0660 0.4040 0.037 Uiso 1 1 calc R . . C48 C 1.0319(14) 0.0030(10) 0.3603(8) 0.045(4) Uani 1 1 d . . . H48A H 1.0963 -0.0337 0.3679 0.054 Uiso 1 1 calc R . . C49 C 1.0169(16) 0.0750(11) 0.3272(9) 0.052(4) Uani 1 1 d . . . H49A H 1.0688 0.0866 0.3112 0.063 Uiso 1 1 calc R . . C50 C 0.9244(13) 0.1302(9) 0.3177(7) 0.037(3) Uani 1 1 d . . . H50A H 0.9149 0.1806 0.2963 0.044 Uiso 1 1 calc R . . H1IR H 0.7494 0.3461 0.3882 0.055 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 0.0242(2) 0.0098(2) 0.0178(2) -0.00097(15) 0.01211(17) 0.00088(15) I1 0.0948(12) 0.0615(9) 0.0874(11) -0.0043(7) 0.0392(9) -0.0077(8) Cl1 0.0335(16) 0.0161(13) 0.0236(14) 0.0028(10) 0.0146(12) 0.0020(10) P1 0.0296(16) 0.0172(14) 0.0164(14) -0.0040(10) 0.0131(12) 0.0002(11) P2 0.0209(14) 0.0148(13) 0.0206(14) -0.0039(10) 0.0118(12) -0.0024(10) P3 0.0211(14) 0.0177(14) 0.0228(15) -0.0013(10) 0.0129(12) 0.0007(11) P4 0.0236(15) 0.0129(13) 0.0174(14) -0.0017(10) 0.0110(12) -0.0007(10) C1 0.033(7) 0.018(6) 0.021(6) -0.011(4) 0.016(5) -0.005(5) C2 0.023(6) 0.022(6) 0.027(6) -0.006(5) 0.009(5) 0.001(4) C3 0.036(7) 0.015(6) 0.039(7) -0.003(5) 0.020(6) 0.000(5) C4 0.040(8) 0.018(6) 0.050(9) -0.006(6) 0.019(7) -0.002(5) C5 0.040(8) 0.022(7) 0.069(11) -0.013(7) 0.026(8) 0.007(6) C6 0.045(9) 0.036(8) 0.052(9) -0.018(7) 0.029(8) 0.004(6) C7 0.032(7) 0.034(7) 0.033(7) -0.012(5) 0.021(6) -0.004(5) C8 0.040(7) 0.027(6) 0.023(6) 0.003(5) 0.022(6) 0.010(5) C9 0.050(8) 0.031(7) 0.035(7) 0.009(5) 0.031(7) 0.012(6) C10 0.089(13) 0.044(9) 0.055(11) 0.021(8) 0.062(11) 0.034(9) C11 0.102(17) 0.090(16) 0.035(9) 0.015(9) 0.044(11) 0.064(14) C12 0.049(10) 0.061(11) 0.040(9) -0.006(8) 0.019(8) 0.017(8) C13 0.044(8) 0.040(8) 0.017(6) 0.000(5) 0.006(6) 0.011(6) C14 0.022(5) 0.020(5) 0.024(6) -0.003(4) 0.013(5) -0.002(4) C15 0.031(7) 0.029(7) 0.035(7) 0.000(5) 0.016(6) -0.002(5) C16 0.028(7) 0.039(7) 0.029(7) 0.005(6) 0.011(6) 0.001(6) C17 0.034(7) 0.034(7) 0.036(7) 0.010(6) 0.018(6) 0.003(6) C18 0.029(7) 0.018(6) 0.039(7) 0.009(5) 0.021(6) 0.001(5) C19 0.028(6) 0.018(5) 0.028(6) -0.002(4) 0.018(5) -0.002(4) C20 0.031(7) 0.021(6) 0.024(6) -0.007(4) 0.018(5) -0.007(5) C21 0.033(7) 0.034(7) 0.026(6) -0.006(5) 0.020(6) -0.009(5) C22 0.034(8) 0.051(9) 0.036(8) -0.012(6) 0.025(7) -0.010(6) C23 0.052(9) 0.054(9) 0.026(7) -0.009(6) 0.026(7) -0.019(7) C24 0.053(9) 0.030(7) 0.033(7) 0.000(5) 0.024(7) -0.009(6) C25 0.047(8) 0.026(7) 0.036(7) -0.001(5) 0.025(7) -0.002(6) C26 0.034(7) 0.015(5) 0.030(6) -0.010(4) 0.019(6) -0.006(5) C27 0.024(6) 0.024(6) 0.037(7) 0.001(5) 0.021(6) 0.006(5) C28 0.131(19) 0.035(9) 0.127(19) -0.018(10) 0.117(18) -0.014(10) C29 0.22(3) 0.047(12) 0.26(4) -0.043(17) 0.22(3) -0.048(16) C30 0.111(18) 0.053(11) 0.128(19) 0.019(12) 0.108(17) 0.007(11) C31 0.040(9) 0.071(11) 0.037(8) 0.006(7) 0.028(7) 0.013(8) C32 0.032(7) 0.043(8) 0.033(7) -0.002(6) 0.017(6) 0.008(6) C33 0.023(6) 0.023(6) 0.028(6) 0.004(5) 0.013(5) 0.005(5) C34 0.030(7) 0.032(7) 0.048(9) 0.002(6) 0.017(7) 0.001(6) C35 0.025(7) 0.056(10) 0.034(8) 0.002(6) 0.009(6) 0.002(6) C36 0.037(8) 0.050(9) 0.036(8) 0.019(7) 0.017(7) 0.013(7) C37 0.051(11) 0.020(8) 0.100(16) 0.002(8) -0.008(10) 0.015(7) C38 0.044(9) 0.031(8) 0.052(10) 0.000(7) -0.009(8) 0.008(7) C39 0.026(6) 0.033(7) 0.014(5) -0.001(5) 0.008(5) -0.003(5) C40 0.039(8) 0.026(7) 0.028(7) -0.012(5) 0.015(6) -0.010(5) C41 0.051(10) 0.067(11) 0.018(7) -0.007(7) 0.007(7) -0.012(8) C42 0.027(7) 0.053(9) 0.017(6) 0.012(6) -0.003(5) -0.003(6) C43 0.048(9) 0.033(8) 0.036(8) 0.020(6) 0.012(7) 0.009(6) C44 0.042(8) 0.024(6) 0.017(6) -0.001(4) 0.008(6) -0.002(5) C45 0.022(6) 0.016(5) 0.017(5) -0.006(4) 0.009(5) -0.003(4) C46 0.031(7) 0.025(6) 0.020(6) -0.005(4) 0.011(5) -0.006(5) C47 0.032(7) 0.023(6) 0.033(7) -0.002(5) 0.012(6) 0.004(5) C48 0.034(8) 0.040(8) 0.057(10) 0.005(7) 0.020(7) 0.019(6) C49 0.051(10) 0.049(10) 0.082(13) 0.016(9) 0.052(10) 0.013(8) C50 0.041(8) 0.035(8) 0.052(9) 0.013(6) 0.036(7) 0.011(6) _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 P2 2.311(3) . ? Ir1 P4 2.316(3) . ? Ir1 P1 2.342(3) . ? Ir1 P3 2.349(3) . ? Ir1 Cl1 2.467(3) . ? P1 C8 1.815(12) . ? P1 C2 1.822(12) . ? P1 C1 1.861(13) . ? P2 C14 1.824(12) . ? P2 C1 1.823(11) . ? P2 C20 1.844(12) . ? P3 C33 1.833(12) . ? P3 C26 1.833(11) . ? P3 C27 1.836(13) . ? P3 P4 2.696(4) . ? P4 C45 1.813(11) . ? P4 C39 1.828(12) . ? P4 C26 1.848(12) . ? C2 C7 1.385(18) . ? C2 C3 1.402(18) . ? C3 C4 1.378(18) . ? C4 C5 1.39(2) . ? C5 C6 1.32(2) . ? C6 C7 1.411(19) . ? C8 C13 1.394(19) . ? C8 C9 1.397(19) . ? C9 C10 1.41(2) . ? C10 C11 1.39(3) . ? C11 C12 1.40(3) . ? C12 C13 1.34(2) . ? C14 C19 1.377(16) . ? C14 C15 1.389(17) . ? C15 C16 1.381(19) . ? C16 C17 1.38(2) . ? C17 C18 1.382(19) . ? C18 C19 1.343(17) . ? C20 C21 1.374(18) . ? C20 C25 1.383(18) . ? C21 C22 1.399(18) . ? C22 C23 1.35(2) . ? C23 C24 1.38(2) . ? C24 C25 1.399(19) . ? C27 C28 1.35(2) . ? C27 C32 1.376(18) . ? C28 C29 1.39(2) . ? C29 C30 1.40(3) . ? C30 C31 1.34(3) . ? C31 C32 1.37(2) . ? C33 C38 1.36(2) . ? C33 C34 1.357(19) . ? C34 C35 1.39(2) . ? C35 C36 1.40(2) . ? C36 C37 1.32(2) . ? C37 C38 1.40(2) . ? C39 C44 1.379(17) . ? C39 C40 1.399(17) . ? C40 C41 1.38(2) . ? C41 C42 1.38(2) . ? C42 C43 1.38(2) . ? C43 C44 1.358(18) . ? C45 C50 1.381(17) . ? C45 C46 1.409(16) . ? C46 C47 1.352(18) . ? C47 C48 1.36(2) . ? C48 C49 1.39(2) . ? C49 C50 1.40(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Ir1 P4 103.59(10) . . ? P2 Ir1 P1 71.48(11) . . ? P4 Ir1 P1 171.65(10) . . ? P2 Ir1 P3 173.35(10) . . ? P4 Ir1 P3 70.60(10) . . ? P1 Ir1 P3 113.87(11) . . ? P2 Ir1 Cl1 99.01(10) . . ? P4 Ir1 Cl1 89.81(10) . . ? P1 Ir1 Cl1 97.57(10) . . ? P3 Ir1 Cl1 84.42(10) . . ? C8 P1 C2 104.4(6) . . ? C8 P1 C1 106.3(6) . . ? C2 P1 C1 106.3(6) . . ? C8 P1 Ir1 121.6(4) . . ? C2 P1 Ir1 122.5(4) . . ? C1 P1 Ir1 92.7(3) . . ? C14 P2 C1 107.8(6) . . ? C14 P2 C20 105.6(6) . . ? C1 P2 C20 108.6(5) . . ? C14 P2 Ir1 119.4(4) . . ? C1 P2 Ir1 94.8(4) . . ? C20 P2 Ir1 119.3(4) . . ? C33 P3 C26 109.0(6) . . ? C33 P3 C27 102.0(6) . . ? C26 P3 C27 106.1(6) . . ? C33 P3 Ir1 117.6(4) . . ? C26 P3 Ir1 94.0(4) . . ? C27 P3 Ir1 126.5(4) . . ? C33 P3 P4 110.5(4) . . ? C26 P3 P4 43.1(4) . . ? C27 P3 P4 140.8(4) . . ? Ir1 P3 P4 54.12(9) . . ? C45 P4 C39 105.3(6) . . ? C45 P4 C26 112.1(5) . . ? C39 P4 C26 104.0(6) . . ? C45 P4 Ir1 118.9(4) . . ? C39 P4 Ir1 120.4(4) . . ? C26 P4 Ir1 94.7(4) . . ? C45 P4 P3 142.3(4) . . ? C39 P4 P3 108.1(4) . . ? C26 P4 P3 42.7(3) . . ? Ir1 P4 P3 55.28(9) . . ? P2 C1 P1 95.1(5) . . ? C7 C2 C3 119.9(12) . . ? C7 C2 P1 121.8(10) . . ? C3 C2 P1 118.3(10) . . ? C4 C3 C2 119.2(13) . . ? C3 C4 C5 120.5(14) . . ? C6 C5 C4 120.2(13) . . ? C5 C6 C7 121.7(14) . . ? C2 C7 C6 118.6(14) . . ? C13 C8 C9 121.1(12) . . ? C13 C8 P1 120.7(11) . . ? C9 C8 P1 118.2(10) . . ? C8 C9 C10 117.9(15) . . ? C11 C10 C9 119.3(17) . . ? C10 C11 C12 121.3(16) . . ? C13 C12 C11 119.2(17) . . ? C12 C13 C8 121.2(16) . . ? C19 C14 C15 119.1(11) . . ? C19 C14 P2 118.9(9) . . ? C15 C14 P2 121.9(9) . . ? C16 C15 C14 119.4(13) . . ? C15 C16 C17 120.1(13) . . ? C18 C17 C16 119.7(13) . . ? C19 C18 C17 120.0(12) . . ? C18 C19 C14 121.5(12) . . ? C21 C20 C25 121.0(12) . . ? C21 C20 P2 121.3(10) . . ? C25 C20 P2 117.6(10) . . ? C20 C21 C22 119.0(13) . . ? C23 C22 C21 120.4(14) . . ? C22 C23 C24 121.1(13) . . ? C23 C24 C25 119.5(14) . . ? C20 C25 C24 119.0(13) . . ? P3 C26 P4 94.2(5) . . ? C28 C27 C32 120.1(13) . . ? C28 C27 P3 120.4(11) . . ? C32 C27 P3 119.1(10) . . ? C27 C28 C29 120.2(18) . . ? C28 C29 C30 119.1(19) . . ? C31 C30 C29 119.8(16) . . ? C30 C31 C32 120.6(15) . . ? C31 C32 C27 120.1(15) . . ? C38 C33 C34 119.7(12) . . ? C38 C33 P3 117.4(10) . . ? C34 C33 P3 122.8(10) . . ? C33 C34 C35 120.3(14) . . ? C34 C35 C36 119.2(14) . . ? C37 C36 C35 119.8(14) . . ? C36 C37 C38 120.7(16) . . ? C33 C38 C37 120.2(14) . . ? C44 C39 C40 119.4(11) . . ? C44 C39 P4 122.3(9) . . ? C40 C39 P4 118.2(10) . . ? C41 C40 C39 119.4(13) . . ? C40 C41 C42 120.9(14) . . ? C43 C42 C41 118.5(13) . . ? C44 C43 C42 121.7(14) . . ? C43 C44 C39 120.0(12) . . ? C50 C45 C46 118.3(11) . . ? C50 C45 P4 119.7(9) . . ? C46 C45 P4 121.3(9) . . ? C47 C46 C45 121.9(12) . . ? C46 C47 C48 119.3(13) . . ? C47 C48 C49 121.4(13) . . ? C48 C49 C50 119.2(14) . . ? C45 C50 C49 119.9(13) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.614 _refine_diff_density_min -1.599 _refine_diff_density_rms 0.336