data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Ken-ichi Fujita' 'Mitsuru Nonogawa' 'Yoshinori Takahashi' 'Ryohei Yamaguchi' _publ_contact_author_name 'Ken-ichi Fujita' _publ_contact_author_address ; Graduate School of Human and Environmental Studies Kyoto University Yoshida Sakyo-ku Kyoto 606-8501 JAPAN ; _publ_contact_author_email FUJITAK@KAGAKU.MBOX.MEDIA.KYOTO-U.AC.JP _publ_requested_journal 'Dalton Transactions' _publ_section_title ; C-H activation on a diphosphine and hydrido-bridged diiridium complex. Generation and detection of an active Ir(II)-Ir(II) species [(Cp*Ir)2(mu-dmpm)(mu-H)]+ ; data__complex3 _database_code_depnum_ccdc_archive 'CCDC 680332' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C25 H46 Ir2 P2 ' _chemical_formula_moiety 'C25 H46 Ir2 P2 ' _chemical_formula_weight 793.03 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 8.505(6) _cell_length_b 16.341(7) _cell_length_c 20.088(4) _cell_angle_alpha 90.0000 _cell_angle_beta 96.95(3) _cell_angle_gamma 90.0000 _cell_volume 2771(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 14.7 _cell_measurement_theta_max 14.9 _cell_measurement_temperature 203.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.30 _exptl_crystal_density_diffrn 1.901 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520.00 _exptl_absorpt_coefficient_mu 9.746 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.023 _exptl_absorpt_correction_T_max 0.054 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 6744 _diffrn_reflns_av_R_equivalents 0.064 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.979 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_standards_number 3 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6213 _reflns_number_gt 5326 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.0738 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 5326 _refine_ls_number_parameters 306 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0048Fo^2^ + 1.0000\s(Fo^2^)]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 3.54 _refine_diff_density_min -4.36 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Ir Ir -1.444 7.990 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.79117(3) 0.74445(2) 0.424620(10) 0.01837(9) Uani 1.00 1 d . . . Ir(2) Ir 0.59345(3) 0.81746(2) 0.322460(10) 0.01746(9) Uani 1.00 1 d . . . P(1) P 0.9088(2) 0.68521(13) 0.34563(12) 0.0250(5) Uani 1.00 1 d . . . P(2) P 0.5846(2) 0.69586(13) 0.27593(12) 0.0278(5) Uani 1.00 1 d . . . C(1) C 0.7502(10) 0.6449(6) 0.5012(4) 0.032(2) Uani 1.00 1 d . . . C(2) C 0.6148(10) 0.6948(5) 0.4940(4) 0.028(2) Uani 1.00 1 d . . . C(3) C 0.6544(11) 0.7756(6) 0.5116(4) 0.033(2) Uani 1.00 1 d . . . C(4) C 0.8189(13) 0.7778(6) 0.5337(5) 0.040(2) Uani 1.00 1 d . . . C(5) C 0.8837(11) 0.6976(6) 0.5269(5) 0.037(2) Uani 1.00 1 d . . . C(6) C 0.7582(18) 0.5544(6) 0.4957(5) 0.062(3) Uani 1.00 1 d . . . C(7) C 0.4463(13) 0.6651(8) 0.4782(5) 0.055(3) Uani 1.00 1 d . . . C(8) C 0.5390(14) 0.8436(7) 0.5157(5) 0.050(3) Uani 1.00 1 d . . . C(9) C 0.9129(16) 0.8475(8) 0.5629(5) 0.060(3) Uani 1.00 1 d . . . C(10) C 1.0436(17) 0.6682(10) 0.5505(6) 0.072(4) Uani 1.00 1 d . . . C(11) C 0.4697(8) 0.9386(4) 0.3212(4) 0.0222(18) Uani 1.00 1 d . . . C(12) C 0.4652(10) 0.9092(4) 0.2530(4) 0.027(2) Uani 1.00 1 d . . . C(13) C 0.6308(10) 0.9068(5) 0.2389(4) 0.032(2) Uani 1.00 1 d . . . C(14) C 0.7287(9) 0.9333(4) 0.2958(4) 0.0251(19) Uani 1.00 1 d . . . C(15) C 0.6281(9) 0.9518(4) 0.3476(4) 0.0230(18) Uani 1.00 1 d . . . C(16) C 0.3296(11) 0.9567(6) 0.3572(5) 0.040(2) Uani 1.00 1 d . . . C(17) C 0.3201(12) 0.8965(6) 0.2036(5) 0.041(2) Uani 1.00 1 d . . . C(18) C 0.6770(14) 0.8925(7) 0.1700(5) 0.051(3) Uani 1.00 1 d . . . C(19) C 0.9010(11) 0.9525(6) 0.3005(5) 0.040(2) Uani 1.00 1 d . . . C(20) C 0.6940(12) 0.9924(6) 0.4123(5) 0.044(2) Uani 1.00 1 d . . . C(21) C 1.0260(14) 0.5937(7) 0.3671(5) 0.050(3) Uani 1.00 1 d . . . C(22) C 1.0577(17) 0.7436(7) 0.3089(7) 0.059(4) Uani 1.00 1 d . . . C(23) C 0.7765(14) 0.6481(7) 0.2702(5) 0.052(3) Uani 1.00 1 d . . . C(24) C 0.4858(16) 0.6131(6) 0.3159(6) 0.056(3) Uani 1.00 1 d . . . C(25) C 0.4956(19) 0.6877(7) 0.1884(6) 0.064(4) Uani 1.00 1 d . . . H(1) H 0.6578 0.5331 0.4779 0.075 Uiso 1.00 1 c R . . H(2) H 0.7889 0.5315 0.5388 0.075 Uiso 1.00 1 c R . . H(3) H 0.8345 0.5406 0.4667 0.075 Uiso 1.00 1 c R . . H(4) H 0.3743 0.7093 0.4798 0.067 Uiso 1.00 1 c R . . H(5) H 0.4269 0.6252 0.5107 0.067 Uiso 1.00 1 c R . . H(6) H 0.4323 0.6411 0.4349 0.067 Uiso 1.00 1 c R . . H(7) H 0.5931 0.8910 0.5338 0.061 Uiso 1.00 1 c R . . H(8) H 0.4623 0.8275 0.5438 0.062 Uiso 1.00 1 c R . . H(9) H 0.4878 0.8555 0.4721 0.061 Uiso 1.00 1 c R . . H(10) H 1.0188 0.8306 0.5764 0.070 Uiso 1.00 1 c R . . H(11) H 0.8676 0.8675 0.6007 0.070 Uiso 1.00 1 c R . . H(12) H 0.9124 0.8896 0.5303 0.070 Uiso 1.00 1 c R . . H(13) H 1.0501 0.6111 0.5424 0.085 Uiso 1.00 1 c R . . H(14) H 1.0667 0.6784 0.5972 0.085 Uiso 1.00 1 c R . . H(15) H 1.1179 0.6962 0.5271 0.085 Uiso 1.00 1 c R . . H(16) H 0.2346 0.9452 0.3287 0.048 Uiso 1.00 1 c R . . H(17) H 0.3313 1.0128 0.3695 0.048 Uiso 1.00 1 c R . . H(18) H 0.3342 0.9237 0.3963 0.048 Uiso 1.00 1 c R . . H(19) H 0.3493 0.8796 0.1615 0.047 Uiso 1.00 1 c R . . H(20) H 0.2623 0.9463 0.1981 0.047 Uiso 1.00 1 c R . . H(21) H 0.2562 0.8555 0.2203 0.047 Uiso 1.00 1 c R . . H(22) H 0.7890 0.8959 0.1723 0.062 Uiso 1.00 1 c R . . H(23) H 0.6299 0.9330 0.1400 0.062 Uiso 1.00 1 c R . . H(24) H 0.6428 0.8398 0.1543 0.062 Uiso 1.00 1 c R . . H(25) H 0.9348 0.9756 0.3432 0.049 Uiso 1.00 1 c R . . H(26) H 0.9192 0.9905 0.2664 0.049 Uiso 1.00 1 c R . . H(27) H 0.9589 0.9037 0.2951 0.049 Uiso 1.00 1 c R . . H(28) H 0.6103 1.0030 0.4384 0.050 Uiso 1.00 1 c R . . H(29) H 0.7434 1.0425 0.4028 0.050 Uiso 1.00 1 c R . . H(30) H 0.7696 0.9574 0.4365 0.050 Uiso 1.00 1 c R . . H(31) H 1.1325 0.6084 0.3821 0.061 Uiso 1.00 1 c R . . H(32) H 1.0235 0.5599 0.3285 0.061 Uiso 1.00 1 c R . . H(33) H 0.9826 0.5648 0.4016 0.061 Uiso 1.00 1 c R . . H(34) H 1.0086 0.7732 0.2713 0.075 Uiso 1.00 1 c R . . H(35) H 1.1347 0.7074 0.2949 0.075 Uiso 1.00 1 c R . . H(36) H 1.1075 0.7808 0.3412 0.075 Uiso 1.00 1 c R . . H(37) H 0.8166 0.6657 0.2304 0.064 Uiso 1.00 1 c R . . H(38) H 0.7681 0.5901 0.2700 0.063 Uiso 1.00 1 c R . . H(39) H 0.5602 0.5858 0.3474 0.066 Uiso 1.00 1 c R . . H(40) H 0.4415 0.5752 0.2830 0.066 Uiso 1.00 1 c R . . H(41) H 0.4039 0.6358 0.3384 0.066 Uiso 1.00 1 c R . . H(42) H 0.3852 0.6775 0.1867 0.072 Uiso 1.00 1 c R . . H(43) H 0.5443 0.6438 0.1675 0.072 Uiso 1.00 1 c R . . H(44) H 0.5119 0.7373 0.1655 0.072 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ir(1) 0.0207(2) 0.01969(19) 0.0145(2) 0.00453(10) 0.00120(13) -0.00027(10) Ir(2) 0.02192(19) 0.01628(18) 0.01343(19) 0.00029(10) -0.00094(12) -0.00016(10) P(1) 0.0269(10) 0.0256(10) 0.0242(11) 0.0063(7) 0.0098(8) -0.0022(8) P(2) 0.0364(11) 0.0226(9) 0.0228(11) 0.0019(8) -0.0037(9) -0.0053(8) C(1) 0.033(4) 0.040(4) 0.020(4) 0.008(3) -0.002(3) 0.005(3) C(2) 0.031(4) 0.037(4) 0.016(4) 0.000(3) 0.008(3) 0.009(3) C(3) 0.043(5) 0.044(5) 0.014(4) 0.010(4) 0.019(3) -0.007(3) C(4) 0.060(6) 0.035(5) 0.025(5) -0.001(4) 0.001(4) 0.003(4) C(5) 0.027(4) 0.048(5) 0.035(5) 0.011(3) 0.004(3) 0.002(4) C(6) 0.111(10) 0.045(6) 0.033(5) 0.022(6) 0.025(6) 0.021(5) C(7) 0.048(6) 0.087(8) 0.034(6) -0.017(6) 0.018(4) 0.010(6) C(8) 0.065(7) 0.058(6) 0.031(5) 0.026(5) 0.021(5) 0.005(5) C(9) 0.076(8) 0.074(8) 0.026(5) -0.007(7) -0.009(5) -0.008(5) C(10) 0.072(8) 0.113(12) 0.027(6) 0.044(8) -0.007(5) 0.016(6) C(11) 0.017(3) 0.014(3) 0.035(4) 0.007(2) 0.001(2) 0.008(3) C(12) 0.037(4) 0.015(3) 0.027(4) 0.006(3) -0.006(3) 0.011(3) C(13) 0.036(4) 0.035(4) 0.024(4) 0.006(3) 0.002(3) 0.015(3) C(14) 0.033(4) 0.016(3) 0.026(4) 0.001(3) 0.000(3) 0.002(3) C(15) 0.031(3) 0.011(3) 0.026(4) 0.001(2) 0.002(3) 0.002(2) C(16) 0.042(5) 0.037(5) 0.041(5) 0.004(4) 0.012(4) 0.002(4) C(17) 0.044(5) 0.045(5) 0.030(5) 0.001(4) -0.015(4) 0.005(4) C(18) 0.063(7) 0.057(6) 0.033(5) 0.018(5) 0.004(5) 0.008(5) C(19) 0.037(4) 0.039(5) 0.045(6) -0.004(4) 0.009(4) 0.003(4) C(20) 0.052(5) 0.038(5) 0.036(5) 0.014(4) -0.015(4) -0.012(4) C(21) 0.063(6) 0.048(6) 0.042(6) 0.023(5) 0.024(5) 0.008(5) C(22) 0.075(8) 0.038(6) 0.074(9) 0.007(5) 0.049(7) 0.007(5) C(23) 0.065(7) 0.056(6) 0.038(6) 0.012(5) 0.020(5) -0.030(5) C(24) 0.097(9) 0.027(5) 0.043(6) -0.021(5) -0.001(6) -0.007(4) C(25) 0.101(10) 0.045(6) 0.036(6) 0.002(6) -0.040(7) -0.016(4) #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction CrystalStructure _computing_structure_solution 'DIRDIF99 (PATTY)' _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ir(1) Ir(2) 2.7618(3) yes . . Ir(1) P(1) 2.200(2) yes . . Ir(1) C(1) 2.295(9) yes . . Ir(1) C(2) 2.314(9) yes . . Ir(1) C(3) 2.271(9) yes . . Ir(1) C(4) 2.243(10) yes . . Ir(1) C(5) 2.244(10) yes . . Ir(2) P(2) 2.193(2) yes . . Ir(2) C(11) 2.241(7) yes . . Ir(2) C(12) 2.239(7) yes . . Ir(2) C(13) 2.276(9) yes . . Ir(2) C(14) 2.311(8) yes . . Ir(2) C(15) 2.263(7) yes . . P(1) C(21) 1.819(11) yes . . P(1) C(22) 1.812(14) yes . . P(1) C(23) 1.876(11) yes . . P(2) C(23) 1.825(12) yes . . P(2) C(24) 1.828(12) yes . . P(2) C(25) 1.834(12) yes . . C(1) C(2) 1.405(12) yes . . C(1) C(5) 1.469(13) yes . . C(1) C(6) 1.485(14) yes . . C(2) C(3) 1.397(13) yes . . C(2) C(7) 1.510(14) yes . . C(3) C(4) 1.416(14) yes . . C(3) C(8) 1.492(16) yes . . C(4) C(5) 1.434(14) yes . . C(4) C(9) 1.471(17) yes . . C(5) C(10) 1.466(17) yes . . C(11) C(12) 1.449(12) yes . . C(11) C(15) 1.404(10) yes . . C(11) C(16) 1.496(13) yes . . C(12) C(13) 1.470(12) yes . . C(12) C(17) 1.501(12) yes . . C(13) C(14) 1.398(11) yes . . C(13) C(18) 1.502(15) yes . . C(14) C(15) 1.457(12) yes . . C(14) C(19) 1.491(12) yes . . C(15) C(20) 1.506(12) yes . . C(6) H(1) 0.950 no . . C(6) H(2) 0.950 no . . C(6) H(3) 0.950 no . . C(7) H(4) 0.950 no . . C(7) H(5) 0.950 no . . C(7) H(6) 0.950 no . . C(8) H(7) 0.950 no . . C(8) H(8) 0.950 no . . C(8) H(9) 0.950 no . . C(9) H(10) 0.950 no . . C(9) H(11) 0.950 no . . C(9) H(12) 0.950 no . . C(10) H(13) 0.950 no . . C(10) H(14) 0.950 no . . C(10) H(15) 0.950 no . . C(16) H(16) 0.950 no . . C(16) H(17) 0.950 no . . C(16) H(18) 0.950 no . . C(17) H(19) 0.950 no . . C(17) H(20) 0.950 no . . C(17) H(21) 0.950 no . . C(18) H(22) 0.950 no . . C(18) H(23) 0.950 no . . C(18) H(24) 0.950 no . . C(19) H(25) 0.950 no . . C(19) H(26) 0.950 no . . C(19) H(27) 0.950 no . . C(20) H(28) 0.950 no . . C(20) H(29) 0.950 no . . C(20) H(30) 0.950 no . . C(21) H(31) 0.950 no . . C(21) H(32) 0.950 no . . C(21) H(33) 0.950 no . . C(22) H(34) 0.950 no . . C(22) H(35) 0.950 no . . C(22) H(36) 0.950 no . . C(23) H(37) 0.950 no . . C(23) H(38) 0.950 no . . C(24) H(39) 0.950 no . . C(24) H(40) 0.950 no . . C(24) H(41) 0.950 no . . C(25) H(42) 0.950 no . . C(25) H(43) 0.950 no . . C(25) H(44) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Ir(2) Ir(1) P(1) 86.75(5) yes . . . Ir(2) Ir(1) C(1) 132.5(2) yes . . . Ir(2) Ir(1) C(2) 102.6(2) yes . . . Ir(2) Ir(1) C(3) 98.8(2) yes . . . Ir(2) Ir(1) C(4) 127.1(2) yes . . . Ir(2) Ir(1) C(5) 160.4(2) yes . . . P(1) Ir(1) C(1) 106.9(2) yes . . . P(1) Ir(1) C(2) 131.6(2) yes . . . P(1) Ir(1) C(3) 166.8(2) yes . . . P(1) Ir(1) C(4) 143.9(2) yes . . . P(1) Ir(1) C(5) 111.7(2) yes . . . C(1) Ir(1) C(2) 35.5(3) yes . . . C(1) Ir(1) C(3) 60.6(3) yes . . . C(1) Ir(1) C(4) 61.6(3) yes . . . C(1) Ir(1) C(5) 37.8(3) yes . . . C(2) Ir(1) C(3) 35.5(3) yes . . . C(2) Ir(1) C(4) 59.7(3) yes . . . C(2) Ir(1) C(5) 60.7(3) yes . . . C(3) Ir(1) C(4) 36.6(3) yes . . . C(3) Ir(1) C(5) 61.8(3) yes . . . C(4) Ir(1) C(5) 37.3(3) yes . . . Ir(1) Ir(2) P(2) 84.94(5) yes . . . Ir(1) Ir(2) C(11) 129.3(2) yes . . . Ir(1) Ir(2) C(12) 163.5(2) yes . . . Ir(1) Ir(2) C(13) 134.3(2) yes . . . Ir(1) Ir(2) C(14) 104.53(19) yes . . . Ir(1) Ir(2) C(15) 101.65(19) yes . . . P(2) Ir(2) C(11) 143.49(19) yes . . . P(2) Ir(2) C(12) 110.6(2) yes . . . P(2) Ir(2) C(13) 105.5(2) yes . . . P(2) Ir(2) C(14) 129.4(2) yes . . . P(2) Ir(2) C(15) 166.0(2) yes . . . C(11) Ir(2) C(12) 37.7(3) yes . . . C(11) Ir(2) C(13) 62.1(3) yes . . . C(11) Ir(2) C(14) 61.3(2) yes . . . C(11) Ir(2) C(15) 36.3(2) yes . . . C(12) Ir(2) C(13) 38.0(3) yes . . . C(12) Ir(2) C(14) 61.7(2) yes . . . C(12) Ir(2) C(15) 62.0(2) yes . . . C(13) Ir(2) C(14) 35.5(2) yes . . . C(13) Ir(2) C(15) 61.1(3) yes . . . C(14) Ir(2) C(15) 37.1(3) yes . . . Ir(1) P(1) C(21) 118.3(3) yes . . . Ir(1) P(1) C(22) 117.6(4) yes . . . Ir(1) P(1) C(23) 116.4(3) yes . . . C(21) P(1) C(22) 98.0(5) yes . . . C(21) P(1) C(23) 100.6(5) yes . . . C(22) P(1) C(23) 102.8(6) yes . . . Ir(2) P(2) C(23) 115.4(3) yes . . . Ir(2) P(2) C(24) 118.5(3) yes . . . Ir(2) P(2) C(25) 117.6(3) yes . . . C(23) P(2) C(24) 100.0(5) yes . . . C(23) P(2) C(25) 100.2(6) yes . . . C(24) P(2) C(25) 102.1(5) yes . . . Ir(1) C(1) C(2) 73.0(5) yes . . . Ir(1) C(1) C(5) 69.3(5) yes . . . Ir(1) C(1) C(6) 130.1(7) yes . . . C(2) C(1) C(5) 106.5(8) yes . . . C(2) C(1) C(6) 128.0(9) yes . . . C(5) C(1) C(6) 124.8(9) yes . . . Ir(1) C(2) C(1) 71.5(5) yes . . . Ir(1) C(2) C(3) 70.6(5) yes . . . Ir(1) C(2) C(7) 130.9(6) yes . . . C(1) C(2) C(3) 110.7(7) yes . . . C(1) C(2) C(7) 125.4(9) yes . . . C(3) C(2) C(7) 123.4(9) yes . . . Ir(1) C(3) C(2) 73.9(5) yes . . . Ir(1) C(3) C(4) 70.6(5) yes . . . Ir(1) C(3) C(8) 127.6(6) yes . . . C(2) C(3) C(4) 107.6(8) yes . . . C(2) C(3) C(8) 125.3(8) yes . . . C(4) C(3) C(8) 126.5(9) yes . . . Ir(1) C(4) C(3) 72.8(5) yes . . . Ir(1) C(4) C(5) 71.4(5) yes . . . Ir(1) C(4) C(9) 124.4(7) yes . . . C(3) C(4) C(5) 108.8(8) yes . . . C(3) C(4) C(9) 127.8(10) yes . . . C(5) C(4) C(9) 123.3(10) yes . . . Ir(1) C(5) C(1) 73.0(5) yes . . . Ir(1) C(5) C(4) 71.3(5) yes . . . Ir(1) C(5) C(10) 128.1(8) yes . . . C(1) C(5) C(4) 106.3(8) yes . . . C(1) C(5) C(10) 124.6(10) yes . . . C(4) C(5) C(10) 128.4(10) yes . . . Ir(2) C(11) C(12) 71.0(4) yes . . . Ir(2) C(11) C(15) 72.7(4) yes . . . Ir(2) C(11) C(16) 124.7(5) yes . . . C(12) C(11) C(15) 108.8(7) yes . . . C(12) C(11) C(16) 126.3(7) yes . . . C(15) C(11) C(16) 124.9(7) yes . . . Ir(2) C(12) C(11) 71.2(4) yes . . . Ir(2) C(12) C(13) 72.4(4) yes . . . Ir(2) C(12) C(17) 128.3(6) yes . . . C(11) C(12) C(13) 106.0(6) yes . . . C(11) C(12) C(17) 126.6(8) yes . . . C(13) C(12) C(17) 126.8(8) yes . . . Ir(2) C(13) C(12) 69.6(4) yes . . . Ir(2) C(13) C(14) 73.6(5) yes . . . Ir(2) C(13) C(18) 131.0(7) yes . . . C(12) C(13) C(14) 108.9(7) yes . . . C(12) C(13) C(18) 123.0(8) yes . . . C(14) C(13) C(18) 127.2(8) yes . . . Ir(2) C(14) C(13) 70.9(4) yes . . . Ir(2) C(14) C(15) 69.7(4) yes . . . Ir(2) C(14) C(19) 132.1(5) yes . . . C(13) C(14) C(15) 107.8(7) yes . . . C(13) C(14) C(19) 126.9(8) yes . . . C(15) C(14) C(19) 124.6(7) yes . . . Ir(2) C(15) C(11) 71.0(4) yes . . . Ir(2) C(15) C(14) 73.2(4) yes . . . Ir(2) C(15) C(20) 130.2(5) yes . . . C(11) C(15) C(14) 108.5(7) yes . . . C(11) C(15) C(20) 129.3(8) yes . . . C(14) C(15) C(20) 121.3(7) yes . . . P(1) C(23) P(2) 105.3(6) yes . . . C(1) C(6) H(1) 110.2 no . . . C(1) C(6) H(2) 109.5 no . . . C(1) C(6) H(3) 108.8 no . . . H(1) C(6) H(2) 109.5 no . . . H(1) C(6) H(3) 109.5 no . . . H(2) C(6) H(3) 109.5 no . . . C(2) C(7) H(4) 110.4 no . . . C(2) C(7) H(5) 108.4 no . . . C(2) C(7) H(6) 109.6 no . . . H(4) C(7) H(5) 109.5 no . . . H(4) C(7) H(6) 109.5 no . . . H(5) C(7) H(6) 109.5 no . . . C(3) C(8) H(7) 109.7 no . . . C(3) C(8) H(8) 109.2 no . . . C(3) C(8) H(9) 109.5 no . . . H(7) C(8) H(8) 109.5 no . . . H(7) C(8) H(9) 109.5 no . . . H(8) C(8) H(9) 109.5 no . . . C(4) C(9) H(10) 109.8 no . . . C(4) C(9) H(11) 109.4 no . . . C(4) C(9) H(12) 109.2 no . . . H(10) C(9) H(11) 109.5 no . . . H(10) C(9) H(12) 109.5 no . . . H(11) C(9) H(12) 109.5 no . . . C(5) C(10) H(13) 109.8 no . . . C(5) C(10) H(14) 109.5 no . . . C(5) C(10) H(15) 109.1 no . . . H(13) C(10) H(14) 109.5 no . . . H(13) C(10) H(15) 109.5 no . . . H(14) C(10) H(15) 109.5 no . . . C(11) C(16) H(16) 109.8 no . . . C(11) C(16) H(17) 109.2 no . . . C(11) C(16) H(18) 109.4 no . . . H(16) C(16) H(17) 109.5 no . . . H(16) C(16) H(18) 109.5 no . . . H(17) C(16) H(18) 109.5 no . . . C(12) C(17) H(19) 110.2 no . . . C(12) C(17) H(20) 109.3 no . . . C(12) C(17) H(21) 108.8 no . . . H(19) C(17) H(20) 109.5 no . . . H(19) C(17) H(21) 109.5 no . . . H(20) C(17) H(21) 109.5 no . . . C(13) C(18) H(22) 108.6 no . . . C(13) C(18) H(23) 109.8 no . . . C(13) C(18) H(24) 110.0 no . . . H(22) C(18) H(23) 109.5 no . . . H(22) C(18) H(24) 109.5 no . . . H(23) C(18) H(24) 109.5 no . . . C(14) C(19) H(25) 109.2 no . . . C(14) C(19) H(26) 109.6 no . . . C(14) C(19) H(27) 109.6 no . . . H(25) C(19) H(26) 109.5 no . . . H(25) C(19) H(27) 109.5 no . . . H(26) C(19) H(27) 109.5 no . . . C(15) C(20) H(28) 109.4 no . . . C(15) C(20) H(29) 109.5 no . . . C(15) C(20) H(30) 109.5 no . . . H(28) C(20) H(29) 109.5 no . . . H(28) C(20) H(30) 109.5 no . . . H(29) C(20) H(30) 109.5 no . . . P(1) C(21) H(31) 110.0 no . . . P(1) C(21) H(32) 109.1 no . . . P(1) C(21) H(33) 109.3 no . . . H(31) C(21) H(32) 109.5 no . . . H(31) C(21) H(33) 109.5 no . . . H(32) C(21) H(33) 109.5 no . . . P(1) C(22) H(34) 109.3 no . . . P(1) C(22) H(35) 109.5 no . . . P(1) C(22) H(36) 109.6 no . . . H(34) C(22) H(35) 109.5 no . . . H(34) C(22) H(36) 109.5 no . . . H(35) C(22) H(36) 109.5 no . . . P(1) C(23) H(37) 109.9 no . . . P(1) C(23) H(38) 111.3 no . . . P(2) C(23) H(37) 109.8 no . . . P(2) C(23) H(38) 111.0 no . . . H(37) C(23) H(38) 109.5 no . . . P(2) C(24) H(39) 109.6 no . . . P(2) C(24) H(40) 109.9 no . . . P(2) C(24) H(41) 108.8 no . . . H(39) C(24) H(40) 109.5 no . . . H(39) C(24) H(41) 109.5 no . . . H(40) C(24) H(41) 109.5 no . . . P(2) C(25) H(42) 109.8 no . . . P(2) C(25) H(43) 109.1 no . . . P(2) C(25) H(44) 109.6 no . . . H(42) C(25) H(43) 109.5 no . . . H(42) C(25) H(44) 109.5 no . . . H(43) C(25) H(44) 109.5 no . . . #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== data__complex8 _database_code_depnum_ccdc_archive 'CCDC 680333' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C26 H45 F3 Ir2 O3 P2 S ' _chemical_formula_moiety 'C26 H45 F3 Ir2 O3 P2 S ' _chemical_formula_weight 941.08 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 9.771(3) _cell_length_b 10.880(3) _cell_length_c 15.431(3) _cell_angle_alpha 80.236(19) _cell_angle_beta 83.09(2) _cell_angle_gamma 86.91(3) _cell_volume 1604.0(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.7 _cell_measurement_theta_max 14.9 _cell_measurement_temperature 296.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_diffrn 1.948 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904.00 _exptl_absorpt_coefficient_mu 8.518 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.063 _exptl_absorpt_correction_T_max 0.078 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 7637 _diffrn_reflns_av_R_equivalents 0.020 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number 3 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7354 _reflns_number_gt 5063 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0497 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 5063 _refine_ls_number_parameters 377 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0016Fo^2^ + 1.0000\s(Fo^2^)]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 2.36 _refine_diff_density_min -1.70 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; F F 0.017 0.010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ir Ir -1.444 7.990 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.66137(3) 0.16787(3) 0.16242(2) 0.03769(8) Uani 1.00 1 d . . . Ir(2) Ir 0.58550(3) 0.23142(3) 0.34551(2) 0.03986(9) Uani 1.00 1 d . . . S(1) S 1.0143(3) 0.3123(3) 0.7784(2) 0.0867(11) Uani 1.00 1 d . . . P(1) P 0.8314(2) 0.3061(2) 0.13932(15) 0.0483(6) Uani 1.00 1 d . . . P(2) P 0.8071(2) 0.1731(2) 0.31764(14) 0.0424(5) Uani 1.00 1 d . . . F(1) F 0.9396(14) 0.3708(12) 0.6215(7) 0.181(5) Uani 1.00 1 d . . . F(2) F 0.9869(14) 0.1799(11) 0.6582(7) 0.192(6) Uani 1.00 1 d . . . F(3) F 0.7975(10) 0.2631(13) 0.7123(8) 0.170(5) Uani 1.00 1 d . . . O(1) O 0.9374(13) 0.4179(9) 0.8055(9) 0.139(5) Uani 1.00 1 d . . . O(2) O 1.1507(11) 0.3339(15) 0.7385(9) 0.185(6) Uani 1.00 1 d . . . O(3) O 0.9993(10) 0.1986(9) 0.8414(6) 0.112(3) Uani 1.00 1 d . . . C(1) C 0.5778(10) -0.0034(8) 0.1274(6) 0.054(2) Uani 1.00 1 d . . . C(2) C 0.4638(9) 0.0801(9) 0.1453(6) 0.056(2) Uani 1.00 1 d . . . C(3) C 0.4844(10) 0.1934(9) 0.0828(6) 0.058(2) Uani 1.00 1 d . . . C(4) C 0.6055(9) 0.1818(9) 0.0262(5) 0.055(2) Uani 1.00 1 d . . . C(5) C 0.6705(10) 0.0573(9) 0.0559(5) 0.056(2) Uani 1.00 1 d . . . C(6) C 0.5987(15) -0.1324(9) 0.1742(8) 0.087(4) Uani 1.00 1 d . . . C(7) C 0.3422(11) 0.0513(12) 0.2154(7) 0.091(4) Uani 1.00 1 d . . . C(8) C 0.3814(12) 0.3010(10) 0.0735(9) 0.087(4) Uani 1.00 1 d . . . C(9) C 0.6570(14) 0.2699(12) -0.0536(7) 0.092(4) Uani 1.00 1 d . . . C(10) C 0.7940(12) -0.0028(11) 0.0113(7) 0.084(4) Uani 1.00 1 d . . . C(11) C 0.5919(10) 0.3870(9) 0.4246(6) 0.062(3) Uani 1.00 1 d . . . C(12) C 0.5328(12) 0.2716(9) 0.4792(6) 0.067(3) Uani 1.00 1 d . . . C(13) C 0.4099(11) 0.2503(9) 0.4477(7) 0.064(3) Uani 1.00 1 d . . . C(14) C 0.3880(9) 0.3403(9) 0.3742(7) 0.060(2) Uani 1.00 1 d . . . C(15) C 0.5019(11) 0.4268(7) 0.3598(7) 0.060(2) Uani 1.00 1 d . . . C(16) C 0.7143(12) 0.4530(11) 0.4399(8) 0.093(4) Uani 1.00 1 d . . . C(17) C 0.5923(17) 0.2015(14) 0.5632(7) 0.109(5) Uani 1.00 1 d . . . C(18) C 0.3128(12) 0.1487(11) 0.4918(8) 0.093(4) Uani 1.00 1 d . . . C(19) C 0.2614(11) 0.3579(11) 0.3276(9) 0.087(4) Uani 1.00 1 d . . . C(20) C 0.5117(15) 0.5439(10) 0.2930(9) 0.101(4) Uani 1.00 1 d . . . C(21) C 0.9783(11) 0.2757(14) 0.0615(7) 0.092(4) Uani 1.00 1 d . . . C(22) C 0.7862(13) 0.4667(9) 0.1015(8) 0.088(4) Uani 1.00 1 d . . . C(23) C 0.9046(9) 0.2967(8) 0.2449(5) 0.054(2) Uani 1.00 1 d . . . C(24) C 0.9167(9) 0.1210(10) 0.4056(6) 0.060(2) Uani 1.00 1 d . . . C(25) C 0.8059(8) 0.0654(7) 0.2450(5) 0.048(2) Uani 1.00 1 d . . . C(26) C 0.9340(16) 0.2763(15) 0.6893(11) 0.105(5) Uani 1.00 1 d . . . H(1) H 0.6797 -0.1685 0.1467 0.108 Uiso 1.00 1 c R . . H(2) H 0.5216 -0.1803 0.1709 0.108 Uiso 1.00 1 c R . . H(3) H 0.6091 -0.1311 0.2344 0.108 Uiso 1.00 1 c R . . H(4) H 0.3542 -0.0306 0.2472 0.110 Uiso 1.00 1 c R . . H(5) H 0.2601 0.0565 0.1875 0.110 Uiso 1.00 1 c R . . H(6) H 0.3357 0.1098 0.2551 0.110 Uiso 1.00 1 c R . . H(7) H 0.3059 0.2864 0.1184 0.106 Uiso 1.00 1 c R . . H(8) H 0.3488 0.3104 0.0171 0.106 Uiso 1.00 1 c R . . H(9) H 0.4251 0.3748 0.0788 0.106 Uiso 1.00 1 c R . . H(10) H 0.5970 0.3418 -0.0584 0.110 Uiso 1.00 1 c R . . H(11) H 0.6587 0.2324 -0.1050 0.110 Uiso 1.00 1 c R . . H(12) H 0.7474 0.2934 -0.0480 0.110 Uiso 1.00 1 c R . . H(13) H 0.8321 0.0542 -0.0383 0.106 Uiso 1.00 1 c R . . H(14) H 0.7675 -0.0755 -0.0081 0.106 Uiso 1.00 1 c R . . H(15) H 0.8610 -0.0251 0.0515 0.106 Uiso 1.00 1 c R . . H(16) H 0.7523 0.4109 0.4912 0.120 Uiso 1.00 1 c R . . H(17) H 0.6873 0.5360 0.4476 0.120 Uiso 1.00 1 c R . . H(18) H 0.7815 0.4547 0.3899 0.120 Uiso 1.00 1 c R . . H(19) H 0.5362 0.1334 0.5896 0.132 Uiso 1.00 1 c R . . H(20) H 0.5934 0.2579 0.6039 0.132 Uiso 1.00 1 c R . . H(21) H 0.6836 0.1714 0.5481 0.132 Uiso 1.00 1 c R . . H(22) H 0.2362 0.1509 0.4590 0.107 Uiso 1.00 1 c R . . H(23) H 0.2815 0.1629 0.5501 0.107 Uiso 1.00 1 c R . . H(24) H 0.3590 0.0692 0.4945 0.107 Uiso 1.00 1 c R . . H(25) H 0.2698 0.4298 0.2831 0.106 Uiso 1.00 1 c R . . H(26) H 0.1841 0.3691 0.3695 0.106 Uiso 1.00 1 c R . . H(27) H 0.2491 0.2870 0.3013 0.106 Uiso 1.00 1 c R . . H(28) H 0.5938 0.5865 0.2937 0.115 Uiso 1.00 1 c R . . H(29) H 0.4339 0.5970 0.3053 0.115 Uiso 1.00 1 c R . . H(30) H 0.5100 0.5212 0.2364 0.115 Uiso 1.00 1 c R . . H(31) H 1.0456 0.2252 0.0919 0.111 Uiso 1.00 1 c R . . H(32) H 1.0171 0.3526 0.0335 0.111 Uiso 1.00 1 c R . . H(33) H 0.9492 0.2337 0.0181 0.111 Uiso 1.00 1 c R . . H(34) H 0.7956 0.4826 0.0386 0.106 Uiso 1.00 1 c R . . H(35) H 0.8456 0.5187 0.1224 0.106 Uiso 1.00 1 c R . . H(36) H 0.6934 0.4838 0.1236 0.106 Uiso 1.00 1 c R . . H(37) H 1.0002 0.2744 0.2385 0.066 Uiso 1.00 1 c R . . H(38) H 0.8914 0.3734 0.2669 0.066 Uiso 1.00 1 c R . . H(39) H 0.9602 0.1910 0.4181 0.073 Uiso 1.00 1 c R . . H(40) H 0.9851 0.0626 0.3869 0.073 Uiso 1.00 1 c R . . H(41) H 0.8623 0.0828 0.4573 0.073 Uiso 1.00 1 c R . . H(42) H 0.7724 -0.0129 0.2743 0.059 Uiso 1.00 1 c R . . H(43) H 0.8938 0.0534 0.2133 0.059 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ir(1) 0.03934(17) 0.03957(18) 0.03522(18) -0.00645(13) -0.01188(13) -0.00218(13) Ir(2) 0.04570(19) 0.03565(17) 0.03875(19) -0.00601(13) -0.00656(14) -0.00487(13) S(1) 0.087(2) 0.084(2) 0.086(2) -0.0167(17) -0.0237(17) 0.0092(17) P(1) 0.0491(12) 0.0563(13) 0.0395(11) -0.0185(10) -0.0097(9) 0.0014(9) P(2) 0.0458(11) 0.0443(11) 0.0398(11) -0.0055(9) -0.0177(9) -0.0042(8) F(1) 0.257(14) 0.182(10) 0.095(7) 0.049(10) -0.068(8) 0.019(7) F(2) 0.274(15) 0.176(10) 0.148(10) 0.117(10) -0.079(9) -0.091(8) F(3) 0.088(6) 0.238(13) 0.195(12) -0.026(7) -0.047(6) -0.042(10) O(1) 0.172(11) 0.074(6) 0.191(12) 0.009(6) -0.085(9) -0.040(7) O(2) 0.082(7) 0.241(15) 0.212(15) -0.072(8) -0.017(8) 0.043(11) O(3) 0.127(8) 0.105(7) 0.084(6) 0.022(6) -0.003(5) 0.030(5) C(1) 0.072(6) 0.043(4) 0.053(5) -0.014(4) -0.030(4) -0.006(4) C(2) 0.056(5) 0.059(5) 0.057(5) -0.022(4) -0.023(4) -0.005(4) C(3) 0.061(5) 0.060(5) 0.062(6) -0.002(4) -0.037(4) -0.011(4) C(4) 0.055(5) 0.077(6) 0.039(4) -0.017(4) -0.015(3) -0.011(4) C(5) 0.072(6) 0.065(5) 0.039(4) -0.010(4) -0.019(4) -0.015(4) C(6) 0.132(11) 0.048(5) 0.090(8) -0.017(6) -0.041(8) -0.008(5) C(7) 0.076(7) 0.126(11) 0.071(7) -0.061(7) -0.015(6) 0.001(7) C(8) 0.073(7) 0.074(7) 0.119(11) -0.006(6) -0.048(7) -0.006(7) C(9) 0.113(9) 0.112(10) 0.051(6) -0.047(8) -0.042(6) 0.024(6) C(10) 0.097(8) 0.101(9) 0.067(7) 0.002(7) -0.020(6) -0.049(7) C(11) 0.073(6) 0.056(5) 0.059(6) -0.014(4) 0.014(5) -0.028(4) C(12) 0.093(7) 0.062(6) 0.051(5) -0.018(5) 0.005(5) -0.025(4) C(13) 0.069(6) 0.047(5) 0.074(7) -0.012(4) 0.010(5) -0.013(4) C(14) 0.049(5) 0.052(5) 0.080(7) 0.006(4) -0.003(4) -0.016(5) C(15) 0.079(6) 0.029(4) 0.066(6) 0.004(4) 0.007(5) -0.005(4) C(16) 0.090(8) 0.100(9) 0.111(10) -0.025(7) -0.006(7) -0.073(8) C(17) 0.162(14) 0.124(12) 0.044(6) -0.020(10) -0.026(7) -0.005(7) C(18) 0.083(8) 0.079(8) 0.104(10) -0.022(6) 0.018(7) 0.003(7) C(19) 0.068(7) 0.080(8) 0.117(11) 0.022(6) -0.020(7) -0.029(7) C(20) 0.133(12) 0.045(6) 0.111(10) 0.011(6) 0.024(9) -0.000(6) C(21) 0.060(6) 0.158(13) 0.060(7) -0.038(7) 0.015(5) -0.033(7) C(22) 0.112(10) 0.064(6) 0.090(8) -0.037(6) -0.046(7) 0.020(6) C(23) 0.058(5) 0.056(5) 0.051(5) -0.020(4) -0.016(4) -0.005(4) C(24) 0.056(5) 0.079(6) 0.047(5) -0.008(4) -0.026(4) 0.001(4) C(25) 0.048(4) 0.046(4) 0.053(5) 0.006(3) -0.021(3) -0.006(3) C(26) 0.094(10) 0.094(10) 0.123(13) 0.021(8) -0.024(9) -0.001(9) #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction CrystalStructure _computing_structure_solution 'DIRDIF99 (PATTY)' _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ir(1) Ir(2) 3.0188(4) yes . . Ir(1) P(1) 2.257(2) yes . . Ir(1) C(1) 2.245(9) yes . . Ir(1) C(2) 2.261(10) yes . . Ir(1) C(3) 2.218(10) yes . . Ir(1) C(4) 2.213(9) yes . . Ir(1) C(5) 2.186(10) yes . . Ir(1) C(25) 2.155(8) yes . . Ir(2) P(2) 2.235(2) yes . . Ir(2) C(11) 2.256(11) yes . . Ir(2) C(12) 2.177(10) yes . . Ir(2) C(13) 2.212(10) yes . . Ir(2) C(14) 2.247(9) yes . . Ir(2) C(15) 2.272(8) yes . . S(1) O(1) 1.433(12) yes . . S(1) O(2) 1.414(11) yes . . S(1) O(3) 1.440(9) yes . . S(1) C(26) 1.770(19) yes . . P(1) C(21) 1.812(11) yes . . P(1) C(22) 1.795(10) yes . . P(1) C(23) 1.842(9) yes . . P(2) C(23) 1.829(8) yes . . P(2) C(24) 1.826(10) yes . . P(2) C(25) 1.755(9) yes . . F(1) C(26) 1.334(19) yes . . F(2) C(26) 1.28(2) yes . . F(3) C(26) 1.347(18) yes . . C(1) C(2) 1.430(13) yes . . C(1) C(5) 1.431(12) yes . . C(1) C(6) 1.481(13) yes . . C(2) C(3) 1.438(12) yes . . C(2) C(7) 1.515(13) yes . . C(3) C(4) 1.397(12) yes . . C(3) C(8) 1.501(14) yes . . C(4) C(5) 1.488(13) yes . . C(4) C(9) 1.480(14) yes . . C(5) C(10) 1.492(15) yes . . C(11) C(12) 1.491(13) yes . . C(11) C(15) 1.410(15) yes . . C(11) C(16) 1.490(17) yes . . C(12) C(13) 1.393(16) yes . . C(12) C(17) 1.548(17) yes . . C(13) C(14) 1.396(14) yes . . C(13) C(18) 1.513(15) yes . . C(14) C(15) 1.468(14) yes . . C(14) C(19) 1.492(16) yes . . C(15) C(20) 1.496(14) yes . . C(6) H(1) 0.950 no . . C(6) H(2) 0.950 no . . C(6) H(3) 0.950 no . . C(7) H(4) 0.950 no . . C(7) H(5) 0.950 no . . C(7) H(6) 0.950 no . . C(8) H(7) 0.950 no . . C(8) H(8) 0.950 no . . C(8) H(9) 0.950 no . . C(9) H(10) 0.950 no . . C(9) H(11) 0.950 no . . C(9) H(12) 0.950 no . . C(10) H(13) 0.950 no . . C(10) H(14) 0.950 no . . C(10) H(15) 0.950 no . . C(16) H(16) 0.950 no . . C(16) H(17) 0.950 no . . C(16) H(18) 0.950 no . . C(17) H(19) 0.950 no . . C(17) H(20) 0.950 no . . C(17) H(21) 0.950 no . . C(18) H(22) 0.950 no . . C(18) H(23) 0.950 no . . C(18) H(24) 0.950 no . . C(19) H(25) 0.950 no . . C(19) H(26) 0.950 no . . C(19) H(27) 0.950 no . . C(20) H(28) 0.950 no . . C(20) H(29) 0.950 no . . C(20) H(30) 0.950 no . . C(21) H(31) 0.950 no . . C(21) H(32) 0.950 no . . C(21) H(33) 0.950 no . . C(22) H(34) 0.950 no . . C(22) H(35) 0.950 no . . C(22) H(36) 0.950 no . . C(23) H(37) 0.950 no . . C(23) H(38) 0.950 no . . C(24) H(39) 0.950 no . . C(24) H(40) 0.950 no . . C(24) H(41) 0.950 no . . C(25) H(42) 0.950 no . . C(25) H(43) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Ir(2) Ir(1) P(1) 89.34(6) yes . . . Ir(2) Ir(1) C(1) 119.6(2) yes . . . Ir(2) Ir(1) C(2) 99.5(2) yes . . . Ir(2) Ir(1) C(3) 112.5(2) yes . . . Ir(2) Ir(1) C(4) 147.4(2) yes . . . Ir(2) Ir(1) C(5) 157.2(2) yes . . . Ir(2) Ir(1) C(25) 73.4(2) yes . . . P(1) Ir(1) C(1) 148.0(2) yes . . . P(1) Ir(1) C(2) 159.2(2) yes . . . P(1) Ir(1) C(3) 121.7(2) yes . . . P(1) Ir(1) C(4) 100.4(2) yes . . . P(1) Ir(1) C(5) 112.1(2) yes . . . P(1) Ir(1) C(25) 80.3(2) yes . . . C(1) Ir(1) C(2) 37.0(3) yes . . . C(1) Ir(1) C(3) 62.3(3) yes . . . C(1) Ir(1) C(4) 63.2(3) yes . . . C(1) Ir(1) C(5) 37.7(3) yes . . . C(1) Ir(1) C(25) 94.5(3) yes . . . C(2) Ir(1) C(3) 37.4(3) yes . . . C(2) Ir(1) C(4) 62.5(3) yes . . . C(2) Ir(1) C(5) 63.2(3) yes . . . C(2) Ir(1) C(25) 120.2(3) yes . . . C(3) Ir(1) C(4) 36.8(3) yes . . . C(3) Ir(1) C(5) 63.7(3) yes . . . C(3) Ir(1) C(25) 156.2(3) yes . . . C(4) Ir(1) C(5) 39.5(3) yes . . . C(4) Ir(1) C(25) 138.7(3) yes . . . C(5) Ir(1) C(25) 101.5(3) yes . . . Ir(1) Ir(2) P(2) 66.11(5) yes . . . Ir(1) Ir(2) C(11) 142.1(2) yes . . . Ir(1) Ir(2) C(12) 178.3(2) yes . . . Ir(1) Ir(2) C(13) 143.3(3) yes . . . Ir(1) Ir(2) C(14) 119.2(3) yes . . . Ir(1) Ir(2) C(15) 119.0(2) yes . . . P(2) Ir(2) C(11) 103.8(2) yes . . . P(2) Ir(2) C(12) 113.0(3) yes . . . P(2) Ir(2) C(13) 146.6(2) yes . . . P(2) Ir(2) C(14) 164.3(2) yes . . . P(2) Ir(2) C(15) 126.4(2) yes . . . C(11) Ir(2) C(12) 39.3(3) yes . . . C(11) Ir(2) C(13) 63.0(3) yes . . . C(11) Ir(2) C(14) 62.5(3) yes . . . C(11) Ir(2) C(15) 36.3(3) yes . . . C(12) Ir(2) C(13) 37.0(4) yes . . . C(12) Ir(2) C(14) 62.1(4) yes . . . C(12) Ir(2) C(15) 62.7(3) yes . . . C(13) Ir(2) C(14) 36.5(3) yes . . . C(13) Ir(2) C(15) 62.1(3) yes . . . C(14) Ir(2) C(15) 37.9(3) yes . . . O(1) S(1) O(2) 116.2(8) yes . . . O(1) S(1) O(3) 114.6(6) yes . . . O(1) S(1) C(26) 105.5(8) yes . . . O(2) S(1) O(3) 114.4(7) yes . . . O(2) S(1) C(26) 101.6(8) yes . . . O(3) S(1) C(26) 101.9(7) yes . . . Ir(1) P(1) C(21) 116.3(5) yes . . . Ir(1) P(1) C(22) 117.5(4) yes . . . Ir(1) P(1) C(23) 107.1(2) yes . . . C(21) P(1) C(22) 102.9(6) yes . . . C(21) P(1) C(23) 104.0(4) yes . . . C(22) P(1) C(23) 108.0(5) yes . . . Ir(2) P(2) C(23) 111.5(2) yes . . . Ir(2) P(2) C(24) 122.4(3) yes . . . Ir(2) P(2) C(25) 104.5(3) yes . . . C(23) P(2) C(24) 103.6(4) yes . . . C(23) P(2) C(25) 99.8(4) yes . . . C(24) P(2) C(25) 112.8(4) yes . . . Ir(1) C(1) C(2) 72.1(5) yes . . . Ir(1) C(1) C(5) 68.9(5) yes . . . Ir(1) C(1) C(6) 125.2(8) yes . . . C(2) C(1) C(5) 109.1(7) yes . . . C(2) C(1) C(6) 126.2(8) yes . . . C(5) C(1) C(6) 124.6(9) yes . . . Ir(1) C(2) C(1) 70.9(5) yes . . . Ir(1) C(2) C(3) 69.7(5) yes . . . Ir(1) C(2) C(7) 126.3(7) yes . . . C(1) C(2) C(3) 107.3(7) yes . . . C(1) C(2) C(7) 125.8(8) yes . . . C(3) C(2) C(7) 126.9(9) yes . . . Ir(1) C(3) C(2) 72.9(5) yes . . . Ir(1) C(3) C(4) 71.4(5) yes . . . Ir(1) C(3) C(8) 127.9(8) yes . . . C(2) C(3) C(4) 109.8(8) yes . . . C(2) C(3) C(8) 124.3(8) yes . . . C(4) C(3) C(8) 125.5(8) yes . . . Ir(1) C(4) C(3) 71.8(5) yes . . . Ir(1) C(4) C(5) 69.3(5) yes . . . Ir(1) C(4) C(9) 128.0(8) yes . . . C(3) C(4) C(5) 107.4(7) yes . . . C(3) C(4) C(9) 127.6(9) yes . . . C(5) C(4) C(9) 124.8(8) yes . . . Ir(1) C(5) C(1) 73.4(5) yes . . . Ir(1) C(5) C(4) 71.2(5) yes . . . Ir(1) C(5) C(10) 128.3(8) yes . . . C(1) C(5) C(4) 106.3(7) yes . . . C(1) C(5) C(10) 125.6(8) yes . . . C(4) C(5) C(10) 127.3(8) yes . . . Ir(2) C(11) C(12) 67.5(5) yes . . . Ir(2) C(11) C(15) 72.5(6) yes . . . Ir(2) C(11) C(16) 128.3(7) yes . . . C(12) C(11) C(15) 105.9(9) yes . . . C(12) C(11) C(16) 127.1(9) yes . . . C(15) C(11) C(16) 126.8(9) yes . . . Ir(2) C(12) C(11) 73.2(5) yes . . . Ir(2) C(12) C(13) 72.9(6) yes . . . Ir(2) C(12) C(17) 125.8(8) yes . . . C(11) C(12) C(13) 108.1(8) yes . . . C(11) C(12) C(17) 123.7(11) yes . . . C(13) C(12) C(17) 127.7(10) yes . . . Ir(2) C(13) C(12) 70.1(6) yes . . . Ir(2) C(13) C(14) 73.1(5) yes . . . Ir(2) C(13) C(18) 126.1(7) yes . . . C(12) C(13) C(14) 109.9(8) yes . . . C(12) C(13) C(18) 123.7(9) yes . . . C(14) C(13) C(18) 126.3(10) yes . . . Ir(2) C(14) C(13) 70.4(5) yes . . . Ir(2) C(14) C(15) 71.9(5) yes . . . Ir(2) C(14) C(19) 130.3(8) yes . . . C(13) C(14) C(15) 107.6(9) yes . . . C(13) C(14) C(19) 126.3(9) yes . . . C(15) C(14) C(19) 125.5(8) yes . . . Ir(2) C(15) C(11) 71.2(5) yes . . . Ir(2) C(15) C(14) 70.1(5) yes . . . Ir(2) C(15) C(20) 129.0(7) yes . . . C(11) C(15) C(14) 108.4(8) yes . . . C(11) C(15) C(20) 126.2(10) yes . . . C(14) C(15) C(20) 125.1(10) yes . . . P(1) C(23) P(2) 103.0(4) yes . . . Ir(1) C(25) P(2) 97.0(3) yes . . . S(1) C(26) F(1) 111.5(12) yes . . . S(1) C(26) F(2) 114.2(12) yes . . . S(1) C(26) F(3) 110.8(12) yes . . . F(1) C(26) F(2) 106.6(14) yes . . . F(1) C(26) F(3) 103.2(13) yes . . . F(2) C(26) F(3) 109.9(15) yes . . . C(1) C(6) H(1) 108.8 no . . . C(1) C(6) H(2) 109.7 no . . . C(1) C(6) H(3) 109.9 no . . . H(1) C(6) H(2) 109.5 no . . . H(1) C(6) H(3) 109.5 no . . . H(2) C(6) H(3) 109.5 no . . . C(2) C(7) H(4) 109.5 no . . . C(2) C(7) H(5) 109.1 no . . . C(2) C(7) H(6) 109.8 no . . . H(4) C(7) H(5) 109.5 no . . . H(4) C(7) H(6) 109.5 no . . . H(5) C(7) H(6) 109.5 no . . . C(3) C(8) H(7) 110.1 no . . . C(3) C(8) H(8) 109.5 no . . . C(3) C(8) H(9) 108.9 no . . . H(7) C(8) H(8) 109.5 no . . . H(7) C(8) H(9) 109.5 no . . . H(8) C(8) H(9) 109.5 no . . . C(4) C(9) H(10) 108.4 no . . . C(4) C(9) H(11) 110.4 no . . . C(4) C(9) H(12) 109.6 no . . . H(10) C(9) H(11) 109.5 no . . . H(10) C(9) H(12) 109.5 no . . . H(11) C(9) H(12) 109.5 no . . . C(5) C(10) H(13) 109.3 no . . . C(5) C(10) H(14) 109.4 no . . . C(5) C(10) H(15) 109.7 no . . . H(13) C(10) H(14) 109.5 no . . . H(13) C(10) H(15) 109.5 no . . . H(14) C(10) H(15) 109.5 no . . . C(11) C(16) H(16) 110.2 no . . . C(11) C(16) H(17) 109.4 no . . . C(11) C(16) H(18) 108.8 no . . . H(16) C(16) H(17) 109.5 no . . . H(16) C(16) H(18) 109.5 no . . . H(17) C(16) H(18) 109.5 no . . . C(12) C(17) H(19) 109.9 no . . . C(12) C(17) H(20) 108.6 no . . . C(12) C(17) H(21) 109.9 no . . . H(19) C(17) H(20) 109.5 no . . . H(19) C(17) H(21) 109.5 no . . . H(20) C(17) H(21) 109.5 no . . . C(13) C(18) H(22) 109.4 no . . . C(13) C(18) H(23) 108.8 no . . . C(13) C(18) H(24) 110.3 no . . . H(22) C(18) H(23) 109.5 no . . . H(22) C(18) H(24) 109.5 no . . . H(23) C(18) H(24) 109.5 no . . . C(14) C(19) H(25) 109.3 no . . . C(14) C(19) H(26) 108.6 no . . . C(14) C(19) H(27) 110.4 no . . . H(25) C(19) H(26) 109.5 no . . . H(25) C(19) H(27) 109.5 no . . . H(26) C(19) H(27) 109.5 no . . . C(15) C(20) H(28) 112.2 no . . . C(15) C(20) H(29) 108.7 no . . . C(15) C(20) H(30) 107.5 no . . . H(28) C(20) H(29) 109.5 no . . . H(28) C(20) H(30) 109.5 no . . . H(29) C(20) H(30) 109.5 no . . . P(1) C(21) H(31) 109.7 no . . . P(1) C(21) H(32) 109.3 no . . . P(1) C(21) H(33) 109.5 no . . . H(31) C(21) H(32) 109.5 no . . . H(31) C(21) H(33) 109.5 no . . . H(32) C(21) H(33) 109.5 no . . . P(1) C(22) H(34) 109.7 no . . . P(1) C(22) H(35) 109.4 no . . . P(1) C(22) H(36) 109.3 no . . . H(34) C(22) H(35) 109.5 no . . . H(34) C(22) H(36) 109.5 no . . . H(35) C(22) H(36) 109.5 no . . . P(1) C(23) H(37) 111.0 no . . . P(1) C(23) H(38) 111.4 no . . . P(2) C(23) H(37) 110.8 no . . . P(2) C(23) H(38) 111.1 no . . . H(37) C(23) H(38) 109.5 no . . . P(2) C(24) H(39) 109.1 no . . . P(2) C(24) H(40) 109.6 no . . . P(2) C(24) H(41) 109.7 no . . . H(39) C(24) H(40) 109.5 no . . . H(39) C(24) H(41) 109.5 no . . . H(40) C(24) H(41) 109.5 no . . . Ir(1) C(25) H(42) 112.3 no . . . Ir(1) C(25) H(43) 112.6 no . . . P(2) C(25) H(42) 112.3 no . . . P(2) C(25) H(43) 112.8 no . . . H(42) C(25) H(43) 109.5 no . . . #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== data__complex12 _database_code_depnum_ccdc_archive 'CCDC 680334' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C31 H50 F3 Ir2 N O3 P2 S ' _chemical_formula_moiety 'C31 H50 F3 Ir2 N O3 P2 S ' _chemical_formula_weight 1020.18 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' _symmetry_space_group_name_Hall '-P 2yab' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,+Z #------------------------------------------------------------------------------ _cell_length_a 17.7878(14) _cell_length_b 12.3618(17) _cell_length_c 18.402(2) _cell_angle_alpha 90.0000 _cell_angle_beta 117.595(7) _cell_angle_gamma 90.0000 _cell_volume 3586.1(7) _cell_formula_units_Z 4 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 14.3 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 293.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_density_diffrn 1.889 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976.00 _exptl_absorpt_coefficient_mu 7.629 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.042 _exptl_absorpt_correction_T_max 0.069 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 8475 _diffrn_reflns_av_R_equivalents 0.023 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 21 _diffrn_standards_number 3 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 8206 _reflns_number_gt 5785 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.0598 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 5785 _refine_ls_number_parameters 436 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0025Fo^2^ + 1.0000\s(Fo^2^)]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 5.55 _refine_diff_density_min -2.43 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ir Ir -1.444 7.990 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.017 0.010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.67122(2) 0.24886(3) 0.32230(2) 0.03259(9) Uani 1.00 1 d . . . Ir(2) Ir 0.56875(2) 0.29872(3) 0.07868(2) 0.03257(9) Uani 1.00 1 d . . . S(1) S 0.3331(2) 0.7506(3) 0.2553(2) 0.0737(10) Uani 1.00 1 d . . . P(1) P 0.73176(16) 0.4081(2) 0.32338(15) 0.0421(6) Uani 1.00 1 d . . . P(2) P 0.69718(15) 0.3771(2) 0.14211(15) 0.0379(6) Uani 1.00 1 d . . . F(1) F 0.4925(6) 0.7147(10) 0.2998(7) 0.130(4) Uani 1.00 1 d . . . F(2) F 0.4468(6) 0.6426(9) 0.3769(5) 0.131(4) Uani 1.00 1 d . . . F(3) F 0.4695(6) 0.8114(8) 0.3847(6) 0.118(3) Uani 1.00 1 d . . . O(1) O 0.3445(10) 0.8483(11) 0.2156(7) 0.155(6) Uani 1.00 1 d . . . O(2) O 0.3153(6) 0.6582(10) 0.2080(6) 0.119(4) Uani 1.00 1 d . . . O(3) O 0.2894(7) 0.7720(9) 0.3027(7) 0.099(4) Uani 1.00 1 d . . . N(1) N 0.5301(4) 0.3540(5) 0.1676(4) 0.0317(18) Uani 1.00 1 d . . . C(1) C 0.6968(8) 0.0746(9) 0.3651(6) 0.061(3) Uani 1.00 1 d . . . C(2) C 0.7695(7) 0.1361(10) 0.4136(6) 0.056(3) Uani 1.00 1 d . . . C(3) C 0.7475(7) 0.2084(10) 0.4588(6) 0.055(3) Uani 1.00 1 d . . . C(4) C 0.6601(8) 0.1954(11) 0.4361(6) 0.065(4) Uani 1.00 1 d . . . C(5) C 0.6269(7) 0.1109(11) 0.3766(6) 0.062(3) Uani 1.00 1 d . . . C(6) C 0.6986(14) -0.0272(12) 0.3173(8) 0.139(7) Uani 1.00 1 d . . . C(7) C 0.8576(8) 0.1116(16) 0.4263(10) 0.122(7) Uani 1.00 1 d . . . C(8) C 0.8065(9) 0.2822(13) 0.5281(6) 0.092(5) Uani 1.00 1 d . . . C(9) C 0.6175(12) 0.2479(15) 0.4832(8) 0.111(7) Uani 1.00 1 d . . . C(10) C 0.5421(9) 0.0628(15) 0.3451(9) 0.123(6) Uani 1.00 1 d . . . C(11) C 0.4545(6) 0.1980(9) 0.0008(6) 0.054(3) Uani 1.00 1 d . . . C(12) C 0.4926(7) 0.2326(8) -0.0454(5) 0.049(2) Uani 1.00 1 d . . . C(13) C 0.5802(7) 0.1890(9) -0.0085(6) 0.055(3) Uani 1.00 1 d . . . C(14) C 0.5895(6) 0.1191(7) 0.0600(5) 0.044(2) Uani 1.00 1 d . . . C(15) C 0.5152(6) 0.1295(7) 0.0659(6) 0.046(2) Uani 1.00 1 d . . . C(16) C 0.3662(7) 0.2178(12) -0.0133(8) 0.079(4) Uani 1.00 1 d . . . C(17) C 0.4484(9) 0.2917(11) -0.1268(7) 0.086(4) Uani 1.00 1 d . . . C(18) C 0.6402(9) 0.1975(12) -0.0446(8) 0.083(5) Uani 1.00 1 d . . . C(19) C 0.6648(8) 0.0542(10) 0.1086(7) 0.080(4) Uani 1.00 1 d . . . C(20) C 0.4955(9) 0.0717(11) 0.1277(7) 0.084(5) Uani 1.00 1 d . . . C(21) C 0.7053(8) 0.5196(10) 0.3721(7) 0.081(4) Uani 1.00 1 d . . . C(22) C 0.8468(7) 0.4129(12) 0.3773(6) 0.077(4) Uani 1.00 1 d . . . C(23) C 0.7079(6) 0.4693(7) 0.2246(5) 0.044(2) Uani 1.00 1 d . . . C(24) C 0.7922(6) 0.2969(10) 0.1822(7) 0.060(3) Uani 1.00 1 d . . . C(25) C 0.7189(7) 0.4678(10) 0.0760(6) 0.067(3) Uani 1.00 1 d . . . C(26) C 0.5603(5) 0.3281(7) 0.2484(5) 0.036(2) Uani 1.00 1 d . . . C(27) C 0.5122(6) 0.3649(9) 0.2867(6) 0.050(3) Uani 1.00 1 d . . . C(28) C 0.4395(6) 0.4263(9) 0.2473(7) 0.057(3) Uani 1.00 1 d . . . C(29) C 0.4162(5) 0.4567(8) 0.1680(6) 0.045(2) Uani 1.00 1 d . . . C(30) C 0.4592(5) 0.4197(8) 0.1299(5) 0.044(2) Uani 1.00 1 d . . . C(31) C 0.4403(9) 0.7297(13) 0.3305(10) 0.080(4) Uani 1.00 1 d . . . H(1) H 0.7541 -0.0383 0.3235 0.169 Uiso 1.00 1 c R . . H(2) H 0.6818 -0.0885 0.3373 0.169 Uiso 1.00 1 c R . . H(3) H 0.6601 -0.0169 0.2610 0.169 Uiso 1.00 1 c R . . H(4) H 0.8955 0.1609 0.4659 0.153 Uiso 1.00 1 c R . . H(5) H 0.8731 0.0396 0.4455 0.153 Uiso 1.00 1 c R . . H(6) H 0.8601 0.1205 0.3762 0.153 Uiso 1.00 1 c R . . H(7) H 0.7766 0.3214 0.5509 0.103 Uiso 1.00 1 c R . . H(8) H 0.8484 0.2382 0.5693 0.103 Uiso 1.00 1 c R . . H(9) H 0.8330 0.3314 0.5075 0.103 Uiso 1.00 1 c R . . H(10) H 0.5613 0.2205 0.4609 0.145 Uiso 1.00 1 c R . . H(11) H 0.6470 0.2311 0.5400 0.145 Uiso 1.00 1 c R . . H(12) H 0.6158 0.3241 0.4761 0.145 Uiso 1.00 1 c R . . H(13) H 0.5383 0.0040 0.3103 0.138 Uiso 1.00 1 c R . . H(14) H 0.5329 0.0374 0.3890 0.138 Uiso 1.00 1 c R . . H(15) H 0.5002 0.1153 0.3145 0.138 Uiso 1.00 1 c R . . H(16) H 0.3384 0.2618 -0.0608 0.094 Uiso 1.00 1 c R . . H(17) H 0.3368 0.1511 -0.0218 0.094 Uiso 1.00 1 c R . . H(18) H 0.3666 0.2540 0.0325 0.094 Uiso 1.00 1 c R . . H(19) H 0.4867 0.3013 -0.1490 0.094 Uiso 1.00 1 c R . . H(20) H 0.3998 0.2533 -0.1649 0.094 Uiso 1.00 1 c R . . H(21) H 0.4316 0.3604 -0.1162 0.094 Uiso 1.00 1 c R . . H(22) H 0.6907 0.1593 -0.0104 0.111 Uiso 1.00 1 c R . . H(23) H 0.6152 0.1671 -0.0981 0.111 Uiso 1.00 1 c R . . H(24) H 0.6533 0.2714 -0.0473 0.111 Uiso 1.00 1 c R . . H(25) H 0.6576 0.0201 0.1512 0.089 Uiso 1.00 1 c R . . H(26) H 0.6715 0.0006 0.0750 0.089 Uiso 1.00 1 c R . . H(27) H 0.7138 0.0989 0.1318 0.089 Uiso 1.00 1 c R . . H(28) H 0.4395 0.0870 0.1186 0.107 Uiso 1.00 1 c R . . H(29) H 0.5015 -0.0040 0.1229 0.107 Uiso 1.00 1 c R . . H(30) H 0.5349 0.0949 0.1812 0.107 Uiso 1.00 1 c R . . H(31) H 0.7444 0.5223 0.4288 0.110 Uiso 1.00 1 c R . . H(32) H 0.7075 0.5857 0.3468 0.110 Uiso 1.00 1 c R . . H(33) H 0.6496 0.5091 0.3655 0.110 Uiso 1.00 1 c R . . H(34) H 0.8680 0.3959 0.3398 0.087 Uiso 1.00 1 c R . . H(35) H 0.8650 0.4834 0.3989 0.087 Uiso 1.00 1 c R . . H(36) H 0.8676 0.3618 0.4207 0.087 Uiso 1.00 1 c R . . H(37) H 0.7523 0.5187 0.2336 0.051 Uiso 1.00 1 c R . . H(38) H 0.6561 0.5077 0.2062 0.051 Uiso 1.00 1 c R . . H(39) H 0.8099 0.2873 0.1412 0.074 Uiso 1.00 1 c R . . H(40) H 0.8360 0.3313 0.2286 0.074 Uiso 1.00 1 c R . . H(41) H 0.7802 0.2283 0.1978 0.074 Uiso 1.00 1 c R . . H(42) H 0.7003 0.5388 0.0796 0.083 Uiso 1.00 1 c R . . H(43) H 0.7782 0.4687 0.0933 0.083 Uiso 1.00 1 c R . . H(44) H 0.6897 0.4434 0.0209 0.083 Uiso 1.00 1 c R . . H(45) H 0.5307 0.3463 0.3425 0.068 Uiso 1.00 1 c R . . H(46) H 0.4083 0.4495 0.2746 0.077 Uiso 1.00 1 c R . . H(47) H 0.3682 0.5019 0.1395 0.055 Uiso 1.00 1 c R . . H(48) H 0.4407 0.4392 0.0742 0.051 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ir(1) 0.03595(19) 0.0332(2) 0.03372(18) 0.00048(15) 0.02045(14) 0.00167(15) Ir(2) 0.03759(19) 0.02815(18) 0.03469(18) 0.00040(16) 0.01904(14) -0.00385(15) S(1) 0.075(2) 0.083(2) 0.0586(18) 0.0338(18) 0.0274(16) -0.0028(17) P(1) 0.0476(13) 0.0419(14) 0.0396(12) -0.0126(11) 0.0227(10) -0.0059(11) P(2) 0.0411(12) 0.0347(13) 0.0429(12) -0.0062(10) 0.0238(10) 0.0002(10) F(1) 0.078(6) 0.189(12) 0.135(8) 0.009(6) 0.060(6) -0.033(7) F(2) 0.141(8) 0.126(8) 0.091(6) 0.049(7) 0.023(6) 0.024(6) F(3) 0.105(6) 0.116(8) 0.126(8) -0.025(6) 0.049(6) -0.048(6) O(1) 0.254(16) 0.140(11) 0.136(10) 0.113(12) 0.145(11) 0.090(9) O(2) 0.087(7) 0.130(10) 0.100(7) 0.039(7) 0.009(6) -0.059(7) O(3) 0.094(7) 0.106(8) 0.113(8) 0.030(6) 0.061(7) 0.003(6) N(1) 0.035(3) 0.027(3) 0.036(3) 0.003(3) 0.020(3) -0.000(3) C(1) 0.106(9) 0.038(6) 0.047(5) 0.017(6) 0.044(6) 0.013(4) C(2) 0.057(6) 0.070(8) 0.046(5) 0.024(5) 0.027(5) 0.025(5) C(3) 0.062(6) 0.067(7) 0.036(5) 0.013(5) 0.022(4) 0.010(4) C(4) 0.088(8) 0.081(8) 0.048(6) 0.017(7) 0.051(6) 0.024(6) C(5) 0.063(7) 0.070(8) 0.050(6) -0.004(6) 0.023(5) 0.010(5) C(6) 0.28(2) 0.058(9) 0.085(10) 0.059(13) 0.088(13) 0.026(8) C(7) 0.076(9) 0.18(2) 0.128(13) 0.061(11) 0.062(9) 0.075(13) C(8) 0.100(11) 0.123(14) 0.035(5) -0.025(9) 0.015(6) 0.006(6) C(9) 0.152(16) 0.143(16) 0.068(9) 0.081(13) 0.077(10) 0.047(9) C(10) 0.103(11) 0.145(17) 0.097(11) -0.063(11) 0.026(9) 0.053(11) C(11) 0.049(5) 0.056(6) 0.053(5) -0.006(5) 0.020(4) -0.032(5) C(12) 0.067(6) 0.043(6) 0.033(4) -0.003(4) 0.020(4) -0.008(4) C(13) 0.058(6) 0.062(7) 0.052(5) -0.014(5) 0.031(5) -0.027(5) C(14) 0.057(5) 0.024(4) 0.051(5) 0.004(4) 0.025(4) -0.011(4) C(15) 0.061(6) 0.023(4) 0.052(5) -0.014(4) 0.027(4) -0.014(4) C(16) 0.046(6) 0.088(10) 0.101(10) -0.008(6) 0.031(6) -0.043(8) C(17) 0.100(11) 0.075(9) 0.060(7) -0.004(8) 0.018(7) 0.002(7) C(18) 0.092(10) 0.096(11) 0.090(10) -0.029(8) 0.067(8) -0.041(8) C(19) 0.083(9) 0.049(7) 0.089(9) 0.012(6) 0.024(7) -0.024(6) C(20) 0.118(12) 0.069(9) 0.079(8) -0.026(8) 0.058(8) -0.015(7) C(21) 0.133(12) 0.058(7) 0.083(8) -0.039(8) 0.077(9) -0.043(7) C(22) 0.068(7) 0.098(10) 0.052(6) -0.039(7) 0.017(5) 0.005(6) C(23) 0.054(5) 0.030(4) 0.043(4) -0.009(4) 0.018(4) 0.001(4) C(24) 0.043(5) 0.070(8) 0.073(7) -0.001(5) 0.031(5) -0.003(6) C(25) 0.088(8) 0.067(8) 0.054(6) -0.038(6) 0.039(6) -0.004(5) C(26) 0.041(4) 0.029(4) 0.036(4) -0.006(3) 0.017(3) -0.008(3) C(27) 0.054(5) 0.056(6) 0.061(6) 0.013(5) 0.043(5) 0.005(5) C(28) 0.064(6) 0.051(6) 0.079(7) 0.002(5) 0.054(6) -0.006(5) C(29) 0.039(4) 0.036(5) 0.062(6) 0.008(4) 0.025(4) 0.000(4) C(30) 0.040(4) 0.041(5) 0.047(5) 0.010(4) 0.017(4) -0.005(4) C(31) 0.075(8) 0.073(10) 0.087(10) -0.000(7) 0.033(8) -0.020(8) #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction CrystalStructure _computing_structure_solution 'DIRDIF99 (PATTY)' _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ir(1) P(1) 2.240(2) yes . . Ir(1) C(1) 2.266(11) yes . . Ir(1) C(2) 2.259(10) yes . . Ir(1) C(3) 2.290(9) yes . . Ir(1) C(4) 2.290(14) yes . . Ir(1) C(5) 2.293(14) yes . . Ir(1) C(26) 2.054(8) yes . . Ir(2) P(2) 2.247(2) yes . . Ir(2) N(1) 2.159(8) yes . . Ir(2) C(11) 2.245(10) yes . . Ir(2) C(12) 2.203(8) yes . . Ir(2) C(13) 2.182(13) yes . . Ir(2) C(14) 2.303(9) yes . . Ir(2) C(15) 2.265(9) yes . . S(1) O(1) 1.473(16) yes . . S(1) O(2) 1.381(12) yes . . S(1) O(3) 1.435(16) yes . . S(1) C(31) 1.782(14) yes . . P(1) C(21) 1.820(14) yes . . P(1) C(22) 1.815(11) yes . . P(1) C(23) 1.828(10) yes . . P(2) C(23) 1.836(10) yes . . P(2) C(24) 1.797(11) yes . . P(2) C(25) 1.822(14) yes . . F(1) C(31) 1.31(2) yes . . F(2) C(31) 1.35(2) yes . . F(3) C(31) 1.344(19) yes . . N(1) C(26) 1.364(11) yes . . N(1) C(30) 1.385(11) yes . . C(1) C(2) 1.406(15) yes . . C(1) C(5) 1.43(2) yes . . C(1) C(6) 1.54(2) yes . . C(2) C(3) 1.395(19) yes . . C(2) C(7) 1.50(2) yes . . C(3) C(4) 1.419(19) yes . . C(3) C(8) 1.523(16) yes . . C(4) C(5) 1.428(17) yes . . C(4) C(9) 1.53(2) yes . . C(5) C(10) 1.47(2) yes . . C(11) C(12) 1.379(19) yes . . C(11) C(15) 1.456(13) yes . . C(11) C(16) 1.488(18) yes . . C(12) C(13) 1.483(16) yes . . C(12) C(17) 1.519(15) yes . . C(13) C(14) 1.475(16) yes . . C(13) C(18) 1.50(2) yes . . C(14) C(15) 1.380(18) yes . . C(14) C(19) 1.459(14) yes . . C(15) C(20) 1.52(2) yes . . C(26) C(27) 1.411(18) yes . . C(27) C(28) 1.380(14) yes . . C(28) C(29) 1.372(16) yes . . C(29) C(30) 1.335(18) yes . . C(6) H(1) 0.950 no . . C(6) H(2) 0.950 no . . C(6) H(3) 0.950 no . . C(7) H(4) 0.950 no . . C(7) H(5) 0.950 no . . C(7) H(6) 0.950 no . . C(8) H(7) 0.950 no . . C(8) H(8) 0.950 no . . C(8) H(9) 0.950 no . . C(9) H(10) 0.950 no . . C(9) H(11) 0.950 no . . C(9) H(12) 0.950 no . . C(10) H(13) 0.950 no . . C(10) H(14) 0.950 no . . C(10) H(15) 0.950 no . . C(16) H(16) 0.950 no . . C(16) H(17) 0.950 no . . C(16) H(18) 0.950 no . . C(17) H(19) 0.950 no . . C(17) H(20) 0.950 no . . C(17) H(21) 0.950 no . . C(18) H(22) 0.950 no . . C(18) H(23) 0.950 no . . C(18) H(24) 0.950 no . . C(19) H(25) 0.950 no . . C(19) H(26) 0.950 no . . C(19) H(27) 0.950 no . . C(20) H(28) 0.950 no . . C(20) H(29) 0.950 no . . C(20) H(30) 0.950 no . . C(21) H(31) 0.950 no . . C(21) H(32) 0.950 no . . C(21) H(33) 0.950 no . . C(22) H(34) 0.950 no . . C(22) H(35) 0.950 no . . C(22) H(36) 0.950 no . . C(23) H(37) 0.950 no . . C(23) H(38) 0.950 no . . C(24) H(39) 0.950 no . . C(24) H(40) 0.950 no . . C(24) H(41) 0.950 no . . C(25) H(42) 0.950 no . . C(25) H(43) 0.950 no . . C(25) H(44) 0.950 no . . C(27) H(45) 0.950 no . . C(28) H(46) 0.950 no . . C(29) H(47) 0.950 no . . C(30) H(48) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 P(1) Ir(1) C(1) 144.5(3) yes . . . P(1) Ir(1) C(2) 109.4(3) yes . . . P(1) Ir(1) C(3) 98.3(3) yes . . . P(1) Ir(1) C(4) 119.4(3) yes . . . P(1) Ir(1) C(5) 155.6(3) yes . . . P(1) Ir(1) C(26) 84.1(2) yes . . . C(1) Ir(1) C(2) 36.2(4) yes . . . C(1) Ir(1) C(3) 59.3(4) yes . . . C(1) Ir(1) C(4) 59.8(5) yes . . . C(1) Ir(1) C(5) 36.5(5) yes . . . C(1) Ir(1) C(26) 131.3(4) yes . . . C(2) Ir(1) C(3) 35.7(4) yes . . . C(2) Ir(1) C(4) 60.4(5) yes . . . C(2) Ir(1) C(5) 61.4(4) yes . . . C(2) Ir(1) C(26) 164.2(4) yes . . . C(3) Ir(1) C(4) 36.1(4) yes . . . C(3) Ir(1) C(5) 60.5(4) yes . . . C(3) Ir(1) C(26) 136.9(4) yes . . . C(4) Ir(1) C(5) 36.3(4) yes . . . C(4) Ir(1) C(26) 106.3(4) yes . . . C(5) Ir(1) C(26) 103.0(4) yes . . . P(2) Ir(2) N(1) 94.23(19) yes . . . P(2) Ir(2) C(11) 166.7(3) yes . . . P(2) Ir(2) C(12) 133.4(3) yes . . . P(2) Ir(2) C(13) 103.4(3) yes . . . P(2) Ir(2) C(14) 107.4(2) yes . . . P(2) Ir(2) C(15) 136.9(2) yes . . . N(1) Ir(2) C(11) 98.5(4) yes . . . N(1) Ir(2) C(12) 130.1(4) yes . . . N(1) Ir(2) C(13) 157.8(4) yes . . . N(1) Ir(2) C(14) 123.2(3) yes . . . N(1) Ir(2) C(15) 96.0(4) yes . . . C(11) Ir(2) C(12) 36.1(5) yes . . . C(11) Ir(2) C(13) 63.3(4) yes . . . C(11) Ir(2) C(14) 62.0(3) yes . . . C(11) Ir(2) C(15) 37.7(3) yes . . . C(12) Ir(2) C(13) 39.5(4) yes . . . C(12) Ir(2) C(14) 63.4(3) yes . . . C(12) Ir(2) C(15) 61.5(3) yes . . . C(13) Ir(2) C(14) 38.3(4) yes . . . C(13) Ir(2) C(15) 61.8(4) yes . . . C(14) Ir(2) C(15) 35.2(4) yes . . . O(1) S(1) O(2) 114.1(8) yes . . . O(1) S(1) O(3) 112.9(8) yes . . . O(1) S(1) C(31) 99.2(8) yes . . . O(2) S(1) O(3) 120.3(7) yes . . . O(2) S(1) C(31) 102.7(7) yes . . . O(3) S(1) C(31) 103.9(8) yes . . . Ir(1) P(1) C(21) 115.9(5) yes . . . Ir(1) P(1) C(22) 116.7(4) yes . . . Ir(1) P(1) C(23) 117.8(2) yes . . . C(21) P(1) C(22) 100.9(6) yes . . . C(21) P(1) C(23) 100.5(5) yes . . . C(22) P(1) C(23) 102.3(5) yes . . . Ir(2) P(2) C(23) 112.9(3) yes . . . Ir(2) P(2) C(24) 120.7(4) yes . . . Ir(2) P(2) C(25) 113.4(3) yes . . . C(23) P(2) C(24) 106.6(4) yes . . . C(23) P(2) C(25) 101.4(5) yes . . . C(24) P(2) C(25) 99.5(6) yes . . . Ir(2) N(1) C(26) 130.5(6) yes . . . Ir(2) N(1) C(30) 109.9(6) yes . . . C(26) N(1) C(30) 119.4(9) yes . . . Ir(1) C(1) C(2) 71.6(6) yes . . . Ir(1) C(1) C(5) 72.8(7) yes . . . Ir(1) C(1) C(6) 129.1(9) yes . . . C(2) C(1) C(5) 110.1(11) yes . . . C(2) C(1) C(6) 123.1(15) yes . . . C(5) C(1) C(6) 126.2(13) yes . . . Ir(1) C(2) C(1) 72.2(5) yes . . . Ir(1) C(2) C(3) 73.4(6) yes . . . Ir(1) C(2) C(7) 129.2(10) yes . . . C(1) C(2) C(3) 107.2(12) yes . . . C(1) C(2) C(7) 125.1(13) yes . . . C(3) C(2) C(7) 126.6(10) yes . . . Ir(1) C(3) C(2) 70.9(5) yes . . . Ir(1) C(3) C(4) 71.9(6) yes . . . Ir(1) C(3) C(8) 128.0(9) yes . . . C(2) C(3) C(4) 108.9(10) yes . . . C(2) C(3) C(8) 127.5(12) yes . . . C(4) C(3) C(8) 123.4(13) yes . . . Ir(1) C(4) C(3) 72.0(8) yes . . . Ir(1) C(4) C(5) 72.0(8) yes . . . Ir(1) C(4) C(9) 132.0(9) yes . . . C(3) C(4) C(5) 108.4(12) yes . . . C(3) C(4) C(9) 123.1(11) yes . . . C(5) C(4) C(9) 127.2(13) yes . . . Ir(1) C(5) C(1) 70.7(7) yes . . . Ir(1) C(5) C(4) 71.7(8) yes . . . Ir(1) C(5) C(10) 128.8(8) yes . . . C(1) C(5) C(4) 105.3(10) yes . . . C(1) C(5) C(10) 128.3(12) yes . . . C(4) C(5) C(10) 125.7(14) yes . . . Ir(2) C(11) C(12) 70.3(5) yes . . . Ir(2) C(11) C(15) 71.9(5) yes . . . Ir(2) C(11) C(16) 126.2(9) yes . . . C(12) C(11) C(15) 107.3(10) yes . . . C(12) C(11) C(16) 128.5(10) yes . . . C(15) C(11) C(16) 124.1(12) yes . . . Ir(2) C(12) C(11) 73.6(5) yes . . . Ir(2) C(12) C(13) 69.5(5) yes . . . Ir(2) C(12) C(17) 129.3(8) yes . . . C(11) C(12) C(13) 108.6(9) yes . . . C(11) C(12) C(17) 125.4(11) yes . . . C(13) C(12) C(17) 125.5(13) yes . . . Ir(2) C(13) C(12) 71.0(6) yes . . . Ir(2) C(13) C(14) 75.3(6) yes . . . Ir(2) C(13) C(18) 127.6(8) yes . . . C(12) C(13) C(14) 106.4(11) yes . . . C(12) C(13) C(18) 125.8(10) yes . . . C(14) C(13) C(18) 126.8(10) yes . . . Ir(2) C(14) C(13) 66.4(5) yes . . . Ir(2) C(14) C(15) 70.9(5) yes . . . Ir(2) C(14) C(19) 127.2(6) yes . . . C(13) C(14) C(15) 106.3(8) yes . . . C(13) C(14) C(19) 123.6(12) yes . . . C(15) C(14) C(19) 130.1(11) yes . . . Ir(2) C(15) C(11) 70.4(5) yes . . . Ir(2) C(15) C(14) 73.9(5) yes . . . Ir(2) C(15) C(20) 126.1(7) yes . . . C(11) C(15) C(14) 111.3(10) yes . . . C(11) C(15) C(20) 123.4(11) yes . . . C(14) C(15) C(20) 125.2(9) yes . . . P(1) C(23) P(2) 116.9(4) yes . . . Ir(1) C(26) N(1) 127.3(8) yes . . . Ir(1) C(26) C(27) 116.2(6) yes . . . N(1) C(26) C(27) 116.4(7) yes . . . C(26) C(27) C(28) 123.5(10) yes . . . C(27) C(28) C(29) 117.2(12) yes . . . C(28) C(29) C(30) 120.0(9) yes . . . N(1) C(30) C(29) 123.2(9) yes . . . S(1) C(31) F(1) 113.9(11) yes . . . S(1) C(31) F(2) 110.8(11) yes . . . S(1) C(31) F(3) 112.0(11) yes . . . F(1) C(31) F(2) 106.9(14) yes . . . F(1) C(31) F(3) 108.7(14) yes . . . F(2) C(31) F(3) 103.9(13) yes . . . C(1) C(6) H(1) 110.1 no . . . C(1) C(6) H(2) 109.7 no . . . C(1) C(6) H(3) 108.5 no . . . H(1) C(6) H(2) 109.5 no . . . H(1) C(6) H(3) 109.5 no . . . H(2) C(6) H(3) 109.5 no . . . C(2) C(7) H(4) 108.0 no . . . C(2) C(7) H(5) 110.5 no . . . C(2) C(7) H(6) 109.9 no . . . H(4) C(7) H(5) 109.5 no . . . H(4) C(7) H(6) 109.5 no . . . H(5) C(7) H(6) 109.5 no . . . C(3) C(8) H(7) 111.5 no . . . C(3) C(8) H(8) 107.8 no . . . C(3) C(8) H(9) 109.1 no . . . H(7) C(8) H(8) 109.5 no . . . H(7) C(8) H(9) 109.5 no . . . H(8) C(8) H(9) 109.5 no . . . C(4) C(9) H(10) 107.6 no . . . C(4) C(9) H(11) 111.3 no . . . C(4) C(9) H(12) 109.5 no . . . H(10) C(9) H(11) 109.5 no . . . H(10) C(9) H(12) 109.5 no . . . H(11) C(9) H(12) 109.5 no . . . C(5) C(10) H(13) 108.4 no . . . C(5) C(10) H(14) 110.3 no . . . C(5) C(10) H(15) 109.7 no . . . H(13) C(10) H(14) 109.5 no . . . H(13) C(10) H(15) 109.5 no . . . H(14) C(10) H(15) 109.5 no . . . C(11) C(16) H(16) 108.2 no . . . C(11) C(16) H(17) 109.9 no . . . C(11) C(16) H(18) 110.3 no . . . H(16) C(16) H(17) 109.5 no . . . H(16) C(16) H(18) 109.5 no . . . H(17) C(16) H(18) 109.5 no . . . C(12) C(17) H(19) 109.7 no . . . C(12) C(17) H(20) 111.5 no . . . C(12) C(17) H(21) 107.2 no . . . H(19) C(17) H(20) 109.5 no . . . H(19) C(17) H(21) 109.5 no . . . H(20) C(17) H(21) 109.5 no . . . C(13) C(18) H(22) 108.8 no . . . C(13) C(18) H(23) 110.1 no . . . C(13) C(18) H(24) 109.5 no . . . H(22) C(18) H(23) 109.5 no . . . H(22) C(18) H(24) 109.5 no . . . H(23) C(18) H(24) 109.5 no . . . C(14) C(19) H(25) 108.2 no . . . C(14) C(19) H(26) 109.9 no . . . C(14) C(19) H(27) 110.3 no . . . H(25) C(19) H(26) 109.5 no . . . H(25) C(19) H(27) 109.5 no . . . H(26) C(19) H(27) 109.5 no . . . C(15) C(20) H(28) 111.1 no . . . C(15) C(20) H(29) 108.6 no . . . C(15) C(20) H(30) 108.6 no . . . H(28) C(20) H(29) 109.5 no . . . H(28) C(20) H(30) 109.5 no . . . H(29) C(20) H(30) 109.5 no . . . P(1) C(21) H(31) 110.1 no . . . P(1) C(21) H(32) 109.3 no . . . P(1) C(21) H(33) 109.0 no . . . H(31) C(21) H(32) 109.5 no . . . H(31) C(21) H(33) 109.5 no . . . H(32) C(21) H(33) 109.5 no . . . P(1) C(22) H(34) 108.8 no . . . P(1) C(22) H(35) 109.8 no . . . P(1) C(22) H(36) 109.8 no . . . H(34) C(22) H(35) 109.5 no . . . H(34) C(22) H(36) 109.5 no . . . H(35) C(22) H(36) 109.5 no . . . P(1) C(23) H(37) 107.6 no . . . P(1) C(23) H(38) 107.6 no . . . P(2) C(23) H(37) 107.6 no . . . P(2) C(23) H(38) 107.6 no . . . H(37) C(23) H(38) 109.5 no . . . P(2) C(24) H(39) 109.7 no . . . P(2) C(24) H(40) 110.2 no . . . P(2) C(24) H(41) 108.5 no . . . H(39) C(24) H(40) 109.5 no . . . H(39) C(24) H(41) 109.5 no . . . H(40) C(24) H(41) 109.5 no . . . P(2) C(25) H(42) 109.5 no . . . P(2) C(25) H(43) 109.2 no . . . P(2) C(25) H(44) 109.7 no . . . H(42) C(25) H(43) 109.5 no . . . H(42) C(25) H(44) 109.5 no . . . H(43) C(25) H(44) 109.5 no . . . C(26) C(27) H(45) 118.3 no . . . C(28) C(27) H(45) 118.2 no . . . C(27) C(28) H(46) 121.6 no . . . C(29) C(28) H(46) 121.2 no . . . C(28) C(29) H(47) 119.9 no . . . C(30) C(29) H(47) 120.0 no . . . N(1) C(30) H(48) 118.1 no . . . C(29) C(30) H(48) 118.7 no . . . #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================