# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Munetaka Akita' _publ_contact_author_address ; Chemical Resources Laboratory Tokyo Institute of Technology R1-27, 4259 Nagatsuta, Midori-ku Yokohama 226-8503 JAPAN ; _publ_contact_author_email MAKITA@RES.TITECH.AC.JP _publ_section_title ; A New Method for the Conversion of Allyl Alcohol into p-Allyl Species Promoted by Nucleophilic Interaction with a CO Ligand ; loop_ _publ_author_name 'Munetaka Akita' 'Christian Dubs' 'Akiko Inagaki' 'Toshiki Yamamoto' # Attachment 'B601143H(rev)CIF' #------------------------------------------------------------------------------ data_compound_4b _database_code_depnum_ccdc_archive 'CCDC 296203' _audit_creation_date 'Wed Jul 20 15:58:22 2005' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C29 H25 Ir N O3 P ' _chemical_formula_moiety 'C29 H25 Ir N O3 P ' _chemical_formula_weight 658.72 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 10.4334(8) _cell_length_b 14.1368(9) _cell_length_c 16.992(1) _cell_angle_alpha 90 _cell_angle_beta 94.627(4) _cell_angle_gamma 90 _cell_volume 2498.0(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 13311 _cell_measurement_theta_min 3.6 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 213 #------------------------------------------------------------------------------ _exptl_crystal_description unknown _exptl_crystal_colour unknown _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.751 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 5.455 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.408 _exptl_absorpt_correction_T_max 0.580 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_ambient_temperature 213 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 19880 _diffrn_reflns_av_R_equivalents 0.041 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5571 _reflns_number_gt 4960 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.1172 _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 4960 _refine_ls_number_parameters 332 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0020 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_diff_density_max 0.86 _refine_diff_density_min -2.69 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) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 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) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.03973(2) 0.65825(1) 0.32160(1) 0.0243(1) Uani 1.00 d . . . P(1) P 0.2118(1) 0.62550(8) 0.24752(7) 0.0246(2) Uani 1.00 d . . . O(1) O 0.1841(4) 0.8341(2) 0.3546(2) 0.0351(8) Uani 1.00 d . . . O(2) O 0.1444(4) 0.5928(3) 0.4843(2) 0.054(1) Uani 1.00 d . . . O(3) O -0.0236(4) 0.8507(2) 0.3621(3) 0.0384(9) Uani 1.00 d . . . N(1) N -0.0098(4) 0.5134(3) 0.2868(2) 0.0280(8) Uani 1.00 d . . . C(1) C 0.0808(5) 0.7935(3) 0.3498(3) 0.0290(9) Uani 1.00 d . . . C(01) C -0.1473(5) 0.8046(4) 0.3603(4) 0.038(1) Uani 1.00 d . . . C(2) C 0.1040(5) 0.6174(4) 0.4233(3) 0.0332(10) Uani 1.00 d . . . C(02) C -0.1486(4) 0.7137(3) 0.3140(3) 0.0305(9) Uani 1.00 d . . . C(03) C -0.1034(4) 0.7179(3) 0.2356(3) 0.0267(9) Uani 1.00 d . . . C(04) C -0.1582(5) 0.6617(3) 0.1678(3) 0.031(1) Uani 1.00 d . . . C(05) C -0.1129(7) 0.6768(5) 0.0921(4) 0.050(2) Uani 1.00 d . . . C(06) C -0.1660(8) 0.6324(6) 0.0261(4) 0.066(2) Uani 1.00 d . . . C(07) C -0.2664(7) 0.5674(5) 0.0320(4) 0.060(2) Uani 1.00 d . . . C(08) C -0.3119(6) 0.5516(4) 0.1040(4) 0.048(1) Uani 1.00 d . . . C(09) C -0.2592(5) 0.5978(3) 0.1712(3) 0.038(1) Uani 1.00 d . . . C(11) C 0.0541(4) 0.4687(3) 0.2322(3) 0.0274(9) Uani 1.00 d . . . C(12) C 0.0314(5) 0.3728(3) 0.2154(3) 0.0324(10) Uani 1.00 d . . . C(13) C -0.0559(5) 0.3240(4) 0.2563(4) 0.039(1) Uani 1.00 d . . . C(14) C -0.1207(5) 0.3702(4) 0.3119(4) 0.038(1) Uani 1.00 d . . . C(15) C -0.0965(4) 0.4651(3) 0.3259(3) 0.0316(10) Uani 1.00 d . . . C(16) C 0.1486(4) 0.5245(3) 0.1890(3) 0.0310(9) Uani 1.00 d . . . C(21) C 0.2673(4) 0.7043(3) 0.1722(3) 0.0279(9) Uani 1.00 d . . . C(22) C 0.2120(5) 0.7928(3) 0.1602(3) 0.0322(10) Uani 1.00 d . . . C(23) C 0.2537(6) 0.8535(4) 0.1027(4) 0.038(1) Uani 1.00 d . . . C(24) C 0.3507(6) 0.8240(4) 0.0570(3) 0.041(1) Uani 1.00 d . . . C(25) C 0.4067(5) 0.7373(4) 0.0688(3) 0.041(1) Uani 1.00 d . . . C(26) C 0.3652(5) 0.6770(4) 0.1259(3) 0.035(1) Uani 1.00 d . . . C(31) C 0.3602(4) 0.5882(3) 0.3029(3) 0.0281(9) Uani 1.00 d . . . C(32) C 0.3964(5) 0.6391(4) 0.3718(3) 0.033(1) Uani 1.00 d . . . C(33) C 0.5062(5) 0.6147(4) 0.4195(3) 0.042(1) Uani 1.00 d . . . C(34) C 0.5808(5) 0.5395(4) 0.3984(4) 0.045(1) Uani 1.00 d . . . C(35) C 0.5471(5) 0.4896(4) 0.3294(3) 0.040(1) Uani 1.00 d . . . C(36) C 0.4387(5) 0.5132(3) 0.2821(3) 0.0328(10) Uani 1.00 d . . . H(1) H -0.169(5) 0.784(4) 0.413(3) 0.0333(2) Uiso 1.00 d . . . H(2) H -0.207(8) 0.849(4) 0.342(5) 0.0621(3) Uiso 1.00 d . . . H(3) H -0.224(5) 0.674(3) 0.326(3) 0.0126(1) Uiso 1.00 d . . . H(4) H -0.078(5) 0.779(4) 0.220(3) 0.0367(2) Uiso 1.00 d . . . H(5) H -0.0429 0.7195 0.0870 0.0610 Uiso 1.00 calc . . . H(6) H -0.1344 0.6442 -0.0242 0.0773 Uiso 1.00 calc . . . H(7) H -0.3036 0.5350 -0.0133 0.0725 Uiso 1.00 calc . . . H(8) H -0.3807 0.5077 0.1086 0.0580 Uiso 1.00 calc . . . H(9) H -0.2939 0.5854 0.2205 0.0464 Uiso 1.00 calc . . . H(10) H 0.1061 0.5475 0.1405 0.0384 Uiso 1.00 calc . . . H(11) H 0.2177 0.4848 0.1769 0.0384 Uiso 1.00 calc . . . H(12) H 0.0768 0.3417 0.1761 0.0393 Uiso 1.00 calc . . . H(13) H -0.0713 0.2578 0.2459 0.0468 Uiso 1.00 calc . . . H(14) H -0.1826 0.3375 0.3403 0.0461 Uiso 1.00 calc . . . H(15) H -0.1409 0.4981 0.3649 0.0390 Uiso 1.00 calc . . . H(16) H 0.1459 0.8126 0.1919 0.0391 Uiso 1.00 calc . . . H(17) H 0.2139 0.9141 0.0939 0.0471 Uiso 1.00 calc . . . H(18) H 0.3785 0.8659 0.0174 0.0495 Uiso 1.00 calc . . . H(19) H 0.4763 0.7173 0.0385 0.0499 Uiso 1.00 calc . . . H(20) H 0.4036 0.6158 0.1336 0.0429 Uiso 1.00 calc . . . H(21) H 0.3459 0.6925 0.3860 0.0413 Uiso 1.00 calc . . . H(22) H 0.5291 0.6501 0.4666 0.0501 Uiso 1.00 calc . . . H(23) H 0.6563 0.5234 0.4318 0.0523 Uiso 1.00 calc . . . H(24) H 0.5994 0.4381 0.3146 0.0481 Uiso 1.00 calc . . . H(25) H 0.4152 0.4776 0.2347 0.0403 Uiso 1.00 calc . . . 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) 0.0231(1) 0.0251(1) 0.0250(1) 0.00176(6) 0.00289(8) 0.00265(5) P(1) 0.0239(5) 0.0252(5) 0.0249(6) -0.0009(5) 0.0031(4) 0.0002(4) O(1) 0.034(2) 0.032(2) 0.039(2) -0.005(1) 0.001(2) -0.003(1) O(2) 0.060(2) 0.074(3) 0.028(2) 0.013(2) -0.001(2) 0.016(2) O(3) 0.034(2) 0.030(2) 0.051(3) 0.005(1) 0.002(2) -0.006(1) N(1) 0.026(2) 0.025(2) 0.033(2) 0.000(2) 0.000(1) 0.003(1) C(1) 0.035(2) 0.028(2) 0.024(2) 0.005(2) 0.003(2) 0.001(2) C(01) 0.031(2) 0.039(3) 0.045(3) 0.011(2) 0.002(2) 0.000(2) C(2) 0.030(2) 0.037(2) 0.033(3) 0.001(2) 0.008(2) 0.001(2) C(02) 0.021(2) 0.034(2) 0.037(3) 0.008(2) 0.004(2) 0.003(2) C(03) 0.026(2) 0.026(2) 0.026(2) 0.004(2) -0.008(2) 0.005(2) C(04) 0.026(2) 0.031(2) 0.035(3) 0.002(2) -0.005(2) 0.006(2) C(05) 0.054(4) 0.059(3) 0.035(3) -0.021(3) -0.007(3) 0.008(3) C(06) 0.074(5) 0.088(5) 0.034(4) -0.027(4) -0.005(3) -0.001(3) C(07) 0.073(4) 0.060(4) 0.044(4) -0.021(4) -0.014(3) -0.004(3) C(08) 0.044(3) 0.037(3) 0.060(4) -0.013(3) -0.014(3) 0.002(2) C(09) 0.036(2) 0.028(2) 0.048(3) -0.002(2) -0.001(2) 0.003(2) C(11) 0.025(2) 0.028(2) 0.028(2) 0.002(2) -0.002(2) 0.001(2) C(12) 0.032(2) 0.026(2) 0.039(3) -0.002(2) -0.003(2) -0.003(2) C(13) 0.027(2) 0.031(2) 0.058(4) -0.005(2) -0.009(2) 0.001(2) C(14) 0.028(2) 0.033(2) 0.051(3) -0.008(2) -0.002(2) 0.010(2) C(15) 0.025(2) 0.031(2) 0.039(3) -0.001(2) 0.006(2) 0.006(2) C(16) 0.029(2) 0.030(2) 0.034(3) -0.001(2) 0.003(2) -0.002(2) C(21) 0.026(2) 0.036(2) 0.023(2) -0.003(2) 0.002(2) 0.000(2) C(22) 0.035(2) 0.033(2) 0.029(2) -0.002(2) 0.005(2) 0.004(2) C(23) 0.043(3) 0.036(2) 0.036(3) -0.002(2) 0.004(2) 0.008(2) C(24) 0.039(3) 0.056(3) 0.028(3) -0.011(3) 0.005(2) 0.009(2) C(25) 0.036(3) 0.057(3) 0.033(3) -0.002(2) 0.011(2) 0.000(2) C(26) 0.037(3) 0.038(2) 0.031(3) 0.000(2) 0.005(2) 0.001(2) C(31) 0.028(2) 0.029(2) 0.029(2) -0.003(2) 0.005(2) 0.005(2) C(32) 0.026(2) 0.037(2) 0.036(3) 0.002(2) -0.001(2) -0.001(2) C(33) 0.034(2) 0.055(3) 0.036(3) 0.005(3) -0.006(2) -0.004(2) C(34) 0.028(2) 0.056(3) 0.049(3) 0.005(2) -0.005(2) 0.010(3) C(35) 0.029(3) 0.032(3) 0.059(4) 0.009(2) 0.006(2) 0.002(2) C(36) 0.032(2) 0.028(2) 0.039(3) 0.001(2) 0.007(2) -0.003(2) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS86 _computing_structure_refinement SHELXL97 _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir(1) P(1) 2.321(1) . . yes Ir(1) N(1) 2.182(4) . . yes Ir(1) C(1) 2.009(5) . . yes Ir(1) C(2) 1.893(5) . . yes Ir(1) C(02) 2.110(4) . . yes Ir(1) C(03) 2.174(4) . . yes P(1) C(16) 1.832(5) . . yes P(1) C(21) 1.826(5) . . yes P(1) C(31) 1.824(4) . . yes O(1) C(1) 1.219(6) . . yes O(2) C(2) 1.140(6) . . yes O(3) C(1) 1.385(6) . . yes O(3) C(01) 1.444(7) . . yes N(1) C(11) 1.343(6) . . yes N(1) C(15) 1.350(6) . . yes C(01) C(02) 1.506(7) . . yes C(02) C(03) 1.449(7) . . yes C(03) C(04) 1.476(7) . . yes C(04) C(05) 1.421(9) . . yes C(04) C(09) 1.393(7) . . yes C(05) C(06) 1.363(10) . . yes C(06) C(07) 1.40(1) . . yes C(07) C(08) 1.367(10) . . yes C(08) C(09) 1.390(8) . . yes C(11) C(12) 1.401(6) . . yes C(11) C(16) 1.500(7) . . yes C(12) C(13) 1.375(8) . . yes C(13) C(14) 1.371(8) . . yes C(14) C(15) 1.382(7) . . yes C(21) C(22) 1.386(7) . . yes C(21) C(26) 1.395(7) . . yes C(22) C(23) 1.395(8) . . yes C(23) C(24) 1.389(9) . . yes C(24) C(25) 1.366(8) . . yes C(25) C(26) 1.387(8) . . yes C(31) C(32) 1.399(7) . . yes C(31) C(36) 1.403(7) . . yes C(32) C(33) 1.392(7) . . yes C(33) C(34) 1.382(8) . . yes C(34) C(35) 1.389(8) . . yes C(35) C(36) 1.375(7) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P(1) Ir(1) N(1) 80.9(1) . . . yes P(1) Ir(1) C(1) 99.2(1) . . . yes P(1) Ir(1) C(2) 101.7(2) . . . yes P(1) Ir(1) C(02) 142.9(1) . . . yes P(1) Ir(1) C(03) 103.4(1) . . . yes N(1) Ir(1) C(1) 177.6(2) . . . yes N(1) Ir(1) C(2) 91.1(2) . . . yes N(1) Ir(1) C(02) 97.7(2) . . . yes N(1) Ir(1) C(03) 92.7(2) . . . yes C(1) Ir(1) C(2) 91.1(2) . . . yes C(1) Ir(1) C(02) 80.8(2) . . . yes C(1) Ir(1) C(03) 85.0(2) . . . yes C(2) Ir(1) C(02) 115.4(2) . . . yes C(2) Ir(1) C(03) 154.9(2) . . . yes C(02) Ir(1) C(03) 39.5(2) . . . yes Ir(1) P(1) C(16) 100.9(2) . . . yes Ir(1) P(1) C(21) 124.1(2) . . . yes Ir(1) P(1) C(31) 116.1(2) . . . yes C(16) P(1) C(21) 102.5(2) . . . yes C(16) P(1) C(31) 108.0(2) . . . yes C(21) P(1) C(31) 103.5(2) . . . yes C(1) O(3) C(01) 116.4(4) . . . yes Ir(1) N(1) C(11) 120.6(3) . . . yes Ir(1) N(1) C(15) 119.7(3) . . . yes C(11) N(1) C(15) 119.4(4) . . . yes Ir(1) C(1) O(1) 129.4(4) . . . yes Ir(1) C(1) O(3) 115.9(3) . . . yes O(1) C(1) O(3) 114.6(4) . . . yes O(3) C(01) C(02) 111.5(4) . . . yes Ir(1) C(2) O(2) 179.0(5) . . . yes Ir(1) C(02) C(01) 108.4(3) . . . yes Ir(1) C(02) C(03) 72.6(3) . . . yes C(01) C(02) C(03) 117.1(4) . . . yes Ir(1) C(03) C(02) 67.9(2) . . . yes Ir(1) C(03) C(04) 121.2(3) . . . yes C(02) C(03) C(04) 124.2(4) . . . yes C(03) C(04) C(05) 119.3(5) . . . yes C(03) C(04) C(09) 124.2(5) . . . yes C(05) C(04) C(09) 116.3(5) . . . yes C(04) C(05) C(06) 122.2(6) . . . yes C(05) C(06) C(07) 120.0(7) . . . yes C(06) C(07) C(08) 119.1(6) . . . yes C(07) C(08) C(09) 121.0(6) . . . yes C(04) C(09) C(08) 121.4(5) . . . yes N(1) C(11) C(12) 120.7(4) . . . yes N(1) C(11) C(16) 118.3(4) . . . yes C(12) C(11) C(16) 121.0(4) . . . yes C(11) C(12) C(13) 119.4(5) . . . yes C(12) C(13) C(14) 119.5(5) . . . yes C(13) C(14) C(15) 119.1(5) . . . yes N(1) C(15) C(14) 121.8(5) . . . yes P(1) C(16) C(11) 111.5(3) . . . yes P(1) C(21) C(22) 120.2(4) . . . yes P(1) C(21) C(26) 121.0(4) . . . yes C(22) C(21) C(26) 118.8(4) . . . yes C(21) C(22) C(23) 120.6(5) . . . yes C(22) C(23) C(24) 119.3(5) . . . yes C(23) C(24) C(25) 120.6(5) . . . yes C(24) C(25) C(26) 120.1(5) . . . yes C(21) C(26) C(25) 120.6(5) . . . yes P(1) C(31) C(32) 116.3(3) . . . yes P(1) C(31) C(36) 125.2(4) . . . yes C(32) C(31) C(36) 118.4(4) . . . yes C(31) C(32) C(33) 120.8(5) . . . yes C(32) C(33) C(34) 119.7(5) . . . yes C(33) C(34) C(35) 120.0(5) . . . yes C(34) C(35) C(36) 120.7(5) . . . yes C(31) C(36) C(35) 120.3(5) . . . yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ir(1) P(1) C(16) C(11) -29.2(3) . . . . yes Ir(1) P(1) C(21) C(22) 4.7(4) . . . . yes Ir(1) P(1) C(21) C(26) -175.2(3) . . . . yes Ir(1) P(1) C(31) C(32) -43.6(4) . . . . yes Ir(1) P(1) C(31) C(36) 135.9(4) . . . . yes Ir(1) N(1) C(11) C(12) 173.6(3) . . . . yes Ir(1) N(1) C(11) C(16) -7.4(5) . . . . yes Ir(1) N(1) C(15) C(14) -172.8(4) . . . . yes Ir(1) C(1) O(3) C(01) 5.4(6) . . . . yes Ir(1) C(02) C(01) O(3) 28.5(5) . . . . yes Ir(1) C(02) C(03) C(04) 113.6(4) . . . . yes Ir(1) C(03) C(02) C(01) 102.2(4) . . . . yes Ir(1) C(03) C(04) C(05) -101.8(5) . . . . yes Ir(1) C(03) C(04) C(09) 82.7(6) . . . . yes P(1) Ir(1) N(1) C(11) -10.1(3) . . . . yes P(1) Ir(1) N(1) C(15) 163.4(3) . . . . yes P(1) Ir(1) C(1) O(1) -25.2(5) . . . . yes P(1) Ir(1) C(1) O(3) 151.4(3) . . . . yes P(1) Ir(1) C(2) O(2) 18(27) . . . . yes P(1) Ir(1) C(02) C(01) -113.4(3) . . . . yes P(1) Ir(1) C(02) C(03) 0.2(4) . . . . yes P(1) Ir(1) C(03) C(02) -179.9(2) . . . . yes P(1) Ir(1) C(03) C(04) 62.5(4) . . . . yes P(1) C(16) C(11) N(1) 25.9(5) . . . . yes P(1) C(16) C(11) C(12) -155.1(4) . . . . yes P(1) C(21) C(22) C(23) -180.0(4) . . . . yes P(1) C(21) C(26) C(25) 180.0(4) . . . . yes P(1) C(31) C(32) C(33) 178.2(4) . . . . yes P(1) C(31) C(36) C(35) -178.3(4) . . . . yes O(1) C(1) Ir(1) N(1) -118(4) . . . . yes O(1) C(1) Ir(1) C(2) 76.8(5) . . . . yes O(1) C(1) Ir(1) C(02) -167.6(5) . . . . yes O(1) C(1) Ir(1) C(03) -128.0(5) . . . . yes O(1) C(1) O(3) C(01) -177.4(5) . . . . yes O(2) C(2) Ir(1) N(1) 99(27) . . . . yes O(2) C(2) Ir(1) C(1) -81(27) . . . . yes O(2) C(2) Ir(1) C(02) -161(27) . . . . yes O(2) C(2) Ir(1) C(03) -162(27) . . . . yes O(3) C(1) Ir(1) N(1) 58(4) . . . . yes O(3) C(1) Ir(1) C(2) -106.6(4) . . . . yes O(3) C(1) Ir(1) C(02) 9.0(4) . . . . yes O(3) C(1) Ir(1) C(03) 48.6(4) . . . . yes O(3) C(01) C(02) C(03) -50.9(6) . . . . yes N(1) Ir(1) P(1) C(16) 19.2(2) . . . . yes N(1) Ir(1) P(1) C(21) 132.6(2) . . . . yes N(1) Ir(1) P(1) C(31) -97.2(2) . . . . yes N(1) Ir(1) C(02) C(01) 161.6(3) . . . . yes N(1) Ir(1) C(02) C(03) -84.9(3) . . . . yes N(1) Ir(1) C(03) C(02) 98.8(3) . . . . yes N(1) Ir(1) C(03) C(04) -18.8(4) . . . . yes N(1) C(11) C(12) C(13) -1.0(7) . . . . yes N(1) C(15) C(14) C(13) -0.7(8) . . . . yes C(1) Ir(1) P(1) C(16) -158.4(2) . . . . yes C(1) Ir(1) P(1) C(21) -45.1(2) . . . . yes C(1) Ir(1) P(1) C(31) 85.2(2) . . . . yes C(1) Ir(1) N(1) C(11) 83(4) . . . . yes C(1) Ir(1) N(1) C(15) -102(4) . . . . yes C(1) Ir(1) C(02) C(01) -20.2(4) . . . . yes C(1) Ir(1) C(02) C(03) 93.3(3) . . . . yes C(1) Ir(1) C(03) C(02) -81.6(3) . . . . yes C(1) Ir(1) C(03) C(04) 160.8(4) . . . . yes C(1) O(3) C(01) C(02) -23.2(6) . . . . yes C(01) C(02) Ir(1) C(2) 66.7(4) . . . . yes C(01) C(02) Ir(1) C(03) -113.5(4) . . . . yes C(01) C(02) C(03) C(04) -144.2(4) . . . . yes C(2) Ir(1) P(1) C(16) 108.5(2) . . . . yes C(2) Ir(1) P(1) C(21) -138.1(2) . . . . yes C(2) Ir(1) P(1) C(31) -7.9(2) . . . . yes C(2) Ir(1) N(1) C(11) -111.7(4) . . . . yes C(2) Ir(1) N(1) C(15) 61.7(4) . . . . yes C(2) Ir(1) C(02) C(03) -179.8(3) . . . . yes C(2) Ir(1) C(03) C(02) 0.4(6) . . . . yes C(2) Ir(1) C(03) C(04) -117.2(5) . . . . yes C(02) Ir(1) P(1) C(16) -71.5(3) . . . . yes C(02) Ir(1) P(1) C(21) 41.9(3) . . . . yes C(02) Ir(1) P(1) C(31) 172.1(3) . . . . yes C(02) Ir(1) N(1) C(11) 132.5(3) . . . . yes C(02) Ir(1) N(1) C(15) -54.1(4) . . . . yes C(02) Ir(1) C(03) C(04) -117.6(5) . . . . yes C(02) C(03) C(04) C(05) 175.2(5) . . . . yes C(02) C(03) C(04) C(09) -0.4(7) . . . . yes C(03) Ir(1) P(1) C(16) -71.4(2) . . . . yes C(03) Ir(1) P(1) C(21) 42.0(2) . . . . yes C(03) Ir(1) P(1) C(31) 172.2(2) . . . . yes C(03) Ir(1) N(1) C(11) 93.1(3) . . . . yes C(03) Ir(1) N(1) C(15) -93.5(3) . . . . yes C(03) C(04) C(05) C(06) -175.0(6) . . . . yes C(03) C(04) C(09) C(08) 175.8(5) . . . . yes C(04) C(05) C(06) C(07) -1(1) . . . . yes C(04) C(09) C(08) C(07) -0.1(8) . . . . yes C(05) C(04) C(09) C(08) 0.1(7) . . . . yes C(05) C(06) C(07) C(08) 1(1) . . . . yes C(06) C(05) C(04) C(09) 0.9(9) . . . . yes C(06) C(07) C(08) C(09) -0.9(10) . . . . yes C(11) N(1) C(15) C(14) 0.7(7) . . . . yes C(11) C(12) C(13) C(14) 1.0(8) . . . . yes C(11) C(16) P(1) C(21) -158.1(3) . . . . yes C(11) C(16) P(1) C(31) 93.0(3) . . . . yes C(12) C(11) N(1) C(15) 0.2(6) . . . . yes C(12) C(13) C(14) C(15) -0.2(8) . . . . yes C(13) C(12) C(11) C(16) 180.0(4) . . . . yes C(15) N(1) C(11) C(16) 179.2(4) . . . . yes C(16) P(1) C(21) C(22) 117.3(4) . . . . yes C(16) P(1) C(21) C(26) -62.6(4) . . . . yes C(16) P(1) C(31) C(32) -156.0(4) . . . . yes C(16) P(1) C(31) C(36) 23.5(5) . . . . yes C(21) P(1) C(31) C(32) 95.9(4) . . . . yes C(21) P(1) C(31) C(36) -84.6(4) . . . . yes C(21) C(22) C(23) C(24) 0.6(8) . . . . yes C(21) C(26) C(25) C(24) -0.7(8) . . . . yes C(22) C(21) P(1) C(31) -130.5(4) . . . . yes C(22) C(21) C(26) C(25) 0.1(7) . . . . yes C(22) C(23) C(24) C(25) -1.3(8) . . . . yes C(23) C(22) C(21) C(26) -0.1(7) . . . . yes C(23) C(24) C(25) C(26) 1.3(8) . . . . yes C(26) C(21) P(1) C(31) 49.7(4) . . . . yes C(31) C(32) C(33) C(34) 0.3(8) . . . . yes C(31) C(36) C(35) C(34) -0.1(8) . . . . yes C(32) C(31) C(36) C(35) 1.2(7) . . . . yes C(32) C(33) C(34) C(35) 0.9(9) . . . . yes C(33) C(32) C(31) C(36) -1.3(8) . . . . yes C(33) C(34) C(35) C(36) -0.9(9) . . . . yes C(33) C(34) C(35) C(36) -0.9(9) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) C(06) 3.230(8) . 4_565 ? O(1) C(07) 3.322(8) . 4_565 ? O(1) C(16) 3.324(6) . 2_555 ? O(1) C(12) 3.331(6) . 2_555 ? O(2) C(15) 3.404(7) . 3_566 ? O(2) C(14) 3.531(7) . 3_566 ? O(2) C(24) 3.593(8) . 4_465 ? O(3) C(08) 3.391(7) . 2_455 ? O(3) C(36) 3.522(7) . 2_555 ? C(01) C(13) 3.550(8) . 2_455 ? C(01) C(08) 3.575(8) . 2_455 ? C(01) C(25) 3.592(8) . 4_465 ? C(02) C(13) 3.573(7) . 2_455 ? C(12) C(22) 3.464(7) . 2_545 ? C(13) C(26) 3.412(8) . 2_545 ? C(13) C(25) 3.465(8) . 2_545 ? C(13) C(21) 3.580(7) . 2_545 ? C(14) C(25) 3.448(8) . 2_545 ? C(14) C(24) 3.509(8) . 2_545 ? #------------------------------------------------------------------------------ #===END #------------------------------------------------------------------------------ data_compound_5_BF4 _database_code_depnum_ccdc_archive 'CCDC 296204' _audit_creation_date 'Wed Aug 24 15:54:34 2005' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C26 H26 B F4 Ir N O3 P ' _chemical_formula_moiety 'C26 H26 B F4 Ir N O3 P ' _chemical_formula_weight 710.49 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 33.60(1) _cell_length_b 10.959(2) _cell_length_c 15.568(5) _cell_angle_alpha 90 _cell_angle_beta 112.406(8) _cell_angle_gamma 90 _cell_volume 5298(2) _cell_formula_units_Z 8 _cell_measurement_reflns_used 18706 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 213 #------------------------------------------------------------------------------ _exptl_crystal_description unknown _exptl_crystal_colour unknown _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.781 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 5.171 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.355 _exptl_absorpt_correction_T_max 0.596 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_ambient_temperature 213 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 18920 _diffrn_reflns_av_R_equivalents 0.087 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5997 _reflns_number_gt 4549 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0633 _refine_ls_wR_factor_ref 0.1710 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4549 _refine_ls_number_parameters 334 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0200 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_diff_density_max 1.20 _refine_diff_density_min -3.14 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) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 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) ; B B 0.001 0.001 ;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) ; 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) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.13431(1) 0.23633(3) 0.33199(2) 0.0544(1) Uani 1.00 d . . . P(1) P 0.13091(6) 0.1087(2) 0.2118(1) 0.0490(4) Uani 1.00 d . . . F(1) F 0.3127(2) 0.1672(7) 0.2124(4) 0.110(2) Uani 1.00 d . . . F(2) F 0.2554(3) 0.2212(9) 0.2304(9) 0.164(4) Uani 1.00 d . . . F(3) F 0.3196(4) 0.2436(8) 0.3455(6) 0.181(6) Uani 1.00 d . . . F(4) F 0.2887(2) 0.0557(6) 0.3063(4) 0.106(2) Uani 1.00 d . . . O(1) O 0.0999(2) 0.4707(6) 0.2431(6) 0.109(3) Uani 1.00 d . . . O(2) O 0.0577(2) 0.1391(7) 0.3684(5) 0.090(2) Uani 1.00 d . . . O(3) O 0.0580(2) 0.3128(7) 0.1830(5) 0.086(2) Uani 1.00 d . . . N(1) N 0.1783(2) 0.0921(5) 0.4113(4) 0.052(1) Uani 1.00 d . . . C(1) C 0.0936(3) 0.3635(8) 0.2447(6) 0.073(2) Uani 1.00 d . . . C(01) C 0.0303(5) 0.392(1) 0.1099(9) 0.124(5) Uani 1.00 d . . . C(2) C 0.0864(3) 0.1741(7) 0.3529(5) 0.063(2) Uani 1.00 d . . . C(02) C -0.0001(6) 0.454(2) 0.131(1) 0.186(9) Uani 1.00 d . . . C(03) C -0.0432(5) 0.453(2) 0.085(1) 0.22(1) Uani 1.00 d . . . C(04) C 0.1887(3) 0.3519(8) 0.3350(7) 0.083(3) Uani 1.00 d . . . C(05) C 0.1865(3) 0.3561(9) 0.4231(8) 0.087(3) Uani 1.00 d . . . C(06) C 0.1521(4) 0.3831(10) 0.4421(7) 0.091(3) Uani 1.00 d . . . C(11) C 0.1958(2) 0.0174(6) 0.3651(5) 0.049(1) Uani 1.00 d . . . C(12) C 0.2250(3) -0.0735(7) 0.4131(5) 0.060(2) Uani 1.00 d . . . C(13) C 0.2357(3) -0.0843(8) 0.5065(5) 0.064(2) Uani 1.00 d . . . C(14) C 0.2168(3) -0.0088(8) 0.5519(5) 0.064(2) Uani 1.00 d . . . C(15) C 0.1892(3) 0.0769(7) 0.5030(5) 0.059(2) Uani 1.00 d . . . C(16) C 0.1833(2) 0.0380(7) 0.2631(5) 0.052(1) Uani 1.00 d . . . C(21) C 0.0913(2) -0.0133(7) 0.1853(5) 0.053(2) Uani 1.00 d . . . C(22) C 0.0481(3) 0.0168(7) 0.1579(6) 0.069(2) Uani 1.00 d . . . C(23) C 0.0175(3) -0.0727(9) 0.1383(8) 0.087(3) Uani 1.00 d . . . C(24) C 0.0292(3) -0.1942(10) 0.1470(8) 0.085(3) Uani 1.00 d . . . C(25) C 0.0728(4) -0.2260(8) 0.1754(8) 0.076(2) Uani 1.00 d . . . C(26) C 0.1028(3) -0.1344(7) 0.1933(5) 0.061(2) Uani 1.00 d . . . C(31) C 0.1284(2) 0.1701(7) 0.1011(5) 0.054(2) Uani 1.00 d . . . C(32) C 0.1533(3) 0.2713(7) 0.0994(6) 0.067(2) Uani 1.00 d . . . C(33) C 0.1544(3) 0.3146(8) 0.0203(6) 0.069(2) Uani 1.00 d . . . C(34) C 0.1303(4) 0.2589(8) -0.0646(7) 0.074(2) Uani 1.00 d . . . C(35) C 0.1047(3) 0.1611(9) -0.0656(5) 0.074(2) Uani 1.00 d . . . C(36) C 0.1044(3) 0.1124(8) 0.0176(5) 0.065(2) Uani 1.00 d . . . B(1) B 0.2957(4) 0.1680(10) 0.2817(9) 0.081(3) Uani 1.00 d . . . H(1) H 0.0464 0.4411 0.0844 0.1539 Uiso 1.00 calc . . . H(2) H 0.0123 0.3376 0.0552 0.1539 Uiso 1.00 calc . . . H(3) H 0.0121 0.5132 0.1890 0.2299 Uiso 1.00 calc . . . H(4) H -0.0644 0.4910 0.0965 0.2564 Uiso 1.00 calc . . . H(5) H -0.0528 0.3936 0.0290 0.2564 Uiso 1.00 calc . . . H(6) H 0.2131 0.3123 0.3281 0.1039 Uiso 1.00 calc . . . H(7) H 0.1828 0.4244 0.2980 0.1039 Uiso 1.00 calc . . . H(8) H 0.2093 0.3160 0.4746 0.1091 Uiso 1.00 calc . . . H(9) H 0.1502 0.3673 0.5003 0.1115 Uiso 1.00 calc . . . H(10) H 0.1390 0.4653 0.4227 0.1115 Uiso 1.00 calc . . . H(11) H 0.2371 -0.1268 0.3799 0.0725 Uiso 1.00 calc . . . H(12) H 0.2565 -0.1443 0.5425 0.0760 Uiso 1.00 calc . . . H(13) H 0.2237 -0.0178 0.6180 0.0771 Uiso 1.00 calc . . . H(14) H 0.1762 0.1297 0.5345 0.0707 Uiso 1.00 calc . . . H(15) H 0.1829 -0.0391 0.2329 0.0614 Uiso 1.00 calc . . . H(16) H 0.2044 0.0887 0.2528 0.0614 Uiso 1.00 calc . . . H(17) H 0.0404 0.1001 0.1558 0.0807 Uiso 1.00 calc . . . H(18) H -0.0119 -0.0496 0.1170 0.1052 Uiso 1.00 calc . . . H(19) H 0.0074 -0.2562 0.1351 0.1013 Uiso 1.00 calc . . . H(20) H 0.0814 -0.3107 0.1795 0.0923 Uiso 1.00 calc . . . H(21) H 0.1331 -0.1547 0.2128 0.0725 Uiso 1.00 calc . . . H(22) H 0.1699 0.3115 0.1566 0.0819 Uiso 1.00 calc . . . H(23) H 0.1722 0.3839 0.0223 0.0815 Uiso 1.00 calc . . . H(24) H 0.1324 0.2910 -0.1202 0.0876 Uiso 1.00 calc . . . H(25) H 0.0867 0.1238 -0.1248 0.0880 Uiso 1.00 calc . . . H(26) H 0.0875 0.0403 0.0180 0.0787 Uiso 1.00 calc . . . 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) 0.0590(2) 0.0471(2) 0.0613(2) -0.0023(1) 0.0275(2) -0.0050(1) P(1) 0.0530(10) 0.0457(9) 0.0505(9) -0.0020(7) 0.0222(8) -0.0006(7) F(1) 0.135(5) 0.113(5) 0.102(4) -0.019(4) 0.067(4) -0.020(4) F(2) 0.141(8) 0.144(7) 0.23(1) 0.036(6) 0.102(8) 0.091(7) F(3) 0.27(1) 0.200(10) 0.108(6) -0.155(9) 0.109(8) -0.078(6) F(4) 0.126(5) 0.077(4) 0.131(5) -0.009(4) 0.068(4) 0.009(3) O(1) 0.102(5) 0.057(4) 0.157(7) -0.002(4) 0.036(5) 0.019(4) O(2) 0.072(4) 0.089(5) 0.122(5) -0.005(3) 0.051(4) 0.005(4) O(3) 0.087(5) 0.069(4) 0.090(4) 0.000(4) 0.019(4) 0.016(3) N(1) 0.053(3) 0.047(3) 0.057(3) 0.006(2) 0.023(3) 0.005(2) C(1) 0.083(6) 0.053(4) 0.082(6) -0.005(4) 0.032(5) 0.002(4) C(01) 0.14(1) 0.103(9) 0.116(9) 0.039(9) 0.034(8) 0.036(7) C(2) 0.071(5) 0.049(4) 0.069(5) 0.007(4) 0.027(4) -0.002(3) C(02) 0.16(2) 0.17(2) 0.25(2) 0.06(1) 0.09(2) 0.13(2) C(03) 0.09(1) 0.28(3) 0.25(2) 0.01(1) 0.02(1) 0.17(2) C(04) 0.088(6) 0.071(5) 0.098(6) -0.056(5) 0.047(5) -0.019(5) C(05) 0.071(6) 0.069(6) 0.112(8) -0.038(5) 0.024(5) -0.052(5) C(06) 0.120(8) 0.084(7) 0.084(6) -0.033(6) 0.054(6) -0.047(5) C(11) 0.050(4) 0.051(4) 0.049(3) -0.003(3) 0.021(3) -0.001(3) C(12) 0.065(4) 0.063(4) 0.056(4) 0.000(3) 0.027(4) -0.003(3) C(13) 0.064(4) 0.067(5) 0.058(4) 0.000(4) 0.022(4) 0.006(3) C(14) 0.067(5) 0.077(5) 0.050(4) -0.014(4) 0.024(4) 0.000(3) C(15) 0.064(4) 0.069(5) 0.050(4) -0.009(4) 0.028(3) -0.010(3) C(16) 0.047(4) 0.060(4) 0.052(4) 0.000(3) 0.022(3) 0.001(3) C(21) 0.050(4) 0.053(4) 0.056(4) 0.000(3) 0.020(3) 0.001(3) C(22) 0.056(4) 0.050(4) 0.093(6) -0.005(3) 0.017(4) -0.005(4) C(23) 0.045(4) 0.074(6) 0.136(9) -0.001(4) 0.026(5) -0.006(6) C(24) 0.078(6) 0.071(6) 0.111(7) -0.025(5) 0.042(6) -0.018(5) C(25) 0.078(6) 0.056(5) 0.091(6) -0.010(4) 0.029(5) 0.001(4) C(26) 0.060(4) 0.049(4) 0.071(5) -0.001(3) 0.022(4) -0.002(3) C(31) 0.053(4) 0.055(4) 0.054(4) -0.001(3) 0.021(3) 0.002(3) C(32) 0.075(6) 0.062(5) 0.062(5) -0.005(4) 0.024(4) 0.008(3) C(33) 0.073(5) 0.062(5) 0.071(5) -0.009(4) 0.025(4) 0.009(4) C(34) 0.078(6) 0.075(6) 0.072(5) -0.001(4) 0.030(5) 0.018(4) C(35) 0.084(6) 0.085(6) 0.051(4) -0.004(5) 0.024(4) 0.003(4) C(36) 0.062(5) 0.074(5) 0.060(4) -0.012(4) 0.024(4) 0.002(3) B(1) 0.091(8) 0.056(5) 0.103(8) -0.015(5) 0.046(7) -0.014(5) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'DIRDIF94 (PATTY)' _computing_structure_refinement SHELXL97 _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir(1) P(1) 2.304(2) . . yes Ir(1) N(1) 2.195(5) . . yes Ir(1) C(1) 2.059(8) . . yes Ir(1) C(2) 1.89(1) . . yes Ir(1) C(04) 2.21(1) . . yes Ir(1) C(05) 2.217(9) . . yes Ir(1) C(06) 2.26(1) . . yes P(1) C(16) 1.806(7) . . yes P(1) C(21) 1.820(7) . . yes P(1) C(31) 1.821(8) . . yes F(1) B(1) 1.40(2) . . yes F(2) B(1) 1.41(2) . . yes F(3) B(1) 1.31(1) . . yes F(4) B(1) 1.34(1) . . yes O(1) C(1) 1.19(1) . . yes O(2) C(2) 1.15(1) . . yes O(3) C(1) 1.34(1) . . yes O(3) C(01) 1.45(1) . . yes N(1) C(11) 1.36(1) . . yes N(1) C(15) 1.341(10) . . yes C(01) C(02) 1.36(3) . . yes C(02) C(03) 1.35(2) . . yes C(04) C(05) 1.40(2) . . yes C(05) C(06) 1.33(2) . . yes C(11) C(12) 1.398(10) . . yes C(11) C(16) 1.497(10) . . yes C(12) C(13) 1.36(1) . . yes C(13) C(14) 1.39(1) . . yes C(14) C(15) 1.34(1) . . yes C(21) C(22) 1.39(1) . . yes C(21) C(26) 1.38(1) . . yes C(22) C(23) 1.37(1) . . yes C(23) C(24) 1.38(1) . . yes C(24) C(25) 1.40(2) . . yes C(25) C(26) 1.37(1) . . yes C(31) C(32) 1.40(1) . . yes C(31) C(36) 1.394(10) . . yes C(32) C(33) 1.33(1) . . yes C(33) C(34) 1.40(1) . . yes C(34) C(35) 1.37(1) . . yes C(35) C(36) 1.40(1) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P(1) Ir(1) N(1) 80.4(2) . . . yes P(1) Ir(1) C(1) 93.5(3) . . . yes P(1) Ir(1) C(2) 98.0(2) . . . yes P(1) Ir(1) C(04) 98.6(3) . . . yes P(1) Ir(1) C(05) 131.4(3) . . . yes P(1) Ir(1) C(06) 164.9(4) . . . yes N(1) Ir(1) C(1) 173.7(3) . . . yes N(1) Ir(1) C(2) 94.5(3) . . . yes N(1) Ir(1) C(04) 91.5(3) . . . yes N(1) Ir(1) C(05) 82.4(3) . . . yes N(1) Ir(1) C(06) 99.2(3) . . . yes C(1) Ir(1) C(2) 87.9(4) . . . yes C(1) Ir(1) C(04) 87.8(4) . . . yes C(1) Ir(1) C(05) 100.7(3) . . . yes C(1) Ir(1) C(06) 86.3(3) . . . yes C(2) Ir(1) C(04) 163.0(4) . . . yes C(2) Ir(1) C(05) 128.5(4) . . . yes C(2) Ir(1) C(06) 97.0(4) . . . yes C(04) Ir(1) C(05) 36.9(4) . . . yes C(04) Ir(1) C(06) 66.3(4) . . . yes C(05) Ir(1) C(06) 34.6(5) . . . yes Ir(1) P(1) C(16) 99.4(2) . . . yes Ir(1) P(1) C(21) 115.8(3) . . . yes Ir(1) P(1) C(31) 120.9(2) . . . yes C(16) P(1) C(21) 106.9(3) . . . yes C(16) P(1) C(31) 105.3(4) . . . yes C(21) P(1) C(31) 106.9(3) . . . yes C(1) O(3) C(01) 116.3(8) . . . yes Ir(1) N(1) C(11) 118.0(4) . . . yes Ir(1) N(1) C(15) 122.6(5) . . . yes C(11) N(1) C(15) 119.3(6) . . . yes Ir(1) C(1) O(1) 127.0(6) . . . yes Ir(1) C(1) O(3) 112.3(6) . . . yes O(1) C(1) O(3) 120.7(8) . . . yes O(3) C(01) C(02) 115(1) . . . yes Ir(1) C(2) O(2) 177.5(7) . . . yes C(01) C(02) C(03) 128(1) . . . yes Ir(1) C(04) C(05) 71.8(6) . . . yes Ir(1) C(05) C(04) 71.3(5) . . . yes Ir(1) C(05) C(06) 74.4(6) . . . yes C(04) C(05) C(06) 126.8(8) . . . yes Ir(1) C(06) C(05) 70.9(6) . . . yes N(1) C(11) C(12) 120.2(6) . . . yes N(1) C(11) C(16) 117.8(6) . . . yes C(12) C(11) C(16) 122.1(7) . . . yes C(11) C(12) C(13) 118.5(8) . . . yes C(12) C(13) C(14) 120.4(7) . . . yes C(13) C(14) C(15) 118.8(7) . . . yes N(1) C(15) C(14) 122.8(8) . . . yes P(1) C(16) C(11) 111.5(6) . . . yes P(1) C(21) C(22) 118.9(6) . . . yes P(1) C(21) C(26) 122.1(6) . . . yes C(22) C(21) C(26) 119.0(7) . . . yes C(21) C(22) C(23) 120.4(8) . . . yes C(22) C(23) C(24) 120.6(8) . . . yes C(23) C(24) C(25) 119.6(9) . . . yes C(24) C(25) C(26) 118.7(8) . . . yes C(21) C(26) C(25) 121.8(8) . . . yes P(1) C(31) C(32) 120.0(5) . . . yes P(1) C(31) C(36) 121.1(6) . . . yes C(32) C(31) C(36) 118.7(8) . . . yes C(31) C(32) C(33) 122.0(8) . . . yes C(32) C(33) C(34) 120.5(9) . . . yes C(33) C(34) C(35) 119(1) . . . yes C(34) C(35) C(36) 120.9(8) . . . yes C(31) C(36) C(35) 118.8(8) . . . yes F(1) B(1) F(2) 98(1) . . . yes F(1) B(1) F(3) 106(1) . . . yes F(1) B(1) F(4) 112.6(10) . . . yes F(2) B(1) F(3) 110(1) . . . yes F(2) B(1) F(4) 107(1) . . . yes F(3) B(1) F(4) 119(1) . . . yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ir(1) P(1) C(16) C(11) 36.6(5) . . . . yes Ir(1) P(1) C(21) C(22) 60.9(7) . . . . yes Ir(1) P(1) C(21) C(26) -117.9(7) . . . . yes Ir(1) P(1) C(31) C(32) 40.1(8) . . . . yes Ir(1) P(1) C(31) C(36) -144.7(6) . . . . yes Ir(1) N(1) C(11) C(12) 178.1(5) . . . . yes Ir(1) N(1) C(11) C(16) -0.8(8) . . . . yes Ir(1) N(1) C(15) C(14) -178.2(6) . . . . yes Ir(1) C(1) O(3) C(01) -171.3(9) . . . . yes Ir(1) C(04) C(05) C(06) -52(1) . . . . yes Ir(1) C(06) C(05) C(04) 51.3(10) . . . . yes P(1) Ir(1) N(1) C(11) 20.0(5) . . . . yes P(1) Ir(1) N(1) C(15) -161.5(6) . . . . yes P(1) Ir(1) C(1) O(1) -128(1) . . . . yes P(1) Ir(1) C(1) O(3) 48.4(8) . . . . yes P(1) Ir(1) C(2) O(2) 173(15) . . . . yes P(1) Ir(1) C(04) C(05) -155.7(5) . . . . yes P(1) Ir(1) C(05) C(04) 32.8(6) . . . . yes P(1) Ir(1) C(05) C(06) 171.5(5) . . . . yes P(1) Ir(1) C(06) C(05) -25(1) . . . . yes P(1) C(16) C(11) N(1) -26.2(8) . . . . yes P(1) C(16) C(11) C(12) 154.9(6) . . . . yes P(1) C(21) C(22) C(23) -179.5(8) . . . . yes P(1) C(21) C(26) C(25) 178.4(8) . . . . yes P(1) C(31) C(32) C(33) 175.8(8) . . . . yes P(1) C(31) C(36) C(35) -177.8(7) . . . . yes O(1) C(1) Ir(1) N(1) -113(2) . . . . yes O(1) C(1) Ir(1) C(2) 133(1) . . . . yes O(1) C(1) Ir(1) C(04) -30(1) . . . . yes O(1) C(1) Ir(1) C(05) 4(1) . . . . yes O(1) C(1) Ir(1) C(06) 36(1) . . . . yes O(1) C(1) O(3) C(01) 5(1) . . . . yes O(2) C(2) Ir(1) N(1) 92(15) . . . . yes O(2) C(2) Ir(1) C(1) -93(15) . . . . yes O(2) C(2) Ir(1) C(04) -18(16) . . . . yes O(2) C(2) Ir(1) C(05) 8(15) . . . . yes O(2) C(2) Ir(1) C(06) -7(15) . . . . yes O(3) C(1) Ir(1) N(1) 63(3) . . . . yes O(3) C(1) Ir(1) C(2) -49.5(8) . . . . yes O(3) C(1) Ir(1) C(04) 146.9(8) . . . . yes O(3) C(1) Ir(1) C(05) -178.3(8) . . . . yes O(3) C(1) Ir(1) C(06) -146.7(9) . . . . yes O(3) C(01) C(02) C(03) -122(2) . . . . yes N(1) Ir(1) P(1) C(16) -27.3(3) . . . . yes N(1) Ir(1) P(1) C(21) 86.7(3) . . . . yes N(1) Ir(1) P(1) C(31) -141.5(3) . . . . yes N(1) Ir(1) C(04) C(05) -75.2(5) . . . . yes N(1) Ir(1) C(05) C(04) 102.8(5) . . . . yes N(1) Ir(1) C(05) C(06) -118.5(6) . . . . yes N(1) Ir(1) C(06) C(05) 62.0(7) . . . . yes N(1) C(11) C(12) C(13) 0(1) . . . . yes N(1) C(15) C(14) C(13) 0(1) . . . . yes C(1) Ir(1) P(1) C(16) 151.0(4) . . . . yes C(1) Ir(1) P(1) C(21) -95.0(4) . . . . yes C(1) Ir(1) P(1) C(31) 36.9(4) . . . . yes C(1) Ir(1) N(1) C(11) 5(3) . . . . yes C(1) Ir(1) N(1) C(15) -176(2) . . . . yes C(1) Ir(1) C(04) C(05) 111.1(6) . . . . yes C(1) Ir(1) C(05) C(04) -71.6(6) . . . . yes C(1) Ir(1) C(05) C(06) 67.1(7) . . . . yes C(1) Ir(1) C(06) C(05) -114.9(7) . . . . yes C(1) O(3) C(01) C(02) -88(1) . . . . yes C(2) Ir(1) P(1) C(16) -120.6(3) . . . . yes C(2) Ir(1) P(1) C(21) -6.6(3) . . . . yes C(2) Ir(1) P(1) C(31) 125.2(4) . . . . yes C(2) Ir(1) N(1) C(11) 117.4(5) . . . . yes C(2) Ir(1) N(1) C(15) -64.1(6) . . . . yes C(2) Ir(1) C(04) C(05) 35(1) . . . . yes C(2) Ir(1) C(05) C(04) -167.4(5) . . . . yes C(2) Ir(1) C(05) C(06) -28.8(8) . . . . yes C(2) Ir(1) C(06) C(05) 157.7(6) . . . . yes C(04) Ir(1) P(1) C(16) 62.8(3) . . . . yes C(04) Ir(1) P(1) C(21) 176.7(3) . . . . yes C(04) Ir(1) P(1) C(31) -51.4(4) . . . . yes C(04) Ir(1) N(1) C(11) -78.4(6) . . . . yes C(04) Ir(1) N(1) C(15) 100.1(6) . . . . yes C(04) Ir(1) C(05) C(06) 138.7(9) . . . . yes C(04) Ir(1) C(06) C(05) -25.7(6) . . . . yes C(04) C(05) Ir(1) C(06) -138.7(9) . . . . yes C(05) Ir(1) P(1) C(16) 43.5(4) . . . . yes C(05) Ir(1) P(1) C(21) 157.5(4) . . . . yes C(05) Ir(1) P(1) C(31) -70.6(4) . . . . yes C(05) Ir(1) N(1) C(11) -114.3(6) . . . . yes C(05) Ir(1) N(1) C(15) 64.2(7) . . . . yes C(05) C(04) Ir(1) C(06) 24.2(5) . . . . yes C(06) Ir(1) P(1) C(16) 62(1) . . . . yes C(06) Ir(1) P(1) C(21) 176.5(10) . . . . yes C(06) Ir(1) P(1) C(31) -51(1) . . . . yes C(06) Ir(1) N(1) C(11) -144.7(6) . . . . yes C(06) Ir(1) N(1) C(15) 33.8(7) . . . . yes C(11) N(1) C(15) C(14) 0(1) . . . . yes C(11) C(12) C(13) C(14) 1(1) . . . . yes C(11) C(16) P(1) C(21) -84.1(5) . . . . yes C(11) C(16) P(1) C(31) 162.4(5) . . . . yes C(12) C(11) N(1) C(15) 0(1) . . . . yes C(12) C(13) C(14) C(15) -2(1) . . . . yes C(13) C(12) C(11) C(16) 178.2(7) . . . . yes C(15) N(1) C(11) C(16) -179.4(7) . . . . yes C(16) P(1) C(21) C(22) 170.5(7) . . . . yes C(16) P(1) C(21) C(26) -8.3(8) . . . . yes C(16) P(1) C(31) C(32) -71.0(8) . . . . yes C(16) P(1) C(31) C(36) 104.2(7) . . . . yes C(21) P(1) C(31) C(32) 175.5(7) . . . . yes C(21) P(1) C(31) C(36) -9.2(8) . . . . yes C(21) C(22) C(23) C(24) 1(1) . . . . yes C(21) C(26) C(25) C(24) 0(1) . . . . yes C(22) C(21) P(1) C(31) -77.2(8) . . . . yes C(22) C(21) C(26) C(25) 0(1) . . . . yes C(22) C(23) C(24) C(25) 0(1) . . . . yes C(23) C(22) C(21) C(26) 0(1) . . . . yes C(23) C(24) C(25) C(26) 0(1) . . . . yes C(26) C(21) P(1) C(31) 104.0(7) . . . . yes C(31) C(32) C(33) C(34) 0(1) . . . . yes C(31) C(36) C(35) C(34) 4(1) . . . . yes C(32) C(31) C(36) C(35) -2(1) . . . . yes C(32) C(33) C(34) C(35) 1(1) . . . . yes C(33) C(32) C(31) C(36) 0(1) . . . . yes C(33) C(34) C(35) C(36) -3(1) . . . . yes C(33) C(34) C(35) C(36) -3(1) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag F(1) C(13) 3.386(9) . 4_554 ? F(1) C(12) 3.41(1) . 6_555 ? F(1) C(26) 3.43(1) . 6_555 ? F(1) O(1) 3.49(1) . 6_545 ? F(1) C(04) 3.53(1) . 6_545 ? F(2) C(12) 3.41(2) . 6_555 ? F(2) C(14) 3.47(1) . 4_554 ? F(3) C(15) 3.17(1) . 7_556 ? F(3) C(26) 3.18(2) . 6_555 ? F(3) C(06) 3.37(1) . 7_556 ? F(4) C(04) 3.42(1) . 6_545 ? O(1) C(25) 3.50(1) . 1_565 ? O(2) C(23) 3.40(1) . 2_555 ? O(2) C(36) 3.56(1) . 4_555 ? O(2) C(03) 3.59(3) . 2_555 ? C(03) C(06) 3.60(2) . 2_555 ? C(04) C(14) 3.44(1) . 7_556 ? C(05) C(13) 3.48(1) . 7_556 ? C(05) C(14) 3.54(1) . 7_556 ? C(06) C(33) 3.52(1) . 4_565 ? #------------------------------------------------------------------------------ #===END #------------------------------------------------------------------------------ data_compound_6_BF4 _database_code_depnum_ccdc_archive 'CCDC 296205' _audit_creation_date 'Wed Aug 24 15:42:06 2005' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C26 H28 B Cl2 F4 Ir N O2 P ' _chemical_formula_moiety 'C26 H28 B Cl2 F4 Ir N O2 P ' _chemical_formula_weight 767.42 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 9.9562(9) _cell_length_b 11.5147(7) _cell_length_c 12.548(1) _cell_angle_alpha 91.706(5) _cell_angle_beta 103.789(3) _cell_angle_gamma 91.982(5) _cell_volume 1395.2(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4260 _cell_measurement_theta_min 3.7 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 213 #------------------------------------------------------------------------------ _exptl_crystal_description unknown _exptl_crystal_colour unknown _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.827 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 5.099 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.450 _exptl_absorpt_correction_T_max 0.601 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_ambient_temperature 213 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 11539 _diffrn_reflns_av_R_equivalents 0.055 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5828 _reflns_number_gt 5644 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1471 _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 5644 _refine_ls_number_parameters 368 _refine_ls_goodness_of_fit_ref 1.210 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_diff_density_max 1.15 _refine_diff_density_min -4.14 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) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 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) ; B B 0.001 0.001 ;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) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ;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 DISPLACEMENT 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.20572(2) 0.88397(1) 0.72050(1) 0.0305(1) Uani 1.00 d . . . Cl(1) Cl 0.2670(5) 0.4364(4) 0.6941(4) 0.118(1) Uani 1.00 d . . . Cl(2) Cl -0.0334(4) 0.4399(2) 0.6535(3) 0.111(1) Uani 1.00 d . . . P(1) P 0.4451(1) 0.8895(1) 0.7627(1) 0.0313(3) Uani 1.00 d . . . F(1) F -0.0245(4) 0.6854(4) 1.0705(4) 0.0564(10) Uani 1.00 d . . . F(2) F -0.1565(5) 0.6426(5) 0.9029(4) 0.072(1) Uani 1.00 d . . . F(3) F -0.1084(6) 0.8315(4) 0.9638(5) 0.077(1) Uani 1.00 d . . . F(4) F -0.2519(4) 0.7161(4) 1.0346(4) 0.065(1) Uani 1.00 d . . . O(1) O 0.1467(5) 1.0996(5) 0.5986(5) 0.058(1) Uani 1.00 d . . . O(3) O 0.1928(5) 0.9557(5) 0.4984(4) 0.054(1) Uani 1.00 d . . . N(1) N 0.2438(6) 0.7517(5) 0.8475(4) 0.0321(10) Uani 1.00 d . . . C(1) C 0.1787(7) 0.9982(6) 0.5979(6) 0.042(1) Uani 1.00 d . . . C(01) C 0.2354(7) 0.8397(7) 0.4923(6) 0.052(2) Uani 1.00 d . . . C(02) C 0.2031(7) 0.7646(6) 0.5818(5) 0.041(1) Uani 1.00 d . . . C(03) C 0.0698(7) 0.7615(5) 0.6004(5) 0.045(1) Uani 1.00 d . . . C(04) C -0.0026(7) 0.9356(7) 0.7441(7) 0.056(2) Uani 1.00 d . . . C(05) C 0.1012(8) 0.9684(6) 0.8374(7) 0.042(2) Uani 0.80 d P . . C(05A) C 0.081(3) 1.028(3) 0.770(3) 0.042(2) Uani 0.20 d P . . C(06) C 0.2190(9) 1.0290(7) 0.8397(7) 0.054(2) Uani 1.00 d . . . C(11) C 0.3715(6) 0.7430(5) 0.9111(4) 0.032(1) Uani 1.00 d . . . C(12) C 0.4056(7) 0.6550(6) 0.9857(5) 0.045(1) Uani 1.00 d . . . C(13) C 0.3029(7) 0.5766(6) 0.9951(5) 0.045(1) Uani 1.00 d . . . C(14) C 0.1692(7) 0.5873(5) 0.9312(6) 0.045(1) Uani 1.00 d . . . C(15) C 0.1438(6) 0.6745(5) 0.8597(5) 0.040(1) Uani 1.00 d . . . C(16) C 0.4792(6) 0.8358(5) 0.9024(5) 0.037(1) Uani 1.00 d . . . C(21) C 0.5346(6) 0.7893(5) 0.6921(5) 0.037(1) Uani 1.00 d . . . C(22) C 0.5302(9) 0.6712(6) 0.7100(7) 0.056(2) Uani 1.00 d . . . C(23) C 0.598(1) 0.5971(8) 0.6541(9) 0.074(2) Uani 1.00 d . . . C(24) C 0.667(1) 0.6356(9) 0.5787(8) 0.061(2) Uani 1.00 d . . . C(25) C 0.6713(8) 0.7512(7) 0.5599(7) 0.055(2) Uani 1.00 d . . . C(26) C 0.6072(6) 0.8305(6) 0.6164(5) 0.042(1) Uani 1.00 d . . . C(31) C 0.5474(5) 1.0245(5) 0.7751(5) 0.035(1) Uani 1.00 d . . . C(32) C 0.4954(6) 1.1220(5) 0.7242(6) 0.048(1) Uani 1.00 d . . . C(33) C 0.5772(8) 1.2245(6) 0.7301(7) 0.058(2) Uani 1.00 d . . . C(34) C 0.7134(7) 1.2279(6) 0.7926(6) 0.050(2) Uani 1.00 d . . . C(35) C 0.7668(8) 1.1294(7) 0.8453(7) 0.047(2) Uani 1.00 d . . . C(36) C 0.6840(6) 1.0266(6) 0.8370(6) 0.041(1) Uani 1.00 d . . . C(41) C 0.120(1) 0.3593(9) 0.708(1) 0.076(3) Uani 1.00 d . . . B(1) B -0.1367(7) 0.7194(6) 0.9909(7) 0.046(2) Uani 1.00 d . . . H(1) H 0.190(8) 0.821(6) 0.407(6) 0.0452(2) Uiso 1.00 d . . . H(2) H 0.333(6) 0.855(5) 0.491(5) 0.0221(2) Uiso 1.00 d . . . H(3) H 0.269(8) 0.701(7) 0.615(7) 0.0458(2) Uiso 1.00 d . . . H(4) H -0.005(6) 0.814(5) 0.551(5) 0.0182(2) Uiso 1.00 d . . . H(5) H 0.089(9) 0.689(8) 0.642(7) 0.0612(3) Uiso 1.00 d . . . H(6) H -0.0487 0.9956 0.7006 0.0674 Uiso 1.00 calc . . . H(7) H -0.0690 0.8758 0.7492 0.0674 Uiso 1.00 calc . . . H(8) H 0.0997 0.9264 0.9021 0.0519 Uiso 1.00 calc . . . H(9) H 0.2114 1.1064 0.8124 0.0645 Uiso 1.00 calc . . . H(10) H 0.2915 1.0310 0.9050 0.0645 Uiso 1.00 calc . . . H(11) H 0.4979 0.6497 1.0282 0.0528 Uiso 1.00 calc . . . H(12) H 0.3229 0.5148 1.0459 0.0544 Uiso 1.00 calc . . . H(13) H 0.0958 0.5347 0.9368 0.0539 Uiso 1.00 calc . . . H(14) H 0.0521 0.6819 0.8158 0.0476 Uiso 1.00 calc . . . H(15) H 0.4791 0.8982 0.9536 0.0454 Uiso 1.00 calc . . . H(16) H 0.5689 0.8027 0.9200 0.0454 Uiso 1.00 calc . . . H(17) H 0.4801 0.6425 0.7610 0.0646 Uiso 1.00 calc . . . H(18) H 0.5940 0.5139 0.6672 0.0854 Uiso 1.00 calc . . . H(19) H 0.7114 0.5832 0.5400 0.0734 Uiso 1.00 calc . . . H(20) H 0.7193 0.7777 0.5085 0.0656 Uiso 1.00 calc . . . H(21) H 0.6127 0.9113 0.6032 0.0497 Uiso 1.00 calc . . . H(22) H 0.4014 1.1198 0.6833 0.0556 Uiso 1.00 calc . . . H(23) H 0.5391 1.2907 0.6917 0.0682 Uiso 1.00 calc . . . H(24) H 0.7681 1.2991 0.8002 0.0589 Uiso 1.00 calc . . . H(25) H 0.8596 1.1314 0.8868 0.0553 Uiso 1.00 calc . . . H(26) H 0.7223 0.9594 0.8743 0.0509 Uiso 1.00 calc . . . H(27) H 0.1262 0.3469 0.7852 0.0909 Uiso 1.00 calc . . . H(28) H 0.1112 0.2858 0.6709 0.0909 Uiso 1.00 calc . . . 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) 0.0276(2) 0.0323(2) 0.0306(2) -0.0043(1) 0.0058(1) 0.0017(1) Cl(1) 0.135(3) 0.109(3) 0.137(3) -0.004(2) 0.086(3) -0.014(2) Cl(2) 0.127(2) 0.063(2) 0.112(2) -0.012(2) -0.030(2) 0.006(1) P(1) 0.0276(6) 0.0298(6) 0.0351(7) -0.0032(5) 0.0049(5) 0.0041(5) F(1) 0.034(2) 0.068(3) 0.063(3) -0.004(2) 0.004(2) 0.008(2) F(2) 0.064(3) 0.089(3) 0.060(3) -0.016(3) 0.013(2) -0.014(2) F(3) 0.088(3) 0.050(2) 0.105(4) 0.004(2) 0.042(3) 0.030(3) F(4) 0.041(2) 0.068(3) 0.092(3) 0.009(2) 0.025(2) 0.023(2) O(1) 0.049(3) 0.046(3) 0.072(3) 0.001(2) -0.002(2) 0.015(2) O(3) 0.054(3) 0.070(3) 0.037(2) -0.004(2) 0.008(2) 0.015(2) N(1) 0.040(3) 0.027(2) 0.031(2) -0.002(2) 0.012(2) 0.005(2) C(1) 0.033(3) 0.042(3) 0.049(4) -0.004(2) 0.002(3) 0.009(3) C(01) 0.046(3) 0.065(4) 0.045(4) -0.001(3) 0.009(3) 0.004(3) C(02) 0.046(3) 0.040(3) 0.031(3) -0.005(3) 0.002(2) -0.015(2) C(03) 0.050(3) 0.030(3) 0.045(3) -0.015(2) -0.005(3) -0.009(2) C(04) 0.032(3) 0.069(5) 0.071(5) 0.013(3) 0.020(3) 0.005(4) C(05) 0.049(4) 0.034(4) 0.052(4) 0.011(3) 0.027(3) -0.007(3) C(05A) 0.049(4) 0.034(4) 0.052(4) 0.011(3) 0.027(3) -0.007(3) C(06) 0.063(4) 0.050(4) 0.047(4) 0.004(3) 0.012(3) -0.025(3) C(11) 0.039(3) 0.033(3) 0.026(2) 0.001(2) 0.009(2) 0.006(2) C(12) 0.050(3) 0.048(4) 0.036(3) 0.001(3) 0.008(2) 0.003(2) C(13) 0.059(4) 0.040(3) 0.040(3) 0.008(3) 0.018(3) 0.012(2) C(14) 0.051(3) 0.040(3) 0.052(4) -0.004(3) 0.025(3) 0.003(3) C(15) 0.037(3) 0.043(3) 0.043(3) -0.008(2) 0.015(2) 0.003(2) C(16) 0.039(3) 0.038(3) 0.033(3) -0.004(2) 0.005(2) 0.006(2) C(21) 0.033(2) 0.040(3) 0.038(3) 0.000(2) 0.010(2) 0.002(2) C(22) 0.070(4) 0.038(3) 0.065(5) -0.002(3) 0.030(4) 0.005(3) C(23) 0.098(7) 0.056(5) 0.081(6) 0.018(4) 0.046(5) 0.011(4) C(24) 0.065(5) 0.066(5) 0.061(5) 0.018(4) 0.029(4) 0.007(4) C(25) 0.044(3) 0.072(5) 0.052(4) 0.007(3) 0.017(3) 0.008(3) C(26) 0.038(3) 0.046(3) 0.046(3) -0.006(2) 0.016(2) 0.010(3) C(31) 0.031(2) 0.035(3) 0.039(3) -0.003(2) 0.008(2) 0.000(2) C(32) 0.035(3) 0.033(3) 0.067(4) -0.007(2) -0.002(3) 0.012(3) C(33) 0.055(4) 0.035(3) 0.079(5) -0.010(3) 0.007(4) 0.012(3) C(34) 0.048(3) 0.048(4) 0.053(4) -0.019(3) 0.016(3) -0.010(3) C(35) 0.040(3) 0.049(4) 0.048(4) -0.013(3) 0.004(3) -0.001(3) C(36) 0.027(2) 0.047(3) 0.047(3) -0.005(2) 0.002(2) 0.004(3) C(41) 0.101(8) 0.042(4) 0.092(8) 0.011(5) 0.034(6) 0.006(4) B(1) 0.039(3) 0.038(4) 0.059(4) 0.002(3) 0.007(3) 0.013(3) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS86 _computing_structure_refinement SHELXL97 _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir(1) P(1) 2.313(1) . . yes Ir(1) N(1) 2.213(5) . . yes Ir(1) C(1) 2.029(8) . . yes Ir(1) C(02) 2.180(7) . . yes Ir(1) C(03) 2.204(6) . . yes Ir(1) C(04) 2.261(7) . . yes Ir(1) C(05) 2.212(9) . . yes Ir(1) C(05A) 2.27(3) . . yes Ir(1) C(06) 2.188(8) . . yes Cl(1) C(41) 1.73(1) . . yes Cl(2) C(41) 1.81(1) . . yes P(1) C(16) 1.834(6) . . yes P(1) C(21) 1.816(7) . . yes P(1) C(31) 1.810(6) . . yes F(1) B(1) 1.387(8) . . yes F(2) B(1) 1.366(10) . . yes F(3) B(1) 1.380(9) . . yes F(4) B(1) 1.384(10) . . yes O(1) C(1) 1.222(9) . . yes O(3) C(1) 1.367(10) . . yes O(3) C(01) 1.421(10) . . yes N(1) C(11) 1.339(7) . . yes N(1) C(15) 1.351(8) . . yes C(01) C(02) 1.52(1) . . yes C(02) C(03) 1.40(1) . . yes C(04) C(05) 1.40(1) . . yes C(04) C(05A) 1.31(3) . . yes C(05) C(05A) 1.09(3) . . yes C(05) C(06) 1.34(1) . . yes C(05A) C(06) 1.44(3) . . yes C(11) C(12) 1.396(9) . . yes C(11) C(16) 1.512(8) . . yes C(12) C(13) 1.37(1) . . yes C(13) C(14) 1.393(9) . . yes C(14) C(15) 1.356(9) . . yes C(21) C(22) 1.385(9) . . yes C(21) C(26) 1.407(10) . . yes C(22) C(23) 1.38(1) . . yes C(23) C(24) 1.38(2) . . yes C(24) C(25) 1.36(1) . . yes C(25) C(26) 1.40(1) . . yes C(31) C(32) 1.365(8) . . yes C(31) C(36) 1.395(7) . . yes C(32) C(33) 1.400(10) . . yes C(33) C(34) 1.39(1) . . yes C(34) C(35) 1.39(1) . . yes C(35) C(36) 1.406(10) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P(1) Ir(1) N(1) 80.5(2) . . . yes P(1) Ir(1) C(1) 97.2(2) . . . yes P(1) Ir(1) C(02) 89.3(2) . . . yes P(1) Ir(1) C(03) 125.2(2) . . . yes P(1) Ir(1) C(04) 154.2(2) . . . yes P(1) Ir(1) C(05) 118.5(2) . . . yes P(1) Ir(1) C(05A) 123.3(8) . . . yes P(1) Ir(1) C(06) 87.9(2) . . . yes N(1) Ir(1) C(1) 175.8(3) . . . yes N(1) Ir(1) C(02) 96.2(2) . . . yes N(1) Ir(1) C(03) 92.0(2) . . . yes N(1) Ir(1) C(04) 96.8(3) . . . yes N(1) Ir(1) C(05) 82.1(3) . . . yes N(1) Ir(1) C(05A) 110.2(9) . . . yes N(1) Ir(1) C(06) 93.8(3) . . . yes C(1) Ir(1) C(02) 80.2(3) . . . yes C(1) Ir(1) C(03) 86.4(2) . . . yes C(1) Ir(1) C(04) 86.8(3) . . . yes C(1) Ir(1) C(05) 102.1(3) . . . yes C(1) Ir(1) C(05A) 74.0(9) . . . yes C(1) Ir(1) C(06) 89.6(3) . . . yes C(02) Ir(1) C(03) 37.3(3) . . . yes C(02) Ir(1) C(04) 116.4(3) . . . yes C(02) Ir(1) C(05) 151.1(3) . . . yes C(02) Ir(1) C(05A) 140.1(8) . . . yes C(02) Ir(1) C(06) 169.1(3) . . . yes C(03) Ir(1) C(04) 80.3(3) . . . yes C(03) Ir(1) C(05) 113.9(3) . . . yes C(03) Ir(1) C(05A) 110.2(8) . . . yes C(03) Ir(1) C(06) 146.8(3) . . . yes C(04) Ir(1) C(05) 36.4(3) . . . yes C(04) Ir(1) C(05A) 33.7(8) . . . yes C(04) Ir(1) C(06) 66.6(3) . . . yes C(05) Ir(1) C(05A) 28.2(9) . . . yes C(05) Ir(1) C(06) 35.4(3) . . . yes C(05A) Ir(1) C(06) 37.7(8) . . . yes Ir(1) P(1) C(16) 99.7(2) . . . yes Ir(1) P(1) C(21) 119.7(2) . . . yes Ir(1) P(1) C(31) 122.3(2) . . . yes C(16) P(1) C(21) 103.2(3) . . . yes C(16) P(1) C(31) 104.9(3) . . . yes C(21) P(1) C(31) 104.1(3) . . . yes C(1) O(3) C(01) 117.6(6) . . . yes Ir(1) N(1) C(11) 119.5(4) . . . yes Ir(1) N(1) C(15) 122.2(4) . . . yes C(11) N(1) C(15) 118.2(5) . . . yes Ir(1) C(1) O(1) 129.3(6) . . . yes Ir(1) C(1) O(3) 116.2(5) . . . yes O(1) C(1) O(3) 114.4(7) . . . yes O(3) C(01) C(02) 113.2(6) . . . yes Ir(1) C(02) C(01) 105.7(4) . . . yes Ir(1) C(02) C(03) 72.3(4) . . . yes C(01) C(02) C(03) 119.8(6) . . . yes Ir(1) C(03) C(02) 70.4(4) . . . yes Ir(1) C(04) C(05) 69.9(5) . . . yes Ir(1) C(04) C(05A) 73(1) . . . yes C(05) C(04) C(05A) 47(1) . . . yes Ir(1) C(05) C(04) 73.7(5) . . . yes Ir(1) C(05) C(05A) 78(1) . . . yes Ir(1) C(05) C(06) 71.3(5) . . . yes C(04) C(05) C(05A) 62(1) . . . yes C(04) C(05) C(06) 126.4(8) . . . yes C(05A) C(05) C(06) 71(1) . . . yes Ir(1) C(05A) C(04) 72(1) . . . yes Ir(1) C(05A) C(05) 73(1) . . . yes Ir(1) C(05A) C(06) 68(1) . . . yes C(04) C(05A) C(05) 70(1) . . . yes C(04) C(05A) C(06) 124(2) . . . yes C(05) C(05A) C(06) 61(1) . . . yes Ir(1) C(06) C(05) 73.3(5) . . . yes Ir(1) C(06) C(05A) 74(1) . . . yes C(05) C(06) C(05A) 46(1) . . . yes N(1) C(11) C(12) 122.5(5) . . . yes N(1) C(11) C(16) 117.3(5) . . . yes C(12) C(11) C(16) 120.1(5) . . . yes C(11) C(12) C(13) 118.1(6) . . . yes C(12) C(13) C(14) 119.4(6) . . . yes C(13) C(14) C(15) 119.2(6) . . . yes N(1) C(15) C(14) 122.5(5) . . . yes P(1) C(16) C(11) 110.6(4) . . . yes P(1) C(21) C(22) 120.7(6) . . . yes P(1) C(21) C(26) 120.3(5) . . . yes C(22) C(21) C(26) 119.0(7) . . . yes C(21) C(22) C(23) 119.5(8) . . . yes C(22) C(23) C(24) 122.3(9) . . . yes C(23) C(24) C(25) 118.7(9) . . . yes C(24) C(25) C(26) 121.2(8) . . . yes C(21) C(26) C(25) 119.3(6) . . . yes P(1) C(31) C(32) 121.9(4) . . . yes P(1) C(31) C(36) 118.2(4) . . . yes C(32) C(31) C(36) 119.9(5) . . . yes C(31) C(32) C(33) 121.5(6) . . . yes C(32) C(33) C(34) 119.1(7) . . . yes C(33) C(34) C(35) 119.8(6) . . . yes C(34) C(35) C(36) 120.4(6) . . . yes C(31) C(36) C(35) 119.4(6) . . . yes Cl(1) C(41) Cl(2) 110.4(6) . . . yes F(1) B(1) F(2) 108.2(6) . . . yes F(1) B(1) F(3) 108.1(5) . . . yes F(1) B(1) F(4) 108.1(6) . . . yes F(2) B(1) F(3) 112.2(7) . . . yes F(2) B(1) F(4) 109.9(6) . . . yes F(3) B(1) F(4) 110.2(6) . . . yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ir(1) P(1) C(16) C(11) 36.6(4) . . . . yes Ir(1) P(1) C(21) C(22) -68.6(5) . . . . yes Ir(1) P(1) C(21) C(26) 110.1(4) . . . . yes Ir(1) P(1) C(31) C(32) -23.9(7) . . . . yes Ir(1) P(1) C(31) C(36) 157.4(4) . . . . yes Ir(1) N(1) C(11) C(12) -174.1(5) . . . . yes Ir(1) N(1) C(11) C(16) 8.1(7) . . . . yes Ir(1) N(1) C(15) C(14) 174.4(5) . . . . yes Ir(1) C(1) O(3) C(01) -4.9(7) . . . . yes Ir(1) C(02) C(01) O(3) -28.4(6) . . . . yes Ir(1) C(03) C(02) C(01) -98.3(6) . . . . yes Ir(1) C(04) C(05) C(05A) 85(2) . . . . yes Ir(1) C(04) C(05) C(06) 50.9(8) . . . . yes Ir(1) C(04) C(05A) C(05) -77(1) . . . . yes Ir(1) C(04) C(05A) C(06) -46(2) . . . . yes Ir(1) C(05) C(04) C(05A) -85(2) . . . . yes Ir(1) C(05) C(05A) C(04) 77(1) . . . . yes Ir(1) C(05) C(05A) C(06) -73.8(8) . . . . yes Ir(1) C(05) C(06) C(05A) 83(1) . . . . yes Ir(1) C(05A) C(04) C(05) 77(1) . . . . yes Ir(1) C(05A) C(05) C(04) -77(1) . . . . yes Ir(1) C(05A) C(05) C(06) 73.8(8) . . . . yes Ir(1) C(05A) C(06) C(05) -81(1) . . . . yes Ir(1) C(06) C(05) C(04) -51.8(8) . . . . yes Ir(1) C(06) C(05) C(05A) -83(1) . . . . yes Ir(1) C(06) C(05A) C(04) 48(2) . . . . yes Ir(1) C(06) C(05A) C(05) 81(1) . . . . yes P(1) Ir(1) N(1) C(11) 13.4(4) . . . . yes P(1) Ir(1) N(1) C(15) -163.1(5) . . . . yes P(1) Ir(1) C(1) O(1) -104.2(6) . . . . yes P(1) Ir(1) C(1) O(3) 78.5(5) . . . . yes P(1) Ir(1) C(02) C(01) -77.6(4) . . . . yes P(1) Ir(1) C(02) C(03) 165.6(4) . . . . yes P(1) Ir(1) C(03) C(02) -17.8(4) . . . . yes P(1) Ir(1) C(04) C(05) -15.6(8) . . . . yes P(1) Ir(1) C(04) C(05A) 34(1) . . . . yes P(1) Ir(1) C(05) C(04) 172.4(4) . . . . yes P(1) Ir(1) C(05) C(05A) 108(1) . . . . yes P(1) Ir(1) C(05) C(06) 33.6(5) . . . . yes P(1) Ir(1) C(05A) C(04) -163.0(8) . . . . yes P(1) Ir(1) C(05A) C(05) -88(1) . . . . yes P(1) Ir(1) C(05A) C(06) -22(1) . . . . yes P(1) Ir(1) C(06) C(05) -150.9(5) . . . . yes P(1) Ir(1) C(06) C(05A) 161(1) . . . . yes P(1) C(16) C(11) N(1) -31.6(7) . . . . yes P(1) C(16) C(11) C(12) 150.5(5) . . . . yes P(1) C(21) C(22) C(23) 179.1(6) . . . . yes P(1) C(21) C(26) C(25) -177.7(5) . . . . yes P(1) C(31) C(32) C(33) -177.0(6) . . . . yes P(1) C(31) C(36) C(35) 178.2(6) . . . . yes O(1) C(1) Ir(1) N(1) -161(2) . . . . yes O(1) C(1) Ir(1) C(02) 167.7(7) . . . . yes O(1) C(1) Ir(1) C(03) 130.7(7) . . . . yes O(1) C(1) Ir(1) C(04) 50.2(6) . . . . yes O(1) C(1) Ir(1) C(05) 17.0(7) . . . . yes O(1) C(1) Ir(1) C(05A) 18.4(10) . . . . yes O(1) C(1) Ir(1) C(06) -16.4(7) . . . . yes O(1) C(1) O(3) C(01) 177.5(6) . . . . yes O(3) C(1) Ir(1) N(1) 21(3) . . . . yes O(3) C(1) Ir(1) C(02) -9.6(5) . . . . yes O(3) C(1) Ir(1) C(03) -46.6(5) . . . . yes O(3) C(1) Ir(1) C(04) -127.0(5) . . . . yes O(3) C(1) Ir(1) C(05) -160.2(5) . . . . yes O(3) C(1) Ir(1) C(05A) -158.8(9) . . . . yes O(3) C(1) Ir(1) C(06) 166.4(5) . . . . yes O(3) C(01) C(02) C(03) 49.9(8) . . . . yes N(1) Ir(1) P(1) C(16) -24.3(2) . . . . yes N(1) Ir(1) P(1) C(21) 87.1(3) . . . . yes N(1) Ir(1) P(1) C(31) -139.0(3) . . . . yes N(1) Ir(1) C(02) C(01) -158.0(4) . . . . yes N(1) Ir(1) C(02) C(03) 85.2(4) . . . . yes N(1) Ir(1) C(03) C(02) -97.6(4) . . . . yes N(1) Ir(1) C(04) C(05) 66.6(5) . . . . yes N(1) Ir(1) C(04) C(05A) 116(1) . . . . yes N(1) Ir(1) C(05) C(04) -113.0(5) . . . . yes N(1) Ir(1) C(05) C(05A) -177(1) . . . . yes N(1) Ir(1) C(05) C(06) 108.2(5) . . . . yes N(1) Ir(1) C(05A) C(04) -71(1) . . . . yes N(1) Ir(1) C(05A) C(05) 2(1) . . . . yes N(1) Ir(1) C(05A) C(06) 68(1) . . . . yes N(1) Ir(1) C(06) C(05) -70.5(5) . . . . yes N(1) Ir(1) C(06) C(05A) -118(1) . . . . yes N(1) C(11) C(12) C(13) -1.4(10) . . . . yes N(1) C(15) C(14) C(13) 0(1) . . . . yes C(1) Ir(1) P(1) C(16) 159.3(3) . . . . yes C(1) Ir(1) P(1) C(21) -89.3(3) . . . . yes C(1) Ir(1) P(1) C(31) 44.6(3) . . . . yes C(1) Ir(1) N(1) C(11) 70(3) . . . . yes C(1) Ir(1) N(1) C(15) -105(3) . . . . yes C(1) Ir(1) C(02) C(01) 19.9(4) . . . . yes C(1) Ir(1) C(02) C(03) -97.0(4) . . . . yes C(1) Ir(1) C(03) C(02) 78.6(4) . . . . yes C(1) Ir(1) C(04) C(05) -115.5(5) . . . . yes C(1) Ir(1) C(04) C(05A) -65(1) . . . . yes C(1) Ir(1) C(05) C(04) 67.1(5) . . . . yes C(1) Ir(1) C(05) C(05A) 2(1) . . . . yes C(1) Ir(1) C(05) C(06) -71.7(5) . . . . yes C(1) Ir(1) C(05A) C(04) 108(1) . . . . yes C(1) Ir(1) C(05A) C(05) -177(1) . . . . yes C(1) Ir(1) C(05A) C(06) -111(1) . . . . yes C(1) Ir(1) C(06) C(05) 111.9(5) . . . . yes C(1) Ir(1) C(06) C(05A) 63(1) . . . . yes C(1) O(3) C(01) C(02) 23.6(8) . . . . yes C(01) C(02) Ir(1) C(03) 116.9(6) . . . . yes C(01) C(02) Ir(1) C(04) 101.3(5) . . . . yes C(01) C(02) Ir(1) C(05) 117.3(6) . . . . yes C(01) C(02) Ir(1) C(05A) 69(1) . . . . yes C(01) C(02) Ir(1) C(06) -2(1) . . . . yes C(02) Ir(1) P(1) C(16) -120.7(3) . . . . yes C(02) Ir(1) P(1) C(21) -9.3(3) . . . . yes C(02) Ir(1) P(1) C(31) 124.7(3) . . . . yes C(02) Ir(1) N(1) C(11) 101.6(5) . . . . yes C(02) Ir(1) N(1) C(15) -74.8(5) . . . . yes C(02) Ir(1) C(04) C(05) 167.0(4) . . . . yes C(02) Ir(1) C(04) C(05A) -143(1) . . . . yes C(02) Ir(1) C(05) C(04) -24.6(8) . . . . yes C(02) Ir(1) C(05) C(05A) -88(1) . . . . yes C(02) Ir(1) C(05) C(06) -163.4(5) . . . . yes C(02) Ir(1) C(05A) C(04) 57(2) . . . . yes C(02) Ir(1) C(05A) C(05) 131(1) . . . . yes C(02) Ir(1) C(05A) C(06) -162.9(6) . . . . yes C(02) Ir(1) C(06) C(05) 133(1) . . . . yes C(02) Ir(1) C(06) C(05A) 85(2) . . . . yes C(02) C(03) Ir(1) C(04) 165.9(4) . . . . yes C(02) C(03) Ir(1) C(05) -179.8(4) . . . . yes C(02) C(03) Ir(1) C(05A) 150(1) . . . . yes C(02) C(03) Ir(1) C(06) 162.3(5) . . . . yes C(03) Ir(1) P(1) C(16) -110.0(3) . . . . yes C(03) Ir(1) P(1) C(21) 1.4(3) . . . . yes C(03) Ir(1) P(1) C(31) 135.3(3) . . . . yes C(03) Ir(1) N(1) C(11) 138.8(5) . . . . yes C(03) Ir(1) N(1) C(15) -37.7(5) . . . . yes C(03) Ir(1) C(04) C(05) 157.5(5) . . . . yes C(03) Ir(1) C(04) C(05A) -152(1) . . . . yes C(03) Ir(1) C(05) C(04) -24.3(5) . . . . yes C(03) Ir(1) C(05) C(05A) -88(1) . . . . yes C(03) Ir(1) C(05) C(06) -163.1(4) . . . . yes C(03) Ir(1) C(05A) C(04) 28(1) . . . . yes C(03) Ir(1) C(05A) C(05) 103(1) . . . . yes C(03) Ir(1) C(05A) C(06) 169.0(9) . . . . yes C(03) Ir(1) C(06) C(05) 29.0(8) . . . . yes C(03) Ir(1) C(06) C(05A) -19(1) . . . . yes C(03) C(02) Ir(1) C(04) -15.6(5) . . . . yes C(03) C(02) Ir(1) C(05) 0.5(7) . . . . yes C(03) C(02) Ir(1) C(05A) -46(1) . . . . yes C(03) C(02) Ir(1) C(06) -118(1) . . . . yes C(04) Ir(1) P(1) C(16) 61.7(5) . . . . yes C(04) Ir(1) P(1) C(21) 173.1(5) . . . . yes C(04) Ir(1) P(1) C(31) -53.0(6) . . . . yes C(04) Ir(1) N(1) C(11) -140.8(5) . . . . yes C(04) Ir(1) N(1) C(15) 42.8(5) . . . . yes C(04) Ir(1) C(05) C(05A) -64(1) . . . . yes C(04) Ir(1) C(05) C(06) -138.8(7) . . . . yes C(04) Ir(1) C(05A) C(05) 74(1) . . . . yes C(04) Ir(1) C(05A) C(06) 140(2) . . . . yes C(04) Ir(1) C(06) C(05) 25.2(5) . . . . yes C(04) Ir(1) C(06) C(05A) -22(1) . . . . yes C(04) C(05) Ir(1) C(05A) 64(1) . . . . yes C(04) C(05) Ir(1) C(06) 138.8(7) . . . . yes C(04) C(05) C(05A) C(06) -151(1) . . . . yes C(04) C(05) C(06) C(05A) 32(2) . . . . yes C(04) C(05A) Ir(1) C(05) -74(1) . . . . yes C(04) C(05A) Ir(1) C(06) -140(2) . . . . yes C(04) C(05A) C(05) C(06) 151(1) . . . . yes C(04) C(05A) C(06) C(05) -33(2) . . . . yes C(05) Ir(1) P(1) C(16) 51.2(3) . . . . yes C(05) Ir(1) P(1) C(21) 162.6(3) . . . . yes C(05) Ir(1) P(1) C(31) -63.4(3) . . . . yes C(05) Ir(1) N(1) C(11) -107.4(5) . . . . yes C(05) Ir(1) N(1) C(15) 76.1(5) . . . . yes C(05) Ir(1) C(04) C(05A) 49(1) . . . . yes C(05) Ir(1) C(05A) C(06) 65(1) . . . . yes C(05) Ir(1) C(06) C(05A) -48(1) . . . . yes C(05) C(04) Ir(1) C(05A) -49(1) . . . . yes C(05) C(04) Ir(1) C(06) -24.6(5) . . . . yes C(05) C(04) C(05A) C(06) 31(1) . . . . yes C(05) C(05A) Ir(1) C(06) -65(1) . . . . yes C(05) C(06) Ir(1) C(05A) 48(1) . . . . yes C(05A) Ir(1) P(1) C(16) 83(1) . . . . yes C(05A) Ir(1) P(1) C(21) -164(1) . . . . yes C(05A) Ir(1) P(1) C(31) -30(1) . . . . yes C(05A) Ir(1) N(1) C(11) -108.8(9) . . . . yes C(05A) Ir(1) N(1) C(15) 74.7(9) . . . . yes C(05A) Ir(1) C(05) C(06) -74(1) . . . . yes C(05A) C(04) Ir(1) C(06) 25(1) . . . . yes C(05A) C(04) C(05) C(06) -34(2) . . . . yes C(05A) C(05) Ir(1) C(06) 74(1) . . . . yes C(06) Ir(1) P(1) C(16) 69.9(3) . . . . yes C(06) Ir(1) P(1) C(21) -178.7(3) . . . . yes C(06) Ir(1) P(1) C(31) -44.7(3) . . . . yes C(06) Ir(1) N(1) C(11) -73.9(5) . . . . yes C(06) Ir(1) N(1) C(15) 109.6(6) . . . . yes C(11) N(1) C(15) C(14) -2.1(10) . . . . yes C(11) C(12) C(13) C(14) 0(1) . . . . yes C(11) C(16) P(1) C(21) -87.3(5) . . . . yes C(11) C(16) P(1) C(31) 163.9(4) . . . . yes C(12) C(11) N(1) C(15) 2.6(9) . . . . yes C(12) C(13) C(14) C(15) 0(1) . . . . yes C(13) C(12) C(11) C(16) 176.5(6) . . . . yes C(15) N(1) C(11) C(16) -175.3(6) . . . . yes C(16) P(1) C(21) C(22) 40.9(6) . . . . yes C(16) P(1) C(21) C(26) -140.4(4) . . . . yes C(16) P(1) C(31) C(32) -135.9(6) . . . . yes C(16) P(1) C(31) C(36) 45.4(6) . . . . yes C(21) P(1) C(31) C(32) 115.9(6) . . . . yes C(21) P(1) C(31) C(36) -62.7(6) . . . . yes C(21) C(22) C(23) C(24) -1(1) . . . . yes C(21) C(26) C(25) C(24) -1.6(10) . . . . yes C(22) C(21) P(1) C(31) 150.3(5) . . . . yes C(22) C(21) C(26) C(25) 1.0(9) . . . . yes C(22) C(23) C(24) C(25) 0(1) . . . . yes C(23) C(22) C(21) C(26) 0(1) . . . . yes C(23) C(24) C(25) C(26) 0(1) . . . . yes C(26) C(21) P(1) C(31) -31.0(5) . . . . yes C(31) C(32) C(33) C(34) -2(1) . . . . yes C(31) C(36) C(35) C(34) 0(1) . . . . yes C(32) C(31) C(36) C(35) 0(1) . . . . yes C(32) C(33) C(34) C(35) 1(1) . . . . yes C(33) C(32) C(31) C(36) 1(1) . . . . yes C(33) C(34) C(35) C(36) 0(1) . . . . yes C(33) C(34) C(35) C(36) 0(1) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag F(1) C(41) 3.19(2) . 2_567 ? F(1) C(35) 3.231(8) . 2_677 ? F(1) C(34) 3.269(8) . 2_677 ? F(1) C(14) 3.407(8) . 2_567 ? F(2) C(13) 3.310(9) . 2_567 ? F(2) C(14) 3.433(9) . 2_567 ? F(2) C(23) 3.49(1) . 1_455 ? F(2) C(22) 3.495(9) . 1_455 ? F(3) C(36) 3.289(8) . 1_455 ? F(3) C(06) 3.33(1) . 2_577 ? F(3) C(05) 3.332(10) . 2_577 ? F(4) C(16) 3.178(7) . 1_455 ? F(4) C(06) 3.260(9) . 2_577 ? F(4) C(41) 3.34(1) . 2_567 ? F(4) C(12) 3.364(8) . 1_455 ? F(4) C(13) 3.386(8) . 2_567 ? O(1) C(41) 3.30(1) . 1_565 ? O(1) O(3) 3.341(7) . 2_576 ? O(1) C(03) 3.369(8) . 2_576 ? O(1) C(25) 3.45(1) . 2_676 ? O(3) C(04) 3.472(9) . 2_576 ? C(12) C(34) 3.52(1) . 2_677 ? C(13) C(34) 3.47(1) . 2_677 ? #------------------------------------------------------------------------------ #===END