# Electronic Supplementary Material (ESI) for Catalysis Science & Technology. # This journal is © The Royal Society of Chemistry 2020 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_sbd1905 _database_code_depnum_ccdc_archive 'CCDC 1957542' loop_ _audit_author_name _audit_author_address 'Adrian C. Whitwood' ;University of York United Kingdom ; _audit_update_record ; 2019-10-04 deposited with the CCDC. 2019-12-10 downloaded from the CCDC. ; _audit_creation_date 2019-09-17 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C54 H48 Ir P3, 0.28(C H4 O)' _chemical_formula_sum 'C54.28 H49.13 Ir O0.28 P3' _chemical_formula_weight 991.09 _chemical_melting_point ? _chemical_oxdiff_formula 'C54.3 H49.1 Ir1 O0.3 P3' _chemical_oxdiff_usercomment 'Ben Tickner PPh3' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -4.7710 6.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.31801(12) _cell_length_b 12.99024(10) _cell_length_c 19.71788(16) _cell_angle_alpha 90 _cell_angle_beta 94.4442(7) _cell_angle_gamma 90 _cell_volume 4422.50(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9261 _cell_measurement_temperature 110.00(10) _cell_measurement_theta_max 71.0080 _cell_measurement_theta_min 4.9940 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 7.149 _exptl_absorpt_correction_T_max 0.898 _exptl_absorpt_correction_T_min 0.375 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier . _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 1996.4 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 1 0.0390 0 0 -1 0.0213 0 0 1 0.0161 -1 0 0 0.0447 2 -1 0 0.0635 1 2 -2 0.0643 -2 2 1 0.0763 -1 -2 0 0.0968 1 0 0 0.0543 -2 1 -2 0.0462 1 0 -2 0.0364 -2 -1 1 0.0670 _exptl_crystal_recrystallization_method 'crystallisation from methanol' _exptl_crystal_size_max 0.197 _exptl_crystal_size_mid 0.099 _exptl_crystal_size_min 0.037 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0.9989 -0.0007 0.9977 0.1098 0.0267 0.0488 0.0006 -0.0000 -0.9992 -0.0722 -0.0069 0.0296 -0.0006 0.0000 0.9992 0.0722 0.0069 -0.0296 -0.9995 0.0007 0.0015 -0.0377 -0.0198 -0.0784 1.9977 -1.0018 -0.0047 0.0561 0.1550 0.1368 1.0030 2.0001 -1.9964 -0.0682 -0.2245 0.1775 -1.9971 2.0023 1.0056 0.0353 -0.2634 -0.1465 -1.0019 -2.0001 -0.0020 -0.0761 0.2108 -0.1183 0.9995 -0.0007 -0.0015 0.0377 0.0198 0.0784 -1.9966 1.0018 -1.9937 -0.2004 -0.1687 -0.0776 1.0006 -0.0007 -1.9999 -0.1066 0.0061 0.1376 -2.0007 -0.9990 1.0004 -0.0224 0.0825 -0.2064 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_unetI/netI 0.0296 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 17542 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 67.076 _diffrn_reflns_theta_max 67.076 _diffrn_reflns_theta_min 4.079 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 110.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1450 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 1.00 26.00 1.00 1.00 -- 0.00 57.00 150.00 25 2 \w -10.00 27.00 1.00 1.00 -- 0.00 93.00 61.00 37 3 \w -39.00 -13.00 1.00 1.00 -- 0.00 93.00 61.00 26 4 \w -21.00 45.00 1.00 1.00 -- 0.00 57.00-180.00 66 5 \w 24.00 109.00 1.00 1.25 -- 54.00-125.00 -90.00 85 6 \w 28.00 114.00 1.00 1.25 -- 54.00 37.00 -30.00 86 7 \w 50.00 100.00 1.00 1.25 -- 54.00 57.00-180.00 50 8 \w -13.00 73.00 1.00 1.25 -- 54.00 -57.00 0.00 86 9 \w 106.00 176.00 1.00 2.50 -- 108.00 111.00 150.00 70 10 \w 47.00 100.00 1.00 2.50 -- 108.00-111.00 -60.00 53 11 \w 55.00 103.00 1.00 2.50 -- 108.00 -50.00-120.00 48 12 \w 39.00 111.00 1.00 2.50 -- 108.00-111.00 90.00 72 13 \w 69.00 125.00 1.00 2.50 -- 108.00 -50.00 150.00 56 14 \w 95.00 162.00 1.00 2.50 -- 108.00 63.00 -30.00 67 15 \w 84.00 150.00 1.00 2.50 -- 108.00 178.00 -60.00 66 16 \w 86.00 163.00 1.00 2.50 -- 108.00 50.00 -60.00 77 17 \w 70.00 95.00 1.00 2.50 -- 108.00-111.00-120.00 25 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0378139000 _diffrn_orient_matrix_UB_12 0.0190542000 _diffrn_orient_matrix_UB_13 0.0722370000 _diffrn_orient_matrix_UB_21 0.0197567000 _diffrn_orient_matrix_UB_22 -0.1153091000 _diffrn_orient_matrix_UB_23 0.0068760000 _diffrn_orient_matrix_UB_31 0.0784119000 _diffrn_orient_matrix_UB_32 0.0199077000 _diffrn_orient_matrix_UB_33 -0.0295763000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 7174 _reflns_number_total 7896 _reflns_odcompleteness_completeness 99.95 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.714 _refine_diff_density_min -0.525 _refine_diff_density_rms 0.073 _refine_ls_extinction_coef 0.000059(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 557 _refine_ls_number_reflns 7896 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0237 _refine_ls_R_factor_gt 0.0199 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+0.6768P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.0480 _refine_special_details 'The asymmetric unit contained a partial methanol whose occupancy refined to be 0.283(5)' _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2. Others Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=Sof(O1)=Sof(H1)=FVAR(1) 3.a Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54) 3.b Idealised Me refined as rotating group: C55(H55A,H55B,H55C) 3.c Idealised tetrahedral OH refined as rotating group: O1(H1) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.64948(12) 0.96767(18) 0.67458(12) 0.0129(5) Uani 1 1 d . . . . . C2 C 0.68615(14) 1.0340(2) 0.63166(13) 0.0186(5) Uani 1 1 d . . . . . H2 H 0.701960 1.009582 0.590599 0.022 Uiso 1 1 calc R . . . . C3 C 0.69931(16) 1.1368(2) 0.64993(14) 0.0249(6) Uani 1 1 d . . . . . H3 H 0.724145 1.180207 0.621083 0.030 Uiso 1 1 calc R . . . . C4 C 0.67559(16) 1.1746(2) 0.71082(14) 0.0248(6) Uani 1 1 d . . . . . H4 H 0.685333 1.242681 0.723272 0.030 Uiso 1 1 calc R . . . . C5 C 0.63723(14) 1.1098(2) 0.75288(13) 0.0214(6) Uani 1 1 d . . . . . H5 H 0.620345 1.134781 0.793382 0.026 Uiso 1 1 calc R . . . . C6 C 0.62393(13) 1.0075(2) 0.73467(13) 0.0175(5) Uani 1 1 d . . . . . H6 H 0.597591 0.964931 0.762988 0.021 Uiso 1 1 calc R . . . . C7 C 0.52819(13) 0.84914(19) 0.61556(13) 0.0152(5) Uani 1 1 d . . . . . C8 C 0.50890(14) 0.8537(2) 0.54587(14) 0.0227(6) Uani 1 1 d . . . . . H8 H 0.546993 0.843354 0.515821 0.027 Uiso 1 1 calc R . . . . C9 C 0.43291(16) 0.8738(2) 0.52059(15) 0.0313(7) Uani 1 1 d . . . . . H9 H 0.420719 0.876647 0.473858 0.038 Uiso 1 1 calc R . . . . C10 C 0.37556(15) 0.8895(2) 0.56460(16) 0.0278(6) Uani 1 1 d . . . . . H10 H 0.324839 0.902083 0.547635 0.033 Uiso 1 1 calc R . . . . C11 C 0.39432(14) 0.8862(2) 0.63414(15) 0.0239(6) Uani 1 1 d . . . . . H11 H 0.356053 0.896845 0.663979 0.029 Uiso 1 1 calc R . . . . C12 C 0.47008(14) 0.8672(2) 0.65951(13) 0.0188(5) Uani 1 1 d . . . . . H12 H 0.482275 0.866547 0.706276 0.023 Uiso 1 1 calc R . . . . C13 C 0.62356(13) 0.76881(18) 0.73028(12) 0.0118(5) Uani 1 1 d . . . . . C14 C 0.68051(13) 0.78807(19) 0.78309(12) 0.0138(5) Uani 1 1 d . . . . . H14 H 0.719416 0.835680 0.776788 0.017 Uiso 1 1 calc R . . . . C15 C 0.67944(14) 0.73669(19) 0.84489(13) 0.0161(5) Uani 1 1 d . . . . . H15 H 0.717559 0.750292 0.879574 0.019 Uiso 1 1 calc R . . . . C16 C 0.62194(14) 0.6653(2) 0.85518(13) 0.0180(5) Uani 1 1 d . . . . . H16 H 0.620879 0.631884 0.896812 0.022 Uiso 1 1 calc R . . . . C17 C 0.56593(14) 0.64412(19) 0.80271(13) 0.0180(5) Uani 1 1 d . . . . . H17 H 0.527686 0.595598 0.809102 0.022 Uiso 1 1 calc R . . . . C18 C 0.56668(13) 0.69500(19) 0.74069(12) 0.0145(5) Uani 1 1 d . . . . . H18 H 0.529100 0.679904 0.705834 0.017 Uiso 1 1 calc R . . . . C19 C 0.62083(13) 0.53220(19) 0.61399(12) 0.0129(5) Uani 1 1 d . . . . . C20 C 0.55342(13) 0.57646(19) 0.58388(12) 0.0156(5) Uani 1 1 d . . . . . H20 H 0.555714 0.640549 0.563109 0.019 Uiso 1 1 calc R . . . . C21 C 0.48256(14) 0.5258(2) 0.58451(13) 0.0203(5) Uani 1 1 d . . . . . H21 H 0.437873 0.556350 0.564481 0.024 Uiso 1 1 calc R . . . . C22 C 0.47857(14) 0.4306(2) 0.61471(13) 0.0226(6) Uani 1 1 d . . . . . H22 H 0.431335 0.396584 0.614679 0.027 Uiso 1 1 calc R . . . . C23 C 0.54525(15) 0.3855(2) 0.64526(14) 0.0237(6) Uani 1 1 d . . . . . H23 H 0.542581 0.321233 0.665711 0.028 Uiso 1 1 calc R . . . . C24 C 0.61586(14) 0.4362(2) 0.64531(13) 0.0183(5) Uani 1 1 d . . . . . H24 H 0.660167 0.406091 0.666355 0.022 Uiso 1 1 calc R . . . . C25 C 0.73896(13) 0.50026(19) 0.53287(12) 0.0145(5) Uani 1 1 d . . . . . C26 C 0.75924(14) 0.3981(2) 0.54723(14) 0.0209(5) Uani 1 1 d . . . . . H26 H 0.770773 0.377731 0.592092 0.025 Uiso 1 1 calc R . . . . C27 C 0.76238(15) 0.3263(2) 0.49505(15) 0.0258(6) Uani 1 1 d . . . . . H27 H 0.776221 0.258524 0.505146 0.031 Uiso 1 1 calc R . . . . C28 C 0.74487(14) 0.3558(2) 0.42807(14) 0.0234(6) Uani 1 1 d . . . . . H28 H 0.745917 0.307726 0.393223 0.028 Uiso 1 1 calc R . . . . C29 C 0.72586(14) 0.4571(2) 0.41334(14) 0.0214(6) Uani 1 1 d . . . . . H29 H 0.714791 0.477324 0.368402 0.026 Uiso 1 1 calc R . . . . C30 C 0.72319(13) 0.5291(2) 0.46563(12) 0.0164(5) Uani 1 1 d . . . . . H30 H 0.710694 0.597233 0.455189 0.020 Uiso 1 1 calc R . . . . C31 C 0.77749(13) 0.54635(18) 0.67382(12) 0.0135(5) Uani 1 1 d . . . . . C32 C 0.75073(14) 0.54883(19) 0.73871(13) 0.0166(5) Uani 1 1 d . . . . . H32 H 0.700025 0.569030 0.743967 0.020 Uiso 1 1 calc R . . . . C33 C 0.79861(15) 0.5216(2) 0.79553(13) 0.0219(6) Uani 1 1 d . . . . . H33 H 0.779804 0.523812 0.838424 0.026 Uiso 1 1 calc R . . . . C34 C 0.87465(15) 0.4911(2) 0.78871(14) 0.0279(6) Uani 1 1 d . . . . . H34 H 0.906512 0.471766 0.826723 0.033 Uiso 1 1 calc R . . . . C35 C 0.90248(14) 0.4897(2) 0.72434(15) 0.0270(6) Uani 1 1 d . . . . . H35 H 0.953466 0.470440 0.719457 0.032 Uiso 1 1 calc R . . . . C36 C 0.85467(14) 0.5170(2) 0.66732(13) 0.0186(5) Uani 1 1 d . . . . . H36 H 0.873881 0.515880 0.624576 0.022 Uiso 1 1 calc R . . . . C37 C 0.86844(13) 0.94240(19) 0.57312(12) 0.0142(5) Uani 1 1 d . . . . . C38 C 0.83560(13) 0.97721(19) 0.51076(13) 0.0154(5) Uani 1 1 d . . . . . H38 H 0.793133 0.942725 0.489825 0.019 Uiso 1 1 calc R . . . . C39 C 0.86507(14) 1.0625(2) 0.47920(13) 0.0201(5) Uani 1 1 d . . . . . H39 H 0.842037 1.084807 0.437613 0.024 Uiso 1 1 calc R . . . . C40 C 0.92861(15) 1.1146(2) 0.50925(14) 0.0228(6) Uani 1 1 d . . . . . H40 H 0.948107 1.172142 0.488260 0.027 Uiso 1 1 calc R . . . . C41 C 0.96284(15) 1.0800(2) 0.57114(15) 0.0258(6) Uani 1 1 d . . . . . H41 H 1.005805 1.114085 0.591502 0.031 Uiso 1 1 calc R . . . . C42 C 0.93339(14) 0.9950(2) 0.60261(13) 0.0199(5) Uani 1 1 d . . . . . H42 H 0.956963 0.972434 0.643926 0.024 Uiso 1 1 calc R . . . . C43 C 0.91808(13) 0.74267(18) 0.59649(13) 0.0136(5) Uani 1 1 d . . . . . C44 C 0.98739(14) 0.74623(19) 0.63811(13) 0.0175(5) Uani 1 1 d . . . . . H44 H 0.990602 0.786942 0.677022 0.021 Uiso 1 1 calc R . . . . C45 C 1.05130(14) 0.6895(2) 0.62175(14) 0.0210(5) Uani 1 1 d . . . . . H45 H 1.096722 0.691587 0.650154 0.025 Uiso 1 1 calc R . . . . C46 C 1.04782(14) 0.6299(2) 0.56347(14) 0.0196(5) Uani 1 1 d . . . . . H46 H 1.090692 0.591893 0.552686 0.024 Uiso 1 1 calc R . . . . C47 C 0.98000(14) 0.6272(2) 0.52121(13) 0.0191(5) Uani 1 1 d . . . . . H47 H 0.977592 0.588024 0.481645 0.023 Uiso 1 1 calc R . . . . C48 C 0.91540(13) 0.68320(19) 0.53787(13) 0.0165(5) Uani 1 1 d . . . . . H48 H 0.870039 0.680635 0.509400 0.020 Uiso 1 1 calc R . . . . C49 C 0.85208(12) 0.85135(19) 0.70372(12) 0.0131(5) Uani 1 1 d . . . . . C50 C 0.86903(13) 0.7709(2) 0.74953(13) 0.0180(5) Uani 1 1 d . . . . . H50 H 0.874499 0.704353 0.733160 0.022 Uiso 1 1 calc R . . . . C51 C 0.87782(14) 0.7888(2) 0.81900(14) 0.0236(6) Uani 1 1 d . . . . . H51 H 0.889674 0.734493 0.848716 0.028 Uiso 1 1 calc R . . . . C52 C 0.86907(15) 0.8871(2) 0.84440(13) 0.0271(6) Uani 1 1 d . . . . . H52 H 0.875024 0.899016 0.891011 0.032 Uiso 1 1 calc R . . . . C53 C 0.85133(14) 0.9676(2) 0.79962(14) 0.0233(6) Uani 1 1 d . . . . . H53 H 0.844872 1.033717 0.816363 0.028 Uiso 1 1 calc R . . . . C54 C 0.84317(13) 0.9500(2) 0.73000(13) 0.0176(5) Uani 1 1 d . . . . . H54 H 0.831612 1.004696 0.700487 0.021 Uiso 1 1 calc R . . . . Ir1 Ir 0.71281(2) 0.76500(2) 0.57051(2) 0.00947(4) Uani 1 1 d . . . . . H H 0.6956(16) 0.868(2) 0.5325(15) 0.031(9) Uiso 1 1 d . . . . . HA H 0.7593(17) 0.743(2) 0.5079(15) 0.024(8) Uiso 1 1 d . . . . . HB H 0.6422(16) 0.733(2) 0.5222(15) 0.019(8) Uiso 1 1 d . . . . . P1 P 0.63074(3) 0.83272(5) 0.64784(3) 0.01082(11) Uani 1 1 d . . . . . P2 P 0.71553(3) 0.59173(5) 0.60036(3) 0.01056(11) Uani 1 1 d . . . . . P3 P 0.83357(3) 0.82402(5) 0.61283(3) 0.01083(12) Uani 1 1 d . . . . . C55 C 0.8930(7) 1.2368(9) 0.6889(7) 0.041(3) Uani 0.283(5) 1 d . . P . . H55A H 0.869970 1.240671 0.643063 0.062 Uiso 0.283(5) 1 calc GR . P . . H55B H 0.906489 1.166736 0.699640 0.062 Uiso 0.283(5) 1 calc GR . P . . H55C H 0.938713 1.278797 0.693202 0.062 Uiso 0.283(5) 1 calc GR . P . . O1 O 0.8391(5) 1.2730(7) 0.7345(6) 0.052(3) Uani 0.283(5) 1 d . . P . . H1 H 0.795713 1.275687 0.714726 0.078 Uiso 0.283(5) 1 calc GR . P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0090(10) 0.0119(12) 0.0171(12) 0.0009(10) -0.0028(9) 0.0025(9) C2 0.0196(12) 0.0164(13) 0.0191(12) 0.0015(10) -0.0027(10) 0.0016(10) C3 0.0338(15) 0.0136(13) 0.0271(14) 0.0067(11) -0.0002(12) -0.0029(11) C4 0.0317(14) 0.0109(13) 0.0297(15) -0.0008(11) -0.0105(12) 0.0040(11) C5 0.0217(12) 0.0206(14) 0.0207(13) -0.0033(11) -0.0062(10) 0.0081(11) C6 0.0154(11) 0.0173(13) 0.0192(12) 0.0020(10) -0.0022(9) 0.0031(10) C7 0.0113(11) 0.0113(12) 0.0224(13) 0.0017(10) -0.0022(9) 0.0012(9) C8 0.0161(12) 0.0282(15) 0.0229(14) 0.0017(12) -0.0044(10) 0.0039(11) C9 0.0218(14) 0.0419(19) 0.0280(15) 0.0015(14) -0.0108(12) 0.0071(13) C10 0.0128(12) 0.0240(15) 0.0450(17) -0.0009(13) -0.0087(11) 0.0033(11) C11 0.0121(12) 0.0195(14) 0.0404(16) -0.0015(12) 0.0038(11) 0.0005(10) C12 0.0154(12) 0.0173(13) 0.0233(13) -0.0001(11) -0.0008(10) 0.0022(10) C13 0.0106(10) 0.0127(12) 0.0124(11) -0.0006(9) 0.0029(9) 0.0020(9) C14 0.0126(11) 0.0126(12) 0.0163(12) 0.0012(10) 0.0014(9) 0.0018(9) C15 0.0182(12) 0.0157(12) 0.0140(12) -0.0018(10) -0.0022(9) 0.0049(10) C16 0.0230(12) 0.0162(13) 0.0156(12) 0.0042(10) 0.0063(10) 0.0058(10) C17 0.0170(12) 0.0144(12) 0.0231(13) 0.0010(10) 0.0056(10) -0.0008(10) C18 0.0121(11) 0.0133(12) 0.0183(12) -0.0003(10) 0.0010(9) 0.0002(9) C19 0.0129(11) 0.0126(12) 0.0134(11) -0.0012(9) 0.0029(9) -0.0031(9) C20 0.0167(11) 0.0129(12) 0.0175(12) -0.0023(10) 0.0023(9) -0.0019(10) C21 0.0126(11) 0.0257(14) 0.0227(13) -0.0025(11) 0.0012(10) -0.0021(10) C22 0.0167(12) 0.0276(15) 0.0246(14) -0.0039(12) 0.0076(10) -0.0106(11) C23 0.0283(14) 0.0178(14) 0.0260(14) 0.0034(11) 0.0082(11) -0.0075(11) C24 0.0176(12) 0.0172(13) 0.0204(13) 0.0035(11) 0.0039(10) -0.0007(10) C25 0.0105(10) 0.0140(12) 0.0195(12) -0.0024(10) 0.0049(9) -0.0024(9) C26 0.0231(13) 0.0182(13) 0.0222(13) 0.0006(11) 0.0074(10) 0.0019(10) C27 0.0262(14) 0.0163(14) 0.0364(16) -0.0034(12) 0.0115(12) 0.0017(11) C28 0.0177(12) 0.0253(15) 0.0282(14) -0.0115(12) 0.0077(10) -0.0037(11) C29 0.0142(11) 0.0292(15) 0.0208(13) -0.0060(11) 0.0021(10) -0.0060(11) C30 0.0118(11) 0.0179(13) 0.0193(12) -0.0016(10) 0.0009(9) -0.0025(9) C31 0.0126(11) 0.0104(11) 0.0172(12) 0.0024(10) -0.0009(9) -0.0002(9) C32 0.0150(11) 0.0151(12) 0.0197(13) 0.0031(10) 0.0012(10) 0.0019(9) C33 0.0220(13) 0.0266(15) 0.0172(13) 0.0045(11) 0.0013(10) 0.0028(11) C34 0.0214(13) 0.0392(17) 0.0222(14) 0.0115(13) -0.0032(11) 0.0072(12) C35 0.0130(12) 0.0364(17) 0.0318(15) 0.0095(13) 0.0025(11) 0.0091(12) C36 0.0167(12) 0.0194(13) 0.0201(13) 0.0042(11) 0.0038(10) 0.0051(10) C37 0.0114(11) 0.0117(12) 0.0202(12) 0.0000(10) 0.0050(9) -0.0002(9) C38 0.0124(11) 0.0141(12) 0.0200(12) -0.0002(10) 0.0025(9) -0.0010(9) C39 0.0218(12) 0.0208(13) 0.0182(13) 0.0036(11) 0.0040(10) 0.0000(11) C40 0.0241(13) 0.0159(13) 0.0296(14) 0.0044(11) 0.0092(11) -0.0056(11) C41 0.0179(12) 0.0229(15) 0.0361(16) 0.0007(12) -0.0012(11) -0.0087(11) C42 0.0159(11) 0.0203(14) 0.0231(13) 0.0056(11) -0.0014(10) -0.0029(10) C43 0.0114(11) 0.0108(11) 0.0188(12) 0.0033(10) 0.0028(9) -0.0003(9) C44 0.0154(12) 0.0176(13) 0.0192(13) -0.0014(10) 0.0003(10) -0.0008(10) C45 0.0137(11) 0.0226(14) 0.0257(14) 0.0043(11) -0.0043(10) 0.0023(10) C46 0.0130(11) 0.0140(13) 0.0321(14) 0.0030(11) 0.0037(10) 0.0032(10) C47 0.0189(12) 0.0149(13) 0.0237(13) -0.0007(11) 0.0024(10) 0.0002(10) C48 0.0136(11) 0.0134(12) 0.0223(13) 0.0008(10) 0.0009(9) -0.0015(10) C49 0.0063(10) 0.0193(13) 0.0133(11) 0.0002(10) -0.0015(8) -0.0017(9) C50 0.0122(11) 0.0218(14) 0.0197(13) 0.0009(11) -0.0007(10) 0.0002(10) C51 0.0176(12) 0.0359(17) 0.0167(13) 0.0070(12) -0.0031(10) 0.0022(11) C52 0.0216(13) 0.0445(19) 0.0142(12) -0.0046(12) -0.0044(10) -0.0034(13) C53 0.0195(12) 0.0250(15) 0.0252(14) -0.0107(12) 0.0016(11) -0.0048(11) C54 0.0133(11) 0.0185(13) 0.0209(13) -0.0026(11) -0.0001(9) -0.0033(10) Ir1 0.00801(5) 0.00996(6) 0.01021(6) 0.00154(4) -0.00087(3) -0.00077(4) P1 0.0087(2) 0.0109(3) 0.0127(3) 0.0013(2) -0.0005(2) 0.0005(2) P2 0.0102(3) 0.0096(3) 0.0119(3) 0.0009(2) 0.0009(2) -0.0003(2) P3 0.0088(2) 0.0102(3) 0.0132(3) 0.0010(2) -0.0008(2) -0.0011(2) C55 0.039(6) 0.031(7) 0.054(8) 0.000(6) 0.000(6) 0.002(5) O1 0.039(5) 0.033(5) 0.085(8) -0.015(5) 0.015(5) -0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.394(3) . ? C1 C6 1.396(3) . ? C1 P1 1.852(2) . ? C2 H2 0.9300 . ? C2 C3 1.397(4) . ? C3 H3 0.9300 . ? C3 C4 1.388(4) . ? C4 H4 0.9300 . ? C4 C5 1.387(4) . ? C5 H5 0.9300 . ? C5 C6 1.391(4) . ? C6 H6 0.9300 . ? C7 C8 1.390(4) . ? C7 C12 1.398(3) . ? C7 P1 1.852(2) . ? C8 H8 0.9300 . ? C8 C9 1.395(4) . ? C9 H9 0.9300 . ? C9 C10 1.384(4) . ? C10 H10 0.9300 . ? C10 C11 1.385(4) . ? C11 H11 0.9300 . ? C11 C12 1.390(3) . ? C12 H12 0.9300 . ? C13 C14 1.400(3) . ? C13 C18 1.401(3) . ? C13 P1 1.838(2) . ? C14 H14 0.9300 . ? C14 C15 1.391(3) . ? C15 H15 0.9300 . ? C15 C16 1.387(4) . ? C16 H16 0.9300 . ? C16 C17 1.390(4) . ? C17 H17 0.9300 . ? C17 C18 1.391(3) . ? C18 H18 0.9300 . ? C19 C20 1.392(3) . ? C19 C24 1.397(3) . ? C19 P2 1.852(2) . ? C20 H20 0.9300 . ? C20 C21 1.393(3) . ? C21 H21 0.9300 . ? C21 C22 1.376(4) . ? C22 H22 0.9300 . ? C22 C23 1.390(4) . ? C23 H23 0.9300 . ? C23 C24 1.389(3) . ? C24 H24 0.9300 . ? C25 C26 1.397(4) . ? C25 C30 1.385(3) . ? C25 P2 1.852(2) . ? C26 H26 0.9300 . ? C26 C27 1.393(4) . ? C27 H27 0.9300 . ? C27 C28 1.386(4) . ? C28 H28 0.9300 . ? C28 C29 1.381(4) . ? C29 H29 0.9300 . ? C29 C30 1.396(3) . ? C30 H30 0.9300 . ? C31 C32 1.395(3) . ? C31 C36 1.405(3) . ? C31 P2 1.832(2) . ? C32 H32 0.9300 . ? C32 C33 1.387(3) . ? C33 H33 0.9300 . ? C33 C34 1.392(4) . ? C34 H34 0.9300 . ? C34 C35 1.392(4) . ? C35 H35 0.9300 . ? C35 C36 1.390(4) . ? C36 H36 0.9300 . ? C37 C38 1.390(3) . ? C37 C42 1.403(3) . ? C37 P3 1.848(2) . ? C38 H38 0.9300 . ? C38 C39 1.387(3) . ? C39 H39 0.9300 . ? C39 C40 1.385(4) . ? C40 H40 0.9300 . ? C40 C41 1.390(4) . ? C41 H41 0.9300 . ? C41 C42 1.383(4) . ? C42 H42 0.9300 . ? C43 C44 1.401(3) . ? C43 C48 1.388(3) . ? C43 P3 1.854(2) . ? C44 H44 0.9300 . ? C44 C45 1.388(3) . ? C45 H45 0.9300 . ? C45 C46 1.383(4) . ? C46 H46 0.9300 . ? C46 C47 1.387(3) . ? C47 H47 0.9300 . ? C47 C48 1.394(3) . ? C48 H48 0.9300 . ? C49 C50 1.398(3) . ? C49 C54 1.396(3) . ? C49 P3 1.831(2) . ? C50 H50 0.9300 . ? C50 C51 1.386(4) . ? C51 H51 0.9300 . ? C51 C52 1.383(4) . ? C52 H52 0.9300 . ? C52 C53 1.388(4) . ? C53 H53 0.9300 . ? C53 C54 1.388(4) . ? C54 H54 0.9300 . ? Ir1 H 1.55(3) . ? Ir1 HA 1.55(3) . ? Ir1 HB 1.55(3) . ? Ir1 P1 2.3354(6) . ? Ir1 P2 2.3261(6) . ? Ir1 P3 2.3211(6) . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C55 O1 1.425(14) . ? O1 H1 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 118.4(2) . . ? C2 C1 P1 119.32(19) . . ? C6 C1 P1 122.16(19) . . ? C1 C2 H2 119.8 . . ? C1 C2 C3 120.4(2) . . ? C3 C2 H2 119.8 . . ? C2 C3 H3 119.7 . . ? C4 C3 C2 120.5(3) . . ? C4 C3 H3 119.7 . . ? C3 C4 H4 120.3 . . ? C5 C4 C3 119.3(3) . . ? C5 C4 H4 120.3 . . ? C4 C5 H5 119.9 . . ? C4 C5 C6 120.2(2) . . ? C6 C5 H5 119.9 . . ? C1 C6 H6 119.5 . . ? C5 C6 C1 121.1(2) . . ? C5 C6 H6 119.5 . . ? C8 C7 C12 118.4(2) . . ? C8 C7 P1 119.69(18) . . ? C12 C7 P1 121.57(19) . . ? C7 C8 H8 119.7 . . ? C7 C8 C9 120.6(3) . . ? C9 C8 H8 119.7 . . ? C8 C9 H9 119.8 . . ? C10 C9 C8 120.4(3) . . ? C10 C9 H9 119.8 . . ? C9 C10 H10 120.3 . . ? C9 C10 C11 119.5(2) . . ? C11 C10 H10 120.3 . . ? C10 C11 H11 119.9 . . ? C10 C11 C12 120.3(2) . . ? C12 C11 H11 119.9 . . ? C7 C12 H12 119.6 . . ? C11 C12 C7 120.8(2) . . ? C11 C12 H12 119.6 . . ? C14 C13 C18 118.4(2) . . ? C14 C13 P1 119.02(17) . . ? C18 C13 P1 122.34(18) . . ? C13 C14 H14 119.7 . . ? C15 C14 C13 120.6(2) . . ? C15 C14 H14 119.7 . . ? C14 C15 H15 119.7 . . ? C16 C15 C14 120.5(2) . . ? C16 C15 H15 119.7 . . ? C15 C16 H16 120.3 . . ? C15 C16 C17 119.4(2) . . ? C17 C16 H16 120.3 . . ? C16 C17 H17 119.8 . . ? C16 C17 C18 120.5(2) . . ? C18 C17 H17 119.8 . . ? C13 C18 H18 119.7 . . ? C17 C18 C13 120.6(2) . . ? C17 C18 H18 119.7 . . ? C20 C19 C24 118.6(2) . . ? C20 C19 P2 119.24(18) . . ? C24 C19 P2 121.50(18) . . ? C19 C20 H20 119.6 . . ? C19 C20 C21 120.7(2) . . ? C21 C20 H20 119.6 . . ? C20 C21 H21 119.9 . . ? C22 C21 C20 120.1(2) . . ? C22 C21 H21 119.9 . . ? C21 C22 H22 120.0 . . ? C21 C22 C23 119.9(2) . . ? C23 C22 H22 120.0 . . ? C22 C23 H23 119.9 . . ? C24 C23 C22 120.1(2) . . ? C24 C23 H23 119.9 . . ? C19 C24 H24 119.8 . . ? C23 C24 C19 120.5(2) . . ? C23 C24 H24 119.8 . . ? C26 C25 P2 122.0(2) . . ? C30 C25 C26 118.6(2) . . ? C30 C25 P2 118.44(19) . . ? C25 C26 H26 119.7 . . ? C27 C26 C25 120.7(3) . . ? C27 C26 H26 119.7 . . ? C26 C27 H27 120.0 . . ? C28 C27 C26 120.0(3) . . ? C28 C27 H27 120.0 . . ? C27 C28 H28 120.2 . . ? C29 C28 C27 119.7(3) . . ? C29 C28 H28 120.2 . . ? C28 C29 H29 119.9 . . ? C28 C29 C30 120.3(3) . . ? C30 C29 H29 119.9 . . ? C25 C30 C29 120.7(2) . . ? C25 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C32 C31 C36 118.4(2) . . ? C32 C31 P2 120.14(18) . . ? C36 C31 P2 121.21(19) . . ? C31 C32 H32 119.5 . . ? C33 C32 C31 121.0(2) . . ? C33 C32 H32 119.5 . . ? C32 C33 H33 119.8 . . ? C32 C33 C34 120.4(2) . . ? C34 C33 H33 119.8 . . ? C33 C34 H34 120.4 . . ? C33 C34 C35 119.2(2) . . ? C35 C34 H34 120.4 . . ? C34 C35 H35 119.7 . . ? C36 C35 C34 120.5(2) . . ? C36 C35 H35 119.7 . . ? C31 C36 H36 119.8 . . ? C35 C36 C31 120.5(2) . . ? C35 C36 H36 119.8 . . ? C38 C37 C42 117.9(2) . . ? C38 C37 P3 121.39(18) . . ? C42 C37 P3 120.49(19) . . ? C37 C38 H38 119.4 . . ? C39 C38 C37 121.1(2) . . ? C39 C38 H38 119.4 . . ? C38 C39 H39 119.8 . . ? C40 C39 C38 120.4(2) . . ? C40 C39 H39 119.8 . . ? C39 C40 H40 120.4 . . ? C39 C40 C41 119.2(2) . . ? C41 C40 H40 120.4 . . ? C40 C41 H41 119.8 . . ? C42 C41 C40 120.4(2) . . ? C42 C41 H41 119.8 . . ? C37 C42 H42 119.5 . . ? C41 C42 C37 121.0(2) . . ? C41 C42 H42 119.5 . . ? C44 C43 P3 122.10(19) . . ? C48 C43 C44 118.6(2) . . ? C48 C43 P3 119.09(18) . . ? C43 C44 H44 119.7 . . ? C45 C44 C43 120.6(2) . . ? C45 C44 H44 119.7 . . ? C44 C45 H45 119.8 . . ? C46 C45 C44 120.4(2) . . ? C46 C45 H45 119.8 . . ? C45 C46 H46 120.2 . . ? C45 C46 C47 119.6(2) . . ? C47 C46 H46 120.2 . . ? C46 C47 H47 119.9 . . ? C46 C47 C48 120.2(2) . . ? C48 C47 H47 119.9 . . ? C43 C48 C47 120.7(2) . . ? C43 C48 H48 119.7 . . ? C47 C48 H48 119.7 . . ? C50 C49 P3 119.98(19) . . ? C54 C49 C50 118.1(2) . . ? C54 C49 P3 121.71(19) . . ? C49 C50 H50 119.5 . . ? C51 C50 C49 121.0(3) . . ? C51 C50 H50 119.5 . . ? C50 C51 H51 119.8 . . ? C52 C51 C50 120.4(3) . . ? C52 C51 H51 119.8 . . ? C51 C52 H52 120.3 . . ? C51 C52 C53 119.3(2) . . ? C53 C52 H52 120.3 . . ? C52 C53 H53 119.8 . . ? C54 C53 C52 120.4(3) . . ? C54 C53 H53 119.8 . . ? C49 C54 H54 119.6 . . ? C53 C54 C49 120.8(3) . . ? C53 C54 H54 119.6 . . ? H Ir1 HA 82.3(14) . . ? H Ir1 HB 79.4(14) . . ? HA Ir1 HB 84.0(15) . . ? P1 Ir1 H 83.5(11) . . ? P1 Ir1 HA 165.5(11) . . ? P1 Ir1 HB 90.6(10) . . ? P2 Ir1 H 162.9(11) . . ? P2 Ir1 HA 91.2(10) . . ? P2 Ir1 HB 84.2(10) . . ? P2 Ir1 P1 101.58(2) . . ? P3 Ir1 H 91.4(11) . . ? P3 Ir1 HA 80.7(11) . . ? P3 Ir1 HB 163.1(10) . . ? P3 Ir1 P1 102.58(2) . . ? P3 Ir1 P2 103.22(2) . . ? C1 P1 Ir1 116.13(8) . . ? C7 P1 C1 97.53(10) . . ? C7 P1 Ir1 115.78(8) . . ? C13 P1 C1 101.42(11) . . ? C13 P1 C7 103.13(11) . . ? C13 P1 Ir1 119.57(7) . . ? C19 P2 C25 94.72(10) . . ? C19 P2 Ir1 116.11(8) . . ? C25 P2 Ir1 116.12(8) . . ? C31 P2 C19 102.83(11) . . ? C31 P2 C25 102.36(11) . . ? C31 P2 Ir1 120.70(8) . . ? C37 P3 C43 96.45(10) . . ? C37 P3 Ir1 115.94(8) . . ? C43 P3 Ir1 116.79(8) . . ? C49 P3 C37 102.43(11) . . ? C49 P3 C43 101.54(11) . . ? C49 P3 Ir1 120.03(7) . . ? H55A C55 H55B 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O1 C55 H55A 109.5 . . ? O1 C55 H55B 109.5 . . ? O1 C55 H55C 109.5 . . ? C55 O1 H1 109.5 . . ? 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 C1 C2 C3 C4 -0.5(4) . . . . ? C2 C1 C6 C5 -2.5(3) . . . . ? C2 C1 P1 C7 -98.4(2) . . . . ? C2 C1 P1 C13 156.52(19) . . . . ? C2 C1 P1 Ir1 25.2(2) . . . . ? C2 C3 C4 C5 -1.3(4) . . . . ? C3 C4 C5 C6 1.1(4) . . . . ? C4 C5 C6 C1 0.8(4) . . . . ? C6 C1 C2 C3 2.3(4) . . . . ? C6 C1 P1 C7 77.7(2) . . . . ? C6 C1 P1 C13 -27.4(2) . . . . ? C6 C1 P1 Ir1 -158.73(16) . . . . ? C7 C8 C9 C10 0.0(5) . . . . ? C8 C7 C12 C11 1.9(4) . . . . ? C8 C7 P1 C1 103.4(2) . . . . ? C8 C7 P1 C13 -153.0(2) . . . . ? C8 C7 P1 Ir1 -20.5(2) . . . . ? C8 C9 C10 C11 0.7(5) . . . . ? C9 C10 C11 C12 -0.1(4) . . . . ? C10 C11 C12 C7 -1.2(4) . . . . ? C12 C7 C8 C9 -1.3(4) . . . . ? C12 C7 P1 C1 -70.2(2) . . . . ? C12 C7 P1 C13 33.4(2) . . . . ? C12 C7 P1 Ir1 165.91(18) . . . . ? C13 C14 C15 C16 0.1(4) . . . . ? C14 C13 C18 C17 1.6(3) . . . . ? C14 C13 P1 C1 -47.9(2) . . . . ? C14 C13 P1 C7 -148.52(19) . . . . ? C14 C13 P1 Ir1 81.2(2) . . . . ? C14 C15 C16 C17 1.1(4) . . . . ? C15 C16 C17 C18 -0.9(4) . . . . ? C16 C17 C18 C13 -0.4(4) . . . . ? C18 C13 C14 C15 -1.4(3) . . . . ? C18 C13 P1 C1 137.4(2) . . . . ? C18 C13 P1 C7 36.8(2) . . . . ? C18 C13 P1 Ir1 -93.45(19) . . . . ? C19 C20 C21 C22 -0.4(4) . . . . ? C20 C19 C24 C23 1.1(4) . . . . ? C20 C19 P2 C25 -99.4(2) . . . . ? C20 C19 P2 C31 156.80(19) . . . . ? C20 C19 P2 Ir1 22.8(2) . . . . ? C20 C21 C22 C23 0.7(4) . . . . ? C21 C22 C23 C24 0.0(4) . . . . ? C22 C23 C24 C19 -0.9(4) . . . . ? C24 C19 C20 C21 -0.5(4) . . . . ? C24 C19 P2 C25 71.2(2) . . . . ? C24 C19 P2 C31 -32.6(2) . . . . ? C24 C19 P2 Ir1 -166.60(17) . . . . ? C25 C26 C27 C28 -0.4(4) . . . . ? C26 C25 C30 C29 1.4(3) . . . . ? C26 C25 P2 C19 -72.2(2) . . . . ? C26 C25 P2 C31 32.0(2) . . . . ? C26 C25 P2 Ir1 165.64(17) . . . . ? C26 C27 C28 C29 1.3(4) . . . . ? C27 C28 C29 C30 -0.9(4) . . . . ? C28 C29 C30 C25 -0.5(4) . . . . ? C30 C25 C26 C27 -1.0(4) . . . . ? C30 C25 P2 C19 96.67(19) . . . . ? C30 C25 P2 C31 -159.08(18) . . . . ? C30 C25 P2 Ir1 -25.5(2) . . . . ? C31 C32 C33 C34 -0.1(4) . . . . ? C32 C31 C36 C35 1.0(4) . . . . ? C32 C31 P2 C19 -45.0(2) . . . . ? C32 C31 P2 C25 -142.9(2) . . . . ? C32 C31 P2 Ir1 86.3(2) . . . . ? C32 C33 C34 C35 1.0(5) . . . . ? C33 C34 C35 C36 -1.0(5) . . . . ? C34 C35 C36 C31 0.0(5) . . . . ? C36 C31 C32 C33 -0.9(4) . . . . ? C36 C31 P2 C19 140.6(2) . . . . ? C36 C31 P2 C25 42.8(2) . . . . ? C36 C31 P2 Ir1 -88.1(2) . . . . ? C37 C38 C39 C40 0.4(4) . . . . ? C38 C37 C42 C41 1.2(4) . . . . ? C38 C37 P3 C43 107.0(2) . . . . ? C38 C37 P3 C49 -149.7(2) . . . . ? C38 C37 P3 Ir1 -17.0(2) . . . . ? C38 C39 C40 C41 0.5(4) . . . . ? C39 C40 C41 C42 -0.6(4) . . . . ? C40 C41 C42 C37 -0.3(4) . . . . ? C42 C37 C38 C39 -1.2(4) . . . . ? C42 C37 P3 C43 -67.7(2) . . . . ? C42 C37 P3 C49 35.7(2) . . . . ? C42 C37 P3 Ir1 168.33(17) . . . . ? C43 C44 C45 C46 1.1(4) . . . . ? C44 C43 C48 C47 0.8(4) . . . . ? C44 C43 P3 C37 81.0(2) . . . . ? C44 C43 P3 C49 -23.2(2) . . . . ? C44 C43 P3 Ir1 -155.65(17) . . . . ? C44 C45 C46 C47 0.1(4) . . . . ? C45 C46 C47 C48 -0.9(4) . . . . ? C46 C47 C48 C43 0.4(4) . . . . ? C48 C43 C44 C45 -1.5(4) . . . . ? C48 C43 P3 C37 -93.1(2) . . . . ? C48 C43 P3 C49 162.79(19) . . . . ? C48 C43 P3 Ir1 30.3(2) . . . . ? C49 C50 C51 C52 0.7(4) . . . . ? C50 C49 C54 C53 0.3(3) . . . . ? C50 C49 P3 C37 -149.56(18) . . . . ? C50 C49 P3 C43 -50.2(2) . . . . ? C50 C49 P3 Ir1 80.29(19) . . . . ? C50 C51 C52 C53 0.1(4) . . . . ? C51 C52 C53 C54 -0.6(4) . . . . ? C52 C53 C54 C49 0.4(4) . . . . ? C54 C49 C50 C51 -0.9(3) . . . . ? C54 C49 P3 C37 36.2(2) . . . . ? C54 C49 P3 C43 135.51(19) . . . . ? C54 C49 P3 Ir1 -93.99(19) . . . . ? P1 C1 C2 C3 178.48(19) . . . . ? P1 C1 C6 C5 -178.54(18) . . . . ? P1 C7 C8 C9 -175.2(2) . . . . ? P1 C7 C12 C11 175.6(2) . . . . ? P1 C13 C14 C15 -176.32(18) . . . . ? P1 C13 C18 C17 176.28(18) . . . . ? P2 C19 C20 C21 170.40(19) . . . . ? P2 C19 C24 C23 -169.6(2) . . . . ? P2 C25 C26 C27 167.87(19) . . . . ? P2 C25 C30 C29 -167.88(18) . . . . ? P2 C31 C32 C33 -175.5(2) . . . . ? P2 C31 C36 C35 175.4(2) . . . . ? P3 C37 C38 C39 -176.00(18) . . . . ? P3 C37 C42 C41 176.0(2) . . . . ? P3 C43 C44 C45 -175.56(19) . . . . ? P3 C43 C48 C47 175.01(19) . . . . ? P3 C49 C50 C51 -175.38(18) . . . . ? P3 C49 C54 C53 174.71(18) . . . . ? _shelx_res_file ; TITL sbd1905_a.res in P2(1)/c sbd1905.res created by SHELXL-2018/3 at 08:54:20 on 17-Sep-2019 REM Old TITL sbd1905 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.048, Rweak 0.003, Alpha 0.025 REM 0.418 for 343 systematic absences, Orientation as input REM Formula found by SHELXT: C54 P3 Ir CELL 1.54184 17.318012 12.990244 19.717879 90 94.4442 90 ZERR 4 0.000115 0.000096 0.00016 0 0.0007 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Ir O P UNIT 217.13 196.53 4 1.13 12 L.S. 16 PLAN 20 BOND $H CONF list 4 fmap 2 53 acta REM REM REM WGHT 0.021600 0.676800 EXTI 0.000059 FVAR 1.98556 0.28295 C1 1 0.649475 0.967670 0.674577 11.00000 0.00902 0.01193 = 0.01706 0.00092 -0.00278 0.00251 C2 1 0.686152 1.033955 0.631655 11.00000 0.01963 0.01640 = 0.01909 0.00151 -0.00267 0.00156 AFIX 43 H2 2 0.701960 1.009582 0.590599 11.00000 -1.20000 AFIX 0 C3 1 0.699308 1.136768 0.649931 11.00000 0.03377 0.01355 = 0.02708 0.00666 -0.00016 -0.00285 AFIX 43 H3 2 0.724145 1.180207 0.621083 11.00000 -1.20000 AFIX 0 C4 1 0.675591 1.174582 0.710820 11.00000 0.03171 0.01092 = 0.02968 -0.00077 -0.01047 0.00401 AFIX 43 H4 2 0.685333 1.242681 0.723272 11.00000 -1.20000 AFIX 0 C5 1 0.637228 1.109776 0.752882 11.00000 0.02166 0.02059 = 0.02066 -0.00330 -0.00623 0.00815 AFIX 43 H5 2 0.620345 1.134781 0.793382 11.00000 -1.20000 AFIX 0 C6 1 0.623929 1.007485 0.734669 11.00000 0.01542 0.01729 = 0.01920 0.00197 -0.00217 0.00307 AFIX 43 H6 2 0.597591 0.964931 0.762988 11.00000 -1.20000 AFIX 0 C7 1 0.528190 0.849144 0.615557 11.00000 0.01127 0.01130 = 0.02236 0.00171 -0.00224 0.00122 C8 1 0.508903 0.853741 0.545867 11.00000 0.01614 0.02817 = 0.02285 0.00171 -0.00442 0.00389 AFIX 43 H8 2 0.546993 0.843354 0.515821 11.00000 -1.20000 AFIX 0 C9 1 0.432909 0.873798 0.520591 11.00000 0.02184 0.04194 = 0.02805 0.00152 -0.01083 0.00710 AFIX 43 H9 2 0.420719 0.876647 0.473858 11.00000 -1.20000 AFIX 0 C10 1 0.375564 0.889478 0.564605 11.00000 0.01275 0.02404 = 0.04497 -0.00094 -0.00870 0.00329 AFIX 43 H10 2 0.324839 0.902083 0.547635 11.00000 -1.20000 AFIX 0 C11 1 0.394325 0.886247 0.634138 11.00000 0.01205 0.01954 = 0.04037 -0.00151 0.00380 0.00046 AFIX 43 H11 2 0.356053 0.896845 0.663979 11.00000 -1.20000 AFIX 0 C12 1 0.470085 0.867239 0.659507 11.00000 0.01539 0.01735 = 0.02326 -0.00007 -0.00079 0.00224 AFIX 43 H12 2 0.482275 0.866547 0.706276 11.00000 -1.20000 AFIX 0 C13 1 0.623564 0.768814 0.730284 11.00000 0.01056 0.01272 = 0.01236 -0.00058 0.00289 0.00196 C14 1 0.680508 0.788074 0.783093 11.00000 0.01256 0.01256 = 0.01626 0.00115 0.00139 0.00182 AFIX 43 H14 2 0.719416 0.835680 0.776788 11.00000 -1.20000 AFIX 0 C15 1 0.679438 0.736686 0.844887 11.00000 0.01820 0.01566 = 0.01405 -0.00184 -0.00216 0.00493 AFIX 43 H15 2 0.717559 0.750292 0.879574 11.00000 -1.20000 AFIX 0 C16 1 0.621938 0.665285 0.855177 11.00000 0.02300 0.01622 = 0.01562 0.00418 0.00631 0.00577 AFIX 43 H16 2 0.620879 0.631884 0.896812 11.00000 -1.20000 AFIX 0 C17 1 0.565933 0.644122 0.802706 11.00000 0.01704 0.01436 = 0.02308 0.00097 0.00557 -0.00083 AFIX 43 H17 2 0.527686 0.595598 0.809102 11.00000 -1.20000 AFIX 0 C18 1 0.566677 0.695003 0.740686 11.00000 0.01209 0.01325 = 0.01826 -0.00033 0.00105 0.00022 AFIX 43 H18 2 0.529100 0.679904 0.705834 11.00000 -1.20000 AFIX 0 C19 1 0.620828 0.532203 0.613987 11.00000 0.01288 0.01261 = 0.01336 -0.00117 0.00287 -0.00306 C20 1 0.553420 0.576459 0.583876 11.00000 0.01665 0.01286 = 0.01754 -0.00228 0.00232 -0.00189 AFIX 43 H20 2 0.555714 0.640549 0.563109 11.00000 -1.20000 AFIX 0 C21 1 0.482557 0.525799 0.584507 11.00000 0.01261 0.02569 = 0.02266 -0.00248 0.00116 -0.00210 AFIX 43 H21 2 0.437873 0.556350 0.564481 11.00000 -1.20000 AFIX 0 C22 1 0.478571 0.430648 0.614709 11.00000 0.01666 0.02758 = 0.02462 -0.00387 0.00762 -0.01059 AFIX 43 H22 2 0.431335 0.396584 0.614679 11.00000 -1.20000 AFIX 0 C23 1 0.545252 0.385515 0.645262 11.00000 0.02827 0.01777 = 0.02601 0.00343 0.00820 -0.00754 AFIX 43 H23 2 0.542581 0.321233 0.665711 11.00000 -1.20000 AFIX 0 C24 1 0.615865 0.436244 0.645310 11.00000 0.01764 0.01717 = 0.02043 0.00353 0.00386 -0.00070 AFIX 43 H24 2 0.660167 0.406091 0.666355 11.00000 -1.20000 AFIX 0 C25 1 0.738964 0.500258 0.532873 11.00000 0.01047 0.01405 = 0.01948 -0.00242 0.00490 -0.00241 C26 1 0.759242 0.398066 0.547226 11.00000 0.02313 0.01817 = 0.02224 0.00056 0.00745 0.00195 AFIX 43 H26 2 0.770773 0.377731 0.592092 11.00000 -1.20000 AFIX 0 C27 1 0.762376 0.326301 0.495048 11.00000 0.02615 0.01627 = 0.03637 -0.00337 0.01148 0.00167 AFIX 43 H27 2 0.776221 0.258524 0.505146 11.00000 -1.20000 AFIX 0 C28 1 0.744869 0.355836 0.428068 11.00000 0.01768 0.02529 = 0.02825 -0.01152 0.00773 -0.00366 AFIX 43 H28 2 0.745917 0.307726 0.393223 11.00000 -1.20000 AFIX 0 C29 1 0.725861 0.457073 0.413344 11.00000 0.01424 0.02924 = 0.02084 -0.00599 0.00208 -0.00604 AFIX 43 H29 2 0.714791 0.477324 0.368402 11.00000 -1.20000 AFIX 0 C30 1 0.723192 0.529132 0.465628 11.00000 0.01184 0.01794 = 0.01926 -0.00161 0.00093 -0.00253 AFIX 43 H30 2 0.710694 0.597233 0.455189 11.00000 -1.20000 AFIX 0 C31 1 0.777488 0.546351 0.673817 11.00000 0.01260 0.01038 = 0.01719 0.00240 -0.00088 -0.00016 C32 1 0.750735 0.548830 0.738712 11.00000 0.01499 0.01513 = 0.01968 0.00313 0.00117 0.00193 AFIX 43 H32 2 0.700025 0.569030 0.743967 11.00000 -1.20000 AFIX 0 C33 1 0.798614 0.521626 0.795531 11.00000 0.02200 0.02661 = 0.01719 0.00449 0.00128 0.00281 AFIX 43 H33 2 0.779804 0.523812 0.838424 11.00000 -1.20000 AFIX 0 C34 1 0.874654 0.491072 0.788714 11.00000 0.02141 0.03916 = 0.02223 0.01151 -0.00322 0.00716 AFIX 43 H34 2 0.906512 0.471766 0.826723 11.00000 -1.20000 AFIX 0 C35 1 0.902481 0.489742 0.724336 11.00000 0.01303 0.03639 = 0.03185 0.00954 0.00254 0.00907 AFIX 43 H35 2 0.953466 0.470440 0.719457 11.00000 -1.20000 AFIX 0 C36 1 0.854669 0.517030 0.667324 11.00000 0.01670 0.01943 = 0.02012 0.00417 0.00380 0.00506 AFIX 43 H36 2 0.873881 0.515880 0.624576 11.00000 -1.20000 AFIX 0 C37 1 0.868441 0.942397 0.573118 11.00000 0.01138 0.01172 = 0.02024 0.00002 0.00501 -0.00016 C38 1 0.835602 0.977206 0.510760 11.00000 0.01244 0.01408 = 0.01998 -0.00023 0.00254 -0.00098 AFIX 43 H38 2 0.793133 0.942725 0.489825 11.00000 -1.20000 AFIX 0 C39 1 0.865073 1.062494 0.479201 11.00000 0.02178 0.02079 = 0.01817 0.00356 0.00405 -0.00004 AFIX 43 H39 2 0.842037 1.084807 0.437613 11.00000 -1.20000 AFIX 0 C40 1 0.928607 1.114641 0.509248 11.00000 0.02407 0.01589 = 0.02957 0.00442 0.00916 -0.00563 AFIX 43 H40 2 0.948107 1.172142 0.488260 11.00000 -1.20000 AFIX 0 C41 1 0.962844 1.079965 0.571139 11.00000 0.01792 0.02295 = 0.03613 0.00070 -0.00124 -0.00867 AFIX 43 H41 2 1.005805 1.114085 0.591502 11.00000 -1.20000 AFIX 0 C42 1 0.933387 0.995020 0.602610 11.00000 0.01592 0.02031 = 0.02310 0.00558 -0.00145 -0.00292 AFIX 43 H42 2 0.956963 0.972434 0.643926 11.00000 -1.20000 AFIX 0 C43 1 0.918081 0.742668 0.596487 11.00000 0.01135 0.01076 = 0.01884 0.00334 0.00276 -0.00033 C44 1 0.987390 0.746230 0.638108 11.00000 0.01538 0.01764 = 0.01919 -0.00143 0.00026 -0.00079 AFIX 43 H44 2 0.990602 0.786942 0.677022 11.00000 -1.20000 AFIX 0 C45 1 1.051300 0.689506 0.621750 11.00000 0.01371 0.02259 = 0.02574 0.00426 -0.00428 0.00232 AFIX 43 H45 2 1.096722 0.691587 0.650154 11.00000 -1.20000 AFIX 0 C46 1 1.047824 0.629924 0.563471 11.00000 0.01302 0.01403 = 0.03212 0.00299 0.00368 0.00318 AFIX 43 H46 2 1.090692 0.591893 0.552686 11.00000 -1.20000 AFIX 0 C47 1 0.979997 0.627247 0.521209 11.00000 0.01886 0.01489 = 0.02369 -0.00075 0.00239 0.00016 AFIX 43 H47 2 0.977592 0.588024 0.481645 11.00000 -1.20000 AFIX 0 C48 1 0.915398 0.683196 0.537867 11.00000 0.01359 0.01338 = 0.02232 0.00085 0.00086 -0.00150 AFIX 43 H48 2 0.870039 0.680635 0.509400 11.00000 -1.20000 AFIX 0 C49 1 0.852080 0.851354 0.703717 11.00000 0.00634 0.01935 = 0.01327 0.00025 -0.00146 -0.00173 C50 1 0.869035 0.770890 0.749525 11.00000 0.01223 0.02177 = 0.01966 0.00088 -0.00066 0.00016 AFIX 43 H50 2 0.874499 0.704353 0.733160 11.00000 -1.20000 AFIX 0 C51 1 0.877825 0.788825 0.819001 11.00000 0.01764 0.03586 = 0.01665 0.00701 -0.00313 0.00217 AFIX 43 H51 2 0.889674 0.734493 0.848716 11.00000 -1.20000 AFIX 0 C52 1 0.869075 0.887060 0.844396 11.00000 0.02156 0.04451 = 0.01425 -0.00464 -0.00439 -0.00335 AFIX 43 H52 2 0.875024 0.899016 0.891011 11.00000 -1.20000 AFIX 0 C53 1 0.851330 0.967600 0.799620 11.00000 0.01949 0.02502 = 0.02524 -0.01075 0.00160 -0.00481 AFIX 43 H53 2 0.844872 1.033717 0.816363 11.00000 -1.20000 AFIX 0 C54 1 0.843167 0.950026 0.729996 11.00000 0.01327 0.01846 = 0.02093 -0.00264 -0.00006 -0.00330 AFIX 43 H54 2 0.831612 1.004696 0.700487 11.00000 -1.20000 AFIX 0 IR1 3 0.712811 0.765004 0.570515 11.00000 0.00801 0.00996 = 0.01021 0.00154 -0.00087 -0.00077 H 2 0.695560 0.867759 0.532469 11.00000 0.03060 HA 2 0.759266 0.742907 0.507898 11.00000 0.02447 HB 2 0.642156 0.733496 0.522151 11.00000 0.01928 P1 5 0.630739 0.832721 0.647835 11.00000 0.00868 0.01088 = 0.01268 0.00128 -0.00047 0.00049 P2 5 0.715531 0.591726 0.600356 11.00000 0.01021 0.00957 = 0.01191 0.00095 0.00090 -0.00026 P3 5 0.833573 0.824022 0.612834 11.00000 0.00882 0.01020 = 0.01322 0.00101 -0.00079 -0.00112 C55 1 0.892960 1.236845 0.688885 21.00000 0.03892 0.03096 = 0.05369 -0.00008 -0.00029 0.00190 AFIX 137 H55A 2 0.869970 1.240671 0.643063 21.00000 -1.50000 H55B 2 0.906489 1.166736 0.699640 21.00000 -1.50000 H55C 2 0.938713 1.278797 0.693202 21.00000 -1.50000 AFIX 0 O1 4 0.839075 1.272973 0.734545 21.00000 0.03920 0.03266 = 0.08488 -0.01523 0.01462 -0.00749 AFIX 147 H1 2 0.795713 1.275687 0.714726 21.00000 -1.50000 AFIX 0 HKLF 4 REM sbd1905_a.res in P2(1)/c REM wR2 = 0.0480, GooF = S = 1.047, Restrained GooF = 1.047 for all data REM R1 = 0.0199 for 7174 Fo > 4sig(Fo) and 0.0237 for all 7896 data REM 557 parameters refined using 0 restraints END WGHT 0.0216 0.6768 REM Highest difference peak 0.714, deepest hole -0.525, 1-sigma level 0.073 Q1 1 0.7356 0.7632 0.6201 11.00000 0.05 0.71 Q2 1 0.6919 0.7634 0.5185 11.00000 0.05 0.68 Q3 1 0.7239 0.5413 0.5615 11.00000 0.05 0.47 Q4 1 0.6607 0.5577 0.6132 11.00000 0.05 0.36 Q5 1 0.8788 0.7858 0.6032 11.00000 0.05 0.36 Q6 1 0.7539 0.5619 0.6408 11.00000 0.05 0.33 Q7 1 0.8444 0.8378 0.6618 11.00000 0.05 0.33 Q8 1 0.6594 0.8126 0.5206 11.00000 0.05 0.32 Q9 1 0.6544 0.9052 0.6608 11.00000 0.05 0.32 Q10 1 0.8566 0.7405 0.7842 11.00000 0.05 0.32 Q11 1 0.7614 0.5403 0.6993 11.00000 0.05 0.31 Q12 1 0.6199 0.4806 0.6241 11.00000 0.05 0.31 Q13 1 0.8908 1.0913 0.5013 11.00000 0.05 0.29 Q14 1 0.5981 0.7544 0.7400 11.00000 0.05 0.28 Q15 1 0.6636 0.7664 0.7562 11.00000 0.05 0.28 Q16 1 0.6377 0.7144 0.5585 11.00000 0.05 0.28 Q17 1 0.8977 0.9622 0.5806 11.00000 0.05 0.28 Q18 1 0.7174 0.5024 0.4996 11.00000 0.05 0.27 Q19 1 0.7381 0.8368 0.5430 11.00000 0.05 0.27 Q20 1 1.0081 0.6373 0.5363 11.00000 0.05 0.27 ; _shelx_res_checksum 62826 _olex2_date_sample_data_collection 2019-09-06 _olex2_date_sample_submission 2019-09-03 _olex2_exptl_crystal_mounting_method 'oil on micromount' _olex2_submission_original_sample_id 'BT PPh3' _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.213 _oxdiff_exptl_absorpt_empirical_full_min 0.794 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_sbd1906 _database_code_depnum_ccdc_archive 'CCDC 1957543' loop_ _audit_author_name _audit_author_address 'Adrian C. Whitwood' ;University of York United Kingdom ; _audit_update_record ; 2019-10-04 deposited with the CCDC. 2019-12-10 downloaded from the CCDC. ; _audit_creation_date 2019-09-30 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C56 H64 Cl2 Ir2 N4 S2, C H4 O' _chemical_formula_sum 'C57 H68 Cl2 Ir2 N4 O S2' _chemical_formula_weight 1344.57 _chemical_melting_point ? _chemical_oxdiff_formula 'C57 H64 Cl2 Ir2 N4 O S2' _chemical_oxdiff_usercomment 'Ben Tickner BT Ma1' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -4.7710 6.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.9317(2) _cell_length_b 16.6000(3) _cell_length_c 25.5365(4) _cell_angle_alpha 90 _cell_angle_beta 90.2757(13) _cell_angle_gamma 90 _cell_volume 5481.76(15) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9511 _cell_measurement_temperature 110.00(10) _cell_measurement_theta_max 70.9880 _cell_measurement_theta_min 6.5490 _shelx_estimated_absorpt_T_max 0.476 _shelx_estimated_absorpt_T_min 0.286 _exptl_absorpt_coefficient_mu 11.192 _exptl_absorpt_correction_T_max 0.674 _exptl_absorpt_correction_T_min 0.403 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier . _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 2664 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.0444 -1 1 2 0.0518 1 1 -5 0.0332 -1 -1 0 0.0661 -2 -1 -2 0.0572 -1 0 -2 0.0535 0 1 -2 0.0254 2 1 -1 0.0654 -1 0 1 0.0657 1 -2 -1 0.0426 2 -2 -1 0.0549 -1 2 1 0.0476 0 2 1 0.0427 0 -2 -1 0.0355 1 1 2 0.0587 0 0 1 0.0395 _exptl_crystal_recrystallization_method 'crystallisation from methanol' _exptl_crystal_size_max 0.149 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.078 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -0.0002 -0.0010 -1.0002 -0.0284 -0.0531 0.0048 -0.9972 1.0043 2.0004 -0.0674 0.1764 0.0393 0.9993 0.9957 -5.0009 -0.1588 -0.2688 -0.1260 -1.0001 -1.0007 -0.0002 0.0169 0.0035 0.1501 -1.9993 -1.0020 -2.0008 -0.0935 -0.0657 0.2592 -0.9992 -0.0013 -2.0006 -0.1104 -0.0692 0.1092 0.0009 0.9995 -2.0004 -0.1273 -0.0727 -0.0409 1.9988 0.9990 -0.9999 0.0084 -0.0935 -0.2448 -0.9987 0.0018 1.0001 -0.0253 0.0899 0.0947 0.9961 -2.0048 -1.0003 0.1663 -0.1567 0.0064 1.9949 -2.0055 -1.0001 0.2200 -0.1936 -0.0931 -0.9961 2.0048 1.0003 -0.1663 0.1567 -0.0064 0.0027 2.0040 1.0004 -0.1127 0.1198 -0.1059 -0.0027 -2.0040 -1.0004 0.1127 -0.1198 0.1059 1.0005 1.0028 2.0007 0.0399 0.1026 -0.1597 0.0002 0.0010 1.0002 0.0284 0.0531 -0.0048 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_unetI/netI 0.0331 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 20688 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 67.076 _diffrn_reflns_theta_max 67.076 _diffrn_reflns_theta_min 3.462 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 110.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1450 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -13.00 52.00 1.00 1.00 -- 0.00 57.00 -60.00 65 2 \w -51.00 -20.00 1.00 1.00 -- 0.00 124.00 101.00 31 3 \w -13.00 13.00 1.00 3.00 -- 54.00 -57.00-150.00 26 4 \w 27.00 105.00 1.00 3.00 -- 54.00-125.00 120.00 78 5 \w -19.00 98.00 1.00 3.00 -- 54.00 -19.00 -60.00 117 6 \w 40.00 74.00 1.00 3.00 -- 54.00 -57.00 120.00 34 7 \w 92.00 119.00 1.00 3.00 -- 54.00 77.00 -90.00 27 8 \w 39.00 97.00 1.00 3.00 -- 108.00-111.00-120.00 58 9 \w 124.00 176.00 1.00 3.00 -- 108.00 50.00-150.00 52 10 \w 38.00 92.00 1.00 3.00 -- 108.00-111.00 120.00 54 11 \w 77.00 103.00 1.00 3.00 -- 108.00 -50.00 -30.00 26 12 \w 36.00 88.00 1.00 3.00 -- 108.00-111.00-180.00 52 13 \w 38.00 73.00 1.00 3.00 -- 108.00 -50.00 -30.00 35 14 \w 106.00 171.00 1.00 3.00 -- 108.00 63.00 0.00 65 15 \w 77.00 113.00 1.00 3.00 -- 108.00-111.00 -90.00 36 16 \w 90.00 176.00 1.00 3.00 -- 108.00 63.00 120.00 86 17 \w 113.00 139.00 1.00 3.00 -- 108.00 -12.00-150.00 26 18 \w 36.00 73.00 1.00 3.00 -- 108.00 -12.00-150.00 37 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0536477000 _diffrn_orient_matrix_UB_12 -0.0704874000 _diffrn_orient_matrix_UB_13 0.0284325000 _diffrn_orient_matrix_UB_21 -0.0369154000 _diffrn_orient_matrix_UB_22 0.0333776000 _diffrn_orient_matrix_UB_23 0.0530168000 _diffrn_orient_matrix_UB_31 -0.0996791000 _diffrn_orient_matrix_UB_32 -0.0503459000 _diffrn_orient_matrix_UB_33 -0.0047444000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 8700 _reflns_number_total 9782 _reflns_odcompleteness_completeness 99.73 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 1.916 _refine_diff_density_min -1.357 _refine_diff_density_rms 0.098 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 650 _refine_ls_number_reflns 9782 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0299 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+13.1045P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.0712 _refine_special_details ; The crystal showed evidence of minor twinning with two residual density peaks close to the iridiums. This could not be resolved as either merohedral or non-merohedral twinning methods. One of the 4-chlorobenzyl groups was disordered and modelled in two positions with refined occupancies of 0.803:0.197(10). pairs of disordered carbons were constrained to have the same ADP (e.g. C43, & C43a, C44 & C44a etc.). The S-CH2 bond-lengths were restrained to be equal as were the CH2-C(ipso) bond-lengths and the C-Cl bond-lengths. The phenyl ring of the minor form was constrained to be a regular hexagon with a C-C bond length of 1.39 angstroms. For the minor form the CH2-C(ortho) distances were restrained to be equal as were the C(meta)-Cl distances. The hydrides were initially located by difference map, the Ir-H bond-length was then adjusted to be 1.65 angstroms and then the location fixed to ride on the iridium. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2. Restrained distances C46A-Cl1A \\sim Cl1A-C48A with sigma of 0.02 C43A-C44A \\sim C44-C43 with sigma of 0.02 S1-C43 \\sim S1-C43A with sigma of 0.02 C49A-C43A \\sim C43A-C45A with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(C49A) = Uanis(C49) Uanis(C48) = Uanis(C48A) Uanis(C47A) = Uanis(C47) Uanis(C46A) = Uanis(C46) Uanis(C45A) = Uanis(C45) Uanis(C44A) = Uanis(C44) Uanis(C43A) = Uanis(C43) 4. Others Sof(C43A)=Sof(H43C)=Sof(H43D)=Sof(C44A)=Sof(C45A)=Sof(H45A)=Sof(C46A)= Sof(H46A)=Sof(C47A)=Sof(C48A)=Sof(H48A)=Sof(C49A)=Sof(H49A)=Sof(Cl1A)=1-FVAR(1) Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)= Sof(C47)=Sof(C48)=Sof(H48)=Sof(C49)=Sof(H49)=Sof(Cl1)=FVAR(1) 5.a Riding coordinates: Ir1(H,HA), Ir2(HB,HC) 5.b Secondary CH2 refined with riding coordinates: C43(H43A,H43B), C43A(H43C,H43D), C50(H50A,H50B) 5.c Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C6(H6), C8(H8), C15(H15), C17(H17), C23(H23), C24(H24), C27(H27), C29(H29), C36(H36), C38(H38), C45A(H45A), C46A(H46A), C48A(H48A), C49A(H49A), C45(H45), C46(H46), C48(H48), C49(H49), C52(H52), C53(H53), C55(H55), C56(H56) 5.d Fitted hexagon refined as free rotating group: C44A(C45A,C46A,C47A,C48A,C49A) 5.e Idealised Me refined as rotating group: C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C19(H19A,H19B, H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C31(H31A,H31B,H31C), C32(H32A, H32B,H32C), C33(H33A,H33B,H33C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C57(H57A,H57B,H57C) 5.f Idealised tetrahedral OH refined as rotating group: O1(H1) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C0AA C 0.2422(4) 0.3839(3) 0.26156(17) 0.0310(10) Uani 1 1 d . . . . . C2 C 0.2507(5) 0.4054(4) 0.17344(19) 0.0579(18) Uani 1 1 d . . . . . H2 H 0.277677 0.408767 0.138962 0.070 Uiso 1 1 calc R . . . . C3 C 0.1544(5) 0.4221(5) 0.1878(2) 0.068(2) Uani 1 1 d . . . . . H3 H 0.100011 0.440039 0.165607 0.082 Uiso 1 1 calc R . . . . C4 C 0.4124(4) 0.3623(3) 0.21638(16) 0.0304(10) Uani 1 1 d . . . . . C5 C 0.4406(4) 0.2822(3) 0.20970(15) 0.0298(10) Uani 1 1 d . . . . . C6 C 0.5454(4) 0.2640(3) 0.20476(17) 0.0372(11) Uani 1 1 d . . . . . H6 H 0.566074 0.209398 0.201231 0.045 Uiso 1 1 calc R . . . . C7 C 0.6198(4) 0.3238(4) 0.20487(17) 0.0409(12) Uani 1 1 d . . . . . C8 C 0.5885(4) 0.4033(4) 0.21075(18) 0.0431(13) Uani 1 1 d . . . . . H8 H 0.639251 0.444629 0.211150 0.052 Uiso 1 1 calc R . . . . C9 C 0.4843(4) 0.4242(3) 0.21610(17) 0.0388(12) Uani 1 1 d . . . . . C10 C 0.3602(4) 0.2163(3) 0.20645(19) 0.0425(12) Uani 1 1 d . . . . . H10A H 0.330470 0.214991 0.171092 0.064 Uiso 1 1 calc GR . . . . H10B H 0.305451 0.226797 0.231924 0.064 Uiso 1 1 calc GR . . . . H10C H 0.392706 0.164243 0.214207 0.064 Uiso 1 1 calc GR . . . . C11 C 0.7329(4) 0.3022(5) 0.1986(2) 0.067(2) Uani 1 1 d . . . . . H11A H 0.751220 0.259435 0.223435 0.100 Uiso 1 1 calc GR . . . . H11B H 0.775646 0.349802 0.205504 0.100 Uiso 1 1 calc GR . . . . H11C H 0.745045 0.283305 0.162783 0.100 Uiso 1 1 calc GR . . . . C12 C 0.4524(5) 0.5105(3) 0.2216(2) 0.0564(16) Uani 1 1 d . . . . . H12A H 0.402020 0.523950 0.194178 0.085 Uiso 1 1 calc GR . . . . H12B H 0.513179 0.545289 0.218247 0.085 Uiso 1 1 calc GR . . . . H12C H 0.420941 0.518706 0.256062 0.085 Uiso 1 1 calc GR . . . . C13 C 0.0547(4) 0.4278(3) 0.26964(18) 0.0391(12) Uani 1 1 d . . . . . C14 C 0.0373(4) 0.5087(3) 0.28073(19) 0.0402(12) Uani 1 1 d . . . . . C15 C -0.0582(4) 0.5291(3) 0.3024(2) 0.0424(12) Uani 1 1 d . . . . . H15 H -0.072782 0.584114 0.309394 0.051 Uiso 1 1 calc R . . . . C16 C -0.1323(4) 0.4717(3) 0.3139(2) 0.0417(12) Uani 1 1 d . . . . . C17 C -0.1104(4) 0.3921(3) 0.3037(2) 0.0457(13) Uani 1 1 d . . . . . H17 H -0.159562 0.352089 0.313015 0.055 Uiso 1 1 calc R . . . . C18 C -0.0181(4) 0.3686(3) 0.2802(2) 0.0433(13) Uani 1 1 d . . . . . C19 C 0.1174(5) 0.5718(4) 0.2705(3) 0.0635(18) Uani 1 1 d . . . . . H19A H 0.136531 0.570623 0.233387 0.095 Uiso 1 1 calc GR . . . . H19B H 0.178760 0.561008 0.292065 0.095 Uiso 1 1 calc GR . . . . H19C H 0.089508 0.624920 0.279257 0.095 Uiso 1 1 calc GR . . . . C20 C -0.2350(4) 0.4957(4) 0.3380(3) 0.0629(17) Uani 1 1 d . . . . . H20A H -0.233793 0.483891 0.375618 0.094 Uiso 1 1 calc GR . . . . H20B H -0.291023 0.465275 0.321248 0.094 Uiso 1 1 calc GR . . . . H20C H -0.246536 0.553520 0.332726 0.094 Uiso 1 1 calc GR . . . . C21 C 0.0000(5) 0.2817(4) 0.2657(3) 0.067(2) Uani 1 1 d . . . . . H21A H -0.030376 0.270932 0.231201 0.101 Uiso 1 1 calc GR . . . . H21B H -0.032440 0.246763 0.291854 0.101 Uiso 1 1 calc GR . . . . H21C H 0.074454 0.271042 0.264763 0.101 Uiso 1 1 calc GR . . . . C22 C 0.2556(3) 0.2869(3) 0.49085(16) 0.0292(10) Uani 1 1 d . . . . . C23 C 0.1576(4) 0.3373(3) 0.55626(19) 0.0419(12) Uani 1 1 d . . . . . H23 H 0.115030 0.373239 0.575500 0.050 Uiso 1 1 calc R . . . . C24 C 0.1889(4) 0.2646(3) 0.57186(18) 0.0411(12) Uani 1 1 d . . . . . H24 H 0.173285 0.238867 0.604088 0.049 Uiso 1 1 calc R . . . . C25 C 0.1818(4) 0.4268(3) 0.48070(18) 0.0372(11) Uani 1 1 d . . . . . C26 C 0.2560(5) 0.4862(3) 0.4874(2) 0.0454(13) Uani 1 1 d . . . . . C27 C 0.2352(5) 0.5597(4) 0.4629(2) 0.0600(18) Uani 1 1 d . . . . . H27 H 0.283280 0.602659 0.466369 0.072 Uiso 1 1 calc R . . . . C28 C 0.1457(6) 0.5715(4) 0.4334(2) 0.0572(16) Uani 1 1 d . . . . . C29 C 0.0756(5) 0.5107(3) 0.4288(2) 0.0502(14) Uani 1 1 d . . . . . H29 H 0.014352 0.519570 0.408943 0.060 Uiso 1 1 calc R . . . . C30 C 0.0909(4) 0.4368(3) 0.45191(19) 0.0417(12) Uani 1 1 d . . . . . C31 C 0.3538(5) 0.4719(4) 0.5189(2) 0.0590(17) Uani 1 1 d . . . . . H31A H 0.335789 0.450978 0.553567 0.088 Uiso 1 1 calc GR . . . . H31B H 0.391540 0.522790 0.522863 0.088 Uiso 1 1 calc GR . . . . H31C H 0.397494 0.432740 0.500704 0.088 Uiso 1 1 calc GR . . . . C32 C 0.1283(7) 0.6532(4) 0.4081(3) 0.092(3) Uani 1 1 d . . . . . H32A H 0.089472 0.646320 0.375320 0.138 Uiso 1 1 calc GR . . . . H32B H 0.195162 0.678399 0.400638 0.138 Uiso 1 1 calc GR . . . . H32C H 0.088889 0.687719 0.431914 0.138 Uiso 1 1 calc GR . . . . C33 C 0.0119(4) 0.3715(4) 0.4457(2) 0.0492(14) Uani 1 1 d . . . . . H33A H 0.044672 0.323458 0.430845 0.074 Uiso 1 1 calc GR . . . . H33B H -0.043384 0.389946 0.422206 0.074 Uiso 1 1 calc GR . . . . H33C H -0.017375 0.358259 0.479971 0.074 Uiso 1 1 calc GR . . . . C34 C 0.2975(4) 0.1567(3) 0.53664(16) 0.0330(10) Uani 1 1 d . . . . . C35 C 0.3980(4) 0.1529(3) 0.55631(16) 0.0346(11) Uani 1 1 d . . . . . C36 C 0.4392(4) 0.0769(3) 0.56540(18) 0.0409(12) Uani 1 1 d . . . . . H36 H 0.507100 0.072824 0.579524 0.049 Uiso 1 1 calc R . . . . C37 C 0.3849(4) 0.0065(3) 0.55460(18) 0.0409(12) Uani 1 1 d . . . . . C38 C 0.2855(4) 0.0132(3) 0.53551(18) 0.0390(11) Uani 1 1 d . . . . . H38 H 0.247003 -0.034488 0.528664 0.047 Uiso 1 1 calc R . . . . C39 C 0.2398(4) 0.0874(3) 0.52597(18) 0.0359(11) Uani 1 1 d . . . . . C40 C 0.4604(4) 0.2273(4) 0.5678(2) 0.0471(13) Uani 1 1 d . . . . . H40A H 0.490103 0.247913 0.535225 0.071 Uiso 1 1 calc GR . . . . H40B H 0.516238 0.213974 0.592433 0.071 Uiso 1 1 calc GR . . . . H40C H 0.415625 0.268410 0.583286 0.071 Uiso 1 1 calc GR . . . . C41 C 0.4350(5) -0.0742(4) 0.5638(2) 0.0536(15) Uani 1 1 d . . . . . H41A H 0.502317 -0.075614 0.546333 0.080 Uiso 1 1 calc GR . . . . H41B H 0.390628 -0.116805 0.549447 0.080 Uiso 1 1 calc GR . . . . H41C H 0.444611 -0.082727 0.601437 0.080 Uiso 1 1 calc GR . . . . C42 C 0.1312(4) 0.0937(4) 0.5047(2) 0.0512(14) Uani 1 1 d . . . . . H42A H 0.088956 0.125724 0.528719 0.077 Uiso 1 1 calc GR . . . . H42B H 0.101487 0.039661 0.501232 0.077 Uiso 1 1 calc GR . . . . H42C H 0.132556 0.119865 0.470299 0.077 Uiso 1 1 calc GR . . . . C43 C 0.2126(10) 0.1586(4) 0.3268(4) 0.0385(13) Uani 0.802(10) 1 d D . P A 1 H43A H 0.164998 0.159028 0.296303 0.046 Uiso 0.802(10) 1 calc R . P A 1 H43B H 0.283955 0.163214 0.313262 0.046 Uiso 0.802(10) 1 calc R . P A 1 C43A C 0.219(4) 0.1649(13) 0.3227(13) 0.0385(13) Uani 0.198(10) 1 d D . P A 2 H43C H 0.181325 0.170914 0.288969 0.046 Uiso 0.198(10) 1 calc R . P A 2 H43D H 0.293987 0.164602 0.315697 0.046 Uiso 0.198(10) 1 calc R . P A 2 C44 C 0.2022(6) 0.0807(5) 0.3541(4) 0.0329(15) Uani 0.802(10) 1 d D . P A 1 C44A C 0.187(2) 0.0903(17) 0.3493(15) 0.0329(15) Uani 0.198(10) 1 d D . P A 2 C45A C 0.083(2) 0.0707(16) 0.3533(14) 0.051(2) Uani 0.198(10) 1 d DG . P A 2 H45A H 0.032081 0.106502 0.340089 0.062 Uiso 0.198(10) 1 calc R . P A 2 C46A C 0.0538(16) -0.0013(15) 0.3767(11) 0.070(3) Uani 0.198(10) 1 d DG . P A 2 H46A H -0.017423 -0.014744 0.379419 0.084 Uiso 0.198(10) 1 calc R . P A 2 C47A C 0.1285(17) -0.0538(13) 0.3961(11) 0.052(2) Uani 0.198(10) 1 d G . P A 2 C48A C 0.2327(16) -0.0342(15) 0.3921(11) 0.0444(17) Uani 0.198(10) 1 d DG . P A 2 H48A H 0.283790 -0.069991 0.405332 0.053 Uiso 0.198(10) 1 calc R . P A 2 C49A C 0.2621(17) 0.0379(17) 0.3687(13) 0.0372(17) Uani 0.198(10) 1 d DG . P A 2 H49A H 0.333296 0.051255 0.366003 0.045 Uiso 0.198(10) 1 calc R . P A 2 C45 C 0.1070(6) 0.0406(5) 0.3576(4) 0.051(2) Uani 0.802(10) 1 d . . P A 1 H45 H 0.048445 0.063121 0.340373 0.062 Uiso 0.802(10) 1 calc R . P A 1 C46 C 0.0953(7) -0.0292(6) 0.3848(4) 0.070(3) Uani 0.802(10) 1 d . . P A 1 H46 H 0.030027 -0.055345 0.385730 0.084 Uiso 0.802(10) 1 calc R . P A 1 C47 C 0.1776(7) -0.0614(4) 0.4106(3) 0.052(2) Uani 0.802(10) 1 d . . P A 1 C48 C 0.2727(6) -0.0268(4) 0.4077(3) 0.0444(17) Uani 0.802(10) 1 d . . P A 1 H48 H 0.330394 -0.051465 0.424346 0.053 Uiso 0.802(10) 1 calc R . P A 1 C49 C 0.2849(6) 0.0445(5) 0.3803(3) 0.0372(17) Uani 0.802(10) 1 d . . P A 1 H49 H 0.351059 0.069316 0.379339 0.045 Uiso 0.802(10) 1 calc R . P A 1 C50 C 0.5390(3) 0.3273(3) 0.34595(17) 0.0292(9) Uani 1 1 d . . . . . H50A H 0.555275 0.350275 0.311168 0.035 Uiso 1 1 calc R . . . . H50B H 0.525970 0.372798 0.370138 0.035 Uiso 1 1 calc R . . . . C51 C 0.6311(3) 0.2806(3) 0.36543(17) 0.0303(10) Uani 1 1 d . . . . . C52 C 0.6779(4) 0.3011(3) 0.4130(2) 0.0424(12) Uani 1 1 d . . . . . H52 H 0.650135 0.343537 0.433497 0.051 Uiso 1 1 calc R . . . . C53 C 0.7646(5) 0.2600(4) 0.4305(3) 0.0566(16) Uani 1 1 d . . . . . H53 H 0.796827 0.274239 0.462663 0.068 Uiso 1 1 calc R . . . . C54 C 0.8032(4) 0.1981(4) 0.4005(3) 0.0567(16) Uani 1 1 d . . . . . C55 C 0.7566(4) 0.1755(4) 0.3544(2) 0.0538(15) Uani 1 1 d . . . . . H55 H 0.783271 0.131802 0.334577 0.065 Uiso 1 1 calc R . . . . C56 C 0.6705(4) 0.2169(3) 0.3371(2) 0.0409(12) Uani 1 1 d . . . . . H56 H 0.637866 0.201414 0.305233 0.049 Uiso 1 1 calc R . . . . Cl1 Cl 0.1612(4) -0.14952(16) 0.44671(12) 0.0881(11) Uani 0.802(10) 1 d . . P A 1 Cl1A Cl 0.092(2) -0.1454(7) 0.4150(12) 0.146(14) Uani 0.198(10) 1 d D . P A 2 Cl2 Cl 0.91403(12) 0.14677(13) 0.42033(11) 0.0991(8) Uani 1 1 d . . . . . Ir1 Ir 0.27973(2) 0.36413(2) 0.33525(2) 0.02535(6) Uani 1 1 d . . . . . H H 0.358988 0.439517 0.322706 0.068(19) Uiso 1 1 d R . . . . HA H 0.183988 0.428027 0.344966 0.047(15) Uiso 1 1 d R . . . . Ir2 Ir 0.33547(2) 0.27300(2) 0.42294(2) 0.02557(6) Uani 1 1 d . . . . . HB H 0.439088 0.324491 0.440569 0.10(2) Uiso 1 1 d R . . . . HC H 0.389488 0.193161 0.450159 0.08(2) Uiso 1 1 d R . . . . N1 N 0.3045(3) 0.3823(3) 0.21792(14) 0.0353(9) Uani 1 1 d . . . . . N2 N 0.1481(3) 0.4084(3) 0.24140(15) 0.0457(11) Uani 1 1 d . . . . . N3 N 0.1983(3) 0.3512(2) 0.50698(14) 0.0340(9) Uani 1 1 d . . . . . N4 N 0.2491(3) 0.2341(2) 0.53133(14) 0.0323(9) Uani 1 1 d . . . . . S1 S 0.18491(9) 0.24786(7) 0.36789(4) 0.0312(2) Uani 1 1 d D . . . . S2 S 0.42171(8) 0.26690(6) 0.34048(4) 0.0262(2) Uani 1 1 d . . . . . C57 C 0.4545(6) 0.5665(4) 0.3773(3) 0.070(2) Uani 1 1 d . . . . . H57A H 0.501637 0.540637 0.352511 0.105 Uiso 1 1 calc GR . . . . H57B H 0.441631 0.529931 0.406730 0.105 Uiso 1 1 calc GR . . . . H57C H 0.485733 0.616383 0.390393 0.105 Uiso 1 1 calc GR . . . . O1 O 0.3598(4) 0.5844(2) 0.35177(17) 0.0616(11) Uani 1 1 d . . . . . H1 H 0.331515 0.541376 0.341897 0.092 Uiso 1 1 calc GR . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C0AA 0.038(3) 0.032(2) 0.023(2) -0.0036(18) 0.0038(18) 0.007(2) C2 0.061(4) 0.097(5) 0.015(2) 0.003(3) -0.001(2) 0.036(4) C3 0.058(4) 0.126(6) 0.020(2) 0.001(3) -0.004(2) 0.045(4) C4 0.035(2) 0.042(3) 0.0139(19) 0.0009(18) 0.0048(17) 0.003(2) C5 0.038(2) 0.039(3) 0.0124(19) -0.0034(18) 0.0025(17) 0.004(2) C6 0.046(3) 0.049(3) 0.017(2) -0.006(2) 0.0022(19) 0.016(2) C7 0.032(3) 0.072(4) 0.018(2) -0.004(2) 0.0042(18) 0.004(3) C8 0.050(3) 0.058(3) 0.022(2) 0.002(2) 0.009(2) -0.015(3) C9 0.054(3) 0.045(3) 0.018(2) 0.005(2) 0.010(2) 0.000(2) C10 0.050(3) 0.047(3) 0.030(3) -0.010(2) 0.002(2) -0.005(2) C11 0.038(3) 0.122(6) 0.040(3) -0.014(4) 0.010(2) 0.011(4) C12 0.088(5) 0.038(3) 0.043(3) 0.001(3) 0.016(3) 0.000(3) C13 0.036(3) 0.055(3) 0.026(2) -0.005(2) 0.0011(19) 0.016(2) C14 0.039(3) 0.049(3) 0.033(3) 0.010(2) 0.004(2) 0.004(2) C15 0.044(3) 0.041(3) 0.042(3) 0.000(2) 0.006(2) 0.013(2) C16 0.032(3) 0.051(3) 0.042(3) -0.008(2) 0.005(2) 0.005(2) C17 0.033(3) 0.049(3) 0.055(3) -0.008(3) -0.004(2) -0.001(2) C18 0.033(3) 0.050(3) 0.047(3) -0.013(3) -0.011(2) 0.008(2) C19 0.056(4) 0.060(4) 0.076(4) 0.023(3) 0.024(3) 0.009(3) C20 0.041(3) 0.071(4) 0.077(4) -0.020(4) 0.018(3) 0.005(3) C21 0.049(3) 0.054(4) 0.098(5) -0.041(4) -0.024(3) 0.012(3) C22 0.033(2) 0.037(3) 0.017(2) -0.0007(18) 0.0056(17) 0.0025(19) C23 0.051(3) 0.047(3) 0.028(2) -0.003(2) 0.018(2) 0.009(2) C24 0.050(3) 0.050(3) 0.024(2) 0.002(2) 0.019(2) 0.000(2) C25 0.054(3) 0.033(3) 0.025(2) -0.0040(19) 0.014(2) 0.010(2) C26 0.065(4) 0.039(3) 0.033(3) -0.012(2) 0.020(2) 0.000(3) C27 0.083(5) 0.040(3) 0.058(4) -0.020(3) 0.035(3) -0.007(3) C28 0.079(4) 0.042(3) 0.050(3) -0.004(3) 0.024(3) 0.017(3) C29 0.068(4) 0.043(3) 0.039(3) -0.001(2) 0.016(3) 0.016(3) C30 0.056(3) 0.036(3) 0.033(3) -0.005(2) 0.019(2) 0.018(2) C31 0.059(4) 0.065(4) 0.053(4) -0.024(3) 0.017(3) -0.017(3) C32 0.143(8) 0.039(4) 0.096(6) 0.013(4) 0.050(5) 0.023(4) C33 0.047(3) 0.057(4) 0.043(3) -0.014(3) 0.005(2) 0.006(3) C34 0.044(3) 0.040(3) 0.015(2) 0.0013(18) 0.0099(18) 0.006(2) C35 0.041(3) 0.048(3) 0.014(2) 0.0067(19) 0.0035(18) -0.003(2) C36 0.038(3) 0.062(4) 0.023(2) 0.010(2) 0.0015(19) 0.007(2) C37 0.054(3) 0.046(3) 0.023(2) 0.007(2) 0.013(2) 0.007(3) C38 0.048(3) 0.041(3) 0.029(2) 0.007(2) 0.008(2) -0.003(2) C39 0.039(3) 0.042(3) 0.026(2) 0.003(2) 0.0088(19) -0.002(2) C40 0.051(3) 0.063(4) 0.028(3) 0.004(2) -0.005(2) -0.013(3) C41 0.065(4) 0.055(4) 0.041(3) 0.016(3) 0.016(3) 0.020(3) C42 0.034(3) 0.060(4) 0.059(4) 0.000(3) 0.005(2) -0.005(3) C43 0.047(3) 0.038(3) 0.031(3) -0.011(2) 0.010(2) -0.005(2) C43A 0.047(3) 0.038(3) 0.031(3) -0.011(2) 0.010(2) -0.005(2) C44 0.030(3) 0.031(3) 0.038(3) -0.014(2) 0.004(3) -0.003(3) C44A 0.030(3) 0.031(3) 0.038(3) -0.014(2) 0.004(3) -0.003(3) C45A 0.040(4) 0.050(5) 0.064(4) 0.018(4) -0.020(3) -0.013(4) C46A 0.065(6) 0.062(6) 0.081(6) 0.037(5) -0.038(5) -0.037(5) C47A 0.067(6) 0.035(4) 0.053(5) 0.000(3) -0.005(4) -0.010(4) C48A 0.041(4) 0.045(4) 0.047(4) -0.008(3) -0.005(3) 0.017(3) C49A 0.033(4) 0.035(3) 0.043(5) -0.015(3) 0.004(3) -0.003(3) C45 0.040(4) 0.050(5) 0.064(4) 0.018(4) -0.020(3) -0.013(4) C46 0.065(6) 0.062(6) 0.081(6) 0.037(5) -0.038(5) -0.037(5) C47 0.067(6) 0.035(4) 0.053(5) 0.000(3) -0.005(4) -0.010(4) C48 0.041(4) 0.045(4) 0.047(4) -0.008(3) -0.005(3) 0.017(3) C49 0.033(4) 0.035(3) 0.043(5) -0.015(3) 0.004(3) -0.003(3) C50 0.029(2) 0.033(2) 0.025(2) 0.0028(19) 0.0044(17) -0.0011(19) C51 0.024(2) 0.037(3) 0.030(2) 0.0038(19) 0.0076(18) -0.0038(19) C52 0.044(3) 0.041(3) 0.043(3) 0.000(2) -0.004(2) -0.006(2) C53 0.046(3) 0.057(4) 0.067(4) 0.009(3) -0.019(3) -0.012(3) C54 0.029(3) 0.062(4) 0.079(4) 0.029(3) -0.003(3) 0.002(3) C55 0.045(3) 0.055(4) 0.062(4) 0.002(3) 0.025(3) 0.011(3) C56 0.040(3) 0.050(3) 0.033(3) 0.000(2) 0.012(2) 0.004(2) Cl1 0.144(3) 0.0391(12) 0.0814(18) 0.0127(11) -0.0141(18) -0.0209(14) Cl1A 0.18(2) 0.042(6) 0.22(3) 0.015(9) 0.13(2) 0.001(8) Cl2 0.0342(8) 0.0941(14) 0.169(2) 0.0531(15) -0.0121(10) 0.0094(8) Ir1 0.03009(10) 0.02852(10) 0.01748(9) -0.00153(7) 0.00447(7) 0.00266(7) Ir2 0.03040(10) 0.02897(10) 0.01741(9) -0.00064(7) 0.00703(7) 0.00272(7) N1 0.040(2) 0.047(2) 0.0185(18) -0.0008(17) 0.0048(16) 0.0095(19) N2 0.039(2) 0.075(3) 0.023(2) -0.004(2) -0.0010(17) 0.020(2) N3 0.040(2) 0.039(2) 0.0231(19) -0.0042(16) 0.0117(16) 0.0049(18) N4 0.039(2) 0.037(2) 0.0209(18) -0.0001(16) 0.0101(16) 0.0032(17) S1 0.0317(6) 0.0349(6) 0.0271(5) -0.0067(5) 0.0081(4) -0.0026(5) S2 0.0285(5) 0.0318(6) 0.0182(5) -0.0005(4) 0.0075(4) 0.0008(4) C57 0.087(5) 0.056(4) 0.067(4) 0.001(3) -0.006(4) -0.033(4) O1 0.083(3) 0.043(2) 0.058(3) 0.001(2) 0.006(2) -0.008(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C0AA Ir1 1.969(4) . ? C0AA N1 1.379(6) . ? C0AA N2 1.380(6) . ? C2 C3 1.329(8) . ? C2 N1 1.383(6) . ? C3 N2 1.389(6) . ? C4 C5 1.390(6) . ? C4 C9 1.386(7) . ? C4 N1 1.436(6) . ? C5 C6 1.395(7) . ? C5 C10 1.510(7) . ? C6 C7 1.383(8) . ? C7 C8 1.388(8) . ? C7 C11 1.515(7) . ? C8 C9 1.398(7) . ? C9 C12 1.497(7) . ? C13 C14 1.390(7) . ? C13 C18 1.389(8) . ? C13 N2 1.446(6) . ? C14 C15 1.397(7) . ? C14 C19 1.498(8) . ? C15 C16 1.383(7) . ? C16 C17 1.376(8) . ? C16 C20 1.520(7) . ? C17 C18 1.396(7) . ? C18 C21 1.506(7) . ? C22 Ir2 2.036(4) . ? C22 N3 1.364(6) . ? C22 N4 1.359(6) . ? C23 C24 1.333(7) . ? C23 N3 1.386(6) . ? C24 N4 1.394(6) . ? C25 C26 1.386(8) . ? C25 C30 1.393(7) . ? C25 N3 1.439(6) . ? C26 C27 1.397(8) . ? C26 C31 1.516(8) . ? C27 C28 1.390(9) . ? C28 C29 1.362(9) . ? C28 C32 1.520(9) . ? C29 C30 1.375(7) . ? C30 C33 1.498(8) . ? C34 C35 1.393(7) . ? C34 C39 1.398(7) . ? C34 N4 1.435(6) . ? C35 C36 1.388(7) . ? C35 C40 1.504(7) . ? C36 C37 1.390(8) . ? C37 C38 1.377(7) . ? C37 C41 1.506(7) . ? C38 C39 1.388(7) . ? C39 C42 1.507(7) . ? C43 C44 1.476(8) . ? C43 S1 1.851(6) . ? C43A C44A 1.472(19) . ? C43A S1 1.851(17) . ? C44 C45 1.402(9) . ? C44 C49 1.395(9) . ? C44A C45A 1.3900 . ? C44A C49A 1.3900 . ? C45A C46A 1.3900 . ? C46A C47A 1.3900 . ? C47A C48A 1.3900 . ? C47A Cl1A 1.66(2) . ? C48A C49A 1.3900 . ? C45 C46 1.360(10) . ? C46 C47 1.358(11) . ? C47 C48 1.359(10) . ? C47 Cl1 1.743(8) . ? C48 C49 1.384(10) . ? C50 C51 1.504(6) . ? C50 S2 1.823(4) . ? C51 C52 1.396(7) . ? C51 C56 1.380(7) . ? C52 C53 1.384(8) . ? C53 C54 1.376(9) . ? C54 C55 1.374(9) . ? C54 Cl2 1.740(6) . ? C55 C56 1.379(8) . ? Ir1 Ir2 2.7941(3) . ? Ir1 S1 2.4357(12) . ? Ir1 S2 2.4478(11) . ? Ir2 S1 2.4321(11) . ? Ir2 S2 2.3896(9) . ? C57 O1 1.417(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C0AA Ir1 128.8(3) . . ? N1 C0AA N2 102.8(4) . . ? N2 C0AA Ir1 128.2(3) . . ? C3 C2 N1 107.4(4) . . ? C2 C3 N2 107.4(5) . . ? C5 C4 N1 118.7(4) . . ? C9 C4 C5 122.3(4) . . ? C9 C4 N1 118.7(4) . . ? C4 C5 C6 118.2(4) . . ? C4 C5 C10 121.3(4) . . ? C6 C5 C10 120.5(4) . . ? C7 C6 C5 121.4(5) . . ? C6 C7 C8 118.6(5) . . ? C6 C7 C11 120.1(6) . . ? C8 C7 C11 121.3(6) . . ? C7 C8 C9 121.9(5) . . ? C4 C9 C8 117.5(5) . . ? C4 C9 C12 121.6(5) . . ? C8 C9 C12 120.9(5) . . ? C14 C13 N2 117.0(5) . . ? C18 C13 C14 122.3(5) . . ? C18 C13 N2 120.5(5) . . ? C13 C14 C15 117.3(5) . . ? C13 C14 C19 121.8(5) . . ? C15 C14 C19 120.9(5) . . ? C16 C15 C14 122.1(5) . . ? C15 C16 C20 120.9(5) . . ? C17 C16 C15 118.5(5) . . ? C17 C16 C20 120.6(5) . . ? C16 C17 C18 121.8(5) . . ? C13 C18 C17 117.8(5) . . ? C13 C18 C21 121.6(5) . . ? C17 C18 C21 120.5(5) . . ? N3 C22 Ir2 128.6(3) . . ? N4 C22 Ir2 127.5(3) . . ? N4 C22 N3 103.9(3) . . ? C24 C23 N3 107.8(4) . . ? C23 C24 N4 106.1(4) . . ? C26 C25 C30 124.2(5) . . ? C26 C25 N3 117.5(5) . . ? C30 C25 N3 118.2(5) . . ? C25 C26 C27 115.8(6) . . ? C25 C26 C31 122.0(5) . . ? C27 C26 C31 122.2(6) . . ? C28 C27 C26 121.5(6) . . ? C27 C28 C32 118.5(7) . . ? C29 C28 C27 119.6(6) . . ? C29 C28 C32 121.8(7) . . ? C28 C29 C30 122.0(6) . . ? C25 C30 C33 122.9(5) . . ? C29 C30 C25 116.9(5) . . ? C29 C30 C33 120.2(5) . . ? C35 C34 C39 121.9(5) . . ? C35 C34 N4 118.8(4) . . ? C39 C34 N4 119.1(4) . . ? C34 C35 C40 122.1(5) . . ? C36 C35 C34 117.3(5) . . ? C36 C35 C40 120.6(5) . . ? C35 C36 C37 122.5(5) . . ? C36 C37 C41 120.0(5) . . ? C38 C37 C36 118.2(5) . . ? C38 C37 C41 121.8(5) . . ? C37 C38 C39 121.9(5) . . ? C34 C39 C42 120.6(5) . . ? C38 C39 C34 118.1(5) . . ? C38 C39 C42 121.3(5) . . ? C44 C43 S1 114.5(6) . . ? C44A C43A S1 106(2) . . ? C45 C44 C43 121.9(6) . . ? C49 C44 C43 122.2(6) . . ? C49 C44 C45 115.9(6) . . ? C45A C44A C43A 120.0(8) . . ? C45A C44A C49A 120.0 . . ? C49A C44A C43A 119.9(8) . . ? C44A C45A C46A 120.0 . . ? C45A C46A C47A 120.0 . . ? C46A C47A Cl1A 118.7(8) . . ? C48A C47A C46A 120.0 . . ? C48A C47A Cl1A 120.6(7) . . ? C49A C48A C47A 120.0 . . ? C48A C49A C44A 120.0 . . ? C46 C45 C44 122.4(7) . . ? C47 C46 C45 119.6(7) . . ? C46 C47 C48 121.0(7) . . ? C46 C47 Cl1 119.3(6) . . ? C48 C47 Cl1 119.7(6) . . ? C47 C48 C49 119.6(6) . . ? C48 C49 C44 121.4(6) . . ? C51 C50 S2 113.5(3) . . ? C52 C51 C50 120.1(4) . . ? C56 C51 C50 121.0(4) . . ? C56 C51 C52 118.8(5) . . ? C53 C52 C51 120.5(5) . . ? C54 C53 C52 119.0(6) . . ? C53 C54 Cl2 120.4(5) . . ? C55 C54 C53 121.4(5) . . ? C55 C54 Cl2 118.2(5) . . ? C54 C55 C56 119.3(5) . . ? C55 C56 C51 120.9(5) . . ? C0AA Ir1 Ir2 156.63(13) . . ? C0AA Ir1 S1 109.70(14) . . ? C0AA Ir1 S2 110.11(13) . . ? S1 Ir1 Ir2 54.91(3) . . ? S1 Ir1 S2 80.65(4) . . ? S2 Ir1 Ir2 53.75(2) . . ? C22 Ir2 Ir1 119.43(13) . . ? C22 Ir2 S1 95.96(13) . . ? C22 Ir2 S2 175.02(13) . . ? S1 Ir2 Ir1 55.03(3) . . ? S2 Ir2 Ir1 55.70(3) . . ? S2 Ir2 S1 81.90(4) . . ? C0AA N1 C2 111.4(4) . . ? C0AA N1 C4 126.8(4) . . ? C2 N1 C4 121.8(4) . . ? C0AA N2 C3 111.0(4) . . ? C0AA N2 C13 128.1(4) . . ? C3 N2 C13 120.6(4) . . ? C22 N3 C23 110.7(4) . . ? C22 N3 C25 128.4(4) . . ? C23 N3 C25 120.8(4) . . ? C22 N4 C24 111.5(4) . . ? C22 N4 C34 128.4(4) . . ? C24 N4 C34 120.0(4) . . ? C43 S1 Ir1 109.9(3) . . ? C43 S1 Ir2 108.0(4) . . ? C43A S1 Ir1 104.8(9) . . ? C43A S1 Ir2 107.3(15) . . ? Ir2 S1 Ir1 70.06(3) . . ? C50 S2 Ir1 105.35(15) . . ? C50 S2 Ir2 107.50(14) . . ? Ir2 S2 Ir1 70.55(3) . . ? _shelx_res_file ; TITL sbd1906_a.res in P2(1)/c sbd1906.res created by SHELXL-2018/3 at 12:17:47 on 30-Sep-2019 REM Old TITL sbd1906 in P21/c #14 REM SHELXT solution in P2(1)/c: R1 0.097, Rweak 0.005, Alpha 0.061 REM 0.535 for 379 systematic absences, Orientation as input REM Formula found by SHELXT: C55 N6 O S4 Ir2 CELL 1.54184 12.931718 16.59997 25.536489 90 90.2757 90 ZERR 4 0.000199 0.0003 0.000382 0 0.0013 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl Ir N O S UNIT 228 272 8 8 16 4 8 SADI C46A Cl1A Cl1A C48A SADI C43A C44A C44 C43 SADI S1 C43 S1 C43A SADI C49A C43A C43A C45A EADP C49A C49 EADP C48 C48A EADP C47A C47 EADP C46A C46 EADP C45A C45 EADP C44A C44 EADP C43A C43 L.S. 14 0 0 PLAN 40 SIZE 0.078 0.09 0.149 TEMP -163.15(10) BOND list 4 fmap 2 53 acta REM REM REM WGHT 0.026500 13.104500 FVAR 1.79572 0.80236 C0AA 1 0.242171 0.383941 0.261557 11.00000 0.03806 0.03150 = 0.02342 -0.00365 0.00379 0.00658 C2 1 0.250746 0.405428 0.173440 11.00000 0.06144 0.09683 = 0.01549 0.00252 -0.00061 0.03553 AFIX 43 H2 2 0.277677 0.408767 0.138962 11.00000 -1.20000 AFIX 0 C3 1 0.154435 0.422098 0.187839 11.00000 0.05793 0.12598 = 0.02050 0.00114 -0.00414 0.04507 AFIX 43 H3 2 0.100011 0.440039 0.165607 11.00000 -1.20000 AFIX 0 C4 1 0.412441 0.362300 0.216379 11.00000 0.03546 0.04178 = 0.01393 0.00095 0.00481 0.00295 C5 1 0.440552 0.282167 0.209703 11.00000 0.03817 0.03891 = 0.01240 -0.00344 0.00248 0.00377 C6 1 0.545374 0.264032 0.204756 11.00000 0.04638 0.04852 = 0.01669 -0.00627 0.00224 0.01589 AFIX 43 H6 2 0.566074 0.209398 0.201231 11.00000 -1.20000 AFIX 0 C7 1 0.619811 0.323821 0.204872 11.00000 0.03241 0.07214 = 0.01804 -0.00424 0.00421 0.00398 C8 1 0.588461 0.403282 0.210751 11.00000 0.04954 0.05771 = 0.02213 0.00203 0.00874 -0.01516 AFIX 43 H8 2 0.639251 0.444629 0.211150 11.00000 -1.20000 AFIX 0 C9 1 0.484312 0.424241 0.216103 11.00000 0.05358 0.04494 = 0.01789 0.00471 0.00977 -0.00007 C10 1 0.360244 0.216263 0.206445 11.00000 0.05025 0.04731 = 0.02984 -0.01018 0.00170 -0.00454 AFIX 137 H10A 2 0.330470 0.214991 0.171092 11.00000 -1.50000 H10B 2 0.305451 0.226797 0.231924 11.00000 -1.50000 H10C 2 0.392706 0.164243 0.214207 11.00000 -1.50000 AFIX 0 C11 1 0.732922 0.302179 0.198594 11.00000 0.03834 0.12212 = 0.04014 -0.01364 0.00989 0.01077 AFIX 137 H11A 2 0.751220 0.259435 0.223435 11.00000 -1.50000 H11B 2 0.775646 0.349802 0.205504 11.00000 -1.50000 H11C 2 0.745045 0.283305 0.162783 11.00000 -1.50000 AFIX 0 C12 1 0.452354 0.510495 0.221625 11.00000 0.08760 0.03836 = 0.04324 0.00133 0.01586 0.00024 AFIX 137 H12A 2 0.402020 0.523950 0.194178 11.00000 -1.50000 H12B 2 0.513179 0.545289 0.218247 11.00000 -1.50000 H12C 2 0.420941 0.518706 0.256062 11.00000 -1.50000 AFIX 0 C13 1 0.054703 0.427839 0.269645 11.00000 0.03626 0.05515 = 0.02579 -0.00473 0.00109 0.01572 C14 1 0.037262 0.508678 0.280725 11.00000 0.03868 0.04893 = 0.03290 0.01012 0.00423 0.00444 C15 1 -0.058228 0.529077 0.302383 11.00000 0.04375 0.04127 = 0.04214 -0.00031 0.00611 0.01322 AFIX 43 H15 2 -0.072782 0.584114 0.309394 11.00000 -1.20000 AFIX 0 C16 1 -0.132254 0.471708 0.313945 11.00000 0.03155 0.05128 = 0.04242 -0.00775 0.00455 0.00490 C17 1 -0.110433 0.392110 0.303744 11.00000 0.03345 0.04858 = 0.05497 -0.00760 -0.00385 -0.00105 AFIX 43 H17 2 -0.159562 0.352089 0.313015 11.00000 -1.20000 AFIX 0 C18 1 -0.018105 0.368569 0.280151 11.00000 0.03306 0.04987 = 0.04689 -0.01287 -0.01070 0.00784 C19 1 0.117443 0.571757 0.270473 11.00000 0.05558 0.05952 = 0.07560 0.02251 0.02414 0.00862 AFIX 137 H19A 2 0.136531 0.570623 0.233387 11.00000 -1.50000 H19B 2 0.178760 0.561008 0.292065 11.00000 -1.50000 H19C 2 0.089508 0.624920 0.279257 11.00000 -1.50000 AFIX 0 C20 1 -0.235034 0.495734 0.338024 11.00000 0.04062 0.07068 = 0.07746 -0.01986 0.01775 0.00497 AFIX 137 H20A 2 -0.233793 0.483891 0.375618 11.00000 -1.50000 H20B 2 -0.291023 0.465275 0.321248 11.00000 -1.50000 H20C 2 -0.246536 0.553520 0.332726 11.00000 -1.50000 AFIX 0 C21 1 -0.000039 0.281744 0.265733 11.00000 0.04869 0.05428 = 0.09822 -0.04097 -0.02384 0.01228 AFIX 137 H21A 2 -0.030376 0.270932 0.231201 11.00000 -1.50000 H21B 2 -0.032440 0.246763 0.291854 11.00000 -1.50000 H21C 2 0.074454 0.271042 0.264763 11.00000 -1.50000 AFIX 0 C22 1 0.255598 0.286909 0.490851 11.00000 0.03313 0.03715 = 0.01731 -0.00074 0.00564 0.00255 C23 1 0.157626 0.337342 0.556260 11.00000 0.05088 0.04728 = 0.02783 -0.00271 0.01850 0.00889 AFIX 43 H23 2 0.115030 0.373239 0.575500 11.00000 -1.20000 AFIX 0 C24 1 0.188882 0.264633 0.571861 11.00000 0.05011 0.04986 = 0.02360 0.00236 0.01887 0.00045 AFIX 43 H24 2 0.173285 0.238867 0.604088 11.00000 -1.20000 AFIX 0 C25 1 0.181779 0.426837 0.480696 11.00000 0.05396 0.03256 = 0.02511 -0.00400 0.01421 0.01043 C26 1 0.255951 0.486232 0.487376 11.00000 0.06469 0.03851 = 0.03328 -0.01246 0.02048 0.00042 C27 1 0.235167 0.559728 0.462852 11.00000 0.08260 0.03965 = 0.05810 -0.01969 0.03460 -0.00727 AFIX 43 H27 2 0.283280 0.602659 0.466369 11.00000 -1.20000 AFIX 0 C28 1 0.145737 0.571521 0.433424 11.00000 0.07938 0.04228 = 0.05002 -0.00425 0.02445 0.01720 C29 1 0.075648 0.510700 0.428771 11.00000 0.06838 0.04274 = 0.03948 -0.00100 0.01570 0.01646 AFIX 43 H29 2 0.014352 0.519570 0.408943 11.00000 -1.20000 AFIX 0 C30 1 0.090921 0.436807 0.451914 11.00000 0.05557 0.03625 = 0.03333 -0.00518 0.01894 0.01813 C31 1 0.353845 0.471920 0.518915 11.00000 0.05897 0.06545 = 0.05269 -0.02440 0.01671 -0.01675 AFIX 137 H31A 2 0.335789 0.450978 0.553567 11.00000 -1.50000 H31B 2 0.391540 0.522790 0.522863 11.00000 -1.50000 H31C 2 0.397494 0.432740 0.500704 11.00000 -1.50000 AFIX 0 C32 1 0.128264 0.653244 0.408074 11.00000 0.14277 0.03901 = 0.09550 0.01310 0.04958 0.02266 AFIX 137 H32A 2 0.089472 0.646320 0.375320 11.00000 -1.50000 H32B 2 0.195162 0.678399 0.400638 11.00000 -1.50000 H32C 2 0.088889 0.687719 0.431914 11.00000 -1.50000 AFIX 0 C33 1 0.011872 0.371466 0.445696 11.00000 0.04702 0.05725 = 0.04326 -0.01448 0.00525 0.00637 AFIX 137 H33A 2 0.044672 0.323458 0.430845 11.00000 -1.50000 H33B 2 -0.043384 0.389946 0.422206 11.00000 -1.50000 H33C 2 -0.017375 0.358259 0.479971 11.00000 -1.50000 AFIX 0 C34 1 0.297507 0.156730 0.536635 11.00000 0.04386 0.03985 = 0.01536 0.00130 0.00994 0.00606 C35 1 0.398006 0.152859 0.556310 11.00000 0.04113 0.04849 = 0.01424 0.00669 0.00346 -0.00330 C36 1 0.439207 0.076880 0.565395 11.00000 0.03776 0.06246 = 0.02253 0.00995 0.00150 0.00668 AFIX 43 H36 2 0.507100 0.072824 0.579524 11.00000 -1.20000 AFIX 0 C37 1 0.384862 0.006504 0.554597 11.00000 0.05428 0.04596 = 0.02269 0.00732 0.01288 0.00710 C38 1 0.285457 0.013157 0.535508 11.00000 0.04764 0.04074 = 0.02861 0.00666 0.00781 -0.00341 AFIX 43 H38 2 0.247003 -0.034488 0.528664 11.00000 -1.20000 AFIX 0 C39 1 0.239795 0.087414 0.525971 11.00000 0.03943 0.04230 = 0.02620 0.00343 0.00876 -0.00217 C40 1 0.460429 0.227269 0.567816 11.00000 0.05096 0.06280 = 0.02757 0.00379 -0.00507 -0.01349 AFIX 137 H40A 2 0.490103 0.247913 0.535225 11.00000 -1.50000 H40B 2 0.516238 0.213974 0.592433 11.00000 -1.50000 H40C 2 0.415625 0.268410 0.583286 11.00000 -1.50000 AFIX 0 C41 1 0.434981 -0.074209 0.563753 11.00000 0.06547 0.05452 = 0.04085 0.01575 0.01627 0.01985 AFIX 137 H41A 2 0.502317 -0.075614 0.546333 11.00000 -1.50000 H41B 2 0.390628 -0.116805 0.549447 11.00000 -1.50000 H41C 2 0.444611 -0.082727 0.601437 11.00000 -1.50000 AFIX 0 C42 1 0.131207 0.093717 0.504696 11.00000 0.03435 0.05998 = 0.05925 -0.00011 0.00514 -0.00539 AFIX 137 H42A 2 0.088956 0.125724 0.528719 11.00000 -1.50000 H42B 2 0.101487 0.039661 0.501232 11.00000 -1.50000 H42C 2 0.132556 0.119865 0.470299 11.00000 -1.50000 AFIX 0 PART 1 C43 1 0.212579 0.158642 0.326788 21.00000 0.04720 0.03754 = 0.03072 -0.01082 0.00982 -0.00546 AFIX 23 H43A 2 0.164998 0.159028 0.296303 21.00000 -1.20000 H43B 2 0.283955 0.163214 0.313262 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C43A 1 0.218743 0.164941 0.322659 -21.00000 0.04720 0.03754 = 0.03072 -0.01082 0.00982 -0.00546 AFIX 23 H43C 2 0.181325 0.170914 0.288969 -21.00000 -1.20000 H43D 2 0.293987 0.164602 0.315697 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C44 1 0.202151 0.080725 0.354115 21.00000 0.02953 0.03093 = 0.03828 -0.01401 0.00382 -0.00326 PART 0 PART 2 AFIX 66 C44A 1 0.187342 0.090279 0.349348 -21.00000 0.02953 0.03093 = 0.03828 -0.01401 0.00382 -0.00326 C45A 1 0.083176 0.070676 0.353333 -21.00000 0.04019 0.04987 = 0.06400 0.01830 -0.01982 -0.01320 AFIX 43 H45A 2 0.032081 0.106502 0.340089 -21.00000 -1.20000 AFIX 65 C46A 1 0.053770 -0.001346 0.376695 -21.00000 0.06537 0.06226 = 0.08103 0.03669 -0.03824 -0.03661 AFIX 43 H46A 2 -0.017423 -0.014744 0.379419 -21.00000 -1.20000 AFIX 65 C47A 1 0.128529 -0.053766 0.396073 -21.00000 0.06705 0.03531 = 0.05342 -0.00030 -0.00514 -0.00980 C48A 1 0.232695 -0.034164 0.392089 -21.00000 0.04072 0.04522 = 0.04733 -0.00818 -0.00491 0.01683 AFIX 43 H48A 2 0.283790 -0.069991 0.405332 -21.00000 -1.20000 AFIX 65 C49A 1 0.262103 0.037858 0.368727 -21.00000 0.03287 0.03545 = 0.04344 -0.01550 0.00389 -0.00279 AFIX 43 H49A 2 0.333296 0.051255 0.366003 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C45 1 0.106962 0.040649 0.357617 21.00000 0.04019 0.04987 = 0.06400 0.01830 -0.01982 -0.01320 AFIX 43 H45 2 0.048445 0.063121 0.340373 21.00000 -1.20000 AFIX 0 C46 1 0.095342 -0.029203 0.384793 21.00000 0.06537 0.06226 = 0.08103 0.03669 -0.03824 -0.03661 AFIX 43 H46 2 0.030027 -0.055345 0.385730 21.00000 -1.20000 AFIX 0 C47 1 0.177624 -0.061379 0.410582 21.00000 0.06705 0.03531 = 0.05342 -0.00030 -0.00514 -0.00980 C48 1 0.272669 -0.026825 0.407684 21.00000 0.04072 0.04522 = 0.04733 -0.00818 -0.00491 0.01683 AFIX 43 H48 2 0.330394 -0.051465 0.424346 21.00000 -1.20000 AFIX 0 C49 1 0.284901 0.044498 0.380311 21.00000 0.03287 0.03545 = 0.04344 -0.01550 0.00389 -0.00279 AFIX 43 H49 2 0.351059 0.069316 0.379339 21.00000 -1.20000 AFIX 0 PART 0 C50 1 0.538987 0.327343 0.345952 11.00000 0.02938 0.03341 = 0.02471 0.00278 0.00444 -0.00112 AFIX 23 H50A 2 0.555275 0.350275 0.311168 11.00000 -1.20000 H50B 2 0.525970 0.372798 0.370138 11.00000 -1.20000 AFIX 0 C51 1 0.631091 0.280645 0.365428 11.00000 0.02418 0.03679 = 0.02997 0.00383 0.00758 -0.00380 C52 1 0.677946 0.301071 0.412983 11.00000 0.04355 0.04111 = 0.04254 -0.00018 -0.00369 -0.00633 AFIX 43 H52 2 0.650135 0.343537 0.433497 11.00000 -1.20000 AFIX 0 C53 1 0.764566 0.259960 0.430476 11.00000 0.04605 0.05662 = 0.06691 0.00931 -0.01930 -0.01215 AFIX 43 H53 2 0.796827 0.274239 0.462663 11.00000 -1.20000 AFIX 0 C54 1 0.803239 0.198106 0.400547 11.00000 0.02932 0.06220 = 0.07865 0.02899 -0.00263 0.00226 C55 1 0.756551 0.175492 0.354368 11.00000 0.04515 0.05478 = 0.06179 0.00204 0.02458 0.01083 AFIX 43 H55 2 0.783271 0.131802 0.334577 11.00000 -1.20000 AFIX 0 C56 1 0.670487 0.216929 0.337082 11.00000 0.03966 0.05041 = 0.03276 0.00031 0.01231 0.00443 AFIX 43 H56 2 0.637866 0.201414 0.305233 11.00000 -1.20000 AFIX 0 PART 1 CL1 3 0.161158 -0.149518 0.446705 21.00000 0.14361 0.03912 = 0.08141 0.01273 -0.01405 -0.02092 PART 0 PART 2 CL1A 3 0.092437 -0.145380 0.415028 -21.00000 0.18092 0.04228 = 0.21526 0.01486 0.13030 0.00104 PART 0 CL2 3 0.914031 0.146767 0.420326 11.00000 0.03419 0.09410 = 0.16903 0.05310 -0.01211 0.00945 IR1 4 0.279728 0.364127 0.335246 11.00000 0.03009 0.02852 = 0.01748 -0.00153 0.00447 0.00266 AFIX 3 1.6500 H 2 0.358988 0.439517 0.322706 11.00000 0.06807 HA 2 0.183988 0.428027 0.344966 11.00000 0.04671 AFIX 0 IR2 4 0.335468 0.273001 0.422939 11.00000 0.03040 0.02897 = 0.01741 -0.00064 0.00703 0.00272 AFIX 3 1.6500 HB 2 0.439088 0.324491 0.440569 11.00000 0.09803 HC 2 0.389488 0.193161 0.450159 11.00000 0.07875 AFIX 0 N1 5 0.304491 0.382328 0.217916 11.00000 0.04021 0.04721 = 0.01853 -0.00079 0.00481 0.00947 N2 5 0.148074 0.408439 0.241399 11.00000 0.03936 0.07479 = 0.02295 -0.00362 -0.00103 0.02009 N3 5 0.198341 0.351234 0.506976 11.00000 0.04032 0.03862 = 0.02308 -0.00422 0.01174 0.00491 N4 5 0.249067 0.234072 0.531328 11.00000 0.03899 0.03722 = 0.02090 -0.00014 0.01011 0.00322 S1 7 0.184912 0.247862 0.367885 11.00000 0.03171 0.03489 = 0.02707 -0.00666 0.00808 -0.00260 S2 7 0.421708 0.266898 0.340482 11.00000 0.02850 0.03184 = 0.01823 -0.00048 0.00745 0.00083 C57 1 0.454492 0.566451 0.377320 11.00000 0.08655 0.05630 = 0.06657 0.00073 -0.00555 -0.03285 AFIX 137 H57A 2 0.501637 0.540637 0.352511 11.00000 -1.50000 H57B 2 0.441631 0.529931 0.406730 11.00000 -1.50000 H57C 2 0.485733 0.616383 0.390393 11.00000 -1.50000 AFIX 0 O1 6 0.359755 0.584381 0.351766 11.00000 0.08331 0.04323 = 0.05829 0.00117 0.00625 -0.00821 AFIX 147 H1 2 0.331515 0.541376 0.341897 11.00000 -1.50000 AFIX 0 HKLF 4 REM sbd1906_a.res in P2(1)/c REM wR2 = 0.0712, GooF = S = 1.036, Restrained GooF = 1.036 for all data REM R1 = 0.0299 for 8700 Fo > 4sig(Fo) and 0.0357 for all 9782 data REM 650 parameters refined using 4 restraints END WGHT 0.0265 13.0995 REM Highest difference peak 1.916, deepest hole -1.357, 1-sigma level 0.098 Q1 1 0.3600 0.3174 0.4332 11.00000 0.05 1.92 Q2 1 0.2899 0.4179 0.3409 11.00000 0.05 1.55 Q3 1 0.9024 0.1395 0.4582 11.00000 0.05 0.93 Q4 1 0.3316 0.1970 0.4216 11.00000 0.05 0.73 Q5 1 0.3806 0.4921 0.3379 11.00000 0.05 0.68 Q6 1 0.2851 0.3795 0.4049 11.00000 0.05 0.67 Q7 1 0.9076 0.1032 0.4005 11.00000 0.05 0.58 Q8 1 0.2170 0.3014 0.3545 11.00000 0.05 0.56 Q9 1 0.2324 -0.1481 0.4396 11.00000 0.05 0.54 Q10 1 0.3346 0.3791 0.4013 11.00000 0.05 0.52 Q11 1 0.2996 0.3012 0.3394 11.00000 0.05 0.44 Q12 1 0.3361 0.4455 0.4201 11.00000 0.05 0.43 Q13 1 0.1346 0.0464 0.3175 11.00000 0.05 0.43 Q14 1 0.3280 0.1496 0.4353 11.00000 0.05 0.41 Q15 1 0.2593 0.3181 0.4253 11.00000 0.05 0.41 Q16 1 0.2580 0.2179 0.4260 11.00000 0.05 0.41 Q17 1 0.4581 0.3041 0.3542 11.00000 0.05 0.38 Q18 1 0.4216 0.2366 0.4210 11.00000 0.05 0.38 Q19 1 0.2745 0.1788 0.3255 11.00000 0.05 0.38 Q20 1 0.9277 0.1687 0.4216 11.00000 0.05 0.37 Q21 1 0.2807 0.3789 0.2397 11.00000 0.05 0.37 Q22 1 0.3076 0.5782 0.4751 11.00000 0.05 0.37 Q23 1 0.2076 0.5933 0.4381 11.00000 0.05 0.37 Q24 1 0.3902 0.1825 0.5178 11.00000 0.05 0.37 Q25 1 0.2094 0.6774 0.4124 11.00000 0.05 0.35 Q26 1 0.2075 0.3545 0.4053 11.00000 0.05 0.35 Q27 1 0.1403 0.3318 0.2764 11.00000 0.05 0.35 Q28 1 0.2253 0.4548 0.2456 11.00000 0.05 0.34 Q29 1 0.4140 0.2383 0.4565 11.00000 0.05 0.34 Q30 1 0.2368 0.3169 0.2982 11.00000 0.05 0.33 Q31 1 0.2618 0.1594 0.4044 11.00000 0.05 0.33 Q32 1 0.1529 0.3616 0.1921 11.00000 0.05 0.32 Q33 1 0.3202 0.7168 0.4168 11.00000 0.05 0.32 Q34 1 0.4437 0.5570 0.2006 11.00000 0.05 0.31 Q35 1 0.1184 -0.0169 0.3541 11.00000 0.05 0.31 Q36 1 0.1035 -0.0342 0.3261 11.00000 0.05 0.31 Q37 1 0.1333 0.3478 0.3780 11.00000 0.05 0.30 Q38 1 0.2645 0.2675 0.3975 11.00000 0.05 0.30 Q39 1 0.2631 0.3399 0.4984 11.00000 0.05 0.30 Q40 1 0.0623 0.1981 0.3374 11.00000 0.05 0.30 ; _shelx_res_checksum 89407 _olex2_date_sample_data_collection 2019-09-20 _olex2_date_sample_submission 2019-09-19 _olex2_exptl_crystal_mounting_method 'oil on 200 micrometre micromount' _olex2_submission_original_sample_id 'BT Ma1' _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.277 _oxdiff_exptl_absorpt_empirical_full_min 0.810 _vrf_PLAT415_sbd1906 ; PROBLEM: Short Inter D-H..H-X H ..H1 . 1.80 Ang. RESPONSE: The short-contact would correspond to a dihydrogen bond between the electronegative hydride and the protic hydrogen of the methanol. Note that whilst there was evidence of the positions of both hydrogens in the difference map, they were modelled using a riding model otherwise their positions changed to unfeasible positions due to the minor unresolved twinning. see e.g. DOI: 10.1021/acs.chemrev.6b00091 ;