#------------------------------------------------------------------------------ #$Date: 2020-01-29 03:45:47 +0200 (Wed, 29 Jan 2020) $ #$Revision: 247329 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/71/1557173.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1557173 loop_ _publ_author_name 'Tickner, Ben. J.' 'Semenova, Olga' 'Iali, Wissam' 'Rayner, Peter J.' 'Whitwood, Adrian C.' 'Duckett, Simon B.' _publ_section_title ; Optimisation of pyruvate hyperpolarisation using SABRE by tuning the active magnetisation transfer catalyst ; _journal_name_full 'Catalysis Science & Technology' _journal_paper_doi 10.1039/C9CY02498K _journal_year 2020 _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 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2019-09-17 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-10-04 deposited with the CCDC. 2019-12-10 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 94.4442(7) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 17.31801(12) _cell_length_b 12.99024(10) _cell_length_c 19.71788(16) _cell_measurement_reflns_used 9261 _cell_measurement_temperature 110.00(10) _cell_measurement_theta_max 71.0080 _cell_measurement_theta_min 4.9940 _cell_volume 4422.50(6) _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)' _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_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_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _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_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.489 _exptl_crystal_description plate _exptl_crystal_F_000 1996.4 _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 _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_restrained_S_all 1.047 _refine_ls_R_factor_all 0.0237 _refine_ls_R_factor_gt 0.0199 _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 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7174 _reflns_number_total 7896 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cy02498k2.cif _cod_data_source_block sbd1905 _cod_database_code 1557173 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C54.3 H49.1 Ir1 O0.3 P3' _chemical_oxdiff_usercomment 'Ben Tickner PPh3' _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. ; _reflns_odcompleteness_completeness 99.95 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _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) ; _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 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' 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_occupancy 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) 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' 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 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle 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_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance 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_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 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) 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