#------------------------------------------------------------------------------ #$Date: 2025-01-10 01:44:43 +0200 (Fri, 10 Jan 2025) $ #$Revision: 297249 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/36/1573648.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_1573648 _journal_paper_doi 10.1039/D4DT03036B _chemical_formula_moiety 'C15 H22 Au O P' _chemical_formula_sum 'C15 H22 Au O P' _chemical_formula_weight 446.26 _space_group_crystal_system orthorhombic _space_group_IT_number 29 _space_group_name_Hall 'P -2a -2ab' _space_group_name_H-M_alt 'P b 21 a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2024-05-06 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _audit_update_record ; 2024-07-24 deposited with the CCDC. 2025-01-09 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 16.7860(17) _cell_length_b 9.80510(19) _cell_length_c 16.5696(3) _cell_measurement_reflns_used 2492 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 20.9350 _cell_measurement_theta_min 1.9830 _cell_volume 2727.2(3) _computing_cell_refinement 'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)' _computing_data_collection 'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)' _computing_data_reduction 'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _diffrn_ambient_environment 'Diamond Anvil Cell filled with daphne-7575' _diffrn_ambient_pressure 2160000 _diffrn_ambient_temperature 293(2) _diffrn_crystal_treatment 'pressurized rapidly in daphne-7575 as a hydrostatic medium' _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 13.3333 _diffrn_measured_fraction_theta_full 0.612 _diffrn_measured_fraction_theta_max 0.408 _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 -39.00 39.00 0.50 1.00 -- 0.00 0.00 0.00 156 ; _diffrn_measurement_device 'abstract diffractometer' _diffrn_measurement_device_type 'esperanto-CrysAlisPro-abstract goniometer imported esperanto images' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'Diamond Anvil Cell, effective opening angle 39 deg.' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0237562084 _diffrn_orient_matrix_UB_12 0.0047854847 _diffrn_orient_matrix_UB_13 -0.0049379604 _diffrn_orient_matrix_UB_21 0.0056189609 _diffrn_orient_matrix_UB_22 0.0198865722 _diffrn_orient_matrix_UB_23 -0.0210250714 _diffrn_orient_matrix_UB_31 -0.0000529571 _diffrn_orient_matrix_UB_32 -0.0364789634 _diffrn_orient_matrix_UB_33 -0.0120952900 _diffrn_radiation_monochromator synchrotron _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.410 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_unetI/netI 0.0908 _diffrn_reflns_Laue_measured_fraction_full 0.612 _diffrn_reflns_Laue_measured_fraction_max 0.408 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 9573 _diffrn_reflns_point_group_measured_fraction_full 0.566 _diffrn_reflns_point_group_measured_fraction_max 0.346 _diffrn_reflns_theta_full 14.241 _diffrn_reflns_theta_max 21.667 _diffrn_reflns_theta_min 1.974 _diffrn_source synchrotron _exptl_absorpt_coefficient_mu 2.650 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.80278 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 2.174 _exptl_crystal_description needle _exptl_crystal_F_000 1712 _exptl_crystal_preparation 'Mounted in a Diamond-Anvil Cell using daphne-7575 as pressure medium.,Luminescent' _exptl_crystal_pressure_history 'Pressurized to 2.16 GPa and left to stabilize over ? hours.' _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: n-pentane/dichloromethane' _exptl_crystal_size_max 0.002 _exptl_crystal_size_mid 0.002 _exptl_crystal_size_min 0.001 _refine_diff_density_max 1.672 _refine_diff_density_min -1.079 _refine_diff_density_rms 0.169 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.58(6) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 334 _refine_ls_number_reflns 5763 _refine_ls_number_restraints 49 _refine_ls_restrained_S_all 1.055 _refine_ls_R_factor_all 0.0721 _refine_ls_R_factor_gt 0.0488 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+2.2345P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1240 _refine_ls_wR_factor_ref 0.1351 _reflns_Friedel_coverage 0.626 _reflns_Friedel_fraction_full 0.515 _reflns_Friedel_fraction_max 0.278 _reflns_number_gt 3940 _reflns_number_total 5763 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4dt03036b3.cif _cod_data_source_block 0011_2p16GPa _cod_database_code 1573648 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C15 H22 O P Au' _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. ; _diffrn_orient_matrix_axis[1] matrixX _diffrn_orient_matrix_axis[2] matrixY _diffrn_orient_matrix_axis[3] matrixZ _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.42(6) 0.58(6) 2. 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 3. Uiso/Uaniso restraints and constraints P2 \\sim C34 \\sim C35: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A C23 \\sim C28 \\sim C27 \\sim C26 \\sim C25 \\sim C24: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.7A 4.a Secondary CH2 refined with riding coordinates: C10(H10A,H10B), C30(H30A,H30B), C32(H32A,H32B), C12(H12A,H12B), C14(H14A, H14B), C34(H34A,H34B) 4.b Aromatic/amide H refined with riding coordinates: C27(H27), C24(H24), C28(H28), C25(H25), C7(H7), C8(H8), C4(H4), C5(H5) 4.c Idealised Me refined as rotating group: C11(H11A,H11B,H11C), C31(H31A,H31B,H31C), C9(H9A,H9B,H9C), C35(H35A,H35B, H35C), C33(H33A,H33B,H33C), C15(H15A,H15B,H15C), C13(H13A,H13B,H13C), C29(H29A, H29B,H29C) ; _shelx_res_file ; TITL 0011_2p16GPa in Pb21a #29 0011_2p16GPa.res created by SHELXL-2018/3 at 16:05:21 on 06-May-2024 CELL 0.41 16.785955 9.8051 16.569634 90 90 90 ZERR 8 0.001734 0.00019 0.000307 0 0 0 LATT -1 SYMM -X,0.5+Y,-Z SYMM 0.5+X,+Y,-Z SYMM 0.5-X,0.5+Y,+Z SFAC C H O P Au DISP Au -0.4672 3.5799 8847.0811 DISP C -0.0001 0.0005 5.0796 DISP H 0 0 0.5971 DISP O 0.0016 0.0018 9.9389 DISP P 0.0342 0.0304 85.9578 UNIT 120 176 8 8 8 SIMU 0.02 0.04 2 P2 C34 C35 SIMU 0.02 0.04 1.7 C23 C28 C27 C26 C25 C24 L.S. 40 0 0 PLAN 5 CONF BOND MORE -1 BOND $H fmap 2 53 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 REM REM REM WGHT 0.000000 2.234500 BASF 0.58051 FVAR 0.77456 AU2 5 0.633310 -0.008590 0.419388 11.00000 0.04997 0.03915 = 0.03667 0.00577 -0.00225 -0.00007 AU1 5 0.379516 0.711641 0.079181 11.00000 0.05190 0.04396 = 0.03819 0.00464 0.00397 -0.00315 P1 4 0.377690 0.909661 0.006027 11.00000 0.04865 0.03505 = 0.03260 0.00035 0.00155 -0.00523 P2 4 0.628174 -0.196900 0.497031 11.00000 0.04478 0.04010 = 0.03403 -0.00081 -0.00054 -0.00188 C23 1 0.630107 0.417068 0.306025 11.00000 0.02280 0.05705 = 0.04705 -0.01117 -0.01896 0.02006 C21 1 0.632651 0.166172 0.363973 11.00000 0.03818 0.04272 = 0.05385 -0.01161 -0.00285 0.01985 C26 1 0.636443 0.673526 0.230475 11.00000 0.01728 0.05298 = 0.03402 -0.01193 0.00666 -0.01059 C22 1 0.631336 0.286946 0.337189 11.00000 0.02744 0.03380 = 0.04135 -0.00789 0.00996 -0.00571 O2 3 0.639270 0.797105 0.197057 11.00000 0.15726 0.03140 = 0.05286 0.01277 0.00681 -0.00843 C1 1 0.382710 0.526054 0.134724 11.00000 0.05962 0.04858 = 0.04186 0.01109 -0.00097 -0.00431 C2 1 0.381893 0.416934 0.159929 11.00000 0.08177 0.09713 = 0.03483 0.02696 0.00488 0.00645 C27 1 0.564529 0.626485 0.260691 11.00000 0.01693 0.04240 = 0.03511 -0.00753 -0.00247 -0.00148 AFIX 43 H27 2 0.517890 0.677306 0.257028 11.00000 -1.20000 AFIX 0 C24 1 0.707455 0.475304 0.275564 11.00000 0.02151 0.04776 = 0.04914 0.00097 0.00161 0.01261 AFIX 43 H24 2 0.754310 0.425209 0.279845 11.00000 -1.20000 AFIX 0 C28 1 0.566484 0.498242 0.296912 11.00000 0.02655 0.04503 = 0.03983 0.00156 -0.00164 -0.00244 AFIX 43 H28 2 0.518412 0.465410 0.316940 11.00000 -1.20000 AFIX 0 C25 1 0.708350 0.603650 0.241213 11.00000 0.02216 0.05922 = 0.04628 -0.00120 0.00117 -0.00450 AFIX 43 H25 2 0.756225 0.643197 0.225393 11.00000 -1.20000 AFIX 0 C7 1 0.447587 0.106896 0.271607 11.00000 0.08958 0.03660 = 0.03627 -0.00650 -0.00708 0.01957 AFIX 43 H7 2 0.491240 0.079608 0.302166 11.00000 -1.20000 AFIX 0 C8 1 0.447470 0.235689 0.237706 11.00000 0.04455 0.04258 = 0.05221 -0.01664 0.00792 0.00909 AFIX 43 H8 2 0.491212 0.293048 0.243579 11.00000 -1.20000 AFIX 0 C3 1 0.381122 0.277761 0.194878 11.00000 0.05782 0.02004 = 0.02949 0.00358 -0.00267 -0.00449 C10 1 0.407990 0.875358 -0.098033 11.00000 0.03571 0.05338 = 0.03614 -0.00151 -0.01724 -0.00559 AFIX 23 H10A 2 0.387404 0.945984 -0.133324 11.00000 -1.20000 H10B 2 0.465653 0.875846 -0.101846 11.00000 -1.20000 AFIX 0 C11 1 0.375104 0.733258 -0.125009 11.00000 0.11424 0.04622 = 0.03601 -0.00861 -0.01970 -0.00764 AFIX 137 H11A 2 0.378657 0.725466 -0.182650 11.00000 -1.50000 H11B 2 0.320461 0.724822 -0.108654 11.00000 -1.50000 H11C 2 0.406008 0.662260 -0.100281 11.00000 -1.50000 AFIX 0 C31 1 0.666036 -0.035638 0.629415 11.00000 0.05112 0.04706 = 0.04666 -0.00096 -0.00602 0.00161 AFIX 137 H31A 2 0.679240 0.035389 0.591848 11.00000 -1.50000 H31B 2 0.698361 -0.026509 0.676904 11.00000 -1.50000 H31C 2 0.610826 -0.028596 0.643947 11.00000 -1.50000 AFIX 0 C30 1 0.681280 -0.172953 0.590906 11.00000 0.04280 0.03948 = 0.04144 -0.00309 0.00121 0.00329 AFIX 23 H30A 2 0.665655 -0.244073 0.628393 11.00000 -1.20000 H30B 2 0.737945 -0.182536 0.580925 11.00000 -1.20000 AFIX 0 O1 3 0.397443 -0.105788 0.300241 11.00000 0.07943 0.06457 = 0.06987 0.02924 -0.01376 -0.00384 C4 1 0.317080 0.191122 0.182914 11.00000 0.05150 0.05705 = 0.03439 -0.00160 0.00184 0.01549 AFIX 43 H4 2 0.272724 0.219356 0.153727 11.00000 -1.20000 AFIX 0 C32 1 0.668950 -0.353966 0.455523 11.00000 0.08329 0.06039 = 0.03247 -0.00672 0.01303 0.01106 AFIX 23 H32A 2 0.647480 -0.365990 0.401640 11.00000 -1.20000 H32B 2 0.726125 -0.342790 0.450188 11.00000 -1.20000 AFIX 0 C12 1 0.280139 0.987812 0.003292 11.00000 0.06695 0.06953 = 0.05979 -0.02334 -0.01187 0.02645 AFIX 23 H12A 2 0.263375 1.005042 0.058380 11.00000 -1.20000 H12B 2 0.284864 1.075482 -0.023405 11.00000 -1.20000 AFIX 0 C14 1 0.450193 1.039050 0.036774 11.00000 0.10634 0.04215 = 0.04233 -0.00557 -0.00830 -0.01132 AFIX 23 H14A 2 0.447292 1.051366 0.094785 11.00000 -1.20000 H14B 2 0.503409 1.007443 0.023704 11.00000 -1.20000 AFIX 0 C9 1 0.354398 -0.213761 0.287697 11.00000 0.07513 0.05521 = 0.06832 0.01485 0.04012 -0.00389 AFIX 137 H9A 2 0.381969 -0.274019 0.251571 11.00000 -1.50000 H9B 2 0.304400 -0.187583 0.264218 11.00000 -1.50000 H9C 2 0.345001 -0.259508 0.338029 11.00000 -1.50000 AFIX 0 C35 1 0.470949 -0.267377 0.454576 11.00000 0.04519 0.06379 = 0.04346 0.00261 0.00022 -0.00429 AFIX 137 H35A 2 0.492908 -0.342574 0.424880 11.00000 -1.50000 H35B 2 0.466553 -0.189429 0.419801 11.00000 -1.50000 H35C 2 0.419125 -0.291635 0.474435 11.00000 -1.50000 AFIX 0 C34 1 0.526636 -0.232423 0.527086 11.00000 0.03085 0.06362 = 0.03921 0.00606 0.00012 -0.00613 AFIX 23 H34A 2 0.526619 -0.308393 0.564584 11.00000 -1.20000 H34B 2 0.505420 -0.153575 0.555159 11.00000 -1.20000 AFIX 0 C6 1 0.383961 0.016354 0.261305 11.00000 0.08783 0.02651 = 0.03192 0.00956 0.00135 0.00525 C5 1 0.320998 0.056082 0.216887 11.00000 0.06292 0.04451 = 0.03380 -0.00349 0.00810 -0.02027 AFIX 43 H5 2 0.279346 -0.004623 0.207981 11.00000 -1.20000 AFIX 0 C33 1 0.653541 -0.483444 0.502808 11.00000 0.09767 0.04633 = 0.06479 -0.00166 -0.01594 0.01039 AFIX 137 H33A 2 0.693807 -0.549605 0.490158 11.00000 -1.50000 H33B 2 0.602137 -0.519140 0.488710 11.00000 -1.50000 H33C 2 0.654909 -0.463682 0.559536 11.00000 -1.50000 AFIX 0 C15 1 0.435562 1.175304 -0.004564 11.00000 0.07359 0.04418 = 0.07451 0.00601 -0.01022 -0.01519 AFIX 137 H15A 2 0.479163 1.195378 -0.040126 11.00000 -1.50000 H15B 2 0.431271 1.245765 0.035428 11.00000 -1.50000 H15C 2 0.387020 1.170751 -0.035079 11.00000 -1.50000 AFIX 0 C13 1 0.218728 0.911521 -0.036276 11.00000 0.02860 0.06666 = 0.06847 0.00224 0.00363 0.00839 AFIX 137 H13A 2 0.172402 0.967887 -0.042739 11.00000 -1.50000 H13B 2 0.205378 0.833148 -0.004293 11.00000 -1.50000 H13C 2 0.237248 0.882403 -0.088313 11.00000 -1.50000 AFIX 0 C29 1 0.576924 0.888630 0.198483 11.00000 0.07955 0.03019 = 0.09587 0.00842 -0.01858 -0.00090 AFIX 137 H29A 2 0.592733 0.971508 0.172121 11.00000 -1.50000 H29B 2 0.562702 0.907935 0.253426 11.00000 -1.50000 H29C 2 0.531929 0.850170 0.170897 11.00000 -1.50000 AFIX 0 HKLF 4 REM 0011_2p16GPa in Pb21a #29 REM wR2 = 0.1351, GooF = S = 1.059, Restrained GooF = 1.055 for all data REM R1 = 0.0488 for 3940 Fo > 4sig(Fo) and 0.0721 for all 5763 data REM 334 parameters refined using 49 restraints END WGHT 0.0000 2.1699 REM Highest difference peak 1.672, deepest hole -1.079, 1-sigma level 0.169 Q1 1 0.3891 0.6527 0.1024 11.00000 0.05 1.67 Q2 1 0.6255 0.0556 0.4089 11.00000 0.05 1.67 Q3 1 0.3755 0.7581 0.1198 11.00000 0.05 1.62 Q4 1 0.6234 -0.0482 0.3804 11.00000 0.05 1.50 Q5 1 0.6221 0.0416 0.4639 11.00000 0.05 1.08 ; _shelx_res_checksum 95449 _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 1.204 _oxdiff_exptl_absorpt_empirical_full_min 0.807 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' 'x+1/2, y, -z' '-x+1/2, y+1/2, z' 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 Au2 Au 0.63331(6) -0.00859(4) 0.41939(3) 0.0419(3) Uani 1 1 d . . . . . Au1 Au 0.37952(7) 0.71164(6) 0.07918(3) 0.0447(4) Uani 1 1 d . . . . . P1 P 0.3777(5) 0.9097(7) 0.0060(2) 0.039(3) Uani 1 1 d . . . . . P2 P 0.6282(6) -0.1969(7) 0.4970(2) 0.040(3) Uani 1 1 d . U . . . C23 C 0.630(2) 0.417(3) 0.3060(11) 0.042(7) Uani 1 1 d . U . . . C21 C 0.6327(19) 0.166(2) 0.3640(11) 0.045(11) Uani 1 1 d . . . . . C26 C 0.6364(18) 0.674(2) 0.2305(9) 0.035(6) Uani 1 1 d . U . . . C22 C 0.6313(17) 0.2869(17) 0.3372(9) 0.034(9) Uani 1 1 d . . . . . O2 O 0.6393(16) 0.7971(15) 0.1971(8) 0.081(11) Uani 1 1 d . . . . . C1 C 0.3827(19) 0.526(2) 0.1347(10) 0.050(11) Uani 1 1 d . . . . . C2 C 0.382(2) 0.417(3) 0.1599(10) 0.071(14) Uani 1 1 d . . . . . C27 C 0.5645(16) 0.6265(16) 0.2607(7) 0.031(5) Uani 1 1 d . U . . . H27 H 0.517890 0.677306 0.257028 0.038 Uiso 1 1 calc R U . . . C24 C 0.7075(18) 0.4753(17) 0.2756(8) 0.039(6) Uani 1 1 d . U . . . H24 H 0.754310 0.425209 0.279845 0.047 Uiso 1 1 calc R U . . . C28 C 0.5665(16) 0.4982(18) 0.2969(7) 0.037(5) Uani 1 1 d . U . . . H28 H 0.518412 0.465410 0.316940 0.045 Uiso 1 1 calc R U . . . C25 C 0.708(2) 0.6037(18) 0.2412(8) 0.043(6) Uani 1 1 d . U . . . H25 H 0.756225 0.643197 0.225393 0.051 Uiso 1 1 calc R U . . . C7 C 0.448(2) 0.1069(16) 0.2716(9) 0.054(10) Uani 1 1 d . . . . . H7 H 0.491240 0.079608 0.302166 0.065 Uiso 1 1 calc R U . . . C8 C 0.447(2) 0.2357(15) 0.2377(9) 0.046(10) Uani 1 1 d . . . . . H8 H 0.491212 0.293048 0.243579 0.056 Uiso 1 1 calc R U . . . C3 C 0.3811(16) 0.2778(16) 0.1949(8) 0.036(8) Uani 1 1 d . . . . . C10 C 0.4080(19) 0.8754(18) -0.0980(8) 0.042(9) Uani 1 1 d . . . . . H10A H 0.387404 0.945984 -0.133324 0.050 Uiso 1 1 calc R U . . . H10B H 0.465653 0.875846 -0.101846 0.050 Uiso 1 1 calc R U . . . C11 C 0.375(2) 0.733(2) -0.1250(9) 0.065(12) Uani 1 1 d . . . . . H11A H 0.378657 0.725466 -0.182650 0.098 Uiso 1 1 calc R U . . . H11B H 0.320461 0.724822 -0.108654 0.098 Uiso 1 1 calc R U . . . H11C H 0.406008 0.662260 -0.100281 0.098 Uiso 1 1 calc R U . . . C31 C 0.666(2) -0.0356(16) 0.6294(9) 0.048(10) Uani 1 1 d . . . . . H31A H 0.679240 0.035389 0.591848 0.072 Uiso 1 1 calc R U . . . H31B H 0.698361 -0.026509 0.676904 0.072 Uiso 1 1 calc R U . . . H31C H 0.610826 -0.028596 0.643947 0.072 Uiso 1 1 calc R U . . . C30 C 0.6813(19) -0.1730(15) 0.5909(7) 0.041(10) Uani 1 1 d . . . . . H30A H 0.665655 -0.244073 0.628393 0.049 Uiso 1 1 calc R U . . . H30B H 0.737945 -0.182536 0.580925 0.049 Uiso 1 1 calc R U . . . O1 O 0.3974(17) -0.106(2) 0.3002(9) 0.071(10) Uani 1 1 d . . . . . C4 C 0.3171(19) 0.1911(18) 0.1829(8) 0.048(10) Uani 1 1 d . . . . . H4 H 0.272724 0.219356 0.153727 0.057 Uiso 1 1 calc R U . . . C32 C 0.669(2) -0.3540(18) 0.4555(7) 0.059(11) Uani 1 1 d . . . . . H32A H 0.647480 -0.365990 0.401640 0.070 Uiso 1 1 calc R U . . . H32B H 0.726125 -0.342790 0.450188 0.070 Uiso 1 1 calc R U . . . C12 C 0.280(2) 0.988(3) 0.0033(10) 0.065(13) Uani 1 1 d . . . . . H12A H 0.263375 1.005042 0.058380 0.079 Uiso 1 1 calc R U . . . H12B H 0.284864 1.075482 -0.023405 0.079 Uiso 1 1 calc R U . . . C14 C 0.450(2) 1.0390(16) 0.0368(8) 0.064(12) Uani 1 1 d . . . . . H14A H 0.447292 1.051366 0.094785 0.076 Uiso 1 1 calc R U . . . H14B H 0.503409 1.007443 0.023704 0.076 Uiso 1 1 calc R U . . . C9 C 0.354(2) -0.214(2) 0.2877(12) 0.066(13) Uani 1 1 d . . . . . H9A H 0.381969 -0.274019 0.251571 0.099 Uiso 1 1 calc R U . . . H9B H 0.304400 -0.187583 0.264218 0.099 Uiso 1 1 calc R U . . . H9C H 0.345001 -0.259508 0.338029 0.099 Uiso 1 1 calc R U . . . C35 C 0.471(2) -0.2674(19) 0.4546(8) 0.051(9) Uani 1 1 d . U . . . H35A H 0.492908 -0.342574 0.424880 0.076 Uiso 1 1 calc R U . . . H35B H 0.466553 -0.189429 0.419801 0.076 Uiso 1 1 calc R U . . . H35C H 0.419125 -0.291635 0.474435 0.076 Uiso 1 1 calc R U . . . C34 C 0.527(2) -0.232(2) 0.5271(8) 0.045(7) Uani 1 1 d . U . . . H34A H 0.526619 -0.308393 0.564584 0.053 Uiso 1 1 calc R U . . . H34B H 0.505420 -0.153575 0.555159 0.053 Uiso 1 1 calc R U . . . C6 C 0.3840(18) 0.0164(15) 0.2613(9) 0.049(10) Uani 1 1 d . . . . . C5 C 0.3210(18) 0.0561(16) 0.2169(8) 0.047(10) Uani 1 1 d . . . . . H5 H 0.279346 -0.004623 0.207981 0.056 Uiso 1 1 calc R U . . . C33 C 0.654(3) -0.483(2) 0.5028(10) 0.070(15) Uani 1 1 d . . . . . H33A H 0.693807 -0.549605 0.490158 0.104 Uiso 1 1 calc R U . . . H33B H 0.602137 -0.519140 0.488710 0.104 Uiso 1 1 calc R U . . . H33C H 0.654909 -0.463682 0.559536 0.104 Uiso 1 1 calc R U . . . C15 C 0.436(3) 1.175(2) -0.0046(11) 0.064(14) Uani 1 1 d . . . . . H15A H 0.479163 1.195378 -0.040126 0.096 Uiso 1 1 calc R U . . . H15B H 0.431271 1.245765 0.035428 0.096 Uiso 1 1 calc R U . . . H15C H 0.387020 1.170751 -0.035079 0.096 Uiso 1 1 calc R U . . . C13 C 0.219(2) 0.912(2) -0.0363(10) 0.055(13) Uani 1 1 d . . . . . H13A H 0.172402 0.967887 -0.042739 0.082 Uiso 1 1 calc R U . . . H13B H 0.205378 0.833148 -0.004293 0.082 Uiso 1 1 calc R U . . . H13C H 0.237248 0.882403 -0.088313 0.082 Uiso 1 1 calc R U . . . C29 C 0.577(3) 0.8886(17) 0.1985(13) 0.069(14) Uani 1 1 d . . . . . H29A H 0.592733 0.971508 0.172121 0.103 Uiso 1 1 calc R U . . . H29B H 0.562702 0.907935 0.253426 0.103 Uiso 1 1 calc R U . . . H29C H 0.531929 0.850170 0.170897 0.103 Uiso 1 1 calc R U . . . 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 Au2 0.0500(11) 0.0392(3) 0.0367(3) 0.0058(4) -0.0023(3) -0.0001(4) Au1 0.0519(12) 0.0440(3) 0.0382(3) 0.0046(4) 0.0040(3) -0.0032(4) P1 0.049(10) 0.035(2) 0.033(2) 0.0003(15) 0.002(2) -0.005(2) P2 0.045(11) 0.040(3) 0.034(2) -0.0008(15) -0.001(2) -0.002(3) C23 0.02(2) 0.057(10) 0.047(8) -0.011(8) -0.019(8) 0.020(10) C21 0.04(4) 0.043(10) 0.054(10) -0.012(8) -0.003(10) 0.020(10) C26 0.017(19) 0.053(9) 0.034(6) -0.012(6) 0.007(7) -0.011(8) C22 0.03(3) 0.034(7) 0.041(8) -0.008(6) 0.010(8) -0.006(8) O2 0.16(4) 0.031(6) 0.053(7) 0.013(5) 0.007(10) -0.008(9) C1 0.06(4) 0.049(11) 0.042(9) 0.011(7) -0.001(9) -0.004(10) C2 0.08(4) 0.097(18) 0.035(8) 0.027(10) 0.005(10) 0.006(16) C27 0.017(18) 0.042(6) 0.035(5) -0.008(5) -0.002(7) -0.001(8) C24 0.02(2) 0.048(7) 0.049(6) 0.001(6) 0.002(7) 0.013(9) C28 0.027(18) 0.045(6) 0.040(5) 0.002(6) -0.002(7) -0.002(9) C25 0.02(2) 0.059(9) 0.046(6) -0.001(6) 0.001(8) -0.004(10) C7 0.09(3) 0.037(7) 0.036(6) -0.006(5) -0.007(10) 0.020(11) C8 0.04(4) 0.043(7) 0.052(8) -0.017(6) 0.008(9) 0.009(10) C3 0.06(3) 0.020(5) 0.029(6) 0.004(5) -0.003(7) -0.004(7) C10 0.04(3) 0.053(8) 0.036(6) -0.002(5) -0.017(8) -0.006(11) C11 0.11(4) 0.046(9) 0.036(6) -0.009(6) -0.020(10) -0.008(11) C31 0.05(4) 0.047(10) 0.047(8) -0.001(6) -0.006(9) 0.002(10) C30 0.04(3) 0.039(6) 0.041(7) -0.003(5) 0.001(8) 0.003(10) O1 0.08(4) 0.065(10) 0.070(9) 0.029(8) -0.014(11) -0.004(12) C4 0.05(3) 0.057(9) 0.034(6) -0.002(6) 0.002(8) 0.015(11) C32 0.08(4) 0.060(10) 0.032(6) -0.007(6) 0.013(9) 0.011(13) C12 0.07(4) 0.070(11) 0.060(9) -0.023(9) -0.012(11) 0.026(17) C14 0.11(4) 0.042(7) 0.042(7) -0.006(6) -0.008(10) -0.011(12) C9 0.08(4) 0.055(10) 0.068(10) 0.015(9) 0.040(14) -0.004(14) C35 0.05(3) 0.064(10) 0.043(7) 0.003(6) 0.000(9) -0.004(12) C34 0.03(2) 0.064(9) 0.039(6) 0.006(6) 0.000(8) -0.006(11) C6 0.09(3) 0.027(6) 0.032(6) 0.010(5) 0.001(8) 0.005(7) C5 0.06(3) 0.045(7) 0.034(6) -0.003(5) 0.008(8) -0.020(10) C33 0.10(5) 0.046(11) 0.065(11) -0.002(7) -0.016(13) 0.010(14) C15 0.07(5) 0.044(10) 0.075(12) 0.006(7) -0.010(13) -0.015(14) C13 0.03(4) 0.067(11) 0.068(10) 0.002(8) 0.004(11) 0.008(15) C29 0.08(5) 0.030(7) 0.096(13) 0.008(8) -0.019(17) -0.001(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0001 0.0005 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0016 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.0342 0.0304 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -0.4672 3.5799 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _axis.id _axis.type _axis.equipment _axis.parity _axis.depends_on _axis.zero _axis.vector[1] _axis.vector[2] _axis.vector[3] source . source . . . 1.00000000 0.00000000 0.00000000 omega rotation goniometer -1 . -0.00106000 0.00000000 0.00000000 1.00000000 kappa rotation goniometer -1 omega 0.00000000 -0.76604444 0.00000000 0.64278761 phi rotation goniometer -1 kappa . 0.00000000 0.00000000 1.00000000 theta rotation goniometer -1 . 0.00200000 0.00000000 0.00000000 1.00000000 matrixX general general . phi . 1.00000000 0.00000000 0.00000000 matrixY general general . phi . 0.00000000 1.00000000 0.00000000 matrixZ general general . phi . 0.00000000 0.00000000 1.00000000 dacX translation general . phi . 0.00000000 1.00000000 0.00000000 dacY translation general . phi . -1.00000000 0.00000000 0.00000000 dacZ translation general . phi . 0.00000000 0.00000000 1.00000000 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 C21 Au2 P2 172.9(6) . . ? C1 Au1 P1 174.8(6) . . ? C10 P1 Au1 109.8(6) . . ? C10 P1 C14 101.8(11) . . ? C12 P1 Au1 112.6(10) . . ? C12 P1 C10 107.8(11) . . ? C12 P1 C14 108.4(13) . . ? C14 P1 Au1 115.6(7) . . ? C30 P2 Au2 111.5(6) . . ? C30 P2 C32 104.4(11) . . ? C30 P2 C34 104.6(10) . . ? C32 P2 Au2 117.6(6) . . ? C34 P2 Au2 110.6(8) . . ? C34 P2 C32 107.2(13) . . ? C22 C23 C24 118(3) . . ? C28 C23 C22 127(3) . . ? C28 C23 C24 115(2) . . ? C22 C21 Au2 172.3(16) . . ? O2 C26 C27 119(3) . . ? O2 C26 C25 118(2) . . ? C27 C26 C25 123(2) . . ? C21 C22 C23 178.5(18) . . ? C26 O2 C29 124(2) . . ? C2 C1 Au1 174(2) . . ? C1 C2 C3 178(3) . . ? C26 C27 H27 122.1 . . ? C26 C27 C28 116(2) . . ? C28 C27 H27 122.1 . . ? C23 C24 H24 120.2 . . ? C25 C24 C23 120(3) . . ? C25 C24 H24 120.2 . . ? C23 C28 C27 127(3) . . ? C23 C28 H28 116.5 . . ? C27 C28 H28 116.5 . . ? C26 C25 H25 120.4 . . ? C24 C25 C26 119(3) . . ? C24 C25 H25 120.4 . . ? C8 C7 H7 119.0 . . ? C8 C7 C6 122(2) . . ? C6 C7 H7 119.0 . . ? C7 C8 H8 120.6 . . ? C7 C8 C3 119(3) . . ? C3 C8 H8 120.6 . . ? C8 C3 C2 118(2) . . ? C8 C3 C4 121.0(16) . . ? C4 C3 C2 121(2) . . ? P1 C10 H10A 109.8 . . ? P1 C10 H10B 109.8 . . ? H10A C10 H10B 108.2 . . ? C11 C10 P1 109.6(16) . . ? C11 C10 H10A 109.8 . . ? C11 C10 H10B 109.8 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? P2 C30 H30A 108.9 . . ? P2 C30 H30B 108.9 . . ? C31 C30 P2 113.3(16) . . ? C31 C30 H30A 108.9 . . ? C31 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? C9 O1 C6 123(2) . . ? C3 C4 H4 120.9 . . ? C3 C4 C5 118(2) . . ? C5 C4 H4 120.9 . . ? P2 C32 H32A 108.1 . . ? P2 C32 H32B 108.1 . . ? H32A C32 H32B 107.3 . . ? C33 C32 P2 116.7(16) . . ? C33 C32 H32A 108.1 . . ? C33 C32 H32B 108.1 . . ? P1 C12 H12A 108.2 . . ? P1 C12 H12B 108.2 . . ? H12A C12 H12B 107.4 . . ? C13 C12 P1 116.2(17) . . ? C13 C12 H12A 108.2 . . ? C13 C12 H12B 108.2 . . ? P1 C14 H14A 109.2 . . ? P1 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C15 C14 P1 112(2) . . ? C15 C14 H14A 109.2 . . ? C15 C14 H14B 109.2 . . ? O1 C9 H9A 109.5 . . ? O1 C9 H9B 109.5 . . ? O1 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? P2 C34 H34A 108.9 . . ? P2 C34 H34B 108.9 . . ? C35 C34 P2 113.2(13) . . ? C35 C34 H34A 108.9 . . ? C35 C34 H34B 108.9 . . ? H34A C34 H34B 107.7 . . ? O1 C6 C7 112(2) . . ? C5 C6 C7 118.9(15) . . ? C5 C6 O1 130(2) . . ? C4 C5 H5 119.5 . . ? C6 C5 C4 121(2) . . ? C6 C5 H5 119.5 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O2 C29 H29A 109.5 . . ? O2 C29 H29B 109.5 . . ? O2 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? 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 Au2 P2 2.252(6) . ? Au2 C21 1.94(2) . ? Au1 P1 2.289(6) . ? Au1 C1 2.040(19) . ? P1 C10 1.829(17) . ? P1 C12 1.81(3) . ? P1 C14 1.83(3) . ? P2 C30 1.808(19) . ? P2 C32 1.82(2) . ? P2 C34 1.81(3) . ? C23 C22 1.38(3) . ? C23 C24 1.51(4) . ? C23 C28 1.34(4) . ? C21 C22 1.26(3) . ? C26 O2 1.33(3) . ? C26 C27 1.39(4) . ? C26 C25 1.40(4) . ? O2 C29 1.38(4) . ? C1 C2 1.15(4) . ? C2 C3 1.48(3) . ? C27 H27 0.9300 . ? C27 C28 1.39(2) . ? C24 H24 0.9300 . ? C24 C25 1.38(2) . ? C28 H28 0.9300 . ? C25 H25 0.9300 . ? C7 H7 0.9300 . ? C7 C8 1.38(2) . ? C7 C6 1.40(4) . ? C8 H8 0.9300 . ? C8 C3 1.38(4) . ? C3 C4 1.38(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 C11 1.56(3) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C31 C30 1.51(2) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? O1 C9 1.30(4) . ? O1 C6 1.38(2) . ? C4 H4 0.9300 . ? C4 C5 1.44(2) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 C33 1.51(3) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 C13 1.43(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 C15 1.52(3) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C35 C34 1.56(3) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C6 C5 1.35(4) . ? C5 H5 0.9300 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? 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 Au2 P2 C30 C31 43(2) . . . . ? Au2 P2 C32 C33 -171(2) . . . . ? Au2 P2 C34 C35 64.1(14) . . . . ? Au1 P1 C10 C11 36(2) . . . . ? Au1 P1 C12 C13 -64.2(17) . . . . ? Au1 P1 C14 C15 -170.0(18) . . . . ? C23 C24 C25 C26 -4(2) . . . . ? C26 C27 C28 C23 1(2) . . . . ? C22 C23 C24 C25 177.7(15) . . . . ? C22 C23 C28 C27 -175.6(15) . . . . ? O2 C26 C27 C28 -178.1(13) . . . . ? O2 C26 C25 C24 -179.9(14) . . . . ? C2 C3 C4 C5 178.5(17) . . . . ? C27 C26 O2 C29 8(3) . . . . ? C27 C26 C25 C24 7(3) . . . . ? C24 C23 C28 C27 2(3) . . . . ? C28 C23 C24 C25 0(2) . . . . ? C25 C26 O2 C29 -166(2) . . . . ? C25 C26 C27 C28 -5(2) . . . . ? C7 C8 C3 C2 179.2(17) . . . . ? C7 C8 C3 C4 -3(3) . . . . ? C7 C6 C5 C4 -2(3) . . . . ? C8 C7 C6 O1 179.8(17) . . . . ? C8 C7 C6 C5 0(3) . . . . ? C8 C3 C4 C5 1(3) . . . . ? C3 C4 C5 C6 2(3) . . . . ? C10 P1 C12 C13 57(2) . . . . ? C10 P1 C14 C15 71(2) . . . . ? C30 P2 C32 C33 65(3) . . . . ? C30 P2 C34 C35 -175.7(13) . . . . ? O1 C6 C5 C4 178.0(19) . . . . ? C32 P2 C30 C31 171(2) . . . . ? C32 P2 C34 C35 -65.2(15) . . . . ? C12 P1 C10 C11 -87(2) . . . . ? C12 P1 C14 C15 -43(2) . . . . ? C14 P1 C10 C11 159.4(19) . . . . ? C14 P1 C12 C13 166.7(16) . . . . ? C9 O1 C6 C7 -167(2) . . . . ? C9 O1 C6 C5 12(4) . . . . ? C34 P2 C30 C31 -77(2) . . . . ? C34 P2 C32 C33 -46(3) . . . . ? C6 C7 C8 C3 2(3) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.42(6) 2 0.58(6)