#------------------------------------------------------------------------------ #$Date: 2025-01-10 01:45:50 +0200 (Fri, 10 Jan 2025) $ #$Revision: 297250 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/36/1573655.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_1573655 _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 monoclinic _space_group_IT_number 7 _space_group_name_Hall 'P -2a' _space_group_name_H-M_alt 'P 1 1 a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2023-05-31 _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _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 93.865(3) _cell_formula_units_Z 8 _cell_length_a 16.7021(6) _cell_length_b 9.8830(3) _cell_length_c 16.8029(4) _cell_measurement_reflns_used 8058 _cell_measurement_temperature 294.7(3) _cell_measurement_theta_max 19.6880 _cell_measurement_theta_min 2.4260 _cell_volume 2767.29(15) _computing_cell_refinement 'CrysAlisPro 1.171.42.36a (Rigaku OD, 2021)' _computing_data_collection 'CrysAlisPro 1.171.42.36a (Rigaku OD, 2021)' _computing_data_reduction 'CrysAlisPro 1.171.42.36a (Rigaku OD, 2021)' _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 silicone oil' _diffrn_ambient_pressure 2130000 _diffrn_ambient_temperature 294.7(3) _diffrn_crystal_treatment 'pressurized rapidly in silicone oil as a hydrostatic medium' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0128 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.651 _diffrn_measured_fraction_theta_max 0.604 _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 10.00 35.00 1.00 60.00 -- 22.04 53.00 -17.00 25 2 \w -20.00 51.00 1.00 95.00 -- 22.04 -53.00 17.00 71 3 \w -27.00 51.00 1.00 95.00 -- 22.04 -39.00-167.00 78 4 \w -50.00 45.00 1.00 95.00 -- 22.04 26.00 -8.00 95 5 \w -13.00 17.00 1.00 95.00 -- 22.04 97.00 143.00 30 6 \w -20.00 7.00 1.00 95.00 -- 22.04 114.00 -45.00 27 7 \w -32.00 -6.00 1.00 95.00 -- 22.04 39.00 167.00 26 8 \w -67.00 -13.00 1.00 95.00 -- -22.19 135.00 123.00 54 9 \w -23.00 28.00 1.00 95.00 -- -22.19 39.00 -12.00 51 10 \w -85.00 1.00 1.00 95.00 -- -22.19 114.00 -45.00 86 11 \w -45.00 48.00 1.00 95.00 -- -22.19 -26.00 8.00 93 12 \w -34.00 29.00 1.00 95.00 -- -22.19 53.00 162.00 63 13 \w -17.00 21.00 1.00 95.00 -- -22.19 -97.00-143.00 38 14 \w -16.00 21.00 1.00 95.00 -- -22.19 -97.00 35.00 37 15 \w -50.00 45.00 1.00 60.00 -- 22.04 26.00 -8.00 95 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, Eos' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'Diamond Anvil Cell, effective opening angle 51 deg.' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0260618715 _diffrn_orient_matrix_UB_12 -0.0379671868 _diffrn_orient_matrix_UB_13 0.0040788950 _diffrn_orient_matrix_UB_21 -0.0089981972 _diffrn_orient_matrix_UB_22 0.0272505665 _diffrn_orient_matrix_UB_23 0.0274262832 _diffrn_orient_matrix_UB_31 -0.0191501385 _diffrn_orient_matrix_UB_32 0.0321626829 _diffrn_orient_matrix_UB_33 -0.0184265919 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Ag K\a' _diffrn_radiation_wavelength 0.56087 _diffrn_reflns_av_R_equivalents 0.0547 _diffrn_reflns_av_unetI/netI 0.0738 _diffrn_reflns_Laue_measured_fraction_full 0.651 _diffrn_reflns_Laue_measured_fraction_max 0.604 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 22719 _diffrn_reflns_point_group_measured_fraction_full 0.643 _diffrn_reflns_point_group_measured_fraction_max 0.583 _diffrn_reflns_theta_full 19.665 _diffrn_reflns_theta_max 20.977 _diffrn_reflns_theta_min 2.513 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Ag) X-ray Source' _exptl_absorpt_coefficient_mu 5.803 _exptl_absorpt_correction_T_max 0.20757 _exptl_absorpt_correction_T_min 0.19601 _exptl_absorpt_correction_type sphere _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.36a (Rigaku Oxford Diffraction, 2021) Spherical absorption correction using equivalent radius and absorption coefficient. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear violet' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary violet _exptl_crystal_density_diffrn 2.142 _exptl_crystal_description needle _exptl_crystal_F_000 1712 _exptl_crystal_preparation 'Mounted in a Diamond-Anvil Cell using silicone oil as pressure medium.,Luminescent' _exptl_crystal_pressure_history 'Pressurized to 2.13 GPa and left to stabilize over ? hours.' _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: n-pentane/dichloromethane' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_size_rad 0.400 _refine_diff_density_max 0.926 _refine_diff_density_min -0.971 _refine_diff_density_rms 0.143 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.06(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 666 _refine_ls_number_reflns 7038 _refine_ls_number_restraints 410 _refine_ls_restrained_S_all 0.986 _refine_ls_R_factor_all 0.0749 _refine_ls_R_factor_gt 0.0432 _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^)+(0.0258P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.0711 _reflns_Friedel_coverage 0.927 _reflns_Friedel_fraction_full 0.636 _reflns_Friedel_fraction_max 0.562 _reflns_number_gt 5324 _reflns_number_total 7038 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4dt03036b2.cif _cod_data_source_block appr5_2p13GPa _cod_original_cell_volume 2767.29(14) _cod_original_sg_symbol_H-M 'P 1 1 a' _cod_database_code 1573655 _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. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.94(3) 0.06(3) 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 C49 \\sim O3 \\sim C46 \\sim C47 \\sim C45 \\sim C44 \\sim C48 \\sim C43 \\sim C42 \\sim C41: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.7A C34 \\sim C35 \\sim C31 \\sim C30 \\sim C33 \\sim C32 \\sim P2: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A C21 \\sim C22 \\sim C23 \\sim C28 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim O2 \\sim C29: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.7A C15 \\sim C14 \\sim C11 \\sim C10 \\sim C13 \\sim C12 \\sim P1: within 2A with sigma of 0.03 and sigma for terminal atoms of 0.06 within 2A C51 \\sim C50 \\sim C53 \\sim C52 \\sim C55 \\sim C54 \\sim P3: within 2A with sigma of 0.03 and sigma for terminal atoms of 0.06 within 2A C9 \\sim O1 \\sim C6 \\sim C5 \\sim C7 \\sim C4 \\sim C8 \\sim C3 \\sim C2 \\sim C1: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.7A C75 \\sim C74 \\sim C73 \\sim C72 \\sim C70 \\sim C71 \\sim P4: within 2A with sigma of 0.03 and sigma for terminal atoms of 0.06 within 2A C61 \\sim C62 \\sim C63 \\sim C64 \\sim C68 \\sim C65 \\sim C67 \\sim C66 \\sim O4 \\sim C69: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.7A Uanis(C29) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C54) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 4.a Secondary CH2 refined with riding coordinates: C74(H74A,H74B), C30(H30A,H30B), C34(H34A,H34B), C70(H70A,H70B), C32(H32A, H32B), C52(H52A,H52B), C54(H54A,H54B), C50(H50A,H50B), C72(H72A,H72B), C14(H14A,H14B), C10(H10A,H10B), C12(H12A,H12B) 4.b Aromatic/amide H refined with riding coordinates: C7(H7), C5(H5), C44(H44), C24(H24), C8(H8), C65(H65), C64(H64), C48(H48), C67(H67), C68(H68), C28(H28), C4(H4), C27(H27), C25(H25), C45(H45), C47(H47) 4.c Idealised Me refined as rotating group: C55(H55A,H55B,H55C), C53(H53A,H53B,H53C), C31(H31A,H31B,H31C), C71(H71A,H71B, H71C), C51(H51A,H51B,H51C), C11(H11A,H11B,H11C), C9(H9A,H9B,H9C), C15(H15A, H15B,H15C), C33(H33A,H33B,H33C), C13(H13A,H13B,H13C), C69(H69A,H69B,H69C), C29(H29A,H29B,H29C), C49(H49A,H49B,H49C), C75(H75A,H75B,H75C), C73(H73A,H73B, H73C), C35(H35A,H35B,H35C) ; _shelx_res_file ; TITL appr5_2p13GPa in P11a #7 appr5_2p13GPa.res created by SHELXL-2018/3 at 12:05:06 on 31-May-2023 REM reset to P11a #7 CELL 0.56087 16.702107 9.882976 16.802906 90 90 93.8649 ZERR 8 0.000565 0.000303 0.000377 0 0 0.0026 LATT -1 SYMM 0.5+X,+Y,-Z SFAC C H Au O P DISP Au -0.657 6.026 19723.5 DISP C 0.0013 0.0009 7.4 DISP H 0 0 0.7 DISP O 0.0058 0.0036 18.2 DISP P 0.0671 0.0586 203.6 UNIT 120 176 8 8 8 SIMU 0.02 0.04 1.7 C49 O3 C46 C47 C45 C44 C48 C43 C42 C41 SIMU 0.02 0.04 2 C34 C35 C31 C30 C33 C32 P2 SIMU 0.02 0.04 1.7 C21 C22 C23 C28 C24 C25 C26 C27 O2 C29 SIMU 0.03 0.06 2 C15 C14 C11 C10 C13 C12 P1 SIMU 0.03 0.06 2 C51 C50 C53 C52 C55 C54 P3 SIMU 0.02 0.04 1.7 C9 O1 C6 C5 C7 C4 C8 C3 C2 C1 SIMU 0.03 0.06 2 C75 C74 C73 C72 C70 C71 P4 SIMU 0.02 0.04 1.7 C61 C62 C63 C64 C68 C65 C67 C66 O4 C69 ISOR 0.01 0.02 C29 C69 C13 C54 L.S. 20 PLAN 20 TEMP 22 CONF BOND MORE -1 BOND $H fmap 2 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 REM REM REM WGHT 0.025800 BASF 0.06339 FVAR 1.19181 AU2 3 0.365677 0.305431 0.923921 11.00000 0.04342 0.04053 = 0.03454 0.00454 -0.00148 0.00801 AU3 3 0.618600 0.982256 0.415571 11.00000 0.04852 0.04062 = 0.03417 -0.00222 -0.00368 0.00536 AU4 3 0.598852 0.780447 0.914766 11.00000 0.04524 0.03666 = 0.03326 0.00495 0.00131 0.00943 AU1 3 0.347010 0.501039 0.428167 11.00000 0.04450 0.03946 = 0.03274 -0.00457 0.00167 0.00809 P3 5 0.612004 1.177540 0.487029 11.00000 0.03645 0.03680 = 0.03035 -0.00085 -0.00691 0.00016 P4 5 0.604759 0.593730 0.992321 11.00000 0.03411 0.03016 = 0.02818 -0.00135 -0.00150 0.00424 P1 5 0.351414 0.700172 0.498819 11.00000 0.03853 0.04236 = 0.03028 0.00017 0.00134 0.01417 P2 5 0.361136 0.112287 0.998490 11.00000 0.03733 0.03532 = 0.02904 0.00110 -0.00404 0.00421 C21 1 0.366527 0.485668 0.868393 11.00000 0.05169 0.04789 = 0.02840 -0.00461 -0.00331 0.01022 C2 1 0.349756 0.212042 0.344622 11.00000 0.03853 0.03850 = 0.03776 0.00001 0.00582 0.01047 C1 1 0.347949 0.326534 0.372891 11.00000 0.03081 0.05965 = 0.04881 0.00603 0.00205 0.02286 C62 1 0.604340 1.077658 0.833911 11.00000 0.01452 0.02910 = 0.03241 -0.00073 -0.00183 -0.00597 C61 1 0.599716 0.958384 0.859460 11.00000 0.02747 0.02814 = 0.02925 0.00089 -0.00116 -0.01474 C3 1 0.348581 0.072648 0.308911 11.00000 0.04804 0.03892 = 0.01988 -0.00188 0.01095 0.00693 C41 1 0.614863 0.802668 0.361690 11.00000 0.03692 0.07862 = 0.04051 -0.01440 -0.00136 0.03067 C74 1 0.707950 0.577773 1.021882 11.00000 0.04475 0.03744 = 0.02793 -0.01026 -0.00430 -0.01261 AFIX 23 H74A 2 0.728467 0.661719 1.046672 11.00000 -1.20000 H74B 2 0.709755 0.506081 1.061138 11.00000 -1.20000 AFIX 0 C30 1 0.413088 0.142372 1.093884 11.00000 0.01492 0.02802 = 0.03037 -0.00087 -0.01131 -0.00977 AFIX 23 H30A 2 0.398776 0.067625 1.129684 11.00000 -1.20000 H30B 2 0.470581 0.145022 1.085155 11.00000 -1.20000 AFIX 0 C34 1 0.261903 0.058981 1.026953 11.00000 0.04013 0.03716 = 0.03349 0.00267 0.00438 -0.00658 AFIX 23 H34A 2 0.263417 -0.020534 1.060620 11.00000 -1.20000 H34B 2 0.239864 0.130194 1.058171 11.00000 -1.20000 AFIX 0 C70 1 0.546871 0.605279 1.082240 11.00000 0.02897 0.03817 = 0.03922 0.01541 -0.00674 -0.01059 AFIX 23 H70A 2 0.490075 0.596457 1.069671 11.00000 -1.20000 H70B 2 0.558533 0.532178 1.118050 11.00000 -1.20000 AFIX 0 C32 1 0.407141 -0.031099 0.956237 11.00000 0.06621 0.03766 = 0.04720 -0.00195 -0.00211 0.01742 AFIX 23 H32A 2 0.386523 -0.045859 0.902747 11.00000 -1.20000 H32B 2 0.464443 -0.008887 0.952001 11.00000 -1.20000 AFIX 0 C52 1 0.507257 1.221588 0.485807 11.00000 0.02794 0.08027 = 0.03868 -0.00509 0.00352 -0.02134 AFIX 23 H52A 2 0.503275 1.288981 0.444279 11.00000 -1.20000 H52B 2 0.475791 1.141139 0.468063 11.00000 -1.20000 AFIX 0 C54 1 0.673829 1.327002 0.457534 11.00000 0.03123 0.03818 = 0.03935 -0.00213 -0.00068 -0.00189 AFIX 23 H54A 2 0.729675 1.311019 0.467142 11.00000 -1.20000 H54B 2 0.667393 1.341093 0.400826 11.00000 -1.20000 AFIX 0 C50 1 0.638891 1.153703 0.591269 11.00000 0.02979 0.05934 = 0.03281 -0.01497 -0.00442 0.00637 AFIX 23 H50A 2 0.696714 1.165382 0.597192 11.00000 -1.20000 H50B 2 0.615128 1.221571 0.623736 11.00000 -1.20000 AFIX 0 C72 1 0.569660 0.429657 0.951486 11.00000 0.06623 0.04334 = 0.04633 -0.01043 -0.00169 0.01361 AFIX 23 H72A 2 0.511801 0.427494 0.945730 11.00000 -1.20000 H72B 2 0.592330 0.421132 0.898719 11.00000 -1.20000 AFIX 0 C55 1 0.654246 1.452283 0.500348 11.00000 0.08104 0.01060 = 0.07824 0.00521 -0.00225 0.00117 AFIX 137 H55A 2 0.601493 1.475938 0.485425 11.00000 -1.50000 H55B 2 0.692713 1.525065 0.486553 11.00000 -1.50000 H55C 2 0.655892 1.436710 0.556700 11.00000 -1.50000 AFIX 0 C53 1 0.467542 1.269986 0.552062 11.00000 0.04767 0.16998 = 0.06214 0.00311 0.01067 0.04958 AFIX 137 H53A 2 0.415508 1.296148 0.536412 11.00000 -1.50000 H53B 2 0.498165 1.347096 0.573667 11.00000 -1.50000 H53C 2 0.461657 1.199977 0.591646 11.00000 -1.50000 AFIX 0 O1 4 0.340282 -0.306462 0.201776 11.00000 0.09215 0.05775 = 0.06493 -0.01065 -0.03077 0.01625 O4 4 0.582644 1.588265 0.700070 11.00000 0.06693 0.04665 = 0.05148 0.01300 -0.00633 0.00283 C6 1 0.350058 -0.175585 0.238603 11.00000 0.05719 0.05159 = 0.02502 -0.01201 0.00023 0.01749 C66 1 0.591880 1.469160 0.733864 11.00000 0.04702 0.02334 = 0.02822 -0.00241 -0.00484 0.00495 C23 1 0.366275 0.726623 0.806889 11.00000 0.04971 0.03085 = 0.02998 -0.00854 0.00064 0.00402 C22 1 0.367336 0.598740 0.841161 11.00000 0.05195 0.02438 = 0.02516 0.00162 0.00934 0.00361 C43 1 0.609360 0.553606 0.298941 11.00000 0.03842 0.05646 = 0.02800 0.01768 0.01337 0.02363 C7 1 0.283379 -0.102451 0.228066 11.00000 0.04320 0.05091 = 0.04301 -0.00332 -0.01074 0.02002 AFIX 43 H7 2 0.238501 -0.137121 0.200134 11.00000 -1.20000 AFIX 0 C63 1 0.596135 1.202878 0.799248 11.00000 0.02895 0.02507 = 0.02691 -0.00252 -0.00178 -0.01237 C5 1 0.410393 -0.134076 0.287251 11.00000 0.04647 0.04828 = 0.02568 -0.00189 0.00375 0.02409 AFIX 43 H5 2 0.451367 -0.190851 0.297551 11.00000 -1.20000 AFIX 0 C44 1 0.550693 0.455752 0.310919 11.00000 0.04726 0.05902 = 0.03269 0.00943 -0.00130 0.01719 AFIX 43 H44 2 0.507246 0.474688 0.342691 11.00000 -1.20000 AFIX 0 C24 1 0.437153 0.793633 0.770671 11.00000 0.03863 0.02887 = 0.04431 0.00224 0.00927 0.00314 AFIX 43 H24 2 0.485968 0.753620 0.771710 11.00000 -1.20000 AFIX 0 C8 1 0.287480 0.028780 0.262432 11.00000 0.04134 0.04167 = 0.04070 0.01050 0.00820 0.01222 AFIX 43 H8 2 0.246553 0.085745 0.252331 11.00000 -1.20000 AFIX 0 C65 1 0.523816 1.383925 0.746393 11.00000 0.04297 0.03571 = 0.02573 -0.00057 -0.01431 0.00531 AFIX 43 H65 2 0.474604 1.414029 0.730891 11.00000 -1.20000 AFIX 0 C64 1 0.524607 1.256204 0.780708 11.00000 0.02769 0.03190 = 0.02968 -0.00613 0.00297 -0.00036 AFIX 43 H64 2 0.476482 1.206531 0.791189 11.00000 -1.20000 AFIX 0 C42 1 0.612085 0.695790 0.335226 11.00000 0.04223 0.06091 = 0.03449 0.00358 0.01105 0.02456 C48 1 0.676516 0.520028 0.252650 11.00000 0.03390 0.05846 = 0.03596 0.01173 0.01269 0.01414 AFIX 43 H48 2 0.719474 0.583821 0.245711 11.00000 -1.20000 AFIX 0 C67 1 0.666103 1.419410 0.753635 11.00000 0.02502 0.03715 = 0.04147 0.00520 0.00149 -0.01621 AFIX 43 H67 2 0.713655 1.471090 0.743690 11.00000 -1.20000 AFIX 0 C68 1 0.667582 1.290293 0.788702 11.00000 0.01984 0.02794 = 0.05055 -0.00149 -0.01034 0.00631 AFIX 43 H68 2 0.716434 1.260589 0.805606 11.00000 -1.20000 AFIX 0 C28 1 0.295208 0.793016 0.803146 11.00000 0.04857 0.03552 = 0.04028 -0.00143 0.00975 -0.00296 AFIX 43 H28 2 0.248967 0.752132 0.825982 11.00000 -1.20000 AFIX 0 C4 1 0.411980 -0.010424 0.321330 11.00000 0.04107 0.03636 = 0.03095 -0.00454 -0.00038 0.00520 AFIX 43 H4 2 0.455203 0.019612 0.353074 11.00000 -1.20000 AFIX 0 C46 1 0.617472 0.301883 0.231344 11.00000 0.07145 0.04523 = 0.03265 -0.00205 0.00775 0.01794 C27 1 0.291327 0.922409 0.765142 11.00000 0.04982 0.01707 = 0.03883 0.00218 -0.00496 0.00449 AFIX 43 H27 2 0.243250 0.964337 0.761588 11.00000 -1.20000 AFIX 0 C31 1 0.392116 0.273285 1.132304 11.00000 0.04873 0.03286 = 0.04283 0.00401 0.00839 -0.00572 AFIX 137 H31A 2 0.338230 0.291821 1.118246 11.00000 -1.50000 H31B 2 0.428532 0.346001 1.114045 11.00000 -1.50000 H31C 2 0.396235 0.265364 1.189077 11.00000 -1.50000 AFIX 0 O3 4 0.627861 0.177596 0.191919 11.00000 0.09592 0.07369 = 0.04407 -0.02022 0.02025 0.00899 C71 1 0.567773 0.743176 1.122995 11.00000 0.02782 0.02232 = 0.03567 -0.00642 0.01158 -0.02262 AFIX 137 H71A 2 0.562528 0.814998 1.085275 11.00000 -1.50000 H71B 2 0.621962 0.746136 1.142296 11.00000 -1.50000 H71C 2 0.531826 0.754133 1.166754 11.00000 -1.50000 AFIX 0 C51 1 0.609380 1.012444 0.619739 11.00000 0.05286 0.04285 = 0.03601 -0.00441 0.00534 -0.00804 AFIX 137 H51A 2 0.638225 0.945630 0.592429 11.00000 -1.50000 H51B 2 0.553083 0.997454 0.608712 11.00000 -1.50000 H51C 2 0.618262 1.005370 0.675988 11.00000 -1.50000 AFIX 0 C26 1 0.363795 0.984381 0.733033 11.00000 0.04143 0.02501 = 0.03627 -0.01053 0.00215 -0.00666 C11 1 0.349914 0.536126 0.635713 11.00000 0.07051 0.05892 = 0.03559 0.00947 0.01514 0.01301 AFIX 137 H11A 2 0.341614 0.464858 0.597169 11.00000 -1.50000 H11B 2 0.320409 0.512073 0.683251 11.00000 -1.50000 H11C 2 0.406039 0.548876 0.648043 11.00000 -1.50000 AFIX 0 C9 1 0.388370 -0.407457 0.227610 11.00000 0.07116 0.03841 = 0.04997 -0.00990 -0.00920 0.01952 AFIX 137 H9A 2 0.439328 -0.397671 0.201064 11.00000 -1.50000 H9B 2 0.362587 -0.494800 0.215541 11.00000 -1.50000 H9C 2 0.396357 -0.399546 0.284041 11.00000 -1.50000 AFIX 0 C15 1 0.303772 0.965349 0.506619 11.00000 0.05998 0.03801 = 0.03839 -0.00714 0.00877 0.01594 AFIX 137 H15A 2 0.354940 1.003020 0.488224 11.00000 -1.50000 H15B 2 0.305205 0.955011 0.563399 11.00000 -1.50000 H15C 2 0.262955 1.024957 0.492581 11.00000 -1.50000 AFIX 0 C33 1 0.393588 -0.164137 1.003274 11.00000 0.08493 0.05107 = 0.06296 -0.00279 0.00470 0.03317 AFIX 137 H33A 2 0.416342 -0.236230 0.974545 11.00000 -1.50000 H33B 2 0.337063 -0.185145 1.010217 11.00000 -1.50000 H33C 2 0.418899 -0.154092 1.054424 11.00000 -1.50000 AFIX 0 C14 1 0.284840 0.825651 0.467499 11.00000 0.03443 0.05380 = 0.02808 0.00146 -0.00382 0.01380 AFIX 23 H14A 2 0.288372 0.835658 0.410155 11.00000 -1.20000 H14B 2 0.230148 0.794026 0.480437 11.00000 -1.20000 AFIX 0 C10 1 0.320821 0.667251 0.601849 11.00000 0.06036 0.04000 = 0.03432 -0.00264 -0.00433 0.02090 AFIX 23 H10A 2 0.341393 0.742464 0.634703 11.00000 -1.20000 H10B 2 0.262709 0.663309 0.604786 11.00000 -1.20000 AFIX 0 C13 1 0.512821 0.691552 0.530688 11.00000 0.02092 0.03925 = 0.05946 0.01994 0.00424 -0.01138 AFIX 137 H13A 2 0.514382 0.615188 0.495546 11.00000 -1.50000 H13B 2 0.499846 0.660290 0.583525 11.00000 -1.50000 H13C 2 0.564293 0.741034 0.531033 11.00000 -1.50000 AFIX 0 C12 1 0.450813 0.781552 0.502766 11.00000 0.02555 0.05741 = 0.04872 0.00503 0.01099 0.00700 AFIX 23 H12A 2 0.465419 0.814915 0.450087 11.00000 -1.20000 H12B 2 0.450468 0.859198 0.538045 11.00000 -1.20000 AFIX 0 C25 1 0.431008 0.912314 0.736271 11.00000 0.03209 0.03359 = 0.04417 -0.00405 0.01811 -0.00572 AFIX 43 H25 2 0.476903 0.951068 0.711719 11.00000 -1.20000 AFIX 0 C45 1 0.552657 0.325238 0.276996 11.00000 0.05933 0.05529 = 0.03226 0.00265 -0.00650 0.01396 AFIX 43 H45 2 0.511582 0.258512 0.285490 11.00000 -1.20000 AFIX 0 C69 1 0.645313 1.675488 0.696852 11.00000 0.08310 0.05820 = 0.08130 0.01174 -0.00801 -0.01168 AFIX 137 H69A 2 0.679337 1.652293 0.653585 11.00000 -1.50000 H69B 2 0.674613 1.672992 0.745924 11.00000 -1.50000 H69C 2 0.627863 1.765028 0.688691 11.00000 -1.50000 AFIX 0 O2 4 0.368596 1.101821 0.693279 11.00000 0.04807 0.02001 = 0.05396 0.00556 -0.00725 -0.01036 C29 1 0.302053 1.186605 0.700065 11.00000 0.06773 0.02954 = 0.06307 0.01794 -0.01114 -0.01423 AFIX 137 H29A 2 0.258042 1.149260 0.668482 11.00000 -1.50000 H29B 2 0.318048 1.276240 0.681494 11.00000 -1.50000 H29C 2 0.285730 1.190807 0.754740 11.00000 -1.50000 AFIX 0 C49 1 0.577105 0.065334 0.212820 11.00000 0.08792 0.05378 = 0.03353 0.00659 0.01451 0.02745 AFIX 137 H49A 2 0.587793 -0.009919 0.179222 11.00000 -1.50000 H49B 2 0.522278 0.086750 0.206270 11.00000 -1.50000 H49C 2 0.586317 0.041917 0.267351 11.00000 -1.50000 AFIX 0 C75 1 0.762528 0.545763 0.950989 11.00000 0.04417 0.06052 = 0.04285 0.00572 0.00394 -0.00204 AFIX 137 H75A 2 0.758983 0.614096 0.910773 11.00000 -1.50000 H75B 2 0.745456 0.458745 0.929221 11.00000 -1.50000 H75C 2 0.817043 0.544565 0.968939 11.00000 -1.50000 AFIX 0 C47 1 0.678546 0.395735 0.218472 11.00000 0.05458 0.04122 = 0.03378 0.00847 0.01257 0.00681 AFIX 43 H47 2 0.721613 0.375541 0.186516 11.00000 -1.20000 AFIX 0 C73 1 0.590300 0.308998 1.000324 11.00000 0.10062 0.02902 = 0.05172 -0.00823 -0.00764 0.01330 AFIX 137 H73A 2 0.562242 0.228579 0.979663 11.00000 -1.50000 H73B 2 0.574742 0.322017 1.054642 11.00000 -1.50000 H73C 2 0.647069 0.299511 0.997789 11.00000 -1.50000 AFIX 0 C35 1 0.206128 0.025015 0.956158 11.00000 0.02768 0.06151 = 0.03340 -0.00331 0.00565 -0.01184 AFIX 137 H35A 2 0.227045 -0.046411 0.925349 11.00000 -1.50000 H35B 2 0.202827 0.104074 0.923437 11.00000 -1.50000 H35C 2 0.153608 -0.003872 0.975385 11.00000 -1.50000 AFIX 0 HKLF 4 REM appr5_2p13GPa in P11a #7 REM wR2 = 0.0711, GooF = S = 1.010, Restrained GooF = 0.986 for all data REM R1 = 0.0432 for 5324 Fo > 4sig(Fo) and 0.0749 for all 7038 data REM 666 parameters refined using 410 restraints END WGHT 0.0258 0.0000 REM Highest difference peak 0.926, deepest hole -0.971, 1-sigma level 0.143 Q1 1 0.5434 0.9447 0.4159 11.00000 0.05 0.93 Q2 1 0.4131 0.5265 0.4350 11.00000 0.05 0.79 Q3 1 0.6283 1.0829 0.4151 11.00000 0.05 0.79 Q4 1 0.6488 0.8981 0.4725 11.00000 0.05 0.74 Q5 1 0.5889 0.6734 0.9169 11.00000 0.05 0.73 Q6 1 0.6683 0.8157 0.9125 11.00000 0.05 0.72 Q7 1 0.5295 0.7511 0.9041 11.00000 0.05 0.71 Q8 1 0.2930 0.6020 0.4267 11.00000 0.05 0.67 Q9 1 0.3082 0.2930 0.9249 11.00000 0.05 0.64 Q10 1 0.4301 0.3430 0.9260 11.00000 0.05 0.64 Q11 1 0.5879 1.0409 0.4318 11.00000 0.05 0.64 Q12 1 0.3656 0.3130 0.8908 11.00000 0.05 0.64 Q13 1 0.5638 0.5771 0.4241 11.00000 0.05 0.63 Q14 1 0.6300 0.7832 1.0708 11.00000 0.05 0.62 Q15 1 0.5853 0.8445 1.0887 11.00000 0.05 0.60 Q16 1 0.5977 1.0688 0.4670 11.00000 0.05 0.59 Q17 1 0.6253 0.9181 0.3424 11.00000 0.05 0.59 Q18 1 0.5738 0.8214 0.8420 11.00000 0.05 0.59 Q19 1 0.3065 0.5536 0.4842 11.00000 0.05 0.58 Q20 1 0.3682 0.5978 0.4159 11.00000 0.05 0.58 ; _shelx_res_checksum 54563 _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 1.599 _oxdiff_exptl_absorpt_empirical_full_min 0.802 loop_ _space_group_symop_operation_xyz 'x, y, z' 'x+1/2, y, -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 0.36568(6) 0.30543(9) 0.92392(5) 0.0393(5) Uani 1 1 d . . . . . Au3 Au 0.61860(7) 0.98226(10) 0.41557(5) 0.0410(5) Uani 1 1 d . . . . . Au4 Au 0.59885(7) 0.78045(9) 0.91477(5) 0.0381(5) Uani 1 1 d . . . . . Au1 Au 0.34701(6) 0.50104(10) 0.42817(4) 0.0387(5) Uani 1 1 d . . . . . P3 P 0.6120(6) 1.1775(10) 0.4870(3) 0.035(3) Uani 1 1 d . U . . . P4 P 0.6048(6) 0.5937(10) 0.9923(3) 0.031(3) Uani 1 1 d . U . . . P1 P 0.3514(7) 0.7002(10) 0.4988(3) 0.037(4) Uani 1 1 d . U . . . P2 P 0.3611(7) 0.1123(10) 0.9985(3) 0.034(4) Uani 1 1 d . U . . . C21 C 0.367(2) 0.486(4) 0.8684(11) 0.042(10) Uani 1 1 d . U . . . C2 C 0.350(2) 0.212(3) 0.3446(11) 0.038(8) Uani 1 1 d . U . . . C1 C 0.3479(19) 0.327(4) 0.3729(13) 0.046(10) Uani 1 1 d . U . . . C62 C 0.6043(18) 1.078(3) 0.8339(11) 0.026(8) Uani 1 1 d . U . . . C61 C 0.5997(18) 0.958(3) 0.8595(11) 0.029(9) Uani 1 1 d . U . . . C3 C 0.349(2) 0.073(4) 0.3089(11) 0.035(7) Uani 1 1 d . U . . . C41 C 0.615(2) 0.803(4) 0.3617(13) 0.051(11) Uani 1 1 d . U . . . C74 C 0.7079(17) 0.578(3) 1.0219(11) 0.037(9) Uani 1 1 d . U . . . H74A H 0.728467 0.661719 1.046672 0.045 Uiso 1 1 calc R U . . . H74B H 0.709755 0.506081 1.061138 0.045 Uiso 1 1 calc R U . . . C30 C 0.4131(15) 0.142(2) 1.0939(10) 0.025(7) Uani 1 1 d . U . . . H30A H 0.398776 0.067625 1.129684 0.030 Uiso 1 1 calc R U . . . H30B H 0.470581 0.145022 1.085155 0.030 Uiso 1 1 calc R U . . . C34 C 0.2619(18) 0.059(3) 1.0270(12) 0.037(8) Uani 1 1 d . U . . . H34A H 0.263417 -0.020534 1.060620 0.045 Uiso 1 1 calc R U . . . H34B H 0.239864 0.130194 1.058171 0.045 Uiso 1 1 calc R U . . . C70 C 0.5469(17) 0.605(3) 1.0822(11) 0.036(9) Uani 1 1 d . U . . . H70A H 0.490075 0.596457 1.069671 0.043 Uiso 1 1 calc R U . . . H70B H 0.558533 0.532178 1.118050 0.043 Uiso 1 1 calc R U . . . C32 C 0.407(2) -0.031(3) 0.9562(11) 0.050(9) Uani 1 1 d . U . . . H32A H 0.386523 -0.045859 0.902747 0.060 Uiso 1 1 calc R U . . . H32B H 0.464443 -0.008887 0.952001 0.060 Uiso 1 1 calc R U . . . C52 C 0.5073(19) 1.222(3) 0.4858(13) 0.050(10) Uani 1 1 d . U . . . H52A H 0.503275 1.288981 0.444279 0.060 Uiso 1 1 calc R U . . . H52B H 0.475791 1.141139 0.468063 0.060 Uiso 1 1 calc R U . . . C54 C 0.6738(18) 1.327(3) 0.4575(11) 0.036(7) Uani 1 1 d . U . . . H54A H 0.729675 1.311019 0.467142 0.044 Uiso 1 1 calc R U . . . H54B H 0.667393 1.341093 0.400826 0.044 Uiso 1 1 calc R U . . . C50 C 0.6389(18) 1.154(3) 0.5913(10) 0.040(10) Uani 1 1 d . U . . . H50A H 0.696714 1.165382 0.597192 0.049 Uiso 1 1 calc R U . . . H50B H 0.615128 1.221571 0.623736 0.049 Uiso 1 1 calc R U . . . C72 C 0.5697(19) 0.430(3) 0.9515(12) 0.052(10) Uani 1 1 d . U . . . H72A H 0.511801 0.427494 0.945730 0.062 Uiso 1 1 calc R U . . . H72B H 0.592330 0.421132 0.898719 0.062 Uiso 1 1 calc R U . . . C55 C 0.654(3) 1.452(3) 0.5003(13) 0.057(15) Uani 1 1 d . U . . . H55A H 0.601493 1.475938 0.485425 0.085 Uiso 1 1 calc R U . . . H55B H 0.692713 1.525065 0.486553 0.085 Uiso 1 1 calc R U . . . H55C H 0.655892 1.436710 0.556700 0.085 Uiso 1 1 calc R U . . . C53 C 0.4675(19) 1.270(4) 0.5521(14) 0.091(18) Uani 1 1 d . U . . . H53A H 0.415508 1.296148 0.536412 0.137 Uiso 1 1 calc R U . . . H53B H 0.498165 1.347096 0.573667 0.137 Uiso 1 1 calc R U . . . H53C H 0.461657 1.199977 0.591646 0.137 Uiso 1 1 calc R U . . . O1 O 0.3403(17) -0.306(3) 0.2018(10) 0.071(9) Uani 1 1 d . U . . . O4 O 0.5826(17) 1.588(3) 0.7001(10) 0.055(9) Uani 1 1 d . U . . . C6 C 0.350(2) -0.176(3) 0.2386(12) 0.044(7) Uani 1 1 d . U . . . C66 C 0.592(2) 1.469(3) 0.7339(12) 0.033(8) Uani 1 1 d . U . . . C23 C 0.366(2) 0.727(4) 0.8069(13) 0.037(8) Uani 1 1 d . U . . . C22 C 0.367(2) 0.599(3) 0.8412(11) 0.034(8) Uani 1 1 d . U . . . C43 C 0.609(2) 0.554(4) 0.2989(13) 0.040(9) Uani 1 1 d . U . . . C7 C 0.2834(19) -0.102(3) 0.2281(12) 0.045(8) Uani 1 1 d . U . . . H7 H 0.238501 -0.137121 0.200134 0.054 Uiso 1 1 calc R U . . . C63 C 0.596(2) 1.203(3) 0.7992(12) 0.028(7) Uani 1 1 d . U . . . C5 C 0.4104(17) -0.134(3) 0.2873(11) 0.039(8) Uani 1 1 d . U . . . H5 H 0.451367 -0.190851 0.297551 0.047 Uiso 1 1 calc R U . . . C44 C 0.551(2) 0.456(3) 0.3109(13) 0.046(9) Uani 1 1 d . U . . . H44 H 0.507246 0.474688 0.342691 0.055 Uiso 1 1 calc R U . . . C24 C 0.437(2) 0.794(3) 0.7707(12) 0.037(8) Uani 1 1 d . U . . . H24 H 0.485968 0.753620 0.771710 0.045 Uiso 1 1 calc R U . . . C8 C 0.287(2) 0.029(3) 0.2624(12) 0.041(8) Uani 1 1 d . U . . . H8 H 0.246553 0.085745 0.252331 0.049 Uiso 1 1 calc R U . . . C65 C 0.5238(19) 1.384(3) 0.7464(10) 0.035(8) Uani 1 1 d . U . . . H65 H 0.474604 1.414029 0.730891 0.042 Uiso 1 1 calc R U . . . C64 C 0.5246(16) 1.256(3) 0.7807(10) 0.030(7) Uani 1 1 d . U . . . H64 H 0.476482 1.206531 0.791189 0.036 Uiso 1 1 calc R U . . . C42 C 0.612(2) 0.696(4) 0.3352(12) 0.045(9) Uani 1 1 d . U . . . C48 C 0.6765(17) 0.520(3) 0.2526(10) 0.042(8) Uani 1 1 d . U . . . H48 H 0.719474 0.583821 0.245711 0.051 Uiso 1 1 calc R U . . . C67 C 0.6661(19) 1.419(3) 0.7536(11) 0.035(8) Uani 1 1 d . U . . . H67 H 0.713655 1.471090 0.743690 0.042 Uiso 1 1 calc R U . . . C68 C 0.668(2) 1.290(3) 0.7887(12) 0.033(8) Uani 1 1 d . U . . . H68 H 0.716434 1.260589 0.805606 0.039 Uiso 1 1 calc R U . . . C28 C 0.2952(19) 0.793(3) 0.8031(11) 0.042(8) Uani 1 1 d . U . . . H28 H 0.248967 0.752132 0.825982 0.050 Uiso 1 1 calc R U . . . C4 C 0.4120(17) -0.010(3) 0.3213(11) 0.036(8) Uani 1 1 d . U . . . H4 H 0.455203 0.019612 0.353074 0.043 Uiso 1 1 calc R U . . . C46 C 0.617(3) 0.302(4) 0.2313(14) 0.049(9) Uani 1 1 d . U . . . C27 C 0.291(2) 0.922(3) 0.7651(12) 0.035(8) Uani 1 1 d . U . . . H27 H 0.243250 0.964337 0.761588 0.042 Uiso 1 1 calc R U . . . C31 C 0.392(2) 0.273(3) 1.1323(11) 0.042(12) Uani 1 1 d . U . . . H31A H 0.338230 0.291821 1.118246 0.063 Uiso 1 1 calc R U . . . H31B H 0.428532 0.346001 1.114045 0.063 Uiso 1 1 calc R U . . . H31C H 0.396235 0.265364 1.189077 0.063 Uiso 1 1 calc R U . . . O3 O 0.6279(19) 0.178(3) 0.1919(10) 0.071(10) Uani 1 1 d . U . . . C71 C 0.5678(17) 0.743(3) 1.1230(11) 0.030(11) Uani 1 1 d . U . . . H71A H 0.562528 0.814998 1.085275 0.045 Uiso 1 1 calc R U . . . H71B H 0.621962 0.746136 1.142296 0.045 Uiso 1 1 calc R U . . . H71C H 0.531826 0.754133 1.166754 0.045 Uiso 1 1 calc R U . . . C51 C 0.609(2) 1.012(3) 0.6197(12) 0.044(12) Uani 1 1 d . U . . . H51A H 0.638225 0.945630 0.592429 0.067 Uiso 1 1 calc R U . . . H51B H 0.553083 0.997454 0.608712 0.067 Uiso 1 1 calc R U . . . H51C H 0.618262 1.005370 0.675988 0.067 Uiso 1 1 calc R U . . . C26 C 0.364(2) 0.984(4) 0.7330(13) 0.035(8) Uani 1 1 d . U . . . C11 C 0.350(2) 0.536(3) 0.6357(12) 0.055(14) Uani 1 1 d . U . . . H11A H 0.341614 0.464858 0.597169 0.082 Uiso 1 1 calc R U . . . H11B H 0.320409 0.512073 0.683251 0.082 Uiso 1 1 calc R U . . . H11C H 0.406039 0.548876 0.648043 0.082 Uiso 1 1 calc R U . . . C9 C 0.388(2) -0.407(3) 0.2276(12) 0.052(12) Uani 1 1 d . U . . . H9A H 0.439328 -0.397671 0.201064 0.079 Uiso 1 1 calc R U . . . H9B H 0.362587 -0.494800 0.215541 0.079 Uiso 1 1 calc R U . . . H9C H 0.396357 -0.399546 0.284041 0.079 Uiso 1 1 calc R U . . . C15 C 0.304(2) 0.965(3) 0.5066(11) 0.045(13) Uani 1 1 d . U . . . H15A H 0.354940 1.003020 0.488224 0.067 Uiso 1 1 calc R U . . . H15B H 0.305205 0.955011 0.563399 0.067 Uiso 1 1 calc R U . . . H15C H 0.262955 1.024957 0.492581 0.067 Uiso 1 1 calc R U . . . C33 C 0.394(3) -0.164(3) 1.0033(13) 0.065(14) Uani 1 1 d . U . . . H33A H 0.416342 -0.236230 0.974545 0.098 Uiso 1 1 calc R U . . . H33B H 0.337063 -0.185145 1.010217 0.098 Uiso 1 1 calc R U . . . H33C H 0.418899 -0.154092 1.054424 0.098 Uiso 1 1 calc R U . . . C14 C 0.2848(18) 0.826(3) 0.4675(11) 0.038(9) Uani 1 1 d . U . . . H14A H 0.288372 0.835658 0.410155 0.046 Uiso 1 1 calc R U . . . H14B H 0.230148 0.794026 0.480437 0.046 Uiso 1 1 calc R U . . . C10 C 0.3208(17) 0.667(3) 0.6018(10) 0.044(10) Uani 1 1 d . U . . . H10A H 0.341393 0.742464 0.634703 0.053 Uiso 1 1 calc R U . . . H10B H 0.262709 0.663309 0.604786 0.053 Uiso 1 1 calc R U . . . C13 C 0.5128(17) 0.692(3) 0.5307(13) 0.040(9) Uani 1 1 d . U . . . H13A H 0.514382 0.615188 0.495546 0.061 Uiso 1 1 calc R U . . . H13B H 0.499846 0.660290 0.583525 0.061 Uiso 1 1 calc R U . . . H13C H 0.564293 0.741034 0.531033 0.061 Uiso 1 1 calc R U . . . C12 C 0.4508(18) 0.782(3) 0.5028(12) 0.044(10) Uani 1 1 d . U . . . H12A H 0.465419 0.814915 0.450087 0.052 Uiso 1 1 calc R U . . . H12B H 0.450468 0.859198 0.538045 0.052 Uiso 1 1 calc R U . . . C25 C 0.4310(19) 0.912(3) 0.7363(12) 0.037(8) Uani 1 1 d . U . . . H25 H 0.476903 0.951068 0.711719 0.044 Uiso 1 1 calc R U . . . C45 C 0.5527(19) 0.325(3) 0.2770(12) 0.049(9) Uani 1 1 d . U . . . H45 H 0.511582 0.258512 0.285490 0.058 Uiso 1 1 calc R U . . . C69 C 0.645(3) 1.675(4) 0.6969(18) 0.075(14) Uani 1 1 d . U . . . H69A H 0.679337 1.652293 0.653585 0.112 Uiso 1 1 calc R U . . . H69B H 0.674613 1.672992 0.745924 0.112 Uiso 1 1 calc R U . . . H69C H 0.627863 1.765028 0.688691 0.112 Uiso 1 1 calc R U . . . O2 O 0.3686(14) 1.102(2) 0.6933(9) 0.041(7) Uani 1 1 d . U . . . C29 C 0.302(2) 1.187(4) 0.7001(13) 0.054(10) Uani 1 1 d . U . . . H29A H 0.258042 1.149260 0.668482 0.081 Uiso 1 1 calc R U . . . H29B H 0.318048 1.276240 0.681494 0.081 Uiso 1 1 calc R U . . . H29C H 0.285730 1.190807 0.754740 0.081 Uiso 1 1 calc R U . . . C49 C 0.577(2) 0.065(4) 0.2128(13) 0.057(14) Uani 1 1 d . U . . . H49A H 0.587793 -0.009919 0.179222 0.086 Uiso 1 1 calc R U . . . H49B H 0.522278 0.086750 0.206270 0.086 Uiso 1 1 calc R U . . . H49C H 0.586317 0.041917 0.267351 0.086 Uiso 1 1 calc R U . . . C75 C 0.763(2) 0.546(3) 0.9510(12) 0.049(13) Uani 1 1 d . U . . . H75A H 0.758983 0.614096 0.910773 0.074 Uiso 1 1 calc R U . . . H75B H 0.745456 0.458745 0.929221 0.074 Uiso 1 1 calc R U . . . H75C H 0.817043 0.544565 0.968939 0.074 Uiso 1 1 calc R U . . . C47 C 0.679(2) 0.396(3) 0.2185(13) 0.043(9) Uani 1 1 d . U . . . H47 H 0.721613 0.375541 0.186516 0.052 Uiso 1 1 calc R U . . . C73 C 0.590(3) 0.309(3) 1.0003(11) 0.060(15) Uani 1 1 d . U . . . H73A H 0.562242 0.228579 0.979663 0.090 Uiso 1 1 calc R U . . . H73B H 0.574742 0.322017 1.054642 0.090 Uiso 1 1 calc R U . . . H73C H 0.647069 0.299511 0.997789 0.090 Uiso 1 1 calc R U . . . C35 C 0.2061(17) 0.025(3) 0.9562(10) 0.042(10) Uani 1 1 d . U . . . H35A H 0.227045 -0.046411 0.925349 0.062 Uiso 1 1 calc R U . . . H35B H 0.202827 0.104074 0.923437 0.062 Uiso 1 1 calc R U . . . H35C H 0.153608 -0.003872 0.975385 0.062 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 0.0434(11) 0.0405(11) 0.0345(5) 0.0045(4) -0.0015(5) 0.0080(11) Au3 0.0485(11) 0.0406(11) 0.0342(5) -0.0022(5) -0.0037(5) 0.0054(11) Au4 0.0452(10) 0.0367(10) 0.0333(5) 0.0049(5) 0.0013(5) 0.0094(10) Au1 0.0445(10) 0.0395(10) 0.0327(5) -0.0046(4) 0.0017(5) 0.0081(10) P3 0.036(8) 0.037(7) 0.030(3) -0.001(3) -0.007(3) 0.000(7) P4 0.034(7) 0.030(7) 0.028(3) -0.001(3) -0.002(3) 0.004(7) P1 0.039(8) 0.042(7) 0.030(3) 0.000(3) 0.001(3) 0.014(8) P2 0.037(8) 0.035(7) 0.029(3) 0.001(3) -0.004(3) 0.004(7) C21 0.05(2) 0.05(2) 0.028(11) -0.005(11) -0.003(11) 0.01(2) C2 0.039(19) 0.038(18) 0.038(11) 0.000(11) 0.006(11) 0.010(17) C1 0.03(2) 0.06(2) 0.049(13) 0.006(13) 0.002(11) 0.02(2) C62 0.015(17) 0.029(17) 0.032(10) -0.001(10) -0.002(9) -0.006(16) C61 0.03(2) 0.028(19) 0.029(11) 0.001(11) -0.001(10) -0.015(19) C3 0.048(17) 0.039(15) 0.020(9) -0.002(9) 0.011(10) 0.007(15) C41 0.04(2) 0.08(2) 0.041(13) -0.014(14) -0.001(12) 0.03(2) C74 0.04(2) 0.04(2) 0.028(10) -0.010(10) -0.004(12) -0.013(19) C30 0.015(16) 0.028(16) 0.030(9) -0.001(9) -0.011(9) -0.010(15) C34 0.040(19) 0.037(17) 0.033(10) 0.003(10) 0.004(11) -0.007(17) C70 0.03(2) 0.04(2) 0.039(11) 0.015(11) -0.007(11) -0.011(19) C32 0.07(2) 0.038(17) 0.047(11) -0.002(11) -0.002(12) 0.017(17) C52 0.03(2) 0.08(2) 0.039(12) -0.005(13) 0.004(13) -0.02(2) C54 0.031(13) 0.038(13) 0.039(9) -0.002(9) -0.001(9) -0.002(11) C50 0.03(2) 0.06(2) 0.033(11) -0.015(11) -0.004(10) 0.01(2) C72 0.07(2) 0.04(2) 0.046(12) -0.010(12) -0.002(13) 0.01(2) C55 0.08(4) 0.01(2) 0.078(17) 0.005(14) -0.002(17) 0.00(3) C53 0.05(3) 0.17(4) 0.062(16) 0.003(18) 0.011(14) 0.05(4) O1 0.09(2) 0.058(17) 0.065(10) -0.011(10) -0.031(11) 0.016(17) O4 0.07(2) 0.047(18) 0.051(10) 0.013(10) -0.006(11) 0.003(18) C6 0.057(17) 0.052(16) 0.025(10) -0.012(10) 0.000(10) 0.017(15) C66 0.05(2) 0.023(17) 0.028(9) -0.002(10) -0.005(10) 0.005(16) C23 0.050(18) 0.031(16) 0.030(10) -0.009(10) 0.001(10) 0.004(16) C22 0.05(2) 0.024(17) 0.025(10) 0.002(9) 0.009(10) 0.004(17) C43 0.038(19) 0.056(18) 0.028(10) 0.018(11) 0.013(11) 0.024(16) C7 0.043(18) 0.051(17) 0.043(11) -0.003(11) -0.011(11) 0.020(16) C63 0.029(17) 0.025(16) 0.027(9) -0.003(9) -0.002(11) -0.012(15) C5 0.046(18) 0.048(16) 0.026(10) -0.002(10) 0.004(10) 0.024(15) C44 0.05(2) 0.06(2) 0.033(11) 0.009(12) -0.001(12) 0.017(18) C24 0.04(2) 0.029(17) 0.044(11) 0.002(10) 0.009(11) 0.003(17) C8 0.041(18) 0.042(17) 0.041(11) 0.011(11) 0.008(11) 0.012(16) C65 0.04(2) 0.036(18) 0.026(9) -0.001(10) -0.014(11) 0.005(17) C64 0.028(17) 0.032(16) 0.030(9) -0.006(9) 0.003(9) 0.000(16) C42 0.04(2) 0.06(2) 0.034(11) 0.004(12) 0.011(11) 0.025(19) C48 0.034(18) 0.058(18) 0.036(11) 0.012(11) 0.013(10) 0.014(17) C67 0.025(19) 0.037(18) 0.041(11) 0.005(11) 0.001(11) -0.016(17) C68 0.020(17) 0.028(17) 0.051(11) -0.001(11) -0.010(11) 0.006(16) C28 0.05(2) 0.036(17) 0.040(11) -0.001(10) 0.010(11) -0.003(17) C4 0.041(18) 0.036(16) 0.031(9) -0.005(10) 0.000(10) 0.005(16) C46 0.07(2) 0.045(19) 0.033(10) -0.002(11) 0.008(12) 0.018(18) C27 0.05(2) 0.017(16) 0.039(11) 0.002(10) -0.005(11) 0.004(17) C31 0.05(3) 0.03(2) 0.043(12) 0.004(12) 0.008(12) -0.01(2) O3 0.10(2) 0.07(2) 0.044(10) -0.020(11) 0.020(11) 0.01(2) C71 0.03(3) 0.02(2) 0.036(12) -0.006(10) 0.012(11) -0.02(2) C51 0.05(3) 0.04(3) 0.036(12) -0.004(13) 0.005(13) -0.01(3) C26 0.041(18) 0.025(16) 0.036(11) -0.011(10) 0.002(10) -0.007(16) C11 0.07(3) 0.06(3) 0.036(12) 0.009(12) 0.015(13) 0.01(3) C9 0.07(3) 0.04(2) 0.050(13) -0.010(12) -0.009(13) 0.02(2) C15 0.06(3) 0.04(2) 0.038(13) -0.007(12) 0.009(12) 0.02(3) C33 0.08(3) 0.05(3) 0.063(17) -0.003(14) 0.005(16) 0.03(3) C14 0.03(2) 0.05(2) 0.028(10) 0.001(11) -0.004(10) 0.01(2) C10 0.06(2) 0.040(19) 0.034(11) -0.003(11) -0.004(11) 0.021(19) C13 0.021(19) 0.039(19) 0.059(12) 0.020(11) 0.004(11) -0.011(18) C12 0.03(2) 0.06(2) 0.049(13) 0.005(12) 0.011(11) 0.01(2) C25 0.032(19) 0.034(17) 0.044(11) -0.004(11) 0.018(11) -0.006(17) C45 0.06(2) 0.055(19) 0.032(11) 0.003(11) -0.007(11) 0.014(18) C69 0.08(3) 0.06(2) 0.081(17) 0.012(17) -0.008(17) -0.01(2) O2 0.048(17) 0.020(15) 0.054(10) 0.006(9) -0.007(9) -0.010(15) C29 0.07(2) 0.030(18) 0.063(13) 0.018(12) -0.011(13) -0.014(19) C49 0.09(3) 0.05(3) 0.034(12) 0.007(13) 0.015(14) 0.03(3) C75 0.04(3) 0.06(3) 0.043(13) 0.006(13) 0.004(12) 0.00(3) C47 0.05(2) 0.041(19) 0.034(10) 0.008(11) 0.013(12) 0.007(18) C73 0.10(4) 0.03(3) 0.052(15) -0.008(14) -0.008(17) 0.01(3) C35 0.03(2) 0.06(2) 0.033(11) -0.003(11) 0.006(11) -0.01(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0013 0.0009 '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' Au Au -0.6570 6.0260 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0058 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.0671 0.0586 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 174.1(6) . . ? C41 Au3 P3 173.5(11) . . ? C61 Au4 P4 172.2(8) . . ? C1 Au1 P1 176.3(7) . . ? C52 P3 Au3 107.2(12) . . ? C54 P3 Au3 119.2(7) . . ? C54 P3 C52 107.7(13) . . ? C54 P3 C50 103.6(15) . . ? C50 P3 Au3 111.7(9) . . ? C50 P3 C52 106.8(11) . . ? C74 P4 Au4 108.8(11) . . ? C74 P4 C72 106.1(11) . . ? C70 P4 Au4 112.2(7) . . ? C70 P4 C74 107.1(10) . . ? C70 P4 C72 103.3(15) . . ? C72 P4 Au4 118.6(7) . . ? C14 P1 Au1 117.0(9) . . ? C14 P1 C10 102.8(9) . . ? C10 P1 Au1 110.2(10) . . ? C12 P1 Au1 112.2(7) . . ? C12 P1 C14 107.3(14) . . ? C12 P1 C10 106.5(12) . . ? C30 P2 Au2 110.8(10) . . ? C34 P2 Au2 112.0(8) . . ? C34 P2 C30 103.6(11) . . ? C34 P2 C32 108.2(16) . . ? C32 P2 Au2 116.7(9) . . ? C32 P2 C30 104.4(10) . . ? C22 C21 Au2 175(2) . . ? C1 C2 C3 178(3) . . ? C2 C1 Au1 174(2) . . ? C61 C62 C63 170(3) . . ? C62 C61 Au4 172(2) . . ? C8 C3 C2 120(2) . . ? C8 C3 C4 119(3) . . ? C4 C3 C2 121(3) . . ? C42 C41 Au3 176(3) . . ? P4 C74 H74A 109.1 . . ? P4 C74 H74B 109.1 . . ? H74A C74 H74B 107.8 . . ? C75 C74 P4 112.6(15) . . ? C75 C74 H74A 109.1 . . ? C75 C74 H74B 109.1 . . ? P2 C30 H30A 109.2 . . ? P2 C30 H30B 109.2 . . ? H30A C30 H30B 107.9 . . ? C31 C30 P2 112.2(13) . . ? C31 C30 H30A 109.2 . . ? C31 C30 H30B 109.2 . . ? P2 C34 H34A 108.9 . . ? P2 C34 H34B 108.9 . . ? H34A C34 H34B 107.7 . . ? C35 C34 P2 113.5(16) . . ? C35 C34 H34A 108.9 . . ? C35 C34 H34B 108.9 . . ? P4 C70 H70A 109.7 . . ? P4 C70 H70B 109.7 . . ? H70A C70 H70B 108.2 . . ? C71 C70 P4 110(2) . . ? C71 C70 H70A 109.7 . . ? C71 C70 H70B 109.7 . . ? P2 C32 H32A 108.5 . . ? P2 C32 H32B 108.5 . . ? H32A C32 H32B 107.5 . . ? C33 C32 P2 115.1(17) . . ? C33 C32 H32A 108.5 . . ? C33 C32 H32B 108.5 . . ? P3 C52 H52A 106.4 . . ? P3 C52 H52B 106.4 . . ? H52A C52 H52B 106.5 . . ? C53 C52 P3 123.8(19) . . ? C53 C52 H52A 106.4 . . ? C53 C52 H52B 106.4 . . ? P3 C54 H54A 108.8 . . ? P3 C54 H54B 108.8 . . ? H54A C54 H54B 107.7 . . ? C55 C54 P3 114(2) . . ? C55 C54 H54A 108.8 . . ? C55 C54 H54B 108.8 . . ? P3 C50 H50A 109.5 . . ? P3 C50 H50B 109.5 . . ? H50A C50 H50B 108.1 . . ? C51 C50 P3 111(2) . . ? C51 C50 H50A 109.5 . . ? C51 C50 H50B 109.5 . . ? P4 C72 H72A 108.5 . . ? P4 C72 H72B 108.5 . . ? H72A C72 H72B 107.5 . . ? C73 C72 P4 115.0(19) . . ? C73 C72 H72A 108.5 . . ? C73 C72 H72B 108.5 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55B 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53B 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C9 O1 C6 118(2) . . ? C69 O4 C66 118(3) . . ? C7 C6 O1 112(3) . . ? C5 C6 O1 125(2) . . ? C5 C6 C7 122(3) . . ? O4 C66 C65 118(3) . . ? O4 C66 C67 125(4) . . ? C65 C66 C67 117(3) . . ? C22 C23 C24 122(2) . . ? C22 C23 C28 121(3) . . ? C28 C23 C24 117(3) . . ? C21 C22 C23 177(4) . . ? C44 C43 C42 125(2) . . ? C44 C43 C48 118(3) . . ? C48 C43 C42 117(3) . . ? C6 C7 H7 122.1 . . ? C6 C7 C8 116(3) . . ? C8 C7 H7 122.1 . . ? C62 C63 C68 118(2) . . ? C64 C63 C62 125(4) . . ? C64 C63 C68 117(3) . . ? C6 C5 H5 119.8 . . ? C6 C5 C4 120(2) . . ? C4 C5 H5 119.8 . . ? C43 C44 H44 118.8 . . ? C43 C44 C45 122(3) . . ? C45 C44 H44 118.8 . . ? C23 C24 H24 120.7 . . ? C25 C24 C23 119(2) . . ? C25 C24 H24 120.7 . . ? C3 C8 C7 122(2) . . ? C3 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C66 C65 H65 118.0 . . ? C66 C65 C64 124(3) . . ? C64 C65 H65 118.0 . . ? C63 C64 C65 120(3) . . ? C63 C64 H64 119.8 . . ? C65 C64 H64 119.8 . . ? C41 C42 C43 179(4) . . ? C43 C48 H48 119.7 . . ? C47 C48 C43 121(3) . . ? C47 C48 H48 119.7 . . ? C66 C67 H67 120.4 . . ? C66 C67 C68 119(3) . . ? C68 C67 H67 120.4 . . ? C63 C68 H68 118.9 . . ? C67 C68 C63 122(2) . . ? C67 C68 H68 118.9 . . ? C23 C28 H28 119.0 . . ? C23 C28 C27 122(3) . . ? C27 C28 H28 119.0 . . ? C3 C4 H4 120.0 . . ? C5 C4 C3 120(3) . . ? C5 C4 H4 120.0 . . ? C45 C46 O3 124(4) . . ? C47 C46 O3 113(3) . . ? C47 C46 C45 123(3) . . ? C28 C27 H27 121.2 . . ? C26 C27 C28 118(2) . . ? C26 C27 H27 121.2 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C49 O3 C46 118(3) . . ? C70 C71 H71A 109.5 . . ? C70 C71 H71B 109.5 . . ? C70 C71 H71C 109.5 . . ? H71A C71 H71B 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51B 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C25 C26 C27 118(3) . . ? O2 C26 C27 124(2) . . ? O2 C26 C25 118(3) . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? 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 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? 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 . . ? P1 C14 H14A 108.9 . . ? P1 C14 H14B 108.9 . . ? C15 C14 P1 113.2(18) . . ? C15 C14 H14A 108.9 . . ? C15 C14 H14B 108.9 . . ? H14A C14 H14B 107.8 . . ? P1 C10 H10A 108.8 . . ? P1 C10 H10B 108.8 . . ? C11 C10 P1 113.8(13) . . ? C11 C10 H10A 108.8 . . ? C11 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? P1 C12 H12A 108.8 . . ? P1 C12 H12B 108.8 . . ? C13 C12 P1 114(2) . . ? C13 C12 H12A 108.8 . . ? C13 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? C24 C25 C26 127(3) . . ? C24 C25 H25 116.7 . . ? C26 C25 H25 116.7 . . ? C44 C45 H45 121.6 . . ? C46 C45 C44 117(4) . . ? C46 C45 H45 121.6 . . ? O4 C69 H69A 109.5 . . ? O4 C69 H69B 109.5 . . ? O4 C69 H69C 109.5 . . ? H69A C69 H69B 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C26 O2 C29 118(2) . . ? 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 . . ? O3 C49 H49A 109.5 . . ? O3 C49 H49B 109.5 . . ? O3 C49 H49C 109.5 . . ? H49A C49 H49B 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C74 C75 H75A 109.5 . . ? C74 C75 H75B 109.5 . . ? C74 C75 H75C 109.5 . . ? H75A C75 H75B 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C48 C47 H47 120.3 . . ? C46 C47 C48 119(3) . . ? C46 C47 H47 120.3 . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73B 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 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 2.280(9) . ? Au2 C21 2.01(3) . ? Au3 P3 2.282(8) . ? Au3 C41 1.99(4) . ? Au4 P4 2.267(8) . ? Au4 C61 1.99(3) . ? Au1 P1 2.295(9) . ? Au1 C1 1.96(3) . ? P3 C52 1.83(3) . ? P3 C54 1.81(3) . ? P3 C50 1.827(18) . ? P4 C74 1.81(3) . ? P4 C70 1.80(2) . ? P4 C72 1.82(3) . ? P1 C14 1.799(19) . ? P1 C10 1.83(2) . ? P1 C12 1.80(4) . ? P2 C30 1.84(2) . ? P2 C34 1.77(4) . ? P2 C32 1.80(2) . ? C21 C22 1.21(4) . ? C2 C1 1.23(4) . ? C2 C3 1.50(4) . ? C62 C61 1.25(4) . ? C62 C63 1.38(4) . ? C3 C8 1.33(5) . ? C3 C4 1.40(3) . ? C41 C42 1.14(5) . ? C74 H74A 0.9700 . ? C74 H74B 0.9700 . ? C74 C75 1.55(3) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 C31 1.51(3) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 C35 1.53(3) . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C70 C71 1.54(4) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 C33 1.54(4) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C52 C53 1.40(2) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C54 C55 1.49(3) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C50 C51 1.53(5) . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C72 C73 1.51(3) . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? O1 C6 1.43(4) . ? O1 C9 1.39(2) . ? O4 C66 1.33(3) . ? O4 C69 1.31(5) . ? C6 C7 1.38(3) . ? C6 C5 1.34(4) . ? C66 C65 1.38(4) . ? C66 C67 1.40(3) . ? C23 C22 1.39(4) . ? C23 C24 1.45(5) . ? C23 C28 1.40(3) . ? C43 C44 1.34(5) . ? C43 C42 1.53(5) . ? C43 C48 1.42(3) . ? C7 H7 0.9300 . ? C7 C8 1.42(4) . ? C63 C64 1.37(3) . ? C63 C68 1.44(5) . ? C5 H5 0.9300 . ? C5 C4 1.35(3) . ? C44 H44 0.9300 . ? C44 C45 1.41(4) . ? C24 H24 0.9300 . ? C24 C25 1.32(3) . ? C8 H8 0.9300 . ? C65 H65 0.9300 . ? C65 C64 1.39(3) . ? C64 H64 0.9300 . ? C48 H48 0.9300 . ? C48 C47 1.36(4) . ? C67 H67 0.9300 . ? C67 C68 1.41(4) . ? C68 H68 0.9300 . ? C28 H28 0.9300 . ? C28 C27 1.43(3) . ? C4 H4 0.9300 . ? C46 O3 1.42(4) . ? C46 C45 1.36(4) . ? C46 C47 1.35(5) . ? C27 H27 0.9300 . ? C27 C26 1.43(5) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? O3 C49 1.40(5) . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C26 C25 1.37(3) . ? C26 O2 1.34(4) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C11 C10 1.52(3) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C15 C14 1.54(4) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C13 C12 1.49(2) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C25 H25 0.9300 . ? C45 H45 0.9300 . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? O2 C29 1.44(3) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C75 H75A 0.9600 . ? C75 H75B 0.9600 . ? C75 H75C 0.9600 . ? C47 H47 0.9300 . ? C73 H73A 0.9600 . ? C73 H73B 0.9600 . ? C73 H73C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 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 44(2) . . . . ? Au2 P2 C34 C35 61.4(18) . . . . ? Au2 P2 C32 C33 -173(2) . . . . ? Au3 P3 C52 C53 139(3) . . . . ? Au3 P3 C54 C55 170.6(15) . . . . ? Au3 P3 C50 C51 -36(2) . . . . ? Au4 P4 C74 C75 -67(2) . . . . ? Au4 P4 C70 C71 -49.0(17) . . . . ? Au4 P4 C72 C73 168.6(19) . . . . ? Au1 P1 C14 C15 -168.3(16) . . . . ? Au1 P1 C10 C11 38(3) . . . . ? Au1 P1 C12 C13 -52.2(16) . . . . ? C2 C3 C8 C7 -179(2) . . . . ? C2 C3 C4 C5 -179(2) . . . . ? C62 C63 C64 C65 180(2) . . . . ? C62 C63 C68 C67 179.6(18) . . . . ? C61 C62 C63 C64 27(13) . . . . ? C61 C62 C63 C68 -159(11) . . . . ? C74 P4 C70 C71 70.3(17) . . . . ? C74 P4 C72 C73 46(2) . . . . ? C30 P2 C34 C35 -179.1(15) . . . . ? C30 P2 C32 C33 65(3) . . . . ? C34 P2 C30 C31 -76(2) . . . . ? C34 P2 C32 C33 -45(3) . . . . ? C70 P4 C74 C75 172(2) . . . . ? C70 P4 C72 C73 -67(2) . . . . ? C32 P2 C30 C31 171(2) . . . . ? C32 P2 C34 C35 -68.7(18) . . . . ? C52 P3 C54 C55 48(2) . . . . ? C52 P3 C50 C51 81(2) . . . . ? C54 P3 C52 C53 -92(3) . . . . ? C54 P3 C50 C51 -165.1(18) . . . . ? C50 P3 C52 C53 19(4) . . . . ? C50 P3 C54 C55 -65(2) . . . . ? C72 P4 C74 C75 62(2) . . . . ? C72 P4 C70 C71 -178.0(15) . . . . ? O1 C6 C7 C8 -180(2) . . . . ? O1 C6 C5 C4 -177(3) . . . . ? O4 C66 C65 C64 179.6(17) . . . . ? O4 C66 C67 C68 -179(2) . . . . ? C6 C7 C8 C3 -7(4) . . . . ? C6 C5 C4 C3 3(4) . . . . ? C66 C65 C64 C63 -5(3) . . . . ? C66 C67 C68 C63 5(3) . . . . ? C23 C24 C25 C26 3(5) . . . . ? C23 C28 C27 C26 -2(4) . . . . ? C22 C23 C24 C25 177(2) . . . . ? C22 C23 C28 C27 -177(2) . . . . ? C43 C44 C45 C46 0(3) . . . . ? C43 C48 C47 C46 -3(3) . . . . ? C7 C6 C5 C4 -7(5) . . . . ? C5 C6 C7 C8 9(5) . . . . ? C44 C43 C48 C47 4(3) . . . . ? C24 C23 C28 C27 0(4) . . . . ? C8 C3 C4 C5 -1(4) . . . . ? C65 C66 C67 C68 -3(3) . . . . ? C64 C63 C68 C67 -6(3) . . . . ? C42 C43 C44 C45 -178.5(18) . . . . ? C42 C43 C48 C47 180.0(19) . . . . ? C48 C43 C44 C45 -2(4) . . . . ? C67 C66 C65 C64 3(3) . . . . ? C68 C63 C64 C65 6(3) . . . . ? C28 C23 C24 C25 0(4) . . . . ? C28 C27 C26 C25 4(4) . . . . ? C28 C27 C26 O2 177(2) . . . . ? C4 C3 C8 C7 3(5) . . . . ? C27 C26 C25 C24 -4(5) . . . . ? C27 C26 O2 C29 16(4) . . . . ? O3 C46 C45 C44 -179(2) . . . . ? O3 C46 C47 C48 179.9(19) . . . . ? C9 O1 C6 C7 -159(3) . . . . ? C9 O1 C6 C5 11(5) . . . . ? C14 P1 C10 C11 163(2) . . . . ? C14 P1 C12 C13 177.9(14) . . . . ? C10 P1 C14 C15 71(2) . . . . ? C10 P1 C12 C13 68.4(17) . . . . ? C12 P1 C14 C15 -41(2) . . . . ? C12 P1 C10 C11 -84(3) . . . . ? C25 C26 O2 C29 -171(3) . . . . ? C45 C46 O3 C49 -13(4) . . . . ? C45 C46 C47 C48 0(4) . . . . ? C69 O4 C66 C65 172(3) . . . . ? C69 O4 C66 C67 -12(4) . . . . ? O2 C26 C25 C24 -178(3) . . . . ? C47 C46 O3 C49 168(3) . . . . ? C47 C46 C45 C44 1(4) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.94(3) 2 0.06(3)