#------------------------------------------------------------------------------ #$Date: 2025-01-10 01:45:50 +0200 (Fri, 10 Jan 2025) $ #$Revision: 297250 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/36/1573665.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_1573665 _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 17.0308(6) _cell_length_b 9.8580(5) _cell_length_c 16.7203(11) _cell_measurement_reflns_used 5346 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25.1720 _cell_measurement_theta_min 2.1040 _cell_volume 2807.2(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 n-pentane/i-pentane 1:1 mixture' _diffrn_ambient_pressure 1640000 _diffrn_ambient_temperature 293(2) _diffrn_crystal_treatment 'pressurized rapidly in n-pentane/i-pentane 1:1 mixture as a hydrostatic medium' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0128 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.737 _diffrn_measured_fraction_theta_max 0.601 _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 -28.00 3.00 1.00 120.00 -- 22.04 39.00 167.00 31 2 \w -42.00 32.00 1.00 120.00 -- 22.04 26.00 -8.00 74 3 \w 59.00 86.00 1.00 120.00 -- 22.04-160.00 60.00 27 4 \w 20.00 56.00 1.00 120.00 -- 22.04-114.00 45.00 36 5 \w -8.00 36.00 1.00 120.00 -- 22.04 -67.00-157.00 44 6 \w -30.00 12.00 1.00 120.00 -- -22.19 67.00 157.00 42 7 \w -39.00 -14.00 1.00 120.00 -- -22.19 97.00 -35.00 25 8 \w -84.00 -13.00 1.00 120.00 -- -22.19 114.00 135.00 71 9 \w -59.00 11.00 1.00 120.00 -- -22.19 67.00 -23.00 70 10 \w -70.00 -43.00 1.00 120.00 -- -22.19 137.00 114.00 27 11 \w -32.00 20.00 1.00 120.00 -- -22.19 -26.00 8.00 52 12 \w -108.00 -73.00 1.00 120.00 -- -22.19-160.00-120.00 35 13 \w -43.00 -16.00 1.00 120.00 -- -22.19 114.00 -45.00 27 ; _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 38.5 deg.' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0041245080 _diffrn_orient_matrix_UB_12 -0.0342718311 _diffrn_orient_matrix_UB_13 -0.0263640927 _diffrn_orient_matrix_UB_21 -0.0325763002 _diffrn_orient_matrix_UB_22 0.0046877274 _diffrn_orient_matrix_UB_23 0.0031113537 _diffrn_orient_matrix_UB_31 0.0002883705 _diffrn_orient_matrix_UB_32 0.0449727352 _diffrn_orient_matrix_UB_33 -0.0203864709 _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 0.0630 _diffrn_reflns_av_unetI/netI 0.1083 _diffrn_reflns_Laue_measured_fraction_full 0.737 _diffrn_reflns_Laue_measured_fraction_max 0.601 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 17793 _diffrn_reflns_point_group_measured_fraction_full 0.666 _diffrn_reflns_point_group_measured_fraction_max 0.496 _diffrn_reflns_theta_full 19.665 _diffrn_reflns_theta_max 25.654 _diffrn_reflns_theta_min 1.887 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Ag) X-ray Source' _exptl_absorpt_coefficient_mu 5.720 _exptl_absorpt_correction_T_max 0.65934 _exptl_absorpt_correction_T_min 0.65185 _exptl_absorpt_correction_type sphere _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022) 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 2.112 _exptl_crystal_description needle _exptl_crystal_F_000 1712 _exptl_crystal_preparation 'Mounted in a Diamond-Anvil Cell using n-pentane/i-pentane 1:1 mixture as pressure medium.,Luminescent' _exptl_crystal_pressure_history 'Pressurized to 1.64 GPa and left to stabilize over ? hours.' _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: n-pentane/dichloromethane' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_size_rad 0.400 _refine_diff_density_max 1.871 _refine_diff_density_min -2.894 _refine_diff_density_rms 0.255 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.35(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 334 _refine_ls_number_reflns 5367 _refine_ls_number_restraints 151 _refine_ls_restrained_S_all 1.013 _refine_ls_R_factor_all 0.1401 _refine_ls_R_factor_gt 0.0536 _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^)+(0.0498P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0988 _refine_ls_wR_factor_ref 0.1343 _reflns_Friedel_coverage 0.572 _reflns_Friedel_fraction_full 0.584 _reflns_Friedel_fraction_max 0.380 _reflns_number_gt 2725 _reflns_number_total 5367 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4dt03036b2.cif _cod_data_source_block appr6_1p64GPa _cod_database_code 1573665 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula C15H22OPAu _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: 0.65(5) 0.35(5) 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 C29 \\sim O2 \\sim C26 \\sim C27 \\sim C25 \\sim C28 \\sim C24 \\sim C23 \\sim C22: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A C1 \\sim C2 \\sim C3 \\sim C8 \\sim C7 \\sim C6 \\sim C5 \\sim C4 \\sim O1 \\sim C9: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.7A C35 \\sim C34 \\sim P2 \\sim C32 \\sim C33 \\sim C30 \\sim C31: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A 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 appr6_1p64GPa in Pb21a #29 appr6_1p64GPa.res created by SHELXL-2018/3 at 15:53:16 on 06-May-2024 REM reset to Pb21a #29 CELL 0.56087 17.030848 9.858014 16.720315 90 90 90 ZERR 8 0.000608 0.000491 0.001099 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 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 0.04 0.08 1.7 C29 O2 C26 C27 C25 C28 C24 C23 C22 SIMU 0.02 0.04 1.7 C1 C2 C3 C8 C7 C6 C5 C4 O1 C9 SIMU C35 C34 P2 C32 C33 C30 C31 L.S. 20 PLAN 6 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 0.049800 BASF 0.34740 FVAR 0.57794 AU2 3 0.633523 -0.007560 0.420652 11.00000 0.04533 0.02950 = 0.03826 0.00405 -0.00174 -0.00118 AU1 3 0.377374 0.708370 0.077749 11.00000 0.04341 0.03114 = 0.03660 0.00463 0.00155 -0.00035 P1 5 0.377437 0.902986 0.004413 11.00000 0.03080 0.02644 = 0.04113 0.00353 0.00291 -0.00096 P2 5 0.628451 -0.198458 0.497001 11.00000 0.04549 0.02591 = 0.02371 -0.00181 0.00014 -0.00165 C23 1 0.634944 0.415482 0.304128 11.00000 0.04049 0.04046 = 0.03089 -0.01180 0.01266 0.00161 C21 1 0.634407 0.174137 0.362374 11.00000 0.03409 0.03107 = 0.05761 0.00646 0.00477 -0.00028 C26 1 0.636402 0.674579 0.236679 11.00000 0.06070 0.01531 = 0.03541 -0.00216 -0.00699 -0.00927 C22 1 0.634431 0.285495 0.341440 11.00000 0.05821 0.03044 = 0.01801 0.01012 -0.00004 0.00496 O2 4 0.642142 0.794682 0.194388 11.00000 0.07311 0.02732 = 0.06613 0.01827 0.00645 -0.00065 C1 1 0.378718 0.525732 0.132500 11.00000 0.06000 0.02818 = 0.04614 -0.00512 0.00286 0.00189 C2 1 0.378410 0.413599 0.160103 11.00000 0.05413 0.02799 = 0.05237 -0.00451 -0.00302 0.00164 C27 1 0.567717 0.620644 0.261344 11.00000 0.05149 0.03295 = 0.04438 0.00792 -0.01111 -0.00344 AFIX 43 H27 2 0.520798 0.666997 0.253418 11.00000 -1.20000 AFIX 0 C24 1 0.704650 0.471029 0.275145 11.00000 0.04005 0.04295 = 0.03485 0.00426 -0.01871 0.00244 AFIX 43 H24 2 0.751349 0.422562 0.278965 11.00000 -1.20000 AFIX 0 C28 1 0.568177 0.493226 0.299230 11.00000 0.04200 0.03407 = 0.05276 0.00056 0.00280 -0.00992 AFIX 43 H28 2 0.521889 0.460647 0.321632 11.00000 -1.20000 AFIX 0 C25 1 0.703991 0.600000 0.240300 11.00000 0.03586 0.03514 = 0.04552 -0.01071 0.00167 -0.00054 AFIX 43 H25 2 0.750182 0.635533 0.219295 11.00000 -1.20000 AFIX 0 C7 1 0.449350 0.111751 0.270104 11.00000 0.03072 0.03417 = 0.06168 0.00613 -0.02266 0.00483 AFIX 43 H7 2 0.494362 0.085894 0.297656 11.00000 -1.20000 AFIX 0 C8 1 0.445837 0.234344 0.237332 11.00000 0.03637 0.03056 = 0.05791 0.00292 -0.01231 0.00500 AFIX 43 H8 2 0.487235 0.294369 0.245283 11.00000 -1.20000 AFIX 0 C3 1 0.380875 0.276224 0.190648 11.00000 0.05191 0.01697 = 0.04438 0.00799 0.00596 0.01559 C10 1 0.404163 0.869700 -0.096799 11.00000 0.05358 0.01518 = 0.04564 -0.00343 0.00310 0.00320 AFIX 23 H10A 2 0.379590 0.936453 -0.131297 11.00000 -1.20000 H10B 2 0.460608 0.878631 -0.102491 11.00000 -1.20000 AFIX 0 C11 1 0.379890 0.731132 -0.122654 11.00000 0.05177 0.04790 = 0.04448 -0.01147 0.01240 -0.00511 AFIX 137 H11A 2 0.389476 0.720880 -0.178909 11.00000 -1.50000 H11B 2 0.324959 0.718721 -0.112047 11.00000 -1.50000 H11C 2 0.409607 0.664590 -0.093652 11.00000 -1.50000 AFIX 0 C31 1 0.662267 -0.035431 0.632027 11.00000 0.05594 0.02333 = 0.06093 -0.00911 -0.01126 0.00349 AFIX 137 H31A 2 0.676819 0.036260 0.596107 11.00000 -1.50000 H31B 2 0.692062 -0.027634 0.680549 11.00000 -1.50000 H31C 2 0.607278 -0.028887 0.644047 11.00000 -1.50000 AFIX 0 C30 1 0.679496 -0.174695 0.592171 11.00000 0.04935 0.02933 = 0.05233 -0.00007 -0.02617 -0.00029 AFIX 23 H30A 2 0.664031 -0.246469 0.628596 11.00000 -1.20000 H30B 2 0.735582 -0.182714 0.583247 11.00000 -1.20000 AFIX 0 O1 4 0.398654 -0.103344 0.297407 11.00000 0.07047 0.05478 = 0.04799 0.02287 -0.02496 -0.01084 C4 1 0.319238 0.182979 0.183319 11.00000 0.03061 0.04524 = 0.04332 -0.00101 -0.00924 -0.00589 AFIX 43 H4 2 0.275506 0.206665 0.153077 11.00000 -1.20000 AFIX 0 C32 1 0.669191 -0.347535 0.456772 11.00000 0.05509 0.01936 = 0.05315 -0.00452 -0.00024 0.00348 AFIX 23 H32A 2 0.648855 -0.359309 0.403029 11.00000 -1.20000 H32B 2 0.725529 -0.335113 0.452420 11.00000 -1.20000 AFIX 0 C12 1 0.283662 0.985300 -0.000500 11.00000 0.04146 0.07211 = 0.03573 -0.01029 0.01021 -0.00890 AFIX 23 H12A 2 0.267866 1.010037 0.053296 11.00000 -1.20000 H12B 2 0.289314 1.068499 -0.030934 11.00000 -1.20000 AFIX 0 C14 1 0.447366 1.033937 0.035804 11.00000 0.03981 0.03977 = 0.04172 0.00228 0.00284 0.00503 AFIX 23 H14A 2 0.440912 1.049998 0.092660 11.00000 -1.20000 H14B 2 0.500270 1.000421 0.027363 11.00000 -1.20000 AFIX 0 C9 1 0.346522 -0.202505 0.282186 11.00000 0.06152 0.03991 = 0.05689 0.00795 0.01211 -0.00432 AFIX 137 H9A 2 0.343214 -0.216943 0.225505 11.00000 -1.50000 H9B 2 0.295910 -0.176650 0.302348 11.00000 -1.50000 H9C 2 0.363229 -0.284707 0.307839 11.00000 -1.50000 AFIX 0 C35 1 0.475963 -0.267078 0.453698 11.00000 0.05305 0.04105 = 0.08393 0.00057 -0.00314 -0.00762 AFIX 137 H35A 2 0.479591 -0.193228 0.416454 11.00000 -1.50000 H35B 2 0.422428 -0.277538 0.470581 11.00000 -1.50000 H35C 2 0.493431 -0.349132 0.428410 11.00000 -1.50000 AFIX 0 C34 1 0.527769 -0.237269 0.526601 11.00000 0.04435 0.06168 = 0.01037 0.00826 -0.00319 0.00337 AFIX 23 H34A 2 0.527772 -0.315392 0.561871 11.00000 -1.20000 H34B 2 0.506132 -0.160988 0.555879 11.00000 -1.20000 AFIX 0 C6 1 0.387574 0.022266 0.264029 11.00000 0.04695 0.04138 = 0.05143 0.00929 -0.01600 -0.00385 C5 1 0.321159 0.059450 0.218788 11.00000 0.04427 0.04365 = 0.04755 0.00652 0.00690 -0.00811 AFIX 43 H5 2 0.279144 -0.000099 0.213342 11.00000 -1.20000 AFIX 0 C33 1 0.653805 -0.478654 0.503881 11.00000 0.09265 0.03047 = 0.04041 -0.00515 -0.00321 0.01575 AFIX 137 H33A 2 0.672565 -0.554948 0.473747 11.00000 -1.50000 H33B 2 0.598450 -0.488319 0.513099 11.00000 -1.50000 H33C 2 0.680786 -0.474636 0.554236 11.00000 -1.50000 AFIX 0 C15 1 0.438024 1.168359 -0.008483 11.00000 0.05263 0.03986 = 0.08144 -0.00560 0.00439 -0.00822 AFIX 137 H15A 2 0.430874 1.151150 -0.064524 11.00000 -1.50000 H15B 2 0.484214 1.222627 -0.000783 11.00000 -1.50000 H15C 2 0.393109 1.215847 0.012001 11.00000 -1.50000 AFIX 0 C13 1 0.221266 0.904339 -0.036516 11.00000 0.03798 0.04156 = 0.06125 -0.00689 -0.00502 -0.00734 AFIX 137 H13A 2 0.230157 0.896886 -0.093042 11.00000 -1.50000 H13B 2 0.171547 0.947394 -0.027164 11.00000 -1.50000 H13C 2 0.221041 0.815470 -0.013041 11.00000 -1.50000 AFIX 0 C29 1 0.573641 0.884847 0.199402 11.00000 0.08856 0.06659 = 0.07222 0.03695 -0.00498 0.01792 AFIX 137 H29A 2 0.529017 0.841118 0.175614 11.00000 -1.50000 H29B 2 0.584557 0.967732 0.171387 11.00000 -1.50000 H29C 2 0.562583 0.904612 0.254483 11.00000 -1.50000 AFIX 0 HKLF 4 REM appr6_1p64GPa in Pb21a #29 REM wR2 = 0.1343, GooF = S = 1.025, Restrained GooF = 1.013 for all data REM R1 = 0.0536 for 2725 Fo > 4sig(Fo) and 0.1401 for all 5367 data REM 334 parameters refined using 151 restraints END WGHT 0.0497 0.0000 REM Highest difference peak 1.871, deepest hole -2.894, 1-sigma level 0.255 Q1 1 0.6008 -0.0050 0.4203 11.00000 0.05 1.87 Q2 1 0.6619 -0.0076 0.4199 11.00000 0.05 1.82 Q3 1 0.3477 0.7112 0.0801 11.00000 0.05 1.58 Q4 1 0.7048 0.0624 0.4172 11.00000 0.05 1.58 Q5 1 0.3153 0.6126 0.0783 11.00000 0.05 1.53 Q6 1 0.5602 -0.0734 0.4198 11.00000 0.05 1.51 ; _shelx_res_checksum 47490 _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 1.362 _oxdiff_exptl_absorpt_empirical_full_min 0.822 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 0.63352(4) -0.00756(7) 0.42065(7) 0.0377(3) Uani 1 1 d . . . . . Au1 Au 0.37737(4) 0.70837(8) 0.07775(8) 0.0371(3) Uani 1 1 d . . . . . P1 P 0.3774(3) 0.9030(12) 0.0044(5) 0.033(3) Uani 1 1 d . . . . . P2 P 0.6285(3) -0.1985(12) 0.4970(5) 0.032(3) Uani 1 1 d . U . . . C23 C 0.6349(11) 0.415(3) 0.304(2) 0.037(7) Uani 1 1 d . U . . . C21 C 0.6344(11) 0.174(4) 0.362(3) 0.041(9) Uani 1 1 d . . . . . C26 C 0.6364(12) 0.675(3) 0.237(2) 0.037(6) Uani 1 1 d . U . . . C22 C 0.6344(12) 0.285(4) 0.341(2) 0.036(7) Uani 1 1 d . U . . . O2 O 0.6421(9) 0.795(2) 0.1944(15) 0.056(6) Uani 1 1 d . U . . . C1 C 0.3787(12) 0.526(4) 0.132(3) 0.045(9) Uani 1 1 d . U . . . C2 C 0.3784(12) 0.414(4) 0.160(3) 0.045(7) Uani 1 1 d . U . . . C27 C 0.5677(13) 0.621(3) 0.2613(18) 0.043(7) Uani 1 1 d . U . . . H27 H 0.520798 0.666997 0.253418 0.052 Uiso 1 1 calc R U . . . C24 C 0.7046(10) 0.471(2) 0.2751(15) 0.039(6) Uani 1 1 d . U . . . H24 H 0.751349 0.422562 0.278965 0.047 Uiso 1 1 calc R U . . . C28 C 0.5682(10) 0.493(3) 0.2992(16) 0.043(6) Uani 1 1 d . U . . . H28 H 0.521889 0.460647 0.321632 0.052 Uiso 1 1 calc R U . . . C25 C 0.7040(11) 0.600(2) 0.2403(17) 0.039(6) Uani 1 1 d . U . . . H25 H 0.750182 0.635533 0.219295 0.047 Uiso 1 1 calc R U . . . C7 C 0.4493(11) 0.112(2) 0.2701(19) 0.042(6) Uani 1 1 d . U . . . H7 H 0.494362 0.085894 0.297656 0.051 Uiso 1 1 calc R U . . . C8 C 0.4458(10) 0.234(2) 0.2373(17) 0.042(6) Uani 1 1 d . U . . . H8 H 0.487235 0.294369 0.245283 0.050 Uiso 1 1 calc R U . . . C3 C 0.3809(11) 0.276(3) 0.191(2) 0.038(6) Uani 1 1 d . U . . . C10 C 0.4042(12) 0.870(2) -0.0968(15) 0.038(6) Uani 1 1 d . . . . . H10A H 0.379590 0.936453 -0.131297 0.046 Uiso 1 1 calc R U . . . H10B H 0.460608 0.878631 -0.102491 0.046 Uiso 1 1 calc R U . . . C11 C 0.3799(11) 0.731(3) -0.123(2) 0.048(8) Uani 1 1 d . . . . . H11A H 0.389476 0.720880 -0.178909 0.072 Uiso 1 1 calc R U . . . H11B H 0.324959 0.718721 -0.112047 0.072 Uiso 1 1 calc R U . . . H11C H 0.409607 0.664590 -0.093652 0.072 Uiso 1 1 calc R U . . . C31 C 0.6623(11) -0.035(2) 0.6320(19) 0.047(7) Uani 1 1 d . U . . . H31A H 0.676819 0.036260 0.596107 0.070 Uiso 1 1 calc R U . . . H31B H 0.692062 -0.027634 0.680549 0.070 Uiso 1 1 calc R U . . . H31C H 0.607278 -0.028887 0.644047 0.070 Uiso 1 1 calc R U . . . C30 C 0.6795(11) -0.175(2) 0.5922(15) 0.044(6) Uani 1 1 d . U . . . H30A H 0.664031 -0.246469 0.628596 0.052 Uiso 1 1 calc R U . . . H30B H 0.735582 -0.182714 0.583247 0.052 Uiso 1 1 calc R U . . . O1 O 0.3987(10) -0.103(2) 0.2974(15) 0.058(6) Uani 1 1 d . U . . . C4 C 0.3192(10) 0.183(2) 0.1833(16) 0.040(6) Uani 1 1 d . U . . . H4 H 0.275506 0.206665 0.153077 0.048 Uiso 1 1 calc R U . . . C32 C 0.6692(12) -0.348(2) 0.4568(16) 0.043(6) Uani 1 1 d . U . . . H32A H 0.648855 -0.359309 0.403029 0.051 Uiso 1 1 calc R U . . . H32B H 0.725529 -0.335113 0.452420 0.051 Uiso 1 1 calc R U . . . C12 C 0.2837(9) 0.985(3) -0.0005(16) 0.050(7) Uani 1 1 d . . . . . H12A H 0.267866 1.010037 0.053296 0.060 Uiso 1 1 calc R U . . . H12B H 0.289314 1.068499 -0.030934 0.060 Uiso 1 1 calc R U . . . C14 C 0.4474(10) 1.034(2) 0.0358(17) 0.040(7) Uani 1 1 d . . . . . H14A H 0.440912 1.049998 0.092660 0.049 Uiso 1 1 calc R U . . . H14B H 0.500270 1.000421 0.027363 0.049 Uiso 1 1 calc R U . . . C9 C 0.3465(11) -0.203(3) 0.2822(18) 0.053(7) Uani 1 1 d . U . . . H9A H 0.343214 -0.216943 0.225505 0.079 Uiso 1 1 calc R U . . . H9B H 0.295910 -0.176650 0.302348 0.079 Uiso 1 1 calc R U . . . H9C H 0.363229 -0.284707 0.307839 0.079 Uiso 1 1 calc R U . . . C35 C 0.4760(11) -0.267(3) 0.4537(18) 0.059(8) Uani 1 1 d . U . . . H35A H 0.479591 -0.193228 0.416454 0.089 Uiso 1 1 calc R U . . . H35B H 0.422428 -0.277538 0.470581 0.089 Uiso 1 1 calc R U . . . H35C H 0.493431 -0.349132 0.428410 0.089 Uiso 1 1 calc R U . . . C34 C 0.5278(10) -0.237(2) 0.5266(17) 0.039(6) Uani 1 1 d . U . . . H34A H 0.527772 -0.315392 0.561871 0.047 Uiso 1 1 calc R U . . . H34B H 0.506132 -0.160988 0.555879 0.047 Uiso 1 1 calc R U . . . C6 C 0.3876(12) 0.022(3) 0.264(2) 0.047(6) Uani 1 1 d . U . . . C5 C 0.3212(12) 0.059(2) 0.2188(19) 0.045(6) Uani 1 1 d . U . . . H5 H 0.279144 -0.000099 0.213342 0.054 Uiso 1 1 calc R U . . . C33 C 0.6538(13) -0.479(3) 0.5039(17) 0.055(8) Uani 1 1 d . U . . . H33A H 0.672565 -0.554948 0.473747 0.082 Uiso 1 1 calc R U . . . H33B H 0.598450 -0.488319 0.513099 0.082 Uiso 1 1 calc R U . . . H33C H 0.680786 -0.474636 0.554236 0.082 Uiso 1 1 calc R U . . . C15 C 0.4380(12) 1.168(3) -0.0085(19) 0.058(9) Uani 1 1 d . . . . . H15A H 0.430874 1.151150 -0.064524 0.087 Uiso 1 1 calc R U . . . H15B H 0.484214 1.222627 -0.000783 0.087 Uiso 1 1 calc R U . . . H15C H 0.393109 1.215847 0.012001 0.087 Uiso 1 1 calc R U . . . C13 C 0.2213(10) 0.904(2) -0.0365(16) 0.047(7) Uani 1 1 d . . . . . H13A H 0.230157 0.896886 -0.093042 0.070 Uiso 1 1 calc R U . . . H13B H 0.171547 0.947394 -0.027164 0.070 Uiso 1 1 calc R U . . . H13C H 0.221041 0.815470 -0.013041 0.070 Uiso 1 1 calc R U . . . C29 C 0.5736(13) 0.885(3) 0.1994(19) 0.076(10) Uani 1 1 d . U . . . H29A H 0.529017 0.841118 0.175614 0.114 Uiso 1 1 calc R U . . . H29B H 0.584557 0.967732 0.171387 0.114 Uiso 1 1 calc R U . . . H29C H 0.562583 0.904612 0.254483 0.114 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 0.0453(4) 0.0295(7) 0.0383(10) 0.0041(9) -0.0017(4) -0.0012(4) Au1 0.0434(4) 0.0311(7) 0.0366(10) 0.0046(9) 0.0016(4) -0.0004(3) P1 0.031(3) 0.026(8) 0.041(10) 0.004(3) 0.003(3) -0.001(2) P2 0.045(4) 0.026(8) 0.024(10) -0.002(3) 0.000(3) -0.002(2) C23 0.040(10) 0.040(16) 0.031(19) -0.012(12) 0.013(11) 0.002(10) C21 0.034(11) 0.03(2) 0.06(3) 0.006(15) 0.005(11) 0.000(9) C26 0.061(12) 0.015(13) 0.035(19) -0.002(10) -0.007(11) -0.009(9) C22 0.058(12) 0.030(17) 0.02(2) 0.010(12) 0.000(11) 0.005(12) O2 0.073(10) 0.027(13) 0.066(19) 0.018(9) 0.006(11) -0.001(9) C1 0.060(12) 0.028(19) 0.05(2) -0.005(14) 0.003(11) 0.002(10) C2 0.054(11) 0.028(16) 0.05(2) -0.005(13) -0.003(11) 0.002(10) C27 0.051(12) 0.033(15) 0.04(2) 0.008(11) -0.011(12) -0.003(10) C24 0.040(9) 0.043(16) 0.035(18) 0.004(10) -0.019(10) 0.002(10) C28 0.042(9) 0.034(14) 0.053(19) 0.001(13) 0.003(10) -0.010(12) C25 0.036(10) 0.035(16) 0.05(2) -0.011(11) 0.002(10) -0.001(9) C7 0.031(8) 0.034(13) 0.062(16) 0.006(10) -0.023(10) 0.005(9) C8 0.036(8) 0.031(13) 0.058(16) 0.003(10) -0.012(9) 0.005(9) C3 0.052(10) 0.017(11) 0.044(16) 0.008(10) 0.006(10) 0.016(9) C10 0.054(12) 0.015(14) 0.05(2) -0.003(9) 0.003(12) 0.003(9) C11 0.052(11) 0.05(2) 0.04(3) -0.011(13) 0.012(12) -0.005(11) C31 0.056(12) 0.023(17) 0.06(3) -0.009(11) -0.011(13) 0.003(11) C30 0.049(11) 0.029(15) 0.05(2) 0.000(10) -0.026(11) 0.000(10) O1 0.070(9) 0.055(14) 0.048(16) 0.023(10) -0.025(11) -0.011(10) C4 0.031(8) 0.045(13) 0.043(16) -0.001(10) -0.009(9) -0.006(9) C32 0.055(12) 0.019(13) 0.05(2) -0.005(10) 0.000(12) 0.003(9) C12 0.041(10) 0.072(18) 0.04(2) -0.010(12) 0.010(10) -0.009(15) C14 0.040(10) 0.040(17) 0.04(3) 0.002(10) 0.003(11) 0.005(9) C9 0.062(13) 0.040(17) 0.06(2) 0.008(12) 0.012(14) -0.004(12) C35 0.053(13) 0.041(18) 0.08(3) 0.001(13) -0.003(14) -0.008(12) C34 0.044(11) 0.062(17) 0.010(19) 0.008(11) -0.003(11) 0.003(10) C6 0.047(9) 0.041(14) 0.051(15) 0.009(11) -0.016(10) -0.004(10) C5 0.044(10) 0.044(14) 0.048(16) 0.007(10) 0.007(11) -0.008(10) C33 0.093(14) 0.030(19) 0.04(3) -0.005(10) -0.003(14) 0.016(13) C15 0.053(12) 0.040(19) 0.08(3) -0.006(13) 0.004(13) -0.008(11) C13 0.038(11) 0.042(16) 0.06(2) -0.007(12) -0.005(11) -0.007(10) C29 0.089(17) 0.07(2) 0.07(3) 0.037(17) -0.005(17) 0.018(16) 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_ _axis.id _axis.type _axis.equipment _axis.parity _axis.depends_on _axis.zero _axis.vector[1] _axis.vector[2] _axis.vector[3] source . source . . . 0.99999995 0.00000000 0.00030037 omega rotation goniometer -1 . 0.33691000 0.00000000 0.00000000 1.00000000 kappa rotation goniometer -1 omega 0.00043000 -0.76615415 0.00000000 0.64265684 phi rotation goniometer -1 kappa . 0.00004800 0.00000000 1.00000000 theta rotation goniometer -1 . 0.40100000 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 174.1(11) . . ? C1 Au1 P1 174.3(12) . . ? C10 P1 Au1 110.9(9) . . ? C10 P1 C12 105.5(12) . . ? C10 P1 C14 103.6(11) . . ? C12 P1 Au1 113.9(10) . . ? C12 P1 C14 105.8(13) . . ? C14 P1 Au1 116.1(9) . . ? C30 P2 Au2 111.4(9) . . ? C32 P2 Au2 117.5(9) . . ? C32 P2 C30 104.6(11) . . ? C32 P2 C34 107.4(11) . . ? C34 P2 Au2 111.2(8) . . ? C34 P2 C30 103.7(12) . . ? C24 C23 C22 121(2) . . ? C28 C23 C22 122(2) . . ? C28 C23 C24 118(3) . . ? C22 C21 Au2 169(4) . . ? C27 C26 O2 124(2) . . ? C27 C26 C25 120(3) . . ? C25 C26 O2 115(2) . . ? C21 C22 C23 172(5) . . ? C26 O2 C29 116(2) . . ? C2 C1 Au1 176(4) . . ? C1 C2 C3 177(4) . . ? C26 C27 H27 120.5 . . ? C26 C27 C28 119(2) . . ? C28 C27 H27 120.5 . . ? C23 C24 H24 120.2 . . ? C23 C24 C25 120(2) . . ? C25 C24 H24 120.2 . . ? C23 C28 C27 122(2) . . ? C23 C28 H28 119.0 . . ? C27 C28 H28 119.0 . . ? C26 C25 C24 121(2) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C8 C7 H7 119.4 . . ? C8 C7 C6 121(2) . . ? C6 C7 H7 119.4 . . ? C7 C8 H8 119.1 . . ? C7 C8 C3 122(2) . . ? C3 C8 H8 119.1 . . ? C8 C3 C2 119(2) . . ? C4 C3 C2 124(2) . . ? C4 C3 C8 116(3) . . ? P1 C10 H10A 109.2 . . ? P1 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? C11 C10 P1 111.9(19) . . ? C11 C10 H10A 109.2 . . ? C11 C10 H10B 109.2 . . ? 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 113.4(16) . . ? C31 C30 H30A 108.9 . . ? C31 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? C9 O1 C6 119(2) . . ? C3 C4 H4 118.9 . . ? C5 C4 C3 122(2) . . ? C5 C4 H4 118.9 . . ? P2 C32 H32A 108.3 . . ? P2 C32 H32B 108.3 . . ? H32A C32 H32B 107.4 . . ? C33 C32 P2 116.1(18) . . ? C33 C32 H32A 108.3 . . ? C33 C32 H32B 108.3 . . ? P1 C12 H12A 108.6 . . ? P1 C12 H12B 108.6 . . ? H12A C12 H12B 107.5 . . ? C13 C12 P1 115(2) . . ? C13 C12 H12A 108.6 . . ? C13 C12 H12B 108.6 . . ? P1 C14 H14A 108.8 . . ? P1 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? C15 C14 P1 113.9(18) . . ? C15 C14 H14A 108.8 . . ? C15 C14 H14B 108.8 . . ? 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 109.3 . . ? P2 C34 H34B 109.3 . . ? C35 C34 P2 111.4(16) . . ? C35 C34 H34A 109.3 . . ? C35 C34 H34B 109.3 . . ? H34A C34 H34B 108.0 . . ? C7 C6 C5 119(3) . . ? O1 C6 C7 116(2) . . ? O1 C6 C5 124(2) . . ? C4 C5 C6 119(2) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? 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 2.276(11) . ? Au2 C21 2.04(4) . ? Au1 P1 2.277(11) . ? Au1 C1 2.02(4) . ? P1 C10 1.78(2) . ? P1 C12 1.79(2) . ? P1 C14 1.83(2) . ? P2 C30 1.83(2) . ? P2 C32 1.76(2) . ? P2 C34 1.825(19) . ? C23 C22 1.43(5) . ? C23 C24 1.39(3) . ? C23 C28 1.37(3) . ? C21 C22 1.15(5) . ? C26 O2 1.38(4) . ? C26 C27 1.35(3) . ? C26 C25 1.37(3) . ? O2 C29 1.47(3) . ? C1 C2 1.20(5) . ? C2 C3 1.45(5) . ? C27 H27 0.9300 . ? C27 C28 1.41(4) . ? C24 H24 0.9300 . ? C24 C25 1.40(3) . ? C28 H28 0.9300 . ? C25 H25 0.9300 . ? C7 H7 0.9300 . ? C7 C8 1.33(3) . ? C7 C6 1.38(3) . ? C8 H8 0.9300 . ? C8 C3 1.42(3) . ? C3 C4 1.40(3) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 C11 1.49(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 1.55(3) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? O1 C9 1.34(3) . ? O1 C6 1.37(4) . ? C4 H4 0.9300 . ? C4 C5 1.35(4) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 C33 1.54(3) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 C13 1.46(3) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 C15 1.53(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 1.53(3) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C6 C5 1.41(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 42.8(19) . . . . ? Au2 P2 C32 C33 -171.0(15) . . . . ? Au2 P2 C34 C35 62.7(16) . . . . ? Au1 P1 C10 C11 30.3(19) . . . . ? Au1 P1 C12 C13 -60(2) . . . . ? Au1 P1 C14 C15 -172.8(16) . . . . ? C23 C24 C25 C26 2(4) . . . . ? C26 C27 C28 C23 -7(4) . . . . ? C22 C23 C24 C25 -179(3) . . . . ? C22 C23 C28 C27 -179(3) . . . . ? O2 C26 C27 C28 176(3) . . . . ? O2 C26 C25 C24 -174(3) . . . . ? C2 C3 C4 C5 -174(3) . . . . ? C27 C26 O2 C29 19(4) . . . . ? C27 C26 C25 C24 -5(5) . . . . ? C24 C23 C28 C27 5(5) . . . . ? C28 C23 C24 C25 -2(4) . . . . ? C25 C26 O2 C29 -172(2) . . . . ? C25 C26 C27 C28 7(5) . . . . ? C7 C8 C3 C2 177(3) . . . . ? C7 C8 C3 C4 2(4) . . . . ? C7 C6 C5 C4 -1(5) . . . . ? C8 C7 C6 O1 178(3) . . . . ? C8 C7 C6 C5 3(5) . . . . ? C8 C3 C4 C5 0(4) . . . . ? C3 C4 C5 C6 -1(4) . . . . ? C10 P1 C12 C13 61(2) . . . . ? C10 P1 C14 C15 65(2) . . . . ? C30 P2 C32 C33 65(2) . . . . ? C30 P2 C34 C35 -177.5(15) . . . . ? O1 C6 C5 C4 -175(3) . . . . ? C32 P2 C30 C31 170.7(17) . . . . ? C32 P2 C34 C35 -67.0(18) . . . . ? C12 P1 C10 C11 -94(2) . . . . ? C12 P1 C14 C15 -45(2) . . . . ? C14 P1 C10 C11 155.5(17) . . . . ? C14 P1 C12 C13 171(2) . . . . ? C9 O1 C6 C7 -169(3) . . . . ? C9 O1 C6 C5 5(5) . . . . ? C34 P2 C30 C31 -77(2) . . . . ? C34 P2 C32 C33 -45(2) . . . . ? C6 C7 C8 C3 -4(5) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.65(5) 2 0.35(5)