# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Nocera, D.' 'Teets, Thomas' 'Neumann, Markus' _publ_contact_author_name 'Nocera, D.' _publ_contact_author_email NOCERA@MIT.EDU _publ_section_title ; Heterobimetallic Rhodium-Gold Halide and Hydride Complexes ; # Attachment '- CIF final.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 789594' #TrackingRef '- CIF final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H94 Au Cl3 F6 O P5 Rh' _chemical_formula_weight 1410.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.031(2) _cell_length_b 21.469(3) _cell_length_c 20.325(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.251(2) _cell_angle_gamma 90.00 _cell_volume 6409.6(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9254 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 30.58 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2872 _exptl_absorpt_coefficient_mu 2.844 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3958 _exptl_absorpt_correction_T_max 0.4825 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 145895 _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 30.03 _reflns_number_total 18727 _reflns_number_gt 16517 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+22.1558P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18727 _refine_ls_number_parameters 687 _refine_ls_number_restraints 253 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0978 _refine_ls_wR_factor_gt 0.0930 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.061318(8) 0.171831(6) 0.688708(6) 0.01406(4) Uani 1 1 d . . . Rh1 Rh 0.203153(16) 0.090214(11) 0.763609(11) 0.01256(5) Uani 1 1 d U . . P1 P 0.10457(5) 0.05855(4) 0.83218(4) 0.01263(14) Uani 1 1 d . . . P2 P -0.04288(5) 0.14962(4) 0.75383(4) 0.01449(14) Uani 1 1 d . . . P3 P 0.31041(5) 0.12285(4) 0.70309(4) 0.01415(14) Uani 1 1 d . A . P4 P 0.15644(5) 0.20554(4) 0.62050(4) 0.01407(14) Uani 1 1 d . . . Cl1 Cl 0.23427(6) 0.18169(4) 0.83023(4) 0.02313(16) Uani 1 1 d U . . C1 C 0.0144(2) 0.11628(15) 0.83471(15) 0.0153(6) Uani 1 1 d . . . H1A H -0.0322 0.0963 0.8555 0.018 Uiso 1 1 calc R . . H1B H 0.0415 0.1508 0.8646 0.018 Uiso 1 1 calc R . . C2 C 0.2771(2) 0.19872(15) 0.66232(15) 0.0160(6) Uani 1 1 d . . . H2A H 0.2916 0.2318 0.6968 0.019 Uiso 1 1 calc R . . H2B H 0.3146 0.2064 0.6285 0.019 Uiso 1 1 calc R . . C3 C 0.1670(3) 0.02668(17) 0.70410(19) 0.0236(7) Uani 1 1 d . . . O1 O 0.1414(2) -0.01026(16) 0.66512(15) 0.0355(7) Uani 1 1 d . . . C11 C 0.1594(2) 0.04564(16) 0.92263(15) 0.0179(6) Uani 1 1 d . . . H11 H 0.1344 0.0056 0.9363 0.021 Uiso 1 1 calc R . . C12 C 0.1390(3) 0.0959(2) 0.97110(18) 0.0284(8) Uani 1 1 d . . . H12A H 0.0724 0.1001 0.9662 0.034 Uiso 1 1 calc R . . H12B H 0.1634 0.1364 0.9599 0.034 Uiso 1 1 calc R . . C13 C 0.1828(3) 0.0782(3) 1.04411(19) 0.0389(11) Uani 1 1 d . . . H13A H 0.1544 0.0395 1.0563 0.047 Uiso 1 1 calc R . . H13B H 0.1710 0.1117 1.0747 0.047 Uiso 1 1 calc R . . C14 C 0.2862(3) 0.0683(2) 1.05395(19) 0.0313(8) Uani 1 1 d . . . H14A H 0.3159 0.1082 1.0469 0.038 Uiso 1 1 calc R . . H14B H 0.3113 0.0542 1.1006 0.038 Uiso 1 1 calc R . . C15 C 0.3067(3) 0.01977(18) 1.00438(18) 0.0266(7) Uani 1 1 d . . . H15A H 0.2838 -0.0213 1.0154 0.032 Uiso 1 1 calc R . . H15B H 0.3734 0.0164 1.0089 0.032 Uiso 1 1 calc R . . C16 C 0.2626(2) 0.03663(17) 0.93170(17) 0.0207(6) Uani 1 1 d . . . H16A H 0.2746 0.0031 0.9013 0.025 Uiso 1 1 calc R . . H16B H 0.2902 0.0755 0.9190 0.025 Uiso 1 1 calc R . . C21 C 0.0458(2) -0.01547(15) 0.80487(15) 0.0144(5) Uani 1 1 d . . . H21 H 0.0221 -0.0116 0.7552 0.017 Uiso 1 1 calc R . . C22 C -0.0364(2) -0.03202(16) 0.83498(16) 0.0175(6) Uani 1 1 d . . . H22A H -0.0795 0.0034 0.8293 0.021 Uiso 1 1 calc R . . H22B H -0.0161 -0.0405 0.8837 0.021 Uiso 1 1 calc R . . C23 C -0.0839(2) -0.08990(17) 0.79915(17) 0.0215(6) Uani 1 1 d . . . H23A H -0.1361 -0.1012 0.8194 0.026 Uiso 1 1 calc R . . H23B H -0.1078 -0.0801 0.7511 0.026 Uiso 1 1 calc R . . C24 C -0.0187(3) -0.14536(17) 0.8046(2) 0.0269(7) Uani 1 1 d . . . H24A H -0.0019 -0.1591 0.8521 0.032 Uiso 1 1 calc R . . H24B H -0.0499 -0.1804 0.7776 0.032 Uiso 1 1 calc R . . C25 C 0.0677(2) -0.12893(17) 0.78003(19) 0.0246(7) Uani 1 1 d . . . H25A H 0.0522 -0.1221 0.7307 0.030 Uiso 1 1 calc R . . H25B H 0.1109 -0.1643 0.7892 0.030 Uiso 1 1 calc R . . C26 C 0.1136(2) -0.07033(15) 0.81463(17) 0.0182(6) Uani 1 1 d . . . H26A H 0.1668 -0.0594 0.7954 0.022 Uiso 1 1 calc R . . H26B H 0.1356 -0.0785 0.8633 0.022 Uiso 1 1 calc R . . C31 C -0.1009(2) 0.21969(16) 0.77621(18) 0.0209(6) Uani 1 1 d . . . H31 H -0.1449 0.2066 0.8043 0.025 Uiso 1 1 calc R . . C32 C -0.0331(3) 0.26635(17) 0.8171(2) 0.0262(7) Uani 1 1 d . . . H32A H -0.0005 0.2464 0.8593 0.031 Uiso 1 1 calc R . . H32B H 0.0125 0.2785 0.7908 0.031 Uiso 1 1 calc R . . C33 C -0.0832(3) 0.32440(18) 0.8340(3) 0.0359(10) Uani 1 1 d . . . H33A H -0.0384 0.3545 0.8587 0.043 Uiso 1 1 calc R . . H33B H -0.1249 0.3125 0.8635 0.043 Uiso 1 1 calc R . . C34 C -0.1378(4) 0.3555(2) 0.7701(3) 0.0493(13) Uani 1 1 d . . . H34A H -0.1718 0.3915 0.7827 0.059 Uiso 1 1 calc R . . H34B H -0.0955 0.3712 0.7426 0.059 Uiso 1 1 calc R . . C35 C -0.2041(4) 0.3097(2) 0.7288(3) 0.0469(12) Uani 1 1 d . . . H35A H -0.2359 0.3300 0.6866 0.056 Uiso 1 1 calc R . . H35B H -0.2505 0.2976 0.7545 0.056 Uiso 1 1 calc R . . C36 C -0.1548(3) 0.2513(2) 0.7118(2) 0.0325(9) Uani 1 1 d . . . H36A H -0.1126 0.2629 0.6826 0.039 Uiso 1 1 calc R . . H36B H -0.1999 0.2216 0.6867 0.039 Uiso 1 1 calc R . . C41 C -0.1303(2) 0.09240(16) 0.71543(15) 0.0166(6) Uani 1 1 d . . . H41 H -0.1010 0.0506 0.7252 0.020 Uiso 1 1 calc R . . C42 C -0.1572(3) 0.09690(18) 0.63820(17) 0.0242(7) Uani 1 1 d . . . H42A H -0.1900 0.1365 0.6252 0.029 Uiso 1 1 calc R . . H42B H -0.1017 0.0968 0.6193 0.029 Uiso 1 1 calc R . . C43 C -0.2184(3) 0.0420(2) 0.60932(19) 0.0276(8) Uani 1 1 d . . . H43A H -0.2377 0.0469 0.5599 0.033 Uiso 1 1 calc R . . H43B H -0.1832 0.0028 0.6183 0.033 Uiso 1 1 calc R . . C44 C -0.3026(3) 0.0377(2) 0.6398(2) 0.0303(8) Uani 1 1 d . . . H44A H -0.3373 -0.0004 0.6231 0.036 Uiso 1 1 calc R . . H44B H -0.3423 0.0741 0.6254 0.036 Uiso 1 1 calc R . . C45 C -0.2765(2) 0.03575(19) 0.7170(2) 0.0269(7) Uani 1 1 d . . . H45A H -0.2442 -0.0037 0.7315 0.032 Uiso 1 1 calc R . . H45B H -0.3325 0.0367 0.7353 0.032 Uiso 1 1 calc R . . C46 C -0.2153(2) 0.09080(17) 0.74583(18) 0.0213(6) Uani 1 1 d . . . H46A H -0.2495 0.1303 0.7355 0.026 Uiso 1 1 calc R . . H46B H -0.1970 0.0867 0.7954 0.026 Uiso 1 1 calc R . . C51 C 0.4267(2) 0.13398(18) 0.75462(18) 0.0257(7) Uani 1 1 d DU . . H51A H 0.4689 0.1191 0.7259 0.031 Uiso 0.806(7) 1 calc PR A 1 H51B H 0.4076 0.1696 0.7802 0.031 Uiso 0.194(7) 1 calc PR A 2 C52 C 0.4439(2) 0.09109(17) 0.81638(16) 0.0215(7) Uani 1 1 d DU A . H52A H 0.4030 0.1034 0.8464 0.026 Uiso 0.806(7) 1 calc PR A 1 H52B H 0.4286 0.0478 0.8015 0.026 Uiso 0.806(7) 1 calc PR A 1 H52C H 0.4620 0.0491 0.8038 0.026 Uiso 0.194(7) 1 calc PR A 2 H52D H 0.3878 0.0870 0.8342 0.026 Uiso 0.194(7) 1 calc PR A 2 C53 C 0.5416(3) 0.0931(2) 0.8559(2) 0.0256(10) Uani 0.806(7) 1 d PDU A 1 H53A H 0.5481 0.0670 0.8967 0.031 Uiso 0.806(7) 1 calc PR A 1 H53B H 0.5827 0.0764 0.8280 0.031 Uiso 0.806(7) 1 calc PR A 1 C54 C 0.5677(4) 0.1599(2) 0.8757(2) 0.0302(12) Uani 0.806(7) 1 d PDU A 1 H54A H 0.6322 0.1614 0.8998 0.036 Uiso 0.806(7) 1 calc PR A 1 H54B H 0.5298 0.1752 0.9067 0.036 Uiso 0.806(7) 1 calc PR A 1 C55 C 0.5540(3) 0.2020(2) 0.8136(3) 0.0253(11) Uani 0.806(7) 1 d PDU A 1 H55A H 0.5953 0.1885 0.7844 0.030 Uiso 0.806(7) 1 calc PR A 1 H55B H 0.5699 0.2454 0.8280 0.030 Uiso 0.806(7) 1 calc PR A 1 C56 C 0.4551(3) 0.19972(19) 0.7736(2) 0.0196(9) Uani 0.806(7) 1 d PDU A 1 H56A H 0.4144 0.2176 0.8011 0.024 Uiso 0.806(7) 1 calc PR A 1 H56B H 0.4493 0.2252 0.7323 0.024 Uiso 0.806(7) 1 calc PR A 1 C2S C 0.0857(5) 0.2657(3) 1.0595(3) 0.0264(14) Uani 0.517(2) 1 d PDU B 1 H2S1 H 0.1448 0.2478 1.0551 0.032 Uiso 0.517(2) 1 calc PR B 1 H2S2 H 0.0395 0.2322 1.0504 0.032 Uiso 0.517(2) 1 calc PR B 1 Cl4S Cl 0.09470(13) 0.29311(9) 1.14271(9) 0.0304(4) Uani 0.517(2) 1 d PDU B 1 Cl3S Cl 0.05555(16) 0.32435(9) 1.00090(9) 0.0330(5) Uani 0.517(2) 1 d PDU B 1 C53A C 0.5227(10) 0.1206(10) 0.8717(7) 0.029(4) Uani 0.194(7) 1 d PDU A 2 H53C H 0.4966 0.1550 0.8940 0.034 Uiso 0.194(7) 1 calc PR A 2 H53D H 0.5450 0.0885 0.9062 0.034 Uiso 0.194(7) 1 calc PR A 2 C54A C 0.6040(10) 0.1460(9) 0.8460(8) 0.029(4) Uani 0.194(7) 1 d PDU A 2 H54C H 0.6479 0.1648 0.8840 0.035 Uiso 0.194(7) 1 calc PR A 2 H54D H 0.6349 0.1111 0.8282 0.035 Uiso 0.194(7) 1 calc PR A 2 C55A C 0.5764(11) 0.1948(8) 0.7908(8) 0.023(4) Uani 0.194(7) 1 d PDU A 2 H55C H 0.6298 0.2059 0.7720 0.028 Uiso 0.194(7) 1 calc PR A 2 H55D H 0.5555 0.2330 0.8104 0.028 Uiso 0.194(7) 1 calc PR A 2 C56A C 0.5002(8) 0.1706(7) 0.7345(7) 0.017(3) Uani 0.194(7) 1 d PDU A 2 H56C H 0.4719 0.2068 0.7078 0.021 Uiso 0.194(7) 1 calc PR A 2 H56D H 0.5282 0.1443 0.7043 0.021 Uiso 0.194(7) 1 calc PR A 2 C1S C 0.2524(5) 0.3069(3) 0.9302(4) 0.0235(14) Uani 0.483(2) 1 d PD B 2 H1S1 H 0.2134 0.3391 0.9446 0.028 Uiso 0.483(2) 1 calc PR B 2 H1S2 H 0.2119 0.2766 0.9016 0.028 Uiso 0.483(2) 1 calc PR B 2 Cl1S Cl 0.31342(15) 0.26811(12) 1.00174(11) 0.0379(5) Uani 0.483(2) 1 d PD B 2 Cl2S Cl 0.32222(17) 0.34239(12) 0.88192(14) 0.0441(6) Uani 0.483(2) 1 d PD B 2 C61 C 0.3285(2) 0.06926(16) 0.63568(16) 0.0188(6) Uani 1 1 d . . . H61 H 0.2665 0.0581 0.6093 0.023 Uiso 1 1 calc R A . C62 C 0.3810(2) 0.09578(18) 0.58468(17) 0.0224(7) Uani 1 1 d . A . H62A H 0.3521 0.1351 0.5654 0.027 Uiso 1 1 calc R . . H62B H 0.4445 0.1051 0.6077 0.027 Uiso 1 1 calc R . . C63 C 0.3810(3) 0.0487(2) 0.52828(19) 0.0294(8) Uani 1 1 d . . . H63A H 0.3177 0.0424 0.5029 0.035 Uiso 1 1 calc R A . H63B H 0.4169 0.0656 0.4968 0.035 Uiso 1 1 calc R . . C64 C 0.4210(3) -0.0136(2) 0.5556(2) 0.0349(10) Uani 1 1 d . A . H64A H 0.4864 -0.0083 0.5763 0.042 Uiso 1 1 calc R . . H64B H 0.4160 -0.0437 0.5181 0.042 Uiso 1 1 calc R . . C65 C 0.3716(3) -0.0397(2) 0.6083(2) 0.0320(8) Uani 1 1 d . . . H65A H 0.4017 -0.0786 0.6275 0.038 Uiso 1 1 calc R A . H65B H 0.3078 -0.0496 0.5866 0.038 Uiso 1 1 calc R . . C66 C 0.3727(3) 0.00775(18) 0.66482(19) 0.0252(7) Uani 1 1 d . A . H66A H 0.4364 0.0156 0.6886 0.030 Uiso 1 1 calc R . . H66B H 0.3391 -0.0093 0.6977 0.030 Uiso 1 1 calc R . . C71 C 0.1441(2) 0.16113(16) 0.54119(16) 0.0185(6) Uani 1 1 d . . . H71 H 0.1851 0.1243 0.5526 0.022 Uiso 1 1 calc R . . C72 C 0.1779(3) 0.19500(19) 0.48501(17) 0.0243(7) Uani 1 1 d . . . H72A H 0.2413 0.2092 0.5020 0.029 Uiso 1 1 calc R . . H72B H 0.1396 0.2321 0.4709 0.029 Uiso 1 1 calc R . . C73 C 0.1743(3) 0.1517(2) 0.42424(18) 0.0309(8) Uani 1 1 d . . . H73A H 0.1913 0.1754 0.3870 0.037 Uiso 1 1 calc R . . H73B H 0.2190 0.1176 0.4369 0.037 Uiso 1 1 calc R . . C74 C 0.0799(3) 0.1240(2) 0.4002(2) 0.0377(10) Uani 1 1 d . . . H74A H 0.0810 0.0944 0.3630 0.045 Uiso 1 1 calc R . . H74B H 0.0364 0.1577 0.3825 0.045 Uiso 1 1 calc R . . C75 C 0.0472(3) 0.0900(2) 0.4569(2) 0.0362(10) Uani 1 1 d . . . H75A H 0.0873 0.0539 0.4720 0.043 Uiso 1 1 calc R . . H75B H -0.0153 0.0741 0.4400 0.043 Uiso 1 1 calc R . . C76 C 0.0480(3) 0.1338(2) 0.51663(19) 0.0283(8) Uani 1 1 d . . . H76A H 0.0298 0.1106 0.5537 0.034 Uiso 1 1 calc R . . H76B H 0.0038 0.1679 0.5028 0.034 Uiso 1 1 calc R . . C81 C 0.1398(2) 0.28924(16) 0.60242(16) 0.0182(6) Uani 1 1 d . . . H81 H 0.1855 0.3035 0.5764 0.022 Uiso 1 1 calc R . . C82 C 0.0432(2) 0.30164(17) 0.56032(17) 0.0211(6) Uani 1 1 d . . . H82A H 0.0350 0.2790 0.5170 0.025 Uiso 1 1 calc R . . H82B H -0.0025 0.2858 0.5848 0.025 Uiso 1 1 calc R . . C83 C 0.0281(3) 0.37132(19) 0.5467(2) 0.0294(8) Uani 1 1 d . . . H83A H 0.0711 0.3865 0.5196 0.035 Uiso 1 1 calc R . . H83B H -0.0346 0.3782 0.5204 0.035 Uiso 1 1 calc R . . C84 C 0.0419(3) 0.40823(19) 0.6123(2) 0.0329(9) Uani 1 1 d . . . H84A H 0.0350 0.4533 0.6022 0.039 Uiso 1 1 calc R . . H84B H -0.0049 0.3961 0.6376 0.039 Uiso 1 1 calc R . . C85 C 0.1365(3) 0.39559(18) 0.6551(2) 0.0334(9) Uani 1 1 d . . . H85A H 0.1432 0.4178 0.6985 0.040 Uiso 1 1 calc R . . H85B H 0.1829 0.4122 0.6317 0.040 Uiso 1 1 calc R . . C86 C 0.1538(3) 0.32614(17) 0.66871(19) 0.0240(7) Uani 1 1 d . . . H86A H 0.1117 0.3103 0.6962 0.029 Uiso 1 1 calc R . . H86B H 0.2169 0.3200 0.6945 0.029 Uiso 1 1 calc R . . P1S P 0.85789(6) 0.16033(4) 0.97786(4) 0.01992(17) Uani 1 1 d . . . F1S F 0.92115(19) 0.11337(13) 1.02809(12) 0.0395(6) Uani 1 1 d . . . F2S F 0.79556(18) 0.20735(12) 0.92695(12) 0.0371(6) Uani 1 1 d . . . F3S F 0.77016(17) 0.13623(12) 1.00323(13) 0.0348(5) Uani 1 1 d . . . F4S F 0.94568(17) 0.18521(12) 0.95235(13) 0.0348(5) Uani 1 1 d . . . F5S F 0.87346(17) 0.21303(12) 1.03566(12) 0.0325(5) Uani 1 1 d . . . F6S F 0.84289(17) 0.10768(11) 0.92045(12) 0.0313(5) Uani 1 1 d . . . 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 Au1 0.01359(6) 0.01573(6) 0.01340(6) 0.00216(4) 0.00409(4) 0.00006(4) Rh1 0.01231(10) 0.01337(11) 0.01270(10) 0.00034(8) 0.00422(8) -0.00013(8) P1 0.0125(3) 0.0134(3) 0.0124(3) 0.0005(3) 0.0036(3) -0.0003(3) P2 0.0140(3) 0.0151(4) 0.0152(3) 0.0016(3) 0.0052(3) 0.0016(3) P3 0.0125(3) 0.0169(4) 0.0136(3) 0.0010(3) 0.0039(3) -0.0005(3) P4 0.0142(3) 0.0164(4) 0.0115(3) 0.0016(3) 0.0025(3) -0.0018(3) Cl1 0.0263(4) 0.0206(4) 0.0241(4) -0.0041(3) 0.0090(3) -0.0035(3) C1 0.0182(14) 0.0154(14) 0.0133(12) 0.0013(10) 0.0054(11) 0.0013(11) C2 0.0152(13) 0.0168(15) 0.0159(13) 0.0020(11) 0.0028(11) -0.0019(11) C3 0.0262(17) 0.0194(16) 0.0312(17) 0.0013(13) 0.0197(14) -0.0012(13) O1 0.0341(15) 0.0463(18) 0.0290(14) -0.0104(13) 0.0132(12) -0.0137(13) C11 0.0175(14) 0.0223(16) 0.0132(13) 0.0016(11) 0.0015(11) -0.0023(12) C12 0.0215(16) 0.045(2) 0.0180(15) -0.0048(15) 0.0033(13) 0.0047(16) C13 0.0261(19) 0.075(3) 0.0157(16) -0.0041(18) 0.0037(14) 0.005(2) C14 0.0244(18) 0.048(2) 0.0188(16) -0.0010(16) -0.0002(13) -0.0033(17) C15 0.0239(17) 0.0271(19) 0.0243(17) 0.0029(14) -0.0048(13) 0.0043(14) C16 0.0181(15) 0.0243(17) 0.0184(14) -0.0022(12) 0.0006(12) 0.0042(12) C21 0.0134(13) 0.0161(14) 0.0134(12) 0.0007(10) 0.0022(10) -0.0007(11) C22 0.0169(14) 0.0201(15) 0.0160(13) 0.0005(11) 0.0049(11) -0.0025(12) C23 0.0198(15) 0.0249(17) 0.0199(14) -0.0018(12) 0.0046(12) -0.0073(13) C24 0.0297(18) 0.0180(17) 0.0305(18) -0.0010(13) 0.0006(15) -0.0087(14) C25 0.0239(16) 0.0168(16) 0.0304(18) -0.0051(13) -0.0007(14) 0.0020(13) C26 0.0175(14) 0.0161(15) 0.0203(14) 0.0010(11) 0.0024(12) 0.0005(11) C31 0.0196(15) 0.0179(16) 0.0271(16) 0.0002(12) 0.0097(13) 0.0043(12) C32 0.0291(18) 0.0156(16) 0.037(2) -0.0043(14) 0.0139(15) -0.0009(13) C33 0.039(2) 0.0171(18) 0.055(3) -0.0071(17) 0.018(2) 0.0012(16) C34 0.055(3) 0.020(2) 0.077(4) 0.003(2) 0.023(3) 0.015(2) C35 0.048(3) 0.031(2) 0.060(3) 0.005(2) 0.007(2) 0.024(2) C36 0.034(2) 0.029(2) 0.035(2) 0.0061(16) 0.0073(17) 0.0140(16) C41 0.0157(13) 0.0195(15) 0.0147(13) 0.0009(11) 0.0036(11) 0.0008(11) C42 0.0259(17) 0.0292(19) 0.0168(14) -0.0003(13) 0.0031(13) -0.0030(14) C43 0.0233(17) 0.037(2) 0.0213(16) -0.0057(14) 0.0013(13) -0.0035(15) C44 0.0204(16) 0.037(2) 0.0307(19) -0.0077(16) 0.0000(14) -0.0028(15) C45 0.0182(15) 0.032(2) 0.0319(18) -0.0024(15) 0.0078(14) -0.0049(14) C46 0.0151(14) 0.0267(18) 0.0234(15) -0.0022(13) 0.0069(12) -0.0009(12) C51 0.0173(15) 0.034(2) 0.0232(16) 0.0110(14) -0.0023(12) -0.0062(14) C52 0.0216(16) 0.0230(17) 0.0195(15) 0.0052(12) 0.0032(12) 0.0029(12) C53 0.023(2) 0.027(2) 0.024(2) 0.0019(18) -0.0025(17) 0.0057(18) C54 0.029(2) 0.033(3) 0.022(2) -0.0001(18) -0.0085(19) -0.006(2) C55 0.024(2) 0.026(2) 0.023(2) -0.0018(18) -0.0026(18) -0.0081(19) C56 0.0193(19) 0.0183(19) 0.0200(18) -0.0016(14) 0.0012(14) -0.0054(15) C2S 0.018(3) 0.024(3) 0.037(4) -0.002(3) 0.006(3) 0.001(3) Cl4S 0.0315(9) 0.0276(9) 0.0298(8) 0.0030(7) 0.0014(7) -0.0085(7) Cl3S 0.0482(12) 0.0281(9) 0.0251(8) 0.0066(6) 0.0134(8) 0.0016(8) C53A 0.019(7) 0.046(11) 0.017(7) 0.006(7) -0.005(5) 0.015(7) C54A 0.021(7) 0.038(9) 0.023(7) -0.013(6) -0.004(6) 0.006(6) C55A 0.015(7) 0.030(9) 0.022(8) -0.014(6) 0.000(6) 0.006(6) C56A 0.006(6) 0.024(8) 0.023(7) 0.000(5) 0.004(5) 0.000(5) C1S 0.022(3) 0.013(3) 0.037(4) -0.007(3) 0.009(3) 0.002(3) Cl1S 0.0272(10) 0.0456(13) 0.0368(11) -0.0005(9) -0.0023(8) -0.0021(9) Cl2S 0.0364(12) 0.0370(12) 0.0630(16) 0.0053(11) 0.0197(11) -0.0156(9) C61 0.0157(14) 0.0220(16) 0.0203(14) -0.0012(12) 0.0076(12) 0.0012(12) C62 0.0190(15) 0.0315(19) 0.0189(14) -0.0056(13) 0.0089(12) -0.0039(13) C63 0.0228(17) 0.043(2) 0.0238(17) -0.0106(16) 0.0087(14) -0.0008(16) C64 0.0237(18) 0.046(3) 0.035(2) -0.0182(18) 0.0072(16) 0.0071(17) C65 0.0277(19) 0.029(2) 0.040(2) -0.0093(16) 0.0076(16) 0.0063(15) C66 0.0239(17) 0.0240(18) 0.0295(18) -0.0019(14) 0.0100(14) 0.0061(14) C71 0.0182(14) 0.0227(16) 0.0138(13) -0.0006(11) 0.0021(11) -0.0016(12) C72 0.0264(17) 0.0315(19) 0.0158(14) 0.0030(13) 0.0066(13) 0.0008(14) C73 0.034(2) 0.045(2) 0.0149(15) -0.0009(15) 0.0067(14) 0.0052(18) C74 0.037(2) 0.054(3) 0.0186(17) -0.0130(17) -0.0012(15) 0.003(2) C75 0.033(2) 0.043(2) 0.031(2) -0.0191(18) 0.0022(16) -0.0062(18) C76 0.0226(17) 0.037(2) 0.0253(17) -0.0091(15) 0.0059(14) -0.0076(15) C81 0.0173(14) 0.0182(15) 0.0193(14) 0.0055(11) 0.0043(11) -0.0012(12) C82 0.0206(15) 0.0219(16) 0.0200(15) 0.0047(12) 0.0029(12) 0.0036(13) C83 0.0294(19) 0.0261(19) 0.0312(19) 0.0087(15) 0.0032(15) 0.0077(15) C84 0.030(2) 0.0231(19) 0.042(2) -0.0005(16) 0.0010(17) 0.0066(15) C85 0.0284(19) 0.0174(17) 0.049(2) -0.0027(16) -0.0033(17) 0.0016(14) C86 0.0228(16) 0.0200(17) 0.0262(17) -0.0009(13) -0.0017(13) -0.0008(13) P1S 0.0217(4) 0.0227(4) 0.0169(4) -0.0008(3) 0.0077(3) 0.0031(3) F1S 0.0465(15) 0.0431(15) 0.0288(12) 0.0101(11) 0.0073(11) 0.0211(12) F2S 0.0457(15) 0.0374(14) 0.0276(12) 0.0053(10) 0.0065(10) 0.0174(11) F3S 0.0329(12) 0.0402(14) 0.0383(13) -0.0061(11) 0.0231(11) -0.0074(11) F4S 0.0334(13) 0.0351(13) 0.0425(14) -0.0087(11) 0.0231(11) -0.0070(10) F5S 0.0332(12) 0.0375(13) 0.0281(11) -0.0136(10) 0.0093(10) 0.0017(10) F6S 0.0387(13) 0.0301(12) 0.0280(11) -0.0100(9) 0.0137(10) -0.0034(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P2 2.3048(8) . ? Au1 P4 2.3089(8) . ? Au1 Rh1 2.9250(4) . ? Rh1 C3 1.828(4) . ? Rh1 P3 2.3333(8) . ? Rh1 P1 2.3402(8) . ? Rh1 Cl1 2.3749(9) . ? P1 C1 1.845(3) . ? P1 C21 1.846(3) . ? P1 C11 1.869(3) . ? P2 C1 1.832(3) . ? P2 C31 1.844(3) . ? P2 C41 1.846(3) . ? P3 C2 1.848(3) . ? P3 C61 1.853(3) . ? P3 C51 1.853(3) . ? P4 C2 1.839(3) . ? P4 C81 1.841(3) . ? P4 C71 1.848(3) . ? C3 O1 1.129(5) . ? C11 C12 1.535(5) . ? C11 C16 1.535(5) . ? C12 C13 1.538(5) . ? C13 C14 1.539(6) . ? C14 C15 1.525(6) . ? C15 C16 1.529(5) . ? C21 C22 1.532(4) . ? C21 C26 1.543(4) . ? C22 C23 1.537(5) . ? C23 C24 1.531(5) . ? C24 C25 1.529(6) . ? C25 C26 1.532(5) . ? C31 C32 1.541(5) . ? C31 C36 1.543(5) . ? C32 C33 1.532(5) . ? C33 C34 1.534(7) . ? C34 C35 1.519(8) . ? C35 C36 1.533(6) . ? C41 C46 1.534(4) . ? C41 C42 1.539(4) . ? C42 C43 1.533(5) . ? C43 C44 1.526(5) . ? C44 C45 1.534(6) . ? C45 C46 1.535(5) . ? C51 C56A 1.482(11) . ? C51 C56 1.501(5) . ? C51 C52 1.534(5) . ? C52 C53 1.518(5) . ? C52 C53A 1.581(12) . ? C53 C54 1.517(7) . ? C54 C55 1.531(6) . ? C55 C56 1.536(6) . ? C2S Cl3S 1.727(7) . ? C2S Cl4S 1.768(7) . ? C53A C54A 1.528(13) . ? C54A C55A 1.526(13) . ? C55A C56A 1.529(12) . ? C1S Cl1S 1.756(7) . ? C1S Cl2S 1.756(7) . ? C61 C62 1.539(5) . ? C61 C66 1.539(5) . ? C62 C63 1.528(5) . ? C63 C64 1.524(6) . ? C64 C65 1.532(6) . ? C65 C66 1.532(5) . ? C71 C72 1.529(5) . ? C71 C76 1.540(5) . ? C72 C73 1.538(5) . ? C73 C74 1.520(6) . ? C74 C75 1.531(7) . ? C75 C76 1.533(5) . ? C81 C86 1.538(5) . ? C81 C82 1.544(5) . ? C82 C83 1.530(5) . ? C83 C84 1.526(6) . ? C84 C85 1.526(6) . ? C85 C86 1.529(5) . ? P1S F1S 1.597(3) . ? P1S F2S 1.599(3) . ? P1S F3S 1.600(2) . ? P1S F6S 1.606(2) . ? P1S F4S 1.608(3) . ? P1S F5S 1.612(2) . ? 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 P2 Au1 P4 172.98(3) . . ? P2 Au1 Rh1 94.95(2) . . ? P4 Au1 Rh1 91.40(2) . . ? C3 Rh1 P3 90.98(11) . . ? C3 Rh1 P1 92.30(11) . . ? P3 Rh1 P1 175.41(3) . . ? C3 Rh1 Cl1 171.67(12) . . ? P3 Rh1 Cl1 88.73(3) . . ? P1 Rh1 Cl1 88.49(3) . . ? C3 Rh1 Au1 91.20(12) . . ? P3 Rh1 Au1 93.13(2) . . ? P1 Rh1 Au1 90.01(2) . . ? Cl1 Rh1 Au1 80.50(2) . . ? C1 P1 C21 106.21(14) . . ? C1 P1 C11 104.20(14) . . ? C21 P1 C11 104.55(14) . . ? C1 P1 Rh1 112.52(10) . . ? C21 P1 Rh1 113.22(10) . . ? C11 P1 Rh1 115.22(11) . . ? C1 P2 C31 104.73(15) . . ? C1 P2 C41 106.04(15) . . ? C31 P2 C41 108.40(16) . . ? C1 P2 Au1 110.41(10) . . ? C31 P2 Au1 112.81(12) . . ? C41 P2 Au1 113.84(10) . . ? C2 P3 C61 106.50(15) . . ? C2 P3 C51 105.84(16) . . ? C61 P3 C51 103.25(17) . . ? C2 P3 Rh1 110.46(11) . . ? C61 P3 Rh1 115.44(11) . . ? C51 P3 Rh1 114.54(12) . . ? C2 P4 C81 104.41(15) . . ? C2 P4 C71 105.61(15) . . ? C81 P4 C71 110.19(15) . . ? C2 P4 Au1 111.93(10) . . ? C81 P4 Au1 110.53(11) . . ? C71 P4 Au1 113.67(11) . . ? P2 C1 P1 116.46(16) . . ? P4 C2 P3 115.09(17) . . ? O1 C3 Rh1 176.1(4) . . ? C12 C11 C16 110.2(3) . . ? C12 C11 P1 114.9(2) . . ? C16 C11 P1 111.1(2) . . ? C11 C12 C13 110.1(3) . . ? C12 C13 C14 111.9(3) . . ? C15 C14 C13 110.4(3) . . ? C14 C15 C16 111.7(3) . . ? C15 C16 C11 111.5(3) . . ? C22 C21 C26 109.8(3) . . ? C22 C21 P1 117.1(2) . . ? C26 C21 P1 110.9(2) . . ? C21 C22 C23 109.3(3) . . ? C24 C23 C22 111.6(3) . . ? C25 C24 C23 111.8(3) . . ? C24 C25 C26 111.7(3) . . ? C25 C26 C21 110.3(3) . . ? C32 C31 C36 109.9(3) . . ? C32 C31 P2 111.7(2) . . ? C36 C31 P2 109.9(3) . . ? C33 C32 C31 110.5(3) . . ? C32 C33 C34 111.4(4) . . ? C35 C34 C33 110.9(4) . . ? C34 C35 C36 111.2(4) . . ? C35 C36 C31 111.1(4) . . ? C46 C41 C42 110.5(3) . . ? C46 C41 P2 115.1(2) . . ? C42 C41 P2 113.5(2) . . ? C43 C42 C41 110.4(3) . . ? C44 C43 C42 111.9(3) . . ? C43 C44 C45 111.3(3) . . ? C44 C45 C46 111.8(3) . . ? C41 C46 C45 110.3(3) . . ? C56A C51 C56 52.0(7) . . ? C56A C51 C52 122.5(6) . . ? C56 C51 C52 111.4(3) . . ? C56A C51 P3 125.6(6) . . ? C56 C51 P3 116.7(3) . . ? C52 C51 P3 111.1(2) . . ? C53 C52 C51 113.1(3) . . ? C53 C52 C53A 28.1(8) . . ? C51 C52 C53A 108.2(7) . . ? C54 C53 C52 109.5(4) . . ? C53 C54 C55 110.9(4) . . ? C54 C55 C56 111.3(4) . . ? C51 C56 C55 110.9(4) . . ? Cl3S C2S Cl4S 111.9(4) . . ? C54A C53A C52 115.6(11) . . ? C55A C54A C53A 112.6(12) . . ? C54A C55A C56A 111.1(11) . . ? C51 C56A C55A 117.2(10) . . ? Cl1S C1S Cl2S 113.5(4) . . ? C62 C61 C66 109.6(3) . . ? C62 C61 P3 116.4(2) . . ? C66 C61 P3 111.5(2) . . ? C63 C62 C61 110.0(3) . . ? C64 C63 C62 111.7(3) . . ? C63 C64 C65 111.3(3) . . ? C64 C65 C66 110.6(4) . . ? C65 C66 C61 110.2(3) . . ? C72 C71 C76 112.1(3) . . ? C72 C71 P4 114.7(2) . . ? C76 C71 P4 113.2(2) . . ? C71 C72 C73 110.6(3) . . ? C74 C73 C72 111.5(3) . . ? C73 C74 C75 111.8(3) . . ? C74 C75 C76 110.7(4) . . ? C75 C76 C71 109.9(3) . . ? C86 C81 C82 109.5(3) . . ? C86 C81 P4 109.9(2) . . ? C82 C81 P4 110.5(2) . . ? C83 C82 C81 110.8(3) . . ? C84 C83 C82 111.3(3) . . ? C85 C84 C83 110.1(3) . . ? C84 C85 C86 112.3(3) . . ? C85 C86 C81 110.9(3) . . ? F1S P1S F2S 179.23(15) . . ? F1S P1S F3S 90.54(15) . . ? F2S P1S F3S 90.17(15) . . ? F1S P1S F6S 89.59(14) . . ? F2S P1S F6S 90.09(14) . . ? F3S P1S F6S 90.48(13) . . ? F1S P1S F4S 89.88(15) . . ? F2S P1S F4S 89.42(15) . . ? F3S P1S F4S 179.45(15) . . ? F6S P1S F4S 89.88(13) . . ? F1S P1S F5S 90.15(14) . . ? F2S P1S F5S 90.17(14) . . ? F3S P1S F5S 89.66(13) . . ? F6S P1S F5S 179.70(17) . . ? F4S P1S F5S 89.98(13) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.246 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.142 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 789595' #TrackingRef '- CIF final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H102 Au Br F6 O2 P5 Rh' _chemical_formula_weight 1444.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.0137(12) _cell_length_b 21.2486(17) _cell_length_c 20.3833(16) _cell_angle_alpha 90.00 _cell_angle_beta 102.5770(10) _cell_angle_gamma 90.00 _cell_volume 6346.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9337 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 31.54 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2944 _exptl_absorpt_coefficient_mu 3.379 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3116 _exptl_absorpt_correction_T_max 0.3843 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 147939 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 31.00 _reflns_number_total 19764 _reflns_number_gt 16736 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0234P)^2^+9.6865P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19764 _refine_ls_number_parameters 698 _refine_ls_number_restraints 338 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0640 _refine_ls_wR_factor_gt 0.0597 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.063401(6) 0.671678(4) -0.310836(4) 0.01283(3) Uani 1 1 d . A . Rh1 Rh 0.205792(12) 0.590136(9) -0.235083(9) 0.01155(4) Uani 1 1 d D . . Br1 Br 0.23663(2) 0.690171(14) -0.167762(14) 0.01811(9) Uani 0.9236(14) 1 d PDU A 1 C3 C 0.1711(2) 0.52498(14) -0.29190(14) 0.0182(5) Uani 0.9236(14) 1 d PDU A 1 O1 O 0.1459(2) 0.48566(16) -0.33126(13) 0.0315(6) Uani 0.9236(14) 1 d PDU A 1 Br1A Br 0.1283(3) 0.5183(3) -0.3307(2) 0.0233(12) Uani 0.0764(14) 1 d PDU A 2 C3A C 0.246(2) 0.6533(13) -0.1756(13) 0.0182(5) Uani 0.0764(14) 1 d PDU A 2 O1A O 0.270(2) 0.6935(13) -0.1371(15) 0.0315(6) Uani 0.0764(14) 1 d PDU A 2 P3 P 0.31239(4) 0.62203(3) -0.29638(3) 0.01419(12) Uani 1 1 d D A . P4 P 0.15717(4) 0.70432(3) -0.38024(3) 0.01364(12) Uani 1 1 d . . . P1 P 0.10714(4) 0.55844(3) -0.16673(3) 0.01211(11) Uani 1 1 d D A . P2 P -0.04047(4) 0.65031(3) -0.24547(3) 0.01258(11) Uani 1 1 d . . . P1S P 0.13912(5) 0.33648(3) 0.02198(3) 0.01869(13) Uani 1 1 d . . . F1S F 0.07934(14) 0.38638(10) -0.02757(9) 0.0393(5) Uani 1 1 d . . . F2S F 0.15516(12) 0.38804(9) 0.08102(8) 0.0291(4) Uani 1 1 d . . . F3S F 0.22934(13) 0.35986(10) -0.00046(9) 0.0342(4) Uani 1 1 d . . . F4S F 0.04920(13) 0.31257(10) 0.04482(10) 0.0343(4) Uani 1 1 d . . . F5S F 0.12315(13) 0.28491(9) -0.03718(9) 0.0332(4) Uani 1 1 d . . . F6S F 0.19846(13) 0.28675(9) 0.07243(9) 0.0329(4) Uani 1 1 d . . . C2 C 0.27880(17) 0.69755(12) -0.33939(12) 0.0153(5) Uani 1 1 d . A . H2A H 0.2945 0.7320 -0.3061 0.018 Uiso 1 1 calc R . . H2B H 0.3153 0.7038 -0.3739 0.018 Uiso 1 1 calc R . . C1 C 0.01714(16) 0.61694(12) -0.16465(11) 0.0135(4) Uani 1 1 d . A . H1A H -0.0295 0.5970 -0.1438 0.016 Uiso 1 1 calc R . . H1B H 0.0445 0.6519 -0.1349 0.016 Uiso 1 1 calc R . . C11 C 0.33016(18) 0.56599(13) -0.36203(13) 0.0198(5) Uani 1 1 d . . . H11 H 0.2679 0.5550 -0.3884 0.024 Uiso 1 1 calc R A . C12 C 0.3728(2) 0.50369(15) -0.33131(15) 0.0273(6) Uani 1 1 d . A . H12A H 0.4369 0.5110 -0.3077 0.033 Uiso 1 1 calc R . . H12B H 0.3388 0.4881 -0.2981 0.033 Uiso 1 1 calc R . . C13 C 0.3697(2) 0.45450(16) -0.38644(18) 0.0349(7) Uani 1 1 d . . . H13A H 0.3987 0.4151 -0.3663 0.042 Uiso 1 1 calc R A . H13B H 0.3053 0.4450 -0.4078 0.042 Uiso 1 1 calc R . . C14 C 0.4189(2) 0.47786(18) -0.43952(17) 0.0385(8) Uani 1 1 d . A . H14A H 0.4849 0.4821 -0.4193 0.046 Uiso 1 1 calc R . . H14B H 0.4119 0.4466 -0.4763 0.046 Uiso 1 1 calc R . . C15 C 0.3818(2) 0.54089(17) -0.46830(15) 0.0329(7) Uani 1 1 d . . . H15A H 0.3184 0.5352 -0.4942 0.039 Uiso 1 1 calc R A . H15B H 0.4190 0.5562 -0.4997 0.039 Uiso 1 1 calc R . . C16 C 0.38294(19) 0.59048(15) -0.41324(13) 0.0240(6) Uani 1 1 d . A . H16A H 0.4467 0.5998 -0.3903 0.029 Uiso 1 1 calc R . . H16B H 0.3547 0.6299 -0.4337 0.029 Uiso 1 1 calc R . . C22 C 0.44911(19) 0.59224(15) -0.18311(13) 0.0234(6) Uani 1 1 d DU . . H22A H 0.4114 0.6095 -0.1531 0.028 Uiso 0.680(5) 1 calc PR B 1 H22B H 0.4296 0.5482 -0.1938 0.028 Uiso 0.680(5) 1 calc PR B 1 H22C H 0.4711 0.5550 -0.2041 0.028 Uiso 0.320(5) 1 d PR B 2 H22D H 0.3972 0.5797 -0.1632 0.028 Uiso 0.320(5) 1 d PR B 2 C21 C 0.4307(3) 0.6304(2) -0.2483(2) 0.0154(8) Uani 0.680(5) 1 d PDU A 1 H21 H 0.4712 0.6131 -0.2769 0.019 Uiso 0.680(5) 1 calc PR B 1 C23 C 0.5475(3) 0.5923(2) -0.1461(2) 0.0250(10) Uani 0.680(5) 1 d PDU A 1 H23A H 0.5861 0.5734 -0.1745 0.030 Uiso 0.680(5) 1 calc PR B 1 H23B H 0.5547 0.5671 -0.1044 0.030 Uiso 0.680(5) 1 calc PR B 1 C24 C 0.5766(3) 0.6597(2) -0.1290(2) 0.0285(11) Uani 0.680(5) 1 d PDU A 1 H24A H 0.6420 0.6606 -0.1064 0.034 Uiso 0.680(5) 1 calc PR B 1 H24B H 0.5411 0.6770 -0.0976 0.034 Uiso 0.680(5) 1 calc PR B 1 C25 C 0.5614(4) 0.7006(3) -0.1925(3) 0.0248(12) Uani 0.680(5) 1 d PDU A 1 H25A H 0.6011 0.6856 -0.2222 0.030 Uiso 0.680(5) 1 calc PR B 1 H25B H 0.5785 0.7447 -0.1798 0.030 Uiso 0.680(5) 1 calc PR B 1 C26 C 0.4611(3) 0.69830(18) -0.23090(19) 0.0187(8) Uani 0.680(5) 1 d PDU A 1 H26A H 0.4219 0.7173 -0.2029 0.022 Uiso 0.680(5) 1 calc PR B 1 H26B H 0.4537 0.7232 -0.2728 0.022 Uiso 0.680(5) 1 calc PR B 1 C21A C 0.4224(7) 0.6481(5) -0.2353(5) 0.0154(8) Uani 0.320(5) 1 d PDU A 2 H21A H 0.4063 0.6850 -0.2098 0.019 Uiso 0.320(5) 1 calc PR B 2 C23A C 0.5295(6) 0.6233(6) -0.1274(4) 0.031(2) Uani 0.320(5) 1 d PDU A 2 H23C H 0.5045 0.6594 -0.1064 0.037 Uiso 0.320(5) 1 calc PR B 2 H23D H 0.5522 0.5920 -0.0918 0.037 Uiso 0.320(5) 1 calc PR B 2 C24A C 0.6091(6) 0.6461(5) -0.1569(5) 0.031(2) Uani 0.320(5) 1 d PDU A 2 H24C H 0.6560 0.6653 -0.1207 0.037 Uiso 0.320(5) 1 calc PR B 2 H24D H 0.6371 0.6097 -0.1749 0.037 Uiso 0.320(5) 1 calc PR B 2 C25A C 0.5787(7) 0.6941(5) -0.2128(5) 0.024(2) Uani 0.320(5) 1 d PDU A 2 H25C H 0.6304 0.7042 -0.2339 0.029 Uiso 0.320(5) 1 calc PR B 2 H25D H 0.5597 0.7334 -0.1936 0.029 Uiso 0.320(5) 1 calc PR B 2 C26A C 0.4985(5) 0.6683(4) -0.2666(4) 0.0215(18) Uani 0.320(5) 1 d PDU A 2 H26C H 0.5196 0.6320 -0.2897 0.026 Uiso 0.320(5) 1 calc PR B 2 H26D H 0.4765 0.7012 -0.3005 0.026 Uiso 0.320(5) 1 calc PR B 2 C31 C 0.14048(18) 0.78865(13) -0.39866(13) 0.0187(5) Uani 1 1 d . A . H31 H 0.1872 0.8032 -0.4235 0.022 Uiso 1 1 calc R . . C32 C 0.1524(2) 0.82573(13) -0.33248(15) 0.0242(6) Uani 1 1 d . . . H32A H 0.1094 0.8094 -0.3060 0.029 Uiso 1 1 calc R A . H32B H 0.2152 0.8197 -0.3057 0.029 Uiso 1 1 calc R . . C33 C 0.1348(2) 0.89604(15) -0.34584(19) 0.0370(8) Uani 1 1 d . A . H33A H 0.1399 0.9182 -0.3025 0.044 Uiso 1 1 calc R . . H33B H 0.1819 0.9133 -0.3681 0.044 Uiso 1 1 calc R . . C34 C 0.0411(2) 0.90816(16) -0.38990(18) 0.0351(7) Uani 1 1 d . . . H34A H 0.0336 0.9537 -0.3997 0.042 Uiso 1 1 calc R A . H34B H -0.0065 0.8951 -0.3658 0.042 Uiso 1 1 calc R . . C35 C 0.0293(2) 0.87181(16) -0.45530(16) 0.0327(7) Uani 1 1 d . A . H35A H 0.0734 0.8876 -0.4812 0.039 Uiso 1 1 calc R . . H35B H -0.0330 0.8787 -0.4826 0.039 Uiso 1 1 calc R . . C36 C 0.0447(2) 0.80142(14) -0.44203(14) 0.0227(6) Uani 1 1 d . . . H36A H 0.0376 0.7789 -0.4854 0.027 Uiso 1 1 calc R A . H36B H -0.0019 0.7851 -0.4187 0.027 Uiso 1 1 calc R . . C41 C 0.14325(18) 0.65932(13) -0.45912(12) 0.0179(5) Uani 1 1 d . A . H41 H 0.1817 0.6208 -0.4474 0.022 Uiso 1 1 calc R . . C42 C 0.0458(2) 0.63531(17) -0.48512(15) 0.0299(7) Uani 1 1 d . . . H42A H 0.0041 0.6714 -0.4984 0.036 Uiso 1 1 calc R A . H42B H 0.0254 0.6120 -0.4490 0.036 Uiso 1 1 calc R . . C43 C 0.0421(2) 0.59191(18) -0.54563(16) 0.0368(8) Uani 1 1 d . A . H43A H 0.0797 0.5540 -0.5313 0.044 Uiso 1 1 calc R . . H43B H -0.0216 0.5781 -0.5632 0.044 Uiso 1 1 calc R . . C44 C 0.0771(2) 0.62535(19) -0.60100(15) 0.0377(8) Uani 1 1 d . . . H44A H 0.0759 0.5959 -0.6388 0.045 Uiso 1 1 calc R A . H44B H 0.0365 0.6612 -0.6179 0.045 Uiso 1 1 calc R . . C45 C 0.1739(2) 0.64932(17) -0.57555(14) 0.0306(7) Uani 1 1 d . A . H45A H 0.1936 0.6727 -0.6120 0.037 Uiso 1 1 calc R . . H45B H 0.2156 0.6131 -0.5630 0.037 Uiso 1 1 calc R . . C46 C 0.1807(2) 0.69260(15) -0.51444(13) 0.0247(6) Uani 1 1 d . . . H46A H 0.1455 0.7316 -0.5282 0.030 Uiso 1 1 calc R A . H46B H 0.2452 0.7044 -0.4967 0.030 Uiso 1 1 calc R . . C51 C 0.16200(18) 0.54562(14) -0.07649(12) 0.0199(5) Uani 1 1 d . . . H51 H 0.1374 0.5047 -0.0640 0.024 Uiso 1 1 calc R A . C52 C 0.26468(18) 0.53621(14) -0.06646(13) 0.0210(5) Uani 1 1 d . A . H52A H 0.2767 0.5020 -0.0964 0.025 Uiso 1 1 calc R . . H52B H 0.2925 0.5752 -0.0794 0.025 Uiso 1 1 calc R . . C53 C 0.3093(2) 0.51975(16) 0.00592(15) 0.0299(7) Uani 1 1 d . . . H53A H 0.2891 0.4773 0.0164 0.036 Uiso 1 1 calc R A . H53B H 0.3763 0.5185 0.0108 0.036 Uiso 1 1 calc R . . C54 C 0.2863(2) 0.56616(19) 0.05558(15) 0.0357(8) Uani 1 1 d . A . H54A H 0.3142 0.6074 0.0498 0.043 Uiso 1 1 calc R . . H54B H 0.3118 0.5513 0.1019 0.043 Uiso 1 1 calc R . . C55 C 0.1828(2) 0.5737(2) 0.04523(14) 0.0423(10) Uani 1 1 d . . . H55A H 0.1691 0.6058 0.0768 0.051 Uiso 1 1 calc R A . H55B H 0.1558 0.5333 0.0553 0.051 Uiso 1 1 calc R . . C56 C 0.1393(2) 0.59372(18) -0.02764(14) 0.0339(8) Uani 1 1 d . A . H56A H 0.0723 0.5969 -0.0333 0.041 Uiso 1 1 calc R . . H56B H 0.1629 0.6355 -0.0370 0.041 Uiso 1 1 calc R . . C61 C 0.04752(17) 0.48381(12) -0.19387(12) 0.0144(4) Uani 1 1 d . . . H61 H 0.0239 0.4875 -0.2435 0.017 Uiso 1 1 calc R A . C62 C -0.03538(17) 0.46795(12) -0.16391(12) 0.0167(5) Uani 1 1 d . A . H62A H -0.0151 0.4596 -0.1152 0.020 Uiso 1 1 calc R . . H62B H -0.0781 0.5040 -0.1700 0.020 Uiso 1 1 calc R . . C63 C -0.08349(19) 0.40982(13) -0.19939(13) 0.0210(5) Uani 1 1 d . . . H63A H -0.1364 0.3992 -0.1797 0.025 Uiso 1 1 calc R A . H63B H -0.1068 0.4195 -0.2476 0.025 Uiso 1 1 calc R . . C64 C -0.0198(2) 0.35345(14) -0.19283(15) 0.0265(6) Uani 1 1 d . A . H64A H -0.0518 0.3180 -0.2195 0.032 Uiso 1 1 calc R . . H64B H -0.0034 0.3401 -0.1452 0.032 Uiso 1 1 calc R . . C65 C 0.0673(2) 0.36836(14) -0.21697(15) 0.0251(6) Uani 1 1 d . . . H65A H 0.0521 0.3744 -0.2663 0.030 Uiso 1 1 calc R A . H65B H 0.1098 0.3323 -0.2068 0.030 Uiso 1 1 calc R . . C66 C 0.11438(18) 0.42783(12) -0.18325(13) 0.0186(5) Uani 1 1 d . A . H66A H 0.1677 0.4380 -0.2026 0.022 Uiso 1 1 calc R . . H66B H 0.1365 0.4201 -0.1345 0.022 Uiso 1 1 calc R . . C71 C -0.12798(17) 0.59211(12) -0.28387(12) 0.0146(5) Uani 1 1 d . A . H71 H -0.0990 0.5499 -0.2729 0.018 Uiso 1 1 calc R . . C72 C -0.21412(18) 0.59169(14) -0.25456(13) 0.0198(5) Uani 1 1 d . . . H72A H -0.2479 0.6317 -0.2658 0.024 Uiso 1 1 calc R A . H72B H -0.1965 0.5881 -0.2050 0.024 Uiso 1 1 calc R . . C73 C -0.2757(2) 0.53596(15) -0.28359(15) 0.0255(6) Uani 1 1 d . A . H73A H -0.2439 0.4960 -0.2682 0.031 Uiso 1 1 calc R . . H73B H -0.3324 0.5375 -0.2664 0.031 Uiso 1 1 calc R . . C74 C -0.2999(2) 0.53709(16) -0.36007(15) 0.0276(6) Uani 1 1 d . . . H74A H -0.3389 0.5741 -0.3755 0.033 Uiso 1 1 calc R A . H74B H -0.3353 0.4988 -0.3768 0.033 Uiso 1 1 calc R . . C75 C -0.2144(2) 0.54007(15) -0.38953(14) 0.0270(6) Uani 1 1 d . A . H75A H -0.1796 0.5004 -0.3793 0.032 Uiso 1 1 calc R . . H75B H -0.2328 0.5442 -0.4390 0.032 Uiso 1 1 calc R . . C76 C -0.15328(19) 0.59551(14) -0.36096(13) 0.0218(5) Uani 1 1 d . . . H76A H -0.1856 0.6355 -0.3751 0.026 Uiso 1 1 calc R A . H76B H -0.0970 0.5947 -0.3788 0.026 Uiso 1 1 calc R . . C81 C -0.09875(17) 0.72094(12) -0.22322(13) 0.0168(5) Uani 1 1 d . A . H81 H -0.1437 0.7076 -0.1962 0.020 Uiso 1 1 calc R . . C82 C -0.03127(19) 0.76764(13) -0.18119(14) 0.0214(5) Uani 1 1 d . . . H82A H 0.0013 0.7469 -0.1393 0.026 Uiso 1 1 calc R A . H82B H 0.0145 0.7807 -0.2069 0.026 Uiso 1 1 calc R . . C83 C -0.0822(2) 0.82565(14) -0.16378(17) 0.0299(7) Uani 1 1 d . A . H83A H -0.1250 0.8128 -0.1356 0.036 Uiso 1 1 calc R . . H83B H -0.0379 0.8556 -0.1375 0.036 Uiso 1 1 calc R . . C84 C -0.1351(3) 0.85801(16) -0.2271(2) 0.0417(9) Uani 1 1 d . . . H84A H -0.1699 0.8939 -0.2144 0.050 Uiso 1 1 calc R A . H84B H -0.0917 0.8748 -0.2531 0.050 Uiso 1 1 calc R . . C85 C -0.2004(3) 0.81233(17) -0.2707(2) 0.0411(9) Uani 1 1 d . A . H85A H -0.2306 0.8336 -0.3129 0.049 Uiso 1 1 calc R . . H85B H -0.2483 0.7997 -0.2468 0.049 Uiso 1 1 calc R . . C86 C -0.1510(2) 0.75378(15) -0.28761(15) 0.0274(6) Uani 1 1 d . . . H86A H -0.1076 0.7659 -0.3157 0.033 Uiso 1 1 calc R A . H86B H -0.1959 0.7242 -0.3139 0.033 Uiso 1 1 calc R . . O1S O -0.3129(2) 0.6951(2) -0.4605(2) 0.0891(14) Uani 1 1 d . . . C1S C -0.4167(4) 0.7116(3) -0.3900(4) 0.088(2) Uani 1 1 d . . . H1S1 H -0.4084 0.6687 -0.3722 0.133 Uiso 1 1 calc R . . H1S2 H -0.4785 0.7261 -0.3895 0.133 Uiso 1 1 calc R . . H1S3 H -0.3720 0.7396 -0.3622 0.133 Uiso 1 1 calc R . . C4S C -0.1970(4) 0.6906(3) -0.5221(3) 0.091(2) Uani 1 1 d . . . H4S1 H -0.1548 0.7226 -0.4987 0.136 Uiso 1 1 calc R . . H4S2 H -0.1915 0.6879 -0.5690 0.136 Uiso 1 1 calc R . . H4S3 H -0.1821 0.6497 -0.5001 0.136 Uiso 1 1 calc R . . C3S C -0.2905(4) 0.7079(3) -0.5196(3) 0.0780(17) Uani 1 1 d . . . H3S1 H -0.2987 0.7535 -0.5288 0.094 Uiso 1 1 calc R . . H3S2 H -0.3330 0.6851 -0.5558 0.094 Uiso 1 1 calc R . . C2S C -0.4043(4) 0.7122(4) -0.4562(3) 0.099(2) Uani 1 1 d . . . H2S1 H -0.4180 0.7548 -0.4753 0.119 Uiso 1 1 calc R . . H2S2 H -0.4479 0.6825 -0.4836 0.119 Uiso 1 1 calc R . . 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 Au1 0.01211(4) 0.01463(5) 0.01191(4) 0.00177(3) 0.00293(3) -0.00056(3) Rh1 0.01107(8) 0.01262(9) 0.01146(8) 0.00058(6) 0.00353(6) -0.00024(7) Br1 0.02117(16) 0.01580(16) 0.01827(14) -0.00309(10) 0.00623(10) -0.00260(11) C3 0.0179(14) 0.0217(15) 0.0163(13) 0.0005(10) 0.0067(11) -0.0002(11) O1 0.0406(16) 0.0274(16) 0.0299(13) -0.0128(12) 0.0149(11) -0.0093(13) Br1A 0.025(2) 0.027(3) 0.0198(19) -0.0035(16) 0.0090(15) -0.0064(18) C3A 0.0179(14) 0.0217(15) 0.0163(13) 0.0005(10) 0.0067(11) -0.0002(11) O1A 0.0406(16) 0.0274(16) 0.0299(13) -0.0128(12) 0.0149(11) -0.0093(13) P3 0.0118(3) 0.0182(3) 0.0130(3) 0.0017(2) 0.0036(2) -0.0005(2) P4 0.0137(3) 0.0161(3) 0.0112(3) 0.0017(2) 0.0029(2) -0.0018(2) P1 0.0117(3) 0.0135(3) 0.0114(3) 0.0011(2) 0.0031(2) 0.0002(2) P2 0.0116(3) 0.0133(3) 0.0130(3) 0.0007(2) 0.0032(2) 0.0004(2) P1S 0.0187(3) 0.0236(4) 0.0143(3) -0.0019(2) 0.0047(2) 0.0028(3) F1S 0.0471(12) 0.0441(12) 0.0256(9) 0.0089(8) 0.0060(8) 0.0235(10) F2S 0.0339(10) 0.0297(10) 0.0255(8) -0.0109(7) 0.0107(7) -0.0022(8) F3S 0.0314(10) 0.0407(12) 0.0368(10) -0.0042(8) 0.0209(8) -0.0031(9) F4S 0.0257(9) 0.0401(11) 0.0415(11) -0.0092(8) 0.0170(8) -0.0069(8) F5S 0.0312(10) 0.0409(11) 0.0257(9) -0.0167(8) 0.0022(7) 0.0047(8) F6S 0.0386(11) 0.0335(11) 0.0248(9) 0.0048(7) 0.0034(7) 0.0122(8) C2 0.0140(11) 0.0168(12) 0.0150(10) 0.0022(9) 0.0028(8) -0.0035(9) C1 0.0144(11) 0.0156(12) 0.0108(10) -0.0003(8) 0.0031(8) 0.0003(9) C11 0.0183(12) 0.0235(14) 0.0193(12) -0.0005(10) 0.0078(9) 0.0018(11) C12 0.0267(15) 0.0284(16) 0.0285(14) -0.0001(12) 0.0100(11) 0.0106(12) C13 0.0322(17) 0.0292(18) 0.0439(18) -0.0081(14) 0.0096(14) 0.0106(14) C14 0.0274(16) 0.052(2) 0.0377(18) -0.0220(16) 0.0105(13) 0.0046(15) C15 0.0265(15) 0.051(2) 0.0236(14) -0.0142(13) 0.0101(12) -0.0063(14) C16 0.0183(13) 0.0369(17) 0.0187(12) -0.0069(11) 0.0080(10) -0.0044(12) C22 0.0215(13) 0.0290(15) 0.0189(12) 0.0061(10) 0.0027(10) 0.0037(11) C21 0.0160(15) 0.017(2) 0.0129(19) -0.0025(14) 0.0023(12) -0.0019(17) C23 0.020(2) 0.029(2) 0.023(2) 0.0036(17) -0.0018(16) 0.0086(18) C24 0.026(2) 0.035(3) 0.020(2) 0.0012(17) -0.0050(17) -0.004(2) C25 0.018(3) 0.027(3) 0.026(3) -0.001(2) -0.0002(19) -0.009(2) C26 0.0178(18) 0.0171(19) 0.0198(17) 0.0014(13) 0.0006(13) -0.0036(15) C21A 0.0160(15) 0.017(2) 0.0129(19) -0.0025(14) 0.0023(12) -0.0019(17) C23A 0.021(4) 0.055(7) 0.013(4) 0.005(4) -0.005(3) 0.012(5) C24A 0.019(4) 0.042(6) 0.026(5) -0.008(4) -0.006(3) -0.001(4) C25A 0.006(4) 0.033(5) 0.033(6) -0.013(4) 0.004(4) -0.001(3) C26A 0.018(4) 0.028(5) 0.019(4) 0.001(3) 0.003(3) -0.002(3) C31 0.0185(12) 0.0166(13) 0.0214(12) 0.0042(9) 0.0054(9) -0.0021(10) C32 0.0225(14) 0.0178(14) 0.0290(14) -0.0024(10) -0.0015(11) -0.0007(11) C33 0.0308(17) 0.0196(16) 0.054(2) -0.0038(14) -0.0054(15) 0.0016(13) C34 0.0317(17) 0.0206(16) 0.0479(19) -0.0005(13) -0.0022(14) 0.0071(13) C35 0.0337(17) 0.0278(17) 0.0339(16) 0.0091(13) 0.0013(13) 0.0078(14) C36 0.0235(14) 0.0233(15) 0.0194(12) 0.0038(10) 0.0001(10) 0.0035(11) C41 0.0176(12) 0.0222(14) 0.0133(10) 0.0000(9) 0.0019(9) -0.0015(10) C42 0.0226(14) 0.0429(19) 0.0239(14) -0.0117(13) 0.0042(11) -0.0093(13) C43 0.0319(17) 0.047(2) 0.0289(15) -0.0182(14) 0.0018(13) -0.0090(15) C44 0.0386(19) 0.054(2) 0.0164(13) -0.0110(13) -0.0028(12) 0.0087(16) C45 0.0349(17) 0.0413(19) 0.0158(12) -0.0017(12) 0.0059(11) 0.0035(14) C46 0.0282(15) 0.0321(16) 0.0151(12) 0.0024(10) 0.0077(10) 0.0001(12) C51 0.0178(12) 0.0265(15) 0.0142(11) 0.0020(9) 0.0006(9) 0.0018(11) C52 0.0173(12) 0.0276(15) 0.0166(11) -0.0019(10) 0.0004(9) 0.0042(11) C53 0.0234(15) 0.0379(19) 0.0237(14) 0.0014(12) -0.0049(11) 0.0040(13) C54 0.0288(16) 0.054(2) 0.0204(14) -0.0020(14) -0.0024(11) -0.0002(15) C55 0.0264(16) 0.087(3) 0.0124(12) -0.0016(15) 0.0030(11) 0.0092(18) C56 0.0273(16) 0.057(2) 0.0177(13) -0.0031(13) 0.0048(11) 0.0093(15) C61 0.0135(11) 0.0155(12) 0.0143(10) 0.0010(8) 0.0031(8) -0.0009(9) C62 0.0172(12) 0.0175(13) 0.0155(11) 0.0012(9) 0.0042(9) -0.0022(10) C63 0.0210(13) 0.0226(14) 0.0191(12) -0.0012(10) 0.0039(10) -0.0075(11) C64 0.0297(16) 0.0189(14) 0.0275(14) -0.0007(11) -0.0010(11) -0.0067(12) C65 0.0238(14) 0.0157(14) 0.0321(15) -0.0033(11) -0.0018(11) 0.0024(11) C66 0.0175(12) 0.0150(13) 0.0216(12) 0.0014(9) 0.0003(9) 0.0008(10) C71 0.0142(11) 0.0149(12) 0.0147(10) -0.0009(8) 0.0029(8) -0.0001(9) C72 0.0155(12) 0.0229(14) 0.0218(12) -0.0027(10) 0.0056(9) -0.0030(10) C73 0.0177(13) 0.0289(16) 0.0305(14) -0.0035(12) 0.0069(11) -0.0077(12) C74 0.0201(14) 0.0291(16) 0.0308(15) -0.0045(12) -0.0006(11) -0.0074(12) C75 0.0284(15) 0.0315(17) 0.0194(12) -0.0054(11) 0.0014(11) -0.0084(13) C76 0.0233(14) 0.0246(15) 0.0172(12) -0.0013(10) 0.0036(10) -0.0052(11) C81 0.0157(12) 0.0138(12) 0.0218(12) 0.0002(9) 0.0062(9) 0.0019(9) C82 0.0217(13) 0.0149(13) 0.0282(13) -0.0026(10) 0.0066(10) -0.0010(10) C83 0.0314(16) 0.0161(14) 0.0439(18) -0.0088(12) 0.0118(13) -0.0013(12) C84 0.046(2) 0.0182(17) 0.060(2) -0.0012(15) 0.0106(18) 0.0125(15) C85 0.040(2) 0.0281(18) 0.052(2) -0.0002(15) 0.0017(16) 0.0174(15) C86 0.0258(15) 0.0239(15) 0.0304(15) 0.0016(11) 0.0016(11) 0.0095(12) O1S 0.055(2) 0.127(4) 0.086(3) 0.065(3) 0.0156(19) 0.033(2) C1S 0.048(3) 0.075(4) 0.134(6) -0.033(4) 0.003(3) 0.018(3) C4S 0.050(3) 0.128(5) 0.096(4) 0.068(4) 0.019(3) 0.014(3) C3S 0.086(4) 0.083(4) 0.065(3) 0.029(3) 0.017(3) 0.029(3) C2S 0.063(4) 0.139(6) 0.087(4) 0.043(4) 0.000(3) 0.056(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P2 2.3063(6) . ? Au1 P4 2.3091(6) . ? Au1 Rh1 2.9187(2) . ? Rh1 C3 1.807(3) . ? Rh1 C3A 1.821(17) . ? Rh1 P3 2.3351(7) . ? Rh1 P1 2.3425(6) . ? Rh1 Br1 2.5177(4) . ? Rh1 Br1A 2.548(4) . ? C3 O1 1.163(4) . ? C3A O1A 1.162(11) . ? P3 C2 1.845(3) . ? P3 C21 1.840(4) . ? P3 C11 1.853(3) . ? P3 C21A 1.920(10) . ? P4 C31 1.837(3) . ? P4 C2 1.840(3) . ? P4 C41 1.843(3) . ? P1 C1 1.843(3) . ? P1 C61 1.845(3) . ? P1 C51 1.864(3) . ? P2 C1 1.829(2) . ? P2 C81 1.843(3) . ? P2 C71 1.849(3) . ? P1S F1S 1.5985(19) . ? P1S F3S 1.6002(19) . ? P1S F6S 1.6027(19) . ? P1S F4S 1.6035(19) . ? P1S F2S 1.6063(18) . ? P1S F5S 1.6083(18) . ? C11 C16 1.533(4) . ? C11 C12 1.542(4) . ? C12 C13 1.528(4) . ? C13 C14 1.521(5) . ? C14 C15 1.518(5) . ? C15 C16 1.537(4) . ? C22 C23 1.506(5) . ? C22 C21 1.530(5) . ? C22 C21A 1.586(10) . ? C22 C23A 1.608(9) . ? C21 C26 1.531(6) . ? C23 C24 1.515(6) . ? C24 C25 1.535(6) . ? C25 C26 1.540(6) . ? C21A C26A 1.487(10) . ? C23A C24A 1.528(11) . ? C24A C25A 1.523(12) . ? C25A C26A 1.543(10) . ? C31 C32 1.539(4) . ? C31 C36 1.539(4) . ? C32 C33 1.531(4) . ? C33 C34 1.517(4) . ? C34 C35 1.517(5) . ? C35 C36 1.528(4) . ? C41 C42 1.531(4) . ? C41 C46 1.537(4) . ? C42 C43 1.531(4) . ? C43 C44 1.521(5) . ? C44 C45 1.520(5) . ? C45 C46 1.534(4) . ? C51 C56 1.517(4) . ? C51 C52 1.523(4) . ? C52 C53 1.522(4) . ? C53 C54 1.506(5) . ? C54 C55 1.530(5) . ? C55 C56 1.546(4) . ? C61 C62 1.538(3) . ? C61 C66 1.541(4) . ? C62 C63 1.531(4) . ? C63 C64 1.521(4) . ? C64 C65 1.527(4) . ? C65 C66 1.535(4) . ? C71 C76 1.536(3) . ? C71 C72 1.538(4) . ? C72 C73 1.539(4) . ? C73 C74 1.522(4) . ? C74 C75 1.533(4) . ? C75 C76 1.529(4) . ? C81 C82 1.539(4) . ? C81 C86 1.541(4) . ? C82 C83 1.532(4) . ? C83 C84 1.524(5) . ? C84 C85 1.522(5) . ? C85 C86 1.526(4) . ? O1S C3S 1.348(6) . ? O1S C2S 1.439(6) . ? C1S C2S 1.401(8) . ? C4S C3S 1.462(7) . ? 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 P2 Au1 P4 172.90(2) . . ? P2 Au1 Rh1 94.991(17) . . ? P4 Au1 Rh1 91.626(17) . . ? C3 Rh1 C3A 176.9(12) . . ? C3 Rh1 P3 90.86(9) . . ? C3A Rh1 P3 88.6(8) . . ? C3 Rh1 P1 91.69(9) . . ? C3A Rh1 P1 88.7(8) . . ? P3 Rh1 P1 175.94(2) . . ? C3 Rh1 Br1 171.53(10) . . ? C3A Rh1 Br1 11.5(12) . . ? P3 Rh1 Br1 88.882(19) . . ? P1 Rh1 Br1 89.062(18) . . ? C3 Rh1 Br1A 14.36(15) . . ? C3A Rh1 Br1A 168.6(12) . . ? P3 Rh1 Br1A 90.98(9) . . ? P1 Rh1 Br1A 92.28(9) . . ? Br1 Rh1 Br1A 157.17(12) . . ? C3 Rh1 Au1 92.29(10) . . ? C3A Rh1 Au1 90.7(12) . . ? P3 Rh1 Au1 93.042(18) . . ? P1 Rh1 Au1 90.012(17) . . ? Br1 Rh1 Au1 79.264(10) . . ? Br1A Rh1 Au1 77.95(12) . . ? O1 C3 Rh1 175.8(3) . . ? O1A C3A Rh1 178(3) . . ? C2 P3 C21 107.52(16) . . ? C2 P3 C11 106.44(12) . . ? C21 P3 C11 99.94(17) . . ? C2 P3 C21A 99.5(3) . . ? C21 P3 C21A 14.8(3) . . ? C11 P3 C21A 114.5(3) . . ? C2 P3 Rh1 111.00(8) . . ? C21 P3 Rh1 115.94(14) . . ? C11 P3 Rh1 115.02(9) . . ? C21A P3 Rh1 109.3(3) . . ? C31 P4 C2 104.28(12) . . ? C31 P4 C41 110.08(12) . . ? C2 P4 C41 105.49(12) . . ? C31 P4 Au1 110.12(9) . . ? C2 P4 Au1 112.12(8) . . ? C41 P4 Au1 114.22(9) . . ? C1 P1 C61 106.03(11) . . ? C1 P1 C51 104.14(11) . . ? C61 P1 C51 104.57(12) . . ? C1 P1 Rh1 112.42(8) . . ? C61 P1 Rh1 113.39(8) . . ? C51 P1 Rh1 115.34(9) . . ? C1 P2 C81 104.53(11) . . ? C1 P2 C71 105.97(11) . . ? C81 P2 C71 108.49(12) . . ? C1 P2 Au1 110.49(8) . . ? C81 P2 Au1 113.50(9) . . ? C71 P2 Au1 113.24(8) . . ? F1S P1S F3S 90.41(11) . . ? F1S P1S F6S 179.26(11) . . ? F3S P1S F6S 90.07(11) . . ? F1S P1S F4S 90.07(12) . . ? F3S P1S F4S 179.51(13) . . ? F6S P1S F4S 89.44(11) . . ? F1S P1S F2S 89.59(11) . . ? F3S P1S F2S 90.24(10) . . ? F6S P1S F2S 89.85(10) . . ? F4S P1S F2S 89.83(10) . . ? F1S P1S F5S 90.37(11) . . ? F3S P1S F5S 89.68(10) . . ? F6S P1S F5S 90.19(10) . . ? F4S P1S F5S 90.25(10) . . ? F2S P1S F5S 179.92(13) . . ? P4 C2 P3 115.13(13) . . ? P2 C1 P1 116.49(12) . . ? C16 C11 C12 109.7(2) . . ? C16 C11 P3 116.8(2) . . ? C12 C11 P3 111.74(18) . . ? C13 C12 C11 110.2(3) . . ? C14 C13 C12 111.0(3) . . ? C15 C14 C13 111.6(3) . . ? C14 C15 C16 112.2(3) . . ? C11 C16 C15 109.9(2) . . ? C23 C22 C21 114.0(3) . . ? C23 C22 C21A 114.4(4) . . ? C21 C22 C21A 18.0(3) . . ? C23 C22 C23A 30.9(4) . . ? C21 C22 C23A 111.2(4) . . ? C21A C22 C23A 102.0(6) . . ? C26 C21 C22 108.0(3) . . ? C26 C21 P3 114.8(3) . . ? C22 C21 P3 112.5(3) . . ? C22 C23 C24 108.5(4) . . ? C23 C24 C25 111.1(4) . . ? C24 C25 C26 111.1(4) . . ? C21 C26 C25 110.9(4) . . ? C26A C21A C22 113.4(7) . . ? C26A C21A P3 116.0(6) . . ? C22 C21A P3 106.0(5) . . ? C24A C23A C22 112.6(6) . . ? C25A C24A C23A 111.9(8) . . ? C24A C25A C26A 110.7(8) . . ? C25A C26A C21A 110.6(7) . . ? C32 C31 C36 109.2(2) . . ? C32 C31 P4 109.62(18) . . ? C36 C31 P4 110.99(19) . . ? C33 C32 C31 111.2(3) . . ? C34 C33 C32 111.9(3) . . ? C33 C34 C35 110.4(3) . . ? C34 C35 C36 111.0(3) . . ? C35 C36 C31 111.1(2) . . ? C42 C41 C46 111.9(2) . . ? C42 C41 P4 113.16(19) . . ? C46 C41 P4 114.27(19) . . ? C41 C42 C43 110.1(3) . . ? C44 C43 C42 111.0(3) . . ? C45 C44 C43 111.3(2) . . ? C44 C45 C46 111.5(3) . . ? C45 C46 C41 110.5(3) . . ? C56 C51 C52 111.4(2) . . ? C56 C51 P1 115.8(2) . . ? C52 C51 P1 111.62(18) . . ? C53 C52 C51 112.3(2) . . ? C54 C53 C52 112.6(3) . . ? C53 C54 C55 110.5(3) . . ? C54 C55 C56 111.4(3) . . ? C51 C56 C55 109.7(3) . . ? C62 C61 C66 109.5(2) . . ? C62 C61 P1 116.79(17) . . ? C66 C61 P1 111.26(17) . . ? C63 C62 C61 109.2(2) . . ? C64 C63 C62 111.8(2) . . ? C63 C64 C65 112.0(2) . . ? C64 C65 C66 111.7(2) . . ? C65 C66 C61 110.5(2) . . ? C76 C71 C72 110.9(2) . . ? C76 C71 P2 113.35(18) . . ? C72 C71 P2 114.79(17) . . ? C71 C72 C73 109.9(2) . . ? C74 C73 C72 111.8(2) . . ? C73 C74 C75 111.6(2) . . ? C76 C75 C74 111.6(2) . . ? C75 C76 C71 110.3(2) . . ? C82 C81 C86 109.5(2) . . ? C82 C81 P2 111.83(18) . . ? C86 C81 P2 109.87(18) . . ? C83 C82 C81 110.3(2) . . ? C84 C83 C82 111.2(3) . . ? C85 C84 C83 110.9(3) . . ? C84 C85 C86 111.6(3) . . ? C85 C86 C81 111.1(3) . . ? C3S O1S C2S 115.5(4) . . ? O1S C3S C4S 114.1(4) . . ? C1S C2S O1S 112.6(4) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.408 _refine_diff_density_min -0.967 _refine_diff_density_rms 0.113 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 789596' #TrackingRef '- CIF final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H46 Au Cl3 F3 O4 P4 Rh S' _chemical_formula_weight 1366.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.4553(11) _cell_length_b 19.2177(19) _cell_length_c 26.395(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5303.4(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9967 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 31.17 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.711 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2696 _exptl_absorpt_coefficient_mu 3.441 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3399 _exptl_absorpt_correction_T_max 0.3399 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 120893 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 31.00 _reflns_number_total 16512 _reflns_number_gt 15614 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0239P)^2^+1.5571P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.009(2) _refine_ls_number_reflns 16512 _refine_ls_number_parameters 631 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0287 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0591 _refine_ls_wR_factor_gt 0.0583 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1S S 1.50222(8) 0.37304(4) 0.16323(3) 0.02346(16) Uani 1 1 d . . . Rh1 Rh 1.23372(2) -0.089519(10) 0.063162(8) 0.01099(4) Uani 1 1 d . . . Au1 Au 1.084458(10) 0.018649(5) 0.116417(4) 0.01340(3) Uani 1 1 d . . . P1 P 1.16486(7) -0.04785(4) -0.01465(3) 0.01138(13) Uani 1 1 d . . . P2 P 1.01750(7) 0.06585(4) 0.04006(3) 0.01252(13) Uani 1 1 d . . . P3 P 1.31674(7) -0.12443(4) 0.14043(3) 0.01183(13) Uani 1 1 d . . . P4 P 1.17241(7) -0.00635(4) 0.19502(3) 0.01336(14) Uani 1 1 d . . . Cl1 Cl 1.36437(6) 0.01226(4) 0.07010(3) 0.01566(12) Uani 1 1 d . . . Cl1S Cl 1.59747(12) 0.04965(6) 0.22078(5) 0.0535(3) Uani 1 1 d . . . Cl2S Cl 1.77890(10) 0.11242(5) 0.15003(4) 0.0408(2) Uani 1 1 d . . . O1 O 1.1057(2) -0.22487(11) 0.04734(9) 0.0231(5) Uani 1 1 d . . . O1S O 1.3735(3) 0.3693(2) 0.14536(12) 0.0493(8) Uani 1 1 d . . . O2S O 1.5174(3) 0.36485(19) 0.21609(11) 0.0504(8) Uani 1 1 d . . . O3S O 1.5786(3) 0.42590(15) 0.14052(16) 0.0630(10) Uani 1 1 d . . . C1S C 1.5743(5) 0.2955(2) 0.13682(17) 0.0406(9) Uani 1 1 d . . . C1 C 1.1289(3) 0.04567(14) -0.01194(11) 0.0131(5) Uani 1 1 d . . . H1A H 1.0908 0.0606 -0.0445 0.016 Uiso 1 1 calc R . . H1B H 1.2093 0.0720 -0.0070 0.016 Uiso 1 1 calc R . . C2 C 1.3233(3) -0.05375(14) 0.18694(11) 0.0135(5) Uani 1 1 d . . . H2A H 1.3903 -0.0204 0.1764 0.016 Uiso 1 1 calc R . . H2B H 1.3490 -0.0734 0.2201 0.016 Uiso 1 1 calc R . . C2S C 1.6216(4) 0.0799(2) 0.15802(18) 0.0445(11) Uani 1 1 d . . . H2S1 H 1.6068 0.0413 0.1339 0.053 Uiso 1 1 calc R . . H2S2 H 1.5592 0.1172 0.1504 0.053 Uiso 1 1 calc R . . C3 C 1.1524(3) -0.17175(15) 0.05447(11) 0.0155(5) Uani 1 1 d . . . C11 C 1.2932(2) -0.05681(14) -0.06061(11) 0.0123(5) Uani 1 1 d . . . C12 C 1.3550(3) -0.12127(15) -0.06227(12) 0.0161(5) Uani 1 1 d . . . H12 H 1.3295 -0.1571 -0.0397 0.019 Uiso 1 1 calc R . . C13 C 1.4534(3) -0.13358(16) -0.09665(13) 0.0200(6) Uani 1 1 d . . . H13 H 1.4938 -0.1778 -0.0979 0.024 Uiso 1 1 calc R . . C14 C 1.4918(3) -0.08070(16) -0.12901(11) 0.0185(6) Uani 1 1 d . . . H14 H 1.5590 -0.0887 -0.1526 0.022 Uiso 1 1 calc R . . C15 C 1.4322(3) -0.01609(16) -0.12706(11) 0.0188(5) Uani 1 1 d . . . H15 H 1.4598 0.0201 -0.1490 0.023 Uiso 1 1 calc R . . C16 C 1.3324(3) -0.00402(15) -0.09323(11) 0.0155(5) Uani 1 1 d . . . H16 H 1.2912 0.0400 -0.0924 0.019 Uiso 1 1 calc R . . C21 C 1.0267(3) -0.08619(15) -0.04671(11) 0.0135(5) Uani 1 1 d . . . C22 C 1.0127(3) -0.07870(16) -0.09877(12) 0.0187(6) Uani 1 1 d . . . H22 H 1.0748 -0.0535 -0.1176 0.022 Uiso 1 1 calc R . . C23 C 0.9077(3) -0.10811(16) -0.12354(12) 0.0231(6) Uani 1 1 d . . . H23 H 0.8995 -0.1040 -0.1593 0.028 Uiso 1 1 calc R . . C24 C 0.8156(3) -0.14325(16) -0.09577(13) 0.0223(7) Uani 1 1 d . . . H24 H 0.7448 -0.1638 -0.1126 0.027 Uiso 1 1 calc R . . C25 C 0.8261(3) -0.14854(16) -0.04384(13) 0.0205(6) Uani 1 1 d . . . H25 H 0.7611 -0.1713 -0.0249 0.025 Uiso 1 1 calc R . . C26 C 0.9317(3) -0.12058(14) -0.01907(12) 0.0167(5) Uani 1 1 d . . . H26 H 0.9393 -0.1249 0.0167 0.020 Uiso 1 1 calc R . . C31 C 1.0182(3) 0.16032(15) 0.04292(12) 0.0174(6) Uani 1 1 d . . . C32 C 1.1335(3) 0.19391(17) 0.05588(14) 0.0231(7) Uani 1 1 d . . . H32 H 1.2089 0.1673 0.0612 0.028 Uiso 1 1 calc R . . C33 C 1.1375(4) 0.26581(18) 0.06098(15) 0.0305(8) Uani 1 1 d . . . H33 H 1.2154 0.2884 0.0694 0.037 Uiso 1 1 calc R . . C34 C 1.0266(4) 0.30453(18) 0.05360(16) 0.0343(9) Uani 1 1 d . . . H34 H 1.0292 0.3537 0.0569 0.041 Uiso 1 1 calc R . . C35 C 0.9118(4) 0.27189(17) 0.04143(14) 0.0315(7) Uani 1 1 d . . . H35 H 0.8365 0.2988 0.0366 0.038 Uiso 1 1 calc R . . C36 C 0.9072(3) 0.19959(15) 0.03636(12) 0.0217(6) Uani 1 1 d . . . H36 H 0.8287 0.1772 0.0285 0.026 Uiso 1 1 calc R . . C41 C 0.8622(3) 0.03826(14) 0.01831(11) 0.0136(5) Uani 1 1 d . . . C42 C 0.7861(3) -0.00222(14) 0.05026(11) 0.0152(6) Uani 1 1 d . . . H42 H 0.8157 -0.0134 0.0833 0.018 Uiso 1 1 calc R . . C43 C 0.6681(3) -0.02627(16) 0.03429(12) 0.0185(6) Uani 1 1 d . . . H43 H 0.6162 -0.0534 0.0562 0.022 Uiso 1 1 calc R . . C44 C 0.6262(3) -0.01003(17) -0.01461(12) 0.0208(6) Uani 1 1 d . . . H44 H 0.5448 -0.0258 -0.0257 0.025 Uiso 1 1 calc R . . C45 C 0.7021(3) 0.02892(15) -0.04711(12) 0.0185(6) Uani 1 1 d . . . H45 H 0.6734 0.0389 -0.0805 0.022 Uiso 1 1 calc R . . C46 C 0.8207(3) 0.05332(15) -0.03069(12) 0.0170(6) Uani 1 1 d . . . H46 H 0.8730 0.0801 -0.0528 0.020 Uiso 1 1 calc R . . C51 C 1.4825(3) -0.15210(14) 0.13280(11) 0.0126(5) Uani 1 1 d . . . C52 C 1.5088(3) -0.19807(16) 0.09329(12) 0.0183(6) Uani 1 1 d . . . H52 H 1.4409 -0.2152 0.0729 0.022 Uiso 1 1 calc R . . C53 C 1.6336(3) -0.21900(17) 0.08355(13) 0.0211(6) Uani 1 1 d . . . H53 H 1.6504 -0.2513 0.0571 0.025 Uiso 1 1 calc R . . C54 C 1.7341(3) -0.19281(15) 0.11232(13) 0.0212(6) Uani 1 1 d . . . H54 H 1.8195 -0.2066 0.1053 0.025 Uiso 1 1 calc R . . C55 C 1.7089(3) -0.14675(16) 0.15111(13) 0.0206(6) Uani 1 1 d . . . H55 H 1.7778 -0.1287 0.1706 0.025 Uiso 1 1 calc R . . C56 C 1.5840(3) -0.12630(15) 0.16221(11) 0.0179(5) Uani 1 1 d . . . H56 H 1.5677 -0.0952 0.1894 0.022 Uiso 1 1 calc R . . C61 C 1.2361(3) -0.19455(14) 0.17343(10) 0.0132(5) Uani 1 1 d . . . C62 C 1.3024(3) -0.23990(16) 0.20545(12) 0.0202(6) Uani 1 1 d . . . H62 H 1.3927 -0.2362 0.2086 0.024 Uiso 1 1 calc R . . C63 C 1.2363(4) -0.29046(17) 0.23270(13) 0.0278(7) Uani 1 1 d . . . H63 H 1.2817 -0.3214 0.2542 0.033 Uiso 1 1 calc R . . C64 C 1.1039(4) -0.29576(17) 0.22847(13) 0.0264(7) Uani 1 1 d . . . H64 H 1.0593 -0.3302 0.2472 0.032 Uiso 1 1 calc R . . C65 C 1.0369(3) -0.25111(17) 0.19709(13) 0.0239(7) Uani 1 1 d . . . H65 H 0.9466 -0.2550 0.1942 0.029 Uiso 1 1 calc R . . C66 C 1.1025(3) -0.20030(15) 0.16962(11) 0.0181(6) Uani 1 1 d . . . H66 H 1.0565 -0.1694 0.1482 0.022 Uiso 1 1 calc R . . C71 C 1.0749(3) -0.05382(15) 0.23992(10) 0.0167(5) Uani 1 1 d . . . C72 C 1.1238(3) -0.10493(16) 0.27269(12) 0.0206(6) Uani 1 1 d . . . H72 H 1.2130 -0.1143 0.2731 0.025 Uiso 1 1 calc R . . C73 C 1.0425(3) -0.14168(16) 0.30434(13) 0.0240(7) Uani 1 1 d . . . H73 H 1.0759 -0.1771 0.3257 0.029 Uiso 1 1 calc R . . C74 C 0.9128(4) -0.12709(17) 0.30505(12) 0.0277(7) Uani 1 1 d . . . H74 H 0.8578 -0.1520 0.3272 0.033 Uiso 1 1 calc R . . C75 C 0.8632(3) -0.0764(2) 0.27362(14) 0.0301(8) Uani 1 1 d . . . H75 H 0.7741 -0.0666 0.2742 0.036 Uiso 1 1 calc R . . C76 C 0.9435(3) -0.03938(18) 0.24088(12) 0.0225(7) Uani 1 1 d . . . H76 H 0.9090 -0.0045 0.2193 0.027 Uiso 1 1 calc R . . C81 C 1.2233(3) 0.07462(14) 0.22465(11) 0.0148(5) Uani 1 1 d . . . C82 C 1.2605(3) 0.07720(16) 0.27489(12) 0.0210(6) Uani 1 1 d . . . H82 H 1.2570 0.0365 0.2953 0.025 Uiso 1 1 calc R . . C83 C 1.3035(3) 0.14046(18) 0.29556(14) 0.0277(7) Uani 1 1 d . . . H83 H 1.3283 0.1427 0.3301 0.033 Uiso 1 1 calc R . . C84 C 1.3098(3) 0.19939(17) 0.26570(15) 0.0273(8) Uani 1 1 d . . . H84 H 1.3397 0.2418 0.2799 0.033 Uiso 1 1 calc R . . C85 C 1.2731(4) 0.19721(17) 0.21544(15) 0.0315(8) Uani 1 1 d . . . H85 H 1.2781 0.2377 0.1949 0.038 Uiso 1 1 calc R . . C86 C 1.2285(4) 0.13440(17) 0.19519(14) 0.0280(7) Uani 1 1 d . . . H86 H 1.2015 0.1327 0.1609 0.034 Uiso 1 1 calc R . . F1S F 1.6965(3) 0.28877(16) 0.14978(13) 0.0629(8) Uani 1 1 d . . . F2S F 1.5169(4) 0.23891(16) 0.1514(2) 0.1141(18) Uani 1 1 d . . . F3S F 1.5714(4) 0.2965(2) 0.08569(12) 0.0888(12) Uani 1 1 d . . . 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 S1S 0.0216(4) 0.0271(4) 0.0217(4) 0.0066(3) 0.0014(3) -0.0001(3) Rh1 0.01323(9) 0.01079(9) 0.00894(9) -0.00002(7) 0.00023(8) 0.00017(7) Au1 0.01259(4) 0.01615(4) 0.01147(5) -0.00136(4) 0.00002(4) 0.00150(4) P1 0.0118(3) 0.0124(3) 0.0100(3) 0.0001(2) 0.0005(3) -0.0002(2) P2 0.0117(3) 0.0127(3) 0.0132(3) -0.0004(2) -0.0003(3) 0.0006(2) P3 0.0132(3) 0.0118(3) 0.0104(3) -0.0003(2) 0.0002(3) 0.0001(2) P4 0.0141(3) 0.0148(3) 0.0112(3) -0.0018(2) 0.0008(3) 0.0006(2) Cl1 0.0129(3) 0.0171(3) 0.0170(3) 0.0012(3) 0.0003(2) -0.0025(2) Cl1S 0.0535(7) 0.0535(6) 0.0534(7) -0.0243(5) 0.0121(6) -0.0300(6) Cl2S 0.0410(5) 0.0422(5) 0.0391(5) -0.0204(4) 0.0117(4) -0.0085(4) O1 0.0343(14) 0.0134(10) 0.0216(12) 0.0006(8) -0.0039(10) -0.0027(9) O1S 0.0253(14) 0.088(2) 0.0347(17) -0.0049(17) -0.0023(12) 0.0113(15) O2S 0.059(2) 0.072(2) 0.0198(15) -0.0016(14) -0.0035(14) 0.0172(18) O3S 0.0513(19) 0.0324(15) 0.105(3) 0.0236(17) 0.037(2) 0.0029(15) C1S 0.039(2) 0.035(2) 0.048(2) -0.0027(17) 0.010(2) -0.0011(18) C1 0.0129(12) 0.0121(12) 0.0144(14) 0.0012(10) 0.0016(10) -0.0002(9) C2 0.0164(13) 0.0158(13) 0.0084(13) -0.0016(9) -0.0009(10) 0.0004(10) C2S 0.032(2) 0.049(3) 0.053(3) -0.009(2) -0.0079(19) -0.0009(17) C3 0.0205(14) 0.0161(13) 0.0098(14) 0.0021(10) -0.0029(11) 0.0023(11) C11 0.0113(12) 0.0161(12) 0.0094(12) -0.0007(10) -0.0015(10) -0.0003(9) C12 0.0170(13) 0.0149(13) 0.0164(14) 0.0022(11) 0.0018(11) -0.0022(10) C13 0.0201(14) 0.0161(13) 0.0237(16) -0.0030(11) 0.0000(12) 0.0031(11) C14 0.0163(13) 0.0242(15) 0.0148(15) -0.0002(11) 0.0021(11) 0.0020(11) C15 0.0181(13) 0.0226(13) 0.0158(14) 0.0062(11) 0.0028(10) -0.0001(12) C16 0.0162(13) 0.0165(13) 0.0138(14) 0.0048(9) 0.0003(11) 0.0012(10) C21 0.0116(12) 0.0143(12) 0.0147(14) -0.0020(10) 0.0001(10) 0.0009(10) C22 0.0192(14) 0.0206(14) 0.0164(14) 0.0013(11) -0.0009(11) -0.0016(11) C23 0.0218(14) 0.0275(15) 0.0200(16) -0.0050(11) -0.0054(14) 0.0004(12) C24 0.0166(14) 0.0188(14) 0.0314(18) -0.0083(12) -0.0054(13) 0.0007(11) C25 0.0139(13) 0.0170(14) 0.0307(18) -0.0051(12) 0.0038(12) -0.0011(10) C26 0.0187(14) 0.0127(12) 0.0186(14) -0.0011(10) 0.0012(12) 0.0014(10) C31 0.0210(15) 0.0153(13) 0.0159(14) -0.0013(10) 0.0024(11) -0.0015(11) C32 0.0197(15) 0.0211(15) 0.0284(18) -0.0042(13) 0.0019(13) -0.0037(12) C33 0.0308(18) 0.0244(17) 0.036(2) -0.0084(15) 0.0048(16) -0.0119(14) C34 0.044(2) 0.0134(15) 0.045(2) -0.0040(14) 0.0071(18) -0.0028(14) C35 0.0359(19) 0.0200(15) 0.039(2) -0.0033(13) 0.0005(18) 0.0044(15) C36 0.0222(15) 0.0172(13) 0.0258(16) -0.0008(11) -0.0003(14) 0.0010(12) C41 0.0120(12) 0.0133(12) 0.0154(14) 0.0000(9) 0.0005(10) 0.0014(9) C42 0.0170(13) 0.0147(13) 0.0139(14) -0.0004(9) -0.0006(10) 0.0018(9) C43 0.0149(12) 0.0194(14) 0.0214(15) -0.0025(11) 0.0049(11) -0.0001(11) C44 0.0145(12) 0.0221(15) 0.0259(16) -0.0049(12) -0.0003(11) 0.0001(11) C45 0.0168(13) 0.0219(15) 0.0167(14) -0.0037(11) -0.0042(11) 0.0033(11) C46 0.0161(13) 0.0146(13) 0.0203(15) -0.0010(11) 0.0008(11) 0.0031(10) C51 0.0147(12) 0.0118(12) 0.0112(13) 0.0014(9) 0.0005(10) 0.0006(10) C52 0.0197(14) 0.0187(14) 0.0163(15) -0.0023(11) -0.0001(12) 0.0001(11) C53 0.0215(15) 0.0213(15) 0.0205(16) -0.0050(12) 0.0025(12) 0.0034(12) C54 0.0195(13) 0.0236(14) 0.0206(15) 0.0021(12) 0.0021(13) 0.0053(11) C55 0.0179(14) 0.0220(15) 0.0220(16) -0.0005(12) -0.0048(12) 0.0006(11) C56 0.0181(13) 0.0211(13) 0.0146(14) -0.0024(10) -0.0037(12) 0.0021(12) C61 0.0183(13) 0.0120(11) 0.0094(12) -0.0013(9) 0.0017(11) -0.0019(10) C62 0.0251(16) 0.0195(14) 0.0160(15) 0.0033(11) 0.0013(12) 0.0015(11) C63 0.041(2) 0.0188(15) 0.0238(17) 0.0075(12) 0.0049(15) 0.0031(14) C64 0.041(2) 0.0185(14) 0.0192(16) -0.0001(11) 0.0088(15) -0.0104(14) C65 0.0260(16) 0.0268(16) 0.0188(16) -0.0045(12) 0.0052(13) -0.0107(12) C66 0.0215(15) 0.0194(13) 0.0134(14) -0.0008(10) 0.0009(12) -0.0046(11) C71 0.0194(14) 0.0183(13) 0.0124(13) -0.0036(10) 0.0017(11) -0.0028(12) C72 0.0249(15) 0.0177(14) 0.0191(15) -0.0027(11) 0.0071(12) -0.0008(11) C73 0.0383(19) 0.0161(14) 0.0174(16) -0.0020(11) 0.0061(13) -0.0051(12) C74 0.0342(17) 0.0300(16) 0.0189(16) -0.0043(12) 0.0064(15) -0.0178(16) C75 0.0183(15) 0.044(2) 0.0279(19) -0.0049(15) 0.0029(14) -0.0087(14) C76 0.0207(16) 0.0296(16) 0.0171(16) -0.0014(11) -0.0005(12) -0.0039(12) C81 0.0192(13) 0.0135(12) 0.0117(13) -0.0041(9) -0.0006(11) 0.0031(10) C82 0.0292(16) 0.0181(14) 0.0156(14) 0.0005(10) 0.0003(13) -0.0032(12) C83 0.0327(18) 0.0275(17) 0.0230(18) -0.0089(13) -0.0040(14) -0.0019(13) C84 0.0242(16) 0.0177(15) 0.040(2) -0.0132(14) 0.0009(15) -0.0008(12) C85 0.045(2) 0.0144(14) 0.035(2) -0.0004(13) -0.0030(17) -0.0013(14) C86 0.041(2) 0.0190(15) 0.0240(17) -0.0003(12) -0.0063(15) -0.0016(14) F1S 0.0475(17) 0.0621(18) 0.079(2) -0.0074(16) -0.0056(15) 0.0284(14) F2S 0.108(3) 0.0310(16) 0.203(5) -0.020(2) 0.074(3) -0.0153(18) F3S 0.082(3) 0.137(3) 0.0469(19) -0.040(2) 0.0004(18) 0.034(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1S O2S 1.413(3) . ? S1S O3S 1.424(3) . ? S1S O1S 1.428(3) . ? S1S C1S 1.809(4) . ? Rh1 C3 1.809(3) . ? Rh1 P3 2.3158(8) . ? Rh1 P1 2.3190(8) . ? Rh1 Cl1 2.3928(7) . ? Rh1 Au1 2.9551(3) . ? Au1 P2 2.3185(8) . ? Au1 P4 2.3198(8) . ? P1 C11 1.817(3) . ? P1 C21 1.829(3) . ? P1 C1 1.837(3) . ? P2 C41 1.802(3) . ? P2 C31 1.817(3) . ? P2 C1 1.841(3) . ? P3 C61 1.813(3) . ? P3 C51 1.824(3) . ? P3 C2 1.832(3) . ? P4 C71 1.810(3) . ? P4 C81 1.821(3) . ? P4 C2 1.834(3) . ? Cl1S C2S 1.774(5) . ? Cl2S C2S 1.771(4) . ? O1 C3 1.147(4) . ? C1S F2S 1.301(5) . ? C1S F1S 1.329(5) . ? C1S F3S 1.350(5) . ? C11 C16 1.392(4) . ? C11 C12 1.398(4) . ? C12 C13 1.392(4) . ? C13 C14 1.387(4) . ? C14 C15 1.390(4) . ? C15 C16 1.393(4) . ? C21 C22 1.389(4) . ? C21 C26 1.398(4) . ? C22 C23 1.397(4) . ? C23 C24 1.386(5) . ? C24 C25 1.379(5) . ? C25 C26 1.391(4) . ? C31 C36 1.395(4) . ? C31 C32 1.410(4) . ? C32 C33 1.389(5) . ? C33 C34 1.391(6) . ? C34 C35 1.392(6) . ? C35 C36 1.397(4) . ? C41 C46 1.394(4) . ? C41 C42 1.396(4) . ? C42 C43 1.384(4) . ? C43 C44 1.398(4) . ? C44 C45 1.388(4) . ? C45 C46 1.395(4) . ? C51 C52 1.394(4) . ? C51 C56 1.405(4) . ? C52 C53 1.390(4) . ? C53 C54 1.390(5) . ? C54 C55 1.379(4) . ? C55 C56 1.395(4) . ? C61 C62 1.398(4) . ? C61 C66 1.404(4) . ? C62 C63 1.392(4) . ? C63 C64 1.393(5) . ? C64 C65 1.383(5) . ? C65 C66 1.396(4) . ? C71 C76 1.402(4) . ? C71 C72 1.405(4) . ? C72 C73 1.385(4) . ? C73 C74 1.385(5) . ? C74 C75 1.381(5) . ? C75 C76 1.399(5) . ? C81 C82 1.383(4) . ? C81 C86 1.388(4) . ? C82 C83 1.407(4) . ? C83 C84 1.381(5) . ? C84 C85 1.382(5) . ? C85 C86 1.400(5) . ? 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 O2S S1S O3S 115.6(2) . . ? O2S S1S O1S 115.2(2) . . ? O3S S1S O1S 115.2(2) . . ? O2S S1S C1S 104.0(2) . . ? O3S S1S C1S 101.0(2) . . ? O1S S1S C1S 102.9(2) . . ? C3 Rh1 P3 91.99(9) . . ? C3 Rh1 P1 92.49(9) . . ? P3 Rh1 P1 175.12(3) . . ? C3 Rh1 Cl1 172.78(10) . . ? P3 Rh1 Cl1 87.45(3) . . ? P1 Rh1 Cl1 87.87(3) . . ? C3 Rh1 Au1 115.25(10) . . ? P3 Rh1 Au1 89.02(2) . . ? P1 Rh1 Au1 90.83(2) . . ? Cl1 Rh1 Au1 71.942(18) . . ? P2 Au1 P4 168.03(2) . . ? P2 Au1 Rh1 91.213(19) . . ? P4 Au1 Rh1 94.037(19) . . ? C11 P1 C21 103.68(13) . . ? C11 P1 C1 105.65(13) . . ? C21 P1 C1 104.50(13) . . ? C11 P1 Rh1 109.22(9) . . ? C21 P1 Rh1 121.05(10) . . ? C1 P1 Rh1 111.51(10) . . ? C41 P2 C31 108.11(14) . . ? C41 P2 C1 105.70(13) . . ? C31 P2 C1 103.81(13) . . ? C41 P2 Au1 115.72(10) . . ? C31 P2 Au1 110.71(11) . . ? C1 P2 Au1 111.99(10) . . ? C61 P3 C51 106.17(13) . . ? C61 P3 C2 104.27(13) . . ? C51 P3 C2 104.75(13) . . ? C61 P3 Rh1 117.66(10) . . ? C51 P3 Rh1 110.08(9) . . ? C2 P3 Rh1 112.91(9) . . ? C71 P4 C81 108.30(13) . . ? C71 P4 C2 108.08(14) . . ? C81 P4 C2 102.90(13) . . ? C71 P4 Au1 117.83(10) . . ? C81 P4 Au1 108.84(10) . . ? C2 P4 Au1 109.86(9) . . ? F2S C1S F1S 106.6(4) . . ? F2S C1S F3S 107.3(4) . . ? F1S C1S F3S 106.3(4) . . ? F2S C1S S1S 112.5(3) . . ? F1S C1S S1S 112.4(3) . . ? F3S C1S S1S 111.4(3) . . ? P1 C1 P2 111.37(15) . . ? P3 C2 P4 114.46(15) . . ? Cl2S C2S Cl1S 111.0(2) . . ? O1 C3 Rh1 176.6(3) . . ? C16 C11 C12 119.4(3) . . ? C16 C11 P1 124.1(2) . . ? C12 C11 P1 116.5(2) . . ? C13 C12 C11 120.8(3) . . ? C14 C13 C12 119.4(3) . . ? C13 C14 C15 120.1(3) . . ? C14 C15 C16 120.6(3) . . ? C11 C16 C15 119.7(3) . . ? C22 C21 C26 119.4(3) . . ? C22 C21 P1 119.9(2) . . ? C26 C21 P1 120.7(2) . . ? C21 C22 C23 120.2(3) . . ? C24 C23 C22 119.7(3) . . ? C25 C24 C23 120.4(3) . . ? C24 C25 C26 120.1(3) . . ? C25 C26 C21 120.1(3) . . ? C36 C31 C32 119.6(3) . . ? C36 C31 P2 122.1(2) . . ? C32 C31 P2 118.1(2) . . ? C33 C32 C31 120.3(3) . . ? C32 C33 C34 119.6(3) . . ? C33 C34 C35 120.6(3) . . ? C34 C35 C36 120.0(4) . . ? C31 C36 C35 119.9(3) . . ? C46 C41 C42 119.9(3) . . ? C46 C41 P2 121.0(2) . . ? C42 C41 P2 119.0(2) . . ? C43 C42 C41 120.7(3) . . ? C42 C43 C44 119.1(3) . . ? C45 C44 C43 120.8(3) . . ? C44 C45 C46 119.8(3) . . ? C41 C46 C45 119.7(3) . . ? C52 C51 C56 119.2(3) . . ? C52 C51 P3 117.0(2) . . ? C56 C51 P3 123.6(2) . . ? C53 C52 C51 120.4(3) . . ? C52 C53 C54 120.2(3) . . ? C55 C54 C53 119.6(3) . . ? C54 C55 C56 121.0(3) . . ? C55 C56 C51 119.5(3) . . ? C62 C61 C66 119.2(3) . . ? C62 C61 P3 121.5(2) . . ? C66 C61 P3 119.1(2) . . ? C63 C62 C61 120.1(3) . . ? C62 C63 C64 120.2(3) . . ? C65 C64 C63 120.4(3) . . ? C64 C65 C66 119.8(3) . . ? C65 C66 C61 120.4(3) . . ? C76 C71 C72 118.9(3) . . ? C76 C71 P4 117.6(2) . . ? C72 C71 P4 123.4(2) . . ? C73 C72 C71 120.3(3) . . ? C74 C73 C72 120.4(3) . . ? C75 C74 C73 120.2(3) . . ? C74 C75 C76 120.3(3) . . ? C75 C76 C71 119.9(3) . . ? C82 C81 C86 119.8(3) . . ? C82 C81 P4 121.6(2) . . ? C86 C81 P4 118.6(2) . . ? C81 C82 C83 119.5(3) . . ? C84 C83 C82 120.2(3) . . ? C83 C84 C85 120.6(3) . . ? C84 C85 C86 119.0(3) . . ? C81 C86 C85 120.8(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.998 _refine_diff_density_min -0.798 _refine_diff_density_rms 0.116 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 789597' #TrackingRef '- CIF final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H48 Au Br Cl4 F3 O4 P4 Rh S' _chemical_formula_weight 1495.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.5635(17) _cell_length_b 10.8423(10) _cell_length_c 28.356(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.659(2) _cell_angle_gamma 90.00 _cell_volume 5910.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9450 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 30.77 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.680 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2936 _exptl_absorpt_coefficient_mu 3.811 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3109 _exptl_absorpt_correction_T_max 0.3944 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 122157 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 30.51 _reflns_number_total 17969 _reflns_number_gt 15054 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0823P)^2^+57.7070P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17969 _refine_ls_number_parameters 760 _refine_ls_number_restraints 796 _refine_ls_R_factor_all 0.0698 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1681 _refine_ls_wR_factor_gt 0.1599 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 1.21837(3) -0.33669(5) 0.22621(2) 0.02061(12) Uani 1 1 d . . . Rh1 Rh 1.32010(2) -0.20273(4) 0.215925(14) 0.01457(9) Uani 1 1 d . . . Au1 Au 1.190426(11) -0.06196(2) 0.184461(7) 0.01832(7) Uani 1 1 d . . . P1 P 1.32509(7) -0.13705(13) 0.29415(5) 0.0143(2) Uani 1 1 d . . . P2 P 1.18915(8) 0.00436(14) 0.26211(5) 0.0186(3) Uani 1 1 d . C . P3 P 1.31066(7) -0.28331(14) 0.13938(5) 0.0166(3) Uani 1 1 d . . . P4 P 1.17422(7) -0.14111(14) 0.10718(5) 0.0177(3) Uani 1 1 d . E . O1 O 1.4531(2) -0.0776(5) 0.21024(17) 0.0308(10) Uani 1 1 d . . . C1 C 1.2389(3) -0.0980(6) 0.3075(2) 0.0193(10) Uani 1 1 d . . . H1A H 1.2122 -0.1749 0.3092 0.023 Uiso 1 1 calc R . . H1B H 1.2450 -0.0573 0.3392 0.023 Uiso 1 1 calc R . . C4S C 0.9225(13) 0.445(5) 0.6182(12) 0.17(3) Uani 0.461(5) 1 d PDU A 1 H4S1 H 0.9270 0.5342 0.6111 0.201 Uiso 0.461(5) 1 calc PR A 1 H4S2 H 0.8990 0.4067 0.5880 0.201 Uiso 0.461(5) 1 calc PR A 1 Cl5S Cl 0.8635(4) 0.4373(7) 0.6573(3) 0.078(2) Uani 0.461(5) 1 d PDU A 1 Cl6S Cl 1.0070(3) 0.3870(6) 0.6292(3) 0.072(2) Uani 0.461(5) 1 d PDU A 1 C1S C 1.0595(7) 0.105(2) 0.5926(6) 0.067(6) Uani 0.539(5) 1 d PDU A 2 H1S1 H 1.0371 0.1824 0.5796 0.080 Uiso 0.539(5) 1 calc PR A 2 H1S2 H 1.0269 0.0572 0.6085 0.080 Uiso 0.539(5) 1 calc PR A 2 Cl1S Cl 1.0886(3) 0.0165(5) 0.54753(17) 0.0645(15) Uani 0.539(5) 1 d PDU A 2 Cl2S Cl 1.13726(17) 0.1309(4) 0.63055(19) 0.0640(16) Uani 0.539(5) 1 d PDU A 2 C2 C 1.2212(3) -0.2878(6) 0.1060(2) 0.0224(11) Uani 1 1 d . . . H2A H 1.1955 -0.3535 0.1196 0.027 Uiso 1 1 calc R . . H2B H 1.2220 -0.3098 0.0722 0.027 Uiso 1 1 calc R . . C3 C 1.4003(3) -0.1244(6) 0.2118(2) 0.0219(11) Uani 1 1 d . . . C11 C 1.3792(3) -0.0041(5) 0.3160(2) 0.0176(10) Uani 1 1 d . . . C12 C 1.4114(3) 0.0047(6) 0.3643(2) 0.0224(11) Uani 1 1 d . . . H12 H 1.4064 -0.0601 0.3860 0.027 Uiso 1 1 calc R . . C13 C 1.4506(3) 0.1083(6) 0.3804(2) 0.0271(12) Uani 1 1 d . . . H13 H 1.4737 0.1127 0.4129 0.032 Uiso 1 1 calc R . . C14 C 1.4566(3) 0.2052(6) 0.3496(3) 0.0288(13) Uani 1 1 d . . . H14 H 1.4825 0.2767 0.3611 0.035 Uiso 1 1 calc R . . C15 C 1.4241(4) 0.1971(6) 0.3015(3) 0.0296(13) Uani 1 1 d . . . H15 H 1.4279 0.2632 0.2801 0.036 Uiso 1 1 calc R . . C16 C 1.3862(3) 0.0920(6) 0.2849(2) 0.0228(11) Uani 1 1 d . . . H16 H 1.3650 0.0860 0.2520 0.027 Uiso 1 1 calc R . . C21 C 1.3572(3) -0.2614(5) 0.3356(2) 0.0169(10) Uani 1 1 d . . . C22 C 1.3300(3) -0.2895(6) 0.3763(2) 0.0233(11) Uani 1 1 d . . . H22 H 1.2923 -0.2429 0.3838 0.028 Uiso 1 1 calc R . . C23 C 1.3582(4) -0.3863(7) 0.4062(2) 0.0293(13) Uani 1 1 d . . . H23 H 1.3390 -0.4065 0.4336 0.035 Uiso 1 1 calc R . . C24 C 1.4141(4) -0.4529(6) 0.3959(2) 0.0283(13) Uani 1 1 d . . . H24 H 1.4337 -0.5175 0.4168 0.034 Uiso 1 1 calc R . . C25 C 1.4414(4) -0.4260(6) 0.3556(3) 0.0287(13) Uani 1 1 d . . . H25 H 1.4796 -0.4719 0.3486 0.034 Uiso 1 1 calc R . . C26 C 1.4124(3) -0.3305(6) 0.3250(2) 0.0221(11) Uani 1 1 d . . . H26 H 1.4305 -0.3129 0.2968 0.026 Uiso 1 1 calc R . . C31 C 1.2214(3) 0.1581(6) 0.2769(2) 0.0247(12) Uani 1 1 d . . . C32 C 1.2356(4) 0.2004(7) 0.3243(3) 0.0335(15) Uani 1 1 d . . . H32 H 1.2266 0.1488 0.3495 0.040 Uiso 1 1 calc R . . C33 C 1.2627(5) 0.3174(7) 0.3345(3) 0.045(2) Uani 1 1 d . . . H33 H 1.2720 0.3459 0.3667 0.054 Uiso 1 1 calc R . . C34 C 1.2767(5) 0.3942(7) 0.2975(3) 0.043(2) Uani 1 1 d . . . H34 H 1.2956 0.4741 0.3047 0.052 Uiso 1 1 calc R . . C35 C 1.2627(5) 0.3529(7) 0.2505(3) 0.0390(17) Uani 1 1 d . . . H35 H 1.2725 0.4044 0.2255 0.047 Uiso 1 1 calc R . . C36 C 1.2343(4) 0.2358(6) 0.2398(3) 0.0298(14) Uani 1 1 d . . . H36 H 1.2236 0.2086 0.2074 0.036 Uiso 1 1 calc R . . C41 C 1.1010(3) 0.0000(6) 0.2736(2) 0.0278(12) Uani 1 1 d DU . . C44 C 0.9620(4) -0.0056(9) 0.2829(4) 0.061(2) Uani 1 1 d DU . . H44 H 0.9139 -0.0087 0.2843 0.073 Uiso 1 1 calc R B 1 C42 C 1.0635(5) 0.1099(9) 0.2733(5) 0.054(3) Uani 0.833(11) 1 d PDU C 1 H42 H 1.0857 0.1871 0.2713 0.065 Uiso 0.833(11) 1 calc PR C 1 C43 C 0.9939(5) 0.1048(10) 0.2760(6) 0.070(4) Uani 0.833(11) 1 d PDU C 1 H43 H 0.9674 0.1788 0.2731 0.085 Uiso 0.833(11) 1 calc PR C 1 C45 C 1.0015(5) -0.1104(11) 0.2876(6) 0.059(3) Uani 0.833(11) 1 d PDU C 1 H45 H 0.9816 -0.1858 0.2955 0.071 Uiso 0.833(11) 1 calc PR C 1 C46 C 1.0694(4) -0.1087(9) 0.2812(5) 0.052(3) Uani 0.833(11) 1 d PDU C 1 H46 H 1.0946 -0.1838 0.2820 0.062 Uiso 0.833(11) 1 calc PR C 1 C42A C 1.0481(9) 0.029(6) 0.2350(10) 0.054(8) Uani 0.167(11) 1 d PDU C 2 H42A H 1.0595 0.0621 0.2066 0.064 Uiso 0.167(11) 1 calc PR C 2 C43A C 0.9790(10) 0.008(7) 0.2378(7) 0.065(8) Uani 0.167(11) 1 d PDU C 2 H43A H 0.9442 0.0044 0.2096 0.078 Uiso 0.167(11) 1 calc PR C 2 C45A C 1.0124(10) -0.056(6) 0.3188(12) 0.053(8) Uani 0.167(11) 1 d PDU C 2 H45A H 1.0004 -0.0848 0.3477 0.064 Uiso 0.167(11) 1 calc PR C 2 C46A C 1.0805(11) -0.062(5) 0.3117(13) 0.044(7) Uani 0.167(11) 1 d PDU C 2 H46A H 1.1135 -0.1101 0.3329 0.053 Uiso 0.167(11) 1 calc PR C 2 C51 C 1.3570(3) -0.2046(6) 0.0984(2) 0.0203(11) Uani 1 1 d . . . C52 C 1.3633(3) -0.0757(6) 0.1009(2) 0.0245(12) Uani 1 1 d . . . H52 H 1.3458 -0.0312 0.1250 0.029 Uiso 1 1 calc R . . C53 C 1.3956(4) -0.0129(8) 0.0679(2) 0.0325(15) Uani 1 1 d . . . H53 H 1.3999 0.0743 0.0694 0.039 Uiso 1 1 calc R . . C54 C 1.4211(4) -0.0784(9) 0.0331(3) 0.0394(18) Uani 1 1 d . . . H54 H 1.4425 -0.0351 0.0105 0.047 Uiso 1 1 calc R . . C55 C 1.4162(4) -0.2032(9) 0.0304(2) 0.0376(17) Uani 1 1 d . . . H55 H 1.4352 -0.2463 0.0066 0.045 Uiso 1 1 calc R . . C56 C 1.3831(3) -0.2691(7) 0.0627(2) 0.0292(13) Uani 1 1 d . . . H56 H 1.3784 -0.3562 0.0603 0.035 Uiso 1 1 calc R . . C61 C 1.3396(3) -0.4435(6) 0.1417(2) 0.0214(11) Uani 1 1 d . . . C62 C 1.3057(4) -0.5382(7) 0.1135(3) 0.0375(17) Uani 1 1 d . . . H62 H 1.2658 -0.5206 0.0898 0.045 Uiso 1 1 calc R . . C63 C 1.3302(4) -0.6586(7) 0.1198(3) 0.046(2) Uani 1 1 d . . . H63 H 1.3057 -0.7229 0.1011 0.055 Uiso 1 1 calc R . . C64 C 1.3888(4) -0.6862(7) 0.1524(3) 0.0361(16) Uani 1 1 d . . . H64 H 1.4054 -0.7686 0.1559 0.043 Uiso 1 1 calc R . . C65 C 1.4238(4) -0.5925(7) 0.1806(3) 0.0301(13) Uani 1 1 d . . . H65 H 1.4648 -0.6110 0.2032 0.036 Uiso 1 1 calc R . . C66 C 1.3993(3) -0.4720(6) 0.1759(2) 0.0250(12) Uani 1 1 d . . . H66 H 1.4227 -0.4089 0.1959 0.030 Uiso 1 1 calc R . . C71 C 1.1952(3) -0.0421(6) 0.0609(2) 0.0233(11) Uani 1 1 d . . . C72 C 1.1931(3) 0.0851(6) 0.0676(2) 0.0264(12) Uani 1 1 d . . . H72 H 1.1844 0.1178 0.0970 0.032 Uiso 1 1 calc R . . C73 C 1.2040(4) 0.1642(7) 0.0309(3) 0.0333(15) Uani 1 1 d . . . H73 H 1.2022 0.2509 0.0353 0.040 Uiso 1 1 calc R . . C74 C 1.2175(4) 0.1176(8) -0.0114(3) 0.0380(17) Uani 1 1 d . . . H74 H 1.2255 0.1723 -0.0360 0.046 Uiso 1 1 calc R . . C75 C 1.2194(4) -0.0086(9) -0.0185(3) 0.0375(17) Uani 1 1 d . . . H75 H 1.2280 -0.0401 -0.0481 0.045 Uiso 1 1 calc R . . C76 C 1.2088(4) -0.0891(7) 0.0175(2) 0.0311(14) Uani 1 1 d . . . H76 H 1.2107 -0.1756 0.0127 0.037 Uiso 1 1 calc R . . C81 C 1.0841(3) -0.1861(6) 0.0871(2) 0.0292(13) Uani 1 1 d DU . . C82 C 1.0448(3) -0.1490(9) 0.0439(3) 0.0428(18) Uani 1 1 d DU E . H82 H 1.0621 -0.0936 0.0230 0.051 Uiso 1 1 calc R D 1 C83 C 0.9776(10) -0.198(4) 0.0331(10) 0.062(7) Uani 0.43(4) 1 d PDU E 1 H83 H 0.9555 -0.2071 0.0005 0.075 Uiso 0.43(4) 1 calc PR E 1 C83A C 0.9747(8) -0.172(3) 0.0304(9) 0.053(5) Uani 0.57(4) 1 d PDU E 2 H83A H 0.9465 -0.1249 0.0058 0.064 Uiso 0.57(4) 1 calc PR E 2 C84 C 0.9425(9) -0.235(3) 0.0692(12) 0.063(7) Uani 0.43(4) 1 d PDU E 1 H84 H 0.8931 -0.2393 0.0635 0.076 Uiso 0.43(4) 1 calc PR E 1 C84A C 0.9469(8) -0.2658(15) 0.0542(7) 0.039(4) Uani 0.57(4) 1 d PDU E 2 H84A H 0.9014 -0.2963 0.0425 0.047 Uiso 0.57(4) 1 calc PR E 2 C85 C 0.9813(9) -0.265(4) 0.1137(11) 0.058(6) Uani 0.43(4) 1 d PDU E 1 H85 H 0.9615 -0.3091 0.1368 0.069 Uiso 0.43(4) 1 calc PR E 1 C85A C 0.9871(8) -0.314(2) 0.0953(10) 0.056(7) Uani 0.57(4) 1 d PD E 2 H85A H 0.9679 -0.3761 0.1126 0.067 Uiso 0.57(4) 1 calc PR E 2 C86 C 1.0504(8) -0.227(3) 0.1234(7) 0.039(5) Uani 0.43(4) 1 d PDU E 1 H86 H 1.0753 -0.2297 0.1555 0.046 Uiso 0.43(4) 1 calc PR E 1 C86A C 1.0546(8) -0.274(2) 0.1120(8) 0.050(5) Uani 0.57(4) 1 d PDU E 2 H86A H 1.0806 -0.3078 0.1407 0.060 Uiso 0.57(4) 1 calc PR E 2 S1S S 1.22513(11) -0.0357(2) 0.45900(6) 0.0367(4) Uani 1 1 d . . . Cl4S Cl 1.38240(12) 0.2173(2) -0.03147(9) 0.0506(5) Uani 1 1 d DU . . Cl3S Cl 1.45634(17) 0.3788(5) 0.04087(14) 0.1035(15) Uani 1 1 d DU . . O3S O 1.2521(4) -0.0988(10) 0.5000(3) 0.081(3) Uani 1 1 d . . . F3S F 1.1655(6) -0.2203(8) 0.4147(4) 0.110(3) Uani 1 1 d . . . C3S C 1.3815(5) 0.3615(9) -0.0037(3) 0.053(2) Uani 1 1 d DU . . H3S1 H 1.3394 0.3688 0.0109 0.064 Uiso 1 1 calc R . . H3S2 H 1.3799 0.4277 -0.0280 0.064 Uiso 1 1 calc R . . F2S F 1.1045(4) -0.1222(13) 0.4604(5) 0.146(5) Uani 1 1 d . . . F1S F 1.1123(8) -0.0419(10) 0.3957(6) 0.226(10) Uani 1 1 d . . . O2S O 1.2704(6) -0.0307(10) 0.4242(3) 0.090(3) Uani 1 1 d . . . O1S O 1.2053(6) 0.0868(10) 0.4685(6) 0.140(6) Uani 1 1 d . . . C2S C 1.1510(6) -0.1074(11) 0.4297(4) 0.062(3) Uani 1 1 d . . . 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 Br1 0.0208(2) 0.0173(2) 0.0236(3) 0.0016(2) 0.00361(19) -0.00227(19) Rh1 0.01379(17) 0.01766(19) 0.01198(18) -0.00024(14) 0.00166(13) 0.00019(13) Au1 0.01891(10) 0.01977(11) 0.01554(10) 0.00018(7) 0.00123(7) 0.00446(7) P1 0.0158(6) 0.0150(6) 0.0120(6) 0.0012(5) 0.0026(4) 0.0012(4) P2 0.0203(6) 0.0190(7) 0.0159(6) 0.0002(5) 0.0020(5) 0.0056(5) P3 0.0167(6) 0.0196(6) 0.0127(6) -0.0011(5) 0.0004(4) 0.0023(5) P4 0.0169(6) 0.0180(6) 0.0164(6) -0.0009(5) -0.0016(5) 0.0010(5) O1 0.022(2) 0.049(3) 0.022(2) 0.000(2) 0.0043(16) -0.008(2) C1 0.019(2) 0.021(3) 0.018(2) 0.002(2) 0.0049(19) 0.004(2) C4S 0.067(18) 0.27(7) 0.16(3) 0.15(4) -0.005(15) 0.03(2) Cl5S 0.066(4) 0.072(4) 0.081(5) 0.002(3) -0.025(3) 0.020(3) Cl6S 0.068(4) 0.049(3) 0.103(5) 0.029(3) 0.027(3) 0.008(3) C1S 0.037(8) 0.120(18) 0.043(10) -0.030(10) 0.006(6) -0.019(10) Cl1S 0.077(3) 0.073(3) 0.043(2) 0.006(2) 0.010(2) 0.035(3) Cl2S 0.0191(14) 0.063(3) 0.100(3) 0.054(2) -0.0138(17) -0.0194(15) C2 0.020(2) 0.025(3) 0.021(3) -0.003(2) -0.002(2) 0.001(2) C3 0.025(3) 0.027(3) 0.013(2) 0.000(2) 0.0001(19) -0.001(2) C11 0.019(2) 0.015(2) 0.018(2) -0.0010(19) 0.0023(18) 0.0031(18) C12 0.023(3) 0.023(3) 0.021(3) -0.001(2) 0.002(2) -0.001(2) C13 0.024(3) 0.027(3) 0.027(3) -0.006(2) -0.003(2) -0.002(2) C14 0.025(3) 0.022(3) 0.038(4) -0.006(3) 0.002(2) -0.004(2) C15 0.030(3) 0.017(3) 0.041(4) 0.003(3) 0.003(3) 0.000(2) C16 0.024(3) 0.018(3) 0.025(3) 0.000(2) 0.002(2) 0.000(2) C21 0.016(2) 0.015(2) 0.018(2) -0.0008(19) 0.0010(18) 0.0008(18) C22 0.020(2) 0.030(3) 0.021(3) 0.006(2) 0.007(2) 0.004(2) C23 0.033(3) 0.034(3) 0.022(3) 0.011(3) 0.007(2) 0.002(3) C24 0.036(3) 0.024(3) 0.024(3) 0.009(2) 0.004(2) 0.006(2) C25 0.031(3) 0.026(3) 0.030(3) 0.007(2) 0.006(2) 0.012(2) C26 0.027(3) 0.022(3) 0.018(3) 0.003(2) 0.006(2) 0.005(2) C31 0.029(3) 0.019(3) 0.024(3) 0.000(2) 0.000(2) 0.007(2) C32 0.048(4) 0.026(3) 0.024(3) -0.001(3) 0.000(3) 0.004(3) C33 0.078(6) 0.026(3) 0.025(3) 0.000(3) -0.012(4) 0.003(4) C34 0.065(5) 0.018(3) 0.039(4) 0.002(3) -0.010(4) 0.002(3) C35 0.054(5) 0.021(3) 0.039(4) 0.007(3) 0.000(3) 0.005(3) C36 0.042(4) 0.016(3) 0.030(3) 0.007(2) 0.002(3) 0.007(2) C41 0.023(3) 0.037(3) 0.024(3) -0.001(3) 0.005(2) 0.009(2) C44 0.026(4) 0.086(7) 0.072(6) -0.002(6) 0.015(4) 0.012(4) C42 0.040(5) 0.042(5) 0.082(8) -0.010(5) 0.019(5) 0.015(4) C43 0.041(5) 0.057(6) 0.119(11) -0.018(7) 0.030(6) 0.019(5) C45 0.028(4) 0.062(6) 0.089(9) 0.013(7) 0.013(5) -0.001(4) C46 0.026(4) 0.047(5) 0.083(8) 0.010(6) 0.011(5) 0.004(4) C42A 0.016(11) 0.09(2) 0.057(15) 0.023(17) 0.003(8) 0.020(15) C43A 0.021(9) 0.10(2) 0.076(13) 0.015(19) 0.015(11) 0.015(17) C45A 0.027(12) 0.07(2) 0.067(16) 0.005(16) 0.016(10) -0.007(15) C46A 0.024(9) 0.056(18) 0.054(15) 0.016(13) 0.009(11) -0.002(13) C51 0.014(2) 0.030(3) 0.015(2) 0.003(2) -0.0006(18) 0.002(2) C52 0.022(3) 0.034(3) 0.017(3) 0.003(2) 0.000(2) -0.002(2) C53 0.030(3) 0.045(4) 0.021(3) 0.011(3) 0.001(2) -0.010(3) C54 0.029(3) 0.069(6) 0.020(3) 0.012(3) 0.005(2) -0.002(3) C55 0.033(3) 0.062(5) 0.020(3) 0.009(3) 0.012(3) 0.013(3) C56 0.027(3) 0.040(4) 0.020(3) 0.002(3) 0.004(2) 0.010(3) C61 0.020(2) 0.023(3) 0.020(3) -0.003(2) 0.002(2) 0.004(2) C62 0.037(4) 0.033(4) 0.035(4) -0.014(3) -0.012(3) 0.010(3) C63 0.045(4) 0.028(4) 0.055(5) -0.018(3) -0.017(4) 0.007(3) C64 0.039(4) 0.025(3) 0.041(4) -0.004(3) -0.001(3) 0.009(3) C65 0.031(3) 0.027(3) 0.030(3) 0.002(3) -0.001(2) 0.007(3) C66 0.026(3) 0.020(3) 0.027(3) 0.003(2) -0.001(2) 0.001(2) C71 0.020(3) 0.028(3) 0.020(3) 0.003(2) -0.001(2) 0.001(2) C72 0.029(3) 0.022(3) 0.026(3) 0.002(2) 0.000(2) 0.000(2) C73 0.032(3) 0.032(4) 0.033(4) 0.011(3) -0.001(3) -0.004(3) C74 0.027(3) 0.055(5) 0.032(4) 0.021(3) 0.003(3) 0.000(3) C75 0.029(3) 0.062(5) 0.024(3) 0.009(3) 0.011(3) 0.012(3) C76 0.033(3) 0.038(4) 0.022(3) -0.002(3) 0.004(2) 0.008(3) C81 0.018(2) 0.028(3) 0.037(3) 0.003(3) -0.006(2) -0.001(2) C82 0.022(3) 0.058(5) 0.042(4) 0.008(4) -0.009(3) 0.003(3) C83 0.036(8) 0.064(16) 0.070(11) 0.017(11) -0.035(8) -0.003(9) C83A 0.031(6) 0.056(12) 0.061(10) 0.019(8) -0.022(6) 0.003(7) C84 0.025(8) 0.047(14) 0.105(15) 0.025(13) -0.022(7) -0.015(9) C84A 0.025(6) 0.032(8) 0.054(9) -0.010(6) -0.009(5) -0.002(5) C85 0.026(7) 0.059(14) 0.085(13) 0.024(12) 0.002(8) -0.017(9) C85A 0.032(8) 0.048(12) 0.077(15) 0.028(11) -0.016(8) -0.014(8) C86 0.018(6) 0.035(12) 0.061(9) 0.011(9) 0.000(6) -0.007(7) C86A 0.027(7) 0.030(9) 0.083(11) 0.028(8) -0.014(7) -0.012(6) S1S 0.0439(10) 0.0436(10) 0.0224(8) 0.0008(7) 0.0056(7) 0.0133(8) Cl4S 0.0483(11) 0.0455(11) 0.0613(14) -0.0020(10) 0.0192(10) -0.0077(9) Cl3S 0.0585(17) 0.161(4) 0.087(2) -0.070(3) 0.0031(15) 0.001(2) O3S 0.059(4) 0.129(8) 0.047(4) 0.047(5) -0.015(3) -0.026(5) F3S 0.128(8) 0.068(5) 0.134(8) -0.031(5) 0.023(6) -0.009(5) C3S 0.048(5) 0.066(6) 0.045(5) -0.016(4) 0.008(4) 0.015(4) F2S 0.055(5) 0.214(13) 0.175(11) -0.098(10) 0.041(6) -0.055(6) F1S 0.204(13) 0.097(8) 0.281(18) 0.047(9) -0.206(14) -0.023(8) O2S 0.122(8) 0.110(8) 0.044(4) -0.017(5) 0.028(5) -0.048(6) O1S 0.072(7) 0.071(6) 0.267(18) -0.075(9) 0.003(9) 0.007(5) C2S 0.061(6) 0.062(7) 0.060(6) -0.015(5) 0.003(5) 0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Rh1 2.5238(7) . ? Rh1 C3 1.807(6) . ? Rh1 P1 2.3145(14) . ? Rh1 P3 2.3152(14) . ? Rh1 Au1 2.9537(5) . ? Au1 P4 2.3199(15) . ? Au1 P2 2.3206(15) . ? P1 C21 1.822(6) . ? P1 C11 1.827(6) . ? P1 C1 1.844(6) . ? P2 C31 1.804(7) . ? P2 C41 1.815(6) . ? P2 C1 1.836(6) . ? P3 C51 1.813(6) . ? P3 C61 1.824(6) . ? P3 C2 1.830(6) . ? P4 C71 1.800(7) . ? P4 C81 1.816(6) . ? P4 C2 1.841(6) . ? O1 C3 1.160(8) . ? C4S Cl5S 1.742(15) . ? C4S Cl6S 1.744(14) . ? C1S Cl2S 1.717(12) . ? C1S Cl1S 1.772(13) . ? C11 C16 1.388(8) . ? C11 C12 1.401(8) . ? C12 C13 1.390(9) . ? C13 C14 1.384(10) . ? C14 C15 1.398(10) . ? C15 C16 1.393(9) . ? C21 C26 1.392(8) . ? C21 C22 1.392(8) . ? C22 C23 1.396(9) . ? C23 C24 1.386(10) . ? C24 C25 1.381(9) . ? C25 C26 1.401(8) . ? C31 C32 1.398(9) . ? C31 C36 1.407(9) . ? C32 C33 1.385(11) . ? C33 C34 1.404(12) . ? C34 C35 1.385(12) . ? C35 C36 1.397(10) . ? C41 C46 1.367(10) . ? C41 C46A 1.394(13) . ? C41 C42A 1.394(13) . ? C41 C42 1.398(9) . ? C44 C45 1.366(11) . ? C44 C43 1.381(11) . ? C44 C43A 1.388(14) . ? C44 C45A 1.390(14) . ? C42 C43 1.378(10) . ? C45 C46 1.373(10) . ? C42A C43A 1.385(14) . ? C45A C46A 1.385(14) . ? C51 C56 1.402(9) . ? C51 C52 1.404(9) . ? C52 C53 1.399(9) . ? C53 C54 1.382(11) . ? C54 C55 1.358(13) . ? C55 C56 1.411(10) . ? C61 C62 1.392(9) . ? C61 C66 1.408(8) . ? C62 C63 1.390(10) . ? C63 C64 1.366(10) . ? C64 C65 1.392(10) . ? C65 C66 1.390(9) . ? C71 C72 1.394(9) . ? C71 C76 1.403(9) . ? C72 C73 1.393(9) . ? C73 C74 1.372(12) . ? C74 C75 1.384(13) . ? C75 C76 1.386(11) . ? C81 C86A 1.376(11) . ? C81 C82 1.379(8) . ? C81 C86 1.396(12) . ? C82 C83A 1.377(12) . ? C82 C83 1.401(13) . ? C83 C84 1.391(14) . ? C83A C84A 1.390(13) . ? C84 C85 1.387(13) . ? C84A C85A 1.381(12) . ? C85 C86 1.390(12) . ? C85A C86A 1.388(11) . ? S1S O3S 1.367(7) . ? S1S O1S 1.424(10) . ? S1S O2S 1.443(9) . ? S1S C2S 1.718(11) . ? Cl4S C3S 1.752(8) . ? Cl3S C3S 1.759(8) . ? F3S C2S 1.344(14) . ? F2S C2S 1.380(15) . ? F1S C2S 1.319(15) . ? 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 C3 Rh1 P1 91.94(18) . . ? C3 Rh1 P3 92.10(19) . . ? P1 Rh1 P3 175.21(5) . . ? C3 Rh1 Br1 172.2(2) . . ? P1 Rh1 Br1 87.75(4) . . ? P3 Rh1 Br1 87.90(4) . . ? C3 Rh1 Au1 116.5(2) . . ? P1 Rh1 Au1 90.69(4) . . ? P3 Rh1 Au1 89.81(4) . . ? Br1 Rh1 Au1 71.381(18) . . ? P4 Au1 P2 170.83(5) . . ? P4 Au1 Rh1 93.09(4) . . ? P2 Au1 Rh1 91.88(4) . . ? C21 P1 C11 104.9(2) . . ? C21 P1 C1 104.9(3) . . ? C11 P1 C1 104.1(3) . . ? C21 P1 Rh1 109.80(19) . . ? C11 P1 Rh1 119.12(19) . . ? C1 P1 Rh1 112.88(19) . . ? C31 P2 C41 106.6(3) . . ? C31 P2 C1 106.2(3) . . ? C41 P2 C1 104.9(3) . . ? C31 P2 Au1 116.3(2) . . ? C41 P2 Au1 109.9(2) . . ? C1 P2 Au1 112.33(19) . . ? C51 P3 C61 106.4(3) . . ? C51 P3 C2 103.0(3) . . ? C61 P3 C2 104.7(3) . . ? C51 P3 Rh1 117.4(2) . . ? C61 P3 Rh1 110.8(2) . . ? C2 P3 Rh1 113.5(2) . . ? C71 P4 C81 105.6(3) . . ? C71 P4 C2 108.7(3) . . ? C81 P4 C2 102.8(3) . . ? C71 P4 Au1 117.3(2) . . ? C81 P4 Au1 110.6(2) . . ? C2 P4 Au1 110.8(2) . . ? P2 C1 P1 112.5(3) . . ? Cl5S C4S Cl6S 125.9(14) . . ? Cl2S C1S Cl1S 100.1(8) . . ? P3 C2 P4 113.6(3) . . ? O1 C3 Rh1 177.5(6) . . ? C16 C11 C12 119.4(5) . . ? C16 C11 P1 119.7(4) . . ? C12 C11 P1 120.8(4) . . ? C13 C12 C11 119.8(6) . . ? C14 C13 C12 120.9(6) . . ? C13 C14 C15 119.4(6) . . ? C16 C15 C14 119.9(6) . . ? C11 C16 C15 120.6(6) . . ? C26 C21 C22 119.5(5) . . ? C26 C21 P1 116.6(4) . . ? C22 C21 P1 123.9(4) . . ? C21 C22 C23 119.9(6) . . ? C24 C23 C22 120.2(6) . . ? C25 C24 C23 120.3(6) . . ? C24 C25 C26 119.7(6) . . ? C21 C26 C25 120.3(6) . . ? C32 C31 C36 119.4(6) . . ? C32 C31 P2 121.7(5) . . ? C36 C31 P2 118.9(5) . . ? C33 C32 C31 120.1(7) . . ? C32 C33 C34 120.5(7) . . ? C35 C34 C33 119.8(7) . . ? C34 C35 C36 120.2(7) . . ? C35 C36 C31 120.1(7) . . ? C46 C41 C46A 42(2) . . ? C46 C41 C42A 91(2) . . ? C46A C41 C42A 115.9(14) . . ? C46 C41 C42 118.9(7) . . ? C46A C41 C42 101(2) . . ? C42A C41 C42 60(3) . . ? C46 C41 P2 121.5(5) . . ? C46A C41 P2 124.8(9) . . ? C42A C41 P2 116.5(10) . . ? C42 C41 P2 119.5(6) . . ? C45 C44 C43 118.2(8) . . ? C45 C44 C43A 87(3) . . ? C43 C44 C43A 65(3) . . ? C45 C44 C45A 45(3) . . ? C43 C44 C45A 99(2) . . ? C43A C44 C45A 117.3(16) . . ? C43 C42 C41 119.2(9) . . ? C42 C43 C44 121.2(9) . . ? C44 C45 C46 121.3(9) . . ? C41 C46 C45 120.5(9) . . ? C43A C42A C41 120.8(16) . . ? C42A C43A C44 118.2(18) . . ? C46A C45A C44 119.1(16) . . ? C45A C46A C41 120.5(17) . . ? C56 C51 C52 119.5(6) . . ? C56 C51 P3 121.3(5) . . ? C52 C51 P3 119.1(5) . . ? C53 C52 C51 119.8(6) . . ? C54 C53 C52 119.7(7) . . ? C55 C54 C53 121.4(7) . . ? C54 C55 C56 120.3(7) . . ? C51 C56 C55 119.3(7) . . ? C62 C61 C66 118.7(6) . . ? C62 C61 P3 124.8(5) . . ? C66 C61 P3 116.5(5) . . ? C63 C62 C61 120.2(6) . . ? C64 C63 C62 121.3(7) . . ? C63 C64 C65 119.5(7) . . ? C66 C65 C64 120.4(6) . . ? C65 C66 C61 120.1(6) . . ? C72 C71 C76 119.5(6) . . ? C72 C71 P4 118.4(5) . . ? C76 C71 P4 122.0(5) . . ? C73 C72 C71 119.7(7) . . ? C74 C73 C72 120.4(7) . . ? C73 C74 C75 120.4(7) . . ? C74 C75 C76 120.3(7) . . ? C75 C76 C71 119.7(7) . . ? C86A C81 C82 116.1(8) . . ? C86A C81 C86 25.7(10) . . ? C82 C81 C86 119.1(9) . . ? C86A C81 P4 120.0(7) . . ? C82 C81 P4 123.4(5) . . ? C86 C81 P4 114.7(9) . . ? C83A C82 C81 124.0(10) . . ? C83A C82 C83 13(2) . . ? C81 C82 C83 115.5(12) . . ? C84 C83 C82 121.3(17) . . ? C82 C83A C84A 117.0(13) . . ? C85 C84 C83 118.3(15) . . ? C85A C84A C83A 118.4(11) . . ? C84 C85 C86 117.4(14) . . ? C84A C85A C86A 121.8(12) . . ? C85 C86 C81 121.6(14) . . ? C81 C86A C85A 120.3(11) . . ? O3S S1S O1S 112.5(9) . . ? O3S S1S O2S 114.2(6) . . ? O1S S1S O2S 108.5(8) . . ? O3S S1S C2S 110.1(6) . . ? O1S S1S C2S 106.2(6) . . ? O2S S1S C2S 104.8(6) . . ? Cl4S C3S Cl3S 110.0(5) . . ? F1S C2S F3S 112.6(12) . . ? F1S C2S F2S 99.6(14) . . ? F3S C2S F2S 107.2(12) . . ? F1S C2S S1S 115.4(10) . . ? F3S C2S S1S 110.9(9) . . ? F2S C2S S1S 110.2(8) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 7.178 _refine_diff_density_min -1.528 _refine_diff_density_rms 0.239 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 789598' #TrackingRef '- CIF final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H94 Au Cl5 F6 O P5 Rh' _chemical_formula_weight 1481.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.6050(13) _cell_length_b 20.5013(17) _cell_length_c 20.6567(18) _cell_angle_alpha 90.00 _cell_angle_beta 95.374(2) _cell_angle_gamma 90.00 _cell_volume 6157.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9543 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 29.19 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3008 _exptl_absorpt_coefficient_mu 3.048 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5162 _exptl_absorpt_correction_T_max 0.6577 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 122466 _diffrn_reflns_av_R_equivalents 0.0685 _diffrn_reflns_av_sigmaI/netI 0.0439 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 29.24 _reflns_number_total 16655 _reflns_number_gt 13444 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+22.7488P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16655 _refine_ls_number_parameters 672 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0899 _refine_ls_wR_factor_gt 0.0814 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au -0.103764(10) -0.100631(6) -0.287527(7) 0.01309(4) Uani 1 1 d . A . Rh1 Rh -0.09949(2) -0.230434(13) -0.302821(14) 0.01159(6) Uani 1 1 d D . . P4 P 0.05836(7) -0.08994(4) -0.27934(5) 0.01376(18) Uani 1 1 d . . . P2 P -0.26558(7) -0.09659(4) -0.28565(5) 0.01357(18) Uani 1 1 d . . . Cl2 Cl -0.09753(7) -0.34726(4) -0.31596(5) 0.01914(19) Uani 1 1 d . A . P1 P -0.25971(7) -0.23524(4) -0.34058(5) 0.01313(18) Uani 1 1 d . A . P3 P 0.06021(7) -0.24039(4) -0.26428(5) 0.01394(19) Uani 1 1 d . A . Cl3 Cl -0.11138(7) 0.01596(4) -0.26690(6) 0.0245(2) Uani 1 1 d . . . C1 C -0.3227(3) -0.17590(17) -0.29577(19) 0.0148(7) Uani 1 1 d . A . H1A H -0.3311 -0.1939 -0.2523 0.018 Uiso 1 1 calc R . . H1B H -0.3845 -0.1695 -0.3190 0.018 Uiso 1 1 calc R . . C2 C 0.1219(3) -0.16653(17) -0.2839(2) 0.0165(8) Uani 1 1 d . A . H2A H 0.1406 -0.1711 -0.3285 0.020 Uiso 1 1 calc R . . H2B H 0.1787 -0.1636 -0.2540 0.020 Uiso 1 1 calc R . . C11 C -0.3192(3) -0.31336(17) -0.32780(19) 0.0149(7) Uani 1 1 d . . . H11A H -0.2857 -0.3477 -0.3506 0.018 Uiso 1 1 calc R A . C71 C 0.1099(3) -0.04154(17) -0.34221(18) 0.0154(7) Uani 1 1 d . A . H71A H 0.1771 -0.0519 -0.3376 0.018 Uiso 1 1 calc R . . C21 C -0.2759(3) -0.21618(19) -0.42866(18) 0.0162(7) Uani 1 1 d . . . H21A H -0.2302 -0.1810 -0.4350 0.019 Uiso 1 1 calc R A . C61 C 0.1227(3) -0.30642(18) -0.30283(19) 0.0161(7) Uani 1 1 d . . . H61A H 0.0974 -0.3486 -0.2878 0.019 Uiso 1 1 calc R A . C31 C -0.3276(3) -0.04226(18) -0.34727(19) 0.0176(8) Uani 1 1 d . A . H31A H -0.3882 -0.0638 -0.3594 0.021 Uiso 1 1 calc R . . C22 C -0.3680(3) -0.1894(2) -0.45971(19) 0.0197(8) Uani 1 1 d . A . H22A H -0.4159 -0.2236 -0.4600 0.024 Uiso 1 1 calc R . . H22B H -0.3876 -0.1520 -0.4341 0.024 Uiso 1 1 calc R . . C56 C 0.0547(3) -0.32310(18) -0.15749(19) 0.0183(8) Uani 1 1 d . A . H56A H -0.0046 -0.3362 -0.1811 0.022 Uiso 1 1 calc R . . H56B H 0.1031 -0.3529 -0.1704 0.022 Uiso 1 1 calc R . . C62 C 0.1056(3) -0.30594(18) -0.37741(19) 0.0185(8) Uani 1 1 d . A . H62A H 0.0387 -0.3089 -0.3903 0.022 Uiso 1 1 calc R . . H62B H 0.1281 -0.2643 -0.3944 0.022 Uiso 1 1 calc R . . C51 C 0.0778(3) -0.25265(18) -0.17528(19) 0.0152(7) Uani 1 1 d . . . H51A H 0.0297 -0.2252 -0.1570 0.018 Uiso 1 1 calc R A . C12 C -0.3143(3) -0.33348(19) -0.2558(2) 0.0193(8) Uani 1 1 d . A . H12A H -0.2491 -0.3358 -0.2378 0.023 Uiso 1 1 calc R . . H12B H -0.3453 -0.3001 -0.2310 0.023 Uiso 1 1 calc R . . C72 C 0.0737(3) -0.06263(19) -0.41102(19) 0.0180(8) Uani 1 1 d . . . H72A H 0.0079 -0.0508 -0.4193 0.022 Uiso 1 1 calc R A . H72B H 0.0790 -0.1106 -0.4151 0.022 Uiso 1 1 calc R . . C13 C -0.3602(3) -0.39981(19) -0.2480(2) 0.0230(9) Uani 1 1 d . . . H13A H -0.3247 -0.4339 -0.2685 0.028 Uiso 1 1 calc R A . H13B H -0.3594 -0.4102 -0.2011 0.028 Uiso 1 1 calc R . . C52 C 0.1692(3) -0.23135(19) -0.13840(19) 0.0181(8) Uani 1 1 d . A . H52A H 0.2195 -0.2602 -0.1501 0.022 Uiso 1 1 calc R . . H52B H 0.1839 -0.1861 -0.1506 0.022 Uiso 1 1 calc R . . C41 C -0.2945(3) -0.06686(18) -0.20570(19) 0.0184(8) Uani 1 1 d . A . H41A H -0.2820 -0.0189 -0.2045 0.022 Uiso 1 1 calc R . . C66 C 0.2260(3) -0.30675(19) -0.2812(2) 0.0195(8) Uani 1 1 d . A . H66A H 0.2531 -0.2645 -0.2928 0.023 Uiso 1 1 calc R . . H66B H 0.2353 -0.3116 -0.2334 0.023 Uiso 1 1 calc R . . C76 C 0.1025(3) 0.03317(18) -0.33561(19) 0.0190(8) Uani 1 1 d . . . H76A H 0.0372 0.0466 -0.3429 0.023 Uiso 1 1 calc R A . H76B H 0.1263 0.0467 -0.2912 0.023 Uiso 1 1 calc R . . C16 C -0.4193(3) -0.31417(19) -0.3586(2) 0.0206(8) Uani 1 1 d . A . H16A H -0.4550 -0.2801 -0.3381 0.025 Uiso 1 1 calc R . . H16B H -0.4206 -0.3041 -0.4055 0.025 Uiso 1 1 calc R . . C36 C -0.2813(3) -0.03681(19) -0.4103(2) 0.0197(8) Uani 1 1 d . . . H36A H -0.2639 -0.0807 -0.4249 0.024 Uiso 1 1 calc R A . H36B H -0.2247 -0.0102 -0.4030 0.024 Uiso 1 1 calc R . . C74 C 0.1265(3) 0.04484(19) -0.45515(19) 0.0191(8) Uani 1 1 d . . . H74A H 0.0632 0.0607 -0.4671 0.023 Uiso 1 1 calc R A . H74B H 0.1672 0.0645 -0.4856 0.023 Uiso 1 1 calc R . . C14 C -0.4592(3) -0.4005(2) -0.2787(2) 0.0272(10) Uani 1 1 d . A . H14A H -0.4852 -0.4448 -0.2752 0.033 Uiso 1 1 calc R . . H14B H -0.4966 -0.3700 -0.2549 0.033 Uiso 1 1 calc R . . C26 C -0.2443(3) -0.27475(19) -0.4682(2) 0.0208(8) Uani 1 1 d . A . H26A H -0.1854 -0.2921 -0.4475 0.025 Uiso 1 1 calc R . . H26B H -0.2908 -0.3100 -0.4693 0.025 Uiso 1 1 calc R . . C75 C 0.1582(3) 0.06625(18) -0.3856(2) 0.0200(8) Uani 1 1 d . A . H75A H 0.1517 0.1142 -0.3822 0.024 Uiso 1 1 calc R . . H75B H 0.2241 0.0553 -0.3758 0.024 Uiso 1 1 calc R . . C46 C -0.2357(3) -0.0970(2) -0.1487(2) 0.0253(9) Uani 1 1 d . . . H46A H -0.1698 -0.0915 -0.1553 0.030 Uiso 1 1 calc R A . H46B H -0.2486 -0.1443 -0.1467 0.030 Uiso 1 1 calc R . . C73 C 0.1287(3) -0.02925(19) -0.4613(2) 0.0194(8) Uani 1 1 d . A . H73A H 0.1933 -0.0444 -0.4554 0.023 Uiso 1 1 calc R . . H73B H 0.1029 -0.0419 -0.5056 0.023 Uiso 1 1 calc R . . C42 C -0.3972(3) -0.0758(2) -0.1960(2) 0.0243(9) Uani 1 1 d . . . H42A H -0.4356 -0.0563 -0.2331 0.029 Uiso 1 1 calc R A . H42B H -0.4120 -0.1228 -0.1941 0.029 Uiso 1 1 calc R . . C23 C -0.3562(3) -0.1677(2) -0.5295(2) 0.0247(9) Uani 1 1 d . . . H23A H -0.3125 -0.1307 -0.5284 0.030 Uiso 1 1 calc R A . H23B H -0.4162 -0.1523 -0.5504 0.030 Uiso 1 1 calc R . . C86 C 0.1997(3) -0.0446(2) -0.1875(2) 0.0242(9) Uani 1 1 d . . . H86A H 0.2254 -0.0892 -0.1824 0.029 Uiso 1 1 calc R A . H86B H 0.2266 -0.0236 -0.2244 0.029 Uiso 1 1 calc R . . C81 C 0.0944(3) -0.0487(2) -0.20220(19) 0.0208(8) Uani 1 1 d . A . H81A H 0.0732 -0.0025 -0.2084 0.025 Uiso 1 1 calc R . . C32 C -0.3505(3) 0.0267(2) -0.3239(2) 0.0247(9) Uani 1 1 d . . . H32A H -0.3786 0.0238 -0.2821 0.030 Uiso 1 1 calc R A . H32B H -0.2935 0.0528 -0.3167 0.030 Uiso 1 1 calc R . . C25 C -0.2321(3) -0.2521(2) -0.5375(2) 0.0247(9) Uani 1 1 d . . . H25A H -0.1827 -0.2190 -0.5362 0.030 Uiso 1 1 calc R A . H25B H -0.2132 -0.2896 -0.5633 0.030 Uiso 1 1 calc R . . C55 C 0.0484(3) -0.3279(2) -0.0841(2) 0.0229(9) Uani 1 1 d . . . H55A H -0.0043 -0.3013 -0.0724 0.027 Uiso 1 1 calc R A . H55B H 0.0366 -0.3738 -0.0725 0.027 Uiso 1 1 calc R . . C24 C -0.3206(3) -0.2232(2) -0.5703(2) 0.0280(10) Uani 1 1 d . A . H24A H -0.3679 -0.2578 -0.5765 0.034 Uiso 1 1 calc R . . H24B H -0.3092 -0.2063 -0.6137 0.034 Uiso 1 1 calc R . . C63 C 0.1550(3) -0.3632(2) -0.4072(2) 0.0227(9) Uani 1 1 d . . . H63A H 0.1297 -0.4049 -0.3925 0.027 Uiso 1 1 calc R A . H63B H 0.1440 -0.3614 -0.4552 0.027 Uiso 1 1 calc R . . C53 C 0.1608(3) -0.2353(2) -0.0653(2) 0.0215(8) Uani 1 1 d . . . H53A H 0.2198 -0.2221 -0.0413 0.026 Uiso 1 1 calc R A . H53B H 0.1127 -0.2045 -0.0536 0.026 Uiso 1 1 calc R . . C15 C -0.4638(3) -0.3807(2) -0.3498(2) 0.0258(9) Uani 1 1 d . . . H15A H -0.5290 -0.3791 -0.3680 0.031 Uiso 1 1 calc R A . H15B H -0.4321 -0.4140 -0.3743 0.031 Uiso 1 1 calc R . . C65 C 0.2752(3) -0.3623(2) -0.3134(2) 0.0253(9) Uani 1 1 d . . . H65A H 0.3421 -0.3590 -0.3007 0.030 Uiso 1 1 calc R A . H65B H 0.2537 -0.4045 -0.2972 0.030 Uiso 1 1 calc R . . C64 C 0.2582(3) -0.3608(2) -0.3872(2) 0.0245(9) Uani 1 1 d . A . H64A H 0.2887 -0.3985 -0.4060 0.029 Uiso 1 1 calc R . . H64B H 0.2845 -0.3204 -0.4042 0.029 Uiso 1 1 calc R . . C35 C -0.3483(3) -0.0048(2) -0.4626(2) 0.0246(9) Uani 1 1 d . A . H35A H -0.3181 -0.0005 -0.5034 0.029 Uiso 1 1 calc R . . H35B H -0.4031 -0.0329 -0.4715 0.029 Uiso 1 1 calc R . . C82 C 0.0474(3) -0.0741(2) -0.1440(2) 0.0252(9) Uani 1 1 d . . . H82A H -0.0202 -0.0717 -0.1540 0.030 Uiso 1 1 calc R A . H82B H 0.0643 -0.1203 -0.1361 0.030 Uiso 1 1 calc R . . C34 C -0.3783(3) 0.0623(2) -0.4411(2) 0.0297(10) Uani 1 1 d . . . H34A H -0.4254 0.0799 -0.4741 0.036 Uiso 1 1 calc R A . H34B H -0.3248 0.0923 -0.4384 0.036 Uiso 1 1 calc R . . C54 C 0.1362(3) -0.3042(2) -0.0450(2) 0.0245(9) Uani 1 1 d . A . H54A H 0.1273 -0.3047 0.0019 0.029 Uiso 1 1 calc R . . H54B H 0.1875 -0.3342 -0.0521 0.029 Uiso 1 1 calc R . . C85 C 0.2259(4) -0.0054(2) -0.1252(2) 0.0313(11) Uani 1 1 d . A . H85A H 0.2935 -0.0063 -0.1152 0.038 Uiso 1 1 calc R . . H85B H 0.2068 0.0406 -0.1322 0.038 Uiso 1 1 calc R . . C83 C 0.0755(4) -0.0342(2) -0.0828(2) 0.0329(11) Uani 1 1 d . A . H83A H 0.0472 -0.0533 -0.0454 0.039 Uiso 1 1 calc R . . H83B H 0.0524 0.0110 -0.0889 0.039 Uiso 1 1 calc R . . C33 C -0.4176(3) 0.0598(2) -0.3752(2) 0.0305(10) Uani 1 1 d . A . H33A H -0.4764 0.0354 -0.3795 0.037 Uiso 1 1 calc R . . H33B H -0.4305 0.1046 -0.3609 0.037 Uiso 1 1 calc R . . C84 C 0.1804(4) -0.0331(3) -0.0680(2) 0.0368(12) Uani 1 1 d . . . H84A H 0.1970 -0.0061 -0.0289 0.044 Uiso 1 1 calc R A . H84B H 0.2030 -0.0779 -0.0588 0.044 Uiso 1 1 calc R . . C45 C -0.2553(4) -0.0649(2) -0.0847(2) 0.0357(12) Uani 1 1 d . A . H45A H -0.2183 -0.0866 -0.0482 0.043 Uiso 1 1 calc R . . H45B H -0.2368 -0.0185 -0.0851 0.043 Uiso 1 1 calc R . . C43 C -0.4182(4) -0.0424(3) -0.1324(2) 0.0365(12) Uani 1 1 d . A . H43A H -0.4078 0.0051 -0.1358 0.044 Uiso 1 1 calc R . . H43B H -0.4836 -0.0494 -0.1254 0.044 Uiso 1 1 calc R . . C44 C -0.3571(4) -0.0696(3) -0.0740(2) 0.0420(14) Uani 1 1 d . . . H44A H -0.3687 -0.0449 -0.0344 0.050 Uiso 1 1 calc R A . H44B H -0.3733 -0.1158 -0.0671 0.050 Uiso 1 1 calc R . . Cl1 Cl -0.14314(9) -0.23709(6) -0.19493(8) 0.0140(5) Uani 0.785(7) 1 d PD A 1 C3 C -0.0677(5) -0.2109(3) -0.3834(3) 0.0123(12) Uani 0.785(7) 1 d PD A 1 O1 O -0.0495(4) -0.1976(3) -0.4357(3) 0.0166(10) Uani 0.785(7) 1 d PD A 1 Cl1A Cl -0.0564(4) -0.2005(3) -0.4082(3) 0.0140(17) Uani 0.215(7) 1 d PD A 2 O1A O -0.1468(11) -0.2476(8) -0.1688(7) 0.0166(10) Uani 0.215(7) 1 d PD A 2 C3A C -0.1319(14) -0.2393(9) -0.2228(8) 0.0123(12) Uani 0.215(7) 1 d PD A 2 P1S P 0.37273(9) -0.14291(7) -0.36465(7) 0.0365(3) Uani 1 1 d . . . F6S F 0.3303(2) -0.12106(18) -0.29934(16) 0.0485(8) Uani 1 1 d . . . F5S F 0.2725(2) -0.16607(19) -0.39322(17) 0.0535(9) Uani 1 1 d . . . F4S F 0.4727(2) -0.11922(19) -0.3351(2) 0.0622(11) Uani 1 1 d . . . F3S F 0.3935(2) -0.21327(18) -0.3340(2) 0.0601(10) Uani 1 1 d . . . F2S F 0.3523(2) -0.07237(18) -0.3941(2) 0.0637(11) Uani 1 1 d . . . F1S F 0.4147(3) -0.1662(2) -0.4297(2) 0.0733(13) Uani 1 1 d . . . Cl1S Cl 0.42794(17) -0.23618(16) -0.15703(13) 0.0759(8) Uani 0.748(3) 1 d PD B 1 Cl2S Cl 0.4192(2) -0.17123(17) -0.03298(16) 0.0878(10) Uani 0.748(3) 1 d PD B 1 C1S C 0.4164(5) -0.2481(4) -0.0734(4) 0.058(2) Uani 0.748(3) 1 d PD B 1 H1SA H 0.4672 -0.2760 -0.0541 0.070 Uiso 0.748(3) 1 calc PR B 1 H1SB H 0.3576 -0.2705 -0.0680 0.070 Uiso 0.748(3) 1 calc PR B 1 Cl3S Cl 0.4205(3) -0.07004(18) -0.01220(17) 0.0187(9) Uani 0.252(3) 1 d PD B 2 Cl4S Cl 0.4060(6) -0.1599(5) -0.0981(5) 0.0878(10) Uani 0.252(3) 1 d PD B 2 C2S C 0.434(2) -0.1556(9) -0.0135(9) 0.058(2) Uani 0.252(3) 1 d PD B 2 H2SA H 0.4975 -0.1699 0.0001 0.070 Uiso 0.252(3) 1 calc PR B 2 H2SB H 0.3895 -0.1789 0.0115 0.070 Uiso 0.252(3) 1 calc PR B 2 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 Au1 0.01259(7) 0.00850(6) 0.01809(7) 0.00010(5) 0.00102(5) 0.00008(5) Rh1 0.01012(14) 0.00842(11) 0.01614(14) -0.00006(10) 0.00078(11) -0.00012(10) P4 0.0133(5) 0.0097(4) 0.0180(5) 0.0009(3) -0.0002(4) -0.0010(3) P2 0.0135(5) 0.0098(4) 0.0175(5) 0.0000(3) 0.0019(4) 0.0018(3) Cl2 0.0146(4) 0.0096(4) 0.0332(5) -0.0021(3) 0.0016(4) -0.0001(3) P1 0.0111(5) 0.0102(4) 0.0179(5) -0.0006(3) 0.0005(4) -0.0002(3) P3 0.0108(5) 0.0093(4) 0.0217(5) 0.0013(3) 0.0009(4) -0.0001(3) Cl3 0.0204(5) 0.0103(4) 0.0427(6) -0.0032(4) 0.0032(4) 0.0007(3) C1 0.0115(18) 0.0114(15) 0.0219(19) 0.0004(14) 0.0032(15) -0.0017(13) C2 0.0127(18) 0.0136(16) 0.023(2) 0.0022(14) 0.0017(15) 0.0020(14) C11 0.0129(18) 0.0096(15) 0.0218(19) -0.0002(14) 0.0004(15) -0.0014(13) C71 0.0167(19) 0.0107(15) 0.0185(18) 0.0018(13) 0.0008(15) -0.0018(13) C21 0.0127(19) 0.0189(17) 0.0168(18) 0.0013(14) 0.0002(15) -0.0019(14) C61 0.0161(19) 0.0127(16) 0.0198(19) 0.0025(14) 0.0026(15) 0.0033(14) C31 0.017(2) 0.0134(16) 0.022(2) 0.0039(14) 0.0000(16) 0.0034(14) C22 0.019(2) 0.0196(18) 0.0200(19) 0.0025(15) -0.0001(16) 0.0002(15) C56 0.021(2) 0.0115(16) 0.022(2) 0.0021(14) -0.0015(16) 0.0002(14) C62 0.018(2) 0.0159(17) 0.022(2) 0.0041(15) 0.0028(16) 0.0039(15) C51 0.0133(19) 0.0136(16) 0.0184(18) -0.0012(14) 0.0000(15) 0.0004(14) C12 0.017(2) 0.0168(17) 0.024(2) 0.0009(15) 0.0031(16) -0.0047(15) C72 0.016(2) 0.0171(17) 0.0217(19) 0.0002(15) 0.0030(16) -0.0025(15) C13 0.019(2) 0.0170(18) 0.033(2) 0.0053(17) 0.0034(18) -0.0031(16) C52 0.017(2) 0.0183(17) 0.0177(19) 0.0024(15) -0.0033(15) -0.0018(15) C41 0.025(2) 0.0130(16) 0.0178(19) -0.0020(14) 0.0031(16) 0.0015(15) C66 0.0138(19) 0.0196(18) 0.025(2) -0.0012(16) 0.0042(16) 0.0038(15) C76 0.027(2) 0.0139(17) 0.0166(18) -0.0010(14) 0.0030(16) -0.0021(15) C16 0.015(2) 0.0155(17) 0.031(2) 0.0017(16) 0.0006(17) -0.0049(15) C36 0.021(2) 0.0174(18) 0.022(2) 0.0036(15) 0.0065(16) 0.0004(15) C74 0.019(2) 0.0179(18) 0.0208(19) 0.0034(15) 0.0038(16) 0.0015(15) C14 0.020(2) 0.021(2) 0.040(3) 0.0053(18) 0.0034(19) -0.0102(17) C26 0.023(2) 0.0185(18) 0.021(2) -0.0039(15) 0.0025(17) -0.0032(16) C75 0.022(2) 0.0131(16) 0.025(2) 0.0018(15) 0.0006(17) -0.0026(15) C46 0.028(2) 0.0211(19) 0.026(2) 0.0024(17) -0.0034(18) 0.0042(17) C73 0.019(2) 0.0179(18) 0.021(2) -0.0003(15) 0.0039(16) -0.0027(15) C42 0.026(2) 0.023(2) 0.025(2) -0.0003(17) 0.0077(18) 0.0074(17) C23 0.026(2) 0.026(2) 0.020(2) 0.0040(17) -0.0042(17) -0.0024(18) C86 0.025(2) 0.0185(18) 0.027(2) 0.0043(16) -0.0041(18) -0.0075(16) C81 0.021(2) 0.0233(19) 0.0176(19) -0.0038(15) -0.0015(16) -0.0062(16) C32 0.032(3) 0.0182(18) 0.025(2) 0.0026(16) 0.0066(19) 0.0099(17) C25 0.028(2) 0.028(2) 0.019(2) -0.0044(17) 0.0043(18) -0.0009(18) C55 0.028(2) 0.0193(19) 0.021(2) 0.0055(16) 0.0013(17) -0.0044(17) C24 0.035(3) 0.032(2) 0.017(2) -0.0011(17) -0.0017(18) -0.006(2) C63 0.026(2) 0.0222(19) 0.021(2) -0.0014(16) 0.0074(17) 0.0019(17) C53 0.022(2) 0.0215(19) 0.021(2) 0.0001(16) -0.0025(16) -0.0011(16) C15 0.019(2) 0.0202(19) 0.037(3) 0.0027(18) -0.0053(18) -0.0094(16) C65 0.016(2) 0.024(2) 0.036(2) 0.0024(18) 0.0051(18) 0.0074(16) C64 0.022(2) 0.0194(19) 0.034(2) -0.0010(17) 0.0091(18) 0.0044(16) C35 0.025(2) 0.027(2) 0.022(2) 0.0069(17) 0.0045(18) 0.0015(17) C82 0.027(2) 0.0213(19) 0.027(2) -0.0005(17) 0.0007(18) -0.0007(17) C34 0.029(3) 0.026(2) 0.034(3) 0.0122(19) 0.003(2) 0.0063(19) C54 0.030(2) 0.023(2) 0.020(2) 0.0056(16) -0.0009(18) -0.0019(18) C85 0.036(3) 0.023(2) 0.032(3) 0.0023(18) -0.011(2) -0.0108(19) C83 0.046(3) 0.030(2) 0.023(2) -0.0065(19) 0.003(2) -0.003(2) C33 0.031(3) 0.023(2) 0.038(3) 0.0070(19) 0.009(2) 0.0121(19) C84 0.046(3) 0.034(3) 0.027(2) -0.006(2) -0.008(2) -0.014(2) C45 0.056(3) 0.027(2) 0.023(2) -0.0023(19) -0.004(2) 0.013(2) C43 0.044(3) 0.038(3) 0.030(2) 0.002(2) 0.015(2) 0.019(2) C44 0.066(4) 0.039(3) 0.023(2) 0.002(2) 0.014(2) 0.020(3) Cl1 0.0143(6) 0.0143(5) 0.0135(9) 0.0015(5) 0.0022(5) 0.0001(4) C3 0.015(3) 0.015(3) 0.008(3) -0.005(2) 0.004(3) 0.002(2) O1 0.021(2) 0.0182(18) 0.011(2) 0.002(2) 0.001(2) -0.0024(14) Cl1A 0.016(3) 0.022(3) 0.004(4) -0.003(3) 0.001(3) 0.002(2) O1A 0.021(2) 0.0182(18) 0.011(2) 0.002(2) 0.001(2) -0.0024(14) C3A 0.015(3) 0.015(3) 0.008(3) -0.005(2) 0.004(3) 0.002(2) P1S 0.0164(6) 0.0476(8) 0.0460(8) 0.0216(6) 0.0063(5) 0.0056(5) F6S 0.0299(17) 0.068(2) 0.0479(19) 0.0004(17) 0.0053(14) -0.0028(16) F5S 0.0275(17) 0.079(3) 0.054(2) -0.0065(18) 0.0012(15) -0.0004(17) F4S 0.0172(16) 0.074(3) 0.094(3) 0.032(2) -0.0035(17) -0.0048(16) F3S 0.045(2) 0.052(2) 0.085(3) 0.0299(19) 0.0150(19) 0.0085(17) F2S 0.046(2) 0.058(2) 0.087(3) 0.043(2) 0.006(2) 0.0117(17) F1S 0.054(2) 0.106(3) 0.065(3) 0.022(2) 0.033(2) 0.023(2) Cl1S 0.0450(14) 0.114(2) 0.0669(16) -0.0146(15) -0.0014(11) -0.0220(14) Cl2S 0.080(2) 0.096(2) 0.090(2) -0.0330(17) 0.0186(17) -0.0334(16) C1S 0.019(4) 0.076(6) 0.076(6) 0.007(5) -0.010(4) 0.011(4) Cl3S 0.022(2) 0.0252(18) 0.0098(16) 0.0008(13) 0.0065(14) 0.0003(15) Cl4S 0.080(2) 0.096(2) 0.090(2) -0.0330(17) 0.0186(17) -0.0334(16) C2S 0.019(4) 0.076(6) 0.076(6) 0.007(5) -0.010(4) 0.011(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P4 2.3681(10) . ? Au1 P2 2.3687(10) . ? Au1 Cl3 2.4323(9) . ? Au1 Rh1 2.6812(4) . ? Rh1 C3A 1.771(16) . ? Rh1 C3 1.813(7) . ? Rh1 Cl1 2.3786(16) . ? Rh1 P1 2.3983(10) . ? Rh1 P3 2.4017(11) . ? Rh1 Cl1A 2.402(7) . ? Rh1 Cl2 2.4109(9) . ? P4 C2 1.831(4) . ? P4 C81 1.837(4) . ? P4 C71 1.850(4) . ? P2 C1 1.830(4) . ? P2 C41 1.846(4) . ? P2 C31 1.862(4) . ? P1 C1 1.828(4) . ? P1 C11 1.852(4) . ? P1 C21 1.854(4) . ? P3 C2 1.827(4) . ? P3 C51 1.850(4) . ? P3 C61 1.853(4) . ? C11 C12 1.538(5) . ? C11 C16 1.540(6) . ? C71 C72 1.532(5) . ? C71 C76 1.542(5) . ? C21 C22 1.537(6) . ? C21 C26 1.547(5) . ? C61 C66 1.533(6) . ? C61 C62 1.537(5) . ? C31 C36 1.527(5) . ? C31 C32 1.541(5) . ? C22 C23 1.534(6) . ? C56 C55 1.530(6) . ? C56 C51 1.535(5) . ? C62 C63 1.537(5) . ? C51 C52 1.538(5) . ? C12 C13 1.532(5) . ? C72 C73 1.533(5) . ? C13 C14 1.523(6) . ? C52 C53 1.529(6) . ? C41 C46 1.522(6) . ? C41 C42 1.543(6) . ? C66 C65 1.530(5) . ? C76 C75 1.533(5) . ? C16 C15 1.529(5) . ? C36 C35 1.535(6) . ? C74 C73 1.525(5) . ? C74 C75 1.531(6) . ? C14 C15 1.520(6) . ? C26 C25 1.531(6) . ? C46 C45 1.529(6) . ? C42 C43 1.537(6) . ? C23 C24 1.535(6) . ? C86 C85 1.533(6) . ? C86 C81 1.542(6) . ? C81 C82 1.531(6) . ? C32 C33 1.532(6) . ? C25 C24 1.522(6) . ? C55 C54 1.530(6) . ? C63 C64 1.526(6) . ? C53 C54 1.527(6) . ? C65 C64 1.524(6) . ? C35 C34 1.522(6) . ? C82 C83 1.530(6) . ? C34 C33 1.528(6) . ? C85 C84 1.519(7) . ? C83 C84 1.534(7) . ? C45 C44 1.527(8) . ? C43 C44 1.535(7) . ? C3 O1 1.169(8) . ? O1A C3A 1.168(16) . ? P1S F2S 1.586(4) . ? P1S F3S 1.593(4) . ? P1S F5S 1.598(4) . ? P1S F6S 1.601(4) . ? P1S F1S 1.602(4) . ? P1S F4S 1.605(4) . ? Cl1S C1S 1.768(9) . ? Cl2S C1S 1.782(9) . ? Cl3S C2S 1.765(17) . ? Cl4S C2S 1.759(16) . ? 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 P4 Au1 P2 171.13(3) . . ? P4 Au1 Cl3 87.61(3) . . ? P2 Au1 Cl3 84.30(3) . . ? P4 Au1 Rh1 93.79(2) . . ? P2 Au1 Rh1 94.07(2) . . ? Cl3 Au1 Rh1 176.32(3) . . ? C3A Rh1 C3 173.2(6) . . ? C3A Rh1 Cl1 2.6(6) . . ? C3 Rh1 Cl1 170.6(2) . . ? C3A Rh1 P1 87.8(7) . . ? C3 Rh1 P1 92.1(2) . . ? Cl1 Rh1 P1 87.90(4) . . ? C3A Rh1 P3 91.0(7) . . ? C3 Rh1 P3 89.9(2) . . ? Cl1 Rh1 P3 91.25(4) . . ? P1 Rh1 P3 172.76(3) . . ? C3A Rh1 Cl1A 171.1(6) . . ? C3 Rh1 Cl1A 2.1(3) . . ? Cl1 Rh1 Cl1A 168.50(14) . . ? P1 Rh1 Cl1A 92.66(15) . . ? P3 Rh1 Cl1A 89.60(15) . . ? C3A Rh1 Cl2 90.6(6) . . ? C3 Rh1 Cl2 96.3(2) . . ? Cl1 Rh1 Cl2 93.18(4) . . ? P1 Rh1 Cl2 86.79(3) . . ? P3 Rh1 Cl2 86.07(3) . . ? Cl1A Rh1 Cl2 98.32(14) . . ? C3A Rh1 Au1 88.9(6) . . ? C3 Rh1 Au1 84.3(2) . . ? Cl1 Rh1 Au1 86.29(3) . . ? P1 Rh1 Au1 92.66(2) . . ? P3 Rh1 Au1 94.47(2) . . ? Cl1A Rh1 Au1 82.21(14) . . ? Cl2 Rh1 Au1 179.25(3) . . ? C2 P4 C81 109.5(2) . . ? C2 P4 C71 100.50(17) . . ? C81 P4 C71 105.04(18) . . ? C2 P4 Au1 115.15(13) . . ? C81 P4 Au1 107.93(14) . . ? C71 P4 Au1 118.01(13) . . ? C1 P2 C41 104.79(18) . . ? C1 P2 C31 105.43(18) . . ? C41 P2 C31 106.05(18) . . ? C1 P2 Au1 114.31(12) . . ? C41 P2 Au1 109.80(14) . . ? C31 P2 Au1 115.61(13) . . ? C1 P1 C11 103.79(17) . . ? C1 P1 C21 109.44(18) . . ? C11 P1 C21 107.68(18) . . ? C1 P1 Rh1 109.25(13) . . ? C11 P1 Rh1 116.44(13) . . ? C21 P1 Rh1 109.95(13) . . ? C2 P3 C51 107.94(18) . . ? C2 P3 C61 103.73(18) . . ? C51 P3 C61 107.45(17) . . ? C2 P3 Rh1 109.85(13) . . ? C51 P3 Rh1 112.40(13) . . ? C61 P3 Rh1 114.93(13) . . ? P1 C1 P2 113.8(2) . . ? P3 C2 P4 115.9(2) . . ? C12 C11 C16 110.6(3) . . ? C12 C11 P1 112.9(3) . . ? C16 C11 P1 113.0(3) . . ? C72 C71 C76 110.0(3) . . ? C72 C71 P4 111.9(3) . . ? C76 C71 P4 115.7(3) . . ? C22 C21 C26 110.4(3) . . ? C22 C21 P1 120.7(3) . . ? C26 C21 P1 109.7(3) . . ? C66 C61 C62 110.8(3) . . ? C66 C61 P3 112.9(3) . . ? C62 C61 P3 112.7(3) . . ? C36 C31 C32 109.1(3) . . ? C36 C31 P2 113.6(3) . . ? C32 C31 P2 116.1(3) . . ? C23 C22 C21 109.0(3) . . ? C55 C56 C51 109.4(3) . . ? C63 C62 C61 111.0(3) . . ? C56 C51 C52 110.4(3) . . ? C56 C51 P3 110.6(3) . . ? C52 C51 P3 119.1(3) . . ? C13 C12 C11 111.1(3) . . ? C71 C72 C73 110.2(3) . . ? C14 C13 C12 111.8(3) . . ? C53 C52 C51 109.2(3) . . ? C46 C41 C42 109.7(3) . . ? C46 C41 P2 113.4(3) . . ? C42 C41 P2 112.6(3) . . ? C65 C66 C61 111.5(3) . . ? C75 C76 C71 109.5(3) . . ? C15 C16 C11 111.0(3) . . ? C31 C36 C35 109.1(3) . . ? C73 C74 C75 110.9(3) . . ? C15 C14 C13 110.8(4) . . ? C25 C26 C21 109.0(3) . . ? C74 C75 C76 111.8(3) . . ? C41 C46 C45 110.9(4) . . ? C74 C73 C72 111.8(3) . . ? C43 C42 C41 109.4(4) . . ? C22 C23 C24 112.0(4) . . ? C85 C86 C81 111.1(4) . . ? C82 C81 C86 112.1(3) . . ? C82 C81 P4 114.3(3) . . ? C86 C81 P4 113.3(3) . . ? C33 C32 C31 109.4(4) . . ? C24 C25 C26 111.5(4) . . ? C54 C55 C56 112.2(4) . . ? C25 C24 C23 111.2(4) . . ? C64 C63 C62 110.8(3) . . ? C54 C53 C52 111.2(3) . . ? C14 C15 C16 111.8(4) . . ? C64 C65 C66 112.4(3) . . ? C65 C64 C63 109.6(3) . . ? C34 C35 C36 111.3(4) . . ? C83 C82 C81 111.2(4) . . ? C35 C34 C33 111.8(4) . . ? C53 C54 C55 110.8(3) . . ? C84 C85 C86 111.3(4) . . ? C82 C83 C84 111.0(4) . . ? C34 C33 C32 111.3(4) . . ? C85 C84 C83 110.7(4) . . ? C44 C45 C46 111.2(4) . . ? C44 C43 C42 111.2(4) . . ? C45 C44 C43 111.5(4) . . ? O1 C3 Rh1 178.2(8) . . ? O1A C3A Rh1 174.8(19) . . ? F2S P1S F3S 179.1(3) . . ? F2S P1S F5S 89.8(2) . . ? F3S P1S F5S 90.6(2) . . ? F2S P1S F6S 89.7(2) . . ? F3S P1S F6S 89.6(2) . . ? F5S P1S F6S 88.89(18) . . ? F2S P1S F1S 91.3(2) . . ? F3S P1S F1S 89.4(2) . . ? F5S P1S F1S 90.6(2) . . ? F6S P1S F1S 178.9(2) . . ? F2S P1S F4S 90.1(2) . . ? F3S P1S F4S 89.5(2) . . ? F5S P1S F4S 179.2(2) . . ? F6S P1S F4S 90.3(2) . . ? F1S P1S F4S 90.2(2) . . ? Cl1S C1S Cl2S 109.6(5) . . ? Cl4S C2S Cl3S 92.8(10) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 29.24 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.651 _refine_diff_density_min -1.686 _refine_diff_density_rms 0.147 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 789599' #TrackingRef '- CIF final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H94 Au Br3 Cl2 F6 O P5 Rh' _chemical_formula_weight 1614.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.6332(13) _cell_length_b 20.6673(18) _cell_length_c 20.6771(18) _cell_angle_alpha 90.00 _cell_angle_beta 95.422(2) _cell_angle_gamma 90.00 _cell_volume 6225.4(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9525 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 31.38 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3224 _exptl_absorpt_coefficient_mu 4.812 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2207 _exptl_absorpt_correction_T_max 0.4462 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 143038 _diffrn_reflns_av_R_equivalents 0.0525 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 30.51 _reflns_number_total 18943 _reflns_number_gt 15856 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+22.0452P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18943 _refine_ls_number_parameters 684 _refine_ls_number_restraints 80 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0829 _refine_ls_wR_factor_gt 0.0772 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.398490(8) 0.602453(5) 0.214437(6) 0.00999(3) Uani 1 1 d D A . Rh1 Rh 0.402587(16) 0.731624(11) 0.196729(11) 0.00848(5) Uani 1 1 d D . . Br1 Br 0.35963(3) 0.73895(2) 0.31114(2) 0.01180(12) Uani 0.8193(18) 1 d PDU A 1 C3 C 0.4331(3) 0.7117(2) 0.1152(3) 0.0101(7) Uani 0.8193(18) 1 d PDU A 1 O1 O 0.4503(5) 0.6971(4) 0.0636(2) 0.0153(12) Uani 0.8193(18) 1 d PDU A 1 Br1A Br 0.4419(3) 0.6983(2) 0.08413(17) 0.0119(7) Uani 0.1807(18) 1 d PDU A 2 O1A O 0.3558(12) 0.7463(9) 0.3332(7) 0.0153(12) Uani 0.1807(18) 1 d PDU A 2 P3 P 0.24136(5) 0.73545(4) 0.16092(4) 0.01033(14) Uani 1 1 d D A . P1S P 0.87407(7) 0.63982(6) 0.13405(6) 0.0335(3) Uani 1 1 d . . . F1S F 0.9152(2) 0.6611(2) 0.06821(18) 0.0714(12) Uani 1 1 d . . . C1 C 0.1790(2) 0.67623(15) 0.20639(15) 0.0116(6) Uani 1 1 d . . . H1A H 0.1708 0.6943 0.2498 0.014 Uiso 1 1 calc R A . H1B H 0.1172 0.6696 0.1834 0.014 Uiso 1 1 calc R . . Br2 Br 0.40488(2) 0.853792(15) 0.180260(17) 0.01464(6) Uani 1 1 d . A . P4 P 0.23657(6) 0.59768(4) 0.21669(4) 0.01083(14) Uani 1 1 d . A . F2S F 0.8951(2) 0.71052(16) 0.16206(18) 0.0543(9) Uani 1 1 d . . . C2 C 0.6234(2) 0.66704(15) 0.21449(16) 0.0130(6) Uani 1 1 d . . . H2A H 0.6411 0.6708 0.1696 0.016 Uiso 1 1 calc R A . H2B H 0.6808 0.6643 0.2438 0.016 Uiso 1 1 calc R . . Br3 Br 0.39158(2) 0.481708(16) 0.239363(19) 0.02000(7) Uani 1 1 d . . . P1 P 0.56354(5) 0.74133(4) 0.23371(4) 0.01070(14) Uani 1 1 d D A . F3S F 0.8534(2) 0.56925(17) 0.1060(2) 0.0648(11) Uani 1 1 d . . . P2 P 0.56050(6) 0.59139(4) 0.22078(4) 0.01074(14) Uani 1 1 d . A . F4S F 0.77402(19) 0.66268(17) 0.10504(15) 0.0484(8) Uani 1 1 d . . . F5S F 0.83211(19) 0.62041(17) 0.20013(15) 0.0464(7) Uani 1 1 d . . . F6S F 0.97388(19) 0.61722(18) 0.16423(19) 0.0597(10) Uani 1 1 d . . . C1S C 0.9211(6) 0.7523(4) 0.4267(4) 0.052(2) Uani 0.622(5) 1 d PDU B 1 H1S1 H 0.8619 0.7737 0.4327 0.062 Uiso 0.622(5) 1 calc PR B 1 H1S2 H 0.9710 0.7807 0.4458 0.062 Uiso 0.622(5) 1 calc PR B 1 C2S C 0.9069(10) 0.6842(6) 0.3206(6) 0.053(3) Uani 0.378(5) 1 d PDU B 2 H2S1 H 0.9393 0.6516 0.2961 0.064 Uiso 0.378(5) 1 calc PR B 2 H2S2 H 0.8426 0.6872 0.3010 0.064 Uiso 0.378(5) 1 calc PR B 2 C3A C 0.3710(11) 0.7415(8) 0.2788(6) 0.0101(7) Uani 0.1807(18) 1 d PDU A 2 C11 C 0.2233(2) 0.71561(16) 0.07347(15) 0.0135(6) Uani 1 1 d . . . H11 H 0.2694 0.6811 0.0668 0.016 Uiso 1 1 calc R A . C12 C 0.2525(2) 0.77385(17) 0.03310(16) 0.0171(6) Uani 1 1 d . A . H12A H 0.2056 0.8084 0.0327 0.021 Uiso 1 1 calc R . . H12B H 0.3115 0.7916 0.0529 0.021 Uiso 1 1 calc R . . C13 C 0.2628(3) 0.7516(2) -0.03627(18) 0.0242(8) Uani 1 1 d . . . H13A H 0.2804 0.7889 -0.0624 0.029 Uiso 1 1 calc R A . H13B H 0.3124 0.7190 -0.0357 0.029 Uiso 1 1 calc R . . C14 C 0.1738(3) 0.7224(2) -0.06769(18) 0.0286(9) Uani 1 1 d . A . H14A H 0.1835 0.7061 -0.1115 0.034 Uiso 1 1 calc R . . H14B H 0.1258 0.7563 -0.0726 0.034 Uiso 1 1 calc R . . C15 C 0.1412(3) 0.66666(19) -0.02650(18) 0.0239(8) Uani 1 1 d . . . H15A H 0.0813 0.6506 -0.0464 0.029 Uiso 1 1 calc R A . H15B H 0.1858 0.6306 -0.0261 0.029 Uiso 1 1 calc R . . C16 C 0.1313(2) 0.68819(18) 0.04347(17) 0.0187(7) Uani 1 1 d . A . H16A H 0.1131 0.6509 0.0694 0.022 Uiso 1 1 calc R . . H16B H 0.0830 0.7217 0.0437 0.022 Uiso 1 1 calc R . . C21 C 0.1802(2) 0.81290(15) 0.17264(16) 0.0131(6) Uani 1 1 d . . . H21 H 0.2127 0.8467 0.1490 0.016 Uiso 1 1 calc R A . C22 C 0.0799(2) 0.81308(17) 0.14259(18) 0.0175(6) Uani 1 1 d . A . H22A H 0.0776 0.8011 0.0961 0.021 Uiso 1 1 calc R . . H22B H 0.0442 0.7806 0.1649 0.021 Uiso 1 1 calc R . . C23 C 0.0373(3) 0.88012(18) 0.14912(19) 0.0221(7) Uani 1 1 d . . . H23A H 0.0698 0.9117 0.1235 0.027 Uiso 1 1 calc R A . H23B H -0.0277 0.8789 0.1310 0.027 Uiso 1 1 calc R . . C24 C 0.0425(3) 0.90222(19) 0.2193(2) 0.0239(8) Uani 1 1 d . A . H24A H 0.0043 0.8735 0.2440 0.029 Uiso 1 1 calc R . . H24B H 0.0178 0.9467 0.2213 0.029 Uiso 1 1 calc R . . C25 C 0.1411(3) 0.90107(17) 0.25010(19) 0.0208(7) Uani 1 1 d . . . H25A H 0.1421 0.9124 0.2967 0.025 Uiso 1 1 calc R A . H25B H 0.1773 0.9340 0.2289 0.025 Uiso 1 1 calc R . . C26 C 0.1857(2) 0.83464(16) 0.24371(16) 0.0163(6) Uani 1 1 d . A . H26A H 0.1542 0.8025 0.2694 0.020 Uiso 1 1 calc R . . H26B H 0.2508 0.8367 0.2616 0.020 Uiso 1 1 calc R . . C31 C 0.2068(2) 0.56773(16) 0.29591(15) 0.0153(6) Uani 1 1 d . . . H31 H 0.2163 0.5198 0.2957 0.018 Uiso 1 1 calc R A . C32 C 0.2680(3) 0.59393(19) 0.35399(17) 0.0220(7) Uani 1 1 d . A . H32A H 0.2581 0.6411 0.3580 0.026 Uiso 1 1 calc R . . H32B H 0.3332 0.5867 0.3471 0.026 Uiso 1 1 calc R . . C33 C 0.2459(3) 0.5601(2) 0.41664(19) 0.0320(9) Uani 1 1 d . . . H33A H 0.2604 0.5135 0.4138 0.038 Uiso 1 1 calc R A . H33B H 0.2849 0.5785 0.4539 0.038 Uiso 1 1 calc R . . C34 C 0.1459(3) 0.5682(2) 0.4280(2) 0.0361(10) Uani 1 1 d . A . H34A H 0.1330 0.6144 0.4358 0.043 Uiso 1 1 calc R . . H34B H 0.1329 0.5435 0.4671 0.043 Uiso 1 1 calc R . . C35 C 0.0828(3) 0.5440(2) 0.36907(19) 0.0315(9) Uani 1 1 d . . . H35A H 0.0910 0.4968 0.3639 0.038 Uiso 1 1 calc R A . H35B H 0.0180 0.5521 0.3765 0.038 Uiso 1 1 calc R . . C36 C 0.1052(3) 0.57874(19) 0.30709(18) 0.0215(7) Uani 1 1 d . A . H36A H 0.0933 0.6257 0.3110 0.026 Uiso 1 1 calc R . . H36B H 0.0653 0.5620 0.2695 0.026 Uiso 1 1 calc R . . C41 C 0.1738(2) 0.54448(15) 0.15494(15) 0.0126(6) Uani 1 1 d . . . H41 H 0.1146 0.5672 0.1418 0.015 Uiso 1 1 calc R A . C42 C 0.2214(2) 0.53694(17) 0.09240(17) 0.0175(7) Uani 1 1 d . A . H42A H 0.2766 0.5095 0.1008 0.021 Uiso 1 1 calc R . . H42B H 0.2410 0.5799 0.0776 0.021 Uiso 1 1 calc R . . C43 C 0.1546(3) 0.50582(19) 0.03961(17) 0.0210(7) Uani 1 1 d . . . H43A H 0.1013 0.5348 0.0297 0.025 Uiso 1 1 calc R A . H43B H 0.1857 0.5005 -0.0006 0.025 Uiso 1 1 calc R . . C44 C 0.1213(3) 0.44018(19) 0.06103(19) 0.0252(8) Uani 1 1 d . A . H44A H 0.1735 0.4095 0.0655 0.030 Uiso 1 1 calc R . . H44B H 0.0748 0.4231 0.0275 0.030 Uiso 1 1 calc R . . C45 C 0.0795(3) 0.44534(19) 0.12571(19) 0.0246(8) Uani 1 1 d . . . H45A H 0.0631 0.4016 0.1402 0.030 Uiso 1 1 calc R A . H45B H 0.0226 0.4714 0.1198 0.030 Uiso 1 1 calc R . . C46 C 0.1467(3) 0.47693(18) 0.17812(18) 0.0211(7) Uani 1 1 d . A . H46A H 0.2022 0.4497 0.1864 0.025 Uiso 1 1 calc R . . H46B H 0.1174 0.4808 0.2192 0.025 Uiso 1 1 calc R . . C51 C 0.5839(2) 0.75469(15) 0.32232(15) 0.0120(6) Uani 1 1 d . . . H51 H 0.5365 0.7279 0.3416 0.014 Uiso 1 1 calc R A . C52 C 0.6755(2) 0.73426(17) 0.35873(16) 0.0155(6) Uani 1 1 d . A . H52A H 0.7253 0.7629 0.3465 0.019 Uiso 1 1 calc R . . H52B H 0.6904 0.6893 0.3470 0.019 Uiso 1 1 calc R . . C53 C 0.6674(3) 0.73905(17) 0.43219(17) 0.0184(7) Uani 1 1 d . . . H53A H 0.6193 0.7088 0.4443 0.022 Uiso 1 1 calc R A . H53B H 0.7263 0.7261 0.4561 0.022 Uiso 1 1 calc R . . C54 C 0.6433(3) 0.80768(19) 0.45180(18) 0.0241(8) Uani 1 1 d . A . H54A H 0.6945 0.8372 0.4443 0.029 Uiso 1 1 calc R . . H54B H 0.6347 0.8087 0.4987 0.029 Uiso 1 1 calc R . . C55 C 0.5555(3) 0.83099(18) 0.41276(18) 0.0220(7) Uani 1 1 d . . . H55A H 0.5443 0.8767 0.4238 0.026 Uiso 1 1 calc R A . H55B H 0.5029 0.8051 0.4251 0.026 Uiso 1 1 calc R . . C56 C 0.5612(2) 0.82516(16) 0.33936(16) 0.0165(6) Uani 1 1 d . A . H56A H 0.6095 0.8544 0.3259 0.020 Uiso 1 1 calc R . . H56B H 0.5020 0.8380 0.3158 0.020 Uiso 1 1 calc R . . C61 C 0.6272(2) 0.80535(15) 0.19370(15) 0.0120(6) Uani 1 1 d . . . H61 H 0.6026 0.8477 0.2076 0.014 Uiso 1 1 calc R A . C62 C 0.6106(2) 0.80328(16) 0.11905(16) 0.0157(6) Uani 1 1 d . A . H62A H 0.6333 0.7617 0.1030 0.019 Uiso 1 1 calc R . . H62B H 0.5439 0.8061 0.1058 0.019 Uiso 1 1 calc R . . C63 C 0.6604(3) 0.85967(17) 0.08875(17) 0.0184(7) Uani 1 1 d . . . H63A H 0.6500 0.8571 0.0408 0.022 Uiso 1 1 calc R A . H63B H 0.6348 0.9012 0.1026 0.022 Uiso 1 1 calc R . . C64 C 0.7631(3) 0.85770(18) 0.10933(18) 0.0213(7) Uani 1 1 d . A . H64A H 0.7897 0.8176 0.0929 0.026 Uiso 1 1 calc R . . H64B H 0.7935 0.8951 0.0904 0.026 Uiso 1 1 calc R . . C65 C 0.7799(2) 0.85989(18) 0.18288(18) 0.0196(7) Uani 1 1 d . . . H65A H 0.7586 0.9021 0.1985 0.024 Uiso 1 1 calc R A . H65B H 0.8466 0.8565 0.1957 0.024 Uiso 1 1 calc R . . C66 C 0.7304(2) 0.80538(17) 0.21544(17) 0.0166(6) Uani 1 1 d . A . H66A H 0.7397 0.8107 0.2632 0.020 Uiso 1 1 calc R . . H66B H 0.7571 0.7633 0.2043 0.020 Uiso 1 1 calc R . . C71 C 0.6104(2) 0.54238(15) 0.15766(15) 0.0126(6) Uani 1 1 d . . . H71 H 0.6771 0.5536 0.1609 0.015 Uiso 1 1 calc R A . C72 C 0.5718(2) 0.56189(17) 0.08872(16) 0.0159(6) Uani 1 1 d . A . H72A H 0.5064 0.5492 0.0814 0.019 Uiso 1 1 calc R . . H72B H 0.5758 0.6094 0.0838 0.019 Uiso 1 1 calc R . . C73 C 0.6264(2) 0.52856(17) 0.03857(16) 0.0167(6) Uani 1 1 d . . . H73A H 0.5991 0.5398 -0.0056 0.020 Uiso 1 1 calc R A . H73B H 0.6903 0.5447 0.0433 0.020 Uiso 1 1 calc R . . C74 C 0.6269(2) 0.45503(17) 0.04644(16) 0.0166(6) Uani 1 1 d . A . H74A H 0.5640 0.4381 0.0359 0.020 Uiso 1 1 calc R . . H74B H 0.6671 0.4356 0.0157 0.020 Uiso 1 1 calc R . . C75 C 0.6613(3) 0.43593(17) 0.11555(17) 0.0185(7) Uani 1 1 d . . . H75A H 0.7268 0.4482 0.1241 0.022 Uiso 1 1 calc R A . H75B H 0.6569 0.3884 0.1202 0.022 Uiso 1 1 calc R . . C76 C 0.6060(3) 0.46876(16) 0.16587(16) 0.0173(6) Uani 1 1 d . A . H76A H 0.5413 0.4541 0.1598 0.021 Uiso 1 1 calc R . . H76B H 0.6316 0.4566 0.2102 0.021 Uiso 1 1 calc R . . C81 C 0.6005(2) 0.55197(16) 0.29825(16) 0.0150(6) Uani 1 1 d . . . H81 H 0.5800 0.5059 0.2936 0.018 Uiso 1 1 calc R A . C82 C 0.5554(2) 0.57867(17) 0.35668(17) 0.0176(6) Uani 1 1 d . A . H82A H 0.5721 0.6248 0.3631 0.021 Uiso 1 1 calc R . . H82B H 0.4878 0.5759 0.3480 0.021 Uiso 1 1 calc R . . C83 C 0.5864(3) 0.5406(2) 0.41830(18) 0.0252(8) Uani 1 1 d . . . H83A H 0.5646 0.4954 0.4134 0.030 Uiso 1 1 calc R A . H83B H 0.5589 0.5599 0.4557 0.030 Uiso 1 1 calc R . . C84 C 0.6911(3) 0.5412(2) 0.43133(18) 0.0267(8) Uani 1 1 d . A . H84A H 0.7127 0.5862 0.4389 0.032 Uiso 1 1 calc R . . H84B H 0.7098 0.5156 0.4709 0.032 Uiso 1 1 calc R . . C85 C 0.7351(3) 0.51260(18) 0.37368(18) 0.0225(7) Uani 1 1 d . . . H85A H 0.7170 0.4666 0.3683 0.027 Uiso 1 1 calc R A . H85B H 0.8028 0.5144 0.3824 0.027 Uiso 1 1 calc R . . C86 C 0.7058(2) 0.54945(16) 0.31102(17) 0.0169(6) Uani 1 1 d . A . H86A H 0.7317 0.5279 0.2741 0.020 Uiso 1 1 calc R . . H86B H 0.7305 0.5941 0.3144 0.020 Uiso 1 1 calc R . . Cl1S Cl 0.9314(2) 0.7428(3) 0.34303(17) 0.0805(13) Uani 0.622(5) 1 d PDU B 1 Cl2S Cl 0.9263(2) 0.67738(16) 0.46831(16) 0.0733(11) Uani 0.622(5) 1 d PDU B 1 Cl3S Cl 0.9608(8) 0.7591(5) 0.3171(6) 0.160(5) Uani 0.378(5) 1 d PDU B 2 Cl4S Cl 0.9092(5) 0.6607(3) 0.4043(4) 0.103(3) Uani 0.378(5) 1 d PDU B 2 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 Au1 0.01010(5) 0.00666(5) 0.01326(6) 0.00018(4) 0.00137(4) -0.00018(4) Rh1 0.00852(10) 0.00661(10) 0.01044(10) 0.00003(8) 0.00146(8) 0.00009(8) Br1 0.01152(19) 0.0133(2) 0.0108(2) -0.00086(16) 0.00254(16) -0.00042(14) C3 0.0119(18) 0.0127(19) 0.006(2) 0.0002(15) -0.0001(15) -0.0022(14) O1 0.018(2) 0.0181(18) 0.011(3) -0.005(2) 0.006(2) 0.0016(13) Br1A 0.0117(11) 0.0140(11) 0.0101(19) -0.0019(15) 0.0014(13) -0.0001(8) O1A 0.018(2) 0.0181(18) 0.011(3) -0.005(2) 0.006(2) 0.0016(13) P3 0.0102(4) 0.0092(3) 0.0118(3) 0.0009(3) 0.0022(3) 0.0005(3) P1S 0.0131(4) 0.0450(7) 0.0429(6) -0.0211(5) 0.0057(4) -0.0046(4) F1S 0.046(2) 0.116(3) 0.056(2) -0.026(2) 0.0269(16) -0.021(2) C1 0.0119(14) 0.0090(13) 0.0140(14) -0.0001(11) 0.0024(11) -0.0020(11) Br2 0.01182(14) 0.00759(13) 0.02452(16) 0.00148(11) 0.00174(11) 0.00025(11) P4 0.0121(4) 0.0083(3) 0.0122(3) 0.0002(3) 0.0018(3) -0.0013(3) F2S 0.0417(17) 0.0467(18) 0.076(2) -0.0239(17) 0.0112(16) -0.0096(14) C2 0.0120(14) 0.0102(14) 0.0171(15) -0.0001(11) 0.0025(11) 0.0003(11) Br3 0.01711(16) 0.00785(14) 0.03493(19) 0.00288(13) 0.00191(13) -0.00019(12) P1 0.0092(3) 0.0079(3) 0.0151(4) -0.0006(3) 0.0017(3) -0.0003(3) F3S 0.0413(18) 0.056(2) 0.095(3) -0.047(2) -0.0004(18) -0.0063(15) P2 0.0110(4) 0.0084(3) 0.0128(4) -0.0002(3) 0.0007(3) 0.0011(3) F4S 0.0243(14) 0.071(2) 0.0494(18) 0.0024(16) 0.0006(12) 0.0003(14) F5S 0.0263(14) 0.066(2) 0.0474(17) 0.0018(15) 0.0063(12) 0.0004(14) F6S 0.0159(13) 0.070(2) 0.091(3) -0.033(2) -0.0041(14) 0.0078(13) C1S 0.034(4) 0.057(5) 0.062(5) -0.001(4) -0.003(4) -0.002(4) C2S 0.043(8) 0.048(7) 0.069(8) -0.031(7) 0.014(7) 0.007(6) C3A 0.0119(18) 0.0127(19) 0.006(2) 0.0002(15) -0.0001(15) -0.0022(14) C11 0.0135(15) 0.0157(15) 0.0115(13) -0.0008(11) 0.0021(11) 0.0012(12) C12 0.0207(17) 0.0167(16) 0.0143(15) 0.0015(12) 0.0029(12) 0.0005(13) C13 0.033(2) 0.0250(19) 0.0151(16) 0.0043(14) 0.0066(14) -0.0008(16) C14 0.039(2) 0.033(2) 0.0137(16) 0.0002(15) -0.0008(15) -0.0022(18) C15 0.028(2) 0.0241(19) 0.0180(17) -0.0047(14) -0.0030(14) -0.0020(15) C16 0.0188(17) 0.0200(17) 0.0168(15) -0.0004(13) -0.0004(12) -0.0003(13) C21 0.0119(14) 0.0095(13) 0.0180(15) -0.0008(11) 0.0022(11) 0.0017(11) C22 0.0120(15) 0.0153(15) 0.0248(17) -0.0017(13) -0.0008(12) 0.0031(12) C23 0.0153(16) 0.0181(17) 0.032(2) -0.0010(15) -0.0029(14) 0.0079(13) C24 0.0184(17) 0.0218(18) 0.032(2) -0.0049(15) 0.0038(14) 0.0071(14) C25 0.0197(17) 0.0136(15) 0.0290(19) -0.0058(14) 0.0025(14) 0.0028(13) C26 0.0178(16) 0.0148(15) 0.0164(15) -0.0017(12) 0.0024(12) 0.0021(12) C31 0.0204(16) 0.0130(14) 0.0125(14) 0.0019(12) 0.0019(12) -0.0024(12) C32 0.0275(19) 0.0217(18) 0.0165(16) -0.0012(13) 0.0004(13) -0.0054(15) C33 0.049(3) 0.029(2) 0.0173(17) -0.0004(16) -0.0023(17) -0.0078(19) C34 0.053(3) 0.037(2) 0.0199(19) 0.0010(17) 0.0111(18) -0.015(2) C35 0.040(2) 0.033(2) 0.0227(19) 0.0009(16) 0.0119(17) -0.0163(19) C36 0.0212(18) 0.0235(18) 0.0208(17) 0.0019(14) 0.0073(13) -0.0052(14) C41 0.0149(15) 0.0094(13) 0.0135(14) -0.0027(11) 0.0013(11) -0.0033(11) C42 0.0190(16) 0.0154(16) 0.0187(16) -0.0041(13) 0.0043(12) -0.0023(12) C43 0.0215(18) 0.0241(18) 0.0181(16) -0.0066(14) 0.0046(13) -0.0041(14) C44 0.027(2) 0.0218(18) 0.0265(19) -0.0100(15) 0.0032(15) -0.0054(15) C45 0.028(2) 0.0198(18) 0.0258(18) -0.0054(15) 0.0026(15) -0.0094(15) C46 0.0266(19) 0.0160(16) 0.0209(17) -0.0025(13) 0.0026(14) -0.0116(14) C51 0.0135(14) 0.0093(13) 0.0131(14) 0.0009(11) 0.0005(11) 0.0008(11) C52 0.0147(15) 0.0158(15) 0.0159(15) -0.0002(12) 0.0002(12) 0.0025(12) C53 0.0199(17) 0.0186(16) 0.0161(15) 0.0015(13) -0.0021(12) 0.0014(13) C54 0.029(2) 0.0237(18) 0.0188(17) -0.0044(14) -0.0014(14) 0.0020(15) C55 0.029(2) 0.0177(17) 0.0199(17) -0.0027(13) 0.0032(14) 0.0071(14) C56 0.0210(17) 0.0125(15) 0.0159(15) 0.0011(12) 0.0007(12) 0.0047(12) C61 0.0116(14) 0.0094(13) 0.0153(14) 0.0003(11) 0.0030(11) -0.0028(11) C62 0.0161(15) 0.0157(15) 0.0153(15) -0.0017(12) 0.0018(12) -0.0022(12) C63 0.0240(18) 0.0159(16) 0.0157(15) 0.0010(12) 0.0043(13) -0.0031(13) C64 0.0236(18) 0.0191(17) 0.0224(17) 0.0026(14) 0.0093(14) -0.0044(14) C65 0.0133(15) 0.0211(17) 0.0246(17) 0.0019(14) 0.0023(13) -0.0059(13) C66 0.0113(15) 0.0188(16) 0.0196(16) 0.0031(13) 0.0012(12) -0.0022(12) C71 0.0128(14) 0.0111(14) 0.0136(14) -0.0015(11) 0.0006(11) 0.0009(11) C72 0.0172(16) 0.0152(15) 0.0152(15) 0.0015(12) 0.0005(12) 0.0026(12) C73 0.0183(16) 0.0173(16) 0.0149(15) 0.0017(12) 0.0038(12) 0.0013(13) C74 0.0186(16) 0.0166(16) 0.0150(15) -0.0033(12) 0.0034(12) -0.0017(12) C75 0.0269(18) 0.0118(15) 0.0170(15) -0.0020(12) 0.0026(13) 0.0036(13) C76 0.0251(18) 0.0109(14) 0.0161(15) 0.0004(12) 0.0029(13) 0.0013(13) C81 0.0177(16) 0.0131(14) 0.0141(14) 0.0010(12) 0.0011(12) 0.0013(12) C82 0.0187(16) 0.0166(16) 0.0180(16) 0.0007(13) 0.0039(12) -0.0006(13) C83 0.035(2) 0.0241(19) 0.0162(16) 0.0040(14) 0.0021(15) 0.0011(16) C84 0.037(2) 0.0246(19) 0.0170(17) 0.0022(14) -0.0057(15) 0.0048(16) C85 0.029(2) 0.0167(17) 0.0204(17) 0.0014(13) -0.0068(14) 0.0075(14) C86 0.0170(16) 0.0131(15) 0.0199(16) -0.0004(12) -0.0021(12) 0.0051(12) Cl1S 0.0410(15) 0.137(4) 0.0638(19) 0.025(2) 0.0054(12) 0.0136(18) Cl2S 0.0557(16) 0.089(2) 0.077(2) 0.0279(17) 0.0120(14) 0.0149(14) Cl3S 0.167(9) 0.171(8) 0.129(8) 0.071(7) -0.053(7) -0.090(7) Cl4S 0.103(5) 0.084(4) 0.121(6) 0.018(4) 0.001(4) 0.026(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P2 2.3730(8) . ? Au1 P4 2.3763(8) . ? Au1 Br3 2.5521(4) . ? Au1 Rh1 2.6960(3) . ? Rh1 C3A 1.812(13) . ? Rh1 C3 1.831(6) . ? Rh1 P3 2.4063(9) . ? Rh1 P1 2.4149(9) . ? Rh1 Br1 2.5092(6) . ? Rh1 Br1A 2.545(4) . ? Rh1 Br2 2.5484(4) . ? C3 O1 1.159(6) . ? O1A C3A 1.170(14) . ? P3 C1 1.837(3) . ? P3 C11 1.849(3) . ? P3 C21 1.861(3) . ? P1S F3S 1.588(3) . ? P1S F2S 1.591(3) . ? P1S F4S 1.600(3) . ? P1S F5S 1.601(3) . ? P1S F1S 1.601(4) . ? P1S F6S 1.603(3) . ? C1 P4 1.832(3) . ? P4 C31 1.842(3) . ? P4 C41 1.860(3) . ? C2 P2 1.825(3) . ? C2 P1 1.830(3) . ? P1 C51 1.849(3) . ? P1 C61 1.857(3) . ? P2 C81 1.842(3) . ? P2 C71 1.855(3) . ? C1S Cl1S 1.763(9) . ? C1S Cl2S 1.769(9) . ? C2S Cl3S 1.743(12) . ? C2S Cl4S 1.796(12) . ? C11 C16 1.536(5) . ? C11 C12 1.548(5) . ? C12 C13 1.528(5) . ? C13 C14 1.524(6) . ? C14 C15 1.535(6) . ? C15 C16 1.534(5) . ? C21 C26 1.532(5) . ? C21 C22 1.538(5) . ? C22 C23 1.531(5) . ? C23 C24 1.516(5) . ? C24 C25 1.522(5) . ? C25 C26 1.531(5) . ? C31 C32 1.528(5) . ? C31 C36 1.542(5) . ? C32 C33 1.533(5) . ? C33 C34 1.514(7) . ? C34 C35 1.540(6) . ? C35 C36 1.531(5) . ? C41 C42 1.534(5) . ? C41 C46 1.540(5) . ? C42 C43 1.535(5) . ? C43 C44 1.521(5) . ? C44 C45 1.526(5) . ? C45 C46 1.538(5) . ? C51 C52 1.533(4) . ? C51 C56 1.542(4) . ? C52 C53 1.538(5) . ? C53 C54 1.526(5) . ? C54 C55 1.529(5) . ? C55 C56 1.533(5) . ? C61 C66 1.534(4) . ? C61 C62 1.540(4) . ? C62 C63 1.539(5) . ? C63 C64 1.523(5) . ? C64 C65 1.518(5) . ? C65 C66 1.530(5) . ? C71 C76 1.533(5) . ? C71 C72 1.537(4) . ? C72 C73 1.531(5) . ? C73 C74 1.528(5) . ? C74 C75 1.522(5) . ? C75 C76 1.535(5) . ? C81 C82 1.533(5) . ? C81 C86 1.541(5) . ? C82 C83 1.529(5) . ? C83 C84 1.530(6) . ? C84 C85 1.526(6) . ? C85 C86 1.529(5) . ? 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 P2 Au1 P4 171.00(3) . . ? P2 Au1 Br3 87.31(2) . . ? P4 Au1 Br3 84.08(2) . . ? P2 Au1 Rh1 93.90(2) . . ? P4 Au1 Rh1 94.52(2) . . ? Br3 Au1 Rh1 175.929(11) . . ? C3A Rh1 C3 173.5(6) . . ? C3A Rh1 P3 87.4(5) . . ? C3 Rh1 P3 92.38(13) . . ? C3A Rh1 P1 91.2(5) . . ? C3 Rh1 P1 89.70(13) . . ? P3 Rh1 P1 173.33(3) . . ? C3A Rh1 Br1 3.1(5) . . ? C3 Rh1 Br1 170.49(13) . . ? P3 Rh1 Br1 87.85(2) . . ? P1 Rh1 Br1 91.15(2) . . ? C3A Rh1 Br1A 170.7(5) . . ? C3 Rh1 Br1A 2.86(15) . . ? P3 Rh1 Br1A 91.57(9) . . ? P1 Rh1 Br1A 90.81(9) . . ? Br1 Rh1 Br1A 167.73(9) . . ? C3A Rh1 Br2 91.2(5) . . ? C3 Rh1 Br2 95.27(13) . . ? P3 Rh1 Br2 87.21(2) . . ? P1 Rh1 Br2 86.29(2) . . ? Br1 Rh1 Br2 94.233(15) . . ? Br1A Rh1 Br2 97.98(9) . . ? C3A Rh1 Au1 88.5(5) . . ? C3 Rh1 Au1 85.03(13) . . ? P3 Rh1 Au1 92.33(2) . . ? P1 Rh1 Au1 94.17(2) . . ? Br1 Rh1 Au1 85.467(12) . . ? Br1A Rh1 Au1 82.31(9) . . ? Br2 Rh1 Au1 179.453(13) . . ? O1 C3 Rh1 177.4(6) . . ? C1 P3 C11 108.71(15) . . ? C1 P3 C21 103.77(14) . . ? C11 P3 C21 106.98(15) . . ? C1 P3 Rh1 109.90(11) . . ? C11 P3 Rh1 109.81(11) . . ? C21 P3 Rh1 117.26(11) . . ? F3S P1S F2S 179.8(2) . . ? F3S P1S F4S 89.90(18) . . ? F2S P1S F4S 90.23(19) . . ? F3S P1S F5S 90.3(2) . . ? F2S P1S F5S 89.78(19) . . ? F4S P1S F5S 89.01(16) . . ? F3S P1S F1S 90.9(2) . . ? F2S P1S F1S 89.0(2) . . ? F4S P1S F1S 90.2(2) . . ? F5S P1S F1S 178.5(2) . . ? F3S P1S F6S 90.56(19) . . ? F2S P1S F6S 89.31(18) . . ? F4S P1S F6S 179.1(2) . . ? F5S P1S F6S 90.21(19) . . ? F1S P1S F6S 90.5(2) . . ? P4 C1 P3 113.87(17) . . ? C1 P4 C31 104.85(15) . . ? C1 P4 C41 104.61(15) . . ? C31 P4 C41 105.59(15) . . ? C1 P4 Au1 114.15(10) . . ? C31 P4 Au1 110.59(11) . . ? C41 P4 Au1 116.09(11) . . ? P2 C2 P1 116.62(17) . . ? C2 P1 C51 107.75(15) . . ? C2 P1 C61 103.31(15) . . ? C51 P1 C61 107.12(15) . . ? C2 P1 Rh1 109.53(11) . . ? C51 P1 Rh1 112.78(11) . . ? C61 P1 Rh1 115.68(11) . . ? C2 P2 C81 108.66(15) . . ? C2 P2 C71 100.54(15) . . ? C81 P2 C71 104.86(15) . . ? C2 P2 Au1 114.93(11) . . ? C81 P2 Au1 108.91(11) . . ? C71 P2 Au1 118.11(11) . . ? Cl1S C1S Cl2S 112.1(6) . . ? Cl3S C2S Cl4S 108.3(8) . . ? O1A C3A Rh1 175.8(17) . . ? C16 C11 C12 110.2(3) . . ? C16 C11 P3 121.0(2) . . ? C12 C11 P3 109.5(2) . . ? C13 C12 C11 109.2(3) . . ? C14 C13 C12 111.3(3) . . ? C13 C14 C15 111.0(3) . . ? C16 C15 C14 111.6(3) . . ? C15 C16 C11 109.3(3) . . ? C26 C21 C22 110.4(3) . . ? C26 C21 P3 113.3(2) . . ? C22 C21 P3 113.7(2) . . ? C23 C22 C21 110.3(3) . . ? C24 C23 C22 111.9(3) . . ? C23 C24 C25 110.8(3) . . ? C24 C25 C26 111.9(3) . . ? C25 C26 C21 111.2(3) . . ? C32 C31 C36 109.4(3) . . ? C32 C31 P4 114.2(2) . . ? C36 C31 P4 113.3(2) . . ? C31 C32 C33 110.4(3) . . ? C34 C33 C32 111.4(4) . . ? C33 C34 C35 111.0(4) . . ? C36 C35 C34 110.5(3) . . ? C35 C36 C31 110.0(3) . . ? C42 C41 C46 108.7(3) . . ? C42 C41 P4 113.9(2) . . ? C46 C41 P4 116.6(2) . . ? C41 C42 C43 109.4(3) . . ? C44 C43 C42 111.5(3) . . ? C43 C44 C45 111.0(3) . . ? C44 C45 C46 111.4(3) . . ? C45 C46 C41 109.4(3) . . ? C52 C51 C56 110.2(3) . . ? C52 C51 P1 119.8(2) . . ? C56 C51 P1 110.5(2) . . ? C51 C52 C53 108.8(3) . . ? C54 C53 C52 111.3(3) . . ? C53 C54 C55 110.9(3) . . ? C54 C55 C56 112.1(3) . . ? C55 C56 C51 109.5(3) . . ? C66 C61 C62 110.6(3) . . ? C66 C61 P1 113.0(2) . . ? C62 C61 P1 112.9(2) . . ? C63 C62 C61 110.6(3) . . ? C64 C63 C62 111.0(3) . . ? C65 C64 C63 110.0(3) . . ? C64 C65 C66 112.4(3) . . ? C65 C66 C61 111.4(3) . . ? C76 C71 C72 110.3(3) . . ? C76 C71 P2 116.1(2) . . ? C72 C71 P2 112.0(2) . . ? C73 C72 C71 109.9(3) . . ? C74 C73 C72 111.9(3) . . ? C75 C74 C73 110.9(3) . . ? C74 C75 C76 111.9(3) . . ? C71 C76 C75 109.5(3) . . ? C82 C81 C86 112.0(3) . . ? C82 C81 P2 113.7(2) . . ? C86 C81 P2 113.2(2) . . ? C83 C82 C81 110.8(3) . . ? C82 C83 C84 110.9(3) . . ? C85 C84 C83 110.4(3) . . ? C84 C85 C86 111.3(3) . . ? C85 C86 C81 111.0(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.996 _refine_diff_density_min -1.010 _refine_diff_density_rms 0.149 #===END data_final _database_code_depnum_ccdc_archive 'CCDC 789600' #TrackingRef '- CIF final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H108 Au F6 O P5 Rh' _chemical_formula_weight 1486.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.5672(15) _cell_length_b 14.0811(15) _cell_length_c 19.974(2) _cell_angle_alpha 76.123(2) _cell_angle_beta 82.666(2) _cell_angle_gamma 66.756(2) _cell_volume 3401.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9631 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 30.58 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1530 _exptl_absorpt_coefficient_mu 2.570 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4263 _exptl_absorpt_correction_T_max 0.5659 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 78297 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 30.03 _reflns_number_total 19683 _reflns_number_gt 17598 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0189P)^2^+5.0590P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19683 _refine_ls_number_parameters 792 _refine_ls_number_restraints 371 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0723 _refine_ls_wR_factor_gt 0.0698 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.325 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.397937(16) 0.031855(10) 0.250798(6) 0.01568(5) Uani 0.9355(9) 1 d PDU A 1 Rh1 Rh 0.17196(4) 0.10676(3) 0.28085(2) 0.01725(7) Uani 0.9355(9) 1 d PDU A 1 H1 H 0.192(3) 0.124(3) 0.1967(18) 0.021 Uiso 1 1 d U B 1 C3 C 0.1284(3) 0.0976(3) 0.37485(18) 0.0270(7) Uani 1 1 d DU A 1 O1 O 0.0925(2) 0.0957(2) 0.43020(14) 0.0389(7) Uani 1 1 d U A 1 Au1A Au 0.2117(3) 0.0978(2) 0.26375(18) 0.0307(8) Uani 0.0645(9) 1 d PDU A 2 Rh1A Rh 0.4457(5) 0.0193(3) 0.2473(2) 0.01725(7) Uani 0.0645(9) 1 d PDU A 2 P1 P 0.17886(7) -0.05805(6) 0.27671(4) 0.01939(16) Uani 1 1 d D . . P2 P 0.40698(7) -0.12490(6) 0.32554(4) 0.01737(15) Uani 1 1 d D . . P3 P 0.16611(7) 0.27695(6) 0.25762(4) 0.01980(16) Uani 1 1 d D . . P4 P 0.39174(7) 0.19095(6) 0.18045(4) 0.01901(16) Uani 1 1 d D . . C1 C 0.3025(2) -0.1689(2) 0.31138(16) 0.0193(6) Uani 1 1 d D A . H1A H 0.2840 -0.2091 0.3556 0.023 Uiso 1 1 calc R . . H1B H 0.3311 -0.2172 0.2787 0.023 Uiso 1 1 calc R . . C2 C 0.2843(3) 0.3015(2) 0.21148(18) 0.0241(7) Uani 1 1 d D A . H2A H 0.2583 0.3604 0.1713 0.029 Uiso 1 1 calc R . . H2B H 0.3162 0.3258 0.2427 0.029 Uiso 1 1 calc R . . P1S P 0.39961(8) -0.47045(7) 0.27430(5) 0.02609(18) Uani 1 1 d . . . F1S F 0.28226(19) -0.4376(2) 0.31065(13) 0.0443(6) Uani 1 1 d . . . F2S F 0.3639(2) -0.52262(19) 0.22357(13) 0.0434(6) Uani 1 1 d . . . F3S F 0.4375(2) -0.58069(17) 0.32875(12) 0.0417(6) Uani 1 1 d . . . F4S F 0.51689(19) -0.50237(18) 0.23792(12) 0.0395(5) Uani 1 1 d . . . F5S F 0.36086(18) -0.35949(16) 0.21964(11) 0.0325(5) Uani 1 1 d . . . F6S F 0.43493(19) -0.41780(16) 0.32491(11) 0.0332(5) Uani 1 1 d . . . C11 C 0.1767(3) -0.0877(3) 0.19167(16) 0.0243(7) Uani 1 1 d . A . H11 H 0.1796 -0.1616 0.2001 0.029 Uiso 1 1 calc R . . C12 C 0.0729(3) -0.0147(3) 0.15335(18) 0.0324(8) Uani 1 1 d . . . H12A H 0.0101 -0.0210 0.1824 0.039 Uiso 1 1 calc R A . H12B H 0.0667 0.0596 0.1452 0.039 Uiso 1 1 calc R . . C13 C 0.0731(3) -0.0437(4) 0.0846(2) 0.0428(10) Uani 1 1 d . A . H13A H 0.0079 0.0071 0.0599 0.051 Uiso 1 1 calc R . . H13B H 0.0704 -0.1149 0.0933 0.051 Uiso 1 1 calc R . . C14 C 0.1721(4) -0.0432(4) 0.0389(2) 0.0455(11) Uani 1 1 d . . . H14A H 0.1716 -0.0680 -0.0034 0.055 Uiso 1 1 calc R A . H14B H 0.1702 0.0299 0.0249 0.055 Uiso 1 1 calc R . . C15 C 0.2742(3) -0.1143(4) 0.07710(19) 0.0370(9) Uani 1 1 d . A . H15A H 0.3373 -0.1091 0.0478 0.044 Uiso 1 1 calc R . . H15B H 0.2801 -0.1886 0.0864 0.044 Uiso 1 1 calc R . . C16 C 0.2744(3) -0.0830(3) 0.14519(17) 0.0265(7) Uani 1 1 d . . . H16A H 0.2736 -0.0104 0.1356 0.032 Uiso 1 1 calc R A . H16B H 0.3409 -0.1313 0.1694 0.032 Uiso 1 1 calc R . . C21 C 0.0725(3) -0.0946(3) 0.33168(17) 0.0223(6) Uani 1 1 d . A . H21 H 0.0944 -0.1118 0.3804 0.027 Uiso 1 1 calc R . . C22 C -0.0370(3) -0.0015(3) 0.32700(18) 0.0278(7) Uani 1 1 d . . . H22A H -0.0287 0.0602 0.3374 0.033 Uiso 1 1 calc R A . H22B H -0.0624 0.0186 0.2794 0.033 Uiso 1 1 calc R . . C23 C -0.1197(3) -0.0307(3) 0.37740(19) 0.0330(8) Uani 1 1 d . A . H23A H -0.0973 -0.0447 0.4252 0.040 Uiso 1 1 calc R . . H23B H -0.1898 0.0295 0.3721 0.040 Uiso 1 1 calc R . . C24 C -0.1318(3) -0.1279(3) 0.3650(2) 0.0344(9) Uani 1 1 d . . . H24A H -0.1836 -0.1469 0.3997 0.041 Uiso 1 1 calc R A . H24B H -0.1606 -0.1119 0.3187 0.041 Uiso 1 1 calc R . . C25 C -0.0245(3) -0.2208(3) 0.3697(2) 0.0333(8) Uani 1 1 d . A . H25A H -0.0337 -0.2816 0.3587 0.040 Uiso 1 1 calc R . . H25B H 0.0002 -0.2418 0.4176 0.040 Uiso 1 1 calc R . . C26 C 0.0609(3) -0.1928(3) 0.31984(18) 0.0263(7) Uani 1 1 d . . . H26A H 0.1308 -0.2531 0.3265 0.032 Uiso 1 1 calc R A . H26B H 0.0405 -0.1802 0.2717 0.032 Uiso 1 1 calc R . . C31 C 0.3754(3) -0.1071(3) 0.41567(15) 0.0214(6) Uani 1 1 d . A . H31 H 0.2953 -0.0798 0.4210 0.026 Uiso 1 1 calc R . . C32 C 0.4076(3) -0.0217(3) 0.42938(17) 0.0265(7) Uani 1 1 d . . . H32A H 0.3769 0.0440 0.3943 0.032 Uiso 1 1 calc R A . H32B H 0.4868 -0.0447 0.4259 0.032 Uiso 1 1 calc R . . C33 C 0.3666(3) -0.0005(3) 0.50158(17) 0.0274(7) Uani 1 1 d . A . H33A H 0.3893 0.0540 0.5105 0.033 Uiso 1 1 calc R . . H33B H 0.2872 0.0270 0.5039 0.033 Uiso 1 1 calc R . . C34 C 0.4101(3) -0.1010(3) 0.55672(17) 0.0299(8) Uani 1 1 d . . . H34A H 0.4893 -0.1257 0.5567 0.036 Uiso 1 1 calc R A . H34B H 0.3811 -0.0857 0.6027 0.036 Uiso 1 1 calc R . . C35 C 0.3791(3) -0.1866(3) 0.54357(18) 0.0315(8) Uani 1 1 d . A . H35A H 0.3001 -0.1646 0.5487 0.038 Uiso 1 1 calc R . . H35B H 0.4114 -0.2520 0.5786 0.038 Uiso 1 1 calc R . . C36 C 0.4163(3) -0.2102(3) 0.47097(17) 0.0263(7) Uani 1 1 d . . . H36A H 0.3881 -0.2613 0.4628 0.032 Uiso 1 1 calc R A . H36B H 0.4956 -0.2422 0.4678 0.032 Uiso 1 1 calc R . . C41 C 0.5344(2) -0.2371(2) 0.32231(16) 0.0188(6) Uani 1 1 d . A . H41 H 0.5282 -0.3005 0.3552 0.023 Uiso 1 1 calc R . . C42 C 0.6288(3) -0.2169(3) 0.34367(18) 0.0255(7) Uani 1 1 d . . . H42A H 0.6350 -0.1531 0.3125 0.031 Uiso 1 1 calc R A . H42B H 0.6150 -0.2043 0.3913 0.031 Uiso 1 1 calc R . . C43 C 0.7340(3) -0.3120(3) 0.3401(2) 0.0319(8) Uani 1 1 d . A . H43A H 0.7940 -0.2969 0.3524 0.038 Uiso 1 1 calc R . . H43B H 0.7297 -0.3745 0.3741 0.038 Uiso 1 1 calc R . . C44 C 0.7563(3) -0.3367(3) 0.2681(2) 0.0343(8) Uani 1 1 d . . . H44A H 0.8225 -0.4006 0.2679 0.041 Uiso 1 1 calc R A . H44B H 0.7679 -0.2771 0.2348 0.041 Uiso 1 1 calc R . . C45 C 0.6627(3) -0.3548(3) 0.24576(18) 0.0268(7) Uani 1 1 d . A . H45A H 0.6771 -0.3664 0.1979 0.032 Uiso 1 1 calc R . . H45B H 0.6562 -0.4190 0.2761 0.032 Uiso 1 1 calc R . . C46 C 0.5577(3) -0.2609(3) 0.24931(16) 0.0226(6) Uani 1 1 d . . . H46A H 0.4982 -0.2762 0.2365 0.027 Uiso 1 1 calc R A . H46B H 0.5617 -0.1980 0.2158 0.027 Uiso 1 1 calc R . . C51 C 0.0483(3) 0.3663(3) 0.20491(17) 0.0225(6) Uani 1 1 d . A . H51 H 0.0315 0.4405 0.2093 0.027 Uiso 1 1 calc R . . C52 C 0.0662(3) 0.3618(3) 0.12828(17) 0.0277(7) Uani 1 1 d . . . H52A H 0.0904 0.2875 0.1235 0.033 Uiso 1 1 calc R A . H52B H 0.1235 0.3882 0.1082 0.033 Uiso 1 1 calc R . . C54 C -0.1276(3) 0.3924(3) 0.1189(2) 0.0344(8) Uani 1 1 d . . . H54A H -0.1083 0.3183 0.1152 0.041 Uiso 1 1 calc R A . H54B H -0.1932 0.4369 0.0927 0.041 Uiso 1 1 calc R . . C53 C -0.0365(3) 0.4283(3) 0.08832(19) 0.0336(8) Uani 1 1 d . A . H53A H -0.0575 0.5036 0.0898 0.040 Uiso 1 1 calc R . . H53B H -0.0227 0.4217 0.0394 0.040 Uiso 1 1 calc R . . C55 C -0.1494(3) 0.4007(3) 0.1944(2) 0.0352(9) Uani 1 1 d . A . H55A H -0.2072 0.3749 0.2141 0.042 Uiso 1 1 calc R . . H55B H -0.1738 0.4756 0.1978 0.042 Uiso 1 1 calc R . . C56 C -0.0481(3) 0.3355(3) 0.23527(19) 0.0303(8) Uani 1 1 d . . . H56A H -0.0289 0.2598 0.2360 0.036 Uiso 1 1 calc R A . H56B H -0.0630 0.3452 0.2835 0.036 Uiso 1 1 calc R . . C61 C 0.1605(5) 0.3488(5) 0.3272(3) 0.0198(12) Uani 0.646(6) 1 d PDU A 1 H61 H 0.1744 0.4140 0.3045 0.024 Uiso 0.646(6) 1 calc PR A 1 C62 C 0.0516(4) 0.3836(4) 0.3660(3) 0.0271(12) Uani 0.646(6) 1 d PDU A 1 H62A H -0.0043 0.4332 0.3333 0.032 Uiso 0.646(6) 1 calc PR A 1 H62B H 0.0328 0.3212 0.3862 0.032 Uiso 0.646(6) 1 calc PR A 1 C63 C 0.0537(5) 0.4375(5) 0.4235(3) 0.0336(14) Uani 0.646(6) 1 d PDU A 1 H63A H 0.0633 0.5048 0.4027 0.040 Uiso 0.646(6) 1 calc PR A 1 H63B H -0.0160 0.4544 0.4497 0.040 Uiso 0.646(6) 1 calc PR A 1 C64 C 0.1438(5) 0.3682(5) 0.4729(3) 0.0343(14) Uani 0.646(6) 1 d PDU A 1 H64A H 0.1450 0.4076 0.5075 0.041 Uiso 0.646(6) 1 calc PR A 1 H64B H 0.1299 0.3046 0.4977 0.041 Uiso 0.646(6) 1 calc PR A 1 C65 C 0.2515(4) 0.3350(4) 0.4347(3) 0.0279(13) Uani 0.646(6) 1 d PDU A 1 H65A H 0.3076 0.2864 0.4676 0.034 Uiso 0.646(6) 1 calc PR A 1 H65B H 0.2691 0.3980 0.4143 0.034 Uiso 0.646(6) 1 calc PR A 1 C66 C 0.2508(7) 0.2801(6) 0.3778(4) 0.0210(16) Uani 0.646(6) 1 d PDU A 1 H66A H 0.2416 0.2128 0.3988 0.025 Uiso 0.646(6) 1 calc PR A 1 H66B H 0.3208 0.2633 0.3520 0.025 Uiso 0.646(6) 1 calc PR A 1 C61A C 0.1395(10) 0.3227(8) 0.3401(5) 0.020(2) Uani 0.354(6) 1 d PDU A 2 H61A H 0.0756 0.3083 0.3634 0.024 Uiso 0.354(6) 1 calc PR A 2 C62A C 0.1130(9) 0.4402(7) 0.3317(5) 0.027(2) Uani 0.354(6) 1 d PDU A 2 H62C H 0.0499 0.4804 0.3025 0.032 Uiso 0.354(6) 1 calc PR A 2 H62D H 0.1743 0.4574 0.3079 0.032 Uiso 0.354(6) 1 calc PR A 2 C63A C 0.0888(11) 0.4741(8) 0.4016(6) 0.039(3) Uani 0.354(6) 1 d PDU A 2 H63C H 0.0766 0.5498 0.3943 0.047 Uiso 0.354(6) 1 calc PR A 2 H63D H 0.0227 0.4644 0.4233 0.047 Uiso 0.354(6) 1 calc PR A 2 C64A C 0.1823(10) 0.4084(8) 0.4492(6) 0.038(3) Uani 0.354(6) 1 d PDU A 2 H64C H 0.2462 0.4249 0.4302 0.046 Uiso 0.354(6) 1 calc PR A 2 H64D H 0.1633 0.4270 0.4952 0.046 Uiso 0.354(6) 1 calc PR A 2 C65A C 0.2084(9) 0.2924(7) 0.4565(5) 0.029(2) Uani 0.354(6) 1 d PDU A 2 H65C H 0.1468 0.2752 0.4798 0.035 Uiso 0.354(6) 1 calc PR A 2 H65D H 0.2712 0.2517 0.4859 0.035 Uiso 0.354(6) 1 calc PR A 2 C66A C 0.2329(12) 0.2592(11) 0.3876(6) 0.021(3) Uani 0.354(6) 1 d PDU A 2 H66C H 0.2468 0.1831 0.3949 0.025 Uiso 0.354(6) 1 calc PR A 2 H66D H 0.2983 0.2703 0.3658 0.025 Uiso 0.354(6) 1 calc PR A 2 C71 C 0.3538(3) 0.2075(2) 0.09211(16) 0.0217(6) Uani 1 1 d . A . H71 H 0.2762 0.2173 0.0961 0.026 Uiso 1 1 calc R . . C72 C 0.4112(3) 0.1101(3) 0.06002(18) 0.0275(7) Uani 1 1 d . . . H72A H 0.4878 0.0995 0.0504 0.033 Uiso 1 1 calc R A . H72B H 0.4072 0.0466 0.0927 0.033 Uiso 1 1 calc R . . C73 C 0.3585(3) 0.1255(3) -0.00711(18) 0.0323(8) Uani 1 1 d . A . H73A H 0.3966 0.0629 -0.0280 0.039 Uiso 1 1 calc R . . H73B H 0.2830 0.1319 0.0031 0.039 Uiso 1 1 calc R . . C74 C 0.3613(3) 0.2240(3) -0.05802(19) 0.0364(9) Uani 1 1 d . . . H74A H 0.4368 0.2141 -0.0721 0.044 Uiso 1 1 calc R A . H74B H 0.3230 0.2343 -0.0998 0.044 Uiso 1 1 calc R . . C75 C 0.3096(3) 0.3216(3) -0.02675(19) 0.0342(8) Uani 1 1 d . A . H75A H 0.2317 0.3373 -0.0189 0.041 Uiso 1 1 calc R . . H75B H 0.3186 0.3827 -0.0598 0.041 Uiso 1 1 calc R . . C76 C 0.3587(3) 0.3073(3) 0.04182(18) 0.0269(7) Uani 1 1 d . . . H76A H 0.3187 0.3699 0.0624 0.032 Uiso 1 1 calc R A . H76B H 0.4343 0.3011 0.0334 0.032 Uiso 1 1 calc R . . C81 C 0.5131(3) 0.2210(3) 0.17744(17) 0.0227(6) Uani 1 1 d . A . H81 H 0.4970 0.2959 0.1528 0.027 Uiso 1 1 calc R . . C82 C 0.5441(3) 0.2076(3) 0.25175(17) 0.0264(7) Uani 1 1 d . . . H82A H 0.4846 0.2573 0.2754 0.032 Uiso 1 1 calc R A . H82B H 0.5555 0.1349 0.2775 0.032 Uiso 1 1 calc R . . C83 C 0.6467(3) 0.2288(3) 0.25194(19) 0.0295(7) Uani 1 1 d . A . H83A H 0.6337 0.3031 0.2291 0.035 Uiso 1 1 calc R . . H83B H 0.6657 0.2181 0.3002 0.035 Uiso 1 1 calc R . . C84 C 0.7395(3) 0.1552(3) 0.2144(2) 0.0326(8) Uani 1 1 d . . . H84A H 0.8037 0.1726 0.2131 0.039 Uiso 1 1 calc R A . H84B H 0.7571 0.0813 0.2400 0.039 Uiso 1 1 calc R . . C85 C 0.7113(3) 0.1650(4) 0.1410(2) 0.0393(10) Uani 1 1 d . A . H85A H 0.7707 0.1124 0.1193 0.047 Uiso 1 1 calc R . . H85B H 0.7033 0.2362 0.1138 0.047 Uiso 1 1 calc R . . C86 C 0.6071(3) 0.1476(3) 0.1389(2) 0.0322(8) Uani 1 1 d . . . H86A H 0.6184 0.0731 0.1602 0.039 Uiso 1 1 calc R A . H86B H 0.5886 0.1609 0.0903 0.039 Uiso 1 1 calc R . . C1S C 0.8315(4) -0.6797(5) 0.4721(3) 0.0609(15) Uani 1 1 d . . . H1S H 0.9016 -0.7308 0.4822 0.073 Uiso 1 1 calc R . . C2S C 0.7860(4) -0.6679(5) 0.4105(2) 0.0552(13) Uani 1 1 d . . . H2S H 0.8249 -0.7107 0.3784 0.066 Uiso 1 1 calc R . . C3S C 0.6839(4) -0.5936(4) 0.3965(2) 0.0518(13) Uani 1 1 d . . . H3S H 0.6529 -0.5848 0.3543 0.062 Uiso 1 1 calc R . . C4S C 0.6268(4) -0.5324(4) 0.4431(2) 0.0487(12) Uani 1 1 d . . . H4S H 0.5560 -0.4826 0.4334 0.058 Uiso 1 1 calc R . . C5S C 0.6722(4) -0.5429(4) 0.5043(2) 0.0472(11) Uani 1 1 d . . . H5S H 0.6334 -0.4996 0.5362 0.057 Uiso 1 1 calc R . . C6S C 0.7750(4) -0.6174(5) 0.5184(2) 0.0556(13) Uani 1 1 d . . . H6S H 0.8064 -0.6254 0.5603 0.067 Uiso 1 1 calc R . . C7S C -0.0056(4) 0.7215(4) 0.0558(3) 0.0536(13) Uani 1 1 d . . . H7S H -0.0399 0.7454 0.0130 0.064 Uiso 1 1 calc R . . C8S C -0.0639(4) 0.7481(5) 0.1142(3) 0.0544(13) Uani 1 1 d . . . H8S H -0.1386 0.7895 0.1124 0.065 Uiso 1 1 calc R . . C9S C -0.0126(4) 0.7142(5) 0.1761(2) 0.0551(14) Uani 1 1 d . . . H9S H -0.0525 0.7329 0.2169 0.066 Uiso 1 1 calc R . . C10S C 0.0950(4) 0.6539(4) 0.1792(2) 0.0488(12) Uani 1 1 d . . . H10S H 0.1292 0.6310 0.2220 0.059 Uiso 1 1 calc R . . C11S C 0.1539(4) 0.6262(4) 0.1208(3) 0.0504(12) Uani 1 1 d . . . H11S H 0.2286 0.5845 0.1228 0.060 Uiso 1 1 calc R . . C12S C 0.1023(4) 0.6602(5) 0.0588(3) 0.0559(13) Uani 1 1 d . . . H12S H 0.1418 0.6411 0.0180 0.067 Uiso 1 1 calc R . . C13S C 0.4606(4) -0.4528(4) 0.0563(2) 0.0454(11) Uani 1 1 d . . . H13S H 0.4332 -0.4201 0.0948 0.054 Uiso 1 1 calc R . . C14S C 0.5588(4) -0.5342(4) 0.0588(2) 0.0453(11) Uani 1 1 d . . . H14S H 0.5997 -0.5580 0.0990 0.054 Uiso 1 1 calc R . . C15S C 0.5986(4) -0.5818(4) 0.0027(2) 0.0496(12) Uani 1 1 d . . . H15S H 0.6667 -0.6383 0.0045 0.060 Uiso 1 1 calc R . . 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 Au1 0.01554(10) 0.01592(6) 0.01483(6) -0.00295(4) -0.00078(5) -0.00523(5) Rh1 0.01518(17) 0.01821(13) 0.01605(16) -0.00255(11) 0.00049(13) -0.00480(13) C3 0.0260(17) 0.0271(17) 0.0273(17) -0.0046(13) 0.0005(14) -0.0106(14) O1 0.0454(17) 0.0434(16) 0.0255(13) -0.0069(11) 0.0066(12) -0.0167(13) Au1A 0.0247(16) 0.0309(13) 0.0361(17) -0.0110(10) 0.0083(12) -0.0107(12) Rh1A 0.01518(17) 0.01821(13) 0.01605(16) -0.00255(11) 0.00049(13) -0.00480(13) P1 0.0200(4) 0.0222(4) 0.0160(4) -0.0017(3) -0.0025(3) -0.0087(3) P2 0.0205(4) 0.0173(4) 0.0145(3) -0.0025(3) -0.0029(3) -0.0072(3) P3 0.0196(4) 0.0196(4) 0.0185(4) -0.0069(3) 0.0001(3) -0.0042(3) P4 0.0196(4) 0.0162(4) 0.0193(4) -0.0024(3) 0.0000(3) -0.0057(3) C1 0.0194(14) 0.0198(14) 0.0200(14) -0.0039(11) -0.0034(12) -0.0082(12) C2 0.0217(16) 0.0194(15) 0.0308(17) -0.0075(12) -0.0006(13) -0.0061(12) P1S 0.0315(5) 0.0232(4) 0.0271(4) -0.0039(3) -0.0055(4) -0.0135(4) F1S 0.0328(13) 0.0568(16) 0.0416(14) -0.0050(11) 0.0006(11) -0.0186(12) F2S 0.0647(17) 0.0389(13) 0.0424(13) -0.0087(10) -0.0140(12) -0.0323(12) F3S 0.0591(16) 0.0253(11) 0.0400(13) 0.0029(9) -0.0090(11) -0.0188(11) F4S 0.0355(13) 0.0376(13) 0.0437(14) -0.0116(10) 0.0036(11) -0.0119(10) F5S 0.0452(13) 0.0259(10) 0.0274(11) -0.0018(8) -0.0115(9) -0.0136(9) F6S 0.0454(13) 0.0285(11) 0.0288(11) -0.0049(8) -0.0128(10) -0.0144(10) C11 0.0247(16) 0.0312(17) 0.0193(15) -0.0045(12) -0.0022(13) -0.0132(14) C12 0.0266(18) 0.049(2) 0.0197(16) -0.0028(15) -0.0061(14) -0.0132(16) C13 0.035(2) 0.074(3) 0.0244(18) -0.0114(19) -0.0063(16) -0.024(2) C14 0.044(2) 0.076(3) 0.0199(18) -0.0111(19) -0.0035(17) -0.025(2) C15 0.037(2) 0.058(3) 0.0211(17) -0.0160(17) 0.0042(15) -0.0206(19) C16 0.0253(17) 0.0359(19) 0.0201(15) -0.0056(13) 0.0001(13) -0.0139(14) C21 0.0204(15) 0.0260(16) 0.0195(15) -0.0025(12) -0.0014(12) -0.0090(13) C22 0.0194(16) 0.0327(18) 0.0264(17) -0.0033(14) 0.0016(13) -0.0070(14) C23 0.0205(17) 0.045(2) 0.0269(18) -0.0032(15) 0.0018(14) -0.0082(15) C24 0.0235(18) 0.048(2) 0.0292(18) 0.0018(16) 0.0006(15) -0.0166(16) C25 0.0254(18) 0.039(2) 0.035(2) 0.0009(16) -0.0013(15) -0.0166(16) C26 0.0234(16) 0.0303(17) 0.0268(17) -0.0033(13) -0.0019(13) -0.0131(14) C31 0.0266(16) 0.0237(15) 0.0143(13) -0.0041(11) -0.0010(12) -0.0098(13) C32 0.0309(18) 0.0297(17) 0.0220(16) -0.0067(13) -0.0019(14) -0.0135(14) C33 0.0309(18) 0.0310(18) 0.0205(16) -0.0068(13) -0.0012(14) -0.0110(15) C34 0.0327(19) 0.039(2) 0.0163(15) -0.0053(14) -0.0006(14) -0.0121(16) C35 0.039(2) 0.036(2) 0.0195(16) -0.0006(14) -0.0011(15) -0.0171(17) C36 0.0338(19) 0.0260(16) 0.0186(15) -0.0004(12) -0.0038(13) -0.0125(14) C41 0.0180(14) 0.0218(15) 0.0178(14) -0.0011(11) -0.0014(11) -0.0102(12) C42 0.0231(16) 0.0308(17) 0.0267(17) -0.0045(13) -0.0036(13) -0.0143(14) C43 0.0227(17) 0.036(2) 0.039(2) -0.0048(16) -0.0085(15) -0.0120(15) C44 0.0206(17) 0.038(2) 0.041(2) -0.0067(16) 0.0012(15) -0.0094(15) C45 0.0231(16) 0.0292(17) 0.0245(16) -0.0043(13) 0.0003(13) -0.0073(14) C46 0.0214(15) 0.0245(16) 0.0208(15) -0.0025(12) -0.0021(12) -0.0085(13) C51 0.0208(15) 0.0195(15) 0.0254(16) -0.0058(12) -0.0040(13) -0.0040(12) C52 0.0230(16) 0.0337(18) 0.0229(16) -0.0034(13) -0.0025(13) -0.0080(14) C54 0.0271(18) 0.035(2) 0.039(2) -0.0052(16) -0.0117(16) -0.0070(15) C53 0.033(2) 0.035(2) 0.0280(18) -0.0010(15) -0.0092(15) -0.0099(16) C55 0.0186(16) 0.041(2) 0.041(2) -0.0106(17) -0.0029(15) -0.0044(15) C56 0.0222(17) 0.037(2) 0.0296(18) -0.0041(15) -0.0043(14) -0.0097(15) C61 0.023(3) 0.022(3) 0.018(3) -0.007(2) 0.001(2) -0.011(2) C62 0.023(3) 0.028(3) 0.028(3) -0.010(2) 0.002(2) -0.007(2) C63 0.035(3) 0.030(3) 0.032(3) -0.017(3) 0.006(3) -0.005(3) C64 0.045(4) 0.038(3) 0.022(3) -0.012(2) 0.001(2) -0.016(3) C65 0.031(3) 0.031(3) 0.026(3) -0.006(2) -0.005(2) -0.014(2) C66 0.023(3) 0.021(4) 0.023(3) -0.005(2) -0.002(2) -0.012(2) C61A 0.025(6) 0.017(5) 0.021(5) -0.005(4) 0.005(4) -0.012(4) C62A 0.035(5) 0.021(4) 0.025(4) -0.010(3) 0.001(4) -0.009(4) C63A 0.060(8) 0.024(5) 0.031(6) -0.019(4) 0.003(5) -0.006(5) C64A 0.059(8) 0.037(6) 0.025(5) -0.014(4) 0.004(5) -0.023(5) C65A 0.036(6) 0.034(5) 0.020(4) -0.003(4) 0.003(4) -0.018(4) C66A 0.025(7) 0.015(5) 0.026(6) -0.008(4) 0.002(4) -0.009(4) C71 0.0227(16) 0.0204(15) 0.0188(14) -0.0023(11) -0.0019(12) -0.0055(12) C72 0.0268(17) 0.0263(17) 0.0234(16) -0.0058(13) -0.0008(14) -0.0033(14) C73 0.035(2) 0.0347(19) 0.0239(17) -0.0096(14) -0.0017(15) -0.0079(16) C74 0.035(2) 0.047(2) 0.0225(17) -0.0014(16) -0.0022(15) -0.0131(18) C75 0.035(2) 0.0332(19) 0.0263(18) 0.0083(14) -0.0084(15) -0.0098(16) C76 0.0256(17) 0.0251(16) 0.0260(17) 0.0026(13) -0.0042(14) -0.0090(13) C81 0.0194(15) 0.0225(15) 0.0230(15) 0.0011(12) -0.0031(12) -0.0072(12) C82 0.0271(17) 0.0300(17) 0.0226(16) -0.0039(13) -0.0009(13) -0.0122(14) C83 0.0286(18) 0.0317(18) 0.0298(18) -0.0046(14) -0.0045(15) -0.0131(15) C84 0.0207(17) 0.038(2) 0.036(2) -0.0051(16) -0.0088(15) -0.0075(15) C85 0.0197(17) 0.058(3) 0.034(2) -0.0089(18) -0.0012(15) -0.0079(17) C86 0.0225(17) 0.042(2) 0.0295(18) -0.0109(16) -0.0007(14) -0.0079(15) C1S 0.039(3) 0.098(4) 0.045(3) -0.007(3) -0.001(2) -0.030(3) C2S 0.062(3) 0.086(4) 0.031(2) -0.005(2) 0.009(2) -0.049(3) C3S 0.072(3) 0.069(3) 0.029(2) 0.017(2) -0.017(2) -0.053(3) C4S 0.054(3) 0.049(3) 0.047(3) 0.018(2) -0.023(2) -0.033(2) C5S 0.050(3) 0.057(3) 0.037(2) 0.005(2) -0.008(2) -0.028(2) C6S 0.047(3) 0.091(4) 0.033(2) -0.003(2) -0.010(2) -0.033(3) C7S 0.046(3) 0.081(4) 0.042(3) -0.018(2) -0.010(2) -0.026(3) C8S 0.035(2) 0.092(4) 0.053(3) -0.027(3) -0.001(2) -0.035(3) C9S 0.046(3) 0.106(4) 0.040(2) -0.028(3) 0.012(2) -0.052(3) C10S 0.053(3) 0.071(3) 0.039(2) -0.003(2) -0.008(2) -0.044(3) C11S 0.045(3) 0.061(3) 0.052(3) -0.018(2) -0.011(2) -0.021(2) C12S 0.048(3) 0.083(4) 0.043(3) -0.029(3) -0.002(2) -0.023(3) C13S 0.054(3) 0.053(3) 0.031(2) -0.0030(19) 0.0053(19) -0.028(2) C14S 0.049(3) 0.059(3) 0.031(2) 0.0077(19) -0.0068(19) -0.032(2) C15S 0.046(3) 0.054(3) 0.039(2) 0.005(2) 0.001(2) -0.018(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P2 2.3170(8) . ? Au1 P4 2.3177(8) . ? Au1 Rh1 2.8556(5) . ? Rh1 C3 1.885(4) . ? Rh1 P3 2.3002(9) . ? Rh1 P1 2.3066(9) . ? Rh1 H1 1.64(4) . ? C3 O1 1.148(4) . ? Au1A P3 2.324(3) . ? Au1A P1 2.356(3) . ? Au1A Rh1A 2.924(6) . ? Au1A H1 1.33(4) . ? Rh1A P4 2.338(4) . ? Rh1A P2 2.439(4) . ? P1 C11 1.850(3) . ? P1 C1 1.855(3) . ? P1 C21 1.861(3) . ? P2 C1 1.831(3) . ? P2 C41 1.831(3) . ? P2 C31 1.850(3) . ? P3 C61A 1.852(10) . ? P3 C2 1.857(4) . ? P3 C51 1.858(3) . ? P3 C61 1.884(6) . ? P4 C71 1.837(3) . ? P4 C2 1.837(3) . ? P4 C81 1.845(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? P1S F4S 1.600(3) . ? P1S F3S 1.600(2) . ? P1S F1S 1.600(3) . ? P1S F2S 1.601(2) . ? P1S F6S 1.601(2) . ? P1S F5S 1.609(2) . ? C11 C16 1.532(5) . ? C11 C12 1.543(5) . ? C11 H11 1.0000 . ? C12 C13 1.524(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.526(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.521(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.527(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C21 C26 1.528(5) . ? C21 C22 1.541(5) . ? C21 H21 1.0000 . ? C22 C23 1.522(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.522(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.520(5) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.539(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C31 C32 1.520(5) . ? C31 C36 1.545(4) . ? C31 H31 1.0000 . ? C32 C33 1.533(5) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.524(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.511(5) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.542(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C41 C46 1.540(4) . ? C41 C42 1.546(4) . ? C41 H41 1.0000 . ? C42 C43 1.532(5) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.526(6) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.527(5) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.522(5) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C51 C52 1.531(5) . ? C51 C56 1.544(5) . ? C51 H51 1.0000 . ? C52 C53 1.533(5) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C54 C53 1.519(6) . ? C54 C55 1.522(6) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C55 C56 1.526(5) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C61 C62 1.530(8) . ? C61 C66 1.539(8) . ? C61 H61 1.0000 . ? C62 C63 1.530(7) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.524(8) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.511(8) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.523(8) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C61A C62A 1.519(11) . ? C61A C66A 1.520(13) . ? C61A H61A 1.0000 . ? C62A C63A 1.536(11) . ? C62A H62C 0.9900 . ? C62A H62D 0.9900 . ? C63A C64A 1.527(12) . ? C63A H63C 0.9900 . ? C63A H63D 0.9900 . ? C64A C65A 1.502(11) . ? C64A H64C 0.9900 . ? C64A H64D 0.9900 . ? C65A C66A 1.513(12) . ? C65A H65C 0.9900 . ? C65A H65D 0.9900 . ? C66A H66C 0.9900 . ? C66A H66D 0.9900 . ? C71 C72 1.532(5) . ? C71 C76 1.539(4) . ? C71 H71 1.0000 . ? C72 C73 1.530(5) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.522(5) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.520(6) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C76 1.534(5) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C81 C86 1.542(5) . ? C81 C82 1.543(5) . ? C81 H81 1.0000 . ? C82 C83 1.535(5) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 C84 1.524(5) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 C85 1.523(5) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C85 C86 1.534(5) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? C1S C6S 1.374(8) . ? C1S C2S 1.392(7) . ? C1S H1S 0.9500 . ? C2S C3S 1.381(8) . ? C2S H2S 0.9500 . ? C3S C4S 1.372(8) . ? C3S H3S 0.9500 . ? C4S C5S 1.388(6) . ? C4S H4S 0.9500 . ? C5S C6S 1.388(7) . ? C5S H5S 0.9500 . ? C6S H6S 0.9500 . ? C7S C8S 1.366(7) . ? C7S C12S 1.376(7) . ? C7S H7S 0.9500 . ? C8S C9S 1.384(7) . ? C8S H8S 0.9500 . ? C9S C10S 1.370(7) . ? C9S H9S 0.9500 . ? C10S C11S 1.373(7) . ? C10S H10S 0.9500 . ? C11S C12S 1.387(6) . ? C11S H11S 0.9500 . ? C12S H12S 0.9500 . ? C13S C14S 1.369(7) . ? C13S C15S 1.389(6) 2_645 ? C13S H13S 0.9500 . ? C14S C15S 1.384(7) . ? C14S H14S 0.9500 . ? C15S C13S 1.389(6) 2_645 ? C15S H15S 0.9500 . ? 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 P2 Au1 P4 177.12(3) . . ? P2 Au1 Rh1 86.55(2) . . ? P4 Au1 Rh1 93.97(2) . . ? C3 Rh1 P3 97.67(11) . . ? C3 Rh1 P1 95.13(11) . . ? P3 Rh1 P1 166.71(3) . . ? C3 Rh1 Au1 116.37(11) . . ? P3 Rh1 Au1 89.67(3) . . ? P1 Rh1 Au1 87.80(2) . . ? C3 Rh1 H1 172.1(13) . . ? P3 Rh1 H1 81.0(12) . . ? P1 Rh1 H1 85.8(12) . . ? Au1 Rh1 H1 71.4(12) . . ? O1 C3 Rh1 173.8(3) . . ? P3 Au1A P1 155.78(18) . . ? P3 Au1A Rh1A 102.50(14) . . ? P1 Au1A Rh1A 101.72(14) . . ? P3 Au1A H1 86.6(15) . . ? P1 Au1A H1 91.3(16) . . ? Rh1A Au1A H1 96.3(16) . . ? P4 Rh1A P2 151.8(3) . . ? P4 Rh1A Au1A 76.84(18) . . ? P2 Rh1A Au1A 74.97(16) . . ? C11 P1 C1 100.62(15) . . ? C11 P1 C21 106.14(15) . . ? C1 P1 C21 101.66(14) . . ? C11 P1 Rh1 118.72(11) . . ? C1 P1 Rh1 114.35(10) . . ? C21 P1 Rh1 113.30(11) . . ? C11 P1 Au1A 110.84(14) . . ? C1 P1 Au1A 106.41(13) . . ? C21 P1 Au1A 127.60(14) . . ? Rh1 P1 Au1A 14.38(8) . . ? C1 P2 C41 106.04(14) . . ? C1 P2 C31 101.73(15) . . ? C41 P2 C31 108.95(14) . . ? C1 P2 Au1 112.58(10) . . ? C41 P2 Au1 115.37(10) . . ? C31 P2 Au1 111.19(10) . . ? C1 P2 Rh1A 123.50(17) . . ? C41 P2 Rh1A 102.02(18) . . ? C31 P2 Rh1A 113.93(15) . . ? Au1 P2 Rh1A 14.18(15) . . ? C61A P3 C2 109.4(4) . . ? C61A P3 C51 104.9(4) . . ? C2 P3 C51 106.36(15) . . ? C61A P3 C61 16.8(3) . . ? C2 P3 C61 93.9(2) . . ? C51 P3 C61 104.1(2) . . ? C61A P3 Rh1 108.1(3) . . ? C2 P3 Rh1 117.64(10) . . ? C51 P3 Rh1 109.70(11) . . ? C61 P3 Rh1 123.0(2) . . ? C61A P3 Au1A 117.4(3) . . ? C2 P3 Au1A 103.21(14) . . ? C51 P3 Au1A 115.04(14) . . ? C61 P3 Au1A 129.9(2) . . ? Rh1 P3 Au1A 14.54(9) . . ? C71 P4 C2 103.15(15) . . ? C71 P4 C81 109.44(15) . . ? C2 P4 C81 104.16(16) . . ? C71 P4 Au1 113.03(11) . . ? C2 P4 Au1 110.08(11) . . ? C81 P4 Au1 115.86(10) . . ? C71 P4 Rh1A 116.14(15) . . ? C2 P4 Rh1A 121.02(18) . . ? C81 P4 Rh1A 102.05(19) . . ? Au1 P4 Rh1A 14.79(16) . . ? P2 C1 P1 112.99(16) . . ? P2 C1 H1A 109.0 . . ? P1 C1 H1A 109.0 . . ? P2 C1 H1B 109.0 . . ? P1 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? P4 C2 P3 117.57(18) . . ? P4 C2 H2A 107.9 . . ? P3 C2 H2A 107.9 . . ? P4 C2 H2B 107.9 . . ? P3 C2 H2B 107.9 . . ? H2A C2 H2B 107.2 . . ? F4S P1S F3S 90.31(14) . . ? F4S P1S F1S 179.55(14) . . ? F3S P1S F1S 90.02(14) . . ? F4S P1S F2S 90.06(14) . . ? F3S P1S F2S 90.25(13) . . ? F1S P1S F2S 90.24(15) . . ? F4S P1S F6S 90.05(13) . . ? F3S P1S F6S 89.97(12) . . ? F1S P1S F6S 89.65(14) . . ? F2S P1S F6S 179.76(15) . . ? F4S P1S F5S 89.97(13) . . ? F3S P1S F5S 179.71(16) . . ? F1S P1S F5S 89.70(13) . . ? F2S P1S F5S 89.66(12) . . ? F6S P1S F5S 90.12(11) . . ? C16 C11 C12 109.5(3) . . ? C16 C11 P1 112.3(2) . . ? C12 C11 P1 112.6(2) . . ? C16 C11 H11 107.4 . . ? C12 C11 H11 107.4 . . ? P1 C11 H11 107.4 . . ? C13 C12 C11 110.9(3) . . ? C13 C12 H12A 109.5 . . ? C11 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 108.0 . . ? C12 C13 C14 112.5(3) . . ? C12 C13 H13A 109.1 . . ? C14 C13 H13A 109.1 . . ? C12 C13 H13B 109.1 . . ? C14 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? C15 C14 C13 110.7(3) . . ? C15 C14 H14A 109.5 . . ? C13 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C14 C15 C16 111.0(3) . . ? C14 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? C14 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C15 C16 C11 111.2(3) . . ? C15 C16 H16A 109.4 . . ? C11 C16 H16A 109.4 . . ? C15 C16 H16B 109.4 . . ? C11 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C26 C21 C22 110.5(3) . . ? C26 C21 P1 114.6(2) . . ? C22 C21 P1 112.3(2) . . ? C26 C21 H21 106.3 . . ? C22 C21 H21 106.3 . . ? P1 C21 H21 106.3 . . ? C23 C22 C21 111.1(3) . . ? C23 C22 H22A 109.4 . . ? C21 C22 H22A 109.4 . . ? C23 C22 H22B 109.4 . . ? C21 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C24 C23 C22 111.3(3) . . ? C24 C23 H23A 109.4 . . ? C22 C23 H23A 109.4 . . ? C24 C23 H23B 109.4 . . ? C22 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? C25 C24 C23 110.8(3) . . ? C25 C24 H24A 109.5 . . ? C23 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? C24 C25 C26 111.5(3) . . ? C24 C25 H25A 109.3 . . ? C26 C25 H25A 109.3 . . ? C24 C25 H25B 109.3 . . ? C26 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? C21 C26 C25 111.3(3) . . ? C21 C26 H26A 109.4 . . ? C25 C26 H26A 109.4 . . ? C21 C26 H26B 109.4 . . ? C25 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C32 C31 C36 112.1(3) . . ? C32 C31 P2 112.3(2) . . ? C36 C31 P2 114.7(2) . . ? C32 C31 H31 105.6 . . ? C36 C31 H31 105.6 . . ? P2 C31 H31 105.6 . . ? C31 C32 C33 110.0(3) . . ? C31 C32 H32A 109.7 . . ? C33 C32 H32A 109.7 . . ? C31 C32 H32B 109.7 . . ? C33 C32 H32B 109.7 . . ? H32A C32 H32B 108.2 . . ? C34 C33 C32 111.0(3) . . ? C34 C33 H33A 109.4 . . ? C32 C33 H33A 109.4 . . ? C34 C33 H33B 109.4 . . ? C32 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? C35 C34 C33 110.7(3) . . ? C35 C34 H34A 109.5 . . ? C33 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? C34 C35 C36 112.3(3) . . ? C34 C35 H35A 109.1 . . ? C36 C35 H35A 109.1 . . ? C34 C35 H35B 109.1 . . ? C36 C35 H35B 109.1 . . ? H35A C35 H35B 107.9 . . ? C35 C36 C31 110.0(3) . . ? C35 C36 H36A 109.7 . . ? C31 C36 H36A 109.7 . . ? C35 C36 H36B 109.7 . . ? C31 C36 H36B 109.7 . . ? H36A C36 H36B 108.2 . . ? C46 C41 C42 109.7(3) . . ? C46 C41 P2 110.3(2) . . ? C42 C41 P2 111.8(2) . . ? C46 C41 H41 108.3 . . ? C42 C41 H41 108.3 . . ? P2 C41 H41 108.3 . . ? C43 C42 C41 110.4(3) . . ? C43 C42 H42A 109.6 . . ? C41 C42 H42A 109.6 . . ? C43 C42 H42B 109.6 . . ? C41 C42 H42B 109.6 . . ? H42A C42 H42B 108.1 . . ? C44 C43 C42 111.2(3) . . ? C44 C43 H43A 109.4 . . ? C42 C43 H43A 109.4 . . ? C44 C43 H43B 109.4 . . ? C42 C43 H43B 109.4 . . ? H43A C43 H43B 108.0 . . ? C43 C44 C45 110.9(3) . . ? C43 C44 H44A 109.5 . . ? C45 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? C45 C44 H44B 109.5 . . ? H44A C44 H44B 108.0 . . ? C46 C45 C44 111.3(3) . . ? C46 C45 H45A 109.4 . . ? C44 C45 H45A 109.4 . . ? C46 C45 H45B 109.4 . . ? C44 C45 H45B 109.4 . . ? H45A C45 H45B 108.0 . . ? C45 C46 C41 111.1(3) . . ? C45 C46 H46A 109.4 . . ? C41 C46 H46A 109.4 . . ? C45 C46 H46B 109.4 . . ? C41 C46 H46B 109.4 . . ? H46A C46 H46B 108.0 . . ? C52 C51 C56 109.9(3) . . ? C52 C51 P3 113.6(2) . . ? C56 C51 P3 107.7(2) . . ? C52 C51 H51 108.5 . . ? C56 C51 H51 108.5 . . ? P3 C51 H51 108.5 . . ? C51 C52 C53 111.6(3) . . ? C51 C52 H52A 109.3 . . ? C53 C52 H52A 109.3 . . ? C51 C52 H52B 109.3 . . ? C53 C52 H52B 109.3 . . ? H52A C52 H52B 108.0 . . ? C53 C54 C55 110.3(3) . . ? C53 C54 H54A 109.6 . . ? C55 C54 H54A 109.6 . . ? C53 C54 H54B 109.6 . . ? C55 C54 H54B 109.6 . . ? H54A C54 H54B 108.1 . . ? C54 C53 C52 111.0(3) . . ? C54 C53 H53A 109.4 . . ? C52 C53 H53A 109.4 . . ? C54 C53 H53B 109.4 . . ? C52 C53 H53B 109.4 . . ? H53A C53 H53B 108.0 . . ? C54 C55 C56 110.5(3) . . ? C54 C55 H55A 109.6 . . ? C56 C55 H55A 109.6 . . ? C54 C55 H55B 109.6 . . ? C56 C55 H55B 109.6 . . ? H55A C55 H55B 108.1 . . ? C55 C56 C51 112.8(3) . . ? C55 C56 H56A 109.0 . . ? C51 C56 H56A 109.0 . . ? C55 C56 H56B 109.0 . . ? C51 C56 H56B 109.0 . . ? H56A C56 H56B 107.8 . . ? C62 C61 C66 110.7(5) . . ? C62 C61 P3 113.8(4) . . ? C66 C61 P3 109.8(4) . . ? C62 C61 H61 107.4 . . ? C66 C61 H61 107.4 . . ? P3 C61 H61 107.4 . . ? C63 C62 C61 111.2(5) . . ? C63 C62 H62A 109.4 . . ? C61 C62 H62A 109.4 . . ? C63 C62 H62B 109.4 . . ? C61 C62 H62B 109.4 . . ? H62A C62 H62B 108.0 . . ? C64 C63 C62 112.1(5) . . ? C64 C63 H63A 109.2 . . ? C62 C63 H63A 109.2 . . ? C64 C63 H63B 109.2 . . ? C62 C63 H63B 109.2 . . ? H63A C63 H63B 107.9 . . ? C65 C64 C63 111.2(5) . . ? C65 C64 H64A 109.4 . . ? C63 C64 H64A 109.4 . . ? C65 C64 H64B 109.4 . . ? C63 C64 H64B 109.4 . . ? H64A C64 H64B 108.0 . . ? C64 C65 C66 111.1(5) . . ? C64 C65 H65A 109.4 . . ? C66 C65 H65A 109.4 . . ? C64 C65 H65B 109.4 . . ? C66 C65 H65B 109.4 . . ? H65A C65 H65B 108.0 . . ? C65 C66 C61 112.2(6) . . ? C65 C66 H66A 109.2 . . ? C61 C66 H66A 109.2 . . ? C65 C66 H66B 109.2 . . ? C61 C66 H66B 109.2 . . ? H66A C66 H66B 107.9 . . ? C62A C61A C66A 110.2(9) . . ? C62A C61A P3 114.2(7) . . ? C66A C61A P3 110.8(8) . . ? C62A C61A H61A 107.1 . . ? C66A C61A H61A 107.1 . . ? P3 C61A H61A 107.1 . . ? C61A C62A C63A 111.9(8) . . ? C61A C62A H62C 109.2 . . ? C63A C62A H62C 109.2 . . ? C61A C62A H62D 109.2 . . ? C63A C62A H62D 109.2 . . ? H62C C62A H62D 107.9 . . ? C64A C63A C62A 110.3(8) . . ? C64A C63A H63C 109.6 . . ? C62A C63A H63C 109.6 . . ? C64A C63A H63D 109.6 . . ? C62A C63A H63D 109.6 . . ? H63C C63A H63D 108.1 . . ? C65A C64A C63A 110.7(9) . . ? C65A C64A H64C 109.5 . . ? C63A C64A H64C 109.5 . . ? C65A C64A H64D 109.5 . . ? C63A C64A H64D 109.5 . . ? H64C C64A H64D 108.1 . . ? C64A C65A C66A 112.5(8) . . ? C64A C65A H65C 109.1 . . ? C66A C65A H65C 109.1 . . ? C64A C65A H65D 109.1 . . ? C66A C65A H65D 109.1 . . ? H65C C65A H65D 107.8 . . ? C65A C66A C61A 110.7(11) . . ? C65A C66A H66C 109.5 . . ? C61A C66A H66C 109.5 . . ? C65A C66A H66D 109.5 . . ? C61A C66A H66D 109.5 . . ? H66C C66A H66D 108.1 . . ? C72 C71 C76 110.5(3) . . ? C72 C71 P4 114.6(2) . . ? C76 C71 P4 114.8(2) . . ? C72 C71 H71 105.3 . . ? C76 C71 H71 105.3 . . ? P4 C71 H71 105.3 . . ? C73 C72 C71 109.7(3) . . ? C73 C72 H72A 109.7 . . ? C71 C72 H72A 109.7 . . ? C73 C72 H72B 109.7 . . ? C71 C72 H72B 109.7 . . ? H72A C72 H72B 108.2 . . ? C74 C73 C72 111.0(3) . . ? C74 C73 H73A 109.4 . . ? C72 C73 H73A 109.4 . . ? C74 C73 H73B 109.4 . . ? C72 C73 H73B 109.4 . . ? H73A C73 H73B 108.0 . . ? C75 C74 C73 111.5(3) . . ? C75 C74 H74A 109.3 . . ? C73 C74 H74A 109.3 . . ? C75 C74 H74B 109.3 . . ? C73 C74 H74B 109.3 . . ? H74A C74 H74B 108.0 . . ? C74 C75 C76 112.2(3) . . ? C74 C75 H75A 109.2 . . ? C76 C75 H75A 109.2 . . ? C74 C75 H75B 109.2 . . ? C76 C75 H75B 109.2 . . ? H75A C75 H75B 107.9 . . ? C75 C76 C71 110.1(3) . . ? C75 C76 H76A 109.6 . . ? C71 C76 H76A 109.6 . . ? C75 C76 H76B 109.6 . . ? C71 C76 H76B 109.6 . . ? H76A C76 H76B 108.1 . . ? C86 C81 C82 109.9(3) . . ? C86 C81 P4 110.9(2) . . ? C82 C81 P4 109.2(2) . . ? C86 C81 H81 108.9 . . ? C82 C81 H81 108.9 . . ? P4 C81 H81 108.9 . . ? C83 C82 C81 111.1(3) . . ? C83 C82 H82A 109.4 . . ? C81 C82 H82A 109.4 . . ? C83 C82 H82B 109.4 . . ? C81 C82 H82B 109.4 . . ? H82A C82 H82B 108.0 . . ? C84 C83 C82 110.8(3) . . ? C84 C83 H83A 109.5 . . ? C82 C83 H83A 109.5 . . ? C84 C83 H83B 109.5 . . ? C82 C83 H83B 109.5 . . ? H83A C83 H83B 108.1 . . ? C85 C84 C83 111.2(3) . . ? C85 C84 H84A 109.4 . . ? C83 C84 H84A 109.4 . . ? C85 C84 H84B 109.4 . . ? C83 C84 H84B 109.4 . . ? H84A C84 H84B 108.0 . . ? C84 C85 C86 112.1(3) . . ? C84 C85 H85A 109.2 . . ? C86 C85 H85A 109.2 . . ? C84 C85 H85B 109.2 . . ? C86 C85 H85B 109.2 . . ? H85A C85 H85B 107.9 . . ? C85 C86 C81 111.8(3) . . ? C85 C86 H86A 109.3 . . ? C81 C86 H86A 109.3 . . ? C85 C86 H86B 109.3 . . ? C81 C86 H86B 109.3 . . ? H86A C86 H86B 107.9 . . ? C6S C1S C2S 120.0(5) . . ? C6S C1S H1S 120.0 . . ? C2S C1S H1S 120.0 . . ? C3S C2S C1S 119.5(5) . . ? C3S C2S H2S 120.2 . . ? C1S C2S H2S 120.2 . . ? C4S C3S C2S 120.5(4) . . ? C4S C3S H3S 119.7 . . ? C2S C3S H3S 119.7 . . ? C3S C4S C5S 120.2(5) . . ? C3S C4S H4S 119.9 . . ? C5S C4S H4S 119.9 . . ? C6S C5S C4S 119.3(5) . . ? C6S C5S H5S 120.3 . . ? C4S C5S H5S 120.3 . . ? C1S C6S C5S 120.4(5) . . ? C1S C6S H6S 119.8 . . ? C5S C6S H6S 119.8 . . ? C8S C7S C12S 120.4(5) . . ? C8S C7S H7S 119.8 . . ? C12S C7S H7S 119.8 . . ? C7S C8S C9S 119.2(5) . . ? C7S C8S H8S 120.4 . . ? C9S C8S H8S 120.4 . . ? C10S C9S C8S 120.6(5) . . ? C10S C9S H9S 119.7 . . ? C8S C9S H9S 119.7 . . ? C9S C10S C11S 120.5(4) . . ? C9S C10S H10S 119.8 . . ? C11S C10S H10S 119.8 . . ? C10S C11S C12S 118.8(5) . . ? C10S C11S H11S 120.6 . . ? C12S C11S H11S 120.6 . . ? C7S C12S C11S 120.5(5) . . ? C7S C12S H12S 119.7 . . ? C11S C12S H12S 119.7 . . ? C14S C13S C15S 119.7(4) . 2_645 ? C14S C13S H13S 120.1 . . ? C15S C13S H13S 120.1 2_645 . ? C13S C14S C15S 120.0(4) . . ? C13S C14S H14S 120.0 . . ? C15S C14S H14S 120.0 . . ? C14S C15S C13S 120.2(5) . 2_645 ? C14S C15S H15S 119.9 . . ? C13S C15S H15S 119.9 2_645 . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.401 _refine_diff_density_min -0.855 _refine_diff_density_rms 0.099