# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email igor.koshevoy@uef.fi _publ_contact_author_name 'Igor Koshevoy' loop_ _publ_author_name I.Koshevoy 'Pi-Tai Chou' T.Pakkanen M.Haukka S.Tunik data_1 _database_code_depnum_ccdc_archive 'CCDC 809015' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C96 H102 Au8 P4, 2(F6 P), C H4 O' _chemical_formula_sum 'C97 H106 Au8 F12 O P6' _chemical_formula_weight 3277.37 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' 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 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 22.3376(17) _cell_length_b 18.7149(14) _cell_length_c 23.4710(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9812.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9361 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 26.18 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.219 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6104 _exptl_absorpt_coefficient_mu 12.079 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1175 _exptl_absorpt_correction_T_max 0.1359 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _publ_section_exptl_refinement ; After the anisotropic refinement of the Au molecule and the anion, some residual electron density remained unassigned. Furthermore, the crystal contained solvent accessible voids. The remaining residual density could not be unambiguously identified and it was equated to 1 molecule of methanol per molecule of the Au complex using the SQUEEZE routine in PLATON (Spek, 2003). Most probably solvent was partially lost from the crystal. The carbon atoms C18 and C16 were disordered over two sites with equal occupacies. The carbon-carbon distances in the disordered units were restrained to be be similar. The carbon atoms C18A, C18B as well as C7 were restrained with effective standard deviation 0.01 so that their U~ij~ components approximate to isotropic behavior. The hydrogen atoms were positioned geometrically and constrained to ride on their parent atoms, with C---H = 0.95-0.98 \%A, and U~iso~ = 1.2-1.5 U~eq~(parent atom). The highest peak is located 0.81 \%A from atom Au1 and the deepest hole is located 1.19 \%A from atom Au1. ; _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 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Bruker KAPPA APEX II CCD' _diffrn_measurement_device '62mm x 62mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 16 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34524 _diffrn_reflns_av_R_equivalents 0.0878 _diffrn_reflns_av_sigmaI/netI 0.0992 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9558 _reflns_number_gt 6161 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT (Bruker AXS, 2009)' _computing_data_reduction 'SAINT (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond v.3.2e (Brandenburg, 2010)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0156P)^2^+0.0000P] 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 9558 _refine_ls_number_parameters 579 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0735 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.0720 _refine_ls_wR_factor_gt 0.0670 _refine_ls_goodness_of_fit_ref 0.879 _refine_ls_restrained_S_all 0.879 _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 0.497511(16) 0.90309(2) 0.313631(14) 0.02010(9) Uani 1 1 d . . . Au2 Au 0.621887(17) 0.85645(2) 0.380440(14) 0.02241(9) Uani 1 1 d . . . Au3 Au 0.532352(17) 0.95480(2) 0.425223(15) 0.02438(10) Uani 1 1 d . . . Au4 Au 0.439587(17) 0.89819(2) 0.529365(15) 0.02423(10) Uani 1 1 d . . . P1 P 0.67790(11) 0.86408(13) 0.46165(10) 0.0221(6) Uani 1 1 d . . . P2 P 0.40905(11) 0.96246(13) 0.31657(9) 0.0184(5) Uani 1 1 d . . . P3 P 0.34259(15) 0.55675(18) 0.34680(12) 0.0448(8) Uani 1 1 d . . . F1 F 0.2985(4) 0.5078(4) 0.3828(3) 0.080(2) Uani 1 1 d . . . F2 F 0.3960(4) 0.5348(4) 0.3870(3) 0.088(3) Uani 1 1 d . . . F3 F 0.3292(3) 0.6215(3) 0.3870(3) 0.066(2) Uani 1 1 d . . . F4 F 0.3869(3) 0.6055(4) 0.3117(2) 0.0586(19) Uani 1 1 d . . . F5 F 0.3559(3) 0.4924(4) 0.3064(3) 0.074(2) Uani 1 1 d . . . F6 F 0.2883(3) 0.5800(3) 0.3082(2) 0.0542(18) Uani 1 1 d . . . C1 C 0.5578(4) 0.8308(5) 0.2594(4) 0.023(2) Uani 1 1 d . . . C2 C 0.5805(4) 0.8418(5) 0.3056(4) 0.026(2) Uani 1 1 d . . . C3 C 0.6496(4) 0.9173(5) 0.5209(3) 0.018(2) Uani 1 1 d . . . C4 C 0.6694(4) 0.9867(5) 0.5314(4) 0.020(2) Uani 1 1 d . . . H4 H 0.6965 1.0083 0.5053 0.024 Uiso 1 1 calc R . . C5 C 0.3493(4) 0.9747(5) 0.4212(3) 0.019(2) Uani 1 1 d . . . H5 H 0.3362 0.9268 0.4160 0.023 Uiso 1 1 calc R . . C6 C 0.3874(4) 1.0065(4) 0.3813(3) 0.016(2) Uani 1 1 d . . . C7 C 0.5836(5) 1.0353(5) 0.4004(4) 0.032(3) Uani 1 1 d U . . C8 C 0.6238(5) 1.0802(6) 0.3917(4) 0.036(3) Uani 1 1 d . . . C9 C 0.4866(4) 0.8714(5) 0.4527(3) 0.024(2) Uani 1 1 d . . . C10 C 0.4637(4) 0.8146(5) 0.4668(4) 0.028(2) Uani 1 1 d . . . C11 C 0.4435(4) 0.7390(5) 0.4727(4) 0.028(2) Uani 1 1 d . . . C12 C 0.3748(4) 0.7394(6) 0.4707(5) 0.045(3) Uani 1 1 d . . . H12B H 0.3613 0.7581 0.4339 0.067 Uiso 1 1 calc R . . H12A H 0.3593 0.7699 0.5014 0.067 Uiso 1 1 calc R . . H12C H 0.3597 0.6906 0.4758 0.067 Uiso 1 1 calc R . . C13 C 0.4663(5) 0.7066(6) 0.5277(5) 0.053(3) Uani 1 1 d . . . H13B H 0.4451 0.7282 0.5600 0.080 Uiso 1 1 calc R . . H13A H 0.5093 0.7158 0.5313 0.080 Uiso 1 1 calc R . . H13C H 0.4591 0.6550 0.5274 0.080 Uiso 1 1 calc R . . C14 C 0.4685(5) 0.6992(5) 0.4200(5) 0.046(3) Uani 1 1 d . . . H14C H 0.5123 0.6998 0.4211 0.069 Uiso 1 1 calc R . . H14A H 0.4546 0.7229 0.3852 0.069 Uiso 1 1 calc R . . H14B H 0.4543 0.6496 0.4203 0.069 Uiso 1 1 calc R . . C15 C 0.6761(5) 1.1202(7) 0.3693(4) 0.048(4) Uani 1 1 d . . . C16A C 0.6544(16) 1.2109(12) 0.3618(12) 0.042(8) Uani 0.50 1 d P A 1 H16A H 0.6887 1.2391 0.3486 0.063 Uiso 0.50 1 calc PR A 1 H16B H 0.6408 1.2293 0.3987 0.063 Uiso 0.50 1 calc PR A 1 H16C H 0.6218 1.2145 0.3341 0.063 Uiso 0.50 1 calc PR A 1 C18A C 0.6919(12) 1.0976(14) 0.3148(10) 0.052(7) Uani 0.50 1 d PU A 1 H18A H 0.6909 1.0453 0.3132 0.078 Uiso 0.50 1 calc PR A 1 H18B H 0.7323 1.1144 0.3058 0.078 Uiso 0.50 1 calc PR A 1 H18C H 0.6635 1.1172 0.2871 0.078 Uiso 0.50 1 calc PR A 1 C16B C 0.6606(15) 1.1757(13) 0.3400(14) 0.060(10) Uani 0.50 1 d P A 2 H16D H 0.6908 1.1850 0.3106 0.090 Uiso 0.50 1 calc PR A 2 H16E H 0.6576 1.2172 0.3653 0.090 Uiso 0.50 1 calc PR A 2 H16F H 0.6218 1.1670 0.3219 0.090 Uiso 0.50 1 calc PR A 2 C18B C 0.7048(10) 1.0546(12) 0.3226(9) 0.039(6) Uani 0.50 1 d PU A 2 H18D H 0.6865 1.0602 0.2849 0.059 Uiso 0.50 1 calc PR A 2 H18E H 0.6956 1.0070 0.3376 0.059 Uiso 0.50 1 calc PR A 2 H18F H 0.7483 1.0602 0.3194 0.059 Uiso 0.50 1 calc PR A 2 C17 C 0.7254(4) 1.1242(6) 0.4123(4) 0.042(3) Uani 1 1 d . A . H17A H 0.7414 1.0762 0.4190 0.064 Uiso 1 1 calc R . . H17C H 0.7097 1.1437 0.4480 0.064 Uiso 1 1 calc R . . H17B H 0.7573 1.1553 0.3979 0.064 Uiso 1 1 calc R . . C19 C 0.5414(4) 0.8086(5) 0.1999(4) 0.028(2) Uani 1 1 d . . . C20 C 0.5136(6) 0.8721(6) 0.1665(4) 0.054(4) Uani 1 1 d . . . H20C H 0.5428 0.9110 0.1640 0.081 Uiso 1 1 calc R . . H20A H 0.4777 0.8890 0.1863 0.081 Uiso 1 1 calc R . . H20B H 0.5028 0.8563 0.1280 0.081 Uiso 1 1 calc R . . C21 C 0.4990(5) 0.7456(6) 0.2026(4) 0.047(3) Uani 1 1 d . . . H21C H 0.4630 0.7591 0.2238 0.070 Uiso 1 1 calc R . . H21A H 0.5188 0.7056 0.2218 0.070 Uiso 1 1 calc R . . H21B H 0.4878 0.7313 0.1638 0.070 Uiso 1 1 calc R . . C22 C 0.5996(4) 0.7857(6) 0.1695(4) 0.038(3) Uani 1 1 d . . . H22B H 0.6211 0.7512 0.1933 0.058 Uiso 1 1 calc R . . H22A H 0.6249 0.8278 0.1632 0.058 Uiso 1 1 calc R . . H22C H 0.5898 0.7637 0.1328 0.058 Uiso 1 1 calc R . . C23 C 0.6109(4) 0.8877(5) 0.5590(4) 0.024(2) Uani 1 1 d . . . H23 H 0.5969 0.8405 0.5525 0.029 Uiso 1 1 calc R . . C24 C 0.4089(4) 1.0753(5) 0.3921(3) 0.024(2) Uani 1 1 d . . . H24 H 0.4367 1.0970 0.3668 0.028 Uiso 1 1 calc R . . C25 C 0.4080(4) 1.0328(4) 0.2632(3) 0.018(2) Uani 1 1 d . . . C26 C 0.4551(4) 1.0409(5) 0.2278(4) 0.030(2) Uani 1 1 d . . . H26 H 0.4882 1.0092 0.2310 0.036 Uiso 1 1 calc R . . C27 C 0.4565(5) 1.0941(6) 0.1870(4) 0.041(3) Uani 1 1 d . . . H27 H 0.4906 1.0994 0.1631 0.049 Uiso 1 1 calc R . . C28 C 0.4085(5) 1.1392(6) 0.1811(4) 0.043(3) Uani 1 1 d . . . H28 H 0.4085 1.1746 0.1520 0.052 Uiso 1 1 calc R . . C29 C 0.3612(4) 1.1330(6) 0.2167(4) 0.034(3) Uani 1 1 d . . . H29 H 0.3283 1.1648 0.2125 0.041 Uiso 1 1 calc R . . C30 C 0.3596(4) 1.0820(5) 0.2589(4) 0.029(2) Uani 1 1 d . . . H30 H 0.3268 1.0797 0.2846 0.034 Uiso 1 1 calc R . . C31 C 0.3492(4) 0.9008(5) 0.3016(3) 0.021(2) Uani 1 1 d . . . C32 C 0.2917(4) 0.9219(5) 0.2878(4) 0.030(3) Uani 1 1 d . . . H32 H 0.2820 0.9714 0.2877 0.036 Uiso 1 1 calc R . . C33 C 0.2475(5) 0.8721(6) 0.2740(4) 0.043(3) Uani 1 1 d . . . H33 H 0.2084 0.8874 0.2635 0.051 Uiso 1 1 calc R . . C34 C 0.2615(5) 0.8003(6) 0.2758(5) 0.045(3) Uani 1 1 d . . . H34 H 0.2316 0.7662 0.2662 0.054 Uiso 1 1 calc R . . C35 C 0.3171(5) 0.7770(6) 0.2909(5) 0.053(4) Uani 1 1 d . . . H35 H 0.3261 0.7274 0.2925 0.064 Uiso 1 1 calc R . . C36 C 0.3601(5) 0.8273(5) 0.3037(4) 0.034(3) Uani 1 1 d . . . H36 H 0.3988 0.8114 0.3146 0.041 Uiso 1 1 calc R . . C37 C 0.6853(4) 0.7765(5) 0.4941(3) 0.020(2) Uani 1 1 d . . . C38 C 0.7220(4) 0.7640(5) 0.5414(4) 0.027(2) Uani 1 1 d . . . H38 H 0.7461 0.8016 0.5560 0.033 Uiso 1 1 calc R . . C39 C 0.7237(4) 0.6983(6) 0.5669(4) 0.034(3) Uani 1 1 d . . . H39 H 0.7492 0.6909 0.5987 0.040 Uiso 1 1 calc R . . C40 C 0.6896(5) 0.6435(5) 0.5475(4) 0.038(3) Uani 1 1 d . . . H40 H 0.6915 0.5977 0.5649 0.045 Uiso 1 1 calc R . . C41 C 0.6517(5) 0.6561(6) 0.5015(5) 0.048(3) Uani 1 1 d . . . H41 H 0.6268 0.6185 0.4879 0.057 Uiso 1 1 calc R . . C42 C 0.6495(5) 0.7211(6) 0.4754(4) 0.035(3) Uani 1 1 d . . . H42 H 0.6232 0.7283 0.4442 0.042 Uiso 1 1 calc R . . C43 C 0.7518(4) 0.8975(5) 0.4435(4) 0.025(2) Uani 1 1 d . . . C44 C 0.7703(5) 0.8945(7) 0.3881(4) 0.050(3) Uani 1 1 d . . . H44 H 0.7447 0.8747 0.3600 0.060 Uiso 1 1 calc R . . C45 C 0.8252(5) 0.9197(7) 0.3730(5) 0.060(4) Uani 1 1 d . . . H45 H 0.8377 0.9163 0.3344 0.072 Uiso 1 1 calc R . . C46 C 0.8622(5) 0.9497(6) 0.4122(5) 0.049(3) Uani 1 1 d . . . H46 H 0.8996 0.9692 0.4008 0.059 Uiso 1 1 calc R . . C47 C 0.8453(4) 0.9517(5) 0.4680(4) 0.035(3) Uani 1 1 d . . . H47 H 0.8714 0.9713 0.4958 0.042 Uiso 1 1 calc R . . C48 C 0.7903(4) 0.9252(5) 0.4842(4) 0.026(2) Uani 1 1 d . . . H48 H 0.7788 0.9260 0.5232 0.032 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 0.0184(2) 0.02380(19) 0.01809(16) -0.00308(17) -0.00068(16) 0.00381(17) Au2 0.0197(2) 0.0285(2) 0.01904(17) -0.00600(17) -0.00278(17) 0.00544(18) Au3 0.01532(19) 0.0350(2) 0.02286(18) -0.00918(19) 0.00107(17) 0.00085(18) Au4 0.0169(2) 0.0314(2) 0.02437(19) -0.00374(19) 0.00095(17) -0.00127(19) P1 0.0175(14) 0.0291(15) 0.0197(12) -0.0025(12) 0.0005(11) 0.0010(12) P2 0.0157(13) 0.0231(14) 0.0165(11) -0.0020(11) -0.0017(10) 0.0013(11) P3 0.052(2) 0.050(2) 0.0321(16) -0.0082(16) -0.0017(16) -0.0025(17) F1 0.127(7) 0.071(5) 0.042(4) 0.007(4) 0.007(5) -0.032(5) F2 0.113(7) 0.068(5) 0.082(5) 0.007(4) -0.047(5) 0.015(5) F3 0.091(6) 0.052(5) 0.054(4) -0.022(4) 0.011(4) -0.013(4) F4 0.031(4) 0.088(5) 0.057(4) 0.000(4) 0.005(3) -0.012(4) F5 0.091(6) 0.058(5) 0.071(5) -0.033(4) -0.006(4) 0.012(4) F6 0.035(4) 0.076(5) 0.052(4) -0.005(4) -0.001(3) -0.004(3) C1 0.016(5) 0.029(6) 0.023(5) -0.001(5) 0.003(4) 0.014(5) C2 0.034(7) 0.015(5) 0.028(5) -0.004(4) 0.003(5) 0.013(5) C3 0.017(5) 0.022(5) 0.015(4) -0.002(4) 0.003(4) 0.011(4) C4 0.012(5) 0.020(5) 0.027(5) 0.004(4) 0.002(4) -0.001(4) C5 0.019(5) 0.018(5) 0.020(5) 0.000(4) 0.003(4) 0.003(4) C6 0.012(5) 0.019(5) 0.017(4) -0.003(4) -0.002(4) 0.001(4) C7 0.031(5) 0.044(6) 0.020(4) -0.008(4) 0.018(4) -0.009(5) C8 0.021(6) 0.066(8) 0.021(5) 0.008(5) -0.005(5) 0.004(6) C9 0.022(6) 0.033(6) 0.016(5) -0.003(4) 0.000(4) -0.005(5) C10 0.025(6) 0.035(6) 0.024(5) -0.009(5) 0.007(5) 0.011(5) C11 0.015(5) 0.016(5) 0.052(6) 0.003(5) 0.011(5) 0.010(4) C12 0.030(7) 0.040(7) 0.065(7) -0.012(6) 0.001(6) -0.008(6) C13 0.055(9) 0.043(7) 0.061(8) 0.006(6) -0.015(7) -0.002(6) C14 0.031(6) 0.031(6) 0.076(8) -0.021(6) -0.005(7) -0.007(5) C15 0.016(6) 0.106(11) 0.022(5) 0.018(6) 0.001(5) -0.019(7) C16A 0.051(18) 0.015(14) 0.060(18) 0.009(13) 0.006(15) 0.010(14) C18A 0.051(11) 0.061(10) 0.045(9) -0.005(9) 0.004(8) -0.006(9) C16B 0.052(19) 0.029(18) 0.10(3) 0.041(18) 0.01(2) -0.002(17) C18B 0.035(10) 0.042(10) 0.040(9) -0.002(8) 0.012(8) -0.004(8) C17 0.023(6) 0.051(8) 0.053(7) 0.007(6) -0.002(6) -0.014(5) C19 0.028(6) 0.032(6) 0.023(5) -0.013(5) -0.001(5) -0.003(5) C20 0.092(11) 0.054(8) 0.016(5) -0.005(5) -0.017(6) 0.023(7) C21 0.038(7) 0.070(9) 0.032(6) -0.014(6) 0.001(6) -0.015(7) C22 0.028(7) 0.055(8) 0.032(6) -0.017(6) 0.003(5) 0.003(6) C23 0.007(5) 0.025(6) 0.041(6) -0.004(5) -0.004(5) 0.004(4) C24 0.016(5) 0.042(6) 0.013(4) -0.008(4) 0.003(4) -0.006(5) C25 0.023(5) 0.013(5) 0.017(4) -0.003(4) -0.007(4) 0.000(4) C26 0.026(6) 0.033(6) 0.032(5) 0.009(5) 0.006(5) 0.020(5) C27 0.053(8) 0.037(6) 0.032(6) 0.017(6) 0.018(6) 0.002(6) C28 0.063(9) 0.028(6) 0.038(6) 0.007(6) -0.007(6) -0.005(6) C29 0.019(6) 0.046(7) 0.037(6) 0.000(6) -0.013(5) 0.005(5) C30 0.019(6) 0.034(6) 0.033(6) -0.002(5) 0.005(5) 0.002(5) C31 0.025(6) 0.022(5) 0.015(4) -0.010(4) 0.011(4) 0.005(5) C32 0.024(6) 0.034(6) 0.034(5) -0.002(5) 0.008(5) 0.000(5) C33 0.019(6) 0.062(9) 0.047(6) -0.004(6) -0.002(5) -0.022(6) C34 0.051(8) 0.030(7) 0.055(7) -0.016(6) 0.021(7) -0.031(6) C35 0.038(8) 0.040(8) 0.081(9) -0.025(7) 0.030(7) -0.011(6) C36 0.034(7) 0.022(6) 0.047(6) 0.001(5) 0.004(5) -0.013(5) C37 0.011(5) 0.029(6) 0.020(5) 0.003(4) 0.006(4) 0.012(4) C38 0.017(6) 0.031(6) 0.033(5) 0.000(5) 0.002(5) 0.010(5) C39 0.029(6) 0.046(7) 0.026(5) 0.008(5) 0.006(5) 0.005(6) C40 0.044(7) 0.019(6) 0.051(7) 0.004(5) 0.014(6) -0.006(5) C41 0.049(8) 0.044(8) 0.050(7) -0.021(6) 0.001(6) -0.004(6) C42 0.036(7) 0.044(7) 0.025(5) 0.004(5) -0.004(5) -0.007(6) C43 0.016(5) 0.032(6) 0.026(5) -0.002(5) -0.001(4) 0.001(5) C44 0.029(7) 0.085(9) 0.036(6) -0.014(7) 0.005(6) 0.004(7) C45 0.035(8) 0.114(12) 0.032(6) -0.013(7) 0.007(6) 0.004(8) C46 0.030(7) 0.064(9) 0.055(8) 0.005(7) 0.023(6) 0.005(6) C47 0.025(6) 0.037(6) 0.042(6) 0.003(6) -0.003(5) -0.010(5) C48 0.020(6) 0.033(6) 0.026(5) 0.011(5) 0.003(5) 0.003(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 Au1 C2 2.187(9) . ? Au1 P2 2.268(2) . yes Au1 C1 2.294(8) . ? Au1 Au3 2.8987(5) . yes Au1 Au2 3.3075(5) . ? Au2 C2 2.005(9) . ? Au2 P1 2.285(2) . yes Au2 Au3 2.9143(5) . yes Au3 C9 1.974(10) . ? Au3 C7 1.980(10) . ? Au3 Au4 3.0165(6) 5_676 yes Au3 Au4 3.3751(5) . yes Au4 C7 2.130(9) 5_676 ? Au4 C9 2.142(9) . ? Au4 C10 2.213(9) . ? Au4 C8 2.366(10) 5_676 ? Au4 Au3 3.0164(6) 5_676 yes P1 C37 1.814(9) . ? P1 C43 1.817(10) . ? P1 C3 1.823(8) . ? P2 C6 1.795(8) . ? P2 C31 1.800(9) . ? P2 C25 1.816(8) . ? P3 F5 1.562(7) . ? P3 F3 1.564(6) . ? P3 F6 1.575(6) . ? P3 F2 1.576(7) . ? P3 F4 1.577(7) . ? P3 F1 1.588(7) . ? C1 C2 1.213(11) . ? C1 C19 1.503(11) . ? C3 C23 1.362(11) . ? C3 C4 1.393(11) . ? C4 C5 1.392(11) 5_676 ? C4 H4 0.9500 . ? C5 C4 1.392(11) 5_676 ? C5 C6 1.398(11) . ? C5 H5 0.9500 . ? C6 C24 1.399(11) . ? C7 C8 1.247(13) . ? C7 Au4 2.130(9) 5_676 ? C8 C15 1.483(14) . ? C8 Au4 2.366(10) 5_676 ? C9 C10 1.226(12) . ? C10 C11 1.491(13) . ? C11 C13 1.514(13) . ? C11 C12 1.537(12) . ? C11 C14 1.546(13) . ? C12 H12B 0.9800 . ? C12 H12A 0.9800 . ? C12 H12C 0.9800 . ? C13 H13B 0.9800 . ? C13 H13A 0.9800 . ? C13 H13C 0.9800 . ? C14 H14C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C16B 1.29(3) . ? C15 C18A 1.39(2) . ? C15 C17 1.495(13) . ? C15 C18B 1.77(2) . ? C15 C16A 1.77(2) . ? C16A H16A 0.9800 . ? C16A H16B 0.9800 . ? C16A H16C 0.9800 . ? C18A H18A 0.9800 . ? C18A H18B 0.9800 . ? C18A H18C 0.9800 . ? C16B H16D 0.9800 . ? C16B H16E 0.9800 . ? C16B H16F 0.9800 . ? C18B H18D 0.9800 . ? C18B H18E 0.9800 . ? C18B H18F 0.9800 . ? C17 H17A 0.9800 . ? C17 H17C 0.9800 . ? C17 H17B 0.9800 . ? C19 C21 1.513(13) . ? C19 C22 1.545(12) . ? C19 C20 1.552(13) . ? C20 H20C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C21 H21C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C22 H22B 0.9800 . ? C22 H22A 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.411(11) 5_676 ? C23 H23 0.9500 . ? C24 C23 1.411(11) 5_676 ? C24 H24 0.9500 . ? C25 C26 1.350(12) . ? C25 C30 1.426(12) . ? C26 C27 1.383(12) . ? C26 H26 0.9500 . ? C27 C28 1.371(14) . ? C27 H27 0.9500 . ? C28 C29 1.353(14) . ? C28 H28 0.9500 . ? C29 C30 1.375(12) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.383(12) . ? C31 C36 1.397(12) . ? C32 C33 1.397(13) . ? C32 H32 0.9500 . ? C33 C34 1.381(14) . ? C33 H33 0.9500 . ? C34 C35 1.364(15) . ? C34 H34 0.9500 . ? C35 C36 1.377(13) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.381(12) . ? C37 C38 1.400(11) . ? C38 C39 1.368(12) . ? C38 H38 0.9500 . ? C39 C40 1.356(13) . ? C39 H39 0.9500 . ? C40 C41 1.393(14) . ? C40 H40 0.9500 . ? C41 C42 1.362(13) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.365(12) . ? C43 C48 1.385(12) . ? C44 C45 1.360(15) . ? C44 H44 0.9500 . ? C45 C46 1.359(14) . ? C45 H45 0.9500 . ? C46 C47 1.365(13) . ? C46 H46 0.9500 . ? C47 C48 1.378(12) . ? C47 H47 0.9500 . ? C48 H48 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 C2 Au1 P2 176.0(2) . . ? C2 Au1 C1 31.3(3) . . ? P2 Au1 C1 144.8(2) . . ? C2 Au1 Au3 91.5(2) . . ? P2 Au1 Au3 92.46(6) . . ? C1 Au1 Au3 122.7(2) . . ? C2 Au1 Au2 36.0(2) . . ? P2 Au1 Au2 147.86(6) . . ? C1 Au1 Au2 67.3(2) . . ? Au3 Au1 Au2 55.542(11) . . ? C2 Au2 P1 173.0(3) . . ? C2 Au2 Au3 94.9(3) . . ? P1 Au2 Au3 92.03(6) . . ? C2 Au2 Au1 39.9(3) . . ? P1 Au2 Au1 147.05(6) . . ? Au3 Au2 Au1 55.099(12) . . ? C9 Au3 C7 175.7(4) . . ? C9 Au3 Au1 83.8(2) . . ? C7 Au3 Au1 98.2(3) . . ? C9 Au3 Au2 88.5(3) . . ? C7 Au3 Au2 88.7(3) . . ? Au1 Au3 Au2 69.358(13) . . ? C9 Au3 Au4 135.5(2) . 5_676 ? C7 Au3 Au4 44.8(2) . 5_676 ? Au1 Au3 Au4 132.814(17) . 5_676 ? Au2 Au3 Au4 124.121(17) . 5_676 ? C9 Au3 Au4 36.6(2) . . ? C7 Au3 Au4 143.8(2) . . ? Au1 Au3 Au4 112.627(16) . . ? Au2 Au3 Au4 118.964(17) . . ? Au4 Au3 Au4 99.091(13) 5_676 . ? C7 Au4 C9 155.0(4) 5_676 . ? C7 Au4 C10 170.5(4) 5_676 . ? C9 Au4 C10 32.7(3) . . ? C7 Au4 C8 31.6(3) 5_676 5_676 ? C9 Au4 C8 172.1(4) . 5_676 ? C10 Au4 C8 141.8(4) . 5_676 ? C7 Au4 Au3 40.9(3) 5_676 5_676 ? C9 Au4 Au3 114.1(3) . 5_676 ? C10 Au4 Au3 146.0(3) . 5_676 ? C8 Au4 Au3 72.1(3) 5_676 5_676 ? C7 Au4 Au3 121.8(3) 5_676 . ? C9 Au4 Au3 33.3(3) . . ? C10 Au4 Au3 65.9(3) . . ? C8 Au4 Au3 151.7(3) 5_676 . ? Au3 Au4 Au3 80.909(14) 5_676 . ? C37 P1 C43 109.1(4) . . ? C37 P1 C3 101.8(4) . . ? C43 P1 C3 107.8(4) . . ? C37 P1 Au2 110.1(3) . . ? C43 P1 Au2 108.9(3) . . ? C3 P1 Au2 118.7(3) . . ? C6 P2 C31 105.1(4) . . ? C6 P2 C25 104.3(4) . . ? C31 P2 C25 108.7(4) . . ? C6 P2 Au1 119.0(3) . . ? C31 P2 Au1 109.1(3) . . ? C25 P2 Au1 110.2(3) . . ? F5 P3 F3 179.7(5) . . ? F5 P3 F6 90.6(4) . . ? F3 P3 F6 89.2(4) . . ? F5 P3 F2 91.0(4) . . ? F3 P3 F2 89.2(4) . . ? F6 P3 F2 178.2(4) . . ? F5 P3 F4 90.5(4) . . ? F3 P3 F4 89.3(4) . . ? F6 P3 F4 91.3(3) . . ? F2 P3 F4 89.3(4) . . ? F5 P3 F1 89.8(4) . . ? F3 P3 F1 90.4(4) . . ? F6 P3 F1 89.3(4) . . ? F2 P3 F1 90.0(4) . . ? F4 P3 F1 179.3(4) . . ? C2 C1 C19 168.1(10) . . ? C2 C1 Au1 69.5(6) . . ? C19 C1 Au1 122.3(6) . . ? C1 C2 Au2 176.7(8) . . ? C1 C2 Au1 79.2(6) . . ? Au2 C2 Au1 104.1(4) . . ? C23 C3 C4 117.6(8) . . ? C23 C3 P1 119.9(7) . . ? C4 C3 P1 122.3(7) . . ? C5 C4 C3 122.1(8) 5_676 . ? C5 C4 H4 119.0 5_676 . ? C3 C4 H4 119.0 . . ? C4 C5 C6 119.8(8) 5_676 . ? C4 C5 H5 120.1 5_676 . ? C6 C5 H5 120.1 . . ? C5 C6 C24 118.7(8) . . ? C5 C6 P2 122.4(7) . . ? C24 C6 P2 118.9(6) . . ? C8 C7 Au3 167.9(9) . . ? C8 C7 Au4 84.7(7) . 5_676 ? Au3 C7 Au4 94.4(3) . 5_676 ? C7 C8 C15 164.8(11) . . ? C7 C8 Au4 63.7(6) . 5_676 ? C15 C8 Au4 131.5(8) . 5_676 ? C10 C9 Au3 172.0(8) . . ? C10 C9 Au4 76.8(6) . . ? Au3 C9 Au4 110.1(4) . . ? C9 C10 C11 167.0(9) . . ? C9 C10 Au4 70.5(6) . . ? C11 C10 Au4 122.4(6) . . ? C10 C11 C13 110.9(9) . . ? C10 C11 C12 107.1(8) . . ? C13 C11 C12 111.2(9) . . ? C10 C11 C14 105.9(8) . . ? C13 C11 C14 111.6(8) . . ? C12 C11 C14 109.8(9) . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12A 109.5 . . ? H12B C12 H12A 109.5 . . ? C11 C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? C11 C13 H13B 109.5 . . ? C11 C13 H13A 109.5 . . ? H13B C13 H13A 109.5 . . ? C11 C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? C11 C14 H14C 109.5 . . ? C11 C14 H14A 109.5 . . ? H14C C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14C C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C16B C15 C18A 79.8(18) . . ? C16B C15 C8 112.6(17) . . ? C18A C15 C8 111.8(14) . . ? C16B C15 C17 121.1(18) . . ? C18A C15 C17 116.6(14) . . ? C8 C15 C17 111.5(8) . . ? C16B C15 C18B 109.0(17) . . ? C8 C15 C18B 98.9(11) . . ? C17 C15 C18B 100.7(11) . . ? C18A C15 C16A 105.6(16) . . ? C8 C15 C16A 107.6(14) . . ? C17 C15 C16A 102.7(13) . . ? C18B C15 C16A 134.7(14) . . ? C15 C16A H16A 109.5 . . ? C15 C16A H16B 109.5 . . ? C15 C16A H16C 109.5 . . ? C15 C18A H18A 109.5 . . ? C15 C18A H18B 109.5 . . ? C15 C18A H18C 109.5 . . ? C15 C16B H16D 109.5 . . ? C15 C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C15 C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C15 C18B H18D 109.5 . . ? C15 C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C15 C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? H17C C17 H17B 109.5 . . ? C1 C19 C21 109.2(8) . . ? C1 C19 C22 107.4(8) . . ? C21 C19 C22 109.2(8) . . ? C1 C19 C20 110.9(8) . . ? C21 C19 C20 111.6(9) . . ? C22 C19 C20 108.4(8) . . ? C19 C20 H20C 109.5 . . ? C19 C20 H20A 109.5 . . ? H20C C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20C C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C21 H21C 109.5 . . ? C19 C21 H21A 109.5 . . ? H21C C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21C C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C22 H22B 109.5 . . ? C19 C22 H22A 109.5 . . ? H22B C22 H22A 109.5 . . ? C19 C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? C3 C23 C24 122.3(9) . 5_676 ? C3 C23 H23 118.9 . . ? C24 C23 H23 118.9 5_676 . ? C6 C24 C23 119.4(8) . 5_676 ? C6 C24 H24 120.3 . . ? C23 C24 H24 120.3 5_676 . ? C26 C25 C30 118.4(8) . . ? C26 C25 P2 119.8(7) . . ? C30 C25 P2 121.8(7) . . ? C25 C26 C27 121.7(9) . . ? C25 C26 H26 119.2 . . ? C27 C26 H26 119.2 . . ? C28 C27 C26 119.8(10) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C29 C28 C27 119.7(10) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C28 C29 C30 121.7(10) . . ? C28 C29 H29 119.1 . . ? C30 C29 H29 119.1 . . ? C29 C30 C25 118.7(9) . . ? C29 C30 H30 120.7 . . ? C25 C30 H30 120.7 . . ? C32 C31 C36 116.8(9) . . ? C32 C31 P2 123.5(8) . . ? C36 C31 P2 119.7(7) . . ? C31 C32 C33 121.4(10) . . ? C31 C32 H32 119.3 . . ? C33 C32 H32 119.3 . . ? C34 C33 C32 118.8(10) . . ? C34 C33 H33 120.6 . . ? C32 C33 H33 120.6 . . ? C35 C34 C33 121.8(10) . . ? C35 C34 H34 119.1 . . ? C33 C34 H34 119.1 . . ? C34 C35 C36 118.2(11) . . ? C34 C35 H35 120.9 . . ? C36 C35 H35 120.9 . . ? C35 C36 C31 123.0(11) . . ? C35 C36 H36 118.5 . . ? C31 C36 H36 118.5 . . ? C42 C37 C38 117.7(9) . . ? C42 C37 P1 119.6(7) . . ? C38 C37 P1 122.5(7) . . ? C39 C38 C37 120.9(9) . . ? C39 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C40 C39 C38 121.2(10) . . ? C40 C39 H39 119.4 . . ? C38 C39 H39 119.4 . . ? C39 C40 C41 118.2(10) . . ? C39 C40 H40 120.9 . . ? C41 C40 H40 120.9 . . ? C42 C41 C40 121.4(10) . . ? C42 C41 H41 119.3 . . ? C40 C41 H41 119.3 . . ? C41 C42 C37 120.6(10) . . ? C41 C42 H42 119.7 . . ? C37 C42 H42 119.7 . . ? C44 C43 C48 119.0(9) . . ? C44 C43 P1 118.9(8) . . ? C48 C43 P1 122.1(7) . . ? C45 C44 C43 120.5(11) . . ? C45 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C46 C45 C44 121.0(10) . . ? C46 C45 H45 119.5 . . ? C44 C45 H45 119.5 . . ? C45 C46 C47 119.4(11) . . ? C45 C46 H46 120.3 . . ? C47 C46 H46 120.3 . . ? C46 C47 C48 120.2(10) . . ? C46 C47 H47 119.9 . . ? C48 C47 H47 119.9 . . ? C47 C48 C43 119.8(9) . . ? C47 C48 H48 120.1 . . ? C43 C48 H48 120.1 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.808 _refine_diff_density_min -1.601 _refine_diff_density_rms 0.210 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 67 20 ' ' 2 0.500 0.000 1.000 67 20 ' ' 3 0.500 0.500 0.500 67 20 ' ' 4 1.000 0.500 0.000 67 20 ' ' _platon_squeeze_details ; The remaining residual density could not be unambiguously identified and it was equated to 1 molecule of methanol per molecule of the Au complex. The potential solvent accessible volume per cell was 265.4 \%A^3^, with a total electron count of 79. The contribution of the missing solvent to the calculated structure factors was taken into account with the BYPASS algorithm (van der Sluis & Spek, 1990), implemented as the SQUEEZE option in PLATON (Spek, 2003). ; #===END======================================================================== data_1a _database_code_depnum_ccdc_archive 'CCDC 809016' #TrackingRef '- all.cif' #_296 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C96 H102 Au8 P4, 2(F6 P)' _chemical_formula_sum 'C96 H102 Au8 F12 P6' _chemical_formula_weight 3245.33 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' 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' 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 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 22.3988(12) _cell_length_b 18.9734(11) _cell_length_c 23.7764(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10104.5(10) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9361 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 26.18 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.133 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6032 _exptl_absorpt_coefficient_mu 11.727 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1219 _exptl_absorpt_correction_T_max 0.1408 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _publ_section_exptl_refinement ; The crystal contained solvent accessible voids but there was no considerable residual electron density. The potential solvent accessible volume per cell was 372.5 \%A^3^, with a total electron count of 52. The SQUEEZE routine in PLATON (Spek, 2003) was not able to handle the voids satisfactorily and the the contribution of the possible solvent was not taken into account. It is likely, that solvent has been lost. The carbon atoms C18 and C16 were disordered over two sites with equal occupacies. The carbon-carbon distances in the disordered units were restrained to be be similar. The carbon atoms C18A, C18B as well as C37 were restrained with effective standard deviation 0.01 so that their U~ij~ components approximate to isotropic behavior. The hydrogen atoms were positioned geometrically and constrained to ride on their parent atoms, with C---H = 0.93-0.96 \%A, and U~iso~ = 1.2-1.5 U~eq~(parent atom). The highest peak is located 0.90 \%A from atom Au2 and the deepest hole is located 0.77 \%A from atom Au4. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Bruker KAPPA APEX II CCD' _diffrn_measurement_device '62mm x 62mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 16 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29060 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9632 _reflns_number_gt 6792 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT (Bruker AXS, 2009)' _computing_data_reduction 'SAINT (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond v.3.2e (Brandenburg, 2010)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0233P)^2^+47.4250P] 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 9632 _refine_ls_number_parameters 567 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0786 _refine_ls_wR_factor_gt 0.0689 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.035 _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 0.498740(15) 0.908709(18) 0.316214(13) 0.04645(10) Uani 1 1 d . . . Au2 Au 0.625054(15) 0.861582(19) 0.380367(13) 0.04889(10) Uani 1 1 d . . . Au3 Au 0.532753(14) 0.954010(19) 0.428367(14) 0.04785(10) Uani 1 1 d . . . Au4 Au 0.443760(15) 0.895286(19) 0.529296(14) 0.05014(10) Uani 1 1 d . . . P1 P 0.68216(10) 0.86698(12) 0.46014(8) 0.0429(5) Uani 1 1 d . . . P2 P 0.40920(9) 0.96503(11) 0.32003(8) 0.0397(5) Uani 1 1 d . . . P3 P 0.3432(2) 0.5545(2) 0.34739(15) 0.1026(12) Uani 1 1 d . . . F1 F 0.3010(7) 0.5067(6) 0.3800(4) 0.244(7) Uani 1 1 d . . . F2 F 0.3935(6) 0.5365(7) 0.3888(5) 0.227(6) Uani 1 1 d . . . F3 F 0.3275(5) 0.6157(5) 0.3873(4) 0.178(4) Uani 1 1 d . . . F4 F 0.3856(4) 0.6050(6) 0.3163(4) 0.162(4) Uani 1 1 d . . . F5 F 0.3601(6) 0.4969(6) 0.3071(5) 0.220(6) Uani 1 1 d . . . F6 F 0.2932(4) 0.5766(6) 0.3066(4) 0.163(4) Uani 1 1 d . . . C1 C 0.5597(4) 0.8378(5) 0.2607(3) 0.049(2) Uani 1 1 d . . . C2 C 0.5828(4) 0.8495(5) 0.3066(4) 0.050(2) Uani 1 1 d . . . C3 C 0.6538(3) 0.9190(4) 0.5194(3) 0.041(2) Uani 1 1 d . . . C4 C 0.6700(4) 0.9881(4) 0.5288(3) 0.049(2) Uani 1 1 d . . . H4 H 0.6943 1.0107 0.5027 0.059 Uiso 1 1 calc R . . C5 C 0.3490(4) 0.9747(4) 0.4234(3) 0.046(2) Uani 1 1 d . . . H5 H 0.3372 0.9283 0.4174 0.055 Uiso 1 1 calc R . . C6 C 0.3861(3) 1.0093(4) 0.3852(3) 0.043(2) Uani 1 1 d . . . C7 C 0.5813(4) 1.0372(5) 0.4034(4) 0.053(2) Uani 1 1 d . . . C8 C 0.6176(4) 1.0812(6) 0.3912(4) 0.061(3) Uani 1 1 d . . . C9 C 0.4902(4) 0.8682(6) 0.4540(4) 0.062(3) Uani 1 1 d . . . C10 C 0.4685(4) 0.8103(6) 0.4676(4) 0.060(3) Uani 1 1 d . . . C11 C 0.4517(4) 0.7364(5) 0.4708(4) 0.065(3) Uani 1 1 d . . . C12 C 0.3820(5) 0.7324(6) 0.4686(6) 0.110(5) Uani 1 1 d . . . H12B H 0.3678 0.7575 0.4362 0.165 Uiso 1 1 calc R . . H12A H 0.3657 0.7532 0.5020 0.165 Uiso 1 1 calc R . . H12C H 0.3698 0.6840 0.4662 0.165 Uiso 1 1 calc R . . C13 C 0.4745(6) 0.7036(6) 0.5241(5) 0.115(5) Uani 1 1 d . . . H13B H 0.4519 0.7211 0.5555 0.172 Uiso 1 1 calc R . . H13A H 0.5159 0.7154 0.5290 0.172 Uiso 1 1 calc R . . H13C H 0.4702 0.6533 0.5220 0.172 Uiso 1 1 calc R . . C14 C 0.4763(6) 0.7000(7) 0.4190(5) 0.110(5) Uani 1 1 d . . . H14C H 0.5191 0.6998 0.4205 0.165 Uiso 1 1 calc R . . H14A H 0.4634 0.7248 0.3859 0.165 Uiso 1 1 calc R . . H14B H 0.4619 0.6524 0.4176 0.165 Uiso 1 1 calc R . . C15 C 0.6690(5) 1.1218(7) 0.3668(5) 0.079(3) Uani 1 1 d D . . C16A C 0.6542(13) 1.2005(12) 0.3620(13) 0.125(8) Uani 0.50 1 d PDU A 1 H16A H 0.6854 1.2240 0.3416 0.187 Uiso 0.50 1 calc PR A 1 H16B H 0.6509 1.2205 0.3989 0.187 Uiso 0.50 1 calc PR A 1 H16C H 0.6170 1.2062 0.3423 0.187 Uiso 0.50 1 calc PR A 1 C18A C 0.681(2) 1.094(3) 0.316(3) 0.140(16) Uani 0.50 1 d P A 1 H18A H 0.6746 1.0444 0.3170 0.210 Uiso 0.50 1 calc PR A 1 H18B H 0.7215 1.1042 0.3061 0.210 Uiso 0.50 1 calc PR A 1 H18C H 0.6546 1.1151 0.2886 0.210 Uiso 0.50 1 calc PR A 1 C16B C 0.6433(13) 1.1716(15) 0.3241(12) 0.125(8) Uani 0.50 1 d PDU A 2 H16D H 0.6751 1.1922 0.3025 0.187 Uiso 0.50 1 calc PR A 2 H16E H 0.6215 1.2082 0.3430 0.187 Uiso 0.50 1 calc PR A 2 H16F H 0.6170 1.1463 0.2994 0.187 Uiso 0.50 1 calc PR A 2 C18B C 0.704(2) 1.059(3) 0.331(3) 0.140(16) Uani 0.50 1 d P A 2 H18D H 0.6760 1.0334 0.3080 0.210 Uiso 0.50 1 calc PR A 2 H18E H 0.7232 1.0267 0.3565 0.210 Uiso 0.50 1 calc PR A 2 H18F H 0.7340 1.0797 0.3069 0.210 Uiso 0.50 1 calc PR A 2 C17 C 0.7149(7) 1.1355(10) 0.4082(6) 0.175(9) Uani 1 1 d . A . H17A H 0.7293 1.0916 0.4230 0.262 Uiso 1 1 calc R . . H17C H 0.6986 1.1633 0.4381 0.262 Uiso 1 1 calc R . . H17B H 0.7473 1.1605 0.3908 0.262 Uiso 1 1 calc R . . C19 C 0.5433(4) 0.8142(5) 0.2037(4) 0.060(3) Uani 1 1 d . . . C20 C 0.5100(6) 0.8732(7) 0.1718(5) 0.116(4) Uani 1 1 d U . . H20C H 0.5362 0.9126 0.1664 0.173 Uiso 1 1 calc R . . H20A H 0.4759 0.8879 0.1933 0.173 Uiso 1 1 calc R . . H20B H 0.4970 0.8558 0.1359 0.173 Uiso 1 1 calc R . . C21 C 0.5025(6) 0.7501(8) 0.2074(5) 0.132(6) Uani 1 1 d . . . H21C H 0.4647 0.7640 0.2228 0.198 Uiso 1 1 calc R . . H21A H 0.5204 0.7153 0.2314 0.198 Uiso 1 1 calc R . . H21B H 0.4968 0.7307 0.1706 0.198 Uiso 1 1 calc R . . C22 C 0.5980(5) 0.7931(8) 0.1726(5) 0.122(5) Uani 1 1 d . . . H22B H 0.6205 0.7602 0.1948 0.182 Uiso 1 1 calc R . . H22A H 0.6220 0.8340 0.1652 0.182 Uiso 1 1 calc R . . H22C H 0.5870 0.7714 0.1376 0.182 Uiso 1 1 calc R . . C23 C 0.6145(4) 0.8883(5) 0.5565(4) 0.052(2) Uani 1 1 d . . . H23 H 0.6015 0.8424 0.5500 0.062 Uiso 1 1 calc R . . C24 C 0.4062(4) 1.0760(4) 0.3966(3) 0.047(2) Uani 1 1 d . . . H24 H 0.4338 1.0973 0.3729 0.057 Uiso 1 1 calc R . . C25 C 0.4053(4) 1.0353(4) 0.2681(3) 0.045(2) Uani 1 1 d . . . C26 C 0.4516(5) 1.0441(5) 0.2314(4) 0.069(3) Uani 1 1 d . . . H26 H 0.4848 1.0149 0.2342 0.083 Uiso 1 1 calc R . . C27 C 0.4502(7) 1.0957(7) 0.1901(5) 0.110(5) Uani 1 1 d . . . H27 H 0.4819 1.1010 0.1652 0.132 Uiso 1 1 calc R . . C28 C 0.4021(7) 1.1378(7) 0.1866(5) 0.093(4) Uani 1 1 d . . . H28 H 0.4007 1.1720 0.1586 0.112 Uiso 1 1 calc R . . C29 C 0.3561(5) 1.1318(6) 0.2224(5) 0.083(3) Uani 1 1 d . . . H29 H 0.3235 1.1620 0.2191 0.100 Uiso 1 1 calc R . . C30 C 0.3568(4) 1.0806(5) 0.2644(4) 0.061(3) Uani 1 1 d . . . H30 H 0.3252 1.0769 0.2897 0.073 Uiso 1 1 calc R . . C31 C 0.3506(4) 0.9025(5) 0.3044(3) 0.048(2) Uani 1 1 d . . . C32 C 0.2939(5) 0.9212(6) 0.2885(5) 0.077(3) Uani 1 1 d . . . H32 H 0.2834 0.9686 0.2869 0.092 Uiso 1 1 calc R . . C33 C 0.2518(5) 0.8696(8) 0.2747(5) 0.097(4) Uani 1 1 d . . . H33 H 0.2140 0.8827 0.2624 0.117 Uiso 1 1 calc R . . C34 C 0.2663(7) 0.8000(8) 0.2793(6) 0.111(5) Uani 1 1 d . . . H34 H 0.2382 0.7654 0.2713 0.133 Uiso 1 1 calc R . . C35 C 0.3222(7) 0.7818(7) 0.2957(6) 0.119(5) Uani 1 1 d . . . H35 H 0.3325 0.7344 0.2986 0.142 Uiso 1 1 calc R . . C36 C 0.3627(5) 0.8315(6) 0.3078(5) 0.081(3) Uani 1 1 d . . . H36 H 0.4007 0.8175 0.3189 0.097 Uiso 1 1 calc R . . C37 C 0.6904(4) 0.7808(4) 0.4918(3) 0.046(2) Uani 1 1 d U . . C38 C 0.7249(4) 0.7684(5) 0.5388(4) 0.063(3) Uani 1 1 d . . . H38 H 0.7471 0.8050 0.5542 0.076 Uiso 1 1 calc R . . C39 C 0.7271(5) 0.7025(6) 0.5633(4) 0.075(3) Uani 1 1 d . . . H39 H 0.7509 0.6952 0.5948 0.090 Uiso 1 1 calc R . . C40 C 0.6954(6) 0.6494(6) 0.5423(5) 0.083(3) Uani 1 1 d . . . H40 H 0.6972 0.6052 0.5592 0.099 Uiso 1 1 calc R . . C41 C 0.6603(6) 0.6594(6) 0.4961(6) 0.101(4) Uani 1 1 d . . . H41 H 0.6378 0.6225 0.4816 0.121 Uiso 1 1 calc R . . C42 C 0.6586(5) 0.7245(6) 0.4711(5) 0.081(3) Uani 1 1 d . . . H42 H 0.6353 0.7307 0.4392 0.097 Uiso 1 1 calc R . . C43 C 0.7559(4) 0.9011(4) 0.4433(3) 0.045(2) Uani 1 1 d . . . C44 C 0.7741(5) 0.8985(7) 0.3879(4) 0.085(4) Uani 1 1 d . . . H44 H 0.7490 0.8800 0.3604 0.102 Uiso 1 1 calc R . . C45 C 0.8292(6) 0.9231(9) 0.3736(5) 0.113(5) Uani 1 1 d . . . H45 H 0.8411 0.9210 0.3362 0.136 Uiso 1 1 calc R . . C46 C 0.8671(5) 0.9507(7) 0.4122(6) 0.094(4) Uani 1 1 d . . . H46 H 0.9044 0.9676 0.4015 0.112 Uiso 1 1 calc R . . C47 C 0.8492(5) 0.9531(5) 0.4677(5) 0.074(3) Uani 1 1 d . . . H47 H 0.8746 0.9719 0.4948 0.089 Uiso 1 1 calc R . . C48 C 0.7947(4) 0.9283(5) 0.4829(4) 0.056(2) Uani 1 1 d . . . H48 H 0.7834 0.9295 0.5205 0.067 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 0.05019(19) 0.0558(2) 0.03337(18) -0.00785(16) -0.00159(15) 0.01178(16) Au2 0.05275(19) 0.0628(2) 0.03115(18) -0.01149(17) -0.00654(16) 0.01634(17) Au3 0.04349(18) 0.0610(2) 0.03901(19) -0.01513(17) 0.00281(15) 0.00039(16) Au4 0.04910(19) 0.0604(2) 0.0409(2) -0.00971(17) 0.00269(16) -0.00045(17) P1 0.0478(12) 0.0524(14) 0.0284(11) -0.0088(10) -0.0026(10) 0.0114(11) P2 0.0434(11) 0.0460(13) 0.0297(11) -0.0065(10) 0.0005(10) 0.0043(10) P3 0.151(4) 0.093(3) 0.064(2) -0.008(2) 0.000(2) -0.026(3) F1 0.415(19) 0.213(11) 0.104(7) 0.028(7) 0.016(9) -0.184(12) F2 0.278(14) 0.230(13) 0.173(10) 0.034(9) -0.114(10) 0.020(11) F3 0.269(13) 0.136(8) 0.130(7) -0.045(6) 0.045(8) -0.023(8) F4 0.120(6) 0.235(11) 0.130(7) 0.018(7) 0.005(5) -0.058(7) F5 0.332(16) 0.162(10) 0.166(10) -0.076(8) -0.013(10) 0.058(10) F6 0.119(6) 0.254(12) 0.117(7) 0.023(7) -0.022(5) -0.029(7) C1 0.055(5) 0.055(5) 0.037(5) -0.009(4) -0.002(4) 0.015(4) C2 0.050(5) 0.059(6) 0.042(5) -0.013(4) -0.005(4) 0.018(4) C3 0.042(4) 0.054(5) 0.028(4) 0.000(4) -0.001(4) 0.010(4) C4 0.070(6) 0.045(5) 0.031(5) 0.004(4) 0.011(4) 0.008(4) C5 0.063(5) 0.040(5) 0.034(5) -0.008(4) 0.008(4) -0.003(4) C6 0.039(4) 0.053(5) 0.037(5) -0.008(4) -0.008(4) 0.011(4) C7 0.057(5) 0.059(6) 0.045(5) -0.015(5) 0.006(5) 0.004(5) C8 0.058(6) 0.081(7) 0.043(6) -0.003(5) 0.007(5) -0.002(5) C9 0.052(5) 0.093(8) 0.041(6) -0.030(6) 0.003(5) 0.018(6) C10 0.060(6) 0.076(7) 0.044(6) -0.015(5) 0.005(5) -0.005(5) C11 0.073(7) 0.049(6) 0.072(7) -0.012(5) 0.011(6) -0.003(5) C12 0.098(9) 0.080(9) 0.153(13) -0.019(8) 0.013(9) -0.038(7) C13 0.163(13) 0.082(9) 0.099(10) 0.021(8) -0.027(9) -0.011(9) C14 0.111(10) 0.091(9) 0.127(12) -0.047(9) 0.017(9) -0.012(8) C15 0.061(6) 0.118(10) 0.056(7) 0.012(7) 0.017(6) -0.015(7) C16A 0.125(9) 0.123(9) 0.125(10) 0.018(7) 0.004(7) -0.008(7) C18A 0.11(3) 0.16(5) 0.15(4) -0.01(3) 0.08(3) -0.01(2) C16B 0.125(9) 0.123(9) 0.125(10) 0.018(7) 0.004(7) -0.008(7) C18B 0.11(3) 0.16(5) 0.15(4) -0.01(3) 0.08(3) -0.01(2) C17 0.124(12) 0.29(2) 0.115(12) 0.025(14) 0.000(11) -0.123(15) C19 0.062(6) 0.084(7) 0.035(5) -0.021(5) -0.009(5) 0.014(5) C20 0.146(8) 0.125(8) 0.076(7) -0.021(6) -0.038(7) 0.044(7) C21 0.128(12) 0.181(15) 0.086(10) -0.036(10) -0.019(9) -0.056(11) C22 0.101(9) 0.200(16) 0.064(8) -0.060(9) 0.005(7) 0.020(10) C23 0.050(5) 0.053(5) 0.053(6) -0.020(5) 0.002(5) -0.007(4) C24 0.050(5) 0.055(6) 0.037(5) -0.011(4) 0.009(4) -0.012(4) C25 0.056(5) 0.044(5) 0.036(5) -0.003(4) -0.007(4) 0.001(4) C26 0.089(7) 0.060(6) 0.057(6) 0.002(5) 0.019(6) 0.008(6) C27 0.155(13) 0.094(10) 0.082(9) 0.033(8) 0.047(9) 0.002(9) C28 0.125(11) 0.086(9) 0.069(8) 0.026(7) 0.000(8) 0.010(9) C29 0.074(7) 0.075(8) 0.101(9) 0.005(7) -0.042(7) 0.017(6) C30 0.049(5) 0.068(7) 0.066(7) 0.006(5) -0.011(5) 0.009(5) C31 0.059(5) 0.053(6) 0.033(5) -0.012(4) 0.010(4) 0.001(5) C32 0.068(7) 0.072(7) 0.091(8) -0.015(6) -0.005(6) -0.017(6) C33 0.083(8) 0.127(12) 0.082(9) -0.010(8) -0.006(7) -0.042(9) C34 0.125(12) 0.086(10) 0.121(11) -0.050(9) 0.043(10) -0.061(10) C35 0.118(11) 0.078(9) 0.160(14) -0.039(9) 0.058(11) -0.029(9) C36 0.076(7) 0.062(7) 0.104(9) -0.013(7) 0.025(7) -0.005(6) C37 0.049(4) 0.051(5) 0.038(4) -0.006(4) 0.001(4) 0.010(4) C38 0.068(6) 0.067(7) 0.055(6) 0.010(5) -0.014(5) -0.003(5) C39 0.084(8) 0.081(8) 0.061(7) 0.022(6) -0.007(6) 0.009(7) C40 0.092(9) 0.070(8) 0.086(9) 0.016(7) 0.018(7) 0.012(7) C41 0.134(11) 0.053(7) 0.116(11) -0.006(8) -0.009(10) 0.002(7) C42 0.102(8) 0.069(8) 0.071(7) -0.003(6) -0.023(7) 0.013(7) C43 0.051(5) 0.046(5) 0.039(5) -0.002(4) 0.000(4) 0.010(4) C44 0.070(7) 0.143(11) 0.040(6) -0.011(7) 0.014(5) 0.002(7) C45 0.078(9) 0.200(16) 0.061(8) 0.012(9) 0.023(7) 0.008(10) C46 0.059(7) 0.109(10) 0.112(11) 0.026(9) 0.029(7) 0.001(7) C47 0.062(6) 0.073(7) 0.089(9) 0.005(7) 0.001(6) 0.000(6) C48 0.051(5) 0.067(6) 0.049(6) 0.008(5) 0.002(5) 0.005(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 Au1 C2 2.203(8) . ? Au1 P2 2.274(2) . yes Au1 C1 2.328(8) . ? Au1 Au3 2.9034(5) . yes Au1 Au2 3.3363(5) . yes Au2 C2 2.005(8) . ? Au2 P1 2.290(2) . yes Au2 Au3 2.9415(5) . ? Au3 C9 1.983(12) . ? Au3 C7 2.006(10) . ? Au3 Au4 3.0767(5) 5_676 yes Au3 Au4 3.3126(5) . yes Au4 C7 2.126(8) 5_676 ? Au4 C9 2.134(8) . ? Au4 C10 2.248(9) . ? Au4 C8 2.380(9) 5_676 ? Au4 Au3 3.0767(5) 5_676 yes P1 C37 1.810(9) . ? P1 C43 1.818(9) . ? P1 C3 1.834(8) . ? P2 C31 1.809(9) . ? P2 C25 1.820(8) . ? P2 C6 1.836(8) . ? P3 F5 1.503(10) . ? P3 F1 1.521(10) . ? P3 F2 1.534(11) . ? P3 F6 1.539(9) . ? P3 F4 1.539(9) . ? P3 F3 1.541(9) . ? C1 C2 1.228(11) . ? C1 C19 1.475(11) . ? C3 C23 1.376(11) . ? C3 C4 1.379(11) . ? C4 C5 1.405(10) 5_676 ? C4 H4 0.9300 . ? C5 C6 1.396(11) . ? C5 C4 1.405(10) 5_676 ? C5 H5 0.9300 . ? C6 C24 1.371(11) . ? C7 C8 1.203(12) . ? C7 Au4 2.126(8) 5_676 ? C8 C15 1.501(14) . ? C8 Au4 2.380(9) 5_676 ? C9 C10 1.243(13) . ? C10 C11 1.455(14) . ? C11 C13 1.502(14) . ? C11 C14 1.516(14) . ? C11 C12 1.563(13) . ? C12 H12B 0.9600 . ? C12 H12A 0.9600 . ? C12 H12C 0.9600 . ? C13 H13B 0.9600 . ? C13 H13A 0.9600 . ? C13 H13C 0.9600 . ? C14 H14C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C15 C18A 1.34(6) . ? C15 C17 1.447(16) . ? C15 C16B 1.50(2) . ? C15 C16A 1.53(2) . ? C15 C18B 1.67(5) . ? C16A H16A 0.9600 . ? C16A H16B 0.9600 . ? C16A H16C 0.9600 . ? C18A H18A 0.9600 . ? C18A H18B 0.9600 . ? C18A H18C 0.9600 . ? C16B H16D 0.9600 . ? C16B H16E 0.9600 . ? C16B H16F 0.9600 . ? C18B H18D 0.9600 . ? C18B H18E 0.9600 . ? C18B H18F 0.9600 . ? C17 H17A 0.9600 . ? C17 H17C 0.9600 . ? C17 H17B 0.9600 . ? C19 C22 1.486(13) . ? C19 C21 1.523(15) . ? C19 C20 1.545(14) . ? C20 H20C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C21 H21C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C22 H22B 0.9600 . ? C22 H22A 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.384(11) 5_676 ? C23 H23 0.9300 . ? C24 C23 1.384(11) 5_676 ? C24 H24 0.9300 . ? C25 C26 1.364(12) . ? C25 C30 1.389(11) . ? C26 C27 1.388(14) . ? C26 H26 0.9300 . ? C27 C28 1.344(17) . ? C27 H27 0.9300 . ? C28 C29 1.342(15) . ? C28 H28 0.9300 . ? C29 C30 1.395(14) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.371(13) . ? C31 C36 1.376(13) . ? C32 C33 1.399(14) . ? C32 H32 0.9300 . ? C33 C34 1.363(17) . ? C33 H33 0.9300 . ? C34 C35 1.356(19) . ? C34 H34 0.9300 . ? C35 C36 1.341(15) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C42 1.375(13) . ? C37 C38 1.378(11) . ? C38 C39 1.379(13) . ? C38 H38 0.9300 . ? C39 C40 1.331(14) . ? C39 H39 0.9300 . ? C40 C41 1.364(16) . ? C40 H40 0.9300 . ? C41 C42 1.369(14) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C44 1.381(12) . ? C43 C48 1.382(11) . ? C44 C45 1.361(15) . ? C44 H44 0.9300 . ? C45 C46 1.355(16) . ? C45 H45 0.9300 . ? C46 C47 1.380(15) . ? C46 H46 0.9300 . ? C47 C48 1.358(12) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? 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 C2 Au1 P2 175.4(2) . . ? C2 Au1 C1 31.3(3) . . ? P2 Au1 C1 144.3(2) . . ? C2 Au1 Au3 91.2(2) . . ? P2 Au1 Au3 93.19(5) . . ? C1 Au1 Au3 122.5(2) . . ? C2 Au1 Au2 35.5(2) . . ? P2 Au1 Au2 148.82(5) . . ? C1 Au1 Au2 66.8(2) . . ? Au3 Au1 Au2 55.732(10) . . ? C2 Au2 P1 173.1(2) . . ? C2 Au2 Au3 94.3(2) . . ? P1 Au2 Au3 92.55(5) . . ? C2 Au2 Au1 39.7(2) . . ? P1 Au2 Au1 147.18(5) . . ? Au3 Au2 Au1 54.659(10) . . ? C9 Au3 C7 175.9(4) . . ? C9 Au3 Au1 85.0(3) . . ? C7 Au3 Au1 95.9(2) . . ? C9 Au3 Au2 88.1(2) . . ? C7 Au3 Au2 88.5(2) . . ? Au1 Au3 Au2 69.609(11) . . ? C9 Au3 Au4 138.2(2) . 5_676 ? C7 Au3 Au4 43.4(2) . 5_676 ? Au1 Au3 Au4 128.351(16) . 5_676 ? Au2 Au3 Au4 124.114(15) . 5_676 ? C9 Au3 Au4 38.0(2) . . ? C7 Au3 Au4 143.6(2) . . ? Au1 Au3 Au4 114.071(14) . . ? Au2 Au3 Au4 120.230(15) . . ? Au4 Au3 Au4 100.281(12) 5_676 . ? C7 Au4 C9 154.9(4) 5_676 . ? C7 Au4 C10 171.2(4) 5_676 . ? C9 Au4 C10 32.8(3) . . ? C7 Au4 C8 30.3(3) 5_676 5_676 ? C9 Au4 C8 173.4(4) . 5_676 ? C10 Au4 C8 142.6(4) . 5_676 ? C7 Au4 Au3 40.4(3) 5_676 5_676 ? C9 Au4 Au3 114.5(3) . 5_676 ? C10 Au4 Au3 146.9(3) . 5_676 ? C8 Au4 Au3 70.4(3) 5_676 5_676 ? C7 Au4 Au3 120.1(3) 5_676 . ? C9 Au4 Au3 34.9(3) . . ? C10 Au4 Au3 67.7(3) . . ? C8 Au4 Au3 149.3(3) 5_676 . ? Au3 Au4 Au3 79.720(12) 5_676 . ? C37 P1 C43 108.7(4) . . ? C37 P1 C3 101.6(4) . . ? C43 P1 C3 107.0(4) . . ? C37 P1 Au2 111.2(3) . . ? C43 P1 Au2 109.9(3) . . ? C3 P1 Au2 117.8(3) . . ? C31 P2 C25 107.8(4) . . ? C31 P2 C6 105.6(4) . . ? C25 P2 C6 103.0(4) . . ? C31 P2 Au1 108.9(3) . . ? C25 P2 Au1 111.1(3) . . ? C6 P2 Au1 119.8(2) . . ? F5 P3 F1 92.8(7) . . ? F5 P3 F2 93.5(7) . . ? F1 P3 F2 89.8(7) . . ? F5 P3 F6 88.8(6) . . ? F1 P3 F6 91.9(7) . . ? F2 P3 F6 177.0(7) . . ? F5 P3 F4 89.5(7) . . ? F1 P3 F4 177.7(6) . . ? F2 P3 F4 89.6(7) . . ? F6 P3 F4 88.7(5) . . ? F5 P3 F3 177.6(7) . . ? F1 P3 F3 89.7(6) . . ? F2 P3 F3 86.6(7) . . ? F6 P3 F3 91.0(7) . . ? F4 P3 F3 88.1(6) . . ? C2 C1 C19 167.8(9) . . ? C2 C1 Au1 68.7(5) . . ? C19 C1 Au1 123.4(6) . . ? C1 C2 Au2 175.0(7) . . ? C1 C2 Au1 80.0(6) . . ? Au2 C2 Au1 104.8(3) . . ? C23 C3 C4 117.9(8) . . ? C23 C3 P1 119.1(7) . . ? C4 C3 P1 123.0(6) . . ? C3 C4 C5 121.9(8) . 5_676 ? C3 C4 H4 119.0 . . ? C5 C4 H4 119.0 5_676 . ? C6 C5 C4 118.1(8) . 5_676 ? C6 C5 H5 120.9 . . ? C4 C5 H5 120.9 5_676 . ? C24 C6 C5 120.0(7) . . ? C24 C6 P2 119.8(7) . . ? C5 C6 P2 120.2(6) . . ? C8 C7 Au3 170.1(9) . . ? C8 C7 Au4 86.7(7) . 5_676 ? Au3 C7 Au4 96.2(4) . 5_676 ? C7 C8 C15 165.7(11) . . ? C7 C8 Au4 63.1(6) . 5_676 ? C15 C8 Au4 130.8(8) . 5_676 ? C10 C9 Au3 173.2(8) . . ? C10 C9 Au4 78.6(6) . . ? Au3 C9 Au4 107.1(4) . . ? C9 C10 C11 165.0(10) . . ? C9 C10 Au4 68.5(6) . . ? C11 C10 Au4 126.4(7) . . ? C10 C11 C13 110.8(9) . . ? C10 C11 C14 107.7(9) . . ? C13 C11 C14 112.0(10) . . ? C10 C11 C12 107.6(8) . . ? C13 C11 C12 110.3(10) . . ? C14 C11 C12 108.3(9) . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12A 109.5 . . ? H12B C12 H12A 109.5 . . ? C11 C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? C11 C13 H13B 109.5 . . ? C11 C13 H13A 109.5 . . ? H13B C13 H13A 109.5 . . ? C11 C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? C11 C14 H14C 109.5 . . ? C11 C14 H14A 109.5 . . ? H14C C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14C C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C18A C15 C17 123(3) . . ? C18A C15 C16B 73(2) . . ? C17 C15 C16B 128.3(17) . . ? C18A C15 C8 107(3) . . ? C17 C15 C8 111.9(9) . . ? C16B C15 C8 106.9(14) . . ? C18A C15 C16A 111(2) . . ? C17 C15 C16A 91.8(16) . . ? C8 C15 C16A 111.3(14) . . ? C17 C15 C18B 98(2) . . ? C16B C15 C18B 107(2) . . ? C8 C15 C18B 101(2) . . ? C16A C15 C18B 140(2) . . ? C15 C16A H16A 109.5 . . ? C15 C16A H16B 109.5 . . ? C15 C16A H16C 109.5 . . ? C15 C18A H18A 109.5 . . ? C15 C18A H18B 109.5 . . ? C15 C18A H18C 109.5 . . ? C15 C16B H16D 109.5 . . ? C15 C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C15 C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C15 C18B H18D 109.5 . . ? C15 C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C15 C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? H17C C17 H17B 109.5 . . ? C1 C19 C22 109.5(8) . . ? C1 C19 C21 109.7(9) . . ? C22 C19 C21 108.0(10) . . ? C1 C19 C20 110.6(8) . . ? C22 C19 C20 110.5(10) . . ? C21 C19 C20 108.5(10) . . ? C19 C20 H20C 109.5 . . ? C19 C20 H20A 109.5 . . ? H20C C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20C C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C21 H21C 109.5 . . ? C19 C21 H21A 109.5 . . ? H21C C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21C C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C22 H22B 109.5 . . ? C19 C22 H22A 109.5 . . ? H22B C22 H22A 109.5 . . ? C19 C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? C3 C23 C24 121.6(8) . 5_676 ? C3 C23 H23 119.2 . . ? C24 C23 H23 119.2 5_676 . ? C6 C24 C23 120.2(8) . 5_676 ? C6 C24 H24 119.9 . . ? C23 C24 H24 119.9 5_676 . ? C26 C25 C30 118.6(8) . . ? C26 C25 P2 119.1(7) . . ? C30 C25 P2 122.2(7) . . ? C25 C26 C27 121.5(10) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C28 C27 C26 118.8(12) . . ? C28 C27 H27 120.6 . . ? C26 C27 H27 120.6 . . ? C29 C28 C27 121.8(12) . . ? C29 C28 H28 119.1 . . ? C27 C28 H28 119.1 . . ? C28 C29 C30 120.3(10) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C25 C30 C29 119.0(9) . . ? C25 C30 H30 120.5 . . ? C29 C30 H30 120.5 . . ? C32 C31 C36 117.0(9) . . ? C32 C31 P2 123.9(7) . . ? C36 C31 P2 119.1(8) . . ? C31 C32 C33 120.4(11) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C34 C33 C32 119.9(13) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C35 C34 C33 119.4(12) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? C36 C35 C34 120.4(14) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C35 C36 C31 122.8(12) . . ? C35 C36 H36 118.6 . . ? C31 C36 H36 118.6 . . ? C42 C37 C38 116.6(9) . . ? C42 C37 P1 120.0(7) . . ? C38 C37 P1 123.3(7) . . ? C37 C38 C39 121.1(10) . . ? C37 C38 H38 119.4 . . ? C39 C38 H38 119.4 . . ? C40 C39 C38 120.6(10) . . ? C40 C39 H39 119.7 . . ? C38 C39 H39 119.7 . . ? C39 C40 C41 120.3(11) . . ? C39 C40 H40 119.9 . . ? C41 C40 H40 119.9 . . ? C40 C41 C42 119.4(12) . . ? C40 C41 H41 120.3 . . ? C42 C41 H41 120.3 . . ? C41 C42 C37 122.0(10) . . ? C41 C42 H42 119.0 . . ? C37 C42 H42 119.0 . . ? C44 C43 C48 118.5(9) . . ? C44 C43 P1 117.8(7) . . ? C48 C43 P1 123.7(6) . . ? C45 C44 C43 119.6(11) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C46 C45 C44 122.1(11) . . ? C46 C45 H45 119.0 . . ? C44 C45 H45 119.0 . . ? C45 C46 C47 118.7(11) . . ? C45 C46 H46 120.7 . . ? C47 C46 H46 120.7 . . ? C48 C47 C46 120.2(11) . . ? C48 C47 H47 119.9 . . ? C46 C47 H47 119.9 . . ? C47 C48 C43 120.9(9) . . ? C47 C48 H48 119.5 . . ? C43 C48 H48 119.5 . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.579 _refine_diff_density_min -1.012 _refine_diff_density_rms 0.140 #===END======================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 809017' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C80 H94 Au8 N8 P4, 0.5(C4 H10 O), 2(F6 P), 2.5(C H2 Cl2)' _chemical_formula_sum 'C84.50 H104 Au8 Cl5 F12 N8 O0.50 P6' _chemical_formula_weight 3406.56 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' N N 0.0061 0.0033 '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' 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 24.3129(6) _cell_length_b 16.0611(4) _cell_length_c 28.0596(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.2450(10) _cell_angle_gamma 90.00 _cell_volume 10948.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9785 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 27.35 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.067 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6344 _exptl_absorpt_coefficient_mu 10.948 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.1883 _exptl_absorpt_correction_T_max 0.5595 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _publ_section_exptl_refinement ; One of the CH~2~Cl~2~ and one of the Et~2~O solvent molecules were partially lost and therefore refined with occupancies 0.5. Furthermore, the carbon atom of the partially lost CH~2~Cl~2~ was disordered over two sites with equal occupancies. Some methyl carbons of the t-butyl moieties were slightly disordered. No satisfactory disorder model was found for these carbons, which led to relatively large displacement parameters. Some of the Au atoms were accompanied by relatively large residual electron densities due to the absorption despite the analytical absorption correction. Hydrogen atoms were positioned geometrically and were also constrained to ride on their parent atoms, with C---H = 0.95-0.99 \%A, and U~iso~ = 1.2-1.5 U~eq~(parent atom). The highest peak is located 0.89 \%A from atom Au7 and the deepest hole is located 0.53 \%A from atom Au8. ; _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 'flat graphite crystal' _diffrn_measurement_device_type 'Bruker SMART APEX II CCD' _diffrn_measurement_device '62mm x 62mm CCD camera on three-circle goniostat' _diffrn_detector_area_resol_mean 16 # 8 for binned mode _diffrn_measurement_method '\f scans and \w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 91935 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0429 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 27.42 _reflns_number_total 24912 _reflns_number_gt 18954 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT (Bruker AXS, 2009)' _computing_data_reduction 'SAINT (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond v.3.2f (Brandenburg, 2010)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0401P)^2^+138.2224P] 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 24912 _refine_ls_number_parameters 1176 _refine_ls_number_restraints 62 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1100 _refine_ls_wR_factor_gt 0.0988 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.031 _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 0.521482(12) 0.36111(2) 0.905543(11) 0.02401(7) Uani 1 1 d . . . Au2 Au 0.388842(12) 0.35389(2) 0.869715(11) 0.02486(8) Uani 1 1 d . . . Au3 Au 0.480160(12) 0.325514(19) 0.806891(11) 0.02150(7) Uani 1 1 d . . . Au4 Au 0.486836(13) 0.12739(2) 0.783533(12) 0.02657(8) Uani 1 1 d . . . Au5 Au 0.517790(13) 0.40290(2) 0.707451(12) 0.02836(8) Uani 1 1 d . . . Au6 Au 0.525749(13) 0.20690(2) 0.686114(12) 0.02902(8) Uani 1 1 d . . . Au7 Au 0.613727(13) 0.12975(2) 0.636366(11) 0.02655(8) Uani 1 1 d . . . Au8 Au 0.483330(13) 0.12954(2) 0.597662(12) 0.03128(9) Uani 1 1 d . . . P1 P 0.60824(8) 0.36464(14) 0.88102(8) 0.0243(4) Uani 1 1 d . . . P2 P 0.33023(9) 0.34682(14) 0.80556(8) 0.0254(5) Uani 1 1 d . . . P3 P 0.67438(8) 0.16290(13) 0.69591(8) 0.0230(4) Uani 1 1 d . . . P4 P 0.39638(9) 0.16510(15) 0.61347(8) 0.0297(5) Uani 1 1 d . . . P5 P 0.17727(11) 0.31087(17) 0.64392(11) 0.0422(6) Uani 1 1 d . . . P6 P 0.84045(10) 0.23813(16) 0.84334(9) 0.0340(5) Uani 1 1 d . . . F1 F 0.1826(3) 0.3960(4) 0.6726(3) 0.077(2) Uani 1 1 d . . . F2 F 0.1721(3) 0.2241(5) 0.6171(3) 0.080(3) Uani 1 1 d . . . F3 F 0.2358(2) 0.2819(4) 0.6669(2) 0.0585(18) Uani 1 1 d . . . F4 F 0.2062(3) 0.3505(6) 0.5997(3) 0.087(3) Uani 1 1 d . . . F5 F 0.1187(2) 0.3401(4) 0.6227(3) 0.0591(18) Uani 1 1 d . . . F6 F 0.1489(3) 0.2711(4) 0.6883(3) 0.0649(19) Uani 1 1 d . . . F7 F 0.8177(3) 0.2009(4) 0.8912(2) 0.0573(17) Uani 1 1 d . . . F8 F 0.8620(2) 0.2750(4) 0.7948(2) 0.0500(15) Uani 1 1 d . . . F9 F 0.9021(2) 0.2272(4) 0.8636(2) 0.0570(17) Uani 1 1 d . . . F10 F 0.8380(3) 0.3290(4) 0.8656(3) 0.0640(19) Uani 1 1 d . . . F11 F 0.7776(2) 0.2490(3) 0.82285(19) 0.0379(13) Uani 1 1 d . . . F12 F 0.8410(2) 0.1471(4) 0.8209(2) 0.0459(14) Uani 1 1 d . . . N1 N 0.6262(3) 0.4650(5) 0.8691(3) 0.0283(16) Uani 1 1 d . . . N2 N 0.6533(3) 0.3298(5) 0.9222(3) 0.0326(17) Uani 1 1 d . . . N3 N 0.3120(3) 0.4423(4) 0.7867(3) 0.0284(16) Uani 1 1 d . . . N4 N 0.2725(3) 0.2955(5) 0.8194(3) 0.0317(17) Uani 1 1 d . . . N5 N 0.7243(3) 0.2242(4) 0.6745(3) 0.0283(16) Uani 1 1 d . . . N6 N 0.7032(3) 0.0762(4) 0.7191(3) 0.0267(15) Uani 1 1 d . . . N7 N 0.3711(3) 0.2323(5) 0.5721(3) 0.0366(18) Uani 1 1 d . . . N8 N 0.3572(3) 0.0796(5) 0.6142(3) 0.039(2) Uani 1 1 d . . . C1 C 0.4465(4) 0.3660(6) 0.9314(3) 0.0295(19) Uani 1 1 d . . . C2 C 0.4016(4) 0.3756(6) 0.9498(3) 0.033(2) Uani 1 1 d . . . C3 C 0.3577(4) 0.3945(7) 0.9836(4) 0.043(3) Uani 1 1 d . . . C4 C 0.3311(5) 0.3147(8) 0.9999(5) 0.064(4) Uani 1 1 d . . . H4A H 0.3155 0.2847 0.9722 0.096 Uiso 1 1 calc R . . H4B H 0.3017 0.3280 1.0217 0.096 Uiso 1 1 calc R . . H4C H 0.3588 0.2798 1.0165 0.096 Uiso 1 1 calc R . . C5 C 0.3153(4) 0.4537(8) 0.9601(4) 0.055(3) Uani 1 1 d . . . H5A H 0.3340 0.5038 0.9490 0.083 Uiso 1 1 calc R . . H5B H 0.2881 0.4694 0.9833 0.083 Uiso 1 1 calc R . . H5C H 0.2968 0.4258 0.9328 0.083 Uiso 1 1 calc R . . C6 C 0.3872(5) 0.4360(8) 1.0267(4) 0.060(3) Uani 1 1 d . . . H6A H 0.4177 0.4005 1.0383 0.090 Uiso 1 1 calc R . . H6B H 0.3612 0.4437 1.0522 0.090 Uiso 1 1 calc R . . H6C H 0.4016 0.4903 1.0172 0.090 Uiso 1 1 calc R . . C7 C 0.5895(4) 0.5285(6) 0.8601(4) 0.037(2) Uani 1 1 d . . . H7 H 0.5505 0.5251 0.8611 0.045 Uiso 1 1 calc R . . C8 C 0.6191(4) 0.5964(6) 0.8496(4) 0.044(3) Uani 1 1 d . . . H8 H 0.6046 0.6498 0.8418 0.053 Uiso 1 1 calc R . . C9 C 0.6751(5) 0.5746(7) 0.8522(4) 0.046(3) Uani 1 1 d . . . H9 H 0.7049 0.6110 0.8463 0.055 Uiso 1 1 calc R . . C10 C 0.6797(4) 0.4944(6) 0.8643(3) 0.033(2) Uani 1 1 d . . . H10 H 0.7128 0.4634 0.8688 0.039 Uiso 1 1 calc R . . C11 C 0.6468(4) 0.3373(7) 0.9713(4) 0.044(3) Uani 1 1 d . . . H11 H 0.6139 0.3525 0.9862 0.053 Uiso 1 1 calc R . . C12 C 0.6957(4) 0.3191(7) 0.9943(4) 0.049(3) Uani 1 1 d . . . H12 H 0.7025 0.3175 1.0278 0.059 Uiso 1 1 calc R . . C13 C 0.7348(4) 0.3028(7) 0.9590(4) 0.046(3) Uani 1 1 d . . . H13 H 0.7725 0.2891 0.9647 0.056 Uiso 1 1 calc R . . C14 C 0.7088(4) 0.3102(6) 0.9160(4) 0.037(2) Uani 1 1 d . . . H14 H 0.7255 0.3033 0.8862 0.045 Uiso 1 1 calc R . . C15 C 0.6252(3) 0.3080(5) 0.8283(3) 0.0238(17) Uani 1 1 d . . . C16 C 0.6385(3) 0.3502(5) 0.7867(3) 0.0282(19) Uani 1 1 d . . . H16 H 0.6379 0.4093 0.7857 0.034 Uiso 1 1 calc R . . C17 C 0.6527(3) 0.3050(5) 0.7468(3) 0.0241(17) Uani 1 1 d . . . H17 H 0.6614 0.3334 0.7184 0.029 Uiso 1 1 calc R . . C18 C 0.6543(3) 0.2193(5) 0.7481(3) 0.0217(17) Uani 1 1 d . . . C19 C 0.6383(3) 0.1770(5) 0.7889(3) 0.0259(18) Uani 1 1 d . . . H19 H 0.6374 0.1179 0.7891 0.031 Uiso 1 1 calc R . . C20 C 0.6237(3) 0.2208(5) 0.8286(3) 0.0248(17) Uani 1 1 d . . . H20 H 0.6127 0.1919 0.8562 0.030 Uiso 1 1 calc R . . C21 C 0.7274(4) 0.2508(6) 0.6276(4) 0.041(2) Uani 1 1 d . . . H21 H 0.7017 0.2383 0.6022 0.049 Uiso 1 1 calc R . . C22 C 0.7728(5) 0.2970(7) 0.6243(4) 0.055(3) Uani 1 1 d . . . H22 H 0.7850 0.3226 0.5960 0.067 Uiso 1 1 calc R . . C23 C 0.7999(4) 0.3015(7) 0.6702(4) 0.048(3) Uani 1 1 d . . . H23 H 0.8330 0.3306 0.6780 0.058 Uiso 1 1 calc R . . C24 C 0.7699(4) 0.2571(6) 0.7003(4) 0.037(2) Uani 1 1 d . . . H24 H 0.7781 0.2493 0.7334 0.044 Uiso 1 1 calc R . . C25 C 0.6936(4) -0.0038(5) 0.7025(3) 0.0277(18) Uani 1 1 d . . . H25 H 0.6692 -0.0189 0.6767 0.033 Uiso 1 1 calc R . . C26 C 0.7249(4) -0.0565(6) 0.7292(3) 0.037(2) Uani 1 1 d . . . H26 H 0.7264 -0.1153 0.7255 0.045 Uiso 1 1 calc R . . C27 C 0.7549(4) -0.0099(6) 0.7634(3) 0.040(2) Uani 1 1 d . . . H27 H 0.7800 -0.0315 0.7872 0.048 Uiso 1 1 calc R . . C28 C 0.7420(4) 0.0715(6) 0.7567(3) 0.032(2) Uani 1 1 d . . . H28 H 0.7568 0.1171 0.7745 0.039 Uiso 1 1 calc R . . C29 C 0.5578(4) 0.0937(7) 0.5768(3) 0.039(2) Uani 1 1 d . . . C30 C 0.6022(4) 0.0694(6) 0.5627(3) 0.033(2) Uani 1 1 d . . . C31 C 0.6482(4) 0.0391(6) 0.5341(3) 0.034(2) Uani 1 1 d . . . C32 C 0.6971(4) 0.0107(7) 0.5659(4) 0.044(3) Uani 1 1 d . . . H32A H 0.7129 0.0588 0.5830 0.066 Uiso 1 1 calc R . . H32B H 0.7250 -0.0144 0.5461 0.066 Uiso 1 1 calc R . . H32C H 0.6847 -0.0304 0.5889 0.066 Uiso 1 1 calc R . . C33 C 0.6637(5) 0.1077(8) 0.4999(4) 0.054(3) Uani 1 1 d . . . H33A H 0.6305 0.1279 0.4826 0.081 Uiso 1 1 calc R . . H33B H 0.6896 0.0857 0.4771 0.081 Uiso 1 1 calc R . . H33C H 0.6810 0.1537 0.5179 0.081 Uiso 1 1 calc R . . C34 C 0.6263(5) -0.0383(8) 0.5077(4) 0.066(4) Uani 1 1 d . . . H34A H 0.6150 -0.0799 0.5309 0.098 Uiso 1 1 calc R . . H34B H 0.6554 -0.0616 0.4884 0.098 Uiso 1 1 calc R . . H34C H 0.5947 -0.0229 0.4868 0.098 Uiso 1 1 calc R . . C35 C 0.3009(4) 0.0766(8) 0.6204(4) 0.056(3) Uani 1 1 d . . . H35 H 0.2757 0.1218 0.6184 0.067 Uiso 1 1 calc R . . C36 C 0.2893(6) -0.0047(9) 0.6299(4) 0.064(4) Uani 1 1 d . . . H36 H 0.2538 -0.0262 0.6355 0.076 Uiso 1 1 calc R . . C37 C 0.3380(6) -0.0517(8) 0.6299(4) 0.066(4) Uani 1 1 d . . . H37 H 0.3411 -0.1098 0.6357 0.079 Uiso 1 1 calc R . . C38 C 0.3794(5) 0.0001(7) 0.6203(4) 0.045(3) Uani 1 1 d . . . H38 H 0.4171 -0.0147 0.6181 0.054 Uiso 1 1 calc R . . C39 C 0.3221(4) 0.2780(7) 0.5721(4) 0.045(3) Uani 1 1 d . . . H39 H 0.2964 0.2782 0.5967 0.054 Uiso 1 1 calc R . . C40 C 0.3177(5) 0.3214(7) 0.5314(4) 0.055(3) Uani 1 1 d . . . H40 H 0.2883 0.3578 0.5223 0.066 Uiso 1 1 calc R . . C41 C 0.3650(5) 0.3036(7) 0.5038(4) 0.058(3) Uani 1 1 d . . . H41 H 0.3723 0.3264 0.4734 0.069 Uiso 1 1 calc R . . C42 C 0.3970(4) 0.2492(7) 0.5282(4) 0.044(2) Uani 1 1 d . . . H42 H 0.4307 0.2261 0.5182 0.053 Uiso 1 1 calc R . . C43 C 0.3802(3) 0.2163(6) 0.6689(3) 0.0298(19) Uani 1 1 d . . . C44 C 0.3618(4) 0.1699(6) 0.7068(3) 0.032(2) Uani 1 1 d . . . H44 H 0.3593 0.1110 0.7043 0.039 Uiso 1 1 calc R . . C45 C 0.3470(4) 0.2099(5) 0.7485(3) 0.0282(19) Uani 1 1 d . . . H45 H 0.3346 0.1784 0.7746 0.034 Uiso 1 1 calc R . . C46 C 0.3504(3) 0.2957(5) 0.7514(3) 0.0244(17) Uani 1 1 d . . . C47 C 0.3719(3) 0.3403(6) 0.7144(3) 0.0293(19) Uani 1 1 d . . . H47 H 0.3764 0.3989 0.7174 0.035 Uiso 1 1 calc R . . C48 C 0.3867(3) 0.3012(6) 0.6735(3) 0.0297(19) Uani 1 1 d . . . H48 H 0.4015 0.3326 0.6483 0.036 Uiso 1 1 calc R . . C49 C 0.2608(4) 0.2656(6) 0.8644(4) 0.042(2) Uani 1 1 d . . . H49 H 0.2844 0.2694 0.8921 0.050 Uiso 1 1 calc R . . C50 C 0.2105(4) 0.2305(6) 0.8625(4) 0.048(3) Uani 1 1 d . . . H50 H 0.1921 0.2064 0.8884 0.057 Uiso 1 1 calc R . . C51 C 0.1903(4) 0.2363(6) 0.8148(4) 0.045(3) Uani 1 1 d . . . H51 H 0.1558 0.2157 0.8028 0.054 Uiso 1 1 calc R . . C52 C 0.2277(4) 0.2754(7) 0.7892(4) 0.041(2) Uani 1 1 d . . . H52 H 0.2242 0.2874 0.7561 0.050 Uiso 1 1 calc R . . C53 C 0.2760(4) 0.4625(6) 0.7492(4) 0.043(2) Uani 1 1 d . . . H53 H 0.2568 0.4239 0.7290 0.052 Uiso 1 1 calc R . . C54 C 0.2727(4) 0.5463(6) 0.7459(4) 0.046(3) Uani 1 1 d . . . H54 H 0.2513 0.5771 0.7230 0.055 Uiso 1 1 calc R . . C55 C 0.3073(5) 0.5802(6) 0.7835(4) 0.047(3) Uani 1 1 d . . . H55 H 0.3128 0.6378 0.7900 0.057 Uiso 1 1 calc R . . C56 C 0.3304(4) 0.5173(5) 0.8077(4) 0.036(2) Uani 1 1 d . . . H56 H 0.3552 0.5222 0.8346 0.043 Uiso 1 1 calc R . . C57 C 0.4674(4) 0.2140(5) 0.8369(3) 0.0273(18) Uani 1 1 d . . . C58 C 0.4550(4) 0.1513(6) 0.8579(3) 0.036(2) Uani 1 1 d . . . C59 C 0.4356(5) 0.0867(6) 0.8916(4) 0.049(3) Uani 1 1 d . . . C60 C 0.3778(6) 0.0578(8) 0.8721(5) 0.075(4) Uani 1 1 d . . . H60A H 0.3529 0.1058 0.8699 0.112 Uiso 1 1 calc R . . H60B H 0.3629 0.0163 0.8938 0.112 Uiso 1 1 calc R . . H60C H 0.3811 0.0331 0.8405 0.112 Uiso 1 1 calc R . . C61 C 0.4288(7) 0.1286(7) 0.9395(4) 0.073(4) Uani 1 1 d . . . H61A H 0.4650 0.1449 0.9530 0.110 Uiso 1 1 calc R . . H61B H 0.4114 0.0899 0.9613 0.110 Uiso 1 1 calc R . . H61C H 0.4057 0.1783 0.9352 0.110 Uiso 1 1 calc R . . C62 C 0.4747(6) 0.0135(7) 0.8953(4) 0.064(4) Uani 1 1 d . . . H62A H 0.5125 0.0339 0.9002 0.096 Uiso 1 1 calc R . . H62B H 0.4718 -0.0191 0.8658 0.096 Uiso 1 1 calc R . . H62C H 0.4652 -0.0217 0.9223 0.096 Uiso 1 1 calc R . . C63 C 0.5139(4) 0.0954(6) 0.7148(3) 0.032(2) Uani 1 1 d . . . C64 C 0.5083(4) 0.0235(7) 0.7297(3) 0.038(2) Uani 1 1 d . . . C65 C 0.5049(5) -0.0686(6) 0.7367(4) 0.049(3) Uani 1 1 d . . . C66 C 0.4485(5) -0.0927(7) 0.7517(5) 0.066(4) Uani 1 1 d . . . H66A H 0.4394 -0.0611 0.7802 0.099 Uiso 1 1 calc R . . H66B H 0.4478 -0.1524 0.7589 0.099 Uiso 1 1 calc R . . H66C H 0.4215 -0.0803 0.7258 0.099 Uiso 1 1 calc R . . C67 C 0.5498(6) -0.0943(8) 0.7737(4) 0.066(4) Uani 1 1 d . . . H67A H 0.5420 -0.0695 0.8046 0.099 Uiso 1 1 calc R . . H67B H 0.5856 -0.0747 0.7635 0.099 Uiso 1 1 calc R . . H67C H 0.5504 -0.1551 0.7766 0.099 Uiso 1 1 calc R . . C68 C 0.5190(6) -0.1071(8) 0.6877(4) 0.067(4) Uani 1 1 d . . . H68A H 0.4887 -0.0964 0.6645 0.101 Uiso 1 1 calc R . . H68B H 0.5242 -0.1674 0.6914 0.101 Uiso 1 1 calc R . . H68C H 0.5528 -0.0819 0.6766 0.101 Uiso 1 1 calc R . . C69 C 0.4884(3) 0.4361(5) 0.7765(3) 0.0272(18) Uani 1 1 d . . . C70 C 0.4911(3) 0.5051(6) 0.7583(3) 0.031(2) Uani 1 1 d . . . C71 C 0.4884(4) 0.5955(6) 0.7459(4) 0.040(2) Uani 1 1 d . . . C72 C 0.4724(4) 0.6433(6) 0.7905(4) 0.045(3) Uani 1 1 d . . . H72A H 0.4366 0.6237 0.8007 0.068 Uiso 1 1 calc R . . H72B H 0.4702 0.7029 0.7833 0.068 Uiso 1 1 calc R . . H72C H 0.5002 0.6339 0.8162 0.068 Uiso 1 1 calc R . . C73 C 0.4451(5) 0.6106(8) 0.7060(5) 0.062(3) Uani 1 1 d . . . H73A H 0.4553 0.5805 0.6773 0.092 Uiso 1 1 calc R . . H73B H 0.4427 0.6703 0.6991 0.092 Uiso 1 1 calc R . . H73C H 0.4092 0.5906 0.7161 0.092 Uiso 1 1 calc R . . C74 C 0.5447(4) 0.6249(6) 0.7303(4) 0.051(3) Uani 1 1 d . . . H74A H 0.5724 0.6139 0.7558 0.077 Uiso 1 1 calc R . . H74B H 0.5433 0.6848 0.7236 0.077 Uiso 1 1 calc R . . H74C H 0.5544 0.5948 0.7014 0.077 Uiso 1 1 calc R . . C75 C 0.5396(4) 0.3162(6) 0.6539(3) 0.035(2) Uani 1 1 d . . . C76 C 0.5514(5) 0.3769(6) 0.6323(4) 0.047(3) Uani 1 1 d . . . C77 C 0.5710(7) 0.4364(9) 0.5962(5) 0.074(4) Uani 1 1 d . . . C78 C 0.5310(8) 0.5068(11) 0.5856(7) 0.114(7) Uani 1 1 d . . . H78A H 0.4947 0.4838 0.5766 0.171 Uiso 1 1 calc R . . H78B H 0.5443 0.5406 0.5594 0.171 Uiso 1 1 calc R . . H78C H 0.5281 0.5416 0.6141 0.171 Uiso 1 1 calc R . . C79 C 0.5791(9) 0.3852(11) 0.5514(5) 0.116(7) Uani 1 1 d . . . H79A H 0.6032 0.3378 0.5591 0.174 Uiso 1 1 calc R . . H79B H 0.5960 0.4200 0.5273 0.174 Uiso 1 1 calc R . . H79C H 0.5434 0.3648 0.5389 0.174 Uiso 1 1 calc R . . C80 C 0.6270(7) 0.4733(10) 0.6140(6) 0.103(6) Uani 1 1 d . . . H80A H 0.6218 0.5061 0.6429 0.154 Uiso 1 1 calc R . . H80B H 0.6416 0.5091 0.5892 0.154 Uiso 1 1 calc R . . H80C H 0.6530 0.4279 0.6211 0.154 Uiso 1 1 calc R . . C81 C 0.5071(6) 0.2335(11) 0.4258(6) 0.088(5) Uani 1 1 d . . . H81A H 0.4822 0.2358 0.3970 0.106 Uiso 1 1 calc R . . H81B H 0.4931 0.2736 0.4493 0.106 Uiso 1 1 calc R . . Cl1 Cl 0.50514(19) 0.1327(4) 0.45011(18) 0.1120(17) Uani 1 1 d . . . Cl2 Cl 0.5695(3) 0.2624(6) 0.4112(3) 0.233(5) Uani 1 1 d . . . C82 C 0.0442(9) 0.1888(9) 0.5746(9) 0.163(12) Uani 1 1 d . . . H82A H 0.0693 0.2098 0.6005 0.195 Uiso 1 1 calc R . . H82B H 0.0595 0.2077 0.5442 0.195 Uiso 1 1 calc R . . Cl3 Cl 0.0487(3) 0.0862(4) 0.5754(3) 0.181(3) Uani 1 1 d . . . Cl4 Cl -0.0124(3) 0.2346(9) 0.5795(4) 0.259(6) Uani 1 1 d . . . C83A C 0.1831(8) 0.0518(19) 0.9350(9) 0.026(5) Uani 0.25 1 d PDU A 1 H83A H 0.1691 0.1095 0.9376 0.031 Uiso 0.25 1 calc PR A 1 H83B H 0.1672 0.0212 0.9618 0.031 Uiso 0.25 1 calc PR A 1 C83B C 0.2129(8) 0.0184(18) 0.9046(9) 0.026(5) Uani 0.25 1 d PDU A 2 H83C H 0.2311 0.0433 0.8770 0.031 Uiso 0.25 1 calc PR A 2 H83D H 0.2245 -0.0407 0.9056 0.031 Uiso 0.25 1 calc PR A 2 Cl5 Cl 0.1502(5) 0.0166(6) 0.8900(4) 0.112(3) Uani 0.50 1 d PDU . . Cl6 Cl 0.2421(5) 0.0597(7) 0.9499(4) 0.119(3) Uani 0.50 1 d PDU . . C84 C 0.5935(8) 0.1250(12) 0.9916(7) 0.039(4) Uani 0.50 1 d PDU . . H84A H 0.5761 0.1676 0.9710 0.059 Uiso 0.50 1 calc PR . . H84B H 0.6020 0.1486 1.0232 0.059 Uiso 0.50 1 calc PR . . H84C H 0.5682 0.0779 0.9946 0.059 Uiso 0.50 1 calc PR . . C85 C 0.6425(8) 0.0974(14) 0.9714(8) 0.051(5) Uani 0.50 1 d PDU . . H85A H 0.6703 0.1425 0.9735 0.061 Uiso 0.50 1 calc PR . . H85B H 0.6573 0.0492 0.9898 0.061 Uiso 0.50 1 calc PR . . C86 C 0.6643(9) 0.0272(14) 0.8947(9) 0.066(7) Uani 0.50 1 d PDU . . H86A H 0.6453 0.0264 0.8628 0.079 Uiso 0.50 1 calc PR . . H86B H 0.6658 -0.0308 0.9066 0.079 Uiso 0.50 1 calc PR . . C87 C 0.7184(8) 0.0562(14) 0.8899(8) 0.048(5) Uani 0.50 1 d PDU . . H87A H 0.7176 0.1081 0.8715 0.073 Uiso 0.50 1 calc PR . . H87B H 0.7398 0.0143 0.8732 0.073 Uiso 0.50 1 calc PR . . H87C H 0.7354 0.0664 0.9215 0.073 Uiso 0.50 1 calc PR . . O1 O 0.6339(6) 0.0750(8) 0.9253(5) 0.050(4) Uani 0.50 1 d PDU . . 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 0.02146(14) 0.03099(17) 0.01982(16) -0.00842(13) 0.00379(12) -0.00008(12) Au2 0.02265(15) 0.03095(17) 0.02126(17) -0.01089(13) 0.00448(12) -0.00306(13) Au3 0.02298(15) 0.02298(15) 0.01878(16) -0.00644(12) 0.00389(12) -0.00134(12) Au4 0.02716(16) 0.02693(17) 0.02574(18) -0.00958(13) 0.00255(13) 0.00127(13) Au5 0.02804(16) 0.03214(18) 0.02488(18) -0.00576(14) 0.00062(13) 0.00114(14) Au6 0.02523(16) 0.03786(19) 0.02398(18) -0.01625(14) 0.00094(13) 0.00321(14) Au7 0.02542(15) 0.03427(18) 0.01997(17) -0.01192(13) 0.00087(13) 0.00293(13) Au8 0.02579(16) 0.0455(2) 0.02256(18) -0.01355(15) 0.00064(13) 0.00216(15) P1 0.0205(10) 0.0326(12) 0.0200(11) -0.0083(9) 0.0026(8) 0.0014(9) P2 0.0237(10) 0.0277(11) 0.0252(12) -0.0110(9) 0.0035(9) -0.0027(9) P3 0.0232(10) 0.0254(11) 0.0204(11) -0.0077(8) 0.0019(8) 0.0018(8) P4 0.0261(11) 0.0384(13) 0.0245(12) -0.0117(10) 0.0003(9) 0.0001(10) P5 0.0391(14) 0.0419(15) 0.0444(17) -0.0005(12) -0.0122(12) 0.0077(12) P6 0.0313(12) 0.0402(14) 0.0303(13) -0.0049(10) -0.0023(10) 0.0037(10) F1 0.079(5) 0.046(4) 0.101(6) -0.023(4) -0.049(5) 0.010(4) F2 0.092(6) 0.061(5) 0.085(6) -0.037(4) -0.037(5) 0.031(4) F3 0.039(3) 0.077(5) 0.058(4) 0.012(4) -0.010(3) 0.017(3) F4 0.071(5) 0.115(7) 0.076(6) 0.052(5) 0.006(4) 0.024(5) F5 0.044(3) 0.053(4) 0.078(5) -0.009(3) -0.026(3) 0.009(3) F6 0.045(4) 0.068(5) 0.082(5) 0.013(4) 0.003(3) 0.016(3) F7 0.055(4) 0.080(5) 0.037(4) 0.015(3) 0.002(3) 0.017(3) F8 0.042(3) 0.059(4) 0.049(4) 0.011(3) 0.011(3) -0.002(3) F9 0.035(3) 0.073(5) 0.061(4) -0.010(4) -0.019(3) 0.006(3) F10 0.069(4) 0.049(4) 0.073(5) -0.029(4) -0.003(4) 0.004(3) F11 0.029(3) 0.049(3) 0.036(3) -0.001(3) 0.000(2) 0.011(2) F12 0.039(3) 0.042(3) 0.056(4) -0.012(3) -0.002(3) 0.004(3) N1 0.023(3) 0.034(4) 0.028(4) -0.008(3) 0.005(3) -0.005(3) N2 0.033(4) 0.040(4) 0.024(4) -0.002(3) 0.002(3) 0.005(3) N3 0.026(4) 0.031(4) 0.029(4) -0.008(3) 0.002(3) 0.002(3) N4 0.029(4) 0.034(4) 0.032(4) -0.009(3) 0.004(3) -0.005(3) N5 0.026(4) 0.031(4) 0.028(4) -0.008(3) 0.004(3) -0.001(3) N6 0.028(4) 0.026(4) 0.026(4) -0.005(3) 0.002(3) 0.001(3) N7 0.039(4) 0.044(5) 0.026(4) -0.006(3) -0.002(3) 0.002(4) N8 0.039(4) 0.043(5) 0.037(5) -0.015(4) 0.012(4) -0.003(4) C1 0.034(5) 0.033(5) 0.021(4) -0.010(4) 0.000(4) -0.002(4) C2 0.028(4) 0.048(6) 0.022(5) -0.008(4) -0.002(4) -0.002(4) C3 0.027(5) 0.067(7) 0.035(6) -0.016(5) 0.012(4) -0.005(5) C4 0.060(7) 0.076(9) 0.059(8) -0.013(7) 0.027(6) -0.020(7) C5 0.032(5) 0.086(9) 0.050(7) -0.021(6) 0.015(5) 0.012(6) C6 0.056(7) 0.085(9) 0.039(7) -0.030(6) 0.015(5) 0.006(6) C7 0.035(5) 0.031(5) 0.045(6) -0.007(4) -0.002(4) 0.002(4) C8 0.045(6) 0.031(5) 0.057(7) 0.002(5) 0.011(5) -0.006(4) C9 0.052(6) 0.048(6) 0.037(6) -0.009(5) 0.010(5) -0.017(5) C10 0.031(5) 0.039(5) 0.029(5) -0.008(4) 0.011(4) -0.005(4) C11 0.041(5) 0.060(7) 0.033(6) -0.006(5) 0.004(5) 0.009(5) C12 0.048(6) 0.064(7) 0.034(6) 0.000(5) -0.005(5) 0.011(5) C13 0.037(5) 0.064(7) 0.038(6) 0.000(5) -0.009(5) 0.010(5) C14 0.029(5) 0.042(6) 0.040(6) -0.006(4) -0.001(4) 0.009(4) C15 0.020(4) 0.035(5) 0.016(4) -0.009(3) -0.005(3) 0.004(3) C16 0.032(4) 0.025(4) 0.027(5) -0.007(4) -0.002(4) 0.002(4) C17 0.024(4) 0.035(5) 0.014(4) -0.007(3) 0.004(3) 0.001(3) C18 0.017(3) 0.023(4) 0.025(4) -0.011(3) 0.001(3) 0.001(3) C19 0.024(4) 0.023(4) 0.031(5) -0.006(3) 0.003(4) -0.002(3) C20 0.026(4) 0.024(4) 0.025(4) -0.005(3) 0.006(3) 0.005(3) C21 0.055(6) 0.035(5) 0.032(5) -0.004(4) 0.006(5) -0.006(5) C22 0.082(9) 0.052(7) 0.034(6) -0.003(5) 0.025(6) -0.019(6) C23 0.041(6) 0.056(7) 0.048(7) -0.016(5) 0.009(5) -0.020(5) C24 0.043(5) 0.036(5) 0.032(5) -0.018(4) 0.003(4) -0.008(4) C25 0.032(4) 0.023(4) 0.028(5) 0.000(3) 0.003(4) -0.006(4) C26 0.050(6) 0.030(5) 0.033(5) -0.003(4) 0.004(4) -0.001(4) C27 0.052(6) 0.038(5) 0.030(5) 0.000(4) -0.003(5) 0.015(5) C28 0.036(5) 0.038(5) 0.023(5) -0.006(4) -0.006(4) 0.010(4) C29 0.031(5) 0.063(7) 0.023(5) -0.019(5) 0.002(4) 0.005(5) C30 0.033(5) 0.045(5) 0.019(4) -0.014(4) -0.005(4) 0.001(4) C31 0.035(5) 0.049(6) 0.017(4) -0.014(4) 0.003(4) 0.007(4) C32 0.045(6) 0.052(6) 0.036(6) -0.004(5) 0.007(5) 0.018(5) C33 0.048(6) 0.078(8) 0.036(6) 0.007(6) 0.013(5) 0.020(6) C34 0.065(8) 0.078(9) 0.055(8) -0.045(7) 0.016(6) -0.007(7) C35 0.042(6) 0.073(8) 0.053(7) -0.032(6) 0.014(5) -0.025(6) C36 0.069(8) 0.071(9) 0.053(8) -0.015(6) 0.025(6) -0.022(7) C37 0.109(11) 0.052(7) 0.037(7) 0.004(5) 0.002(7) -0.020(8) C38 0.052(6) 0.049(6) 0.034(6) -0.002(5) 0.004(5) -0.006(5) C39 0.046(6) 0.057(7) 0.032(6) -0.006(5) -0.004(5) 0.012(5) C40 0.064(7) 0.050(7) 0.049(7) -0.001(5) -0.016(6) 0.008(6) C41 0.074(8) 0.051(7) 0.047(7) 0.000(6) -0.010(6) -0.006(6) C42 0.046(6) 0.054(7) 0.032(6) 0.009(5) 0.003(5) -0.005(5) C43 0.026(4) 0.034(5) 0.030(5) -0.013(4) -0.006(4) 0.000(4) C44 0.037(5) 0.030(5) 0.029(5) -0.009(4) -0.003(4) 0.004(4) C45 0.041(5) 0.023(4) 0.020(4) -0.006(3) -0.001(4) -0.001(4) C46 0.020(4) 0.025(4) 0.028(5) -0.010(3) 0.000(3) 0.000(3) C47 0.026(4) 0.028(4) 0.034(5) -0.002(4) 0.001(4) -0.004(3) C48 0.024(4) 0.042(5) 0.023(5) -0.003(4) 0.003(3) -0.005(4) C49 0.039(5) 0.038(6) 0.050(7) -0.002(5) 0.010(5) -0.004(4) C50 0.044(6) 0.033(5) 0.067(8) -0.005(5) 0.010(6) -0.013(5) C51 0.026(5) 0.039(6) 0.071(8) -0.020(5) 0.007(5) -0.007(4) C52 0.028(5) 0.050(6) 0.045(6) -0.013(5) -0.008(4) -0.010(4) C53 0.041(5) 0.031(5) 0.057(7) -0.009(5) -0.007(5) 0.001(4) C54 0.049(6) 0.033(5) 0.054(7) 0.002(5) 0.004(5) 0.014(5) C55 0.060(7) 0.022(5) 0.061(7) -0.005(5) 0.016(6) -0.006(5) C56 0.042(5) 0.023(5) 0.042(6) -0.009(4) 0.005(4) -0.011(4) C57 0.034(4) 0.023(4) 0.026(5) -0.008(3) 0.005(4) -0.004(4) C58 0.040(5) 0.037(5) 0.031(5) -0.012(4) 0.010(4) 0.001(4) C59 0.076(8) 0.024(5) 0.050(7) -0.001(4) 0.028(6) -0.004(5) C60 0.078(9) 0.042(7) 0.107(12) 0.006(7) 0.036(8) -0.020(6) C61 0.138(13) 0.038(6) 0.046(7) 0.005(5) 0.041(8) -0.001(7) C62 0.097(10) 0.042(7) 0.056(8) 0.011(6) 0.030(7) 0.017(7) C63 0.029(4) 0.040(5) 0.028(5) -0.016(4) -0.005(4) 0.007(4) C64 0.042(5) 0.050(6) 0.024(5) -0.012(4) 0.000(4) 0.014(5) C65 0.075(8) 0.031(5) 0.042(6) 0.004(5) -0.007(6) 0.023(5) C66 0.077(9) 0.036(6) 0.086(10) -0.002(6) 0.006(8) 0.001(6) C67 0.084(9) 0.064(8) 0.049(8) -0.005(6) -0.015(7) 0.030(7) C68 0.105(11) 0.049(7) 0.047(7) -0.015(6) -0.012(7) 0.032(7) C69 0.027(4) 0.026(4) 0.028(5) -0.007(4) 0.005(4) 0.003(3) C70 0.023(4) 0.038(5) 0.032(5) -0.005(4) 0.004(4) -0.002(4) C71 0.034(5) 0.032(5) 0.055(7) 0.010(5) 0.008(5) 0.002(4) C72 0.046(6) 0.026(5) 0.064(7) -0.003(5) 0.015(5) 0.005(4) C73 0.055(7) 0.059(8) 0.072(9) 0.028(7) 0.008(6) 0.011(6) C74 0.054(6) 0.029(5) 0.073(8) 0.015(5) 0.031(6) 0.000(5) C75 0.038(5) 0.036(5) 0.031(5) -0.017(4) 0.001(4) 0.009(4) C76 0.063(7) 0.031(6) 0.046(7) -0.015(5) 0.000(5) 0.006(5) C77 0.112(12) 0.061(8) 0.051(8) 0.001(6) 0.024(8) 0.005(8) C78 0.142(17) 0.101(14) 0.100(14) 0.046(11) 0.008(12) 0.034(13) C79 0.21(2) 0.098(13) 0.042(9) -0.002(8) 0.034(11) -0.012(14) C80 0.136(15) 0.069(10) 0.108(14) 0.008(9) 0.061(12) -0.033(10) C81 0.074(10) 0.113(14) 0.078(11) -0.001(10) -0.004(8) 0.033(9) Cl1 0.083(3) 0.154(5) 0.101(3) 0.035(3) 0.030(3) 0.034(3) Cl2 0.101(4) 0.326(11) 0.270(10) 0.219(9) 0.008(5) -0.005(6) C82 0.162(19) 0.049(9) 0.29(3) 0.051(13) 0.17(2) 0.022(11) Cl3 0.218(8) 0.133(5) 0.197(7) -0.039(5) 0.084(6) -0.054(5) Cl4 0.127(6) 0.440(18) 0.210(9) -0.028(11) 0.006(6) -0.045(9) C83A 0.033(7) 0.022(7) 0.024(7) 0.011(6) 0.006(6) 0.009(6) C83B 0.033(7) 0.022(7) 0.024(7) 0.011(6) 0.006(6) 0.009(6) Cl5 0.142(7) 0.074(5) 0.120(6) 0.001(5) 0.000(6) 0.000(5) Cl6 0.146(7) 0.110(6) 0.102(6) 0.026(5) 0.008(5) 0.012(6) C84 0.052(8) 0.034(8) 0.032(8) -0.010(6) 0.009(7) -0.006(7) C85 0.047(8) 0.039(8) 0.065(10) 0.004(7) -0.012(8) -0.007(7) C86 0.064(10) 0.055(10) 0.079(11) 0.012(8) 0.007(8) 0.004(8) C87 0.043(8) 0.049(9) 0.053(9) 0.011(7) 0.003(7) 0.008(7) O1 0.072(7) 0.037(6) 0.045(7) 0.009(5) 0.041(6) 0.001(6) _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 C1 1.990(9) . ? Au1 P1 2.245(2) . yes Au1 Au3 2.9633(4) . yes Au1 Au2 3.3421(4) . yes Au2 C1 2.194(9) . ? Au2 P2 2.255(2) . yes Au2 C2 2.284(9) . ? Au2 Au3 2.9242(4) . yes Au3 C69 1.983(9) . ? Au3 C57 2.008(9) . ? Au3 Au5 3.2198(5) . yes Au3 Au4 3.2542(4) . yes Au4 C57 2.111(8) . ? Au4 C63 2.126(9) . ? Au4 C58 2.287(9) . ? Au4 C64 2.323(9) . ? Au4 Au6 3.1939(5) . yes Au5 C75 2.131(8) . ? Au5 C69 2.158(8) . ? Au5 C70 2.286(9) . ? Au5 C76 2.328(11) . ? Au5 Au6 3.2116(5) . yes Au6 C63 1.989(10) . ? Au6 C75 2.009(11) . ? Au6 Au7 2.8798(4) . yes Au6 Au8 2.9270(5) . yes Au7 C29 2.190(9) . ? Au7 P3 2.249(2) . yes Au7 C30 2.291(8) . ? Au7 Au8 3.3107(5) . yes Au8 C29 2.008(9) . ? Au8 P4 2.251(2) . yes P1 N2 1.657(8) . ? P1 N1 1.706(8) . ? P1 C15 1.798(8) . ? P2 N3 1.677(8) . ? P2 N4 1.685(7) . ? P2 C46 1.812(8) . ? P3 N6 1.678(7) . ? P3 N5 1.693(7) . ? P3 C18 1.804(8) . ? P4 N8 1.672(8) . ? P4 N7 1.684(8) . ? P4 C43 1.816(9) . ? P5 F6 1.581(8) . ? P5 F4 1.582(8) . ? P5 F2 1.587(7) . ? P5 F1 1.590(7) . ? P5 F5 1.592(6) . ? P5 F3 1.608(6) . ? P6 F10 1.589(7) . ? P6 F7 1.590(7) . ? P6 F9 1.591(6) . ? P6 F12 1.592(6) . ? P6 F8 1.593(6) . ? P6 F11 1.621(5) . ? N1 C7 1.373(12) . ? N1 C10 1.394(11) . ? N2 C11 1.399(12) . ? N2 C14 1.404(11) . ? N3 C53 1.381(13) . ? N3 C56 1.406(11) . ? N4 C52 1.392(11) . ? N4 C49 1.392(13) . ? N5 C21 1.389(12) . ? N5 C24 1.403(11) . ? N6 C25 1.383(11) . ? N6 C28 1.391(11) . ? N7 C39 1.399(12) . ? N7 C42 1.431(12) . ? N8 C35 1.387(13) . ? N8 C38 1.394(13) . ? C1 C2 1.236(12) . ? C2 C3 1.488(12) . ? C3 C4 1.515(16) . ? C3 C5 1.532(16) . ? C3 C6 1.533(14) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.346(13) . ? C7 H7 0.9500 . ? C8 C9 1.406(15) . ? C8 H8 0.9500 . ? C9 C10 1.336(14) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.361(14) . ? C11 H11 0.9500 . ? C12 C13 1.424(15) . ? C12 H12 0.9500 . ? C13 C14 1.343(14) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.400(12) . ? C15 C20 1.401(12) . ? C16 C17 1.389(11) . ? C16 H16 0.9500 . ? C17 C18 1.377(11) . ? C17 H17 0.9500 . ? C18 C19 1.400(12) . ? C19 C20 1.376(11) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.337(15) . ? C21 H21 0.9500 . ? C22 C23 1.426(16) . ? C22 H22 0.9500 . ? C23 C24 1.343(14) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.348(13) . ? C25 H25 0.9500 . ? C26 C27 1.400(14) . ? C26 H26 0.9500 . ? C27 C28 1.356(13) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.229(12) . ? C30 C31 1.483(12) . ? C31 C33 1.519(15) . ? C31 C32 1.527(13) . ? C31 C34 1.531(14) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.364(17) . ? C35 H35 0.9500 . ? C36 C37 1.404(19) . ? C36 H36 0.9500 . ? C37 C38 1.341(16) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.337(15) . ? C39 H39 0.9500 . ? C40 C41 1.441(17) . ? C40 H40 0.9500 . ? C41 C42 1.340(15) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C48 1.378(12) . ? C43 C44 1.387(13) . ? C44 C45 1.394(12) . ? C44 H44 0.9500 . ? C45 C46 1.383(11) . ? C45 H45 0.9500 . ? C46 C47 1.381(12) . ? C47 C48 1.370(12) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C50 1.345(13) . ? C49 H49 0.9500 . ? C50 C51 1.412(16) . ? C50 H50 0.9500 . ? C51 C52 1.337(14) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C54 1.351(14) . ? C53 H53 0.9500 . ? C54 C55 1.428(15) . ? C54 H54 0.9500 . ? C55 C56 1.331(14) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 C58 1.212(13) . ? C58 C59 1.493(14) . ? C59 C62 1.513(15) . ? C59 C61 1.519(15) . ? C59 C60 1.558(18) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C64 1.238(14) . ? C64 C65 1.494(14) . ? C65 C66 1.502(17) . ? C65 C67 1.531(15) . ? C65 C68 1.558(15) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 C70 1.222(12) . ? C70 C71 1.495(13) . ? C71 C73 1.526(16) . ? C71 C74 1.527(13) . ? C71 C72 1.532(14) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 C76 1.188(14) . ? C76 C77 1.485(17) . ? C77 C78 1.51(2) . ? C77 C79 1.521(19) . ? C77 C80 1.55(2) . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 Cl2 1.652(17) . ? C81 Cl1 1.759(18) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 Cl4 1.572(19) . ? C82 Cl3 1.652(16) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83A Cl6 1.483(16) . ? C83A Cl5 1.575(16) . ? C83A H83A 0.9900 . ? C83A H83B 0.9900 . ? C83B Cl5 1.564(16) . ? C83B Cl6 1.578(16) . ? C83B H83C 0.9900 . ? C83B H83D 0.9900 . ? C84 C85 1.41(2) . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C85 O1 1.35(3) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 O1 1.388(10) . ? C86 C87 1.41(2) . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? 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 C1 Au1 P1 174.9(2) . . ? C1 Au1 Au3 93.8(2) . . ? P1 Au1 Au3 90.39(6) . . ? C1 Au1 Au2 39.1(2) . . ? P1 Au1 Au2 144.67(6) . . ? Au3 Au1 Au2 54.863(9) . . ? C1 Au2 P2 177.7(2) . . ? C1 Au2 C2 32.0(3) . . ? P2 Au2 C2 148.3(2) . . ? C1 Au2 Au3 90.7(2) . . ? P2 Au2 Au3 88.96(5) . . ? C2 Au2 Au3 122.7(2) . . ? C1 Au2 Au1 34.9(2) . . ? P2 Au2 Au1 144.51(5) . . ? C2 Au2 Au1 66.8(2) . . ? Au3 Au2 Au1 55.965(10) . . ? C69 Au3 C57 176.8(3) . . ? C69 Au3 Au2 102.2(2) . . ? C57 Au3 Au2 75.7(2) . . ? C69 Au3 Au1 101.1(2) . . ? C57 Au3 Au1 80.4(2) . . ? Au2 Au3 Au1 69.172(11) . . ? C69 Au3 Au5 41.0(2) . . ? C57 Au3 Au5 139.6(2) . . ? Au2 Au3 Au5 135.272(14) . . ? Au1 Au3 Au5 129.613(13) . . ? C69 Au3 Au4 141.5(2) . . ? C57 Au3 Au4 38.9(2) . . ? Au2 Au3 Au4 108.594(13) . . ? Au1 Au3 Au4 111.041(13) . . ? Au5 Au3 Au4 100.650(12) . . ? C57 Au4 C63 152.7(4) . . ? C57 Au4 C58 31.7(3) . . ? C63 Au4 C58 175.4(4) . . ? C57 Au4 C64 175.2(4) . . ? C63 Au4 C64 31.9(4) . . ? C58 Au4 C64 143.7(4) . . ? C57 Au4 Au6 115.2(2) . . ? C63 Au4 Au6 37.6(3) . . ? C58 Au4 Au6 146.8(3) . . ? C64 Au4 Au6 69.5(3) . . ? C57 Au4 Au3 36.7(2) . . ? C63 Au4 Au3 116.0(3) . . ? C58 Au4 Au3 68.3(2) . . ? C64 Au4 Au3 147.9(3) . . ? Au6 Au4 Au3 78.474(11) . . ? C75 Au5 C69 153.5(4) . . ? C75 Au5 C70 173.8(4) . . ? C69 Au5 C70 31.8(3) . . ? C75 Au5 C76 30.5(4) . . ? C69 Au5 C76 175.9(4) . . ? C70 Au5 C76 144.4(4) . . ? C75 Au5 Au6 37.8(3) . . ? C69 Au5 Au6 115.7(2) . . ? C70 Au5 Au6 147.2(2) . . ? C76 Au5 Au6 68.3(3) . . ? C75 Au5 Au3 116.5(3) . . ? C69 Au5 Au3 37.1(2) . . ? C70 Au5 Au3 68.8(2) . . ? C76 Au5 Au3 146.8(3) . . ? Au6 Au5 Au3 78.722(12) . . ? C63 Au6 C75 176.6(3) . . ? C63 Au6 Au7 86.0(2) . . ? C75 Au6 Au7 91.0(2) . . ? C63 Au6 Au8 84.8(2) . . ? C75 Au6 Au8 92.8(3) . . ? Au7 Au6 Au8 69.515(11) . . ? C63 Au6 Au4 40.7(2) . . ? C75 Au6 Au4 142.7(2) . . ? Au7 Au6 Au4 119.561(15) . . ? Au8 Au6 Au4 116.721(15) . . ? C63 Au6 Au5 142.8(2) . . ? C75 Au6 Au5 40.5(2) . . ? Au7 Au6 Au5 124.294(15) . . ? Au8 Au6 Au5 123.532(16) . . ? Au4 Au6 Au5 102.142(12) . . ? C29 Au7 P3 177.2(2) . . ? C29 Au7 C30 31.7(3) . . ? P3 Au7 C30 145.5(2) . . ? C29 Au7 Au6 91.9(2) . . ? P3 Au7 Au6 90.91(5) . . ? C30 Au7 Au6 123.5(2) . . ? C29 Au7 Au8 36.1(2) . . ? P3 Au7 Au8 146.68(5) . . ? C30 Au7 Au8 67.8(2) . . ? Au6 Au7 Au8 55.913(10) . . ? C29 Au8 P4 174.0(3) . . ? C29 Au8 Au6 94.4(3) . . ? P4 Au8 Au6 91.59(6) . . ? C29 Au8 Au7 39.9(3) . . ? P4 Au8 Au7 146.09(6) . . ? Au6 Au8 Au7 54.572(10) . . ? N2 P1 N1 106.7(4) . . ? N2 P1 C15 103.6(4) . . ? N1 P1 C15 104.4(4) . . ? N2 P1 Au1 112.4(3) . . ? N1 P1 Au1 109.6(2) . . ? C15 P1 Au1 119.2(3) . . ? N3 P2 N4 107.9(4) . . ? N3 P2 C46 103.2(4) . . ? N4 P2 C46 103.1(4) . . ? N3 P2 Au2 110.9(3) . . ? N4 P2 Au2 110.3(3) . . ? C46 P2 Au2 120.6(3) . . ? N6 P3 N5 109.1(4) . . ? N6 P3 C18 102.9(4) . . ? N5 P3 C18 102.5(4) . . ? N6 P3 Au7 110.1(3) . . ? N5 P3 Au7 109.4(3) . . ? C18 P3 Au7 122.1(3) . . ? N8 P4 N7 110.0(4) . . ? N8 P4 C43 102.6(4) . . ? N7 P4 C43 102.4(4) . . ? N8 P4 Au8 109.5(3) . . ? N7 P4 Au8 110.3(3) . . ? C43 P4 Au8 121.3(3) . . ? F6 P5 F4 179.5(4) . . ? F6 P5 F2 89.4(5) . . ? F4 P5 F2 90.6(5) . . ? F6 P5 F1 88.7(5) . . ? F4 P5 F1 91.3(5) . . ? F2 P5 F1 177.8(5) . . ? F6 P5 F5 90.1(4) . . ? F4 P5 F5 90.4(4) . . ? F2 P5 F5 91.7(4) . . ? F1 P5 F5 89.4(4) . . ? F6 P5 F3 88.6(4) . . ? F4 P5 F3 90.9(4) . . ? F2 P5 F3 89.3(4) . . ? F1 P5 F3 89.6(4) . . ? F5 P5 F3 178.3(4) . . ? F10 P6 F7 89.6(4) . . ? F10 P6 F9 90.6(4) . . ? F7 P6 F9 90.6(4) . . ? F10 P6 F12 178.4(4) . . ? F7 P6 F12 89.8(4) . . ? F9 P6 F12 91.0(3) . . ? F10 P6 F8 90.8(4) . . ? F7 P6 F8 178.8(4) . . ? F9 P6 F8 90.6(4) . . ? F12 P6 F8 89.7(4) . . ? F10 P6 F11 89.5(3) . . ? F7 P6 F11 89.2(3) . . ? F9 P6 F11 179.8(4) . . ? F12 P6 F11 88.9(3) . . ? F8 P6 F11 89.6(3) . . ? C7 N1 C10 109.5(8) . . ? C7 N1 P1 124.6(6) . . ? C10 N1 P1 125.9(6) . . ? C11 N2 C14 106.6(8) . . ? C11 N2 P1 124.2(7) . . ? C14 N2 P1 127.1(7) . . ? C53 N3 C56 107.5(8) . . ? C53 N3 P2 127.4(6) . . ? C56 N3 P2 125.1(7) . . ? C52 N4 C49 106.7(8) . . ? C52 N4 P2 127.8(7) . . ? C49 N4 P2 125.4(7) . . ? C21 N5 C24 107.7(8) . . ? C21 N5 P3 125.6(7) . . ? C24 N5 P3 126.7(7) . . ? C25 N6 C28 107.8(7) . . ? C25 N6 P3 125.3(6) . . ? C28 N6 P3 126.9(6) . . ? C39 N7 C42 107.7(8) . . ? C39 N7 P4 128.7(7) . . ? C42 N7 P4 123.6(7) . . ? C35 N8 C38 109.5(9) . . ? C35 N8 P4 126.5(8) . . ? C38 N8 P4 122.4(7) . . ? C2 C1 Au1 173.9(8) . . ? C2 C1 Au2 78.0(6) . . ? Au1 C1 Au2 105.9(4) . . ? C1 C2 C3 163.8(9) . . ? C1 C2 Au2 70.0(6) . . ? C3 C2 Au2 125.9(6) . . ? C2 C3 C4 110.2(9) . . ? C2 C3 C5 109.7(9) . . ? C4 C3 C5 111.6(9) . . ? C2 C3 C6 105.4(8) . . ? C4 C3 C6 108.8(10) . . ? C5 C3 C6 110.9(10) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 N1 107.0(9) . . ? C8 C7 H7 126.5 . . ? N1 C7 H7 126.5 . . ? C7 C8 C9 108.2(9) . . ? C7 C8 H8 125.9 . . ? C9 C8 H8 125.9 . . ? C10 C9 C8 108.8(9) . . ? C10 C9 H9 125.6 . . ? C8 C9 H9 125.6 . . ? C9 C10 N1 106.5(9) . . ? C9 C10 H10 126.8 . . ? N1 C10 H10 126.8 . . ? C12 C11 N2 108.6(9) . . ? C12 C11 H11 125.7 . . ? N2 C11 H11 125.7 . . ? C11 C12 C13 107.7(9) . . ? C11 C12 H12 126.2 . . ? C13 C12 H12 126.2 . . ? C14 C13 C12 107.8(9) . . ? C14 C13 H13 126.1 . . ? C12 C13 H13 126.1 . . ? C13 C14 N2 109.3(9) . . ? C13 C14 H14 125.4 . . ? N2 C14 H14 125.4 . . ? C16 C15 C20 119.7(7) . . ? C16 C15 P1 120.6(6) . . ? C20 C15 P1 119.7(6) . . ? C17 C16 C15 119.4(8) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C18 C17 C16 120.7(8) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C19 119.8(7) . . ? C17 C18 P3 119.3(6) . . ? C19 C18 P3 120.8(6) . . ? C20 C19 C18 120.2(8) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C15 120.0(8) . . ? C19 C20 H20 120.0 . . ? C15 C20 H20 120.0 . . ? C22 C21 N5 108.1(9) . . ? C22 C21 H21 125.9 . . ? N5 C21 H21 125.9 . . ? C21 C22 C23 108.6(9) . . ? C21 C22 H22 125.7 . . ? C23 C22 H22 125.7 . . ? C24 C23 C22 107.4(9) . . ? C24 C23 H23 126.3 . . ? C22 C23 H23 126.3 . . ? C23 C24 N5 108.1(9) . . ? C23 C24 H24 125.9 . . ? N5 C24 H24 125.9 . . ? C26 C25 N6 108.3(8) . . ? C26 C25 H25 125.9 . . ? N6 C25 H25 125.9 . . ? C25 C26 C27 108.2(9) . . ? C25 C26 H26 125.9 . . ? C27 C26 H26 125.9 . . ? C28 C27 C26 108.0(9) . . ? C28 C27 H27 126.0 . . ? C26 C27 H27 126.0 . . ? C27 C28 N6 107.7(8) . . ? C27 C28 H28 126.1 . . ? N6 C28 H28 126.1 . . ? C30 C29 Au8 177.1(8) . . ? C30 C29 Au7 78.7(6) . . ? Au8 C29 Au7 104.0(4) . . ? C29 C30 C31 165.8(9) . . ? C29 C30 Au7 69.6(6) . . ? C31 C30 Au7 124.0(6) . . ? C30 C31 C33 108.3(8) . . ? C30 C31 C32 111.6(7) . . ? C33 C31 C32 112.2(9) . . ? C30 C31 C34 105.9(8) . . ? C33 C31 C34 111.9(9) . . ? C32 C31 C34 106.8(9) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 N8 105.6(12) . . ? C36 C35 H35 127.2 . . ? N8 C35 H35 127.2 . . ? C35 C36 C37 109.5(11) . . ? C35 C36 H36 125.2 . . ? C37 C36 H36 125.2 . . ? C38 C37 C36 107.8(12) . . ? C38 C37 H37 126.1 . . ? C36 C37 H37 126.1 . . ? C37 C38 N8 107.6(11) . . ? C37 C38 H38 126.2 . . ? N8 C38 H38 126.2 . . ? C40 C39 N7 108.3(10) . . ? C40 C39 H39 125.9 . . ? N7 C39 H39 125.9 . . ? C39 C40 C41 108.4(11) . . ? C39 C40 H40 125.8 . . ? C41 C40 H40 125.8 . . ? C42 C41 C40 108.3(11) . . ? C42 C41 H41 125.8 . . ? C40 C41 H41 125.8 . . ? C41 C42 N7 107.2(10) . . ? C41 C42 H42 126.4 . . ? N7 C42 H42 126.4 . . ? C48 C43 C44 120.0(8) . . ? C48 C43 P4 120.0(7) . . ? C44 C43 P4 120.0(7) . . ? C43 C44 C45 119.9(8) . . ? C43 C44 H44 120.1 . . ? C45 C44 H44 120.1 . . ? C46 C45 C44 119.5(8) . . ? C46 C45 H45 120.3 . . ? C44 C45 H45 120.3 . . ? C47 C46 C45 119.8(8) . . ? C47 C46 P2 121.2(6) . . ? C45 C46 P2 119.0(7) . . ? C48 C47 C46 120.8(8) . . ? C48 C47 H47 119.6 . . ? C46 C47 H47 119.6 . . ? C47 C48 C43 119.9(8) . . ? C47 C48 H48 120.0 . . ? C43 C48 H48 120.0 . . ? C50 C49 N4 109.1(10) . . ? C50 C49 H49 125.4 . . ? N4 C49 H49 125.4 . . ? C49 C50 C51 107.0(10) . . ? C49 C50 H50 126.5 . . ? C51 C50 H50 126.5 . . ? C52 C51 C50 108.8(9) . . ? C52 C51 H51 125.6 . . ? C50 C51 H51 125.6 . . ? C51 C52 N4 108.4(10) . . ? C51 C52 H52 125.8 . . ? N4 C52 H52 125.8 . . ? C54 C53 N3 108.6(9) . . ? C54 C53 H53 125.7 . . ? N3 C53 H53 125.7 . . ? C53 C54 C55 107.4(10) . . ? C53 C54 H54 126.3 . . ? C55 C54 H54 126.3 . . ? C56 C55 C54 108.2(9) . . ? C56 C55 H55 125.9 . . ? C54 C55 H55 125.9 . . ? C55 C56 N3 108.3(9) . . ? C55 C56 H56 125.8 . . ? N3 C56 H56 125.8 . . ? C58 C57 Au3 172.4(8) . . ? C58 C57 Au4 82.2(6) . . ? Au3 C57 Au4 104.4(4) . . ? C57 C58 C59 167.8(9) . . ? C57 C58 Au4 66.1(6) . . ? C59 C58 Au4 126.0(7) . . ? C58 C59 C62 111.7(9) . . ? C58 C59 C61 107.4(8) . . ? C62 C59 C61 112.0(11) . . ? C58 C59 C60 106.7(10) . . ? C62 C59 C60 110.4(10) . . ? C61 C59 C60 108.4(11) . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C59 C61 H61A 109.5 . . ? C59 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C59 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C59 C62 H62A 109.5 . . ? C59 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C59 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C64 C63 Au6 175.3(8) . . ? C64 C63 Au4 82.8(6) . . ? Au6 C63 Au4 101.8(4) . . ? C63 C64 C65 167.1(10) . . ? C63 C64 Au4 65.2(6) . . ? C65 C64 Au4 127.6(7) . . ? C64 C65 C66 110.4(9) . . ? C64 C65 C67 108.3(10) . . ? C66 C65 C67 112.0(11) . . ? C64 C65 C68 105.2(9) . . ? C66 C65 C68 112.2(11) . . ? C67 C65 C68 108.4(9) . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C65 C67 H67A 109.5 . . ? C65 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C65 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C65 C68 H68A 109.5 . . ? C65 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C65 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C70 C69 Au3 177.1(7) . . ? C70 C69 Au5 79.9(6) . . ? Au3 C69 Au5 102.0(3) . . ? C69 C70 C71 167.4(9) . . ? C69 C70 Au5 68.4(6) . . ? C71 C70 Au5 124.2(7) . . ? C70 C71 C73 110.3(9) . . ? C70 C71 C74 109.7(8) . . ? C73 C71 C74 110.0(9) . . ? C70 C71 C72 107.8(8) . . ? C73 C71 C72 109.2(9) . . ? C74 C71 C72 109.8(9) . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C71 C73 H73A 109.5 . . ? C71 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C71 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C71 C74 H74A 109.5 . . ? C71 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C71 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C76 C75 Au6 173.7(9) . . ? C76 C75 Au5 83.9(7) . . ? Au6 C75 Au5 101.7(4) . . ? C75 C76 C77 164.9(11) . . ? C75 C76 Au5 65.6(7) . . ? C77 C76 Au5 129.5(8) . . ? C76 C77 C78 113.2(13) . . ? C76 C77 C79 105.8(12) . . ? C78 C77 C79 110.3(15) . . ? C76 C77 C80 109.0(12) . . ? C78 C77 C80 109.1(14) . . ? C79 C77 C80 109.4(14) . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C77 C79 H79A 109.5 . . ? C77 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C77 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C77 C80 H80A 109.5 . . ? C77 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C77 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? Cl2 C81 Cl1 113.1(9) . . ? Cl2 C81 H81A 109.0 . . ? Cl1 C81 H81A 109.0 . . ? Cl2 C81 H81B 109.0 . . ? Cl1 C81 H81B 109.0 . . ? H81A C81 H81B 107.8 . . ? Cl4 C82 Cl3 121.6(13) . . ? Cl4 C82 H82A 106.9 . . ? Cl3 C82 H82A 106.9 . . ? Cl4 C82 H82B 106.9 . . ? Cl3 C82 H82B 106.9 . . ? H82A C82 H82B 106.7 . . ? Cl6 C83A Cl5 135.4(19) . . ? Cl6 C83A H83A 103.3 . . ? Cl5 C83A H83A 103.3 . . ? Cl6 C83A H83B 103.3 . . ? Cl5 C83A H83B 103.3 . . ? H83A C83A H83B 105.2 . . ? Cl5 C83B Cl6 128.5(17) . . ? Cl5 C83B H83C 105.2 . . ? Cl6 C83B H83C 105.2 . . ? Cl5 C83B H83D 105.2 . . ? Cl6 C83B H83D 105.2 . . ? H83C C83B H83D 105.9 . . ? C83B Cl5 C83A 47.4(15) . . ? C83A Cl6 C83B 48.5(16) . . ? C85 C84 H84A 109.5 . . ? C85 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C85 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? O1 C85 C84 111.5(18) . . ? O1 C85 H85A 109.3 . . ? C84 C85 H85A 109.3 . . ? O1 C85 H85B 109.3 . . ? C84 C85 H85B 109.3 . . ? H85A C85 H85B 108.0 . . ? O1 C86 C87 113.4(19) . . ? O1 C86 H86A 108.9 . . ? C87 C86 H86A 108.9 . . ? O1 C86 H86B 108.9 . . ? C87 C86 H86B 108.9 . . ? H86A C86 H86B 107.7 . . ? C86 C87 H87A 109.5 . . ? C86 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C86 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C85 O1 C86 132.4(19) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 5.177 _refine_diff_density_min -2.286 _refine_diff_density_rms 0.216 # start Validation Reply Form _vrf_PUBL366_GLOBAL ; PROBLEM: Short? C(sp?)-C(sp?) Bond C75 - C76 ... 1.19 Ang. RESPONSE: The apparently short distance is due to the triple bond. ; _vrf_PUBL973_GLOBAL ; PROBLEM: Large Calcd. Positive Residual Density on Au6 2.07 eA-3 RESPONSE: Some of the Au atoms were accompanied by relatively large residual electron densities due to the absorption despite the analytical absorption correction. ; # end Validation Reply Form #===END======================================================================== data_3 _database_code_depnum_ccdc_archive 'CCDC 809018' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C88 H94 Au8 P4, 2(Cl O4)' _chemical_formula_sum 'C88 H94 Au8 Cl2 O8 P4' _chemical_formula_weight 3050.14 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' 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' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.0014(7) _cell_length_b 17.4798(10) _cell_length_c 23.2057(19) _cell_angle_alpha 106.781(3) _cell_angle_beta 95.591(3) _cell_angle_gamma 111.261(2) _cell_volume 4583.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9229 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 27.53 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.210 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2824 _exptl_absorpt_coefficient_mu 12.931 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.1666 _exptl_absorpt_correction_T_max 0.4097 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _publ_section_exptl_refinement ; One of the ClO~4~^-^ anions was disordered over two sites with equal occupancies. Another ClO~4~^-^ anion was refined with occupancy of 0.5. The carbon atoms C55, C56, C57, C58, C67, C68, C69, and C70 were restrained with effective standard deviation 0.01 so that its U~ij~ components approximate to isotropic behavior. The hydrogen atoms were positioned geometrically and constrained to ride on their parent atoms, with C---H = 0.95-0.98 \%A, and U~iso~ = 1.2-1.5 U~eq~(parent atom). The highest peak is located 0.81 \%A from atom Au3 and the deepest hole is located 0.63 \%A from atom Au1. ; _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 'curved graphite crystal' _diffrn_measurement_device_type 'Bruker KAPPA APEX II DUO CCD' _diffrn_measurement_device '62mm x 62mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 16 # 8 for binned mode _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62956 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 26.75 _reflns_number_total 19414 _reflns_number_gt 15587 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT (Bruker AXS, 2009)' _computing_data_reduction 'SAINT (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond v.3.2e (Brandenburg, 2010)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0369P)^2^+45.0860P] 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 19414 _refine_ls_number_parameters 1054 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0517 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0871 _refine_ls_wR_factor_gt 0.0778 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.030 _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 Au1 Au 0.05459(3) 0.93264(2) 0.331882(15) 0.02799(7) Uani 1 1 d . . . Au2 Au 0.22255(3) 0.808702(19) 0.117291(14) 0.02356(7) Uani 1 1 d . . . Au3 Au 0.15465(2) 0.914124(18) 0.216645(14) 0.02131(7) Uani 1 1 d . . . Au4 Au 0.18449(3) 1.096163(18) 0.276843(14) 0.02322(7) Uani 1 1 d . . . Au5 Au 0.37310(3) 1.266118(19) 0.348579(15) 0.02585(7) Uani 1 1 d . . . Au6 Au 0.41078(3) 1.073084(19) 0.313123(15) 0.02601(7) Uani 1 1 d . . . Au7 Au 0.28940(3) 1.031643(19) 0.147460(15) 0.02512(7) Uani 1 1 d . . . Au8 Au -0.02777(3) 0.998850(19) 0.177969(14) 0.02445(7) Uani 1 1 d . . . P1 P 0.03060(18) 0.79531(14) 0.32558(10) 0.0268(4) Uani 1 1 d . . . P2 P 0.14149(18) 0.68831(13) 0.14389(10) 0.0255(4) Uani 1 1 d . . . P3 P -0.04275(17) 1.12526(13) 0.18222(10) 0.0245(4) Uani 1 1 d . . . P4 P 0.24854(17) 1.33033(13) 0.35159(10) 0.0254(4) Uani 1 1 d . . . C1 C -0.1153(7) 0.7208(6) 0.3149(4) 0.0300(18) Uani 1 1 d . . . C2 C -0.1911(9) 0.7527(7) 0.3400(5) 0.049(3) Uani 1 1 d . . . H2 H -0.1647 0.8129 0.3645 0.059 Uiso 1 1 calc R . . C3 C -0.3041(9) 0.6979(7) 0.3297(6) 0.059(3) Uani 1 1 d . . . H3 H -0.3547 0.7206 0.3471 0.070 Uiso 1 1 calc R . . C4 C -0.3430(9) 0.6117(7) 0.2950(5) 0.052(3) Uani 1 1 d . . . H4 H -0.4213 0.5748 0.2867 0.062 Uiso 1 1 calc R . . C5 C -0.2702(9) 0.5780(7) 0.2720(6) 0.054(3) Uani 1 1 d . . . H5 H -0.2972 0.5170 0.2496 0.065 Uiso 1 1 calc R . . C6 C -0.1558(8) 0.6322(6) 0.2809(5) 0.046(2) Uani 1 1 d . . . H6 H -0.1061 0.6084 0.2636 0.056 Uiso 1 1 calc R . . C7 C 0.1215(7) 0.7921(5) 0.3873(4) 0.0289(18) Uani 1 1 d . . . C8 C 0.1154(8) 0.7134(6) 0.3935(4) 0.036(2) Uani 1 1 d . . . H8 H 0.0575 0.6593 0.3665 0.043 Uiso 1 1 calc R . . C9 C 0.1940(9) 0.7143(7) 0.4391(5) 0.048(3) Uani 1 1 d . . . H9 H 0.1864 0.6610 0.4448 0.057 Uiso 1 1 calc R . . C10 C 0.2819(9) 0.7908(8) 0.4759(5) 0.052(3) Uani 1 1 d . . . H10 H 0.3367 0.7899 0.5057 0.063 Uiso 1 1 calc R . . C11 C 0.2917(9) 0.8694(7) 0.4700(5) 0.051(3) Uani 1 1 d . . . H11 H 0.3528 0.9225 0.4959 0.061 Uiso 1 1 calc R . . C12 C 0.2106(8) 0.8707(6) 0.4254(4) 0.040(2) Uani 1 1 d . . . H12 H 0.2165 0.9246 0.4214 0.048 Uiso 1 1 calc R . . C13 C 0.0717(7) 0.7440(5) 0.2604(4) 0.0294(18) Uani 1 1 d . . . C14 C 0.0997(7) 0.7165(5) 0.2150(4) 0.0303(19) Uani 1 1 d . . . C15 C 0.2314(7) 0.6324(5) 0.1533(4) 0.0297(18) Uani 1 1 d . . . C16 C 0.3340(8) 0.6554(6) 0.1358(5) 0.042(2) Uani 1 1 d . . . H16 H 0.3587 0.7024 0.1206 0.050 Uiso 1 1 calc R . . C17 C 0.4000(10) 0.6107(7) 0.1405(6) 0.057(3) Uani 1 1 d . . . H17 H 0.4700 0.6266 0.1281 0.068 Uiso 1 1 calc R . . C18 C 0.3651(11) 0.5430(8) 0.1629(5) 0.058(3) Uani 1 1 d . . . H18 H 0.4114 0.5124 0.1663 0.069 Uiso 1 1 calc R . . C19 C 0.2646(12) 0.5196(8) 0.1803(5) 0.060(3) Uani 1 1 d . . . H19 H 0.2408 0.4722 0.1953 0.072 Uiso 1 1 calc R . . C20 C 0.1964(10) 0.5639(7) 0.1765(5) 0.048(3) Uani 1 1 d . . . H20 H 0.1269 0.5480 0.1894 0.058 Uiso 1 1 calc R . . C21 C 0.0070(8) 0.6087(5) 0.0945(4) 0.0311(19) Uani 1 1 d . . . C22 C -0.0204(9) 0.6053(6) 0.0350(4) 0.038(2) Uani 1 1 d . . . H22 H 0.0330 0.6429 0.0193 0.046 Uiso 1 1 calc R . . C23 C -0.1275(9) 0.5461(6) -0.0027(5) 0.044(2) Uani 1 1 d . . . H23 H -0.1466 0.5434 -0.0440 0.053 Uiso 1 1 calc R . . C24 C -0.2038(10) 0.4927(7) 0.0200(5) 0.053(3) Uani 1 1 d . . . H24 H -0.2768 0.4533 -0.0053 0.063 Uiso 1 1 calc R . . C25 C -0.1758(10) 0.4954(8) 0.0798(6) 0.066(3) Uani 1 1 d . . . H25 H -0.2289 0.4574 0.0954 0.079 Uiso 1 1 calc R . . C26 C -0.0720(10) 0.5527(7) 0.1164(5) 0.053(3) Uani 1 1 d . . . H26 H -0.0533 0.5545 0.1575 0.064 Uiso 1 1 calc R . . C27 C -0.1794(7) 1.1233(5) 0.1933(4) 0.0263(17) Uani 1 1 d . . . C28 C -0.1913(8) 1.1956(7) 0.2281(5) 0.051(3) Uani 1 1 d . . . H28 H -0.1269 1.2494 0.2480 0.061 Uiso 1 1 calc R . . C29 C -0.2986(9) 1.1897(8) 0.2343(5) 0.064(4) Uani 1 1 d . . . H29 H -0.3072 1.2399 0.2589 0.077 Uiso 1 1 calc R . . C30 C -0.3924(8) 1.1127(7) 0.2056(5) 0.043(2) Uani 1 1 d . . . H30 H -0.4652 1.1095 0.2107 0.052 Uiso 1 1 calc R . . C31 C -0.3812(8) 1.0423(7) 0.1705(6) 0.051(3) Uani 1 1 d . . . H31 H -0.4466 0.9898 0.1489 0.061 Uiso 1 1 calc R . . C32 C -0.2743(8) 1.0451(6) 0.1651(5) 0.048(3) Uani 1 1 d . . . H32 H -0.2665 0.9937 0.1422 0.057 Uiso 1 1 calc R . . C33 C -0.0173(7) 1.1536(6) 0.1141(4) 0.0281(18) Uani 1 1 d . . . C34 C 0.0308(9) 1.2398(7) 0.1169(5) 0.044(2) Uani 1 1 d . . . H34 H 0.0537 1.2860 0.1556 0.053 Uiso 1 1 calc R . . C35 C 0.0457(10) 1.2589(7) 0.0638(5) 0.051(3) Uani 1 1 d . . . H35 H 0.0799 1.3182 0.0663 0.062 Uiso 1 1 calc R . . C36 C 0.0112(9) 1.1923(8) 0.0071(5) 0.048(3) Uani 1 1 d . . . H36 H 0.0189 1.2058 -0.0296 0.058 Uiso 1 1 calc R . . C37 C -0.0340(9) 1.1074(8) 0.0040(4) 0.047(3) Uani 1 1 d . . . H37 H -0.0556 1.0618 -0.0348 0.056 Uiso 1 1 calc R . . C38 C -0.0490(8) 1.0864(6) 0.0568(4) 0.036(2) Uani 1 1 d . . . H38 H -0.0807 1.0269 0.0540 0.043 Uiso 1 1 calc R . . C39 C 0.0589(8) 1.2181(6) 0.2464(4) 0.0281(18) Uani 1 1 d . . . C40 C 0.1282(7) 1.2685(5) 0.2866(4) 0.0251(17) Uani 1 1 d . . . C41 C 0.3054(7) 1.4421(5) 0.3519(4) 0.0275(17) Uani 1 1 d . . . C42 C 0.2403(8) 1.4757(6) 0.3258(5) 0.040(2) Uani 1 1 d . . . H42 H 0.1664 1.4381 0.3011 0.047 Uiso 1 1 calc R . . C43 C 0.2833(10) 1.5647(6) 0.3359(5) 0.048(3) Uani 1 1 d . . . H43 H 0.2381 1.5882 0.3184 0.057 Uiso 1 1 calc R . . C44 C 0.3903(8) 1.6191(6) 0.3707(5) 0.042(2) Uani 1 1 d . . . H44 H 0.4193 1.6799 0.3769 0.050 Uiso 1 1 calc R . . C45 C 0.4551(8) 1.5864(6) 0.3964(5) 0.041(2) Uani 1 1 d . . . H45 H 0.5288 1.6248 0.4212 0.049 Uiso 1 1 calc R . . C46 C 0.4149(7) 1.4972(5) 0.3869(4) 0.0310(19) Uani 1 1 d . . . H46 H 0.4613 1.4744 0.4041 0.037 Uiso 1 1 calc R . . C47 C 0.1888(7) 1.3394(5) 0.4192(4) 0.0306(18) Uani 1 1 d . . . C48 C 0.1007(8) 1.3669(6) 0.4236(5) 0.039(2) Uani 1 1 d . . . H48 H 0.0669 1.3761 0.3895 0.047 Uiso 1 1 calc R . . C49 C 0.0626(9) 1.3808(7) 0.4780(5) 0.050(3) Uani 1 1 d . . . H49 H 0.0023 1.3991 0.4810 0.059 Uiso 1 1 calc R . . C50 C 0.1110(9) 1.3683(7) 0.5265(5) 0.056(3) Uani 1 1 d . . . H50 H 0.0846 1.3785 0.5635 0.067 Uiso 1 1 calc R . . C51 C 0.1974(10) 1.3413(7) 0.5235(5) 0.054(3) Uani 1 1 d . . . H51 H 0.2305 1.3336 0.5585 0.065 Uiso 1 1 calc R . . C52 C 0.2377(8) 1.3248(6) 0.4690(4) 0.037(2) Uani 1 1 d . . . H52 H 0.2962 1.3045 0.4662 0.044 Uiso 1 1 calc R . . C53 C 0.2988(7) 0.9261(5) 0.0911(4) 0.0279(18) Uani 1 1 d . . . C54 C 0.3102(7) 0.8683(6) 0.0514(4) 0.0320(19) Uani 1 1 d . . . C55 C 0.3401(8) 0.8194(6) -0.0048(4) 0.035(2) Uani 1 1 d U . . C56 C 0.3490(14) 0.8701(10) -0.0483(7) 0.089(4) Uani 1 1 d U . . H56A H 0.2840 0.8857 -0.0514 0.133 Uiso 1 1 calc R . . H56B H 0.3495 0.8338 -0.0892 0.133 Uiso 1 1 calc R . . H56C H 0.4193 0.9235 -0.0324 0.133 Uiso 1 1 calc R . . C57 C 0.2451(14) 0.7339(11) -0.0401(8) 0.111(6) Uani 1 1 d U . . H57A H 0.2336 0.6955 -0.0156 0.166 Uiso 1 1 calc R . . H57B H 0.2628 0.7067 -0.0788 0.166 Uiso 1 1 calc R . . H57C H 0.1759 0.7427 -0.0492 0.166 Uiso 1 1 calc R . . C58 C 0.4422(14) 0.8072(13) 0.0137(8) 0.106(5) Uani 1 1 d U . . H58A H 0.5036 0.8642 0.0380 0.159 Uiso 1 1 calc R . . H58B H 0.4644 0.7798 -0.0233 0.159 Uiso 1 1 calc R . . H58C H 0.4268 0.7695 0.0387 0.159 Uiso 1 1 calc R . . C59 C 0.2660(7) 1.1366(5) 0.2162(4) 0.0286(18) Uani 1 1 d . . . C60 C 0.3140(7) 1.1722(5) 0.1811(4) 0.0307(18) Uani 1 1 d . . . C61 C 0.3717(8) 1.2380(5) 0.1530(4) 0.033(2) Uani 1 1 d . . . C62 C 0.3568(9) 1.3222(6) 0.1876(5) 0.045(3) Uani 1 1 d . . . H62A H 0.2758 1.3092 0.1830 0.068 Uiso 1 1 calc R . . H62B H 0.3922 1.3676 0.1703 0.068 Uiso 1 1 calc R . . H62C H 0.3928 1.3431 0.2316 0.068 Uiso 1 1 calc R . . C63 C 0.3168(9) 1.2027(7) 0.0833(5) 0.046(2) Uani 1 1 d . . . H63A H 0.3270 1.1493 0.0629 0.068 Uiso 1 1 calc R . . H63B H 0.3528 1.2470 0.0652 0.068 Uiso 1 1 calc R . . H63C H 0.2357 1.1894 0.0777 0.068 Uiso 1 1 calc R . . C64 C 0.4980(8) 1.2582(7) 0.1626(5) 0.046(2) Uani 1 1 d . . . H64A H 0.5323 1.2821 0.2069 0.070 Uiso 1 1 calc R . . H64B H 0.5347 1.3013 0.1436 0.070 Uiso 1 1 calc R . . H64C H 0.5079 1.2043 0.1434 0.070 Uiso 1 1 calc R . . C65 C 0.0882(7) 1.0666(5) 0.3365(4) 0.0318(19) Uani 1 1 d . . . C66 C 0.0201(8) 1.0563(6) 0.3687(5) 0.041(2) Uani 1 1 d . . . C67 C -0.0554(10) 1.0687(7) 0.4105(6) 0.060(3) Uani 1 1 d U . . C68 C -0.0950(14) 1.1351(11) 0.4003(9) 0.102(5) Uani 1 1 d U . . H68A H -0.0294 1.1898 0.4073 0.153 Uiso 1 1 calc R . . H68B H -0.1425 1.1462 0.4292 0.153 Uiso 1 1 calc R . . H68C H -0.1392 1.1129 0.3578 0.153 Uiso 1 1 calc R . . C69 C 0.0155(15) 1.1070(12) 0.4769(8) 0.116(6) Uani 1 1 d U . . H69A H 0.0462 1.0662 0.4842 0.175 Uiso 1 1 calc R . . H69B H -0.0324 1.1163 0.5060 0.175 Uiso 1 1 calc R . . H69C H 0.0780 1.1631 0.4831 0.175 Uiso 1 1 calc R . . C70 C -0.1534(11) 0.9857(8) 0.4045(7) 0.074(4) Uani 1 1 d U . . H70A H -0.1957 0.9560 0.3613 0.111 Uiso 1 1 calc R . . H70B H -0.2036 0.9998 0.4306 0.111 Uiso 1 1 calc R . . H70C H -0.1250 0.9472 0.4176 0.111 Uiso 1 1 calc R . . C71 C -0.0040(7) 0.8788(5) 0.1721(4) 0.0257(17) Uani 1 1 d . . . C72 C -0.1057(7) 0.8494(5) 0.1520(4) 0.0284(18) Uani 1 1 d . . . C73 C -0.2283(7) 0.7909(5) 0.1291(4) 0.034(2) Uani 1 1 d . . . C74 C -0.2392(9) 0.6980(6) 0.1195(7) 0.064(4) Uani 1 1 d . . . H74A H -0.1968 0.6819 0.0889 0.096 Uiso 1 1 calc R . . H74B H -0.3192 0.6572 0.1047 0.096 Uiso 1 1 calc R . . H74C H -0.2085 0.6952 0.1587 0.096 Uiso 1 1 calc R . . C75 C -0.2736(9) 0.7984(8) 0.0679(5) 0.058(3) Uani 1 1 d . . . H75A H -0.2693 0.8577 0.0756 0.087 Uiso 1 1 calc R . . H75B H -0.3525 0.7559 0.0508 0.087 Uiso 1 1 calc R . . H75C H -0.2275 0.7863 0.0383 0.087 Uiso 1 1 calc R . . C76 C -0.2924(9) 0.8173(7) 0.1772(5) 0.052(3) Uani 1 1 d . . . H76A H -0.2644 0.8111 0.2156 0.078 Uiso 1 1 calc R . . H76B H -0.3734 0.7794 0.1618 0.078 Uiso 1 1 calc R . . H76C H -0.2806 0.8784 0.1851 0.078 Uiso 1 1 calc R . . C77 C 0.4923(7) 1.2018(5) 0.3483(4) 0.0288(18) Uani 1 1 d . . . C78 C 0.5556(7) 1.2805(6) 0.3703(4) 0.0286(18) Uani 1 1 d . . . C79 C 0.6540(7) 1.3678(5) 0.3995(4) 0.0325(19) Uani 1 1 d . . . C80 C 0.6603(8) 1.4213(6) 0.3563(4) 0.035(2) Uani 1 1 d . . . H80A H 0.6677 1.3887 0.3160 0.053 Uiso 1 1 calc R . . H80B H 0.7262 1.4777 0.3744 0.053 Uiso 1 1 calc R . . H80C H 0.5911 1.4313 0.3512 0.053 Uiso 1 1 calc R . . C81 C 0.6404(8) 1.4158(6) 0.4626(4) 0.040(2) Uani 1 1 d . . . H81A H 0.5666 1.4191 0.4582 0.061 Uiso 1 1 calc R . . H81B H 0.7008 1.4751 0.4797 0.061 Uiso 1 1 calc R . . H81C H 0.6452 1.3839 0.4906 0.061 Uiso 1 1 calc R . . C82 C 0.7624(7) 1.3512(6) 0.4065(5) 0.039(2) Uani 1 1 d . . . H82A H 0.7579 1.3158 0.4329 0.058 Uiso 1 1 calc R . . H82B H 0.8285 1.4074 0.4254 0.058 Uiso 1 1 calc R . . H82C H 0.7698 1.3200 0.3658 0.058 Uiso 1 1 calc R . . C83 C 0.3028(7) 0.9340(5) 0.2652(4) 0.0260(17) Uani 1 1 d . . . C84 C 0.3877(7) 0.9345(5) 0.2939(4) 0.0282(18) Uani 1 1 d . . . C85 C 0.4739(8) 0.9076(6) 0.3187(4) 0.034(2) Uani 1 1 d . . . C86 C 0.5569(9) 0.9089(8) 0.2773(5) 0.051(3) Uani 1 1 d . . . H86A H 0.5155 0.8724 0.2346 0.076 Uiso 1 1 calc R . . H86B H 0.6096 0.8861 0.2910 0.076 Uiso 1 1 calc R . . H86C H 0.5993 0.9692 0.2795 0.076 Uiso 1 1 calc R . . C87 C 0.4107(9) 0.8131(6) 0.3168(5) 0.046(2) Uani 1 1 d . . . H87A H 0.3564 0.8118 0.3434 0.069 Uiso 1 1 calc R . . H87B H 0.4653 0.7925 0.3315 0.069 Uiso 1 1 calc R . . H87C H 0.3701 0.7750 0.2743 0.069 Uiso 1 1 calc R . . C88 C 0.5332(8) 0.9676(6) 0.3849(4) 0.040(2) Uani 1 1 d . . . H88A H 0.5764 1.0271 0.3858 0.060 Uiso 1 1 calc R . . H88B H 0.5847 0.9462 0.4019 0.060 Uiso 1 1 calc R . . H88C H 0.4766 0.9682 0.4099 0.060 Uiso 1 1 calc R . . Cl1 Cl -0.3667(4) 0.8551(3) 0.5007(2) 0.0292(8) Uani 0.50 1 d P . . O1 O -0.4201(10) 0.7811(7) 0.5126(5) 0.031(3) Uani 0.50 1 d P . . O2 O -0.3654(16) 0.8290(11) 0.4378(8) 0.070(5) Uani 0.50 1 d P . . O3 O -0.277(3) 0.8948(15) 0.5352(12) 0.118(9) Uani 0.50 1 d P . . O4 O -0.4277(16) 0.9066(11) 0.5122(9) 0.072(5) Uani 0.50 1 d P . . Cl2 Cl -0.0631(2) 1.43993(18) 0.25425(15) 0.0555(7) Uani 1 1 d . . . O5 O -0.1747(7) 1.4198(6) 0.2254(5) 0.081(3) Uani 1 1 d . . . O6 O -0.0140(8) 1.3903(6) 0.2129(5) 0.082(3) Uani 1 1 d . . . O7 O 0.0087(7) 1.5297(5) 0.2674(4) 0.062(2) Uani 1 1 d . . . O8 O -0.0646(9) 1.4193(8) 0.3062(5) 0.099(3) Uani 1 1 d . . . Cl3 Cl 0.4870(5) 0.4321(4) 0.0466(3) 0.0666(18) Uani 0.50 1 d P . . O9 O 0.3737(15) 0.4004(9) 0.0437(8) 0.067(5) Uani 0.50 1 d P . . O10 O 0.5158(12) 0.3859(10) -0.0019(9) 0.071(5) Uani 0.50 1 d P . . O11 O 0.524(3) 0.5172(17) 0.0400(19) 0.23(3) Uani 0.50 1 d P . . O12 O 0.5451(17) 0.4485(16) 0.0968(11) 0.091(7) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.03229(17) 0.02457(15) 0.02558(17) 0.00622(13) 0.00716(13) 0.01180(13) Au2 0.02771(16) 0.02229(14) 0.02247(16) 0.00762(12) 0.00798(12) 0.01176(12) Au3 0.02408(15) 0.01906(14) 0.02112(15) 0.00565(11) 0.00427(12) 0.01050(11) Au4 0.02497(15) 0.01929(14) 0.02420(16) 0.00508(12) 0.00238(12) 0.01052(12) Au5 0.02267(15) 0.02216(14) 0.03075(17) 0.00708(13) 0.00390(13) 0.00925(12) Au6 0.02504(16) 0.02177(15) 0.03074(17) 0.00808(13) 0.00432(13) 0.01041(12) Au7 0.02671(16) 0.02186(14) 0.02699(17) 0.00719(12) 0.00469(13) 0.01156(12) Au8 0.02464(15) 0.02306(15) 0.02462(16) 0.00526(12) 0.00253(12) 0.01182(12) P1 0.0311(11) 0.0285(11) 0.0221(11) 0.0084(9) 0.0095(9) 0.0129(9) P2 0.0321(11) 0.0217(10) 0.0202(10) 0.0047(8) 0.0064(9) 0.0103(9) P3 0.0236(10) 0.0248(10) 0.0235(11) 0.0056(8) 0.0008(8) 0.0116(8) P4 0.0234(10) 0.0231(10) 0.0263(11) 0.0052(8) 0.0043(9) 0.0086(8) C1 0.031(4) 0.038(5) 0.028(5) 0.018(4) 0.012(4) 0.014(4) C2 0.054(6) 0.035(5) 0.056(7) 0.013(5) 0.028(5) 0.014(5) C3 0.048(6) 0.056(7) 0.098(10) 0.042(7) 0.045(7) 0.032(6) C4 0.030(5) 0.059(7) 0.068(8) 0.029(6) 0.020(5) 0.011(5) C5 0.036(6) 0.044(6) 0.071(8) 0.011(6) 0.008(5) 0.009(5) C6 0.029(5) 0.043(6) 0.057(7) 0.008(5) 0.014(5) 0.009(4) C7 0.037(5) 0.032(4) 0.018(4) 0.009(3) 0.012(4) 0.013(4) C8 0.041(5) 0.038(5) 0.028(5) 0.011(4) 0.015(4) 0.015(4) C9 0.058(7) 0.059(7) 0.042(6) 0.028(5) 0.013(5) 0.034(6) C10 0.051(6) 0.076(8) 0.029(5) 0.024(5) 0.003(5) 0.022(6) C11 0.048(6) 0.057(7) 0.032(6) 0.012(5) 0.003(5) 0.009(5) C12 0.043(6) 0.042(5) 0.028(5) 0.010(4) 0.011(4) 0.011(4) C13 0.037(5) 0.024(4) 0.023(4) 0.013(3) 0.000(4) 0.005(4) C14 0.041(5) 0.015(4) 0.021(4) 0.008(3) 0.009(4) -0.005(3) C15 0.037(5) 0.026(4) 0.024(4) 0.005(3) 0.006(4) 0.014(4) C16 0.038(5) 0.026(4) 0.056(7) 0.011(4) 0.003(5) 0.013(4) C17 0.055(7) 0.055(7) 0.077(9) 0.024(6) 0.020(6) 0.037(6) C18 0.076(8) 0.060(7) 0.059(7) 0.023(6) 0.010(6) 0.051(7) C19 0.108(10) 0.056(7) 0.056(7) 0.036(6) 0.041(7) 0.058(7) C20 0.077(8) 0.053(6) 0.047(6) 0.033(5) 0.034(6) 0.044(6) C21 0.040(5) 0.027(4) 0.026(5) 0.005(4) 0.004(4) 0.017(4) C22 0.059(6) 0.027(4) 0.032(5) 0.007(4) 0.004(4) 0.025(4) C23 0.057(6) 0.037(5) 0.034(5) 0.005(4) -0.001(5) 0.024(5) C24 0.049(6) 0.037(6) 0.050(7) 0.004(5) -0.006(5) 0.005(5) C25 0.056(7) 0.050(7) 0.056(8) 0.012(6) 0.005(6) -0.010(5) C26 0.060(7) 0.041(6) 0.035(6) 0.013(5) 0.003(5) -0.004(5) C27 0.027(4) 0.031(4) 0.027(4) 0.013(4) 0.008(3) 0.015(3) C28 0.032(5) 0.048(6) 0.052(7) -0.011(5) -0.005(5) 0.020(5) C29 0.046(6) 0.076(8) 0.052(7) -0.019(6) 0.002(5) 0.039(6) C30 0.035(5) 0.061(7) 0.041(6) 0.024(5) 0.015(4) 0.023(5) C31 0.024(5) 0.041(6) 0.083(8) 0.030(6) 0.006(5) 0.004(4) C32 0.034(5) 0.034(5) 0.070(8) 0.016(5) 0.008(5) 0.011(4) C33 0.027(4) 0.037(5) 0.026(4) 0.013(4) 0.005(3) 0.019(4) C34 0.053(6) 0.048(6) 0.038(6) 0.018(5) 0.005(5) 0.026(5) C35 0.071(8) 0.056(7) 0.050(7) 0.039(6) 0.019(6) 0.033(6) C36 0.050(6) 0.076(8) 0.047(7) 0.040(6) 0.019(5) 0.041(6) C37 0.048(6) 0.073(7) 0.023(5) 0.012(5) 0.005(4) 0.033(6) C38 0.035(5) 0.043(5) 0.031(5) 0.010(4) 0.006(4) 0.020(4) C39 0.039(5) 0.041(5) 0.030(5) 0.025(4) 0.015(4) 0.032(4) C40 0.025(4) 0.020(4) 0.043(5) 0.016(4) 0.017(4) 0.017(3) C41 0.031(4) 0.026(4) 0.032(5) 0.011(4) 0.017(4) 0.016(4) C42 0.037(5) 0.033(5) 0.048(6) 0.013(4) 0.007(4) 0.017(4) C43 0.068(7) 0.040(5) 0.046(6) 0.016(5) 0.011(5) 0.034(5) C44 0.047(6) 0.028(5) 0.053(6) 0.018(4) 0.017(5) 0.014(4) C45 0.030(5) 0.035(5) 0.054(6) 0.017(5) 0.019(5) 0.008(4) C46 0.031(5) 0.024(4) 0.038(5) 0.012(4) 0.007(4) 0.010(3) C47 0.023(4) 0.028(4) 0.032(5) 0.008(4) 0.008(4) 0.002(3) C48 0.032(5) 0.044(5) 0.038(5) 0.009(4) 0.008(4) 0.016(4) C49 0.035(5) 0.052(6) 0.041(6) -0.003(5) 0.009(5) 0.010(5) C50 0.045(6) 0.049(6) 0.038(6) -0.004(5) 0.019(5) -0.006(5) C51 0.055(7) 0.063(7) 0.034(6) 0.023(5) 0.005(5) 0.009(6) C52 0.036(5) 0.042(5) 0.026(5) 0.015(4) 0.009(4) 0.007(4) C53 0.024(4) 0.025(4) 0.036(5) 0.010(4) 0.011(4) 0.012(3) C54 0.026(4) 0.034(5) 0.044(5) 0.026(4) 0.011(4) 0.012(4) C55 0.040(5) 0.041(4) 0.033(5) 0.015(4) 0.020(4) 0.024(4) C56 0.117(9) 0.092(8) 0.080(8) 0.043(6) 0.055(7) 0.050(6) C57 0.099(9) 0.113(9) 0.088(8) -0.009(6) 0.052(7) 0.035(7) C58 0.099(8) 0.149(10) 0.090(9) 0.019(7) 0.018(6) 0.091(8) C59 0.027(4) 0.023(4) 0.032(5) 0.006(4) 0.003(4) 0.010(3) C60 0.028(4) 0.031(4) 0.035(5) 0.010(4) 0.002(4) 0.016(4) C61 0.043(5) 0.028(4) 0.038(5) 0.018(4) 0.013(4) 0.017(4) C62 0.065(7) 0.030(5) 0.059(7) 0.029(5) 0.032(6) 0.023(5) C63 0.056(6) 0.049(6) 0.040(6) 0.026(5) 0.010(5) 0.022(5) C64 0.040(6) 0.047(6) 0.054(7) 0.020(5) 0.015(5) 0.017(5) C65 0.035(5) 0.030(4) 0.025(5) 0.006(4) 0.007(4) 0.009(4) C66 0.032(5) 0.027(5) 0.058(7) 0.008(4) 0.015(5) 0.010(4) C67 0.053(6) 0.046(5) 0.076(7) 0.011(5) 0.034(5) 0.019(4) C68 0.101(8) 0.089(8) 0.135(10) 0.034(7) 0.064(7) 0.055(7) C69 0.106(9) 0.120(10) 0.101(9) 0.021(7) 0.061(8) 0.026(7) C70 0.056(6) 0.060(6) 0.100(8) 0.019(6) 0.039(6) 0.019(5) C71 0.034(5) 0.022(4) 0.021(4) 0.005(3) 0.005(3) 0.014(3) C72 0.033(5) 0.023(4) 0.028(5) 0.005(3) 0.009(4) 0.013(4) C73 0.027(4) 0.025(4) 0.040(5) 0.002(4) 0.002(4) 0.010(4) C74 0.041(6) 0.029(5) 0.101(10) 0.005(6) 0.002(6) 0.008(5) C75 0.029(5) 0.075(8) 0.048(7) 0.004(6) -0.010(5) 0.016(5) C76 0.039(6) 0.039(6) 0.070(8) 0.011(5) 0.022(5) 0.012(5) C77 0.028(4) 0.029(4) 0.036(5) 0.013(4) 0.010(4) 0.017(4) C78 0.027(4) 0.036(5) 0.029(5) 0.012(4) 0.009(4) 0.017(4) C79 0.028(4) 0.024(4) 0.034(5) 0.007(4) 0.003(4) 0.002(3) C80 0.034(5) 0.035(5) 0.033(5) 0.014(4) 0.007(4) 0.008(4) C81 0.041(5) 0.039(5) 0.031(5) 0.009(4) 0.009(4) 0.007(4) C82 0.020(4) 0.044(5) 0.042(6) 0.014(4) 0.001(4) 0.005(4) C83 0.033(4) 0.019(4) 0.024(4) 0.004(3) 0.003(4) 0.011(3) C84 0.034(5) 0.027(4) 0.029(5) 0.014(4) 0.014(4) 0.015(4) C85 0.036(5) 0.036(5) 0.032(5) 0.009(4) -0.002(4) 0.023(4) C86 0.049(6) 0.069(7) 0.053(7) 0.026(6) 0.012(5) 0.039(6) C87 0.059(7) 0.038(5) 0.042(6) 0.011(4) -0.004(5) 0.027(5) C88 0.043(5) 0.041(5) 0.035(5) 0.011(4) 0.001(4) 0.020(4) Cl1 0.027(2) 0.029(2) 0.035(2) 0.0148(18) 0.0055(18) 0.0133(17) O1 0.045(7) 0.015(5) 0.026(6) 0.004(5) 0.003(5) 0.007(5) O2 0.083(13) 0.069(11) 0.072(12) 0.032(10) 0.028(10) 0.038(10) O3 0.18(3) 0.081(16) 0.11(2) 0.044(15) 0.025(19) 0.068(18) O4 0.089(13) 0.056(10) 0.075(13) 0.019(9) 0.026(10) 0.034(10) Cl2 0.0488(15) 0.0481(15) 0.083(2) 0.0317(15) 0.0233(15) 0.0262(12) O5 0.039(4) 0.057(5) 0.125(9) 0.005(5) 0.002(5) 0.021(4) O6 0.082(7) 0.073(6) 0.103(8) 0.021(6) 0.040(6) 0.047(5) O7 0.055(5) 0.053(5) 0.079(6) 0.027(4) 0.023(4) 0.017(4) O8 0.084(7) 0.142(10) 0.087(8) 0.065(8) 0.036(6) 0.040(7) Cl3 0.046(3) 0.049(3) 0.052(4) -0.013(3) 0.014(3) -0.015(3) O9 0.091(13) 0.026(7) 0.067(11) 0.004(7) 0.033(10) 0.011(8) O10 0.033(8) 0.046(9) 0.092(13) -0.007(9) 0.025(8) -0.007(7) O11 0.15(3) 0.071(18) 0.30(5) -0.06(2) 0.14(3) -0.050(17) O12 0.067(12) 0.15(2) 0.101(17) 0.083(16) 0.042(12) 0.053(13) _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 C65 2.188(8) . ? Au1 P1 2.264(2) . yes Au1 C66 2.306(9) . ? Au1 Au3 3.0711(5) . yes Au2 C53 2.219(8) . ? Au2 C54 2.263(8) . ? Au2 P2 2.278(2) . yes Au2 Au3 2.9349(4) . yes Au3 C83 1.992(8) . ? Au3 C71 2.000(8) . ? Au3 Au4 2.9427(4) . yes Au3 Au7 3.1160(4) . yes Au4 C59 1.981(9) . ? Au4 C65 2.008(9) . ? Au4 Au5 2.9455(5) . yes Au4 Au8 2.9802(5) . yes Au4 Au6 3.1784(4) . yes Au5 C77 2.220(8) . ? Au5 P4 2.276(2) . yes Au5 C78 2.282(8) . ? Au6 C77 1.973(8) . ? Au6 C83 2.186(8) . ? Au6 C84 2.232(8) . ? Au7 C53 1.983(8) . ? Au7 C59 2.195(8) . ? Au7 C60 2.240(8) . ? Au8 C71 2.197(7) . ? Au8 P3 2.263(2) . yes Au8 C72 2.295(8) . ? P1 C13 1.761(9) . ? P1 C7 1.794(9) . ? P1 C1 1.813(9) . ? P2 C14 1.777(9) . ? P2 C21 1.797(9) . ? P2 C15 1.809(8) . ? P3 C39 1.806(10) . ? P3 C27 1.809(8) . ? P3 C33 1.814(8) . ? P4 C40 1.807(10) . ? P4 C47 1.808(9) . ? P4 C41 1.818(8) . ? C1 C6 1.386(13) . ? C1 C2 1.394(13) . ? C2 C3 1.383(15) . ? C2 H2 0.9500 . ? C3 C4 1.358(16) . ? C3 H3 0.9500 . ? C4 C5 1.360(15) . ? C4 H4 0.9500 . ? C5 C6 1.398(14) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.398(12) . ? C7 C12 1.399(13) . ? C8 C9 1.391(13) . ? C8 H8 0.9500 . ? C9 C10 1.366(15) . ? C9 H9 0.9500 . ? C10 C11 1.382(15) . ? C10 H10 0.9500 . ? C11 C12 1.415(14) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.177(12) . ? C15 C16 1.384(13) . ? C15 C20 1.398(12) . ? C16 C17 1.368(13) . ? C16 H16 0.9500 . ? C17 C18 1.375(16) . ? C17 H17 0.9500 . ? C18 C19 1.360(17) . ? C18 H18 0.9500 . ? C19 C20 1.385(14) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.371(12) . ? C21 C26 1.389(13) . ? C22 C23 1.403(14) . ? C22 H22 0.9500 . ? C23 C24 1.361(15) . ? C23 H23 0.9500 . ? C24 C25 1.382(16) . ? C24 H24 0.9500 . ? C25 C26 1.360(15) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.361(12) . ? C27 C32 1.386(13) . ? C28 C29 1.386(14) . ? C28 H28 0.9500 . ? C29 C30 1.370(15) . ? C29 H29 0.9500 . ? C30 C31 1.332(15) . ? C30 H30 0.9500 . ? C31 C32 1.391(14) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.385(13) . ? C33 C38 1.398(12) . ? C34 C35 1.379(13) . ? C34 H34 0.9500 . ? C35 C36 1.383(15) . ? C35 H35 0.9500 . ? C36 C37 1.361(15) . ? C36 H36 0.9500 . ? C37 C38 1.388(13) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.116(12) . ? C41 C42 1.376(12) . ? C41 C46 1.394(12) . ? C42 C43 1.387(13) . ? C42 H42 0.9500 . ? C43 C44 1.367(15) . ? C43 H43 0.9500 . ? C44 C45 1.357(13) . ? C44 H44 0.9500 . ? C45 C46 1.393(12) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C48 1.395(12) . ? C47 C52 1.396(12) . ? C48 C49 1.391(14) . ? C48 H48 0.9500 . ? C49 C50 1.346(16) . ? C49 H49 0.9500 . ? C50 C51 1.367(17) . ? C50 H50 0.9500 . ? C51 C52 1.409(14) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C54 1.221(12) . ? C54 C55 1.508(13) . ? C55 C58 1.462(16) . ? C55 C57 1.479(18) . ? C55 C56 1.511(16) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 C60 1.245(12) . ? C60 C61 1.490(12) . ? C61 C64 1.527(13) . ? C61 C63 1.543(13) . ? C61 C62 1.551(12) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 C66 1.211(13) . ? C66 C67 1.472(14) . ? C67 C68 1.495(19) . ? C67 C70 1.502(16) . ? C67 C69 1.54(2) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 C72 1.216(11) . ? C72 C73 1.486(12) . ? C73 C76 1.522(13) . ? C73 C74 1.525(13) . ? C73 C75 1.544(14) . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 C78 1.233(12) . ? C78 C79 1.498(12) . ? C79 C81 1.526(13) . ? C79 C82 1.540(12) . ? C79 C80 1.544(12) . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 C84 1.227(11) . ? C84 C85 1.490(11) . ? C85 C86 1.512(14) . ? C85 C88 1.519(12) . ? C85 C87 1.539(13) . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? Cl1 O3 1.18(3) . ? Cl1 O1 1.351(11) . ? Cl1 O4 1.388(17) . ? Cl1 O2 1.404(18) . ? Cl2 O8 1.355(10) . ? Cl2 O5 1.408(8) . ? Cl2 O7 1.425(8) . ? Cl2 O6 1.458(9) . ? Cl3 O12 1.22(2) . ? Cl3 O10 1.354(17) . ? Cl3 O9 1.359(18) . ? Cl3 O11 1.45(4) . ? O11 O11 1.75(9) 2_665 ? 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 C65 Au1 P1 176.4(2) . . ? C65 Au1 C66 31.1(3) . . ? P1 Au1 C66 152.2(3) . . ? C65 Au1 Au3 86.7(2) . . ? P1 Au1 Au3 90.59(5) . . ? C66 Au1 Au3 116.1(3) . . ? C53 Au2 C54 31.6(3) . . ? C53 Au2 P2 179.1(2) . . ? C54 Au2 P2 148.8(2) . . ? C53 Au2 Au3 88.4(2) . . ? C54 Au2 Au3 119.9(2) . . ? P2 Au2 Au3 91.13(5) . . ? C83 Au3 C71 171.4(3) . . ? C83 Au3 Au2 82.1(2) . . ? C71 Au3 Au2 98.0(2) . . ? C83 Au3 Au4 93.2(2) . . ? C71 Au3 Au4 92.2(2) . . ? Au2 Au3 Au4 140.591(14) . . ? C83 Au3 Au1 91.7(2) . . ? C71 Au3 Au1 83.9(2) . . ? Au2 Au3 Au1 149.512(13) . . ? Au4 Au3 Au1 69.229(11) . . ? C83 Au3 Au7 87.9(2) . . ? C71 Au3 Au7 100.3(2) . . ? Au2 Au3 Au7 70.712(11) . . ? Au4 Au3 Au7 70.030(11) . . ? Au1 Au3 Au7 139.165(13) . . ? C59 Au4 C65 170.9(3) . . ? C59 Au4 Au3 92.9(2) . . ? C65 Au4 Au3 93.6(2) . . ? C59 Au4 Au5 73.9(2) . . ? C65 Au4 Au5 105.3(2) . . ? Au3 Au4 Au5 137.186(14) . . ? C59 Au4 Au8 89.0(2) . . ? C65 Au4 Au8 87.2(3) . . ? Au3 Au4 Au8 69.936(11) . . ? Au5 Au4 Au8 147.138(13) . . ? C59 Au4 Au6 80.6(2) . . ? C65 Au4 Au6 107.8(3) . . ? Au3 Au4 Au6 69.030(10) . . ? Au5 Au4 Au6 68.701(11) . . ? Au8 Au4 Au6 136.964(13) . . ? C77 Au5 P4 178.0(2) . . ? C77 Au5 C78 31.8(3) . . ? P4 Au5 C78 148.9(2) . . ? C77 Au5 Au4 90.7(2) . . ? P4 Au5 Au4 88.91(5) . . ? C78 Au5 Au4 122.0(2) . . ? C77 Au6 C83 171.4(3) . . ? C77 Au6 C84 156.1(3) . . ? C83 Au6 C84 32.2(3) . . ? C77 Au6 Au4 88.9(2) . . ? C83 Au6 Au4 83.4(2) . . ? C84 Au6 Au4 114.6(2) . . ? C53 Au7 C59 172.1(3) . . ? C53 Au7 C60 155.3(3) . . ? C59 Au7 C60 32.6(3) . . ? C53 Au7 Au3 87.8(2) . . ? C59 Au7 Au3 84.3(2) . . ? C60 Au7 Au3 116.8(2) . . ? C71 Au8 P3 176.7(2) . . ? C71 Au8 C72 31.3(3) . . ? P3 Au8 C72 151.2(2) . . ? C71 Au8 Au4 87.3(2) . . ? P3 Au8 Au4 91.18(5) . . ? C72 Au8 Au4 115.7(2) . . ? C13 P1 C7 101.8(4) . . ? C13 P1 C1 103.3(4) . . ? C7 P1 C1 111.2(4) . . ? C13 P1 Au1 111.3(3) . . ? C7 P1 Au1 113.7(3) . . ? C1 P1 Au1 114.4(3) . . ? C14 P2 C21 99.8(4) . . ? C14 P2 C15 106.2(4) . . ? C21 P2 C15 108.5(4) . . ? C14 P2 Au2 110.9(3) . . ? C21 P2 Au2 115.1(3) . . ? C15 P2 Au2 114.9(3) . . ? C39 P3 C27 104.9(4) . . ? C39 P3 C33 105.2(4) . . ? C27 P3 C33 108.2(4) . . ? C39 P3 Au8 112.3(2) . . ? C27 P3 Au8 112.6(3) . . ? C33 P3 Au8 113.0(3) . . ? C40 P4 C47 105.1(4) . . ? C40 P4 C41 106.3(4) . . ? C47 P4 C41 103.1(4) . . ? C40 P4 Au5 111.4(2) . . ? C47 P4 Au5 114.3(3) . . ? C41 P4 Au5 115.7(3) . . ? C6 C1 C2 118.1(8) . . ? C6 C1 P1 122.0(7) . . ? C2 C1 P1 119.9(7) . . ? C3 C2 C1 120.9(10) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C4 C3 C2 120.3(10) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 120.1(10) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 C6 120.7(10) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C1 C6 C5 119.8(9) . . ? C1 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C8 C7 C12 119.2(8) . . ? C8 C7 P1 122.4(7) . . ? C12 C7 P1 117.9(7) . . ? C9 C8 C7 120.0(9) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C10 C9 C8 120.9(10) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C9 C10 C11 120.3(10) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C10 C11 C12 119.9(10) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C7 C12 C11 119.6(9) . . ? C7 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C14 C13 P1 173.4(7) . . ? C13 C14 P2 171.6(7) . . ? C16 C15 C20 119.5(8) . . ? C16 C15 P2 120.2(6) . . ? C20 C15 P2 120.3(7) . . ? C17 C16 C15 120.3(9) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 120.2(11) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C19 C18 C17 120.3(10) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 120.8(10) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C19 C20 C15 118.9(10) . . ? C19 C20 H20 120.5 . . ? C15 C20 H20 120.5 . . ? C22 C21 C26 119.1(9) . . ? C22 C21 P2 119.7(7) . . ? C26 C21 P2 121.1(7) . . ? C21 C22 C23 119.9(9) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C24 C23 C22 119.9(10) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C25 120.3(10) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 119.8(11) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C21 121.0(10) . . ? C25 C26 H26 119.5 . . ? C21 C26 H26 119.5 . . ? C28 C27 C32 119.6(9) . . ? C28 C27 P3 122.1(7) . . ? C32 C27 P3 118.3(7) . . ? C27 C28 C29 119.2(10) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C30 C29 C28 121.1(10) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C31 C30 C29 119.9(9) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C30 C31 C32 120.5(10) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C27 C32 C31 119.7(9) . . ? C27 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C34 C33 C38 119.0(8) . . ? C34 C33 P3 122.0(7) . . ? C38 C33 P3 119.1(7) . . ? C35 C34 C33 120.4(10) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C34 C35 C36 120.5(10) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C37 C36 C35 119.5(9) . . ? C37 C36 H36 120.3 . . ? C35 C36 H36 120.3 . . ? C36 C37 C38 121.1(10) . . ? C36 C37 H37 119.4 . . ? C38 C37 H37 119.4 . . ? C37 C38 C33 119.5(9) . . ? C37 C38 H38 120.3 . . ? C33 C38 H38 120.3 . . ? C40 C39 P3 170.9(7) . . ? C39 C40 P4 167.5(7) . . ? C42 C41 C46 119.9(8) . . ? C42 C41 P4 122.5(7) . . ? C46 C41 P4 117.1(6) . . ? C41 C42 C43 119.6(9) . . ? C41 C42 H42 120.2 . . ? C43 C42 H42 120.2 . . ? C44 C43 C42 120.5(9) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? C45 C44 C43 120.2(9) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? C44 C45 C46 120.8(9) . . ? C44 C45 H45 119.6 . . ? C46 C45 H45 119.6 . . ? C45 C46 C41 118.9(8) . . ? C45 C46 H46 120.5 . . ? C41 C46 H46 120.5 . . ? C48 C47 C52 120.2(8) . . ? C48 C47 P4 120.7(7) . . ? C52 C47 P4 119.0(7) . . ? C49 C48 C47 119.8(9) . . ? C49 C48 H48 120.1 . . ? C47 C48 H48 120.1 . . ? C50 C49 C48 120.1(10) . . ? C50 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? C49 C50 C51 121.5(10) . . ? C49 C50 H50 119.3 . . ? C51 C50 H50 119.3 . . ? C50 C51 C52 120.6(10) . . ? C50 C51 H51 119.7 . . ? C52 C51 H51 119.7 . . ? C47 C52 C51 117.9(9) . . ? C47 C52 H52 121.1 . . ? C51 C52 H52 121.1 . . ? C54 C53 Au7 170.8(7) . . ? C54 C53 Au2 76.2(5) . . ? Au7 C53 Au2 112.9(4) . . ? C53 C54 C55 162.6(8) . . ? C53 C54 Au2 72.2(6) . . ? C55 C54 Au2 125.2(6) . . ? C58 C55 C57 110.5(12) . . ? C58 C55 C54 110.1(9) . . ? C57 C55 C54 111.1(9) . . ? C58 C55 C56 114.9(12) . . ? C57 C55 C56 103.4(12) . . ? C54 C55 C56 106.6(8) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 C57 H57A 109.5 . . ? C55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C55 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C55 C58 H58A 109.5 . . ? C55 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C55 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C60 C59 Au4 171.2(7) . . ? C60 C59 Au7 75.7(6) . . ? Au4 C59 Au7 112.8(4) . . ? C59 C60 C61 163.0(9) . . ? C59 C60 Au7 71.7(5) . . ? C61 C60 Au7 125.2(6) . . ? C60 C61 C64 110.3(7) . . ? C60 C61 C63 109.5(8) . . ? C64 C61 C63 110.2(8) . . ? C60 C61 C62 106.2(7) . . ? C64 C61 C62 109.0(8) . . ? C63 C61 C62 111.5(8) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C66 C65 Au4 168.4(8) . . ? C66 C65 Au1 79.8(6) . . ? Au4 C65 Au1 109.0(4) . . ? C65 C66 C67 164.6(10) . . ? C65 C66 Au1 69.0(6) . . ? C67 C66 Au1 126.2(7) . . ? C66 C67 C68 108.5(11) . . ? C66 C67 C70 114.2(10) . . ? C68 C67 C70 111.4(12) . . ? C66 C67 C69 107.4(11) . . ? C68 C67 C69 107.6(13) . . ? C70 C67 C69 107.4(12) . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C67 C69 H69A 109.5 . . ? C67 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C67 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C67 C70 H70A 109.5 . . ? C67 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C67 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C72 C71 Au3 168.6(7) . . ? C72 C71 Au8 78.8(5) . . ? Au3 C71 Au8 107.9(3) . . ? C71 C72 C73 163.9(8) . . ? C71 C72 Au8 69.9(5) . . ? C73 C72 Au8 125.9(6) . . ? C72 C73 C76 109.4(8) . . ? C72 C73 C74 106.8(7) . . ? C76 C73 C74 110.1(9) . . ? C72 C73 C75 109.5(8) . . ? C76 C73 C75 109.9(8) . . ? C74 C73 C75 111.0(9) . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C73 C75 H75A 109.5 . . ? C73 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C73 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C73 C76 H76A 109.5 . . ? C73 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C73 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C78 C77 Au6 171.9(7) . . ? C78 C77 Au5 76.9(5) . . ? Au6 C77 Au5 111.1(4) . . ? C77 C78 C79 166.0(8) . . ? C77 C78 Au5 71.4(5) . . ? C79 C78 Au5 122.6(6) . . ? C78 C79 C81 109.8(7) . . ? C78 C79 C82 107.6(7) . . ? C81 C79 C82 110.3(8) . . ? C78 C79 C80 109.0(7) . . ? C81 C79 C80 111.0(7) . . ? C82 C79 C80 109.1(7) . . ? C79 C80 H80A 109.5 . . ? C79 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C79 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C79 C81 H81A 109.5 . . ? C79 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C79 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C79 C82 H82A 109.5 . . ? C79 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C79 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C84 C83 Au3 171.5(7) . . ? C84 C83 Au6 75.9(5) . . ? Au3 C83 Au6 112.4(3) . . ? C83 C84 C85 163.5(9) . . ? C83 C84 Au6 71.8(5) . . ? C85 C84 Au6 124.5(6) . . ? C84 C85 C86 108.8(7) . . ? C84 C85 C88 110.3(7) . . ? C86 C85 C88 111.6(8) . . ? C84 C85 C87 107.2(7) . . ? C86 C85 C87 109.1(8) . . ? C88 C85 C87 109.7(8) . . ? C85 C86 H86A 109.5 . . ? C85 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C85 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C85 C87 H87A 109.5 . . ? C85 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C85 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C85 C88 H88A 109.5 . . ? C85 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C85 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? O3 Cl1 O1 108.3(12) . . ? O3 Cl1 O4 107.5(14) . . ? O1 Cl1 O4 109.3(10) . . ? O3 Cl1 O2 115.7(16) . . ? O1 Cl1 O2 106.5(9) . . ? O4 Cl1 O2 109.4(11) . . ? O8 Cl2 O5 109.1(7) . . ? O8 Cl2 O7 111.5(7) . . ? O5 Cl2 O7 111.3(5) . . ? O8 Cl2 O6 109.3(7) . . ? O5 Cl2 O6 110.3(6) . . ? O7 Cl2 O6 105.3(5) . . ? O12 Cl3 O10 114.0(15) . . ? O12 Cl3 O9 114.2(12) . . ? O10 Cl3 O9 113.6(10) . . ? O12 Cl3 O11 102(2) . . ? O10 Cl3 O11 101.8(14) . . ? O9 Cl3 O11 109.4(18) . . ? Cl3 O11 O11 98.6(18) . 2_665 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.75 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.482 _refine_diff_density_min -1.160 _refine_diff_density_rms 0.207 # start Validation Reply Form _vrf_PUBL366_GLOBAL ; PROBLEM: Short? C(sp?)-C(sp?) Bond C39 - C40 ... 1.12 Ang RESPONSE: All of these are due to triple bonds between two Csp carbon atoms. ; _vrf_PUBL220_GLOBAL ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.68 Ratio RESPONSE: Large difference is due to the slight disorder of these carbon atoms. No disorder model was used in the final refinement. ; _vrf_PUBL242_GLOBAL ; PROBLEM: Check Low Ueq as Compared to Neighbors for C55 RESPONSE: This is also due to the sligth disorder of the butyl group. No disorder model was used in the final refinement. ;