# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © 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_name 'Jagadese Vittal' _publ_contact_author_email chmjjv@nus.edu.sg loop_ _publ_author_name 'Jagadese Vittal' 'Mohammad Mir' 'Jun Ong' 'Goutam Kole' 'Geok Tan' 'Michael McGlinchey' 'Yuyang Wu' data_a164 _database_code_depnum_ccdc_archive 'CCDC 836596' #TrackingRef '- Xtl1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H60 Au4 O10 P4' _chemical_formula_weight 1900.87 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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.2747(10) _cell_length_b 17.2947(14) _cell_length_c 16.2187(14) _cell_angle_alpha 90.00 _cell_angle_beta 103.224(2) _cell_angle_gamma 90.00 _cell_volume 3078.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3506 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 26.59 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 2.051 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 9.663 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2250 _exptl_absorpt_correction_T_max 0.4450 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21320 _diffrn_reflns_av_R_equivalents 0.0598 _diffrn_reflns_av_sigmaI/netI 0.0654 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7054 _reflns_number_gt 5412 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0421P)^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 7054 _refine_ls_number_parameters 372 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0623 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.0950 _refine_ls_wR_factor_gt 0.0885 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _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 0.27211(3) 0.412944(16) 0.657518(16) 0.03172(9) Uani 1 1 d . . . Au2 Au 0.28967(2) 0.273684(16) 0.766899(15) 0.03022(9) Uani 1 1 d . . . P1 P 0.28926(16) 0.34577(11) 0.54395(10) 0.0293(4) Uani 1 1 d . . . P2 P 0.22287(17) 0.21141(11) 0.64579(11) 0.0295(4) Uani 1 1 d . . . O1 O 0.2699(5) 0.4799(3) 0.7618(3) 0.0422(13) Uani 1 1 d . . . O2 O 0.1118(5) 0.4164(3) 0.7934(4) 0.0528(16) Uani 1 1 d . . . O3 O 0.6386(5) 0.6762(3) 1.1173(3) 0.0372(12) Uani 1 1 d . . . O4 O 0.4530(5) 0.6773(3) 1.1459(3) 0.0499(15) Uani 1 1 d . . . C1 C 0.1969(6) 0.4625(5) 0.8104(4) 0.0359(18) Uani 1 1 d . . . C2 C 0.2272(7) 0.5052(5) 0.8926(5) 0.0405(19) Uani 1 1 d . . . H2 H 0.1707 0.5049 0.9271 0.049 Uiso 1 1 calc R . . C3 C 0.3308(7) 0.5433(4) 0.9185(4) 0.0358(17) Uani 1 1 d . . . H3 H 0.3844 0.5429 0.8819 0.043 Uiso 1 1 calc R . . C4 C 0.3704(7) 0.5854(4) 0.9963(4) 0.0371(17) Uani 1 1 d . . . H4 H 0.3165 0.5904 1.0325 0.045 Uiso 1 1 calc R . . C5 C 0.4807(7) 0.6178(4) 1.0196(4) 0.0373(18) Uani 1 1 d . . . H5 H 0.5338 0.6133 0.9828 0.045 Uiso 1 1 calc R . . C6 C 0.5237(7) 0.6602(4) 1.1001(4) 0.0352(17) Uani 1 1 d . . . C7 C 0.3093(6) 0.2423(4) 0.5685(4) 0.0302(15) Uani 1 1 d . . . H7A H 0.2824 0.2123 0.5162 0.036 Uiso 1 1 calc R . . H7B H 0.3960 0.2315 0.5911 0.036 Uiso 1 1 calc R . . C1W C 0.0665(6) 0.2245(4) 0.5936(4) 0.0324(16) Uani 1 1 d . . . C2W C 0.0106(7) 0.1800(5) 0.5220(5) 0.0432(19) Uani 1 1 d . . . H2W H 0.0554 0.1400 0.5041 0.052 Uiso 1 1 calc R . . C3W C -0.1069(8) 0.1932(6) 0.4778(6) 0.056(2) Uani 1 1 d . . . H3W H -0.1419 0.1637 0.4297 0.067 Uiso 1 1 calc R . . C4W C -0.1725(8) 0.2515(6) 0.5062(6) 0.064(3) Uani 1 1 d . . . H4W H -0.2535 0.2610 0.4775 0.076 Uiso 1 1 calc R . . C5W C -0.1210(8) 0.2953(6) 0.5754(7) 0.061(3) Uani 1 1 d . . . H5W H -0.1671 0.3345 0.5934 0.073 Uiso 1 1 calc R . . C6W C -0.0023(8) 0.2829(5) 0.6192(5) 0.049(2) Uani 1 1 d . . . H6W H 0.0320 0.3139 0.6663 0.058 Uiso 1 1 calc R . . C1X C 0.1598(6) 0.3570(4) 0.4554(4) 0.0334(17) Uani 1 1 d . . . C2X C 0.1175(7) 0.3002(5) 0.3975(5) 0.0396(18) Uani 1 1 d . . . H2X H 0.1559 0.2517 0.4038 0.047 Uiso 1 1 calc R . . C3X C 0.0187(7) 0.3127(6) 0.3294(5) 0.049(2) Uani 1 1 d . . . H3X H -0.0110 0.2727 0.2910 0.058 Uiso 1 1 calc R . . C4X C -0.0345(7) 0.3847(6) 0.3196(5) 0.051(2) Uani 1 1 d . . . H4X H -0.1000 0.3942 0.2732 0.061 Uiso 1 1 calc R . . C5X C 0.0076(8) 0.4438(5) 0.3775(5) 0.055(2) Uani 1 1 d . . . H5X H -0.0297 0.4927 0.3703 0.066 Uiso 1 1 calc R . . C6X C 0.1049(7) 0.4301(5) 0.4456(5) 0.045(2) Uani 1 1 d . . . H6X H 0.1338 0.4696 0.4849 0.054 Uiso 1 1 calc R . . C1Y C 0.2474(7) 0.1084(4) 0.6621(4) 0.0337(17) Uani 1 1 d . . . C2Y C 0.1535(8) 0.0604(5) 0.6729(5) 0.047(2) Uani 1 1 d . . . H2Y H 0.0740 0.0801 0.6645 0.056 Uiso 1 1 calc R . . C3Y C 0.1760(8) -0.0163(5) 0.6958(5) 0.051(2) Uani 1 1 d . . . H3Y H 0.1119 -0.0488 0.7021 0.061 Uiso 1 1 calc R . . C4Y C 0.2938(9) -0.0446(5) 0.7092(5) 0.051(2) Uani 1 1 d . . . H4Y H 0.3095 -0.0964 0.7257 0.061 Uiso 1 1 calc R . . C5Y C 0.3874(7) 0.0019(5) 0.6989(5) 0.0429(19) Uani 1 1 d . . . H5Y H 0.4668 -0.0181 0.7074 0.051 Uiso 1 1 calc R . . C6Y C 0.3646(7) 0.0789(4) 0.6756(4) 0.0360(17) Uani 1 1 d . . . H6Y H 0.4290 0.1111 0.6690 0.043 Uiso 1 1 calc R . . C1Z C 0.4223(6) 0.3736(4) 0.5055(4) 0.0292(15) Uani 1 1 d . . . C2Z C 0.4285(7) 0.3669(4) 0.4222(5) 0.0398(18) Uani 1 1 d . . . H2Z H 0.3611 0.3481 0.3819 0.048 Uiso 1 1 calc R . . C3Z C 0.5328(7) 0.3877(5) 0.3977(5) 0.045(2) Uani 1 1 d . . . H3Z H 0.5364 0.3823 0.3406 0.054 Uiso 1 1 calc R . . C4Z C 0.6314(7) 0.4161(5) 0.4549(5) 0.046(2) Uani 1 1 d . . . H4Z H 0.7023 0.4297 0.4370 0.055 Uiso 1 1 calc R . . C5Z C 0.6273(7) 0.4248(4) 0.5392(5) 0.044(2) Uani 1 1 d . . . H5Z H 0.6944 0.4451 0.5786 0.053 Uiso 1 1 calc R . . C6Z C 0.5231(7) 0.4033(4) 0.5642(5) 0.0400(18) Uani 1 1 d . . . H6Z H 0.5196 0.4085 0.6213 0.048 Uiso 1 1 calc R . . O1S O 0.5603(5) 0.2398(4) 0.7127(4) 0.0593(17) Uani 1 1 d . . . H1S H 0.5500 0.2704 0.7499 0.089 Uiso 1 1 calc R . . C1S C 0.6813(8) 0.2213(6) 0.7262(7) 0.078(3) Uani 1 1 d . . . H1S1 H 0.7295 0.2683 0.7344 0.117 Uiso 1 1 calc R . . H1S2 H 0.6958 0.1935 0.6775 0.117 Uiso 1 1 calc R . . H1S3 H 0.7043 0.1891 0.7763 0.117 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 0.03652(17) 0.03319(18) 0.02428(14) -0.00341(11) 0.00448(11) 0.00398(12) Au2 0.03301(16) 0.03344(18) 0.02346(13) -0.00199(11) 0.00495(11) -0.00057(12) P1 0.0303(10) 0.0333(11) 0.0235(8) -0.0023(7) 0.0045(7) 0.0013(8) P2 0.0284(10) 0.0328(11) 0.0257(9) -0.0021(7) 0.0030(7) 0.0008(8) O1 0.049(3) 0.045(3) 0.032(3) -0.005(2) 0.010(2) 0.003(3) O2 0.027(3) 0.067(4) 0.062(4) -0.024(3) 0.004(3) -0.007(3) O3 0.039(3) 0.048(3) 0.023(2) -0.003(2) 0.003(2) 0.000(2) O4 0.045(3) 0.062(4) 0.046(3) -0.020(3) 0.019(3) -0.013(3) C1 0.026(4) 0.042(5) 0.034(4) -0.011(3) -0.004(3) 0.014(3) C2 0.032(4) 0.049(5) 0.038(4) -0.009(4) 0.003(3) 0.006(4) C3 0.043(4) 0.035(5) 0.025(3) 0.000(3) -0.001(3) 0.006(4) C4 0.039(4) 0.039(5) 0.031(4) -0.005(3) 0.005(3) 0.002(4) C5 0.045(5) 0.037(5) 0.031(4) -0.008(3) 0.011(3) -0.003(4) C6 0.041(5) 0.035(4) 0.029(4) 0.000(3) 0.005(3) 0.001(3) C7 0.026(4) 0.030(4) 0.031(4) 0.000(3) 0.000(3) 0.001(3) C1W 0.027(4) 0.035(4) 0.031(4) -0.001(3) 0.001(3) -0.003(3) C2W 0.040(5) 0.050(5) 0.039(4) -0.004(4) 0.005(3) -0.011(4) C3W 0.036(5) 0.067(7) 0.056(5) 0.006(5) -0.008(4) -0.012(5) C4W 0.029(5) 0.074(7) 0.080(7) 0.025(6) -0.002(5) -0.001(5) C5W 0.036(5) 0.060(6) 0.079(7) 0.010(5) -0.003(5) 0.017(4) C6W 0.043(5) 0.046(5) 0.054(5) 0.012(4) 0.003(4) 0.006(4) C1X 0.028(4) 0.046(5) 0.026(3) 0.006(3) 0.006(3) 0.002(3) C2X 0.035(4) 0.047(5) 0.038(4) 0.001(4) 0.012(3) 0.006(4) C3X 0.037(5) 0.071(7) 0.035(4) -0.002(4) 0.003(3) -0.005(4) C4X 0.032(4) 0.073(7) 0.042(5) 0.017(4) -0.005(3) -0.001(4) C5X 0.050(6) 0.050(6) 0.059(6) 0.014(5) -0.001(4) 0.011(4) C6X 0.044(5) 0.045(5) 0.041(4) 0.008(4) 0.002(4) 0.009(4) C1Y 0.034(4) 0.037(4) 0.029(4) -0.001(3) 0.005(3) -0.002(3) C2Y 0.043(5) 0.039(5) 0.061(5) -0.001(4) 0.014(4) 0.000(4) C3Y 0.058(6) 0.034(5) 0.061(5) -0.007(4) 0.018(4) -0.007(4) C4Y 0.078(7) 0.036(5) 0.042(5) 0.007(4) 0.022(4) 0.004(5) C5Y 0.044(5) 0.047(5) 0.035(4) 0.003(4) 0.004(3) 0.011(4) C6Y 0.036(4) 0.035(5) 0.036(4) 0.008(3) 0.005(3) 0.005(3) C1Z 0.026(4) 0.032(4) 0.030(3) -0.002(3) 0.005(3) 0.001(3) C2Z 0.045(5) 0.036(5) 0.037(4) -0.007(3) 0.006(3) 0.000(4) C3Z 0.051(5) 0.051(5) 0.039(4) 0.005(4) 0.025(4) 0.000(4) C4Z 0.033(4) 0.047(5) 0.060(5) 0.009(4) 0.017(4) -0.004(4) C5Z 0.029(4) 0.041(5) 0.060(5) -0.003(4) 0.003(4) -0.005(3) C6Z 0.041(5) 0.042(5) 0.036(4) -0.001(3) 0.006(3) 0.006(4) O1S 0.044(4) 0.085(5) 0.047(4) -0.022(3) 0.007(3) 0.004(3) C1S 0.041(6) 0.096(9) 0.102(9) -0.033(7) 0.029(6) 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 O1 2.055(5) . ? Au1 P1 2.2233(17) . ? Au1 Au2 2.9709(4) . ? Au2 O3 2.059(5) 3_667 ? Au2 P2 2.2155(18) . ? P1 C1X 1.809(7) . ? P1 C1Z 1.817(7) . ? P1 C7 1.836(7) . ? P2 C1W 1.787(7) . ? P2 C1Y 1.813(8) . ? P2 C7 1.835(7) . ? O1 C1 1.298(9) . ? O2 C1 1.230(9) . ? O3 C6 1.291(9) . ? O3 Au2 2.059(5) 3_667 ? O4 C6 1.243(9) . ? C1 C2 1.493(9) . ? C2 C3 1.323(10) . ? C3 C4 1.437(9) . ? C4 C5 1.337(10) . ? C5 C6 1.480(9) . ? C1W C6W 1.394(11) . ? C1W C2W 1.416(10) . ? C2W C3W 1.373(11) . ? C3W C4W 1.391(13) . ? C4W C5W 1.368(13) . ? C5W C6W 1.380(11) . ? C1X C2X 1.367(10) . ? C1X C6X 1.400(10) . ? C2X C3X 1.394(10) . ? C3X C4X 1.375(12) . ? C4X C5X 1.396(12) . ? C5X C6X 1.388(11) . ? C1Y C6Y 1.386(10) . ? C1Y C2Y 1.387(11) . ? C2Y C3Y 1.385(11) . ? C3Y C4Y 1.385(12) . ? C4Y C5Y 1.367(11) . ? C5Y C6Y 1.393(10) . ? C1Z C2Z 1.372(9) . ? C1Z C6Z 1.402(10) . ? C2Z C3Z 1.373(10) . ? C3Z C4Z 1.365(11) . ? C4Z C5Z 1.388(11) . ? C5Z C6Z 1.379(11) . ? O1S C1S 1.368(10) . ? 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 O1 Au1 P1 175.02(16) . . ? O1 Au1 Au2 88.69(15) . . ? P1 Au1 Au2 93.70(5) . . ? O3 Au2 P2 175.20(15) 3_667 . ? O3 Au2 Au1 99.30(14) 3_667 . ? P2 Au2 Au1 84.38(5) . . ? C1X P1 C1Z 106.2(3) . . ? C1X P1 C7 108.3(3) . . ? C1Z P1 C7 105.2(3) . . ? C1X P1 Au1 113.2(2) . . ? C1Z P1 Au1 112.4(2) . . ? C7 P1 Au1 111.1(2) . . ? C1W P2 C1Y 107.2(3) . . ? C1W P2 C7 105.1(3) . . ? C1Y P2 C7 107.4(3) . . ? C1W P2 Au2 117.2(2) . . ? C1Y P2 Au2 109.8(2) . . ? C7 P2 Au2 109.8(2) . . ? C1 O1 Au1 119.8(5) . . ? C6 O3 Au2 116.9(4) . 3_667 ? O2 C1 O1 125.8(7) . . ? O2 C1 C2 121.9(7) . . ? O1 C1 C2 112.3(7) . . ? C3 C2 C1 122.4(7) . . ? C2 C3 C4 127.3(7) . . ? C5 C4 C3 122.8(7) . . ? C4 C5 C6 123.5(7) . . ? O4 C6 O3 124.7(7) . . ? O4 C6 C5 121.3(7) . . ? O3 C6 C5 114.0(6) . . ? P2 C7 P1 111.9(4) . . ? C6W C1W C2W 117.7(7) . . ? C6W C1W P2 120.5(6) . . ? C2W C1W P2 121.7(6) . . ? C3W C2W C1W 122.2(8) . . ? C2W C3W C4W 118.0(8) . . ? C5W C4W C3W 121.1(8) . . ? C4W C5W C6W 121.0(9) . . ? C5W C6W C1W 119.9(9) . . ? C2X C1X C6X 119.7(7) . . ? C2X C1X P1 124.0(6) . . ? C6X C1X P1 116.3(6) . . ? C1X C2X C3X 121.5(8) . . ? C4X C3X C2X 118.7(8) . . ? C3X C4X C5X 120.8(8) . . ? C6X C5X C4X 119.7(8) . . ? C5X C6X C1X 119.5(8) . . ? C6Y C1Y C2Y 119.1(7) . . ? C6Y C1Y P2 119.5(6) . . ? C2Y C1Y P2 120.7(6) . . ? C3Y C2Y C1Y 120.6(8) . . ? C2Y C3Y C4Y 119.4(8) . . ? C5Y C4Y C3Y 120.8(8) . . ? C4Y C5Y C6Y 119.8(8) . . ? C1Y C6Y C5Y 120.3(7) . . ? C2Z C1Z C6Z 118.9(7) . . ? C2Z C1Z P1 123.2(5) . . ? C6Z C1Z P1 117.9(5) . . ? C1Z C2Z C3Z 120.2(7) . . ? C4Z C3Z C2Z 121.0(7) . . ? C3Z C4Z C5Z 120.2(7) . . ? C6Z C5Z C4Z 118.9(7) . . ? C5Z C6Z C1Z 120.8(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.140 _refine_diff_density_min -0.850 _refine_diff_density_rms 0.189 # Attachment '- Xtl2.cif' data_9632 _database_code_depnum_ccdc_archive 'CCDC 836597' #TrackingRef '- Xtl2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C67 H64 Au4 Cl4 O9 P4' _chemical_formula_weight 2066.73 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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.1309(8) _cell_length_b 14.7191(8) _cell_length_c 18.2436(11) _cell_angle_alpha 80.6850(10) _cell_angle_beta 81.1810(10) _cell_angle_gamma 87.4960(10) _cell_volume 3437.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 7422 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 27.47 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.997 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1964 _exptl_absorpt_coefficient_mu 8.811 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.0835 _exptl_absorpt_correction_T_max 0.6199 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24202 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0832 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 27.50 _reflns_number_total 15638 _reflns_number_gt 12074 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0857P)^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 15638 _refine_ls_number_parameters 814 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1508 _refine_ls_wR_factor_gt 0.1412 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.981 _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 0.82441(2) 0.20663(2) 0.765444(18) 0.03925(10) Uani 1 1 d . . . Au2 Au 0.76685(2) 0.32987(2) 0.884417(19) 0.04093(10) Uani 1 1 d . . . Au3 Au 0.76280(3) 0.70570(2) 0.659311(17) 0.03665(10) Uani 1 1 d . . . Au4 Au 0.52388(3) 0.797678(19) 0.659448(16) 0.03424(9) Uani 1 1 d . . . P1 P 0.82059(16) 0.32351(13) 0.67295(11) 0.0338(5) Uani 1 1 d . . . P2 P 0.64856(16) 0.41388(13) 0.82788(11) 0.0310(4) Uani 1 1 d . . . P3 P 0.80799(17) 0.76515(14) 0.75324(11) 0.0331(4) Uani 1 1 d . . . P4 P 0.54408(16) 0.91074(13) 0.72274(11) 0.0295(4) Uani 1 1 d . . . O1 O 0.8489(5) 0.0923(4) 0.8413(4) 0.0554(18) Uani 1 1 d . . . O2 O 0.6801(4) 0.0694(4) 0.8723(3) 0.0410(14) Uani 1 1 d . . . O3 O 0.8533(5) 0.2501(5) 0.9547(4) 0.0580(19) Uani 1 1 d . . . O4 O 1.0105(5) 0.2839(4) 0.8951(4) 0.0506(16) Uani 1 1 d . . . O5 O 0.7296(5) 0.6364(4) 0.5763(3) 0.0425(14) Uani 1 1 d . . . O6 O 0.7824(7) 0.7560(5) 0.4891(4) 0.070(2) Uani 1 1 d . . . O7 O 0.4914(5) 0.7070(4) 0.5920(3) 0.0426(14) Uani 1 1 d . . . O8 O 0.4500(7) 0.5968(5) 0.6890(4) 0.068(2) Uani 1 1 d . . . C1 C 0.7021(7) 0.3944(6) 0.6730(5) 0.042(2) Uani 1 1 d . . . H1A H 0.7022 0.4293 0.6225 0.050 Uiso 1 1 calc R . . H1B H 0.6433 0.3531 0.6833 0.050 Uiso 1 1 calc R . . C2 C 0.6850(6) 0.4629(5) 0.7297(4) 0.0337(17) Uani 1 1 d . . . H2A H 0.6312 0.5075 0.7152 0.040 Uiso 1 1 calc R . . H2B H 0.7486 0.4970 0.7252 0.040 Uiso 1 1 calc R . . C3 C 0.7692(7) 0.0489(5) 0.8801(4) 0.0329(17) Uani 1 1 d . . . C4 C 0.7946(6) -0.0303(5) 0.9364(4) 0.0302(16) Uani 1 1 d . . . H4 H 0.7396 -0.0618 0.9679 0.036 Uiso 1 1 calc R . . C5 C 0.8899(6) -0.0596(5) 0.9452(4) 0.0326(17) Uani 1 1 d . . . H5 H 0.9443 -0.0269 0.9139 0.039 Uiso 1 1 calc R . . C6 C 0.9497(7) 0.2394(6) 0.9434(5) 0.0401(19) Uani 1 1 d . . . C7 C 0.9857(7) 0.1615(5) 0.9972(5) 0.044(2) Uani 1 1 d . . . H7 H 0.9345 0.1272 1.0306 0.053 Uiso 1 1 calc R . . C8 C 1.0826(6) 0.1361(5) 1.0025(4) 0.0322(16) Uani 1 1 d . . . H8 H 1.1354 0.1699 0.9703 0.039 Uiso 1 1 calc R . . C9 C 0.7096(6) 0.8376(5) 0.7983(4) 0.0363(18) Uani 1 1 d . . . H9A H 0.6496 0.7999 0.8206 0.044 Uiso 1 1 calc R . . H9B H 0.7366 0.8600 0.8391 0.044 Uiso 1 1 calc R . . C10 C 0.6738(6) 0.9213(5) 0.7447(4) 0.0329(17) Uani 1 1 d . . . H10A H 0.7224 0.9292 0.6978 0.039 Uiso 1 1 calc R . . H10B H 0.6759 0.9768 0.7677 0.039 Uiso 1 1 calc R . . C11 C 0.7480(7) 0.6782(6) 0.5083(4) 0.0380(18) Uani 1 1 d . . . C12 C 0.7213(7) 0.6265(5) 0.4510(5) 0.0395(19) Uani 1 1 d . . . H12 H 0.7448 0.6486 0.4002 0.047 Uiso 1 1 calc R . . C13 C 0.6657(6) 0.5504(5) 0.4675(4) 0.0345(17) Uani 1 1 d . . . H13 H 0.6468 0.5266 0.5185 0.041 Uiso 1 1 calc R . . C14 C 0.4572(7) 0.6284(5) 0.6219(5) 0.0367(18) Uani 1 1 d . . . C15 C 0.4229(6) 0.5748(5) 0.5675(4) 0.0355(18) Uani 1 1 d . . . H15 H 0.4417 0.5964 0.5160 0.043 Uiso 1 1 calc R . . C16 C 0.3675(7) 0.4984(6) 0.5867(5) 0.0395(19) Uani 1 1 d . . . H16 H 0.3494 0.4753 0.6380 0.047 Uiso 1 1 calc R . . C1Q C 0.4596(6) 0.8991(5) 0.8127(4) 0.0302(16) Uani 1 1 d . . . C6Q C 0.4868(7) 0.9296(5) 0.8743(4) 0.0365(18) Uani 1 1 d . . . H6Q H 0.5495 0.9598 0.8702 0.044 Uiso 1 1 calc R . . C5Q C 0.4213(7) 0.9157(6) 0.9426(5) 0.044(2) Uani 1 1 d . . . H5Q H 0.4398 0.9359 0.9850 0.053 Uiso 1 1 calc R . . C4Q C 0.3294(7) 0.8722(5) 0.9476(5) 0.043(2) Uani 1 1 d . . . H4Q H 0.2851 0.8631 0.9936 0.052 Uiso 1 1 calc R . . C3Q C 0.3020(7) 0.8424(6) 0.8874(5) 0.046(2) Uani 1 1 d . . . H3Q H 0.2390 0.8125 0.8921 0.055 Uiso 1 1 calc R . . C2Q C 0.3662(7) 0.8555(5) 0.8182(5) 0.0406(19) Uani 1 1 d . . . H2Q H 0.3468 0.8352 0.7762 0.049 Uiso 1 1 calc R . . C1T C 0.5157(6) 1.0238(5) 0.6728(4) 0.0343(17) Uani 1 1 d . . . C2T C 0.5161(11) 1.1009(7) 0.7074(6) 0.070(3) Uani 1 1 d . . . H2T H 0.5307 1.0946 0.7569 0.084 Uiso 1 1 calc R . . C3T C 0.4955(11) 1.1855(6) 0.6700(6) 0.073(4) Uani 1 1 d . . . H3T H 0.4966 1.2375 0.6938 0.087 Uiso 1 1 calc R . . C4T C 0.4731(9) 1.1964(6) 0.5982(6) 0.062(3) Uani 1 1 d . . . H4T H 0.4598 1.2553 0.5724 0.075 Uiso 1 1 calc R . . C5T C 0.4706(12) 1.1224(8) 0.5658(7) 0.087(4) Uani 1 1 d . . . H5T H 0.4544 1.1300 0.5167 0.105 Uiso 1 1 calc R . . C6T C 0.4910(10) 1.0336(7) 0.6014(6) 0.068(3) Uani 1 1 d . . . H6T H 0.4879 0.9823 0.5772 0.081 Uiso 1 1 calc R . . C1U C 0.8411(7) 0.6777(6) 0.8279(5) 0.041(2) Uani 1 1 d . . . C2U C 0.8329(8) 0.6931(7) 0.9025(5) 0.052(2) Uani 1 1 d . . . H2U H 0.8059 0.7496 0.9154 0.063 Uiso 1 1 calc R . . C3U C 0.8637(9) 0.6272(8) 0.9561(6) 0.062(3) Uani 1 1 d . . . H3U H 0.8568 0.6378 1.0060 0.074 Uiso 1 1 calc R . . C4U C 0.9047(8) 0.5449(7) 0.9378(6) 0.058(3) Uani 1 1 d . . . H4U H 0.9252 0.4995 0.9754 0.070 Uiso 1 1 calc R . . C5U C 0.9157(8) 0.5289(7) 0.8656(7) 0.058(3) Uani 1 1 d . . . H5U H 0.9451 0.4728 0.8536 0.070 Uiso 1 1 calc R . . C6U C 0.8843(7) 0.5944(6) 0.8094(6) 0.048(2) Uani 1 1 d . . . H6U H 0.8918 0.5829 0.7597 0.057 Uiso 1 1 calc R . . C1V C 0.9186(7) 0.8386(6) 0.7256(5) 0.046(2) Uani 1 1 d . . . C2V C 0.9939(10) 0.8392(9) 0.7663(7) 0.076(3) Uani 1 1 d . . . H2V H 0.9924 0.7971 0.8111 0.091 Uiso 1 1 calc R . . C3V C 1.0749(12) 0.9001(12) 0.7449(10) 0.105(5) Uani 1 1 d . . . H3V H 1.1294 0.8964 0.7733 0.126 Uiso 1 1 calc R . . C4V C 1.0751(13) 0.9650(11) 0.6828(10) 0.108(7) Uani 1 1 d . . . H4V H 1.1286 1.0077 0.6699 0.130 Uiso 1 1 calc R . . C5V C 1.0006(12) 0.9693(8) 0.6395(9) 0.089(5) Uani 1 1 d . . . H5V H 1.0023 1.0141 0.5963 0.107 Uiso 1 1 calc R . . C6V C 0.9188(9) 0.9052(7) 0.6599(7) 0.064(3) Uani 1 1 d . . . H6V H 0.8658 0.9071 0.6303 0.076 Uiso 1 1 calc R . . C1W C 0.5335(6) 0.3492(5) 0.8316(4) 0.0333(17) Uani 1 1 d . . . C2W C 0.4470(8) 0.3906(6) 0.8025(5) 0.050(2) Uani 1 1 d . . . H2W H 0.4501 0.4518 0.7777 0.059 Uiso 1 1 calc R . . C3W C 0.3572(9) 0.3422(8) 0.8097(7) 0.065(3) Uani 1 1 d . . . H3W H 0.2994 0.3712 0.7906 0.078 Uiso 1 1 calc R . . C4W C 0.3516(10) 0.2522(8) 0.8445(6) 0.069(3) Uani 1 1 d . . . H4W H 0.2908 0.2191 0.8483 0.083 Uiso 1 1 calc R . . C5W C 0.4360(10) 0.2109(7) 0.8737(6) 0.060(3) Uani 1 1 d . . . H5W H 0.4317 0.1500 0.8991 0.072 Uiso 1 1 calc R . . C6W C 0.5266(8) 0.2575(5) 0.8663(5) 0.050(2) Uani 1 1 d . . . H6W H 0.5842 0.2274 0.8848 0.060 Uiso 1 1 calc R . . C1X C 0.6093(6) 0.5118(5) 0.8747(4) 0.0313(16) Uani 1 1 d . . . C2X C 0.5505(7) 0.5848(5) 0.8424(5) 0.041(2) Uani 1 1 d . . . H2X H 0.5332 0.5858 0.7941 0.049 Uiso 1 1 calc R . . C3X C 0.5180(8) 0.6566(6) 0.8834(6) 0.049(2) Uani 1 1 d . . . H3X H 0.4795 0.7063 0.8616 0.059 Uiso 1 1 calc R . . C4X C 0.5406(8) 0.6558(6) 0.9529(5) 0.051(2) Uani 1 1 d . . . H4X H 0.5167 0.7037 0.9799 0.061 Uiso 1 1 calc R . . C5X C 0.5992(8) 0.5841(7) 0.9841(5) 0.053(2) Uani 1 1 d . . . H5X H 0.6157 0.5840 1.0325 0.064 Uiso 1 1 calc R . . C6X C 0.6338(7) 0.5130(6) 0.9461(5) 0.0395(19) Uani 1 1 d . . . H6X H 0.6741 0.4650 0.9683 0.047 Uiso 1 1 calc R . . C1Y C 0.9221(7) 0.4042(5) 0.6647(4) 0.0381(19) Uani 1 1 d . . . C2Y C 0.9325(8) 0.4790(6) 0.6071(5) 0.050(2) Uani 1 1 d . . . H2Y H 0.8848 0.4887 0.5730 0.060 Uiso 1 1 calc R . . C3Y C 1.0123(10) 0.5391(7) 0.5998(6) 0.070(3) Uani 1 1 d . . . H3Y H 1.0190 0.5888 0.5601 0.083 Uiso 1 1 calc R . . C4Y C 1.0808(9) 0.5277(8) 0.6485(8) 0.074(4) Uani 1 1 d . . . H4Y H 1.1344 0.5697 0.6430 0.089 Uiso 1 1 calc R . . C5Y C 1.0723(8) 0.4540(7) 0.7069(7) 0.064(3) Uani 1 1 d . . . H5Y H 1.1204 0.4454 0.7407 0.077 Uiso 1 1 calc R . . C6Y C 0.9923(7) 0.3929(6) 0.7148(5) 0.046(2) Uani 1 1 d . . . H6Y H 0.9858 0.3434 0.7547 0.055 Uiso 1 1 calc R . . C1Z C 0.8367(7) 0.2820(5) 0.5826(4) 0.0392(19) Uani 1 1 d . . . C2Z C 0.9382(7) 0.2507(6) 0.5574(5) 0.043(2) Uani 1 1 d . . . H2Z H 0.9918 0.2517 0.5860 0.052 Uiso 1 1 calc R . . C3Z C 0.9552(8) 0.2184(6) 0.4889(5) 0.052(2) Uani 1 1 d . . . H3Z H 1.0215 0.1971 0.4711 0.062 Uiso 1 1 calc R . . C4Z C 0.8756(10) 0.2170(7) 0.4456(6) 0.065(3) Uani 1 1 d . . . H4Z H 0.8887 0.1964 0.3989 0.078 Uiso 1 1 calc R . . C5Z C 0.7782(9) 0.2463(7) 0.4728(6) 0.057(3) Uani 1 1 d . . . H5Z H 0.7235 0.2439 0.4455 0.068 Uiso 1 1 calc R . . C6Z C 0.7610(9) 0.2800(7) 0.5416(6) 0.056(3) Uani 1 1 d . . . H6Z H 0.6947 0.3016 0.5592 0.067 Uiso 1 1 calc R . . C1S C 0.1065(9) 0.1352(7) 0.7918(6) 0.065(3) Uani 1 1 d . . . H1S1 H 0.0892 0.1839 0.8228 0.078 Uiso 1 1 calc R . . H1S2 H 0.0426 0.1047 0.7892 0.078 Uiso 1 1 calc R . . Cl1 Cl 0.1622(3) 0.1849(2) 0.70000(19) 0.0858(10) Uani 1 1 d . . . Cl2 Cl 0.1916(3) 0.05443(18) 0.83407(18) 0.0717(8) Uani 1 1 d . . . C3S C 0.7542(14) 0.9931(9) 0.5022(8) 0.117(6) Uani 1 1 d D . . H3S1 H 0.7428 1.0465 0.5275 0.175 Uiso 1 1 calc R . . H3S2 H 0.7122 0.9989 0.4623 0.175 Uiso 1 1 calc R . . H3S3 H 0.8264 0.9889 0.4811 0.175 Uiso 1 1 calc R . . O1S O 0.7269(8) 0.9125(5) 0.5545(5) 0.086(3) Uani 1 1 d D . . H1S H 0.7647 0.8688 0.5428 0.129 Uiso 1 1 calc R . . Cl4 Cl 0.7999(6) 0.3128(5) 0.2474(5) 0.198(3) Uani 1 1 d DU . . C2S C 0.7237(16) 0.3817(19) 0.1901(10) 0.087(10) Uani 0.48(3) 1 d PD A 1 H2SA H 0.7114 0.4422 0.2060 0.104 Uiso 0.48(3) 1 calc PR A 1 H2SB H 0.6570 0.3530 0.1925 0.104 Uiso 0.48(3) 1 calc PR A 1 Cl3 Cl 0.7907(18) 0.393(2) 0.0994(8) 0.213(10) Uani 0.48(3) 1 d PDU A 1 C2SA C 0.745(3) 0.4211(16) 0.2215(12) 0.130(11) Uani 0.52(3) 1 d PDU A 2 H2SC H 0.6692 0.4174 0.2300 0.156 Uiso 0.52(3) 1 calc PR A 2 H2SD H 0.7645 0.4650 0.2516 0.156 Uiso 0.52(3) 1 calc PR A 2 Cl3A Cl 0.7885(12) 0.4569(16) 0.1269(9) 0.180(8) Uani 0.52(3) 1 d PDU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.03645(19) 0.03169(17) 0.04146(19) 0.01144(13) 0.00023(13) 0.00462(13) Au2 0.03348(18) 0.03971(18) 0.04223(19) 0.00944(14) -0.00247(13) 0.01100(14) Au3 0.0491(2) 0.02790(16) 0.03552(17) -0.00978(12) -0.00820(14) -0.00497(13) Au4 0.0469(2) 0.02519(15) 0.03178(16) -0.00695(11) -0.00564(13) -0.00473(13) P1 0.0359(11) 0.0275(9) 0.0327(10) 0.0028(8) 0.0019(8) 0.0047(8) P2 0.0317(11) 0.0260(9) 0.0321(10) 0.0017(7) -0.0026(8) 0.0050(8) P3 0.0358(11) 0.0299(10) 0.0359(11) -0.0118(8) -0.0049(8) -0.0041(8) P4 0.0374(11) 0.0225(9) 0.0292(10) -0.0065(7) -0.0035(8) -0.0020(8) O1 0.040(4) 0.044(4) 0.068(4) 0.030(3) -0.006(3) 0.006(3) O2 0.034(3) 0.035(3) 0.053(4) 0.003(3) -0.015(3) 0.002(3) O3 0.035(3) 0.066(4) 0.057(4) 0.030(3) -0.004(3) 0.016(3) O4 0.047(4) 0.040(3) 0.054(4) 0.015(3) 0.002(3) 0.003(3) O5 0.063(4) 0.035(3) 0.034(3) -0.014(2) -0.016(3) -0.004(3) O6 0.106(6) 0.049(4) 0.055(4) -0.012(3) -0.001(4) -0.040(4) O7 0.065(4) 0.033(3) 0.034(3) -0.012(2) -0.010(3) -0.013(3) O8 0.119(7) 0.051(4) 0.042(4) 0.000(3) -0.035(4) -0.028(4) C1 0.047(5) 0.038(4) 0.037(4) 0.001(3) -0.006(4) 0.009(4) C2 0.036(4) 0.031(4) 0.030(4) 0.003(3) -0.003(3) 0.008(3) C3 0.045(5) 0.019(3) 0.036(4) -0.008(3) -0.007(3) 0.004(3) C4 0.037(4) 0.024(3) 0.027(4) 0.001(3) -0.005(3) 0.001(3) C5 0.037(4) 0.026(4) 0.030(4) 0.004(3) -0.001(3) 0.003(3) C6 0.040(5) 0.035(4) 0.043(5) -0.001(4) -0.008(4) 0.005(4) C7 0.040(5) 0.034(4) 0.045(5) 0.016(4) 0.008(4) 0.005(4) C8 0.036(4) 0.031(4) 0.029(4) 0.001(3) -0.007(3) -0.004(3) C9 0.037(5) 0.039(4) 0.032(4) -0.007(3) -0.001(3) 0.003(4) C10 0.035(4) 0.033(4) 0.030(4) -0.002(3) -0.002(3) -0.006(3) C11 0.041(5) 0.039(4) 0.035(4) -0.012(3) -0.003(3) 0.002(4) C12 0.048(5) 0.032(4) 0.040(4) -0.010(3) -0.004(4) -0.009(4) C13 0.039(5) 0.033(4) 0.033(4) -0.007(3) -0.013(3) 0.006(3) C14 0.043(5) 0.028(4) 0.042(5) -0.007(3) -0.017(4) 0.005(3) C15 0.043(5) 0.031(4) 0.036(4) -0.009(3) -0.011(3) 0.000(3) C16 0.051(5) 0.037(4) 0.033(4) -0.007(3) -0.012(4) -0.001(4) C1Q 0.032(4) 0.021(3) 0.036(4) -0.003(3) -0.003(3) 0.003(3) C6Q 0.037(5) 0.032(4) 0.039(4) -0.005(3) 0.000(3) -0.005(3) C5Q 0.055(6) 0.040(5) 0.034(4) -0.007(4) 0.005(4) -0.002(4) C4Q 0.044(5) 0.030(4) 0.051(5) -0.008(4) 0.008(4) 0.002(4) C3Q 0.030(4) 0.048(5) 0.057(6) -0.007(4) -0.001(4) -0.006(4) C2Q 0.038(5) 0.033(4) 0.047(5) -0.007(4) 0.002(4) 0.003(4) C1T 0.035(4) 0.028(4) 0.039(4) -0.004(3) -0.004(3) -0.002(3) C2T 0.130(11) 0.042(5) 0.038(5) -0.004(4) -0.015(6) -0.006(6) C3T 0.133(12) 0.025(4) 0.059(7) -0.007(4) -0.013(7) 0.006(6) C4T 0.079(8) 0.029(5) 0.069(7) 0.011(4) -0.001(6) 0.007(5) C5T 0.154(14) 0.055(7) 0.055(7) 0.007(5) -0.042(8) 0.018(8) C6T 0.119(10) 0.039(5) 0.056(6) -0.009(4) -0.047(6) 0.012(6) C1U 0.052(5) 0.030(4) 0.045(5) -0.005(3) -0.017(4) -0.005(4) C2U 0.068(7) 0.050(5) 0.047(5) -0.016(4) -0.026(5) 0.007(5) C3U 0.075(8) 0.068(7) 0.047(6) -0.005(5) -0.031(5) -0.002(6) C4U 0.052(6) 0.057(6) 0.066(7) 0.004(5) -0.029(5) 0.007(5) C5U 0.043(6) 0.042(5) 0.093(8) -0.010(5) -0.027(5) 0.011(4) C6U 0.046(5) 0.041(5) 0.060(6) -0.016(4) -0.014(4) -0.001(4) C1V 0.039(5) 0.046(5) 0.058(6) -0.027(4) -0.001(4) -0.012(4) C2V 0.069(8) 0.092(9) 0.068(8) -0.028(7) 0.006(6) -0.014(7) C3V 0.088(11) 0.128(14) 0.113(12) -0.050(11) -0.013(9) -0.060(10) C4V 0.100(12) 0.108(12) 0.122(13) -0.082(10) 0.055(10) -0.082(10) C5V 0.087(10) 0.055(7) 0.115(11) -0.032(7) 0.044(9) -0.021(7) C6V 0.055(6) 0.051(6) 0.079(8) -0.020(5) 0.022(5) -0.003(5) C1W 0.039(4) 0.022(3) 0.037(4) -0.007(3) 0.002(3) 0.008(3) C2W 0.056(6) 0.035(5) 0.057(6) -0.009(4) -0.004(4) -0.005(4) C3W 0.049(6) 0.071(7) 0.079(8) -0.009(6) -0.022(5) -0.011(5) C4W 0.074(8) 0.070(8) 0.067(7) -0.013(6) -0.013(6) -0.028(7) C5W 0.082(8) 0.034(5) 0.062(6) -0.001(4) -0.004(6) -0.025(5) C6W 0.071(7) 0.024(4) 0.050(5) -0.007(4) 0.006(5) 0.000(4) C1X 0.029(4) 0.028(4) 0.036(4) -0.004(3) -0.004(3) 0.000(3) C2X 0.046(5) 0.033(4) 0.047(5) -0.006(4) -0.019(4) 0.005(4) C3X 0.056(6) 0.025(4) 0.064(6) -0.011(4) -0.003(5) 0.005(4) C4X 0.059(6) 0.037(5) 0.053(6) -0.012(4) 0.006(5) 0.000(4) C5X 0.064(7) 0.055(6) 0.043(5) -0.017(4) -0.001(4) -0.013(5) C6X 0.042(5) 0.040(4) 0.039(4) -0.006(4) -0.015(4) 0.005(4) C1Y 0.046(5) 0.031(4) 0.034(4) -0.008(3) 0.008(4) 0.007(4) C2Y 0.074(7) 0.035(5) 0.036(5) 0.003(4) -0.003(4) -0.007(5) C3Y 0.090(9) 0.050(6) 0.057(7) -0.001(5) 0.021(6) -0.014(6) C4Y 0.054(7) 0.059(7) 0.110(10) -0.029(7) 0.005(7) -0.025(6) C5Y 0.048(6) 0.049(6) 0.096(9) -0.012(6) -0.011(6) -0.003(5) C6Y 0.042(5) 0.032(4) 0.058(6) -0.002(4) 0.002(4) 0.004(4) C1Z 0.051(5) 0.032(4) 0.031(4) -0.002(3) 0.000(4) 0.004(4) C2Z 0.044(5) 0.035(4) 0.049(5) -0.009(4) 0.000(4) 0.007(4) C3Z 0.064(7) 0.034(5) 0.057(6) -0.020(4) 0.005(5) 0.005(4) C4Z 0.104(10) 0.042(5) 0.048(6) -0.021(4) -0.002(6) 0.017(6) C5Z 0.071(7) 0.049(6) 0.059(6) -0.020(5) -0.025(5) 0.006(5) C6Z 0.065(7) 0.052(6) 0.053(6) -0.017(5) -0.012(5) 0.014(5) C1S 0.072(8) 0.049(6) 0.064(7) 0.005(5) 0.001(5) 0.024(5) Cl1 0.104(3) 0.0571(17) 0.085(2) 0.0037(15) 0.0072(18) -0.0072(17) Cl2 0.086(2) 0.0482(14) 0.089(2) -0.0182(13) -0.0321(16) 0.0087(14) C3S 0.130(15) 0.093(11) 0.106(12) 0.026(9) 0.007(10) -0.020(10) O1S 0.123(8) 0.050(5) 0.076(6) 0.004(4) 0.001(5) 0.002(5) Cl4 0.216(6) 0.168(5) 0.226(6) -0.022(5) -0.089(5) 0.004(5) C2S 0.11(3) 0.073(18) 0.08(2) -0.020(15) -0.037(18) 0.005(17) Cl3 0.231(14) 0.209(15) 0.197(13) -0.017(10) -0.028(10) -0.044(11) C2SA 0.124(14) 0.135(14) 0.130(11) -0.010(9) -0.027(9) 0.002(10) Cl3A 0.149(10) 0.230(14) 0.142(9) 0.010(9) -0.007(7) 0.018(9) _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 O1 2.047(5) . ? Au1 P1 2.2110(19) . ? Au1 Au2 3.0372(5) . ? Au2 O3 2.038(6) . ? Au2 P2 2.217(2) . ? Au3 O5 2.064(5) . ? Au3 P3 2.213(2) . ? Au3 Au4 3.3619(5) . ? Au4 O7 2.053(5) . ? Au4 P4 2.2199(19) . ? P1 C1Y 1.797(9) . ? P1 C1Z 1.828(8) . ? P1 C1 1.834(8) . ? P2 C1W 1.808(9) . ? P2 C1X 1.809(8) . ? P2 C2 1.818(7) . ? P3 C1V 1.808(9) . ? P3 C1U 1.808(9) . ? P3 C9 1.822(8) . ? P4 C1T 1.815(8) . ? P4 C1Q 1.823(8) . ? P4 C10 1.827(8) . ? O1 C3 1.300(10) . ? O2 C3 1.219(10) . ? O3 C6 1.259(10) . ? O4 C6 1.219(10) . ? O5 C11 1.285(9) . ? O6 C11 1.227(10) . ? O7 C14 1.266(9) . ? O8 C14 1.228(10) . ? C1 C2 1.544(11) . ? C3 C4 1.485(10) . ? C4 C5 1.331(11) . ? C5 C8 1.426(10) 2_757 ? C6 C7 1.493(11) . ? C7 C8 1.323(11) . ? C8 C5 1.426(10) 2_757 ? C9 C10 1.548(11) . ? C11 C12 1.479(11) . ? C12 C13 1.332(11) . ? C13 C16 1.440(11) 2_666 ? C14 C15 1.494(11) . ? C15 C16 1.335(11) . ? C16 C13 1.440(11) 2_666 ? C1Q C6Q 1.375(11) . ? C1Q C2Q 1.391(11) . ? C6Q C5Q 1.393(11) . ? C5Q C4Q 1.375(12) . ? C4Q C3Q 1.348(13) . ? C3Q C2Q 1.396(12) . ? C1T C6T 1.375(12) . ? C1T C2T 1.386(12) . ? C2T C3T 1.357(13) . ? C3T C4T 1.369(15) . ? C4T C5T 1.325(15) . ? C5T C6T 1.396(14) . ? C1U C6U 1.398(12) . ? C1U C2U 1.402(12) . ? C2U C3U 1.357(13) . ? C3U C4U 1.373(15) . ? C4U C5U 1.361(15) . ? C5U C6U 1.387(13) . ? C1V C2V 1.326(16) . ? C1V C6V 1.420(15) . ? C2V C3V 1.390(17) . ? C3V C4V 1.36(2) . ? C4V C5V 1.34(2) . ? C5V C6V 1.427(16) . ? C1W C6W 1.395(10) . ? C1W C2W 1.402(13) . ? C2W C3W 1.382(14) . ? C3W C4W 1.373(15) . ? C4W C5W 1.379(17) . ? C5W C6W 1.376(14) . ? C1X C6X 1.391(11) . ? C1X C2X 1.400(11) . ? C2X C3X 1.406(12) . ? C3X C4X 1.344(14) . ? C4X C5X 1.379(14) . ? C5X C6X 1.372(12) . ? C1Y C6Y 1.381(13) . ? C1Y C2Y 1.389(11) . ? C2Y C3Y 1.377(15) . ? C3Y C4Y 1.347(18) . ? C4Y C5Y 1.387(16) . ? C5Y C6Y 1.388(13) . ? C1Z C6Z 1.337(14) . ? C1Z C2Z 1.424(12) . ? C2Z C3Z 1.390(12) . ? C3Z C4Z 1.406(16) . ? C4Z C5Z 1.376(15) . ? C5Z C6Z 1.407(13) . ? C1S Cl2 1.762(10) . ? C1S Cl1 1.775(10) . ? C3S O1S 1.418(8) . ? Cl4 C2S 1.735(10) . ? Cl4 C2SA 1.747(10) . ? C2S Cl3 1.737(10) . ? C2SA Cl3A 1.736(10) . ? 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 O1 Au1 P1 170.97(19) . . ? O1 Au1 Au2 94.1(2) . . ? P1 Au1 Au2 92.36(6) . . ? O3 Au2 P2 168.53(18) . . ? O3 Au2 Au1 91.1(2) . . ? P2 Au2 Au1 96.38(6) . . ? O5 Au3 P3 173.32(17) . . ? O5 Au3 Au4 85.93(18) . . ? P3 Au3 Au4 99.33(6) . . ? O7 Au4 P4 171.36(18) . . ? O7 Au4 Au3 90.05(18) . . ? P4 Au4 Au3 97.00(6) . . ? C1Y P1 C1Z 105.2(4) . . ? C1Y P1 C1 104.8(4) . . ? C1Z P1 C1 103.9(4) . . ? C1Y P1 Au1 114.0(3) . . ? C1Z P1 Au1 110.3(3) . . ? C1 P1 Au1 117.4(3) . . ? C1W P2 C1X 106.5(3) . . ? C1W P2 C2 105.8(4) . . ? C1X P2 C2 104.7(3) . . ? C1W P2 Au2 111.6(2) . . ? C1X P2 Au2 110.2(3) . . ? C2 P2 Au2 117.2(3) . . ? C1V P3 C1U 105.9(5) . . ? C1V P3 C9 103.9(4) . . ? C1U P3 C9 105.4(4) . . ? C1V P3 Au3 113.4(3) . . ? C1U P3 Au3 112.4(3) . . ? C9 P3 Au3 114.9(3) . . ? C1T P4 C1Q 106.0(3) . . ? C1T P4 C10 103.9(4) . . ? C1Q P4 C10 105.5(4) . . ? C1T P4 Au4 113.0(3) . . ? C1Q P4 Au4 112.0(3) . . ? C10 P4 Au4 115.6(3) . . ? C3 O1 Au1 118.3(5) . . ? C6 O3 Au2 125.9(5) . . ? C11 O5 Au3 117.1(5) . . ? C14 O7 Au4 119.4(5) . . ? C2 C1 P1 116.3(6) . . ? C1 C2 P2 116.5(5) . . ? O2 C3 O1 124.4(7) . . ? O2 C3 C4 121.2(7) . . ? O1 C3 C4 114.4(7) . . ? C5 C4 C3 124.5(7) . . ? C4 C5 C8 126.2(7) . 2_757 ? O4 C6 O3 127.0(8) . . ? O4 C6 C7 121.1(8) . . ? O3 C6 C7 111.9(7) . . ? C8 C7 C6 126.4(7) . . ? C7 C8 C5 122.7(7) . 2_757 ? C10 C9 P3 114.2(5) . . ? C9 C10 P4 113.7(5) . . ? O6 C11 O5 125.2(8) . . ? O6 C11 C12 119.7(8) . . ? O5 C11 C12 115.1(7) . . ? C13 C12 C11 123.5(8) . . ? C12 C13 C16 125.2(8) . 2_666 ? O8 C14 O7 125.4(8) . . ? O8 C14 C15 120.9(7) . . ? O7 C14 C15 113.7(7) . . ? C16 C15 C14 124.8(8) . . ? C15 C16 C13 123.0(8) . 2_666 ? C6Q C1Q C2Q 120.2(7) . . ? C6Q C1Q P4 122.1(6) . . ? C2Q C1Q P4 117.6(6) . . ? C1Q C6Q C5Q 119.9(8) . . ? C4Q C5Q C6Q 119.5(9) . . ? C3Q C4Q C5Q 121.0(8) . . ? C4Q C3Q C2Q 120.7(9) . . ? C1Q C2Q C3Q 118.8(9) . . ? C6T C1T C2T 119.3(8) . . ? C6T C1T P4 120.6(7) . . ? C2T C1T P4 120.1(7) . . ? C3T C2T C1T 120.1(10) . . ? C2T C3T C4T 121.1(10) . . ? C5T C4T C3T 118.7(9) . . ? C4T C5T C6T 122.9(11) . . ? C1T C6T C5T 117.9(10) . . ? C6U C1U C2U 118.9(8) . . ? C6U C1U P3 118.5(7) . . ? C2U C1U P3 122.4(7) . . ? C3U C2U C1U 120.4(9) . . ? C2U C3U C4U 120.4(10) . . ? C5U C4U C3U 120.4(9) . . ? C4U C5U C6U 120.8(9) . . ? C5U C6U C1U 119.0(9) . . ? C2V C1V C6V 118.6(10) . . ? C2V C1V P3 123.9(9) . . ? C6V C1V P3 117.2(8) . . ? C1V C2V C3V 122.1(14) . . ? C4V C3V C2V 119.7(15) . . ? C5V C4V C3V 121.4(13) . . ? C4V C5V C6V 119.2(15) . . ? C1V C6V C5V 118.9(13) . . ? C6W C1W C2W 117.9(9) . . ? C6W C1W P2 121.0(7) . . ? C2W C1W P2 121.0(6) . . ? C3W C2W C1W 120.6(9) . . ? C4W C3W C2W 120.6(11) . . ? C3W C4W C5W 119.2(11) . . ? C6W C5W C4W 121.0(9) . . ? C5W C6W C1W 120.5(10) . . ? C6X C1X C2X 118.9(7) . . ? C6X C1X P2 119.5(6) . . ? C2X C1X P2 121.5(6) . . ? C1X C2X C3X 118.8(8) . . ? C4X C3X C2X 121.6(9) . . ? C3X C4X C5X 119.3(9) . . ? C6X C5X C4X 121.3(9) . . ? C5X C6X C1X 120.1(8) . . ? C6Y C1Y C2Y 118.4(9) . . ? C6Y C1Y P1 120.9(6) . . ? C2Y C1Y P1 120.6(8) . . ? C3Y C2Y C1Y 120.3(10) . . ? C4Y C3Y C2Y 121.1(10) . . ? C3Y C4Y C5Y 119.9(11) . . ? C4Y C5Y C6Y 119.5(11) . . ? C1Y C6Y C5Y 120.7(9) . . ? C6Z C1Z C2Z 120.8(8) . . ? C6Z C1Z P1 124.2(7) . . ? C2Z C1Z P1 115.0(7) . . ? C3Z C2Z C1Z 117.6(9) . . ? C2Z C3Z C4Z 121.5(9) . . ? C5Z C4Z C3Z 119.0(9) . . ? C4Z C5Z C6Z 119.6(10) . . ? C1Z C6Z C5Z 121.5(10) . . ? Cl2 C1S Cl1 111.2(6) . . ? C2S Cl4 C2SA 31.8(14) . . ? Cl4 C2S Cl3 106.7(9) . . ? Cl3A C2SA Cl4 107.7(9) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 3.658 _refine_diff_density_min -2.433 _refine_diff_density_rms 0.266