# 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 'Antonio M. Echavarren' _publ_contact_author_email aechavarren@iciq.es loop_ _publ_author_name 'Mihai Raducan' 'Maria Moreno' 'Christophe Bour' 'Antonio M. Echavarren' data_cb004_0m _database_code_depnum_ccdc_archive 'CCDC 841517' #TrackingRef 'web_deposit_cif_file_0_AntonioM.Echavarren_1314183768.CB004_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75.50 H58.50 Au Cl1.50 O4.50 P2 Si2' _chemical_formula_weight 1405.98 _chemical_absolute_configuration ad 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' Si Si 0.0817 0.0704 '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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.5423(4) _cell_length_b 14.3340(6) _cell_length_c 40.0455(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6625.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3947 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 22.98 _exptl_crystal_description Plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2840 _exptl_absorpt_coefficient_mu 2.415 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8135 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 70 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 40304 _diffrn_reflns_av_R_equivalents 0.1441 _diffrn_reflns_av_sigmaI/netI 0.1549 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -50 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 26.45 _reflns_number_total 13548 _reflns_number_gt 10065 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0467P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.015(8) _refine_ls_number_reflns 13548 _refine_ls_number_parameters 839 _refine_ls_number_restraints 176 _refine_ls_R_factor_all 0.0968 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.1598 _refine_ls_wR_factor_gt 0.1398 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.66408(3) 0.76279(3) 0.099245(9) 0.02726(11) Uani 1 1 d . . . C1 C 0.6255(7) 0.6643(7) 0.1989(2) 0.0198(18) Uani 1 1 d . . . O1 O 0.5996(5) 0.6695(5) 0.16515(16) 0.0258(14) Uani 1 1 d . . . P1 P 0.62220(19) 0.58257(19) 0.14065(6) 0.0245(5) Uani 1 1 d . . . Si1 Si 0.37865(19) 0.69378(18) 0.21015(6) 0.0223(5) Uani 1 1 d . . . C2 C 0.5331(6) 0.6697(6) 0.2221(2) 0.0204(19) Uani 1 1 d . . . O2 O 0.7533(5) 0.5508(5) 0.14929(16) 0.0231(14) Uani 1 1 d . . . P2 P 0.69664(19) 0.91381(18) 0.09654(7) 0.0284(5) Uani 1 1 d . . . Si2 Si 0.9370(17) 0.553(2) 0.0903(7) 0.033(4) Uani 0.549(7) 1 d PU A 1 Si2' Si 0.960(2) 0.546(2) 0.0928(8) 0.022(3) Uani 0.451(7) 1 d PU A 2 C3 C 0.5633(8) 0.6621(7) 0.2547(2) 0.027(2) Uani 1 1 d . . . H3 H 0.5033 0.6655 0.2709 0.033 Uiso 1 1 calc R . . O3 O 0.5471(5) 0.5026(5) 0.14751(17) 0.0307(16) Uani 1 1 d . . . C4 C 0.6796(7) 0.6495(6) 0.2664(2) 0.0232(19) Uani 1 1 d . . . O4 O 0.6184(5) 0.6255(5) 0.10644(15) 0.0289(16) Uani 1 1 d . . . C5 C 0.7064(7) 0.6416(7) 0.3006(2) 0.027(2) Uani 1 1 d . . . H5 H 0.6458 0.6425 0.3166 0.033 Uiso 1 1 calc R . . C6 C 0.8188(8) 0.6326(7) 0.3110(2) 0.029(2) Uani 1 1 d . . . H6 H 0.8370 0.6292 0.3341 0.035 Uiso 1 1 calc R . . C7 C 0.9069(8) 0.6286(7) 0.2867(3) 0.030(2) Uani 1 1 d . . . H7 H 0.9846 0.6203 0.2939 0.036 Uiso 1 1 calc R . . C8 C 0.8856(7) 0.6362(7) 0.2535(2) 0.024(2) Uani 1 1 d . . . H8 H 0.9477 0.6338 0.2379 0.029 Uiso 1 1 calc R . . C9 C 0.7680(7) 0.6480(7) 0.2419(2) 0.022(2) Uani 1 1 d . . . C10 C 0.7419(7) 0.6614(7) 0.2079(2) 0.0208(19) Uani 1 1 d . . . C11 C 0.8350(7) 0.6756(6) 0.1823(2) 0.0267(19) Uani 1 1 d . . . C12 C 0.9105(6) 0.7523(7) 0.1850(2) 0.0227(19) Uani 1 1 d . . . C13 C 0.9022(7) 0.8196(7) 0.2097(3) 0.028(2) Uani 1 1 d . . . H13 H 0.8406 0.8158 0.2254 0.034 Uiso 1 1 calc R . . C14 C 0.9793(7) 0.8911(7) 0.2123(3) 0.031(2) Uani 1 1 d . . . H14 H 0.9711 0.9364 0.2295 0.037 Uiso 1 1 calc R . . C15 C 1.0722(7) 0.8972(7) 0.1892(3) 0.028(2) Uani 1 1 d . . . H15 H 1.1280 0.9455 0.1913 0.033 Uiso 1 1 calc R . . C16 C 1.0808(7) 0.8342(7) 0.1644(2) 0.026(2) Uani 1 1 d . . . H16 H 1.1414 0.8402 0.1485 0.031 Uiso 1 1 calc R . . C17 C 1.0021(6) 0.7595(7) 0.1615(2) 0.0234(18) Uani 1 1 d . . . C18 C 1.0093(7) 0.6940(7) 0.1351(2) 0.024(2) Uani 1 1 d . A . H18 H 1.0724 0.6983 0.1199 0.029 Uiso 1 1 calc R . . C19 C 0.9285(7) 0.6242(7) 0.1305(2) 0.024(2) Uani 1 1 d . . . C20 C 0.8383(7) 0.6194(6) 0.1540(2) 0.0233(18) Uani 1 1 d . A . C21 C 0.3137(6) 0.7640(7) 0.2446(2) 0.0265(19) Uani 1 1 d . . . C22 C 0.1972(6) 0.7521(8) 0.2549(2) 0.029(2) Uani 1 1 d . . . H22 H 0.1534 0.7013 0.2465 0.035 Uiso 1 1 calc R . . C23 C 0.1473(7) 0.8123(8) 0.2769(2) 0.034(2) Uani 1 1 d . . . H23 H 0.0680 0.8039 0.2825 0.040 Uiso 1 1 calc R . . C24 C 0.2079(8) 0.8863(9) 0.2915(3) 0.041(3) Uani 1 1 d . . . H24 H 0.1718 0.9273 0.3070 0.049 Uiso 1 1 calc R . . C25 C 0.3230(9) 0.8967(8) 0.2825(3) 0.042(3) Uani 1 1 d . . . H25 H 0.3677 0.9453 0.2922 0.051 Uiso 1 1 calc R . . C26 C 0.3737(7) 0.8371(8) 0.2594(3) 0.031(2) Uani 1 1 d . . . H26 H 0.4525 0.8467 0.2535 0.038 Uiso 1 1 calc R . . C27 C 0.3025(7) 0.5796(7) 0.2055(2) 0.025(2) Uani 1 1 d . . . C28 C 0.1821(7) 0.5760(7) 0.1970(2) 0.027(2) Uani 1 1 d . . . H28 H 0.1406 0.6322 0.1930 0.033 Uiso 1 1 calc R . . C29 C 0.1260(8) 0.4912(8) 0.1947(3) 0.036(3) Uani 1 1 d . . . H29 H 0.0461 0.4896 0.1891 0.043 Uiso 1 1 calc R . . C30 C 0.1855(9) 0.4076(7) 0.2004(3) 0.034(2) Uani 1 1 d . . . H30 H 0.1461 0.3495 0.1991 0.041 Uiso 1 1 calc R . . C31 C 0.3016(8) 0.4105(7) 0.2081(3) 0.029(2) Uani 1 1 d . . . H31 H 0.3424 0.3541 0.2121 0.035 Uiso 1 1 calc R . . C32 C 0.3596(7) 0.4952(7) 0.2099(3) 0.027(2) Uani 1 1 d . . . H32 H 0.4405 0.4955 0.2143 0.033 Uiso 1 1 calc R . . C33 C 0.3659(6) 0.7668(7) 0.1712(2) 0.0263(19) Uani 1 1 d . . . C34 C 0.3555(6) 0.7263(8) 0.1401(2) 0.029(2) Uani 1 1 d . . . H34 H 0.3546 0.6602 0.1385 0.035 Uiso 1 1 calc R . . C35 C 0.3463(7) 0.7793(8) 0.1109(2) 0.034(2) Uani 1 1 d . . . H35 H 0.3387 0.7498 0.0898 0.041 Uiso 1 1 calc R . . C36 C 0.3485(8) 0.8772(9) 0.1134(3) 0.040(3) Uani 1 1 d . . . H36 H 0.3431 0.9146 0.0938 0.048 Uiso 1 1 calc R . . C37 C 0.3584(7) 0.9187(8) 0.1444(3) 0.033(2) Uani 1 1 d . . . H37 H 0.3585 0.9847 0.1464 0.040 Uiso 1 1 calc R . . C38 C 0.3682(7) 0.8637(7) 0.1726(3) 0.032(2) Uani 1 1 d . . . H38 H 0.3769 0.8932 0.1937 0.038 Uiso 1 1 calc R . . C39 C 1.1016(8) 0.5490(14) 0.0793(4) 0.029(7) Uani 0.549(7) 1 d PGU A 1 C40 C 1.1456(11) 0.5673(15) 0.0476(4) 0.033(6) Uani 0.549(7) 1 d PGU A 1 H40A H 1.0950 0.5862 0.0302 0.040 Uiso 0.549(7) 1 calc PR A 1 C41 C 1.2635(12) 0.5579(13) 0.0415(3) 0.044(5) Uani 0.549(7) 1 d PGU A 1 H41A H 1.2936 0.5704 0.0199 0.053 Uiso 0.549(7) 1 calc PR A 1 C42 C 1.3375(8) 0.5302(11) 0.0670(4) 0.039(4) Uani 0.549(7) 1 d PGU A 1 H42A H 1.4182 0.5238 0.0628 0.047 Uiso 0.549(7) 1 calc PR A 1 C43 C 1.2936(10) 0.5119(11) 0.0987(3) 0.045(5) Uani 0.549(7) 1 d PGU A 1 H43A H 1.3442 0.4930 0.1161 0.054 Uiso 0.549(7) 1 calc PR A 1 C44 C 1.1756(11) 0.5213(11) 0.1048(3) 0.032(4) Uani 0.549(7) 1 d PGU A 1 H44A H 1.1456 0.5088 0.1264 0.039 Uiso 0.549(7) 1 calc PR A 1 C39' C 1.1115(9) 0.5627(18) 0.0783(5) 0.028(8) Uani 0.451(7) 1 d PGU A 2 C40' C 1.1305(14) 0.579(2) 0.0445(5) 0.045(9) Uani 0.451(7) 1 d PGU A 2 H40B H 1.0669 0.5907 0.0301 0.054 Uiso 0.451(7) 1 calc PR A 2 C41' C 1.2427(17) 0.5778(18) 0.0319(4) 0.071(11) Uani 0.451(7) 1 d PGU A 2 H41B H 1.2557 0.5888 0.0088 0.085 Uiso 0.451(7) 1 calc PR A 2 C42' C 1.3358(12) 0.5605(14) 0.0530(4) 0.037(5) Uani 0.451(7) 1 d PGU A 2 H42B H 1.4124 0.5597 0.0444 0.044 Uiso 0.451(7) 1 calc PR A 2 C43' C 1.3167(10) 0.5443(12) 0.0868(4) 0.031(5) Uani 0.451(7) 1 d PGU A 2 H43B H 1.3803 0.5325 0.1013 0.037 Uiso 0.451(7) 1 calc PR A 2 C44' C 1.2045(12) 0.5454(13) 0.0995(4) 0.025(5) Uani 0.451(7) 1 d PGU A 2 H44B H 1.1915 0.5344 0.1226 0.030 Uiso 0.451(7) 1 calc PR A 2 C45' C 0.8519(12) 0.5777(12) 0.0606(4) 0.028(5) Uani 0.451(7) 1 d PGU A 2 C46' C 0.8561(13) 0.6687(11) 0.0487(4) 0.039(6) Uani 0.451(7) 1 d PGU A 2 H46A H 0.9148 0.7100 0.0563 0.046 Uiso 0.451(7) 1 calc PR A 2 C47' C 0.7746(16) 0.6992(11) 0.0256(5) 0.082(11) Uani 0.451(7) 1 d PGU A 2 H47A H 0.7775 0.7613 0.0174 0.098 Uiso 0.451(7) 1 calc PR A 2 C48' C 0.6888(15) 0.6386(14) 0.0144(5) 0.050(11) Uani 0.451(7) 1 d PGU A 2 H48A H 0.6331 0.6595 -0.0013 0.060 Uiso 0.451(7) 1 calc PR A 2 C49' C 0.6846(14) 0.5477(13) 0.0264(5) 0.075(10) Uani 0.451(7) 1 d PGU A 2 H49A H 0.6260 0.5063 0.0188 0.090 Uiso 0.451(7) 1 calc PR A 2 C50' C 0.7661(15) 0.5172(10) 0.0495(5) 0.050(7) Uani 0.451(7) 1 d PGU A 2 H50A H 0.7632 0.4550 0.0576 0.060 Uiso 0.451(7) 1 calc PR A 2 C45 C 0.8611(9) 0.6202(8) 0.0561(3) 0.018(4) Uani 0.549(7) 1 d PGU A 1 C46 C 0.9046(8) 0.7034(8) 0.0434(3) 0.031(4) Uani 0.549(7) 1 d PGU A 1 H46B H 0.9754 0.7279 0.0517 0.038 Uiso 0.549(7) 1 calc PR A 1 C47 C 0.8445(11) 0.7506(8) 0.0185(3) 0.053(5) Uani 0.549(7) 1 d PGU A 1 H47B H 0.8742 0.8075 0.0099 0.064 Uiso 0.549(7) 1 calc PR A 1 C48 C 0.7409(11) 0.7147(10) 0.0064(3) 0.053(6) Uani 0.549(7) 1 d PGU A 1 H48B H 0.6998 0.7471 -0.0106 0.063 Uiso 0.549(7) 1 calc PR A 1 C49 C 0.6974(9) 0.6316(10) 0.0190(4) 0.052(9) Uani 0.549(7) 1 d PGU A 1 H49B H 0.6266 0.6070 0.0107 0.063 Uiso 0.549(7) 1 calc PR A 1 C50 C 0.7575(9) 0.5843(8) 0.0439(3) 0.029(4) Uani 0.549(7) 1 d PGU A 1 H50B H 0.7278 0.5274 0.0526 0.035 Uiso 0.549(7) 1 calc PR A 1 C57 C 0.5817(8) 0.9736(8) 0.0745(2) 0.033(2) Uani 1 1 d . . . C58 C 0.5340(8) 0.9278(9) 0.0460(3) 0.041(3) Uani 1 1 d . . . H58 H 0.5654 0.8696 0.0391 0.050 Uiso 1 1 calc R . . C59 C 0.4440(8) 0.9659(11) 0.0284(3) 0.050(4) Uani 1 1 d . . . H59 H 0.4099 0.9333 0.0102 0.061 Uiso 1 1 calc R . . C60 C 0.4031(9) 1.0546(10) 0.0379(3) 0.049(3) Uani 1 1 d . . . H60 H 0.3441 1.0840 0.0252 0.059 Uiso 1 1 calc R . . C61 C 0.4485(10) 1.0990(9) 0.0657(4) 0.057(4) Uani 1 1 d . . . H61 H 0.4170 1.1571 0.0726 0.068 Uiso 1 1 calc R . . C62 C 0.5391(9) 1.0598(9) 0.0833(3) 0.045(3) Uani 1 1 d . . . H62 H 0.5722 1.0925 0.1016 0.055 Uiso 1 1 calc R . . C63 C 0.7040(8) 0.9625(7) 0.1379(3) 0.029(2) Uani 1 1 d . . . C64 C 0.7494(12) 1.0489(10) 0.1441(3) 0.054(3) Uani 1 1 d . . . H64 H 0.7778 1.0847 0.1259 0.065 Uiso 1 1 calc R . . C65 C 0.7554(11) 1.0862(10) 0.1761(3) 0.053(3) Uani 1 1 d . . . H65 H 0.7922 1.1445 0.1800 0.063 Uiso 1 1 calc R . . C66 C 0.7061(8) 1.0360(8) 0.2025(3) 0.037(3) Uani 1 1 d . . . H66 H 0.7079 1.0606 0.2245 0.045 Uiso 1 1 calc R . . C67 C 0.6560(8) 0.9525(7) 0.1965(3) 0.035(2) Uani 1 1 d . . . H67 H 0.6217 0.9188 0.2144 0.042 Uiso 1 1 calc R . . C68 C 0.6542(8) 0.9151(6) 0.1642(2) 0.029(2) Uani 1 1 d . . . H68 H 0.6182 0.8564 0.1604 0.034 Uiso 1 1 calc R . . C69 C 0.8315(8) 0.9517(7) 0.0771(2) 0.029(2) Uani 1 1 d . . . C70 C 0.8370(8) 1.0079(7) 0.0505(2) 0.032(2) Uani 1 1 d . . . H70 H 0.7666 1.0296 0.0410 0.038 Uiso 1 1 calc R . . C71 C 0.9407(10) 1.0359(10) 0.0362(3) 0.048(3) Uani 1 1 d . . . H71 H 0.9423 1.0734 0.0166 0.057 Uiso 1 1 calc R . . C72 C 1.0436(9) 1.0065(10) 0.0520(3) 0.051(3) Uani 1 1 d . . . H72 H 1.1171 1.0270 0.0442 0.061 Uiso 1 1 calc R . . C73 C 1.0354(10) 0.9500(12) 0.0778(4) 0.061(4) Uani 1 1 d . . . H73 H 1.1051 0.9273 0.0874 0.073 Uiso 1 1 calc R . . C74 C 0.9345(10) 0.9226(10) 0.0912(3) 0.054(4) Uani 1 1 d . . . H74 H 0.9340 0.8833 0.1103 0.064 Uiso 1 1 calc R . . C51 C 0.9049(12) 0.4276(7) 0.0928(4) 0.050 Uiso 0.549(7) 1 d PG A 1 C52 C 0.9078(12) 0.3825(10) 0.1235(3) 0.050 Uiso 0.549(7) 1 d PG A 1 H52A H 0.9027 0.4176 0.1436 0.060 Uiso 0.549(7) 1 calc PR A 1 C53 C 0.9180(11) 0.2859(10) 0.1249(3) 0.050 Uiso 0.549(7) 1 d PG A 1 H53A H 0.9200 0.2551 0.1459 0.060 Uiso 0.549(7) 1 calc PR A 1 C54 C 0.9254(11) 0.2345(7) 0.0955(4) 0.050 Uiso 0.549(7) 1 d PG A 1 H54A H 0.9324 0.1685 0.0965 0.060 Uiso 0.549(7) 1 calc PR A 1 C55 C 0.9226(11) 0.2796(9) 0.0648(3) 0.050 Uiso 0.549(7) 1 d PG A 1 H55A H 0.9276 0.2445 0.0448 0.060 Uiso 0.549(7) 1 calc PR A 1 C56 C 0.9123(12) 0.3762(10) 0.0635(3) 0.050 Uiso 0.549(7) 1 d PG A 1 H56A H 0.9104 0.4070 0.0425 0.060 Uiso 0.549(7) 1 calc PR A 1 C51' C 0.9517(14) 0.4148(9) 0.1040(5) 0.050 Uiso 0.451(7) 1 d PG A 2 C52' C 0.8488(11) 0.3729(11) 0.1140(5) 0.050 Uiso 0.451(7) 1 d PG A 2 H52B H 0.7805 0.4094 0.1164 0.060 Uiso 0.451(7) 1 calc PR A 2 C53' C 0.8458(10) 0.2777(11) 0.1206(4) 0.050 Uiso 0.451(7) 1 d PG A 2 H53B H 0.7754 0.2491 0.1274 0.060 Uiso 0.451(7) 1 calc PR A 2 C54' C 0.9456(13) 0.2244(9) 0.1171(5) 0.050 Uiso 0.451(7) 1 d PG A 2 H54B H 0.9435 0.1594 0.1216 0.060 Uiso 0.451(7) 1 calc PR A 2 C55' C 1.0485(10) 0.2663(11) 0.1071(5) 0.050 Uiso 0.451(7) 1 d PG A 2 H55B H 1.1168 0.2298 0.1047 0.060 Uiso 0.451(7) 1 calc PR A 2 C56' C 1.0516(11) 0.3615(11) 0.1005(5) 0.050 Uiso 0.451(7) 1 d PG A 2 H56B H 1.1219 0.3901 0.0937 0.060 Uiso 0.451(7) 1 calc PR A 2 C1S C 0.469(2) 0.3215(18) 0.1292(7) 0.053(7) Uani 0.50 1 d P . . H1S H 0.4716 0.3828 0.1411 0.063 Uiso 0.50 1 calc PR . . Cl1S Cl 0.5450(5) 0.2433(6) 0.15129(16) 0.0593(16) Uani 0.50 1 d P . . Cl2S Cl 0.3256(6) 0.2916(5) 0.12286(18) 0.0643(17) Uani 0.50 1 d P . . Cl3S Cl 0.5361(6) 0.3356(5) 0.0876(2) 0.070(2) Uani 0.50 1 d P . . O1W O 0.1960(17) 1.2435(18) 0.0401(5) 0.093(6) Uani 0.50 1 d PDU . . H1WA H 0.2573 1.2617 0.0493 0.139 Uiso 0.50 1 calc PR . . C1W C 0.182(2) 1.2907(17) 0.0090(5) 0.067(8) Uani 0.50 1 d PDU . . H1WB H 0.2544 1.3211 0.0014 0.081 Uiso 0.50 1 calc PR . . H1WC H 0.1182 1.3369 0.0096 0.081 Uiso 0.50 1 calc PR . . C2W C 0.151(3) 1.204(2) -0.0120(9) 0.091(10) Uani 0.50 1 d PDU . . H2WA H 0.1061 1.2235 -0.0316 0.136 Uiso 0.50 1 calc PR . . H2WB H 0.1058 1.1608 0.0015 0.136 Uiso 0.50 1 calc PR . . H2WC H 0.2228 1.1737 -0.0194 0.136 Uiso 0.50 1 calc PR . . 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 0.03118(15) 0.02776(18) 0.02285(17) 0.00156(17) -0.00119(14) -0.00018(16) C1 0.029(4) 0.021(5) 0.009(4) -0.005(4) 0.009(3) 0.001(4) O1 0.031(3) 0.025(4) 0.022(3) 0.004(3) 0.006(2) 0.009(3) P1 0.0257(10) 0.0266(14) 0.0213(13) -0.0023(11) -0.0008(9) 0.0022(10) Si1 0.0250(10) 0.0203(13) 0.0216(13) 0.0001(11) 0.0033(9) 0.0015(10) C2 0.021(4) 0.011(4) 0.029(5) 0.004(4) 0.008(3) 0.000(3) O2 0.022(3) 0.018(4) 0.029(4) -0.001(3) -0.001(2) 0.001(3) P2 0.0343(11) 0.0267(13) 0.0243(13) 0.0034(13) -0.0020(10) -0.0009(9) Si2 0.033(8) 0.039(5) 0.027(6) -0.009(4) 0.008(6) 0.000(5) Si2' 0.017(6) 0.025(6) 0.023(5) -0.010(4) 0.002(5) -0.010(5) C3 0.034(5) 0.019(5) 0.029(6) 0.000(4) 0.013(4) 0.005(4) O3 0.031(3) 0.031(4) 0.031(4) 0.007(3) -0.003(3) -0.001(3) C4 0.031(4) 0.016(5) 0.023(5) 0.005(4) 0.000(4) -0.003(4) O4 0.023(3) 0.038(4) 0.025(4) -0.001(3) 0.003(2) -0.005(3) C5 0.033(4) 0.027(6) 0.021(5) 0.000(4) 0.004(4) 0.002(4) C6 0.039(5) 0.030(5) 0.018(5) 0.004(4) -0.008(4) 0.009(5) C7 0.030(4) 0.027(6) 0.033(6) 0.008(5) -0.002(4) 0.007(4) C8 0.027(4) 0.025(5) 0.020(5) -0.004(4) 0.002(3) -0.007(4) C9 0.029(4) 0.012(5) 0.027(5) 0.005(4) 0.004(4) -0.002(4) C10 0.026(4) 0.021(5) 0.015(5) 0.000(4) 0.002(3) -0.001(4) C11 0.018(3) 0.031(5) 0.031(5) 0.000(4) 0.001(4) 0.005(4) C12 0.023(3) 0.024(6) 0.022(4) 0.001(4) -0.006(3) 0.003(4) C13 0.024(4) 0.018(5) 0.043(6) 0.009(4) -0.003(4) 0.007(4) C14 0.031(5) 0.023(6) 0.038(6) -0.008(5) 0.003(4) 0.003(4) C15 0.021(4) 0.019(5) 0.042(6) 0.007(5) 0.003(4) -0.004(4) C16 0.024(4) 0.027(5) 0.026(5) -0.001(4) 0.002(3) 0.002(4) C17 0.027(3) 0.015(5) 0.029(5) 0.005(4) 0.000(3) 0.007(4) C18 0.024(4) 0.028(5) 0.021(5) 0.005(4) -0.002(3) 0.007(4) C19 0.030(4) 0.022(5) 0.019(5) -0.002(4) 0.003(3) 0.000(4) C20 0.021(3) 0.026(5) 0.023(5) 0.007(4) 0.000(4) 0.001(4) C21 0.021(4) 0.027(5) 0.031(5) 0.007(4) 0.003(3) 0.007(4) C22 0.021(3) 0.031(6) 0.036(5) -0.015(5) -0.003(3) -0.005(4) C23 0.021(4) 0.053(7) 0.027(5) -0.004(5) 0.002(4) -0.002(4) C24 0.034(5) 0.050(8) 0.038(6) -0.013(6) 0.000(4) 0.000(5) C25 0.040(5) 0.040(6) 0.047(7) -0.010(5) 0.007(5) -0.004(5) C26 0.024(4) 0.034(6) 0.036(6) -0.010(5) 0.008(4) -0.003(4) C27 0.027(4) 0.034(6) 0.014(5) -0.001(4) -0.003(3) 0.003(4) C28 0.035(5) 0.021(5) 0.026(5) 0.001(4) -0.001(4) -0.002(4) C29 0.033(5) 0.034(6) 0.040(6) 0.009(5) -0.015(4) -0.005(4) C30 0.049(6) 0.025(5) 0.029(6) -0.005(4) -0.003(4) -0.017(5) C31 0.041(5) 0.015(5) 0.032(6) -0.003(4) 0.004(4) 0.003(4) C32 0.027(4) 0.017(5) 0.037(6) 0.003(4) 0.000(4) -0.002(4) C33 0.024(4) 0.023(5) 0.032(5) 0.000(5) 0.000(3) -0.002(4) C34 0.023(4) 0.030(5) 0.034(5) 0.002(5) -0.002(3) 0.010(4) C35 0.025(4) 0.047(6) 0.029(5) 0.002(4) 0.003(3) 0.009(5) C36 0.028(5) 0.055(7) 0.036(6) 0.013(5) 0.010(4) -0.002(5) C37 0.019(4) 0.028(6) 0.053(7) 0.012(5) 0.002(4) 0.003(4) C38 0.025(4) 0.023(5) 0.047(6) 0.011(5) 0.002(4) -0.002(4) C39 0.033(8) 0.026(8) 0.030(8) -0.003(5) 0.003(4) -0.004(4) C40 0.032(7) 0.038(7) 0.029(7) 0.002(4) 0.002(4) 0.003(4) C41 0.045(7) 0.045(7) 0.044(7) -0.003(5) 0.002(5) 0.005(5) C42 0.036(5) 0.042(6) 0.039(6) -0.003(5) 0.001(5) 0.001(5) C43 0.044(6) 0.044(6) 0.046(6) -0.004(5) -0.001(5) 0.007(4) C44 0.034(6) 0.032(6) 0.030(6) -0.006(4) -0.005(4) -0.003(5) C39' 0.031(9) 0.025(9) 0.028(9) 0.000(5) 0.004(5) -0.002(5) C40' 0.043(9) 0.048(10) 0.044(10) 0.001(5) 0.000(5) 0.003(5) C41' 0.071(11) 0.073(11) 0.069(11) 0.001(5) 0.003(5) 0.003(5) C42' 0.035(6) 0.036(7) 0.038(7) -0.001(5) 0.006(5) 0.001(5) C43' 0.028(6) 0.034(7) 0.032(7) -0.002(5) 0.000(4) -0.002(5) C44' 0.024(6) 0.026(6) 0.025(6) -0.001(5) 0.000(5) 0.003(5) C45' 0.030(6) 0.029(7) 0.024(6) 0.001(5) -0.001(4) -0.002(5) C46' 0.040(7) 0.040(7) 0.037(7) -0.002(5) 0.003(5) 0.003(5) C47' 0.084(11) 0.082(12) 0.080(12) -0.002(5) 0.001(5) 0.004(5) C48' 0.044(11) 0.056(12) 0.048(11) -0.002(5) -0.004(5) 0.009(5) C49' 0.075(10) 0.079(11) 0.072(11) -0.003(5) 0.000(5) -0.001(5) C50' 0.049(8) 0.051(8) 0.049(8) -0.001(5) 0.002(5) -0.001(5) C45 0.021(5) 0.016(5) 0.018(5) -0.002(4) -0.001(4) 0.003(4) C46 0.031(5) 0.031(6) 0.032(6) 0.000(4) -0.003(4) -0.001(4) C47 0.056(6) 0.054(7) 0.049(6) 0.001(5) -0.005(5) 0.003(5) C48 0.052(7) 0.055(7) 0.052(7) -0.004(5) -0.006(5) 0.009(5) C49 0.048(10) 0.059(10) 0.049(10) -0.003(5) -0.002(5) 0.009(5) C50 0.026(5) 0.034(6) 0.028(6) -0.006(4) -0.002(4) -0.003(4) C57 0.032(5) 0.048(7) 0.018(5) 0.007(5) 0.008(4) -0.003(5) C58 0.033(5) 0.054(8) 0.038(7) 0.006(6) 0.006(4) 0.011(5) C59 0.033(5) 0.091(11) 0.027(6) 0.012(7) 0.001(4) -0.003(6) C60 0.034(5) 0.051(8) 0.064(9) 0.025(7) -0.003(5) 0.012(5) C61 0.048(6) 0.030(7) 0.092(11) 0.014(7) 0.007(7) 0.021(6) C62 0.048(6) 0.038(7) 0.051(8) 0.012(6) -0.007(5) -0.002(5) C63 0.032(5) 0.026(6) 0.029(6) 0.005(5) -0.012(4) -0.001(4) C64 0.084(9) 0.041(8) 0.038(7) 0.005(6) 0.007(6) -0.026(7) C65 0.083(8) 0.041(8) 0.033(7) -0.006(6) 0.001(6) -0.016(7) C66 0.041(5) 0.038(7) 0.032(6) 0.003(5) -0.007(4) 0.012(5) C67 0.032(4) 0.041(6) 0.032(6) 0.002(5) 0.002(4) -0.003(5) C68 0.037(5) 0.017(5) 0.031(5) 0.005(4) 0.004(4) 0.006(4) C69 0.033(4) 0.032(5) 0.023(5) -0.002(4) 0.000(4) -0.005(5) C70 0.026(4) 0.037(6) 0.034(5) 0.006(4) 0.001(4) 0.003(5) C71 0.055(6) 0.051(8) 0.038(7) 0.009(6) 0.011(5) -0.003(6) C72 0.039(6) 0.066(9) 0.047(8) -0.002(7) 0.013(5) -0.005(6) C73 0.034(6) 0.088(12) 0.061(9) 0.016(9) -0.007(6) 0.003(6) C74 0.046(6) 0.066(9) 0.049(9) 0.029(7) 0.001(5) -0.002(6) C1S 0.065(14) 0.037(15) 0.056(17) -0.023(12) 0.010(12) -0.010(12) Cl1S 0.065(3) 0.059(5) 0.054(4) 0.006(4) 0.007(3) -0.011(4) Cl2S 0.083(4) 0.045(4) 0.065(4) -0.008(3) 0.016(4) -0.012(4) Cl3S 0.084(4) 0.052(4) 0.074(5) -0.005(4) 0.021(4) -0.022(4) O1W 0.092(7) 0.093(8) 0.092(8) 0.000(5) 0.002(5) 0.006(5) C1W 0.070(8) 0.064(9) 0.068(9) 0.003(5) 0.007(5) 0.001(5) C2W 0.089(11) 0.093(11) 0.090(11) -0.001(5) -0.001(5) 0.002(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 O4 2.057(7) . ? Au1 P2 2.200(3) . ? C1 O1 1.388(10) . ? C1 C10 1.391(12) . ? C1 C2 1.415(11) . ? O1 P1 1.607(7) . ? P1 O3 1.463(7) . ? P1 O4 1.503(7) . ? P1 O2 1.617(6) . ? Si1 C21 1.864(9) . ? Si1 C27 1.867(10) . ? Si1 C2 1.878(8) . ? Si1 C33 1.885(10) . ? C2 C3 1.355(13) . ? O2 C20 1.402(11) . ? P2 C63 1.801(11) . ? P2 C57 1.810(10) . ? P2 C69 1.823(10) . ? Si2 C51 1.83(3) . ? Si2 C45 1.89(3) . ? Si2 C19 1.91(3) . ? Si2 C39 1.95(2) . ? Si2' C45' 1.85(3) . ? Si2' C39' 1.86(3) . ? Si2' C19 1.91(3) . ? Si2' C51' 1.94(3) . ? C3 C4 1.433(13) . ? C4 C5 1.409(13) . ? C4 C9 1.415(12) . ? C5 C6 1.368(13) . ? C6 C7 1.407(13) . ? C7 C8 1.358(13) . ? C8 C9 1.445(12) . ? C9 C10 1.408(13) . ? C10 C11 1.499(12) . ? C11 C20 1.392(12) . ? C11 C12 1.407(13) . ? C12 C13 1.384(13) . ? C12 C17 1.422(11) . ? C13 C14 1.361(13) . ? C14 C15 1.418(13) . ? C15 C16 1.348(14) . ? C16 C17 1.408(13) . ? C17 C18 1.415(13) . ? C18 C19 1.381(13) . ? C19 C20 1.406(12) . ? C21 C26 1.389(14) . ? C21 C22 1.418(10) . ? C22 C23 1.359(13) . ? C23 C24 1.399(15) . ? C24 C25 1.385(14) . ? C25 C26 1.388(14) . ? C27 C32 1.389(13) . ? C27 C28 1.431(12) . ? C28 C29 1.381(14) . ? C29 C30 1.400(15) . ? C30 C31 1.375(13) . ? C31 C32 1.389(13) . ? C33 C34 1.379(13) . ? C33 C38 1.390(15) . ? C34 C35 1.398(13) . ? C35 C36 1.407(16) . ? C36 C37 1.383(15) . ? C37 C38 1.380(14) . ? C39 C40 1.3900 . ? C39 C44 1.3900 . ? C40 C41 1.3900 . ? C41 C42 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C39' C40' 1.3900 . ? C39' C44' 1.3900 . ? C40' C41' 1.3900 . ? C41' C42' 1.3900 . ? C42' C43' 1.3900 . ? C43' C44' 1.3900 . ? C45' C46' 1.3900 . ? C45' C50' 1.3900 . ? C46' C47' 1.3900 . ? C47' C48' 1.3900 . ? C48' C49' 1.3900 . ? C49' C50' 1.3900 . ? C45 C46 1.3900 . ? C45 C50 1.3900 . ? C46 C47 1.3900 . ? C47 C48 1.3900 . ? C48 C49 1.3900 . ? C49 C50 1.3900 . ? C57 C62 1.375(17) . ? C57 C58 1.426(15) . ? C58 C59 1.369(15) . ? C59 C60 1.41(2) . ? C60 C61 1.383(19) . ? C61 C62 1.382(16) . ? C63 C64 1.367(16) . ? C63 C68 1.379(13) . ? C64 C65 1.390(17) . ? C65 C66 1.398(16) . ? C66 C67 1.352(16) . ? C67 C68 1.400(14) . ? C69 C70 1.336(13) . ? C69 C74 1.381(15) . ? C70 C71 1.386(15) . ? C71 C72 1.411(17) . ? C72 C73 1.314(19) . ? C73 C74 1.341(17) . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? C51' C52' 1.3900 . ? C51' C56' 1.3900 . ? C52' C53' 1.3900 . ? C53' C54' 1.3900 . ? C54' C55' 1.3900 . ? C55' C56' 1.3900 . ? C1S Cl1S 1.68(3) . ? C1S Cl2S 1.73(2) . ? C1S Cl3S 1.85(3) . ? O1W C1W 1.427(10) . ? C1W C2W 1.538(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 O4 Au1 P2 172.69(18) . . ? O1 C1 C10 117.4(6) . . ? O1 C1 C2 118.3(7) . . ? C10 C1 C2 124.0(8) . . ? C1 O1 P1 121.3(6) . . ? O3 P1 O4 118.4(4) . . ? O3 P1 O1 113.4(4) . . ? O4 P1 O1 103.6(4) . . ? O3 P1 O2 107.1(4) . . ? O4 P1 O2 109.7(3) . . ? O1 P1 O2 103.9(3) . . ? C21 Si1 C27 111.0(4) . . ? C21 Si1 C2 107.0(4) . . ? C27 Si1 C2 108.1(4) . . ? C21 Si1 C33 106.3(4) . . ? C27 Si1 C33 111.6(4) . . ? C2 Si1 C33 112.8(4) . . ? C3 C2 C1 115.7(7) . . ? C3 C2 Si1 120.3(6) . . ? C1 C2 Si1 123.9(7) . . ? C20 O2 P1 119.1(6) . . ? C63 P2 C57 107.5(5) . . ? C63 P2 C69 103.7(4) . . ? C57 P2 C69 106.0(4) . . ? C63 P2 Au1 110.1(4) . . ? C57 P2 Au1 111.4(4) . . ? C69 P2 Au1 117.4(3) . . ? C51 Si2 C45 116.5(14) . . ? C51 Si2 C19 117.9(16) . . ? C45 Si2 C19 108.1(14) . . ? C51 Si2 C39 100.5(14) . . ? C45 Si2 C39 107.5(15) . . ? C19 Si2 C39 104.8(12) . . ? C45' Si2' C39' 112.7(18) . . ? C45' Si2' C19 106.5(15) . . ? C39' Si2' C19 110.5(15) . . ? C45' Si2' C51' 111.4(15) . . ? C39' Si2' C51' 103.7(16) . . ? C19 Si2' C51' 112.2(17) . . ? C2 C3 C4 124.5(8) . . ? C5 C4 C9 120.9(8) . . ? C5 C4 C3 122.3(8) . . ? C9 C4 C3 116.8(8) . . ? P1 O4 Au1 120.8(4) . . ? C6 C5 C4 120.8(8) . . ? C5 C6 C7 118.6(9) . . ? C8 C7 C6 122.8(8) . . ? C7 C8 C9 119.6(8) . . ? C10 C9 C4 120.9(8) . . ? C10 C9 C8 121.8(8) . . ? C4 C9 C8 117.2(8) . . ? C1 C10 C9 117.4(7) . . ? C1 C10 C11 120.8(8) . . ? C9 C10 C11 121.7(7) . . ? C20 C11 C12 119.9(8) . . ? C20 C11 C10 119.9(8) . . ? C12 C11 C10 119.8(8) . . ? C13 C12 C11 123.9(8) . . ? C13 C12 C17 118.3(8) . . ? C11 C12 C17 117.8(8) . . ? C14 C13 C12 122.3(9) . . ? C13 C14 C15 119.4(10) . . ? C16 C15 C14 119.7(9) . . ? C15 C16 C17 121.5(8) . . ? C16 C17 C18 121.9(8) . . ? C16 C17 C12 118.7(8) . . ? C18 C17 C12 119.4(8) . . ? C19 C18 C17 122.8(8) . . ? C18 C19 C20 116.4(8) . . ? C18 C19 Si2' 113.7(10) . . ? C20 C19 Si2' 129.8(10) . . ? C18 C19 Si2 117.9(10) . . ? C20 C19 Si2 125.2(10) . . ? Si2' C19 Si2 8.8(14) . . ? C11 C20 O2 119.8(8) . . ? C11 C20 C19 122.6(8) . . ? O2 C20 C19 117.5(8) . . ? C26 C21 C22 115.9(9) . . ? C26 C21 Si1 121.6(6) . . ? C22 C21 Si1 122.2(7) . . ? C23 C22 C21 121.0(9) . . ? C22 C23 C24 122.7(8) . . ? C25 C24 C23 116.8(10) . . ? C24 C25 C26 120.8(10) . . ? C25 C26 C21 122.6(8) . . ? C32 C27 C28 117.4(9) . . ? C32 C27 Si1 121.8(6) . . ? C28 C27 Si1 120.8(7) . . ? C29 C28 C27 120.2(9) . . ? C28 C29 C30 120.9(9) . . ? C31 C30 C29 119.2(9) . . ? C30 C31 C32 120.6(9) . . ? C31 C32 C27 121.7(8) . . ? C34 C33 C38 117.3(9) . . ? C34 C33 Si1 121.3(8) . . ? C38 C33 Si1 121.4(8) . . ? C33 C34 C35 122.1(10) . . ? C34 C35 C36 118.9(9) . . ? C37 C36 C35 119.5(10) . . ? C38 C37 C36 119.8(10) . . ? C37 C38 C33 122.4(10) . . ? C40 C39 C44 120.0 . . ? C40 C39 Si2 123.8(12) . . ? C44 C39 Si2 116.1(12) . . ? C41 C40 C39 120.0 . . ? C42 C41 C40 120.0 . . ? C41 C42 C43 120.0 . . ? C44 C43 C42 120.0 . . ? C43 C44 C39 120.0 . . ? C40' C39' C44' 120.0 . . ? C40' C39' Si2' 118.3(14) . . ? C44' C39' Si2' 121.0(14) . . ? C39' C40' C41' 120.0 . . ? C42' C41' C40' 120.0 . . ? C43' C42' C41' 120.0 . . ? C42' C43' C44' 120.0 . . ? C43' C44' C39' 120.0 . . ? C46' C45' C50' 120.0 . . ? C46' C45' Si2' 116.4(13) . . ? C50' C45' Si2' 123.5(13) . . ? C45' C46' C47' 120.0 . . ? C48' C47' C46' 120.0 . . ? C49' C48' C47' 120.0 . . ? C48' C49' C50' 120.0 . . ? C49' C50' C45' 120.0 . . ? C46 C45 C50 120.0 . . ? C46 C45 Si2 122.4(10) . . ? C50 C45 Si2 117.6(10) . . ? C47 C46 C45 120.0 . . ? C46 C47 C48 120.0 . . ? C49 C48 C47 120.0 . . ? C50 C49 C48 120.0 . . ? C49 C50 C45 120.0 . . ? C62 C57 C58 118.7(10) . . ? C62 C57 P2 124.2(9) . . ? C58 C57 P2 117.0(8) . . ? C59 C58 C57 121.4(12) . . ? C58 C59 C60 118.3(12) . . ? C61 C60 C59 120.5(10) . . ? C62 C61 C60 120.6(12) . . ? C57 C62 C61 120.4(12) . . ? C64 C63 C68 117.9(10) . . ? C64 C63 P2 122.4(9) . . ? C68 C63 P2 119.4(8) . . ? C63 C64 C65 122.3(12) . . ? C64 C65 C66 118.5(12) . . ? C67 C66 C65 119.7(11) . . ? C66 C67 C68 120.7(10) . . ? C63 C68 C67 120.6(9) . . ? C70 C69 C74 117.9(10) . . ? C70 C69 P2 124.0(8) . . ? C74 C69 P2 118.1(8) . . ? C69 C70 C71 123.0(10) . . ? C70 C71 C72 117.1(11) . . ? C73 C72 C71 118.4(10) . . ? C72 C73 C74 123.9(12) . . ? C73 C74 C69 119.7(12) . . ? C52 C51 C56 120.0 . . ? C52 C51 Si2 119.9(12) . . ? C56 C51 Si2 117.4(12) . . ? C53 C52 C51 120.0 . . ? C54 C53 C52 120.0 . . ? C53 C54 C55 120.0 . . ? C56 C55 C54 120.0 . . ? C55 C56 C51 120.0 . . ? C52' C51' C56' 120.0 . . ? C52' C51' Si2' 121.7(11) . . ? C56' C51' Si2' 118.2(11) . . ? C53' C52' C51' 120.0 . . ? C52' C53' C54' 120.0 . . ? C55' C54' C53' 120.0 . . ? C54' C55' C56' 120.0 . . ? C55' C56' C51' 120.0 . . ? Cl1S C1S Cl2S 114.5(15) . . ? Cl1S C1S Cl3S 109.1(13) . . ? Cl2S C1S Cl3S 107.2(14) . . ? O1W C1W C2W 97(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 C1 O1 P1 69.8(10) . . . . ? C2 C1 O1 P1 -115.0(8) . . . . ? C1 O1 P1 O3 67.3(7) . . . . ? C1 O1 P1 O4 -163.2(6) . . . . ? C1 O1 P1 O2 -48.6(7) . . . . ? O1 C1 C2 C3 178.6(8) . . . . ? C10 C1 C2 C3 -6.6(15) . . . . ? O1 C1 C2 Si1 -5.6(13) . . . . ? C10 C1 C2 Si1 169.3(8) . . . . ? C21 Si1 C2 C3 30.3(9) . . . . ? C27 Si1 C2 C3 -89.4(9) . . . . ? C33 Si1 C2 C3 146.8(8) . . . . ? C21 Si1 C2 C1 -145.4(8) . . . . ? C27 Si1 C2 C1 95.0(8) . . . . ? C33 Si1 C2 C1 -28.9(10) . . . . ? O3 P1 O2 C20 -162.4(6) . . . . ? O4 P1 O2 C20 68.0(7) . . . . ? O1 P1 O2 C20 -42.2(7) . . . . ? O4 Au1 P2 C63 43.0(15) . . . . ? O4 Au1 P2 C57 -76.2(15) . . . . ? O4 Au1 P2 C69 161.3(14) . . . . ? C1 C2 C3 C4 0.0(15) . . . . ? Si1 C2 C3 C4 -176.0(7) . . . . ? C2 C3 C4 C5 -179.7(10) . . . . ? C2 C3 C4 C9 2.2(14) . . . . ? O3 P1 O4 Au1 154.8(4) . . . . ? O1 P1 O4 Au1 28.4(4) . . . . ? O2 P1 O4 Au1 -82.0(5) . . . . ? P2 Au1 O4 P1 -53.6(16) . . . . ? C9 C4 C5 C6 0.2(15) . . . . ? C3 C4 C5 C6 -177.9(9) . . . . ? C4 C5 C6 C7 -1.9(15) . . . . ? C5 C6 C7 C8 2.1(16) . . . . ? C6 C7 C8 C9 -0.6(16) . . . . ? C5 C4 C9 C10 -176.3(9) . . . . ? C3 C4 C9 C10 1.9(13) . . . . ? C5 C4 C9 C8 1.2(14) . . . . ? C3 C4 C9 C8 179.4(9) . . . . ? C7 C8 C9 C10 176.4(9) . . . . ? C7 C8 C9 C4 -1.0(15) . . . . ? O1 C1 C10 C9 -174.6(8) . . . . ? C2 C1 C10 C9 10.5(15) . . . . ? O1 C1 C10 C11 7.6(14) . . . . ? C2 C1 C10 C11 -167.3(9) . . . . ? C4 C9 C10 C1 -7.8(14) . . . . ? C8 C9 C10 C1 174.8(9) . . . . ? C4 C9 C10 C11 169.9(9) . . . . ? C8 C9 C10 C11 -7.5(15) . . . . ? C1 C10 C11 C20 -55.6(13) . . . . ? C9 C10 C11 C20 126.8(10) . . . . ? C1 C10 C11 C12 117.2(10) . . . . ? C9 C10 C11 C12 -60.5(12) . . . . ? C20 C11 C12 C13 170.2(8) . . . . ? C10 C11 C12 C13 -2.6(13) . . . . ? C20 C11 C12 C17 -11.3(12) . . . . ? C10 C11 C12 C17 175.9(8) . . . . ? C11 C12 C13 C14 177.6(9) . . . . ? C17 C12 C13 C14 -0.9(13) . . . . ? C12 C13 C14 C15 -0.4(14) . . . . ? C13 C14 C15 C16 2.1(14) . . . . ? C14 C15 C16 C17 -2.6(14) . . . . ? C15 C16 C17 C18 178.8(9) . . . . ? C15 C16 C17 C12 1.3(13) . . . . ? C13 C12 C17 C16 0.5(12) . . . . ? C11 C12 C17 C16 -178.1(8) . . . . ? C13 C12 C17 C18 -177.1(8) . . . . ? C11 C12 C17 C18 4.3(12) . . . . ? C16 C17 C18 C19 -175.4(9) . . . . ? C12 C17 C18 C19 2.1(13) . . . . ? C17 C18 C19 C20 -1.4(13) . . . . ? C17 C18 C19 Si2' 179.7(12) . . . . ? C17 C18 C19 Si2 171.1(11) . . . . ? C45' Si2' C19 C18 -107.1(13) . . . . ? C39' Si2' C19 C18 16(2) . . . . ? C51' Si2' C19 C18 130.8(12) . . . . ? C45' Si2' C19 C20 74.2(19) . . . . ? C39' Si2' C19 C20 -163.1(12) . . . . ? C51' Si2' C19 C20 -47.9(19) . . . . ? C45' Si2' C19 Si2 13(10) . . . . ? C39' Si2' C19 Si2 135(12) . . . . ? C51' Si2' C19 Si2 -109(11) . . . . ? C51 Si2 C19 C18 142.4(11) . . . . ? C45 Si2 C19 C18 -82.7(12) . . . . ? C39 Si2 C19 C18 31.7(18) . . . . ? C51 Si2 C19 C20 -45.8(18) . . . . ? C45 Si2 C19 C20 89.1(15) . . . . ? C39 Si2 C19 C20 -156.5(11) . . . . ? C51 Si2 C19 Si2' 79(11) . . . . ? C45 Si2 C19 Si2' -147(12) . . . . ? C39 Si2 C19 Si2' -32(10) . . . . ? C12 C11 C20 O2 -171.6(7) . . . . ? C10 C11 C20 O2 1.1(12) . . . . ? C12 C11 C20 C19 12.5(13) . . . . ? C10 C11 C20 C19 -174.7(8) . . . . ? P1 O2 C20 C11 70.3(9) . . . . ? P1 O2 C20 C19 -113.7(8) . . . . ? C18 C19 C20 C11 -5.9(13) . . . . ? Si2' C19 C20 C11 172.7(13) . . . . ? Si2 C19 C20 C11 -177.8(12) . . . . ? C18 C19 C20 O2 178.2(7) . . . . ? Si2' C19 C20 O2 -3.2(17) . . . . ? Si2 C19 C20 O2 6.3(15) . . . . ? C27 Si1 C21 C26 160.7(8) . . . . ? C2 Si1 C21 C26 43.0(9) . . . . ? C33 Si1 C21 C26 -77.8(8) . . . . ? C27 Si1 C21 C22 -25.4(9) . . . . ? C2 Si1 C21 C22 -143.2(8) . . . . ? C33 Si1 C21 C22 96.1(8) . . . . ? C26 C21 C22 C23 3.2(14) . . . . ? Si1 C21 C22 C23 -171.0(8) . . . . ? C21 C22 C23 C24 -2.9(16) . . . . ? C22 C23 C24 C25 0.6(17) . . . . ? C23 C24 C25 C26 1.2(18) . . . . ? C24 C25 C26 C21 -0.8(18) . . . . ? C22 C21 C26 C25 -1.4(15) . . . . ? Si1 C21 C26 C25 172.9(9) . . . . ? C21 Si1 C27 C32 -118.4(8) . . . . ? C2 Si1 C27 C32 -1.3(9) . . . . ? C33 Si1 C27 C32 123.2(8) . . . . ? C21 Si1 C27 C28 61.7(8) . . . . ? C2 Si1 C27 C28 178.8(7) . . . . ? C33 Si1 C27 C28 -56.6(8) . . . . ? C32 C27 C28 C29 2.2(13) . . . . ? Si1 C27 C28 C29 -178.0(8) . . . . ? C27 C28 C29 C30 -0.1(15) . . . . ? C28 C29 C30 C31 -0.9(16) . . . . ? C29 C30 C31 C32 -0.3(15) . . . . ? C30 C31 C32 C27 2.5(15) . . . . ? C28 C27 C32 C31 -3.4(14) . . . . ? Si1 C27 C32 C31 176.8(8) . . . . ? C21 Si1 C33 C34 -150.6(6) . . . . ? C27 Si1 C33 C34 -29.4(7) . . . . ? C2 Si1 C33 C34 92.5(7) . . . . ? C21 Si1 C33 C38 30.3(7) . . . . ? C27 Si1 C33 C38 151.4(6) . . . . ? C2 Si1 C33 C38 -86.7(7) . . . . ? C38 C33 C34 C35 -0.7(11) . . . . ? Si1 C33 C34 C35 -179.8(6) . . . . ? C33 C34 C35 C36 0.4(12) . . . . ? C34 C35 C36 C37 -0.7(13) . . . . ? C35 C36 C37 C38 1.2(13) . . . . ? C36 C37 C38 C33 -1.5(12) . . . . ? C34 C33 C38 C37 1.2(11) . . . . ? Si1 C33 C38 C37 -179.6(6) . . . . ? C51 Si2 C39 C40 104.6(14) . . . . ? C45 Si2 C39 C40 -18(2) . . . . ? C19 Si2 C39 C40 -132.6(12) . . . . ? C51 Si2 C39 C44 -71.8(16) . . . . ? C45 Si2 C39 C44 165.9(12) . . . . ? C19 Si2 C39 C44 51.0(18) . . . . ? C44 C39 C40 C41 0.0 . . . . ? Si2 C39 C40 C41 -176.3(17) . . . . ? C39 C40 C41 C42 0.0 . . . . ? C40 C41 C42 C43 0.0 . . . . ? C41 C42 C43 C44 0.0 . . . . ? C42 C43 C44 C39 0.0 . . . . ? C40 C39 C44 C43 0.0 . . . . ? Si2 C39 C44 C43 176.6(16) . . . . ? C45' Si2' C39' C40' -11(2) . . . . ? C19 Si2' C39' C40' -130.4(14) . . . . ? C51' Si2' C39' C40' 109.2(16) . . . . ? C45' Si2' C39' C44' 178.1(14) . . . . ? C19 Si2' C39' C44' 59(2) . . . . ? C51' Si2' C39' C44' -61(2) . . . . ? C44' C39' C40' C41' 0.0 . . . . ? Si2' C39' C40' C41' -170.5(19) . . . . ? C39' C40' C41' C42' 0.0 . . . . ? C40' C41' C42' C43' 0.0 . . . . ? C41' C42' C43' C44' 0.0 . . . . ? C42' C43' C44' C39' 0.0 . . . . ? C40' C39' C44' C43' 0.0 . . . . ? Si2' C39' C44' C43' 170(2) . . . . ? C39' Si2' C45' C46' -59(2) . . . . ? C19 Si2' C45' C46' 62.6(17) . . . . ? C51' Si2' C45' C46' -174.8(13) . . . . ? C39' Si2' C45' C50' 124.5(16) . . . . ? C19 Si2' C45' C50' -114.2(14) . . . . ? C51' Si2' C45' C50' 8(2) . . . . ? C50' C45' C46' C47' 0.0 . . . . ? Si2' C45' C46' C47' -176.9(16) . . . . ? C45' C46' C47' C48' 0.0 . . . . ? C46' C47' C48' C49' 0.0 . . . . ? C47' C48' C49' C50' 0.0 . . . . ? C48' C49' C50' C45' 0.0 . . . . ? C46' C45' C50' C49' 0.0 . . . . ? Si2' C45' C50' C49' 176.7(17) . . . . ? C51 Si2 C45 C46 -156.4(11) . . . . ? C19 Si2 C45 C46 68.0(14) . . . . ? C39 Si2 C45 C46 -44.7(19) . . . . ? C51 Si2 C45 C50 24.3(19) . . . . ? C19 Si2 C45 C50 -111.3(12) . . . . ? C39 Si2 C45 C50 136.1(12) . . . . ? C50 C45 C46 C47 0.0 . . . . ? Si2 C45 C46 C47 -179.2(14) . . . . ? C45 C46 C47 C48 0.0 . . . . ? C46 C47 C48 C49 0.0 . . . . ? C47 C48 C49 C50 0.0 . . . . ? C48 C49 C50 C45 0.0 . . . . ? C46 C45 C50 C49 0.0 . . . . ? Si2 C45 C50 C49 179.3(13) . . . . ? C63 P2 C57 C62 21.1(11) . . . . ? C69 P2 C57 C62 -89.4(10) . . . . ? Au1 P2 C57 C62 141.8(9) . . . . ? C63 P2 C57 C58 -159.6(7) . . . . ? C69 P2 C57 C58 90.0(8) . . . . ? Au1 P2 C57 C58 -38.9(8) . . . . ? C62 C57 C58 C59 -3.0(15) . . . . ? P2 C57 C58 C59 177.6(9) . . . . ? C57 C58 C59 C60 3.5(16) . . . . ? C58 C59 C60 C61 -3.9(18) . . . . ? C59 C60 C61 C62 3.9(19) . . . . ? C58 C57 C62 C61 2.8(16) . . . . ? P2 C57 C62 C61 -177.9(9) . . . . ? C60 C61 C62 C57 -3.3(19) . . . . ? C57 P2 C63 C64 -74.1(11) . . . . ? C69 P2 C63 C64 38.0(11) . . . . ? Au1 P2 C63 C64 164.4(9) . . . . ? C57 P2 C63 C68 100.6(8) . . . . ? C69 P2 C63 C68 -147.4(8) . . . . ? Au1 P2 C63 C68 -21.0(8) . . . . ? C68 C63 C64 C65 5.5(19) . . . . ? P2 C63 C64 C65 -179.7(10) . . . . ? C63 C64 C65 C66 -4(2) . . . . ? C64 C65 C66 C67 1.2(18) . . . . ? C65 C66 C67 C68 0.8(16) . . . . ? C64 C63 C68 C67 -3.5(15) . . . . ? P2 C63 C68 C67 -178.4(7) . . . . ? C66 C67 C68 C63 0.4(15) . . . . ? C63 P2 C69 C70 -116.9(9) . . . . ? C57 P2 C69 C70 -3.9(10) . . . . ? Au1 P2 C69 C70 121.4(8) . . . . ? C63 P2 C69 C74 61.3(10) . . . . ? C57 P2 C69 C74 174.4(10) . . . . ? Au1 P2 C69 C74 -60.4(10) . . . . ? C74 C69 C70 C71 1.6(17) . . . . ? P2 C69 C70 C71 179.8(9) . . . . ? C69 C70 C71 C72 -3.2(18) . . . . ? C70 C71 C72 C73 4(2) . . . . ? C71 C72 C73 C74 -4(2) . . . . ? C72 C73 C74 C69 2(3) . . . . ? C70 C69 C74 C73 -1(2) . . . . ? P2 C69 C74 C73 -179.3(12) . . . . ? C45 Si2 C51 C52 -149.3(12) . . . . ? C19 Si2 C51 C52 -18.1(16) . . . . ? C39 Si2 C51 C52 95.0(14) . . . . ? C45 Si2 C51 C56 49.3(16) . . . . ? C19 Si2 C51 C56 -179.5(9) . . . . ? C39 Si2 C51 C56 -66.4(14) . . . . ? C56 C51 C52 C53 0.0 . . . . ? Si2 C51 C52 C53 -160.9(12) . . . . ? C51 C52 C53 C54 0.0 . . . . ? C52 C53 C54 C55 0.0 . . . . ? C53 C54 C55 C56 0.0 . . . . ? C54 C55 C56 C51 0.0 . . . . ? C52 C51 C56 C55 0.0 . . . . ? Si2 C51 C56 C55 161.4(11) . . . . ? C45' Si2' C51' C52' -54(2) . . . . ? C39' Si2' C51' C52' -175.9(13) . . . . ? C19 Si2' C51' C52' 64.8(18) . . . . ? C45' Si2' C51' C56' 123.2(14) . . . . ? C39' Si2' C51' C56' 2(2) . . . . ? C19 Si2' C51' C56' -117.5(13) . . . . ? C56' C51' C52' C53' 0.0 . . . . ? Si2' C51' C52' C53' 177.6(18) . . . . ? C51' C52' C53' C54' 0.0 . . . . ? C52' C53' C54' C55' 0.0 . . . . ? C53' C54' C55' C56' 0.0 . . . . ? C54' C55' C56' C51' 0.0 . . . . ? C52' C51' C56' C55' 0.0 . . . . ? Si2' C51' C56' C55' -177.7(17) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.45 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.908 _refine_diff_density_min -1.288 _refine_diff_density_rms 0.146 # Attachment 'web_deposit_cif_file_1_AntonioM.Echavarren_1314183768.MR502b_0mX.cif' data_mr502b_0m _database_code_depnum_ccdc_archive 'CCDC 841518' #TrackingRef 'web_deposit_cif_file_1_AntonioM.Echavarren_1314183768.MR502b_0mX.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H66 Au O7.50 P2 Si2' _chemical_formula_weight 1414.37 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' 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.7382(12) _cell_length_b 14.4403(14) _cell_length_c 40.493(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6863.7(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9954 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 26.99 _exptl_crystal_description Needle _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2876 _exptl_absorpt_coefficient_mu 2.279 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.67 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 70 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 39386 _diffrn_reflns_av_R_equivalents 0.0658 _diffrn_reflns_av_sigmaI/netI 0.0652 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -50 _diffrn_reflns_limit_l_max 51 _diffrn_reflns_theta_min 1.01 _diffrn_reflns_theta_max 26.86 _reflns_number_total 12587 _reflns_number_gt 11714 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmetric unit is made up of two methanol molecules disordered in four positions as well as 1.5 water molecules in three positions. ; _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^)+(0.0739P)^2^+20.6075P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _chemical_absolute_configuration ad _refine_ls_abs_structure_Flack 0.028(7) _refine_ls_number_reflns 12587 _refine_ls_number_parameters 904 _refine_ls_number_restraints 215 _refine_ls_R_factor_all 0.0644 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1464 _refine_ls_wR_factor_gt 0.1424 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.139 _refine_ls_shift/su_max 0.033 _refine_ls_shift/su_mean 0.001 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 0.668480(13) 0.764760(12) 0.097829(3) 0.01969(3) Uani 1 1 d . . . C1 C 0.7100(4) 0.9677(4) 0.13545(11) 0.0302(13) Uani 1 1 d . . . C2 C 0.6535(4) 0.9206(4) 0.16162(10) 0.0297(13) Uani 1 1 d . . . H2A H 0.6156 0.8635 0.1576 0.036 Uiso 1 1 calc R . . C3 C 0.6545(4) 0.9601(4) 0.19388(11) 0.0335(14) Uani 1 1 d . . . H3A H 0.6178 0.9290 0.2116 0.040 Uiso 1 1 calc R . . C4 C 0.7085(4) 1.0434(4) 0.19945(12) 0.0360(15) Uani 1 1 d . . . H4A H 0.7072 1.0701 0.2209 0.043 Uiso 1 1 calc R . . C5 C 0.7650(5) 1.0888(5) 0.17389(13) 0.0489(18) Uani 1 1 d . . . H5A H 0.8032 1.1457 0.1779 0.059 Uiso 1 1 calc R . . C6 C 0.7651(6) 1.0498(5) 0.14243(13) 0.0531(19) Uani 1 1 d . . . H6A H 0.8044 1.0808 0.1252 0.064 Uiso 1 1 calc R . . C7 C 0.5914(4) 0.9755(4) 0.07150(11) 0.0256(12) Uani 1 1 d . . . C8 C 0.5359(4) 0.9269(4) 0.04502(10) 0.0290(13) Uani 1 1 d . . . H8A H 0.5573 0.8653 0.0395 0.035 Uiso 1 1 calc R . . C9 C 0.4499(4) 0.9724(4) 0.02764(11) 0.0355(15) Uani 1 1 d . . . H9A H 0.4131 0.9409 0.0100 0.043 Uiso 1 1 calc R . . C10 C 0.4167(4) 1.0603(5) 0.03496(13) 0.0427(17) Uani 1 1 d . . . H10A H 0.3592 1.0895 0.0222 0.051 Uiso 1 1 calc R . . C11 C 0.4695(5) 1.1095(5) 0.06235(16) 0.059(2) Uani 1 1 d . . . H11A H 0.4445 1.1697 0.0685 0.071 Uiso 1 1 calc R . . C12 C 0.5579(5) 1.0657(5) 0.07931(13) 0.0451(16) Uani 1 1 d . . . H12A H 0.5961 1.0979 0.0965 0.054 Uiso 1 1 calc R . . C13 C 0.8383(4) 0.9514(3) 0.07401(10) 0.0253(11) Uani 1 1 d . . . C14 C 0.9375(4) 0.9246(5) 0.08870(13) 0.0412(16) Uani 1 1 d . . . H14A H 0.9351 0.8882 0.1082 0.049 Uiso 1 1 calc R . . C15 C 1.0455(4) 0.9509(5) 0.07498(15) 0.0414(17) Uani 1 1 d . . . H15A H 1.1149 0.9327 0.0851 0.050 Uiso 1 1 calc R . . C16 C 1.0452(5) 1.0047(5) 0.04597(15) 0.0462(18) Uani 1 1 d . . . H16A H 1.1155 1.0225 0.0363 0.055 Uiso 1 1 calc R . . C17 C 0.9439(4) 1.0321(4) 0.03137(12) 0.0354(15) Uani 1 1 d . . . H17A H 0.9450 1.0683 0.0118 0.043 Uiso 1 1 calc R . . C18 C 0.8412(4) 1.0065(4) 0.04541(11) 0.0305(13) Uani 1 1 d . . . H18A H 0.7718 1.0264 0.0356 0.037 Uiso 1 1 calc R . . C19 C 0.6232(3) 0.6686(3) 0.19853(9) 0.0147(10) Uani 1 1 d . . . C20 C 0.5323(3) 0.6754(3) 0.22180(9) 0.0171(11) Uani 1 1 d . . . C21 C 0.5592(3) 0.6681(3) 0.25504(10) 0.0175(10) Uani 1 1 d . . . H21A H 0.4999 0.6709 0.2710 0.021 Uiso 1 1 calc R . . C22 C 0.6746(4) 0.6565(3) 0.26580(9) 0.0210(10) Uani 1 1 d . . . C23 C 0.7018(3) 0.6452(4) 0.30069(10) 0.0243(13) Uani 1 1 d . . . H23A H 0.6421 0.6437 0.3165 0.029 Uiso 1 1 calc R . . C24 C 0.8135(3) 0.6365(4) 0.31090(10) 0.0261(12) Uani 1 1 d . . . H24A H 0.8307 0.6322 0.3338 0.031 Uiso 1 1 calc R . . C25 C 0.9030(3) 0.6341(4) 0.28716(10) 0.0220(12) Uani 1 1 d . . . H25A H 0.9795 0.6266 0.2943 0.026 Uiso 1 1 calc R . . C26 C 0.8800(3) 0.6423(3) 0.25379(10) 0.0187(11) Uani 1 1 d . . . H26A H 0.9407 0.6391 0.2383 0.022 Uiso 1 1 calc R . . C27 C 0.7652(3) 0.6558(3) 0.24228(9) 0.0143(10) Uani 1 1 d . . . C28 C 0.7362(3) 0.6671(3) 0.20761(9) 0.0159(10) Uani 1 1 d . . . C29 C 0.8278(3) 0.6801(3) 0.18164(8) 0.0153(9) Uani 1 1 d . . . C30 C 0.9089(3) 0.7559(3) 0.18466(8) 0.0162(10) Uani 1 1 d . . . C31 C 0.9009(3) 0.8258(4) 0.20964(10) 0.0201(11) Uani 1 1 d . . . H31A H 0.8405 0.8237 0.2252 0.024 Uiso 1 1 calc R . . C32 C 0.9790(3) 0.8951(3) 0.21119(10) 0.0195(8) Uani 1 1 d U . . H32A H 0.9714 0.9414 0.2277 0.023 Uiso 1 1 calc R . . C33 C 1.0714(3) 0.9000(3) 0.18876(10) 0.0189(7) Uani 1 1 d U . . H33A H 1.1269 0.9475 0.1908 0.023 Uiso 1 1 calc R . . C34 C 1.0798(3) 0.8349(3) 0.16377(10) 0.0191(8) Uani 1 1 d U . . H34A H 1.1407 0.8385 0.1484 0.023 Uiso 1 1 calc R . . C35 C 0.9979(3) 0.7625(3) 0.16103(8) 0.0149(9) Uani 1 1 d . . . C36 C 1.0033(3) 0.6973(3) 0.13442(9) 0.0164(10) Uani 1 1 d . . . H36A H 1.0646 0.7020 0.1192 0.020 Uiso 1 1 calc R . . C37 C 0.9239(3) 0.6278(3) 0.12974(9) 0.0178(11) Uani 1 1 d . A . C38 C 0.8358(3) 0.6223(3) 0.15365(8) 0.0156(9) Uani 1 1 d . . . C39 C 0.3645(3) 0.7731(4) 0.17050(9) 0.0175(10) Uani 1 1 d . . . C40 C 0.3525(3) 0.7286(4) 0.13895(10) 0.0255(12) Uani 1 1 d . . . H40A H 0.3491 0.6630 0.1379 0.031 Uiso 1 1 calc R . . C41 C 0.3456(3) 0.7820(4) 0.10896(10) 0.0304(13) Uani 1 1 d . . . H41A H 0.3397 0.7522 0.0881 0.036 Uiso 1 1 calc R . . C42 C 0.3477(3) 0.8793(4) 0.11124(11) 0.0320(13) Uani 1 1 d . . . H42A H 0.3418 0.9159 0.0918 0.038 Uiso 1 1 calc R . . C43 C 0.3586(3) 0.9229(4) 0.14260(13) 0.0315(14) Uani 1 1 d . . . H43A H 0.3615 0.9885 0.1440 0.038 Uiso 1 1 calc R . . C44 C 0.3651(3) 0.8697(4) 0.17136(11) 0.0224(12) Uani 1 1 d . . . H44A H 0.3700 0.9002 0.1921 0.027 Uiso 1 1 calc R . . C45 C 0.3108(3) 0.7707(3) 0.24443(8) 0.0166(10) Uani 1 1 d . . . C46 C 0.3728(4) 0.8452(4) 0.25887(11) 0.0273(13) Uani 1 1 d . . . H46A H 0.4502 0.8542 0.2528 0.033 Uiso 1 1 calc R . . C47 C 0.3225(4) 0.9058(4) 0.28182(12) 0.0363(13) Uani 1 1 d . . . H47A H 0.3653 0.9557 0.2907 0.044 Uiso 1 1 calc R . . C48 C 0.2092(4) 0.8923(4) 0.29151(13) 0.0355(15) Uani 1 1 d . . . H48A H 0.1743 0.9329 0.3069 0.043 Uiso 1 1 calc R . . C49 C 0.1480(3) 0.8181(4) 0.27813(10) 0.0273(13) Uani 1 1 d . . . H49A H 0.0718 0.8076 0.2851 0.033 Uiso 1 1 calc R . . C50 C 0.1966(3) 0.7597(4) 0.25499(9) 0.0191(11) Uani 1 1 d . . . H50A H 0.1521 0.7109 0.2459 0.023 Uiso 1 1 calc R . . C51 C 0.2999(3) 0.5843(3) 0.20544(9) 0.0168(11) Uani 1 1 d . . . C52 C 0.1821(4) 0.5794(3) 0.19802(9) 0.0208(11) Uani 1 1 d . . . H52A H 0.1420 0.6350 0.1933 0.025 Uiso 1 1 calc R . . C53 C 0.1230(4) 0.4954(4) 0.19741(10) 0.0259(13) Uani 1 1 d . . . H53A H 0.0434 0.4944 0.1932 0.031 Uiso 1 1 calc R . . C54 C 0.1823(4) 0.4127(4) 0.20313(10) 0.0289(12) Uani 1 1 d . . . H54A H 0.1431 0.3552 0.2024 0.035 Uiso 1 1 calc R . . C55 C 0.2985(4) 0.4147(4) 0.20990(12) 0.0302(14) Uani 1 1 d . . . H55A H 0.3390 0.3587 0.2137 0.036 Uiso 1 1 calc R . . C56 C 0.3557(3) 0.5009(4) 0.21111(11) 0.0239(12) Uani 1 1 d . . . H56A H 0.4349 0.5019 0.2160 0.029 Uiso 1 1 calc R . . C57 C 0.8615(4) 0.6199(4) 0.05550(10) 0.0285(13) Uani 1 1 d . A . C58 C 0.7571(4) 0.5894(5) 0.04250(11) 0.0372(16) Uani 1 1 d . . . H58A H 0.7235 0.5340 0.0506 0.045 Uiso 1 1 calc R . . C59 C 0.7017(4) 0.6408(5) 0.01742(12) 0.0438(18) Uani 1 1 d . . . H59A H 0.6302 0.6198 0.0094 0.053 Uiso 1 1 calc R . . C60 C 0.7492(5) 0.7215(5) 0.00411(14) 0.0529(19) Uani 1 1 d . . . H60A H 0.7126 0.7543 -0.0132 0.063 Uiso 1 1 calc R . . C61 C 0.8518(5) 0.7517(5) 0.01722(13) 0.0490(18) Uani 1 1 d . . . H61A H 0.8856 0.8066 0.0088 0.059 Uiso 1 1 calc R . . C62 C 0.9069(4) 0.7033(4) 0.04264(11) 0.0310(14) Uani 1 1 d . . . H62A H 0.9760 0.7270 0.0514 0.037 Uiso 1 1 calc R . . C63 C 1.0989(3) 0.5527(4) 0.08025(10) 0.0229(12) Uani 1 1 d . A . C64 C 1.1486(5) 0.5695(4) 0.04923(10) 0.0361(15) Uani 1 1 d . . . H64A H 1.1012 0.5889 0.0315 0.043 Uiso 1 1 calc R . . C65 C 1.2622(4) 0.5588(4) 0.04369(12) 0.0387(15) Uani 1 1 d . . . H65A H 1.2919 0.5692 0.0222 0.046 Uiso 1 1 calc R . . C66 C 1.3361(4) 0.5326(4) 0.06921(14) 0.0451(16) Uani 1 1 d . . . H66A H 1.4158 0.5281 0.0655 0.054 Uiso 1 1 calc R . . C67 C 1.2900(4) 0.5134(4) 0.09984(16) 0.0437(16) Uani 1 1 d . . . H67A H 1.3383 0.4921 0.1171 0.052 Uiso 1 1 calc R . . C68 C 1.1730(4) 0.5248(4) 0.10602(10) 0.0308(13) Uani 1 1 d . . . H68A H 1.1436 0.5138 0.1275 0.037 Uiso 1 1 calc R . . C69 C 0.8990(2) 0.42858(11) 0.09042(7) 0.0240(16) Uani 0.40 1 d PGDU A 1 C70 C 0.8928(3) 0.3840(2) 0.06005(8) 0.0379(17) Uani 0.40 1 d PGU A 1 H70A H 0.8923 0.4193 0.0402 0.046 Uiso 0.40 1 calc PR A 1 C71 C 0.8874(4) 0.2880(2) 0.05866(12) 0.0268(16) Uani 0.40 1 d PGU A 1 H71A H 0.8832 0.2575 0.0379 0.032 Uiso 0.40 1 calc PR A 1 C72 C 0.8881(5) 0.23643(11) 0.08765(15) 0.0519(17) Uani 0.40 1 d PGU A 1 H72A H 0.8844 0.1708 0.0867 0.062 Uiso 0.40 1 calc PR A 1 C73 C 0.8942(5) 0.28097(19) 0.11803(12) 0.0496(17) Uani 0.40 1 d PGU A 1 H73A H 0.8947 0.2458 0.1378 0.059 Uiso 0.40 1 calc PR A 1 C74 C 0.8997(4) 0.3770(2) 0.11942(8) 0.0312(16) Uani 0.40 1 d PGU A 1 H74A H 0.9039 0.4075 0.1402 0.037 Uiso 0.40 1 calc PR A 1 C69' C 0.8796(2) 0.43340(11) 0.08649(8) 0.0191(16) Uani 0.30 1 d PGDU A 2 C70' C 0.9175(3) 0.3878(2) 0.05832(8) 0.0193(16) Uani 0.30 1 d PGU A 2 H70B H 0.9662 0.4187 0.0432 0.023 Uiso 0.30 1 calc PR A 2 C71' C 0.8839(5) 0.2970(2) 0.05230(11) 0.0375(17) Uani 0.30 1 d PGU A 2 H71B H 0.9098 0.2659 0.0330 0.045 Uiso 0.30 1 calc PR A 2 C72' C 0.8125(5) 0.2519(2) 0.07445(15) 0.0577(18) Uani 0.30 1 d PGU A 2 H72B H 0.7896 0.1898 0.0703 0.069 Uiso 0.30 1 calc PR A 2 C73' C 0.7747(4) 0.2975(2) 0.10262(15) 0.0534(18) Uani 0.30 1 d PGU A 2 H73B H 0.7259 0.2666 0.1178 0.064 Uiso 0.30 1 calc PR A 2 C74' C 0.8082(3) 0.3882(2) 0.10864(10) 0.0341(17) Uani 0.30 1 d PGU A 2 H74B H 0.7823 0.4194 0.1279 0.041 Uiso 0.30 1 calc PR A 2 C69" C 0.9151(2) 0.42730(11) 0.09578(8) 0.0269(17) Uani 0.30 1 d PGDU A 3 C70" C 0.9030(3) 0.37537(17) 0.06709(8) 0.0343(17) Uani 0.30 1 d PGU A 3 H70C H 0.8915 0.4056 0.0465 0.041 Uiso 0.30 1 calc PR A 3 C71" C 0.9079(4) 0.27927(16) 0.06851(12) 0.0459(18) Uani 0.30 1 d PGU A 3 H71C H 0.8997 0.2438 0.0489 0.055 Uiso 0.30 1 calc PR A 3 C72" C 0.9247(5) 0.23511(12) 0.09861(15) 0.0487(18) Uani 0.30 1 d PGU A 3 H72C H 0.9281 0.1694 0.0996 0.058 Uiso 0.30 1 calc PR A 3 C73" C 0.9368(5) 0.2870(2) 0.12730(12) 0.0348(17) Uani 0.30 1 d PGU A 3 H73C H 0.9483 0.2569 0.1479 0.042 Uiso 0.30 1 calc PR A 3 C74" C 0.9319(4) 0.3831(2) 0.12589(8) 0.0339(17) Uani 0.30 1 d PGU A 3 H74C H 0.9401 0.4186 0.1455 0.041 Uiso 0.30 1 calc PR A 3 O1 O 0.5957(2) 0.6739(2) 0.16463(7) 0.0189(8) Uani 1 1 d . . . O2 O 0.7479(2) 0.5549(2) 0.14957(7) 0.0173(7) Uani 1 1 d . . . O3 O 0.5453(2) 0.5048(2) 0.14703(7) 0.0237(8) Uani 1 1 d D . . O4 O 0.6182(2) 0.6270(2) 0.10595(6) 0.0179(8) Uani 1 1 d . . . P1 P 0.70334(9) 0.91554(9) 0.09431(3) 0.0228(3) Uani 1 1 d . . . P2 P 0.61970(8) 0.58645(9) 0.14019(2) 0.0167(3) Uani 1 1 d . . . Si1 Si 0.37574(9) 0.69963(9) 0.20957(3) 0.0161(3) Uani 1 1 d . . . Si2 Si 0.93911(9) 0.55614(8) 0.08971(3) 0.0200(3) Uani 1 1 d D . . C1R C 0.4812(2) 0.3513(10) 0.04527(11) 0.061(2) Uani 0.50 1 d PDU B 1 H1R1 H 0.4537 0.4147 0.0419 0.091 Uiso 0.50 1 calc PR B 1 H1R2 H 0.4201 0.3136 0.0548 0.091 Uiso 0.50 1 calc PRD B 1 H1R3 H 0.5046 0.3248 0.0240 0.091 Uiso 0.50 1 calc PR B 1 O1R O 0.5764(3) 0.3525(10) 0.06731(10) 0.103(2) Uani 0.50 1 d PDU B 1 H1R H 0.5540 0.3413 0.0866 0.154 Uiso 0.50 1 calc PRD B 1 O1M O 0.4708(3) 0.3022(4) 0.13913(14) 0.078(2) Uani 0.50 1 d PDU C 1 H1M H 0.4766 0.3526 0.1493 0.118 Uiso 0.50 1 calc PR C 1 C1M C 0.5627(4) 0.2429(5) 0.1482(3) 0.106(2) Uani 0.50 1 d PDU C 1 H1M1 H 0.6240 0.2484 0.1318 0.159 Uiso 0.50 1 calc PR C 1 H1M2 H 0.5358 0.1786 0.1489 0.159 Uiso 0.50 1 calc PR C 1 H1M3 H 0.5914 0.2607 0.1700 0.159 Uiso 0.50 1 calc PR C 1 O1N O 0.1888(6) 0.2141(2) 0.08266(11) 0.0490(14) Uani 0.50 1 d PDU D 1 H1N H 0.2202 0.2244 0.1009 0.074 Uiso 0.50 1 calc PR D 1 C1N C 0.2099(2) 0.2904(2) 0.06074(6) 0.0703(16) Uani 0.50 1 d PDU D 1 H1N1 H 0.1503 0.3373 0.0636 0.105 Uiso 0.50 1 calc PR D 1 H1N2 H 0.2094 0.2683 0.0379 0.105 Uiso 0.50 1 calc PR D 1 H1N3 H 0.2843 0.3177 0.0658 0.105 Uiso 0.50 1 calc PR D 1 O1W O 1.0527(2) 0.2751(2) 0.13289(7) 0.0695(19) Uani 0.50 1 d PRDU D 2 H11W H 1.0852 0.3161 0.1211 0.104 Uiso 0.50 1 d PRD D 2 H12W H 1.0144 0.2426 0.1193 0.104 Uiso 0.50 1 d PRD D 2 O2W O 0.5030(2) 0.3447(2) 0.11550(7) 0.0719(19) Uani 0.50 1 d PRDU D 2 H21W H 0.4973 0.3539 0.0948 0.108 Uiso 0.50 1 d PRD D 2 H22W H 0.5530 0.3831 0.1221 0.108 Uiso 0.50 1 d PRD D 2 O3W O 0.2196(2) 0.1730(2) 0.09723(7) 0.0342(13) Uani 0.50 1 d PRDU D 2 H31W H 0.1983 0.2268 0.0914 0.051 Uiso 0.50 1 d PRD D 2 H32W H 0.2770 0.1815 0.1096 0.051 Uiso 0.50 1 d PRD D 2 C1P C 0.2527(3) 0.2996(2) 0.03739(7) 0.0361(18) Uani 0.50 1 d PRDU D 2 H1P1 H 0.3254 0.3152 0.0269 0.054 Uiso 0.50 1 calc PR D 2 H1P2 H 0.2637 0.2469 0.0523 0.054 Uiso 0.50 1 calc PR D 2 H1P3 H 0.2250 0.3530 0.0500 0.054 Uiso 0.50 1 calc PR D 2 O1P O 0.1721(4) 0.2758(6) 0.01287(11) 0.0515(16) Uani 0.50 1 d PDU D 2 H1P H 0.1465 0.3243 0.0041 0.077 Uiso 0.50 1 calc PR D 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 0.02398(5) 0.01461(8) 0.02047(5) 0.00007(6) -0.00190(6) -0.00224(6) C1 0.041(2) 0.021(3) 0.028(2) 0.0039(19) -0.0104(18) -0.005(2) C2 0.031(2) 0.029(3) 0.029(2) -0.0048(19) 0.0021(18) 0.003(2) C3 0.036(2) 0.039(3) 0.0256(19) -0.0035(19) 0.0085(19) 0.005(2) C4 0.046(3) 0.033(4) 0.029(2) -0.013(2) -0.0065(19) 0.009(2) C5 0.071(3) 0.041(4) 0.035(3) 0.002(2) -0.010(3) -0.025(3) C6 0.092(4) 0.038(4) 0.030(2) 0.000(2) -0.013(3) -0.032(3) C7 0.028(2) 0.022(3) 0.027(2) 0.0057(18) -0.0018(17) -0.0003(18) C8 0.034(2) 0.028(3) 0.025(2) -0.0054(19) -0.0028(17) 0.002(2) C9 0.039(2) 0.051(4) 0.0163(19) -0.002(2) -0.0001(18) 0.004(2) C10 0.038(2) 0.055(4) 0.035(2) 0.009(2) -0.006(2) 0.014(3) C11 0.064(3) 0.036(4) 0.078(4) -0.006(3) -0.026(3) 0.035(3) C12 0.056(3) 0.026(4) 0.053(3) -0.003(2) -0.037(2) 0.006(2) C13 0.0305(19) 0.013(3) 0.0324(19) 0.0001(16) -0.0051(19) -0.005(2) C14 0.033(2) 0.039(4) 0.052(3) 0.017(2) -0.024(2) 0.006(2) C15 0.028(2) 0.029(4) 0.067(3) 0.003(3) -0.013(2) -0.004(2) C16 0.037(3) 0.044(4) 0.057(3) -0.011(3) 0.012(2) -0.003(3) C17 0.041(2) 0.033(4) 0.033(2) 0.000(2) 0.009(2) -0.008(2) C18 0.033(2) 0.028(3) 0.030(2) 0.0047(18) -0.003(2) 0.000(2) C19 0.0163(15) 0.008(2) 0.0201(17) -0.0010(15) 0.0015(14) -0.0079(15) C20 0.0140(16) 0.015(3) 0.0219(17) 0.0019(16) 0.0010(14) 0.0031(15) C21 0.0143(16) 0.015(3) 0.0229(18) 0.0016(16) 0.0051(14) -0.0001(15) C22 0.0281(18) 0.015(2) 0.0201(16) 0.0012(15) -0.0056(17) 0.0048(19) C23 0.0231(19) 0.032(3) 0.0182(18) 0.0057(17) 0.0044(15) 0.0050(17) C24 0.023(2) 0.035(3) 0.0210(17) 0.0106(17) 0.0015(16) 0.0052(18) C25 0.0204(18) 0.022(3) 0.0233(19) 0.0015(17) -0.0032(15) 0.0040(17) C26 0.0219(17) 0.012(3) 0.0220(18) -0.0003(16) 0.0028(15) -0.0083(16) C27 0.0202(17) 0.006(2) 0.0166(16) -0.0002(14) -0.0033(14) -0.0057(15) C28 0.0143(16) 0.015(2) 0.0188(16) 0.0008(16) 0.0041(14) -0.0035(15) C29 0.0137(14) 0.014(2) 0.0184(15) -0.0018(13) 0.0024(15) -0.0025(17) C30 0.0167(14) 0.012(3) 0.0197(15) 0.0002(15) 0.0001(12) 0.0010(15) C31 0.0143(16) 0.023(3) 0.0225(18) 0.0003(17) 0.0043(15) 0.0005(16) C32 0.0174(14) 0.0110(19) 0.0300(15) -0.0023(14) -0.0001(12) 0.0013(13) C33 0.0147(12) 0.0102(15) 0.0319(13) -0.0009(12) 0.0001(11) -0.0064(12) C34 0.0147(14) 0.0118(18) 0.0307(15) -0.0012(13) 0.0019(12) -0.0043(13) C35 0.0113(13) 0.007(2) 0.0263(16) -0.0001(16) 0.0018(13) 0.0056(15) C36 0.0099(15) 0.024(3) 0.0149(16) 0.0031(15) 0.0017(13) -0.0030(15) C37 0.0161(16) 0.017(3) 0.0208(18) -0.0052(16) -0.0004(14) 0.0017(16) C38 0.0080(13) 0.018(2) 0.0210(16) -0.0041(14) -0.0020(15) -0.0037(17) C39 0.0075(13) 0.016(3) 0.0287(17) 0.0055(17) 0.0047(12) 0.0034(14) C40 0.0247(19) 0.024(3) 0.0275(18) 0.0035(19) -0.0009(15) 0.0089(18) C41 0.0070(15) 0.054(4) 0.0303(18) 0.0121(19) -0.0011(14) 0.0070(18) C42 0.0175(19) 0.042(3) 0.037(2) 0.022(2) -0.0009(17) 0.0101(19) C43 0.0163(19) 0.020(3) 0.058(3) 0.012(2) 0.0012(18) -0.0009(16) C44 0.0159(17) 0.020(3) 0.031(2) 0.0021(18) -0.0007(15) -0.0040(16) C45 0.0172(16) 0.013(2) 0.0195(15) -0.0032(15) 0.0020(12) 0.0016(15) C46 0.0189(18) 0.029(3) 0.034(2) -0.010(2) 0.0037(17) -0.0010(18) C47 0.028(2) 0.028(3) 0.053(3) -0.022(2) -0.001(2) -0.006(2) C48 0.039(2) 0.026(4) 0.041(2) -0.006(2) 0.003(2) 0.009(2) C49 0.0142(18) 0.046(3) 0.0220(18) -0.0071(18) 0.0129(14) -0.0064(17) C50 0.0170(16) 0.018(3) 0.0228(16) -0.0020(17) -0.0016(12) 0.0014(15) C51 0.0134(16) 0.017(3) 0.0197(16) -0.0011(16) 0.0025(13) -0.0020(14) C52 0.0271(19) 0.017(3) 0.0184(16) -0.0008(15) 0.0007(16) -0.0036(18) C53 0.0190(18) 0.038(3) 0.0211(19) -0.0013(19) 0.0001(16) -0.0009(19) C54 0.032(2) 0.024(3) 0.031(2) -0.0040(18) 0.0050(19) -0.014(2) C55 0.029(2) 0.017(3) 0.045(2) 0.004(2) 0.0062(19) 0.0036(18) C56 0.0144(18) 0.022(3) 0.035(2) -0.0012(18) 0.0010(16) -0.0012(15) C57 0.026(2) 0.039(3) 0.0207(18) -0.0082(19) -0.0051(16) 0.0022(19) C58 0.023(2) 0.062(4) 0.027(2) -0.010(2) 0.0019(18) -0.004(2) C59 0.021(2) 0.074(5) 0.036(2) -0.014(3) -0.0072(19) 0.008(2) C60 0.056(3) 0.060(5) 0.043(3) 0.004(3) -0.014(2) 0.025(3) C61 0.060(3) 0.040(4) 0.047(3) 0.016(2) -0.006(2) 0.006(3) C62 0.033(2) 0.025(3) 0.035(2) -0.002(2) -0.0050(19) 0.002(2) C63 0.0234(19) 0.022(3) 0.0235(19) -0.0041(17) 0.0083(16) -0.0080(17) C64 0.055(3) 0.034(4) 0.0191(18) 0.0001(19) -0.004(2) -0.007(2) C65 0.045(2) 0.028(4) 0.043(2) -0.001(2) 0.032(2) -0.009(2) C66 0.0199(19) 0.037(4) 0.079(3) -0.016(3) 0.021(2) -0.009(2) C67 0.043(2) 0.026(4) 0.062(3) -0.013(3) -0.008(3) 0.011(2) C68 0.030(2) 0.036(3) 0.0262(19) -0.0095(17) -0.0016(18) 0.012(2) C69 0.025(2) 0.024(3) 0.023(2) 0.0000(19) 0.0001(19) 0.001(2) C70 0.039(2) 0.037(3) 0.038(3) -0.002(2) 0.001(2) -0.003(2) C71 0.029(2) 0.025(3) 0.026(2) -0.002(2) -0.0013(19) -0.002(2) C72 0.054(3) 0.051(3) 0.051(3) -0.001(2) 0.002(2) -0.001(2) C73 0.051(3) 0.049(3) 0.048(3) 0.001(2) 0.003(2) -0.002(2) C74 0.033(2) 0.031(3) 0.030(2) -0.001(2) 0.001(2) -0.001(2) C69' 0.020(2) 0.019(3) 0.019(3) -0.001(2) 0.002(2) 0.002(2) C70' 0.020(2) 0.019(3) 0.019(3) -0.001(2) 0.001(2) 0.000(2) C71' 0.040(3) 0.037(3) 0.036(3) -0.002(2) 0.000(2) 0.000(2) C72' 0.058(3) 0.058(3) 0.058(3) -0.001(2) 0.001(2) -0.002(2) C73' 0.054(3) 0.053(3) 0.054(3) 0.001(2) 0.002(2) -0.001(2) C74' 0.034(3) 0.034(3) 0.034(3) -0.001(2) 0.003(2) -0.001(2) C69" 0.028(2) 0.027(3) 0.026(3) -0.001(2) 0.001(2) -0.001(2) C70" 0.035(3) 0.034(3) 0.034(3) 0.000(2) 0.000(2) 0.000(2) C71" 0.046(3) 0.046(3) 0.046(3) 0.000(2) -0.002(2) -0.001(2) C72" 0.048(3) 0.048(3) 0.050(3) 0.000(2) 0.001(2) 0.000(2) C73" 0.034(3) 0.035(3) 0.035(3) 0.001(2) 0.001(2) 0.000(2) C74" 0.035(3) 0.033(3) 0.033(3) -0.002(2) 0.000(2) -0.002(2) O1 0.0171(12) 0.0181(19) 0.0213(13) -0.0024(12) 0.0023(10) 0.0013(11) O2 0.0236(13) 0.0030(17) 0.0252(13) 0.0002(11) 0.0058(11) -0.0021(11) O3 0.0249(13) 0.015(2) 0.0313(15) 0.0025(13) 0.0032(12) -0.0063(12) O4 0.0186(12) 0.0173(19) 0.0177(13) -0.0011(11) 0.0037(10) 0.0033(11) P1 0.0279(5) 0.0195(7) 0.0211(5) 0.0005(5) -0.0048(4) -0.0040(4) P2 0.0160(4) 0.0128(7) 0.0212(4) -0.0005(4) 0.0007(4) -0.0041(4) Si1 0.0147(4) 0.0151(7) 0.0185(5) 0.0011(4) 0.0016(4) -0.0008(4) Si2 0.0207(5) 0.0203(8) 0.0189(5) -0.0028(4) 0.0013(4) -0.0001(5) C1R 0.061(3) 0.060(3) 0.061(3) 0.004(3) -0.003(3) 0.003(3) O1R 0.099(3) 0.102(3) 0.107(3) -0.006(3) 0.000(3) -0.001(3) O1M 0.071(3) 0.084(3) 0.080(3) 0.006(2) 0.009(2) -0.007(2) C1M 0.109(3) 0.105(3) 0.104(3) 0.003(3) 0.003(3) -0.001(3) O1N 0.042(2) 0.053(2) 0.052(2) -0.0083(17) 0.0048(19) 0.001(2) C1N 0.067(3) 0.067(3) 0.077(3) 0.0025(19) 0.000(2) -0.002(2) O1W 0.069(3) 0.069(3) 0.071(3) 0.004(2) -0.010(2) 0.003(2) O2W 0.074(3) 0.073(3) 0.069(3) -0.001(2) -0.007(2) 0.001(2) O3W 0.043(2) 0.025(3) 0.035(2) -0.009(2) 0.0265(19) -0.0100(19) C1P 0.035(3) 0.031(3) 0.042(3) 0.005(2) -0.003(2) 0.004(2) O1P 0.049(2) 0.054(3) 0.052(2) -0.005(2) 0.014(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 O4 2.101(3) . ? Au1 P1 2.2201(14) . ? C1 C6 1.380(9) . ? C1 C2 1.423(7) . ? C1 P1 1.830(5) . ? C2 C3 1.426(6) . ? C3 C4 1.378(8) . ? C4 C5 1.393(8) . ? C5 C6 1.393(8) . ? C7 C12 1.396(8) . ? C7 C8 1.438(7) . ? C7 P1 1.825(5) . ? C8 C9 1.396(7) . ? C9 C10 1.359(9) . ? C10 C11 1.456(9) . ? C11 C12 1.396(8) . ? C13 C14 1.364(7) . ? C13 C18 1.406(6) . ? C13 P1 1.858(5) . ? C14 C15 1.435(7) . ? C15 C16 1.408(9) . ? C16 C17 1.386(8) . ? C17 C18 1.383(7) . ? C19 C28 1.377(5) . ? C19 O1 1.412(5) . ? C19 C20 1.426(5) . ? C20 C21 1.387(5) . ? C20 Si1 1.935(4) . ? C21 C22 1.434(6) . ? C22 C27 1.427(6) . ? C22 C23 1.457(5) . ? C23 C24 1.381(6) . ? C24 C25 1.424(6) . ? C25 C26 1.383(6) . ? C26 C27 1.439(5) . ? C27 C28 1.454(5) . ? C28 C29 1.515(5) . ? C29 C38 1.411(5) . ? C29 C30 1.456(6) . ? C30 C35 1.419(5) . ? C30 C31 1.433(6) . ? C31 C32 1.358(6) . ? C32 C33 1.416(6) . ? C33 C34 1.385(6) . ? C34 C35 1.425(6) . ? C35 C36 1.433(6) . ? C36 C37 1.382(6) . ? C37 C38 1.418(5) . ? C37 Si2 1.932(4) . ? C38 O2 1.428(5) . ? C39 C44 1.395(7) . ? C39 C40 1.437(6) . ? C39 Si1 1.910(4) . ? C40 C41 1.441(6) . ? C41 C42 1.408(8) . ? C42 C43 1.423(7) . ? C43 C44 1.397(7) . ? C45 C50 1.415(5) . ? C45 C46 1.425(7) . ? C45 Si1 1.904(4) . ? C46 C47 1.406(7) . ? C47 C48 1.400(7) . ? C48 C49 1.399(8) . ? C49 C50 1.383(6) . ? C51 C56 1.390(7) . ? C51 C52 1.417(5) . ? C51 Si1 1.896(5) . ? C52 C53 1.397(7) . ? C53 C54 1.401(7) . ? C54 C55 1.391(6) . ? C55 C56 1.416(7) . ? C57 C58 1.405(6) . ? C57 C62 1.416(8) . ? C57 Si2 1.896(5) . ? C58 C59 1.415(8) . ? C59 C60 1.400(10) . ? C60 C61 1.386(8) . ? C61 C62 1.402(7) . ? C63 C64 1.406(6) . ? C63 C68 1.418(6) . ? C63 Si2 1.915(4) . ? C64 C65 1.362(7) . ? C65 C66 1.401(8) . ? C66 C67 1.381(9) . ? C67 C68 1.405(7) . ? C69 C70 1.3900 . ? C69 C74 1.3900 . ? C69 Si2 1.9015(18) . ? C70 C71 1.3900 . ? C71 C72 1.3900 . ? C72 C73 1.3900 . ? C73 C74 1.3900 . ? C69' C70' 1.3900 . ? C69' C74' 1.3900 . ? C69' Si2 1.910(2) . ? C70' C71' 1.3900 . ? C71' C72' 1.3900 . ? C72' C73' 1.3900 . ? C73' C74' 1.3900 . ? C69" C70" 1.3900 . ? C69" C74" 1.3900 . ? C69" Si2 1.8978(19) . ? C70" C71" 1.3900 . ? C71" C72" 1.3900 . ? C72" C73" 1.3900 . ? C73" C74" 1.3900 . ? O1 P2 1.629(3) . ? O2 P2 1.617(3) . ? O3 P2 1.493(3) . ? O4 P2 1.505(3) . ? C1R O1R 1.431(4) . ? O1M C1M 1.425(4) . ? O1N C1N 1.437(4) . ? C1P O1P 1.414(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Au1 P1 172.10(8) . . ? C6 C1 C2 118.5(5) . . ? C6 C1 P1 124.0(4) . . ? C2 C1 P1 117.5(4) . . ? C1 C2 C3 119.1(5) . . ? C4 C3 C2 120.3(5) . . ? C3 C4 C5 120.5(5) . . ? C4 C5 C6 119.3(6) . . ? C1 C6 C5 122.3(6) . . ? C12 C7 C8 119.8(4) . . ? C12 C7 P1 122.1(4) . . ? C8 C7 P1 118.1(4) . . ? C9 C8 C7 118.3(5) . . ? C10 C9 C8 122.5(5) . . ? C9 C10 C11 120.0(5) . . ? C12 C11 C10 118.0(6) . . ? C7 C12 C11 121.4(5) . . ? C14 C13 C18 119.9(5) . . ? C14 C13 P1 117.1(4) . . ? C18 C13 P1 122.9(4) . . ? C13 C14 C15 120.7(5) . . ? C16 C15 C14 117.8(5) . . ? C17 C16 C15 121.0(5) . . ? C18 C17 C16 119.7(5) . . ? C17 C18 C13 120.7(5) . . ? C28 C19 O1 118.7(3) . . ? C28 C19 C20 123.0(3) . . ? O1 C19 C20 117.9(3) . . ? C21 C20 C19 117.8(3) . . ? C21 C20 Si1 118.6(3) . . ? C19 C20 Si1 123.6(3) . . ? C20 C21 C22 121.3(3) . . ? C27 C22 C21 120.1(3) . . ? C27 C22 C23 118.9(4) . . ? C21 C22 C23 121.0(4) . . ? C24 C23 C22 120.5(4) . . ? C23 C24 C25 120.0(4) . . ? C26 C25 C24 120.9(4) . . ? C25 C26 C27 120.7(4) . . ? C22 C27 C26 118.8(3) . . ? C22 C27 C28 118.0(3) . . ? C26 C27 C28 123.2(3) . . ? C19 C28 C27 119.0(3) . . ? C19 C28 C29 119.7(3) . . ? C27 C28 C29 121.2(3) . . ? C38 C29 C30 117.9(3) . . ? C38 C29 C28 122.1(4) . . ? C30 C29 C28 120.0(3) . . ? C35 C30 C31 118.5(4) . . ? C35 C30 C29 118.4(4) . . ? C31 C30 C29 123.1(3) . . ? C32 C31 C30 120.5(4) . . ? C31 C32 C33 121.6(4) . . ? C34 C33 C32 119.3(4) . . ? C33 C34 C35 120.4(4) . . ? C30 C35 C34 119.6(4) . . ? C30 C35 C36 119.7(4) . . ? C34 C35 C36 120.7(3) . . ? C37 C36 C35 123.4(3) . . ? C36 C37 C38 116.0(4) . . ? C36 C37 Si2 116.2(3) . . ? C38 C37 Si2 127.6(3) . . ? C29 C38 C37 124.3(4) . . ? C29 C38 O2 116.6(3) . . ? C37 C38 O2 119.1(3) . . ? C44 C39 C40 118.0(4) . . ? C44 C39 Si1 122.3(3) . . ? C40 C39 Si1 119.6(4) . . ? C39 C40 C41 121.0(5) . . ? C42 C41 C40 118.5(4) . . ? C41 C42 C43 120.1(4) . . ? C44 C43 C42 120.4(5) . . ? C39 C44 C43 121.9(4) . . ? C50 C45 C46 116.4(4) . . ? C50 C45 Si1 122.9(3) . . ? C46 C45 Si1 120.4(3) . . ? C47 C46 C45 121.8(4) . . ? C48 C47 C46 119.8(5) . . ? C49 C48 C47 119.0(5) . . ? C50 C49 C48 121.2(4) . . ? C49 C50 C45 121.8(4) . . ? C56 C51 C52 116.9(4) . . ? C56 C51 Si1 121.7(3) . . ? C52 C51 Si1 121.4(4) . . ? C53 C52 C51 122.1(4) . . ? C52 C53 C54 119.3(4) . . ? C55 C54 C53 120.2(5) . . ? C54 C55 C56 119.3(5) . . ? C51 C56 C55 122.2(4) . . ? C58 C57 C62 117.2(5) . . ? C58 C57 Si2 122.7(4) . . ? C62 C57 Si2 120.1(3) . . ? C57 C58 C59 120.4(6) . . ? C60 C59 C58 122.0(5) . . ? C61 C60 C59 117.4(5) . . ? C60 C61 C62 121.7(6) . . ? C61 C62 C57 121.3(5) . . ? C64 C63 C68 116.9(4) . . ? C64 C63 Si2 125.5(3) . . ? C68 C63 Si2 117.5(3) . . ? C65 C64 C63 122.3(4) . . ? C64 C65 C66 121.0(5) . . ? C67 C66 C65 118.3(5) . . ? C66 C67 C68 121.3(5) . . ? C67 C68 C63 120.1(4) . . ? C70 C69 C74 120.0 . . ? C70 C69 Si2 116.60(16) . . ? C74 C69 Si2 122.00(16) . . ? C69 C70 C71 120.0 . . ? C72 C71 C70 120.0 . . ? C71 C72 C73 120.0 . . ? C72 C73 C74 120.0 . . ? C73 C74 C69 120.0 . . ? C70' C69' C74' 120.0 . . ? C70' C69' Si2 112.24(16) . . ? C74' C69' Si2 127.75(16) . . ? C71' C70' C69' 120.0 . . ? C70' C71' C72' 120.0 . . ? C73' C72' C71' 120.0 . . ? C72' C73' C74' 120.0 . . ? C73' C74' C69' 120.0 . . ? C70" C69" C74" 120.0 . . ? C70" C69" Si2 115.83(16) . . ? C74" C69" Si2 122.84(16) . . ? C69" C70" C71" 120.0 . . ? C70" C71" C72" 120.0 . . ? C73" C72" C71" 120.0 . . ? C74" C73" C72" 120.0 . . ? C73" C74" C69" 120.0 . . ? C19 O1 P2 120.6(3) . . ? C38 O2 P2 120.5(3) . . ? P2 O4 Au1 120.63(17) . . ? C7 P1 C1 107.2(2) . . ? C7 P1 C13 104.9(2) . . ? C1 P1 C13 104.6(2) . . ? C7 P1 Au1 111.44(17) . . ? C1 P1 Au1 110.65(18) . . ? C13 P1 Au1 117.30(16) . . ? O3 P2 O4 118.12(17) . . ? O3 P2 O2 106.17(18) . . ? O4 P2 O2 109.67(15) . . ? O3 P2 O1 113.45(16) . . ? O4 P2 O1 104.84(18) . . ? O2 P2 O1 103.68(15) . . ? C51 Si1 C45 110.51(18) . . ? C51 Si1 C39 112.51(18) . . ? C45 Si1 C39 106.7(2) . . ? C51 Si1 C20 108.04(19) . . ? C45 Si1 C20 106.74(17) . . ? C39 Si1 C20 112.20(16) . . ? C57 Si2 C69" 119.95(19) . . ? C57 Si2 C69 111.25(19) . . ? C69" Si2 C69 8.7 . . ? C57 Si2 C69' 103.01(19) . . ? C69" Si2 C69' 17.2 . . ? C69 Si2 C69' 8.6 . . ? C57 Si2 C63 109.66(19) . . ? C69" Si2 C63 98.43(19) . . ? C69 Si2 C63 102.76(19) . . ? C69' Si2 C63 108.72(18) . . ? C57 Si2 C37 108.0(2) . . ? C69" Si2 C37 113.76(17) . . ? C69 Si2 C37 118.92(17) . . ? C69' Si2 C37 121.39(17) . . ? C63 Si2 C37 105.81(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.8(8) . . . . ? P1 C1 C2 C3 -178.6(4) . . . . ? C1 C2 C3 C4 0.7(7) . . . . ? C2 C3 C4 C5 -1.6(8) . . . . ? C3 C4 C5 C6 0.9(9) . . . . ? C2 C1 C6 C5 -1.4(9) . . . . ? P1 C1 C6 C5 177.9(5) . . . . ? C4 C5 C6 C1 0.6(10) . . . . ? C12 C7 C8 C9 0.5(7) . . . . ? P1 C7 C8 C9 179.7(4) . . . . ? C7 C8 C9 C10 -0.3(7) . . . . ? C8 C9 C10 C11 -1.6(8) . . . . ? C9 C10 C11 C12 3.3(9) . . . . ? C8 C7 C12 C11 1.4(8) . . . . ? P1 C7 C12 C11 -177.8(5) . . . . ? C10 C11 C12 C7 -3.2(9) . . . . ? C18 C13 C14 C15 -1.0(8) . . . . ? P1 C13 C14 C15 -178.8(5) . . . . ? C13 C14 C15 C16 -0.2(9) . . . . ? C14 C15 C16 C17 0.7(10) . . . . ? C15 C16 C17 C18 0.1(10) . . . . ? C16 C17 C18 C13 -1.3(8) . . . . ? C14 C13 C18 C17 1.8(8) . . . . ? P1 C13 C18 C17 179.4(4) . . . . ? C28 C19 C20 C21 -8.6(7) . . . . ? O1 C19 C20 C21 178.6(4) . . . . ? C28 C19 C20 Si1 168.6(4) . . . . ? O1 C19 C20 Si1 -4.2(6) . . . . ? C19 C20 C21 C22 1.6(7) . . . . ? Si1 C20 C21 C22 -175.7(4) . . . . ? C20 C21 C22 C27 2.5(7) . . . . ? C20 C21 C22 C23 -177.5(5) . . . . ? C27 C22 C23 C24 1.8(7) . . . . ? C21 C22 C23 C24 -178.2(5) . . . . ? C22 C23 C24 C25 -3.1(8) . . . . ? C23 C24 C25 C26 1.5(8) . . . . ? C24 C25 C26 C27 1.5(8) . . . . ? C21 C22 C27 C26 -178.9(4) . . . . ? C23 C22 C27 C26 1.1(7) . . . . ? C21 C22 C27 C28 -0.1(7) . . . . ? C23 C22 C27 C28 179.9(4) . . . . ? C25 C26 C27 C22 -2.7(7) . . . . ? C25 C26 C27 C28 178.6(5) . . . . ? O1 C19 C28 C27 -176.2(4) . . . . ? C20 C19 C28 C27 11.0(7) . . . . ? O1 C19 C28 C29 5.7(7) . . . . ? C20 C19 C28 C29 -167.1(4) . . . . ? C22 C27 C28 C19 -6.4(7) . . . . ? C26 C27 C28 C19 172.3(4) . . . . ? C22 C27 C28 C29 171.7(4) . . . . ? C26 C27 C28 C29 -9.6(7) . . . . ? C19 C28 C29 C38 -56.7(6) . . . . ? C27 C28 C29 C38 125.3(5) . . . . ? C19 C28 C29 C30 121.6(5) . . . . ? C27 C28 C29 C30 -56.5(6) . . . . ? C38 C29 C30 C35 -5.6(6) . . . . ? C28 C29 C30 C35 176.1(4) . . . . ? C38 C29 C30 C31 172.1(4) . . . . ? C28 C29 C30 C31 -6.2(6) . . . . ? C35 C30 C31 C32 -2.0(6) . . . . ? C29 C30 C31 C32 -179.8(4) . . . . ? C30 C31 C32 C33 -1.0(7) . . . . ? C31 C32 C33 C34 2.7(7) . . . . ? C32 C33 C34 C35 -1.3(6) . . . . ? C31 C30 C35 C34 3.4(6) . . . . ? C29 C30 C35 C34 -178.8(4) . . . . ? C31 C30 C35 C36 -175.6(4) . . . . ? C29 C30 C35 C36 2.2(6) . . . . ? C33 C34 C35 C30 -1.7(6) . . . . ? C33 C34 C35 C36 177.3(4) . . . . ? C30 C35 C36 C37 1.6(6) . . . . ? C34 C35 C36 C37 -177.4(4) . . . . ? C35 C36 C37 C38 -1.7(6) . . . . ? C35 C36 C37 Si2 173.7(3) . . . . ? C30 C29 C38 C37 5.8(6) . . . . ? C28 C29 C38 C37 -175.9(4) . . . . ? C30 C29 C38 O2 -173.5(3) . . . . ? C28 C29 C38 O2 4.7(6) . . . . ? C36 C37 C38 C29 -2.2(6) . . . . ? Si2 C37 C38 C29 -177.0(3) . . . . ? C36 C37 C38 O2 177.2(4) . . . . ? Si2 C37 C38 O2 2.4(6) . . . . ? C44 C39 C40 C41 2.3(5) . . . . ? Si1 C39 C40 C41 -179.0(3) . . . . ? C39 C40 C41 C42 -1.7(5) . . . . ? C40 C41 C42 C43 1.2(6) . . . . ? C41 C42 C43 C44 -1.2(6) . . . . ? C40 C39 C44 C43 -2.4(5) . . . . ? Si1 C39 C44 C43 179.0(3) . . . . ? C42 C43 C44 C39 1.9(6) . . . . ? C50 C45 C46 C47 -1.4(7) . . . . ? Si1 C45 C46 C47 172.3(4) . . . . ? C45 C46 C47 C48 1.3(8) . . . . ? C46 C47 C48 C49 0.2(8) . . . . ? C47 C48 C49 C50 -1.7(8) . . . . ? C48 C49 C50 C45 1.7(7) . . . . ? C46 C45 C50 C49 -0.1(6) . . . . ? Si1 C45 C50 C49 -173.6(3) . . . . ? C56 C51 C52 C53 2.0(6) . . . . ? Si1 C51 C52 C53 -174.9(3) . . . . ? C51 C52 C53 C54 -2.3(6) . . . . ? C52 C53 C54 C55 1.1(6) . . . . ? C53 C54 C55 C56 0.3(7) . . . . ? C52 C51 C56 C55 -0.5(6) . . . . ? Si1 C51 C56 C55 176.4(3) . . . . ? C54 C55 C56 C51 -0.6(7) . . . . ? C62 C57 C58 C59 0.5(7) . . . . ? Si2 C57 C58 C59 178.7(4) . . . . ? C57 C58 C59 C60 1.7(8) . . . . ? C58 C59 C60 C61 -2.2(9) . . . . ? C59 C60 C61 C62 0.5(9) . . . . ? C60 C61 C62 C57 1.7(9) . . . . ? C58 C57 C62 C61 -2.2(7) . . . . ? Si2 C57 C62 C61 179.6(4) . . . . ? C68 C63 C64 C65 0.7(8) . . . . ? Si2 C63 C64 C65 -174.7(5) . . . . ? C63 C64 C65 C66 -1.7(9) . . . . ? C64 C65 C66 C67 3.1(9) . . . . ? C65 C66 C67 C68 -3.6(9) . . . . ? C66 C67 C68 C63 2.7(9) . . . . ? C64 C63 C68 C67 -1.1(8) . . . . ? Si2 C63 C68 C67 174.6(4) . . . . ? C74 C69 C70 C71 0.0 . . . . ? Si2 C69 C70 C71 166.76(17) . . . . ? C69 C70 C71 C72 0.0 . . . . ? C70 C71 C72 C73 0.0 . . . . ? C71 C72 C73 C74 0.0 . . . . ? C72 C73 C74 C69 0.0 . . . . ? C70 C69 C74 C73 0.0 . . . . ? Si2 C69 C74 C73 -166.03(18) . . . . ? C74' C69' C70' C71' 0.0 . . . . ? Si2 C69' C70' C71' 178.94(16) . . . . ? C69' C70' C71' C72' 0.0 . . . . ? C70' C71' C72' C73' 0.0 . . . . ? C71' C72' C73' C74' 0.0 . . . . ? C72' C73' C74' C69' 0.0 . . . . ? C70' C69' C74' C73' 0.0 . . . . ? Si2 C69' C74' C73' -178.76(19) . . . . ? C74" C69" C70" C71" 0.0 . . . . ? Si2 C69" C70" C71" 167.18(17) . . . . ? C69" C70" C71" C72" 0.0 . . . . ? C70" C71" C72" C73" 0.0 . . . . ? C71" C72" C73" C74" 0.0 . . . . ? C72" C73" C74" C69" 0.0 . . . . ? C70" C69" C74" C73" 0.0 . . . . ? Si2 C69" C74" C73" -166.25(18) . . . . ? C28 C19 O1 P2 69.8(5) . . . . ? C20 C19 O1 P2 -117.1(4) . . . . ? C29 C38 O2 P2 69.6(4) . . . . ? C37 C38 O2 P2 -109.8(4) . . . . ? P1 Au1 O4 P2 -56.1(7) . . . . ? C12 C7 P1 C1 24.8(5) . . . . ? C8 C7 P1 C1 -154.4(4) . . . . ? C12 C7 P1 C13 -86.1(4) . . . . ? C8 C7 P1 C13 94.8(4) . . . . ? C12 C7 P1 Au1 146.0(4) . . . . ? C8 C7 P1 Au1 -33.2(4) . . . . ? C6 C1 P1 C7 -80.4(5) . . . . ? C2 C1 P1 C7 98.9(4) . . . . ? C6 C1 P1 C13 30.7(6) . . . . ? C2 C1 P1 C13 -150.0(4) . . . . ? C6 C1 P1 Au1 157.9(5) . . . . ? C2 C1 P1 Au1 -22.8(4) . . . . ? C14 C13 P1 C7 172.6(4) . . . . ? C18 C13 P1 C7 -5.1(5) . . . . ? C14 C13 P1 C1 59.9(5) . . . . ? C18 C13 P1 C1 -117.8(4) . . . . ? C14 C13 P1 Au1 -63.1(4) . . . . ? C18 C13 P1 Au1 119.2(4) . . . . ? O4 Au1 P1 C7 -74.0(6) . . . . ? O4 Au1 P1 C1 45.2(6) . . . . ? O4 Au1 P1 C13 165.1(6) . . . . ? Au1 O4 P2 O3 157.41(17) . . . . ? Au1 O4 P2 O2 -80.8(2) . . . . ? Au1 O4 P2 O1 29.9(2) . . . . ? C38 O2 P2 O3 -164.6(3) . . . . ? C38 O2 P2 O4 66.7(3) . . . . ? C38 O2 P2 O1 -44.8(3) . . . . ? C19 O1 P2 O3 68.3(3) . . . . ? C19 O1 P2 O4 -161.5(3) . . . . ? C19 O1 P2 O2 -46.5(3) . . . . ? C56 C51 Si1 C45 -116.0(3) . . . . ? C52 C51 Si1 C45 60.9(3) . . . . ? C56 C51 Si1 C39 124.9(3) . . . . ? C52 C51 Si1 C39 -58.3(3) . . . . ? C56 C51 Si1 C20 0.5(4) . . . . ? C52 C51 Si1 C20 177.3(3) . . . . ? C50 C45 Si1 C51 -26.1(4) . . . . ? C46 C45 Si1 C51 160.7(3) . . . . ? C50 C45 Si1 C39 96.5(4) . . . . ? C46 C45 Si1 C39 -76.7(4) . . . . ? C50 C45 Si1 C20 -143.3(4) . . . . ? C46 C45 Si1 C20 43.5(4) . . . . ? C44 C39 Si1 C51 150.2(3) . . . . ? C40 C39 Si1 C51 -28.3(3) . . . . ? C44 C39 Si1 C45 28.9(3) . . . . ? C40 C39 Si1 C45 -149.7(3) . . . . ? C44 C39 Si1 C20 -87.7(3) . . . . ? C40 C39 Si1 C20 93.8(3) . . . . ? C21 C20 Si1 C51 -88.5(4) . . . . ? C19 C20 Si1 C51 94.4(4) . . . . ? C21 C20 Si1 C45 30.4(4) . . . . ? C19 C20 Si1 C45 -146.7(4) . . . . ? C21 C20 Si1 C39 146.9(4) . . . . ? C19 C20 Si1 C39 -30.2(5) . . . . ? C58 C57 Si2 C69" 25.4(5) . . . . ? C62 C57 Si2 C69" -156.4(4) . . . . ? C58 C57 Si2 C69 25.1(5) . . . . ? C62 C57 Si2 C69 -156.8(4) . . . . ? C58 C57 Si2 C69' 22.5(4) . . . . ? C62 C57 Si2 C69' -159.4(4) . . . . ? C58 C57 Si2 C63 138.1(4) . . . . ? C62 C57 Si2 C63 -43.8(5) . . . . ? C58 C57 Si2 C37 -107.1(4) . . . . ? C62 C57 Si2 C37 71.1(4) . . . . ? C70" C69" Si2 C57 38.0(3) . . . . ? C74" C69" Si2 C57 -155.3(2) . . . . ? C70" C69" Si2 C69 39.95(8) . . . . ? C74" C69" Si2 C69 -153.27(9) . . . . ? C70" C69" Si2 C69' 47.74(9) . . . . ? C74" C69" Si2 C69' -145.48(8) . . . . ? C70" C69" Si2 C63 -80.6(2) . . . . ? C74" C69" Si2 C63 86.2(2) . . . . ? C70" C69" Si2 C37 167.9(2) . . . . ? C74" C69" Si2 C37 -25.3(2) . . . . ? C70 C69 Si2 C57 43.0(2) . . . . ? C74 C69 Si2 C57 -150.5(2) . . . . ? C70 C69 Si2 C69" -135.12(7) . . . . ? C74 C69 Si2 C69" 31.36(11) . . . . ? C70 C69 Si2 C69' 60.36(8) . . . . ? C74 C69 Si2 C69' -133.16(9) . . . . ? C70 C69 Si2 C63 -74.2(2) . . . . ? C74 C69 Si2 C63 92.2(2) . . . . ? C70 C69 Si2 C37 169.4(2) . . . . ? C74 C69 Si2 C37 -24.1(2) . . . . ? C70' C69' Si2 C57 70.5(2) . . . . ? C74' C69' Si2 C57 -110.7(2) . . . . ? C70' C69' Si2 C69" -100.83(6) . . . . ? C74' C69' Si2 C69" 78.01(12) . . . . ? C70' C69' Si2 C69 -92.96(7) . . . . ? C74' C69' Si2 C69 85.88(12) . . . . ? C70' C69' Si2 C63 -45.8(2) . . . . ? C74' C69' Si2 C63 133.0(2) . . . . ? C70' C69' Si2 C37 -168.7(2) . . . . ? C74' C69' Si2 C37 10.1(3) . . . . ? C64 C63 Si2 C57 -17.2(5) . . . . ? C68 C63 Si2 C57 167.5(4) . . . . ? C64 C63 Si2 C69" 108.9(5) . . . . ? C68 C63 Si2 C69" -66.5(4) . . . . ? C64 C63 Si2 C69 101.2(5) . . . . ? C68 C63 Si2 C69 -74.1(4) . . . . ? C64 C63 Si2 C69' 94.8(5) . . . . ? C68 C63 Si2 C69' -80.6(4) . . . . ? C64 C63 Si2 C37 -133.4(5) . . . . ? C68 C63 Si2 C37 51.3(4) . . . . ? C36 C37 Si2 C57 -85.7(4) . . . . ? C38 C37 Si2 C57 89.1(4) . . . . ? C36 C37 Si2 C69" 138.6(3) . . . . ? C38 C37 Si2 C69" -46.6(4) . . . . ? C36 C37 Si2 C69 146.4(3) . . . . ? C38 C37 Si2 C69 -38.8(4) . . . . ? C36 C37 Si2 C69' 156.0(3) . . . . ? C38 C37 Si2 C69' -29.2(5) . . . . ? C36 C37 Si2 C63 31.7(4) . . . . ? C38 C37 Si2 C63 -153.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 26.86 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.666 _refine_diff_density_min -3.523 _refine_diff_density_rms 0.157 # Attachment 'web_deposit_cif_file_2_AntonioM.Echavarren_1314183768.DSD77AP21212X.cif' data_dsd77ap21212 _database_code_depnum_ccdc_archive 'CCDC 841519' #TrackingRef 'web_deposit_cif_file_2_AntonioM.Echavarren_1314183768.DSD77AP21212X.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59.60 H47.99 Ag Cl2.39 O4.84 P Si2' _chemical_formula_weight 1121.30 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' Si Si 0.0817 0.0704 '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' Ag Ag -0.8971 1.1015 '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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 20.2597(6) _cell_length_b 16.3556(5) _cell_length_c 17.3458(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5747.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9845 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 31.75 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.296 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2300 _exptl_absorpt_coefficient_mu 0.576 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 70 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 116988 _diffrn_reflns_av_R_equivalents 0.0592 _diffrn_reflns_av_sigmaI/netI 0.0594 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 36.51 _reflns_number_total 26827 _reflns_number_gt 17149 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmetric unit of the model is made up of half silver complex 1.18 dichloromethane molecules, 0.4 hexane molecules disordered in two positions with occupations ratio 30:10, and 0.84 water (water hydrogen atoms have not been modeled). A dichloromethane molecule with an occupation of 0.18%, the two water molecules with occupation of 0.42% and the disordered hexane that is occupied a 40% are disordered parts of the same cell site. At the same time phenyl groups C7-C12, C39-C44 and C51-C56 are disordered in two different positions. C39-C44 are disordered in two positions with occupation ratio of 50:50. C8-C12 and C51-C56 are modeled in two different positions with occupation ratio of 68:32 nevertheless this disorder has to be explained since the 0.32 occupied site is not compatible with itself. Then the 0.32 occupied site takes place at the same time that 0.32 of the 0.68 occupied site. ; _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^)+(0.1362P)^2^+2.8289P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _chemical_absolute_configuration ad _refine_ls_abs_structure_Flack -0.06(3) _refine_ls_number_reflns 26827 _refine_ls_number_parameters 684 _refine_ls_number_restraints 216 _refine_ls_R_factor_all 0.1174 _refine_ls_R_factor_gt 0.0692 _refine_ls_wR_factor_ref 0.2312 _refine_ls_wR_factor_gt 0.1898 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.001 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 Ag1 Ag 0.5000 1.0000 0.151973(14) 0.03273(5) Uani 1 2 d S . . Ag2 Ag 0.5000 1.0000 0.329117(14) 0.03302(5) Uani 1 2 d S . . C1 C 0.35236(16) 1.1247(2) 0.0966(2) 0.0508(7) Uani 1 1 d U . . C2 C 0.35767(16) 1.0761(2) 0.0296(2) 0.0509(8) Uani 1 1 d U . . H2 H 0.3192 1.0518 0.0083 0.061 Uiso 1 1 calc R . . C3 C 0.41965(19) 1.0632(3) -0.0066(2) 0.0606(10) Uani 1 1 d U . . H3 H 0.4233 1.0287 -0.0504 0.073 Uiso 1 1 calc R . . C4 C 0.4740(2) 1.1016(3) 0.0233(3) 0.0651(10) Uani 1 1 d U . . H4 H 0.5155 1.0943 -0.0014 0.078 Uiso 1 1 calc R . . C5 C 0.47076(18) 1.1500(2) 0.0869(3) 0.0574(9) Uani 1 1 d U . . H5 H 0.5093 1.1765 0.1056 0.069 Uiso 1 1 calc R . . C6 C 0.40744(18) 1.1612(2) 0.1269(3) 0.0597(9) Uani 1 1 d U . . H6 H 0.4048 1.1930 0.1727 0.072 Uiso 1 1 calc R . . C7 C 0.2668(2) 1.18808(19) 0.2358(2) 0.0559(9) Uani 1 1 d . . . C8 C 0.2390(3) 1.1595(4) 0.3039(3) 0.0563(14) Uani 0.686(3) 1 d PU A 1 H8 H 0.2126 1.1116 0.3038 0.068 Uiso 0.686(3) 1 calc PR A 1 C9 C 0.2499(3) 1.2005(4) 0.3699(3) 0.0527(13) Uani 0.686(3) 1 d PU A 1 H9 H 0.2371 1.1761 0.4173 0.063 Uiso 0.686(3) 1 calc PR A 1 C10 C 0.2786(4) 1.2757(4) 0.3712(4) 0.0645(16) Uani 0.686(3) 1 d PU A 1 H10 H 0.2825 1.3045 0.4185 0.077 Uiso 0.686(3) 1 calc PR A 1 C11 C 0.3021(4) 1.3105(3) 0.3036(4) 0.0609(15) Uani 0.686(3) 1 d PU A 1 H11 H 0.3207 1.3638 0.3040 0.073 Uiso 0.686(3) 1 calc PR A 1 C12 C 0.2982(3) 1.2660(3) 0.2350(3) 0.0477(11) Uani 0.686(3) 1 d PU A 1 H12 H 0.3160 1.2875 0.1885 0.057 Uiso 0.686(3) 1 calc PR A 1 C8' C 0.2508(5) 1.1481(5) 0.3029(6) 0.0293(17) Uani 0.314(3) 1 d PU A 2 H8' H 0.2558 1.0904 0.3042 0.035 Uiso 0.314(3) 1 calc PR A 2 C9' C 0.2248(9) 1.1919(10) 0.3781(9) 0.071(4) Uani 0.314(3) 1 d PU A 2 H9' H 0.1976 1.1658 0.4153 0.085 Uiso 0.314(3) 1 calc PR A 2 C10' C 0.2454(9) 1.2715(8) 0.3840(8) 0.087(4) Uani 0.314(3) 1 d PU A 2 H10' H 0.2453 1.2971 0.4332 0.104 Uiso 0.314(3) 1 calc PR A 2 C11' C 0.2644(12) 1.3114(9) 0.3267(13) 0.107(5) Uani 0.314(3) 1 d PU A 2 H11' H 0.2847 1.3636 0.3306 0.128 Uiso 0.314(3) 1 calc PR A 2 C12' C 0.2536(13) 1.2737(9) 0.2587(11) 0.107(6) Uani 0.314(3) 1 d PU A 2 H12' H 0.2345 1.3070 0.2198 0.129 Uiso 0.314(3) 1 calc PR A 2 C13 C 0.21649(14) 1.20565(18) 0.07547(16) 0.0359(6) Uani 1 1 d U . . C14 C 0.15157(17) 1.2268(2) 0.09444(19) 0.0487(7) Uani 1 1 d U A . H14 H 0.1315 1.2018 0.1380 0.058 Uiso 1 1 calc R . . C15 C 0.11487(19) 1.2839(2) 0.0512(2) 0.0573(9) Uani 1 1 d U . . H15 H 0.0709 1.2973 0.0653 0.069 Uiso 1 1 calc R A . C16 C 0.14438(17) 1.3200(2) -0.0123(2) 0.0511(8) Uani 1 1 d U A . H16 H 0.1207 1.3592 -0.0418 0.061 Uiso 1 1 calc R . . C17 C 0.20755(17) 1.2994(2) -0.0327(2) 0.0592(8) Uani 1 1 d U . . H17 H 0.2271 1.3243 -0.0766 0.071 Uiso 1 1 calc R A . C18 C 0.24376(15) 1.2426(2) 0.00981(18) 0.0502(8) Uani 1 1 d U A . H18 H 0.2873 1.2287 -0.0059 0.060 Uiso 1 1 calc R . . C19 C 0.22619(11) 1.03250(15) 0.14251(13) 0.0263(4) Uani 1 1 d . . . C20 C 0.17753(12) 1.01053(18) 0.09071(12) 0.0315(5) Uani 1 1 d . A . H20 H 0.1637 1.0494 0.0533 0.038 Uiso 1 1 calc R . . C21 C 0.14745(13) 0.93262(17) 0.09112(14) 0.0309(5) Uani 1 1 d . . . C22 C 0.10237(16) 0.9084(2) 0.03275(17) 0.0415(7) Uani 1 1 d . A . H22 H 0.0915 0.9456 -0.0074 0.050 Uiso 1 1 calc R . . C23 C 0.07448(16) 0.8324(2) 0.03350(19) 0.0451(7) Uani 1 1 d . . . H23 H 0.0444 0.8171 -0.0060 0.054 Uiso 1 1 calc R A . C24 C 0.09006(15) 0.7765(2) 0.09253(17) 0.0408(6) Uani 1 1 d . A . H24 H 0.0710 0.7234 0.0925 0.049 Uiso 1 1 calc R . . C25 C 0.13333(14) 0.79918(16) 0.15074(16) 0.0338(5) Uani 1 1 d . . . H25 H 0.1432 0.7616 0.1909 0.041 Uiso 1 1 calc R A . C26 C 0.16295(12) 0.87731(15) 0.15111(13) 0.0282(5) Uani 1 1 d . A . C27 C 0.21142(11) 0.89956(14) 0.20761(12) 0.0243(4) Uani 1 1 d . . . C28 C 0.24449(11) 0.97236(14) 0.19769(12) 0.0239(4) Uani 1 1 d . A . C29 C 0.22741(12) 0.84497(14) 0.27300(13) 0.0269(5) Uani 1 1 d . A . C30 C 0.17782(13) 0.82061(16) 0.32717(14) 0.0306(5) Uani 1 1 d . . . C31 C 0.11331(14) 0.85138(17) 0.32635(15) 0.0335(5) Uani 1 1 d . A . H31 H 0.1010 0.8897 0.2877 0.040 Uiso 1 1 calc R . . C32 C 0.06749(15) 0.8275(2) 0.38005(18) 0.0421(7) Uani 1 1 d . . . H32 H 0.0242 0.8498 0.3788 0.050 Uiso 1 1 calc R A . C33 C 0.08460(18) 0.7701(2) 0.43692(18) 0.0454(7) Uani 1 1 d . A . H33 H 0.0526 0.7534 0.4738 0.054 Uiso 1 1 calc R . . C34 C 0.14627(18) 0.7383(2) 0.43959(18) 0.0466(8) Uani 1 1 d . . . H34 H 0.1567 0.6992 0.4782 0.056 Uiso 1 1 calc R A . C35 C 0.19600(15) 0.76225(17) 0.38591(15) 0.0358(6) Uani 1 1 d . A . C36 C 0.26104(16) 0.73007(18) 0.38807(16) 0.0379(6) Uani 1 1 d . . . H36 H 0.2714 0.6885 0.4244 0.046 Uiso 1 1 calc R A . C37 C 0.30885(14) 0.75717(15) 0.33963(15) 0.0318(5) Uani 1 1 d . A . C38 C 0.29149(12) 0.81763(14) 0.28446(13) 0.0262(4) Uani 1 1 d . . . C39 C 0.41791(10) 0.67608(11) 0.23455(12) 0.0313(11) Uani 0.50 1 d PG A 1 C40 C 0.37198(11) 0.67506(16) 0.17502(14) 0.0410(14) Uani 0.50 1 d PG A 1 H40A H 0.3292 0.6973 0.1829 0.049 Uiso 0.50 1 calc PR A 1 C41 C 0.38868(16) 0.6415(2) 0.10402(13) 0.0444(15) Uani 0.50 1 d PG A 1 H41A H 0.3573 0.6408 0.0633 0.053 Uiso 0.50 1 calc PR A 1 C42 C 0.45130(18) 0.6090(2) 0.09254(16) 0.0736(19) Uani 0.50 1 d PG A 1 H42A H 0.4627 0.5861 0.0440 0.088 Uiso 0.50 1 calc PR A 1 C43 C 0.49722(14) 0.6100(2) 0.1521(2) 0.0541(14) Uani 0.50 1 d PG A 1 H43A H 0.5400 0.5878 0.1442 0.065 Uiso 0.50 1 calc PR A 1 C44 C 0.48053(11) 0.64356(17) 0.22307(17) 0.0417(14) Uani 0.50 1 d PG A 1 H44A H 0.5119 0.6443 0.2638 0.050 Uiso 0.50 1 calc PR A 1 C39' C 0.41994(11) 0.66394(12) 0.25559(12) 0.0394(13) Uani 0.50 1 d PG A 2 C40' C 0.38310(11) 0.67091(14) 0.18830(13) 0.0368(13) Uani 0.50 1 d PG A 2 H40B H 0.3430 0.7010 0.1884 0.044 Uiso 0.50 1 calc PR A 2 C41' C 0.40497(15) 0.63390(17) 0.12084(13) 0.051(2) Uani 0.50 1 d PG A 2 H41B H 0.3798 0.6387 0.0749 0.062 Uiso 0.50 1 calc PR A 2 C42' C 0.46368(17) 0.5899(2) 0.12066(18) 0.084(3) Uani 0.50 1 d PG A 2 H42B H 0.4786 0.5646 0.0745 0.101 Uiso 0.50 1 calc PR A 2 C43' C 0.50052(15) 0.5830(2) 0.1879(2) 0.100(4) Uani 0.50 1 d PG A 2 H43B H 0.5407 0.5529 0.1878 0.121 Uiso 0.50 1 calc PR A 2 C44' C 0.47865(13) 0.61997(18) 0.25541(18) 0.102(3) Uani 0.50 1 d PG A 2 H44B H 0.5038 0.6152 0.3014 0.123 Uiso 0.50 1 calc PR A 2 C45 C 0.45624(16) 0.78667(18) 0.37958(19) 0.0424(7) Uani 1 1 d . A . C46 C 0.51814(18) 0.7988(2) 0.3458(3) 0.0533(9) Uani 1 1 d . . . H46 H 0.5301 0.7685 0.3012 0.064 Uiso 1 1 calc R . . C47 C 0.56262(18) 0.8553(2) 0.3774(3) 0.0569(10) Uani 1 1 d . . . H47 H 0.6044 0.8638 0.3538 0.068 Uiso 1 1 calc R . . C48 C 0.5461(2) 0.8977(2) 0.4413(2) 0.0651(10) Uani 1 1 d . . . H48 H 0.5765 0.9359 0.4622 0.078 Uiso 1 1 calc R . . C49 C 0.4865(2) 0.8868(2) 0.4765(2) 0.0566(9) Uani 1 1 d . . . H49 H 0.4758 0.9170 0.5216 0.068 Uiso 1 1 calc R . . C50 C 0.4412(2) 0.8308(2) 0.44598(19) 0.0480(8) Uani 1 1 d . . . H50 H 0.3999 0.8229 0.4708 0.058 Uiso 1 1 calc R . . C51 C 0.39106(19) 0.62407(18) 0.4166(2) 0.0839(8) Uani 0.686(3) 1 d PGU A 1 C52 C 0.3984(2) 0.6340(2) 0.4957(2) 0.0839(8) Uani 0.686(3) 1 d PGU A 1 H52A H 0.4066 0.6868 0.5165 0.101 Uiso 0.686(3) 1 calc PR A 1 C53 C 0.3936(3) 0.5668(3) 0.5444(2) 0.0839(8) Uani 0.686(3) 1 d PGU A 1 H53A H 0.3986 0.5736 0.5985 0.101 Uiso 0.686(3) 1 calc PR A 1 C54 C 0.3816(3) 0.4896(2) 0.5140(3) 0.0839(8) Uani 0.686(3) 1 d PGU A 1 H54A H 0.3783 0.4437 0.5473 0.101 Uiso 0.686(3) 1 calc PR A 1 C55 C 0.3743(3) 0.47964(18) 0.4349(3) 0.0839(8) Uani 0.686(3) 1 d PGU A 1 H55A H 0.3660 0.4269 0.4141 0.101 Uiso 0.686(3) 1 calc PR A 1 C56 C 0.3790(2) 0.5469(2) 0.3862(2) 0.0839(8) Uani 0.686(3) 1 d PGU A 1 H56A H 0.3740 0.5401 0.3321 0.101 Uiso 0.686(3) 1 calc PR A 1 C51' C 0.4000(2) 0.6129(2) 0.3922(2) 0.0849(13) Uani 0.314(3) 1 d PGU A 2 C52' C 0.44402(18) 0.6019(2) 0.4528(3) 0.0849(13) Uani 0.314(3) 1 d PGU A 2 H52B H 0.4670 0.6475 0.4736 0.102 Uiso 0.314(3) 1 calc PR A 2 C53' C 0.4544(2) 0.5243(3) 0.4830(3) 0.0849(13) Uani 0.314(3) 1 d PGU . 2 H53B H 0.4845 0.5168 0.5244 0.102 Uiso 0.314(3) 1 calc PR A 2 C54' C 0.4208(3) 0.4576(2) 0.4526(3) 0.0849(13) Uani 0.314(3) 1 d PGU A 2 H54B H 0.4279 0.4045 0.4732 0.102 Uiso 0.314(3) 1 calc PR A 2 C55' C 0.3768(3) 0.4685(2) 0.3920(3) 0.0849(13) Uani 0.314(3) 1 d PGU A 2 H55B H 0.3538 0.4230 0.3712 0.102 Uiso 0.314(3) 1 calc PR A 2 C56' C 0.3664(3) 0.5462(2) 0.3618(2) 0.0849(13) Uani 0.314(3) 1 d PGU A 2 H56B H 0.3363 0.5537 0.3204 0.102 Uiso 0.314(3) 1 calc PR A 2 O1 O 0.29705(7) 0.99067(9) 0.24602(8) 0.0235(3) Uani 1 1 d . . . O2 O 0.34133(9) 0.84630(10) 0.23604(10) 0.0270(3) Uani 1 1 d . A . O3 O 0.39993(9) 0.95384(11) 0.16656(10) 0.0296(4) Uani 1 1 d . . . O4 O 0.39833(9) 0.95700(11) 0.31507(10) 0.0292(4) Uani 1 1 d . . . P1 P 0.36518(3) 0.93976(3) 0.24072(3) 0.02382(10) Uani 1 1 d . A . Si1 Si 0.26573(4) 1.13665(5) 0.14007(4) 0.03379(15) Uani 1 1 d . A . Si2 Si 0.39530(4) 0.71110(5) 0.34140(5) 0.03906(18) Uani 1 1 d . . . C1D C 0.5000 0.5000 0.8144(4) 0.208(6) Uani 1 2 d S . . H1D1 H 0.4724 0.4651 0.8481 0.250 Uiso 0.50 1 calc PR . . H1D2 H 0.5276 0.5349 0.8481 0.250 Uiso 0.50 1 calc PR . . Cl1D Cl 0.44817(9) 0.56283(10) 0.76101(10) 0.1101(5) Uani 1 1 d . . . C1L C 0.4794(2) 0.7982(3) 0.7392(4) 0.111(4) Uani 0.516(3) 1 d PD B 1 H1L1 H 0.5175 0.7979 0.7034 0.134 Uiso 0.516(3) 1 calc PR B 1 H1L2 H 0.4849 0.7511 0.7745 0.134 Uiso 0.516(3) 1 calc PR B 1 Cl1L Cl 0.41286(12) 0.78361(19) 0.68906(15) 0.0837(8) Uani 0.516(3) 1 d PD B 1 Cl2L Cl 0.48352(13) 0.89180(13) 0.79651(13) 0.1171(14) Uani 0.516(3) 1 d PD B 1 C1H C 0.16842(13) 0.47870(13) 0.42424(13) 0.093(2) Uani 0.30 1 d PRD B 3 H1HA H 0.1293 0.4663 0.4554 0.140 Uiso 0.30 1 calc PR B 3 H1HB H 0.1984 0.5137 0.4538 0.140 Uiso 0.30 1 calc PR B 3 H1HC H 0.1910 0.4277 0.4107 0.140 Uiso 0.30 1 calc PR B 3 C2H C 0.14711(13) 0.52348(13) 0.34982(13) 0.093(2) Uani 0.30 1 d PRD B 3 H2HA H 0.1135 0.4843 0.3311 0.112 Uiso 0.30 1 calc PR B 3 H2HB H 0.1208 0.5681 0.3731 0.112 Uiso 0.30 1 calc PR B 3 C3H C 0.16513(13) 0.56469(13) 0.27248(13) 0.093(2) Uani 0.30 1 d PRD B 3 H3HA H 0.1201 0.5731 0.2519 0.112 Uiso 0.30 1 calc PR B 3 H3HB H 0.1779 0.6193 0.2922 0.112 Uiso 0.30 1 calc PR B 3 C4H C 0.20365(13) 0.56580(13) 0.19585(13) 0.093(2) Uani 0.30 1 d PRD B 3 H4HA H 0.1795 0.6010 0.1589 0.112 Uiso 0.30 1 calc PR B 3 H4HB H 0.2472 0.5914 0.2052 0.112 Uiso 0.30 1 calc PR B 3 C5H C 0.21496(13) 0.48186(13) 0.15779(13) 0.093(2) Uani 0.30 1 d PRD B 3 H5HA H 0.1949 0.4375 0.1888 0.112 Uiso 0.30 1 calc PR B 3 H5HB H 0.1961 0.4804 0.1052 0.112 Uiso 0.30 1 calc PR B 3 C6H C 0.29059(13) 0.47374(13) 0.15552(13) 0.093(2) Uani 0.30 1 d PRD B 3 H6HA H 0.3026 0.4214 0.1319 0.140 Uiso 0.30 1 calc PR B 3 H6HB H 0.3081 0.4760 0.2081 0.140 Uiso 0.30 1 calc PR B 3 H6HC H 0.3093 0.5186 0.1251 0.140 Uiso 0.30 1 calc PR B 3 C1H' C 0.21891(13) 0.54587(13) 0.54742(13) 0.036(2) Uani 0.10 1 d PRD B 4 H1HD H 0.2305 0.5085 0.5895 0.055 Uiso 0.10 1 calc PR B 4 H1HE H 0.1819 0.5806 0.5634 0.055 Uiso 0.10 1 calc PR B 4 H1HF H 0.2571 0.5802 0.5350 0.055 Uiso 0.10 1 calc PR B 4 C2H' C 0.19864(13) 0.49542(13) 0.47490(13) 0.036(2) Uani 0.10 1 d PRD B 4 H2HC H 0.2373 0.4591 0.4683 0.044 Uiso 0.10 1 calc PR B 4 H2HD H 0.1637 0.4595 0.4961 0.044 Uiso 0.10 1 calc PR B 4 C3H' C 0.17515(13) 0.50669(13) 0.39003(13) 0.036(2) Uani 0.10 1 d PRD B 4 H3HC H 0.1399 0.4649 0.3878 0.044 Uiso 0.10 1 calc PR B 4 H3HD H 0.1511 0.5591 0.3947 0.044 Uiso 0.10 1 calc PR B 4 C4H' C 0.19497(13) 0.51012(13) 0.30440(13) 0.036(2) Uani 0.10 1 d PRD B 4 H4HC H 0.2422 0.5256 0.3018 0.044 Uiso 0.10 1 calc PR B 4 H4HD H 0.1912 0.4541 0.2832 0.044 Uiso 0.10 1 calc PR B 4 C5H' C 0.15653(13) 0.56786(13) 0.25079(13) 0.036(2) Uani 0.10 1 d PRD B 4 H5HC H 0.1391 0.6155 0.2796 0.044 Uiso 0.10 1 calc PR B 4 H5HD H 0.1193 0.5390 0.2257 0.044 Uiso 0.10 1 calc PR B 4 C6H' C 0.20831(13) 0.59473(13) 0.19094(13) 0.036(2) Uani 0.10 1 d PRD B 4 H6HD H 0.1879 0.6322 0.1539 0.055 Uiso 0.10 1 calc PR B 4 H6HE H 0.2252 0.5466 0.1637 0.055 Uiso 0.10 1 calc PR B 4 H6HF H 0.2448 0.6225 0.2172 0.055 Uiso 0.10 1 calc PR B 4 C1E C 0.21215(13) 0.52654(13) 0.52918(13) 0.1182(17) Uani 0.18 1 d PRD B 2 H1EA H 0.1822 0.5171 0.5734 0.142 Uiso 0.18 1 calc PR B 2 H1EB H 0.2120 0.5860 0.5186 0.142 Uiso 0.18 1 calc PR B 2 Cl1E Cl 0.18077(13) 0.48058(13) 0.45457(13) 0.1182(17) Uani 0.18 1 d PRD B 2 Cl2E Cl 0.29593(13) 0.49793(13) 0.55927(13) 0.1182(17) Uani 0.18 1 d PRD B 2 O1W O 0.27090(13) 0.46174(13) 0.12055(13) 0.071(2) Uani 0.42 1 d PR B 1 O2W O 0.21567(13) 0.45821(13) 0.54783(13) 0.103(3) Uani 0.42 1 d PR B 1 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 Ag1 0.01945(9) 0.04737(12) 0.03138(9) 0.000 0.000 -0.00242(11) Ag2 0.02240(10) 0.04509(12) 0.03158(9) 0.000 0.000 -0.00115(12) C1 0.0304(13) 0.0534(14) 0.0687(16) 0.0373(13) -0.0115(12) -0.0058(11) C2 0.0284(13) 0.0744(19) 0.0499(15) 0.0225(14) 0.0087(11) 0.0017(13) C3 0.0428(17) 0.086(2) 0.0529(17) 0.0220(17) 0.0117(14) 0.0075(18) C4 0.0375(16) 0.076(2) 0.082(2) 0.0357(18) 0.0095(16) -0.0044(16) C5 0.0321(14) 0.0547(16) 0.085(2) 0.0291(16) -0.0148(15) -0.0034(13) C6 0.0392(16) 0.0568(16) 0.083(2) 0.0291(16) -0.0186(16) -0.0124(14) C7 0.080(2) 0.0373(13) 0.0503(15) 0.0065(12) -0.0291(16) 0.0043(14) C8 0.075(3) 0.049(2) 0.045(2) -0.0002(18) -0.016(2) 0.024(2) C9 0.060(3) 0.060(2) 0.0384(19) -0.0020(18) 0.005(2) 0.006(2) C10 0.082(4) 0.063(3) 0.049(2) -0.004(2) -0.013(2) 0.008(3) C11 0.085(4) 0.040(2) 0.057(2) -0.0033(19) -0.007(3) 0.002(2) C12 0.065(3) 0.0343(17) 0.0437(19) 0.0044(16) 0.001(2) -0.0011(18) C8' 0.031(3) 0.022(3) 0.034(3) -0.013(2) 0.006(3) -0.001(3) C9' 0.087(11) 0.070(5) 0.055(6) -0.029(5) 0.003(6) 0.023(6) C10' 0.122(11) 0.059(4) 0.079(4) -0.049(4) -0.062(6) 0.039(6) C11' 0.138(15) 0.044(5) 0.137(7) -0.041(5) -0.046(10) -0.013(7) C12' 0.184(19) 0.052(7) 0.087(6) 0.009(6) -0.063(10) -0.023(10) C13 0.0290(12) 0.0415(12) 0.0372(11) 0.0152(10) -0.0023(9) 0.0036(10) C14 0.0387(14) 0.0629(16) 0.0445(13) 0.0233(12) 0.0133(11) 0.0139(13) C15 0.0478(17) 0.0761(19) 0.0481(15) 0.0260(14) 0.0081(13) 0.0251(16) C16 0.0365(15) 0.0614(16) 0.0555(15) 0.0283(13) -0.0068(12) 0.0059(13) C17 0.0310(14) 0.0857(19) 0.0608(16) 0.0477(14) 0.0023(12) -0.0005(14) C18 0.0220(12) 0.0759(18) 0.0526(15) 0.0396(13) 0.0032(11) 0.0025(12) C19 0.0157(8) 0.0379(10) 0.0255(8) 0.0075(8) 0.0012(7) 0.0007(7) C20 0.0233(9) 0.0476(13) 0.0236(8) 0.0054(9) -0.0027(7) 0.0040(10) C21 0.0238(10) 0.0418(12) 0.0272(9) -0.0012(9) -0.0034(8) 0.0023(9) C22 0.0380(14) 0.0520(15) 0.0346(11) -0.0050(11) -0.0115(11) -0.0004(12) C23 0.0362(14) 0.0565(16) 0.0427(13) -0.0113(12) -0.0124(11) -0.0044(13) C24 0.0337(13) 0.0475(14) 0.0411(13) -0.0127(11) -0.0053(11) -0.0047(11) C25 0.0290(11) 0.0356(11) 0.0367(11) -0.0074(9) 0.0019(9) -0.0025(9) C26 0.0213(9) 0.0370(10) 0.0264(9) -0.0017(8) 0.0014(8) -0.0003(8) C27 0.0212(9) 0.0299(9) 0.0217(8) 0.0008(7) 0.0040(7) -0.0003(7) C28 0.0189(8) 0.0319(9) 0.0211(7) 0.0050(7) 0.0010(7) 0.0002(7) C29 0.0269(10) 0.0278(9) 0.0259(9) 0.0011(7) 0.0008(8) -0.0037(8) C30 0.0314(11) 0.0348(10) 0.0256(9) 0.0028(8) 0.0004(8) -0.0079(9) C31 0.0295(11) 0.0403(11) 0.0308(10) 0.0024(9) 0.0065(9) -0.0075(9) C32 0.0321(13) 0.0531(15) 0.0410(13) 0.0028(12) 0.0109(11) -0.0071(12) C33 0.0444(16) 0.0518(15) 0.0400(13) 0.0090(11) 0.0129(12) -0.0128(13) C34 0.0471(17) 0.0527(15) 0.0401(13) 0.0113(12) 0.0050(12) -0.0159(13) C35 0.0374(13) 0.0406(12) 0.0295(10) 0.0105(9) 0.0018(10) -0.0095(10) C36 0.0428(15) 0.0392(12) 0.0317(10) 0.0125(9) -0.0031(11) -0.0069(11) C37 0.0340(12) 0.0305(10) 0.0307(10) 0.0040(8) -0.0019(9) -0.0003(9) C38 0.0253(10) 0.0297(9) 0.0237(8) 0.0023(7) 0.0001(7) -0.0025(8) C39 0.033(2) 0.0249(17) 0.036(2) 0.0032(17) 0.0054(19) 0.0040(16) C40 0.036(3) 0.045(3) 0.042(3) -0.009(2) 0.006(2) -0.010(2) C41 0.051(3) 0.042(3) 0.040(3) -0.016(2) -0.004(3) 0.000(3) C42 0.066(4) 0.048(3) 0.108(4) -0.051(3) 0.056(3) -0.026(3) C43 0.041(3) 0.055(3) 0.066(3) -0.039(2) 0.014(3) -0.008(3) C44 0.034(2) 0.038(2) 0.054(3) -0.007(2) 0.002(2) -0.001(2) C39' 0.045(3) 0.034(2) 0.039(3) -0.009(2) -0.008(2) 0.006(2) C40' 0.043(3) 0.029(2) 0.038(3) -0.001(2) 0.007(2) 0.002(2) C41' 0.071(5) 0.042(3) 0.041(3) -0.003(3) 0.002(3) 0.003(3) C42' 0.088(7) 0.079(6) 0.085(6) -0.032(5) 0.040(5) -0.004(5) C43' 0.088(7) 0.125(8) 0.088(6) -0.047(6) 0.009(7) 0.033(7) C44' 0.099(5) 0.089(4) 0.119(6) -0.068(4) -0.054(5) 0.064(4) C45 0.0406(14) 0.0343(11) 0.0525(15) -0.0009(11) -0.0176(12) 0.0087(11) C46 0.0377(15) 0.0446(15) 0.078(2) -0.0082(16) -0.0099(15) 0.0039(12) C47 0.0368(15) 0.0440(15) 0.090(3) 0.0028(17) -0.0180(17) 0.0027(13) C48 0.076(2) 0.0356(14) 0.084(2) 0.0022(14) -0.0555(17) 0.0013(15) C49 0.075(2) 0.0429(14) 0.0519(15) -0.0040(12) -0.0295(16) 0.0080(15) C50 0.061(2) 0.0404(14) 0.0431(14) 0.0048(11) -0.0170(14) 0.0034(14) C51 0.0969(14) 0.0734(12) 0.0814(12) 0.0142(10) -0.0123(11) 0.0008(11) C52 0.0969(14) 0.0734(12) 0.0814(12) 0.0142(10) -0.0123(11) 0.0008(11) C53 0.0969(14) 0.0734(12) 0.0814(12) 0.0142(10) -0.0123(11) 0.0008(11) C54 0.0969(14) 0.0734(12) 0.0814(12) 0.0142(10) -0.0123(11) 0.0008(11) C55 0.0969(14) 0.0734(12) 0.0814(12) 0.0142(10) -0.0123(11) 0.0008(11) C56 0.0969(14) 0.0734(12) 0.0814(12) 0.0142(10) -0.0123(11) 0.0008(11) C51' 0.0881(18) 0.0829(18) 0.0838(18) 0.0103(14) -0.0052(14) -0.0019(14) C52' 0.0881(18) 0.0829(18) 0.0838(18) 0.0103(14) -0.0052(14) -0.0019(14) C53' 0.0881(18) 0.0829(18) 0.0838(18) 0.0103(14) -0.0052(14) -0.0019(14) C54' 0.0881(18) 0.0829(18) 0.0838(18) 0.0103(14) -0.0052(14) -0.0019(14) C55' 0.0881(18) 0.0829(18) 0.0838(18) 0.0103(14) -0.0052(14) -0.0019(14) C56' 0.0881(18) 0.0829(18) 0.0838(18) 0.0103(14) -0.0052(14) -0.0019(14) O1 0.0182(5) 0.0285(6) 0.0238(6) 0.0033(6) -0.0005(5) -0.0003(5) O2 0.0255(7) 0.0284(6) 0.0270(6) 0.0015(6) 0.0017(6) 0.0015(6) O3 0.0213(7) 0.0410(8) 0.0265(7) 0.0039(6) 0.0010(6) -0.0004(7) O4 0.0239(7) 0.0375(8) 0.0263(7) 0.0025(6) -0.0047(6) 0.0014(7) P1 0.0191(2) 0.0299(2) 0.02255(19) 0.00381(19) -0.00055(19) 0.00039(18) Si1 0.0286(3) 0.0373(3) 0.0355(3) 0.0143(3) -0.0083(3) -0.0035(3) Si2 0.0380(4) 0.0295(3) 0.0497(4) 0.0037(3) -0.0096(3) 0.0043(3) C1D 0.078(3) 0.506(19) 0.040(3) 0.000 0.000 -0.154(7) Cl1D 0.1196(10) 0.0998(8) 0.1109(9) -0.0333(7) 0.0620(8) -0.0430(8) C1L 0.084(6) 0.130(8) 0.120(8) -0.055(7) -0.024(6) 0.046(6) Cl1L 0.0658(14) 0.1073(18) 0.0779(14) -0.0147(13) -0.0107(12) 0.0113(13) Cl2L 0.174(4) 0.0724(15) 0.105(2) -0.0091(14) 0.015(2) -0.007(2) C1H 0.102(5) 0.084(4) 0.094(4) 0.031(4) -0.035(4) -0.026(4) C2H 0.102(5) 0.084(4) 0.094(4) 0.031(4) -0.035(4) -0.026(4) C3H 0.102(5) 0.084(4) 0.094(4) 0.031(4) -0.035(4) -0.026(4) C4H 0.102(5) 0.084(4) 0.094(4) 0.031(4) -0.035(4) -0.026(4) C5H 0.102(5) 0.084(4) 0.094(4) 0.031(4) -0.035(4) -0.026(4) C6H 0.102(5) 0.084(4) 0.094(4) 0.031(4) -0.035(4) -0.026(4) C1H' 0.056(6) 0.015(3) 0.038(4) -0.007(3) 0.017(4) 0.011(4) C2H' 0.056(6) 0.015(3) 0.038(4) -0.007(3) 0.017(4) 0.011(4) C3H' 0.056(6) 0.015(3) 0.038(4) -0.007(3) 0.017(4) 0.011(4) C4H' 0.056(6) 0.015(3) 0.038(4) -0.007(3) 0.017(4) 0.011(4) C5H' 0.056(6) 0.015(3) 0.038(4) -0.007(3) 0.017(4) 0.011(4) C6H' 0.056(6) 0.015(3) 0.038(4) -0.007(3) 0.017(4) 0.011(4) C1E 0.109(3) 0.153(4) 0.092(2) 0.048(3) 0.070(2) 0.073(3) Cl1E 0.109(3) 0.153(4) 0.092(2) 0.048(3) 0.070(2) 0.073(3) Cl2E 0.109(3) 0.153(4) 0.092(2) 0.048(3) 0.070(2) 0.073(3) O1W 0.096(5) 0.071(4) 0.047(3) 0.028(3) 0.019(3) 0.019(4) O2W 0.124(6) 0.131(7) 0.054(3) -0.001(4) 0.048(4) -0.063(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 Ag1 O3 2.1780(18) 2_675 ? Ag1 O3 2.1780(18) . ? Ag1 Ag2 3.0727(3) . ? Ag2 O4 2.1901(18) . ? Ag2 O4 2.1901(18) 2_675 ? C1 C6 1.370(5) . ? C1 C2 1.412(5) . ? C1 Si1 1.920(4) . ? C2 C3 1.419(5) . ? C3 C4 1.370(6) . ? C4 C5 1.360(7) . ? C5 C6 1.470(6) . ? C7 C8' 1.375(10) . ? C7 C8 1.390(7) . ? C7 C12 1.424(6) . ? C7 C12' 1.481(17) . ? C7 Si1 1.861(4) . ? C8 C9 1.345(8) . ? C9 C10 1.361(9) . ? C10 C11 1.387(9) . ? C11 C12 1.397(8) . ? C8' C9' 1.578(17) . ? C9' C10' 1.37(2) . ? C10' C11' 1.25(3) . ? C11' C12' 1.35(3) . ? C13 C14 1.399(4) . ? C13 C18 1.402(4) . ? C13 Si1 1.877(3) . ? C14 C15 1.409(5) . ? C15 C16 1.386(5) . ? C16 C17 1.370(5) . ? C17 C18 1.395(4) . ? C19 C20 1.381(3) . ? C19 C28 1.422(3) . ? C19 Si1 1.883(3) . ? C20 C21 1.412(4) . ? C21 C26 1.414(3) . ? C21 C22 1.420(4) . ? C22 C23 1.366(5) . ? C23 C24 1.409(5) . ? C24 C25 1.388(4) . ? C25 C26 1.412(4) . ? C26 C27 1.434(3) . ? C27 C28 1.377(3) . ? C27 C29 1.479(3) . ? C28 O1 1.388(3) . ? C29 C38 1.387(3) . ? C29 C30 1.432(3) . ? C30 C31 1.401(4) . ? C30 C35 1.444(4) . ? C31 C32 1.372(4) . ? C32 C33 1.406(5) . ? C33 C34 1.354(5) . ? C34 C35 1.426(4) . ? C35 C36 1.419(5) . ? C36 C37 1.357(4) . ? C37 C38 1.420(3) . ? C37 Si2 1.907(3) . ? C38 O2 1.395(3) . ? C39 C40 1.3900 . ? C39 C44 1.3900 . ? C39 Si2 1.993(2) . ? C40 C41 1.3900 . ? C41 C42 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C39' C40' 1.3900 . ? C39' C44' 1.3900 . ? C39' Si2 1.749(2) . ? C40' C41' 1.3900 . ? C41' C42' 1.3900 . ? C42' C43' 1.3900 . ? C43' C44' 1.3900 . ? C45 C50 1.393(5) . ? C45 C46 1.398(5) . ? C45 Si2 1.868(3) . ? C46 C47 1.403(5) . ? C47 C48 1.349(6) . ? C48 C49 1.364(6) . ? C49 C50 1.401(5) . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C51 Si2 1.933(3) . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? C51' C52' 1.3900 . ? C51' C56' 1.3900 . ? C51' Si2 1.834(3) . ? C52' C53' 1.3900 . ? C53' C54' 1.3900 . ? C53' C53' 2.010(8) 2_665 ? C54' C55' 1.3900 . ? C55' C56' 1.3900 . ? O1 P1 1.6146(16) . ? O2 P1 1.6052(17) . ? O3 P1 1.4845(18) . ? O4 P1 1.4811(18) . ? C1D Cl1D 1.737(4) . ? C1D Cl1D 1.737(4) 2_665 ? C1L Cl1L 1.623(4) . ? C1L Cl2L 1.827(4) . ? C1H C2H 1.5457 . ? C2H C3H 1.5451 . ? C3H C4H 1.5415 . ? C4H C5H 1.5405 . ? C5H C6H 1.5385 . ? C1H' C2H' 1.5593 . ? C2H' C3H' 1.5581 . ? C3H' C4H' 1.5397 . ? C4H' C5H' 1.5372 . ? C5H' C6H' 1.5399 . ? C1E Cl1E 1.6260 . ? C1E Cl2E 1.8364 . ? 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 O3 Ag1 O3 166.66(9) 2_675 . ? O3 Ag1 Ag2 83.33(4) 2_675 . ? O3 Ag1 Ag2 83.33(4) . . ? O4 Ag2 O4 167.23(9) . 2_675 ? O4 Ag2 Ag1 83.61(4) . . ? O4 Ag2 Ag1 83.61(4) 2_675 . ? C6 C1 C2 119.9(3) . . ? C6 C1 Si1 123.3(3) . . ? C2 C1 Si1 116.8(2) . . ? C1 C2 C3 121.0(3) . . ? C4 C3 C2 118.4(4) . . ? C5 C4 C3 122.3(4) . . ? C4 C5 C6 119.9(4) . . ? C1 C6 C5 118.4(4) . . ? C8' C7 C8 12.6(5) . . ? C8' C7 C12 122.6(5) . . ? C8 C7 C12 119.3(4) . . ? C8' C7 C12' 100.3(9) . . ? C8 C7 C12' 90.9(9) . . ? C12 C7 C12' 40.3(10) . . ? C8' C7 Si1 122.6(4) . . ? C8 C7 Si1 127.0(3) . . ? C12 C7 Si1 113.7(3) . . ? C12' C7 Si1 131.7(7) . . ? C9 C8 C7 119.4(6) . . ? C8 C9 C10 122.3(6) . . ? C9 C10 C11 120.2(6) . . ? C10 C11 C12 119.2(5) . . ? C11 C12 C7 118.9(5) . . ? C7 C8' C9' 124.3(9) . . ? C10' C9' C8' 113.0(14) . . ? C11' C10' C9' 122.0(14) . . ? C10' C11' C12' 114.0(15) . . ? C11' C12' C7 129.7(16) . . ? C14 C13 C18 117.1(3) . . ? C14 C13 Si1 120.5(2) . . ? C18 C13 Si1 122.3(2) . . ? C13 C14 C15 122.3(3) . . ? C16 C15 C14 118.5(3) . . ? C17 C16 C15 120.3(3) . . ? C16 C17 C18 121.2(3) . . ? C17 C18 C13 120.6(3) . . ? C20 C19 C28 116.4(2) . . ? C20 C19 Si1 121.63(18) . . ? C28 C19 Si1 122.01(17) . . ? C19 C20 C21 122.6(2) . . ? C20 C21 C26 119.0(2) . . ? C20 C21 C22 121.7(2) . . ? C26 C21 C22 119.3(3) . . ? C23 C22 C21 120.9(3) . . ? C22 C23 C24 120.3(3) . . ? C25 C24 C23 119.8(3) . . ? C24 C25 C26 120.9(3) . . ? C25 C26 C21 118.8(2) . . ? C25 C26 C27 121.6(2) . . ? C21 C26 C27 119.5(2) . . ? C28 C27 C26 117.9(2) . . ? C28 C27 C29 120.7(2) . . ? C26 C27 C29 121.4(2) . . ? C27 C28 O1 118.98(18) . . ? C27 C28 C19 123.7(2) . . ? O1 C28 C19 117.22(19) . . ? C38 C29 C30 118.2(2) . . ? C38 C29 C27 120.6(2) . . ? C30 C29 C27 121.1(2) . . ? C31 C30 C29 123.2(2) . . ? C31 C30 C35 118.9(2) . . ? C29 C30 C35 117.9(2) . . ? C32 C31 C30 121.5(3) . . ? C31 C32 C33 120.0(3) . . ? C34 C33 C32 120.5(3) . . ? C33 C34 C35 121.6(3) . . ? C36 C35 C34 122.5(3) . . ? C36 C35 C30 120.0(2) . . ? C34 C35 C30 117.5(3) . . ? C37 C36 C35 121.7(2) . . ? C36 C37 C38 117.9(3) . . ? C36 C37 Si2 121.1(2) . . ? C38 C37 Si2 120.9(2) . . ? C29 C38 O2 118.9(2) . . ? C29 C38 C37 123.5(2) . . ? O2 C38 C37 117.4(2) . . ? C40 C39 C44 120.0 . . ? C40 C39 Si2 122.71(11) . . ? C44 C39 Si2 116.93(11) . . ? C41 C40 C39 120.0 . . ? C40 C41 C42 120.0 . . ? C43 C42 C41 120.0 . . ? C42 C43 C44 120.0 . . ? C43 C44 C39 120.0 . . ? C40' C39' C44' 120.0 . . ? C40' C39' Si2 121.68(13) . . ? C44' C39' Si2 118.31(13) . . ? C39' C40' C41' 120.0 . . ? C42' C41' C40' 120.0 . . ? C43' C42' C41' 120.0 . . ? C44' C43' C42' 120.0 . . ? C43' C44' C39' 120.0 . . ? C50 C45 C46 118.0(3) . . ? C50 C45 Si2 119.5(3) . . ? C46 C45 Si2 122.5(3) . . ? C45 C46 C47 120.4(4) . . ? C48 C47 C46 119.9(4) . . ? C47 C48 C49 121.4(3) . . ? C48 C49 C50 119.7(3) . . ? C45 C50 C49 120.6(4) . . ? C52 C51 C56 120.0 . . ? C52 C51 Si2 125.13(17) . . ? C56 C51 Si2 114.87(17) . . ? C51 C52 C53 120.0 . . ? C54 C53 C52 120.0 . . ? C55 C54 C53 120.0 . . ? C54 C55 C56 120.0 . . ? C55 C56 C51 120.0 . . ? C52' C51' C56' 120.0 . . ? C52' C51' Si2 120.6(2) . . ? C56' C51' Si2 118.7(2) . . ? C51' C52' C53' 120.0 . . ? C54' C53' C52' 120.0 . . ? C54' C53' C53' 98.0(5) . 2_665 ? C52' C53' C53' 120.0(5) . 2_665 ? C55' C54' C53' 120.0 . . ? C56' C55' C54' 120.0 . . ? C55' C56' C51' 120.0 . . ? C28 O1 P1 120.68(14) . . ? C38 O2 P1 120.51(15) . . ? P1 O3 Ag1 126.57(10) . . ? P1 O4 Ag2 125.76(11) . . ? O4 P1 O3 120.66(10) . . ? O4 P1 O2 111.22(10) . . ? O3 P1 O2 104.28(10) . . ? O4 P1 O1 103.88(9) . . ? O3 P1 O1 112.01(9) . . ? O2 P1 O1 103.69(9) . . ? C7 Si1 C13 105.48(14) . . ? C7 Si1 C19 113.20(14) . . ? C13 Si1 C19 109.33(12) . . ? C7 Si1 C1 112.66(18) . . ? C13 Si1 C1 108.23(13) . . ? C19 Si1 C1 107.79(13) . . ? C39' Si2 C51' 90.47(14) . . ? C39' Si2 C45 113.87(14) . . ? C51' Si2 C45 112.00(16) . . ? C39' Si2 C37 115.00(12) . . ? C51' Si2 C37 113.66(16) . . ? C45 Si2 C37 110.57(13) . . ? C39' Si2 C51 105.21(13) . . ? C51' Si2 C51 14.8 . . ? C45 Si2 C51 106.11(15) . . ? C37 Si2 C51 105.14(15) . . ? C39' Si2 C39 10.4 . . ? C51' Si2 C39 100.57(13) . . ? C45 Si2 C39 111.58(13) . . ? C37 Si2 C39 108.03(11) . . ? C51 Si2 C39 115.23(13) . . ? Cl1D C1D Cl1D 115.6(4) . 2_665 ? Cl1L C1L Cl2L 116.9(3) . . ? C3H C2H C1H 150.0 . . ? C4H C3H C2H 150.9 . . ? C5H C4H C3H 115.7 . . ? C6H C5H C4H 103.7 . . ? C3H' C2H' C1H' 141.3 . . ? C4H' C3H' C2H' 146.7 . . ? C5H' C4H' C3H' 118.3 . . ? C4H' C5H' C6H' 103.8 . . ? Cl1E C1E Cl2E 118.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Ag1 Ag2 O4 178.43(7) 2_675 . . . ? O3 Ag1 Ag2 O4 -1.57(7) . . . . ? O3 Ag1 Ag2 O4 -1.58(7) 2_675 . . 2_675 ? O3 Ag1 Ag2 O4 178.42(7) . . . 2_675 ? C6 C1 C2 C3 1.1(5) . . . . ? Si1 C1 C2 C3 -179.6(3) . . . . ? C1 C2 C3 C4 -2.6(6) . . . . ? C2 C3 C4 C5 1.5(6) . . . . ? C3 C4 C5 C6 1.1(6) . . . . ? C2 C1 C6 C5 1.5(5) . . . . ? Si1 C1 C6 C5 -177.8(2) . . . . ? C4 C5 C6 C1 -2.6(5) . . . . ? C8' C7 C8 C9 100(3) . . . . ? C12 C7 C8 C9 -9.0(8) . . . . ? C12' C7 C8 C9 -38.9(11) . . . . ? Si1 C7 C8 C9 173.4(4) . . . . ? C7 C8 C9 C10 10.4(10) . . . . ? C8 C9 C10 C11 -4.6(11) . . . . ? C9 C10 C11 C12 -2.3(11) . . . . ? C10 C11 C12 C7 3.3(9) . . . . ? C8' C7 C12 C11 -11.9(9) . . . . ? C8 C7 C12 C11 2.3(8) . . . . ? C12' C7 C12 C11 52.8(12) . . . . ? Si1 C7 C12 C11 -179.9(5) . . . . ? C8 C7 C8' C9' -41(2) . . . . ? C12 C7 C8' C9' 37.4(14) . . . . ? C12' C7 C8' C9' 1.0(15) . . . . ? Si1 C7 C8' C9' -155.7(10) . . . . ? C7 C8' C9' C10' -26.6(19) . . . . ? C8' C9' C10' C11' 21(3) . . . . ? C9' C10' C11' C12' 9(3) . . . . ? C10' C11' C12' C7 -47(4) . . . . ? C8' C7 C12' C11' 38(3) . . . . ? C8 C7 C12' C11' 46(3) . . . . ? C12 C7 C12' C11' -92(3) . . . . ? Si1 C7 C12' C11' -169(2) . . . . ? C18 C13 C14 C15 -1.3(5) . . . . ? Si1 C13 C14 C15 174.4(3) . . . . ? C13 C14 C15 C16 0.1(6) . . . . ? C14 C15 C16 C17 0.9(6) . . . . ? C15 C16 C17 C18 -0.5(6) . . . . ? C16 C17 C18 C13 -0.8(6) . . . . ? C14 C13 C18 C17 1.7(5) . . . . ? Si1 C13 C18 C17 -174.0(3) . . . . ? C28 C19 C20 C21 -0.6(3) . . . . ? Si1 C19 C20 C21 179.59(19) . . . . ? C19 C20 C21 C26 6.1(4) . . . . ? C19 C20 C21 C22 -173.6(3) . . . . ? C20 C21 C22 C23 179.1(3) . . . . ? C26 C21 C22 C23 -0.7(4) . . . . ? C21 C22 C23 C24 0.0(5) . . . . ? C22 C23 C24 C25 0.8(5) . . . . ? C23 C24 C25 C26 -1.0(4) . . . . ? C24 C25 C26 C21 0.4(4) . . . . ? C24 C25 C26 C27 -175.3(3) . . . . ? C20 C21 C26 C25 -179.3(2) . . . . ? C22 C21 C26 C25 0.5(4) . . . . ? C20 C21 C26 C27 -3.5(4) . . . . ? C22 C21 C26 C27 176.3(2) . . . . ? C25 C26 C27 C28 171.1(2) . . . . ? C21 C26 C27 C28 -4.5(3) . . . . ? C25 C26 C27 C29 -6.6(4) . . . . ? C21 C26 C27 C29 177.7(2) . . . . ? C26 C27 C28 O1 -172.24(19) . . . . ? C29 C27 C28 O1 5.5(3) . . . . ? C26 C27 C28 C19 10.7(3) . . . . ? C29 C27 C28 C19 -171.5(2) . . . . ? C20 C19 C28 C27 -8.2(3) . . . . ? Si1 C19 C28 C27 171.66(18) . . . . ? C20 C19 C28 O1 174.71(19) . . . . ? Si1 C19 C28 O1 -5.5(3) . . . . ? C28 C27 C29 C38 -55.5(3) . . . . ? C26 C27 C29 C38 122.2(3) . . . . ? C28 C27 C29 C30 122.9(3) . . . . ? C26 C27 C29 C30 -59.4(3) . . . . ? C38 C29 C30 C31 172.9(2) . . . . ? C27 C29 C30 C31 -5.6(4) . . . . ? C38 C29 C30 C35 -6.3(3) . . . . ? C27 C29 C30 C35 175.3(2) . . . . ? C29 C30 C31 C32 -178.9(3) . . . . ? C35 C30 C31 C32 0.2(4) . . . . ? C30 C31 C32 C33 -0.9(5) . . . . ? C31 C32 C33 C34 0.5(5) . . . . ? C32 C33 C34 C35 0.6(5) . . . . ? C33 C34 C35 C36 179.6(3) . . . . ? C33 C34 C35 C30 -1.3(5) . . . . ? C31 C30 C35 C36 180.0(3) . . . . ? C29 C30 C35 C36 -0.8(4) . . . . ? C31 C30 C35 C34 0.8(4) . . . . ? C29 C30 C35 C34 -180.0(3) . . . . ? C34 C35 C36 C37 -175.9(3) . . . . ? C30 C35 C36 C37 5.0(4) . . . . ? C35 C36 C37 C38 -1.8(4) . . . . ? C35 C36 C37 Si2 -178.2(2) . . . . ? C30 C29 C38 O2 -174.7(2) . . . . ? C27 C29 C38 O2 3.7(3) . . . . ? C30 C29 C38 C37 10.0(4) . . . . ? C27 C29 C38 C37 -171.6(2) . . . . ? C36 C37 C38 C29 -5.9(4) . . . . ? Si2 C37 C38 C29 170.50(19) . . . . ? C36 C37 C38 O2 178.7(2) . . . . ? Si2 C37 C38 O2 -4.9(3) . . . . ? C44 C39 C40 C41 0.0 . . . . ? Si2 C39 C40 C41 -172.83(13) . . . . ? C39 C40 C41 C42 0.0 . . . . ? C40 C41 C42 C43 0.0 . . . . ? C41 C42 C43 C44 0.0 . . . . ? C42 C43 C44 C39 0.0 . . . . ? C40 C39 C44 C43 0.0 . . . . ? Si2 C39 C44 C43 173.24(13) . . . . ? C44' C39' C40' C41' 0.0 . . . . ? Si2 C39' C40' C41' 178.71(15) . . . . ? C39' C40' C41' C42' 0.0 . . . . ? C40' C41' C42' C43' 0.0 . . . . ? C41' C42' C43' C44' 0.0 . . . . ? C42' C43' C44' C39' 0.0 . . . . ? C40' C39' C44' C43' 0.0 . . . . ? Si2 C39' C44' C43' -178.75(15) . . . . ? C50 C45 C46 C47 -1.6(5) . . . . ? Si2 C45 C46 C47 -179.0(3) . . . . ? C45 C46 C47 C48 0.8(6) . . . . ? C46 C47 C48 C49 0.1(6) . . . . ? C47 C48 C49 C50 -0.2(5) . . . . ? C46 C45 C50 C49 1.4(5) . . . . ? Si2 C45 C50 C49 178.9(2) . . . . ? C48 C49 C50 C45 -0.5(5) . . . . ? C56 C51 C52 C53 0.0 . . . . ? Si2 C51 C52 C53 179.3(3) . . . . ? C51 C52 C53 C54 0.0 . . . . ? C52 C53 C54 C55 0.0 . . . . ? C53 C54 C55 C56 0.0 . . . . ? C54 C55 C56 C51 0.0 . . . . ? C52 C51 C56 C55 0.0 . . . . ? Si2 C51 C56 C55 -179.4(2) . . . . ? C56' C51' C52' C53' 0.0 . . . . ? Si2 C51' C52' C53' -170.1(2) . . . . ? C51' C52' C53' C54' 0.0 . . . . ? C51' C52' C53' C53' 121.4(3) . . . 2_665 ? C52' C53' C54' C55' 0.0 . . . . ? C53' C53' C54' C55' -131.71(19) 2_665 . . . ? C53' C54' C55' C56' 0.0 . . . . ? C54' C55' C56' C51' 0.0 . . . . ? C52' C51' C56' C55' 0.0 . . . . ? Si2 C51' C56' C55' 170.3(2) . . . . ? C27 C28 O1 P1 69.0(2) . . . . ? C19 C28 O1 P1 -113.76(19) . . . . ? C29 C38 O2 P1 69.6(3) . . . . ? C37 C38 O2 P1 -114.8(2) . . . . ? O3 Ag1 O3 P1 1.44(12) 2_675 . . . ? Ag2 Ag1 O3 P1 1.44(12) . . . . ? O4 Ag2 O4 P1 2.37(12) 2_675 . . . ? Ag1 Ag2 O4 P1 2.38(12) . . . . ? Ag2 O4 P1 O3 -2.10(18) . . . . ? Ag2 O4 P1 O2 120.42(12) . . . . ? Ag2 O4 P1 O1 -128.64(11) . . . . ? Ag1 O3 P1 O4 -0.20(18) . . . . ? Ag1 O3 P1 O2 -126.00(12) . . . . ? Ag1 O3 P1 O1 122.52(12) . . . . ? C38 O2 P1 O4 66.84(19) . . . . ? C38 O2 P1 O3 -161.60(17) . . . . ? C38 O2 P1 O1 -44.22(18) . . . . ? C28 O1 P1 O4 -161.65(15) . . . . ? C28 O1 P1 O3 66.55(17) . . . . ? C28 O1 P1 O2 -45.30(16) . . . . ? C8' C7 Si1 C13 130.1(6) . . . . ? C8 C7 Si1 C13 115.7(4) . . . . ? C12 C7 Si1 C13 -62.0(4) . . . . ? C12' C7 Si1 C13 -18.5(14) . . . . ? C8' C7 Si1 C19 10.6(6) . . . . ? C8 C7 Si1 C19 -3.8(5) . . . . ? C12 C7 Si1 C19 178.5(3) . . . . ? C12' C7 Si1 C19 -138.0(14) . . . . ? C8' C7 Si1 C1 -112.1(6) . . . . ? C8 C7 Si1 C1 -126.5(4) . . . . ? C12 C7 Si1 C1 55.8(4) . . . . ? C12' C7 Si1 C1 99.3(14) . . . . ? C14 C13 Si1 C7 -57.5(3) . . . . ? C18 C13 Si1 C7 118.0(3) . . . . ? C14 C13 Si1 C19 64.5(3) . . . . ? C18 C13 Si1 C19 -120.0(3) . . . . ? C14 C13 Si1 C1 -178.3(3) . . . . ? C18 C13 Si1 C1 -2.8(3) . . . . ? C20 C19 Si1 C7 129.7(2) . . . . ? C28 C19 Si1 C7 -50.1(2) . . . . ? C20 C19 Si1 C13 12.4(2) . . . . ? C28 C19 Si1 C13 -167.39(19) . . . . ? C20 C19 Si1 C1 -105.0(2) . . . . ? C28 C19 Si1 C1 75.2(2) . . . . ? C6 C1 Si1 C7 -9.5(3) . . . . ? C2 C1 Si1 C7 171.2(2) . . . . ? C6 C1 Si1 C13 106.7(3) . . . . ? C2 C1 Si1 C13 -72.6(3) . . . . ? C6 C1 Si1 C19 -135.2(3) . . . . ? C2 C1 Si1 C19 45.6(3) . . . . ? C40' C39' Si2 C51' 125.88(18) . . . . ? C44' C39' Si2 C51' -55.39(18) . . . . ? C40' C39' Si2 C45 -119.71(16) . . . . ? C44' C39' Si2 C45 59.02(17) . . . . ? C40' C39' Si2 C37 9.36(18) . . . . ? C44' C39' Si2 C37 -171.91(15) . . . . ? C40' C39' Si2 C51 124.53(17) . . . . ? C44' C39' Si2 C51 -56.74(18) . . . . ? C40' C39' Si2 C39 -40.27(5) . . . . ? C44' C39' Si2 C39 138.46(14) . . . . ? C52' C51' Si2 C39' 117.6(2) . . . . ? C56' C51' Si2 C39' -52.6(2) . . . . ? C52' C51' Si2 C45 1.5(3) . . . . ? C56' C51' Si2 C45 -168.7(2) . . . . ? C52' C51' Si2 C37 -124.7(2) . . . . ? C56' C51' Si2 C37 65.1(2) . . . . ? C52' C51' Si2 C51 -67.47(12) . . . . ? C56' C51' Si2 C51 122.29(13) . . . . ? C52' C51' Si2 C39 120.2(2) . . . . ? C56' C51' Si2 C39 -50.1(2) . . . . ? C50 C45 Si2 C39' 177.4(2) . . . . ? C46 C45 Si2 C39' -5.2(3) . . . . ? C50 C45 Si2 C51' -81.7(3) . . . . ? C46 C45 Si2 C51' 95.7(3) . . . . ? C50 C45 Si2 C37 46.2(3) . . . . ? C46 C45 Si2 C37 -136.5(3) . . . . ? C50 C45 Si2 C51 -67.3(3) . . . . ? C46 C45 Si2 C51 110.0(3) . . . . ? C50 C45 Si2 C39 166.4(2) . . . . ? C46 C45 Si2 C39 -16.2(3) . . . . ? C36 C37 Si2 C39' 118.3(2) . . . . ? C38 C37 Si2 C39' -58.0(2) . . . . ? C36 C37 Si2 C51' 16.0(3) . . . . ? C38 C37 Si2 C51' -160.3(2) . . . . ? C36 C37 Si2 C45 -111.0(2) . . . . ? C38 C37 Si2 C45 72.7(2) . . . . ? C36 C37 Si2 C51 3.1(3) . . . . ? C38 C37 Si2 C51 -173.2(2) . . . . ? C36 C37 Si2 C39 126.7(2) . . . . ? C38 C37 Si2 C39 -49.6(2) . . . . ? C52 C51 Si2 C39' 154.2(2) . . . . ? C56 C51 Si2 C39' -26.5(2) . . . . ? C52 C51 Si2 C51' 148.92(10) . . . . ? C56 C51 Si2 C51' -31.75(17) . . . . ? C52 C51 Si2 C45 33.2(3) . . . . ? C56 C51 Si2 C45 -147.5(2) . . . . ? C52 C51 Si2 C37 -84.0(2) . . . . ? C56 C51 Si2 C37 95.4(2) . . . . ? C52 C51 Si2 C39 157.2(2) . . . . ? C56 C51 Si2 C39 -23.5(2) . . . . ? C40 C39 Si2 C39' 124.03(8) . . . . ? C44 C39 Si2 C39' -49.01(15) . . . . ? C40 C39 Si2 C51' 109.93(18) . . . . ? C44 C39 Si2 C51' -63.11(19) . . . . ? C40 C39 Si2 C45 -131.15(15) . . . . ? C44 C39 Si2 C45 55.82(16) . . . . ? C40 C39 Si2 C37 -9.41(16) . . . . ? C44 C39 Si2 C37 177.55(14) . . . . ? C40 C39 Si2 C51 107.78(18) . . . . ? C44 C39 Si2 C51 -65.26(19) . . . . ? C1H C2H C3H C4H 45.1 . . . . ? C2H C3H C4H C5H 34.6 . . . . ? C3H C4H C5H C6H -118.9 . . . . ? C1H' C2H' C3H' C4H' 96.4 . . . . ? C2H' C3H' C4H' C5H' -146.5 . . . . ? C3H' C4H' C5H' C6H' 148.0 . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 36.51 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.835 _refine_diff_density_min -0.881 _refine_diff_density_rms 0.161