# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'R Puddephatt' 'Dana Eisler' 'Nasser Nasser' _publ_contact_author_name 'R Puddephatt' _publ_contact_author_email PUDD@UWO.CA _publ_section_title ; A Chiral Diphosphine as trans-Chelate Ligand and its Relevance to Catalysis ; # Attachment '2a.cif' data_2a _database_code_depnum_ccdc_archive 'CCDC 755022' #TrackingRef '2a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H40 Au Cl N2 O2 P2, 1.5 (C H2 Cl2), 0.5 (O)' _chemical_formula_sum 'C45.50 H43 Au Cl4 N2 O2.50 P2' _chemical_formula_weight 1058.53 _chemical_absolute_configuration syn loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P 1' _symmetry_space_group_name_Hall 'P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 11.493(2) _cell_length_b 11.622(2) _cell_length_c 17.518(4) _cell_angle_alpha 90.48(3) _cell_angle_beta 104.77(3) _cell_angle_gamma 97.51(3) _cell_volume 2241.1(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1054 _exptl_absorpt_coefficient_mu 3.632 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5303 _exptl_absorpt_correction_T_max 0.8988 _exptl_absorpt_process_details 'Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; Only the heavier atoms (gold, phosphorus and chlorine) were refined with anisotropic thermal displacement parameters. The molecule of adventitious water was refined as a single isotropic oxygen atom. There was a very poorly ordered dichloromethane molecule in the lattice with was refined as a 50:50 isotropic mixture. The poor ordering of this molecule resulted in a somewhat short H...H secondary contact. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_reflns_number 10535 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0621 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 25.03 _reflns_number_total 10535 _reflns_number_gt 9486 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _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^)+(0.0493P)^2^+32.0981P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 3531 Friedel Pairs' _refine_ls_abs_structure_Flack 0.058(11) _refine_ls_number_reflns 10535 _refine_ls_number_parameters 430 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.1408 _refine_ls_wR_factor_gt 0.1345 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.022 _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 0.95723(4) 0.77921(4) 0.31052(3) 0.0269(2) Uani 1 1 d . . . Cl1 Cl 0.6422(4) 0.2951(4) 0.0550(2) 0.0416(10) Uani 1 1 d . . . P1 P 1.1128(5) 0.6716(5) 0.3077(3) 0.0242(13) Uani 1 1 d . . . P2 P 0.8311(5) 0.9188(5) 0.3063(4) 0.0244(13) Uani 1 1 d . . . C1 C 1.0850(14) 0.5832(15) 0.2190(10) 0.022(4) Uiso 1 1 d . . . C2 C 1.1667(14) 0.5876(15) 0.1724(9) 0.028(4) Uiso 1 1 d . . . H2A H 1.2405 0.6392 0.1889 0.033 Uiso 1 1 calc R . . C3 C 1.1466(14) 0.5217(15) 0.1036(10) 0.032(4) Uiso 1 1 d . . . H3A H 1.2052 0.5290 0.0737 0.039 Uiso 1 1 calc R . . C4 C 1.0418(15) 0.4454(16) 0.0783(10) 0.033(4) Uiso 1 1 d . . . H4A H 1.0303 0.3976 0.0320 0.040 Uiso 1 1 calc R . . C5 C 0.9498(17) 0.4359(17) 0.1196(11) 0.032(5) Uiso 1 1 d . . . H5A H 0.8757 0.3857 0.1000 0.038 Uiso 1 1 calc R . . C6 C 0.9714(16) 0.5034(17) 0.1909(11) 0.026(5) Uiso 1 1 d . . . C7 C 0.8860(15) 0.4938(15) 0.2399(10) 0.025(4) Uiso 1 1 d . . . O1 O 0.9268(9) 0.5245(9) 0.3120(6) 0.028(3) Uiso 1 1 d . . . N1 N 0.7673(11) 0.4599(11) 0.2086(8) 0.023(3) Uiso 1 1 d . . . H1A H 0.7412 0.4459 0.1572 0.027 Uiso 1 1 calc R . . C8 C 0.6799(12) 0.4453(12) 0.2556(8) 0.021(3) Uiso 1 1 d . . . H8A H 0.7148 0.4952 0.3049 0.025 Uiso 1 1 calc R . . C9 C 0.6580(16) 0.3194(16) 0.2804(10) 0.029(4) Uiso 1 1 d . . . H9A H 0.6319 0.2670 0.2325 0.035 Uiso 1 1 calc R . . H9B H 0.7354 0.2980 0.3131 0.035 Uiso 1 1 calc R . . C10 C 0.5631(13) 0.3014(14) 0.3266(9) 0.029(3) Uiso 1 1 d . . . H10A H 0.5442 0.2174 0.3343 0.035 Uiso 1 1 calc R . . H10B H 0.5958 0.3412 0.3793 0.035 Uiso 1 1 calc R . . C11 C 0.4486(13) 0.3475(13) 0.2848(9) 0.032(4) Uiso 1 1 d . . . H11A H 0.4086 0.2975 0.2368 0.038 Uiso 1 1 calc R . . H11B H 0.3928 0.3415 0.3198 0.038 Uiso 1 1 calc R . . C12 C 0.4658(15) 0.4669(15) 0.2618(10) 0.031(4) Uiso 1 1 d . . . H12A H 0.4922 0.5190 0.3099 0.037 Uiso 1 1 calc R . . H12B H 0.3873 0.4870 0.2301 0.037 Uiso 1 1 calc R . . C13 C 0.5619(12) 0.4878(13) 0.2128(9) 0.026(3) Uiso 1 1 d . . . H13A H 0.5289 0.4382 0.1631 0.031 Uiso 1 1 calc R . . N2 N 0.5761(11) 0.6083(11) 0.1887(8) 0.025(3) Uiso 1 1 d . . . H2B H 0.5517 0.6203 0.1379 0.030 Uiso 1 1 calc R . . C14 C 0.6232(13) 0.7016(15) 0.2375(9) 0.022(3) Uiso 1 1 d . . . O2 O 0.6789(9) 0.6981(10) 0.3069(6) 0.031(3) Uiso 1 1 d . . . C15 C 0.6065(13) 0.8159(13) 0.2003(9) 0.019(4) Uiso 1 1 d . . . C16 C 0.5004(14) 0.8277(14) 0.1424(9) 0.028(4) Uiso 1 1 d . . . H16A H 0.4405 0.7619 0.1253 0.033 Uiso 1 1 calc R . . C17 C 0.4811(15) 0.9319(14) 0.1098(10) 0.034(4) Uiso 1 1 d . . . H17A H 0.4082 0.9365 0.0702 0.041 Uiso 1 1 calc R . . C18 C 0.5622(13) 1.0289(14) 0.1322(9) 0.029(3) Uiso 1 1 d . . . H18A H 0.5447 1.1007 0.1096 0.034 Uiso 1 1 calc R . . C19 C 0.6704(14) 1.0238(14) 0.1879(9) 0.029(4) Uiso 1 1 d . . . H19A H 0.7297 1.0908 0.2016 0.034 Uiso 1 1 calc R . . C20 C 0.6925(15) 0.9162(16) 0.2248(10) 0.029(4) Uiso 1 1 d . . . C21 C 1.1707(11) 0.5850(10) 0.3926(6) 0.030(4) Uiso 1 1 d G . . C22 C 1.1388(10) 0.5964(9) 0.4634(7) 0.033(4) Uiso 1 1 d G . . H22A H 1.0889 0.6530 0.4697 0.040 Uiso 1 1 calc R . . C23 C 1.1799(11) 0.5251(10) 0.5250(5) 0.038(4) Uiso 1 1 d G . . H23A H 1.1581 0.5330 0.5734 0.045 Uiso 1 1 calc R . . C24 C 1.2530(11) 0.4424(10) 0.5159(6) 0.041(5) Uiso 1 1 d G . . H24A H 1.2811 0.3937 0.5580 0.049 Uiso 1 1 calc R . . C25 C 1.2849(11) 0.4309(10) 0.4451(7) 0.043(5) Uiso 1 1 d G . . H25A H 1.3348 0.3744 0.4388 0.051 Uiso 1 1 calc R . . C26 C 1.2438(11) 0.5022(11) 0.3834(6) 0.034(5) Uiso 1 1 d G . . H26A H 1.2656 0.4944 0.3351 0.041 Uiso 1 1 calc R . . C27 C 1.2435(8) 0.7759(8) 0.3049(6) 0.024(4) Uiso 1 1 d G . . C28 C 1.2204(6) 0.8726(9) 0.2603(6) 0.029(3) Uiso 1 1 d G . . H28A H 1.1397 0.8799 0.2316 0.035 Uiso 1 1 calc R . . C29 C 1.3152(8) 0.9586(7) 0.2576(6) 0.034(4) Uiso 1 1 d G . . H29A H 1.2993 1.0247 0.2271 0.041 Uiso 1 1 calc R . . C30 C 1.4332(7) 0.9480(8) 0.2995(6) 0.031(4) Uiso 1 1 d G . . H30A H 1.4980 1.0068 0.2977 0.037 Uiso 1 1 calc R . . C31 C 1.4564(7) 0.8512(9) 0.3441(6) 0.031(4) Uiso 1 1 d G . . H31A H 1.5370 0.8439 0.3728 0.037 Uiso 1 1 calc R . . C32 C 1.3615(9) 0.7652(8) 0.3468(6) 0.030(4) Uiso 1 1 d G . . H32A H 1.3774 0.6991 0.3773 0.036 Uiso 1 1 calc R . . C33 C 0.9254(10) 1.0531(9) 0.2892(7) 0.031(4) Uiso 1 1 d G . . C34 C 0.9532(11) 1.1514(11) 0.3397(6) 0.036(4) Uiso 1 1 d G . . H34A H 0.9215 1.1524 0.3847 0.043 Uiso 1 1 calc R . . C35 C 1.0272(12) 1.2480(9) 0.3243(7) 0.051(6) Uiso 1 1 d G . . H35A H 1.0462 1.3152 0.3588 0.061 Uiso 1 1 calc R . . C36 C 1.0736(11) 1.2465(9) 0.2584(8) 0.060(6) Uiso 1 1 d G . . H36A H 1.1242 1.3126 0.2479 0.072 Uiso 1 1 calc R . . C37 C 1.0458(11) 1.1483(11) 0.2079(6) 0.055(5) Uiso 1 1 d G . . H37A H 1.0775 1.1472 0.1629 0.067 Uiso 1 1 calc R . . C38 C 0.9718(11) 1.0516(9) 0.2233(6) 0.050(5) Uiso 1 1 d G . . H38A H 0.9528 0.9845 0.1888 0.060 Uiso 1 1 calc R . . C39 C 0.7887(10) 0.9468(10) 0.3968(5) 0.025(4) Uiso 1 1 d G . . C40 C 0.7303(11) 1.0418(9) 0.4052(6) 0.029(4) Uiso 1 1 d G . . H40A H 0.7109 1.0923 0.3629 0.035 Uiso 1 1 calc R . . C41 C 0.7004(11) 1.0630(9) 0.4756(7) 0.042(4) Uiso 1 1 d G . . H41A H 0.6606 1.1279 0.4814 0.051 Uiso 1 1 calc R . . C42 C 0.7289(11) 0.9891(10) 0.5376(5) 0.050(5) Uiso 1 1 d G . . H42A H 0.7085 1.0035 0.5858 0.059 Uiso 1 1 calc R . . C43 C 0.7872(10) 0.8941(9) 0.5292(5) 0.034(4) Uiso 1 1 d G . . H43A H 0.8067 0.8436 0.5716 0.041 Uiso 1 1 calc R . . C44 C 0.8171(9) 0.8729(8) 0.4588(6) 0.034(4) Uiso 1 1 d G . . H44A H 0.8570 0.8080 0.4531 0.041 Uiso 1 1 calc R . . Au2 Au 0.04286(4) 0.22065(4) 0.68933(3) 0.0269(2) Uani 1 1 d . . . Cl2 Cl 0.3941(3) 0.6044(4) 0.0016(2) 0.0392(10) Uani 1 1 d . . . P3 P -0.0958(5) 0.3431(5) 0.6972(4) 0.0254(14) Uani 1 1 d . . . P4 P 0.1510(5) 0.0661(5) 0.6901(3) 0.0263(12) Uani 1 1 d . . . C45 C -0.0669(15) 0.4457(15) 0.7854(10) 0.024(4) Uiso 1 1 d . . . C46 C -0.1618(15) 0.4521(16) 0.8206(10) 0.033(4) Uiso 1 1 d . . . H46A H -0.2384 0.4064 0.7992 0.039 Uiso 1 1 calc R . . C47 C -0.1450(15) 0.5246(16) 0.8864(10) 0.036(4) Uiso 1 1 d . . . H47A H -0.2085 0.5259 0.9119 0.043 Uiso 1 1 calc R . . C48 C -0.0352(15) 0.5955(17) 0.9152(11) 0.037(5) Uiso 1 1 d . . . H48A H -0.0241 0.6482 0.9590 0.044 Uiso 1 1 calc R . . C49 C 0.0559(16) 0.5889(16) 0.8801(11) 0.026(5) Uiso 1 1 d . . . H49A H 0.1311 0.6373 0.9003 0.032 Uiso 1 1 calc R . . C50 C 0.0433(16) 0.5133(16) 0.8154(11) 0.024(4) Uiso 1 1 d . . . C51 C 0.1430(15) 0.5172(14) 0.7712(10) 0.022(4) Uiso 1 1 d . . . O3 O 0.1168(9) 0.4932(9) 0.7004(6) 0.027(3) Uiso 1 1 d . . . N3 N 0.2570(11) 0.5554(11) 0.8156(8) 0.024(3) Uiso 1 1 d . . . H3B H 0.2663 0.5659 0.8667 0.029 Uiso 1 1 calc R . . C52 C 0.3657(12) 0.5805(12) 0.7870(8) 0.021(3) Uiso 1 1 d . . . H52A H 0.4364 0.5986 0.8343 0.026 Uiso 1 1 calc R . . C53 C 0.3574(15) 0.6904(16) 0.7382(10) 0.028(4) Uiso 1 1 d . . . H53A H 0.3423 0.7548 0.7701 0.033 Uiso 1 1 calc R . . H53B H 0.2882 0.6753 0.6906 0.033 Uiso 1 1 calc R . . C54 C 0.4783(14) 0.7270(14) 0.7122(10) 0.035(4) Uiso 1 1 d . . . H54A H 0.4696 0.7956 0.6792 0.042 Uiso 1 1 calc R . . H54B H 0.5464 0.7487 0.7597 0.042 Uiso 1 1 calc R . . C55 C 0.5055(14) 0.6293(14) 0.6666(9) 0.033(4) Uiso 1 1 d . . . H55A H 0.5839 0.6522 0.6535 0.039 Uiso 1 1 calc R . . H55B H 0.4415 0.6137 0.6164 0.039 Uiso 1 1 calc R . . C56 C 0.5122(13) 0.5157(14) 0.7143(9) 0.022(3) Uiso 1 1 d . . . H56A H 0.5262 0.4518 0.6814 0.026 Uiso 1 1 calc R . . H56B H 0.5809 0.5285 0.7622 0.026 Uiso 1 1 calc R . . C57 C 0.3938(12) 0.4824(12) 0.7379(8) 0.023(3) Uiso 1 1 d . . . H57A H 0.3260 0.4658 0.6888 0.028 Uiso 1 1 calc R . . N4 N 0.4015(11) 0.3781(12) 0.7829(8) 0.027(3) Uiso 1 1 d . . . H4B H 0.4395 0.3848 0.8334 0.032 Uiso 1 1 calc R . . C58 C 0.3527(13) 0.2714(14) 0.7505(9) 0.022(4) Uiso 1 1 d . . . O4 O 0.3010(9) 0.2583(9) 0.6783(6) 0.025(2) Uiso 1 1 d . . . C59 C 0.3659(15) 0.1679(16) 0.8001(10) 0.030(4) Uiso 1 1 d . . . C60 C 0.4608(14) 0.1698(14) 0.8656(9) 0.025(4) Uiso 1 1 d . . . H60A H 0.5172 0.2384 0.8812 0.030 Uiso 1 1 calc R . . C61 C 0.4752(14) 0.0689(13) 0.9102(9) 0.030(4) Uiso 1 1 d . . . H61A H 0.5423 0.0688 0.9549 0.036 Uiso 1 1 calc R . . C62 C 0.3902(13) -0.0294(14) 0.8878(9) 0.032(4) Uiso 1 1 d . . . H62A H 0.3987 -0.0978 0.9168 0.038 Uiso 1 1 calc R . . C63 C 0.2928(15) -0.0267(15) 0.8226(10) 0.033(4) Uiso 1 1 d . . . H63A H 0.2327 -0.0930 0.8087 0.039 Uiso 1 1 calc R . . C64 C 0.2807(14) 0.0712(15) 0.7768(9) 0.024(4) Uiso 1 1 d . . . C65 C -0.1511(10) 0.4227(10) 0.6108(5) 0.024(4) Uiso 1 1 d G . . C66 C -0.2383(10) 0.4959(11) 0.6084(5) 0.032(5) Uiso 1 1 d G . . H66A H -0.2699 0.5048 0.6529 0.039 Uiso 1 1 calc R . . C67 C -0.2794(9) 0.5562(10) 0.5407(6) 0.031(4) Uiso 1 1 d G . . H67A H -0.3390 0.6062 0.5390 0.037 Uiso 1 1 calc R . . C68 C -0.2333(10) 0.5432(10) 0.4756(5) 0.028(4) Uiso 1 1 d G . . H68A H -0.2614 0.5844 0.4294 0.034 Uiso 1 1 calc R . . C69 C -0.1461(10) 0.4700(10) 0.4781(5) 0.041(5) Uiso 1 1 d G . . H69A H -0.1146 0.4612 0.4336 0.050 Uiso 1 1 calc R . . C70 C -0.1050(9) 0.4097(9) 0.5457(6) 0.030(4) Uiso 1 1 d G . . H70A H -0.0454 0.3597 0.5474 0.036 Uiso 1 1 calc R . . C71 C -0.2293(8) 0.2417(9) 0.7069(7) 0.032(4) Uiso 1 1 d G . . C72 C -0.3412(10) 0.2294(10) 0.6514(6) 0.037(5) Uiso 1 1 d G . . H72A H -0.3535 0.2776 0.6073 0.044 Uiso 1 1 calc R . . C73 C -0.4350(8) 0.1466(11) 0.6603(6) 0.046(5) Uiso 1 1 d G . . H73A H -0.5115 0.1381 0.6223 0.055 Uiso 1 1 calc R . . C74 C -0.4170(9) 0.0760(10) 0.7248(7) 0.049(5) Uiso 1 1 d G . . H74A H -0.4811 0.0194 0.7309 0.059 Uiso 1 1 calc R . . C75 C -0.3051(10) 0.0883(10) 0.7803(6) 0.054(5) Uiso 1 1 d G . . H75A H -0.2928 0.0401 0.8244 0.065 Uiso 1 1 calc R . . C76 C -0.2113(8) 0.1711(10) 0.7714(6) 0.037(4) Uiso 1 1 d G . . H76A H -0.1348 0.1795 0.8094 0.045 Uiso 1 1 calc R . . C77 C 0.0511(9) -0.0666(8) 0.7009(7) 0.033(4) Uiso 1 1 d G . . C78 C -0.0282(10) -0.0540(8) 0.7476(7) 0.040(4) Uiso 1 1 d G . . H78A H -0.0293 0.0200 0.7706 0.048 Uiso 1 1 calc R . . C79 C -0.1059(10) -0.1497(10) 0.7605(7) 0.053(5) Uiso 1 1 d G . . H79A H -0.1601 -0.1411 0.7923 0.064 Uiso 1 1 calc R . . C80 C -0.1042(10) -0.2580(8) 0.7267(7) 0.042(4) Uiso 1 1 d G . . H80A H -0.1573 -0.3234 0.7355 0.050 Uiso 1 1 calc R . . C81 C -0.0250(11) -0.2705(8) 0.6800(7) 0.039(5) Uiso 1 1 d G . . H81A H -0.0239 -0.3445 0.6570 0.046 Uiso 1 1 calc R . . C82 C 0.0527(10) -0.1748(10) 0.6671(6) 0.038(4) Uiso 1 1 d G . . H82A H 0.1069 -0.1834 0.6352 0.045 Uiso 1 1 calc R . . C83 C 0.2032(10) 0.0328(10) 0.6037(5) 0.026(4) Uiso 1 1 d G . . C84 C 0.1632(10) 0.0881(9) 0.5337(6) 0.039(4) Uiso 1 1 d G . . H84A H 0.1087 0.1437 0.5309 0.047 Uiso 1 1 calc R . . C85 C 0.2030(11) 0.0622(11) 0.4678(5) 0.050(5) Uiso 1 1 d G . . H85A H 0.1757 0.1000 0.4200 0.060 Uiso 1 1 calc R . . C86 C 0.2829(11) -0.0190(11) 0.4720(6) 0.047(5) Uiso 1 1 d G . . H86A H 0.3101 -0.0367 0.4269 0.056 Uiso 1 1 calc R . . C87 C 0.3229(10) -0.0743(10) 0.5420(7) 0.043(5) Uiso 1 1 d G . . H87A H 0.3774 -0.1299 0.5448 0.052 Uiso 1 1 calc R . . C88 C 0.2830(11) -0.0484(10) 0.6079(5) 0.035(4) Uiso 1 1 d G . . H88A H 0.3104 -0.0862 0.6557 0.043 Uiso 1 1 calc R . . C89 C 0.3110(17) 0.2918(19) 0.9992(11) 0.054(5) Uiso 1 1 d . . . H89A H 0.3825 0.2711 0.9833 0.064 Uiso 1 1 calc R . . H89B H 0.3307 0.3731 1.0207 0.064 Uiso 1 1 calc R . . Cl3 Cl 0.2825(8) 0.2015(10) 1.0721(5) 0.092(3) Uani 1 1 d . . . Cl4 Cl 0.1856(7) 0.2818(8) 0.9151(5) 0.072(2) Uani 1 1 d . . . C90 C 0.6921(18) 0.783(2) 0.0206(12) 0.062(6) Uiso 1 1 d . . . H90A H 0.6141 0.7369 0.0220 0.074 Uiso 1 1 calc R . . H90B H 0.6938 0.8620 0.0434 0.074 Uiso 1 1 calc R . . Cl5 Cl 0.6992(7) 0.7944(8) -0.0784(5) 0.076(2) Uani 1 1 d . . . Cl6 Cl 0.8132(8) 0.7181(8) 0.0794(5) 0.074(2) Uani 1 1 d . . . O5 O 0.5645(9) 0.4665(9) 0.9300(6) 0.038(3) Uiso 1 1 d . . . C91 C 1.057(6) 0.961(6) 0.060(2) 0.147(5) Uiso 0.50 1 d PD A 1 H91A H 1.1132 1.0250 0.0929 0.176 Uiso 0.50 1 calc PR A 1 H91B H 1.0024 0.9259 0.0912 0.176 Uiso 0.50 1 calc PR A 1 Cl7 Cl 0.968(2) 1.022(2) -0.0243(13) 0.147(5) Uiso 0.50 1 d PD A 1 Cl8 Cl 1.1430(19) 0.8561(19) 0.0406(13) 0.146(5) Uiso 0.50 1 d PD A 1 C91A C 0.990(7) 0.984(6) 0.028(3) 0.146(5) Uiso 0.50 1 d PD B 2 H91C H 0.9295 0.9216 0.0384 0.175 Uiso 0.50 1 calc PR B 2 H91D H 1.0374 1.0232 0.0786 0.175 Uiso 0.50 1 calc PR B 2 Cl7A Cl 0.915(2) 1.086(2) -0.0366(14) 0.147(5) Uiso 0.50 1 d PD B 2 Cl8A Cl 1.0881(19) 0.9252(19) -0.0225(14) 0.146(5) Uiso 0.50 1 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.0247(4) 0.0222(5) 0.0361(5) 0.0033(4) 0.0107(4) 0.0062(3) Cl1 0.041(2) 0.037(2) 0.039(2) 0.0038(18) 0.0007(19) -0.0035(18) P1 0.022(2) 0.023(3) 0.027(3) 0.003(2) 0.004(2) 0.006(2) P2 0.017(2) 0.020(3) 0.038(3) 0.003(2) 0.009(2) 0.0073(18) Au2 0.0236(4) 0.0258(5) 0.0338(5) 0.0045(4) 0.0096(3) 0.0078(3) Cl2 0.0317(19) 0.050(3) 0.033(2) -0.0065(18) 0.0031(17) 0.0057(18) P3 0.022(2) 0.026(3) 0.034(3) 0.006(2) 0.014(2) 0.012(2) P4 0.034(3) 0.019(3) 0.028(3) 0.005(2) 0.009(2) 0.008(2) Cl3 0.063(4) 0.134(8) 0.064(5) 0.037(5) 0.006(4) -0.020(5) Cl4 0.059(4) 0.084(7) 0.075(5) 0.017(5) 0.014(4) 0.020(4) Cl5 0.080(5) 0.093(6) 0.054(4) 0.013(4) 0.022(4) 0.003(4) Cl6 0.078(5) 0.089(7) 0.067(5) 0.036(5) 0.032(4) 0.025(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 P2 2.303(6) . ? Au1 P1 2.322(6) . ? P1 C1 1.791(17) . ? P1 C27 1.815(9) . ? P1 C21 1.834(10) . ? P2 C39 1.812(10) . ? P2 C20 1.845(18) . ? P2 C33 1.853(11) . ? C1 C2 1.39(2) . ? C1 C6 1.47(2) . ? C2 C3 1.37(2) . ? C2 H2A 0.9500 . ? C3 C4 1.37(2) . ? C3 H3A 0.9500 . ? C4 C5 1.42(3) . ? C4 H4A 0.9500 . ? C5 C6 1.42(3) . ? C5 H5A 0.9500 . ? C6 C7 1.45(3) . ? C7 O1 1.261(19) . ? C7 N1 1.34(2) . ? N1 C8 1.446(18) . ? N1 H1A 0.8800 . ? C8 C13 1.519(19) . ? C8 C9 1.54(2) . ? C8 H8A 1.0000 . ? C9 C10 1.51(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.50(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.45(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.56(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N2 1.467(19) . ? C13 H13A 1.0000 . ? N2 C14 1.34(2) . ? N2 H2B 0.8800 . ? C14 O2 1.224(18) . ? C14 C15 1.50(2) . ? C15 C16 1.40(2) . ? C15 C20 1.41(2) . ? C16 C17 1.36(2) . ? C16 H16A 0.9500 . ? C17 C18 1.35(2) . ? C17 H17A 0.9500 . ? C18 C19 1.38(2) . ? C18 H18A 0.9500 . ? C19 C20 1.44(2) . ? C19 H19A 0.9500 . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C22 H22A 0.9500 . ? C23 C24 1.3900 . ? C23 H23A 0.9500 . ? C24 C25 1.3900 . ? C24 H24A 0.9500 . ? C25 C26 1.3900 . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 C28 1.3900 . ? C27 C32 1.3900 . ? C28 C29 1.3900 . ? C28 H28A 0.9500 . ? C29 C30 1.3900 . ? C29 H29A 0.9500 . ? C30 C31 1.3900 . ? C30 H30A 0.9500 . ? C31 C32 1.3900 . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 C34 1.3900 . ? C33 C38 1.3900 . ? C34 C35 1.3900 . ? C34 H34A 0.9500 . ? C35 C36 1.3900 . ? C35 H35A 0.9500 . ? C36 C37 1.3900 . ? C36 H36A 0.9500 . ? C37 C38 1.3900 . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C40 1.3900 . ? C39 C44 1.3900 . ? C40 C41 1.3900 . ? C40 H40A 0.9500 . ? C41 C42 1.3900 . ? C41 H41A 0.9500 . ? C42 C43 1.3900 . ? C42 H42A 0.9500 . ? C43 C44 1.3900 . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? Au2 P3 2.299(6) . ? Au2 P4 2.312(6) . ? P3 C65 1.799(10) . ? P3 C71 1.853(10) . ? P3 C45 1.878(18) . ? P4 C83 1.820(10) . ? P4 C64 1.832(16) . ? P4 C77 1.840(10) . ? C45 C50 1.38(2) . ? C45 C46 1.39(2) . ? C46 C47 1.38(2) . ? C46 H46A 0.9500 . ? C47 C48 1.39(2) . ? C47 H47A 0.9500 . ? C48 C49 1.35(2) . ? C48 H48A 0.9500 . ? C49 C50 1.39(3) . ? C49 H49A 0.9500 . ? C50 C51 1.53(2) . ? C51 O3 1.220(19) . ? C51 N3 1.36(2) . ? N3 C52 1.457(18) . ? N3 H3B 0.8800 . ? C52 C57 1.537(19) . ? C52 C53 1.54(2) . ? C52 H52A 1.0000 . ? C53 C54 1.58(2) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.49(2) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.57(2) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.524(19) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 N4 1.451(19) . ? C57 H57A 1.0000 . ? N4 C58 1.35(2) . ? N4 H4B 0.8800 . ? C58 O4 1.251(18) . ? C58 C59 1.49(2) . ? C59 C60 1.36(2) . ? C59 C64 1.37(2) . ? C60 C61 1.42(2) . ? C60 H60A 0.9500 . ? C61 C62 1.39(2) . ? C61 H61A 0.9500 . ? C62 C63 1.38(2) . ? C62 H62A 0.9500 . ? C63 C64 1.40(2) . ? C63 H63A 0.9500 . ? C65 C66 1.3900 . ? C65 C70 1.3900 . ? C66 C67 1.3900 . ? C66 H66A 0.9500 . ? C67 C68 1.3900 . ? C67 H67A 0.9500 . ? C68 C69 1.3900 . ? C68 H68A 0.9500 . ? C69 C70 1.3900 . ? C69 H69A 0.9500 . ? C70 H70A 0.9500 . ? C71 C72 1.3900 . ? C71 C76 1.3900 . ? C72 C73 1.3900 . ? C72 H72A 0.9500 . ? C73 C74 1.3900 . ? C73 H73A 0.9500 . ? C74 C75 1.3900 . ? C74 H74A 0.9500 . ? C75 C76 1.3900 . ? C75 H75A 0.9500 . ? C76 H76A 0.9500 . ? C77 C78 1.3900 . ? C77 C82 1.3900 . ? C78 C79 1.3900 . ? C78 H78A 0.9500 . ? C79 C80 1.3900 . ? C79 H79A 0.9500 . ? C80 C81 1.3900 . ? C80 H80A 0.9500 . ? C81 C82 1.3900 . ? C81 H81A 0.9500 . ? C82 H82A 0.9500 . ? C83 C84 1.3900 . ? C83 C88 1.3900 . ? C84 C85 1.3900 . ? C84 H84A 0.9500 . ? C85 C86 1.3900 . ? C85 H85A 0.9500 . ? C86 C87 1.3900 . ? C86 H86A 0.9500 . ? C87 C88 1.3900 . ? C87 H87A 0.9500 . ? C88 H88A 0.9500 . ? C89 Cl3 1.73(2) . ? C89 Cl4 1.77(2) . ? C89 H89A 0.9900 . ? C89 H89B 0.9900 . ? C90 Cl5 1.76(2) . ? C90 Cl6 1.77(2) . ? C90 H90A 0.9900 . ? C90 H90B 0.9900 . ? C91 Cl8 1.75(2) . ? C91 Cl7 1.77(2) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C91A Cl7A 1.79(2) . ? C91A Cl8A 1.79(2) . ? C91A H91C 0.9900 . ? C91A H91D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Au1 P1 167.4(2) . . ? C1 P1 C27 104.0(7) . . ? C1 P1 C21 108.8(7) . . ? C27 P1 C21 103.5(6) . . ? C1 P1 Au1 113.6(6) . . ? C27 P1 Au1 106.2(4) . . ? C21 P1 Au1 119.0(5) . . ? C39 P2 C20 106.7(7) . . ? C39 P2 C33 106.2(6) . . ? C20 P2 C33 102.3(7) . . ? C39 P2 Au1 116.1(4) . . ? C20 P2 Au1 120.5(6) . . ? C33 P2 Au1 103.0(4) . . ? C2 C1 C6 116.5(15) . . ? C2 C1 P1 122.7(13) . . ? C6 C1 P1 120.8(13) . . ? C3 C2 C1 123.7(16) . . ? C3 C2 H2A 118.2 . . ? C1 C2 H2A 118.2 . . ? C4 C3 C2 119.8(16) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? C3 C4 C5 121.6(17) . . ? C3 C4 H4A 119.2 . . ? C5 C4 H4A 119.2 . . ? C6 C5 C4 118.3(17) . . ? C6 C5 H5A 120.8 . . ? C4 C5 H5A 120.8 . . ? C5 C6 C7 122.2(16) . . ? C5 C6 C1 120.0(17) . . ? C7 C6 C1 117.8(15) . . ? O1 C7 N1 121.2(15) . . ? O1 C7 C6 117.6(15) . . ? N1 C7 C6 121.1(15) . . ? C7 N1 C8 122.8(13) . . ? C7 N1 H1A 118.6 . . ? C8 N1 H1A 118.6 . . ? N1 C8 C13 110.9(11) . . ? N1 C8 C9 112.1(12) . . ? C13 C8 C9 111.6(12) . . ? N1 C8 H8A 107.3 . . ? C13 C8 H8A 107.3 . . ? C9 C8 H8A 107.3 . . ? C10 C9 C8 112.8(14) . . ? C10 C9 H9A 109.0 . . ? C8 C9 H9A 109.0 . . ? C10 C9 H9B 109.0 . . ? C8 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? C11 C10 C9 111.6(13) . . ? C11 C10 H10A 109.3 . . ? C9 C10 H10A 109.3 . . ? C11 C10 H10B 109.3 . . ? C9 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C12 C11 C10 114.8(13) . . ? C12 C11 H11A 108.6 . . ? C10 C11 H11A 108.6 . . ? C12 C11 H11B 108.6 . . ? C10 C11 H11B 108.6 . . ? H11A C11 H11B 107.5 . . ? C11 C12 C13 112.4(13) . . ? C11 C12 H12A 109.1 . . ? C13 C12 H12A 109.1 . . ? C11 C12 H12B 109.1 . . ? C13 C12 H12B 109.1 . . ? H12A C12 H12B 107.9 . . ? N2 C13 C8 114.4(11) . . ? N2 C13 C12 111.6(12) . . ? C8 C13 C12 110.8(12) . . ? N2 C13 H13A 106.5 . . ? C8 C13 H13A 106.5 . . ? C12 C13 H13A 106.5 . . ? C14 N2 C13 125.5(13) . . ? C14 N2 H2B 117.3 . . ? C13 N2 H2B 117.3 . . ? O2 C14 N2 124.8(16) . . ? O2 C14 C15 120.4(15) . . ? N2 C14 C15 114.8(13) . . ? C16 C15 C20 117.6(14) . . ? C16 C15 C14 120.2(14) . . ? C20 C15 C14 122.1(13) . . ? C17 C16 C15 121.3(15) . . ? C17 C16 H16A 119.4 . . ? C15 C16 H16A 119.4 . . ? C18 C17 C16 122.1(15) . . ? C18 C17 H17A 118.9 . . ? C16 C17 H17A 118.9 . . ? C17 C18 C19 120.1(15) . . ? C17 C18 H18A 120.0 . . ? C19 C18 H18A 120.0 . . ? C18 C19 C20 119.3(15) . . ? C18 C19 H19A 120.4 . . ? C20 C19 H19A 120.4 . . ? C15 C20 C19 119.6(14) . . ? C15 C20 P2 123.2(13) . . ? C19 C20 P2 117.2(13) . . ? C22 C21 C26 120.0 . . ? C22 C21 P1 121.8(7) . . ? C26 C21 P1 118.1(7) . . ? C21 C22 C23 120.0 . . ? C21 C22 H22A 120.0 . . ? C23 C22 H22A 120.0 . . ? C24 C23 C22 120.0 . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? C23 C24 C25 120.0 . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? C24 C25 C26 120.0 . . ? C24 C25 H25A 120.0 . . ? C26 C25 H25A 120.0 . . ? C25 C26 C21 120.0 . . ? C25 C26 H26A 120.0 . . ? C21 C26 H26A 120.0 . . ? C28 C27 C32 120.0 . . ? C28 C27 P1 116.5(6) . . ? C32 C27 P1 123.4(6) . . ? C29 C28 C27 120.0 . . ? C29 C28 H28A 120.0 . . ? C27 C28 H28A 120.0 . . ? C28 C29 C30 120.0 . . ? C28 C29 H29A 120.0 . . ? C30 C29 H29A 120.0 . . ? C29 C30 C31 120.0 . . ? C29 C30 H30A 120.0 . . ? C31 C30 H30A 120.0 . . ? C30 C31 C32 120.0 . . ? C30 C31 H31A 120.0 . . ? C32 C31 H31A 120.0 . . ? C31 C32 C27 120.0 . . ? C31 C32 H32A 120.0 . . ? C27 C32 H32A 120.0 . . ? C34 C33 C38 120.0 . . ? C34 C33 P2 123.1(7) . . ? C38 C33 P2 116.9(7) . . ? C33 C34 C35 120.0 . . ? C33 C34 H34A 120.0 . . ? C35 C34 H34A 120.0 . . ? C36 C35 C34 120.0 . . ? C36 C35 H35A 120.0 . . ? C34 C35 H35A 120.0 . . ? C35 C36 C37 120.0 . . ? C35 C36 H36A 120.0 . . ? C37 C36 H36A 120.0 . . ? C38 C37 C36 120.0 . . ? C38 C37 H37A 120.0 . . ? C36 C37 H37A 120.0 . . ? C37 C38 C33 120.0 . . ? C37 C38 H38A 120.0 . . ? C33 C38 H38A 120.0 . . ? C40 C39 C44 120.0 . . ? C40 C39 P2 120.9(6) . . ? C44 C39 P2 119.1(6) . . ? C39 C40 C41 120.0 . . ? C39 C40 H40A 120.0 . . ? C41 C40 H40A 120.0 . . ? C40 C41 C42 120.0 . . ? C40 C41 H41A 120.0 . . ? C42 C41 H41A 120.0 . . ? C43 C42 C41 120.0 . . ? C43 C42 H42A 120.0 . . ? C41 C42 H42A 120.0 . . ? C42 C43 C44 120.0 . . ? C42 C43 H43A 120.0 . . ? C44 C43 H43A 120.0 . . ? C43 C44 C39 120.0 . . ? C43 C44 H44A 120.0 . . ? C39 C44 H44A 120.0 . . ? P3 Au2 P4 166.8(2) . . ? C65 P3 C71 105.0(6) . . ? C65 P3 C45 107.3(7) . . ? C71 P3 C45 102.6(7) . . ? C65 P3 Au2 116.7(5) . . ? C71 P3 Au2 103.0(5) . . ? C45 P3 Au2 120.1(6) . . ? C83 P4 C64 107.6(7) . . ? C83 P4 C77 103.9(6) . . ? C64 P4 C77 104.0(7) . . ? C83 P4 Au2 119.6(5) . . ? C64 P4 Au2 112.8(6) . . ? C77 P4 Au2 107.4(4) . . ? C50 C45 C46 120.0(16) . . ? C50 C45 P3 122.3(14) . . ? C46 C45 P3 117.7(13) . . ? C47 C46 C45 120.2(16) . . ? C47 C46 H46A 119.9 . . ? C45 C46 H46A 119.9 . . ? C46 C47 C48 119.9(17) . . ? C46 C47 H47A 120.1 . . ? C48 C47 H47A 120.1 . . ? C49 C48 C47 119.2(17) . . ? C49 C48 H48A 120.4 . . ? C47 C48 H48A 120.4 . . ? C48 C49 C50 122.3(17) . . ? C48 C49 H49A 118.9 . . ? C50 C49 H49A 118.9 . . ? C45 C50 C49 118.3(17) . . ? C45 C50 C51 120.1(16) . . ? C49 C50 C51 121.0(16) . . ? O3 C51 N3 124.5(16) . . ? O3 C51 C50 120.4(15) . . ? N3 C51 C50 115.0(14) . . ? C51 N3 C52 126.4(13) . . ? C51 N3 H3B 116.8 . . ? C52 N3 H3B 116.8 . . ? N3 C52 C57 116.2(12) . . ? N3 C52 C53 109.4(12) . . ? C57 C52 C53 108.9(12) . . ? N3 C52 H52A 107.4 . . ? C57 C52 H52A 107.4 . . ? C53 C52 H52A 107.4 . . ? C52 C53 C54 111.0(13) . . ? C52 C53 H53A 109.4 . . ? C54 C53 H53A 109.4 . . ? C52 C53 H53B 109.4 . . ? C54 C53 H53B 109.4 . . ? H53A C53 H53B 108.0 . . ? C55 C54 C53 110.4(14) . . ? C55 C54 H54A 109.6 . . ? C53 C54 H54A 109.6 . . ? C55 C54 H54B 109.6 . . ? C53 C54 H54B 109.6 . . ? H54A C54 H54B 108.1 . . ? C54 C55 C56 111.8(13) . . ? C54 C55 H55A 109.3 . . ? C56 C55 H55A 109.3 . . ? C54 C55 H55B 109.3 . . ? C56 C55 H55B 109.3 . . ? H55A C55 H55B 107.9 . . ? C57 C56 C55 109.8(12) . . ? C57 C56 H56A 109.7 . . ? C55 C56 H56A 109.7 . . ? C57 C56 H56B 109.7 . . ? C55 C56 H56B 109.7 . . ? H56A C56 H56B 108.2 . . ? N4 C57 C56 109.4(11) . . ? N4 C57 C52 109.6(11) . . ? C56 C57 C52 111.8(12) . . ? N4 C57 H57A 108.7 . . ? C56 C57 H57A 108.7 . . ? C52 C57 H57A 108.7 . . ? C58 N4 C57 122.8(12) . . ? C58 N4 H4B 118.6 . . ? C57 N4 H4B 118.6 . . ? O4 C58 N4 120.3(14) . . ? O4 C58 C59 119.8(14) . . ? N4 C58 C59 119.8(14) . . ? C60 C59 C64 121.8(16) . . ? C60 C59 C58 120.5(15) . . ? C64 C59 C58 117.7(14) . . ? C59 C60 C61 119.8(15) . . ? C59 C60 H60A 120.1 . . ? C61 C60 H60A 120.1 . . ? C62 C61 C60 119.3(14) . . ? C62 C61 H61A 120.3 . . ? C60 C61 H61A 120.3 . . ? C63 C62 C61 119.2(16) . . ? C63 C62 H62A 120.4 . . ? C61 C62 H62A 120.4 . . ? C62 C63 C64 121.6(16) . . ? C62 C63 H63A 119.2 . . ? C64 C63 H63A 119.2 . . ? C59 C64 C63 118.2(15) . . ? C59 C64 P4 123.0(13) . . ? C63 C64 P4 118.8(12) . . ? C66 C65 C70 120.0 . . ? C66 C65 P3 121.3(6) . . ? C70 C65 P3 118.7(6) . . ? C65 C66 C67 120.0 . . ? C65 C66 H66A 120.0 . . ? C67 C66 H66A 120.0 . . ? C68 C67 C66 120.0 . . ? C68 C67 H67A 120.0 . . ? C66 C67 H67A 120.0 . . ? C67 C68 C69 120.0 . . ? C67 C68 H68A 120.0 . . ? C69 C68 H68A 120.0 . . ? C70 C69 C68 120.0 . . ? C70 C69 H69A 120.0 . . ? C68 C69 H69A 120.0 . . ? C69 C70 C65 120.0 . . ? C69 C70 H70A 120.0 . . ? C65 C70 H70A 120.0 . . ? C72 C71 C76 120.0 . . ? C72 C71 P3 123.3(6) . . ? C76 C71 P3 116.6(6) . . ? C71 C72 C73 120.0 . . ? C71 C72 H72A 120.0 . . ? C73 C72 H72A 120.0 . . ? C74 C73 C72 120.0 . . ? C74 C73 H73A 120.0 . . ? C72 C73 H73A 120.0 . . ? C73 C74 C75 120.0 . . ? C73 C74 H74A 120.0 . . ? C75 C74 H74A 120.0 . . ? C76 C75 C74 120.0 . . ? C76 C75 H75A 120.0 . . ? C74 C75 H75A 120.0 . . ? C75 C76 C71 120.0 . . ? C75 C76 H76A 120.0 . . ? C71 C76 H76A 120.0 . . ? C78 C77 C82 120.0 . . ? C78 C77 P4 115.7(6) . . ? C82 C77 P4 124.3(7) . . ? C77 C78 C79 120.0 . . ? C77 C78 H78A 120.0 . . ? C79 C78 H78A 120.0 . . ? C78 C79 C80 120.0 . . ? C78 C79 H79A 120.0 . . ? C80 C79 H79A 120.0 . . ? C81 C80 C79 120.0 . . ? C81 C80 H80A 120.0 . . ? C79 C80 H80A 120.0 . . ? C80 C81 C82 120.0 . . ? C80 C81 H81A 120.0 . . ? C82 C81 H81A 120.0 . . ? C81 C82 C77 120.0 . . ? C81 C82 H82A 120.0 . . ? C77 C82 H82A 120.0 . . ? C84 C83 C88 120.0 . . ? C84 C83 P4 120.2(6) . . ? C88 C83 P4 119.8(6) . . ? C85 C84 C83 120.0 . . ? C85 C84 H84A 120.0 . . ? C83 C84 H84A 120.0 . . ? C86 C85 C84 120.0 . . ? C86 C85 H85A 120.0 . . ? C84 C85 H85A 120.0 . . ? C85 C86 C87 120.0 . . ? C85 C86 H86A 120.0 . . ? C87 C86 H86A 120.0 . . ? C88 C87 C86 120.0 . . ? C88 C87 H87A 120.0 . . ? C86 C87 H87A 120.0 . . ? C87 C88 C83 120.0 . . ? C87 C88 H88A 120.0 . . ? C83 C88 H88A 120.0 . . ? Cl3 C89 Cl4 112.2(11) . . ? Cl3 C89 H89A 109.2 . . ? Cl4 C89 H89A 109.2 . . ? Cl3 C89 H89B 109.2 . . ? Cl4 C89 H89B 109.2 . . ? H89A C89 H89B 107.9 . . ? Cl5 C90 Cl6 112.7(12) . . ? Cl5 C90 H90A 109.1 . . ? Cl6 C90 H90A 109.1 . . ? Cl5 C90 H90B 109.1 . . ? Cl6 C90 H90B 109.1 . . ? H90A C90 H90B 107.8 . . ? Cl8 C91 Cl7 116.0(19) . . ? Cl8 C91 H91A 108.3 . . ? Cl7 C91 H91A 108.3 . . ? Cl8 C91 H91B 108.3 . . ? Cl7 C91 H91B 108.3 . . ? H91A C91 H91B 107.4 . . ? Cl7A C91A Cl8A 106.3(17) . . ? Cl7A C91A H91C 110.5 . . ? Cl8A C91A H91C 110.5 . . ? Cl7A C91A H91D 110.5 . . ? Cl8A C91A H91D 110.5 . . ? H91C C91A H91D 108.7 . . ? 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 P2 Au1 P1 C1 -101.5(12) . . . . ? P2 Au1 P1 C27 12.3(13) . . . . ? P2 Au1 P1 C21 128.4(10) . . . . ? P1 Au1 P2 C39 -120.3(10) . . . . ? P1 Au1 P2 C20 108.3(12) . . . . ? P1 Au1 P2 C33 -4.7(13) . . . . ? C27 P1 C1 C2 11.2(16) . . . . ? C21 P1 C1 C2 -98.6(15) . . . . ? Au1 P1 C1 C2 126.3(13) . . . . ? C27 P1 C1 C6 -167.3(14) . . . . ? C21 P1 C1 C6 82.9(15) . . . . ? Au1 P1 C1 C6 -52.2(16) . . . . ? C6 C1 C2 C3 -1(3) . . . . ? P1 C1 C2 C3 -179.2(14) . . . . ? C1 C2 C3 C4 -1(3) . . . . ? C2 C3 C4 C5 3(3) . . . . ? C3 C4 C5 C6 -3(3) . . . . ? C4 C5 C6 C7 -175.9(17) . . . . ? C4 C5 C6 C1 2(3) . . . . ? C2 C1 C6 C5 0(3) . . . . ? P1 C1 C6 C5 178.6(15) . . . . ? C2 C1 C6 C7 177.9(16) . . . . ? P1 C1 C6 C7 -4(2) . . . . ? C5 C6 C7 O1 156.7(18) . . . . ? C1 C6 C7 O1 -21(3) . . . . ? C5 C6 C7 N1 -27(3) . . . . ? C1 C6 C7 N1 155.2(16) . . . . ? O1 C7 N1 C8 -6(2) . . . . ? C6 C7 N1 C8 177.8(15) . . . . ? C7 N1 C8 C13 141.1(15) . . . . ? C7 N1 C8 C9 -93.5(17) . . . . ? N1 C8 C9 C10 -177.6(13) . . . . ? C13 C8 C9 C10 -52.5(17) . . . . ? C8 C9 C10 C11 50.9(18) . . . . ? C9 C10 C11 C12 -52.3(19) . . . . ? C10 C11 C12 C13 53.0(18) . . . . ? N1 C8 C13 N2 -55.4(16) . . . . ? C9 C8 C13 N2 178.9(12) . . . . ? N1 C8 C13 C12 177.5(12) . . . . ? C9 C8 C13 C12 51.8(17) . . . . ? C11 C12 C13 N2 178.8(12) . . . . ? C11 C12 C13 C8 -52.5(17) . . . . ? C8 C13 N2 C14 -59.5(18) . . . . ? C12 C13 N2 C14 67.3(17) . . . . ? C13 N2 C14 O2 13(2) . . . . ? C13 N2 C14 C15 -169.2(13) . . . . ? O2 C14 C15 C16 -146.2(15) . . . . ? N2 C14 C15 C16 36(2) . . . . ? O2 C14 C15 C20 30(2) . . . . ? N2 C14 C15 C20 -148.1(15) . . . . ? C20 C15 C16 C17 1(2) . . . . ? C14 C15 C16 C17 177.4(15) . . . . ? C15 C16 C17 C18 -1(3) . . . . ? C16 C17 C18 C19 2(3) . . . . ? C17 C18 C19 C20 -4(2) . . . . ? C16 C15 C20 C19 -2(2) . . . . ? C14 C15 C20 C19 -178.9(14) . . . . ? C16 C15 C20 P2 174.7(12) . . . . ? C14 C15 C20 P2 -2(2) . . . . ? C18 C19 C20 C15 4(2) . . . . ? C18 C19 C20 P2 -173.5(12) . . . . ? C39 P2 C20 C15 -85.7(15) . . . . ? C33 P2 C20 C15 163.0(14) . . . . ? Au1 P2 C20 C15 49.7(16) . . . . ? C39 P2 C20 C19 91.5(14) . . . . ? C33 P2 C20 C19 -19.9(15) . . . . ? Au1 P2 C20 C19 -133.2(12) . . . . ? C1 P1 C21 C22 -143.0(8) . . . . ? C27 P1 C21 C22 106.8(8) . . . . ? Au1 P1 C21 C22 -10.7(9) . . . . ? C1 P1 C21 C26 33.9(9) . . . . ? C27 P1 C21 C26 -76.4(8) . . . . ? Au1 P1 C21 C26 166.2(5) . . . . ? C26 C21 C22 C23 0.0 . . . . ? P1 C21 C22 C23 176.8(9) . . . . ? C21 C22 C23 C24 0.0 . . . . ? C22 C23 C24 C25 0.0 . . . . ? C23 C24 C25 C26 0.0 . . . . ? C24 C25 C26 C21 0.0 . . . . ? C22 C21 C26 C25 0.0 . . . . ? P1 C21 C26 C25 -176.9(9) . . . . ? C1 P1 C27 C28 83.0(8) . . . . ? C21 P1 C27 C28 -163.4(6) . . . . ? Au1 P1 C27 C28 -37.2(7) . . . . ? C1 P1 C27 C32 -99.6(8) . . . . ? C21 P1 C27 C32 14.1(8) . . . . ? Au1 P1 C27 C32 140.2(5) . . . . ? C32 C27 C28 C29 0.0 . . . . ? P1 C27 C28 C29 177.6(8) . . . . ? C27 C28 C29 C30 0.0 . . . . ? C28 C29 C30 C31 0.0 . . . . ? C29 C30 C31 C32 0.0 . . . . ? C30 C31 C32 C27 0.0 . . . . ? C28 C27 C32 C31 0.0 . . . . ? P1 C27 C32 C31 -177.4(9) . . . . ? C39 P2 C33 C34 0.1(9) . . . . ? C20 P2 C33 C34 111.8(9) . . . . ? Au1 P2 C33 C34 -122.4(7) . . . . ? C39 P2 C33 C38 178.5(6) . . . . ? C20 P2 C33 C38 -69.9(9) . . . . ? Au1 P2 C33 C38 55.9(7) . . . . ? C38 C33 C34 C35 0.0 . . . . ? P2 C33 C34 C35 178.3(9) . . . . ? C33 C34 C35 C36 0.0 . . . . ? C34 C35 C36 C37 0.0 . . . . ? C35 C36 C37 C38 0.0 . . . . ? C36 C37 C38 C33 0.0 . . . . ? C34 C33 C38 C37 0.0 . . . . ? P2 C33 C38 C37 -178.4(9) . . . . ? C20 P2 C39 C40 -53.3(9) . . . . ? C33 P2 C39 C40 55.2(8) . . . . ? Au1 P2 C39 C40 169.1(5) . . . . ? C20 P2 C39 C44 127.8(8) . . . . ? C33 P2 C39 C44 -123.7(7) . . . . ? Au1 P2 C39 C44 -9.8(8) . . . . ? C44 C39 C40 C41 0.0 . . . . ? P2 C39 C40 C41 -178.9(9) . . . . ? 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 . . . . ? P2 C39 C44 C43 178.9(9) . . . . ? P4 Au2 P3 C65 -125.8(10) . . . . ? P4 Au2 P3 C71 -11.4(12) . . . . ? P4 Au2 P3 C45 101.7(11) . . . . ? P3 Au2 P4 C83 128.2(10) . . . . ? P3 Au2 P4 C64 -103.7(11) . . . . ? P3 Au2 P4 C77 10.3(12) . . . . ? C65 P3 C45 C50 -89.6(16) . . . . ? C71 P3 C45 C50 160.0(15) . . . . ? Au2 P3 C45 C50 46.8(18) . . . . ? C65 P3 C45 C46 90.3(15) . . . . ? C71 P3 C45 C46 -20.1(16) . . . . ? Au2 P3 C45 C46 -133.4(12) . . . . ? C50 C45 C46 C47 -1(3) . . . . ? P3 C45 C46 C47 178.9(14) . . . . ? C45 C46 C47 C48 3(3) . . . . ? C46 C47 C48 C49 -3(3) . . . . ? C47 C48 C49 C50 0(3) . . . . ? C46 C45 C50 C49 -1(3) . . . . ? P3 C45 C50 C49 178.7(14) . . . . ? C46 C45 C50 C51 -172.8(16) . . . . ? P3 C45 C50 C51 7(2) . . . . ? C48 C49 C50 C45 2(3) . . . . ? C48 C49 C50 C51 173.2(17) . . . . ? C45 C50 C51 O3 23(3) . . . . ? C49 C50 C51 O3 -148.1(18) . . . . ? C45 C50 C51 N3 -160.5(17) . . . . ? C49 C50 C51 N3 28(2) . . . . ? O3 C51 N3 C52 4(3) . . . . ? C50 C51 N3 C52 -172.3(14) . . . . ? C51 N3 C52 C57 -54(2) . . . . ? C51 N3 C52 C53 69.8(19) . . . . ? N3 C52 C53 C54 175.1(13) . . . . ? C57 C52 C53 C54 -57.1(16) . . . . ? C52 C53 C54 C55 56.9(17) . . . . ? C53 C54 C55 C56 -55.7(17) . . . . ? C54 C55 C56 C57 56.5(16) . . . . ? C55 C56 C57 N4 -179.2(12) . . . . ? C55 C56 C57 C52 -57.6(15) . . . . ? N3 C52 C57 N4 -55.8(15) . . . . ? C53 C52 C57 N4 -179.8(11) . . . . ? N3 C52 C57 C56 -177.3(12) . . . . ? C53 C52 C57 C56 58.8(15) . . . . ? C56 C57 N4 C58 -99.0(16) . . . . ? C52 C57 N4 C58 138.1(13) . . . . ? C57 N4 C58 O4 2(2) . . . . ? C57 N4 C58 C59 179.0(13) . . . . ? O4 C58 C59 C60 151.4(15) . . . . ? N4 C58 C59 C60 -26(2) . . . . ? O4 C58 C59 C64 -28(2) . . . . ? N4 C58 C59 C64 155.4(15) . . . . ? C64 C59 C60 C61 2(3) . . . . ? C58 C59 C60 C61 -177.2(14) . . . . ? C59 C60 C61 C62 -2(2) . . . . ? C60 C61 C62 C63 0(2) . . . . ? C61 C62 C63 C64 3(2) . . . . ? C60 C59 C64 C63 0(3) . . . . ? C58 C59 C64 C63 179.5(15) . . . . ? C60 C59 C64 P4 179.2(13) . . . . ? C58 C59 C64 P4 -2(2) . . . . ? C62 C63 C64 C59 -3(2) . . . . ? C62 C63 C64 P4 178.4(13) . . . . ? C83 P4 C64 C59 83.1(15) . . . . ? C77 P4 C64 C59 -167.1(14) . . . . ? Au2 P4 C64 C59 -51.0(16) . . . . ? C83 P4 C64 C63 -98.2(14) . . . . ? C77 P4 C64 C63 11.7(15) . . . . ? Au2 P4 C64 C63 127.7(12) . . . . ? C71 P3 C65 C66 64.5(8) . . . . ? C45 P3 C65 C66 -44.2(9) . . . . ? Au2 P3 C65 C66 177.7(5) . . . . ? C71 P3 C65 C70 -115.5(7) . . . . ? C45 P3 C65 C70 135.9(8) . . . . ? Au2 P3 C65 C70 -2.2(8) . . . . ? C70 C65 C66 C67 0.0 . . . . ? P3 C65 C66 C67 -179.9(9) . . . . ? C65 C66 C67 C68 0.0 . . . . ? C66 C67 C68 C69 0.0 . . . . ? C67 C68 C69 C70 0.0 . . . . ? C68 C69 C70 C65 0.0 . . . . ? C66 C65 C70 C69 0.0 . . . . ? P3 C65 C70 C69 179.9(9) . . . . ? C65 P3 C71 C72 5.4(9) . . . . ? C45 P3 C71 C72 117.5(8) . . . . ? Au2 P3 C71 C72 -117.2(6) . . . . ? C65 P3 C71 C76 -178.3(7) . . . . ? C45 P3 C71 C76 -66.3(9) . . . . ? Au2 P3 C71 C76 59.1(7) . . . . ? C76 C71 C72 C73 0.0 . . . . ? P3 C71 C72 C73 176.1(10) . . . . ? C71 C72 C73 C74 0.0 . . . . ? C72 C73 C74 C75 0.0 . . . . ? C73 C74 C75 C76 0.0 . . . . ? C74 C75 C76 C71 0.0 . . . . ? C72 C71 C76 C75 0.0 . . . . ? P3 C71 C76 C75 -176.4(9) . . . . ? C83 P4 C77 C78 -162.1(6) . . . . ? C64 P4 C77 C78 85.4(8) . . . . ? Au2 P4 C77 C78 -34.4(7) . . . . ? C83 P4 C77 C82 19.1(9) . . . . ? C64 P4 C77 C82 -93.4(9) . . . . ? Au2 P4 C77 C82 146.8(6) . . . . ? C82 C77 C78 C79 0.0 . . . . ? P4 C77 C78 C79 -178.9(8) . . . . ? C77 C78 C79 C80 0.0 . . . . ? C78 C79 C80 C81 0.0 . . . . ? C79 C80 C81 C82 0.0 . . . . ? C80 C81 C82 C77 0.0 . . . . ? C78 C77 C82 C81 0.0 . . . . ? P4 C77 C82 C81 178.7(9) . . . . ? C64 P4 C83 C84 -140.1(8) . . . . ? C77 P4 C83 C84 110.1(8) . . . . ? Au2 P4 C83 C84 -9.7(9) . . . . ? C64 P4 C83 C88 40.1(10) . . . . ? C77 P4 C83 C88 -69.8(8) . . . . ? Au2 P4 C83 C88 170.5(5) . . . . ? C88 C83 C84 C85 0.0 . . . . ? P4 C83 C84 C85 -179.8(9) . . . . ? C83 C84 C85 C86 0.0 . . . . ? C84 C85 C86 C87 0.0 . . . . ? C85 C86 C87 C88 0.0 . . . . ? C86 C87 C88 C83 0.0 . . . . ? C84 C83 C88 C87 0.0 . . . . ? P4 C83 C88 C87 179.8(9) . . . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 1.779 _refine_diff_density_min -2.494 _refine_diff_density_rms 0.171 # Attachment '2b.cif' data_09047 _database_code_depnum_ccdc_archive 'CCDC 755023' #TrackingRef '2b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H40 Au N2 O2 P2, B F4, 3 (C H2 Cl2)' _chemical_formula_sum 'C47 H46 Au B Cl6 F4 N2 O2 P2' _chemical_formula_weight 1229.2 _chemical_absolute_configuration syn loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P 1' _symmetry_space_group_name_Hall 'P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 11.9958(4) _cell_length_b 12.1404(3) _cell_length_c 18.3736(6) _cell_angle_alpha 73.731(2) _cell_angle_beta 89.798(2) _cell_angle_gamma 81.870(2) _cell_volume 2541.02(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 50733 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.607 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 3.327 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.461 _exptl_absorpt_correction_T_max 0.512 _exptl_absorpt_process_details ? _exptl_special_details ; Only the heavier atoms (gold, phosphorus and 100% occupancy chlorine) were refined with anisotropic thermal displacement parameters. Two of the solvent molecules were disordered and were modeled as 60:40 isotropic mixtures in each case. Note that ADDSYM suggests the centrosymmetric space group P-1. However, refinement in this spacegroup gives an unsatisfactory answer and results in the racemic mixture, which is not possible due to the use of a single enantiomer in the chemical synthesis. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_reflns_number 23994 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_sigmaI/netI 0.1062 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 26.12 _reflns_number_total 18064 _reflns_number_gt 14395 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _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^)+(0.0900P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 8176 Friedel pairs' _refine_ls_abs_structure_Flack 0.022(9) _refine_ls_number_reflns 18064 _refine_ls_number_parameters 515 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.0846 _refine_ls_R_factor_gt 0.0612 _refine_ls_wR_factor_ref 0.1660 _refine_ls_wR_factor_gt 0.1514 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.03709(3) 0.66063(3) 0.33933(2) 0.01851(19) Uani 1 1 d . . . P1 P -0.0981(4) 0.8188(4) 0.3331(3) 0.0175(11) Uani 1 1 d . . . P2 P 0.1964(4) 0.5248(4) 0.3457(3) 0.0182(11) Uani 1 1 d . . . C1 C -0.1739(12) 0.8085(13) 0.4211(9) 0.012(3) Uiso 1 1 d . . . C2 C -0.1791(11) 0.8941(12) 0.4572(8) 0.018(3) Uiso 1 1 d . . . H2A H -0.1450 0.9589 0.4348 0.021 Uiso 1 1 calc R . . C3 C -0.2322(11) 0.8896(12) 0.5251(8) 0.021(3) Uiso 1 1 d . . . H3A H -0.2385 0.9526 0.5451 0.025 Uiso 1 1 calc R . . C4 C -0.2762(12) 0.7887(13) 0.5632(9) 0.028(4) Uiso 1 1 d . . . H4A H -0.3067 0.7816 0.6106 0.034 Uiso 1 1 calc R . . C5 C -0.2735(12) 0.7001(13) 0.5294(9) 0.018(4) Uiso 1 1 d . . . H5A H -0.3061 0.6348 0.5533 0.022 Uiso 1 1 calc R . . C6 C -0.2210(13) 0.7071(14) 0.4577(10) 0.017(4) Uiso 1 1 d . . . C7 C -0.2181(13) 0.6182(14) 0.4182(10) 0.027(4) Uiso 1 1 d . . . N1 N -0.2213(8) 0.5042(9) 0.4594(7) 0.017(2) Uiso 1 1 d . . . H1A H -0.2199 0.4860 0.5082 0.020 Uiso 1 1 calc R . . O1 O -0.2197(8) 0.6453(9) 0.3486(6) 0.023(2) Uiso 1 1 d . . . C8 C -0.2270(10) 0.4142(10) 0.4211(7) 0.019(2) Uiso 1 1 d . . . H8A H -0.1950 0.4389 0.3710 0.023 Uiso 1 1 calc R . . C9 C -0.3524(12) 0.4013(12) 0.4099(9) 0.024(4) Uiso 1 1 d . . . H9A H -0.3859 0.3771 0.4589 0.029 Uiso 1 1 calc R . . H9B H -0.3940 0.4753 0.3816 0.029 Uiso 1 1 calc R . . C10 C -0.3592(11) 0.3116(11) 0.3672(8) 0.027(3) Uiso 1 1 d . . . H10A H -0.4368 0.2986 0.3641 0.033 Uiso 1 1 calc R . . H10B H -0.3346 0.3408 0.3159 0.033 Uiso 1 1 calc R . . C11 C -0.2867(11) 0.1988(12) 0.4060(8) 0.029(3) Uiso 1 1 d . . . H11A H -0.2868 0.1463 0.3748 0.035 Uiso 1 1 calc R . . H11B H -0.3189 0.1639 0.4540 0.035 Uiso 1 1 calc R . . C12 C -0.1664(12) 0.2138(13) 0.4205(9) 0.026(4) Uiso 1 1 d . . . H12A H -0.1305 0.2383 0.3724 0.031 Uiso 1 1 calc R . . H12B H -0.1251 0.1399 0.4493 0.031 Uiso 1 1 calc R . . C13 C -0.1618(9) 0.3029(10) 0.4639(7) 0.020(2) Uiso 1 1 d . . . H13A H -0.1992 0.2758 0.5117 0.024 Uiso 1 1 calc R . . C14 C 0.0365(12) 0.3480(13) 0.4328(9) 0.018(4) Uiso 1 1 d . . . O2 O 0.0175(8) 0.3921(8) 0.3650(6) 0.022(2) Uiso 1 1 d . . . N2 N -0.0445(9) 0.3130(9) 0.4833(7) 0.022(3) Uiso 1 1 d . . . H2B H -0.0255 0.2952 0.5307 0.027 Uiso 1 1 calc R . . C15 C 0.1523(14) 0.3316(14) 0.4660(10) 0.016(4) Uiso 1 1 d . . . C16 C 0.1885(13) 0.2358(14) 0.5283(9) 0.023(4) Uiso 1 1 d . . . H16A H 0.1377 0.1867 0.5513 0.027 Uiso 1 1 calc R . . C17 C 0.3003(13) 0.2132(14) 0.5561(10) 0.035(4) Uiso 1 1 d . . . H17A H 0.3230 0.1496 0.5976 0.042 Uiso 1 1 calc R . . C18 C 0.3767(12) 0.2843(12) 0.5224(9) 0.026(3) Uiso 1 1 d . . . H18A H 0.4510 0.2692 0.5410 0.032 Uiso 1 1 calc R . . C19 C 0.3428(12) 0.3766(13) 0.4618(9) 0.019(3) Uiso 1 1 d . . . H19A H 0.3950 0.4244 0.4395 0.023 Uiso 1 1 calc R . . C20 C 0.2297(15) 0.4033(15) 0.4309(11) 0.020(4) Uiso 1 1 d . . . C21 C -0.2038(8) 0.8649(9) 0.2555(5) 0.021(4) Uiso 1 1 d G . . C22 C -0.1793(7) 0.8376(9) 0.1880(6) 0.029(4) Uiso 1 1 d G . . H22A H -0.1095 0.7967 0.1828 0.035 Uiso 1 1 calc R . . C23 C -0.2591(8) 0.8716(9) 0.1283(5) 0.036(4) Uiso 1 1 d G . . H23A H -0.2428 0.8534 0.0831 0.043 Uiso 1 1 calc R . . C24 C -0.3634(8) 0.9327(9) 0.1361(5) 0.028(4) Uiso 1 1 d G . . H24A H -0.4168 0.9554 0.0961 0.033 Uiso 1 1 calc R . . C25 C -0.3879(7) 0.9599(9) 0.2036(6) 0.034(4) Uiso 1 1 d G . . H25A H -0.4577 1.0009 0.2088 0.041 Uiso 1 1 calc R . . C26 C -0.3081(9) 0.9260(10) 0.2633(5) 0.026(4) Uiso 1 1 d G . . H26A H -0.3244 0.9442 0.3084 0.031 Uiso 1 1 calc R . . C27 C -0.0273(8) 0.9444(7) 0.3265(6) 0.023(4) Uiso 1 1 d G . . C28 C 0.0618(8) 0.9311(6) 0.3779(5) 0.032(4) Uiso 1 1 d G . . H28A H 0.0841 0.8598 0.4132 0.039 Uiso 1 1 calc R . . C29 C 0.1176(7) 1.0246(8) 0.3763(5) 0.034(3) Uiso 1 1 d G . . H29A H 0.1772 1.0157 0.4107 0.040 Uiso 1 1 calc R . . C30 C 0.0842(7) 1.1313(7) 0.3235(6) 0.031(3) Uiso 1 1 d G . . H30A H 0.1215 1.1938 0.3225 0.037 Uiso 1 1 calc R . . C31 C -0.0049(8) 1.1445(6) 0.2721(5) 0.029(3) Uiso 1 1 d G . . H31A H -0.0272 1.2159 0.2368 0.034 Uiso 1 1 calc R . . C32 C -0.0607(7) 1.0510(8) 0.2736(5) 0.028(3) Uiso 1 1 d G . . H32A H -0.1203 1.0599 0.2393 0.034 Uiso 1 1 calc R . . C33 C 0.2162(9) 0.4654(9) 0.2656(5) 0.021(3) Uiso 1 1 d G . . C34 C 0.1738(8) 0.5328(7) 0.1942(6) 0.031(4) Uiso 1 1 d G . . H34A H 0.1315 0.6053 0.1887 0.037 Uiso 1 1 calc R . . C35 C 0.1945(9) 0.4920(8) 0.1313(5) 0.038(4) Uiso 1 1 d G . . H35A H 0.1661 0.5371 0.0835 0.045 Uiso 1 1 calc R . . C36 C 0.2576(9) 0.3837(9) 0.1396(5) 0.033(4) Uiso 1 1 d G . . H36A H 0.2715 0.3563 0.0975 0.040 Uiso 1 1 calc R . . C37 C 0.3000(9) 0.3162(7) 0.2109(6) 0.036(4) Uiso 1 1 d G . . H37A H 0.3423 0.2438 0.2165 0.043 Uiso 1 1 calc R . . C38 C 0.2793(9) 0.3571(8) 0.2739(5) 0.030(4) Uiso 1 1 d G . . H38A H 0.3077 0.3120 0.3216 0.035 Uiso 1 1 calc R . . C39 C 0.3149(7) 0.6066(9) 0.3423(6) 0.022(4) Uiso 1 1 d G . . C40 C 0.3992(8) 0.6077(8) 0.2901(5) 0.021(3) Uiso 1 1 d G . . H40A H 0.3949 0.5693 0.2532 0.025 Uiso 1 1 calc R . . C41 C 0.4899(7) 0.6662(9) 0.2932(5) 0.034(4) Uiso 1 1 d G . . H41A H 0.5463 0.6669 0.2583 0.040 Uiso 1 1 calc R . . C42 C 0.4963(7) 0.7236(8) 0.3484(6) 0.031(3) Uiso 1 1 d G . . H42A H 0.5569 0.7627 0.3504 0.037 Uiso 1 1 calc R . . C43 C 0.4119(8) 0.7224(9) 0.4006(5) 0.029(3) Uiso 1 1 d G . . H43A H 0.4162 0.7608 0.4375 0.035 Uiso 1 1 calc R . . C44 C 0.3212(7) 0.6640(9) 0.3975(6) 0.030(4) Uiso 1 1 d G . . H44A H 0.2648 0.6632 0.4324 0.036 Uiso 1 1 calc R . . Au2 Au -0.53359(3) -0.25412(3) 0.98624(2) 0.01897(19) Uani 1 1 d . . . P3 P -0.3898(4) -0.4056(4) 0.9915(3) 0.0182(11) Uani 1 1 d . . . P4 P -0.6982(4) -0.1254(4) 0.9799(3) 0.0183(11) Uani 1 1 d . . . C45 C -0.3104(13) -0.3974(14) 0.9035(10) 0.018(4) Uiso 1 1 d . . . C46 C -0.2970(12) -0.4984(13) 0.8783(8) 0.020(3) Uiso 1 1 d . . . H46A H -0.3283 -0.5634 0.9046 0.024 Uiso 1 1 calc R . . C47 C -0.2367(12) -0.4992(13) 0.8141(9) 0.029(4) Uiso 1 1 d . . . H47A H -0.2246 -0.5665 0.7988 0.035 Uiso 1 1 calc R . . C48 C -0.1940(13) -0.4017(14) 0.7724(10) 0.032(4) Uiso 1 1 d . . . H48A H -0.1581 -0.4015 0.7274 0.038 Uiso 1 1 calc R . . C49 C -0.2059(15) -0.3005(17) 0.7996(12) 0.037(5) Uiso 1 1 d . . . H49A H -0.1733 -0.2360 0.7742 0.044 Uiso 1 1 calc R . . C50 C -0.2659(14) -0.3000(15) 0.8634(10) 0.020(4) Uiso 1 1 d . . . C51 C -0.2689(10) -0.1989(11) 0.8960(8) 0.010(3) Uiso 1 1 d . . . N3 N -0.2615(9) -0.0974(9) 0.8442(7) 0.022(3) Uiso 1 1 d . . . H3B H -0.2682 -0.0943 0.7970 0.026 Uiso 1 1 calc R . . O3 O -0.2783(8) -0.2122(9) 0.9638(6) 0.024(2) Uiso 1 1 d . . . C52 C -0.2423(10) 0.0102(11) 0.8632(8) 0.024(3) Uiso 1 1 d . . . H52A H -0.2397 0.0693 0.8145 0.028 Uiso 1 1 calc R . . C53 C -0.1278(13) -0.0050(13) 0.9027(9) 0.029(4) Uiso 1 1 d . . . H53A H -0.1254 -0.0651 0.9506 0.035 Uiso 1 1 calc R . . H53B H -0.0700 -0.0306 0.8716 0.035 Uiso 1 1 calc R . . C54 C -0.1018(11) 0.1045(11) 0.9176(8) 0.029(3) Uiso 1 1 d . . . H54A H -0.0914 0.1606 0.8697 0.035 Uiso 1 1 calc R . . H54B H -0.0320 0.0878 0.9477 0.035 Uiso 1 1 calc R . . C55 C -0.1952(10) 0.1558(12) 0.9589(8) 0.027(3) Uiso 1 1 d . . . H55A H -0.1787 0.2290 0.9644 0.033 Uiso 1 1 calc R . . H55B H -0.2001 0.1037 1.0093 0.033 Uiso 1 1 calc R . . C56 C -0.3083(13) 0.1752(14) 0.9146(9) 0.028(4) Uiso 1 1 d . . . H56A H -0.3679 0.2082 0.9414 0.033 Uiso 1 1 calc R . . H56B H -0.3043 0.2293 0.8649 0.033 Uiso 1 1 calc R . . C57 C -0.3348(10) 0.0591(11) 0.9060(8) 0.023(3) Uiso 1 1 d . . . H57A H -0.3365 0.0049 0.9566 0.027 Uiso 1 1 calc R . . C58 C -0.5344(13) 0.0476(13) 0.9069(9) 0.022(4) Uiso 1 1 d . . . N4 N -0.4451(9) 0.0740(9) 0.8672(7) 0.020(3) Uiso 1 1 d . . . H4B H -0.4515 0.0999 0.8185 0.024 Uiso 1 1 calc R . . O4 O -0.5337(8) 0.0074(9) 0.9769(6) 0.025(2) Uiso 1 1 d . . . C59 C -0.6454(15) 0.0661(16) 0.8628(11) 0.024(5) Uiso 1 1 d . . . C60 C -0.6694(13) 0.1560(14) 0.7942(10) 0.025(4) Uiso 1 1 d . . . H60A H -0.6140 0.2004 0.7731 0.029 Uiso 1 1 calc R . . C61 C -0.7755(12) 0.1784(13) 0.7580(9) 0.026(4) Uiso 1 1 d . . . H61A H -0.7928 0.2400 0.7145 0.032 Uiso 1 1 calc R . . C62 C -0.8553(13) 0.1065(13) 0.7883(9) 0.029(4) Uiso 1 1 d . . . H62A H -0.9261 0.1200 0.7643 0.034 Uiso 1 1 calc R . . C63 C -0.8304(14) 0.0141(14) 0.8545(10) 0.028(4) Uiso 1 1 d . . . H63A H -0.8832 -0.0353 0.8725 0.034 Uiso 1 1 calc R . . C64 C -0.7284(14) -0.0036(14) 0.8928(10) 0.016(4) Uiso 1 1 d . . . C65 C -0.2860(8) -0.4456(9) 1.0698(5) 0.020(4) Uiso 1 1 d G . . C66 C -0.1830(8) -0.5127(10) 1.0669(5) 0.025(4) Uiso 1 1 d G . . H66A H -0.1658 -0.5377 1.0242 0.029 Uiso 1 1 calc R . . C67 C -0.1057(7) -0.5424(9) 1.1280(6) 0.027(4) Uiso 1 1 d G . . H67A H -0.0368 -0.5873 1.1261 0.032 Uiso 1 1 calc R . . C68 C -0.1315(8) -0.5051(10) 1.1918(5) 0.037(4) Uiso 1 1 d G . . H68A H -0.0798 -0.5250 1.2326 0.044 Uiso 1 1 calc R . . C69 C -0.2345(9) -0.4380(10) 1.1946(5) 0.038(4) Uiso 1 1 d G . . H69A H -0.2517 -0.4130 1.2373 0.046 Uiso 1 1 calc R . . C70 C -0.3118(7) -0.4082(9) 1.1336(6) 0.031(4) Uiso 1 1 d G . . H70A H -0.3807 -0.3633 1.1355 0.037 Uiso 1 1 calc R . . C71 C -0.4586(8) -0.5377(6) 1.0079(6) 0.024(4) Uiso 1 1 d G . . C72 C -0.5444(9) -0.5394(7) 0.9578(5) 0.037(4) Uiso 1 1 d G . . H72A H -0.5705 -0.4730 0.9190 0.045 Uiso 1 1 calc R . . C73 C -0.5911(8) -0.6404(9) 0.9657(5) 0.044(4) Uiso 1 1 d G . . H73A H -0.6484 -0.6416 0.9321 0.053 Uiso 1 1 calc R . . C74 C -0.5520(8) -0.7397(7) 1.0237(6) 0.026(3) Uiso 1 1 d G . . H74A H -0.5832 -0.8072 1.0290 0.031 Uiso 1 1 calc R . . C75 C -0.4662(8) -0.7379(6) 1.0738(5) 0.035(3) Uiso 1 1 d G . . H75A H -0.4400 -0.8043 1.1127 0.041 Uiso 1 1 calc R . . C76 C -0.4195(7) -0.6369(8) 1.0660(5) 0.029(3) Uiso 1 1 d G . . H76A H -0.3621 -0.6357 1.0995 0.034 Uiso 1 1 calc R . . C77 C -0.8151(7) -0.2074(9) 0.9770(6) 0.020(4) Uiso 1 1 d G . . C78 C -0.8101(7) -0.2672(10) 0.9224(6) 0.031(4) Uiso 1 1 d G . . H78A H -0.7494 -0.2652 0.8907 0.037 Uiso 1 1 calc R . . C79 C -0.8957(9) -0.3299(9) 0.9152(6) 0.041(4) Uiso 1 1 d G . . H79A H -0.8923 -0.3699 0.8787 0.050 Uiso 1 1 calc R . . C80 C -0.9865(7) -0.3329(8) 0.9627(6) 0.030(3) Uiso 1 1 d G . . H80A H -1.0438 -0.3748 0.9579 0.036 Uiso 1 1 calc R . . C81 C -0.9915(7) -0.2731(8) 1.0173(5) 0.020(3) Uiso 1 1 d G . . H81A H -1.0522 -0.2751 1.0490 0.024 Uiso 1 1 calc R . . C82 C -0.9058(8) -0.2104(8) 1.0245(5) 0.027(3) Uiso 1 1 d G . . H82A H -0.9092 -0.1704 1.0610 0.033 Uiso 1 1 calc R . . C83 C -0.7263(9) -0.0693(9) 1.0599(5) 0.022(4) Uiso 1 1 d G . . C84 C -0.6908(9) -0.1392(7) 1.1321(6) 0.030(4) Uiso 1 1 d G . . H84A H -0.6501 -0.2126 1.1383 0.036 Uiso 1 1 calc R . . C85 C -0.7160(9) -0.0994(9) 1.1951(5) 0.039(4) Uiso 1 1 d G . . H85A H -0.6922 -0.1462 1.2434 0.047 Uiso 1 1 calc R . . C86 C -0.7767(10) 0.0103(9) 1.1858(6) 0.040(4) Uiso 1 1 d G . . H86A H -0.7935 0.0369 1.2280 0.048 Uiso 1 1 calc R . . C87 C -0.8122(10) 0.0801(8) 1.1136(7) 0.043(5) Uiso 1 1 d G . . H87A H -0.8529 0.1535 1.1075 0.051 Uiso 1 1 calc R . . C88 C -0.7870(10) 0.0404(9) 1.0507(5) 0.042(5) Uiso 1 1 d G . . H88A H -0.8108 0.0871 1.0024 0.050 Uiso 1 1 calc R . . B1 B 0.6283(9) 1.0727(10) 0.6483(6) 0.028(4) Uiso 1 1 d D . . F1 F 0.5744(9) 1.1135(9) 0.7040(6) 0.060(3) Uiso 1 1 d D . . F2 F 0.7064(9) 0.9779(9) 0.6829(6) 0.064(3) Uiso 1 1 d D . . F3 F 0.6820(11) 1.1579(10) 0.6035(8) 0.085(5) Uiso 1 1 d D . . F4 F 0.5538(9) 1.0428(9) 0.6033(6) 0.058(3) Uiso 1 1 d D . . B2 B -0.1059(9) 0.3294(9) 0.6779(6) 0.032(5) Uiso 1 1 d D . . F5 F -0.1775(8) 0.4091(8) 0.6238(5) 0.050(3) Uiso 1 1 d D . . F6 F -0.0373(8) 0.2573(9) 0.6445(6) 0.058(3) Uiso 1 1 d D . . F7 F -0.0359(9) 0.3891(10) 0.7063(7) 0.071(4) Uiso 1 1 d D . . F8 F -0.1636(9) 0.2644(9) 0.7345(6) 0.061(3) Uiso 1 1 d D . . C89 C 0.0744(15) 0.3507(16) 0.8659(8) 0.057(5) Uiso 1 1 d D . . H89A H 0.1024 0.2720 0.8654 0.069 Uiso 1 1 calc R . . H89B H -0.0006 0.3711 0.8421 0.069 Uiso 1 1 calc R . . Cl1 Cl 0.1619(6) 0.4439(6) 0.8124(4) 0.0659(19) Uani 1 1 d D . . Cl2 Cl 0.0656(6) 0.3554(6) 0.9606(4) 0.0580(19) Uani 1 1 d D . . C90 C 0.5628(19) 0.3943(19) 0.6719(9) 0.084(7) Uiso 1 1 d D . . H90A H 0.5600 0.3175 0.6665 0.101 Uiso 1 1 calc R . . H90B H 0.6413 0.4015 0.6787 0.101 Uiso 1 1 calc R . . Cl3 Cl 0.5078(6) 0.4974(6) 0.5884(4) 0.0651(18) Uani 1 1 d D . . Cl4 Cl 0.4926(6) 0.4067(6) 0.7524(4) 0.0665(18) Uani 1 1 d D . . C91 C 0.4708(13) 1.0150(15) 0.4611(8) 0.050(4) Uiso 1 1 d D . . H91A H 0.4752 1.0842 0.4770 0.060 Uiso 1 1 calc R . . H91B H 0.5441 0.9671 0.4717 0.060 Uiso 1 1 calc R . . Cl5 Cl 0.3699(7) 0.9382(7) 0.5148(4) 0.071(2) Uani 1 1 d D . . Cl6 Cl 0.4409(6) 1.0553(6) 0.3643(4) 0.062(2) Uani 1 1 d D . . C92 C -0.0321(17) 0.9766(18) 0.6526(9) 0.077(7) Uiso 1 1 d D . . H92A H -0.1091 0.9669 0.6432 0.092 Uiso 1 1 calc R . . H92B H -0.0335 1.0534 0.6589 0.092 Uiso 1 1 calc R . . Cl7 Cl 0.0202(7) 0.8737(7) 0.7370(4) 0.081(2) Uani 1 1 d D . . Cl8 Cl 0.0452(7) 0.9681(6) 0.5737(4) 0.082(2) Uani 1 1 d D . . C93 C 0.414(4) 0.829(3) 0.7010(9) 0.101(6) Uiso 0.60 1 d PD A 1 H93A H 0.3748 0.9061 0.6770 0.122 Uiso 0.60 1 calc PR A 1 H93B H 0.4796 0.8155 0.6719 0.122 Uiso 0.60 1 calc PR A 1 Cl9 Cl 0.3250(15) 0.7265(16) 0.7012(11) 0.147(5) Uiso 0.60 1 d PD A 1 Cl10 Cl 0.4569(7) 0.8189(7) 0.7940(5) 0.0507(19) Uiso 0.60 1 d PD A 1 C93A C 0.4627(18) 0.844(2) 0.730(3) 0.0507(19) Uiso 0.40 1 d PD B 2 H93C H 0.4953 0.8469 0.7772 0.061 Uiso 0.40 1 calc PR B 2 H93D H 0.4972 0.8961 0.6886 0.061 Uiso 0.40 1 calc PR B 2 Cl11 Cl 0.490(2) 0.702(2) 0.7216(16) 0.147(5) Uiso 0.40 1 d PD B 2 Cl12 Cl 0.3171(16) 0.8902(18) 0.7260(12) 0.101(6) Uiso 0.40 1 d PD B 2 C94 C 0.092(3) 0.555(3) 0.557(3) 0.13(2) Uiso 0.60 1 d PD C 1 H94A H 0.1044 0.5634 0.5032 0.161 Uiso 0.60 1 calc PR C 1 H94B H 0.0411 0.4980 0.5737 0.161 Uiso 0.60 1 calc PR C 1 Cl13 Cl 0.2215(11) 0.5073(11) 0.6092(8) 0.094(4) Uiso 0.60 1 d PD C 1 Cl14 Cl 0.0321(11) 0.6882(11) 0.5693(8) 0.107(3) Uiso 0.60 1 d PD C 1 C94A C 0.124(4) 0.553(3) 0.613(2) 0.083(18) Uiso 0.40 1 d PD D 2 H94C H 0.1672 0.4807 0.6098 0.099 Uiso 0.40 1 calc PR D 2 H94D H 0.0766 0.5359 0.6563 0.099 Uiso 0.40 1 calc PR D 2 Cl15 Cl 0.0409(19) 0.6171(19) 0.5303(13) 0.107(3) Uiso 0.40 1 d PD D 2 Cl16 Cl 0.2164(15) 0.6466(16) 0.6254(11) 0.096(5) Uiso 0.40 1 d PD 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 0.0186(4) 0.0152(4) 0.0215(5) -0.0052(3) 0.0015(3) -0.0014(3) P1 0.023(2) 0.012(2) 0.017(3) -0.0035(19) 0.0008(19) -0.0016(18) P2 0.015(2) 0.017(2) 0.021(3) -0.003(2) 0.003(2) -0.0015(19) Au2 0.0173(4) 0.0177(4) 0.0220(5) -0.0056(4) 0.0029(3) -0.0028(3) P3 0.015(2) 0.019(2) 0.022(3) -0.007(2) 0.0062(19) -0.0047(18) P4 0.019(2) 0.017(2) 0.018(3) -0.002(2) 0.000(2) -0.004(2) Cl1 0.094(4) 0.063(4) 0.052(4) -0.022(3) 0.015(3) -0.035(3) Cl2 0.083(5) 0.055(4) 0.041(4) -0.015(3) 0.012(4) -0.019(4) Cl3 0.073(4) 0.066(4) 0.058(4) -0.012(3) 0.000(3) -0.028(3) Cl4 0.084(4) 0.054(3) 0.065(4) -0.013(3) 0.010(3) -0.032(3) Cl5 0.101(5) 0.080(4) 0.050(4) -0.032(3) 0.019(3) -0.046(4) Cl6 0.066(5) 0.058(4) 0.058(5) -0.009(4) -0.002(4) -0.009(4) Cl7 0.109(6) 0.090(5) 0.046(4) 0.002(3) -0.003(3) -0.062(4) Cl8 0.132(6) 0.067(4) 0.050(4) -0.008(3) 0.018(4) -0.038(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.308(5) . ? Au1 P2 2.322(5) . ? P1 C21 1.822(9) . ? P1 C27 1.823(8) . ? P1 C1 1.834(16) . ? P2 C33 1.813(9) . ? P2 C20 1.824(19) . ? P2 C39 1.837(9) . ? C1 C2 1.37(2) . ? C1 C6 1.42(2) . ? C2 C3 1.390(19) . ? C2 H2A 0.9300 . ? C3 C4 1.40(2) . ? C3 H3A 0.9300 . ? C4 C5 1.38(2) . ? C4 H4A 0.9300 . ? C5 C6 1.45(2) . ? C5 H5A 0.9300 . ? C6 C7 1.46(2) . ? C7 O1 1.227(19) . ? C7 N1 1.385(19) . ? N1 C8 1.465(16) . ? N1 H1A 0.8600 . ? C8 C13 1.472(16) . ? C8 C9 1.555(18) . ? C8 H8A 0.9800 . ? C9 C10 1.52(2) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.503(18) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.513(19) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.520(19) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N2 1.483(15) . ? C13 H13A 0.9800 . ? C14 O2 1.219(18) . ? C14 N2 1.369(18) . ? C14 C15 1.48(2) . ? N2 H2B 0.8600 . ? C15 C20 1.39(2) . ? C15 C16 1.40(2) . ? C16 C17 1.40(2) . ? C16 H16A 0.9300 . ? C17 C18 1.37(2) . ? C17 H17A 0.9300 . ? C18 C19 1.35(2) . ? C18 H18A 0.9300 . ? C19 C20 1.43(2) . ? C19 H19A 0.9300 . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C22 H22A 0.9300 . ? C23 C24 1.3900 . ? C23 H23A 0.9300 . ? C24 C25 1.3900 . ? C24 H24A 0.9300 . ? C25 C26 1.3900 . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C27 C28 1.3900 . ? C27 C32 1.3900 . ? C28 C29 1.3900 . ? C28 H28A 0.9300 . ? C29 C30 1.3900 . ? C29 H29A 0.9300 . ? C30 C31 1.3900 . ? C30 H30A 0.9300 . ? C31 C32 1.3900 . ? C31 H31A 0.9300 . ? C32 H32A 0.9300 . ? C33 C34 1.3900 . ? C33 C38 1.3900 . ? C34 C35 1.3900 . ? C34 H34A 0.9300 . ? C35 C36 1.3900 . ? C35 H35A 0.9300 . ? C36 C37 1.3900 . ? C36 H36A 0.9300 . ? C37 C38 1.3900 . ? C37 H37A 0.9300 . ? C38 H38A 0.9300 . ? C39 C40 1.3900 . ? C39 C44 1.3900 . ? C40 C41 1.3900 . ? C40 H40A 0.9300 . ? C41 C42 1.3900 . ? C41 H41A 0.9300 . ? C42 C43 1.3900 . ? C42 H42A 0.9300 . ? C43 C44 1.3900 . ? C43 H43A 0.9300 . ? C44 H44A 0.9300 . ? Au2 P3 2.318(5) . ? Au2 P4 2.319(5) . ? P3 C65 1.817(9) . ? P3 C71 1.856(8) . ? P3 C45 1.860(18) . ? P4 C83 1.798(10) . ? P4 C77 1.840(8) . ? P4 C64 1.845(18) . ? C45 C50 1.38(2) . ? C45 C46 1.42(2) . ? C46 C47 1.38(2) . ? C46 H46A 0.9300 . ? C47 C48 1.38(2) . ? C47 H47A 0.9300 . ? C48 C49 1.44(2) . ? C48 H48A 0.9300 . ? C49 C50 1.38(3) . ? C49 H49A 0.9300 . ? C50 C51 1.50(2) . ? C51 O3 1.217(17) . ? C51 N3 1.344(17) . ? N3 C52 1.491(16) . ? N3 H3B 0.8600 . ? C52 C57 1.507(17) . ? C52 C53 1.520(19) . ? C52 H52A 0.9800 . ? C53 C54 1.50(2) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 C55 1.510(18) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 C56 1.54(2) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 C57 1.537(19) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 N4 1.469(16) . ? C57 H57A 0.9800 . ? C58 O4 1.240(19) . ? C58 N4 1.321(18) . ? C58 C59 1.52(2) . ? N4 H4B 0.8600 . ? C59 C64 1.41(2) . ? C59 C60 1.42(3) . ? C60 C61 1.39(2) . ? C60 H60A 0.9300 . ? C61 C62 1.40(2) . ? C61 H61A 0.9300 . ? C62 C63 1.40(2) . ? C62 H62A 0.9300 . ? C63 C64 1.37(2) . ? C63 H63A 0.9300 . ? C65 C66 1.3900 . ? C65 C70 1.3900 . ? C66 C67 1.3900 . ? C66 H66A 0.9300 . ? C67 C68 1.3900 . ? C67 H67A 0.9300 . ? C68 C69 1.3900 . ? C68 H68A 0.9300 . ? C69 C70 1.3900 . ? C69 H69A 0.9300 . ? C70 H70A 0.9300 . ? C71 C72 1.3900 . ? C71 C76 1.3900 . ? C72 C73 1.3900 . ? C72 H72A 0.9300 . ? C73 C74 1.3900 . ? C73 H73A 0.9300 . ? C74 C75 1.3900 . ? C74 H74A 0.9300 . ? C75 C76 1.3900 . ? C75 H75A 0.9300 . ? C76 H76A 0.9300 . ? C77 C78 1.3900 . ? C77 C82 1.3900 . ? C78 C79 1.3900 . ? C78 H78A 0.9300 . ? C79 C80 1.3900 . ? C79 H79A 0.9300 . ? C80 C81 1.3900 . ? C80 H80A 0.9300 . ? C81 C82 1.3900 . ? C81 H81A 0.9300 . ? C82 H82A 0.9300 . ? C83 C84 1.3900 . ? C83 C88 1.3900 . ? C84 C85 1.3900 . ? C84 H84A 0.9300 . ? C85 C86 1.3900 . ? C85 H85A 0.9300 . ? C86 C87 1.3900 . ? C86 H86A 0.9300 . ? C87 C88 1.3900 . ? C87 H87A 0.9300 . ? C88 H88A 0.9300 . ? B1 F3 1.368(9) . ? B1 F4 1.371(9) . ? B1 F2 1.376(9) . ? B1 F1 1.378(9) . ? B2 F8 1.368(9) . ? B2 F7 1.375(9) . ? B2 F5 1.376(9) . ? B2 F6 1.383(9) . ? C89 Cl1 1.748(14) . ? C89 Cl2 1.759(14) . ? C89 H89A 0.9700 . ? C89 H89B 0.9700 . ? C90 Cl4 1.732(16) . ? C90 Cl3 1.747(16) . ? C90 H90A 0.9700 . ? C90 H90B 0.9700 . ? C91 Cl6 1.733(14) . ? C91 Cl5 1.762(13) . ? C91 H91A 0.9700 . ? C91 H91B 0.9700 . ? C92 Cl8 1.738(15) . ? C92 Cl7 1.750(15) . ? C92 H92A 0.9700 . ? C92 H92B 0.9700 . ? C93 Cl9 1.747(10) . ? C93 Cl10 1.753(10) . ? C93 H93A 0.9700 . ? C93 H93B 0.9700 . ? C93A Cl12 1.751(10) . ? C93A Cl11 1.761(10) . ? C93A H93C 0.9700 . ? C93A H93D 0.9700 . ? C94 Cl14 1.753(10) . ? C94 Cl13 1.769(10) . ? C94 H94A 0.9700 . ? C94 H94B 0.9700 . ? C94A Cl15 1.744(10) . ? C94A Cl16 1.750(10) . ? C94A H94C 0.9700 . ? C94A H94D 0.9700 . ? 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 P1 Au1 P2 169.51(19) . . ? C21 P1 C27 105.5(5) . . ? C21 P1 C1 106.9(6) . . ? C27 P1 C1 101.5(6) . . ? C21 P1 Au1 119.1(4) . . ? C27 P1 Au1 108.4(4) . . ? C1 P1 Au1 113.6(5) . . ? C33 P2 C20 106.6(7) . . ? C33 P2 C39 103.9(5) . . ? C20 P2 C39 103.2(7) . . ? C33 P2 Au1 116.3(4) . . ? C20 P2 Au1 120.1(6) . . ? C39 P2 Au1 104.5(4) . . ? C2 C1 C6 117.6(14) . . ? C2 C1 P1 121.4(12) . . ? C6 C1 P1 120.8(12) . . ? C1 C2 C3 124.1(14) . . ? C1 C2 H2A 118.0 . . ? C3 C2 H2A 118.0 . . ? C2 C3 C4 119.0(14) . . ? C2 C3 H3A 120.5 . . ? C4 C3 H3A 120.5 . . ? C5 C4 C3 119.2(15) . . ? C5 C4 H4A 120.4 . . ? C3 C4 H4A 120.4 . . ? C4 C5 C6 121.2(15) . . ? C4 C5 H5A 119.4 . . ? C6 C5 H5A 119.4 . . ? C1 C6 C5 118.7(15) . . ? C1 C6 C7 117.3(15) . . ? C5 C6 C7 123.8(15) . . ? O1 C7 N1 120.3(15) . . ? O1 C7 C6 120.1(15) . . ? N1 C7 C6 119.5(15) . . ? C7 N1 C8 120.9(12) . . ? C7 N1 H1A 119.6 . . ? C8 N1 H1A 119.6 . . ? N1 C8 C13 111.4(10) . . ? N1 C8 C9 109.2(10) . . ? C13 C8 C9 111.0(10) . . ? N1 C8 H8A 108.4 . . ? C13 C8 H8A 108.4 . . ? C9 C8 H8A 108.4 . . ? C10 C9 C8 109.5(12) . . ? C10 C9 H9A 109.8 . . ? C8 C9 H9A 109.8 . . ? C10 C9 H9B 109.8 . . ? C8 C9 H9B 109.8 . . ? H9A C9 H9B 108.2 . . ? C11 C10 C9 111.1(11) . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C10 C11 C12 112.7(12) . . ? C10 C11 H11A 109.1 . . ? C12 C11 H11A 109.1 . . ? C10 C11 H11B 109.1 . . ? C12 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? C11 C12 C13 111.3(12) . . ? C11 C12 H12A 109.4 . . ? C13 C12 H12A 109.4 . . ? C11 C12 H12B 109.4 . . ? C13 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? C8 C13 N2 113.1(10) . . ? C8 C13 C12 109.4(11) . . ? N2 C13 C12 112.2(10) . . ? C8 C13 H13A 107.2 . . ? N2 C13 H13A 107.2 . . ? C12 C13 H13A 107.2 . . ? O2 C14 N2 124.0(13) . . ? O2 C14 C15 120.5(14) . . ? N2 C14 C15 115.6(14) . . ? C14 N2 C13 126.1(12) . . ? C14 N2 H2B 117.0 . . ? C13 N2 H2B 117.0 . . ? C20 C15 C16 119.2(15) . . ? C20 C15 C14 120.6(15) . . ? C16 C15 C14 119.9(15) . . ? C17 C16 C15 120.7(15) . . ? C17 C16 H16A 119.7 . . ? C15 C16 H16A 119.7 . . ? C18 C17 C16 120.4(15) . . ? C18 C17 H17A 119.8 . . ? C16 C17 H17A 119.8 . . ? C19 C18 C17 119.3(14) . . ? C19 C18 H18A 120.3 . . ? C17 C18 H18A 120.3 . . ? C18 C19 C20 122.5(14) . . ? C18 C19 H19A 118.7 . . ? C20 C19 H19A 118.7 . . ? C15 C20 C19 117.8(16) . . ? C15 C20 P2 123.8(13) . . ? C19 C20 P2 118.4(13) . . ? C22 C21 C26 120.0 . . ? C22 C21 P1 119.2(6) . . ? C26 C21 P1 120.8(6) . . ? C23 C22 C21 120.0 . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C24 C23 C22 120.0 . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? C23 C24 C25 120.0 . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? C26 C25 C24 120.0 . . ? C26 C25 H25A 120.0 . . ? C24 C25 H25A 120.0 . . ? C25 C26 C21 120.0 . . ? C25 C26 H26A 120.0 . . ? C21 C26 H26A 120.0 . . ? C28 C27 C32 120.0 . . ? C28 C27 P1 117.5(5) . . ? C32 C27 P1 122.5(5) . . ? C29 C28 C27 120.0 . . ? C29 C28 H28A 120.0 . . ? C27 C28 H28A 120.0 . . ? C28 C29 C30 120.0 . . ? C28 C29 H29A 120.0 . . ? C30 C29 H29A 120.0 . . ? C31 C30 C29 120.0 . . ? C31 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C30 C31 C32 120.0 . . ? C30 C31 H31A 120.0 . . ? C32 C31 H31A 120.0 . . ? C31 C32 C27 120.0 . . ? C31 C32 H32A 120.0 . . ? C27 C32 H32A 120.0 . . ? C34 C33 C38 120.0 . . ? C34 C33 P2 119.1(6) . . ? C38 C33 P2 120.7(6) . . ? C33 C34 C35 120.0 . . ? C33 C34 H34A 120.0 . . ? C35 C34 H34A 120.0 . . ? C34 C35 C36 120.0 . . ? C34 C35 H35A 120.0 . . ? C36 C35 H35A 120.0 . . ? C35 C36 C37 120.0 . . ? C35 C36 H36A 120.0 . . ? C37 C36 H36A 120.0 . . ? C36 C37 C38 120.0 . . ? C36 C37 H37A 120.0 . . ? C38 C37 H37A 120.0 . . ? C37 C38 C33 120.0 . . ? C37 C38 H38A 120.0 . . ? C33 C38 H38A 120.0 . . ? C40 C39 C44 120.0 . . ? C40 C39 P2 122.8(6) . . ? C44 C39 P2 117.1(6) . . ? C39 C40 C41 120.0 . . ? C39 C40 H40A 120.0 . . ? C41 C40 H40A 120.0 . . ? C42 C41 C40 120.0 . . ? C42 C41 H41A 120.0 . . ? C40 C41 H41A 120.0 . . ? C43 C42 C41 120.0 . . ? C43 C42 H42A 120.0 . . ? C41 C42 H42A 120.0 . . ? C42 C43 C44 120.0 . . ? C42 C43 H43A 120.0 . . ? C44 C43 H43A 120.0 . . ? C43 C44 C39 120.0 . . ? C43 C44 H44A 120.0 . . ? C39 C44 H44A 120.0 . . ? P3 Au2 P4 170.05(19) . . ? C65 P3 C71 102.5(5) . . ? C65 P3 C45 106.8(7) . . ? C71 P3 C45 105.5(7) . . ? C65 P3 Au2 118.2(4) . . ? C71 P3 Au2 105.9(4) . . ? C45 P3 Au2 116.2(6) . . ? C83 P4 C77 103.9(6) . . ? C83 P4 C64 108.0(7) . . ? C77 P4 C64 101.7(7) . . ? C83 P4 Au2 117.2(4) . . ? C77 P4 Au2 106.3(4) . . ? C64 P4 Au2 117.6(6) . . ? C50 C45 C46 120.4(15) . . ? C50 C45 P3 123.6(13) . . ? C46 C45 P3 116.0(12) . . ? C47 C46 C45 119.1(14) . . ? C47 C46 H46A 120.5 . . ? C45 C46 H46A 120.5 . . ? C46 C47 C48 121.3(15) . . ? C46 C47 H47A 119.4 . . ? C48 C47 H47A 119.4 . . ? C47 C48 C49 119.0(16) . . ? C47 C48 H48A 120.5 . . ? C49 C48 H48A 120.5 . . ? C50 C49 C48 119.5(18) . . ? C50 C49 H49A 120.3 . . ? C48 C49 H49A 120.3 . . ? C49 C50 C45 120.6(17) . . ? C49 C50 C51 119.3(16) . . ? C45 C50 C51 119.5(15) . . ? O3 C51 N3 125.2(13) . . ? O3 C51 C50 120.6(13) . . ? N3 C51 C50 114.2(13) . . ? C51 N3 C52 124.2(12) . . ? C51 N3 H3B 117.9 . . ? C52 N3 H3B 117.9 . . ? N3 C52 C57 115.1(10) . . ? N3 C52 C53 111.4(11) . . ? C57 C52 C53 111.4(11) . . ? N3 C52 H52A 106.1 . . ? C57 C52 H52A 106.1 . . ? C53 C52 H52A 106.1 . . ? C54 C53 C52 112.9(12) . . ? C54 C53 H53A 109.0 . . ? C52 C53 H53A 109.0 . . ? C54 C53 H53B 109.0 . . ? C52 C53 H53B 109.0 . . ? H53A C53 H53B 107.8 . . ? C53 C54 C55 111.5(12) . . ? C53 C54 H54A 109.3 . . ? C55 C54 H54A 109.3 . . ? C53 C54 H54B 109.3 . . ? C55 C54 H54B 109.3 . . ? H54A C54 H54B 108.0 . . ? C54 C55 C56 110.1(12) . . ? C54 C55 H55A 109.6 . . ? C56 C55 H55A 109.6 . . ? C54 C55 H55B 109.6 . . ? C56 C55 H55B 109.6 . . ? H55A C55 H55B 108.2 . . ? C57 C56 C55 109.8(12) . . ? C57 C56 H56A 109.7 . . ? C55 C56 H56A 109.7 . . ? C57 C56 H56B 109.7 . . ? C55 C56 H56B 109.7 . . ? H56A C56 H56B 108.2 . . ? N4 C57 C52 111.0(10) . . ? N4 C57 C56 111.1(11) . . ? C52 C57 C56 108.9(11) . . ? N4 C57 H57A 108.6 . . ? C52 C57 H57A 108.6 . . ? C56 C57 H57A 108.6 . . ? O4 C58 N4 125.0(15) . . ? O4 C58 C59 118.1(14) . . ? N4 C58 C59 116.9(15) . . ? C58 N4 C57 120.0(12) . . ? C58 N4 H4B 120.0 . . ? C57 N4 H4B 120.0 . . ? C64 C59 C60 119.4(16) . . ? C64 C59 C58 119.2(16) . . ? C60 C59 C58 121.3(16) . . ? C61 C60 C59 120.5(15) . . ? C61 C60 H60A 119.8 . . ? C59 C60 H60A 119.8 . . ? C60 C61 C62 118.7(14) . . ? C60 C61 H61A 120.6 . . ? C62 C61 H61A 120.6 . . ? C61 C62 C63 121.0(14) . . ? C61 C62 H62A 119.5 . . ? C63 C62 H62A 119.5 . . ? C64 C63 C62 120.2(15) . . ? C64 C63 H63A 119.9 . . ? C62 C63 H63A 119.9 . . ? C63 C64 C59 119.9(16) . . ? C63 C64 P4 119.3(13) . . ? C59 C64 P4 120.7(13) . . ? C66 C65 C70 120.0 . . ? C66 C65 P3 121.4(6) . . ? C70 C65 P3 118.6(6) . . ? C67 C66 C65 120.0 . . ? C67 C66 H66A 120.0 . . ? C65 C66 H66A 120.0 . . ? C66 C67 C68 120.0 . . ? C66 C67 H67A 120.0 . . ? C68 C67 H67A 120.0 . . ? C69 C68 C67 120.0 . . ? C69 C68 H68A 120.0 . . ? C67 C68 H68A 120.0 . . ? C70 C69 C68 120.0 . . ? C70 C69 H69A 120.0 . . ? C68 C69 H69A 120.0 . . ? C69 C70 C65 120.0 . . ? C69 C70 H70A 120.0 . . ? C65 C70 H70A 120.0 . . ? C72 C71 C76 120.0 . . ? C72 C71 P3 119.1(6) . . ? C76 C71 P3 120.7(6) . . ? C73 C72 C71 120.0 . . ? C73 C72 H72A 120.0 . . ? C71 C72 H72A 120.0 . . ? C74 C73 C72 120.0 . . ? C74 C73 H73A 120.0 . . ? C72 C73 H73A 120.0 . . ? C75 C74 C73 120.0 . . ? C75 C74 H74A 120.0 . . ? C73 C74 H74A 120.0 . . ? C76 C75 C74 120.0 . . ? C76 C75 H75A 120.0 . . ? C74 C75 H75A 120.0 . . ? C75 C76 C71 120.0 . . ? C75 C76 H76A 120.0 . . ? C71 C76 H76A 120.0 . . ? C78 C77 C82 120.0 . . ? C78 C77 P4 116.0(6) . . ? C82 C77 P4 124.0(6) . . ? C79 C78 C77 120.0 . . ? C79 C78 H78A 120.0 . . ? C77 C78 H78A 120.0 . . ? C78 C79 C80 120.0 . . ? C78 C79 H79A 120.0 . . ? C80 C79 H79A 120.0 . . ? C79 C80 C81 120.0 . . ? C79 C80 H80A 120.0 . . ? C81 C80 H80A 120.0 . . ? C82 C81 C80 120.0 . . ? C82 C81 H81A 120.0 . . ? C80 C81 H81A 120.0 . . ? C81 C82 C77 120.0 . . ? C81 C82 H82A 120.0 . . ? C77 C82 H82A 120.0 . . ? C84 C83 C88 120.0 . . ? C84 C83 P4 119.1(6) . . ? C88 C83 P4 120.9(6) . . ? C83 C84 C85 120.0 . . ? C83 C84 H84A 120.0 . . ? C85 C84 H84A 120.0 . . ? C86 C85 C84 120.0 . . ? C86 C85 H85A 120.0 . . ? C84 C85 H85A 120.0 . . ? C87 C86 C85 120.0 . . ? C87 C86 H86A 120.0 . . ? C85 C86 H86A 120.0 . . ? C86 C87 C88 120.0 . . ? C86 C87 H87A 120.0 . . ? C88 C87 H87A 120.0 . . ? C87 C88 C83 120.0 . . ? C87 C88 H88A 120.0 . . ? C83 C88 H88A 120.0 . . ? F3 B1 F4 108.3(10) . . ? F3 B1 F2 109.6(10) . . ? F4 B1 F2 110.2(9) . . ? F3 B1 F1 108.9(10) . . ? F4 B1 F1 111.6(10) . . ? F2 B1 F1 108.2(9) . . ? F8 B2 F7 111.1(10) . . ? F8 B2 F5 111.9(10) . . ? F7 B2 F5 107.7(9) . . ? F8 B2 F6 109.7(9) . . ? F7 B2 F6 106.3(10) . . ? F5 B2 F6 110.0(9) . . ? Cl1 C89 Cl2 113.4(9) . . ? Cl1 C89 H89A 108.9 . . ? Cl2 C89 H89A 108.9 . . ? Cl1 C89 H89B 108.9 . . ? Cl2 C89 H89B 108.9 . . ? H89A C89 H89B 107.7 . . ? Cl4 C90 Cl3 114.0(11) . . ? Cl4 C90 H90A 108.7 . . ? Cl3 C90 H90A 108.7 . . ? Cl4 C90 H90B 108.7 . . ? Cl3 C90 H90B 108.7 . . ? H90A C90 H90B 107.6 . . ? Cl6 C91 Cl5 113.2(9) . . ? Cl6 C91 H91A 108.9 . . ? Cl5 C91 H91A 108.9 . . ? Cl6 C91 H91B 108.9 . . ? Cl5 C91 H91B 108.9 . . ? H91A C91 H91B 107.7 . . ? Cl8 C92 Cl7 114.2(11) . . ? Cl8 C92 H92A 108.7 . . ? Cl7 C92 H92A 108.7 . . ? Cl8 C92 H92B 108.7 . . ? Cl7 C92 H92B 108.7 . . ? H92A C92 H92B 107.6 . . ? Cl9 C93 Cl10 110.4(13) . . ? Cl9 C93 H93A 109.6 . . ? Cl10 C93 H93A 109.6 . . ? Cl9 C93 H93B 109.6 . . ? Cl10 C93 H93B 109.6 . . ? H93A C93 H93B 108.1 . . ? Cl12 C93A Cl11 110.4(17) . . ? Cl12 C93A H93C 109.6 . . ? Cl11 C93A H93C 109.6 . . ? Cl12 C93A H93D 109.6 . . ? Cl11 C93A H93D 109.6 . . ? H93C C93A H93D 108.1 . . ? Cl14 C94 Cl13 109.0(12) . . ? Cl14 C94 H94A 109.9 . . ? Cl13 C94 H94A 109.9 . . ? Cl14 C94 H94B 109.9 . . ? Cl13 C94 H94B 109.9 . . ? H94A C94 H94B 108.3 . . ? Cl15 C94A Cl16 110.0(18) . . ? Cl15 C94A H94C 109.7 . . ? Cl16 C94A H94C 109.7 . . ? Cl15 C94A H94D 109.7 . . ? Cl16 C94A H94D 109.7 . . ? H94C C94A H94D 108.2 . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 26.12 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 2.982 _refine_diff_density_min -1.230 _refine_diff_density_rms 0.219 # Attachment '2c.cif' data_2c _database_code_depnum_ccdc_archive 'CCDC 755024' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H40 Ag N2 O2 P2, 2(C3 H6 O), C2 F3 O2 ' _chemical_formula_sum 'C52 H52 Ag F3 N2 O6 P2' _chemical_formula_weight 1027.77 _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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) _symmetry_space_group_name_Hall 'P 2yb ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 17.536(4) _cell_length_b 14.920(3) _cell_length_c 18.883(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.44(3) _cell_angle_gamma 90.00 _cell_volume 4936.2(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 64223 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 25.03 _exptl_crystal_description cube _exptl_crystal_colour colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.383 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 0.535 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9337 _exptl_absorpt_correction_T_max 0.9534 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17399 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0698 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.07 _reflns_number_total 17399 _reflns_number_gt 13409 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1997-2001)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 2001)' _computing_publication_material SHELXTL/PC _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^)+(0.1136P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(3) _refine_ls_number_reflns 17399 _refine_ls_number_parameters 1189 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0917 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1889 _refine_ls_wR_factor_gt 0.1510 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.005 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 0.74099(3) -0.11723(4) 0.96529(3) 0.03042(18) Uani 1 1 d . . . F1 F 0.7015(3) 0.3636(5) 0.7610(4) 0.072(2) Uani 1 1 d . . . P1 P 0.60460(9) -0.10945(16) 0.96155(10) 0.0248(5) Uani 1 1 d . . . N1 N 0.6680(3) -0.3942(4) 0.9518(3) 0.0271(15) Uani 1 1 d . . . H1A H 0.6596 -0.4147 0.9084 0.033 Uiso 1 1 calc R . . O1 O 0.6480(3) -0.2735(4) 1.0237(3) 0.0317(13) Uani 1 1 d . . . C1 C 0.5489(4) -0.1947(6) 0.9143(4) 0.029(2) Uani 1 1 d . . . Ag2 Ag 0.27052(3) 0.12560(4) 0.53598(3) 0.03055(18) Uani 1 1 d . . . F2 F 0.7307(3) 0.4592(5) 0.6845(3) 0.076(2) Uani 1 1 d . . . P2 P 0.87250(11) -0.07862(16) 0.95616(12) 0.0286(5) Uani 1 1 d . . . N2 N 0.8316(3) -0.3607(5) 0.9635(3) 0.0303(16) Uani 1 1 d . . . H2B H 0.8312 -0.3903 0.9232 0.036 Uiso 1 1 calc R . . O2 O 0.8663(3) -0.2382(4) 1.0246(3) 0.0449(16) Uani 1 1 d . . . C2 C 0.4838(4) -0.1721(6) 0.8749(4) 0.0292(19) Uani 1 1 d . . . H2A H 0.4715 -0.1105 0.8684 0.035 Uiso 1 1 calc R . . O3 O 0.3609(3) 0.2648(4) 0.4723(3) 0.0311(13) Uani 1 1 d . . . N3 N 0.3213(3) 0.3836(5) 0.5344(3) 0.0323(15) Uani 1 1 d . . . H3B H 0.3230 0.4142 0.5743 0.039 Uiso 1 1 calc R . . F3 F 0.8182(2) 0.3979(4) 0.7464(3) 0.0548(15) Uani 1 1 d . . . P3 P 0.40604(10) 0.11257(15) 0.54210(11) 0.0252(5) Uani 1 1 d . . . C3 C 0.4361(4) -0.2358(6) 0.8445(5) 0.0295(19) Uani 1 1 d . . . H3A H 0.3905 -0.2181 0.8194 0.035 Uiso 1 1 calc R . . N4 N 0.1576(3) 0.3902(5) 0.5564(4) 0.0376(16) Uani 1 1 d . . . H4B H 0.1512 0.4129 0.5987 0.045 Uiso 1 1 calc R . . O4 O 0.1466(3) 0.2616(4) 0.4888(4) 0.0496(17) Uani 1 1 d . . . F4 F 0.2991(3) 0.6498(4) 0.7327(3) 0.0642(19) Uani 1 1 d . . . P4 P 0.13774(11) 0.09558(15) 0.54591(12) 0.0301(5) Uani 1 1 d . . . C4 C 0.4545(4) -0.3256(6) 0.8505(4) 0.0297(19) Uani 1 1 d . . . H4A H 0.4215 -0.3697 0.8298 0.036 Uiso 1 1 calc R . . O5 O 0.6748(3) 0.5308(4) 0.8141(3) 0.0414(15) Uani 1 1 d . . . F5 F 0.1828(2) 0.6352(4) 0.7554(3) 0.0602(16) Uani 1 1 d . . . C5 C 0.5216(4) -0.3509(6) 0.8872(4) 0.027(2) Uani 1 1 d . . . H5A H 0.5355 -0.4124 0.8894 0.033 Uiso 1 1 calc R . . O6 O 0.8030(3) 0.5386(4) 0.8302(3) 0.0448(16) Uani 1 1 d . . . F6 F 0.2686(4) 0.5575(5) 0.8146(3) 0.0727(19) Uani 1 1 d . . . C6 C 0.5680(4) -0.2878(6) 0.9204(4) 0.0279(19) Uani 1 1 d . . . C7 C 0.6337(4) -0.3169(6) 0.9696(4) 0.0245(18) Uani 1 1 d . . . O7 O 0.3019(3) 0.4852(4) 0.6717(3) 0.0463(16) Uani 1 1 d . . . C8 C 0.7182(4) -0.4458(5) 0.9999(4) 0.0324(18) Uani 1 1 d . . . H8A H 0.7345 -0.5003 0.9736 0.039 Uiso 1 1 calc R . . O8 O 0.1745(3) 0.4815(4) 0.6856(3) 0.0445(16) Uani 1 1 d . . . C9 C 0.6756(5) -0.4780(6) 1.0641(5) 0.038(2) Uani 1 1 d . . . H9A H 0.6303 -0.5130 1.0478 0.046 Uiso 1 1 calc R . . H9B H 0.6578 -0.4255 1.0909 0.046 Uiso 1 1 calc R . . O9 O 0.2377(8) 0.6921(10) 0.5181(7) 0.144(5) Uani 1 1 d . . . C10 C 0.7277(5) -0.5369(6) 1.1135(5) 0.044(2) Uani 1 1 d . . . H10A H 0.7001 -0.5530 1.1564 0.053 Uiso 1 1 calc R . . H10B H 0.7404 -0.5930 1.0886 0.053 Uiso 1 1 calc R . . O10 O 0.2612(4) 0.1640(6) 0.6956(5) 0.081(3) Uani 1 1 d . . . C11 C 0.8006(5) -0.4874(7) 1.1350(5) 0.046(2) Uani 1 1 d . . . H11A H 0.7881 -0.4351 1.1645 0.055 Uiso 1 1 calc R . . H11B H 0.8344 -0.5276 1.1639 0.055 Uiso 1 1 calc R . . O11 O 0.7438(4) -1.1583(6) 0.8122(4) 0.066(2) Uani 1 1 d . . . C12 C 0.8419(5) -0.4562(7) 1.0713(5) 0.041(2) Uani 1 1 d . . . H12A H 0.8577 -0.5087 1.0435 0.049 Uiso 1 1 calc R . . H12B H 0.8885 -0.4230 1.0871 0.049 Uiso 1 1 calc R . . O12 O 0.7645(7) -1.6763(9) 0.9666(5) 0.116(4) Uani 1 1 d . . . C13 C 0.7907(4) -0.3952(6) 1.0243(4) 0.0334(19) Uani 1 1 d . . . H13A H 0.7753 -0.3429 1.0536 0.040 Uiso 1 1 calc R . . C14 C 0.8692(4) -0.2838(6) 0.9710(5) 0.031(2) Uani 1 1 d . . . C15 C 0.9157(4) -0.2510(6) 0.9106(4) 0.030(2) Uani 1 1 d . . . C16 C 0.9547(4) -0.3099(6) 0.8693(5) 0.040(2) Uani 1 1 d . . . H16A H 0.9485 -0.3726 0.8754 0.048 Uiso 1 1 calc R . . C17 C 1.0036(5) -0.2772(6) 0.8183(5) 0.045(2) Uani 1 1 d . . . H17A H 1.0318 -0.3178 0.7908 0.054 Uiso 1 1 calc R . . C18 C 1.0106(5) -0.1868(7) 0.8083(6) 0.050(3) Uani 1 1 d . . . H18A H 1.0426 -0.1651 0.7728 0.060 Uiso 1 1 calc R . . C19 C 0.9717(4) -0.1261(8) 0.8492(4) 0.040(2) Uani 1 1 d . . . H19A H 0.9772 -0.0635 0.8419 0.048 Uiso 1 1 calc R . . C20 C 0.9244(4) -0.1584(6) 0.9015(5) 0.031(2) Uani 1 1 d . . . C21 C 0.5589(4) -0.1011(6) 1.0450(4) 0.032(2) Uani 1 1 d . . . C22 C 0.4804(4) -0.1182(6) 1.0505(4) 0.0344(18) Uani 1 1 d . . . H22A H 0.4507 -0.1352 1.0094 0.041 Uiso 1 1 calc R . . C23 C 0.4464(5) -0.1110(8) 1.1136(6) 0.053(3) Uani 1 1 d . . . H23A H 0.3944 -0.1272 1.1177 0.063 Uiso 1 1 calc R . . C24 C 0.4895(6) -0.0791(7) 1.1726(5) 0.053(3) Uani 1 1 d . . . H24A H 0.4656 -0.0698 1.2162 0.064 Uiso 1 1 calc R . . C25 C 0.5662(6) -0.0612(7) 1.1678(5) 0.047(2) Uani 1 1 d . . . H25A H 0.5951 -0.0405 1.2083 0.056 Uiso 1 1 calc R . . C26 C 0.6009(5) -0.0734(6) 1.1045(4) 0.039(2) Uani 1 1 d . . . H26A H 0.6540 -0.0626 1.1017 0.047 Uiso 1 1 calc R . . C27 C 0.5775(4) -0.0083(6) 0.9125(4) 0.0260(19) Uani 1 1 d . . . C28 C 0.6088(4) 0.0049(6) 0.8466(5) 0.037(2) Uani 1 1 d . . . H28A H 0.6412 -0.0395 0.8280 0.044 Uiso 1 1 calc R . . C29 C 0.5927(5) 0.0828(7) 0.8075(5) 0.042(2) Uani 1 1 d . . . H29A H 0.6144 0.0917 0.7628 0.051 Uiso 1 1 calc R . . C30 C 0.5453(4) 0.1463(6) 0.8344(5) 0.041(2) Uani 1 1 d . . . H30A H 0.5335 0.1986 0.8074 0.049 Uiso 1 1 calc R . . C31 C 0.5146(4) 0.1359(7) 0.8991(5) 0.038(2) Uani 1 1 d . . . H31A H 0.4828 0.1811 0.9174 0.046 Uiso 1 1 calc R . . C32 C 0.5304(4) 0.0587(5) 0.9379(5) 0.0292(19) Uani 1 1 d . . . H32A H 0.5086 0.0512 0.9827 0.035 Uiso 1 1 calc R . . C33 C 0.9300(4) -0.0661(6) 1.0377(4) 0.0268(18) Uani 1 1 d . . . C34 C 1.0090(4) -0.0769(5) 1.0400(5) 0.032(2) Uani 1 1 d . . . H34A H 1.0343 -0.0896 0.9977 0.038 Uiso 1 1 calc R . . C35 C 1.0502(4) -0.0694(6) 1.1024(5) 0.035(2) Uani 1 1 d . . . H35A H 1.1041 -0.0759 1.1030 0.042 Uiso 1 1 calc R . . C36 C 1.0148(5) -0.0527(6) 1.1646(5) 0.037(2) Uani 1 1 d . . . H36A H 1.0437 -0.0489 1.2082 0.045 Uiso 1 1 calc R . . C37 C 0.9360(5) -0.0414(7) 1.1628(5) 0.040(2) Uani 1 1 d . . . H37A H 0.9112 -0.0297 1.2056 0.048 Uiso 1 1 calc R . . C38 C 0.8941(5) -0.0468(6) 1.1006(4) 0.034(2) Uani 1 1 d . . . H38A H 0.8405 -0.0376 1.1000 0.041 Uiso 1 1 calc R . . C39 C 0.8824(4) 0.0303(6) 0.9121(4) 0.031(2) Uani 1 1 d . . . C40 C 0.9363(4) 0.0943(6) 0.9314(5) 0.037(2) Uani 1 1 d . . . H40A H 0.9748 0.0804 0.9666 0.045 Uiso 1 1 calc R . . C41 C 0.9351(5) 0.1782(7) 0.9002(6) 0.045(2) Uani 1 1 d . . . H41A H 0.9725 0.2213 0.9148 0.054 Uiso 1 1 calc R . . C42 C 0.8823(5) 0.1999(7) 0.8500(5) 0.045(2) Uani 1 1 d . . . H42A H 0.8802 0.2587 0.8307 0.054 Uiso 1 1 calc R . . C43 C 0.8297(5) 0.1338(9) 0.8262(5) 0.053(3) Uani 1 1 d . . . H43A H 0.7945 0.1469 0.7880 0.063 Uiso 1 1 calc R . . C44 C 0.8286(5) 0.0505(7) 0.8576(5) 0.044(2) Uani 1 1 d . . . H44A H 0.7916 0.0073 0.8424 0.052 Uiso 1 1 calc R . . C45 C 0.4549(4) 0.2049(6) 0.5886(4) 0.0254(19) Uani 1 1 d . . . C46 C 0.5201(4) 0.1877(6) 0.6332(4) 0.032(2) Uani 1 1 d . . . H46A H 0.5361 0.1277 0.6422 0.039 Uiso 1 1 calc R . . C47 C 0.5614(4) 0.2597(6) 0.6643(4) 0.033(2) Uani 1 1 d . . . H47A H 0.6057 0.2483 0.6935 0.039 Uiso 1 1 calc R . . C48 C 0.5376(5) 0.3460(6) 0.6523(5) 0.037(2) Uani 1 1 d . . . H48A H 0.5667 0.3944 0.6719 0.044 Uiso 1 1 calc R . . C49 C 0.4715(4) 0.3633(6) 0.6120(5) 0.032(2) Uani 1 1 d . . . H49A H 0.4538 0.4232 0.6068 0.039 Uiso 1 1 calc R . . C50 C 0.4307(4) 0.2938(6) 0.5789(4) 0.0251(18) Uani 1 1 d . . . C51 C 0.3679(4) 0.3138(6) 0.5260(5) 0.030(2) Uani 1 1 d . . . C52 C 0.2675(4) 0.4085(5) 0.4767(4) 0.0334(19) Uani 1 1 d . . . H52A H 0.2554 0.3537 0.4479 0.040 Uiso 1 1 calc R . . C53 C 0.3030(5) 0.4789(6) 0.4280(5) 0.039(2) Uani 1 1 d . . . H53A H 0.3135 0.5346 0.4552 0.047 Uiso 1 1 calc R . . H53B H 0.3520 0.4560 0.4112 0.047 Uiso 1 1 calc R . . C54 C 0.2497(5) 0.4998(7) 0.3647(5) 0.055(3) Uani 1 1 d . . . H54A H 0.2726 0.5473 0.3357 0.066 Uiso 1 1 calc R . . H54B H 0.2434 0.4455 0.3348 0.066 Uiso 1 1 calc R . . C55 C 0.1721(5) 0.5305(7) 0.3879(5) 0.056(3) Uani 1 1 d . . . H55A H 0.1370 0.5367 0.3457 0.067 Uiso 1 1 calc R . . H55B H 0.1773 0.5901 0.4107 0.067 Uiso 1 1 calc R . . C56 C 0.1382(5) 0.4640(7) 0.4400(5) 0.046(2) Uani 1 1 d . . . H56A H 0.0894 0.4882 0.4563 0.055 Uiso 1 1 calc R . . H56B H 0.1271 0.4067 0.4152 0.055 Uiso 1 1 calc R . . C57 C 0.1920(4) 0.4461(6) 0.5045(4) 0.0361(19) Uani 1 1 d . . . H57A H 0.2038 0.5051 0.5275 0.043 Uiso 1 1 calc R . . C58 C 0.1343(4) 0.3043(7) 0.5442(5) 0.039(2) Uani 1 1 d . . . C59 C 0.0878(4) 0.2612(6) 0.6001(5) 0.040(2) Uani 1 1 d . . . C60 C 0.0451(5) 0.3140(8) 0.6454(6) 0.056(3) Uani 1 1 d . . . H60A H 0.0475 0.3775 0.6429 0.067 Uiso 1 1 calc R . . C61 C -0.0002(6) 0.2730(8) 0.6932(6) 0.071(4) Uani 1 1 d . . . H61A H -0.0302 0.3089 0.7229 0.085 Uiso 1 1 calc R . . C62 C -0.0031(6) 0.1818(7) 0.6993(6) 0.062(3) Uani 1 1 d . . . H62A H -0.0340 0.1545 0.7334 0.074 Uiso 1 1 calc R . . C63 C 0.0392(4) 0.1306(8) 0.6556(5) 0.049(2) Uani 1 1 d . . . H63A H 0.0373 0.0672 0.6599 0.059 Uiso 1 1 calc R . . C64 C 0.0849(5) 0.1682(7) 0.6050(5) 0.040(2) Uani 1 1 d . . . C65 C 0.4342(4) 0.0130(6) 0.5940(5) 0.030(2) Uani 1 1 d . . . C66 C 0.4022(4) 0.0036(6) 0.6607(5) 0.037(2) Uani 1 1 d . . . H66A H 0.3695 0.0486 0.6780 0.045 Uiso 1 1 calc R . . C67 C 0.4187(5) -0.0710(7) 0.7002(5) 0.043(2) Uani 1 1 d . . . H67A H 0.3994 -0.0755 0.7463 0.052 Uiso 1 1 calc R . . C68 C 0.4629(4) -0.1407(6) 0.6749(5) 0.041(2) Uani 1 1 d . . . H68A H 0.4717 -0.1933 0.7024 0.050 Uiso 1 1 calc R . . C69 C 0.4934(5) -0.1321(7) 0.6096(5) 0.040(2) Uani 1 1 d . . . H69A H 0.5237 -0.1789 0.5915 0.048 Uiso 1 1 calc R . . C70 C 0.4799(4) -0.0549(6) 0.5699(5) 0.037(2) Uani 1 1 d . . . H70A H 0.5026 -0.0488 0.5254 0.044 Uiso 1 1 calc R . . C71 C 0.4565(4) 0.1029(5) 0.4603(4) 0.0234(17) Uani 1 1 d . . . C72 C 0.4150(4) 0.0837(6) 0.3966(4) 0.035(2) Uani 1 1 d . . . H72A H 0.3617 0.0727 0.3971 0.042 Uiso 1 1 calc R . . C73 C 0.4519(5) 0.0809(6) 0.3329(4) 0.036(2) Uani 1 1 d . . . H73A H 0.4239 0.0696 0.2896 0.043 Uiso 1 1 calc R . . C74 C 0.5292(5) 0.0947(6) 0.3334(5) 0.038(2) Uani 1 1 d . . . H74A H 0.5548 0.0913 0.2901 0.046 Uiso 1 1 calc R . . C75 C 0.5699(4) 0.1131(6) 0.3939(4) 0.0331(19) Uani 1 1 d . . . H75A H 0.6233 0.1230 0.3924 0.040 Uiso 1 1 calc R . . C76 C 0.5350(4) 0.1179(6) 0.4585(4) 0.0318(18) Uani 1 1 d . . . H76A H 0.5641 0.1312 0.5007 0.038 Uiso 1 1 calc R . . C77 C 0.1286(4) -0.0161(6) 0.5851(5) 0.035(2) Uani 1 1 d . . . C78 C 0.0756(5) -0.0791(6) 0.5601(5) 0.043(2) Uani 1 1 d . . . H78A H 0.0418 -0.0647 0.5211 0.051 Uiso 1 1 calc R . . C79 C 0.0716(6) -0.1621(7) 0.5913(6) 0.051(3) Uani 1 1 d . . . H79A H 0.0336 -0.2037 0.5754 0.061 Uiso 1 1 calc R . . C80 C 0.1231(6) -0.1851(7) 0.6459(6) 0.054(3) Uani 1 1 d . . . H80A H 0.1206 -0.2430 0.6666 0.065 Uiso 1 1 calc R . . C81 C 0.1768(5) -0.1267(8) 0.6703(5) 0.050(3) Uani 1 1 d . . . H81A H 0.2121 -0.1429 0.7077 0.060 Uiso 1 1 calc R . . C82 C 0.1791(5) -0.0424(8) 0.6396(5) 0.050(3) Uani 1 1 d . . . H82A H 0.2169 -0.0011 0.6565 0.060 Uiso 1 1 calc R . . C83 C 0.0795(4) 0.0899(6) 0.4650(5) 0.032(2) Uani 1 1 d . . . C84 C 0.0014(4) 0.1027(5) 0.4642(5) 0.0312(19) Uani 1 1 d . . . H84A H -0.0227 0.1170 0.5069 0.037 Uiso 1 1 calc R . . C85 C -0.0421(5) 0.0947(6) 0.4013(5) 0.039(2) Uani 1 1 d . . . H85A H -0.0956 0.1045 0.4004 0.047 Uiso 1 1 calc R . . C86 C -0.0065(5) 0.0725(7) 0.3403(5) 0.043(2) Uani 1 1 d . . . H86A H -0.0367 0.0645 0.2978 0.051 Uiso 1 1 calc R . . C87 C 0.0712(5) 0.0613(7) 0.3386(5) 0.049(3) Uani 1 1 d . . . H87A H 0.0947 0.0485 0.2954 0.059 Uiso 1 1 calc R . . C88 C 0.1144(4) 0.0690(6) 0.4014(5) 0.038(2) Uani 1 1 d . . . H88A H 0.1681 0.0602 0.4016 0.046 Uiso 1 1 calc R . . C89 C 0.7489(4) 0.4313(7) 0.7494(5) 0.037(2) Uani 1 1 d . . . C90 C 0.7414(4) 0.5097(6) 0.8035(5) 0.0307(19) Uani 1 1 d . . . C91 C 0.2484(4) 0.5866(7) 0.7478(5) 0.043(2) Uani 1 1 d . . . C92 C 0.2407(5) 0.5092(6) 0.6954(4) 0.034(2) Uani 1 1 d . . . C93 C 0.3056(8) 0.8267(13) 0.5078(9) 0.124(7) Uani 1 1 d . . . H93A H 0.3411 0.7989 0.5428 0.186 Uiso 1 1 calc R . . H93B H 0.2834 0.8806 0.5283 0.186 Uiso 1 1 calc R . . H93C H 0.3331 0.8430 0.4656 0.186 Uiso 1 1 calc R . . C94 C 0.2449(10) 0.7632(11) 0.4882(10) 0.104(5) Uani 1 1 d . . . C95 C 0.1892(8) 0.7938(10) 0.4341(9) 0.100(5) Uani 1 1 d . . . H95A H 0.1522 0.7459 0.4235 0.151 Uiso 1 1 calc R . . H95B H 0.2154 0.8094 0.3910 0.151 Uiso 1 1 calc R . . H95C H 0.1625 0.8467 0.4514 0.151 Uiso 1 1 calc R . . C96 C 0.3496(8) 0.2428(13) 0.7686(8) 0.129(8) Uani 1 1 d . . . H96A H 0.3867 0.2099 0.7412 0.193 Uiso 1 1 calc R . . H96B H 0.3559 0.2263 0.8187 0.193 Uiso 1 1 calc R . . H96C H 0.3579 0.3074 0.7633 0.193 Uiso 1 1 calc R . . C97 C 0.2725(7) 0.2201(9) 0.7425(6) 0.067(3) Uani 1 1 d . . . C98 C 0.2046(8) 0.2630(11) 0.7747(7) 0.102(5) Uani 1 1 d . . . H98A H 0.1577 0.2424 0.7497 0.153 Uiso 1 1 calc R . . H98B H 0.2084 0.3283 0.7706 0.153 Uiso 1 1 calc R . . H98C H 0.2034 0.2464 0.8249 0.153 Uiso 1 1 calc R . . C99 C 0.6614(6) -1.2408(9) 0.7375(6) 0.076(4) Uani 1 1 d . . . H99A H 0.6220 -1.2103 0.7639 0.114 Uiso 1 1 calc R . . H99B H 0.6569 -1.3057 0.7440 0.114 Uiso 1 1 calc R . . H99C H 0.6547 -1.2263 0.6870 0.114 Uiso 1 1 calc R . . C100 C 0.7369(5) -1.2110(7) 0.7639(5) 0.043(2) Uani 1 1 d . . . C101 C 0.8037(6) -1.2499(9) 0.7298(6) 0.071(4) Uani 1 1 d . . . H01A H 0.8506 -1.2237 0.7508 0.106 Uiso 1 1 calc R . . H01B H 0.8002 -1.2369 0.6789 0.106 Uiso 1 1 calc R . . H01C H 0.8044 -1.3150 0.7371 0.106 Uiso 1 1 calc R . . C102 C 0.7044(8) -1.8142(13) 0.9830(9) 0.128(7) Uani 1 1 d . . . H02A H 0.6700 -1.7920 0.9446 0.192 Uiso 1 1 calc R . . H02B H 0.6753 -1.8255 1.0252 0.192 Uiso 1 1 calc R . . H02C H 0.7284 -1.8700 0.9680 0.192 Uiso 1 1 calc R . . C103 C 0.7638(7) -1.7467(10) 0.9995(7) 0.068(3) Uani 1 1 d . . . C104 C 0.8242(7) -1.7626(10) 1.0558(8) 0.089(4) Uani 1 1 d . . . H04A H 0.8590 -1.7113 1.0583 0.133 Uiso 1 1 calc R . . H04B H 0.8527 -1.8169 1.0446 0.133 Uiso 1 1 calc R . . H04C H 0.8005 -1.7702 1.1015 0.133 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0222(3) 0.0312(4) 0.0378(4) -0.0012(3) 0.0008(2) -0.0025(2) F1 0.061(3) 0.059(5) 0.098(5) -0.034(4) 0.020(3) -0.025(3) P1 0.0215(8) 0.0259(12) 0.0273(11) -0.0022(10) 0.0022(7) 0.0019(9) N1 0.030(3) 0.018(4) 0.033(4) 0.000(3) -0.004(3) 0.001(3) O1 0.035(3) 0.024(3) 0.035(3) -0.002(3) -0.003(2) 0.001(2) C1 0.022(4) 0.037(6) 0.029(5) -0.004(4) 0.001(3) 0.010(3) Ag2 0.0226(3) 0.0304(4) 0.0389(4) -0.0025(3) 0.0043(2) -0.0021(2) F2 0.076(4) 0.113(6) 0.038(4) -0.014(4) -0.008(3) 0.021(4) P2 0.0227(9) 0.0317(13) 0.0314(12) -0.0045(10) 0.0036(8) -0.0010(8) N2 0.032(3) 0.027(4) 0.032(4) -0.006(3) 0.003(3) -0.003(3) O2 0.063(4) 0.030(4) 0.042(4) -0.007(3) 0.014(3) -0.011(3) C2 0.034(4) 0.024(5) 0.030(5) 0.004(4) 0.000(3) 0.007(3) O3 0.034(3) 0.029(3) 0.029(3) -0.005(3) -0.004(2) 0.007(2) N3 0.036(3) 0.028(4) 0.033(4) -0.005(3) 0.002(3) 0.005(3) F3 0.037(2) 0.055(4) 0.072(4) -0.026(3) -0.004(2) 0.007(2) P3 0.0241(9) 0.0248(13) 0.0268(11) -0.0012(10) 0.0038(7) -0.0028(8) C3 0.029(4) 0.024(5) 0.034(5) -0.006(4) -0.007(3) 0.001(3) N4 0.037(3) 0.025(4) 0.052(4) -0.011(4) 0.013(3) -0.006(3) O4 0.053(4) 0.037(4) 0.060(5) -0.017(3) 0.019(3) -0.007(3) F4 0.056(3) 0.062(5) 0.076(4) -0.019(3) 0.017(3) -0.023(3) P4 0.0232(9) 0.0302(13) 0.0374(13) -0.0073(10) 0.0079(8) -0.0062(8) C4 0.027(4) 0.035(5) 0.026(5) -0.004(4) -0.003(3) -0.006(3) O5 0.025(3) 0.055(4) 0.045(4) -0.006(3) 0.003(2) 0.005(3) F5 0.036(2) 0.058(4) 0.086(4) -0.028(3) 0.002(2) 0.007(3) C5 0.036(4) 0.024(5) 0.022(5) -0.001(4) 0.002(3) -0.003(3) O6 0.031(3) 0.044(4) 0.059(4) -0.015(3) -0.005(3) -0.007(3) F6 0.095(4) 0.083(5) 0.038(4) -0.004(3) -0.024(3) 0.008(4) C6 0.025(4) 0.033(5) 0.026(5) -0.001(4) -0.004(3) -0.001(3) C7 0.024(4) 0.025(5) 0.024(4) 0.000(4) -0.003(3) 0.000(3) O7 0.029(3) 0.048(4) 0.063(4) -0.011(3) 0.013(3) -0.003(3) C8 0.031(4) 0.028(5) 0.039(5) 0.009(4) 0.006(3) 0.001(3) O8 0.033(3) 0.054(4) 0.046(4) -0.011(3) -0.001(3) -0.011(3) C9 0.038(5) 0.031(5) 0.046(6) 0.011(4) 0.010(4) 0.008(4) O9 0.201(12) 0.084(9) 0.142(11) 0.001(8) -0.051(9) 0.026(9) C10 0.047(5) 0.040(5) 0.045(5) 0.013(4) 0.002(4) 0.000(4) O10 0.072(5) 0.084(7) 0.087(6) -0.042(6) -0.006(4) 0.002(4) C11 0.036(5) 0.053(6) 0.048(6) 0.017(5) 0.000(4) 0.012(4) O11 0.059(4) 0.068(6) 0.071(5) -0.032(4) -0.008(4) 0.010(4) C12 0.036(5) 0.043(6) 0.043(6) 0.004(4) -0.004(4) 0.005(4) O12 0.187(11) 0.088(9) 0.075(7) -0.006(6) 0.010(7) 0.013(8) C13 0.022(4) 0.042(5) 0.036(5) 0.007(4) 0.000(3) -0.002(3) C14 0.023(4) 0.022(5) 0.047(6) 0.001(4) 0.001(3) 0.002(3) C15 0.027(4) 0.036(5) 0.028(5) -0.009(4) 0.002(3) -0.004(3) C16 0.031(4) 0.031(5) 0.057(6) -0.012(4) 0.003(4) 0.001(4) C17 0.039(5) 0.034(6) 0.064(7) -0.018(5) 0.019(4) 0.002(4) C18 0.038(5) 0.053(7) 0.061(7) -0.011(5) 0.017(4) -0.002(4) C19 0.034(4) 0.046(6) 0.041(5) -0.010(5) 0.016(3) -0.007(4) C20 0.017(3) 0.029(5) 0.045(5) -0.004(4) -0.007(3) -0.001(3) C21 0.038(4) 0.023(5) 0.035(5) 0.007(4) 0.004(3) 0.007(4) C22 0.043(4) 0.019(4) 0.041(5) -0.002(4) 0.011(3) 0.013(4) C23 0.055(5) 0.044(6) 0.062(7) 0.002(6) 0.031(5) 0.006(5) C24 0.087(8) 0.041(6) 0.034(6) 0.016(5) 0.030(5) 0.031(5) C25 0.072(7) 0.036(6) 0.032(5) -0.004(4) 0.003(4) 0.020(5) C26 0.052(5) 0.037(5) 0.027(5) 0.005(4) -0.005(4) 0.017(4) C27 0.020(4) 0.025(5) 0.033(5) -0.007(4) 0.003(3) 0.000(3) C28 0.042(5) 0.033(5) 0.035(5) 0.000(4) 0.007(4) 0.003(4) C29 0.049(5) 0.042(6) 0.036(5) 0.014(5) 0.008(4) 0.000(4) C30 0.041(4) 0.033(6) 0.049(6) 0.019(4) 0.002(4) 0.009(4) C31 0.044(4) 0.027(5) 0.046(6) 0.004(5) 0.013(4) 0.007(4) C32 0.035(4) 0.021(5) 0.033(5) 0.003(4) 0.009(3) 0.002(3) C33 0.026(4) 0.022(4) 0.033(5) -0.003(4) 0.008(3) -0.005(3) C34 0.031(4) 0.023(4) 0.041(5) -0.002(4) 0.009(4) -0.007(3) C35 0.023(4) 0.032(5) 0.050(6) -0.007(4) -0.010(4) -0.006(3) C36 0.041(5) 0.027(5) 0.043(6) -0.002(4) -0.011(4) -0.008(4) C37 0.042(5) 0.042(6) 0.037(5) -0.013(5) 0.006(4) -0.008(4) C38 0.037(4) 0.032(5) 0.035(5) -0.004(4) 0.006(4) -0.002(4) C39 0.036(4) 0.028(5) 0.029(5) -0.005(4) 0.006(3) 0.004(4) C40 0.030(4) 0.035(6) 0.047(5) -0.001(4) 0.001(4) -0.010(3) C41 0.053(5) 0.029(5) 0.054(7) 0.003(5) 0.021(5) -0.002(4) C42 0.048(5) 0.035(6) 0.052(6) 0.006(5) 0.007(4) -0.002(4) C43 0.056(5) 0.055(7) 0.047(6) 0.021(6) -0.006(4) -0.001(6) C44 0.040(5) 0.048(7) 0.042(6) 0.006(5) -0.011(4) -0.012(4) C45 0.030(4) 0.028(5) 0.019(4) 0.003(4) 0.004(3) -0.010(3) C46 0.037(4) 0.029(5) 0.030(5) 0.001(4) -0.002(3) -0.003(4) C47 0.033(4) 0.039(6) 0.027(5) -0.002(4) -0.001(3) -0.009(4) C48 0.043(5) 0.035(5) 0.032(5) -0.007(4) 0.001(4) -0.007(4) C49 0.036(4) 0.025(6) 0.037(5) -0.001(4) 0.007(3) 0.000(3) C50 0.027(4) 0.022(5) 0.027(5) 0.003(4) 0.007(3) 0.003(3) C51 0.029(4) 0.017(4) 0.044(6) 0.004(4) 0.011(4) -0.004(3) C52 0.030(4) 0.028(5) 0.041(5) 0.006(4) -0.004(3) 0.002(3) C53 0.036(4) 0.037(5) 0.046(6) 0.011(4) -0.004(4) 0.001(4) C54 0.053(6) 0.053(6) 0.059(7) 0.026(5) 0.002(5) 0.005(5) C55 0.048(5) 0.044(6) 0.074(7) 0.018(5) -0.009(5) 0.016(4) C56 0.038(5) 0.040(6) 0.059(6) 0.003(5) -0.002(4) 0.010(4) C57 0.031(4) 0.032(5) 0.045(5) 0.003(4) 0.002(4) 0.000(3) C58 0.027(4) 0.035(5) 0.056(6) -0.007(5) 0.013(4) -0.005(4) C59 0.032(4) 0.029(5) 0.059(6) -0.009(5) 0.007(4) 0.000(4) C60 0.039(5) 0.058(7) 0.072(7) -0.028(6) 0.030(5) -0.011(5) C61 0.055(6) 0.077(9) 0.085(9) -0.036(7) 0.043(6) -0.018(6) C62 0.071(7) 0.041(6) 0.078(8) -0.029(6) 0.052(6) -0.027(5) C63 0.042(5) 0.046(6) 0.061(6) -0.006(6) 0.014(4) -0.010(5) C64 0.033(4) 0.050(6) 0.038(5) -0.017(5) 0.013(4) -0.006(4) C65 0.026(4) 0.027(5) 0.037(5) 0.002(4) 0.005(3) 0.002(3) C66 0.040(4) 0.035(5) 0.038(5) 0.002(4) 0.015(4) 0.013(4) C67 0.062(6) 0.038(6) 0.031(5) 0.008(4) 0.015(4) 0.005(4) C68 0.042(5) 0.040(6) 0.043(5) 0.010(4) 0.013(4) 0.011(4) C69 0.043(4) 0.034(6) 0.043(6) 0.005(4) 0.009(4) 0.011(4) C70 0.033(4) 0.037(6) 0.040(5) -0.002(4) 0.008(4) -0.001(4) C71 0.028(4) 0.020(5) 0.022(4) -0.003(3) 0.003(3) 0.007(3) C72 0.034(4) 0.033(5) 0.038(5) -0.004(4) -0.005(3) 0.009(4) C73 0.059(5) 0.035(5) 0.014(4) 0.000(4) 0.001(4) 0.012(4) C74 0.051(5) 0.031(5) 0.035(5) 0.004(4) 0.022(4) 0.007(4) C75 0.046(4) 0.023(5) 0.031(5) 0.001(4) 0.016(4) 0.004(4) C76 0.026(4) 0.032(5) 0.037(5) 0.000(4) 0.005(3) -0.003(4) C77 0.034(4) 0.040(6) 0.032(5) -0.004(4) 0.004(4) -0.010(4) C78 0.044(5) 0.030(5) 0.054(6) 0.000(5) 0.003(4) -0.003(4) C79 0.055(6) 0.031(6) 0.067(8) -0.001(5) -0.005(5) -0.015(4) C80 0.079(7) 0.034(6) 0.052(7) 0.010(5) 0.018(5) -0.006(5) C81 0.065(6) 0.046(7) 0.039(6) 0.012(6) -0.003(4) -0.007(6) C82 0.052(6) 0.059(8) 0.039(6) 0.015(6) -0.002(4) -0.014(5) C83 0.023(4) 0.024(5) 0.049(5) -0.007(4) 0.008(3) 0.003(3) C84 0.027(4) 0.022(5) 0.045(5) -0.007(4) 0.005(3) -0.001(3) C85 0.035(4) 0.028(5) 0.055(6) 0.016(4) 0.002(4) -0.005(3) C86 0.042(5) 0.047(6) 0.038(6) 0.006(5) -0.008(4) -0.014(4) C87 0.047(5) 0.054(7) 0.046(6) -0.007(5) -0.003(4) -0.002(5) C88 0.030(4) 0.030(5) 0.055(6) -0.013(4) 0.010(4) -0.010(4) C89 0.024(4) 0.046(6) 0.041(6) -0.003(5) 0.001(4) 0.002(4) C90 0.033(4) 0.022(4) 0.036(5) -0.003(4) -0.003(3) -0.003(3) C91 0.028(4) 0.053(7) 0.048(6) -0.011(5) -0.002(4) 0.003(4) C92 0.036(5) 0.035(5) 0.031(5) 0.013(4) 0.004(4) -0.001(4) C93 0.104(11) 0.129(16) 0.141(15) -0.069(13) 0.021(10) -0.019(11) C94 0.134(13) 0.054(10) 0.123(13) -0.001(10) -0.024(11) 0.021(9) C95 0.118(11) 0.065(9) 0.116(13) 0.010(9) -0.017(10) 0.004(8) C96 0.108(11) 0.171(18) 0.111(13) -0.083(13) 0.034(9) -0.076(12) C97 0.095(9) 0.053(8) 0.053(8) -0.010(7) 0.017(6) 0.008(7) C98 0.137(12) 0.098(13) 0.071(10) 0.001(9) 0.003(9) 0.056(10) C99 0.070(7) 0.085(10) 0.073(9) -0.016(7) -0.005(6) -0.030(7) C100 0.058(6) 0.029(6) 0.041(6) -0.013(5) -0.008(4) 0.000(4) C101 0.087(8) 0.059(8) 0.067(8) -0.015(7) 0.003(6) 0.025(6) C102 0.090(10) 0.156(18) 0.141(15) -0.059(14) 0.028(10) -0.041(11) C103 0.079(8) 0.071(9) 0.056(8) -0.022(7) 0.020(6) 0.017(7) C104 0.082(8) 0.090(11) 0.095(10) -0.018(8) 0.001(7) 0.020(8) _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 P2 2.390(2) . ? Ag1 P1 2.3926(18) . ? F1 C89 1.333(11) . ? P1 C21 1.803(8) . ? P1 C1 1.816(9) . ? P1 C27 1.823(9) . ? N1 C7 1.350(10) . ? N1 C8 1.458(10) . ? N1 H1A 0.8800 . ? O1 C7 1.227(9) . ? C1 C2 1.378(11) . ? C1 C6 1.432(12) . ? Ag2 P3 2.3823(18) . ? Ag2 P4 2.386(2) . ? F2 C89 1.321(11) . ? P2 C33 1.814(8) . ? P2 C39 1.837(9) . ? P2 C20 1.840(8) . ? N2 C14 1.328(10) . ? N2 C13 1.473(10) . ? N2 H2B 0.8800 . ? O2 C14 1.222(10) . ? C2 C3 1.375(11) . ? C2 H2A 0.9500 . ? O3 C51 1.251(10) . ? N3 C51 1.337(11) . ? N3 C52 1.458(10) . ? N3 H3B 0.8800 . ? F3 C89 1.316(9) . ? P3 C71 1.818(7) . ? P3 C45 1.827(8) . ? P3 C65 1.836(9) . ? C3 C4 1.380(12) . ? C3 H3A 0.9500 . ? N4 C58 1.362(12) . ? N4 C57 1.438(10) . ? N4 H4B 0.8800 . ? O4 C58 1.252(11) . ? F4 C91 1.336(11) . ? P4 C83 1.804(9) . ? P4 C77 1.833(10) . ? P4 C64 1.834(9) . ? C4 C5 1.392(10) . ? C4 H4A 0.9500 . ? O5 C90 1.235(9) . ? F5 C91 1.373(10) . ? C5 C6 1.378(11) . ? C5 H5A 0.9500 . ? O6 C90 1.248(9) . ? F6 C91 1.367(11) . ? C6 C7 1.514(10) . ? O7 C92 1.234(10) . ? C8 C9 1.529(11) . ? C8 C13 1.534(11) . ? C8 H8A 1.0000 . ? O8 C92 1.239(10) . ? C9 C10 1.550(11) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? O9 C94 1.21(2) . ? C10 C11 1.516(12) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? O10 C97 1.228(14) . ? C11 C12 1.505(12) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? O11 C100 1.207(11) . ? C12 C13 1.533(11) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? O12 C103 1.221(16) . ? C13 H13A 1.0000 . ? C14 C15 1.513(12) . ? C15 C16 1.374(12) . ? C15 C20 1.401(12) . ? C16 C17 1.405(12) . ? C16 H16A 0.9500 . ? C17 C18 1.369(14) . ? C17 H17A 0.9500 . ? C18 C19 1.387(13) . ? C18 H18A 0.9500 . ? C19 C20 1.403(12) . ? C19 H19A 0.9500 . ? C21 C26 1.380(12) . ? C21 C22 1.409(11) . ? C22 C23 1.360(12) . ? C22 H22A 0.9500 . ? C23 C24 1.401(15) . ? C23 H23A 0.9500 . ? C24 C25 1.377(14) . ? C24 H24A 0.9500 . ? C25 C26 1.377(13) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 C28 1.396(12) . ? C27 C32 1.395(11) . ? C28 C29 1.400(12) . ? C28 H28A 0.9500 . ? C29 C30 1.371(13) . ? C29 H29A 0.9500 . ? C30 C31 1.365(12) . ? C30 H30A 0.9500 . ? C31 C32 1.387(12) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 C34 1.394(10) . ? C33 C38 1.399(11) . ? C34 C35 1.360(12) . ? C34 H34A 0.9500 . ? C35 C36 1.374(13) . ? C35 H35A 0.9500 . ? C36 C37 1.390(12) . ? C36 H36A 0.9500 . ? C37 C38 1.362(12) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C40 1.382(12) . ? C39 C44 1.399(12) . ? C40 C41 1.384(13) . ? C40 H40A 0.9500 . ? C41 C42 1.336(13) . ? C41 H41A 0.9500 . ? C42 C43 1.411(14) . ? C42 H42A 0.9500 . ? C43 C44 1.377(15) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? C45 C50 1.403(12) . ? C45 C46 1.415(11) . ? C46 C47 1.409(12) . ? C46 H46A 0.9500 . ? C47 C48 1.370(13) . ? C47 H47A 0.9500 . ? C48 C49 1.384(12) . ? C48 H48A 0.9500 . ? C49 C50 1.393(12) . ? C49 H49A 0.9500 . ? C50 C51 1.486(11) . ? C52 C53 1.544(11) . ? C52 C57 1.551(11) . ? C52 H52A 1.0000 . ? C53 C54 1.517(12) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.519(13) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.536(13) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.533(12) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 H57A 1.0000 . ? C58 C59 1.505(13) . ? C59 C64 1.391(13) . ? C59 C60 1.403(13) . ? C60 C61 1.371(15) . ? C60 H60A 0.9500 . ? C61 C62 1.366(16) . ? C61 H61A 0.9500 . ? C62 C63 1.368(13) . ? C62 H62A 0.9500 . ? C63 C64 1.391(13) . ? C63 H63A 0.9500 . ? C65 C70 1.382(12) . ? C65 C66 1.407(12) . ? C66 C67 1.364(13) . ? C66 H66A 0.9500 . ? C67 C68 1.394(12) . ? C67 H67A 0.9500 . ? C68 C69 1.370(12) . ? C68 H68A 0.9500 . ? C69 C70 1.389(13) . ? C69 H69A 0.9500 . ? C70 H70A 0.9500 . ? C71 C76 1.396(10) . ? C71 C72 1.409(11) . ? C72 C73 1.390(12) . ? C72 H72A 0.9500 . ? C73 C74 1.372(12) . ? C73 H73A 0.9500 . ? C74 C75 1.350(12) . ? C74 H74A 0.9500 . ? C75 C76 1.389(10) . ? C75 H75A 0.9500 . ? C76 H76A 0.9500 . ? C77 C82 1.386(13) . ? C77 C78 1.391(13) . ? C78 C79 1.374(13) . ? C78 H78A 0.9500 . ? C79 C80 1.384(14) . ? C79 H79A 0.9500 . ? C80 C81 1.349(15) . ? C80 H80A 0.9500 . ? C81 C82 1.386(15) . ? C81 H81A 0.9500 . ? C82 H82A 0.9500 . ? C83 C84 1.383(10) . ? C83 C88 1.404(11) . ? C84 C85 1.390(12) . ? C84 H84A 0.9500 . ? C85 C86 1.372(13) . ? C85 H85A 0.9500 . ? C86 C87 1.375(12) . ? C86 H86A 0.9500 . ? C87 C88 1.385(12) . ? C87 H87A 0.9500 . ? C88 H88A 0.9500 . ? C89 C90 1.562(13) . ? C91 C92 1.522(13) . ? C93 C94 1.46(2) . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? C94 C95 1.46(2) . ? C95 H95A 0.9800 . ? C95 H95B 0.9800 . ? C95 H95C 0.9800 . ? C96 C97 1.459(17) . ? C96 H96A 0.9800 . ? C96 H96B 0.9800 . ? C96 H96C 0.9800 . ? C97 C98 1.503(16) . ? C98 H98A 0.9800 . ? C98 H98B 0.9800 . ? C98 H98C 0.9800 . ? C99 C100 1.465(13) . ? C99 H99A 0.9800 . ? C99 H99B 0.9800 . ? C99 H99C 0.9800 . ? C100 C101 1.479(14) . ? C101 H01A 0.9800 . ? C101 H01B 0.9800 . ? C101 H01C 0.9800 . ? C102 C103 1.474(19) . ? C102 H02A 0.9800 . ? C102 H02B 0.9800 . ? C102 H02C 0.9800 . ? C103 C104 1.486(17) . ? C104 H04A 0.9800 . ? C104 H04B 0.9800 . ? C104 H04C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Ag1 P1 162.26(9) . . ? C21 P1 C1 103.2(4) . . ? C21 P1 C27 105.7(4) . . ? C1 P1 C27 102.0(4) . . ? C21 P1 Ag1 117.3(3) . . ? C1 P1 Ag1 119.8(2) . . ? C27 P1 Ag1 107.1(2) . . ? C7 N1 C8 124.0(7) . . ? C7 N1 H1A 118.0 . . ? C8 N1 H1A 118.0 . . ? C2 C1 C6 117.8(8) . . ? C2 C1 P1 120.7(7) . . ? C6 C1 P1 121.4(6) . . ? P3 Ag2 P4 162.85(8) . . ? C33 P2 C39 103.5(4) . . ? C33 P2 C20 105.8(4) . . ? C39 P2 C20 105.0(4) . . ? C33 P2 Ag1 117.8(2) . . ? C39 P2 Ag1 110.8(3) . . ? C20 P2 Ag1 112.7(3) . . ? C14 N2 C13 118.4(7) . . ? C14 N2 H2B 120.8 . . ? C13 N2 H2B 120.8 . . ? C3 C2 C1 122.0(8) . . ? C3 C2 H2A 119.0 . . ? C1 C2 H2A 119.0 . . ? C51 N3 C52 119.3(7) . . ? C51 N3 H3B 120.4 . . ? C52 N3 H3B 120.4 . . ? C71 P3 C45 103.5(3) . . ? C71 P3 C65 105.0(4) . . ? C45 P3 C65 104.1(4) . . ? C71 P3 Ag2 119.1(2) . . ? C45 P3 Ag2 114.1(3) . . ? C65 P3 Ag2 109.7(2) . . ? C2 C3 C4 120.1(7) . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C58 N4 C57 124.2(8) . . ? C58 N4 H4B 117.9 . . ? C57 N4 H4B 117.9 . . ? C83 P4 C77 104.1(4) . . ? C83 P4 C64 105.1(4) . . ? C77 P4 C64 103.7(4) . . ? C83 P4 Ag2 117.5(3) . . ? C77 P4 Ag2 107.8(3) . . ? C64 P4 Ag2 117.2(3) . . ? C3 C4 C5 119.6(7) . . ? C3 C4 H4A 120.2 . . ? C5 C4 H4A 120.2 . . ? C6 C5 C4 120.7(8) . . ? C6 C5 H5A 119.6 . . ? C4 C5 H5A 119.6 . . ? C5 C6 C1 119.7(7) . . ? C5 C6 C7 120.2(8) . . ? C1 C6 C7 119.8(7) . . ? O1 C7 N1 125.6(7) . . ? O1 C7 C6 118.9(7) . . ? N1 C7 C6 115.3(7) . . ? N1 C8 C9 111.0(6) . . ? N1 C8 C13 113.5(6) . . ? C9 C8 C13 110.0(7) . . ? N1 C8 H8A 107.4 . . ? C9 C8 H8A 107.4 . . ? C13 C8 H8A 107.4 . . ? C8 C9 C10 111.1(6) . . ? C8 C9 H9A 109.4 . . ? C10 C9 H9A 109.4 . . ? C8 C9 H9B 109.4 . . ? C10 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C11 C10 C9 110.7(7) . . ? C11 C10 H10A 109.5 . . ? C9 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? C12 C11 C10 111.5(7) . . ? C12 C11 H11A 109.3 . . ? C10 C11 H11A 109.3 . . ? C12 C11 H11B 109.3 . . ? C10 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? C11 C12 C13 110.9(7) . . ? C11 C12 H12A 109.5 . . ? C13 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 108.0 . . ? N2 C13 C12 111.5(6) . . ? N2 C13 C8 111.2(6) . . ? C12 C13 C8 109.9(7) . . ? N2 C13 H13A 108.0 . . ? C12 C13 H13A 108.0 . . ? C8 C13 H13A 108.0 . . ? O2 C14 N2 122.1(8) . . ? O2 C14 C15 119.1(8) . . ? N2 C14 C15 118.7(8) . . ? C16 C15 C20 120.2(8) . . ? C16 C15 C14 121.1(8) . . ? C20 C15 C14 118.4(7) . . ? C15 C16 C17 120.0(9) . . ? C15 C16 H16A 120.0 . . ? C17 C16 H16A 120.0 . . ? C18 C17 C16 119.8(8) . . ? C18 C17 H17A 120.1 . . ? C16 C17 H17A 120.1 . . ? C17 C18 C19 121.2(9) . . ? C17 C18 H18A 119.4 . . ? C19 C18 H18A 119.4 . . ? C18 C19 C20 119.2(10) . . ? C18 C19 H19A 120.4 . . ? C20 C19 H19A 120.4 . . ? C15 C20 C19 119.6(8) . . ? C15 C20 P2 120.7(6) . . ? C19 C20 P2 119.7(7) . . ? C26 C21 C22 119.0(8) . . ? C26 C21 P1 119.4(6) . . ? C22 C21 P1 121.6(6) . . ? C23 C22 C21 121.0(8) . . ? C23 C22 H22A 119.5 . . ? C21 C22 H22A 119.5 . . ? C22 C23 C24 118.8(9) . . ? C22 C23 H23A 120.6 . . ? C24 C23 H23A 120.6 . . ? C25 C24 C23 120.6(9) . . ? C25 C24 H24A 119.7 . . ? C23 C24 H24A 119.7 . . ? C26 C25 C24 119.9(9) . . ? C26 C25 H25A 120.0 . . ? C24 C25 H25A 120.0 . . ? C25 C26 C21 120.4(9) . . ? C25 C26 H26A 119.8 . . ? C21 C26 H26A 119.8 . . ? C28 C27 C32 117.8(8) . . ? C28 C27 P1 117.8(6) . . ? C32 C27 P1 124.3(6) . . ? C27 C28 C29 120.6(8) . . ? C27 C28 H28A 119.7 . . ? C29 C28 H28A 119.7 . . ? C30 C29 C28 119.4(8) . . ? C30 C29 H29A 120.3 . . ? C28 C29 H29A 120.3 . . ? C31 C30 C29 121.4(9) . . ? C31 C30 H30A 119.3 . . ? C29 C30 H30A 119.3 . . ? C30 C31 C32 119.4(8) . . ? C30 C31 H31A 120.3 . . ? C32 C31 H31A 120.3 . . ? C31 C32 C27 121.4(8) . . ? C31 C32 H32A 119.3 . . ? C27 C32 H32A 119.3 . . ? C34 C33 C38 118.7(7) . . ? C34 C33 P2 122.1(6) . . ? C38 C33 P2 119.2(6) . . ? C35 C34 C33 120.5(8) . . ? C35 C34 H34A 119.7 . . ? C33 C34 H34A 119.7 . . ? C34 C35 C36 120.9(7) . . ? C34 C35 H35A 119.6 . . ? C36 C35 H35A 119.6 . . ? C35 C36 C37 119.1(8) . . ? C35 C36 H36A 120.5 . . ? C37 C36 H36A 120.5 . . ? C38 C37 C36 120.9(8) . . ? C38 C37 H37A 119.6 . . ? C36 C37 H37A 119.6 . . ? C37 C38 C33 120.0(8) . . ? C37 C38 H38A 120.0 . . ? C33 C38 H38A 120.0 . . ? C40 C39 C44 118.5(8) . . ? C40 C39 P2 124.6(7) . . ? C44 C39 P2 116.8(7) . . ? C39 C40 C41 121.0(9) . . ? C39 C40 H40A 119.5 . . ? C41 C40 H40A 119.5 . . ? C42 C41 C40 121.3(10) . . ? C42 C41 H41A 119.4 . . ? C40 C41 H41A 119.4 . . ? C41 C42 C43 118.7(10) . . ? C41 C42 H42A 120.7 . . ? C43 C42 H42A 120.7 . . ? C44 C43 C42 121.0(9) . . ? C44 C43 H43A 119.5 . . ? C42 C43 H43A 119.5 . . ? C43 C44 C39 119.3(9) . . ? C43 C44 H44A 120.3 . . ? C39 C44 H44A 120.3 . . ? C50 C45 C46 118.8(7) . . ? C50 C45 P3 121.1(6) . . ? C46 C45 P3 120.0(7) . . ? C47 C46 C45 119.8(8) . . ? C47 C46 H46A 120.1 . . ? C45 C46 H46A 120.1 . . ? C48 C47 C46 120.1(8) . . ? C48 C47 H47A 120.0 . . ? C46 C47 H47A 120.0 . . ? C47 C48 C49 120.5(8) . . ? C47 C48 H48A 119.8 . . ? C49 C48 H48A 119.8 . . ? C48 C49 C50 120.7(8) . . ? C48 C49 H49A 119.6 . . ? C50 C49 H49A 119.6 . . ? C49 C50 C45 119.9(7) . . ? C49 C50 C51 120.3(8) . . ? C45 C50 C51 119.3(7) . . ? O3 C51 N3 120.8(8) . . ? O3 C51 C50 118.1(7) . . ? N3 C51 C50 121.1(8) . . ? N3 C52 C53 110.8(6) . . ? N3 C52 C57 111.9(6) . . ? C53 C52 C57 109.1(6) . . ? N3 C52 H52A 108.3 . . ? C53 C52 H52A 108.3 . . ? C57 C52 H52A 108.3 . . ? C54 C53 C52 111.0(7) . . ? C54 C53 H53A 109.4 . . ? C52 C53 H53A 109.4 . . ? C54 C53 H53B 109.4 . . ? C52 C53 H53B 109.4 . . ? H53A C53 H53B 108.0 . . ? C55 C54 C53 111.3(8) . . ? C55 C54 H54A 109.4 . . ? C53 C54 H54A 109.4 . . ? C55 C54 H54B 109.4 . . ? C53 C54 H54B 109.4 . . ? H54A C54 H54B 108.0 . . ? C54 C55 C56 111.5(7) . . ? C54 C55 H55A 109.3 . . ? C56 C55 H55A 109.3 . . ? C54 C55 H55B 109.3 . . ? C56 C55 H55B 109.3 . . ? H55A C55 H55B 108.0 . . ? C57 C56 C55 112.3(7) . . ? C57 C56 H56A 109.1 . . ? C55 C56 H56A 109.1 . . ? C57 C56 H56B 109.1 . . ? C55 C56 H56B 109.1 . . ? H56A C56 H56B 107.9 . . ? N4 C57 C56 112.4(7) . . ? N4 C57 C52 114.3(7) . . ? C56 C57 C52 107.4(7) . . ? N4 C57 H57A 107.5 . . ? C56 C57 H57A 107.5 . . ? C52 C57 H57A 107.5 . . ? O4 C58 N4 124.0(8) . . ? O4 C58 C59 119.1(8) . . ? N4 C58 C59 116.8(8) . . ? C64 C59 C60 119.9(9) . . ? C64 C59 C58 119.7(8) . . ? C60 C59 C58 120.4(9) . . ? C61 C60 C59 119.3(11) . . ? C61 C60 H60A 120.3 . . ? C59 C60 H60A 120.3 . . ? C62 C61 C60 121.6(10) . . ? C62 C61 H61A 119.2 . . ? C60 C61 H61A 119.2 . . ? C63 C62 C61 118.8(10) . . ? C63 C62 H62A 120.6 . . ? C61 C62 H62A 120.6 . . ? C62 C63 C64 122.2(11) . . ? C62 C63 H63A 118.9 . . ? C64 C63 H63A 118.9 . . ? C63 C64 C59 118.1(9) . . ? C63 C64 P4 120.0(8) . . ? C59 C64 P4 121.9(7) . . ? C70 C65 C66 118.7(8) . . ? C70 C65 P3 124.4(7) . . ? C66 C65 P3 116.8(6) . . ? C67 C66 C65 119.2(8) . . ? C67 C66 H66A 120.4 . . ? C65 C66 H66A 120.4 . . ? C66 C67 C68 122.0(8) . . ? C66 C67 H67A 119.0 . . ? C68 C67 H67A 119.0 . . ? C69 C68 C67 118.8(9) . . ? C69 C68 H68A 120.6 . . ? C67 C68 H68A 120.6 . . ? C68 C69 C70 120.0(8) . . ? C68 C69 H69A 120.0 . . ? C70 C69 H69A 120.0 . . ? C65 C70 C69 121.2(8) . . ? C65 C70 H70A 119.4 . . ? C69 C70 H70A 119.4 . . ? C76 C71 C72 119.0(7) . . ? C76 C71 P3 121.6(6) . . ? C72 C71 P3 119.3(5) . . ? C73 C72 C71 120.2(7) . . ? C73 C72 H72A 119.9 . . ? C71 C72 H72A 119.9 . . ? C74 C73 C72 119.1(8) . . ? C74 C73 H73A 120.5 . . ? C72 C73 H73A 120.5 . . ? C75 C74 C73 121.5(8) . . ? C75 C74 H74A 119.2 . . ? C73 C74 H74A 119.2 . . ? C74 C75 C76 121.2(7) . . ? C74 C75 H75A 119.4 . . ? C76 C75 H75A 119.4 . . ? C75 C76 C71 119.0(7) . . ? C75 C76 H76A 120.5 . . ? C71 C76 H76A 120.5 . . ? C82 C77 C78 117.2(9) . . ? C82 C77 P4 119.5(7) . . ? C78 C77 P4 123.2(7) . . ? C79 C78 C77 120.6(10) . . ? C79 C78 H78A 119.7 . . ? C77 C78 H78A 119.7 . . ? C78 C79 C80 119.9(9) . . ? C78 C79 H79A 120.0 . . ? C80 C79 H79A 120.0 . . ? C81 C80 C79 121.2(10) . . ? C81 C80 H80A 119.4 . . ? C79 C80 H80A 119.4 . . ? C80 C81 C82 118.4(9) . . ? C80 C81 H81A 120.8 . . ? C82 C81 H81A 120.8 . . ? C77 C82 C81 122.6(9) . . ? C77 C82 H82A 118.7 . . ? C81 C82 H82A 118.7 . . ? C84 C83 C88 119.3(8) . . ? C84 C83 P4 121.8(6) . . ? C88 C83 P4 118.9(6) . . ? C83 C84 C85 120.2(8) . . ? C83 C84 H84A 119.9 . . ? C85 C84 H84A 119.9 . . ? C86 C85 C84 119.1(8) . . ? C86 C85 H85A 120.5 . . ? C84 C85 H85A 120.4 . . ? C85 C86 C87 122.4(9) . . ? C85 C86 H86A 118.8 . . ? C87 C86 H86A 118.8 . . ? C86 C87 C88 118.5(9) . . ? C86 C87 H87A 120.8 . . ? C88 C87 H87A 120.8 . . ? C87 C88 C83 120.5(8) . . ? C87 C88 H88A 119.7 . . ? C83 C88 H88A 119.7 . . ? F3 C89 F2 105.5(7) . . ? F3 C89 F1 107.7(8) . . ? F2 C89 F1 105.2(8) . . ? F3 C89 C90 114.6(7) . . ? F2 C89 C90 110.3(8) . . ? F1 C89 C90 112.9(7) . . ? O5 C90 O6 130.9(8) . . ? O5 C90 C89 113.8(7) . . ? O6 C90 C89 115.2(7) . . ? F4 C91 F6 105.8(7) . . ? F4 C91 F5 102.6(8) . . ? F6 C91 F5 104.9(7) . . ? F4 C91 C92 116.0(8) . . ? F6 C91 C92 111.8(8) . . ? F5 C91 C92 114.6(7) . . ? O7 C92 O8 132.3(9) . . ? O7 C92 C91 113.6(7) . . ? O8 C92 C91 114.0(7) . . ? C94 C93 H93A 109.5 . . ? C94 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C94 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? O9 C94 C95 121.5(17) . . ? O9 C94 C93 122.6(17) . . ? C95 C94 C93 115.8(16) . . ? C94 C95 H95A 109.5 . . ? C94 C95 H95B 109.5 . . ? H95A C95 H95B 109.5 . . ? C94 C95 H95C 109.5 . . ? H95A C95 H95C 109.5 . . ? H95B C95 H95C 109.5 . . ? C97 C96 H96A 109.5 . . ? C97 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? C97 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? O10 C97 C96 121.3(11) . . ? O10 C97 C98 118.5(13) . . ? C96 C97 C98 120.2(13) . . ? C97 C98 H98A 109.5 . . ? C97 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? C97 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? C100 C99 H99A 109.5 . . ? C100 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? C100 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? O11 C100 C99 121.0(10) . . ? O11 C100 C101 122.1(9) . . ? C99 C100 C101 117.0(10) . . ? C100 C101 H01A 109.5 . . ? C100 C101 H01B 109.5 . . ? H01A C101 H01B 109.5 . . ? C100 C101 H01C 109.5 . . ? H01A C101 H01C 109.5 . . ? H01B C101 H01C 109.5 . . ? C103 C102 H02A 109.5 . . ? C103 C102 H02B 109.5 . . ? H02A C102 H02B 109.5 . . ? C103 C102 H02C 109.5 . . ? H02A C102 H02C 109.5 . . ? H02B C102 H02C 109.5 . . ? O12 C103 C102 120.2(15) . . ? O12 C103 C104 118.6(14) . . ? C102 C103 C104 121.2(16) . . ? C103 C104 H04A 109.5 . . ? C103 C104 H04B 109.5 . . ? H04A C104 H04B 109.5 . . ? C103 C104 H04C 109.5 . . ? H04A C104 H04C 109.5 . . ? H04B C104 H04C 109.5 . . ? 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 P2 Ag1 P1 C21 -106.2(4) . . . . ? P2 Ag1 P1 C1 127.5(4) . . . . ? P2 Ag1 P1 C27 12.3(4) . . . . ? C21 P1 C1 C2 86.7(7) . . . . ? C27 P1 C1 C2 -22.9(8) . . . . ? Ag1 P1 C1 C2 -140.7(6) . . . . ? C21 P1 C1 C6 -89.3(7) . . . . ? C27 P1 C1 C6 161.2(7) . . . . ? Ag1 P1 C1 C6 43.3(8) . . . . ? P1 Ag1 P2 C33 110.5(4) . . . . ? P1 Ag1 P2 C39 -8.4(4) . . . . ? P1 Ag1 P2 C20 -125.8(4) . . . . ? C6 C1 C2 C3 2.9(13) . . . . ? P1 C1 C2 C3 -173.2(6) . . . . ? P4 Ag2 P3 C71 112.7(4) . . . . ? P4 Ag2 P3 C45 -124.6(4) . . . . ? P4 Ag2 P3 C65 -8.3(4) . . . . ? C1 C2 C3 C4 -2.8(13) . . . . ? P3 Ag2 P4 C83 -118.3(4) . . . . ? P3 Ag2 P4 C77 -1.3(4) . . . . ? P3 Ag2 P4 C64 115.0(4) . . . . ? C2 C3 C4 C5 -0.3(13) . . . . ? C3 C4 C5 C6 3.1(12) . . . . ? C4 C5 C6 C1 -2.9(12) . . . . ? C4 C5 C6 C7 170.3(7) . . . . ? C2 C1 C6 C5 0.0(12) . . . . ? P1 C1 C6 C5 176.0(6) . . . . ? C2 C1 C6 C7 -173.3(7) . . . . ? P1 C1 C6 C7 2.8(11) . . . . ? C8 N1 C7 O1 10.9(12) . . . . ? C8 N1 C7 C6 -163.6(7) . . . . ? C5 C6 C7 O1 -141.5(8) . . . . ? C1 C6 C7 O1 31.7(11) . . . . ? C5 C6 C7 N1 33.4(11) . . . . ? C1 C6 C7 N1 -153.4(7) . . . . ? C7 N1 C8 C9 61.6(10) . . . . ? C7 N1 C8 C13 -62.9(9) . . . . ? N1 C8 C9 C10 177.2(7) . . . . ? C13 C8 C9 C10 -56.4(9) . . . . ? C8 C9 C10 C11 54.9(10) . . . . ? C9 C10 C11 C12 -55.4(10) . . . . ? C10 C11 C12 C13 57.8(10) . . . . ? C14 N2 C13 C12 -90.1(9) . . . . ? C14 N2 C13 C8 146.9(7) . . . . ? C11 C12 C13 N2 177.4(7) . . . . ? C11 C12 C13 C8 -58.9(10) . . . . ? N1 C8 C13 N2 -53.0(9) . . . . ? C9 C8 C13 N2 -178.0(6) . . . . ? N1 C8 C13 C12 -177.0(7) . . . . ? C9 C8 C13 C12 58.0(9) . . . . ? C13 N2 C14 O2 -5.3(11) . . . . ? C13 N2 C14 C15 175.9(6) . . . . ? O2 C14 C15 C16 144.9(8) . . . . ? N2 C14 C15 C16 -36.3(11) . . . . ? O2 C14 C15 C20 -29.0(11) . . . . ? N2 C14 C15 C20 149.7(7) . . . . ? C20 C15 C16 C17 0.4(12) . . . . ? C14 C15 C16 C17 -173.5(8) . . . . ? C15 C16 C17 C18 -2.0(14) . . . . ? C16 C17 C18 C19 1.9(15) . . . . ? C17 C18 C19 C20 -0.2(14) . . . . ? C16 C15 C20 C19 1.3(12) . . . . ? C14 C15 C20 C19 175.3(7) . . . . ? C16 C15 C20 P2 179.9(6) . . . . ? C14 C15 C20 P2 -6.1(10) . . . . ? C18 C19 C20 C15 -1.4(12) . . . . ? C18 C19 C20 P2 180.0(7) . . . . ? C33 P2 C20 C15 84.3(7) . . . . ? C39 P2 C20 C15 -166.6(7) . . . . ? Ag1 P2 C20 C15 -45.8(7) . . . . ? C33 P2 C20 C19 -97.1(7) . . . . ? C39 P2 C20 C19 12.0(7) . . . . ? Ag1 P2 C20 C19 132.8(6) . . . . ? C1 P1 C21 C26 152.9(7) . . . . ? C27 P1 C21 C26 -100.4(7) . . . . ? Ag1 P1 C21 C26 18.9(8) . . . . ? C1 P1 C21 C22 -30.0(8) . . . . ? C27 P1 C21 C22 76.7(8) . . . . ? Ag1 P1 C21 C22 -164.0(6) . . . . ? C26 C21 C22 C23 -2.3(14) . . . . ? P1 C21 C22 C23 -179.5(8) . . . . ? C21 C22 C23 C24 5.0(15) . . . . ? C22 C23 C24 C25 -4.4(15) . . . . ? C23 C24 C25 C26 0.9(15) . . . . ? C24 C25 C26 C21 1.8(14) . . . . ? C22 C21 C26 C25 -1.2(13) . . . . ? P1 C21 C26 C25 176.0(7) . . . . ? C21 P1 C27 C28 176.7(6) . . . . ? C1 P1 C27 C28 -75.7(7) . . . . ? Ag1 P1 C27 C28 50.9(7) . . . . ? C21 P1 C27 C32 -0.4(8) . . . . ? C1 P1 C27 C32 107.2(7) . . . . ? Ag1 P1 C27 C32 -126.1(6) . . . . ? C32 C27 C28 C29 -0.2(12) . . . . ? P1 C27 C28 C29 -177.4(7) . . . . ? C27 C28 C29 C30 -0.5(13) . . . . ? C28 C29 C30 C31 1.4(14) . . . . ? C29 C30 C31 C32 -1.4(13) . . . . ? C30 C31 C32 C27 0.6(13) . . . . ? C28 C27 C32 C31 0.1(12) . . . . ? P1 C27 C32 C31 177.2(6) . . . . ? C39 P2 C33 C34 -81.6(8) . . . . ? C20 P2 C33 C34 28.6(8) . . . . ? Ag1 P2 C33 C34 155.7(6) . . . . ? C39 P2 C33 C38 99.7(7) . . . . ? C20 P2 C33 C38 -150.1(7) . . . . ? Ag1 P2 C33 C38 -23.0(8) . . . . ? C38 C33 C34 C35 0.5(12) . . . . ? P2 C33 C34 C35 -178.2(7) . . . . ? C33 C34 C35 C36 1.1(13) . . . . ? C34 C35 C36 C37 -1.5(14) . . . . ? C35 C36 C37 C38 0.1(14) . . . . ? C36 C37 C38 C33 1.5(14) . . . . ? C34 C33 C38 C37 -1.8(13) . . . . ? P2 C33 C38 C37 177.0(7) . . . . ? C33 P2 C39 C40 13.6(8) . . . . ? C20 P2 C39 C40 -97.1(8) . . . . ? Ag1 P2 C39 C40 140.9(7) . . . . ? C33 P2 C39 C44 -162.9(7) . . . . ? C20 P2 C39 C44 86.3(7) . . . . ? Ag1 P2 C39 C44 -35.6(8) . . . . ? C44 C39 C40 C41 3.2(13) . . . . ? P2 C39 C40 C41 -173.3(7) . . . . ? C39 C40 C41 C42 -0.7(14) . . . . ? C40 C41 C42 C43 -3.4(15) . . . . ? C41 C42 C43 C44 5.0(15) . . . . ? C42 C43 C44 C39 -2.5(15) . . . . ? C40 C39 C44 C43 -1.6(14) . . . . ? P2 C39 C44 C43 175.2(7) . . . . ? C71 P3 C45 C50 90.0(7) . . . . ? C65 P3 C45 C50 -160.4(6) . . . . ? Ag2 P3 C45 C50 -40.9(7) . . . . ? C71 P3 C45 C46 -87.6(7) . . . . ? C65 P3 C45 C46 22.0(7) . . . . ? Ag2 P3 C45 C46 141.5(6) . . . . ? C50 C45 C46 C47 -2.9(12) . . . . ? P3 C45 C46 C47 174.7(6) . . . . ? C45 C46 C47 C48 1.2(13) . . . . ? C46 C47 C48 C49 2.4(13) . . . . ? C47 C48 C49 C50 -4.3(13) . . . . ? C48 C49 C50 C45 2.5(12) . . . . ? C48 C49 C50 C51 -169.5(7) . . . . ? C46 C45 C50 C49 1.1(11) . . . . ? P3 C45 C50 C49 -176.5(6) . . . . ? C46 C45 C50 C51 173.1(7) . . . . ? P3 C45 C50 C51 -4.5(10) . . . . ? C52 N3 C51 O3 -6.9(11) . . . . ? C52 N3 C51 C50 171.3(7) . . . . ? C49 C50 C51 O3 141.0(8) . . . . ? C45 C50 C51 O3 -31.1(11) . . . . ? C49 C50 C51 N3 -37.2(11) . . . . ? C45 C50 C51 N3 150.7(7) . . . . ? C51 N3 C52 C53 -91.6(9) . . . . ? C51 N3 C52 C57 146.4(7) . . . . ? N3 C52 C53 C54 175.6(8) . . . . ? C57 C52 C53 C54 -60.8(10) . . . . ? C52 C53 C54 C55 56.1(11) . . . . ? C53 C54 C55 C56 -52.5(12) . . . . ? C54 C55 C56 C57 55.2(11) . . . . ? C58 N4 C57 C56 62.4(10) . . . . ? C58 N4 C57 C52 -60.3(10) . . . . ? C55 C56 C57 N4 174.8(8) . . . . ? C55 C56 C57 C52 -58.7(10) . . . . ? N3 C52 C57 N4 -50.9(9) . . . . ? C53 C52 C57 N4 -173.9(7) . . . . ? N3 C52 C57 C56 -176.3(7) . . . . ? C53 C52 C57 C56 60.7(9) . . . . ? C57 N4 C58 O4 6.9(13) . . . . ? C57 N4 C58 C59 -170.1(7) . . . . ? O4 C58 C59 C64 25.5(13) . . . . ? N4 C58 C59 C64 -157.3(8) . . . . ? O4 C58 C59 C60 -151.9(9) . . . . ? N4 C58 C59 C60 25.3(13) . . . . ? C64 C59 C60 C61 -1.1(15) . . . . ? C58 C59 C60 C61 176.3(9) . . . . ? C59 C60 C61 C62 1.8(18) . . . . ? C60 C61 C62 C63 -1.2(19) . . . . ? C61 C62 C63 C64 -0.2(17) . . . . ? C62 C63 C64 C59 0.9(15) . . . . ? C62 C63 C64 P4 -177.9(8) . . . . ? C60 C59 C64 C63 -0.2(14) . . . . ? C58 C59 C64 C63 -177.7(8) . . . . ? C60 C59 C64 P4 178.5(7) . . . . ? C58 C59 C64 P4 1.1(13) . . . . ? C83 P4 C64 C63 97.6(8) . . . . ? C77 P4 C64 C63 -11.4(8) . . . . ? Ag2 P4 C64 C63 -129.9(7) . . . . ? C83 P4 C64 C59 -81.2(8) . . . . ? C77 P4 C64 C59 169.9(8) . . . . ? Ag2 P4 C64 C59 51.3(9) . . . . ? C71 P3 C65 C70 -4.1(8) . . . . ? C45 P3 C65 C70 -112.5(7) . . . . ? Ag2 P3 C65 C70 125.0(7) . . . . ? C71 P3 C65 C66 -179.6(7) . . . . ? C45 P3 C65 C66 72.0(7) . . . . ? Ag2 P3 C65 C66 -50.5(7) . . . . ? C70 C65 C66 C67 1.6(13) . . . . ? P3 C65 C66 C67 177.3(7) . . . . ? C65 C66 C67 C68 -3.7(14) . . . . ? C66 C67 C68 C69 2.9(14) . . . . ? C67 C68 C69 C70 -0.1(13) . . . . ? C66 C65 C70 C69 1.2(13) . . . . ? P3 C65 C70 C69 -174.2(7) . . . . ? C68 C69 C70 C65 -2.0(13) . . . . ? C45 P3 C71 C76 35.5(8) . . . . ? C65 P3 C71 C76 -73.4(8) . . . . ? Ag2 P3 C71 C76 163.4(6) . . . . ? C45 P3 C71 C72 -141.5(7) . . . . ? C65 P3 C71 C72 109.6(7) . . . . ? Ag2 P3 C71 C72 -13.7(8) . . . . ? C76 C71 C72 C73 -0.7(12) . . . . ? P3 C71 C72 C73 176.4(6) . . . . ? C71 C72 C73 C74 1.7(13) . . . . ? C72 C73 C74 C75 -1.7(13) . . . . ? C73 C74 C75 C76 0.7(14) . . . . ? C74 C75 C76 C71 0.4(14) . . . . ? C72 C71 C76 C75 -0.3(12) . . . . ? P3 C71 C76 C75 -177.4(7) . . . . ? C83 P4 C77 C82 165.5(7) . . . . ? C64 P4 C77 C82 -84.8(8) . . . . ? Ag2 P4 C77 C82 40.0(8) . . . . ? C83 P4 C77 C78 -10.6(9) . . . . ? C64 P4 C77 C78 99.2(8) . . . . ? Ag2 P4 C77 C78 -136.0(7) . . . . ? C82 C77 C78 C79 3.4(14) . . . . ? P4 C77 C78 C79 179.5(7) . . . . ? C77 C78 C79 C80 -3.1(15) . . . . ? C78 C79 C80 C81 1.2(16) . . . . ? C79 C80 C81 C82 0.3(16) . . . . ? C78 C77 C82 C81 -1.9(15) . . . . ? P4 C77 C82 C81 -178.2(8) . . . . ? C80 C81 C82 C77 0.1(16) . . . . ? C77 P4 C83 C84 82.9(8) . . . . ? C64 P4 C83 C84 -25.8(8) . . . . ? Ag2 P4 C83 C84 -158.1(6) . . . . ? C77 P4 C83 C88 -95.0(7) . . . . ? C64 P4 C83 C88 156.3(7) . . . . ? Ag2 P4 C83 C88 23.9(8) . . . . ? C88 C83 C84 C85 0.2(12) . . . . ? P4 C83 C84 C85 -177.7(6) . . . . ? C83 C84 C85 C86 1.1(13) . . . . ? C84 C85 C86 C87 -2.7(14) . . . . ? C85 C86 C87 C88 2.8(16) . . . . ? C86 C87 C88 C83 -1.4(15) . . . . ? C84 C83 C88 C87 0.0(13) . . . . ? P4 C83 C88 C87 177.9(8) . . . . ? F3 C89 C90 O5 -169.1(8) . . . . ? F2 C89 C90 O5 72.1(9) . . . . ? F1 C89 C90 O5 -45.3(11) . . . . ? F3 C89 C90 O6 8.8(12) . . . . ? F2 C89 C90 O6 -110.0(9) . . . . ? F1 C89 C90 O6 132.6(8) . . . . ? F4 C91 C92 O7 38.3(11) . . . . ? F6 C91 C92 O7 -83.2(9) . . . . ? F5 C91 C92 O7 157.7(8) . . . . ? F4 C91 C92 O8 -142.7(8) . . . . ? F6 C91 C92 O8 95.8(9) . . . . ? F5 C91 C92 O8 -23.4(12) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.729 _refine_diff_density_min -1.634 _refine_diff_density_rms 0.249