# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_mah4 _database_code_depnum_ccdc_archive 'CCDC 915439' #TrackingRef 'allenylideneChemSci2012.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '3 in manuscript' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H41 Au Cl2 N2 O2' _chemical_formula_weight 753.53 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.2769(4) _cell_length_b 12.2829(5) _cell_length_c 22.2697(8) _cell_angle_alpha 90.00 _cell_angle_beta 91.868(2) _cell_angle_gamma 90.00 _cell_volume 3356.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedron _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 4.571 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5283 _exptl_absorpt_correction_T_max 0.6578 _exptl_absorpt_process_details ; Sheldrick, G. M. (2008). SADABS. University of G\"ottingen, Germany. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'ImuS microsource' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Bruker APEX-II Quazar' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 75424 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 30.69 _reflns_number_total 10380 _reflns_number_gt 7907 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0253P)^2^+4.7934P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10380 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0701 _refine_ls_wR_factor_gt 0.0629 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 0.736254(8) 0.244575(8) 0.191174(4) 0.02821(4) Uani 1 1 d . . . C1 C 0.8903(2) 0.2775(2) 0.16930(13) 0.0279(5) Uani 1 1 d . . . N2 N 0.92377(18) 0.32500(19) 0.11818(10) 0.0287(5) Uani 1 1 d . . . C3 C 1.0365(2) 0.3262(3) 0.11653(14) 0.0375(7) Uani 1 1 d . . . H3 H 1.0791 0.3548 0.0853 0.045 Uiso 1 1 calc R . . C4 C 1.0741(2) 0.2789(3) 0.16768(15) 0.0371(7) Uani 1 1 d . . . H4 H 1.1483 0.2679 0.1796 0.045 Uiso 1 1 calc R . . N5 N 0.98402(19) 0.24968(19) 0.19937(10) 0.0291(5) Uani 1 1 d . . . C11 C 0.8514(2) 0.3646(2) 0.07063(12) 0.0291(6) Uani 1 1 d . . . C12 C 0.8358(2) 0.4770(2) 0.06612(13) 0.0321(6) Uani 1 1 d . . . C13 C 0.7671(3) 0.5133(3) 0.01869(14) 0.0406(7) Uani 1 1 d . . . H13 H 0.7544 0.5891 0.0137 0.049 Uiso 1 1 calc R . . C14 C 0.7177(3) 0.4407(3) -0.02077(15) 0.0460(8) Uani 1 1 d . . . H14 H 0.6710 0.4669 -0.0524 0.055 Uiso 1 1 calc R . . C15 C 0.7355(3) 0.3306(3) -0.01466(14) 0.0428(8) Uani 1 1 d . . . H15 H 0.7012 0.2818 -0.0425 0.051 Uiso 1 1 calc R . . C16 C 0.8025(3) 0.2892(3) 0.03143(14) 0.0362(6) Uani 1 1 d . . . C17 C 0.8874(3) 0.5579(3) 0.10925(14) 0.0367(7) Uani 1 1 d . . . H17 H 0.9309 0.5166 0.1404 0.044 Uiso 1 1 calc R . . C19 C 0.8201(3) 0.1672(3) 0.03707(16) 0.0435(8) Uani 1 1 d . . . H19 H 0.8601 0.1535 0.0762 0.052 Uiso 1 1 calc R . . C21 C 0.9874(2) 0.1854(2) 0.25399(13) 0.0297(6) Uani 1 1 d . . . C22 C 0.9823(2) 0.0725(2) 0.24793(14) 0.0339(6) Uani 1 1 d . . . C23 C 0.9820(3) 0.0112(3) 0.30029(16) 0.0411(7) Uani 1 1 d . . . H23 H 0.9776 -0.0659 0.2978 0.049 Uiso 1 1 calc R . . C24 C 0.9882(3) 0.0609(3) 0.35588(15) 0.0422(8) Uani 1 1 d . . . H24 H 0.9874 0.0179 0.3913 0.051 Uiso 1 1 calc R . . C25 C 0.9957(3) 0.1726(3) 0.36029(14) 0.0397(7) Uani 1 1 d . . . H25 H 1.0009 0.2055 0.3989 0.048 Uiso 1 1 calc R . . C26 C 0.9956(2) 0.2385(2) 0.30927(14) 0.0323(6) Uani 1 1 d . . . C27 C 0.9768(3) 0.0166(3) 0.18717(16) 0.0470(8) Uani 1 1 d . . . H27 H 0.9795 0.0742 0.1555 0.056 Uiso 1 1 calc R . . C29 C 1.0043(3) 0.3609(3) 0.31453(15) 0.0404(7) Uani 1 1 d . . . H29 H 0.9871 0.3931 0.2741 0.048 Uiso 1 1 calc R . . C31 C 0.5851(3) 0.2070(3) 0.21175(15) 0.0359(6) Uani 1 1 d . . . C32 C 0.4951(2) 0.1829(3) 0.22613(14) 0.0372(7) Uani 1 1 d . . . C33 C 0.3860(2) 0.1606(3) 0.24445(15) 0.0402(7) Uani 1 1 d . . . O33 O 0.3053(2) 0.1969(3) 0.22017(15) 0.0791(10) Uani 1 1 d . . . O34 O 0.38359(19) 0.0940(2) 0.29122(11) 0.0537(7) Uani 1 1 d . . . C34 C 0.2770(3) 0.0680(5) 0.3130(2) 0.0720(14) Uani 1 1 d . . . H34A H 0.2848 0.0183 0.3473 0.086 Uiso 1 1 calc R . . H34B H 0.2332 0.0331 0.2809 0.086 Uiso 1 1 calc R . . H34C H 0.2409 0.1350 0.3256 0.086 Uiso 1 1 calc R . . C171 C 0.9647(4) 0.6337(4) 0.0769(2) 0.0671(12) Uani 1 1 d . . . H17A H 0.9979 0.6850 0.1058 0.080 Uiso 1 1 calc R . . H17B H 0.9238 0.6741 0.0456 0.080 Uiso 1 1 calc R . . H17C H 1.0219 0.5906 0.0585 0.080 Uiso 1 1 calc R . . C172 C 0.8017(4) 0.6244(5) 0.1410(2) 0.0801(16) Uani 1 1 d . . . H17D H 0.8378 0.6755 0.1689 0.096 Uiso 1 1 calc R . . H17E H 0.7546 0.5755 0.1632 0.096 Uiso 1 1 calc R . . H17F H 0.7576 0.6650 0.1111 0.096 Uiso 1 1 calc R . . C191 C 0.8896(5) 0.1250(4) -0.0122(3) 0.106(2) Uani 1 1 d . . . H19A H 0.9584 0.1655 -0.0121 0.127 Uiso 1 1 calc R . . H19B H 0.8510 0.1345 -0.0510 0.127 Uiso 1 1 calc R . . H19C H 0.9048 0.0475 -0.0055 0.127 Uiso 1 1 calc R . . C192 C 0.7144(4) 0.1045(3) 0.0378(2) 0.0697(12) Uani 1 1 d . . . H19D H 0.6703 0.1312 0.0706 0.084 Uiso 1 1 calc R . . H19E H 0.7300 0.0269 0.0438 0.084 Uiso 1 1 calc R . . H19F H 0.6743 0.1146 -0.0006 0.084 Uiso 1 1 calc R . . C271 C 1.0755(4) -0.0576(4) 0.1802(2) 0.0781(14) Uani 1 1 d . . . H27A H 1.0715 -0.0923 0.1406 0.094 Uiso 1 1 calc R . . H27B H 1.0759 -0.1137 0.2115 0.094 Uiso 1 1 calc R . . H27C H 1.1424 -0.0143 0.1841 0.094 Uiso 1 1 calc R . . C272 C 0.8701(4) -0.0451(3) 0.1779(2) 0.0673(12) Uani 1 1 d . . . H27D H 0.8682 -0.0799 0.1383 0.081 Uiso 1 1 calc R . . H27E H 0.8089 0.0057 0.1804 0.081 Uiso 1 1 calc R . . H27F H 0.8644 -0.1009 0.2091 0.081 Uiso 1 1 calc R . . C291 C 1.1191(4) 0.3935(4) 0.3332(3) 0.0851(17) Uani 1 1 d . . . H29A H 1.1236 0.4730 0.3364 0.102 Uiso 1 1 calc R . . H29B H 1.1697 0.3679 0.3032 0.102 Uiso 1 1 calc R . . H29C H 1.1385 0.3608 0.3723 0.102 Uiso 1 1 calc R . . C292 C 0.9257(5) 0.4077(4) 0.3584(3) 0.120(3) Uani 1 1 d . . . H29D H 0.9341 0.4870 0.3600 0.144 Uiso 1 1 calc R . . H29E H 0.9410 0.3769 0.3983 0.144 Uiso 1 1 calc R . . H29F H 0.8509 0.3896 0.3452 0.144 Uiso 1 1 calc R . . C41 C 0.3920(6) 0.2131(9) 0.0778(4) 0.180(5) Uani 1 1 d . . . H41A H 0.4357 0.1460 0.0836 0.216 Uiso 1 1 calc R . . H41B H 0.3798 0.2438 0.1181 0.216 Uiso 1 1 calc R . . Cl1 Cl 0.46763(14) 0.30391(14) 0.03921(7) 0.0984(5) Uani 1 1 d . . . Cl2 Cl 0.26936(18) 0.17766(16) 0.04671(11) 0.1343(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.02368(5) 0.03550(6) 0.02532(5) 0.00290(5) -0.00130(3) 0.00005(5) C1 0.0272(13) 0.0311(13) 0.0252(13) 0.0024(10) -0.0038(10) -0.0007(10) N2 0.0240(11) 0.0372(12) 0.0247(12) 0.0080(9) -0.0044(9) -0.0014(9) C3 0.0262(14) 0.0514(18) 0.0348(16) 0.0117(14) 0.0020(12) -0.0022(13) C4 0.0227(13) 0.0492(17) 0.0393(17) 0.0089(13) -0.0027(12) 0.0001(12) N5 0.0258(10) 0.0353(12) 0.0260(11) 0.0079(10) -0.0038(8) -0.0005(10) C11 0.0271(13) 0.0397(15) 0.0204(13) 0.0063(11) -0.0032(10) -0.0018(11) C12 0.0286(14) 0.0408(15) 0.0265(14) 0.0038(12) -0.0040(11) -0.0013(12) C13 0.0448(18) 0.0432(17) 0.0328(16) 0.0086(13) -0.0119(14) 0.0019(14) C14 0.049(2) 0.053(2) 0.0344(17) 0.0065(15) -0.0187(15) 0.0003(16) C15 0.0480(19) 0.0507(19) 0.0288(16) -0.0013(14) -0.0119(14) -0.0070(15) C16 0.0374(16) 0.0422(16) 0.0287(15) 0.0031(12) -0.0017(12) -0.0032(13) C17 0.0361(16) 0.0418(16) 0.0315(16) 0.0019(13) -0.0105(12) -0.0020(13) C19 0.052(2) 0.0409(17) 0.0368(18) -0.0002(14) -0.0055(15) -0.0050(15) C21 0.0247(13) 0.0367(14) 0.0272(14) 0.0094(11) -0.0054(10) 0.0017(11) C22 0.0328(15) 0.0367(15) 0.0320(15) 0.0052(12) -0.0033(12) 0.0003(12) C23 0.0403(17) 0.0366(16) 0.0459(19) 0.0099(14) -0.0083(14) -0.0007(13) C24 0.0413(18) 0.0484(18) 0.0364(17) 0.0188(14) -0.0072(14) -0.0023(14) C25 0.0377(17) 0.0531(19) 0.0277(16) 0.0063(14) -0.0058(13) -0.0030(14) C26 0.0284(13) 0.0371(15) 0.0309(14) 0.0058(12) -0.0059(10) 0.0009(11) C27 0.065(2) 0.0386(17) 0.0370(18) -0.0013(14) -0.0097(16) 0.0034(16) C29 0.0453(18) 0.0385(16) 0.0369(18) 0.0010(13) -0.0076(14) 0.0011(14) C31 0.0311(15) 0.0400(15) 0.0363(17) 0.0001(13) -0.0029(12) 0.0032(12) C32 0.0285(15) 0.0492(18) 0.0339(16) 0.0024(13) -0.0023(12) 0.0008(13) C33 0.0270(15) 0.0544(19) 0.0392(18) 0.0021(15) -0.0017(13) 0.0010(13) O33 0.0302(13) 0.125(3) 0.082(2) 0.049(2) -0.0026(14) 0.0079(16) O34 0.0311(12) 0.0839(19) 0.0461(15) 0.0198(14) 0.0027(10) -0.0010(12) C34 0.041(2) 0.111(4) 0.065(3) 0.029(3) 0.016(2) -0.003(2) C171 0.072(3) 0.071(3) 0.057(3) 0.010(2) -0.014(2) -0.033(2) C172 0.063(3) 0.111(4) 0.065(3) -0.045(3) -0.009(2) 0.008(3) C191 0.118(5) 0.055(3) 0.149(6) 0.006(3) 0.075(4) 0.012(3) C192 0.076(3) 0.047(2) 0.086(3) 0.003(2) 0.002(3) -0.015(2) C271 0.094(4) 0.082(3) 0.058(3) -0.018(2) 0.001(3) 0.026(3) C272 0.084(3) 0.053(2) 0.063(3) -0.002(2) -0.027(2) -0.011(2) C291 0.076(3) 0.053(3) 0.124(5) 0.006(3) -0.030(3) -0.022(2) C292 0.124(5) 0.053(3) 0.188(7) -0.004(4) 0.083(5) 0.017(3) C41 0.089(5) 0.334(13) 0.115(6) 0.135(7) -0.023(4) -0.040(7) Cl1 0.1039(11) 0.1003(11) 0.0917(11) 0.0091(9) 0.0153(9) 0.0162(9) Cl2 0.1288(16) 0.1059(13) 0.168(2) -0.0180(13) 0.0017(14) -0.0138(12) _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 C31 1.981(3) . ? Au1 C1 2.010(3) . ? C1 N2 1.354(4) . ? C1 N5 1.356(3) . ? N2 C3 1.386(4) . ? N2 C11 1.444(3) . ? C3 C4 1.346(4) . ? C3 H3 0.9500 . ? C4 N5 1.379(4) . ? C4 H4 0.9500 . ? N5 C21 1.450(3) . ? C11 C16 1.395(4) . ? C11 C12 1.397(4) . ? C12 C13 1.403(4) . ? C12 C17 1.507(4) . ? C13 C14 1.378(5) . ? C13 H13 0.9500 . ? C14 C15 1.377(5) . ? C14 H14 0.9500 . ? C15 C16 1.391(4) . ? C15 H15 0.9500 . ? C16 C19 1.518(5) . ? C17 C172 1.524(5) . ? C17 C171 1.527(5) . ? C17 H17 1.0000 . ? C19 C191 1.503(6) . ? C19 C192 1.510(5) . ? C19 H19 1.0000 . ? C21 C22 1.393(4) . ? C21 C26 1.394(4) . ? C22 C23 1.389(4) . ? C22 C27 1.517(4) . ? C23 C24 1.381(5) . ? C23 H23 0.9500 . ? C24 C25 1.379(5) . ? C24 H24 0.9500 . ? C25 C26 1.395(4) . ? C25 H25 0.9500 . ? C26 C29 1.512(4) . ? C27 C272 1.522(5) . ? C27 C271 1.528(6) . ? C27 H27 1.0000 . ? C29 C292 1.508(6) . ? C29 C291 1.510(5) . ? C29 H29 1.0000 . ? C31 C32 1.197(4) . ? C32 C33 1.439(4) . ? C33 O33 1.199(4) . ? C33 O34 1.325(4) . ? O34 C34 1.446(4) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C171 H17A 0.9800 . ? C171 H17B 0.9800 . ? C171 H17C 0.9800 . ? C172 H17D 0.9800 . ? C172 H17E 0.9800 . ? C172 H17F 0.9800 . ? C191 H19A 0.9800 . ? C191 H19B 0.9800 . ? C191 H19C 0.9800 . ? C192 H19D 0.9800 . ? C192 H19E 0.9800 . ? C192 H19F 0.9800 . ? C271 H27A 0.9800 . ? C271 H27B 0.9800 . ? C271 H27C 0.9800 . ? C272 H27D 0.9800 . ? C272 H27E 0.9800 . ? C272 H27F 0.9800 . ? C291 H29A 0.9800 . ? C291 H29B 0.9800 . ? C291 H29C 0.9800 . ? C292 H29D 0.9800 . ? C292 H29E 0.9800 . ? C292 H29F 0.9800 . ? C41 Cl2 1.693(8) . ? C41 Cl1 1.702(7) . ? C41 H41A 0.9900 . ? C41 H41B 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 C31 Au1 C1 178.06(12) . . ? N2 C1 N5 104.4(2) . . ? N2 C1 Au1 127.1(2) . . ? N5 C1 Au1 128.3(2) . . ? C1 N2 C3 110.9(2) . . ? C1 N2 C11 124.4(2) . . ? C3 N2 C11 124.6(2) . . ? C4 C3 N2 106.8(3) . . ? C4 C3 H3 126.6 . . ? N2 C3 H3 126.6 . . ? C3 C4 N5 106.6(3) . . ? C3 C4 H4 126.7 . . ? N5 C4 H4 126.7 . . ? C1 N5 C4 111.3(2) . . ? C1 N5 C21 123.6(2) . . ? C4 N5 C21 124.7(2) . . ? C16 C11 C12 123.8(3) . . ? C16 C11 N2 118.5(3) . . ? C12 C11 N2 117.7(3) . . ? C11 C12 C13 116.5(3) . . ? C11 C12 C17 123.5(3) . . ? C13 C12 C17 120.0(3) . . ? C14 C13 C12 121.0(3) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C15 C14 C13 120.5(3) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 121.4(3) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C15 C16 C11 116.8(3) . . ? C15 C16 C19 120.1(3) . . ? C11 C16 C19 123.1(3) . . ? C12 C17 C172 111.5(3) . . ? C12 C17 C171 110.8(3) . . ? C172 C17 C171 109.9(4) . . ? C12 C17 H17 108.2 . . ? C172 C17 H17 108.2 . . ? C171 C17 H17 108.2 . . ? C191 C19 C192 109.9(4) . . ? C191 C19 C16 111.2(3) . . ? C192 C19 C16 112.6(3) . . ? C191 C19 H19 107.6 . . ? C192 C19 H19 107.6 . . ? C16 C19 H19 107.6 . . ? C22 C21 C26 123.6(3) . . ? C22 C21 N5 117.4(3) . . ? C26 C21 N5 119.0(3) . . ? C23 C22 C21 117.4(3) . . ? C23 C22 C27 120.1(3) . . ? C21 C22 C27 122.5(3) . . ? C24 C23 C22 120.7(3) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C25 C24 C23 120.4(3) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 121.4(3) . . ? C24 C25 H25 119.3 . . ? C26 C25 H25 119.3 . . ? C21 C26 C25 116.5(3) . . ? C21 C26 C29 122.5(3) . . ? C25 C26 C29 121.1(3) . . ? C22 C27 C272 111.1(3) . . ? C22 C27 C271 110.4(3) . . ? C272 C27 C271 111.8(4) . . ? C22 C27 H27 107.8 . . ? C272 C27 H27 107.8 . . ? C271 C27 H27 107.8 . . ? C292 C29 C291 109.4(4) . . ? C292 C29 C26 112.6(3) . . ? C291 C29 C26 110.4(3) . . ? C292 C29 H29 108.1 . . ? C291 C29 H29 108.1 . . ? C26 C29 H29 108.1 . . ? C32 C31 Au1 177.7(3) . . ? C31 C32 C33 176.6(4) . . ? O33 C33 O34 123.0(3) . . ? O33 C33 C32 124.3(3) . . ? O34 C33 C32 112.7(3) . . ? C33 O34 C34 116.4(3) . . ? O34 C34 H34A 109.5 . . ? O34 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O34 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C17 C171 H17A 109.5 . . ? C17 C171 H17B 109.5 . . ? H17A C171 H17B 109.5 . . ? C17 C171 H17C 109.5 . . ? H17A C171 H17C 109.5 . . ? H17B C171 H17C 109.5 . . ? C17 C172 H17D 109.5 . . ? C17 C172 H17E 109.5 . . ? H17D C172 H17E 109.5 . . ? C17 C172 H17F 109.5 . . ? H17D C172 H17F 109.5 . . ? H17E C172 H17F 109.5 . . ? C19 C191 H19A 109.5 . . ? C19 C191 H19B 109.5 . . ? H19A C191 H19B 109.5 . . ? C19 C191 H19C 109.5 . . ? H19A C191 H19C 109.5 . . ? H19B C191 H19C 109.5 . . ? C19 C192 H19D 109.5 . . ? C19 C192 H19E 109.5 . . ? H19D C192 H19E 109.5 . . ? C19 C192 H19F 109.5 . . ? H19D C192 H19F 109.5 . . ? H19E C192 H19F 109.5 . . ? C27 C271 H27A 109.5 . . ? C27 C271 H27B 109.5 . . ? H27A C271 H27B 109.5 . . ? C27 C271 H27C 109.5 . . ? H27A C271 H27C 109.5 . . ? H27B C271 H27C 109.5 . . ? C27 C272 H27D 109.5 . . ? C27 C272 H27E 109.5 . . ? H27D C272 H27E 109.5 . . ? C27 C272 H27F 109.5 . . ? H27D C272 H27F 109.5 . . ? H27E C272 H27F 109.5 . . ? C29 C291 H29A 109.5 . . ? C29 C291 H29B 109.5 . . ? H29A C291 H29B 109.5 . . ? C29 C291 H29C 109.5 . . ? H29A C291 H29C 109.5 . . ? H29B C291 H29C 109.5 . . ? C29 C292 H29D 109.5 . . ? C29 C292 H29E 109.5 . . ? H29D C292 H29E 109.5 . . ? C29 C292 H29F 109.5 . . ? H29D C292 H29F 109.5 . . ? H29E C292 H29F 109.5 . . ? Cl2 C41 Cl1 117.1(4) . . ? Cl2 C41 H41A 108.0 . . ? Cl1 C41 H41A 108.0 . . ? Cl2 C41 H41B 108.0 . . ? Cl1 C41 H41B 108.0 . . ? H41A C41 H41B 107.3 . . ? 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 C31 Au1 C1 N2 97(3) . . . . ? C31 Au1 C1 N5 -77(3) . . . . ? N5 C1 N2 C3 0.2(3) . . . . ? Au1 C1 N2 C3 -174.9(2) . . . . ? N5 C1 N2 C11 177.6(3) . . . . ? Au1 C1 N2 C11 2.6(4) . . . . ? C1 N2 C3 C4 -0.2(4) . . . . ? C11 N2 C3 C4 -177.7(3) . . . . ? N2 C3 C4 N5 0.1(4) . . . . ? N2 C1 N5 C4 -0.1(3) . . . . ? Au1 C1 N5 C4 174.9(2) . . . . ? N2 C1 N5 C21 -172.9(3) . . . . ? Au1 C1 N5 C21 2.1(4) . . . . ? C3 C4 N5 C1 0.0(4) . . . . ? C3 C4 N5 C21 172.7(3) . . . . ? C1 N2 C11 C16 -76.9(4) . . . . ? C3 N2 C11 C16 100.3(4) . . . . ? C1 N2 C11 C12 104.1(3) . . . . ? C3 N2 C11 C12 -78.8(4) . . . . ? C16 C11 C12 C13 -0.4(5) . . . . ? N2 C11 C12 C13 178.6(3) . . . . ? C16 C11 C12 C17 179.0(3) . . . . ? N2 C11 C12 C17 -2.1(4) . . . . ? C11 C12 C13 C14 0.4(5) . . . . ? C17 C12 C13 C14 -179.0(3) . . . . ? C12 C13 C14 C15 -0.5(6) . . . . ? C13 C14 C15 C16 0.5(6) . . . . ? C14 C15 C16 C11 -0.5(5) . . . . ? C14 C15 C16 C19 179.8(3) . . . . ? C12 C11 C16 C15 0.5(5) . . . . ? N2 C11 C16 C15 -178.5(3) . . . . ? C12 C11 C16 C19 -179.8(3) . . . . ? N2 C11 C16 C19 1.2(4) . . . . ? C11 C12 C17 C172 -120.1(4) . . . . ? C13 C12 C17 C172 59.2(4) . . . . ? C11 C12 C17 C171 117.1(4) . . . . ? C13 C12 C17 C171 -63.6(4) . . . . ? C15 C16 C19 C191 71.4(5) . . . . ? C11 C16 C19 C191 -108.3(4) . . . . ? C15 C16 C19 C192 -52.5(5) . . . . ? C11 C16 C19 C192 127.9(4) . . . . ? C1 N5 C21 C22 83.3(4) . . . . ? C4 N5 C21 C22 -88.6(4) . . . . ? C1 N5 C21 C26 -96.7(3) . . . . ? C4 N5 C21 C26 91.4(4) . . . . ? C26 C21 C22 C23 2.0(5) . . . . ? N5 C21 C22 C23 -178.0(3) . . . . ? C26 C21 C22 C27 -178.1(3) . . . . ? N5 C21 C22 C27 1.8(4) . . . . ? C21 C22 C23 C24 -0.9(5) . . . . ? C27 C22 C23 C24 179.3(3) . . . . ? C22 C23 C24 C25 -0.5(5) . . . . ? C23 C24 C25 C26 0.9(5) . . . . ? C22 C21 C26 C25 -1.7(4) . . . . ? N5 C21 C26 C25 178.4(3) . . . . ? C22 C21 C26 C29 178.2(3) . . . . ? N5 C21 C26 C29 -1.8(4) . . . . ? C24 C25 C26 C21 0.1(5) . . . . ? C24 C25 C26 C29 -179.7(3) . . . . ? C23 C22 C27 C272 63.3(4) . . . . ? C21 C22 C27 C272 -116.5(4) . . . . ? C23 C22 C27 C271 -61.3(5) . . . . ? C21 C22 C27 C271 118.9(4) . . . . ? C21 C26 C29 C292 131.3(4) . . . . ? C25 C26 C29 C292 -48.8(5) . . . . ? C21 C26 C29 C291 -106.2(4) . . . . ? C25 C26 C29 C291 73.6(4) . . . . ? C1 Au1 C31 C32 85(9) . . . . ? Au1 C31 C32 C33 98(9) . . . . ? C31 C32 C33 O33 66(6) . . . . ? C31 C32 C33 O34 -114(6) . . . . ? O33 C33 O34 C34 -1.2(6) . . . . ? C32 C33 O34 C34 179.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.69 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.077 _refine_diff_density_min -1.036 _refine_diff_density_rms 0.092 data_mah12 _database_code_depnum_ccdc_archive 'CCDC 915440' #TrackingRef 'allenylideneChemSci2012.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '4 in manuscript' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H46 Au Cl2 N3 O' _chemical_formula_weight 792.61 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.2357(3) _cell_length_b 12.3159(3) _cell_length_c 28.5345(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.224(2) _cell_angle_gamma 90.00 _cell_volume 3575.91(16) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 9900 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.37 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 4.293 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2137 _exptl_absorpt_correction_T_max 0.7827 _exptl_absorpt_process_details ; Sheldrick, G. M. (2008). SADABS. University of G\"ottingen, Germany. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 41179 _diffrn_reflns_av_R_equivalents 0.0631 _diffrn_reflns_av_sigmaI/netI 0.0480 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 27.56 _reflns_number_total 8216 _reflns_number_gt 6846 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+7.0703P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8216 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0797 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 0.539596(16) 0.109080(11) 0.854492(5) 0.02556(6) Uani 1 1 d . . . C1 C 0.5397(4) -0.0475(3) 0.83405(12) 0.0220(8) Uani 1 1 d . . . N2 N 0.5504(3) -0.0884(2) 0.79090(10) 0.0236(7) Uani 1 1 d . . . C3 C 0.5417(4) -0.2010(3) 0.79132(14) 0.0308(9) Uani 1 1 d . . . H3 H 0.5467 -0.2481 0.7652 0.037 Uiso 1 1 calc R . . C4 C 0.5250(4) -0.2305(3) 0.83551(14) 0.0319(9) Uani 1 1 d . . . H4 H 0.5154 -0.3024 0.8468 0.038 Uiso 1 1 calc R . . N5 N 0.5245(3) -0.1356(2) 0.86151(10) 0.0233(7) Uani 1 1 d . . . C11 C 0.5740(4) -0.0262(3) 0.74959(13) 0.0255(8) Uani 1 1 d . . . C12 C 0.7014(4) -0.0232(3) 0.73703(13) 0.0292(9) Uani 1 1 d . . . C13 C 0.7214(5) 0.0307(4) 0.69562(15) 0.0425(11) Uani 1 1 d . . . H13 H 0.8066 0.0323 0.6853 0.051 Uiso 1 1 calc R . . C14 C 0.6185(6) 0.0817(4) 0.66941(17) 0.0545(14) Uani 1 1 d . . . H14 H 0.6335 0.1195 0.6415 0.065 Uiso 1 1 calc R . . C15 C 0.4949(5) 0.0784(4) 0.68319(17) 0.0469(12) Uani 1 1 d . . . H15 H 0.4253 0.1141 0.6645 0.056 Uiso 1 1 calc R . . C16 C 0.4680(4) 0.0244(3) 0.72385(14) 0.0334(9) Uani 1 1 d . . . C17 C 0.8161(5) -0.0771(4) 0.76620(16) 0.0382(10) Uani 1 1 d . . . H17 H 0.7839 -0.1057 0.7957 0.046 Uiso 1 1 calc R . . C19 C 0.3285(5) 0.0195(4) 0.73742(18) 0.0452(12) Uani 1 1 d . . . H19 H 0.3306 -0.0243 0.7670 0.054 Uiso 1 1 calc R . . C21 C 0.5052(4) -0.1321(3) 0.91084(13) 0.0242(8) Uani 1 1 d . . . C22 C 0.3790(4) -0.1136(3) 0.92335(14) 0.0283(8) Uani 1 1 d . . . C23 C 0.3627(5) -0.1190(3) 0.97126(14) 0.0325(9) Uani 1 1 d . . . H23 H 0.2776 -0.1093 0.9810 0.039 Uiso 1 1 calc R . . C24 C 0.4676(5) -0.1381(3) 1.00466(14) 0.0331(10) Uani 1 1 d . . . H24 H 0.4544 -0.1414 1.0371 0.040 Uiso 1 1 calc R . . C25 C 0.5919(5) -0.1526(3) 0.99116(14) 0.0319(9) Uani 1 1 d . . . H25 H 0.6637 -0.1648 1.0146 0.038 Uiso 1 1 calc R . . C26 C 0.6144(4) -0.1496(3) 0.94370(13) 0.0271(8) Uani 1 1 d . . . C27 C 0.2619(5) -0.0893(4) 0.88706(16) 0.0375(10) Uani 1 1 d . . . H27 H 0.2932 -0.0900 0.8551 0.045 Uiso 1 1 calc R . . C29 C 0.7526(4) -0.1622(4) 0.92931(15) 0.0367(10) Uani 1 1 d . . . H29 H 0.7451 -0.1680 0.8942 0.044 Uiso 1 1 calc R . . C31 C 0.5295(4) 0.2634(3) 0.87518(14) 0.0322(9) Uani 1 1 d . . . C32 C 0.5198(4) 0.3550(3) 0.88778(15) 0.0328(9) Uani 1 1 d . . . C33 C 0.5071(4) 0.4671(3) 0.90195(14) 0.0322(9) Uani 1 1 d . . . O33 O 0.5813(4) 0.5385(2) 0.89094(13) 0.0558(10) Uani 1 1 d . . . N34 N 0.4100(4) 0.4875(3) 0.92850(12) 0.0337(8) Uani 1 1 d . . . C35 C 0.3876(6) 0.5967(4) 0.9459(2) 0.0555(15) Uani 1 1 d . . . H35A H 0.3642 0.6477 0.9196 0.067 Uiso 1 1 calc R . . H35B H 0.4665 0.6242 0.9655 0.067 Uiso 1 1 calc R . . C36 C 0.2750(7) 0.5818(5) 0.9750(2) 0.0730(19) Uani 1 1 d . . . H36A H 0.3075 0.5680 1.0084 0.088 Uiso 1 1 calc R . . H36B H 0.2181 0.6470 0.9732 0.088 Uiso 1 1 calc R . . C37 C 0.2031(7) 0.4876(5) 0.9542(3) 0.078(2) Uani 1 1 d . . . H37A H 0.1429 0.5090 0.9262 0.094 Uiso 1 1 calc R . . H37B H 0.1514 0.4525 0.9774 0.094 Uiso 1 1 calc R . . C38 C 0.3097(5) 0.4121(4) 0.9405(2) 0.0481(13) Uani 1 1 d . . . H38A H 0.3432 0.3646 0.9671 0.058 Uiso 1 1 calc R . . H38B H 0.2772 0.3665 0.9131 0.058 Uiso 1 1 calc R . . C171 C 0.8701(6) -0.1727(5) 0.7400(2) 0.0684(17) Uani 1 1 d . . . H17A H 0.9441 -0.2054 0.7598 0.103 Uiso 1 1 calc R . . H17B H 0.9001 -0.1469 0.7105 0.103 Uiso 1 1 calc R . . H17C H 0.8008 -0.2270 0.7330 0.103 Uiso 1 1 calc R . . C172 C 0.9231(7) 0.0056(6) 0.7802(3) 0.092(2) Uani 1 1 d . . . H17D H 0.9968 -0.0301 0.7989 0.138 Uiso 1 1 calc R . . H17E H 0.8880 0.0632 0.7989 0.138 Uiso 1 1 calc R . . H17F H 0.9536 0.0371 0.7518 0.138 Uiso 1 1 calc R . . C191 C 0.2364(6) -0.0372(7) 0.6999(3) 0.090(2) Uani 1 1 d . . . H19A H 0.1476 -0.0390 0.7097 0.135 Uiso 1 1 calc R . . H19B H 0.2671 -0.1115 0.6957 0.135 Uiso 1 1 calc R . . H19C H 0.2349 0.0024 0.6701 0.135 Uiso 1 1 calc R . . C192 C 0.2784(6) 0.1326(5) 0.7480(3) 0.077(2) Uani 1 1 d . . . H19D H 0.1885 0.1273 0.7567 0.115 Uiso 1 1 calc R . . H19E H 0.2790 0.1786 0.7200 0.115 Uiso 1 1 calc R . . H19F H 0.3354 0.1647 0.7742 0.115 Uiso 1 1 calc R . . C271 C 0.1552(5) -0.1762(5) 0.8882(2) 0.0625(16) Uani 1 1 d . . . H27A H 0.0811 -0.1588 0.8647 0.094 Uiso 1 1 calc R . . H27B H 0.1248 -0.1781 0.9196 0.094 Uiso 1 1 calc R . . H27C H 0.1913 -0.2472 0.8810 0.094 Uiso 1 1 calc R . . C272 C 0.2059(5) 0.0230(4) 0.89538(19) 0.0535(14) Uani 1 1 d . . . H27D H 0.1307 0.0370 0.8719 0.080 Uiso 1 1 calc R . . H27E H 0.2737 0.0781 0.8926 0.080 Uiso 1 1 calc R . . H27F H 0.1772 0.0260 0.9270 0.080 Uiso 1 1 calc R . . C291 C 0.8198(5) -0.2643(4) 0.94957(18) 0.0484(12) Uani 1 1 d . . . H29A H 0.9083 -0.2690 0.9396 0.073 Uiso 1 1 calc R . . H29B H 0.7686 -0.3281 0.9381 0.073 Uiso 1 1 calc R . . H29C H 0.8259 -0.2618 0.9841 0.073 Uiso 1 1 calc R . . C292 C 0.8337(6) -0.0609(5) 0.9436(3) 0.074(2) Uani 1 1 d . . . H29D H 0.9226 -0.0695 0.9343 0.112 Uiso 1 1 calc R . . H29E H 0.8386 -0.0510 0.9778 0.112 Uiso 1 1 calc R . . H29F H 0.7920 0.0028 0.9277 0.112 Uiso 1 1 calc R . . C41 C 0.8721(7) 0.2927(8) 0.8858(3) 0.102(3) Uani 1 1 d . . . H41A H 0.7945 0.2516 0.8717 0.123 Uiso 1 1 calc R . . H41B H 0.8471 0.3702 0.8870 0.123 Uiso 1 1 calc R . . Cl1 Cl 0.9171(3) 0.2461(2) 0.94300(7) 0.1174(8) Uani 1 1 d . . . Cl2 Cl 0.9968(2) 0.27869(18) 0.85081(6) 0.0916(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.03843(10) 0.01514(8) 0.02411(8) -0.00115(6) 0.00791(6) 0.00039(7) C1 0.026(2) 0.0209(18) 0.0206(17) 0.0000(15) 0.0077(14) -0.0011(15) N2 0.0359(19) 0.0156(15) 0.0197(15) -0.0028(12) 0.0053(13) -0.0007(13) C3 0.050(3) 0.0169(19) 0.027(2) -0.0033(16) 0.0107(18) -0.0008(18) C4 0.055(3) 0.0168(19) 0.0252(19) -0.0058(16) 0.0107(18) -0.0027(18) N5 0.038(2) 0.0120(14) 0.0217(15) -0.0012(11) 0.0096(14) 0.0003(13) C11 0.037(2) 0.0197(18) 0.0200(17) 0.0012(15) 0.0055(16) -0.0012(17) C12 0.037(2) 0.029(2) 0.0230(19) 0.0000(16) 0.0073(16) -0.0021(18) C13 0.049(3) 0.046(3) 0.034(2) 0.005(2) 0.015(2) -0.009(2) C14 0.085(4) 0.048(3) 0.031(2) 0.018(2) 0.012(3) -0.009(3) C15 0.057(3) 0.044(3) 0.038(3) 0.016(2) -0.003(2) 0.006(2) C16 0.037(2) 0.032(2) 0.031(2) 0.0035(18) 0.0007(18) 0.0024(19) C17 0.036(3) 0.042(3) 0.037(2) 0.000(2) 0.0067(19) 0.004(2) C19 0.035(3) 0.047(3) 0.052(3) 0.000(2) -0.001(2) 0.005(2) C21 0.041(2) 0.0129(17) 0.0199(17) -0.0023(14) 0.0096(16) -0.0038(15) C22 0.038(2) 0.0196(18) 0.029(2) -0.0019(16) 0.0082(17) 0.0001(17) C23 0.042(3) 0.026(2) 0.032(2) -0.0033(17) 0.0175(19) -0.0008(19) C24 0.051(3) 0.027(2) 0.0231(19) 0.0000(16) 0.0125(19) -0.0034(19) C25 0.050(3) 0.023(2) 0.0228(19) 0.0022(16) 0.0017(18) -0.0007(19) C26 0.034(2) 0.0195(18) 0.029(2) -0.0001(16) 0.0072(17) -0.0009(16) C27 0.039(3) 0.039(3) 0.036(2) -0.0043(19) 0.0056(19) 0.000(2) C29 0.040(3) 0.037(2) 0.034(2) -0.0004(19) 0.0060(19) 0.005(2) C31 0.046(3) 0.029(2) 0.0232(19) -0.0033(17) 0.0096(18) 0.0035(19) C32 0.043(3) 0.021(2) 0.035(2) -0.0010(17) 0.0083(19) 0.0000(18) C33 0.045(3) 0.0180(19) 0.035(2) -0.0014(17) 0.0073(19) -0.0004(18) O33 0.074(3) 0.0215(16) 0.079(3) -0.0067(16) 0.041(2) -0.0123(16) N34 0.047(2) 0.0159(16) 0.040(2) -0.0046(14) 0.0149(17) -0.0024(15) C35 0.072(4) 0.024(2) 0.074(4) -0.015(2) 0.028(3) -0.001(2) C36 0.097(5) 0.051(4) 0.078(4) -0.010(3) 0.045(4) 0.008(3) C37 0.072(4) 0.061(4) 0.109(5) 0.008(4) 0.047(4) 0.006(3) C38 0.054(3) 0.028(2) 0.066(3) 0.005(2) 0.022(3) 0.000(2) C171 0.078(4) 0.064(4) 0.066(4) 0.002(3) 0.019(3) 0.032(3) C172 0.062(4) 0.089(5) 0.114(6) -0.004(5) -0.033(4) -0.008(4) C191 0.051(4) 0.121(7) 0.097(5) -0.039(5) 0.001(4) -0.017(4) C192 0.056(4) 0.079(5) 0.097(5) -0.007(4) 0.013(4) 0.023(3) C271 0.050(3) 0.048(3) 0.085(4) -0.009(3) -0.014(3) -0.005(3) C272 0.054(3) 0.039(3) 0.064(3) -0.002(2) -0.010(3) 0.006(2) C291 0.044(3) 0.045(3) 0.057(3) 0.001(2) 0.008(2) 0.008(2) C292 0.056(4) 0.038(3) 0.134(6) -0.008(4) 0.035(4) -0.007(3) C41 0.055(4) 0.148(8) 0.103(6) 0.036(6) 0.006(4) 0.008(5) Cl1 0.140(2) 0.143(2) 0.0713(12) 0.0061(13) 0.0207(12) -0.0013(17) Cl2 0.1010(14) 0.0971(15) 0.0778(12) 0.0155(10) 0.0152(10) 0.0034(12) _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 C31 1.996(4) . ? Au1 C1 2.014(4) . ? C1 N2 1.346(4) . ? C1 N5 1.358(5) . ? N2 C3 1.389(5) . ? N2 C11 1.448(5) . ? C3 C4 1.341(5) . ? C3 H3 0.9500 . ? C4 N5 1.384(5) . ? C4 H4 0.9500 . ? N5 C21 1.443(4) . ? C11 C16 1.390(6) . ? C11 C12 1.390(6) . ? C12 C13 1.389(6) . ? C12 C17 1.517(6) . ? C13 C14 1.376(7) . ? C13 H13 0.9500 . ? C14 C15 1.365(8) . ? C14 H14 0.9500 . ? C15 C16 1.391(6) . ? C15 H15 0.9500 . ? C16 C19 1.520(6) . ? C17 C172 1.516(8) . ? C17 C171 1.530(7) . ? C17 H17 1.0000 . ? C19 C191 1.518(7) . ? C19 C192 1.527(7) . ? C19 H19 1.0000 . ? C21 C22 1.396(6) . ? C21 C26 1.396(6) . ? C22 C23 1.397(5) . ? C22 C27 1.526(6) . ? C23 C24 1.376(6) . ? C23 H23 0.9500 . ? C24 C25 1.380(6) . ? C24 H24 0.9500 . ? C25 C26 1.399(5) . ? C25 H25 0.9500 . ? C26 C29 1.523(6) . ? C27 C272 1.525(6) . ? C27 C271 1.533(7) . ? C27 H27 1.0000 . ? C29 C291 1.518(6) . ? C29 C292 1.529(7) . ? C29 H29 1.0000 . ? C31 C32 1.191(6) . ? C32 C33 1.449(5) . ? C33 O33 1.225(5) . ? C33 N34 1.337(5) . ? N34 C38 1.452(6) . ? N34 C35 1.460(5) . ? C35 C36 1.502(8) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.464(9) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.517(7) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C171 H17A 0.9800 . ? C171 H17B 0.9800 . ? C171 H17C 0.9800 . ? C172 H17D 0.9800 . ? C172 H17E 0.9800 . ? C172 H17F 0.9800 . ? C191 H19A 0.9800 . ? C191 H19B 0.9800 . ? C191 H19C 0.9800 . ? C192 H19D 0.9800 . ? C192 H19E 0.9800 . ? C192 H19F 0.9800 . ? C271 H27A 0.9800 . ? C271 H27B 0.9800 . ? C271 H27C 0.9800 . ? C272 H27D 0.9800 . ? C272 H27E 0.9800 . ? C272 H27F 0.9800 . ? C291 H29A 0.9800 . ? C291 H29B 0.9800 . ? C291 H29C 0.9800 . ? C292 H29D 0.9800 . ? C292 H29E 0.9800 . ? C292 H29F 0.9800 . ? C41 Cl2 1.712(7) . ? C41 Cl1 1.745(7) . ? C41 H41A 0.9900 . ? C41 H41B 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 C31 Au1 C1 176.99(16) . . ? N2 C1 N5 104.7(3) . . ? N2 C1 Au1 128.8(3) . . ? N5 C1 Au1 126.5(3) . . ? C1 N2 C3 110.8(3) . . ? C1 N2 C11 125.7(3) . . ? C3 N2 C11 123.5(3) . . ? C4 C3 N2 107.1(3) . . ? C4 C3 H3 126.5 . . ? N2 C3 H3 126.5 . . ? C3 C4 N5 106.4(3) . . ? C3 C4 H4 126.8 . . ? N5 C4 H4 126.8 . . ? C1 N5 C4 111.0(3) . . ? C1 N5 C21 125.1(3) . . ? C4 N5 C21 123.8(3) . . ? C16 C11 C12 123.5(4) . . ? C16 C11 N2 118.6(4) . . ? C12 C11 N2 117.9(3) . . ? C13 C12 C11 117.4(4) . . ? C13 C12 C17 120.0(4) . . ? C11 C12 C17 122.6(4) . . ? C14 C13 C12 120.4(5) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C15 C14 C13 120.6(4) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 121.9(5) . . ? C14 C15 H15 119.1 . . ? C16 C15 H15 119.1 . . ? C11 C16 C15 116.2(4) . . ? C11 C16 C19 123.3(4) . . ? C15 C16 C19 120.5(4) . . ? C172 C17 C12 110.1(4) . . ? C172 C17 C171 110.9(5) . . ? C12 C17 C171 111.6(4) . . ? C172 C17 H17 108.0 . . ? C12 C17 H17 108.0 . . ? C171 C17 H17 108.0 . . ? C191 C19 C16 111.5(4) . . ? C191 C19 C192 111.3(5) . . ? C16 C19 C192 111.1(4) . . ? C191 C19 H19 107.6 . . ? C16 C19 H19 107.6 . . ? C192 C19 H19 107.6 . . ? C22 C21 C26 123.4(3) . . ? C22 C21 N5 118.9(4) . . ? C26 C21 N5 117.8(3) . . ? C21 C22 C23 117.0(4) . . ? C21 C22 C27 122.6(4) . . ? C23 C22 C27 120.4(4) . . ? C24 C23 C22 121.3(4) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C25 120.2(4) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C24 C25 C26 121.4(4) . . ? C24 C25 H25 119.3 . . ? C26 C25 H25 119.3 . . ? C21 C26 C25 116.8(4) . . ? C21 C26 C29 122.3(3) . . ? C25 C26 C29 120.9(4) . . ? C272 C27 C22 110.7(4) . . ? C272 C27 C271 110.4(4) . . ? C22 C27 C271 111.0(4) . . ? C272 C27 H27 108.2 . . ? C22 C27 H27 108.2 . . ? C271 C27 H27 108.2 . . ? C291 C29 C26 112.1(4) . . ? C291 C29 C292 111.4(4) . . ? C26 C29 C292 109.8(4) . . ? C291 C29 H29 107.8 . . ? C26 C29 H29 107.8 . . ? C292 C29 H29 107.8 . . ? C32 C31 Au1 178.1(4) . . ? C31 C32 C33 178.6(5) . . ? O33 C33 N34 122.0(4) . . ? O33 C33 C32 122.4(4) . . ? N34 C33 C32 115.5(4) . . ? C33 N34 C38 127.0(4) . . ? C33 N34 C35 121.3(4) . . ? C38 N34 C35 111.6(4) . . ? N34 C35 C36 103.5(4) . . ? N34 C35 H35A 111.1 . . ? C36 C35 H35A 111.1 . . ? N34 C35 H35B 111.1 . . ? C36 C35 H35B 111.1 . . ? H35A C35 H35B 109.0 . . ? C37 C36 C35 104.8(5) . . ? C37 C36 H36A 110.8 . . ? C35 C36 H36A 110.8 . . ? C37 C36 H36B 110.8 . . ? C35 C36 H36B 110.8 . . ? H36A C36 H36B 108.9 . . ? C36 C37 C38 104.2(5) . . ? C36 C37 H37A 110.9 . . ? C38 C37 H37A 110.9 . . ? C36 C37 H37B 110.9 . . ? C38 C37 H37B 110.9 . . ? H37A C37 H37B 108.9 . . ? N34 C38 C37 102.5(4) . . ? N34 C38 H38A 111.3 . . ? C37 C38 H38A 111.3 . . ? N34 C38 H38B 111.3 . . ? C37 C38 H38B 111.3 . . ? H38A C38 H38B 109.2 . . ? C17 C171 H17A 109.5 . . ? C17 C171 H17B 109.5 . . ? H17A C171 H17B 109.5 . . ? C17 C171 H17C 109.5 . . ? H17A C171 H17C 109.5 . . ? H17B C171 H17C 109.5 . . ? C17 C172 H17D 109.5 . . ? C17 C172 H17E 109.5 . . ? H17D C172 H17E 109.5 . . ? C17 C172 H17F 109.5 . . ? H17D C172 H17F 109.5 . . ? H17E C172 H17F 109.5 . . ? C19 C191 H19A 109.5 . . ? C19 C191 H19B 109.5 . . ? H19A C191 H19B 109.5 . . ? C19 C191 H19C 109.5 . . ? H19A C191 H19C 109.5 . . ? H19B C191 H19C 109.5 . . ? C19 C192 H19D 109.5 . . ? C19 C192 H19E 109.5 . . ? H19D C192 H19E 109.5 . . ? C19 C192 H19F 109.5 . . ? H19D C192 H19F 109.5 . . ? H19E C192 H19F 109.5 . . ? C27 C271 H27A 109.5 . . ? C27 C271 H27B 109.5 . . ? H27A C271 H27B 109.5 . . ? C27 C271 H27C 109.5 . . ? H27A C271 H27C 109.5 . . ? H27B C271 H27C 109.5 . . ? C27 C272 H27D 109.5 . . ? C27 C272 H27E 109.5 . . ? H27D C272 H27E 109.5 . . ? C27 C272 H27F 109.5 . . ? H27D C272 H27F 109.5 . . ? H27E C272 H27F 109.5 . . ? C29 C291 H29A 109.5 . . ? C29 C291 H29B 109.5 . . ? H29A C291 H29B 109.5 . . ? C29 C291 H29C 109.5 . . ? H29A C291 H29C 109.5 . . ? H29B C291 H29C 109.5 . . ? C29 C292 H29D 109.5 . . ? C29 C292 H29E 109.5 . . ? H29D C292 H29E 109.5 . . ? C29 C292 H29F 109.5 . . ? H29D C292 H29F 109.5 . . ? H29E C292 H29F 109.5 . . ? Cl2 C41 Cl1 112.0(4) . . ? Cl2 C41 H41A 109.2 . . ? Cl1 C41 H41A 109.2 . . ? Cl2 C41 H41B 109.2 . . ? Cl1 C41 H41B 109.2 . . ? H41A C41 H41B 107.9 . . ? 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 C31 Au1 C1 N2 110(3) . . . . ? C31 Au1 C1 N5 -68(3) . . . . ? N5 C1 N2 C3 0.1(4) . . . . ? Au1 C1 N2 C3 -178.0(3) . . . . ? N5 C1 N2 C11 -177.2(4) . . . . ? Au1 C1 N2 C11 4.7(6) . . . . ? C1 N2 C3 C4 0.1(5) . . . . ? C11 N2 C3 C4 177.5(4) . . . . ? N2 C3 C4 N5 -0.4(5) . . . . ? N2 C1 N5 C4 -0.4(4) . . . . ? Au1 C1 N5 C4 177.9(3) . . . . ? N2 C1 N5 C21 -178.1(3) . . . . ? Au1 C1 N5 C21 0.1(6) . . . . ? C3 C4 N5 C1 0.5(5) . . . . ? C3 C4 N5 C21 178.2(4) . . . . ? C1 N2 C11 C16 -81.9(5) . . . . ? C3 N2 C11 C16 101.1(5) . . . . ? C1 N2 C11 C12 100.0(5) . . . . ? C3 N2 C11 C12 -76.9(5) . . . . ? C16 C11 C12 C13 -2.1(6) . . . . ? N2 C11 C12 C13 175.8(4) . . . . ? C16 C11 C12 C17 178.8(4) . . . . ? N2 C11 C12 C17 -3.3(6) . . . . ? C11 C12 C13 C14 2.2(7) . . . . ? C17 C12 C13 C14 -178.7(4) . . . . ? C12 C13 C14 C15 -1.2(8) . . . . ? C13 C14 C15 C16 0.2(8) . . . . ? C12 C11 C16 C15 1.1(6) . . . . ? N2 C11 C16 C15 -176.8(4) . . . . ? C12 C11 C16 C19 179.2(4) . . . . ? N2 C11 C16 C19 1.3(6) . . . . ? C14 C15 C16 C11 -0.1(7) . . . . ? C14 C15 C16 C19 -178.2(5) . . . . ? C13 C12 C17 C172 57.5(6) . . . . ? C11 C12 C17 C172 -123.4(5) . . . . ? C13 C12 C17 C171 -66.1(6) . . . . ? C11 C12 C17 C171 113.0(5) . . . . ? C11 C16 C19 C191 -117.2(6) . . . . ? C15 C16 C19 C191 60.8(7) . . . . ? C11 C16 C19 C192 118.0(5) . . . . ? C15 C16 C19 C192 -64.0(6) . . . . ? C1 N5 C21 C22 82.4(5) . . . . ? C4 N5 C21 C22 -95.0(5) . . . . ? C1 N5 C21 C26 -98.7(4) . . . . ? C4 N5 C21 C26 83.8(5) . . . . ? C26 C21 C22 C23 -3.5(6) . . . . ? N5 C21 C22 C23 175.3(3) . . . . ? C26 C21 C22 C27 177.0(4) . . . . ? N5 C21 C22 C27 -4.1(5) . . . . ? C21 C22 C23 C24 2.2(6) . . . . ? C27 C22 C23 C24 -178.4(4) . . . . ? C22 C23 C24 C25 -0.1(6) . . . . ? C23 C24 C25 C26 -0.8(6) . . . . ? C22 C21 C26 C25 2.7(6) . . . . ? N5 C21 C26 C25 -176.2(3) . . . . ? C22 C21 C26 C29 -175.8(4) . . . . ? N5 C21 C26 C29 5.4(5) . . . . ? C24 C25 C26 C21 -0.4(6) . . . . ? C24 C25 C26 C29 178.1(4) . . . . ? C21 C22 C27 C272 -118.2(5) . . . . ? C23 C22 C27 C272 62.4(5) . . . . ? C21 C22 C27 C271 118.8(5) . . . . ? C23 C22 C27 C271 -60.6(5) . . . . ? C21 C26 C29 C291 -127.7(4) . . . . ? C25 C26 C29 C291 53.9(5) . . . . ? C21 C26 C29 C292 107.8(5) . . . . ? C25 C26 C29 C292 -70.5(5) . . . . ? C1 Au1 C31 C32 5(14) . . . . ? Au1 C31 C32 C33 -95(23) . . . . ? C31 C32 C33 O33 -66(21) . . . . ? C31 C32 C33 N34 115(21) . . . . ? O33 C33 N34 C38 174.4(5) . . . . ? C32 C33 N34 C38 -6.5(7) . . . . ? O33 C33 N34 C35 -0.2(7) . . . . ? C32 C33 N34 C35 178.9(4) . . . . ? C33 N34 C35 C36 -177.9(5) . . . . ? C38 N34 C35 C36 6.7(6) . . . . ? N34 C35 C36 C37 -27.1(7) . . . . ? C35 C36 C37 C38 37.1(7) . . . . ? C33 N34 C38 C37 -159.6(5) . . . . ? C35 N34 C38 C37 15.4(6) . . . . ? C36 C37 C38 N34 -32.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.102 _refine_diff_density_min -1.556 _refine_diff_density_rms 0.109 data_mah6 _database_code_depnum_ccdc_archive 'CCDC 915441' #TrackingRef 'allenylideneChemSci2012.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '5 in manuscript' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36.25 H47.50 Au Cl F3 N3 O4 S' _chemical_formula_weight 910.75 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+1/4' 'y, -x, z+3/4' _cell_length_a 27.6000(18) _cell_length_b 27.6000(18) _cell_length_c 21.2131(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 16159.3(18) _cell_formula_units_Z 16 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9824 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 23.12 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.71 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7312 _exptl_absorpt_coefficient_mu 3.812 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1738 _exptl_absorpt_correction_T_max 0.8412 _exptl_absorpt_process_details ; Sheldrick, G. M. (2008). SADABS. University of G\"ottingen, Germany. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'ImuS microsource' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Bruker APEX-II Quazar' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 175832 _diffrn_reflns_av_R_equivalents 0.0586 _diffrn_reflns_av_sigmaI/netI 0.0575 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 25.37 _reflns_number_total 29623 _reflns_number_gt 21579 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. PLAT241_ALERT_2_A Check High Ueq as Compared to Neighbors for C36_1 PLAT241_ALERT_2_A Check High Ueq as Compared to Neighbors for C37_2 PLAT241_ALERT_2_A Check High Ueq as Compared to Neighbors for C36_3 PLAT241_ALERT_2_A Check High Ueq as Compared to Neighbors for C36_4 PLAT241_ALERT_2_A Check High Ueq as Compared to Neighbors for C37_4 These level-A-alerts all refer to the same group of atoms in the four independent molecules. We ascribe this to a unresolved conformational disorder of the atoms C36 and C37 in the 5-ring. All ellipsoids in question are elongated perpendicular to the 5-ring. Unfortunately the data is too bad for resolution of this disorder. Particularly it is clear from a chemical point of view, that this is not due to a wrong atom type assignment. ; _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^)+(0.0621P)^2^+57.8899P] 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 0.098(8) _refine_ls_number_reflns 29623 _refine_ls_number_parameters 1775 _refine_ls_number_restraints 4745 _refine_ls_R_factor_all 0.0874 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1458 _refine_ls_wR_factor_gt 0.1305 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.033 _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_1 Au -0.029348(15) 0.113150(13) 0.352388(16) 0.04887(11) Uani 1 1 d DU . . C1_1 C -0.0389(3) 0.1853(2) 0.3579(4) 0.047(2) Uani 1 1 d DU . . N2_1 N -0.0231(3) 0.2143(2) 0.4045(4) 0.0533(19) Uani 1 1 d DU . . C3_1 C -0.0421(4) 0.2607(3) 0.3972(6) 0.082(4) Uani 1 1 d DU . . H3_1 H -0.0357 0.2879 0.4233 0.098 Uiso 1 1 calc R . . C4_1 C -0.0706(4) 0.2598(3) 0.3471(5) 0.077(3) Uani 1 1 d DU . . H4_1 H -0.0893 0.2861 0.3314 0.092 Uiso 1 1 calc R . . N5_1 N -0.0683(3) 0.2138(3) 0.3220(4) 0.060(2) Uani 1 1 d DU . . C11_1 C 0.0114(3) 0.1997(3) 0.4521(4) 0.058(2) Uani 1 1 d DU . . C12_1 C 0.0600(3) 0.2099(4) 0.4430(4) 0.073(3) Uani 1 1 d DU . . C13_1 C 0.0926(4) 0.1957(5) 0.4895(5) 0.104(4) Uani 1 1 d DU . . H13_1 H 0.1264 0.2008 0.4841 0.125 Uiso 1 1 calc R . . C14_1 C 0.0750(4) 0.1741(5) 0.5433(6) 0.106(4) Uani 1 1 d DU . . H14_1 H 0.0969 0.1651 0.5758 0.127 Uiso 1 1 calc R . . C15_1 C 0.0270(4) 0.1656(4) 0.5507(5) 0.087(3) Uani 1 1 d DU . . H15_1 H 0.0160 0.1507 0.5884 0.104 Uiso 1 1 calc R . . C16_1 C -0.0063(3) 0.1780(4) 0.5050(4) 0.068(3) Uani 1 1 d DU . . C17_1 C 0.0796(4) 0.2349(4) 0.3842(5) 0.098(4) Uani 1 1 d DU . . H17_1 H 0.0499 0.2471 0.3623 0.118 Uiso 1 1 calc R . . C19_1 C -0.0601(3) 0.1690(3) 0.5146(5) 0.070(3) Uani 1 1 d DU . . H19_1 H -0.0777 0.1810 0.4765 0.084 Uiso 1 1 calc R . . C21_1 C -0.0957(3) 0.1982(4) 0.2675(4) 0.065(2) Uani 1 1 d DU . . C22_1 C -0.1432(3) 0.1835(4) 0.2757(4) 0.067(3) Uani 1 1 d DU . . C23_1 C -0.1699(4) 0.1706(5) 0.2228(5) 0.093(4) Uani 1 1 d DU . . H23_1 H -0.2033 0.1626 0.2269 0.112 Uiso 1 1 calc R . . C24_1 C -0.1484(4) 0.1696(6) 0.1654(6) 0.117(5) Uani 1 1 d DU . . H24_1 H -0.1668 0.1608 0.1294 0.141 Uiso 1 1 calc R . . C25_1 C -0.1002(4) 0.1810(5) 0.1588(5) 0.111(5) Uani 1 1 d DU . . H25_1 H -0.0853 0.1777 0.1186 0.133 Uiso 1 1 calc R . . C26_1 C -0.0726(3) 0.1972(5) 0.2096(4) 0.085(3) Uani 1 1 d DU . . C27_1 C -0.1675(4) 0.1849(4) 0.3397(5) 0.093(4) Uani 1 1 d DU . . H27_1 H -0.1461 0.2035 0.3690 0.112 Uiso 1 1 calc R . . C29_1 C -0.0199(4) 0.2112(5) 0.1991(6) 0.113(5) Uani 1 1 d DU . . H29_1 H -0.0084 0.2304 0.2361 0.135 Uiso 1 1 calc R . . C171_1 C 0.1095(8) 0.2796(6) 0.3937(8) 0.267(11) Uani 1 1 d DU . . H17A_1 H 0.0941 0.3003 0.4255 0.400 Uiso 1 1 calc R . . H17B_1 H 0.1121 0.2973 0.3538 0.400 Uiso 1 1 calc R . . H17C_1 H 0.1420 0.2704 0.4082 0.400 Uiso 1 1 calc R . . C172_1 C 0.1027(6) 0.2021(5) 0.3365(7) 0.145(7) Uani 1 1 d DU . . H17D_1 H 0.0796 0.1768 0.3243 0.217 Uiso 1 1 calc R . . H17E_1 H 0.1316 0.1872 0.3548 0.217 Uiso 1 1 calc R . . H17F_1 H 0.1118 0.2210 0.2992 0.217 Uiso 1 1 calc R . . C191_1 C -0.0786(6) 0.1966(5) 0.5714(7) 0.134(6) Uani 1 1 d DU . . H19A_1 H -0.1134 0.1904 0.5766 0.201 Uiso 1 1 calc R . . H19B_1 H -0.0733 0.2314 0.5651 0.201 Uiso 1 1 calc R . . H19C_1 H -0.0613 0.1859 0.6092 0.201 Uiso 1 1 calc R . . C192_1 C -0.0716(5) 0.1148(3) 0.5227(6) 0.086(4) Uani 1 1 d DU . . H19D_1 H -0.0595 0.0969 0.4861 0.128 Uiso 1 1 calc R . . H19E_1 H -0.1067 0.1104 0.5262 0.128 Uiso 1 1 calc R . . H19F_1 H -0.0559 0.1027 0.5610 0.128 Uiso 1 1 calc R . . C271_1 C -0.2168(5) 0.2111(6) 0.3367(8) 0.160(7) Uani 1 1 d DU . . H27A_1 H -0.2119 0.2443 0.3216 0.240 Uiso 1 1 calc R . . H27B_1 H -0.2313 0.2119 0.3788 0.240 Uiso 1 1 calc R . . H27C_1 H -0.2383 0.1938 0.3077 0.240 Uiso 1 1 calc R . . C272_1 C -0.1753(6) 0.1354(5) 0.3676(8) 0.136(7) Uani 1 1 d DU . . H27D_1 H -0.1445 0.1179 0.3688 0.204 Uiso 1 1 calc R . . H27E_1 H -0.1986 0.1174 0.3417 0.204 Uiso 1 1 calc R . . H27F_1 H -0.1881 0.1386 0.4106 0.204 Uiso 1 1 calc R . . C291_1 C -0.0136(7) 0.2415(7) 0.1397(8) 0.216(9) Uani 1 1 d DU . . H29A_1 H -0.0338 0.2706 0.1426 0.324 Uiso 1 1 calc R . . H29B_1 H -0.0234 0.2224 0.1028 0.324 Uiso 1 1 calc R . . H29C_1 H 0.0205 0.2509 0.1353 0.324 Uiso 1 1 calc R . . C292_1 C 0.0130(5) 0.1670(6) 0.1913(8) 0.150(6) Uani 1 1 d DU . . H29D_1 H 0.0108 0.1466 0.2289 0.225 Uiso 1 1 calc R . . H29E_1 H 0.0466 0.1778 0.1856 0.225 Uiso 1 1 calc R . . H29F_1 H 0.0028 0.1485 0.1542 0.225 Uiso 1 1 calc R . . C31_1 C -0.0219(4) 0.0419(3) 0.3501(5) 0.056(3) Uani 1 1 d DU . . C32_1 C -0.0192(4) -0.0015(3) 0.3505(6) 0.079(4) Uani 1 1 d DU . . C33_1 C -0.0130(4) -0.0533(3) 0.3484(4) 0.067(3) Uani 1 1 d DU . . N34_1 N 0.0117(3) -0.0713(2) 0.3023(4) 0.064(2) Uani 1 1 d DU . . C35_1 C 0.0157(5) -0.1246(3) 0.2971(5) 0.081(3) Uani 1 1 d DU . . H35A_1 H -0.0162 -0.1400 0.2895 0.097 Uiso 1 1 calc R . . H35B_1 H 0.0309 -0.1391 0.3349 0.097 Uiso 1 1 calc R . . C36_1 C 0.0489(6) -0.1276(4) 0.2389(8) 0.153(7) Uani 1 1 d DU . . H36A_1 H 0.0815 -0.1389 0.2517 0.184 Uiso 1 1 calc R . . H36B_1 H 0.0355 -0.1512 0.2083 0.184 Uiso 1 1 calc R . . C37_1 C 0.0526(6) -0.0783(4) 0.2085(6) 0.119(6) Uani 1 1 d DU . . H37A_1 H 0.0870 -0.0703 0.2002 0.142 Uiso 1 1 calc R . . H37B_1 H 0.0349 -0.0781 0.1679 0.142 Uiso 1 1 calc R . . C38_1 C 0.0318(5) -0.0435(4) 0.2509(6) 0.085(4) Uani 1 1 d DU . . H38A_1 H 0.0062 -0.0245 0.2296 0.102 Uiso 1 1 calc R . . H38B_1 H 0.0569 -0.0209 0.2666 0.102 Uiso 1 1 calc R . . O39_1 O -0.0310(3) -0.0851(3) 0.3888(4) 0.087(3) Uani 1 1 d DU . . C39_1 C -0.0494(6) -0.0703(6) 0.4474(6) 0.122(6) Uani 1 1 d DU . . H39A_1 H -0.0610 -0.0986 0.4707 0.183 Uiso 1 1 calc R . . H39B_1 H -0.0762 -0.0476 0.4409 0.183 Uiso 1 1 calc R . . H39C_1 H -0.0237 -0.0543 0.4715 0.183 Uiso 1 1 calc R . . Au1_2 Au 0.387871(13) 0.474462(15) 1.096157(17) 0.04870(11) Uani 1 1 d DU . . C1_2 C 0.3177(3) 0.4634(3) 1.1188(4) 0.044(2) Uani 1 1 d DU . . N2_2 N 0.2926(2) 0.4820(2) 1.1677(3) 0.0449(18) Uani 1 1 d DU . . C3_2 C 0.2484(3) 0.4597(3) 1.1753(5) 0.057(3) Uani 1 1 d DU . . H3_2 H 0.2246 0.4670 1.2062 0.069 Uiso 1 1 calc R . . C4_2 C 0.2455(3) 0.4263(4) 1.1312(5) 0.066(3) Uani 1 1 d DU . . H4_2 H 0.2193 0.4046 1.1247 0.080 Uiso 1 1 calc R . . N5_2 N 0.2879(2) 0.4284(3) 1.0960(4) 0.0530(19) Uani 1 1 d DU . . C11_2 C 0.3091(3) 0.5218(3) 1.2069(4) 0.050(2) Uani 1 1 d DU . . C12_2 C 0.3322(3) 0.5106(3) 1.2633(4) 0.059(2) Uani 1 1 d DU . . C13_2 C 0.3510(4) 0.5492(3) 1.2979(5) 0.081(3) Uani 1 1 d DU . . H13_2 H 0.3675 0.5434 1.3364 0.097 Uiso 1 1 calc R . . C14_2 C 0.3453(5) 0.5958(4) 1.2758(6) 0.103(4) Uani 1 1 d DU . . H14_2 H 0.3566 0.6220 1.3010 0.124 Uiso 1 1 calc R . . C15_2 C 0.3239(4) 0.6059(4) 1.2187(5) 0.081(4) Uani 1 1 d DU . . H15_2 H 0.3240 0.6380 1.2026 0.097 Uiso 1 1 calc R . . C16_2 C 0.3020(3) 0.5687(3) 1.1845(4) 0.059(3) Uani 1 1 d DU . . C17_2 C 0.3383(3) 0.4593(4) 1.2876(5) 0.078(3) Uani 1 1 d DU . . H17_2 H 0.3186 0.4377 1.2596 0.093 Uiso 1 1 calc R . . C19_2 C 0.2747(3) 0.5808(4) 1.1250(4) 0.063(3) Uani 1 1 d DU . . H19_2 H 0.2562 0.5513 1.1121 0.076 Uiso 1 1 calc R . . C21_2 C 0.2993(3) 0.3949(3) 1.0458(4) 0.059(2) Uani 1 1 d DU . . C22_2 C 0.2830(4) 0.4070(3) 0.9861(4) 0.061(3) Uani 1 1 d DU . . C23_2 C 0.2920(5) 0.3731(4) 0.9391(5) 0.091(4) Uani 1 1 d DU . . H23_2 H 0.2826 0.3803 0.8971 0.109 Uiso 1 1 calc R . . C24_2 C 0.3142(5) 0.3297(4) 0.9515(5) 0.089(4) Uani 1 1 d DU . . H24_2 H 0.3199 0.3072 0.9184 0.107 Uiso 1 1 calc R . . C25_2 C 0.3280(5) 0.3189(4) 1.0120(5) 0.084(3) Uani 1 1 d DU . . H25_2 H 0.3420 0.2881 1.0206 0.100 Uiso 1 1 calc R . . C26_2 C 0.3220(3) 0.3515(3) 1.0607(4) 0.061(2) Uani 1 1 d DU . . C27_2 C 0.2591(4) 0.4554(3) 0.9711(6) 0.087(3) Uani 1 1 d DU . . H27_2 H 0.2523 0.4720 1.0121 0.104 Uiso 1 1 calc R . . C29_2 C 0.3381(3) 0.3388(4) 1.1272(5) 0.077(3) Uani 1 1 d DU . . H29_2 H 0.3295 0.3660 1.1562 0.092 Uiso 1 1 calc R . . C171_2 C 0.3185(5) 0.4539(5) 1.3536(6) 0.106(5) Uani 1 1 d DU . . H17A_2 H 0.3231 0.4204 1.3679 0.159 Uiso 1 1 calc R . . H17B_2 H 0.2838 0.4616 1.3537 0.159 Uiso 1 1 calc R . . H17C_2 H 0.3356 0.4760 1.3820 0.159 Uiso 1 1 calc R . . C172_2 C 0.3908(3) 0.4424(5) 1.2828(7) 0.097(5) Uani 1 1 d DU . . H17D_2 H 0.3935 0.4091 1.2987 0.146 Uiso 1 1 calc R . . H17E_2 H 0.4115 0.4638 1.3081 0.146 Uiso 1 1 calc R . . H17F_2 H 0.4013 0.4434 1.2387 0.146 Uiso 1 1 calc R . . C191_2 C 0.2383(4) 0.6215(5) 1.1346(7) 0.101(5) Uani 1 1 d DU . . H19A_2 H 0.2170 0.6135 1.1701 0.152 Uiso 1 1 calc R . . H19B_2 H 0.2188 0.6254 1.0963 0.152 Uiso 1 1 calc R . . H19C_2 H 0.2556 0.6517 1.1436 0.152 Uiso 1 1 calc R . . C192_2 C 0.3068(5) 0.5948(6) 1.0707(6) 0.118(5) Uani 1 1 d DU . . H19D_2 H 0.2868 0.6018 1.0336 0.177 Uiso 1 1 calc R . . H19E_2 H 0.3289 0.5680 1.0611 0.177 Uiso 1 1 calc R . . H19F_2 H 0.3256 0.6236 1.0820 0.177 Uiso 1 1 calc R . . C271_2 C 0.2106(4) 0.4486(5) 0.9371(8) 0.120(6) Uani 1 1 d DU . . H27A_2 H 0.1895 0.4278 0.9624 0.180 Uiso 1 1 calc R . . H27B_2 H 0.2163 0.4334 0.8959 0.180 Uiso 1 1 calc R . . H27C_2 H 0.1951 0.4802 0.9310 0.180 Uiso 1 1 calc R . . C272_2 C 0.2930(5) 0.4883(5) 0.9331(7) 0.111(5) Uani 1 1 d DU . . H27D_2 H 0.2768 0.5192 0.9247 0.166 Uiso 1 1 calc R . . H27E_2 H 0.3012 0.4725 0.8931 0.166 Uiso 1 1 calc R . . H27F_2 H 0.3227 0.4941 0.9572 0.166 Uiso 1 1 calc R . . C291_2 C 0.3146(6) 0.2917(5) 1.1517(8) 0.141(6) Uani 1 1 d DU . . H29A_2 H 0.2793 0.2952 1.1515 0.212 Uiso 1 1 calc R . . H29B_2 H 0.3258 0.2853 1.1948 0.212 Uiso 1 1 calc R . . H29C_2 H 0.3239 0.2646 1.1243 0.212 Uiso 1 1 calc R . . C292_2 C 0.3920(4) 0.3312(6) 1.1286(7) 0.125(6) Uani 1 1 d DU . . H29D_2 H 0.4023 0.3238 1.1717 0.188 Uiso 1 1 calc R . . H29E_2 H 0.4082 0.3608 1.1141 0.188 Uiso 1 1 calc R . . H29F_2 H 0.4006 0.3042 1.1007 0.188 Uiso 1 1 calc R . . C31_2 C 0.4578(3) 0.4830(4) 1.0790(6) 0.063(3) Uani 1 1 d DU . . C32_2 C 0.5006(3) 0.4878(4) 1.0722(5) 0.061(3) Uani 1 1 d DU . . C33_2 C 0.5524(3) 0.4931(4) 1.0698(4) 0.059(3) Uani 1 1 d DU . . N34_2 N 0.5778(3) 0.4747(3) 1.1135(4) 0.066(2) Uani 1 1 d DU . . C35_2 C 0.6310(3) 0.4802(5) 1.1130(6) 0.086(4) Uani 1 1 d DU . . H35A_2 H 0.6407 0.5139 1.1230 0.103 Uiso 1 1 calc R . . H35B_2 H 0.6450 0.4708 1.0718 0.103 Uiso 1 1 calc R . . C36_2 C 0.6463(4) 0.4450(7) 1.1653(7) 0.155(8) Uani 1 1 d DU . . H36A_2 H 0.6607 0.4154 1.1469 0.186 Uiso 1 1 calc R . . H36B_2 H 0.6705 0.4604 1.1934 0.186 Uiso 1 1 calc R . . C37_2 C 0.6015(5) 0.4330(8) 1.2010(8) 0.184(9) Uani 1 1 d DU . . H37A_2 H 0.6012 0.3980 1.2111 0.221 Uiso 1 1 calc R . . H37B_2 H 0.6010 0.4513 1.2411 0.221 Uiso 1 1 calc R . . C38_2 C 0.5598(4) 0.4449(5) 1.1649(5) 0.094(4) Uani 1 1 d DU . . H38A_2 H 0.5361 0.4630 1.1908 0.113 Uiso 1 1 calc R . . H38B_2 H 0.5441 0.4152 1.1485 0.113 Uiso 1 1 calc R . . O39_2 O 0.5743(3) 0.5181(3) 1.0249(3) 0.072(2) Uani 1 1 d DU . . C39_2 C 0.5507(5) 0.5291(5) 0.9676(5) 0.092(4) Uani 1 1 d DU . . H39A_2 H 0.5725 0.5478 0.9406 0.138 Uiso 1 1 calc R . . H39B_2 H 0.5215 0.5481 0.9764 0.138 Uiso 1 1 calc R . . H39C_2 H 0.5416 0.4989 0.9462 0.138 Uiso 1 1 calc R . . Au1_3 Au -0.110012(13) 0.463122(15) 1.04402(2) 0.05277(11) Uani 1 1 d DU . . C1_3 C -0.1821(2) 0.4525(3) 1.0377(4) 0.047(2) Uani 1 1 d DU . . N2_3 N -0.2115(2) 0.4714(3) 0.9943(3) 0.053(2) Uani 1 1 d DU . . C3_3 C -0.2581(3) 0.4505(4) 1.0008(5) 0.060(3) Uani 1 1 d DU . . H3_3 H -0.2853 0.4561 0.9743 0.072 Uiso 1 1 calc R . . C4_3 C -0.2569(3) 0.4219(4) 1.0502(5) 0.066(3) Uani 1 1 d DU . . H4_3 H -0.2832 0.4038 1.0670 0.079 Uiso 1 1 calc R . . N5_3 N -0.2103(2) 0.4230(3) 1.0729(3) 0.052(2) Uani 1 1 d DU . . C11_3 C -0.1983(3) 0.5073(3) 0.9480(4) 0.056(2) Uani 1 1 d DU . . C12_3 C -0.2020(4) 0.5556(3) 0.9633(4) 0.081(3) Uani 1 1 d DU . . C13_3 C -0.1919(5) 0.5899(4) 0.9181(5) 0.096(4) Uani 1 1 d DU . . H13_3 H -0.1995 0.6230 0.9255 0.115 Uiso 1 1 calc R . . C14_3 C -0.1711(6) 0.5763(4) 0.8629(6) 0.123(6) Uani 1 1 d DU . . H14_3 H -0.1584 0.6000 0.8349 0.148 Uiso 1 1 calc R . . C15_3 C -0.1686(5) 0.5273(4) 0.8475(5) 0.095(4) Uani 1 1 d DU . . H15_3 H -0.1572 0.5182 0.8069 0.115 Uiso 1 1 calc R . . C16_3 C -0.1822(4) 0.4911(3) 0.8897(4) 0.066(3) Uani 1 1 d DU . . C17_3 C -0.2249(4) 0.5719(4) 1.0259(5) 0.084(3) Uani 1 1 d DU . . H17_3 H -0.2300 0.5421 1.0519 0.101 Uiso 1 1 calc R . . C19_3 C -0.1759(4) 0.4382(4) 0.8725(5) 0.078(3) Uani 1 1 d DU . . H19_3 H -0.1911 0.4188 0.9071 0.094 Uiso 1 1 calc R . . C21_3 C -0.1950(4) 0.3939(3) 1.1259(4) 0.068(3) Uani 1 1 d DU . . C22_3 C -0.1817(4) 0.3463(3) 1.1145(5) 0.092(3) Uani 1 1 d DU . . C23_3 C -0.1683(6) 0.3196(5) 1.1670(6) 0.129(5) Uani 1 1 d DU . . H23_3 H -0.1572 0.2873 1.1618 0.155 Uiso 1 1 calc R . . C24_3 C -0.1708(7) 0.3391(5) 1.2259(7) 0.162(7) Uani 1 1 d DU . . H24_3 H -0.1608 0.3198 1.2607 0.194 Uiso 1 1 calc R . . C25_3 C -0.1869(7) 0.3849(5) 1.2371(5) 0.137(6) Uani 1 1 d DU . . H25_3 H -0.1895 0.3968 1.2790 0.164 Uiso 1 1 calc R . . C26_3 C -0.1996(5) 0.4143(4) 1.1858(4) 0.087(3) Uani 1 1 d DU . . C27_3 C -0.1785(4) 0.3262(4) 1.0479(6) 0.136(5) Uani 1 1 d DU . . H27_3 H -0.1902 0.3536 1.0210 0.164 Uiso 1 1 calc R . . C29_3 C -0.2150(5) 0.4668(4) 1.1962(6) 0.132(5) Uani 1 1 d DU . . H29_3 H -0.2358 0.4779 1.1604 0.159 Uiso 1 1 calc R . . C171_3 C -0.2739(5) 0.5945(6) 1.0156(8) 0.157(7) Uani 1 1 d DU . . H17A_3 H -0.2954 0.5709 0.9954 0.235 Uiso 1 1 calc R . . H17B_3 H -0.2705 0.6230 0.9884 0.235 Uiso 1 1 calc R . . H17C_3 H -0.2876 0.6042 1.0563 0.235 Uiso 1 1 calc R . . C172_3 C -0.1914(6) 0.6042(6) 1.0619(7) 0.143(7) Uani 1 1 d DU . . H17D_3 H -0.1600 0.5882 1.0669 0.215 Uiso 1 1 calc R . . H17E_3 H -0.2052 0.6111 1.1035 0.215 Uiso 1 1 calc R . . H17F_3 H -0.1870 0.6347 1.0388 0.215 Uiso 1 1 calc R . . C191_3 C -0.2017(5) 0.4245(6) 0.8117(6) 0.120(5) Uani 1 1 d DU . . H19A_3 H -0.2359 0.4339 0.8145 0.180 Uiso 1 1 calc R . . H19B_3 H -0.1994 0.3894 0.8052 0.180 Uiso 1 1 calc R . . H19C_3 H -0.1865 0.4414 0.7761 0.180 Uiso 1 1 calc R . . C192_3 C -0.1230(4) 0.4253(5) 0.8715(7) 0.097(5) Uani 1 1 d DU . . H19D_3 H -0.1193 0.3910 0.8605 0.146 Uiso 1 1 calc R . . H19E_3 H -0.1089 0.4312 0.9132 0.146 Uiso 1 1 calc R . . H19F_3 H -0.1063 0.4453 0.8401 0.146 Uiso 1 1 calc R . . C271_3 C -0.2124(6) 0.2860(7) 1.0326(14) 0.285(14) Uani 1 1 d DU . . H27A_3 H -0.2453 0.2948 1.0458 0.427 Uiso 1 1 calc R . . H27B_3 H -0.2023 0.2565 1.0549 0.427 Uiso 1 1 calc R . . H27C_3 H -0.2120 0.2800 0.9871 0.427 Uiso 1 1 calc R . . C272_3 C -0.1275(5) 0.3194(6) 1.0276(8) 0.142(7) Uani 1 1 d DU . . H27D_3 H -0.1089 0.3488 1.0367 0.213 Uiso 1 1 calc R . . H27E_3 H -0.1265 0.3128 0.9822 0.213 Uiso 1 1 calc R . . H27F_3 H -0.1133 0.2920 1.0505 0.213 Uiso 1 1 calc R . . C291_3 C -0.2429(6) 0.4707(7) 1.2582(6) 0.174(8) Uani 1 1 d DU . . H29A_3 H -0.2519 0.5045 1.2656 0.262 Uiso 1 1 calc R . . H29B_3 H -0.2225 0.4592 1.2929 0.262 Uiso 1 1 calc R . . H29C_3 H -0.2723 0.4508 1.2558 0.262 Uiso 1 1 calc R . . C292_3 C -0.1702(7) 0.4993(6) 1.2017(10) 0.186(9) Uani 1 1 d DU . . H29D_3 H -0.1511 0.4971 1.1629 0.279 Uiso 1 1 calc R . . H29E_3 H -0.1505 0.4888 1.2376 0.279 Uiso 1 1 calc R . . H29F_3 H -0.1805 0.5330 1.2082 0.279 Uiso 1 1 calc R . . C31_3 C -0.0383(3) 0.4677(4) 1.0451(7) 0.077(4) Uani 1 1 d DU . . C32_3 C 0.0051(3) 0.4704(5) 1.0461(7) 0.094(4) Uani 1 1 d DU . . C33_3 C 0.0572(3) 0.4734(4) 1.0450(5) 0.079(3) Uani 1 1 d DU . . N34_3 N 0.0787(3) 0.4951(4) 1.0900(4) 0.085(3) Uani 1 1 d DU . . C35_3 C 0.1326(3) 0.4976(5) 1.0877(6) 0.098(4) Uani 1 1 d DU . . H35A_3 H 0.1445 0.5080 1.0458 0.118 Uiso 1 1 calc R . . H35B_3 H 0.1478 0.4663 1.0994 0.118 Uiso 1 1 calc R . . C36_3 C 0.1405(5) 0.5368(7) 1.1385(9) 0.181(9) Uani 1 1 d DU . . H36A_3 H 0.1697 0.5294 1.1640 0.218 Uiso 1 1 calc R . . H36B_3 H 0.1446 0.5691 1.1189 0.218 Uiso 1 1 calc R . . C37_3 C 0.0952(5) 0.5355(7) 1.1794(7) 0.135(6) Uani 1 1 d DU . . H37A_3 H 0.1006 0.5141 1.2161 0.162 Uiso 1 1 calc R . . H37B_3 H 0.0880 0.5685 1.1952 0.162 Uiso 1 1 calc R . . C38_3 C 0.0556(4) 0.5182(7) 1.1434(6) 0.123(6) Uani 1 1 d DU . . H38A_3 H 0.0344 0.5451 1.1296 0.148 Uiso 1 1 calc R . . H38B_3 H 0.0360 0.4946 1.1677 0.148 Uiso 1 1 calc R . . O39_3 O 0.0838(3) 0.4518(4) 1.0017(4) 0.094(3) Uani 1 1 d DU . . C39_3 C 0.0640(7) 0.4325(7) 0.9461(7) 0.153(8) Uani 1 1 d DU . . H39A_3 H 0.0898 0.4181 0.9205 0.229 Uiso 1 1 calc R . . H39B_3 H 0.0481 0.4584 0.9221 0.229 Uiso 1 1 calc R . . H39C_3 H 0.0401 0.4076 0.9568 0.229 Uiso 1 1 calc R . . Au1_4 Au 0.015311(16) 0.383610(14) 0.79107(2) 0.05699(12) Uani 1 1 d DU . . C1_4 C 0.0272(3) 0.3128(3) 0.7727(4) 0.051(2) Uani 1 1 d DU . . N2_4 N 0.0593(3) 0.2830(2) 0.8005(4) 0.061(2) Uani 1 1 d DU . . C3_4 C 0.0600(4) 0.2389(3) 0.7701(6) 0.079(4) Uani 1 1 d DU . . H3_4 H 0.0804 0.2123 0.7802 0.095 Uiso 1 1 calc R . . C4_4 C 0.0277(4) 0.2400(3) 0.7249(6) 0.070(3) Uani 1 1 d DU . . H4_4 H 0.0199 0.2146 0.6965 0.084 Uiso 1 1 calc R . . N5_4 N 0.0069(3) 0.2863(2) 0.7268(4) 0.053(2) Uani 1 1 d DU . . C11_4 C 0.0910(3) 0.2958(3) 0.8516(4) 0.071(3) Uani 1 1 d DU . . C12_4 C 0.1360(3) 0.3144(4) 0.8380(5) 0.082(3) Uani 1 1 d DU . . C13_4 C 0.1658(4) 0.3259(5) 0.8880(6) 0.111(4) Uani 1 1 d DU . . H13_4 H 0.1965 0.3405 0.8805 0.133 Uiso 1 1 calc R . . C14_4 C 0.1513(4) 0.3161(6) 0.9484(6) 0.123(5) Uani 1 1 d DU . . H14_4 H 0.1726 0.3233 0.9824 0.148 Uiso 1 1 calc R . . C15_4 C 0.1070(4) 0.2963(5) 0.9609(6) 0.118(5) Uani 1 1 d DU . . H15_4 H 0.0971 0.2911 1.0033 0.141 Uiso 1 1 calc R . . C16_4 C 0.0765(3) 0.2837(4) 0.9118(5) 0.086(3) Uani 1 1 d DU . . C17_4 C 0.1507(5) 0.3268(4) 0.7706(6) 0.115(4) Uani 1 1 d DU . . H17_4 H 0.1225 0.3179 0.7434 0.138 Uiso 1 1 calc R . . C19_4 C 0.0275(4) 0.2598(4) 0.9249(6) 0.106(4) Uani 1 1 d DU . . H19_4 H 0.0114 0.2555 0.8830 0.127 Uiso 1 1 calc R . . C21_4 C -0.0294(3) 0.3032(3) 0.6842(4) 0.063(3) Uani 1 1 d DU . . C22_4 C -0.0776(3) 0.2925(4) 0.6976(5) 0.071(3) Uani 1 1 d DU . . C23_4 C -0.1114(4) 0.3088(5) 0.6546(6) 0.099(4) Uani 1 1 d DU . . H23_4 H -0.1446 0.3009 0.6608 0.118 Uiso 1 1 calc R . . C24_4 C -0.0987(5) 0.3361(6) 0.6034(7) 0.134(6) Uani 1 1 d DU . . H24_4 H -0.1231 0.3496 0.5771 0.161 Uiso 1 1 calc R . . C25_4 C -0.0508(4) 0.3440(6) 0.5899(6) 0.127(5) Uani 1 1 d DU . . H25_4 H -0.0421 0.3598 0.5517 0.153 Uiso 1 1 calc R . . C26_4 C -0.0147(3) 0.3293(4) 0.6315(5) 0.075(3) Uani 1 1 d DU . . C27_4 C -0.0922(4) 0.2628(4) 0.7551(5) 0.077(3) Uani 1 1 d DU . . H27_4 H -0.0638 0.2431 0.7691 0.092 Uiso 1 1 calc R . . C29_4 C 0.0387(4) 0.3389(4) 0.6169(6) 0.099(4) Uani 1 1 d DU . . H29_4 H 0.0592 0.3230 0.6498 0.119 Uiso 1 1 calc R . . C171_4 C 0.1928(5) 0.2960(6) 0.7486(10) 0.166(8) Uani 1 1 d DU . . H17A_4 H 0.1845 0.2616 0.7534 0.249 Uiso 1 1 calc R . . H17B_4 H 0.2215 0.3034 0.7741 0.249 Uiso 1 1 calc R . . H17C_4 H 0.1996 0.3029 0.7042 0.249 Uiso 1 1 calc R . . C172_4 C 0.1590(6) 0.3801(4) 0.7608(8) 0.128(6) Uani 1 1 d DU . . H17D_4 H 0.1681 0.3860 0.7168 0.193 Uiso 1 1 calc R . . H17E_4 H 0.1851 0.3912 0.7885 0.193 Uiso 1 1 calc R . . H17F_4 H 0.1292 0.3979 0.7706 0.193 Uiso 1 1 calc R . . C191_4 C 0.0331(6) 0.2090(5) 0.9529(11) 0.216(10) Uani 1 1 d DU . . H19A_4 H 0.0532 0.1892 0.9248 0.324 Uiso 1 1 calc R . . H19B_4 H 0.0011 0.1940 0.9574 0.324 Uiso 1 1 calc R . . H19C_4 H 0.0486 0.2113 0.9943 0.324 Uiso 1 1 calc R . . C192_4 C -0.0041(6) 0.2941(7) 0.9623(10) 0.206(9) Uani 1 1 d DU . . H19D_4 H -0.0358 0.2791 0.9695 0.309 Uiso 1 1 calc R . . H19E_4 H -0.0083 0.3243 0.9386 0.309 Uiso 1 1 calc R . . H19F_4 H 0.0114 0.3011 1.0028 0.309 Uiso 1 1 calc R . . C271_4 C -0.1348(4) 0.2286(4) 0.7414(7) 0.097(4) Uani 1 1 d DU . . H27A_4 H -0.1256 0.2058 0.7080 0.145 Uiso 1 1 calc R . . H27B_4 H -0.1629 0.2476 0.7277 0.145 Uiso 1 1 calc R . . H27C_4 H -0.1431 0.2106 0.7797 0.145 Uiso 1 1 calc R . . C272_4 C -0.1069(6) 0.2968(5) 0.8079(7) 0.131(6) Uani 1 1 d DU . . H27D_4 H -0.1160 0.2778 0.8451 0.197 Uiso 1 1 calc R . . H27E_4 H -0.1345 0.3165 0.7944 0.197 Uiso 1 1 calc R . . H27F_4 H -0.0796 0.3180 0.8185 0.197 Uiso 1 1 calc R . . C291_4 C 0.0507(8) 0.3171(6) 0.5527(8) 0.217(10) Uani 1 1 d DU . . H29A_4 H 0.0453 0.2820 0.5539 0.325 Uiso 1 1 calc R . . H29B_4 H 0.0848 0.3236 0.5425 0.325 Uiso 1 1 calc R . . H29C_4 H 0.0299 0.3317 0.5204 0.325 Uiso 1 1 calc R . . C292_4 C 0.0499(6) 0.3930(4) 0.6157(8) 0.121(6) Uani 1 1 d DU . . H29D_4 H 0.0446 0.4067 0.6577 0.182 Uiso 1 1 calc R . . H29E_4 H 0.0285 0.4091 0.5853 0.182 Uiso 1 1 calc R . . H29F_4 H 0.0837 0.3979 0.6032 0.182 Uiso 1 1 calc R . . C31_4 C 0.0063(4) 0.4539(3) 0.8034(7) 0.079(4) Uani 1 1 d DU . . C32_4 C 0.0032(5) 0.4969(3) 0.8039(8) 0.105(5) Uani 1 1 d DU . . C33_4 C -0.0037(5) 0.5477(3) 0.8155(5) 0.089(3) Uani 1 1 d DU . . N34_4 N 0.0141(4) 0.5758(3) 0.7742(5) 0.092(3) Uani 1 1 d DU . . C35_4 C 0.0034(8) 0.6273(4) 0.7880(9) 0.193(9) Uani 1 1 d DU . . H35A_4 H 0.0168 0.6381 0.8290 0.232 Uiso 1 1 calc R . . H35B_4 H -0.0316 0.6349 0.7856 0.232 Uiso 1 1 calc R . . C36_4 C 0.0328(12) 0.6479(5) 0.7300(12) 0.324(18) Uani 1 1 d DU . . H36A_4 H 0.0122 0.6701 0.7049 0.389 Uiso 1 1 calc R . . H36B_4 H 0.0615 0.6661 0.7448 0.389 Uiso 1 1 calc R . . C37_4 C 0.0487(12) 0.6044(6) 0.6896(10) 0.291(16) Uani 1 1 d DU . . H37A_4 H 0.0277 0.6021 0.6519 0.349 Uiso 1 1 calc R . . H37B_4 H 0.0824 0.6093 0.6751 0.349 Uiso 1 1 calc R . . C38_4 C 0.0457(6) 0.5609(5) 0.7244(7) 0.121(5) Uani 1 1 d DU . . H38A_4 H 0.0777 0.5507 0.7406 0.146 Uiso 1 1 calc R . . H38B_4 H 0.0314 0.5343 0.6992 0.146 Uiso 1 1 calc R . . O39_4 O -0.0289(4) 0.5683(3) 0.8611(4) 0.104(3) Uani 1 1 d DU . . C39_4 C -0.0447(6) 0.5435(6) 0.9156(7) 0.129(6) Uani 1 1 d DU . . H39A_4 H -0.0636 0.5655 0.9422 0.193 Uiso 1 1 calc R . . H39B_4 H -0.0165 0.5318 0.9393 0.193 Uiso 1 1 calc R . . H39C_4 H -0.0649 0.5159 0.9033 0.193 Uiso 1 1 calc R . . S1 S 0.10829(15) 0.10073(14) 0.7270(2) 0.0984(12) Uani 1 1 d DU . . O11 O 0.0999(5) 0.1352(4) 0.7740(6) 0.174(5) Uani 1 1 d DU . . O12 O 0.0816(5) 0.1004(7) 0.6715(5) 0.245(8) Uani 1 1 d DU . . O13 O 0.1201(5) 0.0561(3) 0.7541(6) 0.174(6) Uani 1 1 d DU . . C51 C 0.1625(4) 0.1192(4) 0.6995(5) 0.121(4) Uani 1 1 d DU . . F11 F 0.1793(4) 0.0963(5) 0.6487(5) 0.234(6) Uani 1 1 d DU . . F12 F 0.1986(4) 0.1130(5) 0.7400(5) 0.195(5) Uani 1 1 d DU . . F13 F 0.1633(5) 0.1632(4) 0.6792(7) 0.217(6) Uani 1 1 d DU . . S2 S -0.1203(3) 0.6263(3) 0.7003(3) 0.237(3) Uani 1 1 d DU . . O21 O -0.0734(5) 0.6075(7) 0.6786(12) 0.358(11) Uani 1 1 d DU . . O22 O -0.1115(6) 0.6669(5) 0.7427(6) 0.212(6) Uani 1 1 d DU . . O23 O -0.1514(6) 0.5907(6) 0.7027(7) 0.279(8) Uani 1 1 d DU . . C52 C -0.1255(5) 0.6584(5) 0.6347(6) 0.208(6) Uani 1 1 d DU . . F21 F -0.1631(7) 0.6847(7) 0.6515(12) 0.436(10) Uani 1 1 d DU . . F22 F -0.1335(6) 0.6307(5) 0.5873(5) 0.231(6) Uani 1 1 d DU . . F23 F -0.0873(7) 0.6859(7) 0.6259(8) 0.405(10) Uani 1 1 d DU . . S3 S 0.09977(16) 0.59125(14) 0.9240(2) 0.0979(12) Uani 1 1 d DU . . O31 O 0.0725(4) 0.6341(4) 0.9285(7) 0.163(5) Uani 1 1 d DU . . O32 O 0.0991(6) 0.5625(6) 0.8692(6) 0.226(7) Uani 1 1 d DU . . O33 O 0.0936(6) 0.5640(5) 0.9789(6) 0.212(6) Uani 1 1 d DU . . C53 C 0.1556(4) 0.6138(4) 0.9287(6) 0.136(4) Uani 1 1 d DU . . F31 F 0.1893(4) 0.5819(6) 0.9198(10) 0.320(9) Uani 1 1 d DU . . F32 F 0.1683(4) 0.6367(6) 0.9794(5) 0.211(6) Uani 1 1 d DU . . F33 F 0.1675(6) 0.6455(6) 0.8834(6) 0.269(7) Uani 1 1 d DU . . S4 S 0.60212(16) 0.38641(17) 0.9694(3) 0.1234(16) Uani 1 1 d DU . . O41 O 0.5860(6) 0.3890(8) 0.9064(6) 0.340(9) Uani 1 1 d DU . . O42 O 0.5624(4) 0.3842(7) 1.0108(7) 0.264(8) Uani 1 1 d DU . . O43 O 0.6413(4) 0.4111(6) 0.9876(10) 0.295(10) Uani 1 1 d DU . . C54 C 0.6221(5) 0.3304(5) 0.9692(6) 0.204(6) Uani 1 1 d DU . . F41 F 0.6308(9) 0.3154(8) 1.0259(8) 0.446(12) Uani 1 1 d DU . . F42 F 0.6603(6) 0.3250(8) 0.9343(8) 0.348(9) Uani 1 1 d DU . . F43 F 0.5871(7) 0.3031(5) 0.9487(14) 0.439(12) Uani 1 1 d DU . . C61 C 0.2246(7) 0.2793(10) 1.2920(13) 0.207(7) Uani 1 1 d U . . H61A H 0.2231 0.2894 1.2473 0.249 Uiso 1 1 calc R . . H61B H 0.1915 0.2813 1.3097 0.249 Uiso 1 1 calc R . . Cl1 Cl 0.2581(3) 0.3139(4) 1.3284(6) 0.349(6) Uani 1 1 d U . . Cl2 Cl 0.2465(4) 0.2145(4) 1.2964(7) 0.302(5) Uani 1 1 d U . . Cl3 Cl -0.2535(7) 0.7509(5) 1.1101(11) 0.557(11) Uani 1 1 d U . . Cl4 Cl -0.2726(5) 0.7339(3) 1.0229(8) 0.379(7) Uani 1 1 d U . . 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_1 0.0625(2) 0.0343(2) 0.0498(2) -0.00534(18) -0.0028(2) 0.00653(18) C1_1 0.056(5) 0.029(3) 0.055(5) 0.012(4) 0.009(4) 0.001(4) N2_1 0.052(4) 0.037(4) 0.071(5) -0.007(4) 0.014(4) -0.002(3) C3_1 0.067(8) 0.032(5) 0.147(10) -0.016(6) 0.005(6) 0.007(5) C4_1 0.066(7) 0.033(4) 0.132(10) 0.031(5) 0.009(6) -0.003(5) N5_1 0.044(4) 0.047(4) 0.087(5) 0.022(4) 0.007(4) 0.005(4) C11_1 0.066(5) 0.047(6) 0.061(5) -0.019(4) 0.007(4) -0.003(4) C12_1 0.062(5) 0.066(7) 0.091(7) -0.029(5) 0.002(4) -0.004(5) C13_1 0.076(7) 0.117(12) 0.118(9) -0.033(8) -0.007(6) -0.001(8) C14_1 0.106(7) 0.107(10) 0.104(8) -0.026(8) -0.045(8) 0.004(8) C15_1 0.112(7) 0.089(8) 0.060(7) -0.008(6) -0.019(6) -0.018(7) C16_1 0.078(5) 0.064(7) 0.063(6) -0.009(5) -0.003(4) -0.004(5) C17_1 0.075(8) 0.116(10) 0.104(8) -0.032(6) 0.030(6) -0.027(7) C19_1 0.085(6) 0.055(6) 0.070(7) -0.004(5) 0.012(5) -0.011(6) C21_1 0.052(5) 0.064(6) 0.080(5) 0.034(5) 0.001(4) 0.014(5) C22_1 0.063(5) 0.046(6) 0.090(6) 0.007(5) 0.011(4) -0.003(5) C23_1 0.070(7) 0.100(10) 0.110(7) 0.013(9) -0.018(5) 0.011(7) C24_1 0.114(8) 0.152(15) 0.086(7) 0.030(10) -0.029(7) -0.027(10) C25_1 0.113(8) 0.153(14) 0.065(6) 0.063(7) -0.014(6) -0.007(9) C26_1 0.075(6) 0.107(10) 0.074(6) 0.044(7) 0.007(5) -0.003(6) C27_1 0.085(7) 0.082(8) 0.111(7) 0.001(7) 0.039(7) -0.020(6) C29_1 0.086(7) 0.156(12) 0.095(10) 0.029(9) 0.023(7) -0.020(8) C171_1 0.41(3) 0.280(15) 0.111(14) -0.100(11) 0.110(16) -0.274(16) C172_1 0.162(16) 0.124(12) 0.149(13) -0.018(10) 0.072(12) 0.024(11) C191_1 0.131(12) 0.117(10) 0.154(14) -0.069(10) 0.054(10) -0.001(10) C192_1 0.114(10) 0.066(6) 0.077(9) -0.007(6) 0.025(8) -0.014(6) C271_1 0.175(12) 0.139(12) 0.165(16) 0.068(11) 0.097(11) 0.086(10) C272_1 0.157(15) 0.117(10) 0.132(13) 0.067(10) 0.038(11) 0.043(10) C291_1 0.157(16) 0.317(18) 0.174(17) 0.121(15) -0.001(13) -0.128(14) C292_1 0.081(9) 0.241(16) 0.128(13) -0.052(12) 0.045(10) 0.014(10) C31_1 0.063(6) 0.045(4) 0.061(7) -0.017(5) -0.024(6) 0.006(5) C32_1 0.092(8) 0.048(4) 0.097(9) -0.027(6) -0.043(7) 0.008(5) C33_1 0.096(8) 0.044(4) 0.061(6) -0.019(4) -0.033(5) 0.001(5) N34_1 0.099(6) 0.033(4) 0.059(5) -0.003(4) -0.028(4) 0.011(4) C35_1 0.141(10) 0.043(5) 0.059(6) -0.014(5) -0.025(6) 0.028(6) C36_1 0.171(15) 0.063(7) 0.224(17) 0.010(8) 0.111(13) 0.041(10) C37_1 0.197(17) 0.086(8) 0.074(8) -0.008(6) 0.017(8) 0.022(10) C38_1 0.085(9) 0.050(6) 0.121(9) -0.006(6) 0.022(7) 0.005(6) O39_1 0.129(7) 0.063(5) 0.068(5) -0.002(4) -0.013(5) -0.004(5) C39_1 0.140(14) 0.119(13) 0.107(9) -0.044(9) 0.029(9) -0.027(11) Au1_2 0.0342(2) 0.0568(2) 0.0551(3) 0.0000(2) 0.00582(18) -0.01138(17) C1_2 0.039(4) 0.045(5) 0.048(5) 0.000(4) -0.003(4) -0.007(4) N2_2 0.030(4) 0.046(4) 0.058(5) -0.003(3) 0.004(3) -0.007(3) C3_2 0.032(5) 0.065(7) 0.076(7) -0.001(5) 0.009(4) -0.009(4) C4_2 0.031(5) 0.069(7) 0.099(8) -0.007(6) 0.001(5) -0.013(5) N5_2 0.043(4) 0.047(4) 0.069(5) -0.004(4) -0.005(4) -0.007(3) C11_2 0.042(5) 0.051(4) 0.055(5) 0.003(4) 0.006(4) -0.015(4) C12_2 0.041(6) 0.073(5) 0.064(6) 0.004(4) -0.004(4) -0.001(5) C13_2 0.088(8) 0.094(6) 0.061(7) -0.017(5) -0.009(6) 0.013(7) C14_2 0.100(10) 0.083(6) 0.127(10) -0.030(7) -0.046(8) 0.011(8) C15_2 0.084(9) 0.049(6) 0.109(9) -0.010(6) -0.015(7) 0.009(6) C16_2 0.050(6) 0.046(5) 0.080(6) 0.005(4) 0.003(5) 0.001(4) C17_2 0.061(6) 0.094(6) 0.079(7) 0.013(6) -0.006(6) 0.025(6) C19_2 0.053(6) 0.067(7) 0.070(6) 0.011(5) 0.009(4) -0.008(5) C21_2 0.050(5) 0.061(5) 0.066(5) -0.009(4) -0.018(5) -0.021(4) C22_2 0.057(6) 0.067(5) 0.060(5) -0.003(4) -0.007(5) -0.009(5) C23_2 0.118(11) 0.096(8) 0.059(6) -0.010(5) -0.024(7) 0.005(7) C24_2 0.087(9) 0.084(7) 0.096(7) -0.033(7) -0.026(8) 0.005(7) C25_2 0.082(9) 0.072(7) 0.097(7) -0.009(5) -0.013(7) -0.007(6) C26_2 0.046(5) 0.053(5) 0.084(6) -0.010(4) -0.010(5) -0.011(4) C27_2 0.108(9) 0.066(6) 0.085(9) 0.001(6) -0.029(6) -0.012(6) C29_2 0.065(6) 0.082(8) 0.083(6) 0.001(6) -0.002(6) 0.006(6) C171_2 0.113(10) 0.108(11) 0.097(9) 0.028(8) 0.033(8) 0.020(9) C172_2 0.070(7) 0.095(9) 0.126(12) 0.041(9) 0.016(8) 0.026(6) C191_2 0.089(9) 0.112(10) 0.103(11) 0.033(8) 0.011(7) 0.037(7) C192_2 0.083(9) 0.155(13) 0.117(9) 0.075(10) 0.041(7) 0.014(9) C271_2 0.103(8) 0.094(11) 0.163(15) 0.011(10) -0.056(9) 0.013(7) C272_2 0.138(11) 0.083(9) 0.112(12) 0.017(8) -0.011(10) -0.024(9) C291_2 0.127(11) 0.146(13) 0.150(14) 0.072(11) 0.014(12) -0.009(10) C292_2 0.068(6) 0.204(17) 0.103(11) 0.055(12) -0.010(7) 0.027(9) C31_2 0.046(4) 0.068(7) 0.075(8) -0.004(6) 0.014(5) -0.005(5) C32_2 0.041(4) 0.071(7) 0.071(7) -0.008(6) 0.014(5) -0.010(5) C33_2 0.057(4) 0.069(7) 0.052(5) -0.009(4) 0.013(4) -0.002(5) N34_2 0.058(4) 0.084(6) 0.056(5) -0.005(4) 0.021(4) 0.004(5) C35_2 0.063(5) 0.117(10) 0.078(8) -0.009(6) -0.003(6) -0.004(7) C36_2 0.088(7) 0.27(2) 0.108(12) 0.079(12) -0.008(8) -0.012(12) C37_2 0.088(9) 0.33(3) 0.137(14) 0.127(14) 0.015(8) 0.043(14) C38_2 0.087(6) 0.123(11) 0.072(8) 0.029(7) 0.021(6) 0.031(8) O39_2 0.061(4) 0.096(6) 0.061(4) 0.001(4) 0.010(3) -0.031(4) C39_2 0.088(9) 0.109(11) 0.079(8) 0.036(8) -0.005(7) -0.012(8) Au1_3 0.0339(2) 0.0674(3) 0.0570(3) 0.0075(2) -0.00917(19) -0.00651(18) C1_3 0.033(4) 0.051(5) 0.056(6) -0.001(4) -0.010(4) 0.006(4) N2_3 0.033(4) 0.077(5) 0.051(5) -0.004(4) -0.003(3) -0.003(4) C3_3 0.029(4) 0.095(8) 0.056(6) -0.022(5) -0.004(4) 0.002(5) C4_3 0.037(4) 0.093(8) 0.068(7) -0.008(6) 0.009(5) -0.012(5) N5_3 0.029(4) 0.066(5) 0.062(5) -0.001(4) 0.002(3) -0.006(3) C11_3 0.034(5) 0.084(5) 0.051(5) 0.005(4) -0.010(4) 0.018(5) C12_3 0.093(9) 0.081(6) 0.069(6) 0.006(4) -0.012(6) 0.020(7) C13_3 0.131(12) 0.073(7) 0.083(8) 0.004(5) -0.004(8) 0.021(8) C14_3 0.201(18) 0.083(6) 0.085(9) 0.033(7) 0.015(9) 0.041(10) C15_3 0.116(11) 0.100(6) 0.070(8) 0.012(6) 0.019(8) 0.040(8) C16_3 0.056(6) 0.088(6) 0.055(5) 0.009(4) -0.003(5) 0.017(5) C17_3 0.119(9) 0.062(7) 0.071(7) -0.010(5) -0.012(6) 0.016(6) C19_3 0.087(7) 0.094(6) 0.053(7) -0.006(5) -0.002(6) 0.018(7) C21_3 0.061(7) 0.064(5) 0.079(5) 0.017(4) 0.012(5) 0.014(5) C22_3 0.061(7) 0.052(5) 0.162(7) 0.002(5) 0.016(7) -0.006(5) C23_3 0.091(11) 0.088(9) 0.208(9) 0.045(7) 0.016(12) 0.048(9) C24_3 0.163(17) 0.155(11) 0.168(9) 0.090(9) 0.065(14) 0.053(13) C25_3 0.174(17) 0.153(10) 0.084(7) 0.059(7) 0.053(10) 0.039(12) C26_3 0.087(9) 0.106(7) 0.067(6) 0.012(5) 0.008(7) 0.016(7) C27_3 0.111(8) 0.092(9) 0.206(9) -0.080(9) -0.066(10) 0.050(7) C29_3 0.211(15) 0.112(8) 0.075(9) 0.010(7) 0.062(10) 0.030(9) C171_3 0.141(10) 0.195(17) 0.134(14) -0.098(13) -0.045(9) 0.081(11) C172_3 0.144(12) 0.183(17) 0.103(12) -0.037(10) -0.030(11) -0.018(12) C191_3 0.123(10) 0.143(13) 0.095(10) -0.042(9) -0.017(8) 0.016(11) C192_3 0.100(8) 0.087(9) 0.105(11) -0.034(8) -0.002(8) 0.027(7) C271_3 0.143(13) 0.24(2) 0.47(4) -0.23(2) -0.02(2) -0.024(13) C272_3 0.141(10) 0.128(13) 0.157(15) -0.087(12) -0.008(10) 0.017(10) C291_3 0.187(14) 0.29(2) 0.045(8) -0.021(11) 0.022(8) 0.110(14) C292_3 0.28(2) 0.113(12) 0.169(19) -0.055(14) 0.048(17) -0.003(12) C31_3 0.041(4) 0.085(8) 0.104(10) 0.025(8) -0.024(7) -0.013(5) C32_3 0.046(4) 0.112(9) 0.125(11) 0.055(9) -0.032(6) -0.022(6) C33_3 0.050(5) 0.119(9) 0.068(6) 0.038(5) -0.025(5) -0.010(6) N34_3 0.033(4) 0.147(9) 0.073(6) 0.030(5) -0.014(4) -0.016(5) C35_3 0.040(5) 0.128(11) 0.127(11) 0.006(8) -0.013(6) -0.020(7) C36_3 0.067(8) 0.25(2) 0.23(2) -0.106(15) 0.003(9) -0.044(11) C37_3 0.109(10) 0.170(16) 0.126(11) -0.032(10) -0.004(7) -0.068(11) C38_3 0.041(6) 0.218(19) 0.111(10) -0.024(10) -0.031(6) 0.005(8) O39_3 0.073(5) 0.134(8) 0.076(6) 0.023(5) -0.020(4) -0.003(5) C39_3 0.151(16) 0.163(17) 0.143(13) -0.052(12) -0.059(11) -0.011(14) Au1_4 0.0723(3) 0.0399(2) 0.0588(3) -0.0085(2) -0.0048(3) 0.0162(2) C1_4 0.047(5) 0.042(4) 0.064(6) -0.002(4) 0.006(4) 0.010(4) N2_4 0.050(4) 0.042(4) 0.092(6) 0.005(4) 0.000(4) 0.007(3) C3_4 0.054(6) 0.033(5) 0.150(11) 0.004(5) -0.006(6) 0.010(5) C4_4 0.050(6) 0.039(5) 0.120(9) -0.017(5) 0.004(5) 0.009(4) N5_4 0.051(4) 0.029(4) 0.079(5) -0.011(3) 0.007(4) 0.007(3) C11_4 0.070(6) 0.044(6) 0.099(6) 0.032(5) -0.016(5) 0.000(5) C12_4 0.078(6) 0.048(6) 0.119(7) -0.009(6) -0.007(5) -0.008(5) C13_4 0.078(8) 0.084(10) 0.170(8) 0.023(10) -0.028(7) -0.023(7) C14_4 0.109(9) 0.118(13) 0.143(8) 0.038(11) -0.066(8) -0.025(9) C15_4 0.126(9) 0.105(11) 0.122(8) 0.065(9) -0.059(7) -0.043(8) C16_4 0.077(6) 0.086(8) 0.095(6) 0.038(7) -0.030(5) -0.007(6) C17_4 0.098(9) 0.101(8) 0.147(8) -0.010(9) 0.050(8) -0.010(8) C19_4 0.082(8) 0.136(10) 0.099(11) 0.033(8) -0.013(6) -0.015(7) C21_4 0.077(5) 0.043(6) 0.068(6) 0.002(5) -0.015(4) 0.005(5) C22_4 0.072(5) 0.050(6) 0.091(7) -0.009(5) -0.004(5) 0.019(5) C23_4 0.088(7) 0.086(9) 0.123(10) -0.018(7) -0.038(7) 0.012(7) C24_4 0.152(8) 0.126(14) 0.124(11) 0.016(9) -0.078(10) -0.001(11) C25_4 0.171(8) 0.133(13) 0.077(10) 0.032(9) -0.045(8) -0.017(12) C26_4 0.106(6) 0.054(7) 0.065(7) -0.015(5) 0.002(5) -0.005(6) C27_4 0.066(7) 0.066(8) 0.098(8) -0.016(5) 0.013(6) 0.011(5) C29_4 0.121(7) 0.070(7) 0.107(9) -0.017(7) 0.049(7) 0.006(7) C171_4 0.085(11) 0.182(13) 0.231(19) -0.045(17) 0.059(12) 0.011(11) C172_4 0.141(14) 0.110(8) 0.133(14) 0.007(9) 0.047(12) -0.047(9) C191_4 0.134(14) 0.206(11) 0.31(3) 0.177(14) -0.089(15) -0.084(10) C192_4 0.151(13) 0.268(16) 0.20(2) -0.151(16) 0.064(13) -0.089(12) C271_4 0.084(9) 0.089(9) 0.118(11) -0.042(7) 0.022(8) -0.010(6) C272_4 0.145(14) 0.129(12) 0.119(10) -0.064(9) 0.036(10) -0.036(11) C291_4 0.28(2) 0.160(13) 0.209(15) -0.118(13) 0.169(15) -0.091(16) C292_4 0.149(13) 0.081(7) 0.134(14) -0.023(8) 0.076(12) -0.037(8) C31_4 0.087(8) 0.049(4) 0.100(10) -0.026(7) -0.031(8) 0.023(6) C32_4 0.105(9) 0.047(4) 0.164(14) -0.023(6) -0.064(10) 0.028(6) C33_4 0.118(10) 0.045(5) 0.105(8) -0.008(5) -0.051(6) 0.009(6) N34_4 0.127(9) 0.041(4) 0.108(7) -0.029(4) -0.051(5) 0.015(5) C35_4 0.34(3) 0.037(6) 0.205(17) -0.014(8) 0.001(15) 0.012(11) C36_4 0.55(5) 0.081(8) 0.34(3) -0.022(11) 0.15(3) -0.097(18) C37_4 0.47(4) 0.113(12) 0.29(2) 0.034(12) 0.16(2) -0.01(2) C38_4 0.135(13) 0.096(8) 0.133(12) -0.019(8) -0.021(8) -0.033(9) O39_4 0.134(8) 0.068(6) 0.110(7) -0.029(5) -0.050(5) 0.034(5) C39_4 0.147(15) 0.116(14) 0.122(11) -0.015(9) -0.028(10) -0.011(12) S1 0.101(3) 0.075(2) 0.120(3) 0.004(2) 0.028(2) 0.014(2) O11 0.223(13) 0.110(7) 0.188(10) -0.035(8) 0.062(9) 0.033(9) O12 0.139(9) 0.48(2) 0.116(8) 0.073(10) -0.033(7) -0.113(13) O13 0.233(14) 0.075(6) 0.214(13) 0.052(7) 0.066(10) -0.001(7) C51 0.147(8) 0.174(10) 0.041(7) 0.002(6) -0.001(5) -0.092(9) F11 0.180(9) 0.356(12) 0.165(8) -0.127(10) 0.099(7) -0.149(10) F12 0.110(6) 0.310(15) 0.164(9) -0.002(9) -0.027(7) -0.009(9) F13 0.196(12) 0.190(8) 0.266(16) 0.083(8) -0.005(10) -0.093(8) S2 0.221(6) 0.334(8) 0.156(5) 0.020(5) -0.054(5) -0.189(5) O21 0.305(12) 0.255(18) 0.51(4) -0.162(15) -0.038(17) -0.038(11) O22 0.233(17) 0.241(13) 0.161(10) 0.005(9) -0.059(11) -0.012(11) O23 0.324(14) 0.315(15) 0.199(13) 0.149(10) -0.157(12) -0.205(13) C52 0.336(15) 0.167(14) 0.120(8) -0.045(6) 0.097(12) -0.119(8) F21 0.469(15) 0.291(19) 0.55(3) -0.203(15) -0.12(2) 0.133(15) F22 0.355(18) 0.210(12) 0.129(7) -0.039(8) -0.013(11) -0.096(11) F23 0.535(16) 0.49(2) 0.195(14) 0.049(13) -0.025(16) -0.400(16) S3 0.123(3) 0.076(2) 0.095(3) -0.008(2) -0.028(2) 0.021(2) O31 0.160(9) 0.138(8) 0.192(13) 0.011(7) -0.008(10) 0.065(8) O32 0.204(14) 0.291(15) 0.183(9) -0.154(10) -0.028(11) -0.014(12) O33 0.238(15) 0.205(13) 0.195(9) 0.097(10) 0.061(12) 0.020(11) C53 0.131(7) 0.149(13) 0.127(11) -0.051(8) 0.006(10) -0.003(7) F31 0.126(7) 0.357(14) 0.48(2) -0.178(12) -0.063(14) 0.110(11) F32 0.158(10) 0.359(17) 0.117(7) -0.099(9) 0.004(7) -0.066(10) F33 0.279(15) 0.370(16) 0.160(8) 0.024(11) 0.119(11) -0.090(11) S4 0.084(3) 0.120(3) 0.166(4) -0.017(3) 0.004(3) -0.034(2) O41 0.212(16) 0.57(3) 0.236(8) 0.265(15) -0.090(9) -0.151(15) O42 0.084(7) 0.45(2) 0.264(11) -0.243(13) 0.054(8) -0.010(9) O43 0.080(8) 0.310(13) 0.50(3) -0.19(2) -0.021(11) -0.039(10) C54 0.263(14) 0.217(9) 0.131(11) -0.099(10) -0.028(11) 0.102(9) F41 0.64(3) 0.45(2) 0.252(13) 0.194(16) 0.040(13) 0.20(2) F42 0.332(13) 0.48(2) 0.231(14) -0.090(16) 0.055(13) 0.213(14) F43 0.423(17) 0.145(10) 0.75(4) -0.213(19) -0.05(2) 0.017(14) C61 0.133(15) 0.294(13) 0.19(2) 0.040(17) 0.069(15) -0.040(12) Cl1 0.228(8) 0.388(9) 0.431(13) -0.206(10) -0.120(8) 0.141(8) Cl2 0.256(9) 0.304(8) 0.348(13) -0.004(10) 0.034(10) 0.025(8) Cl3 0.88(3) 0.307(14) 0.486(13) 0.139(11) -0.334(16) -0.116(16) Cl4 0.493(15) 0.174(7) 0.469(13) 0.035(10) -0.162(14) 0.003(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1_1 C31_1 1.977(7) . ? Au1_1 C1_1 2.013(7) . ? C1_1 N2_1 1.345(9) . ? C1_1 N5_1 1.362(9) . ? N2_1 C3_1 1.392(9) . ? N2_1 C11_1 1.444(9) . ? C3_1 C4_1 1.322(12) . ? C3_1 H3_1 0.9500 . ? C4_1 N5_1 1.378(10) . ? C4_1 H4_1 0.9500 . ? N5_1 C21_1 1.447(9) . ? C11_1 C16_1 1.362(10) . ? C11_1 C12_1 1.384(9) . ? C12_1 C13_1 1.392(11) . ? C12_1 C17_1 1.525(11) . ? C13_1 C14_1 1.375(12) . ? C13_1 H13_1 0.9500 . ? C14_1 C15_1 1.354(11) . ? C14_1 H14_1 0.9500 . ? C15_1 C16_1 1.379(10) . ? C15_1 H15_1 0.9500 . ? C16_1 C19_1 1.519(10) . ? C17_1 C172_1 1.498(11) . ? C17_1 C171_1 1.498(11) . ? C17_1 H17_1 1.0000 . ? C19_1 C191_1 1.513(11) . ? C19_1 C192_1 1.538(10) . ? C19_1 H19_1 1.0000 . ? C21_1 C22_1 1.383(9) . ? C21_1 C26_1 1.386(10) . ? C22_1 C23_1 1.388(10) . ? C22_1 C27_1 1.516(10) . ? C23_1 C24_1 1.355(11) . ? C23_1 H23_1 0.9500 . ? C24_1 C25_1 1.375(11) . ? C24_1 H24_1 0.9500 . ? C25_1 C26_1 1.393(11) . ? C25_1 H25_1 0.9500 . ? C26_1 C29_1 1.522(11) . ? C27_1 C272_1 1.505(11) . ? C27_1 C271_1 1.541(11) . ? C27_1 H27_1 1.0000 . ? C29_1 C291_1 1.523(12) . ? C29_1 C292_1 1.528(12) . ? C29_1 H29_1 1.0000 . ? C171_1 H17A_1 0.9800 . ? C171_1 H17B_1 0.9800 . ? C171_1 H17C_1 0.9800 . ? C172_1 H17D_1 0.9800 . ? C172_1 H17E_1 0.9800 . ? C172_1 H17F_1 0.9800 . ? C191_1 H19A_1 0.9800 . ? C191_1 H19B_1 0.9800 . ? C191_1 H19C_1 0.9800 . ? C192_1 H19D_1 0.9800 . ? C192_1 H19E_1 0.9800 . ? C192_1 H19F_1 0.9800 . ? C271_1 H27A_1 0.9800 . ? C271_1 H27B_1 0.9800 . ? C271_1 H27C_1 0.9800 . ? C272_1 H27D_1 0.9800 . ? C272_1 H27E_1 0.9800 . ? C272_1 H27F_1 0.9800 . ? C291_1 H29A_1 0.9800 . ? C291_1 H29B_1 0.9800 . ? C291_1 H29C_1 0.9800 . ? C292_1 H29D_1 0.9800 . ? C292_1 H29E_1 0.9800 . ? C292_1 H29F_1 0.9800 . ? C31_1 C32_1 1.201(10) . ? C32_1 C33_1 1.442(10) . ? C33_1 N34_1 1.291(10) . ? C33_1 O39_1 1.323(10) . ? N34_1 C38_1 1.444(11) . ? N34_1 C35_1 1.477(10) . ? C35_1 C36_1 1.542(14) . ? C35_1 H35A_1 0.9900 . ? C35_1 H35B_1 0.9900 . ? C36_1 C37_1 1.509(14) . ? C36_1 H36A_1 0.9900 . ? C36_1 H36B_1 0.9900 . ? C37_1 C38_1 1.438(13) . ? C37_1 H37A_1 0.9900 . ? C37_1 H37B_1 0.9900 . ? C38_1 H38A_1 0.9900 . ? C38_1 H38B_1 0.9900 . ? O39_1 C39_1 1.403(12) . ? C39_1 H39A_1 0.9800 . ? C39_1 H39B_1 0.9800 . ? C39_1 H39C_1 0.9800 . ? Au1_2 C31_2 1.979(8) . ? Au1_2 C1_2 2.018(7) . ? C1_2 N2_2 1.348(9) . ? C1_2 N5_2 1.359(8) . ? N2_2 C3_2 1.377(9) . ? N2_2 C11_2 1.451(9) . ? C3_2 C4_2 1.316(11) . ? C3_2 H3_2 0.9500 . ? C4_2 N5_2 1.389(9) . ? C4_2 H4_2 0.9500 . ? N5_2 C21_2 1.446(9) . ? C11_2 C12_2 1.389(9) . ? C11_2 C16_2 1.393(9) . ? C12_2 C13_2 1.394(10) . ? C12_2 C17_2 1.516(10) . ? C13_2 C14_2 1.378(11) . ? C13_2 H13_2 0.9500 . ? C14_2 C15_2 1.377(11) . ? C14_2 H14_2 0.9500 . ? C15_2 C16_2 1.393(10) . ? C15_2 H15_2 0.9500 . ? C16_2 C19_2 1.509(10) . ? C17_2 C171_2 1.510(11) . ? C17_2 C172_2 1.527(10) . ? C17_2 H17_2 1.0000 . ? C19_2 C192_2 1.503(10) . ? C19_2 C191_2 1.521(11) . ? C19_2 H19_2 1.0000 . ? C21_2 C22_2 1.385(9) . ? C21_2 C26_2 1.388(9) . ? C22_2 C23_2 1.388(10) . ? C22_2 C27_2 1.524(10) . ? C23_2 C24_2 1.371(11) . ? C23_2 H23_2 0.9500 . ? C24_2 C25_2 1.372(11) . ? C24_2 H24_2 0.9500 . ? C25_2 C26_2 1.380(10) . ? C25_2 H25_2 0.9500 . ? C26_2 C29_2 1.521(10) . ? C27_2 C272_2 1.533(11) . ? C27_2 C271_2 1.533(11) . ? C27_2 H27_2 1.0000 . ? C29_2 C292_2 1.502(11) . ? C29_2 C291_2 1.542(11) . ? C29_2 H29_2 1.0000 . ? C171_2 H17A_2 0.9800 . ? C171_2 H17B_2 0.9800 . ? C171_2 H17C_2 0.9800 . ? C172_2 H17D_2 0.9800 . ? C172_2 H17E_2 0.9800 . ? C172_2 H17F_2 0.9800 . ? C191_2 H19A_2 0.9800 . ? C191_2 H19B_2 0.9800 . ? C191_2 H19C_2 0.9800 . ? C192_2 H19D_2 0.9800 . ? C192_2 H19E_2 0.9800 . ? C192_2 H19F_2 0.9800 . ? C271_2 H27A_2 0.9800 . ? C271_2 H27B_2 0.9800 . ? C271_2 H27C_2 0.9800 . ? C272_2 H27D_2 0.9800 . ? C272_2 H27E_2 0.9800 . ? C272_2 H27F_2 0.9800 . ? C291_2 H29A_2 0.9800 . ? C291_2 H29B_2 0.9800 . ? C291_2 H29C_2 0.9800 . ? C292_2 H29D_2 0.9800 . ? C292_2 H29E_2 0.9800 . ? C292_2 H29F_2 0.9800 . ? C31_2 C32_2 1.195(10) . ? C32_2 C33_2 1.440(10) . ? C33_2 N34_2 1.268(10) . ? C33_2 O39_2 1.323(9) . ? N34_2 C38_2 1.454(11) . ? N34_2 C35_2 1.477(10) . ? C35_2 C36_2 1.533(14) . ? C35_2 H35A_2 0.9900 . ? C35_2 H35B_2 0.9900 . ? C36_2 C37_2 1.487(14) . ? C36_2 H36A_2 0.9900 . ? C36_2 H36B_2 0.9900 . ? C37_2 C38_2 1.420(13) . ? C37_2 H37A_2 0.9900 . ? C37_2 H37B_2 0.9900 . ? C38_2 H38A_2 0.9900 . ? C38_2 H38B_2 0.9900 . ? O39_2 C39_2 1.412(11) . ? C39_2 H39A_2 0.9800 . ? C39_2 H39B_2 0.9800 . ? C39_2 H39C_2 0.9800 . ? Au1_3 C31_3 1.985(7) . ? Au1_3 C1_3 2.015(7) . ? C1_3 N2_3 1.334(9) . ? C1_3 N5_3 1.354(9) . ? N2_3 C3_3 1.416(9) . ? N2_3 C11_3 1.442(9) . ? C3_3 C4_3 1.311(11) . ? C3_3 H3_3 0.9500 . ? C4_3 N5_3 1.373(9) . ? C4_3 H4_3 0.9500 . ? N5_3 C21_3 1.444(9) . ? C11_3 C12_3 1.376(10) . ? C11_3 C16_3 1.388(9) . ? C12_3 C13_3 1.377(11) . ? C12_3 C17_3 1.538(10) . ? C13_3 C14_3 1.357(11) . ? C13_3 H13_3 0.9500 . ? C14_3 C15_3 1.394(11) . ? C14_3 H14_3 0.9500 . ? C15_3 C16_3 1.393(11) . ? C15_3 H15_3 0.9500 . ? C16_3 C19_3 1.515(10) . ? C17_3 C172_3 1.496(11) . ? C17_3 C171_3 1.503(11) . ? C17_3 H17_3 1.0000 . ? C19_3 C192_3 1.502(11) . ? C19_3 C191_3 1.523(11) . ? C19_3 H19_3 1.0000 . ? C21_3 C22_3 1.386(10) . ? C21_3 C26_3 1.395(10) . ? C22_3 C23_3 1.386(11) . ? C22_3 C27_3 1.519(11) . ? C23_3 C24_3 1.362(12) . ? C23_3 H23_3 0.9500 . ? C24_3 C25_3 1.363(12) . ? C24_3 H24_3 0.9500 . ? C25_3 C26_3 1.401(11) . ? C25_3 H25_3 0.9500 . ? C26_3 C29_3 1.527(11) . ? C27_3 C272_3 1.484(11) . ? C27_3 C271_3 1.489(12) . ? C27_3 H27_3 1.0000 . ? C29_3 C291_3 1.528(11) . ? C29_3 C292_3 1.532(13) . ? C29_3 H29_3 1.0000 . ? C171_3 H17A_3 0.9800 . ? C171_3 H17B_3 0.9800 . ? C171_3 H17C_3 0.9800 . ? C172_3 H17D_3 0.9800 . ? C172_3 H17E_3 0.9800 . ? C172_3 H17F_3 0.9800 . ? C191_3 H19A_3 0.9800 . ? C191_3 H19B_3 0.9800 . ? C191_3 H19C_3 0.9800 . ? C192_3 H19D_3 0.9800 . ? C192_3 H19E_3 0.9800 . ? C192_3 H19F_3 0.9800 . ? C271_3 H27A_3 0.9800 . ? C271_3 H27B_3 0.9800 . ? C271_3 H27C_3 0.9800 . ? C272_3 H27D_3 0.9800 . ? C272_3 H27E_3 0.9800 . ? C272_3 H27F_3 0.9800 . ? C291_3 H29A_3 0.9800 . ? C291_3 H29B_3 0.9800 . ? C291_3 H29C_3 0.9800 . ? C292_3 H29D_3 0.9800 . ? C292_3 H29E_3 0.9800 . ? C292_3 H29F_3 0.9800 . ? C31_3 C32_3 1.199(10) . ? C32_3 C33_3 1.441(10) . ? C33_3 N34_3 1.275(11) . ? C33_3 O39_3 1.319(11) . ? N34_3 C38_3 1.446(12) . ? N34_3 C35_3 1.489(10) . ? C35_3 C36_3 1.544(14) . ? C35_3 H35A_3 0.9900 . ? C35_3 H35B_3 0.9900 . ? C36_3 C37_3 1.522(15) . ? C36_3 H36A_3 0.9900 . ? C36_3 H36B_3 0.9900 . ? C37_3 C38_3 1.418(13) . ? C37_3 H37A_3 0.9900 . ? C37_3 H37B_3 0.9900 . ? C38_3 H38A_3 0.9900 . ? C38_3 H38B_3 0.9900 . ? O39_3 C39_3 1.406(12) . ? C39_3 H39A_3 0.9800 . ? C39_3 H39B_3 0.9800 . ? C39_3 H39C_3 0.9800 . ? Au1_4 C31_4 1.973(8) . ? Au1_4 C1_4 2.021(7) . ? C1_4 N5_4 1.339(9) . ? C1_4 N2_4 1.343(9) . ? N2_4 C3_4 1.378(10) . ? N2_4 C11_4 1.437(9) . ? C3_4 C4_4 1.311(12) . ? C3_4 H3_4 0.9500 . ? C4_4 N5_4 1.400(9) . ? C4_4 H4_4 0.9500 . ? N5_4 C21_4 1.428(9) . ? C11_4 C12_4 1.374(10) . ? C11_4 C16_4 1.380(10) . ? C12_4 C13_4 1.379(11) . ? C12_4 C17_4 1.525(11) . ? C13_4 C14_4 1.370(12) . ? C13_4 H13_4 0.9500 . ? C14_4 C15_4 1.366(11) . ? C14_4 H14_4 0.9500 . ? C15_4 C16_4 1.386(11) . ? C15_4 H15_4 0.9500 . ? C16_4 C19_4 1.530(11) . ? C17_4 C172_4 1.503(11) . ? C17_4 C171_4 1.513(11) . ? C17_4 H17_4 1.0000 . ? C19_4 C192_4 1.512(12) . ? C19_4 C191_4 1.529(12) . ? C19_4 H19_4 1.0000 . ? C21_4 C26_4 1.390(10) . ? C21_4 C22_4 1.393(10) . ? C22_4 C23_4 1.380(11) . ? C22_4 C27_4 1.523(10) . ? C23_4 C24_4 1.368(12) . ? C23_4 H23_4 0.9500 . ? C24_4 C25_4 1.369(12) . ? C24_4 H24_4 0.9500 . ? C25_4 C26_4 1.392(11) . ? C25_4 H25_4 0.9500 . ? C26_4 C29_4 1.529(11) . ? C27_4 C272_4 1.517(11) . ? C27_4 C271_4 1.536(11) . ? C27_4 H27_4 1.0000 . ? C29_4 C292_4 1.524(11) . ? C29_4 C291_4 1.526(12) . ? C29_4 H29_4 1.0000 . ? C171_4 H17A_4 0.9800 . ? C171_4 H17B_4 0.9800 . ? C171_4 H17C_4 0.9800 . ? C172_4 H17D_4 0.9800 . ? C172_4 H17E_4 0.9800 . ? C172_4 H17F_4 0.9800 . ? C191_4 H19A_4 0.9800 . ? C191_4 H19B_4 0.9800 . ? C191_4 H19C_4 0.9800 . ? C192_4 H19D_4 0.9800 . ? C192_4 H19E_4 0.9800 . ? C192_4 H19F_4 0.9800 . ? C271_4 H27A_4 0.9800 . ? C271_4 H27B_4 0.9800 . ? C271_4 H27C_4 0.9800 . ? C272_4 H27D_4 0.9800 . ? C272_4 H27E_4 0.9800 . ? C272_4 H27F_4 0.9800 . ? C291_4 H29A_4 0.9800 . ? C291_4 H29B_4 0.9800 . ? C291_4 H29C_4 0.9800 . ? C292_4 H29D_4 0.9800 . ? C292_4 H29E_4 0.9800 . ? C292_4 H29F_4 0.9800 . ? C31_4 C32_4 1.189(10) . ? C32_4 C33_4 1.438(11) . ? C33_4 N34_4 1.268(11) . ? C33_4 O39_4 1.320(11) . ? N34_4 C38_4 1.430(12) . ? N34_4 C35_4 1.481(11) . ? C35_4 C36_4 1.579(16) . ? C35_4 H35A_4 0.9900 . ? C35_4 H35B_4 0.9900 . ? C36_4 C37_4 1.540(16) . ? C36_4 H36A_4 0.9900 . ? C36_4 H36B_4 0.9900 . ? C37_4 C38_4 1.412(15) . ? C37_4 H37A_4 0.9900 . ? C37_4 H37B_4 0.9900 . ? C38_4 H38A_4 0.9900 . ? C38_4 H38B_4 0.9900 . ? O39_4 C39_4 1.414(13) . ? C39_4 H39A_4 0.9800 . ? C39_4 H39B_4 0.9800 . ? C39_4 H39C_4 0.9800 . ? S1 O12 1.388(10) . ? S1 O11 1.398(9) . ? S1 O13 1.399(9) . ? S1 C51 1.683(11) . ? C51 F13 1.290(11) . ? C51 F12 1.328(11) . ? C51 F11 1.332(11) . ? S2 O23 1.305(10) . ? S2 O22 1.459(11) . ? S2 O21 1.468(12) . ? S2 C52 1.658(13) . ? C52 F22 1.283(11) . ? C52 F23 1.311(12) . ? C52 F21 1.317(13) . ? S3 O33 1.396(10) . ? S3 O31 1.406(9) . ? S3 O32 1.408(9) . ? S3 C53 1.664(12) . ? C53 F31 1.296(12) . ? C53 F32 1.296(11) . ? C53 F33 1.341(12) . ? S4 O43 1.334(10) . ? S4 O42 1.406(10) . ? S4 O41 1.411(11) . ? S4 C54 1.640(13) . ? C54 F41 1.295(12) . ? C54 F42 1.298(12) . ? C54 F43 1.300(13) . ? C61 Cl1 1.54(3) . ? C61 Cl2 1.89(3) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? Cl3 Cl4 1.98(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C31_1 Au1_1 C1_1 177.5(4) . . ? N2_1 C1_1 N5_1 105.1(6) . . ? N2_1 C1_1 Au1_1 126.1(5) . . ? N5_1 C1_1 Au1_1 128.1(6) . . ? C1_1 N2_1 C3_1 110.0(7) . . ? C1_1 N2_1 C11_1 124.2(7) . . ? C3_1 N2_1 C11_1 125.7(8) . . ? C4_1 C3_1 N2_1 107.3(8) . . ? C4_1 C3_1 H3_1 126.4 . . ? N2_1 C3_1 H3_1 126.4 . . ? C3_1 C4_1 N5_1 107.5(8) . . ? C3_1 C4_1 H4_1 126.3 . . ? N5_1 C4_1 H4_1 126.3 . . ? C1_1 N5_1 C4_1 110.0(7) . . ? C1_1 N5_1 C21_1 125.8(7) . . ? C4_1 N5_1 C21_1 124.0(8) . . ? C16_1 C11_1 C12_1 123.5(8) . . ? C16_1 C11_1 N2_1 117.6(7) . . ? C12_1 C11_1 N2_1 118.9(7) . . ? C11_1 C12_1 C13_1 118.0(9) . . ? C11_1 C12_1 C17_1 123.5(9) . . ? C13_1 C12_1 C17_1 118.5(9) . . ? C14_1 C13_1 C12_1 118.8(10) . . ? C14_1 C13_1 H13_1 120.6 . . ? C12_1 C13_1 H13_1 120.6 . . ? C15_1 C14_1 C13_1 121.0(11) . . ? C15_1 C14_1 H14_1 119.5 . . ? C13_1 C14_1 H14_1 119.5 . . ? C14_1 C15_1 C16_1 121.9(10) . . ? C14_1 C15_1 H15_1 119.0 . . ? C16_1 C15_1 H15_1 119.0 . . ? C11_1 C16_1 C15_1 116.6(8) . . ? C11_1 C16_1 C19_1 122.2(8) . . ? C15_1 C16_1 C19_1 121.1(8) . . ? C172_1 C17_1 C171_1 110.8(11) . . ? C172_1 C17_1 C12_1 115.5(10) . . ? C171_1 C17_1 C12_1 117.2(10) . . ? C172_1 C17_1 H17_1 103.8 . . ? C171_1 C17_1 H17_1 103.8 . . ? C12_1 C17_1 H17_1 103.8 . . ? C191_1 C19_1 C16_1 110.8(9) . . ? C191_1 C19_1 C192_1 109.3(9) . . ? C16_1 C19_1 C192_1 112.1(9) . . ? C191_1 C19_1 H19_1 108.2 . . ? C16_1 C19_1 H19_1 108.2 . . ? C192_1 C19_1 H19_1 108.2 . . ? C22_1 C21_1 C26_1 122.8(8) . . ? C22_1 C21_1 N5_1 119.0(7) . . ? C26_1 C21_1 N5_1 118.2(7) . . ? C21_1 C22_1 C23_1 118.6(8) . . ? C21_1 C22_1 C27_1 121.5(8) . . ? C23_1 C22_1 C27_1 119.7(8) . . ? C24_1 C23_1 C22_1 119.8(10) . . ? C24_1 C23_1 H23_1 120.1 . . ? C22_1 C23_1 H23_1 120.1 . . ? C23_1 C24_1 C25_1 120.8(11) . . ? C23_1 C24_1 H24_1 119.6 . . ? C25_1 C24_1 H24_1 119.6 . . ? C24_1 C25_1 C26_1 121.5(10) . . ? C24_1 C25_1 H25_1 119.2 . . ? C26_1 C25_1 H25_1 119.2 . . ? C21_1 C26_1 C25_1 116.2(8) . . ? C21_1 C26_1 C29_1 124.4(9) . . ? C25_1 C26_1 C29_1 119.4(9) . . ? C272_1 C27_1 C22_1 113.1(10) . . ? C272_1 C27_1 C271_1 108.5(10) . . ? C22_1 C27_1 C271_1 111.4(10) . . ? C272_1 C27_1 H27_1 107.9 . . ? C22_1 C27_1 H27_1 107.9 . . ? C271_1 C27_1 H27_1 107.9 . . ? C26_1 C29_1 C291_1 111.7(10) . . ? C26_1 C29_1 C292_1 112.4(10) . . ? C291_1 C29_1 C292_1 106.3(12) . . ? C26_1 C29_1 H29_1 108.8 . . ? C291_1 C29_1 H29_1 108.8 . . ? C292_1 C29_1 H29_1 108.8 . . ? C17_1 C171_1 H17A_1 109.5 . . ? C17_1 C171_1 H17B_1 109.5 . . ? H17A_1 C171_1 H17B_1 109.5 . . ? C17_1 C171_1 H17C_1 109.5 . . ? H17A_1 C171_1 H17C_1 109.5 . . ? H17B_1 C171_1 H17C_1 109.5 . . ? C17_1 C172_1 H17D_1 109.5 . . ? C17_1 C172_1 H17E_1 109.5 . . ? H17D_1 C172_1 H17E_1 109.5 . . ? C17_1 C172_1 H17F_1 109.5 . . ? H17D_1 C172_1 H17F_1 109.5 . . ? H17E_1 C172_1 H17F_1 109.5 . . ? C19_1 C191_1 H19A_1 109.5 . . ? C19_1 C191_1 H19B_1 109.5 . . ? H19A_1 C191_1 H19B_1 109.5 . . ? C19_1 C191_1 H19C_1 109.5 . . ? H19A_1 C191_1 H19C_1 109.5 . . ? H19B_1 C191_1 H19C_1 109.5 . . ? C19_1 C192_1 H19D_1 109.5 . . ? C19_1 C192_1 H19E_1 109.5 . . ? H19D_1 C192_1 H19E_1 109.5 . . ? C19_1 C192_1 H19F_1 109.5 . . ? H19D_1 C192_1 H19F_1 109.5 . . ? H19E_1 C192_1 H19F_1 109.5 . . ? C27_1 C271_1 H27A_1 109.5 . . ? C27_1 C271_1 H27B_1 109.5 . . ? H27A_1 C271_1 H27B_1 109.5 . . ? C27_1 C271_1 H27C_1 109.5 . . ? H27A_1 C271_1 H27C_1 109.5 . . ? H27B_1 C271_1 H27C_1 109.5 . . ? C27_1 C272_1 H27D_1 109.5 . . ? C27_1 C272_1 H27E_1 109.5 . . ? H27D_1 C272_1 H27E_1 109.5 . . ? C27_1 C272_1 H27F_1 109.5 . . ? H27D_1 C272_1 H27F_1 109.5 . . ? H27E_1 C272_1 H27F_1 109.5 . . ? C29_1 C291_1 H29A_1 109.5 . . ? C29_1 C291_1 H29B_1 109.5 . . ? H29A_1 C291_1 H29B_1 109.5 . . ? C29_1 C291_1 H29C_1 109.5 . . ? H29A_1 C291_1 H29C_1 109.5 . . ? H29B_1 C291_1 H29C_1 109.5 . . ? C29_1 C292_1 H29D_1 109.5 . . ? C29_1 C292_1 H29E_1 109.5 . . ? H29D_1 C292_1 H29E_1 109.5 . . ? C29_1 C292_1 H29F_1 109.5 . . ? H29D_1 C292_1 H29F_1 109.5 . . ? H29E_1 C292_1 H29F_1 109.5 . . ? C32_1 C31_1 Au1_1 177.0(11) . . ? C31_1 C32_1 C33_1 176.0(14) . . ? N34_1 C33_1 O39_1 115.8(8) . . ? N34_1 C33_1 C32_1 117.9(9) . . ? O39_1 C33_1 C32_1 126.3(9) . . ? C33_1 N34_1 C38_1 124.7(7) . . ? C33_1 N34_1 C35_1 118.5(8) . . ? C38_1 N34_1 C35_1 116.4(8) . . ? N34_1 C35_1 C36_1 99.1(8) . . ? N34_1 C35_1 H35A_1 112.0 . . ? C36_1 C35_1 H35A_1 112.0 . . ? N34_1 C35_1 H35B_1 112.0 . . ? C36_1 C35_1 H35B_1 112.0 . . ? H35A_1 C35_1 H35B_1 109.6 . . ? C37_1 C36_1 C35_1 109.5(9) . . ? C37_1 C36_1 H36A_1 109.8 . . ? C35_1 C36_1 H36A_1 109.8 . . ? C37_1 C36_1 H36B_1 109.8 . . ? C35_1 C36_1 H36B_1 109.8 . . ? H36A_1 C36_1 H36B_1 108.2 . . ? C38_1 C37_1 C36_1 107.9(10) . . ? C38_1 C37_1 H37A_1 110.1 . . ? C36_1 C37_1 H37A_1 110.1 . . ? C38_1 C37_1 H37B_1 110.1 . . ? C36_1 C37_1 H37B_1 110.1 . . ? H37A_1 C37_1 H37B_1 108.4 . . ? C37_1 C38_1 N34_1 105.7(8) . . ? C37_1 C38_1 H38A_1 110.6 . . ? N34_1 C38_1 H38A_1 110.6 . . ? C37_1 C38_1 H38B_1 110.6 . . ? N34_1 C38_1 H38B_1 110.6 . . ? H38A_1 C38_1 H38B_1 108.7 . . ? C33_1 O39_1 C39_1 121.1(10) . . ? O39_1 C39_1 H39A_1 109.5 . . ? O39_1 C39_1 H39B_1 109.5 . . ? H39A_1 C39_1 H39B_1 109.5 . . ? O39_1 C39_1 H39C_1 109.5 . . ? H39A_1 C39_1 H39C_1 109.5 . . ? H39B_1 C39_1 H39C_1 109.5 . . ? C31_2 Au1_2 C1_2 176.3(4) . . ? N2_2 C1_2 N5_2 103.5(6) . . ? N2_2 C1_2 Au1_2 128.2(5) . . ? N5_2 C1_2 Au1_2 127.1(5) . . ? C1_2 N2_2 C3_2 112.1(6) . . ? C1_2 N2_2 C11_2 124.6(6) . . ? C3_2 N2_2 C11_2 123.3(7) . . ? C4_2 C3_2 N2_2 106.4(7) . . ? C4_2 C3_2 H3_2 126.8 . . ? N2_2 C3_2 H3_2 126.8 . . ? C3_2 C4_2 N5_2 107.6(7) . . ? C3_2 C4_2 H4_2 126.2 . . ? N5_2 C4_2 H4_2 126.2 . . ? C1_2 N5_2 C4_2 110.4(7) . . ? C1_2 N5_2 C21_2 125.9(7) . . ? C4_2 N5_2 C21_2 123.6(7) . . ? C12_2 C11_2 C16_2 124.4(7) . . ? C12_2 C11_2 N2_2 118.0(7) . . ? C16_2 C11_2 N2_2 117.6(7) . . ? C11_2 C12_2 C13_2 116.9(8) . . ? C11_2 C12_2 C17_2 123.5(8) . . ? C13_2 C12_2 C17_2 119.6(8) . . ? C14_2 C13_2 C12_2 119.6(9) . . ? C14_2 C13_2 H13_2 120.2 . . ? C12_2 C13_2 H13_2 120.2 . . ? C15_2 C14_2 C13_2 122.3(10) . . ? C15_2 C14_2 H14_2 118.8 . . ? C13_2 C14_2 H14_2 118.8 . . ? C14_2 C15_2 C16_2 119.7(9) . . ? C14_2 C15_2 H15_2 120.2 . . ? C16_2 C15_2 H15_2 120.2 . . ? C11_2 C16_2 C15_2 116.5(8) . . ? C11_2 C16_2 C19_2 124.2(8) . . ? C15_2 C16_2 C19_2 119.2(8) . . ? C171_2 C17_2 C12_2 111.6(9) . . ? C171_2 C17_2 C172_2 112.0(10) . . ? C12_2 C17_2 C172_2 111.5(8) . . ? C171_2 C17_2 H17_2 107.1 . . ? C12_2 C17_2 H17_2 107.1 . . ? C172_2 C17_2 H17_2 107.1 . . ? C192_2 C19_2 C16_2 113.8(9) . . ? C192_2 C19_2 C191_2 107.6(9) . . ? C16_2 C19_2 C191_2 112.4(9) . . ? C192_2 C19_2 H19_2 107.6 . . ? C16_2 C19_2 H19_2 107.6 . . ? C191_2 C19_2 H19_2 107.6 . . ? C22_2 C21_2 C26_2 124.3(7) . . ? C22_2 C21_2 N5_2 116.7(7) . . ? C26_2 C21_2 N5_2 118.8(7) . . ? C21_2 C22_2 C23_2 115.8(8) . . ? C21_2 C22_2 C27_2 122.8(8) . . ? C23_2 C22_2 C27_2 121.3(8) . . ? C24_2 C23_2 C22_2 122.1(9) . . ? C24_2 C23_2 H23_2 118.9 . . ? C22_2 C23_2 H23_2 118.9 . . ? C23_2 C24_2 C25_2 119.5(10) . . ? C23_2 C24_2 H24_2 120.3 . . ? C25_2 C24_2 H24_2 120.3 . . ? C24_2 C25_2 C26_2 121.7(10) . . ? C24_2 C25_2 H25_2 119.1 . . ? C26_2 C25_2 H25_2 119.1 . . ? C25_2 C26_2 C21_2 116.5(8) . . ? C25_2 C26_2 C29_2 120.6(8) . . ? C21_2 C26_2 C29_2 122.9(8) . . ? C22_2 C27_2 C272_2 111.4(9) . . ? C22_2 C27_2 C271_2 111.6(9) . . ? C272_2 C27_2 C271_2 111.0(10) . . ? C22_2 C27_2 H27_2 107.6 . . ? C272_2 C27_2 H27_2 107.6 . . ? C271_2 C27_2 H27_2 107.6 . . ? C292_2 C29_2 C26_2 109.7(9) . . ? C292_2 C29_2 C291_2 107.0(10) . . ? C26_2 C29_2 C291_2 112.6(10) . . ? C292_2 C29_2 H29_2 109.1 . . ? C26_2 C29_2 H29_2 109.1 . . ? C291_2 C29_2 H29_2 109.1 . . ? C17_2 C171_2 H17A_2 109.5 . . ? C17_2 C171_2 H17B_2 109.5 . . ? H17A_2 C171_2 H17B_2 109.5 . . ? C17_2 C171_2 H17C_2 109.5 . . ? H17A_2 C171_2 H17C_2 109.5 . . ? H17B_2 C171_2 H17C_2 109.5 . . ? C17_2 C172_2 H17D_2 109.5 . . ? C17_2 C172_2 H17E_2 109.5 . . ? H17D_2 C172_2 H17E_2 109.5 . . ? C17_2 C172_2 H17F_2 109.5 . . ? H17D_2 C172_2 H17F_2 109.5 . . ? H17E_2 C172_2 H17F_2 109.5 . . ? C19_2 C191_2 H19A_2 109.5 . . ? C19_2 C191_2 H19B_2 109.5 . . ? H19A_2 C191_2 H19B_2 109.5 . . ? C19_2 C191_2 H19C_2 109.5 . . ? H19A_2 C191_2 H19C_2 109.5 . . ? H19B_2 C191_2 H19C_2 109.5 . . ? C19_2 C192_2 H19D_2 109.5 . . ? C19_2 C192_2 H19E_2 109.5 . . ? H19D_2 C192_2 H19E_2 109.5 . . ? C19_2 C192_2 H19F_2 109.5 . . ? H19D_2 C192_2 H19F_2 109.5 . . ? H19E_2 C192_2 H19F_2 109.5 . . ? C27_2 C271_2 H27A_2 109.5 . . ? C27_2 C271_2 H27B_2 109.5 . . ? H27A_2 C271_2 H27B_2 109.5 . . ? C27_2 C271_2 H27C_2 109.5 . . ? H27A_2 C271_2 H27C_2 109.5 . . ? H27B_2 C271_2 H27C_2 109.5 . . ? C27_2 C272_2 H27D_2 109.5 . . ? C27_2 C272_2 H27E_2 109.5 . . ? H27D_2 C272_2 H27E_2 109.5 . . ? C27_2 C272_2 H27F_2 109.5 . . ? H27D_2 C272_2 H27F_2 109.5 . . ? H27E_2 C272_2 H27F_2 109.5 . . ? C29_2 C291_2 H29A_2 109.5 . . ? C29_2 C291_2 H29B_2 109.5 . . ? H29A_2 C291_2 H29B_2 109.5 . . ? C29_2 C291_2 H29C_2 109.5 . . ? H29A_2 C291_2 H29C_2 109.5 . . ? H29B_2 C291_2 H29C_2 109.5 . . ? C29_2 C292_2 H29D_2 109.5 . . ? C29_2 C292_2 H29E_2 109.5 . . ? H29D_2 C292_2 H29E_2 109.5 . . ? C29_2 C292_2 H29F_2 109.5 . . ? H29D_2 C292_2 H29F_2 109.5 . . ? H29E_2 C292_2 H29F_2 109.5 . . ? C32_2 C31_2 Au1_2 176.3(11) . . ? C31_2 C32_2 C33_2 175.1(12) . . ? N34_2 C33_2 O39_2 118.9(8) . . ? N34_2 C33_2 C32_2 118.9(8) . . ? O39_2 C33_2 C32_2 122.1(8) . . ? C33_2 N34_2 C38_2 126.0(8) . . ? C33_2 N34_2 C35_2 120.1(8) . . ? C38_2 N34_2 C35_2 113.8(8) . . ? N34_2 C35_2 C36_2 101.7(8) . . ? N34_2 C35_2 H35A_2 111.4 . . ? C36_2 C35_2 H35A_2 111.4 . . ? N34_2 C35_2 H35B_2 111.4 . . ? C36_2 C35_2 H35B_2 111.4 . . ? H35A_2 C35_2 H35B_2 109.3 . . ? C37_2 C36_2 C35_2 106.4(10) . . ? C37_2 C36_2 H36A_2 110.5 . . ? C35_2 C36_2 H36A_2 110.5 . . ? C37_2 C36_2 H36B_2 110.5 . . ? C35_2 C36_2 H36B_2 110.5 . . ? H36A_2 C36_2 H36B_2 108.6 . . ? C38_2 C37_2 C36_2 110.3(11) . . ? C38_2 C37_2 H37A_2 109.6 . . ? C36_2 C37_2 H37A_2 109.6 . . ? C38_2 C37_2 H37B_2 109.6 . . ? C36_2 C37_2 H37B_2 109.6 . . ? H37A_2 C37_2 H37B_2 108.1 . . ? C37_2 C38_2 N34_2 105.0(10) . . ? C37_2 C38_2 H38A_2 110.8 . . ? N34_2 C38_2 H38A_2 110.8 . . ? C37_2 C38_2 H38B_2 110.8 . . ? N34_2 C38_2 H38B_2 110.8 . . ? H38A_2 C38_2 H38B_2 108.8 . . ? C33_2 O39_2 C39_2 121.4(8) . . ? O39_2 C39_2 H39A_2 109.5 . . ? O39_2 C39_2 H39B_2 109.5 . . ? H39A_2 C39_2 H39B_2 109.5 . . ? O39_2 C39_2 H39C_2 109.5 . . ? H39A_2 C39_2 H39C_2 109.5 . . ? H39B_2 C39_2 H39C_2 109.5 . . ? C31_3 Au1_3 C1_3 174.4(5) . . ? N2_3 C1_3 N5_3 105.4(6) . . ? N2_3 C1_3 Au1_3 126.2(6) . . ? N5_3 C1_3 Au1_3 128.3(5) . . ? C1_3 N2_3 C3_3 109.0(7) . . ? C1_3 N2_3 C11_3 125.7(7) . . ? C3_3 N2_3 C11_3 125.3(7) . . ? C4_3 C3_3 N2_3 107.5(7) . . ? C4_3 C3_3 H3_3 126.2 . . ? N2_3 C3_3 H3_3 126.2 . . ? C3_3 C4_3 N5_3 106.9(8) . . ? C3_3 C4_3 H4_3 126.6 . . ? N5_3 C4_3 H4_3 126.6 . . ? C1_3 N5_3 C4_3 111.0(7) . . ? C1_3 N5_3 C21_3 126.6(7) . . ? C4_3 N5_3 C21_3 122.3(8) . . ? C12_3 C11_3 C16_3 123.1(8) . . ? C12_3 C11_3 N2_3 119.0(7) . . ? C16_3 C11_3 N2_3 117.8(7) . . ? C11_3 C12_3 C13_3 119.1(8) . . ? C11_3 C12_3 C17_3 121.2(8) . . ? C13_3 C12_3 C17_3 118.9(9) . . ? C14_3 C13_3 C12_3 119.8(10) . . ? C14_3 C13_3 H13_3 120.1 . . ? C12_3 C13_3 H13_3 120.1 . . ? C13_3 C14_3 C15_3 119.4(11) . . ? C13_3 C14_3 H14_3 120.3 . . ? C15_3 C14_3 H14_3 120.3 . . ? C16_3 C15_3 C14_3 122.2(10) . . ? C16_3 C15_3 H15_3 118.9 . . ? C14_3 C15_3 H15_3 118.9 . . ? C11_3 C16_3 C15_3 115.3(8) . . ? C11_3 C16_3 C19_3 124.1(8) . . ? C15_3 C16_3 C19_3 120.4(8) . . ? C172_3 C17_3 C171_3 112.5(10) . . ? C172_3 C17_3 C12_3 111.1(10) . . ? C171_3 C17_3 C12_3 111.5(10) . . ? C172_3 C17_3 H17_3 107.1 . . ? C171_3 C17_3 H17_3 107.1 . . ? C12_3 C17_3 H17_3 107.1 . . ? C192_3 C19_3 C16_3 110.1(9) . . ? C192_3 C19_3 C191_3 112.6(10) . . ? C16_3 C19_3 C191_3 112.9(9) . . ? C192_3 C19_3 H19_3 107.0 . . ? C16_3 C19_3 H19_3 107.0 . . ? C191_3 C19_3 H19_3 107.0 . . ? C22_3 C21_3 C26_3 124.5(8) . . ? C22_3 C21_3 N5_3 117.8(8) . . ? C26_3 C21_3 N5_3 117.4(7) . . ? C23_3 C22_3 C21_3 115.7(9) . . ? C23_3 C22_3 C27_3 122.5(9) . . ? C21_3 C22_3 C27_3 121.6(9) . . ? C24_3 C23_3 C22_3 120.9(11) . . ? C24_3 C23_3 H23_3 119.5 . . ? C22_3 C23_3 H23_3 119.5 . . ? C23_3 C24_3 C25_3 122.9(13) . . ? C23_3 C24_3 H24_3 118.5 . . ? C25_3 C24_3 H24_3 118.5 . . ? C24_3 C25_3 C26_3 118.9(11) . . ? C24_3 C25_3 H25_3 120.6 . . ? C26_3 C25_3 H25_3 120.6 . . ? C21_3 C26_3 C25_3 116.9(9) . . ? C21_3 C26_3 C29_3 122.6(9) . . ? C25_3 C26_3 C29_3 120.5(9) . . ? C272_3 C27_3 C271_3 116.0(11) . . ? C272_3 C27_3 C22_3 111.8(10) . . ? C271_3 C27_3 C22_3 116.0(14) . . ? C272_3 C27_3 H27_3 103.7 . . ? C271_3 C27_3 H27_3 103.7 . . ? C22_3 C27_3 H27_3 103.7 . . ? C26_3 C29_3 C291_3 109.3(10) . . ? C26_3 C29_3 C292_3 110.0(11) . . ? C291_3 C29_3 C292_3 107.4(12) . . ? C26_3 C29_3 H29_3 110.0 . . ? C291_3 C29_3 H29_3 110.0 . . ? C292_3 C29_3 H29_3 110.0 . . ? C17_3 C171_3 H17A_3 109.5 . . ? C17_3 C171_3 H17B_3 109.5 . . ? H17A_3 C171_3 H17B_3 109.5 . . ? C17_3 C171_3 H17C_3 109.5 . . ? H17A_3 C171_3 H17C_3 109.5 . . ? H17B_3 C171_3 H17C_3 109.5 . . ? C17_3 C172_3 H17D_3 109.5 . . ? C17_3 C172_3 H17E_3 109.5 . . ? H17D_3 C172_3 H17E_3 109.5 . . ? C17_3 C172_3 H17F_3 109.5 . . ? H17D_3 C172_3 H17F_3 109.5 . . ? H17E_3 C172_3 H17F_3 109.5 . . ? C19_3 C191_3 H19A_3 109.5 . . ? C19_3 C191_3 H19B_3 109.5 . . ? H19A_3 C191_3 H19B_3 109.5 . . ? C19_3 C191_3 H19C_3 109.5 . . ? H19A_3 C191_3 H19C_3 109.5 . . ? H19B_3 C191_3 H19C_3 109.5 . . ? C19_3 C192_3 H19D_3 109.5 . . ? C19_3 C192_3 H19E_3 109.5 . . ? H19D_3 C192_3 H19E_3 109.5 . . ? C19_3 C192_3 H19F_3 109.5 . . ? H19D_3 C192_3 H19F_3 109.5 . . ? H19E_3 C192_3 H19F_3 109.5 . . ? C27_3 C271_3 H27A_3 109.5 . . ? C27_3 C271_3 H27B_3 109.5 . . ? H27A_3 C271_3 H27B_3 109.5 . . ? C27_3 C271_3 H27C_3 109.5 . . ? H27A_3 C271_3 H27C_3 109.5 . . ? H27B_3 C271_3 H27C_3 109.5 . . ? C27_3 C272_3 H27D_3 109.5 . . ? C27_3 C272_3 H27E_3 109.5 . . ? H27D_3 C272_3 H27E_3 109.5 . . ? C27_3 C272_3 H27F_3 109.5 . . ? H27D_3 C272_3 H27F_3 109.5 . . ? H27E_3 C272_3 H27F_3 109.5 . . ? C29_3 C291_3 H29A_3 109.5 . . ? C29_3 C291_3 H29B_3 109.5 . . ? H29A_3 C291_3 H29B_3 109.5 . . ? C29_3 C291_3 H29C_3 109.5 . . ? H29A_3 C291_3 H29C_3 109.5 . . ? H29B_3 C291_3 H29C_3 109.5 . . ? C29_3 C292_3 H29D_3 109.5 . . ? C29_3 C292_3 H29E_3 109.5 . . ? H29D_3 C292_3 H29E_3 109.5 . . ? C29_3 C292_3 H29F_3 109.5 . . ? H29D_3 C292_3 H29F_3 109.5 . . ? H29E_3 C292_3 H29F_3 109.5 . . ? C32_3 C31_3 Au1_3 179.7(14) . . ? C31_3 C32_3 C33_3 178.1(16) . . ? N34_3 C33_3 O39_3 118.3(8) . . ? N34_3 C33_3 C32_3 118.7(10) . . ? O39_3 C33_3 C32_3 122.8(10) . . ? C33_3 N34_3 C38_3 125.9(8) . . ? C33_3 N34_3 C35_3 117.5(9) . . ? C38_3 N34_3 C35_3 116.6(8) . . ? N34_3 C35_3 C36_3 98.6(9) . . ? N34_3 C35_3 H35A_3 112.0 . . ? C36_3 C35_3 H35A_3 112.0 . . ? N34_3 C35_3 H35B_3 112.0 . . ? C36_3 C35_3 H35B_3 112.0 . . ? H35A_3 C35_3 H35B_3 109.7 . . ? C37_3 C36_3 C35_3 105.4(10) . . ? C37_3 C36_3 H36A_3 110.7 . . ? C35_3 C36_3 H36A_3 110.7 . . ? C37_3 C36_3 H36B_3 110.7 . . ? C35_3 C36_3 H36B_3 110.7 . . ? H36A_3 C36_3 H36B_3 108.8 . . ? C38_3 C37_3 C36_3 109.6(11) . . ? C38_3 C37_3 H37A_3 109.8 . . ? C36_3 C37_3 H37A_3 109.8 . . ? C38_3 C37_3 H37B_3 109.8 . . ? C36_3 C37_3 H37B_3 109.8 . . ? H37A_3 C37_3 H37B_3 108.2 . . ? C37_3 C38_3 N34_3 103.2(9) . . ? C37_3 C38_3 H38A_3 111.1 . . ? N34_3 C38_3 H38A_3 111.1 . . ? C37_3 C38_3 H38B_3 111.1 . . ? N34_3 C38_3 H38B_3 111.1 . . ? H38A_3 C38_3 H38B_3 109.1 . . ? C33_3 O39_3 C39_3 122.6(11) . . ? O39_3 C39_3 H39A_3 109.5 . . ? O39_3 C39_3 H39B_3 109.5 . . ? H39A_3 C39_3 H39B_3 109.5 . . ? O39_3 C39_3 H39C_3 109.5 . . ? H39A_3 C39_3 H39C_3 109.5 . . ? H39B_3 C39_3 H39C_3 109.5 . . ? C31_4 Au1_4 C1_4 175.9(5) . . ? N5_4 C1_4 N2_4 105.2(6) . . ? N5_4 C1_4 Au1_4 126.9(6) . . ? N2_4 C1_4 Au1_4 127.8(6) . . ? C1_4 N2_4 C3_4 110.1(7) . . ? C1_4 N2_4 C11_4 125.7(7) . . ? C3_4 N2_4 C11_4 124.1(8) . . ? C4_4 C3_4 N2_4 108.2(8) . . ? C4_4 C3_4 H3_4 125.9 . . ? N2_4 C3_4 H3_4 125.9 . . ? C3_4 C4_4 N5_4 106.2(8) . . ? C3_4 C4_4 H4_4 126.9 . . ? N5_4 C4_4 H4_4 126.9 . . ? C1_4 N5_4 C4_4 110.3(7) . . ? C1_4 N5_4 C21_4 125.2(7) . . ? C4_4 N5_4 C21_4 124.4(8) . . ? C12_4 C11_4 C16_4 123.2(8) . . ? C12_4 C11_4 N2_4 119.0(8) . . ? C16_4 C11_4 N2_4 117.5(8) . . ? C11_4 C12_4 C13_4 117.7(9) . . ? C11_4 C12_4 C17_4 121.4(9) . . ? C13_4 C12_4 C17_4 120.6(9) . . ? C14_4 C13_4 C12_4 120.0(10) . . ? C14_4 C13_4 H13_4 120.0 . . ? C12_4 C13_4 H13_4 120.0 . . ? C15_4 C14_4 C13_4 121.5(11) . . ? C15_4 C14_4 H14_4 119.3 . . ? C13_4 C14_4 H14_4 119.3 . . ? C14_4 C15_4 C16_4 119.9(11) . . ? C14_4 C15_4 H15_4 120.0 . . ? C16_4 C15_4 H15_4 120.0 . . ? C11_4 C16_4 C15_4 117.3(9) . . ? C11_4 C16_4 C19_4 122.0(9) . . ? C15_4 C16_4 C19_4 120.6(9) . . ? C172_4 C17_4 C171_4 113.0(11) . . ? C172_4 C17_4 C12_4 113.0(10) . . ? C171_4 C17_4 C12_4 111.5(11) . . ? C172_4 C17_4 H17_4 106.2 . . ? C171_4 C17_4 H17_4 106.2 . . ? C12_4 C17_4 H17_4 106.2 . . ? C192_4 C19_4 C191_4 115.4(13) . . ? C192_4 C19_4 C16_4 109.5(11) . . ? C191_4 C19_4 C16_4 112.1(10) . . ? C192_4 C19_4 H19_4 106.4 . . ? C191_4 C19_4 H19_4 106.4 . . ? C16_4 C19_4 H19_4 106.4 . . ? C26_4 C21_4 C22_4 123.6(8) . . ? C26_4 C21_4 N5_4 118.2(8) . . ? C22_4 C21_4 N5_4 118.2(7) . . ? C23_4 C22_4 C21_4 116.2(9) . . ? C23_4 C22_4 C27_4 121.8(9) . . ? C21_4 C22_4 C27_4 122.0(8) . . ? C24_4 C23_4 C22_4 122.1(11) . . ? C24_4 C23_4 H23_4 119.0 . . ? C22_4 C23_4 H23_4 119.0 . . ? C23_4 C24_4 C25_4 120.1(12) . . ? C23_4 C24_4 H24_4 119.9 . . ? C25_4 C24_4 H24_4 119.9 . . ? C24_4 C25_4 C26_4 120.8(11) . . ? C24_4 C25_4 H25_4 119.6 . . ? C26_4 C25_4 H25_4 119.6 . . ? C21_4 C26_4 C25_4 116.8(9) . . ? C21_4 C26_4 C29_4 122.3(9) . . ? C25_4 C26_4 C29_4 120.7(9) . . ? C272_4 C27_4 C22_4 109.3(9) . . ? C272_4 C27_4 C271_4 108.4(9) . . ? C22_4 C27_4 C271_4 112.4(9) . . ? C272_4 C27_4 H27_4 108.9 . . ? C22_4 C27_4 H27_4 108.9 . . ? C271_4 C27_4 H27_4 108.9 . . ? C292_4 C29_4 C291_4 109.1(11) . . ? C292_4 C29_4 C26_4 111.7(9) . . ? C291_4 C29_4 C26_4 108.8(11) . . ? C292_4 C29_4 H29_4 109.1 . . ? C291_4 C29_4 H29_4 109.1 . . ? C26_4 C29_4 H29_4 109.1 . . ? C17_4 C171_4 H17A_4 109.5 . . ? C17_4 C171_4 H17B_4 109.5 . . ? H17A_4 C171_4 H17B_4 109.5 . . ? C17_4 C171_4 H17C_4 109.5 . . ? H17A_4 C171_4 H17C_4 109.5 . . ? H17B_4 C171_4 H17C_4 109.5 . . ? C17_4 C172_4 H17D_4 109.5 . . ? C17_4 C172_4 H17E_4 109.5 . . ? H17D_4 C172_4 H17E_4 109.5 . . ? C17_4 C172_4 H17F_4 109.5 . . ? H17D_4 C172_4 H17F_4 109.5 . . ? H17E_4 C172_4 H17F_4 109.5 . . ? C19_4 C191_4 H19A_4 109.5 . . ? C19_4 C191_4 H19B_4 109.5 . . ? H19A_4 C191_4 H19B_4 109.5 . . ? C19_4 C191_4 H19C_4 109.5 . . ? H19A_4 C191_4 H19C_4 109.5 . . ? H19B_4 C191_4 H19C_4 109.5 . . ? C19_4 C192_4 H19D_4 109.5 . . ? C19_4 C192_4 H19E_4 109.5 . . ? H19D_4 C192_4 H19E_4 109.5 . . ? C19_4 C192_4 H19F_4 109.5 . . ? H19D_4 C192_4 H19F_4 109.5 . . ? H19E_4 C192_4 H19F_4 109.5 . . ? C27_4 C271_4 H27A_4 109.5 . . ? C27_4 C271_4 H27B_4 109.5 . . ? H27A_4 C271_4 H27B_4 109.5 . . ? C27_4 C271_4 H27C_4 109.5 . . ? H27A_4 C271_4 H27C_4 109.5 . . ? H27B_4 C271_4 H27C_4 109.5 . . ? C27_4 C272_4 H27D_4 109.5 . . ? C27_4 C272_4 H27E_4 109.5 . . ? H27D_4 C272_4 H27E_4 109.5 . . ? C27_4 C272_4 H27F_4 109.5 . . ? H27D_4 C272_4 H27F_4 109.5 . . ? H27E_4 C272_4 H27F_4 109.5 . . ? C29_4 C291_4 H29A_4 109.5 . . ? C29_4 C291_4 H29B_4 109.5 . . ? H29A_4 C291_4 H29B_4 109.5 . . ? C29_4 C291_4 H29C_4 109.5 . . ? H29A_4 C291_4 H29C_4 109.5 . . ? H29B_4 C291_4 H29C_4 109.5 . . ? C29_4 C292_4 H29D_4 109.5 . . ? C29_4 C292_4 H29E_4 109.5 . . ? H29D_4 C292_4 H29E_4 109.5 . . ? C29_4 C292_4 H29F_4 109.5 . . ? H29D_4 C292_4 H29F_4 109.5 . . ? H29E_4 C292_4 H29F_4 109.5 . . ? C32_4 C31_4 Au1_4 172.2(15) . . ? C31_4 C32_4 C33_4 170.1(18) . . ? N34_4 C33_4 O39_4 116.6(9) . . ? N34_4 C33_4 C32_4 115.4(11) . . ? O39_4 C33_4 C32_4 127.9(11) . . ? C33_4 N34_4 C38_4 124.7(9) . . ? C33_4 N34_4 C35_4 111.9(10) . . ? C38_4 N34_4 C35_4 123.0(10) . . ? N34_4 C35_4 C36_4 95.1(10) . . ? N34_4 C35_4 H35A_4 112.7 . . ? C36_4 C35_4 H35A_4 112.7 . . ? N34_4 C35_4 H35B_4 112.7 . . ? C36_4 C35_4 H35B_4 112.7 . . ? H35A_4 C35_4 H35B_4 110.2 . . ? C37_4 C36_4 C35_4 107.4(11) . . ? C37_4 C36_4 H36A_4 110.2 . . ? C35_4 C36_4 H36A_4 110.2 . . ? C37_4 C36_4 H36B_4 110.2 . . ? C35_4 C36_4 H36B_4 110.2 . . ? H36A_4 C36_4 H36B_4 108.5 . . ? C38_4 C37_4 C36_4 110.8(14) . . ? C38_4 C37_4 H37A_4 109.5 . . ? C36_4 C37_4 H37A_4 109.5 . . ? C38_4 C37_4 H37B_4 109.5 . . ? C36_4 C37_4 H37B_4 109.5 . . ? H37A_4 C37_4 H37B_4 108.1 . . ? C37_4 C38_4 N34_4 100.2(11) . . ? C37_4 C38_4 H38A_4 111.7 . . ? N34_4 C38_4 H38A_4 111.7 . . ? C37_4 C38_4 H38B_4 111.7 . . ? N34_4 C38_4 H38B_4 111.7 . . ? H38A_4 C38_4 H38B_4 109.5 . . ? C33_4 O39_4 C39_4 123.7(10) . . ? O39_4 C39_4 H39A_4 109.5 . . ? O39_4 C39_4 H39B_4 109.5 . . ? H39A_4 C39_4 H39B_4 109.5 . . ? O39_4 C39_4 H39C_4 109.5 . . ? H39A_4 C39_4 H39C_4 109.5 . . ? H39B_4 C39_4 H39C_4 109.5 . . ? O12 S1 O11 121.5(10) . . ? O12 S1 O13 117.7(10) . . ? O11 S1 O13 110.2(8) . . ? O12 S1 C51 100.4(7) . . ? O11 S1 C51 100.8(7) . . ? O13 S1 C51 101.7(7) . . ? F13 C51 F12 108.8(11) . . ? F13 C51 F11 99.8(11) . . ? F12 C51 F11 101.7(11) . . ? F13 C51 S1 114.6(10) . . ? F12 C51 S1 113.8(8) . . ? F11 C51 S1 116.5(8) . . ? O23 S2 O22 131.7(12) . . ? O23 S2 O21 109.1(12) . . ? O22 S2 O21 108.5(10) . . ? O23 S2 C52 112.2(8) . . ? O22 S2 C52 96.9(8) . . ? O21 S2 C52 90.1(11) . . ? F22 C52 F23 111.9(13) . . ? F22 C52 F21 113.8(15) . . ? F23 C52 F21 110.8(15) . . ? F22 C52 S2 110.7(11) . . ? F23 C52 S2 111.0(12) . . ? F21 C52 S2 97.8(13) . . ? O33 S3 O31 109.4(9) . . ? O33 S3 O32 112.6(10) . . ? O31 S3 O32 121.5(9) . . ? O33 S3 C53 105.3(8) . . ? O31 S3 C53 100.2(7) . . ? O32 S3 C53 105.8(8) . . ? F31 C53 F32 104.9(13) . . ? F31 C53 F33 99.4(13) . . ? F32 C53 F33 102.1(12) . . ? F31 C53 S3 113.8(10) . . ? F32 C53 S3 118.9(10) . . ? F33 C53 S3 115.4(11) . . ? O43 S4 O42 118.3(10) . . ? O43 S4 O41 120.2(12) . . ? O42 S4 O41 110.3(9) . . ? O43 S4 C54 102.1(9) . . ? O42 S4 C54 102.9(9) . . ? O41 S4 C54 98.6(10) . . ? F41 C54 F42 109.9(15) . . ? F41 C54 F43 105.2(17) . . ? F42 C54 F43 110.3(15) . . ? F41 C54 S4 111.1(12) . . ? F42 C54 S4 112.6(13) . . ? F43 C54 S4 107.4(11) . . ? Cl1 C61 Cl2 111.8(16) . . ? Cl1 C61 H61A 109.3 . . ? Cl2 C61 H61A 109.3 . . ? Cl1 C61 H61B 109.3 . . ? Cl2 C61 H61B 109.3 . . ? H61A C61 H61B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.625 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.109 #===END