# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Catherine Hemmert' _publ_contact_author_email HEMMERT@LCC-TOULOUSE.FR _publ_section_title ; Dinuclear gold(I) and gold(III) complexes of bridging functionalized bis(N-heterocyclic carbene) ligands: synthesis, structural, spectroscopic and electrochemical characterizations ; loop_ _publ_author_name 'Catherine Hemmert' 'Francois Jean-Baptiste dit Dominique' 'Heinz Gornitzka' 'Alix Sournia-Saquet' # Attachment 'ch_lastone.cif' data_11 _database_code_depnum_ccdc_archive 'CCDC 691315' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H34 Au2 F12 N10 O4 P2' _chemical_formula_weight 1282.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5723(4) _cell_length_b 11.8949(4) _cell_length_c 14.8191(6) _cell_angle_alpha 81.481(2) _cell_angle_beta 76.0170(10) _cell_angle_gamma 84.7700(10) _cell_volume 1954.32(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9904 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.179 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 7.689 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.3085 _exptl_absorpt_correction_T_max 0.5136 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17635 _diffrn_reflns_av_R_equivalents 0.1587 _diffrn_reflns_av_sigmaI/netI 0.0999 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 5.12 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7870 _reflns_number_gt 6197 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0551P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7870 _refine_ls_number_parameters 619 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1147 _refine_ls_wR_factor_gt 0.1088 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.978 _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 0.95185(2) 0.58807(2) 0.749460(17) 0.02031(10) Uani 1 1 d . B . Au2 Au 0.88235(2) 0.86410(2) 0.722937(19) 0.02769(10) Uani 1 1 d . B . N1 N 1.1900(5) 0.5706(5) 0.8034(4) 0.0293(14) Uani 1 1 d . . . N2 N 1.0534(5) 0.6271(5) 0.9158(4) 0.0262(13) Uani 1 1 d . . . N3 N 0.8669(5) 0.7166(5) 0.9172(4) 0.0284(14) Uani 1 1 d . . . N4 N 0.6848(6) 0.8105(7) 0.9033(5) 0.0398(17) Uani 1 1 d . . . N5 N 0.6134(6) 0.8742(7) 0.7859(5) 0.049(2) Uani 1 1 d . . . N6 N 1.1169(6) 0.9778(6) 0.6514(5) 0.0371(16) Uani 1 1 d . B . N7 N 1.0939(5) 0.8777(5) 0.5491(4) 0.0275(13) Uani 1 1 d . B . N8 N 0.9708(5) 0.7322(5) 0.5584(4) 0.0251(13) Uani 1 1 d . B . N9 N 0.8392(5) 0.5882(5) 0.5800(4) 0.0269(13) Uani 1 1 d . B . N10 N 0.7434(5) 0.4879(6) 0.7033(4) 0.0319(14) Uani 1 1 d . B . O1 O 1.3262(5) 0.7354(5) 0.6660(4) 0.0445(14) Uani 1 1 d . . . H1 H 1.2859 0.7559 0.7167 0.067 Uiso 1 1 calc R . . O2 O 0.5535(7) 0.7178(8) 0.6793(5) 0.069(2) Uani 1 1 d . . . H2 H 0.4831 0.7355 0.6745 0.104 Uiso 1 1 calc R . . O4 O 0.5274(5) 0.5562(7) 0.8366(5) 0.065(2) Uani 1 1 d . . . H4A H 0.5399 0.6152 0.7975 0.097 Uiso 1 1 calc R . . C1 C 1.2673(7) 0.6496(8) 0.6403(5) 0.0367(19) Uani 1 1 d . . . H1A H 1.3123 0.6291 0.5786 0.044 Uiso 1 1 calc R . . H1B H 1.1867 0.6799 0.6339 0.044 Uiso 1 1 calc R . . C2 C 1.2562(6) 0.5445(7) 0.7114(6) 0.0349(18) Uani 1 1 d . . . H2A H 1.2147 0.4871 0.6909 0.042 Uiso 1 1 calc R . . H2B H 1.3367 0.5116 0.7155 0.042 Uiso 1 1 calc R . . C3 C 1.0718(6) 0.5998(6) 0.8264(5) 0.0225(14) Uani 1 1 d . . . C4 C 1.2447(7) 0.5773(7) 0.8758(6) 0.0344(18) Uani 1 1 d . . . H4 H 1.3267 0.5599 0.8752 0.041 Uiso 1 1 calc R . . C5 C 1.1606(7) 0.6127(7) 0.9468(6) 0.0347(18) Uani 1 1 d . . . H5 H 1.1709 0.6255 1.0061 0.042 Uiso 1 1 calc R . . C6 C 0.9423(6) 0.6744(6) 0.9680(5) 0.0236(14) Uani 1 1 d . . . C7 C 0.9232(7) 0.6747(7) 1.0642(5) 0.0339(18) Uani 1 1 d . . . H7 H 0.9803 0.6421 1.0985 0.041 Uiso 1 1 calc R . . C8 C 0.8155(7) 0.7257(7) 1.1065(5) 0.0362(19) Uani 1 1 d . . . H8 H 0.7967 0.7269 1.1724 0.043 Uiso 1 1 calc R . . C9 C 0.7372(7) 0.7733(7) 1.0570(5) 0.0362(19) Uani 1 1 d . . . H9 H 0.6645 0.8107 1.0860 0.043 Uiso 1 1 calc R . . C10 C 0.7667(6) 0.7658(7) 0.9613(5) 0.0315(17) Uani 1 1 d . . . C11 C 0.7177(7) 0.8442(7) 0.8092(5) 0.0339(18) Uani 1 1 d . . . C12 C 0.5625(8) 0.8216(11) 0.9370(7) 0.070(4) Uani 1 1 d . . . H12 H 0.5193 0.8048 1.0002 0.084 Uiso 1 1 calc R . . C13 C 0.5180(9) 0.8602(12) 0.8634(8) 0.079(4) Uani 1 1 d . . . H13 H 0.4360 0.8756 0.8635 0.095 Uiso 1 1 calc R . . C14 C 0.5962(10) 0.9073(10) 0.6909(7) 0.063(3) Uani 1 1 d . . . H14A H 0.6493 0.9689 0.6585 0.076 Uiso 1 1 calc R . . H14B H 0.5127 0.9366 0.6937 0.076 Uiso 1 1 calc R . . C15 C 0.6242(11) 0.8047(12) 0.6354(8) 0.067(3) Uani 1 1 d . . . H15A H 0.6112 0.8281 0.5715 0.081 Uiso 1 1 calc R . . H15B H 0.7091 0.7783 0.6295 0.081 Uiso 1 1 calc R . . O3 O 1.2095(5) 0.8644(5) 0.8053(4) 0.0475(16) Uani 1 1 d D . . H3 H 1.2134 0.8341 0.7569 0.071 Uiso 1 1 calc R A 1 C16 C 1.2120(12) 0.9809(11) 0.7823(10) 0.045(4) Uani 0.63(2) 1 d PD B 1 H16A H 1.2874 1.0003 0.7364 0.053 Uiso 0.63(2) 1 calc PR B 1 H16B H 1.2084 1.0169 0.8391 0.053 Uiso 0.63(2) 1 calc PR B 1 C17 C 1.1031(9) 1.0276(7) 0.7389(6) 0.045(2) Uani 1 1 d D . . H17A H 1.0274 1.0057 0.7833 0.054 Uiso 0.63(2) 1 calc PR B 1 H17B H 1.1018 1.1117 0.7257 0.054 Uiso 0.63(2) 1 calc PR B 1 H17C H 1.0272 1.0746 0.7504 0.054 Uiso 0.37(2) 1 calc PR B 2 H17D H 1.1691 1.0781 0.7317 0.054 Uiso 0.37(2) 1 calc PR B 2 C16' C 1.1034(16) 0.9328(15) 0.8272(11) 0.031(6) Uani 0.37(2) 1 d PD B 2 H16C H 1.1005 0.9690 0.8838 0.037 Uiso 0.37(2) 1 calc PR B 2 H16D H 1.0333 0.8862 0.8395 0.037 Uiso 0.37(2) 1 calc PR B 2 C18 C 1.0411(7) 0.9089(6) 0.6352(5) 0.0298(16) Uani 1 1 d . . . C19 C 1.2157(8) 0.9918(8) 0.5763(7) 0.048(2) Uani 1 1 d . . . H19 H 1.2810 1.0370 0.5714 0.058 Uiso 1 1 calc R B . C20 C 1.2008(7) 0.9297(8) 0.5127(6) 0.042(2) Uani 1 1 d . B . H20 H 1.2535 0.9224 0.4535 0.050 Uiso 1 1 calc R . . C21 C 1.0498(6) 0.8010(6) 0.5025(5) 0.0276(15) Uani 1 1 d . . . C22 C 1.0867(7) 0.8018(7) 0.4059(5) 0.0359(18) Uani 1 1 d . B . H22 H 1.1424 0.8537 0.3685 0.043 Uiso 1 1 calc R . . C23 C 1.0381(7) 0.7230(8) 0.3661(5) 0.039(2) Uani 1 1 d . . . H23 H 1.0610 0.7202 0.3004 0.046 Uiso 1 1 calc R B . C24 C 0.9575(7) 0.6499(7) 0.4221(5) 0.0320(17) Uani 1 1 d . B . H24 H 0.9243 0.5953 0.3964 0.038 Uiso 1 1 calc R . . C25 C 0.9253(6) 0.6581(6) 0.5184(5) 0.0272(16) Uani 1 1 d . . . C26 C 0.8370(6) 0.5557(6) 0.6734(5) 0.0251(15) Uani 1 1 d . . . C27 C 0.7492(7) 0.5422(8) 0.5545(6) 0.041(2) Uani 1 1 d . . . H27 H 0.7319 0.5526 0.4942 0.049 Uiso 1 1 calc R B . C28 C 0.6898(7) 0.4789(8) 0.6332(7) 0.046(2) Uani 1 1 d . B . H28 H 0.6226 0.4361 0.6381 0.055 Uiso 1 1 calc R . . C29 C 0.7033(8) 0.4336(8) 0.7997(7) 0.046(2) Uani 1 1 d . . . H29A H 0.7736 0.4020 0.8241 0.056 Uiso 1 1 calc R B . H29B H 0.6539 0.3696 0.8004 0.056 Uiso 1 1 calc R . . C30 C 0.6322(7) 0.5155(9) 0.8622(6) 0.048(2) Uani 1 1 d . B . H30A H 0.6131 0.4771 0.9276 0.058 Uiso 1 1 calc R . . H30B H 0.6810 0.5804 0.8601 0.058 Uiso 1 1 calc R . . P1 P 0.44846(18) 0.23450(18) 0.64374(15) 0.0344(5) Uani 1 1 d . . . F1 F 0.5880(4) 0.2115(5) 0.6395(4) 0.0599(16) Uani 1 1 d . . . F2 F 0.4418(5) 0.3267(5) 0.7130(4) 0.0632(17) Uani 1 1 d . . . F3 F 0.3087(4) 0.2583(5) 0.6490(5) 0.0650(16) Uani 1 1 d . . . F4 F 0.4171(6) 0.1415(5) 0.7332(4) 0.0689(17) Uani 1 1 d . . . F5 F 0.4770(6) 0.3293(6) 0.5556(5) 0.085(2) Uani 1 1 d . . . F6 F 0.4551(5) 0.1372(5) 0.5788(4) 0.0672(17) Uani 1 1 d . . . P2 P 0.8015(7) 0.1209(6) 0.9289(5) 0.0348(16) Uani 0.596(11) 1 d PD C 1 F7 F 0.8920(11) 0.2036(9) 0.8541(8) 0.055(3) Uani 0.596(11) 1 d PD C 1 F8 F 0.7152(9) 0.2297(7) 0.9569(7) 0.042(3) Uani 0.596(11) 1 d PD C 1 F9 F 0.8753(7) 0.1395(7) 1.0042(6) 0.050(3) Uani 0.596(11) 1 d PD C 1 F10 F 0.7150(7) 0.0438(7) 1.0096(7) 0.051(3) Uani 0.596(11) 1 d PD C 1 F11 F 0.8858(14) 0.0110(12) 0.9039(11) 0.059(4) Uani 0.596(11) 1 d PD C 1 F12 F 0.7335(14) 0.1071(12) 0.8517(10) 0.074(4) Uani 0.596(11) 1 d PD C 1 P2' P 0.7567(8) 0.1246(10) 0.9188(7) 0.028(2) Uani 0.404(11) 1 d PD C 2 F7' F 0.6529(11) 0.0411(10) 0.9411(11) 0.063(5) Uani 0.404(11) 1 d PD C 2 F8' F 0.7449(16) 0.136(2) 1.0263(9) 0.123(11) Uani 0.404(11) 1 d PD C 2 F9' F 0.6591(16) 0.2288(14) 0.9123(17) 0.103(9) Uani 0.404(11) 1 d PD C 2 F10' F 0.8603(18) 0.215(2) 0.8912(18) 0.128(14) Uani 0.404(11) 1 d PD C 2 F11' F 0.774(2) 0.125(2) 0.8096(10) 0.088(8) Uani 0.404(11) 1 d PD C 2 F12' F 0.857(2) 0.025(2) 0.9235(18) 0.100(13) Uani 0.404(11) 1 d PD C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01841(15) 0.01914(16) 0.02439(15) -0.00524(11) -0.00534(10) -0.00145(10) Au2 0.03783(18) 0.01944(17) 0.02629(16) -0.00657(12) -0.00702(12) 0.00053(12) N1 0.033(3) 0.022(3) 0.037(4) -0.005(3) -0.013(3) -0.001(3) N2 0.028(3) 0.027(3) 0.026(3) -0.003(3) -0.009(2) -0.008(2) N3 0.025(3) 0.028(3) 0.029(3) -0.007(3) 0.004(2) -0.003(3) N4 0.031(4) 0.055(5) 0.032(4) -0.016(3) -0.002(3) 0.015(3) N5 0.040(4) 0.062(5) 0.043(4) -0.018(4) -0.014(3) 0.030(4) N6 0.039(4) 0.023(4) 0.057(4) -0.013(3) -0.021(3) -0.002(3) N7 0.031(3) 0.024(3) 0.028(3) 0.005(3) -0.012(3) -0.005(3) N8 0.028(3) 0.025(3) 0.022(3) -0.008(3) -0.002(2) -0.003(2) N9 0.026(3) 0.029(3) 0.031(3) -0.009(3) -0.013(2) -0.003(2) N10 0.025(3) 0.036(4) 0.037(4) -0.005(3) -0.009(3) -0.011(3) O1 0.046(3) 0.043(4) 0.043(4) -0.006(3) -0.003(3) -0.010(3) O2 0.070(5) 0.086(6) 0.061(5) -0.007(4) -0.034(4) 0.004(5) O4 0.033(3) 0.092(6) 0.063(5) -0.003(4) -0.002(3) -0.007(3) C1 0.034(4) 0.045(5) 0.027(4) -0.007(4) 0.000(3) 0.005(4) C2 0.024(4) 0.035(5) 0.046(5) -0.014(4) -0.008(3) 0.009(3) C3 0.021(3) 0.012(3) 0.035(4) -0.004(3) -0.007(3) -0.001(2) C4 0.024(4) 0.037(5) 0.045(5) -0.002(4) -0.015(3) -0.004(3) C5 0.036(4) 0.037(5) 0.034(4) 0.003(4) -0.018(3) -0.008(3) C6 0.030(4) 0.020(3) 0.022(3) -0.002(3) -0.006(3) -0.009(3) C7 0.043(5) 0.034(5) 0.025(4) 0.000(3) -0.005(3) -0.017(4) C8 0.043(5) 0.041(5) 0.023(4) -0.009(4) 0.003(3) -0.012(4) C9 0.040(4) 0.034(5) 0.032(4) -0.011(4) 0.004(3) -0.010(3) C10 0.032(4) 0.029(4) 0.032(4) -0.008(3) -0.001(3) -0.004(3) C11 0.040(4) 0.029(4) 0.030(4) -0.011(3) -0.003(3) 0.012(3) C12 0.037(5) 0.114(10) 0.050(6) -0.025(6) 0.001(4) 0.034(6) C13 0.034(5) 0.134(12) 0.065(7) -0.038(8) -0.008(5) 0.049(7) C14 0.075(7) 0.062(7) 0.045(6) 0.001(5) -0.018(5) 0.033(6) C15 0.070(7) 0.088(9) 0.048(6) -0.017(6) -0.028(5) 0.023(7) O3 0.068(4) 0.035(4) 0.040(3) -0.013(3) -0.013(3) 0.007(3) C16 0.060(10) 0.036(8) 0.043(8) -0.013(7) -0.019(7) -0.001(7) C17 0.073(6) 0.023(4) 0.049(5) -0.011(4) -0.035(5) 0.006(4) C16' 0.045(13) 0.030(12) 0.022(11) -0.014(9) -0.014(9) 0.004(9) C18 0.042(4) 0.016(4) 0.032(4) -0.002(3) -0.009(3) -0.004(3) C19 0.037(5) 0.041(5) 0.070(6) 0.000(5) -0.018(4) -0.016(4) C20 0.042(5) 0.042(5) 0.042(5) 0.004(4) -0.011(4) -0.016(4) C21 0.034(4) 0.017(4) 0.032(4) -0.002(3) -0.009(3) 0.000(3) C22 0.047(5) 0.030(4) 0.029(4) 0.000(3) -0.006(3) -0.003(4) C23 0.044(5) 0.049(5) 0.018(4) -0.003(4) -0.004(3) 0.009(4) C24 0.035(4) 0.033(4) 0.032(4) -0.014(4) -0.014(3) 0.008(3) C25 0.030(4) 0.025(4) 0.027(4) -0.012(3) -0.006(3) 0.007(3) C26 0.023(3) 0.021(4) 0.031(4) -0.005(3) -0.006(3) 0.002(3) C27 0.038(4) 0.052(6) 0.040(5) -0.013(4) -0.019(4) -0.011(4) C28 0.034(5) 0.053(6) 0.061(6) -0.020(5) -0.018(4) -0.013(4) C29 0.037(5) 0.048(6) 0.052(5) 0.003(5) -0.004(4) -0.023(4) C30 0.028(4) 0.073(7) 0.039(5) 0.001(5) -0.002(4) -0.010(4) P1 0.0300(10) 0.0275(11) 0.0445(12) -0.0069(9) -0.0039(9) -0.0048(8) F1 0.033(3) 0.066(4) 0.083(4) -0.036(3) -0.005(3) 0.005(2) F2 0.051(3) 0.049(4) 0.098(5) -0.042(3) -0.018(3) 0.008(3) F3 0.035(3) 0.067(4) 0.097(5) -0.013(4) -0.019(3) -0.007(3) F4 0.088(4) 0.050(4) 0.055(4) 0.007(3) 0.003(3) -0.002(3) F5 0.077(4) 0.077(5) 0.089(5) 0.052(4) -0.023(4) -0.025(4) F6 0.070(4) 0.074(4) 0.068(4) -0.039(3) -0.013(3) -0.019(3) P2 0.051(4) 0.025(2) 0.024(2) -0.0091(17) 0.005(3) -0.005(3) F7 0.080(9) 0.035(6) 0.040(6) 0.011(5) -0.003(6) -0.014(5) F8 0.053(6) 0.017(4) 0.047(6) -0.006(4) 0.005(4) 0.003(4) F9 0.053(6) 0.044(6) 0.050(6) -0.009(4) -0.007(4) 0.000(4) F10 0.044(5) 0.027(5) 0.065(7) 0.007(4) 0.015(5) -0.007(4) F11 0.090(11) 0.034(6) 0.045(7) -0.026(5) 0.010(7) 0.011(6) F12 0.110(12) 0.067(9) 0.063(10) -0.027(8) -0.045(9) -0.011(8) P2' 0.025(4) 0.028(3) 0.029(4) -0.011(3) 0.005(3) -0.005(4) F7' 0.050(8) 0.033(8) 0.093(12) -0.031(8) 0.023(8) -0.008(6) F8' 0.097(15) 0.23(3) 0.052(11) -0.068(16) 0.011(10) -0.054(17) F9' 0.061(13) 0.052(11) 0.14(2) 0.039(13) 0.047(12) 0.017(10) F10' 0.061(12) 0.17(3) 0.16(3) -0.11(2) 0.044(14) -0.073(14) F11' 0.108(16) 0.119(18) 0.019(9) 0.005(10) 0.010(9) -0.001(13) F12' 0.066(12) 0.10(2) 0.081(19) 0.049(15) 0.028(12) 0.051(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 C3 2.023(7) . ? Au1 C26 2.033(7) . ? Au1 Au2 3.2971(4) . ? Au2 C11 2.034(8) . ? Au2 C18 2.042(8) . ? N1 C3 1.353(8) . ? N1 C4 1.386(10) . ? N1 C2 1.455(9) . ? N2 C3 1.373(9) . ? N2 C5 1.411(9) . ? N2 C6 1.445(9) . ? N3 C6 1.306(9) . ? N3 C10 1.319(9) . ? N4 C11 1.362(10) . ? N4 C12 1.384(11) . ? N4 C10 1.444(10) . ? N5 C11 1.338(10) . ? N5 C13 1.389(13) . ? N5 C14 1.460(12) . ? N6 C18 1.338(10) . ? N6 C19 1.392(11) . ? N6 C17 1.472(10) . ? N7 C18 1.364(9) . ? N7 C20 1.387(10) . ? N7 C21 1.418(9) . ? N8 C21 1.327(9) . ? N8 C25 1.341(9) . ? N9 C27 1.372(9) . ? N9 C26 1.375(9) . ? N9 C25 1.415(10) . ? N10 C28 1.353(10) . ? N10 C26 1.357(9) . ? N10 C29 1.462(11) . ? O1 C1 1.421(11) . ? O2 C15 1.364(15) . ? O4 C30 1.383(10) . ? C1 C2 1.504(12) . ? C4 C5 1.340(10) . ? C6 C7 1.388(10) . ? C7 C8 1.382(11) . ? C8 C9 1.336(12) . ? C9 C10 1.391(11) . ? C12 C13 1.321(14) . ? C14 C15 1.538(15) . ? O3 C16 1.378(13) . ? O3 C16' 1.405(15) . ? C16 C17 1.570(14) . ? C17 C16' 1.596(17) . ? C19 C20 1.331(13) . ? C21 C22 1.390(10) . ? C22 C23 1.402(12) . ? C23 C24 1.369(12) . ? C24 C25 1.401(10) . ? C27 C28 1.358(13) . ? C29 C30 1.496(13) . ? P1 F5 1.584(6) . ? P1 F4 1.587(6) . ? P1 F2 1.594(5) . ? P1 F6 1.597(5) . ? P1 F1 1.601(5) . ? P1 F3 1.601(5) . ? P2 F12 1.572(12) . ? P2 F11 1.591(13) . ? P2 F10 1.593(10) . ? P2 F8 1.603(10) . ? P2 F9 1.610(11) . ? P2 F7 1.612(12) . ? P2' F7' 1.571(14) . ? P2' F11' 1.582(16) . ? P2' F12' 1.583(17) . ? P2' F8' 1.591(13) . ? P2' F9' 1.607(14) . ? P2' F10' 1.618(16) . ? 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 C3 Au1 C26 173.1(3) . . ? C3 Au1 Au2 94.36(19) . . ? C26 Au1 Au2 92.6(2) . . ? C11 Au2 C18 171.7(3) . . ? C11 Au2 Au1 92.3(2) . . ? C18 Au2 Au1 96.0(2) . . ? C3 N1 C4 112.1(6) . . ? C3 N1 C2 125.0(6) . . ? C4 N1 C2 122.7(6) . . ? C3 N2 C5 110.9(6) . . ? C3 N2 C6 124.7(6) . . ? C5 N2 C6 124.1(6) . . ? C6 N3 C10 116.6(6) . . ? C11 N4 C12 112.0(8) . . ? C11 N4 C10 124.5(6) . . ? C12 N4 C10 123.5(7) . . ? C11 N5 C13 111.6(8) . . ? C11 N5 C14 126.1(8) . . ? C13 N5 C14 122.1(8) . . ? C18 N6 C19 111.1(7) . . ? C18 N6 C17 125.2(7) . . ? C19 N6 C17 123.5(7) . . ? C18 N7 C20 110.4(7) . . ? C18 N7 C21 126.1(6) . . ? C20 N7 C21 123.5(6) . . ? C21 N8 C25 117.2(6) . . ? C27 N9 C26 111.2(7) . . ? C27 N9 C25 124.9(7) . . ? C26 N9 C25 123.9(6) . . ? C28 N10 C26 111.6(7) . . ? C28 N10 C29 124.1(7) . . ? C26 N10 C29 124.3(6) . . ? O1 C1 C2 112.0(7) . . ? N1 C2 C1 111.1(6) . . ? N1 C3 N2 103.6(6) . . ? N1 C3 Au1 126.6(5) . . ? N2 C3 Au1 129.5(5) . . ? C5 C4 N1 107.3(6) . . ? C4 C5 N2 106.1(6) . . ? N3 C6 C7 125.2(7) . . ? N3 C6 N2 114.5(6) . . ? C7 C6 N2 120.3(7) . . ? C8 C7 C6 115.4(8) . . ? C9 C8 C7 121.7(7) . . ? C8 C9 C10 117.1(7) . . ? N3 C10 C9 124.1(8) . . ? N3 C10 N4 115.2(6) . . ? C9 C10 N4 120.7(7) . . ? N5 C11 N4 103.2(6) . . ? N5 C11 Au2 126.1(6) . . ? N4 C11 Au2 130.4(6) . . ? C13 C12 N4 105.9(9) . . ? C12 C13 N5 107.4(8) . . ? N5 C14 C15 110.4(8) . . ? O2 C15 C14 110.8(10) . . ? C16 O3 C16' 60.4(11) . . ? O3 C16 C17 109.8(9) . . ? N6 C17 C16 107.6(7) . . ? N6 C17 C16' 112.4(8) . . ? C16 C17 C16' 52.5(9) . . ? O3 C16' C17 107.0(11) . . ? N6 C18 N7 104.7(7) . . ? N6 C18 Au2 126.1(6) . . ? N7 C18 Au2 129.3(5) . . ? C20 C19 N6 106.8(8) . . ? C19 C20 N7 107.0(8) . . ? N8 C21 C22 124.3(7) . . ? N8 C21 N7 114.4(6) . . ? C22 C21 N7 121.3(7) . . ? C21 C22 C23 117.2(8) . . ? C24 C23 C22 119.9(7) . . ? C23 C24 C25 118.0(8) . . ? N8 C25 C24 123.4(7) . . ? N8 C25 N9 115.5(6) . . ? C24 C25 N9 121.1(7) . . ? N10 C26 N9 103.6(6) . . ? N10 C26 Au1 126.7(5) . . ? N9 C26 Au1 129.6(5) . . ? C28 C27 N9 105.9(7) . . ? N10 C28 C27 107.7(7) . . ? N10 C29 C30 111.8(8) . . ? O4 C30 C29 112.4(8) . . ? F5 P1 F4 178.5(4) . . ? F5 P1 F2 90.9(4) . . ? F4 P1 F2 88.2(4) . . ? F5 P1 F6 92.0(4) . . ? F4 P1 F6 89.0(3) . . ? F2 P1 F6 177.1(4) . . ? F5 P1 F1 90.2(4) . . ? F4 P1 F1 90.9(4) . . ? F2 P1 F1 89.5(3) . . ? F6 P1 F1 89.9(3) . . ? F5 P1 F3 90.0(4) . . ? F4 P1 F3 88.9(4) . . ? F2 P1 F3 89.9(3) . . ? F6 P1 F3 90.7(3) . . ? F1 P1 F3 179.3(3) . . ? F12 P2 F11 90.4(7) . . ? F12 P2 F10 94.0(9) . . ? F11 P2 F10 89.9(8) . . ? F12 P2 F8 90.2(7) . . ? F11 P2 F8 178.4(9) . . ? F10 P2 F8 88.7(5) . . ? F12 P2 F9 177.1(9) . . ? F11 P2 F9 89.9(7) . . ? F10 P2 F9 88.9(6) . . ? F8 P2 F9 89.5(6) . . ? F12 P2 F7 90.5(8) . . ? F11 P2 F7 91.9(8) . . ? F10 P2 F7 175.2(8) . . ? F8 P2 F7 89.5(6) . . ? F9 P2 F7 86.6(7) . . ? F7' P2' F11' 91.7(11) . . ? F7' P2' F12' 93.9(13) . . ? F11' P2' F12' 91.5(11) . . ? F7' P2' F8' 93.4(11) . . ? F11' P2' F8' 174.5(15) . . ? F12' P2' F8' 90.3(13) . . ? F7' P2' F9' 88.3(9) . . ? F11' P2' F9' 88.0(13) . . ? F12' P2' F9' 177.7(14) . . ? F8' P2' F9' 90.0(12) . . ? F7' P2' F10' 176.8(14) . . ? F11' P2' F10' 86.0(12) . . ? F12' P2' F10' 88.4(13) . . ? F8' P2' F10' 88.8(12) . . ? F9' P2' F10' 89.3(12) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 3.131 _refine_diff_density_min -3.204 _refine_diff_density_rms 0.232 #===END data_12 _database_code_depnum_ccdc_archive 'CCDC 691316' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H48 Au2 Br2 N8 O4' _chemical_formula_weight 1138.52 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' Br Br -0.2901 2.4595 '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 Trigonal _symmetry_space_group_name_H-M R32 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' _cell_length_a 18.5387(3) _cell_length_b 18.5387(3) _cell_length_c 30.0782(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 8952.4(3) _cell_formula_units_Z 9 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 5702 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 21.90 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.901 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4896 _exptl_absorpt_coefficient_mu 9.416 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.2546 _exptl_absorpt_correction_T_max 0.6503 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23037 _diffrn_reflns_av_R_equivalents 0.0688 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 5.12 _diffrn_reflns_theta_max 24.70 _reflns_number_total 3378 _reflns_number_gt 3050 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+246.9595P] 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 -0.01(2) _refine_ls_number_reflns 3378 _refine_ls_number_parameters 219 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0563 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1032 _refine_ls_wR_factor_gt 0.0998 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.000 _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 -0.10880(3) 0.76030(3) -0.006351(15) 0.03522(15) Uani 1 1 d . . . N1 N -0.2233(7) 0.7185(8) 0.0728(4) 0.046(3) Uani 1 1 d . . . N2 N -0.1030(7) 0.8199(7) 0.0902(3) 0.036(2) Uani 1 1 d . . . N3 N 0.0351(7) 0.8432(6) 0.1005(3) 0.035(3) Uani 1 1 d . . . N4 N 0.1181(7) 0.7957(7) 0.0953(3) 0.037(3) Uani 1 1 d . . . O1 O -0.3425(7) 0.5582(7) 0.1138(3) 0.065(3) Uani 1 1 d . . . H1 H -0.3566 0.5109 0.1242 0.097 Uiso 1 1 calc R . . O2 O 0.1260(9) 0.6448(8) 0.1154(4) 0.077(4) Uani 1 1 d . . . H2 H 0.0797 0.6007 0.1143 0.115 Uiso 1 1 calc R . . C1 C -0.1459(8) 0.7664(8) 0.0570(5) 0.040(4) Uani 1 1 d . . . C2 C -0.2247(10) 0.7470(11) 0.1171(5) 0.050(4) Uani 1 1 d . . . H2A H -0.2719 0.7239 0.1361 0.060 Uiso 1 1 calc R . . C3 C -0.1519(10) 0.8088(9) 0.1273(4) 0.044(3) Uani 1 1 d . . . H3 H -0.1356 0.8396 0.1543 0.052 Uiso 1 1 calc R . . C4 C -0.2906(9) 0.6491(11) 0.0517(5) 0.058(4) Uani 1 1 d . . . H4A H -0.2780 0.6511 0.0196 0.069 Uiso 1 1 calc R . . H4B H -0.3410 0.6543 0.0547 0.069 Uiso 1 1 calc R . . C5 C -0.3101(11) 0.5650(12) 0.0697(5) 0.064(5) Uani 1 1 d . . . C6 C -0.3750(12) 0.4986(11) 0.0384(7) 0.092(7) Uani 1 1 d . . . H6A H -0.3952 0.4432 0.0513 0.138 Uiso 1 1 calc R . . H6B H -0.3493 0.5017 0.0094 0.138 Uiso 1 1 calc R . . H6C H -0.4218 0.5085 0.0345 0.138 Uiso 1 1 calc R . . C7 C -0.2299(12) 0.5594(10) 0.0736(6) 0.075(5) Uani 1 1 d . . . H7A H -0.1895 0.6048 0.0925 0.112 Uiso 1 1 calc R . . H7B H -0.2059 0.5641 0.0440 0.112 Uiso 1 1 calc R . . H7C H -0.2433 0.5058 0.0868 0.112 Uiso 1 1 calc R . . C8 C -0.0151(9) 0.8805(9) 0.0889(5) 0.046(4) Uani 1 1 d . . . H8A H -0.0031 0.9262 0.1099 0.055 Uiso 1 1 calc R . . H8B H 0.0001 0.9045 0.0586 0.055 Uiso 1 1 calc R . . C9 C 0.0828(8) 0.8321(7) 0.0707(4) 0.033(3) Uani 1 1 d . . . C10 C 0.0394(9) 0.8144(9) 0.1407(4) 0.045(4) Uani 1 1 d . . . H10 H 0.0105 0.8156 0.1665 0.054 Uiso 1 1 calc R . . C11 C 0.0899(9) 0.7845(9) 0.1387(5) 0.047(4) Uani 1 1 d . . . H11 H 0.1042 0.7599 0.1622 0.056 Uiso 1 1 calc R . . C12 C 0.1797(9) 0.7747(9) 0.0783(5) 0.054(4) Uani 1 1 d . . . H12A H 0.2278 0.7973 0.0989 0.065 Uiso 1 1 calc R . . H12B H 0.2001 0.8018 0.0491 0.065 Uiso 1 1 calc R . . C13 C 0.1456(9) 0.6828(10) 0.0733(5) 0.047(4) Uani 1 1 d . . . C14 C 0.2141(13) 0.6665(14) 0.0532(7) 0.086(7) Uani 1 1 d . . . H14A H 0.2680 0.7045 0.0670 0.128 Uiso 1 1 calc R . . H14B H 0.2178 0.6761 0.0211 0.128 Uiso 1 1 calc R . . H14C H 0.1996 0.6088 0.0592 0.128 Uiso 1 1 calc R . . C15 C 0.0687(12) 0.6444(13) 0.0451(7) 0.082(6) Uani 1 1 d . . . H15A H 0.0566 0.5891 0.0352 0.123 Uiso 1 1 calc R . . H15B H 0.0775 0.6798 0.0191 0.123 Uiso 1 1 calc R . . H15C H 0.0216 0.6393 0.0625 0.123 Uiso 1 1 calc R . . Br1 Br 0.9091(3) 0.3751(3) 0.8665(2) 0.1150(19) Uani 0.50 1 d P . . Br2 Br 0.3333 0.6667 0.85963(8) 0.0574(7) Uani 1 3 d S . . Br3 Br 0.0000 0.0000 0.0000 0.0898(15) Uani 1 6 d S . . 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 0.0413(3) 0.0431(3) 0.0253(2) 0.0100(2) 0.0070(2) 0.0241(3) N1 0.037(6) 0.064(8) 0.030(7) 0.014(6) 0.004(5) 0.020(6) N2 0.044(6) 0.041(6) 0.031(6) 0.014(5) 0.016(5) 0.026(5) N3 0.052(6) 0.036(6) 0.023(6) 0.001(5) 0.010(5) 0.027(6) N4 0.048(7) 0.045(6) 0.021(6) -0.008(5) -0.007(5) 0.025(6) O1 0.067(7) 0.058(7) 0.031(6) 0.018(5) 0.007(5) 0.002(6) O2 0.087(10) 0.081(9) 0.079(10) 0.016(7) 0.024(8) 0.054(8) C1 0.051(9) 0.046(8) 0.027(7) 0.022(6) 0.011(6) 0.026(7) C2 0.062(10) 0.071(11) 0.029(8) 0.024(7) 0.021(7) 0.041(9) C3 0.055(9) 0.040(8) 0.034(8) 0.008(6) 0.018(7) 0.022(7) C4 0.036(8) 0.093(13) 0.035(8) 0.018(8) 0.011(7) 0.025(8) C5 0.056(10) 0.074(12) 0.041(10) 0.015(9) -0.013(8) 0.015(9) C6 0.075(12) 0.062(12) 0.079(14) -0.008(10) -0.009(11) -0.011(10) C7 0.089(13) 0.052(10) 0.064(10) 0.017(8) 0.005(10) 0.020(10) C8 0.070(10) 0.042(8) 0.032(8) 0.000(6) 0.019(7) 0.033(8) C9 0.037(7) 0.025(6) 0.036(7) -0.005(5) -0.005(6) 0.014(5) C10 0.064(9) 0.056(9) 0.012(7) 0.004(6) 0.005(6) 0.028(8) C11 0.055(9) 0.046(8) 0.039(9) 0.005(7) -0.002(7) 0.025(7) C12 0.042(8) 0.058(10) 0.061(10) -0.003(8) 0.000(7) 0.024(7) C13 0.039(8) 0.061(9) 0.044(9) -0.009(7) -0.004(7) 0.028(8) C14 0.093(15) 0.127(18) 0.084(15) 0.001(12) 0.001(12) 0.091(15) C15 0.071(12) 0.079(13) 0.110(17) -0.043(12) -0.012(11) 0.047(11) Br1 0.102(4) 0.085(3) 0.168(6) 0.050(3) 0.034(4) 0.054(3) Br2 0.0651(11) 0.0651(11) 0.0420(13) 0.000 0.000 0.0326(5) Br3 0.094(2) 0.094(2) 0.081(3) 0.000 0.000 0.0470(11) _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 C9 2.030(13) 6 ? Au1 C1 2.048(14) . ? N1 C1 1.342(16) . ? N1 C4 1.42(2) . ? N1 C2 1.439(18) . ? N2 C1 1.349(17) . ? N2 C3 1.387(15) . ? N2 C8 1.446(17) . ? N3 C10 1.338(16) . ? N3 C9 1.346(16) . ? N3 C8 1.451(17) . ? N4 C9 1.367(16) . ? N4 C11 1.381(18) . ? N4 C12 1.471(18) . ? O1 C5 1.44(2) . ? O2 C13 1.407(18) . ? C2 C3 1.30(2) . ? C4 C5 1.51(2) . ? C5 C6 1.54(2) . ? C5 C7 1.55(3) . ? C9 Au1 2.030(13) 6 ? C10 C11 1.306(19) . ? C12 C13 1.50(2) . ? C13 C15 1.50(2) . ? C13 C14 1.57(2) . ? Br1 Br1 2.404(14) 17_556 ? 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 C9 Au1 C1 175.0(5) 6 . ? C1 N1 C4 127.4(12) . . ? C1 N1 C2 107.1(12) . . ? C4 N1 C2 125.4(12) . . ? C1 N2 C3 112.7(12) . . ? C1 N2 C8 124.9(11) . . ? C3 N2 C8 122.4(12) . . ? C10 N3 C9 111.4(11) . . ? C10 N3 C8 126.1(11) . . ? C9 N3 C8 122.6(11) . . ? C9 N4 C11 110.3(11) . . ? C9 N4 C12 124.7(12) . . ? C11 N4 C12 125.0(12) . . ? N1 C1 N2 105.5(12) . . ? N1 C1 Au1 124.8(11) . . ? N2 C1 Au1 129.6(9) . . ? C3 C2 N1 110.0(12) . . ? C2 C3 N2 104.8(12) . . ? N1 C4 C5 115.0(13) . . ? O1 C5 C4 107.1(15) . . ? O1 C5 C6 111.7(14) . . ? C4 C5 C6 107.1(14) . . ? O1 C5 C7 107.3(12) . . ? C4 C5 C7 110.8(13) . . ? C6 C5 C7 112.7(18) . . ? N2 C8 N3 111.5(11) . . ? N3 C9 N4 103.2(11) . . ? N3 C9 Au1 130.3(9) . 6 ? N4 C9 Au1 126.3(9) . 6 ? C11 C10 N3 109.1(13) . . ? C10 C11 N4 106.1(13) . . ? N4 C12 C13 113.2(12) . . ? O2 C13 C15 109.1(15) . . ? O2 C13 C12 109.5(12) . . ? C15 C13 C12 110.9(14) . . ? O2 C13 C14 106.3(14) . . ? C15 C13 C14 111.3(14) . . ? C12 C13 C14 109.6(13) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 24.70 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.738 _refine_diff_density_min -2.707 _refine_diff_density_rms 0.170 #===END data_15.MeOH.H2O _database_code_depnum_ccdc_archive 'CCDC 691317' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H62 Au2 F12 N8 O6 P2' _chemical_formula_weight 1374.80 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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 15.814(3) _cell_length_b 12.286(2) _cell_length_c 28.357(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.366(3) _cell_angle_gamma 90.00 _cell_volume 5419.3(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4404 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 29.79 _exptl_crystal_description plate _exptl_crystal_colour clear _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.685 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2688 _exptl_absorpt_coefficient_mu 5.553 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.1678 _exptl_absorpt_correction_T_max 0.6067 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16612 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0842 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 5.11 _diffrn_reflns_theta_max 26.37 _reflns_number_total 10577 _reflns_number_gt 7222 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0861P)^2^+145.4051P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10577 _refine_ls_number_parameters 681 _refine_ls_number_restraints 192 _refine_ls_R_factor_all 0.1090 _refine_ls_R_factor_gt 0.0736 _refine_ls_wR_factor_ref 0.2099 _refine_ls_wR_factor_gt 0.1890 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.032 _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 0.77544(3) 0.35367(4) 0.179384(18) 0.02075(16) Uani 1 1 d . . . Au2 Au 1.17630(3) 0.34828(4) 0.179127(19) 0.02368(17) Uani 1 1 d . . . N1 N 1.2326(7) 0.5808(10) 0.1648(5) 0.031(3) Uani 1 1 d . . . N2 N 1.1420(7) 0.5768(9) 0.2125(4) 0.026(3) Uani 1 1 d . . . N3 N 0.8343(7) 0.5751(9) 0.2183(4) 0.023(2) Uani 1 1 d . . . N4 N 0.7121(7) 0.5882(9) 0.1705(4) 0.022(2) Uani 1 1 d . . . O1 O 1.1789(10) 0.4712(17) 0.0715(6) 0.086(6) Uani 1 1 d . . . H1 H 1.1789 0.4409 0.0450 0.129 Uiso 1 1 calc R . . O2 O 0.7120(7) 0.4780(11) 0.0774(4) 0.049(3) Uani 1 1 d . . . H2 H 0.7619 0.5013 0.0771 0.073 Uiso 1 1 calc R . . C1 C 1.1824(9) 0.5088(11) 0.1851(6) 0.030(3) Uani 1 1 d U . . C2 C 1.2263(10) 0.6871(12) 0.1820(7) 0.038(4) Uani 1 1 d . . . H2 H 1.2555 0.7497 0.1736 0.046 Uiso 1 1 calc R . . C3 C 1.1697(10) 0.6832(12) 0.2135(6) 0.036(4) Uani 1 1 d . . . H3 H 1.1532 0.7414 0.2320 0.043 Uiso 1 1 calc R . . C4 C 1.2865(8) 0.5528(12) 0.1304(5) 0.026(3) Uani 1 1 d . . . H4A H 1.3096 0.4787 0.1379 0.031 Uiso 1 1 calc R . . H4B H 1.3359 0.6036 0.1348 0.031 Uiso 1 1 calc R . . C5 C 1.2441(10) 0.5556(16) 0.0789(7) 0.046(4) Uani 1 1 d . . . C6 C 1.3102(14) 0.535(2) 0.0485(7) 0.065(6) Uani 1 1 d . . . H6A H 1.3425 0.4688 0.0597 0.097 Uiso 1 1 calc R . . H6B H 1.3496 0.5968 0.0507 0.097 Uiso 1 1 calc R . . H6C H 1.2817 0.5250 0.0151 0.097 Uiso 1 1 calc R . . C7 C 1.205(2) 0.672(2) 0.0662(9) 0.103(11) Uani 1 1 d . . . H7A H 1.1419 0.6668 0.0598 0.155 Uiso 1 1 calc R . . H7B H 1.2246 0.6995 0.0377 0.155 Uiso 1 1 calc R . . H7C H 1.2233 0.7211 0.0932 0.155 Uiso 1 1 calc R . . C8 C 1.0776(8) 0.5372(13) 0.2405(5) 0.030(3) Uani 1 1 d . . . H8A H 1.0872 0.5719 0.2725 0.036 Uiso 1 1 calc R . . H8B H 1.0828 0.4574 0.2449 0.036 Uiso 1 1 calc R . . C9 C 0.9881(8) 0.5662(13) 0.2130(5) 0.030(3) Uani 1 1 d . . . H9A H 0.9774 0.5271 0.1819 0.036 Uiso 1 1 calc R . . H9B H 0.9851 0.6453 0.2062 0.036 Uiso 1 1 calc R . . C10 C 0.9172(8) 0.5345(11) 0.2428(5) 0.024(3) Uani 1 1 d . . . H10A H 0.9149 0.4544 0.2461 0.029 Uiso 1 1 calc R . . H10B H 0.9313 0.5666 0.2753 0.029 Uiso 1 1 calc R . . C11 C 0.7740(10) 0.5119(11) 0.1897(5) 0.030(3) Uani 1 1 d . . . C12 C 0.7332(10) 0.6901(12) 0.1889(6) 0.030(3) Uani 1 1 d . . . H12 H 0.6997 0.7541 0.1814 0.036 Uiso 1 1 calc R . . C13 C 0.8096(9) 0.6846(10) 0.2194(5) 0.024(3) Uani 1 1 d . . . H13 H 0.8397 0.7421 0.2376 0.029 Uiso 1 1 calc R . . C14 C 0.6375(8) 0.5649(11) 0.1341(5) 0.022(3) Uani 1 1 d . . . H14A H 0.5922 0.6191 0.1365 0.026 Uiso 1 1 calc R . . H14B H 0.6149 0.4922 0.1403 0.026 Uiso 1 1 calc R . . C15 C 0.6571(9) 0.5671(14) 0.0838(6) 0.035(4) Uani 1 1 d . . . C16 C 0.6979(14) 0.6740(16) 0.0713(8) 0.060(6) Uani 1 1 d . . . H16A H 0.7554 0.6813 0.0909 0.091 Uiso 1 1 calc R . . H16B H 0.6620 0.7353 0.0778 0.091 Uiso 1 1 calc R . . H16C H 0.7024 0.6737 0.0373 0.091 Uiso 1 1 calc R . . C17 C 0.5691(11) 0.544(2) 0.0498(7) 0.059(6) Uani 1 1 d . . . H17A H 0.5797 0.5238 0.0179 0.089 Uiso 1 1 calc R . . H17B H 0.5331 0.6093 0.0473 0.089 Uiso 1 1 calc R . . H17C H 0.5395 0.4840 0.0629 0.089 Uiso 1 1 calc R . . N5 N 1.2300(7) 0.1152(9) 0.1605(5) 0.027(3) Uani 1 1 d . . . N6 N 1.1382(9) 0.1195(11) 0.2065(5) 0.039(3) Uani 1 1 d . . . N7 N 0.8240(7) 0.1172(9) 0.2001(5) 0.028(3) Uani 1 1 d . . . N8 N 0.7062(8) 0.1262(9) 0.1500(5) 0.029(3) Uani 1 1 d . . . O3 O 1.1764(14) 0.2285(19) 0.0689(7) 0.112(8) Uani 1 1 d . . . H3A H 1.1310 0.2060 0.0515 0.168 Uiso 1 1 calc R . . O4 O 0.7204(9) 0.2456(13) 0.0628(5) 0.065(4) Uani 1 1 d . . . H4 H 0.7053 0.3100 0.0668 0.097 Uiso 1 1 calc R . . C18 C 1.1800(8) 0.1834(12) 0.1811(5) 0.027(3) Uani 1 1 d . . . C19 C 1.2217(9) 0.0061(17) 0.1750(7) 0.051(5) Uani 1 1 d . . . H19 H 1.2508 -0.0563 0.1662 0.061 Uiso 1 1 calc R . . C20 C 1.1633(10) 0.0107(12) 0.2038(6) 0.037(4) Uani 1 1 d . . . H20 H 1.1426 -0.0491 0.2197 0.044 Uiso 1 1 calc R . . C21 C 1.2865(10) 0.1480(14) 0.1276(6) 0.037(4) Uani 1 1 d . . . H21A H 1.3381 0.1008 0.1324 0.044 Uiso 1 1 calc R . . H21B H 1.3056 0.2240 0.1345 0.044 Uiso 1 1 calc R . . C22 C 1.2409(12) 0.1396(17) 0.0761(8) 0.055(5) Uani 1 1 d . . . C23 C 1.2106(17) 0.027(2) 0.0633(7) 0.082(9) Uani 1 1 d . . . H23A H 1.1715 0.0034 0.0845 0.123 Uiso 1 1 calc R . . H23B H 1.2601 -0.0225 0.0670 0.123 Uiso 1 1 calc R . . H23C H 1.1804 0.0253 0.0299 0.123 Uiso 1 1 calc R . . C24 C 1.3135(19) 0.1718(19) 0.0459(9) 0.083(8) Uani 1 1 d . . . H24A H 1.3551 0.1122 0.0474 0.124 Uiso 1 1 calc R . . H24B H 1.3430 0.2379 0.0594 0.124 Uiso 1 1 calc R . . H24C H 1.2868 0.1849 0.0124 0.124 Uiso 1 1 calc R . . C25 C 1.0697(10) 0.1561(13) 0.2324(6) 0.041(4) Uani 1 1 d . . . H25A H 1.0736 0.2358 0.2373 0.049 Uiso 1 1 calc R . . H25B H 1.0773 0.1205 0.2642 0.049 Uiso 1 1 calc R . . C26 C 0.9810(9) 0.1264(13) 0.2028(7) 0.038(4) Uani 1 1 d . . . H26A H 0.9710 0.1694 0.1728 0.046 Uiso 1 1 calc R . . H26B H 0.9807 0.0484 0.1940 0.046 Uiso 1 1 calc R . . C27 C 0.9079(8) 0.1483(13) 0.2308(5) 0.029(3) Uani 1 1 d . . . H27A H 0.9171 0.1051 0.2607 0.035 Uiso 1 1 calc R . . H27B H 0.9071 0.2263 0.2393 0.035 Uiso 1 1 calc R . . C28 C 0.7719(8) 0.1864(11) 0.1754(5) 0.021(3) Uani 1 1 d . . . C29 C 0.7226(10) 0.0167(15) 0.1621(6) 0.044(4) Uani 1 1 d . . . H29 H 0.6870 -0.0431 0.1503 0.053 Uiso 1 1 calc R . . C30 C 0.7955(9) 0.0107(11) 0.1926(6) 0.031(3) Uani 1 1 d . . . H30 H 0.8229 -0.0533 0.2066 0.037 Uiso 1 1 calc R . . C31 C 0.6325(9) 0.1694(12) 0.1157(6) 0.032(3) Uani 1 1 d . . . H31A H 0.6187 0.2435 0.1258 0.039 Uiso 1 1 calc R . . H31B H 0.5816 0.1227 0.1163 0.039 Uiso 1 1 calc R . . C32 C 0.6503(11) 0.1739(14) 0.0652(6) 0.041(4) Uani 1 1 d . . . C33 C 0.6735(14) 0.0628(19) 0.0470(8) 0.062(6) Uani 1 1 d . . . H33A H 0.6742 0.0673 0.0126 0.094 Uiso 1 1 calc R . . H33B H 0.6307 0.0089 0.0527 0.094 Uiso 1 1 calc R . . H33C H 0.7304 0.0408 0.0641 0.094 Uiso 1 1 calc R . . C34 C 0.5675(15) 0.2183(19) 0.0340(7) 0.066(6) Uani 1 1 d . . . H34A H 0.5587 0.2940 0.0428 0.100 Uiso 1 1 calc R . . H34B H 0.5183 0.1742 0.0392 0.100 Uiso 1 1 calc R . . H34C H 0.5728 0.2148 0.0001 0.100 Uiso 1 1 calc R . . O5 O 0.8895(13) 0.5047(18) 0.0905(8) 0.048(6) Uani 0.57(2) 1 d PDU A 1 H5 H 0.9237 0.5549 0.0865 0.073 Uiso 0.57(2) 1 calc PR A 1 C35 C 0.937(2) 0.401(3) 0.0991(15) 0.067(11) Uani 0.57(2) 1 d PDU A 1 H35A H 0.9989 0.4143 0.1003 0.100 Uiso 0.57(2) 1 calc PR A 1 H35B H 0.9165 0.3496 0.0731 0.100 Uiso 0.57(2) 1 calc PR A 1 H35C H 0.9287 0.3696 0.1297 0.100 Uiso 0.57(2) 1 calc PR A 1 O5' O 0.9387(13) 0.576(2) 0.0077(9) 0.032(7) Uani 0.43(2) 1 d PDU A 2 H5' H 0.9172 0.6190 -0.0140 0.048 Uiso 0.43(2) 1 calc PR A 2 C35' C 0.873(4) 0.547(6) 0.038(2) 0.102(18) Uani 0.43(2) 1 d PDU A 2 H35D H 0.8967 0.5603 0.0715 0.153 Uiso 0.43(2) 1 calc PR A 2 H35E H 0.8573 0.4701 0.0331 0.153 Uiso 0.43(2) 1 calc PR A 2 H35F H 0.8216 0.5922 0.0280 0.153 Uiso 0.43(2) 1 calc PR A 2 O6 O 0.9753(16) 0.791(2) -0.0108(12) 0.063(8) Uani 0.50 1 d P . . O7 O 1.108(2) 0.843(4) -0.060(2) 0.16(2) Uani 0.50 1 d P . . P1 P 0.0169(2) 0.8551(3) 0.30195(13) 0.0253(7) Uani 1 1 d D . . F1 F 0.1170(6) 0.8550(10) 0.3007(4) 0.068(3) Uani 1 1 d D . . F2 F 0.0144(8) 0.7245(7) 0.3013(4) 0.069(3) Uani 1 1 d D . . F3 F 0.0385(7) 0.8530(8) 0.3579(3) 0.054(3) Uani 1 1 d D . . F4 F -0.0820(6) 0.8558(10) 0.3033(4) 0.069(4) Uani 1 1 d D . . F5 F 0.0184(7) 0.9836(7) 0.3052(4) 0.062(3) Uani 1 1 d D . . F6 F -0.0038(6) 0.8582(10) 0.2452(3) 0.055(3) Uani 1 1 d D . . P2 P 0.0363(2) 0.3553(3) 0.36691(15) 0.0301(8) Uani 1 1 d DU . . F7 F -0.0403(15) 0.3668(19) 0.3962(9) 0.101(8) Uani 0.73(3) 1 d PDU B 1 F8 F 0.0230(13) 0.4786(10) 0.3500(8) 0.073(6) Uani 0.73(3) 1 d PDU B 1 F9 F -0.0347(13) 0.3218(16) 0.3236(7) 0.084(6) Uani 0.73(3) 1 d PDU B 1 F10 F 0.1078(14) 0.3447(18) 0.3355(9) 0.092(7) Uani 0.73(3) 1 d PDU B 1 F11 F 0.0481(14) 0.2317(10) 0.3810(10) 0.090(7) Uani 0.73(3) 1 d PDU B 1 F12 F 0.1026(17) 0.3886(19) 0.4126(7) 0.113(8) Uani 0.73(3) 1 d PDU B 1 F7' F -0.0652(10) 0.350(3) 0.361(2) 0.079(14) Uani 0.27(3) 1 d PDU B 2 F8' F 0.032(3) 0.475(2) 0.3445(19) 0.092(15) Uani 0.27(3) 1 d PDU B 2 F9' F 0.026(4) 0.311(4) 0.3142(9) 0.101(15) Uani 0.27(3) 1 d PDU B 2 F10' F 0.1366(11) 0.356(3) 0.370(2) 0.071(13) Uani 0.27(3) 1 d PDU B 2 F11' F 0.042(3) 0.2341(18) 0.3855(18) 0.072(14) Uani 0.27(3) 1 d PDU B 2 F12' F 0.043(4) 0.401(4) 0.4189(9) 0.097(15) Uani 0.27(3) 1 d PDU B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.0180(2) 0.0208(3) 0.0250(3) 0.0014(2) 0.00796(19) 0.00115(19) Au2 0.0189(2) 0.0205(3) 0.0347(3) -0.0003(2) 0.0132(2) 0.0004(2) N1 0.023(6) 0.038(7) 0.038(8) 0.000(6) 0.021(5) 0.007(5) N2 0.026(6) 0.016(6) 0.039(7) -0.004(5) 0.014(5) -0.003(4) N3 0.021(5) 0.015(6) 0.032(7) 0.001(5) 0.005(5) 0.003(4) N4 0.017(5) 0.023(6) 0.026(6) 0.003(5) 0.006(5) -0.004(4) O1 0.054(9) 0.130(16) 0.075(11) -0.041(11) 0.014(8) -0.032(9) O2 0.035(6) 0.072(9) 0.042(7) -0.003(7) 0.016(5) 0.025(6) C1 0.037(6) 0.011(5) 0.041(7) 0.006(5) 0.004(6) 0.012(5) C2 0.044(9) 0.013(7) 0.066(12) 0.003(7) 0.032(9) -0.010(6) C3 0.042(9) 0.024(8) 0.050(11) 0.002(7) 0.030(8) -0.002(6) C4 0.023(6) 0.025(7) 0.034(8) 0.001(7) 0.019(6) -0.002(5) C5 0.032(8) 0.057(11) 0.049(11) -0.018(10) 0.009(8) 0.000(8) C6 0.078(14) 0.096(18) 0.029(10) -0.011(11) 0.032(10) -0.008(13) C7 0.15(3) 0.11(2) 0.055(15) 0.042(16) 0.021(16) 0.07(2) C8 0.027(7) 0.033(8) 0.035(9) 0.000(7) 0.022(6) 0.006(6) C9 0.022(7) 0.042(9) 0.028(8) 0.005(7) 0.011(6) 0.007(6) C10 0.018(6) 0.024(7) 0.031(8) 0.005(6) 0.003(5) -0.005(5) C11 0.053(9) 0.016(7) 0.029(8) 0.012(6) 0.027(7) -0.001(6) C12 0.042(8) 0.015(7) 0.034(9) 0.001(6) 0.007(7) -0.006(6) C13 0.036(7) 0.007(6) 0.029(8) -0.002(5) 0.002(6) 0.005(5) C14 0.016(6) 0.022(7) 0.030(8) -0.008(6) 0.011(5) 0.002(5) C15 0.031(8) 0.044(10) 0.031(9) -0.001(8) 0.009(6) 0.007(7) C16 0.079(14) 0.045(12) 0.061(14) 0.008(10) 0.023(11) -0.019(10) C17 0.037(9) 0.090(16) 0.044(11) -0.004(11) -0.012(8) 0.020(10) N5 0.026(6) 0.010(5) 0.046(8) -0.004(5) 0.013(5) 0.004(4) N6 0.043(8) 0.030(7) 0.049(9) 0.001(6) 0.022(7) -0.010(6) N7 0.019(5) 0.018(6) 0.047(8) -0.005(6) 0.008(5) -0.001(4) N8 0.032(6) 0.018(6) 0.041(8) 0.006(5) 0.019(6) 0.001(5) O3 0.109(15) 0.148(19) 0.081(14) 0.025(13) 0.021(11) 0.075(14) O4 0.076(10) 0.075(10) 0.043(8) 0.010(8) 0.009(7) -0.038(8) C18 0.013(6) 0.027(7) 0.044(9) 0.004(6) 0.017(6) 0.010(5) C19 0.016(7) 0.071(13) 0.070(13) 0.003(11) 0.022(8) 0.006(7) C20 0.045(9) 0.015(7) 0.051(11) 0.009(7) 0.012(8) 0.002(6) C21 0.034(8) 0.039(9) 0.043(9) 0.000(8) 0.020(7) 0.004(7) C22 0.044(10) 0.062(13) 0.062(13) -0.017(11) 0.017(9) 0.004(9) C23 0.13(2) 0.086(17) 0.028(11) -0.013(11) 0.018(12) -0.076(16) C24 0.14(2) 0.054(14) 0.072(16) -0.006(12) 0.054(16) -0.008(14) C25 0.049(9) 0.025(8) 0.058(11) 0.021(8) 0.037(8) 0.008(7) C26 0.025(7) 0.033(9) 0.060(11) -0.001(8) 0.018(7) 0.001(6) C27 0.024(6) 0.033(8) 0.032(8) -0.003(7) 0.009(6) 0.000(6) C28 0.018(6) 0.020(7) 0.031(8) -0.007(6) 0.018(6) -0.005(5) C29 0.033(8) 0.057(12) 0.041(10) -0.006(9) 0.004(7) -0.016(8) C30 0.039(8) 0.005(6) 0.050(10) -0.010(6) 0.011(7) 0.007(5) C31 0.035(8) 0.026(8) 0.039(9) -0.014(7) 0.014(7) -0.006(6) C32 0.044(9) 0.038(10) 0.042(10) -0.007(8) 0.013(8) -0.014(7) C33 0.064(12) 0.073(15) 0.053(13) -0.027(12) 0.017(10) 0.002(11) C34 0.082(15) 0.067(15) 0.041(12) 0.002(11) -0.012(11) 0.003(12) O5 0.036(11) 0.064(14) 0.052(14) 0.001(12) 0.026(10) 0.000(9) C35 0.05(2) 0.07(2) 0.08(3) -0.02(2) 0.028(19) 0.013(15) O5' 0.019(11) 0.033(14) 0.044(16) 0.001(12) 0.006(10) -0.008(9) C35' 0.08(3) 0.12(4) 0.12(4) 0.02(4) 0.06(3) -0.03(3) O6 0.045(14) 0.040(15) 0.10(2) 0.019(15) 0.007(15) 0.017(11) O7 0.037(18) 0.21(5) 0.25(6) 0.01(4) 0.08(3) -0.02(2) P1 0.0244(16) 0.0224(18) 0.0313(19) 0.0006(17) 0.0111(14) -0.0031(14) F1 0.035(5) 0.095(9) 0.074(8) -0.017(7) 0.009(5) 0.000(6) F2 0.101(9) 0.025(6) 0.080(8) -0.015(6) 0.018(7) -0.003(5) F3 0.084(8) 0.047(6) 0.033(5) -0.008(5) 0.016(5) -0.010(6) F4 0.036(5) 0.102(10) 0.074(8) -0.041(8) 0.022(5) -0.012(6) F5 0.083(8) 0.029(6) 0.070(8) 0.012(5) 0.001(6) 0.000(5) F6 0.040(5) 0.094(9) 0.029(5) 0.008(6) 0.000(4) -0.003(5) P2 0.0237(17) 0.0262(19) 0.042(2) 0.0061(19) 0.0099(15) -0.0010(15) F7 0.099(13) 0.110(16) 0.119(16) 0.020(15) 0.087(13) 0.020(13) F8 0.058(11) 0.031(6) 0.129(16) 0.030(8) 0.012(10) 0.005(7) F9 0.074(11) 0.079(12) 0.088(11) -0.009(10) -0.017(9) -0.029(11) F10 0.072(11) 0.092(14) 0.136(17) 0.024(14) 0.081(12) 0.018(12) F11 0.053(13) 0.038(7) 0.18(2) 0.043(10) 0.031(12) 0.005(8) F12 0.122(16) 0.119(16) 0.074(11) 0.021(11) -0.046(10) -0.041(15) F7' 0.021(8) 0.04(2) 0.18(4) -0.01(3) 0.007(17) 0.013(13) F8' 0.09(3) 0.042(15) 0.16(4) 0.057(19) 0.06(3) 0.033(19) F9' 0.13(3) 0.11(3) 0.057(15) -0.016(18) 0.02(2) -0.02(4) F10' 0.024(8) 0.04(2) 0.16(4) 0.00(3) 0.028(17) -0.001(14) F11' 0.04(2) 0.042(14) 0.13(3) 0.047(19) 0.00(3) 0.002(18) F12' 0.10(3) 0.13(3) 0.060(15) -0.024(19) 0.01(2) 0.03(3) _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 C11 1.966(14) . ? Au1 C28 2.059(13) . ? Au2 C1 1.980(14) . ? Au2 C18 2.027(14) . ? N1 C1 1.380(19) . ? N1 C2 1.405(19) . ? N1 C4 1.447(16) . ? N2 C1 1.375(18) . ? N2 C3 1.377(18) . ? N2 C8 1.481(16) . ? N3 C11 1.375(19) . ? N3 C13 1.403(16) . ? N3 C10 1.457(16) . ? N4 C12 1.374(18) . ? N4 C11 1.394(18) . ? N4 C14 1.448(17) . ? O1 C5 1.45(2) . ? O2 C15 1.430(18) . ? C2 C3 1.37(2) . ? C4 C5 1.49(2) . ? C5 C6 1.49(2) . ? C5 C7 1.57(3) . ? C8 C9 1.531(19) . ? C9 C10 1.570(17) . ? C12 C13 1.36(2) . ? C14 C15 1.513(19) . ? C15 C16 1.53(2) . ? C15 C17 1.57(2) . ? N5 C18 1.354(16) . ? N5 C19 1.41(2) . ? N5 C21 1.461(18) . ? N6 C18 1.321(18) . ? N6 C20 1.400(19) . ? N6 C25 1.481(18) . ? N7 C28 1.297(18) . ? N7 C30 1.389(17) . ? N7 C27 1.498(18) . ? N8 C28 1.369(18) . ? N8 C29 1.40(2) . ? N8 C31 1.48(2) . ? O3 C22 1.48(2) . ? O4 C32 1.426(19) . ? C19 C20 1.34(2) . ? C21 C22 1.51(3) . ? C22 C23 1.49(3) . ? C22 C24 1.60(3) . ? C25 C26 1.54(2) . ? C26 C27 1.539(18) . ? C29 C30 1.31(2) . ? C31 C32 1.51(2) . ? C32 C33 1.53(3) . ? C32 C34 1.54(3) . ? O5 C35 1.48(3) . ? O5' C35' 1.50(3) . ? P1 F3 1.562(9) . ? P1 F4 1.572(9) . ? P1 F5 1.581(9) . ? P1 F6 1.583(9) . ? P1 F1 1.590(9) . ? P1 F2 1.604(9) . ? P2 F12' 1.562(17) . ? P2 F9 1.562(13) . ? P2 F10 1.565(11) . ? P2 F12 1.567(13) . ? P2 F9' 1.571(17) . ? P2 F10' 1.572(15) . ? P2 F11 1.573(11) . ? P2 F11' 1.577(15) . ? P2 F7' 1.584(15) . ? P2 F8 1.591(11) . ? P2 F7 1.592(12) . ? P2 F8' 1.595(15) . ? 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 C11 Au1 C28 173.8(5) . . ? C1 Au2 C18 172.9(6) . . ? C1 N1 C2 111.6(11) . . ? C1 N1 C4 125.5(12) . . ? C2 N1 C4 122.9(12) . . ? C1 N2 C3 114.2(11) . . ? C1 N2 C8 122.5(12) . . ? C3 N2 C8 123.2(12) . . ? C11 N3 C13 112.9(11) . . ? C11 N3 C10 123.8(11) . . ? C13 N3 C10 123.2(11) . . ? C12 N4 C11 111.1(12) . . ? C12 N4 C14 124.1(12) . . ? C11 N4 C14 124.8(12) . . ? N2 C1 N1 101.9(11) . . ? N2 C1 Au2 129.3(11) . . ? N1 C1 Au2 128.7(10) . . ? C3 C2 N1 106.8(12) . . ? C2 C3 N2 105.1(13) . . ? N1 C4 C5 116.0(12) . . ? O1 C5 C6 110.3(16) . . ? O1 C5 C4 107.9(15) . . ? C6 C5 C4 108.9(14) . . ? O1 C5 C7 111.9(19) . . ? C6 C5 C7 108.2(19) . . ? C4 C5 C7 109.5(16) . . ? N2 C8 C9 108.2(12) . . ? C8 C9 C10 110.6(11) . . ? N3 C10 C9 109.0(11) . . ? N3 C11 N4 102.4(11) . . ? N3 C11 Au1 128.4(11) . . ? N4 C11 Au1 129.3(12) . . ? C13 C12 N4 108.9(13) . . ? C12 C13 N3 104.6(12) . . ? N4 C14 C15 112.9(10) . . ? O2 C15 C14 109.8(13) . . ? O2 C15 C16 109.6(14) . . ? C14 C15 C16 113.5(14) . . ? O2 C15 C17 105.9(14) . . ? C14 C15 C17 105.5(13) . . ? C16 C15 C17 112.1(16) . . ? C18 N5 C19 111.7(12) . . ? C18 N5 C21 125.2(12) . . ? C19 N5 C21 123.1(12) . . ? C18 N6 C20 111.3(13) . . ? C18 N6 C25 124.9(13) . . ? C20 N6 C25 123.8(12) . . ? C28 N7 C30 112.2(12) . . ? C28 N7 C27 123.8(12) . . ? C30 N7 C27 123.9(12) . . ? C28 N8 C29 107.5(12) . . ? C28 N8 C31 125.9(12) . . ? C29 N8 C31 126.5(13) . . ? N6 C18 N5 104.8(13) . . ? N6 C18 Au2 126.4(10) . . ? N5 C18 Au2 128.5(10) . . ? C20 C19 N5 104.2(14) . . ? C19 C20 N6 107.9(14) . . ? N5 C21 C22 111.0(13) . . ? O3 C22 C23 118(2) . . ? O3 C22 C21 106.3(16) . . ? C23 C22 C21 112.1(18) . . ? O3 C22 C24 106.6(19) . . ? C23 C22 C24 109.2(17) . . ? C21 C22 C24 103.7(16) . . ? N6 C25 C26 109.5(14) . . ? C27 C26 C25 111.9(14) . . ? N7 C27 C26 109.0(12) . . ? N7 C28 N8 106.1(12) . . ? N7 C28 Au1 128.0(10) . . ? N8 C28 Au1 125.4(10) . . ? C30 C29 N8 108.5(14) . . ? C29 C30 N7 105.7(14) . . ? N8 C31 C32 112.2(12) . . ? O4 C32 C31 110.3(14) . . ? O4 C32 C33 107.5(15) . . ? C31 C32 C33 112.6(15) . . ? O4 C32 C34 109.9(16) . . ? C31 C32 C34 105.8(15) . . ? C33 C32 C34 110.6(16) . . ? F3 P1 F4 90.6(6) . . ? F3 P1 F5 87.6(6) . . ? F4 P1 F5 89.8(6) . . ? F3 P1 F6 179.2(6) . . ? F4 P1 F6 90.0(6) . . ? F5 P1 F6 91.9(6) . . ? F3 P1 F1 89.3(6) . . ? F4 P1 F1 179.7(7) . . ? F5 P1 F1 89.9(6) . . ? F6 P1 F1 90.1(6) . . ? F3 P1 F2 89.8(6) . . ? F4 P1 F2 89.0(7) . . ? F5 P1 F2 177.1(7) . . ? F6 P1 F2 90.7(6) . . ? F1 P1 F2 91.3(7) . . ? F12' P2 F9 139(2) . . ? F12' P2 F10 129(2) . . ? F9 P2 F10 91.2(11) . . ? F12' P2 F12 37.1(16) . . ? F9 P2 F12 176.1(12) . . ? F10 P2 F12 92.7(12) . . ? F12' P2 F9' 178(2) . . ? F9 P2 F9' 38.9(17) . . ? F10 P2 F9' 52.8(19) . . ? F12 P2 F9' 145(2) . . ? F12' P2 F10' 92.2(17) . . ? F9 P2 F10' 129(2) . . ? F10 P2 F10' 38.0(17) . . ? F12 P2 F10' 55.2(19) . . ? F9' P2 F10' 89.8(17) . . ? F12' P2 F11 97(3) . . ? F9 P2 F11 89.0(11) . . ? F10 P2 F11 90.0(10) . . ? F12 P2 F11 90.6(11) . . ? F9' P2 F11 84(3) . . ? F10' P2 F11 85(2) . . ? F12' P2 F11' 91.9(16) . . ? F9 P2 F11' 90(2) . . ? F10 P2 F11' 96(2) . . ? F12 P2 F11' 89(2) . . ? F9' P2 F11' 89.0(16) . . ? F10' P2 F11' 89.2(14) . . ? F11 P2 F11' 6(2) . . ? F12' P2 F7' 91.3(17) . . ? F9 P2 F7' 47.9(19) . . ? F10 P2 F7' 139(2) . . ? F12 P2 F7' 128(2) . . ? F9' P2 F7' 86.7(17) . . ? F10' P2 F7' 176.4(19) . . ? F11 P2 F7' 93(2) . . ? F11' P2 F7' 89.9(15) . . ? F12' P2 F8 86(2) . . ? F9 P2 F8 88.6(9) . . ? F10 P2 F8 88.7(10) . . ? F12 P2 F8 91.9(10) . . ? F9' P2 F8 93(2) . . ? F10' P2 F8 95(2) . . ? F11 P2 F8 177.2(12) . . ? F11' P2 F8 175(2) . . ? F7' P2 F8 86.0(19) . . ? F12' P2 F7 53.8(19) . . ? F9 P2 F7 85.8(11) . . ? F10 P2 F7 176.8(12) . . ? F12 P2 F7 90.3(12) . . ? F9' P2 F7 124(2) . . ? F10' P2 F7 145(2) . . ? F11 P2 F7 91.1(10) . . ? F11' P2 F7 85(2) . . ? F7' P2 F7 38.1(17) . . ? F8 P2 F7 90.1(10) . . ? F12' P2 F8' 92.1(16) . . ? F9 P2 F8' 87(2) . . ? F10 P2 F8' 80(2) . . ? F12 P2 F8' 94(2) . . ? F9' P2 F8' 87.0(16) . . ? F10' P2 F8' 89.3(15) . . ? F11 P2 F8' 170(2) . . ? F11' P2 F8' 175.7(18) . . ? F7' P2 F8' 91.4(15) . . ? F8 P2 F8' 8(2) . . ? F7 P2 F8' 98(2) . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 3.155 _refine_diff_density_min -6.708 _refine_diff_density_rms 0.274 #===END