# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Bochmann, Manfred' _publ_contact_author_email M.Bochmann@uea.ac.uk _publ_section_title ; Synthesis and Structures of Gold Perfluorophthalimido Complexes ; _publ_author_name M.Bochmann data_nickys1 _database_code_depnum_ccdc_archive 'CCDC 791405' #TrackingRef '- combined.cif' _audit_creation_method 'SHELXL-97 and CrysAlisPro RED' _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 2' _chemical_melting_point ? _chemical_formula_structural tetrafluorophthalimide _chemical_formula_moiety 'C8 H F4 N O2' _chemical_formula_sum 'C8 H F4 N O2' _chemical_formula_weight 219.10 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.0520(5) _cell_length_b 5.4998(2) _cell_length_c 11.4291(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.626(4) _cell_angle_gamma 90.00 _cell_volume 755.09(5) _cell_formula_units_Z 4 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'flat prism' _exptl_crystal_colour 'very pale yellow' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.927 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 432 _exptl_absorpt_coefficient_mu 0.203 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.926 _exptl_absorpt_correction_T_max 1.069 _exptl_absorpt_process_details ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_reflns_number 13776 _diffrn_reflns_av_R_equivalents 0.0747 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1334 _reflns_number_gt 1181 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlisPro CCD, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_cell_refinement ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_data_reduction ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0497P)^2^+0.3735P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1334 _refine_ls_number_parameters 140 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1028 _refine_ls_wR_factor_gt 0.0970 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.129 _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 C1 C 0.19844(19) 0.2607(4) 0.56131(19) 0.0232(5) Uani 1 1 d . . . F1 F 0.12080(11) 0.0888(2) 0.57192(12) 0.0335(4) Uani 1 1 d . . . C2 C 0.29648(19) 0.2491(4) 0.63233(19) 0.0235(5) Uani 1 1 d . . . F2 F 0.31228(12) 0.0681(2) 0.71040(12) 0.0332(4) Uani 1 1 d . . . C3 C 0.37894(18) 0.4211(4) 0.62467(19) 0.0247(5) Uani 1 1 d . . . F3 F 0.47309(11) 0.4032(3) 0.69404(12) 0.0349(4) Uani 1 1 d . . . C4 C 0.36446(19) 0.6116(4) 0.5452(2) 0.0231(5) Uani 1 1 d . . . F4 F 0.44564(11) 0.7757(3) 0.53992(12) 0.0362(4) Uani 1 1 d . . . C5 C 0.26733(18) 0.6218(4) 0.47420(18) 0.0214(5) Uani 1 1 d . . . C6 C 0.22808(19) 0.7971(4) 0.38029(19) 0.0252(5) Uani 1 1 d . . . O6 O 0.27322(15) 0.9785(3) 0.34894(14) 0.0337(4) Uani 1 1 d . . . N7 N 0.12502(17) 0.7098(4) 0.33578(18) 0.0277(5) Uani 1 1 d . . . C8 C 0.0930(2) 0.5004(4) 0.39040(19) 0.0244(5) Uani 1 1 d . . . O8 O 0.00848(14) 0.3854(3) 0.36607(14) 0.0325(4) Uani 1 1 d . . . C9 C 0.18474(18) 0.4463(4) 0.48146(18) 0.0214(5) Uani 1 1 d . . . H7 H 0.085(2) 0.770(5) 0.284(3) 0.038(8) Uiso 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 C1 0.0270(12) 0.0195(11) 0.0238(11) -0.0035(9) 0.0057(9) -0.0038(10) F1 0.0347(8) 0.0258(7) 0.0398(8) 0.0024(6) 0.0019(6) -0.0103(6) C2 0.0307(13) 0.0202(12) 0.0197(11) 0.0006(9) 0.0026(9) 0.0047(10) F2 0.0411(8) 0.0265(7) 0.0312(8) 0.0088(6) -0.0011(6) 0.0029(6) C3 0.0222(12) 0.0283(12) 0.0230(12) -0.0045(9) -0.0016(9) 0.0019(10) F3 0.0277(8) 0.0415(9) 0.0337(8) 0.0006(6) -0.0090(6) 0.0012(6) C4 0.0215(11) 0.0242(12) 0.0239(11) -0.0055(9) 0.0043(9) -0.0043(9) F4 0.0313(8) 0.0372(8) 0.0400(9) 0.0000(6) 0.0024(6) -0.0107(7) C5 0.0247(12) 0.0196(11) 0.0205(11) -0.0043(9) 0.0056(9) 0.0007(9) C6 0.0321(13) 0.0236(12) 0.0206(11) -0.0020(10) 0.0073(10) 0.0034(11) O6 0.0479(11) 0.0247(9) 0.0293(9) 0.0047(7) 0.0082(8) -0.0031(8) N7 0.0317(12) 0.0292(11) 0.0211(10) 0.0018(9) -0.0039(9) 0.0056(10) C8 0.0256(12) 0.0264(12) 0.0211(11) -0.0051(10) 0.0018(9) 0.0024(10) O8 0.0281(9) 0.0392(10) 0.0292(9) -0.0042(8) -0.0037(7) -0.0057(8) C9 0.0232(12) 0.0209(11) 0.0202(11) -0.0045(9) 0.0028(9) 0.0005(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 C1 F1 1.343(2) . ? C1 C9 1.370(3) . ? C1 C2 1.380(3) . ? C2 F2 1.340(2) . ? C2 C3 1.380(3) . ? C3 F3 1.335(3) . ? C3 C4 1.389(3) . ? C4 F4 1.336(3) . ? C4 C5 1.370(3) . ? C5 C9 1.394(3) . ? C5 C6 1.491(3) . ? C6 O6 1.205(3) . ? C6 N7 1.389(3) . ? N7 C8 1.380(3) . ? N7 H7 0.80(3) . ? C8 O8 1.212(3) . ? C8 C9 1.486(3) . ? 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 F1 C1 C9 122.5(2) . . ? F1 C1 C2 118.95(19) . . ? C9 C1 C2 118.5(2) . . ? F2 C2 C1 119.7(2) . . ? F2 C2 C3 119.15(19) . . ? C1 C2 C3 121.2(2) . . ? F3 C3 C2 119.6(2) . . ? F3 C3 C4 120.0(2) . . ? C2 C3 C4 120.4(2) . . ? F4 C4 C5 122.7(2) . . ? F4 C4 C3 119.0(2) . . ? C5 C4 C3 118.3(2) . . ? C4 C5 C9 121.1(2) . . ? C4 C5 C6 131.2(2) . . ? C9 C5 C6 107.70(19) . . ? O6 C6 N7 126.1(2) . . ? O6 C6 C5 128.7(2) . . ? N7 C6 C5 105.23(19) . . ? C8 N7 C6 113.4(2) . . ? C8 N7 H7 120(2) . . ? C6 N7 H7 126(2) . . ? O8 C8 N7 126.3(2) . . ? O8 C8 C9 128.3(2) . . ? N7 C8 C9 105.3(2) . . ? C1 C9 C5 120.5(2) . . ? C1 C9 C8 131.2(2) . . ? C5 C9 C8 108.30(19) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N7 H7 O8 0.80(3) 2.07(3) 2.871(3) 171(3) 2 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.240 _refine_diff_density_min -0.230 _refine_diff_density_rms 0.050 #===END data_simonl17a _database_code_depnum_ccdc_archive 'CCDC 791406' #TrackingRef '- combined.cif' _audit_creation_method 'SHELXL-97 and CrysAlisPro RED' _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 4' _chemical_melting_point ? _chemical_formula_structural 'trimethyl silyl tetrafluorophthalimide' _chemical_formula_moiety 'C11 H9 F4 N O2 Si' _chemical_formula_sum 'C11 H9 F4 N O2 Si' _chemical_formula_weight 291.28 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.5135(8) _cell_length_b 24.759(2) _cell_length_c 10.7793(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.391(6) _cell_angle_gamma 90.00 _cell_volume 2538.3(3) _cell_formula_units_Z 8 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 0.231 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.967 _exptl_absorpt_correction_T_max 1.029 _exptl_absorpt_process_details ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_reflns_number 27063 _diffrn_reflns_av_R_equivalents 0.2034 _diffrn_reflns_av_sigmaI/netI 0.1570 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 20.00 _reflns_number_total 2357 _reflns_number_gt 1262 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlisPro CCD, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_cell_refinement ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_data_reduction ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0000P)^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 2357 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1449 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.0495 _refine_ls_wR_factor_gt 0.0388 _refine_ls_goodness_of_fit_ref 0.869 _refine_ls_restrained_S_all 0.869 _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 N1 N 0.2159(6) 0.3360(2) 0.9246(5) 0.0233(17) Uani 1 1 d . . . C2 C 0.1573(8) 0.2981(3) 1.0055(6) 0.023(2) Uani 1 1 d . . . O2 O 0.0911(6) 0.30821(16) 1.0967(4) 0.0352(16) Uani 1 1 d . . . C3 C 0.1998(7) 0.2437(3) 0.9605(6) 0.0208(19) Uani 1 1 d . . . C4 C 0.1626(8) 0.1924(3) 0.9998(6) 0.023(2) Uani 1 1 d . . . F4 F 0.0816(4) 0.18477(13) 1.0964(3) 0.0366(13) Uani 1 1 d . . . C5 C 0.2136(8) 0.1492(3) 0.9365(7) 0.028(2) Uani 1 1 d . . . F5 F 0.1796(4) 0.09913(15) 0.9692(3) 0.0428(13) Uani 1 1 d . . . C6 C 0.2985(9) 0.1558(3) 0.8347(7) 0.028(2) Uani 1 1 d . . . F6 F 0.3475(4) 0.11224(15) 0.7749(3) 0.0464(13) Uani 1 1 d . . . C7 C 0.3316(8) 0.2068(3) 0.7933(6) 0.028(2) Uani 1 1 d . . . F7 F 0.4123(4) 0.21246(13) 0.6932(3) 0.0403(13) Uani 1 1 d . . . C8 C 0.2818(8) 0.2511(3) 0.8565(6) 0.0215(19) Uani 1 1 d . . . C9 C 0.2960(8) 0.3101(3) 0.8347(6) 0.023(2) Uani 1 1 d . . . O9 O 0.3576(5) 0.33263(17) 0.7523(4) 0.0337(15) Uani 1 1 d . . . Si1 Si 0.2011(2) 0.40925(8) 0.93037(17) 0.0309(7) Uani 1 1 d . . . C1A C 0.0722(6) 0.4265(2) 1.0484(5) 0.038(2) Uani 1 1 d . . . H1A1 H -0.0170 0.4106 1.0262 0.057 Uiso 1 1 calc R . . H1A2 H 0.0624 0.4650 1.0529 0.057 Uiso 1 1 calc R . . H1A3 H 0.1039 0.4128 1.1276 0.057 Uiso 1 1 calc R . . C1B C 0.3782(7) 0.4350(2) 0.9718(5) 0.042(2) Uani 1 1 d . . . H1B1 H 0.4421 0.4258 0.9075 0.063 Uiso 1 1 calc R . . H1B2 H 0.4101 0.4190 1.0486 0.063 Uiso 1 1 calc R . . H1B3 H 0.3746 0.4735 0.9809 0.063 Uiso 1 1 calc R . . C1C C 0.1425(7) 0.4328(2) 0.7759(5) 0.036(2) Uani 1 1 d . . . H1C1 H 0.0505 0.4187 0.7568 0.054 Uiso 1 1 calc R . . H1C2 H 0.2071 0.4204 0.7150 0.054 Uiso 1 1 calc R . . H1C3 H 0.1393 0.4715 0.7751 0.054 Uiso 1 1 calc R . . N11 N 0.7230(7) 0.14556(19) 0.1347(6) 0.0274(18) Uani 1 1 d . . . C12 C 0.6674(8) 0.1803(3) 0.0449(7) 0.030(2) Uani 1 1 d . . . O12 O 0.6049(6) 0.16819(19) -0.0513(4) 0.0371(16) Uani 1 1 d . . . C13 C 0.7033(7) 0.2368(3) 0.0870(7) 0.0198(19) Uani 1 1 d . . . C14 C 0.6707(8) 0.2865(3) 0.0362(7) 0.025(2) Uani 1 1 d . . . F14 F 0.5930(4) 0.29257(14) -0.0685(3) 0.0411(12) Uani 1 1 d . . . C15 C 0.7225(8) 0.3322(3) 0.0982(7) 0.027(2) Uani 1 1 d . . . F15 F 0.6924(4) 0.38123(16) 0.0514(3) 0.0438(13) Uani 1 1 d . . . C16 C 0.8011(8) 0.3272(3) 0.2052(7) 0.031(2) Uani 1 1 d . . . F16 F 0.8500(4) 0.37228(15) 0.2613(3) 0.0450(13) Uani 1 1 d . . . C17 C 0.8304(8) 0.2770(3) 0.2555(6) 0.023(2) Uani 1 1 d . . . F17 F 0.9059(4) 0.27510(14) 0.3625(3) 0.0409(12) Uani 1 1 d . . . C18 C 0.7793(8) 0.2314(3) 0.1962(6) 0.021(2) Uani 1 1 d . . . C19 C 0.7966(8) 0.1731(3) 0.2292(7) 0.023(2) Uani 1 1 d . . . O19 O 0.8599(6) 0.15436(17) 0.3155(4) 0.0350(15) Uani 1 1 d . . . Si2 Si 0.6928(3) 0.07269(8) 0.12297(18) 0.0332(7) Uani 1 1 d . . . C2A C 0.7348(6) 0.0429(2) 0.2780(5) 0.044(2) Uani 1 1 d . . . H2A1 H 0.8335 0.0467 0.2964 0.066 Uiso 1 1 calc R . . H2A2 H 0.7104 0.0052 0.2775 0.066 Uiso 1 1 calc R . . H2A3 H 0.6821 0.0612 0.3401 0.066 Uiso 1 1 calc R . . C2B C 0.5049(7) 0.0643(2) 0.0855(5) 0.045(2) Uani 1 1 d . . . H2B1 H 0.4829 0.0814 0.0075 0.068 Uiso 1 1 calc R . . H2B2 H 0.4506 0.0805 0.1494 0.068 Uiso 1 1 calc R . . H2B3 H 0.4830 0.0265 0.0800 0.068 Uiso 1 1 calc R . . C2C C 0.8097(7) 0.0464(2) 0.0044(5) 0.044(2) Uani 1 1 d . . . H2C1 H 0.7869 0.0631 -0.0740 0.067 Uiso 1 1 calc R . . H2C2 H 0.7978 0.0080 -0.0026 0.067 Uiso 1 1 calc R . . H2C3 H 0.9055 0.0544 0.0276 0.067 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.023(5) 0.022(4) 0.025(4) 0.001(3) 0.006(3) 0.003(4) C2 0.017(6) 0.031(6) 0.022(5) 0.007(5) 0.000(4) 0.004(5) O2 0.047(4) 0.032(3) 0.027(3) 0.003(3) 0.017(3) 0.001(3) C3 0.015(5) 0.025(5) 0.022(5) 0.003(4) 0.003(4) 0.005(5) C4 0.018(6) 0.018(5) 0.033(5) 0.002(5) 0.005(4) -0.002(5) F4 0.039(3) 0.031(3) 0.041(2) 0.018(2) 0.020(3) -0.002(2) C5 0.029(7) 0.019(6) 0.036(6) 0.008(5) -0.004(5) -0.004(5) F5 0.046(4) 0.027(3) 0.056(3) 0.011(2) 0.002(2) 0.002(3) C6 0.036(7) 0.020(5) 0.029(5) -0.010(5) -0.007(5) 0.010(5) F6 0.056(4) 0.037(3) 0.047(3) -0.009(2) 0.008(2) 0.006(3) C7 0.030(6) 0.034(6) 0.022(5) 0.007(5) 0.015(4) -0.004(5) F7 0.045(3) 0.038(3) 0.038(2) 0.001(2) 0.018(3) 0.001(3) C8 0.024(6) 0.021(5) 0.019(5) -0.001(5) -0.003(4) -0.006(5) C9 0.019(6) 0.029(6) 0.021(5) 0.006(4) -0.003(5) -0.001(5) O9 0.038(4) 0.030(3) 0.033(3) 0.011(3) 0.009(3) -0.002(3) Si1 0.0304(19) 0.0285(15) 0.0337(14) -0.0019(11) 0.0011(13) -0.0004(14) C1A 0.041(6) 0.027(5) 0.046(5) -0.006(4) -0.002(5) 0.004(5) C1B 0.050(6) 0.029(5) 0.047(5) -0.003(4) -0.005(5) -0.017(5) C1C 0.034(6) 0.034(5) 0.040(5) 0.005(4) 0.007(4) 0.001(5) N11 0.029(5) 0.024(4) 0.028(4) 0.002(4) -0.006(4) 0.002(4) C12 0.024(7) 0.041(7) 0.024(6) -0.002(6) 0.007(5) -0.003(5) O12 0.052(5) 0.030(3) 0.029(3) -0.006(3) -0.009(3) -0.001(3) C13 0.013(5) 0.023(6) 0.023(5) 0.001(5) -0.001(4) 0.003(5) C14 0.013(6) 0.036(6) 0.026(5) -0.001(5) -0.001(4) -0.001(5) F14 0.042(3) 0.042(3) 0.039(3) 0.011(2) -0.007(3) 0.000(3) C15 0.022(7) 0.015(5) 0.043(6) -0.001(5) 0.003(5) 0.006(5) F15 0.051(4) 0.029(3) 0.051(3) 0.007(2) 0.002(3) 0.003(3) C16 0.021(6) 0.033(6) 0.037(6) -0.003(6) -0.004(5) -0.009(5) F16 0.051(4) 0.037(3) 0.047(3) -0.008(2) 0.003(3) -0.010(3) C17 0.021(6) 0.026(6) 0.023(5) 0.005(5) 0.001(4) 0.007(5) F17 0.039(3) 0.046(3) 0.037(3) -0.003(2) -0.014(2) -0.006(3) C18 0.022(6) 0.027(6) 0.015(5) -0.003(5) 0.000(4) 0.002(5) C19 0.015(6) 0.028(6) 0.027(6) -0.002(5) 0.002(5) 0.000(5) O19 0.040(4) 0.034(3) 0.030(3) 0.006(3) -0.018(3) 0.010(3) Si2 0.0297(18) 0.0290(14) 0.0410(15) -0.0047(12) 0.0014(13) 0.0008(14) C2A 0.048(7) 0.030(5) 0.054(5) 0.006(4) 0.007(5) -0.009(5) C2B 0.046(7) 0.022(5) 0.068(6) -0.014(4) 0.006(5) 0.005(5) C2C 0.062(7) 0.024(5) 0.048(5) -0.007(4) 0.025(5) -0.008(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N1 C9 1.402(7) . ? N1 C2 1.405(7) . ? N1 Si1 1.821(5) . ? C2 O2 1.207(6) . ? C2 C3 1.490(8) . ? C3 C4 1.386(8) . ? C3 C8 1.393(7) . ? C4 F4 1.323(7) . ? C4 C5 1.365(8) . ? C5 F5 1.331(6) . ? C5 C6 1.388(8) . ? C6 F6 1.346(6) . ? C6 C7 1.379(8) . ? C7 F7 1.347(6) . ? C7 C8 1.380(8) . ? C8 C9 1.488(8) . ? C9 O9 1.212(6) . ? Si1 C1A 1.838(5) . ? Si1 C1C 1.838(5) . ? Si1 C1B 1.847(6) . ? C1A H1A1 0.9600 . ? C1A H1A2 0.9600 . ? C1A H1A3 0.9600 . ? C1B H1B1 0.9600 . ? C1B H1B2 0.9600 . ? C1B H1B3 0.9600 . ? C1C H1C1 0.9600 . ? C1C H1C2 0.9600 . ? C1C H1C3 0.9600 . ? N11 C12 1.391(8) . ? N11 C19 1.400(8) . ? N11 Si2 1.831(5) . ? C12 O12 1.220(8) . ? C12 C13 1.506(9) . ? C13 C18 1.373(8) . ? C13 C14 1.378(9) . ? C14 F14 1.343(7) . ? C14 C15 1.397(9) . ? C15 F15 1.344(7) . ? C15 C16 1.364(9) . ? C16 F16 1.347(7) . ? C16 C17 1.381(9) . ? C17 F17 1.345(7) . ? C17 C18 1.381(8) . ? C18 C19 1.495(9) . ? C19 O19 1.190(7) . ? Si2 C2B 1.834(6) . ? Si2 C2C 1.834(5) . ? Si2 C2A 1.862(5) . ? C2A H2A1 0.9600 . ? C2A H2A2 0.9600 . ? C2A H2A3 0.9600 . ? C2B H2B1 0.9600 . ? C2B H2B2 0.9600 . ? C2B H2B3 0.9600 . ? C2C H2C1 0.9600 . ? C2C H2C2 0.9600 . ? C2C H2C3 0.9600 . ? 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 N1 C2 110.8(5) . . ? C9 N1 Si1 121.5(5) . . ? C2 N1 Si1 127.7(5) . . ? O2 C2 N1 126.1(7) . . ? O2 C2 C3 127.1(7) . . ? N1 C2 C3 106.7(6) . . ? C4 C3 C8 121.2(6) . . ? C4 C3 C2 130.9(6) . . ? C8 C3 C2 107.8(6) . . ? F4 C4 C5 120.1(6) . . ? F4 C4 C3 122.0(7) . . ? C5 C4 C3 117.9(7) . . ? F5 C5 C4 120.4(7) . . ? F5 C5 C6 117.9(7) . . ? C4 C5 C6 121.6(7) . . ? F6 C6 C7 119.6(7) . . ? F6 C6 C5 120.0(7) . . ? C7 C6 C5 120.4(7) . . ? F7 C7 C6 119.6(7) . . ? F7 C7 C8 121.5(7) . . ? C6 C7 C8 118.9(6) . . ? C7 C8 C3 120.0(6) . . ? C7 C8 C9 131.9(7) . . ? C3 C8 C9 108.1(6) . . ? O9 C9 N1 125.3(6) . . ? O9 C9 C8 128.0(7) . . ? N1 C9 C8 106.7(6) . . ? N1 Si1 C1A 108.0(3) . . ? N1 Si1 C1C 107.9(3) . . ? C1A Si1 C1C 111.1(3) . . ? N1 Si1 C1B 106.3(3) . . ? C1A Si1 C1B 111.9(3) . . ? C1C Si1 C1B 111.4(3) . . ? Si1 C1A H1A1 109.5 . . ? Si1 C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? Si1 C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? Si1 C1B H1B1 109.5 . . ? Si1 C1B H1B2 109.5 . . ? H1B1 C1B H1B2 109.5 . . ? Si1 C1B H1B3 109.5 . . ? H1B1 C1B H1B3 109.5 . . ? H1B2 C1B H1B3 109.5 . . ? Si1 C1C H1C1 109.5 . . ? Si1 C1C H1C2 109.5 . . ? H1C1 C1C H1C2 109.5 . . ? Si1 C1C H1C3 109.5 . . ? H1C1 C1C H1C3 109.5 . . ? H1C2 C1C H1C3 109.5 . . ? C12 N11 C19 112.4(6) . . ? C12 N11 Si2 120.4(6) . . ? C19 N11 Si2 127.3(5) . . ? O12 C12 N11 127.5(8) . . ? O12 C12 C13 125.9(8) . . ? N11 C12 C13 106.6(7) . . ? C18 C13 C14 122.4(8) . . ? C18 C13 C12 106.2(7) . . ? C14 C13 C12 131.4(7) . . ? F14 C14 C13 123.2(7) . . ? F14 C14 C15 119.4(7) . . ? C13 C14 C15 117.4(7) . . ? F15 C15 C16 120.4(8) . . ? F15 C15 C14 118.9(7) . . ? C16 C15 C14 120.7(8) . . ? F16 C16 C15 118.8(8) . . ? F16 C16 C17 120.3(7) . . ? C15 C16 C17 120.9(8) . . ? F17 C17 C16 117.9(7) . . ? F17 C17 C18 122.9(7) . . ? C16 C17 C18 119.2(7) . . ? C13 C18 C17 119.3(7) . . ? C13 C18 C19 110.5(7) . . ? C17 C18 C19 130.1(7) . . ? O19 C19 N11 127.9(8) . . ? O19 C19 C18 127.8(8) . . ? N11 C19 C18 104.3(6) . . ? N11 Si2 C2B 106.1(3) . . ? N11 Si2 C2C 107.5(3) . . ? C2B Si2 C2C 114.2(3) . . ? N11 Si2 C2A 107.4(3) . . ? C2B Si2 C2A 109.8(3) . . ? C2C Si2 C2A 111.4(3) . . ? Si2 C2A H2A1 109.5 . . ? Si2 C2A H2A2 109.5 . . ? H2A1 C2A H2A2 109.5 . . ? Si2 C2A H2A3 109.5 . . ? H2A1 C2A H2A3 109.5 . . ? H2A2 C2A H2A3 109.5 . . ? Si2 C2B H2B1 109.5 . . ? Si2 C2B H2B2 109.5 . . ? H2B1 C2B H2B2 109.5 . . ? Si2 C2B H2B3 109.5 . . ? H2B1 C2B H2B3 109.5 . . ? H2B2 C2B H2B3 109.5 . . ? Si2 C2C H2C1 109.5 . . ? Si2 C2C H2C2 109.5 . . ? H2C1 C2C H2C2 109.5 . . ? Si2 C2C H2C3 109.5 . . ? H2C1 C2C H2C3 109.5 . . ? H2C2 C2C H2C3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.196 _refine_diff_density_min -0.195 _refine_diff_density_rms 0.046 #===END data_nickys11a _database_code_depnum_ccdc_archive 'CCDC 791407' #TrackingRef '- combined.cif' _audit_creation_method 'SHELXL-97 and CrysAlisPro RED' _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 5' _chemical_melting_point ? _chemical_formula_structural '[Me3Sn-tetrafluorophthalimide]' _chemical_formula_moiety 'C11 H9 F4 N O2 Sn' _chemical_formula_sum 'C11 H9 F4 N O2 Sn' _chemical_formula_weight 381.88 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' 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' Sn Sn -0.6537 1.4246 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.1926(6) _cell_length_b 6.6264(2) _cell_length_c 20.1512(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.257(3) _cell_angle_gamma 90.00 _cell_volume 2562.76(14) _cell_formula_units_Z 8 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.980 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 2.039 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.873 _exptl_absorpt_correction_T_max 1.112 _exptl_absorpt_process_details ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_reflns_number 48849 _diffrn_reflns_av_R_equivalents 0.0699 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 30.00 _reflns_number_total 7468 _reflns_number_gt 5577 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlisPro CCD, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_cell_refinement ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_data_reduction ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Johnson, 1976 and Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0271P)^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 7468 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0500 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0583 _refine_ls_wR_factor_gt 0.0555 _refine_ls_goodness_of_fit_ref 0.912 _refine_ls_restrained_S_all 0.912 _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 Sn1 Sn 0.272841(9) 0.99131(2) 0.419118(8) 0.01945(5) Uani 1 1 d . . . C1A C 0.34795(14) 1.0624(4) 0.34658(13) 0.0267(6) Uani 1 1 d . . . H1A1 H 0.3758 0.9453 0.3375 0.040 Uiso 1 1 calc R . . H1A2 H 0.3773 1.1692 0.3626 0.040 Uiso 1 1 calc R . . H1A3 H 0.3249 1.1050 0.3066 0.040 Uiso 1 1 calc R . . C1B C 0.19712(15) 0.7653(4) 0.40060(13) 0.0268(6) Uani 1 1 d . . . H1B1 H 0.1623 0.8171 0.3708 0.040 Uiso 1 1 calc R . . H1B2 H 0.1757 0.7266 0.4416 0.040 Uiso 1 1 calc R . . H1B3 H 0.2191 0.6499 0.3809 0.040 Uiso 1 1 calc R . . C1C C 0.23748(15) 1.2348(3) 0.47891(13) 0.0261(6) Uani 1 1 d . . . H1C1 H 0.2714 1.2628 0.5129 0.039 Uiso 1 1 calc R . . H1C2 H 0.1940 1.1991 0.4991 0.039 Uiso 1 1 calc R . . H1C3 H 0.2311 1.3525 0.4518 0.039 Uiso 1 1 calc R . . N1 N 0.33663(11) 0.8211(3) 0.48945(10) 0.0202(4) Uani 1 1 d . . . C2 C 0.36160(13) 0.6352(3) 0.46820(13) 0.0211(5) Uani 1 1 d . . . O2 O 0.35321(10) 0.5648(2) 0.41343(9) 0.0273(4) Uani 1 1 d . . . C3 C 0.40211(13) 0.5435(3) 0.52393(13) 0.0209(5) Uani 1 1 d . . . C4 C 0.43534(15) 0.3614(4) 0.53014(13) 0.0253(6) Uani 1 1 d . . . F4 F 0.43498(9) 0.2219(2) 0.48201(8) 0.0319(4) Uani 1 1 d . . . C5 C 0.47207(15) 0.3216(4) 0.58801(15) 0.0293(6) Uani 1 1 d . . . F5 F 0.50521(9) 0.1447(2) 0.59504(9) 0.0419(5) Uani 1 1 d . . . C6 C 0.47638(15) 0.4645(4) 0.63791(14) 0.0318(6) Uani 1 1 d . . . F6 F 0.51342(10) 0.4246(3) 0.69222(9) 0.0498(5) Uani 1 1 d . . . C7 C 0.44268(15) 0.6495(4) 0.63121(13) 0.0279(6) Uani 1 1 d . . . F7 F 0.45013(10) 0.7848(3) 0.67963(8) 0.0414(4) Uani 1 1 d . . . C8 C 0.40432(14) 0.6858(4) 0.57495(12) 0.0215(5) Uani 1 1 d . . . C9 C 0.35954(14) 0.8614(4) 0.55326(12) 0.0213(5) Uani 1 1 d . . . O9 O 0.34533(10) 1.0097(2) 0.58618(9) 0.0269(4) Uani 1 1 d . . . Sn11 Sn 0.227803(10) 0.45689(2) 0.187183(9) 0.02305(5) Uani 1 1 d . . . C11A C 0.24263(18) 0.1460(4) 0.16636(15) 0.0382(8) Uani 1 1 d . . . H11A H 0.2905 0.1226 0.1550 0.057 Uiso 1 1 calc R . . H11B H 0.2132 0.1071 0.1299 0.057 Uiso 1 1 calc R . . H11C H 0.2309 0.0677 0.2048 0.057 Uiso 1 1 calc R . . C11B C 0.30490(18) 0.5973(5) 0.24518(15) 0.0466(8) Uani 1 1 d . . . H11D H 0.2985 0.5617 0.2909 0.070 Uiso 1 1 calc R . . H11E H 0.3014 0.7411 0.2403 0.070 Uiso 1 1 calc R . . H11F H 0.3501 0.5533 0.2309 0.070 Uiso 1 1 calc R . . C11C C 0.17896(16) 0.6231(4) 0.10980(14) 0.0324(7) Uani 1 1 d . . . H11G H 0.1634 0.7507 0.1267 0.049 Uiso 1 1 calc R . . H11H H 0.1398 0.5485 0.0931 0.049 Uiso 1 1 calc R . . H11I H 0.2117 0.6453 0.0746 0.049 Uiso 1 1 calc R . . N11 N 0.14530(12) 0.4523(3) 0.25944(10) 0.0236(5) Uani 1 1 d . . . C12 C 0.09094(15) 0.5917(4) 0.26660(13) 0.0284(6) Uani 1 1 d . . . O12 O 0.08166(13) 0.7383(3) 0.23202(10) 0.0436(6) Uani 1 1 d . . . C13 C 0.04848(15) 0.5254(4) 0.32468(13) 0.0263(6) Uani 1 1 d . . . C14 C -0.00899(16) 0.6062(4) 0.35388(14) 0.0330(7) Uani 1 1 d . . . F14 F -0.03886(11) 0.7772(3) 0.33226(10) 0.0552(6) Uani 1 1 d . . . C15 C -0.03799(15) 0.5088(4) 0.40820(15) 0.0346(7) Uani 1 1 d . . . F15 F -0.09429(10) 0.5857(3) 0.43828(9) 0.0493(5) Uani 1 1 d . . . C16 C -0.00891(16) 0.3333(4) 0.43220(14) 0.0311(6) Uani 1 1 d . . . F16 F -0.03798(10) 0.2417(3) 0.48437(8) 0.0427(5) Uani 1 1 d . . . C17 C 0.04986(16) 0.2534(4) 0.40340(14) 0.0289(6) Uani 1 1 d . . . F17 F 0.07706(10) 0.0835(2) 0.42846(9) 0.0427(5) Uani 1 1 d . . . C18 C 0.07920(14) 0.3510(4) 0.35006(13) 0.0245(6) Uani 1 1 d . . . C19 C 0.14288(15) 0.3116(4) 0.30972(13) 0.0254(6) Uani 1 1 d . . . O19 O 0.18659(11) 0.1824(3) 0.31994(9) 0.0322(5) 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 Sn1 0.02286(9) 0.01814(8) 0.01731(8) 0.00118(6) -0.00266(7) 0.00142(6) C1A 0.0263(16) 0.0293(13) 0.0246(14) 0.0038(10) -0.0004(11) 0.0013(11) C1B 0.0286(17) 0.0244(12) 0.0274(15) 0.0003(10) -0.0078(12) -0.0001(10) C1C 0.0334(18) 0.0217(12) 0.0232(14) -0.0004(10) -0.0005(12) 0.0035(10) N1 0.0221(12) 0.0203(9) 0.0181(11) 0.0007(8) -0.0031(9) 0.0023(8) C2 0.0201(14) 0.0208(11) 0.0223(14) 0.0026(9) -0.0021(11) -0.0012(9) O2 0.0336(12) 0.0272(9) 0.0212(10) -0.0051(7) -0.0036(8) 0.0040(8) C3 0.0185(13) 0.0230(12) 0.0212(12) 0.0039(9) -0.0024(10) -0.0008(9) C4 0.0228(15) 0.0246(13) 0.0285(15) 0.0045(10) 0.0011(12) 0.0000(10) F4 0.0346(11) 0.0237(7) 0.0374(10) -0.0039(6) -0.0008(8) 0.0067(7) C5 0.0204(16) 0.0309(13) 0.0365(17) 0.0127(12) -0.0015(13) 0.0075(11) F5 0.0357(11) 0.0369(9) 0.0531(12) 0.0148(8) -0.0052(9) 0.0156(8) C6 0.0236(15) 0.0453(16) 0.0263(14) 0.0119(12) -0.0066(11) 0.0069(12) F6 0.0474(13) 0.0697(12) 0.0322(10) 0.0119(9) -0.0179(9) 0.0178(10) C7 0.0250(17) 0.0401(15) 0.0185(14) -0.0011(11) -0.0025(12) 0.0021(12) F7 0.0457(12) 0.0563(11) 0.0222(9) -0.0091(8) -0.0147(8) 0.0110(8) C8 0.0194(15) 0.0256(12) 0.0195(13) 0.0031(9) -0.0016(11) 0.0017(10) C9 0.0205(15) 0.0250(12) 0.0185(13) 0.0035(9) -0.0015(11) -0.0011(10) O9 0.0329(12) 0.0260(9) 0.0218(9) -0.0043(7) -0.0041(8) 0.0033(8) Sn11 0.02879(11) 0.02136(8) 0.01895(9) 0.00088(6) -0.00369(7) 0.00109(7) C11A 0.055(2) 0.0261(14) 0.0332(17) 0.0032(12) 0.0018(15) 0.0094(13) C11B 0.043(2) 0.068(2) 0.0292(18) -0.0054(15) -0.0028(15) -0.0178(17) C11C 0.0404(19) 0.0301(14) 0.0268(15) 0.0052(11) -0.0024(13) 0.0033(12) N11 0.0259(13) 0.0241(10) 0.0209(11) 0.0047(8) -0.0033(9) 0.0020(9) C12 0.0332(17) 0.0282(13) 0.0237(14) -0.0007(11) -0.0060(12) 0.0052(11) O12 0.0579(17) 0.0398(11) 0.0331(13) 0.0119(9) 0.0016(11) 0.0210(10) C13 0.0237(15) 0.0293(13) 0.0260(14) -0.0015(10) -0.0077(11) 0.0033(11) C14 0.0314(18) 0.0399(15) 0.0276(16) -0.0015(12) -0.0084(13) 0.0121(13) F14 0.0577(15) 0.0613(12) 0.0466(12) 0.0085(9) 0.0014(10) 0.0389(10) C15 0.0211(15) 0.0496(17) 0.0330(16) -0.0111(13) -0.0027(12) 0.0051(13) F15 0.0315(12) 0.0719(12) 0.0445(12) -0.0106(10) 0.0056(9) 0.0156(9) C16 0.0245(17) 0.0438(16) 0.0249(15) -0.0024(12) -0.0009(12) -0.0078(12) F16 0.0333(12) 0.0586(11) 0.0362(11) 0.0022(8) 0.0107(9) -0.0096(8) C17 0.0256(17) 0.0295(13) 0.0316(16) 0.0041(11) -0.0022(13) -0.0038(11) F17 0.0453(12) 0.0368(9) 0.0460(11) 0.0181(8) 0.0106(9) 0.0053(8) C18 0.0226(15) 0.0266(13) 0.0244(15) -0.0001(10) -0.0046(11) -0.0019(10) C19 0.0265(16) 0.0259(12) 0.0236(14) 0.0038(10) -0.0051(12) -0.0016(11) O19 0.0299(12) 0.0354(10) 0.0313(11) 0.0099(8) 0.0019(9) 0.0110(8) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Sn1 C1A 2.111(3) . ? Sn1 C1B 2.119(3) . ? Sn1 C1C 2.127(2) . ? Sn1 N1 2.183(2) . ? C1A H1A1 0.9600 . ? C1A H1A2 0.9600 . ? C1A H1A3 0.9600 . ? C1B H1B1 0.9600 . ? C1B H1B2 0.9600 . ? C1B H1B3 0.9600 . ? C1C H1C1 0.9600 . ? C1C H1C2 0.9600 . ? C1C H1C3 0.9600 . ? N1 C9 1.383(3) . ? N1 C2 1.390(3) . ? C2 O2 1.208(3) . ? C2 C3 1.492(3) . ? C3 C4 1.370(3) . ? C3 C8 1.396(3) . ? C4 F4 1.340(3) . ? C4 C5 1.385(4) . ? C5 F5 1.341(3) . ? C5 C6 1.383(4) . ? C6 F6 1.329(3) . ? C6 C7 1.393(4) . ? C7 F7 1.332(3) . ? C7 C8 1.370(3) . ? C8 C9 1.510(3) . ? C9 O9 1.217(3) . ? Sn11 C11B 2.099(3) . ? Sn11 C11A 2.122(3) . ? Sn11 C11C 2.124(3) . ? Sn11 N11 2.156(2) . ? C11A H11A 0.9600 . ? C11A H11B 0.9600 . ? C11A H11C 0.9600 . ? C11B H11D 0.9600 . ? C11B H11E 0.9600 . ? C11B H11F 0.9600 . ? C11C H11G 0.9600 . ? C11C H11H 0.9600 . ? C11C H11I 0.9600 . ? N11 C19 1.378(3) . ? N11 C12 1.401(3) . ? C12 O12 1.208(3) . ? C12 C13 1.495(4) . ? C13 C14 1.362(4) . ? C13 C18 1.394(3) . ? C14 F14 1.341(3) . ? C14 C15 1.389(4) . ? C15 F15 1.342(3) . ? C15 C16 1.377(4) . ? C16 F16 1.338(3) . ? C16 C17 1.377(4) . ? C17 F17 1.339(3) . ? C17 C18 1.377(4) . ? C18 C19 1.494(4) . ? C19 O19 1.215(3) . ? 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 C1A Sn1 C1B 120.39(11) . . ? C1A Sn1 C1C 116.33(10) . . ? C1B Sn1 C1C 114.56(11) . . ? C1A Sn1 N1 100.50(9) . . ? C1B Sn1 N1 97.56(9) . . ? C1C Sn1 N1 101.75(9) . . ? Sn1 C1A H1A1 109.5 . . ? Sn1 C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? Sn1 C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? Sn1 C1B H1B1 109.5 . . ? Sn1 C1B H1B2 109.5 . . ? H1B1 C1B H1B2 109.5 . . ? Sn1 C1B H1B3 109.5 . . ? H1B1 C1B H1B3 109.5 . . ? H1B2 C1B H1B3 109.5 . . ? Sn1 C1C H1C1 109.5 . . ? Sn1 C1C H1C2 109.5 . . ? H1C1 C1C H1C2 109.5 . . ? Sn1 C1C H1C3 109.5 . . ? H1C1 C1C H1C3 109.5 . . ? H1C2 C1C H1C3 109.5 . . ? C9 N1 C2 110.4(2) . . ? C9 N1 Sn1 132.75(16) . . ? C2 N1 Sn1 116.82(15) . . ? O2 C2 N1 125.4(2) . . ? O2 C2 C3 126.7(2) . . ? N1 C2 C3 108.0(2) . . ? C4 C3 C8 121.0(2) . . ? C4 C3 C2 131.9(2) . . ? C8 C3 C2 107.0(2) . . ? F4 C4 C3 122.7(2) . . ? F4 C4 C5 118.6(2) . . ? C3 C4 C5 118.6(2) . . ? F5 C5 C6 119.6(2) . . ? F5 C5 C4 119.7(3) . . ? C6 C5 C4 120.7(2) . . ? F6 C6 C5 119.5(2) . . ? F6 C6 C7 120.1(3) . . ? C5 C6 C7 120.4(2) . . ? F7 C7 C8 122.9(2) . . ? F7 C7 C6 118.3(2) . . ? C8 C7 C6 118.8(2) . . ? C7 C8 C3 120.3(2) . . ? C7 C8 C9 132.7(2) . . ? C3 C8 C9 107.0(2) . . ? O9 C9 N1 126.3(2) . . ? O9 C9 C8 126.4(2) . . ? N1 C9 C8 107.4(2) . . ? C11B Sn11 C11A 116.47(14) . . ? C11B Sn11 C11C 119.12(13) . . ? C11A Sn11 C11C 114.68(11) . . ? C11B Sn11 N11 98.52(11) . . ? C11A Sn11 N11 102.68(10) . . ? C11C Sn11 N11 100.37(10) . . ? Sn11 C11A H11A 109.5 . . ? Sn11 C11A H11B 109.5 . . ? H11A C11A H11B 109.5 . . ? Sn11 C11A H11C 109.5 . . ? H11A C11A H11C 109.5 . . ? H11B C11A H11C 109.5 . . ? Sn11 C11B H11D 109.5 . . ? Sn11 C11B H11E 109.5 . . ? H11D C11B H11E 109.5 . . ? Sn11 C11B H11F 109.5 . . ? H11D C11B H11F 109.5 . . ? H11E C11B H11F 109.5 . . ? Sn11 C11C H11G 109.5 . . ? Sn11 C11C H11H 109.5 . . ? H11G C11C H11H 109.5 . . ? Sn11 C11C H11I 109.5 . . ? H11G C11C H11I 109.5 . . ? H11H C11C H11I 109.5 . . ? C19 N11 C12 110.1(2) . . ? C19 N11 Sn11 122.22(17) . . ? C12 N11 Sn11 127.57(17) . . ? O12 C12 N11 125.3(3) . . ? O12 C12 C13 127.5(3) . . ? N11 C12 C13 107.2(2) . . ? C14 C13 C18 120.6(3) . . ? C14 C13 C12 131.9(2) . . ? C18 C13 C12 107.5(2) . . ? F14 C14 C13 122.5(3) . . ? F14 C14 C15 118.4(3) . . ? C13 C14 C15 119.1(3) . . ? F15 C15 C16 119.2(3) . . ? F15 C15 C14 120.4(3) . . ? C16 C15 C14 120.4(3) . . ? F16 C16 C17 120.2(3) . . ? F16 C16 C15 119.3(3) . . ? C17 C16 C15 120.5(3) . . ? F17 C17 C16 118.9(3) . . ? F17 C17 C18 122.0(3) . . ? C16 C17 C18 119.2(3) . . ? C17 C18 C13 120.1(3) . . ? C17 C18 C19 132.9(2) . . ? C13 C18 C19 106.9(2) . . ? O19 C19 N11 125.2(3) . . ? O19 C19 C18 126.6(2) . . ? N11 C19 C18 108.2(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1A Sn1 N1 C9 111.3(2) . . . . ? C1B Sn1 N1 C9 -125.8(2) . . . . ? C1C Sn1 N1 C9 -8.7(2) . . . . ? C1A Sn1 N1 C2 -67.55(19) . . . . ? C1B Sn1 N1 C2 55.37(19) . . . . ? C1C Sn1 N1 C2 172.49(18) . . . . ? C9 N1 C2 O2 -175.9(3) . . . . ? Sn1 N1 C2 O2 3.2(3) . . . . ? C9 N1 C2 C3 2.2(3) . . . . ? Sn1 N1 C2 C3 -178.73(16) . . . . ? O2 C2 C3 C4 -4.4(5) . . . . ? N1 C2 C3 C4 177.6(3) . . . . ? O2 C2 C3 C8 173.6(3) . . . . ? N1 C2 C3 C8 -4.5(3) . . . . ? C8 C3 C4 F4 -179.3(2) . . . . ? C2 C3 C4 F4 -1.6(5) . . . . ? C8 C3 C4 C5 -0.7(4) . . . . ? C2 C3 C4 C5 177.0(3) . . . . ? F4 C4 C5 F5 -1.1(4) . . . . ? C3 C4 C5 F5 -179.7(2) . . . . ? F4 C4 C5 C6 177.3(2) . . . . ? C3 C4 C5 C6 -1.4(4) . . . . ? F5 C5 C6 F6 0.1(4) . . . . ? C4 C5 C6 F6 -178.3(3) . . . . ? F5 C5 C6 C7 179.6(3) . . . . ? C4 C5 C6 C7 1.2(4) . . . . ? F6 C6 C7 F7 1.6(4) . . . . ? C5 C6 C7 F7 -177.9(3) . . . . ? F6 C6 C7 C8 -179.4(3) . . . . ? C5 C6 C7 C8 1.1(4) . . . . ? F7 C7 C8 C3 175.8(2) . . . . ? C6 C7 C8 C3 -3.2(4) . . . . ? F7 C7 C8 C9 -4.2(5) . . . . ? C6 C7 C8 C9 176.8(3) . . . . ? C4 C3 C8 C7 3.1(4) . . . . ? C2 C3 C8 C7 -175.2(2) . . . . ? C4 C3 C8 C9 -177.0(2) . . . . ? C2 C3 C8 C9 4.8(3) . . . . ? C2 N1 C9 O9 -178.2(3) . . . . ? Sn1 N1 C9 O9 2.9(4) . . . . ? C2 N1 C9 C8 0.8(3) . . . . ? Sn1 N1 C9 C8 -178.12(17) . . . . ? C7 C8 C9 O9 -4.7(5) . . . . ? C3 C8 C9 O9 175.4(3) . . . . ? C7 C8 C9 N1 176.4(3) . . . . ? C3 C8 C9 N1 -3.6(3) . . . . ? C11B Sn11 N11 C19 -78.8(2) . . . . ? C11A Sn11 N11 C19 40.9(2) . . . . ? C11C Sn11 N11 C19 159.3(2) . . . . ? C11B Sn11 N11 C12 96.1(2) . . . . ? C11A Sn11 N11 C12 -144.2(2) . . . . ? C11C Sn11 N11 C12 -25.7(2) . . . . ? C19 N11 C12 O12 176.1(3) . . . . ? Sn11 N11 C12 O12 0.7(4) . . . . ? C19 N11 C12 C13 -3.2(3) . . . . ? Sn11 N11 C12 C13 -178.64(16) . . . . ? O12 C12 C13 C14 -0.5(5) . . . . ? N11 C12 C13 C14 178.8(3) . . . . ? O12 C12 C13 C18 -178.9(3) . . . . ? N11 C12 C13 C18 0.4(3) . . . . ? C18 C13 C14 F14 177.9(3) . . . . ? C12 C13 C14 F14 -0.3(5) . . . . ? C18 C13 C14 C15 -2.0(4) . . . . ? C12 C13 C14 C15 179.7(3) . . . . ? F14 C14 C15 F15 -0.4(4) . . . . ? C13 C14 C15 F15 179.5(3) . . . . ? F14 C14 C15 C16 -179.8(3) . . . . ? C13 C14 C15 C16 0.1(4) . . . . ? F15 C15 C16 F16 0.9(4) . . . . ? C14 C15 C16 F16 -179.7(3) . . . . ? F15 C15 C16 C17 -178.4(3) . . . . ? C14 C15 C16 C17 1.0(4) . . . . ? F16 C16 C17 F17 0.1(4) . . . . ? C15 C16 C17 F17 179.4(2) . . . . ? F16 C16 C17 C18 -179.5(2) . . . . ? C15 C16 C17 C18 -0.2(4) . . . . ? F17 C17 C18 C13 178.8(2) . . . . ? C16 C17 C18 C13 -1.7(4) . . . . ? F17 C17 C18 C19 -2.3(5) . . . . ? C16 C17 C18 C19 177.2(3) . . . . ? C14 C13 C18 C17 2.8(4) . . . . ? C12 C13 C18 C17 -178.6(2) . . . . ? C14 C13 C18 C19 -176.3(3) . . . . ? C12 C13 C18 C19 2.3(3) . . . . ? C12 N11 C19 O19 -173.4(3) . . . . ? Sn11 N11 C19 O19 2.4(4) . . . . ? C12 N11 C19 C18 4.6(3) . . . . ? Sn11 N11 C19 C18 -179.64(15) . . . . ? C17 C18 C19 O19 -5.4(5) . . . . ? C13 C18 C19 O19 173.7(3) . . . . ? C17 C18 C19 N11 176.7(3) . . . . ? C13 C18 C19 N11 -4.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.816 _refine_diff_density_min -0.803 _refine_diff_density_rms 0.097 #===END data_simonl18 _database_code_depnum_ccdc_archive 'CCDC 791408' #TrackingRef '- combined.cif' _audit_creation_method 'SHELXL-97 and CrysAlisPro RED' _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 6' _chemical_melting_point ? _chemical_formula_structural '[(MeCN)2 Ag-Ag (tetrafluorophthalimide)2]' _chemical_formula_moiety 'C20 H6 Ag2 F8 N4 O4' _chemical_formula_sum 'C20 H6 Ag2 F8 N4 O4' _chemical_formula_weight 734.03 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.93961(12) _cell_length_b 26.9636(4) _cell_length_c 10.48883(15) _cell_angle_alpha 90.00 _cell_angle_beta 105.245(2) _cell_angle_gamma 90.00 _cell_volume 2166.43(5) _cell_formula_units_Z 4 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 1.915 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.978 _exptl_absorpt_correction_T_max 1.038 _exptl_absorpt_process_details ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_reflns_number 47568 _diffrn_reflns_av_R_equivalents 0.0439 _diffrn_reflns_av_sigmaI/netI 0.0188 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4974 _reflns_number_gt 4481 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlisPro CCD, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_cell_refinement ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_data_reduction ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0144P)^2^+2.3936P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4974 _refine_ls_number_parameters 367 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0508 _refine_ls_wR_factor_gt 0.0496 _refine_ls_goodness_of_fit_ref 1.181 _refine_ls_restrained_S_all 1.181 _refine_ls_shift/su_max 0.003 _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 Ag1 Ag 0.70005(2) 0.532449(6) 0.527526(18) 0.02118(5) Uani 1 1 d . . . Ag2 Ag 0.48539(2) 0.587030(7) 0.288635(19) 0.02503(5) Uani 1 1 d . . . N1 N 0.7264(3) 0.47636(7) 0.4001(2) 0.0210(4) Uani 1 1 d . . . C2 C 0.8430(3) 0.43743(9) 0.4306(3) 0.0214(5) Uani 1 1 d . . . O2 O 0.9542(2) 0.43170(7) 0.53372(19) 0.0298(4) Uani 1 1 d . . . C3 C 0.8091(3) 0.40363(9) 0.3118(2) 0.0196(5) Uani 1 1 d . . . C4 C 0.8813(3) 0.35969(9) 0.2874(3) 0.0229(5) Uani 1 1 d . . . F4 F 1.01210(19) 0.33727(6) 0.37615(16) 0.0314(3) Uani 1 1 d . . . C5 C 0.8184(3) 0.33728(9) 0.1655(3) 0.0240(5) Uani 1 1 d . . . F5 F 0.8846(2) 0.29369(6) 0.13994(17) 0.0344(4) Uani 1 1 d . . . C6 C 0.6854(3) 0.35863(9) 0.0691(2) 0.0241(5) Uani 1 1 d . . . F6 F 0.6237(2) 0.33529(6) -0.04622(15) 0.0337(4) Uani 1 1 d . . . C7 C 0.6118(3) 0.40336(9) 0.0941(2) 0.0221(5) Uani 1 1 d . . . F7 F 0.4799(2) 0.42224(6) -0.00006(15) 0.0316(3) Uani 1 1 d . . . C8 C 0.6746(3) 0.42531(8) 0.2149(2) 0.0192(5) Uani 1 1 d . . . C9 C 0.6244(3) 0.47207(9) 0.2740(2) 0.0209(5) Uani 1 1 d . . . O9 O 0.5122(2) 0.50125(6) 0.21607(18) 0.0263(4) Uani 1 1 d . . . N11 N 0.6596(3) 0.59274(7) 0.6386(2) 0.0206(4) Uani 1 1 d . . . C12 C 0.5382(3) 0.62880(8) 0.5919(2) 0.0188(5) Uani 1 1 d . . . O12 O 0.4297(2) 0.62922(6) 0.48462(16) 0.0228(4) Uani 1 1 d . . . C13 C 0.5582(3) 0.66859(9) 0.6959(2) 0.0212(5) Uani 1 1 d . . . C14 C 0.4705(4) 0.71219(9) 0.6997(3) 0.0272(6) Uani 1 1 d . . . F14 F 0.3370(2) 0.72715(6) 0.60145(17) 0.0361(4) Uani 1 1 d . . . C15 C 0.5224(4) 0.74135(10) 0.8126(3) 0.0348(7) Uani 1 1 d . . . F15 F 0.4371(3) 0.78361(6) 0.8201(2) 0.0500(5) Uani 1 1 d . . . C16 C 0.6585(4) 0.72704(11) 0.9161(3) 0.0382(7) Uani 1 1 d . . . F16 F 0.7070(3) 0.75607(8) 1.0235(2) 0.0579(6) Uani 1 1 d . . . C17 C 0.7454(4) 0.68250(11) 0.9123(3) 0.0326(6) Uani 1 1 d . . . F17 F 0.8764(2) 0.66947(8) 1.01601(16) 0.0484(5) Uani 1 1 d . . . C18 C 0.6945(3) 0.65340(9) 0.8014(2) 0.0238(5) Uani 1 1 d . . . C19 C 0.7577(3) 0.60436(10) 0.7642(2) 0.0240(5) Uani 1 1 d . . . O19 O 0.8745(2) 0.57925(7) 0.83220(19) 0.0319(4) Uani 1 1 d . . . N31 N 0.7187(3) 0.63261(8) 0.2905(2) 0.0288(5) Uani 1 1 d . . . C32 C 0.8507(3) 0.65208(9) 0.3086(3) 0.0255(5) Uani 1 1 d . . . C33 C 1.0178(4) 0.67709(12) 0.3296(4) 0.0351(7) Uani 1 1 d . . . N41 N 0.2042(3) 0.57674(9) 0.1811(3) 0.0346(5) Uani 1 1 d . . . C42 C 0.0747(3) 0.55637(10) 0.1589(3) 0.0267(5) Uani 1 1 d . . . C43 C -0.0906(4) 0.53013(11) 0.1321(3) 0.0329(6) Uani 1 1 d . . . H33A H 1.028(5) 0.6988(16) 0.394(4) 0.066(13) Uiso 1 1 d . . . H33B H 1.028(5) 0.6930(15) 0.258(4) 0.061(12) Uiso 1 1 d . . . H33C H 1.108(5) 0.6546(16) 0.367(4) 0.066(12) Uiso 1 1 d . . . H43A H -0.146(5) 0.5374(14) 0.192(4) 0.054(11) Uiso 1 1 d . . . H43B H -0.155(4) 0.5385(13) 0.044(4) 0.046(10) Uiso 1 1 d . . . H43C H -0.078(4) 0.4950(14) 0.134(3) 0.051(10) Uiso 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 Ag1 0.02438(9) 0.01768(9) 0.02107(9) -0.00248(7) 0.00523(7) 0.00109(7) Ag2 0.02581(10) 0.02480(10) 0.02290(10) -0.00210(7) 0.00357(7) 0.00034(7) N1 0.0218(10) 0.0173(10) 0.0239(10) -0.0012(8) 0.0063(8) -0.0006(8) C2 0.0200(11) 0.0169(11) 0.0290(13) -0.0011(10) 0.0095(10) -0.0022(9) O2 0.0240(9) 0.0293(10) 0.0319(10) -0.0032(8) -0.0001(8) 0.0000(7) C3 0.0185(11) 0.0187(11) 0.0235(12) -0.0010(9) 0.0090(10) -0.0041(9) C4 0.0188(11) 0.0200(11) 0.0313(13) 0.0039(10) 0.0092(10) 0.0012(9) F4 0.0263(8) 0.0278(8) 0.0391(9) 0.0028(7) 0.0067(7) 0.0089(6) C5 0.0297(13) 0.0139(11) 0.0349(14) -0.0006(10) 0.0199(11) 0.0019(9) F5 0.0439(9) 0.0204(7) 0.0430(9) -0.0044(7) 0.0188(8) 0.0080(7) C6 0.0368(14) 0.0179(11) 0.0221(12) -0.0022(10) 0.0155(11) -0.0047(10) F6 0.0527(10) 0.0258(8) 0.0236(8) -0.0067(6) 0.0116(7) -0.0012(7) C7 0.0280(13) 0.0203(12) 0.0199(12) 0.0042(9) 0.0096(10) 0.0000(9) F7 0.0411(9) 0.0292(8) 0.0215(7) 0.0023(6) 0.0026(7) 0.0075(7) C8 0.0220(11) 0.0149(10) 0.0239(12) 0.0015(9) 0.0116(10) -0.0013(9) C9 0.0241(12) 0.0165(11) 0.0250(12) 0.0015(10) 0.0115(10) -0.0032(9) O9 0.0322(10) 0.0187(8) 0.0278(10) 0.0024(7) 0.0075(8) 0.0038(7) N11 0.0231(10) 0.0211(10) 0.0182(10) -0.0008(8) 0.0066(8) -0.0018(8) C12 0.0238(12) 0.0151(10) 0.0210(12) -0.0008(9) 0.0119(10) -0.0045(9) O12 0.0278(9) 0.0213(8) 0.0193(9) 0.0003(7) 0.0062(7) -0.0009(7) C13 0.0281(13) 0.0173(11) 0.0218(12) -0.0031(9) 0.0130(10) -0.0078(9) C14 0.0364(14) 0.0193(12) 0.0320(14) -0.0027(10) 0.0194(12) -0.0073(10) F14 0.0467(10) 0.0227(8) 0.0413(10) 0.0028(7) 0.0156(8) 0.0073(7) C15 0.0462(17) 0.0211(13) 0.0476(18) -0.0137(12) 0.0307(15) -0.0116(12) F15 0.0692(13) 0.0244(8) 0.0701(13) -0.0197(9) 0.0425(11) -0.0069(8) C16 0.0464(17) 0.0405(16) 0.0364(16) -0.0249(14) 0.0266(15) -0.0235(14) F16 0.0645(13) 0.0660(13) 0.0515(12) -0.0444(10) 0.0301(10) -0.0279(11) C17 0.0295(14) 0.0471(17) 0.0240(13) -0.0120(12) 0.0122(11) -0.0158(12) F17 0.0412(10) 0.0783(14) 0.0236(9) -0.0164(9) 0.0049(8) -0.0143(9) C18 0.0273(13) 0.0264(13) 0.0209(12) -0.0048(10) 0.0121(10) -0.0099(10) C19 0.0233(12) 0.0290(13) 0.0220(12) -0.0018(10) 0.0102(10) -0.0067(10) O19 0.0252(9) 0.0422(11) 0.0271(10) 0.0040(9) 0.0047(8) 0.0008(8) N31 0.0273(12) 0.0291(12) 0.0280(12) 0.0007(9) 0.0038(9) -0.0003(9) C32 0.0310(14) 0.0180(11) 0.0268(13) -0.0003(10) 0.0061(11) 0.0014(10) C33 0.0324(16) 0.0325(15) 0.0367(17) 0.0015(14) 0.0027(13) -0.0105(13) N41 0.0268(12) 0.0348(13) 0.0412(14) -0.0033(11) 0.0073(11) -0.0009(10) C42 0.0256(13) 0.0258(13) 0.0294(14) 0.0028(11) 0.0085(11) 0.0050(11) C43 0.0291(14) 0.0286(15) 0.0430(18) 0.0027(13) 0.0132(13) -0.0026(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 Ag1 N1 2.065(2) . ? Ag1 N11 2.074(2) . ? Ag1 Ag2 3.0172(3) . ? Ag2 N31 2.219(2) . ? Ag2 N41 2.238(2) . ? Ag2 O9 2.4616(17) . ? Ag2 O12 2.4885(17) . ? N1 C9 1.362(3) . ? N1 C2 1.381(3) . ? C2 O2 1.213(3) . ? C2 C3 1.510(3) . ? C3 C4 1.369(3) . ? C3 C8 1.395(3) . ? C4 F4 1.342(3) . ? C4 C5 1.383(4) . ? C5 F5 1.343(3) . ? C5 C6 1.381(4) . ? C6 F6 1.337(3) . ? C6 C7 1.395(3) . ? C7 F7 1.337(3) . ? C7 C8 1.368(3) . ? C8 C9 1.504(3) . ? C9 O9 1.224(3) . ? N11 C12 1.366(3) . ? N11 C19 1.378(3) . ? C12 O12 1.224(3) . ? C12 C13 1.509(3) . ? C13 C14 1.372(4) . ? C13 C18 1.390(4) . ? C14 F14 1.332(3) . ? C14 C15 1.390(4) . ? C15 F15 1.338(3) . ? C15 C16 1.370(5) . ? C16 F16 1.342(3) . ? C16 C17 1.391(4) . ? C17 F17 1.339(3) . ? C17 C18 1.373(4) . ? C18 C19 1.502(4) . ? C19 O19 1.216(3) . ? N31 C32 1.142(3) . ? C32 C33 1.452(4) . ? C33 H33A 0.88(4) . ? C33 H33B 0.89(4) . ? C33 H33C 0.94(4) . ? N41 C42 1.135(3) . ? C42 C43 1.452(4) . ? C43 H43A 0.88(4) . ? C43 H43B 0.96(4) . ? C43 H43C 0.95(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N11 174.16(8) . . ? N1 Ag1 Ag2 87.19(6) . . ? N11 Ag1 Ag2 86.98(6) . . ? N31 Ag2 N41 142.45(9) . . ? N31 Ag2 O9 112.53(7) . . ? N41 Ag2 O9 83.31(8) . . ? N31 Ag2 O12 93.95(7) . . ? N41 Ag2 O12 95.91(8) . . ? O9 Ag2 O12 137.18(6) . . ? N31 Ag2 Ag1 88.56(6) . . ? N41 Ag2 Ag1 128.97(7) . . ? O9 Ag2 Ag1 73.89(4) . . ? O12 Ag2 Ag1 73.81(4) . . ? C9 N1 C2 110.6(2) . . ? C9 N1 Ag1 123.73(16) . . ? C2 N1 Ag1 125.65(16) . . ? O2 C2 N1 126.1(2) . . ? O2 C2 C3 126.1(2) . . ? N1 C2 C3 107.7(2) . . ? C4 C3 C8 120.3(2) . . ? C4 C3 C2 133.2(2) . . ? C8 C3 C2 106.5(2) . . ? F4 C4 C3 123.1(2) . . ? F4 C4 C5 118.0(2) . . ? C3 C4 C5 118.9(2) . . ? F5 C5 C6 118.9(2) . . ? F5 C5 C4 120.1(2) . . ? C6 C5 C4 121.0(2) . . ? F6 C6 C5 119.6(2) . . ? F6 C6 C7 120.3(2) . . ? C5 C6 C7 120.0(2) . . ? F7 C7 C8 122.9(2) . . ? F7 C7 C6 118.4(2) . . ? C8 C7 C6 118.6(2) . . ? C7 C8 C3 121.1(2) . . ? C7 C8 C9 132.3(2) . . ? C3 C8 C9 106.6(2) . . ? O9 C9 N1 126.6(2) . . ? O9 C9 C8 124.9(2) . . ? N1 C9 C8 108.5(2) . . ? C9 O9 Ag2 124.16(16) . . ? C12 N11 C19 110.4(2) . . ? C12 N11 Ag1 123.70(16) . . ? C19 N11 Ag1 125.68(17) . . ? O12 C12 N11 126.6(2) . . ? O12 C12 C13 125.0(2) . . ? N11 C12 C13 108.4(2) . . ? C12 O12 Ag2 121.34(15) . . ? C14 C13 C18 121.6(2) . . ? C14 C13 C12 132.2(2) . . ? C18 C13 C12 106.1(2) . . ? F14 C14 C13 123.0(2) . . ? F14 C14 C15 119.0(2) . . ? C13 C14 C15 118.0(3) . . ? F15 C15 C16 119.9(3) . . ? F15 C15 C14 119.4(3) . . ? C16 C15 C14 120.7(3) . . ? F16 C16 C15 119.5(3) . . ? F16 C16 C17 119.5(3) . . ? C15 C16 C17 120.9(3) . . ? F17 C17 C18 122.1(3) . . ? F17 C17 C16 119.2(3) . . ? C18 C17 C16 118.7(3) . . ? C17 C18 C13 120.0(3) . . ? C17 C18 C19 132.8(3) . . ? C13 C18 C19 107.2(2) . . ? O19 C19 N11 125.9(2) . . ? O19 C19 C18 126.4(2) . . ? N11 C19 C18 107.8(2) . . ? C32 N31 Ag2 169.4(2) . . ? N31 C32 C33 179.1(3) . . ? C32 C33 H33A 109(3) . . ? C32 C33 H33B 112(3) . . ? H33A C33 H33B 108(4) . . ? C32 C33 H33C 109(2) . . ? H33A C33 H33C 102(3) . . ? H33B C33 H33C 115(3) . . ? C42 N41 Ag2 153.3(2) . . ? N41 C42 C43 179.4(3) . . ? C42 C43 H43A 111(2) . . ? C42 C43 H43B 107(2) . . ? H43A C43 H43B 113(3) . . ? C42 C43 H43C 113(2) . . ? H43A C43 H43C 106(3) . . ? H43B C43 H43C 106(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.649 _refine_diff_density_min -0.527 _refine_diff_density_rms 0.072 #===END data_ns23a _database_code_depnum_ccdc_archive 'CCDC 791409' #TrackingRef '- combined.cif' _audit_creation_method 'SHELXL-97 and CrysAlisPro RED' _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 7' _chemical_melting_point ? _chemical_formula_structural Iodo-tetrafluorophthalimide.MeCN _chemical_formula_moiety 'C8 F4 I N O2, C2 H3 N' _chemical_formula_sum 'C10 H3 F4 I N2 O2' _chemical_formula_weight 386.04 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' 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' I I -0.4742 1.8119 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 9.4073(7) _cell_length_b 6.3030(5) _cell_length_c 10.1518(10) _cell_angle_alpha 90.00 _cell_angle_beta 108.929(9) _cell_angle_gamma 90.00 _cell_volume 569.39(8) _cell_formula_units_Z 2 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used 3055 _cell_measurement_theta_min 3.5838 _cell_measurement_theta_max 29.1978 _exptl_crystal_description 'hexagonal plate' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.252 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 364 _exptl_absorpt_coefficient_mu 2.865 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.962 _exptl_absorpt_correction_T_max 1.054 _exptl_absorpt_process_details ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.33.55 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/Sapphire3 CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_reflns_number 6985 _diffrn_reflns_av_R_equivalents 0.1044 _diffrn_reflns_av_sigmaI/netI 0.0700 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1103 _reflns_number_gt 902 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlisPro CCD, Oxford Diffraction Ltd., Version 1.171.33.55 ; _computing_cell_refinement ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.33.55 ; _computing_data_reduction ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.33.55 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Johnson, 1976 and Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008) and WINGX (Farrugia, 1999)' _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^ > 2\s(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^)+(0.0729P)^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 1103 _refine_ls_number_parameters 119 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0786 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1228 _refine_ls_wR_factor_gt 0.1159 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 I1 I 0.52648(9) 0.2500 0.75180(9) 0.0248(3) Uani 1 2 d S . . N1 N 0.6546(10) 0.2500 0.6196(11) 0.021(2) Uani 1 2 d S . . C2 C 0.5866(13) 0.2500 0.4743(14) 0.022(3) Uani 1 2 d S . . O2 O 0.4553(8) 0.2500 0.4161(10) 0.027(2) Uani 1 2 d S . . C3 C 0.7156(12) 0.2500 0.4185(14) 0.023(3) Uani 1 2 d S . . C4 C 0.7193(12) 0.2500 0.2837(14) 0.026(3) Uani 1 2 d S . . C5 C 0.8546(14) 0.2500 0.2599(14) 0.027(3) Uani 1 2 d S . . C6 C 0.9886(12) 0.2500 0.3737(14) 0.025(3) Uani 1 2 d S . . C7 C 0.9857(13) 0.2500 0.5087(13) 0.021(3) Uani 1 2 d S . . C8 C 0.8484(12) 0.2500 0.5297(14) 0.023(3) Uani 1 2 d S . . C9 C 0.8108(13) 0.2500 0.6615(13) 0.023(3) Uani 1 2 d S . . O9 O 0.8950(9) 0.2500 0.7809(10) 0.032(2) Uani 1 2 d S . . F4 F 0.5931(7) 0.2500 0.1736(8) 0.0303(17) Uani 1 2 d S . . F5 F 0.8625(8) 0.2500 0.1322(8) 0.0330(18) Uani 1 2 d S . . F6 F 1.1196(7) 0.2500 0.3480(8) 0.0349(19) Uani 1 2 d S . . F7 F 1.1166(7) 0.2500 0.6141(8) 0.0318(18) Uani 1 2 d S . . N11 N 0.3481(13) 0.23(3) 0.9007(16) 0.03(2) Uani 0.50 1 d P . . C12 C 0.2792(13) 0.2500 0.9745(14) 0.030(3) Uani 1 2 d S . . C13 C 0.1954(16) 0.2500 1.0709(16) 0.045(4) Uani 1 2 d S . . H13A H 0.1520 0.1124 1.0717 0.067 Uiso 0.50 1 calc PR . . H13B H 0.1170 0.3543 1.0426 0.067 Uiso 0.50 1 calc PR . . H13C H 0.2615 0.2833 1.1626 0.067 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0202(4) 0.0276(5) 0.0307(5) 0.000 0.0140(3) 0.000 N1 0.012(5) 0.024(5) 0.029(6) 0.000 0.010(4) 0.000 C2 0.023(7) 0.014(6) 0.034(8) 0.000 0.014(6) 0.000 O2 0.008(4) 0.035(5) 0.040(6) 0.000 0.008(4) 0.000 C3 0.020(6) 0.018(6) 0.032(8) 0.000 0.008(5) 0.000 C4 0.017(6) 0.026(7) 0.028(8) 0.000 -0.002(5) 0.000 C5 0.032(7) 0.030(7) 0.022(8) 0.000 0.012(6) 0.000 C6 0.017(6) 0.017(6) 0.040(9) 0.000 0.011(6) 0.000 C7 0.025(6) 0.015(6) 0.020(7) 0.000 0.004(5) 0.000 C8 0.012(6) 0.017(6) 0.040(8) 0.000 0.010(5) 0.000 C9 0.023(6) 0.022(6) 0.023(8) 0.000 0.008(5) 0.000 O9 0.023(5) 0.047(6) 0.025(6) 0.000 0.007(4) 0.000 F4 0.019(4) 0.036(4) 0.031(5) 0.000 0.001(3) 0.000 F5 0.031(4) 0.038(4) 0.036(5) 0.000 0.019(3) 0.000 F6 0.020(4) 0.040(4) 0.053(6) 0.000 0.023(4) 0.000 F7 0.010(3) 0.038(4) 0.043(5) 0.000 0.002(3) 0.000 N11 0.014(6) 0.03(6) 0.050(9) -0.005(15) 0.014(6) 0.010(19) C12 0.018(7) 0.046(8) 0.023(8) 0.000 0.002(6) 0.000 C13 0.033(8) 0.071(11) 0.038(10) 0.000 0.022(7) 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 I1 N1 2.074(9) . ? N1 C9 1.391(14) . ? N1 C2 1.405(17) . ? C2 O2 1.184(14) . ? C2 C3 1.497(16) . ? C3 C4 1.380(19) . ? C3 C8 1.386(17) . ? C4 F4 1.341(13) . ? C4 C5 1.370(17) . ? C5 F5 1.323(14) . ? C5 C6 1.407(18) . ? C6 F6 1.340(13) . ? C6 C7 1.380(19) . ? C7 F7 1.344(14) . ? C7 C8 1.376(16) . ? C8 C9 1.491(18) . ? C9 O9 1.214(15) . ? N11 N11 0.3(3) 4_565 ? N11 C12 1.15(3) . ? C12 N11 1.15(3) 4_565 ? C12 C13 1.442(19) . ? C12 C13 1.442(19) 4_565 ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? 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 N1 C2 113.4(9) . . ? C9 N1 I1 125.5(8) . . ? C2 N1 I1 121.2(7) . . ? O2 C2 N1 124.7(11) . . ? O2 C2 C3 130.9(13) . . ? N1 C2 C3 104.4(9) . . ? C4 C3 C8 120.1(11) . . ? C4 C3 C2 131.3(11) . . ? C8 C3 C2 108.6(12) . . ? F4 C4 C5 118.3(12) . . ? F4 C4 C3 121.8(10) . . ? C5 C4 C3 119.9(11) . . ? F5 C5 C4 121.6(11) . . ? F5 C5 C6 119.0(11) . . ? C4 C5 C6 119.4(12) . . ? F6 C6 C7 120.6(11) . . ? F6 C6 C5 118.4(12) . . ? C7 C6 C5 121.0(11) . . ? F7 C7 C8 122.7(11) . . ? F7 C7 C6 118.9(10) . . ? C8 C7 C6 118.4(11) . . ? C7 C8 C3 121.2(13) . . ? C7 C8 C9 130.3(11) . . ? C3 C8 C9 108.5(10) . . ? O9 C9 N1 126.0(11) . . ? O9 C9 C8 128.9(11) . . ? N1 C9 C8 105.1(10) . . ? N11 N11 C12 83(9) 4_565 . ? N11 C12 N11 14(10) . 4_565 ? N11 C12 C13 173(8) . . ? N11 C12 C13 173(8) 4_565 . ? N11 C12 C13 173(8) . 4_565 ? N11 C12 C13 173(8) 4_565 4_565 ? C13 C12 C13 0.0(8) . 4_565 ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.453 _refine_diff_density_min -1.043 _refine_diff_density_rms 0.197 #===END data_nickys3 _database_code_depnum_ccdc_archive 'CCDC 791410' #TrackingRef '- combined.cif' _audit_creation_method 'SHELXL-97 and CrysAlisPro RED' _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 8a' _chemical_melting_point ? _chemical_formula_structural (Ph3P)Au(tetrafluorophthalimide) _chemical_formula_moiety 'C26 H15 Au F4 N O2 P' _chemical_formula_sum 'C26 H15 Au F4 N O2 P' _chemical_formula_weight 677.33 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 Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.79281(11) _cell_length_b 12.00838(11) _cell_length_c 28.1090(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.4139(10) _cell_angle_gamma 90.00 _cell_volume 4578.99(7) _cell_formula_units_Z 8 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.965 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2592 _exptl_absorpt_coefficient_mu 6.553 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.497 _exptl_absorpt_correction_T_max 1.325 _exptl_absorpt_process_details ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_reflns_number 117169 _diffrn_reflns_av_R_equivalents 0.0708 _diffrn_reflns_av_sigmaI/netI 0.0444 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 30.00 _reflns_number_total 13315 _reflns_number_gt 11064 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlisPro CCD, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_cell_refinement ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_data_reduction ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Johnson, 1971 and Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0193P)^2^+13.3166P] 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 13315 _refine_ls_number_parameters 631 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0716 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.0737 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 1.214 _refine_ls_restrained_S_all 1.214 _refine_ls_shift/su_max 0.003 _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 0.026762(13) 0.287537(15) 0.678015(6) 0.01749(4) Uani 1 1 d . . . P1 P -0.03912(9) 0.38373(10) 0.73245(4) 0.0162(2) Uani 1 1 d . . . C11 C -0.1096(3) 0.5044(4) 0.70790(17) 0.0169(9) Uani 1 1 d . . . C12 C -0.1226(3) 0.5274(4) 0.65851(17) 0.0186(9) Uani 1 1 d . . . H12 H -0.0980 0.4786 0.6379 0.022 Uiso 1 1 calc R . . C13 C -0.1721(3) 0.6225(4) 0.63998(17) 0.0218(10) Uani 1 1 d . . . H13 H -0.1812 0.6371 0.6070 0.026 Uiso 1 1 calc R . . C14 C -0.2081(4) 0.6958(4) 0.67043(19) 0.0227(10) Uani 1 1 d . . . H14 H -0.2401 0.7605 0.6580 0.027 Uiso 1 1 calc R . . C15 C -0.1967(3) 0.6732(4) 0.71946(18) 0.0216(10) Uani 1 1 d . . . H15 H -0.2222 0.7221 0.7397 0.026 Uiso 1 1 calc R . . C16 C -0.1477(4) 0.5785(4) 0.73826(17) 0.0210(10) Uani 1 1 d . . . H16 H -0.1400 0.5638 0.7712 0.025 Uiso 1 1 calc R . . C21 C -0.1177(3) 0.3048(4) 0.76564(16) 0.0166(9) Uani 1 1 d . . . C22 C -0.2195(4) 0.3183(4) 0.75767(19) 0.0269(11) Uani 1 1 d . . . H22 H -0.2495 0.3722 0.7362 0.032 Uiso 1 1 calc R . . C23 C -0.2759(4) 0.2510(5) 0.7820(2) 0.0361(14) Uani 1 1 d . . . H23 H -0.3441 0.2589 0.7763 0.043 Uiso 1 1 calc R . . C24 C -0.2314(4) 0.1723(5) 0.8145(2) 0.0313(13) Uani 1 1 d . . . H24 H -0.2698 0.1279 0.8309 0.038 Uiso 1 1 calc R . . C25 C -0.1310(4) 0.1592(4) 0.82285(19) 0.0282(12) Uani 1 1 d . . . H25 H -0.1012 0.1063 0.8449 0.034 Uiso 1 1 calc R . . C26 C -0.0740(4) 0.2255(4) 0.79811(18) 0.0237(10) Uani 1 1 d . . . H26 H -0.0060 0.2163 0.8035 0.028 Uiso 1 1 calc R . . C31 C 0.0608(3) 0.4383(4) 0.77753(17) 0.0173(9) Uani 1 1 d . . . C32 C 0.0500(4) 0.4607(4) 0.82511(18) 0.0236(10) Uani 1 1 d . . . H32 H -0.0093 0.4455 0.8350 0.028 Uiso 1 1 calc R . . C33 C 0.1283(4) 0.5059(4) 0.8576(2) 0.0305(12) Uani 1 1 d . . . H33 H 0.1213 0.5202 0.8893 0.037 Uiso 1 1 calc R . . C34 C 0.2162(4) 0.5295(4) 0.8430(2) 0.0307(12) Uani 1 1 d . . . H34 H 0.2684 0.5596 0.8648 0.037 Uiso 1 1 calc R . . C35 C 0.2267(4) 0.5081(4) 0.7959(2) 0.0300(12) Uani 1 1 d . . . H35 H 0.2859 0.5247 0.7860 0.036 Uiso 1 1 calc R . . C36 C 0.1499(4) 0.4624(4) 0.76325(18) 0.0234(10) Uani 1 1 d . . . H36 H 0.1579 0.4476 0.7317 0.028 Uiso 1 1 calc R . . N41 N 0.1077(3) 0.2094(3) 0.63301(14) 0.0180(8) Uani 1 1 d . . . C42 C 0.2089(4) 0.2198(4) 0.64201(17) 0.0199(9) Uani 1 1 d . . . O42 O 0.2582(3) 0.2660(3) 0.67649(13) 0.0275(8) Uani 1 1 d . . . C43 C 0.2464(4) 0.1642(4) 0.60135(17) 0.0187(9) Uani 1 1 d . . . C44 C 0.3399(4) 0.1542(4) 0.59094(19) 0.0246(11) Uani 1 1 d . . . F44 F 0.4199(2) 0.1953(3) 0.61988(11) 0.0334(7) Uani 1 1 d . . . C45 C 0.3513(4) 0.0999(4) 0.5488(2) 0.0258(11) Uani 1 1 d . . . F45 F 0.4408(2) 0.0903(3) 0.53712(12) 0.0353(8) Uani 1 1 d . . . C46 C 0.2714(4) 0.0540(4) 0.51883(19) 0.0273(12) Uani 1 1 d . . . F46 F 0.2848(3) -0.0003(3) 0.47873(12) 0.0406(9) Uani 1 1 d . . . C47 C 0.1774(4) 0.0631(4) 0.52941(18) 0.0246(11) Uani 1 1 d . . . F47 F 0.1020(2) 0.0181(3) 0.49919(11) 0.0378(8) Uani 1 1 d . . . C48 C 0.1656(4) 0.1200(4) 0.57042(17) 0.0199(10) Uani 1 1 d . . . C49 C 0.0751(4) 0.1512(4) 0.59067(17) 0.0201(10) Uani 1 1 d . . . O49 O -0.0094(3) 0.1327(3) 0.57236(13) 0.0288(8) Uani 1 1 d . . . Au2 Au 0.305564(13) 0.469395(15) 0.580999(7) 0.01819(4) Uani 1 1 d . . . P6 P 0.45896(9) 0.51626(10) 0.61542(4) 0.0173(2) Uani 1 1 d . . . C61 C 0.5469(3) 0.4193(4) 0.59775(17) 0.0184(9) Uani 1 1 d . . . C62 C 0.6333(4) 0.3926(4) 0.62917(19) 0.0270(11) Uani 1 1 d . . . H62 H 0.6479 0.4261 0.6594 0.032 Uiso 1 1 calc R . . C63 C 0.6979(4) 0.3157(4) 0.6153(2) 0.0302(12) Uani 1 1 d . . . H63 H 0.7555 0.2972 0.6365 0.036 Uiso 1 1 calc R . . C64 C 0.6773(4) 0.2668(4) 0.5704(2) 0.0266(11) Uani 1 1 d . . . H64 H 0.7204 0.2146 0.5614 0.032 Uiso 1 1 calc R . . C65 C 0.5927(4) 0.2952(5) 0.53885(19) 0.0302(12) Uani 1 1 d . . . H65 H 0.5796 0.2636 0.5082 0.036 Uiso 1 1 calc R . . C66 C 0.5271(4) 0.3704(4) 0.55238(18) 0.0251(11) Uani 1 1 d . . . H66 H 0.4695 0.3882 0.5310 0.030 Uiso 1 1 calc R . . C71 C 0.4942(3) 0.6544(4) 0.59878(16) 0.0177(9) Uani 1 1 d . . . C72 C 0.4337(4) 0.7436(4) 0.60622(18) 0.0239(11) Uani 1 1 d . . . H72 H 0.3753 0.7305 0.6174 0.029 Uiso 1 1 calc R . . C73 C 0.4603(4) 0.8510(4) 0.59698(18) 0.0251(11) Uani 1 1 d . . . H73 H 0.4199 0.9103 0.6020 0.030 Uiso 1 1 calc R . . C74 C 0.5474(4) 0.8705(4) 0.58022(19) 0.0263(11) Uani 1 1 d . . . H74 H 0.5660 0.9431 0.5746 0.032 Uiso 1 1 calc R . . C75 C 0.6068(4) 0.7828(4) 0.57185(18) 0.0235(10) Uani 1 1 d . . . H75 H 0.6646 0.7962 0.5602 0.028 Uiso 1 1 calc R . . C76 C 0.5801(4) 0.6746(4) 0.58091(17) 0.0203(10) Uani 1 1 d . . . H76 H 0.6197 0.6154 0.5750 0.024 Uiso 1 1 calc R . . C81 C 0.4827(3) 0.5168(4) 0.68085(17) 0.0191(9) Uani 1 1 d . . . C82 C 0.5436(4) 0.5962(5) 0.70779(18) 0.0271(11) Uani 1 1 d . . . H82 H 0.5723 0.6518 0.6920 0.032 Uiso 1 1 calc R . . C83 C 0.5615(4) 0.5924(5) 0.7581(2) 0.0341(13) Uani 1 1 d . . . H83 H 0.6012 0.6460 0.7758 0.041 Uiso 1 1 calc R . . C84 C 0.5200(5) 0.5088(5) 0.7813(2) 0.0367(14) Uani 1 1 d . . . H84 H 0.5321 0.5059 0.8149 0.044 Uiso 1 1 calc R . . C85 C 0.4610(5) 0.4298(5) 0.7553(2) 0.0355(14) Uani 1 1 d . . . H85 H 0.4340 0.3733 0.7714 0.043 Uiso 1 1 calc R . . C86 C 0.4413(4) 0.4334(4) 0.70517(19) 0.0268(11) Uani 1 1 d . . . H86 H 0.4005 0.3802 0.6878 0.032 Uiso 1 1 calc R . . N91 N 0.1719(3) 0.4161(3) 0.54467(13) 0.0162(8) Uani 1 1 d . . . C92 C 0.1674(3) 0.3482(4) 0.50418(17) 0.0181(9) Uani 1 1 d . . . O92 O 0.2380(3) 0.3198(3) 0.48644(13) 0.0276(8) Uani 1 1 d . . . C93 C 0.0622(3) 0.3156(4) 0.48797(17) 0.0183(9) Uani 1 1 d . . . C94 C 0.0173(4) 0.2458(4) 0.45187(18) 0.0246(11) Uani 1 1 d . . . F94 F 0.0676(3) 0.1940(2) 0.42176(11) 0.0352(8) Uani 1 1 d . . . C95 C -0.0834(4) 0.2273(4) 0.44684(18) 0.0279(12) Uani 1 1 d . . . F95 F -0.1286(3) 0.1576(3) 0.41294(12) 0.0415(9) Uani 1 1 d . . . C96 C -0.1368(4) 0.2794(5) 0.47763(18) 0.0275(11) Uani 1 1 d . . . F96 F -0.2337(2) 0.2590(3) 0.47168(12) 0.0431(9) Uani 1 1 d . . . C97 C -0.0916(4) 0.3505(4) 0.51379(18) 0.0222(10) Uani 1 1 d . . . F97 F -0.1461(2) 0.3987(3) 0.54292(11) 0.0333(7) Uani 1 1 d . . . C98 C 0.0080(3) 0.3674(4) 0.51898(16) 0.0178(9) Uani 1 1 d . . . C99 C 0.0788(3) 0.4312(4) 0.55540(17) 0.0174(9) Uani 1 1 d . . . O99 O 0.0590(3) 0.4870(3) 0.58835(12) 0.0248(8) 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 0.02001(9) 0.01862(8) 0.01449(8) -0.00123(7) 0.00482(7) -0.00048(7) P1 0.0169(6) 0.0182(6) 0.0137(5) 0.0011(4) 0.0039(5) 0.0008(5) C11 0.016(2) 0.017(2) 0.018(2) 0.0008(17) 0.0028(18) -0.0008(17) C12 0.018(2) 0.020(2) 0.018(2) -0.0027(19) 0.0039(18) -0.0036(19) C13 0.019(2) 0.029(3) 0.015(2) 0.0051(19) -0.0028(19) -0.004(2) C14 0.019(2) 0.017(2) 0.030(3) 0.005(2) -0.001(2) -0.0006(19) C15 0.019(2) 0.021(2) 0.025(3) -0.003(2) 0.004(2) -0.0008(19) C16 0.024(2) 0.023(2) 0.016(2) -0.0004(19) 0.0044(19) -0.003(2) C21 0.018(2) 0.019(2) 0.014(2) 0.0000(17) 0.0048(17) -0.0013(18) C22 0.024(3) 0.030(3) 0.026(3) 0.007(2) 0.002(2) 0.003(2) C23 0.023(3) 0.041(3) 0.047(4) 0.004(3) 0.015(3) -0.003(2) C24 0.038(3) 0.031(3) 0.031(3) 0.003(2) 0.021(3) -0.003(2) C25 0.043(3) 0.019(2) 0.026(3) 0.006(2) 0.015(2) 0.003(2) C26 0.026(3) 0.025(3) 0.021(2) 0.005(2) 0.008(2) 0.005(2) C31 0.017(2) 0.016(2) 0.019(2) 0.0029(17) 0.0017(18) 0.0049(17) C32 0.023(2) 0.028(3) 0.019(2) -0.004(2) 0.0028(19) 0.001(2) C33 0.037(3) 0.031(3) 0.022(3) -0.009(2) 0.003(2) 0.004(2) C34 0.030(3) 0.024(3) 0.034(3) -0.009(2) -0.006(2) -0.004(2) C35 0.026(3) 0.025(3) 0.038(3) -0.003(2) 0.005(2) -0.006(2) C36 0.026(3) 0.022(2) 0.023(2) 0.000(2) 0.007(2) -0.001(2) N41 0.0178(19) 0.0204(19) 0.0158(18) -0.0029(16) 0.0030(15) -0.0007(16) C42 0.024(2) 0.020(2) 0.016(2) 0.0016(19) 0.0032(19) -0.002(2) O42 0.0253(19) 0.038(2) 0.0188(18) -0.0058(16) 0.0033(15) -0.0075(16) C43 0.023(2) 0.016(2) 0.017(2) 0.0031(18) 0.0054(19) 0.0031(19) C44 0.024(2) 0.026(3) 0.025(3) 0.007(2) 0.007(2) 0.004(2) F44 0.0230(15) 0.047(2) 0.0294(17) 0.0019(15) 0.0042(13) -0.0017(14) C45 0.029(3) 0.020(2) 0.032(3) 0.009(2) 0.017(2) 0.009(2) F45 0.0320(18) 0.0396(18) 0.0396(19) 0.0075(15) 0.0207(16) 0.0112(15) C46 0.043(3) 0.017(2) 0.027(3) 0.001(2) 0.019(2) 0.004(2) F46 0.060(2) 0.0329(17) 0.037(2) -0.0133(15) 0.0299(18) -0.0023(16) C47 0.037(3) 0.017(2) 0.021(2) -0.0047(19) 0.010(2) -0.007(2) F47 0.044(2) 0.0435(19) 0.0275(17) -0.0171(15) 0.0104(15) -0.0151(16) C48 0.028(3) 0.016(2) 0.017(2) -0.0003(18) 0.007(2) -0.0020(19) C49 0.028(3) 0.019(2) 0.015(2) -0.0017(18) 0.008(2) -0.005(2) O49 0.0244(19) 0.039(2) 0.0234(19) -0.0052(16) 0.0045(16) -0.0092(17) Au2 0.01486(8) 0.02025(9) 0.01848(9) -0.00032(7) 0.00040(6) -0.00145(7) P6 0.0159(5) 0.0194(6) 0.0161(6) -0.0006(5) 0.0012(5) -0.0007(5) C61 0.017(2) 0.017(2) 0.021(2) 0.0007(18) 0.0027(19) 0.0001(18) C62 0.025(3) 0.029(3) 0.025(3) -0.006(2) -0.002(2) 0.004(2) C63 0.026(3) 0.028(3) 0.033(3) -0.002(2) -0.003(2) 0.009(2) C64 0.027(3) 0.022(3) 0.033(3) -0.001(2) 0.012(2) 0.002(2) C65 0.034(3) 0.037(3) 0.022(3) -0.006(2) 0.008(2) 0.001(3) C66 0.020(2) 0.033(3) 0.021(2) -0.001(2) 0.000(2) 0.001(2) C71 0.019(2) 0.020(2) 0.013(2) -0.0009(18) 0.0002(18) -0.0019(19) C72 0.023(3) 0.030(3) 0.021(2) 0.003(2) 0.010(2) 0.004(2) C73 0.030(3) 0.022(2) 0.024(3) 0.003(2) 0.007(2) 0.008(2) C74 0.033(3) 0.020(2) 0.025(3) 0.005(2) 0.004(2) 0.000(2) C75 0.021(2) 0.026(2) 0.025(2) 0.005(2) 0.006(2) -0.001(2) C76 0.020(2) 0.021(2) 0.021(2) 0.0011(19) 0.0048(19) 0.0036(19) C81 0.016(2) 0.022(2) 0.020(2) 0.0015(19) 0.0044(18) 0.0035(19) C82 0.029(3) 0.032(3) 0.019(2) 0.003(2) 0.001(2) -0.007(2) C83 0.042(3) 0.038(3) 0.020(3) -0.003(2) -0.003(2) -0.010(3) C84 0.046(4) 0.045(3) 0.018(3) 0.005(2) 0.004(3) 0.002(3) C85 0.047(4) 0.035(3) 0.027(3) 0.010(2) 0.012(3) -0.004(3) C86 0.027(3) 0.026(3) 0.027(3) 0.000(2) 0.004(2) -0.007(2) N91 0.0190(19) 0.0161(18) 0.0130(18) -0.0020(15) 0.0015(15) -0.0034(15) C92 0.020(2) 0.017(2) 0.017(2) 0.0011(18) 0.0038(19) 0.0001(18) O92 0.0257(19) 0.0304(19) 0.029(2) -0.0055(16) 0.0107(16) 0.0021(16) C93 0.019(2) 0.018(2) 0.018(2) 0.0013(17) 0.0047(19) -0.0027(18) C94 0.034(3) 0.023(2) 0.017(2) -0.0019(19) 0.004(2) -0.004(2) F94 0.050(2) 0.0318(17) 0.0260(16) -0.0140(13) 0.0135(15) -0.0084(15) C95 0.039(3) 0.025(3) 0.017(2) -0.002(2) -0.002(2) -0.015(2) F95 0.053(2) 0.0434(19) 0.0251(17) -0.0071(15) -0.0009(16) -0.0278(17) C96 0.023(2) 0.036(3) 0.022(3) 0.006(2) -0.001(2) -0.011(2) F96 0.0234(17) 0.067(2) 0.037(2) 0.0010(17) -0.0005(15) -0.0212(16) C97 0.020(2) 0.029(3) 0.018(2) 0.004(2) 0.0040(19) -0.003(2) F97 0.0178(15) 0.053(2) 0.0311(17) -0.0035(15) 0.0094(13) -0.0021(14) C98 0.019(2) 0.020(2) 0.015(2) 0.0009(17) 0.0024(18) -0.0025(18) C99 0.018(2) 0.017(2) 0.017(2) 0.0002(17) 0.0024(18) -0.0023(18) O99 0.0271(19) 0.0286(19) 0.0202(18) -0.0076(15) 0.0086(15) -0.0022(15) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N41 2.058(4) . ? Au1 P1 2.2370(11) . ? P1 C11 1.810(5) . ? P1 C31 1.817(5) . ? P1 C21 1.819(4) . ? C11 C12 1.395(6) . ? C11 C16 1.400(6) . ? C12 C13 1.383(7) . ? C12 H12 0.9300 . ? C13 C14 1.381(7) . ? C13 H13 0.9300 . ? C14 C15 1.385(7) . ? C14 H14 0.9300 . ? C15 C16 1.378(7) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C21 C26 1.380(6) . ? C21 C22 1.391(7) . ? C22 C23 1.385(7) . ? C22 H22 0.9300 . ? C23 C24 1.379(8) . ? C23 H23 0.9300 . ? C24 C25 1.372(8) . ? C24 H24 0.9300 . ? C25 C26 1.390(7) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C31 C36 1.391(6) . ? C31 C32 1.398(6) . ? C32 C33 1.392(7) . ? C32 H32 0.9300 . ? C33 C34 1.378(8) . ? C33 H33 0.9300 . ? C34 C35 1.381(8) . ? C34 H34 0.9300 . ? C35 C36 1.384(7) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? N41 C42 1.379(6) . ? N41 C49 1.383(6) . ? C42 O42 1.213(6) . ? C42 C43 1.494(6) . ? C43 C44 1.378(6) . ? C43 C48 1.389(7) . ? C44 F44 1.342(6) . ? C44 C45 1.387(7) . ? C45 F45 1.338(5) . ? C45 C46 1.375(8) . ? C46 F46 1.343(5) . ? C46 C47 1.387(7) . ? C47 F47 1.332(6) . ? C47 C48 1.375(6) . ? C48 C49 1.510(6) . ? C49 O49 1.207(6) . ? Au2 N91 2.042(4) . ? Au2 P6 2.2336(12) . ? P6 C81 1.809(5) . ? P6 C71 1.814(5) . ? P6 C61 1.814(5) . ? C61 C66 1.386(7) . ? C61 C62 1.386(7) . ? C62 C63 1.386(7) . ? C62 H62 0.9300 . ? C63 C64 1.374(7) . ? C63 H63 0.9300 . ? C64 C65 1.375(8) . ? C64 H64 0.9300 . ? C65 C66 1.380(7) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C71 C76 1.389(6) . ? C71 C72 1.396(7) . ? C72 C73 1.379(7) . ? C72 H72 0.9300 . ? C73 C74 1.389(7) . ? C73 H73 0.9300 . ? C74 C75 1.380(7) . ? C74 H74 0.9300 . ? C75 C76 1.387(7) . ? C75 H75 0.9300 . ? C76 H76 0.9300 . ? C81 C86 1.392(7) . ? C81 C82 1.399(7) . ? C82 C83 1.390(7) . ? C82 H82 0.9300 . ? C83 C84 1.378(8) . ? C83 H83 0.9300 . ? C84 C85 1.373(8) . ? C84 H84 0.9300 . ? C85 C86 1.386(7) . ? C85 H85 0.9300 . ? C86 H86 0.9300 . ? N91 C99 1.384(6) . ? N91 C92 1.392(6) . ? C92 O92 1.220(5) . ? C92 C93 1.492(6) . ? C93 C94 1.374(7) . ? C93 C98 1.393(6) . ? C94 F94 1.340(6) . ? C94 C95 1.388(7) . ? C95 F95 1.336(6) . ? C95 C96 1.383(7) . ? C96 F96 1.340(6) . ? C96 C97 1.386(7) . ? C97 F97 1.338(5) . ? C97 C98 1.371(6) . ? C98 C99 1.492(6) . ? C99 O99 1.214(5) . ? 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 N41 Au1 P1 171.19(11) . . ? C11 P1 C31 105.3(2) . . ? C11 P1 C21 106.5(2) . . ? C31 P1 C21 106.1(2) . . ? C11 P1 Au1 114.14(15) . . ? C31 P1 Au1 108.23(15) . . ? C21 P1 Au1 115.80(15) . . ? C12 C11 C16 119.0(4) . . ? C12 C11 P1 120.1(3) . . ? C16 C11 P1 120.8(4) . . ? C13 C12 C11 120.3(4) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C14 C13 C12 120.1(4) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 120.2(4) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C16 C15 C14 120.1(4) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C11 120.2(4) . . ? C15 C16 H16 119.9 . . ? C11 C16 H16 119.9 . . ? C26 C21 C22 119.6(4) . . ? C26 C21 P1 118.0(3) . . ? C22 C21 P1 122.3(4) . . ? C23 C22 C21 119.6(5) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C24 C23 C22 120.3(5) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C25 C24 C23 120.4(5) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 119.6(5) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C21 C26 C25 120.5(5) . . ? C21 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C36 C31 C32 119.2(5) . . ? C36 C31 P1 118.2(4) . . ? C32 C31 P1 122.6(4) . . ? C33 C32 C31 119.9(5) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C34 C33 C32 120.3(5) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 C35 119.8(5) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C34 C35 C36 120.6(5) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C35 C36 C31 120.1(5) . . ? C35 C36 H36 119.9 . . ? C31 C36 H36 119.9 . . ? C42 N41 C49 111.4(4) . . ? C42 N41 Au1 119.3(3) . . ? C49 N41 Au1 129.1(3) . . ? O42 C42 N41 126.2(4) . . ? O42 C42 C43 126.5(4) . . ? N41 C42 C43 107.3(4) . . ? C44 C43 C48 120.6(4) . . ? C44 C43 C42 131.9(5) . . ? C48 C43 C42 107.5(4) . . ? F44 C44 C43 122.6(5) . . ? F44 C44 C45 118.9(4) . . ? C43 C44 C45 118.6(5) . . ? F45 C45 C46 119.2(5) . . ? F45 C45 C44 120.1(5) . . ? C46 C45 C44 120.6(5) . . ? F46 C46 C45 119.5(5) . . ? F46 C46 C47 119.6(5) . . ? C45 C46 C47 120.9(5) . . ? F47 C47 C48 122.6(5) . . ? F47 C47 C46 118.9(4) . . ? C48 C47 C46 118.4(5) . . ? C47 C48 C43 120.8(5) . . ? C47 C48 C49 132.1(5) . . ? C43 C48 C49 107.1(4) . . ? O49 C49 N41 126.8(4) . . ? O49 C49 C48 126.5(4) . . ? N41 C49 C48 106.7(4) . . ? N91 Au2 P6 173.90(11) . . ? C81 P6 C71 104.5(2) . . ? C81 P6 C61 105.9(2) . . ? C71 P6 C61 107.0(2) . . ? C81 P6 Au2 115.11(16) . . ? C71 P6 Au2 113.32(16) . . ? C61 P6 Au2 110.36(16) . . ? C66 C61 C62 119.5(4) . . ? C66 C61 P6 119.5(4) . . ? C62 C61 P6 121.0(4) . . ? C61 C62 C63 119.8(5) . . ? C61 C62 H62 120.1 . . ? C63 C62 H62 120.1 . . ? C64 C63 C62 120.4(5) . . ? C64 C63 H63 119.8 . . ? C62 C63 H63 119.8 . . ? C63 C64 C65 119.8(5) . . ? C63 C64 H64 120.1 . . ? C65 C64 H64 120.1 . . ? C64 C65 C66 120.4(5) . . ? C64 C65 H65 119.8 . . ? C66 C65 H65 119.8 . . ? C65 C66 C61 120.0(5) . . ? C65 C66 H66 120.0 . . ? C61 C66 H66 120.0 . . ? C76 C71 C72 119.5(4) . . ? C76 C71 P6 122.6(4) . . ? C72 C71 P6 117.9(3) . . ? C73 C72 C71 120.2(4) . . ? C73 C72 H72 119.9 . . ? C71 C72 H72 119.9 . . ? C72 C73 C74 119.9(5) . . ? C72 C73 H73 120.1 . . ? C74 C73 H73 120.1 . . ? C75 C74 C73 120.4(5) . . ? C75 C74 H74 119.8 . . ? C73 C74 H74 119.8 . . ? C74 C75 C76 119.9(4) . . ? C74 C75 H75 120.1 . . ? C76 C75 H75 120.1 . . ? C75 C76 C71 120.1(4) . . ? C75 C76 H76 119.9 . . ? C71 C76 H76 119.9 . . ? C86 C81 C82 118.9(5) . . ? C86 C81 P6 118.8(4) . . ? C82 C81 P6 122.2(4) . . ? C83 C82 C81 120.5(5) . . ? C83 C82 H82 119.8 . . ? C81 C82 H82 119.8 . . ? C84 C83 C82 119.6(5) . . ? C84 C83 H83 120.2 . . ? C82 C83 H83 120.2 . . ? C85 C84 C83 120.5(5) . . ? C85 C84 H84 119.7 . . ? C83 C84 H84 119.7 . . ? C84 C85 C86 120.6(5) . . ? C84 C85 H85 119.7 . . ? C86 C85 H85 119.7 . . ? C85 C86 C81 119.9(5) . . ? C85 C86 H86 120.0 . . ? C81 C86 H86 120.0 . . ? C99 N91 C92 110.4(4) . . ? C99 N91 Au2 129.8(3) . . ? C92 N91 Au2 119.7(3) . . ? O92 C92 N91 125.2(4) . . ? O92 C92 C93 127.3(4) . . ? N91 C92 C93 107.5(4) . . ? C94 C93 C98 120.9(4) . . ? C94 C93 C92 132.0(4) . . ? C98 C93 C92 107.1(4) . . ? F94 C94 C93 122.3(5) . . ? F94 C94 C95 118.9(5) . . ? C93 C94 C95 118.8(5) . . ? F95 C95 C96 119.8(5) . . ? F95 C95 C94 120.2(5) . . ? C96 C95 C94 120.0(5) . . ? F96 C96 C95 118.1(5) . . ? F96 C96 C97 120.7(5) . . ? C95 C96 C97 121.2(5) . . ? F97 C97 C98 122.2(4) . . ? F97 C97 C96 119.2(4) . . ? C98 C97 C96 118.6(5) . . ? C97 C98 C93 120.6(4) . . ? C97 C98 C99 131.9(4) . . ? C93 C98 C99 107.4(4) . . ? O99 C99 N91 125.8(4) . . ? O99 C99 C98 126.7(4) . . ? N91 C99 C98 107.5(4) . . ? 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 N41 Au1 P1 C11 106.4(8) . . . . ? N41 Au1 P1 C31 -10.5(8) . . . . ? N41 Au1 P1 C21 -129.4(8) . . . . ? C31 P1 C11 C12 121.4(4) . . . . ? C21 P1 C11 C12 -126.2(4) . . . . ? Au1 P1 C11 C12 2.9(4) . . . . ? C31 P1 C11 C16 -55.6(4) . . . . ? C21 P1 C11 C16 56.8(4) . . . . ? Au1 P1 C11 C16 -174.1(3) . . . . ? C16 C11 C12 C13 0.3(7) . . . . ? P1 C11 C12 C13 -176.7(4) . . . . ? C11 C12 C13 C14 0.6(7) . . . . ? C12 C13 C14 C15 -1.4(7) . . . . ? C13 C14 C15 C16 1.2(7) . . . . ? C14 C15 C16 C11 -0.3(7) . . . . ? C12 C11 C16 C15 -0.5(7) . . . . ? P1 C11 C16 C15 176.5(4) . . . . ? C11 P1 C21 C26 -163.4(4) . . . . ? C31 P1 C21 C26 -51.6(4) . . . . ? Au1 P1 C21 C26 68.5(4) . . . . ? C11 P1 C21 C22 19.7(5) . . . . ? C31 P1 C21 C22 131.5(4) . . . . ? Au1 P1 C21 C22 -108.4(4) . . . . ? C26 C21 C22 C23 -0.8(8) . . . . ? P1 C21 C22 C23 176.1(4) . . . . ? C21 C22 C23 C24 1.1(9) . . . . ? C22 C23 C24 C25 -0.5(9) . . . . ? C23 C24 C25 C26 -0.3(8) . . . . ? C22 C21 C26 C25 0.0(7) . . . . ? P1 C21 C26 C25 -177.1(4) . . . . ? C24 C25 C26 C21 0.6(8) . . . . ? C11 P1 C31 C36 -92.7(4) . . . . ? C21 P1 C31 C36 154.6(4) . . . . ? Au1 P1 C31 C36 29.7(4) . . . . ? C11 P1 C31 C32 84.8(4) . . . . ? C21 P1 C31 C32 -27.9(4) . . . . ? Au1 P1 C31 C32 -152.8(4) . . . . ? C36 C31 C32 C33 -0.4(7) . . . . ? P1 C31 C32 C33 -177.9(4) . . . . ? C31 C32 C33 C34 0.5(8) . . . . ? C32 C33 C34 C35 0.0(8) . . . . ? C33 C34 C35 C36 -0.5(8) . . . . ? C34 C35 C36 C31 0.6(8) . . . . ? C32 C31 C36 C35 -0.1(7) . . . . ? P1 C31 C36 C35 177.5(4) . . . . ? P1 Au1 N41 C42 5.2(10) . . . . ? P1 Au1 N41 C49 -169.4(5) . . . . ? C49 N41 C42 O42 -179.5(5) . . . . ? Au1 N41 C42 O42 5.0(7) . . . . ? C49 N41 C42 C43 0.7(5) . . . . ? Au1 N41 C42 C43 -174.8(3) . . . . ? O42 C42 C43 C44 -3.1(9) . . . . ? N41 C42 C43 C44 176.7(5) . . . . ? O42 C42 C43 C48 178.5(5) . . . . ? N41 C42 C43 C48 -1.7(5) . . . . ? C48 C43 C44 F44 -179.8(4) . . . . ? C42 C43 C44 F44 2.0(8) . . . . ? C48 C43 C44 C45 0.5(7) . . . . ? C42 C43 C44 C45 -177.7(5) . . . . ? F44 C44 C45 F45 -0.9(7) . . . . ? C43 C44 C45 F45 178.9(4) . . . . ? F44 C44 C45 C46 178.2(4) . . . . ? C43 C44 C45 C46 -2.0(7) . . . . ? F45 C45 C46 F46 0.5(7) . . . . ? C44 C45 C46 F46 -178.6(4) . . . . ? F45 C45 C46 C47 -179.3(4) . . . . ? C44 C45 C46 C47 1.6(8) . . . . ? F46 C46 C47 F47 -0.4(7) . . . . ? C45 C46 C47 F47 179.5(5) . . . . ? F46 C46 C47 C48 -179.4(4) . . . . ? C45 C46 C47 C48 0.5(7) . . . . ? F47 C47 C48 C43 179.0(4) . . . . ? C46 C47 C48 C43 -2.0(7) . . . . ? F47 C47 C48 C49 -3.2(8) . . . . ? C46 C47 C48 C49 175.7(5) . . . . ? C44 C43 C48 C47 1.6(7) . . . . ? C42 C43 C48 C47 -179.8(4) . . . . ? C44 C43 C48 C49 -176.7(4) . . . . ? C42 C43 C48 C49 1.9(5) . . . . ? C42 N41 C49 O49 -176.9(5) . . . . ? Au1 N41 C49 O49 -1.9(7) . . . . ? C42 N41 C49 C48 0.4(5) . . . . ? Au1 N41 C49 C48 175.4(3) . . . . ? C47 C48 C49 O49 -2.2(9) . . . . ? C43 C48 C49 O49 175.8(5) . . . . ? C47 C48 C49 N41 -179.5(5) . . . . ? C43 C48 C49 N41 -1.5(5) . . . . ? N91 Au2 P6 C81 -135.5(10) . . . . ? N91 Au2 P6 C71 104.2(10) . . . . ? N91 Au2 P6 C61 -15.7(11) . . . . ? C81 P6 C61 C66 157.3(4) . . . . ? C71 P6 C61 C66 -91.6(4) . . . . ? Au2 P6 C61 C66 32.1(4) . . . . ? C81 P6 C61 C62 -22.1(5) . . . . ? C71 P6 C61 C62 89.0(4) . . . . ? Au2 P6 C61 C62 -147.2(4) . . . . ? C66 C61 C62 C63 -1.3(8) . . . . ? P6 C61 C62 C63 178.1(4) . . . . ? C61 C62 C63 C64 0.7(8) . . . . ? C62 C63 C64 C65 0.8(8) . . . . ? C63 C64 C65 C66 -1.7(8) . . . . ? C64 C65 C66 C61 1.1(8) . . . . ? C62 C61 C66 C65 0.4(7) . . . . ? P6 C61 C66 C65 -179.0(4) . . . . ? C81 P6 C71 C76 105.9(4) . . . . ? C61 P6 C71 C76 -6.2(5) . . . . ? Au2 P6 C71 C76 -128.1(4) . . . . ? C81 P6 C71 C72 -71.6(4) . . . . ? C61 P6 C71 C72 176.3(4) . . . . ? Au2 P6 C71 C72 54.4(4) . . . . ? C76 C71 C72 C73 -1.6(8) . . . . ? P6 C71 C72 C73 176.0(4) . . . . ? C71 C72 C73 C74 0.0(8) . . . . ? C72 C73 C74 C75 1.3(8) . . . . ? C73 C74 C75 C76 -1.0(8) . . . . ? C74 C75 C76 C71 -0.6(8) . . . . ? C72 C71 C76 C75 1.8(7) . . . . ? P6 C71 C76 C75 -175.6(4) . . . . ? C71 P6 C81 C86 164.4(4) . . . . ? C61 P6 C81 C86 -82.8(4) . . . . ? Au2 P6 C81 C86 39.4(4) . . . . ? C71 P6 C81 C82 -17.7(5) . . . . ? C61 P6 C81 C82 95.1(4) . . . . ? Au2 P6 C81 C82 -142.7(4) . . . . ? C86 C81 C82 C83 -0.8(8) . . . . ? P6 C81 C82 C83 -178.7(4) . . . . ? C81 C82 C83 C84 1.0(9) . . . . ? C82 C83 C84 C85 -0.3(9) . . . . ? C83 C84 C85 C86 -0.7(9) . . . . ? C84 C85 C86 C81 0.9(9) . . . . ? C82 C81 C86 C85 -0.2(8) . . . . ? P6 C81 C86 C85 177.8(4) . . . . ? P6 Au2 N91 C99 170.7(8) . . . . ? P6 Au2 N91 C92 -4.9(13) . . . . ? C99 N91 C92 O92 -179.5(5) . . . . ? Au2 N91 C92 O92 -3.1(6) . . . . ? C99 N91 C92 C93 -0.9(5) . . . . ? Au2 N91 C92 C93 175.5(3) . . . . ? O92 C92 C93 C94 2.5(9) . . . . ? N91 C92 C93 C94 -176.1(5) . . . . ? O92 C92 C93 C98 179.8(5) . . . . ? N91 C92 C93 C98 1.2(5) . . . . ? C98 C93 C94 F94 -179.4(4) . . . . ? C92 C93 C94 F94 -2.4(8) . . . . ? C98 C93 C94 C95 -0.2(7) . . . . ? C92 C93 C94 C95 176.8(5) . . . . ? F94 C94 C95 F95 1.1(7) . . . . ? C93 C94 C95 F95 -178.2(4) . . . . ? F94 C94 C95 C96 179.7(5) . . . . ? C93 C94 C95 C96 0.4(8) . . . . ? F95 C95 C96 F96 -1.1(7) . . . . ? C94 C95 C96 F96 -179.7(5) . . . . ? F95 C95 C96 C97 178.7(5) . . . . ? C94 C95 C96 C97 0.1(8) . . . . ? F96 C96 C97 F97 0.1(7) . . . . ? C95 C96 C97 F97 -179.7(5) . . . . ? F96 C96 C97 C98 179.0(5) . . . . ? C95 C96 C97 C98 -0.8(8) . . . . ? F97 C97 C98 C93 179.9(4) . . . . ? C96 C97 C98 C93 1.1(7) . . . . ? F97 C97 C98 C99 3.4(8) . . . . ? C96 C97 C98 C99 -175.4(5) . . . . ? C94 C93 C98 C97 -0.6(7) . . . . ? C92 C93 C98 C97 -178.3(4) . . . . ? C94 C93 C98 C99 176.7(4) . . . . ? C92 C93 C98 C99 -1.0(5) . . . . ? C92 N91 C99 O99 -179.3(5) . . . . ? Au2 N91 C99 O99 4.8(7) . . . . ? C92 N91 C99 C98 0.3(5) . . . . ? Au2 N91 C99 C98 -175.6(3) . . . . ? C97 C98 C99 O99 -3.1(9) . . . . ? C93 C98 C99 O99 -180.0(5) . . . . ? C97 C98 C99 N91 177.3(5) . . . . ? C93 C98 C99 N91 0.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.805 _refine_diff_density_min -2.431 _refine_diff_density_rms 0.165 #===END data_nickys16 _database_code_depnum_ccdc_archive 'CCDC 791411' #TrackingRef '- combined.cif' _audit_creation_method 'SHELXL-97 and CrysAlisPro RED' _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 8b' _chemical_melting_point ? _chemical_formula_structural '[F4-phthalimido-Au-P(Cy)3].0.5(toluene)' _chemical_formula_moiety 'C26 H33 Au F4 N O2 P, 0.5(C7 H8)' _chemical_formula_sum 'C29.50 H37 Au F4 N O2 P' _chemical_formula_weight 741.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3527(8) _cell_length_b 11.7282(9) _cell_length_c 11.9341(9) _cell_angle_alpha 74.895(6) _cell_angle_beta 69.615(7) _cell_angle_gamma 72.833(6) _cell_volume 1400.86(18) _cell_formula_units_Z 2 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used 7491 _cell_measurement_theta_min 3.3682 _cell_measurement_theta_max 32.3063 _exptl_crystal_description 'block, cut from prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.758 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 734 _exptl_absorpt_coefficient_mu 5.363 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.796 _exptl_absorpt_correction_T_max 1.159 _exptl_absorpt_process_details ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_reflns_number 15566 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 30.00 _reflns_number_total 8119 _reflns_number_gt 7071 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlisPro CCD, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_cell_refinement ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_data_reduction ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Johnson, 1976 and Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008) and WINGX (Farrugia, 1999)' _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^ > 2\s(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^)+(0.0524P)^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 8119 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0833 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 Au Au 0.281860(12) 0.446955(12) 0.389715(12) 0.01642(5) Uani 1 1 d . . . N11 N 0.3336(3) 0.5353(3) 0.2133(3) 0.0180(6) Uani 1 1 d . . . C12 C 0.4594(3) 0.5476(3) 0.1561(3) 0.0192(7) Uani 1 1 d . . . O12 O 0.5508(3) 0.4983(3) 0.1947(3) 0.0270(6) Uani 1 1 d . . . C13 C 0.4605(3) 0.6333(3) 0.0387(3) 0.0183(7) Uani 1 1 d . . . C14 C 0.5582(4) 0.6766(4) -0.0526(4) 0.0219(7) Uani 1 1 d . . . F14 F 0.6811(2) 0.6420(2) -0.0503(2) 0.0317(6) Uani 1 1 d . . . C15 C 0.5289(4) 0.7600(4) -0.1512(4) 0.0269(8) Uani 1 1 d . . . F15 F 0.6219(3) 0.8043(3) -0.2410(2) 0.0380(6) Uani 1 1 d . . . C16 C 0.4027(4) 0.7989(4) -0.1558(3) 0.0250(8) Uani 1 1 d . . . F16 F 0.3765(3) 0.8806(2) -0.2507(2) 0.0365(6) Uani 1 1 d . . . C17 C 0.3038(4) 0.7548(3) -0.0633(4) 0.0219(7) Uani 1 1 d . . . F17 F 0.1839(2) 0.7967(2) -0.0725(2) 0.0299(5) Uani 1 1 d . . . C18 C 0.3343(3) 0.6714(3) 0.0318(3) 0.0186(7) Uani 1 1 d . . . C19 C 0.2532(3) 0.6063(3) 0.1446(3) 0.0182(7) Uani 1 1 d . . . O19 O 0.1384(2) 0.6139(3) 0.1700(3) 0.0255(6) Uani 1 1 d . . . P2 P 0.24182(8) 0.36245(8) 0.58733(8) 0.01462(16) Uani 1 1 d . . . C21 C 0.1233(3) 0.2663(3) 0.6425(3) 0.0175(7) Uani 1 1 d . . . H21 H 0.0378 0.3211 0.6610 0.021 Uiso 1 1 calc R . . C22 C 0.1308(4) 0.2028(3) 0.5409(4) 0.0215(7) Uani 1 1 d . . . H22A H 0.1200 0.2633 0.4701 0.026 Uiso 1 1 calc R . . H22B H 0.2152 0.1491 0.5179 0.026 Uiso 1 1 calc R . . C23 C 0.0265(4) 0.1297(4) 0.5829(4) 0.0310(9) Uani 1 1 d . . . H23A H -0.0580 0.1844 0.5993 0.037 Uiso 1 1 calc R . . H23B H 0.0356 0.0884 0.5188 0.037 Uiso 1 1 calc R . . C24 C 0.0373(4) 0.0377(4) 0.6963(5) 0.0326(10) Uani 1 1 d . . . H24A H 0.1190 -0.0209 0.6781 0.039 Uiso 1 1 calc R . . H24B H -0.0314 -0.0054 0.7229 0.039 Uiso 1 1 calc R . . C25 C 0.0285(4) 0.0992(4) 0.7973(4) 0.0312(9) Uani 1 1 d . . . H25A H 0.0395 0.0379 0.8675 0.037 Uiso 1 1 calc R . . H25B H -0.0567 0.1515 0.8208 0.037 Uiso 1 1 calc R . . C26 C 0.1297(4) 0.1743(4) 0.7599(4) 0.0240(8) Uani 1 1 d . . . H26A H 0.2149 0.1209 0.7473 0.029 Uiso 1 1 calc R . . H26B H 0.1154 0.2172 0.8245 0.029 Uiso 1 1 calc R . . C31 C 0.3937(3) 0.2728(3) 0.6185(3) 0.0168(6) Uani 1 1 d . . . H31 H 0.3763 0.2447 0.7064 0.020 Uiso 1 1 calc R . . C32 C 0.4489(3) 0.1617(4) 0.5555(4) 0.0223(7) Uani 1 1 d . . . H32A H 0.3880 0.1096 0.5867 0.027 Uiso 1 1 calc R . . H32B H 0.4604 0.1880 0.4691 0.027 Uiso 1 1 calc R . . C33 C 0.5780(4) 0.0900(4) 0.5761(5) 0.0292(9) Uani 1 1 d . . . H33A H 0.6117 0.0224 0.5326 0.035 Uiso 1 1 calc R . . H33B H 0.5652 0.0574 0.6619 0.035 Uiso 1 1 calc R . . C34 C 0.6757(4) 0.1698(4) 0.5327(5) 0.0325(10) Uani 1 1 d . . . H34A H 0.7553 0.1232 0.5504 0.039 Uiso 1 1 calc R . . H34B H 0.6948 0.1963 0.4455 0.039 Uiso 1 1 calc R . . C35 C 0.6230(3) 0.2803(4) 0.5953(4) 0.0228(7) Uani 1 1 d . . . H35A H 0.6126 0.2540 0.6816 0.027 Uiso 1 1 calc R . . H35B H 0.6840 0.3322 0.5630 0.027 Uiso 1 1 calc R . . C36 C 0.4933(3) 0.3516(3) 0.5761(4) 0.0196(7) Uani 1 1 d . . . H36A H 0.5059 0.3853 0.4905 0.023 Uiso 1 1 calc R . . H36B H 0.4601 0.4186 0.6204 0.023 Uiso 1 1 calc R . . C41 C 0.1839(3) 0.4862(3) 0.6751(3) 0.0164(6) Uani 1 1 d . . . H41 H 0.2522 0.5315 0.6448 0.020 Uiso 1 1 calc R . . C42 C 0.0643(3) 0.5763(3) 0.6459(3) 0.0188(7) Uani 1 1 d . . . H42A H 0.0816 0.6009 0.5586 0.023 Uiso 1 1 calc R . . H42B H -0.0079 0.5373 0.6761 0.023 Uiso 1 1 calc R . . C43 C 0.0294(4) 0.6886(4) 0.7048(4) 0.0238(8) Uani 1 1 d . . . H43A H 0.0971 0.7332 0.6668 0.029 Uiso 1 1 calc R . . H43B H -0.0499 0.7414 0.6911 0.029 Uiso 1 1 calc R . . C44 C 0.0122(4) 0.6538(4) 0.8405(4) 0.0246(8) Uani 1 1 d . . . H44A H -0.0627 0.6187 0.8800 0.030 Uiso 1 1 calc R . . H44B H -0.0030 0.7259 0.8735 0.030 Uiso 1 1 calc R . . C45 C 0.1304(4) 0.5632(4) 0.8675(4) 0.0230(8) Uani 1 1 d . . . H45A H 0.1148 0.5400 0.9547 0.028 Uiso 1 1 calc R . . H45B H 0.2036 0.6010 0.8348 0.028 Uiso 1 1 calc R . . C46 C 0.1624(4) 0.4499(3) 0.8121(3) 0.0210(7) Uani 1 1 d . . . H46A H 0.2395 0.3949 0.8284 0.025 Uiso 1 1 calc R . . H46B H 0.0920 0.4085 0.8485 0.025 Uiso 1 1 calc R . . C51 C 0.4366(13) 1.0262(11) 0.0065(10) 0.053(3) Uani 0.50 1 d P A -1 C52 C 0.4901(8) 0.9138(6) 0.0780(6) 0.0615(18) Uani 0.50 1 d P A -1 H52 H 0.4406 0.8644 0.1386 0.074 Uiso 0.50 1 calc PR A -1 C53 C 0.634(2) 0.8878(11) 0.0417(11) 0.080(6) Uani 0.50 1 d P A -1 H53 H 0.6753 0.8198 0.0859 0.096 Uiso 0.50 1 calc PR A -1 C54 C 0.7046(8) 0.9489(8) -0.0423(7) 0.072(2) Uani 0.50 1 d P A -1 H54 H 0.7937 0.9214 -0.0602 0.086 Uiso 0.50 1 calc PR A -1 C55 C 0.6522(11) 1.0612(10) -0.1129(10) 0.044(2) Uani 0.50 1 d P A -1 H55 H 0.7019 1.1111 -0.1726 0.053 Uiso 0.50 1 calc PR A -1 C56 C 0.5099(8) 1.0862(6) -0.0780(6) 0.0615(18) Uani 0.50 1 d P A -1 H56 H 0.4697 1.1539 -0.1233 0.074 Uiso 0.50 1 calc PR A -1 C57 C 0.2954(8) 1.0511(8) 0.0423(7) 0.072(2) Uani 0.50 1 d P A -1 H57A H 0.2633 1.1251 -0.0065 0.107 Uiso 0.50 1 calc PR A -1 H57B H 0.2612 1.0590 0.1264 0.107 Uiso 0.50 1 calc PR A -1 H57C H 0.2691 0.9855 0.0304 0.107 Uiso 0.50 1 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au 0.01947(7) 0.01509(7) 0.01502(7) -0.00062(4) -0.00661(5) -0.00431(5) N11 0.0178(13) 0.0180(14) 0.0177(15) -0.0034(11) -0.0052(11) -0.0033(11) C12 0.0213(16) 0.0187(16) 0.0183(17) -0.0024(13) -0.0076(13) -0.0044(13) O12 0.0218(13) 0.0352(16) 0.0243(15) -0.0004(12) -0.0129(11) -0.0038(12) C13 0.0215(16) 0.0155(15) 0.0189(18) -0.0043(13) -0.0072(13) -0.0032(13) C14 0.0200(16) 0.0217(18) 0.0238(19) -0.0053(14) -0.0043(14) -0.0058(14) F14 0.0195(11) 0.0391(15) 0.0357(15) -0.0039(11) -0.0057(10) -0.0108(10) C15 0.031(2) 0.0230(19) 0.025(2) -0.0002(15) -0.0038(16) -0.0124(16) F15 0.0427(15) 0.0352(15) 0.0291(14) 0.0052(11) 0.0001(11) -0.0210(12) C16 0.039(2) 0.0182(17) 0.0149(18) 0.0024(14) -0.0084(15) -0.0057(16) F16 0.0508(16) 0.0288(13) 0.0211(13) 0.0078(10) -0.0116(11) -0.0054(12) C17 0.0255(18) 0.0166(16) 0.0233(19) -0.0036(14) -0.0105(15) -0.0006(14) F17 0.0285(12) 0.0283(13) 0.0310(14) 0.0010(10) -0.0169(10) 0.0006(10) C18 0.0197(16) 0.0163(16) 0.0197(18) -0.0017(13) -0.0073(13) -0.0035(13) C19 0.0211(16) 0.0163(16) 0.0143(16) -0.0026(12) -0.0031(13) -0.0028(13) O19 0.0174(12) 0.0277(15) 0.0294(16) -0.0025(12) -0.0070(11) -0.0042(11) P2 0.0171(4) 0.0122(4) 0.0154(4) -0.0018(3) -0.0061(3) -0.0035(3) C21 0.0177(15) 0.0153(15) 0.0195(18) -0.0046(13) -0.0047(13) -0.0034(13) C22 0.0227(17) 0.0197(17) 0.027(2) -0.0034(14) -0.0126(15) -0.0060(14) C23 0.030(2) 0.027(2) 0.044(3) -0.0058(18) -0.0177(18) -0.0112(17) C24 0.033(2) 0.0187(19) 0.049(3) -0.0066(18) -0.0094(19) -0.0130(17) C25 0.034(2) 0.0201(19) 0.034(2) 0.0018(16) -0.0022(18) -0.0133(17) C26 0.0263(18) 0.0202(18) 0.025(2) 0.0017(15) -0.0068(15) -0.0104(15) C31 0.0173(15) 0.0136(15) 0.0195(17) -0.0024(12) -0.0062(13) -0.0031(12) C32 0.0182(16) 0.0201(17) 0.032(2) -0.0088(15) -0.0105(15) -0.0023(14) C33 0.0210(18) 0.0207(19) 0.052(3) -0.0164(18) -0.0159(18) 0.0016(15) C34 0.0141(16) 0.038(2) 0.049(3) -0.018(2) -0.0079(17) -0.0037(16) C35 0.0200(16) 0.0234(18) 0.030(2) -0.0047(15) -0.0086(14) -0.0100(14) C36 0.0226(16) 0.0152(16) 0.0240(19) -0.0031(13) -0.0075(14) -0.0082(13) C41 0.0177(15) 0.0132(15) 0.0184(17) -0.0014(12) -0.0066(13) -0.0031(12) C42 0.0206(16) 0.0178(16) 0.0175(17) -0.0052(13) -0.0071(13) 0.0000(13) C43 0.0244(17) 0.0207(18) 0.027(2) -0.0086(15) -0.0112(15) 0.0020(15) C44 0.0204(17) 0.028(2) 0.024(2) -0.0101(15) -0.0054(14) 0.0006(15) C45 0.0251(18) 0.0258(19) 0.0198(18) -0.0065(15) -0.0096(14) -0.0027(15) C46 0.0195(16) 0.0198(17) 0.0223(19) -0.0031(14) -0.0090(14) 0.0004(14) C51 0.089(8) 0.050(7) 0.029(5) -0.018(5) -0.004(6) -0.036(7) C52 0.108(6) 0.044(3) 0.040(3) -0.010(3) -0.029(4) -0.015(4) C53 0.171(18) 0.029(6) 0.028(6) 0.001(5) -0.041(9) 0.004(8) C54 0.080(5) 0.084(6) 0.064(5) -0.024(4) -0.030(4) -0.017(4) C55 0.057(6) 0.038(5) 0.037(6) -0.001(4) -0.021(5) -0.008(5) C56 0.108(6) 0.044(3) 0.040(3) -0.010(3) -0.029(4) -0.015(4) C57 0.080(5) 0.084(6) 0.064(5) -0.024(4) -0.030(4) -0.017(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Au N11 2.052(3) . ? Au P2 2.2476(9) . ? N11 C19 1.383(4) . ? N11 C12 1.385(5) . ? C12 O12 1.210(4) . ? C12 C13 1.495(5) . ? C13 C14 1.370(5) . ? C13 C18 1.394(5) . ? C14 F14 1.341(4) . ? C14 C15 1.391(6) . ? C15 F15 1.333(5) . ? C15 C16 1.385(6) . ? C16 F16 1.338(4) . ? C16 C17 1.389(6) . ? C17 F17 1.337(4) . ? C17 C18 1.363(5) . ? C18 C19 1.503(5) . ? C19 O19 1.212(5) . ? P2 C41 1.840(4) . ? P2 C31 1.841(3) . ? P2 C21 1.846(4) . ? C21 C26 1.539(5) . ? C21 C22 1.546(5) . ? C21 H21 0.9800 . ? C22 C23 1.533(6) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.512(6) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.520(7) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.527(6) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C31 C32 1.535(5) . ? C31 C36 1.538(5) . ? C31 H31 0.9800 . ? C32 C33 1.527(5) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.529(6) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.526(6) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.525(5) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C41 C46 1.528(5) . ? C41 C42 1.541(5) . ? C41 H41 0.9800 . ? C42 C43 1.539(5) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.520(6) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.521(5) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.529(5) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C51 C56 1.263(14) . ? C51 C52 1.462(14) . ? C51 C57 1.466(15) . ? C52 C53 1.50(2) . ? C52 H52 0.9300 . ? C53 C54 1.250(19) . ? C53 H53 0.9300 . ? C54 C55 1.452(12) . ? C54 H54 0.9300 . ? C55 C56 1.478(14) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? 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 N11 Au P2 172.54(9) . . ? C19 N11 C12 110.8(3) . . ? C19 N11 Au 127.8(2) . . ? C12 N11 Au 120.3(2) . . ? O12 C12 N11 126.1(4) . . ? O12 C12 C13 126.7(4) . . ? N11 C12 C13 107.2(3) . . ? C14 C13 C18 120.4(3) . . ? C14 C13 C12 131.8(3) . . ? C18 C13 C12 107.8(3) . . ? F14 C14 C13 122.5(3) . . ? F14 C14 C15 118.7(3) . . ? C13 C14 C15 118.8(3) . . ? F15 C15 C16 119.7(4) . . ? F15 C15 C14 120.1(4) . . ? C16 C15 C14 120.2(4) . . ? F16 C16 C15 119.2(4) . . ? F16 C16 C17 119.9(4) . . ? C15 C16 C17 120.9(3) . . ? F17 C17 C18 123.7(4) . . ? F17 C17 C16 118.0(3) . . ? C18 C17 C16 118.3(3) . . ? C17 C18 C13 121.4(4) . . ? C17 C18 C19 132.1(3) . . ? C13 C18 C19 106.5(3) . . ? O19 C19 N11 126.3(3) . . ? O19 C19 C18 126.0(3) . . ? N11 C19 C18 107.7(3) . . ? C41 P2 C31 105.93(16) . . ? C41 P2 C21 109.29(16) . . ? C31 P2 C21 109.13(16) . . ? C41 P2 Au 107.49(12) . . ? C31 P2 Au 109.60(12) . . ? C21 P2 Au 115.00(12) . . ? C26 C21 C22 111.0(3) . . ? C26 C21 P2 115.1(3) . . ? C22 C21 P2 110.7(3) . . ? C26 C21 H21 106.5 . . ? C22 C21 H21 106.5 . . ? P2 C21 H21 106.5 . . ? C23 C22 C21 111.2(3) . . ? C23 C22 H22A 109.4 . . ? C21 C22 H22A 109.4 . . ? C23 C22 H22B 109.4 . . ? C21 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C24 C23 C22 110.9(3) . . ? C24 C23 H23A 109.5 . . ? C22 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 108.1 . . ? C23 C24 C25 110.8(4) . . ? C23 C24 H24A 109.5 . . ? C25 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? C24 C25 C26 112.6(4) . . ? C24 C25 H25A 109.1 . . ? C26 C25 H25A 109.1 . . ? C24 C25 H25B 109.1 . . ? C26 C25 H25B 109.1 . . ? H25A C25 H25B 107.8 . . ? C25 C26 C21 111.0(3) . . ? C25 C26 H26A 109.4 . . ? C21 C26 H26A 109.4 . . ? C25 C26 H26B 109.4 . . ? C21 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C32 C31 C36 109.7(3) . . ? C32 C31 P2 111.2(3) . . ? C36 C31 P2 110.2(2) . . ? C32 C31 H31 108.6 . . ? C36 C31 H31 108.6 . . ? P2 C31 H31 108.6 . . ? C33 C32 C31 111.5(3) . . ? C33 C32 H32A 109.3 . . ? C31 C32 H32A 109.3 . . ? C33 C32 H32B 109.3 . . ? C31 C32 H32B 109.3 . . ? H32A C32 H32B 108.0 . . ? C32 C33 C34 111.2(4) . . ? C32 C33 H33A 109.4 . . ? C34 C33 H33A 109.4 . . ? C32 C33 H33B 109.4 . . ? C34 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? C35 C34 C33 110.7(3) . . ? C35 C34 H34A 109.5 . . ? C33 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? C36 C35 C34 111.0(3) . . ? C36 C35 H35A 109.4 . . ? C34 C35 H35A 109.4 . . ? C36 C35 H35B 109.4 . . ? C34 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? C35 C36 C31 112.4(3) . . ? C35 C36 H36A 109.1 . . ? C31 C36 H36A 109.1 . . ? C35 C36 H36B 109.1 . . ? C31 C36 H36B 109.1 . . ? H36A C36 H36B 107.9 . . ? C46 C41 C42 111.1(3) . . ? C46 C41 P2 116.9(2) . . ? C42 C41 P2 111.0(2) . . ? C46 C41 H41 105.6 . . ? C42 C41 H41 105.6 . . ? P2 C41 H41 105.6 . . ? C43 C42 C41 110.3(3) . . ? C43 C42 H42A 109.6 . . ? C41 C42 H42A 109.6 . . ? C43 C42 H42B 109.6 . . ? C41 C42 H42B 109.6 . . ? H42A C42 H42B 108.1 . . ? C44 C43 C42 111.6(3) . . ? C44 C43 H43A 109.3 . . ? C42 C43 H43A 109.3 . . ? C44 C43 H43B 109.3 . . ? C42 C43 H43B 109.3 . . ? H43A C43 H43B 108.0 . . ? C43 C44 C45 111.5(3) . . ? C43 C44 H44A 109.3 . . ? C45 C44 H44A 109.3 . . ? C43 C44 H44B 109.3 . . ? C45 C44 H44B 109.3 . . ? H44A C44 H44B 108.0 . . ? C44 C45 C46 111.4(3) . . ? C44 C45 H45A 109.3 . . ? C46 C45 H45A 109.3 . . ? C44 C45 H45B 109.3 . . ? C46 C45 H45B 109.3 . . ? H45A C45 H45B 108.0 . . ? C41 C46 C45 109.6(3) . . ? C41 C46 H46A 109.8 . . ? C45 C46 H46A 109.8 . . ? C41 C46 H46B 109.8 . . ? C45 C46 H46B 109.8 . . ? H46A C46 H46B 108.2 . . ? C56 C51 C52 120.7(11) . . ? C56 C51 C57 127.7(12) . . ? C52 C51 C57 111.5(10) . . ? C51 C52 C53 111.7(9) . . ? C51 C52 H52 124.1 . . ? C53 C52 H52 124.1 . . ? C54 C53 C52 126.2(10) . . ? C54 C53 H53 116.9 . . ? C52 C53 H53 116.9 . . ? C53 C54 C55 122.3(11) . . ? C53 C54 H54 118.9 . . ? C55 C54 H54 118.9 . . ? C54 C55 C56 111.4(9) . . ? C54 C55 H55 124.3 . . ? C56 C55 H55 124.3 . . ? C51 C56 C55 127.4(10) . . ? C51 C56 H56 116.3 . . ? C55 C56 H56 116.3 . . ? 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 P2 Au N11 C19 -127.3(6) . . . . ? P2 Au N11 C12 40.1(8) . . . . ? C19 N11 C12 O12 178.8(4) . . . . ? Au N11 C12 O12 9.4(6) . . . . ? C19 N11 C12 C13 -0.9(4) . . . . ? Au N11 C12 C13 -170.3(2) . . . . ? O12 C12 C13 C14 0.5(7) . . . . ? N11 C12 C13 C14 -179.7(4) . . . . ? O12 C12 C13 C18 -178.2(4) . . . . ? N11 C12 C13 C18 1.6(4) . . . . ? C18 C13 C14 F14 -179.6(4) . . . . ? C12 C13 C14 F14 1.9(7) . . . . ? C18 C13 C14 C15 0.6(6) . . . . ? C12 C13 C14 C15 -177.9(4) . . . . ? F14 C14 C15 F15 -0.2(6) . . . . ? C13 C14 C15 F15 179.6(4) . . . . ? F14 C14 C15 C16 -179.2(4) . . . . ? C13 C14 C15 C16 0.6(6) . . . . ? F15 C15 C16 F16 0.0(6) . . . . ? C14 C15 C16 F16 179.0(4) . . . . ? F15 C15 C16 C17 -179.7(4) . . . . ? C14 C15 C16 C17 -0.7(7) . . . . ? F16 C16 C17 F17 -0.3(6) . . . . ? C15 C16 C17 F17 179.4(4) . . . . ? F16 C16 C17 C18 179.9(4) . . . . ? C15 C16 C17 C18 -0.5(6) . . . . ? F17 C17 C18 C13 -178.1(4) . . . . ? C16 C17 C18 C13 1.7(6) . . . . ? F17 C17 C18 C19 0.1(7) . . . . ? C16 C17 C18 C19 179.9(4) . . . . ? C14 C13 C18 C17 -1.8(6) . . . . ? C12 C13 C18 C17 177.0(4) . . . . ? C14 C13 C18 C19 179.6(4) . . . . ? C12 C13 C18 C19 -1.6(4) . . . . ? C12 N11 C19 O19 179.2(4) . . . . ? Au N11 C19 O19 -12.4(6) . . . . ? C12 N11 C19 C18 0.0(4) . . . . ? Au N11 C19 C18 168.4(2) . . . . ? C17 C18 C19 O19 3.5(7) . . . . ? C13 C18 C19 O19 -178.2(4) . . . . ? C17 C18 C19 N11 -177.3(4) . . . . ? C13 C18 C19 N11 1.0(4) . . . . ? N11 Au P2 C41 54.5(7) . . . . ? N11 Au P2 C31 -60.2(7) . . . . ? N11 Au P2 C21 176.4(6) . . . . ? C41 P2 C21 C26 -79.7(3) . . . . ? C31 P2 C21 C26 35.7(3) . . . . ? Au P2 C21 C26 159.4(2) . . . . ? C41 P2 C21 C22 153.4(2) . . . . ? C31 P2 C21 C22 -91.2(3) . . . . ? Au P2 C21 C22 32.4(3) . . . . ? C26 C21 C22 C23 54.8(4) . . . . ? P2 C21 C22 C23 -176.0(3) . . . . ? C21 C22 C23 C24 -56.9(4) . . . . ? C22 C23 C24 C25 57.1(5) . . . . ? C23 C24 C25 C26 -56.3(5) . . . . ? C24 C25 C26 C21 54.2(5) . . . . ? C22 C21 C26 C25 -52.9(4) . . . . ? P2 C21 C26 C25 -179.8(3) . . . . ? C41 P2 C31 C32 177.0(3) . . . . ? C21 P2 C31 C32 59.4(3) . . . . ? Au P2 C31 C32 -67.3(3) . . . . ? C41 P2 C31 C36 -61.2(3) . . . . ? C21 P2 C31 C36 -178.7(3) . . . . ? Au P2 C31 C36 54.5(3) . . . . ? C36 C31 C32 C33 55.2(4) . . . . ? P2 C31 C32 C33 177.4(3) . . . . ? C31 C32 C33 C34 -56.9(5) . . . . ? C32 C33 C34 C35 56.4(5) . . . . ? C33 C34 C35 C36 -55.6(5) . . . . ? C34 C35 C36 C31 55.8(5) . . . . ? C32 C31 C36 C35 -55.0(4) . . . . ? P2 C31 C36 C35 -177.7(3) . . . . ? C31 P2 C41 C46 -57.3(3) . . . . ? C21 P2 C41 C46 60.2(3) . . . . ? Au P2 C41 C46 -174.4(2) . . . . ? C31 P2 C41 C42 173.9(3) . . . . ? C21 P2 C41 C42 -68.7(3) . . . . ? Au P2 C41 C42 56.8(3) . . . . ? C46 C41 C42 C43 56.6(4) . . . . ? P2 C41 C42 C43 -171.5(3) . . . . ? C41 C42 C43 C44 -54.5(4) . . . . ? C42 C43 C44 C45 54.6(5) . . . . ? C43 C44 C45 C46 -56.3(5) . . . . ? C42 C41 C46 C45 -58.0(4) . . . . ? P2 C41 C46 C45 173.2(3) . . . . ? C44 C45 C46 C41 57.6(4) . . . . ? C56 C51 C52 C53 3.0(11) . . . . ? C57 C51 C52 C53 179.9(8) . . . . ? C51 C52 C53 C54 -3.1(16) . . . . ? C52 C53 C54 C55 4.0(19) . . . . ? C53 C54 C55 C56 -4.0(14) . . . . ? C52 C51 C56 C55 -4.1(13) . . . . ? C57 C51 C56 C55 179.4(9) . . . . ? C54 C55 C56 C51 4.3(14) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.788 _refine_diff_density_min -3.677 _refine_diff_density_rms 0.186 #===END data_nickys9b _database_code_depnum_ccdc_archive 'CCDC 791412' #TrackingRef '- combined.cif' _audit_creation_method 'SHELXL-97 and CrysAlisPro RED' _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 9' _chemical_melting_point ? _chemical_formula_structural '[Au (tht) (tetrafluorophthalimide)].toluene' _chemical_formula_moiety 'C12 H8 Au F4 N O2 S, C7 H8' _chemical_formula_sum 'C19 H16 Au F4 N O2 S' _chemical_formula_weight 595.35 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, z+1/2' '-x, -y, -z' '-x, y-1/2, -z-1/2' _cell_length_a 11.8670(17) _cell_length_b 23.7634(14) _cell_length_c 6.6297(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.071(9) _cell_angle_gamma 90.00 _cell_volume 1869.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.115 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 8.034 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.827 _exptl_absorpt_correction_T_max 1.177 _exptl_absorpt_process_details ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_reflns_number 18667 _diffrn_reflns_av_R_equivalents 0.1194 _diffrn_reflns_av_sigmaI/netI 0.0793 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 22.50 _reflns_number_total 2437 _reflns_number_gt 1759 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlisPro CCD, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_cell_refinement ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_data_reduction ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Johnson, 1976 and Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0414P)^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 2437 _refine_ls_number_parameters 219 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0824 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.0991 _refine_ls_wR_factor_gt 0.0915 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.003 _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 Au Au 0.66002(6) 0.24548(2) 0.72062(11) 0.0455(2) Uani 1 1 d . . . S1 S 0.8226(4) 0.1956(2) 0.7210(11) 0.0760(18) Uani 1 1 d . . . C101 C 0.799(2) 0.1370(9) 0.533(3) 0.067(7) Uiso 1 1 d . . . H10A H 0.7633 0.1516 0.4120 0.081 Uiso 1 1 calc R . . H10B H 0.8700 0.1199 0.4961 0.081 Uiso 1 1 calc R . . C102 C 0.726(3) 0.0959(13) 0.631(5) 0.132(11) Uiso 1 1 d . . . H10C H 0.6487 0.1018 0.5870 0.159 Uiso 1 1 calc R . . H10D H 0.7483 0.0583 0.5906 0.159 Uiso 1 1 calc R . . C103 C 0.731(3) 0.1002(13) 0.830(6) 0.131(12) Uiso 1 1 d . . . H10E H 0.7515 0.0633 0.8813 0.157 Uiso 1 1 calc R . . H10F H 0.6555 0.1080 0.8771 0.157 Uiso 1 1 calc R . . C104 C 0.8057(19) 0.1407(10) 0.924(3) 0.069(7) Uani 1 1 d . . . H10G H 0.8775 0.1238 0.9594 0.083 Uiso 1 1 calc R . . H10H H 0.7720 0.1566 1.0449 0.083 Uiso 1 1 calc R . . N11 N 0.5138(9) 0.2894(5) 0.720(3) 0.037(3) Uani 1 1 d . . . C12 C 0.5043(12) 0.3473(6) 0.730(4) 0.038(4) Uani 1 1 d . . . O12 O 0.5760(8) 0.3814(4) 0.736(3) 0.046(3) Uani 1 1 d . . . C13 C 0.3786(11) 0.3580(5) 0.733(3) 0.036(4) Uani 1 1 d . . . C14 C 0.3189(14) 0.4077(6) 0.742(3) 0.048(5) Uani 1 1 d . . . C15 C 0.2013(16) 0.4040(7) 0.742(4) 0.057(5) Uiso 1 1 d . . . C16 C 0.1507(15) 0.3545(7) 0.727(5) 0.054(4) Uani 1 1 d . . . C17 C 0.2076(13) 0.3034(7) 0.719(5) 0.055(5) Uani 1 1 d . . . C18 C 0.3226(14) 0.3068(6) 0.720(3) 0.047(4) Uiso 1 1 d . . . C19 C 0.4126(12) 0.2620(6) 0.712(3) 0.043(4) Uani 1 1 d . . . O19 O 0.3981(9) 0.2123(4) 0.700(3) 0.067(4) Uani 1 1 d . . . F14 F 0.3686(8) 0.4577(3) 0.752(2) 0.059(3) Uani 1 1 d . . . F15 F 0.1414(8) 0.4510(4) 0.753(2) 0.078(3) Uani 1 1 d . . . F16 F 0.0352(8) 0.3516(4) 0.7344(19) 0.078(3) Uani 1 1 d . . . F17 F 0.1531(8) 0.2546(4) 0.708(2) 0.069(2) Uani 1 1 d . . . C91 C 0.7019(14) 0.5587(6) 0.754(5) 0.050(5) Uiso 1 1 d . . . C92 C 0.7531(16) 0.5065(7) 0.742(4) 0.067(6) Uani 1 1 d . . . H92 H 0.7087 0.4743 0.7386 0.080 Uiso 1 1 calc R . . C93 C 0.8695(14) 0.5013(7) 0.735(4) 0.062(5) Uani 1 1 d . . . H93 H 0.9022 0.4660 0.7205 0.075 Uiso 1 1 calc R . . C94 C 0.9349(14) 0.5474(7) 0.748(4) 0.058(5) Uani 1 1 d . . . H94 H 1.0128 0.5433 0.7477 0.070 Uiso 1 1 calc R . . C95 C 0.8906(12) 0.5991(6) 0.763(4) 0.038(5) Uani 1 1 d . . . H95 H 0.9371 0.6305 0.7719 0.045 Uiso 1 1 calc R . . C96 C 0.7740(14) 0.6052(6) 0.764(4) 0.043(5) Uiso 1 1 d . . . H96 H 0.7432 0.6411 0.7723 0.052 Uiso 1 1 calc R . . C97 C 0.5766(13) 0.5661(7) 0.749(4) 0.062(5) Uani 1 1 d . . . H97A H 0.5585 0.6051 0.7679 0.092 Uiso 1 1 calc R . . H97B H 0.5430 0.5442 0.8547 0.092 Uiso 1 1 calc R . . H97C H 0.5481 0.5537 0.6208 0.092 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au 0.0202(3) 0.0567(4) 0.0595(4) 0.0033(5) -0.0006(4) 0.0040(4) S1 0.021(3) 0.090(3) 0.117(6) 0.000(4) -0.002(4) 0.011(2) C104 0.042(16) 0.115(18) 0.051(14) -0.013(12) 0.010(11) 0.042(13) N11 0.016(7) 0.056(8) 0.039(9) -0.012(13) 0.003(10) -0.014(6) C12 0.024(10) 0.058(10) 0.032(11) 0.018(15) -0.011(13) -0.006(8) O12 0.027(7) 0.049(6) 0.062(9) 0.009(9) -0.004(10) -0.012(5) C13 0.010(8) 0.045(8) 0.053(12) 0.009(11) 0.006(9) 0.006(6) C14 0.045(12) 0.056(10) 0.043(12) 0.012(12) 0.010(13) 0.006(8) C16 0.017(9) 0.111(13) 0.036(9) 0.00(2) -0.003(14) 0.012(10) C17 0.024(10) 0.085(12) 0.057(13) 0.032(17) -0.008(14) -0.019(9) C19 0.025(9) 0.052(10) 0.054(11) 0.005(12) 0.015(9) -0.013(7) O19 0.047(8) 0.050(7) 0.104(13) 0.007(9) -0.003(9) -0.018(5) F14 0.059(7) 0.053(5) 0.066(8) 0.007(7) -0.011(9) 0.010(4) F15 0.059(7) 0.096(6) 0.079(8) 0.009(8) 0.015(11) 0.055(5) F16 0.023(6) 0.148(9) 0.063(8) 0.005(9) 0.013(8) 0.013(5) F17 0.028(4) 0.097(6) 0.081(6) 0.004(11) 0.003(6) -0.023(6) C92 0.053(12) 0.085(12) 0.062(16) 0.001(17) -0.007(16) -0.026(10) C93 0.045(13) 0.065(10) 0.077(16) -0.003(13) 0.012(16) 0.013(9) C94 0.041(11) 0.065(11) 0.070(16) 0.005(17) 0.002(15) -0.006(9) C95 0.018(8) 0.056(9) 0.039(13) 0.001(12) 0.004(11) -0.002(7) C97 0.033(12) 0.105(13) 0.046(15) 0.004(16) -0.007(13) -0.017(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Au N11 2.025(12) . ? Au S1 2.264(4) . ? Au Au 3.3218(3) 2 ? Au Au 3.3218(3) 2_554 ? S1 C104 1.89(2) . ? S1 C101 1.89(2) . ? C101 C102 1.46(4) . ? C101 H10A 0.9700 . ? C101 H10B 0.9700 . ? C102 C103 1.32(3) . ? C102 H10C 0.9700 . ? C102 H10D 0.9700 . ? C103 C104 1.45(4) . ? C103 H10E 0.9700 . ? C103 H10F 0.9700 . ? C104 H10G 0.9700 . ? C104 H10H 0.9700 . ? N11 C19 1.367(16) . ? N11 C12 1.381(17) . ? C12 O12 1.175(15) . ? C12 C13 1.513(18) . ? C13 C14 1.378(18) . ? C13 C18 1.389(18) . ? C14 F14 1.328(17) . ? C14 C15 1.398(19) . ? C15 C16 1.32(2) . ? C15 F15 1.327(18) . ? C16 F16 1.373(19) . ? C16 C17 1.39(2) . ? C17 F17 1.329(16) . ? C17 C18 1.367(19) . ? C18 C19 1.509(19) . ? C19 O19 1.196(15) . ? C91 C92 1.38(2) . ? C91 C96 1.400(19) . ? C91 C97 1.50(2) . ? C92 C93 1.39(2) . ? C92 H92 0.9300 . ? C93 C94 1.35(2) . ? C93 H93 0.9300 . ? C94 C95 1.339(19) . ? C94 H94 0.9300 . ? C95 C96 1.391(18) . ? C95 H95 0.9300 . ? C96 H96 0.9300 . ? C97 H97A 0.9600 . ? C97 H97B 0.9600 . ? C97 H97C 0.9600 . ? 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 N11 Au S1 179.5(3) . . ? N11 Au Au 88.1(6) . 2 ? S1 Au Au 91.94(19) . 2 ? N11 Au Au 88.1(6) . 2_554 ? S1 Au Au 91.94(19) . 2_554 ? Au Au Au 172.58(4) 2 2_554 ? C104 S1 C101 86.9(7) . . ? C104 S1 Au 105.7(7) . . ? C101 S1 Au 105.0(8) . . ? C102 C101 S1 106.8(19) . . ? C102 C101 H10A 110.4 . . ? S1 C101 H10A 110.4 . . ? C102 C101 H10B 110.4 . . ? S1 C101 H10B 110.4 . . ? H10A C101 H10B 108.6 . . ? C103 C102 C101 111(3) . . ? C103 C102 H10C 109.4 . . ? C101 C102 H10C 109.4 . . ? C103 C102 H10D 109.4 . . ? C101 C102 H10D 109.4 . . ? H10C C102 H10D 108.0 . . ? C102 C103 C104 121(3) . . ? C102 C103 H10E 107.1 . . ? C104 C103 H10E 107.1 . . ? C102 C103 H10F 107.1 . . ? C104 C103 H10F 107.1 . . ? H10E C103 H10F 106.8 . . ? C103 C104 S1 102.4(19) . . ? C103 C104 H10G 111.3 . . ? S1 C104 H10G 111.3 . . ? C103 C104 H10H 111.3 . . ? S1 C104 H10H 111.3 . . ? H10G C104 H10H 109.2 . . ? C19 N11 C12 113.9(12) . . ? C19 N11 Au 120.4(10) . . ? C12 N11 Au 125.7(9) . . ? O12 C12 N11 128.9(14) . . ? O12 C12 C13 126.7(14) . . ? N11 C12 C13 104.4(12) . . ? C14 C13 C18 120.4(14) . . ? C14 C13 C12 130.7(14) . . ? C18 C13 C12 108.9(12) . . ? F14 C14 C13 122.7(14) . . ? F14 C14 C15 119.9(13) . . ? C13 C14 C15 117.4(15) . . ? C16 C15 F15 120.6(17) . . ? C16 C15 C14 120.6(17) . . ? F15 C15 C14 118.8(14) . . ? C15 C16 F16 119.7(16) . . ? C15 C16 C17 123.9(18) . . ? F16 C16 C17 116.2(14) . . ? F17 C17 C18 122.5(16) . . ? F17 C17 C16 121.8(15) . . ? C18 C17 C16 115.7(15) . . ? C17 C18 C13 122.0(14) . . ? C17 C18 C19 131.7(14) . . ? C13 C18 C19 106.4(13) . . ? O19 C19 N11 126.9(14) . . ? O19 C19 C18 126.6(14) . . ? N11 C19 C18 106.5(12) . . ? C92 C91 C96 116.2(15) . . ? C92 C91 C97 122.7(14) . . ? C96 C91 C97 121.0(14) . . ? C91 C92 C93 121.3(16) . . ? C91 C92 H92 119.3 . . ? C93 C92 H92 119.3 . . ? C94 C93 C92 120.0(17) . . ? C94 C93 H93 120.0 . . ? C92 C93 H93 120.0 . . ? C95 C94 C93 121.7(17) . . ? C95 C94 H94 119.2 . . ? C93 C94 H94 119.2 . . ? C94 C95 C96 119.1(15) . . ? C94 C95 H95 120.5 . . ? C96 C95 H95 120.5 . . ? C95 C96 C91 121.7(15) . . ? C95 C96 H96 119.1 . . ? C91 C96 H96 119.1 . . ? C91 C97 H97A 109.5 . . ? C91 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? C91 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N11 Au S1 C104 -45(68) . . . . ? Au Au S1 C104 45.2(8) 2 . . . ? Au Au S1 C104 -141.1(8) 2_554 . . . ? N11 Au S1 C101 46(68) . . . . ? Au Au S1 C101 136.2(7) 2 . . . ? Au Au S1 C101 -50.1(7) 2_554 . . . ? C104 S1 C101 C102 29.9(18) . . . . ? Au S1 C101 C102 -75.6(19) . . . . ? S1 C101 C102 C103 -22(4) . . . . ? C101 C102 C103 C104 -2(6) . . . . ? C102 C103 C104 S1 25(4) . . . . ? C101 S1 C104 C103 -28.9(17) . . . . ? Au S1 C104 C103 75.8(17) . . . . ? S1 Au N11 C19 -5(69) . . . . ? Au Au N11 C19 -95.7(16) 2 . . . ? Au Au N11 C19 90.7(16) 2_554 . . . ? S1 Au N11 C12 174(100) . . . . ? Au Au N11 C12 84(2) 2 . . . ? Au Au N11 C12 -90(2) 2_554 . . . ? C19 N11 C12 O12 -179(3) . . . . ? Au N11 C12 O12 1(5) . . . . ? C19 N11 C12 C13 1(3) . . . . ? Au N11 C12 C13 -177.9(14) . . . . ? O12 C12 C13 C14 1(5) . . . . ? N11 C12 C13 C14 -180(2) . . . . ? O12 C12 C13 C18 179(3) . . . . ? N11 C12 C13 C18 -2(3) . . . . ? C18 C13 C14 F14 -178.9(18) . . . . ? C12 C13 C14 F14 -1(4) . . . . ? C18 C13 C14 C15 1(3) . . . . ? C12 C13 C14 C15 180(2) . . . . ? F14 C14 C15 C16 178(2) . . . . ? C13 C14 C15 C16 -2(4) . . . . ? F14 C14 C15 F15 -1(4) . . . . ? C13 C14 C15 F15 179.1(19) . . . . ? F15 C15 C16 F16 -4(4) . . . . ? C14 C15 C16 F16 178(2) . . . . ? F15 C15 C16 C17 -179(3) . . . . ? C14 C15 C16 C17 3(5) . . . . ? C15 C16 C17 F17 179(3) . . . . ? F16 C16 C17 F17 4(5) . . . . ? C15 C16 C17 C18 -2(5) . . . . ? F16 C16 C17 C18 -178(2) . . . . ? F17 C17 C18 C13 -180(2) . . . . ? C16 C17 C18 C13 2(4) . . . . ? F17 C17 C18 C19 -1(5) . . . . ? C16 C17 C18 C19 -180(3) . . . . ? C14 C13 C18 C17 -1(3) . . . . ? C12 C13 C18 C17 -180(3) . . . . ? C14 C13 C18 C19 179.7(18) . . . . ? C12 C13 C18 C19 1(2) . . . . ? C12 N11 C19 O19 179(3) . . . . ? Au N11 C19 O19 -2(3) . . . . ? C12 N11 C19 C18 -1(3) . . . . ? Au N11 C19 C18 178.6(12) . . . . ? C17 C18 C19 O19 1(4) . . . . ? C13 C18 C19 O19 -180(2) . . . . ? C17 C18 C19 N11 -179(2) . . . . ? C13 C18 C19 N11 0(2) . . . . ? C96 C91 C92 C93 -2(5) . . . . ? C97 C91 C92 C93 176(3) . . . . ? C91 C92 C93 C94 3(5) . . . . ? C92 C93 C94 C95 -2(5) . . . . ? C93 C94 C95 C96 0(4) . . . . ? C94 C95 C96 C91 1(4) . . . . ? C92 C91 C96 C95 0(4) . . . . ? C97 C91 C96 C95 -178(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.590 _refine_diff_density_min -1.089 _refine_diff_density_rms 0.173 #===END #791413 data_nickys4 _database_code_depnum_ccdc_archive 'CCDC 791413' #TrackingRef '- combined_revised.cif' _audit_creation_method 'SHELXL-97 and CrysAlisPro RED' _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 10' _chemical_melting_point ? _chemical_formula_structural '[Au(F4-phthalimide)2-Ag(CNMe)2].MeCN' _chemical_formula_moiety 'C20 H6 Ag Au F8 N4 O4, C2 H3 N' _chemical_formula_sum 'C22 H9 Ag Au F8 N5 O4' _chemical_formula_weight 864.18 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' Ag Ag -0.8971 1.1015 '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' F F 0.0171 0.0103 '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' _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 8.24928(9) _cell_length_b 9.49150(15) _cell_length_c 16.8812(3) _cell_angle_alpha 94.1577(13) _cell_angle_beta 94.4125(11) _cell_angle_gamma 111.3597(12) _cell_volume 1220.12(3) _cell_formula_units_Z 2 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used 26250 _cell_measurement_theta_min 3.3964 _cell_measurement_theta_max 32.4749 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 6.911 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.676 _exptl_absorpt_correction_T_max 1.278 _exptl_absorpt_process_details ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_reflns_number 34701 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 30.00 _reflns_number_total 7115 _reflns_number_gt 6535 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlisPro CCD, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_cell_refinement ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_data_reduction ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Johnson, 1971 and Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The non-hydrogen atoms were refined with anisotropic thermal parameters. Hydrogen atoms were included in idealised positions and their Uiso values were set to ride on the Ueq values of the parent carbon atoms. However, difference peaks indicated that one NCMe ligand was disordered over two distinct positions; six half-occupancy atoms were then included in the refinement with restrained C-H and H...H distances. ; _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^+0.0535P] 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 7115 _refine_ls_number_parameters 390 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0211 _refine_ls_R_factor_gt 0.0174 _refine_ls_wR_factor_ref 0.0418 _refine_ls_wR_factor_gt 0.0411 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.058 _refine_ls_shift/su_mean 0.002 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 Au Au 0.414860(10) 0.491064(9) 0.646836(5) 0.01725(3) Uani 1 1 d . . . Ag Ag 0.65298(2) 0.81385(2) 0.664045(10) 0.02398(4) Uani 1 1 d . . . N1 N 0.3125(2) 0.5206(2) 0.54115(10) 0.0178(3) Uani 1 1 d . . . C2 C 0.3729(3) 0.6521(2) 0.50515(13) 0.0184(4) Uani 1 1 d . . . O2 O 0.4975(2) 0.76794(19) 0.53036(10) 0.0266(4) Uani 1 1 d . . . C3 C 0.2567(3) 0.6300(2) 0.42893(13) 0.0180(4) Uani 1 1 d . . . C4 C 0.2568(3) 0.7228(3) 0.37103(14) 0.0229(4) Uani 1 1 d . . . F4 F 0.37363(18) 0.86534(17) 0.37462(9) 0.0355(4) Uani 1 1 d . . . C5 C 0.1306(3) 0.6669(3) 0.30485(14) 0.0240(5) Uani 1 1 d . . . F5 F 0.1319(2) 0.75400(19) 0.24608(10) 0.0390(4) Uani 1 1 d . . . C6 C 0.0070(3) 0.5220(3) 0.29913(13) 0.0228(5) Uani 1 1 d . . . F6 F -0.11067(19) 0.46950(17) 0.23427(8) 0.0322(3) Uani 1 1 d . . . C7 C 0.0055(3) 0.4287(2) 0.35866(13) 0.0203(4) Uani 1 1 d . . . F7 F -0.11858(18) 0.28876(15) 0.35096(9) 0.0292(3) Uani 1 1 d . . . C8 C 0.1315(3) 0.4826(2) 0.42342(12) 0.0175(4) Uani 1 1 d . . . C9 C 0.1650(3) 0.4125(2) 0.49647(12) 0.0171(4) Uani 1 1 d . . . O9 O 0.0806(2) 0.28906(17) 0.51499(10) 0.0243(3) Uani 1 1 d . . . N11 N 0.5124(2) 0.4660(2) 0.75496(11) 0.0190(4) Uani 1 1 d . . . C12 C 0.4213(3) 0.3582(2) 0.80261(13) 0.0190(4) Uani 1 1 d . . . O12 O 0.2805(2) 0.25692(18) 0.78320(10) 0.0284(4) Uani 1 1 d . . . C13 C 0.5303(3) 0.3898(2) 0.88193(13) 0.0180(4) Uani 1 1 d . . . C14 C 0.5023(3) 0.3243(2) 0.95183(13) 0.0201(4) Uani 1 1 d . . . F14 F 0.35508(18) 0.20827(15) 0.96058(8) 0.0276(3) Uani 1 1 d . . . C15 C 0.6296(3) 0.3833(2) 1.01700(13) 0.0222(4) Uani 1 1 d . . . F15 F 0.6044(2) 0.32317(16) 1.08610(8) 0.0304(3) Uani 1 1 d . . . C16 C 0.7806(3) 0.5058(3) 1.01157(13) 0.0225(4) Uani 1 1 d . . . F16 F 0.9008(2) 0.56240(17) 1.07548(8) 0.0332(3) Uani 1 1 d . . . C17 C 0.8093(3) 0.5735(2) 0.94082(14) 0.0211(4) Uani 1 1 d . . . F17 F 0.95710(18) 0.69316(16) 0.93859(9) 0.0312(3) Uani 1 1 d . . . C18 C 0.6834(3) 0.5143(2) 0.87652(12) 0.0177(4) Uani 1 1 d . . . C19 C 0.6699(3) 0.5643(2) 0.79491(12) 0.0173(4) Uani 1 1 d . . . O19 O 0.7770(2) 0.67233(17) 0.76928(9) 0.0224(3) Uani 1 1 d . . . N21 N 0.4878(3) 0.8663(2) 0.74938(13) 0.0280(4) Uani 1 1 d . . . C22 C 0.3882(3) 0.8852(2) 0.78643(14) 0.0227(4) Uani 1 1 d . . . C23 C 0.2580(3) 0.9100(3) 0.83333(15) 0.0288(5) Uani 1 1 d . . . H23A H 0.2406 1.0003 0.8197 0.043 Uiso 1 1 calc R . . H23B H 0.2983 0.9218 0.8892 0.043 Uiso 1 1 calc R . . H23C H 0.1494 0.8243 0.8220 0.043 Uiso 1 1 calc R . . N31 N 0.9179(2) 0.9478(2) 0.63703(13) 0.0300(5) Uani 1 1 d . . . C32 C 1.0514(3) 0.9920(3) 0.61586(14) 0.0249(5) Uani 1 1 d . . . C33 C 1.2254(3) 1.0467(3) 0.58864(18) 0.0329(6) Uani 1 1 d D . . N41 N 0.6842(3) 0.0995(3) 0.94332(16) 0.0415(6) Uani 1 1 d . . . C42 C 0.7877(3) 0.0676(3) 0.91469(15) 0.0267(5) Uani 1 1 d . . . C43 C 0.9218(3) 0.0272(3) 0.87867(17) 0.0331(6) Uani 1 1 d . . . H43A H 0.9895 -0.0006 0.9190 0.050 Uiso 1 1 calc R . . H43B H 0.9971 0.1128 0.8551 0.050 Uiso 1 1 calc R . . H43C H 0.8670 -0.0571 0.8382 0.050 Uiso 1 1 calc R . . H33A H 1.305(6) 1.125(6) 0.628(3) 0.050 Uiso 0.50 1 d PD . . H33B H 1.209(7) 1.090(8) 0.540(2) 0.050 Uiso 0.50 1 d PD . . H33C H 1.271(7) 0.969(4) 0.578(4) 0.050 Uiso 0.50 1 d PD . . H33D H 1.209(7) 0.990(6) 0.537(2) 0.050 Uiso 0.50 1 d PD . . H33E H 1.300(6) 1.019(7) 0.625(3) 0.050 Uiso 0.50 1 d PD . . H33F H 1.275(7) 1.1540(18) 0.583(4) 0.050 Uiso 0.50 1 d PD . . 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 Au 0.01970(4) 0.01800(4) 0.01329(4) 0.00249(3) 0.00107(3) 0.00613(3) Ag 0.02000(8) 0.02640(9) 0.02261(9) 0.00448(7) 0.00471(6) 0.00437(7) N1 0.0178(8) 0.0185(8) 0.0159(9) 0.0017(6) 0.0001(7) 0.0058(7) C2 0.0165(9) 0.0229(10) 0.0161(10) 0.0037(8) 0.0035(8) 0.0070(8) O2 0.0216(8) 0.0258(8) 0.0239(9) 0.0070(6) -0.0014(6) -0.0013(6) C3 0.0172(9) 0.0210(10) 0.0162(10) 0.0034(8) 0.0029(8) 0.0071(8) C4 0.0188(10) 0.0235(11) 0.0263(12) 0.0088(9) 0.0036(9) 0.0062(9) F4 0.0262(7) 0.0302(8) 0.0419(9) 0.0208(7) -0.0027(6) -0.0010(6) C5 0.0255(11) 0.0312(12) 0.0206(11) 0.0134(9) 0.0042(9) 0.0145(10) F5 0.0395(8) 0.0449(9) 0.0320(9) 0.0236(7) -0.0023(7) 0.0128(7) C6 0.0236(11) 0.0302(12) 0.0165(10) 0.0006(8) -0.0035(8) 0.0137(9) F6 0.0365(8) 0.0367(8) 0.0214(7) 0.0012(6) -0.0119(6) 0.0146(7) C7 0.0219(10) 0.0184(10) 0.0200(11) -0.0010(8) -0.0020(8) 0.0081(8) F7 0.0303(7) 0.0180(6) 0.0314(8) -0.0004(5) -0.0119(6) 0.0034(6) C8 0.0184(9) 0.0199(10) 0.0158(10) 0.0018(7) 0.0016(8) 0.0092(8) C9 0.0189(9) 0.0180(9) 0.0152(10) 0.0013(7) 0.0015(7) 0.0080(8) O9 0.0290(8) 0.0172(7) 0.0237(8) 0.0035(6) -0.0011(7) 0.0055(6) N11 0.0219(9) 0.0193(9) 0.0148(9) 0.0033(6) 0.0009(7) 0.0065(7) C12 0.0236(10) 0.0171(9) 0.0168(10) 0.0030(7) 0.0012(8) 0.0082(8) O12 0.0279(8) 0.0232(8) 0.0260(9) 0.0061(7) -0.0019(7) 0.0004(7) C13 0.0232(10) 0.0169(9) 0.0157(10) 0.0029(7) 0.0022(8) 0.0093(8) C14 0.0254(11) 0.0169(10) 0.0204(11) 0.0052(8) 0.0048(8) 0.0097(8) F14 0.0332(7) 0.0217(6) 0.0254(7) 0.0089(5) 0.0068(6) 0.0053(6) C15 0.0358(12) 0.0237(10) 0.0147(10) 0.0067(8) 0.0044(9) 0.0190(10) F15 0.0459(8) 0.0321(8) 0.0185(7) 0.0111(6) 0.0034(6) 0.0191(7) C16 0.0272(11) 0.0246(11) 0.0178(11) 0.0004(8) -0.0045(8) 0.0138(9) F16 0.0376(8) 0.0398(8) 0.0205(7) 0.0028(6) -0.0099(6) 0.0152(7) C17 0.0210(10) 0.0206(10) 0.0218(11) 0.0025(8) -0.0004(8) 0.0084(8) F17 0.0240(7) 0.0309(7) 0.0293(8) 0.0064(6) -0.0053(6) 0.0003(6) C18 0.0219(10) 0.0175(9) 0.0152(10) 0.0035(7) 0.0017(8) 0.0090(8) C19 0.0212(10) 0.0174(9) 0.0152(10) 0.0020(7) 0.0022(8) 0.0094(8) O19 0.0219(8) 0.0222(8) 0.0221(8) 0.0067(6) 0.0039(6) 0.0058(6) N21 0.0257(10) 0.0299(11) 0.0258(11) -0.0001(8) 0.0072(8) 0.0069(8) C22 0.0275(11) 0.0183(10) 0.0202(11) 0.0030(8) 0.0018(9) 0.0060(9) C23 0.0334(13) 0.0252(11) 0.0311(13) 0.0034(10) 0.0112(10) 0.0132(10) N31 0.0224(10) 0.0291(10) 0.0346(12) 0.0042(9) 0.0055(9) 0.0045(8) C32 0.0236(11) 0.0225(11) 0.0272(12) 0.0055(9) 0.0010(9) 0.0068(9) C33 0.0213(11) 0.0308(13) 0.0480(17) 0.0156(11) 0.0122(11) 0.0075(10) N41 0.0399(13) 0.0353(13) 0.0510(16) 0.0004(11) 0.0109(11) 0.0156(11) C42 0.0295(12) 0.0206(11) 0.0286(13) 0.0001(9) 0.0001(10) 0.0089(9) C43 0.0350(13) 0.0339(13) 0.0359(15) 0.0042(11) 0.0067(11) 0.0188(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 Au N1 1.9972(17) . ? Au N11 2.0030(17) . ? Au Ag 2.95442(19) . ? Ag N31 2.194(2) . ? Ag N21 2.207(2) . ? Ag O2 2.4358(16) . ? Ag O19 2.6598(15) . ? N1 C2 1.371(3) . ? N1 C9 1.393(3) . ? C2 O2 1.219(3) . ? C2 C3 1.498(3) . ? C3 C4 1.362(3) . ? C3 C8 1.395(3) . ? C4 F4 1.339(3) . ? C4 C5 1.395(3) . ? C5 F5 1.335(2) . ? C5 C6 1.372(3) . ? C6 F6 1.339(2) . ? C6 C7 1.385(3) . ? C7 F7 1.339(3) . ? C7 C8 1.376(3) . ? C8 C9 1.497(3) . ? C9 O9 1.203(3) . ? N11 C19 1.380(3) . ? N11 C12 1.382(3) . ? C12 O12 1.210(3) . ? C12 C13 1.500(3) . ? C13 C14 1.370(3) . ? C13 C18 1.395(3) . ? C14 F14 1.336(2) . ? C14 C15 1.390(3) . ? C15 F15 1.333(2) . ? C15 C16 1.375(3) . ? C16 F16 1.341(2) . ? C16 C17 1.393(3) . ? C17 F17 1.335(3) . ? C17 C18 1.373(3) . ? C18 C19 1.498(3) . ? C19 O19 1.218(3) . ? N21 C22 1.126(3) . ? C22 C23 1.457(3) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? N31 C32 1.124(3) . ? C32 C33 1.461(3) . ? C33 H33A 0.960(10) . ? C33 H33B 0.961(10) . ? C33 H33C 0.956(10) . ? C33 H33D 0.961(10) . ? C33 H33E 0.952(10) . ? C33 H33F 0.964(10) . ? N41 C42 1.134(3) . ? C42 C43 1.455(4) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? 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 N1 Au N11 177.73(7) . . ? N1 Au Ag 88.99(5) . . ? N11 Au Ag 90.40(5) . . ? N31 Ag N21 130.95(8) . . ? N31 Ag O2 99.25(7) . . ? N21 Ag O2 108.11(7) . . ? N31 Ag O19 91.55(7) . . ? N21 Ag O19 92.02(7) . . ? O2 Ag O19 140.68(5) . . ? N31 Ag Au 137.80(6) . . ? N21 Ag Au 89.24(5) . . ? O2 Ag Au 74.80(4) . . ? O19 Ag Au 72.00(3) . . ? C2 N1 C9 111.36(17) . . ? C2 N1 Au 124.47(14) . . ? C9 N1 Au 124.11(14) . . ? O2 C2 N1 126.76(19) . . ? O2 C2 C3 125.4(2) . . ? N1 C2 C3 107.79(17) . . ? C2 O2 Ag 124.14(14) . . ? C4 C3 C8 121.1(2) . . ? C4 C3 C2 132.3(2) . . ? C8 C3 C2 106.56(18) . . ? F4 C4 C3 122.8(2) . . ? F4 C4 C5 118.5(2) . . ? C3 C4 C5 118.7(2) . . ? F5 C5 C6 119.8(2) . . ? F5 C5 C4 119.7(2) . . ? C6 C5 C4 120.5(2) . . ? F6 C6 C5 119.5(2) . . ? F6 C6 C7 119.8(2) . . ? C5 C6 C7 120.7(2) . . ? F7 C7 C8 122.3(2) . . ? F7 C7 C6 118.69(19) . . ? C8 C7 C6 119.0(2) . . ? C7 C8 C3 120.0(2) . . ? C7 C8 C9 132.0(2) . . ? C3 C8 C9 107.92(17) . . ? O9 C9 N1 125.92(19) . . ? O9 C9 C8 127.71(19) . . ? N1 C9 C8 106.35(17) . . ? C19 N11 C12 111.35(17) . . ? C19 N11 Au 124.29(14) . . ? C12 N11 Au 123.98(14) . . ? O12 C12 N11 125.95(19) . . ? O12 C12 C13 126.8(2) . . ? N11 C12 C13 107.28(17) . . ? C14 C13 C18 120.52(19) . . ? C14 C13 C12 132.6(2) . . ? C18 C13 C12 106.83(18) . . ? F14 C14 C13 122.59(19) . . ? F14 C14 C15 118.6(2) . . ? C13 C14 C15 118.8(2) . . ? F15 C15 C16 119.3(2) . . ? F15 C15 C14 120.0(2) . . ? C16 C15 C14 120.6(2) . . ? F16 C16 C15 119.7(2) . . ? F16 C16 C17 119.5(2) . . ? C15 C16 C17 120.8(2) . . ? F17 C17 C18 123.0(2) . . ? F17 C17 C16 118.71(19) . . ? C18 C17 C16 118.3(2) . . ? C17 C18 C13 120.9(2) . . ? C17 C18 C19 131.4(2) . . ? C13 C18 C19 107.54(18) . . ? O19 C19 N11 126.69(19) . . ? O19 C19 C18 126.33(19) . . ? N11 C19 C18 106.98(18) . . ? C19 O19 Ag 116.67(13) . . ? C22 N21 Ag 172.22(19) . . ? N21 C22 C23 179.2(3) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C32 N31 Ag 167.3(2) . . ? N31 C32 C33 178.9(3) . . ? C32 C33 H33A 109(3) . . ? C32 C33 H33B 104(3) . . ? H33A C33 H33B 109.4(15) . . ? C32 C33 H33C 114(3) . . ? H33A C33 H33C 110.0(15) . . ? H33B C33 H33C 110.0(15) . . ? C32 C33 H33D 104(3) . . ? H33A C33 H33D 147(5) . . ? H33B C33 H33D 59(3) . . ? H33C C33 H33D 56(3) . . ? C32 C33 H33E 107(3) . . ? H33A C33 H33E 62(3) . . ? H33B C33 H33E 149(5) . . ? H33C C33 H33E 54(3) . . ? H33D C33 H33E 110.3(15) . . ? C32 C33 H33F 116(3) . . ? H33A C33 H33F 53(3) . . ? H33B C33 H33F 56(3) . . ? H33C C33 H33F 130(5) . . ? H33D C33 H33F 108.8(15) . . ? H33E C33 H33F 110.3(15) . . ? N41 C42 C43 179.4(3) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Au Ag N31 -92.34(10) . . . . ? N11 Au Ag N31 89.85(10) . . . . ? N1 Au Ag N21 103.71(8) . . . . ? N11 Au Ag N21 -74.10(8) . . . . ? N1 Au Ag O2 -5.30(7) . . . . ? N11 Au Ag O2 176.89(7) . . . . ? N1 Au Ag O19 -163.92(6) . . . . ? N11 Au Ag O19 18.27(7) . . . . ? N11 Au N1 C2 79.3(18) . . . . ? Ag Au N1 C2 4.81(17) . . . . ? N11 Au N1 C9 -97.5(17) . . . . ? Ag Au N1 C9 -171.93(16) . . . . ? C9 N1 C2 O2 178.6(2) . . . . ? Au N1 C2 O2 1.5(3) . . . . ? C9 N1 C2 C3 -0.6(2) . . . . ? Au N1 C2 C3 -177.67(14) . . . . ? N1 C2 O2 Ag -9.5(3) . . . . ? C3 C2 O2 Ag 169.52(15) . . . . ? N31 Ag O2 C2 146.28(18) . . . . ? N21 Ag O2 C2 -74.97(19) . . . . ? O19 Ag O2 C2 42.3(2) . . . . ? Au Ag O2 C2 9.10(17) . . . . ? O2 C2 C3 C4 0.6(4) . . . . ? N1 C2 C3 C4 179.8(2) . . . . ? O2 C2 C3 C8 -179.7(2) . . . . ? N1 C2 C3 C8 -0.5(2) . . . . ? C8 C3 C4 F4 179.3(2) . . . . ? C2 C3 C4 F4 -1.0(4) . . . . ? C8 C3 C4 C5 -1.1(4) . . . . ? C2 C3 C4 C5 178.6(2) . . . . ? F4 C4 C5 F5 1.9(4) . . . . ? C3 C4 C5 F5 -177.8(2) . . . . ? F4 C4 C5 C6 -179.2(2) . . . . ? C3 C4 C5 C6 1.1(4) . . . . ? F5 C5 C6 F6 0.3(3) . . . . ? C4 C5 C6 F6 -178.6(2) . . . . ? F5 C5 C6 C7 178.7(2) . . . . ? C4 C5 C6 C7 -0.2(4) . . . . ? F6 C6 C7 F7 -2.3(3) . . . . ? C5 C6 C7 F7 179.4(2) . . . . ? F6 C6 C7 C8 177.5(2) . . . . ? C5 C6 C7 C8 -0.8(4) . . . . ? F7 C7 C8 C3 -179.3(2) . . . . ? C6 C7 C8 C3 0.9(3) . . . . ? F7 C7 C8 C9 -0.6(4) . . . . ? C6 C7 C8 C9 179.6(2) . . . . ? C4 C3 C8 C7 0.0(3) . . . . ? C2 C3 C8 C7 -179.7(2) . . . . ? C4 C3 C8 C9 -179.0(2) . . . . ? C2 C3 C8 C9 1.3(2) . . . . ? C2 N1 C9 O9 -177.0(2) . . . . ? Au N1 C9 O9 0.1(3) . . . . ? C2 N1 C9 C8 1.3(2) . . . . ? Au N1 C9 C8 178.46(13) . . . . ? C7 C8 C9 O9 -2.2(4) . . . . ? C3 C8 C9 O9 176.7(2) . . . . ? C7 C8 C9 N1 179.5(2) . . . . ? C3 C8 C9 N1 -1.6(2) . . . . ? N1 Au N11 C19 -92.4(17) . . . . ? Ag Au N11 C19 -17.94(17) . . . . ? N1 Au N11 C12 79.9(18) . . . . ? Ag Au N11 C12 154.31(17) . . . . ? C19 N11 C12 O12 -179.2(2) . . . . ? Au N11 C12 O12 7.6(3) . . . . ? C19 N11 C12 C13 0.2(2) . . . . ? Au N11 C12 C13 -172.91(14) . . . . ? O12 C12 C13 C14 -3.6(4) . . . . ? N11 C12 C13 C14 176.9(2) . . . . ? O12 C12 C13 C18 178.4(2) . . . . ? N11 C12 C13 C18 -1.1(2) . . . . ? C18 C13 C14 F14 177.7(2) . . . . ? C12 C13 C14 F14 -0.1(4) . . . . ? C18 C13 C14 C15 -0.5(3) . . . . ? C12 C13 C14 C15 -178.3(2) . . . . ? F14 C14 C15 F15 0.7(3) . . . . ? C13 C14 C15 F15 178.98(19) . . . . ? F14 C14 C15 C16 -177.9(2) . . . . ? C13 C14 C15 C16 0.4(3) . . . . ? F15 C15 C16 F16 0.4(3) . . . . ? C14 C15 C16 F16 179.1(2) . . . . ? F15 C15 C16 C17 -178.5(2) . . . . ? C14 C15 C16 C17 0.1(3) . . . . ? F16 C16 C17 F17 0.4(3) . . . . ? C15 C16 C17 F17 179.3(2) . . . . ? F16 C16 C17 C18 -179.4(2) . . . . ? C15 C16 C17 C18 -0.4(3) . . . . ? F17 C17 C18 C13 -179.5(2) . . . . ? C16 C17 C18 C13 0.3(3) . . . . ? F17 C17 C18 C19 -3.3(4) . . . . ? C16 C17 C18 C19 176.5(2) . . . . ? C14 C13 C18 C17 0.2(3) . . . . ? C12 C13 C18 C17 178.5(2) . . . . ? C14 C13 C18 C19 -176.82(19) . . . . ? C12 C13 C18 C19 1.4(2) . . . . ? C12 N11 C19 O19 -178.5(2) . . . . ? Au N11 C19 O19 -5.4(3) . . . . ? C12 N11 C19 C18 0.7(2) . . . . ? Au N11 C19 C18 173.77(13) . . . . ? C17 C18 C19 O19 1.3(4) . . . . ? C13 C18 C19 O19 177.9(2) . . . . ? C17 C18 C19 N11 -177.9(2) . . . . ? C13 C18 C19 N11 -1.3(2) . . . . ? N11 C19 O19 Ag 30.7(3) . . . . ? C18 C19 O19 Ag -148.33(17) . . . . ? N31 Ag O19 C19 -170.18(16) . . . . ? N21 Ag O19 C19 58.75(16) . . . . ? O2 Ag O19 C19 -63.51(18) . . . . ? Au Ag O19 C19 -29.79(14) . . . . ? N31 Ag N21 C22 141.0(15) . . . . ? O2 Ag N21 C22 20.5(15) . . . . ? O19 Ag N21 C22 -125.2(15) . . . . ? Au Ag N21 C22 -53.2(15) . . . . ? Ag N21 C22 C23 -38(19) . . . . ? N21 Ag N31 C32 168.3(9) . . . . ? O2 Ag N31 C32 -67.8(9) . . . . ? O19 Ag N31 C32 74.2(9) . . . . ? Au Ag N31 C32 9.7(10) . . . . ? Ag N31 C32 C33 -40(15) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.863 _refine_diff_density_min -0.911 _refine_diff_density_rms 0.090 #===END #791414 data_2009src1339r _database_code_depnum_ccdc_archive 'CCDC 791414' #TrackingRef 'combined-edit-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 11' _chemical_melting_point ? _chemical_formula_moiety 'C36 H30 Au P2, C44 B2 F34 N O2, ca 1.5(C4 H8 O)' _chemical_formula_sum 'C86 H42 Au B2 F34 N O3.50 P2' _chemical_formula_weight 2071.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' B B 0.0013 0.0007 '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 P21/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 15.4133(11) _cell_length_b 32.505(2) _cell_length_c 16.4236(12) _cell_angle_alpha 90.00 _cell_angle_beta 89.997(2) _cell_angle_gamma 90.00 _cell_volume 8228.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.672 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4072 _exptl_absorpt_coefficient_mu 1.956 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.651 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius Roper CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37322 _diffrn_reflns_av_R_equivalents 0.0751 _diffrn_reflns_av_sigmaI/netI 0.0745 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 22.50 _reflns_number_total 10292 _reflns_number_gt 8628 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' # Although determined using DirAx, the cell is refined in the HKL # package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Johnson, 1976 and Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008) and WINGX (Farrugia, 1999)' _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^ > 2\s(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. This crystal is a merohedral twin. The twinning causes rest electron density which we tried to model as non coordinating solvent molecules but failed. The model of clusters C881-C895 and C991-C997 is chemically meaningless. ; _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^)+(0.0083P)^2^+227.2459P] 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 10292 _refine_ls_number_parameters 1145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1111 _refine_ls_R_factor_gt 0.0878 _refine_ls_wR_factor_ref 0.1924 _refine_ls_wR_factor_gt 0.1794 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au Au 0.53784(6) 0.311553(19) 0.43581(6) 0.0412(2) Uani 1 1 d . . . P1 P 0.5257(3) 0.35814(14) 0.5404(3) 0.0390(12) Uani 1 1 d . . . C111 C 0.4117(12) 0.3747(5) 0.5410(15) 0.047(6) Uani 1 1 d . . . C112 C 0.3777(14) 0.3869(6) 0.4673(13) 0.054(6) Uani 1 1 d . . . H112 H 0.4110 0.3859 0.4201 0.064 Uiso 1 1 calc R . . C113 C 0.2916(15) 0.4009(8) 0.4652(15) 0.071(8) Uani 1 1 d . . . H113 H 0.2672 0.4096 0.4163 0.085 Uiso 1 1 calc R . . C114 C 0.2422(13) 0.4016(6) 0.5373(14) 0.050(6) Uani 1 1 d . . . H114 H 0.1841 0.4092 0.5352 0.060 Uiso 1 1 calc R . . C115 C 0.2771(17) 0.3915(7) 0.6076(15) 0.061(7) Uani 1 1 d . . . H115 H 0.2447 0.3944 0.6550 0.073 Uiso 1 1 calc R . . C116 C 0.3633(16) 0.3765(6) 0.6124(16) 0.060(7) Uani 1 1 d . . . H116 H 0.3868 0.3680 0.6618 0.072 Uiso 1 1 calc R . . C121 C 0.5460(14) 0.3366(5) 0.6425(11) 0.038(5) Uani 1 1 d . . . C122 C 0.5717(12) 0.3604(6) 0.7091(14) 0.045(5) Uani 1 1 d . . . H122 H 0.5841 0.3882 0.7028 0.054 Uiso 1 1 calc R . . C123 C 0.5782(13) 0.3426(6) 0.7813(14) 0.053(6) Uani 1 1 d . . . H123 H 0.5957 0.3585 0.8254 0.064 Uiso 1 1 calc R . . C124 C 0.5596(13) 0.3005(6) 0.7940(13) 0.051(6) Uani 1 1 d . . . H124 H 0.5645 0.2887 0.8454 0.062 Uiso 1 1 calc R . . C125 C 0.5342(15) 0.2779(5) 0.7284(12) 0.051(5) Uani 1 1 d . . . H125 H 0.5191 0.2504 0.7350 0.061 Uiso 1 1 calc R . . C126 C 0.5310(14) 0.2960(5) 0.6507(12) 0.044(5) Uani 1 1 d . . . H126 H 0.5186 0.2800 0.6052 0.053 Uiso 1 1 calc R . . C131 C 0.5865(14) 0.4033(6) 0.5284(13) 0.050(6) Uani 1 1 d . . . C132 C 0.5603(12) 0.4428(5) 0.5489(14) 0.053(6) Uani 1 1 d . . . H132 H 0.5065 0.4460 0.5736 0.064 Uiso 1 1 calc R . . C133 C 0.6082(14) 0.4772(6) 0.5351(13) 0.048(6) Uani 1 1 d . . . H133 H 0.5881 0.5027 0.5528 0.058 Uiso 1 1 calc R . . C134 C 0.6863(18) 0.4744(7) 0.4952(14) 0.063(7) Uani 1 1 d . . . H134 H 0.7194 0.4976 0.4839 0.076 Uiso 1 1 calc R . . C135 C 0.7125(13) 0.4371(7) 0.4733(15) 0.061(7) Uani 1 1 d . . . H135 H 0.7657 0.4350 0.4468 0.074 Uiso 1 1 calc R . . C136 C 0.6672(16) 0.4020(6) 0.4869(14) 0.055(6) Uani 1 1 d . . . H136 H 0.6892 0.3769 0.4690 0.066 Uiso 1 1 calc R . . P2 P 0.5269(3) 0.27023(13) 0.3225(3) 0.0383(12) Uani 1 1 d . . . C211 C 0.4679(14) 0.2248(5) 0.3440(12) 0.043(5) Uani 1 1 d . . . C212 C 0.4918(11) 0.2008(5) 0.4128(12) 0.042(5) Uani 1 1 d . . . H212 H 0.5366 0.2104 0.4456 0.051 Uiso 1 1 calc R . . C213 C 0.4531(12) 0.1647(5) 0.4337(13) 0.046(5) Uani 1 1 d . . . H213 H 0.4732 0.1490 0.4771 0.056 Uiso 1 1 calc R . . C214 C 0.3820(13) 0.1522(6) 0.3870(13) 0.042(5) Uani 1 1 d . . . H214 H 0.3540 0.1278 0.4008 0.051 Uiso 1 1 calc R . . C215 C 0.3521(14) 0.1738(6) 0.3232(15) 0.057(6) Uani 1 1 d . . . H215 H 0.3041 0.1646 0.2942 0.068 Uiso 1 1 calc R . . C216 C 0.3942(13) 0.2107(6) 0.3002(14) 0.051(6) Uani 1 1 d . . . H216 H 0.3736 0.2258 0.2562 0.061 Uiso 1 1 calc R . . C221 C 0.4657(15) 0.2995(5) 0.2451(10) 0.040(5) Uani 1 1 d . . . C222 C 0.3873(13) 0.3146(6) 0.2655(13) 0.050(5) Uani 1 1 d . . . H222 H 0.3640 0.3075 0.3157 0.060 Uiso 1 1 calc R . . C223 C 0.3402(14) 0.3401(6) 0.2155(14) 0.050(6) Uani 1 1 d . . . H223 H 0.2873 0.3511 0.2321 0.060 Uiso 1 1 calc R . . C224 C 0.3743(15) 0.3489(6) 0.1398(14) 0.054(6) Uani 1 1 d . . . H224 H 0.3426 0.3644 0.1026 0.065 Uiso 1 1 calc R . . C225 C 0.4563(15) 0.3345(5) 0.1196(11) 0.045(5) Uani 1 1 d . . . H225 H 0.4810 0.3423 0.0703 0.054 Uiso 1 1 calc R . . C226 C 0.5014(11) 0.3090(6) 0.1702(12) 0.040(5) Uani 1 1 d . . . H226 H 0.5549 0.2983 0.1548 0.048 Uiso 1 1 calc R . . C231 C 0.6261(12) 0.2536(6) 0.2747(14) 0.048(6) Uani 1 1 d . . . C232 C 0.7052(15) 0.2696(7) 0.3026(15) 0.066(7) Uani 1 1 d . . . H232 H 0.7071 0.2897 0.3428 0.080 Uiso 1 1 calc R . . C233 C 0.7826(16) 0.2538(10) 0.2667(17) 0.078(8) Uani 1 1 d . . . H233 H 0.8360 0.2637 0.2844 0.094 Uiso 1 1 calc R . . C234 C 0.7803(16) 0.2251(9) 0.2082(19) 0.080(9) Uani 1 1 d . . . H234 H 0.8321 0.2160 0.1855 0.096 Uiso 1 1 calc R . . C235 C 0.7018(16) 0.2086(7) 0.1803(15) 0.063(7) Uani 1 1 d . . . H235 H 0.6986 0.1890 0.1391 0.075 Uiso 1 1 calc R . . C236 C 0.6304(16) 0.2239(6) 0.2189(17) 0.071(8) Uani 1 1 d . . . H236 H 0.5778 0.2120 0.2044 0.085 Uiso 1 1 calc R . . N31 N 0.7537(9) 0.5004(4) 0.0275(9) 0.033(4) Uani 1 1 d . . . C32 C 0.7462(11) 0.4653(5) -0.0124(10) 0.026(4) Uiso 1 1 d . . . O32 O 0.7381(7) 0.4297(4) 0.0127(8) 0.034(3) Uani 1 1 d . . . C33 C 0.7431(10) 0.4750(5) -0.1005(11) 0.029(4) Uani 1 1 d . . . C34 C 0.7370(10) 0.4502(5) -0.1700(10) 0.022(4) Uiso 1 1 d . . . C35 C 0.7432(10) 0.4691(6) -0.2485(12) 0.040(5) Uani 1 1 d . . . C36 C 0.7569(12) 0.5113(5) -0.2528(13) 0.038(5) Uani 1 1 d . . . C37 C 0.7597(10) 0.5353(4) -0.1830(12) 0.028(4) Uani 1 1 d . . . C38 C 0.7553(10) 0.5166(5) -0.1082(11) 0.026(4) Uani 1 1 d . . . C39 C 0.7603(11) 0.5319(5) -0.0234(11) 0.030(4) Uiso 1 1 d . . . O39 O 0.7655(7) 0.5693(3) -0.0094(8) 0.033(3) Uani 1 1 d . . . F34 F 0.7262(6) 0.4094(3) -0.1670(6) 0.039(3) Uani 1 1 d . . . F35 F 0.7348(7) 0.4457(3) -0.3134(7) 0.048(3) Uani 1 1 d . . . F36 F 0.7581(7) 0.5279(3) -0.3281(7) 0.050(3) Uani 1 1 d . . . F37 F 0.7724(7) 0.5754(3) -0.1931(7) 0.043(3) Uani 1 1 d . . . B3 B 0.7406(11) 0.4142(6) 0.1033(13) 0.027(5) Uani 1 1 d . . . C41 C 0.7554(12) 0.3649(5) 0.0856(11) 0.037(5) Uani 1 1 d . . . C42 C 0.7040(13) 0.3426(6) 0.0314(13) 0.043(5) Uani 1 1 d . . . C43 C 0.7195(15) 0.3036(6) 0.0083(14) 0.054(6) Uani 1 1 d . . . C44 C 0.7897(11) 0.2824(5) 0.0360(11) 0.032(4) Uiso 1 1 d . . . C45 C 0.8418(12) 0.3023(6) 0.0920(11) 0.041(5) Uiso 1 1 d . . . C46 C 0.8250(11) 0.3418(6) 0.1165(14) 0.043(5) Uani 1 1 d . . . F42 F 0.6338(6) 0.3626(3) 0.0002(7) 0.049(3) Uani 1 1 d . . . F43 F 0.6641(9) 0.2853(3) -0.0426(8) 0.071(4) Uani 1 1 d . . . F44 F 0.8056(9) 0.2441(3) 0.0133(8) 0.063(4) Uani 1 1 d . . . F45 F 0.9121(7) 0.2820(3) 0.1221(8) 0.058(3) Uani 1 1 d . . . F46 F 0.8807(7) 0.3564(3) 0.1736(7) 0.051(3) Uani 1 1 d . . . C51 C 0.6429(11) 0.4204(5) 0.1446(12) 0.034(5) Uani 1 1 d . . . C52 C 0.6256(12) 0.4025(5) 0.2178(10) 0.028(4) Uani 1 1 d . . . C53 C 0.5492(12) 0.4073(5) 0.2609(10) 0.034(4) Uani 1 1 d . . . C54 C 0.4853(11) 0.4306(5) 0.2271(12) 0.033(5) Uani 1 1 d . . . C55 C 0.4978(11) 0.4494(5) 0.1541(12) 0.031(5) Uani 1 1 d . . . C56 C 0.5754(12) 0.4449(6) 0.1156(10) 0.032(5) Uani 1 1 d . . . F52 F 0.6899(6) 0.3786(3) 0.2538(7) 0.043(3) Uani 1 1 d . . . F53 F 0.5392(8) 0.3884(3) 0.3320(6) 0.051(3) Uani 1 1 d . . . F54 F 0.4107(6) 0.4349(3) 0.2696(7) 0.050(3) Uani 1 1 d . . . F55 F 0.4346(6) 0.4719(3) 0.1216(7) 0.050(3) Uani 1 1 d . . . F56 F 0.5825(6) 0.4655(3) 0.0428(7) 0.041(3) Uani 1 1 d . . . C61 C 0.8198(12) 0.4375(5) 0.1486(12) 0.036(5) Uani 1 1 d . . . C62 C 0.9027(12) 0.4351(6) 0.1209(13) 0.042(5) Uani 1 1 d . . . C63 C 0.9747(12) 0.4484(5) 0.1563(14) 0.046(5) Uani 1 1 d . . . C64 C 0.9691(12) 0.4680(5) 0.2321(12) 0.035(4) Uani 1 1 d . . . C65 C 0.8857(12) 0.4728(6) 0.2679(13) 0.036(5) Uani 1 1 d . . . C66 C 0.8145(12) 0.4566(6) 0.2268(13) 0.041(5) Uani 1 1 d . . . F62 F 0.9168(6) 0.4166(3) 0.0432(6) 0.043(3) Uani 1 1 d . . . F63 F 1.0571(6) 0.4440(3) 0.1254(7) 0.050(3) Uani 1 1 d . . . F64 F 1.0387(8) 0.4825(3) 0.2718(7) 0.054(3) Uani 1 1 d . . . F65 F 0.8798(7) 0.4908(4) 0.3391(8) 0.059(3) Uani 1 1 d . . . F66 F 0.7393(6) 0.4619(3) 0.2631(7) 0.042(3) Uani 1 1 d . . . B9 B 0.7642(11) 0.5905(6) 0.0753(15) 0.033(5) Uani 1 1 d . . . C71 C 0.8601(12) 0.5861(6) 0.1200(13) 0.041(5) Uani 1 1 d . . . C72 C 0.8766(13) 0.6095(5) 0.1927(12) 0.042(5) Uani 1 1 d . . . C73 C 0.9483(12) 0.6079(5) 0.2359(11) 0.041(5) Uani 1 1 d . . . C74 C 1.0139(12) 0.5809(6) 0.2115(13) 0.047(6) Uani 1 1 d . . . C75 C 1.0056(11) 0.5583(5) 0.1432(11) 0.032(4) Uani 1 1 d . . . C76 C 0.9281(11) 0.5606(5) 0.0980(11) 0.033(4) Uiso 1 1 d . . . F72 F 0.8100(7) 0.6345(3) 0.2156(7) 0.045(3) Uani 1 1 d . . . F73 F 0.9569(8) 0.6299(3) 0.3029(7) 0.061(3) Uani 1 1 d . . . F74 F 1.0878(7) 0.5800(4) 0.2560(8) 0.062(4) Uani 1 1 d . . . F75 F 1.0693(6) 0.5337(3) 0.1191(8) 0.056(3) Uani 1 1 d . . . F76 F 0.9241(6) 0.5357(3) 0.0358(7) 0.042(3) Uani 1 1 d . . . C81 C 0.6809(11) 0.5727(5) 0.1255(12) 0.032(4) Uani 1 1 d . . . C82 C 0.6860(12) 0.5543(6) 0.2042(14) 0.046(6) Uani 1 1 d . . . C83 C 0.6145(12) 0.5404(5) 0.2424(12) 0.036(5) Uani 1 1 d . . . C84 C 0.5313(12) 0.5461(5) 0.2099(11) 0.040(5) Uani 1 1 d . . . C85 C 0.5268(12) 0.5641(5) 0.1343(10) 0.034(4) Uiso 1 1 d . . . C86 C 0.5989(12) 0.5766(6) 0.0953(12) 0.037(5) Uani 1 1 d . . . F82 F 0.7635(6) 0.5467(3) 0.2398(7) 0.046(3) Uani 1 1 d . . . F83 F 0.6210(6) 0.5224(3) 0.3187(7) 0.044(3) Uani 1 1 d . . . F84 F 0.4612(7) 0.5337(3) 0.2530(6) 0.045(3) Uani 1 1 d . . . F85 F 0.4464(6) 0.5703(3) 0.1039(7) 0.048(3) Uani 1 1 d . . . F86 F 0.5876(6) 0.5936(3) 0.0214(7) 0.040(3) Uani 1 1 d . . . C91 C 0.7553(10) 0.6397(5) 0.0489(11) 0.034(4) Uani 1 1 d . . . C92 C 0.8136(13) 0.6545(6) -0.0112(14) 0.046(6) Uani 1 1 d . . . C93 C 0.8081(14) 0.6935(6) -0.0404(13) 0.047(6) Uani 1 1 d . . . C94 C 0.7497(16) 0.7209(7) -0.0154(16) 0.063(7) Uani 1 1 d . . . C95 C 0.6878(15) 0.7082(6) 0.0463(14) 0.055(7) Uani 1 1 d . . . C96 C 0.6943(12) 0.6680(5) 0.0745(14) 0.047(6) Uani 1 1 d . . . F92 F 0.8768(6) 0.6307(3) -0.0396(6) 0.044(3) Uani 1 1 d . . . F93 F 0.8691(9) 0.7069(4) -0.0961(9) 0.073(4) Uani 1 1 d . . . F94 F 0.7417(9) 0.7593(3) -0.0417(9) 0.081(5) Uani 1 1 d . . . F95 F 0.6268(8) 0.7331(3) 0.0697(9) 0.066(3) Uani 1 1 d . . . F96 F 0.6365(7) 0.6579(3) 0.1338(8) 0.054(3) Uani 1 1 d . . . C881 C 0.505(8) 0.126(4) 0.825(8) 0.10(4) Uiso 0.30 1 d P . . C882 C 0.466(12) 0.158(5) 0.859(9) 0.12(4) Uiso 0.25 1 d P . . C883 C 0.635(5) 0.186(2) 0.877(5) 0.10(2) Uiso 0.45 1 d P . . C884 C 0.609(11) 0.165(5) 0.821(11) 0.09(5) Uiso 0.20 1 d P . . C885 C 0.562(7) 0.142(3) 0.788(6) 0.09(3) Uiso 0.30 1 d P . . C886 C 0.392(6) 0.150(3) 0.894(6) 0.09(3) Uiso 0.35 1 d P . . C887 C 0.434(6) 0.163(2) 0.949(6) 0.10(2) Uiso 0.40 1 d P . . C888 C 0.520(8) 0.141(4) 0.866(7) 0.10(3) Uiso 0.35 1 d P . . C889 C 0.375(5) 0.161(2) 0.960(4) 0.09(2) Uiso 0.45 1 d P . . C890 C 0.556(6) 0.170(3) 0.861(5) 0.09(2) Uiso 0.40 1 d P . . C891 C 0.500(5) 0.184(3) 0.987(5) 0.10(2) Uiso 0.40 1 d P . . C892 C 0.473(6) 0.195(3) 1.045(6) 0.11(3) Uiso 0.35 1 d P . . C894 C 0.502(8) 0.170(3) 0.911(7) 0.09(3) Uiso 0.30 1 d P . . C895 C 0.572(5) 0.187(3) 0.952(5) 0.09(2) Uiso 0.35 1 d P . . C991 C 0.495(5) 0.044(3) 0.016(5) 0.10(2) Uiso 0.40 1 d P . . C992 C 0.547(5) 0.026(2) -0.040(4) 0.085(19) Uiso 0.40 1 d P . . C993 C 0.438(5) 0.014(2) 0.046(5) 0.10(2) Uiso 0.40 1 d P . . C996 C 0.477(5) 0.079(2) 0.021(4) 0.09(2) Uiso 0.40 1 d P . . C995 C 0.597(3) 0.0563(15) -0.076(3) 0.077(14) Uiso 0.50 1 d P . . C997 C 0.376(5) 0.026(2) 0.099(5) 0.09(2) Uiso 0.40 1 d P . . 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 Au 0.0399(4) 0.0281(3) 0.0555(4) 0.0004(4) -0.0045(5) -0.0026(4) P1 0.040(3) 0.026(2) 0.052(3) -0.011(2) -0.002(3) -0.005(2) C111 0.034(11) 0.010(9) 0.10(2) -0.006(10) 0.009(12) -0.007(8) C112 0.055(14) 0.052(13) 0.054(15) 0.031(11) -0.003(11) 0.034(11) C113 0.053(15) 0.090(19) 0.070(19) 0.032(14) -0.021(14) -0.006(13) C114 0.033(11) 0.058(14) 0.059(16) 0.003(11) 0.024(12) -0.012(10) C115 0.075(19) 0.056(15) 0.053(16) -0.015(13) 0.003(14) -0.035(13) C116 0.069(18) 0.034(12) 0.076(18) 0.005(12) 0.001(15) -0.022(12) C121 0.049(12) 0.021(9) 0.043(11) -0.002(8) 0.021(11) 0.007(10) C122 0.035(11) 0.028(10) 0.073(16) -0.002(11) 0.001(10) -0.009(8) C123 0.059(14) 0.035(12) 0.065(16) 0.001(11) -0.017(12) 0.004(10) C124 0.068(16) 0.038(12) 0.048(13) 0.007(10) -0.026(11) -0.004(10) C125 0.061(13) 0.023(9) 0.069(14) 0.011(10) 0.016(14) -0.021(11) C126 0.054(13) 0.027(10) 0.051(12) 0.002(9) 0.005(12) -0.017(11) C131 0.049(13) 0.047(13) 0.055(14) -0.009(11) -0.017(11) 0.009(10) C132 0.041(12) 0.037(11) 0.082(16) -0.009(11) -0.016(11) -0.010(9) C133 0.058(14) 0.022(10) 0.065(16) 0.020(9) -0.023(12) -0.018(10) C134 0.082(19) 0.057(17) 0.050(15) 0.001(12) -0.016(14) -0.018(14) C135 0.025(11) 0.072(17) 0.086(18) -0.016(14) -0.020(11) -0.007(11) C136 0.078(17) 0.026(11) 0.060(16) 0.021(11) -0.013(13) -0.019(11) P2 0.037(3) 0.028(2) 0.050(3) -0.001(2) -0.002(3) -0.002(2) C211 0.050(12) 0.019(9) 0.059(12) -0.018(9) -0.011(12) 0.016(10) C212 0.041(11) 0.027(10) 0.059(14) -0.008(9) 0.007(9) 0.002(8) C213 0.054(12) 0.031(10) 0.054(12) 0.005(9) 0.013(15) 0.002(9) C214 0.044(12) 0.031(11) 0.052(14) -0.002(10) 0.012(11) -0.001(10) C215 0.052(14) 0.041(13) 0.077(18) -0.014(12) -0.019(13) -0.011(11) C216 0.050(13) 0.031(12) 0.072(16) 0.013(11) -0.014(12) 0.018(10) C221 0.052(12) 0.041(10) 0.027(10) -0.003(8) -0.025(11) 0.003(11) C222 0.047(12) 0.046(12) 0.057(14) -0.009(11) -0.006(11) 0.021(11) C223 0.048(14) 0.046(13) 0.057(16) 0.003(11) 0.002(12) 0.001(10) C224 0.068(16) 0.026(11) 0.067(17) -0.010(11) -0.035(14) 0.008(11) C225 0.050(12) 0.043(11) 0.041(12) 0.002(9) -0.003(12) -0.017(12) C226 0.027(9) 0.042(11) 0.051(13) -0.001(10) -0.003(9) 0.005(9) C231 0.029(11) 0.048(13) 0.069(15) 0.022(12) 0.003(11) 0.005(10) C232 0.057(15) 0.067(16) 0.075(18) 0.005(13) -0.018(14) 0.002(12) C233 0.048(16) 0.12(2) 0.065(19) 0.020(17) 0.012(14) -0.010(16) C234 0.048(16) 0.09(2) 0.11(2) 0.040(18) 0.016(16) 0.045(15) C235 0.069(17) 0.041(13) 0.078(18) 0.019(12) 0.036(15) -0.006(12) C236 0.068(17) 0.022(11) 0.12(2) -0.005(14) 0.034(16) 0.000(11) N31 0.017(7) 0.026(8) 0.054(10) -0.006(7) -0.001(7) 0.000(6) O32 0.023(7) 0.026(7) 0.055(9) 0.002(6) 0.004(6) 0.002(5) C33 0.013(8) 0.015(9) 0.059(13) 0.008(8) 0.000(8) 0.003(7) C35 0.003(8) 0.071(15) 0.047(13) -0.023(11) -0.007(8) 0.003(9) C36 0.030(10) 0.021(10) 0.062(15) 0.018(10) -0.002(10) 0.002(8) C37 0.014(9) 0.005(8) 0.065(14) -0.007(9) -0.010(9) 0.005(6) C38 0.009(8) 0.027(10) 0.040(11) 0.020(9) -0.008(8) 0.000(7) O39 0.027(7) 0.015(6) 0.056(8) -0.002(6) -0.003(6) -0.009(5) F34 0.039(6) 0.023(5) 0.054(7) -0.007(5) 0.004(5) -0.002(5) F35 0.042(6) 0.050(7) 0.053(7) 0.001(6) -0.006(6) -0.001(5) F36 0.055(7) 0.043(7) 0.053(8) 0.015(6) -0.003(6) -0.004(6) F37 0.045(6) 0.026(6) 0.060(7) 0.017(5) -0.013(6) 0.002(5) B3 0.009(9) 0.026(11) 0.047(13) -0.011(10) 0.012(9) -0.009(8) C41 0.039(11) 0.024(10) 0.048(13) 0.000(9) -0.004(10) -0.011(9) C42 0.046(12) 0.032(12) 0.052(13) 0.011(10) -0.001(10) 0.021(10) C43 0.072(16) 0.026(12) 0.064(15) -0.003(10) -0.018(12) -0.017(11) C46 0.011(9) 0.037(11) 0.081(16) 0.009(11) 0.006(10) -0.001(8) F42 0.035(6) 0.030(6) 0.082(9) 0.003(6) -0.019(6) -0.006(5) F43 0.093(9) 0.032(6) 0.088(11) -0.021(7) -0.030(8) -0.002(6) F44 0.095(10) 0.023(6) 0.071(8) 0.001(6) 0.005(7) 0.013(6) F45 0.032(6) 0.050(7) 0.092(10) 0.016(7) -0.004(6) 0.010(5) F46 0.042(6) 0.036(6) 0.076(8) 0.001(6) -0.017(6) 0.000(5) C51 0.026(10) 0.021(9) 0.056(14) -0.011(9) 0.007(9) -0.012(8) C52 0.042(12) 0.021(9) 0.020(10) 0.012(8) -0.005(9) -0.009(8) C53 0.037(12) 0.030(10) 0.033(11) 0.014(8) 0.014(10) 0.006(9) C54 0.028(11) 0.025(9) 0.045(12) -0.017(9) 0.012(9) -0.014(8) C55 0.027(10) 0.012(9) 0.053(13) 0.004(9) -0.002(9) 0.008(7) C56 0.038(11) 0.049(12) 0.008(10) -0.006(8) 0.000(8) 0.014(9) F52 0.029(6) 0.037(6) 0.064(8) 0.010(6) 0.001(5) 0.002(5) F53 0.042(6) 0.060(7) 0.049(7) 0.014(6) 0.006(7) 0.004(6) F54 0.028(6) 0.050(7) 0.072(8) 0.003(6) 0.014(6) 0.002(5) F55 0.039(7) 0.044(6) 0.066(8) 0.004(6) -0.004(6) 0.015(5) F56 0.021(5) 0.045(6) 0.058(8) 0.004(5) 0.001(5) 0.004(4) C61 0.029(11) 0.023(10) 0.056(14) 0.011(9) 0.013(10) 0.011(8) C62 0.025(12) 0.045(13) 0.056(15) 0.012(11) 0.005(10) -0.004(9) C63 0.022(11) 0.027(10) 0.088(16) 0.005(10) -0.002(11) -0.018(9) C64 0.025(10) 0.023(9) 0.057(13) 0.016(9) 0.003(11) -0.002(9) C65 0.020(10) 0.036(11) 0.053(14) 0.008(10) -0.015(10) -0.004(8) C66 0.023(11) 0.045(12) 0.054(14) 0.005(11) 0.012(10) 0.003(9) F62 0.022(5) 0.053(7) 0.052(8) 0.003(6) -0.001(5) -0.002(5) F63 0.020(6) 0.063(7) 0.067(8) -0.001(6) -0.010(5) -0.005(5) F64 0.030(6) 0.060(7) 0.073(8) -0.006(6) -0.009(7) -0.006(6) F65 0.040(7) 0.070(8) 0.066(9) -0.018(7) -0.015(6) 0.002(6) F66 0.033(6) 0.040(6) 0.053(7) 0.000(5) -0.004(5) 0.004(5) B9 0.012(9) 0.022(10) 0.065(16) -0.011(11) 0.008(11) 0.006(8) C71 0.031(10) 0.030(10) 0.063(14) 0.009(10) 0.012(10) 0.011(8) C72 0.059(14) 0.024(10) 0.044(13) 0.002(9) 0.016(11) 0.016(10) C73 0.034(12) 0.044(11) 0.044(12) -0.007(9) -0.025(10) -0.019(10) C74 0.036(13) 0.043(12) 0.062(15) 0.028(11) -0.013(11) 0.018(9) C75 0.031(10) 0.030(10) 0.034(11) 0.010(9) -0.005(9) -0.001(8) F72 0.039(6) 0.040(6) 0.056(7) -0.017(5) -0.009(5) -0.002(5) F73 0.052(7) 0.055(7) 0.076(8) -0.025(6) -0.011(8) -0.003(7) F74 0.041(7) 0.047(7) 0.096(10) -0.001(7) -0.007(7) 0.000(6) F75 0.027(6) 0.050(7) 0.092(9) -0.007(7) -0.007(6) 0.015(5) F76 0.023(5) 0.039(6) 0.065(8) -0.016(5) 0.001(5) 0.001(4) C81 0.026(11) 0.024(10) 0.047(13) 0.009(9) 0.010(9) 0.011(8) C82 0.023(11) 0.033(11) 0.082(17) -0.016(11) 0.006(11) -0.011(9) C83 0.034(12) 0.026(10) 0.050(14) 0.011(9) -0.016(10) -0.013(9) C84 0.023(10) 0.039(10) 0.057(12) -0.003(9) 0.017(11) -0.018(9) C86 0.027(11) 0.050(13) 0.034(12) -0.010(10) 0.000(9) -0.014(9) F82 0.017(5) 0.037(6) 0.083(9) 0.014(6) 0.004(6) 0.002(5) F83 0.023(5) 0.043(6) 0.066(8) 0.002(6) 0.000(5) -0.001(5) F84 0.030(6) 0.042(6) 0.061(7) -0.011(5) 0.003(6) 0.000(6) F85 0.027(6) 0.050(6) 0.066(7) 0.006(5) 0.003(5) -0.013(5) F86 0.029(6) 0.039(6) 0.052(7) 0.007(5) 0.011(5) -0.001(5) C91 0.021(9) 0.036(10) 0.044(13) -0.004(9) 0.008(9) 0.007(8) C92 0.035(12) 0.024(11) 0.079(17) -0.008(11) -0.009(11) 0.009(9) C93 0.056(13) 0.022(11) 0.064(16) 0.000(10) -0.012(12) 0.002(11) C94 0.054(15) 0.043(14) 0.091(19) 0.042(13) -0.031(14) -0.017(12) C95 0.073(15) 0.020(10) 0.072(17) -0.032(11) -0.036(14) 0.027(11) C96 0.045(12) 0.026(11) 0.070(16) -0.040(11) -0.026(13) 0.019(9) F92 0.043(6) 0.035(6) 0.054(8) 0.003(5) -0.004(5) 0.002(5) F93 0.081(10) 0.043(7) 0.096(11) 0.019(7) 0.006(8) -0.007(7) F94 0.113(11) 0.024(6) 0.105(12) 0.032(7) -0.017(9) 0.005(6) F95 0.081(8) 0.030(6) 0.085(9) -0.015(7) -0.009(8) 0.033(6) F96 0.035(6) 0.044(7) 0.084(9) -0.004(6) 0.013(7) 0.007(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Au P1 2.297(5) . ? Au P2 2.301(5) . ? P1 C131 1.75(2) . ? P1 C111 1.837(19) . ? P1 C121 1.843(18) . ? C111 C112 1.38(3) . ? C111 C116 1.39(3) . ? C112 C113 1.40(3) . ? C112 H112 0.9300 . ? C113 C114 1.41(3) . ? C113 H113 0.9300 . ? C114 C115 1.31(3) . ? C114 H114 0.9300 . ? C115 C116 1.42(3) . ? C115 H115 0.9300 . ? C116 H116 0.9300 . ? C121 C126 1.35(2) . ? C121 C122 1.40(3) . ? C122 C123 1.32(3) . ? C122 H122 0.9300 . ? C123 C124 1.41(3) . ? C123 H123 0.9300 . ? C124 C125 1.36(3) . ? C124 H124 0.9300 . ? C125 C126 1.41(3) . ? C125 H125 0.9300 . ? C126 H126 0.9300 . ? C131 C132 1.39(3) . ? C131 C136 1.42(3) . ? C132 C133 1.36(2) . ? C132 H132 0.9300 . ? C133 C134 1.37(3) . ? C133 H133 0.9300 . ? C134 C135 1.33(3) . ? C134 H134 0.9300 . ? C135 C136 1.36(3) . ? C135 H135 0.9300 . ? C136 H136 0.9300 . ? P2 C211 1.769(19) . ? P2 C231 1.80(2) . ? P2 C221 1.848(17) . ? C211 C212 1.42(2) . ? C211 C216 1.42(3) . ? C212 C213 1.36(2) . ? C212 H212 0.9300 . ? C213 C214 1.40(3) . ? C213 H213 0.9300 . ? C214 C215 1.34(3) . ? C214 H214 0.9300 . ? C215 C216 1.41(3) . ? C215 H215 0.9300 . ? C216 H216 0.9300 . ? C221 C222 1.35(3) . ? C221 C226 1.38(3) . ? C222 C223 1.37(3) . ? C222 H222 0.9300 . ? C223 C224 1.38(3) . ? C223 H223 0.9300 . ? C224 C225 1.39(3) . ? C224 H224 0.9300 . ? C225 C226 1.36(3) . ? C225 H225 0.9300 . ? C226 H226 0.9300 . ? C231 C236 1.33(3) . ? C231 C232 1.40(3) . ? C232 C233 1.43(3) . ? C232 H232 0.9300 . ? C233 C234 1.34(4) . ? C233 H233 0.9300 . ? C234 C235 1.40(3) . ? C234 H234 0.9300 . ? C235 C236 1.36(3) . ? C235 H235 0.9300 . ? C236 H236 0.9300 . ? N31 C32 1.32(2) . ? N31 C39 1.33(2) . ? C32 O32 1.23(2) . ? C32 C33 1.48(2) . ? O32 B3 1.57(2) . ? C33 C38 1.37(2) . ? C33 C34 1.40(2) . ? C34 F34 1.339(18) . ? C34 C35 1.43(3) . ? C35 F35 1.32(2) . ? C35 C36 1.39(3) . ? C36 F36 1.35(2) . ? C36 C37 1.39(3) . ? C37 F37 1.326(17) . ? C37 C38 1.37(2) . ? C38 C39 1.48(2) . ? C39 O39 1.24(2) . ? O39 B9 1.55(3) . ? B3 C61 1.62(3) . ? B3 C41 1.64(2) . ? B3 C51 1.66(2) . ? C41 C42 1.39(3) . ? C41 C46 1.41(2) . ? C42 C43 1.35(3) . ? C42 F42 1.36(2) . ? C43 F43 1.34(2) . ? C43 C44 1.36(3) . ? C44 F44 1.32(2) . ? C44 C45 1.38(2) . ? C45 F45 1.36(2) . ? C45 C46 1.37(3) . ? C46 F46 1.36(2) . ? C51 C52 1.36(2) . ? C51 C56 1.40(2) . ? C52 C53 1.38(3) . ? C52 F52 1.392(19) . ? C53 F53 1.330(18) . ? C53 C54 1.36(2) . ? C54 F54 1.352(19) . ? C54 C55 1.36(3) . ? C55 F55 1.331(18) . ? C55 C56 1.36(2) . ? C56 F56 1.37(2) . ? C61 C62 1.36(3) . ? C61 C66 1.43(3) . ? C62 C63 1.33(3) . ? C62 F62 1.43(2) . ? C63 F63 1.38(2) . ? C63 C64 1.40(3) . ? C64 F64 1.34(2) . ? C64 C65 1.42(3) . ? C65 F65 1.31(2) . ? C65 C66 1.39(3) . ? C66 F66 1.31(2) . ? B9 C81 1.63(3) . ? B9 C71 1.66(3) . ? B9 C91 1.66(2) . ? C71 C76 1.39(2) . ? C71 C72 1.44(3) . ? C72 C73 1.31(3) . ? C72 F72 1.36(2) . ? C73 F73 1.321(19) . ? C73 C74 1.40(3) . ? C74 C75 1.35(3) . ? C74 F74 1.35(2) . ? C75 F75 1.327(19) . ? C75 C76 1.41(2) . ? C76 F76 1.304(19) . ? C81 C86 1.36(2) . ? C81 C82 1.43(3) . ? C82 C83 1.35(3) . ? C82 F82 1.35(2) . ? C83 F83 1.39(2) . ? C83 C84 1.40(3) . ? C84 F84 1.35(2) . ? C84 C85 1.37(2) . ? C85 C86 1.34(3) . ? C85 F85 1.35(2) . ? C86 F86 1.34(2) . ? C91 C96 1.38(2) . ? C91 C92 1.42(3) . ? C92 F92 1.33(2) . ? C92 C93 1.36(3) . ? C93 C94 1.33(3) . ? C93 F93 1.38(2) . ? C94 F94 1.33(2) . ? C94 C95 1.45(3) . ? C95 F95 1.30(2) . ? C95 C96 1.39(3) . ? C96 F96 1.36(2) . ? C881 C888 0.86(13) . ? C881 C885 1.17(13) . ? C881 C882 1.32(19) . ? C881 C890 1.74(15) . ? C881 C894 2.02(16) . ? C881 C884 2.0(2) . ? C882 C888 1.00(17) . ? C882 C894 1.10(16) . ? C882 C886 1.32(17) . ? C882 C890 1.4(2) . ? C882 C887 1.57(18) . ? C882 C885 1.9(2) . ? C883 C884 1.21(17) . ? C883 C890 1.35(10) . ? C883 C895 1.58(11) . ? C884 C890 1.06(16) . ? C884 C885 1.17(17) . ? C884 C888 1.7(2) . ? C885 C888 1.42(14) . ? C885 C890 1.51(13) . ? C886 C889 1.16(10) . ? C886 C887 1.19(11) . ? C886 C894 1.85(15) . ? C886 C888 2.06(14) . ? C887 C889 0.93(9) . ? C887 C894 1.24(12) . ? C887 C891 1.37(10) . ? C887 C892 1.98(12) . ? C887 C888 2.04(15) . ? C888 C890 1.10(12) . ? C888 C894 1.24(15) . ? C890 C894 1.17(12) . ? C890 C895 1.62(12) . ? C891 C892 1.10(10) . ? C891 C895 1.25(10) . ? C891 C894 1.32(13) . ? C894 C895 1.39(12) . ? C991 C996 1.15(9) . ? C991 C992 1.36(9) . ? C991 C993 1.40(9) . ? C992 C993 1.32(8) 3_655 ? C992 C995 1.38(8) . ? C993 C992 1.32(8) 3_655 ? C993 C997 1.36(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au P2 169.52(19) . . ? C131 P1 C111 105.5(9) . . ? C131 P1 C121 109.2(9) . . ? C111 P1 C121 105.6(10) . . ? C131 P1 Au 115.1(8) . . ? C111 P1 Au 106.0(7) . . ? C121 P1 Au 114.6(5) . . ? C112 C111 C116 121.7(19) . . ? C112 C111 P1 116.3(17) . . ? C116 C111 P1 122.0(18) . . ? C111 C112 C113 118(2) . . ? C111 C112 H112 120.8 . . ? C113 C112 H112 120.8 . . ? C112 C113 C114 120(2) . . ? C112 C113 H113 120.1 . . ? C114 C113 H113 120.1 . . ? C115 C114 C113 121(2) . . ? C115 C114 H114 119.5 . . ? C113 C114 H114 119.5 . . ? C114 C115 C116 121(2) . . ? C114 C115 H115 119.4 . . ? C116 C115 H115 119.4 . . ? C111 C116 C115 118(2) . . ? C111 C116 H116 121.0 . . ? C115 C116 H116 121.0 . . ? C126 C121 C122 120.8(18) . . ? C126 C121 P1 115.7(15) . . ? C122 C121 P1 123.4(13) . . ? C123 C122 C121 118.8(18) . . ? C123 C122 H122 120.6 . . ? C121 C122 H122 120.6 . . ? C122 C123 C124 123(2) . . ? C122 C123 H123 118.6 . . ? C124 C123 H123 118.6 . . ? C125 C124 C123 117.6(19) . . ? C125 C124 H124 121.2 . . ? C123 C124 H124 121.2 . . ? C124 C125 C126 120.2(16) . . ? C124 C125 H125 119.9 . . ? C126 C125 H125 119.9 . . ? C121 C126 C125 119.6(17) . . ? C121 C126 H126 120.2 . . ? C125 C126 H126 120.2 . . ? C132 C131 C136 113(2) . . ? C132 C131 P1 126.4(17) . . ? C136 C131 P1 119.9(16) . . ? C133 C132 C131 124(2) . . ? C133 C132 H132 117.8 . . ? C131 C132 H132 117.8 . . ? C132 C133 C134 120(2) . . ? C132 C133 H133 120.0 . . ? C134 C133 H133 120.0 . . ? C135 C134 C133 117(2) . . ? C135 C134 H134 121.3 . . ? C133 C134 H134 121.4 . . ? C134 C135 C136 125(2) . . ? C134 C135 H135 117.7 . . ? C136 C135 H135 117.7 . . ? C135 C136 C131 120(2) . . ? C135 C136 H136 119.8 . . ? C131 C136 H136 119.8 . . ? C211 P2 C231 105.8(9) . . ? C211 P2 C221 107.7(9) . . ? C231 P2 C221 106.8(10) . . ? C211 P2 Au 111.3(6) . . ? C231 P2 Au 117.8(8) . . ? C221 P2 Au 107.1(5) . . ? C212 C211 C216 115.6(17) . . ? C212 C211 P2 118.9(14) . . ? C216 C211 P2 125.5(15) . . ? C213 C212 C211 124.1(18) . . ? C213 C212 H212 117.9 . . ? C211 C212 H212 117.9 . . ? C212 C213 C214 117.1(19) . . ? C212 C213 H213 121.4 . . ? C214 C213 H213 121.4 . . ? C215 C214 C213 123.0(19) . . ? C215 C214 H214 118.5 . . ? C213 C214 H214 118.5 . . ? C214 C215 C216 119.6(19) . . ? C214 C215 H215 120.2 . . ? C216 C215 H215 120.2 . . ? C215 C216 C211 120.4(19) . . ? C215 C216 H216 119.8 . . ? C211 C216 H216 119.8 . . ? C222 C221 C226 119.8(17) . . ? C222 C221 P2 118.4(16) . . ? C226 C221 P2 121.6(16) . . ? C221 C222 C223 123(2) . . ? C221 C222 H222 118.4 . . ? C223 C222 H222 118.4 . . ? C222 C223 C224 117(2) . . ? C222 C223 H223 121.3 . . ? C224 C223 H223 121.3 . . ? C223 C224 C225 119.5(19) . . ? C223 C224 H224 120.3 . . ? C225 C224 H224 120.3 . . ? C226 C225 C224 121.6(19) . . ? C226 C225 H225 119.2 . . ? C224 C225 H225 119.2 . . ? C225 C226 C221 118.3(18) . . ? C225 C226 H226 120.8 . . ? C221 C226 H226 120.8 . . ? C236 C231 C232 117(2) . . ? C236 C231 P2 124.0(17) . . ? C232 C231 P2 119.0(19) . . ? C231 C232 C233 117(2) . . ? C231 C232 H232 121.3 . . ? C233 C232 H232 121.3 . . ? C234 C233 C232 122(3) . . ? C234 C233 H233 119.2 . . ? C232 C233 H233 119.2 . . ? C233 C234 C235 122(2) . . ? C233 C234 H234 119.2 . . ? C235 C234 H234 119.2 . . ? C236 C235 C234 114(2) . . ? C236 C235 H235 123.1 . . ? C234 C235 H235 123.1 . . ? C231 C236 C235 129(2) . . ? C231 C236 H236 115.7 . . ? C235 C236 H236 115.7 . . ? C32 N31 C39 111.2(15) . . ? O32 C32 N31 130.7(16) . . ? O32 C32 C33 121.5(16) . . ? N31 C32 C33 107.6(15) . . ? C32 O32 B3 128.0(14) . . ? C38 C33 C34 120.1(17) . . ? C38 C33 C32 107.2(16) . . ? C34 C33 C32 132.5(15) . . ? F34 C34 C33 123.3(15) . . ? F34 C34 C35 117.9(14) . . ? C33 C34 C35 118.9(15) . . ? F35 C35 C36 122.9(19) . . ? F35 C35 C34 118.4(17) . . ? C36 C35 C34 118.7(17) . . ? F36 C36 C37 122.2(15) . . ? F36 C36 C35 116.3(18) . . ? C37 C36 C35 121.1(17) . . ? F37 C37 C38 123.6(16) . . ? F37 C37 C36 116.9(16) . . ? C38 C37 C36 119.3(15) . . ? C33 C38 C37 121.7(17) . . ? C33 C38 C39 104.6(15) . . ? C37 C38 C39 133.7(15) . . ? O39 C39 N31 130.2(17) . . ? O39 C39 C38 120.4(15) . . ? N31 C39 C38 109.3(14) . . ? C39 O39 B9 126.9(14) . . ? O32 B3 C61 107.7(14) . . ? O32 B3 C41 98.6(13) . . ? C61 B3 C41 115.5(15) . . ? O32 B3 C51 109.0(15) . . ? C61 B3 C51 116.1(15) . . ? C41 B3 C51 108.3(13) . . ? C42 C41 C46 112.6(16) . . ? C42 C41 B3 122.8(16) . . ? C46 C41 B3 124.4(16) . . ? C43 C42 F42 118.9(19) . . ? C43 C42 C41 124.8(18) . . ? F42 C42 C41 116.3(16) . . ? F43 C43 C42 119(2) . . ? F43 C43 C44 119.5(17) . . ? C42 C43 C44 121.6(19) . . ? F44 C44 C43 122.0(17) . . ? F44 C44 C45 121.4(16) . . ? C43 C44 C45 116.6(17) . . ? F45 C45 C46 120.0(17) . . ? F45 C45 C44 118.5(16) . . ? C46 C45 C44 121.6(18) . . ? F46 C46 C45 114.3(16) . . ? F46 C46 C41 122.9(16) . . ? C45 C46 C41 122.8(19) . . ? C52 C51 C56 113.6(16) . . ? C52 C51 B3 119.1(17) . . ? C56 C51 B3 127.2(17) . . ? C51 C52 C53 124.8(16) . . ? C51 C52 F52 118.3(16) . . ? C53 C52 F52 116.9(14) . . ? F53 C53 C54 122.1(16) . . ? F53 C53 C52 119.7(16) . . ? C54 C53 C52 118.1(15) . . ? F54 C54 C55 121.9(16) . . ? F54 C54 C53 117.6(16) . . ? C55 C54 C53 120.4(16) . . ? F55 C55 C54 119.8(16) . . ? F55 C55 C56 121.0(16) . . ? C54 C55 C56 119.2(16) . . ? C55 C56 F56 115.0(15) . . ? C55 C56 C51 123.8(17) . . ? F56 C56 C51 121.1(16) . . ? C62 C61 C66 112.3(18) . . ? C62 C61 B3 121.9(18) . . ? C66 C61 B3 125.0(16) . . ? C63 C62 C61 128(2) . . ? C63 C62 F62 113.7(17) . . ? C61 C62 F62 117.9(17) . . ? C62 C63 F63 125.3(19) . . ? C62 C63 C64 119.1(19) . . ? F63 C63 C64 115.6(16) . . ? F64 C64 C63 122.8(17) . . ? F64 C64 C65 118.9(17) . . ? C63 C64 C65 118.2(18) . . ? F65 C65 C66 123.2(18) . . ? F65 C65 C64 118.7(16) . . ? C66 C65 C64 118.1(19) . . ? F66 C66 C65 115.2(18) . . ? F66 C66 C61 121.0(17) . . ? C65 C66 C61 123.7(18) . . ? O39 B9 C81 107.8(14) . . ? O39 B9 C71 110.4(13) . . ? C81 B9 C71 116.6(17) . . ? O39 B9 C91 101.2(15) . . ? C81 B9 C91 114.1(13) . . ? C71 B9 C91 105.7(13) . . ? C76 C71 C72 113.5(17) . . ? C76 C71 B9 127.7(18) . . ? C72 C71 B9 118.7(16) . . ? C73 C72 F72 120.6(18) . . ? C73 C72 C71 125.1(17) . . ? F72 C72 C71 114.3(17) . . ? C72 C73 F73 120.8(18) . . ? C72 C73 C74 118.6(17) . . ? F73 C73 C74 120.5(17) . . ? C75 C74 F74 121.2(17) . . ? C75 C74 C73 120.8(17) . . ? F74 C74 C73 117.9(19) . . ? F75 C75 C74 120.4(15) . . ? F75 C75 C76 120.2(16) . . ? C74 C75 C76 119.4(17) . . ? F76 C76 C71 122.7(16) . . ? F76 C76 C75 114.9(16) . . ? C71 C76 C75 122.4(18) . . ? C86 C81 C82 114.8(17) . . ? C86 C81 B9 120.8(17) . . ? C82 C81 B9 124.3(16) . . ? C83 C82 F82 117.3(19) . . ? C83 C82 C81 121.2(18) . . ? F82 C82 C81 121.2(16) . . ? C82 C83 F83 120.2(17) . . ? C82 C83 C84 121.8(18) . . ? F83 C83 C84 117.8(16) . . ? F84 C84 C85 124.0(18) . . ? F84 C84 C83 119.5(16) . . ? C85 C84 C83 116.5(17) . . ? C86 C85 F85 122.5(16) . . ? C86 C85 C84 121.1(18) . . ? F85 C85 C84 116.3(17) . . ? C85 C86 F86 116.5(16) . . ? C85 C86 C81 124.3(18) . . ? F86 C86 C81 119.2(16) . . ? C96 C91 C92 114.6(18) . . ? C96 C91 B9 128.2(17) . . ? C92 C91 B9 117.0(15) . . ? F92 C92 C93 118(2) . . ? F92 C92 C91 120.8(16) . . ? C93 C92 C91 121.5(19) . . ? C94 C93 C92 124(2) . . ? C94 C93 F93 117.0(18) . . ? C92 C93 F93 119.0(19) . . ? F94 C94 C93 126(2) . . ? F94 C94 C95 116(2) . . ? C93 C94 C95 118.1(18) . . ? F95 C95 C96 123(2) . . ? F95 C95 C94 120(2) . . ? C96 C95 C94 116.9(19) . . ? F96 C96 C91 120.2(18) . . ? F96 C96 C95 114.7(17) . . ? C91 C96 C95 125(2) . . ? C888 C881 C885 88(10) . . ? C888 C881 C882 49(10) . . ? C885 C881 C882 103(10) . . ? C888 C881 C890 32(10) . . ? C885 C881 C890 59(8) . . ? C882 C881 C890 54(10) . . ? C888 C881 C894 19(10) . . ? C885 C881 C894 94(10) . . ? C882 C881 C894 30(9) . . ? C890 C881 C894 35(5) . . ? C888 C881 C884 58(10) . . ? C885 C881 C884 30(8) . . ? C882 C881 C884 84(10) . . ? C890 C881 C884 32(5) . . ? C894 C881 C884 67(7) . . ? C888 C882 C894 72(10) . . ? C888 C882 C886 125(10) . . ? C894 C882 C886 99(10) . . ? C888 C882 C881 41(10) . . ? C894 C882 C881 113(10) . . ? C886 C882 C881 116(10) . . ? C888 C882 C890 50(10) . . ? C894 C882 C890 53(10) . . ? C886 C882 C890 152(10) . . ? C881 C882 C890 78(10) . . ? C888 C882 C887 103(10) . . ? C894 C882 C887 51(10) . . ? C886 C882 C887 48(7) . . ? C881 C882 C887 130(10) . . ? C890 C882 C887 104(10) . . ? C888 C882 C885 45(10) . . ? C894 C882 C885 101(10) . . ? C886 C882 C885 151(10) . . ? C881 C882 C885 36(7) . . ? C890 C882 C885 50(7) . . ? C887 C882 C885 146(10) . . ? C884 C883 C890 49(8) . . ? C884 C883 C895 114(10) . . ? C890 C883 C895 67(6) . . ? C890 C884 C885 85(10) . . ? C890 C884 C883 73(10) . . ? C885 C884 C883 156(10) . . ? C890 C884 C888 38(8) . . ? C885 C884 C888 55(9) . . ? C883 C884 C888 101(10) . . ? C890 C884 C881 59(10) . . ? C885 C884 C881 30(8) . . ? C883 C884 C881 126(10) . . ? C888 C884 C881 25(5) . . ? C884 C885 C881 120(10) . . ? C884 C885 C888 83(10) . . ? C881 C885 C888 37(7) . . ? C884 C885 C890 44(9) . . ? C881 C885 C890 80(9) . . ? C888 C885 C890 44(6) . . ? C884 C885 C882 92(10) . . ? C881 C885 C882 41(8) . . ? C888 C885 C882 30(6) . . ? C890 C885 C882 47(7) . . ? C889 C886 C887 46(6) . . ? C889 C886 C882 123(10) . . ? C887 C886 C882 78(10) . . ? C889 C886 C894 87(8) . . ? C887 C886 C894 41(6) . . ? C882 C886 C894 36(8) . . ? C889 C886 C888 118(8) . . ? C887 C886 C888 73(7) . . ? C882 C886 C888 24(7) . . ? C894 C886 C888 36(5) . . ? C889 C887 C886 65(8) . . ? C889 C887 C894 160(10) . . ? C886 C887 C894 99(10) . . ? C889 C887 C891 133(10) . . ? C886 C887 C891 159(10) . . ? C894 C887 C891 61(7) . . ? C889 C887 C882 119(10) . . ? C886 C887 C882 55(8) . . ? C894 C887 C882 44(8) . . ? C891 C887 C882 104(10) . . ? C889 C887 C892 101(9) . . ? C886 C887 C892 164(9) . . ? C894 C887 C892 93(8) . . ? C891 C887 C892 32(5) . . ? C882 C887 C892 136(9) . . ? C889 C887 C888 137(10) . . ? C886 C887 C888 74(8) . . ? C894 C887 C888 34(7) . . ? C891 C887 C888 89(7) . . ? C882 C887 C888 28(7) . . ? C892 C887 C888 121(7) . . ? C881 C888 C882 90(10) . . ? C881 C888 C890 124(10) . . ? C882 C888 C890 86(10) . . ? C881 C888 C894 148(10) . . ? C882 C888 C894 58(10) . . ? C890 C888 C894 60(9) . . ? C881 C888 C885 55(10) . . ? C882 C888 C885 105(10) . . ? C890 C888 C885 72(9) . . ? C894 C888 C885 129(10) . . ? C881 C888 C884 97(10) . . ? C882 C888 C884 112(10) . . ? C890 C888 C884 36(8) . . ? C894 C888 C884 96(10) . . ? C885 C888 C884 42(7) . . ? C881 C888 C887 124(10) . . ? C882 C888 C887 49(10) . . ? C890 C888 C887 94(10) . . ? C894 C888 C887 34(7) . . ? C885 C888 C887 152(9) . . ? C884 C888 C887 130(10) . . ? C881 C888 C886 90(10) . . ? C882 C888 C886 32(10) . . ? C890 C888 C886 112(10) . . ? C894 C888 C886 62(8) . . ? C885 C888 C886 130(9) . . ? C884 C888 C886 143(9) . . ? C887 C888 C886 34(4) . . ? C887 C889 C886 68(9) . . ? C884 C890 C888 106(10) . . ? C884 C890 C894 168(10) . . ? C888 C890 C894 66(10) . . ? C884 C890 C883 59(10) . . ? C888 C890 C883 140(10) . . ? C894 C890 C883 121(10) . . ? C884 C890 C882 132(10) . . ? C888 C890 C882 44(8) . . ? C894 C890 C882 48(8) . . ? C883 C890 C882 169(10) . . ? C884 C890 C885 50(10) . . ? C888 C890 C885 64(8) . . ? C894 C890 C885 126(10) . . ? C883 C890 C885 109(9) . . ? C882 C890 C885 82(9) . . ? C884 C890 C895 121(10) . . ? C888 C890 C895 108(10) . . ? C894 C890 C895 57(7) . . ? C883 C890 C895 63(6) . . ? C882 C890 C895 106(9) . . ? C885 C890 C895 159(7) . . ? C884 C890 C881 90(10) . . ? C888 C890 C881 24(7) . . ? C894 C890 C881 85(9) . . ? C883 C890 C881 141(8) . . ? C882 C890 C881 48(8) . . ? C885 C890 C881 42(5) . . ? C895 C890 C881 132(9) . . ? C892 C891 C895 134(10) . . ? C892 C891 C894 159(10) . . ? C895 C891 C894 66(8) . . ? C892 C891 C887 106(10) . . ? C895 C891 C887 120(9) . . ? C894 C891 C887 55(6) . . ? C891 C892 C887 42(6) . . ? C882 C894 C890 79(10) . . ? C882 C894 C888 50(10) . . ? C890 C894 C888 54(8) . . ? C882 C894 C887 84(10) . . ? C890 C894 C887 163(10) . . ? C888 C894 C887 111(10) . . ? C882 C894 C891 149(10) . . ? C890 C894 C891 132(10) . . ? C888 C894 C891 147(10) . . ? C887 C894 C891 65(8) . . ? C882 C894 C895 156(10) . . ? C890 C894 C895 78(9) . . ? C888 C894 C895 115(10) . . ? C887 C894 C895 119(10) . . ? C891 C894 C895 55(6) . . ? C882 C894 C886 45(10) . . ? C890 C894 C886 123(10) . . ? C888 C894 C886 81(9) . . ? C887 C894 C886 40(6) . . ? C891 C894 C886 104(9) . . ? C895 C894 C886 159(10) . . ? C882 C894 C881 37(10) . . ? C890 C894 C881 59(8) . . ? C888 C894 C881 13(7) . . ? C887 C894 C881 105(9) . . ? C891 C894 C881 155(9) . . ? C895 C894 C881 127(9) . . ? C886 C894 C881 70(6) . . ? C891 C895 C894 60(7) . . ? C891 C895 C883 155(9) . . ? C894 C895 C883 95(7) . . ? C891 C895 C890 105(8) . . ? C894 C895 C890 45(6) . . ? C883 C895 C890 50(5) . . ? C996 C991 C992 128(9) . . ? C996 C991 C993 121(9) . . ? C992 C991 C993 107(7) . . ? C993 C992 C991 125(7) 3_655 . ? C993 C992 C995 125(7) 3_655 . ? C991 C992 C995 108(6) . . ? C992 C993 C997 118(8) 3_655 . ? C992 C993 C991 124(8) 3_655 . ? C997 C993 C991 117(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Au P1 C131 -96.9(12) . . . . ? P2 Au P1 C111 19.2(13) . . . . ? P2 Au P1 C121 135.2(11) . . . . ? C131 P1 C111 C112 72.9(17) . . . . ? C121 P1 C111 C112 -171.5(15) . . . . ? Au P1 C111 C112 -49.6(15) . . . . ? C131 P1 C111 C116 -104.6(17) . . . . ? C121 P1 C111 C116 10.9(17) . . . . ? Au P1 C111 C116 132.9(15) . . . . ? C116 C111 C112 C113 -1(3) . . . . ? P1 C111 C112 C113 -178.3(17) . . . . ? C111 C112 C113 C114 -1(3) . . . . ? C112 C113 C114 C115 4(4) . . . . ? C113 C114 C115 C116 -5(3) . . . . ? C112 C111 C116 C115 0(3) . . . . ? P1 C111 C116 C115 177.0(14) . . . . ? C114 C115 C116 C111 3(3) . . . . ? C131 P1 C121 C126 -156.6(17) . . . . ? C111 P1 C121 C126 90.5(17) . . . . ? Au P1 C121 C126 -25.8(19) . . . . ? C131 P1 C121 C122 26(2) . . . . ? C111 P1 C121 C122 -86.9(18) . . . . ? Au P1 C121 C122 156.8(15) . . . . ? C126 C121 C122 C123 -2(3) . . . . ? P1 C121 C122 C123 174.9(16) . . . . ? C121 C122 C123 C124 0(3) . . . . ? C122 C123 C124 C125 0(3) . . . . ? C123 C124 C125 C126 3(3) . . . . ? C122 C121 C126 C125 5(3) . . . . ? P1 C121 C126 C125 -172.1(17) . . . . ? C124 C125 C126 C121 -6(3) . . . . ? C111 P1 C131 C132 24(2) . . . . ? C121 P1 C131 C132 -89(2) . . . . ? Au P1 C131 C132 140.6(17) . . . . ? C111 P1 C131 C136 -149.0(18) . . . . ? C121 P1 C131 C136 97.9(18) . . . . ? Au P1 C131 C136 -32.6(19) . . . . ? C136 C131 C132 C133 -3(3) . . . . ? P1 C131 C132 C133 -176.9(16) . . . . ? C131 C132 C133 C134 3(3) . . . . ? C132 C133 C134 C135 -2(3) . . . . ? C133 C134 C135 C136 1(4) . . . . ? C134 C135 C136 C131 -1(4) . . . . ? C132 C131 C136 C135 2(3) . . . . ? P1 C131 C136 C135 176.2(17) . . . . ? P1 Au P2 C211 -90.5(12) . . . . ? P1 Au P2 C231 147.0(11) . . . . ? P1 Au P2 C221 26.9(14) . . . . ? C231 P2 C211 C212 78.3(16) . . . . ? C221 P2 C211 C212 -167.8(14) . . . . ? Au P2 C211 C212 -50.7(16) . . . . ? C231 P2 C211 C216 -104.9(18) . . . . ? C221 P2 C211 C216 9(2) . . . . ? Au P2 C211 C216 126.0(16) . . . . ? C216 C211 C212 C213 5(3) . . . . ? P2 C211 C212 C213 -177.7(14) . . . . ? C211 C212 C213 C214 -4(3) . . . . ? C212 C213 C214 C215 1(3) . . . . ? C213 C214 C215 C216 1(3) . . . . ? C214 C215 C216 C211 0(3) . . . . ? C212 C211 C216 C215 -3(3) . . . . ? P2 C211 C216 C215 -179.9(16) . . . . ? C211 P2 C221 C222 65.3(17) . . . . ? C231 P2 C221 C222 178.6(16) . . . . ? Au P2 C221 C222 -54.5(16) . . . . ? C211 P2 C221 C226 -120.3(15) . . . . ? C231 P2 C221 C226 -7.1(17) . . . . ? Au P2 C221 C226 119.9(14) . . . . ? C226 C221 C222 C223 -1(3) . . . . ? P2 C221 C222 C223 173.4(16) . . . . ? C221 C222 C223 C224 3(3) . . . . ? C222 C223 C224 C225 -5(3) . . . . ? C223 C224 C225 C226 5(3) . . . . ? C224 C225 C226 C221 -4(3) . . . . ? C222 C221 C226 C225 1(3) . . . . ? P2 C221 C226 C225 -172.9(13) . . . . ? C211 P2 C231 C236 42(2) . . . . ? C221 P2 C231 C236 -73(2) . . . . ? Au P2 C231 C236 167.0(17) . . . . ? C211 P2 C231 C232 -131.7(17) . . . . ? C221 P2 C231 C232 113.8(17) . . . . ? Au P2 C231 C232 -6.5(19) . . . . ? C236 C231 C232 C233 2(3) . . . . ? P2 C231 C232 C233 176.2(17) . . . . ? C231 C232 C233 C234 1(4) . . . . ? C232 C233 C234 C235 -1(4) . . . . ? C233 C234 C235 C236 -1(4) . . . . ? C232 C231 C236 C235 -5(4) . . . . ? P2 C231 C236 C235 -179(2) . . . . ? C234 C235 C236 C231 5(4) . . . . ? C39 N31 C32 O32 -179.4(17) . . . . ? C39 N31 C32 C33 -3(2) . . . . ? N31 C32 O32 B3 -5(3) . . . . ? C33 C32 O32 B3 179.4(15) . . . . ? O32 C32 C33 C38 -179.1(15) . . . . ? N31 C32 C33 C38 4.1(19) . . . . ? O32 C32 C33 C34 -4(3) . . . . ? N31 C32 C33 C34 178.8(16) . . . . ? C38 C33 C34 F34 179.1(14) . . . . ? C32 C33 C34 F34 5(3) . . . . ? C38 C33 C34 C35 0(2) . . . . ? C32 C33 C34 C35 -174.5(17) . . . . ? F34 C34 C35 F35 3(2) . . . . ? C33 C34 C35 F35 -178.0(14) . . . . ? F34 C34 C35 C36 -178.2(14) . . . . ? C33 C34 C35 C36 1(2) . . . . ? F35 C35 C36 F36 2(2) . . . . ? C34 C35 C36 F36 -176.9(15) . . . . ? F35 C35 C36 C37 175.6(15) . . . . ? C34 C35 C36 C37 -4(2) . . . . ? F36 C36 C37 F37 -7(2) . . . . ? C35 C36 C37 F37 -179.5(14) . . . . ? F36 C36 C37 C38 177.9(15) . . . . ? C35 C36 C37 C38 5(2) . . . . ? C34 C33 C38 C37 2(2) . . . . ? C32 C33 C38 C37 177.2(15) . . . . ? C34 C33 C38 C39 -178.8(15) . . . . ? C32 C33 C38 C39 -3.4(17) . . . . ? F37 C37 C38 C33 -179.2(14) . . . . ? C36 C37 C38 C33 -4(2) . . . . ? F37 C37 C38 C39 2(3) . . . . ? C36 C37 C38 C39 176.8(18) . . . . ? C32 N31 C39 O39 177.4(17) . . . . ? C32 N31 C39 C38 1(2) . . . . ? C33 C38 C39 O39 -175.1(15) . . . . ? C37 C38 C39 O39 4(3) . . . . ? C33 C38 C39 N31 1.7(19) . . . . ? C37 C38 C39 N31 -179.0(17) . . . . ? N31 C39 O39 B9 -1(3) . . . . ? C38 C39 O39 B9 175.0(14) . . . . ? C32 O32 B3 C61 -43(2) . . . . ? C32 O32 B3 C41 -163.7(15) . . . . ? C32 O32 B3 C51 83.5(19) . . . . ? O32 B3 C41 C42 -50(2) . . . . ? C61 B3 C41 C42 -164.7(18) . . . . ? C51 B3 C41 C42 63(2) . . . . ? O32 B3 C41 C46 123.3(19) . . . . ? C61 B3 C41 C46 9(3) . . . . ? C51 B3 C41 C46 -123.3(19) . . . . ? C46 C41 C42 C43 -2(3) . . . . ? B3 C41 C42 C43 172(2) . . . . ? C46 C41 C42 F42 178.5(16) . . . . ? B3 C41 C42 F42 -7(3) . . . . ? F42 C42 C43 F43 -2(3) . . . . ? C41 C42 C43 F43 178.4(19) . . . . ? F42 C42 C43 C44 178.5(19) . . . . ? C41 C42 C43 C44 -1(4) . . . . ? F43 C43 C44 F44 1(3) . . . . ? C42 C43 C44 F44 -179.6(19) . . . . ? F43 C43 C44 C45 -176.5(18) . . . . ? C42 C43 C44 C45 3(3) . . . . ? F44 C44 C45 F45 2(3) . . . . ? C43 C44 C45 F45 179.2(18) . . . . ? F44 C44 C45 C46 -179.2(18) . . . . ? C43 C44 C45 C46 -2(3) . . . . ? F45 C45 C46 F46 -3(3) . . . . ? C44 C45 C46 F46 178.0(16) . . . . ? F45 C45 C46 C41 177.7(17) . . . . ? C44 C45 C46 C41 -1(3) . . . . ? C42 C41 C46 F46 -176.2(17) . . . . ? B3 C41 C46 F46 10(3) . . . . ? C42 C41 C46 C45 3(3) . . . . ? B3 C41 C46 C45 -171.1(18) . . . . ? O32 B3 C51 C52 168.6(14) . . . . ? C61 B3 C51 C52 -70(2) . . . . ? C41 B3 C51 C52 62(2) . . . . ? O32 B3 C51 C56 -17(2) . . . . ? C61 B3 C51 C56 105(2) . . . . ? C41 B3 C51 C56 -122.9(19) . . . . ? C56 C51 C52 C53 0(2) . . . . ? B3 C51 C52 C53 175.8(16) . . . . ? C56 C51 C52 F52 -177.7(14) . . . . ? B3 C51 C52 F52 -2(2) . . . . ? C51 C52 C53 F53 180.0(15) . . . . ? F52 C52 C53 F53 -2(2) . . . . ? C51 C52 C53 C54 2(3) . . . . ? F52 C52 C53 C54 179.9(14) . . . . ? F53 C53 C54 F54 2(2) . . . . ? C52 C53 C54 F54 179.7(15) . . . . ? F53 C53 C54 C55 -179.7(15) . . . . ? C52 C53 C54 C55 -2(3) . . . . ? F54 C54 C55 F55 -2(2) . . . . ? C53 C54 C55 F55 179.6(16) . . . . ? F54 C54 C55 C56 177.9(15) . . . . ? C53 C54 C55 C56 -1(3) . . . . ? F55 C55 C56 F56 1(2) . . . . ? C54 C55 C56 F56 -179.0(14) . . . . ? F55 C55 C56 C51 -177.1(16) . . . . ? C54 C55 C56 C51 3(3) . . . . ? C52 C51 C56 C55 -3(3) . . . . ? B3 C51 C56 C55 -178.0(16) . . . . ? C52 C51 C56 F56 179.4(15) . . . . ? B3 C51 C56 F56 4(3) . . . . ? O32 B3 C61 C62 -57(2) . . . . ? C41 B3 C61 C62 52(2) . . . . ? C51 B3 C61 C62 -179.8(17) . . . . ? O32 B3 C61 C66 133.3(17) . . . . ? C41 B3 C61 C66 -117.7(19) . . . . ? C51 B3 C61 C66 11(3) . . . . ? C66 C61 C62 C63 -1(3) . . . . ? B3 C61 C62 C63 -171.7(19) . . . . ? C66 C61 C62 F62 -179.9(15) . . . . ? B3 C61 C62 F62 9(3) . . . . ? C61 C62 C63 F63 178.3(18) . . . . ? F62 C62 C63 F63 -3(3) . . . . ? C61 C62 C63 C64 0(3) . . . . ? F62 C62 C63 C64 178.6(14) . . . . ? C62 C63 C64 F64 -179.7(16) . . . . ? F63 C63 C64 F64 2(2) . . . . ? C62 C63 C64 C65 0(3) . . . . ? F63 C63 C64 C65 -178.8(15) . . . . ? F64 C64 C65 F65 -1(2) . . . . ? C63 C64 C65 F65 179.6(15) . . . . ? F64 C64 C65 C66 -178.4(16) . . . . ? C63 C64 C65 C66 2(2) . . . . ? F65 C65 C66 F66 2(3) . . . . ? C64 C65 C66 F66 179.8(15) . . . . ? F65 C65 C66 C61 178.9(17) . . . . ? C64 C65 C66 C61 -4(3) . . . . ? C62 C61 C66 F66 179.5(17) . . . . ? B3 C61 C66 F66 -10(3) . . . . ? C62 C61 C66 C65 3(3) . . . . ? B3 C61 C66 C65 173.4(18) . . . . ? C39 O39 B9 C81 -50(2) . . . . ? C39 O39 B9 C71 78(2) . . . . ? C39 O39 B9 C91 -170.2(15) . . . . ? O39 B9 C71 C76 -14(3) . . . . ? C81 B9 C71 C76 110(2) . . . . ? C91 B9 C71 C76 -122(2) . . . . ? O39 B9 C71 C72 169.9(15) . . . . ? C81 B9 C71 C72 -67(2) . . . . ? C91 B9 C71 C72 61(2) . . . . ? C76 C71 C72 C73 0(3) . . . . ? B9 C71 C72 C73 177.5(18) . . . . ? C76 C71 C72 F72 -179.5(15) . . . . ? B9 C71 C72 F72 -2(2) . . . . ? F72 C72 C73 F73 1(3) . . . . ? C71 C72 C73 F73 -178.7(17) . . . . ? F72 C72 C73 C74 178.2(16) . . . . ? C71 C72 C73 C74 -2(3) . . . . ? C72 C73 C74 C75 3(3) . . . . ? F73 C73 C74 C75 179.9(17) . . . . ? C72 C73 C74 F74 179.3(17) . . . . ? F73 C73 C74 F74 -4(3) . . . . ? F74 C74 C75 F75 2(3) . . . . ? C73 C74 C75 F75 177.9(16) . . . . ? F74 C74 C75 C76 -179.1(16) . . . . ? C73 C74 C75 C76 -3(3) . . . . ? C72 C71 C76 F76 177.0(16) . . . . ? B9 C71 C76 F76 0(3) . . . . ? C72 C71 C76 C75 0(3) . . . . ? B9 C71 C76 C75 -177.1(17) . . . . ? F75 C75 C76 F76 3(2) . . . . ? C74 C75 C76 F76 -176.0(16) . . . . ? F75 C75 C76 C71 -179.1(17) . . . . ? C74 C75 C76 C71 2(3) . . . . ? O39 B9 C81 C86 -58(2) . . . . ? C71 B9 C81 C86 176.9(17) . . . . ? C91 B9 C81 C86 53(2) . . . . ? O39 B9 C81 C82 125.2(18) . . . . ? C71 B9 C81 C82 0(2) . . . . ? C91 B9 C81 C82 -123.3(19) . . . . ? C86 C81 C82 C83 3(3) . . . . ? B9 C81 C82 C83 179.7(17) . . . . ? C86 C81 C82 F82 176.8(16) . . . . ? B9 C81 C82 F82 -7(3) . . . . ? F82 C82 C83 F83 6(3) . . . . ? C81 C82 C83 F83 179.6(16) . . . . ? F82 C82 C83 C84 -178.9(16) . . . . ? C81 C82 C83 C84 -5(3) . . . . ? C82 C83 C84 F84 -176.1(17) . . . . ? F83 C83 C84 F84 0(2) . . . . ? C82 C83 C84 C85 4(3) . . . . ? F83 C83 C84 C85 179.8(15) . . . . ? F84 C84 C85 C86 178.4(16) . . . . ? C83 C84 C85 C86 -2(3) . . . . ? F84 C84 C85 F85 2(2) . . . . ? C83 C84 C85 F85 -178.6(15) . . . . ? F85 C85 C86 F86 -4(3) . . . . ? C84 C85 C86 F86 179.5(15) . . . . ? F85 C85 C86 C81 176.8(17) . . . . ? C84 C85 C86 C81 0(3) . . . . ? C82 C81 C86 C85 -1(3) . . . . ? B9 C81 C86 C85 -177.5(17) . . . . ? C82 C81 C86 F86 -179.9(15) . . . . ? B9 C81 C86 F86 3(3) . . . . ? O39 B9 C91 C96 126.3(19) . . . . ? C81 B9 C91 C96 11(3) . . . . ? C71 B9 C91 C96 -119(2) . . . . ? O39 B9 C91 C92 -49.3(19) . . . . ? C81 B9 C91 C92 -164.8(17) . . . . ? C71 B9 C91 C92 66(2) . . . . ? C96 C91 C92 F92 178.3(16) . . . . ? B9 C91 C92 F92 -5(3) . . . . ? C96 C91 C92 C93 0(3) . . . . ? B9 C91 C92 C93 175.9(18) . . . . ? F92 C92 C93 C94 -177.9(19) . . . . ? C91 C92 C93 C94 1(3) . . . . ? F92 C92 C93 F93 -2(3) . . . . ? C91 C92 C93 F93 177.1(17) . . . . ? C92 C93 C94 F94 180(2) . . . . ? F93 C93 C94 F94 3(3) . . . . ? C92 C93 C94 C95 0(3) . . . . ? F93 C93 C94 C95 -176.8(17) . . . . ? F94 C94 C95 F95 3(3) . . . . ? C93 C94 C95 F95 -176.5(19) . . . . ? F94 C94 C95 C96 179.5(17) . . . . ? C93 C94 C95 C96 0(3) . . . . ? C92 C91 C96 F96 -177.8(16) . . . . ? B9 C91 C96 F96 6(3) . . . . ? C92 C91 C96 C95 0(3) . . . . ? B9 C91 C96 C95 -176.2(18) . . . . ? F95 C95 C96 F96 -6(3) . . . . ? C94 C95 C96 F96 178.2(16) . . . . ? F95 C95 C96 C91 176.9(18) . . . . ? C94 C95 C96 C91 1(3) . . . . ? C885 C881 C882 C888 -76(16) . . . . ? C890 C881 C882 C888 -40(14) . . . . ? C894 C881 C882 C888 1(18) . . . . ? C884 C881 C882 C888 -52(14) . . . . ? C888 C881 C882 C894 -1(18) . . . . ? C885 C881 C882 C894 -76(18) . . . . ? C890 C881 C882 C894 -41(12) . . . . ? C884 C881 C882 C894 -53(16) . . . . ? C888 C881 C882 C886 -114(20) . . . . ? C885 C881 C882 C886 170(13) . . . . ? C890 C881 C882 C886 -154(17) . . . . ? C894 C881 C882 C886 -113(21) . . . . ? C884 C881 C882 C886 -166(14) . . . . ? C888 C881 C882 C890 40(14) . . . . ? C885 C881 C882 C890 -36(11) . . . . ? C894 C881 C882 C890 41(12) . . . . ? C884 C881 C882 C890 -12(8) . . . . ? C888 C881 C882 C887 -59(21) . . . . ? C885 C881 C882 C887 -134(17) . . . . ? C890 C881 C882 C887 -99(19) . . . . ? C894 C881 C882 C887 -58(15) . . . . ? C884 C881 C882 C887 -111(18) . . . . ? C888 C881 C882 C885 76(16) . . . . ? C890 C881 C882 C885 36(11) . . . . ? C894 C881 C882 C885 76(18) . . . . ? C884 C881 C882 C885 23(9) . . . . ? C895 C883 C884 C890 15(13) . . . . ? C890 C883 C884 C885 -21(35) . . . . ? C895 C883 C884 C885 -6(45) . . . . ? C890 C883 C884 C888 -24(7) . . . . ? C895 C883 C884 C888 -9(13) . . . . ? C890 C883 C884 C881 -25(9) . . . . ? C895 C883 C884 C881 -10(17) . . . . ? C888 C881 C884 C890 -26(14) . . . . ? C885 C881 C884 C890 148(21) . . . . ? C882 C881 C884 C890 19(13) . . . . ? C894 C881 C884 C890 -7(9) . . . . ? C888 C881 C884 C885 -174(23) . . . . ? C882 C881 C884 C885 -129(18) . . . . ? C890 C881 C884 C885 -148(21) . . . . ? C894 C881 C884 C885 -155(17) . . . . ? C888 C881 C884 C883 2(18) . . . . ? C885 C881 C884 C883 176(24) . . . . ? C882 C881 C884 C883 47(17) . . . . ? C890 C881 C884 C883 28(11) . . . . ? C894 C881 C884 C883 22(13) . . . . ? C885 C881 C884 C888 174(23) . . . . ? C882 C881 C884 C888 45(12) . . . . ? C890 C881 C884 C888 26(14) . . . . ? C894 C881 C884 C888 19(12) . . . . ? C890 C884 C885 C881 -27(18) . . . . ? C883 C884 C885 C881 -7(49) . . . . ? C888 C884 C885 C881 -3(12) . . . . ? C890 C884 C885 C888 -24(11) . . . . ? C883 C884 C885 C888 -4(41) . . . . ? C881 C884 C885 C888 3(12) . . . . ? C883 C884 C885 C890 20(34) . . . . ? C888 C884 C885 C890 24(11) . . . . ? C881 C884 C885 C890 27(18) . . . . ? C890 C884 C885 C882 4(12) . . . . ? C883 C884 C885 C882 24(42) . . . . ? C888 C884 C885 C882 29(6) . . . . ? C881 C884 C885 C882 32(11) . . . . ? C888 C881 C885 C884 5(20) . . . . ? C882 C881 C885 C884 52(18) . . . . ? C890 C881 C885 C884 19(13) . . . . ? C894 C881 C885 C884 23(15) . . . . ? C882 C881 C885 C888 47(11) . . . . ? C890 C881 C885 C888 14(12) . . . . ? C894 C881 C885 C888 18(10) . . . . ? C884 C881 C885 C888 -5(20) . . . . ? C888 C881 C885 C890 -14(12) . . . . ? C882 C881 C885 C890 33(11) . . . . ? C894 C881 C885 C890 4(6) . . . . ? C884 C881 C885 C890 -19(13) . . . . ? C888 C881 C885 C882 -47(11) . . . . ? C890 C881 C885 C882 -33(11) . . . . ? C894 C881 C885 C882 -29(9) . . . . ? C884 C881 C885 C882 -52(18) . . . . ? C888 C882 C885 C884 -73(17) . . . . ? C894 C882 C885 C884 -22(15) . . . . ? C886 C882 C885 C884 -155(26) . . . . ? C881 C882 C885 C884 -137(16) . . . . ? C890 C882 C885 C884 -4(11) . . . . ? C887 C882 C885 C884 -53(22) . . . . ? C888 C882 C885 C881 64(14) . . . . ? C894 C882 C885 C881 114(17) . . . . ? C886 C882 C885 C881 -18(23) . . . . ? C890 C882 C885 C881 133(15) . . . . ? C887 C882 C885 C881 84(21) . . . . ? C894 C882 C885 C888 51(15) . . . . ? C886 C882 C885 C888 -82(28) . . . . ? C881 C882 C885 C888 -64(14) . . . . ? C890 C882 C885 C888 69(15) . . . . ? C887 C882 C885 C888 20(17) . . . . ? C888 C882 C885 C890 -69(15) . . . . ? C894 C882 C885 C890 -18(9) . . . . ? C886 C882 C885 C890 -151(29) . . . . ? C881 C882 C885 C890 -133(15) . . . . ? C887 C882 C885 C890 -49(18) . . . . ? C888 C882 C886 C889 85(23) . . . . ? C894 C882 C886 C889 11(19) . . . . ? C881 C882 C886 C889 132(14) . . . . ? C890 C882 C886 C889 17(37) . . . . ? C887 C882 C886 C889 11(10) . . . . ? C885 C882 C886 C889 144(21) . . . . ? C888 C882 C886 C887 75(21) . . . . ? C894 C882 C886 C887 0(12) . . . . ? C881 C882 C886 C887 121(15) . . . . ? C890 C882 C886 C887 7(30) . . . . ? C885 C882 C886 C887 133(26) . . . . ? C888 C882 C886 C894 74(20) . . . . ? C881 C882 C886 C894 121(21) . . . . ? C890 C882 C886 C894 6(21) . . . . ? C887 C882 C886 C894 0(12) . . . . ? C885 C882 C886 C894 133(33) . . . . ? C894 C882 C886 C888 -74(20) . . . . ? C881 C882 C886 C888 47(15) . . . . ? C890 C882 C886 C888 -68(30) . . . . ? C887 C882 C886 C888 -75(21) . . . . ? C885 C882 C886 C888 58(24) . . . . ? C882 C886 C887 C889 168(12) . . . . ? C894 C886 C887 C889 168(11) . . . . ? C888 C886 C887 C889 -169(9) . . . . ? C889 C886 C887 C894 -168(11) . . . . ? C882 C886 C887 C894 0(11) . . . . ? C888 C886 C887 C894 23(7) . . . . ? C889 C886 C887 C891 -153(27) . . . . ? C882 C886 C887 C891 15(26) . . . . ? C894 C886 C887 C891 15(21) . . . . ? C888 C886 C887 C891 39(24) . . . . ? C889 C886 C887 C882 -168(12) . . . . ? C894 C886 C887 C882 0(11) . . . . ? C888 C886 C887 C882 24(8) . . . . ? C889 C886 C887 C892 -32(30) . . . . ? C882 C886 C887 C892 136(31) . . . . ? C894 C886 C887 C892 136(35) . . . . ? C888 C886 C887 C892 160(32) . . . . ? C889 C886 C887 C888 169(9) . . . . ? C882 C886 C887 C888 -24(8) . . . . ? C894 C886 C887 C888 -23(7) . . . . ? C888 C882 C887 C889 -138(15) . . . . ? C894 C882 C887 C889 168(14) . . . . ? C886 C882 C887 C889 -13(12) . . . . ? C881 C882 C887 C889 -103(20) . . . . ? C890 C882 C887 C889 170(11) . . . . ? C885 C882 C887 C889 -153(17) . . . . ? C888 C882 C887 C886 -125(17) . . . . ? C894 C882 C887 C886 -179(15) . . . . ? C881 C882 C887 C886 -90(19) . . . . ? C890 C882 C887 C886 -177(14) . . . . ? C885 C882 C887 C886 -140(22) . . . . ? C888 C882 C887 C894 54(15) . . . . ? C886 C882 C887 C894 179(15) . . . . ? C881 C882 C887 C894 89(21) . . . . ? C890 C882 C887 C894 3(9) . . . . ? C885 C882 C887 C894 39(17) . . . . ? C888 C882 C887 C891 60(16) . . . . ? C894 C882 C887 C891 6(12) . . . . ? C886 C882 C887 C891 -174(10) . . . . ? C881 C882 C887 C891 95(19) . . . . ? C890 C882 C887 C891 9(12) . . . . ? C885 C882 C887 C891 46(21) . . . . ? C888 C882 C887 C892 70(18) . . . . ? C894 C882 C887 C892 16(15) . . . . ? C886 C882 C887 C892 -164(11) . . . . ? C881 C882 C887 C892 105(18) . . . . ? C890 C882 C887 C892 19(17) . . . . ? C885 C882 C887 C892 56(23) . . . . ? C894 C882 C887 C888 -54(15) . . . . ? C886 C882 C887 C888 125(17) . . . . ? C881 C882 C887 C888 35(14) . . . . ? C890 C882 C887 C888 -51(13) . . . . ? C885 C882 C887 C888 -15(12) . . . . ? C885 C881 C888 C882 109(14) . . . . ? C890 C881 C888 C882 86(20) . . . . ? C894 C881 C888 C882 -1(27) . . . . ? C884 C881 C888 C882 112(15) . . . . ? C885 C881 C888 C890 23(20) . . . . ? C882 C881 C888 C890 -86(20) . . . . ? C894 C881 C888 C890 -87(33) . . . . ? C884 C881 C888 C890 26(14) . . . . ? C885 C881 C888 C894 110(31) . . . . ? C882 C881 C888 C894 1(27) . . . . ? C890 C881 C888 C894 87(33) . . . . ? C884 C881 C888 C894 113(33) . . . . ? C882 C881 C888 C885 -109(14) . . . . ? C890 C881 C888 C885 -23(20) . . . . ? C894 C881 C888 C885 -110(31) . . . . ? C884 C881 C888 C885 3(12) . . . . ? C885 C881 C888 C884 -3(12) . . . . ? C882 C881 C888 C884 -112(15) . . . . ? C890 C881 C888 C884 -26(14) . . . . ? C894 C881 C888 C884 -113(33) . . . . ? C885 C881 C888 C887 146(11) . . . . ? C882 C881 C888 C887 37(12) . . . . ? C890 C881 C888 C887 123(24) . . . . ? C894 C881 C888 C887 36(24) . . . . ? C884 C881 C888 C887 149(17) . . . . ? C885 C881 C888 C886 141(8) . . . . ? C882 C881 C888 C886 32(10) . . . . ? C890 C881 C888 C886 117(18) . . . . ? C894 C881 C888 C886 31(29) . . . . ? C884 C881 C888 C886 144(10) . . . . ? C894 C882 C888 C881 179(17) . . . . ? C886 C882 C888 C881 91(21) . . . . ? C890 C882 C888 C881 -124(16) . . . . ? C887 C882 C888 C881 138(15) . . . . ? C885 C882 C888 C881 -54(11) . . . . ? C894 C882 C888 C890 -56(10) . . . . ? C886 C882 C888 C890 -145(18) . . . . ? C881 C882 C888 C890 124(16) . . . . ? C887 C882 C888 C890 -98(11) . . . . ? C885 C882 C888 C890 71(11) . . . . ? C886 C882 C888 C894 -89(19) . . . . ? C881 C882 C888 C894 -179(17) . . . . ? C890 C882 C888 C894 56(10) . . . . ? C887 C882 C888 C894 -42(9) . . . . ? C885 C882 C888 C894 127(13) . . . . ? C894 C882 C888 C885 -127(13) . . . . ? C886 C882 C888 C885 144(15) . . . . ? C881 C882 C888 C885 54(11) . . . . ? C890 C882 C888 C885 -71(10) . . . . ? C887 C882 C888 C885 -169(10) . . . . ? C894 C882 C888 C884 -83(15) . . . . ? C886 C882 C888 C884 -172(14) . . . . ? C881 C882 C888 C884 98(16) . . . . ? C890 C882 C888 C884 -26(10) . . . . ? C887 C882 C888 C884 -124(12) . . . . ? C885 C882 C888 C884 44(9) . . . . ? C894 C882 C888 C887 42(9) . . . . ? C886 C882 C888 C887 -47(14) . . . . ? C881 C882 C888 C887 -138(15) . . . . ? C890 C882 C888 C887 98(11) . . . . ? C885 C882 C888 C887 169(10) . . . . ? C894 C882 C888 C886 89(19) . . . . ? C881 C882 C888 C886 -91(21) . . . . ? C890 C882 C888 C886 145(18) . . . . ? C887 C882 C888 C886 47(14) . . . . ? C885 C882 C888 C886 -144(15) . . . . ? C884 C885 C888 C881 -176(17) . . . . ? C890 C885 C888 C881 160(18) . . . . ? C882 C885 C888 C881 79(17) . . . . ? C884 C885 C888 C882 106(17) . . . . ? C881 C885 C888 C882 -79(17) . . . . ? C890 C885 C888 C882 81(15) . . . . ? C884 C885 C888 C890 24(11) . . . . ? C881 C885 C888 C890 -160(18) . . . . ? C882 C885 C888 C890 -81(15) . . . . ? C884 C885 C888 C894 45(17) . . . . ? C881 C885 C888 C894 -140(22) . . . . ? C890 C885 C888 C894 20(12) . . . . ? C882 C885 C888 C894 -61(15) . . . . ? C881 C885 C888 C884 176(17) . . . . ? C890 C885 C888 C884 -24(11) . . . . ? C882 C885 C888 C884 -106(17) . . . . ? C884 C885 C888 C887 87(24) . . . . ? C881 C885 C888 C887 -97(25) . . . . ? C890 C885 C888 C887 63(21) . . . . ? C882 C885 C888 C887 -19(16) . . . . ? C884 C885 C888 C886 129(14) . . . . ? C881 C885 C888 C886 -55(14) . . . . ? C890 C885 C888 C886 105(14) . . . . ? C882 C885 C888 C886 23(11) . . . . ? C890 C884 C888 C881 142(20) . . . . ? C885 C884 C888 C881 4(14) . . . . ? C883 C884 C888 C881 -178(15) . . . . ? C890 C884 C888 C882 49(19) . . . . ? C885 C884 C888 C882 -89(17) . . . . ? C883 C884 C888 C882 89(18) . . . . ? C881 C884 C888 C882 -93(18) . . . . ? C885 C884 C888 C890 -138(18) . . . . ? C883 C884 C888 C890 40(12) . . . . ? C881 C884 C888 C890 -142(20) . . . . ? C890 C884 C888 C894 -9(13) . . . . ? C885 C884 C888 C894 -147(13) . . . . ? C883 C884 C888 C894 32(13) . . . . ? C881 C884 C888 C894 -150(18) . . . . ? C890 C884 C888 C885 138(18) . . . . ? C883 C884 C888 C885 178(17) . . . . ? C881 C884 C888 C885 -4(14) . . . . ? C890 C884 C888 C887 -5(15) . . . . ? C885 C884 C888 C887 -143(12) . . . . ? C883 C884 C888 C887 36(16) . . . . ? C881 C884 C888 C887 -146(19) . . . . ? C890 C884 C888 C886 42(20) . . . . ? C885 C884 C888 C886 -96(17) . . . . ? C883 C884 C888 C886 82(18) . . . . ? C881 C884 C888 C886 -100(19) . . . . ? C889 C887 C888 C881 5(24) . . . . ? C886 C887 C888 C881 -10(17) . . . . ? C894 C887 C888 C881 -146(22) . . . . ? C891 C887 C888 C881 -177(17) . . . . ? C882 C887 C888 C881 -54(19) . . . . ? C892 C887 C888 C881 176(15) . . . . ? C889 C887 C888 C882 59(20) . . . . ? C886 C887 C888 C882 44(15) . . . . ? C894 C887 C888 C882 -92(17) . . . . ? C891 C887 C888 C882 -123(16) . . . . ? C892 C887 C888 C882 -130(16) . . . . ? C889 C887 C888 C890 141(14) . . . . ? C886 C887 C888 C890 126(11) . . . . ? C894 C887 C888 C890 -10(11) . . . . ? C891 C887 C888 C890 -41(9) . . . . ? C882 C887 C888 C890 82(16) . . . . ? C892 C887 C888 C890 -48(10) . . . . ? C889 C887 C888 C894 151(19) . . . . ? C886 C887 C888 C894 136(14) . . . . ? C891 C887 C888 C894 -31(11) . . . . ? C882 C887 C888 C894 92(17) . . . . ? C892 C887 C888 C894 -38(12) . . . . ? C889 C887 C888 C885 83(26) . . . . ? C886 C887 C888 C885 68(23) . . . . ? C894 C887 C888 C885 -68(23) . . . . ? C891 C887 C888 C885 -99(22) . . . . ? C882 C887 C888 C885 24(21) . . . . ? C892 C887 C888 C885 -106(22) . . . . ? C889 C887 C888 C884 144(15) . . . . ? C886 C887 C888 C884 129(12) . . . . ? C894 C887 C888 C884 -7(13) . . . . ? C891 C887 C888 C884 -38(12) . . . . ? C882 C887 C888 C884 85(18) . . . . ? C892 C887 C888 C884 -45(12) . . . . ? C889 C887 C888 C886 15(12) . . . . ? C894 C887 C888 C886 -136(14) . . . . ? C891 C887 C888 C886 -167(9) . . . . ? C882 C887 C888 C886 -44(15) . . . . ? C892 C887 C888 C886 -174(9) . . . . ? C889 C886 C888 C881 162(13) . . . . ? C887 C886 C888 C881 172(14) . . . . ? C882 C886 C888 C881 -89(23) . . . . ? C894 C886 C888 C881 -162(17) . . . . ? C889 C886 C888 C882 -108(23) . . . . ? C887 C886 C888 C882 -99(22) . . . . ? C894 C886 C888 C882 -73(21) . . . . ? C889 C886 C888 C890 -70(14) . . . . ? C887 C886 C888 C890 -61(11) . . . . ? C882 C886 C888 C890 38(20) . . . . ? C894 C886 C888 C890 -34(9) . . . . ? C889 C886 C888 C894 -36(11) . . . . ? C887 C886 C888 C894 -26(8) . . . . ? C882 C886 C888 C894 73(21) . . . . ? C889 C886 C888 C885 -155(12) . . . . ? C887 C886 C888 C885 -146(13) . . . . ? C882 C886 C888 C885 -47(21) . . . . ? C894 C886 C888 C885 -119(15) . . . . ? C889 C886 C888 C884 -95(18) . . . . ? C887 C886 C888 C884 -86(18) . . . . ? C882 C886 C888 C884 13(22) . . . . ? C894 C886 C888 C884 -60(17) . . . . ? C889 C886 C888 C887 -9(7) . . . . ? C882 C886 C888 C887 99(22) . . . . ? C894 C886 C888 C887 26(8) . . . . ? C894 C887 C889 C886 37(35) . . . . ? C891 C887 C889 C886 167(14) . . . . ? C882 C887 C889 C886 12(11) . . . . ? C892 C887 C889 C886 172(8) . . . . ? C888 C887 C889 C886 -16(13) . . . . ? C882 C886 C889 C887 -14(13) . . . . ? C894 C886 C889 C887 -8(7) . . . . ? C888 C886 C889 C887 12(10) . . . . ? C885 C884 C890 C888 33(14) . . . . ? C883 C884 C890 C888 -139(11) . . . . ? C881 C884 C890 C888 18(9) . . . . ? C885 C884 C890 C894 80(75) . . . . ? C883 C884 C890 C894 -91(73) . . . . ? C888 C884 C890 C894 47(70) . . . . ? C881 C884 C890 C894 65(73) . . . . ? C885 C884 C890 C883 172(14) . . . . ? C888 C884 C890 C883 139(11) . . . . ? C881 C884 C890 C883 156(8) . . . . ? C885 C884 C890 C882 -8(21) . . . . ? C883 C884 C890 C882 -180(15) . . . . ? C888 C884 C890 C882 -41(13) . . . . ? C881 C884 C890 C882 -23(14) . . . . ? C883 C884 C890 C885 -172(14) . . . . ? C888 C884 C890 C885 -33(14) . . . . ? C881 C884 C890 C885 -15(10) . . . . ? C885 C884 C890 C895 156(10) . . . . ? C883 C884 C890 C895 -16(13) . . . . ? C888 C884 C890 C895 123(16) . . . . ? C881 C884 C890 C895 141(12) . . . . ? C885 C884 C890 C881 15(10) . . . . ? C883 C884 C890 C881 -156(8) . . . . ? C888 C884 C890 C881 -18(9) . . . . ? C881 C888 C890 C884 -48(24) . . . . ? C882 C888 C890 C884 -135(17) . . . . ? C894 C888 C890 C884 170(15) . . . . ? C885 C888 C890 C884 -28(13) . . . . ? C887 C888 C890 C884 176(12) . . . . ? C886 C888 C890 C884 -154(12) . . . . ? C881 C888 C890 C894 142(22) . . . . ? C882 C888 C890 C894 54(11) . . . . ? C885 C888 C890 C894 162(10) . . . . ? C884 C888 C890 C894 -170(15) . . . . ? C887 C888 C890 C894 6(7) . . . . ? C886 C888 C890 C894 35(9) . . . . ? C881 C888 C890 C883 -109(22) . . . . ? C882 C888 C890 C883 164(17) . . . . ? C894 C888 C890 C883 109(17) . . . . ? C885 C888 C890 C883 -89(17) . . . . ? C884 C888 C890 C883 -61(17) . . . . ? C887 C888 C890 C883 116(16) . . . . ? C886 C888 C890 C883 145(14) . . . . ? C881 C888 C890 C882 87(21) . . . . ? C894 C888 C890 C882 -54(11) . . . . ? C885 C888 C890 C882 107(13) . . . . ? C884 C888 C890 C882 135(17) . . . . ? C887 C888 C890 C882 -48(11) . . . . ? C886 C888 C890 C882 -19(10) . . . . ? C881 C888 C890 C885 -20(18) . . . . ? C882 C888 C890 C885 -107(13) . . . . ? C894 C888 C890 C885 -162(10) . . . . ? C884 C888 C890 C885 28(13) . . . . ? C887 C888 C890 C885 -155(8) . . . . ? C886 C888 C890 C885 -126(10) . . . . ? C881 C888 C890 C895 -179(17) . . . . ? C882 C888 C890 C895 94(13) . . . . ? C894 C888 C890 C895 40(9) . . . . ? C885 C888 C890 C895 -159(8) . . . . ? C884 C888 C890 C895 -131(15) . . . . ? C887 C888 C890 C895 46(8) . . . . ? C886 C888 C890 C895 75(10) . . . . ? C882 C888 C890 C881 -87(21) . . . . ? C894 C888 C890 C881 -142(22) . . . . ? C885 C888 C890 C881 20(18) . . . . ? C884 C888 C890 C881 48(24) . . . . ? C887 C888 C890 C881 -136(22) . . . . ? C886 C888 C890 C881 -106(21) . . . . ? C895 C883 C890 C884 -165(13) . . . . ? C884 C883 C890 C888 78(20) . . . . ? C895 C883 C890 C888 -87(18) . . . . ? C884 C883 C890 C894 166(17) . . . . ? C895 C883 C890 C894 1(10) . . . . ? C884 C883 C890 C882 179(100) . . . . ? C895 C883 C890 C882 14(52) . . . . ? C884 C883 C890 C885 7(11) . . . . ? C895 C883 C890 C885 -158(8) . . . . ? C884 C883 C890 C895 165(13) . . . . ? C884 C883 C890 C881 40(15) . . . . ? C895 C883 C890 C881 -125(14) . . . . ? C888 C882 C890 C884 66(21) . . . . ? C894 C882 C890 C884 164(20) . . . . ? C886 C882 C890 C884 156(27) . . . . ? C881 C882 C890 C884 33(20) . . . . ? C887 C882 C890 C884 161(16) . . . . ? C885 C882 C890 C884 6(16) . . . . ? C894 C882 C890 C888 97(15) . . . . ? C886 C882 C890 C888 90(31) . . . . ? C881 C882 C890 C888 -34(11) . . . . ? C887 C882 C890 C888 95(15) . . . . ? C885 C882 C890 C888 -60(12) . . . . ? C888 C882 C890 C894 -97(15) . . . . ? C886 C882 C890 C894 -8(26) . . . . ? C881 C882 C890 C894 -131(14) . . . . ? C887 C882 C890 C894 -3(9) . . . . ? C885 C882 C890 C894 -157(12) . . . . ? C888 C882 C890 C883 -113(54) . . . . ? C894 C882 C890 C883 -15(55) . . . . ? C886 C882 C890 C883 -23(76) . . . . ? C881 C882 C890 C883 -146(51) . . . . ? C887 C882 C890 C883 -18(58) . . . . ? C885 C882 C890 C883 -172(54) . . . . ? C888 C882 C890 C885 60(12) . . . . ? C894 C882 C890 C885 157(12) . . . . ? C886 C882 C890 C885 150(30) . . . . ? C881 C882 C890 C885 26(8) . . . . ? C887 C882 C890 C885 155(10) . . . . ? C888 C882 C890 C895 -100(14) . . . . ? C894 C882 C890 C895 -2(11) . . . . ? C886 C882 C890 C895 -10(33) . . . . ? C881 C882 C890 C895 -133(9) . . . . ? C887 C882 C890 C895 -5(12) . . . . ? C885 C882 C890 C895 -160(8) . . . . ? C888 C882 C890 C881 34(11) . . . . ? C894 C882 C890 C881 131(14) . . . . ? C886 C882 C890 C881 123(33) . . . . ? C887 C882 C890 C881 128(13) . . . . ? C885 C882 C890 C881 -26(8) . . . . ? C881 C885 C890 C884 156(16) . . . . ? C888 C885 C890 C884 144(16) . . . . ? C882 C885 C890 C884 -174(16) . . . . ? C884 C885 C890 C888 -144(16) . . . . ? C881 C885 C890 C888 12(11) . . . . ? C882 C885 C890 C888 42(8) . . . . ? C884 C885 C890 C894 -165(18) . . . . ? C881 C885 C890 C894 -9(13) . . . . ? C888 C885 C890 C894 -21(11) . . . . ? C882 C885 C890 C894 21(11) . . . . ? C884 C885 C890 C883 -7(13) . . . . ? C881 C885 C890 C883 149(9) . . . . ? C888 C885 C890 C883 137(11) . . . . ? C882 C885 C890 C883 178(11) . . . . ? C884 C885 C890 C882 174(16) . . . . ? C881 C885 C890 C882 -30(10) . . . . ? C888 C885 C890 C882 -42(8) . . . . ? C884 C885 C890 C895 -73(27) . . . . ? C881 C885 C890 C895 83(27) . . . . ? C888 C885 C890 C895 71(26) . . . . ? C882 C885 C890 C895 113(27) . . . . ? C884 C885 C890 C881 -156(16) . . . . ? C888 C885 C890 C881 -12(11) . . . . ? C882 C885 C890 C881 30(10) . . . . ? C888 C881 C890 C884 134(24) . . . . ? C885 C881 C890 C884 -18(12) . . . . ? C882 C881 C890 C884 -157(15) . . . . ? C894 C881 C890 C884 169(14) . . . . ? C885 C881 C890 C888 -153(24) . . . . ? C882 C881 C890 C888 69(20) . . . . ? C894 C881 C890 C888 34(20) . . . . ? C884 C881 C890 C888 -134(24) . . . . ? C888 C881 C890 C894 -34(20) . . . . ? C885 C881 C890 C894 173(11) . . . . ? C882 C881 C890 C894 35(10) . . . . ? C884 C881 C890 C894 -169(14) . . . . ? C888 C881 C890 C883 101(24) . . . . ? C885 C881 C890 C883 -52(15) . . . . ? C882 C881 C890 C883 170(16) . . . . ? C894 C881 C890 C883 135(16) . . . . ? C884 C881 C890 C883 -33(13) . . . . ? C888 C881 C890 C882 -69(20) . . . . ? C885 C881 C890 C882 139(13) . . . . ? C894 C881 C890 C882 -35(10) . . . . ? C884 C881 C890 C882 157(15) . . . . ? C888 C881 C890 C885 153(24) . . . . ? C882 C881 C890 C885 -139(13) . . . . ? C894 C881 C890 C885 -173(11) . . . . ? C884 C881 C890 C885 18(12) . . . . ? C888 C881 C890 C895 2(22) . . . . ? C885 C881 C890 C895 -151(11) . . . . ? C882 C881 C890 C895 71(13) . . . . ? C894 C881 C890 C895 36(9) . . . . ? C884 C881 C890 C895 -133(15) . . . . ? C889 C887 C891 C892 9(17) . . . . ? C886 C887 C891 C892 154(23) . . . . ? C894 C887 C891 C892 172(11) . . . . ? C882 C887 C891 C892 167(9) . . . . ? C888 C887 C891 C892 -169(8) . . . . ? C889 C887 C891 C895 -169(12) . . . . ? C886 C887 C891 C895 -24(29) . . . . ? C894 C887 C891 C895 -6(10) . . . . ? C882 C887 C891 C895 -11(12) . . . . ? C892 C887 C891 C895 -178(15) . . . . ? C888 C887 C891 C895 13(10) . . . . ? C889 C887 C891 C894 -163(16) . . . . ? C886 C887 C891 C894 -18(24) . . . . ? C882 C887 C891 C894 -5(9) . . . . ? C892 C887 C891 C894 -172(11) . . . . ? C888 C887 C891 C894 19(7) . . . . ? C895 C891 C892 C887 177(18) . . . . ? C894 C891 C892 C887 19(25) . . . . ? C889 C887 C892 C891 -173(13) . . . . ? C886 C887 C892 C891 -144(34) . . . . ? C894 C887 C892 C891 -7(10) . . . . ? C882 C887 C892 C891 -19(13) . . . . ? C888 C887 C892 C891 13(9) . . . . ? C888 C882 C894 C890 53(10) . . . . ? C886 C882 C894 C890 176(12) . . . . ? C881 C882 C894 C890 53(15) . . . . ? C887 C882 C894 C890 177(11) . . . . ? C885 C882 C894 C890 18(9) . . . . ? C886 C882 C894 C888 124(16) . . . . ? C881 C882 C894 C888 0(12) . . . . ? C890 C882 C894 C888 -53(10) . . . . ? C887 C882 C894 C888 124(13) . . . . ? C885 C882 C894 C888 -35(10) . . . . ? C888 C882 C894 C887 -124(13) . . . . ? C886 C882 C894 C887 0(11) . . . . ? C881 C882 C894 C887 -124(14) . . . . ? C890 C882 C894 C887 -177(11) . . . . ? C885 C882 C894 C887 -159(9) . . . . ? C888 C882 C894 C891 -136(25) . . . . ? C886 C882 C894 C891 -12(31) . . . . ? C881 C882 C894 C891 -136(22) . . . . ? C890 C882 C894 C891 171(28) . . . . ? C887 C882 C894 C891 -12(22) . . . . ? C885 C882 C894 C891 -171(21) . . . . ? C888 C882 C894 C895 59(36) . . . . ? C886 C882 C894 C895 -177(27) . . . . ? C881 C882 C894 C895 60(38) . . . . ? C890 C882 C894 C895 6(31) . . . . ? C887 C882 C894 C895 -177(36) . . . . ? C885 C882 C894 C895 24(38) . . . . ? C888 C882 C894 C886 -124(16) . . . . ? C881 C882 C894 C886 -123(18) . . . . ? C890 C882 C894 C886 -176(12) . . . . ? C887 C882 C894 C886 0(11) . . . . ? C885 C882 C894 C886 -159(15) . . . . ? C888 C882 C894 C881 0(12) . . . . ? C886 C882 C894 C881 123(18) . . . . ? C890 C882 C894 C881 -53(15) . . . . ? C887 C882 C894 C881 124(14) . . . . ? C885 C882 C894 C881 -36(10) . . . . ? C884 C890 C894 C882 -99(74) . . . . ? C888 C890 C894 C882 -49(10) . . . . ? C883 C890 C894 C882 177(12) . . . . ? C885 C890 C894 C882 -28(14) . . . . ? C895 C890 C894 C882 177(13) . . . . ? C881 C890 C894 C882 -34(10) . . . . ? C884 C890 C894 C888 -50(74) . . . . ? C883 C890 C894 C888 -135(12) . . . . ? C882 C890 C894 C888 49(10) . . . . ? C885 C890 C894 C888 20(11) . . . . ? C895 C890 C894 C888 -134(10) . . . . ? C881 C890 C894 C888 15(8) . . . . ? C884 C890 C894 C887 -88(82) . . . . ? C888 C890 C894 C887 -38(39) . . . . ? C883 C890 C894 C887 -172(35) . . . . ? C882 C890 C894 C887 11(36) . . . . ? C885 C890 C894 C887 -17(46) . . . . ? C895 C890 C894 C887 -172(42) . . . . ? C881 C890 C894 C887 -23(40) . . . . ? C884 C890 C894 C891 87(76) . . . . ? C888 C890 C894 C891 137(16) . . . . ? C883 C890 C894 C891 3(20) . . . . ? C882 C890 C894 C891 -174(20) . . . . ? C885 C890 C894 C891 158(11) . . . . ? C895 C890 C894 C891 4(11) . . . . ? C881 C890 C894 C891 152(14) . . . . ? C884 C890 C894 C895 83(74) . . . . ? C888 C890 C894 C895 134(10) . . . . ? C883 C890 C894 C895 -1(10) . . . . ? C882 C890 C894 C895 -177(13) . . . . ? C885 C890 C894 C895 154(9) . . . . ? C881 C890 C894 C895 149(7) . . . . ? C884 C890 C894 C886 -96(73) . . . . ? C888 C890 C894 C886 -46(11) . . . . ? C883 C890 C894 C886 180(7) . . . . ? C882 C890 C894 C886 3(10) . . . . ? C885 C890 C894 C886 -25(16) . . . . ? C895 C890 C894 C886 -180(12) . . . . ? C881 C890 C894 C886 -31(10) . . . . ? C884 C890 C894 C881 -65(74) . . . . ? C888 C890 C894 C881 -15(8) . . . . ? C883 C890 C894 C881 -149(11) . . . . ? C882 C890 C894 C881 34(10) . . . . ? C885 C890 C894 C881 6(9) . . . . ? C895 C890 C894 C881 -149(7) . . . . ? C881 C888 C894 C882 -1(32) . . . . ? C890 C888 C894 C882 106(15) . . . . ? C885 C888 C894 C882 84(18) . . . . ? C884 C888 C894 C882 112(15) . . . . ? C887 C888 C894 C882 -63(15) . . . . ? C886 C888 C894 C882 -36(12) . . . . ? C881 C888 C894 C890 -107(34) . . . . ? C882 C888 C894 C890 -106(15) . . . . ? C885 C888 C894 C890 -23(13) . . . . ? C884 C888 C894 C890 6(9) . . . . ? C887 C888 C894 C890 -169(13) . . . . ? C886 C888 C894 C890 -143(9) . . . . ? C881 C888 C894 C887 61(35) . . . . ? C882 C888 C894 C887 63(15) . . . . ? C890 C888 C894 C887 169(13) . . . . ? C885 C888 C894 C887 146(12) . . . . ? C884 C888 C894 C887 175(10) . . . . ? C886 C888 C894 C887 26(8) . . . . ? C881 C888 C894 C891 138(30) . . . . ? C882 C888 C894 C891 139(27) . . . . ? C890 C888 C894 C891 -115(24) . . . . ? C885 C888 C894 C891 -137(19) . . . . ? C884 C888 C894 C891 -109(22) . . . . ? C887 C888 C894 C891 76(22) . . . . ? C886 C888 C894 C891 102(24) . . . . ? C881 C888 C894 C895 -159(30) . . . . ? C882 C888 C894 C895 -157(17) . . . . ? C890 C888 C894 C895 -51(11) . . . . ? C885 C888 C894 C895 -74(17) . . . . ? C884 C888 C894 C895 -45(12) . . . . ? C887 C888 C894 C895 140(16) . . . . ? C886 C888 C894 C895 166(12) . . . . ? C881 C888 C894 C886 35(33) . . . . ? C882 C888 C894 C886 36(12) . . . . ? C890 C888 C894 C886 143(9) . . . . ? C885 C888 C894 C886 120(14) . . . . ? C884 C888 C894 C886 149(8) . . . . ? C887 C888 C894 C886 -26(8) . . . . ? C882 C888 C894 C881 1(32) . . . . ? C890 C888 C894 C881 107(34) . . . . ? C885 C888 C894 C881 85(32) . . . . ? C884 C888 C894 C881 113(34) . . . . ? C887 C888 C894 C881 -61(35) . . . . ? C886 C888 C894 C881 -35(33) . . . . ? C889 C887 C894 C882 -33(39) . . . . ? C886 C887 C894 C882 0(13) . . . . ? C891 C887 C894 C882 -173(13) . . . . ? C892 C887 C894 C882 -169(11) . . . . ? C888 C887 C894 C882 43(10) . . . . ? C889 C887 C894 C890 -44(64) . . . . ? C886 C887 C894 C890 -10(42) . . . . ? C891 C887 C894 C890 176(42) . . . . ? C882 C887 C894 C890 -11(36) . . . . ? C892 C887 C894 C890 -179(100) . . . . ? C888 C887 C894 C890 32(35) . . . . ? C889 C887 C894 C888 -77(37) . . . . ? C886 C887 C894 C888 -43(13) . . . . ? C891 C887 C894 C888 144(12) . . . . ? C882 C887 C894 C888 -43(10) . . . . ? C892 C887 C894 C888 148(10) . . . . ? C889 C887 C894 C891 140(36) . . . . ? C886 C887 C894 C891 174(9) . . . . ? C882 C887 C894 C891 173(13) . . . . ? C892 C887 C894 C891 5(6) . . . . ? C888 C887 C894 C891 -144(12) . . . . ? C889 C887 C894 C895 145(32) . . . . ? C886 C887 C894 C895 179(9) . . . . ? C891 C887 C894 C895 5(9) . . . . ? C882 C887 C894 C895 179(17) . . . . ? C892 C887 C894 C895 10(10) . . . . ? C888 C887 C894 C895 -138(17) . . . . ? C889 C887 C894 C886 -34(33) . . . . ? C891 C887 C894 C886 -174(9) . . . . ? C882 C887 C894 C886 0(13) . . . . ? C892 C887 C894 C886 -169(9) . . . . ? C888 C887 C894 C886 43(13) . . . . ? C889 C887 C894 C881 -65(37) . . . . ? C886 C887 C894 C881 -31(10) . . . . ? C891 C887 C894 C881 156(9) . . . . ? C882 C887 C894 C881 -31(9) . . . . ? C892 C887 C894 C881 160(6) . . . . ? C888 C887 C894 C881 12(8) . . . . ? C892 C891 C894 C882 -10(49) . . . . ? C895 C891 C894 C882 -173(27) . . . . ? C887 C891 C894 C882 13(24) . . . . ? C892 C891 C894 C890 158(25) . . . . ? C895 C891 C894 C890 -4(14) . . . . ? C887 C891 C894 C890 -178(17) . . . . ? C892 C891 C894 C888 -114(31) . . . . ? C895 C891 C894 C888 83(24) . . . . ? C887 C891 C894 C888 -91(24) . . . . ? C892 C891 C894 C887 -23(30) . . . . ? C895 C891 C894 C887 174(9) . . . . ? C892 C891 C894 C895 163(31) . . . . ? C887 C891 C894 C895 -174(9) . . . . ? C892 C891 C894 C886 -19(32) . . . . ? C895 C891 C894 C886 178(8) . . . . ? C887 C891 C894 C886 4(6) . . . . ? C892 C891 C894 C881 -93(35) . . . . ? C895 C891 C894 C881 104(24) . . . . ? C887 C891 C894 C881 -70(23) . . . . ? C889 C886 C894 C882 -171(16) . . . . ? C887 C886 C894 C882 -179(18) . . . . ? C888 C886 C894 C882 40(13) . . . . ? C889 C886 C894 C890 -175(11) . . . . ? C887 C886 C894 C890 176(15) . . . . ? C882 C886 C894 C890 -4(14) . . . . ? C888 C886 C894 C890 36(9) . . . . ? C889 C886 C894 C888 149(10) . . . . ? C887 C886 C894 C888 140(12) . . . . ? C882 C886 C894 C888 -40(13) . . . . ? C889 C886 C894 C887 9(8) . . . . ? C882 C886 C894 C887 179(18) . . . . ? C888 C886 C894 C887 -140(12) . . . . ? C889 C886 C894 C891 3(9) . . . . ? C887 C886 C894 C891 -6(8) . . . . ? C882 C886 C894 C891 173(17) . . . . ? C888 C886 C894 C891 -146(12) . . . . ? C889 C886 C894 C895 6(25) . . . . ? C887 C886 C894 C895 -2(22) . . . . ? C882 C886 C894 C895 177(31) . . . . ? C888 C886 C894 C895 -143(27) . . . . ? C889 C886 C894 C881 157(8) . . . . ? C887 C886 C894 C881 148(10) . . . . ? C882 C886 C894 C881 -32(13) . . . . ? C888 C886 C894 C881 8(7) . . . . ? C888 C881 C894 C882 178(40) . . . . ? C885 C881 C894 C882 108(18) . . . . ? C890 C881 C894 C882 114(18) . . . . ? C884 C881 C894 C882 120(18) . . . . ? C888 C881 C894 C890 64(32) . . . . ? C885 C881 C894 C890 -6(9) . . . . ? C882 C881 C894 C890 -114(18) . . . . ? C884 C881 C894 C890 6(8) . . . . ? C885 C881 C894 C888 -70(33) . . . . ? C882 C881 C894 C888 -178(40) . . . . ? C890 C881 C894 C888 -64(32) . . . . ? C884 C881 C894 C888 -58(32) . . . . ? C888 C881 C894 C887 -122(35) . . . . ? C885 C881 C894 C887 167(10) . . . . ? C882 C881 C894 C887 59(17) . . . . ? C890 C881 C894 C887 173(12) . . . . ? C884 C881 C894 C887 179(9) . . . . ? C888 C881 C894 C891 -61(40) . . . . ? C885 C881 C894 C891 -131(23) . . . . ? C882 C881 C894 C891 121(31) . . . . ? C890 C881 C894 C891 -125(27) . . . . ? C884 C881 C894 C891 -119(24) . . . . ? C888 C881 C894 C895 24(34) . . . . ? C885 C881 C894 C895 -46(14) . . . . ? C882 C881 C894 C895 -154(21) . . . . ? C890 C881 C894 C895 -40(10) . . . . ? C884 C881 C894 C895 -34(11) . . . . ? C888 C881 C894 C886 -143(35) . . . . ? C885 C881 C894 C886 147(9) . . . . ? C882 C881 C894 C886 39(15) . . . . ? C890 C881 C894 C886 153(9) . . . . ? C884 C881 C894 C886 159(8) . . . . ? C892 C891 C895 C894 -171(15) . . . . ? C887 C891 C895 C894 5(9) . . . . ? C892 C891 C895 C883 -163(15) . . . . ? C894 C891 C895 C883 9(20) . . . . ? C887 C891 C895 C883 14(25) . . . . ? C892 C891 C895 C890 -169(11) . . . . ? C894 C891 C895 C890 2(8) . . . . ? C887 C891 C895 C890 8(11) . . . . ? C882 C894 C895 C891 170(36) . . . . ? C890 C894 C895 C891 177(10) . . . . ? C888 C894 C895 C891 -143(13) . . . . ? C887 C894 C895 C891 -6(9) . . . . ? C886 C894 C895 C891 -4(23) . . . . ? C881 C894 C895 C891 -149(12) . . . . ? C882 C894 C895 C883 -6(36) . . . . ? C890 C894 C895 C883 1(8) . . . . ? C888 C894 C895 C883 41(12) . . . . ? C887 C894 C895 C883 178(9) . . . . ? C891 C894 C895 C883 -176(8) . . . . ? C886 C894 C895 C883 179(100) . . . . ? C881 C894 C895 C883 35(11) . . . . ? C882 C894 C895 C890 -6(32) . . . . ? C888 C894 C895 C890 40(9) . . . . ? C887 C894 C895 C890 177(14) . . . . ? C891 C894 C895 C890 -177(10) . . . . ? C886 C894 C895 C890 179(100) . . . . ? C881 C894 C895 C890 34(9) . . . . ? C884 C883 C895 C891 -20(24) . . . . ? C890 C883 C895 C891 -8(20) . . . . ? C884 C883 C895 C894 -13(12) . . . . ? C890 C883 C895 C894 -1(7) . . . . ? C884 C883 C895 C890 -12(10) . . . . ? C884 C890 C895 C891 -169(14) . . . . ? C888 C890 C895 C891 -47(12) . . . . ? C894 C890 C895 C891 -3(9) . . . . ? C883 C890 C895 C891 176(9) . . . . ? C882 C890 C895 C891 -1(11) . . . . ? C885 C890 C895 C891 -110(25) . . . . ? C881 C890 C895 C891 -47(12) . . . . ? C884 C890 C895 C894 -166(17) . . . . ? C888 C890 C895 C894 -44(10) . . . . ? C883 C890 C895 C894 179(10) . . . . ? C882 C890 C895 C894 2(10) . . . . ? C885 C890 C895 C894 -107(27) . . . . ? C881 C890 C895 C894 -44(11) . . . . ? C884 C890 C895 C883 15(13) . . . . ? C888 C890 C895 C883 137(11) . . . . ? C894 C890 C895 C883 -179(10) . . . . ? C882 C890 C895 C883 -177(11) . . . . ? C885 C890 C895 C883 74(25) . . . . ? C881 C890 C895 C883 136(11) . . . . ? C996 C991 C992 C993 -176(9) . . . 3_655 ? C993 C991 C992 C993 -19(12) . . . 3_655 ? C996 C991 C992 C995 17(12) . . . . ? C993 C991 C992 C995 174(6) . . . . ? C996 C991 C993 C992 177(8) . . . 3_655 ? C992 C991 C993 C992 19(12) . . . 3_655 ? C996 C991 C993 C997 -17(12) . . . . ? C992 C991 C993 C997 -176(6) . . . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 1.947 _refine_diff_density_min -1.344 _refine_diff_density_rms 0.175