# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_section_title ; Non Covalent Interactions at Bis(pyrazole)silver(I) or -gold(I) Cation ; _audit_creation_method SHELXL _publ_contact_author ; Fernando Villafa\~ne IU CINQUIMA/Quimica Inorganica Facultad de Ciencias Universidad de Valladolid C/ Prado de la Magdalena s/n 47005 Valladolid SPAIN ; _publ_contact_author_phone +34-983-184096 _publ_contact_author_fax +34-983-423013 _publ_contact_author_email fervilla@qi.uva.es loop_ _publ_author_name _publ_author_address 'Vanesa Garcia-Pacios' ; IU CINQUIMA/Quimica Inorganica Facultad de Ciencias Universidad de Valladolid C/ Prado de la Magdalena s/n 47005 Valladolid SPAIN ; 'Marta Arroyo' ; IU CINQUIMA/Quimica Inorganica Facultad de Ciencias Universidad de Valladolid C/ Prado de la Magdalena s/n 47005 Valladolid SPAIN ; 'Noelia Anton' ; IU CINQUIMA/Quimica Inorganica Facultad de Ciencias Universidad de Valladolid C/ Prado de la Magdalena s/n 47005 Valladolid SPAIN ; 'Daniel Miguel' ; IU CINQUIMA/Quimica Inorganica Facultad de Ciencias Universidad de Valladolid C/ Prado de la Magdalena s/n 47005 Valladolid SPAIN ; 'Fernando Villafane' ; IU CINQUIMA/Quimica Inorganica Facultad de Ciencias Universidad de Valladolid C/ Prado de la Magdalena s/n 47005 Valladolid SPAIN ; _publ_contact_author_name 'Fernando Villafane' #-------------------------- data section of block --------------------------- data_Compound_1a_(vg54am) _database_code_depnum_ccdc_archive 'CCDC 708793' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H8 Ag B F4 N4' _chemical_formula_weight 330.84 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' B B 0.0013 0.0007 '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' Ag Ag -0.8971 1.1015 '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 5.3607(11) _cell_length_b 8.0567(16) _cell_length_c 12.792(3) _cell_angle_alpha 81.567(4) _cell_angle_beta 88.779(4) _cell_angle_gamma 85.826(4) _cell_volume 545.04(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PRISM _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.016 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 320 _exptl_absorpt_coefficient_mu 1.881 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.519547 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2397 _diffrn_reflns_av_R_equivalents 0.0180 _diffrn_reflns_av_sigmaI/netI 0.0157 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 23.26 _reflns_number_total 1545 _reflns_number_gt 1328 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0804P)^2^+0.6370P] 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 SHELXL _refine_ls_extinction_coef 0.013(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1545 _refine_ls_number_parameters 153 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1291 _refine_ls_wR_factor_gt 0.1235 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 Ag1 Ag 0.0000 0.5000 0.5000 0.0768(4) Uani 1 2 d S . . N1 N 0.2821(8) 0.5962(6) 0.5828(3) 0.0594(11) Uani 1 1 d . . . N2 N 0.3290(11) 0.7588(7) 0.5717(4) 0.0759(14) Uani 1 1 d . . . H2 H 0.2384 0.8384 0.5354 0.091 Uiso 1 1 calc R . . C11 C 0.4622(10) 0.5163(7) 0.6421(4) 0.0651(14) Uani 1 1 d . . . H11 H 0.4783 0.4005 0.6629 0.078 Uiso 1 1 calc R . . C12 C 0.6253(11) 0.6284(10) 0.6694(4) 0.0791(18) Uani 1 1 d . . . H12 H 0.7678 0.6029 0.7105 0.095 Uiso 1 1 calc R . . C13 C 0.5346(13) 0.7824(10) 0.6240(6) 0.0867(19) Uani 1 1 d . . . H13 H 0.6015 0.8845 0.6283 0.104 Uiso 1 1 calc R . . Ag2 Ag 1.0000 0.0000 1.0000 0.0762(4) Uani 1 2 d S . . N3 N 0.6703(8) 0.1686(6) 0.9953(3) 0.0624(11) Uani 1 1 d . . . N4 N 0.5437(10) 0.2308(7) 0.9078(4) 0.0740(14) Uani 1 1 d . . . C21 C 0.5324(12) 0.2115(8) 1.0741(5) 0.0718(15) Uani 1 1 d . . . H21 H 0.5726 0.1837 1.1452 0.086 Uiso 1 1 calc R . . C22 C 0.3158(13) 0.3054(9) 1.0353(6) 0.085(2) Uani 1 1 d . . . H22 H 0.1885 0.3526 1.0745 0.102 Uiso 1 1 calc R . . C23 C 0.3298(12) 0.3130(8) 0.9306(5) 0.0819(17) Uani 1 1 d . . . H23 H 0.2116 0.3661 0.8824 0.098 Uiso 1 1 calc R . . B1 B 0.0389(12) 0.1064(8) 0.7001(4) 0.0603(15) Uani 1 1 d . . . F1 F -0.0214(13) -0.0318(7) 0.7647(4) 0.156(2) Uani 1 1 d . . . F2 F 0.2875(9) 0.1171(7) 0.7174(5) 0.1336(18) Uani 1 1 d . . . F3 F -0.0798(12) 0.2486(6) 0.7239(4) 0.1370(19) Uani 1 1 d . . . F4 F 0.0103(9) 0.0869(5) 0.5981(3) 0.1069(14) Uani 1 1 d . . . H4 H 0.595(14) 0.221(9) 0.849(6) 0.10(2) 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 0.0631(5) 0.1003(6) 0.0685(5) -0.0102(3) -0.0139(3) -0.0150(3) N1 0.051(2) 0.072(3) 0.055(2) -0.0078(19) -0.0062(19) -0.002(2) N2 0.072(3) 0.069(3) 0.085(3) -0.007(2) -0.010(3) 0.000(3) C11 0.063(3) 0.080(4) 0.049(3) -0.005(2) -0.006(2) 0.008(3) C12 0.054(3) 0.131(6) 0.055(3) -0.026(3) -0.012(3) 0.001(3) C13 0.082(5) 0.093(5) 0.092(4) -0.030(4) -0.002(4) -0.022(4) Ag2 0.0539(5) 0.0827(5) 0.0882(5) -0.0049(3) -0.0052(3) 0.0059(3) N3 0.052(2) 0.071(3) 0.061(3) -0.003(2) -0.009(2) -0.001(2) N4 0.069(3) 0.089(3) 0.058(3) 0.003(2) -0.003(2) 0.003(3) C21 0.073(4) 0.088(4) 0.057(3) -0.021(3) -0.009(3) 0.000(3) C22 0.069(4) 0.089(4) 0.102(5) -0.037(4) 0.009(4) 0.008(3) C23 0.074(4) 0.078(4) 0.090(5) -0.005(3) -0.016(3) 0.012(3) B1 0.065(4) 0.067(4) 0.046(3) 0.000(3) -0.014(3) 0.001(3) F1 0.240(7) 0.131(4) 0.093(3) 0.027(3) -0.006(4) -0.064(4) F2 0.099(3) 0.152(4) 0.161(5) -0.060(4) -0.034(3) 0.002(3) F3 0.152(4) 0.134(4) 0.121(3) -0.036(3) -0.004(3) 0.058(3) F4 0.146(4) 0.118(3) 0.0545(19) -0.0127(18) -0.033(2) 0.018(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.119(4) 2_566 ? Ag1 N1 2.119(4) . ? N1 C11 1.311(6) . ? N1 N2 1.339(7) . ? N2 C13 1.341(9) . ? C11 C12 1.387(8) . ? C12 C13 1.351(10) . ? Ag2 N3 2.145(4) . ? Ag2 N3 2.145(4) 2_757 ? N3 C21 1.310(7) . ? N3 N4 1.335(6) . ? N4 C23 1.331(8) . ? C21 C22 1.397(10) . ? C22 C23 1.333(9) . ? B1 F1 1.340(8) . ? B1 F3 1.341(8) . ? B1 F4 1.350(7) . ? B1 F2 1.367(8) . ? 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 N1 180.000(1) 2_566 . ? C11 N1 N2 105.5(5) . . ? C11 N1 Ag1 129.9(4) . . ? N2 N1 Ag1 124.1(3) . . ? N1 N2 C13 111.7(5) . . ? N1 C11 C12 110.6(5) . . ? C13 C12 C11 105.8(5) . . ? N2 C13 C12 106.4(6) . . ? N3 Ag2 N3 180.000(1) . 2_757 ? C21 N3 N4 105.8(5) . . ? C21 N3 Ag2 128.7(4) . . ? N4 N3 Ag2 124.7(4) . . ? C23 N4 N3 111.2(5) . . ? N3 C21 C22 109.8(5) . . ? C23 C22 C21 105.6(6) . . ? N4 C23 C22 107.5(6) . . ? F1 B1 F3 113.6(6) . . ? F1 B1 F4 110.6(6) . . ? F3 B1 F4 112.6(5) . . ? F1 B1 F2 104.5(5) . . ? F3 B1 F2 106.7(6) . . ? F4 B1 F2 108.4(6) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.586 _refine_diff_density_min -0.588 _refine_diff_density_rms 0.093 #===END data_Compound_1b_(vg14a) _database_code_depnum_ccdc_archive 'CCDC 708794' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H16 Ag B F4 N4' _chemical_formula_weight 386.95 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' B B 0.0013 0.0007 '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' 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 P2(1)/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 13.486(10) _cell_length_b 15.850(11) _cell_length_c 7.112(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.881(13) _cell_angle_gamma 90.00 _cell_volume 1512.2(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PRISM _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.700 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 1.369 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.410938 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6492 _diffrn_reflns_av_R_equivalents 0.1050 _diffrn_reflns_av_sigmaI/netI 0.1099 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 23.42 _reflns_number_total 2172 _reflns_number_gt 1144 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1321P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2172 _refine_ls_number_parameters 189 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1576 _refine_ls_R_factor_gt 0.0848 _refine_ls_wR_factor_ref 0.2403 _refine_ls_wR_factor_gt 0.2006 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _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 Ag1 Ag 0.77703(8) 0.78230(8) 0.21673(19) 0.0692(6) Uani 1 1 d . . . N1 N 0.9320(7) 0.7651(7) 0.2551(18) 0.060(3) Uani 1 1 d . . . N2 N 0.9769(8) 0.6893(7) 0.2726(17) 0.059(3) Uani 1 1 d . . . H2 H 0.9457 0.6419 0.2664 0.070 Uiso 1 1 calc R . . N3 N 0.6224(8) 0.7969(7) 0.1826(17) 0.056(3) Uani 1 1 d . . . N4 N 0.5586(8) 0.7308(7) 0.1609(17) 0.055(3) Uani 1 1 d . . . C11 C 1.0045(10) 0.8210(8) 0.2772(19) 0.051(4) Uani 1 1 d . . . C12 C 1.0957(10) 0.7812(8) 0.301(2) 0.060(4) Uani 1 1 d . . . H12 H 1.1582 0.8066 0.3145 0.072 Uiso 1 1 calc R . . C13 C 1.0754(10) 0.6968(8) 0.301(2) 0.054(4) Uani 1 1 d . . . C14 C 0.9845(12) 0.9151(9) 0.265(2) 0.081(5) Uani 1 1 d . . . H14A H 1.0069 0.9369 0.1505 0.122 Uiso 1 1 calc R . . H14B H 1.0196 0.9428 0.3717 0.122 Uiso 1 1 calc R . . H14C H 0.9142 0.9251 0.2643 0.122 Uiso 1 1 calc R . . C15 C 1.1415(12) 0.6195(9) 0.321(3) 0.087(6) Uani 1 1 d . . . H15A H 1.1017 0.5707 0.3404 0.131 Uiso 1 1 calc R . . H15B H 1.1907 0.6267 0.4273 0.131 Uiso 1 1 calc R . . H15C H 1.1741 0.6122 0.2082 0.131 Uiso 1 1 calc R . . C21 C 0.5627(10) 0.8646(8) 0.1777(19) 0.053(4) Uani 1 1 d . . . C22 C 0.4637(11) 0.8404(9) 0.1499(19) 0.062(4) Uani 1 1 d . . . H22 H 0.4084 0.8758 0.1387 0.074 Uiso 1 1 calc R . . C23 C 0.4632(10) 0.7549(9) 0.142(2) 0.055(4) Uani 1 1 d . . . C24 C 0.6086(15) 0.9536(10) 0.190(3) 0.102(7) Uani 1 1 d . . . H24A H 0.6796 0.9493 0.2179 0.153 Uiso 1 1 calc R . . H24B H 0.5814 0.9850 0.2880 0.153 Uiso 1 1 calc R . . H24C H 0.5935 0.9821 0.0712 0.153 Uiso 1 1 calc R . . C25 C 0.3802(11) 0.6919(11) 0.125(2) 0.078(5) Uani 1 1 d . . . H25A H 0.3913 0.6514 0.0295 0.117 Uiso 1 1 calc R . . H25B H 0.3181 0.7204 0.0916 0.117 Uiso 1 1 calc R . . H25C H 0.3779 0.6636 0.2441 0.117 Uiso 1 1 calc R . . B1 B 0.7544(12) 0.5435(12) 0.214(3) 0.064(5) Uani 1 1 d . . . F1 F 0.8006(11) 0.5770(10) 0.0724(19) 0.164(6) Uani 1 1 d . . . F2 F 0.6609(8) 0.5737(7) 0.1976(19) 0.130(4) Uani 1 1 d . . . F3 F 0.7470(9) 0.4610(6) 0.206(2) 0.174(7) Uani 1 1 d . . . F4 F 0.8115(10) 0.5695(8) 0.3662(18) 0.150(6) Uani 1 1 d . . . H4 H 0.571(8) 0.676(7) 0.152(14) 0.03(3) 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 0.0442(7) 0.0761(9) 0.0863(10) 0.0017(7) 0.0019(5) -0.0018(6) N1 0.022(6) 0.062(8) 0.100(10) -0.009(7) 0.016(6) -0.001(6) N2 0.038(7) 0.038(6) 0.100(10) 0.003(6) 0.009(6) -0.010(5) N3 0.038(6) 0.048(7) 0.082(9) -0.005(6) 0.007(6) 0.001(6) N4 0.049(7) 0.038(7) 0.077(9) -0.002(6) -0.001(6) -0.003(6) C11 0.061(9) 0.040(7) 0.048(9) -0.004(6) -0.006(7) -0.005(7) C12 0.054(9) 0.050(9) 0.073(11) -0.005(8) -0.002(7) -0.011(7) C13 0.056(9) 0.042(8) 0.065(10) 0.005(7) 0.002(7) 0.002(7) C14 0.083(12) 0.050(9) 0.107(15) -0.006(9) -0.004(10) -0.002(8) C15 0.074(12) 0.058(10) 0.130(17) 0.013(10) 0.009(11) -0.003(8) C21 0.060(9) 0.041(8) 0.055(10) 0.004(7) -0.012(7) 0.011(7) C22 0.065(10) 0.065(10) 0.054(10) 0.009(8) 0.002(7) 0.018(8) C23 0.046(9) 0.066(10) 0.051(10) 0.013(7) -0.002(7) -0.009(7) C24 0.118(16) 0.065(11) 0.116(16) 0.010(11) -0.025(13) -0.023(10) C25 0.062(10) 0.107(13) 0.065(12) 0.017(9) 0.006(8) -0.012(9) B1 0.046(10) 0.069(13) 0.076(14) 0.019(11) -0.002(10) -0.004(8) F1 0.153(13) 0.217(15) 0.130(12) 0.014(10) 0.054(9) -0.069(11) F2 0.092(8) 0.110(8) 0.186(12) 0.005(8) 0.001(8) 0.040(7) F3 0.107(10) 0.049(6) 0.35(2) -0.021(8) -0.032(11) 0.003(5) F4 0.152(11) 0.138(10) 0.144(11) 0.002(9) -0.065(9) -0.047(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 Ag1 N3 2.088(10) . ? Ag1 N1 2.097(10) . ? N1 C11 1.316(16) . ? N1 N2 1.346(15) . ? N2 C13 1.328(17) . ? N3 C21 1.339(15) . ? N3 N4 1.354(14) . ? N4 C23 1.336(17) . ? C11 C12 1.376(18) . ? C11 C14 1.517(19) . ? C12 C13 1.366(18) . ? C13 C15 1.513(19) . ? C21 C22 1.383(19) . ? C21 C24 1.541(19) . ? C22 C23 1.36(2) . ? C23 C25 1.49(2) . ? B1 F3 1.31(2) . ? B1 F4 1.326(19) . ? B1 F2 1.342(19) . ? B1 F1 1.35(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ag1 N1 178.7(5) . . ? C11 N1 N2 105.5(10) . . ? C11 N1 Ag1 130.3(10) . . ? N2 N1 Ag1 124.1(8) . . ? C13 N2 N1 111.6(10) . . ? C21 N3 N4 104.1(11) . . ? C21 N3 Ag1 133.1(9) . . ? N4 N3 Ag1 122.8(8) . . ? C23 N4 N3 112.6(11) . . ? N1 C11 C12 110.5(11) . . ? N1 C11 C14 121.9(13) . . ? C12 C11 C14 127.5(13) . . ? C13 C12 C11 105.8(12) . . ? N2 C13 C12 106.6(11) . . ? N2 C13 C15 120.8(12) . . ? C12 C13 C15 132.6(13) . . ? N3 C21 C22 110.6(12) . . ? N3 C21 C24 119.7(14) . . ? C22 C21 C24 129.7(13) . . ? C23 C22 C21 106.4(12) . . ? N4 C23 C22 106.3(12) . . ? N4 C23 C25 121.6(14) . . ? C22 C23 C25 132.1(14) . . ? F3 B1 F4 112.5(15) . . ? F3 B1 F2 106.6(14) . . ? F4 B1 F2 115.1(18) . . ? F3 B1 F1 113.3(19) . . ? F4 B1 F1 102.3(15) . . ? F2 B1 F1 107.1(15) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 23.42 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.228 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.151 #===END data_Compound_2_(vg35b) _database_code_depnum_ccdc_archive 'CCDC 708795' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H16 Au2 Cl2 N4' _chemical_formula_weight 657.10 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 19.906(7) _cell_length_b 10.207(4) _cell_length_c 7.944(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1614.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PRISM _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.704 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 18.478 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.386443 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6871 _diffrn_reflns_av_R_equivalents 0.0572 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 23.27 _reflns_number_total 2302 _reflns_number_gt 1915 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0695P)^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 SHELXL _refine_ls_extinction_coef 0.0035(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(2) _refine_ls_number_reflns 2302 _refine_ls_number_parameters 168 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0513 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1107 _refine_ls_wR_factor_gt 0.1062 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 1.00016(3) 0.99474(5) 0.4831(2) 0.0443(3) Uani 1 1 d . . . N1 N 1.0767(6) 0.8659(9) 0.499(3) 0.038(3) Uani 1 1 d . . . N2 N 1.0680(8) 0.7477(11) 0.5728(17) 0.044(3) Uani 1 1 d . . . H2 H 1.0318 0.7260 0.6247 0.053 Uiso 1 1 calc R . . C11 C 1.1194(8) 0.6701(15) 0.5582(18) 0.030(3) Uani 1 1 d . . . C12 C 1.1679(11) 0.7454(14) 0.468(4) 0.056(5) Uani 1 1 d . . . H12 H 1.2110 0.7198 0.4364 0.067 Uiso 1 1 calc R . . C13 C 1.1367(8) 0.8667(16) 0.4352(17) 0.037(4) Uani 1 1 d . . . C14 C 1.1280(12) 0.5412(17) 0.619(3) 0.077(7) Uani 1 1 d . . . H14A H 1.0946 0.5230 0.7026 0.115 Uiso 1 1 calc R . . H14B H 1.1719 0.5324 0.6671 0.115 Uiso 1 1 calc R . . H14C H 1.1232 0.4805 0.5271 0.115 Uiso 1 1 calc R . . C15 C 1.1662(11) 0.9849(16) 0.348(2) 0.059(5) Uani 1 1 d . . . H15A H 1.1340 1.0195 0.2693 0.089 Uiso 1 1 calc R . . H15B H 1.2061 0.9596 0.2884 0.089 Uiso 1 1 calc R . . H15C H 1.1771 1.0506 0.4297 0.089 Uiso 1 1 calc R . . N3 N 0.9236(6) 1.1243(10) 0.470(3) 0.039(3) Uani 1 1 d . . . N4 N 0.8630(7) 1.0919(14) 0.3946(16) 0.046(4) Uani 1 1 d . . . H4 H 0.8566 1.0204 0.3398 0.055 Uiso 1 1 calc R . . C21 C 0.8165(9) 1.1808(18) 0.415(2) 0.044(4) Uani 1 1 d . . . C22 C 0.8521(11) 1.2827(18) 0.507(3) 0.053(6) Uani 1 1 d . . . H22 H 0.8343 1.3630 0.5389 0.064 Uiso 1 1 calc R . . C23 C 0.9144(10) 1.2420(13) 0.5362(16) 0.043(5) Uani 1 1 d . . . C24 C 0.7511(11) 1.169(2) 0.350(2) 0.073(6) Uani 1 1 d . . . H24A H 0.7442 1.0819 0.3088 0.110 Uiso 1 1 calc R . . H24B H 0.7455 1.2304 0.2586 0.110 Uiso 1 1 calc R . . H24C H 0.7190 1.1882 0.4363 0.110 Uiso 1 1 calc R . . C25 C 0.9695(11) 1.3130(18) 0.624(3) 0.062(5) Uani 1 1 d . . . H25A H 0.9856 1.2607 0.7162 0.092 Uiso 1 1 calc R . . H25B H 0.9528 1.3949 0.6665 0.092 Uiso 1 1 calc R . . H25C H 1.0055 1.3292 0.5467 0.092 Uiso 1 1 calc R . . Au2 Au 0.88358(3) 0.74018(5) 0.48332(18) 0.0505(3) Uani 1 1 d . . . Cl1 Cl 0.9265(3) 0.6682(6) 0.7290(8) 0.0745(15) Uani 1 1 d . . . Cl2 Cl 0.8382(3) 0.8089(5) 0.2373(8) 0.0685(14) 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 0.0425(4) 0.0412(4) 0.0491(4) 0.0008(5) -0.0002(5) 0.0086(2) N1 0.033(7) 0.027(5) 0.055(9) 0.002(8) 0.008(10) 0.015(5) N2 0.054(9) 0.036(7) 0.042(7) -0.001(5) 0.003(7) 0.005(7) C11 0.018(8) 0.033(8) 0.040(8) -0.017(6) -0.002(6) 0.003(7) C12 0.070(11) 0.057(9) 0.041(10) -0.007(10) 0.002(14) 0.024(9) C13 0.029(10) 0.051(10) 0.032(11) -0.010(6) -0.002(6) 0.008(8) C14 0.10(2) 0.047(11) 0.083(14) -0.021(10) -0.013(13) 0.001(12) C15 0.066(15) 0.058(11) 0.054(12) 0.001(8) 0.003(10) -0.004(10) N3 0.037(6) 0.036(6) 0.045(7) 0.009(8) 0.003(10) 0.014(5) N4 0.052(11) 0.044(8) 0.042(7) 0.000(6) -0.010(7) 0.012(7) C21 0.036(10) 0.060(11) 0.038(8) 0.008(7) 0.016(7) 0.009(10) C22 0.065(11) 0.061(10) 0.033(15) 0.008(9) 0.016(10) 0.027(9) C23 0.068(13) 0.027(8) 0.034(10) 0.005(5) 0.012(7) 0.010(8) C24 0.052(14) 0.113(16) 0.055(13) 0.013(10) -0.001(9) 0.032(13) C25 0.069(15) 0.051(10) 0.065(11) -0.006(8) -0.010(11) -0.018(11) Au2 0.0483(4) 0.0477(4) 0.0554(4) -0.0022(7) 0.0050(11) -0.0004(3) Cl1 0.068(4) 0.096(4) 0.060(3) 0.023(3) 0.008(3) 0.003(3) Cl2 0.083(4) 0.067(3) 0.056(3) -0.010(2) -0.013(3) 0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 N1 2.016(10) . ? Au1 N3 2.020(10) . ? N1 C13 1.30(2) . ? N1 N2 1.355(16) . ? N2 C11 1.30(2) . ? C11 C14 1.41(2) . ? C11 C12 1.43(3) . ? C12 C13 1.41(2) . ? C13 C15 1.51(2) . ? N3 C23 1.326(18) . ? N3 N4 1.387(19) . ? N4 C21 1.31(2) . ? C21 C24 1.41(3) . ? C21 C22 1.45(3) . ? C22 C23 1.33(3) . ? C23 C25 1.49(3) . ? Au2 Cl1 2.253(7) . ? Au2 Cl2 2.264(6) . ? 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 Au1 N3 179.5(10) . . ? C13 N1 N2 107.0(12) . . ? C13 N1 Au1 132.0(12) . . ? N2 N1 Au1 120.7(11) . . ? C11 N2 N1 113.8(14) . . ? N2 C11 C14 129.3(18) . . ? N2 C11 C12 104.4(14) . . ? C14 C11 C12 126.3(16) . . ? C13 C12 C11 105.5(15) . . ? N1 C13 C12 109.3(15) . . ? N1 C13 C15 122.8(15) . . ? C12 C13 C15 127.9(16) . . ? C23 N3 N4 105.4(13) . . ? C23 N3 Au1 132.7(13) . . ? N4 N3 Au1 121.6(9) . . ? C21 N4 N3 113.4(14) . . ? N4 C21 C24 123.5(18) . . ? N4 C21 C22 102.3(15) . . ? C24 C21 C22 134.1(18) . . ? C23 C22 C21 108.7(14) . . ? N3 C23 C22 110.0(17) . . ? N3 C23 C25 121.7(17) . . ? C22 C23 C25 128.2(16) . . ? Cl1 Au2 Cl2 178.5(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.379 _refine_diff_density_min -1.703 _refine_diff_density_rms 0.235 #===END data_Compound_3_(vg18am) _database_code_depnum_ccdc_archive 'CCDC 708796' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H16 Au B F4 N4' _chemical_formula_weight 476.04 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' H H 0.0000 0.0000 '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' N N 0.0061 0.0033 '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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 7.020(7) _cell_length_b 10.416(10) _cell_length_c 20.59(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.948(19) _cell_angle_gamma 90.00 _cell_volume 1503(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PRISM _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.103 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 9.822 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.196886 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6496 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.0425 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 23.43 _reflns_number_total 2169 _reflns_number_gt 1883 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+90.8959P] 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 2169 _refine_ls_number_parameters 176 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1114 _refine_ls_R_factor_gt 0.0979 _refine_ls_wR_factor_ref 0.2523 _refine_ls_wR_factor_gt 0.2472 _refine_ls_goodness_of_fit_ref 1.335 _refine_ls_restrained_S_all 1.335 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.74723(17) 0.97906(11) -0.01353(6) 0.0570(5) Uani 1 1 d . . . N1 N 0.715(3) 1.103(2) -0.0867(10) 0.040(5) Uani 1 1 d . . . N2 N 0.698(3) 1.228(2) -0.0750(12) 0.055(6) Uani 1 1 d . . . H2 H 0.7023 1.2600 -0.0365 0.066 Uiso 1 1 calc R . . C11 C 0.702(4) 1.090(3) -0.1518(11) 0.047(7) Uani 1 1 d . . . C12 C 0.677(5) 1.212(3) -0.1791(16) 0.066(9) Uani 1 1 d . . . H12 H 0.6638 1.2316 -0.2231 0.079 Uiso 1 1 calc R . . C13 C 0.675(4) 1.296(3) -0.1285(15) 0.060(8) Uani 1 1 d . . . C14 C 0.710(5) 0.965(3) -0.1838(17) 0.073(9) Uani 1 1 d . . . H14A H 0.6145 0.9101 -0.1674 0.110 Uiso 1 1 calc R . . H14B H 0.8338 0.9281 -0.1753 0.110 Uiso 1 1 calc R . . H14C H 0.6869 0.9763 -0.2299 0.110 Uiso 1 1 calc R . . C15 C 0.660(5) 1.439(3) -0.1289(19) 0.079(10) Uani 1 1 d . . . H15A H 0.7852 1.4763 -0.1300 0.118 Uiso 1 1 calc R . . H15B H 0.6007 1.4675 -0.0904 0.118 Uiso 1 1 calc R . . H15C H 0.5845 1.4665 -0.1666 0.118 Uiso 1 1 calc R . . N3 N 0.784(3) 0.862(2) 0.0626(11) 0.046(5) Uani 1 1 d . . . N4 N 0.790(3) 0.909(2) 0.1226(12) 0.049(6) Uani 1 1 d . . . H4 H 0.7773 0.9890 0.1314 0.059 Uiso 1 1 calc R . . C21 C 0.799(4) 0.736(2) 0.0707(14) 0.045(7) Uani 1 1 d . . . C22 C 0.820(5) 0.710(3) 0.1363(18) 0.070(10) Uani 1 1 d . . . H22 H 0.8330 0.6291 0.1551 0.084 Uiso 1 1 calc R . . C23 C 0.819(4) 0.819(3) 0.1671(15) 0.057(8) Uani 1 1 d . . . C24 C 0.789(6) 0.652(3) 0.0106(19) 0.086(12) Uani 1 1 d . . . H24A H 0.7542 0.7034 -0.0269 0.130 Uiso 1 1 calc R . . H24B H 0.6950 0.5863 0.0155 0.130 Uiso 1 1 calc R . . H24C H 0.9111 0.6132 0.0052 0.130 Uiso 1 1 calc R . . C25 C 0.836(6) 0.847(4) 0.2375(19) 0.091(12) Uani 1 1 d . . . H25A H 0.9277 0.7895 0.2581 0.137 Uiso 1 1 calc R . . H25B H 0.7143 0.8344 0.2559 0.137 Uiso 1 1 calc R . . H25C H 0.8768 0.9338 0.2443 0.137 Uiso 1 1 calc R . . B1 B 0.262(3) 0.7122(15) -0.1190(7) 0.055(9) Uani 1 1 d G . . F1 F 0.182(5) 0.8225(15) -0.1332(13) 0.20(2) Uani 1 1 d G . . F2 F 0.147(6) 0.6194(18) -0.1379(15) 0.24(3) Uani 1 1 d G . . F3 F 0.297(4) 0.705(2) -0.0563(7) 0.158(14) Uani 1 1 d G . . F4 F 0.421(5) 0.702(5) -0.1488(16) 0.36(5) Uani 1 1 d G . . 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 0.0574(8) 0.0532(8) 0.0603(8) 0.0041(6) 0.0022(5) 0.0020(6) N1 0.035(12) 0.045(13) 0.041(13) 0.005(10) 0.015(9) -0.003(10) N2 0.061(16) 0.057(16) 0.048(15) -0.006(12) 0.011(12) -0.009(13) C11 0.039(14) 0.08(2) 0.024(13) -0.012(13) -0.002(11) -0.010(14) C12 0.06(2) 0.09(2) 0.050(19) 0.014(18) 0.002(15) 0.007(18) C13 0.058(19) 0.07(2) 0.05(2) -0.001(17) 0.015(15) 0.006(16) C14 0.08(2) 0.07(2) 0.07(2) -0.008(18) 0.000(18) -0.011(19) C15 0.08(2) 0.07(2) 0.09(3) 0.017(19) 0.00(2) -0.006(19) N3 0.041(13) 0.052(14) 0.045(14) 0.000(11) 0.007(10) -0.010(11) N4 0.052(14) 0.029(12) 0.068(16) 0.008(11) 0.012(12) 0.002(10) C21 0.048(16) 0.034(15) 0.053(18) -0.009(12) -0.005(13) 0.008(12) C22 0.07(2) 0.039(18) 0.09(3) 0.011(17) -0.038(19) 0.003(15) C23 0.058(19) 0.052(19) 0.06(2) 0.012(16) 0.002(15) -0.003(15) C24 0.10(3) 0.06(2) 0.10(3) -0.02(2) 0.02(2) 0.00(2) C25 0.09(3) 0.08(3) 0.09(3) 0.03(2) -0.01(2) 0.00(2) B1 0.09(3) 0.039(19) 0.034(18) 0.008(13) -0.006(18) -0.006(18) F1 0.30(5) 0.059(16) 0.24(4) -0.05(2) -0.12(4) 0.08(2) F2 0.42(7) 0.066(17) 0.22(4) 0.02(2) -0.20(4) -0.05(3) F3 0.23(3) 0.18(3) 0.060(15) -0.028(16) -0.072(19) 0.05(3) F4 0.39(8) 0.51(11) 0.19(5) 0.10(6) 0.19(5) 0.19(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 N1 1.99(2) . ? Au1 N3 1.99(2) . ? N1 N2 1.32(3) . ? N1 C11 1.35(3) . ? N2 C13 1.32(4) . ? C11 C12 1.39(4) . ? C11 C14 1.46(4) . ? C12 C13 1.36(4) . ? C13 C15 1.49(5) . ? N3 C21 1.32(3) . ? N3 N4 1.33(3) . ? N4 C23 1.31(4) . ? C21 C22 1.38(4) . ? C21 C24 1.52(4) . ? C22 C23 1.30(4) . ? C23 C25 1.48(5) . ? B1 F2 1.3041 . ? B1 F3 1.3044 . ? B1 F1 1.3045 . ? B1 F4 1.3089 . ? 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 Au1 N3 177.1(9) . . ? N2 N1 C11 106(2) . . ? N2 N1 Au1 120.5(17) . . ? C11 N1 Au1 133.3(19) . . ? C13 N2 N1 113(2) . . ? N1 C11 C12 108(3) . . ? N1 C11 C14 123(3) . . ? C12 C11 C14 129(3) . . ? C13 C12 C11 107(3) . . ? N2 C13 C12 106(3) . . ? N2 C13 C15 124(3) . . ? C12 C13 C15 130(3) . . ? C21 N3 N4 104(2) . . ? C21 N3 Au1 135(2) . . ? N4 N3 Au1 120.2(17) . . ? C23 N4 N3 113(2) . . ? N3 C21 C22 109(2) . . ? N3 C21 C24 118(3) . . ? C22 C21 C24 133(3) . . ? C23 C22 C21 107(3) . . ? C22 C23 N4 107(3) . . ? C22 C23 C25 130(3) . . ? N4 C23 C25 123(3) . . ? F2 B1 F3 109.6 . . ? F2 B1 F1 109.5 . . ? F3 B1 F1 109.5 . . ? F2 B1 F4 109.3 . . ? F3 B1 F4 109.5 . . ? F1 B1 F4 109.5 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 23.43 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 3.445 _refine_diff_density_min -1.528 _refine_diff_density_rms 0.293 #===END data_Compound_4.H2O_(vg37a) _database_code_depnum_ccdc_archive 'CCDC 708797' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H36 Au2 N10 O8' _chemical_formula_weight 938.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 19.284(4) _cell_length_b 11.856(2) _cell_length_c 13.920(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.91(3) _cell_angle_gamma 90.00 _cell_volume 3102.2(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PRISM _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.009 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 9.504 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.273142 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14308 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 23.33 _reflns_number_total 4473 _reflns_number_gt 3462 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0744P)^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 4473 _refine_ls_number_parameters 355 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0475 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.1240 _refine_ls_wR_factor_gt 0.1181 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.213146(18) 0.29921(3) 0.12267(2) 0.04641(17) Uani 1 1 d . . . N1 N 0.1424(4) 0.4218(5) 0.1197(5) 0.0476(18) Uani 1 1 d . . . N2 N 0.0734(4) 0.4016(6) 0.1200(5) 0.0515(19) Uani 1 1 d . . . H2 H 0.0551 0.3352 0.1158 0.062 Uiso 1 1 calc R . . N3 N 0.2863(4) 0.1799(5) 0.1227(5) 0.0429(16) Uani 1 1 d . . . N4 N 0.2732(4) 0.0694(6) 0.1201(5) 0.0457(17) Uani 1 1 d . . . H4 H 0.2321 0.0403 0.1191 0.055 Uiso 1 1 calc R . . C11 C 0.1496(5) 0.5331(8) 0.1262(6) 0.054(2) Uani 1 1 d . . . C12 C 0.0838(6) 0.5826(7) 0.1299(7) 0.061(3) Uani 1 1 d . . . H12 H 0.0746 0.6594 0.1332 0.073 Uiso 1 1 calc R . . C13 C 0.0362(5) 0.4968(7) 0.1277(6) 0.056(3) Uani 1 1 d . . . C14 C 0.2196(5) 0.5854(9) 0.1293(8) 0.075(3) Uani 1 1 d . . . H14A H 0.2562 0.5292 0.1456 0.112 Uiso 1 1 calc R . . H14B H 0.2281 0.6438 0.1784 0.112 Uiso 1 1 calc R . . H14C H 0.2201 0.6173 0.0661 0.112 Uiso 1 1 calc R . . C15 C -0.0403(5) 0.4930(8) 0.1338(8) 0.075(3) Uani 1 1 d . . . H15A H -0.0583 0.4178 0.1203 0.113 Uiso 1 1 calc R . . H15B H -0.0674 0.5441 0.0864 0.113 Uiso 1 1 calc R . . H15C H -0.0443 0.5147 0.1988 0.113 Uiso 1 1 calc R . . C21 C 0.3550(5) 0.1884(7) 0.1225(6) 0.048(2) Uani 1 1 d . . . C22 C 0.3854(5) 0.0858(7) 0.1213(6) 0.049(2) Uani 1 1 d . . . H22 H 0.4328 0.0701 0.1217 0.059 Uiso 1 1 calc R . . C23 C 0.3312(5) 0.0098(7) 0.1193(6) 0.053(2) Uani 1 1 d . . . C24 C 0.3899(6) 0.3027(8) 0.1263(8) 0.065(3) Uani 1 1 d . . . H24A H 0.3793 0.3357 0.0616 0.097 Uiso 1 1 calc R . . H24B H 0.4404 0.2945 0.1487 0.097 Uiso 1 1 calc R . . H24C H 0.3721 0.3507 0.1708 0.097 Uiso 1 1 calc R . . C25 C 0.3324(2) -0.1158(3) 0.1219(8) 0.075(3) Uani 1 1 d . . . H25A H 0.2949 -0.1426 0.1511 0.113 Uiso 1 1 calc R . . H25B H 0.3774 -0.1411 0.1602 0.113 Uiso 1 1 calc R . . H25C H 0.3256 -0.1445 0.0560 0.113 Uiso 1 1 calc R . . N5 N 0.1136(2) -0.0688(3) 0.1268(3) 0.059(2) Uani 1 1 d R . . O1 O 0.1306(2) 0.0323(3) 0.1438(3) 0.075(2) Uani 1 1 d R . . O2 O 0.0509(2) -0.0960(3) 0.1072(3) 0.087(2) Uani 1 1 d R . . O3 O 0.1611(2) -0.1370(3) 0.1301(3) 0.109(3) Uani 1 1 d R . . O11 O 0.0207(4) 0.1866(5) 0.0834(6) 0.075(2) Uani 1 1 d G . . H11A H 0.0560 0.1319 0.1027 0.07(3) Uiso 1 1 d G . . H11B H -0.0030 0.1671 0.0225 0.07(3) Uiso 1 1 d G . . Au51 Au 0.284749(19) 0.28462(3) 0.36829(2) 0.05002(17) Uani 1 1 d . . . N53 N 0.2124(4) 0.4049(6) 0.3710(5) 0.0468(18) Uani 1 1 d . . . N54 N 0.2254(4) 0.5162(6) 0.3766(5) 0.0484(18) Uani 1 1 d . . . H54 H 0.2662 0.5458 0.3769 0.058 Uiso 1 1 calc R . . N51 N 0.3565(4) 0.1619(6) 0.3697(5) 0.0523(19) Uani 1 1 d . . . N52 N 0.4246(4) 0.1841(6) 0.3691(5) 0.0504(19) Uani 1 1 d . . . H52 H 0.4420 0.2506 0.3674 0.061 Uiso 1 1 calc R . . C72 C 0.1438(5) 0.3939(7) 0.3699(6) 0.047(2) Uani 1 1 d . . . C73 C 0.1157(5) 0.4986(8) 0.3785(6) 0.054(2) Uani 1 1 d . . . H73A H 0.0690 0.5142 0.3816 0.065 Uiso 1 1 calc R . . C74 C 0.1680(5) 0.5749(7) 0.3816(6) 0.051(2) Uani 1 1 d . . . C75 C 0.1088(6) 0.2794(8) 0.3659(9) 0.068(3) Uani 1 1 d . . . H75A H 0.1235 0.2337 0.3171 0.101 Uiso 1 1 calc R . . H75B H 0.0581 0.2883 0.3490 0.101 Uiso 1 1 calc R . . H75C H 0.1227 0.2436 0.4292 0.101 Uiso 1 1 calc R . . C76 C 0.1685(6) 0.7007(8) 0.3851(8) 0.075(3) Uani 1 1 d . . . H76A H 0.1710 0.7253 0.4515 0.113 Uiso 1 1 calc R . . H76B H 0.1258 0.7292 0.3430 0.113 Uiso 1 1 calc R . . H76C H 0.2090 0.7287 0.3631 0.113 Uiso 1 1 calc R . . C71 C 0.3518(6) 0.0477(8) 0.3716(6) 0.059(3) Uani 1 1 d . . . C62 C 0.4151(6) 0.0013(8) 0.3728(7) 0.063(3) Uani 1 1 d . . . H62 H 0.4253 -0.0754 0.3743 0.076 Uiso 1 1 calc R . . C63 C 0.4619(5) 0.0876(8) 0.3713(7) 0.058(3) Uani 1 1 d . . . C64 C 0.2818(5) -0.0065(9) 0.3736(7) 0.074(3) Uani 1 1 d . . . H64A H 0.2713 0.0048 0.4372 0.111 Uiso 1 1 calc R . . H64B H 0.2844 -0.0858 0.3611 0.111 Uiso 1 1 calc R . . H64C H 0.2450 0.0269 0.3239 0.111 Uiso 1 1 calc R . . C65 C 0.5395(3) 0.0926(4) 0.3660(9) 0.091(4) Uani 1 1 d . . . H65A H 0.5686 0.0658 0.4269 0.136 Uiso 1 1 calc R . . H65B H 0.5521 0.1691 0.3551 0.136 Uiso 1 1 calc R . . H65C H 0.5469 0.0462 0.3127 0.136 Uiso 1 1 calc R . . N55 N 0.3860(2) 0.6563(4) 0.3782(3) 0.064(2) Uani 1 1 d R . . O51 O 0.3709(2) 0.5557(4) 0.3772(3) 0.099(3) Uani 1 1 d R . . O52 O 0.4486(2) 0.6862(4) 0.4031(3) 0.112(3) Uani 1 1 d R . . O53 O 0.3393(2) 0.7229(4) 0.3541(3) 0.121(4) Uani 1 1 d R . . O61 O 0.4789(4) 0.3944(6) 0.4016(7) 0.079(2) Uani 1 1 d G . . H61A H 0.4468 0.4352 0.3808 0.03(2) Uiso 1 1 d G . . H61B H 0.4966 0.4032 0.4629 0.07(4) Uiso 1 1 d G . . 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 0.0472(3) 0.0419(3) 0.0476(3) -0.00107(13) 0.00520(18) 0.00076(14) N1 0.056(5) 0.039(4) 0.046(4) -0.001(3) 0.006(3) 0.002(3) N2 0.059(5) 0.037(4) 0.056(5) 0.001(3) 0.006(4) 0.001(4) N3 0.045(5) 0.037(4) 0.048(4) 0.000(3) 0.013(3) -0.002(3) N4 0.036(4) 0.046(5) 0.057(4) -0.003(3) 0.015(3) -0.004(3) C11 0.070(7) 0.042(5) 0.047(5) -0.002(4) 0.006(4) -0.011(5) C12 0.086(8) 0.028(5) 0.067(6) -0.003(4) 0.013(5) 0.010(5) C13 0.071(7) 0.040(6) 0.052(6) -0.004(4) 0.000(5) 0.015(5) C14 0.085(9) 0.058(7) 0.087(8) -0.001(5) 0.031(6) -0.006(5) C15 0.064(7) 0.067(7) 0.095(8) -0.004(5) 0.018(6) 0.022(5) C21 0.045(6) 0.048(6) 0.049(5) 0.003(4) 0.007(4) -0.015(4) C22 0.039(5) 0.050(6) 0.059(5) 0.001(4) 0.013(4) 0.002(4) C23 0.051(6) 0.054(6) 0.054(5) 0.000(4) 0.011(4) 0.002(5) C24 0.060(7) 0.058(7) 0.075(7) 0.007(5) 0.013(5) -0.012(5) C25 0.072(7) 0.051(6) 0.107(9) -0.005(5) 0.031(6) 0.002(5) N5 0.048(5) 0.058(6) 0.074(5) -0.003(4) 0.018(4) -0.003(4) O1 0.056(4) 0.056(4) 0.111(6) -0.005(4) 0.016(4) -0.014(4) O2 0.045(4) 0.095(6) 0.123(6) -0.024(4) 0.022(4) -0.024(4) O3 0.073(6) 0.067(5) 0.191(9) -0.009(5) 0.040(5) 0.013(4) O11 0.063(5) 0.050(4) 0.106(6) -0.008(4) 0.007(4) -0.009(4) Au51 0.0504(3) 0.0500(3) 0.0489(3) -0.00184(14) 0.00948(18) 0.00081(15) N53 0.038(5) 0.050(5) 0.051(4) -0.002(3) 0.007(3) 0.001(3) N54 0.046(5) 0.040(4) 0.057(4) -0.003(3) 0.008(3) -0.009(3) N51 0.063(6) 0.047(5) 0.048(4) 0.001(3) 0.014(4) -0.002(4) N52 0.057(5) 0.040(4) 0.052(4) 0.002(3) 0.008(4) 0.001(4) C72 0.048(6) 0.053(6) 0.037(5) 0.005(4) 0.005(4) -0.005(4) C73 0.039(6) 0.064(6) 0.059(6) 0.000(4) 0.012(4) 0.003(5) C74 0.046(6) 0.051(6) 0.054(5) -0.001(4) 0.009(4) 0.007(4) C75 0.056(7) 0.051(6) 0.093(8) 0.007(5) 0.012(6) -0.016(5) C76 0.081(8) 0.056(7) 0.086(8) -0.004(5) 0.013(6) 0.002(5) C71 0.081(8) 0.048(6) 0.048(5) 0.005(4) 0.015(5) -0.003(5) C62 0.080(8) 0.040(6) 0.068(6) 0.004(4) 0.015(5) 0.016(5) C63 0.066(7) 0.043(6) 0.062(6) 0.003(4) 0.008(5) 0.011(5) C64 0.087(9) 0.061(7) 0.077(7) 0.001(5) 0.027(6) -0.009(6) C65 0.082(9) 0.058(7) 0.127(10) -0.003(6) 0.013(7) 0.022(6) N55 0.049(6) 0.053(5) 0.092(6) 0.005(4) 0.018(4) -0.002(4) O51 0.057(5) 0.063(5) 0.178(9) 0.020(5) 0.030(5) -0.005(4) O52 0.052(5) 0.105(7) 0.174(9) 0.001(6) 0.014(5) -0.022(5) O53 0.075(6) 0.073(6) 0.205(11) 0.028(6) 0.008(6) 0.019(5) O61 0.054(5) 0.059(5) 0.116(7) -0.007(4) 0.003(4) -0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 N1 1.987(7) . ? Au1 N3 1.997(7) . ? N1 C11 1.327(10) . ? N1 N2 1.353(10) . ? N2 C13 1.355(11) . ? N3 C21 1.328(10) . ? N3 N4 1.334(9) . ? N4 C23 1.326(11) . ? C11 C12 1.410(13) . ? C11 C14 1.477(13) . ? C12 C13 1.367(13) . ? C13 C15 1.497(13) . ? C21 C22 1.352(12) . ? C21 C24 1.509(12) . ? C22 C23 1.376(12) . ? C23 C25 1.490(9) . ? N5 O3 1.2158 . ? N5 O2 1.2220 . ? N5 O1 1.2517 . ? Au51 N53 2.001(7) . ? Au51 N51 2.005(7) . ? N53 C72 1.327(10) . ? N53 N54 1.342(9) . ? N54 C74 1.322(11) . ? N51 N52 1.340(10) . ? N51 C71 1.358(11) . ? N52 C63 1.348(11) . ? C72 C73 1.371(12) . ? C72 C75 1.510(12) . ? C73 C74 1.350(12) . ? C74 C76 1.492(12) . ? C71 C62 1.335(13) . ? C71 C64 1.501(13) . ? C62 C63 1.368(13) . ? C63 C65 1.516(11) . ? N55 O53 1.1889 . ? N55 O51 1.2274 . ? N55 O52 1.2312 . ? 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 Au1 N3 177.7(3) . . ? C11 N1 N2 105.3(7) . . ? C11 N1 Au1 131.6(7) . . ? N2 N1 Au1 122.8(5) . . ? N1 N2 C13 113.1(7) . . ? C21 N3 N4 104.9(7) . . ? C21 N3 Au1 130.6(6) . . ? N4 N3 Au1 124.5(5) . . ? C23 N4 N3 111.6(7) . . ? N1 C11 C12 109.6(8) . . ? N1 C11 C14 120.0(9) . . ? C12 C11 C14 130.4(9) . . ? C13 C12 C11 107.1(8) . . ? N2 C13 C12 104.8(9) . . ? N2 C13 C15 121.8(8) . . ? C12 C13 C15 133.4(8) . . ? N3 C21 C22 111.6(7) . . ? N3 C21 C24 120.3(8) . . ? C22 C21 C24 128.1(9) . . ? C21 C22 C23 105.0(8) . . ? N4 C23 C22 106.9(8) . . ? N4 C23 C25 122.7(8) . . ? C22 C23 C25 130.3(8) . . ? O3 N5 O2 122.2 . . ? O3 N5 O1 117.8 . . ? O2 N5 O1 120.0 . . ? N53 Au51 N51 178.1(3) . . ? C72 N53 N54 105.7(7) . . ? C72 N53 Au51 128.8(6) . . ? N54 N53 Au51 125.5(6) . . ? C74 N54 N53 111.9(7) . . ? N52 N51 C71 105.4(8) . . ? N52 N51 Au51 122.2(5) . . ? C71 N51 Au51 132.4(7) . . ? N51 N52 C63 110.6(7) . . ? N53 C72 C73 108.8(8) . . ? N53 C72 C75 121.7(8) . . ? C73 C72 C75 129.4(9) . . ? C74 C73 C72 107.6(8) . . ? N54 C74 C73 105.9(8) . . ? N54 C74 C76 122.0(9) . . ? C73 C74 C76 132.1(9) . . ? C62 C71 N51 110.3(9) . . ? C62 C71 C64 130.3(10) . . ? N51 C71 C64 119.4(9) . . ? C71 C62 C63 107.2(9) . . ? N52 C63 C62 106.5(9) . . ? N52 C63 C65 119.5(8) . . ? C62 C63 C65 133.8(8) . . ? O53 N55 O51 118.6 . . ? O53 N55 O52 121.4 . . ? O51 N55 O52 119.9 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.33 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.122 _refine_diff_density_min -1.558 _refine_diff_density_rms 0.171 #===END