data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'A L Balch' 'Marylin Olmstead' 'Daniel Rios' _publ_contact_author_name 'A L Balch' _publ_contact_author_email ALBALCH@UCDAVIS.EDU _publ_section_title ; Colorless, Non-Luminescent; Colorless, Luminescent; and Yellow, Luminescent Crystals of the Cation [Au{C(NHCH3)(NHCH2CH2OH)}2]+. The Roles of Anions and Hydrogen Bonding in Determining the Aggregation of Two-Coordinate Gold(I) Cations ; # Attachment 'DR123_2.CIF' data_dr123 _database_code_depnum_ccdc_archive 'CCDC 686038' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Au{c(NHCH3)(NHCH2CH2OH)}2]AsF6' _chemical_melting_point ? _chemical_formula_moiety 'C8 H20 Au N4 O2, As F6' _chemical_formula_sum 'C8 H20 As Au F6 N4 O2' _chemical_formula_weight 590.17 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' As As 0.0499 2.0058 '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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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' '-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 12.8324(16) _cell_length_b 21.471(3) _cell_length_c 12.9356(16) _cell_angle_alpha 90.00 _cell_angle_beta 105.233(2) _cell_angle_gamma 90.00 _cell_volume 3438.9(7) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5921 _cell_measurement_theta_min 3.288 _cell_measurement_theta_max 28.02 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.280 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224 _exptl_absorpt_coefficient_mu 10.557 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2055 _exptl_absorpt_correction_T_max 0.3870 _exptl_absorpt_process_details 'SADABS 2.10 (Sheldrick, 2003)' _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 'Bruker SMART 1000' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22189 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 28.10 _reflns_number_total 4161 _reflns_number_gt 3667 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2007)' _computing_cell_refinement SAINT _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXS-97 _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^)+(0.0371P)^2^+4.0672P] 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 4161 _refine_ls_number_parameters 202 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0284 _refine_ls_R_factor_gt 0.0233 _refine_ls_wR_factor_ref 0.0649 _refine_ls_wR_factor_gt 0.0621 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.548609(10) 0.006798(6) 0.149608(10) 0.04182(6) Uani 1 1 d . . . As1 As 1.0000 0.11396(3) 0.7500 0.05147(13) Uani 1 2 d S . . As2 As 1.0000 0.19205(3) 0.2500 0.06541(18) Uani 1 2 d S . . F1 F 0.9487(3) 0.16940(18) 0.6579(4) 0.1262(14) Uani 1 1 d . . . F2 F 0.9501(3) 0.05604(17) 0.6609(2) 0.1023(10) Uani 1 1 d . . . F3 F 1.1162(3) 0.1123(2) 0.7134(4) 0.1331(15) Uani 1 1 d . . . F4 F 1.0673(2) 0.13578(17) 0.3325(3) 0.0970(10) Uani 1 1 d . . . F5 F 0.9011(2) 0.19237(15) 0.3179(3) 0.0940(9) Uani 1 1 d . . . F6 F 0.9328(3) 0.24799(19) 0.1665(4) 0.153(2) Uani 1 1 d . . . O1 O 0.7835(2) 0.04091(15) 0.4704(2) 0.0605(7) Uani 1 1 d . . . H1A H 0.8156 0.0449 0.5338 0.091 Uiso 1 1 calc R . . O2 O 0.6402(2) -0.14601(16) -0.0463(2) 0.0618(7) Uani 1 1 d . . . H2B H 0.6805 -0.1160 -0.0427 0.093 Uiso 1 1 calc R . . N1 N 0.5810(2) 0.14200(16) 0.1672(2) 0.0490(7) Uani 1 1 d . . . H1B H 0.5157 0.1403 0.1276 0.059 Uiso 1 1 calc R . . N2 N 0.7316(2) 0.09060(14) 0.2545(2) 0.0467(6) Uani 1 1 d . . . H2A H 0.7589 0.1268 0.2727 0.056 Uiso 1 1 calc R . . N3 N 0.3582(2) -0.07223(16) 0.0758(2) 0.0484(7) Uani 1 1 d . . . H3C H 0.3281 -0.0364 0.0755 0.058 Uiso 1 1 calc R . . N4 N 0.5116(2) -0.12918(15) 0.1096(2) 0.0477(7) Uani 1 1 d . . . H4A H 0.4697 -0.1611 0.0954 0.057 Uiso 1 1 calc R . . C1 C 0.6257(3) 0.20351(19) 0.1951(4) 0.0608(10) Uani 1 1 d . . . H1C H 0.5708 0.2343 0.1689 0.091 Uiso 1 1 calc R . . H1D H 0.6846 0.2101 0.1635 0.091 Uiso 1 1 calc R . . H1E H 0.6514 0.2069 0.2716 0.091 Uiso 1 1 calc R . . C2 C 0.6299(2) 0.08842(16) 0.1960(2) 0.0399(7) Uani 1 1 d . . . C3 C 0.8004(3) 0.03720(19) 0.2905(3) 0.0528(9) Uani 1 1 d . . . H3A H 0.8521 0.0337 0.2480 0.063 Uiso 1 1 calc R . . H3B H 0.7566 -0.0003 0.2794 0.063 Uiso 1 1 calc R . . C4 C 0.8598(3) 0.0420(2) 0.4067(3) 0.0595(10) Uani 1 1 d . . . H4B H 0.9099 0.0075 0.4265 0.071 Uiso 1 1 calc R . . H4C H 0.9009 0.0805 0.4193 0.071 Uiso 1 1 calc R . . C5 C 0.2849(3) -0.1251(2) 0.0448(3) 0.0566(10) Uani 1 1 d . . . H5A H 0.2115 -0.1109 0.0302 0.085 Uiso 1 1 calc R . . H5B H 0.2985 -0.1550 0.1020 0.085 Uiso 1 1 calc R . . H5C H 0.2965 -0.1442 -0.0184 0.085 Uiso 1 1 calc R . . C6 C 0.4658(2) -0.07261(18) 0.1047(2) 0.0401(7) Uani 1 1 d . . . C7 C 0.6286(3) -0.1400(2) 0.1377(3) 0.0555(9) Uani 1 1 d . . . H7A H 0.6496 -0.1625 0.2051 0.067 Uiso 1 1 calc R . . H7B H 0.6656 -0.1002 0.1478 0.067 Uiso 1 1 calc R . . C8 C 0.6634(3) -0.1764(2) 0.0537(3) 0.0566(9) Uani 1 1 d . . . H8A H 0.7405 -0.1839 0.0779 0.068 Uiso 1 1 calc R . . H8B H 0.6274 -0.2166 0.0449 0.068 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 Au1 0.04198(9) 0.04648(9) 0.03694(9) -0.00085(5) 0.01025(6) -0.00746(5) As1 0.0377(2) 0.0517(3) 0.0596(3) 0.000 0.0033(2) 0.000 As2 0.0393(3) 0.0414(3) 0.1140(5) 0.000 0.0172(3) 0.000 F1 0.113(3) 0.091(3) 0.149(3) 0.055(2) -0.011(2) 0.004(2) F2 0.118(2) 0.096(2) 0.0712(18) -0.0166(16) -0.0133(16) -0.017(2) F3 0.080(2) 0.155(4) 0.186(4) 0.004(3) 0.073(2) -0.006(2) F4 0.0819(19) 0.103(3) 0.099(2) 0.0148(19) 0.0119(16) 0.0281(18) F5 0.0651(16) 0.082(2) 0.144(3) -0.0253(19) 0.0436(17) -0.0073(15) F6 0.090(2) 0.106(3) 0.267(5) 0.099(3) 0.058(3) 0.046(2) O1 0.0530(14) 0.074(2) 0.0494(14) -0.0039(13) 0.0038(11) 0.0012(13) O2 0.0454(14) 0.080(2) 0.0586(16) 0.0062(14) 0.0119(12) -0.0111(13) N1 0.0411(14) 0.0515(18) 0.0523(17) 0.0009(13) 0.0087(12) -0.0008(13) N2 0.0429(14) 0.0393(15) 0.0536(16) -0.0023(12) 0.0050(12) -0.0016(12) N3 0.0422(14) 0.0560(18) 0.0473(15) -0.0073(13) 0.0121(12) -0.0045(13) N4 0.0374(14) 0.0536(18) 0.0500(16) -0.0043(13) 0.0079(12) -0.0080(12) C1 0.065(2) 0.044(2) 0.073(3) -0.0018(19) 0.017(2) 0.0047(18) C2 0.0393(15) 0.0456(18) 0.0366(15) 0.0006(13) 0.0133(12) -0.0040(13) C3 0.0462(18) 0.055(2) 0.056(2) -0.0006(17) 0.0101(16) 0.0077(16) C4 0.0391(17) 0.070(3) 0.063(2) -0.0004(19) 0.0018(16) 0.0026(17) C5 0.0412(18) 0.073(3) 0.056(2) -0.0107(19) 0.0131(16) -0.0135(17) C6 0.0350(14) 0.063(2) 0.0231(13) -0.0063(12) 0.0086(11) -0.0068(14) C7 0.0426(18) 0.068(3) 0.051(2) -0.0002(18) 0.0035(15) -0.0007(17) C8 0.0457(19) 0.056(2) 0.064(2) 0.0038(18) 0.0073(17) 0.0058(16) _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 C6 2.012(3) . ? Au1 C2 2.047(3) . ? Au1 Au1 3.1630(4) 2_655 ? As1 F3 1.679(3) . ? As1 F3 1.679(3) 2_756 ? As1 F1 1.690(3) 2_756 ? As1 F1 1.690(3) . ? As1 F2 1.702(3) . ? As1 F2 1.702(3) 2_756 ? As2 F4 1.691(3) 2_755 ? As2 F4 1.691(3) . ? As2 F6 1.692(3) 2_755 ? As2 F6 1.692(3) . ? As2 F5 1.723(3) 2_755 ? As2 F5 1.723(3) . ? O1 C4 1.436(5) . ? O1 H1A 0.8200 . ? O2 C8 1.410(5) . ? O2 H2B 0.8200 . ? N1 C2 1.316(5) . ? N1 C1 1.448(5) . ? N1 H1B 0.8600 . ? N2 C2 1.327(4) . ? N2 C3 1.447(5) . ? N2 H2A 0.8600 . ? N3 C6 1.333(4) . ? N3 C5 1.462(5) . ? N3 H3C 0.8600 . ? N4 C6 1.344(5) . ? N4 C7 1.466(4) . ? N4 H4A 0.8600 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C1 H1E 0.9600 . ? C3 C4 1.499(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C7 C8 1.500(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 Au1 C2 178.74(12) . . ? C6 Au1 Au1 86.84(8) . 2_655 ? C2 Au1 Au1 92.28(8) . 2_655 ? F3 As1 F3 177.5(3) . 2_756 ? F3 As1 F1 90.2(2) . 2_756 ? F3 As1 F1 91.5(2) 2_756 2_756 ? F3 As1 F1 91.5(2) . . ? F3 As1 F1 90.2(2) 2_756 . ? F1 As1 F1 90.4(3) 2_756 . ? F3 As1 F2 89.8(2) . . ? F3 As1 F2 88.4(2) 2_756 . ? F1 As1 F2 177.8(2) 2_756 . ? F1 As1 F2 91.7(2) . . ? F3 As1 F2 88.4(2) . 2_756 ? F3 As1 F2 89.8(2) 2_756 2_756 ? F1 As1 F2 91.7(2) 2_756 2_756 ? F1 As1 F2 177.8(2) . 2_756 ? F2 As1 F2 86.1(2) . 2_756 ? F4 As2 F4 88.8(3) 2_755 . ? F4 As2 F6 179.5(2) 2_755 2_755 ? F4 As2 F6 90.8(2) . 2_755 ? F4 As2 F6 90.8(2) 2_755 . ? F4 As2 F6 179.5(2) . . ? F6 As2 F6 89.6(4) 2_755 . ? F4 As2 F5 90.18(17) 2_755 2_755 ? F4 As2 F5 90.14(15) . 2_755 ? F6 As2 F5 90.17(19) 2_755 2_755 ? F6 As2 F5 89.51(18) . 2_755 ? F4 As2 F5 90.14(15) 2_755 . ? F4 As2 F5 90.18(17) . . ? F6 As2 F5 89.51(18) 2_755 . ? F6 As2 F5 90.17(19) . . ? F5 As2 F5 179.5(2) 2_755 . ? C4 O1 H1A 109.5 . . ? C8 O2 H2B 109.5 . . ? C2 N1 C1 126.7(3) . . ? C2 N1 H1B 116.6 . . ? C1 N1 H1B 116.6 . . ? C2 N2 C3 125.5(3) . . ? C2 N2 H2A 117.2 . . ? C3 N2 H2A 117.2 . . ? C6 N3 C5 128.1(3) . . ? C6 N3 H3C 116.0 . . ? C5 N3 H3C 116.0 . . ? C6 N4 C7 124.2(3) . . ? C6 N4 H4A 117.9 . . ? C7 N4 H4A 117.9 . . ? N1 C1 H1C 109.5 . . ? N1 C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? N1 C1 H1E 109.5 . . ? H1C C1 H1E 109.5 . . ? H1D C1 H1E 109.5 . . ? N1 C2 N2 117.1(3) . . ? N1 C2 Au1 119.8(2) . . ? N2 C2 Au1 123.1(3) . . ? N2 C3 C4 112.0(3) . . ? N2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? N2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? O1 C4 C3 109.2(3) . . ? O1 C4 H4B 109.8 . . ? C3 C4 H4B 109.8 . . ? O1 C4 H4C 109.8 . . ? C3 C4 H4C 109.8 . . ? H4B C4 H4C 108.3 . . ? N3 C5 H5A 109.5 . . ? N3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 N4 115.3(3) . . ? N3 C6 Au1 120.4(3) . . ? N4 C6 Au1 124.1(2) . . ? N4 C7 C8 112.6(3) . . ? N4 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? N4 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? O2 C8 C7 113.1(3) . . ? O2 C8 H8A 109.0 . . ? C7 C8 H8A 109.0 . . ? O2 C8 H8B 109.0 . . ? C7 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? 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 O1 H1A F2 0.82 2.06 2.825(4) 154.9 . N1 H1B O2 0.86 2.00 2.859(4) 172.4 5_655 N4 H4A F6 0.86 2.26 2.985(5) 141.9 3_445 N2 H2A F5 0.86 2.26 3.040(4) 151.6 . O2 H2B O1 0.82 2.06 2.883(4) 178.6 6 N3 H3C O1 0.86 2.17 2.999(4) 161.5 2_655 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.10 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.103 _refine_diff_density_min -0.722 _refine_diff_density_rms 0.106 # Attachment 'DR89_1.CIF' data_dr89 _database_code_depnum_ccdc_archive 'CCDC 686039' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Au{C(NHCH3)(NHCH2CH2OH)}2]Cl' _chemical_melting_point ? _chemical_formula_moiety 'C8 H20 Au N4 O2, Cl' _chemical_formula_sum 'C8 H20 Au Cl N4 O2' _chemical_formula_weight 436.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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' '-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 12.807(3) _cell_length_b 6.7890(11) _cell_length_c 16.070(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.420(4) _cell_angle_gamma 90.00 _cell_volume 1325.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 881 _cell_measurement_theta_min 2.672 _cell_measurement_theta_max 31.139 _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.188 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 11.292 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1334 _exptl_absorpt_correction_T_max 0.4522 _exptl_absorpt_process_details 'SADABS 2.10 (sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8082 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1534 _reflns_number_gt 1204 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.054 (Bruker, 2003)' _computing_cell_refinement SAINT _computing_data_reduction 'SAINT 6.45A (Bruker, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1 XP (Sheldrick, 1994)' _computing_publication_material 'SHELXS-97 (Sheldrick, 1990)' _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 H atom on the OH group was located in a difference map and refined with a distance restraint of 0.84(1) \%A. All other H atoms were riding on their bonded C atoms. ; _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^)+(0.0244P)^2^+4.7952P] 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 1534 _refine_ls_number_parameters 80 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0298 _refine_ls_R_factor_gt 0.0187 _refine_ls_wR_factor_ref 0.0519 _refine_ls_wR_factor_gt 0.0450 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _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 0.5000 0.5000 0.5000 0.01248(8) Uani 1 2 d S . . Cl1 Cl 0.5000 0.2800(2) 0.2500 0.0163(3) Uani 1 2 d S . . O1 O 0.6866(3) 0.4075(4) 0.81171(17) 0.0179(6) Uani 1 1 d D . . H1 H 0.634(3) 0.484(6) 0.805(4) 0.035(18) Uiso 1 1 d D . . N1 N 0.6086(3) 0.1534(5) 0.4532(2) 0.0144(7) Uani 1 1 d . . . H1A H 0.5861 0.2120 0.4017 0.017 Uiso 1 1 calc R . . N2 N 0.6226(3) 0.1522(5) 0.5970(2) 0.0132(7) Uani 1 1 d . . . H2 H 0.6615 0.0438 0.6007 0.016 Uiso 1 1 calc R . . C1 C 0.5845(3) 0.2397(6) 0.5193(2) 0.0135(7) Uani 1 1 d . . . C2 C 0.6695(4) -0.0315(5) 0.4595(3) 0.0166(8) Uani 1 1 d . . . H2B H 0.6663 -0.0750 0.4006 0.025 Uiso 1 1 calc R . . H2C H 0.6365 -0.1323 0.4870 0.025 Uiso 1 1 calc R . . H2D H 0.7464 -0.0109 0.4950 0.025 Uiso 1 1 calc R . . C3 C 0.6038(3) 0.2250(6) 0.6766(2) 0.0144(8) Uani 1 1 d . . . H3A H 0.5989 0.1120 0.7142 0.017 Uiso 1 1 calc R . . H3B H 0.5329 0.2967 0.6607 0.017 Uiso 1 1 calc R . . C4 C 0.6955(3) 0.3610(6) 0.7274(2) 0.0154(8) Uani 1 1 d . . . H4A H 0.7674 0.2972 0.7349 0.018 Uiso 1 1 calc R . . H4B H 0.6926 0.4841 0.6938 0.018 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 Au1 0.01137(11) 0.01194(11) 0.01124(11) 0.00232(8) -0.00055(7) 0.00056(9) Cl1 0.0158(7) 0.0195(7) 0.0109(6) 0.000 0.0004(5) 0.000 O1 0.0195(16) 0.0198(16) 0.0117(13) -0.0019(12) 0.0012(12) 0.0002(13) N1 0.0175(18) 0.0141(16) 0.0098(15) 0.0011(12) 0.0019(13) 0.0007(14) N2 0.0161(17) 0.0115(15) 0.0104(15) -0.0017(12) 0.0020(13) 0.0003(13) C1 0.0117(19) 0.0125(18) 0.0141(17) 0.0010(14) 0.0009(15) -0.0032(15) C2 0.019(2) 0.013(2) 0.0170(19) -0.0023(14) 0.0054(16) -0.0003(15) C3 0.017(2) 0.0158(19) 0.0094(16) 0.0000(14) 0.0019(15) 0.0017(16) C4 0.016(2) 0.0146(19) 0.0143(18) -0.0021(15) 0.0037(16) -0.0006(16) _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 C1 2.044(4) 5_666 ? Au1 C1 2.044(4) . ? O1 C4 1.430(4) . ? O1 H1 0.83(4) . ? N1 C1 1.333(5) . ? N1 C2 1.465(5) . ? N1 H1A 0.8800 . ? N2 C1 1.328(5) . ? N2 C3 1.461(4) . ? N2 H2 0.8800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C2 H2D 0.9800 . ? C3 C4 1.514(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Au1 C1 180.000(1) 5_666 . ? C4 O1 H1 109(5) . . ? C1 N1 C2 125.0(3) . . ? C1 N1 H1A 117.5 . . ? C2 N1 H1A 117.5 . . ? C1 N2 C3 123.9(3) . . ? C1 N2 H2 118.0 . . ? C3 N2 H2 118.0 . . ? N2 C1 N1 116.3(3) . . ? N2 C1 Au1 123.3(3) . . ? N1 C1 Au1 120.2(3) . . ? N1 C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C2 H2D 109.5 . . ? H2B C2 H2D 109.5 . . ? H2C C2 H2D 109.5 . . ? N2 C3 C4 111.4(3) . . ? N2 C3 H3A 109.4 . . ? C4 C3 H3A 109.4 . . ? N2 C3 H3B 109.4 . . ? C4 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? O1 C4 C3 111.4(3) . . ? O1 C4 H4A 109.4 . . ? C3 C4 H4A 109.4 . . ? O1 C4 H4B 109.4 . . ? C3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? 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 O1 H1 Cl1 0.83(4) 2.31(5) 3.114(3) 163(6) 5_666 N1 H1A Cl1 0.88 2.38 3.235(3) 163 . N2 H2 O1 0.88 2.21 2.936(4) 139 4_646 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.307 _refine_diff_density_min -1.631 _refine_diff_density_rms 0.150 # Attachment 'dr60_1.cif' data_dr60 _database_code_depnum_ccdc_archive 'CCDC 686040' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Au{C(NHCH3)(NHCH2CH2OH)}2]3(AsF6)2Cl.0.5(H2O)2' _chemical_melting_point ? _chemical_formula_moiety ;3(C8 H20 Au N4 O2), 2(As F6), Cl, 0.5(H2O), 0.5(H2O) ; _chemical_formula_sum 'C24 H62 As2 Au3 Cl F12 N12 O7' _chemical_formula_weight 1635.06 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 9.373(4) _cell_length_b 20.654(9) _cell_length_c 24.579(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.651(8) _cell_angle_gamma 90.00 _cell_volume 4758(3) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 1013 _cell_measurement_theta_min 2.518 _cell_measurement_theta_max 30.427 _exptl_crystal_description Needle _exptl_crystal_colour yellow/green _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.280 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3088.0 _exptl_absorpt_coefficient_mu 10.762 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3635 _exptl_absorpt_correction_T_max 0.5848 _exptl_absorpt_process_details 'SADABS 2.10 (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50933 _diffrn_reflns_av_R_equivalents 0.0802 _diffrn_reflns_av_sigmaI/netI 0.0714 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10923 _reflns_number_gt 7842 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.054 (Bruker, 2003)' _computing_cell_refinement SAINT _computing_data_reduction 'SAINT 6.45A (Bruker, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material 'SHELXS-97 (Sheldrick, 1990)' _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. 041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?, this can be explained since the hydrogens could not be found for the waters at half occupancy. The thermal ellipsoid of atom C18 was given a restraint ISOR 0.005. ; _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^)+(0.0359P)^2^+43.5314P] 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 10923 _refine_ls_number_parameters 556 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0794 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1191 _refine_ls_wR_factor_gt 0.1109 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.004 _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 0.40891(3) 0.742917(15) 0.637902(13) 0.01430(9) Uani 1 1 d . . . Au2 Au 0.74083(3) 0.739442(15) 0.625537(13) 0.01452(9) Uani 1 1 d . . . Au3 Au 1.07527(4) 0.756571(16) 0.632093(13) 0.01660(9) Uani 1 1 d . . . As1 As 0.30316(10) 0.38402(4) 0.60565(4) 0.0185(2) Uani 1 1 d . . . As2 As 0.91786(10) 0.91233(4) 0.38092(4) 0.01716(19) Uani 1 1 d . . . Cl1 Cl 0.9036(2) 0.45888(10) 0.69308(9) 0.0209(5) Uani 1 1 d . . . F1 F 0.4034(7) 0.4555(3) 0.6054(3) 0.0386(16) Uani 1 1 d . . . F2 F 0.2101(6) 0.3122(2) 0.6074(2) 0.0292(13) Uani 1 1 d . . . F3 F 0.4551(6) 0.3429(3) 0.6277(2) 0.0314(13) Uani 1 1 d . . . F4 F 0.3479(6) 0.3694(3) 0.5392(2) 0.0311(13) Uani 1 1 d . . . F5 F 0.2618(6) 0.3966(2) 0.6731(2) 0.0263(12) Uani 1 1 d . . . F6 F 0.1547(7) 0.4258(3) 0.5848(2) 0.0406(16) Uani 1 1 d . . . F7 F 0.7357(6) 0.9163(3) 0.3805(3) 0.0466(18) Uani 1 1 d . . . F8 F 1.1004(7) 0.9098(4) 0.3810(3) 0.061(2) Uani 1 1 d . . . F9 F 0.9178(9) 0.8344(3) 0.4021(4) 0.075(3) Uani 1 1 d . . . F10 F 0.9204(9) 0.9378(4) 0.4473(3) 0.076(3) Uani 1 1 d . . . F11 F 0.9204(9) 0.9907(3) 0.3608(4) 0.077(3) Uani 1 1 d . . . F12 F 0.9185(8) 0.8873(4) 0.3153(3) 0.056(2) Uani 1 1 d . . . O1 O 0.7138(8) 0.7712(3) 0.7841(3) 0.039(2) Uani 1 1 d . . . H1 H 0.7760 0.7639 0.8082 0.059 Uiso 1 1 calc R . . O2 O 0.1117(6) 0.5744(3) 0.6905(2) 0.0197(13) Uani 1 1 d . . . H2 H 0.0530 0.5436 0.6907 0.030 Uiso 1 1 calc R . . O3 O 0.4384(7) 0.7799(4) 0.4869(3) 0.041(2) Uani 1 1 d . . . H3 H 0.3689 0.7827 0.4652 0.062 Uiso 1 1 calc R . . O4 O 1.0350(7) 0.5846(4) 0.5749(3) 0.0356(18) Uani 1 1 d . . . H4 H 1.0564 0.5818 0.6081 0.053 Uiso 1 1 calc R . . O5 O 1.3647(6) 0.8975(3) 0.5320(3) 0.0216(14) Uani 1 1 d . . . H5 H 1.4179 0.9301 0.5354 0.032 Uiso 1 1 calc R . . O6 O 0.8038(6) 0.8908(3) 0.7347(2) 0.0208(14) Uani 1 1 d . . . H6 H 0.7929 0.8563 0.7523 0.031 Uiso 1 1 calc R . . O7 O 0.2737(16) 0.7960(7) 0.3915(6) 0.038(4) Uiso 0.50 1 d P . . O8 O 0.5576(14) 0.9688(6) 0.4701(5) 0.025(3) Uiso 0.50 1 d P . . N1 N 0.4141(7) 0.8856(3) 0.6506(3) 0.0164(15) Uani 1 1 d . . . H1A H 0.3955 0.8830 0.6155 0.020 Uiso 1 1 calc R . . N2 N 0.4532(8) 0.8346(3) 0.7315(3) 0.0168(15) Uani 1 1 d . . . H2A H 0.4695 0.8733 0.7451 0.020 Uiso 1 1 calc R . . N3 N 0.3935(8) 0.6500(4) 0.5454(3) 0.0197(16) Uani 1 1 d . . . H3A H 0.4144 0.6853 0.5271 0.024 Uiso 1 1 calc R . . N4 N 0.3682(8) 0.6005(3) 0.6271(3) 0.0181(16) Uani 1 1 d . . . H4A H 0.3569 0.5644 0.6085 0.022 Uiso 1 1 calc R . . N5 N 0.7544(7) 0.8819(3) 0.6171(3) 0.0153(15) Uani 1 1 d . . . H5A H 0.7737 0.8771 0.6520 0.018 Uiso 1 1 calc R . . N6 N 0.7111(8) 0.8354(3) 0.5345(3) 0.0179(16) Uani 1 1 d . . . H6A H 0.7048 0.8752 0.5218 0.021 Uiso 1 1 calc R . . N7 N 0.7441(7) 0.6541(3) 0.7202(3) 0.0172(15) Uani 1 1 d . . . H7A H 0.7278 0.6921 0.7352 0.021 Uiso 1 1 calc R . . N8 N 0.7695(8) 0.5956(3) 0.6422(3) 0.0165(15) Uani 1 1 d . . . H8A H 0.7794 0.5614 0.6633 0.020 Uiso 1 1 calc R . . N9 N 1.0686(8) 0.7023(4) 0.5208(3) 0.031(2) Uani 1 1 d . . . H9A H 1.0478 0.6672 0.5394 0.037 Uiso 1 1 calc R . . N10 N 1.1059(8) 0.8118(4) 0.5198(3) 0.031(2) Uani 1 1 d . . . H10A H 1.1179 0.8081 0.4845 0.037 Uiso 1 1 calc R . . N11 N 1.0774(7) 0.7016(3) 0.7434(3) 0.0193(16) Uani 1 1 d . . . H11A H 1.0871 0.6659 0.7243 0.023 Uiso 1 1 calc R . . N12 N 1.0604(7) 0.8112(3) 0.7452(3) 0.0163(15) Uani 1 1 d . . . H12A H 1.0564 0.8077 0.7809 0.020 Uiso 1 1 calc R . . C1 C 0.4272(10) 0.9506(4) 0.6736(4) 0.021(2) Uani 1 1 d . . . H1B H 0.4096 0.9828 0.6450 0.032 Uiso 1 1 calc R . . H1C H 0.5236 0.9565 0.6887 0.032 Uiso 1 1 calc R . . H1D H 0.3572 0.9561 0.7026 0.032 Uiso 1 1 calc R . . C2 C 0.4276(8) 0.8295(4) 0.6779(4) 0.0147(17) Uani 1 1 d . . . C3 C 0.4557(11) 0.7783(4) 0.7692(4) 0.023(2) Uani 1 1 d . . . H3B H 0.4639 0.7379 0.7477 0.028 Uiso 1 1 calc R . . H3C H 0.3646 0.7766 0.7891 0.028 Uiso 1 1 calc R . . C4 C 0.5771(12) 0.7816(5) 0.8095(4) 0.032(3) Uani 1 1 d . . . H4B H 0.5769 0.8245 0.8274 0.039 Uiso 1 1 calc R . . H4C H 0.5629 0.7483 0.8380 0.039 Uiso 1 1 calc R . . C5 C 0.3684(11) 0.5911(4) 0.5133(4) 0.028(2) Uani 1 1 d . . . H5B H 0.3717 0.6016 0.4745 0.042 Uiso 1 1 calc R . . H5C H 0.2744 0.5733 0.5220 0.042 Uiso 1 1 calc R . . H5D H 0.4423 0.5590 0.5221 0.042 Uiso 1 1 calc R . . C6 C 0.3881(9) 0.6557(4) 0.5992(3) 0.0177(18) Uani 1 1 d . . . C7 C 0.3641(10) 0.5968(4) 0.6866(4) 0.0212(19) Uani 1 1 d . . . H7B H 0.3464 0.6406 0.7015 0.025 Uiso 1 1 calc R . . H7C H 0.4582 0.5821 0.7005 0.025 Uiso 1 1 calc R . . C8 C 0.2496(9) 0.5510(4) 0.7067(4) 0.0178(18) Uani 1 1 d . . . H8B H 0.2650 0.5073 0.6913 0.021 Uiso 1 1 calc R . . H8C H 0.2551 0.5477 0.7469 0.021 Uiso 1 1 calc R . . C9 C 0.7472(10) 0.9483(4) 0.5958(4) 0.0212(19) Uani 1 1 d . . . H9B H 0.7622 0.9791 0.6256 0.032 Uiso 1 1 calc R . . H9C H 0.6532 0.9557 0.5791 0.032 Uiso 1 1 calc R . . H9D H 0.8213 0.9544 0.5685 0.032 Uiso 1 1 calc R . . C10 C 0.7338(8) 0.8279(4) 0.5874(4) 0.0155(17) Uani 1 1 d . . . C11 C 0.6958(10) 0.7817(4) 0.4956(4) 0.0197(19) Uani 1 1 d . . . H11B H 0.6858 0.7407 0.5160 0.024 Uiso 1 1 calc R . . H11C H 0.7837 0.7787 0.4737 0.024 Uiso 1 1 calc R . . C12 C 0.5697(12) 0.7894(5) 0.4578(4) 0.033(2) Uani 1 1 d . . . H12B H 0.5705 0.8333 0.4416 0.039 Uiso 1 1 calc R . . H12C H 0.5759 0.7575 0.4279 0.039 Uiso 1 1 calc R . . C13 C 0.7591(10) 0.5988(4) 0.7570(4) 0.022(2) Uani 1 1 d . . . H13B H 0.7412 0.6128 0.7944 0.033 Uiso 1 1 calc R . . H13C H 0.8561 0.5814 0.7546 0.033 Uiso 1 1 calc R . . H13D H 0.6902 0.5652 0.7467 0.033 Uiso 1 1 calc R . . C14 C 0.7526(8) 0.6525(4) 0.6659(4) 0.0159(17) Uani 1 1 d . . . C15 C 0.7727(10) 0.5857(5) 0.5824(4) 0.023(2) Uani 1 1 d . . . H15B H 0.7695 0.6284 0.5641 0.028 Uiso 1 1 calc R . . H15C H 0.6867 0.5611 0.5710 0.028 Uiso 1 1 calc R . . C16 C 0.9059(11) 0.5491(5) 0.5643(4) 0.029(2) Uani 1 1 d . . . H16B H 0.9107 0.5070 0.5836 0.035 Uiso 1 1 calc R . . H16C H 0.8980 0.5400 0.5248 0.035 Uiso 1 1 calc R . . C17 C 1.0838(13) 0.6960(7) 0.4611(5) 0.050(3) Uani 1 1 d . . . H17B H 1.0618 0.6514 0.4501 0.076 Uiso 1 1 calc R . . H17C H 1.1820 0.7065 0.4510 0.076 Uiso 1 1 calc R . . H17D H 1.0178 0.7258 0.4427 0.076 Uiso 1 1 calc R . . C18 C 1.0841(9) 0.7575(5) 0.5482(4) 0.023(2) Uani 1 1 d U . . C19 C 1.1113(11) 0.8767(5) 0.5432(4) 0.031(2) Uani 1 1 d . . . H19B H 1.1321 0.8735 0.5827 0.037 Uiso 1 1 calc R . . H19C H 1.0170 0.8977 0.5385 0.037 Uiso 1 1 calc R . . C20 C 1.2244(10) 0.9180(5) 0.5165(4) 0.027(2) Uani 1 1 d . . . H20B H 1.2135 0.9151 0.4765 0.033 Uiso 1 1 calc R . . H20C H 1.2110 0.9638 0.5272 0.033 Uiso 1 1 calc R . . C21 C 1.0718(11) 0.6942(5) 0.8021(4) 0.028(2) Uani 1 1 d . . . H21B H 1.0842 0.6484 0.8116 0.043 Uiso 1 1 calc R . . H21C H 0.9792 0.7093 0.8151 0.043 Uiso 1 1 calc R . . H21D H 1.1482 0.7197 0.8191 0.043 Uiso 1 1 calc R . . C22 C 1.0694(9) 0.7564(4) 0.7155(4) 0.0165(17) Uani 1 1 d . . . C23 C 1.0568(9) 0.8762(4) 0.7213(4) 0.0173(18) Uani 1 1 d . . . H23B H 1.0378 0.8728 0.6817 0.021 Uiso 1 1 calc R . . H23C H 1.1510 0.8971 0.7265 0.021 Uiso 1 1 calc R . . C24 C 0.9422(9) 0.9179(4) 0.7472(4) 0.0193(18) Uani 1 1 d . . . H24B H 0.9572 0.9193 0.7871 0.023 Uiso 1 1 calc R . . H24C H 0.9480 0.9626 0.7330 0.023 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 Au1 0.00958(17) 0.01312(16) 0.02023(17) -0.00174(13) 0.00181(12) -0.00059(11) Au2 0.00977(17) 0.01223(15) 0.02160(17) 0.00415(13) 0.00190(12) 0.00225(12) Au3 0.01171(17) 0.01861(16) 0.01947(16) -0.00203(14) 0.00019(12) 0.00229(13) As1 0.0214(5) 0.0148(4) 0.0194(5) -0.0001(3) 0.0002(4) 0.0006(3) As2 0.0181(5) 0.0172(4) 0.0161(4) 0.0036(3) -0.0030(3) -0.0006(3) Cl1 0.0172(11) 0.0135(9) 0.0320(12) 0.0071(9) 0.0008(9) 0.0004(8) F1 0.050(4) 0.016(3) 0.049(4) -0.004(3) 0.019(3) -0.010(3) F2 0.035(3) 0.020(3) 0.032(3) -0.004(2) 0.000(3) -0.010(2) F3 0.031(3) 0.029(3) 0.034(3) -0.004(3) -0.009(3) 0.008(3) F4 0.041(4) 0.026(3) 0.027(3) -0.001(2) 0.008(3) 0.000(3) F5 0.033(3) 0.020(3) 0.026(3) -0.001(2) 0.002(2) 0.001(2) F6 0.051(4) 0.041(4) 0.029(3) 0.007(3) -0.001(3) 0.021(3) F7 0.012(3) 0.036(4) 0.092(6) -0.015(3) 0.002(3) 0.003(3) F8 0.024(4) 0.088(6) 0.070(5) -0.039(4) -0.005(3) -0.006(4) F9 0.097(6) 0.023(3) 0.108(7) 0.035(4) 0.069(5) 0.036(4) F10 0.082(6) 0.111(7) 0.035(4) -0.034(4) -0.024(4) 0.071(5) F11 0.090(6) 0.024(4) 0.119(8) 0.025(4) 0.033(6) -0.009(4) F12 0.054(5) 0.093(6) 0.021(3) -0.009(3) -0.015(3) 0.025(4) O1 0.043(5) 0.016(3) 0.058(5) 0.004(3) -0.028(4) 0.007(3) O2 0.018(3) 0.016(3) 0.025(3) 0.002(3) 0.001(3) -0.005(2) O3 0.025(4) 0.050(5) 0.049(5) -0.027(4) -0.016(4) 0.020(3) O4 0.028(4) 0.059(5) 0.019(4) 0.000(3) 0.000(3) 0.007(4) O5 0.018(3) 0.019(3) 0.028(4) 0.000(3) -0.007(3) -0.003(3) O6 0.018(3) 0.023(3) 0.022(3) -0.003(3) -0.006(3) 0.005(3) N1 0.019(4) 0.008(3) 0.021(4) 0.001(3) -0.001(3) 0.003(3) N2 0.020(4) 0.009(3) 0.022(4) 0.003(3) 0.002(3) 0.000(3) N3 0.020(4) 0.020(4) 0.019(4) 0.001(3) 0.000(3) -0.001(3) N4 0.020(4) 0.017(4) 0.017(4) -0.003(3) 0.003(3) -0.007(3) N5 0.015(4) 0.010(3) 0.020(4) 0.002(3) -0.004(3) 0.001(3) N6 0.024(4) 0.013(3) 0.016(4) 0.001(3) 0.000(3) -0.002(3) N7 0.017(4) 0.013(3) 0.022(4) 0.000(3) 0.006(3) 0.000(3) N8 0.024(4) 0.011(3) 0.015(4) 0.005(3) 0.003(3) 0.006(3) N9 0.012(4) 0.048(5) 0.033(5) -0.017(4) -0.013(3) 0.004(4) N10 0.017(4) 0.056(6) 0.020(4) 0.002(4) 0.001(3) 0.000(4) N11 0.011(4) 0.018(4) 0.029(4) 0.001(3) -0.006(3) 0.005(3) N12 0.015(4) 0.016(4) 0.019(4) 0.004(3) 0.003(3) 0.004(3) C1 0.022(5) 0.012(4) 0.030(5) -0.001(4) -0.004(4) 0.002(3) C2 0.004(4) 0.018(4) 0.022(5) 0.000(3) 0.001(3) 0.004(3) C3 0.036(6) 0.013(4) 0.021(5) 0.001(4) 0.011(4) 0.001(4) C4 0.067(8) 0.016(4) 0.014(5) 0.002(4) -0.008(5) -0.007(5) C5 0.030(6) 0.025(5) 0.030(6) -0.010(4) 0.004(4) 0.001(4) C6 0.009(4) 0.028(5) 0.017(4) 0.001(4) 0.002(3) 0.002(3) C7 0.020(5) 0.022(5) 0.022(5) 0.000(4) 0.004(4) -0.002(4) C8 0.019(5) 0.016(4) 0.019(5) 0.003(3) -0.002(4) -0.001(3) C9 0.022(5) 0.014(4) 0.027(5) -0.001(4) -0.006(4) -0.004(4) C10 0.004(4) 0.022(4) 0.021(5) 0.000(4) -0.003(3) 0.005(3) C11 0.021(5) 0.018(4) 0.020(5) -0.002(4) 0.007(4) 0.001(4) C12 0.055(7) 0.026(5) 0.017(5) -0.003(4) -0.004(5) 0.014(5) C13 0.030(5) 0.017(4) 0.019(5) 0.004(4) 0.011(4) -0.001(4) C14 0.007(4) 0.019(4) 0.022(5) 0.003(3) -0.005(3) 0.005(3) C15 0.021(5) 0.032(5) 0.017(5) 0.000(4) 0.000(4) 0.004(4) C16 0.035(6) 0.031(5) 0.021(5) 0.002(4) 0.001(4) 0.012(4) C17 0.040(7) 0.077(9) 0.033(7) -0.030(6) -0.015(5) 0.020(6) C18 0.012(3) 0.038(4) 0.019(3) -0.006(3) 0.000(3) 0.005(3) C19 0.022(5) 0.045(6) 0.025(5) 0.012(5) 0.003(4) 0.005(5) C20 0.023(5) 0.038(6) 0.021(5) 0.010(4) 0.004(4) 0.014(4) C21 0.029(6) 0.028(5) 0.028(5) 0.012(4) -0.004(4) -0.004(4) C22 0.007(4) 0.017(4) 0.026(5) -0.002(4) 0.007(3) 0.000(3) C23 0.018(5) 0.014(4) 0.020(5) 0.004(3) 0.005(4) -0.002(3) C24 0.016(5) 0.019(4) 0.023(5) -0.006(4) -0.002(4) 0.006(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 C6 2.046(9) . ? Au1 C2 2.048(8) . ? Au1 Au2 3.1301(14) . ? Au1 Au3 3.1415(14) 1_455 ? Au2 C10 2.053(8) . ? Au2 C14 2.053(8) . ? Au2 Au3 3.1569(14) . ? Au3 C22 2.051(9) . ? Au3 C18 2.066(9) . ? Au3 Au1 3.1415(14) 1_655 ? As1 F6 1.710(6) . ? As1 F4 1.716(6) . ? As1 F2 1.722(5) . ? As1 F5 1.727(5) . ? As1 F3 1.740(6) . ? As1 F1 1.750(5) . ? As2 F9 1.692(6) . ? As2 F11 1.693(7) . ? As2 F12 1.694(6) . ? As2 F7 1.709(6) . ? As2 F8 1.712(7) . ? As2 F10 1.714(7) . ? O1 C4 1.448(13) . ? O1 H1 0.8400 . ? O2 C8 1.432(10) . ? O2 H2 0.8400 . ? O3 C12 1.444(13) . ? O3 H3 0.8400 . ? O4 C16 1.436(12) . ? O4 H4 0.8400 . ? O5 C20 1.428(10) . ? O5 H5 0.8400 . ? O6 C24 1.443(10) . ? O6 H6 0.8400 . ? N1 C2 1.345(10) . ? N1 C1 1.461(10) . ? N1 H1A 0.8800 . ? N2 C2 1.341(11) . ? N2 C3 1.486(11) . ? N2 H2A 0.8800 . ? N3 C6 1.329(11) . ? N3 C5 1.468(11) . ? N3 H3A 0.8800 . ? N4 C6 1.343(11) . ? N4 C7 1.467(11) . ? N4 H4A 0.8800 . ? N5 C10 1.347(11) . ? N5 C9 1.469(10) . ? N5 H5A 0.8800 . ? N6 C10 1.324(11) . ? N6 C11 1.472(11) . ? N6 H6A 0.8800 . ? N7 C14 1.338(11) . ? N7 C13 1.464(11) . ? N7 H7A 0.8800 . ? N8 C14 1.322(10) . ? N8 C15 1.484(11) . ? N8 H8A 0.8800 . ? N9 C18 1.331(12) . ? N9 C17 1.482(13) . ? N9 H9A 0.8800 . ? N10 C18 1.338(13) . ? N10 C19 1.460(13) . ? N10 H10A 0.8800 . ? N11 C22 1.324(11) . ? N11 C21 1.452(12) . ? N11 H11A 0.8800 . ? N12 C22 1.351(10) . ? N12 C23 1.465(10) . ? N12 H12A 0.8800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C3 C4 1.501(14) . ? C3 H3B 0.9900 . ? C3 H3C 0.9900 . ? C4 H4B 0.9900 . ? C4 H4C 0.9900 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C5 H5D 0.9800 . ? C7 C8 1.518(12) . ? C7 H7B 0.9900 . ? C7 H7C 0.9900 . ? C8 H8B 0.9900 . ? C8 H8C 0.9900 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C9 H9D 0.9800 . ? C11 C12 1.504(13) . ? C11 H11B 0.9900 . ? C11 H11C 0.9900 . ? C12 H12B 0.9900 . ? C12 H12C 0.9900 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C13 H13D 0.9800 . ? C15 C16 1.530(13) . ? C15 H15B 0.9900 . ? C15 H15C 0.9900 . ? C16 H16B 0.9900 . ? C16 H16C 0.9900 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C17 H17D 0.9800 . ? C19 C20 1.516(13) . ? C19 H19B 0.9900 . ? C19 H19C 0.9900 . ? C20 H20B 0.9900 . ? C20 H20C 0.9900 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C21 H21D 0.9800 . ? C23 C24 1.522(11) . ? C23 H23B 0.9900 . ? C23 H23C 0.9900 . ? C24 H24B 0.9900 . ? C24 H24C 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 Au1 C2 178.9(3) . . ? C6 Au1 Au2 91.4(2) . . ? C2 Au1 Au2 89.3(2) . . ? C6 Au1 Au3 88.2(2) . 1_455 ? C2 Au1 Au3 91.3(2) . 1_455 ? Au2 Au1 Au3 170.971(15) . 1_455 ? C10 Au2 C14 177.9(3) . . ? C10 Au2 Au1 89.8(2) . . ? C14 Au2 Au1 91.2(2) . . ? C10 Au2 Au3 87.2(2) . . ? C14 Au2 Au3 91.5(2) . . ? Au1 Au2 Au3 168.497(16) . . ? C22 Au3 C18 179.1(4) . . ? C22 Au3 Au1 89.6(2) . 1_655 ? C18 Au3 Au1 89.7(2) . 1_655 ? C22 Au3 Au2 90.7(2) . . ? C18 Au3 Au2 90.1(3) . . ? Au1 Au3 Au2 168.410(15) 1_655 . ? F6 As1 F4 90.6(3) . . ? F6 As1 F2 91.8(3) . . ? F4 As1 F2 90.1(3) . . ? F6 As1 F5 91.2(3) . . ? F4 As1 F5 178.1(3) . . ? F2 As1 F5 89.2(3) . . ? F6 As1 F3 178.8(3) . . ? F4 As1 F3 90.2(3) . . ? F2 As1 F3 89.1(3) . . ? F5 As1 F3 88.0(3) . . ? F6 As1 F1 90.5(3) . . ? F4 As1 F1 90.5(3) . . ? F2 As1 F1 177.7(3) . . ? F5 As1 F1 90.2(3) . . ? F3 As1 F1 88.6(3) . . ? F9 As2 F11 178.8(5) . . ? F9 As2 F12 90.1(4) . . ? F11 As2 F12 90.7(4) . . ? F9 As2 F7 92.5(4) . . ? F11 As2 F7 88.3(4) . . ? F12 As2 F7 91.3(4) . . ? F9 As2 F8 88.5(4) . . ? F11 As2 F8 90.7(4) . . ? F12 As2 F8 88.7(3) . . ? F7 As2 F8 179.0(4) . . ? F9 As2 F10 90.0(4) . . ? F11 As2 F10 89.2(4) . . ? F12 As2 F10 179.0(4) . . ? F7 As2 F10 89.6(4) . . ? F8 As2 F10 90.3(4) . . ? C4 O1 H1 109.5 . . ? C8 O2 H2 109.5 . . ? C12 O3 H3 109.5 . . ? C16 O4 H4 109.5 . . ? C20 O5 H5 109.5 . . ? C24 O6 H6 109.5 . . ? C2 N1 C1 126.2(8) . . ? C2 N1 H1A 116.9 . . ? C1 N1 H1A 116.9 . . ? C2 N2 C3 123.6(7) . . ? C2 N2 H2A 118.2 . . ? C3 N2 H2A 118.2 . . ? C6 N3 C5 126.8(8) . . ? C6 N3 H3A 116.6 . . ? C5 N3 H3A 116.6 . . ? C6 N4 C7 123.9(7) . . ? C6 N4 H4A 118.0 . . ? C7 N4 H4A 118.0 . . ? C10 N5 C9 125.1(7) . . ? C10 N5 H5A 117.5 . . ? C9 N5 H5A 117.5 . . ? C10 N6 C11 124.2(7) . . ? C10 N6 H6A 117.9 . . ? C11 N6 H6A 117.9 . . ? C14 N7 C13 126.2(7) . . ? C14 N7 H7A 116.9 . . ? C13 N7 H7A 116.9 . . ? C14 N8 C15 124.2(7) . . ? C14 N8 H8A 117.9 . . ? C15 N8 H8A 117.9 . . ? C18 N9 C17 124.3(10) . . ? C18 N9 H9A 117.8 . . ? C17 N9 H9A 117.8 . . ? C18 N10 C19 124.7(8) . . ? C18 N10 H10A 117.6 . . ? C19 N10 H10A 117.6 . . ? C22 N11 C21 127.0(8) . . ? C22 N11 H11A 116.5 . . ? C21 N11 H11A 116.5 . . ? C22 N12 C23 123.5(7) . . ? C22 N12 H12A 118.2 . . ? C23 N12 H12A 118.2 . . ? N1 C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? N2 C2 N1 116.0(7) . . ? N2 C2 Au1 123.6(6) . . ? N1 C2 Au1 120.4(6) . . ? N2 C3 C4 112.5(8) . . ? N2 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 . . ? N2 C3 H3C 109.1 . . ? C4 C3 H3C 109.1 . . ? H3B C3 H3C 107.8 . . ? O1 C4 C3 112.2(8) . . ? O1 C4 H4B 109.2 . . ? C3 C4 H4B 109.2 . . ? O1 C4 H4C 109.2 . . ? C3 C4 H4C 109.2 . . ? H4B C4 H4C 107.9 . . ? N3 C5 H5B 109.5 . . ? N3 C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C5 H5D 109.5 . . ? H5B C5 H5D 109.5 . . ? H5C C5 H5D 109.5 . . ? N3 C6 N4 116.1(8) . . ? N3 C6 Au1 122.4(6) . . ? N4 C6 Au1 121.5(6) . . ? N4 C7 C8 112.5(7) . . ? N4 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? N4 C7 H7C 109.1 . . ? C8 C7 H7C 109.1 . . ? H7B C7 H7C 107.8 . . ? O2 C8 C7 109.8(7) . . ? O2 C8 H8B 109.7 . . ? C7 C8 H8B 109.7 . . ? O2 C8 H8C 109.7 . . ? C7 C8 H8C 109.7 . . ? H8B C8 H8C 108.2 . . ? N5 C9 H9B 109.5 . . ? N5 C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N5 C9 H9D 109.5 . . ? H9B C9 H9D 109.5 . . ? H9C C9 H9D 109.5 . . ? N6 C10 N5 117.0(8) . . ? N6 C10 Au2 123.9(6) . . ? N5 C10 Au2 119.1(6) . . ? N6 C11 C12 113.1(7) . . ? N6 C11 H11B 109.0 . . ? C12 C11 H11B 109.0 . . ? N6 C11 H11C 109.0 . . ? C12 C11 H11C 109.0 . . ? H11B C11 H11C 107.8 . . ? O3 C12 C11 110.3(8) . . ? O3 C12 H12B 109.6 . . ? C11 C12 H12B 109.6 . . ? O3 C12 H12C 109.6 . . ? C11 C12 H12C 109.6 . . ? H12B C12 H12C 108.1 . . ? N7 C13 H13B 109.5 . . ? N7 C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N7 C13 H13D 109.5 . . ? H13B C13 H13D 109.5 . . ? H13C C13 H13D 109.5 . . ? N8 C14 N7 118.0(7) . . ? N8 C14 Au2 124.8(6) . . ? N7 C14 Au2 117.2(6) . . ? N8 C15 C16 112.5(8) . . ? N8 C15 H15B 109.1 . . ? C16 C15 H15B 109.1 . . ? N8 C15 H15C 109.1 . . ? C16 C15 H15C 109.1 . . ? H15B C15 H15C 107.8 . . ? O4 C16 C15 112.5(8) . . ? O4 C16 H16B 109.1 . . ? C15 C16 H16B 109.1 . . ? O4 C16 H16C 109.1 . . ? C15 C16 H16C 109.1 . . ? H16B C16 H16C 107.8 . . ? N9 C17 H17B 109.5 . . ? N9 C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N9 C17 H17D 109.5 . . ? H17B C17 H17D 109.5 . . ? H17C C17 H17D 109.5 . . ? N9 C18 N10 118.1(9) . . ? N9 C18 Au3 119.4(7) . . ? N10 C18 Au3 122.4(7) . . ? N10 C19 C20 111.6(8) . . ? N10 C19 H19B 109.3 . . ? C20 C19 H19B 109.3 . . ? N10 C19 H19C 109.3 . . ? C20 C19 H19C 109.3 . . ? H19B C19 H19C 108.0 . . ? O5 C20 C19 111.4(7) . . ? O5 C20 H20B 109.4 . . ? C19 C20 H20B 109.4 . . ? O5 C20 H20C 109.4 . . ? C19 C20 H20C 109.4 . . ? H20B C20 H20C 108.0 . . ? N11 C21 H21B 109.5 . . ? N11 C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N11 C21 H21D 109.5 . . ? H21B C21 H21D 109.5 . . ? H21C C21 H21D 109.5 . . ? N11 C22 N12 116.1(8) . . ? N11 C22 Au3 121.1(6) . . ? N12 C22 Au3 122.8(6) . . ? N12 C23 C24 111.3(7) . . ? N12 C23 H23B 109.4 . . ? C24 C23 H23B 109.4 . . ? N12 C23 H23C 109.4 . . ? C24 C23 H23C 109.4 . . ? H23B C23 H23C 108.0 . . ? O6 C24 C23 109.2(7) . . ? O6 C24 H24B 109.8 . . ? C23 C24 H24B 109.8 . . ? O6 C24 H24C 109.8 . . ? C23 C24 H24C 109.8 . . ? H24B C24 H24C 108.3 . . ? 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 O1 H1 O7 0.84 2.39 3.029(17) 133 4_676 O2 H2 Cl1 0.84 2.24 3.082(6) 177 1_455 O3 H3 O7 0.84 2.03 2.813(17) 155 . O4 H4 O2 0.84 2.09 2.931(9) 179 1_655 O5 H5 O8 0.84 2.11 2.855(14) 148 3_776 O5 H5 O8 0.84 2.23 2.795(14) 125 1_655 O6 H6 O1 0.84 2.06 2.882(10) 164. . N1 H1A O5 0.88 2.09 2.956(10) 168 1_455 N2 H2A Cl1 0.88 2.61 3.431(8) 156. 2_656 N3 H3A O3 0.88 2.20 3.074(11) 171 . N4 H4A F1 0.88 2.29 3.060(9) 146 . N5 H5A O6 0.88 2.07 2.929(9) 165 . N7 H7A O1 0.88 2.04 2.900(10) 167 . N8 H8A Cl1 0.88 2.52 3.329(7) 153 . N9 H9A O4 0.88 1.92 2.790(12) 169 . N11 H11A O2 0.88 2.08 2.951(9) 171 1_655 N12 H12A F3 0.88 2.37 3.196(9) 157 2_656 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.533 _refine_diff_density_min -5.974 _refine_diff_density_rms 0.264 # Attachment 'dr61_1.cif' data_dr61 _database_code_depnum_ccdc_archive 'CCDC 686041' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Au{C(NHCH3)2(NHCH2CH2OH)}2]AsF6' _chemical_melting_point ? _chemical_formula_moiety 'C8 H20 Au N4 O2, As F6' _chemical_formula_sum 'C8 H20 As Au F6 N4 O2' _chemical_formula_weight 590.17 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' As As 0.0499 2.0058 '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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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' '-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 12.6805(14) _cell_length_b 21.170(2) _cell_length_c 12.8027(14) _cell_angle_alpha 90.00 _cell_angle_beta 104.325(2) _cell_angle_gamma 90.00 _cell_volume 3329.9(6) _cell_formula_units_Z 8 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 1011 _cell_measurement_theta_min 3.835 _cell_measurement_theta_max 27.46 _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224 _exptl_absorpt_coefficient_mu 10.878 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.081 _exptl_absorpt_correction_T_max 0.196 _exptl_absorpt_process_details 'SADABS 2.10 (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21152 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0219 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.53 _reflns_number_total 3841 _reflns_number_gt 3470 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.054 (Bruker, 2003)' _computing_cell_refinement SAINT _computing_data_reduction 'SAINT 6.45A (Bruker, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material 'SHELXS-97 (Sheldrick, 1990)' _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. Isotropic non-H Atoms in Main Residue(s) ....... 1, this is because C2 could not refine as anisotropic. ; _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^)+(0.0269P)^2^+30.6832P] 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 3841 _refine_ls_number_parameters 195 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0271 _refine_ls_R_factor_gt 0.0230 _refine_ls_wR_factor_ref 0.0596 _refine_ls_wR_factor_gt 0.0569 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.454320(11) 0.495434(7) 0.352863(11) 0.01521(6) Uani 1 1 d . . . As1 As 0.0000 0.61438(3) 0.2500 0.01812(12) Uani 1 2 d S . . As2 As 0.5000 0.81398(3) 0.2500 0.02413(14) Uani 1 2 d S . . F1 F 0.1225(2) 0.61309(14) 0.2154(2) 0.0350(6) Uani 1 1 d . . . F2 F -0.0480(2) 0.55556(13) 0.1563(2) 0.0292(6) Uani 1 1 d . . . F3 F -0.0488(2) 0.67071(14) 0.1539(3) 0.0387(7) Uani 1 1 d . . . F4 F 0.5985(2) 0.81287(13) 0.1776(2) 0.0325(6) Uani 1 1 d . . . F5 F 0.4284(3) 0.75682(15) 0.1661(3) 0.0534(10) Uani 1 1 d . . . F6 F 0.4299(2) 0.87132(13) 0.1665(2) 0.0310(6) Uani 1 1 d . . . O1 O 0.3578(2) 0.64785(15) 0.5469(2) 0.0226(6) Uani 1 1 d . . . H1A H 0.3170 0.6161 0.5413 0.034 Uiso 1 1 calc R . . O2 O 0.2194(2) 0.46017(14) 0.0264(2) 0.0223(6) Uani 1 1 d . . . H2A H 0.1880 0.4486 -0.0363 0.033 Uiso 1 1 calc R . . N1 N 0.6464(3) 0.57606(16) 0.4269(3) 0.0179(7) Uani 1 1 d . . . H1E H 0.6783 0.5390 0.4292 0.021 Uiso 1 1 calc R . . N2 N 0.4913(3) 0.63400(16) 0.3894(3) 0.0187(7) Uani 1 1 d . . . H2B H 0.5346 0.6671 0.4035 0.022 Uiso 1 1 calc R . . N3 N 0.4200(3) 0.35786(16) 0.3337(3) 0.0183(7) Uani 1 1 d . . . H3A H 0.4864 0.3587 0.3759 0.022 Uiso 1 1 calc R . . N4 N 0.2701(3) 0.41129(16) 0.2449(3) 0.0184(7) Uani 1 1 d . . . H4A H 0.2418 0.3739 0.2251 0.022 Uiso 1 1 calc R . . C1 C 0.7187(3) 0.6306(2) 0.4569(3) 0.0216(8) Uani 1 1 d . . . H1B H 0.7946 0.6163 0.4748 0.032 Uiso 1 1 calc R . . H1C H 0.7031 0.6516 0.5196 0.032 Uiso 1 1 calc R . . H1D H 0.7067 0.6602 0.3964 0.032 Uiso 1 1 calc R . . C2 C 0.5375(3) 0.57598(19) 0.3964(3) 0.0172(8) Uiso 1 1 d . . . C3 C 0.3736(3) 0.6450(2) 0.3598(3) 0.0208(8) Uani 1 1 d . . . H3B H 0.3354 0.6039 0.3467 0.025 Uiso 1 1 calc R . . H3C H 0.3541 0.6696 0.2919 0.025 Uiso 1 1 calc R . . C4 C 0.3356(3) 0.6806(2) 0.4467(3) 0.0208(8) Uani 1 1 d . . . H4B H 0.3719 0.7223 0.4576 0.025 Uiso 1 1 calc R . . H4C H 0.2562 0.6879 0.4218 0.025 Uiso 1 1 calc R . . C5 C 0.3724(3) 0.29576(19) 0.3014(4) 0.0223(8) Uani 1 1 d . . . H5A H 0.4240 0.2628 0.3347 0.033 Uiso 1 1 calc R . . H5B H 0.3563 0.2918 0.2228 0.033 Uiso 1 1 calc R . . H5C H 0.3050 0.2911 0.3251 0.033 Uiso 1 1 calc R . . C6 C 0.3719(3) 0.41323(19) 0.3051(3) 0.0158(7) Uani 1 1 d . . . C7 C 0.2021(3) 0.46649(19) 0.2096(3) 0.0204(8) Uani 1 1 d . . . H7A H 0.2483 0.5048 0.2203 0.024 Uiso 1 1 calc R . . H7B H 0.1489 0.4708 0.2541 0.024 Uiso 1 1 calc R . . C8 C 0.1418(3) 0.4616(2) 0.0920(3) 0.0225(8) Uani 1 1 d . . . H8A H 0.0971 0.4227 0.0801 0.027 Uiso 1 1 calc R . . H8B H 0.0926 0.4983 0.0717 0.027 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 Au1 0.01448(8) 0.01617(8) 0.01538(8) -0.00025(5) 0.00446(6) -0.00230(5) As1 0.0128(3) 0.0173(3) 0.0234(3) 0.000 0.0029(2) 0.000 As2 0.0135(3) 0.0143(3) 0.0440(4) 0.000 0.0059(3) 0.000 F1 0.0197(13) 0.0413(17) 0.0475(17) 0.0058(13) 0.0150(12) -0.0014(11) F2 0.0299(14) 0.0297(14) 0.0242(13) -0.0059(11) -0.0003(11) -0.0014(11) F3 0.0298(15) 0.0317(15) 0.0478(18) 0.0173(13) -0.0031(13) -0.0013(12) F4 0.0213(13) 0.0269(14) 0.0520(18) -0.0108(12) 0.0139(12) -0.0033(11) F5 0.0316(16) 0.0336(17) 0.098(3) -0.0349(18) 0.0223(17) -0.0159(13) F6 0.0258(14) 0.0342(15) 0.0303(14) 0.0030(11) 0.0018(11) 0.0076(11) O1 0.0187(14) 0.0267(16) 0.0224(15) 0.0034(12) 0.0052(12) -0.0025(12) O2 0.0192(14) 0.0260(16) 0.0204(14) -0.0030(12) 0.0024(11) 0.0006(12) N1 0.0163(16) 0.0188(16) 0.0187(16) -0.0009(13) 0.0048(13) -0.0013(13) N2 0.0130(16) 0.0197(17) 0.0224(17) -0.0028(13) 0.0027(13) -0.0015(13) N3 0.0151(16) 0.0199(17) 0.0193(16) 0.0000(13) 0.0032(13) -0.0006(13) N4 0.0159(16) 0.0152(16) 0.0238(17) -0.0033(13) 0.0043(13) -0.0007(12) C1 0.0175(19) 0.027(2) 0.020(2) -0.0060(16) 0.0046(15) -0.0036(16) C3 0.0154(19) 0.025(2) 0.021(2) -0.0003(16) 0.0030(16) 0.0002(15) C4 0.0167(19) 0.022(2) 0.023(2) 0.0019(16) 0.0050(16) 0.0010(15) C5 0.023(2) 0.0165(19) 0.027(2) -0.0009(16) 0.0060(17) 0.0014(16) C6 0.0139(17) 0.0199(19) 0.0157(17) -0.0021(14) 0.0078(14) -0.0036(14) C7 0.0182(19) 0.020(2) 0.024(2) -0.0009(16) 0.0057(16) 0.0019(15) C8 0.0134(18) 0.026(2) 0.027(2) -0.0003(17) 0.0030(16) 0.0018(15) _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 C2 2.010(4) . ? Au1 C6 2.044(4) . ? Au1 Au1 3.1288(4) 2_655 ? Au1 Au1 3.6625(5) 5_666 ? As1 F3 1.715(3) 2 ? As1 F3 1.715(3) . ? As1 F1 1.718(3) . ? As1 F1 1.718(3) 2 ? As1 F2 1.732(3) . ? As1 F2 1.732(3) 2 ? As2 F6 1.714(3) 2_655 ? As2 F6 1.714(3) . ? As2 F5 1.720(3) . ? As2 F5 1.720(3) 2_655 ? As2 F4 1.730(3) . ? As2 F4 1.730(3) 2_655 ? O1 C4 1.423(5) . ? O1 H1A 0.8400 . ? O2 C8 1.444(5) . ? O2 H2A 0.8400 . ? N1 C2 1.340(5) . ? N1 C1 1.464(5) . ? N1 H1E 0.8800 . ? N2 C2 1.354(5) . ? N2 C3 1.465(5) . ? N2 H2B 0.8800 . ? N3 C6 1.330(5) . ? N3 C5 1.463(5) . ? N3 H3A 0.8800 . ? N4 C6 1.331(5) . ? N4 C7 1.456(5) . ? N4 H4A 0.8800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C3 C4 1.517(6) . ? C3 H3B 0.9900 . ? C3 H3C 0.9900 . ? C4 H4B 0.9900 . ? C4 H4C 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C7 C8 1.513(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Au1 C6 178.38(14) . . ? C2 Au1 Au1 87.45(11) . 2_655 ? C6 Au1 Au1 90.95(10) . 2_655 ? C2 Au1 Au1 70.07(11) . 5_666 ? C6 Au1 Au1 111.14(11) . 5_666 ? Au1 Au1 Au1 141.004(11) 2_655 5_666 ? F3 As1 F3 91.9(2) 2 . ? F3 As1 F1 90.42(15) 2 . ? F3 As1 F1 90.84(14) . . ? F3 As1 F1 90.84(14) 2 2 ? F3 As1 F1 90.42(15) . 2 ? F1 As1 F1 178.2(2) . 2 ? F3 As1 F2 178.05(14) 2 . ? F3 As1 F2 90.03(14) . . ? F1 As1 F2 89.73(14) . . ? F1 As1 F2 88.96(13) 2 . ? F3 As1 F2 90.03(14) 2 2 ? F3 As1 F2 178.05(14) . 2 ? F1 As1 F2 88.96(13) . 2 ? F1 As1 F2 89.73(14) 2 2 ? F2 As1 F2 88.04(18) . 2 ? F6 As2 F6 89.80(19) 2_655 . ? F6 As2 F5 179.44(15) 2_655 . ? F6 As2 F5 89.80(17) . . ? F6 As2 F5 89.80(17) 2_655 2_655 ? F6 As2 F5 179.44(15) . 2_655 ? F5 As2 F5 90.6(3) . 2_655 ? F6 As2 F4 90.68(13) 2_655 . ? F6 As2 F4 90.42(14) . . ? F5 As2 F4 89.71(15) . . ? F5 As2 F4 89.20(15) 2_655 . ? F6 As2 F4 90.42(14) 2_655 2_655 ? F6 As2 F4 90.68(13) . 2_655 ? F5 As2 F4 89.20(15) . 2_655 ? F5 As2 F4 89.71(15) 2_655 2_655 ? F4 As2 F4 178.45(18) . 2_655 ? C4 O1 H1A 109.5 . . ? C8 O2 H2A 109.5 . . ? C2 N1 C1 127.6(4) . . ? C2 N1 H1E 116.2 . . ? C1 N1 H1E 116.2 . . ? C2 N2 C3 123.9(3) . . ? C2 N2 H2B 118.0 . . ? C3 N2 H2B 118.0 . . ? C6 N3 C5 125.8(3) . . ? C6 N3 H3A 117.1 . . ? C5 N3 H3A 117.1 . . ? C6 N4 C7 124.8(3) . . ? C6 N4 H4A 117.6 . . ? C7 N4 H4A 117.6 . . ? N1 C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? N1 C2 N2 114.6(4) . . ? N1 C2 Au1 121.0(3) . . ? N2 C2 Au1 124.3(3) . . ? N2 C3 C4 112.2(3) . . ? N2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? N2 C3 H3C 109.2 . . ? C4 C3 H3C 109.2 . . ? H3B C3 H3C 107.9 . . ? O1 C4 C3 113.1(3) . . ? O1 C4 H4B 109.0 . . ? C3 C4 H4B 109.0 . . ? O1 C4 H4C 109.0 . . ? C3 C4 H4C 109.0 . . ? H4B C4 H4C 107.8 . . ? N3 C5 H5A 109.5 . . ? N3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 N4 116.4(4) . . ? N3 C6 Au1 120.2(3) . . ? N4 C6 Au1 123.4(3) . . ? N4 C7 C8 111.7(3) . . ? N4 C7 H7A 109.3 . . ? C8 C7 H7A 109.3 . . ? N4 C7 H7B 109.3 . . ? C8 C7 H7B 109.3 . . ? H7A C7 H7B 107.9 . . ? O2 C8 C7 109.3(3) . . ? O2 C8 H8A 109.8 . . ? C7 C8 H8A 109.8 . . ? O2 C8 H8B 109.8 . . ? C7 C8 H8B 109.8 . . ? H8A C8 H8B 108.3 . . ? 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 O1 H1A O2 0.84 2.01 2.855(4) 179 6_566 O2 H2A F2 0.84 2.04 2.791(4) 148 5_565 N1 H1E O2 0.88 2.10 2.961(5) 165 2_655 N2 H2B F5 0.88 2.20 2.943(5) 142 2_655 N3 H3A O1 0.88 1.98 2.856(5) 171 5_666 N4 H4A F4 0.88 2.19 2.982(4) 150 3_445 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 4.196 _refine_diff_density_min -0.892 _refine_diff_density_rms 0.141 # Attachment 'dr71_1.cif' data_dr71 _database_code_depnum_ccdc_archive 'CCDC 686042' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Au{C(NHCH3)(NHCH2CH2OH)}2]PF6' _chemical_melting_point ? _chemical_formula_moiety 'C8 H20 Au N4 O2, F6 P' _chemical_formula_sum 'C8 H20 Au F6 N4 O2 P' _chemical_formula_weight 546.22 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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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' '-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 12.5320(17) _cell_length_b 21.058(3) _cell_length_c 12.794(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.630(2) _cell_angle_gamma 90.00 _cell_volume 3266.9(10) _cell_formula_units_Z 8 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 8918 _cell_measurement_theta_min 2.804 _cell_measurement_theta_max 30.488 _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.221 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 9.175 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.249 _exptl_absorpt_correction_T_max 0.438 _exptl_absorpt_process_details 'SADABS 2.10 (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23025 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 30.49 _reflns_number_total 4900 _reflns_number_gt 4575 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2007)' _computing_cell_refinement SAINT _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXS-97 _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. Isotropic non-H Atoms in Main Residue(s) ....... 1 because C6 could not be refined as anisotropic. There is a large difference map peak near Au1 that may be an artifact of absorption. ; _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^)+(0.0385P)^2^+12.4604P] 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 4900 _refine_ls_number_parameters 195 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0284 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0765 _refine_ls_wR_factor_gt 0.0753 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.545723(9) 0.506982(6) 0.147553(9) 0.01556(5) Uani 1 1 d . . . P1 P 0.0000 0.38863(6) 0.2500 0.0197(2) Uani 1 2 d S . . P2 P 0.5000 0.19049(7) 0.2500 0.0254(3) Uani 1 2 d S . . F1 F 0.11541(18) 0.38982(13) 0.2188(2) 0.0357(6) Uani 1 1 d . . . F2 F -0.04491(19) 0.44375(12) 0.16187(17) 0.0291(5) Uani 1 1 d . . . F3 F -0.0453(2) 0.33599(14) 0.1607(2) 0.0419(7) Uani 1 1 d . . . F4 F 0.40818(18) 0.19121(12) 0.3186(2) 0.0334(5) Uani 1 1 d . . . F5 F 0.43317(19) 0.13699(13) 0.17270(19) 0.0328(5) Uani 1 1 d . . . F6 F 0.4319(2) 0.24395(16) 0.1721(3) 0.0608(10) Uani 1 1 d . . . O1 O 0.7847(2) 0.54262(14) 0.4735(2) 0.0236(5) Uani 1 1 d . . . H1B H 0.8177 0.5466 0.5373 0.035 Uiso 1 1 calc R . . O2 O 0.64505(19) 0.34960(13) -0.04616(19) 0.0221(5) Uani 1 1 d . . . H2A H 0.6848 0.3809 -0.0419 0.033 Uiso 1 1 calc R . . N1 N 0.5796(2) 0.64523(14) 0.1654(2) 0.0176(5) Uani 1 1 d . . . H1A H 0.5137 0.6444 0.1243 0.021 Uiso 1 1 calc R . . N2 N 0.7327(2) 0.59201(14) 0.2549(2) 0.0180(5) Uani 1 1 d . . . H2B H 0.7607 0.6288 0.2741 0.022 Uiso 1 1 calc R . . N3 N 0.3512(2) 0.42536(14) 0.0729(2) 0.0180(5) Uani 1 1 d . . . H3C H 0.3198 0.4618 0.0710 0.022 Uiso 1 1 calc R . . N4 N 0.5092(2) 0.36774(15) 0.1103(2) 0.0187(5) Uani 1 1 d . . . H4A H 0.4668 0.3351 0.0960 0.022 Uiso 1 1 calc R . . C1 C 0.6284(3) 0.70755(17) 0.1974(3) 0.0228(7) Uani 1 1 d . . . H1C H 0.5756 0.7401 0.1682 0.034 Uiso 1 1 calc R . . H1D H 0.6925 0.7129 0.1701 0.034 Uiso 1 1 calc R . . H1E H 0.6492 0.7106 0.2747 0.034 Uiso 1 1 calc R . . C2 C 0.6285(3) 0.58981(17) 0.1946(2) 0.0174(6) Uani 1 1 d . . . C3 C 0.8017(3) 0.53670(17) 0.2902(3) 0.0200(6) Uani 1 1 d . . . H3A H 0.8544 0.5326 0.2465 0.024 Uiso 1 1 calc R . . H3B H 0.7561 0.4989 0.2794 0.024 Uiso 1 1 calc R . . C4 C 0.8631(3) 0.54156(19) 0.4079(3) 0.0222(6) Uani 1 1 d . . . H4B H 0.9123 0.5055 0.4279 0.027 Uiso 1 1 calc R . . H4C H 0.9071 0.5800 0.4198 0.027 Uiso 1 1 calc R . . C5 C 0.2783(3) 0.37083(19) 0.0424(3) 0.0225(7) Uani 1 1 d . . . H5A H 0.2030 0.3850 0.0233 0.034 Uiso 1 1 calc R . . H5B H 0.2892 0.3419 0.1021 0.034 Uiso 1 1 calc R . . H5C H 0.2945 0.3498 -0.0183 0.034 Uiso 1 1 calc R . . C6 C 0.4620(3) 0.42507(15) 0.1035(2) 0.0167(6) Uiso 1 1 d . . . C7 C 0.6286(3) 0.35703(18) 0.1407(3) 0.0212(6) Uani 1 1 d . . . H7A H 0.6487 0.3347 0.2092 0.025 Uiso 1 1 calc R . . H7B H 0.6662 0.3977 0.1503 0.025 Uiso 1 1 calc R . . C8 C 0.6669(3) 0.31872(18) 0.0564(3) 0.0216(6) Uani 1 1 d . . . H8A H 0.7456 0.3112 0.0818 0.026 Uiso 1 1 calc R . . H8B H 0.6302 0.2778 0.0479 0.026 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 Au1 0.01332(8) 0.02038(8) 0.01326(7) -0.00011(4) 0.00387(5) -0.00257(4) P1 0.0117(5) 0.0220(6) 0.0238(6) 0.000 0.0016(4) 0.000 P2 0.0136(5) 0.0198(6) 0.0431(8) 0.000 0.0076(5) 0.000 F1 0.0182(10) 0.0448(15) 0.0471(14) -0.0056(12) 0.0141(10) 0.0008(10) F2 0.0282(11) 0.0356(13) 0.0202(10) 0.0047(9) 0.0002(8) 0.0027(9) F3 0.0290(13) 0.0368(15) 0.0539(16) -0.0209(13) -0.0008(11) -0.0006(10) F4 0.0195(10) 0.0327(13) 0.0510(14) -0.0122(11) 0.0147(10) -0.0041(9) F5 0.0239(11) 0.0444(15) 0.0291(11) -0.0044(10) 0.0045(9) -0.0102(10) F6 0.0335(14) 0.0478(18) 0.109(3) 0.0441(19) 0.0324(16) 0.0219(13) O1 0.0184(11) 0.0326(14) 0.0186(11) -0.0022(10) 0.0025(9) 0.0012(10) O2 0.0176(11) 0.0277(13) 0.0208(11) 0.0024(10) 0.0043(9) -0.0048(9) N1 0.0128(12) 0.0202(13) 0.0195(12) -0.0002(10) 0.0031(10) -0.0013(10) N2 0.0142(12) 0.0183(13) 0.0203(12) -0.0023(10) 0.0025(10) -0.0014(9) N3 0.0140(12) 0.0225(14) 0.0185(12) -0.0023(10) 0.0058(10) -0.0019(10) N4 0.0120(12) 0.0230(14) 0.0209(13) -0.0027(11) 0.0037(10) -0.0027(10) C1 0.0216(15) 0.0187(16) 0.0277(17) -0.0023(13) 0.0056(13) 0.0024(12) C2 0.0155(13) 0.0229(16) 0.0149(13) 0.0008(11) 0.0061(11) -0.0001(11) C3 0.0175(14) 0.0205(16) 0.0212(14) -0.0010(12) 0.0034(12) 0.0029(11) C4 0.0130(13) 0.0284(17) 0.0242(15) -0.0008(13) 0.0029(11) 0.0010(12) C5 0.0150(14) 0.0322(19) 0.0209(15) -0.0042(13) 0.0056(12) -0.0071(13) C7 0.0147(14) 0.0274(17) 0.0210(15) 0.0000(13) 0.0034(12) 0.0008(12) C8 0.0165(14) 0.0252(17) 0.0230(15) 0.0027(13) 0.0050(12) 0.0022(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 C6 2.024(3) . ? Au1 C2 2.041(3) . ? Au1 Au1 3.1149(6) 2_655 ? Au1 Au1 3.6701(8) 5_665 ? P1 F3 1.590(3) . ? P1 F3 1.590(3) 2 ? P1 F1 1.595(2) . ? P1 F1 1.595(2) 2 ? P1 F2 1.617(2) 2 ? P1 F2 1.617(2) . ? P2 F5 1.591(3) . ? P2 F5 1.591(3) 2_655 ? P2 F6 1.600(3) 2_655 ? P2 F6 1.600(3) . ? P2 F4 1.614(2) 2_655 ? P2 F4 1.614(2) . ? O1 C4 1.445(4) . ? O1 H1B 0.8200 . ? O2 C8 1.428(4) . ? O2 H2A 0.8200 . ? N1 C2 1.327(4) . ? N1 C1 1.462(4) . ? N1 H1A 0.8600 . ? N2 C2 1.339(4) . ? N2 C3 1.453(4) . ? N2 H2B 0.8600 . ? N3 C6 1.344(4) . ? N3 C5 1.458(4) . ? N3 H3C 0.8600 . ? N4 C6 1.338(4) . ? N4 C7 1.465(4) . ? N4 H4A 0.8600 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C1 H1E 0.9600 . ? C3 C4 1.512(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C7 C8 1.519(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 Au1 C2 178.78(11) . . ? C6 Au1 Au1 87.68(8) . 2_655 ? C2 Au1 Au1 91.11(8) . 2_655 ? C6 Au1 Au1 68.89(8) . 5_665 ? C2 Au1 Au1 112.05(9) . 5_665 ? Au1 Au1 Au1 141.272(11) 2_655 5_665 ? F3 P1 F3 91.6(2) . 2 ? F3 P1 F1 90.72(14) . . ? F3 P1 F1 90.54(15) 2 . ? F3 P1 F1 90.54(15) . 2 ? F3 P1 F1 90.72(14) 2 2 ? F1 P1 F1 178.2(2) . 2 ? F3 P1 F2 178.33(16) . 2 ? F3 P1 F2 90.08(14) 2 2 ? F1 P1 F2 89.16(13) . 2 ? F1 P1 F2 89.54(13) 2 2 ? F3 P1 F2 90.08(14) . . ? F3 P1 F2 178.33(16) 2 . ? F1 P1 F2 89.54(13) . . ? F1 P1 F2 89.16(13) 2 . ? F2 P1 F2 88.26(18) 2 . ? F5 P2 F5 89.8(2) . 2_655 ? F5 P2 F6 179.55(16) . 2_655 ? F5 P2 F6 89.82(18) 2_655 2_655 ? F5 P2 F6 89.82(18) . . ? F5 P2 F6 179.55(16) 2_655 . ? F6 P2 F6 90.5(3) 2_655 . ? F5 P2 F4 90.25(13) . 2_655 ? F5 P2 F4 90.52(13) 2_655 2_655 ? F6 P2 F4 89.49(15) 2_655 2_655 ? F6 P2 F4 89.75(14) . 2_655 ? F5 P2 F4 90.52(13) . . ? F5 P2 F4 90.25(13) 2_655 . ? F6 P2 F4 89.75(14) 2_655 . ? F6 P2 F4 89.49(15) . . ? F4 P2 F4 178.9(2) 2_655 . ? C4 O1 H1B 109.5 . . ? C8 O2 H2A 109.5 . . ? C2 N1 C1 125.4(3) . . ? C2 N1 H1A 117.3 . . ? C1 N1 H1A 117.3 . . ? C2 N2 C3 124.6(3) . . ? C2 N2 H2B 117.7 . . ? C3 N2 H2B 117.7 . . ? C6 N3 C5 127.3(3) . . ? C6 N3 H3C 116.3 . . ? C5 N3 H3C 116.3 . . ? C6 N4 C7 124.2(3) . . ? C6 N4 H4A 117.9 . . ? C7 N4 H4A 117.9 . . ? N1 C1 H1C 109.5 . . ? N1 C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? N1 C1 H1E 109.5 . . ? H1C C1 H1E 109.5 . . ? H1D C1 H1E 109.5 . . ? N1 C2 N2 116.5(3) . . ? N1 C2 Au1 120.3(2) . . ? N2 C2 Au1 123.3(3) . . ? N2 C3 C4 111.6(3) . . ? N2 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 . . ? N2 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? O1 C4 C3 109.3(3) . . ? O1 C4 H4B 109.8 . . ? C3 C4 H4B 109.8 . . ? O1 C4 H4C 109.8 . . ? C3 C4 H4C 109.8 . . ? H4B C4 H4C 108.3 . . ? N3 C5 H5A 109.5 . . ? N3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N4 C6 N3 115.5(3) . . ? N4 C6 Au1 124.2(2) . . ? N3 C6 Au1 120.1(2) . . ? N4 C7 C8 112.2(3) . . ? N4 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? N4 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? O2 C8 C7 112.9(3) . . ? O2 C8 H8A 109.0 . . ? C7 C8 H8A 109.0 . . ? O2 C8 H8B 109.0 . . ? C7 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? 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 O2 H2A O1 0.82 2.02 2.838(4) 178 6_565 N2 H2B F4 0.86 2.22 2.993(4) 149 3 N1 H1A O2 0.86 1.99 2.845(4) 171 5_665 N4 H4A F6 0.86 2.24 2.957(4) 140 . O1 H1B F2 0.82 2.04 2.801(3) 154 6_666 N3 H3C O1 0.86 2.14 2.973(4) 165 2_655 _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 30.49 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 3.335 _refine_diff_density_min -1.792 _refine_diff_density_rms 0.204 # Attachment 'dr85_1.cif' data_dr85 _database_code_depnum_ccdc_archive 'CCDC 686043' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Au{C(NHCH3)(NHCH2CH2OH)}2]3(PF6)2Cl.(H2O)2' _chemical_melting_point ? _chemical_formula_moiety '3(C8 H20 Au N4 O2), 2(F6 P), Cl, (H2O)2' _chemical_formula_sum 'C24 H64 Au3 Cl F12 N12 O8 P2' _chemical_formula_weight 1565.15 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 9.3313(15) _cell_length_b 20.479(3) _cell_length_c 24.237(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.087(2) _cell_angle_gamma 90.00 _cell_volume 4630.7(13) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 1025 _cell_measurement_theta_min 2.525 _cell_measurement_theta_max 30.438 _exptl_crystal_description needle _exptl_crystal_colour yellow/green _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.216 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2944 _exptl_absorpt_coefficient_mu 9.708 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.446 _exptl_absorpt_correction_T_max 0.679 _exptl_absorpt_process_details 'TWINABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14052 _diffrn_reflns_av_R_equivalents 0.0655 _diffrn_reflns_av_sigmaI/netI 0.0837 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 27.50 _reflns_number_total 14210 _reflns_number_gt 9832 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2007)' _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _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. This structure is a rotational twin. Several large difference maps are likely to result from this defect. 201_ALERT_2_A Isotropic non-H Atoms in Main Residue(s) ....... 24 306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O7 306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O8 430_ALERT_2_A Short Inter D...A Contact O7 .. O7 .. 2.50 Ang. These alerts are because the water hydrogens could not be found. ; _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^)+(0.0418P)^2^+80.1147P] 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 14054 _refine_ls_number_parameters 436 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1045 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.1463 _refine_ls_wR_factor_gt 0.1298 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.07489(5) 0.74402(2) 0.130843(17) 0.01834(11) Uani 1 1 d . . . Au2 Au 0.40809(4) 0.75872(2) 0.136935(18) 0.01881(11) Uani 1 1 d . . . Au3 Au 0.74049(4) 0.76130(2) 0.123909(18) 0.01778(11) Uani 1 1 d . . . P1 P 0.1913(4) 0.61725(17) 0.39425(13) 0.0229(7) Uani 1 1 d . . . P2 P 0.0825(4) 0.41272(17) 0.12011(13) 0.0236(7) Uani 1 1 d . . . Cl1 Cl 0.5963(3) 0.54374(15) 0.30889(13) 0.0234(6) Uani 1 1 d . . . F1 F 0.2785(8) 0.6844(4) 0.3935(3) 0.0331(18) Uani 1 1 d . . . F2 F 0.2303(8) 0.6061(4) 0.3311(3) 0.0285(17) Uani 1 1 d . . . F3 F 0.3315(9) 0.5790(4) 0.4135(3) 0.039(2) Uani 1 1 d . . . F4 F 0.0987(9) 0.5506(4) 0.3932(3) 0.0358(19) Uani 1 1 d . . . F5 F 0.1498(8) 0.6300(4) 0.4567(3) 0.0327(18) Uani 1 1 d . . . F6 F 0.0493(8) 0.6561(4) 0.3732(3) 0.0358(19) Uani 1 1 d . . . F7 F 0.0793(10) 0.4364(6) 0.0582(4) 0.071(4) Uani 1 1 d . . . F8 F 0.0820(13) 0.4863(5) 0.1379(6) 0.086(4) Uani 1 1 d . . . F9 F -0.0912(9) 0.4100(6) 0.1211(4) 0.063(3) Uani 1 1 d . . . F10 F 0.0854(10) 0.3883(5) 0.1818(3) 0.056(3) Uani 1 1 d . . . F11 F 0.0838(11) 0.3398(5) 0.1015(4) 0.064(3) Uani 1 1 d . . . F12 F 0.2536(9) 0.4158(5) 0.1201(4) 0.058(3) Uani 1 1 d . . . O1 O -0.1951(9) 0.6096(5) 0.2345(4) 0.027(2) Uani 1 1 d . . . H1B H -0.2055 0.6449 0.2516 0.040 Uiso 1 1 calc R . . O2 O 0.3626(9) 0.6011(4) 0.0310(3) 0.0229(19) Uani 1 1 d . . . H2A H 0.4159 0.5684 0.0355 0.034 Uiso 1 1 calc R . . O3 O 0.7141(11) 0.7298(5) 0.2841(5) 0.048(3) Uani 1 1 d . . . H3C H 0.7680 0.7527 0.3044 0.071 Uiso 1 1 calc R . . O4 O 0.1100(8) 0.9278(4) 0.1899(3) 0.0202(18) Uani 1 1 d . . . H4A H 0.0514 0.9589 0.1899 0.030 Uiso 1 1 calc R . . O5 O 0.4371(11) 0.7201(6) -0.0141(4) 0.054(3) Uani 1 1 d . . . H5E H 0.3657 0.7153 -0.0354 0.081 Uiso 1 1 calc R . . O6 O 1.0343(9) 0.9166(5) 0.0727(4) 0.035(2) Uani 1 1 d . . . H6B H 1.0573 0.9197 0.1062 0.053 Uiso 1 1 calc R . . O7 O 0.434(2) 0.4650(9) 0.0334(8) 0.115(6) Uiso 1 1 d . . . O8 O -0.271(3) 0.3031(12) 0.1110(9) 0.149(8) Uiso 1 1 d . . . N1 N 0.0766(10) 0.7996(5) 0.2429(4) 0.022(2) Uani 1 1 d . . . H1A H 0.0851 0.8358 0.2236 0.027 Uiso 1 1 calc R . . N2 N 0.0608(10) 0.6891(5) 0.2457(4) 0.020(2) Uani 1 1 d . . . H2B H 0.0563 0.6930 0.2818 0.024 Uiso 1 1 calc R . . N3 N 0.0693(11) 0.7983(6) 0.0182(4) 0.029(3) Uani 1 1 d . . . H3D H 0.0481 0.8341 0.0364 0.034 Uiso 1 1 calc R . . N4 N 0.1037(11) 0.6882(7) 0.0180(5) 0.036(3) Uani 1 1 d . . . H4B H 0.1128 0.6920 -0.0179 0.043 Uiso 1 1 calc R . . N5 N 0.4146(10) 0.6153(5) 0.1501(4) 0.023(2) Uani 1 1 d . . . H5A H 0.3961 0.6176 0.1144 0.027 Uiso 1 1 calc R . . N6 N 0.4540(10) 0.6677(5) 0.2316(4) 0.022(2) Uani 1 1 d . . . H6A H 0.4710 0.6288 0.2457 0.026 Uiso 1 1 calc R . . N7 N 0.3928(11) 0.8518(5) 0.0434(4) 0.023(2) Uani 1 1 d . . . H7A H 0.4124 0.8159 0.0250 0.027 Uiso 1 1 calc R . . N8 N 0.3676(10) 0.9020(5) 0.1258(4) 0.021(2) Uani 1 1 d . . . H8A H 0.3573 0.9387 0.1072 0.025 Uiso 1 1 calc R . . N9 N 0.7521(10) 0.6189(5) 0.1161(4) 0.020(2) Uani 1 1 d . . . H9D H 0.7700 0.6244 0.1516 0.024 Uiso 1 1 calc R . . N10 N 0.7100(11) 0.6630(5) 0.0326(4) 0.024(2) Uani 1 1 d . . . H10A H 0.7054 0.6225 0.0204 0.028 Uiso 1 1 calc R . . N11 N 0.7454(11) 0.8481(5) 0.2194(5) 0.024(2) Uani 1 1 d . . . H11C H 0.7310 0.8097 0.2347 0.029 Uiso 1 1 calc R . . N12 N 0.7706(11) 0.9053(5) 0.1405(4) 0.020(2) Uani 1 1 d . . . H12C H 0.7827 0.9397 0.1619 0.024 Uiso 1 1 calc R . . C1 C 0.0720(14) 0.8066(7) 0.3030(5) 0.028(3) Uiso 1 1 d . . . H1C H 0.0922 0.8521 0.3132 0.042 Uiso 1 1 calc R . . H1D H 0.1442 0.7781 0.3203 0.042 Uiso 1 1 calc R . . H1E H -0.0233 0.7945 0.3158 0.042 Uiso 1 1 calc R . . C2 C 0.0692(12) 0.7442(6) 0.2145(4) 0.016(2) Uiso 1 1 d . . . C3 C 0.0591(13) 0.6242(6) 0.2215(5) 0.019(2) Uiso 1 1 d . . . H3A H 0.1536 0.6031 0.2277 0.023 Uiso 1 1 calc R . . H3B H 0.0414 0.6275 0.1812 0.023 Uiso 1 1 calc R . . C4 C -0.0561(13) 0.5831(6) 0.2469(5) 0.022(3) Uiso 1 1 d . . . H4C H -0.0503 0.5379 0.2326 0.027 Uiso 1 1 calc R . . H4D H -0.0408 0.5815 0.2875 0.027 Uiso 1 1 calc R . . C5 C 0.0828(16) 0.8036(7) -0.0414(6) 0.038(4) Uiso 1 1 d . . . H5B H 0.0713 0.8493 -0.0525 0.057 Uiso 1 1 calc R . . H5C H 0.0085 0.7770 -0.0596 0.057 Uiso 1 1 calc R . . H5D H 0.1776 0.7880 -0.0521 0.057 Uiso 1 1 calc R . . C6 C 0.0865(12) 0.7437(6) 0.0475(4) 0.020(2) Uiso 1 1 d . . . C7 C 0.1083(14) 0.6226(6) 0.0415(6) 0.028(3) Uiso 1 1 d . . . H7B H 0.0133 0.6017 0.0362 0.034 Uiso 1 1 calc R . . H7C H 0.1283 0.6257 0.0817 0.034 Uiso 1 1 calc R . . C8 C 0.2218(14) 0.5801(7) 0.0154(6) 0.030(3) Uiso 1 1 d . . . H8B H 0.2083 0.5342 0.0270 0.036 Uiso 1 1 calc R . . H8C H 0.2105 0.5819 -0.0253 0.036 Uiso 1 1 calc R . . C9 C 0.4288(13) 0.5499(6) 0.1735(5) 0.022(3) Uiso 1 1 d . . . H9A H 0.4112 0.5173 0.1446 0.033 Uiso 1 1 calc R . . H9B H 0.3589 0.5442 0.2028 0.033 Uiso 1 1 calc R . . H9C H 0.5259 0.5442 0.1889 0.033 Uiso 1 1 calc R . . C10 C 0.4264(13) 0.6709(6) 0.1765(5) 0.020(2) Uiso 1 1 d . . . C11 C 0.4581(14) 0.7232(6) 0.2696(5) 0.027(3) Uiso 1 1 d . . . H11A H 0.3673 0.7245 0.2901 0.033 Uiso 1 1 calc R . . H11B H 0.4645 0.7641 0.2479 0.033 Uiso 1 1 calc R . . C12 C 0.5806(15) 0.7207(8) 0.3101(6) 0.037(3) Uiso 1 1 d . . . H12A H 0.5681 0.7552 0.3382 0.045 Uiso 1 1 calc R . . H12B H 0.5806 0.6780 0.3291 0.045 Uiso 1 1 calc R . . C13 C 0.3704(14) 0.9117(6) 0.0118(5) 0.029(3) Uiso 1 1 d . . . H13A H 0.3793 0.9023 -0.0277 0.043 Uiso 1 1 calc R . . H13B H 0.4424 0.9441 0.0230 0.043 Uiso 1 1 calc R . . H13C H 0.2744 0.9288 0.0188 0.043 Uiso 1 1 calc R . . C14 C 0.3856(13) 0.8480(6) 0.0979(5) 0.020(2) Uiso 1 1 d . . . C15 C 0.3636(14) 0.9048(6) 0.1863(5) 0.026(3) Uiso 1 1 d . . . H15A H 0.4585 0.9187 0.2010 0.031 Uiso 1 1 calc R . . H15B H 0.3436 0.8606 0.2010 0.031 Uiso 1 1 calc R . . C16 C 0.2508(13) 0.9515(6) 0.2057(5) 0.024(3) Uiso 1 1 d . . . H16A H 0.2578 0.9560 0.2463 0.029 Uiso 1 1 calc R . . H16B H 0.2665 0.9950 0.1891 0.029 Uiso 1 1 calc R . . C17 C 0.7477(14) 0.5515(6) 0.0954(5) 0.025(3) Uiso 1 1 d . . . H17A H 0.7735 0.5213 0.1254 0.037 Uiso 1 1 calc R . . H17B H 0.8158 0.5467 0.0654 0.037 Uiso 1 1 calc R . . H17C H 0.6508 0.5414 0.0816 0.037 Uiso 1 1 calc R . . C18 C 0.7313(12) 0.6724(5) 0.0859(5) 0.016(2) Uiso 1 1 d . . . C19 C 0.6936(13) 0.7165(6) -0.0076(5) 0.021(3) Uiso 1 1 d . . . H19A H 0.7801 0.7183 -0.0306 0.025 Uiso 1 1 calc R . . H19B H 0.6871 0.7584 0.0126 0.025 Uiso 1 1 calc R . . C20 C 0.5656(16) 0.7095(8) -0.0442(6) 0.041(4) Uiso 1 1 d . . . H20A H 0.5707 0.7415 -0.0747 0.049 Uiso 1 1 calc R . . H20B H 0.5638 0.6652 -0.0604 0.049 Uiso 1 1 calc R . . C22 C 0.7590(14) 0.9035(6) 0.2568(5) 0.024(3) Uiso 1 1 d . . . H22A H 0.7540 0.8881 0.2950 0.036 Uiso 1 1 calc R . . H22B H 0.6810 0.9344 0.2493 0.036 Uiso 1 1 calc R . . H22C H 0.8513 0.9251 0.2512 0.036 Uiso 1 1 calc R . . C23 C 0.7524(12) 0.8494(6) 0.1645(5) 0.017(2) Uiso 1 1 d . . . C24 C 0.7728(14) 0.9163(6) 0.0802(5) 0.025(3) Uiso 1 1 d . . . H24A H 0.6867 0.9416 0.0690 0.030 Uiso 1 1 calc R . . H24B H 0.7681 0.8736 0.0612 0.030 Uiso 1 1 calc R . . C26 C 0.9041(14) 0.9522(7) 0.0622(6) 0.030(3) Uiso 1 1 d . . . H26A H 0.8952 0.9614 0.0221 0.036 Uiso 1 1 calc R . . H26B H 0.9095 0.9946 0.0817 0.036 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 Au1 0.0110(2) 0.0254(2) 0.01852(19) 0.0031(2) 0.00011(13) -0.00186(19) Au2 0.0109(2) 0.0226(2) 0.0230(2) 0.0037(2) 0.00168(15) 0.00055(17) Au3 0.0105(2) 0.0197(2) 0.0232(2) -0.0048(2) 0.00206(15) -0.00192(17) P1 0.0234(17) 0.0254(18) 0.0201(15) 0.0006(14) 0.0000(13) -0.0004(13) P2 0.0212(17) 0.0256(17) 0.0239(17) -0.0016(13) -0.0039(14) -0.0002(13) Cl1 0.0176(14) 0.0181(15) 0.0344(16) 0.0059(12) 0.0021(12) -0.0006(11) F1 0.030(4) 0.030(4) 0.040(4) -0.006(4) 0.003(3) -0.009(3) F2 0.031(4) 0.029(4) 0.025(4) 0.002(3) 0.000(3) 0.002(3) F3 0.033(5) 0.047(5) 0.038(5) 0.010(4) 0.002(4) 0.014(4) F4 0.042(5) 0.026(4) 0.040(5) -0.004(4) 0.013(4) -0.010(4) F5 0.032(4) 0.042(5) 0.024(4) 0.001(3) 0.011(3) 0.003(4) F6 0.025(4) 0.037(5) 0.045(5) -0.008(4) -0.009(4) 0.006(4) F7 0.049(6) 0.125(10) 0.038(5) 0.027(6) -0.019(5) -0.053(6) F8 0.090(9) 0.032(6) 0.138(12) -0.020(7) 0.032(8) 0.012(6) F9 0.015(5) 0.102(9) 0.073(7) 0.043(6) -0.005(4) 0.004(5) F10 0.049(6) 0.098(8) 0.021(4) 0.009(5) -0.010(4) -0.016(5) F11 0.069(7) 0.038(5) 0.089(8) -0.028(5) 0.051(6) -0.024(5) F12 0.018(5) 0.062(6) 0.092(8) 0.027(6) -0.014(5) -0.012(4) O1 0.012(4) 0.037(5) 0.031(5) 0.005(4) -0.004(4) -0.002(4) O2 0.016(4) 0.019(4) 0.033(5) -0.003(4) -0.003(4) 0.004(3) O3 0.047(7) 0.020(5) 0.074(8) -0.003(5) -0.030(6) -0.005(5) O4 0.014(4) 0.015(4) 0.031(5) -0.003(4) 0.001(3) 0.008(3) O5 0.029(6) 0.084(9) 0.048(6) 0.028(6) -0.012(5) -0.024(6) O6 0.016(5) 0.070(8) 0.021(5) -0.002(5) 0.001(4) 0.000(5) N1 0.018(5) 0.015(5) 0.034(6) 0.002(5) 0.002(5) 0.003(4) N2 0.014(5) 0.025(6) 0.021(5) 0.005(4) 0.005(4) 0.000(4) N3 0.013(5) 0.049(8) 0.025(6) 0.011(5) -0.011(4) -0.006(5) N4 0.012(6) 0.078(10) 0.017(5) -0.005(6) 0.003(4) -0.002(6) N5 0.017(5) 0.031(6) 0.020(5) -0.002(5) -0.001(4) -0.002(4) N6 0.019(5) 0.016(5) 0.030(6) 0.004(4) 0.008(4) 0.003(4) N7 0.022(6) 0.027(6) 0.019(5) -0.001(5) 0.001(4) 0.002(4) N8 0.012(5) 0.026(6) 0.026(6) 0.006(5) 0.002(4) -0.003(4) N9 0.009(5) 0.024(5) 0.026(5) -0.006(4) -0.003(4) 0.000(4) N10 0.024(6) 0.024(6) 0.024(5) -0.002(5) 0.005(4) -0.007(4) N11 0.019(5) 0.015(5) 0.039(6) 0.002(5) 0.005(5) -0.003(4) N12 0.017(5) 0.017(5) 0.025(5) -0.004(5) 0.001(4) 0.000(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 C6 2.024(11) . ? Au1 C2 2.030(10) . ? Au1 Au2 3.1244(9) . ? Au1 Au3 3.1417(8) 1_455 ? Au2 C10 2.043(12) . ? Au2 C14 2.067(12) . ? Au2 Au3 3.1242(7) . ? Au3 C18 2.041(11) . ? Au3 C23 2.057(11) . ? Au3 Au1 3.1417(8) 1_655 ? P1 F3 1.588(8) . ? P1 F5 1.592(8) . ? P1 F2 1.597(8) . ? P1 F1 1.598(8) . ? P1 F4 1.616(8) . ? P1 F6 1.620(8) . ? P2 F11 1.561(9) . ? P2 F8 1.567(10) . ? P2 F7 1.575(9) . ? P2 F10 1.577(9) . ? P2 F12 1.598(9) . ? P2 F9 1.622(9) . ? O1 C4 1.433(14) . ? O1 H1B 0.8400 . ? O2 C8 1.427(15) . ? O2 H2A 0.8400 . ? O3 C12 1.419(18) . ? O3 H3C 0.8400 . ? O4 C16 1.445(14) . ? O4 H4A 0.8400 . ? O5 C20 1.431(18) . ? O5 H5E 0.8400 . ? O6 C26 1.436(16) . ? O6 H6B 0.8400 . ? N1 C2 1.329(14) . ? N1 C1 1.466(16) . ? N1 H1A 0.8800 . ? N2 C2 1.360(14) . ? N2 C3 1.453(15) . ? N2 H2B 0.8800 . ? N3 C6 1.333(15) . ? N3 C5 1.456(17) . ? N3 H3D 0.8800 . ? N4 C6 1.354(17) . ? N4 C7 1.461(18) . ? N4 H4B 0.8800 . ? N5 C10 1.310(15) . ? N5 C9 1.459(16) . ? N5 H5A 0.8800 . ? N6 C10 1.356(15) . ? N6 C11 1.464(16) . ? N6 H6A 0.8800 . ? N7 C14 1.326(15) . ? N7 C13 1.458(16) . ? N7 H7A 0.8800 . ? N8 C14 1.309(16) . ? N8 C15 1.470(15) . ? N8 H8A 0.8800 . ? N9 C18 1.330(15) . ? N9 C17 1.471(15) . ? N9 H9D 0.8800 . ? N10 C18 1.317(14) . ? N10 C19 1.473(15) . ? N10 H10A 0.8800 . ? N11 C23 1.334(15) . ? N11 C22 1.454(15) . ? N11 H11C 0.8800 . ? N12 C23 1.298(15) . ? N12 C24 1.477(15) . ? N12 H12C 0.8800 . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C1 H1E 0.9800 . ? C3 C4 1.506(16) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4C 0.9900 . ? C4 H4D 0.9900 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C5 H5D 0.9800 . ? C7 C8 1.519(18) . ? C7 H7B 0.9900 . ? C7 H7C 0.9900 . ? C8 H8B 0.9900 . ? C8 H8C 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C11 C12 1.493(18) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C15 C16 1.504(17) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C19 C20 1.481(18) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C24 C26 1.501(18) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 Au1 C2 178.4(5) . . ? C6 Au1 Au2 88.6(3) . . ? C2 Au1 Au2 89.9(3) . . ? C6 Au1 Au3 91.1(3) . 1_455 ? C2 Au1 Au3 90.5(3) . 1_455 ? Au2 Au1 Au3 167.998(18) . 1_455 ? C10 Au2 C14 178.8(5) . . ? C10 Au2 Au3 89.3(3) . . ? C14 Au2 Au3 91.8(3) . . ? C10 Au2 Au1 90.7(3) . . ? C14 Au2 Au1 88.4(3) . . ? Au3 Au2 Au1 170.35(2) . . ? C18 Au3 C23 178.1(5) . . ? C18 Au3 Au2 89.8(3) . . ? C23 Au3 Au2 90.7(3) . . ? C18 Au3 Au1 87.5(3) . 1_655 ? C23 Au3 Au1 91.6(3) . 1_655 ? Au2 Au3 Au1 168.42(2) . 1_655 ? F3 P1 F5 90.9(4) . . ? F3 P1 F2 90.6(4) . . ? F5 P1 F2 178.4(5) . . ? F3 P1 F1 90.7(5) . . ? F5 P1 F1 90.2(4) . . ? F2 P1 F1 89.2(4) . . ? F3 P1 F4 91.4(5) . . ? F5 P1 F4 90.8(4) . . ? F2 P1 F4 89.8(4) . . ? F1 P1 F4 177.6(5) . . ? F3 P1 F6 178.7(5) . . ? F5 P1 F6 90.4(4) . . ? F2 P1 F6 88.1(4) . . ? F1 P1 F6 89.2(4) . . ? F4 P1 F6 88.6(5) . . ? F11 P2 F8 179.1(7) . . ? F11 P2 F7 91.1(6) . . ? F8 P2 F7 88.1(7) . . ? F11 P2 F10 88.3(6) . . ? F8 P2 F10 92.5(7) . . ? F7 P2 F10 179.4(6) . . ? F11 P2 F12 91.3(5) . . ? F8 P2 F12 88.3(6) . . ? F7 P2 F12 89.3(5) . . ? F10 P2 F12 90.7(5) . . ? F11 P2 F9 89.1(6) . . ? F8 P2 F9 91.2(7) . . ? F7 P2 F9 91.4(5) . . ? F10 P2 F9 88.5(5) . . ? F12 P2 F9 179.1(7) . . ? C4 O1 H1B 109.5 . . ? C8 O2 H2A 109.5 . . ? C12 O3 H3C 109.5 . . ? C16 O4 H4A 109.5 . . ? C20 O5 H5E 109.5 . . ? C26 O6 H6B 109.5 . . ? C2 N1 C1 126.6(10) . . ? C2 N1 H1A 116.7 . . ? C1 N1 H1A 116.7 . . ? C2 N2 C3 122.3(10) . . ? C2 N2 H2B 118.8 . . ? C3 N2 H2B 118.8 . . ? C6 N3 C5 125.4(12) . . ? C6 N3 H3D 117.3 . . ? C5 N3 H3D 117.3 . . ? C6 N4 C7 124.7(11) . . ? C6 N4 H4B 117.7 . . ? C7 N4 H4B 117.7 . . ? C10 N5 C9 127.0(10) . . ? C10 N5 H5A 116.5 . . ? C9 N5 H5A 116.5 . . ? C10 N6 C11 125.8(10) . . ? C10 N6 H6A 117.1 . . ? C11 N6 H6A 117.1 . . ? C14 N7 C13 124.3(11) . . ? C14 N7 H7A 117.8 . . ? C13 N7 H7A 117.8 . . ? C14 N8 C15 123.7(11) . . ? C14 N8 H8A 118.1 . . ? C15 N8 H8A 118.1 . . ? C18 N9 C17 125.7(10) . . ? C18 N9 H9D 117.2 . . ? C17 N9 H9D 117.2 . . ? C18 N10 C19 123.4(10) . . ? C18 N10 H10A 118.3 . . ? C19 N10 H10A 118.3 . . ? C23 N11 C22 126.9(11) . . ? C23 N11 H11C 116.6 . . ? C22 N11 H11C 116.6 . . ? C23 N12 C24 125.6(11) . . ? C23 N12 H12C 117.2 . . ? C24 N12 H12C 117.2 . . ? N1 C1 H1C 109.5 . . ? N1 C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? N1 C1 H1E 109.5 . . ? H1C C1 H1E 109.5 . . ? H1D C1 H1E 109.5 . . ? N1 C2 N2 115.1(9) . . ? N1 C2 Au1 121.0(8) . . ? N2 C2 Au1 123.8(8) . . ? N2 C3 C4 110.4(10) . . ? N2 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 . . ? N2 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? O1 C4 C3 110.6(10) . . ? O1 C4 H4C 109.5 . . ? C3 C4 H4C 109.5 . . ? O1 C4 H4D 109.5 . . ? C3 C4 H4D 109.5 . . ? H4C C4 H4D 108.1 . . ? N3 C5 H5B 109.5 . . ? N3 C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C5 H5D 109.5 . . ? H5B C5 H5D 109.5 . . ? H5C C5 H5D 109.5 . . ? N3 C6 N4 115.8(10) . . ? N3 C6 Au1 121.4(9) . . ? N4 C6 Au1 122.6(9) . . ? N4 C7 C8 112.3(11) . . ? N4 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? N4 C7 H7C 109.1 . . ? C8 C7 H7C 109.1 . . ? H7B C7 H7C 107.9 . . ? O2 C8 C7 111.2(11) . . ? O2 C8 H8B 109.4 . . ? C7 C8 H8B 109.4 . . ? O2 C8 H8C 109.4 . . ? C7 C8 H8C 109.4 . . ? H8B C8 H8C 108.0 . . ? N5 C9 H9A 109.5 . . ? N5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N5 C10 N6 116.8(11) . . ? N5 C10 Au2 122.0(9) . . ? N6 C10 Au2 121.1(9) . . ? N6 C11 C12 113.4(11) . . ? N6 C11 H11A 108.9 . . ? C12 C11 H11A 108.9 . . ? N6 C11 H11B 108.9 . . ? C12 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? O3 C12 C11 111.8(11) . . ? O3 C12 H12A 109.3 . . ? C11 C12 H12A 109.3 . . ? O3 C12 H12B 109.3 . . ? C11 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? N7 C13 H13A 109.5 . . ? N7 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N7 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N8 C14 N7 118.3(11) . . ? N8 C14 Au2 121.5(9) . . ? N7 C14 Au2 120.2(9) . . ? N8 C15 C16 111.5(10) . . ? N8 C15 H15A 109.3 . . ? C16 C15 H15A 109.3 . . ? N8 C15 H15B 109.3 . . ? C16 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? O4 C16 C15 110.0(10) . . ? O4 C16 H16A 109.7 . . ? C15 C16 H16A 109.7 . . ? O4 C16 H16B 109.7 . . ? C15 C16 H16B 109.7 . . ? H16A C16 H16B 108.2 . . ? N9 C17 H17A 109.5 . . ? N9 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N9 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N10 C18 N9 115.9(10) . . ? N10 C18 Au3 125.3(9) . . ? N9 C18 Au3 118.8(8) . . ? N10 C19 C20 113.4(11) . . ? N10 C19 H19A 108.9 . . ? C20 C19 H19A 108.9 . . ? N10 C19 H19B 108.9 . . ? C20 C19 H19B 108.9 . . ? H19A C19 H19B 107.7 . . ? O5 C20 C19 110.8(12) . . ? O5 C20 H20A 109.5 . . ? C19 C20 H20A 109.5 . . ? O5 C20 H20B 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 108.1 . . ? N11 C22 H22A 109.5 . . ? N11 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N11 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N12 C23 N11 118.3(11) . . ? N12 C23 Au3 124.4(9) . . ? N11 C23 Au3 117.2(8) . . ? N12 C24 C26 112.9(10) . . ? N12 C24 H24A 109.0 . . ? C26 C24 H24A 109.0 . . ? N12 C24 H24B 109.0 . . ? C26 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? O6 C26 C24 113.1(11) . . ? O6 C26 H26A 109.0 . . ? C24 C26 H26A 109.0 . . ? O6 C26 H26B 109.0 . . ? C24 C26 H26B 109.0 . . ? H26A C26 H26B 107.8 . . ? 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 O1 H1B O3 0.84 2.06 2.874(14) 164 1_455 O2 H2A O7 0.84 2.12 2.87(2) 147 . O2 H2A O7 0.84 2.30 2.82(2) 120 3_665 O3 H3C O8 0.84 2.29 2.99(3) 141 2 O4 H4A Cl1 0.84 2.22 3.057(8) 178 2 O5 H5E O8 0.84 2.05 2.83(2) 153 3_565 O6 H6B O4 0.84 2.08 2.925(12) 179 1_655 N1 H1A O4 0.88 2.07 2.940(13) 171 . N2 H2B F6 0.88 2.34 3.166(13) 156 . N3 H3D O6 0.88 1.91 2.781(16) 170 1_455 N5 H5A O2 0.88 2.07 2.934(13) 167 . N6 H6A Cl1 0.88 2.59 3.410(11) 156 . N7 H7A O5 0.88 2.19 3.068(17) 172 . N8 H8A F4 0.88 2.33 3.095(13) 146 2 N9 H9D O1 0.88 2.05 2.907(13) 164 1_655 N10 H10A O7 0.88 2.56 3.34(2) 148 3_665 N11 H11C O3 0.88 2.04 2.903(15) 168 . N12 H12C Cl1 0.88 2.51 3.320(10) 154 2_655 _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 2.885 _refine_diff_density_min -2.290 _refine_diff_density_rms 0.265 # Attachment 'dr99_1.cif' data_dr99 _database_code_depnum_ccdc_archive 'CCDC 686044' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ;[Au{C(NHCH3)(NHCH2CH2OH)}2]3(AsF6)2Cl.0.5(H2O)2 ; _chemical_melting_point ? _chemical_formula_moiety ;3(C8 H20 Au N4 O2), 2(As F6), Cl, 0.5(H2O), 0.5(H2O) ; _chemical_formula_sum 'C24 H62 As2 Au3 Cl F12 N12 O7' _chemical_formula_weight 1635.06 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 9.4814(5) _cell_length_b 20.7388(10) _cell_length_c 24.6413(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.9650(10) _cell_angle_gamma 90.00 _cell_volume 4844.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9532 _cell_measurement_theta_min 2.905 _cell_measurement_theta_max 27.25 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.242 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3088 _exptl_absorpt_coefficient_mu 10.570 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.219 _exptl_absorpt_correction_T_max 0.591 _exptl_absorpt_process_details 'SADABS 2.10 (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61618 _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11123 _reflns_number_gt 7179 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2007)' _computing_cell_refinement SAINT _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXS-97 _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. H atoms on half-occupied water molecules were not located. Other H atoms were treated as riding on their bonded atoms. ; _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^)+(0.0386P)^2^] 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 11123 _refine_ls_number_parameters 555 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0722 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0846 _refine_ls_wR_factor_gt 0.0758 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.40430(2) 0.742252(11) 0.641036(10) 0.04167(7) Uani 1 1 d . . . Au2 Au 0.73603(2) 0.738273(11) 0.624402(10) 0.04276(7) Uani 1 1 d . . . Au3 Au 1.07114(2) 0.760702(12) 0.631795(9) 0.04267(7) Uani 1 1 d . . . As1 As 0.31272(8) 0.39099(3) 0.60549(3) 0.0641(2) Uani 1 1 d . . . As2 As 0.91079(7) 0.91063(3) 0.38244(3) 0.05667(18) Uani 1 1 d . . . Cl1 Cl 0.89958(16) 0.46182(8) 0.69747(7) 0.0642(5) Uani 1 1 d . . . F1 F 0.4135(6) 0.4584(2) 0.6077(2) 0.1273(19) Uani 1 1 d . . . F2 F 0.2198(5) 0.3207(2) 0.6052(2) 0.1110(16) Uani 1 1 d . . . F3 F 0.4569(5) 0.3469(2) 0.6256(2) 0.1074(16) Uani 1 1 d . . . F4 F 0.3527(5) 0.3780(2) 0.54041(17) 0.1138(17) Uani 1 1 d . . . F5 F 0.2728(5) 0.4001(2) 0.67278(17) 0.1012(15) Uani 1 1 d . . . F6 F 0.1751(6) 0.4365(3) 0.5882(2) 0.143(2) Uani 1 1 d . . . F7 F 0.7341(5) 0.9147(3) 0.3808(3) 0.136(2) Uani 1 1 d . . . F8 F 1.0871(5) 0.9071(3) 0.3841(2) 0.157(3) Uani 1 1 d . . . F9 F 0.9081(8) 0.8344(3) 0.4019(3) 0.185(3) Uani 1 1 d . . . F10 F 0.9090(7) 0.9335(3) 0.4473(2) 0.177(3) Uani 1 1 d . . . F11 F 0.9123(7) 0.9879(3) 0.3654(3) 0.171(3) Uani 1 1 d . . . F12 F 0.9149(6) 0.8865(3) 0.31867(19) 0.152(2) Uani 1 1 d . . . O1 O 0.7108(5) 0.7755(2) 0.7810(2) 0.0801(15) Uani 1 1 d . . . H1E H 0.7672 0.7551 0.8012 0.120 Uiso 1 1 calc R . . O2 O 0.1021(4) 0.57820(19) 0.69277(16) 0.0567(11) Uani 1 1 d . . . H2B H 0.0434 0.5479 0.6928 0.085 Uiso 1 1 calc R . . O3 O 0.4370(5) 0.7767(2) 0.4881(2) 0.0905(17) Uani 1 1 d . . . H3D H 0.3679 0.7795 0.4664 0.136 Uiso 1 1 calc R . . O4 O 1.0197(5) 0.5903(2) 0.57810(18) 0.0768(14) Uani 1 1 d . . . H4D H 1.0430 0.5882 0.6111 0.115 Uiso 1 1 calc R . . O5 O 1.3656(4) 0.8958(2) 0.53224(17) 0.0639(12) Uani 1 1 d . . . H5E H 1.4192 0.9278 0.5357 0.096 Uiso 1 1 calc R . . O6 O 0.8025(4) 0.8947(2) 0.72959(17) 0.0584(11) Uani 1 1 d . . . H6B H 0.7896 0.8603 0.7467 0.088 Uiso 1 1 calc R . . O7 O 0.2701(16) 0.7937(8) 0.3893(6) 0.158(6) Uiso 0.50 1 d P . . O8 O 0.5487(9) 0.9681(5) 0.4666(4) 0.078(3) Uiso 0.50 1 d P . . N1 N 0.4161(5) 0.8834(2) 0.6508(2) 0.0476(12) Uani 1 1 d . . . H1A H 0.4006 0.8791 0.6157 0.057 Uiso 1 1 calc R . . N2 N 0.4519(5) 0.8350(2) 0.73242(19) 0.0445(11) Uani 1 1 d . . . H2A H 0.4660 0.8740 0.7456 0.053 Uiso 1 1 calc R . . N3 N 0.3859(5) 0.6499(2) 0.5501(2) 0.0529(13) Uani 1 1 d . . . H3C H 0.4066 0.6850 0.5318 0.064 Uiso 1 1 calc R . . N4 N 0.3559(5) 0.6017(2) 0.63055(19) 0.0497(12) Uani 1 1 d . . . H4A H 0.3429 0.5659 0.6119 0.060 Uiso 1 1 calc R . . N5 N 0.7528(5) 0.8793(2) 0.6127(2) 0.0479(12) Uani 1 1 d . . . H5D H 0.7708 0.8756 0.6477 0.057 Uiso 1 1 calc R . . N6 N 0.7080(5) 0.8306(2) 0.5323(2) 0.0496(12) Uani 1 1 d . . . H6A H 0.7047 0.8699 0.5187 0.060 Uiso 1 1 calc R . . N7 N 0.7394(5) 0.6562(2) 0.7200(2) 0.0514(13) Uani 1 1 d . . . H7C H 0.7287 0.6947 0.7343 0.062 Uiso 1 1 calc R . . N8 N 0.7599(5) 0.5958(2) 0.6439(2) 0.0500(12) Uani 1 1 d . . . H8C H 0.7667 0.5623 0.6657 0.060 Uiso 1 1 calc R . . N9 N 1.0639(5) 0.7065(3) 0.5219(2) 0.0584(14) Uani 1 1 d . . . H9D H 1.0426 0.6719 0.5408 0.070 Uiso 1 1 calc R . . N10 N 1.1065(5) 0.8130(3) 0.5204(2) 0.0555(13) Uani 1 1 d . . . H10A H 1.1169 0.8088 0.4851 0.067 Uiso 1 1 calc R . . N11 N 1.0690(5) 0.7071(2) 0.74242(19) 0.0480(12) Uani 1 1 d . . . H11C H 1.0755 0.6712 0.7235 0.058 Uiso 1 1 calc R . . N12 N 1.0564(5) 0.8152(2) 0.74325(18) 0.0449(12) Uani 1 1 d . . . H12C H 1.0530 0.8117 0.7788 0.054 Uiso 1 1 calc R . . C1 C 0.4267(7) 0.9487(3) 0.6711(3) 0.0611(18) Uani 1 1 d . . . H1B H 0.4048 0.9791 0.6417 0.092 Uiso 1 1 calc R . . H1C H 0.5228 0.9565 0.6849 0.092 Uiso 1 1 calc R . . H1D H 0.3597 0.9547 0.7006 0.092 Uiso 1 1 calc R . . C2 C 0.4271(5) 0.8295(3) 0.6793(2) 0.0399(13) Uani 1 1 d . . . C3 C 0.4572(7) 0.7811(3) 0.7704(3) 0.0573(17) Uani 1 1 d . . . H3A H 0.4606 0.7402 0.7497 0.069 Uiso 1 1 calc R . . H3B H 0.3701 0.7808 0.7920 0.069 Uiso 1 1 calc R . . C4 C 0.5826(9) 0.7846(3) 0.8080(3) 0.074(2) Uani 1 1 d . . . H4B H 0.5840 0.8273 0.8260 0.089 Uiso 1 1 calc R . . H4C H 0.5735 0.7513 0.8364 0.089 Uiso 1 1 calc R . . C5 C 0.3618(7) 0.5914(3) 0.5189(3) 0.068(2) Uani 1 1 d . . . H5A H 0.3798 0.5999 0.4805 0.102 Uiso 1 1 calc R . . H5B H 0.2638 0.5774 0.5230 0.102 Uiso 1 1 calc R . . H5C H 0.4254 0.5574 0.5321 0.102 Uiso 1 1 calc R . . C6 C 0.3796(5) 0.6553(3) 0.6033(2) 0.0421(13) Uani 1 1 d . . . C7 C 0.3499(6) 0.5978(3) 0.6902(2) 0.0548(16) Uani 1 1 d . . . H7A H 0.3344 0.6415 0.7052 0.066 Uiso 1 1 calc R . . H7B H 0.4416 0.5819 0.7047 0.066 Uiso 1 1 calc R . . C8 C 0.2363(6) 0.5545(3) 0.7085(2) 0.0548(16) Uani 1 1 d . . . H8A H 0.2500 0.5111 0.6928 0.066 Uiso 1 1 calc R . . H8B H 0.2414 0.5505 0.7486 0.066 Uiso 1 1 calc R . . C9 C 0.7502(7) 0.9437(3) 0.5909(3) 0.0614(18) Uani 1 1 d . . . H9A H 0.7717 0.9747 0.6199 0.092 Uiso 1 1 calc R . . H9B H 0.6565 0.9528 0.5754 0.092 Uiso 1 1 calc R . . H9C H 0.8209 0.9475 0.5625 0.092 Uiso 1 1 calc R . . C10 C 0.7308(5) 0.8247(3) 0.5854(2) 0.0421(13) Uani 1 1 d . . . C11 C 0.6881(6) 0.7771(3) 0.4949(3) 0.0547(16) Uani 1 1 d . . . H11A H 0.6799 0.7366 0.5159 0.066 Uiso 1 1 calc R . . H11B H 0.7719 0.7734 0.4717 0.066 Uiso 1 1 calc R . . C12 C 0.5609(8) 0.7851(4) 0.4601(3) 0.072(2) Uani 1 1 d . . . H12A H 0.5615 0.8289 0.4440 0.086 Uiso 1 1 calc R . . H12B H 0.5640 0.7536 0.4300 0.086 Uiso 1 1 calc R . . C13 C 0.7474(7) 0.6025(3) 0.7574(2) 0.0606(18) Uani 1 1 d . . . H13A H 0.7248 0.6173 0.7940 0.091 Uiso 1 1 calc R . . H13B H 0.8430 0.5845 0.7575 0.091 Uiso 1 1 calc R . . H13C H 0.6798 0.5692 0.7460 0.091 Uiso 1 1 calc R . . C14 C 0.7465(5) 0.6532(3) 0.6660(2) 0.0430(14) Uani 1 1 d . . . C15 C 0.7641(6) 0.5839(3) 0.5854(2) 0.0588(17) Uani 1 1 d . . . H15A H 0.7546 0.6254 0.5659 0.071 Uiso 1 1 calc R . . H15B H 0.6829 0.5565 0.5746 0.071 Uiso 1 1 calc R . . C16 C 0.9000(7) 0.5510(3) 0.5682(3) 0.0641(19) Uani 1 1 d . . . H16A H 0.9112 0.5100 0.5884 0.077 Uiso 1 1 calc R . . H16B H 0.8935 0.5406 0.5291 0.077 Uiso 1 1 calc R . . C17 C 1.0762(7) 0.6985(4) 0.4627(3) 0.078(2) Uani 1 1 d . . . H17A H 1.0509 0.6542 0.4526 0.117 Uiso 1 1 calc R . . H17B H 1.1734 0.7073 0.4521 0.117 Uiso 1 1 calc R . . H17C H 1.0123 0.7287 0.4441 0.117 Uiso 1 1 calc R . . C18 C 1.0821(5) 0.7607(3) 0.5491(2) 0.0457(14) Uani 1 1 d . . . C19 C 1.1174(6) 0.8779(3) 0.5438(3) 0.0593(17) Uani 1 1 d . . . H19A H 1.1403 0.8744 0.5830 0.071 Uiso 1 1 calc R . . H19B H 1.0251 0.8999 0.5399 0.071 Uiso 1 1 calc R . . C20 C 1.2271(7) 0.9172(3) 0.5171(3) 0.0615(17) Uani 1 1 d . . . H20A H 1.2147 0.9141 0.4772 0.074 Uiso 1 1 calc R . . H20B H 1.2159 0.9630 0.5276 0.074 Uiso 1 1 calc R . . C21 C 1.0651(7) 0.7008(3) 0.8008(2) 0.0617(18) Uani 1 1 d . . . H21A H 1.0701 0.6551 0.8108 0.093 Uiso 1 1 calc R . . H21B H 0.9770 0.7193 0.8141 0.093 Uiso 1 1 calc R . . H21C H 1.1454 0.7239 0.8172 0.093 Uiso 1 1 calc R . . C22 C 1.0637(5) 0.7620(3) 0.7147(2) 0.0405(13) Uani 1 1 d . . . C23 C 1.0537(6) 0.8800(3) 0.7201(3) 0.0513(16) Uani 1 1 d . . . H23A H 1.0399 0.8770 0.6802 0.062 Uiso 1 1 calc R . . H23B H 1.1455 0.9014 0.7273 0.062 Uiso 1 1 calc R . . C24 C 0.9375(6) 0.9202(3) 0.7435(3) 0.0545(16) Uani 1 1 d . . . H24A H 0.9486 0.9215 0.7835 0.065 Uiso 1 1 calc R . . H24B H 0.9446 0.9649 0.7297 0.065 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 Au1 0.03576(12) 0.03968(13) 0.04964(14) -0.00356(10) 0.00253(9) -0.00247(10) Au2 0.03722(13) 0.03987(13) 0.05124(14) 0.00650(10) 0.00268(9) 0.00463(10) Au3 0.03736(12) 0.05071(14) 0.03996(13) -0.00208(10) 0.00151(9) 0.00307(10) As1 0.0827(5) 0.0539(4) 0.0555(4) -0.0020(3) -0.0047(4) 0.0058(4) As2 0.0600(4) 0.0605(5) 0.0494(4) 0.0087(3) -0.0029(3) 0.0030(3) Cl1 0.0557(10) 0.0503(10) 0.0869(12) 0.0254(9) 0.0068(9) -0.0007(8) F1 0.165(5) 0.063(3) 0.154(5) 0.002(3) 0.020(4) -0.020(3) F2 0.106(3) 0.106(4) 0.121(4) -0.026(3) 0.012(3) -0.035(3) F3 0.104(3) 0.085(4) 0.132(4) -0.014(3) -0.036(3) 0.023(3) F4 0.153(4) 0.122(4) 0.067(3) 0.000(3) 0.019(3) 0.004(3) F5 0.150(4) 0.083(3) 0.070(3) -0.001(2) 0.007(3) 0.010(3) F6 0.148(5) 0.182(6) 0.101(4) 0.032(4) -0.001(3) 0.099(4) F7 0.064(3) 0.112(4) 0.232(7) -0.017(4) -0.003(3) 0.004(3) F8 0.065(3) 0.250(8) 0.156(5) -0.081(5) -0.008(3) 0.014(4) F9 0.249(7) 0.093(4) 0.215(7) 0.071(4) 0.101(6) 0.065(5) F10 0.218(6) 0.239(7) 0.074(3) -0.048(4) -0.023(4) 0.137(6) F11 0.194(6) 0.083(4) 0.237(8) 0.053(4) 0.020(6) -0.026(4) F12 0.152(5) 0.239(7) 0.064(3) -0.030(4) -0.012(3) 0.035(5) O1 0.078(3) 0.054(3) 0.108(4) 0.002(3) -0.029(3) 0.012(3) O2 0.051(3) 0.054(3) 0.065(3) 0.007(2) 0.009(2) -0.008(2) O3 0.073(4) 0.086(4) 0.112(5) -0.023(3) -0.018(3) 0.013(3) O4 0.075(3) 0.100(4) 0.056(3) 0.019(3) 0.010(3) -0.008(3) O5 0.057(3) 0.070(3) 0.065(3) -0.012(2) -0.001(2) -0.010(2) O6 0.054(3) 0.055(3) 0.066(3) -0.009(2) -0.005(2) 0.007(2) N1 0.049(3) 0.045(3) 0.049(3) 0.005(2) -0.006(2) 0.002(2) N2 0.046(3) 0.037(3) 0.050(3) -0.001(2) -0.002(2) -0.003(2) N3 0.056(3) 0.050(3) 0.054(3) -0.002(3) 0.013(3) -0.007(3) N4 0.053(3) 0.048(3) 0.047(3) -0.007(2) 0.003(2) -0.010(2) N5 0.048(3) 0.045(3) 0.051(3) -0.002(2) -0.005(2) 0.002(2) N6 0.059(3) 0.032(3) 0.058(3) 0.007(2) -0.003(3) 0.004(2) N7 0.057(3) 0.046(3) 0.051(3) 0.003(2) 0.012(3) 0.003(2) N8 0.056(3) 0.040(3) 0.054(3) 0.005(2) -0.001(3) 0.012(2) N9 0.055(3) 0.068(4) 0.052(3) -0.006(3) -0.010(3) -0.001(3) N10 0.059(3) 0.069(4) 0.038(3) 0.003(3) 0.007(2) 0.000(3) N11 0.052(3) 0.042(3) 0.050(3) 0.003(2) 0.000(2) 0.006(2) N12 0.052(3) 0.048(3) 0.036(3) -0.002(2) 0.006(2) 0.006(2) C1 0.074(5) 0.033(4) 0.076(5) 0.000(3) -0.004(4) 0.003(3) C2 0.024(3) 0.045(4) 0.050(4) -0.005(3) 0.001(2) 0.006(2) C3 0.071(4) 0.048(4) 0.053(4) 0.006(3) 0.013(3) -0.007(3) C4 0.135(7) 0.040(4) 0.046(4) 0.002(3) -0.012(5) 0.000(4) C5 0.074(5) 0.077(5) 0.053(4) -0.022(4) 0.008(4) -0.006(4) C6 0.034(3) 0.048(4) 0.044(3) -0.003(3) 0.008(3) -0.002(3) C7 0.053(4) 0.063(4) 0.048(4) -0.002(3) 0.004(3) -0.015(3) C8 0.068(4) 0.044(4) 0.053(4) 0.006(3) 0.001(3) -0.011(3) C9 0.065(4) 0.042(4) 0.077(5) -0.003(3) -0.005(4) -0.010(3) C10 0.030(3) 0.048(4) 0.048(4) 0.005(3) 0.003(3) 0.003(3) C11 0.059(4) 0.051(4) 0.055(4) -0.002(3) 0.001(3) 0.011(3) C12 0.092(6) 0.072(5) 0.051(4) -0.019(4) -0.005(4) 0.005(4) C13 0.076(4) 0.051(4) 0.055(4) 0.011(3) 0.017(3) 0.004(3) C14 0.028(3) 0.046(4) 0.055(4) 0.006(3) 0.000(3) 0.003(2) C15 0.061(4) 0.057(4) 0.057(4) 0.000(3) -0.010(3) 0.005(3) C16 0.091(5) 0.049(4) 0.052(4) -0.001(3) 0.010(4) 0.007(4) C17 0.081(5) 0.100(6) 0.053(4) -0.020(4) -0.010(4) 0.014(5) C18 0.031(3) 0.061(4) 0.046(3) -0.009(3) -0.003(2) 0.002(3) C19 0.050(4) 0.065(5) 0.063(4) 0.000(4) 0.012(3) 0.011(3) C20 0.067(4) 0.059(4) 0.058(4) 0.005(3) 0.003(4) 0.004(4) C21 0.075(5) 0.064(5) 0.046(4) 0.013(3) -0.001(3) 0.001(4) C22 0.029(3) 0.053(4) 0.040(3) -0.007(3) 0.003(2) 0.004(3) C23 0.054(4) 0.043(4) 0.058(4) -0.002(3) 0.009(3) 0.005(3) C24 0.056(4) 0.048(4) 0.059(4) -0.007(3) 0.001(3) 0.006(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 C6 2.040(6) . ? Au1 C2 2.049(5) . ? Au1 Au2 3.1797(3) . ? Au1 Au3 3.1862(3) 1_455 ? Au2 C10 2.035(6) . ? Au2 C14 2.042(6) . ? Au2 Au3 3.2134(3) . ? Au3 C18 2.042(6) . ? Au3 C22 2.046(5) . ? Au3 Au1 3.1862(3) 1_655 ? As1 F6 1.660(4) . ? As1 F4 1.676(4) . ? As1 F1 1.693(5) . ? As1 F2 1.703(5) . ? As1 F3 1.711(4) . ? As1 F5 1.718(4) . ? As2 F12 1.650(5) . ? As2 F9 1.652(5) . ? As2 F11 1.656(5) . ? As2 F10 1.668(5) . ? As2 F8 1.673(5) . ? As2 F7 1.678(4) . ? O1 C4 1.408(8) . ? O1 H1E 0.8400 . ? O2 C8 1.412(7) . ? O2 H2B 0.8400 . ? O3 C12 1.384(8) . ? O3 H3D 0.8400 . ? O4 C16 1.416(7) . ? O4 H4D 0.8400 . ? O5 C20 1.429(7) . ? O5 H5E 0.8400 . ? O6 C24 1.420(7) . ? O6 H6B 0.8400 . ? N1 C2 1.324(7) . ? N1 C1 1.446(7) . ? N1 H1A 0.8800 . ? N2 C2 1.331(7) . ? N2 C3 1.458(7) . ? N2 H2A 0.8800 . ? N3 C6 1.318(7) . ? N3 C5 1.452(7) . ? N3 H3C 0.8800 . ? N4 C6 1.320(7) . ? N4 C7 1.475(7) . ? N4 H4A 0.8800 . ? N5 C10 1.330(7) . ? N5 C9 1.441(7) . ? N5 H5D 0.8800 . ? N6 C10 1.329(7) . ? N6 C11 1.454(7) . ? N6 H6A 0.8800 . ? N7 C14 1.334(7) . ? N7 C13 1.447(7) . ? N7 H7C 0.8800 . ? N8 C14 1.317(7) . ? N8 C15 1.465(7) . ? N8 H8C 0.8800 . ? N9 C18 1.319(7) . ? N9 C17 1.474(7) . ? N9 H9D 0.8800 . ? N10 C18 1.318(7) . ? N10 C19 1.467(8) . ? N10 H10A 0.8800 . ? N11 C22 1.329(7) . ? N11 C21 1.446(7) . ? N11 H11C 0.8800 . ? N12 C22 1.311(7) . ? N12 C23 1.460(7) . ? N12 H12C 0.8800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C3 C4 1.497(9) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4B 0.9900 . ? C4 H4C 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C7 C8 1.478(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C11 C12 1.478(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C15 C16 1.523(8) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C19 C20 1.484(8) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C23 C24 1.504(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 Au1 C2 179.4(2) . . ? C6 Au1 Au2 91.41(14) . . ? C2 Au1 Au2 89.15(13) . . ? C6 Au1 Au3 88.13(15) . 1_455 ? C2 Au1 Au3 91.36(13) . 1_455 ? Au2 Au1 Au3 167.291(10) . 1_455 ? C10 Au2 C14 177.6(2) . . ? C10 Au2 Au1 91.24(14) . . ? C14 Au2 Au1 89.86(14) . . ? C10 Au2 Au3 85.15(14) . . ? C14 Au2 Au3 93.26(14) . . ? Au1 Au2 Au3 165.513(11) . . ? C18 Au3 C22 178.8(2) . . ? C18 Au3 Au1 90.25(15) . 1_655 ? C22 Au3 Au1 88.92(14) . 1_655 ? C18 Au3 Au2 90.59(15) . . ? C22 Au3 Au2 90.45(14) . . ? Au1 Au3 Au2 164.757(11) 1_655 . ? F6 As1 F4 92.0(3) . . ? F6 As1 F1 88.9(3) . . ? F4 As1 F1 91.5(3) . . ? F6 As1 F2 94.6(3) . . ? F4 As1 F2 89.1(2) . . ? F1 As1 F2 176.5(3) . . ? F6 As1 F3 177.2(3) . . ? F4 As1 F3 89.9(2) . . ? F1 As1 F3 89.1(2) . . ? F2 As1 F3 87.4(2) . . ? F6 As1 F5 90.0(2) . . ? F4 As1 F5 177.0(2) . . ? F1 As1 F5 90.7(2) . . ? F2 As1 F5 88.6(2) . . ? F3 As1 F5 88.1(2) . . ? F12 As2 F9 89.2(3) . . ? F12 As2 F11 93.0(3) . . ? F9 As2 F11 177.8(3) . . ? F12 As2 F10 178.6(3) . . ? F9 As2 F10 89.6(4) . . ? F11 As2 F10 88.2(3) . . ? F12 As2 F8 88.3(3) . . ? F9 As2 F8 88.3(4) . . ? F11 As2 F8 92.0(3) . . ? F10 As2 F8 90.9(3) . . ? F12 As2 F7 91.9(3) . . ? F9 As2 F7 92.0(3) . . ? F11 As2 F7 87.6(3) . . ? F10 As2 F7 89.0(3) . . ? F8 As2 F7 179.6(3) . . ? C4 O1 H1E 109.5 . . ? C8 O2 H2B 109.5 . . ? C12 O3 H3D 109.5 . . ? C16 O4 H4D 109.5 . . ? C20 O5 H5E 109.5 . . ? C24 O6 H6B 109.5 . . ? C2 N1 C1 127.1(5) . . ? C2 N1 H1A 116.4 . . ? C1 N1 H1A 116.4 . . ? C2 N2 C3 124.6(5) . . ? C2 N2 H2A 117.7 . . ? C3 N2 H2A 117.7 . . ? C6 N3 C5 126.1(5) . . ? C6 N3 H3C 116.9 . . ? C5 N3 H3C 116.9 . . ? C6 N4 C7 124.3(5) . . ? C6 N4 H4A 117.9 . . ? C7 N4 H4A 117.9 . . ? C10 N5 C9 126.8(5) . . ? C10 N5 H5D 116.6 . . ? C9 N5 H5D 116.6 . . ? C10 N6 C11 124.8(5) . . ? C10 N6 H6A 117.6 . . ? C11 N6 H6A 117.6 . . ? C14 N7 C13 126.6(5) . . ? C14 N7 H7C 116.7 . . ? C13 N7 H7C 116.7 . . ? C14 N8 C15 124.4(5) . . ? C14 N8 H8C 117.8 . . ? C15 N8 H8C 117.8 . . ? C18 N9 C17 125.9(6) . . ? C18 N9 H9D 117.0 . . ? C17 N9 H9D 117.0 . . ? C18 N10 C19 123.7(5) . . ? C18 N10 H10A 118.1 . . ? C19 N10 H10A 118.1 . . ? C22 N11 C21 125.9(5) . . ? C22 N11 H11C 117.1 . . ? C21 N11 H11C 117.1 . . ? C22 N12 C23 124.5(5) . . ? C22 N12 H12C 117.8 . . ? C23 N12 H12C 117.8 . . ? N1 C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? N1 C2 N2 117.3(5) . . ? N1 C2 Au1 119.7(4) . . ? N2 C2 Au1 123.0(4) . . ? N2 C3 C4 112.2(5) . . ? N2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? N2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? O1 C4 C3 112.6(5) . . ? O1 C4 H4B 109.1 . . ? C3 C4 H4B 109.1 . . ? O1 C4 H4C 109.1 . . ? C3 C4 H4C 109.1 . . ? H4B C4 H4C 107.8 . . ? N3 C5 H5A 109.5 . . ? N3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 N4 116.4(5) . . ? N3 C6 Au1 121.5(4) . . ? N4 C6 Au1 122.2(4) . . ? N4 C7 C8 112.2(5) . . ? N4 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? N4 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? O2 C8 C7 111.3(5) . . ? O2 C8 H8A 109.4 . . ? C7 C8 H8A 109.4 . . ? O2 C8 H8B 109.4 . . ? C7 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? N5 C9 H9A 109.5 . . ? N5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N6 C10 N5 116.2(5) . . ? N6 C10 Au2 123.3(4) . . ? N5 C10 Au2 120.5(4) . . ? N6 C11 C12 112.2(5) . . ? N6 C11 H11A 109.2 . . ? C12 C11 H11A 109.2 . . ? N6 C11 H11B 109.2 . . ? C12 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? O3 C12 C11 112.8(6) . . ? O3 C12 H12A 109.0 . . ? C11 C12 H12A 109.0 . . ? O3 C12 H12B 109.0 . . ? C11 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? N7 C13 H13A 109.5 . . ? N7 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N7 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N8 C14 N7 117.5(5) . . ? N8 C14 Au2 125.3(4) . . ? N7 C14 Au2 117.3(4) . . ? N8 C15 C16 112.7(5) . . ? N8 C15 H15A 109.0 . . ? C16 C15 H15A 109.0 . . ? N8 C15 H15B 109.0 . . ? C16 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? O4 C16 C15 111.9(5) . . ? O4 C16 H16A 109.2 . . ? C15 C16 H16A 109.2 . . ? O4 C16 H16B 109.2 . . ? C15 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? N9 C17 H17A 109.5 . . ? N9 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N9 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N10 C18 N9 116.8(6) . . ? N10 C18 Au3 123.3(5) . . ? N9 C18 Au3 119.9(5) . . ? N10 C19 C20 112.0(5) . . ? N10 C19 H19A 109.2 . . ? C20 C19 H19A 109.2 . . ? N10 C19 H19B 109.2 . . ? C20 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? O5 C20 C19 111.2(5) . . ? O5 C20 H20A 109.4 . . ? C19 C20 H20A 109.4 . . ? O5 C20 H20B 109.4 . . ? C19 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? N11 C21 H21A 109.5 . . ? N11 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N11 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N12 C22 N11 116.7(5) . . ? N12 C22 Au3 123.3(4) . . ? N11 C22 Au3 120.0(4) . . ? N12 C23 C24 111.6(5) . . ? N12 C23 H23A 109.3 . . ? C24 C23 H23A 109.3 . . ? N12 C23 H23B 109.3 . . ? C24 C23 H23B 109.3 . . ? H23A C23 H23B 108.0 . . ? O6 C24 C23 111.4(5) . . ? O6 C24 H24A 109.4 . . ? C23 C24 H24A 109.4 . . ? O6 C24 H24B 109.4 . . ? C23 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? 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 O1 H1E O7 0.84 2.39 3.075(16) 138 4_676 O2 H2B Cl1 0.84 2.25 3.088(4) 175 1_455 O3 H3D O7 0.84 2.12 2.902(16) 155 . O4 H4D O2 0.84 2.09 2.930(6) 177 1_655 O5 H5E O8 0.84 2.18 2.937(10) 150 3_776 O5 H5E O8 0.84 2.27 2.823(10) 123 1_655 O6 H6B O1 0.84 2.09 2.917(6) 167 . N1 H1A O5 0.88 2.11 2.965(6) 165 1_455 N2 H2A Cl1 0.88 2.62 3.436(5) 155 2_656 N3 H3C O3 0.88 2.21 3.084(8) 174 . N4 H4A F1 0.88 2.33 3.076(7) 142 . N5 H5D O6 0.88 2.07 2.929(6) 164 . N7 H7C O1 0.88 2.04 2.910(7) 169 . N8 H8C Cl1 0.88 2.55 3.340(5) 150 . N9 H9D O4 0.88 1.94 2.814(7) 172 . N11 H11C O2 0.88 2.09 2.958(6) 169 1_655 N12 H12C F3 0.88 2.47 3.301(7) 158 2_656 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.533 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.135