Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Kunihiko Kitadai' _publ_contact_author_address ; Department of Chemistry, Faculty of Science Toho University Funabashi 274-8510 JAPAN ; _publ_contact_author_email KITADAI@CHEM.SCI.TOHO-U.AC.JP _publ_section_title ; Synthesis, structure and reaction of a cyclometallated gold(I) complexes having bridging and bidentate and (2-diphenylarsino-n-methyl)phenyl (n = 5, 6) ; loop_ _publ_author_name 'Kunihiko Kitadai' 'Masashi Takahashi' 'Masuo Takeda' 'Steven H. Priver' 'Suresh K. Bhargava' ; M.A.Bennett ; data_compound2a _database_code_depnum_ccdc_archive 'CCDC 290381' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H32 As2 Au2 Cl2' _chemical_formula_weight 1103.31 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' 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 Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 17.4586(14) _cell_length_b 12.1644(10) _cell_length_c 16.7311(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3553.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.062 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2072 _exptl_absorpt_coefficient_mu 10.273 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS Sheldrick 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25230 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 28.37 _reflns_number_total 4443 _reflns_number_gt 3778 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+1.1606P] 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 4443 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0603 _refine_ls_wR_factor_gt 0.0564 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 As2 As 0.270421(19) 0.55613(3) 0.155375(17) 0.03190(8) Uani 1 1 d . . . Au1 Au 0.321610(6) 0.728901(10) 0.100444(7) 0.02987(5) Uani 1 1 d . . . C1 C 0.19632(17) 0.5260(3) 0.07378(18) 0.0344(6) Uani 1 1 d . . . C2 C 0.18213(18) 0.4245(3) 0.0400(2) 0.0429(8) Uani 1 1 d . . . C3 C 0.1306(2) 0.4153(3) -0.0228(2) 0.0461(8) Uani 1 1 d . . . C4 C 0.09270(18) 0.5071(3) -0.05161(19) 0.0410(7) Uani 1 1 d . . . C5 C 0.10699(18) 0.6092(3) -0.01610(18) 0.0380(7) Uani 1 1 d . . . C6 C 0.15824(18) 0.6208(3) 0.04636(17) 0.0332(6) Uani 1 1 d . . . C7 C 0.0364(2) 0.4970(4) -0.1199(2) 0.0564(10) Uani 1 1 d . . . C8 C 0.33336(19) 0.4272(3) 0.1685(2) 0.0397(7) Uani 1 1 d . . . C9 C 0.3316(3) 0.3676(4) 0.2379(3) 0.0650(12) Uani 1 1 d . . . C10 C 0.3807(4) 0.2788(4) 0.2482(4) 0.093(2) Uani 1 1 d . . . C11 C 0.4306(3) 0.2520(4) 0.1891(5) 0.0909(19) Uani 1 1 d . . . C12 C 0.4314(3) 0.3092(5) 0.1184(4) 0.0822(16) Uani 1 1 d . . . C13 C 0.3833(2) 0.3986(4) 0.1084(3) 0.0616(11) Uani 1 1 d . . . C14 C 0.21103(18) 0.5647(3) 0.25217(18) 0.0359(7) Uani 1 1 d . . . C15 C 0.2425(2) 0.6076(4) 0.3207(3) 0.0648(12) Uani 1 1 d . . . C16 C 0.1991(3) 0.6126(6) 0.3897(2) 0.0815(18) Uani 1 1 d . . . C17 C 0.1263(3) 0.5750(5) 0.3915(2) 0.0702(14) Uani 1 1 d . . . C18 C 0.0945(3) 0.5319(4) 0.3235(3) 0.0731(13) Uani 1 1 d . . . C19 C 0.1368(2) 0.5271(4) 0.2532(2) 0.0565(10) Uani 1 1 d . . . Cl1 Cl 0.45272(5) 0.68194(9) 0.10181(6) 0.0531(2) Uani 1 1 d . . . H2 H 0.2070 0.3623 0.0593 0.051 Uiso 1 1 calc R . . H3 H 0.1215 0.3469 -0.0457 0.055 Uiso 1 1 calc R . . H5 H 0.0813 0.6709 -0.0350 0.046 Uiso 1 1 calc R . . H7A H 0.0593 0.5251 -0.1679 0.085 Uiso 1 1 calc R . . H7B H -0.0089 0.5384 -0.1077 0.085 Uiso 1 1 calc R . . H7C H 0.0232 0.4211 -0.1273 0.085 Uiso 1 1 calc R . . H9 H 0.2974 0.3866 0.2783 0.078 Uiso 1 1 calc R . . H10 H 0.3795 0.2381 0.2952 0.112 Uiso 1 1 calc R . . H11 H 0.4646 0.1941 0.1966 0.109 Uiso 1 1 calc R . . H12 H 0.4642 0.2880 0.0774 0.099 Uiso 1 1 calc R . . H13 H 0.3848 0.4392 0.0613 0.074 Uiso 1 1 calc R . . H15 H 0.2927 0.6332 0.3206 0.078 Uiso 1 1 calc R . . H16 H 0.2204 0.6425 0.4358 0.098 Uiso 1 1 calc R . . H17 H 0.0980 0.5783 0.4386 0.084 Uiso 1 1 calc R . . H18 H 0.0444 0.5058 0.3244 0.088 Uiso 1 1 calc R . . H19 H 0.1150 0.4986 0.2070 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 As2 0.03338(16) 0.02927(16) 0.03304(16) 0.00123(12) -0.00262(11) 0.00291(12) Au1 0.02774(8) 0.02974(9) 0.03213(8) 0.00078(4) -0.00098(4) 0.00300(4) C1 0.0313(15) 0.0399(18) 0.0320(14) -0.0007(13) -0.0020(12) 0.0010(13) C2 0.047(2) 0.036(2) 0.0456(19) -0.0028(15) -0.0036(14) 0.0018(14) C3 0.054(2) 0.0373(19) 0.0466(18) -0.0102(15) -0.0053(16) -0.0048(16) C4 0.0365(17) 0.048(2) 0.0385(16) -0.0062(15) -0.0030(13) -0.0017(14) C5 0.0342(16) 0.0392(18) 0.0407(16) -0.0007(14) -0.0041(13) 0.0046(13) C6 0.0318(14) 0.0339(17) 0.0338(14) -0.0038(13) 0.0021(12) -0.0007(12) C7 0.052(2) 0.065(3) 0.052(2) -0.0127(19) -0.0142(17) 0.000(2) C8 0.0356(17) 0.0285(17) 0.0548(19) -0.0018(15) -0.0095(14) 0.0050(13) C9 0.091(3) 0.046(3) 0.058(2) 0.002(2) -0.008(2) 0.023(2) C10 0.136(5) 0.049(3) 0.095(4) 0.000(3) -0.033(4) 0.041(3) C11 0.078(4) 0.048(3) 0.146(6) -0.022(3) -0.037(4) 0.030(3) C12 0.053(3) 0.051(3) 0.142(5) -0.023(3) 0.016(3) 0.013(2) C13 0.054(2) 0.049(3) 0.083(3) -0.004(2) 0.015(2) 0.007(2) C14 0.0370(16) 0.0372(17) 0.0334(15) 0.0030(13) -0.0006(12) 0.0062(13) C15 0.045(2) 0.107(4) 0.043(2) -0.013(2) -0.0088(16) 0.000(2) C16 0.067(3) 0.139(6) 0.038(2) -0.022(3) -0.007(2) 0.010(4) C17 0.077(3) 0.094(4) 0.039(2) 0.008(2) 0.0150(19) 0.017(3) C18 0.064(3) 0.090(4) 0.065(3) -0.007(3) 0.022(2) -0.018(3) C19 0.053(2) 0.067(3) 0.050(2) -0.0131(19) 0.0087(17) -0.0166(19) Cl1 0.0314(4) 0.0512(6) 0.0766(6) 0.0092(4) -0.0045(4) 0.0077(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 As2 C1 1.916(3) . ? As2 C8 1.927(3) . ? As2 C14 1.926(3) . ? Au1 As2 2.4618(4) . ? Au1 Au1 2.5526(3) 2_565 ? Au1 C6 2.070(3) 2_565 ? Au1 Cl1 2.3592(9) . ? C1 C6 1.408(5) . ? C2 C1 1.381(5) . ? C2 C3 1.387(5) . ? C3 C4 1.385(5) . ? C4 C7 1.511(5) . ? C5 C4 1.399(5) . ? C6 Au1 2.070(3) 2_565 ? C6 C5 1.383(4) . ? C8 C9 1.369(6) . ? C8 C13 1.376(5) . ? C9 C10 1.390(6) . ? C11 C10 1.357(9) . ? C12 C11 1.372(9) . ? C13 C12 1.384(7) . ? C14 C15 1.374(5) . ? C14 C19 1.374(5) . ? C15 C16 1.383(6) . ? C17 C16 1.351(7) . ? C17 C18 1.370(7) . ? C19 C18 1.390(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag As2 Au1 Au1 79.401(10) . 2_565 ? C1 As2 Au1 98.18(10) . . ? C1 As2 C8 108.10(14) . . ? C1 As2 C14 104.24(13) . . ? C1 C2 C3 119.8(3) . . ? C1 C6 Au1 120.0(2) . 2_565 ? C2 C1 As2 125.7(3) . . ? C2 C1 C6 121.0(3) . . ? C3 C4 C5 118.8(3) . . ? C3 C4 C7 120.6(3) . . ? C4 C3 C2 120.6(3) . . ? C5 C4 C7 120.6(3) . . ? C5 C6 Au1 122.1(2) . 2_565 ? C5 C6 C1 117.9(3) . . ? C6 Au1 As2 168.21(8) 2_565 . ? C6 Au1 Au1 89.36(9) 2_565 2_565 ? C6 Au1 Cl1 93.05(9) 2_565 . ? C6 C1 As2 113.2(2) . . ? C6 C5 C4 121.8(3) . . ? C8 As2 Au1 122.02(11) . . ? C8 C9 C10 120.2(5) . . ? C8 C13 C12 119.6(5) . . ? C9 C8 As2 121.0(3) . . ? C9 C8 C13 120.0(4) . . ? C10 C11 C12 120.8(4) . . ? C11 C10 C9 119.5(5) . . ? C11 C12 C13 119.8(5) . . ? C13 C8 As2 118.9(3) . . ? C14 As2 Au1 117.59(10) . . ? C14 As2 C8 104.78(14) . . ? C14 C15 C16 119.6(4) . . ? C14 C19 C18 119.9(4) . . ? C15 C14 As2 120.4(3) . . ? C16 C17 C18 119.5(4) . . ? C17 C16 C15 121.3(4) . . ? C17 C18 C19 120.1(4) . . ? C19 C14 As2 120.0(2) . . ? C19 C14 C15 119.5(3) . . ? Cl1 Au1 As2 98.16(3) . . ? Cl1 Au1 Au1 177.52(3) . 2_565 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.114 _refine_diff_density_min -0.681 _refine_diff_density_rms 0.123 #===END data_compound2b _database_code_depnum_ccdc_archive 'CCDC 290382' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H32 As2 Au2 Br2' _chemical_formula_weight 1192.23 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 17.6413(12) _cell_length_b 12.2384(8) _cell_length_c 16.7360(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3613.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.192 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2216 _exptl_absorpt_coefficient_mu 12.166 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS Sheldrick 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25520 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 28.29 _reflns_number_total 4496 _reflns_number_gt 3689 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+0.3917P] 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 4496 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0665 _refine_ls_wR_factor_gt 0.0622 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As2 As 0.26933(2) 0.55748(3) 0.15331(2) 0.03077(9) Uani 1 1 d . . . Au1 Au 0.321180(7) 0.728671(11) 0.098670(8) 0.02875(6) Uani 1 1 d . . . Br1 Br 0.45779(2) 0.68023(4) 0.10531(3) 0.05186(12) Uani 1 1 d . . . C1 C 0.1957(2) 0.5283(3) 0.0718(2) 0.0323(8) Uani 1 1 d . . . C2 C 0.1822(2) 0.4271(3) 0.0382(2) 0.0412(9) Uani 1 1 d . . . C3 C 0.1308(2) 0.4179(3) -0.0244(2) 0.0457(10) Uani 1 1 d . . . C4 C 0.0933(2) 0.5089(3) -0.0536(2) 0.0397(9) Uani 1 1 d . . . C5 C 0.1074(2) 0.6104(3) -0.0182(2) 0.0369(8) Uani 1 1 d . . . C6 C 0.15803(19) 0.6221(3) 0.0447(2) 0.0302(7) Uani 1 1 d . . . C7 C 0.0379(3) 0.5002(4) -0.1219(3) 0.0573(13) Uani 1 1 d . . . C8 C 0.3306(2) 0.4280(3) 0.1672(3) 0.0377(9) Uani 1 1 d . . . C9 C 0.3270(3) 0.3684(4) 0.2363(3) 0.0593(13) Uani 1 1 d . . . C10 C 0.3737(4) 0.2777(4) 0.2460(4) 0.0827(19) Uani 1 1 d . . . C11 C 0.4227(3) 0.2496(4) 0.1880(5) 0.0811(19) Uani 1 1 d . . . C12 C 0.4255(3) 0.3077(5) 0.1173(4) 0.0738(17) Uani 1 1 d . . . C13 C 0.3800(3) 0.3978(4) 0.1074(3) 0.0552(12) Uani 1 1 d . . . C14 C 0.2105(2) 0.5685(3) 0.2496(2) 0.0348(8) Uani 1 1 d . . . C15 C 0.2425(3) 0.6071(5) 0.3187(3) 0.0652(15) Uani 1 1 d . . . C16 C 0.1994(4) 0.6130(6) 0.3875(3) 0.083(2) Uani 1 1 d . . . C17 C 0.1261(3) 0.5822(5) 0.3891(3) 0.0672(15) Uani 1 1 d . . . C18 C 0.0936(3) 0.5440(4) 0.3195(3) 0.0678(15) Uani 1 1 d . . . C19 C 0.1358(2) 0.5372(4) 0.2509(3) 0.0554(12) Uani 1 1 d . . . H2 H 0.2074 0.3656 0.0573 0.049 Uiso 1 1 calc R . . H3 H 0.1215 0.3498 -0.0469 0.055 Uiso 1 1 calc R . . H5 H 0.0822 0.6717 -0.0374 0.044 Uiso 1 1 calc R . . H7A H 0.0291 0.4246 -0.1340 0.086 Uiso 1 1 calc R . . H7B H 0.0585 0.5362 -0.1681 0.086 Uiso 1 1 calc R . . H7C H -0.0090 0.5344 -0.1071 0.086 Uiso 1 1 calc R . . H9 H 0.2936 0.3884 0.2767 0.071 Uiso 1 1 calc R . . H10 H 0.3711 0.2365 0.2926 0.099 Uiso 1 1 calc R . . H11 H 0.4550 0.1905 0.1955 0.097 Uiso 1 1 calc R . . H12 H 0.4581 0.2861 0.0766 0.089 Uiso 1 1 calc R . . H13 H 0.3824 0.4382 0.0604 0.066 Uiso 1 1 calc R . . H15 H 0.2930 0.6292 0.3192 0.078 Uiso 1 1 calc R . . H16 H 0.2217 0.6390 0.4342 0.099 Uiso 1 1 calc R . . H17 H 0.0981 0.5867 0.4360 0.081 Uiso 1 1 calc R . . H18 H 0.0430 0.5228 0.3192 0.081 Uiso 1 1 calc R . . H19 H 0.1135 0.5109 0.2044 0.067 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As2 0.03091(19) 0.02884(18) 0.0326(2) 0.00164(15) -0.00217(15) 0.00206(14) Au1 0.02552(9) 0.02890(10) 0.03182(9) 0.00115(5) -0.00095(5) 0.00208(5) Br1 0.0291(2) 0.0502(3) 0.0763(3) 0.0105(2) -0.00682(19) 0.00546(18) C1 0.0292(17) 0.038(2) 0.0295(17) -0.0013(16) 0.0005(14) 0.0002(15) C2 0.042(2) 0.035(2) 0.046(2) 0.0002(18) -0.0027(17) 0.0028(16) C3 0.051(2) 0.037(2) 0.048(2) -0.0105(18) -0.0056(19) -0.0032(18) C4 0.0320(19) 0.047(2) 0.040(2) -0.0056(18) -0.0012(16) -0.0032(16) C5 0.034(2) 0.038(2) 0.038(2) -0.0027(16) -0.0032(15) 0.0024(15) C6 0.0272(16) 0.0308(19) 0.0327(18) -0.0010(14) 0.0010(14) -0.0008(14) C7 0.052(3) 0.065(3) 0.054(3) -0.016(2) -0.016(2) -0.001(2) C8 0.033(2) 0.0268(19) 0.054(2) -0.0020(17) -0.0071(17) 0.0044(14) C9 0.074(3) 0.047(3) 0.057(3) 0.004(2) -0.006(2) 0.018(2) C10 0.115(5) 0.052(3) 0.081(4) 0.005(3) -0.016(4) 0.035(3) C11 0.077(4) 0.045(3) 0.120(5) -0.016(3) -0.029(4) 0.028(3) C12 0.054(3) 0.055(3) 0.112(5) -0.022(3) 0.011(3) 0.011(3) C13 0.050(3) 0.046(3) 0.070(3) -0.001(2) 0.010(2) 0.002(2) C14 0.0348(19) 0.036(2) 0.0332(19) 0.0019(15) -0.0019(16) 0.0069(15) C15 0.040(3) 0.115(5) 0.041(3) -0.013(3) -0.0081(19) 0.001(3) C16 0.069(4) 0.145(7) 0.034(3) -0.021(3) -0.011(3) 0.014(4) C17 0.077(4) 0.085(4) 0.039(3) 0.006(2) 0.016(2) 0.015(3) C18 0.055(3) 0.081(4) 0.067(3) -0.009(3) 0.023(3) -0.014(3) C19 0.050(3) 0.071(3) 0.046(2) -0.015(2) 0.010(2) -0.019(2) _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 As2 C1 1.917(4) . ? As2 C8 1.931(4) . ? As2 C14 1.922(4) . ? Au1 As2 2.4622(4) . ? Au1 Au1 2.5651(3) 2_565 ? Au1 Br1 2.4842(4) . ? Au1 C6 2.071(3) 2_565 ? C1 C6 1.402(5) . ? C2 C1 1.381(5) . ? C2 C3 1.390(5) . ? C3 C4 1.384(6) . ? C4 C5 1.398(5) . ? C4 C7 1.508(6) . ? C6 Au1 2.071(3) 2_565 ? C6 C5 1.387(5) . ? C8 C9 1.369(6) . ? C8 C13 1.379(6) . ? C9 C10 1.392(6) . ? C10 C11 1.345(9) . ? C12 C11 1.380(9) . ? C13 C12 1.374(8) . ? C14 C15 1.370(6) . ? C14 C19 1.372(6) . ? C15 C16 1.383(7) . ? C17 C16 1.346(8) . ? C18 C17 1.380(8) . ? C19 C18 1.372(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag As2 Au1 Au1 79.016(11) . 2_565 ? As2 Au1 Br1 98.089(15) . . ? Br1 Au1 Au1 176.701(12) . 2_565 ? C1 As2 Au1 98.38(12) . . ? C1 As2 C8 108.18(16) . . ? C1 As2 C14 104.13(15) . . ? C1 C2 C3 119.4(4) . . ? C1 C6 Au1 119.8(3) . 2_565 ? C2 C1 As2 125.0(3) . . ? C2 C1 C6 121.4(3) . . ? C3 C4 C5 118.6(4) . . ? C3 C4 C7 121.4(4) . . ? C4 C3 C2 120.9(4) . . ? C5 C4 C7 119.9(4) . . ? C5 C6 Au1 122.4(3) . 2_565 ? C5 C6 C1 117.8(3) . . ? C6 Au1 As2 168.10(9) 2_565 . ? C6 Au1 Au1 89.65(10) 2_565 2_565 ? C6 Au1 Br1 93.34(10) 2_565 . ? C6 C1 As2 113.6(3) . . ? C6 C5 C4 121.8(4) . . ? C8 As2 Au1 122.34(12) . . ? C8 C9 C10 119.8(5) . . ? C9 C8 As2 120.9(3) . . ? C9 C8 C13 119.9(4) . . ? C10 C11 C12 120.7(5) . . ? C11 C10 C9 120.0(6) . . ? C12 C13 C8 119.8(5) . . ? C13 C8 As2 119.1(3) . . ? C13 C12 C11 119.7(5) . . ? C14 As2 Au1 116.89(12) . . ? C14 As2 C8 104.98(17) . . ? C14 C15 C16 119.6(4) . . ? C14 C19 C18 121.1(4) . . ? C15 C14 As2 120.6(3) . . ? C15 C14 C19 118.6(4) . . ? C16 C17 C18 118.5(4) . . ? C17 C16 C15 122.0(5) . . ? C19 C14 As2 120.8(3) . . ? C19 C18 C17 120.1(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.183 _refine_diff_density_min -0.820 _refine_diff_density_rms 0.137 #===END data_compound2c _database_code_depnum_ccdc_archive 'CCDC 290383' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H32 As2 Au2 I2' _chemical_formula_weight 1286.21 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 17.8668(12) _cell_length_b 12.4610(9) _cell_length_c 16.7927(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3738.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.087 _exptl_crystal_size_min 0.065 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2360 _exptl_absorpt_coefficient_mu 11.272 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS Sheldrick 1996' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26626 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 28.32 _reflns_number_total 4667 _reflns_number_gt 3842 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+2.0865P] 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 4667 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0707 _refine_ls_wR_factor_gt 0.0664 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 As1 As 0.26737(2) 0.56093(4) 0.15010(3) 0.03370(11) Uani 1 1 d . . . Au1 Au 0.320780(8) 0.727990(14) 0.096290(10) 0.03166(6) Uani 1 1 d . . . C1 C 0.1941(2) 0.5333(4) 0.0687(3) 0.0363(10) Uani 1 1 d . . . C2 C 0.1812(3) 0.4343(4) 0.0347(3) 0.0454(12) Uani 1 1 d . . . C3 C 0.1306(3) 0.4264(4) -0.0271(3) 0.0482(12) Uani 1 1 d . . . C4 C 0.0935(3) 0.5158(4) -0.0561(3) 0.0435(11) Uani 1 1 d . . . C5 C 0.1074(2) 0.6152(4) -0.0207(3) 0.0401(10) Uani 1 1 d . . . C6 C 0.1574(2) 0.6259(4) 0.0422(3) 0.0335(9) Uani 1 1 d . . . C7 C 0.0392(3) 0.5082(5) -0.1256(4) 0.0621(16) Uani 1 1 d . . . C8 C 0.3252(2) 0.4324(4) 0.1636(3) 0.0410(11) Uani 1 1 d . . . C9 C 0.3206(3) 0.3721(5) 0.2327(4) 0.0613(15) Uani 1 1 d . . . C10 C 0.3632(4) 0.2808(5) 0.2415(5) 0.081(2) Uani 1 1 d . . . C11 C 0.4096(4) 0.2490(5) 0.1833(5) 0.080(2) Uani 1 1 d . . . C12 C 0.4158(4) 0.3079(6) 0.1128(5) 0.076(2) Uani 1 1 d . . . C13 C 0.3736(3) 0.3993(5) 0.1041(4) 0.0582(15) Uani 1 1 d . . . C14 C 0.2098(2) 0.5740(4) 0.2463(3) 0.0364(10) Uani 1 1 d . . . C15 C 0.2423(3) 0.6088(6) 0.3159(4) 0.0659(17) Uani 1 1 d . . . C16 C 0.2003(4) 0.6171(7) 0.3843(4) 0.086(2) Uani 1 1 d . . . C17 C 0.1267(4) 0.5931(6) 0.3843(4) 0.0706(19) Uani 1 1 d . . . C18 C 0.0934(3) 0.5597(5) 0.3157(4) 0.0675(17) Uani 1 1 d . . . C19 C 0.1344(3) 0.5502(4) 0.2473(3) 0.0530(13) Uani 1 1 d . . . H2 H 0.2062 0.3737 0.0532 0.054 Uiso 1 1 calc R . . H3 H 0.1212 0.3596 -0.0498 0.058 Uiso 1 1 calc R . . H5 H 0.0827 0.6757 -0.0397 0.048 Uiso 1 1 calc R . . H7A H 0.0586 0.5479 -0.1700 0.093 Uiso 1 1 calc R . . H7B H -0.0083 0.5374 -0.1102 0.093 Uiso 1 1 calc R . . H7C H 0.0331 0.4343 -0.1405 0.093 Uiso 1 1 calc R . . H9 H 0.2885 0.3934 0.2734 0.074 Uiso 1 1 calc R . . H10 H 0.3598 0.2408 0.2881 0.097 Uiso 1 1 calc R . . H11 H 0.4380 0.1871 0.1900 0.096 Uiso 1 1 calc R . . H12 H 0.4479 0.2855 0.0724 0.091 Uiso 1 1 calc R . . H13 H 0.3776 0.4394 0.0576 0.070 Uiso 1 1 calc R . . H15 H 0.2928 0.6268 0.3167 0.079 Uiso 1 1 calc R . . H16 H 0.2230 0.6396 0.4313 0.103 Uiso 1 1 calc R . . H17 H 0.0989 0.5993 0.4309 0.085 Uiso 1 1 calc R . . H18 H 0.0426 0.5432 0.3154 0.081 Uiso 1 1 calc R . . H19 H 0.1111 0.5274 0.2007 0.064 Uiso 1 1 calc R . . I1 I 0.464255(17) 0.67786(3) 0.11221(2) 0.05716(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.0339(2) 0.0349(2) 0.0323(2) 0.00168(18) -0.00242(17) 0.00026(18) Au1 0.02921(9) 0.03492(11) 0.03084(10) 0.00150(6) -0.00094(6) 0.00036(7) C1 0.035(2) 0.042(3) 0.031(2) -0.0030(19) -0.0052(18) -0.0020(19) C2 0.048(3) 0.040(3) 0.048(3) -0.002(2) -0.007(2) 0.001(2) C3 0.055(3) 0.043(3) 0.047(3) -0.011(2) -0.004(2) -0.005(2) C4 0.039(2) 0.052(3) 0.039(3) -0.008(2) -0.003(2) -0.002(2) C5 0.039(2) 0.043(3) 0.038(3) -0.002(2) -0.0016(19) 0.007(2) C6 0.033(2) 0.036(2) 0.032(2) -0.0024(18) 0.0033(17) -0.0040(18) C7 0.059(3) 0.066(4) 0.062(4) -0.019(3) -0.024(3) -0.001(3) C8 0.034(2) 0.035(2) 0.054(3) -0.001(2) -0.007(2) 0.0024(19) C9 0.072(4) 0.050(3) 0.062(4) 0.011(3) -0.002(3) 0.015(3) C10 0.097(5) 0.065(5) 0.079(5) 0.013(4) -0.012(4) 0.029(4) C11 0.075(4) 0.051(4) 0.114(7) -0.011(4) -0.018(4) 0.023(3) C12 0.057(4) 0.064(4) 0.107(6) -0.028(4) 0.013(3) 0.006(3) C13 0.053(3) 0.052(3) 0.070(4) -0.004(3) 0.007(3) 0.004(3) C14 0.042(2) 0.038(2) 0.029(2) 0.0063(18) -0.0007(18) 0.0000(19) C15 0.048(3) 0.110(5) 0.040(3) -0.014(3) -0.011(2) 0.005(3) C16 0.078(5) 0.145(8) 0.034(3) -0.019(4) -0.011(3) 0.016(5) C17 0.082(5) 0.089(5) 0.041(4) 0.004(3) 0.024(3) 0.011(4) C18 0.065(4) 0.080(5) 0.057(4) -0.007(3) 0.023(3) -0.018(3) C19 0.053(3) 0.062(4) 0.044(3) -0.010(2) 0.004(2) -0.019(3) I1 0.03326(16) 0.0613(3) 0.0769(3) 0.01411(18) -0.00976(15) 0.00213(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 As1 C1 1.923(4) . ? As1 C8 1.920(4) . ? As1 C14 1.922(4) . ? Au1 As1 2.4619(5) . ? Au1 Au1 2.5880(3) 2_565 ? Au1 C6 2.072(4) 2_565 ? Au1 I1 2.6520(4) . ? C1 C2 1.379(7) . ? C1 C6 1.400(6) . ? C2 C3 1.380(7) . ? C3 C4 1.385(7) . ? C4 C7 1.520(7) . ? C5 C4 1.396(7) . ? C6 Au1 2.072(4) 2_565 ? C6 C5 1.389(6) . ? C8 C9 1.385(8) . ? C8 C13 1.384(7) . ? C9 C10 1.378(8) . ? C10 C11 1.341(10) . ? C12 C11 1.398(11) . ? C13 C12 1.373(9) . ? C14 C15 1.376(7) . ? C14 C19 1.379(7) . ? C15 C16 1.376(9) . ? C17 C16 1.348(9) . ? C18 C17 1.361(9) . ? C19 C18 1.369(7) . ? 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 As1 Au1 Au1 78.486(13) . 2_565 ? As1 Au1 I1 97.961(15) . . ? Au1 Au1 I1 174.034(10) 2_565 . ? C1 As1 Au1 98.89(14) . . ? C1 C2 C3 119.1(5) . . ? C1 C6 Au1 119.7(3) . 2_565 ? C2 C1 As1 124.7(4) . . ? C2 C1 C6 121.8(4) . . ? C2 C3 C4 121.3(5) . . ? C3 C4 C5 118.6(4) . . ? C3 C4 C7 121.6(5) . . ? C5 C4 C7 119.7(5) . . ? C5 C6 Au1 122.5(3) . 2_565 ? C5 C6 C1 117.7(4) . . ? C6 Au1 As1 167.68(12) 2_565 . ? C6 Au1 Au1 89.86(12) 2_565 2_565 ? C6 Au1 I1 93.98(12) 2_565 . ? C6 C1 As1 113.4(3) . . ? C6 C5 C4 121.5(4) . . ? C8 As1 Au1 122.70(14) . . ? C8 As1 C1 107.5(2) . . ? C8 As1 C14 105.1(2) . . ? C9 C8 As1 121.3(4) . . ? C10 C9 C8 120.3(6) . . ? C10 C11 C12 120.8(6) . . ? C11 C10 C9 120.5(7) . . ? C12 C13 C8 120.9(6) . . ? C13 C8 As1 120.0(4) . . ? C13 C8 C9 118.7(5) . . ? C13 C12 C11 118.8(6) . . ? C14 As1 Au1 116.37(14) . . ? C14 As1 C1 104.34(19) . . ? C14 C15 C16 120.2(5) . . ? C15 C14 As1 121.0(4) . . ? C15 C14 C19 118.0(5) . . ? C16 C17 C18 119.6(6) . . ? C17 C16 C15 121.0(6) . . ? C17 C18 C19 120.2(6) . . ? C18 C19 C14 121.0(5) . . ? C19 C14 As1 121.0(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.472 _refine_diff_density_min -0.749 _refine_diff_density_rms 0.149 #===END data_compound4 _database_code_depnum_ccdc_archive 'CCDC 290384' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H38 As2 Au2 O4' _chemical_formula_weight 1150.50 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' O O 0.0106 0.0060 '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 C2/c 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 18.9303(12) _cell_length_b 10.8309(7) _cell_length_c 19.5860(12) _cell_angle_alpha 90.00 _cell_angle_beta 103.1240(10) _cell_angle_gamma 90.00 _cell_volume 3910.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.954 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2184 _exptl_absorpt_coefficient_mu 9.213 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS Sheldrick 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14257 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 28.34 _reflns_number_total 4862 _reflns_number_gt 4398 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+11.0991P] 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 4862 _refine_ls_number_parameters 228 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0251 _refine_ls_R_factor_gt 0.0217 _refine_ls_wR_factor_ref 0.0551 _refine_ls_wR_factor_gt 0.0532 _refine_ls_goodness_of_fit_ref 0.869 _refine_ls_restrained_S_all 0.869 _refine_ls_shift/su_max 0.077 _refine_ls_shift/su_mean 0.004 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 As1 As 0.574595(17) 0.22638(3) 0.375321(16) 0.02732(7) Uani 1 1 d . . . Au1 Au 0.462292(6) 0.292131(9) 0.295703(5) 0.02311(4) Uani 1 1 d . . . C1 C 0.64287(17) 0.3336(3) 0.34598(17) 0.0318(6) Uani 1 1 d . . . C2 C 0.7039(2) 0.3843(4) 0.39088(19) 0.0450(9) Uani 1 1 d . . . C3 C 0.74544(19) 0.4695(4) 0.3654(2) 0.0452(9) Uani 1 1 d . . . C4 C 0.72910(19) 0.5032(3) 0.29596(19) 0.0391(7) Uani 1 1 d . . . C5 C 0.66954(17) 0.4487(3) 0.25102(17) 0.0323(7) Uani 1 1 d . . . C6 C 0.62527(15) 0.3642(3) 0.27524(16) 0.0267(6) Uani 1 1 d . . . C7 C 0.7739(2) 0.5989(4) 0.2686(2) 0.0551(11) Uani 1 1 d . . . C8 C 0.58235(18) 0.2593(3) 0.47361(17) 0.0310(6) Uani 1 1 d . . . C9 C 0.5847(2) 0.1638(3) 0.52125(18) 0.0388(8) Uani 1 1 d . . . C10 C 0.5874(3) 0.1909(4) 0.5909(2) 0.0480(10) Uani 1 1 d . . . C11 C 0.5865(3) 0.3111(4) 0.6126(2) 0.0540(11) Uani 1 1 d . . . C12 C 0.5827(3) 0.4055(4) 0.5649(2) 0.0579(11) Uani 1 1 d . . . C13 C 0.5805(2) 0.3806(3) 0.4954(2) 0.0475(9) Uani 1 1 d . . . C14 C 0.6098(2) 0.0611(3) 0.36964(17) 0.0364(7) Uani 1 1 d . . . C15 C 0.6831(2) 0.0354(5) 0.3935(3) 0.0608(12) Uani 1 1 d . . . C16 C 0.7080(4) -0.0834(6) 0.3844(3) 0.086(2) Uani 1 1 d . . . C17 C 0.6612(5) -0.1730(6) 0.3535(4) 0.091(2) Uani 1 1 d . . . C18 C 0.5892(4) -0.1476(5) 0.3307(3) 0.0837(18) Uani 1 1 d . . . C19 C 0.5633(3) -0.0298(4) 0.3382(2) 0.0553(11) Uani 1 1 d . . . C20 C 0.40873(19) 0.2058(3) 0.41476(18) 0.0327(7) Uani 1 1 d . . . C21 C 0.3816(3) 0.2235(4) 0.4808(2) 0.0563(11) Uani 1 1 d . . . H2 H 0.7164 0.3607 0.4377 0.054 Uiso 1 1 calc R . . H3 H 0.7853 0.5048 0.3957 0.054 Uiso 1 1 calc R . . H5 H 0.6590 0.4693 0.2037 0.039 Uiso 1 1 calc R . . H7A H 0.7817 0.6687 0.2996 0.083 Uiso 1 1 calc R . . H7B H 0.7485 0.6251 0.2227 0.083 Uiso 1 1 calc R . . H7C H 0.8197 0.5638 0.2660 0.083 Uiso 1 1 calc R . . H9 H 0.5846 0.0822 0.5065 0.047 Uiso 1 1 calc R . . H10 H 0.5898 0.1271 0.6232 0.058 Uiso 1 1 calc R . . H11 H 0.5884 0.3288 0.6595 0.065 Uiso 1 1 calc R . . H12 H 0.5816 0.4869 0.5796 0.069 Uiso 1 1 calc R . . H13 H 0.5779 0.4448 0.4634 0.057 Uiso 1 1 calc R . . H15 H 0.7151 0.0963 0.4152 0.073 Uiso 1 1 calc R . . H16 H 0.7571 -0.1015 0.3997 0.103 Uiso 1 1 calc R . . H17 H 0.6784 -0.2520 0.3480 0.109 Uiso 1 1 calc R . . H18 H 0.5574 -0.2094 0.3101 0.100 Uiso 1 1 calc R . . H19 H 0.5143 -0.0125 0.3219 0.066 Uiso 1 1 calc R . . H21A H 0.3296 0.2174 0.4699 0.084 Uiso 1 1 calc R . . H21B H 0.3959 0.3034 0.5002 0.084 Uiso 1 1 calc R . . H21C H 0.4018 0.1608 0.5142 0.084 Uiso 1 1 calc R . . O1 O 0.40515(14) 0.3041(2) 0.37663(12) 0.0333(5) Uani 1 1 d . . . O2 O 0.43230(16) 0.1069(2) 0.40126(15) 0.0474(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.02875(16) 0.02730(15) 0.02242(15) 0.00463(11) -0.00151(12) 0.00224(12) Au1 0.02487(7) 0.02196(7) 0.01976(6) 0.00089(4) -0.00063(4) 0.00067(4) C1 0.0264(15) 0.0363(16) 0.0288(16) 0.0045(13) -0.0019(12) -0.0003(13) C2 0.0374(19) 0.061(2) 0.0287(18) 0.0049(16) -0.0079(14) -0.0089(18) C3 0.0320(18) 0.058(2) 0.039(2) -0.0034(17) -0.0056(14) -0.0178(17) C4 0.0316(17) 0.0427(19) 0.042(2) -0.0072(15) 0.0054(14) -0.0088(15) C5 0.0333(16) 0.0366(17) 0.0254(15) 0.0001(12) 0.0029(12) -0.0043(13) C6 0.0202(13) 0.0299(14) 0.0272(15) -0.0018(11) -0.0009(11) -0.0012(11) C7 0.050(2) 0.066(3) 0.050(2) -0.008(2) 0.0131(18) -0.029(2) C8 0.0352(17) 0.0293(15) 0.0249(15) 0.0017(12) -0.0010(12) 0.0021(13) C9 0.053(2) 0.0294(16) 0.0306(18) 0.0014(13) 0.0029(15) 0.0042(15) C10 0.068(3) 0.045(2) 0.0285(19) 0.0068(15) 0.0060(17) 0.0021(19) C11 0.076(3) 0.054(2) 0.030(2) -0.0085(17) 0.0069(19) -0.003(2) C12 0.085(3) 0.036(2) 0.049(2) -0.0110(17) 0.009(2) -0.001(2) C13 0.069(3) 0.0315(18) 0.038(2) 0.0018(14) 0.0044(18) -0.0013(17) C14 0.048(2) 0.0339(17) 0.0295(17) 0.0073(13) 0.0142(14) 0.0131(15) C15 0.050(2) 0.064(3) 0.068(3) 0.024(2) 0.012(2) 0.022(2) C16 0.085(4) 0.085(4) 0.101(5) 0.045(4) 0.049(4) 0.058(3) C17 0.148(7) 0.051(3) 0.094(5) 0.020(3) 0.071(5) 0.049(4) C18 0.134(6) 0.041(3) 0.083(4) -0.012(2) 0.039(4) 0.015(3) C19 0.074(3) 0.039(2) 0.053(3) -0.0042(18) 0.015(2) 0.008(2) C20 0.0329(17) 0.0336(17) 0.0288(16) 0.0032(12) 0.0013(13) -0.0064(13) C21 0.071(3) 0.062(3) 0.042(2) 0.0108(19) 0.026(2) 0.009(2) O1 0.0449(14) 0.0310(12) 0.0219(11) 0.0024(8) 0.0033(10) 0.0061(10) O2 0.0637(18) 0.0289(12) 0.0504(16) 0.0051(11) 0.0149(13) 0.0003(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 As1 C1 1.920(3) . ? As1 C8 1.930(3) . ? As1 C14 1.922(3) . ? Au1 As1 2.4399(3) . ? Au1 Au1 2.5306(2) 2_655 ? Au1 C6 2.059(3) 2_655 ? Au1 O1 2.116(2) . ? C1 C2 1.395(5) . ? C1 C6 1.390(4) . ? C2 C3 1.378(5) . ? C3 C4 1.373(5) . ? C4 C7 1.513(5) . ? C5 C4 1.394(5) . ? C6 Au1 2.059(3) 2_655 ? C6 C5 1.395(4) . ? C8 C9 1.387(5) . ? C8 C13 1.383(5) . ? C9 C10 1.385(5) . ? C10 C11 1.371(5) . ? C11 C12 1.377(6) . ? C13 C12 1.379(6) . ? C14 C15 1.389(6) . ? C14 C19 1.369(6) . ? C16 C15 1.395(7) . ? C16 C17 1.360(10) . ? C18 C17 1.361(10) . ? C18 C19 1.386(6) . ? C20 C21 1.508(5) . ? O1 C20 1.294(4) . ? O2 C20 1.212(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag As1 Au1 Au1 84.405(10) . 2_655 ? C1 As1 Au1 100.39(9) . . ? C1 As1 C8 106.42(14) . . ? C1 As1 C14 106.26(14) . . ? C1 C6 Au1 123.8(2) . 2_655 ? C1 C6 C5 118.0(3) . . ? C2 C1 As1 124.5(3) . . ? C3 C2 C1 119.6(3) . . ? C3 C4 C5 118.7(3) . . ? C3 C4 C7 121.0(3) . . ? C4 C3 C2 121.2(3) . . ? C5 C4 C7 120.3(3) . . ? C5 C6 Au1 118.2(2) . 2_655 ? C6 Au1 As1 173.13(8) 2_655 . ? C6 Au1 Au1 91.12(8) 2_655 2_655 ? C6 Au1 O1 90.69(11) 2_655 . ? C6 C1 As1 114.7(2) . . ? C6 C1 C2 120.7(3) . . ? C6 C5 C4 121.7(3) . . ? C8 As1 Au1 116.19(10) . . ? C8 C9 C10 119.5(3) . . ? C8 C13 C12 119.5(3) . . ? C9 C8 As1 121.1(3) . . ? C10 C11 C12 119.8(4) . . ? C11 C10 C9 120.4(4) . . ? C11 C12 C13 120.7(4) . . ? C13 C8 As1 118.8(3) . . ? C13 C8 C9 120.0(3) . . ? C14 As1 Au1 119.87(11) . . ? C14 As1 C8 106.33(14) . . ? C14 C15 C16 118.8(5) . . ? C14 C19 C18 120.2(5) . . ? C15 C14 As1 120.0(3) . . ? C17 C16 C15 120.7(5) . . ? C17 C18 C19 120.2(6) . . ? C18 C17 C16 120.2(5) . . ? C19 C14 As1 120.0(3) . . ? C19 C14 C15 119.9(4) . . ? C20 O1 Au1 114.4(2) . . ? O1 Au1 As1 93.36(7) . . ? O1 Au1 Au1 175.10(7) . 2_655 ? O1 C20 C21 114.0(3) . . ? O2 C20 C21 120.9(3) . . ? O2 C20 O1 125.1(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.241 _refine_diff_density_min -1.316 _refine_diff_density_rms 0.152 #===END data_compound5a _database_code_depnum_ccdc_archive 'CCDC 290385' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H32 As2 Au2 Cl2' _chemical_formula_weight 1103.31 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' 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 C2/c 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 19.1148(15) _cell_length_b 10.7477(8) _cell_length_c 18.6647(14) _cell_angle_alpha 90.00 _cell_angle_beta 112.638(2) _cell_angle_gamma 90.00 _cell_volume 3539.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.096 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.071 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2072 _exptl_absorpt_coefficient_mu 10.314 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS Sheldrick 1996' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12922 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 28.32 _reflns_number_total 4405 _reflns_number_gt 3802 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4405 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0288 _refine_ls_R_factor_gt 0.0233 _refine_ls_wR_factor_ref 0.0555 _refine_ls_wR_factor_gt 0.0536 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 As1 As 0.454429(18) 0.31932(3) 0.122868(17) 0.03400(8) Uani 1 1 d . . . Au1 Au 0.421287(7) 0.159163(11) 0.188853(6) 0.04050(5) Uani 1 1 d . . . C1 C 0.53756(16) 0.4304(3) 0.17978(16) 0.0326(6) Uani 1 1 d . . . C2 C 0.53360(16) 0.5077(2) 0.23880(15) 0.0322(6) Uani 1 1 d . . . C3 C 0.59413(19) 0.5873(3) 0.27616(17) 0.0406(7) Uani 1 1 d . . . C4 C 0.65889(19) 0.5899(3) 0.25973(18) 0.0440(7) Uani 1 1 d . . . C5 C 0.66175(19) 0.5120(3) 0.20271(19) 0.0454(7) Uani 1 1 d . . . C6 C 0.60152(19) 0.4342(3) 0.16221(18) 0.0442(7) Uani 1 1 d . . . C7 C 0.7231(2) 0.6762(3) 0.3029(3) 0.0679(11) Uani 1 1 d . . . C8 C 0.48392(18) 0.2472(3) 0.04375(16) 0.0375(6) Uani 1 1 d . . . C9 C 0.5439(2) 0.1637(3) 0.0667(2) 0.0485(8) Uani 1 1 d . . . C10 C 0.5650(2) 0.1095(4) 0.0104(3) 0.0628(10) Uani 1 1 d . . . C11 C 0.5275(3) 0.1358(4) -0.0663(3) 0.0667(12) Uani 1 1 d . . . C12 C 0.4674(3) 0.2159(4) -0.0889(2) 0.0630(11) Uani 1 1 d . . . C13 C 0.4455(2) 0.2726(3) -0.03449(18) 0.0487(8) Uani 1 1 d . . . C14 C 0.36988(18) 0.4235(3) 0.06450(17) 0.0378(6) Uani 1 1 d . . . C15 C 0.2975(2) 0.3824(3) 0.0515(2) 0.0498(8) Uani 1 1 d . . . C16 C 0.2355(2) 0.4504(4) 0.0039(3) 0.0652(11) Uani 1 1 d . . . C17 C 0.2455(2) 0.5604(4) -0.0273(2) 0.0598(10) Uani 1 1 d . . . C18 C 0.3167(2) 0.6042(3) -0.0125(2) 0.0571(9) Uani 1 1 d . . . C19 C 0.3793(2) 0.5355(3) 0.03248(19) 0.0473(8) Uani 1 1 d . . . Cl1 Cl 0.37909(6) -0.00383(10) 0.23919(6) 0.0706(3) Uani 1 1 d . . . H3 H 0.5910 0.6412 0.3138 0.049 Uiso 1 1 calc R . . H5 H 0.7048 0.5113 0.1910 0.055 Uiso 1 1 calc R . . H6 H 0.6042 0.3839 0.1228 0.053 Uiso 1 1 calc R . . H7A H 0.7683 0.6486 0.2969 0.102 Uiso 1 1 calc R . . H7B H 0.7312 0.6764 0.3569 0.102 Uiso 1 1 calc R . . H7C H 0.7108 0.7588 0.2823 0.102 Uiso 1 1 calc R . . H9 H 0.5696 0.1443 0.1189 0.058 Uiso 1 1 calc R . . H10 H 0.6055 0.0541 0.0254 0.075 Uiso 1 1 calc R . . H11 H 0.5428 0.0995 -0.1031 0.080 Uiso 1 1 calc R . . H12 H 0.4410 0.2323 -0.1414 0.076 Uiso 1 1 calc R . . H13 H 0.4049 0.3278 -0.0503 0.058 Uiso 1 1 calc R . . H15 H 0.2905 0.3093 0.0746 0.060 Uiso 1 1 calc R . . H16 H 0.1868 0.4208 -0.0069 0.078 Uiso 1 1 calc R . . H17 H 0.2035 0.6059 -0.0587 0.072 Uiso 1 1 calc R . . H18 H 0.3231 0.6804 -0.0327 0.069 Uiso 1 1 calc R . . H19 H 0.4278 0.5644 0.0412 0.057 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 As1 0.03035(16) 0.03955(15) 0.03105(15) -0.00167(11) 0.01066(13) -0.00335(12) Au1 0.03735(8) 0.04660(8) 0.03441(8) 0.00169(5) 0.01035(6) -0.00758(5) C1 0.0267(15) 0.0377(14) 0.0321(14) -0.0003(11) 0.0100(12) -0.0026(12) C2 0.0330(16) 0.0350(14) 0.0275(13) 0.0035(11) 0.0106(12) 0.0020(12) C3 0.0448(19) 0.0397(15) 0.0353(16) -0.0030(12) 0.0131(14) -0.0047(14) C4 0.0388(19) 0.0441(17) 0.0438(17) 0.0003(13) 0.0102(15) -0.0072(14) C5 0.0314(17) 0.0528(18) 0.056(2) -0.0023(15) 0.0214(15) -0.0072(14) C6 0.0422(19) 0.0527(18) 0.0436(18) -0.0081(14) 0.0230(15) -0.0042(15) C7 0.050(3) 0.071(3) 0.077(3) -0.020(2) 0.019(2) -0.022(2) C8 0.0405(18) 0.0385(15) 0.0345(15) -0.0031(12) 0.0156(13) -0.0057(13) C9 0.047(2) 0.0521(19) 0.0455(19) -0.0045(14) 0.0163(16) 0.0007(16) C10 0.059(3) 0.061(2) 0.077(3) -0.013(2) 0.035(2) 0.005(2) C11 0.089(4) 0.064(2) 0.064(3) -0.020(2) 0.048(3) -0.012(2) C12 0.088(3) 0.063(2) 0.0406(19) -0.0072(17) 0.028(2) -0.007(2) C13 0.056(2) 0.0492(18) 0.0408(18) 0.0000(14) 0.0184(16) 0.0023(16) C14 0.0312(16) 0.0419(15) 0.0374(16) -0.0062(12) 0.0100(13) 0.0004(13) C15 0.0378(19) 0.0411(16) 0.065(2) -0.0062(16) 0.0141(17) -0.0019(15) C16 0.037(2) 0.061(2) 0.086(3) -0.019(2) 0.011(2) 0.0053(18) C17 0.051(2) 0.059(2) 0.061(2) -0.0019(18) 0.0114(19) 0.0162(19) C18 0.063(3) 0.056(2) 0.054(2) 0.0133(17) 0.0233(19) 0.0154(19) C19 0.044(2) 0.0513(18) 0.0455(18) 0.0053(15) 0.0166(16) 0.0014(15) Cl1 0.0724(7) 0.0716(6) 0.0605(6) 0.0168(5) 0.0175(5) -0.0255(5) _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 As1 C1 1.944(3) . ? As1 C8 1.934(3) . ? As1 C14 1.923(3) . ? Au1 As1 2.3413(3) . ? Au1 Au1 2.9963(3) 2_655 ? Au1 Cl1 2.2772(9) . ? C1 C6 1.383(4) . ? C2 C1 1.405(4) . ? C2 C2 1.496(5) 2_655 ? C2 C3 1.391(4) . ? C4 C3 1.385(4) . ? C4 C7 1.501(5) . ? C5 C4 1.372(4) . ? C5 C6 1.388(4) . ? C8 C9 1.388(5) . ? C8 C13 1.386(4) . ? C9 C10 1.390(5) . ? C10 C11 1.361(6) . ? C12 C11 1.366(6) . ? C13 C12 1.380(5) . ? C14 C15 1.381(5) . ? C14 C19 1.386(4) . ? C15 C16 1.385(5) . ? C17 C16 1.363(6) . ? C18 C17 1.364(6) . ? C19 C18 1.382(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag As1 Au1 Au1 90.286(10) . 2_655 ? C1 As1 Au1 119.60(8) . . ? C1 C2 C2 122.0(3) . 2_655 ? C1 C6 C5 120.8(3) . . ? C2 C1 As1 120.8(2) . . ? C3 C2 C1 118.1(3) . . ? C3 C2 C2 119.9(2) . 2_655 ? C3 C4 C7 120.6(3) . . ? C4 C3 C2 122.9(3) . . ? C4 C5 C6 121.2(3) . . ? C5 C4 C3 117.7(3) . . ? C5 C4 C7 121.7(3) . . ? C6 C1 As1 120.0(2) . . ? C6 C1 C2 119.2(3) . . ? C8 As1 Au1 108.93(9) . . ? C8 As1 C1 104.25(12) . . ? C8 C9 C10 118.9(3) . . ? C9 C8 As1 118.2(2) . . ? C10 C11 C12 119.7(3) . . ? C11 C10 C9 121.3(4) . . ? C11 C12 C13 120.5(4) . . ? C12 C13 C8 120.1(3) . . ? C13 C8 As1 122.3(2) . . ? C13 C8 C9 119.5(3) . . ? C14 As1 Au1 112.81(9) . . ? C14 As1 C1 106.49(13) . . ? C14 As1 C8 103.25(13) . . ? C14 C15 C16 119.7(3) . . ? C15 C14 As1 118.7(2) . . ? C15 C14 C19 119.3(3) . . ? C16 C17 C18 120.3(4) . . ? C17 C16 C15 120.4(4) . . ? C17 C18 C19 120.2(4) . . ? C18 C19 C14 120.0(3) . . ? C19 C14 As1 122.0(2) . . ? Cl1 Au1 As1 173.28(3) . . ? Cl1 Au1 Au1 95.57(3) . 2_655 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.843 _refine_diff_density_min -0.759 _refine_diff_density_rms 0.108 #===END data_compound5b _database_code_depnum_ccdc_archive 'CCDC 290386' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H32 As2 Au2 Br2' _chemical_formula_weight 1192.23 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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 19.2239(15) _cell_length_b 10.7877(9) _cell_length_c 18.8728(15) _cell_angle_alpha 90.00 _cell_angle_beta 112.499(2) _cell_angle_gamma 90.00 _cell_volume 3616.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.190 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2216 _exptl_absorpt_coefficient_mu 12.157 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS Sheldrick 1996' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13291 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 28.33 _reflns_number_total 4492 _reflns_number_gt 3672 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+0.2065P] 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 4492 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0666 _refine_ls_wR_factor_gt 0.0630 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.015 _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 As1 As 0.45394(2) 0.32241(3) 0.12233(2) 0.03384(10) Uani 1 1 d . . . Au1 Au 0.422762(8) 0.161134(15) 0.188315(9) 0.04002(7) Uani 1 1 d . . . Br1 Br 0.37995(3) -0.01246(5) 0.23948(3) 0.06600(15) Uani 1 1 d . . . C1 C 0.5364(2) 0.4330(3) 0.1789(2) 0.0335(8) Uani 1 1 d . . . C2 C 0.53369(19) 0.5075(3) 0.2386(2) 0.0305(7) Uani 1 1 d . . . C3 C 0.5935(2) 0.5840(4) 0.2768(2) 0.0409(9) Uani 1 1 d . . . C4 C 0.6582(2) 0.5863(4) 0.2598(2) 0.0416(9) Uani 1 1 d . . . C5 C 0.6600(2) 0.5127(4) 0.2014(3) 0.0447(10) Uani 1 1 d . . . C6 C 0.5998(2) 0.4371(4) 0.1609(2) 0.0430(10) Uani 1 1 d . . . C7 C 0.7243(3) 0.6694(4) 0.3052(3) 0.0639(14) Uani 1 1 d . . . C8 C 0.4838(2) 0.2530(4) 0.0437(2) 0.0376(9) Uani 1 1 d . . . C9 C 0.5425(3) 0.1670(4) 0.0664(3) 0.0513(11) Uani 1 1 d . . . C10 C 0.5644(3) 0.1144(5) 0.0112(4) 0.0644(14) Uani 1 1 d . . . C11 C 0.5267(3) 0.1403(5) -0.0650(3) 0.0672(15) Uani 1 1 d . . . C12 C 0.4677(3) 0.2227(5) -0.0871(3) 0.0620(13) Uani 1 1 d . . . C13 C 0.4457(3) 0.2782(4) -0.0332(3) 0.0505(11) Uani 1 1 d . . . C14 C 0.3690(2) 0.4257(4) 0.0646(2) 0.0370(9) Uani 1 1 d . . . C15 C 0.2978(2) 0.3829(4) 0.0522(3) 0.0521(12) Uani 1 1 d . . . C16 C 0.2356(3) 0.4497(5) 0.0061(4) 0.0664(15) Uani 1 1 d . . . C17 C 0.2447(3) 0.5594(5) -0.0259(3) 0.0656(14) Uani 1 1 d . . . C18 C 0.3153(3) 0.6036(5) -0.0116(3) 0.0563(12) Uani 1 1 d . . . C19 C 0.3781(3) 0.5363(4) 0.0327(3) 0.0498(11) Uani 1 1 d . . . H3 H 0.5909 0.6357 0.3151 0.049 Uiso 1 1 calc R . . H5 H 0.7022 0.5135 0.1888 0.054 Uiso 1 1 calc R . . H6 H 0.6018 0.3884 0.1211 0.052 Uiso 1 1 calc R . . H7A H 0.7339 0.6630 0.3589 0.096 Uiso 1 1 calc R . . H7B H 0.7125 0.7538 0.2889 0.096 Uiso 1 1 calc R . . H7C H 0.7682 0.6439 0.2966 0.096 Uiso 1 1 calc R . . H9 H 0.5666 0.1453 0.1178 0.062 Uiso 1 1 calc R . . H10 H 0.6053 0.0606 0.0261 0.077 Uiso 1 1 calc R . . H11 H 0.5410 0.1024 -0.1016 0.081 Uiso 1 1 calc R . . H12 H 0.4424 0.2411 -0.1388 0.074 Uiso 1 1 calc R . . H13 H 0.4052 0.3328 -0.0488 0.061 Uiso 1 1 calc R . . H15 H 0.2916 0.3093 0.0747 0.063 Uiso 1 1 calc R . . H16 H 0.1875 0.4200 -0.0032 0.080 Uiso 1 1 calc R . . H17 H 0.2028 0.6036 -0.0574 0.079 Uiso 1 1 calc R . . H18 H 0.3212 0.6797 -0.0318 0.068 Uiso 1 1 calc R . . H19 H 0.4261 0.5654 0.0408 0.060 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 As1 0.0309(2) 0.0395(2) 0.0290(2) -0.00123(16) 0.00909(16) -0.00305(15) Au1 0.03678(10) 0.04646(10) 0.03294(10) 0.00202(7) 0.00901(7) -0.00652(7) Br1 0.0660(3) 0.0670(3) 0.0575(3) 0.0154(3) 0.0153(3) -0.0213(3) C1 0.0304(19) 0.0372(19) 0.032(2) 0.0012(16) 0.0107(16) -0.0030(15) C2 0.0317(19) 0.0318(17) 0.0264(17) 0.0039(16) 0.0092(15) 0.0028(15) C3 0.050(2) 0.039(2) 0.031(2) -0.0016(18) 0.0138(19) -0.0006(18) C4 0.034(2) 0.040(2) 0.044(2) -0.0010(19) 0.0089(19) -0.0071(17) C5 0.034(2) 0.050(2) 0.053(3) -0.004(2) 0.020(2) -0.0078(18) C6 0.037(2) 0.053(2) 0.041(2) -0.009(2) 0.0166(19) -0.0045(18) C7 0.045(3) 0.065(3) 0.072(4) -0.016(3) 0.011(3) -0.020(2) C8 0.041(2) 0.0378(19) 0.033(2) -0.0022(17) 0.0124(18) -0.0028(17) C9 0.050(3) 0.054(3) 0.049(3) 0.001(2) 0.017(2) 0.007(2) C10 0.065(3) 0.059(3) 0.074(4) -0.009(3) 0.032(3) 0.010(3) C11 0.086(4) 0.066(3) 0.065(4) -0.023(3) 0.047(3) -0.011(3) C12 0.081(4) 0.066(3) 0.042(3) -0.006(3) 0.027(3) -0.004(3) C13 0.062(3) 0.051(3) 0.038(2) -0.002(2) 0.019(2) 0.004(2) C14 0.033(2) 0.041(2) 0.032(2) -0.0072(17) 0.0071(17) 0.0015(16) C15 0.038(2) 0.044(2) 0.066(3) -0.008(2) 0.011(2) -0.0016(19) C16 0.034(2) 0.061(3) 0.090(4) -0.011(3) 0.008(3) 0.002(2) C17 0.052(3) 0.073(3) 0.059(3) -0.003(3) 0.007(3) 0.026(3) C18 0.062(3) 0.054(3) 0.049(3) 0.011(2) 0.016(2) 0.014(2) C19 0.049(3) 0.055(3) 0.044(3) 0.004(2) 0.016(2) 0.004(2) _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 As1 C1 1.945(4) . ? As1 C8 1.934(4) . ? As1 C14 1.932(4) . ? Au1 As1 2.3469(4) . ? Au1 Au1 2.9913(4) 2_655 ? Au1 Br1 2.3927(5) . ? C1 C2 1.402(5) . ? C1 C6 1.384(5) . ? C2 C2 1.513(7) 2_655 ? C2 C3 1.374(5) . ? C3 C4 1.400(5) . ? C4 C7 1.523(6) . ? C5 C4 1.370(6) . ? C5 C6 1.383(6) . ? C8 C9 1.396(6) . ? C8 C13 1.380(6) . ? C9 C10 1.386(7) . ? C11 C10 1.369(8) . ? C12 C11 1.375(8) . ? C13 C12 1.378(6) . ? C14 C15 1.377(6) . ? C14 C19 1.377(6) . ? C15 C16 1.381(6) . ? C17 C16 1.370(8) . ? C18 C17 1.364(7) . ? C19 C18 1.382(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag As1 Au1 Au1 91.947(12) . 2_655 ? As1 Au1 Br1 172.507(17) . . ? Br1 Au1 Au1 94.486(14) . 2_655 ? C1 As1 Au1 118.95(11) . . ? C1 C2 C2 121.9(3) . 2_655 ? C2 C1 As1 121.3(3) . . ? C2 C3 C4 122.0(4) . . ? C3 C2 C1 119.0(3) . . ? C3 C2 C2 119.1(3) . 2_655 ? C3 C4 C7 120.3(4) . . ? C4 C5 C6 120.9(4) . . ? C5 C4 C3 118.2(4) . . ? C5 C4 C7 121.5(4) . . ? C5 C6 C1 120.7(4) . . ? C6 C1 As1 119.6(3) . . ? C6 C1 C2 119.1(3) . . ? C8 As1 Au1 109.32(12) . . ? C8 As1 C1 103.85(16) . . ? C9 C8 As1 117.7(3) . . ? C10 C9 C8 119.0(5) . . ? C10 C11 C12 119.6(5) . . ? C11 C10 C9 121.1(5) . . ? C11 C12 C13 120.5(5) . . ? C12 C13 C8 120.2(5) . . ? C13 C8 As1 122.5(3) . . ? C13 C8 C9 119.6(4) . . ? C14 As1 Au1 113.24(12) . . ? C14 As1 C1 106.91(16) . . ? C14 As1 C8 103.02(17) . . ? C14 C15 C16 119.8(4) . . ? C14 C19 C18 119.5(4) . . ? C15 C14 As1 118.2(3) . . ? C17 C16 C15 120.2(5) . . ? C17 C18 C19 120.6(5) . . ? C18 C17 C16 120.0(5) . . ? C19 C14 As1 121.7(3) . . ? C19 C14 C15 120.0(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.021 _refine_diff_density_min -0.685 _refine_diff_density_rms 0.124 #===END data_compound5c _database_code_depnum_ccdc_archive 'CCDC 290387' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H32 As2 Au2 I2' _chemical_formula_weight 1286.21 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2/c 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 19.4517(10) _cell_length_b 10.8921(6) _cell_length_c 19.1704(10) _cell_angle_alpha 90.00 _cell_angle_beta 112.2280(10) _cell_angle_gamma 90.00 _cell_volume 3759.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.087 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.272 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2360 _exptl_absorpt_coefficient_mu 11.209 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS Sheldrick 1996' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13750 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 28.31 _reflns_number_total 4682 _reflns_number_gt 3983 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0274P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4682 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0303 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0555 _refine_ls_wR_factor_gt 0.0531 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.010 _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 As1 As 0.453408(17) 0.32619(3) 0.121940(17) 0.03794(8) Uani 1 1 d . . . Au1 Au 0.424658(7) 0.164262(13) 0.188113(7) 0.04421(5) Uani 1 1 d . . . C1 C 0.53401(16) 0.4356(3) 0.17714(16) 0.0377(7) Uani 1 1 d . . . C2 C 0.53280(15) 0.5051(3) 0.23844(16) 0.0343(6) Uani 1 1 d . . . C3 C 0.59349(17) 0.5783(3) 0.27762(17) 0.0429(7) Uani 1 1 d . . . C4 C 0.65705(17) 0.5816(3) 0.26043(18) 0.0441(7) Uani 1 1 d . . . C5 C 0.65653(18) 0.5131(3) 0.1997(2) 0.0503(8) Uani 1 1 d . . . C6 C 0.59654(17) 0.4415(3) 0.15879(18) 0.0462(8) Uani 1 1 d . . . C7 C 0.7232(2) 0.6585(4) 0.3065(3) 0.0653(11) Uani 1 1 d . . . C8 C 0.48322(18) 0.2565(3) 0.04462(17) 0.0411(7) Uani 1 1 d . . . C9 C 0.5406(2) 0.1719(4) 0.0662(2) 0.0582(10) Uani 1 1 d . . . C10 C 0.5620(2) 0.1178(4) 0.0124(3) 0.0682(11) Uani 1 1 d . . . C11 C 0.5268(2) 0.1471(4) -0.0624(2) 0.0683(12) Uani 1 1 d . . . C12 C 0.4700(2) 0.2307(4) -0.0834(2) 0.0652(11) Uani 1 1 d . . . C13 C 0.4481(2) 0.2849(4) -0.03054(19) 0.0529(9) Uani 1 1 d . . . C14 C 0.36891(17) 0.4265(3) 0.06514(17) 0.0431(7) Uani 1 1 d . . . C15 C 0.29886(19) 0.3823(4) 0.0540(2) 0.0571(9) Uani 1 1 d . . . C16 C 0.2370(2) 0.4498(5) 0.0092(3) 0.0739(13) Uani 1 1 d . . . C17 C 0.2452(2) 0.5579(5) -0.0224(2) 0.0732(13) Uani 1 1 d . . . C18 C 0.3148(2) 0.6028(4) -0.0104(2) 0.0666(11) Uani 1 1 d . . . C19 C 0.3764(2) 0.5357(4) 0.0328(2) 0.0531(9) Uani 1 1 d . . . H3 H 0.5918 0.6270 0.3168 0.051 Uiso 1 1 calc R . . H5 H 0.6976 0.5153 0.1862 0.060 Uiso 1 1 calc R . . H6 H 0.5978 0.3963 0.1181 0.055 Uiso 1 1 calc R . . H7A H 0.7650 0.6060 0.3312 0.098 Uiso 1 1 calc R . . H7B H 0.7117 0.7039 0.3437 0.098 Uiso 1 1 calc R . . H7C H 0.7350 0.7147 0.2741 0.098 Uiso 1 1 calc R . . H9 H 0.5647 0.1516 0.1167 0.070 Uiso 1 1 calc R . . H10 H 0.6005 0.0609 0.0270 0.082 Uiso 1 1 calc R . . H11 H 0.5414 0.1105 -0.0985 0.082 Uiso 1 1 calc R . . H12 H 0.4460 0.2510 -0.1340 0.078 Uiso 1 1 calc R . . H13 H 0.4092 0.3411 -0.0456 0.063 Uiso 1 1 calc R . . H15 H 0.2931 0.3089 0.0759 0.069 Uiso 1 1 calc R . . H16 H 0.1896 0.4207 0.0009 0.089 Uiso 1 1 calc R . . H17 H 0.2034 0.6016 -0.0523 0.088 Uiso 1 1 calc R . . H18 H 0.3204 0.6776 -0.0311 0.080 Uiso 1 1 calc R . . H19 H 0.4236 0.5648 0.0402 0.064 Uiso 1 1 calc R . . I1 I 0.379766(14) -0.02169(3) 0.239027(15) 0.06349(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.03561(17) 0.0460(2) 0.03113(16) -0.00062(13) 0.01141(13) -0.00231(12) Au1 0.04091(8) 0.05325(9) 0.03603(8) 0.00219(5) 0.01181(6) -0.00600(5) C1 0.0339(15) 0.0462(18) 0.0317(15) 0.0015(13) 0.0111(12) -0.0002(13) C2 0.0339(16) 0.0397(17) 0.0280(13) 0.0050(12) 0.0101(12) 0.0020(12) C3 0.0454(19) 0.046(2) 0.0365(16) 0.0003(14) 0.0151(14) -0.0045(14) C4 0.0331(16) 0.047(2) 0.0469(18) 0.0024(15) 0.0098(14) -0.0020(13) C5 0.0338(17) 0.063(2) 0.057(2) -0.0007(17) 0.0207(16) -0.0027(15) C6 0.0436(18) 0.060(2) 0.0398(17) -0.0075(15) 0.0207(15) -0.0035(15) C7 0.045(2) 0.071(3) 0.071(3) -0.012(2) 0.0126(19) -0.0118(17) C8 0.0442(18) 0.0446(19) 0.0337(16) -0.0012(13) 0.0139(13) -0.0024(13) C9 0.055(2) 0.071(3) 0.048(2) 0.0001(18) 0.0186(18) 0.0112(18) C10 0.065(3) 0.071(3) 0.075(3) -0.006(2) 0.034(2) 0.016(2) C11 0.080(3) 0.077(3) 0.058(3) -0.023(2) 0.038(2) -0.007(2) C12 0.081(3) 0.077(3) 0.038(2) -0.0048(19) 0.0220(19) -0.001(2) C13 0.059(2) 0.058(2) 0.0395(19) -0.0051(16) 0.0161(16) 0.0023(17) C14 0.0379(17) 0.051(2) 0.0368(16) -0.0051(14) 0.0099(13) 0.0020(13) C15 0.044(2) 0.054(2) 0.068(2) -0.0114(19) 0.0154(18) -0.0039(17) C16 0.037(2) 0.078(3) 0.093(3) -0.018(3) 0.010(2) 0.0031(19) C17 0.058(3) 0.085(4) 0.060(3) -0.008(2) 0.002(2) 0.023(2) C18 0.069(3) 0.068(3) 0.059(2) 0.012(2) 0.021(2) 0.022(2) C19 0.051(2) 0.060(2) 0.049(2) 0.0067(17) 0.0194(17) 0.0012(16) I1 0.05953(16) 0.06828(19) 0.05777(16) 0.01261(12) 0.01667(12) -0.01565(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 As1 C1 1.935(3) . ? As1 C8 1.939(3) . ? As1 C14 1.931(3) . ? Au1 As1 2.3600(3) . ? Au1 Au1 2.9932(3) 2_655 ? Au1 I1 2.5421(3) . ? C1 C6 1.390(4) . ? C2 C1 1.405(4) . ? C2 C2 1.501(6) 2_655 ? C2 C3 1.387(4) . ? C3 C4 1.395(4) . ? C4 C5 1.379(5) . ? C4 C7 1.510(5) . ? C6 C5 1.376(5) . ? C8 C9 1.385(5) . ? C8 C13 1.376(4) . ? C9 C10 1.381(5) . ? C11 C10 1.373(6) . ? C12 C11 1.370(6) . ? C13 C12 1.373(5) . ? C14 C15 1.383(5) . ? C14 C19 1.374(5) . ? C15 C16 1.394(6) . ? C16 C17 1.360(7) . ? C18 C17 1.376(6) . ? C19 C18 1.379(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag As1 Au1 Au1 93.784(9) . 2_655 ? As1 Au1 I1 170.931(11) . . ? C1 As1 Au1 118.31(9) . . ? C1 As1 C8 104.15(13) . . ? C1 C2 C2 122.1(3) . 2_655 ? C2 C1 As1 121.5(2) . . ? C2 C3 C4 122.4(3) . . ? C3 C2 C1 118.8(3) . . ? C3 C2 C2 119.0(3) . 2_655 ? C3 C4 C7 120.8(3) . . ? C5 C4 C3 117.4(3) . . ? C5 C4 C7 121.8(3) . . ? C5 C6 C1 121.1(3) . . ? C6 C1 As1 119.7(2) . . ? C6 C1 C2 118.7(3) . . ? C6 C5 C4 121.5(3) . . ? C8 As1 Au1 108.58(10) . . ? C9 C8 As1 118.2(2) . . ? C10 C9 C8 119.9(4) . . ? C11 C10 C9 120.6(4) . . ? C11 C12 C13 120.7(4) . . ? C12 C11 C10 119.3(4) . . ? C12 C13 C8 120.5(4) . . ? C13 C8 As1 122.6(3) . . ? C13 C8 C9 119.1(3) . . ? C14 As1 Au1 113.70(10) . . ? C14 As1 C1 107.49(14) . . ? C14 As1 C8 103.14(13) . . ? C14 C15 C16 118.8(4) . . ? C14 C19 C18 120.9(4) . . ? C15 C14 As1 118.0(3) . . ? C16 C17 C18 120.5(4) . . ? C17 C16 C15 120.7(4) . . ? C17 C18 C19 119.2(4) . . ? C19 C14 As1 122.1(2) . . ? C19 C14 C15 119.8(3) . . ? I1 Au1 Au1 94.084(7) . 2_655 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.826 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.105 #===END data_compound6 _database_code_depnum_ccdc_archive 'CCDC 290388' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H32 As2 Au2 F10' _chemical_formula_weight 1366.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.7505(8) _cell_length_b 21.7158(12) _cell_length_c 14.9318(8) _cell_angle_alpha 90.00 _cell_angle_beta 95.7420(10) _cell_angle_gamma 90.00 _cell_volume 4436.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.046 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2584 _exptl_absorpt_coefficient_mu 8.164 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS Sheldrick 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32838 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0561 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 28.30 _reflns_number_total 11013 _reflns_number_gt 7802 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11013 _refine_ls_number_parameters 578 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0911 _refine_ls_wR_factor_gt 0.0821 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.959 _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 As1 As 0.21549(4) 0.41412(3) 0.67105(3) 0.04217(13) Uani 1 1 d . . . As2 As 0.20304(4) 0.58297(2) 0.88820(3) 0.04055(13) Uani 1 1 d . . . Au1 Au 0.279942(14) 0.445810(9) 0.820827(13) 0.03568(6) Uani 1 1 d . . . Au2 Au 0.254192(14) 0.554525(9) 0.743927(13) 0.03646(6) Uani 1 1 d . . . C1 C 0.3223(3) 0.4826(2) 0.9474(3) 0.0366(11) Uani 1 1 d . . . C2 C 0.3856(4) 0.4505(2) 1.0111(4) 0.0447(13) Uani 1 1 d . . . C3 C 0.4076(4) 0.4707(3) 1.0986(4) 0.0498(14) Uani 1 1 d . . . C4 C 0.3645(5) 0.5245(3) 1.1248(4) 0.0636(17) Uani 1 1 d . . . C5 C 0.3039(5) 0.5580(3) 1.0646(4) 0.0576(16) Uani 1 1 d . . . C6 C 0.2824(4) 0.5370(2) 0.9771(3) 0.0420(12) Uani 1 1 d . . . C7 C 0.4753(5) 0.4346(3) 1.1650(4) 0.073(2) Uani 1 1 d . . . C8 C 0.2425(5) 0.3308(3) 0.6363(4) 0.0527(15) Uani 1 1 d . . . C9 C 0.3376(5) 0.3126(3) 0.6378(4) 0.0640(17) Uani 1 1 d . . . C10 C 0.3608(6) 0.2522(3) 0.6188(5) 0.079(2) Uani 1 1 d . . . C11 C 0.2862(8) 0.2109(3) 0.5989(5) 0.093(3) Uani 1 1 d . . . C12 C 0.1922(8) 0.2295(3) 0.5955(6) 0.102(3) Uani 1 1 d . . . C13 C 0.1697(6) 0.2892(3) 0.6156(5) 0.078(2) Uani 1 1 d . . . C14 C 0.0747(4) 0.4225(3) 0.6527(4) 0.0495(14) Uani 1 1 d . . . C15 C 0.0230(5) 0.4205(4) 0.7262(5) 0.074(2) Uani 1 1 d . . . C16 C -0.0784(6) 0.4273(4) 0.7162(6) 0.090(2) Uani 1 1 d . . . C17 C -0.1249(6) 0.4365(3) 0.6350(7) 0.084(2) Uani 1 1 d . . . C18 C -0.0755(7) 0.4384(4) 0.5609(6) 0.089(3) Uani 1 1 d . . . C19 C 0.0251(6) 0.4308(4) 0.5692(5) 0.079(2) Uani 1 1 d . . . C20 C 0.2743(4) 0.4665(2) 0.5892(3) 0.0424(12) Uani 1 1 d . . . C21 C 0.2975(5) 0.4477(3) 0.5045(4) 0.0555(16) Uani 1 1 d . . . C22 C 0.3492(5) 0.4867(3) 0.4552(4) 0.0598(16) Uani 1 1 d . . . C23 C 0.3800(4) 0.5434(3) 0.4862(4) 0.0540(15) Uani 1 1 d . . . C24 C 0.3541(4) 0.5618(3) 0.5698(4) 0.0457(13) Uani 1 1 d . . . C25 C 0.3007(4) 0.5243(2) 0.6232(3) 0.0405(12) Uani 1 1 d . . . C26 C 0.4395(5) 0.5845(3) 0.4304(4) 0.0716(19) Uani 1 1 d . . . C27 C 0.2188(4) 0.6695(3) 0.9173(3) 0.0445(12) Uani 1 1 d . . . C28 C 0.3082(5) 0.6933(3) 0.9520(4) 0.0574(15) Uani 1 1 d . . . C29 C 0.3188(6) 0.7557(3) 0.9661(4) 0.0707(19) Uani 1 1 d . . . C30 C 0.2423(6) 0.7941(3) 0.9457(5) 0.0691(19) Uani 1 1 d . . . C31 C 0.1536(5) 0.7710(3) 0.9109(4) 0.0658(18) Uani 1 1 d . . . C32 C 0.1417(5) 0.7089(3) 0.8982(4) 0.0563(15) Uani 1 1 d . . . C33 C 0.0662(4) 0.5712(2) 0.9005(4) 0.0438(13) Uani 1 1 d . . . C34 C 0.0302(5) 0.5776(3) 0.9830(4) 0.0631(17) Uani 1 1 d . . . C35 C -0.0697(6) 0.5750(3) 0.9885(6) 0.077(2) Uani 1 1 d . . . C36 C -0.1310(5) 0.5670(3) 0.9132(6) 0.076(2) Uani 1 1 d . . . C37 C -0.0959(6) 0.5607(4) 0.8321(6) 0.083(2) Uani 1 1 d . . . C38 C 0.0036(5) 0.5632(3) 0.8258(5) 0.0684(19) Uani 1 1 d . . . C39 C 0.3076(4) 0.3525(2) 0.8578(3) 0.0425(12) Uani 1 1 d . . . C40 C 0.2360(4) 0.3085(3) 0.8634(4) 0.0533(14) Uani 1 1 d . . . C41 C 0.2545(6) 0.2464(3) 0.8697(5) 0.0699(19) Uani 1 1 d . . . C42 C 0.3471(6) 0.2258(3) 0.8719(5) 0.071(2) Uani 1 1 d . . . C43 C 0.4214(5) 0.2668(3) 0.8673(4) 0.0662(18) Uani 1 1 d . . . C44 C 0.4008(4) 0.3281(3) 0.8605(4) 0.0525(14) Uani 1 1 d . . . C45 C 0.2284(5) 0.6444(3) 0.6972(4) 0.0528(15) Uani 1 1 d . . . C46 C 0.2917(6) 0.6916(3) 0.7184(4) 0.0615(17) Uani 1 1 d . . . C47 C 0.2696(8) 0.7531(4) 0.7008(6) 0.087(3) Uani 1 1 d . . . C48 C 0.1789(9) 0.7663(4) 0.6600(7) 0.102(4) Uani 1 1 d . . . C49 C 0.1126(7) 0.7228(5) 0.6362(6) 0.102(3) Uani 1 1 d . . . C50 C 0.1376(6) 0.6623(3) 0.6553(4) 0.0676(19) Uani 1 1 d . . . F1 F 0.1424(3) 0.32718(18) 0.8597(3) 0.0902(13) Uani 1 1 d . . . F2 F 0.1811(4) 0.20660(19) 0.8718(4) 0.125(2) Uani 1 1 d . . . F3 F 0.3664(4) 0.16560(17) 0.8773(3) 0.1124(17) Uani 1 1 d . . . F4 F 0.5136(3) 0.2454(2) 0.8698(3) 0.1071(16) Uani 1 1 d . . . F5 F 0.4768(3) 0.36641(18) 0.8518(3) 0.0833(12) Uani 1 1 d . . . F6 F 0.3810(3) 0.67898(18) 0.7594(3) 0.0845(12) Uani 1 1 d . . . F7 F 0.3324(5) 0.7980(2) 0.7256(4) 0.142(2) Uani 1 1 d . . . F8 F 0.1551(5) 0.8264(2) 0.6423(4) 0.172(3) Uani 1 1 d . . . F9 F 0.0243(4) 0.7362(3) 0.5937(4) 0.162(3) Uani 1 1 d . . . F10 F 0.0690(3) 0.6189(3) 0.6331(3) 0.1024(15) Uani 1 1 d . . . H2 H 0.4138 0.4141 0.9935 0.054 Uiso 1 1 calc R . . H4 H 0.3767 0.5381 1.1839 0.076 Uiso 1 1 calc R . . H5 H 0.2772 0.5948 1.0825 0.069 Uiso 1 1 calc R . . H7A H 0.5294 0.4601 1.1872 0.109 Uiso 1 1 calc R . . H7B H 0.4989 0.3991 1.1357 0.109 Uiso 1 1 calc R . . H7C H 0.4404 0.4217 1.2143 0.109 Uiso 1 1 calc R . . H9 H 0.3874 0.3410 0.6518 0.077 Uiso 1 1 calc R . . H10 H 0.4256 0.2400 0.6195 0.095 Uiso 1 1 calc R . . H11 H 0.3004 0.1699 0.5876 0.112 Uiso 1 1 calc R . . H12 H 0.1422 0.2015 0.5795 0.123 Uiso 1 1 calc R . . H13 H 0.1047 0.3012 0.6150 0.094 Uiso 1 1 calc R . . H15 H 0.0556 0.4146 0.7831 0.089 Uiso 1 1 calc R . . H16 H -0.1134 0.4253 0.7663 0.107 Uiso 1 1 calc R . . H17 H -0.1924 0.4418 0.6289 0.101 Uiso 1 1 calc R . . H18 H -0.1091 0.4447 0.5045 0.107 Uiso 1 1 calc R . . H19 H 0.0588 0.4315 0.5182 0.095 Uiso 1 1 calc R . . H21 H 0.2781 0.4092 0.4820 0.067 Uiso 1 1 calc R . . H22 H 0.3639 0.4742 0.3985 0.072 Uiso 1 1 calc R . . H24 H 0.3731 0.6007 0.5911 0.055 Uiso 1 1 calc R . . H26A H 0.4872 0.5602 0.4037 0.107 Uiso 1 1 calc R . . H26B H 0.4720 0.6155 0.4683 0.107 Uiso 1 1 calc R . . H26C H 0.3969 0.6039 0.3839 0.107 Uiso 1 1 calc R . . H28 H 0.3611 0.6671 0.9657 0.069 Uiso 1 1 calc R . . H29 H 0.3788 0.7715 0.9896 0.085 Uiso 1 1 calc R . . H30 H 0.2498 0.8363 0.9554 0.083 Uiso 1 1 calc R . . H31 H 0.1014 0.7976 0.8959 0.079 Uiso 1 1 calc R . . H32 H 0.0809 0.6933 0.8764 0.068 Uiso 1 1 calc R . . H34 H 0.0728 0.5836 1.0347 0.076 Uiso 1 1 calc R . . H35 H -0.0944 0.5788 1.0440 0.092 Uiso 1 1 calc R . . H36 H -0.1981 0.5658 0.9169 0.091 Uiso 1 1 calc R . . H37 H -0.1388 0.5547 0.7807 0.100 Uiso 1 1 calc R . . H38 H 0.0276 0.5592 0.7700 0.082 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 As1 0.0504(3) 0.0343(3) 0.0412(3) -0.0026(2) 0.0017(2) -0.0010(2) As2 0.0489(3) 0.0321(3) 0.0414(3) -0.0008(2) 0.0081(2) -0.0005(2) Au1 0.03871(11) 0.02951(11) 0.03872(12) 0.00098(8) 0.00328(8) -0.00167(8) Au2 0.04136(12) 0.03046(11) 0.03784(12) 0.00180(8) 0.00540(8) 0.00121(8) C1 0.038(3) 0.036(3) 0.035(3) 0.004(2) -0.002(2) -0.004(2) C2 0.038(3) 0.043(3) 0.052(3) 0.003(2) 0.003(2) -0.002(2) C3 0.052(3) 0.054(4) 0.042(3) 0.007(3) -0.006(2) -0.017(3) C4 0.085(5) 0.066(4) 0.036(3) -0.003(3) -0.008(3) -0.021(4) C5 0.085(5) 0.040(3) 0.046(4) -0.004(3) 0.001(3) -0.004(3) C6 0.049(3) 0.039(3) 0.037(3) 0.005(2) 0.001(2) -0.002(2) C7 0.066(4) 0.098(6) 0.050(4) 0.009(4) -0.016(3) -0.009(4) C8 0.069(4) 0.043(3) 0.045(3) -0.010(3) 0.002(3) -0.005(3) C9 0.072(5) 0.051(4) 0.069(4) 0.000(3) 0.010(3) 0.001(3) C10 0.102(6) 0.060(5) 0.079(5) -0.002(4) 0.022(4) 0.026(4) C11 0.147(9) 0.040(4) 0.094(6) -0.016(4) 0.015(6) 0.013(5) C12 0.126(8) 0.044(5) 0.133(8) -0.022(5) -0.002(6) -0.002(5) C13 0.085(5) 0.041(4) 0.107(6) -0.014(4) 0.001(4) -0.003(4) C14 0.057(4) 0.043(3) 0.046(3) 0.002(3) -0.006(3) -0.007(3) C15 0.048(4) 0.100(6) 0.072(5) 0.014(4) 0.000(3) 0.008(4) C16 0.057(5) 0.107(6) 0.104(7) 0.013(5) 0.007(4) 0.001(4) C17 0.069(5) 0.051(4) 0.127(8) -0.004(4) -0.012(5) -0.001(4) C18 0.081(6) 0.088(6) 0.089(6) 0.012(5) -0.038(5) 0.002(4) C19 0.084(6) 0.080(5) 0.071(5) 0.006(4) -0.010(4) 0.002(4) C20 0.048(3) 0.041(3) 0.038(3) 0.001(2) 0.005(2) 0.002(2) C21 0.071(4) 0.049(4) 0.046(4) -0.008(3) 0.008(3) 0.004(3) C22 0.075(4) 0.065(4) 0.042(3) 0.002(3) 0.017(3) 0.019(3) C23 0.056(4) 0.054(4) 0.053(4) 0.015(3) 0.010(3) 0.018(3) C24 0.045(3) 0.048(3) 0.045(3) 0.003(2) 0.005(2) 0.007(2) C25 0.042(3) 0.041(3) 0.038(3) 0.005(2) 0.004(2) 0.004(2) C26 0.081(5) 0.077(5) 0.062(4) 0.018(4) 0.027(4) 0.015(4) C27 0.053(3) 0.041(3) 0.041(3) -0.003(2) 0.008(2) -0.004(3) C28 0.058(4) 0.045(4) 0.069(4) 0.002(3) 0.005(3) 0.001(3) C29 0.087(5) 0.049(4) 0.074(5) -0.005(3) -0.003(4) -0.022(4) C30 0.093(5) 0.038(4) 0.075(5) -0.009(3) 0.007(4) -0.014(4) C31 0.078(5) 0.035(4) 0.085(5) -0.004(3) 0.016(4) 0.003(3) C32 0.056(4) 0.049(4) 0.064(4) -0.005(3) 0.008(3) -0.006(3) C33 0.054(3) 0.036(3) 0.044(3) -0.003(2) 0.014(3) -0.001(2) C34 0.076(5) 0.050(4) 0.065(4) -0.007(3) 0.020(3) -0.007(4) C35 0.096(6) 0.059(4) 0.083(6) -0.003(4) 0.048(5) -0.005(4) C36 0.055(4) 0.055(4) 0.121(7) 0.008(4) 0.031(5) -0.004(3) C37 0.068(5) 0.097(6) 0.083(6) -0.001(4) 0.002(4) -0.003(4) C38 0.061(4) 0.085(5) 0.061(4) -0.008(3) 0.013(3) -0.010(4) C39 0.050(3) 0.037(3) 0.039(3) 0.003(2) 0.001(2) -0.004(2) C40 0.053(4) 0.043(3) 0.065(4) 0.010(3) 0.007(3) -0.003(3) C41 0.085(5) 0.047(4) 0.082(5) 0.012(3) 0.026(4) -0.008(4) C42 0.105(6) 0.040(4) 0.071(5) 0.014(3) 0.025(4) 0.015(4) C43 0.074(5) 0.057(4) 0.067(4) 0.010(3) 0.007(3) 0.025(4) C44 0.049(3) 0.050(4) 0.057(4) -0.001(3) 0.000(3) 0.001(3) C45 0.072(4) 0.045(4) 0.044(3) 0.014(3) 0.018(3) 0.013(3) C46 0.089(5) 0.041(4) 0.059(4) 0.010(3) 0.029(4) -0.003(4) C47 0.134(8) 0.050(5) 0.086(6) 0.010(4) 0.061(5) 0.000(5) C48 0.154(10) 0.058(6) 0.109(7) 0.037(5) 0.087(7) 0.045(6) C49 0.112(7) 0.119(8) 0.082(6) 0.053(6) 0.043(5) 0.069(6) C50 0.081(5) 0.073(5) 0.051(4) 0.023(3) 0.020(3) 0.021(4) F1 0.059(2) 0.060(2) 0.155(4) 0.009(3) 0.027(2) -0.005(2) F2 0.119(4) 0.052(3) 0.214(6) 0.012(3) 0.064(4) -0.026(3) F3 0.173(5) 0.036(2) 0.135(4) 0.023(2) 0.051(3) 0.029(3) F4 0.089(3) 0.091(3) 0.142(4) 0.010(3) 0.013(3) 0.047(3) F5 0.051(2) 0.071(3) 0.127(3) -0.009(2) 0.010(2) -0.002(2) F6 0.092(3) 0.066(3) 0.097(3) 0.005(2) 0.015(2) -0.025(2) F7 0.231(7) 0.051(3) 0.162(5) -0.012(3) 0.108(5) -0.038(4) F8 0.264(8) 0.082(4) 0.194(6) 0.078(4) 0.142(6) 0.099(4) F9 0.121(4) 0.207(7) 0.164(5) 0.110(5) 0.047(4) 0.102(5) F10 0.080(3) 0.144(5) 0.080(3) 0.023(3) -0.007(2) 0.015(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 As1 C8 1.929(6) . ? As1 C14 1.936(6) . ? As1 C20 1.907(5) . ? As2 C6 1.914(5) . ? As2 C27 1.937(5) . ? As2 C33 1.926(6) . ? Au1 As1 2.4216(6) . ? Au1 Au2 2.6336(3) . ? Au1 C1 2.081(5) . ? Au1 C39 2.124(5) . ? Au2 As2 2.4125(6) . ? Au2 C25 2.078(5) . ? Au2 C45 2.090(6) . ? C1 C2 1.408(7) . ? C1 C6 1.392(7) . ? C2 C3 1.383(7) . ? C3 C7 1.509(8) . ? C4 C3 1.383(9) . ? C4 C5 1.371(8) . ? C6 C5 1.388(7) . ? C8 C13 1.361(9) . ? C9 C8 1.364(9) . ? C9 C10 1.385(8) . ? C11 C10 1.373(11) . ? C12 C11 1.349(11) . ? C13 C12 1.373(10) . ? C14 C15 1.366(8) . ? C14 C19 1.374(8) . ? C15 C16 1.396(9) . ? C17 C16 1.328(11) . ? C18 C17 1.356(12) . ? C18 C19 1.386(11) . ? C21 C20 1.397(7) . ? C21 C22 1.368(8) . ? C23 C22 1.370(8) . ? C23 C24 1.391(8) . ? C23 C26 1.515(8) . ? C25 C20 1.390(7) . ? C25 C24 1.398(7) . ? C27 C28 1.385(8) . ? C27 C32 1.369(8) . ? C28 C29 1.377(8) . ? C30 C29 1.354(9) . ? C30 C31 1.373(9) . ? C32 C31 1.370(8) . ? C33 C34 1.379(8) . ? C33 C38 1.350(8) . ? C34 C35 1.386(10) . ? C36 C35 1.347(11) . ? C36 C37 1.355(10) . ? C38 C37 1.382(9) . ? C39 C40 1.381(7) . ? C39 C44 1.385(8) . ? C40 C41 1.373(8) . ? C42 C41 1.347(10) . ? C43 C42 1.362(10) . ? C44 C43 1.364(8) . ? C45 C46 1.362(9) . ? C45 C50 1.395(9) . ? C46 C47 1.388(9) . ? C47 C48 1.363(13) . ? C48 F8 1.366(8) . ? C49 C48 1.336(13) . ? C49 C50 1.381(10) . ? C49 F9 1.344(10) . ? C50 F10 1.350(8) . ? F1 C40 1.346(7) . ? F2 C41 1.332(8) . ? F3 C42 1.335(7) . ? F4 C43 1.346(7) . ? F5 C44 1.352(7) . ? F6 C46 1.345(8) . ? F7 C47 1.331(10) . ? 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 As1 Au1 Au2 80.285(15) . . ? As2 Au2 Au1 83.031(15) . . ? C1 Au1 As1 172.43(14) . . ? C1 Au1 Au2 93.70(13) . . ? C1 Au1 C39 95.98(19) . . ? C1 C6 As2 115.9(4) . . ? C2 C1 Au1 121.4(4) . . ? C2 C3 C7 121.2(6) . . ? C3 C2 C1 122.9(5) . . ? C4 C3 C2 118.3(5) . . ? C4 C3 C7 120.5(5) . . ? C4 C5 C6 120.1(6) . . ? C5 C4 C3 120.8(5) . . ? C5 C6 As2 122.3(4) . . ? C5 C6 C1 121.7(5) . . ? C6 As2 Au2 106.78(16) . . ? C6 As2 C27 107.9(2) . . ? C6 As2 C33 111.1(2) . . ? C6 C1 Au1 122.1(4) . . ? C6 C1 C2 116.2(5) . . ? C8 As1 Au1 116.92(18) . . ? C8 As1 C14 105.5(3) . . ? C8 C9 C10 120.8(7) . . ? C8 C13 C12 119.9(8) . . ? C9 C8 As1 118.5(5) . . ? C11 C10 C9 118.7(7) . . ? C11 C12 C13 120.7(8) . . ? C12 C11 C10 120.3(7) . . ? C13 C8 As1 121.8(5) . . ? C13 C8 C9 119.6(6) . . ? C14 As1 Au1 111.85(17) . . ? C14 C15 C16 120.4(7) . . ? C14 C19 C18 119.8(7) . . ? C15 C14 As1 118.5(5) . . ? C15 C14 C19 118.8(6) . . ? C16 C17 C18 120.9(8) . . ? C17 C16 C15 119.9(8) . . ? C17 C18 C19 120.1(8) . . ? C19 C14 As1 122.7(5) . . ? C20 As1 Au1 106.43(16) . . ? C20 As1 C8 106.4(2) . . ? C20 As1 C14 109.6(2) . . ? C20 C25 Au2 120.7(4) . . ? C20 C25 C24 116.8(5) . . ? C21 C20 As1 123.8(4) . . ? C21 C22 C23 122.4(6) . . ? C22 C21 C20 119.0(5) . . ? C22 C23 C24 117.6(6) . . ? C22 C23 C26 120.7(6) . . ? C23 C24 C25 122.8(5) . . ? C24 C23 C26 121.7(6) . . ? C24 C25 Au2 122.4(4) . . ? C25 Au2 As2 176.20(14) . . ? C25 Au2 Au1 93.19(14) . . ? C25 Au2 C45 93.5(2) . . ? C25 C20 As1 114.7(4) . . ? C25 C20 C21 121.3(5) . . ? C27 As2 Au2 114.39(15) . . ? C27 C32 C31 120.4(6) . . ? C28 C27 As2 121.4(4) . . ? C29 C28 C27 120.0(6) . . ? C29 C30 C31 120.0(6) . . ? C30 C29 C28 120.3(7) . . ? C32 C27 As2 119.5(4) . . ? C32 C27 C28 119.0(5) . . ? C32 C31 C30 120.1(7) . . ? C33 As2 Au2 115.23(16) . . ? C33 As2 C27 101.3(2) . . ? C33 C34 C35 119.6(7) . . ? C33 C38 C37 120.1(7) . . ? C34 C33 As2 120.8(5) . . ? C35 C36 C37 120.6(7) . . ? C36 C35 C34 119.8(6) . . ? C36 C37 C38 120.1(7) . . ? C38 C33 As2 119.1(4) . . ? C38 C33 C34 119.7(6) . . ? C39 Au1 As1 90.48(14) . . ? C39 Au1 Au2 168.83(14) . . ? C40 C39 Au1 124.5(4) . . ? C40 C39 C44 113.4(5) . . ? C41 C40 C39 123.8(6) . . ? C41 C42 C43 119.6(6) . . ? C42 C41 C40 119.7(7) . . ? C42 C43 C44 119.4(6) . . ? C43 C44 C39 124.1(6) . . ? C44 C39 Au1 120.9(4) . . ? C45 Au2 As2 90.24(15) . . ? C45 Au2 Au1 173.27(15) . . ? C45 C46 C47 123.9(8) . . ? C46 C45 Au2 122.9(5) . . ? C46 C45 C50 114.6(6) . . ? C47 C48 F8 118.6(11) . . ? C48 C47 C46 117.4(9) . . ? C48 C49 C50 117.9(9) . . ? C48 C49 F9 122.2(10) . . ? C49 C48 C47 122.7(8) . . ? C49 C48 F8 118.7(11) . . ? C49 C50 C45 123.5(9) . . ? C50 C45 Au2 121.6(5) . . ? F1 C40 C39 118.2(5) . . ? F1 C40 C41 118.0(6) . . ? F2 C41 C40 120.2(7) . . ? F2 C41 C42 120.1(6) . . ? F3 C42 C41 120.5(7) . . ? F3 C42 C43 119.8(7) . . ? F4 C43 C42 118.9(6) . . ? F4 C43 C44 121.8(7) . . ? F5 C44 C39 119.0(5) . . ? F5 C44 C43 116.8(6) . . ? F6 C46 C45 119.0(6) . . ? F6 C46 C47 117.1(7) . . ? F7 C47 C46 121.9(9) . . ? F7 C47 C48 120.7(8) . . ? F9 C49 C50 119.9(11) . . ? F10 C50 C45 119.2(6) . . ? F10 C50 C49 117.3(8) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.653 _refine_diff_density_min -0.901 _refine_diff_density_rms 0.141 #===END data_compound7 _database_code_depnum_ccdc_archive 'CCDC 290389' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H32 As2 Au2 F10' _chemical_formula_weight 1366.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.0980(9) _cell_length_b 20.5775(16) _cell_length_c 18.6526(15) _cell_angle_alpha 90.00 _cell_angle_beta 97.678(2) _cell_angle_gamma 90.00 _cell_volume 4601.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.972 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2584 _exptl_absorpt_coefficient_mu 7.871 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS Sheldrick 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33783 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 28.35 _reflns_number_total 11431 _reflns_number_gt 7707 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11431 _refine_ls_number_parameters 579 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1093 _refine_ls_wR_factor_gt 0.0954 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _refine_ls_shift/su_max 0.130 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.51908(4) 0.35705(2) 0.27579(3) 0.04987(13) Uani 1 1 d . . . As2 As 0.23746(4) 0.38600(3) 0.08485(3) 0.05805(14) Uani 1 1 d . . . Au1 Au 0.387711(18) 0.272484(10) 0.243518(12) 0.05692(8) Uani 1 1 d . . . Au2 Au 0.209750(18) 0.424177(12) 0.201314(14) 0.06787(9) Uani 1 1 d . . . C1 C 0.2846(4) 0.1941(2) 0.2259(3) 0.0560(12) Uani 1 1 d . . . C2 C 0.3033(5) 0.1461(3) 0.1788(3) 0.0645(14) Uani 1 1 d . . . C3 C 0.2391(6) 0.0920(3) 0.1678(4) 0.0748(17) Uani 1 1 d . . . C4 C 0.1541(6) 0.0816(3) 0.2060(5) 0.084(2) Uani 1 1 d . . . C5 C 0.1317(5) 0.1285(3) 0.2557(4) 0.0799(19) Uani 1 1 d . . . C6 C 0.1978(5) 0.1824(3) 0.2644(4) 0.0697(16) Uani 1 1 d . . . C7 C 0.5148(4) 0.3811(2) 0.3759(3) 0.0534(12) Uani 1 1 d . . . C8 C 0.4135(5) 0.3782(3) 0.4011(3) 0.0663(15) Uani 1 1 d . . . C9 C 0.4029(7) 0.3961(3) 0.4702(4) 0.086(2) Uani 1 1 d . . . C10 C 0.4932(7) 0.4170(3) 0.5154(4) 0.083(2) Uani 1 1 d . . . C11 C 0.5943(7) 0.4198(3) 0.4914(4) 0.090(2) Uani 1 1 d . . . C12 C 0.6063(6) 0.4012(3) 0.4215(3) 0.0745(16) Uani 1 1 d . . . C13 C 0.6727(4) 0.3332(2) 0.2718(3) 0.0537(12) Uani 1 1 d . . . C14 C 0.7000(6) 0.2690(3) 0.2664(4) 0.0743(17) Uani 1 1 d . . . C15 C 0.8096(7) 0.2512(4) 0.2645(4) 0.093(2) Uani 1 1 d . . . C16 C 0.8912(6) 0.2973(4) 0.2671(4) 0.091(2) Uani 1 1 d . . . C17 C 0.8635(5) 0.3607(4) 0.2721(4) 0.0842(19) Uani 1 1 d . . . C18 C 0.7556(5) 0.3800(3) 0.2739(3) 0.0654(14) Uani 1 1 d . . . C19 C 0.4980(4) 0.4388(2) 0.2238(3) 0.0469(11) Uani 1 1 d . . . C20 C 0.4983(4) 0.4965(3) 0.2623(3) 0.0558(12) Uani 1 1 d . . . C21 C 0.4763(5) 0.5551(3) 0.2259(3) 0.0661(15) Uani 1 1 d . . . C22 C 0.4550(5) 0.5569(3) 0.1512(3) 0.0650(15) Uani 1 1 d . . . C23 C 0.4564(5) 0.4991(2) 0.1141(3) 0.0584(13) Uani 1 1 d . . . C24 C 0.4771(4) 0.4393(2) 0.1494(3) 0.0456(10) Uani 1 1 d . . . C25 C 0.4300(7) 0.6199(3) 0.1113(4) 0.102(3) Uani 1 1 d . . . C26 C 0.4787(4) 0.3785(2) 0.1057(2) 0.0464(10) Uani 1 1 d . . . C27 C 0.5805(4) 0.3507(2) 0.0976(3) 0.0550(12) Uani 1 1 d . . . C28 C 0.5881(5) 0.2942(2) 0.0568(3) 0.0578(13) Uani 1 1 d . . . C29 C 0.4904(6) 0.2666(3) 0.0250(4) 0.0696(16) Uani 1 1 d . . . C30 C 0.3889(5) 0.2928(3) 0.0319(3) 0.0613(14) Uani 1 1 d . . . C31 C 0.3811(4) 0.3486(2) 0.0727(3) 0.0497(11) Uani 1 1 d . . . C32 C 0.7004(6) 0.2664(3) 0.0485(4) 0.093(2) Uani 1 1 d . . . C33 C 0.1306(4) 0.3192(3) 0.0506(3) 0.0593(13) Uani 1 1 d . . . C34 C 0.0954(6) 0.3103(4) -0.0209(4) 0.096(2) Uani 1 1 d . . . C35 C 0.0185(7) 0.2593(5) -0.0418(5) 0.114(3) Uani 1 1 d . . . C36 C -0.0205(6) 0.2236(4) 0.0092(5) 0.093(2) Uani 1 1 d . . . C37 C 0.0139(6) 0.2331(4) 0.0807(5) 0.102(3) Uani 1 1 d . . . C38 C 0.0889(5) 0.2818(3) 0.1022(4) 0.0800(18) Uani 1 1 d . . . C39 C 0.2137(5) 0.4539(3) 0.0125(4) 0.0757(18) Uani 1 1 d . . . C40 C 0.1514(6) 0.5066(4) 0.0256(5) 0.103(3) Uani 1 1 d . . . C41 C 0.1257(8) 0.5558(5) -0.0244(8) 0.142(5) Uani 1 1 d . . . C42 C 0.1668(9) 0.5470(7) -0.0910(8) 0.151(5) Uani 1 1 d . . . C43 C 0.2320(9) 0.4964(5) -0.1047(5) 0.123(3) Uani 1 1 d . . . C44 C 0.2544(6) 0.4488(4) -0.0531(4) 0.095(2) Uani 1 1 d . . . C45 C 0.1752(4) 0.4649(3) 0.2960(4) 0.0656(15) Uani 1 1 d . . . C46 C 0.1457(5) 0.4292(3) 0.3526(4) 0.0741(18) Uani 1 1 d . . . C47 C 0.1251(5) 0.4563(4) 0.4168(4) 0.0827(19) Uani 1 1 d . . . C48 C 0.1307(6) 0.5221(4) 0.4241(5) 0.094(2) Uani 1 1 d . . . C49 C 0.1592(6) 0.5597(4) 0.3697(5) 0.086(2) Uani 1 1 d . . . C50 C 0.1805(5) 0.5299(3) 0.3065(4) 0.0775(18) Uani 1 1 d . . . F1 F 0.3870(4) 0.15266(19) 0.1383(2) 0.0985(13) Uani 1 1 d . . . F2 F 0.2624(4) 0.0449(2) 0.1204(3) 0.1135(15) Uani 1 1 d . . . F3 F 0.0932(4) 0.02692(19) 0.2000(3) 0.1169(16) Uani 1 1 d . . . F4 F 0.0469(4) 0.1202(3) 0.2946(3) 0.1288(18) Uani 1 1 d . . . F5 F 0.1723(4) 0.22603(19) 0.3135(3) 0.1055(15) Uani 1 1 d . . . F6 F 0.1381(3) 0.36375(18) 0.3484(3) 0.0953(12) Uani 1 1 d . . . F7 F 0.0993(4) 0.4194(3) 0.4712(3) 0.1236(17) Uani 1 1 d . . . F8 F 0.1127(4) 0.5496(3) 0.4872(3) 0.139(2) Uani 1 1 d . . . F9 F 0.1670(4) 0.6239(2) 0.3774(3) 0.1263(18) Uani 1 1 d . . . F10 F 0.2077(4) 0.56984(19) 0.2539(3) 0.1082(14) Uani 1 1 d . . . H8 H 0.3511 0.3639 0.3706 0.080 Uiso 1 1 calc R . . H9 H 0.3335 0.3940 0.4864 0.103 Uiso 1 1 calc R . . H10 H 0.4858 0.4294 0.5625 0.100 Uiso 1 1 calc R . . H11 H 0.6562 0.4342 0.5223 0.108 Uiso 1 1 calc R . . H12 H 0.6760 0.4024 0.4057 0.089 Uiso 1 1 calc R . . H14 H 0.6447 0.2374 0.2639 0.089 Uiso 1 1 calc R . . H15 H 0.8280 0.2075 0.2615 0.112 Uiso 1 1 calc R . . H16 H 0.9650 0.2853 0.2655 0.109 Uiso 1 1 calc R . . H17 H 0.9193 0.3920 0.2744 0.101 Uiso 1 1 calc R . . H18 H 0.7381 0.4238 0.2766 0.078 Uiso 1 1 calc R . . H20 H 0.5133 0.4960 0.3125 0.067 Uiso 1 1 calc R . . H21 H 0.4759 0.5935 0.2522 0.079 Uiso 1 1 calc R . . H23 H 0.4432 0.4998 0.0638 0.070 Uiso 1 1 calc R . . H25A H 0.4961 0.6352 0.0934 0.154 Uiso 1 1 calc R . . H25B H 0.4057 0.6516 0.1435 0.154 Uiso 1 1 calc R . . H25C H 0.3722 0.6130 0.0714 0.154 Uiso 1 1 calc R . . H27 H 0.6456 0.3701 0.1199 0.066 Uiso 1 1 calc R . . H29 H 0.4936 0.2288 -0.0020 0.084 Uiso 1 1 calc R . . H30 H 0.3244 0.2731 0.0091 0.074 Uiso 1 1 calc R . . H32A H 0.7110 0.2265 0.0751 0.139 Uiso 1 1 calc R . . H32B H 0.7575 0.2968 0.0669 0.139 Uiso 1 1 calc R . . H32C H 0.7046 0.2582 -0.0017 0.139 Uiso 1 1 calc R . . H34 H 0.1211 0.3369 -0.0554 0.116 Uiso 1 1 calc R . . H35 H -0.0045 0.2509 -0.0905 0.136 Uiso 1 1 calc R . . H36 H -0.0728 0.1912 -0.0047 0.111 Uiso 1 1 calc R . . H37 H -0.0130 0.2068 0.1150 0.123 Uiso 1 1 calc R . . H38 H 0.1113 0.2895 0.1511 0.096 Uiso 1 1 calc R . . H40 H 0.1249 0.5096 0.0700 0.124 Uiso 1 1 calc R . . H41 H 0.0843 0.5921 -0.0147 0.170 Uiso 1 1 calc R . . H42 H 0.1481 0.5775 -0.1273 0.181 Uiso 1 1 calc R . . H43 H 0.2613 0.4939 -0.1483 0.148 Uiso 1 1 calc R . . H44 H 0.2971 0.4130 -0.0623 0.114 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 As1 0.0524(3) 0.0441(3) 0.0521(3) 0.0045(2) 0.0032(2) -0.0035(2) As2 0.0519(3) 0.0549(3) 0.0674(4) -0.0046(2) 0.0084(2) -0.0075(2) Au1 0.06123(14) 0.04856(12) 0.06036(14) 0.00327(9) 0.00593(10) -0.00985(9) Au2 0.05426(14) 0.06928(16) 0.08075(18) -0.01944(11) 0.01154(11) -0.00101(10) C1 0.058(3) 0.050(3) 0.060(3) 0.006(2) 0.003(2) 0.000(2) C2 0.070(4) 0.057(3) 0.066(4) 0.002(3) 0.009(3) -0.006(3) C3 0.088(5) 0.058(4) 0.075(4) -0.009(3) -0.004(3) 0.004(3) C4 0.072(4) 0.051(4) 0.119(6) 0.006(4) -0.022(4) -0.011(3) C5 0.049(3) 0.074(4) 0.119(6) 0.011(4) 0.020(3) -0.012(3) C6 0.062(3) 0.057(3) 0.091(5) -0.013(3) 0.013(3) -0.002(3) C7 0.066(3) 0.047(3) 0.046(3) 0.009(2) 0.004(2) -0.002(2) C8 0.060(3) 0.074(4) 0.065(4) 0.006(3) 0.009(3) 0.013(3) C9 0.105(5) 0.082(4) 0.074(5) 0.010(3) 0.027(4) 0.025(4) C10 0.121(6) 0.068(4) 0.062(4) 0.000(3) 0.019(4) -0.001(4) C11 0.111(6) 0.088(5) 0.065(4) -0.008(3) -0.014(4) -0.024(4) C12 0.080(4) 0.078(4) 0.065(4) -0.002(3) 0.008(3) -0.017(3) C13 0.058(3) 0.046(3) 0.056(3) 0.004(2) 0.002(2) 0.005(2) C14 0.077(4) 0.060(4) 0.084(5) 0.002(3) 0.004(3) 0.004(3) C15 0.102(6) 0.080(5) 0.098(6) 0.002(4) 0.013(4) 0.041(5) C16 0.069(4) 0.109(6) 0.095(5) 0.014(4) 0.012(4) 0.030(4) C17 0.058(4) 0.101(6) 0.092(5) 0.011(4) 0.005(3) 0.002(4) C18 0.060(3) 0.061(3) 0.075(4) 0.011(3) 0.007(3) 0.001(3) C19 0.046(3) 0.035(2) 0.056(3) 0.0009(19) -0.004(2) -0.0014(19) C20 0.064(3) 0.055(3) 0.046(3) -0.004(2) 0.001(2) -0.006(2) C21 0.080(4) 0.050(3) 0.066(4) -0.003(3) 0.005(3) -0.002(3) C22 0.080(4) 0.040(3) 0.074(4) 0.005(2) 0.004(3) 0.001(3) C23 0.071(3) 0.051(3) 0.053(3) 0.001(2) 0.005(2) -0.003(3) C24 0.047(3) 0.045(2) 0.044(3) -0.0019(19) 0.003(2) -0.004(2) C25 0.157(8) 0.053(4) 0.091(5) 0.015(3) -0.004(5) 0.008(4) C26 0.053(3) 0.044(2) 0.044(3) 0.0033(19) 0.009(2) -0.003(2) C27 0.054(3) 0.051(3) 0.059(3) 0.001(2) 0.005(2) 0.001(2) C28 0.066(3) 0.048(3) 0.061(3) 0.004(2) 0.013(3) 0.012(3) C29 0.090(4) 0.043(3) 0.079(4) -0.002(3) 0.022(3) -0.003(3) C30 0.061(3) 0.053(3) 0.070(4) -0.010(3) 0.013(3) -0.014(3) C31 0.051(3) 0.044(3) 0.054(3) -0.002(2) 0.006(2) -0.003(2) C32 0.080(4) 0.078(5) 0.120(6) -0.007(4) 0.013(4) 0.026(4) C33 0.052(3) 0.059(3) 0.069(4) -0.003(3) 0.012(3) -0.005(2) C34 0.097(5) 0.114(6) 0.080(5) -0.016(4) 0.018(4) -0.055(5) C35 0.115(6) 0.141(8) 0.085(6) -0.045(5) 0.014(5) -0.051(6) C36 0.073(4) 0.081(5) 0.126(7) -0.014(5) 0.016(5) -0.024(4) C37 0.084(5) 0.086(5) 0.132(8) 0.030(5) -0.004(5) -0.037(4) C38 0.073(4) 0.073(4) 0.089(5) 0.013(3) -0.007(3) -0.018(3) C39 0.052(3) 0.068(4) 0.103(5) 0.018(3) -0.005(3) -0.011(3) C40 0.082(5) 0.086(5) 0.143(8) 0.037(5) 0.023(5) 0.003(4) C41 0.084(6) 0.107(7) 0.233(14) 0.076(8) 0.018(7) 0.014(5) C42 0.086(7) 0.147(10) 0.204(13) 0.092(10) -0.041(7) -0.033(7) C43 0.123(8) 0.126(8) 0.115(7) 0.044(6) -0.011(6) -0.046(7) C44 0.094(5) 0.093(5) 0.096(6) 0.018(4) 0.003(4) -0.036(4) C45 0.038(3) 0.072(4) 0.087(4) -0.019(3) 0.009(3) 0.006(3) C46 0.046(3) 0.068(4) 0.108(5) -0.029(4) 0.009(3) 0.001(3) C47 0.061(4) 0.096(5) 0.095(5) -0.011(4) 0.027(4) 0.001(3) C48 0.067(4) 0.110(6) 0.109(6) -0.056(5) 0.027(4) 0.006(4) C49 0.066(4) 0.076(4) 0.117(6) -0.035(4) 0.017(4) 0.013(3) C50 0.054(3) 0.076(4) 0.103(5) -0.017(4) 0.012(3) 0.009(3) F1 0.130(3) 0.085(3) 0.090(3) -0.012(2) 0.048(3) -0.016(2) F2 0.148(4) 0.077(3) 0.115(4) -0.038(2) 0.013(3) -0.013(3) F3 0.089(3) 0.068(2) 0.185(5) -0.011(3) -0.016(3) -0.034(2) F4 0.085(3) 0.117(4) 0.195(5) -0.002(3) 0.059(3) -0.027(3) F5 0.111(3) 0.084(3) 0.135(4) -0.024(2) 0.063(3) -0.015(2) F6 0.085(3) 0.070(2) 0.135(4) -0.014(2) 0.031(2) -0.0106(19) F7 0.116(4) 0.144(4) 0.121(4) -0.013(3) 0.057(3) -0.013(3) F8 0.118(4) 0.161(4) 0.144(5) -0.080(4) 0.042(3) 0.000(3) F9 0.125(4) 0.077(3) 0.180(5) -0.051(3) 0.031(3) 0.013(3) F10 0.120(3) 0.077(3) 0.131(4) 0.001(2) 0.028(3) 0.015(2) _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 As1 C7 1.938(5) . ? As1 C13 1.933(5) . ? As1 C19 1.941(5) . ? As2 C31 1.941(5) . ? As2 C33 1.936(5) . ? As2 C39 1.938(6) . ? Au1 As1 2.3792(5) . ? Au1 C1 2.038(5) . ? Au2 As2 2.3755(6) . ? Au2 C45 2.048(6) . ? C1 C2 1.361(8) . ? C1 C6 1.371(8) . ? C2 C3 1.356(8) . ? C2 F1 1.350(7) . ? C3 C4 1.344(10) . ? C5 C4 1.390(10) . ? C6 C5 1.363(8) . ? C6 F5 1.347(7) . ? C7 C8 1.372(7) . ? C7 C12 1.367(8) . ? C8 C9 1.363(8) . ? C10 C9 1.358(10) . ? C10 C11 1.359(10) . ? C12 C11 1.385(9) . ? C13 C14 1.369(7) . ? C13 C18 1.386(7) . ? C14 C15 1.380(9) . ? C15 C16 1.366(11) . ? C17 C16 1.353(10) . ? C17 C18 1.370(8) . ? C19 C20 1.387(7) . ? C19 C24 1.378(7) . ? C20 C21 1.392(8) . ? C21 C22 1.384(8) . ? C22 C25 1.506(8) . ? C23 C22 1.378(8) . ? C24 C23 1.402(7) . ? C24 C26 1.494(6) . ? C27 C26 1.384(7) . ? C27 C28 1.399(7) . ? C28 C29 1.373(8) . ? C28 C32 1.501(8) . ? C29 C30 1.363(8) . ? C31 C26 1.400(7) . ? C31 C30 1.388(7) . ? C33 C34 1.356(9) . ? C33 C38 1.380(8) . ? C34 C35 1.422(10) . ? C36 C35 1.338(11) . ? C36 C37 1.357(11) . ? C38 C37 1.375(9) . ? C39 C40 1.360(10) . ? C39 C44 1.383(10) . ? C40 C41 1.383(12) . ? C42 C41 1.411(17) . ? C43 C42 1.351(15) . ? C44 C43 1.375(11) . ? C45 C50 1.352(9) . ? C46 C45 1.373(9) . ? C46 C47 1.373(9) . ? C48 C47 1.362(10) . ? C48 C49 1.356(11) . ? C48 F8 1.350(8) . ? C50 C49 1.385(10) . ? C50 F10 1.353(8) . ? F2 C3 1.367(7) . ? F3 C4 1.342(7) . ? F4 C5 1.345(7) . ? F6 C46 1.351(7) . ? F7 C47 1.339(8) . ? F9 C49 1.331(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Au1 As1 173.28(15) . . ? C2 C1 Au1 121.9(4) . . ? C2 C1 C6 114.5(5) . . ? C2 C3 F2 121.1(6) . . ? C3 C2 C1 123.5(6) . . ? C3 C4 C5 118.3(6) . . ? C4 C3 C2 120.9(6) . . ? C4 C3 F2 117.9(6) . . ? C5 C6 C1 124.0(6) . . ? C6 C1 Au1 123.4(4) . . ? C6 C5 C4 118.7(6) . . ? C7 As1 Au1 109.11(15) . . ? C7 As1 C19 104.0(2) . . ? C7 C12 C11 119.5(6) . . ? C8 C7 As1 117.3(4) . . ? C9 C8 C7 120.9(6) . . ? C10 C9 C8 120.3(7) . . ? C10 C11 C12 120.7(7) . . ? C11 C10 C9 119.5(7) . . ? C12 C7 As1 123.6(4) . . ? C12 C7 C8 119.0(5) . . ? C13 As1 Au1 114.71(16) . . ? C13 As1 C7 104.6(2) . . ? C13 As1 C19 105.3(2) . . ? C13 C14 C15 120.0(7) . . ? C14 C13 As1 119.4(4) . . ? C14 C13 C18 119.4(5) . . ? C16 C15 C14 120.4(7) . . ? C16 C17 C18 121.8(7) . . ? C17 C16 C15 119.2(6) . . ? C17 C18 C13 119.1(6) . . ? C18 C13 As1 121.2(4) . . ? C19 As1 Au1 117.95(14) . . ? C19 C20 C21 120.1(5) . . ? C19 C24 C23 118.5(4) . . ? C19 C24 C26 122.0(4) . . ? C20 C19 As1 119.5(4) . . ? C21 C22 C25 121.3(6) . . ? C22 C21 C20 120.8(5) . . ? C22 C23 C24 122.3(5) . . ? C23 C22 C21 118.0(5) . . ? C23 C22 C25 120.6(6) . . ? C23 C24 C26 119.5(4) . . ? C24 C19 As1 120.3(3) . . ? C24 C19 C20 120.2(4) . . ? C26 C27 C28 121.8(5) . . ? C26 C31 As2 119.4(3) . . ? C27 C26 C24 118.8(4) . . ? C27 C26 C31 118.7(4) . . ? C27 C28 C32 119.9(6) . . ? C29 C28 C27 117.6(5) . . ? C29 C28 C32 122.4(5) . . ? C29 C30 C31 120.5(5) . . ? C30 C29 C28 122.0(5) . . ? C30 C31 As2 121.3(4) . . ? C30 C31 C26 119.3(5) . . ? C31 As2 Au2 118.41(15) . . ? C31 C26 C24 122.4(4) . . ? C33 As2 Au2 111.54(17) . . ? C33 As2 C31 104.4(2) . . ? C33 As2 C39 104.6(3) . . ? C33 C34 C35 118.6(7) . . ? C34 C33 As2 121.9(5) . . ? C34 C33 C38 121.0(6) . . ? C35 C36 C37 121.9(7) . . ? C36 C35 C34 119.3(8) . . ? C36 C37 C38 119.8(7) . . ? C37 C38 C33 119.4(7) . . ? C38 C33 As2 117.1(5) . . ? C39 As2 Au2 111.9(2) . . ? C39 As2 C31 104.9(2) . . ? C39 C40 C41 122.8(9) . . ? C40 C39 As2 118.9(6) . . ? C40 C39 C44 119.4(7) . . ? C40 C41 C42 115.2(10) . . ? C42 C43 C44 118.7(11) . . ? C43 C42 C41 123.4(10) . . ? C43 C44 C39 120.4(9) . . ? C44 C39 As2 121.6(6) . . ? C45 Au2 As2 173.74(18) . . ? C45 C46 C47 123.3(6) . . ? C45 C50 C49 123.4(7) . . ? C45 C50 F10 120.5(6) . . ? C46 C45 Au2 123.2(4) . . ? C48 C47 C46 118.7(7) . . ? C48 C49 C50 118.7(7) . . ? C49 C48 C47 120.4(6) . . ? C50 C45 Au2 121.2(5) . . ? C50 C45 C46 115.6(6) . . ? F1 C2 C1 119.4(5) . . ? F1 C2 C3 117.1(6) . . ? F3 C4 C3 122.7(7) . . ? F3 C4 C5 118.9(7) . . ? F4 C5 C4 120.2(6) . . ? F4 C5 C6 121.2(7) . . ? F5 C6 C1 119.9(5) . . ? F5 C6 C5 116.0(5) . . ? F6 C46 C45 120.8(6) . . ? F6 C46 C47 115.9(7) . . ? F7 C47 C46 121.2(7) . . ? F7 C47 C48 120.1(7) . . ? F8 C48 C47 119.5(9) . . ? F8 C48 C49 120.0(7) . . ? F9 C49 C48 120.5(7) . . ? F9 C49 C50 120.9(8) . . ? F10 C50 C49 116.0(6) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.963 _refine_diff_density_min -1.093 _refine_diff_density_rms 0.122 #===END data_compound8 _database_code_depnum_ccdc_archive 'CCDC 290390' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H32 As2' _chemical_formula_weight 638.48 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 19.799(4) _cell_length_b 6.8375(15) _cell_length_c 12.489(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.204(4) _cell_angle_gamma 90.00 _cell_volume 1576.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.345 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 2.144 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS Sheldrick 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5585 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0588 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 28.34 _reflns_number_total 3661 _reflns_number_gt 3002 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.062(16) _refine_ls_number_reflns 3661 _refine_ls_number_parameters 182 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1009 _refine_ls_wR_factor_gt 0.0981 _refine_ls_goodness_of_fit_ref 0.971 _refine_ls_restrained_S_all 0.971 _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 As1 As 0.514532(16) 0.77801(7) 0.66445(2) 0.04866(13) Uani 1 1 d . . . C1 C 0.57448(19) 0.5890(6) 0.6195(3) 0.0448(8) Uani 1 1 d . . . C2 C 0.54040(19) 0.4593(6) 0.5303(3) 0.0429(8) Uani 1 1 d . . . C3 C 0.5807(2) 0.3245(6) 0.4964(3) 0.0517(11) Uani 1 1 d . . . C4 C 0.6562(2) 0.3176(7) 0.5471(3) 0.0553(12) Uani 1 1 d . . . C5 C 0.6896(2) 0.4510(7) 0.6342(3) 0.0572(10) Uani 1 1 d . . . C6 C 0.6504(2) 0.5842(7) 0.6704(3) 0.0527(9) Uani 1 1 d . . . C7 C 0.6988(3) 0.1733(9) 0.5071(5) 0.0874(16) Uani 1 1 d . . . C8 C 0.5894(2) 0.8902(6) 0.8014(3) 0.0502(8) Uani 1 1 d . . . C9 C 0.6009(2) 0.8376(6) 0.9132(3) 0.0600(11) Uani 1 1 d . . . C10 C 0.6522(3) 0.9341(9) 1.0033(4) 0.0772(14) Uani 1 1 d . . . C11 C 0.6945(3) 1.0779(8) 0.9829(4) 0.0715(12) Uani 1 1 d . . . C12 C 0.6840(3) 1.1304(7) 0.8727(4) 0.0702(12) Uani 1 1 d . . . C13 C 0.6303(3) 1.0390(7) 0.7820(4) 0.0640(11) Uani 1 1 d . . . C14 C 0.4697(2) 0.6005(7) 0.7397(3) 0.0523(9) Uani 1 1 d . . . C15 C 0.4007(2) 0.6513(8) 0.7378(5) 0.0757(14) Uani 1 1 d . . . C16 C 0.3662(3) 0.5333(12) 0.7892(6) 0.102(2) Uani 1 1 d . . . C17 C 0.3947(4) 0.3610(11) 0.8386(6) 0.109(2) Uani 1 1 d . . . C18 C 0.4634(4) 0.3045(13) 0.8397(4) 0.0917(18) Uani 1 1 d . . . C19 C 0.4990(3) 0.4260(8) 0.7911(4) 0.0682(12) Uani 1 1 d . . . H3 H 0.5570 0.2361 0.4383 0.062 Uiso 1 1 calc R . . H5 H 0.7398 0.4500 0.6689 0.069 Uiso 1 1 calc R . . H6 H 0.6743 0.6717 0.7289 0.063 Uiso 1 1 calc R . . H7A H 0.6709 0.0560 0.4819 0.131 Uiso 1 1 calc R . . H7B H 0.7431 0.1428 0.5692 0.131 Uiso 1 1 calc R . . H7C H 0.7098 0.2283 0.4446 0.131 Uiso 1 1 calc R . . H9 H 0.5741 0.7366 0.9280 0.072 Uiso 1 1 calc R . . H10 H 0.6582 0.9013 1.0784 0.093 Uiso 1 1 calc R . . H11 H 0.7301 1.1392 1.0439 0.086 Uiso 1 1 calc R . . H12 H 0.7126 1.2270 0.8583 0.084 Uiso 1 1 calc R . . H13 H 0.6219 1.0791 0.7072 0.077 Uiso 1 1 calc R . . H15 H 0.3786 0.7655 0.7014 0.091 Uiso 1 1 calc R . . H16 H 0.3215 0.5722 0.7906 0.123 Uiso 1 1 calc R . . H17 H 0.3693 0.2813 0.8712 0.131 Uiso 1 1 calc R . . H18 H 0.4841 0.1867 0.8729 0.110 Uiso 1 1 calc R . . H19 H 0.5447 0.3899 0.7928 0.082 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 As1 0.04836(19) 0.0502(2) 0.04438(17) 0.0031(2) 0.01312(12) 0.0110(2) C1 0.0440(19) 0.048(2) 0.0447(17) 0.0031(15) 0.0189(15) 0.0035(16) C2 0.0417(19) 0.046(2) 0.0428(16) 0.0037(14) 0.0168(15) -0.0007(15) C3 0.0504(19) 0.056(3) 0.0519(18) -0.0034(15) 0.0226(16) 0.0013(16) C4 0.053(2) 0.061(4) 0.0589(19) 0.0054(18) 0.0281(17) 0.0080(19) C5 0.0393(19) 0.069(3) 0.063(2) 0.007(2) 0.0185(17) 0.0078(18) C6 0.045(2) 0.060(2) 0.0492(18) 0.0005(17) 0.0124(16) -0.0031(18) C7 0.075(3) 0.094(4) 0.100(4) -0.006(3) 0.040(3) 0.024(3) C8 0.053(2) 0.048(2) 0.0479(18) 0.0008(15) 0.0157(16) 0.0120(16) C9 0.062(2) 0.061(3) 0.055(2) 0.0003(16) 0.0186(18) 0.0018(18) C10 0.090(4) 0.085(4) 0.047(2) 0.001(2) 0.014(2) 0.010(3) C11 0.069(3) 0.064(3) 0.069(3) -0.012(2) 0.010(2) 0.002(2) C12 0.063(3) 0.062(3) 0.080(3) -0.006(2) 0.019(2) -0.008(2) C13 0.074(3) 0.065(3) 0.054(2) 0.0044(19) 0.024(2) 0.002(2) C14 0.049(2) 0.059(2) 0.0503(19) -0.0010(18) 0.0195(16) 0.0119(18) C15 0.053(3) 0.091(4) 0.090(3) -0.003(3) 0.033(2) 0.014(2) C16 0.083(4) 0.118(6) 0.133(5) -0.003(4) 0.072(4) -0.004(4) C17 0.128(6) 0.115(6) 0.115(5) 0.007(4) 0.081(5) -0.026(4) C18 0.132(4) 0.075(5) 0.089(3) 0.015(3) 0.065(3) 0.008(4) C19 0.069(3) 0.074(3) 0.070(3) 0.010(2) 0.035(2) 0.013(2) _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 As1 C8 1.969(4) . ? As1 C14 1.936(4) . ? C1 As1 1.969(4) . ? C2 C1 1.393(5) . ? C2 C2 1.502(7) 2_656 ? C2 C3 1.382(5) . ? C4 C3 1.397(5) . ? C4 C5 1.390(6) . ? C4 C7 1.496(6) . ? C6 C1 1.405(5) . ? C6 C5 1.375(6) . ? C8 C9 1.379(5) . ? C8 C13 1.375(6) . ? C9 C10 1.380(7) . ? C11 C10 1.374(8) . ? C12 C11 1.363(7) . ? C12 C13 1.390(6) . ? C15 C14 1.400(6) . ? C15 C16 1.359(8) . ? C16 C17 1.354(9) . ? C18 C17 1.408(9) . ? C19 C14 1.380(7) . ? C19 C18 1.366(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 C2 C2 121.5(3) . 2_656 ? C2 C1 As1 118.6(3) . . ? C2 C1 C6 118.5(3) . . ? C2 C3 C4 121.7(4) . . ? C3 C2 C1 120.2(3) . . ? C3 C2 C2 118.3(3) . 2_656 ? C3 C4 C7 120.7(4) . . ? C5 C4 C3 117.4(4) . . ? C5 C4 C7 121.9(4) . . ? C5 C6 C1 120.3(4) . . ? C6 C1 As1 122.9(3) . . ? C6 C5 C4 121.8(4) . . ? C8 As1 C1 99.30(15) . . ? C8 C9 C10 120.3(4) . . ? C8 C13 C12 121.0(4) . . ? C9 C8 As1 125.1(3) . . ? C11 C10 C9 120.6(4) . . ? C11 C12 C13 119.8(5) . . ? C12 C11 C10 119.7(5) . . ? C13 C8 As1 116.2(3) . . ? C13 C8 C9 118.6(4) . . ? C14 As1 C1 99.01(17) . . ? C14 As1 C8 98.97(17) . . ? C15 C14 As1 116.9(3) . . ? C16 C15 C14 119.9(5) . . ? C16 C17 C18 119.1(6) . . ? C17 C16 C15 122.2(6) . . ? C18 C19 C14 122.3(5) . . ? C19 C14 As1 125.3(3) . . ? C19 C14 C15 117.8(4) . . ? C19 C18 C17 118.7(7) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.058 _refine_diff_density_min -0.483 _refine_diff_density_rms 0.093 #===END data_compound9 _database_code_depnum_ccdc_archive 'CCDC 290391' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H32 As2 Au2' _chemical_formula_weight 1032.41 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' 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 C2/c 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 23.051(7) _cell_length_b 8.910(3) _cell_length_c 18.718(6) _cell_angle_alpha 90.00 _cell_angle_beta 121.310(13) _cell_angle_gamma 90.00 _cell_volume 3284.4(18) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.088 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 10.948 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS Sheldrick 1996' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5526 _diffrn_reflns_av_R_equivalents 0.1598 _diffrn_reflns_av_sigmaI/netI 0.1125 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 28.28 _reflns_number_total 3848 _reflns_number_gt 3022 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0896P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3848 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0668 _refine_ls_R_factor_gt 0.0591 _refine_ls_wR_factor_ref 0.1463 _refine_ls_wR_factor_gt 0.1419 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.979 _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 As1 As 0.11760(3) 0.92015(8) 0.31588(4) 0.0442(2) Uani 1 1 d . . . Au1 Au 0.020993(14) 1.00722(3) 0.187673(16) 0.04377(15) Uani 1 1 d . . . C1 C 0.0707(4) 1.0563(9) 0.4161(4) 0.0473(16) Uani 1 1 d . . . C2 C 0.1304(4) 1.0166(8) 0.4157(5) 0.0467(17) Uani 1 1 d . . . C3 C 0.1954(5) 1.0430(12) 0.4833(6) 0.063(2) Uani 1 1 d . . . C4 C 0.2027(5) 1.1158(14) 0.5523(5) 0.076(3) Uani 1 1 d . . . C5 C 0.1459(5) 1.1595(13) 0.5550(5) 0.071(3) Uani 1 1 d . . . C6 C 0.0798(4) 1.1323(10) 0.4864(4) 0.0535(18) Uani 1 1 d . . . C7 C 0.0199(5) 1.1903(14) 0.4892(6) 0.074(3) Uani 1 1 d . . . C8 C 0.1036(4) 0.7126(9) 0.3298(5) 0.0536(18) Uani 1 1 d . . . C9 C 0.0844(6) 0.6161(11) 0.2620(8) 0.079(3) Uani 1 1 d . . . C10 C 0.0802(8) 0.4656(16) 0.2739(13) 0.111(5) Uani 1 1 d . . . C11 C 0.0952(9) 0.4132(16) 0.3497(17) 0.133(7) Uani 1 1 d . . . C12 C 0.1131(9) 0.5043(18) 0.4134(13) 0.112(7) Uani 1 1 d . . . C13 C 0.1171(5) 0.6523(14) 0.4038(6) 0.082(3) Uani 1 1 d . . . C14 C 0.2068(4) 0.9134(9) 0.3285(4) 0.0507(17) Uani 1 1 d . . . C15 C 0.2234(6) 1.0173(11) 0.2879(7) 0.067(3) Uani 1 1 d . . . C16 C 0.2852(7) 1.0121(15) 0.2941(8) 0.085(4) Uani 1 1 d . . . C17 C 0.3300(5) 0.8998(16) 0.3385(6) 0.080(3) Uani 1 1 d . . . C18 C 0.3143(4) 0.7959(15) 0.3781(5) 0.078(3) Uani 1 1 d . . . C19 C 0.2516(4) 0.8004(12) 0.3721(5) 0.064(2) Uani 1 1 d . . . H3 H 0.2333 1.0119 0.4819 0.076 Uiso 1 1 calc R . . H4 H 0.2459 1.1359 0.5975 0.091 Uiso 1 1 calc R . . H5 H 0.1516 1.2072 0.6024 0.086 Uiso 1 1 calc R . . H7A H -0.0213 1.1535 0.4417 0.111 Uiso 1 1 calc R . . H7B H 0.0199 1.2980 0.4882 0.111 Uiso 1 1 calc R . . H7C H 0.0227 1.1565 0.5396 0.111 Uiso 1 1 calc R . . H9 H 0.0747 0.6530 0.2104 0.095 Uiso 1 1 calc R . . H10 H 0.0670 0.3991 0.2298 0.133 Uiso 1 1 calc R . . H11 H 0.0927 0.3106 0.3569 0.160 Uiso 1 1 calc R . . H12 H 0.1229 0.4660 0.4647 0.134 Uiso 1 1 calc R . . H13 H 0.1294 0.7157 0.4490 0.098 Uiso 1 1 calc R . . H15 H 0.1924 1.0919 0.2560 0.080 Uiso 1 1 calc R . . H16 H 0.2966 1.0850 0.2680 0.102 Uiso 1 1 calc R . . H17 H 0.3715 0.8950 0.3415 0.096 Uiso 1 1 calc R . . H18 H 0.3454 0.7211 0.4094 0.094 Uiso 1 1 calc R . . H19 H 0.2402 0.7265 0.3978 0.077 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 As1 0.0412(4) 0.0401(4) 0.0458(4) 0.0065(3) 0.0188(3) 0.0031(3) Au1 0.0441(2) 0.0435(2) 0.0411(2) 0.00307(10) 0.02033(16) 0.00404(10) C1 0.052(4) 0.040(4) 0.045(4) 0.003(3) 0.022(3) 0.001(3) C2 0.047(4) 0.047(4) 0.036(4) 0.006(3) 0.014(3) -0.001(3) C3 0.047(4) 0.060(5) 0.063(5) 0.001(4) 0.015(4) 0.003(4) C4 0.059(5) 0.092(8) 0.043(4) 0.002(5) 0.003(4) -0.002(5) C5 0.072(5) 0.083(7) 0.043(4) -0.013(4) 0.018(4) -0.010(5) C6 0.064(5) 0.044(4) 0.045(4) 0.000(3) 0.024(4) -0.005(4) C7 0.082(6) 0.081(7) 0.068(5) -0.017(5) 0.046(5) -0.005(6) C8 0.040(3) 0.041(4) 0.078(5) 0.015(4) 0.029(4) 0.004(3) C9 0.095(7) 0.051(5) 0.128(8) -0.017(6) 0.084(7) -0.012(5) C10 0.128(11) 0.059(6) 0.213(18) -0.023(10) 0.136(13) -0.015(8) C11 0.125(12) 0.054(8) 0.27(2) 0.041(12) 0.141(15) 0.011(8) C12 0.087(10) 0.101(13) 0.128(13) 0.055(10) 0.041(10) -0.002(8) C13 0.076(6) 0.072(7) 0.080(6) 0.020(5) 0.028(5) -0.012(6) C14 0.045(4) 0.055(5) 0.049(4) 0.002(3) 0.022(3) -0.003(3) C15 0.060(5) 0.076(7) 0.063(6) 0.013(4) 0.031(5) -0.009(4) C16 0.072(7) 0.117(12) 0.079(7) 0.018(6) 0.048(6) -0.008(6) C17 0.052(5) 0.120(11) 0.071(6) -0.006(6) 0.033(5) -0.004(6) C18 0.046(4) 0.111(9) 0.072(5) -0.002(6) 0.027(4) 0.012(5) C19 0.053(4) 0.073(6) 0.070(5) 0.018(5) 0.033(4) 0.007(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 As1 C2 1.935(8) . ? As1 C8 1.918(8) . ? As1 C14 1.944(8) . ? Au1 As1 2.4011(10) . ? Au1 Au1 2.9543(10) 2 ? Au1 C1 2.040(7) 2 ? C1 Au1 2.040(7) 2 ? C1 C2 1.425(12) . ? C2 C3 1.389(12) . ? C3 C4 1.375(15) . ? C5 C4 1.390(14) . ? C5 C6 1.412(11) . ? C6 C1 1.396(11) . ? C6 C7 1.502(13) . ? C8 C9 1.402(13) . ? C8 C13 1.362(12) . ? C9 C10 1.370(17) . ? C11 C10 1.36(3) . ? C11 C12 1.32(2) . ? C13 C12 1.341(18) . ? C14 C15 1.372(12) . ? C14 C19 1.368(12) . ? C15 C16 1.370(16) . ? C16 C17 1.367(17) . ? C18 C17 1.347(16) . ? C19 C18 1.390(12) . ? 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 As1 Au1 Au1 74.03(3) . 2 ? C1 Au1 As1 169.9(2) 2 . ? C1 Au1 Au1 98.6(2) 2 2 ? C1 C2 As1 116.9(6) . . ? C1 C6 C5 120.2(8) . . ? C1 C6 C7 120.6(7) . . ? C2 As1 Au1 114.7(2) . . ? C2 As1 C14 106.0(3) . . ? C2 C1 Au1 117.9(6) . 2 ? C3 C2 As1 120.4(7) . . ? C3 C2 C1 122.7(8) . . ? C3 C4 C5 120.5(8) . . ? C4 C3 C2 118.9(9) . . ? C4 C5 C6 120.7(8) . . ? C5 C6 C7 119.2(8) . . ? C6 C1 Au1 125.2(6) . 2 ? C6 C1 C2 116.9(7) . . ? C8 As1 Au1 108.3(2) . . ? C8 As1 C2 104.4(3) . . ? C8 As1 C14 101.3(3) . . ? C9 C8 As1 117.7(7) . . ? C10 C9 C8 117.9(13) . . ? C11 C10 C9 120.4(15) . . ? C11 C12 C13 119.7(15) . . ? C12 C11 C10 121.6(13) . . ? C12 C13 C8 121.9(14) . . ? C13 C8 As1 123.6(8) . . ? C13 C8 C9 118.5(9) . . ? C14 As1 Au1 120.3(2) . . ? C14 C19 C18 120.0(9) . . ? C15 C14 As1 119.5(7) . . ? C16 C15 C14 120.5(10) . . ? C17 C16 C15 120.0(11) . . ? C17 C18 C19 120.1(10) . . ? C18 C17 C16 120.2(9) . . ? C19 C14 As1 121.3(6) . . ? C19 C14 C15 119.0(8) . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 3.415 _refine_diff_density_min -3.283 _refine_diff_density_rms 0.351 #===END data_compound10 _database_code_depnum_ccdc_archive 'CCDC 290392' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H32 As2 Au2 Cl2' _chemical_formula_weight 1103.31 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' 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 C2/c 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 25.691(2) _cell_length_b 20.4189(18) _cell_length_c 19.0832(17) _cell_angle_alpha 90.00 _cell_angle_beta 130.1910(10) _cell_angle_gamma 90.00 _cell_volume 7647.0(12) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.062 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.917 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4144 _exptl_absorpt_coefficient_mu 9.547 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS Sheldrick 1996' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27580 _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_sigmaI/netI 0.0653 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 28.43 _reflns_number_total 9609 _reflns_number_gt 6032 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9609 _refine_ls_number_parameters 399 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0915 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1043 _refine_ls_wR_factor_gt 0.0859 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.009 _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 As1 As 0.13331(4) 0.14591(3) 0.01717(5) 0.03836(17) Uani 1 1 d . . . As2 As 0.33883(4) -0.04691(4) 0.20479(5) 0.04524(19) Uani 1 1 d . . . Au1 Au 0.180815(13) 0.033674(12) 0.070534(17) 0.03410(8) Uani 1 1 d . . . Au2 Au 0.337536(16) 0.060703(14) 0.24433(2) 0.04752(10) Uani 1 1 d . . . C1 C 0.1663(3) 0.0744(3) 0.1562(5) 0.0376(16) Uani 1 1 d . . . C2 C 0.1359(4) 0.1353(3) 0.1189(4) 0.0421(17) Uani 1 1 d . . . C3 C 0.1169(4) 0.1757(4) 0.1568(6) 0.059(2) Uani 1 1 d . . . C4 C 0.1292(5) 0.1535(5) 0.2360(6) 0.074(3) Uani 1 1 d . . . C5 C 0.1611(4) 0.0949(4) 0.2738(6) 0.060(2) Uani 1 1 d . . . C6 C 0.1802(4) 0.0532(3) 0.2354(5) 0.0432(17) Uani 1 1 d . . . C7 C 0.2166(4) -0.0092(4) 0.2838(5) 0.054(2) Uani 1 1 d . . . C8 C 0.1945(4) -0.0640(3) 0.1096(4) 0.0414(17) Uani 1 1 d . . . C9 C 0.1368(4) -0.1003(4) 0.0761(5) 0.052(2) Uani 1 1 d . . . C10 C 0.1447(5) -0.1678(4) 0.0940(6) 0.064(2) Uani 1 1 d . . . C11 C 0.2065(5) -0.1988(4) 0.1409(7) 0.073(3) Uani 1 1 d . . . C12 C 0.2617(4) -0.1628(4) 0.1717(6) 0.060(2) Uani 1 1 d . . . C13 C 0.2569(3) -0.0951(3) 0.1558(5) 0.0419(17) Uani 1 1 d . . . C14 C 0.0676(4) -0.0689(4) 0.0234(7) 0.074(3) Uani 1 1 d . . . C15 C 0.3553(5) -0.0548(5) 0.1189(6) 0.062(2) Uani 1 1 d . . . C16 C 0.3252(5) -0.1008(6) 0.0534(7) 0.088(3) Uani 1 1 d . . . C17 C 0.3368(7) -0.1037(8) -0.0084(8) 0.122(6) Uani 1 1 d . . . C18 C 0.3833(9) -0.0592(9) 0.0028(12) 0.144(8) Uani 1 1 d . . . C19 C 0.4150(8) -0.0116(8) 0.0706(12) 0.130(6) Uani 1 1 d . . . C20 C 0.3994(6) -0.0104(6) 0.1275(8) 0.090(3) Uani 1 1 d . . . C21 C 0.4107(4) -0.0993(4) 0.3103(6) 0.054(2) Uani 1 1 d . . . C22 C 0.4195(5) -0.0932(5) 0.3885(6) 0.081(3) Uani 1 1 d . . . C23 C 0.4691(6) -0.1306(6) 0.4645(7) 0.100(4) Uani 1 1 d . . . C24 C 0.5058(5) -0.1749(6) 0.4592(8) 0.091(4) Uani 1 1 d . . . C25 C 0.4965(5) -0.1821(5) 0.3803(8) 0.089(3) Uani 1 1 d . . . C26 C 0.4479(5) -0.1433(4) 0.3035(7) 0.074(3) Uani 1 1 d . . . C27 C 0.0394(4) 0.1430(4) -0.0944(5) 0.0417(17) Uani 1 1 d . . . C28 C -0.0034(4) 0.1963(4) -0.1273(6) 0.063(2) Uani 1 1 d . . . C29 C -0.0704(5) 0.1906(6) -0.2057(7) 0.082(3) Uani 1 1 d . . . C30 C -0.0953(4) 0.1321(6) -0.2505(6) 0.077(3) Uani 1 1 d . . . C31 C -0.0537(4) 0.0786(5) -0.2190(6) 0.073(3) Uani 1 1 d . . . C32 C 0.0148(4) 0.0838(4) -0.1394(5) 0.054(2) Uani 1 1 d . . . C33 C 0.1651(4) 0.2320(3) 0.0205(5) 0.0423(17) Uani 1 1 d . . . C34 C 0.1986(4) 0.2699(4) 0.0977(6) 0.064(2) Uani 1 1 d . . . C35 C 0.2186(5) 0.3324(5) 0.0979(7) 0.077(3) Uani 1 1 d . . . C36 C 0.2064(5) 0.3566(5) 0.0216(8) 0.084(3) Uani 1 1 d . . . C37 C 0.1735(6) 0.3185(5) -0.0552(8) 0.095(4) Uani 1 1 d . . . C38 C 0.1515(5) 0.2552(4) -0.0564(6) 0.072(3) Uani 1 1 d . . . Cl1 Cl 0.18551(11) 0.00229(10) -0.04372(13) 0.0547(5) Uani 1 1 d . . . Cl2 Cl 0.34098(15) 0.16461(11) 0.28899(18) 0.0856(8) Uani 1 1 d . . . H3 H 0.0968 0.2162 0.1310 0.071 Uiso 1 1 calc R . . H4 H 0.1157 0.1785 0.2625 0.089 Uiso 1 1 calc R . . H5 H 0.1707 0.0819 0.3278 0.072 Uiso 1 1 calc R . . H7A H 0.1864 -0.0456 0.2500 0.081 Uiso 1 1 calc R . . H7B H 0.2308 -0.0087 0.3442 0.081 Uiso 1 1 calc R . . H7C H 0.2558 -0.0135 0.2881 0.081 Uiso 1 1 calc R . . H10 H 0.1068 -0.1925 0.0735 0.077 Uiso 1 1 calc R . . H11 H 0.2102 -0.2437 0.1511 0.088 Uiso 1 1 calc R . . H12 H 0.3038 -0.1833 0.2043 0.072 Uiso 1 1 calc R . . H14A H 0.0677 -0.0401 0.0632 0.111 Uiso 1 1 calc R . . H14B H 0.0338 -0.1023 0.0007 0.111 Uiso 1 1 calc R . . H14C H 0.0572 -0.0444 -0.0272 0.111 Uiso 1 1 calc R . . H16 H 0.2962 -0.1311 0.0491 0.106 Uiso 1 1 calc R . . H17 H 0.3145 -0.1343 -0.0558 0.146 Uiso 1 1 calc R . . H18 H 0.3931 -0.0617 -0.0363 0.173 Uiso 1 1 calc R . . H19 H 0.4454 0.0181 0.0775 0.156 Uiso 1 1 calc R . . H20 H 0.4192 0.0214 0.1730 0.108 Uiso 1 1 calc R . . H22 H 0.3926 -0.0644 0.3909 0.098 Uiso 1 1 calc R . . H23 H 0.4772 -0.1252 0.5192 0.120 Uiso 1 1 calc R . . H24 H 0.5378 -0.2008 0.5099 0.109 Uiso 1 1 calc R . . H25 H 0.5222 -0.2124 0.3776 0.106 Uiso 1 1 calc R . . H26 H 0.4410 -0.1473 0.2495 0.089 Uiso 1 1 calc R . . H28 H 0.0130 0.2361 -0.0964 0.076 Uiso 1 1 calc R . . H29 H -0.0990 0.2269 -0.2284 0.098 Uiso 1 1 calc R . . H30 H -0.1410 0.1286 -0.3028 0.092 Uiso 1 1 calc R . . H31 H -0.0707 0.0390 -0.2503 0.088 Uiso 1 1 calc R . . H32 H 0.0434 0.0476 -0.1172 0.065 Uiso 1 1 calc R . . H34 H 0.2079 0.2533 0.1501 0.077 Uiso 1 1 calc R . . H35 H 0.2405 0.3584 0.1501 0.093 Uiso 1 1 calc R . . H36 H 0.2203 0.3987 0.0220 0.101 Uiso 1 1 calc R . . H37 H 0.1658 0.3346 -0.1069 0.114 Uiso 1 1 calc R . . H38 H 0.1280 0.2297 -0.1091 0.087 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 As1 0.0485(4) 0.0290(4) 0.0350(4) 0.0030(3) 0.0258(3) 0.0020(3) As2 0.0492(5) 0.0376(4) 0.0481(5) 0.0033(3) 0.0310(4) 0.0066(3) Au1 0.04124(15) 0.02759(14) 0.03392(14) 0.00103(11) 0.02446(12) -0.00044(11) Au2 0.0548(2) 0.03483(17) 0.04962(19) -0.00006(13) 0.03218(16) -0.00314(13) C1 0.047(4) 0.033(4) 0.039(4) 0.000(3) 0.031(3) 0.001(3) C2 0.052(4) 0.040(4) 0.034(4) 0.006(3) 0.028(4) 0.002(3) C3 0.081(6) 0.037(5) 0.064(5) 0.006(4) 0.049(5) 0.014(4) C4 0.114(8) 0.066(6) 0.083(7) 0.007(5) 0.082(7) 0.025(6) C5 0.090(6) 0.054(6) 0.059(5) 0.010(4) 0.058(5) 0.012(5) C6 0.055(5) 0.039(4) 0.041(4) 0.003(3) 0.033(4) 0.001(3) C7 0.076(6) 0.047(5) 0.051(5) 0.013(4) 0.046(5) 0.008(4) C8 0.061(5) 0.030(4) 0.029(3) -0.005(3) 0.027(4) -0.006(3) C9 0.068(5) 0.035(4) 0.053(5) -0.006(4) 0.039(4) -0.011(4) C10 0.082(6) 0.042(5) 0.068(6) -0.015(4) 0.048(5) -0.032(5) C11 0.089(7) 0.029(5) 0.087(7) 0.006(5) 0.050(6) -0.003(5) C12 0.057(5) 0.035(5) 0.069(6) 0.000(4) 0.033(5) 0.005(4) C13 0.052(4) 0.032(4) 0.048(4) 0.000(3) 0.035(4) -0.001(3) C14 0.060(6) 0.067(7) 0.088(7) -0.003(5) 0.045(6) -0.014(5) C15 0.064(6) 0.068(6) 0.058(5) 0.011(5) 0.042(5) 0.024(5) C16 0.077(7) 0.110(9) 0.074(7) -0.007(6) 0.047(6) 0.030(6) C17 0.130(12) 0.170(16) 0.073(8) 0.009(9) 0.070(9) 0.065(11) C18 0.183(18) 0.18(2) 0.131(13) 0.088(13) 0.131(15) 0.125(16) C19 0.177(15) 0.125(13) 0.192(16) 0.075(12) 0.166(15) 0.062(11) C20 0.110(9) 0.094(9) 0.116(9) 0.033(7) 0.095(8) 0.021(7) C21 0.046(5) 0.044(5) 0.057(5) 0.006(4) 0.026(4) 0.004(4) C22 0.097(7) 0.080(7) 0.055(6) 0.021(5) 0.044(6) 0.030(6) C23 0.113(9) 0.102(10) 0.065(7) 0.026(6) 0.048(7) 0.026(7) C24 0.069(7) 0.076(8) 0.078(8) 0.025(6) 0.025(6) 0.000(6) C25 0.054(6) 0.066(7) 0.110(9) 0.017(7) 0.037(6) 0.011(5) C26 0.069(6) 0.060(6) 0.081(7) 0.015(5) 0.043(6) 0.021(5) C27 0.041(4) 0.044(4) 0.041(4) 0.006(3) 0.026(4) 0.005(3) C28 0.069(6) 0.056(6) 0.055(5) 0.010(4) 0.035(5) 0.017(4) C29 0.068(7) 0.101(9) 0.066(7) 0.029(6) 0.039(6) 0.037(6) C30 0.039(5) 0.120(10) 0.055(6) 0.016(6) 0.023(5) 0.000(6) C31 0.052(5) 0.093(8) 0.052(5) 0.003(5) 0.024(5) -0.006(5) C32 0.044(4) 0.056(5) 0.047(5) -0.009(4) 0.023(4) 0.001(4) C33 0.050(4) 0.027(4) 0.047(4) 0.003(3) 0.030(4) 0.000(3) C34 0.069(6) 0.047(5) 0.065(6) -0.006(4) 0.038(5) -0.012(4) C35 0.086(7) 0.055(6) 0.084(7) -0.015(5) 0.052(6) -0.020(5) C36 0.080(7) 0.039(5) 0.111(9) 0.002(6) 0.051(7) -0.014(5) C37 0.112(9) 0.077(8) 0.091(8) 0.028(6) 0.062(7) -0.019(7) C38 0.107(8) 0.053(6) 0.064(6) -0.006(5) 0.058(6) -0.020(5) Cl1 0.0727(14) 0.0553(13) 0.0498(11) 0.0043(9) 0.0458(11) 0.0106(10) Cl2 0.118(2) 0.0391(13) 0.0857(18) -0.0110(12) 0.0596(17) -0.0062(13) _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 As1 C2 1.912(7) . ? As1 C27 1.930(7) . ? As1 C33 1.922(7) . ? As2 C13 1.933(7) . ? As2 C15 1.945(9) . ? As2 C21 1.952(8) . ? Au1 As1 2.4849(7) . ? Au1 Au2 3.2063(5) . ? Au1 C1 2.071(7) . ? Au1 C8 2.077(7) . ? Au1 Cl1 2.3491(18) . ? Au2 As2 2.3305(8) . ? Au2 Cl2 2.267(2) . ? C1 C2 1.395(9) . ? C1 C6 1.379(9) . ? C2 C3 1.378(10) . ? C3 C4 1.405(11) . ? C4 C5 1.363(11) . ? C6 C5 1.403(11) . ? C6 C7 1.495(10) . ? C8 C9 1.390(10) . ? C8 C13 1.388(10) . ? C9 C10 1.404(11) . ? C9 C14 1.508(11) . ? C10 C11 1.373(12) . ? C12 C11 1.349(11) . ? C13 C12 1.404(10) . ? C15 C16 1.341(13) . ? C15 C20 1.375(13) . ? C16 C17 1.394(15) . ? C17 C18 1.40(2) . ? C18 C19 1.39(2) . ? C20 C19 1.380(15) . ? C21 C22 1.365(12) . ? C21 C26 1.377(11) . ? C22 C23 1.387(13) . ? C24 C23 1.357(15) . ? C25 C24 1.373(15) . ? C26 C25 1.403(13) . ? C27 C28 1.377(10) . ? C27 C32 1.378(10) . ? C28 C29 1.376(12) . ? C30 C29 1.364(14) . ? C31 C30 1.368(13) . ? C32 C31 1.402(11) . ? C33 C34 1.369(11) . ? C33 C38 1.356(11) . ? C34 C35 1.377(12) . ? C35 C36 1.368(14) . ? C37 C36 1.366(14) . ? C38 C37 1.405(12) . ? 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 As1 Au1 Au2 102.824(19) . . ? As2 Au2 Au1 76.91(2) . . ? C1 Au1 As1 70.26(19) . . ? C1 Au1 Au2 81.97(19) . . ? C1 Au1 C8 100.2(3) . . ? C1 Au1 Cl1 170.17(19) . . ? C1 C2 As1 105.1(5) . . ? C1 C6 C5 116.8(7) . . ? C1 C6 C7 124.2(7) . . ? C2 As1 Au1 78.1(2) . . ? C2 As1 C27 108.4(3) . . ? C2 As1 C33 109.6(3) . . ? C2 C1 Au1 106.4(5) . . ? C2 C3 C4 117.4(7) . . ? C3 C2 As1 132.3(6) . . ? C3 C2 C1 122.5(7) . . ? C4 C5 C6 123.3(8) . . ? C5 C4 C3 119.6(8) . . ? C5 C6 C7 119.0(7) . . ? C6 C1 Au1 133.4(5) . . ? C6 C1 C2 120.2(6) . . ? C8 Au1 As1 163.1(2) . . ? C8 Au1 Au2 89.2(2) . . ? C8 Au1 Cl1 88.46(19) . . ? C8 C13 As2 121.7(5) . . ? C8 C13 C12 119.5(7) . . ? C8 C9 C10 117.8(8) . . ? C8 C9 C14 121.9(7) . . ? C9 C8 Au1 117.6(6) . . ? C10 C9 C14 120.2(7) . . ? C11 C10 C9 122.5(8) . . ? C11 C12 C13 121.4(8) . . ? C12 C11 C10 118.7(8) . . ? C12 C13 As2 118.7(5) . . ? C13 As2 Au2 113.5(2) . . ? C13 As2 C15 108.2(4) . . ? C13 As2 C21 103.3(3) . . ? C13 C8 Au1 121.8(5) . . ? C13 C8 C9 120.0(7) . . ? C15 As2 Au2 114.0(3) . . ? C15 As2 C21 104.4(4) . . ? C15 C16 C17 120.6(13) . . ? C15 C20 C19 122.0(13) . . ? C16 C15 As2 122.3(8) . . ? C16 C15 C20 120.6(10) . . ? C16 C17 C18 118.0(15) . . ? C19 C18 C17 121.7(14) . . ? C20 C15 As2 117.1(8) . . ? C20 C19 C18 117.0(15) . . ? C21 As2 Au2 112.6(2) . . ? C21 C22 C23 119.1(10) . . ? C21 C26 C25 118.4(10) . . ? C22 C21 As2 117.2(7) . . ? C22 C21 C26 121.8(8) . . ? C23 C24 C25 121.1(10) . . ? C24 C23 C22 120.2(11) . . ? C24 C25 C26 119.5(11) . . ? C26 C21 As2 120.9(7) . . ? C27 As1 Au1 110.9(2) . . ? C27 C32 C31 119.5(8) . . ? C28 C27 As1 122.7(6) . . ? C28 C27 C32 119.9(7) . . ? C29 C28 C27 120.0(9) . . ? C29 C30 C31 120.4(9) . . ? C30 C29 C28 120.5(9) . . ? C30 C31 C32 119.7(10) . . ? C32 C27 As1 117.3(5) . . ? C33 As1 Au1 138.1(2) . . ? C33 As1 C27 105.5(3) . . ? C33 C34 C35 120.1(9) . . ? C33 C38 C37 119.0(9) . . ? C34 C33 As1 120.7(6) . . ? C36 C35 C34 120.2(9) . . ? C36 C37 C38 120.2(9) . . ? C37 C36 C35 119.8(9) . . ? C38 C33 As1 118.5(6) . . ? C38 C33 C34 120.8(7) . . ? Cl1 Au1 As1 100.20(5) . . ? Cl1 Au1 Au2 102.99(5) . . ? Cl2 Au2 As2 177.42(8) . . ? Cl2 Au2 Au1 105.57(7) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.43 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.945 _refine_diff_density_min -0.706 _refine_diff_density_rms 0.193 #===END data_compound11 _database_code_depnum_ccdc_archive 'CCDC 290393' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H32 As2 Au2 Cl2' _chemical_formula_weight 1103.31 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' 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.0921(12) _cell_length_b 15.991(2) _cell_length_c 24.704(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.868(3) _cell_angle_gamma 90.00 _cell_volume 3558.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.060 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2072 _exptl_absorpt_coefficient_mu 10.259 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS Sheldrick 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25596 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.0738 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 28.30 _reflns_number_total 8775 _reflns_number_gt 5833 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0779P)^2^+8.5327P] 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 8775 _refine_ls_number_parameters 399 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0957 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1642 _refine_ls_wR_factor_gt 0.1483 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.36361(11) 0.09838(6) 0.10781(4) 0.0454(2) Uani 1 1 d . . . As2 As 0.30499(13) 0.41903(7) 0.13472(5) 0.0550(3) Uani 1 1 d . . . Au1 Au 0.25335(5) 0.15919(3) 0.177928(16) 0.05430(14) Uani 1 1 d . . . Au2 Au 0.24746(4) 0.29601(3) 0.079031(16) 0.05077(14) Uani 1 1 d . . . C1 C 0.5639(11) 0.1330(6) 0.0998(4) 0.050(2) Uani 1 1 d . . . C2 C 0.6683(14) 0.1428(10) 0.1446(6) 0.087(4) Uani 1 1 d . . . C3 C 0.8088(16) 0.1603(10) 0.1395(8) 0.101(5) Uani 1 1 d . . . C4 C 0.8519(17) 0.1770(10) 0.0933(9) 0.101(5) Uani 1 1 d . . . C5 C 0.7498(18) 0.1678(8) 0.0449(8) 0.092(5) Uani 1 1 d . . . C6 C 0.6080(14) 0.1462(7) 0.0496(5) 0.065(3) Uani 1 1 d . . . C7 C 0.3859(11) -0.0212(7) 0.1156(4) 0.053(3) Uani 1 1 d . . . C8 C 0.4949(14) -0.0650(7) 0.0930(4) 0.062(3) Uani 1 1 d . . . C9 C 0.5067(17) -0.1499(8) 0.1001(6) 0.079(4) Uani 1 1 d . . . C10 C 0.4099(17) -0.1912(9) 0.1310(6) 0.086(4) Uani 1 1 d . . . C11 C 0.3036(16) -0.1506(9) 0.1513(6) 0.079(4) Uani 1 1 d . . . C12 C 0.2922(14) -0.0634(8) 0.1463(5) 0.073(3) Uani 1 1 d . . . C13 C 0.2456(10) 0.1178(6) 0.0379(4) 0.047(2) Uani 1 1 d . . . C14 C 0.2091(13) 0.0500(7) 0.0027(4) 0.058(3) Uani 1 1 d . . . C15 C 0.1238(14) 0.0634(8) -0.0462(4) 0.065(3) Uani 1 1 d . . . C16 C 0.0719(13) 0.1418(8) -0.0594(5) 0.063(3) Uani 1 1 d . . . C17 C 0.1031(11) 0.2101(7) -0.0239(4) 0.055(3) Uani 1 1 d . . . C18 C 0.1931(9) 0.1974(6) 0.0262(4) 0.041(2) Uani 1 1 d . . . C19 C 0.0373(16) 0.2938(8) -0.0401(5) 0.079(4) Uani 1 1 d . . . C20 C 0.3980(16) 0.5104(7) 0.0971(5) 0.068(3) Uani 1 1 d . . . C21 C 0.3337(17) 0.5375(8) 0.0477(6) 0.080(4) Uani 1 1 d . . . C22 C 0.409(2) 0.6008(10) 0.0164(7) 0.092(5) Uani 1 1 d . . . C23 C 0.533(2) 0.6279(11) 0.0401(10) 0.104(6) Uani 1 1 d . . . C24 C 0.592(2) 0.6048(12) 0.0889(10) 0.118(7) Uani 1 1 d . . . C25 C 0.5284(15) 0.5450(7) 0.1186(6) 0.076(4) Uani 1 1 d . . . C26 C 0.332(3) 0.6207(12) -0.0401(9) 0.170(12) Uani 1 1 d . . . C27 C 0.4446(14) 0.4023(9) 0.2004(5) 0.071(3) Uani 1 1 d . . . C28 C 0.4576(17) 0.4599(11) 0.2431(5) 0.089(4) Uani 1 1 d . . . C29 C 0.568(2) 0.4414(15) 0.2882(6) 0.120(8) Uani 1 1 d . . . C30 C 0.6511(18) 0.3753(16) 0.2922(9) 0.123(8) Uani 1 1 d . . . C31 C 0.6366(19) 0.3169(14) 0.2493(8) 0.116(7) Uani 1 1 d . . . C32 C 0.5331(17) 0.3303(9) 0.2022(7) 0.094(5) Uani 1 1 d . . . C33 C 0.1388(12) 0.4741(8) 0.1622(5) 0.063(3) Uani 1 1 d . . . C34 C 0.1321(16) 0.5596(9) 0.1689(6) 0.084(4) Uani 1 1 d . . . C35 C 0.020(2) 0.5932(11) 0.1894(6) 0.100(5) Uani 1 1 d . . . C36 C -0.0937(18) 0.5409(17) 0.2055(7) 0.119(7) Uani 1 1 d . . . C37 C -0.086(2) 0.4640(16) 0.1974(11) 0.156(10) Uani 1 1 d . . . C38 C 0.028(2) 0.4237(12) 0.1776(8) 0.119(6) Uani 1 1 d . . . Cl1 Cl 0.1305(5) 0.2091(3) 0.24525(14) 0.0918(11) Uani 1 1 d . . . Cl2 Cl 0.1673(5) 0.4966(3) 0.0200(2) 0.1112(14) Uani 1 1 d . . . H2 H 0.6407 0.1371 0.1793 0.105 Uiso 1 1 calc R . . H3 H 0.8788 0.1604 0.1707 0.122 Uiso 1 1 calc R . . H4 H 0.9485 0.1947 0.0916 0.122 Uiso 1 1 calc R . . H5 H 0.7793 0.1765 0.0108 0.110 Uiso 1 1 calc R . . H6 H 0.5394 0.1403 0.0183 0.078 Uiso 1 1 calc R . . H8 H 0.5595 -0.0369 0.0732 0.074 Uiso 1 1 calc R . . H9 H 0.5781 -0.1799 0.0847 0.095 Uiso 1 1 calc R . . H10 H 0.4210 -0.2483 0.1373 0.103 Uiso 1 1 calc R . . H11 H 0.2359 -0.1799 0.1690 0.094 Uiso 1 1 calc R . . H12 H 0.2228 -0.0342 0.1633 0.087 Uiso 1 1 calc R . . H14 H 0.2427 -0.0035 0.0127 0.070 Uiso 1 1 calc R . . H15 H 0.1011 0.0194 -0.0705 0.078 Uiso 1 1 calc R . . H16 H 0.0139 0.1504 -0.0929 0.075 Uiso 1 1 calc R . . H19A H 0.1085 0.3267 -0.0561 0.118 Uiso 1 1 calc R . . H19B H 0.0115 0.3219 -0.0083 0.118 Uiso 1 1 calc R . . H19C H -0.0501 0.2865 -0.0662 0.118 Uiso 1 1 calc R . . H23 H 0.5842 0.6663 0.0215 0.125 Uiso 1 1 calc R . . H24 H 0.6810 0.6295 0.1042 0.142 Uiso 1 1 calc R . . H25 H 0.5746 0.5288 0.1529 0.091 Uiso 1 1 calc R . . H26A H 0.3077 0.6792 -0.0424 0.254 Uiso 1 1 calc R . . H26B H 0.2421 0.5884 -0.0473 0.254 Uiso 1 1 calc R . . H26C H 0.3961 0.6072 -0.0665 0.254 Uiso 1 1 calc R . . H28 H 0.3981 0.5073 0.2422 0.107 Uiso 1 1 calc R . . H29 H 0.5815 0.4796 0.3168 0.144 Uiso 1 1 calc R . . H30 H 0.7197 0.3666 0.3232 0.147 Uiso 1 1 calc R . . H31 H 0.6956 0.2691 0.2520 0.140 Uiso 1 1 calc R . . H32 H 0.5238 0.2926 0.1733 0.112 Uiso 1 1 calc R . . H34 H 0.2069 0.5935 0.1588 0.101 Uiso 1 1 calc R . . H35 H 0.0151 0.6509 0.1935 0.120 Uiso 1 1 calc R . . H36 H -0.1716 0.5635 0.2215 0.143 Uiso 1 1 calc R . . H37 H -0.1647 0.4313 0.2056 0.188 Uiso 1 1 calc R . . H38 H 0.0316 0.3658 0.1747 0.143 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 As1 0.0434(5) 0.0495(6) 0.0438(5) 0.0018(4) 0.0080(4) 0.0001(4) As2 0.0559(6) 0.0500(6) 0.0590(6) -0.0009(5) 0.0077(5) -0.0078(5) Au1 0.0531(3) 0.0642(3) 0.0457(2) -0.00715(18) 0.00680(18) 0.00047(18) Au2 0.0507(2) 0.0485(2) 0.0527(2) 0.00035(17) 0.00549(17) -0.00391(17) C1 0.050(6) 0.040(5) 0.062(6) 0.007(5) 0.006(5) 0.001(4) C2 0.048(7) 0.122(12) 0.087(10) 0.014(9) -0.009(7) -0.012(7) C3 0.052(8) 0.108(13) 0.135(16) 0.018(11) -0.020(9) -0.005(8) C4 0.051(8) 0.091(11) 0.163(18) 0.000(11) 0.018(10) -0.017(7) C5 0.091(11) 0.058(8) 0.137(14) 0.011(8) 0.052(11) 0.003(7) C6 0.063(7) 0.059(7) 0.079(8) 0.006(6) 0.031(6) 0.002(5) C7 0.044(6) 0.063(7) 0.050(6) 0.010(5) -0.001(4) -0.013(5) C8 0.072(8) 0.058(7) 0.056(6) 0.003(5) 0.006(6) 0.012(5) C9 0.096(10) 0.062(8) 0.079(9) 0.001(7) 0.008(8) 0.016(7) C10 0.085(10) 0.074(9) 0.094(11) 0.030(8) -0.007(8) 0.002(8) C11 0.076(9) 0.076(9) 0.083(9) 0.032(7) 0.005(7) -0.004(7) C12 0.057(7) 0.081(9) 0.080(8) 0.015(7) 0.009(6) -0.001(6) C13 0.039(5) 0.055(6) 0.047(5) 0.007(4) 0.012(4) -0.006(4) C14 0.067(7) 0.052(6) 0.055(6) -0.003(5) 0.009(5) 0.009(5) C15 0.082(8) 0.060(7) 0.048(6) -0.013(5) -0.010(6) 0.007(6) C16 0.056(7) 0.073(8) 0.055(6) -0.008(6) -0.006(5) 0.000(5) C17 0.039(5) 0.065(7) 0.060(6) 0.000(5) 0.006(5) 0.003(5) C18 0.030(4) 0.049(5) 0.045(5) 0.003(4) 0.007(4) -0.007(4) C19 0.082(9) 0.078(9) 0.070(8) 0.021(7) -0.016(7) 0.011(7) C20 0.101(10) 0.050(7) 0.058(7) -0.010(5) 0.028(7) -0.010(6) C21 0.110(11) 0.057(8) 0.078(9) -0.010(7) 0.036(8) 0.010(7) C22 0.128(15) 0.072(10) 0.081(10) 0.000(8) 0.039(10) 0.039(10) C23 0.114(15) 0.079(11) 0.134(17) -0.004(11) 0.068(13) -0.006(10) C24 0.113(15) 0.109(14) 0.144(17) -0.036(13) 0.061(14) -0.041(11) C25 0.084(9) 0.049(7) 0.103(10) -0.008(7) 0.045(8) -0.021(6) C26 0.29(3) 0.094(14) 0.15(2) 0.052(13) 0.13(2) 0.076(17) C27 0.068(8) 0.082(9) 0.057(7) 0.016(6) -0.006(6) -0.022(6) C28 0.094(11) 0.117(12) 0.055(7) -0.005(8) 0.001(7) 0.002(9) C29 0.094(13) 0.21(2) 0.060(9) -0.029(12) 0.024(9) -0.065(14) C30 0.046(8) 0.20(2) 0.117(15) 0.055(16) 0.005(9) 0.011(11) C31 0.076(11) 0.145(17) 0.116(15) 0.022(13) -0.030(10) -0.031(10) C32 0.086(10) 0.064(9) 0.119(13) 0.005(8) -0.029(9) -0.002(7) C33 0.039(6) 0.076(8) 0.076(8) 0.000(6) 0.007(5) -0.005(5) C34 0.065(8) 0.087(10) 0.103(11) -0.019(8) 0.024(8) -0.007(7) C35 0.095(12) 0.114(13) 0.088(11) -0.038(9) 0.006(9) 0.014(10) C36 0.064(10) 0.20(2) 0.098(12) -0.051(14) 0.021(8) 0.027(12) C37 0.107(16) 0.138(19) 0.25(3) -0.017(19) 0.104(18) -0.010(14) C38 0.111(14) 0.100(13) 0.160(17) -0.009(11) 0.070(13) -0.031(10) Cl1 0.096(3) 0.119(3) 0.0635(19) -0.0308(19) 0.0209(18) 0.015(2) Cl2 0.117(3) 0.091(3) 0.121(3) 0.022(2) -0.001(3) 0.004(2) _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 As1 C1 1.939(10) . ? As1 C7 1.929(11) . ? As1 C13 1.930(10) . ? As2 C20 1.982(12) . ? As2 C27 1.937(12) . ? As2 C33 1.949(12) . ? Au1 As1 2.3294(11) . ? Au1 Cl1 2.271(3) . ? Au2 As2 2.4166(12) . ? Au2 Au1 3.2747(7) . ? Au2 C18 2.063(9) . ? C1 C2 1.365(16) . ? C1 C6 1.370(15) . ? C2 C3 1.33(2) . ? C4 C3 1.29(2) . ? C5 C4 1.42(2) . ? C6 C5 1.355(18) . ? C8 C7 1.391(16) . ? C8 C9 1.371(17) . ? C9 C10 1.41(2) . ? C10 C11 1.32(2) . ? C12 C7 1.391(15) . ? C12 C11 1.402(18) . ? C13 C14 1.400(14) . ? C14 C15 1.361(15) . ? C15 C16 1.363(16) . ? C17 C16 1.405(15) . ? C17 C19 1.499(16) . ? C18 C13 1.376(14) . ? C18 C17 1.402(14) . ? C20 C25 1.349(18) . ? C21 C20 1.352(18) . ? C21 C22 1.49(2) . ? C21 Cl2 1.704(16) . ? C22 C23 1.28(3) . ? C22 C26 1.51(3) . ? C23 C24 1.31(3) . ? C25 C24 1.38(2) . ? C27 C28 1.393(19) . ? C27 C32 1.40(2) . ? C28 C29 1.43(2) . ? C29 C30 1.29(3) . ? C30 C31 1.41(3) . ? C32 C31 1.41(2) . ? C33 C34 1.380(18) . ? C33 C38 1.380(19) . ? C34 C35 1.31(2) . ? C35 C36 1.43(3) . ? C36 C37 1.25(3) . ? C38 C37 1.37(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag As1 Au1 Au2 71.88(3) . . ? As2 Au2 Au1 97.99(3) . . ? C1 As1 Au1 117.5(3) . . ? C2 C1 As1 120.6(9) . . ? C2 C1 C6 117.3(11) . . ? C3 C2 C1 121.1(15) . . ? C3 C4 C5 118.9(14) . . ? C4 C3 C2 122.8(16) . . ? C5 C6 C1 121.1(14) . . ? C6 C1 As1 122.1(8) . . ? C6 C5 C4 118.4(15) . . ? C7 As1 Au1 113.0(3) . . ? C7 As1 C1 101.9(4) . . ? C7 As1 C13 106.6(4) . . ? C7 C12 C11 119.2(13) . . ? C8 C7 As1 122.1(8) . . ? C8 C9 C10 119.4(14) . . ? C9 C8 C7 119.7(12) . . ? C10 C11 C12 120.4(13) . . ? C11 C10 C9 121.4(13) . . ? C12 C7 As1 118.1(9) . . ? C12 C7 C8 119.8(11) . . ? C13 As1 Au1 110.8(3) . . ? C13 As1 C1 106.1(4) . . ? C13 C18 Au2 121.9(7) . . ? C13 C18 C17 117.5(9) . . ? C14 C13 As1 119.1(8) . . ? C14 C15 C16 119.5(10) . . ? C15 C14 C13 119.2(10) . . ? C15 C16 C17 122.2(10) . . ? C16 C17 C19 119.2(10) . . ? C17 C18 Au2 120.5(7) . . ? C18 Au2 As2 175.4(3) . . ? C18 Au2 Au1 86.5(3) . . ? C18 C13 As1 118.0(7) . . ? C18 C13 C14 122.7(9) . . ? C18 C17 C16 118.8(10) . . ? C18 C17 C19 121.9(10) . . ? C20 As2 Au2 114.0(3) . . ? C20 C21 C22 120.9(15) . . ? C20 C21 Cl2 119.3(11) . . ? C20 C25 C24 119.2(17) . . ? C21 C20 As2 120.0(11) . . ? C21 C22 C26 115.8(19) . . ? C22 C21 Cl2 119.7(13) . . ? C22 C23 C24 123.9(19) . . ? C23 C22 C21 115.5(16) . . ? C23 C22 C26 129(2) . . ? C23 C24 C25 122.3(19) . . ? C25 C20 As2 121.8(10) . . ? C25 C20 C21 118.1(12) . . ? C27 As2 Au2 115.5(4) . . ? C27 As2 C20 102.8(5) . . ? C27 As2 C33 102.8(6) . . ? C27 C28 C29 115.6(16) . . ? C27 C32 C31 117.9(16) . . ? C28 C27 As2 121.4(11) . . ? C28 C27 C32 122.0(12) . . ? C29 C30 C31 119.4(18) . . ? C30 C29 C28 124.8(19) . . ? C30 C31 C32 120.2(19) . . ? C32 C27 As2 116.6(10) . . ? C33 As2 Au2 116.6(3) . . ? C33 As2 C20 103.4(5) . . ? C34 C33 As2 122.5(9) . . ? C34 C33 C38 120.0(13) . . ? C34 C35 C36 119.9(17) . . ? C35 C34 C33 120.1(15) . . ? C36 C37 C38 126(2) . . ? C37 C36 C35 118.2(16) . . ? C37 C38 C33 116.2(18) . . ? C38 C33 As2 117.4(12) . . ? Cl1 Au1 As1 174.84(11) . . ? Cl1 Au1 Au2 110.61(11) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 4.485 _refine_diff_density_min -1.154 _refine_diff_density_rms 0.199 #===END data_compound12 _database_code_depnum_ccdc_archive 'CCDC 290394' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H33 As2 Au2 Br' _chemical_formula_weight 1113.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.9939(7) _cell_length_b 15.7013(13) _cell_length_c 25.199(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.491(2) _cell_angle_gamma 90.00 _cell_volume 3535.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.091 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 11.302 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS Sheldrick 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26126 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0707 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 28.33 _reflns_number_total 8765 _reflns_number_gt 5767 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8765 _refine_ls_number_parameters 390 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0784 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.0928 _refine_ls_wR_factor_gt 0.0812 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.79243(7) 0.93171(4) 0.13800(3) 0.05419(18) Uani 1 1 d . . . As2 As 0.84624(7) 0.60878(4) 0.10371(2) 0.04813(16) Uani 1 1 d . . . Au1 Au 0.73233(3) 0.809948(16) 0.081516(10) 0.05297(9) Uani 1 1 d . . . Au2 Au 0.73527(3) 0.674291(17) 0.172666(9) 0.05434(9) Uani 1 1 d . . . Br1 Br 0.60610(10) 0.73255(6) 0.24184(3) 0.0900(3) Uani 1 1 d . . . C1 C 0.8773(7) 1.0187(4) 0.0963(3) 0.0589(18) Uani 1 1 d . . . C2 C 0.8148(9) 1.0305(4) 0.0450(3) 0.071(2) Uani 1 1 d . . . C3 C 0.8739(12) 1.0884(5) 0.0118(3) 0.084(3) Uani 1 1 d . . . C4 C 1.0007(13) 1.1339(6) 0.0326(5) 0.105(4) Uani 1 1 d . . . C5 C 1.0643(11) 1.1222(6) 0.0828(5) 0.107(3) Uani 1 1 d . . . C6 C 1.0032(8) 1.0644(5) 0.1156(3) 0.079(2) Uani 1 1 d . . . C7 C 0.8009(14) 1.1010(6) -0.0437(4) 0.140(5) Uani 1 1 d . . . C8 C 0.9397(7) 0.9139(4) 0.1984(3) 0.0578(17) Uani 1 1 d . . . C9 C 0.9586(8) 0.9662(6) 0.2420(3) 0.083(2) Uani 1 1 d . . . C10 C 1.0669(10) 0.9503(8) 0.2847(4) 0.108(3) Uani 1 1 d . . . C11 C 1.1584(11) 0.8826(8) 0.2827(4) 0.110(3) Uani 1 1 d . . . C12 C 1.1423(10) 0.8289(6) 0.2390(4) 0.103(3) Uani 1 1 d . . . C13 C 1.0329(9) 0.8445(5) 0.1969(3) 0.082(2) Uani 1 1 d . . . C14 C 0.6304(7) 0.9933(5) 0.1653(2) 0.0592(17) Uani 1 1 d . . . C15 C 0.6379(8) 1.0789(5) 0.1755(3) 0.077(2) Uani 1 1 d . . . C16 C 0.5194(10) 1.1194(6) 0.1947(3) 0.089(3) Uani 1 1 d . . . C17 C 0.3957(10) 1.0795(7) 0.2030(4) 0.098(3) Uani 1 1 d . . . C18 C 0.3829(10) 0.9955(8) 0.1911(4) 0.121(4) Uani 1 1 d . . . C19 C 0.5020(9) 0.9508(5) 0.1726(4) 0.098(3) Uani 1 1 d . . . C20 C 0.6883(7) 0.7146(4) 0.0256(2) 0.0545(16) Uani 1 1 d . . . C21 C 0.6073(7) 0.7325(5) -0.0245(3) 0.069(2) Uani 1 1 d . . . C22 C 0.5820(9) 0.6665(6) -0.0613(3) 0.089(3) Uani 1 1 d . . . C23 C 0.6262(9) 0.5851(6) -0.0501(3) 0.089(3) Uani 1 1 d . . . C24 C 0.7051(8) 0.5661(5) -0.0017(3) 0.0678(19) Uani 1 1 d . . . C25 C 0.7365(6) 0.6308(4) 0.0354(2) 0.0498(15) Uani 1 1 d . . . C26 C 0.5456(9) 0.8204(5) -0.0385(3) 0.093(3) Uani 1 1 d . . . C27 C 0.8640(7) 0.4873(4) 0.1119(2) 0.0524(16) Uani 1 1 d . . . C28 C 0.9754(9) 0.4415(5) 0.0917(3) 0.071(2) Uani 1 1 d . . . C29 C 0.9848(10) 0.3550(5) 0.0988(3) 0.084(2) Uani 1 1 d . . . C30 C 0.8834(11) 0.3118(5) 0.1255(3) 0.086(3) Uani 1 1 d . . . C31 C 0.7742(10) 0.3583(6) 0.1455(3) 0.091(3) Uani 1 1 d . . . C32 C 0.7648(8) 0.4444(5) 0.1386(3) 0.076(2) Uani 1 1 d . . . C33 C 1.0494(7) 0.6402(4) 0.0960(2) 0.0508(15) Uani 1 1 d . . . C34 C 1.0966(8) 0.6530(4) 0.0467(3) 0.0669(19) Uani 1 1 d . . . C35 C 1.2480(10) 0.6688(5) 0.0429(4) 0.093(3) Uani 1 1 d . . . C36 C 1.3434(10) 0.6732(6) 0.0879(5) 0.105(4) Uani 1 1 d . . . C37 C 1.2984(9) 0.6599(6) 0.1370(4) 0.104(3) Uani 1 1 d . . . C38 C 1.1508(8) 0.6450(5) 0.1407(3) 0.078(2) Uani 1 1 d . . . H2 H 0.7308 0.9990 0.0321 0.085 Uiso 1 1 calc R . . H4 H 1.0421 1.1734 0.0111 0.126 Uiso 1 1 calc R . . H5 H 1.1494 1.1529 0.0955 0.128 Uiso 1 1 calc R . . H6 H 1.0467 1.0563 0.1505 0.095 Uiso 1 1 calc R . . H7A H 0.7724 1.0467 -0.0592 0.210 Uiso 1 1 calc R . . H7B H 0.8696 1.1284 -0.0647 0.210 Uiso 1 1 calc R . . H7C H 0.7135 1.1359 -0.0430 0.210 Uiso 1 1 calc R . . H9 H 0.8974 1.0138 0.2432 0.099 Uiso 1 1 calc R . . H10 H 1.0763 0.9860 0.3143 0.129 Uiso 1 1 calc R . . H11 H 1.2324 0.8720 0.3108 0.132 Uiso 1 1 calc R . . H12 H 1.2053 0.7821 0.2379 0.123 Uiso 1 1 calc R . . H13 H 1.0224 0.8081 0.1676 0.099 Uiso 1 1 calc R . . H15 H 0.7228 1.1096 0.1694 0.093 Uiso 1 1 calc R . . H16 H 0.5272 1.1773 0.2020 0.107 Uiso 1 1 calc R . . H17 H 0.3184 1.1084 0.2168 0.118 Uiso 1 1 calc R . . H18 H 0.2942 0.9671 0.1952 0.145 Uiso 1 1 calc R . . H19 H 0.4935 0.8928 0.1655 0.118 Uiso 1 1 calc R . . H22 H 0.5328 0.6786 -0.0949 0.107 Uiso 1 1 calc R . . H23 H 0.6030 0.5424 -0.0752 0.107 Uiso 1 1 calc R . . H24 H 0.7369 0.5107 0.0061 0.081 Uiso 1 1 calc R . . H26A H 0.5708 0.8365 -0.0731 0.139 Uiso 1 1 calc R . . H26B H 0.5880 0.8606 -0.0124 0.139 Uiso 1 1 calc R . . H26C H 0.4387 0.8198 -0.0389 0.139 Uiso 1 1 calc R . . H28 H 1.0447 0.4694 0.0732 0.086 Uiso 1 1 calc R . . H29 H 1.0613 0.3250 0.0852 0.100 Uiso 1 1 calc R . . H30 H 0.8889 0.2531 0.1299 0.103 Uiso 1 1 calc R . . H31 H 0.7048 0.3307 0.1641 0.109 Uiso 1 1 calc R . . H32 H 0.6888 0.4743 0.1526 0.091 Uiso 1 1 calc R . . H34 H 1.0284 0.6512 0.0160 0.080 Uiso 1 1 calc R . . H35 H 1.2823 0.6762 0.0097 0.112 Uiso 1 1 calc R . . H36 H 1.4434 0.6858 0.0853 0.126 Uiso 1 1 calc R . . H37 H 1.3672 0.6609 0.1674 0.125 Uiso 1 1 calc R . . H38 H 1.1184 0.6380 0.1742 0.094 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 As1 0.0551(4) 0.0544(4) 0.0539(4) 0.0025(3) 0.0102(3) -0.0020(3) As2 0.0440(3) 0.0597(4) 0.0416(3) -0.0033(3) 0.0090(3) -0.0029(3) Au1 0.05192(16) 0.05868(17) 0.04893(16) 0.00163(12) 0.00840(12) -0.00066(12) Au2 0.05205(16) 0.07208(19) 0.03934(14) -0.00659(12) 0.00711(11) 0.00017(12) Br1 0.0963(6) 0.1256(7) 0.0499(4) -0.0203(4) 0.0164(4) 0.0252(5) C1 0.058(4) 0.055(4) 0.068(5) 0.009(3) 0.023(4) 0.003(3) C2 0.096(6) 0.060(5) 0.062(5) 0.002(4) 0.028(4) 0.014(4) C3 0.139(8) 0.056(5) 0.063(5) 0.009(4) 0.044(6) 0.037(5) C4 0.138(9) 0.055(6) 0.137(9) 0.026(6) 0.086(8) 0.021(6) C5 0.094(7) 0.074(6) 0.158(10) 0.030(7) 0.041(7) -0.007(5) C6 0.080(6) 0.069(5) 0.094(6) 0.011(4) 0.031(5) -0.005(4) C7 0.245(14) 0.094(7) 0.092(7) 0.029(6) 0.067(9) 0.045(8) C8 0.055(4) 0.054(4) 0.064(4) 0.014(3) 0.006(3) -0.009(3) C9 0.058(5) 0.122(7) 0.067(5) -0.008(5) 0.005(4) 0.010(5) C10 0.072(6) 0.185(11) 0.068(6) -0.008(6) 0.013(5) -0.002(7) C11 0.074(7) 0.165(11) 0.088(7) 0.022(7) -0.009(6) -0.013(7) C12 0.069(6) 0.103(8) 0.130(9) 0.025(7) -0.015(6) -0.001(5) C13 0.071(5) 0.077(6) 0.094(6) 0.005(5) -0.014(5) -0.006(4) C14 0.054(4) 0.071(5) 0.056(4) -0.001(4) 0.018(3) -0.006(3) C15 0.061(5) 0.076(6) 0.097(6) -0.016(5) 0.020(4) 0.003(4) C16 0.079(6) 0.088(6) 0.103(7) -0.023(5) 0.026(5) 0.009(5) C17 0.068(6) 0.127(9) 0.103(7) -0.008(6) 0.026(5) 0.011(6) C18 0.074(6) 0.132(9) 0.167(10) 0.003(8) 0.058(7) -0.013(6) C19 0.072(5) 0.081(6) 0.147(9) 0.005(6) 0.041(6) -0.003(5) C20 0.041(3) 0.078(5) 0.045(4) 0.000(3) 0.010(3) -0.002(3) C21 0.050(4) 0.104(6) 0.052(4) 0.006(4) 0.002(3) 0.007(4) C22 0.086(6) 0.123(8) 0.050(4) -0.009(5) -0.024(4) 0.012(5) C23 0.096(6) 0.107(7) 0.061(5) -0.024(5) -0.006(5) 0.006(5) C24 0.075(5) 0.074(5) 0.054(4) -0.017(4) 0.007(4) 0.003(4) C25 0.039(3) 0.064(4) 0.046(3) -0.005(3) 0.005(3) -0.004(3) C26 0.085(6) 0.120(7) 0.069(5) 0.014(5) -0.009(5) 0.028(5) C27 0.053(4) 0.066(4) 0.038(3) 0.003(3) 0.009(3) -0.004(3) C28 0.092(6) 0.063(5) 0.063(5) 0.009(4) 0.028(4) 0.001(4) C29 0.121(7) 0.071(6) 0.062(5) 0.005(4) 0.025(5) 0.021(5) C30 0.115(7) 0.066(5) 0.077(6) 0.028(4) 0.008(5) 0.004(5) C31 0.084(6) 0.089(7) 0.099(7) 0.036(5) 0.010(5) -0.007(5) C32 0.054(4) 0.082(6) 0.093(6) 0.025(5) 0.018(4) 0.006(4) C33 0.042(3) 0.052(4) 0.058(4) -0.002(3) 0.006(3) 0.006(3) C34 0.065(5) 0.069(5) 0.069(5) -0.004(4) 0.020(4) -0.005(4) C35 0.076(6) 0.080(6) 0.135(9) 0.010(6) 0.064(6) -0.005(5) C36 0.047(5) 0.091(7) 0.179(12) 0.000(7) 0.025(7) -0.007(4) C37 0.040(5) 0.141(9) 0.127(9) 0.011(7) -0.012(5) -0.001(5) C38 0.052(4) 0.107(6) 0.074(5) 0.002(5) 0.001(4) -0.007(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 As1 C1 1.933(6) . ? As1 C14 1.938(6) . ? As1 C8 1.922(7) . ? As2 C25 1.917(6) . ? As2 C27 1.924(7) . ? As2 C33 1.924(6) . ? Au1 As1 2.4082(7) . ? Au1 C20 2.063(6) . ? Au2 As2 2.3379(6) . ? Au2 Au1 3.1304(4) . ? Au2 Br1 2.3839(7) . ? C1 C2 1.362(10) . ? C1 C6 1.382(10) . ? C2 C3 1.382(10) . ? C3 C4 1.397(14) . ? C3 C7 1.489(12) . ? C4 C5 1.340(13) . ? C6 C5 1.382(10) . ? C8 C9 1.368(9) . ? C8 C13 1.379(10) . ? C9 C10 1.389(11) . ? C10 C11 1.349(13) . ? C11 C12 1.380(13) . ? C13 C12 1.386(11) . ? C14 C15 1.369(9) . ? C14 C19 1.364(9) . ? C16 C15 1.374(9) . ? C16 C17 1.315(11) . ? C17 C18 1.355(12) . ? C19 C18 1.403(11) . ? C20 C21 1.413(9) . ? C21 C22 1.392(11) . ? C21 C26 1.514(10) . ? C22 C23 1.358(11) . ? C24 C23 1.373(10) . ? C25 C20 1.399(9) . ? C25 C24 1.387(8) . ? C27 C28 1.376(9) . ? C27 C32 1.357(8) . ? C28 C29 1.370(9) . ? C29 C30 1.373(10) . ? C30 C31 1.364(11) . ? C32 C31 1.364(10) . ? C33 C34 1.374(8) . ? C33 C38 1.368(9) . ? C34 C35 1.398(10) . ? C35 C36 1.344(13) . ? C36 C37 1.361(13) . ? C38 C37 1.361(10) . ? 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 As1 Au1 Au2 97.113(19) . . ? As2 Au2 Au1 73.914(19) . . ? As2 Au2 Br1 175.27(3) . . ? Br1 Au2 Au1 108.12(3) . . ? C1 As1 Au1 108.4(2) . . ? C1 As1 C14 101.5(3) . . ? C1 C2 C3 121.2(8) . . ? C1 C6 C5 119.7(8) . . ? C2 C1 As1 117.8(6) . . ? C2 C1 C6 119.9(7) . . ? C2 C3 C4 117.5(8) . . ? C2 C3 C7 119.8(10) . . ? C4 C3 C7 122.7(9) . . ? C4 C5 C6 119.8(10) . . ? C5 C4 C3 121.9(9) . . ? C6 C1 As1 122.2(6) . . ? C8 As1 Au1 116.2(2) . . ? C8 As1 C1 104.8(3) . . ? C8 As1 C14 105.7(3) . . ? C8 C13 C12 119.9(8) . . ? C8 C9 C10 121.8(8) . . ? C9 C8 As1 124.2(6) . . ? C9 C8 C13 118.5(7) . . ? C10 C11 C12 120.1(10) . . ? C11 C10 C9 119.4(9) . . ? C11 C12 C13 120.3(10) . . ? C13 C8 As1 117.4(6) . . ? C14 As1 Au1 118.6(2) . . ? C14 C15 C16 119.8(7) . . ? C14 C19 C18 119.3(8) . . ? C15 C14 As1 122.2(5) . . ? C16 C17 C18 118.7(8) . . ? C17 C16 C15 122.7(9) . . ? C17 C18 C19 120.8(9) . . ? C19 C14 As1 119.1(6) . . ? C19 C14 C15 118.6(7) . . ? C20 Au1 As1 172.98(17) . . ? C20 Au1 Au2 89.60(18) . . ? C20 C21 C26 121.8(7) . . ? C20 C25 As2 116.5(5) . . ? C21 C20 Au1 120.4(5) . . ? C22 C21 C20 118.4(7) . . ? C22 C21 C26 119.7(7) . . ? C22 C23 C24 120.0(8) . . ? C23 C22 C21 122.7(8) . . ? C23 C24 C25 119.0(7) . . ? C24 C25 As2 121.2(5) . . ? C24 C25 C20 122.3(6) . . ? C25 As2 Au2 111.63(18) . . ? C25 As2 C27 107.6(3) . . ? C25 As2 C33 105.2(3) . . ? C25 C20 Au1 122.0(5) . . ? C25 C20 C21 117.6(6) . . ? C27 As2 Au2 113.23(17) . . ? C27 C32 C31 121.3(7) . . ? C28 C27 As2 122.3(5) . . ? C28 C29 C30 121.2(8) . . ? C29 C28 C27 120.4(7) . . ? C30 C31 C32 121.4(8) . . ? C31 C30 C29 117.6(8) . . ? C32 C27 As2 119.6(5) . . ? C32 C27 C28 118.1(6) . . ? C33 As2 Au2 116.87(18) . . ? C33 As2 C27 101.4(3) . . ? C33 C34 C35 119.4(8) . . ? C34 C33 As2 121.5(5) . . ? C35 C36 C37 122.2(8) . . ? C36 C35 C34 119.0(8) . . ? C37 C38 C33 121.2(8) . . ? C38 C33 As2 118.9(5) . . ? C38 C33 C34 119.4(6) . . ? C38 C37 C36 118.7(9) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.389 _refine_diff_density_min -0.566 _refine_diff_density_rms 0.132 #===END data_compound13 _database_code_depnum_ccdc_archive 'CCDC 290395' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H16 As I' _chemical_formula_weight 446.14 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3408(6) _cell_length_b 9.8564(6) _cell_length_c 11.1989(7) _cell_angle_alpha 112.6130(10) _cell_angle_beta 111.2450(10) _cell_angle_gamma 97.2830(10) _cell_volume 843.60(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.54 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 432 _exptl_absorpt_coefficient_mu 3.836 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS Sheldrick 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6289 _diffrn_reflns_av_R_equivalents 0.0131 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 28.27 _reflns_number_total 4124 _reflns_number_gt 3696 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+0.2706P] 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 4124 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0316 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0775 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 As1 As 0.67157(3) 0.77861(3) 0.64354(3) 0.03804(8) Uani 1 1 d . . . C1 C 0.8833(3) 0.7449(2) 0.6833(2) 0.0360(4) Uani 1 1 d . . . C2 C 0.9510(3) 0.7364(3) 0.5890(2) 0.0379(4) Uani 1 1 d . . . C3 C 1.0988(3) 0.7083(3) 0.6097(3) 0.0460(5) Uani 1 1 d . . . C4 C 1.1760(3) 0.6848(3) 0.7291(3) 0.0521(6) Uani 1 1 d . . . C5 C 1.1128(3) 0.6926(3) 0.8243(3) 0.0512(6) Uani 1 1 d . . . C6 C 0.9667(3) 0.7224(3) 0.8014(3) 0.0435(5) Uani 1 1 d . . . C7 C 1.1744(4) 0.7009(4) 0.5110(4) 0.0662(8) Uani 1 1 d . . . C8 C 0.6469(3) 0.7708(3) 0.8076(3) 0.0380(4) Uani 1 1 d . . . C9 C 0.5890(3) 0.6261(3) 0.7935(3) 0.0484(6) Uani 1 1 d . . . C10 C 0.5629(4) 0.6124(3) 0.9032(3) 0.0570(7) Uani 1 1 d . . . C11 C 0.5901(4) 0.7419(4) 1.0254(3) 0.0547(6) Uani 1 1 d . . . C12 C 0.6459(4) 0.8858(3) 1.0392(3) 0.0598(7) Uani 1 1 d . . . C13 C 0.6741(3) 0.8999(3) 0.9306(3) 0.0504(6) Uani 1 1 d . . . C14 C 0.7384(3) 1.0028(3) 0.7171(2) 0.0379(4) Uani 1 1 d . . . C15 C 0.6174(3) 1.0706(3) 0.6875(3) 0.0476(5) Uani 1 1 d . . . C16 C 0.6551(4) 1.2278(4) 0.7334(4) 0.0566(7) Uani 1 1 d . . . C17 C 0.8137(4) 1.3190(3) 0.8087(3) 0.0554(7) Uani 1 1 d . . . C18 C 0.9362(4) 1.2535(3) 0.8393(3) 0.0536(6) Uani 1 1 d . . . C19 C 0.8979(3) 1.0953(3) 0.7931(3) 0.0449(5) Uani 1 1 d . . . H4 H 1.2733 0.6631 0.7450 0.063 Uiso 1 1 calc R . . H5 H 1.1680 0.6780 0.9038 0.061 Uiso 1 1 calc R . . H6 H 0.9241 0.7273 0.8657 0.052 Uiso 1 1 calc R . . H7A H 1.1010 0.6230 0.4142 0.099 Uiso 1 1 calc R . . H7B H 1.2726 0.6755 0.5431 0.099 Uiso 1 1 calc R . . H7C H 1.1979 0.7993 0.5124 0.099 Uiso 1 1 calc R . . H9 H 0.5677 0.5378 0.7101 0.058 Uiso 1 1 calc R . . H10 H 0.5267 0.5149 0.8940 0.068 Uiso 1 1 calc R . . H11 H 0.5708 0.7323 1.0981 0.066 Uiso 1 1 calc R . . H12 H 0.6649 0.9739 1.1218 0.072 Uiso 1 1 calc R . . H13 H 0.7117 0.9977 0.9408 0.060 Uiso 1 1 calc R . . H15 H 0.5098 1.0096 0.6361 0.057 Uiso 1 1 calc R . . H16 H 0.5729 1.2721 0.7133 0.068 Uiso 1 1 calc R . . H17 H 0.8388 1.4248 0.8391 0.066 Uiso 1 1 calc R . . H18 H 1.0436 1.3151 0.8907 0.064 Uiso 1 1 calc R . . H19 H 0.9802 1.0513 0.8133 0.054 Uiso 1 1 calc R . . I1 I 0.82893(2) 0.77131(2) 0.408364(19) 0.05512(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.03620(13) 0.03978(13) 0.04069(13) 0.01946(10) 0.01850(10) 0.01341(9) C1 0.0365(10) 0.0337(10) 0.0372(10) 0.0156(8) 0.0162(9) 0.0126(8) C2 0.0387(11) 0.0364(10) 0.0356(10) 0.0150(8) 0.0160(9) 0.0104(8) C3 0.0406(12) 0.0432(12) 0.0474(13) 0.0130(10) 0.0222(11) 0.0104(9) C4 0.0390(12) 0.0534(14) 0.0597(16) 0.0219(12) 0.0205(12) 0.0206(11) C5 0.0479(13) 0.0575(15) 0.0488(14) 0.0276(12) 0.0169(11) 0.0235(12) C6 0.0471(13) 0.0473(12) 0.0410(12) 0.0231(10) 0.0209(10) 0.0184(10) C7 0.0527(16) 0.080(2) 0.071(2) 0.0275(16) 0.0402(16) 0.0201(15) C8 0.0366(10) 0.0391(11) 0.0457(12) 0.0228(9) 0.0214(9) 0.0145(8) C9 0.0571(15) 0.0376(11) 0.0544(14) 0.0224(10) 0.0277(12) 0.0148(10) C10 0.0677(18) 0.0499(14) 0.0671(18) 0.0381(13) 0.0332(15) 0.0161(13) C11 0.0583(16) 0.0668(17) 0.0554(15) 0.0401(14) 0.0292(13) 0.0201(13) C12 0.079(2) 0.0521(15) 0.0511(15) 0.0218(12) 0.0357(15) 0.0175(14) C13 0.0628(16) 0.0401(12) 0.0489(14) 0.0195(10) 0.0291(13) 0.0098(11) C14 0.0443(11) 0.0412(11) 0.0392(11) 0.0244(9) 0.0221(9) 0.0182(9) C15 0.0454(13) 0.0529(14) 0.0534(14) 0.0307(12) 0.0227(11) 0.0220(11) C16 0.0703(18) 0.0570(15) 0.0649(17) 0.0391(14) 0.0355(15) 0.0378(14) C17 0.082(2) 0.0423(13) 0.0562(15) 0.0288(12) 0.0377(15) 0.0233(13) C18 0.0599(16) 0.0469(14) 0.0480(14) 0.0206(11) 0.0228(13) 0.0073(12) C19 0.0435(12) 0.0468(12) 0.0468(13) 0.0238(10) 0.0196(10) 0.0170(10) I1 0.05604(12) 0.07209(14) 0.04570(11) 0.03410(9) 0.02452(9) 0.01892(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 C1 1.965(2) . ? As1 C8 1.962(2) . ? As1 C14 1.956(2) . ? C1 C6 1.390(3) . ? C2 C1 1.396(3) . ? C2 C3 1.397(3) . ? C3 C4 1.394(4) . ? C3 C7 1.498(4) . ? C5 C4 1.377(4) . ? C5 C6 1.385(4) . ? C8 C9 1.386(3) . ? C8 C13 1.377(3) . ? C10 C9 1.387(4) . ? C11 C10 1.375(4) . ? C11 C12 1.375(4) . ? C13 C12 1.386(4) . ? C14 C15 1.388(3) . ? C14 C19 1.385(3) . ? C15 C16 1.381(4) . ? C16 C17 1.374(5) . ? C18 C17 1.384(4) . ? C19 C18 1.389(4) . ? I1 C2 2.115(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 C2 C3 122.8(2) . . ? C1 C2 I1 119.36(16) . . ? C2 C1 As1 120.44(17) . . ? C2 C3 C7 123.6(3) . . ? C3 C2 I1 117.80(18) . . ? C4 C3 C2 116.6(2) . . ? C4 C3 C7 119.8(3) . . ? C4 C5 C6 119.9(3) . . ? C5 C4 C3 122.1(2) . . ? C5 C6 C1 120.6(2) . . ? C6 C1 As1 121.47(18) . . ? C6 C1 C2 118.0(2) . . ? C8 As1 C1 99.49(9) . . ? C8 C13 C12 120.7(2) . . ? C9 C8 As1 117.28(18) . . ? C10 C9 C8 120.3(2) . . ? C11 C10 C9 120.5(2) . . ? C11 C12 C13 120.2(3) . . ? C12 C11 C10 119.5(3) . . ? C13 C8 As1 123.75(18) . . ? C13 C8 C9 118.8(2) . . ? C14 As1 C1 99.34(9) . . ? C14 As1 C8 99.19(9) . . ? C14 C19 C18 120.6(2) . . ? C15 C14 As1 117.31(18) . . ? C16 C15 C14 120.7(3) . . ? C16 C17 C18 120.0(3) . . ? C17 C16 C15 120.2(3) . . ? C17 C18 C19 119.7(3) . . ? C19 C14 As1 123.83(18) . . ? C19 C14 C15 118.8(2) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.751 _refine_diff_density_min -1.086 _refine_diff_density_rms 0.094 #===END data_compound14 _database_code_depnum_ccdc_archive 'CCDC 290396' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H32 As2 Au2 I2' _chemical_formula_weight 1286.21 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1944(9) _cell_length_b 12.0156(11) _cell_length_c 20.2994(19) _cell_angle_alpha 83.702(2) _cell_angle_beta 81.403(2) _cell_angle_gamma 77.640(2) _cell_volume 2159.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.090 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.979 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1180 _exptl_absorpt_coefficient_mu 9.760 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS Sheldrick 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16075 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.02 _diffrn_reflns_theta_max 28.37 _reflns_number_total 10595 _reflns_number_gt 7865 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1360P)^2^+0.4373P] 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 10595 _refine_ls_number_parameters 399 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.2135 _refine_ls_wR_factor_gt 0.1960 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.21202(13) 0.74550(9) 0.34523(5) 0.0457(3) Uani 1 1 d . . . As2 As 0.26761(11) 1.04526(9) 0.14900(5) 0.0411(2) Uani 1 1 d . . . Au1 Au 0.19341(5) 0.79751(4) 0.22818(2) 0.04485(14) Uani 1 1 d . . . Au2 Au 0.10491(5) 1.07159(4) 0.24979(2) 0.04978(15) Uani 1 1 d . . . C1 C 0.3522(14) 0.6045(10) 0.3659(7) 0.056(3) Uani 1 1 d . . . C2 C 0.3527(17) 0.5013(11) 0.3425(7) 0.064(3) Uani 1 1 d . . . C3 C 0.4581(18) 0.4036(11) 0.3525(8) 0.071(4) Uani 1 1 d . . . C4 C 0.569(2) 0.4119(13) 0.3909(10) 0.096(6) Uani 1 1 d . . . C5 C 0.5700(19) 0.5088(14) 0.4183(11) 0.094(6) Uani 1 1 d . . . C6 C 0.4665(17) 0.6063(13) 0.4014(8) 0.074(4) Uani 1 1 d . . . C7 C 0.461(3) 0.2906(12) 0.3258(11) 0.117(8) Uani 1 1 d . . . C8 C 0.2848(15) 0.8582(10) 0.3847(6) 0.055(3) Uani 1 1 d . . . C9 C 0.2240(16) 0.8989(12) 0.4464(6) 0.065(3) Uani 1 1 d . . . C10 C 0.279(2) 0.9844(16) 0.4698(8) 0.092(5) Uani 1 1 d . . . C11 C 0.395(2) 1.0248(13) 0.4333(8) 0.084(5) Uani 1 1 d . . . C12 C 0.450(2) 0.9917(13) 0.3734(8) 0.076(4) Uani 1 1 d . . . C13 C 0.4004(15) 0.9067(11) 0.3486(6) 0.058(3) Uani 1 1 d . . . C14 C 0.0281(14) 0.7283(10) 0.4037(6) 0.053(3) Uani 1 1 d . . . C15 C 0.038(2) 0.6682(14) 0.4656(8) 0.088(5) Uani 1 1 d . . . C16 C -0.099(3) 0.660(2) 0.5059(9) 0.120(8) Uani 1 1 d . . . C17 C -0.233(2) 0.7089(19) 0.4818(15) 0.115(8) Uani 1 1 d . . . C18 C -0.236(2) 0.7649(17) 0.4243(11) 0.096(6) Uani 1 1 d . . . C19 C -0.1050(15) 0.7760(13) 0.3843(8) 0.069(4) Uani 1 1 d . . . C20 C 0.1854(11) 0.8356(8) 0.1274(5) 0.042(2) Uani 1 1 d . . . C21 C 0.1434(14) 0.7618(11) 0.0884(6) 0.054(3) Uani 1 1 d . . . C22 C 0.1427(18) 0.7878(13) 0.0212(7) 0.068(3) Uani 1 1 d . . . C23 C 0.1772(17) 0.8904(14) -0.0111(7) 0.073(4) Uani 1 1 d . . . C24 C 0.2196(15) 0.9682(12) 0.0254(6) 0.060(3) Uani 1 1 d . . . C25 C 0.2197(11) 0.9397(9) 0.0955(5) 0.042(2) Uani 1 1 d . . . C26 C 0.102(2) 0.6531(13) 0.1182(9) 0.084(5) Uani 1 1 d . . . C27 C 0.4768(12) 0.9960(9) 0.1597(5) 0.046(2) Uani 1 1 d . . . C28 C 0.5372(15) 1.0558(13) 0.1970(8) 0.072(4) Uani 1 1 d . . . C29 C 0.6901(19) 1.025(2) 0.2051(9) 0.101(6) Uani 1 1 d . . . C30 C 0.7745(17) 0.9273(19) 0.1763(10) 0.099(6) Uani 1 1 d . . . C31 C 0.7159(17) 0.8669(16) 0.1390(9) 0.087(5) Uani 1 1 d . . . C32 C 0.5633(15) 0.9001(13) 0.1322(8) 0.070(4) Uani 1 1 d . . . C33 C 0.2658(12) 1.1847(9) 0.0901(6) 0.047(2) Uani 1 1 d . . . C34 C 0.3832(17) 1.2017(12) 0.0447(7) 0.066(3) Uani 1 1 d . . . C35 C 0.381(2) 1.2975(13) 0.0035(8) 0.080(4) Uani 1 1 d . . . C36 C 0.254(2) 1.3842(13) 0.0052(8) 0.080(4) Uani 1 1 d . . . C37 C 0.129(2) 1.3650(12) 0.0518(10) 0.086(5) Uani 1 1 d . . . C38 C 0.1374(15) 1.2673(11) 0.0944(8) 0.067(3) Uani 1 1 d . . . H4 H 0.6445 0.3483 0.3977 0.115 Uiso 1 1 calc R . . H5 H 0.6380 0.5103 0.4476 0.113 Uiso 1 1 calc R . . H6 H 0.4754 0.6758 0.4149 0.089 Uiso 1 1 calc R . . H7A H 0.4538 0.3021 0.2788 0.175 Uiso 1 1 calc R . . H7B H 0.3778 0.2590 0.3485 0.175 Uiso 1 1 calc R . . H7C H 0.5533 0.2388 0.3333 0.175 Uiso 1 1 calc R . . H9 H 0.1463 0.8693 0.4720 0.078 Uiso 1 1 calc R . . H10 H 0.2369 1.0135 0.5105 0.111 Uiso 1 1 calc R . . H11 H 0.4370 1.0772 0.4509 0.100 Uiso 1 1 calc R . . H12 H 0.5229 1.0263 0.3475 0.091 Uiso 1 1 calc R . . H13 H 0.4445 0.8812 0.3072 0.069 Uiso 1 1 calc R . . H15 H 0.1297 0.6351 0.4799 0.106 Uiso 1 1 calc R . . H16 H -0.0988 0.6211 0.5482 0.144 Uiso 1 1 calc R . . H17 H -0.3232 0.7012 0.5079 0.138 Uiso 1 1 calc R . . H18 H -0.3278 0.7983 0.4096 0.116 Uiso 1 1 calc R . . H19 H -0.1092 0.8175 0.3430 0.083 Uiso 1 1 calc R . . H22 H 0.1187 0.7359 -0.0040 0.081 Uiso 1 1 calc R . . H23 H 0.1718 0.9068 -0.0566 0.087 Uiso 1 1 calc R . . H24 H 0.2465 1.0352 0.0049 0.072 Uiso 1 1 calc R . . H26A H -0.0044 0.6657 0.1322 0.126 Uiso 1 1 calc R . . H26B H 0.1543 0.6255 0.1561 0.126 Uiso 1 1 calc R . . H26C H 0.1286 0.5976 0.0856 0.126 Uiso 1 1 calc R . . H28 H 0.4771 1.1183 0.2175 0.087 Uiso 1 1 calc R . . H29 H 0.7335 1.0678 0.2290 0.122 Uiso 1 1 calc R . . H30 H 0.8747 0.9035 0.1830 0.119 Uiso 1 1 calc R . . H31 H 0.7753 0.8045 0.1181 0.104 Uiso 1 1 calc R . . H32 H 0.5195 0.8566 0.1087 0.084 Uiso 1 1 calc R . . H34 H 0.4696 1.1448 0.0417 0.080 Uiso 1 1 calc R . . H35 H 0.4656 1.3057 -0.0265 0.095 Uiso 1 1 calc R . . H36 H 0.2509 1.4511 -0.0227 0.096 Uiso 1 1 calc R . . H37 H 0.0403 1.4194 0.0537 0.103 Uiso 1 1 calc R . . H38 H 0.0558 1.2574 0.1259 0.080 Uiso 1 1 calc R . . I1 I 0.17074(16) 0.48945(9) 0.29266(6) 0.0907(4) Uani 1 1 d . . . I2 I -0.08079(13) 1.11965(11) 0.35330(5) 0.0865(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.0548(6) 0.0404(5) 0.0410(6) -0.0008(4) -0.0069(5) -0.0085(5) As2 0.0402(5) 0.0429(5) 0.0391(5) -0.0073(4) -0.0037(4) -0.0048(4) Au1 0.0525(3) 0.0427(2) 0.0404(2) -0.00447(16) -0.00769(17) -0.01027(17) Au2 0.0469(2) 0.0552(3) 0.0432(2) -0.01107(19) -0.00048(17) -0.00161(19) C1 0.054(7) 0.047(6) 0.060(7) -0.003(5) 0.007(6) -0.002(5) C2 0.083(9) 0.053(7) 0.050(7) 0.007(6) 0.007(6) -0.014(6) C3 0.073(9) 0.048(7) 0.083(10) -0.015(7) 0.026(8) -0.013(6) C4 0.093(12) 0.050(8) 0.121(15) 0.016(9) 0.023(11) 0.003(8) C5 0.072(10) 0.070(10) 0.130(16) 0.016(10) -0.021(10) 0.003(8) C6 0.066(8) 0.064(8) 0.087(10) 0.006(7) -0.020(8) 0.000(7) C7 0.17(2) 0.033(7) 0.127(17) -0.014(9) 0.003(14) 0.012(9) C8 0.073(8) 0.045(6) 0.048(6) -0.002(5) -0.026(6) -0.003(5) C9 0.076(9) 0.074(8) 0.049(7) -0.015(6) 0.003(6) -0.026(7) C10 0.141(16) 0.091(12) 0.058(9) -0.021(8) -0.011(10) -0.045(12) C11 0.143(15) 0.068(9) 0.057(8) 0.000(7) -0.022(9) -0.055(10) C12 0.103(11) 0.065(8) 0.068(9) -0.002(7) -0.007(8) -0.040(8) C13 0.067(8) 0.052(6) 0.051(7) -0.004(5) 0.001(6) -0.010(6) C14 0.065(7) 0.044(6) 0.049(6) -0.006(5) -0.008(5) -0.010(5) C15 0.097(12) 0.084(11) 0.073(10) 0.012(9) 0.016(9) -0.022(9) C16 0.17(2) 0.130(17) 0.064(11) 0.006(11) 0.029(12) -0.064(16) C17 0.062(11) 0.091(13) 0.19(3) -0.053(16) 0.024(13) -0.016(10) C18 0.079(11) 0.095(13) 0.110(15) 0.015(12) -0.011(10) -0.020(10) C19 0.056(7) 0.081(9) 0.072(9) -0.005(7) -0.008(6) -0.018(7) C20 0.035(5) 0.035(5) 0.053(6) -0.010(4) -0.001(4) 0.001(4) C21 0.057(7) 0.055(7) 0.052(6) -0.015(5) -0.004(5) -0.008(5) C22 0.091(10) 0.070(8) 0.049(7) -0.016(6) -0.014(7) -0.023(7) C23 0.076(9) 0.101(11) 0.044(7) -0.019(7) -0.013(6) -0.016(8) C24 0.073(8) 0.064(7) 0.045(6) -0.012(5) -0.015(6) -0.013(6) C25 0.035(5) 0.051(6) 0.039(5) -0.009(4) -0.002(4) -0.005(4) C26 0.106(12) 0.059(8) 0.096(12) -0.021(8) -0.034(10) -0.017(8) C27 0.050(6) 0.047(6) 0.043(5) 0.001(4) -0.011(5) -0.010(5) C28 0.053(7) 0.074(9) 0.098(11) -0.016(8) -0.020(7) -0.021(6) C29 0.064(10) 0.155(19) 0.095(13) -0.022(13) -0.030(9) -0.025(11) C30 0.043(7) 0.138(17) 0.098(13) 0.018(12) -0.014(8) 0.012(9) C31 0.050(8) 0.102(13) 0.100(12) -0.014(10) -0.015(8) 0.012(8) C32 0.051(7) 0.075(9) 0.083(10) -0.035(8) -0.005(6) 0.002(6) C33 0.048(6) 0.045(6) 0.050(6) -0.011(5) -0.008(5) -0.008(5) C34 0.073(9) 0.057(7) 0.064(8) -0.017(6) 0.002(7) -0.005(6) C35 0.093(11) 0.067(9) 0.070(9) 0.005(7) 0.002(8) -0.012(8) C36 0.116(13) 0.063(9) 0.066(9) 0.008(7) -0.018(9) -0.031(9) C37 0.091(11) 0.047(7) 0.121(14) -0.006(8) -0.049(11) 0.010(7) C38 0.051(7) 0.054(7) 0.091(10) -0.008(7) -0.018(7) 0.003(6) I1 0.1351(10) 0.0643(6) 0.0850(7) -0.0075(5) -0.0240(7) -0.0399(6) I2 0.0813(6) 0.1009(8) 0.0536(5) -0.0100(5) 0.0147(4) 0.0195(6) _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 As1 C1 1.944(12) . ? As1 C8 1.926(12) . ? As1 C14 1.950(12) . ? As2 C25 1.915(11) . ? As2 C27 1.925(11) . ? As2 C33 1.947(11) . ? Au1 As1 2.4114(12) . ? Au1 Au2 3.2807(7) . ? Au1 C20 2.056(11) . ? Au2 As2 2.3556(11) . ? Au2 I2 2.5367(9) . ? C1 C2 1.374(19) . ? C1 C6 1.37(2) . ? C2 C3 1.371(19) . ? C3 C4 1.40(3) . ? C3 C7 1.51(2) . ? C4 C5 1.35(3) . ? C6 C5 1.39(2) . ? C8 C9 1.388(17) . ? C8 C13 1.395(18) . ? C9 C10 1.39(2) . ? C11 C10 1.35(2) . ? C12 C11 1.31(2) . ? C13 C12 1.372(19) . ? C14 C15 1.385(19) . ? C14 C19 1.332(18) . ? C15 C16 1.41(3) . ? C17 C16 1.38(3) . ? C17 C18 1.28(3) . ? C19 C18 1.37(2) . ? C20 C21 1.398(16) . ? C20 C25 1.418(15) . ? C21 C26 1.48(2) . ? C22 C21 1.366(18) . ? C22 C23 1.41(2) . ? C24 C23 1.403(19) . ? C25 C24 1.427(16) . ? C27 C28 1.346(18) . ? C27 C32 1.374(17) . ? C28 C29 1.41(2) . ? C30 C29 1.39(3) . ? C30 C31 1.34(3) . ? C32 C31 1.40(2) . ? C33 C34 1.347(18) . ? C33 C38 1.369(16) . ? C34 C35 1.34(2) . ? C35 C36 1.39(2) . ? C37 C36 1.42(2) . ? C37 C38 1.37(2) . ? I1 C2 2.117(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag As1 Au1 Au2 92.72(3) . . ? As2 Au2 Au1 71.48(3) . . ? As2 Au2 I2 174.30(4) . . ? C1 As1 Au1 115.8(4) . . ? C1 As1 C14 103.5(5) . . ? C1 C2 I1 117.8(10) . . ? C1 C6 C5 122.8(17) . . ? C2 C1 As1 124.2(11) . . ? C2 C3 C4 116.0(14) . . ? C2 C3 C7 124.9(18) . . ? C3 C2 C1 124.6(15) . . ? C3 C2 I1 117.5(12) . . ? C4 C3 C7 119.2(16) . . ? C4 C5 C6 118.0(19) . . ? C5 C4 C3 122.3(16) . . ? C6 C1 As1 119.8(11) . . ? C6 C1 C2 115.8(13) . . ? C8 As1 Au1 111.3(4) . . ? C8 As1 C1 103.2(6) . . ? C8 As1 C14 103.9(5) . . ? C8 C9 C10 119.9(14) . . ? C9 C8 As1 123.8(11) . . ? C9 C8 C13 117.2(12) . . ? C11 C10 C9 119.8(15) . . ? C11 C12 C13 120.8(14) . . ? C12 C11 C10 121.3(15) . . ? C12 C13 C8 120.7(12) . . ? C13 C8 As1 118.9(9) . . ? C14 As1 Au1 117.5(4) . . ? C14 C15 C16 116.9(19) . . ? C14 C19 C18 121.2(16) . . ? C15 C14 As1 119.4(11) . . ? C17 C16 C15 119.3(19) . . ? C17 C18 C19 120.5(19) . . ? C18 C17 C16 121.4(19) . . ? C19 C14 As1 120.0(10) . . ? C19 C14 C15 120.6(14) . . ? C20 Au1 As1 177.4(3) . . ? C20 Au1 Au2 89.4(3) . . ? C20 C21 C26 121.3(12) . . ? C20 C25 As2 118.5(8) . . ? C20 C25 C24 122.4(11) . . ? C21 C20 Au1 121.5(8) . . ? C21 C20 C25 117.9(10) . . ? C21 C22 C23 122.3(13) . . ? C22 C21 C20 120.3(12) . . ? C22 C21 C26 118.4(13) . . ? C23 C24 C25 117.0(12) . . ? C24 C23 C22 120.0(12) . . ? C24 C25 As2 119.1(9) . . ? C25 As2 Au2 113.5(3) . . ? C25 As2 C27 107.1(4) . . ? C25 As2 C33 104.4(5) . . ? C25 C20 Au1 120.5(8) . . ? C27 As2 Au2 114.5(3) . . ? C27 As2 C33 102.6(5) . . ? C27 C28 C29 120.6(15) . . ? C27 C32 C31 121.0(15) . . ? C28 C27 As2 118.5(10) . . ? C28 C27 C32 119.8(12) . . ? C30 C29 C28 118.0(17) . . ? C30 C31 C32 118.4(16) . . ? C31 C30 C29 122.0(15) . . ? C32 C27 As2 121.6(9) . . ? C33 As2 Au2 113.5(3) . . ? C33 C38 C37 119.8(15) . . ? C34 C33 As2 122.9(9) . . ? C34 C33 C38 119.1(12) . . ? C34 C35 C36 120.9(15) . . ? C35 C34 C33 122.8(14) . . ? C35 C36 C37 116.2(13) . . ? C38 C33 As2 118.0(10) . . ? C38 C37 C36 121.1(14) . . ? I2 Au2 Au1 113.57(3) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 3.312 _refine_diff_density_min -1.393 _refine_diff_density_rms 0.302 #===END data_compound15 _database_code_depnum_ccdc_archive 'CCDC 290397' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H32 As2 Au2 I2' _chemical_formula_weight 1286.21 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.8379(15) _cell_length_b 14.0363(15) _cell_length_c 17.4504(17) _cell_angle_alpha 90.00 _cell_angle_beta 111.217(3) _cell_angle_gamma 90.00 _cell_volume 3616.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2360 _exptl_absorpt_coefficient_mu 11.653 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS Sheldrick 1996' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12188 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0635 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 28.28 _reflns_number_total 8316 _reflns_number_gt 6276 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8316 _refine_ls_number_parameters 399 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0774 _refine_ls_wR_factor_gt 0.0733 _refine_ls_goodness_of_fit_ref 0.822 _refine_ls_restrained_S_all 0.822 _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 As1 As 0.40323(4) 0.00560(5) 0.21997(4) 0.03411(14) Uani 1 1 d . . . As2 As 0.43655(4) 0.28986(5) 0.08573(4) 0.03432(14) Uani 1 1 d . . . Au1 Au 0.253962(15) 0.112402(16) 0.025099(13) 0.03029(7) Uani 1 1 d . . . Au2 Au 0.430059(17) 0.146345(18) 0.156236(15) 0.03830(7) Uani 1 1 d . . . C1 C 0.2333(4) -0.0157(4) 0.0803(3) 0.0333(13) Uani 1 1 d . . . C2 C 0.1533(4) -0.0672(4) 0.0361(4) 0.0363(14) Uani 1 1 d . . . C3 C 0.1369(5) -0.1545(5) 0.0662(4) 0.0432(16) Uani 1 1 d . . . C4 C 0.1981(4) -0.1939(5) 0.1362(4) 0.0445(16) Uani 1 1 d . . . C5 C 0.2755(5) -0.1448(5) 0.1799(4) 0.0421(15) Uani 1 1 d . . . C6 C 0.2924(4) -0.0569(4) 0.1529(3) 0.0318(13) Uani 1 1 d . . . C7 C 0.0860(4) -0.0297(5) -0.0418(4) 0.0497(17) Uani 1 1 d . . . C8 C 0.2646(4) 0.2351(4) -0.0412(3) 0.0330(13) Uani 1 1 d . . . C9 C 0.1943(4) 0.2516(5) -0.1187(4) 0.0479(17) Uani 1 1 d . . . C10 C 0.2013(5) 0.3270(6) -0.1660(4) 0.058(2) Uani 1 1 d . . . C11 C 0.2717(5) 0.3886(5) -0.1433(4) 0.057(2) Uani 1 1 d . . . C12 C 0.3407(5) 0.3737(5) -0.0683(4) 0.0525(19) Uani 1 1 d . . . C13 C 0.3360(4) 0.2996(5) -0.0188(4) 0.0369(14) Uani 1 1 d . . . C14 C 0.1131(5) 0.1882(6) -0.1486(5) 0.074(3) Uani 1 1 d . . . C15 C 0.4336(4) 0.4033(5) 0.1465(4) 0.0367(14) Uani 1 1 d . . . C16 C 0.4095(4) 0.3950(5) 0.2155(4) 0.0422(15) Uani 1 1 d . . . C17 C 0.4080(5) 0.4748(6) 0.2618(4) 0.0503(18) Uani 1 1 d . . . C18 C 0.4306(5) 0.5633(6) 0.2404(4) 0.0576(19) Uani 1 1 d . . . C19 C 0.4537(6) 0.5717(6) 0.1717(5) 0.069(2) Uani 1 1 d . . . C20 C 0.4551(5) 0.4924(5) 0.1255(4) 0.0553(19) Uani 1 1 d . . . C21 C 0.5422(4) 0.3003(4) 0.0562(4) 0.0346(13) Uani 1 1 d . . . C22 C 0.5465(5) 0.2428(5) -0.0052(5) 0.0539(19) Uani 1 1 d . . . C23 C 0.6237(6) 0.2419(6) -0.0258(5) 0.069(2) Uani 1 1 d . . . C24 C 0.6953(6) 0.2987(6) 0.0155(6) 0.065(2) Uani 1 1 d . . . C25 C 0.6930(5) 0.3566(7) 0.0770(6) 0.068(2) Uani 1 1 d . . . C26 C 0.6160(5) 0.3561(6) 0.0989(5) 0.0537(19) Uani 1 1 d . . . C27 C 0.4942(4) -0.0927(5) 0.2470(3) 0.0370(14) Uani 1 1 d . . . C28 C 0.5053(4) -0.1560(5) 0.3114(4) 0.0426(16) Uani 1 1 d . . . C29 C 0.5683(5) -0.2294(5) 0.3267(4) 0.0521(18) Uani 1 1 d . . . C30 C 0.6199(5) -0.2384(6) 0.2783(5) 0.063(2) Uani 1 1 d . . . C31 C 0.6116(6) -0.1749(7) 0.2159(5) 0.068(2) Uani 1 1 d . . . C32 C 0.5485(5) -0.1043(6) 0.2002(4) 0.0537(19) Uani 1 1 d . . . C33 C 0.3918(4) 0.0326(4) 0.3251(3) 0.0367(14) Uani 1 1 d . . . C34 C 0.3237(5) -0.0017(6) 0.3465(4) 0.0514(19) Uani 1 1 d . . . C35 C 0.3194(5) 0.0206(7) 0.4219(5) 0.064(2) Uani 1 1 d . . . C36 C 0.3857(5) 0.0728(6) 0.4775(4) 0.059(2) Uani 1 1 d . . . C37 C 0.4560(5) 0.1083(5) 0.4567(4) 0.0512(18) Uani 1 1 d . . . C38 C 0.4605(5) 0.0891(5) 0.3806(4) 0.0461(16) Uani 1 1 d . . . H3 H 0.0833 -0.1867 0.0381 0.052 Uiso 1 1 calc R . . H4 H 0.1871 -0.2536 0.1540 0.053 Uiso 1 1 calc R . . H5 H 0.3168 -0.1708 0.2279 0.051 Uiso 1 1 calc R . . H7A H 0.0346 -0.0715 -0.0605 0.075 Uiso 1 1 calc R . . H7B H 0.1131 -0.0259 -0.0827 0.075 Uiso 1 1 calc R . . H7C H 0.0668 0.0327 -0.0323 0.075 Uiso 1 1 calc R . . H10 H 0.1549 0.3363 -0.2165 0.070 Uiso 1 1 calc R . . H11 H 0.2737 0.4392 -0.1770 0.068 Uiso 1 1 calc R . . H12 H 0.3905 0.4142 -0.0514 0.063 Uiso 1 1 calc R . . H14A H 0.0704 0.2134 -0.1988 0.111 Uiso 1 1 calc R . . H14B H 0.0855 0.1851 -0.1079 0.111 Uiso 1 1 calc R . . H14C H 0.1312 0.1255 -0.1583 0.111 Uiso 1 1 calc R . . H16 H 0.3943 0.3358 0.2305 0.051 Uiso 1 1 calc R . . H17 H 0.3917 0.4687 0.3077 0.060 Uiso 1 1 calc R . . H18 H 0.4301 0.6166 0.2719 0.069 Uiso 1 1 calc R . . H19 H 0.4685 0.6311 0.1565 0.082 Uiso 1 1 calc R . . H20 H 0.4708 0.4992 0.0794 0.066 Uiso 1 1 calc R . . H22 H 0.4976 0.2039 -0.0335 0.065 Uiso 1 1 calc R . . H23 H 0.6262 0.2024 -0.0678 0.083 Uiso 1 1 calc R . . H24 H 0.7465 0.2978 0.0013 0.078 Uiso 1 1 calc R . . H25 H 0.7418 0.3961 0.1042 0.081 Uiso 1 1 calc R . . H26 H 0.6147 0.3935 0.1424 0.064 Uiso 1 1 calc R . . H28 H 0.4705 -0.1493 0.3440 0.051 Uiso 1 1 calc R . . H29 H 0.5756 -0.2720 0.3694 0.063 Uiso 1 1 calc R . . H30 H 0.6610 -0.2884 0.2880 0.076 Uiso 1 1 calc R . . H31 H 0.6484 -0.1801 0.1849 0.081 Uiso 1 1 calc R . . H32 H 0.5415 -0.0626 0.1570 0.064 Uiso 1 1 calc R . . H34 H 0.2795 -0.0404 0.3102 0.062 Uiso 1 1 calc R . . H35 H 0.2705 -0.0004 0.4349 0.077 Uiso 1 1 calc R . . H36 H 0.3839 0.0845 0.5293 0.071 Uiso 1 1 calc R . . H37 H 0.5006 0.1455 0.4942 0.061 Uiso 1 1 calc R . . H38 H 0.5077 0.1128 0.3664 0.055 Uiso 1 1 calc R . . I1 I 0.34225(4) 0.01432(4) -0.04757(4) 0.07224(18) Uani 1 1 d . . . I2 I 0.17313(3) 0.20983(4) 0.10558(3) 0.05617(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.0370(4) 0.0304(3) 0.0351(3) 0.0038(3) 0.0132(3) -0.0045(3) As2 0.0351(4) 0.0301(3) 0.0393(3) 0.0034(3) 0.0153(3) -0.0057(3) Au1 0.03154(13) 0.02808(12) 0.03301(11) 0.00010(9) 0.01378(9) -0.00385(10) Au2 0.03786(15) 0.03273(14) 0.04184(13) 0.00703(10) 0.01144(11) -0.00715(11) C1 0.040(4) 0.031(3) 0.037(3) -0.003(3) 0.024(3) -0.003(3) C2 0.036(3) 0.031(3) 0.044(3) -0.007(3) 0.016(3) -0.013(3) C3 0.045(4) 0.039(4) 0.048(4) -0.009(3) 0.020(3) -0.010(3) C4 0.056(4) 0.035(4) 0.048(4) -0.005(3) 0.026(3) -0.014(3) C5 0.050(4) 0.036(4) 0.041(3) 0.000(3) 0.017(3) -0.004(3) C6 0.037(3) 0.030(3) 0.031(3) -0.003(2) 0.015(2) -0.005(3) C7 0.044(4) 0.046(4) 0.056(4) 0.001(3) 0.014(3) -0.016(3) C8 0.035(3) 0.030(3) 0.038(3) 0.001(2) 0.017(3) 0.002(3) C9 0.040(4) 0.049(4) 0.047(4) 0.008(3) 0.007(3) -0.003(3) C10 0.058(5) 0.057(5) 0.047(4) 0.013(4) 0.003(3) -0.004(4) C11 0.063(5) 0.046(5) 0.054(4) 0.020(4) 0.012(4) -0.009(4) C12 0.055(5) 0.040(4) 0.055(4) 0.010(3) 0.012(3) -0.015(3) C13 0.040(4) 0.034(4) 0.036(3) 0.005(3) 0.014(3) -0.002(3) C14 0.062(5) 0.064(6) 0.065(5) 0.017(4) -0.015(4) -0.025(5) C15 0.032(3) 0.038(4) 0.040(3) 0.000(3) 0.013(3) -0.008(3) C16 0.040(4) 0.046(4) 0.043(3) 0.000(3) 0.018(3) -0.005(3) C17 0.046(4) 0.061(5) 0.045(4) -0.012(4) 0.017(3) -0.005(4) C18 0.068(5) 0.048(5) 0.058(4) -0.013(4) 0.024(4) 0.000(4) C19 0.102(7) 0.034(4) 0.081(6) 0.001(4) 0.045(5) -0.017(5) C20 0.090(6) 0.033(4) 0.055(4) 0.007(3) 0.040(4) 0.000(4) C21 0.030(3) 0.030(3) 0.047(3) 0.007(3) 0.018(3) -0.002(3) C22 0.060(5) 0.044(4) 0.070(5) -0.012(4) 0.037(4) -0.018(4) C23 0.089(6) 0.047(5) 0.092(6) -0.002(5) 0.059(5) 0.005(5) C24 0.055(5) 0.051(5) 0.108(7) 0.010(5) 0.054(5) 0.007(4) C25 0.039(5) 0.070(6) 0.094(6) -0.006(5) 0.023(4) -0.008(4) C26 0.046(4) 0.056(5) 0.062(4) -0.010(4) 0.022(4) -0.014(4) C27 0.041(4) 0.037(4) 0.033(3) 0.000(3) 0.013(3) -0.004(3) C28 0.047(4) 0.039(4) 0.041(3) 0.002(3) 0.015(3) -0.005(3) C29 0.068(5) 0.036(4) 0.051(4) 0.010(3) 0.020(4) 0.010(4) C30 0.067(5) 0.049(5) 0.071(5) -0.002(4) 0.021(4) 0.019(4) C31 0.073(6) 0.073(6) 0.072(5) 0.003(5) 0.045(5) 0.016(5) C32 0.062(5) 0.057(5) 0.048(4) 0.009(4) 0.027(4) -0.001(4) C33 0.038(4) 0.031(3) 0.037(3) 0.003(3) 0.009(3) 0.008(3) C34 0.040(4) 0.065(5) 0.053(4) -0.016(4) 0.022(3) -0.011(4) C35 0.059(5) 0.081(7) 0.059(5) -0.014(4) 0.031(4) -0.004(5) C36 0.066(5) 0.068(6) 0.040(4) -0.003(4) 0.016(4) 0.022(4) C37 0.062(5) 0.033(4) 0.045(4) -0.012(3) 0.004(3) 0.007(3) C38 0.048(4) 0.039(4) 0.049(4) -0.001(3) 0.014(3) -0.001(3) I1 0.1083(5) 0.0486(3) 0.0973(4) 0.0073(3) 0.0822(4) 0.0128(3) I2 0.0671(3) 0.0468(3) 0.0693(3) -0.0085(2) 0.0422(3) 0.0047(2) _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 As1 C6 1.933(6) . ? As1 C27 1.926(6) . ? As1 C33 1.944(6) . ? As2 C13 1.944(6) . ? As2 C15 1.922(7) . ? As2 C21 1.927(6) . ? Au1 Au2 2.9365(4) . ? Au1 C1 2.120(6) . ? Au1 C8 2.116(6) . ? Au1 I1 2.5965(5) . ? Au1 I2 2.6043(5) . ? Au2 As1 2.3795(7) . ? Au2 As2 2.3820(7) . ? C1 C2 1.419(8) . ? C1 C6 1.399(8) . ? C2 C3 1.393(9) . ? C2 C7 1.487(9) . ? C4 C3 1.372(9) . ? C5 C4 1.373(9) . ? C6 C5 1.381(9) . ? C8 C9 1.425(8) . ? C8 C13 1.390(8) . ? C10 C9 1.371(10) . ? C10 C11 1.352(10) . ? C11 C12 1.383(9) . ? C13 C12 1.372(9) . ? C14 C9 1.494(9) . ? C15 C16 1.393(8) . ? C15 C20 1.380(9) . ? C17 C16 1.386(9) . ? C18 C17 1.380(11) . ? C19 C18 1.379(10) . ? C19 C20 1.378(10) . ? C21 C22 1.362(9) . ? C23 C22 1.393(10) . ? C23 C24 1.360(11) . ? C25 C24 1.357(11) . ? C25 C26 1.405(10) . ? C26 C21 1.380(9) . ? C27 C28 1.394(8) . ? C28 C29 1.391(9) . ? C30 C29 1.377(10) . ? C31 C30 1.377(11) . ? C31 C32 1.363(10) . ? C32 C27 1.393(9) . ? C33 C34 1.352(9) . ? C33 C38 1.410(9) . ? C35 C34 1.379(9) . ? C35 C36 1.358(11) . ? C36 C37 1.383(10) . ? C38 C37 1.381(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag As1 Au2 As2 172.71(2) . . ? As1 Au2 Au1 87.115(17) . . ? As2 Au2 Au1 86.621(17) . . ? C1 Au1 Au2 92.46(16) . . ? C1 Au1 C8 174.2(2) . . ? C1 Au1 I1 88.34(15) . . ? C1 Au1 I2 90.78(15) . . ? C1 C2 C7 121.3(6) . . ? C1 C6 As1 121.6(4) . . ? C2 C1 Au1 116.1(4) . . ? C3 C2 C1 119.6(6) . . ? C3 C2 C7 119.1(6) . . ? C4 C3 C2 121.5(6) . . ? C4 C5 C6 120.2(6) . . ? C5 C4 C3 119.5(6) . . ? C5 C6 As1 116.4(5) . . ? C5 C6 C1 122.0(6) . . ? C6 As1 Au2 111.74(17) . . ? C6 As1 C33 106.6(2) . . ? C6 C1 Au1 126.8(4) . . ? C6 C1 C2 117.0(5) . . ? C8 Au1 Au2 93.04(16) . . ? C8 Au1 I1 90.04(15) . . ? C8 Au1 I2 91.13(15) . . ? C8 C9 C14 120.9(6) . . ? C8 C13 As2 121.7(4) . . ? C9 C8 Au1 117.5(5) . . ? C9 C10 C11 123.7(7) . . ? C10 C9 C8 119.4(6) . . ? C10 C9 C14 119.7(6) . . ? C10 C11 C12 117.8(7) . . ? C12 C13 As2 115.6(5) . . ? C12 C13 C8 122.7(6) . . ? C13 As2 Au2 111.74(19) . . ? C13 C12 C11 120.4(7) . . ? C13 C8 Au1 126.4(4) . . ? C13 C8 C9 116.0(6) . . ? C15 As2 Au2 113.66(18) . . ? C15 As2 C13 106.5(3) . . ? C15 As2 C21 106.3(3) . . ? C15 C16 C17 120.3(7) . . ? C15 C20 C19 121.3(7) . . ? C16 C15 As2 118.5(5) . . ? C17 C18 C19 119.2(7) . . ? C18 C17 C16 120.5(7) . . ? C18 C19 C20 120.3(7) . . ? C20 C15 As2 123.2(5) . . ? C20 C15 C16 118.3(6) . . ? C21 As2 Au2 113.97(18) . . ? C21 As2 C13 103.9(3) . . ? C21 C22 C23 120.5(7) . . ? C21 C26 C25 120.3(7) . . ? C22 C21 As2 117.4(5) . . ? C22 C21 C26 119.2(6) . . ? C24 C23 C22 119.9(8) . . ? C24 C25 C26 119.1(8) . . ? C25 C24 C23 121.0(7) . . ? C26 C21 As2 123.1(5) . . ? C27 As1 Au2 117.68(18) . . ? C27 As1 C6 104.9(3) . . ? C27 As1 C33 103.0(2) . . ? C27 C28 C29 120.0(6) . . ? C28 C27 As1 121.3(5) . . ? C28 C27 C32 118.2(6) . . ? C28 C29 C30 119.6(7) . . ? C31 C30 C29 121.2(7) . . ? C31 C32 C27 122.1(7) . . ? C32 C27 As1 120.5(5) . . ? C32 C31 C30 118.8(7) . . ? C33 As1 Au2 111.87(19) . . ? C33 C34 C35 120.2(7) . . ? C34 C33 As1 123.2(5) . . ? C34 C33 C38 120.3(6) . . ? C35 C36 C37 119.8(7) . . ? C36 C35 C34 120.7(7) . . ? C36 C37 C38 120.5(7) . . ? C37 C38 C33 118.4(6) . . ? C38 C33 As1 116.5(5) . . ? I1 Au1 Au2 86.512(19) . . ? I1 Au1 I2 176.81(2) . . ? I2 Au1 Au2 90.467(16) . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 1.703 _refine_diff_density_min -1.268 _refine_diff_density_rms 0.173 #===END