# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Thomas Gray' 'Allen Hunter' 'David V. Partyka' 'James B. UpdegraffIII' 'Matthias Zeller' _publ_contact_author_name 'Thomas Gray' _publ_contact_author_email TGRAY@CASE.EDU _publ_section_title ; Gold(I) Halide Complexes of Bis(diphenylphosphine)diphenyl Ether Ligands: A Balance of Ligand Strain and Non-Covalent Interactions ; # Attachment 'gray1.cif' data_08mz221_0m _database_code_depnum_ccdc_archive 'CCDC 750030' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H29 Au2 Br2 Cl3 O P2' _chemical_formula_weight 1211.65 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' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 '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 8.981(3) _cell_length_b 20.448(7) _cell_length_c 19.993(7) _cell_angle_alpha 90.00 _cell_angle_beta 102.957(5) _cell_angle_gamma 90.00 _cell_volume 3578(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7478 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 31.88 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.249 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 10.769 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.201 _exptl_absorpt_correction_T_max 0.524 _exptl_absorpt_process_details 'Apex2 v2008.2-4 (Bruker, 2008)' _exptl_special_details ; The crystal under investigation was found to be pseudo-merohedrally twinned. Application of the twin law 1 0 0 0 -1 0 -1 0 -1 resulted in a BASF value of 0.322(1). All atoms were restrained to have similar ADPs (SIMU 0.01). ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 28618 _diffrn_reflns_av_R_equivalents 0.1144 _diffrn_reflns_av_sigmaI/netI 0.1333 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.00 _diffrn_reflns_theta_max 28.28 _reflns_number_total 8965 _reflns_number_gt 6440 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2008.2-4 (Bruker, 2008)' _computing_cell_refinement 'Apex2 v2008.2-4 ' _computing_data_reduction 'Apex2 v2008.2-4 ' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.0891P)^2^+63.8405P] 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 8965 _refine_ls_number_parameters 425 _refine_ls_number_restraints 234 _refine_ls_R_factor_all 0.1223 _refine_ls_R_factor_gt 0.0813 _refine_ls_wR_factor_ref 0.1974 _refine_ls_wR_factor_gt 0.1749 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.82966(8) 0.78722(4) 0.28744(4) 0.02233(18) Uani 1 1 d . . . Au2 Au 0.66821(8) 0.66034(4) 0.28930(4) 0.02258(18) Uani 1 1 d . . . C1 C 0.733(2) 0.9261(10) 0.3420(10) 0.029(3) Uani 1 1 d U . . C2 C 0.823(2) 0.9505(10) 0.2982(10) 0.031(4) Uani 1 1 d U . . H2 H 0.8931 0.9222 0.2832 0.037 Uiso 1 1 calc R . . C3 C 0.811(3) 1.0162(11) 0.2763(11) 0.038(4) Uani 1 1 d U . . H3 H 0.8709 1.0321 0.2462 0.045 Uiso 1 1 calc R . . C4 C 0.711(3) 1.0571(11) 0.2991(10) 0.035(4) Uani 1 1 d U . . H4 H 0.7064 1.1019 0.2865 0.042 Uiso 1 1 calc R . . C5 C 0.615(3) 1.0330(11) 0.3412(11) 0.034(4) Uani 1 1 d U . . H5 H 0.5397 1.0607 0.3529 0.041 Uiso 1 1 calc R . . C6 C 0.630(2) 0.9715(10) 0.3645(10) 0.025(3) Uani 1 1 d U . . H6 H 0.5725 0.9572 0.3962 0.031 Uiso 1 1 calc R . . C7 C 0.567(2) 0.8244(10) 0.3900(10) 0.023(3) Uani 1 1 d U . . C8 C 0.549(2) 0.8299(11) 0.4559(10) 0.027(3) Uani 1 1 d U . . H8 H 0.6329 0.8412 0.4919 0.033 Uiso 1 1 calc R . . C9 C 0.407(2) 0.8189(11) 0.4697(12) 0.033(4) Uani 1 1 d U . . H9 H 0.3947 0.8204 0.5157 0.039 Uiso 1 1 calc R . . C10 C 0.281(3) 0.8055(11) 0.4159(11) 0.035(4) Uani 1 1 d U . . H10 H 0.1825 0.7987 0.4252 0.041 Uiso 1 1 calc R . . C11 C 0.299(2) 0.8025(11) 0.3521(11) 0.034(4) Uani 1 1 d U . . H11 H 0.2124 0.7956 0.3157 0.040 Uiso 1 1 calc R . . C12 C 0.439(2) 0.8089(10) 0.3374(11) 0.028(3) Uani 1 1 d U . . H12 H 0.4499 0.8029 0.2917 0.034 Uiso 1 1 calc R . . C13 C 0.888(2) 0.8383(10) 0.4479(9) 0.020(3) Uani 1 1 d U . . C14 C 0.972(2) 0.8920(10) 0.4761(9) 0.024(3) Uani 1 1 d U . . H14 H 0.9540 0.9336 0.4546 0.029 Uiso 1 1 calc R . . C15 C 1.082(2) 0.8843(10) 0.5358(9) 0.022(3) Uani 1 1 d U . . H15 H 1.1397 0.9212 0.5558 0.027 Uiso 1 1 calc R . . C16 C 1.110(2) 0.8240(11) 0.5672(9) 0.026(3) Uani 1 1 d U . . H16 H 1.1865 0.8197 0.6082 0.031 Uiso 1 1 calc R . . C17 C 1.027(2) 0.7702(11) 0.5392(9) 0.026(3) Uani 1 1 d U . . H17 H 1.0496 0.7282 0.5593 0.032 Uiso 1 1 calc R . . C18 C 0.910(2) 0.7785(9) 0.4804(8) 0.019(3) Uani 1 1 d U . . C19 C 0.769(2) 0.6784(10) 0.4862(10) 0.022(3) Uani 1 1 d U . . C20 C 0.728(2) 0.6921(11) 0.5475(10) 0.027(3) Uani 1 1 d U . . H20 H 0.7357 0.7353 0.5656 0.032 Uiso 1 1 calc R . . C21 C 0.676(2) 0.6413(11) 0.5814(10) 0.029(3) Uani 1 1 d U . . H21 H 0.6503 0.6495 0.6242 0.035 Uiso 1 1 calc R . . C22 C 0.661(2) 0.5804(11) 0.5553(11) 0.031(4) Uani 1 1 d U . . H22 H 0.6211 0.5464 0.5786 0.038 Uiso 1 1 calc R . . C23 C 0.703(2) 0.5677(11) 0.4941(10) 0.027(3) Uani 1 1 d U . . H23 H 0.6957 0.5242 0.4770 0.033 Uiso 1 1 calc R . . C24 C 0.757(2) 0.6160(11) 0.4571(10) 0.025(3) Uani 1 1 d U . . C25 C 1.013(2) 0.6192(11) 0.3954(10) 0.029(3) Uani 1 1 d U . . C26 C 1.083(2) 0.6319(12) 0.3439(11) 0.031(3) Uani 1 1 d U . . H26 H 1.0238 0.6337 0.2981 0.037 Uiso 1 1 calc R . . C27 C 1.240(2) 0.6423(11) 0.3561(11) 0.031(4) Uani 1 1 d U . . H27 H 1.2877 0.6542 0.3200 0.037 Uiso 1 1 calc R . . C28 C 1.323(2) 0.6349(12) 0.4215(11) 0.035(4) Uani 1 1 d U . . H28 H 1.4302 0.6417 0.4310 0.042 Uiso 1 1 calc R . . C29 C 1.255(2) 0.6177(12) 0.4744(12) 0.035(4) Uani 1 1 d U . . H29 H 1.3151 0.6099 0.5192 0.042 Uiso 1 1 calc R . . C30 C 1.099(2) 0.6121(12) 0.4611(11) 0.033(4) Uani 1 1 d U . . H30 H 1.0496 0.6032 0.4976 0.039 Uiso 1 1 calc R . . C31 C 0.786(2) 0.5164(11) 0.3600(10) 0.029(4) Uani 1 1 d U . . C32 C 0.908(3) 0.4737(10) 0.3716(10) 0.028(3) Uani 1 1 d U . . H32 H 1.0076 0.4901 0.3904 0.033 Uiso 1 1 calc R . . C33 C 0.891(3) 0.4100(10) 0.3571(10) 0.031(4) Uani 1 1 d U . . H33 H 0.9773 0.3821 0.3642 0.037 Uiso 1 1 calc R . . C34 C 0.745(3) 0.3846(10) 0.3315(10) 0.030(4) Uani 1 1 d U . . H34 H 0.7297 0.3393 0.3218 0.036 Uiso 1 1 calc R . . C35 C 0.622(3) 0.4284(11) 0.3205(10) 0.036(4) Uani 1 1 d U . . H35 H 0.5221 0.4119 0.3028 0.043 Uiso 1 1 calc R . . C36 C 0.639(3) 0.4943(11) 0.3343(10) 0.035(4) Uani 1 1 d U . . H36 H 0.5538 0.5231 0.3264 0.042 Uiso 1 1 calc R . . C37 C 0.813(3) 0.5229(13) 0.1168(10) 0.041(5) Uani 1 1 d U . . H37 H 0.9186 0.5151 0.1105 0.050 Uiso 1 1 calc R . . Cl1 Cl 0.7861(8) 0.4701(4) 0.1825(3) 0.0536(18) Uani 1 1 d . . . Cl2 Cl 0.8049(10) 0.6033(4) 0.1418(4) 0.062(2) Uani 1 1 d . . . Cl3 Cl 0.6918(8) 0.5055(4) 0.0408(3) 0.0519(17) Uani 1 1 d U . . Br1 Br 0.9627(2) 0.74878(11) 0.20352(10) 0.0293(4) Uani 1 1 d . . . Br2 Br 0.5017(2) 0.71121(11) 0.19153(10) 0.0321(5) Uani 1 1 d . . . O1 O 0.8242(14) 0.7255(7) 0.4483(6) 0.022(2) Uani 1 1 d U . . P1 P 0.7454(5) 0.8429(3) 0.3677(2) 0.0216(10) Uani 1 1 d . . . P2 P 0.8089(6) 0.6042(2) 0.3768(2) 0.0191(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.0190(3) 0.0239(4) 0.0231(3) 0.0001(3) 0.0028(3) -0.0025(3) Au2 0.0141(3) 0.0207(4) 0.0286(3) 0.0015(3) -0.0043(3) -0.0007(3) C1 0.027(7) 0.020(7) 0.035(7) 0.003(6) -0.004(6) -0.001(6) C2 0.030(7) 0.023(7) 0.037(7) -0.002(6) 0.001(6) -0.005(6) C3 0.041(8) 0.029(8) 0.040(7) 0.000(6) -0.001(7) -0.006(7) C4 0.039(8) 0.025(8) 0.035(7) 0.001(6) -0.005(6) -0.002(7) C5 0.031(7) 0.026(8) 0.039(7) 0.001(6) -0.003(6) -0.001(7) C6 0.027(7) 0.016(7) 0.030(7) -0.002(6) 0.000(6) -0.001(6) C7 0.016(6) 0.020(7) 0.035(7) 0.006(6) 0.006(6) -0.003(6) C8 0.017(6) 0.029(8) 0.037(7) 0.005(6) 0.008(6) 0.004(6) C9 0.016(7) 0.035(8) 0.047(7) -0.001(7) 0.006(6) 0.001(6) C10 0.018(7) 0.038(8) 0.048(7) 0.000(7) 0.009(6) -0.002(7) C11 0.023(7) 0.032(8) 0.045(7) 0.000(7) 0.005(6) -0.007(7) C12 0.019(7) 0.026(8) 0.039(7) 0.003(6) 0.005(6) -0.003(6) C13 0.014(6) 0.020(7) 0.024(6) -0.003(5) 0.003(5) 0.000(6) C14 0.012(6) 0.027(7) 0.032(6) 0.001(6) 0.002(5) 0.001(6) C15 0.007(6) 0.034(8) 0.025(6) 0.003(6) 0.003(5) 0.002(6) C16 0.015(6) 0.038(8) 0.025(6) 0.005(6) 0.008(5) 0.006(6) C17 0.022(7) 0.032(8) 0.025(6) 0.004(6) 0.005(5) 0.008(6) C18 0.014(5) 0.022(6) 0.021(5) 0.002(5) 0.006(5) -0.002(5) C19 0.009(5) 0.025(6) 0.031(6) 0.001(5) 0.002(5) -0.001(5) C20 0.016(6) 0.030(7) 0.034(6) 0.000(6) 0.005(6) -0.008(6) C21 0.017(7) 0.034(8) 0.037(7) -0.004(6) 0.007(6) -0.011(6) C22 0.022(7) 0.032(8) 0.040(7) -0.003(6) 0.006(6) -0.003(7) C23 0.017(6) 0.023(7) 0.041(7) -0.003(6) 0.005(6) -0.004(6) C24 0.014(6) 0.027(7) 0.032(7) 0.000(6) 0.001(5) 0.003(6) C25 0.014(6) 0.037(8) 0.037(7) -0.003(6) 0.007(6) -0.003(6) C26 0.015(7) 0.040(8) 0.038(7) 0.002(7) 0.009(6) 0.001(6) C27 0.016(7) 0.038(8) 0.041(7) 0.002(7) 0.009(6) 0.002(6) C28 0.018(7) 0.039(8) 0.045(7) 0.000(7) 0.003(6) 0.006(7) C29 0.019(7) 0.036(8) 0.047(7) 0.004(7) 0.001(6) 0.007(7) C30 0.018(7) 0.038(8) 0.041(7) 0.000(7) 0.006(6) 0.003(7) C31 0.029(7) 0.021(8) 0.032(7) -0.005(6) -0.003(6) -0.001(6) C32 0.031(7) 0.016(7) 0.032(6) -0.006(6) -0.001(6) 0.005(6) C33 0.038(7) 0.016(7) 0.034(7) 0.002(6) 0.000(6) 0.007(6) C34 0.041(8) 0.012(7) 0.031(7) -0.001(6) -0.003(6) 0.000(6) C35 0.037(8) 0.028(8) 0.038(7) -0.003(6) -0.003(6) -0.005(7) C36 0.035(8) 0.029(8) 0.034(7) -0.007(6) -0.005(6) -0.004(7) C37 0.039(11) 0.062(13) 0.024(9) -0.014(9) 0.010(8) -0.012(11) Cl1 0.038(3) 0.072(5) 0.049(3) 0.021(3) 0.006(3) -0.010(3) Cl2 0.081(6) 0.043(4) 0.067(4) -0.018(3) 0.025(4) -0.003(4) Cl3 0.045(4) 0.061(5) 0.046(3) -0.005(3) 0.002(3) -0.011(3) Br1 0.0297(10) 0.0350(12) 0.0249(9) -0.0025(8) 0.0095(8) -0.0006(9) Br2 0.0228(10) 0.0274(12) 0.0374(10) 0.0025(9) -0.0117(8) -0.0004(9) O1 0.012(5) 0.023(6) 0.026(5) -0.001(5) -0.004(4) -0.005(4) P1 0.016(2) 0.020(3) 0.027(2) -0.001(2) -0.0004(18) -0.002(2) P2 0.016(2) 0.008(2) 0.030(2) 0.0010(18) -0.0013(18) 0.0022(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.234(5) . ? Au1 Br1 2.400(2) . ? Au1 Au2 2.9764(13) . ? Au2 P2 2.233(5) . ? Au2 Br2 2.414(2) . ? C1 C2 1.41(3) . ? C1 C6 1.45(3) . ? C1 P1 1.77(2) . ? C2 C3 1.41(3) . ? C2 H2 0.9500 . ? C3 C4 1.37(3) . ? C3 H3 0.9500 . ? C4 C5 1.42(3) . ? C4 H4 0.9500 . ? C5 C6 1.34(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.37(3) . ? C7 C12 1.41(3) . ? C7 P1 1.80(2) . ? C8 C9 1.38(3) . ? C8 H8 0.9500 . ? C9 C10 1.40(3) . ? C9 H9 0.9500 . ? C10 C11 1.32(3) . ? C10 H10 0.9500 . ? C11 C12 1.36(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.38(3) . ? C13 C18 1.38(3) . ? C13 P1 1.817(17) . ? C14 C15 1.38(2) . ? C14 H14 0.9500 . ? C15 C16 1.38(3) . ? C15 H15 0.9500 . ? C16 C17 1.37(3) . ? C16 H16 0.9500 . ? C17 C18 1.40(2) . ? C17 H17 0.9500 . ? C18 O1 1.40(2) . ? C19 C20 1.38(3) . ? C19 O1 1.38(2) . ? C19 C24 1.40(3) . ? C20 C21 1.38(3) . ? C20 H20 0.9500 . ? C21 C22 1.35(3) . ? C21 H21 0.9500 . ? C22 C23 1.38(3) . ? C22 H22 0.9500 . ? C23 C24 1.38(3) . ? C23 H23 0.9500 . ? C24 P2 1.79(2) . ? C25 C26 1.35(3) . ? C25 C30 1.37(3) . ? C25 P2 1.81(2) . ? C26 C27 1.39(3) . ? C26 H26 0.9500 . ? C27 C28 1.36(3) . ? C27 H27 0.9500 . ? C28 C29 1.38(3) . ? C28 H28 0.9500 . ? C29 C30 1.37(3) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.38(3) . ? C31 C36 1.38(3) . ? C31 P2 1.83(2) . ? C32 C33 1.34(3) . ? C32 H32 0.9500 . ? C33 C34 1.39(3) . ? C33 H33 0.9500 . ? C34 C35 1.40(3) . ? C34 H34 0.9500 . ? C35 C36 1.38(3) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 Cl3 1.70(2) . ? C37 Cl2 1.72(3) . ? C37 Cl1 1.76(2) . ? C37 H37 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 Br1 166.24(15) . . ? P1 Au1 Au2 100.98(14) . . ? Br1 Au1 Au2 92.50(6) . . ? P2 Au2 Br2 174.32(14) . . ? P2 Au2 Au1 105.44(13) . . ? Br2 Au2 Au1 80.17(6) . . ? C2 C1 C6 117.5(19) . . ? C2 C1 P1 120.9(17) . . ? C6 C1 P1 121.7(17) . . ? C1 C2 C3 121(2) . . ? C1 C2 H2 119.5 . . ? C3 C2 H2 119.5 . . ? C4 C3 C2 119(2) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 121(2) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C6 C5 C4 120(2) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C1 121(2) . . ? C5 C6 H6 119.5 . . ? C1 C6 H6 119.5 . . ? C8 C7 C12 118.7(19) . . ? C8 C7 P1 121.9(15) . . ? C12 C7 P1 119.2(15) . . ? C7 C8 C9 120(2) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C8 C9 C10 120(2) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C11 C10 C9 119(2) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 122(2) . . ? C10 C11 H11 119.1 . . ? C12 C11 H11 119.1 . . ? C11 C12 C7 120(2) . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? C14 C13 C18 120.5(17) . . ? C14 C13 P1 122.2(15) . . ? C18 C13 P1 117.3(14) . . ? C13 C14 C15 119.0(19) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C14 C15 C16 121.1(19) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C17 C16 C15 120.3(17) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 118.7(18) . . ? C16 C17 H17 120.7 . . ? C18 C17 H17 120.7 . . ? C13 C18 O1 117.8(15) . . ? C13 C18 C17 120.2(17) . . ? O1 C18 C17 121.6(17) . . ? C20 C19 O1 122.9(18) . . ? C20 C19 C24 122.8(19) . . ? O1 C19 C24 114.3(17) . . ? C21 C20 C19 118(2) . . ? C21 C20 H20 121.0 . . ? C19 C20 H20 121.0 . . ? C22 C21 C20 122(2) . . ? C22 C21 H21 119.2 . . ? C20 C21 H21 119.2 . . ? C21 C22 C23 119(2) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C24 C23 C22 122(2) . . ? C24 C23 H23 118.8 . . ? C22 C23 H23 118.8 . . ? C23 C24 C19 115.7(18) . . ? C23 C24 P2 125.3(17) . . ? C19 C24 P2 119.0(16) . . ? C26 C25 C30 119.6(19) . . ? C26 C25 P2 120.0(15) . . ? C30 C25 P2 120.2(16) . . ? C25 C26 C27 122(2) . . ? C25 C26 H26 119.2 . . ? C27 C26 H26 119.2 . . ? C28 C27 C26 118(2) . . ? C28 C27 H27 121.1 . . ? C26 C27 H27 121.1 . . ? C27 C28 C29 122(2) . . ? C27 C28 H28 119.2 . . ? C29 C28 H28 119.2 . . ? C30 C29 C28 119(2) . . ? C30 C29 H29 120.6 . . ? C28 C29 H29 120.6 . . ? C29 C30 C25 120(2) . . ? C29 C30 H30 119.8 . . ? C25 C30 H30 119.8 . . ? C32 C31 C36 121(2) . . ? C32 C31 P2 122.6(16) . . ? C36 C31 P2 116.6(17) . . ? C33 C32 C31 122(2) . . ? C33 C32 H32 119.0 . . ? C31 C32 H32 119.0 . . ? C32 C33 C34 120(2) . . ? C32 C33 H33 120.1 . . ? C34 C33 H33 120.1 . . ? C33 C34 C35 117.4(19) . . ? C33 C34 H34 121.3 . . ? C35 C34 H34 121.3 . . ? C36 C35 C34 123(2) . . ? C36 C35 H35 118.4 . . ? C34 C35 H35 118.4 . . ? C35 C36 C31 117(2) . . ? C35 C36 H36 121.7 . . ? C31 C36 H36 121.7 . . ? Cl3 C37 Cl2 113.6(15) . . ? Cl3 C37 Cl1 111.9(14) . . ? Cl2 C37 Cl1 110.4(11) . . ? Cl3 C37 H37 106.8 . . ? Cl2 C37 H37 106.8 . . ? Cl1 C37 H37 106.8 . . ? C19 O1 C18 121.0(13) . . ? C1 P1 C7 105.9(10) . . ? C1 P1 C13 106.8(9) . . ? C7 P1 C13 105.2(9) . . ? C1 P1 Au1 106.8(8) . . ? C7 P1 Au1 122.4(7) . . ? C13 P1 Au1 108.8(6) . . ? C24 P2 C25 104.5(9) . . ? C24 P2 C31 104.8(10) . . ? C25 P2 C31 105.7(10) . . ? C24 P2 Au2 114.7(7) . . ? C25 P2 Au2 116.2(7) . . ? C31 P2 Au2 109.9(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 4.824 _refine_diff_density_min -2.875 _refine_diff_density_rms 0.418 #===END data_08mz213_0m _database_code_depnum_ccdc_archive 'CCDC 750031' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H29 Au2 Cl3 I2 O P2' _chemical_formula_weight 1305.63 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' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 '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 9.0814(13) _cell_length_b 20.656(3) _cell_length_c 20.934(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.566(2) _cell_angle_gamma 90.00 _cell_volume 3832.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9937 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 31.76 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.263 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 9.579 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.300 _exptl_absorpt_correction_T_max 0.563 _exptl_absorpt_process_details 'Apex2 v2008.2-0 (Bruker, 2008)' _exptl_special_details ; The crystal under investigation was found to be pseudo-merohedrally twinned. Application of the twin law 1 0 0 0 -1 0 -1 0 -1 resulted in a BASF value of 0.4397(8). C7 was set to have the same ADP as neighboring P1. C1, C2 and C3 were restrained to have similar ADPs (SIMU 0.01). ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 36368 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 0.99 _diffrn_reflns_theta_max 28.28 _reflns_number_total 9613 _reflns_number_gt 8921 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2008.2-4 (Bruker, 2008)' _computing_cell_refinement 'Apex2 v2008.2-4 ' _computing_data_reduction 'Apex2 v2008.2-4 ' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.0244P)^2^+50.5082P] 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 9613 _refine_ls_number_parameters 419 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1060 _refine_ls_wR_factor_gt 0.1025 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.143 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.86059(5) 0.77462(2) 0.275958(19) 0.02147(9) Uani 1 1 d . . . Au2 Au 0.69133(5) 0.65325(2) 0.28937(2) 0.02464(10) Uani 1 1 d . . . C1 C 0.7767(14) 0.9210(6) 0.3248(5) 0.029(2) Uani 1 1 d U . . C2 C 0.8363(16) 0.9396(5) 0.2742(7) 0.036(2) Uani 1 1 d U . . H2 H 0.8841 0.9083 0.2523 0.043 Uiso 1 1 calc R . . C3 C 0.8293(19) 1.0024(6) 0.2536(8) 0.049(3) Uani 1 1 d U . . H3 H 0.8741 1.0148 0.2185 0.059 Uiso 1 1 calc R . . C4 C 0.7594(15) 1.0463(6) 0.2830(7) 0.043(3) Uani 1 1 d . . . H4 H 0.7586 1.0904 0.2699 0.051 Uiso 1 1 calc R . . C5 C 0.6888(15) 1.0288(6) 0.3319(7) 0.037(3) Uani 1 1 d . . . H5 H 0.6317 1.0597 0.3498 0.045 Uiso 1 1 calc R . . C6 C 0.7004(16) 0.9669(6) 0.3548(6) 0.035(3) Uani 1 1 d . . . H6 H 0.6574 0.9550 0.3906 0.042 Uiso 1 1 calc R . . C7 C 0.6054(11) 0.8227(5) 0.3719(5) 0.0181(5) Uani 1 1 d . . . C8 C 0.5813(13) 0.8259(7) 0.4357(7) 0.035(3) Uani 1 1 d . . . H8 H 0.6636 0.8351 0.4711 0.042 Uiso 1 1 calc R . . C9 C 0.4394(16) 0.8159(7) 0.4480(7) 0.041(3) Uani 1 1 d . . . H9 H 0.4253 0.8159 0.4916 0.050 Uiso 1 1 calc R . . C10 C 0.3185(15) 0.8059(9) 0.3963(8) 0.051(4) Uani 1 1 d . . . H10 H 0.2207 0.7995 0.4046 0.061 Uiso 1 1 calc R . . C11 C 0.3372(14) 0.8051(7) 0.3349(6) 0.042(3) Uani 1 1 d . . . H11 H 0.2519 0.7989 0.3001 0.050 Uiso 1 1 calc R . . C12 C 0.4783(12) 0.8132(6) 0.3204(5) 0.026(2) Uani 1 1 d . . . H12 H 0.4891 0.8123 0.2763 0.031 Uiso 1 1 calc R . . C13 C 0.9214(12) 0.8336(5) 0.4285(5) 0.020(2) Uani 1 1 d . . . C14 C 1.0181(14) 0.8844(7) 0.4504(6) 0.034(3) Uani 1 1 d . . . H14 H 1.0094 0.9234 0.4259 0.040 Uiso 1 1 calc R . . C15 C 1.1289(14) 0.8792(8) 0.5082(6) 0.040(3) Uani 1 1 d . . . H15 H 1.1925 0.9150 0.5234 0.048 Uiso 1 1 calc R . . C16 C 1.1453(14) 0.8235(7) 0.5425(6) 0.038(3) Uani 1 1 d . . . H16 H 1.2200 0.8207 0.5819 0.046 Uiso 1 1 calc R . . C17 C 1.0543(13) 0.7696(7) 0.5210(5) 0.033(3) Uani 1 1 d . . . H17 H 1.0692 0.7298 0.5443 0.039 Uiso 1 1 calc R . . C18 C 0.9414(13) 0.7758(6) 0.4645(5) 0.026(2) Uani 1 1 d . . . C19 C 0.7917(14) 0.6801(6) 0.4782(5) 0.029(3) Uani 1 1 d . . . C20 C 0.7534(13) 0.6971(6) 0.5362(5) 0.030(3) Uani 1 1 d . . . H20 H 0.7665 0.7406 0.5512 0.036 Uiso 1 1 calc R . . C21 C 0.6966(13) 0.6519(7) 0.5722(6) 0.032(3) Uani 1 1 d . . . H21 H 0.6699 0.6641 0.6120 0.038 Uiso 1 1 calc R . . C22 C 0.6778(14) 0.5869(7) 0.5500(6) 0.034(3) Uani 1 1 d . . . H22 H 0.6407 0.5548 0.5751 0.041 Uiso 1 1 calc R . . C23 C 0.7143(13) 0.5713(6) 0.4915(6) 0.031(3) Uani 1 1 d . . . H23 H 0.7000 0.5281 0.4757 0.038 Uiso 1 1 calc R . . C24 C 0.7713(12) 0.6170(5) 0.4553(5) 0.022(2) Uani 1 1 d . . . C25 C 1.0274(12) 0.6108(6) 0.3975(6) 0.029(3) Uani 1 1 d . . . C26 C 1.1010(13) 0.6301(6) 0.3494(6) 0.031(3) Uani 1 1 d . . . H26 H 1.0465 0.6352 0.3055 0.037 Uiso 1 1 calc R . . C27 C 1.2552(16) 0.6419(7) 0.3658(6) 0.040(3) Uani 1 1 d . . . H27 H 1.3051 0.6571 0.3331 0.047 Uiso 1 1 calc R . . C28 C 1.3374(14) 0.6320(8) 0.4290(7) 0.044(3) Uani 1 1 d . . . H28 H 1.4436 0.6383 0.4391 0.052 Uiso 1 1 calc R . . C29 C 1.2653(16) 0.6133(8) 0.4764(6) 0.046(4) Uani 1 1 d . . . H29 H 1.3205 0.6082 0.5202 0.055 Uiso 1 1 calc R . . C30 C 1.1111(14) 0.6015(6) 0.4610(6) 0.033(3) Uani 1 1 d . . . H30 H 1.0620 0.5870 0.4941 0.040 Uiso 1 1 calc R . . C31 C 0.7930(14) 0.5131(6) 0.3632(5) 0.028(2) Uani 1 1 d . . . C32 C 0.9130(14) 0.4696(5) 0.3751(5) 0.024(2) Uani 1 1 d . . . H32 H 1.0131 0.4836 0.3930 0.029 Uiso 1 1 calc R . . C33 C 0.8807(15) 0.4047(6) 0.3597(6) 0.032(3) Uani 1 1 d . . . H33 H 0.9615 0.3745 0.3662 0.039 Uiso 1 1 calc R . . C34 C 0.7386(16) 0.3830(6) 0.3358(6) 0.037(3) Uani 1 1 d . . . H34 H 0.7215 0.3385 0.3255 0.044 Uiso 1 1 calc R . . C35 C 0.6156(16) 0.4266(6) 0.3263(6) 0.036(3) Uani 1 1 d . . . H35 H 0.5154 0.4114 0.3111 0.043 Uiso 1 1 calc R . . C36 C 0.6436(13) 0.4920(6) 0.3394(6) 0.032(3) Uani 1 1 d . . . H36 H 0.5627 0.5221 0.3324 0.038 Uiso 1 1 calc R . . C37 C 0.7353(17) 0.5559(8) 0.1222(8) 0.048(4) Uani 1 1 d . . . H37 H 0.7260 0.5985 0.1438 0.058 Uiso 1 1 calc R . . Cl1 Cl 0.7466(8) 0.4976(4) 0.1809(3) 0.121(3) Uani 1 1 d . . . Cl2 Cl 0.8941(6) 0.5609(2) 0.0884(3) 0.0687(13) Uani 1 1 d . . . Cl3 Cl 0.5764(7) 0.5471(4) 0.0609(2) 0.100(2) Uani 1 1 d . . . I1 I 0.99236(9) 0.72471(4) 0.19047(3) 0.02914(16) Uani 1 1 d . . . I2 I 0.51513(9) 0.69891(4) 0.18497(4) 0.0355(2) Uani 1 1 d . . . O1 O 0.8471(10) 0.7244(4) 0.4380(3) 0.0287(17) Uani 1 1 d . . . P1 P 0.7846(3) 0.83603(13) 0.35186(12) 0.0181(5) Uani 1 1 d . . . P2 P 0.8247(3) 0.59918(14) 0.37747(13) 0.0223(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 Au1 0.02612(19) 0.02061(18) 0.01862(17) -0.00182(15) 0.00692(15) 0.00064(17) Au2 0.02415(18) 0.02317(19) 0.02158(18) 0.00337(16) -0.00605(15) -0.00039(17) C1 0.043(6) 0.022(5) 0.026(5) 0.000(4) 0.016(4) 0.006(5) C2 0.054(6) 0.008(4) 0.054(6) 0.003(4) 0.028(5) 0.010(4) C3 0.068(8) 0.025(6) 0.065(7) 0.010(5) 0.041(6) 0.004(6) C4 0.042(7) 0.028(6) 0.059(9) 0.010(6) 0.013(7) -0.008(6) C5 0.035(7) 0.022(6) 0.058(8) 0.004(5) 0.018(6) 0.018(5) C6 0.048(8) 0.029(6) 0.034(6) 0.012(5) 0.020(6) 0.009(6) C7 0.0190(11) 0.0182(12) 0.0167(11) -0.0015(9) 0.0031(9) 0.0036(10) C8 0.017(5) 0.042(7) 0.046(7) 0.004(6) 0.007(5) 0.004(5) C9 0.035(7) 0.051(8) 0.043(7) -0.014(6) 0.017(6) -0.001(7) C10 0.025(6) 0.073(11) 0.053(9) -0.016(8) 0.003(6) -0.011(7) C11 0.020(6) 0.056(9) 0.039(7) -0.008(6) -0.017(5) 0.007(6) C12 0.017(5) 0.035(6) 0.022(5) -0.009(4) -0.005(4) 0.002(4) C13 0.018(5) 0.028(6) 0.015(4) -0.002(4) 0.005(4) 0.001(4) C14 0.026(6) 0.045(7) 0.030(6) -0.005(5) 0.005(5) -0.003(6) C15 0.024(6) 0.058(9) 0.036(7) -0.014(6) 0.004(5) -0.004(6) C16 0.030(6) 0.064(9) 0.018(5) 0.006(6) -0.001(5) 0.002(6) C17 0.024(6) 0.055(8) 0.018(5) 0.005(5) 0.000(4) 0.001(6) C18 0.026(5) 0.031(6) 0.021(5) -0.002(4) 0.004(4) 0.007(5) C19 0.029(6) 0.038(7) 0.018(5) 0.005(4) 0.002(4) 0.011(5) C20 0.024(6) 0.040(7) 0.026(5) -0.001(5) 0.007(4) 0.001(5) C21 0.028(6) 0.041(7) 0.028(6) -0.001(5) 0.007(5) 0.005(5) C22 0.028(6) 0.049(8) 0.028(6) 0.005(5) 0.014(5) 0.003(6) C23 0.020(5) 0.037(7) 0.036(6) 0.002(5) 0.005(5) 0.003(5) C24 0.025(5) 0.017(5) 0.021(5) 0.000(4) -0.004(4) 0.005(4) C25 0.019(5) 0.024(6) 0.035(6) -0.007(5) -0.011(4) 0.002(4) C26 0.029(6) 0.039(7) 0.024(5) 0.001(5) 0.005(4) 0.007(5) C27 0.051(8) 0.038(7) 0.034(6) 0.000(5) 0.018(6) 0.004(6) C28 0.019(6) 0.062(10) 0.046(8) -0.001(7) -0.001(5) 0.011(6) C29 0.037(7) 0.067(10) 0.026(6) -0.004(6) -0.008(5) 0.007(7) C30 0.034(6) 0.035(7) 0.027(6) 0.002(5) -0.003(5) 0.007(6) C31 0.039(6) 0.026(6) 0.016(5) 0.003(4) -0.002(4) -0.008(5) C32 0.032(6) 0.020(5) 0.020(5) 0.005(4) 0.005(4) 0.011(5) C33 0.035(6) 0.024(6) 0.035(6) -0.003(5) 0.003(5) 0.005(5) C34 0.058(9) 0.022(6) 0.028(6) -0.007(5) 0.008(6) 0.006(6) C35 0.044(7) 0.032(6) 0.027(6) -0.008(5) -0.001(5) 0.004(6) C36 0.019(5) 0.032(6) 0.039(6) 0.002(5) -0.005(5) -0.004(5) C37 0.044(8) 0.052(9) 0.051(9) -0.001(7) 0.018(7) 0.000(7) Cl1 0.102(4) 0.166(7) 0.106(5) 0.080(5) 0.046(4) 0.022(5) Cl2 0.070(3) 0.059(3) 0.090(3) -0.012(2) 0.045(3) -0.011(2) Cl3 0.078(4) 0.169(7) 0.054(3) 0.009(3) 0.014(3) -0.013(4) I1 0.0370(4) 0.0327(4) 0.0199(3) -0.0025(3) 0.0108(3) 0.0035(3) I2 0.0312(4) 0.0322(4) 0.0332(4) 0.0069(3) -0.0146(3) -0.0014(3) O1 0.037(4) 0.033(4) 0.015(3) -0.002(3) 0.003(3) -0.003(4) P1 0.0190(11) 0.0182(12) 0.0167(11) -0.0015(9) 0.0031(9) 0.0036(10) P2 0.0236(13) 0.0226(14) 0.0170(12) 0.0013(10) -0.0039(10) -0.0002(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.256(3) . ? Au1 I1 2.5748(8) . ? Au1 Au2 2.9857(7) . ? Au2 P2 2.268(3) . ? Au2 I2 2.5893(8) . ? C1 C2 1.346(17) . ? C1 C6 1.401(16) . ? C1 P1 1.841(12) . ? C2 C3 1.365(16) . ? C2 H2 0.9500 . ? C3 C4 1.33(2) . ? C3 H3 0.9500 . ? C4 C5 1.370(19) . ? C4 H4 0.9500 . ? C5 C6 1.361(16) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.401(17) . ? C7 C12 1.411(13) . ? C7 P1 1.787(10) . ? C8 C9 1.383(17) . ? C8 H8 0.9500 . ? C9 C10 1.378(19) . ? C9 H9 0.9500 . ? C10 C11 1.33(2) . ? C10 H10 0.9500 . ? C11 C12 1.388(18) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.381(16) . ? C13 C18 1.402(15) . ? C13 P1 1.804(10) . ? C14 C15 1.399(17) . ? C14 H14 0.9500 . ? C15 C16 1.35(2) . ? C15 H15 0.9500 . ? C16 C17 1.402(19) . ? C16 H16 0.9500 . ? C17 C18 1.392(14) . ? C17 H17 0.9500 . ? C18 O1 1.401(14) . ? C19 C20 1.378(15) . ? C19 C24 1.389(16) . ? C19 O1 1.408(14) . ? C20 C21 1.370(17) . ? C20 H20 0.9500 . ? C21 C22 1.420(19) . ? C21 H21 0.9500 . ? C22 C23 1.375(17) . ? C22 H22 0.9500 . ? C23 C24 1.380(16) . ? C23 H23 0.9500 . ? C24 P2 1.835(11) . ? C25 C26 1.382(17) . ? C25 C30 1.394(15) . ? C25 P2 1.813(11) . ? C26 C27 1.389(19) . ? C26 H26 0.9500 . ? C27 C28 1.386(18) . ? C27 H27 0.9500 . ? C28 C29 1.36(2) . ? C28 H28 0.9500 . ? C29 C30 1.389(19) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.393(16) . ? C31 C36 1.408(16) . ? C31 P2 1.815(12) . ? C32 C33 1.396(15) . ? C32 H32 0.9500 . ? C33 C34 1.354(18) . ? C33 H33 0.9500 . ? C34 C35 1.414(18) . ? C34 H34 0.9500 . ? C35 C36 1.391(17) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 Cl1 1.708(17) . ? C37 Cl3 1.718(16) . ? C37 Cl2 1.742(15) . ? C37 H37 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 I1 167.06(7) . . ? P1 Au1 Au2 99.39(7) . . ? I1 Au1 Au2 93.20(3) . . ? P2 Au2 I2 171.24(8) . . ? P2 Au2 Au1 107.18(7) . . ? I2 Au2 Au1 81.43(2) . . ? C2 C1 C6 118.9(11) . . ? C2 C1 P1 121.2(8) . . ? C6 C1 P1 119.8(9) . . ? C1 C2 C3 121.3(12) . . ? C1 C2 H2 119.3 . . ? C3 C2 H2 119.3 . . ? C4 C3 C2 119.8(13) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 120.8(12) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C6 C5 C4 120.0(12) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 119.0(11) . . ? C5 C6 H6 120.5 . . ? C1 C6 H6 120.5 . . ? C8 C7 C12 117.5(10) . . ? C8 C7 P1 123.8(8) . . ? C12 C7 P1 118.5(8) . . ? C9 C8 C7 121.0(12) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C10 C9 C8 119.5(13) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C11 C10 C9 120.7(13) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 121.7(11) . . ? C10 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? C11 C12 C7 119.4(10) . . ? C11 C12 H12 120.3 . . ? C7 C12 H12 120.3 . . ? C14 C13 C18 118.0(10) . . ? C14 C13 P1 122.6(9) . . ? C18 C13 P1 119.0(8) . . ? C13 C14 C15 120.9(13) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C16 C15 C14 120.1(13) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 121.2(11) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C18 C17 C16 118.2(12) . . ? C18 C17 H17 120.9 . . ? C16 C17 H17 120.9 . . ? C17 C18 O1 122.6(11) . . ? C17 C18 C13 121.3(11) . . ? O1 C18 C13 115.9(9) . . ? C20 C19 C24 120.2(11) . . ? C20 C19 O1 123.5(11) . . ? C24 C19 O1 116.2(9) . . ? C21 C20 C19 120.6(12) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C22 119.8(11) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C23 C22 C21 118.5(12) . . ? C23 C22 H22 120.7 . . ? C21 C22 H22 120.7 . . ? C22 C23 C24 121.5(12) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 119.3 . . ? C23 C24 C19 119.4(10) . . ? C23 C24 P2 123.7(9) . . ? C19 C24 P2 117.0(8) . . ? C26 C25 C30 119.0(11) . . ? C26 C25 P2 119.8(8) . . ? C30 C25 P2 121.2(10) . . ? C25 C26 C27 119.5(11) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C28 C27 C26 120.9(13) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C29 C28 C27 119.7(12) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C28 C29 C30 120.1(12) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C29 C30 C25 120.7(13) . . ? C29 C30 H30 119.6 . . ? C25 C30 H30 119.6 . . ? C32 C31 C36 121.2(11) . . ? C32 C31 P2 120.8(9) . . ? C36 C31 P2 117.9(9) . . ? C31 C32 C33 117.5(11) . . ? C31 C32 H32 121.2 . . ? C33 C32 H32 121.2 . . ? C34 C33 C32 122.5(12) . . ? C34 C33 H33 118.7 . . ? C32 C33 H33 118.7 . . ? C33 C34 C35 120.1(11) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C36 C35 C34 119.0(12) . . ? C36 C35 H35 120.5 . . ? C34 C35 H35 120.5 . . ? C35 C36 C31 119.5(12) . . ? C35 C36 H36 120.3 . . ? C31 C36 H36 120.3 . . ? Cl1 C37 Cl3 111.8(9) . . ? Cl1 C37 Cl2 114.1(9) . . ? Cl3 C37 Cl2 109.8(9) . . ? Cl1 C37 H37 106.9 . . ? Cl3 C37 H37 106.9 . . ? Cl2 C37 H37 106.9 . . ? C18 O1 C19 121.5(8) . . ? C7 P1 C13 105.8(5) . . ? C7 P1 C1 104.1(5) . . ? C13 P1 C1 105.8(5) . . ? C7 P1 Au1 120.8(3) . . ? C13 P1 Au1 110.7(3) . . ? C1 P1 Au1 108.5(4) . . ? C25 P2 C31 106.5(6) . . ? C25 P2 C24 102.7(5) . . ? C31 P2 C24 106.2(5) . . ? C25 P2 Au2 117.3(4) . . ? C31 P2 Au2 108.1(4) . . ? C24 P2 Au2 115.2(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Au1 Au2 P2 -80.66(10) . . . . ? I1 Au1 Au2 P2 96.32(8) . . . . ? P1 Au1 Au2 I2 101.01(7) . . . . ? I1 Au1 Au2 I2 -82.01(3) . . . . ? C6 C1 C2 C3 3(2) . . . . ? P1 C1 C2 C3 179.4(12) . . . . ? C1 C2 C3 C4 -2(3) . . . . ? C2 C3 C4 C5 -3(2) . . . . ? C3 C4 C5 C6 6(2) . . . . ? C4 C5 C6 C1 -4(2) . . . . ? C2 C1 C6 C5 0(2) . . . . ? P1 C1 C6 C5 -176.5(11) . . . . ? C12 C7 C8 C9 4.1(19) . . . . ? P1 C7 C8 C9 179.1(11) . . . . ? C7 C8 C9 C10 -3(2) . . . . ? C8 C9 C10 C11 1(3) . . . . ? C9 C10 C11 C12 1(3) . . . . ? C10 C11 C12 C7 0(2) . . . . ? C8 C7 C12 C11 -2.3(17) . . . . ? P1 C7 C12 C11 -177.6(10) . . . . ? C18 C13 C14 C15 -2.6(17) . . . . ? P1 C13 C14 C15 -176.1(9) . . . . ? C13 C14 C15 C16 2.0(19) . . . . ? C14 C15 C16 C17 1(2) . . . . ? C15 C16 C17 C18 -2.7(19) . . . . ? C16 C17 C18 O1 178.3(10) . . . . ? C16 C17 C18 C13 2.0(17) . . . . ? C14 C13 C18 C17 0.6(16) . . . . ? P1 C13 C18 C17 174.3(9) . . . . ? C14 C13 C18 O1 -175.9(10) . . . . ? P1 C13 C18 O1 -2.2(13) . . . . ? C24 C19 C20 C21 0.8(17) . . . . ? O1 C19 C20 C21 178.4(10) . . . . ? C19 C20 C21 C22 0.4(18) . . . . ? C20 C21 C22 C23 -1.5(18) . . . . ? C21 C22 C23 C24 1.4(18) . . . . ? C22 C23 C24 C19 -0.3(17) . . . . ? C22 C23 C24 P2 179.2(9) . . . . ? C20 C19 C24 C23 -0.9(16) . . . . ? O1 C19 C24 C23 -178.6(10) . . . . ? C20 C19 C24 P2 179.6(9) . . . . ? O1 C19 C24 P2 1.9(13) . . . . ? C30 C25 C26 C27 -2.3(18) . . . . ? P2 C25 C26 C27 176.9(10) . . . . ? C25 C26 C27 C28 3(2) . . . . ? C26 C27 C28 C29 -3(2) . . . . ? C27 C28 C29 C30 3(2) . . . . ? C28 C29 C30 C25 -2(2) . . . . ? C26 C25 C30 C29 2(2) . . . . ? P2 C25 C30 C29 -177.2(11) . . . . ? C36 C31 C32 C33 3.0(16) . . . . ? P2 C31 C32 C33 -176.7(8) . . . . ? C31 C32 C33 C34 -2.0(18) . . . . ? C32 C33 C34 C35 -1(2) . . . . ? C33 C34 C35 C36 2.3(19) . . . . ? C34 C35 C36 C31 -1.3(19) . . . . ? C32 C31 C36 C35 -1.4(18) . . . . ? P2 C31 C36 C35 178.3(9) . . . . ? C17 C18 O1 C19 39.0(16) . . . . ? C13 C18 O1 C19 -144.5(10) . . . . ? C20 C19 O1 C18 35.2(16) . . . . ? C24 C19 O1 C18 -147.2(10) . . . . ? C8 C7 P1 C13 13.5(11) . . . . ? C12 C7 P1 C13 -171.5(9) . . . . ? C8 C7 P1 C1 -97.8(10) . . . . ? C12 C7 P1 C1 77.2(10) . . . . ? C8 C7 P1 Au1 140.2(9) . . . . ? C12 C7 P1 Au1 -44.8(10) . . . . ? C14 C13 P1 C7 -122.7(10) . . . . ? C18 C13 P1 C7 63.8(10) . . . . ? C14 C13 P1 C1 -12.7(11) . . . . ? C18 C13 P1 C1 173.9(9) . . . . ? C14 C13 P1 Au1 104.7(9) . . . . ? C18 C13 P1 Au1 -68.8(9) . . . . ? C2 C1 P1 C7 -141.0(11) . . . . ? C6 C1 P1 C7 35.4(12) . . . . ? C2 C1 P1 C13 107.7(12) . . . . ? C6 C1 P1 C13 -75.9(12) . . . . ? C2 C1 P1 Au1 -11.2(13) . . . . ? C6 C1 P1 Au1 165.3(10) . . . . ? I1 Au1 P1 C7 165.7(4) . . . . ? Au2 Au1 P1 C7 -27.9(4) . . . . ? I1 Au1 P1 C13 -69.9(5) . . . . ? Au2 Au1 P1 C13 96.5(4) . . . . ? I1 Au1 P1 C1 45.8(6) . . . . ? Au2 Au1 P1 C1 -147.8(4) . . . . ? C26 C25 P2 C31 97.3(10) . . . . ? C30 C25 P2 C31 -83.6(11) . . . . ? C26 C25 P2 C24 -151.3(10) . . . . ? C30 C25 P2 C24 27.8(11) . . . . ? C26 C25 P2 Au2 -23.9(11) . . . . ? C30 C25 P2 Au2 155.2(9) . . . . ? C32 C31 P2 C25 6.7(11) . . . . ? C36 C31 P2 C25 -172.9(9) . . . . ? C32 C31 P2 C24 -102.2(10) . . . . ? C36 C31 P2 C24 78.1(10) . . . . ? C32 C31 P2 Au2 133.6(8) . . . . ? C36 C31 P2 Au2 -46.1(10) . . . . ? C23 C24 P2 C25 -113.7(10) . . . . ? C19 C24 P2 C25 65.8(9) . . . . ? C23 C24 P2 C31 -2.0(11) . . . . ? C19 C24 P2 C31 177.5(9) . . . . ? C23 C24 P2 Au2 117.7(9) . . . . ? C19 C24 P2 Au2 -62.9(9) . . . . ? Au1 Au2 P2 C25 -29.0(4) . . . . ? Au1 Au2 P2 C31 -149.4(4) . . . . ? Au1 Au2 P2 C24 92.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.234 _refine_diff_density_min -1.940 _refine_diff_density_rms 0.267 #===END data_ju042308b_0m _database_code_depnum_ccdc_archive 'CCDC 750032' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H26 Au2 Br2 O P2' _chemical_formula_sum 'C36 H26 Au2 Br2 O P2' _chemical_formula_weight 1090.26 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' P P 0.1023 0.0942 '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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0279(19) _cell_length_b 12.491(2) _cell_length_c 12.561(2) _cell_angle_alpha 109.152(2) _cell_angle_beta 92.054(2) _cell_angle_gamma 94.291(2) _cell_volume 1774.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9525 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 26.93 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.041 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 10.629 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2137 _exptl_absorpt_correction_T_max 0.5680 _exptl_absorpt_process_details 'AXScale in APEX2 (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 20142 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 26.99 _reflns_number_total 7622 _reflns_number_gt 6515 _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^)+(0.0591P)^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 7622 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.1007 _refine_ls_wR_factor_gt 0.0988 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.115 _refine_ls_shift/su_max 0.009 _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 Au1 Au 1.003506(18) -0.187202(19) 0.840824(19) 0.01733(8) Uani 1 1 d . . . Au2 Au 0.639977(19) 0.145834(19) 0.631933(19) 0.01910(8) Uani 1 1 d . . . Br1 Br 1.14269(5) -0.31469(5) 0.84182(5) 0.02248(14) Uani 1 1 d . . . Br2 Br 0.70118(7) 0.02519(6) 0.45793(6) 0.03474(18) Uani 1 1 d . . . P1 P 0.86632(12) -0.07996(13) 0.82933(13) 0.0150(3) Uani 1 1 d . . . P2 P 0.58695(12) 0.27401(13) 0.78665(13) 0.0145(3) Uani 1 1 d . . . O1 O 0.6791(3) 0.0980(3) 0.8989(3) 0.0144(8) Uani 1 1 d . . . C18 C 0.6835(4) -0.1194(5) 0.6730(4) 0.0112(11) Uani 1 1 d . . . H18 H 0.6918 -0.0396 0.6867 0.013 Uiso 1 1 calc R . . C11 C 0.5929(5) 0.1609(5) 0.9481(5) 0.0154(12) Uani 1 1 d . . . C12 C 0.7105(5) 0.0443(5) 0.9731(5) 0.0134(11) Uani 1 1 d . . . C10 C 0.5397(5) 0.2337(5) 0.9031(5) 0.0173(12) Uani 1 1 d . . . C36 C 0.7657(5) 0.4186(5) 0.7730(5) 0.0183(12) Uani 1 1 d . . . H36 H 0.7536 0.3810 0.6939 0.022 Uiso 1 1 calc R . . C14 C 0.7448(5) -0.2820(5) 0.7060(5) 0.0231(14) Uani 1 1 d . . . H14 H 0.7947 -0.3154 0.7435 0.028 Uiso 1 1 calc R . . C1 C 0.7952(5) -0.0272(5) 0.9579(5) 0.0156(12) Uani 1 1 d . . . C25 C 0.4701(5) 0.3416(5) 0.7495(5) 0.0172(12) Uani 1 1 d . . . C9 C 0.4524(5) 0.2849(5) 0.9660(5) 0.0197(13) Uani 1 1 d . . . H9 H 0.4124 0.3355 0.9403 0.024 Uiso 1 1 calc R . . C31 C 0.6971(5) 0.3864(5) 0.8466(5) 0.0161(12) Uani 1 1 d . . . C13 C 0.7555(5) -0.1655(5) 0.7261(5) 0.0168(12) Uani 1 1 d . . . C21 C 0.9537(5) 0.2406(5) 0.8221(5) 0.0191(13) Uani 1 1 d . . . H21 H 0.9536 0.3168 0.8712 0.023 Uiso 1 1 calc R . . C20 C 0.9118(5) 0.1515(5) 0.8559(5) 0.0161(12) Uani 1 1 d . . . H20 H 0.8820 0.1670 0.9278 0.019 Uiso 1 1 calc R . . C6 C 0.5680(5) 0.1455(5) 1.0493(5) 0.0150(12) Uani 1 1 d . . . C7 C 0.4791(5) 0.1982(5) 1.1074(5) 0.0208(13) Uani 1 1 d . . . H7 H 0.4590 0.1875 1.1759 0.025 Uiso 1 1 calc R . . C2 C 0.8196(5) -0.0686(5) 1.0471(5) 0.0231(14) Uani 1 1 d . . . H2 H 0.8789 -0.1159 1.0417 0.028 Uiso 1 1 calc R . . C3 C 0.7582(5) -0.0411(5) 1.1433(6) 0.0243(14) Uani 1 1 d . . . H3 H 0.7762 -0.0701 1.2022 0.029 Uiso 1 1 calc R . . C26 C 0.3767(5) 0.2724(6) 0.6946(5) 0.0244(14) Uani 1 1 d . . . H26 H 0.3764 0.1923 0.6764 0.029 Uiso 1 1 calc R . . C5 C 0.6471(5) 0.0708(5) 1.0672(5) 0.0187(13) Uani 1 1 d . . . C30 C 0.4712(5) 0.4572(5) 0.7725(5) 0.0226(13) Uani 1 1 d . . . H30 H 0.5352 0.5061 0.8100 0.027 Uiso 1 1 calc R . . C35 C 0.8504(5) 0.5041(6) 0.8140(6) 0.0251(14) Uani 1 1 d . . . H35 H 0.8970 0.5248 0.7631 0.030 Uiso 1 1 calc R . . C19 C 0.9129(4) 0.0387(5) 0.7847(5) 0.0171(12) Uani 1 1 d . . . C4 C 0.6704(5) 0.0287(5) 1.1539(5) 0.0212(13) Uani 1 1 d . . . H4 H 0.6279 0.0466 1.2189 0.025 Uiso 1 1 calc R . . C8 C 0.4220(5) 0.2655(5) 1.0626(6) 0.0224(14) Uani 1 1 d . . . H8 H 0.3596 0.2998 1.0993 0.027 Uiso 1 1 calc R . . C17 C 0.5976(5) -0.1856(6) 0.5987(5) 0.0252(14) Uani 1 1 d . . . H17 H 0.5465 -0.1521 0.5626 0.030 Uiso 1 1 calc R . . C34 C 0.8682(5) 0.5604(6) 0.9290(6) 0.0287(15) Uani 1 1 d . . . H34 H 0.9267 0.6199 0.9569 0.034 Uiso 1 1 calc R . . C33 C 0.8004(5) 0.5298(6) 1.0035(5) 0.0263(15) Uani 1 1 d . . . H33 H 0.8121 0.5682 1.0825 0.032 Uiso 1 1 calc R . . C32 C 0.7149(5) 0.4420(5) 0.9612(5) 0.0204(13) Uani 1 1 d . . . H32 H 0.6687 0.4204 1.0118 0.024 Uiso 1 1 calc R . . C22 C 0.9955(6) 0.2187(6) 0.7180(6) 0.0296(15) Uani 1 1 d . . . H22 H 1.0225 0.2798 0.6938 0.036 Uiso 1 1 calc R . . C24 C 0.9579(6) 0.0186(6) 0.6820(6) 0.0339(17) Uani 1 1 d . . . H24 H 0.9611 -0.0575 0.6336 0.041 Uiso 1 1 calc R . . C23 C 0.9984(7) 0.1078(6) 0.6483(6) 0.040(2) Uani 1 1 d . . . H23 H 1.0285 0.0928 0.5764 0.048 Uiso 1 1 calc R . . C15 C 0.6602(5) -0.3488(6) 0.6306(6) 0.0269(15) Uani 1 1 d . . . H15 H 0.6528 -0.4288 0.6154 0.032 Uiso 1 1 calc R . . C16 C 0.5880(5) -0.3017(6) 0.5783(5) 0.0266(15) Uani 1 1 d . . . H16 H 0.5302 -0.3488 0.5270 0.032 Uiso 1 1 calc R . . C28 C 0.2853(5) 0.4319(6) 0.6891(5) 0.0244(14) Uani 1 1 d . . . H28 H 0.2214 0.4634 0.6695 0.029 Uiso 1 1 calc R . . C27 C 0.2846(5) 0.3167(6) 0.6659(6) 0.0266(15) Uani 1 1 d . . . H27 H 0.2201 0.2678 0.6298 0.032 Uiso 1 1 calc R . . C29 C 0.3797(6) 0.5016(6) 0.7412(6) 0.0288(15) Uani 1 1 d . . . H29 H 0.3813 0.5812 0.7555 0.035 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01580(13) 0.01822(13) 0.01923(14) 0.00725(10) 0.00172(9) 0.00438(9) Au2 0.02528(14) 0.01630(13) 0.01523(13) 0.00387(10) 0.00346(10) 0.00403(9) Br1 0.0199(3) 0.0224(3) 0.0255(3) 0.0070(3) 0.0019(2) 0.0086(2) Br2 0.0588(5) 0.0225(3) 0.0206(4) 0.0022(3) 0.0140(3) 0.0070(3) P1 0.0143(7) 0.0161(7) 0.0164(8) 0.0071(6) 0.0022(6) 0.0041(6) P2 0.0142(7) 0.0145(7) 0.0143(7) 0.0035(6) 0.0025(6) 0.0039(6) O1 0.017(2) 0.017(2) 0.013(2) 0.0082(17) 0.0008(16) 0.0055(16) C18 0.008(2) 0.022(3) 0.004(2) 0.004(2) 0.0013(19) 0.003(2) C11 0.013(3) 0.020(3) 0.013(3) 0.003(2) 0.003(2) 0.001(2) C12 0.014(3) 0.018(3) 0.008(3) 0.005(2) -0.001(2) -0.003(2) C10 0.014(3) 0.018(3) 0.020(3) 0.008(3) -0.001(2) -0.004(2) C36 0.015(3) 0.021(3) 0.021(3) 0.009(3) -0.001(2) 0.004(2) C14 0.023(3) 0.023(3) 0.024(3) 0.008(3) 0.007(3) 0.007(3) C1 0.017(3) 0.018(3) 0.010(3) 0.004(2) -0.004(2) -0.004(2) C25 0.015(3) 0.023(3) 0.011(3) 0.004(2) 0.001(2) 0.000(2) C9 0.017(3) 0.022(3) 0.022(3) 0.007(3) 0.011(2) 0.008(2) C31 0.011(3) 0.016(3) 0.023(3) 0.007(2) 0.004(2) 0.008(2) C13 0.014(3) 0.019(3) 0.020(3) 0.009(3) 0.006(2) 0.006(2) C21 0.020(3) 0.017(3) 0.022(3) 0.009(3) -0.003(2) 0.003(2) C20 0.016(3) 0.020(3) 0.009(3) 0.001(2) 0.001(2) 0.000(2) C6 0.018(3) 0.013(3) 0.011(3) 0.000(2) 0.002(2) 0.003(2) C7 0.025(3) 0.024(3) 0.007(3) -0.001(2) 0.007(2) -0.006(3) C2 0.024(3) 0.025(3) 0.023(3) 0.010(3) 0.002(3) 0.007(3) C3 0.035(4) 0.021(3) 0.023(3) 0.015(3) 0.003(3) 0.003(3) C26 0.030(4) 0.019(3) 0.020(3) 0.003(3) -0.001(3) 0.002(3) C5 0.021(3) 0.016(3) 0.023(3) 0.012(3) 0.000(3) -0.001(2) C30 0.024(3) 0.023(3) 0.022(3) 0.006(3) 0.001(3) 0.007(3) C35 0.027(3) 0.029(4) 0.027(4) 0.018(3) 0.007(3) 0.001(3) C19 0.010(3) 0.018(3) 0.021(3) 0.003(2) 0.000(2) 0.001(2) C4 0.024(3) 0.018(3) 0.017(3) 0.001(3) 0.003(3) -0.004(2) C8 0.019(3) 0.016(3) 0.031(4) 0.003(3) 0.014(3) 0.009(2) C17 0.021(3) 0.041(4) 0.019(3) 0.016(3) -0.001(3) 0.007(3) C34 0.026(3) 0.027(4) 0.034(4) 0.015(3) -0.009(3) -0.008(3) C33 0.026(3) 0.038(4) 0.014(3) 0.009(3) -0.003(3) -0.003(3) C32 0.018(3) 0.021(3) 0.018(3) 0.004(3) 0.002(2) -0.006(2) C22 0.037(4) 0.021(3) 0.035(4) 0.015(3) 0.007(3) 0.000(3) C24 0.055(5) 0.021(4) 0.025(4) 0.006(3) 0.014(3) 0.000(3) C23 0.065(5) 0.034(4) 0.019(4) 0.007(3) 0.021(4) -0.006(4) C15 0.022(3) 0.024(4) 0.031(4) 0.005(3) 0.004(3) 0.001(3) C16 0.019(3) 0.035(4) 0.019(3) 0.001(3) 0.003(3) -0.009(3) C28 0.020(3) 0.034(4) 0.019(3) 0.007(3) -0.002(3) 0.013(3) C27 0.017(3) 0.034(4) 0.025(4) 0.005(3) -0.009(3) 0.001(3) C29 0.033(4) 0.025(4) 0.028(4) 0.007(3) -0.003(3) 0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.2312(15) . ? Au1 Br1 2.3978(7) . ? Au2 P2 2.2243(15) . ? Au2 Br2 2.3896(8) . ? P1 C19 1.808(6) . ? P1 C1 1.805(6) . ? P1 C13 1.831(6) . ? P2 C10 1.793(6) . ? P2 C31 1.802(6) . ? P2 C25 1.815(6) . ? O1 C12 1.373(6) . ? O1 C11 1.388(7) . ? C18 C13 1.347(8) . ? C18 C17 1.386(8) . ? C18 H18 0.9500 . ? C11 C6 1.386(8) . ? C11 C10 1.397(8) . ? C12 C1 1.382(8) . ? C12 C5 1.390(8) . ? C10 C9 1.401(8) . ? C36 C35 1.372(9) . ? C36 C31 1.395(8) . ? C36 H36 0.9500 . ? C14 C15 1.384(9) . ? C14 C13 1.388(8) . ? C14 H14 0.9500 . ? C1 C2 1.409(8) . ? C25 C26 1.375(8) . ? C25 C30 1.376(9) . ? C9 C8 1.370(9) . ? C9 H9 0.9500 . ? C31 C32 1.379(8) . ? C21 C22 1.368(9) . ? C21 C20 1.383(8) . ? C21 H21 0.9500 . ? C20 C19 1.401(8) . ? C20 H20 0.9500 . ? C6 C7 1.399(8) . ? C6 C5 1.443(8) . ? C7 C8 1.366(9) . ? C7 H7 0.9500 . ? C2 C3 1.398(9) . ? C2 H2 0.9500 . ? C3 C4 1.402(9) . ? C3 H3 0.9500 . ? C26 C27 1.362(9) . ? C26 H26 0.9500 . ? C5 C4 1.385(9) . ? C30 C29 1.369(9) . ? C30 H30 0.9500 . ? C35 C34 1.384(9) . ? C35 H35 0.9500 . ? C19 C24 1.371(9) . ? C4 H4 0.9500 . ? C8 H8 0.9500 . ? C17 C16 1.383(10) . ? C17 H17 0.9500 . ? C34 C33 1.390(9) . ? C34 H34 0.9500 . ? C33 C32 1.398(9) . ? C33 H33 0.9500 . ? C32 H32 0.9500 . ? C22 C23 1.378(10) . ? C22 H22 0.9500 . ? C24 C23 1.379(9) . ? C24 H24 0.9500 . ? C23 H23 0.9500 . ? C15 C16 1.349(10) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C28 C27 1.371(10) . ? C28 C29 1.378(10) . ? C28 H28 0.9500 . ? C27 H27 0.9500 . ? C29 H29 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 Br1 175.47(4) . . ? P2 Au2 Br2 173.65(4) . . ? C19 P1 C1 108.8(3) . . ? C19 P1 C13 107.2(3) . . ? C1 P1 C13 103.6(3) . . ? C19 P1 Au1 112.66(19) . . ? C1 P1 Au1 114.0(2) . . ? C13 P1 Au1 109.92(19) . . ? C10 P2 C31 105.3(3) . . ? C10 P2 C25 103.2(3) . . ? C31 P2 C25 105.9(3) . . ? C10 P2 Au2 121.2(2) . . ? C31 P2 Au2 110.56(19) . . ? C25 P2 Au2 109.4(2) . . ? C12 O1 C11 105.1(4) . . ? C13 C18 C17 121.4(6) . . ? C13 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? O1 C11 C6 111.7(5) . . ? O1 C11 C10 124.3(5) . . ? C6 C11 C10 124.0(5) . . ? O1 C12 C1 124.7(5) . . ? O1 C12 C5 111.9(5) . . ? C1 C12 C5 123.4(5) . . ? C11 C10 C9 113.7(5) . . ? C11 C10 P2 124.3(5) . . ? C9 C10 P2 121.5(5) . . ? C35 C36 C31 120.5(6) . . ? C35 C36 H36 119.7 . . ? C31 C36 H36 119.7 . . ? C15 C14 C13 119.0(6) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? C12 C1 C2 116.3(5) . . ? C12 C1 P1 124.9(4) . . ? C2 C1 P1 118.6(5) . . ? C26 C25 C30 119.0(6) . . ? C26 C25 P2 117.6(5) . . ? C30 C25 P2 123.4(5) . . ? C8 C9 C10 123.2(6) . . ? C8 C9 H9 118.4 . . ? C10 C9 H9 118.4 . . ? C32 C31 C36 119.2(5) . . ? C32 C31 P2 122.7(4) . . ? C36 C31 P2 118.1(5) . . ? C18 C13 C14 119.8(6) . . ? C18 C13 P1 122.7(5) . . ? C14 C13 P1 117.5(5) . . ? C22 C21 C20 119.9(6) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C20 C19 120.5(5) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C11 C6 C7 119.3(5) . . ? C11 C6 C5 105.6(5) . . ? C7 C6 C5 135.1(6) . . ? C8 C7 C6 118.0(6) . . ? C8 C7 H7 121.0 . . ? C6 C7 H7 121.0 . . ? C3 C2 C1 121.1(6) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? C2 C3 C4 120.9(6) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C27 C26 C25 121.2(6) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C4 C5 C12 120.1(6) . . ? C4 C5 C6 134.2(6) . . ? C12 C5 C6 105.7(5) . . ? C29 C30 C25 119.8(6) . . ? C29 C30 H30 120.1 . . ? C25 C30 H30 120.1 . . ? C36 C35 C34 120.4(6) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C24 C19 C20 118.6(6) . . ? C24 C19 P1 119.6(5) . . ? C20 C19 P1 121.7(5) . . ? C5 C4 C3 118.2(6) . . ? C5 C4 H4 120.9 . . ? C3 C4 H4 120.9 . . ? C7 C8 C9 121.6(6) . . ? C7 C8 H8 119.2 . . ? C9 C8 H8 119.2 . . ? C16 C17 C18 118.4(6) . . ? C16 C17 H17 120.8 . . ? C18 C17 H17 120.8 . . ? C35 C34 C33 119.9(6) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C34 C33 C32 119.4(6) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C31 C32 C33 120.6(6) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C21 C22 C23 119.9(6) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C19 C24 C23 120.6(7) . . ? C19 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C22 C23 C24 120.5(6) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C16 C15 C14 120.8(6) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C17 120.5(6) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C27 C28 C29 119.3(6) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C26 C27 C28 119.8(6) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C30 C29 C28 120.7(6) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.147 _refine_diff_density_min -1.934 _refine_diff_density_rms 0.224 _platon_squeeze_details ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.500 0.500 257.9 109.2 ; _vrf_PLAT601_ju042308b_0m ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 218.00 A**3 RESPONSE: The structure contains disordered solvent molecules that were not able to be adequately resolved from one another. Platon was used to remove this electron density in an atttempt to attain a better quality structure solution. ; #===END data_ju050208_0m _database_code_depnum_ccdc_archive 'CCDC 750033' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H21 Au2 I2 O P2' _chemical_formula_weight 1179.20 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 9.5702(9) _cell_length_b 19.0596(18) _cell_length_c 19.3026(18) _cell_angle_alpha 90.00 _cell_angle_beta 103.1610(10) _cell_angle_gamma 90.00 _cell_volume 3428.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9927 _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 28.78 _exptl_crystal_description Irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2156 _exptl_absorpt_coefficient_mu 10.470 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1024 _exptl_absorpt_correction_T_max 0.4207 _exptl_absorpt_process_details 'AXScale in APEX 2 (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 40442 _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7882 _reflns_number_gt 7171 _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^)+(0.0149P)^2^+12.0341P] 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 7882 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0291 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0573 _refine_ls_wR_factor_gt 0.0561 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.057 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.389308(17) 0.120827(9) 0.135255(9) 0.01703(5) Uani 1 1 d . . . Au2 Au 0.220320(18) 0.137415(9) 0.256727(9) 0.01937(5) Uani 1 1 d . . . I1 I 0.42985(3) 0.002914(14) 0.201887(15) 0.01914(7) Uani 1 1 d . . . I2 I 0.46305(3) 0.187290(17) 0.325024(17) 0.02611(7) Uani 1 1 d . . . P2 P -0.01847(11) 0.11940(6) 0.22626(6) 0.0149(2) Uani 1 1 d . . . P1 P 0.31628(11) 0.20679(6) 0.05506(6) 0.0151(2) Uani 1 1 d . . . C1 C -0.0618(4) 0.0936(2) 0.0805(2) 0.0158(8) Uani 1 1 d . . . C3 C -0.2296(4) 0.0385(2) 0.1331(2) 0.0170(9) Uani 1 1 d . . . H3 H -0.2667 0.0271 0.1733 0.020 Uiso 1 1 calc R . . C2 C -0.1080(4) 0.0807(2) 0.1420(2) 0.0164(8) Uani 1 1 d . . . C12 C 0.0675(5) 0.1335(2) 0.0089(2) 0.0168(9) Uani 1 1 d . . . C7 C -0.0403(4) 0.0948(2) -0.0341(2) 0.0167(9) Uani 1 1 d . . . C30 C -0.0717(5) 0.0638(2) 0.2920(2) 0.0193(9) Uani 1 1 d . . . C29 C -0.1963(5) 0.0769(3) 0.3160(2) 0.0227(10) Uani 1 1 d . . . H29 H -0.2561 0.1156 0.2979 0.027 Uiso 1 1 calc R . . C25 C 0.0140(6) 0.0076(3) 0.3186(3) 0.0310(11) Uani 1 1 d . . . H25 H 0.0979 -0.0019 0.3017 0.037 Uiso 1 1 calc R . . C31 C -0.1064(4) 0.2034(2) 0.2281(2) 0.0169(9) Uani 1 1 d . . . C36 C -0.0408(5) 0.2518(3) 0.2790(3) 0.0241(10) Uani 1 1 d . . . H36 H 0.0462 0.2398 0.3116 0.029 Uiso 1 1 calc R . . C13 C 0.4473(4) 0.2441(2) 0.0117(2) 0.0159(8) Uani 1 1 d . . . C14 C 0.4393(5) 0.3141(2) -0.0104(2) 0.0206(9) Uani 1 1 d . . . H14 H 0.3608 0.3424 -0.0049 0.025 Uiso 1 1 calc R . . C19 C 0.2258(5) 0.2788(2) 0.0873(3) 0.0223(10) Uani 1 1 d . . . O1 O 0.0559(3) 0.13478(16) 0.07884(16) 0.0173(6) Uani 1 1 d . . . C10 C 0.1747(5) 0.1613(2) -0.0857(2) 0.0169(9) Uani 1 1 d . . . H10 H 0.2468 0.1835 -0.1046 0.020 Uiso 1 1 calc R . . C5 C -0.2477(4) 0.0263(2) 0.0066(2) 0.0176(9) Uani 1 1 d . . . H5 H -0.2950 0.0076 -0.0383 0.021 Uiso 1 1 calc R . . C9 C 0.0660(5) 0.1233(2) -0.1307(2) 0.0200(9) Uani 1 1 d . . . H9 H 0.0658 0.1204 -0.1799 0.024 Uiso 1 1 calc R . . C4 C -0.2979(5) 0.0127(2) 0.0666(2) 0.0200(9) Uani 1 1 d . . . H4 H -0.3816 -0.0152 0.0624 0.024 Uiso 1 1 calc R . . C6 C -0.1261(5) 0.0681(2) 0.0131(2) 0.0172(9) Uani 1 1 d . . . C11 C 0.1784(4) 0.1671(2) -0.0131(2) 0.0143(8) Uani 1 1 d . . . C34 C -0.2241(6) 0.3361(3) 0.2338(3) 0.0283(11) Uani 1 1 d . . . H34 H -0.2637 0.3816 0.2350 0.034 Uiso 1 1 calc R . . C16 C 0.6598(5) 0.3006(3) -0.0484(3) 0.0276(11) Uani 1 1 d . . . H16 H 0.7333 0.3201 -0.0682 0.033 Uiso 1 1 calc R . . C35 C -0.1010(6) 0.3175(3) 0.2825(3) 0.0286(11) Uani 1 1 d . . . H35 H -0.0572 0.3496 0.3186 0.034 Uiso 1 1 calc R . . C33 C -0.2898(6) 0.2880(3) 0.1831(3) 0.0307(11) Uani 1 1 d . . . H33 H -0.3753 0.3006 0.1498 0.037 Uiso 1 1 calc R . . C32 C -0.2329(5) 0.2221(3) 0.1804(3) 0.0249(10) Uani 1 1 d . . . H32 H -0.2801 0.1892 0.1459 0.030 Uiso 1 1 calc R . . C18 C 0.5612(5) 0.2024(2) 0.0021(2) 0.0214(9) Uani 1 1 d . . . H18 H 0.5663 0.1545 0.0161 0.026 Uiso 1 1 calc R . . C15 C 0.5453(5) 0.3423(2) -0.0400(2) 0.0236(10) Uani 1 1 d . . . H15 H 0.5400 0.3900 -0.0546 0.028 Uiso 1 1 calc R . . C27 C -0.1453(7) -0.0223(3) 0.3941(3) 0.0375(13) Uani 1 1 d . . . H27 H -0.1699 -0.0515 0.4294 0.045 Uiso 1 1 calc R . . C8 C -0.0412(5) 0.0898(2) -0.1063(2) 0.0200(9) Uani 1 1 d . . . H8 H -0.1138 0.0640 -0.1378 0.024 Uiso 1 1 calc R . . C20 C 0.2755(5) 0.3022(2) 0.1566(3) 0.0242(10) Uani 1 1 d . . . C26 C -0.0221(7) -0.0353(3) 0.3702(3) 0.0408(14) Uani 1 1 d . . . H26 H 0.0380 -0.0736 0.3890 0.049 Uiso 1 1 calc R . . C17 C 0.6668(5) 0.2309(3) -0.0280(3) 0.0274(11) Uani 1 1 d . . . H17 H 0.7443 0.2025 -0.0346 0.033 Uiso 1 1 calc R . . C28 C -0.2316(6) 0.0329(3) 0.3666(3) 0.0302(11) Uani 1 1 d . . . H28 H -0.3171 0.0412 0.3824 0.036 Uiso 1 1 calc R . . C22 C 0.0951(16) 0.3977(8) 0.1310(8) 0.035(3) Uani 0.50 1 d P . . C21 C 0.2036(6) 0.3556(3) 0.1837(3) 0.0383(14) Uani 1 1 d . . . C23A C 0.0506(12) 0.3760(6) 0.0610(6) 0.028(2) Uani 0.50 1 d P . . C23 C 0.0107(12) 0.3452(6) 0.0837(7) 0.033(3) Uani 0.50 1 d P . . C22A C 0.0701(16) 0.3713(7) 0.1508(8) 0.033(3) Uani 0.50 1 d P . . C24 C 0.0904(19) 0.2981(8) 0.0514(8) 0.024(3) Uani 0.50 1 d P . . C24A C 0.116(2) 0.3193(9) 0.0360(10) 0.030(4) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01649(8) 0.01762(8) 0.01631(9) 0.00300(6) 0.00235(6) -0.00122(6) Au2 0.01456(8) 0.02421(9) 0.01811(9) -0.00216(7) 0.00117(6) -0.00241(6) I1 0.01978(14) 0.01812(14) 0.01847(14) 0.00407(11) 0.00217(11) -0.00188(11) I2 0.01612(14) 0.03527(18) 0.02541(16) -0.00834(13) 0.00153(12) -0.00496(12) P2 0.0134(5) 0.0168(5) 0.0138(5) 0.0000(4) 0.0015(4) -0.0015(4) P1 0.0158(5) 0.0155(5) 0.0141(5) 0.0007(4) 0.0033(4) 0.0000(4) C1 0.016(2) 0.0129(19) 0.018(2) -0.0015(16) 0.0036(17) -0.0018(16) C3 0.016(2) 0.016(2) 0.018(2) 0.0005(17) 0.0026(17) -0.0015(16) C2 0.017(2) 0.017(2) 0.013(2) -0.0005(16) 0.0002(16) 0.0028(16) C12 0.021(2) 0.016(2) 0.014(2) -0.0005(16) 0.0042(17) 0.0029(17) C7 0.016(2) 0.0126(19) 0.022(2) -0.0004(17) 0.0040(17) 0.0014(16) C30 0.022(2) 0.018(2) 0.016(2) 0.0012(17) 0.0017(17) -0.0072(17) C29 0.021(2) 0.027(2) 0.018(2) 0.0013(19) 0.0028(18) -0.0079(19) C25 0.039(3) 0.027(3) 0.028(3) 0.003(2) 0.010(2) 0.004(2) C31 0.017(2) 0.021(2) 0.014(2) 0.0009(17) 0.0046(16) -0.0024(17) C36 0.027(2) 0.026(2) 0.019(2) -0.0016(19) 0.0034(19) -0.004(2) C13 0.015(2) 0.020(2) 0.012(2) 0.0021(16) 0.0003(16) -0.0018(16) C14 0.022(2) 0.017(2) 0.021(2) 0.0007(17) 0.0023(18) -0.0020(18) C19 0.020(2) 0.023(2) 0.023(2) -0.0052(19) 0.0039(19) 0.0005(18) O1 0.0156(14) 0.0224(16) 0.0131(15) -0.0010(12) 0.0015(12) -0.0037(12) C10 0.022(2) 0.014(2) 0.016(2) 0.0035(16) 0.0060(17) 0.0048(16) C5 0.014(2) 0.018(2) 0.018(2) -0.0032(17) -0.0036(17) -0.0002(16) C9 0.026(2) 0.022(2) 0.011(2) -0.0021(17) 0.0030(17) 0.0023(18) C4 0.016(2) 0.018(2) 0.025(2) -0.0022(18) 0.0037(18) -0.0011(17) C6 0.018(2) 0.014(2) 0.019(2) -0.0003(16) 0.0030(17) 0.0044(16) C11 0.015(2) 0.0129(19) 0.015(2) -0.0023(16) 0.0047(16) 0.0019(16) C34 0.037(3) 0.021(2) 0.030(3) 0.000(2) 0.015(2) 0.005(2) C16 0.019(2) 0.043(3) 0.019(2) 0.007(2) 0.0011(18) -0.011(2) C35 0.038(3) 0.026(3) 0.022(3) -0.006(2) 0.006(2) -0.003(2) C33 0.028(3) 0.030(3) 0.031(3) 0.000(2) 0.000(2) 0.006(2) C32 0.024(2) 0.023(2) 0.025(3) -0.0030(19) -0.0002(19) 0.0015(19) C18 0.019(2) 0.024(2) 0.020(2) 0.0028(18) 0.0019(18) 0.0030(18) C15 0.031(3) 0.020(2) 0.016(2) 0.0063(18) -0.0010(19) -0.0054(19) C27 0.057(4) 0.028(3) 0.029(3) 0.008(2) 0.012(3) -0.014(3) C8 0.021(2) 0.021(2) 0.016(2) -0.0035(17) -0.0019(17) 0.0006(18) C20 0.029(2) 0.021(2) 0.023(2) -0.0033(19) 0.007(2) -0.0060(19) C26 0.057(4) 0.026(3) 0.037(3) 0.011(2) 0.008(3) 0.007(3) C17 0.022(2) 0.037(3) 0.024(3) 0.005(2) 0.008(2) 0.004(2) C28 0.030(3) 0.041(3) 0.019(2) 0.001(2) 0.004(2) -0.013(2) C22 0.037(7) 0.031(8) 0.042(9) -0.013(6) 0.019(6) 0.008(6) C21 0.035(3) 0.045(3) 0.034(3) -0.022(3) 0.008(2) -0.002(3) C23A 0.030(6) 0.031(6) 0.024(6) -0.010(5) 0.008(5) 0.003(5) C23 0.028(6) 0.027(6) 0.038(7) -0.011(5) -0.001(5) 0.003(5) C22A 0.036(7) 0.032(8) 0.032(8) -0.014(6) 0.007(6) 0.002(6) C24 0.033(8) 0.021(8) 0.015(7) -0.006(5) -0.002(5) 0.009(6) C24A 0.034(8) 0.027(9) 0.030(9) 0.000(6) 0.010(6) 0.012(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 Au1 P1 2.2532(11) . ? Au1 I1 2.5745(4) . ? Au1 Au2 3.1528(3) . ? Au2 P2 2.2526(11) . ? Au2 I2 2.5775(4) . ? P2 C31 1.813(4) . ? P2 C30 1.814(4) . ? P2 C2 1.813(4) . ? P1 C11 1.803(4) . ? P1 C13 1.805(4) . ? P1 C19 1.808(5) . ? C1 C2 1.380(6) . ? C1 O1 1.379(5) . ? C1 C6 1.393(6) . ? C3 C2 1.393(6) . ? C3 C4 1.392(6) . ? C3 H3 0.9500 . ? C12 C7 1.380(6) . ? C12 O1 1.380(5) . ? C12 C11 1.386(6) . ? C7 C8 1.394(6) . ? C7 C6 1.452(6) . ? C30 C25 1.375(7) . ? C30 C29 1.396(6) . ? C29 C28 1.386(7) . ? C29 H29 0.9500 . ? C25 C26 1.392(7) . ? C25 H25 0.9500 . ? C31 C32 1.390(6) . ? C31 C36 1.389(6) . ? C36 C35 1.386(7) . ? C36 H36 0.9500 . ? C13 C14 1.397(6) . ? C13 C18 1.395(6) . ? C14 C15 1.382(6) . ? C14 H14 0.9500 . ? C19 C24 1.374(18) . ? C19 C20 1.387(7) . ? C19 C24A 1.486(18) . ? C10 C11 1.399(6) . ? C10 C9 1.397(6) . ? C10 H10 0.9500 . ? C5 C4 1.375(6) . ? C5 C6 1.392(6) . ? C5 H5 0.9500 . ? C9 C8 1.379(6) . ? C9 H9 0.9500 . ? C4 H4 0.9500 . ? C34 C35 1.376(7) . ? C34 C33 1.383(7) . ? C34 H34 0.9500 . ? C16 C17 1.382(7) . ? C16 C15 1.393(7) . ? C16 H16 0.9500 . ? C35 H35 0.9500 . ? C33 C32 1.375(7) . ? C33 H33 0.9500 . ? C32 H32 0.9500 . ? C18 C17 1.386(6) . ? C18 H18 0.9500 . ? C15 H15 0.9500 . ? C27 C28 1.367(8) . ? C27 C26 1.383(9) . ? C27 H27 0.9500 . ? C8 H8 0.9500 . ? C20 C21 1.396(7) . ? C26 H26 0.9500 . ? C17 H17 0.9500 . ? C28 H28 0.9500 . ? C22 C22A 0.705(15) . ? C22 C23A 1.384(19) . ? C22 C21 1.508(17) . ? C21 C22A 1.325(16) . ? C23A C23 0.872(14) . ? C23A C24A 1.39(2) . ? C23 C22A 1.383(18) . ? C23 C24 1.41(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 P1 Au1 I1 164.99(3) . . ? P1 Au1 Au2 107.86(3) . . ? I1 Au1 Au2 76.142(9) . . ? P2 Au2 I2 158.81(3) . . ? P2 Au2 Au1 116.89(3) . . ? I2 Au2 Au1 82.078(11) . . ? C31 P2 C30 107.3(2) . . ? C31 P2 C2 104.5(2) . . ? C30 P2 C2 103.9(2) . . ? C31 P2 Au2 107.95(14) . . ? C30 P2 Au2 109.65(15) . . ? C2 P2 Au2 122.70(14) . . ? C11 P1 C13 107.28(19) . . ? C11 P1 C19 104.0(2) . . ? C13 P1 C19 107.4(2) . . ? C11 P1 Au1 104.87(14) . . ? C13 P1 Au1 117.74(14) . . ? C19 P1 Au1 114.41(16) . . ? C2 C1 O1 123.0(4) . . ? C2 C1 C6 125.5(4) . . ? O1 C1 C6 111.5(4) . . ? C2 C3 C4 121.4(4) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C1 C2 C3 114.8(4) . . ? C1 C2 P2 121.4(3) . . ? C3 C2 P2 123.8(3) . . ? C7 C12 O1 112.5(4) . . ? C7 C12 C11 125.6(4) . . ? O1 C12 C11 121.9(4) . . ? C12 C7 C8 118.1(4) . . ? C12 C7 C6 105.2(4) . . ? C8 C7 C6 136.7(4) . . ? C25 C30 C29 119.9(4) . . ? C25 C30 P2 118.5(4) . . ? C29 C30 P2 121.7(4) . . ? C28 C29 C30 119.3(5) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? C30 C25 C26 120.0(5) . . ? C30 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C32 C31 C36 118.9(4) . . ? C32 C31 P2 123.5(3) . . ? C36 C31 P2 117.6(3) . . ? C35 C36 C31 120.6(4) . . ? C35 C36 H36 119.7 . . ? C31 C36 H36 119.7 . . ? C14 C13 C18 119.6(4) . . ? C14 C13 P1 121.4(3) . . ? C18 C13 P1 118.9(3) . . ? C15 C14 C13 120.2(4) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C24 C19 C20 118.6(8) . . ? C24 C19 C24A 23.4(7) . . ? C20 C19 C24A 120.8(8) . . ? C24 C19 P1 120.0(7) . . ? C20 C19 P1 119.4(4) . . ? C24A C19 P1 119.0(8) . . ? C1 O1 C12 105.1(3) . . ? C11 C10 C9 120.6(4) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C4 C5 C6 118.4(4) . . ? C4 C5 H5 120.8 . . ? C6 C5 H5 120.8 . . ? C8 C9 C10 122.3(4) . . ? C8 C9 H9 118.9 . . ? C10 C9 H9 118.9 . . ? C5 C4 C3 122.0(4) . . ? C5 C4 H4 119.0 . . ? C3 C4 H4 119.0 . . ? C1 C6 C5 117.9(4) . . ? C1 C6 C7 105.7(4) . . ? C5 C6 C7 136.4(4) . . ? C12 C11 C10 115.1(4) . . ? C12 C11 P1 117.1(3) . . ? C10 C11 P1 127.7(3) . . ? C35 C34 C33 119.6(5) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C17 C16 C15 120.3(4) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C34 C35 C36 120.0(5) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C32 C33 C34 120.8(5) . . ? C32 C33 H33 119.6 . . ? C34 C33 H33 119.6 . . ? C33 C32 C31 120.1(4) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C17 C18 C13 119.8(4) . . ? C17 C18 H18 120.1 . . ? C13 C18 H18 120.1 . . ? C14 C15 C16 119.8(4) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C28 C27 C26 119.6(5) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C9 C8 C7 118.3(4) . . ? C9 C8 H8 120.9 . . ? C7 C8 H8 120.9 . . ? C19 C20 C21 120.3(5) . . ? C27 C26 C25 120.2(5) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C18 C17 C16 120.3(5) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C27 C28 C29 121.1(5) . . ? C27 C28 H28 119.5 . . ? C29 C28 H28 119.5 . . ? C22A C22 C23A 104(2) . . ? C22A C22 C21 61(2) . . ? C23A C22 C21 120.7(11) . . ? C22A C21 C20 119.3(7) . . ? C22A C21 C22 27.9(6) . . ? C20 C21 C22 117.3(7) . . ? C23 C23A C22 77.4(13) . . ? C23 C23A C24A 86.3(14) . . ? C22 C23A C24A 120.5(13) . . ? C23A C23 C22A 95.4(13) . . ? C23A C23 C24 82.2(14) . . ? C22A C23 C24 119.7(12) . . ? C22 C22A C21 91(2) . . ? C22 C22A C23 82(2) . . ? C21 C22A C23 120.9(12) . . ? C19 C24 C23 119.3(12) . . ? C23A C24A C19 118.6(14) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.095 _refine_diff_density_min -1.024 _refine_diff_density_rms 0.153 #===END data_ju022008a_0m _database_code_depnum_ccdc_archive 'CCDC 750034' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H32 Au2 Br2 O P2' _chemical_formula_sum 'C39 H32 Au2 Br2 O P2' _chemical_formula_weight 1132.34 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' P P 0.1023 0.0942 '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 _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.5328(19) _cell_length_b 18.360(3) _cell_length_c 19.185(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.391(2) _cell_angle_gamma 90.00 _cell_volume 3687.1(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9097 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 26.76 _exptl_crystal_description Needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.040 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2128 _exptl_absorpt_coefficient_mu 10.232 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0974 _exptl_absorpt_correction_T_max 0.3593 _exptl_absorpt_process_details 'AXScale in APEX2 (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 33682 _diffrn_reflns_av_R_equivalents 0.0815 _diffrn_reflns_av_sigmaI/netI 0.0682 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 26.91 _reflns_number_total 7742 _reflns_number_gt 6188 _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^)+(0.0945P)^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 7742 _refine_ls_number_parameters 417 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0667 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1416 _refine_ls_wR_factor_gt 0.1331 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 Au2 Au 0.36913(3) 0.288493(18) 0.766045(17) 0.01895(12) Uani 1 1 d . . . Au1 Au 0.64472(3) 0.265427(19) 0.793996(19) 0.02170(12) Uani 1 1 d . . . Br1 Br 0.63092(8) 0.13801(5) 0.82171(6) 0.0332(2) Uani 1 1 d . . . Br2 Br 0.40426(8) 0.25177(5) 0.64944(5) 0.0267(2) Uani 1 1 d . . . P2 P 0.32671(17) 0.33802(12) 0.86704(12) 0.0180(4) Uani 1 1 d . . . P1 P 0.69914(18) 0.37697(13) 0.76240(12) 0.0202(5) Uani 1 1 d . . . C29 C 0.5368(7) 0.2838(5) 0.9503(5) 0.0234(19) Uani 1 1 d . . . H29 H 0.5292 0.2425 0.9202 0.028 Uiso 1 1 calc R . . C39 C 0.0803(7) 0.2838(5) 0.8631(5) 0.0223(19) Uani 1 1 d . . . H39 H 0.0704 0.2992 0.8155 0.027 Uiso 1 1 calc R . . C28 C 0.4530(6) 0.3433(5) 0.9370(5) 0.0205(18) Uani 1 1 d . . . C33 C 0.4634(7) 0.4011(5) 0.9837(4) 0.0217(18) Uani 1 1 d . . . H33 H 0.4068 0.4414 0.9766 0.026 Uiso 1 1 calc R . . C34 C 0.1955(7) 0.2950(5) 0.9058(5) 0.0226(19) Uani 1 1 d . . . C11 C 0.2733(7) 0.4296(5) 0.8480(4) 0.0177(17) Uani 1 1 d . . . C35 C 0.2067(8) 0.2722(5) 0.9752(5) 0.030(2) Uani 1 1 d . . . H35 H 0.2840 0.2807 1.0046 0.035 Uiso 1 1 calc R . . O1 O 0.4527(4) 0.4490(3) 0.7873(3) 0.0202(13) Uani 1 1 d . . . C30 C 0.6293(8) 0.2852(5) 1.0065(5) 0.0227(19) Uani 1 1 d . . . H30 H 0.6874 0.2457 1.0144 0.027 Uiso 1 1 calc R . . C7 C 0.2790(7) 0.5352(5) 0.7725(4) 0.0207(18) Uani 1 1 d . . . C31 C 0.6382(7) 0.3437(5) 1.0516(5) 0.026(2) Uani 1 1 d . . . H31 H 0.7023 0.3445 1.0905 0.031 Uiso 1 1 calc R . . C13 C 0.4899(7) 0.4673(5) 0.7225(4) 0.0196(18) Uani 1 1 d . . . C36 C 0.1075(9) 0.2377(5) 1.0017(5) 0.030(2) Uani 1 1 d . . . H36 H 0.1169 0.2214 1.0490 0.036 Uiso 1 1 calc R . . C12 C 0.3347(7) 0.4725(5) 0.8017(5) 0.0233(19) Uani 1 1 d . . . C37 C -0.0040(9) 0.2267(6) 0.9609(6) 0.035(2) Uani 1 1 d . . . H37 H -0.0727 0.2029 0.9797 0.041 Uiso 1 1 calc R . . C32 C 0.5559(7) 0.4002(5) 1.0404(5) 0.028(2) Uani 1 1 d . . . H32 H 0.5620 0.4400 1.0723 0.034 Uiso 1 1 calc R . . C16 C 0.8394(7) 0.3655(5) 0.7178(5) 0.0217(19) Uani 1 1 d . . . C21 C 0.8546(7) 0.3005(5) 0.6821(5) 0.0236(19) Uani 1 1 d . . . H21 H 0.7903 0.2642 0.6812 0.028 Uiso 1 1 calc R . . C6 C 0.3445(7) 0.5762(5) 0.7171(5) 0.027(2) Uani 1 1 d . . . C22 C 0.7442(7) 0.4418(5) 0.8320(4) 0.0220(19) Uani 1 1 d . . . C38 C -0.0183(8) 0.2499(5) 0.8920(6) 0.031(2) Uani 1 1 d . . . H38 H -0.0975 0.2425 0.8641 0.037 Uiso 1 1 calc R . . C23 C 0.7836(7) 0.4164(5) 0.8993(4) 0.025(2) Uani 1 1 d . . . H23 H 0.7840 0.3655 0.9087 0.030 Uiso 1 1 calc R . . C9 C 0.1106(7) 0.5219(5) 0.8453(5) 0.025(2) Uani 1 1 d . . . H9 H 0.0370 0.5413 0.8631 0.031 Uiso 1 1 calc R . . C1 C 0.5942(7) 0.4302(5) 0.7016(4) 0.0215(19) Uani 1 1 d . . . C10 C 0.1606(7) 0.4561(5) 0.8696(5) 0.0248(19) Uani 1 1 d . . . H10 H 0.1174 0.4286 0.9017 0.030 Uiso 1 1 calc R . . C27 C 0.7451(7) 0.5163(5) 0.8181(5) 0.025(2) Uani 1 1 d . . . H27 H 0.7191 0.5338 0.7721 0.029 Uiso 1 1 calc R . . C5 C 0.4320(7) 0.5240(5) 0.6830(5) 0.025(2) Uani 1 1 d . . . C17 C 0.9337(7) 0.4178(6) 0.7182(5) 0.030(2) Uani 1 1 d . . . H17 H 0.9248 0.4628 0.7417 0.036 Uiso 1 1 calc R . . C18 C 1.0400(8) 0.4051(6) 0.6849(5) 0.030(2) Uani 1 1 d . . . H18 H 1.1048 0.4412 0.6860 0.036 Uiso 1 1 calc R . . C26 C 0.7839(7) 0.5645(5) 0.8712(5) 0.029(2) Uani 1 1 d . . . H26 H 0.7845 0.6152 0.8615 0.035 Uiso 1 1 calc R . . C20 C 0.9613(9) 0.2879(6) 0.6480(5) 0.032(2) Uani 1 1 d . . . H20 H 0.9702 0.2435 0.6236 0.038 Uiso 1 1 calc R . . C25 C 0.8223(7) 0.5400(6) 0.9390(5) 0.032(2) Uani 1 1 d . . . H25 H 0.8481 0.5735 0.9755 0.039 Uiso 1 1 calc R . . C19 C 1.0539(8) 0.3403(6) 0.6498(5) 0.035(2) Uani 1 1 d . . . H19 H 1.1281 0.3321 0.6269 0.042 Uiso 1 1 calc R . . C8 C 0.1670(7) 0.5586(5) 0.7959(5) 0.028(2) Uani 1 1 d . . . H8 H 0.1280 0.6019 0.7767 0.034 Uiso 1 1 calc R . . C24 C 0.8221(8) 0.4651(6) 0.9524(5) 0.031(2) Uani 1 1 d . . . H24 H 0.8487 0.4477 0.9983 0.038 Uiso 1 1 calc R . . C2 C 0.6261(8) 0.4427(6) 0.6343(5) 0.037(3) Uani 1 1 d . . . H2 H 0.6931 0.4156 0.6173 0.045 Uiso 1 1 calc R . . C15 C 0.2479(8) 0.6117(5) 0.6641(5) 0.029(2) Uani 1 1 d . . . H15A H 0.1972 0.6468 0.6878 0.044 Uiso 1 1 calc R . . H15B H 0.1914 0.5744 0.6410 0.044 Uiso 1 1 calc R . . H15C H 0.2922 0.6371 0.6289 0.044 Uiso 1 1 calc R . . C14 C 0.4317(8) 0.6343(5) 0.7568(5) 0.033(2) Uani 1 1 d . . . H14A H 0.4839 0.6578 0.7242 0.049 Uiso 1 1 calc R . . H14B H 0.4875 0.6107 0.7945 0.049 Uiso 1 1 calc R . . H14C H 0.3787 0.6709 0.7769 0.049 Uiso 1 1 calc R . . C4 C 0.4682(9) 0.5359(6) 0.6172(5) 0.039(3) Uani 1 1 d . . . H4 H 0.4280 0.5735 0.5888 0.047 Uiso 1 1 calc R . . C3 C 0.5607(9) 0.4945(7) 0.5920(5) 0.046(3) Uani 1 1 d . . . H3 H 0.5802 0.5014 0.5452 0.055 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 Au2 0.01509(16) 0.0190(2) 0.0232(2) -0.00182(13) 0.00404(12) -0.00092(11) Au1 0.01535(16) 0.0203(2) 0.0296(2) -0.00189(14) 0.00293(13) 0.00059(11) Br1 0.0310(4) 0.0211(5) 0.0488(6) 0.0002(4) 0.0105(4) 0.0005(4) Br2 0.0238(4) 0.0327(5) 0.0246(5) -0.0070(4) 0.0067(3) -0.0052(3) P2 0.0144(8) 0.0183(12) 0.0218(12) -0.0018(9) 0.0037(7) 0.0019(8) P1 0.0159(9) 0.0195(12) 0.0250(13) -0.0033(10) 0.0016(8) 0.0012(8) C29 0.020(4) 0.021(5) 0.030(5) 0.005(4) 0.006(3) 0.003(3) C39 0.015(4) 0.024(5) 0.028(5) -0.001(4) 0.005(3) 0.003(3) C28 0.009(3) 0.025(5) 0.028(5) -0.001(4) 0.004(3) 0.001(3) C33 0.020(4) 0.018(5) 0.028(5) -0.004(4) 0.005(3) 0.000(3) C34 0.020(4) 0.016(5) 0.032(5) -0.003(4) 0.006(3) -0.003(3) C11 0.018(3) 0.019(5) 0.017(4) -0.002(3) 0.006(3) -0.002(3) C35 0.024(4) 0.032(6) 0.032(6) -0.002(4) -0.001(4) -0.005(4) O1 0.013(2) 0.021(3) 0.027(3) 0.004(3) 0.005(2) 0.006(2) C30 0.025(4) 0.028(5) 0.016(5) 0.010(4) 0.008(3) 0.006(3) C7 0.026(4) 0.014(4) 0.021(5) 0.000(4) 0.000(3) 0.000(3) C31 0.022(4) 0.032(5) 0.023(5) 0.005(4) -0.005(3) -0.006(4) C13 0.019(4) 0.016(4) 0.022(5) -0.003(4) -0.003(3) -0.003(3) C36 0.032(5) 0.035(6) 0.026(6) 0.008(4) 0.011(4) 0.004(4) C12 0.013(3) 0.024(5) 0.032(5) -0.005(4) -0.003(3) 0.004(3) C37 0.025(4) 0.039(6) 0.042(7) 0.000(5) 0.015(4) -0.003(4) C32 0.024(4) 0.026(5) 0.033(6) -0.002(4) 0.000(4) -0.005(4) C16 0.021(4) 0.018(5) 0.025(5) -0.007(4) -0.001(3) 0.007(3) C21 0.020(4) 0.028(5) 0.022(5) 0.001(4) 0.001(3) 0.002(3) C6 0.022(4) 0.020(5) 0.038(6) -0.008(4) -0.004(4) 0.003(3) C22 0.016(3) 0.029(5) 0.022(5) -0.005(4) 0.006(3) 0.003(3) C38 0.020(4) 0.024(5) 0.051(7) -0.002(5) 0.010(4) -0.005(4) C23 0.020(4) 0.034(6) 0.021(5) 0.003(4) 0.006(3) 0.000(3) C9 0.021(4) 0.027(5) 0.028(5) -0.001(4) 0.003(3) 0.004(3) C1 0.015(3) 0.027(5) 0.022(5) -0.009(4) 0.002(3) -0.003(3) C10 0.018(4) 0.022(5) 0.035(5) -0.002(4) 0.006(3) -0.001(3) C27 0.018(4) 0.022(5) 0.032(5) -0.006(4) -0.002(3) -0.002(3) C5 0.022(4) 0.022(5) 0.028(5) 0.004(4) -0.006(3) 0.003(3) C17 0.019(4) 0.038(6) 0.034(6) -0.009(5) 0.004(3) -0.003(4) C18 0.021(4) 0.040(6) 0.030(5) -0.011(5) 0.003(3) -0.003(4) C26 0.021(4) 0.020(5) 0.048(6) -0.003(4) 0.005(4) -0.002(3) C20 0.036(5) 0.031(6) 0.030(6) -0.008(4) 0.014(4) 0.008(4) C25 0.021(4) 0.040(6) 0.036(6) -0.015(5) 0.004(4) -0.009(4) C19 0.020(4) 0.048(7) 0.038(6) 0.001(5) 0.011(4) 0.004(4) C8 0.017(4) 0.022(5) 0.045(6) -0.005(4) -0.001(4) 0.001(3) C24 0.030(4) 0.037(6) 0.028(5) -0.004(5) 0.008(4) 0.000(4) C2 0.025(4) 0.064(8) 0.025(5) -0.009(5) 0.008(4) 0.015(4) C15 0.034(4) 0.026(5) 0.028(5) 0.005(4) 0.001(4) 0.008(4) C14 0.030(4) 0.023(5) 0.046(6) -0.002(5) 0.004(4) -0.001(4) C4 0.040(5) 0.052(7) 0.026(6) 0.013(5) 0.005(4) 0.024(5) C3 0.044(5) 0.074(9) 0.021(5) 0.019(6) 0.008(4) 0.027(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 Au2 P2 2.230(2) . ? Au2 Br2 2.4043(10) . ? Au2 Au1 2.9233(6) . ? Au1 P1 2.229(2) . ? Au1 Br1 2.4071(11) . ? P2 C28 1.784(8) . ? P2 C11 1.797(9) . ? P2 C34 1.821(9) . ? P1 C16 1.801(9) . ? P1 C1 1.802(9) . ? P1 C22 1.813(9) . ? C29 C30 1.371(12) . ? C29 C28 1.410(11) . ? C29 H29 0.9500 . ? C39 C38 1.379(12) . ? C39 C34 1.402(11) . ? C39 H39 0.9500 . ? C28 C33 1.386(12) . ? C33 C32 1.378(11) . ? C33 H33 0.9500 . ? C34 C35 1.388(13) . ? C11 C10 1.389(10) . ? C11 C12 1.399(12) . ? C35 C36 1.367(13) . ? C35 H35 0.9500 . ? O1 C12 1.373(9) . ? O1 C13 1.385(10) . ? C30 C31 1.375(13) . ? C30 H30 0.9500 . ? C7 C8 1.377(11) . ? C7 C12 1.381(12) . ? C7 C6 1.528(13) . ? C31 C32 1.354(12) . ? C31 H31 0.9500 . ? C13 C5 1.388(12) . ? C13 C1 1.390(11) . ? C36 C37 1.352(14) . ? C36 H36 0.9500 . ? C37 C38 1.381(14) . ? C37 H37 0.9500 . ? C32 H32 0.9500 . ? C16 C17 1.382(12) . ? C16 C21 1.392(12) . ? C21 C20 1.382(12) . ? C21 H21 0.9500 . ? C6 C15 1.506(11) . ? C6 C5 1.527(12) . ? C6 C14 1.550(12) . ? C22 C23 1.391(12) . ? C22 C27 1.393(13) . ? C38 H38 0.9500 . ? C23 C24 1.383(13) . ? C23 H23 0.9500 . ? C9 C8 1.354(13) . ? C9 C10 1.377(12) . ? C9 H9 0.9500 . ? C1 C2 1.390(13) . ? C10 H10 0.9500 . ? C27 C26 1.376(12) . ? C27 H27 0.9500 . ? C5 C4 1.376(13) . ? C17 C18 1.369(12) . ? C17 H17 0.9500 . ? C18 C19 1.384(14) . ? C18 H18 0.9500 . ? C26 C25 1.392(13) . ? C26 H26 0.9500 . ? C20 C19 1.367(13) . ? C20 H20 0.9500 . ? C25 C24 1.398(15) . ? C25 H25 0.9500 . ? C19 H19 0.9500 . ? C8 H8 0.9500 . ? C24 H24 0.9500 . ? C2 C3 1.384(13) . ? C2 H2 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C4 C3 1.366(13) . ? C4 H4 0.9500 . ? C3 H3 0.9500 . ? 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 P2 Au2 Br2 171.58(6) . . ? P2 Au2 Au1 100.99(5) . . ? Br2 Au2 Au1 82.97(2) . . ? P1 Au1 Br1 167.63(6) . . ? P1 Au1 Au2 95.58(5) . . ? Br1 Au1 Au2 95.64(2) . . ? C28 P2 C11 107.0(4) . . ? C28 P2 C34 104.7(4) . . ? C11 P2 C34 104.8(4) . . ? C28 P2 Au2 118.1(3) . . ? C11 P2 Au2 107.0(3) . . ? C34 P2 Au2 114.3(3) . . ? C16 P1 C1 103.4(4) . . ? C16 P1 C22 105.4(4) . . ? C1 P1 C22 102.2(4) . . ? C16 P1 Au1 105.7(3) . . ? C1 P1 Au1 121.1(3) . . ? C22 P1 Au1 117.2(3) . . ? C30 C29 C28 120.3(9) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C38 C39 C34 118.2(9) . . ? C38 C39 H39 120.9 . . ? C34 C39 H39 120.9 . . ? C33 C28 C29 118.2(8) . . ? C33 C28 P2 121.8(6) . . ? C29 C28 P2 119.6(7) . . ? C32 C33 C28 120.0(8) . . ? C32 C33 H33 120.0 . . ? C28 C33 H33 120.0 . . ? C35 C34 C39 119.5(8) . . ? C35 C34 P2 122.4(6) . . ? C39 C34 P2 118.1(7) . . ? C10 C11 C12 117.6(8) . . ? C10 C11 P2 121.7(7) . . ? C12 C11 P2 120.0(6) . . ? C36 C35 C34 120.6(8) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C12 O1 C13 117.1(6) . . ? C29 C30 C31 120.1(8) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C8 C7 C12 117.9(8) . . ? C8 C7 C6 122.9(8) . . ? C12 C7 C6 119.2(7) . . ? C32 C31 C30 120.1(8) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? O1 C13 C5 121.4(8) . . ? O1 C13 C1 116.8(7) . . ? C5 C13 C1 121.6(8) . . ? C37 C36 C35 120.3(10) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? O1 C12 C7 122.3(8) . . ? O1 C12 C11 116.3(7) . . ? C7 C12 C11 121.4(7) . . ? C36 C37 C38 120.2(9) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C31 C32 C33 121.2(9) . . ? C31 C32 H32 119.4 . . ? C33 C32 H32 119.4 . . ? C17 C16 C21 118.5(8) . . ? C17 C16 P1 122.9(7) . . ? C21 C16 P1 118.7(7) . . ? C20 C21 C16 121.4(9) . . ? C20 C21 H21 119.3 . . ? C16 C21 H21 119.3 . . ? C15 C6 C5 112.1(8) . . ? C15 C6 C7 111.1(7) . . ? C5 C6 C7 109.2(8) . . ? C15 C6 C14 110.7(8) . . ? C5 C6 C14 106.9(7) . . ? C7 C6 C14 106.6(8) . . ? C23 C22 C27 120.0(8) . . ? C23 C22 P1 119.3(7) . . ? C27 C22 P1 120.7(7) . . ? C39 C38 C37 121.2(9) . . ? C39 C38 H38 119.4 . . ? C37 C38 H38 119.4 . . ? C24 C23 C22 119.9(9) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C8 C9 C10 119.5(8) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C13 C1 C2 117.9(8) . . ? C13 C1 P1 121.8(7) . . ? C2 C1 P1 119.8(6) . . ? C9 C10 C11 120.9(8) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C26 C27 C22 119.8(9) . . ? C26 C27 H27 120.1 . . ? C22 C27 H27 120.1 . . ? C4 C5 C13 118.0(9) . . ? C4 C5 C6 122.4(8) . . ? C13 C5 C6 119.1(8) . . ? C18 C17 C16 120.2(9) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 120.7(9) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C27 C26 C25 121.0(9) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C19 C20 C21 119.0(9) . . ? C19 C20 H20 120.5 . . ? C21 C20 H20 120.5 . . ? C26 C25 C24 118.9(9) . . ? C26 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? C20 C19 C18 120.2(8) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C9 C8 C7 122.2(9) . . ? C9 C8 H8 118.9 . . ? C7 C8 H8 118.9 . . ? C23 C24 C25 120.4(9) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C3 C2 C1 120.2(9) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C6 C15 H15A 109.5 . . ? C6 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C6 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C6 C14 H14A 109.5 . . ? C6 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C6 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C3 C4 C5 121.3(9) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C4 C3 C2 120.1(9) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 26.91 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.359 _refine_diff_density_min -3.129 _refine_diff_density_rms 0.363 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.500 0.500 180.1 76.2 2 0.500 1.000 1.000 180.1 76.6 #===END data_08mz222_0m _database_code_depnum_ccdc_archive 'CCDC 750035' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H32 Au2 I2 O3 P2' _chemical_formula_weight 1258.32 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' P P 0.1023 0.0942 '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 10.604(4) _cell_length_b 18.383(7) _cell_length_c 19.367(7) _cell_angle_alpha 90.00 _cell_angle_beta 95.031(8) _cell_angle_gamma 90.00 _cell_volume 3761(3) _cell_formula_units_Z 4 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 5432 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 30.63 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 9.556 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2980 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_process_details 'Apex2 v2008.2-4 (Bruker, 2008)' _exptl_special_details ; Global SIMU and DELU restraints were applied with esds of 0.02 and 0.004. ; _diffrn_ambient_temperature 140(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 31171 _diffrn_reflns_av_R_equivalents 0.2373 _diffrn_reflns_av_sigmaI/netI 0.2596 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 28.28 _reflns_number_total 9251 _reflns_number_gt 4305 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2008.2-4 (Bruker, 2008)' _computing_cell_refinement 'Apex2 v2008.2-4 ' _computing_data_reduction 'Apex2 v2008.2-4 ' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.1302P)^2^+868.7471P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0049(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9251 _refine_ls_number_parameters 436 _refine_ls_number_restraints 386 _refine_ls_R_factor_all 0.2674 _refine_ls_R_factor_gt 0.1546 _refine_ls_wR_factor_ref 0.4358 _refine_ls_wR_factor_gt 0.3748 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.85140(15) 0.73741(8) 0.20185(10) 0.0337(5) Uani 1 1 d U . . Au2 Au 1.12109(14) 0.71544(8) 0.23003(9) 0.0297(5) Uani 1 1 d U . . C1 C 0.657(4) 0.639(2) 0.279(2) 0.033(5) Uani 1 1 d U . . C2 C 0.564(4) 0.591(3) 0.279(2) 0.037(6) Uani 1 1 d U . . H2 H 0.5744 0.5472 0.2544 0.045 Uiso 1 1 calc R . . C3 C 0.452(4) 0.597(3) 0.312(2) 0.045(7) Uani 1 1 d U . . H3 H 0.3901 0.5598 0.3121 0.054 Uiso 1 1 calc R . . C4 C 0.439(4) 0.665(3) 0.344(3) 0.047(7) Uani 1 1 d U . . H4 H 0.3623 0.6771 0.3623 0.056 Uiso 1 1 calc R . . C5 C 0.540(4) 0.713(3) 0.348(3) 0.044(6) Uani 1 1 d U . . H5 H 0.5339 0.7551 0.3770 0.053 Uiso 1 1 calc R . . C6 C 0.645(4) 0.706(3) 0.316(2) 0.036(6) Uani 1 1 d U . . H6 H 0.7076 0.7429 0.3166 0.043 Uiso 1 1 calc R . . C7 C 0.756(4) 0.561(2) 0.166(2) 0.037(5) Uani 1 1 d U . . C8 C 0.757(4) 0.488(2) 0.179(2) 0.035(6) Uani 1 1 d U . . H8 H 0.7855 0.4692 0.2239 0.043 Uiso 1 1 calc R . . C9 C 0.715(4) 0.440(3) 0.125(3) 0.042(6) Uani 1 1 d U . . H9 H 0.7156 0.3894 0.1332 0.051 Uiso 1 1 calc R . . C10 C 0.673(5) 0.465(3) 0.062(3) 0.045(7) Uani 1 1 d U . . H10 H 0.6431 0.4317 0.0267 0.054 Uiso 1 1 calc R . . C11 C 0.675(5) 0.539(3) 0.049(3) 0.046(6) Uani 1 1 d U . . H11 H 0.6480 0.5570 0.0041 0.055 Uiso 1 1 calc R . . C12 C 0.716(4) 0.586(3) 0.100(2) 0.042(6) Uani 1 1 d U . . H12 H 0.7160 0.6372 0.0912 0.050 Uiso 1 1 calc R . . C13 C 1.005(4) 0.534(2) 0.275(2) 0.032(5) Uani 1 1 d U . . C14 C 0.897(4) 0.573(2) 0.299(2) 0.032(4) Uani 1 1 d U . . C15 C 0.867(4) 0.562(2) 0.359(2) 0.034(5) Uani 1 1 d U . . H15 H 0.7978 0.5890 0.3741 0.040 Uiso 1 1 calc R . . C16 C 0.924(4) 0.514(2) 0.404(3) 0.038(5) Uani 1 1 d U . . H16 H 0.8973 0.5075 0.4495 0.045 Uiso 1 1 calc R . . C17 C 1.027(4) 0.474(2) 0.382(3) 0.038(6) Uani 1 1 d U . . H17 H 1.0710 0.4408 0.4129 0.046 Uiso 1 1 calc R . . C18 C 1.064(4) 0.483(2) 0.315(2) 0.031(4) Uani 1 1 d U . . C19 C 1.146(3) 0.430(2) 0.284(2) 0.030(4) Uani 1 1 d U . . C20 C 1.220(3) 0.4705(19) 0.229(2) 0.027(4) Uani 1 1 d U . . C21 C 1.328(3) 0.444(2) 0.209(2) 0.030(5) Uani 1 1 d U . . H21 H 1.3647 0.4014 0.2290 0.036 Uiso 1 1 calc R . . C22 C 1.384(3) 0.482(2) 0.158(2) 0.030(5) Uani 1 1 d U . . H22 H 1.4571 0.4627 0.1398 0.035 Uiso 1 1 calc R . . C23 C 1.334(3) 0.547(2) 0.133(2) 0.028(5) Uani 1 1 d U . . H23 H 1.3775 0.5744 0.1009 0.033 Uiso 1 1 calc R . . C24 C 1.221(3) 0.572(2) 0.154(2) 0.028(4) Uani 1 1 d U . . C25 C 1.162(4) 0.532(2) 0.199(2) 0.029(4) Uani 1 1 d U . . C26 C 1.061(3) 0.370(2) 0.245(3) 0.038(8) Uani 1 1 d U . . H26A H 0.9927 0.3930 0.2158 0.057 Uiso 1 1 calc R . . H26B H 1.0256 0.3381 0.2789 0.057 Uiso 1 1 calc R . . H26C H 1.1133 0.3407 0.2158 0.057 Uiso 1 1 calc R . . C27 C 1.247(4) 0.393(3) 0.338(3) 0.040(8) Uani 1 1 d U . . H27A H 1.2999 0.4312 0.3612 0.060 Uiso 1 1 calc R . . H27B H 1.3009 0.3602 0.3134 0.060 Uiso 1 1 calc R . . H27C H 1.2040 0.3658 0.3720 0.060 Uiso 1 1 calc R . . C28 C 1.302(4) 0.705(2) 0.095(3) 0.036(5) Uani 1 1 d U . . C29 C 1.405(4) 0.717(2) 0.137(3) 0.040(6) Uani 1 1 d U . . H29 H 1.4083 0.7017 0.1841 0.048 Uiso 1 1 calc R . . C30 C 1.518(4) 0.753(2) 0.110(3) 0.039(6) Uani 1 1 d U . . H30 H 1.5968 0.7589 0.1368 0.047 Uiso 1 1 calc R . . C31 C 1.495(5) 0.777(2) 0.045(3) 0.045(7) Uani 1 1 d U . . H31 H 1.5628 0.8020 0.0259 0.054 Uiso 1 1 calc R . . C32 C 1.384(5) 0.769(2) 0.001(3) 0.046(6) Uani 1 1 d U . . H32 H 1.3771 0.7882 -0.0445 0.055 Uiso 1 1 calc R . . C33 C 1.281(5) 0.733(2) 0.028(3) 0.046(6) Uani 1 1 d U . . H33 H 1.2022 0.7271 0.0012 0.055 Uiso 1 1 calc R . . C34 C 1.050(4) 0.656(2) 0.060(2) 0.033(5) Uani 1 1 d U . . C35 C 1.042(4) 0.596(2) 0.015(2) 0.033(6) Uani 1 1 d U . . H35 H 1.0958 0.5550 0.0233 0.040 Uiso 1 1 calc R . . C36 C 0.956(5) 0.597(2) -0.041(3) 0.040(6) Uani 1 1 d U . . H36 H 0.9556 0.5571 -0.0730 0.048 Uiso 1 1 calc R . . C37 C 0.869(4) 0.651(2) -0.055(2) 0.039(6) Uani 1 1 d U . . H37 H 0.8058 0.6481 -0.0926 0.047 Uiso 1 1 calc R . . C38 C 0.877(4) 0.712(2) -0.010(2) 0.037(6) Uani 1 1 d U . . H38 H 0.8249 0.7525 -0.0212 0.044 Uiso 1 1 calc R . . C39 C 0.955(4) 0.713(2) 0.046(2) 0.036(6) Uani 1 1 d U . . H39 H 0.9496 0.7522 0.0779 0.043 Uiso 1 1 calc R . . I1 I 0.8540(3) 0.87071(15) 0.1671(2) 0.0486(9) Uani 1 1 d U . . I2 I 1.0814(3) 0.75442(17) 0.35224(17) 0.0429(8) Uani 1 1 d U . . O1 O 1.045(2) 0.5548(13) 0.2145(15) 0.028(4) Uani 1 1 d U . . O2 O 0.311(6) 0.559(3) 0.469(2) 0.12(2) Uani 1 1 d . . . O3 O 0.428(8) 0.445(6) 0.512(2) 0.25(7) Uani 1 1 d . . . P1 P 0.7967(9) 0.6259(5) 0.2348(6) 0.030(2) Uani 1 1 d U . . P2 P 1.1681(9) 0.6629(5) 0.1316(6) 0.0293(17) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.0272(8) 0.0160(7) 0.0586(12) 0.0013(7) 0.0083(7) 0.0012(6) Au2 0.0227(7) 0.0163(7) 0.0511(10) -0.0020(7) 0.0085(6) -0.0014(5) C1 0.028(7) 0.041(11) 0.029(13) 0.007(9) 0.008(8) 0.006(6) C2 0.031(10) 0.051(14) 0.032(15) 0.003(12) 0.019(11) 0.000(9) C3 0.033(11) 0.065(15) 0.041(16) 0.003(13) 0.021(11) 0.006(11) C4 0.035(12) 0.064(16) 0.045(16) 0.005(13) 0.022(12) 0.014(11) C5 0.034(13) 0.056(15) 0.045(15) 0.003(12) 0.012(11) 0.018(10) C6 0.032(12) 0.044(13) 0.033(15) 0.005(10) 0.009(10) 0.011(9) C7 0.040(14) 0.024(7) 0.049(9) -0.004(7) 0.020(9) -0.008(10) C8 0.040(15) 0.023(7) 0.046(12) -0.008(8) 0.023(12) -0.009(11) C9 0.049(16) 0.031(9) 0.050(14) -0.013(9) 0.020(13) -0.009(12) C10 0.053(16) 0.040(11) 0.046(12) -0.016(11) 0.024(13) -0.002(13) C11 0.051(16) 0.042(12) 0.047(11) -0.009(10) 0.022(12) 0.000(13) C12 0.048(16) 0.032(11) 0.048(9) -0.004(9) 0.024(12) -0.001(12) C13 0.025(9) 0.020(10) 0.053(10) 0.005(8) 0.014(7) 0.005(7) C14 0.027(10) 0.018(9) 0.053(8) 0.003(7) 0.016(6) 0.002(7) C15 0.032(12) 0.022(12) 0.049(9) -0.003(10) 0.014(9) 0.001(9) C16 0.034(13) 0.030(14) 0.051(11) 0.003(10) 0.012(10) -0.001(10) C17 0.032(13) 0.031(13) 0.053(11) 0.007(10) 0.008(10) 0.003(9) C18 0.023(10) 0.015(10) 0.056(11) 0.006(7) 0.011(8) -0.002(7) C19 0.018(9) 0.017(8) 0.056(12) 0.002(6) 0.003(7) -0.001(5) C20 0.017(9) 0.012(9) 0.052(11) -0.005(7) 0.005(7) 0.000(6) C21 0.010(10) 0.016(11) 0.063(14) -0.002(9) 0.002(9) -0.003(7) C22 0.019(11) 0.016(10) 0.054(15) -0.011(10) 0.009(9) -0.001(7) C23 0.022(11) 0.020(10) 0.043(14) -0.008(9) 0.010(9) 0.001(7) C24 0.019(9) 0.021(6) 0.046(11) -0.001(5) 0.008(7) 0.002(6) C25 0.020(9) 0.020(8) 0.049(12) 0.000(7) 0.011(7) 0.005(6) C26 0.013(14) 0.027(15) 0.08(2) -0.009(13) 0.008(12) -0.006(10) C27 0.022(15) 0.04(2) 0.059(18) 0.009(13) 0.003(11) 0.005(11) C28 0.028(8) 0.019(10) 0.062(11) -0.001(9) 0.018(7) 0.002(9) C29 0.026(9) 0.026(13) 0.070(14) -0.002(12) 0.019(9) -0.007(10) C30 0.034(10) 0.016(13) 0.072(16) 0.001(13) 0.025(11) -0.006(10) C31 0.046(12) 0.019(14) 0.072(16) 0.001(12) 0.023(11) -0.004(11) C32 0.057(14) 0.013(13) 0.071(15) 0.003(12) 0.017(10) -0.016(12) C33 0.049(12) 0.020(13) 0.069(13) 0.009(12) 0.015(10) -0.009(12) C34 0.030(8) 0.019(11) 0.051(8) -0.006(8) 0.002(8) 0.008(7) C35 0.037(13) 0.015(11) 0.047(12) -0.002(9) 0.007(9) -0.002(9) C36 0.049(15) 0.022(12) 0.050(13) -0.002(10) 0.001(10) -0.006(10) C37 0.039(14) 0.033(14) 0.045(14) 0.002(11) 0.003(11) -0.004(11) C38 0.034(13) 0.033(13) 0.043(14) 0.002(11) 0.002(9) 0.007(10) C39 0.037(12) 0.021(12) 0.048(13) 0.001(10) -0.002(9) 0.011(9) I1 0.0481(18) 0.0138(12) 0.085(3) 0.0011(14) 0.0113(16) 0.0009(11) I2 0.0449(16) 0.0328(16) 0.0523(17) -0.0071(13) 0.0112(13) -0.0073(12) O1 0.020(8) 0.012(9) 0.053(10) 0.002(8) 0.012(7) 0.004(6) O2 0.21(6) 0.08(3) 0.07(3) -0.02(2) 0.08(3) -0.10(4) O3 0.27(10) 0.45(16) 0.02(3) 0.06(5) 0.02(4) 0.26(11) P1 0.020(3) 0.015(3) 0.057(6) -0.001(3) 0.009(4) 0.000(3) P2 0.018(3) 0.019(4) 0.051(4) -0.001(4) 0.004(3) 0.000(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.238(10) . ? Au1 I1 2.542(3) . ? Au1 Au2 2.892(2) . ? Au2 P2 2.231(12) . ? Au2 I2 2.543(4) . ? C1 C2 1.33(6) . ? C1 C6 1.43(6) . ? C1 P1 1.79(4) . ? C2 C3 1.40(6) . ? C2 H2 0.9500 . ? C3 C4 1.39(7) . ? C3 H3 0.9500 . ? C4 C5 1.39(7) . ? C4 H4 0.9500 . ? C5 C6 1.33(6) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.38(7) . ? C7 C8 1.38(6) . ? C7 P1 1.81(5) . ? C8 C9 1.41(6) . ? C8 H8 0.9500 . ? C9 C10 1.33(7) . ? C9 H9 0.9500 . ? C10 C11 1.39(7) . ? C10 H10 0.9500 . ? C11 C12 1.36(7) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 O1 1.33(5) . ? C13 C18 1.35(6) . ? C13 C14 1.45(5) . ? C14 C15 1.26(6) . ? C14 P1 1.84(5) . ? C15 C16 1.35(6) . ? C15 H15 0.9500 . ? C16 C17 1.41(6) . ? C16 H16 0.9500 . ? C17 C18 1.40(6) . ? C17 H17 0.9500 . ? C18 C19 1.47(5) . ? C19 C26 1.57(5) . ? C19 C20 1.57(6) . ? C19 C27 1.58(6) . ? C20 C21 1.32(5) . ? C20 C25 1.39(5) . ? C21 C22 1.38(6) . ? C21 H21 0.9500 . ? C22 C23 1.37(5) . ? C22 H22 0.9500 . ? C23 C24 1.38(5) . ? C23 H23 0.9500 . ? C24 C25 1.32(5) . ? C24 P2 1.81(4) . ? C25 O1 1.38(4) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.32(7) . ? C28 C33 1.40(7) . ? C28 P2 1.81(4) . ? C29 C30 1.50(5) . ? C29 H29 0.9500 . ? C30 C31 1.34(7) . ? C30 H30 0.9500 . ? C31 C32 1.40(7) . ? C31 H31 0.9500 . ? C32 C33 1.41(6) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.41(6) . ? C34 C39 1.47(5) . ? C34 P2 1.79(4) . ? C35 C36 1.35(6) . ? C35 H35 0.9500 . ? C36 C37 1.37(6) . ? C36 H36 0.9500 . ? C37 C38 1.41(6) . ? C37 H37 0.9500 . ? C38 C39 1.30(6) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 I1 165.3(3) . . ? P1 Au1 Au2 95.5(3) . . ? I1 Au1 Au2 98.68(9) . . ? P2 Au2 I2 169.9(3) . . ? P2 Au2 Au1 101.0(3) . . ? I2 Au2 Au1 83.94(9) . . ? C2 C1 C6 118(4) . . ? C2 C1 P1 124(4) . . ? C6 C1 P1 118(3) . . ? C1 C2 C3 127(5) . . ? C1 C2 H2 116.3 . . ? C3 C2 H2 116.3 . . ? C4 C3 C2 113(5) . . ? C4 C3 H3 123.5 . . ? C2 C3 H3 123.5 . . ? C5 C4 C3 120(4) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C6 C5 C4 125(5) . . ? C6 C5 H5 117.7 . . ? C4 C5 H5 117.7 . . ? C5 C6 C1 116(5) . . ? C5 C6 H6 122.0 . . ? C1 C6 H6 122.0 . . ? C12 C7 C8 120(4) . . ? C12 C7 P1 119(3) . . ? C8 C7 P1 120(4) . . ? C7 C8 C9 118(5) . . ? C7 C8 H8 121.1 . . ? C9 C8 H8 121.1 . . ? C10 C9 C8 122(5) . . ? C10 C9 H9 118.9 . . ? C8 C9 H9 118.9 . . ? C9 C10 C11 119(5) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C12 C11 C10 120(5) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C7 121(5) . . ? C11 C12 H12 119.7 . . ? C7 C12 H12 119.7 . . ? O1 C13 C18 122(4) . . ? O1 C13 C14 118(4) . . ? C18 C13 C14 120(4) . . ? C15 C14 C13 120(4) . . ? C15 C14 P1 122(3) . . ? C13 C14 P1 118(3) . . ? C14 C15 C16 125(4) . . ? C14 C15 H15 117.7 . . ? C16 C15 H15 117.7 . . ? C15 C16 C17 117(4) . . ? C15 C16 H16 121.4 . . ? C17 C16 H16 121.4 . . ? C18 C17 C16 121(4) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C13 C18 C17 117(4) . . ? C13 C18 C19 120(4) . . ? C17 C18 C19 122(4) . . ? C18 C19 C26 109(3) . . ? C18 C19 C20 108(3) . . ? C26 C19 C20 108(4) . . ? C18 C19 C27 114(4) . . ? C26 C19 C27 110(3) . . ? C20 C19 C27 107(3) . . ? C21 C20 C25 122(4) . . ? C21 C20 C19 122(3) . . ? C25 C20 C19 116(3) . . ? C20 C21 C22 118(4) . . ? C20 C21 H21 121.1 . . ? C22 C21 H21 121.1 . . ? C23 C22 C21 121(3) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C24 120(4) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C25 C24 C23 119(4) . . ? C25 C24 P2 121(3) . . ? C23 C24 P2 119(3) . . ? C24 C25 O1 118(3) . . ? C24 C25 C20 120(3) . . ? O1 C25 C20 122(4) . . ? C19 C26 H26A 109.5 . . ? C19 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C19 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C19 C27 H27A 109.5 . . ? C19 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C19 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C33 124(4) . . ? C29 C28 P2 118(4) . . ? C33 C28 P2 117(3) . . ? C28 C29 C30 120(5) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C31 C30 C29 113(4) . . ? C31 C30 H30 123.5 . . ? C29 C30 H30 123.5 . . ? C30 C31 C32 127(4) . . ? C30 C31 H31 116.3 . . ? C32 C31 H31 116.3 . . ? C31 C32 C33 118(5) . . ? C31 C32 H32 121.1 . . ? C33 C32 H32 121.1 . . ? C28 C33 C32 117(5) . . ? C28 C33 H33 121.7 . . ? C32 C33 H33 121.7 . . ? C35 C34 C39 116(4) . . ? C35 C34 P2 123(3) . . ? C39 C34 P2 121(3) . . ? C36 C35 C34 119(4) . . ? C36 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? C35 C36 C37 124(4) . . ? C35 C36 H36 118.2 . . ? C37 C36 H36 118.2 . . ? C36 C37 C38 117(4) . . ? C36 C37 H37 121.4 . . ? C38 C37 H37 121.4 . . ? C39 C38 C37 122(4) . . ? C39 C38 H38 118.9 . . ? C37 C38 H38 118.9 . . ? C38 C39 C34 121(4) . . ? C38 C39 H39 119.7 . . ? C34 C39 H39 119.7 . . ? C13 O1 C25 118(3) . . ? C1 P1 C7 107(2) . . ? C1 P1 C14 102.0(19) . . ? C7 P1 C14 104(2) . . ? C1 P1 Au1 104.9(15) . . ? C7 P1 Au1 116.1(15) . . ? C14 P1 Au1 121.8(13) . . ? C34 P2 C28 104(2) . . ? C34 P2 C24 107.5(19) . . ? C28 P2 C24 104.6(18) . . ? C34 P2 Au2 120.0(14) . . ? C28 P2 Au2 112.9(15) . . ? C24 P2 Au2 106.5(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Au1 Au2 P2 84.9(4) . . . . ? I1 Au1 Au2 P2 -99.1(3) . . . . ? P1 Au1 Au2 I2 -86.2(3) . . . . ? I1 Au1 Au2 I2 89.82(13) . . . . ? C6 C1 C2 C3 0(7) . . . . ? P1 C1 C2 C3 -180(4) . . . . ? C1 C2 C3 C4 3(8) . . . . ? C2 C3 C4 C5 -8(7) . . . . ? C3 C4 C5 C6 10(8) . . . . ? C4 C5 C6 C1 -6(7) . . . . ? C2 C1 C6 C5 1(6) . . . . ? P1 C1 C6 C5 -179(3) . . . . ? C12 C7 C8 C9 -1(6) . . . . ? P1 C7 C8 C9 175(3) . . . . ? C7 C8 C9 C10 -1(7) . . . . ? C8 C9 C10 C11 2(7) . . . . ? C9 C10 C11 C12 -2(7) . . . . ? C10 C11 C12 C7 0(7) . . . . ? C8 C7 C12 C11 1(7) . . . . ? P1 C7 C12 C11 -175(4) . . . . ? O1 C13 C14 C15 -171(4) . . . . ? C18 C13 C14 C15 6(7) . . . . ? O1 C13 C14 P1 18(5) . . . . ? C18 C13 C14 P1 -165(3) . . . . ? C13 C14 C15 C16 -2(7) . . . . ? P1 C14 C15 C16 168(4) . . . . ? C14 C15 C16 C17 0(7) . . . . ? C15 C16 C17 C18 -2(7) . . . . ? O1 C13 C18 C17 170(4) . . . . ? C14 C13 C18 C17 -7(6) . . . . ? O1 C13 C18 C19 -21(6) . . . . ? C14 C13 C18 C19 162(4) . . . . ? C16 C17 C18 C13 5(6) . . . . ? C16 C17 C18 C19 -164(4) . . . . ? C13 C18 C19 C26 -79(5) . . . . ? C17 C18 C19 C26 90(5) . . . . ? C13 C18 C19 C20 39(5) . . . . ? C17 C18 C19 C20 -153(4) . . . . ? C13 C18 C19 C27 158(4) . . . . ? C17 C18 C19 C27 -34(5) . . . . ? C18 C19 C20 C21 158(4) . . . . ? C26 C19 C20 C21 -83(5) . . . . ? C27 C19 C20 C21 36(5) . . . . ? C18 C19 C20 C25 -27(5) . . . . ? C26 C19 C20 C25 91(4) . . . . ? C27 C19 C20 C25 -150(4) . . . . ? C25 C20 C21 C22 2(6) . . . . ? C19 C20 C21 C22 176(4) . . . . ? C20 C21 C22 C23 5(6) . . . . ? C21 C22 C23 C24 -6(6) . . . . ? C22 C23 C24 C25 0(6) . . . . ? C22 C23 C24 P2 171(3) . . . . ? C23 C24 C25 O1 -175(4) . . . . ? P2 C24 C25 O1 15(6) . . . . ? C23 C24 C25 C20 7(7) . . . . ? P2 C24 C25 C20 -163(3) . . . . ? C21 C20 C25 C24 -8(7) . . . . ? C19 C20 C25 C24 177(4) . . . . ? C21 C20 C25 O1 173(4) . . . . ? C19 C20 C25 O1 -1(6) . . . . ? C33 C28 C29 C30 -9(7) . . . . ? P2 C28 C29 C30 -178(3) . . . . ? C28 C29 C30 C31 6(6) . . . . ? C29 C30 C31 C32 -2(7) . . . . ? C30 C31 C32 C33 0(7) . . . . ? C29 C28 C33 C32 7(7) . . . . ? P2 C28 C33 C32 176(3) . . . . ? C31 C32 C33 C28 -2(6) . . . . ? C39 C34 C35 C36 6(6) . . . . ? P2 C34 C35 C36 -175(4) . . . . ? C34 C35 C36 C37 -5(7) . . . . ? C35 C36 C37 C38 5(7) . . . . ? C36 C37 C38 C39 -7(7) . . . . ? C37 C38 C39 C34 9(7) . . . . ? C35 C34 C39 C38 -8(7) . . . . ? P2 C34 C39 C38 173(4) . . . . ? C18 C13 O1 C25 -12(6) . . . . ? C14 C13 O1 C25 165(4) . . . . ? C24 C25 O1 C13 -156(4) . . . . ? C20 C25 O1 C13 23(6) . . . . ? C2 C1 P1 C7 24(4) . . . . ? C6 C1 P1 C7 -155(3) . . . . ? C2 C1 P1 C14 -84(4) . . . . ? C6 C1 P1 C14 96(4) . . . . ? C2 C1 P1 Au1 148(4) . . . . ? C6 C1 P1 Au1 -32(4) . . . . ? C12 C7 P1 C1 93(4) . . . . ? C8 C7 P1 C1 -82(4) . . . . ? C12 C7 P1 C14 -160(3) . . . . ? C8 C7 P1 C14 25(4) . . . . ? C12 C7 P1 Au1 -23(4) . . . . ? C8 C7 P1 Au1 161(3) . . . . ? C15 C14 P1 C1 -8(4) . . . . ? C13 C14 P1 C1 163(3) . . . . ? C15 C14 P1 C7 -118(4) . . . . ? C13 C14 P1 C7 52(4) . . . . ? C15 C14 P1 Au1 109(4) . . . . ? C13 C14 P1 Au1 -81(3) . . . . ? I1 Au1 P1 C1 -23(2) . . . . ? Au2 Au1 P1 C1 141.3(15) . . . . ? I1 Au1 P1 C7 95(2) . . . . ? Au2 Au1 P1 C7 -101.1(16) . . . . ? I1 Au1 P1 C14 -137.6(18) . . . . ? Au2 Au1 P1 C14 26.7(16) . . . . ? C35 C34 P2 C28 88(4) . . . . ? C39 C34 P2 C28 -93(4) . . . . ? C35 C34 P2 C24 -23(4) . . . . ? C39 C34 P2 C24 156(4) . . . . ? C35 C34 P2 Au2 -144(3) . . . . ? C39 C34 P2 Au2 34(4) . . . . ? C29 C28 P2 C34 -180(3) . . . . ? C33 C28 P2 C34 10(4) . . . . ? C29 C28 P2 C24 -67(4) . . . . ? C33 C28 P2 C24 123(3) . . . . ? C29 C28 P2 Au2 48(4) . . . . ? C33 C28 P2 Au2 -122(3) . . . . ? C25 C24 P2 C34 -88(4) . . . . ? C23 C24 P2 C34 101(4) . . . . ? C25 C24 P2 C28 161(4) . . . . ? C23 C24 P2 C28 -9(4) . . . . ? C25 C24 P2 Au2 41(4) . . . . ? C23 C24 P2 Au2 -129(3) . . . . ? I2 Au2 P2 C34 125(2) . . . . ? Au1 Au2 P2 C34 7.1(17) . . . . ? I2 Au2 P2 C28 -111(2) . . . . ? Au1 Au2 P2 C28 130.7(16) . . . . ? I2 Au2 P2 C24 3(2) . . . . ? Au1 Au2 P2 C24 -115.1(13) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 6.744 _refine_diff_density_min -4.857 _refine_diff_density_rms 0.671 #===END data_08mz057_0m _database_code_depnum_ccdc_archive 'CCDC 750036' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H48 Au2 Cl2 O P2' _chemical_formula_weight 963.47 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7849(8) _cell_length_b 13.2014(13) _cell_length_c 16.5664(17) _cell_angle_alpha 80.4660(10) _cell_angle_beta 82.6840(10) _cell_angle_gamma 83.3700(10) _cell_volume 1657.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8166 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 31.79 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.301 _exptl_crystal_size_mid 0.206 _exptl_crystal_size_min 0.186 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.930 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 9.121 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.076 _exptl_absorpt_correction_T_max 0.183 _exptl_absorpt_process_details 'Apex2 v2.1-4 (Bruker, 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 17058 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 28.28 _reflns_number_total 8175 _reflns_number_gt 7206 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2.1-4 (Bruker, 2007)' _computing_cell_refinement 'Apex2 v2.1-4' _computing_data_reduction 'Apex2 v2.1-4' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.0318P)^2^+0.6069P] 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 8175 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0290 _refine_ls_R_factor_gt 0.0230 _refine_ls_wR_factor_ref 0.0664 _refine_ls_wR_factor_gt 0.0531 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.166022(17) 0.772486(10) 0.184835(9) 0.01175(4) Uani 1 1 d . . . Au2 Au 0.637714(19) 0.257262(11) 0.156061(11) 0.02198(5) Uani 1 1 d . . . C1 C 0.0125(4) 0.9307(3) 0.3136(2) 0.0129(7) Uani 1 1 d . . . C2 C -0.0657(5) 1.0239(3) 0.3378(2) 0.0159(8) Uani 1 1 d . . . H2 H -0.0340 1.0859 0.3073 0.019 Uiso 1 1 calc R . . C3 C -0.1887(5) 1.0259(3) 0.4059(2) 0.0183(8) Uani 1 1 d . . . H3 H -0.2419 1.0886 0.4193 0.022 Uiso 1 1 calc R . . C4 C -0.2323(5) 0.9339(3) 0.4540(2) 0.0183(8) Uani 1 1 d . . . H4 H -0.3136 0.9356 0.5002 0.022 Uiso 1 1 calc R . . C5 C -0.1563(5) 0.8396(3) 0.4342(2) 0.0142(7) Uani 1 1 d . . . C6 C -0.0395(4) 0.8395(3) 0.3634(2) 0.0130(7) Uani 1 1 d . . . C7 C -0.1838(5) 0.7348(3) 0.4879(2) 0.0167(8) Uani 1 1 d . . . C8 C -0.3465(6) 0.7399(3) 0.5504(3) 0.0231(9) Uani 1 1 d . . . H8A H -0.4479 0.7590 0.5217 0.035 Uiso 1 1 calc R . . H8B H -0.3377 0.7904 0.5849 0.035 Uiso 1 1 calc R . . H8C H -0.3559 0.6736 0.5838 0.035 Uiso 1 1 calc R . . C9 C -0.0226(6) 0.7008(3) 0.5349(3) 0.0240(9) Uani 1 1 d . . . H9A H -0.0310 0.6321 0.5642 0.036 Uiso 1 1 calc R . . H9B H -0.0174 0.7472 0.5732 0.036 Uiso 1 1 calc R . . H9C H 0.0807 0.7018 0.4965 0.036 Uiso 1 1 calc R . . C10 C -0.1919(5) 0.6574(3) 0.4297(2) 0.0145(7) Uani 1 1 d . . . C11 C -0.2970(5) 0.5773(3) 0.4460(3) 0.0189(8) Uani 1 1 d . . . H11 H -0.3733 0.5702 0.4941 0.023 Uiso 1 1 calc R . . C12 C -0.2903(5) 0.5075(3) 0.3915(3) 0.0194(8) Uani 1 1 d . . . H12 H -0.3615 0.4538 0.4034 0.023 Uiso 1 1 calc R . . C13 C -0.1786(5) 0.5173(3) 0.3197(2) 0.0155(8) Uani 1 1 d . . . H13 H -0.1745 0.4695 0.2839 0.019 Uiso 1 1 calc R . . C14 C -0.0705(5) 0.5984(3) 0.2994(2) 0.0134(7) Uani 1 1 d . . . C15 C -0.0797(5) 0.6658(3) 0.3567(2) 0.0128(7) Uani 1 1 d . . . C16 C 0.1367(5) 1.0399(3) 0.1428(2) 0.0141(7) Uani 1 1 d . . . C17 C -0.0525(5) 1.0367(3) 0.1276(3) 0.0197(8) Uani 1 1 d . . . H17A H -0.1289 1.0574 0.1734 0.030 Uiso 1 1 calc R . . H17B H -0.0707 0.9678 0.1215 0.030 Uiso 1 1 calc R . . H17C H -0.0764 1.0830 0.0783 0.030 Uiso 1 1 calc R . . C18 C 0.1656(5) 1.1479(3) 0.1587(3) 0.0190(8) Uani 1 1 d . . . H18A H 0.1383 1.1981 0.1120 0.028 Uiso 1 1 calc R . . H18B H 0.2849 1.1491 0.1673 0.028 Uiso 1 1 calc R . . H18C H 0.0915 1.1639 0.2067 0.028 Uiso 1 1 calc R . . C19 C 0.2548(5) 1.0169(3) 0.0650(2) 0.0205(8) Uani 1 1 d . . . H19A H 0.2397 0.9492 0.0546 0.031 Uiso 1 1 calc R . . H19B H 0.3740 1.0200 0.0728 0.031 Uiso 1 1 calc R . . H19C H 0.2245 1.0671 0.0188 0.031 Uiso 1 1 calc R . . C20 C 0.3861(5) 0.9355(3) 0.2746(3) 0.0164(8) Uani 1 1 d . . . C21 C 0.4161(5) 0.8319(3) 0.3313(3) 0.0269(10) Uani 1 1 d . . . H21A H 0.4260 0.7764 0.2996 0.040 Uiso 1 1 calc R . . H21B H 0.3198 0.8242 0.3735 0.040 Uiso 1 1 calc R . . H21C H 0.5213 0.8302 0.3563 0.040 Uiso 1 1 calc R . . C22 C 0.5395(5) 0.9473(3) 0.2079(3) 0.0235(9) Uani 1 1 d . . . H22A H 0.6460 0.9371 0.2330 0.035 Uiso 1 1 calc R . . H22B H 0.5285 1.0153 0.1766 0.035 Uiso 1 1 calc R . . H22C H 0.5408 0.8970 0.1721 0.035 Uiso 1 1 calc R . . C23 C 0.3693(5) 1.0240(4) 0.3256(3) 0.0263(10) Uani 1 1 d . . . H23A H 0.4752 1.0234 0.3498 0.039 Uiso 1 1 calc R . . H23B H 0.2743 1.0152 0.3684 0.039 Uiso 1 1 calc R . . H23C H 0.3480 1.0887 0.2906 0.039 Uiso 1 1 calc R . . C24 C 0.2292(5) 0.5025(3) 0.1995(2) 0.0141(7) Uani 1 1 d . . . C25 C 0.1640(5) 0.3960(3) 0.2253(3) 0.0192(8) Uani 1 1 d . . . H25A H 0.0841 0.3860 0.1884 0.029 Uiso 1 1 calc R . . H25B H 0.1061 0.3910 0.2803 0.029 Uiso 1 1 calc R . . H25C H 0.2609 0.3440 0.2234 0.029 Uiso 1 1 calc R . . C26 C 0.3314(5) 0.5086(3) 0.1136(3) 0.0203(8) Uani 1 1 d . . . H26A H 0.4333 0.4602 0.1156 0.030 Uiso 1 1 calc R . . H26B H 0.3654 0.5771 0.0959 0.030 Uiso 1 1 calc R . . H26C H 0.2595 0.4923 0.0754 0.030 Uiso 1 1 calc R . . C27 C 0.3479(5) 0.5203(3) 0.2619(3) 0.0219(9) Uani 1 1 d . . . H27A H 0.2821 0.5200 0.3150 0.033 Uiso 1 1 calc R . . H27B H 0.3941 0.5858 0.2446 0.033 Uiso 1 1 calc R . . H27C H 0.4419 0.4664 0.2652 0.033 Uiso 1 1 calc R . . C28 C -0.1020(5) 0.6219(3) 0.1212(2) 0.0143(7) Uani 1 1 d . . . C29 C -0.2580(5) 0.6954(3) 0.1480(3) 0.0219(9) Uani 1 1 d . . . H29A H -0.3322 0.7130 0.1047 0.033 Uiso 1 1 calc R . . H29B H -0.2176 0.7569 0.1595 0.033 Uiso 1 1 calc R . . H29C H -0.3221 0.6622 0.1967 0.033 Uiso 1 1 calc R . . C30 C -0.1627(6) 0.5196(3) 0.1092(3) 0.0217(9) Uani 1 1 d . . . H30A H -0.2167 0.4866 0.1607 0.033 Uiso 1 1 calc R . . H30B H -0.0644 0.4754 0.0902 0.033 Uiso 1 1 calc R . . H30C H -0.2450 0.5326 0.0694 0.033 Uiso 1 1 calc R . . C31 C -0.0164(5) 0.6729(3) 0.0375(2) 0.0202(8) Uani 1 1 d . . . H31A H 0.0895 0.6323 0.0220 0.030 Uiso 1 1 calc R . . H31B H 0.0091 0.7410 0.0419 0.030 Uiso 1 1 calc R . . H31C H -0.0945 0.6770 -0.0036 0.030 Uiso 1 1 calc R . . Cl1 Cl 0.70525(14) 0.27614(8) 0.28183(7) 0.0288(2) Uani 1 1 d . . . Cl2 Cl 0.57123(14) 0.23708(9) 0.03079(8) 0.0317(2) Uani 1 1 d . . . O1 O 0.0308(3) 0.74486(19) 0.34159(15) 0.0122(5) Uani 1 1 d . . . P1 P 0.18422(12) 0.92905(7) 0.22593(6) 0.01103(18) Uani 1 1 d . . . P2 P 0.05798(12) 0.61434(7) 0.19765(6) 0.01088(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01339(7) 0.00876(7) 0.01289(7) -0.00241(5) 0.00131(5) -0.00219(5) Au2 0.01608(8) 0.01205(8) 0.03522(11) -0.00093(7) 0.00318(7) -0.00102(6) C1 0.0107(16) 0.0184(19) 0.0102(17) -0.0021(14) -0.0014(13) -0.0036(14) C2 0.0172(18) 0.0130(18) 0.0165(19) -0.0005(15) -0.0005(15) -0.0013(14) C3 0.0211(19) 0.0167(19) 0.017(2) -0.0060(16) -0.0022(16) 0.0016(15) C4 0.0186(19) 0.022(2) 0.0138(19) -0.0068(16) 0.0025(15) 0.0006(15) C5 0.0147(17) 0.0168(19) 0.0119(18) -0.0036(15) -0.0019(14) -0.0031(14) C6 0.0114(16) 0.0139(18) 0.0147(18) -0.0044(15) -0.0038(14) 0.0007(13) C7 0.0197(19) 0.020(2) 0.0107(18) -0.0044(15) 0.0009(15) -0.0008(15) C8 0.030(2) 0.021(2) 0.017(2) -0.0039(17) 0.0049(17) -0.0053(17) C9 0.032(2) 0.024(2) 0.016(2) 0.0014(17) -0.0088(18) -0.0034(18) C10 0.0151(17) 0.0135(18) 0.0130(18) 0.0014(14) 0.0003(14) 0.0003(14) C11 0.0193(19) 0.019(2) 0.0154(19) 0.0018(16) 0.0042(15) -0.0041(15) C12 0.0193(19) 0.018(2) 0.020(2) -0.0004(16) 0.0011(16) -0.0069(15) C13 0.0174(18) 0.0145(18) 0.0146(19) -0.0035(15) 0.0016(15) -0.0031(14) C14 0.0132(16) 0.0123(18) 0.0137(18) 0.0012(14) -0.0014(14) -0.0012(13) C15 0.0127(16) 0.0124(17) 0.0137(18) -0.0009(14) -0.0028(14) -0.0019(13) C16 0.0185(18) 0.0118(18) 0.0114(18) 0.0005(14) -0.0010(14) -0.0032(14) C17 0.0205(19) 0.018(2) 0.021(2) 0.0013(16) -0.0105(16) -0.0007(15) C18 0.025(2) 0.0105(18) 0.021(2) -0.0020(15) 0.0009(16) -0.0041(15) C19 0.030(2) 0.019(2) 0.0129(19) -0.0034(16) 0.0027(16) -0.0064(17) C20 0.0129(17) 0.0155(19) 0.023(2) -0.0061(16) -0.0068(15) -0.0016(14) C21 0.019(2) 0.031(2) 0.030(2) 0.002(2) -0.0093(18) -0.0036(18) C22 0.0136(18) 0.024(2) 0.032(2) -0.0052(18) 0.0015(17) -0.0012(16) C23 0.020(2) 0.034(3) 0.030(2) -0.013(2) -0.0071(18) -0.0048(18) C24 0.0134(17) 0.0108(17) 0.0177(19) -0.0021(14) -0.0021(14) 0.0015(13) C25 0.0198(19) 0.0120(19) 0.026(2) -0.0030(16) -0.0023(16) -0.0005(15) C26 0.022(2) 0.0151(19) 0.020(2) -0.0008(16) 0.0050(16) 0.0035(15) C27 0.0177(19) 0.017(2) 0.031(2) -0.0013(17) -0.0099(17) 0.0034(15) C28 0.0173(18) 0.0123(18) 0.0122(18) 0.0006(14) -0.0023(14) 0.0002(14) C29 0.0168(19) 0.023(2) 0.026(2) -0.0028(18) -0.0059(17) 0.0030(16) C30 0.029(2) 0.019(2) 0.020(2) -0.0043(16) -0.0062(17) -0.0069(17) C31 0.027(2) 0.020(2) 0.0128(19) 0.0007(16) -0.0032(16) -0.0042(16) Cl1 0.0302(5) 0.0174(5) 0.0375(6) -0.0045(4) -0.0001(5) -0.0010(4) Cl2 0.0286(6) 0.0290(6) 0.0361(6) -0.0001(5) -0.0004(5) -0.0075(4) O1 0.0138(12) 0.0111(13) 0.0115(13) -0.0019(10) 0.0006(10) -0.0018(10) P1 0.0109(4) 0.0097(4) 0.0129(4) -0.0030(4) -0.0003(3) -0.0018(3) P2 0.0123(4) 0.0090(4) 0.0113(4) -0.0022(3) 0.0004(3) -0.0019(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.3051(10) . ? Au1 P2 2.3075(9) . ? Au2 Cl2 2.2659(13) . ? Au2 Cl1 2.2718(12) . ? C1 C2 1.405(5) . ? C1 C6 1.412(5) . ? C1 P1 1.846(4) . ? C2 C3 1.385(5) . ? C2 H2 0.9300 . ? C3 C4 1.390(6) . ? C3 H3 0.9300 . ? C4 C5 1.387(5) . ? C4 H4 0.9300 . ? C5 C6 1.389(5) . ? C5 C7 1.538(5) . ? C6 O1 1.391(4) . ? C7 C10 1.527(5) . ? C7 C8 1.534(5) . ? C7 C9 1.545(6) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.382(5) . ? C10 C15 1.395(5) . ? C11 C12 1.385(6) . ? C11 H11 0.9300 . ? C12 C13 1.379(5) . ? C12 H12 0.9300 . ? C13 C14 1.408(5) . ? C13 H13 0.9300 . ? C14 C15 1.395(5) . ? C14 P2 1.840(4) . ? C15 O1 1.399(4) . ? C16 C17 1.532(5) . ? C16 C19 1.537(5) . ? C16 C18 1.538(5) . ? C16 P1 1.875(4) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C22 1.523(5) . ? C20 C23 1.536(6) . ? C20 C21 1.539(6) . ? C20 P1 1.872(4) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.525(5) . ? C24 C26 1.534(5) . ? C24 C27 1.534(5) . ? C24 P2 1.871(4) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.532(5) . ? C28 C30 1.532(5) . ? C28 C31 1.542(5) . ? C28 P2 1.870(4) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 P2 153.41(3) . . ? Cl2 Au2 Cl1 179.54(4) . . ? C2 C1 C6 116.1(3) . . ? C2 C1 P1 121.4(3) . . ? C6 C1 P1 122.4(3) . . ? C3 C2 C1 121.8(4) . . ? C3 C2 H2 119.1 . . ? C1 C2 H2 119.1 . . ? C2 C3 C4 119.8(4) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 120.9(4) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C4 C5 C6 118.2(4) . . ? C4 C5 C7 124.5(3) . . ? C6 C5 C7 117.2(3) . . ? C5 C6 O1 118.1(3) . . ? C5 C6 C1 123.1(3) . . ? O1 C6 C1 118.8(3) . . ? C10 C7 C8 112.1(3) . . ? C10 C7 C5 107.2(3) . . ? C8 C7 C5 112.5(3) . . ? C10 C7 C9 108.2(3) . . ? C8 C7 C9 108.8(3) . . ? C5 C7 C9 107.9(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 117.9(4) . . ? C11 C10 C7 124.6(3) . . ? C15 C10 C7 117.5(3) . . ? C10 C11 C12 120.9(4) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C13 C12 C11 120.3(4) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 121.3(4) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C15 C14 C13 116.4(3) . . ? C15 C14 P2 124.7(3) . . ? C13 C14 P2 118.7(3) . . ? C10 C15 C14 123.3(3) . . ? C10 C15 O1 117.8(3) . . ? C14 C15 O1 118.9(3) . . ? C17 C16 C19 108.2(3) . . ? C17 C16 C18 110.4(3) . . ? C19 C16 C18 108.4(3) . . ? C17 C16 P1 106.2(3) . . ? C19 C16 P1 106.4(3) . . ? C18 C16 P1 116.9(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C22 C20 C23 109.9(3) . . ? C22 C20 C21 109.2(3) . . ? C23 C20 C21 109.3(4) . . ? C22 C20 P1 109.4(3) . . ? C23 C20 P1 112.7(3) . . ? C21 C20 P1 106.2(3) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C26 109.7(3) . . ? C25 C24 C27 109.0(3) . . ? C26 C24 C27 109.7(3) . . ? C25 C24 P2 115.8(3) . . ? C26 C24 P2 108.0(3) . . ? C27 C24 P2 104.6(3) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C30 110.3(3) . . ? C29 C28 C31 107.6(3) . . ? C30 C28 C31 108.2(3) . . ? C29 C28 P2 106.7(3) . . ? C30 C28 P2 116.5(3) . . ? C31 C28 P2 107.2(3) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C6 O1 C15 116.5(3) . . ? C1 P1 C20 102.71(17) . . ? C1 P1 C16 110.08(17) . . ? C20 P1 C16 114.27(17) . . ? C1 P1 Au1 102.72(12) . . ? C20 P1 Au1 114.09(13) . . ? C16 P1 Au1 111.84(12) . . ? C14 P2 C28 105.61(17) . . ? C14 P2 C24 106.28(17) . . ? C28 P2 C24 115.89(17) . . ? C14 P2 Au1 105.05(12) . . ? C28 P2 Au1 108.98(12) . . ? C24 P2 Au1 114.07(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.0(5) . . . . ? P1 C1 C2 C3 -176.9(3) . . . . ? C1 C2 C3 C4 2.6(6) . . . . ? C2 C3 C4 C5 -1.0(6) . . . . ? C3 C4 C5 C6 -2.0(6) . . . . ? C3 C4 C5 C7 174.2(4) . . . . ? C4 C5 C6 O1 -177.2(3) . . . . ? C7 C5 C6 O1 6.3(5) . . . . ? C4 C5 C6 C1 3.7(6) . . . . ? C7 C5 C6 C1 -172.8(3) . . . . ? C2 C1 C6 C5 -2.2(5) . . . . ? P1 C1 C6 C5 173.7(3) . . . . ? C2 C1 C6 O1 178.7(3) . . . . ? P1 C1 C6 O1 -5.4(5) . . . . ? C4 C5 C7 C10 142.3(4) . . . . ? C6 C5 C7 C10 -41.4(4) . . . . ? C4 C5 C7 C8 18.7(5) . . . . ? C6 C5 C7 C8 -165.0(3) . . . . ? C4 C5 C7 C9 -101.4(4) . . . . ? C6 C5 C7 C9 74.9(4) . . . . ? C8 C7 C10 C11 -20.7(5) . . . . ? C5 C7 C10 C11 -144.5(4) . . . . ? C9 C7 C10 C11 99.3(4) . . . . ? C8 C7 C10 C15 162.2(3) . . . . ? C5 C7 C10 C15 38.4(4) . . . . ? C9 C7 C10 C15 -77.8(4) . . . . ? C15 C10 C11 C12 0.2(6) . . . . ? C7 C10 C11 C12 -176.9(4) . . . . ? C10 C11 C12 C13 -0.3(6) . . . . ? C11 C12 C13 C14 -0.7(6) . . . . ? C12 C13 C14 C15 1.7(6) . . . . ? C12 C13 C14 P2 -173.7(3) . . . . ? C11 C10 C15 C14 0.9(6) . . . . ? C7 C10 C15 C14 178.2(3) . . . . ? C11 C10 C15 O1 -177.9(3) . . . . ? C7 C10 C15 O1 -0.6(5) . . . . ? C13 C14 C15 C10 -1.8(5) . . . . ? P2 C14 C15 C10 173.2(3) . . . . ? C13 C14 C15 O1 177.0(3) . . . . ? P2 C14 C15 O1 -8.0(5) . . . . ? C5 C6 O1 C15 36.5(5) . . . . ? C1 C6 O1 C15 -144.4(3) . . . . ? C10 C15 O1 C6 -39.6(4) . . . . ? C14 C15 O1 C6 141.5(3) . . . . ? C2 C1 P1 C20 85.4(3) . . . . ? C6 C1 P1 C20 -90.3(3) . . . . ? C2 C1 P1 C16 -36.7(4) . . . . ? C6 C1 P1 C16 147.6(3) . . . . ? C2 C1 P1 Au1 -156.0(3) . . . . ? C6 C1 P1 Au1 28.4(3) . . . . ? C22 C20 P1 C1 -173.5(3) . . . . ? C23 C20 P1 C1 -51.0(3) . . . . ? C21 C20 P1 C1 68.7(3) . . . . ? C22 C20 P1 C16 -54.3(3) . . . . ? C23 C20 P1 C16 68.2(3) . . . . ? C21 C20 P1 C16 -172.1(3) . . . . ? C22 C20 P1 Au1 76.1(3) . . . . ? C23 C20 P1 Au1 -161.4(3) . . . . ? C21 C20 P1 Au1 -41.7(3) . . . . ? C17 C16 P1 C1 -50.1(3) . . . . ? C19 C16 P1 C1 -165.3(2) . . . . ? C18 C16 P1 C1 73.5(3) . . . . ? C17 C16 P1 C20 -165.1(3) . . . . ? C19 C16 P1 C20 79.8(3) . . . . ? C18 C16 P1 C20 -41.5(3) . . . . ? C17 C16 P1 Au1 63.4(3) . . . . ? C19 C16 P1 Au1 -51.8(3) . . . . ? C18 C16 P1 Au1 -173.0(2) . . . . ? P2 Au1 P1 C1 -5.26(15) . . . . ? P2 Au1 P1 C20 105.11(16) . . . . ? P2 Au1 P1 C16 -123.27(14) . . . . ? C15 C14 P2 C28 -121.0(3) . . . . ? C13 C14 P2 C28 53.9(3) . . . . ? C15 C14 P2 C24 115.3(3) . . . . ? C13 C14 P2 C24 -69.7(3) . . . . ? C15 C14 P2 Au1 -5.9(3) . . . . ? C13 C14 P2 Au1 169.0(3) . . . . ? C29 C28 P2 C14 45.2(3) . . . . ? C30 C28 P2 C14 -78.5(3) . . . . ? C31 C28 P2 C14 160.2(3) . . . . ? C29 C28 P2 C24 162.5(3) . . . . ? C30 C28 P2 C24 38.8(3) . . . . ? C31 C28 P2 C24 -82.4(3) . . . . ? C29 C28 P2 Au1 -67.2(3) . . . . ? C30 C28 P2 Au1 169.1(3) . . . . ? C31 C28 P2 Au1 47.8(3) . . . . ? C25 C24 P2 C14 52.7(3) . . . . ? C26 C24 P2 C14 176.0(3) . . . . ? C27 C24 P2 C14 -67.3(3) . . . . ? C25 C24 P2 C28 -64.3(3) . . . . ? C26 C24 P2 C28 59.1(3) . . . . ? C27 C24 P2 C28 175.8(2) . . . . ? C25 C24 P2 Au1 167.9(2) . . . . ? C26 C24 P2 Au1 -68.7(3) . . . . ? C27 C24 P2 Au1 48.0(3) . . . . ? P1 Au1 P2 C14 -9.24(15) . . . . ? P1 Au1 P2 C28 103.54(14) . . . . ? P1 Au1 P2 C24 -125.21(15) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.102 _refine_diff_density_min -1.320 _refine_diff_density_rms 0.174 #===END data_ju020808_0m _database_code_depnum_ccdc_archive 'CCDC 750037' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H48 Au O P2, Au Br2' _chemical_formula_sum 'C31 H48 Au2 Br2 O P2' _chemical_formula_weight 1052.39 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' P P 0.1023 0.0942 '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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.8004(15) _cell_length_b 13.229(3) _cell_length_c 16.615(3) _cell_angle_alpha 80.764(2) _cell_angle_beta 83.754(2) _cell_angle_gamma 83.867(2) _cell_volume 1675.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9982 _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 26.98 _exptl_crystal_description Irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.086 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 11.250 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0727 _exptl_absorpt_correction_T_max 0.3708 _exptl_absorpt_process_details 'Axscale in APEX2 (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 18664 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0401 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 27.04 _reflns_number_total 7183 _reflns_number_gt 6652 _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^)+(0.1000P)^2^+0.3396P] 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 7183 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.1241 _refine_ls_wR_factor_gt 0.1201 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.33942(2) 0.229022(14) 0.313724(12) 0.01578(9) Uani 1 1 d . . . Au2 Au 0.13255(3) 0.254646(15) 0.656367(14) 0.02242(10) Uani 1 1 d . . . Br3 Br 0.19633(8) 0.26989(4) 0.79029(4) 0.02695(15) Uani 1 1 d . . . Br4 Br 0.07070(8) 0.23527(5) 0.52321(4) 0.03010(15) Uani 1 1 d . . . P1 P 0.44882(16) 0.38622(10) 0.30178(8) 0.0150(3) Uani 1 1 d . . . P2 P 0.31531(17) 0.07429(10) 0.27159(8) 0.0149(3) Uani 1 1 d . . . C20 C 0.6100(7) 0.3790(4) 0.3785(3) 0.0174(10) Uani 1 1 d . . . C12 C 0.4770(7) 0.0742(4) 0.1826(3) 0.0174(10) Uani 1 1 d . . . C8 C 0.6422(7) 0.1646(4) 0.0636(3) 0.0181(10) Uani 1 1 d . . . C2 C 0.5749(7) 0.4020(4) 0.2006(3) 0.0187(10) Uani 1 1 d . . . O1 O 0.4647(5) 0.2586(3) 0.1572(2) 0.0172(7) Uani 1 1 d . . . C16 C 0.2805(7) 0.4978(4) 0.2994(3) 0.0188(11) Uani 1 1 d . . . C3 C 0.6852(7) 0.4804(4) 0.1824(3) 0.0195(11) Uani 1 1 d . . . H3 H 0.6844 0.5284 0.2193 0.023 Uiso 1 1 calc R . . C1 C 0.5767(6) 0.3354(4) 0.1439(3) 0.0161(10) Uani 1 1 d . . . C11 C 0.5503(7) -0.0184(4) 0.1578(4) 0.0212(11) Uani 1 1 d . . . H11 H 0.5196 -0.0819 0.1887 0.025 Uiso 1 1 calc R . . C21 C 0.6732(8) 0.4807(5) 0.3902(4) 0.0261(12) Uani 1 1 d . . . H21A H 0.5743 0.5267 0.4079 0.039 Uiso 1 1 calc R . . H21B H 0.7300 0.5129 0.3383 0.039 Uiso 1 1 calc R . . H21C H 0.7558 0.4676 0.4319 0.039 Uiso 1 1 calc R . . C17 C 0.1579(8) 0.4787(5) 0.2375(4) 0.0267(13) Uani 1 1 d . . . H17A H 0.1135 0.4113 0.2548 0.040 Uiso 1 1 calc R . . H17B H 0.2216 0.4804 0.1831 0.040 Uiso 1 1 calc R . . H17C H 0.0609 0.5324 0.2352 0.040 Uiso 1 1 calc R . . C6 C 0.6853(7) 0.3438(4) 0.0712(3) 0.0181(10) Uani 1 1 d . . . C28 C 0.3679(7) -0.0359(4) 0.3517(3) 0.0204(11) Uani 1 1 d . . . C18 C 0.3479(7) 0.6035(4) 0.2718(4) 0.0231(12) Uani 1 1 d . . . H18A H 0.2499 0.6564 0.2678 0.035 Uiso 1 1 calc R . . H18B H 0.4144 0.6045 0.2181 0.035 Uiso 1 1 calc R . . H18C H 0.4227 0.6174 0.3117 0.035 Uiso 1 1 calc R . . C7 C 0.6702(7) 0.2692(4) 0.0119(3) 0.0210(11) Uani 1 1 d . . . C13 C 0.5290(6) 0.1648(4) 0.1347(3) 0.0168(10) Uani 1 1 d . . . C5 C 0.7966(7) 0.4210(4) 0.0564(4) 0.0231(12) Uani 1 1 d . . . H5 H 0.8744 0.4270 0.0081 0.028 Uiso 1 1 calc R . . C29 C 0.5599(7) -0.0343(4) 0.3645(4) 0.0231(12) Uani 1 1 d . . . H29A H 0.5810 0.0345 0.3735 0.035 Uiso 1 1 calc R . . H29B H 0.6323 -0.0521 0.3159 0.035 Uiso 1 1 calc R . . H29C H 0.5888 -0.0845 0.4124 0.035 Uiso 1 1 calc R . . C4 C 0.7954(7) 0.4893(4) 0.1113(4) 0.0217(11) Uani 1 1 d . . . H4 H 0.8709 0.5426 0.1000 0.026 Uiso 1 1 calc R . . C23 C 0.7621(7) 0.3066(5) 0.3500(4) 0.0256(12) Uani 1 1 d . . . H23A H 0.8298 0.3428 0.3031 0.038 Uiso 1 1 calc R . . H23B H 0.7184 0.2468 0.3338 0.038 Uiso 1 1 calc R . . H23C H 0.8359 0.2837 0.3948 0.038 Uiso 1 1 calc R . . C30 C 0.2627(8) -0.0151(5) 0.4313(4) 0.0266(13) Uani 1 1 d . . . H30A H 0.1389 -0.0130 0.4249 0.040 Uiso 1 1 calc R . . H30B H 0.2881 0.0511 0.4444 0.040 Uiso 1 1 calc R . . H30C H 0.2935 -0.0699 0.4758 0.040 Uiso 1 1 calc R . . C31 C 0.3359(8) -0.1437(4) 0.3355(4) 0.0260(12) Uani 1 1 d . . . H31A H 0.3663 -0.1951 0.3824 0.039 Uiso 1 1 calc R . . H31B H 0.4076 -0.1597 0.2861 0.039 Uiso 1 1 calc R . . H31C H 0.2134 -0.1450 0.3276 0.039 Uiso 1 1 calc R . . C19 C 0.1812(8) 0.4938(5) 0.3834(4) 0.0273(13) Uani 1 1 d . . . H19A H 0.2576 0.5069 0.4229 0.041 Uiso 1 1 calc R . . H19B H 0.1393 0.4257 0.4004 0.041 Uiso 1 1 calc R . . H19C H 0.0824 0.5463 0.3810 0.041 Uiso 1 1 calc R . . C10 C 0.6672(7) -0.0185(4) 0.0889(4) 0.0236(12) Uani 1 1 d . . . H10 H 0.7166 -0.0821 0.0733 0.028 Uiso 1 1 calc R . . C22 C 0.5271(8) 0.3268(5) 0.4617(3) 0.0243(12) Uani 1 1 d . . . H22A H 0.6123 0.3159 0.5021 0.036 Uiso 1 1 calc R . . H22B H 0.4900 0.2603 0.4551 0.036 Uiso 1 1 calc R . . H22C H 0.4267 0.3709 0.4804 0.036 Uiso 1 1 calc R . . C24 C 0.1084(7) 0.0694(4) 0.2262(4) 0.0220(12) Uani 1 1 d . . . C9 C 0.7129(7) 0.0720(5) 0.0426(4) 0.0228(11) Uani 1 1 d . . . H9 H 0.7940 0.0703 -0.0043 0.027 Uiso 1 1 calc R . . C26 C 0.1179(8) -0.0186(6) 0.1748(5) 0.0349(15) Uani 1 1 d . . . H26A H 0.1539 -0.0838 0.2083 0.052 Uiso 1 1 calc R . . H26B H 0.2022 -0.0055 0.1270 0.052 Uiso 1 1 calc R . . H26C H 0.0037 -0.0223 0.1566 0.052 Uiso 1 1 calc R . . C14 C 0.5077(8) 0.3059(5) -0.0342(4) 0.0285(13) Uani 1 1 d . . . H14A H 0.5192 0.3752 -0.0643 0.043 Uiso 1 1 calc R . . H14B H 0.4048 0.3070 0.0053 0.043 Uiso 1 1 calc R . . H14C H 0.4960 0.2587 -0.0727 0.043 Uiso 1 1 calc R . . C15 C 0.8274(8) 0.2635(5) -0.0501(4) 0.0281(13) Uani 1 1 d . . . H15A H 0.9298 0.2357 -0.0217 0.042 Uiso 1 1 calc R . . H15B H 0.8451 0.3326 -0.0794 0.042 Uiso 1 1 calc R . . H15C H 0.8088 0.2186 -0.0893 0.042 Uiso 1 1 calc R . . C25 C -0.0382(7) 0.0569(5) 0.2936(4) 0.0299(14) Uani 1 1 d . . . H25A H -0.0321 0.1055 0.3316 0.045 Uiso 1 1 calc R . . H25B H -0.0280 -0.0135 0.3231 0.045 Uiso 1 1 calc R . . H25C H -0.1492 0.0705 0.2696 0.045 Uiso 1 1 calc R . . C27 C 0.0757(8) 0.1725(5) 0.1711(4) 0.0289(13) Uani 1 1 d . . . H27A H -0.0352 0.1751 0.1479 0.043 Uiso 1 1 calc R . . H27B H 0.1691 0.1800 0.1266 0.043 Uiso 1 1 calc R . . H27C H 0.0724 0.2286 0.2034 0.043 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01472(13) 0.01197(13) 0.02017(14) -0.00160(9) 0.00103(9) -0.00293(8) Au2 0.01678(14) 0.01540(14) 0.03345(16) 0.00013(10) -0.00030(10) -0.00188(9) Br3 0.0271(3) 0.0185(3) 0.0349(3) -0.0039(2) -0.0018(2) -0.0018(2) Br4 0.0272(3) 0.0289(3) 0.0330(3) 0.0023(3) -0.0039(2) -0.0066(2) P1 0.0137(6) 0.0124(6) 0.0186(6) -0.0013(5) -0.0005(5) -0.0024(5) P2 0.0134(6) 0.0116(6) 0.0195(6) -0.0025(5) 0.0006(5) -0.0030(5) C20 0.019(3) 0.011(2) 0.022(3) -0.0011(19) -0.003(2) -0.0005(19) C12 0.015(2) 0.018(3) 0.020(3) -0.002(2) 0.0016(19) -0.0042(19) C8 0.018(3) 0.018(3) 0.018(3) 0.001(2) -0.005(2) -0.004(2) C2 0.014(2) 0.018(3) 0.024(3) -0.004(2) -0.002(2) -0.001(2) O1 0.0142(17) 0.0154(17) 0.0213(19) 0.0000(14) -0.0008(14) -0.0039(14) C16 0.017(2) 0.016(2) 0.023(3) 0.001(2) 0.000(2) -0.004(2) C3 0.020(3) 0.015(2) 0.023(3) 0.000(2) 0.001(2) -0.002(2) C1 0.014(2) 0.011(2) 0.021(3) 0.0028(19) -0.003(2) -0.0017(18) C11 0.021(3) 0.016(3) 0.026(3) -0.002(2) -0.001(2) -0.004(2) C21 0.034(3) 0.027(3) 0.019(3) -0.001(2) -0.004(2) -0.011(3) C17 0.023(3) 0.023(3) 0.033(3) 0.003(2) -0.008(2) -0.001(2) C6 0.016(2) 0.024(3) 0.011(2) 0.007(2) -0.0017(19) 0.000(2) C28 0.022(3) 0.020(3) 0.020(3) -0.001(2) 0.001(2) -0.005(2) C18 0.023(3) 0.013(2) 0.032(3) -0.001(2) -0.003(2) 0.000(2) C7 0.022(3) 0.018(3) 0.021(3) 0.001(2) 0.001(2) 0.001(2) C13 0.013(2) 0.014(2) 0.023(3) -0.002(2) -0.003(2) -0.0004(18) C5 0.019(3) 0.024(3) 0.024(3) 0.001(2) 0.003(2) -0.004(2) C29 0.022(3) 0.019(3) 0.027(3) 0.000(2) -0.008(2) 0.002(2) C4 0.020(3) 0.019(3) 0.027(3) -0.001(2) 0.001(2) -0.008(2) C23 0.021(3) 0.030(3) 0.025(3) -0.004(2) -0.001(2) 0.002(2) C30 0.030(3) 0.019(3) 0.030(3) -0.002(2) 0.006(2) -0.005(2) C31 0.035(3) 0.017(3) 0.023(3) 0.001(2) 0.009(2) -0.008(2) C19 0.031(3) 0.019(3) 0.027(3) -0.003(2) 0.009(2) 0.004(2) C10 0.021(3) 0.020(3) 0.031(3) -0.010(2) -0.003(2) 0.000(2) C22 0.032(3) 0.026(3) 0.015(3) 0.001(2) -0.003(2) -0.008(2) C24 0.017(3) 0.020(3) 0.032(3) -0.010(2) -0.006(2) -0.002(2) C9 0.018(3) 0.028(3) 0.021(3) -0.004(2) 0.002(2) 0.000(2) C26 0.026(3) 0.041(4) 0.043(4) -0.019(3) -0.006(3) -0.006(3) C14 0.027(3) 0.032(3) 0.027(3) 0.002(2) -0.007(2) -0.006(2) C15 0.033(3) 0.025(3) 0.027(3) -0.007(2) 0.007(3) -0.011(2) C25 0.013(3) 0.030(3) 0.045(4) -0.001(3) 0.003(2) -0.006(2) C27 0.022(3) 0.033(3) 0.034(3) -0.002(3) -0.014(2) -0.006(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 Au1 P2 2.2993(13) . ? Au1 P1 2.3027(13) . ? Au2 Br4 2.3736(8) . ? Au2 Br3 2.3761(8) . ? P1 C2 1.847(6) . ? P1 C16 1.866(6) . ? P1 C20 1.870(5) . ? P2 C12 1.836(5) . ? P2 C28 1.852(6) . ? P2 C24 1.866(6) . ? C20 C23 1.527(7) . ? C20 C21 1.529(7) . ? C20 C22 1.550(7) . ? C12 C11 1.399(8) . ? C12 C13 1.401(7) . ? C8 C9 1.371(8) . ? C8 C13 1.396(8) . ? C8 C7 1.530(7) . ? C2 C1 1.387(8) . ? C2 C3 1.394(7) . ? O1 C13 1.382(6) . ? O1 C1 1.384(6) . ? C16 C19 1.516(8) . ? C16 C18 1.530(7) . ? C16 C17 1.545(8) . ? C3 C4 1.380(8) . ? C3 H3 0.9500 . ? C1 C6 1.394(7) . ? C11 C10 1.385(8) . ? C11 H11 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C6 C5 1.386(8) . ? C6 C7 1.524(8) . ? C28 C30 1.528(8) . ? C28 C29 1.539(8) . ? C28 C31 1.544(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C7 C15 1.517(8) . ? C7 C14 1.545(8) . ? C5 C4 1.382(8) . ? C5 H5 0.9500 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C4 H4 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C10 C9 1.374(8) . ? C10 H10 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C24 C25 1.514(8) . ? C24 C27 1.530(8) . ? C24 C26 1.541(8) . ? C9 H9 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? 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 P2 Au1 P1 153.46(5) . . ? Br4 Au2 Br3 178.68(2) . . ? C2 P1 C16 106.1(2) . . ? C2 P1 C20 105.7(2) . . ? C16 P1 C20 115.7(2) . . ? C2 P1 Au1 104.97(18) . . ? C16 P1 Au1 114.25(17) . . ? C20 P1 Au1 109.15(17) . . ? C12 P2 C28 110.3(2) . . ? C12 P2 C24 102.7(3) . . ? C28 P2 C24 114.4(3) . . ? C12 P2 Au1 102.95(17) . . ? C28 P2 Au1 111.82(18) . . ? C24 P2 Au1 113.52(18) . . ? C23 C20 C21 110.3(5) . . ? C23 C20 C22 107.9(4) . . ? C21 C20 C22 109.0(5) . . ? C23 C20 P1 105.2(4) . . ? C21 C20 P1 116.7(4) . . ? C22 C20 P1 107.4(4) . . ? C11 C12 C13 116.6(5) . . ? C11 C12 P2 120.6(4) . . ? C13 C12 P2 122.7(4) . . ? C9 C8 C13 118.5(5) . . ? C9 C8 C7 124.6(5) . . ? C13 C8 C7 116.8(5) . . ? C1 C2 C3 117.8(5) . . ? C1 C2 P1 123.8(4) . . ? C3 C2 P1 118.3(4) . . ? C13 O1 C1 116.9(4) . . ? C19 C16 C18 110.3(5) . . ? C19 C16 C17 109.0(5) . . ? C18 C16 C17 108.8(5) . . ? C19 C16 P1 108.6(4) . . ? C18 C16 P1 115.4(4) . . ? C17 C16 P1 104.4(4) . . ? C4 C3 C2 120.8(5) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? O1 C1 C2 120.2(5) . . ? O1 C1 C6 117.4(5) . . ? C2 C1 C6 122.4(5) . . ? C10 C11 C12 120.6(5) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C5 C6 C1 118.1(5) . . ? C5 C6 C7 124.1(5) . . ? C1 C6 C7 117.7(5) . . ? C30 C28 C29 107.0(5) . . ? C30 C28 C31 108.6(5) . . ? C29 C28 C31 109.4(5) . . ? C30 C28 P2 107.5(4) . . ? C29 C28 P2 106.7(4) . . ? C31 C28 P2 117.2(4) . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C15 C7 C6 112.2(5) . . ? C15 C7 C8 112.0(5) . . ? C6 C7 C8 106.9(4) . . ? C15 C7 C14 109.0(5) . . ? C6 C7 C14 108.4(5) . . ? C8 C7 C14 108.2(5) . . ? O1 C13 C8 118.0(5) . . ? O1 C13 C12 119.4(5) . . ? C8 C13 C12 122.6(5) . . ? C4 C5 C6 120.6(5) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C3 C4 C5 120.3(5) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C9 C10 C11 121.1(5) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C25 C24 C27 109.4(5) . . ? C25 C24 C26 109.5(5) . . ? C27 C24 C26 109.4(5) . . ? C25 C24 P2 109.7(4) . . ? C27 C24 P2 106.4(4) . . ? C26 C24 P2 112.3(4) . . ? C8 C9 C10 120.4(5) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C7 C14 H14A 109.5 . . ? C7 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C7 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C7 C15 H15A 109.5 . . ? C7 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C7 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.263 _refine_diff_density_min -3.331 _refine_diff_density_rms 0.244 #===END data_08mz219_0m _database_code_depnum_ccdc_archive 'CCDC 750038' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H48 Au2 I2 O P2' _chemical_formula_weight 1146.37 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' P P 0.1023 0.0942 '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 7.9986(4) _cell_length_b 13.4430(7) _cell_length_c 16.9930(9) _cell_angle_alpha 80.9230(10) _cell_angle_beta 83.9480(10) _cell_angle_gamma 84.2300(10) _cell_volume 1787.68(16) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8687 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.130 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 10.035 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5717 _exptl_absorpt_correction_T_max 0.7463 _exptl_absorpt_process_details 'Apex2 v2008.2-4 (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 18279 _diffrn_reflns_av_R_equivalents 0.0188 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 28.28 _reflns_number_total 8765 _reflns_number_gt 7864 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2008.2-4 (Bruker, 2008)' _computing_cell_refinement 'Apex2 v2008.2-4 ' _computing_data_reduction 'Apex2 v2008.2-4 ' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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 8765 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0264 _refine_ls_R_factor_gt 0.0213 _refine_ls_wR_factor_ref 0.0615 _refine_ls_wR_factor_gt 0.0507 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.135 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.872423(19) 0.752028(11) 0.341178(10) 0.02792(5) Uani 1 1 d . . . Au2 Au 0.655184(17) 0.766015(10) 0.688718(9) 0.01956(4) Uani 1 1 d . . . I1 I 0.93230(4) 0.76850(2) 0.481889(18) 0.03715(7) Uani 1 1 d . . . I2 I 0.80998(4) 0.74303(2) 0.199295(18) 0.03228(7) Uani 1 1 d . . . P1 P 0.54618(11) 0.61108(7) 0.69927(5) 0.01670(18) Uani 1 1 d . . . P2 P 0.68467(12) 0.91670(7) 0.73285(6) 0.02057(19) Uani 1 1 d . . . C8 C 0.3760(5) 0.8223(3) 0.9391(2) 0.0227(8) Uani 1 1 d . . . C1 C 0.4251(4) 0.6583(3) 0.8562(2) 0.0183(7) Uani 1 1 d . . . O1 O 0.5392(3) 0.73264(18) 0.84308(15) 0.0191(5) Uani 1 1 d . . . C13 C 0.4821(4) 0.8251(3) 0.8679(2) 0.0186(7) Uani 1 1 d . . . C2 C 0.4233(4) 0.5954(3) 0.7976(2) 0.0185(7) Uani 1 1 d . . . C16 C 0.7094(5) 0.5007(3) 0.7022(2) 0.0225(8) Uani 1 1 d . . . C3 C 0.3102(5) 0.5200(3) 0.8155(2) 0.0237(8) Uani 1 1 d . . . H3 H 0.3081 0.4744 0.7799 0.028 Uiso 1 1 calc R . . C7 C 0.3427(5) 0.7191(3) 0.9871(2) 0.0264(8) Uani 1 1 d . . . C12 C 0.5345(5) 0.9142(3) 0.8230(2) 0.0221(8) Uani 1 1 d . . . C6 C 0.3204(5) 0.6495(3) 0.9272(2) 0.0207(7) Uani 1 1 d . . . C11 C 0.4704(5) 1.0041(3) 0.8518(2) 0.0284(9) Uani 1 1 d . . . H11 H 0.5030 1.0655 0.8241 0.034 Uiso 1 1 calc R . . C4 C 0.2017(5) 0.5116(3) 0.8847(2) 0.0274(8) Uani 1 1 d . . . H4 H 0.1251 0.4624 0.8940 0.033 Uiso 1 1 calc R . . C5 C 0.2067(5) 0.5758(3) 0.9397(2) 0.0262(8) Uani 1 1 d . . . H5 H 0.1330 0.5697 0.9860 0.031 Uiso 1 1 calc R . . C18 C 0.6408(5) 0.3973(3) 0.7311(3) 0.0293(9) Uani 1 1 d . . . H18A H 0.5602 0.3859 0.6962 0.044 Uiso 1 1 calc R . . H18B H 0.5872 0.3960 0.7845 0.044 Uiso 1 1 calc R . . H18C H 0.7322 0.3452 0.7308 0.044 Uiso 1 1 calc R . . C20 C 0.3890(5) 0.6188(3) 0.6238(2) 0.0245(8) Uani 1 1 d . . . C9 C 0.3135(5) 0.9142(3) 0.9636(2) 0.0288(9) Uani 1 1 d . . . H9 H 0.2395 0.9150 1.0095 0.035 Uiso 1 1 calc R . . C28 C 0.6240(5) 1.0287(3) 0.6571(2) 0.0265(8) Uani 1 1 d . . . C29 C 0.4330(5) 1.0263(3) 0.6514(3) 0.0322(9) Uani 1 1 d . . . H29A H 0.3718 1.0418 0.7003 0.048 Uiso 1 1 calc R . . H29B H 0.4105 0.9602 0.6428 0.048 Uiso 1 1 calc R . . H29C H 0.3981 1.0755 0.6076 0.048 Uiso 1 1 calc R . . C19 C 0.8313(5) 0.5198(3) 0.7609(3) 0.0351(10) Uani 1 1 d . . . H19A H 0.9224 0.4674 0.7633 0.053 Uiso 1 1 calc R . . H19B H 0.7723 0.5198 0.8131 0.053 Uiso 1 1 calc R . . H19C H 0.8757 0.5841 0.7431 0.053 Uiso 1 1 calc R . . C24 C 0.8921(5) 0.9207(3) 0.7731(3) 0.0344(10) Uani 1 1 d . . . C17 C 0.8030(6) 0.5017(3) 0.6189(3) 0.0367(11) Uani 1 1 d . . . H17A H 0.8404 0.5677 0.6000 0.055 Uiso 1 1 calc R . . H17B H 0.7286 0.4856 0.5828 0.055 Uiso 1 1 calc R . . H17C H 0.8988 0.4526 0.6215 0.055 Uiso 1 1 calc R . . C21 C 0.3288(6) 0.5188(3) 0.6100(3) 0.0351(10) Uani 1 1 d . . . H21A H 0.2491 0.5320 0.5704 0.053 Uiso 1 1 calc R . . H21B H 0.2760 0.4857 0.6592 0.053 Uiso 1 1 calc R . . H21C H 0.4237 0.4760 0.5918 0.053 Uiso 1 1 calc R . . C10 C 0.3608(6) 1.0040(3) 0.9199(2) 0.0316(9) Uani 1 1 d . . . H10 H 0.3183 1.0650 0.9365 0.038 Uiso 1 1 calc R . . C15 C 0.1923(6) 0.7250(3) 1.0493(3) 0.0384(11) Uani 1 1 d . . . H15A H 0.0930 0.7512 1.0231 0.058 Uiso 1 1 calc R . . H15B H 0.2126 0.7689 1.0861 0.058 Uiso 1 1 calc R . . H15C H 0.1763 0.6587 1.0779 0.058 Uiso 1 1 calc R . . C14 C 0.5016(6) 0.6774(3) 1.0295(2) 0.0348(10) Uani 1 1 d . . . H14A H 0.4838 0.6123 1.0601 0.052 Uiso 1 1 calc R . . H14B H 0.5240 0.7229 1.0647 0.052 Uiso 1 1 calc R . . H14C H 0.5962 0.6710 0.9903 0.052 Uiso 1 1 calc R . . C22 C 0.4684(5) 0.6714(3) 0.5435(2) 0.0318(9) Uani 1 1 d . . . H22A H 0.5637 0.6294 0.5247 0.048 Uiso 1 1 calc R . . H22B H 0.5044 0.7351 0.5507 0.048 Uiso 1 1 calc R . . H22C H 0.3864 0.6826 0.5049 0.048 Uiso 1 1 calc R . . C23 C 0.2385(5) 0.6893(4) 0.6521(3) 0.0350(10) Uani 1 1 d . . . H23A H 0.2791 0.7491 0.6650 0.052 Uiso 1 1 calc R . . H23B H 0.1783 0.6550 0.6988 0.052 Uiso 1 1 calc R . . H23C H 0.1644 0.7078 0.6103 0.052 Uiso 1 1 calc R . . C31 C 0.6597(6) 1.1329(3) 0.6730(3) 0.0388(11) Uani 1 1 d . . . H31A H 0.7786 1.1346 0.6756 0.058 Uiso 1 1 calc R . . H31B H 0.6003 1.1462 0.7229 0.058 Uiso 1 1 calc R . . H31C H 0.6224 1.1835 0.6306 0.058 Uiso 1 1 calc R . . C30 C 0.7151(6) 1.0099(3) 0.5761(3) 0.0394(11) Uani 1 1 d . . . H30A H 0.6751 1.0612 0.5347 0.059 Uiso 1 1 calc R . . H30B H 0.6928 0.9447 0.5655 0.059 Uiso 1 1 calc R . . H30C H 0.8343 1.0121 0.5774 0.059 Uiso 1 1 calc R . . C25 C 0.9301(6) 0.8177(4) 0.8230(3) 0.0438(12) Uani 1 1 d . . . H25A H 1.0380 0.8153 0.8435 0.066 Uiso 1 1 calc R . . H25B H 0.9318 0.7656 0.7901 0.066 Uiso 1 1 calc R . . H25C H 0.8444 0.8072 0.8667 0.066 Uiso 1 1 calc R . . C27 C 1.0289(5) 0.9350(4) 0.7022(4) 0.0511(14) Uani 1 1 d . . . H27A H 1.1385 0.9206 0.7217 0.077 Uiso 1 1 calc R . . H27B H 1.0176 1.0035 0.6756 0.077 Uiso 1 1 calc R . . H27C H 1.0157 0.8898 0.6653 0.077 Uiso 1 1 calc R . . C26 C 0.8913(6) 1.0034(4) 0.8260(4) 0.0543(15) Uani 1 1 d . . . H26A H 0.8094 0.9913 0.8713 0.081 Uiso 1 1 calc R . . H26B H 0.8628 1.0682 0.7956 0.081 Uiso 1 1 calc R . . H26C H 1.0010 1.0023 0.8443 0.081 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.02443(8) 0.02163(8) 0.03678(10) -0.00253(6) -0.00233(7) -0.00082(6) Au2 0.02023(7) 0.01492(7) 0.02334(8) -0.00481(5) 0.00272(5) -0.00243(5) I1 0.03483(15) 0.03954(16) 0.03533(16) 0.00284(12) -0.00644(12) -0.00463(12) I2 0.03368(14) 0.02521(13) 0.03869(16) -0.00924(11) -0.00099(12) -0.00148(11) P1 0.0187(4) 0.0147(4) 0.0168(4) -0.0039(3) 0.0003(3) -0.0016(3) P2 0.0171(4) 0.0162(4) 0.0287(5) -0.0065(4) 0.0026(4) -0.0029(3) C8 0.0264(19) 0.028(2) 0.0150(17) -0.0058(15) -0.0039(14) -0.0018(15) C1 0.0159(16) 0.0201(17) 0.0179(17) -0.0008(14) 0.0001(13) -0.0011(13) O1 0.0183(12) 0.0175(12) 0.0225(13) -0.0068(10) -0.0007(10) -0.0014(10) C13 0.0190(17) 0.0192(17) 0.0189(17) -0.0060(14) -0.0043(14) -0.0007(13) C2 0.0194(17) 0.0187(17) 0.0171(17) -0.0032(13) -0.0021(13) 0.0004(13) C16 0.0216(18) 0.0152(17) 0.028(2) 0.0003(15) 0.0001(15) 0.0016(14) C3 0.0260(19) 0.0245(19) 0.0217(19) -0.0046(15) -0.0021(15) -0.0054(15) C7 0.037(2) 0.029(2) 0.0127(17) -0.0054(15) 0.0000(15) 0.0005(17) C12 0.0210(18) 0.0220(18) 0.0246(19) -0.0079(15) -0.0034(15) 0.0005(14) C6 0.0248(18) 0.0200(18) 0.0161(17) -0.0002(14) -0.0024(14) 0.0009(14) C11 0.035(2) 0.0200(19) 0.030(2) -0.0059(16) 0.0028(17) -0.0009(16) C4 0.025(2) 0.029(2) 0.028(2) -0.0025(16) 0.0032(16) -0.0092(16) C5 0.027(2) 0.029(2) 0.0197(19) 0.0003(16) 0.0073(15) -0.0048(16) C18 0.034(2) 0.0161(18) 0.036(2) -0.0019(16) 0.0000(18) 0.0001(16) C20 0.0241(19) 0.027(2) 0.0233(19) -0.0070(16) -0.0038(15) -0.0017(15) C9 0.039(2) 0.029(2) 0.0183(19) -0.0078(16) 0.0005(17) 0.0000(17) C28 0.028(2) 0.0160(18) 0.033(2) -0.0002(16) 0.0058(17) -0.0006(15) C29 0.032(2) 0.030(2) 0.032(2) -0.0001(18) -0.0035(18) 0.0036(17) C19 0.026(2) 0.030(2) 0.050(3) -0.006(2) -0.013(2) 0.0040(17) C24 0.023(2) 0.029(2) 0.054(3) -0.015(2) -0.0057(19) -0.0002(17) C17 0.040(3) 0.027(2) 0.037(2) -0.0036(18) 0.015(2) 0.0069(18) C21 0.042(3) 0.041(3) 0.026(2) -0.0086(19) -0.0065(19) -0.013(2) C10 0.043(3) 0.024(2) 0.027(2) -0.0109(17) 0.0028(18) 0.0039(18) C15 0.053(3) 0.038(3) 0.023(2) -0.0057(18) 0.011(2) -0.010(2) C14 0.045(3) 0.038(2) 0.022(2) 0.0006(18) -0.0121(18) 0.000(2) C22 0.037(2) 0.035(2) 0.022(2) -0.0004(17) -0.0030(17) -0.0034(18) C23 0.031(2) 0.045(3) 0.027(2) -0.0037(19) -0.0083(18) 0.0103(19) C31 0.042(3) 0.021(2) 0.051(3) -0.0045(19) 0.010(2) -0.0074(18) C30 0.050(3) 0.026(2) 0.039(3) -0.0037(19) 0.015(2) -0.006(2) C25 0.029(2) 0.040(3) 0.065(3) -0.010(2) -0.020(2) 0.002(2) C27 0.020(2) 0.038(3) 0.094(4) -0.013(3) 0.011(2) -0.0053(19) C26 0.035(3) 0.052(3) 0.088(4) -0.037(3) -0.021(3) -0.003(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 Au1 I1 2.5349(4) . ? Au1 I2 2.5367(3) . ? Au2 P2 2.3096(9) . ? Au2 P1 2.3118(9) . ? P1 C2 1.840(4) . ? P1 C20 1.873(4) . ? P1 C16 1.873(4) . ? P2 C12 1.842(4) . ? P2 C24 1.869(4) . ? P2 C28 1.879(4) . ? C8 C9 1.394(5) . ? C8 C13 1.400(5) . ? C8 C7 1.527(5) . ? C1 C6 1.390(5) . ? C1 O1 1.397(4) . ? C1 C2 1.407(5) . ? O1 C13 1.393(4) . ? C13 C12 1.392(5) . ? C2 C3 1.402(5) . ? C16 C17 1.529(6) . ? C16 C19 1.533(6) . ? C16 C18 1.535(5) . ? C3 C4 1.382(5) . ? C3 H3 0.9300 . ? C7 C15 1.519(6) . ? C7 C6 1.522(5) . ? C7 C14 1.540(6) . ? C12 C11 1.406(5) . ? C6 C5 1.389(5) . ? C11 C10 1.375(6) . ? C11 H11 0.9300 . ? C4 C5 1.375(6) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C20 C21 1.532(6) . ? C20 C23 1.540(6) . ? C20 C22 1.540(5) . ? C9 C10 1.379(6) . ? C9 H9 0.9300 . ? C28 C31 1.528(6) . ? C28 C30 1.533(6) . ? C28 C29 1.544(6) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C24 C25 1.526(6) . ? C24 C26 1.535(6) . ? C24 C27 1.541(7) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C10 H10 0.9300 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I1 Au1 I2 177.744(11) . . ? P2 Au2 P1 153.32(3) . . ? C2 P1 C20 105.66(17) . . ? C2 P1 C16 105.75(16) . . ? C20 P1 C16 116.04(18) . . ? C2 P1 Au2 104.89(12) . . ? C20 P1 Au2 109.19(13) . . ? C16 P1 Au2 114.26(12) . . ? C12 P2 C24 102.90(19) . . ? C12 P2 C28 109.64(17) . . ? C24 P2 C28 114.6(2) . . ? C12 P2 Au2 103.31(12) . . ? C24 P2 Au2 113.57(14) . . ? C28 P2 Au2 111.69(14) . . ? C9 C8 C13 117.8(4) . . ? C9 C8 C7 124.0(3) . . ? C13 C8 C7 118.1(3) . . ? C6 C1 O1 118.1(3) . . ? C6 C1 C2 123.4(3) . . ? O1 C1 C2 118.5(3) . . ? C13 O1 C1 116.7(3) . . ? C12 C13 O1 119.6(3) . . ? C12 C13 C8 123.4(3) . . ? O1 C13 C8 117.0(3) . . ? C3 C2 C1 115.8(3) . . ? C3 C2 P1 119.3(3) . . ? C1 C2 P1 124.8(3) . . ? C17 C16 C19 109.4(4) . . ? C17 C16 C18 109.9(3) . . ? C19 C16 C18 108.8(3) . . ? C17 C16 P1 108.7(3) . . ? C19 C16 P1 105.0(3) . . ? C18 C16 P1 114.9(3) . . ? C4 C3 C2 121.9(4) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C15 C7 C6 112.4(4) . . ? C15 C7 C8 112.4(3) . . ? C6 C7 C8 107.0(3) . . ? C15 C7 C14 109.2(3) . . ? C6 C7 C14 107.7(3) . . ? C8 C7 C14 107.9(3) . . ? C13 C12 C11 116.0(3) . . ? C13 C12 P2 123.1(3) . . ? C11 C12 P2 120.8(3) . . ? C5 C6 C1 117.8(3) . . ? C5 C6 C7 124.5(3) . . ? C1 C6 C7 117.6(3) . . ? C10 C11 C12 121.9(4) . . ? C10 C11 H11 119.1 . . ? C12 C11 H11 119.1 . . ? C5 C4 C3 120.1(4) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 121.0(4) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C21 C20 C23 110.4(3) . . ? C21 C20 C22 108.3(3) . . ? C23 C20 C22 107.7(3) . . ? C21 C20 P1 116.8(3) . . ? C23 C20 P1 105.6(3) . . ? C22 C20 P1 107.6(3) . . ? C10 C9 C8 120.3(4) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C31 C28 C30 108.9(3) . . ? C31 C28 C29 109.6(3) . . ? C30 C28 C29 107.4(4) . . ? C31 C28 P2 117.5(3) . . ? C30 C28 P2 107.3(3) . . ? C29 C28 P2 105.7(3) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C25 C24 C26 109.0(4) . . ? C25 C24 C27 108.7(4) . . ? C26 C24 C27 110.7(4) . . ? C25 C24 P2 106.4(3) . . ? C26 C24 P2 113.3(3) . . ? C27 C24 P2 108.6(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C11 C10 C9 120.6(4) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C7 C15 H15A 109.5 . . ? C7 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C7 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C7 C14 H14A 109.5 . . ? C7 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C7 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Au2 P1 C2 -5.07(15) . . . . ? P2 Au2 P1 C20 107.78(15) . . . . ? P2 Au2 P1 C16 -120.41(15) . . . . ? P1 Au2 P2 C12 -4.39(15) . . . . ? P1 Au2 P2 C24 106.32(18) . . . . ? P1 Au2 P2 C28 -122.15(14) . . . . ? C6 C1 O1 C13 -38.8(4) . . . . ? C2 C1 O1 C13 142.0(3) . . . . ? C1 O1 C13 C12 -144.2(3) . . . . ? C1 O1 C13 C8 37.2(4) . . . . ? C9 C8 C13 C12 3.4(5) . . . . ? C7 C8 C13 C12 -173.7(3) . . . . ? C9 C8 C13 O1 -178.0(3) . . . . ? C7 C8 C13 O1 4.8(5) . . . . ? C6 C1 C2 C3 -1.3(5) . . . . ? O1 C1 C2 C3 177.9(3) . . . . ? C6 C1 C2 P1 174.5(3) . . . . ? O1 C1 C2 P1 -6.3(5) . . . . ? C20 P1 C2 C3 50.6(3) . . . . ? C16 P1 C2 C3 -73.0(3) . . . . ? Au2 P1 C2 C3 165.9(3) . . . . ? C20 P1 C2 C1 -125.1(3) . . . . ? C16 P1 C2 C1 111.4(3) . . . . ? Au2 P1 C2 C1 -9.7(3) . . . . ? C2 P1 C16 C17 173.3(3) . . . . ? C20 P1 C16 C17 56.5(3) . . . . ? Au2 P1 C16 C17 -71.9(3) . . . . ? C2 P1 C16 C19 -69.7(3) . . . . ? C20 P1 C16 C19 173.5(3) . . . . ? Au2 P1 C16 C19 45.1(3) . . . . ? C2 P1 C16 C18 49.7(3) . . . . ? C20 P1 C16 C18 -67.0(3) . . . . ? Au2 P1 C16 C18 164.5(2) . . . . ? C1 C2 C3 C4 3.1(5) . . . . ? P1 C2 C3 C4 -173.0(3) . . . . ? C9 C8 C7 C15 18.5(5) . . . . ? C13 C8 C7 C15 -164.5(4) . . . . ? C9 C8 C7 C6 142.4(4) . . . . ? C13 C8 C7 C6 -40.7(5) . . . . ? C9 C8 C7 C14 -102.0(4) . . . . ? C13 C8 C7 C14 75.0(4) . . . . ? O1 C13 C12 C11 179.6(3) . . . . ? C8 C13 C12 C11 -1.9(5) . . . . ? O1 C13 C12 P2 -2.5(5) . . . . ? C8 C13 C12 P2 176.0(3) . . . . ? C24 P2 C12 C13 -93.9(3) . . . . ? C28 P2 C12 C13 143.7(3) . . . . ? Au2 P2 C12 C13 24.6(3) . . . . ? C24 P2 C12 C11 83.9(3) . . . . ? C28 P2 C12 C11 -38.5(4) . . . . ? Au2 P2 C12 C11 -157.6(3) . . . . ? O1 C1 C6 C5 179.7(3) . . . . ? C2 C1 C6 C5 -1.1(5) . . . . ? O1 C1 C6 C7 -2.4(5) . . . . ? C2 C1 C6 C7 176.8(3) . . . . ? C15 C7 C6 C5 -19.1(5) . . . . ? C8 C7 C6 C5 -143.0(4) . . . . ? C14 C7 C6 C5 101.2(4) . . . . ? C15 C7 C6 C1 163.1(3) . . . . ? C8 C7 C6 C1 39.3(4) . . . . ? C14 C7 C6 C1 -76.6(4) . . . . ? C13 C12 C11 C10 -0.7(6) . . . . ? P2 C12 C11 C10 -178.7(3) . . . . ? C2 C3 C4 C5 -2.4(6) . . . . ? C3 C4 C5 C6 -0.2(6) . . . . ? C1 C6 C5 C4 1.9(6) . . . . ? C7 C6 C5 C4 -175.8(4) . . . . ? C2 P1 C20 C21 -79.4(3) . . . . ? C16 P1 C20 C21 37.4(4) . . . . ? Au2 P1 C20 C21 168.2(3) . . . . ? C2 P1 C20 C23 43.8(3) . . . . ? C16 P1 C20 C23 160.6(3) . . . . ? Au2 P1 C20 C23 -68.5(3) . . . . ? C2 P1 C20 C22 158.6(3) . . . . ? C16 P1 C20 C22 -84.6(3) . . . . ? Au2 P1 C20 C22 46.3(3) . . . . ? C13 C8 C9 C10 -2.3(6) . . . . ? C7 C8 C9 C10 174.7(4) . . . . ? C12 P2 C28 C31 74.2(3) . . . . ? C24 P2 C28 C31 -40.9(4) . . . . ? Au2 P2 C28 C31 -171.9(3) . . . . ? C12 P2 C28 C30 -162.8(3) . . . . ? C24 P2 C28 C30 82.1(3) . . . . ? Au2 P2 C28 C30 -48.9(3) . . . . ? C12 P2 C28 C29 -48.4(3) . . . . ? C24 P2 C28 C29 -163.5(3) . . . . ? Au2 P2 C28 C29 65.5(3) . . . . ? C12 P2 C24 C25 69.4(3) . . . . ? C28 P2 C24 C25 -171.7(3) . . . . ? Au2 P2 C24 C25 -41.6(4) . . . . ? C12 P2 C24 C26 -50.5(4) . . . . ? C28 P2 C24 C26 68.5(4) . . . . ? Au2 P2 C24 C26 -161.4(3) . . . . ? C12 P2 C24 C27 -173.8(3) . . . . ? C28 P2 C24 C27 -54.8(3) . . . . ? Au2 P2 C24 C27 75.2(3) . . . . ? C12 C11 C10 C9 1.7(7) . . . . ? C8 C9 C10 C11 -0.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.849 _refine_diff_density_min -0.810 _refine_diff_density_rms 0.165 #===END