Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email ALAGUNA@UNIZAR.ES _publ_contact_author_name 'Prof Antonio Laguna' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Departamento de Quimica Inorganica Universidad de Zaragoza Instituto de Ciencia de Materiales Zaragoza E-50009 SPAIN ; _publ_section_title ; Synthesis and Structural Characterization of Luminescent Gold(I) Derivatives with an Asymmetric Bisphosphine ; loop_ _publ_author_name 'Antonio Laguna' 'Manuel Bardaji' 'Peter G. Jones' 'M. Dolores Villacampa' 'Noelia Villaverde' data_cleave _database_code_CSD 216496 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H32 Au2 Cl2 O P2' _chemical_formula_weight 839.25 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 monoclinic _symmetry_space_group_name_H-M 'P 21/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 14.9066(11) _cell_length_b 12.1750(8) _cell_length_c 14.8415(11) _cell_angle_alpha 90.00 _cell_angle_beta 97.518(3) _cell_angle_gamma 90.00 _cell_volume 2670.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 7416 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 30.5 _exptl_crystal_description tablet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.087 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 11.306 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.387 _exptl_absorpt_correction_T_max 0.564 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method '\w- & \f-scan' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47562 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 30.03 _reflns_number_total 7785 _reflns_number_gt 6702 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0189P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'rigid methyls, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7785 _refine_ls_number_parameters 268 _refine_ls_number_restraints 49 _refine_ls_R_factor_all 0.0239 _refine_ls_R_factor_gt 0.0174 _refine_ls_wR_factor_ref 0.0386 _refine_ls_wR_factor_gt 0.0374 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.986 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.866209(6) 0.367639(8) 0.431035(7) 0.02214(3) Uani 1 1 d . . . Au2 Au 0.715537(6) 0.156227(7) 0.432387(7) 0.02015(3) Uani 1 1 d . . . Cl1 Cl 0.84188(5) 0.42560(6) 0.28229(4) 0.03116(14) Uani 1 1 d . . . Cl2 Cl 0.74309(4) 0.02864(5) 0.32521(4) 0.02650(13) Uani 1 1 d . . . P1 P 0.89264(4) 0.32232(6) 0.57811(5) 0.02217(13) Uani 1 1 d . . . P2 P 0.68887(4) 0.27001(5) 0.54426(4) 0.01837(12) Uani 1 1 d . . . C1 C 0.78883(15) 0.2914(2) 0.62792(16) 0.0194(5) Uani 1 1 d . . . H1A H 0.7991 0.2245 0.6658 0.023 Uiso 1 1 calc R . . H1B H 0.7766 0.3527 0.6684 0.023 Uiso 1 1 calc R . . C2 C 0.96526(17) 0.2008(2) 0.60077(19) 0.0308(6) Uani 1 1 d U . . H2 H 0.9722 0.1860 0.6676 0.037 Uiso 1 1 calc R . . C3 C 1.0596(2) 0.2239(3) 0.5740(3) 0.0506(9) Uani 1 1 d U . . H3A H 1.0974 0.1581 0.5850 0.061 Uiso 1 1 calc R . . H3B H 1.0876 0.2849 0.6104 0.061 Uiso 1 1 calc R . . H3C H 1.0540 0.2432 0.5094 0.061 Uiso 1 1 calc R . . C4 C 0.9231(2) 0.1000(2) 0.5519(2) 0.0373(7) Uani 1 1 d U . . H4A H 0.9144 0.1133 0.4863 0.045 Uiso 1 1 calc R . . H4B H 0.8645 0.0848 0.5725 0.045 Uiso 1 1 calc R . . H4C H 0.9633 0.0367 0.5656 0.045 Uiso 1 1 calc R . . C5 C 0.94741(18) 0.4330(2) 0.64853(19) 0.0306(6) Uani 1 1 d U . . H5 H 1.0067 0.4476 0.6261 0.037 Uiso 1 1 calc R . . C6 C 0.9691(2) 0.4004(3) 0.7492(2) 0.0397(7) Uani 1 1 d U . . H6A H 1.0016 0.4605 0.7832 0.048 Uiso 1 1 calc R . . H6B H 1.0068 0.3342 0.7544 0.048 Uiso 1 1 calc R . . H6C H 0.9126 0.3857 0.7742 0.048 Uiso 1 1 calc R . . C7 C 0.8934(2) 0.5383(2) 0.6361(2) 0.0387(7) Uani 1 1 d U . . H7A H 0.8364 0.5293 0.6615 0.046 Uiso 1 1 calc R . . H7B H 0.8805 0.5554 0.5711 0.046 Uiso 1 1 calc R . . H7C H 0.9283 0.5984 0.6675 0.046 Uiso 1 1 calc R . . C11 C 0.65251(15) 0.40605(19) 0.50595(17) 0.0199(5) Uani 1 1 d DU . . C12 C 0.64352(16) 0.4311(2) 0.41378(17) 0.0245(5) Uani 1 1 d DU . . H12 H 0.6563 0.3765 0.3715 0.029 Uiso 1 1 calc R . . C13 C 0.61619(18) 0.5347(2) 0.3829(2) 0.0311(6) Uani 1 1 d DU . . H13 H 0.6102 0.5512 0.3198 0.037 Uiso 1 1 calc R . . C14 C 0.59750(18) 0.6146(2) 0.4451(2) 0.0323(6) Uani 1 1 d DU . . H14 H 0.5793 0.6860 0.4245 0.039 Uiso 1 1 calc R . . C15 C 0.60529(18) 0.5903(2) 0.5361(2) 0.0310(6) Uani 1 1 d DU . . H15 H 0.5915 0.6449 0.5779 0.037 Uiso 1 1 calc R . . C16 C 0.63305(17) 0.4867(2) 0.56768(18) 0.0265(5) Uani 1 1 d DU . . H16 H 0.6388 0.4708 0.6308 0.032 Uiso 1 1 calc R . . C21 C 0.60419(16) 0.21682(19) 0.61047(17) 0.0208(5) Uani 1 1 d DU . . C22 C 0.5469(2) 0.1342(2) 0.5745(2) 0.0394(8) Uani 1 1 d DU . . H22 H 0.5536 0.1038 0.5168 0.047 Uiso 1 1 calc R . . C23 C 0.4793(2) 0.0954(2) 0.6225(2) 0.0437(8) Uani 1 1 d DU . . H23 H 0.4399 0.0388 0.5971 0.052 Uiso 1 1 calc R . . C24 C 0.46870(19) 0.1379(2) 0.7062(2) 0.0336(7) Uani 1 1 d DU . . H24 H 0.4227 0.1104 0.7387 0.040 Uiso 1 1 calc R . . C25 C 0.52571(18) 0.2211(3) 0.74286(19) 0.0334(6) Uani 1 1 d DU . . H25 H 0.5184 0.2516 0.8004 0.040 Uiso 1 1 calc R . . C26 C 0.59332(17) 0.2597(2) 0.69532(18) 0.0283(6) Uani 1 1 d DU . . H26 H 0.6327 0.3160 0.7210 0.034 Uiso 1 1 calc R . . C97 C 0.2458(4) 0.3547(4) 0.9309(4) 0.0898(17) Uani 1 1 d U . . H97A H 0.2459 0.2872 0.9669 0.108 Uiso 1 1 calc R . . H97B H 0.1837 0.3721 0.9045 0.108 Uiso 1 1 calc R . . H97C H 0.2702 0.4153 0.9701 0.108 Uiso 1 1 calc R . . C98 C 0.3029(3) 0.3388(3) 0.8567(3) 0.0483(9) Uani 1 1 d U . . C99 C 0.2572(3) 0.2877(3) 0.7722(3) 0.0595(10) Uani 1 1 d U . . H99A H 0.3027 0.2648 0.7339 0.071 Uiso 1 1 calc R . . H99B H 0.2160 0.3411 0.7392 0.071 Uiso 1 1 calc R . . H99C H 0.2227 0.2235 0.7878 0.071 Uiso 1 1 calc R . . O99 O 0.3823(2) 0.3606(2) 0.8667(2) 0.0707(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.02097(5) 0.02616(5) 0.02004(5) -0.00191(4) 0.00546(4) -0.00324(4) Au2 0.02202(5) 0.01910(5) 0.01964(5) -0.00146(3) 0.00382(4) -0.00017(3) Cl1 0.0371(4) 0.0364(4) 0.0202(3) -0.0013(3) 0.0045(3) -0.0084(3) Cl2 0.0341(3) 0.0238(3) 0.0227(3) -0.0039(2) 0.0081(3) -0.0006(2) P1 0.0180(3) 0.0282(3) 0.0208(3) -0.0018(3) 0.0042(2) -0.0008(2) P2 0.0186(3) 0.0170(3) 0.0198(3) -0.0002(2) 0.0036(2) -0.0005(2) C1 0.0175(11) 0.0216(12) 0.0196(12) -0.0008(9) 0.0045(9) 0.0007(9) C2 0.0229(13) 0.0442(16) 0.0252(15) 0.0015(12) 0.0027(11) 0.0121(12) C3 0.0247(16) 0.074(3) 0.056(2) 0.0072(19) 0.0126(15) 0.0134(15) C4 0.0427(17) 0.0376(16) 0.0318(17) -0.0001(13) 0.0054(13) 0.0189(13) C5 0.0262(14) 0.0393(16) 0.0271(15) -0.0074(12) 0.0065(11) -0.0117(11) C6 0.0325(15) 0.058(2) 0.0280(16) -0.0125(14) 0.0009(12) -0.0113(14) C7 0.0440(18) 0.0339(16) 0.0394(18) -0.0091(13) 0.0097(14) -0.0135(13) C11 0.0176(11) 0.0175(11) 0.0248(13) 0.0009(9) 0.0034(9) -0.0014(9) C12 0.0209(12) 0.0304(13) 0.0220(13) 0.0013(10) 0.0027(10) 0.0004(10) C13 0.0302(15) 0.0354(15) 0.0273(15) 0.0109(12) 0.0015(11) 0.0017(11) C14 0.0269(14) 0.0240(13) 0.0452(18) 0.0114(12) 0.0013(13) 0.0021(11) C15 0.0315(14) 0.0210(13) 0.0399(17) -0.0027(11) 0.0023(12) 0.0043(11) C16 0.0317(14) 0.0249(13) 0.0230(14) 0.0010(10) 0.0036(11) 0.0043(11) C21 0.0190(12) 0.0184(11) 0.0254(13) 0.0036(9) 0.0048(10) 0.0017(9) C22 0.0432(18) 0.0283(15) 0.051(2) -0.0170(13) 0.0232(15) -0.0107(12) C23 0.0419(18) 0.0261(15) 0.069(2) -0.0124(15) 0.0290(16) -0.0152(13) C24 0.0293(15) 0.0295(15) 0.0447(18) 0.0116(12) 0.0152(13) -0.0001(11) C25 0.0308(15) 0.0481(18) 0.0220(14) 0.0060(12) 0.0059(11) -0.0039(12) C26 0.0240(13) 0.0401(16) 0.0202(13) 0.0016(11) 0.0004(10) -0.0082(11) C97 0.087(4) 0.091(4) 0.099(4) -0.016(3) 0.042(3) 0.027(3) C98 0.052(2) 0.0286(16) 0.066(3) 0.0088(15) 0.0162(18) 0.0075(14) C99 0.063(2) 0.045(2) 0.071(3) 0.0040(19) 0.013(2) 0.0014(18) O99 0.0547(18) 0.0662(19) 0.093(2) 0.0054(16) 0.0166(16) -0.0115(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.2358(7) . Y Au1 Cl1 2.3008(7) . Y Au2 P2 2.2375(6) . Y Au2 Cl2 2.2985(6) . Y Au1 Au2 3.4179(2) . y P1 C5 1.831(3) . Y P1 C2 1.838(3) . Y P1 C1 1.839(2) . Y P2 C11 1.811(2) . Y P2 C21 1.817(2) . Y P2 C1 1.829(2) . Y C2 C4 1.520(4) . ? C2 C3 1.537(4) . ? C5 C7 1.512(4) . ? C5 C6 1.539(4) . ? C11 C12 1.391(3) . ? C11 C16 1.399(3) . ? C12 C13 1.385(3) . ? C13 C14 1.394(4) . ? C14 C15 1.372(4) . ? C15 C16 1.389(4) . ? C21 C22 1.382(4) . ? C21 C26 1.392(3) . ? C22 C23 1.391(4) . ? C23 C24 1.374(4) . ? C24 C25 1.387(4) . ? C25 C26 1.386(3) . ? C97 C98 1.490(6) . ? C98 O99 1.203(4) . ? C98 C99 1.482(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 Cl1 176.31(2) . . Y P2 Au2 Cl2 175.67(2) . . Y P1 Au1 Au2 80.818(17) . . y Cl1 Au1 Au2 102.441(17) . . y P2 Au2 Au1 73.666(16) . . y Cl2 Au2 Au1 109.136(17) . . y C5 P1 C2 106.25(13) . . Y C5 P1 C1 104.90(12) . . Y C2 P1 C1 105.54(12) . . Y C5 P1 Au1 112.59(9) . . Y C2 P1 Au1 113.68(9) . . Y C1 P1 Au1 113.14(8) . . Y C11 P2 C21 107.17(11) . . Y C11 P2 C1 105.48(11) . . Y C21 P2 C1 104.20(11) . . Y C11 P2 Au2 114.09(8) . . Y C21 P2 Au2 112.58(8) . . Y C1 P2 Au2 112.56(8) . . Y P2 C1 P1 114.19(13) . . Y C4 C2 C3 111.0(2) . . ? C4 C2 P1 111.49(19) . . ? C3 C2 P1 110.1(2) . . ? C7 C5 C6 112.2(2) . . ? C7 C5 P1 111.3(2) . . ? C6 C5 P1 112.7(2) . . ? C12 C11 C16 119.3(2) . . ? C12 C11 P2 119.71(19) . . ? C16 C11 P2 121.04(19) . . ? C13 C12 C11 120.8(2) . . ? C12 C13 C14 119.4(3) . . ? C15 C14 C13 120.2(3) . . ? C14 C15 C16 120.7(3) . . ? C15 C16 C11 119.6(2) . . ? C22 C21 C26 118.9(2) . . ? C22 C21 P2 119.2(2) . . ? C26 C21 P2 121.80(19) . . ? C21 C22 C23 120.1(3) . . ? C24 C23 C22 120.8(3) . . ? C23 C24 C25 119.5(3) . . ? C26 C25 C24 119.8(3) . . ? C25 C26 C21 120.8(3) . . ? O99 C98 C99 122.2(4) . . ? O99 C98 C97 121.8(4) . . ? C99 C98 C97 115.8(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C1 H1A Cl1 0.99 2.54 3.518(3) 170.1 4_566 C1 H1B Cl2 0.99 2.84 3.790(2) 161.3 4_566 C6 H6C Cl2 0.98 2.92 3.789(3) 147.9 4_566 C26 H26 Cl2 0.95 2.83 3.771(3) 170.5 4_566 C5 H5 Cl1 1.00 2.92 3.611(3) 127.0 3_766 C6 H6A Cl1 0.98 2.98 3.605(3) 122.3 3_766 C99 H99B Cl1 0.98 2.97 3.835(4) 147.2 3_666 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.897 _refine_diff_density_min -0.616 _refine_diff_density_rms 0.106 #===END data_klemm _database_code_CSD 216497 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23.50 H35 Au2 Br2 O1.50 P2' _chemical_formula_weight 957.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.7999(14) _cell_length_b 16.6728(12) _cell_length_c 18.2896(12) _cell_angle_alpha 90.00 _cell_angle_beta 105.643(3) _cell_angle_gamma 90.00 _cell_volume 5814.1(7) _cell_formula_units_Z 8 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 6163 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 30.5 _exptl_crystal_description tablet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.187 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3568 _exptl_absorpt_coefficient_mu 12.956 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.283 _exptl_absorpt_correction_T_max 0.494 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method '\w- & \f-scan' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52984 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 30.03 _reflns_number_total 8508 _reflns_number_gt 7384 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The second acetone molecule is disordered over a twofold axis; it was refined isotropically without hydrogens. ; _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^)+(0.0277P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'rigid methyls, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8508 _refine_ls_number_parameters 284 _refine_ls_number_restraints 67 _refine_ls_R_factor_all 0.0255 _refine_ls_R_factor_gt 0.0199 _refine_ls_wR_factor_ref 0.0491 _refine_ls_wR_factor_gt 0.0479 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.997 _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 0.899918(6) 0.595263(6) 0.256969(6) 0.01999(3) Uani 1 1 d . . . Au2 Au 0.771251(6) 0.609221(6) 0.328091(6) 0.01892(3) Uani 1 1 d . . . Br1 Br 0.980971(16) 0.657165(18) 0.365368(17) 0.02941(7) Uani 1 1 d . . . Br2 Br 0.76334(2) 0.745004(17) 0.369694(19) 0.03489(8) Uani 1 1 d . . . P2 P 0.76797(4) 0.48056(4) 0.29196(4) 0.01666(13) Uani 1 1 d . . . P1 P 0.82731(4) 0.52937(4) 0.16012(4) 0.01758(14) Uani 1 1 d . . . C1 C 0.76272(14) 0.46759(16) 0.19133(15) 0.0189(5) Uani 1 1 d . . . H1A H 0.7149 0.4820 0.1608 0.023 Uiso 1 1 calc R . . H1B H 0.7706 0.4104 0.1816 0.023 Uiso 1 1 calc R . . C2 C 0.77318(15) 0.59324(16) 0.08531(16) 0.0199(5) Uani 1 1 d U . . H2 H 0.7411 0.5579 0.0471 0.024 Uiso 1 1 calc R . . C3 C 0.81916(17) 0.64042(19) 0.04486(18) 0.0288(6) Uani 1 1 d U . . H3A H 0.7893 0.6734 0.0046 0.035 Uiso 1 1 calc R . . H3B H 0.8462 0.6029 0.0226 0.035 Uiso 1 1 calc R . . H3C H 0.8514 0.6751 0.0815 0.035 Uiso 1 1 calc R . . C4 C 0.72822(18) 0.65057(19) 0.11799(19) 0.0327(7) Uani 1 1 d U . . H4A H 0.7588 0.6861 0.1553 0.039 Uiso 1 1 calc R . . H4B H 0.6986 0.6195 0.1427 0.039 Uiso 1 1 calc R . . H4C H 0.6985 0.6828 0.0769 0.039 Uiso 1 1 calc R . . C5 C 0.87573(15) 0.45921(17) 0.11519(16) 0.0225(6) Uani 1 1 d U . . H5 H 0.9132 0.4908 0.1010 0.027 Uiso 1 1 calc R . . C6 C 0.83130(17) 0.41992(18) 0.04253(17) 0.0270(6) Uani 1 1 d U . . H6A H 0.8605 0.3830 0.0226 0.032 Uiso 1 1 calc R . . H6B H 0.8123 0.4614 0.0046 0.032 Uiso 1 1 calc R . . H6C H 0.7926 0.3901 0.0538 0.032 Uiso 1 1 calc R . . C7 C 0.91243(18) 0.39680(19) 0.1735(2) 0.0321(7) Uani 1 1 d U . . H7A H 0.8775 0.3603 0.1841 0.038 Uiso 1 1 calc R . . H7B H 0.9377 0.4238 0.2205 0.038 Uiso 1 1 calc R . . H7C H 0.9457 0.3662 0.1533 0.038 Uiso 1 1 calc R . . C11 C 0.84270(14) 0.42095(16) 0.34302(15) 0.0183(5) Uani 1 1 d DU . . C12 C 0.89827(14) 0.45631(16) 0.39789(15) 0.0207(5) Uani 1 1 d DU . . H12 H 0.8978 0.5123 0.4071 0.025 Uiso 1 1 calc R . . C13 C 0.95394(16) 0.40996(17) 0.43876(17) 0.0250(6) Uani 1 1 d DU . . H13 H 0.9918 0.4343 0.4752 0.030 Uiso 1 1 calc R . . C14 C 0.95408(16) 0.32769(18) 0.42613(18) 0.0278(6) Uani 1 1 d DU . . H14 H 0.9913 0.2955 0.4552 0.033 Uiso 1 1 calc R . . C15 C 0.89978(16) 0.29260(17) 0.37111(18) 0.0271(6) Uani 1 1 d DU . . H15 H 0.9007 0.2367 0.3615 0.033 Uiso 1 1 calc R . . C16 C 0.84417(15) 0.33871(16) 0.33012(17) 0.0240(6) Uani 1 1 d DU . . H16 H 0.8069 0.3141 0.2931 0.029 Uiso 1 1 calc R . . C21 C 0.69370(14) 0.42735(16) 0.30944(15) 0.0190(5) Uani 1 1 d DU . . C22 C 0.65749(15) 0.36684(17) 0.26208(18) 0.0256(6) Uani 1 1 d DU . . H22 H 0.6685 0.3545 0.2159 0.031 Uiso 1 1 calc R . . C23 C 0.60514(16) 0.32483(18) 0.2833(2) 0.0316(7) Uani 1 1 d DU . . H23 H 0.5803 0.2837 0.2512 0.038 Uiso 1 1 calc R . . C24 C 0.58867(17) 0.34184(18) 0.35047(19) 0.0312(7) Uani 1 1 d DU . . H24 H 0.5531 0.3122 0.3645 0.037 Uiso 1 1 calc R . . C25 C 0.62423(17) 0.40213(19) 0.39707(19) 0.0316(7) Uani 1 1 d DU . . H25 H 0.6131 0.4139 0.4433 0.038 Uiso 1 1 calc R . . C26 C 0.67612(16) 0.44547(18) 0.37676(17) 0.0261(6) Uani 1 1 d DU . . H26 H 0.6998 0.4875 0.4086 0.031 Uiso 1 1 calc R . . O91 O 0.64070(16) 0.45758(18) 0.03175(16) 0.0617(9) Uani 1 1 d DU . . C91 C 0.60443(19) 0.3986(2) 0.0135(2) 0.0399(9) Uani 1 1 d DU . . C92 C 0.5472(3) 0.3795(3) 0.0477(3) 0.0660(13) Uani 1 1 d DU . . H92A H 0.5466 0.4189 0.0872 0.079 Uiso 1 1 calc R . . H92B H 0.5545 0.3257 0.0701 0.079 Uiso 1 1 calc R . . H92C H 0.5024 0.3810 0.0084 0.079 Uiso 1 1 calc R . . C93 C 0.6168(3) 0.3418(3) -0.0444(3) 0.0730(14) Uani 1 1 d DU . . H93A H 0.6532 0.3634 -0.0660 0.088 Uiso 1 1 calc R . . H93B H 0.5732 0.3347 -0.0848 0.088 Uiso 1 1 calc R . . H93C H 0.6320 0.2899 -0.0205 0.088 Uiso 1 1 calc R . . O92 O 0.4511(7) 0.5930(6) 0.3296(7) 0.135(4) Uiso 0.50 1 d PDU A -1 C94 C 0.4783(7) 0.5968(6) 0.2767(8) 0.093(4) Uiso 0.50 1 d PDU A -1 C95 C 0.4810(5) 0.6779(5) 0.2421(8) 0.076(3) Uiso 0.50 1 d PDU A -1 C96 C 0.5080(10) 0.5256(5) 0.2445(11) 0.077(3) Uiso 0.50 1 d PDU A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.02205(5) 0.02249(5) 0.01473(5) 0.00043(4) 0.00373(4) -0.00475(4) Au2 0.02534(6) 0.01705(5) 0.01586(5) 0.00035(4) 0.00809(4) 0.00014(4) Br1 0.03399(16) 0.02836(15) 0.02010(14) 0.00179(11) -0.00263(12) -0.01068(12) Br2 0.0594(2) 0.01760(14) 0.03443(18) 0.00020(12) 0.02436(16) 0.00311(13) P2 0.0185(3) 0.0181(3) 0.0142(3) -0.0004(2) 0.0058(3) -0.0012(2) P1 0.0188(3) 0.0214(3) 0.0132(3) -0.0007(3) 0.0054(3) -0.0014(2) C1 0.0212(13) 0.0206(13) 0.0146(13) -0.0010(10) 0.0044(10) -0.0009(10) C2 0.0217(13) 0.0237(13) 0.0145(13) 0.0021(10) 0.0049(11) 0.0002(10) C3 0.0339(16) 0.0287(15) 0.0257(16) 0.0046(12) 0.0115(13) 0.0012(12) C4 0.0404(18) 0.0337(17) 0.0291(17) 0.0077(13) 0.0180(14) 0.0141(14) C5 0.0259(14) 0.0249(14) 0.0200(14) 0.0002(11) 0.0119(12) 0.0030(11) C6 0.0336(16) 0.0262(15) 0.0230(15) -0.0047(12) 0.0107(13) 0.0005(12) C7 0.0285(16) 0.0392(18) 0.0304(17) 0.0050(13) 0.0114(14) 0.0134(13) C11 0.0209(13) 0.0205(12) 0.0151(13) 0.0015(10) 0.0073(10) -0.0007(10) C12 0.0236(14) 0.0224(13) 0.0170(13) 0.0018(10) 0.0068(11) -0.0026(10) C13 0.0237(14) 0.0304(15) 0.0204(15) 0.0019(11) 0.0052(12) -0.0028(11) C14 0.0244(15) 0.0310(15) 0.0296(16) 0.0104(13) 0.0100(12) 0.0050(12) C15 0.0326(16) 0.0193(13) 0.0315(17) 0.0025(11) 0.0123(13) 0.0027(11) C16 0.0253(14) 0.0201(13) 0.0265(16) 0.0006(11) 0.0066(12) -0.0027(10) C21 0.0181(12) 0.0195(12) 0.0196(13) -0.0011(10) 0.0053(10) -0.0005(10) C22 0.0253(14) 0.0236(14) 0.0301(16) -0.0090(12) 0.0110(12) -0.0033(11) C23 0.0258(15) 0.0238(15) 0.046(2) -0.0102(13) 0.0116(14) -0.0058(11) C24 0.0269(15) 0.0285(16) 0.0420(19) 0.0008(13) 0.0155(14) -0.0067(12) C25 0.0298(16) 0.0442(19) 0.0249(16) -0.0009(13) 0.0142(13) -0.0081(13) C26 0.0252(15) 0.0341(16) 0.0202(14) -0.0032(12) 0.0080(12) -0.0073(12) O91 0.0613(19) 0.0668(19) 0.0441(17) 0.0163(14) -0.0081(14) -0.0319(15) C91 0.0327(18) 0.047(2) 0.035(2) 0.0100(15) 0.0007(15) -0.0089(15) C92 0.063(3) 0.076(3) 0.069(3) -0.004(3) 0.035(3) -0.018(2) C93 0.058(3) 0.087(4) 0.073(4) -0.014(3) 0.017(3) 0.005(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 2.2445(7) . Y Au1 Br1 2.4198(3) . Y Au1 Au2 3.1660(2) . Y Au2 P2 2.2403(7) . Y Au2 Br2 2.4069(3) . Y P2 C11 1.818(3) . Y P2 C21 1.818(3) . Y P2 C1 1.828(3) . Y P1 C2 1.834(3) . Y P1 C5 1.841(3) . Y P1 C1 1.848(3) . Y C2 C4 1.533(4) . ? C2 C3 1.536(4) . ? C5 C7 1.526(4) . ? C5 C6 1.529(4) . ? C11 C16 1.393(4) . ? C11 C12 1.403(4) . ? C12 C13 1.388(4) . ? C13 C14 1.391(4) . ? C14 C15 1.388(4) . ? C15 C16 1.386(4) . ? C21 C22 1.395(4) . ? C21 C26 1.400(4) . ? C22 C23 1.391(4) . ? C23 C24 1.382(4) . ? C24 C25 1.382(4) . ? C25 C26 1.386(4) . ? O91 C91 1.210(4) . ? C91 C92 1.468(5) . ? C91 C93 1.489(6) . ? O92 C94 1.229(13) . ? C94 C95 1.499(11) . ? C94 C96 1.513(11) . ? 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 175.94(2) . . Y P1 Au1 Au2 86.853(19) . . Y Br1 Au1 Au2 93.520(10) . . Y P2 Au2 Br2 174.08(2) . . Y P2 Au2 Au1 76.759(18) . . Y Br2 Au2 Au1 109.098(10) . . Y C11 P2 C21 103.17(12) . . Y C11 P2 C1 105.67(13) . . Y C21 P2 C1 106.87(12) . . Y C11 P2 Au2 114.66(9) . . Y C21 P2 Au2 112.08(9) . . Y C1 P2 Au2 113.55(9) . . Y C2 P1 C5 107.81(13) . . Y C2 P1 C1 103.89(13) . . Y C5 P1 C1 105.71(13) . . Y C2 P1 Au1 115.19(9) . . Y C5 P1 Au1 111.32(10) . . Y C1 P1 Au1 112.23(9) . . Y P2 C1 P1 112.87(14) . . Y C4 C2 C3 110.5(2) . . ? C4 C2 P1 110.8(2) . . ? C3 C2 P1 110.7(2) . . ? C7 C5 C6 111.7(2) . . ? C7 C5 P1 109.2(2) . . ? C6 C5 P1 114.4(2) . . ? C16 C11 C12 119.1(3) . . ? C16 C11 P2 120.2(2) . . ? C12 C11 P2 120.7(2) . . ? C13 C12 C11 120.5(3) . . ? C12 C13 C14 119.8(3) . . ? C15 C14 C13 120.0(3) . . ? C16 C15 C14 120.4(3) . . ? C15 C16 C11 120.3(3) . . ? C22 C21 C26 119.6(3) . . ? C22 C21 P2 123.2(2) . . ? C26 C21 P2 117.0(2) . . ? C23 C22 C21 119.2(3) . . ? C24 C23 C22 121.2(3) . . ? C25 C24 C23 119.6(3) . . ? C24 C25 C26 120.3(3) . . ? C25 C26 C21 120.1(3) . . ? O91 C91 C92 121.9(4) . . ? O91 C91 C93 120.9(4) . . ? C92 C91 C93 117.2(4) . . ? O92 C94 C95 116.8(11) . . ? O92 C94 C96 124.4(11) . . ? C95 C94 C96 118.8(11) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C1 H1A O91 0.99 2.45 3.253(4) 137.4 . C2 H2 O91 1.00 2.55 3.401(4) 142.4 . C24 H24 Br1 0.95 2.96 3.797(3) 148.2 3_445 C23 H23 Br1 0.95 3.01 3.952(3) 170.5 4_645 C1 H1B Br2 0.99 2.93 3.870(3) 158.4 4_645 C6 H6C Br2 0.98 3.14 4.027(3) 150.8 4_645 C16 H16 Br2 0.95 3.14 4.016(3) 153.3 4_645 C22 H22 Br2 0.95 2.96 3.799(3) 148.3 4_645 C93 H93C Br2 0.98 3.06 3.789(5) 132.1 4_645 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.427 _refine_diff_density_min -1.195 _refine_diff_density_rms 0.128 #===END data_lol33as _database_code_CSD 216498 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H26 Au2 F10 P2' _chemical_formula_weight 1044.39 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.9723(10) _cell_length_b 16.9452(13) _cell_length_c 15.1980(11) _cell_angle_alpha 90.00 _cell_angle_beta 108.926(2) _cell_angle_gamma 90.00 _cell_volume 3160.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4475 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 28 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.195 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 9.456 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.6997 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; SADABS; Area-Detector Absorption Correction. Bruker-AXS within SAINT+ package, v. 6.02 (1999). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20427 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0675 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 28.43 _reflns_number_total 7342 _reflns_number_gt 5606 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v. 5.611 (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT+ 6.02 (Bruker AXS, 1999)' _computing_data_reduction 'SAINT+ 6.02 (Bruker AXS, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, SHELXTL v. 6.10 (Bruker, 2000)' _computing_publication_material 'XCIF, SHELXTL v. 6.10 (Bruker, 2000)' _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^)+(0.0122P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7342 _refine_ls_number_parameters 410 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0566 _refine_ls_wR_factor_gt 0.0534 _refine_ls_goodness_of_fit_ref 0.880 _refine_ls_restrained_S_all 0.880 _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 -0.023038(18) 0.053257(12) 0.158728(15) 0.01878(6) Uani 1 1 d . . . Au2 Au 0.028704(19) 0.136221(12) 0.349423(15) 0.01992(6) Uani 1 1 d . . . P1 P 0.13250(12) 0.10050(9) 0.14072(10) 0.0176(3) Uani 1 1 d . . . P2 P 0.20538(12) 0.12128(9) 0.35528(10) 0.0181(3) Uani 1 1 d . . . C1 C -0.1674(4) 0.0089(3) 0.1642(3) 0.0177(13) Uani 1 1 d . . . C2 C -0.2656(5) 0.0465(3) 0.1258(4) 0.0227(13) Uani 1 1 d . . . C3 C -0.3636(5) 0.0178(3) 0.1298(4) 0.0250(14) Uani 1 1 d . . . C4 C -0.3645(5) -0.0516(4) 0.1768(4) 0.0282(15) Uani 1 1 d . . . C5 C -0.2673(5) -0.0906(3) 0.2176(4) 0.0260(15) Uani 1 1 d . . . C6 C -0.1736(5) -0.0607(3) 0.2107(4) 0.0217(13) Uani 1 1 d . . . F1 F -0.2702(3) 0.1147(2) 0.0790(2) 0.0348(9) Uani 1 1 d . . . F2 F -0.4573(3) 0.0558(2) 0.0881(3) 0.0444(10) Uani 1 1 d . . . F3 F -0.4584(3) -0.0803(2) 0.1825(3) 0.0430(10) Uani 1 1 d . . . F4 F -0.2675(3) -0.15746(19) 0.2651(2) 0.0374(9) Uani 1 1 d . . . F5 F -0.0811(3) -0.10214(19) 0.2517(2) 0.0299(8) Uani 1 1 d . . . C11 C -0.1294(5) 0.1412(3) 0.3480(4) 0.0216(13) Uani 1 1 d . . . C12 C -0.1972(5) 0.2061(4) 0.3159(4) 0.0257(14) Uani 1 1 d . . . C13 C -0.3058(5) 0.2078(4) 0.3101(4) 0.0295(15) Uani 1 1 d . . . C14 C -0.3514(5) 0.1412(4) 0.3331(4) 0.0286(15) Uani 1 1 d . . . C15 C -0.2885(5) 0.0760(4) 0.3646(4) 0.0252(15) Uani 1 1 d . . . C16 C -0.1809(5) 0.0777(3) 0.3719(4) 0.0225(14) Uani 1 1 d . . . F6 F -0.1570(3) 0.27167(19) 0.2886(2) 0.0360(9) Uani 1 1 d . . . F7 F -0.3663(3) 0.2726(2) 0.2805(2) 0.0439(10) Uani 1 1 d . . . F8 F -0.4581(3) 0.1414(2) 0.3246(2) 0.0431(10) Uani 1 1 d . . . F9 F -0.3355(3) 0.0112(2) 0.3861(2) 0.0418(10) Uani 1 1 d . . . F10 F -0.1225(3) 0.01116(19) 0.4055(2) 0.0351(9) Uani 1 1 d . . . C21 C 0.2490(5) 0.0201(3) 0.3823(3) 0.0195(13) Uani 1 1 d . . . C22 C 0.3571(5) -0.0020(3) 0.4021(3) 0.0247(14) Uani 1 1 d . . . H22 H 0.4093 0.0363 0.4044 0.030 Uiso 1 1 calc R . . C23 C 0.3883(5) -0.0794(3) 0.4183(4) 0.0299(16) Uani 1 1 d . . . H23 H 0.4610 -0.0936 0.4320 0.036 Uiso 1 1 calc R . . C24 C 0.3098(5) -0.1364(4) 0.4140(4) 0.0304(16) Uani 1 1 d . . . H24 H 0.3299 -0.1892 0.4237 0.036 Uiso 1 1 calc R . . C25 C 0.2034(5) -0.1154(3) 0.3955(4) 0.0291(15) Uani 1 1 d . . . H25 H 0.1516 -0.1538 0.3937 0.035 Uiso 1 1 calc R . . C26 C 0.1717(5) -0.0369(3) 0.3794(3) 0.0229(14) Uani 1 1 d . . . H26 H 0.0990 -0.0228 0.3666 0.027 Uiso 1 1 calc R . . C31 C 0.3080(4) 0.1802(3) 0.4400(4) 0.0180(13) Uani 1 1 d . . . C32 C 0.3782(5) 0.2313(3) 0.4174(4) 0.0239(14) Uani 1 1 d . . . H32 H 0.3737 0.2369 0.3554 0.029 Uiso 1 1 calc R . . C33 C 0.4544(5) 0.2742(3) 0.4840(4) 0.0246(14) Uani 1 1 d . . . H33 H 0.5006 0.3085 0.4669 0.029 Uiso 1 1 calc R . . C34 C 0.4625(5) 0.2664(3) 0.5757(4) 0.0253(14) Uani 1 1 d . . . H34 H 0.5136 0.2957 0.6211 0.030 Uiso 1 1 calc R . . C35 C 0.3937(5) 0.2145(3) 0.6001(4) 0.0259(14) Uani 1 1 d . . . H35 H 0.4000 0.2081 0.6624 0.031 Uiso 1 1 calc R . . C36 C 0.3160(4) 0.1723(3) 0.5327(4) 0.0221(14) Uani 1 1 d . . . H36 H 0.2689 0.1387 0.5495 0.027 Uiso 1 1 calc R . . C37 C 0.2303(4) 0.1426(3) 0.2465(3) 0.0209(13) Uani 1 1 d . . . H37A H 0.3024 0.1233 0.2515 0.025 Uiso 1 1 calc R . . H37B H 0.2310 0.1994 0.2391 0.025 Uiso 1 1 calc R . . C38 C 0.2064(4) 0.0271(3) 0.0963(4) 0.0198(13) Uani 1 1 d . . . H38 H 0.1561 0.0104 0.0359 0.024 Uiso 1 1 calc R . . C39 C 0.2329(5) -0.0467(3) 0.1558(4) 0.0336(16) Uani 1 1 d . . . H39A H 0.2559 -0.0877 0.1228 0.050 Uiso 1 1 calc R . . H39B H 0.1692 -0.0637 0.1696 0.050 Uiso 1 1 calc R . . H39C H 0.2903 -0.0355 0.2128 0.050 Uiso 1 1 calc R . . C40 C 0.3062(5) 0.0598(4) 0.0771(4) 0.0370(17) Uani 1 1 d . . . H40A H 0.3580 0.0781 0.1341 0.056 Uiso 1 1 calc R . . H40B H 0.2849 0.1030 0.0340 0.056 Uiso 1 1 calc R . . H40C H 0.3387 0.0191 0.0509 0.056 Uiso 1 1 calc R . . C41 C 0.1056(5) 0.1835(3) 0.0602(4) 0.0229(14) Uani 1 1 d . . . H41 H 0.1754 0.2079 0.0638 0.028 Uiso 1 1 calc R . . C42 C 0.0364(5) 0.2446(3) 0.0878(4) 0.0351(17) Uani 1 1 d . . . H42A H 0.0326 0.2917 0.0517 0.053 Uiso 1 1 calc R . . H42B H 0.0684 0.2568 0.1527 0.053 Uiso 1 1 calc R . . H42C H -0.0358 0.2241 0.0766 0.053 Uiso 1 1 calc R . . C43 C 0.0492(5) 0.1575(3) -0.0397(4) 0.0335(16) Uani 1 1 d . . . H43A H -0.0209 0.1356 -0.0451 0.050 Uiso 1 1 calc R . . H43B H 0.0928 0.1183 -0.0566 0.050 Uiso 1 1 calc R . . H43C H 0.0400 0.2022 -0.0804 0.050 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 0.01491(12) 0.02252(13) 0.01927(12) -0.00153(10) 0.00606(9) -0.00347(10) Au2 0.01633(12) 0.02271(13) 0.02034(12) -0.00320(10) 0.00545(9) 0.00180(10) P1 0.0152(8) 0.0185(8) 0.0193(8) -0.0011(6) 0.0059(6) -0.0033(6) P2 0.0161(8) 0.0202(8) 0.0176(8) -0.0036(6) 0.0047(6) -0.0015(6) C1 0.015(3) 0.028(3) 0.013(3) -0.007(2) 0.007(2) -0.005(2) C2 0.025(4) 0.022(3) 0.025(3) -0.004(3) 0.014(3) -0.001(3) C3 0.013(3) 0.025(4) 0.040(4) -0.007(3) 0.013(3) 0.003(3) C4 0.024(4) 0.028(4) 0.042(4) -0.010(3) 0.024(3) -0.008(3) C5 0.041(4) 0.016(3) 0.026(3) -0.003(3) 0.018(3) -0.001(3) C6 0.020(3) 0.025(3) 0.021(3) -0.004(3) 0.008(3) 0.000(3) F1 0.027(2) 0.031(2) 0.046(2) 0.0095(18) 0.0127(18) 0.0025(17) F2 0.020(2) 0.043(2) 0.069(3) 0.004(2) 0.014(2) 0.0082(18) F3 0.022(2) 0.044(2) 0.070(3) -0.001(2) 0.025(2) -0.0095(18) F4 0.040(2) 0.026(2) 0.053(2) 0.0077(18) 0.0251(19) -0.0037(18) F5 0.024(2) 0.031(2) 0.035(2) 0.0070(16) 0.0095(16) 0.0032(16) C11 0.025(3) 0.024(4) 0.014(3) -0.007(2) 0.005(2) -0.004(3) C12 0.024(4) 0.026(4) 0.026(3) -0.005(3) 0.006(3) 0.001(3) C13 0.019(4) 0.031(4) 0.032(4) -0.010(3) 0.000(3) 0.007(3) C14 0.015(3) 0.047(5) 0.026(3) -0.011(3) 0.009(3) -0.003(3) C15 0.030(4) 0.026(4) 0.024(3) -0.008(3) 0.015(3) -0.009(3) C16 0.022(4) 0.028(4) 0.017(3) -0.005(3) 0.006(3) 0.005(3) F6 0.028(2) 0.025(2) 0.049(2) 0.0027(17) 0.0040(18) -0.0005(17) F7 0.025(2) 0.035(2) 0.063(3) -0.0050(19) 0.0024(19) 0.0142(18) F8 0.014(2) 0.067(3) 0.047(2) -0.009(2) 0.0098(17) 0.0002(19) F9 0.039(3) 0.048(3) 0.046(2) 0.0032(19) 0.025(2) -0.0063(19) F10 0.038(2) 0.032(2) 0.038(2) 0.0054(17) 0.0164(18) 0.0063(18) C21 0.021(3) 0.022(3) 0.015(3) -0.006(2) 0.004(2) -0.003(3) C22 0.019(3) 0.030(4) 0.021(3) -0.005(3) 0.001(3) 0.001(3) C23 0.024(4) 0.031(4) 0.031(4) -0.003(3) 0.003(3) 0.008(3) C24 0.036(4) 0.021(4) 0.031(4) -0.004(3) 0.005(3) 0.011(3) C25 0.039(4) 0.019(3) 0.032(4) -0.003(3) 0.016(3) -0.009(3) C26 0.025(4) 0.028(4) 0.016(3) 0.000(3) 0.007(3) 0.000(3) C31 0.013(3) 0.019(3) 0.020(3) -0.002(2) 0.004(2) 0.003(2) C32 0.021(4) 0.024(4) 0.023(3) 0.002(3) 0.003(3) 0.001(3) C33 0.020(3) 0.022(3) 0.029(3) -0.004(3) 0.004(3) -0.006(3) C34 0.024(4) 0.018(3) 0.028(3) -0.009(3) 0.000(3) -0.003(3) C35 0.026(4) 0.032(4) 0.021(3) -0.003(3) 0.008(3) 0.005(3) C36 0.014(3) 0.026(4) 0.027(3) -0.001(3) 0.007(3) 0.000(2) C37 0.020(3) 0.025(3) 0.016(3) -0.001(2) 0.004(2) -0.004(3) C38 0.016(3) 0.028(3) 0.017(3) -0.006(2) 0.008(2) -0.004(3) C39 0.037(4) 0.027(4) 0.033(4) -0.009(3) 0.005(3) 0.004(3) C40 0.024(4) 0.047(4) 0.046(4) -0.019(3) 0.020(3) -0.003(3) C41 0.024(4) 0.020(3) 0.024(3) 0.001(3) 0.006(3) -0.001(3) C42 0.036(4) 0.024(4) 0.039(4) 0.004(3) 0.003(3) 0.002(3) C43 0.047(5) 0.028(4) 0.022(3) 0.005(3) 0.007(3) 0.003(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 C1 2.044(5) . ? Au1 P1 2.2682(15) . ? Au1 Au2 3.0926(3) . ? Au2 C11 2.046(6) . ? Au2 P2 2.2787(15) . ? P1 C41 1.822(5) . ? P1 C38 1.827(5) . ? P1 C37 1.838(5) . ? P2 C21 1.811(6) . ? P2 C37 1.821(5) . ? P2 C31 1.821(5) . ? C1 C2 1.374(7) . ? C1 C6 1.391(7) . ? C2 F1 1.348(6) . ? C2 C3 1.381(7) . ? C3 F2 1.339(6) . ? C3 C4 1.378(8) . ? C4 F3 1.340(6) . ? C4 C5 1.379(8) . ? C5 F4 1.344(6) . ? C5 C6 1.352(8) . ? C6 F5 1.355(6) . ? C11 C16 1.376(7) . ? C11 C12 1.393(7) . ? C12 F6 1.348(6) . ? C12 C13 1.383(8) . ? C13 F7 1.341(6) . ? C13 C14 1.370(8) . ? C14 F8 1.348(6) . ? C14 C15 1.365(8) . ? C15 F9 1.346(6) . ? C15 C16 1.364(8) . ? C16 F10 1.362(6) . ? C21 C26 1.382(7) . ? C21 C22 1.387(7) . ? C22 C23 1.371(7) . ? C23 C24 1.390(8) . ? C24 C25 1.363(8) . ? C25 C26 1.390(7) . ? C31 C32 1.379(7) . ? C31 C36 1.385(7) . ? C32 C33 1.371(7) . ? C33 C34 1.369(7) . ? C34 C35 1.387(8) . ? C35 C36 1.382(7) . ? C38 C39 1.517(7) . ? C38 C40 1.522(7) . ? C41 C42 1.517(7) . ? C41 C43 1.521(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Au1 P1 175.59(14) . . ? C1 Au1 Au2 92.98(14) . . ? P1 Au1 Au2 91.23(4) . . ? C11 Au2 P2 175.70(16) . . ? C11 Au2 Au1 95.54(14) . . ? P2 Au2 Au1 84.03(4) . . ? C41 P1 C38 106.6(3) . . ? C41 P1 C37 102.5(2) . . ? C38 P1 C37 106.9(3) . . ? C41 P1 Au1 111.7(2) . . ? C38 P1 Au1 113.46(18) . . ? C37 P1 Au1 114.84(18) . . ? C21 P2 C37 105.0(2) . . ? C21 P2 C31 104.8(2) . . ? C37 P2 C31 103.3(2) . . ? C21 P2 Au2 110.51(19) . . ? C37 P2 Au2 114.53(18) . . ? C31 P2 Au2 117.54(18) . . ? C2 C1 C6 114.2(5) . . ? C2 C1 Au1 123.2(4) . . ? C6 C1 Au1 122.5(4) . . ? F1 C2 C1 119.9(5) . . ? F1 C2 C3 116.2(5) . . ? C1 C2 C3 123.9(6) . . ? F2 C3 C4 119.8(5) . . ? F2 C3 C2 121.1(5) . . ? C4 C3 C2 119.1(6) . . ? F3 C4 C3 120.2(6) . . ? F3 C4 C5 121.0(6) . . ? C3 C4 C5 118.8(5) . . ? F4 C5 C6 121.0(6) . . ? F4 C5 C4 119.0(6) . . ? C6 C5 C4 120.0(6) . . ? C5 C6 F5 117.1(5) . . ? C5 C6 C1 124.0(6) . . ? F5 C6 C1 118.9(5) . . ? C16 C11 C12 113.8(6) . . ? C16 C11 Au2 122.4(4) . . ? C12 C11 Au2 123.6(4) . . ? F6 C12 C13 116.8(5) . . ? F6 C12 C11 119.7(5) . . ? C13 C12 C11 123.5(6) . . ? F7 C13 C14 120.4(6) . . ? F7 C13 C12 120.8(6) . . ? C14 C13 C12 118.8(6) . . ? F8 C14 C15 120.9(6) . . ? F8 C14 C13 119.2(6) . . ? C15 C14 C13 119.9(6) . . ? F9 C15 C16 122.0(6) . . ? F9 C15 C14 118.7(6) . . ? C16 C15 C14 119.3(6) . . ? F10 C16 C15 116.3(5) . . ? F10 C16 C11 119.1(5) . . ? C15 C16 C11 124.6(6) . . ? C26 C21 C22 119.4(5) . . ? C26 C21 P2 118.9(5) . . ? C22 C21 P2 121.6(4) . . ? C23 C22 C21 121.0(6) . . ? C22 C23 C24 119.2(6) . . ? C25 C24 C23 120.4(6) . . ? C24 C25 C26 120.5(6) . . ? C21 C26 C25 119.5(6) . . ? C32 C31 C36 118.5(5) . . ? C32 C31 P2 124.0(4) . . ? C36 C31 P2 117.6(4) . . ? C33 C32 C31 121.7(6) . . ? C34 C33 C32 120.0(6) . . ? C33 C34 C35 119.3(5) . . ? C36 C35 C34 120.5(5) . . ? C35 C36 C31 120.0(5) . . ? P2 C37 P1 116.2(3) . . ? C39 C38 C40 111.9(5) . . ? C39 C38 P1 112.7(4) . . ? C40 C38 P1 113.9(4) . . ? C42 C41 C43 109.7(5) . . ? C42 C41 P1 110.0(4) . . ? C43 C41 P1 111.9(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C37 H37B F4 0.97 2.48 3.436(6) 169.9 2 C35 H35 F4 0.93 2.48 3.160(7) 130.5 3_556 C32 H32 F4 0.93 2.61 3.275(6) 128.7 2 C43 H43C Au2 0.96 2.93 3.852(6) 162.6 4_565 _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 28.43 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 1.649 _refine_diff_density_min -1.178 _refine_diff_density_rms 0.170 #===END data_lol37a _database_code_CSD 216499 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H52 Au2 I2 P4' _chemical_formula_weight 1280.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 12.1033(10) _cell_length_b 14.3905(12) _cell_length_c 12.1366(9) _cell_angle_alpha 90.00 _cell_angle_beta 100.2340(10) _cell_angle_gamma 90.00 _cell_volume 2080.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6579 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 28.3 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.044 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 8.708 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.408380 _exptl_absorpt_correction_T_max 0.928070 _exptl_absorpt_process_details ; SADABS; Area-Detector Absorption Correction. Bruker-AXS within SAINT+ package, v. 6.02 (1999). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13318 _diffrn_reflns_av_R_equivalents 0.1046 _diffrn_reflns_av_sigmaI/netI 0.0778 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 28.42 _reflns_number_total 4802 _reflns_number_gt 4165 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v. 5.611 (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT+ 6.02 (Bruker AXS, 1999)' _computing_data_reduction 'SAINT+ 6.02 (Bruker AXS, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, SHELXTL v. 6.10 (Bruker, 2000)' _computing_publication_material 'XCIF, SHELXTL v. 6.10 (Bruker, 2000)' _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^)+(0.0937P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4802 _refine_ls_number_parameters 212 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0639 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1501 _refine_ls_wR_factor_gt 0.1470 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 0.52554(2) 0.035447(18) 0.89134(2) 0.02302(13) Uani 1 1 d . . . P1 P 0.62997(16) 0.15852(13) 0.97606(16) 0.0219(4) Uani 1 1 d . . . P2 P 0.49745(15) -0.11849(13) 0.83357(16) 0.0211(4) Uani 1 1 d . . . I1 I 0.28030(4) 0.08965(4) 0.79148(5) 0.03155(17) Uani 1 1 d . . . C1 C 0.5914(6) 0.2751(5) 0.9272(6) 0.0239(15) Uani 1 1 d . . . C2 C 0.4941(7) 0.2906(5) 0.8548(7) 0.0282(17) Uani 1 1 d . . . H2 H 0.4509 0.2401 0.8250 0.034 Uiso 1 1 calc R . . C3 C 0.4572(7) 0.3800(6) 0.8238(7) 0.0346(19) Uani 1 1 d . . . H3 H 0.3912 0.3887 0.7724 0.042 Uiso 1 1 calc R . . C4 C 0.5182(8) 0.4551(6) 0.8691(8) 0.034(2) Uani 1 1 d . . . H4 H 0.4920 0.5150 0.8514 0.041 Uiso 1 1 calc R . . C5 C 0.6196(8) 0.4418(6) 0.9416(8) 0.037(2) Uani 1 1 d . . . H5 H 0.6631 0.4924 0.9705 0.044 Uiso 1 1 calc R . . C6 C 0.6546(7) 0.3524(6) 0.9701(7) 0.0307(17) Uani 1 1 d . . . H6 H 0.7221 0.3433 1.0191 0.037 Uiso 1 1 calc R . . C11 C 0.7781(6) 0.1463(5) 0.9692(7) 0.0272(16) Uani 1 1 d . . . C12 C 0.8616(7) 0.1900(6) 1.0452(7) 0.0331(19) Uani 1 1 d . . . H12 H 0.8426 0.2276 1.1012 0.040 Uiso 1 1 calc R . . C13 C 0.9736(7) 0.1771(7) 1.0368(8) 0.040(2) Uani 1 1 d . . . H13 H 1.0295 0.2069 1.0869 0.048 Uiso 1 1 calc R . . C14 C 1.0015(7) 0.1224(7) 0.9576(8) 0.038(2) Uani 1 1 d . . . H14 H 1.0769 0.1144 0.9536 0.045 Uiso 1 1 calc R . . C15 C 0.9225(8) 0.0782(7) 0.8828(8) 0.039(2) Uani 1 1 d . . . H15 H 0.9440 0.0398 0.8286 0.047 Uiso 1 1 calc R . . C16 C 0.8099(7) 0.0902(6) 0.8869(8) 0.0360(19) Uani 1 1 d . . . H16 H 0.7555 0.0608 0.8347 0.043 Uiso 1 1 calc R . . C17 C 0.6084(6) -0.1978(5) 0.9025(7) 0.0255(16) Uani 1 1 d . . . H17 H 0.6117 -0.1902 0.9833 0.031 Uiso 1 1 calc R . . C18 C 0.7236(8) -0.1714(7) 0.8795(10) 0.050(3) Uani 1 1 d . . . H18A H 0.7799 -0.2076 0.9264 0.075 Uiso 1 1 calc R . . H18B H 0.7368 -0.1066 0.8951 0.075 Uiso 1 1 calc R . . H18C H 0.7268 -0.1834 0.8023 0.075 Uiso 1 1 calc R . . C19 C 0.5826(8) -0.3004(5) 0.8771(8) 0.0355(19) Uani 1 1 d . . . H19A H 0.5710 -0.3102 0.7976 0.053 Uiso 1 1 calc R . . H19B H 0.5160 -0.3177 0.9049 0.053 Uiso 1 1 calc R . . H19C H 0.6445 -0.3377 0.9127 0.053 Uiso 1 1 calc R . . C20 C 0.4858(7) -0.1386(6) 0.6806(7) 0.0317(18) Uani 1 1 d . . . H20 H 0.5141 -0.2013 0.6705 0.038 Uiso 1 1 calc R . . C21 C 0.5601(9) -0.0702(8) 0.6317(8) 0.049(2) Uani 1 1 d . . . H21A H 0.5554 -0.0824 0.5533 0.073 Uiso 1 1 calc R . . H21B H 0.6365 -0.0772 0.6692 0.073 Uiso 1 1 calc R . . H21C H 0.5353 -0.0079 0.6419 0.073 Uiso 1 1 calc R . . C22 C 0.3654(8) -0.1342(7) 0.6181(7) 0.040(2) Uani 1 1 d . . . H22A H 0.3356 -0.0732 0.6255 0.060 Uiso 1 1 calc R . . H22B H 0.3207 -0.1791 0.6490 0.060 Uiso 1 1 calc R . . H22C H 0.3637 -0.1477 0.5403 0.060 Uiso 1 1 calc R . . C23 C 0.3681(6) -0.1624(5) 0.8723(6) 0.0236(15) Uani 1 1 d . . . H23A H 0.3564 -0.2260 0.8466 0.028 Uiso 1 1 calc R . . H23B H 0.3053 -0.1257 0.8346 0.028 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 0.0250(2) 0.02190(19) 0.0222(2) -0.00036(9) 0.00417(13) -0.00312(10) P1 0.0172(9) 0.0210(9) 0.0267(10) 0.0014(7) 0.0020(7) -0.0008(7) P2 0.0149(9) 0.0244(9) 0.0231(9) -0.0027(7) 0.0010(7) -0.0013(7) I1 0.0211(3) 0.0279(3) 0.0406(3) 0.0000(2) -0.0086(2) 0.00033(18) C1 0.025(4) 0.019(3) 0.027(4) 0.002(3) 0.004(3) -0.003(3) C2 0.024(4) 0.022(4) 0.035(4) 0.003(3) -0.002(3) 0.000(3) C3 0.025(4) 0.037(4) 0.037(5) 0.003(4) -0.006(3) 0.004(3) C4 0.040(5) 0.028(4) 0.034(5) 0.003(3) 0.006(4) 0.000(3) C5 0.038(5) 0.026(4) 0.045(5) -0.004(4) 0.003(4) -0.009(4) C6 0.024(4) 0.034(4) 0.032(4) -0.004(3) 0.001(3) -0.003(3) C11 0.017(4) 0.032(4) 0.034(4) 0.008(3) 0.007(3) 0.002(3) C12 0.017(4) 0.047(5) 0.034(5) 0.006(4) 0.000(3) 0.000(3) C13 0.020(4) 0.052(5) 0.047(6) 0.008(4) 0.006(4) -0.004(4) C14 0.021(4) 0.053(5) 0.041(5) 0.016(4) 0.010(3) 0.003(4) C15 0.039(5) 0.049(5) 0.033(5) 0.011(4) 0.016(4) 0.003(4) C16 0.026(4) 0.042(5) 0.042(5) 0.005(4) 0.013(4) 0.001(3) C17 0.021(4) 0.018(3) 0.037(4) -0.006(3) 0.003(3) 0.002(3) C18 0.023(5) 0.044(5) 0.081(8) 0.022(5) 0.002(5) 0.005(4) C19 0.038(5) 0.021(4) 0.050(5) -0.002(3) 0.012(4) 0.005(3) C20 0.034(5) 0.036(4) 0.025(4) -0.006(3) 0.004(3) 0.002(3) C21 0.047(6) 0.074(7) 0.027(5) 0.004(5) 0.012(4) -0.015(5) C22 0.038(5) 0.057(6) 0.022(4) -0.008(4) -0.001(3) -0.001(4) C23 0.024(4) 0.025(4) 0.020(4) -0.001(3) 0.001(3) -0.002(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 2.3086(19) . y Au1 P2 2.3302(19) . y Au1 Au1 2.9931(6) 3_657 y Au1 I1 3.0999(6) . y P1 C1 1.812(7) . ? P1 C11 1.818(8) . ? P1 C23 1.837(7) 3_657 ? P2 C23 1.826(8) . ? P2 C17 1.846(8) . ? P2 C20 1.859(8) . ? C1 C2 1.357(11) . ? C1 C6 1.398(10) . ? C2 C3 1.392(11) . ? C3 C4 1.368(12) . ? C4 C5 1.390(12) . ? C5 C6 1.380(12) . ? C11 C16 1.390(12) . ? C11 C12 1.392(11) . ? C12 C13 1.389(12) . ? C13 C14 1.331(14) . ? C14 C15 1.355(14) . ? C15 C16 1.384(13) . ? C17 C18 1.518(12) . ? C17 C19 1.529(11) . ? C20 C22 1.520(12) . ? C20 C21 1.523(13) . ? C23 P1 1.837(7) 3_657 ? 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 154.47(7) . . y P1 Au1 Au1 92.95(5) . 3_657 ? P2 Au1 Au1 84.21(5) . 3_657 ? P1 Au1 I1 113.05(5) . . y P2 Au1 I1 92.48(5) . . y Au1 Au1 I1 95.563(18) 3_657 . y C1 P1 C11 105.9(4) . . ? C1 P1 C23 104.9(4) . 3_657 ? C11 P1 C23 102.2(4) . 3_657 ? C1 P1 Au1 118.4(2) . . ? C11 P1 Au1 111.8(3) . . ? C23 P1 Au1 112.2(2) 3_657 . ? C23 P2 C17 104.9(4) . . ? C23 P2 C20 106.7(4) . . ? C17 P2 C20 106.1(4) . . ? C23 P2 Au1 109.7(3) . . ? C17 P2 Au1 113.3(2) . . ? C20 P2 Au1 115.4(3) . . ? C2 C1 C6 117.7(7) . . ? C2 C1 P1 120.5(5) . . ? C6 C1 P1 121.5(6) . . ? C1 C2 C3 121.8(7) . . ? C4 C3 C2 119.8(8) . . ? C3 C4 C5 119.9(8) . . ? C6 C5 C4 119.0(8) . . ? C5 C6 C1 121.7(7) . . ? C16 C11 C12 118.5(8) . . ? C16 C11 P1 119.4(6) . . ? C12 C11 P1 122.1(7) . . ? C13 C12 C11 119.6(9) . . ? C14 C13 C12 120.5(9) . . ? C13 C14 C15 121.5(9) . . ? C14 C15 C16 119.9(9) . . ? C15 C16 C11 119.9(9) . . ? C18 C17 C19 111.5(7) . . ? C18 C17 P2 112.3(6) . . ? C19 C17 P2 113.5(6) . . ? C22 C20 C21 111.0(8) . . ? C22 C20 P2 112.8(6) . . ? C21 C20 P2 110.1(6) . . ? P2 C23 P1 112.9(4) . 3_657 ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 28.42 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 3.270 _refine_diff_density_min -2.761 _refine_diff_density_rms 0.341 #===END data_lol44as _database_code_CSD 216500 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H60 Au2 Cl4 F6 O6 P4 S2' _chemical_formula_weight 1522.65 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 10.0765(9) _cell_length_b 11.6880(10) _cell_length_c 13.2223(12) _cell_angle_alpha 70.5620(10) _cell_angle_beta 69.619(2) _cell_angle_gamma 89.378(2) _cell_volume 1366.8(2) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3288 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 27 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.850 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 5.814 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.829702 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ; SADABS; Area-Detector Absorption Correction. Bruker-AXS within SAINT+ package, v. 6.02 (1999). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9037 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0803 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 28.49 _reflns_number_total 6053 _reflns_number_gt 5040 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v. 5.611 (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT+ 6.02 (Bruker AXS, 1999)' _computing_data_reduction 'SAINT+ 6.02 (Bruker AXS, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, SHELXTL v. 6.10 (Bruker, 2000)' _computing_publication_material 'XCIF, SHELXTL v. 6.10 (Bruker, 2000)' _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^)+(0.0253P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6053 _refine_ls_number_parameters 311 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0710 _refine_ls_wR_factor_gt 0.0692 _refine_ls_goodness_of_fit_ref 0.896 _refine_ls_restrained_S_all 0.896 _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 0.97743(2) 0.548941(19) 0.594794(19) 0.01622(7) Uani 1 1 d . . . P1 P 0.74282(14) 0.46455(12) 0.68401(12) 0.0166(3) Uani 1 1 d . . . P2 P 1.20077(15) 0.65799(12) 0.49726(12) 0.0163(3) Uani 1 1 d . . . C1 C 0.6348(5) 0.5811(5) 0.7214(4) 0.0168(11) Uani 1 1 d . . . C2 C 0.5490(5) 0.5664(5) 0.8326(5) 0.0196(12) Uani 1 1 d . . . H2 H 0.5403 0.4932 0.8923 0.024 Uiso 1 1 calc R . . C3 C 0.4755(6) 0.6619(5) 0.8551(5) 0.0221(13) Uani 1 1 d . . . H3 H 0.4166 0.6525 0.9301 0.027 Uiso 1 1 calc R . . C4 C 0.4898(6) 0.7705(5) 0.7668(5) 0.0243(13) Uani 1 1 d . . . H4 H 0.4409 0.8343 0.7824 0.029 Uiso 1 1 calc R . . C5 C 0.5761(6) 0.7851(5) 0.6553(5) 0.0238(13) Uani 1 1 d . . . H5 H 0.5857 0.8587 0.5958 0.029 Uiso 1 1 calc R . . C6 C 0.6480(5) 0.6904(5) 0.6323(5) 0.0201(12) Uani 1 1 d . . . H6 H 0.7054 0.6996 0.5571 0.024 Uiso 1 1 calc R . . C11 C 0.6963(6) 0.3305(4) 0.8118(5) 0.0186(12) Uani 1 1 d . . . C12 C 0.5588(6) 0.2694(5) 0.8675(5) 0.0237(13) Uani 1 1 d . . . H12 H 0.4877 0.2997 0.8396 0.028 Uiso 1 1 calc R . . C13 C 0.5265(7) 0.1659(5) 0.9622(5) 0.0318(15) Uani 1 1 d . . . H13 H 0.4336 0.1271 1.0000 0.038 Uiso 1 1 calc R . . C14 C 0.6328(7) 0.1190(5) 1.0017(5) 0.0357(16) Uani 1 1 d . . . H14 H 0.6108 0.0479 1.0659 0.043 Uiso 1 1 calc R . . C15 C 0.7698(7) 0.1753(5) 0.9481(5) 0.0325(15) Uani 1 1 d . . . H15 H 0.8405 0.1421 0.9752 0.039 Uiso 1 1 calc R . . C16 C 0.8027(6) 0.2821(5) 0.8533(5) 0.0255(13) Uani 1 1 d . . . H16 H 0.8954 0.3216 0.8172 0.031 Uiso 1 1 calc R . . C17 C 1.1960(6) 0.8070(5) 0.3932(5) 0.0204(12) Uani 1 1 d . . . H17 H 1.1801 0.7895 0.3305 0.024 Uiso 1 1 calc R . . C18 C 1.0689(6) 0.8716(5) 0.4431(5) 0.0270(14) Uani 1 1 d . . . H18A H 1.0817 0.8948 0.5026 0.041 Uiso 1 1 calc R . . H18B H 0.9824 0.8170 0.4749 0.041 Uiso 1 1 calc R . . H18C H 1.0634 0.9431 0.3830 0.041 Uiso 1 1 calc R . . C19 C 1.3372(6) 0.8902(5) 0.3377(5) 0.0287(14) Uani 1 1 d . . . H19A H 1.3308 0.9628 0.2790 0.043 Uiso 1 1 calc R . . H19B H 1.4126 0.8480 0.3038 0.043 Uiso 1 1 calc R . . H19C H 1.3570 0.9120 0.3953 0.043 Uiso 1 1 calc R . . C20 C 1.3211(5) 0.5757(5) 0.4139(5) 0.0187(12) Uani 1 1 d . . . H20A H 1.4124 0.6258 0.3696 0.022 Uiso 1 1 calc R . . H20B H 1.3367 0.5014 0.4671 0.022 Uiso 1 1 calc R . . C21 C 1.2881(6) 0.6809(5) 0.5899(5) 0.0197(12) Uani 1 1 d . . . H21 H 1.3846 0.7224 0.5415 0.024 Uiso 1 1 calc R . . C22 C 1.2076(6) 0.7602(5) 0.6557(5) 0.0278(14) Uani 1 1 d . . . H22A H 1.1077 0.7313 0.6887 0.042 Uiso 1 1 calc R . . H22B H 1.2223 0.8433 0.6040 0.042 Uiso 1 1 calc R . . H22C H 1.2418 0.7563 0.7159 0.042 Uiso 1 1 calc R . . C23 C 1.2993(6) 0.5579(5) 0.6731(5) 0.0266(14) Uani 1 1 d . . . H23A H 1.3376 0.5707 0.7261 0.040 Uiso 1 1 calc R . . H23B H 1.3610 0.5131 0.6306 0.040 Uiso 1 1 calc R . . H23C H 1.2063 0.5122 0.7151 0.040 Uiso 1 1 calc R . . C24 C 0.8944(7) 0.7550(6) 0.9207(6) 0.0412(17) Uani 1 1 d . . . H24A H 0.9970 0.7571 0.8872 0.049 Uiso 1 1 calc R . . H24B H 0.8748 0.8072 0.9667 0.049 Uiso 1 1 calc R . . Cl2 Cl 0.82687(19) 0.81364(16) 0.80811(16) 0.0485(5) Uani 1 1 d . . . Cl3 Cl 0.87469(19) 0.52336(15) 0.92061(16) 0.0476(5) Uani 1 1 d . . . C25 C 0.8312(8) 0.6277(6) 0.9970(6) 0.0454(18) Uani 1 1 d . . . H25A H 0.7284 0.6250 1.0298 0.055 Uiso 1 1 calc R . . H25B H 0.8661 0.6027 1.0600 0.055 Uiso 1 1 calc R . . C26 C 0.8058(7) 0.9166(5) 0.2712(6) 0.0322(15) Uani 1 1 d . . . S1 S 0.77419(16) 0.75604(13) 0.29094(13) 0.0253(3) Uani 1 1 d . . . F1 F 0.7743(4) 0.9317(3) 0.3718(3) 0.0428(10) Uani 1 1 d . . . F2 F 0.7271(5) 0.9848(3) 0.2186(4) 0.0634(13) Uani 1 1 d . . . F3 F 0.9408(4) 0.9619(3) 0.2096(4) 0.0596(12) Uani 1 1 d . . . O1 O 0.6251(4) 0.7251(4) 0.3592(4) 0.0404(12) Uani 1 1 d . . . O2 O 0.8634(4) 0.6990(3) 0.3524(4) 0.0340(10) Uani 1 1 d . . . O3 O 0.8172(6) 0.7574(4) 0.1757(4) 0.0572(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01674(12) 0.01546(11) 0.01994(11) -0.00849(8) -0.00862(9) 0.00227(8) P1 0.0174(8) 0.0142(7) 0.0205(8) -0.0068(6) -0.0088(6) 0.0036(6) P2 0.0179(8) 0.0142(7) 0.0214(8) -0.0090(6) -0.0100(6) 0.0033(6) C1 0.018(3) 0.017(3) 0.020(3) -0.009(2) -0.010(2) 0.002(2) C2 0.021(3) 0.017(3) 0.023(3) -0.007(2) -0.011(3) 0.004(2) C3 0.022(3) 0.030(3) 0.025(3) -0.020(3) -0.011(3) 0.008(2) C4 0.030(4) 0.024(3) 0.029(3) -0.016(3) -0.016(3) 0.012(3) C5 0.028(3) 0.019(3) 0.031(3) -0.009(3) -0.018(3) 0.008(2) C6 0.016(3) 0.021(3) 0.026(3) -0.011(3) -0.009(3) 0.003(2) C11 0.027(3) 0.009(3) 0.020(3) -0.006(2) -0.009(3) 0.002(2) C12 0.030(4) 0.018(3) 0.026(3) -0.013(3) -0.009(3) 0.004(2) C13 0.042(4) 0.020(3) 0.026(3) -0.007(3) -0.005(3) -0.004(3) C14 0.067(5) 0.014(3) 0.024(3) -0.005(3) -0.016(3) 0.000(3) C15 0.048(4) 0.032(4) 0.029(4) -0.015(3) -0.024(3) 0.017(3) C16 0.029(4) 0.022(3) 0.027(3) -0.012(3) -0.009(3) 0.003(3) C17 0.028(3) 0.016(3) 0.022(3) -0.008(2) -0.012(3) 0.005(2) C18 0.033(4) 0.020(3) 0.039(4) -0.014(3) -0.023(3) 0.008(3) C19 0.034(4) 0.017(3) 0.032(4) -0.008(3) -0.008(3) 0.004(3) C20 0.017(3) 0.014(3) 0.028(3) -0.009(2) -0.011(3) 0.005(2) C21 0.024(3) 0.019(3) 0.019(3) -0.009(2) -0.010(3) 0.002(2) C22 0.026(3) 0.034(4) 0.035(4) -0.022(3) -0.017(3) 0.012(3) C23 0.030(4) 0.030(3) 0.029(3) -0.014(3) -0.018(3) 0.003(3) C24 0.051(5) 0.038(4) 0.035(4) -0.012(3) -0.017(3) 0.000(3) Cl2 0.0516(12) 0.0442(11) 0.0509(11) -0.0103(9) -0.0264(9) 0.0088(8) Cl3 0.0574(12) 0.0380(10) 0.0568(12) -0.0241(9) -0.0247(10) 0.0094(8) C25 0.063(5) 0.030(4) 0.041(4) -0.017(3) -0.011(4) 0.001(3) C26 0.047(4) 0.020(3) 0.034(4) -0.006(3) -0.023(3) 0.004(3) S1 0.0322(9) 0.0192(7) 0.0277(8) -0.0101(7) -0.0131(7) 0.0025(6) F1 0.064(3) 0.027(2) 0.049(2) -0.0218(19) -0.028(2) 0.0081(18) F2 0.109(4) 0.026(2) 0.080(3) -0.012(2) -0.071(3) 0.026(2) F3 0.062(3) 0.035(2) 0.059(3) -0.008(2) -0.002(2) -0.023(2) O1 0.024(2) 0.034(3) 0.068(3) -0.024(2) -0.017(2) 0.0028(19) O2 0.033(3) 0.024(2) 0.050(3) -0.013(2) -0.021(2) 0.0078(19) O3 0.105(4) 0.033(3) 0.037(3) -0.015(2) -0.028(3) 0.003(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 2.2993(14) . ? Au1 P2 2.3020(14) . ? Au1 Au1 2.9838(5) 2_766 ? Au1 O2 3.284(4) 2_766 ? P1 C11 1.798(5) . ? P1 C20 1.818(5) 2_766 ? P1 C1 1.823(5) . ? P2 C21 1.823(5) . ? P2 C20 1.833(5) . ? P2 C17 1.838(5) . ? C1 C2 1.375(7) . ? C1 C6 1.389(7) . ? C2 C3 1.391(7) . ? C3 C4 1.377(7) . ? C4 C5 1.379(8) . ? C5 C6 1.377(7) . ? C11 C12 1.391(7) . ? C11 C16 1.400(7) . ? C12 C13 1.361(7) . ? C13 C14 1.380(8) . ? C14 C15 1.367(8) . ? C15 C16 1.385(8) . ? C17 C19 1.528(7) . ? C17 C18 1.539(7) . ? C20 P1 1.818(5) 2_766 ? C21 C22 1.517(7) . ? C21 C23 1.524(7) . ? C24 C25 1.487(8) . ? C24 Cl2 1.779(6) . ? Cl3 C25 1.789(6) . ? C26 F2 1.322(6) . ? C26 F3 1.323(7) . ? C26 F1 1.328(7) . ? C26 S1 1.822(6) . ? S1 O3 1.426(5) . ? S1 O2 1.432(4) . ? S1 O1 1.433(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 P2 172.32(5) . . ? P1 Au1 Au1 92.13(4) . 2_766 ? P2 Au1 Au1 89.70(4) . 2_766 ? P1 Au1 O2 100.18(8) . 2_766 ? P2 Au1 O2 87.47(8) . 2_766 ? Au1 Au1 O2 71.42(7) 2_766 2_766 ? C11 P1 C20 105.9(2) . 2_766 ? C11 P1 C1 107.6(2) . . ? C20 P1 C1 105.2(2) 2_766 . ? C11 P1 Au1 117.97(18) . . ? C20 P1 Au1 111.33(18) 2_766 . ? C1 P1 Au1 108.17(17) . . ? C21 P2 C20 104.9(2) . . ? C21 P2 C17 109.2(2) . . ? C20 P2 C17 106.4(2) . . ? C21 P2 Au1 114.35(19) . . ? C20 P2 Au1 110.17(17) . . ? C17 P2 Au1 111.36(17) . . ? C2 C1 C6 120.3(5) . . ? C2 C1 P1 122.7(4) . . ? C6 C1 P1 116.9(4) . . ? C1 C2 C3 119.4(5) . . ? C4 C3 C2 120.2(5) . . ? C3 C4 C5 120.3(5) . . ? C6 C5 C4 119.7(5) . . ? C5 C6 C1 120.1(5) . . ? C12 C11 C16 118.8(5) . . ? C12 C11 P1 121.8(4) . . ? C16 C11 P1 119.3(4) . . ? C13 C12 C11 121.0(5) . . ? C12 C13 C14 119.5(6) . . ? C15 C14 C13 121.2(6) . . ? C14 C15 C16 119.6(5) . . ? C15 C16 C11 119.9(5) . . ? C19 C17 C18 112.3(4) . . ? C19 C17 P2 113.5(4) . . ? C18 C17 P2 112.5(4) . . ? P1 C20 P2 114.6(3) 2_766 . ? C22 C21 C23 110.5(5) . . ? C22 C21 P2 110.8(4) . . ? C23 C21 P2 109.9(3) . . ? C25 C24 Cl2 112.8(5) . . ? C24 C25 Cl3 111.8(5) . . ? F2 C26 F3 107.6(5) . . ? F2 C26 F1 107.1(5) . . ? F3 C26 F1 107.0(5) . . ? F2 C26 S1 112.0(4) . . ? F3 C26 S1 111.9(4) . . ? F1 C26 S1 111.0(4) . . ? O3 S1 O2 115.3(3) . . ? O3 S1 O1 116.5(3) . . ? O2 S1 O1 113.2(3) . . ? O3 S1 C26 103.1(3) . . ? O2 S1 C26 103.0(3) . . ? O1 S1 C26 103.1(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C24 H24B O3 0.97 2.48 3.195(8) 130.7 1_556 C20 H20A O1 0.97 2.39 3.269(6) 150.9 1_655 _diffrn_measured_fraction_theta_max 0.872 _diffrn_reflns_theta_full 28.49 _diffrn_measured_fraction_theta_full 0.872 _refine_diff_density_max 2.313 _refine_diff_density_min -1.374 _refine_diff_density_rms 0.164 #========================================END