Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Puddephatt, Richard' _publ_contact_author_name 'Dr Richard Puddephatt' _publ_contact_author_address ; Chemistry University of Western Ontario Richmond Street London Ontario N6A 5B7 CANADA ; _publ_contact_author_email 'PUDD@UWO.CA' _publ_section_title ; Interpenetrating Digold(I) Diacetylide Macrocycles ; data_complex3g _database_code_CSD 181890 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H38 Au2 O4 P2' _chemical_formula_weight 1110.64 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 14.7711(5) _cell_length_b 15.2895(5) _cell_length_c 18.3486(8) _cell_angle_alpha 90.00 _cell_angle_beta 107.0996(17) _cell_angle_gamma 90.00 _cell_volume 3960.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'hexagonal plates' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.863 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2136 _exptl_absorpt_coefficient_mu 7.524 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.1622 _exptl_absorpt_correction_T_max 0.5200 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi/omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35062 _diffrn_reflns_av_R_equivalents 0.081 _diffrn_reflns_av_sigmaI/netI 0.0619 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9050 _reflns_number_gt 6633 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _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^)+(0.0619P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9050 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0639 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1081 _refine_ls_wR_factor_gt 0.0993 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.981 _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 1.055017(16) 0.649413(14) 0.328681(14) 0.03922(8) Uani 1 1 d . . . Au2 Au 0.945182(15) 0.489111(15) 0.347800(13) 0.03790(8) Uani 1 1 d . . . P2 P 1.07725(10) 0.40615(10) 0.39518(9) 0.0376(3) Uani 1 1 d . . . P1 P 1.03948(11) 0.72378(9) 0.43160(9) 0.0365(3) Uani 1 1 d . . . O1 O 0.6344(3) 0.6182(3) 0.7199(3) 0.0640(13) Uani 1 1 d . . . O2 O 0.5974(3) 0.5898(4) 0.3278(3) 0.0690(14) Uani 1 1 d . . . C8 C 0.8204(4) 0.5538(4) 0.3105(3) 0.0396(13) Uani 1 1 d . . . C10 C 1.0097(4) 0.6586(4) 0.5030(3) 0.0390(14) Uani 1 1 d . . . H10A H 1.0551 0.6158 0.5273 0.047 Uiso 1 1 calc R . . C9 C 1.0674(4) 0.3374(4) 0.4739(4) 0.0426(14) Uani 1 1 d . . . H9A H 1.1174 0.2987 0.4983 0.051 Uiso 1 1 calc R . . C61 C 1.1480(4) 0.7749(3) 0.4890(4) 0.0399(14) Uani 1 1 d . . . C14 C 0.5826(5) 0.6858(5) 0.5024(4) 0.0538(17) Uani 1 1 d . . . C31 C 1.1851(4) 0.4681(4) 0.4344(4) 0.0379(13) Uani 1 1 d . . . C36 C 1.2433(4) 0.4868(4) 0.3905(4) 0.0488(16) Uani 1 1 d . . . H36A H 1.2318 0.4614 0.3414 0.059 Uiso 1 1 calc R . . C7 C 0.7430(5) 0.5810(4) 0.2940(4) 0.0547(17) Uani 1 1 d . . . C71 C 1.0655(4) 0.5911(4) 0.2327(4) 0.0417(14) Uani 1 1 d . . . C51 C 0.9473(4) 0.8076(4) 0.4021(4) 0.0435(15) Uani 1 1 d . . . C32 C 1.2022(5) 0.5041(4) 0.5050(4) 0.0488(16) Uani 1 1 d . . . H32A H 1.1619 0.4903 0.5353 0.059 Uiso 1 1 calc R . . C21 C 1.1013(5) 0.3315(4) 0.3256(4) 0.0459(15) Uani 1 1 d . . . C63 C 1.3027(5) 0.8325(5) 0.4981(5) 0.066(2) Uani 1 1 d . . . H63A H 1.3514 0.8451 0.4754 0.079 Uiso 1 1 calc R . . C42 C 0.5796(5) 0.5369(6) 0.8120(5) 0.071(2) Uani 1 1 d . . . H42A H 0.5157 0.5535 0.7885 0.085 Uiso 1 1 calc R . . C56 C 0.8820(4) 0.8013(4) 0.3328(4) 0.0509(16) Uani 1 1 d . . . H56A H 0.8834 0.7525 0.3011 0.061 Uiso 1 1 calc R . . C70 C 1.0671(4) 0.5537(5) 0.1778(4) 0.0515(16) Uani 1 1 d . . . C15 C 0.5767(4) 0.6279(5) 0.4440(4) 0.0551(18) Uani 1 1 d . . . H15A H 0.5482 0.5723 0.4441 0.066 Uiso 1 1 calc R . . C65 C 1.2499(5) 0.8281(4) 0.6080(4) 0.0591(19) Uani 1 1 d . . . H65A H 1.2616 0.8384 0.6611 0.071 Uiso 1 1 calc R . . C52 C 0.9443(4) 0.8784(4) 0.4485(4) 0.0458(15) Uani 1 1 d . . . H52A H 0.9894 0.8835 0.4974 0.055 Uiso 1 1 calc R . . C35 C 1.3182(5) 0.5425(5) 0.4183(5) 0.065(2) Uani 1 1 d . . . H35A H 1.3596 0.5542 0.3885 0.078 Uiso 1 1 calc R . . C26 C 1.0504(5) 0.3365(5) 0.2505(4) 0.0605(19) Uani 1 1 d . . . H26A H 0.9994 0.3768 0.2343 0.073 Uiso 1 1 calc R . . C55 C 0.8141(5) 0.8642(5) 0.3081(5) 0.062(2) Uani 1 1 d . . . H55A H 0.7695 0.8595 0.2590 0.075 Uiso 1 1 calc R . . C34 C 1.3347(5) 0.5817(5) 0.4882(6) 0.075(3) Uani 1 1 d . . . H34A H 1.3848 0.6227 0.5054 0.090 Uiso 1 1 calc R . . C66 C 1.1649(5) 0.7911(4) 0.5660(4) 0.0517(16) Uani 1 1 d . . . H66A H 1.1182 0.7768 0.5902 0.062 Uiso 1 1 calc R . . C62 C 1.2177(5) 0.7968(4) 0.4549(4) 0.0573(18) Uani 1 1 d . . . H62A H 1.2069 0.7871 0.4018 0.069 Uiso 1 1 calc R . . C54 C 0.8102(5) 0.9336(5) 0.3539(5) 0.061(2) Uani 1 1 d . . . H54A H 0.7620 0.9764 0.3372 0.073 Uiso 1 1 calc R . . C25 C 1.0736(6) 0.2821(6) 0.1975(5) 0.076(2) Uani 1 1 d . . . H25A H 1.0382 0.2860 0.1452 0.091 Uiso 1 1 calc R . . C41 C 0.6499(5) 0.5655(4) 0.7834(4) 0.0516(16) Uani 1 1 d . . . C64 C 1.3160(5) 0.8495(4) 0.5738(6) 0.067(2) Uani 1 1 d . . . H64A H 1.3730 0.8769 0.6027 0.080 Uiso 1 1 calc R . . C53 C 0.8757(5) 0.9412(4) 0.4235(4) 0.0557(18) Uani 1 1 d . . . H53A H 0.8739 0.9902 0.4549 0.067 Uiso 1 1 calc R . . C6 C 0.6421(5) 0.6061(6) 0.2678(5) 0.069(2) Uani 1 1 d . . . H6A H 0.6365 0.6689 0.2540 0.083 Uiso 1 1 calc R . . H6B H 0.6092 0.5719 0.2218 0.083 Uiso 1 1 calc R . . C43 C 0.6023(6) 0.4848(6) 0.8740(6) 0.085(3) Uani 1 1 d . . . H43A H 0.5533 0.4643 0.8935 0.102 Uiso 1 1 calc R . . C44 C 0.6952(7) 0.4602(6) 0.9101(5) 0.085(3) Uani 1 1 d . . . H44A H 0.7097 0.4230 0.9535 0.102 Uiso 1 1 calc R . . C13 C 0.6194(6) 0.7691(5) 0.5002(5) 0.072(2) Uani 1 1 d . . . H13A H 0.6181 0.8119 0.5374 0.086 Uiso 1 1 calc R . . C16 C 0.6129(5) 0.6513(5) 0.3845(4) 0.0549(18) Uani 1 1 d . . . C33 C 1.2780(5) 0.5609(5) 0.5333(5) 0.065(2) Uani 1 1 d . . . H33A H 1.2904 0.5850 0.5829 0.078 Uiso 1 1 calc R . . C12 C 0.6582(6) 0.7874(6) 0.4415(5) 0.084(3) Uani 1 1 d . . . H12A H 0.6877 0.8426 0.4411 0.101 Uiso 1 1 calc R . . C24 C 1.1436(7) 0.2257(5) 0.2187(6) 0.081(3) Uani 1 1 d . . . H24A H 1.1572 0.1886 0.1817 0.097 Uiso 1 1 calc R . . C23 C 1.1971(7) 0.2195(5) 0.2930(6) 0.084(3) Uani 1 1 d . . . H23A H 1.2490 0.1800 0.3072 0.101 Uiso 1 1 calc R . . C22 C 1.1751(6) 0.2716(5) 0.3486(5) 0.068(2) Uani 1 1 d . . . H22A H 1.2099 0.2660 0.4009 0.081 Uiso 1 1 calc R . . C11 C 0.6557(6) 0.7294(6) 0.3840(5) 0.075(2) Uani 1 1 d . . . H11A H 0.6833 0.7436 0.3448 0.090 Uiso 1 1 calc R . . O3 O 0.5516(4) 0.6542(3) 0.5605(3) 0.0628(13) Uani 1 1 d . . . O4 O 0.8564(4) 0.4681(4) 0.9217(3) 0.0723(15) Uani 1 1 d . . . C46 C 0.7433(5) 0.5426(5) 0.8176(4) 0.0574(18) Uani 1 1 d . . . H46A H 0.7912 0.5627 0.7967 0.069 Uiso 1 1 calc R . . C45 C 0.7671(6) 0.4913(5) 0.8813(4) 0.062(2) Uani 1 1 d . . . C74 C 1.0679(6) 0.5078(5) 0.1082(4) 0.065(2) Uani 1 1 d . . . H74A H 1.0718 0.4442 0.1186 0.078 Uiso 1 1 calc R . . H74B H 1.0070 0.5190 0.0686 0.078 Uiso 1 1 calc R . . C72 C 0.5431(5) 0.6517(5) 0.6870(5) 0.067(2) Uani 1 1 d . . . H72A H 0.5218 0.6850 0.7252 0.080 Uiso 1 1 calc R . . H72B H 0.4977 0.6035 0.6673 0.080 Uiso 1 1 calc R . . C73 C 0.5494(5) 0.7105(5) 0.6231(5) 0.069(2) Uani 1 1 d . . . H73A H 0.4939 0.7499 0.6078 0.083 Uiso 1 1 calc R . . H73B H 0.6076 0.7466 0.6391 0.083 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 0.04636(14) 0.04019(14) 0.03416(15) -0.00015(9) 0.01656(11) 0.00044(9) Au2 0.03784(13) 0.04174(13) 0.03389(15) 0.00108(9) 0.01019(10) -0.00050(9) P2 0.0391(8) 0.0400(8) 0.0356(9) 0.0031(7) 0.0141(7) 0.0015(6) P1 0.0436(8) 0.0357(7) 0.0330(9) 0.0011(6) 0.0154(7) -0.0010(6) O1 0.053(3) 0.083(3) 0.061(4) 0.007(3) 0.024(3) 0.007(3) O2 0.058(3) 0.095(4) 0.059(4) -0.012(3) 0.025(3) 0.002(3) C8 0.040(3) 0.045(3) 0.033(4) -0.001(3) 0.009(3) 0.004(3) C10 0.045(3) 0.038(3) 0.032(4) 0.000(2) 0.009(3) 0.000(2) C9 0.049(3) 0.042(3) 0.037(4) 0.007(3) 0.014(3) 0.003(3) C61 0.042(3) 0.037(3) 0.040(4) -0.002(3) 0.010(3) 0.002(2) C14 0.045(4) 0.065(4) 0.051(5) 0.006(4) 0.014(3) 0.003(3) C31 0.036(3) 0.036(3) 0.042(4) 0.004(3) 0.012(3) 0.004(2) C36 0.043(3) 0.063(4) 0.037(4) 0.011(3) 0.007(3) -0.004(3) C7 0.056(4) 0.065(4) 0.045(5) 0.001(3) 0.018(3) 0.008(3) C71 0.054(4) 0.039(3) 0.031(4) 0.001(3) 0.011(3) 0.005(3) C51 0.044(3) 0.043(3) 0.051(4) 0.006(3) 0.024(3) -0.005(3) C32 0.053(4) 0.045(3) 0.055(5) -0.003(3) 0.026(4) 0.005(3) C21 0.056(4) 0.042(3) 0.043(4) -0.003(3) 0.020(3) -0.003(3) C63 0.050(4) 0.065(4) 0.082(7) 0.017(4) 0.019(4) -0.011(3) C42 0.057(4) 0.092(6) 0.077(6) -0.006(5) 0.041(4) -0.002(4) C56 0.049(4) 0.059(4) 0.042(4) 0.003(3) 0.010(3) 0.000(3) C70 0.045(3) 0.069(4) 0.039(4) 0.004(3) 0.011(3) 0.015(3) C15 0.045(4) 0.060(4) 0.059(5) 0.007(4) 0.014(3) 0.011(3) C65 0.059(4) 0.059(4) 0.050(5) -0.011(3) 0.001(4) 0.006(3) C52 0.054(4) 0.043(3) 0.041(4) -0.002(3) 0.016(3) 0.001(3) C35 0.052(4) 0.061(4) 0.084(7) 0.019(4) 0.021(4) -0.010(3) C26 0.067(4) 0.070(5) 0.049(5) -0.014(4) 0.026(4) -0.002(4) C55 0.059(4) 0.063(4) 0.063(6) 0.009(4) 0.015(4) -0.001(4) C34 0.053(4) 0.049(4) 0.109(8) -0.011(5) 0.004(5) -0.014(3) C66 0.050(4) 0.058(4) 0.047(4) -0.006(3) 0.013(3) -0.001(3) C62 0.061(4) 0.061(4) 0.055(5) 0.006(3) 0.025(4) -0.009(3) C54 0.052(4) 0.056(4) 0.076(6) 0.025(4) 0.023(4) 0.015(3) C25 0.098(6) 0.078(5) 0.055(6) -0.025(4) 0.027(5) -0.016(5) C41 0.063(4) 0.057(4) 0.040(4) -0.004(3) 0.024(3) 0.000(3) C64 0.047(4) 0.055(4) 0.088(7) -0.008(4) 0.004(4) -0.003(3) C53 0.067(4) 0.044(3) 0.066(5) 0.004(3) 0.033(4) 0.011(3) C6 0.053(4) 0.105(6) 0.049(5) 0.002(4) 0.014(4) 0.012(4) C43 0.082(6) 0.103(7) 0.093(8) 0.034(6) 0.062(6) 0.015(5) C44 0.112(7) 0.083(6) 0.082(7) 0.018(5) 0.064(6) 0.013(5) C13 0.076(5) 0.065(5) 0.069(6) -0.002(4) 0.013(4) 0.002(4) C16 0.044(4) 0.066(4) 0.052(5) -0.001(4) 0.010(3) 0.005(3) C33 0.065(5) 0.060(4) 0.057(5) -0.020(4) -0.004(4) 0.005(4) C12 0.089(6) 0.091(6) 0.064(6) 0.009(5) 0.010(5) -0.037(5) C24 0.102(7) 0.062(5) 0.081(7) -0.039(5) 0.030(6) -0.008(5) C23 0.098(6) 0.065(5) 0.093(8) -0.018(5) 0.033(6) 0.028(4) C22 0.086(5) 0.065(5) 0.051(5) -0.004(4) 0.018(4) 0.022(4) C11 0.075(5) 0.091(6) 0.057(6) 0.005(5) 0.017(4) -0.023(4) O3 0.068(3) 0.071(3) 0.051(3) -0.003(2) 0.021(3) 0.001(2) O4 0.078(4) 0.102(4) 0.042(3) 0.007(3) 0.026(3) 0.038(3) C46 0.060(4) 0.068(4) 0.051(5) -0.001(4) 0.027(4) 0.005(3) C45 0.084(5) 0.070(5) 0.039(4) 0.002(3) 0.029(4) 0.016(4) C74 0.069(5) 0.090(6) 0.035(4) -0.008(4) 0.013(4) 0.015(4) C72 0.061(4) 0.084(6) 0.056(5) 0.008(4) 0.018(4) 0.025(4) C73 0.061(4) 0.078(5) 0.070(6) -0.009(4) 0.020(4) 0.020(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 C71 2.020(6) . ? Au1 P1 2.2729(15) . ? Au1 Au2 3.0161(3) . ? Au2 C8 2.026(6) . ? Au2 P2 2.2744(15) . ? P2 C31 1.811(6) . ? P2 C21 1.823(6) . ? P2 C9 1.827(6) . ? P1 C10 1.800(6) . ? P1 C61 1.816(6) . ? P1 C51 1.832(6) . ? O1 C41 1.380(8) . ? O1 C72 1.401(8) . ? O2 C16 1.371(8) . ? O2 C6 1.462(9) . ? C8 C7 1.170(8) . ? C10 C9 1.328(8) 3_766 ? C9 C10 1.328(8) 3_766 ? C61 C66 1.383(9) . ? C61 C62 1.394(9) . ? C14 O3 1.367(8) . ? C14 C15 1.373(10) . ? C14 C13 1.390(10) . ? C31 C32 1.361(9) . ? C31 C36 1.369(8) . ? C36 C35 1.371(9) . ? C7 C6 1.476(9) . ? C71 C70 1.166(9) . ? C51 C56 1.355(9) . ? C51 C52 1.385(9) . ? C32 C33 1.391(9) . ? C21 C26 1.364(10) . ? C21 C22 1.391(9) . ? C63 C64 1.369(11) . ? C63 C62 1.385(10) . ? C42 C43 1.348(11) . ? C42 C41 1.365(9) . ? C56 C55 1.367(9) . ? C70 C74 1.460(10) . ? C15 C16 1.395(10) . ? C65 C64 1.348(11) . ? C65 C66 1.386(9) . ? C52 C53 1.373(8) . ? C35 C34 1.371(12) . ? C26 C25 1.397(10) . ? C55 C54 1.364(10) . ? C34 C33 1.376(12) . ? C54 C53 1.362(10) . ? C25 C24 1.315(12) . ? C41 C46 1.383(9) . ? C43 C44 1.388(12) . ? C44 C45 1.402(11) . ? C13 C12 1.390(12) . ? C16 C11 1.353(10) . ? C12 C11 1.371(12) . ? C24 C23 1.363(12) . ? C23 C22 1.406(11) . ? O3 C73 1.443(9) . ? O4 C45 1.356(9) . ? O4 C74 1.432(9) 3_766 ? C46 C45 1.365(10) . ? C74 O4 1.432(9) 3_766 ? C72 C73 1.503(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 C71 Au1 P1 175.91(16) . . ? C71 Au1 Au2 85.66(17) . . ? P1 Au1 Au2 96.93(4) . . ? C8 Au2 P2 174.02(17) . . ? C8 Au2 Au1 91.78(17) . . ? P2 Au2 Au1 93.87(4) . . ? C31 P2 C21 106.0(3) . . ? C31 P2 C9 104.6(3) . . ? C21 P2 C9 105.7(3) . . ? C31 P2 Au2 114.58(18) . . ? C21 P2 Au2 113.8(2) . . ? C9 P2 Au2 111.4(2) . . ? C10 P1 C61 100.3(3) . . ? C10 P1 C51 106.4(3) . . ? C61 P1 C51 108.8(3) . . ? C10 P1 Au1 115.71(19) . . ? C61 P1 Au1 114.2(2) . . ? C51 P1 Au1 110.7(2) . . ? C41 O1 C72 118.4(6) . . ? C16 O2 C6 116.4(6) . . ? C7 C8 Au2 169.8(6) . . ? C9 C10 P1 128.5(5) 3_766 . ? C10 C9 P2 120.1(5) 3_766 . ? C66 C61 C62 118.7(6) . . ? C66 C61 P1 122.2(5) . . ? C62 C61 P1 119.0(5) . . ? O3 C14 C15 115.0(7) . . ? O3 C14 C13 124.8(7) . . ? C15 C14 C13 120.2(8) . . ? C32 C31 C36 120.2(6) . . ? C32 C31 P2 119.0(5) . . ? C36 C31 P2 120.4(5) . . ? C31 C36 C35 119.2(7) . . ? C8 C7 C6 173.4(8) . . ? C70 C71 Au1 175.6(6) . . ? C56 C51 C52 119.3(6) . . ? C56 C51 P1 119.3(5) . . ? C52 C51 P1 121.4(5) . . ? C31 C32 C33 120.7(7) . . ? C26 C21 C22 119.5(6) . . ? C26 C21 P2 120.6(5) . . ? C22 C21 P2 119.8(5) . . ? C64 C63 C62 119.4(7) . . ? C43 C42 C41 119.1(8) . . ? C51 C56 C55 120.7(7) . . ? C71 C70 C74 179.1(8) . . ? C14 C15 C16 119.7(7) . . ? C64 C65 C66 120.1(8) . . ? C53 C52 C51 119.7(6) . . ? C34 C35 C36 121.5(7) . . ? C21 C26 C25 119.7(8) . . ? C54 C55 C56 120.2(7) . . ? C35 C34 C33 119.2(7) . . ? C61 C66 C65 120.2(7) . . ? C63 C62 C61 120.2(7) . . ? C53 C54 C55 119.8(6) . . ? C24 C25 C26 121.1(9) . . ? C42 C41 O1 123.8(7) . . ? C42 C41 C46 121.0(7) . . ? O1 C41 C46 115.3(6) . . ? C65 C64 C63 121.3(7) . . ? C54 C53 C52 120.2(6) . . ? O2 C6 C7 110.2(6) . . ? C42 C43 C44 121.9(8) . . ? C43 C44 C45 118.7(8) . . ? C12 C13 C14 117.5(8) . . ? C11 C16 O2 125.0(8) . . ? C11 C16 C15 121.3(8) . . ? O2 C16 C15 113.7(7) . . ? C34 C33 C32 119.1(7) . . ? C11 C12 C13 122.8(8) . . ? C25 C24 C23 121.1(8) . . ? C24 C23 C22 119.8(8) . . ? C21 C22 C23 118.7(8) . . ? C16 C11 C12 118.2(8) . . ? C14 O3 C73 120.0(6) . . ? C45 O4 C74 117.9(6) . 3_766 ? C45 C46 C41 120.4(7) . . ? O4 C45 C46 125.6(7) . . ? O4 C45 C44 115.4(7) . . ? C46 C45 C44 119.0(8) . . ? O4 C74 C70 114.8(6) 3_766 . ? O1 C72 C73 106.3(6) . . ? O3 C73 C72 106.6(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.383 _refine_diff_density_min -1.527 _refine_diff_density_rms 0.172 #===END data_complexd _database_code_CSD 181891 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49.50 H49 Au2 Cl O4.50 P2' _chemical_formula_weight 1207.21 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' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 10.6544(6) _cell_length_b 27.8275(14) _cell_length_c 16.5665(9) _cell_angle_alpha 90.00 _cell_angle_beta 98.3770(10) _cell_angle_gamma 90.00 _cell_volume 4859.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max .1 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2348 _exptl_absorpt_coefficient_mu 6.194 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25363 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0545 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8551 _reflns_number_gt 4486 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 SHELXL _refine_ls_extinction_coef 0.00086(19) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8551 _refine_ls_number_parameters 519 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1588 _refine_ls_R_factor_gt 0.1062 _refine_ls_wR_factor_ref 0.3186 _refine_ls_wR_factor_gt 0.2845 _refine_ls_goodness_of_fit_ref 1.877 _refine_ls_restrained_S_all 1.877 _refine_ls_shift/su_max 0.567 _refine_ls_shift/su_mean 0.048 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 0.71137(7) 0.06277(3) 0.53826(5) 0.0682(4) Uani 1 1 d . . . Au2 Au 0.70292(7) 0.17294(3) 0.52513(5) 0.0717(4) Uani 1 1 d . . . P1 P 0.6585(5) 0.03930(17) 0.4071(3) 0.0678(13) Uani 1 1 d . . . P2 P 0.5400(5) 0.18404(18) 0.5986(3) 0.0720(14) Uani 1 1 d . . . O1 O 0.763(2) 0.0443(7) 0.8611(9) 0.134(7) Uani 1 1 d . . . O2 O 0.385(2) -0.0371(6) 0.9114(11) 0.116(6) Uani 1 1 d . . . O3 O 0.2953(17) -0.1259(6) 0.8589(10) 0.122(6) Uani 1 1 d . . . O4 O 1.0562(13) 0.1900(5) 0.3128(9) 0.089(4) Uani 1 1 d . . . C1 C 0.757(2) 0.0752(6) 0.6606(14) 0.088(7) Uani 1 1 d . . . C2 C 0.788(2) 0.0782(8) 0.7305(14) 0.096(7) Uani 1 1 d . . . C3 C 0.829(2) 0.0830(9) 0.8168(14) 0.110(8) Uani 1 1 d . . . H3A H 0.8075 0.1150 0.8353 0.132 Uiso 1 1 calc R . . H3B H 0.9215 0.0790 0.8286 0.132 Uiso 1 1 calc R . . C4 C 0.632(3) 0.0479(10) 0.8575(15) 0.105(8) Uani 1 1 d . . . C5 C 0.554(4) 0.0866(8) 0.8376(15) 0.125(11) Uani 1 1 d . . . H5A H 0.5885 0.1162 0.8245 0.150 Uiso 1 1 calc R . . C6 C 0.427(3) 0.0826(11) 0.837(2) 0.132(12) Uani 1 1 d . . . H6A H 0.3751 0.1077 0.8133 0.159 Uiso 1 1 calc R . . C7 C 0.369(4) 0.0438(13) 0.8680(18) 0.133(11) Uani 1 1 d . . . H7A H 0.2825 0.0433 0.8733 0.159 Uiso 1 1 calc R . . C8 C 0.445(2) 0.008(2) 0.8896(19) 0.17(2) Uani 1 1 d . . . C9 C 0.557(4) 0.0037(9) 0.8852(13) 0.154(14) Uani 1 1 d . . . H9A H 0.5664 -0.0228 0.8474 0.185 Uiso 1 1 calc R . . H9B H 0.5999 -0.0063 0.9390 0.185 Uiso 1 1 calc R . . C10 C 0.453(3) -0.0792(9) 0.9244(16) 0.122(10) Uani 1 1 d . . . H10A H 0.5179 -0.0759 0.9727 0.146 Uiso 1 1 calc R . . H10B H 0.4964 -0.0861 0.8773 0.146 Uiso 1 1 calc R . . C11 C 0.369(3) -0.1179(11) 0.9363(14) 0.117(10) Uani 1 1 d . . . H11A H 0.4174 -0.1468 0.9551 0.141 Uiso 1 1 calc R . . H11B H 0.3149 -0.1091 0.9769 0.141 Uiso 1 1 calc R . . C12 C 0.195(3) -0.1567(9) 0.8491(14) 0.108(8) Uani 1 1 d . . . C13 C 0.884(2) 0.1575(8) 0.2245(12) 0.085(6) Uani 1 1 d . . . H13A H 0.8697 0.1355 0.2652 0.102 Uiso 1 1 calc R . . C14 C 0.979(2) 0.1881(8) 0.2397(14) 0.082(6) Uani 1 1 d . . . C15 C 1.021(3) 0.2112(11) 0.1812(18) 0.130(10) Uani 1 1 d . . . H15A H 1.1010 0.2259 0.1897 0.156 Uiso 1 1 calc R . . C16 C 0.942(2) 0.2140(9) 0.1026(16) 0.106(8) Uani 1 1 d . . . H16A H 0.9591 0.2366 0.0635 0.127 Uiso 1 1 calc R . . C17 C 0.846(3) 0.1849(10) 0.0871(13) 0.119(9) Uani 1 1 d . . . H17A H 0.8034 0.1822 0.0335 0.143 Uiso 1 1 calc R . . C18 C 1.044(2) 0.1563(8) 0.3770(12) 0.093(6) Uani 1 1 d . . . H18A H 1.1140 0.1600 0.4218 0.111 Uiso 1 1 calc R . . H18B H 1.0444 0.1233 0.3565 0.111 Uiso 1 1 calc R . . C19 C 0.901(2) 0.1684(5) 0.4105(10) 0.064(6) Uani 1 1 d . . . H19A H 0.8483 0.1812 0.3653 0.077 Uiso 1 1 calc R . . C20 C 0.849(3) 0.1680(7) 0.4566(13) 0.096(8) Uani 1 1 d . . . C21 C 0.798(2) 0.0352(6) 0.3542(12) 0.074(5) Uani 1 1 d . . . C22 C 0.902(2) 0.0402(14) 0.3992(12) 0.161(16) Uani 1 1 d . . . H22A H 0.9108 0.0546 0.4510 0.193 Uiso 1 1 calc R . . C23 C 1.009(2) 0.0209(8) 0.3622(14) 0.105(8) Uani 1 1 d . . . H23A H 1.0820 0.0099 0.3961 0.126 Uiso 1 1 calc R . . C24 C 1.004(2) 0.0188(7) 0.2733(16) 0.096(7) Uani 1 1 d . . . H24A H 1.0747 0.0104 0.2481 0.115 Uiso 1 1 calc R . . C25 C 0.883(2) 0.0308(10) 0.2279(13) 0.104(8) Uani 1 1 d . . . H25A H 0.8737 0.0347 0.1709 0.125 Uiso 1 1 calc R . . C26 C 0.779(2) 0.0366(9) 0.2700(14) 0.096(7) Uani 1 1 d . . . H26A H 0.6971 0.0414 0.2411 0.116 Uiso 1 1 calc R . . C31 C 0.5422(16) 0.0755(7) 0.3433(11) 0.066(5) Uani 1 1 d . . . C32 C 0.418(2) 0.0620(8) 0.3230(14) 0.090(7) Uani 1 1 d . . . H32A H 0.3926 0.0314 0.3387 0.108 Uiso 1 1 calc R . . C33 C 0.328(2) 0.0919(8) 0.2801(13) 0.095(7) Uani 1 1 d . . . H33A H 0.2455 0.0804 0.2618 0.114 Uiso 1 1 calc R . . C34 C 0.358(2) 0.1373(8) 0.2647(13) 0.090(6) Uani 1 1 d . . . H34A H 0.2962 0.1586 0.2392 0.108 Uiso 1 1 calc R . . C35 C 0.483(2) 0.1528(8) 0.2869(12) 0.092(7) Uani 1 1 d . . . H35A H 0.5050 0.1844 0.2746 0.110 Uiso 1 1 calc R . . C36 C 0.572(2) 0.1229(6) 0.3259(11) 0.075(5) Uani 1 1 d . . . H36A H 0.6551 0.1343 0.3414 0.089 Uiso 1 1 calc R . . C41 C 0.596(2) 0.2022(7) 0.7049(13) 0.076(5) Uani 1 1 d . . . C42 C 0.719(3) 0.2177(8) 0.7265(16) 0.111(8) Uani 1 1 d . . . H42A H 0.7722 0.2196 0.6863 0.133 Uiso 1 1 calc R . . C43 C 0.764(3) 0.2303(9) 0.8050(18) 0.121(10) Uani 1 1 d . . . H43A H 0.8494 0.2399 0.8187 0.145 Uiso 1 1 calc R . . C44 C 0.686(3) 0.2289(9) 0.8638(16) 0.112(9) Uani 1 1 d . . . H44A H 0.7188 0.2364 0.9181 0.134 Uiso 1 1 calc R . . C45 C 0.566(3) 0.2173(9) 0.8454(17) 0.113(8) Uani 1 1 d . . . H45A H 0.5115 0.2187 0.8851 0.136 Uiso 1 1 calc R . . C46 C 0.518(3) 0.2020(7) 0.7621(15) 0.099(7) Uani 1 1 d . . . H46A H 0.4332 0.1921 0.7486 0.119 Uiso 1 1 calc R . . C51 C 0.4125(16) 0.2244(4) 0.5584(9) 0.125(10) Uani 1 1 d G . . C52 C 0.3637(17) 0.2180(4) 0.4766(9) 0.133(10) Uani 1 1 d G . . H52A H 0.3781 0.1890 0.4502 0.160 Uiso 1 1 calc R . . C53 C 0.2935(14) 0.2544(4) 0.4339(6) 0.154(14) Uani 1 1 d G . . H53A H 0.2605 0.2500 0.3786 0.185 Uiso 1 1 calc R . . C54 C 0.2722(12) 0.2972(4) 0.4729(7) 0.046(4) Uani 1 1 d G . . H54A H 0.2248 0.3218 0.4440 0.056 Uiso 1 1 calc R . . C55 C 0.3210(17) 0.3036(4) 0.5547(7) 0.165(14) Uani 1 1 d G . . H55A H 0.3066 0.3325 0.5811 0.198 Uiso 1 1 calc R . . C56 C 0.3912(18) 0.2672(5) 0.5974(7) 0.162(15) Uani 1 1 d G . . H56A H 0.4242 0.2715 0.6527 0.195 Uiso 1 1 calc R . . C61 C 0.5882(19) -0.0217(6) 0.4009(11) 0.078(6) Uani 1 1 d . . . H61A H 0.5102 -0.0214 0.4259 0.094 Uiso 1 1 calc R . . H61B H 0.5658 -0.0309 0.3435 0.094 Uiso 1 1 calc R . . C62 C 0.683(2) -0.0594(7) 0.4456(13) 0.085(6) Uani 1 1 d . . . H62A H 0.7585 -0.0654 0.4187 0.102 Uiso 1 1 calc R . . C63 C 0.7109(14) -0.0465(5) 0.5276(13) 0.078(7) Uani 1 1 d . . . H63A H 0.7716 -0.0690 0.5557 0.117 Uiso 1 1 calc R . . H63B H 0.6339 -0.0470 0.5523 0.117 Uiso 1 1 calc R . . H63C H 0.7469 -0.0144 0.5317 0.117 Uiso 1 1 calc R . . C64 C 0.391(2) 0.1059(6) 0.5368(12) 0.075(5) Uani 1 1 d . . . H64A H 0.4563 0.0978 0.5034 0.090 Uiso 1 1 calc R . . H64B H 0.3319 0.1287 0.5059 0.090 Uiso 1 1 calc R . . C65 C 0.453(2) 0.1297(7) 0.6167(12) 0.078(6) Uani 1 1 d . . . H65A H 0.5109 0.1068 0.6476 0.093 Uiso 1 1 calc R . . H65B H 0.3868 0.1378 0.6499 0.093 Uiso 1 1 calc R . . C100 C 0.949(4) -0.1454(14) 0.351(2) 0.074(10) Uiso 0.50 1 d P . . H10C H 1.0348 -0.1580 0.3662 0.089 Uiso 0.50 1 calc PR . . H10D H 0.9476 -0.1122 0.3701 0.089 Uiso 0.50 1 calc PR . . Cl1 Cl 0.8593(9) -0.1743(3) 0.3902(6) 0.072(2) Uiso 0.50 1 d P . . Cl2 Cl 0.9079(16) -0.1459(7) 0.2331(12) 0.153(6) Uiso 0.50 1 d P . . O10 O 0.2909(18) 0.0892(8) -0.0361(12) 0.060(6) Uiso 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 0.0834(6) 0.0540(5) 0.0641(6) -0.0008(3) 0.0005(4) 0.0008(3) Au2 0.0877(6) 0.0562(5) 0.0690(6) 0.0016(3) 0.0046(4) -0.0034(3) P1 0.082(3) 0.058(3) 0.059(3) 0.001(2) -0.002(2) -0.002(2) P2 0.094(4) 0.062(3) 0.057(3) 0.000(2) 0.001(3) -0.006(3) O1 0.184(18) 0.147(16) 0.058(10) 0.017(10) -0.026(11) -0.043(15) O2 0.158(17) 0.086(11) 0.101(13) 0.009(10) 0.014(11) -0.004(11) O3 0.141(14) 0.122(13) 0.087(12) 0.015(10) -0.040(10) -0.056(11) O4 0.087(9) 0.102(10) 0.073(10) 0.030(8) 0.001(8) -0.017(8) C1 0.121(17) 0.054(11) 0.078(16) 0.004(10) -0.027(13) -0.006(11) C2 0.14(2) 0.081(14) 0.061(15) -0.013(11) -0.006(14) -0.012(13) C3 0.13(2) 0.101(17) 0.083(17) 0.013(14) -0.022(15) -0.033(15) C4 0.12(2) 0.11(2) 0.085(17) -0.002(15) 0.003(15) -0.027(17) C5 0.22(4) 0.060(14) 0.075(17) -0.002(12) -0.03(2) 0.022(19) C6 0.12(2) 0.11(2) 0.16(3) -0.03(2) -0.03(2) -0.019(19) C7 0.15(3) 0.15(3) 0.09(2) 0.008(19) 0.00(2) 0.03(3) C8 0.054(16) 0.38(7) 0.08(2) -0.05(3) 0.013(14) -0.05(3) C9 0.32(4) 0.070(15) 0.047(14) 0.005(11) -0.05(2) -0.02(2) C10 0.15(2) 0.11(2) 0.088(18) 0.029(15) -0.022(16) -0.08(2) C11 0.12(2) 0.18(3) 0.058(14) -0.003(15) 0.028(14) 0.005(18) C12 0.16(2) 0.094(16) 0.067(15) 0.007(13) 0.004(15) -0.036(16) C13 0.104(15) 0.089(14) 0.058(13) 0.014(11) 0.000(11) -0.029(12) C14 0.090(15) 0.083(14) 0.076(15) -0.016(12) 0.018(12) -0.027(12) C15 0.12(2) 0.17(3) 0.10(2) 0.03(2) 0.030(18) -0.018(19) C16 0.127(19) 0.097(17) 0.092(18) 0.028(14) 0.016(15) -0.024(15) C17 0.16(2) 0.14(2) 0.048(13) 0.024(13) 0.001(14) -0.071(19) C18 0.121(17) 0.100(15) 0.050(12) 0.006(11) -0.013(12) -0.001(14) C19 0.139(17) 0.029(8) 0.035(9) -0.016(7) 0.050(11) -0.054(9) C20 0.17(2) 0.067(13) 0.041(12) 0.014(10) -0.015(13) 0.053(14) C21 0.103(15) 0.055(10) 0.068(13) -0.008(9) 0.022(11) -0.012(10) C22 0.067(13) 0.38(5) 0.046(12) -0.018(19) 0.027(11) -0.15(2) C23 0.13(2) 0.099(16) 0.068(15) 0.026(13) -0.040(14) 0.001(15) C24 0.093(15) 0.062(12) 0.14(2) 0.001(13) 0.036(15) 0.008(11) C25 0.112(19) 0.15(2) 0.051(13) -0.003(14) 0.007(13) -0.009(17) C26 0.078(14) 0.127(19) 0.085(16) -0.039(14) 0.013(13) -0.015(13) C31 0.062(11) 0.082(13) 0.051(11) -0.013(9) -0.005(9) 0.007(9) C32 0.090(15) 0.091(15) 0.083(16) 0.023(12) -0.012(12) -0.006(12) C33 0.133(19) 0.087(15) 0.064(14) 0.002(12) 0.013(13) -0.002(14) C34 0.117(19) 0.077(14) 0.077(15) 0.017(12) 0.013(13) -0.005(13) C35 0.13(2) 0.090(15) 0.054(13) 0.016(11) -0.002(13) 0.009(15) C36 0.100(15) 0.062(11) 0.056(12) 0.018(9) -0.008(10) -0.004(10) C41 0.084(14) 0.071(12) 0.065(13) 0.005(10) -0.013(11) -0.002(11) C42 0.16(2) 0.092(16) 0.087(18) -0.014(14) 0.029(17) -0.010(16) C43 0.15(2) 0.094(17) 0.10(2) 0.012(16) -0.054(19) -0.036(17) C44 0.18(3) 0.083(16) 0.070(17) 0.020(13) 0.001(19) -0.029(18) C45 0.16(3) 0.090(17) 0.10(2) 0.009(15) 0.047(19) -0.007(18) C46 0.16(2) 0.063(12) 0.080(17) 0.003(12) 0.019(16) -0.015(13) C51 0.16(2) 0.110(18) 0.081(16) -0.055(14) -0.065(15) 0.035(16) C52 0.22(3) 0.051(12) 0.12(2) 0.022(13) -0.02(2) 0.009(16) C53 0.12(2) 0.20(3) 0.14(3) 0.12(3) 0.006(18) -0.04(2) C54 0.076(11) 0.018(6) 0.038(8) -0.001(6) -0.014(7) 0.031(6) C55 0.24(4) 0.20(3) 0.052(15) -0.046(18) 0.003(18) 0.10(3) C56 0.25(4) 0.063(14) 0.14(2) 0.010(16) -0.10(2) 0.015(18) C61 0.104(14) 0.069(12) 0.057(11) -0.013(9) -0.002(10) -0.046(11) C62 0.092(14) 0.078(13) 0.071(14) -0.022(11) -0.033(11) -0.006(11) C63 0.043(9) 0.020(7) 0.17(2) -0.026(10) 0.024(12) -0.001(6) C64 0.095(14) 0.053(10) 0.075(14) 0.008(9) 0.002(11) 0.004(9) C65 0.093(14) 0.063(11) 0.078(14) -0.020(10) 0.016(11) -0.021(10) _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 2.04(2) . ? Au1 P1 2.260(5) . ? Au1 Au2 3.0738(10) . ? Au2 C20 2.06(3) . ? Au2 P2 2.281(6) . ? P1 C31 1.813(18) . ? P1 C21 1.83(2) . ? P1 C61 1.851(16) . ? P2 C51 1.812(11) . ? P2 C65 1.822(19) . ? P2 C41 1.85(2) . ? O1 C4 1.39(3) . ? O1 C3 1.53(3) . ? O2 C10 1.38(3) . ? O2 C8 1.47(5) . ? O3 C12 1.36(3) . ? O3 C11 1.42(3) . ? O4 C14 1.36(2) . ? O4 C18 1.44(2) . ? C1 C2 1.16(3) . ? C2 C3 1.44(3) . ? C4 C5 1.38(4) . ? C4 C9 1.57(4) . ? C5 C6 1.35(4) . ? C6 C7 1.38(4) . ? C7 C8 1.30(5) . ? C8 C9 1.22(4) . ? C10 C11 1.43(3) . ? C12 C13 1.38(3) 3_656 ? C12 C17 1.43(3) 3_656 ? C13 C14 1.32(3) . ? C13 C12 1.38(3) 3_656 ? C14 C15 1.29(3) . ? C15 C16 1.45(3) . ? C16 C17 1.30(3) . ? C17 C12 1.43(3) 3_656 ? C18 C19 1.72(3) . ? C19 C20 1.01(3) . ? C21 C22 1.25(3) . ? C21 C26 1.38(3) . ? C22 C23 1.47(4) . ? C23 C24 1.47(3) . ? C24 C25 1.44(3) . ? C25 C26 1.40(3) . ? C31 C32 1.37(3) . ? C31 C36 1.40(2) . ? C32 C33 1.39(3) . ? C33 C34 1.34(3) . ? C34 C35 1.39(3) . ? C35 C36 1.35(3) . ? C41 C46 1.34(3) . ? C41 C42 1.38(3) . ? C42 C43 1.37(3) . ? C43 C44 1.37(4) . ? C44 C45 1.31(3) . ? C45 C46 1.46(3) . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? C61 C62 1.57(3) . ? C62 C63 1.39(3) . ? C62 C64 1.56(3) 3_656 ? C64 C65 1.54(3) . ? C64 C62 1.56(3) 3_656 ? C100 Cl1 1.47(4) . ? C100 Cl2 1.93(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 C1 Au1 P1 172.9(5) . . ? C1 Au1 Au2 84.3(5) . . ? P1 Au1 Au2 102.68(12) . . ? C20 Au2 P2 175.9(5) . . ? C20 Au2 Au1 87.5(6) . . ? P2 Au2 Au1 96.55(13) . . ? C31 P1 C21 106.7(9) . . ? C31 P1 C61 103.9(9) . . ? C21 P1 C61 105.5(9) . . ? C31 P1 Au1 117.0(6) . . ? C21 P1 Au1 111.8(7) . . ? C61 P1 Au1 111.1(6) . . ? C51 P2 C65 101.6(10) . . ? C51 P2 C41 107.4(8) . . ? C65 P2 C41 99.8(10) . . ? C51 P2 Au2 118.4(7) . . ? C65 P2 Au2 115.0(7) . . ? C41 P2 Au2 112.5(8) . . ? C4 O1 C3 117(2) . . ? C10 O2 C8 121(3) . . ? C12 O3 C11 122(2) . . ? C14 O4 C18 121.5(16) . . ? C2 C1 Au1 174(2) . . ? C1 C2 C3 178(3) . . ? C2 C3 O1 108.4(18) . . ? C5 C4 O1 130(3) . . ? C5 C4 C9 112(3) . . ? O1 C4 C9 119(3) . . ? C6 C5 C4 120(3) . . ? C5 C6 C7 124(3) . . ? C8 C7 C6 114(4) . . ? C7 C8 C9 129(5) . . ? C7 C8 O2 117(3) . . ? C9 C8 O2 113(5) . . ? C8 C9 C4 119(4) . . ? O2 C10 C11 109(3) . . ? O3 C11 C10 106(2) . . ? O3 C12 C13 119(2) . 3_656 ? O3 C12 C17 125(2) . 3_656 ? C13 C12 C17 116(2) 3_656 3_656 ? C14 C13 C12 122(2) . 3_656 ? C13 C14 C15 121(2) . . ? C13 C14 O4 123(2) . . ? C15 C14 O4 115(2) . . ? C14 C15 C16 119(3) . . ? C17 C16 C15 119(2) . . ? C16 C17 C12 121(2) . 3_656 ? O4 C18 C19 107.0(15) . . ? C20 C19 C18 148(2) . . ? C19 C20 Au2 164(2) . . ? C22 C21 C26 126(2) . . ? C22 C21 P1 114.7(16) . . ? C26 C21 P1 118.2(16) . . ? C21 C22 C23 113(2) . . ? C22 C23 C24 121.0(19) . . ? C25 C24 C23 115(2) . . ? C24 C25 C26 119(2) . . ? C21 C26 C25 119(2) . . ? C32 C31 C36 116.7(18) . . ? C32 C31 P1 123.0(16) . . ? C36 C31 P1 119.3(13) . . ? C31 C32 C33 122(2) . . ? C34 C33 C32 120(2) . . ? C33 C34 C35 119(2) . . ? C36 C35 C34 121(2) . . ? C35 C36 C31 121(2) . . ? C46 C41 C42 119(2) . . ? C46 C41 P2 121.8(18) . . ? C42 C41 P2 119.6(19) . . ? C43 C42 C41 121(3) . . ? C42 C43 C44 120(3) . . ? C45 C44 C43 121(3) . . ? C44 C45 C46 119(3) . . ? C41 C46 C45 120(2) . . ? C52 C51 C56 120.0 . . ? C52 C51 P2 115.6(9) . . ? C56 C51 P2 121.6(9) . . ? C53 C52 C51 120.0 . . ? C52 C53 C54 120.0 . . ? C55 C54 C53 120.0 . . ? C54 C55 C56 120.0 . . ? C55 C56 C51 120.0 . . ? C62 C61 P1 111.2(12) . . ? C63 C62 C64 94.3(17) . 3_656 ? C63 C62 C61 108.6(17) . . ? C64 C62 C61 109.8(15) 3_656 . ? C65 C64 C62 111.1(16) . 3_656 ? C64 C65 P2 112.4(14) . . ? Cl1 C100 Cl2 112(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 4.883 _refine_diff_density_min -2.581 _refine_diff_density_rms 0.330 #===END