# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1375 data_hitchcock-lappert-layh _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '[{Au[mu-N(SiMe3)C(Ph)C(SiMe3)2]}2]' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C34 H64 Au2 N2 Si6' _chemical_formula_weight 1063.35 _chemical_melting_point ? _chemical_compound_source ? 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' 'Au' 'Au' -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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 10.087(7) _cell_length_b 17.602(5) _cell_length_c 13.092(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.78(3) _cell_angle_gamma 90.00 _cell_volume 2200.7(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method ? _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 6.846 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 1.00 _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 ' Enraf-Nonius CAD4' _diffrn_measurement_method \w--2\q _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4079 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 24.96 _reflns_number_total 3855 _reflns_number_observed 2932 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'CAMERON (Watkin and Pearce,1993)' _computing_publication_material SHELXL-93 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0179P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3854 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_obs 0.0340 _refine_ls_wR_factor_all 0.0717 _refine_ls_wR_factor_obs 0.0639 _refine_ls_goodness_of_fit_all 0.997 _refine_ls_goodness_of_fit_obs 1.029 _refine_ls_restrained_S_all 0.998 _refine_ls_restrained_S_obs 1.029 _refine_ls_shift/esd_max -0.009 _refine_ls_shift/esd_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Au Au 0.52042(3) 0.064174(13) 0.05871(2) 0.03335(9) Uani 1 d . . Si1 Si 0.3277(2) 0.20559(11) -0.0452(2) 0.0468(5) Uani 1 d . . Si2 Si 0.4338(2) 0.01434(12) -0.2797(2) 0.0438(5) Uani 1 d . . Si3 Si 0.1912(2) -0.08562(11) -0.2350(2) 0.0469(5) Uani 1 d . . N N 0.3550(5) 0.1073(3) -0.0705(4) 0.0327(12) Uani 1 d . . C1 C 0.2821(6) 0.0646(4) -0.1493(5) 0.0342(14) Uani 1 d . . C2 C 0.3276(7) -0.0083(3) -0.1853(5) 0.0336(15) Uani 1 d . . C3 C 0.1374(7) 0.0918(4) -0.2094(5) 0.039(2) Uani 1 d . . C4 C 0.0381(8) 0.0922(4) -0.1560(7) 0.056(2) Uani 1 d . . H4 H 0.0627(8) 0.0757(4) -0.0848(7) 0.067 Uiso 1 calc R . C5 C -0.0973(9) 0.1170(5) -0.2086(8) 0.075(3) Uani 1 d . . H5 H -0.1644(9) 0.1160(5) -0.1737(8) 0.090 Uiso 1 calc R . C6 C -0.1312(9) 0.1430(5) -0.3132(9) 0.078(3) Uani 1 d . . H6 H -0.2211(9) 0.1613(5) -0.3477(9) 0.093 Uiso 1 calc R . C7 C -0.0372(9) 0.1427(4) -0.3665(7) 0.062(2) Uani 1 d . . H7 H -0.0623(9) 0.1605(4) -0.4370(7) 0.075 Uiso 1 calc R . C8 C 0.0968(8) 0.1157(4) -0.3162(6) 0.052(2) Uani 1 d . . H8 H 0.1603(8) 0.1135(4) -0.3542(6) 0.062 Uiso 1 calc R . C9 C 0.2620(11) 0.2106(5) 0.0716(6) 0.082(3) Uani 1 d . . H9A H 0.1714(11) 0.1872(5) 0.0529(6) 0.122 Uiso 1 calc R . H9B H 0.2550(11) 0.2628(5) 0.0905(6) 0.122 Uiso 1 calc R . H9C H 0.3257(11) 0.1844(5) 0.1318(6) 0.122 Uiso 1 calc R . C10 C 0.5026(9) 0.2509(4) -0.0137(7) 0.076(3) Uani 1 d . . H10A H 0.5687(9) 0.2243(4) 0.0448(7) 0.115 Uiso 1 calc R . H10B H 0.4969(9) 0.3029(4) 0.0066(7) 0.115 Uiso 1 calc R . H10C H 0.5327(9) 0.2490(4) -0.0761(7) 0.115 Uiso 1 calc R . C11 C 0.2121(9) 0.2625(4) -0.1579(6) 0.066(2) Uani 1 d . . H11A H 0.1187(9) 0.2423(4) -0.1786(6) 0.099 Uiso 1 calc R . H11B H 0.2463(9) 0.2603(4) -0.2183(6) 0.099 Uiso 1 calc R . H11C H 0.2113(9) 0.3143(4) -0.1353(6) 0.099 Uiso 1 calc R . C12 C 0.5068(9) 0.1129(5) -0.2501(7) 0.067(2) Uani 1 d . . H12A H 0.4319(9) 0.1480(5) -0.2556(7) 0.101 Uiso 1 calc R . H12B H 0.5529(9) 0.1265(5) -0.3012(7) 0.101 Uiso 1 calc R . H12C H 0.5727(9) 0.1146(5) -0.1785(7) 0.101 Uiso 1 calc R . C13 C 0.3276(10) 0.0108(6) -0.4283(6) 0.078(3) Uani 1 d . . H13A H 0.2466(10) 0.0427(6) -0.4416(6) 0.118 Uiso 1 calc R . H13B H 0.2986(10) -0.0405(6) -0.4484(6) 0.118 Uiso 1 calc R . H13C H 0.3840(10) 0.0285(6) -0.4703(6) 0.118 Uiso 1 calc R . C14 C 0.5863(10) -0.0492(5) -0.2672(7) 0.075(3) Uani 1 d . . H14A H 0.5543(10) -0.1007(5) -0.2819(7) 0.112 Uiso 1 calc R . H14B H 0.6514(10) -0.0459(5) -0.1954(7) 0.112 Uiso 1 calc R . H14C H 0.6317(10) -0.0338(5) -0.3180(7) 0.112 Uiso 1 calc R . C15 C 0.0297(8) -0.0633(4) -0.3517(6) 0.064(2) Uani 1 d . . H15A H 0.0564(8) -0.0473(4) -0.4124(6) 0.096 Uiso 1 calc R . H15B H -0.0218(8) -0.0234(4) -0.3316(6) 0.096 Uiso 1 calc R . H15C H -0.0279(8) -0.1079(4) -0.3707(6) 0.096 Uiso 1 calc R . C16 C 0.2694(10) -0.1691(4) -0.2840(6) 0.072(3) Uani 1 d . . H16A H 0.3022(10) -0.1534(4) -0.3418(6) 0.108 Uiso 1 calc R . H16B H 0.1996(10) -0.2079(4) -0.3093(6) 0.108 Uiso 1 calc R . H16C H 0.3463(10) -0.1888(4) -0.2258(6) 0.108 Uiso 1 calc R . C17 C 0.1284(9) -0.1160(5) -0.1232(7) 0.071(3) Uani 1 d . . H17A H 0.2071(9) -0.1282(5) -0.0612(7) 0.106 Uiso 1 calc R . H17B H 0.0697(9) -0.1600(5) -0.1450(7) 0.106 Uiso 1 calc R . H17C H 0.0757(9) -0.0756(5) -0.1055(7) 0.106 Uiso 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 Au 0.03466(14) 0.03182(13) 0.02842(13) -0.00086(13) 0.00299(10) 0.00236(14) Si1 0.0563(13) 0.0372(11) 0.0415(11) -0.0010(9) 0.0083(10) 0.0090(10) Si2 0.0420(12) 0.0548(12) 0.0354(11) 0.0043(9) 0.0136(9) 0.0059(10) Si3 0.0459(12) 0.0418(12) 0.0437(12) -0.0001(9) 0.0014(10) -0.0084(9) N 0.032(3) 0.034(3) 0.027(3) 0.004(2) 0.003(2) 0.003(2) C1 0.030(3) 0.044(4) 0.026(3) 0.012(3) 0.007(3) -0.003(3) C2 0.035(4) 0.036(4) 0.025(3) 0.002(3) 0.002(3) 0.000(3) C3 0.032(4) 0.037(4) 0.038(4) 0.003(3) 0.000(3) 0.002(3) C4 0.045(5) 0.062(5) 0.057(5) 0.008(4) 0.014(4) 0.004(4) C5 0.039(5) 0.087(7) 0.099(8) 0.006(6) 0.025(5) 0.015(5) C6 0.039(5) 0.078(6) 0.100(8) 0.003(6) 0.000(5) 0.011(5) C7 0.054(5) 0.061(5) 0.048(5) 0.013(4) -0.017(4) 0.013(4) C8 0.048(5) 0.058(5) 0.044(4) 0.006(4) 0.007(4) 0.010(4) C9 0.126(9) 0.069(6) 0.066(6) -0.003(5) 0.054(6) 0.026(6) C10 0.079(7) 0.038(5) 0.093(7) 0.002(5) 0.002(5) -0.006(4) C11 0.082(7) 0.041(4) 0.070(6) 0.009(4) 0.018(5) 0.011(4) C12 0.060(6) 0.072(6) 0.087(7) 0.010(5) 0.046(5) -0.008(5) C13 0.078(7) 0.119(8) 0.035(5) 0.000(5) 0.014(4) 0.004(6) C14 0.085(7) 0.077(6) 0.077(6) 0.022(5) 0.046(6) 0.026(5) C15 0.054(5) 0.054(5) 0.064(5) 0.002(4) -0.009(4) -0.020(4) C16 0.100(7) 0.042(5) 0.060(5) -0.006(4) 0.007(5) -0.006(5) C17 0.066(6) 0.067(6) 0.077(6) 0.007(5) 0.019(5) -0.013(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au N 2.099(5) . ? Au C2 2.104(6) 3_655 ? Au Au 2.6887(8) 3_655 ? Au Si3 3.100(3) 3_655 ? Au Si2 3.103(2) 3_655 ? Si1 N 1.799(5) . ? Si1 C10 1.858(8) . ? Si1 C11 1.852(7) . ? Si1 C9 1.854(8) . ? Si2 C14 1.866(8) . ? Si2 C12 1.875(8) . ? Si2 C13 1.897(7) . ? Si2 C2 1.920(7) . ? Si2 Au 3.103(2) 3_655 ? Si3 C17 1.851(8) . ? Si3 C15 1.881(7) . ? Si3 C16 1.876(8) . ? Si3 C2 1.895(6) . ? Si3 Au 3.100(3) 3_655 ? N C1 1.297(8) . ? C1 C3 1.497(9) . ? C1 C2 1.490(9) . ? C2 Au 2.104(6) 3_655 ? C3 C8 1.389(9) . ? C3 C4 1.394(10) . ? C4 C5 1.387(11) . ? C5 C6 1.379(12) . ? C6 C7 1.346(13) . ? C7 C8 1.383(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N Au C2 173.0(2) . 3_655 ? N Au Au 84.69(14) . 3_655 ? C2 Au Au 89.8(2) 3_655 3_655 ? N Au Si3 150.22(14) . 3_655 ? C2 Au Si3 36.8(2) 3_655 3_655 ? Au Au Si3 117.54(4) 3_655 3_655 ? N Au Si2 138.92(15) . 3_655 ? C2 Au Si2 37.4(2) 3_655 3_655 ? Au Au Si2 96.21(4) 3_655 3_655 ? Si3 Au Si2 62.48(6) 3_655 3_655 ? N Si1 C10 105.2(3) . . ? N Si1 C11 117.9(3) . . ? C10 Si1 C11 104.7(4) . . ? N Si1 C9 108.3(3) . . ? C10 Si1 C9 111.2(4) . . ? C11 Si1 C9 109.3(4) . . ? C14 Si2 C12 106.2(4) . . ? C14 Si2 C13 104.3(4) . . ? C12 Si2 C13 107.2(4) . . ? C14 Si2 C2 115.7(3) . . ? C12 Si2 C2 108.8(3) . . ? C13 Si2 C2 113.9(4) . . ? C14 Si2 Au 77.3(3) . 3_655 ? C12 Si2 Au 106.8(3) . 3_655 ? C13 Si2 Au 143.8(3) . 3_655 ? C2 Si2 Au 41.8(2) . 3_655 ? C17 Si3 C15 106.0(4) . . ? C17 Si3 C16 109.4(4) . . ? C15 Si3 C16 103.6(4) . . ? C17 Si3 C2 109.3(3) . . ? C15 Si3 C2 118.2(3) . . ? C16 Si3 C2 109.9(4) . . ? C17 Si3 Au 85.7(3) . 3_655 ? C15 Si3 Au 159.9(2) . 3_655 ? C16 Si3 Au 87.3(3) . 3_655 ? C2 Si3 Au 41.7(2) . 3_655 ? C1 N Si1 128.5(5) . . ? C1 N Au 122.1(4) . . ? Si1 N Au 109.2(3) . . ? N C1 C3 116.1(6) . . ? N C1 C2 126.7(6) . . ? C3 C1 C2 117.2(5) . . ? C1 C2 Si3 117.7(5) . . ? C1 C2 Si2 108.4(4) . . ? Si3 C2 Si2 115.0(3) . . ? C1 C2 Au 112.0(4) . 3_655 ? Si3 C2 Au 101.5(3) . 3_655 ? Si2 C2 Au 100.8(3) . 3_655 ? C8 C3 C4 118.5(7) . . ? C8 C3 C1 123.2(6) . . ? C4 C3 C1 118.4(6) . . ? C5 C4 C3 120.3(8) . . ? C4 C5 C6 119.2(9) . . ? C7 C6 C5 121.5(8) . . ? C6 C7 C8 119.9(8) . . ? C7 C8 C3 120.6(8) . . ? _refine_diff_density_max 1.101 _refine_diff_density_min -0.648 _refine_diff_density_rms 0.120