# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Steven Nolan' 'Xavier Bantreil' 'Sylvain Gaillard' 'Alexandra Slawin' _publ_contact_author_name 'Steven Nolan' _publ_contact_author_email SN17@ST-ANDREWS.AC.UK _publ_section_title ; Syntheses and characterizations of IPrMe-containing silver(I), gold(I) and gold(III) complexes ; # Attachment 'compound3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 727081' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_absolute_configuration ad _chemical_formula_moiety 'C29 H40 Ag Cl N2,C H2 Cl2' _chemical_formula_sum 'C30 H42 Ag Cl3 N2' _chemical_formula_weight 644.88 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' N N 0.0061 0.0033 '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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.203(4) _cell_length_b 14.287(5) _cell_length_c 18.176(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3169.1(19) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 7063 _cell_measurement_theta_min 1.8129 _cell_measurement_theta_max 27.6589 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.1000 _exptl_crystal_size_min 0.0300 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 0.909 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8934 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29178 _diffrn_reflns_av_R_equivalents 0.0843 _diffrn_reflns_av_sigmaI/netI 0.0712 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 25.34 _reflns_number_total 5709 _reflns_number_gt 5419 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _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^)+(0.0566P)^2^+1.6985P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(3) _refine_ls_number_reflns 5709 _refine_ls_number_parameters 328 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0411 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.0962 _refine_ls_wR_factor_gt 0.0940 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _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 Ag1 Ag 0.19987(2) 0.366719(17) 0.535618(14) 0.02501(10) Uani 1 1 d . . . Cl1 Cl 0.16457(8) 0.28387(7) 0.64367(5) 0.0325(2) Uani 1 1 d . . . C1 C 0.2330(3) 0.4446(3) 0.4410(2) 0.0246(8) Uani 1 1 d . . . N2 N 0.2955(3) 0.52306(19) 0.43842(16) 0.0228(6) Uani 1 1 d . . . C3 C 0.3034(3) 0.5578(2) 0.36646(19) 0.0227(7) Uani 1 1 d . . . C4 C 0.2423(3) 0.5006(3) 0.3238(2) 0.0237(8) Uani 1 1 d . . . N5 N 0.2002(3) 0.43220(18) 0.37120(15) 0.0216(6) Uani 1 1 d . . . C6 C 0.3544(3) 0.5596(2) 0.5009(2) 0.0238(7) Uani 1 1 d . . . C7 C 0.3106(3) 0.6363(2) 0.5382(2) 0.0301(8) Uani 1 1 d . . . C8 C 0.3694(4) 0.6695(3) 0.5988(2) 0.0362(10) Uani 1 1 d . . . H8A H 0.3427 0.7221 0.6253 0.043 Uiso 1 1 calc R . . C9 C 0.4660(3) 0.6269(3) 0.6209(2) 0.0372(10) Uani 1 1 d . . . H9A H 0.5040 0.6499 0.6628 0.045 Uiso 1 1 calc R . . C10 C 0.5073(4) 0.5515(3) 0.5826(2) 0.0356(9) Uani 1 1 d . . . H10A H 0.5733 0.5227 0.5986 0.043 Uiso 1 1 calc R . . C11 C 0.4533(3) 0.5167(3) 0.5203(2) 0.0279(8) Uani 1 1 d . . . C12 C 0.2031(4) 0.6796(3) 0.5152(2) 0.0404(10) Uani 1 1 d . . . H12A H 0.1938 0.6683 0.4612 0.048 Uiso 1 1 calc R . . C13 C 0.1069(4) 0.6324(4) 0.5549(3) 0.0532(13) Uani 1 1 d . . . H13A H 0.1106 0.5646 0.5474 0.080 Uiso 1 1 calc R . . H13B H 0.0377 0.6563 0.5351 0.080 Uiso 1 1 calc R . . H13C H 0.1110 0.6462 0.6077 0.080 Uiso 1 1 calc R . . C14 C 0.1976(5) 0.7859(3) 0.5282(3) 0.0621(14) Uani 1 1 d . . . H14A H 0.2588 0.8164 0.5027 0.093 Uiso 1 1 calc R . . H14B H 0.2026 0.7987 0.5811 0.093 Uiso 1 1 calc R . . H14C H 0.1282 0.8103 0.5091 0.093 Uiso 1 1 calc R . . C15 C 0.5030(3) 0.4368(3) 0.4756(2) 0.0294(8) Uani 1 1 d . . . H15A H 0.4537 0.4246 0.4328 0.035 Uiso 1 1 calc R . . C16 C 0.5089(4) 0.3474(3) 0.5214(3) 0.0452(11) Uani 1 1 d . . . H16A H 0.4358 0.3323 0.5403 0.068 Uiso 1 1 calc R . . H16B H 0.5594 0.3567 0.5627 0.068 Uiso 1 1 calc R . . H16C H 0.5352 0.2958 0.4906 0.068 Uiso 1 1 calc R . . C17 C 0.6153(4) 0.4629(3) 0.4456(3) 0.0461(12) Uani 1 1 d . . . H17A H 0.6095 0.5205 0.4166 0.069 Uiso 1 1 calc R . . H17B H 0.6426 0.4121 0.4143 0.069 Uiso 1 1 calc R . . H17C H 0.6662 0.4728 0.4866 0.069 Uiso 1 1 calc R . . C18 C 0.1322(3) 0.3556(2) 0.34565(19) 0.0217(7) Uani 1 1 d . . . C19 C 0.0192(3) 0.3676(3) 0.3451(2) 0.0313(8) Uani 1 1 d . . . C20 C -0.0439(4) 0.2939(3) 0.3176(2) 0.0382(10) Uani 1 1 d . . . H20A H -0.1216 0.2985 0.3181 0.046 Uiso 1 1 calc R . . C21 C 0.0052(4) 0.2150(3) 0.2899(3) 0.0430(11) Uani 1 1 d . . . H21A H -0.0390 0.1667 0.2696 0.052 Uiso 1 1 calc R . . C22 C 0.1180(4) 0.2043(3) 0.2910(2) 0.0378(10) Uani 1 1 d . . . H22A H 0.1502 0.1487 0.2722 0.045 Uiso 1 1 calc R . . C23 C 0.1848(3) 0.2747(2) 0.3195(2) 0.0272(8) Uani 1 1 d . . . C24 C -0.0340(3) 0.4530(3) 0.3765(3) 0.0384(10) Uani 1 1 d . . . H24A H 0.0236 0.5025 0.3808 0.046 Uiso 1 1 calc R . . C25 C -0.1252(5) 0.4916(4) 0.3272(3) 0.0598(15) Uani 1 1 d . . . H25A H -0.0961 0.5029 0.2778 0.090 Uiso 1 1 calc R . . H25B H -0.1526 0.5505 0.3479 0.090 Uiso 1 1 calc R . . H25C H -0.1851 0.4461 0.3245 0.090 Uiso 1 1 calc R . . C26 C -0.0793(4) 0.4342(4) 0.4543(3) 0.0476(12) Uani 1 1 d . . . H26A H -0.0207 0.4093 0.4855 0.071 Uiso 1 1 calc R . . H26B H -0.1391 0.3886 0.4514 0.071 Uiso 1 1 calc R . . H26C H -0.1068 0.4928 0.4754 0.071 Uiso 1 1 calc R . . C27 C 0.3075(4) 0.2609(3) 0.3255(2) 0.0331(9) Uani 1 1 d . . . H27A H 0.3412 0.3233 0.3360 0.040 Uiso 1 1 calc R . . C28 C 0.3343(4) 0.1960(3) 0.3905(3) 0.0459(11) Uani 1 1 d . . . H28A H 0.3006 0.2208 0.4354 0.069 Uiso 1 1 calc R . . H28B H 0.4139 0.1927 0.3970 0.069 Uiso 1 1 calc R . . H28C H 0.3055 0.1333 0.3805 0.069 Uiso 1 1 calc R . . C29 C 0.3596(4) 0.2229(4) 0.2551(3) 0.0446(11) Uani 1 1 d . . . H29A H 0.3415 0.2643 0.2138 0.067 Uiso 1 1 calc R . . H29B H 0.3313 0.1600 0.2452 0.067 Uiso 1 1 calc R . . H29C H 0.4393 0.2201 0.2611 0.067 Uiso 1 1 calc R . . C30 C 0.3712(4) 0.6415(3) 0.3483(2) 0.0322(9) Uani 1 1 d . . . H30A H 0.3695 0.6524 0.2951 0.048 Uiso 1 1 calc R . . H30B H 0.4470 0.6308 0.3640 0.048 Uiso 1 1 calc R . . H30C H 0.3418 0.6964 0.3739 0.048 Uiso 1 1 calc R . . C31 C 0.2196(4) 0.5007(3) 0.2432(2) 0.0312(9) Uani 1 1 d . . . H31A H 0.2523 0.5565 0.2208 0.047 Uiso 1 1 calc R . . H31B H 0.1403 0.5011 0.2349 0.047 Uiso 1 1 calc R . . H31C H 0.2514 0.4445 0.2208 0.047 Uiso 1 1 calc R . . C41 C 0.3963(4) 0.8837(4) 0.2824(3) 0.0525(12) Uani 1 1 d . . . H41A H 0.4400 0.8303 0.3009 0.063 Uiso 1 1 calc R . . H41B H 0.3630 0.8646 0.2350 0.063 Uiso 1 1 calc R . . Cl2 Cl 0.29162(14) 0.90823(11) 0.34530(9) 0.0754(4) Uani 1 1 d . . . Cl3 Cl 0.48230(15) 0.97771(12) 0.26730(13) 0.0898(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02718(15) 0.02721(14) 0.02063(15) 0.00313(11) 0.00097(11) -0.00311(11) Cl1 0.0394(5) 0.0354(5) 0.0225(5) 0.0072(4) 0.0011(4) -0.0069(4) C1 0.0221(18) 0.0280(17) 0.0239(19) 0.0008(15) -0.0009(14) 0.0005(14) N2 0.0267(15) 0.0221(13) 0.0196(14) -0.0001(11) 0.0004(13) -0.0033(13) C3 0.0262(17) 0.0210(15) 0.0210(17) 0.0017(13) 0.0045(16) -0.0003(15) C4 0.0254(18) 0.0266(18) 0.019(2) 0.0032(14) 0.0029(15) 0.0004(15) N5 0.0237(14) 0.0194(13) 0.0217(15) 0.0013(11) 0.0011(13) -0.0017(13) C6 0.0269(18) 0.0242(17) 0.0203(18) 0.0005(15) 0.0040(15) -0.0041(15) C7 0.041(2) 0.0280(17) 0.0208(18) -0.0027(16) 0.0056(17) -0.0039(16) C8 0.054(3) 0.033(2) 0.021(2) -0.0086(17) 0.0071(19) -0.0094(19) C9 0.042(2) 0.047(2) 0.023(2) -0.0124(19) -0.0018(17) -0.014(2) C10 0.033(2) 0.047(2) 0.026(2) -0.0004(18) -0.0014(18) -0.0038(18) C11 0.0249(18) 0.0352(19) 0.024(2) -0.0008(16) 0.0028(15) -0.0059(15) C12 0.055(3) 0.039(2) 0.027(2) -0.0060(16) -0.002(2) 0.012(2) C13 0.040(2) 0.053(3) 0.067(3) -0.014(3) 0.003(2) 0.011(2) C14 0.097(4) 0.039(2) 0.050(3) -0.003(2) 0.005(4) 0.019(3) C15 0.0254(18) 0.0320(19) 0.031(2) 0.0010(17) 0.0031(17) -0.0015(15) C16 0.048(3) 0.042(2) 0.046(3) 0.008(2) 0.001(2) 0.009(2) C17 0.034(2) 0.048(3) 0.056(3) -0.011(2) 0.013(2) -0.0046(19) C18 0.0247(17) 0.0245(17) 0.0158(17) 0.0049(14) -0.0034(14) -0.0057(15) C19 0.0275(18) 0.037(2) 0.029(2) 0.0121(18) 0.0025(16) -0.0048(18) C20 0.030(2) 0.050(2) 0.035(2) 0.015(2) -0.0070(18) -0.0117(19) C21 0.047(3) 0.048(3) 0.035(2) 0.007(2) -0.012(2) -0.027(2) C22 0.047(3) 0.037(2) 0.029(2) -0.0030(18) -0.002(2) -0.0148(19) C23 0.035(2) 0.0251(17) 0.0218(19) 0.0008(14) 0.0009(17) -0.0051(16) C24 0.024(2) 0.040(2) 0.052(3) 0.014(2) 0.0049(19) 0.0066(17) C25 0.052(3) 0.076(4) 0.052(3) 0.025(3) 0.006(3) 0.027(3) C26 0.040(2) 0.064(3) 0.039(3) 0.008(2) 0.004(2) 0.010(2) C27 0.035(2) 0.0298(19) 0.034(2) -0.0006(16) 0.001(2) -0.0021(18) C28 0.043(3) 0.050(3) 0.044(3) 0.006(2) 0.004(2) 0.015(2) C29 0.046(3) 0.051(3) 0.037(3) 0.003(2) 0.011(2) 0.010(2) C30 0.049(2) 0.0259(18) 0.0217(19) 0.0066(16) 0.0021(17) -0.0092(19) C31 0.041(2) 0.0292(19) 0.024(2) 0.0014(15) -0.0003(18) -0.0061(17) C41 0.051(3) 0.052(3) 0.055(3) -0.016(2) 0.013(2) -0.001(2) Cl2 0.0685(9) 0.0765(9) 0.0813(10) 0.0056(8) 0.0337(9) 0.0159(8) Cl3 0.0685(10) 0.0650(9) 0.1360(17) 0.0430(11) 0.0203(11) -0.0076(8) _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 Ag1 C1 2.089(4) . ? Ag1 Cl1 2.3332(11) . ? C1 N5 1.341(5) . ? C1 N2 1.356(5) . ? N2 C3 1.402(4) . ? N2 C6 1.442(5) . ? C3 C4 1.351(5) . ? C3 C30 1.492(5) . ? C4 N5 1.401(4) . ? C4 C31 1.491(5) . ? N5 C18 1.450(4) . ? C6 C7 1.396(5) . ? C6 C11 1.399(6) . ? C7 C8 1.397(6) . ? C7 C12 1.510(6) . ? C8 C9 1.386(7) . ? C8 H8A 0.9500 . ? C9 C10 1.379(6) . ? C9 H9A 0.9500 . ? C10 C11 1.401(6) . ? C10 H10A 0.9500 . ? C11 C15 1.526(5) . ? C12 C13 1.534(7) . ? C12 C14 1.539(6) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.521(6) . ? C15 C16 1.526(6) . ? C15 H15A 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.389(5) . ? C18 C23 1.406(5) . ? C19 C20 1.397(6) . ? C19 C24 1.496(6) . ? C20 C21 1.373(7) . ? C20 H20A 0.9500 . ? C21 C22 1.385(7) . ? C21 H21A 0.9500 . ? C22 C23 1.394(5) . ? C22 H22A 0.9500 . ? C23 C27 1.514(6) . ? C24 C25 1.531(6) . ? C24 C26 1.542(6) . ? C24 H24A 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.529(6) . ? C27 C28 1.536(6) . ? C27 H27A 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C41 Cl3 1.727(5) . ? C41 Cl2 1.750(5) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? 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 Ag1 Cl1 178.14(11) . . ? N5 C1 N2 104.2(3) . . ? N5 C1 Ag1 130.6(3) . . ? N2 C1 Ag1 125.3(3) . . ? C1 N2 C3 111.3(3) . . ? C1 N2 C6 123.6(3) . . ? C3 N2 C6 124.9(3) . . ? C4 C3 N2 106.5(3) . . ? C4 C3 C30 131.6(3) . . ? N2 C3 C30 121.9(3) . . ? C3 C4 N5 105.7(3) . . ? C3 C4 C31 131.8(3) . . ? N5 C4 C31 122.5(3) . . ? C1 N5 C4 112.4(3) . . ? C1 N5 C18 125.0(3) . . ? C4 N5 C18 122.6(3) . . ? C7 C6 C11 123.5(4) . . ? C7 C6 N2 118.4(3) . . ? C11 C6 N2 118.0(3) . . ? C6 C7 C8 116.9(4) . . ? C6 C7 C12 121.3(4) . . ? C8 C7 C12 121.8(4) . . ? C9 C8 C7 121.1(4) . . ? C9 C8 H8A 119.4 . . ? C7 C8 H8A 119.4 . . ? C10 C9 C8 120.5(4) . . ? C10 C9 H9A 119.8 . . ? C8 C9 H9A 119.8 . . ? C9 C10 C11 121.0(4) . . ? C9 C10 H10A 119.5 . . ? C11 C10 H10A 119.5 . . ? C6 C11 C10 117.0(4) . . ? C6 C11 C15 122.5(3) . . ? C10 C11 C15 120.6(4) . . ? C7 C12 C13 110.7(3) . . ? C7 C12 C14 113.5(4) . . ? C13 C12 C14 109.2(4) . . ? C7 C12 H12A 107.7 . . ? C13 C12 H12A 107.7 . . ? C14 C12 H12A 107.7 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C15 C11 111.4(3) . . ? C17 C15 C16 111.0(4) . . ? C11 C15 C16 110.8(3) . . ? C17 C15 H15A 107.8 . . ? C11 C15 H15A 107.8 . . ? C16 C15 H15A 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 123.5(4) . . ? C19 C18 N5 118.6(3) . . ? C23 C18 N5 117.8(3) . . ? C18 C19 C20 117.2(4) . . ? C18 C19 C24 121.9(4) . . ? C20 C19 C24 120.8(4) . . ? C21 C20 C19 120.6(4) . . ? C21 C20 H20A 119.7 . . ? C19 C20 H20A 119.7 . . ? C20 C21 C22 121.3(4) . . ? C20 C21 H21A 119.4 . . ? C22 C21 H21A 119.4 . . ? C21 C22 C23 120.4(4) . . ? C21 C22 H22A 119.8 . . ? C23 C22 H22A 119.8 . . ? C22 C23 C18 116.9(4) . . ? C22 C23 C27 120.7(4) . . ? C18 C23 C27 122.3(3) . . ? C19 C24 C25 112.7(4) . . ? C19 C24 C26 111.3(4) . . ? C25 C24 C26 109.8(4) . . ? C19 C24 H24A 107.6 . . ? C25 C24 H24A 107.6 . . ? C26 C24 H24A 107.6 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C29 113.4(4) . . ? C23 C27 C28 110.2(3) . . ? C29 C27 C28 110.0(4) . . ? C23 C27 H27A 107.7 . . ? C29 C27 H27A 107.7 . . ? C28 C27 H27A 107.7 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C3 C30 H30A 109.5 . . ? C3 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C3 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C4 C31 H31A 109.5 . . ? C4 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C4 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Cl3 C41 Cl2 113.0(3) . . ? Cl3 C41 H41A 109.0 . . ? Cl2 C41 H41A 109.0 . . ? Cl3 C41 H41B 109.0 . . ? Cl2 C41 H41B 109.0 . . ? H41A C41 H41B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 C1 N2 C3 -1.5(4) . . . . ? Ag1 C1 N2 C3 178.9(3) . . . . ? N5 C1 N2 C6 -175.7(3) . . . . ? Ag1 C1 N2 C6 4.6(5) . . . . ? C1 N2 C3 C4 1.4(4) . . . . ? C6 N2 C3 C4 175.6(3) . . . . ? C1 N2 C3 C30 -177.6(3) . . . . ? C6 N2 C3 C30 -3.4(6) . . . . ? N2 C3 C4 N5 -0.7(4) . . . . ? C30 C3 C4 N5 178.1(4) . . . . ? N2 C3 C4 C31 -179.4(4) . . . . ? C30 C3 C4 C31 -0.5(7) . . . . ? N2 C1 N5 C4 1.0(4) . . . . ? Ag1 C1 N5 C4 -179.4(3) . . . . ? N2 C1 N5 C18 179.0(3) . . . . ? Ag1 C1 N5 C18 -1.4(5) . . . . ? C3 C4 N5 C1 -0.2(4) . . . . ? C31 C4 N5 C1 178.6(3) . . . . ? C3 C4 N5 C18 -178.2(3) . . . . ? C31 C4 N5 C18 0.6(6) . . . . ? C1 N2 C6 C7 -102.0(4) . . . . ? C3 N2 C6 C7 84.5(5) . . . . ? C1 N2 C6 C11 78.6(5) . . . . ? C3 N2 C6 C11 -94.9(4) . . . . ? C11 C6 C7 C8 -1.1(6) . . . . ? N2 C6 C7 C8 179.5(3) . . . . ? C11 C6 C7 C12 -179.7(4) . . . . ? N2 C6 C7 C12 1.0(5) . . . . ? C6 C7 C8 C9 -0.9(6) . . . . ? C12 C7 C8 C9 177.7(4) . . . . ? C7 C8 C9 C10 1.1(6) . . . . ? C8 C9 C10 C11 0.5(6) . . . . ? C7 C6 C11 C10 2.7(6) . . . . ? N2 C6 C11 C10 -177.9(3) . . . . ? C7 C6 C11 C15 -176.2(3) . . . . ? N2 C6 C11 C15 3.2(5) . . . . ? C9 C10 C11 C6 -2.4(6) . . . . ? C9 C10 C11 C15 176.5(4) . . . . ? C6 C7 C12 C13 89.6(5) . . . . ? C8 C7 C12 C13 -88.9(5) . . . . ? C6 C7 C12 C14 -147.2(4) . . . . ? C8 C7 C12 C14 34.3(6) . . . . ? C6 C11 C15 C17 119.2(4) . . . . ? C10 C11 C15 C17 -59.6(5) . . . . ? C6 C11 C15 C16 -116.7(4) . . . . ? C10 C11 C15 C16 64.5(5) . . . . ? C1 N5 C18 C19 91.0(4) . . . . ? C4 N5 C18 C19 -91.2(4) . . . . ? C1 N5 C18 C23 -91.9(4) . . . . ? C4 N5 C18 C23 85.9(4) . . . . ? C23 C18 C19 C20 0.7(6) . . . . ? N5 C18 C19 C20 177.7(3) . . . . ? C23 C18 C19 C24 177.3(3) . . . . ? N5 C18 C19 C24 -5.8(5) . . . . ? C18 C19 C20 C21 -2.4(6) . . . . ? C24 C19 C20 C21 -179.0(4) . . . . ? C19 C20 C21 C22 2.6(7) . . . . ? C20 C21 C22 C23 -0.9(7) . . . . ? C21 C22 C23 C18 -0.7(6) . . . . ? C21 C22 C23 C27 175.9(4) . . . . ? C19 C18 C23 C22 0.8(6) . . . . ? N5 C18 C23 C22 -176.1(3) . . . . ? C19 C18 C23 C27 -175.7(4) . . . . ? N5 C18 C23 C27 7.3(5) . . . . ? C18 C19 C24 C25 136.3(4) . . . . ? C20 C19 C24 C25 -47.3(5) . . . . ? C18 C19 C24 C26 -99.9(4) . . . . ? C20 C19 C24 C26 76.5(5) . . . . ? C22 C23 C27 C29 48.1(5) . . . . ? C18 C23 C27 C29 -135.5(4) . . . . ? C22 C23 C27 C28 -75.6(5) . . . . ? C18 C23 C27 C28 100.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.145 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.077 # Attachment 'compound4.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 727082' # start Validation Reply Form _vrf_PLAT216_4 ; PROBLEM: Disordered Cl3 (An/Solv) ADP max/min Ratio 15.80 RESPONSE: see _refine_special_details ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H40 Au Cl N2,C H2 Cl2' _chemical_formula_sum 'C30 H42 Au Cl3 N2' _chemical_formula_weight 733.97 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' N N 0.0061 0.0033 '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 P2(1)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 8.795(2) _cell_length_b 17.615(4) _cell_length_c 10.610(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.841(6) _cell_angle_gamma 90.00 _cell_volume 1619.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 5884 _cell_measurement_theta_min 2.2653 _cell_measurement_theta_max 28.3885 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.1200 _exptl_crystal_size_mid 0.1200 _exptl_crystal_size_min 0.0300 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_absorpt_coefficient_mu 4.809 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5832 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10323 _diffrn_reflns_av_R_equivalents 0.0868 _diffrn_reflns_av_sigmaI/netI 0.0902 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 25.37 _reflns_number_total 3047 _reflns_number_gt 2802 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _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. The CH2Cl2 is disordered over the mirror plane. No hydrogen atoms were allowed for in the disordered solvent. ; _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^)+(0.0792P)^2^+9.6837P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3047 _refine_ls_number_parameters 177 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0553 _refine_ls_wR_factor_ref 0.1490 _refine_ls_wR_factor_gt 0.1436 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _refine_ls_shift/su_max 0.014 _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 -0.01434(5) 0.2500 0.00795(3) 0.0206(2) Uani 1 2 d S . . Cl1 Cl -0.2733(3) 0.2500 -0.0733(3) 0.0253(6) Uani 1 2 d S . . C1 C 0.2112(13) 0.2500 0.0787(9) 0.019(2) Uani 1 2 d S . . N2 N 0.3037(7) 0.1899(4) 0.1067(5) 0.0189(13) Uani 1 1 d . . . C3 C 0.4538(8) 0.2119(4) 0.1518(6) 0.0182(15) Uani 1 1 d . . . C4 C 0.2568(8) 0.1099(4) 0.0850(6) 0.0177(15) Uani 1 1 d . . . C5 C 0.2168(9) 0.0687(5) 0.1868(7) 0.0220(16) Uani 1 1 d . . . C6 C 0.1762(10) -0.0056(4) 0.1632(9) 0.0239(19) Uani 1 1 d . . . H6A H 0.1495 -0.0359 0.2302 0.029 Uiso 1 1 calc R . . C7 C 0.1734(9) -0.0374(5) 0.0442(8) 0.0293(19) Uani 1 1 d . . . H7A H 0.1441 -0.0891 0.0306 0.035 Uiso 1 1 calc R . . C8 C 0.2120(10) 0.0042(4) -0.0549(9) 0.0226(19) Uani 1 1 d . . . H8A H 0.2081 -0.0185 -0.1366 0.027 Uiso 1 1 calc R . . C9 C 0.2567(9) 0.0792(4) -0.0359(7) 0.0223(17) Uani 1 1 d . . . C10 C 0.3033(10) 0.1257(5) -0.1456(7) 0.0265(18) Uani 1 1 d . . . H10A H 0.3426 0.1761 -0.1108 0.032 Uiso 1 1 calc R . . C11 C 0.4309(10) 0.0868(6) -0.2020(8) 0.037(2) Uani 1 1 d . . . H11A H 0.5205 0.0788 -0.1346 0.056 Uiso 1 1 calc R . . H11B H 0.4607 0.1189 -0.2693 0.056 Uiso 1 1 calc R . . H11C H 0.3937 0.0378 -0.2385 0.056 Uiso 1 1 calc R . . C12 C 0.1588(10) 0.1395(5) -0.2509(8) 0.034(2) Uani 1 1 d . . . H12A H 0.0785 0.1650 -0.2128 0.051 Uiso 1 1 calc R . . H12B H 0.1197 0.0908 -0.2873 0.051 Uiso 1 1 calc R . . H12C H 0.1876 0.1716 -0.3185 0.051 Uiso 1 1 calc R . . C13 C 0.2157(10) 0.1036(5) 0.3167(7) 0.0285(19) Uani 1 1 d . . . H13A H 0.2737 0.1526 0.3189 0.034 Uiso 1 1 calc R . . C14 C 0.0545(12) 0.1230(7) 0.3346(9) 0.049(3) Uani 1 1 d . . . H14A H 0.0052 0.1544 0.2629 0.074 Uiso 1 1 calc R . . H14B H 0.0581 0.1511 0.4148 0.074 Uiso 1 1 calc R . . H14C H -0.0049 0.0762 0.3377 0.074 Uiso 1 1 calc R . . C15 C 0.2975(14) 0.0558(6) 0.4255(9) 0.049(3) Uani 1 1 d . . . H15A H 0.4024 0.0446 0.4113 0.073 Uiso 1 1 calc R . . H15B H 0.2409 0.0082 0.4297 0.073 Uiso 1 1 calc R . . H15C H 0.3023 0.0836 0.5061 0.073 Uiso 1 1 calc R . . C16 C 0.5821(9) 0.1555(5) 0.1870(8) 0.0271(18) Uani 1 1 d . . . H16A H 0.6811 0.1823 0.2039 0.041 Uiso 1 1 calc R . . H16B H 0.5822 0.1197 0.1163 0.041 Uiso 1 1 calc R . . H16C H 0.5668 0.1277 0.2638 0.041 Uiso 1 1 calc R . . C21 C 0.3291(17) 0.7500 0.4039(14) 0.049(4) Uani 1 2 d S . . Cl2 Cl 0.5242(5) 0.7500 0.4763(4) 0.0585(11) Uani 1 2 d S . . Cl3 Cl 0.2447(6) 0.8331(3) 0.4476(4) 0.0493(15) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.0180(3) 0.0195(3) 0.0233(3) 0.000 0.00055(18) 0.000 Cl1 0.0160(14) 0.0268(15) 0.0309(14) 0.000 -0.0022(11) 0.000 C1 0.025(6) 0.018(6) 0.012(5) 0.000 -0.003(4) 0.000 N2 0.018(3) 0.020(3) 0.019(3) -0.004(3) 0.004(2) 0.002(3) C3 0.015(4) 0.021(4) 0.018(3) -0.002(3) 0.004(3) 0.002(3) C4 0.015(4) 0.020(4) 0.018(3) 0.000(3) 0.001(3) 0.004(3) C5 0.015(4) 0.025(4) 0.025(4) 0.000(3) 0.004(3) 0.002(3) C6 0.018(4) 0.022(5) 0.029(5) 0.009(3) -0.002(4) -0.003(3) C7 0.013(4) 0.025(5) 0.048(5) -0.005(4) -0.003(3) 0.000(3) C8 0.018(4) 0.020(5) 0.029(5) -0.006(3) 0.000(3) -0.001(3) C9 0.018(4) 0.022(4) 0.026(4) -0.004(3) 0.004(3) 0.003(3) C10 0.035(5) 0.027(5) 0.020(4) -0.002(3) 0.012(3) 0.003(4) C11 0.021(5) 0.062(7) 0.030(4) 0.001(4) 0.005(3) 0.008(4) C12 0.032(5) 0.037(5) 0.033(4) 0.004(4) 0.008(4) 0.005(4) C13 0.033(5) 0.035(5) 0.018(4) 0.004(3) 0.005(3) -0.006(4) C14 0.047(7) 0.066(8) 0.037(5) -0.010(5) 0.014(5) 0.008(6) C15 0.067(8) 0.046(6) 0.028(5) 0.005(4) -0.009(5) 0.004(6) C16 0.019(4) 0.033(5) 0.029(4) -0.003(4) 0.003(3) 0.004(4) C21 0.029(8) 0.068(11) 0.048(8) 0.000 0.001(6) 0.000 Cl2 0.045(3) 0.062(3) 0.063(2) 0.000 -0.009(2) 0.000 Cl3 0.055(3) 0.056(3) 0.031(2) -0.012(2) -0.011(2) 0.055(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 1.997(11) . ? Au1 Cl1 2.293(3) . ? C1 N2 1.337(9) 4_565 ? C1 N2 1.337(9) . ? N2 C3 1.381(9) . ? N2 C4 1.475(10) . ? C3 C3 1.343(15) 4_565 ? C3 C16 1.502(11) . ? C4 C5 1.396(10) . ? C4 C9 1.392(10) . ? C5 C6 1.369(11) . ? C5 C13 1.511(11) . ? C6 C7 1.377(12) . ? C6 H6A 0.9500 . ? C7 C8 1.371(12) . ? C7 H7A 0.9500 . ? C8 C9 1.384(11) . ? C8 H8A 0.9500 . ? C9 C10 1.535(11) . ? C10 C11 1.522(11) . ? C10 C12 1.561(12) . ? C10 H10A 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.502(13) . ? C13 C15 1.508(12) . ? C13 H13A 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C21 Cl3 1.740(9) 4_575 ? C21 Cl3 1.740(9) . ? C21 Cl2 1.756(15) . ? 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 Cl1 180.0(3) . . ? N2 C1 N2 104.7(9) 4_565 . ? N2 C1 Au1 127.6(5) 4_565 . ? N2 C1 Au1 127.6(5) . . ? C1 N2 C3 111.3(7) . . ? C1 N2 C4 125.3(7) . . ? C3 N2 C4 123.2(6) . . ? C3 C3 N2 106.3(4) 4_565 . ? C3 C3 C16 131.4(4) 4_565 . ? N2 C3 C16 122.3(7) . . ? C5 C4 C9 123.4(7) . . ? C5 C4 N2 118.5(6) . . ? C9 C4 N2 118.1(6) . . ? C6 C5 C4 116.6(7) . . ? C6 C5 C13 121.0(7) . . ? C4 C5 C13 122.4(7) . . ? C5 C6 C7 121.3(8) . . ? C5 C6 H6A 119.3 . . ? C7 C6 H6A 119.3 . . ? C8 C7 C6 121.2(8) . . ? C8 C7 H7A 119.4 . . ? C6 C7 H7A 119.4 . . ? C7 C8 C9 120.0(8) . . ? C7 C8 H8A 120.0 . . ? C9 C8 H8A 120.0 . . ? C8 C9 C4 117.4(7) . . ? C8 C9 C10 120.4(7) . . ? C4 C9 C10 122.2(7) . . ? C11 C10 C9 111.6(7) . . ? C11 C10 C12 110.7(6) . . ? C9 C10 C12 109.6(7) . . ? C11 C10 H10A 108.3 . . ? C9 C10 H10A 108.3 . . ? C12 C10 H10A 108.3 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C5 111.2(7) . . ? C14 C13 C15 111.6(8) . . ? C5 C13 C15 113.2(8) . . ? C14 C13 H13A 106.8 . . ? C5 C13 H13A 106.8 . . ? C15 C13 H13A 106.8 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C3 C16 H16A 109.5 . . ? C3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Cl3 C21 Cl3 114.6(9) 4_575 . ? Cl3 C21 Cl2 108.2(6) 4_575 . ? Cl3 C21 Cl2 108.2(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C1 N2 C3 -0.2(10) 4_565 . . . ? Au1 C1 N2 C3 178.9(6) . . . . ? N2 C1 N2 C4 -176.3(4) 4_565 . . . ? Au1 C1 N2 C4 2.8(12) . . . . ? C1 N2 C3 C3 0.1(7) . . . 4_565 ? C4 N2 C3 C3 176.3(5) . . . 4_565 ? C1 N2 C3 C16 -178.3(7) . . . . ? C4 N2 C3 C16 -2.1(10) . . . . ? C1 N2 C4 C5 -96.8(9) . . . . ? C3 N2 C4 C5 87.6(9) . . . . ? C1 N2 C4 C9 84.1(10) . . . . ? C3 N2 C4 C9 -91.6(8) . . . . ? C9 C4 C5 C6 0.1(12) . . . . ? N2 C4 C5 C6 -179.0(7) . . . . ? C9 C4 C5 C13 -179.1(7) . . . . ? N2 C4 C5 C13 1.7(11) . . . . ? C4 C5 C6 C7 -0.8(12) . . . . ? C13 C5 C6 C7 178.4(8) . . . . ? C5 C6 C7 C8 0.4(13) . . . . ? C6 C7 C8 C9 0.8(13) . . . . ? C7 C8 C9 C4 -1.5(12) . . . . ? C7 C8 C9 C10 178.7(7) . . . . ? C5 C4 C9 C8 1.0(12) . . . . ? N2 C4 C9 C8 -179.8(7) . . . . ? C5 C4 C9 C10 -179.1(7) . . . . ? N2 C4 C9 C10 0.0(11) . . . . ? C8 C9 C10 C11 -54.7(10) . . . . ? C4 C9 C10 C11 125.5(8) . . . . ? C8 C9 C10 C12 68.3(10) . . . . ? C4 C9 C10 C12 -111.5(8) . . . . ? C6 C5 C13 C14 -77.9(11) . . . . ? C4 C5 C13 C14 101.3(10) . . . . ? C6 C5 C13 C15 48.6(11) . . . . ? C4 C5 C13 C15 -132.2(9) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.350 _refine_diff_density_min -1.640 _refine_diff_density_rms 0.224 # Attachment 'compound5and6.cif' data_5and6 _database_code_depnum_ccdc_archive 'CCDC 727083' # start Validation Reply Form _vrf_PLAT220_snsg7 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.40 Ratio RESPONSE: see _refine_special_details ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C29 H40 Au Cl3 N2)0.5,(C29 H39 Au Cl4 N2)0.5' _chemical_formula_sum 'C29 H39.50 Au Cl3.50 N2' _chemical_formula_weight 737.17 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' N N 0.0061 0.0033 '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 P2(1)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 9.4271(19) _cell_length_b 17.845(3) _cell_length_c 9.7182(18) _cell_angle_alpha 90.00 _cell_angle_beta 110.881(5) _cell_angle_gamma 90.00 _cell_volume 1527.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 5554 _cell_measurement_theta_min 2.2825 _cell_measurement_theta_max 28.6563 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.1000 _exptl_crystal_size_mid 0.0600 _exptl_crystal_size_min 0.0500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_absorpt_coefficient_mu 5.142 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7027 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9841 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0725 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.37 _reflns_number_total 2880 _reflns_number_gt 2562 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _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. The disordered hydrogen atom is not allowed for in the refinement. There is some unresolved disorder in the isopropyl units, where the largest residual electron density exists. ; _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^)+(0.0434P)^2^+2.3152P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0023(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2880 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1067 _refine_ls_wR_factor_gt 0.0988 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.115 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.53372(4) 0.2500 0.08207(4) 0.02629(19) Uani 1 2 d S . . Cl1 Cl 0.3537(3) 0.2500 0.1927(3) 0.0441(7) Uani 1 2 d S . . Cl2 Cl 0.7216(3) 0.2500 0.3080(3) 0.0456(7) Uani 1 2 d S . . Cl3 Cl 0.3472(3) 0.2500 -0.1401(3) 0.0571(9) Uani 1 2 d S . . C1 C 0.6978(9) 0.2500 -0.0061(8) 0.0151(18) Uani 1 2 d S . . N2 N 0.7671(5) 0.3110(3) -0.0346(5) 0.0201(11) Uani 1 1 d . . . C3 C 0.8876(7) 0.2876(4) -0.0761(7) 0.0248(15) Uani 1 1 d . . . C4 C 0.7214(7) 0.3878(4) -0.0369(6) 0.0207(14) Uani 1 1 d . . . C5 C 0.6154(7) 0.4161(4) -0.1686(7) 0.0259(15) Uani 1 1 d . . . C6 C 0.5796(7) 0.4927(4) -0.1724(7) 0.0297(16) Uani 1 1 d . . . H6A H 0.5086 0.5137 -0.2596 0.036 Uiso 1 1 calc R . . C7 C 0.6449(8) 0.5370(4) -0.0535(8) 0.0346(17) Uani 1 1 d . . . H7A H 0.6186 0.5886 -0.0583 0.041 Uiso 1 1 calc R . . C8 C 0.7493(7) 0.5083(4) 0.0746(7) 0.0306(16) Uani 1 1 d . . . H8A H 0.7937 0.5405 0.1565 0.037 Uiso 1 1 calc R . . C9 C 0.7904(7) 0.4333(4) 0.0860(7) 0.0247(15) Uani 1 1 d . . . C10 C 0.5454(8) 0.3679(4) -0.3065(7) 0.0348(18) Uani 1 1 d . . . H10A H 0.5600 0.3140 -0.2767 0.042 Uiso 1 1 calc R . . C11 C 0.6257(12) 0.3828(7) -0.4180(9) 0.081(4) Uani 1 1 d . . . H11A H 0.5800 0.3513 -0.5053 0.122 Uiso 1 1 calc R . . H11B H 0.7339 0.3708 -0.3721 0.122 Uiso 1 1 calc R . . H11C H 0.6140 0.4357 -0.4470 0.122 Uiso 1 1 calc R . . C12 C 0.3786(10) 0.3819(6) -0.3825(10) 0.068(3) Uani 1 1 d . . . H12A H 0.3257 0.3720 -0.3140 0.102 Uiso 1 1 calc R . . H12B H 0.3388 0.3487 -0.4680 0.102 Uiso 1 1 calc R . . H12C H 0.3623 0.4342 -0.4152 0.102 Uiso 1 1 calc R . . C13 C 0.9110(8) 0.4051(4) 0.2249(7) 0.0368(18) Uani 1 1 d . . . H13A H 0.9185 0.3495 0.2180 0.044 Uiso 1 1 calc R . . C14 C 1.0688(9) 0.4403(6) 0.2441(9) 0.064(3) Uani 1 1 d . . . H14A H 1.0958 0.4279 0.1583 0.095 Uiso 1 1 calc R . . H14B H 1.1460 0.4201 0.3333 0.095 Uiso 1 1 calc R . . H14C H 1.0635 0.4948 0.2528 0.095 Uiso 1 1 calc R . . C15 C 0.8741(11) 0.4241(5) 0.3633(8) 0.060(3) Uani 1 1 d . . . H15A H 0.7767 0.4013 0.3550 0.090 Uiso 1 1 calc R . . H15B H 0.8677 0.4786 0.3721 0.090 Uiso 1 1 calc R . . H15C H 0.9543 0.4043 0.4508 0.090 Uiso 1 1 calc R . . C16 C 0.9942(8) 0.3401(4) -0.1108(8) 0.0369(17) Uani 1 1 d . . . H16A H 1.0992 0.3315 -0.0419 0.044 Uiso 1 1 calc R . . H16B H 0.9662 0.3926 -0.0995 0.044 Uiso 1 1 calc R . . Cl4 Cl 0.9832(9) 0.3240(5) -0.2976(9) 0.053(2) Uiso 0.25 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 0.0263(3) 0.0188(3) 0.0403(3) 0.000 0.01990(19) 0.000 Cl1 0.0430(15) 0.0393(18) 0.0680(17) 0.000 0.0420(14) 0.000 Cl2 0.0510(16) 0.056(2) 0.0345(14) 0.000 0.0218(12) 0.000 Cl3 0.0254(14) 0.099(3) 0.0484(16) 0.000 0.0151(13) 0.000 C1 0.014(4) 0.006(4) 0.019(4) 0.000 -0.002(3) 0.000 N2 0.018(3) 0.016(3) 0.028(3) 0.003(2) 0.011(2) 0.003(2) C3 0.020(3) 0.023(4) 0.035(4) -0.001(3) 0.015(3) 0.001(3) C4 0.020(3) 0.014(3) 0.034(3) 0.004(3) 0.017(3) 0.006(3) C5 0.023(3) 0.027(4) 0.030(4) 0.004(3) 0.012(3) -0.002(3) C6 0.030(4) 0.017(4) 0.043(4) 0.009(3) 0.015(3) 0.011(3) C7 0.031(4) 0.027(4) 0.055(5) 0.003(3) 0.025(4) 0.004(3) C8 0.030(4) 0.019(4) 0.051(4) -0.012(3) 0.025(3) -0.012(3) C9 0.025(3) 0.021(4) 0.032(3) 0.003(3) 0.014(3) -0.005(3) C10 0.044(4) 0.023(4) 0.029(4) 0.007(3) 0.003(3) 0.010(3) C11 0.099(8) 0.107(10) 0.049(5) -0.028(6) 0.040(6) -0.015(7) C12 0.058(6) 0.051(6) 0.067(6) -0.002(5) -0.011(5) 0.010(5) C13 0.048(4) 0.027(4) 0.026(4) 0.000(3) 0.002(3) -0.008(4) C14 0.041(5) 0.070(7) 0.063(6) 0.021(5) -0.001(4) -0.006(5) C15 0.095(7) 0.042(6) 0.037(4) -0.008(4) 0.016(5) -0.002(5) C16 0.032(4) 0.020(4) 0.068(5) 0.007(3) 0.029(4) 0.004(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 2.018(9) . ? Au1 Cl3 2.247(3) . ? Au1 Cl2 2.277(3) . ? Au1 Cl1 2.311(3) . ? C1 N2 1.348(7) 4_565 ? C1 N2 1.348(7) . ? N2 C3 1.398(8) . ? N2 C4 1.435(8) . ? C3 C3 1.343(13) 4_565 ? C3 C16 1.496(9) . ? C4 C9 1.398(9) . ? C4 C5 1.407(8) . ? C5 C6 1.405(9) . ? C5 C10 1.530(9) . ? C6 C7 1.353(9) . ? C6 H6A 0.9500 . ? C7 C8 1.381(9) . ? C7 H7A 0.9500 . ? C8 C9 1.386(9) . ? C8 H8A 0.9500 . ? C9 C13 1.507(9) . ? C10 C12 1.501(11) . ? C10 C11 1.550(11) . ? C10 H10A 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.542(10) . ? C13 C14 1.563(11) . ? C13 H13A 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 Cl4 1.805(11) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? 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 Cl3 92.7(2) . . ? C1 Au1 Cl2 87.7(2) . . ? Cl3 Au1 Cl2 179.60(9) . . ? C1 Au1 Cl1 177.6(2) . . ? Cl3 Au1 Cl1 89.66(10) . . ? Cl2 Au1 Cl1 89.94(10) . . ? N2 C1 N2 107.7(7) 4_565 . ? N2 C1 Au1 126.0(4) 4_565 . ? N2 C1 Au1 126.0(4) . . ? C1 N2 C3 108.7(5) . . ? C1 N2 C4 127.6(5) . . ? C3 N2 C4 123.4(5) . . ? C3 C3 N2 107.4(3) 4_565 . ? C3 C3 C16 128.7(4) 4_565 . ? N2 C3 C16 123.9(6) . . ? C9 C4 C5 122.2(6) . . ? C9 C4 N2 119.7(5) . . ? C5 C4 N2 118.0(5) . . ? C6 C5 C4 117.3(6) . . ? C6 C5 C10 119.9(6) . . ? C4 C5 C10 122.7(6) . . ? C7 C6 C5 120.9(6) . . ? C7 C6 H6A 119.5 . . ? C5 C6 H6A 119.5 . . ? C6 C7 C8 120.9(7) . . ? C6 C7 H7A 119.5 . . ? C8 C7 H7A 119.5 . . ? C7 C8 C9 121.3(6) . . ? C7 C8 H8A 119.3 . . ? C9 C8 H8A 119.3 . . ? C8 C9 C4 117.4(6) . . ? C8 C9 C13 119.6(6) . . ? C4 C9 C13 123.0(6) . . ? C12 C10 C5 112.8(7) . . ? C12 C10 C11 108.3(6) . . ? C5 C10 C11 110.5(6) . . ? C12 C10 H10A 108.4 . . ? C5 C10 H10A 108.4 . . ? C11 C10 H10A 108.4 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 C15 112.0(7) . . ? C9 C13 C14 110.8(6) . . ? C15 C13 C14 108.0(6) . . ? C9 C13 H13A 108.6 . . ? C15 C13 H13A 108.6 . . ? C14 C13 H13A 108.6 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C3 C16 Cl4 108.9(6) . . ? C3 C16 H16A 109.9 . . ? Cl4 C16 H16A 109.9 . . ? C3 C16 H16B 109.9 . . ? Cl4 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl3 Au1 C1 N2 -93.2(6) . . . 4_565 ? Cl2 Au1 C1 N2 86.8(6) . . . 4_565 ? Cl1 Au1 C1 N2 86.8(6) . . . 4_565 ? Cl3 Au1 C1 N2 93.2(6) . . . . ? Cl2 Au1 C1 N2 -86.8(6) . . . . ? Cl1 Au1 C1 N2 -86.8(6) . . . . ? N2 C1 N2 C3 -2.5(8) 4_565 . . . ? Au1 C1 N2 C3 172.0(5) . . . . ? N2 C1 N2 C4 172.0(4) 4_565 . . . ? Au1 C1 N2 C4 -13.5(9) . . . . ? C1 N2 C3 C3 1.6(5) . . . 4_565 ? C4 N2 C3 C3 -173.3(4) . . . 4_565 ? C1 N2 C3 C16 -177.7(6) . . . . ? C4 N2 C3 C16 7.5(9) . . . . ? C1 N2 C4 C9 98.6(8) . . . . ? C3 N2 C4 C9 -87.5(7) . . . . ? C1 N2 C4 C5 -86.0(8) . . . . ? C3 N2 C4 C5 87.9(7) . . . . ? C9 C4 C5 C6 -0.5(9) . . . . ? N2 C4 C5 C6 -175.7(6) . . . . ? C9 C4 C5 C10 176.7(6) . . . . ? N2 C4 C5 C10 1.5(9) . . . . ? C4 C5 C6 C7 -0.1(10) . . . . ? C10 C5 C6 C7 -177.4(6) . . . . ? C5 C6 C7 C8 0.4(10) . . . . ? C6 C7 C8 C9 -0.1(10) . . . . ? C7 C8 C9 C4 -0.4(10) . . . . ? C7 C8 C9 C13 176.7(6) . . . . ? C5 C4 C9 C8 0.7(9) . . . . ? N2 C4 C9 C8 175.9(6) . . . . ? C5 C4 C9 C13 -176.3(6) . . . . ? N2 C4 C9 C13 -1.1(9) . . . . ? C6 C5 C10 C12 -44.7(9) . . . . ? C4 C5 C10 C12 138.1(7) . . . . ? C6 C5 C10 C11 76.7(9) . . . . ? C4 C5 C10 C11 -100.4(8) . . . . ? C8 C9 C13 C15 54.3(9) . . . . ? C4 C9 C13 C15 -128.8(7) . . . . ? C8 C9 C13 C14 -66.4(9) . . . . ? C4 C9 C13 C14 110.5(8) . . . . ? C3 C3 C16 Cl4 60.6(6) 4_565 . . . ? N2 C3 C16 Cl4 -120.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.703 _refine_diff_density_min -1.540 _refine_diff_density_rms 0.166