Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_autr_cor #Francesco Abbate, June 2001 _database_code_CSD 176425 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Orioli, Pierluigi' _publ_contact_author_name 'Prof Pierluigi Orioli' _publ_contact_author_address ; University of Florence Via Gino Capponi, 7 Firenze 50121 ITALY ; _publ_contact_author_email 'ORIOLI@CERM.UNIFI.IT' _publ_section_title ; Au2trien: a Dinuclear Gold(III) Complex with Unprecedented Structural Features ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common AuTrien _chemical_formula_sum 'C6 H17 Au2 Cl5 N4 O2' _chemical_formula_weight 748.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Au' 'Au' -4.4197 7.2980 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 11.504(5) _cell_length_b 11.909(5) _cell_length_c 13.031(5) _cell_angle_alpha 90.0(5) _cell_angle_beta 100.2(5) _cell_angle_gamma 90.0(5) _cell_volume 1757.2(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 64.21 _exptl_crystal_colour yellow _exptl_crystal_size_max 1 _exptl_crystal_size_min 0.8 _exptl_crystal_density_diffrn 2.829 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 37.982 _exptl_absorpt_correction_type PSI-scan _exptl_absorpt_process_details 'the absorption correction were performed with the Xprep program' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Rotating anode' _diffrn_radiation_monochromator 'Goebel mirror' _diffrn_measurement_device_type 'P4 Siemens' _diffrn_measurement_method Theta2Theta _diffrn_reflns_number 3628 _diffrn_reflns_av_R_equivalents 0.0531 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.90 _diffrn_reflns_theta_max 64.22 _reflns_number_total 2806 _reflns_number_gt 2537 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0592P)^2^+19.2689P] 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 0.00014(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2806 _refine_ls_number_parameters 228 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.1014 _refine_ls_wR_factor_gt 0.0983 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.893 _refine_ls_shift/su_mean 0.148 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 -0.21840(3) 0.05934(3) 0.29225(3) 0.01146(17) Uani 1 1 d . . . Au2 Au 0.05560(3) 0.13027(3) 0.23584(3) 0.01332(17) Uani 1 1 d . . . Cl3 Cl 0.2169(2) 0.0889(3) 0.1631(2) 0.0335(7) Uani 1 1 d . . . Cl2 Cl -0.0721(2) 0.0796(2) 0.08933(19) 0.0282(6) Uani 1 1 d . . . Cl1 Cl -0.0984(2) -0.0942(2) 0.3268(2) 0.0246(6) Uani 1 1 d . . . C6 C -0.1385(9) 0.2831(8) 0.2677(9) 0.019(2) Uani 1 1 d . . . H6A H -0.090(10) 0.346(11) 0.297(9) 0.023 Uiso 1 1 calc . . . H6B H -0.144(10) 0.284(10) 0.193(10) 0.023 Uiso 1 1 calc . . . N10 N 0.1614(8) 0.1737(8) 0.3711(7) 0.0205(19) Uani 1 1 d . . . H10A H 0.190(11) 0.112(11) 0.406(10) 0.025 Uiso 1 1 calc . . . H10B H 0.223(11) 0.215(11) 0.358(9) 0.025 Uiso 1 1 calc . . . C8 C -0.0287(10) 0.1814(10) 0.4246(8) 0.024(2) Uani 1 1 d . . . H8A H -0.018(11) 0.107(11) 0.454(10) 0.028 Uiso 1 1 calc . . . H8B H -0.081(11) 0.223(11) 0.462(10) 0.028 Uiso 1 1 calc . . . C5 C -0.2600(11) 0.2937(9) 0.2945(9) 0.026(2) Uani 1 1 d . . . H5A H -0.255(11) 0.298(11) 0.369(11) 0.031 Uiso 1 1 calc . . . H5B H -0.299(11) 0.361(12) 0.263(10) 0.031 Uiso 1 1 calc . . . N7 N -0.0823(8) 0.1741(7) 0.3112(6) 0.0167(18) Uani 1 1 d . . . N1 N -0.3728(8) -0.0286(8) 0.2810(8) 0.023(2) Uani 1 1 d . . . H1A H -0.375(11) -0.083(12) 0.233(10) 0.028 Uiso 1 1 calc . . . H1B H -0.377(11) -0.062(11) 0.343(11) 0.028 Uiso 1 1 calc . . . N4 N -0.3256(8) 0.1922(7) 0.2522(7) 0.0193(18) Uani 1 1 d . . . C2 C -0.4759(12) 0.0492(12) 0.2516(11) 0.035(3) Uani 1 1 d . . . H2A H -0.542(13) 0.024(13) 0.283(11) 0.042 Uiso 1 1 calc . . . H2B H -0.501(12) 0.050(12) 0.176(12) 0.042 Uiso 1 1 calc . . . C3 C -0.4400(11) 0.1659(11) 0.2898(11) 0.031(3) Uani 1 1 d . . . H3A H -0.428(12) 0.169(12) 0.365(12) 0.037 Uiso 1 1 calc . . . H3B H -0.501(12) 0.220(12) 0.262(10) 0.037 Uiso 1 1 calc . . . C9 C 0.0902(10) 0.2403(9) 0.4356(9) 0.022(2) Uani 1 1 d . . . H9A H 0.080(10) 0.317(11) 0.410(9) 0.026 Uiso 1 1 calc . . . H9B H 0.129(11) 0.242(11) 0.508(10) 0.026 Uiso 1 1 calc . . . Cl4 Cl 0.2645(3) -0.0557(2) 0.4717(2) 0.0358(7) Uani 1 1 d . . . Cl5 Cl -0.3774(3) -0.1577(3) 0.0719(2) 0.0361(7) Uani 1 1 d . . . O1 O -0.3573(9) 0.1209(9) 0.0339(8) 0.051(4) Uani 1.00(3) 1 d . . . O2 O -0.5033(9) -0.1598(9) 0.4066(8) 0.051(4) Uani 1.00(3) 1 d . . . H4 H -0.326(8) 0.196(8) 0.176(8) 0.00(3) Uiso 1.0(3) 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.0118(3) 0.0112(2) 0.0113(2) -0.00028(13) 0.00180(16) 0.00025(14) Au2 0.0139(3) 0.0131(2) 0.0131(2) 0.00231(14) 0.00258(16) 0.00085(15) Cl3 0.0221(15) 0.0438(16) 0.0384(16) 0.0088(13) 0.0160(12) 0.0138(13) Cl2 0.0308(16) 0.0406(15) 0.0121(11) -0.0067(11) 0.0009(10) -0.0062(12) Cl1 0.0294(15) 0.0164(12) 0.0282(13) 0.0034(10) 0.0055(11) 0.0091(10) C6 0.016(6) 0.010(5) 0.034(6) -0.005(4) 0.009(4) -0.008(4) N10 0.017(5) 0.023(5) 0.020(5) 0.000(4) -0.002(4) -0.006(4) C8 0.023(6) 0.037(7) 0.010(5) 0.007(5) 0.002(4) -0.006(5) C5 0.036(7) 0.016(5) 0.029(6) 0.003(5) 0.011(5) 0.001(5) N7 0.023(5) 0.012(4) 0.015(4) -0.004(3) 0.002(3) -0.003(3) N1 0.016(5) 0.028(5) 0.025(5) 0.001(4) 0.002(4) -0.002(4) N4 0.020(5) 0.020(4) 0.018(5) 0.005(4) 0.003(4) 0.002(4) C2 0.021(7) 0.044(8) 0.040(8) 0.017(6) 0.004(6) 0.012(6) C3 0.025(7) 0.033(6) 0.038(7) 0.001(5) 0.015(5) 0.013(5) C9 0.025(6) 0.016(5) 0.020(6) -0.002(4) -0.005(4) -0.010(4) Cl4 0.0435(19) 0.0356(16) 0.0272(15) 0.0030(12) 0.0033(13) 0.0122(13) Cl5 0.0245(16) 0.0414(16) 0.0393(16) -0.0083(13) -0.0029(12) 0.0102(13) O1 0.046(7) 0.062(7) 0.039(6) 0.000(5) -0.006(5) 0.011(5) O2 0.057(8) 0.051(6) 0.048(7) 0.011(5) 0.017(5) -0.006(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 Au1 N4 2.017(9) . ? Au1 N1 2.045(9) . ? Au1 N7 2.060(8) . ? Au1 Cl1 2.287(3) . ? Au2 N10 2.024(9) . ? Au2 N7 2.074(8) . ? Au2 Cl2 2.275(3) . ? Au2 Cl3 2.282(3) . ? C6 C5 1.505(15) . ? C6 N7 1.515(13) . ? N10 C9 1.500(14) . ? C8 N7 1.499(13) . ? C8 C9 1.521(15) . ? C5 N4 1.479(14) . ? N1 C2 1.500(15) . ? N4 C3 1.515(14) . ? C2 C3 1.509(19) . ? 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 N4 Au1 N1 84.2(4) . . ? N4 Au1 N7 85.9(3) . . ? N1 Au1 N7 168.7(4) . . ? N4 Au1 Cl1 176.4(3) . . ? N1 Au1 Cl1 95.2(3) . . ? N7 Au1 Cl1 95.0(2) . . ? N10 Au2 N7 85.2(4) . . ? N10 Au2 Cl2 176.6(3) . . ? N7 Au2 Cl2 91.7(2) . . ? N10 Au2 Cl3 90.5(3) . . ? N7 Au2 Cl3 175.6(2) . . ? Cl2 Au2 Cl3 92.63(11) . . ? C5 C6 N7 109.8(8) . . ? C9 N10 Au2 108.6(7) . . ? N7 C8 C9 109.0(8) . . ? N4 C5 C6 106.2(8) . . ? C8 N7 C6 113.1(8) . . ? C8 N7 Au1 109.1(6) . . ? C6 N7 Au1 104.9(6) . . ? C8 N7 Au2 105.4(6) . . ? C6 N7 Au2 110.5(6) . . ? Au1 N7 Au2 113.9(4) . . ? C2 N1 Au1 109.8(8) . . ? C5 N4 C3 117.6(9) . . ? C5 N4 Au1 107.2(7) . . ? C3 N4 Au1 106.3(7) . . ? N1 C2 C3 109.1(11) . . ? C2 C3 N4 106.6(9) . . ? N10 C9 C8 105.9(8) . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 64.22 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 1.748 _refine_diff_density_min -1.834 _refine_diff_density_rms 0.300