# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_aus8tl _refine_special_details ; Disorder of the C8, C9, C11 and C12 methylene groups of the macrocycle was modelled in terms of alternative sites. Distance restraints of 1.82(1) and 1.52(1) Angstroms were applied to all macrocyclic S---C and all C---C distances, respectively. The occupancies of the two alternative orientations refined to 0.53(2) and 0.47(2), respectively. Rigid-bond and similarity restraints were applied to the displacement parameters. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H16 Au Cl10 S4 Tl' _chemical_formula_sum 'C20 H16 Au Cl10 S4 Tl' _chemical_formula_weight 1140.40 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6829(11) _cell_length_b 11.9086(10) _cell_length_c 14.4564(12) _cell_angle_alpha 66.786(8) _cell_angle_beta 78.615(8) _cell_angle_gamma 66.326(9) _cell_volume 1546.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3825 _cell_measurement_theta_min 3.067 _cell_measurement_theta_max 27.91 _exptl_crystal_description tablet _exptl_crystal_colour 'luminescent green' _exptl_crystal_size_max 0.1401 _exptl_crystal_size_mid 0.095 _exptl_crystal_size_min 0.033 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.449 _exptl_crystal_density_method ? _exptl_crystal_F_000 1060 _exptl_absorpt_coefficient_mu 11.091 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.350 _exptl_absorpt_correction_T_max 0.691 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'microfocus sealed tube' _diffrn_radiation_monochromator 'mirror optics' _diffrn_measurement_device_type 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1592 _diffrn_reflns_number 8439 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_av_sigmaI/netI 0.056 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 25.10 _reflns_number_total 5438 _reflns_number_gt 4340 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON (Spek, 2009)' _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^)+(0.059P)^2^+7.709P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5438 _refine_ls_number_parameters 322 _refine_ls_number_restraints 309 _refine_ls_R_factor_all 0.0676 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.136 _refine_ls_wR_factor_gt 0.122 _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_restrained_S_all 1.17 _refine_ls_shift/su_max 0.006 _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 Tl1 Tl 0.17467(8) 0.30635(6) 0.09796(5) 0.0841(3) Uani 1 1 d U . . Au1 Au 0.34272(5) 0.09977(5) 0.02088(3) 0.0471(2) Uani 1 1 d U . . C20 C 0.3847(11) -0.0039(11) 0.1703(9) 0.045(2) Uani 1 1 d U . . C21 C 0.3220(12) -0.0917(12) 0.2300(9) 0.047(2) Uani 1 1 d U . . C22 C 0.3429(13) -0.1620(12) 0.3322(9) 0.051(2) Uani 1 1 d U . . C23 C 0.4322(13) -0.1436(12) 0.3781(9) 0.052(2) Uani 1 1 d U . . C24 C 0.5005(13) -0.0584(12) 0.3214(9) 0.051(2) Uani 1 1 d U . . C25 C 0.4750(12) 0.0079(12) 0.2201(9) 0.050(2) Uani 1 1 d U . . Cl21 Cl 0.2024(3) -0.1090(3) 0.1757(3) 0.0623(9) Uani 1 1 d U . . Cl22 Cl 0.2582(4) -0.2660(4) 0.4022(3) 0.0777(11) Uani 1 1 d U . . Cl23 Cl 0.4595(5) -0.2274(4) 0.5045(3) 0.0865(12) Uani 1 1 d U . . Cl24 Cl 0.6129(4) -0.0384(4) 0.3785(3) 0.0789(11) Uani 1 1 d U . . Cl25 Cl 0.5559(4) 0.1196(4) 0.1502(3) 0.0686(9) Uani 1 1 d U . . C30 C 0.2869(13) 0.2115(12) -0.1243(9) 0.051(2) Uani 1 1 d U . . C31 C 0.3400(13) 0.3068(12) -0.1865(9) 0.051(2) Uani 1 1 d U . . C32 C 0.3064(13) 0.3804(12) -0.2858(9) 0.053(2) Uani 1 1 d U . . C33 C 0.2129(13) 0.3645(13) -0.3275(9) 0.056(3) Uani 1 1 d U . . C34 C 0.1520(13) 0.2738(13) -0.2665(9) 0.054(2) Uani 1 1 d U . . C35 C 0.1901(12) 0.1992(12) -0.1695(9) 0.051(2) Uani 1 1 d U . . Cl31 Cl 0.4560(4) 0.3335(3) -0.1365(3) 0.0647(9) Uani 1 1 d U . . Cl32 Cl 0.3875(4) 0.4882(4) -0.3619(3) 0.0715(10) Uani 1 1 d U . . Cl33 Cl 0.1651(4) 0.4592(4) -0.4497(3) 0.0790(11) Uani 1 1 d U . . Cl34 Cl 0.0300(4) 0.2564(4) -0.3184(3) 0.0784(11) Uani 1 1 d U . . Cl35 Cl 0.1095(4) 0.0888(4) -0.0969(3) 0.0717(10) Uani 1 1 d U . . S1 S -0.1563(7) 0.3770(6) 0.0807(6) 0.139(2) Uani 1 1 d DU . . C2 C -0.227(2) 0.3022(18) 0.2035(12) 0.139(5) Uani 1 1 d DU . . H2A H -0.2408 0.3554 0.2437 0.166 Uiso 1 1 calc R . . H2B H -0.3163 0.3059 0.1946 0.166 Uiso 1 1 calc R . . C3 C -0.1454(14) 0.1631(18) 0.2629(17) 0.128(5) Uani 1 1 d DU . . H3A H -0.1380 0.1084 0.2255 0.154 Uiso 1 1 calc R . . H3B H -0.1962 0.1356 0.3257 0.154 Uiso 1 1 calc R . . S4 S 0.0261(6) 0.1319(6) 0.2923(5) 0.1150(17) Uani 1 1 d DU . . C5 C -0.013(2) 0.230(2) 0.3709(16) 0.133(4) Uani 1 1 d DU . . H5A H -0.0519 0.3225 0.3312 0.160 Uiso 1 1 calc R . . H5B H -0.0788 0.2082 0.4250 0.160 Uiso 1 1 calc R . . C6 C 0.1194(17) 0.201(2) 0.4137(13) 0.143(5) Uani 1 1 d DU A . H6A H 0.1558 0.1077 0.4523 0.172 Uiso 1 1 calc R . . H6B H 0.0986 0.2467 0.4604 0.172 Uiso 1 1 calc R . . S7 S 0.2529(7) 0.2428(8) 0.3243(5) 0.144(2) Uani 1 1 d DU . . C8 C 0.235(6) 0.402(3) 0.321(4) 0.135(5) Uiso 0.47(2) 1 d PDU A 1 H8A H 0.1374 0.4500 0.3239 0.162 Uiso 0.47(2) 1 calc PR A 1 H8B H 0.2678 0.3861 0.3849 0.162 Uiso 0.47(2) 1 calc PR A 1 C8' C 0.177(4) 0.4181(15) 0.296(4) 0.138(5) Uiso 0.53(2) 1 d PDU A 2 H8'A H 0.1125 0.4639 0.2425 0.166 Uiso 0.53(2) 1 calc PR A 2 H8'B H 0.1386 0.4435 0.3543 0.166 Uiso 0.53(2) 1 calc PR A 2 C9 C 0.295(6) 0.499(5) 0.242(2) 0.136(5) Uiso 0.47(2) 1 d PDU A 1 H9A H 0.3722 0.4967 0.2701 0.163 Uiso 0.47(2) 1 calc PR A 1 H9B H 0.2265 0.5868 0.2288 0.163 Uiso 0.47(2) 1 calc PR A 1 C9' C 0.321(4) 0.422(5) 0.2610(11) 0.138(5) Uiso 0.53(2) 1 d PDU A 2 H9'A H 0.3882 0.3355 0.2926 0.165 Uiso 0.53(2) 1 calc PR A 2 H9'B H 0.3347 0.4826 0.2835 0.165 Uiso 0.53(2) 1 calc PR A 2 S10 S 0.3514(6) 0.4701(6) 0.1240(5) 0.1098(16) Uani 1 1 d DU . . C11 C 0.297(4) 0.638(2) 0.035(3) 0.116(5) Uiso 0.47(2) 1 d PDU A 1 H11A H 0.3138 0.6901 0.0650 0.139 Uiso 0.47(2) 1 calc PR A 1 H11B H 0.3585 0.6382 -0.0242 0.139 Uiso 0.47(2) 1 calc PR A 1 C11' C 0.207(3) 0.624(2) 0.097(2) 0.117(5) Uiso 0.53(2) 1 d PDU A 2 H11C H 0.1211 0.6101 0.1155 0.140 Uiso 0.53(2) 1 calc PR A 2 H11D H 0.2119 0.6765 0.1329 0.140 Uiso 0.53(2) 1 calc PR A 2 C12 C 0.152(4) 0.712(4) -0.003(3) 0.121(7) Uiso 0.47(2) 1 d PDU . 1 H12A H 0.1371 0.8038 -0.0423 0.146 Uiso 0.47(2) 1 calc PR A 1 H12B H 0.0834 0.7059 0.0516 0.146 Uiso 0.47(2) 1 calc PR A 1 C12' C 0.226(5) 0.688(4) -0.016(2) 0.121(7) Uiso 0.53(2) 1 d PDU . 2 H12C H 0.3220 0.6712 -0.0348 0.146 Uiso 0.53(2) 1 calc PR A 2 H12D H 0.1784 0.7823 -0.0355 0.146 Uiso 0.53(2) 1 calc PR A 2 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 Tl1 0.1050(6) 0.0693(4) 0.0805(5) -0.0385(4) -0.0133(4) -0.0175(4) Au1 0.0523(3) 0.0486(3) 0.0393(3) -0.0079(2) -0.00243(19) -0.0241(2) C20 0.043(5) 0.046(5) 0.043(5) -0.010(4) 0.003(4) -0.020(4) C21 0.048(5) 0.050(5) 0.041(5) -0.007(4) -0.007(4) -0.021(4) C22 0.055(5) 0.051(5) 0.044(5) -0.005(4) -0.005(4) -0.026(4) C23 0.060(6) 0.054(5) 0.042(5) -0.012(4) -0.008(4) -0.022(4) C24 0.054(5) 0.054(5) 0.049(5) -0.020(4) -0.010(4) -0.019(4) C25 0.048(5) 0.045(5) 0.052(5) -0.010(4) -0.003(4) -0.019(4) Cl21 0.064(2) 0.072(2) 0.0580(19) -0.0062(17) -0.0134(15) -0.0426(17) Cl22 0.086(3) 0.084(3) 0.058(2) 0.0100(19) -0.0109(18) -0.055(2) Cl23 0.119(3) 0.092(3) 0.046(2) 0.0019(19) -0.028(2) -0.051(3) Cl24 0.088(3) 0.091(3) 0.078(3) -0.026(2) -0.027(2) -0.044(2) Cl25 0.073(2) 0.070(2) 0.073(2) -0.0120(18) -0.0053(18) -0.0469(19) C30 0.060(6) 0.051(5) 0.044(5) -0.016(4) 0.001(4) -0.024(4) C31 0.062(6) 0.048(5) 0.043(5) -0.013(4) -0.002(4) -0.025(4) C32 0.063(6) 0.052(5) 0.043(5) -0.008(4) 0.001(4) -0.031(4) C33 0.061(6) 0.064(6) 0.039(5) -0.007(4) -0.004(4) -0.030(5) C34 0.055(5) 0.071(6) 0.045(5) -0.018(4) 0.001(4) -0.035(5) C35 0.053(5) 0.059(5) 0.044(5) -0.011(4) 0.002(4) -0.033(4) Cl31 0.079(2) 0.068(2) 0.059(2) -0.0127(17) -0.0130(17) -0.0432(18) Cl32 0.095(3) 0.068(2) 0.054(2) -0.0010(17) -0.0027(18) -0.052(2) Cl33 0.094(3) 0.095(3) 0.0438(19) -0.0042(19) -0.0152(18) -0.043(2) Cl34 0.069(2) 0.113(3) 0.064(2) -0.017(2) -0.0129(18) -0.053(2) Cl35 0.066(2) 0.087(3) 0.062(2) -0.0025(19) -0.0042(17) -0.049(2) S1 0.138(5) 0.103(4) 0.152(6) -0.022(4) -0.026(4) -0.033(4) C2 0.130(8) 0.114(8) 0.149(9) -0.037(7) -0.006(8) -0.029(7) C3 0.118(7) 0.110(8) 0.138(8) -0.038(7) 0.011(7) -0.035(7) S4 0.113(4) 0.101(3) 0.115(4) -0.045(3) 0.018(3) -0.025(3) C5 0.134(8) 0.137(8) 0.110(8) -0.056(6) 0.007(7) -0.024(8) C6 0.142(8) 0.157(9) 0.108(8) -0.058(7) -0.008(7) -0.019(8) S7 0.137(4) 0.163(5) 0.113(4) -0.064(4) -0.017(3) -0.015(4) S10 0.102(3) 0.125(4) 0.114(3) -0.047(3) -0.015(3) -0.043(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 Tl1 Au1 2.8881(8) . ? Tl1 S1 3.327(7) . ? Tl1 S4 3.319(6) . ? Tl1 S7 3.256(7) . ? Tl1 S10 3.366(6) . ? Tl1 S1 3.587(7) 2_565 ? Au1 C30 2.046(12) . ? Au1 C20 2.056(11) . ? Au1 Au1 3.3497(11) 2_655 ? C20 C21 1.381(15) . ? C20 C25 1.391(16) . ? C21 C22 1.392(16) . ? C21 Cl21 1.740(12) . ? C22 C23 1.389(17) . ? C22 Cl22 1.711(12) . ? C23 C24 1.392(17) . ? C23 Cl23 1.721(12) . ? C24 C25 1.384(17) . ? C24 Cl24 1.720(12) . ? C25 Cl25 1.748(12) . ? C30 C31 1.389(16) . ? C30 C35 1.408(17) . ? C31 C32 1.385(17) . ? C31 Cl31 1.734(13) . ? C32 C33 1.370(17) . ? C32 Cl32 1.736(12) . ? C33 C34 1.398(17) . ? C33 Cl33 1.726(13) . ? C34 C35 1.369(17) . ? C34 Cl34 1.741(12) . ? C35 Cl35 1.742(12) . ? S1 C2 1.810(11) . ? S1 C12 1.810(11) 2_565 ? S1 C12' 1.828(11) 2_565 ? C2 C3 1.502(11) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 S4 1.820(10) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? S4 C5 1.818(10) . ? C5 C6 1.512(11) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 S7 1.814(11) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? S7 C8' 1.811(11) . ? S7 C8 1.812(11) . ? C8 C9 1.521(12) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8' C9' 1.538(12) . ? C8' H8'A 0.9700 . ? C8' H8'B 0.9700 . ? C9 S10 1.818(11) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9' S10 1.832(11) . ? C9' H9'A 0.9700 . ? C9' H9'B 0.9700 . ? S10 C11' 1.814(11) . ? S10 C11 1.824(11) . ? C11 C12 1.525(12) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11' C12' 1.520(12) . ? C11' H11C 0.9700 . ? C11' H11D 0.9700 . ? C12 S1 1.810(11) 2_565 ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12' S1 1.828(11) 2_565 ? C12' H12C 0.9700 . ? C12' H12D 0.9700 . ? 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 Au1 Tl1 S7 111.99(13) . . ? Au1 Tl1 S4 97.59(10) . . ? Au1 Tl1 S1 111.23(13) . . ? Au1 Tl1 S1 111.89(13) . 2_565 ? Au1 Tl1 S10 112.96(10) . . ? S1 Tl1 S1 91.58(17) . 2_565 ? S1 Tl1 S10 133.34(16) . . ? S4 Tl1 S1 64.04(16) . . ? S4 Tl1 S1 147.43(15) . 2_565 ? S7 Tl1 S1 112.90(19) . . ? S7 Tl1 S1 115.71(19) . 2_565 ? S7 Tl1 S4 61.56(19) . . ? S7 Tl1 S10 62.25(18) . . ? S4 Tl1 S10 122.65(15) . . ? S10 Tl1 S1 58.46(16) . 2_565 ? C30 Au1 C20 175.6(5) . . ? C30 Au1 Tl1 93.7(3) . . ? C20 Au1 Tl1 82.4(3) . . ? C30 Au1 Au1 100.1(3) . 2_655 ? C20 Au1 Au1 84.2(3) . 2_655 ? Tl1 Au1 Au1 147.89(3) . 2_655 ? C21 C20 C25 114.4(11) . . ? C21 C20 Au1 121.4(9) . . ? C25 C20 Au1 124.2(8) . . ? C20 C21 C22 124.3(11) . . ? C20 C21 Cl21 117.9(9) . . ? C22 C21 Cl21 117.8(9) . . ? C23 C22 C21 118.5(11) . . ? C23 C22 Cl22 119.8(9) . . ? C21 C22 Cl22 121.7(9) . . ? C22 C23 C24 119.9(11) . . ? C22 C23 Cl23 120.0(10) . . ? C24 C23 Cl23 120.1(9) . . ? C25 C24 C23 118.4(11) . . ? C25 C24 Cl24 122.1(10) . . ? C23 C24 Cl24 119.5(9) . . ? C24 C25 C20 124.5(11) . . ? C24 C25 Cl25 118.3(9) . . ? C20 C25 Cl25 117.1(9) . . ? C31 C30 C35 114.1(11) . . ? C31 C30 Au1 123.1(9) . . ? C35 C30 Au1 122.8(9) . . ? C32 C31 C30 123.7(12) . . ? C32 C31 Cl31 118.5(9) . . ? C30 C31 Cl31 117.7(9) . . ? C33 C32 C31 120.3(11) . . ? C33 C32 Cl32 118.6(10) . . ? C31 C32 Cl32 121.0(10) . . ? C32 C33 C34 118.1(11) . . ? C32 C33 Cl33 121.0(10) . . ? C34 C33 Cl33 120.8(10) . . ? C35 C34 C33 120.5(11) . . ? C35 C34 Cl34 121.4(9) . . ? C33 C34 Cl34 118.1(10) . . ? C34 C35 C30 123.1(11) . . ? C34 C35 Cl35 118.3(9) . . ? C30 C35 Cl35 118.5(9) . . ? C2 S1 C12 107(2) . 2_565 ? C2 S1 C12' 94.3(14) . 2_565 ? C3 C2 S1 117.4(15) . . ? C3 C2 H2A 108.0 . . ? S1 C2 H2A 108.0 . . ? C3 C2 H2B 108.0 . . ? S1 C2 H2B 108.0 . . ? H2A C2 H2B 107.2 . . ? C2 C3 S4 116.2(15) . . ? C2 C3 H3A 108.2 . . ? S4 C3 H3A 108.2 . . ? C2 C3 H3B 108.2 . . ? S4 C3 H3B 108.2 . . ? H3A C3 H3B 107.4 . . ? C5 S4 C3 100.6(10) . . ? C6 C5 S4 107.3(14) . . ? C6 C5 H5A 110.3 . . ? S4 C5 H5A 110.3 . . ? C6 C5 H5B 110.3 . . ? S4 C5 H5B 110.3 . . ? H5A C5 H5B 108.5 . . ? C5 C6 S7 116.9(15) . . ? C5 C6 H6A 108.1 . . ? S7 C6 H6A 108.1 . . ? C5 C6 H6B 108.1 . . ? S7 C6 H6B 108.1 . . ? H6A C6 H6B 107.3 . . ? C8' S7 C6 97.0(16) . . ? C8 S7 C6 105.0(18) . . ? C9 C8 S7 128(3) . . ? C9 C8 H8A 105.3 . . ? S7 C8 H8A 105.3 . . ? C9 C8 H8B 105.3 . . ? S7 C8 H8B 105.3 . . ? H8A C8 H8B 106.0 . . ? C9' C8' S7 87(2) . . ? C9' C8' H8'A 114.2 . . ? S7 C8' H8'A 114.1 . . ? C9' C8' H8'B 114.2 . . ? S7 C8' H8'B 114.2 . . ? H8'A C8' H8'B 111.3 . . ? C8 C9 S10 114(3) . . ? C8 C9 H9A 108.6 . . ? S10 C9 H9A 108.6 . . ? C8 C9 H9B 108.7 . . ? S10 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? C8' C9' S10 113(3) . . ? C8' C9' H9'A 109.0 . . ? S10 C9' H9'A 109.0 . . ? C8' C9' H9'B 109.0 . . ? S10 C9' H9'B 109.0 . . ? H9'A C9' H9'B 107.8 . . ? C9 S10 C11 100(2) . . ? C11' S10 C9' 94.6(19) . . ? C11 S10 C9' 125(2) . . ? C12 C11 S10 123(3) . . ? C12 C11 H11A 106.6 . . ? S10 C11 H11A 106.6 . . ? C12 C11 H11B 106.6 . . ? S10 C11 H11B 106.6 . . ? H11A C11 H11B 106.6 . . ? C12' C11' S10 102(3) . . ? C12' C11' H11C 111.3 . . ? S10 C11' H11C 111.3 . . ? C12' C11' H11D 111.3 . . ? S10 C11' H11D 111.3 . . ? H11C C11' H11D 109.2 . . ? C11 C12 S1 100(3) . 2_565 ? C11 C12 H12A 111.9 . . ? S1 C12 H12A 111.9 2_565 . ? C11 C12 H12B 111.9 . . ? S1 C12 H12B 111.9 2_565 . ? H12A C12 H12B 109.6 . . ? C11' C12' S1 110(2) . 2_565 ? C11' C12' H12C 109.7 . . ? S1 C12' H12C 109.7 2_565 . ? C11' C12' H12D 109.7 . . ? S1 C12' H12D 109.7 2_565 . ? H12C C12' H12D 108.2 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.98 _refine_diff_density_min -1.57 _refine_diff_density_rms 0.16 _database_code_depnum_ccdc_archive 'CCDC 935229' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_t86 _audit_creation_date 2013-02-13T10:30:30-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'RD73 thf/hx' _chemical_formula_moiety 'C36 H24 Au2 F20 S6 Tl2' _chemical_formula_sum 'C36 H24 Au2 F20 S6 Tl2' _chemical_formula_weight 1831.58 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 10.9933(3) _cell_length_b 11.7372(4) _cell_length_c 17.4726(6) _cell_angle_alpha 90 _cell_angle_beta 92.688(2) _cell_angle_gamma 90 _cell_volume 2252.02(13) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 1724 _cell_measurement_theta_min 1.85 _cell_measurement_theta_max 27.54 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 2.701 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 14.019 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.0224 _exptl_absorpt_correction_T_max 0.0578 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.0746993 _diffrn_orient_matrix_ub_12 -0.0388218 _diffrn_orient_matrix_ub_13 0.0175802 _diffrn_orient_matrix_ub_21 0.0098329 _diffrn_orient_matrix_ub_22 -0.0610803 _diffrn_orient_matrix_ub_23 -0.0391288 _diffrn_orient_matrix_ub_31 0.051148 _diffrn_orient_matrix_ub_32 -0.0449552 _diffrn_orient_matrix_ub_33 0.0379823 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0803 _diffrn_reflns_av_unetI/netI 0.0424 _diffrn_reflns_number 29515 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 27.54 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 5174 _reflns_number_gt 4437 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; FLAT and SAME restraints were applied to both aryl groups. DELU was applied to all light atoms: C and F. 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^ > 2\s(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^)+(0.0643P)^2^+2.1819P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.00263(16) _refine_ls_number_reflns 5174 _refine_ls_number_parameters 299 _refine_ls_number_restraints 97 _refine_ls_R_factor_all 0.0488 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.109 _refine_ls_wR_factor_gt 0.1042 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.562 _refine_diff_density_min -2.115 _refine_diff_density_rms 0.251 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Au Au 0.42740(2) 0.39353(2) 0.041216(16) 0.03047(11) Uani 1 1 d . . . Tl Tl 0.22188(2) 0.22991(2) 0.072951(15) 0.03170(11) Uani 1 1 d . . . C1 C 0.2974(6) 0.5192(6) 0.0444(3) 0.0306(14) Uani 1 1 d DU . . C2 C 0.1998(6) 0.5276(6) -0.0086(4) 0.0351(15) Uani 1 1 d DU . . C3 C 0.1162(6) 0.6128(6) -0.0078(4) 0.0360(16) Uani 1 1 d DU . . C4 C 0.1256(7) 0.6939(7) 0.0468(4) 0.0402(17) Uani 1 1 d DU . . C5 C 0.2179(6) 0.6904(6) 0.1008(4) 0.0353(15) Uani 1 1 d DU . . C6 C 0.3012(6) 0.6034(6) 0.0988(4) 0.0319(15) Uani 1 1 d DU . . F1 F 0.1851(5) 0.4464(4) -0.0635(3) 0.0500(12) Uani 1 1 d DU . . F2 F 0.0243(5) 0.6154(4) -0.0628(3) 0.0545(14) Uani 1 1 d DU . . F3 F 0.0418(5) 0.7793(4) 0.0460(4) 0.0586(15) Uani 1 1 d DU . . F4 F 0.2281(5) 0.7728(4) 0.1549(3) 0.0538(13) Uani 1 1 d DU . . F5 F 0.3921(5) 0.6050(5) 0.1540(3) 0.0548(14) Uani 1 1 d DU . . C11 C 0.5513(6) 0.2627(6) 0.0415(4) 0.0305(14) Uani 1 1 d DU . . C12 C 0.6464(6) 0.2532(6) 0.0947(4) 0.0333(15) Uani 1 1 d DU . . C13 C 0.7306(6) 0.1660(6) 0.0961(5) 0.0412(18) Uani 1 1 d DU . . C14 C 0.7212(7) 0.0819(6) 0.0413(4) 0.0415(17) Uani 1 1 d DU . . C15 C 0.6290(7) 0.0870(6) -0.0137(5) 0.0408(17) Uani 1 1 d DU . . C16 C 0.5454(7) 0.1763(7) -0.0129(4) 0.0364(16) Uani 1 1 d DU . . F6 F 0.6612(4) 0.3331(4) 0.1501(3) 0.0495(12) Uani 1 1 d DU . . F7 F 0.8209(5) 0.1622(5) 0.1503(4) 0.0697(18) Uani 1 1 d DU . . F8 F 0.8024(5) -0.0036(5) 0.0423(4) 0.0646(16) Uani 1 1 d DU . . F9 F 0.6187(5) 0.0065(4) -0.0683(3) 0.0580(14) Uani 1 1 d DU . . F10 F 0.4531(5) 0.1729(5) -0.0666(3) 0.0566(14) Uani 1 1 d DU . . S1 S 0.10044(16) 0.09587(16) 0.20300(12) 0.0328(4) Uani 1 1 d . . . S2 S 0.16519(18) 0.38482(16) 0.20744(11) 0.0363(4) Uani 1 1 d . . . S3 S 0.40047(15) 0.18643(18) 0.20673(11) 0.0339(4) Uani 1 1 d . . . C21 C 0.0549(7) 0.1902(7) 0.2772(5) 0.0384(17) Uani 1 1 d U . . H21A H -0.0216 0.1635 0.2961 0.046 Uiso 1 1 calc R . . H21B H 0.1154 0.1872 0.3194 0.046 Uiso 1 1 calc R . . C22 C 0.0394(7) 0.3145(7) 0.2512(5) 0.0410(18) Uani 1 1 d U . . H22A H 0.0189 0.3591 0.2955 0.049 Uiso 1 1 calc R . . H22B H -0.0302 0.3177 0.215 0.049 Uiso 1 1 calc R . . C23 C 0.2902(7) 0.3730(7) 0.2798(5) 0.0398(18) Uani 1 1 d U . . H23A H 0.3069 0.448 0.3012 0.048 Uiso 1 1 calc R . . H23B H 0.2643 0.3246 0.3209 0.048 Uiso 1 1 calc R . . C24 C 0.4077(7) 0.3249(7) 0.2499(4) 0.0390(17) Uani 1 1 d U . . H24A H 0.4679 0.3224 0.2922 0.047 Uiso 1 1 calc R . . H24B H 0.4372 0.378 0.2124 0.047 Uiso 1 1 calc R . . C25 C 0.3357(7) 0.0982(7) 0.2790(5) 0.0396(18) Uani 1 1 d U . . H25A H 0.3992 0.0495 0.3014 0.048 Uiso 1 1 calc R . . H25B H 0.3073 0.1469 0.3193 0.048 Uiso 1 1 calc R . . C26 C 0.2306(7) 0.0239(7) 0.2493(5) 0.0386(17) Uani 1 1 d U . . H26A H 0.2019 -0.0196 0.2921 0.046 Uiso 1 1 calc R . . H26B H 0.262 -0.0301 0.2131 0.046 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 Au 0.02616(17) 0.03006(17) 0.03543(17) 0.00149(10) 0.00400(11) 0.00148(10) Tl 0.02871(17) 0.03217(18) 0.03385(17) -0.00015(10) -0.00265(11) -0.00027(10) C1 0.020(3) 0.037(4) 0.035(3) 0.002(3) 0.001(2) -0.007(3) C2 0.036(4) 0.039(4) 0.030(3) 0.005(3) 0.004(3) -0.003(3) C3 0.029(4) 0.039(4) 0.040(4) 0.009(3) -0.003(3) 0.002(3) C4 0.034(4) 0.032(4) 0.054(5) 0.006(3) 0.004(3) 0.006(3) C5 0.028(3) 0.032(4) 0.046(4) -0.007(3) 0.008(3) -0.002(3) C6 0.027(3) 0.032(4) 0.037(4) -0.002(3) -0.003(3) 0.000(3) F1 0.055(3) 0.054(3) 0.040(3) -0.011(2) -0.009(2) 0.001(2) F2 0.047(3) 0.058(3) 0.056(3) 0.005(2) -0.023(2) 0.010(2) F3 0.049(3) 0.047(3) 0.080(4) 0.003(3) 0.001(3) 0.025(2) F4 0.053(3) 0.044(3) 0.065(3) -0.021(2) 0.005(3) 0.003(2) F5 0.044(3) 0.065(3) 0.054(3) -0.020(3) -0.016(2) 0.008(2) C11 0.023(3) 0.031(4) 0.037(4) 0.001(3) 0.006(3) -0.006(3) C12 0.025(3) 0.031(4) 0.045(4) -0.007(3) 0.003(3) -0.004(3) C13 0.028(4) 0.035(4) 0.061(5) -0.007(3) -0.004(3) -0.003(3) C14 0.038(4) 0.027(4) 0.060(5) 0.000(3) 0.012(3) 0.001(3) C15 0.044(4) 0.031(4) 0.048(4) -0.009(3) 0.013(3) -0.003(3) C16 0.040(4) 0.040(4) 0.030(3) -0.003(3) 0.001(3) 0.000(3) F6 0.039(2) 0.044(3) 0.064(3) -0.024(2) -0.008(2) 0.000(2) F7 0.040(3) 0.067(4) 0.099(5) -0.015(3) -0.027(3) 0.016(3) F8 0.048(3) 0.044(3) 0.102(5) -0.011(3) 0.006(3) 0.021(2) F9 0.071(4) 0.041(3) 0.063(3) -0.023(2) 0.009(3) 0.007(3) F10 0.063(3) 0.062(3) 0.043(3) -0.012(2) -0.015(2) 0.006(3) S1 0.0222(8) 0.0307(9) 0.0451(10) 0.0053(8) -0.0014(7) 0.0004(7) S2 0.0402(10) 0.0299(9) 0.0390(10) 0.0001(7) 0.0045(8) 0.0028(8) S3 0.0227(8) 0.0443(11) 0.0346(9) 0.0051(8) -0.0007(7) -0.0006(7) C21 0.029(4) 0.038(4) 0.049(4) 0.011(4) 0.013(3) 0.004(3) C22 0.032(4) 0.037(4) 0.055(5) 0.005(4) 0.015(3) 0.006(3) C23 0.042(4) 0.039(4) 0.038(4) -0.007(3) -0.008(3) -0.008(3) C24 0.032(4) 0.049(5) 0.035(4) -0.001(3) -0.006(3) -0.010(3) C25 0.030(4) 0.040(4) 0.048(5) 0.015(3) -0.009(3) 0.003(3) C26 0.032(4) 0.032(4) 0.052(5) 0.008(3) 0.002(3) 0.005(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C11 2.052(7) . ? Au C1 2.056(7) . ? Au Tl 3.0360(4) . ? Au Au 3.3294(6) 3_665 ? Tl S3 3.0246(17) . ? Tl S2 3.058(2) . ? Tl S1 3.1154(19) . ? C1 C6 1.370(9) . ? C1 C2 1.386(8) . ? C2 F1 1.357(8) . ? C2 C3 1.360(10) . ? C3 C4 1.348(10) . ? C3 F2 1.361(8) . ? C4 C5 1.354(9) . ? C4 F3 1.361(9) . ? C5 F4 1.353(8) . ? C5 C6 1.373(9) . ? C6 F5 1.356(7) . ? C11 C12 1.370(9) . ? C11 C16 1.390(9) . ? C12 F6 1.353(8) . ? C12 C13 1.379(10) . ? C13 F7 1.339(8) . ? C13 C14 1.376(9) . ? C14 F8 1.343(9) . ? C14 C15 1.365(10) . ? C15 F9 1.344(8) . ? C15 C16 1.394(10) . ? C16 F10 1.350(8) . ? S1 C21 1.793(9) . ? S1 C26 1.819(7) . ? S2 C22 1.810(8) . ? S2 C23 1.828(8) . ? S3 C24 1.792(8) . ? S3 C25 1.805(8) . ? C21 C22 1.535(11) . ? C21 H21A 0.97 . ? C21 H21B 0.97 . ? C22 H22A 0.97 . ? C22 H22B 0.97 . ? C23 C24 1.524(11) . ? C23 H23A 0.97 . ? C23 H23B 0.97 . ? C24 H24A 0.97 . ? C24 H24B 0.97 . ? C25 C26 1.519(11) . ? C25 H25A 0.97 . ? C25 H25B 0.97 . ? C26 H26A 0.97 . ? C26 H26B 0.97 . ? 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 C11 Au C1 176.9(3) . . ? C11 Au Tl 91.48(17) . . ? C1 Au Tl 85.68(17) . . ? C11 Au Au 103.36(18) . 3_665 ? C1 Au Au 79.69(18) . 3_665 ? Tl Au Au 158.410(14) . 3_665 ? S3 Tl Au 77.66(4) . . ? S3 Tl S2 69.81(5) . . ? Au Tl S2 86.82(4) . . ? S3 Tl S1 68.65(5) . . ? Au Tl S1 143.20(4) . . ? S2 Tl S1 68.29(5) . . ? C6 C1 C2 114.2(7) . . ? C6 C1 Au 122.5(5) . . ? C2 C1 Au 123.4(5) . . ? F1 C2 C3 117.7(6) . . ? F1 C2 C1 119.0(6) . . ? C3 C2 C1 123.2(7) . . ? C4 C3 C2 119.8(6) . . ? C4 C3 F2 120.9(7) . . ? C2 C3 F2 119.3(7) . . ? C3 C4 C5 120.1(7) . . ? C3 C4 F3 118.9(6) . . ? C5 C4 F3 121.0(7) . . ? F4 C5 C4 120.0(7) . . ? F4 C5 C6 121.1(6) . . ? C4 C5 C6 118.9(7) . . ? F5 C6 C1 120.1(6) . . ? F5 C6 C5 116.2(6) . . ? C1 C6 C5 123.7(6) . . ? C12 C11 C16 114.5(7) . . ? C12 C11 Au 123.2(5) . . ? C16 C11 Au 122.3(5) . . ? F6 C12 C11 119.4(6) . . ? F6 C12 C13 116.3(6) . . ? C11 C12 C13 124.3(7) . . ? F7 C13 C14 119.8(7) . . ? F7 C13 C12 120.9(7) . . ? C14 C13 C12 119.4(7) . . ? F8 C14 C15 120.9(7) . . ? F8 C14 C13 119.9(7) . . ? C15 C14 C13 119.2(7) . . ? F9 C15 C14 120.3(7) . . ? F9 C15 C16 120.1(7) . . ? C14 C15 C16 119.6(7) . . ? F10 C16 C11 120.4(6) . . ? F10 C16 C15 116.5(6) . . ? C11 C16 C15 123.1(7) . . ? C21 S1 C26 101.9(4) . . ? C21 S1 Tl 111.0(3) . . ? C26 S1 Tl 101.8(3) . . ? C22 S2 C23 103.8(4) . . ? C22 S2 Tl 103.9(3) . . ? C23 S2 Tl 108.2(3) . . ? C24 S3 C25 103.7(4) . . ? C24 S3 Tl 100.7(3) . . ? C25 S3 Tl 112.0(2) . . ? C22 C21 S1 113.8(6) . . ? C22 C21 H21A 108.8 . . ? S1 C21 H21A 108.8 . . ? C22 C21 H21B 108.8 . . ? S1 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C21 C22 S2 118.8(5) . . ? C21 C22 H22A 107.6 . . ? S2 C22 H22A 107.6 . . ? C21 C22 H22B 107.6 . . ? S2 C22 H22B 107.6 . . ? H22A C22 H22B 107 . . ? C24 C23 S2 114.4(5) . . ? C24 C23 H23A 108.7 . . ? S2 C23 H23A 108.7 . . ? C24 C23 H23B 108.7 . . ? S2 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? C23 C24 S3 117.3(5) . . ? C23 C24 H24A 108 . . ? S3 C24 H24A 108 . . ? C23 C24 H24B 108 . . ? S3 C24 H24B 108 . . ? H24A C24 H24B 107.2 . . ? C26 C25 S3 114.1(6) . . ? C26 C25 H25A 108.7 . . ? S3 C25 H25A 108.7 . . ? C26 C25 H25B 108.7 . . ? S3 C25 H25B 108.7 . . ? H25A C25 H25B 107.6 . . ? C25 C26 S1 117.1(5) . . ? C25 C26 H26A 108 . . ? S1 C26 H26A 108 . . ? C25 C26 H26B 108 . . ? S1 C26 H26B 108 . . ? H26A C26 H26B 107.3 . . ? _database_code_depnum_ccdc_archive 'CCDC 935230' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_em15rd75 _audit_creation_date 2013-02-11T10:19:53-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'em15rd75 thf/hex' _chemical_formula_moiety 'C40 H32 Au2 F20 S8 Tl2' _chemical_formula_sum 'C40 H32 Au2 F20 S8 Tl2' _chemical_formula_weight 1951.81 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0826(5) _cell_length_b 12.5273(7) _cell_length_c 12.9677(5) _cell_angle_alpha 115.204(3) _cell_angle_beta 98.272(3) _cell_angle_gamma 103.410(3) _cell_volume 1248.28(11) _cell_formula_units_Z 1 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 5328 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 27.49 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour 'pale green' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 2.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_special_details ; 'multi-scan based on symmetry-related measurements' ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 12.735 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details Scalepack _exptl_absorpt_correction_T_min 0.0367 _exptl_absorpt_correction_T_max 0.3293 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.789795E-1 _diffrn_orient_matrix_ub_12 -0.81746E-2 _diffrn_orient_matrix_ub_13 0.560042E-1 _diffrn_orient_matrix_ub_21 -0.18465E-2 _diffrn_orient_matrix_ub_22 0.782524E-1 _diffrn_orient_matrix_ub_23 0.667814E-1 _diffrn_orient_matrix_ub_31 -0.873142E-1 _diffrn_orient_matrix_ub_32 -0.502801E-1 _diffrn_orient_matrix_ub_33 0.162828E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0601 _diffrn_reflns_av_unetI/netI 0.0357 _diffrn_reflns_number 19740 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.9 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 5679 _reflns_number_gt 4564 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Disorder of atoms S3, C23 and C24 of the macrocycle was modelled in terms of alternative sites. For the atoms involved in the disorder, distance restraints of 1.485(200) and 1.82(2) Angstroms were applied to C-C and S-C distances, respectively. Restraints were also applied to fix the C-S-C and C-C-S angles to 109.5 degrees, with distance restraints of 2.92(2) and 2.67(2) Angstroms for C-C and S-C distances, respectively. The occupancies of the two alternative orientations were set at 0.8 and 0.2, respectively. FLAT and SAME restraints were applied to both aryl groups. DELU was applied to all light atoms: C and F. 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^ > 2\s(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^)+(0.0726P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_number_reflns 5679 _refine_ls_number_parameters 352 _refine_ls_number_restraints 125 _refine_ls_R_factor_all 0.0537 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.1068 _refine_ls_wR_factor_gt 0.0984 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.03 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.506 _refine_diff_density_min -3.054 _refine_diff_density_rms 0.239 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Au Au 0.69876(3) 0.61265(2) 0.52209(2) 0.03145(10) Uani 1 1 d . . . Tl Tl 0.74880(3) 0.88991(2) 0.57401(2) 0.03212(10) Uani 1 1 d . . . C1 C 0.7785(7) 0.5615(6) 0.3740(5) 0.0314(14) Uani 1 1 d DU . . C2 C 0.7800(7) 0.6087(6) 0.2981(6) 0.0355(15) Uani 1 1 d DU . . C3 C 0.8392(8) 0.5678(7) 0.1984(6) 0.0395(16) Uani 1 1 d DU . . C4 C 0.9008(8) 0.4732(7) 0.1757(6) 0.0388(15) Uani 1 1 d DU . . C5 C 0.9000(9) 0.4172(6) 0.2471(6) 0.0379(15) Uani 1 1 d DU . . C6 C 0.8410(8) 0.4625(6) 0.3441(6) 0.0337(14) Uani 1 1 d DU . . F1 F 0.7205(6) 0.7033(4) 0.3137(4) 0.0511(11) Uani 1 1 d DU . . F2 F 0.8422(6) 0.6244(4) 0.1297(4) 0.0590(13) Uani 1 1 d DU . . F3 F 0.9599(6) 0.4319(4) 0.0814(4) 0.0584(13) Uani 1 1 d DU . . F4 F 0.9546(6) 0.3198(4) 0.2216(4) 0.0524(12) Uani 1 1 d DU . . F5 F 0.8452(6) 0.4049(4) 0.4116(4) 0.0490(11) Uani 1 1 d DU . . C11 C 0.6288(7) 0.6472(5) 0.6730(6) 0.0304(13) Uani 1 1 d DU . . C12 C 0.6602(7) 0.5857(6) 0.7348(6) 0.0375(15) Uani 1 1 d DU . . C13 C 0.6171(8) 0.5975(8) 0.8358(6) 0.0467(17) Uani 1 1 d DU . . C14 C 0.5387(9) 0.6832(8) 0.8814(6) 0.0484(17) Uani 1 1 d DU . . C15 C 0.5042(9) 0.7488(7) 0.8253(7) 0.0497(18) Uani 1 1 d DU . . C16 C 0.5474(8) 0.7281(6) 0.7237(7) 0.0386(15) Uani 1 1 d DU . . F6 F 0.7372(6) 0.5002(4) 0.6923(4) 0.0558(12) Uani 1 1 d DU . . F7 F 0.6480(7) 0.5314(6) 0.8889(5) 0.0780(16) Uani 1 1 d DU . . F8 F 0.4927(6) 0.6973(5) 0.9807(4) 0.0712(15) Uani 1 1 d DU . . F9 F 0.4247(7) 0.8286(5) 0.8681(5) 0.0765(17) Uani 1 1 d DU . . F10 F 0.5035(6) 0.7916(5) 0.6690(5) 0.0655(15) Uani 1 1 d DU . . C20 C 1.1401(8) 1.0035(7) 0.8567(6) 0.0376(16) Uani 1 1 d . . . H20A H 1.1939 1.0531 0.9407 0.045 Uiso 1 1 calc R . . H20B H 1.1611 0.9249 0.8289 0.045 Uiso 1 1 calc R . . S1 S 0.93282(19) 0.97127(15) 0.83942(13) 0.0297(3) Uani 1 1 d . . . C21 C 0.9271(8) 1.1272(6) 0.9278(6) 0.0347(15) Uani 1 1 d U B . H21A H 0.9894 1.1615 1.0089 0.042 Uiso 1 1 calc R . . H21B H 0.9716 1.1811 0.8964 0.042 Uiso 1 1 calc R . . C22 C 0.7602(8) 1.1219(6) 0.9255(5) 0.0339(15) Uani 1 1 d DU . . H22A H 0.7604 1.2025 0.984 0.041 Uiso 1 1 calc R A 1 H22B H 0.7143 1.0607 0.949 0.041 Uiso 1 1 calc R A 1 S2A S 0.6353(2) 1.08238(17) 0.78312(15) 0.0354(4) Uani 0.8 1 d PD B 1 C23A C 0.7032(18) 1.2302(10) 0.7795(10) 0.059(3) Uani 0.8 1 d PDU B 1 H23A H 0.6945 1.2974 0.8497 0.07 Uiso 0.8 1 calc PR B 1 H23B H 0.8129 1.2489 0.7795 0.07 Uiso 0.8 1 calc PR B 1 C24A C 0.6080(13) 1.2214(9) 0.6732(7) 0.047(2) Uani 0.8 1 d PDU B 1 H24A H 0.6305 1.3042 0.6804 0.056 Uiso 0.8 1 calc PR B 1 H24B H 0.4975 1.1912 0.6686 0.056 Uiso 0.8 1 calc PR B 1 S3A S 0.6430(3) 1.1184(2) 0.53635(19) 0.0359(5) Uani 0.8 1 d PD B 1 C25A C 0.8141(12) 1.2109(8) 0.5247(7) 0.064(3) Uani 0.8 1 d PDU B 1 H25A H 0.8069 1.2933 0.5458 0.077 Uiso 0.8 1 calc PR B 1 H25B H 0.9061 1.2204 0.5804 0.077 Uiso 0.8 1 calc PR B 1 S2B S 0.6353(2) 1.08238(17) 0.78312(15) 0.0354(4) Uani 0.2 1 d PD B 2 C23B C 0.663(4) 1.227(3) 0.778(3) 0.047(7) Uani 0.2 1 d PDU B 2 H23C H 0.5766 1.2135 0.7149 0.056 Uiso 0.2 1 calc PR B 2 H23D H 0.6537 1.2883 0.8517 0.056 Uiso 0.2 1 calc PR B 2 C24B C 0.791(4) 1.2746(18) 0.761(2) 0.048(6) Uani 0.2 1 d PDU B 2 H24C H 0.8726 1.307 0.8338 0.058 Uiso 0.2 1 calc PR B 2 H24D H 0.7811 1.3461 0.7525 0.058 Uiso 0.2 1 calc PR B 2 S3B S 0.8639(13) 1.1864(9) 0.6411(9) 0.048(2) Uani 0.2 1 d PD B 2 C25B C 0.8141(12) 1.2109(8) 0.5247(7) 0.064(3) Uani 0.2 1 d PDU B 2 H25C H 0.7021 1.198 0.512 0.077 Uiso 0.2 1 calc PR B 2 H25D H 0.864 1.2999 0.5558 0.077 Uiso 0.2 1 calc PR B 2 C26 C 0.8334(9) 1.1556(7) 0.4054(6) 0.0398(16) Uani 1 1 d U . . H26A H 0.9221 1.2125 0.401 0.048 Uiso 1 1 calc R B 1 H26B H 0.7398 1.1429 0.3491 0.048 Uiso 1 1 calc R B 1 S4 S 0.8668(2) 1.00579(17) 0.36555(16) 0.0366(4) Uani 1 1 d . B . C27 C 0.7879(9) 0.9290(7) 0.2066(7) 0.0416(17) Uani 1 1 d . . . H27A H 0.801 0.8474 0.1741 0.05 Uiso 1 1 calc R B . H27B H 0.6758 0.9159 0.1887 0.05 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 Au 0.03263(16) 0.02729(15) 0.03435(16) 0.01347(12) 0.01209(11) 0.01036(11) Tl 0.03739(16) 0.03069(16) 0.02928(15) 0.01417(12) 0.01076(11) 0.01217(12) C1 0.038(4) 0.019(3) 0.029(3) 0.009(3) 0.005(3) 0.004(3) C2 0.039(4) 0.027(3) 0.034(3) 0.010(3) 0.004(3) 0.009(3) C3 0.048(4) 0.040(4) 0.026(3) 0.012(3) 0.008(3) 0.013(3) C4 0.038(4) 0.038(4) 0.027(3) 0.007(3) 0.010(3) 0.006(3) C5 0.047(4) 0.025(3) 0.033(3) 0.006(3) 0.013(3) 0.011(3) C6 0.039(4) 0.031(3) 0.033(3) 0.017(3) 0.011(3) 0.011(3) F1 0.078(3) 0.047(3) 0.040(2) 0.022(2) 0.019(2) 0.038(2) F2 0.089(4) 0.062(3) 0.039(2) 0.031(2) 0.023(2) 0.033(3) F3 0.077(3) 0.052(3) 0.044(3) 0.013(2) 0.034(2) 0.025(2) F4 0.064(3) 0.036(2) 0.058(3) 0.015(2) 0.025(2) 0.027(2) F5 0.071(3) 0.042(2) 0.056(3) 0.033(2) 0.029(2) 0.029(2) C11 0.029(3) 0.023(3) 0.038(3) 0.015(3) 0.011(3) 0.004(2) C12 0.035(4) 0.041(4) 0.041(4) 0.020(3) 0.014(3) 0.018(3) C13 0.042(4) 0.061(5) 0.036(4) 0.025(4) 0.007(3) 0.012(3) C14 0.037(4) 0.057(5) 0.031(4) 0.009(3) 0.014(3) 0.001(3) C15 0.046(4) 0.034(4) 0.060(5) 0.011(3) 0.030(4) 0.010(3) C16 0.035(4) 0.026(3) 0.056(4) 0.019(3) 0.023(3) 0.006(3) F6 0.070(3) 0.065(3) 0.065(3) 0.042(3) 0.034(2) 0.047(3) F7 0.082(4) 0.123(5) 0.063(3) 0.065(3) 0.026(3) 0.048(4) F8 0.066(3) 0.089(4) 0.039(3) 0.014(2) 0.027(2) 0.016(3) F9 0.079(4) 0.055(3) 0.109(4) 0.030(3) 0.068(3) 0.035(3) F10 0.061(3) 0.069(3) 0.124(4) 0.072(3) 0.064(3) 0.045(3) C20 0.035(4) 0.048(4) 0.038(4) 0.024(3) 0.011(3) 0.019(3) S1 0.0327(8) 0.0316(8) 0.0268(8) 0.0143(7) 0.0107(6) 0.0117(7) C21 0.037(4) 0.033(4) 0.031(3) 0.011(3) 0.010(3) 0.016(3) C22 0.039(4) 0.040(4) 0.028(3) 0.015(3) 0.016(3) 0.019(3) S2A 0.0379(9) 0.0431(10) 0.0323(9) 0.0188(8) 0.0133(7) 0.0218(8) C23A 0.094(9) 0.054(6) 0.041(5) 0.023(5) 0.025(5) 0.041(6) C24A 0.069(6) 0.057(5) 0.038(4) 0.028(4) 0.029(4) 0.040(5) S3A 0.0441(12) 0.0383(12) 0.0332(11) 0.0202(9) 0.0165(9) 0.0173(10) C25A 0.097(7) 0.046(5) 0.046(4) 0.016(4) 0.023(5) 0.026(5) S2B 0.0379(9) 0.0431(10) 0.0323(9) 0.0188(8) 0.0133(7) 0.0218(8) C23B 0.094(13) 0.052(11) 0.030(10) 0.032(9) 0.044(9) 0.046(10) C24B 0.088(12) 0.043(10) 0.048(10) 0.039(8) 0.037(9) 0.035(10) S3B 0.057(6) 0.044(5) 0.048(5) 0.021(5) 0.022(5) 0.021(5) C25B 0.097(7) 0.046(5) 0.046(4) 0.016(4) 0.023(5) 0.026(5) C26 0.047(4) 0.038(4) 0.047(4) 0.026(3) 0.020(3) 0.019(3) S4 0.0396(10) 0.0424(10) 0.0433(10) 0.0278(8) 0.0206(7) 0.0200(8) C27 0.037(4) 0.036(4) 0.049(4) 0.014(3) 0.016(3) 0.015(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C11 2.046(7) . ? Au C1 2.047(7) . ? Au Tl 3.1483(4) . ? C1 C2 1.348(9) . ? C1 C6 1.410(9) . ? C2 F1 1.364(8) . ? C2 C3 1.410(10) . ? C3 F2 1.353(8) . ? C3 C4 1.364(10) . ? C4 F3 1.353(8) . ? C4 C5 1.379(10) . ? C5 F4 1.352(8) . ? C5 C6 1.385(9) . ? C6 F5 1.352(8) . ? C11 C12 1.371(9) . ? C11 C16 1.388(9) . ? C12 F6 1.377(8) . ? C12 C13 1.378(10) . ? C13 F7 1.332(10) . ? C13 C14 1.394(11) . ? C14 F8 1.364(8) . ? C14 C15 1.366(12) . ? C15 F9 1.345(8) . ? C15 C16 1.364(10) . ? C16 F10 1.356(9) . ? C20 C27 1.519(11) 2_776 ? C20 S1 1.791(7) . ? C20 H20A 0.97 . ? C20 H20B 0.97 . ? S1 C21 1.814(6) . ? C21 C22 1.497(9) . ? C21 H21A 0.97 . ? C21 H21B 0.97 . ? C22 S2A 1.816(6) . ? C22 H22A 0.97 . ? C22 H22B 0.97 . ? S2A C23A 1.834(11) . ? C23A C24A 1.464(14) . ? C23A H23A 0.97 . ? C23A H23B 0.97 . ? C24A S3A 1.821(8) . ? C24A H24A 0.97 . ? C24A H24B 0.97 . ? S3A C25A 1.778(10) . ? C25A C26 1.457(10) . ? C25A H25A 0.97 . ? C25A H25B 0.97 . ? C23B C24B 1.27(4) . ? C23B H23C 0.97 . ? C23B H23D 0.97 . ? C24B S3B 1.805(17) . ? C24B H24C 0.97 . ? C24B H24D 0.97 . ? C26 S4 1.834(7) . ? C26 H26A 0.97 . ? C26 H26B 0.97 . ? S4 C27 1.803(8) . ? C27 C20 1.519(11) 2_776 ? C27 H27A 0.97 . ? C27 H27B 0.97 . ? 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 C11 Au C1 172.7(3) . . ? C11 Au Tl 90.78(17) . . ? C1 Au Tl 95.59(18) . . ? C2 C1 C6 113.5(6) . . ? C2 C1 Au 129.2(5) . . ? C6 C1 Au 117.2(5) . . ? C1 C2 F1 120.5(6) . . ? C1 C2 C3 125.2(7) . . ? F1 C2 C3 114.3(6) . . ? F2 C3 C4 120.5(6) . . ? F2 C3 C2 121.2(6) . . ? C4 C3 C2 118.3(7) . . ? F3 C4 C3 120.1(7) . . ? F3 C4 C5 119.5(7) . . ? C3 C4 C5 120.3(6) . . ? F4 C5 C4 120.3(6) . . ? F4 C5 C6 121.3(7) . . ? C4 C5 C6 118.4(6) . . ? F5 C6 C5 115.7(6) . . ? F5 C6 C1 120.1(6) . . ? C5 C6 C1 124.2(6) . . ? C12 C11 C16 112.8(6) . . ? C12 C11 Au 119.9(5) . . ? C16 C11 Au 127.3(5) . . ? C11 C12 F6 118.7(6) . . ? C11 C12 C13 126.1(7) . . ? F6 C12 C13 115.1(7) . . ? F7 C13 C12 122.6(7) . . ? F7 C13 C14 120.6(7) . . ? C12 C13 C14 116.8(7) . . ? F8 C14 C15 120.7(8) . . ? F8 C14 C13 118.8(8) . . ? C15 C14 C13 120.5(7) . . ? F9 C15 C16 121.3(8) . . ? F9 C15 C14 120.1(8) . . ? C16 C15 C14 118.6(7) . . ? F10 C16 C15 115.9(7) . . ? F10 C16 C11 118.9(6) . . ? C15 C16 C11 125.2(7) . . ? C27 C20 S1 116.6(5) 2_776 . ? C27 C20 H20A 108.1 2_776 . ? S1 C20 H20A 108.1 . . ? C27 C20 H20B 108.1 2_776 . ? S1 C20 H20B 108.1 . . ? H20A C20 H20B 107.3 . . ? C20 S1 C21 100.5(3) . . ? C22 C21 S1 109.5(5) . . ? C22 C21 H21A 109.8 . . ? S1 C21 H21A 109.8 . . ? C22 C21 H21B 109.8 . . ? S1 C21 H21B 109.8 . . ? H21A C21 H21B 108.2 . . ? C21 C22 S2A 115.0(4) . . ? C21 C22 H22A 108.5 . . ? S2A C22 H22A 108.5 . . ? C21 C22 H22B 108.5 . . ? S2A C22 H22B 108.5 . . ? H22A C22 H22B 107.5 . . ? C22 S2A C23A 100.9(4) . . ? C24A C23A S2A 109.9(9) . . ? C24A C23A H23A 109.7 . . ? S2A C23A H23A 109.7 . . ? C24A C23A H23B 109.7 . . ? S2A C23A H23B 109.7 . . ? H23A C23A H23B 108.2 . . ? C23A C24A S3A 113.6(7) . . ? C23A C24A H24A 108.9 . . ? S3A C24A H24A 108.9 . . ? C23A C24A H24B 108.9 . . ? S3A C24A H24B 108.9 . . ? H24A C24A H24B 107.7 . . ? C25A S3A C24A 105.1(4) . . ? C26 C25A S3A 112.1(6) . . ? C26 C25A H25A 109.2 . . ? S3A C25A H25A 109.2 . . ? C26 C25A H25B 109.2 . . ? S3A C25A H25B 109.2 . . ? H25A C25A H25B 107.9 . . ? C24B C23B H23C 107.9 . . ? C24B C23B H23D 107.9 . . ? H23C C23B H23D 107.2 . . ? C23B C24B S3B 122(2) . . ? C23B C24B H24C 106.7 . . ? S3B C24B H24C 106.7 . . ? C23B C24B H24D 106.7 . . ? S3B C24B H24D 106.7 . . ? H24C C24B H24D 106.6 . . ? C25A C26 S4 111.3(6) . . ? C25A C26 H26A 109.4 . . ? S4 C26 H26A 109.4 . . ? C25A C26 H26B 109.4 . . ? S4 C26 H26B 109.4 . . ? H26A C26 H26B 108 . . ? C27 S4 C26 100.2(3) . . ? C20 C27 S4 116.3(5) 2_776 . ? C20 C27 H27A 108.2 2_776 . ? S4 C27 H27A 108.2 . . ? C20 C27 H27B 108.2 2_776 . ? S4 C27 H27B 108.2 . . ? H27A C27 H27B 107.4 . . ? #############################################################END _database_code_depnum_ccdc_archive 'CCDC 935231'