# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_requested_category FM _publ_contact_author_name 'M. Elena Olmos' _publ_contact_author_email m-elena.olmos@unirioja.es loop_ _publ_author_name 'J.M.L.de Luzuriaga' 'Miguel Monge' 'M. Elena Olmos' 'David Pascual' 'Tania Lasanta' data_t40 _database_code_depnum_ccdc_archive 'CCDC 808670' #TrackingRef 'archive.cif' _audit_creation_date 2011-01-12T16:21:06-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'DP131 CH2Cl2' _chemical_formula_moiety 'C30 H18 Au2 F20 Hg P2' _chemical_formula_sum 'C30 H18 Au2 F20 Hg P2' _chemical_formula_weight 1414.91 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.3049(9) _cell_length_b 10.4688(5) _cell_length_c 18.1473(5) _cell_angle_alpha 90 _cell_angle_beta 109.352(3) _cell_angle_gamma 90 _cell_volume 3460.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4103 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 27.46 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 2.716 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2584 _exptl_special_details ; 'multi-scan based on symmetry-related measurements' ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 13.109 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details Scalepack _exptl_absorpt_correction_T_min 0.0282 _exptl_absorpt_correction_T_max 0.154 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 120(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 0.287462E-1 _diffrn_orient_matrix_ub_12 -0.283667E-1 _diffrn_orient_matrix_ub_13 -0.338701E-1 _diffrn_orient_matrix_ub_21 -0.467298E-1 _diffrn_orient_matrix_ub_22 -0.134822E-1 _diffrn_orient_matrix_ub_23 -0.44333E-1 _diffrn_orient_matrix_ub_31 0.20553E-2 _diffrn_orient_matrix_ub_32 0.902109E-1 _diffrn_orient_matrix_ub_33 -0.172761E-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 0.086 _diffrn_reflns_av_unetI/netI 0.0505 _diffrn_reflns_number 27611 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 3921 _reflns_number_gt 3106 _reflns_threshold_expression >2sigma(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_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0370P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_number_reflns 3921 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.056 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0738 _refine_ls_wR_factor_gt 0.0667 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.255 _refine_diff_density_min -2.382 _refine_diff_density_rms 0.281 #----------------------------------------------------------------------------# # 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' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.469379(15) 0.46658(2) 0.160981(13) 0.01572(9) Uani 1 1 d . . . Hg Hg 0.5 0.5 0 0.01911(10) Uani 1 2 d S . . P P 0.38697(10) 0.30242(15) 0.14159(9) 0.0171(4) Uani 1 1 d . . . C7 C 0.3933(4) 0.2094(6) 0.2280(3) 0.0254(16) Uani 1 1 d . . . H7A H 0.3533 0.1498 0.2159 0.038 Uiso 1 1 calc R . . H7B H 0.391 0.2655 0.2689 0.038 Uiso 1 1 calc R . . H7C H 0.439 0.1636 0.2447 0.038 Uiso 1 1 calc R . . C8 C 0.3919(4) 0.1839(6) 0.0708(4) 0.0239(15) Uani 1 1 d . . . H8A H 0.3564 0.118 0.0674 0.036 Uiso 1 1 calc R . . H8B H 0.4402 0.1471 0.0868 0.036 Uiso 1 1 calc R . . H8C H 0.3818 0.2236 0.0206 0.036 Uiso 1 1 calc R . . C9 C 0.2922(4) 0.3543(6) 0.1054(3) 0.0218(15) Uani 1 1 d . . . H9A H 0.2827 0.396 0.0559 0.033 Uiso 1 1 calc R . . H9B H 0.2833 0.4129 0.1419 0.033 Uiso 1 1 calc R . . H9C H 0.2605 0.2816 0.0992 0.033 Uiso 1 1 calc R . . C1 C 0.5392(4) 0.6230(6) 0.1757(3) 0.0178(14) Uani 1 1 d . . . C2 C 0.5120(4) 0.7468(6) 0.1640(3) 0.0182(14) Uani 1 1 d . . . C3 C 0.5552(4) 0.8535(6) 0.1760(4) 0.0200(14) Uani 1 1 d . . . C4 C 0.6299(4) 0.8407(6) 0.2020(3) 0.0212(15) Uani 1 1 d . . . C5 C 0.6603(4) 0.7185(6) 0.2162(3) 0.0175(14) Uani 1 1 d . . . C6 C 0.6143(4) 0.6146(6) 0.2017(3) 0.0163(14) Uani 1 1 d . . . F1 F 0.4379(2) 0.7664(3) 0.13836(19) 0.0234(9) Uani 1 1 d . . . F2 F 0.5260(2) 0.9712(3) 0.1625(2) 0.0328(10) Uani 1 1 d . . . F3 F 0.6744(2) 0.9429(3) 0.2153(2) 0.0305(10) Uani 1 1 d . . . F4 F 0.7342(2) 0.7051(3) 0.24305(19) 0.0257(9) Uani 1 1 d . . . F5 F 0.6480(2) 0.4980(3) 0.2175(2) 0.0238(9) Uani 1 1 d . . . C11 C 0.4049(4) 0.6111(6) -0.0363(3) 0.0218(16) Uani 1 1 d . . . C12 C 0.3368(4) 0.5587(6) -0.0606(4) 0.0212(15) Uani 1 1 d . . . C13 C 0.2725(4) 0.6300(6) -0.0825(3) 0.0198(14) Uani 1 1 d . . . C14 C 0.2781(4) 0.7618(6) -0.0807(3) 0.0209(15) Uani 1 1 d . . . C15 C 0.3461(4) 0.8190(6) -0.0567(3) 0.0183(15) Uani 1 1 d . . . C16 C 0.4084(4) 0.7432(6) -0.0345(3) 0.0193(15) Uani 1 1 d . . . F6 F 0.3284(2) 0.4298(3) -0.0638(2) 0.0262(9) Uani 1 1 d . . . F7 F 0.2063(2) 0.5752(4) -0.1065(2) 0.0321(10) Uani 1 1 d . . . F8 F 0.2171(2) 0.8334(4) -0.1017(2) 0.0283(9) Uani 1 1 d . . . F9 F 0.3512(2) 0.9468(3) -0.0532(2) 0.0294(10) Uani 1 1 d . . . F10 F 0.4737(2) 0.8030(3) -0.0106(2) 0.0268(9) 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 Au 0.01383(15) 0.01839(13) 0.01488(14) 0.00011(9) 0.00469(10) -0.00270(10) Hg 0.0187(2) 0.02285(19) 0.01607(19) 0.00191(13) 0.00616(16) 0.00743(15) P 0.0129(10) 0.0166(8) 0.0202(9) 0.0011(6) 0.0036(7) -0.0029(7) C7 0.013(4) 0.027(4) 0.032(4) 0.011(3) 0.003(3) -0.003(3) C8 0.014(4) 0.024(3) 0.035(4) -0.004(3) 0.010(3) -0.001(3) C9 0.018(4) 0.026(4) 0.023(4) 0.001(3) 0.009(3) -0.001(3) C1 0.014(4) 0.026(3) 0.013(3) -0.002(2) 0.005(3) -0.004(3) C2 0.016(4) 0.022(3) 0.016(3) 0.000(2) 0.004(3) 0.000(3) C3 0.021(4) 0.017(3) 0.024(3) -0.002(3) 0.011(3) 0.000(3) C4 0.025(4) 0.020(3) 0.022(3) -0.009(3) 0.011(3) -0.010(3) C5 0.012(4) 0.024(3) 0.017(3) -0.001(2) 0.006(3) -0.003(3) C6 0.020(4) 0.021(3) 0.010(3) -0.003(2) 0.007(3) 0.002(3) F1 0.015(2) 0.030(2) 0.022(2) -0.0019(16) 0.0020(17) 0.0045(17) F2 0.031(3) 0.019(2) 0.045(3) -0.0032(16) 0.007(2) 0.0010(17) F3 0.029(3) 0.025(2) 0.041(2) -0.0096(17) 0.016(2) -0.0165(19) F4 0.010(2) 0.036(2) 0.030(2) -0.0016(17) 0.0060(18) -0.0044(18) F5 0.020(2) 0.0197(18) 0.031(2) 0.0051(15) 0.0079(19) 0.0044(16) C11 0.028(5) 0.024(3) 0.014(3) 0.000(2) 0.007(3) 0.010(3) C12 0.023(4) 0.022(3) 0.020(4) -0.002(3) 0.009(3) 0.005(3) C13 0.012(4) 0.024(3) 0.020(3) 0.000(3) 0.001(3) -0.001(3) C14 0.017(4) 0.023(3) 0.021(4) 0.004(3) 0.005(3) 0.010(3) C15 0.025(4) 0.016(3) 0.015(3) 0.002(2) 0.008(3) 0.004(3) C16 0.019(4) 0.023(3) 0.018(3) -0.001(3) 0.009(3) 0.003(3) F6 0.036(3) 0.0161(18) 0.030(2) 0.0040(16) 0.015(2) 0.0016(18) F7 0.022(3) 0.031(2) 0.042(2) -0.0005(19) 0.010(2) -0.0014(19) F8 0.016(2) 0.031(2) 0.036(2) 0.0029(17) 0.0059(19) 0.0131(18) F9 0.032(3) 0.0178(19) 0.037(2) -0.0017(16) 0.009(2) 0.0041(18) F10 0.020(2) 0.030(2) 0.030(2) 0.0001(16) 0.0075(18) -0.0015(18) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au C1 2.081(6) . ? Au P 2.2884(16) . ? Au Au 3.0504(5) 2_655 ? Au Hg 3.1860(2) . ? Hg C11 2.087(7) 5_665 ? Hg C11 2.087(7) . ? Hg Au 3.1860(2) 5_665 ? P C9 1.810(7) . ? P C8 1.812(6) . ? P C7 1.815(6) . ? C1 C6 1.371(9) . ? C1 C2 1.388(9) . ? C2 F1 1.367(7) . ? C2 C3 1.368(9) . ? C3 F2 1.343(7) . ? C3 C4 1.367(9) . ? C4 F3 1.343(7) . ? C4 C5 1.396(9) . ? C5 F4 1.353(7) . ? C5 C6 1.373(8) . ? C6 F5 1.368(7) . ? C11 C12 1.357(10) . ? C11 C16 1.385(8) . ? C12 F6 1.358(7) . ? C12 C13 1.387(9) . ? C13 F7 1.337(7) . ? C13 C14 1.383(8) . ? C14 F8 1.340(7) . ? C14 C15 1.375(9) . ? C15 F9 1.342(7) . ? C15 C16 1.385(9) . ? C16 F10 1.344(7) . ? 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 Au P 176.67(19) . . ? C1 Au Au 81.76(15) . 2_655 ? P Au Au 99.70(4) . 2_655 ? C1 Au Hg 73.87(15) . . ? P Au Hg 105.80(4) . . ? Au Au Hg 147.847(14) 2_655 . ? C11 Hg C11 180.0(3) 5_665 . ? C11 Hg Au 86.54(16) 5_665 5_665 ? C11 Hg Au 93.46(16) . 5_665 ? C11 Hg Au 93.46(16) 5_665 . ? C11 Hg Au 86.54(16) . . ? Au Hg Au 180.000(12) 5_665 . ? C9 P C8 103.5(3) . . ? C9 P C7 104.2(3) . . ? C8 P C7 103.9(3) . . ? C9 P Au 113.4(2) . . ? C8 P Au 115.2(2) . . ? C7 P Au 115.2(2) . . ? C6 C1 C2 114.5(6) . . ? C6 C1 Au 124.1(5) . . ? C2 C1 Au 121.3(5) . . ? F1 C2 C3 116.5(6) . . ? F1 C2 C1 119.5(6) . . ? C3 C2 C1 124.0(6) . . ? F2 C3 C4 119.0(6) . . ? F2 C3 C2 121.5(6) . . ? C4 C3 C2 119.5(6) . . ? F3 C4 C3 121.5(6) . . ? F3 C4 C5 119.5(6) . . ? C3 C4 C5 119.0(6) . . ? F4 C5 C6 121.6(6) . . ? F4 C5 C4 119.4(6) . . ? C6 C5 C4 119.0(6) . . ? F5 C6 C1 120.3(6) . . ? F5 C6 C5 115.7(6) . . ? C1 C6 C5 124.0(6) . . ? C12 C11 C16 116.4(6) . . ? C12 C11 Hg 122.3(5) . . ? C16 C11 Hg 121.2(5) . . ? C11 C12 F6 120.2(6) . . ? C11 C12 C13 123.7(6) . . ? F6 C12 C13 116.1(6) . . ? F7 C13 C14 119.6(6) . . ? F7 C13 C12 122.0(6) . . ? C14 C13 C12 118.3(6) . . ? F8 C14 C15 120.2(6) . . ? F8 C14 C13 119.8(6) . . ? C15 C14 C13 120.0(6) . . ? F9 C15 C14 119.8(6) . . ? F9 C15 C16 121.0(6) . . ? C14 C15 C16 119.2(6) . . ? F10 C16 C11 120.4(6) . . ? F10 C16 C15 117.2(5) . . ? C11 C16 C15 122.3(7) . . ?