data_MK05_a _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H17 Au Cl F6 P' _chemical_formula_weight 718.79 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' 'F' 'F' 0.0171 0.0103 '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' '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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6440(2) _cell_length_b 10.0254(2) _cell_length_c 14.5537(3) _cell_angle_alpha 81.7475(8) _cell_angle_beta 87.4505(8) _cell_angle_gamma 73.0847(7) _cell_volume 1194.15(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9589 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 26.39 _exptl_crystal_description 'rod' _exptl_crystal_colour 'colourless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.999 _exptl_crystal_F_000 688 _exptl_transmission_factor_min 0.0583 _exptl_transmission_factor_max 0.1008 _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.090 _exptl_absorpt_coefficient_mu 6.401 _shelx_estimated_absorpt_T_min 0.114 _shelx_estimated_absorpt_T_max 0.597 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'sealed tube' _diffrn_measurement_device_type 'D8 Venture, Bruker Photon CMOS Detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 20118 _diffrn_reflns_av_unetI/netI 0.0423 _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.143 _diffrn_reflns_theta_max 26.409 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 4867 _reflns_number_gt 4374 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'Diamond 2.1e' _computing_publication_material 'X-STEP32, Microsoft Word' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0147P)^2^+4.8096P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4867 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0690 _refine_ls_wR_factor_gt 0.0664 _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_restrained_S_all 1.149 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6317(6) 0.5133(6) 0.6408(4) 0.0178(11) Uani 1 1 d . . . . . C2 C 0.5884(6) 0.4108(5) 0.6881(3) 0.0164(11) Uani 1 1 d . . . . . H2 H 0.6000 0.3275 0.6612 0.020 Uiso 1 1 calc R U . . . C3 C 0.5176(6) 0.4202(5) 0.7881(4) 0.0163(11) Uani 1 1 d . . . . . C4 C 0.3726(6) 0.5538(5) 0.7827(3) 0.0163(11) Uani 1 1 d . . . . . H4 H 0.2697 0.5475 0.8052 0.020 Uiso 1 1 calc R U . . . C5 C 0.3909(6) 0.6775(5) 0.7467(3) 0.0183(11) Uani 1 1 d . . . . . C6 C 0.2642(6) 0.8140(5) 0.7396(3) 0.0151(10) Uani 1 1 d . . . . . C7 C 0.1589(6) 0.8480(6) 0.8141(4) 0.0206(11) Uani 1 1 d . . . . . H7 H 0.1673 0.7820 0.8688 0.025 Uiso 1 1 calc R U . . . C8 C 0.0421(6) 0.9778(6) 0.8085(4) 0.0229(12) Uani 1 1 d . . . . . H8 H -0.0289 1.0003 0.8594 0.027 Uiso 1 1 calc R U . . . C9 C 0.0290(7) 1.0740(6) 0.7292(4) 0.0257(13) Uani 1 1 d . . . . . H9 H -0.0489 1.1636 0.7263 0.031 Uiso 1 1 calc R U . . . C10 C 0.1285(6) 1.0406(6) 0.6541(4) 0.0254(13) Uani 1 1 d . . . . . H10 H 0.1161 1.1056 0.5987 0.031 Uiso 1 1 calc R U . . . C11 C 0.2468(6) 0.9121(6) 0.6593(4) 0.0211(11) Uani 1 1 d . . . . . H11 H 0.3166 0.8905 0.6078 0.025 Uiso 1 1 calc R U . . . C12 C 0.7046(6) 0.5185(5) 0.5468(3) 0.0163(11) Uani 1 1 d . . . . . C13 C 0.6687(6) 0.6415(6) 0.4829(4) 0.0197(11) Uani 1 1 d . . . . . H13 H 0.5932 0.7247 0.4990 0.024 Uiso 1 1 calc R U . . . C14 C 0.7417(7) 0.6435(6) 0.3967(4) 0.0238(12) Uani 1 1 d . . . . . H14 H 0.7156 0.7277 0.3539 0.029 Uiso 1 1 calc R U . . . C15 C 0.8533(7) 0.5229(7) 0.3721(4) 0.0273(13) Uani 1 1 d . . . . . H15 H 0.9051 0.5253 0.3132 0.033 Uiso 1 1 calc R U . . . C16 C 0.8888(7) 0.3989(6) 0.4341(4) 0.0262(13) Uani 1 1 d . . . . . H16 H 0.9637 0.3161 0.4170 0.031 Uiso 1 1 calc R U . . . C17 C 0.8156(7) 0.3960(6) 0.5203(4) 0.0214(12) Uani 1 1 d . . . . . H17 H 0.8401 0.3108 0.5621 0.026 Uiso 1 1 calc R U . . . C18 C 0.4778(6) 0.2824(5) 0.8253(3) 0.0174(11) Uani 1 1 d . . . . . C19 C 0.3325(7) 0.2790(6) 0.8693(4) 0.0220(12) Uani 1 1 d . . . . . H19 H 0.2527 0.3645 0.8776 0.026 Uiso 1 1 calc R U . . . C20 C 0.3040(7) 0.1510(6) 0.9010(4) 0.0271(13) Uani 1 1 d . . . . . H20 H 0.2033 0.1497 0.9295 0.033 Uiso 1 1 calc R U . . . C21 C 0.4204(8) 0.0245(6) 0.8917(4) 0.0289(14) Uani 1 1 d . . . . . H21 H 0.4010 -0.0627 0.9150 0.035 Uiso 1 1 calc R U . . . C22 C 0.5636(7) 0.0278(6) 0.8483(4) 0.0255(13) Uani 1 1 d . . . . . H22 H 0.6438 -0.0579 0.8411 0.031 Uiso 1 1 calc R U . . . C23 C 0.5928(7) 0.1558(5) 0.8147(4) 0.0216(12) Uani 1 1 d . . . . . H23 H 0.6921 0.1564 0.7842 0.026 Uiso 1 1 calc R U . . . C24 C 0.7028(6) 0.5601(6) 0.8119(4) 0.0170(11) Uani 1 1 d . . . . . C25 C 0.6471(6) 0.4541(5) 0.8470(4) 0.0163(11) Uani 1 1 d . . . . . C26 C 0.8413(6) 0.6015(6) 0.8488(4) 0.0205(11) Uani 1 1 d . . . . . C27 C 0.6955(6) 0.3675(5) 0.9410(4) 0.0196(11) Uani 1 1 d . . . . . F1 F 0.9092(4) 0.6713(4) 0.7814(2) 0.0289(8) Uani 1 1 d . . . . . F2 F 0.9614(4) 0.4886(3) 0.8832(2) 0.0256(7) Uani 1 1 d . . . . . F3 F 0.7957(4) 0.6853(3) 0.9152(2) 0.0271(7) Uani 1 1 d . . . . . F4 F 0.8112(4) 0.2466(3) 0.9347(2) 0.0299(8) Uani 1 1 d . . . . . F5 F 0.7533(4) 0.4380(3) 0.9969(2) 0.0246(7) Uani 1 1 d . . . . . F6 F 0.5708(4) 0.3370(3) 0.9864(2) 0.0250(7) Uani 1 1 d . . . . . P1 P 0.59677(16) 0.66493(14) 0.70559(9) 0.0159(3) Uani 1 1 d . . . . . Cl1 Cl 0.69958(18) 1.06666(14) 0.58320(9) 0.0259(3) Uani 1 1 d . . . . . Au1 Au 0.65009(3) 0.86243(2) 0.64624(2) 0.01750(7) 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 C1 0.009(2) 0.026(3) 0.016(3) -0.006(2) -0.002(2) 0.001(2) C2 0.020(3) 0.010(3) 0.018(3) -0.004(2) -0.005(2) -0.001(2) C3 0.016(3) 0.014(3) 0.020(3) -0.005(2) 0.001(2) -0.004(2) C4 0.018(3) 0.017(3) 0.013(3) -0.001(2) -0.002(2) -0.003(2) C5 0.022(3) 0.018(3) 0.014(3) -0.007(2) 0.000(2) -0.003(2) C6 0.009(2) 0.018(3) 0.018(3) -0.004(2) -0.0014(19) -0.003(2) C7 0.021(3) 0.019(3) 0.021(3) -0.001(2) 0.001(2) -0.005(2) C8 0.018(3) 0.022(3) 0.025(3) -0.005(2) 0.002(2) -0.001(2) C9 0.021(3) 0.013(3) 0.037(3) 0.001(2) -0.006(2) 0.002(2) C10 0.016(3) 0.022(3) 0.033(3) 0.007(2) -0.002(2) -0.003(2) C11 0.018(3) 0.020(3) 0.023(3) 0.001(2) -0.002(2) -0.004(2) C12 0.018(3) 0.020(3) 0.014(3) -0.003(2) -0.001(2) -0.010(2) C13 0.019(3) 0.022(3) 0.020(3) -0.004(2) -0.007(2) -0.009(2) C14 0.035(3) 0.024(3) 0.016(3) 0.001(2) -0.005(2) -0.016(3) C15 0.029(3) 0.040(4) 0.019(3) -0.007(3) 0.002(2) -0.018(3) C16 0.022(3) 0.030(3) 0.026(3) -0.014(3) 0.003(2) -0.003(2) C17 0.025(3) 0.017(3) 0.022(3) -0.004(2) 0.000(2) -0.006(2) C18 0.024(3) 0.014(3) 0.015(3) -0.002(2) -0.003(2) -0.007(2) C19 0.023(3) 0.022(3) 0.021(3) -0.001(2) 0.001(2) -0.007(2) C20 0.027(3) 0.030(3) 0.027(3) 0.000(2) 0.000(2) -0.014(3) C21 0.045(4) 0.018(3) 0.027(3) -0.002(2) -0.008(3) -0.014(3) C22 0.038(3) 0.012(3) 0.024(3) -0.003(2) -0.001(3) -0.003(2) C23 0.033(3) 0.013(3) 0.017(3) -0.001(2) 0.002(2) -0.004(2) C24 0.014(3) 0.021(3) 0.017(3) -0.007(2) 0.001(2) -0.004(2) C25 0.014(3) 0.014(3) 0.018(3) -0.006(2) 0.005(2) 0.001(2) C26 0.022(3) 0.017(3) 0.023(3) -0.004(2) -0.001(2) -0.005(2) C27 0.020(3) 0.014(3) 0.024(3) -0.006(2) -0.002(2) -0.002(2) F1 0.0268(18) 0.035(2) 0.0286(19) 0.0031(15) -0.0038(14) -0.0182(15) F2 0.0161(16) 0.0207(17) 0.0373(19) -0.0030(14) -0.0074(14) -0.0008(13) F3 0.0289(18) 0.0242(18) 0.0318(19) -0.0140(14) -0.0014(14) -0.0081(14) F4 0.0325(19) 0.0184(18) 0.0305(19) -0.0023(14) -0.0048(15) 0.0057(14) F5 0.0327(18) 0.0238(18) 0.0196(17) -0.0015(13) -0.0062(14) -0.0114(14) F6 0.0294(18) 0.0285(19) 0.0183(16) 0.0009(13) 0.0008(13) -0.0121(14) P1 0.0181(7) 0.0129(7) 0.0168(7) -0.0019(5) -0.0006(5) -0.0044(5) Cl1 0.0395(8) 0.0183(7) 0.0226(7) -0.0003(5) -0.0003(6) -0.0137(6) Au1 0.02196(11) 0.01275(11) 0.01809(11) -0.00202(7) 0.00082(7) -0.00563(7) _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 C1 C2 1.291(7) . ? C1 C12 1.481(7) . ? C1 P1 1.847(5) . ? C2 C3 1.559(7) . ? C2 H2 0.9500 . ? C3 C18 1.537(7) . ? C3 C4 1.541(7) . ? C3 C25 1.579(7) . ? C4 C5 1.326(7) . ? C4 H4 0.9500 . ? C5 C6 1.477(7) . ? C5 P1 1.827(5) . ? C6 C11 1.399(7) . ? C6 C7 1.399(7) . ? C7 C8 1.390(7) . ? C7 H7 0.9500 . ? C8 C9 1.380(8) . ? C8 H8 0.9500 . ? C9 C10 1.378(8) . ? C9 H9 0.9500 . ? C10 C11 1.386(8) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.398(7) . ? C12 C17 1.412(7) . ? C13 C14 1.379(8) . ? C13 H13 0.9500 . ? C14 C15 1.391(8) . ? C14 H14 0.9500 . ? C15 C16 1.390(8) . ? C15 H15 0.9500 . ? C16 C17 1.380(8) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C23 1.390(7) . ? C18 C19 1.391(7) . ? C19 C20 1.388(8) . ? C19 H19 0.9500 . ? C20 C21 1.390(8) . ? C20 H20 0.9500 . ? C21 C22 1.371(8) . ? C21 H21 0.9500 . ? C22 C23 1.395(7) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.320(7) . ? C24 C26 1.518(7) . ? C24 P1 1.854(5) . ? C25 C27 1.516(7) . ? C26 F1 1.336(6) . ? C26 F3 1.343(6) . ? C26 F2 1.345(6) . ? C27 F6 1.327(6) . ? C27 F4 1.340(6) . ? C27 F5 1.347(6) . ? P1 Au1 2.2099(13) . ? Cl1 Au1 2.2699(13) . ? 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 C2 C1 C12 128.0(5) . . ? C2 C1 P1 111.9(4) . . ? C12 C1 P1 120.2(4) . . ? C1 C2 C3 121.7(5) . . ? C1 C2 H2 119.1 . . ? C3 C2 H2 119.1 . . ? C18 C3 C4 115.0(4) . . ? C18 C3 C2 109.1(4) . . ? C4 C3 C2 107.1(4) . . ? C18 C3 C25 114.4(4) . . ? C4 C3 C25 104.1(4) . . ? C2 C3 C25 106.4(4) . . ? C5 C4 C3 120.2(5) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 125.9(5) . . ? C4 C5 P1 112.7(4) . . ? C6 C5 P1 121.4(4) . . ? C11 C6 C7 118.5(5) . . ? C11 C6 C5 121.3(5) . . ? C7 C6 C5 120.2(5) . . ? C8 C7 C6 120.4(5) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C9 C8 C7 120.1(5) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C10 C9 C8 120.3(5) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 120.1(5) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C6 120.6(5) . . ? C10 C11 H11 119.7 . . ? C6 C11 H11 119.7 . . ? C13 C12 C17 118.3(5) . . ? C13 C12 C1 122.3(5) . . ? C17 C12 C1 119.4(5) . . ? C14 C13 C12 120.8(5) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 120.4(5) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 119.8(5) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C17 C16 C15 120.2(5) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C12 120.6(5) . . ? C16 C17 H17 119.7 . . ? C12 C17 H17 119.7 . . ? C23 C18 C19 118.7(5) . . ? C23 C18 C3 118.3(5) . . ? C19 C18 C3 122.9(5) . . ? C20 C19 C18 120.0(5) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 121.1(6) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C22 C21 C20 118.9(5) . . ? C22 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? C21 C22 C23 120.7(5) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C18 C23 C22 120.6(5) . . ? C18 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C25 C24 C26 127.1(5) . . ? C25 C24 P1 114.2(4) . . ? C26 C24 P1 118.7(4) . . ? C24 C25 C27 124.0(5) . . ? C24 C25 C3 117.3(5) . . ? C27 C25 C3 118.7(4) . . ? F1 C26 F3 106.5(4) . . ? F1 C26 F2 105.5(4) . . ? F3 C26 F2 107.8(4) . . ? F1 C26 C24 111.3(4) . . ? F3 C26 C24 113.3(4) . . ? F2 C26 C24 112.0(4) . . ? F6 C27 F4 108.1(4) . . ? F6 C27 F5 105.5(4) . . ? F4 C27 F5 106.7(4) . . ? F6 C27 C25 112.1(4) . . ? F4 C27 C25 112.5(4) . . ? F5 C27 C25 111.6(4) . . ? C5 P1 C1 99.5(2) . . ? C5 P1 C24 97.1(2) . . ? C1 P1 C24 95.0(2) . . ? C5 P1 Au1 117.46(18) . . ? C1 P1 Au1 122.56(18) . . ? C24 P1 Au1 119.89(17) . . ? P1 Au1 Cl1 178.66(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 C12 C1 C2 C3 178.1(5) . . . . ? P1 C1 C2 C3 -0.6(6) . . . . ? C1 C2 C3 C18 179.8(5) . . . . ? C1 C2 C3 C4 54.8(6) . . . . ? C1 C2 C3 C25 -56.2(6) . . . . ? C18 C3 C4 C5 -176.1(5) . . . . ? C2 C3 C4 C5 -54.7(6) . . . . ? C25 C3 C4 C5 57.8(6) . . . . ? C3 C4 C5 C6 -178.1(5) . . . . ? C3 C4 C5 P1 1.2(6) . . . . ? C4 C5 C6 C11 -137.6(6) . . . . ? P1 C5 C6 C11 43.1(6) . . . . ? C4 C5 C6 C7 42.7(8) . . . . ? P1 C5 C6 C7 -136.6(4) . . . . ? C11 C6 C7 C8 -1.3(8) . . . . ? C5 C6 C7 C8 178.4(5) . . . . ? C6 C7 C8 C9 0.1(8) . . . . ? C7 C8 C9 C10 1.8(9) . . . . ? C8 C9 C10 C11 -2.6(9) . . . . ? C9 C10 C11 C6 1.4(8) . . . . ? C7 C6 C11 C10 0.5(8) . . . . ? C5 C6 C11 C10 -179.2(5) . . . . ? C2 C1 C12 C13 144.1(6) . . . . ? P1 C1 C12 C13 -37.3(6) . . . . ? C2 C1 C12 C17 -36.6(8) . . . . ? P1 C1 C12 C17 142.0(4) . . . . ? C17 C12 C13 C14 -0.9(7) . . . . ? C1 C12 C13 C14 178.5(5) . . . . ? C12 C13 C14 C15 -0.4(8) . . . . ? C13 C14 C15 C16 1.4(8) . . . . ? C14 C15 C16 C17 -1.0(8) . . . . ? C15 C16 C17 C12 -0.3(8) . . . . ? C13 C12 C17 C16 1.2(8) . . . . ? C1 C12 C17 C16 -178.2(5) . . . . ? C4 C3 C18 C23 167.0(5) . . . . ? C2 C3 C18 C23 46.7(6) . . . . ? C25 C3 C18 C23 -72.4(6) . . . . ? C4 C3 C18 C19 -13.3(7) . . . . ? C2 C3 C18 C19 -133.6(5) . . . . ? C25 C3 C18 C19 107.3(6) . . . . ? C23 C18 C19 C20 -0.5(8) . . . . ? C3 C18 C19 C20 179.8(5) . . . . ? C18 C19 C20 C21 1.6(9) . . . . ? C19 C20 C21 C22 -1.6(9) . . . . ? C20 C21 C22 C23 0.5(9) . . . . ? C19 C18 C23 C22 -0.6(8) . . . . ? C3 C18 C23 C22 179.1(5) . . . . ? C21 C22 C23 C18 0.6(8) . . . . ? C26 C24 C25 C27 10.5(8) . . . . ? P1 C24 C25 C27 -170.1(4) . . . . ? C26 C24 C25 C3 -171.8(5) . . . . ? P1 C24 C25 C3 7.6(6) . . . . ? C18 C3 C25 C24 170.9(4) . . . . ? C4 C3 C25 C24 -62.7(6) . . . . ? C2 C3 C25 C24 50.3(6) . . . . ? C18 C3 C25 C27 -11.2(6) . . . . ? C4 C3 C25 C27 115.2(5) . . . . ? C2 C3 C25 C27 -131.8(4) . . . . ? C25 C24 C26 F1 154.5(5) . . . . ? P1 C24 C26 F1 -24.8(6) . . . . ? C25 C24 C26 F3 -85.5(7) . . . . ? P1 C24 C26 F3 95.1(5) . . . . ? C25 C24 C26 F2 36.7(7) . . . . ? P1 C24 C26 F2 -142.7(4) . . . . ? C24 C25 C27 F6 139.7(5) . . . . ? C3 C25 C27 F6 -38.0(6) . . . . ? C24 C25 C27 F4 -98.2(6) . . . . ? C3 C25 C27 F4 84.1(5) . . . . ? C24 C25 C27 F5 21.7(7) . . . . ? C3 C25 C27 F5 -156.0(4) . . . . ? C4 C5 P1 C1 46.7(4) . . . . ? C6 C5 P1 C1 -133.9(4) . . . . ? C4 C5 P1 C24 -49.6(4) . . . . ? C6 C5 P1 C24 129.8(4) . . . . ? C4 C5 P1 Au1 -178.7(3) . . . . ? C6 C5 P1 Au1 0.7(5) . . . . ? C2 C1 P1 C5 -47.0(4) . . . . ? C12 C1 P1 C5 134.2(4) . . . . ? C2 C1 P1 C24 51.1(4) . . . . ? C12 C1 P1 C24 -127.7(4) . . . . ? C2 C1 P1 Au1 -178.4(3) . . . . ? C12 C1 P1 Au1 2.7(5) . . . . ? C25 C24 P1 C5 44.8(4) . . . . ? C26 C24 P1 C5 -135.8(4) . . . . ? C25 C24 P1 C1 -55.5(4) . . . . ? C26 C24 P1 C1 124.0(4) . . . . ? C25 C24 P1 Au1 172.2(3) . . . . ? C26 C24 P1 Au1 -8.3(5) . . . . ? _refine_diff_density_max 1.179 _refine_diff_density_min -1.061 _refine_diff_density_rms 0.158 _shelx_res_file ; MK05_a.res created by SHELXL-2014/7 TITL MK05_a.res in P-1 REM Old TITL MK05 in P-1 REM SHELXT solution in P-1 REM R1 0.073, Rweak 0.016, Alpha 0.047, Orientation as input REM Formula found by SHELXT: C30 F3 P Cl Au CELL 0.71073 8.6440 10.0254 14.5537 81.7475 87.4505 73.0847 ZERR 2.000 0.0002 0.0002 0.0003 0.0008 0.0008 0.0007 LATT 1 SFAC C H F P CL AU UNIT 54 34 12 2 2 2 TEMP -100.00 SIZE 0.090 0.100 0.600 L.S. 30 BOND $H LIST 6 acta conf FMAP 2 PLAN 20 WGHT 0.014700 4.809600 FVAR 0.33844 C1 1 0.631660 0.513290 0.640751 11.00000 0.00897 0.02580 = 0.01624 -0.00644 -0.00189 0.00071 C2 1 0.588367 0.410782 0.688057 11.00000 0.02004 0.01047 = 0.01771 -0.00444 -0.00506 -0.00111 AFIX 43 H2 2 0.599959 0.327463 0.661171 11.00000 -1.20000 AFIX 0 C3 1 0.517594 0.420164 0.788103 11.00000 0.01588 0.01407 = 0.01972 -0.00547 0.00124 -0.00422 C4 1 0.372556 0.553757 0.782680 11.00000 0.01769 0.01712 = 0.01322 -0.00148 -0.00209 -0.00349 AFIX 43 H4 2 0.269684 0.547500 0.805174 11.00000 -1.20000 AFIX 0 C5 1 0.390933 0.677454 0.746697 11.00000 0.02219 0.01796 = 0.01447 -0.00658 0.00021 -0.00344 C6 1 0.264177 0.813985 0.739613 11.00000 0.00907 0.01787 = 0.01844 -0.00351 -0.00143 -0.00348 C7 1 0.158912 0.848005 0.814081 11.00000 0.02066 0.01866 = 0.02141 -0.00074 0.00068 -0.00517 AFIX 43 H7 2 0.167332 0.782038 0.868784 11.00000 -1.20000 AFIX 0 C8 1 0.042070 0.977784 0.808487 11.00000 0.01809 0.02241 = 0.02521 -0.00461 0.00200 -0.00082 AFIX 43 H8 2 -0.028911 1.000302 0.859357 11.00000 -1.20000 AFIX 0 C9 1 0.028995 1.073990 0.729153 11.00000 0.02101 0.01339 = 0.03743 0.00060 -0.00597 0.00237 AFIX 43 H9 2 -0.048939 1.163623 0.726263 11.00000 -1.20000 AFIX 0 C10 1 0.128531 1.040562 0.654111 11.00000 0.01626 0.02171 = 0.03339 0.00707 -0.00193 -0.00269 AFIX 43 H10 2 0.116098 1.105641 0.598745 11.00000 -1.20000 AFIX 0 C11 1 0.246777 0.912113 0.659291 11.00000 0.01815 0.02021 = 0.02310 0.00060 -0.00172 -0.00427 AFIX 43 H11 2 0.316615 0.890544 0.607826 11.00000 -1.20000 AFIX 0 C12 1 0.704588 0.518485 0.546764 11.00000 0.01755 0.01997 = 0.01445 -0.00267 -0.00081 -0.00979 C13 1 0.668718 0.641491 0.482881 11.00000 0.01935 0.02219 = 0.02025 -0.00428 -0.00664 -0.00857 AFIX 43 H13 2 0.593211 0.724657 0.499045 11.00000 -1.20000 AFIX 0 C14 1 0.741689 0.643462 0.396686 11.00000 0.03541 0.02393 = 0.01641 0.00069 -0.00513 -0.01617 AFIX 43 H14 2 0.715575 0.727652 0.353857 11.00000 -1.20000 AFIX 0 C15 1 0.853285 0.522923 0.372093 11.00000 0.02892 0.03984 = 0.01878 -0.00654 0.00170 -0.01786 AFIX 43 H15 2 0.905058 0.525281 0.313166 11.00000 -1.20000 AFIX 0 C16 1 0.888809 0.398947 0.434062 11.00000 0.02222 0.02989 = 0.02635 -0.01361 0.00254 -0.00318 AFIX 43 H16 2 0.963651 0.316066 0.417024 11.00000 -1.20000 AFIX 0 C17 1 0.815612 0.395998 0.520262 11.00000 0.02527 0.01719 = 0.02228 -0.00422 -0.00017 -0.00601 AFIX 43 H17 2 0.840120 0.310819 0.562148 11.00000 -1.20000 AFIX 0 C18 1 0.477794 0.282398 0.825257 11.00000 0.02441 0.01441 = 0.01483 -0.00169 -0.00301 -0.00743 C19 1 0.332487 0.279045 0.869272 11.00000 0.02338 0.02168 = 0.02082 -0.00140 0.00115 -0.00698 AFIX 43 H19 2 0.252729 0.364476 0.877630 11.00000 -1.20000 AFIX 0 C20 1 0.303999 0.150954 0.900977 11.00000 0.02700 0.03014 = 0.02665 -0.00009 -0.00008 -0.01374 AFIX 43 H20 2 0.203327 0.149671 0.929491 11.00000 -1.20000 AFIX 0 C21 1 0.420360 0.024546 0.891684 11.00000 0.04491 0.01808 = 0.02733 -0.00167 -0.00787 -0.01436 AFIX 43 H21 2 0.400994 -0.062670 0.914978 11.00000 -1.20000 AFIX 0 C22 1 0.563619 0.027817 0.848321 11.00000 0.03790 0.01223 = 0.02381 -0.00337 -0.00125 -0.00282 AFIX 43 H22 2 0.643787 -0.057907 0.841142 11.00000 -1.20000 AFIX 0 C23 1 0.592779 0.155782 0.814651 11.00000 0.03283 0.01312 = 0.01693 -0.00073 0.00186 -0.00437 AFIX 43 H23 2 0.692139 0.156377 0.784197 11.00000 -1.20000 AFIX 0 C24 1 0.702794 0.560076 0.811929 11.00000 0.01388 0.02079 = 0.01673 -0.00710 0.00114 -0.00352 C25 1 0.647136 0.454059 0.847007 11.00000 0.01431 0.01400 = 0.01804 -0.00573 0.00489 0.00108 C26 1 0.841296 0.601514 0.848772 11.00000 0.02174 0.01718 = 0.02271 -0.00403 -0.00105 -0.00480 C27 1 0.695524 0.367484 0.941021 11.00000 0.02013 0.01396 = 0.02432 -0.00622 -0.00244 -0.00216 F1 3 0.909176 0.671260 0.781369 11.00000 0.02678 0.03518 = 0.02860 0.00308 -0.00381 -0.01817 F2 3 0.961352 0.488581 0.883235 11.00000 0.01613 0.02068 = 0.03734 -0.00297 -0.00736 -0.00075 F3 3 0.795688 0.685284 0.915249 11.00000 0.02893 0.02416 = 0.03178 -0.01398 -0.00143 -0.00806 F4 3 0.811225 0.246563 0.934672 11.00000 0.03252 0.01836 = 0.03046 -0.00229 -0.00480 0.00569 F5 3 0.753262 0.437954 0.996854 11.00000 0.03268 0.02385 = 0.01964 -0.00146 -0.00621 -0.01143 F6 3 0.570831 0.336986 0.986359 11.00000 0.02941 0.02848 = 0.01826 0.00089 0.00078 -0.01215 P1 4 0.596769 0.664932 0.705590 11.00000 0.01813 0.01289 = 0.01678 -0.00187 -0.00062 -0.00444 CL1 5 0.699584 1.066659 0.583196 11.00000 0.03949 0.01831 = 0.02264 -0.00035 -0.00029 -0.01369 AU1 6 0.650087 0.862433 0.646241 11.00000 0.02196 0.01275 = 0.01809 -0.00202 0.00082 -0.00563 HKLF 4 REM MK05_a.res in P-1 REM R1 = 0.0308 for 4374 Fo > 4sig(Fo) and 0.0380 for all 4867 data REM 325 parameters refined using 0 restraints END WGHT 0.0147 4.8096 REM Highest difference peak 1.179, deepest hole -1.061, 1-sigma level 0.158 Q1 1 0.6659 0.2625 0.6547 11.00000 0.05 1.18 Q2 1 0.7133 0.8335 0.7154 11.00000 0.05 1.12 Q3 1 0.5237 0.8783 0.6352 11.00000 0.05 1.06 Q4 1 0.6962 0.8768 0.5827 11.00000 0.05 0.92 Q5 1 0.5000 0.5000 0.5000 10.50000 0.05 0.85 Q6 1 0.6052 0.8413 0.7031 11.00000 0.05 0.83 Q7 1 0.9388 0.2980 0.3576 11.00000 0.05 0.72 Q8 1 0.7836 0.8214 0.6501 11.00000 0.05 0.69 Q9 1 0.3194 0.0221 0.9392 11.00000 0.05 0.68 Q10 1 0.0259 1.2965 0.6412 11.00000 0.05 0.66 Q11 1 0.6537 0.4364 0.6523 11.00000 0.05 0.62 Q12 1 -0.1343 1.0115 0.9209 11.00000 0.05 0.62 Q13 1 0.7208 0.4825 0.8214 11.00000 0.05 0.61 Q14 1 0.0445 0.8908 0.6240 11.00000 0.05 0.59 Q15 1 0.3596 0.4197 0.9433 11.00000 0.05 0.59 Q16 1 0.4698 0.2549 1.0583 11.00000 0.05 0.58 Q17 1 0.8294 0.8625 0.5786 11.00000 0.05 0.55 Q18 1 0.7857 0.0560 0.7813 11.00000 0.05 0.54 Q19 1 0.9361 0.6634 0.9362 11.00000 0.05 0.54 Q20 1 0.5778 0.9305 0.4623 11.00000 0.05 0.54 ; _shelx_res_checksum 30981 _shelx_hkl_file ; -1 0 0 2311.57 75.19 -1 0 0 2401.56 75.99 -1 0 0 2326.07 75.19 1 0 0 2264.07 75.79 1 0 0 2394.26 75.19 -2 0 0 1127.69 39.50 -2 0 0 1159.78 41.00 -2 0 0 1162.58 39.60 2 0 0 1116.39 39.70 2 0 0 1090.99 40.20 -3 0 0 2616.64 90.29 -3 0 0 2722.63 88.39 -3 0 0 2607.14 88.09 3 0 0 2611.74 88.59 3 0 0 2546.25 88.99 3 0 0 2614.94 88.09 -4 0 0 1293.07 49.60 -4 0 0 1287.67 52.39 -4 0 0 1434.66 50.19 4 0 0 1262.87 50.09 4 0 0 1274.57 49.60 4 0 0 1403.16 48.30 -5 0 0 12.60 7.60 -5 0 0 6.80 7.00 -5 0 0 3.40 8.00 5 0 0 11.30 7.40 5 0 0 13.50 8.10 5 0 0 18.00 6.80 -6 0 0 414.36 25.10 -6 0 0 388.26 28.50 -6 0 0 409.76 25.30 6 0 0 347.47 23.90 6 0 0 394.86 25.80 6 0 0 406.86 24.30 -7 0 0 272.87 23.60 -7 0 0 269.77 27.80 -7 0 0 285.27 27.80 7 0 0 316.87 25.80 7 0 0 285.17 23.90 7 0 0 248.78 25.20 -8 0 0 18.10 15.20 -8 0 0 -1.90 14.70 -8 0 0 27.40 13.70 8 0 0 29.00 19.40 8 0 0 11.20 12.00 -9 0 0 51.79 18.30 -9 0 0 25.10 20.80 -9 0 0 22.20 16.30 9 0 0 49.00 19.50 9 0 0 36.30 16.20 -10 0 0 150.68 26.80 -10 0 0 125.89 31.50 10 0 0 168.58 32.20 10 0 0 147.79 25.60 10 -1 0 69.99 22.70 -10 1 0 51.79 24.00 -10 1 0 81.79 26.10 9 -1 0 318.07 34.40 9 -1 0 390.26 38.80 -9 1 0 310.77 44.00 8 -1 0 277.57 31.20 8 -1 0 246.78 26.80 -8 1 0 214.88 27.00 -8 1 0 254.27 35.50 7 -1 0 27.40 11.30 7 -1 0 36.30 13.90 -7 1 0 42.30 16.90 -7 1 0 24.50 11.90 -7 1 0 40.20 12.60 6 -1 0 815.22 39.60 6 -1 0 794.82 37.70 -6 1 0 820.02 44.30 -6 1 0 787.02 37.60 -6 1 0 807.92 37.50 5 -1 0 921.91 42.10 5 -1 0 910.21 39.40 5 -1 0 897.21 40.00 5 -1 0 913.91 39.00 -5 1 0 890.51 38.40 -5 1 0 878.11 38.40 -5 1 0 932.81 44.90 4 -1 0 77.09 10.30 4 -1 0 94.89 13.20 4 -1 0 107.19 12.90 4 -1 0 75.39 10.60 -4 1 0 89.19 11.40 -4 1 0 92.79 13.40 -4 1 0 89.79 11.00 3 -1 0 1636.24 54.39 3 -1 0 1480.85 56.69 3 -1 0 1489.05 53.09 -3 1 0 1500.15 52.69 -3 1 0 1440.86 52.59 -3 1 0 1408.66 57.19 2 -1 0 1364.16 50.39 2 -1 0 1388.86 46.90 2 -1 0 1350.06 46.80 2 -1 0 1412.76 48.30 -2 1 0 1305.87 46.40 -2 1 0 1357.46 46.60 -2 1 0 1354.16 50.79 1 -1 0 191.68 8.20 1 -1 0 193.58 8.20 1 -1 0 216.28 10.10 1 -1 0 193.28 10.80 -1 1 0 210.28 9.10 -1 1 0 189.68 10.90 -1 1 0 186.38 9.60 -1 1 0 188.88 8.00 0 -1 0 20.70 3.80 -1 -1 0 1411.26 45.90 -1 -1 0 1312.87 44.40 -1 -1 0 1376.06 44.50 1 1 0 1277.37 44.30 1 1 0 1454.65 44.10 1 1 0 1322.17 44.30 -2 -1 0 723.03 26.80 -2 -1 0 737.03 27.10 2 1 0 731.73 27.00 2 1 0 714.93 26.70 -3 -1 0 213.38 11.90 -3 -1 0 197.78 12.10 3 1 0 205.98 12.60 3 1 0 202.68 12.10 -4 -1 0 1406.56 51.49 -4 -1 0 1336.47 50.69 -4 -1 0 1391.26 50.99 4 1 0 1324.27 51.09 4 1 0 1327.87 50.49 -5 -1 0 534.95 27.40 -5 -1 0 530.75 26.50 -5 -1 0 519.15 26.80 5 1 0 488.25 25.90 5 1 0 513.35 27.20 5 1 0 562.54 22.90 -6 -1 0 7.40 8.90 -6 -1 0 4.10 9.10 -6 -1 0 -4.90 8.00 6 1 0 16.60 7.80 6 1 0 2.30 8.60 6 1 0 3.20 7.70 -7 -1 0 256.27 23.40 -7 -1 0 253.77 25.60 7 1 0 289.77 24.80 7 1 0 277.37 21.00 7 1 0 253.27 22.60 -8 -1 0 384.06 33.10 -8 -1 0 405.26 31.20 -8 -1 0 371.56 30.00 8 1 0 447.76 28.50 8 1 0 293.77 36.70 -9 -1 0 8.50 15.70 -9 -1 0 -23.00 17.80 -9 -1 0 9.20 16.90 9 1 0 3.40 21.30 9 1 0 23.50 15.00 -10 -1 0 140.99 28.10 -10 -1 0 213.98 32.00 -10 -1 0 130.19 25.60 10 1 0 117.99 28.20 10 1 0 158.98 25.00 9 -2 0 173.38 27.40 9 -2 0 139.59 25.10 -9 2 0 214.08 36.20 -9 2 0 178.88 24.80 8 -2 0 445.56 35.80 8 -2 0 414.26 32.30 -8 2 0 401.66 32.80 -8 2 0 372.06 33.60 -8 2 0 546.15 70.69 7 -2 0 177.18 25.10 7 -2 0 244.78 23.10 -7 2 0 209.48 23.50 -7 2 0 223.68 33.40 -7 2 0 226.78 19.60 6 -2 0 216.48 24.20 6 -2 0 201.88 23.00 6 -2 0 261.47 20.70 -6 2 0 255.07 21.00 -6 2 0 256.87 28.60 5 -2 0 1277.47 54.79 5 -2 0 1150.08 51.99 5 -2 0 1153.08 49.80 5 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400.46 42.10 -1 -5 -17 394.36 44.10 1 5 17 408.26 41.20 1 5 17 424.46 44.10 -2 -5 -17 300.17 41.00 -2 -5 -17 401.86 52.79 2 5 17 382.16 41.40 2 5 17 397.26 39.80 -3 -5 -17 25.40 23.30 3 5 17 -24.00 20.10 3 5 17 33.70 26.30 1 6 17 -63.79 26.00 2 6 17 112.89 31.80 0 -1 -18 369.16 44.40 0 1 18 348.67 44.70 -1 -1 -18 164.68 28.70 1 1 18 176.18 29.40 -1 2 18 34.10 28.80 0 -2 -18 73.59 24.70 0 2 18 76.29 25.00 0 2 18 106.09 32.00 -1 -2 -18 116.99 26.90 1 2 18 116.49 27.30 1 2 18 94.39 31.50 0 -3 -18 -21.40 22.50 0 3 18 -4.70 27.10 -1 -3 -18 144.19 26.70 1 3 18 152.78 27.30 1 3 18 134.19 30.50 2 3 18 158.88 34.20 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 41565 #============================================================================== _publ_requested_journal '??????' _publ_contact_author ; Prof. Dr.Christian M\"uller Freie Universit\"at Berlin Institut f\"ur Chemie und Biochemie Anorganische Chemie Fabeckstr. 34-36 14195 Berlin Germany ; _publ_contact_letter ; ; _publ_requested_coeditor_name ? _publ_contact_author_phone '+49/(0)3083854004' _publ_contact_author_fax '+49/(0)3083852440' _publ_contact_author_email c.mueller@fu-berlin.de loop_ _publ_author_name _publ_author_address 'M\"uller, Christian' ; Freie Universit\"at Berlin Institut f\"ur Chemie und Biochemie Anorganische Chemie Fabeckstr. 34-36 14195 Berlin Germany ; 'Rigo, Massimo' ; Freie Universit\"at Berlin Institut f\"ur Chemie und Biochemie Anorganische Chemie Fabeckstr. 34-36 14195 Berlin Germany ; 'Kleoff, Merlin' ; Freie Universit\"at Berlin Institut f\"ur Chemie und Biochemie Anorganische Chemie Fabeckstr. 34-36 14195 Berlin Germany ; 'Weber, Manuela' ; Freie Universit\"at Berlin Institut f\"ur Chemie und Biochemie Anorganische Chemie Fabeckstr. 34-36 14195 Berlin Germany ; 'Wiecko, Jelena' ; Freie Universit\"at Berlin Institut f\"ur Chemie und Biochemie Anorganische Chemie Fabeckstr. 34-36 14195 Berlin Germany ; _publ_section_title ; ... see the published paper. ; _publ_section_abstract ; ... and following paragraphs: see the published paper. ; _publ_section_experimental ; ; _publ_section_comment ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; #END====================================================