# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name _publ_author_address 'Ross Widenhoefer' ;French Family Science Center Duke University Durham, North Carolina 27708-0346 ; 'Timothy J. Brown' ;French Family Science Center Duke University Durham, North Carolina 27708-0346 ; 'Marina G. Dickens' ;French Family Science Center Duke University Durham, North Carolina 27708-0346 ; _publ_contact_author_name 'Ross Widenhoefer' _publ_contact_author_email RWIDENHO@CHEM.DUKE.EDU _publ_section_title ; Syntheses and X-ray Crystal Structures of Cationic, Two-Coordinate Gold(I) pi-Alkene Complexes that Contain a Sterically Hindered o-Biphenylphosphine Ligand ; _publ_contact_author_address ;French Family Science Center Duke University Durham, North Carolina 27708-0346 ; _publ_contact_author_phone '(919) 660-1533' # Attachment '1a-i_structures_final_9_1.cif' data_mono _database_code_depnum_ccdc_archive 'CCDC 740535' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '((P)Au(eta2-H2C=C(CH2)5))+ SbF6-' _chemical_melting_point ? _chemical_formula_moiety 'C27 H39 Au P, F6 Sb' _chemical_formula_sum 'C27 H39 Au F6 P Sb' _chemical_formula_weight 827.27 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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' _symmetry_space_group_name_Hall '-P 2ybc' 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 8.1045(9) _cell_length_b 17.2929(19) _cell_length_c 20.611(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.833(6) _cell_angle_gamma 90.00 _cell_volume 2873.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9923 _cell_measurement_theta_min 2.78 _cell_measurement_theta_max 33.55 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max .21 _exptl_crystal_size_mid .19 _exptl_crystal_size_min .12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.912 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 6.149 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.268 _exptl_absorpt_correction_T_max 0.478 _exptl_absorpt_process_details 'SADABS 2.10 (Sheldrick, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 73553 _diffrn_reflns_av_R_equivalents 0.0587 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 34.65 _reflns_number_total 11601 _reflns_number_gt 9446 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex II 2.0 Rev.2 (Bruker, 2005)' _computing_cell_refinement SAINT _computing_data_reduction 'SAINT 7.12A (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material 'SHELXS-97 (Sheldrick, 1990)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The diffraction measured theta max is 0.94 - very near 1.0. While a full collection was completed, some significant icing occured during collection and required the exclusion of some frames. The low Ueq for Sb can be explained by the motion of the F atoms, yielding higher Ueqs, around the central Sb. The short bond length of C1 to C2 is typical of double bonds conjugated to a gold atom. The counterion was not moved into the cell, as it is not pertinent to the main residue. ; _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^)+(0.0236P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11601 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0650 _refine_ls_wR_factor_gt 0.0612 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.142 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.403085(12) 0.757925(5) 0.173337(4) 0.01821(3) Uani 1 1 d . . . P1 P 0.49722(7) 0.79533(3) 0.07657(3) 0.01489(11) Uani 1 1 d . . . C1 C 0.3576(4) 0.71493(16) 0.27091(13) 0.0279(6) Uani 1 1 d . . . H1A H 0.2674 0.6764 0.2715 0.033 Uiso 1 1 calc R . . H1B H 0.4579 0.7003 0.2997 0.033 Uiso 1 1 calc R . . C2 C 0.3097(3) 0.79057(14) 0.27486(11) 0.0194(5) Uani 1 1 d . . . C3 C 0.4219(3) 0.85153(15) 0.30665(12) 0.0225(5) Uani 1 1 d . . . H3A H 0.4261 0.8964 0.2771 0.027 Uiso 1 1 calc R . . H3B H 0.5356 0.8307 0.3159 0.027 Uiso 1 1 calc R . . C4 C 0.3554(3) 0.87717(16) 0.37086(12) 0.0252(5) Uani 1 1 d . . . H4A H 0.3616 0.8333 0.4018 0.030 Uiso 1 1 calc R . . H4B H 0.4254 0.9195 0.3908 0.030 Uiso 1 1 calc R . . C5 C 0.1772(3) 0.90469(15) 0.35863(14) 0.0277(6) Uani 1 1 d . . . H5A H 0.1726 0.9516 0.3310 0.033 Uiso 1 1 calc R . . H5B H 0.1357 0.9185 0.4007 0.033 Uiso 1 1 calc R . . C6 C 0.0670(3) 0.84236(17) 0.32509(13) 0.0276(6) Uani 1 1 d . . . H6A H -0.0470 0.8628 0.3154 0.033 Uiso 1 1 calc R . . H6B H 0.0622 0.7976 0.3548 0.033 Uiso 1 1 calc R . . C7 C 0.1324(3) 0.81551(15) 0.26124(13) 0.0238(5) Uani 1 1 d . . . H7A H 0.0645 0.7718 0.2424 0.029 Uiso 1 1 calc R . . H7B H 0.1242 0.8584 0.2292 0.029 Uiso 1 1 calc R . . C8 C 0.6873(3) 0.85511(15) 0.10325(12) 0.0221(5) Uani 1 1 d . . . C9 C 0.7458(3) 0.91017(16) 0.05196(14) 0.0283(6) Uani 1 1 d . . . H9A H 0.8448 0.9381 0.0706 0.042 Uiso 1 1 calc R . . H9B H 0.6575 0.9473 0.0385 0.042 Uiso 1 1 calc R . . H9C H 0.7726 0.8804 0.0140 0.042 Uiso 1 1 calc R . . C10 C 0.8261(3) 0.79790(18) 0.12557(15) 0.0322(6) Uani 1 1 d . . . H10A H 0.9278 0.8265 0.1398 0.048 Uiso 1 1 calc R . . H10B H 0.8461 0.7637 0.0893 0.048 Uiso 1 1 calc R . . H10C H 0.7931 0.7669 0.1619 0.048 Uiso 1 1 calc R . . C11 C 0.6513(4) 0.90428(17) 0.16293(14) 0.0341(7) Uani 1 1 d . . . H11A H 0.7489 0.9356 0.1774 0.051 Uiso 1 1 calc R . . H11B H 0.6257 0.8700 0.1985 0.051 Uiso 1 1 calc R . . H11C H 0.5564 0.9383 0.1508 0.051 Uiso 1 1 calc R . . C12 C 0.3379(3) 0.84763(13) 0.02164(12) 0.0196(5) Uani 1 1 d . . . C13 C 0.3928(3) 0.86860(15) -0.04573(13) 0.0247(5) Uani 1 1 d . . . H13A H 0.3026 0.8959 -0.0715 0.037 Uiso 1 1 calc R . . H13B H 0.4199 0.8212 -0.0685 0.037 Uiso 1 1 calc R . . H13C H 0.4909 0.9020 -0.0399 0.037 Uiso 1 1 calc R . . C14 C 0.2850(4) 0.92027(15) 0.05668(15) 0.0300(6) Uani 1 1 d . . . H14A H 0.2014 0.9484 0.0281 0.045 Uiso 1 1 calc R . . H14B H 0.3817 0.9536 0.0675 0.045 Uiso 1 1 calc R . . H14C H 0.2379 0.9053 0.0968 0.045 Uiso 1 1 calc R . . C15 C 0.1870(3) 0.79374(16) 0.00946(15) 0.0277(6) Uani 1 1 d . . . H15A H 0.1004 0.8194 -0.0195 0.042 Uiso 1 1 calc R . . H15B H 0.1441 0.7817 0.0511 0.042 Uiso 1 1 calc R . . H15C H 0.2203 0.7458 -0.0110 0.042 Uiso 1 1 calc R . . C16 C 0.5722(3) 0.71378(13) 0.03098(11) 0.0155(4) Uani 1 1 d . . . C17 C 0.5503(3) 0.63617(13) 0.04969(11) 0.0165(4) Uani 1 1 d . . . C18 C 0.6422(3) 0.57908(14) 0.02182(13) 0.0223(5) Uani 1 1 d . . . H18A H 0.6331 0.5270 0.0358 0.027 Uiso 1 1 calc R . . C19 C 0.7468(3) 0.59606(15) -0.02587(14) 0.0263(5) Uani 1 1 d . . . H19A H 0.8091 0.5561 -0.0436 0.032 Uiso 1 1 calc R . . C20 C 0.7594(3) 0.67148(15) -0.04724(13) 0.0235(5) Uani 1 1 d . . . H20A H 0.8258 0.6834 -0.0813 0.028 Uiso 1 1 calc R . . C21 C 0.6743(3) 0.72924(14) -0.01841(13) 0.0210(5) Uani 1 1 d . . . H21A H 0.6853 0.7811 -0.0325 0.025 Uiso 1 1 calc R . . C22 C 0.4297(3) 0.60898(13) 0.09512(12) 0.0190(4) Uani 1 1 d . . . C23 C 0.4839(3) 0.57414(14) 0.15430(13) 0.0243(5) Uani 1 1 d . . . H23A H 0.5992 0.5714 0.1681 0.029 Uiso 1 1 calc R . . C24 C 0.3694(4) 0.54306(15) 0.19365(14) 0.0310(6) Uani 1 1 d . . . H24A H 0.4077 0.5192 0.2339 0.037 Uiso 1 1 calc R . . C25 C 0.2010(4) 0.54676(15) 0.17439(15) 0.0325(7) Uani 1 1 d . . . H25A H 0.1237 0.5255 0.2012 0.039 Uiso 1 1 calc R . . C26 C 0.1463(3) 0.58171(16) 0.11587(15) 0.0303(6) Uani 1 1 d . . . H26A H 0.0308 0.5854 0.1028 0.036 Uiso 1 1 calc R . . C27 C 0.2595(3) 0.61156(14) 0.07597(14) 0.0246(5) Uani 1 1 d . . . H27A H 0.2205 0.6340 0.0352 0.030 Uiso 1 1 calc R . . Sb1 Sb -0.13653(2) 0.596555(9) 0.323635(9) 0.02346(4) Uani 1 1 d . . . F1 F -0.3502(3) 0.55477(14) 0.31519(12) 0.0670(7) Uani 1 1 d . . . F2 F 0.0743(2) 0.63808(14) 0.33085(10) 0.0568(6) Uani 1 1 d . . . F3 F -0.1515(3) 0.61508(15) 0.23402(11) 0.0678(7) Uani 1 1 d . . . F4 F -0.1149(3) 0.57783(17) 0.41284(10) 0.0844(10) Uani 1 1 d . . . F5 F -0.0527(3) 0.49936(12) 0.31050(13) 0.0672(7) Uani 1 1 d . . . F6 F -0.2285(4) 0.69352(14) 0.33375(18) 0.1010(11) 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 Au1 0.02328(5) 0.01949(4) 0.01317(5) -0.00133(3) 0.00823(3) -0.00436(3) P1 0.0177(3) 0.0159(3) 0.0118(3) -0.0009(2) 0.0052(2) -0.0024(2) C1 0.0423(16) 0.0251(12) 0.0187(13) 0.0055(10) 0.0156(11) 0.0000(11) C2 0.0261(12) 0.0239(11) 0.0094(11) 0.0033(8) 0.0071(9) -0.0011(9) C3 0.0210(11) 0.0318(13) 0.0149(12) -0.0044(9) 0.0035(9) -0.0012(10) C4 0.0315(14) 0.0293(13) 0.0148(12) -0.0047(10) 0.0027(10) 0.0013(10) C5 0.0332(14) 0.0288(13) 0.0223(14) -0.0031(10) 0.0086(11) 0.0075(11) C6 0.0241(13) 0.0340(14) 0.0260(15) -0.0001(11) 0.0089(11) 0.0029(10) C7 0.0226(12) 0.0287(13) 0.0201(13) -0.0003(10) 0.0028(10) -0.0029(10) C8 0.0227(12) 0.0279(12) 0.0163(12) -0.0024(9) 0.0052(9) -0.0107(9) C9 0.0299(14) 0.0318(14) 0.0239(14) -0.0001(11) 0.0061(11) -0.0148(11) C10 0.0222(13) 0.0437(16) 0.0291(15) 0.0034(12) -0.0051(11) -0.0078(11) C11 0.0423(16) 0.0383(15) 0.0234(15) -0.0139(12) 0.0122(12) -0.0217(13) C12 0.0197(11) 0.0196(11) 0.0203(12) 0.0018(9) 0.0053(9) 0.0039(8) C13 0.0270(13) 0.0292(13) 0.0183(13) 0.0034(10) 0.0038(10) 0.0045(10) C14 0.0361(15) 0.0222(12) 0.0338(16) 0.0013(11) 0.0139(12) 0.0076(11) C15 0.0199(12) 0.0309(14) 0.0321(15) 0.0021(11) 0.0015(10) 0.0007(10) C16 0.0155(10) 0.0182(10) 0.0131(11) 0.0000(8) 0.0036(8) 0.0009(8) C17 0.0147(10) 0.0192(10) 0.0153(11) 0.0007(8) 0.0012(8) 0.0001(8) C18 0.0238(12) 0.0199(11) 0.0236(13) 0.0004(9) 0.0047(10) 0.0020(9) C19 0.0232(12) 0.0281(13) 0.0294(15) -0.0051(10) 0.0109(10) 0.0041(10) C20 0.0235(12) 0.0284(12) 0.0205(13) -0.0021(10) 0.0119(10) 0.0004(10) C21 0.0199(11) 0.0240(11) 0.0204(13) -0.0012(9) 0.0083(9) -0.0010(9) C22 0.0235(11) 0.0151(10) 0.0192(12) -0.0010(8) 0.0068(9) -0.0013(8) C23 0.0323(14) 0.0216(11) 0.0195(13) 0.0021(9) 0.0054(10) 0.0007(10) C24 0.0529(18) 0.0181(11) 0.0245(14) 0.0034(10) 0.0151(13) 0.0002(11) C25 0.0446(17) 0.0194(12) 0.0378(17) -0.0052(11) 0.0248(14) -0.0080(11) C26 0.0259(13) 0.0259(13) 0.0415(17) -0.0053(12) 0.0141(12) -0.0055(10) C27 0.0251(12) 0.0209(11) 0.0288(14) 0.0000(10) 0.0065(10) -0.0017(9) Sb1 0.02394(8) 0.02132(8) 0.02696(10) -0.00194(6) 0.01148(7) -0.00466(6) F1 0.0349(11) 0.0783(16) 0.0869(18) 0.0262(14) 0.0017(11) -0.0244(11) F2 0.0345(10) 0.0841(16) 0.0500(13) 0.0256(11) -0.0037(9) -0.0270(10) F3 0.0529(13) 0.1073(19) 0.0406(13) 0.0380(13) -0.0079(10) -0.0185(13) F4 0.111(2) 0.123(2) 0.0218(11) -0.0126(12) 0.0213(12) -0.0807(18) F5 0.0882(17) 0.0365(11) 0.0779(17) -0.0078(11) 0.0135(14) 0.0181(11) F6 0.0823(19) 0.0399(13) 0.187(4) -0.0261(17) 0.047(2) 0.0072(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 C1 2.210(3) . ? Au1 P1 2.2996(6) . ? Au1 C2 2.365(2) . ? P1 C16 1.832(2) . ? P1 C12 1.863(2) . ? P1 C8 1.890(2) . ? C1 C2 1.369(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.499(3) . ? C2 C7 1.499(3) . ? C3 C4 1.544(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.517(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.521(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.540(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C10 1.533(4) . ? C8 C9 1.533(3) . ? C8 C11 1.548(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C14 1.532(3) . ? C12 C15 1.538(4) . ? C12 C13 1.544(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.401(3) . ? C16 C17 1.413(3) . ? C17 C18 1.395(3) . ? C17 C22 1.496(3) . ? C18 C19 1.393(3) . ? C18 H18A 0.9500 . ? C19 C20 1.384(4) . ? C19 H19A 0.9500 . ? C20 C21 1.382(3) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C23 1.391(4) . ? C22 C27 1.396(4) . ? C23 C24 1.400(4) . ? C23 H23A 0.9500 . ? C24 C25 1.384(4) . ? C24 H24A 0.9500 . ? C25 C26 1.381(4) . ? C25 H25A 0.9500 . ? C26 C27 1.392(4) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? Sb1 F5 1.843(2) . ? Sb1 F2 1.8457(18) . ? Sb1 F6 1.855(2) . ? Sb1 F4 1.858(2) . ? Sb1 F3 1.866(2) . ? Sb1 F1 1.8679(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Au1 P1 169.97(8) . . ? C1 Au1 C2 34.62(9) . . ? P1 Au1 C2 149.83(6) . . ? C16 P1 C12 107.91(11) . . ? C16 P1 C8 105.49(11) . . ? C12 P1 C8 113.92(11) . . ? C16 P1 Au1 112.64(8) . . ? C12 P1 Au1 113.15(8) . . ? C8 P1 Au1 103.53(8) . . ? C2 C1 Au1 78.88(15) . . ? C2 C1 H1A 115.4 . . ? Au1 C1 H1A 115.4 . . ? C2 C1 H1B 115.4 . . ? Au1 C1 H1B 115.4 . . ? H1A C1 H1B 112.4 . . ? C1 C2 C3 122.4(2) . . ? C1 C2 C7 122.4(2) . . ? C3 C2 C7 114.0(2) . . ? C1 C2 Au1 66.50(13) . . ? C3 C2 Au1 108.69(15) . . ? C7 C2 Au1 106.85(16) . . ? C2 C3 C4 109.1(2) . . ? C2 C3 H3A 109.9 . . ? C4 C3 H3A 109.9 . . ? C2 C3 H3B 109.9 . . ? C4 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? C5 C4 C3 110.9(2) . . ? C5 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.0 . . ? C4 C5 C6 111.0(2) . . ? C4 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? C4 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C5 C6 C7 111.4(2) . . ? C5 C6 H6A 109.3 . . ? C7 C6 H6A 109.3 . . ? C5 C6 H6B 109.3 . . ? C7 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? C2 C7 C6 109.5(2) . . ? C2 C7 H7A 109.8 . . ? C6 C7 H7A 109.8 . . ? C2 C7 H7B 109.8 . . ? C6 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? C10 C8 C9 109.8(2) . . ? C10 C8 C11 107.9(2) . . ? C9 C8 C11 107.7(2) . . ? C10 C8 P1 106.60(17) . . ? C9 C8 P1 116.04(18) . . ? C11 C8 P1 108.52(17) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C14 C12 C15 108.5(2) . . ? C14 C12 C13 110.6(2) . . ? C15 C12 C13 107.0(2) . . ? C14 C12 P1 108.76(18) . . ? C15 C12 P1 107.20(17) . . ? C13 C12 P1 114.53(16) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 118.6(2) . . ? C21 C16 P1 118.48(17) . . ? C17 C16 P1 122.26(17) . . ? C18 C17 C16 118.2(2) . . ? C18 C17 C22 116.4(2) . . ? C16 C17 C22 125.3(2) . . ? C19 C18 C17 122.0(2) . . ? C19 C18 H18A 119.0 . . ? C17 C18 H18A 119.0 . . ? C20 C19 C18 119.5(2) . . ? C20 C19 H19A 120.2 . . ? C18 C19 H19A 120.2 . . ? C21 C20 C19 119.2(2) . . ? C21 C20 H20A 120.4 . . ? C19 C20 H20A 120.4 . . ? C20 C21 C16 122.1(2) . . ? C20 C21 H21A 118.9 . . ? C16 C21 H21A 118.9 . . ? C23 C22 C27 118.5(2) . . ? C23 C22 C17 121.1(2) . . ? C27 C22 C17 120.2(2) . . ? C22 C23 C24 120.3(3) . . ? C22 C23 H23A 119.8 . . ? C24 C23 H23A 119.8 . . ? C25 C24 C23 120.6(3) . . ? C25 C24 H24A 119.7 . . ? C23 C24 H24A 119.7 . . ? C26 C25 C24 119.4(3) . . ? C26 C25 H25A 120.3 . . ? C24 C25 H25A 120.3 . . ? C25 C26 C27 120.4(3) . . ? C25 C26 H26A 119.8 . . ? C27 C26 H26A 119.8 . . ? C26 C27 C22 120.8(3) . . ? C26 C27 H27A 119.6 . . ? C22 C27 H27A 119.6 . . ? F5 Sb1 F2 90.82(11) . . ? F5 Sb1 F6 177.37(14) . . ? F2 Sb1 F6 91.06(12) . . ? F5 Sb1 F4 89.27(13) . . ? F2 Sb1 F4 89.68(9) . . ? F6 Sb1 F4 92.58(15) . . ? F5 Sb1 F3 89.94(12) . . ? F2 Sb1 F3 88.82(9) . . ? F6 Sb1 F3 88.26(15) . . ? F4 Sb1 F3 178.29(11) . . ? F5 Sb1 F1 89.18(11) . . ? F2 Sb1 F1 179.27(10) . . ? F6 Sb1 F1 88.91(12) . . ? F4 Sb1 F1 91.05(10) . . ? F3 Sb1 F1 90.45(10) . . ? 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 C1 Au1 P1 C16 61.6(4) . . . . ? C2 Au1 P1 C16 170.52(14) . . . . ? C1 Au1 P1 C12 -175.7(4) . . . . ? C2 Au1 P1 C12 -66.75(15) . . . . ? C1 Au1 P1 C8 -51.9(4) . . . . ? C2 Au1 P1 C8 57.06(15) . . . . ? P1 Au1 C1 C2 123.2(4) . . . . ? Au1 C1 C2 C3 -97.9(2) . . . . ? Au1 C1 C2 C7 95.7(2) . . . . ? P1 Au1 C2 C1 -163.14(15) . . . . ? C1 Au1 C2 C3 118.0(3) . . . . ? P1 Au1 C2 C3 -45.2(2) . . . . ? C1 Au1 C2 C7 -118.6(2) . . . . ? P1 Au1 C2 C7 78.3(2) . . . . ? C1 C2 C3 C4 -110.2(3) . . . . ? C7 C2 C3 C4 57.2(3) . . . . ? Au1 C2 C3 C4 176.29(16) . . . . ? C2 C3 C4 C5 -56.0(3) . . . . ? C3 C4 C5 C6 56.5(3) . . . . ? C4 C5 C6 C7 -55.8(3) . . . . ? C1 C2 C7 C6 110.9(3) . . . . ? C3 C2 C7 C6 -56.5(3) . . . . ? Au1 C2 C7 C6 -176.60(17) . . . . ? C5 C6 C7 C2 54.4(3) . . . . ? C16 P1 C8 C10 -41.6(2) . . . . ? C12 P1 C8 C10 -159.78(17) . . . . ? Au1 P1 C8 C10 76.92(17) . . . . ? C16 P1 C8 C9 81.0(2) . . . . ? C12 P1 C8 C9 -37.1(2) . . . . ? Au1 P1 C8 C9 -160.43(18) . . . . ? C16 P1 C8 C11 -157.63(19) . . . . ? C12 P1 C8 C11 84.2(2) . . . . ? Au1 P1 C8 C11 -39.1(2) . . . . ? C16 P1 C12 C14 -174.90(17) . . . . ? C8 P1 C12 C14 -58.1(2) . . . . ? Au1 P1 C12 C14 59.78(18) . . . . ? C16 P1 C12 C15 67.95(19) . . . . ? C8 P1 C12 C15 -175.28(16) . . . . ? Au1 P1 C12 C15 -57.37(18) . . . . ? C16 P1 C12 C13 -50.6(2) . . . . ? C8 P1 C12 C13 66.2(2) . . . . ? Au1 P1 C12 C13 -175.94(15) . . . . ? C12 P1 C16 C21 72.1(2) . . . . ? C8 P1 C16 C21 -50.0(2) . . . . ? Au1 P1 C16 C21 -162.26(17) . . . . ? C12 P1 C16 C17 -116.9(2) . . . . ? C8 P1 C16 C17 120.9(2) . . . . ? Au1 P1 C16 C17 8.7(2) . . . . ? C21 C16 C17 C18 5.2(3) . . . . ? P1 C16 C17 C18 -165.77(18) . . . . ? C21 C16 C17 C22 -171.8(2) . . . . ? P1 C16 C17 C22 17.3(3) . . . . ? C16 C17 C18 C19 -3.4(4) . . . . ? C22 C17 C18 C19 173.8(2) . . . . ? C17 C18 C19 C20 -0.9(4) . . . . ? C18 C19 C20 C21 3.3(4) . . . . ? C19 C20 C21 C16 -1.4(4) . . . . ? C17 C16 C21 C20 -2.9(4) . . . . ? P1 C16 C21 C20 168.4(2) . . . . ? C18 C17 C22 C23 66.2(3) . . . . ? C16 C17 C22 C23 -116.8(3) . . . . ? C18 C17 C22 C27 -107.7(3) . . . . ? C16 C17 C22 C27 69.3(3) . . . . ? C27 C22 C23 C24 -0.5(4) . . . . ? C17 C22 C23 C24 -174.5(2) . . . . ? C22 C23 C24 C25 -0.2(4) . . . . ? C23 C24 C25 C26 -0.2(4) . . . . ? C24 C25 C26 C27 1.3(4) . . . . ? C25 C26 C27 C22 -2.0(4) . . . . ? C23 C22 C27 C26 1.6(4) . . . . ? C17 C22 C27 C26 175.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 34.65 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 1.860 _refine_diff_density_min -1.859 _refine_diff_density_rms 0.210 #===END data_tetra _database_code_depnum_ccdc_archive 'CCDC 740536' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '((P)Au(eta2-(CH3)2C=C(CH3)2))+ SbF6-' _chemical_melting_point ? _chemical_formula_moiety 'C26 H39 Au P, F6 Sb, C H2 Cl2' _chemical_formula_sum 'C27 H41 Au Cl2 F6 P Sb' _chemical_formula_weight 900.18 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' Sb Sb -0.5866 1.5461 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' _symmetry_space_group_name_Hall '-P 2ybc' 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 9.4018(9) _cell_length_b 16.0494(16) _cell_length_c 21.377(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.985(5) _cell_angle_gamma 90.00 _cell_volume 3217.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9729 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 28.36 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.858 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 5.660 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3690 _exptl_absorpt_correction_T_max 0.5749 _exptl_absorpt_process_details 'SADABS 2.10 (Sheldrick, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 61645 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 28.59 _reflns_number_total 8078 _reflns_number_gt 7221 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex II 2.0 Rev.2 (Bruker, 2005)' _computing_cell_refinement SAINT _computing_data_reduction 'SAINT 7.12A (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material 'SHELXS-97 (Sheldrick, 1990)' _refine_special_details ; Very mild disorder may exist in the alkene portion of the main residue, C1-C6. A second orientation may exist at a low percentage and this is what leads to the elongated thermal ellipsoids. This disorder was not modeled during the solution, as data was collected at 100K. 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^)+(0.0322P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8078 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0310 _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_ref 0.0670 _refine_ls_wR_factor_gt 0.0652 _refine_ls_goodness_of_fit_ref 1.307 _refine_ls_restrained_S_all 1.307 _refine_ls_shift/su_max 0.069 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.122233(12) 0.723591(7) 0.346139(5) 0.02233(4) Uani 1 1 d . . . Sb1 Sb 0.64187(2) 0.847615(12) 0.171002(9) 0.02059(5) Uani 1 1 d . . . F1 F 0.7216(2) 0.93402(12) 0.12641(10) 0.0371(5) Uani 1 1 d . . . F2 F 0.5885(3) 0.92369(13) 0.23138(10) 0.0432(5) Uani 1 1 d . . . F3 F 0.5608(2) 0.75958(12) 0.21418(10) 0.0326(5) Uani 1 1 d . . . F4 F 0.6950(3) 0.77050(11) 0.11145(10) 0.0385(5) Uani 1 1 d . . . F5 F 0.4666(2) 0.86431(12) 0.12541(10) 0.0353(5) Uani 1 1 d . . . F6 F 0.8166(2) 0.83075(13) 0.21698(11) 0.0418(5) Uani 1 1 d . . . P1 P -0.01122(8) 0.71758(4) 0.43152(4) 0.01822(15) Uani 1 1 d . . . C1 C 0.3360(5) 0.7227(2) 0.3007(2) 0.0426(10) Uani 1 1 d . . . C2 C 0.2524(5) 0.7760(3) 0.2683(3) 0.0610(15) Uani 1 1 d . . . C3 C 0.3658(4) 0.6332(2) 0.28502(18) 0.0355(8) Uani 1 1 d . . . H3A H 0.4550 0.6297 0.2659 0.053 Uiso 1 1 calc R . . H3B H 0.2908 0.6125 0.2564 0.053 Uiso 1 1 calc R . . H3C H 0.3705 0.6005 0.3227 0.053 Uiso 1 1 calc R . . C4 C 0.4435(5) 0.7604(3) 0.3510(2) 0.0555(12) Uani 1 1 d . . . H4A H 0.5366 0.7618 0.3352 0.083 Uiso 1 1 calc R . . H4B H 0.4460 0.7268 0.3882 0.083 Uiso 1 1 calc R . . H4C H 0.4146 0.8160 0.3607 0.083 Uiso 1 1 calc R . . C5 C 0.2479(6) 0.8683(3) 0.2737(3) 0.083(2) Uani 1 1 d . . . H5A H 0.3008 0.8928 0.2416 0.125 Uiso 1 1 calc R . . H5B H 0.2892 0.8848 0.3141 0.125 Uiso 1 1 calc R . . H5C H 0.1507 0.8869 0.2689 0.125 Uiso 1 1 calc R . . C6 C 0.1767(6) 0.7526(4) 0.2047(2) 0.0672(14) Uani 1 1 d . . . H6A H 0.2296 0.7743 0.1715 0.101 Uiso 1 1 calc R . . H6B H 0.0824 0.7758 0.2016 0.101 Uiso 1 1 calc R . . H6C H 0.1708 0.6931 0.2011 0.101 Uiso 1 1 calc R . . C7 C 0.1072(3) 0.6703(2) 0.49639(14) 0.0261(7) Uani 1 1 d . . . C8 C 0.2391(4) 0.7255(2) 0.50978(19) 0.0365(8) Uani 1 1 d . . . H8A H 0.2997 0.7012 0.5429 0.055 Uiso 1 1 calc R . . H8B H 0.2098 0.7800 0.5222 0.055 Uiso 1 1 calc R . . H8C H 0.2904 0.7298 0.4726 0.055 Uiso 1 1 calc R . . C9 C 0.1563(4) 0.5854(2) 0.47006(18) 0.0391(9) Uani 1 1 d . . . H9A H 0.2179 0.5577 0.5012 0.059 Uiso 1 1 calc R . . H9B H 0.2070 0.5949 0.4332 0.059 Uiso 1 1 calc R . . H9C H 0.0745 0.5511 0.4595 0.059 Uiso 1 1 calc R . . C10 C 0.0343(4) 0.6513(2) 0.55683(16) 0.0369(8) Uani 1 1 d . . . H10A H 0.1023 0.6273 0.5872 0.055 Uiso 1 1 calc R . . H10B H -0.0425 0.6128 0.5479 0.055 Uiso 1 1 calc R . . H10C H -0.0026 0.7020 0.5732 0.055 Uiso 1 1 calc R . . C11 C -0.0709(4) 0.82755(19) 0.44696(17) 0.0292(7) Uani 1 1 d . . . C12 C 0.0496(4) 0.8882(2) 0.43243(19) 0.0361(8) Uani 1 1 d . . . H12A H 0.0202 0.9443 0.4401 0.054 Uiso 1 1 calc R . . H12B H 0.0702 0.8825 0.3893 0.054 Uiso 1 1 calc R . . H12C H 0.1336 0.8755 0.4589 0.054 Uiso 1 1 calc R . . C13 C -0.1033(5) 0.8456(2) 0.5160(2) 0.0487(12) Uani 1 1 d . . . H13A H -0.1331 0.9025 0.5198 0.073 Uiso 1 1 calc R . . H13B H -0.0190 0.8362 0.5431 0.073 Uiso 1 1 calc R . . H13C H -0.1780 0.8093 0.5279 0.073 Uiso 1 1 calc R . . C14 C -0.1995(5) 0.8433(2) 0.4029(2) 0.0515(11) Uani 1 1 d . . . H14A H -0.2340 0.8988 0.4092 0.077 Uiso 1 1 calc R . . H14B H -0.2728 0.8039 0.4110 0.077 Uiso 1 1 calc R . . H14C H -0.1740 0.8374 0.3604 0.077 Uiso 1 1 calc R . . C15 C -0.1701(3) 0.65160(17) 0.42505(14) 0.0193(6) Uani 1 1 d . . . C16 C -0.2032(3) 0.59762(17) 0.37433(14) 0.0186(6) Uani 1 1 d . . . C17 C -0.3253(3) 0.54825(19) 0.37558(15) 0.0241(6) Uani 1 1 d . . . H17A H -0.3472 0.5118 0.3425 0.029 Uiso 1 1 calc R . . C18 C -0.4147(3) 0.55161(19) 0.42408(15) 0.0260(7) Uani 1 1 d . . . H18A H -0.4953 0.5179 0.4235 0.031 Uiso 1 1 calc R . . C19 C -0.3834(3) 0.60551(18) 0.47345(14) 0.0229(6) Uani 1 1 d . . . H19A H -0.4436 0.6090 0.5061 0.027 Uiso 1 1 calc R . . C20 C -0.2620(3) 0.65437(18) 0.47408(15) 0.0228(6) Uani 1 1 d . . . H20A H -0.2407 0.6899 0.5078 0.027 Uiso 1 1 calc R . . C21 C -0.1243(3) 0.59064(18) 0.31590(13) 0.0190(6) Uani 1 1 d . . . C22 C -0.0145(3) 0.53262(19) 0.31058(15) 0.0256(6) Uani 1 1 d . . . H22A H 0.0215 0.5032 0.3457 0.031 Uiso 1 1 calc R . . C23 C 0.0406(4) 0.5191(2) 0.25254(16) 0.0289(7) Uani 1 1 d . . . H23A H 0.1127 0.4802 0.2489 0.035 Uiso 1 1 calc R . . C24 C -0.0115(4) 0.5634(2) 0.20051(15) 0.0304(7) Uani 1 1 d . . . H24A H 0.0252 0.5541 0.1618 0.036 Uiso 1 1 calc R . . C25 C -0.1171(4) 0.6211(3) 0.20601(16) 0.0368(8) Uani 1 1 d . . . H25A H -0.1514 0.6512 0.1710 0.044 Uiso 1 1 calc R . . C26 C -0.1738(4) 0.6349(2) 0.26344(16) 0.0315(7) Uani 1 1 d . . . H26A H -0.2455 0.6743 0.2666 0.038 Uiso 1 1 calc R . . Cl1 Cl 0.33441(15) 0.57878(8) 0.10644(8) 0.0722(4) Uani 1 1 d . . . Cl2 Cl 0.60827(17) 0.50753(10) 0.08217(7) 0.0813(4) Uani 1 1 d . . . C1X C 0.5091(5) 0.5582(3) 0.1368(3) 0.0673(14) Uani 1 1 d . . . H1XA H 0.5556 0.6102 0.1490 0.081 Uiso 1 1 calc R . . H1XB H 0.5060 0.5238 0.1740 0.081 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 Au1 0.02017(7) 0.02967(7) 0.01786(7) 0.00309(4) 0.00637(4) -0.00054(4) Sb1 0.02071(10) 0.02107(10) 0.02055(10) 0.00322(7) 0.00541(8) 0.00011(7) F1 0.0354(11) 0.0328(10) 0.0439(12) 0.0137(9) 0.0095(10) -0.0055(9) F2 0.0564(14) 0.0377(11) 0.0369(12) -0.0085(9) 0.0133(11) 0.0049(10) F3 0.0325(11) 0.0297(9) 0.0372(12) 0.0138(9) 0.0144(9) -0.0018(8) F4 0.0549(14) 0.0326(11) 0.0308(12) -0.0008(8) 0.0221(10) 0.0052(9) F5 0.0281(10) 0.0326(10) 0.0441(12) 0.0082(9) -0.0058(9) -0.0005(8) F6 0.0304(11) 0.0379(11) 0.0551(14) 0.0118(10) -0.0116(10) -0.0019(9) P1 0.0174(4) 0.0208(4) 0.0169(4) -0.0001(3) 0.0039(3) -0.0028(3) C1 0.038(2) 0.052(2) 0.041(2) 0.0121(18) 0.0213(18) 0.0039(17) C2 0.048(3) 0.072(3) 0.068(3) 0.031(2) 0.045(3) 0.020(2) C3 0.0312(19) 0.0340(18) 0.043(2) -0.0003(16) 0.0129(16) 0.0001(14) C4 0.039(2) 0.085(3) 0.044(3) -0.014(2) 0.016(2) -0.024(2) C5 0.081(4) 0.064(3) 0.113(5) 0.057(3) 0.072(4) 0.039(3) C6 0.052(3) 0.105(4) 0.045(3) 0.019(3) 0.004(2) -0.007(3) C7 0.0235(16) 0.0387(17) 0.0160(14) 0.0036(13) 0.0015(12) -0.0014(13) C8 0.0293(19) 0.047(2) 0.032(2) 0.0003(15) -0.0057(15) -0.0035(15) C9 0.043(2) 0.0370(19) 0.037(2) 0.0075(16) 0.0000(17) 0.0094(16) C10 0.037(2) 0.051(2) 0.0231(17) 0.0093(16) 0.0036(15) -0.0013(16) C11 0.0303(17) 0.0162(13) 0.043(2) -0.0006(13) 0.0139(15) -0.0020(12) C12 0.041(2) 0.0237(16) 0.045(2) 0.0011(15) 0.0094(17) -0.0109(14) C13 0.067(3) 0.0310(19) 0.053(3) -0.0083(17) 0.037(2) -0.0079(18) C14 0.041(2) 0.0304(19) 0.081(3) 0.005(2) -0.007(2) 0.0050(17) C15 0.0186(14) 0.0211(13) 0.0186(14) 0.0025(11) 0.0034(11) -0.0031(11) C16 0.0189(14) 0.0185(13) 0.0187(14) 0.0038(11) 0.0023(11) 0.0031(11) C17 0.0258(16) 0.0236(14) 0.0229(15) -0.0005(12) 0.0022(12) -0.0027(12) C18 0.0218(15) 0.0297(16) 0.0271(17) 0.0017(13) 0.0059(13) -0.0074(12) C19 0.0213(15) 0.0254(15) 0.0227(15) 0.0040(12) 0.0074(12) -0.0025(12) C20 0.0239(15) 0.0247(15) 0.0201(15) -0.0013(12) 0.0045(12) -0.0043(12) C21 0.0177(14) 0.0225(14) 0.0170(14) -0.0004(11) 0.0019(11) -0.0027(11) C22 0.0299(17) 0.0239(14) 0.0237(16) 0.0033(12) 0.0065(13) 0.0047(12) C23 0.0311(17) 0.0268(16) 0.0300(18) -0.0047(13) 0.0100(14) 0.0028(13) C24 0.0361(19) 0.0362(17) 0.0196(16) -0.0041(13) 0.0077(14) -0.0026(15) C25 0.039(2) 0.054(2) 0.0179(16) 0.0090(15) 0.0051(14) 0.0106(17) C26 0.0293(18) 0.0407(18) 0.0254(17) 0.0091(14) 0.0083(14) 0.0127(14) Cl1 0.0617(8) 0.0582(7) 0.0967(11) 0.0119(7) 0.0070(7) 0.0137(6) Cl2 0.0820(10) 0.0888(10) 0.0773(10) -0.0006(8) 0.0359(8) 0.0166(8) C1X 0.059(3) 0.072(3) 0.072(4) -0.017(3) 0.009(3) 0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.2876(8) . ? Au1 C2 2.293(4) . ? Au1 C1 2.292(4) . ? Sb1 F4 1.8682(19) . ? Sb1 F2 1.870(2) . ? Sb1 F1 1.8691(18) . ? Sb1 F6 1.875(2) . ? Sb1 F5 1.874(2) . ? Sb1 F3 1.8780(18) . ? P1 C15 1.829(3) . ? P1 C7 1.877(3) . ? P1 C11 1.888(3) . ? C1 C2 1.325(6) . ? C1 C3 1.505(5) . ? C1 C4 1.546(6) . ? C2 C5 1.486(7) . ? C2 C6 1.537(8) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.535(5) . ? C7 C10 1.535(4) . ? C7 C9 1.557(5) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C14 1.502(6) . ? C11 C12 1.541(4) . ? C11 C13 1.556(5) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.406(4) . ? C15 C20 1.404(4) . ? C16 C17 1.397(4) . ? C16 C21 1.501(4) . ? C17 C18 1.381(4) . ? C17 H17A 0.9300 . ? C18 C19 1.381(4) . ? C18 H18A 0.9300 . ? C19 C20 1.384(4) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C26 1.381(4) . ? C21 C22 1.401(4) . ? C22 C23 1.394(4) . ? C22 H22A 0.9300 . ? C23 C24 1.381(5) . ? C23 H23A 0.9300 . ? C24 C25 1.368(5) . ? C24 H24A 0.9300 . ? C25 C26 1.390(4) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? Cl1 C1X 1.755(5) . ? Cl2 C1X 1.745(5) . ? C1X H1XA 0.9700 . ? C1X H1XB 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 P1 Au1 C2 160.82(13) . . ? P1 Au1 C1 152.05(12) . . ? C2 Au1 C1 33.60(16) . . ? F4 Sb1 F2 179.26(9) . . ? F4 Sb1 F1 90.47(9) . . ? F2 Sb1 F1 90.22(10) . . ? F4 Sb1 F6 89.74(11) . . ? F2 Sb1 F6 89.98(10) . . ? F1 Sb1 F6 90.37(9) . . ? F4 Sb1 F5 90.43(10) . . ? F2 Sb1 F5 89.85(10) . . ? F1 Sb1 F5 89.89(9) . . ? F6 Sb1 F5 179.69(10) . . ? F4 Sb1 F3 88.47(9) . . ? F2 Sb1 F3 90.84(9) . . ? F1 Sb1 F3 178.77(10) . . ? F6 Sb1 F3 90.25(9) . . ? F5 Sb1 F3 89.49(9) . . ? C15 P1 C7 105.14(14) . . ? C15 P1 C11 107.67(14) . . ? C7 P1 C11 114.64(16) . . ? C15 P1 Au1 117.04(10) . . ? C7 P1 Au1 106.05(10) . . ? C11 P1 Au1 106.63(10) . . ? C2 C1 C3 127.7(5) . . ? C2 C1 C4 116.5(4) . . ? C3 C1 C4 113.9(4) . . ? C2 C1 Au1 73.2(2) . . ? C3 C1 Au1 106.4(2) . . ? C4 C1 Au1 104.7(3) . . ? C1 C2 C5 128.4(6) . . ? C1 C2 C6 121.8(5) . . ? C5 C2 C6 107.4(5) . . ? C1 C2 Au1 73.2(2) . . ? C5 C2 Au1 106.8(3) . . ? C6 C2 Au1 108.4(3) . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C10 111.1(3) . . ? C8 C7 C9 108.4(3) . . ? C10 C7 C9 107.0(3) . . ? C8 C7 P1 109.6(2) . . ? C10 C7 P1 115.2(2) . . ? C9 C7 P1 105.2(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C14 C11 C12 109.8(3) . . ? C14 C11 C13 111.2(3) . . ? C12 C11 C13 105.6(3) . . ? C14 C11 P1 106.5(2) . . ? C12 C11 P1 108.9(2) . . ? C13 C11 P1 114.9(2) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C20 118.7(3) . . ? C16 C15 P1 123.4(2) . . ? C20 C15 P1 117.8(2) . . ? C17 C16 C15 118.2(3) . . ? C17 C16 C21 115.3(3) . . ? C15 C16 C21 126.3(3) . . ? C18 C17 C16 122.5(3) . . ? C18 C17 H17A 118.8 . . ? C16 C17 H17A 118.8 . . ? C19 C18 C17 119.3(3) . . ? C19 C18 H18A 120.3 . . ? C17 C18 H18A 120.3 . . ? C18 C19 C20 119.6(3) . . ? C18 C19 H19A 120.2 . . ? C20 C19 H19A 120.2 . . ? C19 C20 C15 121.6(3) . . ? C19 C20 H20A 119.2 . . ? C15 C20 H20A 119.2 . . ? C26 C21 C22 119.0(3) . . ? C26 C21 C16 118.7(3) . . ? C22 C21 C16 121.8(3) . . ? C23 C22 C21 119.8(3) . . ? C23 C22 H22A 120.1 . . ? C21 C22 H22A 120.1 . . ? C24 C23 C22 120.3(3) . . ? C24 C23 H23A 119.9 . . ? C22 C23 H23A 119.9 . . ? C25 C24 C23 119.8(3) . . ? C25 C24 H24A 120.1 . . ? C23 C24 H24A 120.1 . . ? C24 C25 C26 120.6(3) . . ? C24 C25 H25A 119.7 . . ? C26 C25 H25A 119.7 . . ? C21 C26 C25 120.4(3) . . ? C21 C26 H26A 119.8 . . ? C25 C26 H26A 119.8 . . ? Cl2 C1X Cl1 111.7(3) . . ? Cl2 C1X H1XA 109.3 . . ? Cl1 C1X H1XA 109.3 . . ? Cl2 C1X H1XB 109.3 . . ? Cl1 C1X H1XB 109.3 . . ? H1XA C1X H1XB 107.9 . . ? 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 C2 Au1 P1 C15 133.8(5) . . . . ? C1 Au1 P1 C15 -135.7(2) . . . . ? C2 Au1 P1 C7 -109.3(5) . . . . ? C1 Au1 P1 C7 -18.8(2) . . . . ? C2 Au1 P1 C11 13.3(5) . . . . ? C1 Au1 P1 C11 103.8(2) . . . . ? P1 Au1 C1 C2 -143.6(3) . . . . ? P1 Au1 C1 C3 91.2(4) . . . . ? C2 Au1 C1 C3 -125.3(5) . . . . ? P1 Au1 C1 C4 -29.8(4) . . . . ? C2 Au1 C1 C4 113.8(5) . . . . ? C3 C1 C2 C5 -163.5(4) . . . . ? C4 C1 C2 C5 0.0(6) . . . . ? Au1 C1 C2 C5 98.4(4) . . . . ? C3 C1 C2 C6 -3.5(6) . . . . ? C4 C1 C2 C6 160.1(4) . . . . ? Au1 C1 C2 C6 -101.5(4) . . . . ? C3 C1 C2 Au1 98.1(4) . . . . ? C4 C1 C2 Au1 -98.4(3) . . . . ? P1 Au1 C2 C1 122.1(4) . . . . ? P1 Au1 C2 C5 -3.8(8) . . . . ? C1 Au1 C2 C5 -125.9(6) . . . . ? P1 Au1 C2 C6 -119.2(5) . . . . ? C1 Au1 C2 C6 118.7(5) . . . . ? C15 P1 C7 C8 -175.1(2) . . . . ? C11 P1 C7 C8 -57.1(3) . . . . ? Au1 P1 C7 C8 60.3(2) . . . . ? C15 P1 C7 C10 -49.0(3) . . . . ? C11 P1 C7 C10 69.0(3) . . . . ? Au1 P1 C7 C10 -173.6(2) . . . . ? C15 P1 C7 C9 68.5(2) . . . . ? C11 P1 C7 C9 -173.5(2) . . . . ? Au1 P1 C7 C9 -56.1(2) . . . . ? C15 P1 C11 C14 -44.3(3) . . . . ? C7 P1 C11 C14 -160.9(3) . . . . ? Au1 P1 C11 C14 82.1(3) . . . . ? C15 P1 C11 C12 -162.6(2) . . . . ? C7 P1 C11 C12 80.8(3) . . . . ? Au1 P1 C11 C12 -36.2(3) . . . . ? C15 P1 C11 C13 79.3(3) . . . . ? C7 P1 C11 C13 -37.3(3) . . . . ? Au1 P1 C11 C13 -154.4(3) . . . . ? C7 P1 C15 C16 -109.2(3) . . . . ? C11 P1 C15 C16 128.2(3) . . . . ? Au1 P1 C15 C16 8.2(3) . . . . ? C7 P1 C15 C20 69.7(3) . . . . ? C11 P1 C15 C20 -53.0(3) . . . . ? Au1 P1 C15 C20 -173.0(2) . . . . ? C20 C15 C16 C17 -0.9(4) . . . . ? P1 C15 C16 C17 178.0(2) . . . . ? C20 C15 C16 C21 175.3(3) . . . . ? P1 C15 C16 C21 -5.9(4) . . . . ? C15 C16 C17 C18 0.9(5) . . . . ? C21 C16 C17 C18 -175.6(3) . . . . ? C16 C17 C18 C19 0.0(5) . . . . ? C17 C18 C19 C20 -1.0(5) . . . . ? C18 C19 C20 C15 1.0(5) . . . . ? C16 C15 C20 C19 -0.1(4) . . . . ? P1 C15 C20 C19 -179.0(2) . . . . ? C17 C16 C21 C26 80.7(4) . . . . ? C15 C16 C21 C26 -95.6(4) . . . . ? C17 C16 C21 C22 -90.8(4) . . . . ? C15 C16 C21 C22 93.0(4) . . . . ? C26 C21 C22 C23 -1.5(5) . . . . ? C16 C21 C22 C23 169.9(3) . . . . ? C21 C22 C23 C24 0.8(5) . . . . ? C22 C23 C24 C25 0.3(5) . . . . ? C23 C24 C25 C26 -0.6(6) . . . . ? C22 C21 C26 C25 1.1(5) . . . . ? C16 C21 C26 C25 -170.6(3) . . . . ? C24 C25 C26 C21 -0.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 28.59 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.708 _refine_diff_density_min -0.862 _refine_diff_density_rms 0.114 #===END data_o1 _database_code_depnum_ccdc_archive 'CCDC 740537' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '((P)Au(eta2-H2=CH-4-C6H4Me))+ SbF6-' _chemical_melting_point ? _chemical_formula_moiety 'C29 H37 Au P, F6 Sb' _chemical_formula_sum 'C29 H37 Au F6 P Sb' _chemical_formula_weight 849.27 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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pbca ' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.702(4) _cell_length_b 18.693(6) _cell_length_c 25.481(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6050(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8609 _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 26.62 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.865 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3280 _exptl_absorpt_coefficient_mu 5.844 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2915 _exptl_absorpt_correction_T_max 0.6851 _exptl_absorpt_process_details 'SADABS 2.10 (Sheldrick, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 104499 _diffrn_reflns_av_R_equivalents 0.0826 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.20 _reflns_number_total 6695 _reflns_number_gt 5501 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex II 2.0 Rev.2 (Bruker, 2005)' _computing_cell_refinement SAINT _computing_data_reduction 'SAINT 7.12A (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material 'SHELXS-97 (Sheldrick, 1990)' _refine_special_details ; The short C1-C2 distance is expected, as it is based on the alkene bonding into the Au atom, leading to an unusual bond length. Additional disorder is to be expected due to the presence of the antimonate anion and terminal t-butyl groups. This disorder was minimized by collecting the data at 100K. SADABS was used to refine the data. 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^)+(0.0212P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6695 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0683 _refine_ls_wR_factor_gt 0.0649 _refine_ls_goodness_of_fit_ref 1.426 _refine_ls_restrained_S_all 1.426 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.717864(12) 0.195883(8) 0.649246(6) 0.02237(6) Uani 1 1 d . . . Sb1 Sb 0.16784(2) 0.077853(16) 0.662069(10) 0.02674(8) Uani 1 1 d . . . F1 F 0.0806(3) 0.1136(2) 0.71364(12) 0.0879(13) Uani 1 1 d . . . F2 F 0.0520(2) 0.06484(16) 0.61878(11) 0.0474(7) Uani 1 1 d . . . F3 F 0.1801(4) 0.1720(2) 0.63669(18) 0.1034(16) Uani 1 1 d . . . F4 F 0.2562(3) 0.0500(3) 0.61026(14) 0.145(3) Uani 1 1 d . . . F5 F 0.2829(2) 0.0922(2) 0.70668(13) 0.0747(12) Uani 1 1 d . . . F6 F 0.1545(4) -0.01149(18) 0.69020(17) 0.0990(15) Uani 1 1 d . . . P1 P 0.61774(8) 0.29752(5) 0.64980(4) 0.0174(2) Uani 1 1 d . . . C1 C 0.8153(4) 0.0988(2) 0.6531(2) 0.0453(14) Uani 1 1 d . . . H1A H 0.8384 0.0798 0.6196 0.054 Uiso 1 1 calc R . . H1B H 0.8711 0.0994 0.6791 0.054 Uiso 1 1 calc R . . C2 C 0.7231(4) 0.0757(2) 0.6698(2) 0.0420(12) Uani 1 1 d . . . H2A H 0.7207 0.0658 0.7076 0.050 Uiso 1 1 calc R . . C3 C 0.6429(4) 0.0391(2) 0.63991(19) 0.0378(12) Uani 1 1 d . . . C4 C 0.5494(4) 0.0168(3) 0.66569(18) 0.0413(13) Uani 1 1 d . . . H4A H 0.5393 0.0288 0.7008 0.050 Uiso 1 1 calc R . . C5 C 0.4749(4) -0.0215(3) 0.6402(2) 0.0457(13) Uani 1 1 d . . . H5A H 0.4145 -0.0348 0.6584 0.055 Uiso 1 1 calc R . . C6 C 0.4850(4) -0.0411(3) 0.5893(2) 0.0423(12) Uani 1 1 d . . . C7 C 0.5753(4) -0.0204(3) 0.56361(19) 0.0396(12) Uani 1 1 d . . . H7A H 0.5842 -0.0341 0.5288 0.047 Uiso 1 1 calc R . . C8 C 0.6528(3) 0.0197(2) 0.58696(18) 0.0344(11) Uani 1 1 d . . . H8A H 0.7114 0.0339 0.5678 0.041 Uiso 1 1 calc R . . C9 C 0.4020(5) -0.0849(3) 0.5628(3) 0.0716(19) Uani 1 1 d . . . H9A H 0.4220 -0.0934 0.5270 0.107 Uiso 1 1 calc R . . H9B H 0.3362 -0.0596 0.5636 0.107 Uiso 1 1 calc R . . H9C H 0.3944 -0.1298 0.5807 0.107 Uiso 1 1 calc R . . C10 C 0.4774(3) 0.2664(2) 0.64670(15) 0.0231(9) Uani 1 1 d . . . C11 C 0.4714(3) 0.2174(2) 0.59860(17) 0.0311(10) Uani 1 1 d . . . H11A H 0.4009 0.1996 0.5948 0.047 Uiso 1 1 calc R . . H11B H 0.5190 0.1779 0.6031 0.047 Uiso 1 1 calc R . . H11C H 0.4906 0.2438 0.5678 0.047 Uiso 1 1 calc R . . C12 C 0.3945(3) 0.3250(2) 0.64002(17) 0.0313(10) Uani 1 1 d . . . H12A H 0.3257 0.3038 0.6390 0.047 Uiso 1 1 calc R . . H12B H 0.4072 0.3504 0.6079 0.047 Uiso 1 1 calc R . . H12C H 0.3986 0.3577 0.6690 0.047 Uiso 1 1 calc R . . C13 C 0.4521(4) 0.2231(2) 0.69608(17) 0.0347(11) Uani 1 1 d . . . H13A H 0.3803 0.2073 0.6947 0.052 Uiso 1 1 calc R . . H13B H 0.4623 0.2526 0.7265 0.052 Uiso 1 1 calc R . . H13C H 0.4980 0.1824 0.6980 0.052 Uiso 1 1 calc R . . C14 C 0.6561(3) 0.3508(2) 0.70924(15) 0.0264(9) Uani 1 1 d . . . C15 C 0.7710(4) 0.3717(3) 0.69966(17) 0.0383(12) Uani 1 1 d . . . H15A H 0.7961 0.3997 0.7287 0.057 Uiso 1 1 calc R . . H15B H 0.7759 0.3993 0.6680 0.057 Uiso 1 1 calc R . . H15C H 0.8130 0.3293 0.6963 0.057 Uiso 1 1 calc R . . C16 C 0.5911(5) 0.4178(3) 0.71935(19) 0.0508(15) Uani 1 1 d . . . H16A H 0.6168 0.4415 0.7502 0.076 Uiso 1 1 calc R . . H16B H 0.5187 0.4047 0.7244 0.076 Uiso 1 1 calc R . . H16C H 0.5966 0.4494 0.6898 0.076 Uiso 1 1 calc R . . C17 C 0.6536(4) 0.3023(2) 0.75817(16) 0.0410(12) Uani 1 1 d . . . H17A H 0.6733 0.3296 0.7885 0.061 Uiso 1 1 calc R . . H17B H 0.7022 0.2635 0.7536 0.061 Uiso 1 1 calc R . . H17C H 0.5839 0.2837 0.7629 0.061 Uiso 1 1 calc R . . C18 C 0.6374(3) 0.3556(2) 0.59322(14) 0.0167(8) Uani 1 1 d . . . C19 C 0.7056(3) 0.3383(2) 0.55159(15) 0.0185(8) Uani 1 1 d . . . C20 C 0.7094(3) 0.3836(2) 0.50819(15) 0.0208(8) Uani 1 1 d . . . H20A H 0.7529 0.3715 0.4802 0.025 Uiso 1 1 calc R . . C21 C 0.6518(3) 0.44507(19) 0.50533(15) 0.0193(8) Uani 1 1 d . . . H21A H 0.6565 0.4744 0.4759 0.023 Uiso 1 1 calc R . . C22 C 0.5859(3) 0.4635(2) 0.54676(14) 0.0198(8) Uani 1 1 d . . . H22A H 0.5469 0.5056 0.5455 0.024 Uiso 1 1 calc R . . C23 C 0.5788(3) 0.4189(2) 0.58975(14) 0.0180(8) Uani 1 1 d . . . H23A H 0.5341 0.4312 0.6172 0.022 Uiso 1 1 calc R . . C24 C 0.7796(3) 0.2761(2) 0.55002(15) 0.0215(8) Uani 1 1 d . . . C25 C 0.7601(4) 0.2187(2) 0.51658(17) 0.0294(10) Uani 1 1 d . . . H25A H 0.6960 0.2156 0.4991 0.035 Uiso 1 1 calc R . . C26 C 0.8358(4) 0.1659(2) 0.50921(18) 0.0376(12) Uani 1 1 d . . . H26A H 0.8225 0.1277 0.4868 0.045 Uiso 1 1 calc R . . C27 C 0.9300(4) 0.1704(2) 0.5350(2) 0.0421(13) Uani 1 1 d . . . H27A H 0.9809 0.1355 0.5295 0.051 Uiso 1 1 calc R . . C28 C 0.9505(4) 0.2260(2) 0.5691(2) 0.0409(13) Uani 1 1 d . . . H28A H 1.0144 0.2282 0.5868 0.049 Uiso 1 1 calc R . . C29 C 0.8747(3) 0.2790(2) 0.57681(18) 0.0297(10) Uani 1 1 d . . . H29A H 0.8878 0.3164 0.6000 0.036 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 Au1 0.02212(9) 0.01807(9) 0.02692(9) 0.00651(6) 0.00294(6) 0.00498(6) Sb1 0.02121(14) 0.03934(18) 0.01966(14) 0.00337(12) -0.00120(11) -0.00572(13) F1 0.097(3) 0.132(4) 0.0352(17) -0.0302(19) -0.0077(18) 0.055(3) F2 0.0361(15) 0.065(2) 0.0414(16) -0.0128(14) -0.0162(12) -0.0036(14) F3 0.107(3) 0.083(3) 0.120(4) 0.060(3) -0.056(3) -0.052(3) F4 0.084(3) 0.323(8) 0.029(2) -0.004(3) 0.0004(18) 0.129(4) F5 0.0453(19) 0.127(3) 0.052(2) 0.031(2) -0.0260(15) -0.036(2) F6 0.142(4) 0.035(2) 0.120(3) 0.027(2) -0.066(3) -0.033(2) P1 0.0188(5) 0.0151(5) 0.0184(5) 0.0015(4) 0.0009(4) 0.0017(4) C1 0.039(3) 0.020(2) 0.077(4) 0.023(2) 0.019(3) 0.017(2) C2 0.048(3) 0.024(2) 0.054(3) 0.012(2) -0.001(2) 0.013(2) C3 0.048(3) 0.017(2) 0.048(3) -0.002(2) -0.020(2) 0.011(2) C4 0.057(3) 0.041(3) 0.026(2) 0.008(2) 0.011(2) 0.025(3) C5 0.038(3) 0.045(3) 0.055(3) 0.015(3) 0.002(2) 0.001(2) C6 0.040(3) 0.030(3) 0.056(3) 0.003(2) -0.004(2) 0.009(2) C7 0.041(3) 0.038(3) 0.039(3) -0.009(2) 0.003(2) 0.008(2) C8 0.025(2) 0.035(3) 0.044(3) 0.008(2) 0.005(2) 0.009(2) C9 0.057(4) 0.052(4) 0.106(5) 0.002(4) -0.026(4) -0.006(3) C10 0.019(2) 0.021(2) 0.029(2) 0.0024(17) 0.0035(16) -0.0007(16) C11 0.025(2) 0.028(2) 0.040(3) 0.000(2) -0.0073(19) -0.0020(19) C12 0.021(2) 0.033(2) 0.040(3) 0.002(2) 0.0040(19) 0.0033(19) C13 0.028(2) 0.040(3) 0.037(3) 0.011(2) 0.004(2) -0.008(2) C14 0.038(3) 0.023(2) 0.018(2) 0.0021(16) -0.0043(17) -0.0021(19) C15 0.048(3) 0.038(3) 0.029(2) 0.002(2) -0.012(2) -0.020(2) C16 0.077(4) 0.045(3) 0.031(3) -0.018(2) -0.017(3) 0.019(3) C17 0.059(3) 0.044(3) 0.019(2) 0.006(2) -0.010(2) -0.012(3) C18 0.0179(19) 0.0165(19) 0.0157(18) 0.0010(15) -0.0031(14) -0.0038(15) C19 0.022(2) 0.0133(18) 0.0205(19) -0.0020(15) -0.0021(15) -0.0014(16) C20 0.0200(19) 0.022(2) 0.021(2) -0.0006(16) -0.0001(16) -0.0031(16) C21 0.023(2) 0.017(2) 0.0174(19) 0.0036(15) -0.0034(15) -0.0034(16) C22 0.0198(19) 0.0156(19) 0.024(2) 0.0003(16) -0.0067(15) 0.0018(16) C23 0.0157(18) 0.021(2) 0.0177(18) -0.0025(16) -0.0016(14) 0.0028(16) C24 0.021(2) 0.0172(19) 0.026(2) 0.0072(16) 0.0117(17) 0.0034(17) C25 0.035(2) 0.024(2) 0.029(2) -0.0016(18) 0.0110(19) 0.0038(19) C26 0.053(3) 0.022(2) 0.038(3) -0.002(2) 0.024(2) 0.008(2) C27 0.042(3) 0.024(2) 0.061(3) 0.018(2) 0.035(3) 0.015(2) C28 0.024(2) 0.030(3) 0.069(3) 0.023(2) 0.014(2) 0.010(2) C29 0.023(2) 0.022(2) 0.044(3) 0.009(2) 0.0037(19) 0.0038(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 C1 2.199(4) . ? Au1 P1 2.2863(11) . ? Au1 C2 2.308(5) . ? Sb1 F4 1.809(3) . ? Sb1 F6 1.825(3) . ? Sb1 F1 1.844(3) . ? Sb1 F2 1.855(2) . ? Sb1 F5 1.871(3) . ? Sb1 F3 1.882(4) . ? P1 C18 1.822(4) . ? P1 C10 1.877(4) . ? P1 C14 1.877(4) . ? C1 C2 1.319(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.445(7) . ? C2 H2A 0.9800 . ? C3 C8 1.403(6) . ? C3 C4 1.419(7) . ? C4 C5 1.352(7) . ? C4 H4A 0.9300 . ? C5 C6 1.354(7) . ? C5 H5A 0.9300 . ? C6 C7 1.377(7) . ? C6 C9 1.497(7) . ? C7 C8 1.372(6) . ? C7 H7A 0.9300 . ? C8 H8A 0.9300 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C12 1.529(6) . ? C10 C13 1.530(5) . ? C10 C11 1.533(6) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C16 1.522(6) . ? C14 C15 1.530(6) . ? C14 C17 1.542(5) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C23 1.401(5) . ? C18 C19 1.407(5) . ? C19 C20 1.393(5) . ? C19 C24 1.497(5) . ? C20 C21 1.365(5) . ? C20 H20A 0.9300 . ? C21 C22 1.391(5) . ? C21 H21A 0.9300 . ? C22 C23 1.380(5) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C24 C29 1.388(6) . ? C24 C25 1.392(6) . ? C25 C26 1.390(6) . ? C25 H25A 0.9300 . ? C26 C27 1.367(7) . ? C26 H26A 0.9300 . ? C27 C28 1.379(7) . ? C27 H27A 0.9300 . ? C28 C29 1.395(6) . ? C28 H28A 0.9300 . ? C29 H29A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Au1 P1 177.02(16) . . ? C1 Au1 C2 33.92(17) . . ? P1 Au1 C2 145.44(13) . . ? F4 Sb1 F6 94.6(3) . . ? F4 Sb1 F1 175.5(2) . . ? F6 Sb1 F1 89.7(2) . . ? F4 Sb1 F2 91.19(16) . . ? F6 Sb1 F2 92.28(15) . . ? F1 Sb1 F2 89.68(15) . . ? F4 Sb1 F5 89.99(19) . . ? F6 Sb1 F5 88.02(16) . . ? F1 Sb1 F5 89.11(17) . . ? F2 Sb1 F5 178.76(16) . . ? F4 Sb1 F3 88.1(3) . . ? F6 Sb1 F3 176.9(2) . . ? F1 Sb1 F3 87.5(2) . . ? F2 Sb1 F3 89.09(15) . . ? F5 Sb1 F3 90.56(17) . . ? C18 P1 C10 106.33(17) . . ? C18 P1 C14 106.68(18) . . ? C10 P1 C14 116.41(19) . . ? C18 P1 Au1 114.46(13) . . ? C10 P1 Au1 105.71(13) . . ? C14 P1 Au1 107.54(14) . . ? C2 C1 Au1 77.6(3) . . ? C2 C1 H1A 115.6 . . ? Au1 C1 H1A 115.6 . . ? C2 C1 H1B 115.6 . . ? Au1 C1 H1B 115.6 . . ? H1A C1 H1B 112.6 . . ? C1 C2 C3 127.7(5) . . ? C1 C2 Au1 68.5(3) . . ? C3 C2 Au1 108.7(3) . . ? C1 C2 H2A 114.0 . . ? C3 C2 H2A 114.0 . . ? Au1 C2 H2A 114.0 . . ? C8 C3 C4 116.4(4) . . ? C8 C3 C2 124.6(5) . . ? C4 C3 C2 119.0(5) . . ? C5 C4 C3 121.2(4) . . ? C5 C4 H4A 119.4 . . ? C3 C4 H4A 119.4 . . ? C4 C5 C6 122.5(5) . . ? C4 C5 H5A 118.8 . . ? C6 C5 H5A 118.8 . . ? C5 C6 C7 117.3(5) . . ? C5 C6 C9 121.0(5) . . ? C7 C6 C9 121.7(5) . . ? C8 C7 C6 123.0(5) . . ? C8 C7 H7A 118.5 . . ? C6 C7 H7A 118.5 . . ? C7 C8 C3 119.6(4) . . ? C7 C8 H8A 120.2 . . ? C3 C8 H8A 120.2 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C13 109.0(3) . . ? C12 C10 C11 107.8(3) . . ? C13 C10 C11 109.3(4) . . ? C12 C10 P1 115.9(3) . . ? C13 C10 P1 109.2(3) . . ? C11 C10 P1 105.4(3) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C16 C14 C15 109.5(4) . . ? C16 C14 C17 109.6(4) . . ? C15 C14 C17 107.4(4) . . ? C16 C14 P1 115.6(3) . . ? C15 C14 P1 104.7(3) . . ? C17 C14 P1 109.6(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 118.2(3) . . ? C23 C18 P1 118.7(3) . . ? C19 C18 P1 123.0(3) . . ? C20 C19 C18 118.7(3) . . ? C20 C19 C24 115.4(3) . . ? C18 C19 C24 125.8(3) . . ? C21 C20 C19 122.3(4) . . ? C21 C20 H20A 118.8 . . ? C19 C20 H20A 118.8 . . ? C20 C21 C22 119.4(3) . . ? C20 C21 H21A 120.3 . . ? C22 C21 H21A 120.3 . . ? C23 C22 C21 119.5(3) . . ? C23 C22 H22A 120.3 . . ? C21 C22 H22A 120.3 . . ? C22 C23 C18 121.8(3) . . ? C22 C23 H23A 119.1 . . ? C18 C23 H23A 119.1 . . ? C29 C24 C25 119.1(4) . . ? C29 C24 C19 120.2(4) . . ? C25 C24 C19 120.3(4) . . ? C26 C25 C24 120.4(4) . . ? C26 C25 H25A 119.8 . . ? C24 C25 H25A 119.8 . . ? C27 C26 C25 119.8(5) . . ? C27 C26 H26A 120.1 . . ? C25 C26 H26A 120.1 . . ? C26 C27 C28 120.9(4) . . ? C26 C27 H27A 119.5 . . ? C28 C27 H27A 119.5 . . ? C27 C28 C29 119.6(5) . . ? C27 C28 H28A 120.2 . . ? C29 C28 H28A 120.2 . . ? C24 C29 C28 120.2(4) . . ? C24 C29 H29A 119.9 . . ? C28 C29 H29A 119.9 . . ? 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 C2 Au1 P1 C18 -143.5(3) . . . . ? C2 Au1 P1 C10 -26.8(3) . . . . ? C2 Au1 P1 C14 98.2(3) . . . . ? Au1 C1 C2 C3 97.6(5) . . . . ? P1 Au1 C2 C1 -174.8(3) . . . . ? C1 Au1 C2 C3 -124.0(6) . . . . ? P1 Au1 C2 C3 61.1(5) . . . . ? C1 C2 C3 C8 2.3(8) . . . . ? Au1 C2 C3 C8 79.2(5) . . . . ? C1 C2 C3 C4 178.3(5) . . . . ? Au1 C2 C3 C4 -104.8(4) . . . . ? C8 C3 C4 C5 0.5(7) . . . . ? C2 C3 C4 C5 -175.9(4) . . . . ? C3 C4 C5 C6 0.5(8) . . . . ? C4 C5 C6 C7 -0.1(8) . . . . ? C4 C5 C6 C9 178.6(5) . . . . ? C5 C6 C7 C8 -1.2(7) . . . . ? C9 C6 C7 C8 -179.9(5) . . . . ? C6 C7 C8 C3 2.2(7) . . . . ? C4 C3 C8 C7 -1.7(6) . . . . ? C2 C3 C8 C7 174.4(4) . . . . ? C18 P1 C10 C12 -51.0(3) . . . . ? C14 P1 C10 C12 67.7(3) . . . . ? Au1 P1 C10 C12 -173.0(3) . . . . ? C18 P1 C10 C13 -174.5(3) . . . . ? C14 P1 C10 C13 -55.9(3) . . . . ? Au1 P1 C10 C13 63.4(3) . . . . ? C18 P1 C10 C11 68.1(3) . . . . ? C14 P1 C10 C11 -173.2(3) . . . . ? Au1 P1 C10 C11 -53.9(3) . . . . ? C18 P1 C14 C16 62.0(4) . . . . ? C10 P1 C14 C16 -56.5(4) . . . . ? Au1 P1 C14 C16 -174.8(3) . . . . ? C18 P1 C14 C15 -58.7(3) . . . . ? C10 P1 C14 C15 -177.1(3) . . . . ? Au1 P1 C14 C15 64.6(3) . . . . ? C18 P1 C14 C17 -173.6(3) . . . . ? C10 P1 C14 C17 68.0(4) . . . . ? Au1 P1 C14 C17 -50.3(3) . . . . ? C10 P1 C18 C23 63.2(3) . . . . ? C14 P1 C18 C23 -61.7(3) . . . . ? Au1 P1 C18 C23 179.5(2) . . . . ? C10 P1 C18 C19 -114.1(3) . . . . ? C14 P1 C18 C19 121.0(3) . . . . ? Au1 P1 C18 C19 2.2(3) . . . . ? C23 C18 C19 C20 -2.0(5) . . . . ? P1 C18 C19 C20 175.3(3) . . . . ? C23 C18 C19 C24 175.4(4) . . . . ? P1 C18 C19 C24 -7.3(5) . . . . ? C18 C19 C20 C21 2.0(6) . . . . ? C24 C19 C20 C21 -175.7(3) . . . . ? C19 C20 C21 C22 -0.5(6) . . . . ? C20 C21 C22 C23 -0.8(5) . . . . ? C21 C22 C23 C18 0.7(6) . . . . ? C19 C18 C23 C22 0.7(5) . . . . ? P1 C18 C23 C22 -176.7(3) . . . . ? C20 C19 C24 C29 98.8(4) . . . . ? C18 C19 C24 C29 -78.6(5) . . . . ? C20 C19 C24 C25 -73.0(5) . . . . ? C18 C19 C24 C25 109.5(4) . . . . ? C29 C24 C25 C26 -1.5(6) . . . . ? C19 C24 C25 C26 170.5(4) . . . . ? C24 C25 C26 C27 0.0(7) . . . . ? C25 C26 C27 C28 1.2(7) . . . . ? C26 C27 C28 C29 -0.9(7) . . . . ? C25 C24 C29 C28 1.7(6) . . . . ? C19 C24 C29 C28 -170.2(4) . . . . ? C27 C28 C29 C24 -0.6(6) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.20 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.190 _refine_diff_density_min -1.002 _refine_diff_density_rms 0.124