# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address S.K.Bhargava ; Department of Applied Chemistry, RMIT University, GPO Box 2476V, Melbourne, Victoria, 3001, Australia ; K.Kitadai ; Department of Chemistry Toho University Chiba, Japan ; M.Takahashi ; Department of Chemistry Toho University Chiba, Japan ; D.Drumm ; Department of Applied Chemistry, RMIT University, GPO Box 2476V, Melbourne, Victoria, 3001, Australia ; S.Russo ; Department of Applied Chemistry, RMIT University, GPO Box 2476V, Melbourne, Victoria, 3001, Australia ; ; V.Wing-Wah Yam ; ; Department of Chemistry, The University of Hong Kong, Pokfulam Road, Hong Kong, P.R. China ; 'T.Kwok-Ming Lee' ; Department of Chemistry, The University of Hong Kong, Pokfulam Road, Hong Kong, P.R. China ; J.Wagler ; Institut f\"ur Anorganische Chemie Technische Universit\"at Bergakademie Freiberg Leipziger Str. 29 09596 Freiberg Bundesrepublik Deutschland ; N.Mirzadeh ; Department of Applied Chemistry, RMIT University, GPO Box 2476V, Melbourne, Victoria, 3001, Australia ; #TrackingRef '- all-in-one.cif' # 1. SUBMISSION DETAILS _publ_contact_author ;Wagler, J\"org Institut f\"ur Anorganische Chemie Technische Universit\"at Bergakademie Freiberg Leipziger Str. 29 09596 Freiberg Bundesrepublik Deutschland ; _publ_contact_author_fax ' 03731 39-4058 ' _publ_contact_author_phone ' 03731 39-3556 ' _publ_section_title ; Synthesis, structures and luminescent properties of cyclic gold complexes containing diphosphine ligands ; _publ_contact_author_name 'Wagler, Jorg' _publ_contact_author_email joerg.wagler@chemie.tu-freiberg.de data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 843620' _publ_section_abstract ; A mixture of cyclic gold(I) complexes [Au2(mu-cis-dppen)2]X2 (X =OTf 1, PF6 3) and [Au(cis-dppen)2]X (X = OTf 2, PF6 4) is obtained from the reaction of [Au(tht)2]X (tht = tetrahydrothiophene) with one equivalent of cis-dppen [dppen = 1,2-bis(diphenylphosphino)ethylene]. The analogous reaction with trans-dppen or dppa [dppa = bis(diphenylphosphino)acetylene] affords the cyclic trinuclear [Au3(mu-trans-dppen)3]X3 (X = OTf 11, PF6 12) and tetranuclear [Au4(mu-dppa)4]X4 (X = OTf 13, PF6 14, ClO4 15) gold complexes, respectively. Recrystallization of 15 from CH2Cl2/MeOH yielded a crystal of the octanuclear gold cluster [Au8Cl2(mu-dppa)4](ClO4)2 16. Attempts to prepare dicationic binuclear gold(II) species from the reaction of a mixture of 3 and 4 with halogens gave a mixture of products, the components of which confirmed to be acyclic binuclear gold(I) [Au2X2(cis-dppen)] (X = I 5, Br 7) and cyclic mononuclear gold(III) [AuX2(cis-dppen)]PF6 (X = I 6 , Br 8) complexes. Complexes 11-14 reveal weak emission in butyronitrile glass at 77 K, but they are non-emissive at room temperature. Ab initio modelling was performed to rationalize the conformations adopted in tri- and tetranuclear structures. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H44 Au2 P4, 2(C F3 O3 S)' _chemical_formula_sum 'C54 H44 Au2 F6 O6 P4 S2' _chemical_formula_weight 1484.82 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' O O 0.0106 0.0060 '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' S S 0.1246 0.1234 '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 triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8043(6) _cell_length_b 10.9164(6) _cell_length_c 11.7847(6) _cell_angle_alpha 76.4730(10) _cell_angle_beta 82.9560(10) _cell_angle_gamma 73.3400(10) _cell_volume 1292.35(12) _cell_formula_units_Z 1 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.908 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 5.947 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.227 _exptl_absorpt_correction_T_max 0.435 _exptl_absorpt_process_details 'SADABS Sheldrick 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9611 _diffrn_reflns_av_R_equivalents 0.0179 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 28.30 _reflns_number_total 6330 _reflns_number_gt 6187 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+0.8615P] 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 6330 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0221 _refine_ls_R_factor_gt 0.0217 _refine_ls_wR_factor_ref 0.0586 _refine_ls_wR_factor_gt 0.0583 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.004 _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 -0.029356(8) 0.503798(8) 0.626220(7) 0.00888(4) Uani 1 1 d . . . C1 C 0.2218(2) 0.2843(2) 0.7940(2) 0.0101(4) Uani 1 1 d . . . C2 C 0.3518(3) 0.2331(3) 0.8192(2) 0.0134(5) Uani 1 1 d . . . C3 C 0.3916(3) 0.1094(3) 0.8899(2) 0.0152(5) Uani 1 1 d . . . C4 C 0.3025(3) 0.0384(3) 0.9368(2) 0.0174(5) Uani 1 1 d . . . C5 C 0.1736(3) 0.0895(3) 0.9104(3) 0.0180(5) Uani 1 1 d . . . C6 C 0.1329(3) 0.2117(3) 0.8380(2) 0.0146(5) Uani 1 1 d . . . C7 C 0.1461(2) 0.5546(2) 0.8161(2) 0.0104(4) Uani 1 1 d . . . C8 C 0.1813(3) 0.5051(3) 0.9313(2) 0.0166(5) Uani 1 1 d . . . C9 C 0.1715(3) 0.5904(3) 1.0050(2) 0.0199(6) Uani 1 1 d . . . C10 C 0.1243(3) 0.7241(3) 0.9648(2) 0.0188(5) Uani 1 1 d . . . C11 C 0.0853(3) 0.7736(3) 0.8513(3) 0.0214(6) Uani 1 1 d . . . C12 C 0.0965(3) 0.6892(3) 0.7770(2) 0.0185(6) Uani 1 1 d . . . C13 C 0.2937(2) 0.4884(2) 0.6125(2) 0.0112(5) Uani 1 1 d . . . C14 C 0.3204(2) 0.4669(2) 0.5043(2) 0.0111(5) Uani 1 1 d . . . C15 C 0.3421(2) 0.3594(3) 0.2997(2) 0.0119(5) Uani 1 1 d . . . C16 C 0.4265(3) 0.4343(3) 0.2459(2) 0.0162(5) Uani 1 1 d . . . C17 C 0.5014(3) 0.4056(3) 0.1459(3) 0.0224(6) Uani 1 1 d . . . C18 C 0.4901(3) 0.3056(3) 0.0971(3) 0.0243(6) Uani 1 1 d . . . C19 C 0.4036(3) 0.2332(3) 0.1482(3) 0.0245(6) Uani 1 1 d . . . C20 C 0.3300(3) 0.2596(3) 0.2495(2) 0.0175(5) Uani 1 1 d . . . C21 C 0.2479(3) 0.2270(3) 0.5171(2) 0.0115(5) Uani 1 1 d . . . C22 C 0.1376(3) 0.1815(3) 0.5468(2) 0.0139(5) Uani 1 1 d . . . C23 C 0.1481(3) 0.0554(3) 0.6128(3) 0.0188(5) Uani 1 1 d . . . C24 C 0.2680(3) -0.0235(3) 0.6494(2) 0.0189(6) Uani 1 1 d . . . C25 C 0.3779(3) 0.0215(3) 0.6198(2) 0.0177(5) Uani 1 1 d . . . C26 C 0.3683(3) 0.1467(3) 0.5536(2) 0.0151(5) Uani 1 1 d . . . C27 C 0.2669(3) 0.8455(3) 0.3639(3) 0.0214(6) Uani 1 1 d . . . F1 F 0.1657(2) 0.8641(3) 0.4408(2) 0.0425(6) Uani 1 1 d . . . F2 F 0.3041(2) 0.9553(2) 0.3316(2) 0.0369(5) Uani 1 1 d . . . F3 F 0.3640(2) 0.7543(2) 0.42057(18) 0.0300(4) Uani 1 1 d . . . H2 H 0.4125 0.2823 0.7884 0.016 Uiso 1 1 calc R . . H3 H 0.4802 0.0731 0.9061 0.018 Uiso 1 1 calc R . . H4 H 0.3297 -0.0450 0.9870 0.021 Uiso 1 1 calc R . . H5 H 0.1129 0.0405 0.9420 0.022 Uiso 1 1 calc R . . H6 H 0.0450 0.2456 0.8185 0.018 Uiso 1 1 calc R . . H8 H 0.2118 0.4134 0.9592 0.020 Uiso 1 1 calc R . . H9 H 0.1971 0.5570 1.0830 0.024 Uiso 1 1 calc R . . H10 H 0.1187 0.7821 1.0152 0.023 Uiso 1 1 calc R . . H11 H 0.0510 0.8651 0.8248 0.026 Uiso 1 1 calc R . . H12 H 0.0703 0.7230 0.6992 0.022 Uiso 1 1 calc R . . H13 H 0.3486 0.5283 0.6395 0.013 Uiso 1 1 calc R . . H14 H 0.3909 0.4958 0.4616 0.013 Uiso 1 1 calc R . . H16 H 0.4328 0.5047 0.2774 0.019 Uiso 1 1 calc R . . H17 H 0.5609 0.4549 0.1108 0.027 Uiso 1 1 calc R . . H18 H 0.5416 0.2867 0.0288 0.029 Uiso 1 1 calc R . . H19 H 0.3946 0.1658 0.1141 0.029 Uiso 1 1 calc R . . H20 H 0.2712 0.2096 0.2847 0.021 Uiso 1 1 calc R . . H22 H 0.0557 0.2362 0.5221 0.017 Uiso 1 1 calc R . . H23 H 0.0735 0.0235 0.6328 0.023 Uiso 1 1 calc R . . H24 H 0.2749 -0.1090 0.6950 0.023 Uiso 1 1 calc R . . H25 H 0.4596 -0.0333 0.6448 0.021 Uiso 1 1 calc R . . H26 H 0.4434 0.1777 0.5332 0.018 Uiso 1 1 calc R . . O1 O 0.1854(2) 0.6789(2) 0.29444(18) 0.0189(4) Uani 1 1 d . . . O2 O 0.1277(2) 0.9043(2) 0.18563(19) 0.0211(4) Uani 1 1 d . . . O3 O 0.3501(2) 0.7688(2) 0.17163(19) 0.0214(4) Uani 1 1 d . . . P1 P 0.16317(6) 0.44902(6) 0.71331(5) 0.00885(12) Uani 1 1 d . . . P2 P 0.23799(6) 0.38899(6) 0.42927(5) 0.00885(12) Uani 1 1 d . . . S1 S 0.22779(6) 0.79422(6) 0.23888(6) 0.01252(12) 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 0.00786(6) 0.01045(6) 0.00743(6) -0.00203(4) 0.00092(4) -0.00150(4) C1 0.0127(11) 0.0104(11) 0.0064(10) -0.0018(9) 0.0013(9) -0.0025(9) C2 0.0121(12) 0.0142(12) 0.0126(11) -0.0018(9) 0.0015(9) -0.0032(9) C3 0.0140(12) 0.0167(12) 0.0124(11) -0.0027(10) -0.0016(9) -0.0002(10) C4 0.0224(14) 0.0128(12) 0.0136(12) -0.0005(10) -0.0001(10) -0.0015(10) C5 0.0185(13) 0.0156(13) 0.0186(13) 0.0001(10) 0.0024(11) -0.0067(10) C6 0.0130(12) 0.0166(12) 0.0141(12) -0.0032(10) 0.0016(9) -0.0046(10) C7 0.0110(11) 0.0122(11) 0.0084(11) -0.0039(9) 0.0018(9) -0.0030(9) C8 0.0180(13) 0.0175(13) 0.0120(12) -0.0049(10) -0.0019(10) 0.0010(10) C9 0.0205(14) 0.0258(15) 0.0131(12) -0.0083(11) -0.0003(10) -0.0027(11) C10 0.0210(13) 0.0238(14) 0.0151(13) -0.0118(11) 0.0046(10) -0.0077(11) C11 0.0336(16) 0.0139(13) 0.0167(13) -0.0064(11) 0.0050(12) -0.0061(12) C12 0.0271(15) 0.0135(12) 0.0126(12) -0.0019(10) -0.0003(11) -0.0027(11) C13 0.0092(11) 0.0116(11) 0.0128(11) -0.0022(9) 0.0004(9) -0.0036(9) C14 0.0095(11) 0.0119(11) 0.0118(11) -0.0015(9) 0.0015(9) -0.0046(9) C15 0.0110(11) 0.0132(11) 0.0086(11) -0.0024(9) 0.0015(9) 0.0005(9) C16 0.0151(12) 0.0214(14) 0.0117(12) -0.0032(10) 0.0015(10) -0.0054(10) C17 0.0177(13) 0.0310(16) 0.0135(13) -0.0017(11) 0.0055(11) -0.0038(12) C18 0.0267(15) 0.0257(15) 0.0110(12) -0.0037(11) 0.0061(11) 0.0045(12) C19 0.0382(18) 0.0159(13) 0.0145(13) -0.0066(11) 0.0021(12) 0.0018(12) C20 0.0279(15) 0.0121(12) 0.0101(12) -0.0024(10) 0.0009(11) -0.0024(11) C21 0.0140(12) 0.0125(12) 0.0079(11) -0.0023(9) 0.0005(9) -0.0038(9) C22 0.0121(12) 0.0147(12) 0.0142(12) -0.0028(10) 0.0019(9) -0.0038(10) C23 0.0222(14) 0.0163(13) 0.0176(13) -0.0015(11) 0.0042(11) -0.0083(11) C24 0.0274(15) 0.0126(12) 0.0137(12) -0.0010(10) 0.0028(11) -0.0037(11) C25 0.0185(13) 0.0155(13) 0.0152(12) -0.0028(10) -0.0036(10) 0.0025(10) C26 0.0136(12) 0.0158(12) 0.0154(12) -0.0032(10) -0.0007(10) -0.0031(10) C27 0.0222(14) 0.0244(15) 0.0209(14) -0.0069(12) -0.0025(11) -0.0091(12) F1 0.0338(12) 0.0739(17) 0.0316(12) -0.0349(12) 0.0093(9) -0.0184(12) F2 0.0500(13) 0.0230(10) 0.0470(13) -0.0073(9) -0.0156(11) -0.0189(9) F3 0.0322(11) 0.0316(10) 0.0294(10) 0.0018(8) -0.0153(9) -0.0143(9) O1 0.0199(10) 0.0177(10) 0.0208(10) -0.0008(8) 0.0006(8) -0.0112(8) O2 0.0192(10) 0.0192(10) 0.0215(10) 0.0001(8) -0.0025(8) -0.0027(8) O3 0.0163(10) 0.0256(11) 0.0207(10) -0.0045(9) 0.0070(8) -0.0067(8) P1 0.0089(3) 0.0104(3) 0.0066(3) -0.0016(2) 0.0006(2) -0.0022(2) P2 0.0081(3) 0.0103(3) 0.0075(3) -0.0022(2) 0.0018(2) -0.0019(2) S1 0.0122(3) 0.0130(3) 0.0124(3) -0.0018(2) 0.0015(2) -0.0051(2) _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 Au1 2.9802(2) 2_566 ? Au1 P1 2.2937(6) . ? Au1 P2 2.3172(6) 2_566 ? C1 C2 1.397(4) . ? C1 C6 1.394(4) . ? C1 P1 1.798(3) . ? C2 C3 1.390(4) . ? C3 C4 1.389(4) . ? C4 C5 1.389(4) . ? C5 C6 1.387(4) . ? C7 C12 1.397(4) . ? C7 C8 1.394(3) . ? C7 P1 1.818(3) . ? C8 C9 1.390(4) . ? C9 C10 1.387(4) . ? C10 C11 1.388(4) . ? C11 C12 1.385(4) . ? C13 C14 1.333(4) . ? C13 P1 1.812(3) . ? C14 P2 1.810(3) . ? C15 C16 1.394(4) . ? C15 C20 1.399(4) . ? C15 P2 1.818(3) . ? C16 C17 1.391(4) . ? C17 C18 1.387(5) . ? C18 C19 1.387(5) . ? C19 C20 1.392(4) . ? C21 C22 1.395(4) . ? C21 C26 1.397(4) . ? C21 P2 1.809(3) . ? C22 C23 1.394(4) . ? C23 C24 1.389(4) . ? C24 C25 1.387(4) . ? C25 C26 1.388(4) . ? C27 F3 1.342(4) . ? F1 C27 1.332(4) . ? F2 C27 1.330(4) . ? P2 Au1 2.3172(6) 2_566 ? S1 C27 1.826(3) . ? S1 O1 1.448(2) . ? S1 O2 1.441(2) . ? S1 O3 1.445(2) . ? 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 P1 Au1 118.12(9) . . ? C1 P1 C13 107.69(12) . . ? C1 P1 C7 106.26(11) . . ? C2 C1 P1 120.89(19) . . ? C3 C2 C1 119.3(2) . . ? C4 C3 C2 120.3(2) . . ? C5 C4 C3 119.9(3) . . ? C5 C6 C1 119.5(2) . . ? C6 C1 C2 120.4(2) . . ? C6 C1 P1 118.50(19) . . ? C6 C5 C4 120.4(3) . . ? C7 P1 Au1 107.91(8) . . ? C8 C7 C12 119.7(2) . . ? C8 C7 P1 122.0(2) . . ? C9 C10 C11 120.4(3) . . ? C9 C8 C7 119.8(3) . . ? C10 C9 C8 120.0(3) . . ? C11 C12 C7 120.2(3) . . ? C12 C11 C10 119.8(3) . . ? C12 C7 P1 118.26(19) . . ? C13 C14 P2 127.6(2) . . ? C13 P1 Au1 112.89(9) . . ? C13 P1 C7 102.65(12) . . ? C14 C13 P1 126.5(2) . . ? C14 P2 Au1 119.17(9) . 2_566 ? C14 P2 C15 104.91(12) . . ? C15 P2 Au1 108.94(8) . 2_566 ? C16 C15 C20 119.4(2) . . ? C16 C15 P2 123.7(2) . . ? C17 C16 C15 119.8(3) . . ? C18 C17 C16 120.6(3) . . ? C18 C19 C20 119.9(3) . . ? C19 C18 C17 120.0(3) . . ? C19 C20 C15 120.3(3) . . ? C20 C15 P2 116.8(2) . . ? C21 P2 Au1 111.72(9) . 2_566 ? C21 P2 C14 106.91(12) . . ? C21 P2 C15 103.96(12) . . ? C22 C21 C26 120.1(2) . . ? C22 C21 P2 120.7(2) . . ? C23 C22 C21 119.6(3) . . ? C24 C23 C22 119.8(3) . . ? C24 C25 C26 119.9(3) . . ? C25 C24 C23 120.6(3) . . ? C25 C26 C21 119.9(3) . . ? C26 C21 P2 119.1(2) . . ? F1 C27 F3 107.0(3) . . ? F1 C27 S1 111.1(2) . . ? F2 C27 F1 108.5(3) . . ? F2 C27 F3 106.9(2) . . ? F2 C27 S1 111.9(2) . . ? F3 C27 S1 111.2(2) . . ? O1 S1 C27 102.17(13) . . ? O2 S1 C27 103.91(14) . . ? O2 S1 O1 114.90(13) . . ? O2 S1 O3 115.71(13) . . ? O3 S1 C27 102.88(14) . . ? O3 S1 O1 114.70(13) . . ? P1 Au1 Au1 108.115(17) . 2_566 ? P1 Au1 P2 161.95(2) . 2_566 ? P2 Au1 Au1 84.561(16) 2_566 2_566 ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.881 _refine_diff_density_min -2.224 _refine_diff_density_rms 0.134 #===END data_compound_7 _database_code_depnum_ccdc_archive 'CCDC 843621' #TrackingRef '- all-in-one.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H22 Au2 Br2 P2' _chemical_formula_sum 'C26 H22 Au2 Br2 P2' _chemical_formula_weight 950.12 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 Cc _symmetry_space_group_name_Hall C-2yc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 13.2194(7) _cell_length_b 12.9069(7) _cell_length_c 15.6042(8) _cell_angle_alpha 90.00 _cell_angle_beta 101.7360(10) _cell_angle_gamma 90.00 _cell_volume 2606.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 14.444 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.015 _exptl_absorpt_correction_T_max 0.042 _exptl_absorpt_process_details 'SADABS Sheldrick 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9391 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 28.31 _reflns_number_total 4834 _reflns_number_gt 4728 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0221P)^2^+9.4068P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(1) _refine_ls_number_reflns 4834 _refine_ls_number_parameters 289 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0265 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0626 _refine_ls_wR_factor_gt 0.0624 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.056 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.238552(19) 0.39945(2) 0.624701(17) 0.01909(7) Uani 1 1 d . . . Au2 Au 0.228344(19) 0.474122(19) 0.440942(17) 0.01900(7) Uani 1 1 d . . . Br1 Br 0.05591(6) 0.43819(7) 0.60609(5) 0.02771(17) Uani 1 1 d . . . Br2 Br 0.15502(7) 0.64617(6) 0.42683(5) 0.03026(18) Uani 1 1 d . . . C1 C 0.4199(5) 0.2522(6) 0.7401(5) 0.0196(14) Uani 1 1 d . . . C2 C 0.4690(6) 0.1589(6) 0.7280(5) 0.0240(16) Uani 1 1 d . . . C3 C 0.4780(7) 0.0828(6) 0.7922(5) 0.0260(17) Uani 1 1 d . . . C4 C 0.4368(7) 0.0967(6) 0.8660(6) 0.0281(18) Uani 1 1 d . . . C5 C 0.3874(7) 0.1874(7) 0.8774(6) 0.0316(19) Uani 1 1 d . . . C6 C 0.3787(6) 0.2659(7) 0.8147(5) 0.0251(16) Uani 1 1 d . . . C7 C 0.4880(6) 0.4601(6) 0.7084(5) 0.0223(16) Uani 1 1 d . . . C8 C 0.5830(8) 0.4382(8) 0.7638(7) 0.041(2) Uani 1 1 d . . . C9 C 0.6508(10) 0.5203(9) 0.7926(8) 0.053(3) Uani 1 1 d . . . C10 C 0.6225(9) 0.6204(9) 0.7673(8) 0.044(3) Uani 1 1 d . . . C11 C 0.5311(8) 0.6410(8) 0.7146(8) 0.045(3) Uani 1 1 d . . . C12 C 0.4625(7) 0.5612(7) 0.6823(7) 0.0318(19) Uani 1 1 d . . . C13 C 0.4694(6) 0.3162(6) 0.5755(5) 0.0198(14) Uani 1 1 d . . . C14 C 0.4334(5) 0.3092(6) 0.4898(5) 0.0195(14) Uani 1 1 d . . . C15 C 0.2393(6) 0.2096(6) 0.4772(5) 0.0220(15) Uani 1 1 d . . . C16 C 0.2991(7) 0.1222(7) 0.5112(6) 0.0289(18) Uani 1 1 d . . . C17 C 0.2499(9) 0.0363(8) 0.5385(7) 0.046(3) Uani 1 1 d . . . C18 C 0.1441(11) 0.0362(9) 0.5321(9) 0.056(3) Uani 1 1 d . . . C19 C 0.0845(8) 0.1227(9) 0.4982(8) 0.048(3) Uani 1 1 d . . . C20 C 0.1328(7) 0.2073(7) 0.4718(6) 0.0297(18) Uani 1 1 d . . . C21 C 0.2959(6) 0.2813(6) 0.3224(5) 0.0188(14) Uani 1 1 d . . . C22 C 0.3470(7) 0.1926(7) 0.3014(6) 0.0284(18) Uani 1 1 d . . . C23 C 0.3378(7) 0.1641(7) 0.2146(6) 0.0320(19) Uani 1 1 d . . . C24 C 0.2788(7) 0.2207(7) 0.1496(5) 0.0278(17) Uani 1 1 d . . . C25 C 0.2289(6) 0.3099(6) 0.1686(5) 0.0230(15) Uani 1 1 d . . . C26 C 0.2378(6) 0.3397(6) 0.2545(5) 0.0235(15) Uani 1 1 d . . . H2 H 0.4957 0.1477 0.6767 0.029 Uiso 1 1 calc R . . H3 H 0.5132 0.0202 0.7851 0.031 Uiso 1 1 calc R . . H4 H 0.4427 0.0434 0.9087 0.034 Uiso 1 1 calc R . . H5 H 0.3591 0.1969 0.9281 0.038 Uiso 1 1 calc R . . H6 H 0.3446 0.3288 0.8230 0.030 Uiso 1 1 calc R . . H8 H 0.6010 0.3691 0.7815 0.049 Uiso 1 1 calc R . . H9 H 0.7160 0.5070 0.8295 0.064 Uiso 1 1 calc R . . H10 H 0.6686 0.6758 0.7875 0.053 Uiso 1 1 calc R . . H11 H 0.5129 0.7107 0.6991 0.054 Uiso 1 1 calc R . . H12 H 0.3993 0.5760 0.6429 0.038 Uiso 1 1 calc R . . H13 H 0.5400 0.2978 0.5947 0.024 Uiso 1 1 calc R . . H14 H 0.4827 0.2985 0.4541 0.023 Uiso 1 1 calc R . . H16 H 0.3718 0.1221 0.5153 0.035 Uiso 1 1 calc R . . H17 H 0.2894 -0.0225 0.5616 0.055 Uiso 1 1 calc R . . H18 H 0.1114 -0.0228 0.5507 0.067 Uiso 1 1 calc R . . H19 H 0.0118 0.1225 0.4936 0.057 Uiso 1 1 calc R . . H20 H 0.0926 0.2660 0.4492 0.036 Uiso 1 1 calc R . . H22 H 0.3878 0.1523 0.3465 0.034 Uiso 1 1 calc R . . H23 H 0.3731 0.1044 0.2004 0.038 Uiso 1 1 calc R . . H24 H 0.2716 0.1989 0.0905 0.033 Uiso 1 1 calc R . . H25 H 0.1890 0.3499 0.1228 0.028 Uiso 1 1 calc R . . H26 H 0.2041 0.4009 0.2677 0.028 Uiso 1 1 calc R . . P1 P 0.40318(14) 0.35609(15) 0.66105(13) 0.0180(4) Uani 1 1 d . . . P2 P 0.29890(14) 0.31803(14) 0.43454(12) 0.0164(3) 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 0.01638(12) 0.02060(13) 0.02080(13) 0.00014(11) 0.00496(9) 0.00145(10) Au2 0.02305(14) 0.01482(12) 0.01967(12) 0.00052(10) 0.00558(10) 0.00366(10) Br1 0.0179(3) 0.0340(4) 0.0327(4) -0.0011(3) 0.0084(3) 0.0040(3) Br2 0.0430(5) 0.0176(4) 0.0314(4) 0.0027(3) 0.0105(4) 0.0107(3) C1 0.011(3) 0.022(4) 0.024(4) 0.002(3) 0.000(3) -0.001(2) C2 0.019(4) 0.026(4) 0.026(4) -0.001(3) 0.002(3) -0.002(3) C3 0.029(4) 0.018(4) 0.027(4) 0.002(3) -0.004(3) -0.003(3) C4 0.023(4) 0.023(4) 0.035(5) 0.009(3) -0.003(4) -0.005(3) C5 0.029(4) 0.040(5) 0.028(4) 0.004(4) 0.011(3) -0.004(3) C6 0.022(4) 0.030(4) 0.025(4) 0.003(3) 0.007(3) 0.002(3) C7 0.018(4) 0.024(4) 0.024(4) -0.008(3) 0.001(3) -0.004(3) C8 0.040(5) 0.035(5) 0.038(5) -0.001(4) -0.014(4) -0.013(4) C9 0.045(6) 0.044(6) 0.059(7) -0.010(5) -0.016(6) -0.016(5) C10 0.042(6) 0.037(6) 0.052(6) -0.017(5) 0.007(5) -0.019(4) C11 0.040(6) 0.025(5) 0.072(8) -0.016(5) 0.016(5) 0.000(4) C12 0.024(4) 0.022(4) 0.048(5) -0.004(4) 0.004(4) 0.002(3) C13 0.018(4) 0.015(3) 0.024(4) 0.000(3) -0.001(3) -0.002(2) C14 0.013(3) 0.021(4) 0.024(4) 0.002(3) 0.003(3) 0.001(2) C15 0.023(4) 0.019(4) 0.022(3) 0.004(3) 0.001(3) -0.005(3) C16 0.033(5) 0.018(4) 0.032(4) 0.009(3) -0.003(4) 0.000(3) C17 0.056(7) 0.028(5) 0.048(6) 0.022(4) 0.001(5) -0.011(4) C18 0.061(7) 0.040(6) 0.071(8) 0.014(5) 0.024(6) -0.024(5) C19 0.033(5) 0.057(7) 0.054(7) 0.011(5) 0.013(5) -0.012(5) C20 0.027(4) 0.030(4) 0.033(4) -0.001(4) 0.010(4) -0.008(3) C21 0.021(4) 0.019(4) 0.017(3) -0.004(3) 0.007(3) 0.001(3) C22 0.033(5) 0.021(4) 0.033(5) 0.004(3) 0.010(4) 0.008(3) C23 0.041(5) 0.024(4) 0.032(4) -0.007(4) 0.009(4) 0.012(3) C24 0.035(5) 0.029(4) 0.020(4) -0.004(3) 0.006(3) 0.002(3) C25 0.023(4) 0.020(4) 0.026(4) 0.000(3) 0.007(3) -0.001(3) C26 0.026(4) 0.022(4) 0.024(4) 0.003(3) 0.008(3) 0.001(3) P1 0.0148(8) 0.0185(9) 0.0200(9) 0.0005(7) 0.0021(7) 0.0008(6) P2 0.0166(9) 0.0142(8) 0.0187(8) 0.0002(7) 0.0046(7) 0.0019(6) _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 Br1 2.4246(8) . ? Au1 P1 2.2065(19) . ? Au2 Au1 3.0020(4) . ? Au2 Br2 2.4149(8) . ? Au2 P2 2.2308(18) . ? C2 C1 1.399(11) . ? C2 C3 1.389(11) . ? C3 C4 1.383(13) . ? C4 C5 1.369(13) . ? C6 C1 1.394(11) . ? C6 C5 1.397(12) . ? C7 C12 1.388(12) . ? C7 C8 1.401(12) . ? C8 C9 1.401(14) . ? C10 C11 1.342(16) . ? C10 C9 1.381(17) . ? C12 C11 1.397(14) . ? C13 C14 1.328(10) . ? C15 C20 1.394(12) . ? C16 C15 1.418(11) . ? C16 C17 1.395(12) . ? C17 C18 1.381(18) . ? C19 C18 1.406(18) . ? C20 C19 1.370(13) . ? C21 C22 1.401(11) . ? C21 C26 1.396(11) . ? C22 C23 1.384(12) . ? C24 C23 1.360(12) . ? C25 C24 1.389(11) . ? C26 C25 1.376(11) . ? P1 C1 1.804(8) . ? P1 C13 1.814(8) . ? P1 C7 1.808(8) . ? P2 C14 1.815(7) . ? P2 C15 1.799(8) . ? P2 C21 1.806(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Br1 Au1 Au2 88.23(2) . . ? Br2 Au2 Au1 108.76(2) . . ? C1 C6 C5 120.1(8) . . ? C1 P1 Au1 110.0(2) . . ? C1 P1 C13 106.4(3) . . ? C1 P1 C7 107.0(4) . . ? C2 C1 P1 122.9(6) . . ? C3 C2 C1 119.1(8) . . ? C4 C3 C2 121.2(8) . . ? C4 C5 C6 120.2(8) . . ? C5 C4 C3 119.9(8) . . ? C6 C1 C2 119.5(7) . . ? C6 C1 P1 117.6(6) . . ? C7 C12 C11 119.1(9) . . ? C7 C8 C9 118.7(10) . . ? C7 P1 Au1 114.4(3) . . ? C7 P1 C13 99.2(4) . . ? C8 C7 P1 120.4(7) . . ? C10 C11 C12 120.8(10) . . ? C10 C9 C8 119.8(11) . . ? C11 C10 C9 121.2(9) . . ? C12 C7 C8 120.3(8) . . ? C12 C7 P1 119.0(6) . . ? C13 C14 P2 126.2(6) . . ? C13 P1 Au1 118.8(3) . . ? C14 C13 P1 129.2(6) . . ? C14 P2 Au2 114.4(3) . . ? C15 P2 Au2 117.9(3) . . ? C15 P2 C14 103.6(4) . . ? C15 P2 C21 103.3(4) . . ? C16 C15 P2 120.3(6) . . ? C17 C16 C15 119.2(9) . . ? C17 C18 C19 120.5(9) . . ? C18 C17 C16 120.5(9) . . ? C19 C20 C15 121.7(9) . . ? C20 C15 C16 119.1(7) . . ? C20 C15 P2 120.5(6) . . ? C20 C19 C18 119.1(10) . . ? C21 P2 Au2 110.7(3) . . ? C21 P2 C14 105.7(4) . . ? C22 C21 P2 121.6(6) . . ? C23 C22 C21 119.7(8) . . ? C23 C24 C25 120.7(7) . . ? C24 C23 C22 120.6(8) . . ? C25 C26 C21 120.8(7) . . ? C26 C21 C22 118.7(7) . . ? C26 C21 P2 119.6(6) . . ? C26 C25 C24 119.3(8) . . ? P1 Au1 Au2 100.21(5) . . ? P1 Au1 Br1 171.55(6) . . ? P2 Au2 Au1 79.33(5) . . ? P2 Au2 Br2 171.90(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.229 _refine_diff_density_min -1.005 _refine_diff_density_rms 0.143 #===END data_compound_5 _database_code_depnum_ccdc_archive 'CCDC 843622' #TrackingRef '- all-in-one.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H22 Au2 I2 P2' _chemical_formula_sum 'C26 H22 Au2 I2 P2' _chemical_formula_weight 1044.12 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 Cc _symmetry_space_group_name_Hall C-2yc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 13.340(4) _cell_length_b 12.988(4) _cell_length_c 16.396(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.629(6) _cell_angle_gamma 90.00 _cell_volume 2760.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.098 _exptl_crystal_size_min 0.093 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 12.980 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.237 _exptl_absorpt_correction_T_max 0.299 _exptl_absorpt_process_details 'SADABS Sheldrick 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9041 _diffrn_reflns_av_R_equivalents 0.0496 _diffrn_reflns_av_sigmaI/netI 0.0827 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 28.30 _reflns_number_total 4731 _reflns_number_gt 4033 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0895P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(1) _refine_ls_number_reflns 4731 _refine_ls_number_parameters 289 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0651 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1427 _refine_ls_wR_factor_gt 0.1360 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.980 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.003 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 0.34268(5) 0.96442(5) 0.32300(4) 0.03002(18) Uani 1 1 d . . . Au2 Au 0.34613(5) 0.88651(5) 0.49403(4) 0.03015(18) Uani 1 1 d . . . C1 C 0.4075(15) 0.7697(15) 0.2088(11) 0.032(4) Uani 1 1 d . . . C2 C 0.453(2) 0.6867(18) 0.1881(14) 0.049(6) Uani 1 1 d . . . C3 C 0.442(3) 0.657(2) 0.1044(16) 0.058(7) Uani 1 1 d . . . C4 C 0.396(2) 0.723(2) 0.0432(15) 0.055(6) Uani 1 1 d . . . C5 C 0.3506(17) 0.8144(15) 0.0592(13) 0.035(4) Uani 1 1 d . . . C6 C 0.3541(19) 0.8371(19) 0.1437(13) 0.045(5) Uani 1 1 d . . . C7 C 0.3429(13) 0.6975(14) 0.3522(11) 0.028(4) Uani 1 1 d . . . C8 C 0.2358(19) 0.6994(18) 0.3402(16) 0.048(6) Uani 1 1 d . . . C9 C 0.187(2) 0.616(2) 0.362(3) 0.075(10) Uani 1 1 d . . . C10 C 0.238(3) 0.533(3) 0.399(3) 0.095(13) Uani 1 1 d . . . C11 C 0.344(3) 0.530(2) 0.416(3) 0.089(12) Uani 1 1 d . . . C12 C 0.3960(18) 0.6109(15) 0.3884(17) 0.043(5) Uani 1 1 d . . . C13 C 0.5406(15) 0.7924(16) 0.3732(11) 0.034(4) Uani 1 1 d . . . C14 C 0.5772(14) 0.8038(14) 0.4537(12) 0.031(4) Uani 1 1 d . . . C15 C 0.5341(14) 0.7432(13) 0.6105(12) 0.029(4) Uani 1 1 d . . . C16 C 0.5888(16) 0.6551(15) 0.6052(13) 0.036(4) Uani 1 1 d . . . C17 C 0.5975(14) 0.5796(15) 0.6646(12) 0.033(4) Uani 1 1 d . . . C18 C 0.5530(17) 0.5912(15) 0.7333(16) 0.041(5) Uani 1 1 d . . . C19 C 0.4967(16) 0.6788(17) 0.7398(14) 0.041(5) Uani 1 1 d . . . C20 C 0.4853(17) 0.7573(16) 0.6794(13) 0.040(5) Uani 1 1 d . . . C21 C 0.5950(17) 0.9517(16) 0.5787(12) 0.034(4) Uani 1 1 d . . . C22 C 0.691(2) 0.934(2) 0.636(2) 0.071(10) Uani 1 1 d . . . C23 C 0.753(2) 1.016(2) 0.664(2) 0.074(10) Uani 1 1 d . . . C24 C 0.725(2) 1.117(2) 0.637(2) 0.061(8) Uani 1 1 d . . . C25 C 0.631(2) 1.1329(19) 0.576(2) 0.067(10) Uani 1 1 d . . . C26 C 0.5684(19) 1.0489(18) 0.553(2) 0.058(7) Uani 1 1 d . . . H2 H 0.4940 0.6457 0.2313 0.059 Uiso 1 1 calc R . . H3 H 0.4673 0.5926 0.0909 0.070 Uiso 1 1 calc R . . H4 H 0.3939 0.7056 -0.0134 0.066 Uiso 1 1 calc R . . H5 H 0.3187 0.8597 0.0152 0.042 Uiso 1 1 calc R . . H6 H 0.3211 0.8972 0.1577 0.054 Uiso 1 1 calc R . . H8 H 0.1976 0.7585 0.3170 0.058 Uiso 1 1 calc R . . H9 H 0.1141 0.6170 0.3504 0.090 Uiso 1 1 calc R . . H10 H 0.2004 0.4757 0.4134 0.114 Uiso 1 1 calc R . . H11 H 0.3807 0.4747 0.4466 0.106 Uiso 1 1 calc R . . H12 H 0.4685 0.6064 0.3944 0.052 Uiso 1 1 calc R . . H13 H 0.5887 0.7754 0.3408 0.040 Uiso 1 1 calc R . . H14 H 0.6484 0.7881 0.4734 0.038 Uiso 1 1 calc R . . H16 H 0.6210 0.6464 0.5598 0.043 Uiso 1 1 calc R . . H17 H 0.6344 0.5184 0.6592 0.040 Uiso 1 1 calc R . . H18 H 0.5615 0.5392 0.7752 0.049 Uiso 1 1 calc R . . H19 H 0.4651 0.6860 0.7857 0.049 Uiso 1 1 calc R . . H20 H 0.4467 0.8177 0.6838 0.048 Uiso 1 1 calc R . . H22 H 0.7119 0.8659 0.6539 0.086 Uiso 1 1 calc R . . H23 H 0.8169 1.0047 0.7034 0.089 Uiso 1 1 calc R . . H24 H 0.7680 1.1732 0.6593 0.073 Uiso 1 1 calc R . . H25 H 0.6128 1.1990 0.5528 0.081 Uiso 1 1 calc R . . H26 H 0.5025 1.0598 0.5166 0.069 Uiso 1 1 calc R . . I1 I 0.28074(11) 1.15203(9) 0.31141(9) 0.0393(3) Uani 1 1 d . . . I2 I 0.15265(10) 0.92595(11) 0.47646(8) 0.0373(3) Uani 1 1 d . . . P1 P 0.4064(4) 0.8056(4) 0.3165(3) 0.0280(9) Uani 1 1 d . . . P2 P 0.5129(4) 0.8451(4) 0.5337(3) 0.0283(10) 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 0.0354(4) 0.0277(3) 0.0242(3) 0.0008(3) 0.0016(3) 0.0044(3) Au2 0.0294(3) 0.0337(3) 0.0241(3) 0.0007(3) -0.0002(2) 0.0028(3) C1 0.035(9) 0.036(9) 0.021(8) 0.005(7) -0.002(7) 0.011(8) C2 0.065(16) 0.040(11) 0.031(11) 0.002(9) -0.010(10) 0.018(11) C3 0.09(2) 0.052(13) 0.032(12) -0.010(10) 0.003(12) 0.021(13) C4 0.070(16) 0.058(14) 0.031(11) 0.005(10) 0.002(11) 0.025(13) C5 0.044(11) 0.027(8) 0.034(10) -0.004(8) 0.011(8) -0.006(8) C6 0.051(13) 0.058(13) 0.024(9) 0.021(10) 0.008(9) 0.022(11) C7 0.023(8) 0.034(9) 0.024(8) 0.003(7) 0.003(7) 0.006(7) C8 0.053(14) 0.040(11) 0.054(14) 0.001(10) 0.014(11) 0.011(10) C9 0.047(15) 0.061(16) 0.11(3) -0.002(17) 0.007(17) -0.026(13) C10 0.09(3) 0.06(2) 0.13(3) 0.009(18) 0.00(2) -0.039(18) C11 0.08(2) 0.049(15) 0.14(4) 0.035(18) 0.03(2) -0.001(15) C12 0.030(10) 0.035(10) 0.062(16) 0.013(10) 0.007(10) -0.002(8) C13 0.030(9) 0.052(11) 0.021(8) -0.004(8) 0.009(7) 0.000(8) C14 0.022(8) 0.039(9) 0.030(9) -0.002(8) -0.003(7) 0.006(7) C15 0.024(8) 0.031(8) 0.029(9) 0.002(7) -0.003(7) -0.006(7) C16 0.038(11) 0.036(9) 0.028(10) 0.000(8) 0.000(8) 0.002(8) C17 0.024(8) 0.036(9) 0.030(10) -0.006(8) -0.012(7) 0.011(7) C18 0.037(11) 0.029(9) 0.052(14) 0.007(9) 0.000(10) -0.001(8) C19 0.034(10) 0.053(12) 0.034(10) 0.015(9) 0.004(8) -0.017(9) C20 0.051(12) 0.037(10) 0.025(9) 0.017(8) -0.009(8) -0.013(9) C21 0.036(10) 0.044(11) 0.020(9) -0.003(8) 0.000(7) 0.005(8) C22 0.072(18) 0.046(13) 0.068(19) -0.010(12) -0.040(15) -0.009(13) C23 0.052(15) 0.069(18) 0.08(2) -0.004(15) -0.034(15) -0.013(13) C24 0.047(15) 0.050(14) 0.08(2) -0.008(13) 0.007(14) -0.026(12) C25 0.044(14) 0.031(11) 0.12(3) -0.012(13) 0.005(16) -0.005(10) C26 0.035(12) 0.044(13) 0.09(2) 0.005(13) 0.004(13) -0.011(10) I1 0.0524(8) 0.0283(5) 0.0374(7) 0.0030(5) 0.0107(6) 0.0078(5) I2 0.0314(6) 0.0451(7) 0.0340(7) -0.0006(6) 0.0048(5) 0.0051(5) P1 0.030(2) 0.029(2) 0.022(2) -0.0009(18) 0.0004(17) 0.0027(19) P2 0.027(2) 0.029(2) 0.025(2) 0.0006(18) -0.0015(18) 0.0014(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 Au2 2.9714(12) . ? Au1 I1 2.5656(15) . ? Au1 P1 2.243(5) . ? Au2 I2 2.5801(16) . ? Au2 P2 2.231(5) . ? C2 C1 1.32(3) . ? C2 C3 1.40(3) . ? C4 C3 1.35(3) . ? C5 C4 1.39(3) . ? C6 C1 1.43(2) . ? C6 C5 1.41(3) . ? C7 C12 1.39(3) . ? C7 C8 1.40(3) . ? C8 C9 1.35(4) . ? C10 C11 1.37(5) . ? C10 C9 1.35(5) . ? C12 C11 1.39(4) . ? C14 C13 1.30(3) . ? C15 C16 1.37(3) . ? C17 C16 1.37(3) . ? C17 C18 1.40(3) . ? C19 C18 1.38(3) . ? C20 C15 1.44(3) . ? C20 C19 1.40(3) . ? C21 C22 1.42(3) . ? C21 C26 1.35(3) . ? C23 C22 1.36(4) . ? C23 C24 1.40(4) . ? C24 C25 1.42(4) . ? C25 C26 1.37(3) . ? P1 C1 1.83(2) . ? P1 C13 1.82(2) . ? P1 C7 1.81(2) . ? P2 C14 1.81(2) . ? P2 C15 1.803(18) . ? P2 C21 1.81(2) . ? 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 C2 C3 122(2) . . ? C1 P1 Au1 111.7(6) . . ? C2 C1 C6 119.0(19) . . ? C2 C1 P1 124.4(15) . . ? C3 C4 C5 123(2) . . ? C4 C3 C2 119(2) . . ? C4 C5 C6 117(2) . . ? C5 C6 C1 120(2) . . ? C6 C1 P1 116.6(16) . . ? C7 C12 C11 120(3) . . ? C7 P1 Au1 119.2(6) . . ? C7 P1 C1 103.0(9) . . ? C7 P1 C13 104.0(9) . . ? C8 C7 P1 118.9(15) . . ? C8 C9 C10 123(3) . . ? C9 C8 C7 119(2) . . ? C10 C11 C12 119(3) . . ? C11 C10 C9 119(3) . . ? C12 C7 C8 118.6(19) . . ? C12 C7 P1 122.5(15) . . ? C13 C14 P2 129.7(15) . . ? C13 P1 Au1 113.6(7) . . ? C13 P1 C1 103.8(9) . . ? C14 C13 P1 126.5(16) . . ? C14 P2 Au2 118.1(6) . . ? C14 P2 C21 100.2(10) . . ? C15 C16 C17 121(2) . . ? C15 P2 Au2 111.2(6) . . ? C15 P2 C14 105.4(9) . . ? C15 P2 C21 107.2(8) . . ? C16 C15 C20 120.1(18) . . ? C16 C15 P2 124.5(17) . . ? C16 C17 C18 121.0(19) . . ? C18 C19 C20 121(2) . . ? C19 C18 C17 119(2) . . ? C19 C20 C15 118(2) . . ? C20 C15 P2 115.4(14) . . ? C21 C26 C25 124(3) . . ? C21 P2 Au2 113.6(7) . . ? C22 C21 P2 120.7(16) . . ? C22 C23 C24 122(2) . . ? C23 C22 C21 119(2) . . ? C23 C24 C25 119(2) . . ? C26 C21 C22 119(2) . . ? C26 C21 P2 119.9(17) . . ? C26 C25 C24 117(2) . . ? I1 Au1 Au2 109.06(4) . . ? I2 Au2 Au1 91.97(4) . . ? P1 Au1 Au2 79.04(13) . . ? P1 Au1 I1 171.44(14) . . ? P2 Au2 Au1 98.61(13) . . ? P2 Au2 I2 169.37(14) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 3.867 _refine_diff_density_min -4.442 _refine_diff_density_rms 0.357 #===END data_compound_6 _database_code_depnum_ccdc_archive 'CCDC 843623' #TrackingRef '- all-in-one.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H22 Au I2 P2, F6 P' _chemical_formula_sum 'C26 H22 Au F6 I2 P3' _chemical_formula_weight 992.11 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' I I -0.4742 1.8119 '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 -P2ybc 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 17.6151(8) _cell_length_b 9.3424(4) _cell_length_c 19.5736(9) _cell_angle_alpha 90.00 _cell_angle_beta 111.3970(10) _cell_angle_gamma 90.00 _cell_volume 2999.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.096 _exptl_crystal_size_min 0.064 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.197 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 7.177 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.442 _exptl_absorpt_correction_T_max 0.632 _exptl_absorpt_process_details 'SADABS Sheldrick 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21835 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 28.34 _reflns_number_total 7463 _reflns_number_gt 6233 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0556P)^2^+3.9304P] 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 7463 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0942 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 0.948 _refine_ls_restrained_S_all 0.948 _refine_ls_shift/su_max 0.290 _refine_ls_shift/su_mean 0.017 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 0.334199(10) 0.607336(19) 0.189239(9) 0.03985(7) Uani 1 1 d . . . C1 C 0.3456(3) 0.5361(5) 0.3657(3) 0.0475(11) Uani 1 1 d . . . C2 C 0.4097(3) 0.4494(6) 0.3675(3) 0.0549(12) Uani 1 1 d . . . C3 C 0.4473(4) 0.3623(7) 0.4285(4) 0.0709(17) Uani 1 1 d . . . C4 C 0.4207(5) 0.3622(8) 0.4855(4) 0.079(2) Uani 1 1 d . . . C5 C 0.3571(6) 0.4464(10) 0.4831(4) 0.091(2) Uani 1 1 d . . . C6 C 0.3190(4) 0.5345(9) 0.4247(3) 0.0773(19) Uani 1 1 d . . . C7 C 0.2828(3) 0.8221(5) 0.3110(3) 0.0461(10) Uani 1 1 d . . . C8 C 0.3480(4) 0.8863(6) 0.3649(3) 0.0649(16) Uani 1 1 d . . . C9 C 0.3424(5) 1.0287(7) 0.3819(4) 0.0784(19) Uani 1 1 d . . . C10 C 0.2727(5) 1.1042(7) 0.3468(4) 0.0754(19) Uani 1 1 d . . . C11 C 0.2077(4) 1.0414(7) 0.2926(4) 0.0717(17) Uani 1 1 d . . . C12 C 0.2128(4) 0.8994(6) 0.2737(3) 0.0565(13) Uani 1 1 d . . . C13 C 0.1871(3) 0.5689(6) 0.2536(3) 0.0464(11) Uani 1 1 d . . . C14 C 0.1558(3) 0.5051(5) 0.1899(3) 0.0466(11) Uani 1 1 d . . . C15 C 0.1497(3) 0.5636(5) 0.0443(3) 0.0456(10) Uani 1 1 d . . . C16 C 0.1006(3) 0.6797(6) 0.0453(3) 0.0547(12) Uani 1 1 d . . . C17 C 0.0557(4) 0.7467(7) -0.0200(4) 0.0669(16) Uani 1 1 d . . . C18 C 0.0572(4) 0.6958(8) -0.0855(3) 0.0712(17) Uani 1 1 d . . . C19 C 0.1034(4) 0.5803(8) -0.0870(3) 0.0744(18) Uani 1 1 d . . . C20 C 0.1509(4) 0.5154(7) -0.0226(3) 0.0610(14) Uani 1 1 d . . . C21 C 0.2284(3) 0.2985(5) 0.1225(3) 0.0442(10) Uani 1 1 d . . . C22 C 0.1699(4) 0.2156(7) 0.0731(4) 0.0756(19) Uani 1 1 d . . . C23 C 0.1803(5) 0.0695(7) 0.0708(5) 0.090(2) Uani 1 1 d . . . C24 C 0.2493(4) 0.0071(6) 0.1170(4) 0.0704(16) Uani 1 1 d . . . C25 C 0.3082(4) 0.0873(7) 0.1665(4) 0.0677(16) Uani 1 1 d . . . C26 C 0.2985(3) 0.2344(6) 0.1691(3) 0.0588(13) Uani 1 1 d . . . F1 F 0.1071(3) 0.4933(6) 0.3741(3) 0.1038(15) Uani 1 1 d . . . F2 F 0.0863(7) 0.2637(9) 0.3949(5) 0.245(6) Uani 1 1 d . . . F3 F -0.0273(3) 0.2579(6) 0.3075(4) 0.1223(19) Uani 1 1 d . . . F4 F 0.0025(5) 0.4763(9) 0.2805(5) 0.228(5) Uani 1 1 d . . . F5 F 0.0880(5) 0.3171(8) 0.2936(5) 0.193(4) Uani 1 1 d . . . F6 F -0.0034(7) 0.4268(10) 0.3858(6) 0.258(6) Uani 1 1 d . . . H2 H 0.4277 0.4490 0.3284 0.066 Uiso 1 1 calc R . . H3 H 0.4907 0.3040 0.4301 0.085 Uiso 1 1 calc R . . H4 H 0.4460 0.3044 0.5262 0.095 Uiso 1 1 calc R . . H5 H 0.3389 0.4444 0.5221 0.109 Uiso 1 1 calc R . . H6 H 0.2759 0.5925 0.4243 0.093 Uiso 1 1 calc R . . H8 H 0.3951 0.8344 0.3895 0.078 Uiso 1 1 calc R . . H9 H 0.3864 1.0732 0.4175 0.094 Uiso 1 1 calc R . . H10 H 0.2691 1.1991 0.3596 0.090 Uiso 1 1 calc R . . H11 H 0.1606 1.0938 0.2688 0.086 Uiso 1 1 calc R . . H12 H 0.1697 0.8567 0.2364 0.068 Uiso 1 1 calc R . . H13 H 0.1560 0.5780 0.2828 0.056 Uiso 1 1 calc R . . H14 H 0.1032 0.4684 0.1753 0.056 Uiso 1 1 calc R . . H16 H 0.0979 0.7118 0.0894 0.066 Uiso 1 1 calc R . . H17 H 0.0244 0.8267 -0.0197 0.080 Uiso 1 1 calc R . . H18 H 0.0263 0.7409 -0.1291 0.085 Uiso 1 1 calc R . . H19 H 0.1029 0.5452 -0.1317 0.089 Uiso 1 1 calc R . . H20 H 0.1841 0.4387 -0.0237 0.073 Uiso 1 1 calc R . . H22 H 0.1227 0.2581 0.0408 0.091 Uiso 1 1 calc R . . H23 H 0.1398 0.0139 0.0375 0.108 Uiso 1 1 calc R . . H24 H 0.2564 -0.0912 0.1149 0.085 Uiso 1 1 calc R . . H25 H 0.3551 0.0436 0.1987 0.081 Uiso 1 1 calc R . . H26 H 0.3394 0.2896 0.2023 0.071 Uiso 1 1 calc R . . I1 I 0.46808(2) 0.75214(5) 0.25967(2) 0.06774(12) Uani 1 1 d . . . I2 I 0.37689(3) 0.55694(6) 0.07628(3) 0.07959(15) Uani 1 1 d . . . P1 P 0.28911(7) 0.63944(14) 0.28567(7) 0.0410(3) Uani 1 1 d . . . P2 P 0.21220(7) 0.48671(13) 0.12990(6) 0.0404(2) Uani 1 1 d . . . P3 P 0.04073(9) 0.37284(16) 0.34078(8) 0.0542(3) 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 0.03492(10) 0.04146(11) 0.04524(11) -0.00282(7) 0.01708(8) -0.00470(6) C1 0.049(3) 0.046(3) 0.047(3) -0.005(2) 0.018(2) -0.007(2) C2 0.056(3) 0.045(3) 0.059(3) -0.003(2) 0.015(3) 0.000(2) C3 0.064(4) 0.052(3) 0.079(4) 0.003(3) 0.006(3) 0.003(3) C4 0.092(5) 0.061(4) 0.067(4) 0.009(3) 0.008(4) -0.013(4) C5 0.110(6) 0.112(6) 0.055(4) 0.018(4) 0.035(4) 0.002(5) C6 0.083(4) 0.099(5) 0.053(3) 0.012(3) 0.028(3) 0.018(4) C7 0.048(3) 0.043(3) 0.050(3) -0.009(2) 0.021(2) -0.006(2) C8 0.069(4) 0.053(3) 0.059(3) -0.009(3) 0.008(3) -0.005(3) C9 0.106(6) 0.057(4) 0.070(4) -0.018(3) 0.029(4) -0.018(4) C10 0.106(6) 0.047(3) 0.089(5) -0.017(3) 0.054(5) -0.009(3) C11 0.073(4) 0.050(3) 0.103(5) 0.000(3) 0.045(4) 0.009(3) C12 0.054(3) 0.054(3) 0.064(3) -0.008(2) 0.023(3) -0.004(2) C13 0.043(2) 0.053(3) 0.048(3) -0.003(2) 0.022(2) -0.006(2) C14 0.033(2) 0.055(3) 0.052(3) -0.005(2) 0.017(2) -0.009(2) C15 0.044(2) 0.045(2) 0.046(3) -0.008(2) 0.015(2) -0.004(2) C16 0.047(3) 0.055(3) 0.057(3) -0.008(2) 0.013(2) 0.001(2) C17 0.055(3) 0.054(3) 0.077(4) 0.001(3) 0.006(3) 0.009(3) C18 0.065(4) 0.077(4) 0.056(3) 0.013(3) 0.004(3) -0.005(3) C19 0.085(5) 0.089(5) 0.043(3) 0.000(3) 0.016(3) 0.009(4) C20 0.062(3) 0.074(4) 0.048(3) -0.004(3) 0.021(3) 0.013(3) C21 0.038(2) 0.042(2) 0.052(3) -0.005(2) 0.016(2) -0.0020(19) C22 0.065(4) 0.055(3) 0.078(4) -0.007(3) -0.008(3) -0.009(3) C23 0.093(5) 0.053(4) 0.095(5) -0.019(4) 0.000(4) -0.017(4) C24 0.090(5) 0.041(3) 0.084(4) 0.001(3) 0.036(4) -0.002(3) C25 0.057(3) 0.059(4) 0.080(4) 0.014(3) 0.016(3) 0.008(3) C26 0.050(3) 0.053(3) 0.066(3) -0.006(3) 0.013(3) -0.006(2) F1 0.089(3) 0.118(4) 0.106(3) -0.034(3) 0.038(3) -0.048(3) F2 0.265(11) 0.163(7) 0.183(8) 0.094(6) -0.065(8) 0.003(7) F3 0.097(3) 0.101(4) 0.177(5) -0.051(3) 0.060(3) -0.047(3) F4 0.208(8) 0.156(7) 0.195(8) 0.085(6) -0.076(6) -0.020(6) F5 0.213(8) 0.129(5) 0.327(11) -0.100(7) 0.204(8) -0.072(5) F6 0.327(11) 0.215(8) 0.395(13) -0.201(9) 0.326(11) -0.184(8) I1 0.04294(19) 0.0728(3) 0.0846(3) -0.0086(2) 0.01993(18) -0.02124(17) I2 0.0816(3) 0.1047(4) 0.0733(3) -0.0169(2) 0.0530(2) -0.0206(3) P1 0.0384(6) 0.0426(6) 0.0424(6) -0.0067(5) 0.0152(5) -0.0047(5) P2 0.0368(6) 0.0419(6) 0.0415(6) -0.0062(5) 0.0131(5) -0.0035(5) P3 0.0488(7) 0.0546(8) 0.0583(8) 0.0088(6) 0.0185(6) -0.0053(6) _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 I1 2.6306(4) . ? Au1 I2 2.6246(4) . ? Au1 P1 2.3189(12) . ? Au1 P2 2.3273(12) . ? C1 C6 1.395(8) . ? C1 P1 1.800(5) . ? C2 C1 1.379(7) . ? C2 C3 1.397(8) . ? C4 C3 1.359(11) . ? C4 C5 1.355(11) . ? C6 C5 1.369(10) . ? C7 C8 1.382(7) . ? C7 P1 1.792(5) . ? C8 C9 1.383(8) . ? C10 C9 1.364(11) . ? C11 C10 1.376(10) . ? C12 C11 1.389(8) . ? C12 C7 1.384(8) . ? C13 C14 1.308(7) . ? C13 P1 1.798(5) . ? C15 C16 1.392(7) . ? C15 C20 1.394(7) . ? C15 P2 1.785(5) . ? C16 C17 1.384(8) . ? C17 C18 1.376(9) . ? C19 C18 1.359(10) . ? C20 C19 1.374(8) . ? C21 C22 1.367(7) . ? C21 C26 1.376(7) . ? C21 P2 1.796(5) . ? C22 C23 1.380(9) . ? C24 C23 1.355(10) . ? C25 C24 1.357(9) . ? C26 C25 1.389(8) . ? P2 C14 1.802(5) . ? P3 F1 1.582(4) . ? P3 F2 1.478(6) . ? P3 F3 1.563(4) . ? P3 F4 1.483(6) . ? P3 F5 1.543(6) . ? P3 F6 1.461(6) . ? 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 C2 C3 119.4(6) . . ? C1 P1 Au1 113.23(17) . . ? C1 P1 C13 105.8(2) . . ? C2 C1 C6 119.5(5) . . ? C2 C1 P1 121.6(4) . . ? C3 C4 C5 119.9(7) . . ? C4 C3 C2 120.3(7) . . ? C5 C6 C1 119.1(7) . . ? C6 C1 P1 118.7(4) . . ? C6 C5 C4 121.7(7) . . ? C7 C12 C11 119.3(6) . . ? C7 C8 C9 119.2(6) . . ? C7 P1 Au1 115.02(17) . . ? C7 P1 C1 109.9(2) . . ? C7 P1 C13 106.9(2) . . ? C8 C7 P1 120.4(4) . . ? C9 C10 C11 120.7(6) . . ? C10 C11 C12 119.7(6) . . ? C10 C9 C8 120.4(7) . . ? C12 C7 C8 120.6(5) . . ? C12 C7 P1 119.0(4) . . ? C13 C14 P2 121.6(4) . . ? C13 P1 Au1 105.29(17) . . ? C14 C13 P1 121.3(4) . . ? C14 P2 Au1 104.87(16) . . ? C15 C16 C17 119.2(5) . . ? C15 P2 Au1 114.48(17) . . ? C15 P2 C14 106.0(2) . . ? C15 P2 C21 112.3(2) . . ? C16 C15 P2 118.3(4) . . ? C17 C18 C19 120.7(6) . . ? C18 C17 C16 120.4(6) . . ? C18 C19 C20 120.0(6) . . ? C19 C20 C15 120.5(6) . . ? C20 C15 C16 119.2(5) . . ? C20 C15 P2 122.5(4) . . ? C21 C26 C25 119.9(5) . . ? C21 P2 Au1 111.67(15) . . ? C21 P2 C14 106.7(2) . . ? C22 C21 P2 120.7(4) . . ? C23 C22 C21 120.6(6) . . ? C23 C24 C25 120.4(6) . . ? C24 C23 C22 120.1(6) . . ? C24 C25 C26 120.0(6) . . ? C26 C21 C22 119.0(5) . . ? C26 C21 P2 120.2(4) . . ? F2 P3 F1 93.9(4) . . ? F2 P3 F3 87.6(4) . . ? F2 P3 F4 171.7(8) . . ? F2 P3 F5 85.7(7) . . ? F3 P3 F1 177.9(3) . . ? F4 P3 F1 85.3(4) . . ? F4 P3 F3 93.4(4) . . ? F4 P3 F5 86.1(6) . . ? F5 P3 F1 90.5(3) . . ? F5 P3 F3 91.0(3) . . ? F6 P3 F1 88.9(3) . . ? F6 P3 F2 94.3(7) . . ? F6 P3 F3 89.6(3) . . ? F6 P3 F4 93.9(7) . . ? F6 P3 F5 179.4(4) . . ? I2 Au1 I1 93.218(15) . . ? P1 Au1 I1 90.84(3) . . ? P1 Au1 I2 175.83(3) . . ? P1 Au1 P2 86.60(4) . . ? P2 Au1 I1 177.00(3) . . ? P2 Au1 I2 89.36(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.621 _refine_diff_density_min -1.270 _refine_diff_density_rms 0.120 #===END data_compound_1_6 _database_code_depnum_ccdc_archive 'CCDC 843624' #TrackingRef '- all-in-one.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C104 H80 Au8 Cl2 P8, 2(Cl O4), 2(C H Cl3)' _chemical_formula_sum 'C106 H82 Au8 Cl10 O8 P8' _chemical_formula_weight 3661.71 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' O O 0.0106 0.0060 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6200(11) _cell_length_b 13.6183(11) _cell_length_c 16.8190(14) _cell_angle_alpha 72.088(2) _cell_angle_beta 73.716(2) _cell_angle_gamma 82.431(2) _cell_volume 2636.8(4) _cell_formula_units_Z 1 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.063 _exptl_crystal_size_min 0.044 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.306 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 11.513 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.423 _exptl_absorpt_correction_T_max 0.603 _exptl_absorpt_process_details 'SADABS Sheldrick 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19687 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0828 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 28.34 _reflns_number_total 12955 _reflns_number_gt 9932 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0628P)^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 12955 _refine_ls_number_parameters 631 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0783 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1291 _refine_ls_wR_factor_gt 0.1194 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.61793(3) 0.41989(3) 0.09525(2) 0.01499(10) Uani 1 1 d . . . Au2 Au 0.99477(3) 0.46813(3) 0.08277(2) 0.01188(9) Uani 1 1 d . . . Au3 Au 0.86210(3) 0.37477(3) 0.01762(2) 0.01340(9) Uani 1 1 d . . . Au4 Au 0.80287(3) 0.56184(3) 0.03141(2) 0.01300(9) Uani 1 1 d . . . C1 C 0.5585(9) 0.2340(8) 0.2907(6) 0.018(2) Uani 1 1 d . . . C2 C 0.4791(9) 0.1959(8) 0.2694(6) 0.019(2) Uani 1 1 d . . . C3 C 0.4482(10) 0.0934(9) 0.3113(7) 0.027(3) Uani 1 1 d . . . C4 C 0.4989(10) 0.0333(8) 0.3720(8) 0.026(3) Uani 1 1 d . . . C5 C 0.5783(11) 0.0702(9) 0.3953(8) 0.033(3) Uani 1 1 d . . . C6 C 0.6088(10) 0.1717(9) 0.3550(7) 0.026(3) Uani 1 1 d . . . C7 C 0.4960(8) 0.4440(8) 0.2993(6) 0.016(2) Uani 1 1 d . . . C8 C 0.4940(10) 0.4351(11) 0.3841(7) 0.031(3) Uani 1 1 d . . . C9 C 0.4123(11) 0.4904(10) 0.4311(8) 0.034(3) Uani 1 1 d . . . C10 C 0.3358(11) 0.5536(9) 0.3928(9) 0.038(3) Uani 1 1 d . . . C11 C 0.3383(12) 0.5605(11) 0.3087(10) 0.045(4) Uani 1 1 d . . . C12 C 0.4176(10) 0.5081(9) 0.2614(7) 0.027(3) Uani 1 1 d . . . C13 C 0.7206(8) 0.3729(8) 0.2617(6) 0.017(2) Uani 1 1 d . . . C14 C 0.8153(9) 0.3793(8) 0.2598(6) 0.016(2) Uani 1 1 d . . . C15 C 0.9688(8) 0.4832(7) 0.2930(7) 0.016(2) Uani 1 1 d . . . C16 C 1.0270(10) 0.5710(9) 0.2541(8) 0.027(3) Uani 1 1 d . . . C17 C 1.0367(12) 0.6356(10) 0.3002(8) 0.038(3) Uani 1 1 d . . . C18 C 0.9833(11) 0.6149(10) 0.3865(8) 0.031(3) Uani 1 1 d . . . C19 C 0.9217(11) 0.5270(9) 0.4277(7) 0.029(3) Uani 1 1 d . . . C20 C 0.9141(10) 0.4616(9) 0.3804(7) 0.025(3) Uani 1 1 d . . . C21 C 1.0245(9) 0.2767(8) 0.2657(6) 0.017(2) Uani 1 1 d . . . C22 C 0.9748(10) 0.2044(8) 0.3414(7) 0.023(2) Uani 1 1 d . . . C23 C 1.0293(12) 0.1096(9) 0.3672(8) 0.032(3) Uani 1 1 d . . . C24 C 1.1308(12) 0.0882(9) 0.3193(8) 0.034(3) Uani 1 1 d . . . C25 C 1.1814(11) 0.1591(11) 0.2443(8) 0.038(3) Uani 1 1 d . . . C26 C 1.1253(10) 0.2548(9) 0.2163(7) 0.026(3) Uani 1 1 d . . . C27 C 0.8650(9) 0.1753(8) -0.0761(6) 0.017(2) Uani 1 1 d . . . C28 C 0.9269(10) 0.1028(9) -0.1146(7) 0.026(3) Uani 1 1 d . . . C29 C 0.8922(11) 0.0801(9) -0.1795(8) 0.031(3) Uani 1 1 d . . . C30 C 0.7981(11) 0.1257(10) -0.2003(8) 0.034(3) Uani 1 1 d . . . C31 C 0.7351(10) 0.1964(8) -0.1596(7) 0.026(3) Uani 1 1 d . . . C32 C 0.7702(9) 0.2223(8) -0.1003(7) 0.019(2) Uani 1 1 d . . . C33 C 0.8522(8) 0.1070(8) 0.1091(6) 0.017(2) Uani 1 1 d . . . C34 C 0.8710(10) 0.1168(9) 0.1845(7) 0.024(2) Uani 1 1 d . . . C35 C 0.8350(11) 0.0435(10) 0.2601(8) 0.035(3) Uani 1 1 d . . . C36 C 0.7816(12) -0.0406(10) 0.2626(8) 0.038(3) Uani 1 1 d . . . C37 C 0.7614(11) -0.0484(9) 0.1890(8) 0.032(3) Uani 1 1 d . . . C38 C 0.7970(9) 0.0243(8) 0.1126(7) 0.019(2) Uani 1 1 d . . . C39 C 1.0455(8) 0.1948(7) -0.0127(6) 0.014(2) Uani 1 1 d . . . C40 C 0.8591(9) 0.7883(7) 0.0248(7) 0.018(2) Uani 1 1 d . . . C41 C 0.6761(9) 0.7165(8) 0.1642(6) 0.017(2) Uani 1 1 d . . . C42 C 0.5744(9) 0.7614(9) 0.1897(7) 0.025(3) Uani 1 1 d . . . C43 C 0.5302(10) 0.7584(9) 0.2750(7) 0.026(3) Uani 1 1 d . . . C44 C 0.5886(10) 0.7103(9) 0.3353(7) 0.029(3) Uani 1 1 d . . . C45 C 0.6909(11) 0.6659(10) 0.3086(8) 0.033(3) Uani 1 1 d . . . C46 C 0.7336(11) 0.6669(9) 0.2243(7) 0.029(3) Uani 1 1 d . . . C47 C 0.6471(8) 0.8001(8) -0.0101(6) 0.015(2) Uani 1 1 d . . . C48 C 0.5634(9) 0.7524(9) -0.0204(7) 0.022(2) Uani 1 1 d . . . C49 C 0.4890(9) 0.8111(9) -0.0645(7) 0.025(3) Uani 1 1 d . . . C50 C 0.4976(9) 0.9168(9) -0.0984(7) 0.024(2) Uani 1 1 d . . . C51 C 0.5809(9) 0.9616(9) -0.0875(8) 0.026(2) Uani 1 1 d . . . C52 C 0.6553(9) 0.9060(8) -0.0438(7) 0.020(2) Uani 1 1 d . . . C53 C 0.2265(10) 0.1949(10) 0.4599(8) 0.032(3) Uani 1 1 d . . . Cl1 Cl 0.6377(2) 0.4665(2) -0.05229(16) 0.0228(6) Uani 1 1 d . . . Cl2 Cl 0.7324(3) 0.1702(2) 0.55021(18) 0.0283(6) Uani 1 1 d . . . Cl3 Cl 0.1968(3) 0.3159(3) 0.3922(2) 0.0481(9) Uani 1 1 d . . . Cl4 Cl 0.3346(3) 0.2032(3) 0.5030(2) 0.0430(8) Uani 1 1 d . . . Cl5 Cl 0.1083(3) 0.1492(3) 0.5421(2) 0.0422(8) Uani 1 1 d . . . H2 H 0.4446 0.2384 0.2263 0.023 Uiso 1 1 calc R . . H3 H 0.3923 0.0666 0.2971 0.033 Uiso 1 1 calc R . . H4 H 0.4789 -0.0363 0.3991 0.032 Uiso 1 1 calc R . . H5 H 0.6121 0.0269 0.4386 0.040 Uiso 1 1 calc R . . H6 H 0.6631 0.1985 0.3708 0.032 Uiso 1 1 calc R . . H8 H 0.5477 0.3917 0.4102 0.037 Uiso 1 1 calc R . . H9 H 0.4100 0.4842 0.4894 0.041 Uiso 1 1 calc R . . H10 H 0.2811 0.5925 0.4240 0.046 Uiso 1 1 calc R . . H11 H 0.2836 0.6029 0.2832 0.054 Uiso 1 1 calc R . . H12 H 0.4191 0.5152 0.2030 0.032 Uiso 1 1 calc R . . H16 H 1.0614 0.5876 0.1939 0.033 Uiso 1 1 calc R . . H17 H 1.0802 0.6944 0.2725 0.046 Uiso 1 1 calc R . . H18 H 0.9883 0.6604 0.4181 0.038 Uiso 1 1 calc R . . H19 H 0.8853 0.5121 0.4875 0.035 Uiso 1 1 calc R . . H20 H 0.8715 0.4021 0.4078 0.030 Uiso 1 1 calc R . . H22 H 0.9041 0.2198 0.3751 0.027 Uiso 1 1 calc R . . H23 H 0.9956 0.0593 0.4185 0.038 Uiso 1 1 calc R . . H24 H 1.1677 0.0231 0.3379 0.041 Uiso 1 1 calc R . . H25 H 1.2531 0.1439 0.2119 0.045 Uiso 1 1 calc R . . H26 H 1.1575 0.3036 0.1634 0.031 Uiso 1 1 calc R . . H28 H 0.9913 0.0691 -0.0978 0.032 Uiso 1 1 calc R . . H29 H 0.9350 0.0327 -0.2085 0.038 Uiso 1 1 calc R . . H30 H 0.7747 0.1092 -0.2434 0.041 Uiso 1 1 calc R . . H31 H 0.6678 0.2263 -0.1734 0.032 Uiso 1 1 calc R . . H32 H 0.7293 0.2736 -0.0748 0.023 Uiso 1 1 calc R . . H34 H 0.9084 0.1739 0.1826 0.028 Uiso 1 1 calc R . . H35 H 0.8463 0.0498 0.3118 0.042 Uiso 1 1 calc R . . H36 H 0.7591 -0.0929 0.3156 0.046 Uiso 1 1 calc R . . H37 H 0.7223 -0.1047 0.1914 0.038 Uiso 1 1 calc R . . H38 H 0.7838 0.0182 0.0615 0.023 Uiso 1 1 calc R . . H42 H 0.5336 0.7951 0.1483 0.030 Uiso 1 1 calc R . . H43 H 0.4590 0.7898 0.2923 0.031 Uiso 1 1 calc R . . H44 H 0.5587 0.7078 0.3943 0.035 Uiso 1 1 calc R . . H45 H 0.7329 0.6339 0.3494 0.040 Uiso 1 1 calc R . . H46 H 0.8034 0.6330 0.2074 0.035 Uiso 1 1 calc R . . H48 H 0.5574 0.6798 0.0027 0.027 Uiso 1 1 calc R . . H49 H 0.4314 0.7788 -0.0717 0.030 Uiso 1 1 calc R . . H50 H 0.4464 0.9575 -0.1288 0.028 Uiso 1 1 calc R . . H51 H 0.5873 1.0342 -0.1113 0.031 Uiso 1 1 calc R . . H52 H 0.7121 0.9394 -0.0365 0.023 Uiso 1 1 calc R . . H53 H 0.2505 0.1451 0.4244 0.039 Uiso 1 1 calc R . . O1 O 0.7662(8) 0.0950(7) 0.5029(6) 0.039(2) Uani 1 1 d . . . O2 O 0.6928(7) 0.1194(7) 0.6394(5) 0.035(2) Uani 1 1 d . . . O3 O 0.6465(11) 0.2377(9) 0.5204(7) 0.075(4) Uani 1 1 d . . . O4 O 0.8196(10) 0.2314(9) 0.5387(8) 0.072(4) Uani 1 1 d . . . P1 P 0.5950(2) 0.3678(2) 0.23899(16) 0.0146(5) Uani 1 1 d . . . P2 P 0.9569(2) 0.40263(19) 0.22905(16) 0.0132(5) Uani 1 1 d . . . P3 P 0.9014(2) 0.2080(2) 0.00948(17) 0.0150(5) Uani 1 1 d . . . P4 P 0.7381(2) 0.7199(2) 0.05217(17) 0.0151(5) 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 0.0150(2) 0.01535(19) 0.01280(19) -0.00171(15) -0.00101(15) -0.00559(15) Au2 0.01314(19) 0.01174(18) 0.00887(17) -0.00141(13) 0.00005(14) -0.00401(14) Au3 0.01408(19) 0.01060(18) 0.01464(19) -0.00372(14) -0.00024(14) -0.00478(14) Au4 0.01265(19) 0.01078(18) 0.01415(19) -0.00349(14) -0.00020(14) -0.00286(14) C1 0.017(5) 0.016(5) 0.010(5) 0.002(4) 0.008(4) -0.005(4) C2 0.025(6) 0.021(5) 0.012(5) -0.002(4) -0.005(4) -0.009(4) C3 0.025(6) 0.032(7) 0.028(6) -0.010(5) -0.001(5) -0.019(5) C4 0.027(6) 0.011(5) 0.037(7) -0.003(5) -0.006(5) -0.001(5) C5 0.038(8) 0.022(6) 0.037(7) 0.001(5) -0.014(6) -0.004(5) C6 0.024(6) 0.032(7) 0.021(6) -0.004(5) -0.004(5) -0.006(5) C7 0.011(5) 0.024(5) 0.010(5) -0.002(4) 0.004(4) -0.007(4) C8 0.025(7) 0.050(8) 0.020(6) -0.011(6) -0.004(5) -0.010(6) C9 0.039(8) 0.032(7) 0.024(6) -0.012(6) 0.008(5) -0.007(6) C10 0.042(8) 0.016(6) 0.041(8) -0.008(6) 0.016(6) -0.011(6) C11 0.041(9) 0.034(8) 0.047(9) -0.001(7) -0.007(7) 0.006(6) C12 0.033(7) 0.029(6) 0.011(5) -0.002(5) 0.000(5) -0.002(5) C13 0.012(5) 0.024(6) 0.015(5) -0.004(4) -0.003(4) -0.003(4) C14 0.021(6) 0.014(5) 0.010(5) -0.002(4) -0.001(4) -0.002(4) C15 0.016(5) 0.011(5) 0.022(5) -0.010(4) 0.000(4) 0.000(4) C16 0.029(7) 0.030(6) 0.023(6) -0.007(5) -0.002(5) -0.009(5) C17 0.052(9) 0.033(7) 0.033(7) -0.011(6) -0.008(6) -0.020(6) C18 0.037(8) 0.035(7) 0.028(7) -0.018(6) -0.007(5) -0.001(6) C19 0.039(7) 0.034(7) 0.016(6) -0.013(5) 0.000(5) -0.010(6) C20 0.034(7) 0.024(6) 0.016(5) -0.003(5) -0.004(5) -0.010(5) C21 0.021(6) 0.017(5) 0.016(5) -0.007(4) -0.009(4) 0.007(4) C22 0.024(6) 0.022(6) 0.021(6) -0.007(5) -0.004(5) -0.005(5) C23 0.057(9) 0.012(5) 0.027(6) 0.002(5) -0.016(6) -0.004(6) C24 0.060(10) 0.016(6) 0.033(7) -0.009(5) -0.027(7) 0.012(6) C25 0.033(8) 0.053(9) 0.028(7) -0.021(6) -0.014(6) 0.030(7) C26 0.040(7) 0.021(6) 0.018(6) -0.005(5) -0.013(5) 0.009(5) C27 0.016(5) 0.019(5) 0.017(5) -0.005(4) -0.001(4) -0.007(4) C28 0.029(7) 0.025(6) 0.027(6) -0.015(5) -0.008(5) 0.007(5) C29 0.043(8) 0.021(6) 0.031(7) -0.014(5) -0.002(6) -0.007(5) C30 0.042(8) 0.040(7) 0.024(6) 0.002(5) -0.017(6) -0.026(6) C31 0.033(7) 0.017(6) 0.028(6) 0.009(5) -0.017(5) -0.013(5) C32 0.020(6) 0.010(5) 0.019(5) 0.004(4) -0.002(4) 0.001(4) C33 0.012(5) 0.025(6) 0.010(5) -0.004(4) 0.000(4) 0.001(4) C34 0.034(7) 0.022(6) 0.019(6) -0.006(5) -0.007(5) -0.011(5) C35 0.042(8) 0.041(8) 0.023(6) -0.005(6) -0.004(5) -0.021(6) C36 0.048(9) 0.031(7) 0.025(7) 0.007(5) -0.001(6) -0.020(6) C37 0.045(8) 0.018(6) 0.032(7) -0.007(5) -0.002(6) -0.021(5) C38 0.021(6) 0.014(5) 0.021(5) -0.005(4) -0.001(4) -0.008(4) C39 0.015(5) 0.009(5) 0.013(5) -0.001(4) 0.001(4) 0.002(4) C40 0.026(6) 0.007(5) 0.020(5) 0.000(4) -0.006(4) -0.005(4) C41 0.022(6) 0.019(5) 0.014(5) -0.008(4) -0.001(4) -0.012(4) C42 0.021(6) 0.038(7) 0.012(5) -0.006(5) 0.002(4) -0.004(5) C43 0.019(6) 0.026(6) 0.025(6) -0.007(5) 0.008(5) -0.002(5) C44 0.033(7) 0.032(7) 0.018(6) -0.005(5) 0.006(5) -0.016(5) C45 0.031(7) 0.035(7) 0.023(6) -0.003(5) -0.003(5) 0.012(6) C46 0.032(7) 0.028(6) 0.025(6) -0.006(5) -0.010(5) 0.006(5) C47 0.007(5) 0.021(5) 0.014(5) -0.004(4) 0.000(4) 0.003(4) C48 0.016(5) 0.031(6) 0.019(5) -0.010(5) 0.003(4) -0.014(5) C49 0.020(6) 0.039(7) 0.021(6) -0.011(5) -0.005(5) -0.010(5) C50 0.019(6) 0.030(6) 0.017(5) -0.002(5) -0.004(4) 0.002(5) C51 0.018(6) 0.024(6) 0.036(7) -0.009(5) -0.005(5) -0.004(5) C52 0.018(6) 0.017(5) 0.021(6) -0.002(4) -0.005(4) -0.002(4) C53 0.032(7) 0.038(7) 0.022(6) -0.002(5) -0.005(5) -0.012(6) Cl1 0.0234(14) 0.0311(15) 0.0135(12) -0.0044(11) -0.0052(10) -0.0033(11) Cl2 0.0356(17) 0.0230(14) 0.0219(14) -0.0054(11) -0.0008(12) -0.0031(12) Cl3 0.062(3) 0.043(2) 0.041(2) -0.0022(16) -0.0226(18) -0.0097(18) Cl4 0.041(2) 0.046(2) 0.0389(19) -0.0019(16) -0.0130(15) -0.0124(16) Cl5 0.043(2) 0.0437(19) 0.0377(19) -0.0122(15) -0.0002(15) -0.0151(16) O1 0.044(6) 0.043(5) 0.033(5) -0.020(4) -0.003(4) -0.003(4) O2 0.037(5) 0.036(5) 0.027(5) -0.009(4) 0.000(4) 0.000(4) O3 0.113(11) 0.070(8) 0.045(7) -0.027(6) -0.044(7) 0.058(8) O4 0.068(8) 0.078(8) 0.069(8) -0.047(7) 0.030(6) -0.036(7) P1 0.0136(13) 0.0148(13) 0.0123(12) 0.0004(10) -0.0005(10) -0.0061(10) P2 0.0141(13) 0.0135(12) 0.0106(12) -0.0023(10) -0.0009(10) -0.0037(10) P3 0.0139(13) 0.0133(12) 0.0184(13) -0.0052(10) -0.0025(10) -0.0044(10) P4 0.0143(13) 0.0128(12) 0.0179(13) -0.0036(10) -0.0023(10) -0.0049(10) _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 Cl1 2.313(2) . ? Au1 P1 2.245(3) . ? Au2 Au2 2.6192(7) 2_765 ? Au2 Au3 2.7887(5) 2_765 ? Au2 Au4 2.7989(6) 2_765 ? Au2 P2 2.276(2) . ? Au3 Au1 3.0522(6) . ? Au3 Au2 2.7887(5) 2_765 ? Au3 Au2 2.8403(5) . ? Au3 Au4 2.6205(6) . ? Au3 P3 2.297(3) . ? Au4 Au1 2.9738(6) . ? Au4 Au2 2.7989(5) 2_765 ? Au4 Au2 2.8144(6) . ? Au4 P4 2.294(3) . ? C1 C2 1.362(14) . ? C1 C6 1.404(15) . ? C2 C3 1.407(15) . ? C3 C4 1.355(16) . ? C4 C5 1.373(17) . ? C6 C5 1.391(16) . ? C7 C12 1.390(15) . ? C7 C8 1.388(15) . ? C8 C9 1.400(17) . ? C10 C11 1.38(2) . ? C10 C9 1.371(19) . ? C12 C11 1.364(18) . ? C14 C13 1.201(14) . ? C15 C16 1.370(15) . ? C15 C20 1.395(14) . ? C16 C17 1.376(16) . ? C18 C17 1.375(17) . ? C18 C19 1.396(17) . ? C20 C19 1.392(15) . ? C21 C22 1.389(15) . ? C21 C26 1.362(16) . ? C22 C23 1.384(16) . ? C23 C24 1.357(19) . ? C25 C24 1.375(19) . ? C26 C25 1.410(16) . ? C27 C28 1.382(15) . ? C28 C29 1.409(16) . ? C30 C29 1.350(18) . ? C30 C31 1.387(18) . ? C32 C27 1.385(14) . ? C32 C31 1.350(15) . ? C33 C34 1.400(14) . ? C33 C38 1.379(14) . ? C34 C35 1.355(15) . ? C35 C36 1.388(17) . ? C37 C36 1.370(17) . ? C38 C37 1.358(15) . ? C39 C40 1.204(14) 2_765 ? C40 C39 1.204(14) 2_765 ? C41 C42 1.360(15) . ? C41 C46 1.366(15) . ? C42 C43 1.376(15) . ? C44 C43 1.373(17) . ? C44 C45 1.367(17) . ? C46 C45 1.365(16) . ? C47 C48 1.386(14) . ? C47 C52 1.384(14) . ? C48 C49 1.379(16) . ? C50 C49 1.382(16) . ? C51 C50 1.362(15) . ? C52 C51 1.362(15) . ? Cl2 O1 1.435(9) . ? Cl2 O2 1.418(9) . ? Cl2 O3 1.426(10) . ? Cl2 O4 1.402(12) . ? Cl3 C53 1.753(13) . ? Cl4 C53 1.746(13) . ? Cl5 C53 1.756(12) . ? P1 C1 1.819(10) . ? P1 C13 1.746(10) . ? P1 C7 1.805(11) . ? P2 C14 1.758(11) . ? P2 C15 1.801(10) . ? P2 C21 1.819(10) . ? P3 C27 1.816(10) . ? P3 C33 1.819(10) . ? P3 C39 1.748(10) . ? P4 C40 1.768(11) . ? P4 C41 1.815(10) . ? P4 C47 1.803(10) . ? 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 Au2 Au2 Au3 61.275(16) 2_765 . ? Au2 Au2 Au3 63.274(16) 2_765 2_765 ? Au2 Au2 Au4 61.886(16) 2_765 . ? Au2 Au2 Au4 62.487(17) 2_765 2_765 ? Au2 Au3 Au1 109.853(16) . . ? Au2 Au3 Au1 122.060(17) 2_765 . ? Au2 Au3 Au2 55.451(15) 2_765 . ? Au2 Au4 Au1 112.874(17) . . ? Au2 Au4 Au1 124.594(17) 2_765 . ? Au2 Au4 Au2 55.627(16) 2_765 . ? Au3 Au2 Au3 124.549(15) 2_765 . ? Au3 Au2 Au4 55.938(13) 2_765 2_765 ? Au3 Au2 Au4 97.959(17) 2_765 . ? Au3 Au4 Au1 65.776(15) . . ? Au3 Au4 Au2 61.834(14) . 2_765 ? Au3 Au4 Au2 62.893(14) . . ? Au4 Au1 Au3 51.535(13) . . ? Au4 Au2 Au3 55.215(14) . . ? Au4 Au2 Au3 97.118(16) 2_765 . ? Au4 Au2 Au4 124.373(16) 2_765 . ? Au4 Au3 Au1 62.689(14) . . ? Au4 Au3 Au2 61.891(14) . . ? Au4 Au3 Au2 62.228(14) . 2_765 ? C1 C2 C3 120.0(10) . . ? C1 P1 Au1 114.9(3) . . ? C2 C1 C6 120.1(10) . . ? C2 C1 P1 119.8(8) . . ? C3 C4 C5 121.9(11) . . ? C4 C3 C2 119.3(10) . . ? C4 C5 C6 119.3(11) . . ? C5 C6 C1 119.4(11) . . ? C6 C1 P1 120.0(9) . . ? C7 C8 C9 119.6(12) . . ? C7 P1 Au1 116.0(3) . . ? C7 P1 C1 106.3(5) . . ? C8 C7 C12 119.9(10) . . ? C8 C7 P1 120.7(9) . . ? C9 C10 C11 119.7(12) . . ? C10 C9 C8 119.8(12) . . ? C11 C12 C7 119.4(11) . . ? C12 C11 C10 121.5(13) . . ? C12 C7 P1 119.3(8) . . ? C13 C14 P2 165.6(9) . . ? C13 P1 Au1 109.0(3) . . ? C13 P1 C1 104.0(5) . . ? C13 P1 C7 105.8(5) . . ? C14 C13 P1 166.8(9) . . ? C14 P2 Au2 103.8(3) . . ? C14 P2 C15 104.1(5) . . ? C14 P2 C21 104.7(5) . . ? C15 C16 C17 121.5(11) . . ? C15 P2 Au2 119.2(3) . . ? C15 P2 C21 109.2(5) . . ? C16 C15 C20 119.1(10) . . ? C16 C15 P2 119.6(8) . . ? C17 C18 C19 120.1(11) . . ? C18 C17 C16 119.8(12) . . ? C19 C20 C15 120.0(10) . . ? C20 C15 P2 121.2(8) . . ? C20 C19 C18 119.4(11) . . ? C21 C26 C25 119.4(11) . . ? C21 P2 Au2 114.0(3) . . ? C22 C21 P2 121.2(8) . . ? C23 C22 C21 119.3(11) . . ? C23 C24 C25 121.2(11) . . ? C24 C23 C22 120.2(11) . . ? C24 C25 C26 119.0(12) . . ? C26 C21 C22 120.8(10) . . ? C26 C21 P2 118.1(8) . . ? C27 C28 C29 118.5(11) . . ? C27 P3 Au3 117.6(4) . . ? C27 P3 C33 107.3(5) . . ? C28 C27 C32 120.0(10) . . ? C28 C27 P3 121.8(8) . . ? C29 C30 C31 121.0(11) . . ? C30 C29 C28 120.0(11) . . ? C31 C32 C27 121.0(11) . . ? C32 C27 P3 118.2(8) . . ? C32 C31 C30 119.4(11) . . ? C33 P3 Au3 115.9(3) . . ? C34 C33 P3 117.2(8) . . ? C34 C35 C36 120.4(11) . . ? C35 C34 C33 119.0(10) . . ? C37 C36 C35 120.2(11) . . ? C37 C38 C33 120.1(10) . . ? C38 C33 C34 120.1(10) . . ? C38 C33 P3 122.7(8) . . ? C38 C37 C36 120.1(11) . . ? C39 C40 P4 160.5(9) 2_765 . ? C39 P3 Au3 103.7(3) . . ? C39 P3 C27 105.9(5) . . ? C39 P3 C33 105.2(5) . . ? C40 C39 P3 162.3(9) 2_765 . ? C40 P4 Au4 104.0(4) . . ? C40 P4 C41 103.6(5) . . ? C40 P4 C47 107.0(5) . . ? C41 C42 C43 120.5(11) . . ? C41 P4 Au4 114.3(4) . . ? C42 C41 C46 119.4(10) . . ? C42 C41 P4 121.9(8) . . ? C44 C43 C42 120.2(11) . . ? C45 C44 C43 118.6(11) . . ? C45 C46 C41 120.1(11) . . ? C46 C41 P4 118.6(9) . . ? C46 C45 C44 121.1(12) . . ? C47 P4 Au4 119.4(3) . . ? C47 P4 C41 107.0(5) . . ? C48 C47 P4 117.4(8) . . ? C48 C49 C50 120.4(10) . . ? C49 C48 C47 119.5(10) . . ? C51 C50 C49 118.9(10) . . ? C51 C52 C47 119.0(10) . . ? C52 C47 C48 120.0(10) . . ? C52 C47 P4 122.6(8) . . ? C52 C51 C50 122.3(11) . . ? Cl1 Au1 Au3 74.92(7) . . ? Cl1 Au1 Au4 78.68(7) . . ? Cl3 C53 Cl5 110.7(7) . . ? Cl4 C53 Cl3 109.9(7) . . ? Cl4 C53 Cl5 111.0(7) . . ? O2 Cl2 O1 109.6(5) . . ? O2 Cl2 O3 109.2(6) . . ? O3 Cl2 O1 109.8(6) . . ? O4 Cl2 O1 111.7(6) . . ? O4 Cl2 O2 109.2(7) . . ? O4 Cl2 O3 107.3(8) . . ? P1 Au1 Au3 105.71(7) . . ? P1 Au1 Au4 103.83(7) . . ? P1 Au1 Cl1 177.26(10) . . ? P2 Au2 Au2 170.11(7) . 2_765 ? P2 Au2 Au3 109.47(7) . . ? P2 Au2 Au3 125.86(7) . 2_765 ? P2 Au2 Au4 110.60(7) . . ? P2 Au2 Au4 124.61(7) . 2_765 ? P3 Au3 Au1 113.33(7) . . ? P3 Au3 Au2 120.95(7) . . ? P3 Au3 Au2 121.50(7) . 2_765 ? P3 Au3 Au4 176.02(7) . . ? P4 Au4 Au1 109.75(7) . . ? P4 Au4 Au2 118.96(7) . . ? P4 Au4 Au2 122.95(7) . 2_765 ? P4 Au4 Au3 175.21(7) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 4.114 _refine_diff_density_min -1.551 _refine_diff_density_rms 0.344 #===END data_compound_1_4 _database_code_depnum_ccdc_archive 'CCDC 843625' #TrackingRef '- all-in-one.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C104 H80 Au4 P8, 4(F6 P), 4.5(C H2 Cl2)' _chemical_formula_sum 'C108.50 H89 Au4 Cl9 F24 P12' _chemical_formula_weight 3327.35 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' 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 tetragonal _symmetry_space_group_name_H-M P4/ncc _symmetry_space_group_name_Hall -P4a2ac loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' '-y-1/2, -x-1/2, z-1/2' 'y, x, z-1/2' _cell_length_a 19.2584(2) _cell_length_b 19.2584(2) _cell_length_c 32.3309(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11991.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7634 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 24.66 _exptl_crystal_description piece _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.843 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6420 _exptl_absorpt_coefficient_mu 5.323 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4615 _exptl_absorpt_correction_T_max 0.5676 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49276 _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5283 _reflns_number_gt 3711 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP32 (Farugia)' _computing_publication_material 'Ciftab (Sheldrick)' _refine_special_details ; The asymmetric unit consists of 1/4 of a cyclo-tetrameric Au-complex tetra-cation and one PF6-anion. The latter occupies three different sites (with s.o.f. 0.5, 0.25, 0.25). One of them is heavily disordered (with alternative site occupancy by the anion or solvent, i.e., dichloromethane), and therefore four out of sixteen PF6-anions per unit cell as well as the solvent of crystallization could not be refined. Thus, the data set was treated with SQUEEZE as implemented in WinGX PLATON for the final stages of the refinement. The SQUEEZE procedure yielded 1023 electrons per unit cell, which correspond nicely to the omitted PF6-anions (276 electrons) plus 18 dichloromethane molecules (756 electrons) = 1032 electrons. Thus, these moieties were included in the sum formula for calculation of F(000), M, density and absorption coefficient. The cationic moiety suffers disorder. Two of the four phenyl groups of the asymmetric unit were refined disordered over two positions each, with site occupancies of 0.5 and 0.5 for one and 0.64 and 0.36 for the other phenyl group. The similar separations of neighboring P-atoms (4.57 A and 4.70 A) gives rise to an additional disorder, which is the alternative site occupancy of the idealized P-P-line by an Au-atom or an acetylenic CC moiety, thus relating the alternative part to the predominant part by a 1/8 rotation of the [P-Au-P-CC-]4 cycle in combination with a mirror parallel to the crystallographic a-b-plane. Site occupancies for this disorder are 0.90 and 0.10. 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^)+(0.1000P)^2^+4.0000P] 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 5283 _refine_ls_number_parameters 275 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0703 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1586 _refine_ls_wR_factor_gt 0.1484 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.004 _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 P3 P 0.2500 0.2500 0.10784(11) 0.0382(9) Uani 1 4 d S . . F1 F 0.2500 0.2500 0.0583(3) 0.075(3) Uani 1 4 d S . . F2 F 0.2403(3) 0.1681(3) 0.10755(15) 0.0802(16) Uani 1 1 d . . . F3 F 0.2500 0.2500 0.1565(3) 0.076(3) Uani 1 4 d S . . P4 P 0.91274(17) 0.08726(17) 0.2500 0.0731(10) Uani 1 2 d S . . F4 F 0.9597(3) 0.1328(3) 0.21969(19) 0.0945(19) Uani 1 1 d . . . F5 F 0.9778(3) 0.0702(5) 0.2779(2) 0.146(3) Uani 1 1 d . . . F6 F 0.8959(4) 0.1525(3) 0.2767(2) 0.113(2) Uani 1 1 d . . . P1 P -0.01681(11) 0.31073(11) 0.32499(7) 0.0422(5) Uani 1 1 d D . . P2 P 0.01550(11) 0.10748(10) 0.39554(6) 0.0397(5) Uani 1 1 d D . . Au1 Au -0.000099(18) 0.208486(17) 0.359004(10) 0.03899(17) Uani 0.8984(16) 1 d PD A 1 C25 C 0.0737(6) 0.0592(7) 0.3685(4) 0.057(2) Uani 0.8984(16) 1 d PD A 1 C26 C 0.1199(6) 0.0266(7) 0.3503(4) 0.057(2) Uani 0.8984(16) 1 d PD A 1 Au1A Au 0.1007(3) 0.0388(2) 0.36549(15) 0.057(2) Uani 0.1016(16) 1 d PD A 2 C25A C 0.003(3) 0.1878(8) 0.3751(3) 0.03899(17) Uani 0.1016(16) 1 d PD A 2 C26A C -0.0173(13) 0.2365(16) 0.3534(15) 0.03899(17) Uani 0.1016(16) 1 d PD A 2 C1 C -0.1038(3) 0.3445(6) 0.3175(3) 0.049(3) Uani 0.50 1 d PGD A 1 C2 C -0.1317(5) 0.3818(6) 0.3503(3) 0.049(3) Uani 0.50 1 d PG A 1 H2 H -0.1039 0.3919 0.3738 0.059 Uiso 0.50 1 calc PR A 1 C3 C -0.2002(5) 0.4044(7) 0.3487(3) 0.080(4) Uani 0.50 1 d PG A 1 H3 H -0.2192 0.4300 0.3711 0.096 Uiso 0.50 1 calc PR A 1 C4 C -0.2408(3) 0.3897(7) 0.3143(4) 0.080(4) Uani 0.50 1 d PG A 1 H4 H -0.2876 0.4051 0.3132 0.096 Uiso 0.50 1 calc PR A 1 C5 C -0.2129(4) 0.3523(7) 0.2815(3) 0.080(4) Uani 0.50 1 d PG A 1 H5 H -0.2407 0.3422 0.2579 0.096 Uiso 0.50 1 calc PR A 1 C6 C -0.1444(5) 0.3297(6) 0.2831(3) 0.049(3) Uani 0.50 1 d PG A 1 H6 H -0.1254 0.3041 0.2606 0.059 Uiso 0.50 1 calc PR A 1 C1A C -0.1087(3) 0.3301(5) 0.3289(3) 0.044(2) Uani 0.50 1 d PGD A 2 C2A C -0.1304(4) 0.3989(4) 0.3270(3) 0.044(2) Uani 0.50 1 d PG A 2 H2A H -0.0973 0.4349 0.3232 0.053 Uiso 0.50 1 calc PR A 2 C3A C -0.2004(4) 0.4150(4) 0.3307(3) 0.053(3) Uani 0.50 1 d PG A 2 H3A H -0.2152 0.4620 0.3294 0.064 Uiso 0.50 1 calc PR A 2 C4A C -0.2489(3) 0.3624(6) 0.3363(3) 0.053(3) Uani 0.50 1 d PG A 2 H4A H -0.2968 0.3734 0.3389 0.064 Uiso 0.50 1 calc PR A 2 C5A C -0.2272(4) 0.2936(5) 0.3383(3) 0.053(3) Uani 0.50 1 d PG . 2 H5A H -0.2604 0.2576 0.3421 0.064 Uiso 0.50 1 calc PR A 2 C6A C -0.1572(4) 0.2775(4) 0.3346(3) 0.044(2) Uani 0.50 1 d PG A 2 H6A H -0.1424 0.2305 0.3359 0.053 Uiso 0.50 1 calc PR A 2 C7 C 0.0199(5) 0.3118(4) 0.2753(2) 0.050(2) Uani 1 1 d . . . C8 C 0.0467(5) 0.2541(6) 0.2575(3) 0.069(3) Uani 1 1 d . . . H8 H 0.0429 0.2109 0.2716 0.083 Uiso 1 1 calc R A . C9 C 0.0807(6) 0.2562(6) 0.2180(3) 0.088(3) Uani 1 1 d . . . H9 H 0.0997 0.2154 0.2060 0.105 Uiso 1 1 calc R . . C10 C 0.0848(8) 0.3175(6) 0.1984(3) 0.099(4) Uani 1 1 d . . . H10 H 0.1018 0.3192 0.1708 0.119 Uiso 1 1 calc R A . C11 C 0.0656(7) 0.3756(6) 0.2170(3) 0.093(4) Uani 1 1 d . . . H11 H 0.0756 0.4188 0.2041 0.112 Uiso 1 1 calc R . . C12 C 0.0321(6) 0.3752(5) 0.2537(3) 0.071(3) Uani 1 1 d . . . H12 H 0.0165 0.4178 0.2652 0.085 Uiso 1 1 calc R A . C13 C -0.0636(4) 0.0558(4) 0.4004(2) 0.0376(17) Uani 1 1 d . . . C14 C -0.0757(6) -0.0040(5) 0.3797(3) 0.077(3) Uani 1 1 d . . . H14 H -0.0400 -0.0233 0.3631 0.092 Uiso 1 1 calc R A . C15 C -0.1391(6) -0.0377(6) 0.3823(3) 0.072(3) Uani 1 1 d . . . H15 H -0.1468 -0.0788 0.3667 0.086 Uiso 1 1 calc R . . C16 C -0.1878(6) -0.0136(5) 0.4058(3) 0.064(3) Uani 1 1 d . . . H16 H -0.2295 -0.0393 0.4090 0.076 Uiso 1 1 calc R A . C17 C -0.1802(6) 0.0507(7) 0.4269(4) 0.112(5) Uani 1 1 d . . . H17 H -0.2170 0.0693 0.4430 0.134 Uiso 1 1 calc R . . C18 C -0.1180(5) 0.0850(5) 0.4233(3) 0.071(3) Uani 1 1 d . . . H18 H -0.1119 0.1287 0.4364 0.085 Uiso 1 1 calc R A . C19 C 0.0551(7) 0.1191(7) 0.4451(2) 0.039(2) Uani 0.64(3) 1 d PGD A 1 C20 C 0.0734(10) 0.0616(6) 0.4686(3) 0.070(3) Uani 0.64(3) 1 d PG A 1 H20 H 0.0661 0.0161 0.4580 0.083 Uiso 0.64(3) 1 calc PR A 1 C21 C 0.1024(10) 0.0704(6) 0.5076(3) 0.070(3) Uani 0.64(3) 1 d PG A 1 H21 H 0.1149 0.0311 0.5237 0.083 Uiso 0.64(3) 1 calc PR A 1 C22 C 0.1131(6) 0.1369(7) 0.5231(2) 0.070(3) Uani 0.64(3) 1 d PG A 1 H22 H 0.1329 0.1430 0.5498 0.083 Uiso 0.64(3) 1 calc PR A 1 C23 C 0.0948(8) 0.1945(6) 0.4996(3) 0.070(3) Uani 0.64(3) 1 d PG A 1 H23 H 0.1022 0.2399 0.5102 0.083 Uiso 0.64(3) 1 calc PR A 1 C24 C 0.0658(9) 0.1856(6) 0.4606(3) 0.070(3) Uani 0.64(3) 1 d PG A 1 H24 H 0.0533 0.2250 0.4445 0.083 Uiso 0.64(3) 1 calc PR A 1 C19A C 0.0450(13) 0.1259(11) 0.4468(3) 0.039(2) Uani 0.36(3) 1 d PGD A 2 C20A C 0.0373(16) 0.0773(11) 0.4783(6) 0.064(6) Uani 0.36(3) 1 d PG A 2 H20A H 0.0120 0.0357 0.4734 0.077 Uiso 0.36(3) 1 calc PR A 2 C21A C 0.0666(16) 0.0895(13) 0.5169(5) 0.064(6) Uani 0.36(3) 1 d PG A 2 H21A H 0.0613 0.0563 0.5384 0.077 Uiso 0.36(3) 1 calc PR A 2 C22A C 0.1035(10) 0.1504(11) 0.5241(3) 0.064(6) Uani 0.36(3) 1 d PG A 2 H22A H 0.1235 0.1587 0.5505 0.077 Uiso 0.36(3) 1 calc PR A 2 C23A C 0.1112(12) 0.1989(9) 0.4926(5) 0.064(6) Uani 0.36(3) 1 d PG A 2 H23A H 0.1365 0.2405 0.4975 0.077 Uiso 0.36(3) 1 calc PR A 2 C24A C 0.0820(15) 0.1867(11) 0.4540(4) 0.064(6) Uani 0.36(3) 1 d PG A 2 H24A H 0.0872 0.2199 0.4325 0.077 Uiso 0.36(3) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P3 0.0417(14) 0.0417(14) 0.031(2) 0.000 0.000 0.000 F1 0.091(5) 0.091(5) 0.044(6) 0.000 0.000 0.000 F2 0.120(5) 0.042(3) 0.079(4) 0.001(2) -0.004(3) -0.011(3) F3 0.093(5) 0.093(5) 0.040(5) 0.000 0.000 0.000 P4 0.0720(16) 0.0720(16) 0.075(2) 0.0072(13) 0.0072(13) -0.021(2) F4 0.092(5) 0.097(5) 0.094(4) 0.017(4) 0.030(4) -0.025(4) F5 0.058(4) 0.259(10) 0.120(6) 0.081(6) 0.013(4) 0.016(5) F6 0.102(5) 0.096(5) 0.140(6) -0.035(4) 0.060(4) -0.032(4) P1 0.0434(12) 0.0407(11) 0.0424(11) 0.0021(9) -0.0050(9) 0.0017(9) P2 0.0476(12) 0.0410(11) 0.0306(10) -0.0012(8) 0.0026(8) 0.0013(9) Au1 0.0433(2) 0.0388(2) 0.0349(2) 0.00202(14) 0.00481(14) 0.00489(15) C25 0.070(5) 0.059(4) 0.043(2) 0.008(2) -0.010(3) -0.005(3) C26 0.070(5) 0.059(4) 0.043(2) 0.008(2) -0.010(3) -0.005(3) Au1A 0.070(5) 0.059(4) 0.043(2) 0.008(2) -0.010(3) -0.005(3) C25A 0.0433(2) 0.0388(2) 0.0349(2) 0.00202(14) 0.00481(14) 0.00489(15) C26A 0.0433(2) 0.0388(2) 0.0349(2) 0.00202(14) 0.00481(14) 0.00489(15) C1 0.041(6) 0.061(7) 0.045(5) 0.008(5) -0.001(4) -0.008(5) C2 0.041(6) 0.061(7) 0.045(5) 0.008(5) -0.001(4) -0.008(5) C3 0.061(8) 0.095(10) 0.084(10) 0.002(7) -0.004(6) -0.003(7) C4 0.061(8) 0.095(10) 0.084(10) 0.002(7) -0.004(6) -0.003(7) C5 0.061(8) 0.095(10) 0.084(10) 0.002(7) -0.004(6) -0.003(7) C6 0.041(6) 0.061(7) 0.045(5) 0.008(5) -0.001(4) -0.008(5) C1A 0.042(5) 0.038(5) 0.053(6) 0.000(5) -0.003(4) -0.002(4) C2A 0.042(5) 0.038(5) 0.053(6) 0.000(5) -0.003(4) -0.002(4) C3A 0.039(6) 0.082(8) 0.038(5) -0.009(5) 0.005(4) 0.013(5) C4A 0.039(6) 0.082(8) 0.038(5) -0.009(5) 0.005(4) 0.013(5) C5A 0.039(6) 0.082(8) 0.038(5) -0.009(5) 0.005(4) 0.013(5) C6A 0.042(5) 0.038(5) 0.053(6) 0.000(5) -0.003(4) -0.002(4) C7 0.059(5) 0.044(5) 0.046(5) -0.012(4) -0.024(4) 0.008(4) C8 0.089(7) 0.062(6) 0.057(5) 0.000(5) 0.006(5) -0.007(6) C9 0.130(10) 0.088(8) 0.046(6) -0.028(6) 0.022(6) -0.010(8) C10 0.187(13) 0.061(7) 0.048(6) -0.031(5) 0.019(7) -0.034(8) C11 0.155(12) 0.073(7) 0.051(6) 0.014(5) -0.008(7) -0.011(7) C12 0.122(9) 0.058(6) 0.034(5) -0.004(4) 0.002(5) 0.002(6) C13 0.045(4) 0.035(4) 0.033(4) 0.005(3) 0.004(3) 0.000(3) C14 0.083(8) 0.089(8) 0.058(6) -0.016(5) 0.030(5) -0.035(6) C15 0.086(8) 0.088(8) 0.041(5) -0.016(5) -0.003(5) -0.027(6) C16 0.076(7) 0.068(6) 0.047(5) -0.002(5) -0.004(5) -0.027(5) C17 0.080(8) 0.117(11) 0.139(12) -0.035(9) 0.054(8) -0.027(8) C18 0.066(6) 0.070(6) 0.077(7) -0.005(5) 0.016(5) -0.004(5) C19 0.039(6) 0.041(5) 0.039(4) 0.008(4) 0.004(4) 0.016(4) C20 0.102(8) 0.064(5) 0.043(4) -0.001(4) -0.009(5) -0.005(5) C21 0.102(8) 0.064(5) 0.043(4) -0.001(4) -0.009(5) -0.005(5) C22 0.102(8) 0.064(5) 0.043(4) -0.001(4) -0.009(5) -0.005(5) C23 0.102(8) 0.064(5) 0.043(4) -0.001(4) -0.009(5) -0.005(5) C24 0.102(8) 0.064(5) 0.043(4) -0.001(4) -0.009(5) -0.005(5) C19A 0.039(6) 0.041(5) 0.039(4) 0.008(4) 0.004(4) 0.016(4) C20A 0.086(12) 0.052(9) 0.056(8) 0.008(6) -0.029(8) -0.026(7) C21A 0.086(12) 0.052(9) 0.056(8) 0.008(6) -0.029(8) -0.026(7) C22A 0.086(12) 0.052(9) 0.056(8) 0.008(6) -0.029(8) -0.026(7) C23A 0.086(12) 0.052(9) 0.056(8) 0.008(6) -0.029(8) -0.026(7) C24A 0.086(12) 0.052(9) 0.056(8) 0.008(6) -0.029(8) -0.026(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 P3 F3 1.573(10) . ? P3 F2 1.589(5) 3 ? P3 F2 1.589(5) . ? P3 F2 1.589(5) 2 ? P3 F2 1.589(5) 4 ? P3 F1 1.601(10) . ? P4 F6 1.560(7) 8_665 ? P4 F6 1.560(7) . ? P4 F5 1.579(7) . ? P4 F5 1.579(7) 8_665 ? P4 F4 1.595(5) . ? P4 F4 1.595(5) 8_665 ? P1 C26A 1.698(9) . ? P1 C7 1.756(9) . ? P1 C26 1.775(9) 4 ? P1 C1 1.813(5) . ? P1 C1A 1.814(5) . ? P1 Au1 2.278(2) . ? P1 Au1A 2.403(5) 4 ? P2 C25 1.698(9) . ? P2 C25A 1.698(9) . ? P2 C19 1.788(4) . ? P2 C19A 1.788(4) . ? P2 C13 1.826(7) . ? P2 Au1 2.295(2) . ? P2 Au1A 2.320(5) . ? C25 C26 1.239(16) . ? C26 P1 1.775(9) 3 ? Au1A P1 2.403(5) 3 ? C25A C26A 1.239(16) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C2 H2 0.9500 . ? C3 C4 1.3900 . ? C3 H3 0.9500 . ? C4 C5 1.3900 . ? C4 H4 0.9500 . ? C5 C6 1.3900 . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C1A C2A 1.3900 . ? C1A C6A 1.3900 . ? C2A C3A 1.3900 . ? C2A H2A 0.9500 . ? C3A C4A 1.3900 . ? C3A H3A 0.9500 . ? C4A C5A 1.3900 . ? C4A H4A 0.9500 . ? C5A C6A 1.3900 . ? C5A H5A 0.9500 . ? C6A H6A 0.9500 . ? C7 C8 1.354(12) . ? C7 C12 1.427(13) . ? C8 C9 1.437(13) . ? C8 H8 0.9500 . ? C9 C10 1.341(15) . ? C9 H9 0.9500 . ? C10 C11 1.323(14) . ? C10 H10 0.9500 . ? C11 C12 1.349(14) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.352(11) . ? C13 C18 1.401(11) . ? C14 C15 1.385(13) . ? C14 H14 0.9500 . ? C15 C16 1.293(14) . ? C15 H15 0.9500 . ? C16 C17 1.421(15) . ? C16 H16 0.9500 . ? C17 C18 1.372(14) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.3900 . ? C19 C24 1.3900 . ? C20 C21 1.3900 . ? C20 H20 0.9500 . ? C21 C22 1.3900 . ? C21 H21 0.9500 . ? C22 C23 1.3900 . ? C22 H22 0.9500 . ? C23 C24 1.3900 . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C19A C20A 1.3900 . ? C19A C24A 1.3900 . ? C20A C21A 1.3900 . ? C20A H20A 0.9500 . ? C21A C22A 1.3900 . ? C21A H21A 0.9500 . ? C22A C23A 1.3900 . ? C22A H22A 0.9500 . ? C23A C24A 1.3900 . ? C23A H23A 0.9500 . ? C24A H24A 0.9500 . ? 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 F3 P3 F2 90.3(2) . 3 ? F3 P3 F2 90.3(2) . . ? F2 P3 F2 89.998(3) 3 . ? F3 P3 F2 90.3(2) . 2 ? F2 P3 F2 89.998(3) 3 2 ? F2 P3 F2 179.3(4) . 2 ? F3 P3 F2 90.3(2) . 4 ? F2 P3 F2 179.3(4) 3 4 ? F2 P3 F2 89.998(3) . 4 ? F2 P3 F2 89.998(3) 2 4 ? F3 P3 F1 180.000(1) . . ? F2 P3 F1 89.7(2) 3 . ? F2 P3 F1 89.7(2) . . ? F2 P3 F1 89.7(2) 2 . ? F2 P3 F1 89.7(2) 4 . ? F6 P4 F6 88.3(7) 8_665 . ? F6 P4 F5 178.8(4) 8_665 . ? F6 P4 F5 91.0(5) . . ? F6 P4 F5 91.0(5) 8_665 8_665 ? F6 P4 F5 178.8(4) . 8_665 ? F5 P4 F5 89.8(8) . 8_665 ? F6 P4 F4 90.1(4) 8_665 . ? F6 P4 F4 90.9(3) . . ? F5 P4 F4 90.9(4) . . ? F5 P4 F4 88.1(4) 8_665 . ? F6 P4 F4 90.9(3) 8_665 8_665 ? F6 P4 F4 90.1(4) . 8_665 ? F5 P4 F4 88.1(4) . 8_665 ? F5 P4 F4 90.9(4) 8_665 8_665 ? F4 P4 F4 178.6(6) . 8_665 ? C26A P1 C7 120.4(14) . . ? C26A P1 C26 113(2) . 4 ? C7 P1 C26 102.9(5) . 4 ? C26A P1 C1 111.6(8) . . ? C7 P1 C1 104.2(4) . . ? C26 P1 C1 103.1(6) 4 . ? C26A P1 C1A 97.4(7) . . ? C7 P1 C1A 117.1(5) . . ? C26 P1 C1A 105.8(6) 4 . ? C7 P1 Au1 113.3(3) . . ? C26 P1 Au1 111.2(5) 4 . ? C1 P1 Au1 120.3(4) . . ? C1A P1 Au1 106.4(3) . . ? C26A P1 Au1A 108(2) . 4 ? C7 P1 Au1A 108.1(3) . 4 ? C1 P1 Au1A 103.3(4) . 4 ? C1A P1 Au1A 104.5(3) . 4 ? Au1 P1 Au1A 106.73(14) . 4 ? C25 P2 C25A 112.9(13) . . ? C25 P2 C19 104.4(7) . . ? C25A P2 C19 107.0(10) . . ? C25 P2 C19A 112.1(10) . . ? C25A P2 C19A 102.9(10) . . ? C25 P2 C13 107.3(6) . . ? C25A P2 C13 115(2) . . ? C19 P2 C13 110.3(5) . . ? C19A P2 C13 107.1(8) . . ? C25 P2 Au1 106.6(5) . . ? C19 P2 Au1 114.2(5) . . ? C19A P2 Au1 110.5(7) . . ? C13 P2 Au1 113.4(2) . . ? C25A P2 Au1A 117.0(14) . . ? C19 P2 Au1A 98.3(5) . . ? C19A P2 Au1A 106.1(9) . . ? C13 P2 Au1A 108.4(3) . . ? Au1 P2 Au1A 111.11(13) . . ? P1 Au1 P2 177.85(7) . . ? C26 C25 P2 175.3(16) . . ? C25 C26 P1 177.0(16) . 3 ? P2 Au1A P1 169.8(2) . 3 ? C26A C25A P2 163(2) . . ? C25A C26A P1 160.4(19) . . ? C2 C1 C6 120.0 . . ? C2 C1 P1 116.1(6) . . ? C6 C1 P1 123.6(6) . . ? C1 C2 C3 120.0 . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? C2A C1A C6A 120.0 . . ? C2A C1A P1 119.1(5) . . ? C6A C1A P1 120.9(5) . . ? C3A C2A C1A 120.0 . . ? C3A C2A H2A 120.0 . . ? C1A C2A H2A 120.0 . . ? C4A C3A C2A 120.0 . . ? C4A C3A H3A 120.0 . . ? C2A C3A H3A 120.0 . . ? C5A C4A C3A 120.0 . . ? C5A C4A H4A 120.0 . . ? C3A C4A H4A 120.0 . . ? C4A C5A C6A 120.0 . . ? C4A C5A H5A 120.0 . . ? C6A C5A H5A 120.0 . . ? C5A C6A C1A 120.0 . . ? C5A C6A H6A 120.0 . . ? C1A C6A H6A 120.0 . . ? C8 C7 C12 115.6(9) . . ? C8 C7 P1 122.2(7) . . ? C12 C7 P1 121.7(6) . . ? C7 C8 C9 121.8(10) . . ? C7 C8 H8 119.1 . . ? C9 C8 H8 119.1 . . ? C10 C9 C8 118.2(10) . . ? C10 C9 H9 120.9 . . ? C8 C9 H9 120.9 . . ? C11 C10 C9 120.9(10) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C12 121.9(10) . . ? C10 C11 H11 119.1 . . ? C12 C11 H11 119.1 . . ? C11 C12 C7 120.9(9) . . ? C11 C12 H12 119.5 . . ? C7 C12 H12 119.5 . . ? C14 C13 C18 118.3(8) . . ? C14 C13 P2 124.4(6) . . ? C18 C13 P2 116.8(6) . . ? C13 C14 C15 121.5(9) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C16 C15 C14 120.3(9) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 121.4(9) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C18 C17 C16 117.9(10) . . ? C18 C17 H17 121.0 . . ? C16 C17 H17 121.0 . . ? C17 C18 C13 120.3(10) . . ? C17 C18 H18 119.9 . . ? C13 C18 H18 119.9 . . ? C20 C19 C24 120.0 . . ? C20 C19 P2 119.9(7) . . ? C24 C19 P2 120.1(7) . . ? C19 C20 C21 120.0 . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C22 C21 C20 120.0 . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.0 . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C19 120.0 . . ? C23 C24 H24 120.0 . . ? C19 C24 H24 120.0 . . ? C20A C19A C24A 120.0 . . ? C20A C19A P2 120.8(12) . . ? C24A C19A P2 118.9(12) . . ? C21A C20A C19A 120.0 . . ? C21A C20A H20A 120.0 . . ? C19A C20A H20A 120.0 . . ? C20A C21A C22A 120.0 . . ? C20A C21A H21A 120.0 . . ? C22A C21A H21A 120.0 . . ? C23A C22A C21A 120.0 . . ? C23A C22A H22A 120.0 . . ? C21A C22A H22A 120.0 . . ? C24A C23A C22A 120.0 . . ? C24A C23A H23A 120.0 . . ? C22A C23A H23A 120.0 . . ? C23A C24A C19A 120.0 . . ? C23A C24A H24A 120.0 . . ? C19A C24A H24A 120.0 . . ? 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 C19 P2 Au1A P1 -124.2(14) . . . 3 ? C19A P2 Au1A P1 -124.3(14) . . . 3 ? C13 P2 Au1A P1 121.0(13) . . . 3 ? Au1 P2 Au1A P1 -4.2(14) . . . 3 ? C25 P2 C25A C26A 82(14) . . . . ? C19 P2 C25A C26A -164(13) . . . . ? C19A P2 C25A C26A -157(13) . . . . ? C13 P2 C25A C26A -41(14) . . . . ? Au1 P2 C25A C26A 42(2) . . . . ? Au1A P2 C25A C26A 87(14) . . . . ? P2 C25A C26A P1 -140(6) . . . . ? C7 P1 C26A C25A 74(14) . . . . ? C26 P1 C26A C25A -47(13) 4 . . . ? C1 P1 C26A C25A -163(12) . . . . ? C1A P1 C26A C25A -158(12) . . . . ? Au1 P1 C26A C25A 34.4(11) . . . . ? Au1A P1 C26A C25A -50(13) 4 . . . ? C26A P1 C1 C2 80(2) . . . . ? C7 P1 C1 C2 -148.2(6) . . . . ? C26 P1 C1 C2 -41.1(8) 4 . . . ? C1A P1 C1 C2 61.1(19) . . . . ? Au1 P1 C1 C2 83.4(6) . . . . ? Au1A P1 C1 C2 -35.3(6) 4 . . . ? C26A P1 C1 C6 -94(2) . . . . ? C7 P1 C1 C6 37.6(8) . . . . ? C26 P1 C1 C6 144.7(8) 4 . . . ? C1A P1 C1 C6 -113(2) . . . . ? Au1 P1 C1 C6 -90.8(7) . . . . ? Au1A P1 C1 C6 150.5(6) 4 . . . ? C6 C1 C2 C3 0.0 . . . . ? P1 C1 C2 C3 -174.4(8) . . . . ? C1 C2 C3 C4 0.0 . . . . ? C2 C3 C4 C5 0.0 . . . . ? C3 C4 C5 C6 0.0 . . . . ? C4 C5 C6 C1 0.0 . . . . ? C2 C1 C6 C5 0.0 . . . . ? P1 C1 C6 C5 174.0(9) . . . . ? C26A P1 C1A C2A 151(2) . . . . ? C7 P1 C1A C2A -78.7(7) . . . . ? C26 P1 C1A C2A 35.2(7) 4 . . . ? C1 P1 C1A C2A -46.5(18) . . . . ? Au1 P1 C1A C2A 153.5(5) . . . . ? Au1A P1 C1A C2A 40.8(6) 4 . . . ? C26A P1 C1A C6A -27(2) . . . . ? C7 P1 C1A C6A 102.4(6) . . . . ? C26 P1 C1A C6A -143.7(7) 4 . . . ? C1 P1 C1A C6A 135(2) . . . . ? Au1 P1 C1A C6A -25.3(6) . . . . ? Au1A P1 C1A C6A -138.0(5) 4 . . . ? C6A C1A C2A C3A 0.0 . . . . ? P1 C1A C2A C3A -178.9(8) . . . . ? C1A C2A C3A C4A 0.0 . . . . ? C2A C3A C4A C5A 0.0 . . . . ? C3A C4A C5A C6A 0.0 . . . . ? C4A C5A C6A C1A 0.0 . . . . ? C2A C1A C6A C5A 0.0 . . . . ? P1 C1A C6A C5A 178.8(8) . . . . ? C26A P1 C7 C8 2(2) . . . . ? C26 P1 C7 C8 128.6(9) 4 . . . ? C1 P1 C7 C8 -124.0(8) . . . . ? C1A P1 C7 C8 -115.9(8) . . . . ? Au1 P1 C7 C8 8.5(8) . . . . ? Au1A P1 C7 C8 126.5(7) 4 . . . ? C26A P1 C7 C12 -169(2) . . . . ? C26 P1 C7 C12 -42.3(9) 4 . . . ? C1 P1 C7 C12 65.0(9) . . . . ? C1A P1 C7 C12 73.2(9) . . . . ? Au1 P1 C7 C12 -162.5(7) . . . . ? Au1A P1 C7 C12 -44.4(8) 4 . . . ? C12 C7 C8 C9 -4.4(14) . . . . ? P1 C7 C8 C9 -175.8(8) . . . . ? C7 C8 C9 C10 -0.7(16) . . . . ? C8 C9 C10 C11 8(2) . . . . ? C9 C10 C11 C12 -10(2) . . . . ? C10 C11 C12 C7 4.0(19) . . . . ? C8 C7 C12 C11 2.9(15) . . . . ? P1 C7 C12 C11 174.4(9) . . . . ? C25 P2 C13 C14 -10.4(9) . . . . ? C25A P2 C13 C14 115.8(9) . . . . ? C19 P2 C13 C14 -123.5(9) . . . . ? C19A P2 C13 C14 -130.9(11) . . . . ? Au1 P2 C13 C14 107.0(8) . . . . ? Au1A P2 C13 C14 -16.9(8) . . . . ? C25 P2 C13 C18 177.5(8) . . . . ? C25A P2 C13 C18 -56.3(9) . . . . ? C19 P2 C13 C18 64.4(9) . . . . ? C19A P2 C13 C18 57.0(11) . . . . ? Au1 P2 C13 C18 -65.1(7) . . . . ? Au1A P2 C13 C18 171.0(6) . . . . ? C18 C13 C14 C15 -2.7(14) . . . . ? P2 C13 C14 C15 -174.7(8) . . . . ? C13 C14 C15 C16 -2.2(16) . . . . ? C14 C15 C16 C17 5.2(17) . . . . ? C15 C16 C17 C18 -3.2(19) . . . . ? C16 C17 C18 C13 -1.8(18) . . . . ? C14 C13 C18 C17 4.6(15) . . . . ? P2 C13 C18 C17 177.3(9) . . . . ? C25 P2 C19 C20 -58.0(11) . . . . ? C25A P2 C19 C20 -178(2) . . . . ? C19A P2 C19 C20 123(8) . . . . ? C13 P2 C19 C20 57.0(10) . . . . ? Au1 P2 C19 C20 -173.9(8) . . . . ? Au1A P2 C19 C20 -56.2(9) . . . . ? C25 P2 C19 C24 123.9(11) . . . . ? C25A P2 C19 C24 4(2) . . . . ? C19A P2 C19 C24 -55(8) . . . . ? C13 P2 C19 C24 -121.2(9) . . . . ? Au1 P2 C19 C24 7.9(11) . . . . ? Au1A P2 C19 C24 125.6(9) . . . . ? C24 C19 C20 C21 0.0 . . . . ? P2 C19 C20 C21 -178.2(10) . . . . ? C19 C20 C21 C22 0.0 . . . . ? C20 C21 C22 C23 0.0 . . . . ? C21 C22 C23 C24 0.0 . . . . ? C22 C23 C24 C19 0.0 . . . . ? C20 C19 C24 C23 0.0 . . . . ? P2 C19 C24 C23 178.2(10) . . . . ? C25 P2 C19A C20A -81.8(18) . . . . ? C25A P2 C19A C20A 157(2) . . . . ? C19 P2 C19A C20A -81(8) . . . . ? C13 P2 C19A C20A 35.5(19) . . . . ? Au1 P2 C19A C20A 159.5(16) . . . . ? Au1A P2 C19A C20A -80.0(17) . . . . ? C25 P2 C19A C24A 91.9(16) . . . . ? C25A P2 C19A C24A -30(3) . . . . ? C19 P2 C19A C24A 93(8) . . . . ? C13 P2 C19A C24A -150.8(15) . . . . ? Au1 P2 C19A C24A -26.8(18) . . . . ? Au1A P2 C19A C24A 93.7(15) . . . . ? C24A C19A C20A C21A 0.0 . . . . ? P2 C19A C20A C21A 173.6(19) . . . . ? C19A C20A C21A C22A 0.0 . . . . ? C20A C21A C22A C23A 0.0 . . . . ? C21A C22A C23A C24A 0.0 . . . . ? C22A C23A C24A C19A 0.0 . . . . ? C20A C19A C24A C23A 0.0 . . . . ? P2 C19A C24A C23A -173.8(19) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.289 _refine_diff_density_min -1.250 _refine_diff_density_rms 0.116 #===END #===END data_compound_1_1 _database_code_depnum_ccdc_archive 'CCDC 843626' #TrackingRef '- all-in-one.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C78 H66 Au3 P6, 3(C F3 O3 S), 7(C H2 Cl2)' _chemical_formula_sum 'C88 H80 Au3 Cl14 F9 O9 P6 S3' _chemical_formula_weight 2821.71 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' O O 0.0106 0.0060 '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' S S 0.1246 0.1234 '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 trigonal _symmetry_space_group_name_H-M R3c _symmetry_space_group_name_Hall ' R 3 -2"c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z+1/2' '-x+y, y, z+1/2' 'x, x-y, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+5/6' '-x+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+7/6' '-x+y+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' _cell_length_a 19.9108(2) _cell_length_b 19.9108(2) _cell_length_c 39.4563(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 13546.4(3) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9902 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 25.80 _exptl_crystal_description piece _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.075 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8244 _exptl_absorpt_coefficient_mu 5.531 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4741 _exptl_absorpt_correction_T_max 0.5566 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 77102 _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 28.00 _reflns_number_total 7265 _reflns_number_gt 6920 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP32 (Farugia)' _computing_publication_material 'Ciftab (Sheldrick)' _refine_special_details ; The crystal was found to be a merohedral twin, thus the twin matrix (0 1 0)(1 0 0)(0 0 -1) was applied in the refinement (BASF 0.471(5)). The asymmetric unit comprises one Au-atom, one Ph2P-CH=CH-PPh2 ligand and one triflate ion as well as solvent molecules. Only the Au-site, the phosphine ligand and 2/3 of the triflate ions could be located, whereas solvent molecules and 1/3 triflate are heavily disordered. Thus, the data set was treated with SQUEEZE as implemented in WinGX PLATON. The SQUEEZE procedure yielded 2203 electrons per unit cell, which would correspond to 1/3 of the triflate ions and 2.333 CH2Cl2 molecules (solvent used for crystallization). (expected electron count for these moieties which were omitted from refinement: 2202). The resulting composition of the unit cell contents (792 non-hydrogen atoms per cell) appears reasonable with an average spatial demand of 17.1 A3 per non-H atom. Thus, 2.333 CH2Cl2-molecules were added to the asymmetric unit (42 per unit cell) for calculation of F(000), M, absorption coefficient and density. 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^)+(0.0395P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(8) _refine_ls_number_reflns 7265 _refine_ls_number_parameters 311 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0276 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0626 _refine_ls_wR_factor_gt 0.0618 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.206037(8) 0.066111(9) 0.137112(4) 0.02628(5) Uani 1 1 d . . . P1 P 0.25615(6) 0.19412(7) 0.15112(3) 0.0288(2) Uani 1 1 d . . . P2 P 0.05888(6) 0.22613(6) 0.12018(3) 0.0251(2) Uani 1 1 d . . . C1 C 0.2867(3) 0.2189(3) 0.19457(13) 0.0320(10) Uani 1 1 d . . . C2 C 0.3655(4) 0.2579(5) 0.2042(2) 0.078(3) Uani 1 1 d . . . H2 H 0.4049 0.2717 0.1877 0.094 Uiso 1 1 calc R . . C3 C 0.3848(4) 0.2757(5) 0.23768(18) 0.072(2) Uani 1 1 d . . . H3 H 0.4377 0.3042 0.2443 0.086 Uiso 1 1 calc R . . C4 C 0.3281(4) 0.2526(4) 0.26119(16) 0.0571(17) Uani 1 1 d . . . H4 H 0.3418 0.2642 0.2844 0.068 Uiso 1 1 calc R . . C5 C 0.2531(4) 0.2135(4) 0.25248(15) 0.0532(15) Uani 1 1 d . . . H5 H 0.2145 0.1978 0.2696 0.064 Uiso 1 1 calc R . . C6 C 0.2310(3) 0.1959(3) 0.21915(14) 0.0454(13) Uani 1 1 d . . . H6 H 0.1776 0.1679 0.2133 0.054 Uiso 1 1 calc R . . C7 C 0.3390(3) 0.2551(3) 0.12404(13) 0.0396(11) Uani 1 1 d . . . C8 C 0.3873(4) 0.2308(4) 0.1136(2) 0.083(3) Uani 1 1 d . . . H8 H 0.3763 0.1808 0.1209 0.100 Uiso 1 1 calc R . . C9 C 0.4516(5) 0.2715(5) 0.0933(3) 0.099(4) Uani 1 1 d . . . H9 H 0.4841 0.2516 0.0866 0.119 Uiso 1 1 calc R . . C10 C 0.4648(4) 0.3446(5) 0.0834(2) 0.074(2) Uani 1 1 d . . . H10 H 0.5099 0.3768 0.0705 0.089 Uiso 1 1 calc R . . C11 C 0.4153(3) 0.3727(4) 0.09158(16) 0.0559(17) Uani 1 1 d . . . H11 H 0.4235 0.4208 0.0830 0.067 Uiso 1 1 calc R . . C12 C 0.3523(4) 0.3264(3) 0.11323(14) 0.0485(14) Uani 1 1 d . . . H12 H 0.3187 0.3447 0.1204 0.058 Uiso 1 1 calc R . . C13 C 0.1892(3) 0.2282(3) 0.14570(11) 0.0299(9) Uani 1 1 d . . . H13 H 0.2001 0.2756 0.1562 0.036 Uiso 1 1 calc R . . C14 C 0.1255(2) 0.1904(3) 0.12782(11) 0.0265(9) Uani 1 1 d . . . H14 H 0.1135 0.1418 0.1184 0.032 Uiso 1 1 calc R . . C15 C 0.0993(3) 0.3166(3) 0.14368(12) 0.0322(10) Uani 1 1 d . . . C16 C 0.0828(5) 0.3118(4) 0.17675(17) 0.092(3) Uani 1 1 d . . . H16 H 0.0466 0.2629 0.1861 0.111 Uiso 1 1 calc R . . C17 C 0.1171(5) 0.3766(5) 0.1980(2) 0.102(4) Uani 1 1 d . . . H17 H 0.1065 0.3715 0.2217 0.122 Uiso 1 1 calc R . . C18 C 0.1662(4) 0.4472(4) 0.1840(2) 0.068(2) Uani 1 1 d . . . H18 H 0.1880 0.4926 0.1977 0.081 Uiso 1 1 calc R . . C19 C 0.1837(4) 0.4525(4) 0.1506(2) 0.065(2) Uani 1 1 d . . . H19 H 0.2183 0.5019 0.1411 0.077 Uiso 1 1 calc R . . C20 C 0.1524(4) 0.3878(3) 0.13012(16) 0.0513(15) Uani 1 1 d . . . H20 H 0.1671 0.3920 0.1070 0.062 Uiso 1 1 calc R . . C21 C 0.0700(3) 0.2467(3) 0.07550(12) 0.0274(9) Uani 1 1 d . . . C22 C 0.1444(3) 0.2834(3) 0.06034(15) 0.0490(13) Uani 1 1 d . . . H22 H 0.1891 0.2988 0.0740 0.059 Uiso 1 1 calc R . . C23 C 0.1527(4) 0.2971(4) 0.02566(14) 0.0580(17) Uani 1 1 d . . . H23 H 0.2026 0.3206 0.0154 0.070 Uiso 1 1 calc R . . C24 C 0.0885(4) 0.2762(4) 0.00656(17) 0.0599(18) Uani 1 1 d . . . H24 H 0.0939 0.2868 -0.0171 0.072 Uiso 1 1 calc R . . C25 C 0.0151(3) 0.2399(4) 0.02094(14) 0.0510(15) Uani 1 1 d . . . H25 H -0.0292 0.2246 0.0070 0.061 Uiso 1 1 calc R . . C26 C 0.0059(3) 0.2258(3) 0.05551(13) 0.0376(11) Uani 1 1 d . . . H26 H -0.0443 0.2018 0.0653 0.045 Uiso 1 1 calc R . . S1 S 0.0000 0.0000 0.19631(6) 0.0419(5) Uani 1 3 d S . . F1 F 0.06902(18) 0.05220(19) 0.25488(9) 0.0501(8) Uani 1 1 d . . . C27 C 0.0000 0.0000 0.2417(2) 0.0384(19) Uani 1 3 d S . . O1 O 0.0623(3) -0.0131(3) 0.18810(12) 0.0649(13) Uani 1 1 d . . . S2 S 0.3333 0.6667 0.24044(5) 0.0252(4) Uani 1 3 d S . . F2 F 0.37656(19) 0.73811(19) 0.18156(8) 0.0508(8) Uani 1 1 d . . . O2 O 0.2957(2) 0.58525(18) 0.24842(9) 0.0364(8) Uani 1 1 d . . . C28 C 0.3333 0.6667 0.1938(2) 0.0367(19) Uani 1 3 d S . . 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 0.02120(8) 0.02209(8) 0.03474(7) -0.00220(6) -0.00364(7) 0.01021(7) P1 0.0183(5) 0.0242(6) 0.0408(6) -0.0063(5) -0.0054(4) 0.0083(4) P2 0.0212(5) 0.0217(5) 0.0327(6) -0.0060(4) -0.0013(4) 0.0109(4) C1 0.030(2) 0.024(2) 0.046(3) -0.0058(19) -0.0096(19) 0.0163(19) C2 0.032(3) 0.121(7) 0.081(5) -0.054(5) -0.027(3) 0.038(4) C3 0.046(4) 0.114(6) 0.069(4) -0.056(4) -0.036(3) 0.050(4) C4 0.080(5) 0.060(4) 0.049(3) -0.029(3) -0.039(3) 0.047(4) C5 0.061(4) 0.042(3) 0.044(3) 0.001(2) -0.007(3) 0.017(3) C6 0.040(3) 0.030(3) 0.045(3) 0.001(2) -0.012(2) 0.001(2) C7 0.026(2) 0.034(3) 0.048(3) -0.010(2) 0.003(2) 0.007(2) C8 0.038(4) 0.063(4) 0.153(8) 0.037(5) 0.041(4) 0.029(3) C9 0.052(5) 0.072(6) 0.172(11) 0.035(6) 0.055(5) 0.030(4) C10 0.041(4) 0.062(4) 0.087(5) -0.009(4) 0.027(3) 0.003(3) C11 0.043(3) 0.043(3) 0.055(3) -0.019(3) 0.014(3) 0.002(3) C12 0.053(3) 0.031(3) 0.043(3) -0.015(2) 0.017(2) 0.007(2) C13 0.030(2) 0.034(2) 0.032(2) -0.0035(18) -0.0050(18) 0.020(2) C14 0.024(2) 0.020(2) 0.031(2) -0.0010(16) 0.0046(17) 0.0074(16) C15 0.024(2) 0.033(2) 0.041(3) -0.0115(19) 0.0006(18) 0.0152(19) C16 0.102(6) 0.048(4) 0.057(4) -0.026(3) 0.045(4) -0.014(4) C17 0.094(6) 0.071(5) 0.077(5) -0.053(4) 0.037(5) -0.007(4) C18 0.050(4) 0.047(4) 0.096(6) -0.039(4) -0.008(4) 0.017(3) C19 0.074(5) 0.032(3) 0.074(5) -0.015(3) -0.014(4) 0.017(3) C20 0.065(4) 0.025(3) 0.060(4) -0.007(2) -0.018(3) 0.020(3) C21 0.027(2) 0.019(2) 0.040(2) -0.0015(17) -0.0007(18) 0.0144(17) C22 0.036(3) 0.062(4) 0.052(3) 0.008(3) 0.000(2) 0.027(3) C23 0.061(4) 0.080(5) 0.039(3) 0.023(3) 0.018(3) 0.039(4) C24 0.054(4) 0.090(5) 0.050(3) 0.034(3) 0.011(3) 0.046(4) C25 0.043(3) 0.068(4) 0.042(3) 0.013(3) -0.011(2) 0.028(3) C26 0.028(2) 0.033(3) 0.048(3) 0.008(2) -0.005(2) 0.013(2) S1 0.0393(7) 0.0393(7) 0.0469(13) 0.000 0.000 0.0197(4) F1 0.0362(17) 0.0464(19) 0.064(2) -0.0085(16) -0.0087(15) 0.0177(15) C27 0.038(3) 0.038(3) 0.040(5) 0.000 0.000 0.0189(14) O1 0.063(3) 0.077(3) 0.061(3) -0.007(2) 0.017(2) 0.040(3) S2 0.0209(5) 0.0209(5) 0.0340(9) 0.000 0.000 0.0104(3) F2 0.0440(19) 0.0484(19) 0.0528(19) 0.0108(15) 0.0013(15) 0.0177(16) O2 0.0336(18) 0.0249(16) 0.049(2) 0.0066(14) 0.0138(15) 0.0132(14) C28 0.028(3) 0.028(3) 0.053(5) 0.000 0.000 0.0142(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 P1 2.2923(11) . ? Au1 P2 2.3054(11) 3 ? P1 C13 1.786(4) . ? P1 C1 1.803(5) . ? P1 C7 1.826(5) . ? P2 C21 1.798(5) . ? P2 C14 1.816(4) . ? P2 C15 1.818(4) . ? C1 C6 1.368(7) . ? C1 C2 1.412(7) . ? C2 C3 1.370(10) . ? C2 H2 0.9500 . ? C3 C4 1.351(10) . ? C3 H3 0.9500 . ? C4 C5 1.339(9) . ? C4 H4 0.9500 . ? C5 C6 1.376(8) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.341(8) . ? C7 C12 1.375(8) . ? C8 C9 1.377(10) . ? C8 H8 0.9500 . ? C9 C10 1.401(12) . ? C9 H9 0.9500 . ? C10 C11 1.393(10) . ? C10 H10 0.9500 . ? C11 C12 1.413(8) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.311(6) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.337(8) . ? C15 C20 1.384(7) . ? C16 C17 1.397(8) . ? C16 H16 0.9500 . ? C17 C18 1.366(11) . ? C17 H17 0.9500 . ? C18 C19 1.355(11) . ? C18 H18 0.9500 . ? C19 C20 1.378(8) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C26 1.375(6) . ? C21 C22 1.416(7) . ? C22 C23 1.389(7) . ? C22 H22 0.9500 . ? C23 C24 1.358(9) . ? C23 H23 0.9500 . ? C24 C25 1.387(9) . ? C24 H24 0.9500 . ? C25 C26 1.386(7) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? S1 O1 1.427(5) . ? S1 C27 1.790(9) . ? F1 C27 1.346(5) . ? S2 O2 1.440(3) . ? S2 C28 1.840(9) . ? F2 C28 1.332(5) . ? 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 P2 174.20(4) . 3 ? C13 P1 C1 102.9(2) . . ? C13 P1 C7 105.9(2) . . ? C1 P1 C7 107.8(2) . . ? C13 P1 Au1 113.64(16) . . ? C1 P1 Au1 115.65(15) . . ? C7 P1 Au1 110.17(17) . . ? C21 P2 C14 102.8(2) . . ? C21 P2 C15 109.3(2) . . ? C14 P2 C15 104.8(2) . . ? C21 P2 Au1 114.68(15) . 2 ? C14 P2 Au1 112.83(14) . 2 ? C15 P2 Au1 111.60(15) . 2 ? C6 C1 C2 119.0(5) . . ? C6 C1 P1 118.4(4) . . ? C2 C1 P1 122.5(5) . . ? C3 C2 C1 119.5(7) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C4 C3 C2 119.7(6) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C5 C4 C3 121.4(6) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? C4 C5 C6 121.0(6) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C1 C6 C5 119.4(5) . . ? C1 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C8 C7 C12 118.4(5) . . ? C8 C7 P1 120.8(5) . . ? C12 C7 P1 120.8(4) . . ? C7 C8 C9 126.1(7) . . ? C7 C8 H8 117.0 . . ? C9 C8 H8 117.0 . . ? C8 C9 C10 114.2(7) . . ? C8 C9 H9 122.9 . . ? C10 C9 H9 122.9 . . ? C11 C10 C9 123.4(6) . . ? C11 C10 H10 118.3 . . ? C9 C10 H10 118.3 . . ? C10 C11 C12 117.0(7) . . ? C10 C11 H11 121.5 . . ? C12 C11 H11 121.5 . . ? C7 C12 C11 120.7(6) . . ? C7 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C14 C13 P1 122.6(4) . . ? C14 C13 H13 118.7 . . ? P1 C13 H13 118.7 . . ? C13 C14 P2 123.4(3) . . ? C13 C14 H14 118.3 . . ? P2 C14 H14 118.3 . . ? C16 C15 C20 119.0(5) . . ? C16 C15 P2 117.1(4) . . ? C20 C15 P2 123.4(4) . . ? C15 C16 C17 122.1(7) . . ? C15 C16 H16 118.9 . . ? C17 C16 H16 118.9 . . ? C18 C17 C16 118.4(7) . . ? C18 C17 H17 120.8 . . ? C16 C17 H17 120.8 . . ? C19 C18 C17 119.9(6) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 121.3(7) . . ? C18 C19 H19 119.4 . . ? C20 C19 H19 119.4 . . ? C19 C20 C15 119.2(6) . . ? C19 C20 H20 120.4 . . ? C15 C20 H20 120.4 . . ? C26 C21 C22 119.1(5) . . ? C26 C21 P2 120.3(4) . . ? C22 C21 P2 120.6(4) . . ? C23 C22 C21 120.5(5) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C24 C23 C22 119.0(6) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? C23 C24 C25 121.2(6) . . ? C23 C24 H24 119.4 . . ? C25 C24 H24 119.4 . . ? C26 C25 C24 120.4(5) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C21 C26 C25 119.7(5) . . ? C21 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? O1 S1 O1 115.01(16) . 3 ? O1 S1 O1 115.01(16) . 2 ? O1 S1 O1 115.01(16) 3 2 ? O1 S1 C27 103.1(2) . . ? O1 S1 C27 103.1(2) 3 . ? O1 S1 C27 103.1(2) 2 . ? F1 C27 F1 106.0(4) 3 . ? F1 C27 F1 106.0(4) 3 2 ? F1 C27 F1 106.0(4) . 2 ? F1 C27 S1 112.8(4) 3 . ? F1 C27 S1 112.8(4) . . ? F1 C27 S1 112.8(4) 2 . ? O2 S2 O2 115.36(11) 3_565 2_665 ? O2 S2 O2 115.36(11) 3_565 . ? O2 S2 O2 115.36(11) 2_665 . ? O2 S2 C28 102.63(16) 3_565 . ? O2 S2 C28 102.63(16) 2_665 . ? O2 S2 C28 102.63(16) . . ? F2 C28 F2 107.6(4) 2_665 . ? F2 C28 F2 107.6(4) 2_665 3_565 ? F2 C28 F2 107.6(4) . 3_565 ? F2 C28 S2 111.3(4) 2_665 . ? F2 C28 S2 111.3(4) . . ? F2 C28 S2 111.3(4) 3_565 . ? 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 C13 P1 C1 C6 51.9(4) . . . . ? C7 P1 C1 C6 163.6(4) . . . . ? Au1 P1 C1 C6 -72.6(4) . . . . ? C13 P1 C1 C2 -131.0(5) . . . . ? C7 P1 C1 C2 -19.3(6) . . . . ? Au1 P1 C1 C2 104.5(5) . . . . ? C6 C1 C2 C3 -3.6(11) . . . . ? P1 C1 C2 C3 179.3(6) . . . . ? C1 C2 C3 C4 3.1(13) . . . . ? C2 C3 C4 C5 -1.2(12) . . . . ? C3 C4 C5 C6 -0.2(10) . . . . ? C2 C1 C6 C5 2.2(9) . . . . ? P1 C1 C6 C5 179.4(4) . . . . ? C4 C5 C6 C1 -0.3(9) . . . . ? C13 P1 C7 C8 -158.3(6) . . . . ? C1 P1 C7 C8 92.0(6) . . . . ? Au1 P1 C7 C8 -35.0(7) . . . . ? C13 P1 C7 C12 20.2(5) . . . . ? C1 P1 C7 C12 -89.4(5) . . . . ? Au1 P1 C7 C12 143.5(4) . . . . ? C12 C7 C8 C9 1.6(14) . . . . ? P1 C7 C8 C9 -179.8(9) . . . . ? C7 C8 C9 C10 0.0(17) . . . . ? C8 C9 C10 C11 -3.6(16) . . . . ? C9 C10 C11 C12 5.2(12) . . . . ? C8 C7 C12 C11 0.2(9) . . . . ? P1 C7 C12 C11 -178.4(4) . . . . ? C10 C11 C12 C7 -3.4(9) . . . . ? C1 P1 C13 C14 -141.8(4) . . . . ? C7 P1 C13 C14 105.2(4) . . . . ? Au1 P1 C13 C14 -15.9(5) . . . . ? P1 C13 C14 P2 -176.8(2) . . . . ? C21 P2 C14 C13 111.7(4) . . . . ? C15 P2 C14 C13 -2.6(5) . . . . ? Au1 P2 C14 C13 -124.2(4) 2 . . . ? C21 P2 C15 C16 167.4(6) . . . . ? C14 P2 C15 C16 -83.0(6) . . . . ? Au1 P2 C15 C16 39.4(6) 2 . . . ? C21 P2 C15 C20 -20.3(5) . . . . ? C14 P2 C15 C20 89.3(5) . . . . ? Au1 P2 C15 C20 -148.2(4) 2 . . . ? C20 C15 C16 C17 0.5(14) . . . . ? P2 C15 C16 C17 173.2(9) . . . . ? C15 C16 C17 C18 3.1(17) . . . . ? C16 C17 C18 C19 -3.5(15) . . . . ? C17 C18 C19 C20 0.5(13) . . . . ? C18 C19 C20 C15 3.0(10) . . . . ? C16 C15 C20 C19 -3.5(10) . . . . ? P2 C15 C20 C19 -175.7(5) . . . . ? C14 P2 C21 C26 136.7(4) . . . . ? C15 P2 C21 C26 -112.4(4) . . . . ? Au1 P2 C21 C26 13.9(4) 2 . . . ? C14 P2 C21 C22 -42.2(4) . . . . ? C15 P2 C21 C22 68.7(4) . . . . ? Au1 P2 C21 C22 -165.1(4) 2 . . . ? C26 C21 C22 C23 -1.0(8) . . . . ? P2 C21 C22 C23 177.9(5) . . . . ? C21 C22 C23 C24 1.4(10) . . . . ? C22 C23 C24 C25 -1.8(11) . . . . ? C23 C24 C25 C26 1.7(11) . . . . ? C22 C21 C26 C25 0.9(8) . . . . ? P2 C21 C26 C25 -178.1(4) . . . . ? C24 C25 C26 C21 -1.2(9) . . . . ? O1 S1 C27 F1 -64.1(3) . . . 3 ? O1 S1 C27 F1 55.9(3) 3 . . 3 ? O1 S1 C27 F1 175.9(3) 2 . . 3 ? O1 S1 C27 F1 55.9(3) . . . . ? O1 S1 C27 F1 175.9(3) 3 . . . ? O1 S1 C27 F1 -64.1(3) 2 . . . ? O1 S1 C27 F1 175.9(3) . . . 2 ? O1 S1 C27 F1 -64.1(3) 3 . . 2 ? O1 S1 C27 F1 55.9(3) 2 . . 2 ? O2 S2 C28 F2 -50.6(2) 3_565 . . 2_665 ? O2 S2 C28 F2 -170.6(2) 2_665 . . 2_665 ? O2 S2 C28 F2 69.4(2) . . . 2_665 ? O2 S2 C28 F2 69.4(2) 3_565 . . . ? O2 S2 C28 F2 -50.6(2) 2_665 . . . ? O2 S2 C28 F2 -170.6(2) . . . . ? O2 S2 C28 F2 -170.6(2) 3_565 . . 3_565 ? O2 S2 C28 F2 69.4(2) 2_665 . . 3_565 ? O2 S2 C28 F2 -50.6(2) . . . 3_565 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.730 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.089