# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Tzi Sum Andy Hor' _publ_contact_author_address ; Department of Chemistry National University of Singapore 3 Science Drive 3 S117543 SINGAPORE ; _publ_contact_author_email ANDYHOR@NUS.EDU.SG _publ_section_title ; Assembly of gold rings and chains with pyridyl carboxylate as directional spacer ; loop_ _publ_author_name 'Hor Andy' 'L. L. Koh' 'Peili Teo' data_6145 _database_code_depnum_ccdc_archive 'CCDC 632232' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C126 H100.50 Au6 F9 Fe3 N4.50 O17 P6 S3' _chemical_formula_weight 3751.96 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' N N 0.0061 0.0033 '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' Fe Fe 0.3463 0.8444 '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 Rhombohedral _symmetry_space_group_name_H-M R-3c 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' '-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-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-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+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 19.0071(4) _cell_length_b 19.0071(4) _cell_length_c 123.338(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 38588.6(19) _cell_formula_units_Z 12 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3155 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 26.77 _exptl_crystal_description Block _exptl_crystal_colour Gold _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.937 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 21540 _exptl_absorpt_coefficient_mu 7.343 _exptl_absorpt_correction_type 'Sadabs, (Sheldrick 2001)' _exptl_absorpt_correction_T_min 0.3214 _exptl_absorpt_correction_T_max 0.5911 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 64068 _diffrn_reflns_av_R_equivalents 0.1441 _diffrn_reflns_av_sigmaI/netI 0.0762 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -141 _diffrn_reflns_limit_l_max 124 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 24.00 _reflns_number_total 6735 _reflns_number_gt 4436 _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 ; Due to poor data quality, some restraints were applied during final refinement cycles. These included: phenyl rings refined as fixed hexagons, restraints in bond lengths and thermal parameters of one of the Otf anion so that the atoms retain the expected geometry. 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^)+(0.1384P)^2^+0.0202P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6735 _refine_ls_number_parameters 444 _refine_ls_number_restraints 41 _refine_ls_R_factor_all 0.1198 _refine_ls_R_factor_gt 0.0792 _refine_ls_wR_factor_ref 0.2321 _refine_ls_wR_factor_gt 0.2079 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.022 _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 0.27647(5) 1.00832(4) 0.613428(6) 0.0629(3) Uani 1 1 d . . . Au2 Au 0.24674(5) 0.96381(6) 0.637059(6) 0.0726(3) Uani 1 1 d . . . Fe1 Fe 0.42095(14) 0.91535(15) 0.62626(2) 0.0575(6) Uani 1 1 d . . . P1 P 0.2875(3) 0.9050(3) 0.60687(4) 0.0541(11) Uani 1 1 d . . . P2 P 0.3715(3) 1.0259(3) 0.64365(4) 0.0643(13) Uani 1 1 d . . . N1 N 0.2512(11) 1.0986(10) 0.61865(11) 0.071(4) Uani 1 1 d . . . O1 O 0.0927(11) 1.2204(8) 0.63149(10) 0.080(4) Uani 1 1 d . . . O2 O 0.2173(10) 1.3276(9) 0.63179(11) 0.090(4) Uani 1 1 d . . . C1 C 0.1672(16) 1.2553(14) 0.63015(14) 0.068(5) Uani 1 1 d . . . C2 C 0.1969(15) 1.1990(11) 0.62606(13) 0.071(5) Uani 1 1 d . . . C3 C 0.1444(15) 1.1262(13) 0.6216(2) 0.109(8) Uani 1 1 d . . . H3 H 0.0887 1.1087 0.6210 0.131 Uiso 1 1 calc R . . C4 C 0.1748(15) 1.0795(15) 0.6179(2) 0.111(9) Uani 1 1 d . . . H4 H 0.1384 1.0298 0.6146 0.134 Uiso 1 1 calc R . . C5 C 0.2762(16) 1.2213(14) 0.6257(2) 0.106(8) Uani 1 1 d . . . H5 H 0.3161 1.2737 0.6278 0.127 Uiso 1 1 calc R . . C6 C 0.2973(14) 1.1680(12) 0.62217(19) 0.090(7) Uani 1 1 d . . . H6 H 0.3530 1.1848 0.6224 0.108 Uiso 1 1 calc R . . C7 C 0.3264(9) 0.8581(9) 0.61595(12) 0.045(4) Uani 1 1 d . . . C8 C 0.3862(11) 0.8376(10) 0.61339(12) 0.058(5) Uani 1 1 d . . . H8 H 0.4155 0.8495 0.6064 0.070 Uiso 1 1 calc R . . C9 C 0.4002(11) 0.8014(10) 0.62216(15) 0.065(5) Uani 1 1 d . . . H9 H 0.4402 0.7825 0.6225 0.078 Uiso 1 1 calc R . . C10 C 0.3489(14) 0.7977(11) 0.63051(17) 0.084(7) Uani 1 1 d . . . H10 H 0.3447 0.7743 0.6378 0.101 Uiso 1 1 calc R . . C11 C 0.2994(10) 0.8313(10) 0.62633(14) 0.058(4) Uani 1 1 d . . . H11 H 0.2562 0.8353 0.6303 0.070 Uiso 1 1 calc R . . C12 C 0.4435(10) 1.0120(10) 0.63601(15) 0.064(5) Uani 1 1 d . . . C13 C 0.4895(11) 0.9733(10) 0.63936(14) 0.064(5) Uani 1 1 d . . . H13 H 0.4857 0.9482 0.6465 0.077 Uiso 1 1 calc R . . C14 C 0.5395(10) 0.9770(13) 0.63087(16) 0.074(5) Uani 1 1 d . . . H14 H 0.5767 0.9546 0.6310 0.089 Uiso 1 1 calc R . . C15 C 0.5267(12) 1.0153(12) 0.62192(18) 0.083(6) Uani 1 1 d . . . H15 H 0.5534 1.0234 0.6148 0.100 Uiso 1 1 calc R . . C16 C 0.4706(11) 1.0393(10) 0.62453(14) 0.062(5) Uani 1 1 d . . . H16 H 0.4508 1.0672 0.6197 0.074 Uiso 1 1 calc R . . C1A C 0.1869(5) 0.8240(6) 0.60278(8) 0.050(4) Uani 1 1 d G . . C2A C 0.1689(7) 0.7436(7) 0.60241(9) 0.072(5) Uani 1 1 d G . . H2A H 0.2090 0.7304 0.6042 0.086 Uiso 1 1 calc R . . C3A C 0.0917(8) 0.6828(5) 0.59940(10) 0.077(6) Uani 1 1 d G . . H3A H 0.0796 0.6284 0.5992 0.092 Uiso 1 1 calc R . . C4A C 0.0325(6) 0.7023(7) 0.59675(9) 0.082(6) Uani 1 1 d G . . H4A H -0.0197 0.6612 0.5947 0.098 Uiso 1 1 calc R . . C5A C 0.0505(6) 0.7827(8) 0.59711(9) 0.080(6) Uani 1 1 d G . . H5A H 0.0104 0.7960 0.5953 0.096 Uiso 1 1 calc R . . C6A C 0.1277(7) 0.8436(6) 0.60013(9) 0.066(5) Uani 1 1 d G . . H6A H 0.1398 0.8979 0.6004 0.080 Uiso 1 1 calc R . . C1B C 0.3549(7) 0.9353(8) 0.59521(8) 0.055(4) Uani 1 1 d G . . C2B C 0.4207(8) 1.0140(7) 0.59485(9) 0.080(6) Uani 1 1 d G . . H2B H 0.4272 1.0515 0.6003 0.096 Uiso 1 1 calc R . . C3B C 0.4769(7) 1.0371(7) 0.58647(12) 0.091(7) Uani 1 1 d G . . H3B H 0.5214 1.0903 0.5862 0.109 Uiso 1 1 calc R . . C4B C 0.4672(8) 0.9816(9) 0.57845(9) 0.085(6) Uani 1 1 d G . . H4B H 0.5052 0.9973 0.5728 0.101 Uiso 1 1 calc R . . C5B C 0.4014(9) 0.9030(8) 0.57881(9) 0.082(6) Uani 1 1 d G . . H5B H 0.3949 0.8654 0.5734 0.098 Uiso 1 1 calc R . . C6B C 0.3452(7) 0.8798(6) 0.58719(10) 0.067(5) Uani 1 1 d G . . H6B H 0.3007 0.8266 0.5874 0.080 Uiso 1 1 calc R . . C1C C 0.3756(7) 0.9890(7) 0.65694(8) 0.065(5) Uani 1 1 d G . . C2C C 0.3211(7) 0.9081(7) 0.65930(10) 0.073(5) Uani 1 1 d G . . H2C H 0.2828 0.8747 0.6541 0.088 Uiso 1 1 calc R . . C3C C 0.3233(9) 0.8764(7) 0.66937(12) 0.085(6) Uani 1 1 d G . . H3C H 0.2864 0.8217 0.6710 0.102 Uiso 1 1 calc R . . C4C C 0.3799(10) 0.9257(10) 0.67708(9) 0.098(8) Uani 1 1 d G . . H4C H 0.3814 0.9043 0.6839 0.117 Uiso 1 1 calc R . . C5C C 0.4344(9) 1.0067(10) 0.67472(10) 0.107(8) Uani 1 1 d G . . H5C H 0.4727 1.0400 0.6799 0.129 Uiso 1 1 calc R . . C6C C 0.4322(7) 1.0384(7) 0.66464(11) 0.090(7) Uani 1 1 d G . . H6C H 0.4690 1.0931 0.6630 0.108 Uiso 1 1 calc R . . C1D C 0.4106(11) 1.1309(8) 0.64540(13) 0.083(6) Uani 1 1 d GU . . C2D C 0.3616(9) 1.1578(11) 0.65003(13) 0.110(8) Uani 1 1 d GU . . H2D H 0.3086 1.1201 0.6523 0.132 Uiso 1 1 calc R . . C3D C 0.3911(13) 1.2406(12) 0.65136(15) 0.150(11) Uani 1 1 d GU . . H3D H 0.3580 1.2588 0.6545 0.179 Uiso 1 1 calc R . . C4D C 0.4696(14) 1.2963(8) 0.64806(18) 0.177(14) Uani 1 1 d GU . . H4D H 0.4895 1.3523 0.6490 0.212 Uiso 1 1 calc R . . C5D C 0.5185(10) 1.2693(11) 0.64343(17) 0.187(14) Uani 1 1 d GU . . H5D H 0.5716 1.3070 0.6412 0.224 Uiso 1 1 calc R . . C6D C 0.4890(10) 1.1866(12) 0.64210(14) 0.131(10) Uani 1 1 d GU . . H6D H 0.5221 1.1684 0.6390 0.157 Uiso 1 1 calc R . . S1 S 0.3333 0.6667 0.57101(8) 0.084(3) Uani 1 3 d S . . O3 O 0.4195(9) 0.7044(10) 0.56792(13) 0.109(5) Uani 1 1 d . . . C17 C 0.3333 0.6667 0.5858(3) 0.079(10) Uani 1 3 d S . . F1 F 0.2610(7) 0.6555(8) 0.58942(9) 0.102(4) Uani 1 1 d . . . S2 S 1.0000 0.0000 0.50807(18) 0.079(4) Uani 0.50 3 d SPD . . O4 O 0.9156(12) -0.053(3) 0.5100(5) 0.118(10) Uani 0.50 1 d PD . . C18 C 1.0000 0.0000 0.4935(3) 0.079(4) Uani 0.50 3 d SPD . . F2 F 1.0592(13) 0.070(2) 0.4891(4) 0.118(10) Uani 0.50 1 d PD . . S3 S 0.549(2) 0.358(2) 0.6019(3) 0.265(14) Uiso 0.50 1 d P A 1 C1N C 0.460(3) 0.314(3) 0.6026(4) 0.100 Uiso 0.50 1 d PD B 2 C2N C 0.492(3) 0.263(3) 0.6063(4) 0.100 Uiso 0.50 1 d PD B 2 N1N N 0.522(2) 0.227(2) 0.6060(3) 0.100 Uiso 0.50 1 d PD B 2 O1W O 0.6667 0.3333 0.5833 0.16(2) Uani 1 6 d S . . O2W O 0.146(2) 0.091(2) 0.6518(2) 0.119(11) Uiso 0.50 1 d P . . 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 0.0749(5) 0.0618(5) 0.0705(5) -0.0077(4) -0.0103(4) 0.0481(4) Au2 0.0566(5) 0.0917(7) 0.0753(5) -0.0062(4) -0.0114(4) 0.0415(5) Fe1 0.0455(14) 0.0528(15) 0.0732(15) 0.0087(12) -0.0028(11) 0.0239(12) P1 0.056(3) 0.056(3) 0.063(3) 0.001(2) -0.002(2) 0.037(2) P2 0.056(3) 0.067(3) 0.076(3) -0.004(3) -0.016(2) 0.036(3) N1 0.103(13) 0.068(11) 0.065(9) -0.014(8) -0.016(9) 0.060(11) O1 0.117(13) 0.068(9) 0.084(9) -0.012(7) 0.009(8) 0.069(9) O2 0.113(12) 0.077(10) 0.108(10) -0.043(8) -0.036(9) 0.068(10) C1 0.099(17) 0.082(16) 0.053(10) -0.016(10) -0.010(11) 0.068(15) C2 0.107(17) 0.050(11) 0.067(11) -0.011(9) -0.007(11) 0.047(12) C3 0.090(17) 0.064(14) 0.16(2) -0.054(15) -0.020(16) 0.028(13) C4 0.090(17) 0.096(18) 0.19(2) -0.059(18) -0.043(17) 0.074(16) C5 0.11(2) 0.074(16) 0.16(2) -0.037(15) -0.033(17) 0.066(15) C6 0.086(15) 0.057(13) 0.15(2) -0.028(13) -0.011(14) 0.056(13) C7 0.037(8) 0.036(8) 0.060(9) -0.001(7) -0.010(7) 0.015(7) C8 0.088(13) 0.057(10) 0.047(9) 0.014(8) 0.016(9) 0.049(10) C9 0.049(11) 0.051(11) 0.103(13) 0.006(10) 0.008(10) 0.031(9) C10 0.104(17) 0.036(10) 0.101(15) -0.008(10) -0.033(14) 0.026(11) C11 0.047(10) 0.049(10) 0.074(11) 0.001(9) -0.014(9) 0.021(8) C12 0.045(10) 0.051(11) 0.084(12) -0.006(9) -0.023(9) 0.015(9) C13 0.060(12) 0.066(12) 0.071(11) 0.011(9) -0.013(10) 0.035(10) C14 0.036(10) 0.090(15) 0.088(13) 0.015(11) -0.006(10) 0.026(10) C15 0.054(12) 0.075(14) 0.099(15) 0.013(12) 0.017(11) 0.017(11) C16 0.054(11) 0.043(10) 0.086(12) 0.002(9) -0.003(9) 0.022(9) C1A 0.061(11) 0.047(10) 0.045(8) 0.011(7) 0.006(8) 0.031(8) C2A 0.062(12) 0.070(13) 0.097(14) 0.019(11) 0.004(10) 0.043(11) C3A 0.068(13) 0.045(11) 0.100(14) 0.006(10) -0.017(11) 0.016(10) C4A 0.048(11) 0.072(14) 0.091(14) 0.020(11) -0.001(10) 0.004(11) C5A 0.081(15) 0.102(18) 0.077(13) -0.002(12) -0.014(11) 0.061(15) C6A 0.070(13) 0.055(11) 0.077(11) 0.011(9) -0.014(10) 0.035(10) C1B 0.052(10) 0.065(12) 0.053(9) 0.002(9) -0.006(8) 0.033(10) C2B 0.102(17) 0.081(15) 0.074(12) -0.005(11) 0.004(12) 0.058(14) C3B 0.087(16) 0.058(13) 0.107(16) 0.018(12) 0.027(13) 0.019(12) C4B 0.087(16) 0.085(16) 0.090(14) 0.037(13) 0.028(12) 0.049(14) C5B 0.102(17) 0.091(17) 0.081(13) 0.006(12) 0.008(12) 0.070(15) C6B 0.069(13) 0.061(12) 0.079(12) 0.014(10) -0.001(10) 0.039(10) C1C 0.041(10) 0.074(13) 0.075(11) -0.017(10) -0.016(9) 0.024(10) C2C 0.070(13) 0.064(13) 0.072(12) 0.000(10) 0.007(10) 0.024(11) C3C 0.060(13) 0.078(15) 0.096(15) 0.004(13) 0.008(12) 0.018(11) C4C 0.13(2) 0.12(2) 0.084(15) 0.029(15) 0.024(15) 0.10(2) C5C 0.098(19) 0.14(2) 0.081(15) 0.005(15) -0.021(13) 0.060(19) C6C 0.096(17) 0.103(18) 0.091(14) -0.015(13) -0.018(13) 0.066(15) C1D 0.084(12) 0.069(11) 0.113(13) -0.002(10) -0.002(10) 0.051(10) C2D 0.119(15) 0.090(14) 0.132(15) -0.005(12) -0.009(12) 0.061(12) C3D 0.143(19) 0.149(19) 0.19(2) -0.014(15) -0.019(15) 0.098(15) C4D 0.20(2) 0.135(19) 0.23(2) -0.013(15) 0.021(17) 0.110(17) C5D 0.17(2) 0.16(2) 0.22(2) -0.024(17) 0.032(17) 0.076(16) C6D 0.149(18) 0.085(14) 0.183(18) -0.015(13) 0.004(15) 0.076(13) S1 0.072(4) 0.072(4) 0.107(7) 0.000 0.000 0.0362(19) O3 0.072(10) 0.105(12) 0.153(13) 0.025(11) 0.020(9) 0.047(9) C17 0.057(13) 0.057(13) 0.12(3) 0.000 0.000 0.029(6) F1 0.089(9) 0.099(9) 0.113(9) 0.001(7) 0.004(7) 0.044(8) S2 0.086(7) 0.086(7) 0.065(9) 0.000 0.000 0.043(3) O4 0.070(16) 0.21(3) 0.089(11) 0.052(15) 0.016(16) 0.078(16) C18 0.086(7) 0.086(7) 0.065(9) 0.000 0.000 0.043(3) F2 0.070(16) 0.21(3) 0.089(11) 0.052(15) 0.016(16) 0.078(16) O1W 0.22(3) 0.22(3) 0.031(17) 0.000 0.000 0.111(17) _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 N1 2.102(15) . ? Au1 P1 2.228(4) . ? Au1 Au2 3.0085(11) . ? Au2 O1 2.077(13) 3_465 ? Au2 P2 2.209(5) . ? Fe1 C7 2.019(14) . ? Fe1 C13 2.021(17) . ? Fe1 C10 2.02(2) . ? Fe1 C15 2.03(2) . ? Fe1 C14 2.033(18) . ? Fe1 C8 2.041(16) . ? Fe1 C11 2.049(17) . ? Fe1 C12 2.053(19) . ? Fe1 C9 2.061(18) . ? Fe1 C16 2.064(17) . ? P1 C7 1.804(15) . ? P1 C1B 1.818(10) . ? P1 C1A 1.826(10) . ? P2 C1D 1.761(14) . ? P2 C12 1.79(2) . ? P2 C1C 1.798(11) . ? N1 C6 1.24(2) . ? N1 C4 1.31(3) . ? O1 C1 1.24(2) . ? O1 Au2 2.077(13) 2_675 ? O2 C1 1.24(3) . ? C1 C2 1.52(3) . ? C2 C5 1.35(3) . ? C2 C3 1.36(3) . ? C3 C4 1.35(3) . ? C5 C6 1.33(3) . ? C7 C11 1.38(2) . ? C7 C8 1.41(2) . ? C8 C9 1.38(2) . ? C9 C10 1.40(3) . ? C10 C11 1.47(3) . ? C12 C13 1.46(2) . ? C12 C16 1.51(2) . ? C13 C14 1.39(3) . ? C14 C15 1.41(3) . ? C15 C16 1.39(3) . ? C1A C2A 1.3900 . ? C1A C6A 1.3900 . ? C2A C3A 1.3900 . ? C3A C4A 1.3900 . ? C4A C5A 1.3900 . ? C5A C6A 1.3900 . ? C1B C2B 1.3900 . ? C1B C6B 1.3900 . ? C2B C3B 1.3900 . ? C3B C4B 1.3900 . ? C4B C5B 1.3900 . ? C5B C6B 1.3900 . ? C1C C2C 1.3900 . ? C1C C6C 1.3900 . ? C2C C3C 1.3900 . ? C3C C4C 1.3900 . ? C4C C5C 1.3900(10) . ? C5C C6C 1.3900 . ? C1D C2D 1.3900 . ? C1D C6D 1.3900(11) . ? C2D C3D 1.3900 . ? C3D C4D 1.3900(12) . ? C4D C5D 1.3900 . ? C5D C6D 1.3900 . ? S1 O3 1.473(14) 2_665 ? S1 O3 1.473(14) 3_565 ? S1 O3 1.473(14) . ? S1 C17 1.83(4) . ? C17 F1 1.356(17) 3_565 ? C17 F1 1.356(17) . ? C17 F1 1.356(17) 2_665 ? S2 O4 1.424(19) 3_765 ? S2 O4 1.424(18) 2_645 ? S2 O4 1.424(19) . ? S2 C18 1.80(2) . ? O4 C18 1.47(2) 19_756 ? C18 F2 1.353(19) . ? C18 F2 1.353(18) 2_645 ? C18 F2 1.353(18) 3_765 ? C1N C2N 1.47(2) . ? C2N N1N 1.091(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Au1 P1 172.5(5) . . ? N1 Au1 Au2 81.1(4) . . ? P1 Au1 Au2 101.02(12) . . ? O1 Au2 P2 177.3(4) 3_465 . ? O1 Au2 Au1 80.1(4) 3_465 . ? P2 Au2 Au1 101.87(14) . . ? C7 Fe1 C13 162.7(7) . . ? C7 Fe1 C10 68.8(7) . . ? C13 Fe1 C10 106.9(8) . . ? C7 Fe1 C15 122.4(8) . . ? C13 Fe1 C15 68.5(8) . . ? C10 Fe1 C15 155.5(10) . . ? C7 Fe1 C14 156.6(8) . . ? C13 Fe1 C14 40.2(7) . . ? C10 Fe1 C14 120.5(8) . . ? C15 Fe1 C14 40.6(8) . . ? C7 Fe1 C8 40.7(6) . . ? C13 Fe1 C8 154.6(7) . . ? C10 Fe1 C8 66.8(7) . . ? C15 Fe1 C8 106.4(8) . . ? C14 Fe1 C8 119.9(8) . . ? C7 Fe1 C11 39.6(6) . . ? C13 Fe1 C11 126.2(7) . . ? C10 Fe1 C11 42.3(8) . . ? C15 Fe1 C11 159.1(8) . . ? C14 Fe1 C11 160.2(7) . . ? C8 Fe1 C11 66.9(7) . . ? C7 Fe1 C12 125.6(7) . . ? C13 Fe1 C12 41.9(7) . . ? C10 Fe1 C12 124.1(8) . . ? C15 Fe1 C12 69.6(8) . . ? C14 Fe1 C12 69.2(8) . . ? C8 Fe1 C12 161.9(7) . . ? C11 Fe1 C12 110.2(7) . . ? C7 Fe1 C9 68.2(7) . . ? C13 Fe1 C9 120.1(7) . . ? C10 Fe1 C9 40.0(7) . . ? C15 Fe1 C9 119.9(8) . . ? C14 Fe1 C9 104.4(8) . . ? C8 Fe1 C9 39.2(6) . . ? C11 Fe1 C9 68.5(7) . . ? C12 Fe1 C9 158.2(7) . . ? C7 Fe1 C16 109.0(7) . . ? C13 Fe1 C16 70.1(7) . . ? C10 Fe1 C16 163.6(9) . . ? C15 Fe1 C16 39.7(8) . . ? C14 Fe1 C16 68.2(8) . . ? C8 Fe1 C16 122.9(7) . . ? C11 Fe1 C16 125.7(7) . . ? C12 Fe1 C16 43.0(7) . . ? C9 Fe1 C16 155.7(7) . . ? C7 P1 C1B 104.5(6) . . ? C7 P1 C1A 105.7(6) . . ? C1B P1 C1A 108.9(6) . . ? C7 P1 Au1 116.9(5) . . ? C1B P1 Au1 111.7(5) . . ? C1A P1 Au1 108.9(4) . . ? C1D P2 C12 108.2(9) . . ? C1D P2 C1C 104.7(7) . . ? C12 P2 C1C 103.8(7) . . ? C1D P2 Au2 112.4(6) . . ? C12 P2 Au2 115.1(6) . . ? C1C P2 Au2 111.8(5) . . ? C6 N1 C4 114.5(18) . . ? C6 N1 Au1 130.3(15) . . ? C4 N1 Au1 115.2(14) . . ? C1 O1 Au2 121.2(13) . 2_675 ? O2 C1 O1 127.7(18) . . ? O2 C1 C2 119(2) . . ? O1 C1 C2 113(2) . . ? C5 C2 C3 116(2) . . ? C5 C2 C1 123(2) . . ? C3 C2 C1 121(2) . . ? C4 C3 C2 118(2) . . ? N1 C4 C3 125(2) . . ? C6 C5 C2 119(2) . . ? N1 C6 C5 127(2) . . ? C11 C7 C8 107.9(14) . . ? C11 C7 P1 126.2(12) . . ? C8 C7 P1 125.8(12) . . ? C11 C7 Fe1 71.4(9) . . ? C8 C7 Fe1 70.5(9) . . ? P1 C7 Fe1 126.9(8) . . ? C9 C8 C7 110.3(14) . . ? C9 C8 Fe1 71.2(10) . . ? C7 C8 Fe1 68.8(9) . . ? C8 C9 C10 107.4(16) . . ? C8 C9 Fe1 69.6(10) . . ? C10 C9 Fe1 68.5(10) . . ? C9 C10 C11 107.6(17) . . ? C9 C10 Fe1 71.5(12) . . ? C11 C10 Fe1 69.8(10) . . ? C7 C11 C10 106.6(17) . . ? C7 C11 Fe1 69.0(9) . . ? C10 C11 Fe1 67.9(11) . . ? C13 C12 C16 104.6(16) . . ? C13 C12 P2 128.5(14) . . ? C16 C12 P2 126.9(13) . . ? C13 C12 Fe1 67.9(10) . . ? C16 C12 Fe1 68.9(10) . . ? P2 C12 Fe1 127.5(9) . . ? C14 C13 C12 109.2(16) . . ? C14 C13 Fe1 70.4(10) . . ? C12 C13 Fe1 70.3(10) . . ? C13 C14 C15 109.0(18) . . ? C13 C14 Fe1 69.4(10) . . ? C15 C14 Fe1 69.6(11) . . ? C16 C15 C14 110.3(19) . . ? C16 C15 Fe1 71.5(11) . . ? C14 C15 Fe1 69.9(11) . . ? C15 C16 C12 106.9(16) . . ? C15 C16 Fe1 68.8(11) . . ? C12 C16 Fe1 68.1(9) . . ? C2A C1A C6A 120.0 . . ? C2A C1A P1 120.9(7) . . ? C6A C1A P1 119.1(7) . . ? C3A C2A C1A 120.0 . . ? C2A C3A C4A 120.0 . . ? C3A C4A C5A 120.0 . . ? C6A C5A C4A 120.0 . . ? C5A C6A C1A 120.0 . . ? C2B C1B C6B 120.0 . . ? C2B C1B P1 118.6(8) . . ? C6B C1B P1 121.2(8) . . ? C3B C2B C1B 120.0 . . ? C2B C3B C4B 120.00(7) . . ? C5B C4B C3B 120.0 . . ? C6B C5B C4B 120.0 . . ? C5B C6B C1B 120.00(6) . . ? C2C C1C C6C 120.0 . . ? C2C C1C P2 118.0(8) . . ? C6C C1C P2 122.0(8) . . ? C3C C2C C1C 120.0 . . ? C2C C3C C4C 120.0 . . ? C5C C4C C3C 120.0 . . ? C4C C5C C6C 120.0 . . ? C5C C6C C1C 120.0 . . ? C2D C1D C6D 120.0 . . ? C2D C1D P2 119.2(11) . . ? C6D C1D P2 120.8(11) . . ? C3D C2D C1D 120.00(7) . . ? C2D C3D C4D 120.0 . . ? C5D C4D C3D 120.00(6) . . ? C4D C5D C6D 120.00(8) . . ? C5D C6D C1D 120.0 . . ? O3 S1 O3 113.6(6) 2_665 3_565 ? O3 S1 O3 113.6(6) 2_665 . ? O3 S1 O3 113.6(6) 3_565 . ? O3 S1 C17 105.0(7) 2_665 . ? O3 S1 C17 105.0(8) 3_565 . ? O3 S1 C17 105.0(8) . . ? F1 C17 F1 109.9(17) 3_565 . ? F1 C17 F1 109.9(17) 3_565 2_665 ? F1 C17 F1 109.9(17) . 2_665 ? F1 C17 S1 109.0(17) 3_565 . ? F1 C17 S1 109.0(17) . . ? F1 C17 S1 109.0(17) 2_665 . ? O4 S2 O4 117.2(14) 3_765 2_645 ? O4 S2 O4 117.2(15) 3_765 . ? O4 S2 O4 117.2(15) 2_645 . ? O4 S2 C18 100(3) 3_765 . ? O4 S2 C18 100(3) 2_645 . ? O4 S2 C18 100(3) . . ? S2 O4 C18 7(2) . 19_756 ? F2 C18 F2 105(3) . 2_645 ? F2 C18 F2 105(3) . 3_765 ? F2 C18 F2 105(3) 2_645 3_765 ? F2 C18 S2 113(3) . . ? F2 C18 S2 113(3) 2_645 . ? F2 C18 S2 113(3) 3_765 . ? N1N C2N C1N 160(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.899 _refine_diff_density_min -0.788 _refine_diff_density_rms 0.211 # Attachment '6219.cif' data_6219 _database_code_depnum_ccdc_archive 'CCDC 632233' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H46 Au2 Cl12 F6 Fe N2 O10 P2 S' _chemical_formula_weight 1990.13 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' N N 0.0061 0.0033 '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' 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 15.9755(10) _cell_length_b 14.3238(9) _cell_length_c 15.9882(10) _cell_angle_alpha 90.00 _cell_angle_beta 103.661(2) _cell_angle_gamma 90.00 _cell_volume 3555.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2364 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 17.32 _exptl_crystal_description Block _exptl_crystal_colour Gold _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.859 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 4.913 _exptl_absorpt_correction_type 'Sadabs, (Sheldrick 2001)' _exptl_absorpt_correction_T_min 0.4399 _exptl_absorpt_correction_T_max 0.8277 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 20170 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0610 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6255 _reflns_number_gt 3263 _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^)+(0.1924P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6255 _refine_ls_number_parameters 382 _refine_ls_number_restraints 143 _refine_ls_R_factor_all 0.1447 _refine_ls_R_factor_gt 0.0858 _refine_ls_wR_factor_ref 0.2974 _refine_ls_wR_factor_gt 0.2540 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.000 _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 0.22961(5) 0.44296(4) 0.38235(5) 0.1141(4) Uani 1 1 d . . . Fe1 Fe 0.5000 0.5000 0.5000 0.0820(8) Uani 1 2 d S . . P1 P 0.3006(3) 0.5777(3) 0.3879(3) 0.0936(11) Uani 1 1 d . . . O1 O -0.0934(14) -0.0907(15) 0.333(2) 0.271(16) Uani 1 1 d D . . H1O H -0.187(4) -0.082(4) 0.413(5) 0.220 Uiso 1 1 d D . . O2 O -0.1508(13) -0.0381(10) 0.4193(14) 0.176(7) Uani 1 1 d D . . C1 C 0.3933(10) 0.5844(8) 0.4741(9) 0.085(4) Uani 1 1 d . . . C2 C 0.4022(12) 0.5334(10) 0.5547(9) 0.094(4) Uani 1 1 d . . . H2 H 0.3629 0.4905 0.5682 0.113 Uiso 1 1 calc R . . C3 C 0.4819(13) 0.5614(12) 0.6082(10) 0.108(6) Uani 1 1 d . . . H3 H 0.5040 0.5389 0.6643 0.129 Uiso 1 1 calc R . . C4 C 0.5227(11) 0.6252(10) 0.5683(10) 0.099(4) Uani 1 1 d . . . H4 H 0.5753 0.6550 0.5921 0.119 Uiso 1 1 calc R . . C5 C 0.4704(10) 0.6377(8) 0.4842(10) 0.092(4) Uani 1 1 d . . . H5 H 0.4845 0.6755 0.4415 0.110 Uiso 1 1 calc R . . N1 N 0.1588(7) 0.3220(7) 0.3790(9) 0.123(4) Uani 1 1 d GU . . C6 C 0.1109(11) 0.3061(11) 0.4398(9) 0.227(12) Uani 1 1 d GU . . H6 H 0.1131 0.3491 0.4847 0.272 Uiso 1 1 calc R . . C7 C 0.0598(11) 0.2268(13) 0.4341(12) 0.232(13) Uani 1 1 d GU . . H7 H 0.0274 0.2161 0.4752 0.279 Uiso 1 1 calc R . . C8 C 0.0565(9) 0.1633(9) 0.3677(13) 0.156(7) Uani 1 1 d GU . . C9 C 0.1044(11) 0.1792(8) 0.3069(11) 0.196(11) Uani 1 1 d G . . H9 H 0.1022 0.1363 0.2619 0.236 Uiso 1 1 calc R . . C10 C 0.1555(9) 0.2585(9) 0.3125(9) 0.188(12) Uani 1 1 d G . . H10 H 0.1879 0.2693 0.2714 0.226 Uiso 1 1 calc R . . C11 C 0.0104(17) 0.0786(14) 0.3600(17) 0.211(17) Uani 1 1 d D . . H11 H 0.0283 0.0347 0.3241 0.253 Uiso 1 1 calc R . . C12 C -0.0485(13) 0.0509(13) 0.3911(17) 0.150(9) Uani 1 1 d D . . H12 H -0.0643 0.0934 0.4295 0.180 Uiso 1 1 calc R . . C13 C -0.0986(13) -0.0349(14) 0.3800(17) 0.121(6) Uani 1 1 d D . . C1A C 0.2299(5) 0.6732(5) 0.4032(5) 0.105(5) Uani 1 1 d G . . C2A C 0.2567(6) 0.7384(7) 0.4685(5) 0.148(7) Uani 1 1 d G . . H2A H 0.3119 0.7338 0.5053 0.178 Uiso 1 1 calc R . . C3A C 0.2018(7) 0.8104(7) 0.4793(7) 0.165(8) Uani 1 1 d G . . H3A H 0.2200 0.8544 0.5235 0.198 Uiso 1 1 calc R . . C4A C 0.1202(7) 0.8172(8) 0.4249(7) 0.166(8) Uani 1 1 d G . . H4A H 0.0831 0.8658 0.4322 0.200 Uiso 1 1 calc R . . C5A C 0.0934(5) 0.7520(9) 0.3596(7) 0.197(13) Uani 1 1 d G . . H5A H 0.0382 0.7566 0.3228 0.237 Uiso 1 1 calc R . . C6A C 0.1483(4) 0.6801(7) 0.3488(6) 0.147(7) Uani 1 1 d G . . H6A H 0.1302 0.6360 0.3046 0.177 Uiso 1 1 calc R . . C1B C 0.3353(4) 0.6031(5) 0.2913(4) 0.096(4) Uani 1 1 d G . . C2B C 0.3552(4) 0.6946(5) 0.2743(5) 0.133(6) Uani 1 1 d G . . H2B H 0.3501 0.7425 0.3130 0.160 Uiso 1 1 calc R . . C3B C 0.3825(6) 0.7152(7) 0.2001(6) 0.142(7) Uani 1 1 d G . . H3B H 0.3960 0.7771 0.1886 0.171 Uiso 1 1 calc R . . C4B C 0.3901(6) 0.6444(8) 0.1429(5) 0.156(8) Uani 1 1 d G . . H4B H 0.4086 0.6584 0.0927 0.187 Uiso 1 1 calc R . . C5B C 0.3702(6) 0.5529(8) 0.1599(5) 0.151(9) Uani 1 1 d G . . H5B H 0.3753 0.5050 0.1212 0.181 Uiso 1 1 calc R . . C6B C 0.3428(6) 0.5323(6) 0.2341(6) 0.105(5) Uani 1 1 d G . . H6B H 0.3294 0.4704 0.2456 0.126 Uiso 1 1 calc R . . C1X C 0.1379(15) 0.9867(17) 0.1425(15) 0.217(12) Uani 1 1 d DU . . H1X H 0.1855 1.0308 0.1656 0.261 Uiso 1 1 calc R . . Cl1 Cl 0.0336(12) 1.0313(14) 0.1236(13) 0.420(11) Uani 1 1 d DU . . Cl2 Cl 0.1268(19) 0.8934(16) 0.2074(14) 0.559(17) Uani 1 1 d DU . . Cl3 Cl 0.1366(12) 0.9394(11) 0.0491(12) 0.389(12) Uani 1 1 d DU . . Cl4 Cl 0.4143(11) 0.5401(10) 0.8462(15) 0.381(10) Uani 1 1 d DU . . Cl5 Cl 0.3784(15) 0.3954(12) 0.9393(11) 0.426(10) Uani 1 1 d DU . . Cl6 Cl 0.2617(10) 0.5249(16) 0.8840(16) 0.492(15) Uani 1 1 d DU . . C2X C 0.3377(16) 0.4594(17) 0.8513(18) 0.244(16) Uani 1 1 d DU . . H2X H 0.3161 0.4232 0.7978 0.293 Uiso 1 1 calc R . . O4 O -0.2600(10) -0.1802(12) 0.3809(12) 0.260(12) Uani 1 1 d DU . . O3 O -0.2487(12) -0.3379(15) 0.3347(16) 0.309(14) Uani 1 1 d DU . . O5 O -0.3214(15) -0.3038(14) 0.4513(9) 0.289(13) Uani 1 1 d DU . . S1 S -0.2883(7) -0.2751(8) 0.3797(7) 0.163(5) Uani 0.50 1 d PDU . . F1 F -0.3587(17) -0.230(2) 0.2328(10) 0.330(14) Uani 1 1 d D . . F2 F -0.4261(9) -0.3456(10) 0.3024(10) 0.201(6) Uani 1 1 d D . . F3 F -0.4315(10) -0.2082(13) 0.3439(16) 0.265(9) Uani 1 1 d D . . C1S C -0.3845(10) -0.2633(14) 0.3040(12) 0.259(17) Uani 1 1 d DU . . 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 0.1244(7) 0.0763(5) 0.1385(7) -0.0091(3) 0.0251(5) -0.0411(3) Fe1 0.106(2) 0.0597(14) 0.0839(16) -0.0134(12) 0.0307(14) -0.0205(13) P1 0.106(3) 0.068(2) 0.106(3) -0.0049(18) 0.026(2) -0.0259(19) O1 0.203(19) 0.175(16) 0.49(4) -0.16(2) 0.20(3) -0.111(15) O2 0.165(15) 0.121(11) 0.248(19) -0.009(11) 0.059(14) -0.063(10) C1 0.121(11) 0.047(6) 0.091(9) -0.010(6) 0.032(8) -0.033(7) C2 0.130(13) 0.084(9) 0.076(9) -0.014(7) 0.043(9) -0.011(8) C3 0.133(15) 0.130(15) 0.072(9) -0.021(9) 0.049(10) 0.014(11) C4 0.132(12) 0.073(8) 0.087(10) -0.033(7) 0.016(9) -0.024(8) C5 0.122(11) 0.050(7) 0.114(11) -0.009(6) 0.049(9) -0.010(7) N1 0.121(9) 0.089(8) 0.155(10) 0.000(8) 0.021(8) -0.053(7) C6 0.25(2) 0.179(18) 0.26(2) -0.027(16) 0.069(17) -0.089(16) C7 0.24(2) 0.22(2) 0.25(2) 0.001(16) 0.075(16) -0.090(16) C8 0.158(14) 0.106(12) 0.175(14) 0.020(12) -0.017(12) -0.017(11) C9 0.17(2) 0.122(18) 0.29(3) -0.017(19) 0.05(2) -0.048(16) C10 0.137(16) 0.054(9) 0.36(4) -0.015(15) 0.023(19) -0.038(10) C11 0.22(3) 0.088(13) 0.25(3) 0.049(16) -0.08(3) -0.075(16) C12 0.098(13) 0.104(14) 0.23(2) 0.014(13) 0.015(14) -0.043(10) C13 0.083(11) 0.094(12) 0.181(19) -0.027(12) 0.022(12) -0.031(10) C1A 0.117(13) 0.089(10) 0.123(11) -0.014(9) 0.053(10) -0.019(9) C2A 0.131(15) 0.109(13) 0.179(17) -0.044(13) -0.014(13) -0.008(11) C3A 0.146(17) 0.134(17) 0.20(2) -0.033(15) 0.015(16) 0.022(15) C4A 0.128(17) 0.15(2) 0.21(2) 0.015(17) 0.012(16) 0.020(15) C5A 0.137(18) 0.23(3) 0.21(2) -0.11(2) 0.009(17) 0.027(18) C6A 0.104(13) 0.163(18) 0.155(16) -0.054(14) -0.010(12) 0.014(12) C1B 0.111(11) 0.075(9) 0.102(10) -0.004(8) 0.025(8) -0.017(8) C2B 0.153(16) 0.119(14) 0.120(13) 0.023(11) 0.017(12) -0.020(12) C3B 0.174(19) 0.098(13) 0.157(17) 0.043(12) 0.044(15) -0.016(12) C4B 0.153(18) 0.20(3) 0.108(14) 0.030(15) 0.016(12) 0.013(18) C5B 0.18(2) 0.17(2) 0.093(13) 0.007(12) 0.018(13) 0.048(16) C6B 0.109(12) 0.108(11) 0.096(11) 0.005(9) 0.020(9) 0.000(9) C1X 0.21(2) 0.20(2) 0.23(2) -0.05(2) 0.033(19) 0.02(2) Cl1 0.308(17) 0.53(3) 0.46(2) -0.072(19) 0.161(17) 0.102(16) Cl2 0.67(3) 0.48(3) 0.53(3) 0.15(2) 0.16(3) -0.08(3) Cl3 0.44(2) 0.43(2) 0.39(2) 0.054(14) 0.266(19) 0.079(15) Cl4 0.351(18) 0.276(14) 0.58(3) 0.108(15) 0.232(19) 0.067(12) Cl5 0.65(3) 0.346(16) 0.312(16) -0.020(15) 0.174(19) -0.02(2) Cl6 0.316(18) 0.61(3) 0.58(3) -0.24(2) 0.17(2) -0.08(2) C2X 0.23(3) 0.27(3) 0.26(3) -0.04(2) 0.12(2) 0.02(2) O4 0.185(16) 0.28(2) 0.33(2) 0.127(19) 0.101(17) -0.037(15) O3 0.23(2) 0.38(3) 0.32(3) -0.08(2) 0.082(19) -0.14(2) O5 0.37(3) 0.32(2) 0.169(13) 0.057(14) 0.041(16) -0.20(2) S1 0.155(9) 0.133(8) 0.191(10) 0.016(7) 0.020(8) -0.099(7) F1 0.43(3) 0.40(3) 0.173(13) 0.119(18) 0.100(18) 0.10(3) F2 0.242(15) 0.140(10) 0.208(12) -0.001(9) 0.023(11) -0.047(11) F3 0.210(16) 0.217(18) 0.40(3) -0.047(18) 0.136(18) -0.035(14) C1S 0.30(2) 0.22(2) 0.26(2) -0.014(18) 0.063(19) -0.001(19) _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 N1 2.063(8) . ? Au1 P1 2.230(3) . ? Fe1 C2 2.019(15) . ? Fe1 C2 2.019(15) 3_666 ? Fe1 C3 2.021(13) . ? Fe1 C3 2.021(13) 3_666 ? Fe1 C5 2.030(12) 3_666 ? Fe1 C5 2.030(12) . ? Fe1 C1 2.051(15) 3_666 ? Fe1 C1 2.051(15) . ? Fe1 C4 2.086(12) 3_666 ? Fe1 C4 2.086(12) . ? P1 C1 1.772(15) . ? P1 C1B 1.797(8) . ? P1 C1A 1.826(9) . ? O1 C13 1.12(2) . ? O2 C13 1.16(2) . ? C1 C5 1.426(18) . ? C1 C2 1.46(2) . ? C2 C3 1.41(3) . ? C3 C4 1.36(2) . ? C4 C5 1.42(2) . ? N1 C6 1.3900 . ? N1 C10 1.3900 . ? C6 C7 1.3900 . ? C7 C8 1.3900 . ? C8 C9 1.3900 . ? C8 C11 1.409(19) . ? C9 C10 1.3900 . ? C11 C12 1.230(19) . ? C12 C13 1.45(2) . ? C1A C2A 1.3900 . ? C1A C6A 1.3900 . ? C2A C3A 1.3900 . ? C3A C4A 1.3900 . ? C4A C5A 1.3900 . ? C5A C6A 1.3900 . ? C1B C2B 1.3900 . ? C1B C6B 1.3901 . ? C2B C3B 1.3901 . ? C3B C4B 1.3899 . ? C4B C5B 1.3901 . ? C5B C6B 1.3900 . ? C1X Cl3 1.636(18) . ? C1X Cl2 1.727(19) . ? C1X Cl1 1.744(19) . ? Cl4 C2X 1.699(19) . ? Cl5 C2X 1.677(19) . ? Cl6 C2X 1.711(18) . ? O4 S1 1.432(15) . ? O3 S1 1.393(16) . ? O5 S1 1.429(14) . ? S1 C1S 1.725(15) . ? F1 C1S 1.387(17) . ? F2 C1S 1.351(17) . ? F3 C1S 1.350(17) . ? 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 N1 Au1 P1 177.0(4) . . ? C2 Fe1 C2 179.997(2) . 3_666 ? C2 Fe1 C3 41.0(7) . . ? C2 Fe1 C3 139.0(7) 3_666 . ? C2 Fe1 C3 139.0(7) . 3_666 ? C2 Fe1 C3 41.0(7) 3_666 3_666 ? C3 Fe1 C3 179.997(2) . 3_666 ? C2 Fe1 C5 110.9(6) . 3_666 ? C2 Fe1 C5 69.1(6) 3_666 3_666 ? C3 Fe1 C5 113.1(6) . 3_666 ? C3 Fe1 C5 66.9(6) 3_666 3_666 ? C2 Fe1 C5 69.1(6) . . ? C2 Fe1 C5 110.9(6) 3_666 . ? C3 Fe1 C5 66.9(6) . . ? C3 Fe1 C5 113.1(6) 3_666 . ? C5 Fe1 C5 179.999(2) 3_666 . ? C2 Fe1 C1 138.0(6) . 3_666 ? C2 Fe1 C1 42.0(6) 3_666 3_666 ? C3 Fe1 C1 111.4(6) . 3_666 ? C3 Fe1 C1 68.6(6) 3_666 3_666 ? C5 Fe1 C1 40.9(5) 3_666 3_666 ? C5 Fe1 C1 139.1(5) . 3_666 ? C2 Fe1 C1 42.0(6) . . ? C2 Fe1 C1 138.0(6) 3_666 . ? C3 Fe1 C1 68.6(6) . . ? C3 Fe1 C1 111.4(6) 3_666 . ? C5 Fe1 C1 139.1(5) 3_666 . ? C5 Fe1 C1 40.9(5) . . ? C1 Fe1 C1 179.998(3) 3_666 . ? C2 Fe1 C4 111.9(6) . 3_666 ? C2 Fe1 C4 68.1(6) 3_666 3_666 ? C3 Fe1 C4 141.2(6) . 3_666 ? C3 Fe1 C4 38.8(6) 3_666 3_666 ? C5 Fe1 C4 40.2(6) 3_666 3_666 ? C5 Fe1 C4 139.8(6) . 3_666 ? C1 Fe1 C4 68.4(6) 3_666 3_666 ? C1 Fe1 C4 111.6(6) . 3_666 ? C2 Fe1 C4 68.1(6) . . ? C2 Fe1 C4 111.9(6) 3_666 . ? C3 Fe1 C4 38.8(6) . . ? C3 Fe1 C4 141.2(6) 3_666 . ? C5 Fe1 C4 139.8(6) 3_666 . ? C5 Fe1 C4 40.2(6) . . ? C1 Fe1 C4 111.6(6) 3_666 . ? C1 Fe1 C4 68.4(6) . . ? C4 Fe1 C4 179.997(2) 3_666 . ? C1 P1 C1B 106.7(5) . . ? C1 P1 C1A 106.5(5) . . ? C1B P1 C1A 106.8(4) . . ? C1 P1 Au1 113.7(4) . . ? C1B P1 Au1 113.5(3) . . ? C1A P1 Au1 109.2(3) . . ? C5 C1 C2 105.5(13) . . ? C5 C1 P1 131.2(11) . . ? C2 C1 P1 123.3(11) . . ? C5 C1 Fe1 68.8(8) . . ? C2 C1 Fe1 67.9(9) . . ? P1 C1 Fe1 128.9(7) . . ? C3 C2 C1 106.1(13) . . ? C3 C2 Fe1 69.6(9) . . ? C1 C2 Fe1 70.2(8) . . ? C4 C3 C2 111.6(15) . . ? C4 C3 Fe1 73.2(8) . . ? C2 C3 Fe1 69.5(8) . . ? C3 C4 C5 106.8(14) . . ? C3 C4 Fe1 68.0(7) . . ? C5 C4 Fe1 67.8(7) . . ? C4 C5 C1 109.8(12) . . ? C4 C5 Fe1 72.0(8) . . ? C1 C5 Fe1 70.3(7) . . ? C6 N1 C10 120.0 . . ? C6 N1 Au1 120.5(8) . . ? C10 N1 Au1 119.4(8) . . ? N1 C6 C7 120.0 . . ? C8 C7 C6 120.0 . . ? C9 C8 C7 120.0 . . ? C9 C8 C11 116.3(18) . . ? C7 C8 C11 123.6(18) . . ? C8 C9 C10 120.0 . . ? C9 C10 N1 120.0 . . ? C12 C11 C8 133(3) . . ? C11 C12 C13 132(2) . . ? O1 C13 O2 121(2) . . ? O1 C13 C12 124(3) . . ? O2 C13 C12 114(2) . . ? C2A C1A C6A 120.0 . . ? C2A C1A P1 120.9(4) . . ? C6A C1A P1 119.1(4) . . ? C1A C2A C3A 120.0 . . ? C2A C3A C4A 120.0 . . ? C5A C4A C3A 120.0 . . ? C4A C5A C6A 120.0 . . ? C5A C6A C1A 120.0 . . ? C2B C1B C6B 120.0 . . ? C2B C1B P1 119.3(3) . . ? C6B C1B P1 120.7(3) . . ? C1B C2B C3B 120.0 . . ? C4B C3B C2B 120.0 . . ? C3B C4B C5B 120.0 . . ? C6B C5B C4B 120.0 . . ? C5B C6B C1B 120.0 . . ? Cl3 C1X Cl2 104.3(14) . . ? Cl3 C1X Cl1 100.9(13) . . ? Cl2 C1X Cl1 99.1(14) . . ? Cl5 C2X Cl4 105.8(15) . . ? Cl5 C2X Cl6 101.9(14) . . ? Cl4 C2X Cl6 102.3(13) . . ? O3 S1 O5 121.8(12) . . ? O3 S1 O4 116.0(11) . . ? O5 S1 O4 116.0(11) . . ? O3 S1 C1S 98.0(11) . . ? O5 S1 C1S 98.9(10) . . ? O4 S1 C1S 98.2(10) . . ? F3 C1S F2 101.2(17) . . ? F3 C1S F1 119(2) . . ? F2 C1S F1 122(2) . . ? F3 C1S S1 103.2(13) . . ? F2 C1S S1 106.3(12) . . ? F1 C1S S1 102.8(12) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H1O O4 0.85(2) 1.82(3) 2.66(2) 169(5) . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.147 _refine_diff_density_min -0.842 _refine_diff_density_rms 0.166 # Attachment '6243.cif' data_6243 _database_code_depnum_ccdc_archive 'CCDC 632234' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C71 H57 Au4 Cl3 F6 Fe2 O6 P4 S3' _chemical_formula_weight 2346.14 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 15.1716(12) _cell_length_b 14.9383(12) _cell_length_c 32.609(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.997(2) _cell_angle_gamma 90.00 _cell_volume 7254.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 7506 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.16 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.148 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4448 _exptl_absorpt_coefficient_mu 8.800 _exptl_absorpt_correction_type 'Sadabs, (Sheldrick 2001)' _exptl_absorpt_correction_T_min 0.1777 _exptl_absorpt_correction_T_max 0.4732 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 49779 _diffrn_reflns_av_R_equivalents 0.0710 _diffrn_reflns_av_sigmaI/netI 0.0868 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.50 _reflns_number_total 16641 _reflns_number_gt 10611 _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^)+(0.0633P)^2^+13.2863P] 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 16641 _refine_ls_number_parameters 916 _refine_ls_number_restraints 86 _refine_ls_R_factor_all 0.1042 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1363 _refine_ls_wR_factor_gt 0.1208 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.003 _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 0.57330(2) 0.53555(3) 0.559177(13) 0.03403(11) Uani 1 1 d . . . Au2 Au 0.53833(2) 0.41142(3) 0.620980(12) 0.03139(11) Uani 1 1 d . . . Au3 Au 0.34989(2) 0.44059(3) 0.599327(12) 0.03186(11) Uani 1 1 d . . . Au4 Au 0.37772(2) 0.56466(3) 0.534711(12) 0.03237(11) Uani 1 1 d . . . S3 S 0.45356(16) 0.42763(17) 0.55138(7) 0.0303(5) Uani 1 1 d . . . Fe1 Fe 0.77531(9) 0.55407(10) 0.67169(4) 0.0313(3) Uani 1 1 d . . . Fe2 Fe 0.19384(9) 0.67471(10) 0.60543(5) 0.0349(3) Uani 1 1 d . . . P1 P 0.69166(16) 0.63162(18) 0.57387(8) 0.0323(6) Uani 1 1 d . . . P2 P 0.62634(16) 0.39318(19) 0.68430(8) 0.0321(6) Uani 1 1 d . . . P3 P 0.25384(17) 0.46444(18) 0.64354(8) 0.0324(6) Uani 1 1 d . . . P4 P 0.30155(17) 0.69517(18) 0.52415(8) 0.0328(6) Uani 1 1 d . . . C1 C 0.7780(6) 0.5810(7) 0.6113(3) 0.031(2) Uani 1 1 d . . . C2 C 0.8529(7) 0.6233(7) 0.6384(3) 0.039(3) Uani 1 1 d . . . H2 H 0.8659 0.6848 0.6403 0.047 Uiso 1 1 calc R . . C3 C 0.9024(7) 0.5544(9) 0.6612(3) 0.049(3) Uani 1 1 d . . . H3 H 0.9551 0.5628 0.6813 0.058 Uiso 1 1 calc R . . C4 C 0.8631(7) 0.4725(8) 0.6501(3) 0.044(3) Uani 1 1 d . . . H4 H 0.8841 0.4167 0.6613 0.053 Uiso 1 1 calc R . . C5 C 0.7861(6) 0.4868(7) 0.6190(3) 0.031(2) Uani 1 1 d . . . H5 H 0.7469 0.4424 0.6056 0.038 Uiso 1 1 calc R . . C6 C 0.6840(6) 0.4955(8) 0.7008(3) 0.036(2) Uani 1 1 d . . . C7 C 0.7662(7) 0.5086(9) 0.7301(3) 0.046(3) Uani 1 1 d . . . H7 H 0.8013 0.4637 0.7455 0.055 Uiso 1 1 calc R . . C8 C 0.7847(9) 0.6006(8) 0.7316(4) 0.053(3) Uani 1 1 d . . . H8 H 0.8350 0.6278 0.7483 0.064 Uiso 1 1 calc R . . C9 C 0.7162(8) 0.6457(8) 0.7043(4) 0.050(3) Uani 1 1 d . . . H9 H 0.7126 0.7077 0.6993 0.061 Uiso 1 1 calc R . . C10 C 0.6528(7) 0.5795(7) 0.6855(3) 0.036(2) Uani 1 1 d . . . H10 H 0.5994 0.5906 0.6663 0.043 Uiso 1 1 calc R . . C11 C 0.1722(6) 0.5462(6) 0.6218(3) 0.030(2) Uani 1 1 d . . . C12 C 0.1252(7) 0.6082(7) 0.6439(4) 0.045(3) Uani 1 1 d . . . H12 H 0.1325 0.6153 0.6730 0.053 Uiso 1 1 calc R . . C13 C 0.0657(7) 0.6561(7) 0.6129(4) 0.050(3) Uani 1 1 d . . . H13 H 0.0261 0.7014 0.6180 0.060 Uiso 1 1 calc R . . C14 C 0.0750(7) 0.6255(8) 0.5736(4) 0.047(3) Uani 1 1 d . . . H14 H 0.0426 0.6469 0.5480 0.057 Uiso 1 1 calc R . . C15 C 0.1400(6) 0.5581(6) 0.5782(3) 0.031(2) Uani 1 1 d . . . H15 H 0.1590 0.5265 0.5565 0.037 Uiso 1 1 calc R . . C16 C 0.2800(7) 0.7332(6) 0.5734(3) 0.035(2) Uani 1 1 d . . . C17 C 0.2111(7) 0.7948(7) 0.5795(4) 0.045(3) Uani 1 1 d . . . H17 H 0.1693 0.8229 0.5584 0.053 Uiso 1 1 calc R . . C18 C 0.2180(8) 0.8055(8) 0.6234(4) 0.057(4) Uani 1 1 d . . . H18 H 0.1821 0.8425 0.6368 0.069 Uiso 1 1 calc R . . C19 C 0.2898(8) 0.7494(9) 0.6431(4) 0.053(3) Uani 1 1 d . . . H19 H 0.3090 0.7432 0.6722 0.063 Uiso 1 1 calc R . . C20 C 0.3275(6) 0.7048(7) 0.6126(3) 0.036(2) Uani 1 1 d . . . H20 H 0.3754 0.6639 0.6175 0.044 Uiso 1 1 calc R . . C1A C 0.7428(6) 0.6617(6) 0.5304(3) 0.031(2) Uani 1 1 d . . . C2A C 0.8241(7) 0.6276(7) 0.5261(3) 0.036(2) Uani 1 1 d . . . H2A H 0.8563 0.5913 0.5474 0.044 Uiso 1 1 calc R . . C3A C 0.8599(8) 0.6458(8) 0.4910(4) 0.051(3) Uani 1 1 d . . . H3A H 0.9160 0.6224 0.4881 0.061 Uiso 1 1 calc R . . C4A C 0.8112(8) 0.6990(9) 0.4603(4) 0.053(3) Uani 1 1 d . . . H4A H 0.8350 0.7127 0.4365 0.063 Uiso 1 1 calc R . . C5A C 0.7309(9) 0.7317(8) 0.4636(3) 0.052(3) Uani 1 1 d . . . H5A H 0.6983 0.7666 0.4419 0.063 Uiso 1 1 calc R . . C6A C 0.6954(7) 0.7141(7) 0.4992(3) 0.043(3) Uani 1 1 d . . . H6A H 0.6394 0.7380 0.5018 0.051 Uiso 1 1 calc R . . C1B C 0.6603(7) 0.7371(7) 0.5928(3) 0.037(3) Uani 1 1 d . . . C2B C 0.7238(8) 0.8041(8) 0.6036(4) 0.055(3) Uani 1 1 d . . . H2B H 0.7840 0.7939 0.6017 0.066 Uiso 1 1 calc R . . C3B C 0.6980(9) 0.8850(9) 0.6170(5) 0.072(4) Uani 1 1 d . . . H3B H 0.7411 0.9304 0.6243 0.086 Uiso 1 1 calc R . . C4B C 0.6112(10) 0.9012(10) 0.6200(4) 0.068(4) Uani 1 1 d . . . H4B H 0.5948 0.9570 0.6295 0.082 Uiso 1 1 calc R . . C5B C 0.5482(9) 0.8362(10) 0.6091(4) 0.065(4) Uani 1 1 d . . . H5B H 0.4879 0.8471 0.6105 0.077 Uiso 1 1 calc R . . C6B C 0.5737(7) 0.7541(8) 0.5959(3) 0.048(3) Uani 1 1 d . . . H6B H 0.5303 0.7089 0.5889 0.057 Uiso 1 1 calc R . . C1C C 0.7094(7) 0.3062(8) 0.6835(4) 0.043(3) Uani 1 1 d . . . C2C C 0.7125(9) 0.2668(9) 0.6455(4) 0.062(4) Uani 1 1 d . . . H2C H 0.6713 0.2838 0.6215 0.074 Uiso 1 1 calc R . . C3C C 0.7765(11) 0.2024(11) 0.6430(6) 0.085(5) Uani 1 1 d . . . H3C H 0.7783 0.1744 0.6174 0.102 Uiso 1 1 calc R . . C4C C 0.8366(10) 0.1796(11) 0.6778(7) 0.091(6) Uani 1 1 d . . . H4C H 0.8808 0.1365 0.6759 0.109 Uiso 1 1 calc R . . C5C C 0.8343(10) 0.2173(10) 0.7146(7) 0.087(6) Uani 1 1 d . . . H5C H 0.8767 0.2004 0.7383 0.104 Uiso 1 1 calc R . . C6C C 0.7691(8) 0.2820(9) 0.7183(5) 0.065(4) Uani 1 1 d . . . H6C H 0.7669 0.3080 0.7443 0.078 Uiso 1 1 calc R . . C1D C 0.5634(6) 0.3663(7) 0.7247(3) 0.031(2) Uani 1 1 d . . . C2D C 0.4915(7) 0.3064(8) 0.7136(3) 0.044(3) Uani 1 1 d . . . H2D H 0.4791 0.2803 0.6869 0.053 Uiso 1 1 calc R . . C3D C 0.4406(8) 0.2869(8) 0.7422(4) 0.048(3) Uani 1 1 d . . . H3D H 0.3914 0.2480 0.7347 0.058 Uiso 1 1 calc R . . C4D C 0.4586(9) 0.3220(8) 0.7817(4) 0.056(3) Uani 1 1 d . . . H4D H 0.4226 0.3072 0.8012 0.068 Uiso 1 1 calc R . . C5D C 0.5312(9) 0.3801(9) 0.7924(4) 0.063(4) Uani 1 1 d . . . H5D H 0.5456 0.4032 0.8197 0.076 Uiso 1 1 calc R . . C6D C 0.5812(8) 0.4035(9) 0.7637(3) 0.054(3) Uani 1 1 d . . . H6D H 0.6280 0.4453 0.7707 0.065 Uiso 1 1 calc R . . C1E C 0.3069(7) 0.5069(8) 0.6935(3) 0.042(3) Uani 1 1 d . . . C2E C 0.3926(7) 0.5460(9) 0.6988(4) 0.056(3) Uani 1 1 d . . . H2E H 0.4237 0.5472 0.6765 0.067 Uiso 1 1 calc R . . C3E C 0.4304(10) 0.5823(11) 0.7365(5) 0.084(5) Uani 1 1 d . . . H3E H 0.4869 0.6100 0.7398 0.100 Uiso 1 1 calc R . . C4E C 0.3869(11) 0.5786(11) 0.7693(4) 0.079(5) Uani 1 1 d . . . H4E H 0.4131 0.6052 0.7949 0.095 Uiso 1 1 calc R . . C5E C 0.3066(11) 0.5372(11) 0.7656(4) 0.079(5) Uani 1 1 d . . . H5E H 0.2786 0.5332 0.7889 0.095 Uiso 1 1 calc R . . C6E C 0.2652(8) 0.5008(9) 0.7278(3) 0.050(3) Uani 1 1 d . . . H6E H 0.2093 0.4722 0.7253 0.060 Uiso 1 1 calc R . . C1F C 0.1896(6) 0.3680(7) 0.6543(3) 0.034(2) Uani 1 1 d . . . C2F C 0.2310(8) 0.2858(8) 0.6579(4) 0.049(3) Uani 1 1 d . . . H2F H 0.2906 0.2806 0.6541 0.059 Uiso 1 1 calc R . . C3F C 0.1853(8) 0.2109(8) 0.6671(4) 0.057(3) Uani 1 1 d . . . H3F H 0.2130 0.1543 0.6688 0.069 Uiso 1 1 calc R . . C4F C 0.0993(8) 0.2197(9) 0.6738(4) 0.057(3) Uani 1 1 d . . . H4F H 0.0678 0.1686 0.6797 0.068 Uiso 1 1 calc R . . C5F C 0.0590(8) 0.3006(9) 0.6720(4) 0.060(4) Uani 1 1 d . . . H5F H 0.0009 0.3068 0.6777 0.072 Uiso 1 1 calc R . . C6F C 0.1054(7) 0.3744(8) 0.6615(4) 0.049(3) Uani 1 1 d . . . H6F H 0.0772 0.4307 0.6594 0.059 Uiso 1 1 calc R . . C1G C 0.3606(7) 0.7820(7) 0.5019(3) 0.040(3) Uani 1 1 d . . . C2G C 0.4084(7) 0.7575(7) 0.4720(4) 0.047(3) Uani 1 1 d . . . H2G H 0.4128 0.6966 0.4654 0.056 Uiso 1 1 calc R . . C3G C 0.4501(9) 0.8203(9) 0.4516(4) 0.059(4) Uani 1 1 d . . . H3G H 0.4861 0.8027 0.4325 0.071 Uiso 1 1 calc R . . C4G C 0.4382(9) 0.9091(9) 0.4596(4) 0.061(4) Uani 1 1 d . . . H4G H 0.4632 0.9527 0.4445 0.074 Uiso 1 1 calc R . . C5G C 0.3916(9) 0.9351(8) 0.4886(5) 0.066(4) Uani 1 1 d . . . H5G H 0.3843 0.9964 0.4936 0.079 Uiso 1 1 calc R . . C6G C 0.3543(8) 0.8713(8) 0.5111(4) 0.052(3) Uani 1 1 d . . . H6G H 0.3247 0.8892 0.5326 0.063 Uiso 1 1 calc R . . C1H C 0.1956(6) 0.6869(7) 0.4878(3) 0.036(2) Uani 1 1 d . . . C2H C 0.1607(7) 0.6064(8) 0.4754(4) 0.046(3) Uani 1 1 d . . . H2H H 0.1924 0.5544 0.4856 0.055 Uiso 1 1 calc R . . C3H C 0.0791(8) 0.5985(9) 0.4480(4) 0.053(3) Uani 1 1 d . . . H3H H 0.0561 0.5420 0.4389 0.063 Uiso 1 1 calc R . . C4H C 0.0324(8) 0.6759(10) 0.4346(4) 0.055(3) Uani 1 1 d . . . H4H H -0.0235 0.6715 0.4164 0.066 Uiso 1 1 calc R . . C5H C 0.0653(8) 0.7574(10) 0.4469(5) 0.067(4) Uani 1 1 d . . . H5H H 0.0318 0.8090 0.4378 0.080 Uiso 1 1 calc R . . C6H C 0.1475(8) 0.7651(8) 0.4727(4) 0.053(3) Uani 1 1 d . . . H6H H 0.1718 0.8219 0.4804 0.064 Uiso 1 1 calc R . . S1 S 0.4114(2) 0.1126(2) 0.63672(10) 0.0521(8) Uani 1 1 d . . . O1 O 0.3834(6) 0.1034(7) 0.6764(3) 0.071(3) Uani 1 1 d . . . O2 O 0.4936(7) 0.0685(7) 0.6331(3) 0.093(4) Uani 1 1 d . . . O3 O 0.4042(5) 0.2009(5) 0.6197(3) 0.056(2) Uani 1 1 d . . . C21 C 0.3315(13) 0.0532(10) 0.6014(6) 0.082(5) Uani 1 1 d . . . F1 F 0.3305(10) -0.0343(7) 0.6119(4) 0.166(6) Uani 1 1 d . . . F2 F 0.2482(7) 0.0821(8) 0.5993(3) 0.111(4) Uani 1 1 d . . . F3 F 0.3446(8) 0.0565(6) 0.5620(3) 0.111(4) Uani 1 1 d . . . S2 S 1.0012(4) 0.8265(4) 0.69115(16) 0.0718(15) Uani 0.70 1 d PD A 1 O4 O 1.0944(8) 0.8480(11) 0.6974(5) 0.088(5) Uani 0.70 1 d PDU A 1 O5 O 0.9727(15) 0.7549(10) 0.7158(5) 0.154(9) Uani 0.70 1 d PDU A 1 O6 O 0.9504(9) 0.8290(9) 0.6495(3) 0.056(3) Uani 0.70 1 d PDU A 1 F4 F 0.9994(13) 0.9332(13) 0.7532(4) 0.129(6) Uani 0.70 1 d PDU A 1 F6 F 0.8722(10) 0.9201(14) 0.7123(6) 0.162(8) Uani 0.70 1 d PDU A 1 F5 F 0.9793(19) 0.9969(9) 0.6956(8) 0.213(11) Uani 0.70 1 d PDU A 1 C22 C 0.9575(11) 0.9232(11) 0.7142(5) 0.101(9) Uani 0.70 1 d PD A 1 S2A S 1.0024(11) 0.9007(12) 0.6794(5) 0.100 Uiso 0.30 1 d PD B 2 O4A O 1.0942(14) 0.894(3) 0.6922(13) 0.150 Uiso 0.30 1 d PD B 2 O5A O 0.975(3) 0.9892(18) 0.6708(13) 0.150 Uiso 0.30 1 d PD B 2 O6A O 0.968(3) 0.844(3) 0.6459(9) 0.150 Uiso 0.30 1 d PD B 2 C22A C 0.9537(19) 0.8642(19) 0.7212(8) 0.100 Uiso 0.30 1 d PD B 2 F4A F 0.978(3) 0.911(3) 0.7557(8) 0.150 Uiso 0.30 1 d PD B 2 F5A F 0.979(3) 0.780(2) 0.7333(12) 0.150 Uiso 0.30 1 d PD B 2 F6A F 0.8660(17) 0.859(3) 0.7142(12) 0.150 Uiso 0.30 1 d PD B 2 C1S C 0.0521(10) 0.0631(10) 0.4318(6) 0.088(5) Uani 1 1 d . . . H1S H 0.0490 0.0835 0.4027 0.105 Uiso 1 1 calc R . . Cl2 Cl 0.1463(4) -0.0010(4) 0.4460(3) 0.183(4) Uani 1 1 d . . . Cl3 Cl -0.0435(4) 0.0015(4) 0.4340(3) 0.156(3) Uani 1 1 d . . . Cl4 Cl 0.0562(4) 0.1556(4) 0.46328(19) 0.138(2) 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 0.0233(2) 0.0405(3) 0.0389(2) 0.00642(18) 0.00768(16) 0.00026(16) Au2 0.0259(2) 0.0401(3) 0.0290(2) 0.00034(17) 0.00723(15) 0.00066(16) Au3 0.0254(2) 0.0380(2) 0.0346(2) -0.00079(17) 0.01196(16) 0.00137(16) Au4 0.0266(2) 0.0330(2) 0.0385(2) 0.00167(17) 0.00886(17) 0.00189(15) S3 0.0259(13) 0.0376(15) 0.0282(13) -0.0030(10) 0.0075(10) 0.0039(10) Fe1 0.0248(7) 0.0389(9) 0.0317(8) 0.0023(6) 0.0094(6) 0.0004(6) Fe2 0.0283(8) 0.0351(9) 0.0454(9) -0.0026(7) 0.0171(7) -0.0017(6) P1 0.0247(13) 0.0371(16) 0.0368(15) 0.0053(12) 0.0098(11) 0.0014(10) P2 0.0250(13) 0.0420(17) 0.0301(14) 0.0042(12) 0.0072(11) -0.0016(11) P3 0.0264(14) 0.0385(16) 0.0339(15) -0.0002(12) 0.0100(11) -0.0002(11) P4 0.0292(14) 0.0332(16) 0.0376(15) 0.0014(12) 0.0105(12) -0.0002(11) C1 0.025(5) 0.039(6) 0.032(5) 0.002(4) 0.011(4) 0.003(4) C2 0.033(6) 0.035(6) 0.054(7) 0.003(5) 0.024(5) -0.009(4) C3 0.020(6) 0.086(10) 0.041(7) 0.009(6) 0.009(5) 0.008(6) C4 0.038(7) 0.049(8) 0.049(7) 0.015(6) 0.019(5) 0.012(5) C5 0.035(6) 0.041(7) 0.021(5) 0.008(4) 0.016(4) 0.010(4) C6 0.028(6) 0.056(7) 0.028(5) -0.003(5) 0.014(4) -0.003(5) C7 0.029(6) 0.074(9) 0.033(6) 0.004(6) 0.004(5) -0.010(5) C8 0.066(9) 0.054(8) 0.042(7) -0.021(6) 0.017(6) -0.028(7) C9 0.055(8) 0.039(7) 0.067(8) -0.009(6) 0.035(7) 0.001(6) C10 0.032(6) 0.037(7) 0.041(6) -0.003(5) 0.014(5) 0.000(4) C11 0.019(5) 0.022(5) 0.052(7) 0.007(4) 0.014(4) -0.001(4) C12 0.036(6) 0.053(8) 0.053(7) -0.003(6) 0.029(5) 0.006(5) C13 0.028(6) 0.035(7) 0.095(10) 0.011(6) 0.029(6) 0.005(5) C14 0.023(6) 0.051(8) 0.068(8) 0.022(6) 0.009(5) 0.000(5) C15 0.032(6) 0.020(5) 0.039(6) -0.003(4) 0.004(4) -0.008(4) C16 0.038(6) 0.023(6) 0.049(7) -0.005(5) 0.020(5) -0.011(4) C17 0.043(7) 0.033(7) 0.065(8) 0.005(6) 0.029(6) 0.001(5) C18 0.062(9) 0.036(7) 0.085(10) -0.027(7) 0.040(7) -0.013(6) C19 0.047(7) 0.066(9) 0.044(7) -0.028(6) 0.007(6) -0.024(6) C20 0.018(5) 0.042(7) 0.051(7) -0.007(5) 0.014(5) -0.009(4) C1A 0.026(5) 0.033(6) 0.036(6) -0.002(4) 0.007(4) -0.008(4) C2A 0.040(6) 0.038(6) 0.032(6) 0.003(5) 0.010(5) 0.003(5) C3A 0.050(7) 0.054(8) 0.055(8) -0.002(6) 0.025(6) 0.002(6) C4A 0.055(8) 0.068(9) 0.036(7) 0.001(6) 0.010(6) -0.013(6) C5A 0.072(9) 0.045(8) 0.034(7) 0.017(5) -0.003(6) -0.005(6) C6A 0.042(7) 0.048(7) 0.038(6) 0.007(5) 0.006(5) 0.000(5) C1B 0.043(6) 0.041(7) 0.030(6) 0.011(5) 0.010(5) 0.017(5) C2B 0.057(8) 0.042(8) 0.073(9) -0.002(6) 0.030(7) 0.007(6) C3B 0.069(10) 0.042(8) 0.108(12) -0.014(8) 0.028(9) 0.002(7) C4B 0.090(12) 0.061(10) 0.058(9) -0.005(7) 0.026(8) 0.028(8) C5B 0.051(9) 0.079(11) 0.064(9) -0.005(8) 0.012(7) 0.026(7) C6B 0.036(6) 0.060(8) 0.045(7) -0.004(6) 0.002(5) 0.018(5) C1C 0.026(6) 0.045(7) 0.061(8) 0.008(6) 0.014(5) -0.001(5) C2C 0.058(9) 0.068(10) 0.064(9) 0.006(7) 0.023(7) 0.021(7) C3C 0.088(13) 0.080(12) 0.097(13) 0.004(10) 0.044(11) 0.026(9) C4C 0.051(10) 0.059(11) 0.17(2) 0.023(12) 0.048(12) 0.014(8) C5C 0.050(9) 0.052(10) 0.147(18) 0.029(11) -0.013(10) 0.004(7) C6C 0.041(8) 0.063(9) 0.089(11) 0.018(8) 0.007(7) 0.000(6) C1D 0.032(6) 0.036(6) 0.027(5) 0.006(4) 0.008(4) 0.005(4) C2D 0.053(7) 0.055(8) 0.029(6) -0.007(5) 0.016(5) -0.010(5) C3D 0.048(7) 0.048(8) 0.050(7) 0.000(6) 0.012(6) -0.019(5) C4D 0.077(9) 0.054(8) 0.047(7) -0.001(6) 0.033(7) -0.021(7) C5D 0.081(10) 0.069(10) 0.047(8) -0.017(7) 0.029(7) -0.034(7) C6D 0.057(8) 0.073(9) 0.035(6) -0.010(6) 0.016(6) -0.030(6) C1E 0.027(6) 0.065(8) 0.033(6) -0.011(5) 0.004(5) -0.005(5) C2E 0.030(6) 0.080(10) 0.056(8) -0.001(7) 0.006(6) -0.001(6) C3E 0.051(9) 0.103(13) 0.080(11) -0.028(9) -0.028(8) -0.004(8) C4E 0.088(12) 0.101(13) 0.043(8) -0.030(8) -0.001(8) 0.015(9) C5E 0.079(12) 0.114(14) 0.045(8) -0.023(8) 0.018(8) 0.009(9) C6E 0.042(7) 0.078(9) 0.030(6) -0.009(6) 0.007(5) -0.003(6) C1F 0.025(5) 0.057(7) 0.022(5) 0.003(5) 0.006(4) -0.003(5) C2F 0.040(7) 0.058(8) 0.057(8) 0.013(6) 0.028(6) 0.006(6) C3F 0.062(9) 0.046(8) 0.071(9) 0.015(6) 0.030(7) 0.009(6) C4F 0.045(8) 0.056(9) 0.072(9) 0.030(7) 0.015(6) 0.000(6) C5F 0.028(6) 0.071(10) 0.083(10) 0.025(7) 0.017(6) 0.000(6) C6F 0.043(7) 0.040(7) 0.069(8) -0.001(6) 0.024(6) -0.003(5) C1G 0.030(6) 0.044(7) 0.049(7) 0.009(5) 0.015(5) -0.001(4) C2G 0.057(7) 0.029(6) 0.065(8) 0.009(5) 0.043(6) 0.010(5) C3G 0.074(9) 0.045(8) 0.070(9) 0.004(7) 0.042(7) 0.000(6) C4G 0.069(9) 0.065(10) 0.055(8) 0.016(7) 0.023(7) -0.017(7) C5G 0.087(11) 0.032(7) 0.089(11) -0.005(7) 0.042(9) -0.013(6) C6G 0.066(8) 0.033(7) 0.065(8) -0.007(6) 0.033(7) -0.008(6) C1H 0.025(5) 0.046(7) 0.035(6) 0.003(5) 0.004(4) -0.005(4) C2H 0.043(7) 0.042(7) 0.057(8) -0.011(6) 0.018(6) 0.004(5) C3H 0.047(7) 0.066(9) 0.045(7) -0.024(6) 0.008(6) -0.011(6) C4H 0.043(7) 0.078(10) 0.045(7) -0.004(7) 0.011(6) -0.003(7) C5H 0.036(7) 0.066(10) 0.093(11) 0.018(8) -0.005(7) 0.010(6) C6H 0.049(8) 0.032(7) 0.075(9) 0.010(6) 0.004(6) 0.004(5) S1 0.060(2) 0.051(2) 0.0451(18) 0.0034(14) 0.0086(15) 0.0201(15) O1 0.068(6) 0.095(8) 0.053(6) 0.013(5) 0.020(5) 0.026(5) O2 0.103(8) 0.117(9) 0.065(7) 0.012(6) 0.034(6) 0.077(7) O3 0.057(5) 0.048(5) 0.060(5) 0.000(4) 0.006(4) 0.006(4) C21 0.103(14) 0.048(10) 0.101(14) -0.007(8) 0.035(11) -0.023(8) F1 0.276(17) 0.045(6) 0.168(12) 0.002(7) 0.017(11) -0.056(8) F2 0.080(7) 0.154(10) 0.097(7) -0.028(7) 0.009(6) -0.060(7) F3 0.187(11) 0.088(7) 0.056(6) -0.034(5) 0.017(6) -0.006(6) S2 0.068(4) 0.091(4) 0.055(3) -0.020(3) 0.009(3) 0.003(3) O4 0.056(8) 0.132(13) 0.084(10) -0.016(9) 0.030(7) 0.007(8) O5 0.202(16) 0.132(14) 0.099(13) 0.050(11) -0.048(11) -0.082(12) O6 0.063(8) 0.069(8) 0.035(6) -0.018(6) 0.005(6) -0.008(6) F4 0.153(13) 0.175(14) 0.061(8) -0.065(9) 0.029(8) -0.030(10) F6 0.113(12) 0.223(16) 0.164(14) -0.066(12) 0.066(11) 0.055(11) F5 0.260(19) 0.136(15) 0.227(19) -0.010(14) 0.004(15) 0.038(14) C22 0.13(2) 0.12(2) 0.063(16) -0.045(15) 0.026(16) 0.021(18) C1S 0.083(12) 0.062(11) 0.128(15) 0.015(10) 0.045(10) -0.009(8) Cl2 0.108(4) 0.096(4) 0.361(11) 0.081(6) 0.087(6) 0.034(3) Cl3 0.090(4) 0.093(4) 0.285(9) 0.006(5) 0.038(5) -0.013(3) Cl4 0.172(6) 0.090(4) 0.142(5) -0.015(3) 0.003(4) 0.004(4) _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 2.277(3) . ? Au1 S3 2.406(3) . ? Au1 Au2 2.8618(6) . ? Au1 Au4 2.9541(6) . ? Au2 P2 2.251(3) . ? Au2 S3 2.398(2) . ? Au2 Au3 2.8446(6) . ? Au3 P3 2.265(2) . ? Au3 S3 2.428(2) . ? Au3 Au4 2.8970(6) . ? Au4 P4 2.259(3) . ? Au4 S3 2.360(2) . ? Fe1 C1 2.018(9) . ? Fe1 C6 2.022(9) . ? Fe1 C3 2.022(10) . ? Fe1 C5 2.024(9) . ? Fe1 C4 2.029(10) . ? Fe1 C2 2.031(9) . ? Fe1 C10 2.031(9) . ? Fe1 C9 2.043(11) . ? Fe1 C7 2.051(10) . ? Fe1 C8 2.054(11) . ? Fe2 C16 2.020(9) . ? Fe2 C17 2.022(11) . ? Fe2 C13 2.024(10) . ? Fe2 C12 2.035(10) . ? Fe2 C11 2.036(9) . ? Fe2 C14 2.038(11) . ? Fe2 C20 2.047(9) . ? Fe2 C19 2.048(11) . ? Fe2 C18 2.053(11) . ? Fe2 C15 2.053(9) . ? P1 C1 1.780(10) . ? P1 C1B 1.790(11) . ? P1 C1A 1.797(9) . ? P2 C6 1.792(11) . ? P2 C1D 1.812(9) . ? P2 C1C 1.813(11) . ? P3 C11 1.788(9) . ? P3 C1E 1.789(10) . ? P3 C1F 1.812(10) . ? P4 C16 1.793(10) . ? P4 C1G 1.806(10) . ? P4 C1H 1.811(10) . ? C1 C5 1.430(14) . ? C1 C2 1.444(14) . ? C2 C3 1.402(15) . ? C3 C4 1.379(16) . ? C4 C5 1.411(14) . ? C6 C10 1.398(15) . ? C6 C7 1.433(14) . ? C7 C8 1.401(16) . ? C8 C9 1.405(17) . ? C9 C10 1.433(15) . ? C11 C15 1.424(14) . ? C11 C12 1.442(13) . ? C12 C13 1.415(16) . ? C13 C14 1.390(16) . ? C14 C15 1.397(14) . ? C16 C20 1.407(15) . ? C16 C17 1.435(14) . ? C17 C18 1.424(16) . ? C18 C19 1.427(18) . ? C19 C20 1.407(14) . ? C1A C2A 1.366(13) . ? C1A C6A 1.374(14) . ? C2A C3A 1.386(14) . ? C3A C4A 1.378(16) . ? C4A C5A 1.335(16) . ? C5A C6A 1.394(14) . ? C1B C6B 1.360(13) . ? C1B C2B 1.388(16) . ? C2B C3B 1.368(16) . ? C3B C4B 1.360(18) . ? C4B C5B 1.362(19) . ? C5B C6B 1.379(17) . ? C1C C6C 1.358(17) . ? C1C C2C 1.381(16) . ? C2C C3C 1.381(18) . ? C3C C4C 1.36(2) . ? C4C C5C 1.33(2) . ? C5C C6C 1.405(19) . ? C1D C6D 1.369(14) . ? C1D C2D 1.404(14) . ? C2D C3D 1.350(13) . ? C3D C4D 1.369(15) . ? C4D C5D 1.394(16) . ? C5D C6D 1.359(14) . ? C1E C6E 1.390(14) . ? C1E C2E 1.405(15) . ? C2E C3E 1.366(18) . ? C3E C4E 1.36(2) . ? C4E C5E 1.35(2) . ? C5E C6E 1.384(17) . ? C1F C6F 1.345(13) . ? C1F C2F 1.373(15) . ? C2F C3F 1.379(16) . ? C3F C4F 1.369(15) . ? C4F C5F 1.352(17) . ? C5F C6F 1.385(15) . ? C1G C2G 1.371(13) . ? C1G C6G 1.374(15) . ? C2G C3G 1.372(15) . ? C3G C4G 1.371(17) . ? C4G C5G 1.340(17) . ? C5G C6G 1.388(16) . ? C1H C2H 1.344(15) . ? C1H C6H 1.414(15) . ? C2H C3H 1.387(16) . ? C3H C4H 1.382(17) . ? C4H C5H 1.348(18) . ? C5H C6H 1.370(16) . ? S1 O3 1.427(8) . ? S1 O2 1.435(9) . ? S1 O1 1.442(9) . ? S1 C21 1.747(17) . ? C21 F2 1.324(18) . ? C21 F3 1.338(18) . ? C21 F1 1.351(17) . ? S2 O4 1.426(12) . ? S2 O6 1.429(11) . ? S2 O5 1.452(14) . ? S2 C22 1.812(14) . ? F4 C22 1.315(15) . ? F6 C22 1.285(15) . ? F5 C22 1.330(17) . ? S2A O4A 1.379(17) . ? S2A O5A 1.397(17) . ? S2A O6A 1.400(17) . ? S2A C22A 1.758(16) . ? C22A F6A 1.308(18) . ? C22A F4A 1.314(18) . ? C22A F5A 1.359(18) . ? C1S Cl2 1.709(17) . ? C1S Cl4 1.715(17) . ? C1S Cl3 1.731(15) . ? 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 S3 173.63(9) . . ? P1 Au1 Au2 120.32(7) . . ? S3 Au1 Au2 53.31(6) . . ? P1 Au1 Au4 132.47(7) . . ? S3 Au1 Au4 51.01(6) . . ? Au2 Au1 Au4 88.507(15) . . ? P2 Au2 S3 175.90(8) . . ? P2 Au2 Au3 129.67(6) . . ? S3 Au2 Au3 54.37(5) . . ? P2 Au2 Au1 124.55(7) . . ? S3 Au2 Au1 53.56(6) . . ? Au3 Au2 Au1 92.206(16) . . ? P3 Au3 S3 175.52(9) . . ? P3 Au3 Au2 127.18(7) . . ? S3 Au3 Au2 53.40(6) . . ? P3 Au3 Au4 124.27(7) . . ? S3 Au3 Au4 51.71(6) . . ? Au2 Au3 Au4 89.972(15) . . ? P4 Au4 S3 175.07(9) . . ? P4 Au4 Au3 121.44(6) . . ? S3 Au4 Au3 53.84(6) . . ? P4 Au4 Au1 128.79(7) . . ? S3 Au4 Au1 52.39(6) . . ? Au3 Au4 Au1 89.293(15) . . ? Au4 S3 Au2 117.10(10) . . ? Au4 S3 Au1 76.60(8) . . ? Au2 S3 Au1 73.13(7) . . ? Au4 S3 Au3 74.45(7) . . ? Au2 S3 Au3 72.24(7) . . ? Au1 S3 Au3 116.58(10) . . ? C1 Fe1 C6 133.5(4) . . ? C1 Fe1 C3 68.7(4) . . ? C6 Fe1 C3 147.3(5) . . ? C1 Fe1 C5 41.4(4) . . ? C6 Fe1 C5 110.9(4) . . ? C3 Fe1 C5 67.9(4) . . ? C1 Fe1 C4 69.1(4) . . ? C6 Fe1 C4 117.2(5) . . ? C3 Fe1 C4 39.8(5) . . ? C5 Fe1 C4 40.7(4) . . ? C1 Fe1 C2 41.8(4) . . ? C6 Fe1 C2 172.2(4) . . ? C3 Fe1 C2 40.5(4) . . ? C5 Fe1 C2 69.5(4) . . ? C4 Fe1 C2 68.5(4) . . ? C1 Fe1 C10 111.7(4) . . ? C6 Fe1 C10 40.4(4) . . ? C3 Fe1 C10 168.6(5) . . ? C5 Fe1 C10 120.5(4) . . ? C4 Fe1 C10 151.6(5) . . ? C2 Fe1 C10 132.3(4) . . ? C1 Fe1 C9 117.9(5) . . ? C6 Fe1 C9 68.7(4) . . ? C3 Fe1 C9 127.9(5) . . ? C5 Fe1 C9 152.8(5) . . ? C4 Fe1 C9 165.0(5) . . ? C2 Fe1 C9 107.2(5) . . ? C10 Fe1 C9 41.2(4) . . ? C1 Fe1 C7 171.7(5) . . ? C6 Fe1 C7 41.2(4) . . ? C3 Fe1 C7 113.2(4) . . ? C5 Fe1 C7 130.9(5) . . ? C4 Fe1 C7 106.8(5) . . ? C2 Fe1 C7 144.5(4) . . ? C10 Fe1 C7 68.2(4) . . ? C9 Fe1 C7 67.9(5) . . ? C1 Fe1 C8 148.3(5) . . ? C6 Fe1 C8 68.2(4) . . ? C3 Fe1 C8 105.4(5) . . ? C5 Fe1 C8 166.9(5) . . ? C4 Fe1 C8 127.1(5) . . ? C2 Fe1 C8 113.3(5) . . ? C10 Fe1 C8 68.0(5) . . ? C9 Fe1 C8 40.1(5) . . ? C7 Fe1 C8 39.9(5) . . ? C16 Fe2 C17 41.6(4) . . ? C16 Fe2 C13 148.5(5) . . ? C17 Fe2 C13 112.1(4) . . ? C16 Fe2 C12 170.7(5) . . ? C17 Fe2 C12 144.4(4) . . ? C13 Fe2 C12 40.8(4) . . ? C16 Fe2 C11 134.1(4) . . ? C17 Fe2 C11 170.6(5) . . ? C13 Fe2 C11 68.4(4) . . ? C12 Fe2 C11 41.5(4) . . ? C16 Fe2 C14 119.4(5) . . ? C17 Fe2 C14 106.2(5) . . ? C13 Fe2 C14 40.0(5) . . ? C12 Fe2 C14 68.3(5) . . ? C11 Fe2 C14 67.8(4) . . ? C16 Fe2 C20 40.5(4) . . ? C17 Fe2 C20 69.4(4) . . ? C13 Fe2 C20 165.9(5) . . ? C12 Fe2 C20 130.5(5) . . ? C11 Fe2 C20 112.5(4) . . ? C14 Fe2 C20 154.0(4) . . ? C16 Fe2 C19 67.6(4) . . ? C17 Fe2 C19 68.5(5) . . ? C13 Fe2 C19 126.3(5) . . ? C12 Fe2 C19 106.6(5) . . ? C11 Fe2 C19 119.3(5) . . ? C14 Fe2 C19 163.9(5) . . ? C20 Fe2 C19 40.2(4) . . ? C16 Fe2 C18 68.7(4) . . ? C17 Fe2 C18 40.9(5) . . ? C13 Fe2 C18 102.7(5) . . ? C12 Fe2 C18 112.0(5) . . ? C11 Fe2 C18 148.4(5) . . ? C14 Fe2 C18 125.5(5) . . ? C20 Fe2 C18 68.8(4) . . ? C19 Fe2 C18 40.7(5) . . ? C16 Fe2 C15 112.7(4) . . ? C17 Fe2 C15 130.1(5) . . ? C13 Fe2 C15 67.9(4) . . ? C12 Fe2 C15 69.2(4) . . ? C11 Fe2 C15 40.8(4) . . ? C14 Fe2 C15 40.0(4) . . ? C20 Fe2 C15 122.7(4) . . ? C19 Fe2 C15 154.3(5) . . ? C18 Fe2 C15 165.0(5) . . ? C1 P1 C1B 110.3(5) . . ? C1 P1 C1A 105.9(4) . . ? C1B P1 C1A 103.6(5) . . ? C1 P1 Au1 108.9(3) . . ? C1B P1 Au1 112.1(4) . . ? C1A P1 Au1 115.7(3) . . ? C6 P2 C1D 105.4(4) . . ? C6 P2 C1C 108.3(5) . . ? C1D P2 C1C 108.4(5) . . ? C6 P2 Au2 110.0(4) . . ? C1D P2 Au2 113.0(3) . . ? C1C P2 Au2 111.5(4) . . ? C11 P3 C1E 106.0(5) . . ? C11 P3 C1F 105.2(4) . . ? C1E P3 C1F 105.7(5) . . ? C11 P3 Au3 109.6(3) . . ? C1E P3 Au3 113.7(3) . . ? C1F P3 Au3 115.7(3) . . ? C16 P4 C1G 108.8(5) . . ? C16 P4 C1H 108.5(5) . . ? C1G P4 C1H 103.4(5) . . ? C16 P4 Au4 108.2(4) . . ? C1G P4 Au4 113.8(3) . . ? C1H P4 Au4 113.9(4) . . ? C5 C1 C2 107.0(9) . . ? C5 C1 P1 124.4(8) . . ? C2 C1 P1 128.6(8) . . ? C5 C1 Fe1 69.5(5) . . ? C2 C1 Fe1 69.6(5) . . ? P1 C1 Fe1 127.2(5) . . ? C3 C2 C1 106.4(10) . . ? C3 C2 Fe1 69.4(6) . . ? C1 C2 Fe1 68.6(5) . . ? C4 C3 C2 110.5(10) . . ? C4 C3 Fe1 70.4(6) . . ? C2 C3 Fe1 70.1(6) . . ? C3 C4 C5 108.2(10) . . ? C3 C4 Fe1 69.8(6) . . ? C5 C4 Fe1 69.5(5) . . ? C4 C5 C1 107.8(10) . . ? C4 C5 Fe1 69.8(6) . . ? C1 C5 Fe1 69.0(5) . . ? C10 C6 C7 107.9(10) . . ? C10 C6 P2 123.1(8) . . ? C7 C6 P2 129.0(9) . . ? C10 C6 Fe1 70.2(6) . . ? C7 C6 Fe1 70.5(6) . . ? P2 C6 Fe1 124.6(5) . . ? C8 C7 C6 107.5(11) . . ? C8 C7 Fe1 70.1(6) . . ? C6 C7 Fe1 68.3(6) . . ? C7 C8 C9 109.1(11) . . ? C7 C8 Fe1 70.0(6) . . ? C9 C8 Fe1 69.5(7) . . ? C8 C9 C10 107.2(11) . . ? C8 C9 Fe1 70.3(6) . . ? C10 C9 Fe1 69.0(6) . . ? C6 C10 C9 108.2(10) . . ? C6 C10 Fe1 69.5(5) . . ? C9 C10 Fe1 69.9(6) . . ? C15 C11 C12 108.1(9) . . ? C15 C11 P3 124.2(7) . . ? C12 C11 P3 127.7(8) . . ? C15 C11 Fe2 70.3(5) . . ? C12 C11 Fe2 69.2(6) . . ? P3 C11 Fe2 127.9(5) . . ? C13 C12 C11 106.1(10) . . ? C13 C12 Fe2 69.2(6) . . ? C11 C12 Fe2 69.3(5) . . ? C14 C13 C12 109.2(10) . . ? C14 C13 Fe2 70.5(6) . . ? C12 C13 Fe2 70.0(6) . . ? C13 C14 C15 109.5(10) . . ? C13 C14 Fe2 69.5(7) . . ? C15 C14 Fe2 70.6(6) . . ? C14 C15 C11 107.2(9) . . ? C14 C15 Fe2 69.4(6) . . ? C11 C15 Fe2 69.0(5) . . ? C20 C16 C17 109.2(9) . . ? C20 C16 P4 124.7(8) . . ? C17 C16 P4 126.1(9) . . ? C20 C16 Fe2 70.8(5) . . ? C17 C16 Fe2 69.3(5) . . ? P4 C16 Fe2 124.9(5) . . ? C18 C17 C16 107.1(11) . . ? C18 C17 Fe2 70.7(7) . . ? C16 C17 Fe2 69.1(6) . . ? C17 C18 C19 107.0(10) . . ? C17 C18 Fe2 68.4(6) . . ? C19 C18 Fe2 69.5(7) . . ? C20 C19 C18 109.7(11) . . ? C20 C19 Fe2 69.9(6) . . ? C18 C19 Fe2 69.8(6) . . ? C19 C20 C16 107.0(10) . . ? C19 C20 Fe2 69.9(6) . . ? C16 C20 Fe2 68.7(5) . . ? C2A C1A C6A 119.4(9) . . ? C2A C1A P1 121.5(8) . . ? C6A C1A P1 118.9(8) . . ? C1A C2A C3A 121.1(10) . . ? C4A C3A C2A 118.2(11) . . ? C5A C4A C3A 121.5(11) . . ? C4A C5A C6A 120.2(11) . . ? C1A C6A C5A 119.6(10) . . ? C6B C1B C2B 118.7(11) . . ? C6B C1B P1 121.0(9) . . ? C2B C1B P1 120.3(8) . . ? C3B C2B C1B 119.4(11) . . ? C4B C3B C2B 121.3(13) . . ? C3B C4B C5B 119.7(13) . . ? C4B C5B C6B 119.4(12) . . ? C1B C6B C5B 121.4(12) . . ? C6C C1C C2C 120.2(12) . . ? C6C C1C P2 122.3(10) . . ? C2C C1C P2 117.4(9) . . ? C3C C2C C1C 119.7(14) . . ? C4C C3C C2C 119.5(16) . . ? C5C C4C C3C 121.2(15) . . ? C4C C5C C6C 120.6(16) . . ? C1C C6C C5C 118.7(15) . . ? C6D C1D C2D 120.2(9) . . ? C6D C1D P2 123.2(8) . . ? C2D C1D P2 116.5(7) . . ? C3D C2D C1D 118.7(10) . . ? C2D C3D C4D 121.9(11) . . ? C3D C4D C5D 118.7(10) . . ? C6D C5D C4D 120.4(11) . . ? C5D C6D C1D 120.0(11) . . ? C6E C1E C2E 118.7(10) . . ? C6E C1E P3 121.0(8) . . ? C2E C1E P3 120.3(8) . . ? C3E C2E C1E 119.7(12) . . ? C4E C3E C2E 120.6(14) . . ? C5E C4E C3E 120.8(13) . . ? C4E C5E C6E 120.5(13) . . ? C5E C6E C1E 119.6(12) . . ? C6F C1F C2F 118.9(10) . . ? C6F C1F P3 122.7(9) . . ? C2F C1F P3 118.2(7) . . ? C1F C2F C3F 120.2(10) . . ? C4F C3F C2F 119.4(11) . . ? C5F C4F C3F 121.0(11) . . ? C4F C5F C6F 118.4(11) . . ? C1F C6F C5F 122.0(11) . . ? C2G C1G C6G 118.8(10) . . ? C2G C1G P4 117.7(9) . . ? C6G C1G P4 123.3(8) . . ? C1G C2G C3G 121.2(11) . . ? C4G C3G C2G 118.6(11) . . ? C5G C4G C3G 121.5(11) . . ? C4G C5G C6G 119.7(12) . . ? C1G C6G C5G 119.9(11) . . ? C2H C1H C6H 119.2(11) . . ? C2H C1H P4 120.4(9) . . ? C6H C1H P4 120.4(9) . . ? C1H C2H C3H 121.4(11) . . ? C4H C3H C2H 118.3(12) . . ? C5H C4H C3H 121.5(12) . . ? C4H C5H C6H 120.1(12) . . ? C5H C6H C1H 119.5(12) . . ? O3 S1 O2 113.3(6) . . ? O3 S1 O1 115.0(5) . . ? O2 S1 O1 116.1(5) . . ? O3 S1 C21 102.8(7) . . ? O2 S1 C21 102.5(8) . . ? O1 S1 C21 104.8(7) . . ? F2 C21 F3 104.6(15) . . ? F2 C21 F1 105.8(14) . . ? F3 C21 F1 106.9(14) . . ? F2 C21 S1 113.8(11) . . ? F3 C21 S1 113.7(11) . . ? F1 C21 S1 111.4(14) . . ? O4 S2 O6 118.0(9) . . ? O4 S2 O5 118.6(12) . . ? O6 S2 O5 112.5(10) . . ? O4 S2 C22 101.1(7) . . ? O6 S2 C22 101.6(7) . . ? O5 S2 C22 100.7(9) . . ? F6 C22 F4 110.3(16) . . ? F6 C22 F5 110(2) . . ? F4 C22 F5 103.3(19) . . ? F6 C22 S2 113.3(12) . . ? F4 C22 S2 110.1(12) . . ? F5 C22 S2 109.1(12) . . ? O4A S2A O5A 111.8(17) . . ? O4A S2A O6A 113.7(17) . . ? O5A S2A O6A 111.1(17) . . ? O4A S2A C22A 107.0(13) . . ? O5A S2A C22A 107.3(13) . . ? O6A S2A C22A 105.4(13) . . ? F6A C22A F4A 106.5(14) . . ? F6A C22A F5A 103.0(13) . . ? F4A C22A F5A 103.3(14) . . ? F6A C22A S2A 116.4(14) . . ? F4A C22A S2A 114.3(14) . . ? F5A C22A S2A 112.0(14) . . ? Cl2 C1S Cl4 110.9(11) . . ? Cl2 C1S Cl3 110.8(9) . . ? Cl4 C1S Cl3 109.8(9) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.851 _refine_diff_density_min -1.131 _refine_diff_density_rms 0.223 # Attachment '6334.cif' data_6334 _database_code_depnum_ccdc_archive 'CCDC 632235' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H39 Au2 Cl3 F6 Fe N2 O10 P2 S2' _chemical_formula_weight 1612.02 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' N N 0.0061 0.0033 '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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.596(3) _cell_length_b 15.116(6) _cell_length_c 21.344(8) _cell_angle_alpha 90.00 _cell_angle_beta 91.555(10) _cell_angle_gamma 90.00 _cell_volume 2772.4(17) _cell_formula_units_Z 2 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 845 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.931 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1556 _exptl_absorpt_coefficient_mu 5.892 _exptl_absorpt_correction_type 'Sadabs, (Sheldrick 2001)' _exptl_absorpt_correction_T_min 0.3854 _exptl_absorpt_correction_T_max 0.7188 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(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 18428 _diffrn_reflns_av_R_equivalents 0.1023 _diffrn_reflns_av_sigmaI/netI 0.1219 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6350 _reflns_number_gt 3886 _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^)+(0.0446P)^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 6350 _refine_ls_number_parameters 362 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1087 _refine_ls_R_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.1347 _refine_ls_wR_factor_gt 0.1179 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _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 0.88667(4) 0.56888(2) 0.620935(14) 0.04176(13) Uani 1 1 d . . . Fe1 Fe 0.5000 0.5000 0.5000 0.0479(5) Uani 1 2 d S . . P1 P 0.7994(2) 0.64436(15) 0.53659(9) 0.0343(5) Uani 1 1 d . . . N1 N 0.9694(9) 0.4935(5) 0.6966(3) 0.0449(19) Uani 1 1 d . . . O1 O 0.8876(9) 0.2348(5) 0.8185(3) 0.077(2) Uani 1 1 d . . . O2 O 0.7208(8) 0.2777(5) 0.7433(3) 0.064(2) Uani 1 1 d . . . H2 H 0.6737 0.2327 0.7544 0.096 Uiso 1 1 calc R . . C1 C 1.1061(15) 0.5100(8) 0.7253(5) 0.081(4) Uani 1 1 d . . . H1 H 1.1645 0.5593 0.7129 0.097 Uiso 1 1 calc R . . C2 C 1.1627(17) 0.4571(10) 0.7719(7) 0.117(6) Uani 1 1 d . . . H2A H 1.2607 0.4687 0.7908 0.141 Uiso 1 1 calc R . . C3 C 1.0739(15) 0.3851(9) 0.7919(5) 0.085(4) Uani 1 1 d . . . H3 H 1.1093 0.3495 0.8254 0.102 Uiso 1 1 calc R . . C4 C 0.9374(11) 0.3676(6) 0.7622(4) 0.047(2) Uani 1 1 d . . . C5 C 0.8864(12) 0.4233(6) 0.7160(4) 0.046(2) Uani 1 1 d . . . H5 H 0.7887 0.4124 0.6967 0.056 Uiso 1 1 calc R . . C6 C 0.8469(12) 0.2884(7) 0.7792(4) 0.050(2) Uani 1 1 d . . . C7 C 0.6907(10) 0.5754(6) 0.4826(4) 0.041(2) Uani 1 1 d . . . C8 C 0.5666(11) 0.5979(7) 0.4402(4) 0.053(3) Uani 1 1 d . . . H8 H 0.5176 0.6570 0.4360 0.064 Uiso 1 1 calc R . . C9 C 0.5253(15) 0.5219(10) 0.4047(4) 0.078(4) Uani 1 1 d . . . H9 H 0.4418 0.5183 0.3720 0.093 Uiso 1 1 calc R . . C10 C 0.6226(15) 0.4514(9) 0.4254(5) 0.077(4) Uani 1 1 d . . . H10 H 0.6193 0.3899 0.4095 0.093 Uiso 1 1 calc R . . C11 C 0.7251(12) 0.4843(7) 0.4730(4) 0.052(2) Uani 1 1 d . . . H11 H 0.8067 0.4498 0.4958 0.063 Uiso 1 1 calc R . . C1A C 0.6823(9) 0.7402(6) 0.5540(4) 0.039(2) Uani 1 1 d . . . C2A C 0.6588(13) 0.8064(7) 0.5098(5) 0.069(3) Uani 1 1 d . . . H2A1 H 0.7038 0.8008 0.4704 0.083 Uiso 1 1 calc R . . C3A C 0.5725(17) 0.8789(9) 0.5222(6) 0.097(5) Uani 1 1 d . . . H3A H 0.5506 0.9202 0.4902 0.116 Uiso 1 1 calc R . . C4A C 0.5152(13) 0.8929(9) 0.5827(5) 0.075(3) Uani 1 1 d . . . H4A H 0.4638 0.9456 0.5930 0.090 Uiso 1 1 calc R . . C5A C 0.5369(12) 0.8269(8) 0.6261(5) 0.063(3) Uani 1 1 d . . . H5A H 0.4953 0.8337 0.6661 0.076 Uiso 1 1 calc R . . C6A C 0.6186(10) 0.7505(7) 0.6128(4) 0.049(2) Uani 1 1 d . . . H6A H 0.6308 0.7059 0.6432 0.059 Uiso 1 1 calc R . . C1B C 0.9599(10) 0.6873(6) 0.4932(3) 0.038(2) Uani 1 1 d . . . C2B C 1.0868(10) 0.7192(7) 0.5260(4) 0.053(3) Uani 1 1 d . . . H2B H 1.0897 0.7163 0.5700 0.064 Uiso 1 1 calc R . . C3B C 1.2115(12) 0.7559(8) 0.4951(5) 0.073(3) Uani 1 1 d . . . H3B H 1.2994 0.7763 0.5179 0.087 Uiso 1 1 calc R . . C4B C 1.2051(12) 0.7624(8) 0.4298(5) 0.069(3) Uani 1 1 d . . . H4B H 1.2883 0.7867 0.4079 0.083 Uiso 1 1 calc R . . C5B C 1.0742(14) 0.7323(8) 0.3985(5) 0.069(3) Uani 1 1 d . . . H5B H 1.0660 0.7394 0.3548 0.082 Uiso 1 1 calc R . . C6B C 0.9560(11) 0.6925(7) 0.4288(4) 0.051(3) Uani 1 1 d . . . H6B H 0.8714 0.6686 0.4057 0.062 Uiso 1 1 calc R . . S1 S 0.4601(4) 0.0944(2) 0.71851(15) 0.0685(8) Uani 1 1 d . . . O3 O 0.5481(13) 0.0949(8) 0.6596(5) 0.134(4) Uani 1 1 d . . . O4 O 0.5410(10) 0.1406(6) 0.7660(3) 0.082(2) Uani 1 1 d . . . O5 O 0.3990(11) 0.0121(7) 0.7303(5) 0.122(4) Uani 1 1 d . . . C12 C 0.3035(17) 0.1678(12) 0.6961(6) 0.088(4) Uani 1 1 d . . . F1 F 0.3491(13) 0.2436(7) 0.6801(5) 0.164(5) Uani 1 1 d . . . F2 F 0.2187(12) 0.1351(10) 0.6490(5) 0.177(5) Uani 1 1 d . . . F3 F 0.2053(10) 0.1745(7) 0.7420(4) 0.139(4) Uani 1 1 d . . . C1S C 0.0087(15) 0.4518(14) 0.0386(7) 0.19(3) Uiso 0.50 1 d PD A -1 H1S H 0.0403 0.3891 0.0430 0.232 Uiso 0.50 1 calc PR A -1 Cl3 Cl -0.007(2) 0.4887(15) -0.0398(6) 0.215(7) Uani 0.50 1 d PD A -1 Cl2 Cl 0.1433(11) 0.5276(8) 0.0727(6) 0.151(4) Uani 0.50 1 d PD A -1 Cl1 Cl -0.1699(11) 0.4774(7) 0.0742(6) 0.157(4) Uani 0.50 1 d PD A -1 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 0.0431(2) 0.0386(2) 0.0431(2) 0.00488(16) -0.00938(14) 0.00003(19) Fe1 0.0502(12) 0.0510(13) 0.0419(10) 0.0004(8) -0.0084(8) -0.0189(10) P1 0.0322(12) 0.0317(13) 0.0386(11) -0.0003(8) -0.0061(9) -0.0019(10) N1 0.050(5) 0.044(5) 0.040(4) 0.005(3) -0.015(3) 0.005(4) O1 0.094(6) 0.066(6) 0.070(5) 0.031(4) -0.016(4) -0.001(5) O2 0.054(4) 0.066(5) 0.070(4) 0.028(4) -0.010(4) -0.008(4) C1 0.091(9) 0.064(9) 0.086(8) 0.021(6) -0.047(7) -0.030(7) C2 0.093(11) 0.092(12) 0.162(14) 0.056(10) -0.084(10) -0.038(9) C3 0.090(10) 0.070(9) 0.091(8) 0.030(7) -0.060(7) -0.015(8) C4 0.055(6) 0.042(6) 0.044(5) 0.003(4) -0.007(4) 0.013(5) C5 0.055(6) 0.033(6) 0.051(5) 0.006(4) -0.010(4) 0.000(5) C6 0.060(7) 0.049(7) 0.041(5) 0.000(4) -0.001(5) 0.005(5) C7 0.035(5) 0.046(6) 0.041(4) 0.011(4) -0.001(4) -0.006(5) C8 0.047(6) 0.064(7) 0.048(5) 0.017(4) -0.009(4) -0.006(5) C9 0.081(9) 0.112(12) 0.039(6) 0.002(6) -0.020(6) -0.048(8) C10 0.083(9) 0.092(10) 0.057(7) -0.016(6) 0.010(6) -0.034(8) C11 0.055(6) 0.042(6) 0.060(6) -0.011(4) -0.003(5) -0.011(5) C1A 0.032(5) 0.038(5) 0.048(5) -0.001(4) 0.001(4) 0.006(4) C2A 0.085(8) 0.049(7) 0.075(7) 0.019(5) 0.034(6) 0.016(6) C3A 0.117(12) 0.056(9) 0.119(11) 0.039(7) 0.034(9) 0.037(8) C4A 0.071(8) 0.075(9) 0.082(8) 0.004(7) 0.024(7) -0.001(7) C5A 0.054(7) 0.080(9) 0.057(6) -0.025(6) 0.006(5) 0.004(6) C6A 0.043(6) 0.060(7) 0.045(5) -0.001(4) -0.003(4) -0.006(5) C1B 0.036(5) 0.046(6) 0.032(4) -0.001(4) 0.003(4) -0.001(4) C2B 0.036(5) 0.071(8) 0.053(5) -0.006(5) -0.003(4) -0.016(5) C3B 0.044(6) 0.098(10) 0.076(8) 0.007(6) 0.001(5) -0.016(6) C4B 0.039(6) 0.087(10) 0.082(8) 0.004(6) 0.027(6) -0.003(6) C5B 0.071(8) 0.074(9) 0.063(6) -0.007(6) 0.030(6) 0.022(7) C6B 0.053(6) 0.058(7) 0.044(5) -0.012(4) 0.007(4) -0.005(5) S1 0.0636(19) 0.056(2) 0.086(2) 0.0013(15) 0.0011(16) 0.0003(16) O3 0.128(9) 0.132(10) 0.144(9) -0.036(7) 0.068(7) -0.023(7) O4 0.095(6) 0.070(6) 0.082(5) 0.020(4) -0.013(5) -0.013(5) O5 0.087(7) 0.087(8) 0.189(10) 0.056(7) -0.022(7) -0.027(6) C12 0.084(10) 0.122(14) 0.058(7) 0.030(8) 0.006(7) 0.021(9) F1 0.149(9) 0.112(9) 0.228(11) 0.087(8) -0.033(8) 0.015(7) F2 0.140(9) 0.264(16) 0.124(8) 0.021(8) -0.059(7) 0.022(10) F3 0.109(6) 0.173(10) 0.137(7) 0.025(6) 0.026(6) 0.064(7) Cl3 0.238(19) 0.23(2) 0.172(11) 0.075(11) -0.032(12) -0.023(14) Cl2 0.075(6) 0.152(11) 0.225(12) -0.008(8) -0.006(7) -0.006(6) Cl1 0.091(6) 0.126(9) 0.256(13) -0.051(8) 0.014(7) -0.003(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 N1 2.086(7) . ? Au1 P1 2.243(2) . ? Fe1 C7 2.039(8) 3_666 ? Fe1 C7 2.039(8) . ? Fe1 C8 2.047(9) . ? Fe1 C8 2.047(9) 3_666 ? Fe1 C11 2.048(10) 3_666 ? Fe1 C11 2.048(10) . ? Fe1 C10 2.068(11) . ? Fe1 C10 2.068(11) 3_666 ? Fe1 C9 2.077(10) . ? Fe1 C9 2.077(10) 3_666 ? P1 C7 1.797(9) . ? P1 C1B 1.803(8) . ? P1 C1A 1.809(9) . ? N1 C1 1.334(13) . ? N1 C5 1.350(11) . ? O1 C6 1.211(11) . ? O2 C6 1.321(11) . ? C1 C2 1.357(16) . ? C2 C3 1.402(17) . ? C3 C4 1.344(14) . ? C4 C5 1.359(12) . ? C4 C6 1.479(13) . ? C7 C8 1.422(12) . ? C7 C11 1.424(13) . ? C8 C9 1.415(15) . ? C9 C10 1.418(17) . ? C10 C11 1.417(14) . ? C1A C2A 1.386(13) . ? C1A C6A 1.390(10) . ? C2A C3A 1.353(15) . ? C3A C4A 1.411(15) . ? C4A C5A 1.370(15) . ? C5A C6A 1.386(13) . ? C1B C2B 1.368(12) . ? C1B C6B 1.376(11) . ? C2B C3B 1.390(13) . ? C3B C4B 1.395(14) . ? C4B C5B 1.370(15) . ? C5B C6B 1.359(14) . ? S1 O5 1.377(10) . ? S1 O4 1.400(8) . ? S1 O3 1.484(9) . ? S1 C12 1.799(14) . ? C12 F1 1.261(17) . ? C12 F3 1.315(13) . ? C12 F2 1.321(17) . ? C1S Cl3 1.765(10) . ? C1S Cl2 1.770(10) . ? C1S Cl1 1.774(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 N1 Au1 P1 177.3(2) . . ? C7 Fe1 C7 179.997(1) 3_666 . ? C7 Fe1 C8 139.3(3) 3_666 . ? C7 Fe1 C8 40.7(3) . . ? C7 Fe1 C8 40.7(3) 3_666 3_666 ? C7 Fe1 C8 139.3(3) . 3_666 ? C8 Fe1 C8 179.997(2) . 3_666 ? C7 Fe1 C11 40.8(4) 3_666 3_666 ? C7 Fe1 C11 139.2(4) . 3_666 ? C8 Fe1 C11 112.0(4) . 3_666 ? C8 Fe1 C11 68.0(4) 3_666 3_666 ? C7 Fe1 C11 139.2(4) 3_666 . ? C7 Fe1 C11 40.8(4) . . ? C8 Fe1 C11 68.0(4) . . ? C8 Fe1 C11 112.0(4) 3_666 . ? C11 Fe1 C11 179.998(2) 3_666 . ? C7 Fe1 C10 111.8(4) 3_666 . ? C7 Fe1 C10 68.2(4) . . ? C8 Fe1 C10 67.6(5) . . ? C8 Fe1 C10 112.4(5) 3_666 . ? C11 Fe1 C10 139.7(4) 3_666 . ? C11 Fe1 C10 40.3(4) . . ? C7 Fe1 C10 68.2(4) 3_666 3_666 ? C7 Fe1 C10 111.8(4) . 3_666 ? C8 Fe1 C10 112.4(5) . 3_666 ? C8 Fe1 C10 67.6(5) 3_666 3_666 ? C11 Fe1 C10 40.3(4) 3_666 3_666 ? C11 Fe1 C10 139.7(4) . 3_666 ? C10 Fe1 C10 179.998(3) . 3_666 ? C7 Fe1 C9 111.9(4) 3_666 . ? C7 Fe1 C9 68.1(4) . . ? C8 Fe1 C9 40.1(4) . . ? C8 Fe1 C9 139.9(4) 3_666 . ? C11 Fe1 C9 112.4(5) 3_666 . ? C11 Fe1 C9 67.6(5) . . ? C10 Fe1 C9 40.0(5) . . ? C10 Fe1 C9 140.0(5) 3_666 . ? C7 Fe1 C9 68.1(4) 3_666 3_666 ? C7 Fe1 C9 111.9(4) . 3_666 ? C8 Fe1 C9 139.9(4) . 3_666 ? C8 Fe1 C9 40.1(4) 3_666 3_666 ? C11 Fe1 C9 67.6(5) 3_666 3_666 ? C11 Fe1 C9 112.4(5) . 3_666 ? C10 Fe1 C9 140.0(5) . 3_666 ? C10 Fe1 C9 40.0(5) 3_666 3_666 ? C9 Fe1 C9 179.998(3) . 3_666 ? C7 P1 C1B 105.7(4) . . ? C7 P1 C1A 108.3(4) . . ? C1B P1 C1A 104.8(4) . . ? C7 P1 Au1 112.1(3) . . ? C1B P1 Au1 110.6(3) . . ? C1A P1 Au1 114.7(3) . . ? C1 N1 C5 118.2(8) . . ? C1 N1 Au1 122.0(7) . . ? C5 N1 Au1 119.7(6) . . ? N1 C1 C2 121.3(11) . . ? C1 C2 C3 119.5(12) . . ? C4 C3 C2 119.0(10) . . ? C3 C4 C5 118.7(10) . . ? C3 C4 C6 120.1(9) . . ? C5 C4 C6 121.2(9) . . ? N1 C5 C4 123.1(9) . . ? O1 C6 O2 122.5(10) . . ? O1 C6 C4 124.6(9) . . ? O2 C6 C4 112.7(8) . . ? C8 C7 C11 107.2(8) . . ? C8 C7 P1 129.6(8) . . ? C11 C7 P1 123.2(7) . . ? C8 C7 Fe1 69.9(5) . . ? C11 C7 Fe1 69.9(5) . . ? P1 C7 Fe1 127.9(4) . . ? C9 C8 C7 108.6(10) . . ? C9 C8 Fe1 71.1(6) . . ? C7 C8 Fe1 69.3(5) . . ? C8 C9 C10 107.9(10) . . ? C8 C9 Fe1 68.8(5) . . ? C10 C9 Fe1 69.6(6) . . ? C11 C10 C9 108.0(11) . . ? C11 C10 Fe1 69.1(6) . . ? C9 C10 Fe1 70.4(7) . . ? C10 C11 C7 108.3(10) . . ? C10 C11 Fe1 70.6(6) . . ? C7 C11 Fe1 69.3(5) . . ? C2A C1A C6A 118.6(9) . . ? C2A C1A P1 120.7(7) . . ? C6A C1A P1 120.7(7) . . ? C3A C2A C1A 121.5(10) . . ? C2A C3A C4A 120.4(11) . . ? C5A C4A C3A 117.7(11) . . ? C4A C5A C6A 121.9(10) . . ? C5A C6A C1A 119.5(9) . . ? C2B C1B C6B 119.2(8) . . ? C2B C1B P1 118.3(6) . . ? C6B C1B P1 122.4(7) . . ? C1B C2B C3B 120.8(9) . . ? C2B C3B C4B 119.5(10) . . ? C5B C4B C3B 118.2(9) . . ? C6B C5B C4B 121.9(10) . . ? C5B C6B C1B 120.2(10) . . ? O5 S1 O4 120.2(6) . . ? O5 S1 O3 111.4(7) . . ? O4 S1 O3 110.9(6) . . ? O5 S1 C12 108.6(7) . . ? O4 S1 C12 103.8(7) . . ? O3 S1 C12 99.6(6) . . ? F1 C12 F3 110.0(15) . . ? F1 C12 F2 107.6(12) . . ? F3 C12 F2 104.1(13) . . ? F1 C12 S1 113.4(11) . . ? F3 C12 S1 109.9(8) . . ? F2 C12 S1 111.4(12) . . ? Cl3 C1S Cl2 102.5(14) . . ? Cl3 C1S Cl1 107.0(12) . . ? Cl2 C1S Cl1 104.3(9) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.306 _refine_diff_density_min -0.720 _refine_diff_density_rms 0.175