# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 870559' #TrackingRef 'PerC6F4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H20 Co2 O6' _chemical_formula_weight 618.34 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' Co Co 0.3494 0.9721 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.818(7) _cell_length_b 14.019(11) _cell_length_c 22.704(18) _cell_angle_alpha 78.851(16) _cell_angle_beta 84.38(2) _cell_angle_gamma 89.824(19) _cell_volume 2740(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 979 _cell_measurement_theta_min 5.160 _cell_measurement_theta_max 35.148 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 1.255 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.739836 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details (G.M.Sheldrick,SADABS,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 18633 _diffrn_reflns_av_R_equivalents 0.0941 _diffrn_reflns_av_sigmaI/netI 0.1458 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 0.92 _diffrn_reflns_theta_max 23.56 _reflns_number_total 7968 _reflns_number_gt 3578 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0716P)^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 7968 _refine_ls_number_parameters 723 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1646 _refine_ls_R_factor_gt 0.0579 _refine_ls_wR_factor_ref 0.1735 _refine_ls_wR_factor_gt 0.1205 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _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 Co1 Co 0.30900(13) 0.89621(8) 0.32077(5) 0.0536(4) Uani 1 1 d . . . Co2 Co 0.29803(13) 0.74110(8) 0.28586(5) 0.0520(4) Uani 1 1 d . . . C21 C 0.2263(8) 0.8688(5) 0.2466(4) 0.043(2) Uani 1 1 d . . . C22 C 0.1337(9) 0.8318(5) 0.2959(4) 0.048(2) Uani 1 1 d . . . C31 C 0.5007(12) 0.9360(7) 0.2901(4) 0.065(3) Uani 1 1 d . . . C32 C 0.3194(11) 0.8412(7) 0.3984(5) 0.074(3) Uani 1 1 d . . . C33 C 0.2286(11) 1.0087(8) 0.3327(4) 0.080(3) Uani 1 1 d . . . C34 C 0.4959(11) 0.7357(6) 0.2570(4) 0.063(3) Uani 1 1 d . . . C35 C 0.2826(11) 0.6525(7) 0.3561(5) 0.073(3) Uani 1 1 d . . . C36 C 0.2185(11) 0.6678(7) 0.2413(4) 0.063(3) Uani 1 1 d . . . O1 O 0.6208(8) 0.9613(5) 0.2703(3) 0.087(2) Uani 1 1 d . . . O2 O 0.3297(10) 0.8073(6) 0.4473(3) 0.123(3) Uani 1 1 d . . . O3 O 0.1696(10) 1.0765(6) 0.3427(4) 0.132(3) Uani 1 1 d . . . O4 O 0.6219(8) 0.7323(5) 0.2397(3) 0.094(2) Uani 1 1 d . . . O5 O 0.2785(10) 0.5937(6) 0.3987(3) 0.123(3) Uani 1 1 d . . . O6 O 0.1676(8) 0.6205(5) 0.2119(3) 0.085(2) Uani 1 1 d . . . C1 C 0.2323(8) 0.9170(5) 0.1827(3) 0.0388(19) Uani 1 1 d . . . C2 C 0.3226(9) 0.8809(6) 0.1401(4) 0.052(2) Uani 1 1 d . . . H2 H 0.3872 0.8299 0.1525 0.062 Uiso 1 1 calc R . . C3 C 0.3212(9) 0.9182(6) 0.0785(4) 0.054(2) Uani 1 1 d . . . H3 H 0.3834 0.8904 0.0511 0.064 Uiso 1 1 calc R . . C4 C 0.2304(8) 0.9949(5) 0.0570(3) 0.0369(19) Uani 1 1 d . . . C5 C 0.1401(8) 1.0385(5) 0.1000(3) 0.0353(18) Uani 1 1 d . . . C6 C 0.1392(8) 1.0000(5) 0.1629(3) 0.0401(19) Uani 1 1 d . . . C7 C 0.0474(8) 1.0447(6) 0.2040(3) 0.047(2) Uani 1 1 d . . . H7 H 0.0427 1.0190 0.2451 0.057 Uiso 1 1 calc R . . C8 C -0.0335(9) 1.1243(6) 0.1842(4) 0.058(2) Uani 1 1 d . . . H8 H -0.0918 1.1535 0.2120 0.069 Uiso 1 1 calc R . . C9 C -0.0313(9) 1.1631(6) 0.1232(4) 0.057(2) Uani 1 1 d . . . H9 H -0.0868 1.2188 0.1110 0.069 Uiso 1 1 calc R . . C10 C 0.0513(8) 1.1216(5) 0.0795(3) 0.0381(19) Uani 1 1 d . . . C11 C 0.0470(8) 1.1598(5) 0.0145(3) 0.041(2) Uani 1 1 d . . . C12 C -0.0361(9) 1.2391(6) -0.0084(4) 0.051(2) Uani 1 1 d . . . H12 H -0.0912 1.2715 0.0186 0.061 Uiso 1 1 calc R . . C13 C -0.0418(9) 1.2734(7) -0.0702(4) 0.065(3) Uani 1 1 d . . . H13 H -0.0993 1.3276 -0.0836 0.078 Uiso 1 1 calc R . . C14 C 0.0368(9) 1.2275(6) -0.1105(4) 0.058(2) Uani 1 1 d . . . H14 H 0.0334 1.2503 -0.1516 0.070 Uiso 1 1 calc R . . C15 C 0.1233(8) 1.1455(6) -0.0905(4) 0.046(2) Uani 1 1 d . . . C16 C 0.1313(8) 1.1112(5) -0.0278(3) 0.0375(19) Uani 1 1 d . . . C17 C 0.2229(8) 1.0304(5) -0.0079(3) 0.0370(19) Uani 1 1 d . . . C18 C 0.3005(9) 0.9858(6) -0.0514(4) 0.052(2) Uani 1 1 d . . . H18 H 0.3608 0.9324 -0.0393 0.062 Uiso 1 1 calc R . . C19 C 0.2895(9) 1.0199(7) -0.1132(4) 0.058(2) Uani 1 1 d . . . H19 H 0.3417 0.9882 -0.1412 0.070 Uiso 1 1 calc R . . C20 C 0.2057(9) 1.0967(6) -0.1325(4) 0.051(2) Uani 1 1 d . . . H20 H 0.2012 1.1186 -0.1736 0.062 Uiso 1 1 calc R . . C23 C -0.0349(9) 0.8185(6) 0.3176(4) 0.058(2) Uani 1 1 d . . . H23A H -0.0792 0.8823 0.3157 0.069 Uiso 1 1 calc R . . H23B H -0.0834 0.7870 0.2897 0.069 Uiso 1 1 calc R . . C24 C -0.0724(10) 0.7608(7) 0.3798(4) 0.075(3) Uani 1 1 d . . . H24A H -0.0371 0.7967 0.4085 0.090 Uiso 1 1 calc R . . H24B H -0.0175 0.7002 0.3836 0.090 Uiso 1 1 calc R . . C25 C -0.2412(11) 0.7381(8) 0.3959(5) 0.103(4) Uani 1 1 d . . . H25A H -0.2943 0.7990 0.3948 0.123 Uiso 1 1 calc R . . H25B H -0.2774 0.7074 0.3651 0.123 Uiso 1 1 calc R . . C26 C -0.2837(14) 0.6749(10) 0.4553(6) 0.156(6) Uani 1 1 d . . . H26A H -0.2147 0.6216 0.4612 0.235 Uiso 1 1 calc R . . H26B H -0.3857 0.6503 0.4566 0.235 Uiso 1 1 calc R . . H26C H -0.2785 0.7118 0.4865 0.235 Uiso 1 1 calc R . . Co3 Co 0.61979(14) 0.35190(9) 0.34649(5) 0.0634(4) Uani 1 1 d . . . Co4 Co 0.90002(15) 0.36086(11) 0.32947(6) 0.0797(5) Uani 1 1 d . . . C71 C 0.7562(9) 0.3221(6) 0.2777(4) 0.054(2) Uani 1 1 d . . . C72 C 0.7692(10) 0.2531(6) 0.3257(4) 0.063(3) Uani 1 1 d . . . C91 C 0.5395(14) 0.4520(8) 0.3010(5) 0.100(4) Uani 1 1 d . . . C92 C 0.6260(12) 0.3844(9) 0.4176(5) 0.098(4) Uani 1 1 d . . . C93 C 0.4663(13) 0.2721(9) 0.3680(5) 0.095(4) Uani 1 1 d . . . C94 C 0.8998(16) 0.4915(10) 0.3159(6) 0.116(5) Uani 1 1 d . . . C95 C 0.9590(15) 0.3214(12) 0.4054(6) 0.142(6) Uani 1 1 d . . . C96 C 1.0706(13) 0.3386(10) 0.2859(5) 0.104(4) Uani 1 1 d . . . O11 O 0.4786(12) 0.5104(7) 0.2671(4) 0.160(4) Uani 1 1 d . . . O12 O 0.6364(11) 0.4093(8) 0.4632(4) 0.162(4) Uani 1 1 d . . . O13 O 0.3643(11) 0.2186(8) 0.3811(4) 0.164(4) Uani 1 1 d . . . O14 O 0.8932(13) 0.5735(7) 0.3046(5) 0.169(5) Uani 1 1 d . . . O15 O 0.9944(13) 0.3044(11) 0.4518(4) 0.230(7) Uani 1 1 d . . . O16 O 1.1767(10) 0.3244(8) 0.2575(4) 0.146(4) Uani 1 1 d . . . C51 C 0.7469(9) 0.3521(6) 0.2108(4) 0.046(2) Uani 1 1 d . . . C52 C 0.8324(9) 0.4307(6) 0.1774(4) 0.051(2) Uani 1 1 d . . . H52 H 0.8977 0.4632 0.1969 0.062 Uiso 1 1 calc R . . C53 C 0.8240(9) 0.4622(6) 0.1170(4) 0.053(2) Uani 1 1 d . . . H53 H 0.8835 0.5155 0.0968 0.064 Uiso 1 1 calc R . . C54 C 0.7300(8) 0.4174(5) 0.0848(3) 0.0363(19) Uani 1 1 d . . . C55 C 0.6393(8) 0.3344(5) 0.1168(3) 0.0360(19) Uani 1 1 d . . . C56 C 0.6455(8) 0.3033(6) 0.1810(3) 0.040(2) Uani 1 1 d . . . C57 C 0.5534(9) 0.2240(6) 0.2113(4) 0.054(2) Uani 1 1 d . . . H57 H 0.5567 0.2023 0.2526 0.064 Uiso 1 1 calc R . . C58 C 0.4601(10) 0.1791(6) 0.1812(4) 0.062(2) Uani 1 1 d . . . H58 H 0.3983 0.1275 0.2023 0.074 Uiso 1 1 calc R . . C59 C 0.4544(9) 0.2081(6) 0.1197(4) 0.053(2) Uani 1 1 d . . . H59 H 0.3888 0.1754 0.1004 0.064 Uiso 1 1 calc R . . C60 C 0.5436(8) 0.2843(6) 0.0860(4) 0.043(2) Uani 1 1 d . . . C61 C 0.5361(8) 0.3171(6) 0.0206(4) 0.042(2) Uani 1 1 d . . . C62 C 0.6219(8) 0.4007(6) -0.0109(3) 0.0396(19) Uani 1 1 d . . . C63 C 0.7201(8) 0.4519(5) 0.0193(3) 0.0368(19) Uani 1 1 d . . . C64 C 0.7971(8) 0.5332(6) -0.0134(4) 0.047(2) Uani 1 1 d . . . H64 H 0.8599 0.5675 0.0061 0.057 Uiso 1 1 calc R . . C65 C 0.7844(10) 0.5662(6) -0.0748(4) 0.058(2) Uani 1 1 d . . . H65 H 0.8395 0.6210 -0.0955 0.069 Uiso 1 1 calc R . . C66 C 0.6925(10) 0.5190(6) -0.1045(4) 0.053(2) Uani 1 1 d . . . H66 H 0.6846 0.5419 -0.1453 0.063 Uiso 1 1 calc R . . C67 C 0.6078(9) 0.4349(6) -0.0739(4) 0.048(2) Uani 1 1 d . . . C68 C 0.5136(10) 0.3844(7) -0.1039(4) 0.058(2) Uani 1 1 d . . . H68 H 0.5054 0.4053 -0.1448 0.069 Uiso 1 1 calc R . . C69 C 0.4350(10) 0.3054(7) -0.0731(4) 0.062(3) Uani 1 1 d . . . H69 H 0.3723 0.2726 -0.0935 0.074 Uiso 1 1 calc R . . C70 C 0.4440(9) 0.2708(6) -0.0116(4) 0.053(2) Uani 1 1 d . . . H70 H 0.3874 0.2160 0.0080 0.064 Uiso 1 1 calc R . . C73 C 0.7686(13) 0.1448(6) 0.3451(4) 0.087(3) Uani 1 1 d . . . H73A H 0.8569 0.1198 0.3243 0.104 Uiso 1 1 calc R . . H73B H 0.6786 0.1185 0.3321 0.104 Uiso 1 1 calc R . . C74 C 0.7705(15) 0.1079(8) 0.4116(4) 0.114(4) Uani 1 1 d . . . H74A H 0.8641 0.1302 0.4240 0.137 Uiso 1 1 calc R . . H74B H 0.6864 0.1366 0.4326 0.137 Uiso 1 1 calc R . . C75 C 0.759(2) 0.0002(9) 0.4313(6) 0.173(7) Uani 1 1 d . . . H75A H 0.6648 -0.0221 0.4193 0.208 Uiso 1 1 calc R . . H75B H 0.8424 -0.0286 0.4101 0.208 Uiso 1 1 calc R . . C76 C 0.762(2) -0.0359(10) 0.4962(6) 0.229(10) Uani 1 1 d . . . H76A H 0.8519 -0.0115 0.5093 0.344 Uiso 1 1 calc R . . H76B H 0.7628 -0.1057 0.5042 0.344 Uiso 1 1 calc R . . H76C H 0.6733 -0.0142 0.5176 0.344 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0564(8) 0.0581(8) 0.0485(8) -0.0133(6) -0.0105(6) 0.0039(6) Co2 0.0538(8) 0.0513(8) 0.0507(8) -0.0084(6) -0.0069(6) 0.0094(6) C21 0.041(5) 0.047(5) 0.043(6) -0.020(4) 0.000(4) 0.003(4) C22 0.050(6) 0.046(5) 0.049(6) -0.014(4) -0.004(4) 0.003(4) C31 0.065(7) 0.065(7) 0.065(7) -0.014(5) -0.008(6) -0.008(6) C32 0.100(8) 0.074(7) 0.051(7) -0.020(6) -0.009(6) 0.006(6) C33 0.073(7) 0.106(9) 0.078(7) -0.053(7) -0.025(6) 0.017(7) C34 0.064(7) 0.057(6) 0.066(7) -0.005(5) -0.008(5) 0.008(6) C35 0.103(8) 0.053(7) 0.069(8) -0.020(5) -0.021(6) 0.027(6) C36 0.065(7) 0.047(6) 0.075(7) -0.009(5) -0.005(5) 0.010(5) O1 0.068(5) 0.102(6) 0.091(5) -0.020(4) 0.004(4) -0.021(4) O2 0.182(9) 0.127(7) 0.058(5) -0.004(5) -0.026(5) 0.005(6) O3 0.154(8) 0.115(7) 0.164(8) -0.093(6) -0.072(6) 0.072(6) O4 0.062(5) 0.094(5) 0.119(6) -0.012(4) 0.002(4) 0.009(4) O5 0.178(8) 0.100(6) 0.075(6) 0.018(5) -0.006(5) 0.022(6) O6 0.091(5) 0.079(5) 0.090(5) -0.029(4) -0.016(4) 0.001(4) C1 0.033(5) 0.046(5) 0.040(5) -0.009(4) -0.009(4) 0.001(4) C2 0.050(6) 0.051(5) 0.057(6) -0.016(5) -0.007(5) 0.017(4) C3 0.054(6) 0.062(6) 0.047(6) -0.021(5) 0.002(4) 0.014(5) C4 0.025(4) 0.039(5) 0.048(5) -0.014(4) 0.002(4) 0.001(4) C5 0.034(5) 0.029(4) 0.045(5) -0.008(4) -0.009(4) -0.003(4) C6 0.035(5) 0.039(5) 0.049(5) -0.014(4) -0.005(4) 0.010(4) C7 0.050(5) 0.058(6) 0.036(5) -0.011(4) -0.013(4) 0.019(5) C8 0.064(6) 0.067(6) 0.045(6) -0.017(5) -0.003(4) 0.027(5) C9 0.067(6) 0.052(6) 0.055(6) -0.015(5) -0.008(5) 0.026(5) C10 0.031(5) 0.038(5) 0.047(5) -0.014(4) -0.003(4) -0.002(4) C11 0.032(5) 0.044(5) 0.047(6) -0.009(4) -0.007(4) 0.000(4) C12 0.044(5) 0.049(5) 0.060(6) -0.009(5) -0.005(4) 0.010(4) C13 0.052(6) 0.075(7) 0.059(7) 0.011(5) -0.012(5) 0.010(5) C14 0.053(6) 0.066(7) 0.050(6) 0.003(5) -0.010(5) 0.002(5) C15 0.032(5) 0.052(6) 0.051(6) 0.000(5) -0.001(4) -0.013(4) C16 0.027(4) 0.034(5) 0.050(6) -0.003(4) -0.007(4) -0.011(4) C17 0.038(5) 0.041(5) 0.034(5) -0.016(4) 0.003(4) -0.006(4) C18 0.050(6) 0.049(5) 0.055(6) -0.007(5) -0.005(4) 0.002(4) C19 0.056(6) 0.073(7) 0.045(6) -0.013(5) -0.001(4) 0.003(5) C20 0.045(5) 0.073(7) 0.033(5) -0.002(5) -0.003(4) -0.009(5) C23 0.056(6) 0.059(6) 0.056(6) -0.012(5) 0.004(5) 0.005(5) C24 0.051(6) 0.100(8) 0.066(7) -0.002(6) 0.003(5) -0.002(6) C25 0.067(8) 0.135(10) 0.087(9) 0.013(7) 0.012(6) -0.001(7) C26 0.116(11) 0.206(16) 0.116(12) 0.031(11) 0.021(9) -0.010(10) Co3 0.0731(9) 0.0620(9) 0.0539(8) -0.0131(6) 0.0024(6) 0.0046(7) Co4 0.0686(10) 0.1163(13) 0.0570(9) -0.0193(8) -0.0144(7) -0.0123(9) C71 0.046(5) 0.060(6) 0.058(6) -0.019(5) -0.005(4) 0.006(5) C72 0.095(7) 0.054(6) 0.037(6) -0.004(5) -0.005(5) 0.012(5) C91 0.132(10) 0.082(8) 0.075(8) -0.009(7) 0.026(7) 0.042(8) C92 0.105(9) 0.132(10) 0.063(8) -0.045(7) 0.018(6) -0.027(7) C93 0.078(8) 0.107(10) 0.103(9) -0.027(7) -0.006(7) -0.028(7) C94 0.144(12) 0.106(11) 0.106(10) -0.057(9) 0.023(8) -0.066(11) C95 0.106(10) 0.242(17) 0.082(10) -0.027(11) -0.029(8) -0.041(10) C96 0.064(8) 0.165(12) 0.071(8) 0.001(8) -0.001(6) 0.017(8) O11 0.229(11) 0.116(7) 0.121(8) -0.002(6) 0.001(7) 0.106(7) O12 0.197(10) 0.216(11) 0.087(7) -0.082(7) 0.024(6) -0.043(8) O13 0.136(9) 0.198(10) 0.154(9) -0.031(7) 0.002(7) -0.091(8) O14 0.204(11) 0.111(8) 0.190(10) -0.062(8) 0.054(8) -0.078(8) O15 0.194(11) 0.412(19) 0.080(7) -0.007(9) -0.073(7) -0.076(11) O16 0.076(6) 0.213(10) 0.133(8) -0.007(7) 0.009(5) 0.029(6) C51 0.044(5) 0.047(5) 0.048(6) -0.014(4) 0.000(4) 0.013(5) C52 0.052(6) 0.056(6) 0.051(6) -0.016(5) -0.017(5) -0.004(5) C53 0.055(6) 0.054(6) 0.051(6) -0.011(5) -0.006(5) -0.006(5) C54 0.029(4) 0.035(5) 0.044(5) -0.005(4) -0.007(4) 0.001(4) C55 0.032(5) 0.034(5) 0.047(5) -0.020(4) -0.005(4) 0.011(4) C56 0.030(5) 0.049(5) 0.043(5) -0.007(4) -0.009(4) 0.004(4) C57 0.052(6) 0.054(6) 0.049(6) -0.001(5) 0.003(5) -0.005(5) C58 0.062(6) 0.055(6) 0.062(7) 0.003(5) -0.004(5) -0.018(5) C59 0.054(6) 0.049(6) 0.062(7) -0.020(5) -0.013(5) -0.014(5) C60 0.033(5) 0.043(5) 0.054(6) -0.012(4) -0.007(4) 0.006(4) C61 0.029(5) 0.044(5) 0.057(6) -0.019(5) -0.009(4) 0.008(4) C62 0.031(5) 0.048(5) 0.043(5) -0.015(4) -0.007(4) 0.011(4) C63 0.031(5) 0.032(5) 0.048(5) -0.009(4) -0.003(4) 0.004(4) C64 0.040(5) 0.042(5) 0.063(6) -0.015(5) -0.009(4) 0.007(4) C65 0.059(6) 0.057(6) 0.050(6) -0.001(5) 0.006(5) 0.009(5) C66 0.056(6) 0.055(6) 0.045(6) -0.004(5) -0.006(5) 0.016(5) C67 0.034(5) 0.051(6) 0.060(6) -0.016(5) -0.001(5) 0.014(5) C68 0.055(6) 0.079(7) 0.044(6) -0.023(5) -0.008(5) 0.016(6) C69 0.048(6) 0.080(7) 0.068(7) -0.038(6) -0.014(5) 0.011(6) C70 0.047(6) 0.051(6) 0.063(7) -0.015(5) 0.004(5) -0.005(4) C73 0.149(10) 0.065(7) 0.046(7) -0.011(5) -0.011(6) 0.024(7) C74 0.190(13) 0.079(8) 0.062(8) 0.009(6) -0.011(7) 0.036(8) C75 0.34(2) 0.083(10) 0.094(11) -0.006(8) -0.038(12) 0.045(12) C76 0.45(3) 0.125(13) 0.082(11) 0.040(9) -0.011(14) 0.032(16) _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 Co1 C33 1.784(11) . ? Co1 C32 1.793(11) . ? Co1 C31 1.811(11) . ? Co1 C22 1.974(8) . ? Co1 C21 2.001(8) . ? Co1 Co2 2.459(2) . ? Co2 C36 1.765(11) . ? Co2 C34 1.809(10) . ? Co2 C35 1.816(11) . ? Co2 C22 1.951(8) . ? Co2 C21 1.971(8) . ? C21 C22 1.337(10) . ? C21 C1 1.473(10) . ? C22 C23 1.520(10) . ? C31 O1 1.139(9) . ? C32 O2 1.134(10) . ? C33 O3 1.133(10) . ? C34 O4 1.146(9) . ? C35 O5 1.141(10) . ? C36 O6 1.149(10) . ? C1 C2 1.364(10) . ? C1 C6 1.447(9) . ? C2 C3 1.396(10) . ? C3 C4 1.381(10) . ? C4 C5 1.427(9) . ? C4 C17 1.470(9) . ? C5 C6 1.426(9) . ? C5 C10 1.430(9) . ? C6 C7 1.412(9) . ? C7 C8 1.349(10) . ? C8 C9 1.387(10) . ? C9 C10 1.389(9) . ? C10 C11 1.475(10) . ? C11 C12 1.374(10) . ? C11 C16 1.431(10) . ? C12 C13 1.400(10) . ? C13 C14 1.354(11) . ? C14 C15 1.404(10) . ? C15 C20 1.419(10) . ? C15 C16 1.420(10) . ? C16 C17 1.417(9) . ? C17 C18 1.391(9) . ? C18 C19 1.404(10) . ? C19 C20 1.332(10) . ? C23 C24 1.493(10) . ? C24 C25 1.517(12) . ? C25 C26 1.477(13) . ? Co3 C93 1.729(12) . ? Co3 C91 1.765(12) . ? Co3 C92 1.766(11) . ? Co3 C71 1.984(8) . ? Co3 C72 2.000(9) . ? Co3 Co4 2.463(3) . ? Co4 C96 1.778(12) . ? Co4 C94 1.798(14) . ? Co4 C95 1.831(14) . ? Co4 C72 1.924(9) . ? Co4 C71 1.956(8) . ? C71 C72 1.324(11) . ? C71 C51 1.507(11) . ? C72 C73 1.496(11) . ? C91 O11 1.177(11) . ? C92 O12 1.166(10) . ? C93 O13 1.151(11) . ? C94 O14 1.130(14) . ? C95 O15 1.110(12) . ? C96 O16 1.123(11) . ? C51 C52 1.389(10) . ? C51 C56 1.424(10) . ? C52 C53 1.366(10) . ? C53 C54 1.383(10) . ? C54 C55 1.444(10) . ? C54 C63 1.483(10) . ? C55 C60 1.415(10) . ? C55 C56 1.444(10) . ? C56 C57 1.403(10) . ? C57 C58 1.350(11) . ? C58 C59 1.383(10) . ? C59 C60 1.384(10) . ? C60 C61 1.475(10) . ? C61 C70 1.384(10) . ? C61 C62 1.426(10) . ? C62 C63 1.431(10) . ? C62 C67 1.435(10) . ? C63 C64 1.375(10) . ? C64 C65 1.398(10) . ? C65 C66 1.352(11) . ? C66 C67 1.420(11) . ? C67 C68 1.399(11) . ? C68 C69 1.343(11) . ? C69 C70 1.397(11) . ? C73 C74 1.502(11) . ? C74 C75 1.490(14) . ? C75 C76 1.464(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 C33 Co1 C32 97.6(4) . . ? C33 Co1 C31 100.5(4) . . ? C32 Co1 C31 106.6(4) . . ? C33 Co1 C22 101.6(4) . . ? C32 Co1 C22 105.3(4) . . ? C31 Co1 C22 138.0(4) . . ? C33 Co1 C21 106.0(4) . . ? C32 Co1 C21 140.2(4) . . ? C31 Co1 C21 100.1(4) . . ? C22 Co1 C21 39.3(3) . . ? C33 Co1 Co2 152.0(3) . . ? C32 Co1 Co2 94.9(3) . . ? C31 Co1 Co2 99.7(3) . . ? C22 Co1 Co2 50.8(2) . . ? C21 Co1 Co2 51.2(2) . . ? C36 Co2 C34 98.5(4) . . ? C36 Co2 C35 97.4(4) . . ? C34 Co2 C35 103.7(4) . . ? C36 Co2 C22 101.5(4) . . ? C34 Co2 C22 142.5(4) . . ? C35 Co2 C22 104.8(4) . . ? C36 Co2 C21 99.0(4) . . ? C34 Co2 C21 105.8(4) . . ? C35 Co2 C21 143.5(4) . . ? C22 Co2 C21 39.9(3) . . ? C36 Co2 Co1 149.9(3) . . ? C34 Co2 Co1 98.5(3) . . ? C35 Co2 Co1 102.5(3) . . ? C22 Co2 Co1 51.6(2) . . ? C21 Co2 Co1 52.3(2) . . ? C22 C21 C1 144.6(7) . . ? C22 C21 Co2 69.3(5) . . ? C1 C21 Co2 131.8(5) . . ? C22 C21 Co1 69.2(5) . . ? C1 C21 Co1 136.1(5) . . ? Co2 C21 Co1 76.5(3) . . ? C21 C22 C23 140.6(7) . . ? C21 C22 Co2 70.9(5) . . ? C23 C22 Co2 133.3(6) . . ? C21 C22 Co1 71.5(5) . . ? C23 C22 Co1 135.5(6) . . ? Co2 C22 Co1 77.6(3) . . ? O1 C31 Co1 179.4(10) . . ? O2 C32 Co1 178.3(10) . . ? O3 C33 Co1 175.3(11) . . ? O4 C34 Co2 178.9(9) . . ? O5 C35 Co2 176.1(9) . . ? O6 C36 Co2 179.4(10) . . ? C2 C1 C6 118.2(7) . . ? C2 C1 C21 119.9(7) . . ? C6 C1 C21 121.8(7) . . ? C1 C2 C3 122.1(7) . . ? C4 C3 C2 122.1(7) . . ? C3 C4 C5 117.8(7) . . ? C3 C4 C17 121.9(7) . . ? C5 C4 C17 120.2(7) . . ? C6 C5 C4 120.4(7) . . ? C6 C5 C10 120.1(6) . . ? C4 C5 C10 119.5(7) . . ? C7 C6 C5 118.7(7) . . ? C7 C6 C1 122.1(7) . . ? C5 C6 C1 119.2(6) . . ? C8 C7 C6 120.6(7) . . ? C7 C8 C9 121.1(7) . . ? C8 C9 C10 122.1(7) . . ? C9 C10 C5 117.4(7) . . ? C9 C10 C11 122.1(7) . . ? C5 C10 C11 120.6(6) . . ? C12 C11 C16 117.5(7) . . ? C12 C11 C10 123.7(7) . . ? C16 C11 C10 118.8(7) . . ? C11 C12 C13 123.2(8) . . ? C14 C13 C12 119.7(8) . . ? C13 C14 C15 120.3(8) . . ? C14 C15 C20 120.6(8) . . ? C14 C15 C16 120.2(8) . . ? C20 C15 C16 119.2(8) . . ? C17 C16 C15 119.9(7) . . ? C17 C16 C11 120.9(7) . . ? C15 C16 C11 119.1(7) . . ? C18 C17 C16 118.0(7) . . ? C18 C17 C4 122.2(7) . . ? C16 C17 C4 119.8(6) . . ? C17 C18 C19 121.2(8) . . ? C20 C19 C18 121.3(8) . . ? C19 C20 C15 120.3(8) . . ? C24 C23 C22 115.9(7) . . ? C23 C24 C25 113.6(8) . . ? C26 C25 C24 116.0(9) . . ? C93 Co3 C91 102.5(6) . . ? C93 Co3 C92 96.0(5) . . ? C91 Co3 C92 105.6(5) . . ? C93 Co3 C71 113.4(4) . . ? C91 Co3 C71 92.8(4) . . ? C92 Co3 C71 141.1(4) . . ? C93 Co3 C72 96.1(5) . . ? C91 Co3 C72 131.4(4) . . ? C92 Co3 C72 116.7(5) . . ? C71 Co3 C72 38.8(3) . . ? C93 Co3 Co4 143.4(4) . . ? C91 Co3 Co4 110.4(4) . . ? C92 Co3 Co4 90.4(4) . . ? C71 Co3 Co4 50.8(2) . . ? C72 Co3 Co4 49.7(3) . . ? C96 Co4 C94 101.5(6) . . ? C96 Co4 C95 99.7(6) . . ? C94 Co4 C95 106.1(7) . . ? C96 Co4 C72 103.4(5) . . ? C94 Co4 C72 140.0(5) . . ? C95 Co4 C72 99.9(5) . . ? C96 Co4 C71 97.5(5) . . ? C94 Co4 C71 106.2(5) . . ? C95 Co4 C71 139.2(5) . . ? C72 Co4 C71 39.9(3) . . ? C96 Co4 Co3 149.1(4) . . ? C94 Co4 Co3 91.8(4) . . ? C95 Co4 Co3 103.1(4) . . ? C72 Co4 Co3 52.5(3) . . ? C71 Co4 Co3 51.8(2) . . ? C72 C71 C51 149.7(8) . . ? C72 C71 Co4 68.7(5) . . ? C51 C71 Co4 130.7(6) . . ? C72 C71 Co3 71.2(5) . . ? C51 C71 Co3 130.2(6) . . ? Co4 C71 Co3 77.4(3) . . ? C71 C72 C73 141.5(8) . . ? C71 C72 Co4 71.4(5) . . ? C73 C72 Co4 137.3(7) . . ? C71 C72 Co3 70.0(5) . . ? C73 C72 Co3 130.9(7) . . ? Co4 C72 Co3 77.8(3) . . ? O11 C91 Co3 171.6(12) . . ? O12 C92 Co3 176.4(11) . . ? O13 C93 Co3 178.6(11) . . ? O14 C94 Co4 175.5(14) . . ? O15 C95 Co4 174.9(17) . . ? O16 C96 Co4 178.7(12) . . ? C52 C51 C56 118.6(8) . . ? C52 C51 C71 120.5(8) . . ? C56 C51 C71 120.8(7) . . ? C53 C52 C51 122.5(8) . . ? C52 C53 C54 122.1(8) . . ? C53 C54 C55 118.2(7) . . ? C53 C54 C63 122.1(7) . . ? C55 C54 C63 119.7(7) . . ? C60 C55 C54 120.7(7) . . ? C60 C55 C56 119.9(7) . . ? C54 C55 C56 119.4(7) . . ? C57 C56 C51 122.4(8) . . ? C57 C56 C55 118.4(7) . . ? C51 C56 C55 119.2(7) . . ? C58 C57 C56 120.6(8) . . ? C57 C58 C59 121.3(8) . . ? C58 C59 C60 121.9(8) . . ? C59 C60 C55 117.8(8) . . ? C59 C60 C61 122.3(8) . . ? C55 C60 C61 119.8(7) . . ? C70 C61 C62 118.1(8) . . ? C70 C61 C60 122.0(8) . . ? C62 C61 C60 119.8(7) . . ? C61 C62 C63 121.2(7) . . ? C61 C62 C67 119.4(7) . . ? C63 C62 C67 119.4(7) . . ? C64 C63 C62 118.3(7) . . ? C64 C63 C54 122.9(7) . . ? C62 C63 C54 118.8(7) . . ? C63 C64 C65 122.3(8) . . ? C66 C65 C64 120.5(8) . . ? C65 C66 C67 120.7(8) . . ? C68 C67 C66 121.6(9) . . ? C68 C67 C62 119.6(8) . . ? C66 C67 C62 118.7(8) . . ? C69 C68 C67 119.7(9) . . ? C68 C69 C70 122.3(9) . . ? C61 C70 C69 120.9(8) . . ? C72 C73 C74 115.4(8) . . ? C75 C74 C73 115.3(10) . . ? C76 C75 C74 115.3(11) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 23.56 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.436 _refine_diff_density_min -0.371 _refine_diff_density_rms 0.079 data_2 _database_code_depnum_ccdc_archive 'CCDC 870560' #TrackingRef 'PerC6F4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H20 Au F4 N' _chemical_formula_weight 679.45 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 7.685(3) _cell_length_b 24.297(8) _cell_length_c 30.344(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5666(3) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 875 _cell_measurement_theta_min 5.560 _cell_measurement_theta_max 33.478 _exptl_crystal_description BLOCK _exptl_crystal_colour ORANGE _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2624 _exptl_absorpt_coefficient_mu 5.238 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.596514 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details (G.M.Sheldrick,SADABS,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 47834 _diffrn_reflns_av_R_equivalents 0.1158 _diffrn_reflns_av_sigmaI/netI 0.0698 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 26.66 _reflns_number_total 5939 _reflns_number_gt 2961 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1133P)^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 5939 _refine_ls_number_parameters 336 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1471 _refine_ls_R_factor_gt 0.0657 _refine_ls_wR_factor_ref 0.2173 _refine_ls_wR_factor_gt 0.1679 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 0.41830(7) 0.714329(19) 0.218104(17) 0.0629(2) Uani 1 1 d . . . C27 C 0.3237(18) 0.6546(5) 0.2545(4) 0.072(4) Uani 1 1 d . . . C1 C 0.5227(14) 0.7741(5) 0.1813(4) 0.057(3) Uani 1 1 d . . . C2 C 0.5313(16) 0.7739(5) 0.1362(5) 0.060(3) Uani 1 1 d . . . C3 C 0.6025(15) 0.8150(5) 0.1121(4) 0.059(3) Uani 1 1 d . . . C4 C 0.6744(14) 0.8623(5) 0.1300(4) 0.052(3) Uani 1 1 d . . . C5 C 0.6683(14) 0.8636(5) 0.1750(4) 0.053(3) Uani 1 1 d . . . C6 C 0.6004(15) 0.8204(5) 0.1999(4) 0.059(3) Uani 1 1 d . . . F2 F 0.4636(10) 0.7304(3) 0.1141(2) 0.078(2) Uani 1 1 d . . . F3 F 0.6024(10) 0.8097(3) 0.0670(2) 0.081(2) Uani 1 1 d . . . F5 F 0.7287(11) 0.9075(3) 0.1968(2) 0.081(2) Uani 1 1 d . . . F6 F 0.6018(10) 0.8266(3) 0.2440(2) 0.083(2) Uani 1 1 d . . . C7 C 0.7405(15) 0.9078(4) 0.1027(4) 0.050(3) Uani 1 1 d . . . C8 C 0.6343(15) 0.9319(5) 0.0731(4) 0.056(3) Uani 1 1 d . . . H8 H 0.5246 0.9170 0.0681 0.067 Uiso 1 1 calc R . . C9 C 0.6842(15) 0.9783(5) 0.0497(4) 0.060(3) Uani 1 1 d . . . H9 H 0.6068 0.9934 0.0295 0.072 Uiso 1 1 calc R . . C10 C 0.8438(15) 1.0028(5) 0.0554(4) 0.052(3) Uani 1 1 d . . . C11 C 0.9645(13) 0.9780(4) 0.0852(3) 0.047(3) Uani 1 1 d . . . C12 C 0.9123(14) 0.9289(5) 0.1082(3) 0.050(3) Uani 1 1 d . . . C13 C 1.0329(14) 0.9031(5) 0.1360(4) 0.057(3) Uani 1 1 d . . . H13 H 1.0005 0.8715 0.1512 0.068 Uiso 1 1 calc R . . C14 C 1.2001(16) 0.9238(6) 0.1412(4) 0.075(4) Uani 1 1 d . . . H14 H 1.2815 0.9056 0.1586 0.090 Uiso 1 1 calc R . . C15 C 1.2425(16) 0.9730(5) 0.1196(4) 0.065(3) Uani 1 1 d . . . H15 H 1.3528 0.9877 0.1243 0.077 Uiso 1 1 calc R . . C16 C 1.1309(14) 1.0014(5) 0.0916(4) 0.055(3) Uani 1 1 d . . . C17 C 1.1807(16) 1.0505(5) 0.0685(4) 0.059(3) Uani 1 1 d . . . C18 C 1.0614(16) 1.0762(5) 0.0400(4) 0.060(3) Uani 1 1 d . . . C19 C 0.8932(15) 1.0529(5) 0.0328(4) 0.056(3) Uani 1 1 d . . . C20 C 0.7839(18) 1.0793(5) 0.0037(4) 0.073(4) Uani 1 1 d . . . H20 H 0.6744 1.0645 -0.0016 0.087 Uiso 1 1 calc R . . C21 C 0.832(2) 1.1282(6) -0.0184(5) 0.087(4) Uani 1 1 d . . . H21 H 0.7552 1.1446 -0.0381 0.105 Uiso 1 1 calc R . . C22 C 0.992(2) 1.1514(6) -0.0109(5) 0.085(4) Uani 1 1 d . . . H22 H 1.0230 1.1834 -0.0257 0.102 Uiso 1 1 calc R . . C23 C 1.1064(19) 1.1279(5) 0.0185(4) 0.071(4) Uani 1 1 d . . . C24 C 1.266(2) 1.1513(6) 0.0251(5) 0.086(4) Uani 1 1 d . . . H24 H 1.2955 1.1841 0.0113 0.103 Uiso 1 1 calc R . . C25 C 1.383(2) 1.1257(8) 0.0525(6) 0.105(6) Uani 1 1 d . . . H25 H 1.4909 1.1417 0.0572 0.125 Uiso 1 1 calc R . . C26 C 1.3403(19) 1.0734(7) 0.0746(5) 0.084(4) Uani 1 1 d . . . H26 H 1.4220 1.0562 0.0925 0.100 Uiso 1 1 calc R . . N1 N 0.2699(16) 0.6204(5) 0.2749(4) 0.081(3) Uani 1 1 d . . . C28 C 0.197(3) 0.5740(8) 0.3020(7) 0.119(7) Uani 1 1 d . . . C29 C 0.076(5) 0.6006(14) 0.3344(12) 0.35(3) Uani 1 1 d . . . H29A H 0.0124 0.5727 0.3501 0.530 Uiso 1 1 d R . . H29B H -0.0045 0.6232 0.3183 0.530 Uiso 1 1 d R . . H29C H 0.1387 0.6230 0.3550 0.530 Uiso 1 1 d R . . C30 C 0.346(3) 0.5471(10) 0.3237(9) 0.209(15) Uani 1 1 d . . . H30A H 0.3082 0.5131 0.3367 0.314 Uiso 1 1 calc R . . H30B H 0.3910 0.5709 0.3462 0.314 Uiso 1 1 calc R . . H30C H 0.4348 0.5399 0.3023 0.314 Uiso 1 1 calc R . . C31 C 0.115(4) 0.5336(13) 0.2734(10) 0.27(2) Uani 1 1 d . . . H31A H 0.1034 0.5486 0.2443 0.404 Uiso 1 1 calc R . . H31B H 0.0023 0.5245 0.2848 0.404 Uiso 1 1 calc R . . H31C H 0.1858 0.5011 0.2722 0.404 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.0655(3) 0.0552(3) 0.0681(4) 0.0121(2) 0.0104(2) 0.0014(2) C27 0.074(9) 0.070(9) 0.071(9) 0.027(7) 0.003(7) 0.003(7) C1 0.041(6) 0.056(8) 0.073(8) -0.006(6) 0.013(6) 0.004(5) C2 0.057(7) 0.054(8) 0.070(8) -0.004(6) 0.003(6) -0.003(6) C3 0.054(7) 0.066(8) 0.058(8) -0.002(6) 0.006(6) 0.000(6) C4 0.044(6) 0.050(7) 0.061(7) 0.003(6) 0.006(5) 0.000(5) C5 0.053(6) 0.045(6) 0.061(7) -0.004(6) 0.009(6) 0.004(5) C6 0.058(7) 0.074(9) 0.044(6) -0.003(6) 0.011(6) -0.001(6) F2 0.093(5) 0.064(5) 0.078(5) 0.005(4) 0.009(4) -0.020(4) F3 0.112(6) 0.080(5) 0.052(4) -0.002(4) 0.004(4) -0.022(4) F5 0.107(6) 0.063(5) 0.072(5) -0.013(4) 0.014(4) -0.017(4) F6 0.108(6) 0.088(5) 0.053(4) -0.004(4) 0.005(4) -0.013(4) C7 0.048(6) 0.046(6) 0.057(7) -0.006(5) -0.007(5) 0.005(5) C8 0.050(7) 0.059(7) 0.059(7) -0.006(6) 0.010(5) -0.007(5) C9 0.051(7) 0.068(8) 0.060(7) 0.015(6) -0.005(6) 0.001(6) C10 0.055(6) 0.046(6) 0.054(7) 0.002(5) -0.001(5) -0.002(5) C11 0.045(6) 0.057(7) 0.039(6) -0.004(5) 0.011(5) 0.007(5) C12 0.047(6) 0.055(7) 0.046(6) -0.005(5) 0.002(5) 0.002(5) C13 0.052(7) 0.055(7) 0.063(7) 0.012(6) -0.003(6) 0.006(5) C14 0.056(8) 0.089(10) 0.079(9) 0.015(8) -0.003(7) 0.005(7) C15 0.045(6) 0.078(9) 0.071(8) 0.000(7) -0.003(6) -0.003(6) C16 0.045(6) 0.061(7) 0.059(7) -0.007(6) 0.015(5) 0.007(5) C17 0.059(7) 0.062(8) 0.055(7) -0.017(6) 0.014(6) -0.013(6) C18 0.067(8) 0.064(8) 0.047(7) -0.003(6) 0.000(6) -0.003(6) C19 0.061(8) 0.059(7) 0.049(7) -0.005(5) 0.005(6) 0.007(6) C20 0.072(9) 0.071(9) 0.074(9) 0.004(7) 0.008(7) -0.004(7) C21 0.108(12) 0.076(10) 0.077(10) 0.028(8) -0.001(9) 0.002(9) C22 0.116(12) 0.076(10) 0.063(9) 0.023(8) 0.012(9) -0.008(9) C23 0.087(10) 0.062(8) 0.065(8) 0.001(7) 0.022(7) -0.010(7) C24 0.110(13) 0.085(11) 0.063(9) 0.004(7) 0.007(9) -0.029(10) C25 0.103(13) 0.116(14) 0.095(12) -0.015(11) 0.044(10) -0.062(11) C26 0.066(8) 0.103(12) 0.082(10) -0.004(9) 0.005(8) -0.007(8) N1 0.092(9) 0.076(8) 0.076(8) 0.027(6) 0.002(7) 0.000(7) C28 0.130(16) 0.091(13) 0.135(15) 0.073(12) -0.010(13) -0.011(12) C29 0.50(7) 0.22(4) 0.34(5) 0.18(4) 0.34(5) 0.14(4) C30 0.19(2) 0.18(2) 0.25(3) 0.16(2) -0.09(2) -0.040(19) C31 0.34(5) 0.18(3) 0.29(4) 0.15(3) -0.20(3) -0.17(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 C27 1.964(13) . ? Au1 C1 1.999(12) . ? Au1 Au1 3.1139(13) 2_565 ? C27 N1 1.115(15) . ? C1 C2 1.371(17) . ? C1 C6 1.392(17) . ? C2 C3 1.354(17) . ? C2 F2 1.355(13) . ? C3 F3 1.374(13) . ? C3 C4 1.386(16) . ? C4 C5 1.365(15) . ? C4 C7 1.472(15) . ? C5 F5 1.338(12) . ? C5 C6 1.395(16) . ? C6 F6 1.349(13) . ? C7 C8 1.349(15) . ? C7 C12 1.425(15) . ? C8 C9 1.385(15) . ? C9 C10 1.374(16) . ? C10 C11 1.430(15) . ? C10 C19 1.448(16) . ? C11 C16 1.412(15) . ? C11 C12 1.441(15) . ? C12 C13 1.399(15) . ? C13 C14 1.389(16) . ? C14 C15 1.402(16) . ? C15 C16 1.390(16) . ? C16 C17 1.435(16) . ? C17 C26 1.360(17) . ? C17 C18 1.407(17) . ? C18 C19 1.428(16) . ? C18 C23 1.457(17) . ? C19 C20 1.377(17) . ? C20 C21 1.413(17) . ? C21 C22 1.37(2) . ? C22 C23 1.38(2) . ? C23 C24 1.369(19) . ? C24 C25 1.37(2) . ? C25 C26 1.47(2) . ? N1 C28 1.502(18) . ? C28 C31 1.45(3) . ? C28 C30 1.47(3) . ? C28 C29 1.50(3) . ? 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 C27 Au1 C1 178.1(5) . . ? C27 Au1 Au1 96.0(4) . 2_565 ? C1 Au1 Au1 85.9(3) . 2_565 ? N1 C27 Au1 179.4(14) . . ? C2 C1 C6 112.7(11) . . ? C2 C1 Au1 125.1(9) . . ? C6 C1 Au1 122.2(9) . . ? C3 C2 F2 117.5(12) . . ? C3 C2 C1 123.8(12) . . ? F2 C2 C1 118.6(11) . . ? C2 C3 F3 117.9(11) . . ? C2 C3 C4 124.0(12) . . ? F3 C3 C4 118.0(11) . . ? C5 C4 C3 113.5(10) . . ? C5 C4 C7 123.8(11) . . ? C3 C4 C7 122.6(11) . . ? F5 C5 C4 120.1(10) . . ? F5 C5 C6 117.5(10) . . ? C4 C5 C6 122.4(11) . . ? F6 C6 C1 119.7(11) . . ? F6 C6 C5 116.8(11) . . ? C1 C6 C5 123.4(11) . . ? C8 C7 C12 118.9(10) . . ? C8 C7 C4 119.5(10) . . ? C12 C7 C4 121.6(10) . . ? C7 C8 C9 121.8(11) . . ? C10 C9 C8 122.4(11) . . ? C9 C10 C11 118.4(10) . . ? C9 C10 C19 122.7(11) . . ? C11 C10 C19 118.9(10) . . ? C16 C11 C10 120.4(10) . . ? C16 C11 C12 121.2(10) . . ? C10 C11 C12 118.4(10) . . ? C13 C12 C7 121.6(10) . . ? C13 C12 C11 118.5(10) . . ? C7 C12 C11 119.9(10) . . ? C14 C13 C12 121.3(11) . . ? C13 C14 C15 118.1(12) . . ? C16 C15 C14 124.4(12) . . ? C15 C16 C11 116.4(11) . . ? C15 C16 C17 123.1(11) . . ? C11 C16 C17 120.5(11) . . ? C26 C17 C18 119.2(13) . . ? C26 C17 C16 121.0(13) . . ? C18 C17 C16 119.8(11) . . ? C17 C18 C19 120.5(11) . . ? C17 C18 C23 120.3(12) . . ? C19 C18 C23 119.2(11) . . ? C20 C19 C18 117.7(12) . . ? C20 C19 C10 122.3(11) . . ? C18 C19 C10 119.9(11) . . ? C19 C20 C21 122.4(13) . . ? C22 C21 C20 120.1(14) . . ? C21 C22 C23 120.7(13) . . ? C24 C23 C22 119.9(14) . . ? C24 C23 C18 120.3(14) . . ? C22 C23 C18 119.7(13) . . ? C23 C24 C25 119.2(14) . . ? C24 C25 C26 121.5(15) . . ? C17 C26 C25 119.5(15) . . ? C27 N1 C28 179.4(17) . . ? C31 C28 C30 108(2) . . ? C31 C28 N1 110.0(18) . . ? C30 C28 N1 106.8(16) . . ? C31 C28 C29 114(3) . . ? C30 C28 C29 112(3) . . ? N1 C28 C29 105.5(17) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.66 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.180 _refine_diff_density_min -1.087 _refine_diff_density_rms 0.290 data_6 _database_code_depnum_ccdc_archive 'CCDC 870561' #TrackingRef 'PerC6F4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H43 Cl2 F4 N P2 Pd S' _chemical_formula_weight 1173.29 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' 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' Pd Pd -0.9988 1.0072 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.526(3) _cell_length_b 12.499(4) _cell_length_c 20.347(6) _cell_angle_alpha 78.327(6) _cell_angle_beta 80.155(6) _cell_angle_gamma 70.918(6) _cell_volume 2695.5(14) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 996 _cell_measurement_theta_min 4.315 _cell_measurement_theta_max 49.812 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 0.598 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.786607 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details (G.M.Sheldrick,SADABS,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 23773 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.03 _diffrn_reflns_theta_max 26.43 _reflns_number_total 11010 _reflns_number_gt 7776 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0903P)^2^+2.9966P] 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 11010 _refine_ls_number_parameters 676 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0868 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1733 _refine_ls_wR_factor_gt 0.1480 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.007 _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 Pd1 Pd 0.57870(3) 0.79931(3) 0.706046(16) 0.04234(13) Uani 1 1 d . . . P1 P 0.54058(11) 0.64004(10) 0.67851(6) 0.0434(3) Uani 1 1 d . . . P2 P 0.60373(11) 0.96705(10) 0.72534(6) 0.0435(3) Uani 1 1 d . . . C1 C 0.4798(4) 0.7819(4) 0.7962(2) 0.0424(9) Uani 1 1 d . . . N1 N 0.6940(5) 0.8178(4) 0.6134(3) 0.0640(11) Uani 1 1 d . . . C27 C 0.7582(4) 0.8199(4) 0.5785(2) 0.0418(10) Uani 1 1 d . . . S1 S 0.8650(2) 0.8332(2) 0.50929(12) 0.1279(9) Uani 1 1 d . . . C2 C 0.3546(4) 0.7946(4) 0.8061(2) 0.0471(10) Uani 1 1 d . . . C3 C 0.2911(4) 0.7726(5) 0.8677(2) 0.0543(12) Uani 1 1 d . . . C4 C 0.3468(5) 0.7366(5) 0.9266(2) 0.0564(12) Uani 1 1 d . . . C5 C 0.4729(4) 0.7273(4) 0.9182(2) 0.0542(11) Uani 1 1 d . . . C6 C 0.5339(4) 0.7491(4) 0.8557(2) 0.0500(11) Uani 1 1 d . . . F2 F 0.2900(2) 0.8280(3) 0.75155(13) 0.0639(8) Uani 1 1 d . . . F3 F 0.1698(3) 0.7848(3) 0.87175(15) 0.0812(10) Uani 1 1 d . . . F5 F 0.5347(3) 0.6952(3) 0.97305(14) 0.0805(10) Uani 1 1 d . . . F6 F 0.6560(3) 0.7365(3) 0.85344(14) 0.0693(8) Uani 1 1 d . . . C7 C 0.2823(5) 0.7011(5) 0.9944(3) 0.0611(13) Uani 1 1 d . . . C8 C 0.2973(5) 0.5887(5) 1.0185(3) 0.0644(14) Uani 1 1 d . . . H8 H 0.3481 0.5332 0.9932 0.077 Uiso 1 1 calc R . . C9 C 0.2366(6) 0.5556(5) 1.0815(3) 0.0733(15) Uani 1 1 d . . . H9 H 0.2490 0.4780 1.0975 0.088 Uiso 1 1 calc R . . C10 C 0.1591(5) 0.6350(5) 1.1202(3) 0.0636(14) Uani 1 1 d . . . C11 C 0.1416(5) 0.7537(5) 1.0960(2) 0.0617(13) Uani 1 1 d . . . C12 C 0.2062(5) 0.7876(5) 1.0320(3) 0.0637(13) Uani 1 1 d . . . C13 C 0.1891(6) 0.9038(5) 1.0096(3) 0.0751(16) Uani 1 1 d . . . H13 H 0.2280 0.9268 0.9677 0.090 Uiso 1 1 calc R . . C14 C 0.1188(8) 0.9826(7) 1.0465(4) 0.115(3) Uani 1 1 d . . . H14 H 0.1127 1.0594 1.0311 0.138 Uiso 1 1 calc R . . C15 C 0.0542(7) 0.9523(7) 1.1077(4) 0.102(2) Uani 1 1 d . . . H15 H 0.0034 1.0093 1.1319 0.122 Uiso 1 1 calc R . . C16 C 0.0639(5) 0.8387(6) 1.1333(3) 0.0719(15) Uani 1 1 d . . . C17 C -0.0053(5) 0.8052(6) 1.1964(3) 0.0740(16) Uani 1 1 d . . . C18 C 0.0109(5) 0.6881(6) 1.2219(3) 0.0678(15) Uani 1 1 d . . . C19 C 0.0940(5) 0.5997(6) 1.1874(3) 0.0668(14) Uani 1 1 d . . . C20 C 0.1121(7) 0.4883(7) 1.2166(3) 0.095(2) Uani 1 1 d . . . H20 H 0.1685 0.4318 1.1939 0.114 Uiso 1 1 calc R . . C21 C 0.0527(9) 0.4547(8) 1.2771(4) 0.109(3) Uani 1 1 d . . . H21 H 0.0694 0.3774 1.2952 0.131 Uiso 1 1 calc R . . C22 C -0.0338(8) 0.5382(9) 1.3116(3) 0.112(3) Uani 1 1 d . . . H22 H -0.0775 0.5161 1.3521 0.134 Uiso 1 1 calc R . . C23 C -0.0559(6) 0.6577(8) 1.2852(3) 0.087(2) Uani 1 1 d . . . C24 C -0.1356(7) 0.7459(11) 1.3193(4) 0.114(3) Uani 1 1 d . . . H24 H -0.1789 0.7265 1.3605 0.137 Uiso 1 1 calc R . . C25 C -0.1513(7) 0.8541(11) 1.2954(5) 0.119(3) Uani 1 1 d . . . H25 H -0.2051 0.9099 1.3197 0.143 Uiso 1 1 calc R . . C26 C -0.0879(6) 0.8870(8) 1.2336(4) 0.102(2) Uani 1 1 d . . . H26 H -0.1008 0.9645 1.2170 0.123 Uiso 1 1 calc R . . C28 C 0.4651(5) 0.5584(4) 0.7462(2) 0.0504(11) Uani 1 1 d . . . C29 C 0.5251(6) 0.5054(5) 0.8031(3) 0.0662(14) Uani 1 1 d . . . H29 H 0.6012 0.5141 0.8057 0.079 Uiso 1 1 calc R . . C30 C 0.4746(8) 0.4405(6) 0.8559(3) 0.090(2) Uani 1 1 d . . . H30 H 0.5163 0.4050 0.8936 0.107 Uiso 1 1 calc R . . C31 C 0.3622(8) 0.4289(7) 0.8519(4) 0.104(2) Uani 1 1 d . . . H31 H 0.3277 0.3842 0.8870 0.125 Uiso 1 1 calc R . . C32 C 0.2989(7) 0.4832(7) 0.7961(4) 0.098(2) Uani 1 1 d . . . H32 H 0.2217 0.4761 0.7942 0.118 Uiso 1 1 calc R . . C33 C 0.3509(5) 0.5476(5) 0.7435(3) 0.0668(14) Uani 1 1 d . . . H33 H 0.3087 0.5840 0.7061 0.080 Uiso 1 1 calc R . . C34 C 0.6722(4) 0.5320(4) 0.6425(3) 0.0548(12) Uani 1 1 d . . . C35 C 0.7103(6) 0.4188(5) 0.6721(3) 0.0741(16) Uani 1 1 d . . . H35 H 0.6685 0.3938 0.7125 0.089 Uiso 1 1 calc R . . C36 C 0.8122(7) 0.3413(6) 0.6412(4) 0.095(2) Uani 1 1 d . . . H36 H 0.8385 0.2650 0.6613 0.114 Uiso 1 1 calc R . . C37 C 0.8725(6) 0.3777(8) 0.5820(5) 0.104(3) Uani 1 1 d . . . H37 H 0.9401 0.3255 0.5620 0.125 Uiso 1 1 calc R . . C38 C 0.8366(6) 0.4879(7) 0.5514(4) 0.088(2) Uani 1 1 d . . . H38 H 0.8786 0.5113 0.5106 0.106 Uiso 1 1 calc R . . C39 C 0.7363(5) 0.5659(5) 0.5816(3) 0.0696(15) Uani 1 1 d . . . H39 H 0.7115 0.6419 0.5608 0.084 Uiso 1 1 calc R . . C40 C 0.4380(4) 0.6897(4) 0.6122(2) 0.0490(11) Uani 1 1 d . . . C41 C 0.4233(5) 0.6131(5) 0.5753(3) 0.0643(13) Uani 1 1 d . . . H41 H 0.4708 0.5365 0.5821 0.077 Uiso 1 1 calc R . . C42 C 0.3389(6) 0.6507(7) 0.5290(3) 0.0836(19) Uani 1 1 d . . . H42 H 0.3281 0.5988 0.5055 0.100 Uiso 1 1 calc R . . C43 C 0.2716(6) 0.7621(7) 0.5173(3) 0.086(2) Uani 1 1 d . . . H43 H 0.2145 0.7860 0.4861 0.103 Uiso 1 1 calc R . . C44 C 0.2864(5) 0.8404(6) 0.5511(3) 0.0754(16) Uani 1 1 d . . . H44 H 0.2409 0.9173 0.5420 0.090 Uiso 1 1 calc R . . C45 C 0.3701(4) 0.8041(5) 0.5991(2) 0.0581(12) Uani 1 1 d . . . H45 H 0.3801 0.8568 0.6223 0.070 Uiso 1 1 calc R . . C46 C 0.5417(5) 1.0180(4) 0.8062(2) 0.0534(11) Uani 1 1 d . . . C47 C 0.4143(5) 1.0472(5) 0.8224(3) 0.0646(13) Uani 1 1 d . . . H47 H 0.3659 1.0368 0.7934 0.078 Uiso 1 1 calc R . . C48 C 0.3586(7) 1.0914(5) 0.8809(3) 0.0818(18) Uani 1 1 d . . . H48 H 0.2732 1.1111 0.8913 0.098 Uiso 1 1 calc R . . C49 C 0.4300(9) 1.1058(7) 0.9233(3) 0.103(2) Uani 1 1 d . . . H49 H 0.3935 1.1351 0.9630 0.123 Uiso 1 1 calc R . . C50 C 0.5527(9) 1.0778(8) 0.9078(4) 0.114(3) Uani 1 1 d . . . H50 H 0.6004 1.0881 0.9372 0.137 Uiso 1 1 calc R . . C51 C 0.6113(6) 1.0338(6) 0.8488(3) 0.0817(18) Uani 1 1 d . . . H51 H 0.6966 1.0155 0.8388 0.098 Uiso 1 1 calc R . . C52 C 0.7671(4) 0.9535(4) 0.7116(2) 0.0534(11) Uani 1 1 d . . . C53 C 0.8469(5) 0.8681(5) 0.7508(3) 0.0752(16) Uani 1 1 d . . . H53 H 0.8153 0.8223 0.7865 0.090 Uiso 1 1 calc R . . C54 C 0.9724(5) 0.8488(6) 0.7384(4) 0.0841(18) Uani 1 1 d . . . H54 H 1.0247 0.7917 0.7662 0.101 Uiso 1 1 calc R . . C55 C 1.0201(6) 0.9129(7) 0.6857(4) 0.093(2) Uani 1 1 d . . . H55 H 1.1051 0.8996 0.6771 0.111 Uiso 1 1 calc R . . C56 C 0.9429(7) 0.9972(8) 0.6452(4) 0.107(3) Uani 1 1 d . . . H56 H 0.9760 1.0396 0.6082 0.129 Uiso 1 1 calc R . . C57 C 0.8154(5) 1.0203(6) 0.6586(3) 0.0795(18) Uani 1 1 d . . . H57 H 0.7633 1.0802 0.6321 0.095 Uiso 1 1 calc R . . C58 C 0.5298(4) 1.0913(4) 0.6663(2) 0.0510(11) Uani 1 1 d . . . C59 C 0.5063(6) 1.2005(5) 0.6809(3) 0.0755(16) Uani 1 1 d . . . H59 H 0.5295 1.2097 0.7205 0.091 Uiso 1 1 calc R . . C60 C 0.4487(7) 1.2956(5) 0.6374(3) 0.088(2) Uani 1 1 d . . . H60 H 0.4328 1.3684 0.6480 0.106 Uiso 1 1 calc R . . C61 C 0.4150(6) 1.2840(5) 0.5793(3) 0.0797(18) Uani 1 1 d . . . H61 H 0.3780 1.3486 0.5496 0.096 Uiso 1 1 calc R . . C62 C 0.4358(5) 1.1764(6) 0.5642(3) 0.0734(16) Uani 1 1 d . . . H62 H 0.4107 1.1684 0.5248 0.088 Uiso 1 1 calc R . . C63 C 0.4941(4) 1.0793(5) 0.6076(2) 0.0567(12) Uani 1 1 d . . . H63 H 0.5090 1.0067 0.5970 0.068 Uiso 1 1 calc R . . C70 C 0.0262(19) 0.344(2) 0.0123(14) 0.405(18) Uani 1 1 d . . . H70A H -0.0227 0.2937 0.0129 0.485 Uiso 1 1 calc R . . H70B H -0.0176 0.4203 -0.0088 0.485 Uiso 1 1 calc R . . Cl1 Cl 0.1345(8) 0.3069(8) -0.0226(8) 0.551(11) Uani 1 1 d . . . Cl2 Cl 0.0455(10) 0.3475(10) 0.0905(4) 0.475(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 Pd1 0.0449(2) 0.0489(2) 0.03620(19) -0.00842(13) -0.00060(13) -0.01905(15) P1 0.0463(6) 0.0461(6) 0.0402(6) -0.0091(5) -0.0036(5) -0.0163(5) P2 0.0465(6) 0.0493(6) 0.0392(6) -0.0064(5) -0.0045(5) -0.0209(5) C1 0.045(2) 0.042(2) 0.041(2) -0.0074(18) -0.0043(18) -0.0137(18) N1 0.080(3) 0.052(3) 0.069(3) -0.018(2) -0.022(3) -0.021(2) C27 0.040(2) 0.047(3) 0.039(2) -0.024(2) 0.0088(19) -0.010(2) S1 0.1231(17) 0.1229(17) 0.1191(17) -0.0381(13) 0.0761(14) -0.0461(14) C2 0.047(2) 0.059(3) 0.037(2) -0.0090(19) -0.0066(18) -0.016(2) C3 0.042(2) 0.075(3) 0.049(3) -0.014(2) 0.001(2) -0.022(2) C4 0.064(3) 0.073(3) 0.038(2) -0.009(2) 0.003(2) -0.032(3) C5 0.056(3) 0.069(3) 0.040(2) -0.001(2) -0.011(2) -0.024(2) C6 0.044(2) 0.063(3) 0.046(2) -0.003(2) -0.0088(19) -0.021(2) F2 0.0500(15) 0.096(2) 0.0430(15) -0.0069(14) -0.0092(12) -0.0180(15) F3 0.0486(17) 0.136(3) 0.0592(18) -0.0099(18) 0.0013(14) -0.0356(18) F5 0.079(2) 0.125(3) 0.0444(16) 0.0079(17) -0.0205(15) -0.046(2) F6 0.0517(16) 0.105(2) 0.0531(16) 0.0049(15) -0.0110(13) -0.0337(16) C7 0.059(3) 0.075(4) 0.052(3) -0.011(2) -0.005(2) -0.022(3) C8 0.074(3) 0.060(3) 0.047(3) -0.006(2) 0.009(2) -0.014(3) C9 0.082(4) 0.071(4) 0.059(3) -0.007(3) 0.006(3) -0.023(3) C10 0.050(3) 0.094(4) 0.051(3) -0.024(3) 0.000(2) -0.022(3) C11 0.053(3) 0.091(4) 0.046(3) -0.011(3) -0.006(2) -0.029(3) C12 0.059(3) 0.076(4) 0.061(3) -0.015(3) -0.010(2) -0.022(3) C13 0.091(4) 0.062(3) 0.069(4) -0.012(3) 0.004(3) -0.024(3) C14 0.142(7) 0.079(5) 0.114(6) -0.028(4) 0.023(6) -0.031(5) C15 0.111(6) 0.081(5) 0.104(6) -0.037(4) 0.009(5) -0.013(4) C16 0.061(3) 0.089(4) 0.063(3) -0.023(3) -0.002(3) -0.015(3) C17 0.052(3) 0.112(5) 0.060(3) -0.026(3) -0.001(2) -0.022(3) C18 0.052(3) 0.111(5) 0.047(3) -0.024(3) 0.001(2) -0.031(3) C19 0.063(3) 0.093(4) 0.047(3) -0.010(3) -0.005(2) -0.028(3) C20 0.112(6) 0.114(6) 0.064(4) -0.016(4) 0.008(4) -0.050(5) C21 0.143(7) 0.130(7) 0.069(4) -0.010(4) 0.005(5) -0.074(6) C22 0.118(6) 0.189(9) 0.053(4) -0.006(5) 0.007(4) -0.097(7) C23 0.067(4) 0.159(7) 0.050(3) -0.031(4) 0.010(3) -0.055(4) C24 0.069(5) 0.206(10) 0.078(5) -0.061(6) 0.028(4) -0.050(6) C25 0.071(5) 0.186(10) 0.099(6) -0.075(7) 0.024(4) -0.020(6) C26 0.076(4) 0.122(6) 0.106(6) -0.049(5) -0.005(4) -0.011(4) C28 0.064(3) 0.048(3) 0.044(2) -0.010(2) 0.000(2) -0.025(2) C29 0.087(4) 0.060(3) 0.054(3) 0.000(2) -0.013(3) -0.029(3) C30 0.127(6) 0.078(4) 0.064(4) 0.012(3) -0.017(4) -0.042(4) C31 0.140(7) 0.105(6) 0.074(5) 0.013(4) 0.011(4) -0.074(5) C32 0.100(5) 0.130(6) 0.083(5) -0.009(4) 0.011(4) -0.074(5) C33 0.075(4) 0.078(4) 0.054(3) -0.008(3) 0.000(3) -0.037(3) C34 0.050(3) 0.061(3) 0.059(3) -0.024(2) -0.011(2) -0.015(2) C35 0.073(4) 0.066(4) 0.084(4) -0.021(3) -0.018(3) -0.011(3) C36 0.084(5) 0.075(4) 0.122(6) -0.041(4) -0.032(5) 0.007(4) C37 0.058(4) 0.122(7) 0.136(7) -0.087(6) -0.017(4) 0.009(4) C38 0.057(3) 0.127(6) 0.093(5) -0.069(5) 0.011(3) -0.024(4) C39 0.065(3) 0.085(4) 0.067(3) -0.032(3) 0.007(3) -0.027(3) C40 0.052(3) 0.062(3) 0.036(2) -0.005(2) -0.0046(19) -0.023(2) C41 0.080(4) 0.072(3) 0.053(3) -0.008(2) -0.012(3) -0.037(3) C42 0.094(5) 0.117(6) 0.060(4) -0.014(4) -0.024(3) -0.052(4) C43 0.076(4) 0.127(6) 0.057(4) 0.000(4) -0.026(3) -0.033(4) C44 0.060(3) 0.088(4) 0.060(3) -0.001(3) -0.008(3) -0.004(3) C45 0.052(3) 0.065(3) 0.052(3) -0.009(2) -0.003(2) -0.012(2) C46 0.071(3) 0.052(3) 0.041(2) -0.007(2) -0.005(2) -0.024(2) C47 0.076(4) 0.061(3) 0.062(3) -0.016(2) 0.001(3) -0.027(3) C48 0.095(5) 0.068(4) 0.074(4) -0.018(3) 0.016(3) -0.022(3) C49 0.141(7) 0.105(6) 0.057(4) -0.033(4) -0.007(4) -0.020(5) C50 0.125(7) 0.150(8) 0.081(5) -0.047(5) -0.036(5) -0.029(6) C51 0.084(4) 0.104(5) 0.064(4) -0.035(3) -0.020(3) -0.019(4) C52 0.050(3) 0.064(3) 0.054(3) -0.011(2) -0.007(2) -0.026(2) C53 0.056(3) 0.083(4) 0.083(4) 0.001(3) -0.004(3) -0.027(3) C54 0.056(3) 0.097(5) 0.094(5) -0.006(4) -0.013(3) -0.020(3) C55 0.053(3) 0.131(6) 0.099(5) -0.029(5) 0.000(3) -0.033(4) C56 0.071(4) 0.149(7) 0.099(5) 0.014(5) 0.006(4) -0.058(5) C57 0.059(3) 0.091(4) 0.086(4) 0.014(3) -0.010(3) -0.036(3) C58 0.050(3) 0.055(3) 0.048(3) -0.001(2) -0.001(2) -0.023(2) C59 0.115(5) 0.054(3) 0.064(3) 0.002(3) -0.021(3) -0.036(3) C60 0.123(6) 0.060(4) 0.079(4) 0.006(3) -0.011(4) -0.034(4) C61 0.080(4) 0.068(4) 0.069(4) 0.013(3) 0.003(3) -0.013(3) C62 0.065(3) 0.103(5) 0.043(3) 0.002(3) -0.008(2) -0.020(3) C63 0.054(3) 0.067(3) 0.048(3) -0.008(2) -0.004(2) -0.019(2) C70 0.27(2) 0.50(4) 0.50(4) 0.03(3) -0.32(3) -0.11(3) Cl1 0.301(9) 0.360(10) 0.96(3) -0.279(13) 0.345(13) -0.166(8) Cl2 0.547(8) 0.796(11) 0.263(7) 0.130(9) -0.149(8) -0.523 _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 Pd1 C1 2.000(4) . ? Pd1 N1 2.131(6) . ? Pd1 P2 2.3239(13) . ? Pd1 P1 2.3617(13) . ? P1 C28 1.816(5) . ? P1 C40 1.825(5) . ? P1 C34 1.828(5) . ? P2 C52 1.812(5) . ? P2 C58 1.820(5) . ? P2 C46 1.830(5) . ? C1 C6 1.383(6) . ? C1 C2 1.383(6) . ? N1 C27 0.937(6) . ? C27 S1 1.724(5) . ? C2 F2 1.361(5) . ? C2 C3 1.364(6) . ? C3 F3 1.345(5) . ? C3 C4 1.382(7) . ? C4 C5 1.402(7) . ? C4 C7 1.507(7) . ? C5 F5 1.348(5) . ? C5 C6 1.365(6) . ? C6 F6 1.357(5) . ? C7 C8 1.355(7) . ? C7 C12 1.418(7) . ? C8 C9 1.404(7) . ? C9 C10 1.378(8) . ? C10 C11 1.424(8) . ? C10 C19 1.501(7) . ? C11 C16 1.407(8) . ? C11 C12 1.442(7) . ? C12 C13 1.389(8) . ? C13 C14 1.328(9) . ? C14 C15 1.387(10) . ? C15 C16 1.385(9) . ? C16 C17 1.453(8) . ? C17 C26 1.398(9) . ? C17 C18 1.411(9) . ? C18 C19 1.423(8) . ? C18 C23 1.431(8) . ? C19 C20 1.361(9) . ? C20 C21 1.360(9) . ? C21 C22 1.398(12) . ? C22 C23 1.435(12) . ? C23 C24 1.404(12) . ? C24 C25 1.305(12) . ? C25 C26 1.399(12) . ? C28 C33 1.377(7) . ? C28 C29 1.386(7) . ? C29 C30 1.376(8) . ? C30 C31 1.367(10) . ? C31 C32 1.390(10) . ? C32 C33 1.379(8) . ? C34 C35 1.377(8) . ? C34 C39 1.394(7) . ? C35 C36 1.401(9) . ? C36 C37 1.355(11) . ? C37 C38 1.351(11) . ? C38 C39 1.388(8) . ? C40 C45 1.383(7) . ? C40 C41 1.396(7) . ? C41 C42 1.375(8) . ? C42 C43 1.348(10) . ? C43 C44 1.371(9) . ? C44 C45 1.396(7) . ? C46 C51 1.357(7) . ? C46 C47 1.390(7) . ? C47 C48 1.382(8) . ? C48 C49 1.363(10) . ? C49 C50 1.339(11) . ? C50 C51 1.396(9) . ? C52 C53 1.373(7) . ? C52 C57 1.381(7) . ? C53 C54 1.373(8) . ? C54 C55 1.353(9) . ? C55 C56 1.367(10) . ? C56 C57 1.390(9) . ? C58 C63 1.378(7) . ? C58 C59 1.386(7) . ? C59 C60 1.377(8) . ? C60 C61 1.354(9) . ? C61 C62 1.376(9) . ? C62 C63 1.393(7) . ? C70 Cl1 1.31(3) . ? C70 Cl2 1.66(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 Pd1 N1 176.15(17) . . ? C1 Pd1 P2 91.12(12) . . ? N1 Pd1 P2 86.82(11) . . ? C1 Pd1 P1 90.78(12) . . ? N1 Pd1 P1 91.57(11) . . ? P2 Pd1 P1 174.44(4) . . ? C28 P1 C40 105.2(2) . . ? C28 P1 C34 104.5(2) . . ? C40 P1 C34 102.8(2) . . ? C28 P1 Pd1 116.26(15) . . ? C40 P1 Pd1 109.05(16) . . ? C34 P1 Pd1 117.57(16) . . ? C52 P2 C58 106.2(2) . . ? C52 P2 C46 107.7(2) . . ? C58 P2 C46 101.3(2) . . ? C52 P2 Pd1 108.47(17) . . ? C58 P2 Pd1 112.21(16) . . ? C46 P2 Pd1 120.00(16) . . ? C6 C1 C2 113.2(4) . . ? C6 C1 Pd1 121.9(3) . . ? C2 C1 Pd1 124.8(3) . . ? C27 N1 Pd1 167.8(5) . . ? N1 C27 S1 174.1(6) . . ? F2 C2 C3 117.1(4) . . ? F2 C2 C1 119.0(4) . . ? C3 C2 C1 123.8(4) . . ? F3 C3 C2 119.3(4) . . ? F3 C3 C4 118.2(4) . . ? C2 C3 C4 122.5(4) . . ? C3 C4 C5 114.7(4) . . ? C3 C4 C7 123.8(4) . . ? C5 C4 C7 121.4(4) . . ? F5 C5 C6 119.7(4) . . ? F5 C5 C4 119.0(4) . . ? C6 C5 C4 121.4(4) . . ? F6 C6 C5 116.4(4) . . ? F6 C6 C1 119.2(4) . . ? C5 C6 C1 124.4(4) . . ? C8 C7 C12 121.1(5) . . ? C8 C7 C4 120.3(5) . . ? C12 C7 C4 118.6(5) . . ? C7 C8 C9 120.3(5) . . ? C10 C9 C8 121.7(6) . . ? C9 C10 C11 119.0(5) . . ? C9 C10 C19 121.7(6) . . ? C11 C10 C19 119.2(5) . . ? C16 C11 C10 121.6(5) . . ? C16 C11 C12 119.2(6) . . ? C10 C11 C12 119.2(5) . . ? C13 C12 C7 123.1(5) . . ? C13 C12 C11 118.4(5) . . ? C7 C12 C11 118.5(5) . . ? C14 C13 C12 121.6(6) . . ? C13 C14 C15 121.0(7) . . ? C16 C15 C14 121.2(6) . . ? C15 C16 C11 118.5(6) . . ? C15 C16 C17 122.1(6) . . ? C11 C16 C17 119.4(6) . . ? C26 C17 C18 118.5(6) . . ? C26 C17 C16 121.3(7) . . ? C18 C17 C16 120.2(5) . . ? C17 C18 C19 121.9(5) . . ? C17 C18 C23 119.0(6) . . ? C19 C18 C23 119.1(6) . . ? C20 C19 C18 119.3(6) . . ? C20 C19 C10 123.2(6) . . ? C18 C19 C10 117.5(5) . . ? C21 C20 C19 123.9(8) . . ? C20 C21 C22 119.0(8) . . ? C21 C22 C23 120.6(6) . . ? C24 C23 C18 118.5(8) . . ? C24 C23 C22 123.5(7) . . ? C18 C23 C22 118.0(7) . . ? C25 C24 C23 122.5(8) . . ? C24 C25 C26 120.5(8) . . ? C17 C26 C25 121.0(9) . . ? C33 C28 C29 118.8(5) . . ? C33 C28 P1 122.9(4) . . ? C29 C28 P1 118.3(4) . . ? C30 C29 C28 121.6(6) . . ? C31 C30 C29 118.9(6) . . ? C30 C31 C32 120.7(6) . . ? C33 C32 C31 119.7(7) . . ? C28 C33 C32 120.3(6) . . ? C35 C34 C39 118.4(5) . . ? C35 C34 P1 123.5(4) . . ? C39 C34 P1 118.2(4) . . ? C34 C35 C36 119.9(7) . . ? C37 C36 C35 120.0(7) . . ? C38 C37 C36 121.6(6) . . ? C37 C38 C39 119.2(7) . . ? C38 C39 C34 121.0(6) . . ? C45 C40 C41 118.7(5) . . ? C45 C40 P1 120.3(4) . . ? C41 C40 P1 121.0(4) . . ? C42 C41 C40 120.1(6) . . ? C43 C42 C41 120.7(6) . . ? C42 C43 C44 120.7(6) . . ? C43 C44 C45 119.7(6) . . ? C40 C45 C44 120.0(5) . . ? C51 C46 C47 119.0(5) . . ? C51 C46 P2 124.2(4) . . ? C47 C46 P2 116.7(4) . . ? C48 C47 C46 120.8(6) . . ? C49 C48 C47 119.3(7) . . ? C50 C49 C48 119.9(7) . . ? C49 C50 C51 121.9(7) . . ? C46 C51 C50 119.0(7) . . ? C53 C52 C57 118.6(5) . . ? C53 C52 P2 119.6(4) . . ? C57 C52 P2 121.5(4) . . ? C52 C53 C54 121.4(6) . . ? C55 C54 C53 120.0(6) . . ? C54 C55 C56 119.8(6) . . ? C55 C56 C57 120.8(6) . . ? C52 C57 C56 119.3(6) . . ? C63 C58 C59 118.9(5) . . ? C63 C58 P2 121.4(4) . . ? C59 C58 P2 119.7(4) . . ? C60 C59 C58 120.6(6) . . ? C61 C60 C59 120.5(6) . . ? C60 C61 C62 119.9(6) . . ? C61 C62 C63 120.3(6) . . ? C58 C63 C62 119.7(5) . . ? Cl1 C70 Cl2 109.7(11) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.019 _refine_diff_density_min -0.940 _refine_diff_density_rms 0.092