# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Bochmann, Manfred' 'Savjani, Nicky' 'Carrera, Nora' 'Simpson, Jason' 'Hughes, David' _publ_contact_author_name 'Bochmann, Manfred' _publ_contact_author_email M.Bochmann@uea.ac.uk _publ_section_title ; Syntheses and Structures of Thermally Stable Diketiminato Complexes of Gold and Copper ; # Attachment '- nora_combined_cif.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 800528' #TrackingRef '- nora_combined_cif.cif' _audit_creation_method 'SHELXL-97 and CrysAlisPro' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_structural '[Cu(PPh3)2{HC(C(CF3)NC6H3(CF3)2)2}].ca 0.7(C6H14)' _chemical_formula_moiety 'C57 H37 F18 N2 P2 CU, C4.4' _chemical_formula_sum 'C61.40 H37 Cu F18 N2 P2' _chemical_formula_weight 1270.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.2547(5) _cell_length_b 20.3882(5) _cell_length_c 14.5824(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.886(2) _cell_angle_gamma 90.00 _cell_volume 5621.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used 14767 _cell_measurement_theta_min 3.3765 _cell_measurement_theta_max 29.9991 _exptl_crystal_description block _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.501 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2562 _exptl_absorpt_coefficient_mu 0.548 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.863 _exptl_absorpt_correction_T_max 1.157 _exptl_absorpt_process_details ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.33.55 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_reflns_number 45449 _diffrn_reflns_av_R_equivalents 0.0613 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6449 _reflns_number_gt 4561 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Johnson, 1976 and Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008) and WINGX (Farrugia, 1999)' _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^ > 2\s(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^)+(0.0501P)^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 6449 _refine_ls_number_parameters 411 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0873 _refine_ls_wR_factor_gt 0.0833 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.924 _refine_ls_shift/su_max 0.153 _refine_ls_shift/su_mean 0.005 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 Cu Cu 0.5000 0.653282(16) 0.7500 0.01634(9) Uani 1 2 d S . . P1 P 0.40683(2) 0.70436(2) 0.65550(3) 0.01827(11) Uani 1 1 d . . . C11 C 0.36313(10) 0.77233(9) 0.70323(13) 0.0208(4) Uani 1 1 d . . . C12 C 0.32380(11) 0.81953(10) 0.64749(15) 0.0296(5) Uani 1 1 d . . . H12 H 0.3189 0.8169 0.5829 0.036 Uiso 1 1 calc R . . C13 C 0.29188(12) 0.87033(11) 0.68641(16) 0.0349(5) Uani 1 1 d . . . H13 H 0.2659 0.9015 0.6479 0.042 Uiso 1 1 calc R . . C14 C 0.29821(12) 0.87521(12) 0.78166(17) 0.0382(6) Uani 1 1 d . . . H14 H 0.2766 0.9094 0.8078 0.046 Uiso 1 1 calc R . . C15 C 0.33717(12) 0.82865(12) 0.83809(16) 0.0382(6) Uani 1 1 d . . . H15 H 0.3418 0.8316 0.9026 0.046 Uiso 1 1 calc R . . C16 C 0.36938(11) 0.77752(10) 0.79947(14) 0.0276(5) Uani 1 1 d . . . H16 H 0.3954 0.7464 0.8383 0.033 Uiso 1 1 calc R . . C21 C 0.33610(10) 0.64435(9) 0.61968(12) 0.0206(4) Uani 1 1 d . . . C22 C 0.26445(10) 0.65821(10) 0.61352(13) 0.0254(4) Uani 1 1 d . . . H22 H 0.2501 0.7001 0.6272 0.030 Uiso 1 1 calc R . . C23 C 0.21453(11) 0.60917(11) 0.58687(14) 0.0304(5) Uani 1 1 d . . . H23 H 0.1668 0.6185 0.5830 0.036 Uiso 1 1 calc R . . C24 C 0.23476(11) 0.54712(11) 0.56620(14) 0.0320(5) Uani 1 1 d . . . H24 H 0.2008 0.5149 0.5478 0.038 Uiso 1 1 calc R . . C25 C 0.30586(11) 0.53276(10) 0.57286(14) 0.0293(5) Uani 1 1 d . . . H25 H 0.3198 0.4907 0.5594 0.035 Uiso 1 1 calc R . . C26 C 0.35609(10) 0.58103(10) 0.59959(13) 0.0234(4) Uani 1 1 d . . . H26 H 0.4038 0.5711 0.6042 0.028 Uiso 1 1 calc R . . C31 C 0.41982(10) 0.73897(10) 0.54386(13) 0.0224(4) Uani 1 1 d . . . C32 C 0.38599(11) 0.71587(11) 0.45784(13) 0.0283(5) Uani 1 1 d . . . H32 H 0.3546 0.6809 0.4546 0.034 Uiso 1 1 calc R . . C33 C 0.39859(13) 0.74453(12) 0.37646(14) 0.0382(6) Uani 1 1 d . . . H33 H 0.3755 0.7287 0.3189 0.046 Uiso 1 1 calc R . . C34 C 0.44501(13) 0.79622(13) 0.38021(16) 0.0428(6) Uani 1 1 d . . . H34 H 0.4533 0.8153 0.3254 0.051 Uiso 1 1 calc R . . C35 C 0.47901(12) 0.81939(12) 0.46534(17) 0.0411(6) Uani 1 1 d . . . H35 H 0.5104 0.8543 0.4680 0.049 Uiso 1 1 calc R . . C36 C 0.46691(11) 0.79120(11) 0.54692(15) 0.0320(5) Uani 1 1 d . . . H36 H 0.4903 0.8071 0.6042 0.038 Uiso 1 1 calc R . . N4 N 0.55040(8) 0.58370(7) 0.67972(10) 0.0175(3) Uani 1 1 d . . . C41 C 0.60329(10) 0.60507(9) 0.63012(12) 0.0188(4) Uani 1 1 d . . . C42 C 0.67449(10) 0.59338(9) 0.66563(13) 0.0204(4) Uani 1 1 d . . . H42 H 0.6878 0.5722 0.7228 0.025 Uiso 1 1 calc R . . C43 C 0.72585(10) 0.61314(10) 0.61620(13) 0.0214(4) Uani 1 1 d . . . C44 C 0.70759(10) 0.64632(10) 0.53229(14) 0.0248(4) Uani 1 1 d . . . H44 H 0.7422 0.6598 0.4997 0.030 Uiso 1 1 calc R . . C45 C 0.63697(11) 0.65896(10) 0.49794(13) 0.0254(4) Uani 1 1 d . . . C46 C 0.58478(10) 0.63938(10) 0.54602(13) 0.0228(4) Uani 1 1 d . . . H46 H 0.5376 0.6491 0.5224 0.027 Uiso 1 1 calc R . . C431 C 0.80203(11) 0.59763(11) 0.65409(15) 0.0309(5) Uani 1 1 d . . . F431 F 0.81027(7) 0.54072(7) 0.69947(11) 0.0532(4) Uani 1 1 d . . . F432 F 0.84017(6) 0.59429(8) 0.58633(9) 0.0499(4) Uani 1 1 d . . . F433 F 0.83338(7) 0.64315(7) 0.71377(9) 0.0462(4) Uani 1 1 d . . . C451 C 0.61852(13) 0.69391(14) 0.40670(17) 0.0454(7) Uani 1 1 d . . . F451 F 0.66216(17) 0.6812(2) 0.35069(17) 0.1041(19) Uani 0.833(6) 1 d P . . F452 F 0.62495(14) 0.76135(12) 0.42075(19) 0.0701(11) Uani 0.833(6) 1 d P . . F453 F 0.5525(2) 0.6857(2) 0.3626(3) 0.0429(7) Uani 0.833(6) 1 d P . . F454 F 0.6541(6) 0.7349(6) 0.3885(7) 0.044(3) Uiso 0.167(6) 1 d P . . F455 F 0.6305(5) 0.6415(4) 0.3364(6) 0.036(3) Uiso 0.167(6) 1 d P . . F456 F 0.5546(14) 0.7020(10) 0.3732(17) 0.045(6) Uiso 0.167(6) 1 d P . . C5 C 0.54067(9) 0.52058(9) 0.69116(12) 0.0197(4) Uani 1 1 d . . . C51 C 0.5000 0.49152(13) 0.7500 0.0223(6) Uani 1 2 d S . . H51 H 0.5000 0.4459 0.7500 0.027 Uiso 1 2 calc SR . . C52 C 0.57482(11) 0.46992(10) 0.63533(15) 0.0298(5) Uani 1 1 d . . . F521 F 0.54111(7) 0.41243(6) 0.62678(10) 0.0441(4) Uani 1 1 d . . . F522 F 0.64183(7) 0.45667(7) 0.67520(10) 0.0480(4) Uani 1 1 d . . . F523 F 0.57574(8) 0.48993(7) 0.54831(9) 0.0457(4) Uani 1 1 d . . . C91 C 0.0171(13) 0.5312(12) 0.378(2) 0.117(7) Uiso 0.25 1 d P . . C92 C -0.0377(12) 0.5102(10) 0.409(2) 0.118(7) Uiso 0.30 1 d P . . C93 C -0.0183(14) 0.5442(13) 0.313(2) 0.116(8) Uiso 0.25 1 d P . . C94 C -0.036(2) 0.5108(19) 0.363(3) 0.122(11) Uiso 0.20 1 d P . . C95 C -0.0124(8) 0.4912(6) 0.5552(11) 0.104(4) Uiso 0.40 1 d P . . C96 C 0.006(3) 0.523(4) 0.284(5) 0.090(17) Uiso 0.10 1 d P . . C97 C 0.0000 0.498(2) 0.2500 0.125(14) Uiso 0.25 2 d SP . . C98 C 0.0000 0.5545(19) 0.2500 0.112(11) Uiso 0.25 2 d SP . . C99 C 0.000(3) 0.498(2) 0.329(4) 0.123(13) Uiso 0.15 1 d P . . C100 C 0.0217(7) 0.4984(9) 0.5092(16) 0.091(4) Uiso 0.30 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 Cu 0.01601(16) 0.01617(17) 0.01727(16) 0.000 0.00429(12) 0.000 P1 0.0189(2) 0.0179(2) 0.0176(2) -0.00002(19) 0.00238(19) 0.0030(2) C11 0.0203(9) 0.0181(10) 0.0241(10) -0.0011(8) 0.0045(8) 0.0032(8) C12 0.0324(11) 0.0280(11) 0.0274(11) 0.0008(9) 0.0031(9) 0.0072(10) C13 0.0338(12) 0.0263(12) 0.0437(13) 0.0015(10) 0.0048(10) 0.0120(10) C14 0.0349(12) 0.0305(13) 0.0525(15) -0.0098(11) 0.0165(11) 0.0086(11) C15 0.0444(13) 0.0422(14) 0.0310(12) -0.0091(10) 0.0145(10) 0.0079(12) C16 0.0307(11) 0.0269(11) 0.0260(11) 0.0010(8) 0.0074(9) 0.0064(9) C21 0.0219(9) 0.0248(11) 0.0144(9) 0.0002(8) 0.0014(7) -0.0002(8) C22 0.0243(10) 0.0255(11) 0.0250(10) 0.0004(8) 0.0012(8) 0.0048(9) C23 0.0191(10) 0.0385(13) 0.0323(11) 0.0019(10) 0.0018(9) -0.0007(10) C24 0.0279(11) 0.0346(13) 0.0322(12) -0.0042(10) 0.0028(9) -0.0088(10) C25 0.0341(12) 0.0245(11) 0.0303(11) -0.0079(9) 0.0084(9) -0.0019(10) C26 0.0216(10) 0.0282(11) 0.0203(9) -0.0039(8) 0.0040(8) -0.0003(9) C31 0.0211(10) 0.0242(11) 0.0224(10) 0.0046(8) 0.0055(8) 0.0088(9) C32 0.0300(11) 0.0314(12) 0.0232(10) 0.0024(9) 0.0046(9) 0.0099(10) C33 0.0430(14) 0.0517(16) 0.0207(11) 0.0057(10) 0.0080(10) 0.0198(13) C34 0.0416(14) 0.0535(16) 0.0386(13) 0.0233(12) 0.0206(11) 0.0216(13) C35 0.0350(13) 0.0424(14) 0.0487(15) 0.0180(12) 0.0153(11) 0.0058(11) C36 0.0294(11) 0.0319(12) 0.0346(12) 0.0060(10) 0.0060(9) 0.0000(10) N4 0.0164(7) 0.0191(8) 0.0181(7) -0.0009(6) 0.0061(6) -0.0003(7) C41 0.0207(9) 0.0177(9) 0.0200(9) -0.0058(7) 0.0094(8) -0.0012(8) C42 0.0229(10) 0.0201(10) 0.0189(9) -0.0029(8) 0.0055(8) -0.0005(8) C43 0.0192(9) 0.0214(10) 0.0251(10) -0.0046(8) 0.0079(8) -0.0017(8) C44 0.0250(10) 0.0249(11) 0.0282(10) -0.0011(9) 0.0144(8) -0.0032(9) C45 0.0297(11) 0.0247(11) 0.0240(10) 0.0024(8) 0.0110(8) 0.0031(9) C46 0.0202(9) 0.0269(11) 0.0224(10) -0.0002(8) 0.0065(8) 0.0038(8) C431 0.0244(11) 0.0383(13) 0.0311(11) 0.0009(10) 0.0081(9) -0.0044(10) F431 0.0264(7) 0.0483(9) 0.0847(11) 0.0264(8) 0.0099(7) 0.0079(7) F432 0.0226(6) 0.0875(12) 0.0432(8) -0.0022(7) 0.0150(6) 0.0053(7) F433 0.0318(7) 0.0605(10) 0.0420(8) -0.0071(7) -0.0036(6) -0.0129(7) C451 0.0329(13) 0.0668(19) 0.0417(14) 0.0251(13) 0.0206(11) 0.0108(13) F451 0.076(2) 0.202(5) 0.0485(14) 0.069(2) 0.0495(14) 0.086(3) F452 0.0732(17) 0.0461(15) 0.0828(17) 0.0399(13) -0.0061(14) -0.0177(13) F453 0.0477(15) 0.045(2) 0.0331(14) 0.0142(15) -0.0009(10) -0.0020(16) C5 0.0168(9) 0.0196(10) 0.0229(10) -0.0048(8) 0.0042(8) 0.0007(8) C51 0.0221(13) 0.0153(13) 0.0308(15) 0.000 0.0083(12) 0.000 C52 0.0308(11) 0.0215(11) 0.0405(13) -0.0077(9) 0.0155(10) -0.0026(9) F521 0.0512(8) 0.0239(7) 0.0647(9) -0.0201(6) 0.0301(7) -0.0109(6) F522 0.0285(7) 0.0375(8) 0.0792(10) -0.0132(7) 0.0134(7) 0.0127(6) F523 0.0686(9) 0.0384(8) 0.0380(7) -0.0140(6) 0.0306(7) -0.0029(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Cu N4 2.0929(15) 2_656 ? Cu N4 2.0929(15) . ? Cu P1 2.2953(5) 2_656 ? Cu P1 2.2953(5) . ? P1 C11 1.8258(19) . ? P1 C21 1.8318(19) . ? P1 C31 1.8343(19) . ? C11 C12 1.388(3) . ? C11 C16 1.390(3) . ? C12 C13 1.380(3) . ? C12 H12 0.9300 . ? C13 C14 1.375(3) . ? C13 H13 0.9300 . ? C14 C15 1.381(3) . ? C14 H14 0.9300 . ? C15 C16 1.386(3) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C21 C26 1.394(3) . ? C21 C22 1.394(3) . ? C22 C23 1.391(3) . ? C22 H22 0.9300 . ? C23 C24 1.374(3) . ? C23 H23 0.9300 . ? C24 C25 1.385(3) . ? C24 H24 0.9300 . ? C25 C26 1.383(3) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C31 C32 1.382(3) . ? C31 C36 1.394(3) . ? C32 C33 1.385(3) . ? C32 H32 0.9300 . ? C33 C34 1.376(4) . ? C33 H33 0.9300 . ? C34 C35 1.373(3) . ? C34 H34 0.9300 . ? C35 C36 1.380(3) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? N4 C5 1.316(2) . ? N4 C41 1.424(2) . ? C41 C42 1.391(3) . ? C41 C46 1.398(3) . ? C42 C43 1.389(3) . ? C42 H42 0.9300 . ? C43 C44 1.384(3) . ? C43 C431 1.500(3) . ? C44 C45 1.382(3) . ? C44 H44 0.9300 . ? C45 C46 1.388(3) . ? C45 C451 1.492(3) . ? C46 H46 0.9300 . ? C431 F431 1.330(2) . ? C431 F433 1.336(2) . ? C431 F432 1.339(2) . ? C451 F454 1.143(10) . ? C451 F456 1.25(3) . ? C451 F451 1.304(3) . ? C451 F453 1.322(5) . ? C451 F452 1.392(4) . ? C451 F455 1.528(9) . ? F451 F455 1.011(8) . ? F451 F454 1.249(11) . ? F452 F454 0.962(12) . ? C5 C51 1.398(2) . ? C5 C52 1.538(3) . ? C51 C5 1.398(2) 2_656 ? C51 H51 0.9300 . ? C52 F521 1.334(2) . ? C52 F523 1.336(2) . ? C52 F522 1.339(2) . ? C91 C94 1.08(4) . ? C91 C93 1.09(3) . ? C91 C95 1.10(2) 5_566 ? C91 C92 1.30(3) . ? C91 C96 1.35(7) . ? C92 C95 1.01(2) 5_566 ? C92 C100 1.19(3) 5_566 ? C92 C99 1.51(6) . ? C92 C93 1.67(4) . ? C92 C100 1.69(4) . ? C93 C99 1.01(5) . ? C93 C94 1.10(4) . ? C93 C98 1.06(3) . ? C93 C97 1.41(4) . ? C93 C96 1.54(7) 2 ? C94 C95 1.36(4) 5_566 ? C94 C96 1.55(8) . ? C95 C92 1.01(2) 5_566 ? C95 C100 1.03(2) . ? C95 C91 1.10(2) 5_566 ? C95 C94 1.36(4) 5_566 ? C95 C99 1.67(6) 5_566 ? C96 C93 1.54(7) 2 ? C96 C99 1.71(9) 2 ? C97 C99 1.16(6) . ? C97 C99 1.16(6) 2 ? C97 C98 1.16(6) . ? C97 C93 1.41(4) 2 ? C98 C93 1.06(3) 2 ? C98 C99 1.63(5) 2 ? C98 C99 1.63(5) . ? C99 C96 1.71(9) 2 ? C99 C95 1.67(6) 5_566 ? C100 C92 1.19(3) 5_566 ? 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 N4 Cu N4 94.65(8) 2_656 . ? N4 Cu P1 113.31(4) 2_656 2_656 ? N4 Cu P1 102.67(4) . 2_656 ? N4 Cu P1 102.67(4) 2_656 . ? N4 Cu P1 113.31(4) . . ? P1 Cu P1 126.03(3) 2_656 . ? C11 P1 C21 104.14(9) . . ? C11 P1 C31 101.32(9) . . ? C21 P1 C31 102.85(9) . . ? C11 P1 Cu 118.67(6) . . ? C21 P1 Cu 108.83(6) . . ? C31 P1 Cu 119.03(6) . . ? C12 C11 C16 118.17(18) . . ? C12 C11 P1 122.86(15) . . ? C16 C11 P1 118.97(14) . . ? C13 C12 C11 121.03(19) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C14 C13 C12 120.6(2) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C15 119.1(2) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C14 C15 C16 120.6(2) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C16 C11 120.50(19) . . ? C15 C16 H16 119.8 . . ? C11 C16 H16 119.8 . . ? C26 C21 C22 118.90(18) . . ? C26 C21 P1 117.30(14) . . ? C22 C21 P1 123.79(15) . . ? C23 C22 C21 119.71(19) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C24 C23 C22 120.9(2) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C24 C25 119.8(2) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C26 C25 C24 119.9(2) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C21 120.80(19) . . ? C25 C26 H26 119.6 . . ? C21 C26 H26 119.6 . . ? C32 C31 C36 118.78(19) . . ? C32 C31 P1 123.68(16) . . ? C36 C31 P1 117.54(15) . . ? C31 C32 C33 120.4(2) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C34 C33 C32 120.4(2) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C35 C34 C33 119.6(2) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C34 C35 C36 120.4(2) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C35 C36 C31 120.4(2) . . ? C35 C36 H36 119.8 . . ? C31 C36 H36 119.8 . . ? C5 N4 C41 119.75(16) . . ? C5 N4 Cu 120.70(12) . . ? C41 N4 Cu 118.92(12) . . ? C42 C41 C46 118.82(17) . . ? C42 C41 N4 120.49(16) . . ? C46 C41 N4 120.68(16) . . ? C43 C42 C41 120.35(17) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C44 C43 C42 120.89(18) . . ? C44 C43 C431 119.74(17) . . ? C42 C43 C431 119.36(17) . . ? C45 C44 C43 118.69(17) . . ? C45 C44 H44 120.7 . . ? C43 C44 H44 120.7 . . ? C44 C45 C46 121.33(18) . . ? C44 C45 C451 117.69(18) . . ? C46 C45 C451 120.98(18) . . ? C45 C46 C41 119.87(18) . . ? C45 C46 H46 120.1 . . ? C41 C46 H46 120.1 . . ? F431 C431 F433 106.57(17) . . ? F431 C431 F432 106.99(18) . . ? F433 C431 F432 105.83(17) . . ? F431 C431 C43 112.54(17) . . ? F433 C431 C43 112.55(18) . . ? F432 C431 C43 111.90(17) . . ? F454 C451 F456 113.7(12) . . ? F454 C451 F451 61.0(6) . . ? F456 C451 F451 119.1(11) . . ? F454 C451 F453 122.9(6) . . ? F456 C451 F453 16.1(10) . . ? F451 C451 F453 110.1(3) . . ? F454 C451 F452 43.2(6) . . ? F456 C451 F452 88.9(9) . . ? F451 C451 F452 103.8(3) . . ? F453 C451 F452 104.4(3) . . ? F454 C451 C45 120.3(5) . . ? F456 C451 C45 117.7(12) . . ? F451 C451 C45 113.0(2) . . ? F453 C451 C45 114.7(2) . . ? F452 C451 C45 109.9(2) . . ? F454 C451 F455 100.5(7) . . ? F456 C451 F455 95.3(10) . . ? F451 C451 F455 40.9(3) . . ? F453 C451 F455 80.7(4) . . ? F452 C451 F455 140.3(4) . . ? C45 C451 F455 102.9(4) . . ? F455 F451 F454 132.2(8) . . ? F455 F451 C451 81.6(6) . . ? F454 F451 C451 53.1(5) . . ? F454 F452 C451 54.4(6) . . ? F452 F454 C451 82.3(9) . . ? F452 F454 F451 147.1(11) . . ? C451 F454 F451 65.9(6) . . ? F451 F455 C451 57.5(5) . . ? N4 C5 C51 127.02(19) . . ? N4 C5 C52 120.29(16) . . ? C51 C5 C52 112.68(18) . . ? C5 C51 C5 129.9(3) 2_656 . ? C5 C51 H51 115.1 2_656 . ? C5 C51 H51 115.1 . . ? F521 C52 F523 105.84(17) . . ? F521 C52 F522 105.97(17) . . ? F523 C52 F522 106.83(17) . . ? F521 C52 C5 112.97(16) . . ? F523 C52 C5 112.42(17) . . ? F522 C52 C5 112.28(17) . . ? C99 C91 C95 107(4) . 5_566 ? C92 C91 C96 109(3) . . ? C92 C91 C98 115(2) . . ? C95 C91 C97 133(2) 5_566 . ? C92 C91 C97 103(2) . . ? C99 C91 C100 114(4) . . ? C99 C91 C100 105(4) . 5_566 ? C93 C91 C100 121(2) . 5_566 ? C97 C91 C100 130.6(16) . 5_566 ? C94 C92 C95 106(5) . 5_566 ? C100 C92 C91 109(3) 5_566 . ? C100 C92 C99 133(3) 5_566 . ? C95 C92 C93 96(2) 5_566 . ? C94 C92 C100 134(5) . . ? C99 C92 C100 107(2) . . ? C93 C92 C100 124.1(18) . . ? C96 C93 C94 107(6) . . ? C99 C93 C98 103(5) . . ? C91 C93 C98 123(3) . . ? C91 C93 C97 102(3) . . ? C94 C93 C97 100(3) . . ? C91 C93 C96 123(3) . 2 ? C94 C93 C96 124(4) . 2 ? C96 C93 C92 117(7) . . ? C97 C93 C92 113(2) . . ? C96 C93 C95 102(6) . 5_566 ? C97 C93 C95 108.3(18) . 5_566 ? C96 C93 C95 135(3) 2 5_566 ? C92 C94 C99 133(7) . . ? C92 C94 C91 92(5) . . ? C99 C94 C95 90(4) . 5_566 ? C93 C94 C95 111(3) . 5_566 ? C95 C94 C96 107(4) 5_566 . ? C99 C94 C100 121(5) . 5_566 ? C95 C94 C97 117(3) 5_566 . ? C100 C95 C92 120(3) 5_566 5_566 ? C100 C95 C94 99(3) . 5_566 ? C100 C95 C99 131(3) . 5_566 ? C92 C95 C95 94(2) 5_566 5_566 ? C94 C95 C95 122(3) 5_566 5_566 ? C100 C95 C93 123.7(19) . 5_566 ? C98 C96 C97 99(10) . . ? C97 C96 C93 135(8) . . ? C97 C96 C99 95(10) . . ? C93 C96 C96 118(9) . 2 ? C98 C96 C91 120(8) . . ? C98 C96 C94 123(7) . . ? C97 C96 C94 111(7) . . ? C96 C96 C94 134(8) 2 . ? C93 C96 C93 122(9) . 2 ? C93 C96 C99 135(6) . 2 ? C99 C96 C99 125(10) . 2 ? C96 C97 C99 132(9) 2 . ? C96 C97 C99 132(9) . 2 ? C99 C97 C93 134(5) 2 . ? C99 C97 C93 134(5) . 2 ? C93 C97 C93 96(4) . 2 ? C96 C97 C94 117(7) . 2 ? C93 C97 C94 130(3) . 2 ? C96 C97 C94 117(7) 2 . ? C93 C97 C94 130(3) 2 . ? C96 C97 C91 113(8) 2 . ? C93 C97 C91 112(3) 2 . ? C96 C97 C91 113(8) . 2 ? C93 C97 C91 112(3) . 2 ? C96 C98 C93 110(7) . 2 ? C96 C98 C93 110(7) 2 . ? C93 C98 C99 121(4) . 2 ? C93 C98 C99 121(4) 2 . ? C99 C98 C99 91(4) 2 . ? C96 C98 C91 113(6) . 2 ? C99 C98 C91 120(3) . 2 ? C96 C98 C91 113(6) 2 . ? C99 C98 C91 120(3) 2 . ? C96 C99 C94 117(8) . . ? C96 C99 C91 95(7) . . ? C94 C99 C97 131(5) . . ? C91 C99 C97 132(6) . . ? C96 C99 C92 131(8) . . ? C94 C99 C98 106(5) . . ? C92 C99 C98 120(3) . . ? C94 C99 C96 120(5) . 2 ? C91 C99 C96 117(4) . 2 ? C96 C99 C95 134(8) . 5_566 ? C93 C99 C95 95(5) . 5_566 ? C98 C99 C95 127(3) . 5_566 ? C95 C100 C95 131(2) 5_566 . ? C100 C100 C92 113(4) 5_566 5_566 ? C95 C100 C92 99.8(13) . . ? C100 C100 C94 106(3) 5_566 5_566 ? C92 C100 C91 116.8(13) . 5_566 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Cu P1 C11 85.50(8) 2_656 . . . ? N4 Cu P1 C11 -173.69(8) . . . . ? P1 Cu P1 C11 -46.19(7) 2_656 . . . ? N4 Cu P1 C21 -33.23(8) 2_656 . . . ? N4 Cu P1 C21 67.57(8) . . . . ? P1 Cu P1 C21 -164.92(6) 2_656 . . . ? N4 Cu P1 C31 -150.49(9) 2_656 . . . ? N4 Cu P1 C31 -49.69(9) . . . . ? P1 Cu P1 C31 77.82(8) 2_656 . . . ? C21 P1 C11 C12 -80.78(18) . . . . ? C31 P1 C11 C12 25.74(19) . . . . ? Cu P1 C11 C12 158.08(15) . . . . ? C21 P1 C11 C16 99.39(17) . . . . ? C31 P1 C11 C16 -154.09(16) . . . . ? Cu P1 C11 C16 -21.76(19) . . . . ? C16 C11 C12 C13 0.2(3) . . . . ? P1 C11 C12 C13 -179.68(17) . . . . ? C11 C12 C13 C14 -0.2(3) . . . . ? C12 C13 C14 C15 0.2(4) . . . . ? C13 C14 C15 C16 -0.2(4) . . . . ? C14 C15 C16 C11 0.1(3) . . . . ? C12 C11 C16 C15 -0.1(3) . . . . ? P1 C11 C16 C15 179.71(17) . . . . ? C11 P1 C21 C26 -166.06(14) . . . . ? C31 P1 C21 C26 88.57(15) . . . . ? Cu P1 C21 C26 -38.56(15) . . . . ? C11 P1 C21 C22 12.53(18) . . . . ? C31 P1 C21 C22 -92.84(17) . . . . ? Cu P1 C21 C22 140.02(14) . . . . ? C26 C21 C22 C23 -0.5(3) . . . . ? P1 C21 C22 C23 -179.11(15) . . . . ? C21 C22 C23 C24 -0.2(3) . . . . ? C22 C23 C24 C25 0.7(3) . . . . ? C23 C24 C25 C26 -0.5(3) . . . . ? C24 C25 C26 C21 -0.3(3) . . . . ? C22 C21 C26 C25 0.8(3) . . . . ? P1 C21 C26 C25 179.43(15) . . . . ? C11 P1 C31 C32 -113.36(17) . . . . ? C21 P1 C31 C32 -5.82(19) . . . . ? Cu P1 C31 C32 114.53(16) . . . . ? C11 P1 C31 C36 67.05(17) . . . . ? C21 P1 C31 C36 174.59(16) . . . . ? Cu P1 C31 C36 -65.06(17) . . . . ? C36 C31 C32 C33 -0.3(3) . . . . ? P1 C31 C32 C33 -179.93(16) . . . . ? C31 C32 C33 C34 0.1(3) . . . . ? C32 C33 C34 C35 0.0(3) . . . . ? C33 C34 C35 C36 0.0(3) . . . . ? C34 C35 C36 C31 -0.2(3) . . . . ? C32 C31 C36 C35 0.4(3) . . . . ? P1 C31 C36 C35 179.99(17) . . . . ? N4 Cu N4 C5 0.97(11) 2_656 . . . ? P1 Cu N4 C5 116.14(13) 2_656 . . . ? P1 Cu N4 C5 -104.97(13) . . . . ? N4 Cu N4 C41 -169.92(15) 2_656 . . . ? P1 Cu N4 C41 -54.76(13) 2_656 . . . ? P1 Cu N4 C41 84.13(13) . . . . ? C5 N4 C41 C42 -65.3(2) . . . . ? Cu N4 C41 C42 105.68(17) . . . . ? C5 N4 C41 C46 116.1(2) . . . . ? Cu N4 C41 C46 -72.91(19) . . . . ? C46 C41 C42 C43 -2.7(3) . . . . ? N4 C41 C42 C43 178.73(17) . . . . ? C41 C42 C43 C44 1.8(3) . . . . ? C41 C42 C43 C431 -177.60(17) . . . . ? C42 C43 C44 C45 -0.6(3) . . . . ? C431 C43 C44 C45 178.80(19) . . . . ? C43 C44 C45 C46 0.3(3) . . . . ? C43 C44 C45 C451 -179.1(2) . . . . ? C44 C45 C46 C41 -1.2(3) . . . . ? C451 C45 C46 C41 178.2(2) . . . . ? C42 C41 C46 C45 2.4(3) . . . . ? N4 C41 C46 C45 -179.04(17) . . . . ? C44 C43 C431 F431 -145.69(19) . . . . ? C42 C43 C431 F431 33.7(3) . . . . ? C44 C43 C431 F433 93.9(2) . . . . ? C42 C43 C431 F433 -86.7(2) . . . . ? C44 C43 C431 F432 -25.2(3) . . . . ? C42 C43 C431 F432 154.27(18) . . . . ? C44 C45 C451 F454 -37.6(9) . . . . ? C46 C45 C451 F454 142.9(8) . . . . ? C44 C45 C451 F456 176.0(11) . . . . ? C46 C45 C451 F456 -3.4(11) . . . . ? C44 C45 C451 F451 31.1(4) . . . . ? C46 C45 C451 F451 -148.4(3) . . . . ? C44 C45 C451 F453 158.4(3) . . . . ? C46 C45 C451 F453 -21.0(4) . . . . ? C44 C45 C451 F452 -84.4(3) . . . . ? C46 C45 C451 F452 96.2(3) . . . . ? C44 C45 C451 F455 72.9(5) . . . . ? C46 C45 C451 F455 -106.5(5) . . . . ? F454 C451 F451 F455 -163.8(8) . . . . ? F456 C451 F451 F455 -61.3(12) . . . . ? F453 C451 F451 F455 -46.6(6) . . . . ? F452 C451 F451 F455 -157.8(6) . . . . ? C45 C451 F451 F455 83.1(6) . . . . ? F456 C451 F451 F454 102.6(12) . . . . ? F453 C451 F451 F454 117.3(6) . . . . ? F452 C451 F451 F454 6.0(6) . . . . ? C45 C451 F451 F454 -113.0(6) . . . . ? F455 C451 F451 F454 163.8(8) . . . . ? F456 C451 F452 F454 -127.4(14) . . . . ? F451 C451 F452 F454 -7.7(7) . . . . ? F453 C451 F452 F454 -123.1(7) . . . . ? C45 C451 F452 F454 113.4(7) . . . . ? F455 C451 F452 F454 -30.5(10) . . . . ? C451 F452 F454 F451 14.5(14) . . . . ? F456 C451 F454 F452 60.1(13) . . . . ? F451 C451 F454 F452 171.4(8) . . . . ? F453 C451 F454 F452 75.1(8) . . . . ? C45 C451 F454 F452 -87.4(8) . . . . ? F455 C451 F454 F452 160.7(6) . . . . ? F456 C451 F454 F451 -111.3(12) . . . . ? F453 C451 F454 F451 -96.3(7) . . . . ? F452 C451 F454 F451 -171.4(8) . . . . ? C45 C451 F454 F451 101.1(5) . . . . ? F455 C451 F454 F451 -10.7(5) . . . . ? F455 F451 F454 F452 6(2) . . . . ? C451 F451 F454 F452 -15.8(15) . . . . ? F455 F451 F454 C451 21.8(10) . . . . ? F454 F451 F455 C451 -17.5(8) . . . . ? F454 C451 F455 F451 14.3(7) . . . . ? F456 C451 F455 F451 129.7(12) . . . . ? F453 C451 F455 F451 136.3(5) . . . . ? F452 C451 F455 F451 35.0(8) . . . . ? C45 C451 F455 F451 -110.3(5) . . . . ? C41 N4 C5 C51 168.71(15) . . . . ? Cu N4 C5 C51 -2.1(2) . . . . ? C41 N4 C5 C52 -12.4(3) . . . . ? Cu N4 C5 C52 176.79(13) . . . . ? N4 C5 C51 C5 1.27(14) . . . 2_656 ? C52 C5 C51 C5 -177.70(16) . . . 2_656 ? N4 C5 C52 F521 -156.49(17) . . . . ? C51 C5 C52 F521 22.6(2) . . . . ? N4 C5 C52 F523 -36.8(2) . . . . ? C51 C5 C52 F523 142.27(15) . . . . ? N4 C5 C52 F522 83.7(2) . . . . ? C51 C5 C52 F522 -97.22(18) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.361 _refine_diff_density_min -0.332 _refine_diff_density_rms 0.055 #===END data_norac1 _database_code_depnum_ccdc_archive 'CCDC 800529' #TrackingRef '- nora_combined_cif.cif' _audit_creation_method 'SHELXL-97 and CrysAlisPro RED' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_structural 'Ar-NC(CF3)CHC(CF3)NH-Ar, Ar= C6H3(CF3)2-3,5' _chemical_formula_moiety 'C21 H8 F18 N2' _chemical_formula_sum 'C21 H8 F18 N2' _chemical_formula_weight 630.29 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.0973(13) _cell_length_b 7.9809(5) _cell_length_c 15.6913(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.109(6) _cell_angle_gamma 90.00 _cell_volume 2264.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.849 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.214 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.873 _exptl_absorpt_correction_T_max 1.116 _exptl_absorpt_process_details ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_reflns_number 15811 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0404 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.78 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2567 _reflns_number_gt 1656 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlisPro CCD, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_cell_refinement ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_data_reduction ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Johnson, 1976 and Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0619P)^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 2567 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0758 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.1085 _refine_ls_wR_factor_gt 0.1006 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _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 C1 C 0.40046(10) 0.7086(2) 0.37147(11) 0.0244(4) Uani 1 1 d . . . C2 C 0.33709(10) 0.6356(2) 0.34096(11) 0.0252(4) Uani 1 1 d . . . H2 H 0.3236 0.6463 0.2835 0.030 Uiso 1 1 calc R . . C3 C 0.29112(10) 0.5435(2) 0.39518(11) 0.0255(4) Uani 1 1 d . . . C4 C 0.30802(11) 0.5205(2) 0.47965(11) 0.0265(4) Uani 1 1 d . . . H4 H 0.2776 0.4598 0.5148 0.032 Uiso 1 1 calc R . . C5 C 0.37197(11) 0.5917(2) 0.50927(11) 0.0273(4) Uani 1 1 d . . . C6 C 0.41832(10) 0.6858(2) 0.45577(11) 0.0280(4) Uani 1 1 d . . . H6 H 0.4617 0.7327 0.4788 0.034 Uiso 1 1 calc R . . C31 C 0.22314(12) 0.4635(3) 0.36349(13) 0.0336(5) Uani 1 1 d . . . F31A F 0.20664(9) 0.5118(3) 0.28538(9) 0.0629(7) Uani 0.893(3) 1 d P . . F31B F 0.16346(8) 0.4974(3) 0.41050(12) 0.0730(8) Uani 0.893(3) 1 d P . . F31C F 0.22918(10) 0.2990(2) 0.35791(17) 0.0866(9) Uani 0.893(3) 1 d P . . F31D F 0.1976(6) 0.3423(14) 0.4217(7) 0.030(3) Uiso 0.107(3) 1 d P . . F31E F 0.2335(7) 0.386(2) 0.2989(9) 0.048(4) Uiso 0.107(3) 1 d P . . F31F F 0.1725(10) 0.561(2) 0.3527(13) 0.073(5) Uiso 0.107(3) 1 d P . . C51 C 0.39066(12) 0.5628(3) 0.60006(13) 0.0386(5) Uani 1 1 d . . . F51A F 0.33267(8) 0.5905(2) 0.65342(8) 0.0655(5) Uani 1 1 d . . . F51B F 0.40990(8) 0.40542(19) 0.61478(9) 0.0609(4) Uani 1 1 d . . . F51C F 0.44534(10) 0.6564(2) 0.62486(8) 0.0875(6) Uani 1 1 d . . . N1 N 0.44788(8) 0.80040(19) 0.31382(9) 0.0267(4) Uani 1 1 d . . . H1 H 0.4745 0.7421 0.2806 0.032 Uiso 0.50 1 calc PR . . C11 C 0.45310(10) 0.9646(2) 0.30868(11) 0.0223(4) Uani 1 1 d . . . C12 C 0.5000 1.0472(3) 0.2500 0.0226(5) Uani 1 2 d S . . H12 H 0.5000 1.1637 0.2500 0.027 Uiso 1 2 calc SR . . C13 C 0.40836(10) 1.0743(2) 0.37090(12) 0.0274(4) Uani 1 1 d . . . F13A F 0.33900(6) 1.02040(14) 0.38417(8) 0.0364(3) Uani 1 1 d . . . F13B F 0.43923(7) 1.07675(16) 0.44712(7) 0.0417(3) Uani 1 1 d . . . F13C F 0.40441(6) 1.23151(14) 0.34488(7) 0.0401(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 C1 0.0261(10) 0.0227(10) 0.0250(10) -0.0014(8) 0.0087(7) 0.0001(8) C2 0.0291(10) 0.0262(10) 0.0204(9) -0.0029(7) 0.0015(7) 0.0016(8) C3 0.0253(10) 0.0254(10) 0.0260(10) -0.0037(8) 0.0034(8) 0.0011(8) C4 0.0292(10) 0.0274(10) 0.0234(10) 0.0010(8) 0.0078(8) -0.0041(8) C5 0.0290(10) 0.0306(10) 0.0224(9) -0.0009(8) 0.0028(7) -0.0036(9) C6 0.0270(10) 0.0313(11) 0.0258(10) -0.0032(8) 0.0026(8) -0.0055(8) C31 0.0312(11) 0.0358(12) 0.0336(12) -0.0001(9) 0.0003(9) -0.0033(10) F31A 0.0505(10) 0.0987(16) 0.0378(10) 0.0158(8) -0.0197(7) -0.0310(10) F31B 0.0271(8) 0.144(2) 0.0485(11) -0.0342(11) 0.0096(7) -0.0223(10) F31C 0.0678(13) 0.0349(10) 0.153(2) -0.0058(12) -0.0553(13) -0.0117(9) C51 0.0396(12) 0.0497(14) 0.0262(11) 0.0044(10) -0.0010(9) -0.0143(11) F51A 0.0669(10) 0.1074(13) 0.0226(7) 0.0066(7) 0.0081(6) 0.0145(9) F51B 0.0671(10) 0.0696(10) 0.0448(8) 0.0168(7) -0.0159(7) 0.0077(8) F51C 0.1030(13) 0.1233(15) 0.0341(8) 0.0172(8) -0.0260(8) -0.0778(12) N1 0.0299(9) 0.0240(9) 0.0268(9) -0.0010(6) 0.0076(6) -0.0010(7) C11 0.0201(9) 0.0260(10) 0.0206(9) -0.0007(7) -0.0032(7) 0.0015(8) C12 0.0242(13) 0.0227(13) 0.0209(13) 0.000 -0.0009(10) 0.000 C13 0.0247(10) 0.0301(11) 0.0278(10) -0.0008(8) 0.0050(8) -0.0010(8) F13A 0.0248(6) 0.0383(7) 0.0467(7) -0.0044(5) 0.0093(5) 0.0014(5) F13B 0.0453(8) 0.0524(8) 0.0272(6) -0.0126(5) -0.0008(5) 0.0009(6) F13C 0.0447(7) 0.0261(6) 0.0504(8) 0.0001(5) 0.0163(6) 0.0074(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.357(3) . ? C1 C6 1.362(3) . ? C1 N1 1.466(2) . ? C2 C3 1.417(3) . ? C2 H2 0.9300 . ? C3 C4 1.362(3) . ? C3 C31 1.457(3) . ? C4 C5 1.356(3) . ? C4 H4 0.9300 . ? C5 C6 1.423(3) . ? C5 C51 1.470(3) . ? C6 H6 0.9300 . ? C31 F31F 1.208(17) . ? C31 F31E 1.209(13) . ? C31 F31A 1.309(3) . ? C31 F31C 1.321(3) . ? C31 F31B 1.357(3) . ? C31 F31D 1.420(10) . ? F31A F31E 1.134(16) . ? F31A F31F 1.30(2) . ? F31B F31F 1.055(19) . ? F31B F31D 1.392(11) . ? F31C F31E 1.160(15) . ? F31C F31D 1.221(11) . ? C51 F51C 1.288(2) . ? C51 F51B 1.322(3) . ? C51 F51A 1.384(3) . ? N1 C11 1.316(2) . ? N1 H1 0.8600 . ? C11 C12 1.435(2) . ? C11 C13 1.560(3) . ? C12 C11 1.435(2) 2_655 ? C12 H12 0.9300 . ? C13 F13B 1.302(2) . ? C13 F13C 1.320(2) . ? C13 F13A 1.350(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 C2 C1 C6 116.90(16) . . ? C2 C1 N1 120.20(16) . . ? C6 C1 N1 122.85(17) . . ? C1 C2 C3 121.18(17) . . ? C1 C2 H2 119.4 . . ? C3 C2 H2 119.4 . . ? C4 C3 C2 122.58(17) . . ? C4 C3 C31 115.45(16) . . ? C2 C3 C31 121.96(17) . . ? C5 C4 C3 115.81(16) . . ? C5 C4 H4 122.1 . . ? C3 C4 H4 122.1 . . ? C4 C5 C6 122.23(17) . . ? C4 C5 C51 115.43(17) . . ? C6 C5 C51 122.33(17) . . ? C1 C6 C5 121.29(17) . . ? C1 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? F31F C31 F31E 110.7(12) . . ? F31F C31 F31A 62.3(10) . . ? F31E C31 F31A 53.4(8) . . ? F31F C31 F31C 133.9(8) . . ? F31E C31 F31C 54.4(8) . . ? F31A C31 F31C 104.30(19) . . ? F31F C31 F31B 48.1(9) . . ? F31E C31 F31B 135.2(6) . . ? F31A C31 F31B 106.96(19) . . ? F31C C31 F31B 107.7(2) . . ? F31F C31 F31D 105.3(10) . . ? F31E C31 F31D 104.7(9) . . ? F31A C31 F31D 137.3(5) . . ? F31C C31 F31D 52.8(5) . . ? F31B C31 F31D 60.1(5) . . ? F31F C31 C3 113.2(8) . . ? F31E C31 C3 110.8(6) . . ? F31A C31 C3 110.57(17) . . ? F31C C31 C3 112.77(18) . . ? F31B C31 C3 113.95(17) . . ? F31D C31 C3 111.7(5) . . ? F31E F31A F31F 109.0(11) . . ? F31E F31A C31 58.8(7) . . ? F31F F31A C31 55.1(8) . . ? F31F F31B C31 58.5(10) . . ? F31F F31B F31D 116.9(11) . . ? C31 F31B F31D 62.2(4) . . ? F31E F31C F31D 122.2(9) . . ? F31E F31C C31 57.9(7) . . ? F31D F31C C31 67.8(5) . . ? F31C F31D F31B 111.5(7) . . ? F31C F31D C31 59.5(5) . . ? F31B F31D C31 57.7(4) . . ? F31A F31E F31C 129.6(12) . . ? F31A F31E C31 67.8(8) . . ? F31C F31E C31 67.7(8) . . ? F31B F31F C31 73.4(11) . . ? F31B F31F F31A 130.3(15) . . ? C31 F31F F31A 62.7(9) . . ? F51C C51 F51B 107.7(2) . . ? F51C C51 F51A 108.42(19) . . ? F51B C51 F51A 104.27(17) . . ? F51C C51 C5 110.40(17) . . ? F51B C51 C5 111.59(18) . . ? F51A C51 C5 114.12(18) . . ? C11 N1 C1 125.48(15) . . ? C11 N1 H1 117.3 . . ? C1 N1 H1 117.3 . . ? N1 C11 C12 122.81(17) . . ? N1 C11 C13 118.72(16) . . ? C12 C11 C13 118.44(17) . . ? C11 C12 C11 125.3(2) 2_655 . ? C11 C12 H12 117.3 2_655 . ? C11 C12 H12 117.3 . . ? F13B C13 F13C 106.65(16) . . ? F13B C13 F13A 103.47(14) . . ? F13C C13 F13A 108.09(16) . . ? F13B C13 C11 111.61(16) . . ? F13C C13 C11 111.31(14) . . ? F13A C13 C11 115.10(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 1.4(3) . . . . ? N1 C1 C2 C3 178.76(16) . . . . ? C1 C2 C3 C4 -1.1(3) . . . . ? C1 C2 C3 C31 -179.65(18) . . . . ? C2 C3 C4 C5 0.1(3) . . . . ? C31 C3 C4 C5 178.73(18) . . . . ? C3 C4 C5 C6 0.5(3) . . . . ? C3 C4 C5 C51 -178.59(18) . . . . ? C2 C1 C6 C5 -0.8(3) . . . . ? N1 C1 C6 C5 -178.11(18) . . . . ? C4 C5 C6 C1 -0.2(3) . . . . ? C51 C5 C6 C1 178.89(19) . . . . ? C4 C3 C31 F31F 103.6(11) . . . . ? C2 C3 C31 F31F -77.7(11) . . . . ? C4 C3 C31 F31E -131.4(9) . . . . ? C2 C3 C31 F31E 47.3(9) . . . . ? C4 C3 C31 F31A 171.26(19) . . . . ? C2 C3 C31 F31A -10.1(3) . . . . ? C4 C3 C31 F31C -72.4(2) . . . . ? C2 C3 C31 F31C 106.3(2) . . . . ? C4 C3 C31 F31B 50.8(3) . . . . ? C2 C3 C31 F31B -130.6(2) . . . . ? C4 C3 C31 F31D -15.0(6) . . . . ? C2 C3 C31 F31D 163.6(5) . . . . ? F31F C31 F31A F31E -152.6(12) . . . . ? F31C C31 F31A F31E -20.3(8) . . . . ? F31B C31 F31A F31E -134.2(8) . . . . ? F31D C31 F31A F31E -70.1(11) . . . . ? C3 C31 F31A F31E 101.2(8) . . . . ? F31E C31 F31A F31F 152.6(12) . . . . ? F31C C31 F31A F31F 132.4(9) . . . . ? F31B C31 F31A F31F 18.5(9) . . . . ? F31D C31 F31A F31F 82.5(11) . . . . ? C3 C31 F31A F31F -106.1(9) . . . . ? F31E C31 F31B F31F -76.8(16) . . . . ? F31A C31 F31B F31F -22.1(11) . . . . ? F31C C31 F31B F31F -133.7(11) . . . . ? F31D C31 F31B F31F -157.4(12) . . . . ? C3 C31 F31B F31F 100.4(11) . . . . ? F31F C31 F31B F31D 157.4(12) . . . . ? F31E C31 F31B F31D 80.6(13) . . . . ? F31A C31 F31B F31D 135.3(5) . . . . ? F31C C31 F31B F31D 23.7(5) . . . . ? C3 C31 F31B F31D -102.2(5) . . . . ? F31F C31 F31C F31E 85.1(16) . . . . ? F31A C31 F31C F31E 20.0(8) . . . . ? F31B C31 F31C F31E 133.4(8) . . . . ? F31D C31 F31C F31E 159.4(10) . . . . ? C3 C31 F31C F31E -100.0(8) . . . . ? F31F C31 F31C F31D -74.3(15) . . . . ? F31E C31 F31C F31D -159.4(10) . . . . ? F31A C31 F31C F31D -139.4(6) . . . . ? F31B C31 F31C F31D -26.0(6) . . . . ? C3 C31 F31C F31D 100.6(6) . . . . ? F31E F31C F31D F31B 5.3(13) . . . . ? C31 F31C F31D F31B 25.9(5) . . . . ? F31E F31C F31D C31 -20.6(9) . . . . ? F31F F31B F31D F31C -4.9(14) . . . . ? C31 F31B F31D F31C -26.5(5) . . . . ? F31F F31B F31D C31 21.5(11) . . . . ? F31F C31 F31D F31C 134.0(9) . . . . ? F31E C31 F31D F31C 17.2(9) . . . . ? F31A C31 F31D F31C 68.5(8) . . . . ? F31B C31 F31D F31C 151.2(6) . . . . ? C3 C31 F31D F31C -102.8(4) . . . . ? F31F C31 F31D F31B -17.2(9) . . . . ? F31E C31 F31D F31B -134.0(8) . . . . ? F31A C31 F31D F31B -82.7(7) . . . . ? F31C C31 F31D F31B -151.2(6) . . . . ? C3 C31 F31D F31B 106.0(3) . . . . ? F31F F31A F31E F31C 6.2(19) . . . . ? C31 F31A F31E F31C 29.7(11) . . . . ? F31F F31A F31E C31 -23.5(10) . . . . ? F31D F31C F31E F31A -7(2) . . . . ? C31 F31C F31E F31A -29.8(11) . . . . ? F31D F31C F31E C31 22.7(10) . . . . ? F31F C31 F31E F31A 25.8(12) . . . . ? F31C C31 F31E F31A 155.6(9) . . . . ? F31B C31 F31E F31A 76.6(11) . . . . ? F31D C31 F31E F31A 138.8(6) . . . . ? C3 C31 F31E F31A -100.7(5) . . . . ? F31F C31 F31E F31C -129.8(10) . . . . ? F31A C31 F31E F31C -155.6(9) . . . . ? F31B C31 F31E F31C -79.0(11) . . . . ? F31D C31 F31E F31C -16.8(8) . . . . ? C3 C31 F31E F31C 103.7(5) . . . . ? F31D F31B F31F C31 -22.4(11) . . . . ? C31 F31B F31F F31A 28.2(13) . . . . ? F31D F31B F31F F31A 6(2) . . . . ? F31E C31 F31F F31B 132.8(10) . . . . ? F31A C31 F31F F31B 156.0(11) . . . . ? F31C C31 F31F F31B 72.8(14) . . . . ? F31D C31 F31F F31B 20.2(10) . . . . ? C3 C31 F31F F31B -102.1(7) . . . . ? F31E C31 F31F F31A -23.2(10) . . . . ? F31C C31 F31F F31A -83.2(11) . . . . ? F31B C31 F31F F31A -156.0(11) . . . . ? F31D C31 F31F F31A -135.8(6) . . . . ? C3 C31 F31F F31A 101.9(5) . . . . ? F31E F31A F31F F31B -6(2) . . . . ? C31 F31A F31F F31B -30.7(14) . . . . ? F31E F31A F31F C31 24.6(10) . . . . ? C4 C5 C51 F51C -169.8(2) . . . . ? C6 C5 C51 F51C 11.1(3) . . . . ? C4 C5 C51 F51B 70.5(2) . . . . ? C6 C5 C51 F51B -108.6(2) . . . . ? C4 C5 C51 F51A -47.4(3) . . . . ? C6 C5 C51 F51A 133.5(2) . . . . ? C2 C1 N1 C11 104.4(2) . . . . ? C6 C1 N1 C11 -78.4(2) . . . . ? C1 N1 C11 C12 -179.20(14) . . . . ? C1 N1 C11 C13 2.8(3) . . . . ? N1 C11 C12 C11 -0.75(13) . . . 2_655 ? C13 C11 C12 C11 177.27(16) . . . 2_655 ? N1 C11 C13 F13B 76.6(2) . . . . ? C12 C11 C13 F13B -101.52(17) . . . . ? N1 C11 C13 F13C -164.38(17) . . . . ? C12 C11 C13 F13C 17.5(2) . . . . ? N1 C11 C13 F13A -41.0(2) . . . . ? C12 C11 C13 F13A 140.94(15) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.359 _refine_diff_density_min -0.226 _refine_diff_density_rms 0.050 #===END data_3a _database_code_depnum_ccdc_archive 'CCDC 800530' #TrackingRef '- nora_combined_cif.cif' _audit_creation_method 'SHELXL-97 and CrysAlisPro RED' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_structural '[(Ph3P)Au{N(C6H3-(CF3)2-3,5)C(CF3)=CHC(CF3)=N-C6H3-(CF3)2-3,5}]' _chemical_formula_moiety 'C39 H22 Au F18 N2 P' _chemical_formula_sum 'C39 H22 Au F18 N2 P' _chemical_formula_weight 1088.52 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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.7418(5) _cell_length_b 16.0248(4) _cell_length_c 25.9858(9) _cell_angle_alpha 90.00 _cell_angle_beta 111.892(3) _cell_angle_gamma 90.00 _cell_volume 7628.0(4) _cell_formula_units_Z 8 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.896 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4208 _exptl_absorpt_coefficient_mu 4.021 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.868 _exptl_absorpt_correction_T_max 1.110 _exptl_absorpt_process_details ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_reflns_number 76538 _diffrn_reflns_av_R_equivalents 0.1014 _diffrn_reflns_av_sigmaI/netI 0.0703 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 30.00 _reflns_number_total 11104 _reflns_number_gt 7971 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlisPro CCD, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_cell_refinement ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_data_reduction ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Johnson, 1976 and Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0516P)^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 11104 _refine_ls_number_parameters 546 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0766 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1049 _refine_ls_wR_factor_gt 0.0980 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.008 _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 0.187060(9) 0.131281(11) 0.121735(7) 0.02554(6) Uani 1 1 d . . . P1 P 0.30801(6) 0.13848(8) 0.14527(5) 0.0297(3) Uani 1 1 d . . . C11A C 0.3292(3) 0.2118(4) 0.1005(2) 0.0358(12) Uani 1 1 d . . . C12A C 0.2908(3) 0.2859(4) 0.0865(3) 0.0492(15) Uani 1 1 d . . . H12A H 0.2547 0.2974 0.1005 0.059 Uiso 1 1 calc R . . C13A C 0.3051(4) 0.3434(4) 0.0521(3) 0.0605(18) Uani 1 1 d . . . H13A H 0.2786 0.3928 0.0429 0.073 Uiso 1 1 calc R . . C14A C 0.3586(4) 0.3268(6) 0.0317(2) 0.065(2) Uani 1 1 d . . . H14A H 0.3693 0.3657 0.0093 0.079 Uiso 1 1 calc R . . C15A C 0.3962(3) 0.2532(6) 0.0444(2) 0.065(2) Uani 1 1 d . . . H15A H 0.4313 0.2417 0.0295 0.078 Uiso 1 1 calc R . . C16A C 0.3826(3) 0.1949(5) 0.0793(2) 0.0552(18) Uani 1 1 d . . . H16A H 0.4090 0.1454 0.0882 0.066 Uiso 1 1 calc R . . C11B C 0.3482(3) 0.0386(4) 0.1396(2) 0.0399(13) Uani 1 1 d . . . C12B C 0.3048(3) -0.0228(4) 0.1063(2) 0.0429(13) Uani 1 1 d . . . H12B H 0.2554 -0.0126 0.0868 0.052 Uiso 1 1 calc R . . C13B C 0.3336(3) -0.0982(4) 0.1016(3) 0.0520(15) Uani 1 1 d . . . H13B H 0.3041 -0.1386 0.0782 0.062 Uiso 1 1 calc R . . C14B C 0.4073(3) -0.1154(4) 0.1317(3) 0.0575(18) Uani 1 1 d . . . H14B H 0.4265 -0.1675 0.1291 0.069 Uiso 1 1 calc R . . C15B C 0.4512(4) -0.0545(5) 0.1652(3) 0.079(3) Uani 1 1 d . . . H15B H 0.5003 -0.0651 0.1851 0.095 Uiso 1 1 calc R . . C16B C 0.4217(3) 0.0233(4) 0.1693(3) 0.061(2) Uani 1 1 d . . . H16B H 0.4512 0.0646 0.1919 0.073 Uiso 1 1 calc R . . C11C C 0.3584(3) 0.1727(4) 0.2163(2) 0.0384(13) Uani 1 1 d . . . C12C C 0.3919(3) 0.2489(5) 0.2290(2) 0.061(2) Uani 1 1 d . . . H12C H 0.3914 0.2845 0.2006 0.074 Uiso 1 1 calc R . . C13C C 0.4268(4) 0.2734(6) 0.2842(3) 0.081(3) Uani 1 1 d . . . H13C H 0.4498 0.3250 0.2926 0.098 Uiso 1 1 calc R . . C14C C 0.4268(4) 0.2216(6) 0.3256(3) 0.074(3) Uani 1 1 d . . . H14C H 0.4497 0.2382 0.3624 0.089 Uiso 1 1 calc R . . C15C C 0.3938(6) 0.1458(5) 0.3139(3) 0.101(4) Uani 1 1 d . . . H15C H 0.3945 0.1107 0.3426 0.121 Uiso 1 1 calc R . . C16C C 0.3589(6) 0.1206(4) 0.2589(2) 0.086(3) Uani 1 1 d . . . H16C H 0.3360 0.0689 0.2508 0.104 Uiso 1 1 calc R . . N21 N 0.07400(19) 0.1285(2) 0.09402(16) 0.0251(8) Uani 1 1 d . . . C211 C 0.0375(2) 0.2034(3) 0.07114(18) 0.0205(8) Uani 1 1 d . . . C212 C 0.0730(3) 0.2801(3) 0.08798(18) 0.0263(10) Uani 1 1 d . . . H212 H 0.1195 0.2816 0.1156 0.032 Uiso 1 1 calc R . . C213 C 0.0394(3) 0.3536(3) 0.0637(2) 0.0402(13) Uani 1 1 d . . . C214 C -0.0287(3) 0.3544(3) 0.0219(2) 0.0369(12) Uani 1 1 d . . . H214 H -0.0503 0.4042 0.0054 0.044 Uiso 1 1 calc R . . C215 C -0.0637(2) 0.2792(3) 0.00533(18) 0.0257(9) Uani 1 1 d . . . C216 C -0.0321(2) 0.2058(3) 0.02911(19) 0.0254(9) Uani 1 1 d . . . H216 H -0.0573 0.1561 0.0170 0.031 Uiso 1 1 calc R . . C21A C 0.0725(5) 0.4389(6) 0.0866(4) 0.046(2) Uiso 0.683(8) 1 d P . . F21A F 0.0382(3) 0.4999(2) 0.07158(16) 0.0859(15) Uani 0.683(8) 1 d P . . F21B F 0.1264(4) 0.4470(4) 0.0646(3) 0.068(2) Uiso 0.683(8) 1 d P . . F21C F 0.1075(3) 0.4386(3) 0.1402(2) 0.0534(17) Uiso 0.683(8) 1 d P . . C21X C 0.0913(11) 0.4282(11) 0.0745(7) 0.033(4) Uiso 0.317(8) 1 d P . . F21X F 0.0382(3) 0.4999(2) 0.07158(16) 0.0859(15) Uani 0.317(8) 1 d P . . F21Y F 0.1080(7) 0.4514(8) 0.0244(6) 0.064(4) Uiso 0.317(8) 1 d P . . F21Z F 0.1566(10) 0.4218(11) 0.1069(7) 0.099(6) Uiso 0.317(8) 1 d P . . C21D C -0.1397(3) 0.2785(4) -0.0381(3) 0.0439(13) Uani 1 1 d . . . F21D F -0.15573(18) 0.2098(2) -0.06835(15) 0.0611(10) Uani 1 1 d . . . F21E F -0.1508(2) 0.3408(3) -0.07442(18) 0.0769(13) Uani 1 1 d . . . F21F F -0.1894(2) 0.2862(3) -0.01565(19) 0.0857(15) Uani 1 1 d . . . C22 C 0.0347(3) 0.0575(3) 0.0925(2) 0.0337(11) Uani 1 1 d . . . C221 C 0.0690(3) -0.0216(3) 0.0804(3) 0.0489(16) Uani 1 1 d . . . F22A F 0.02382(19) -0.08687(18) 0.07032(18) 0.0641(11) Uani 1 1 d . . . F22B F 0.12875(18) -0.04319(19) 0.12420(16) 0.0583(10) Uani 1 1 d . . . F22C F 0.08888(19) -0.0132(2) 0.03715(16) 0.0543(9) Uani 1 1 d . . . C23 C -0.0280(3) 0.0494(3) 0.1010(3) 0.0440(14) Uani 1 1 d . . . H23 H -0.0508 -0.0024 0.0930 0.053 Uiso 1 1 calc R . . C24 C -0.0639(3) 0.1141(3) 0.1217(3) 0.0424(14) Uani 1 1 d . . . C241 C -0.1460(3) 0.1176(4) 0.0925(4) 0.062(2) Uani 1 1 d . . . F24A F -0.16726(19) 0.1154(3) 0.0382(2) 0.0771(13) Uani 1 1 d . . . F24B F -0.1761(2) 0.1825(3) 0.10654(19) 0.0783(13) Uani 1 1 d . . . F24C F -0.1751(3) 0.0507(3) 0.1079(3) 0.1115(19) Uani 1 1 d . . . N25 N -0.0370(3) 0.1652(3) 0.1611(2) 0.0444(12) Uani 1 1 d . . . C251 C 0.0377(3) 0.1625(4) 0.1969(2) 0.0435(13) Uani 1 1 d . . . C252 C 0.0737(5) 0.0880(4) 0.2216(3) 0.066(2) Uani 1 1 d . . . H252 H 0.0487 0.0375 0.2139 0.080 Uiso 1 1 calc R . . C253 C 0.1456(6) 0.0902(6) 0.2571(3) 0.085(3) Uani 1 1 d . . . C254 C 0.1842(5) 0.1625(6) 0.2695(3) 0.075(2) Uani 1 1 d . . . H254 H 0.2331 0.1625 0.2929 0.090 Uiso 1 1 calc R . . C255 C 0.1494(3) 0.2361(4) 0.2468(2) 0.0490(16) Uani 1 1 d . . . C256 C 0.0772(3) 0.2362(3) 0.2115(2) 0.0366(12) Uani 1 1 d . . . H256 H 0.0546 0.2865 0.1972 0.044 Uiso 1 1 calc R . . C25A C 0.1696(13) 0.0066(15) 0.2801(9) 0.095(6) Uiso 0.536(9) 1 d P . . F25A F 0.2449(3) 0.0160(4) 0.3217(2) 0.123(2) Uani 0.536(9) 1 d P . . F25B F 0.1640(6) -0.0506(6) 0.2397(4) 0.099(4) Uiso 0.536(9) 1 d P . . F25C F 0.1225(5) -0.0366(5) 0.3031(3) 0.071(3) Uiso 0.536(9) 1 d P . . C25X C 0.2065(11) 0.0130(11) 0.2776(8) 0.063(4) Uiso 0.464(9) 1 d P . . F25X F 0.2449(3) 0.0160(4) 0.3217(2) 0.123(2) Uani 0.464(9) 1 d P . . F25Y F 0.2306(5) -0.0118(6) 0.2406(4) 0.079(3) Uiso 0.464(9) 1 d P . . F25Z F 0.1591(6) -0.0441(7) 0.2840(4) 0.072(3) Uiso 0.464(9) 1 d P . . C25D C 0.1934(4) 0.3167(5) 0.2571(3) 0.063(2) Uani 1 1 d . . . F25D F 0.1520(2) 0.3821(3) 0.25432(18) 0.0822(14) Uani 1 1 d . . . F25E F 0.2470(3) 0.3181(4) 0.30628(17) 0.1010(18) Uani 1 1 d . . . F25F F 0.2235(2) 0.3253(3) 0.21955(16) 0.0658(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.02136(8) 0.02644(9) 0.03166(9) -0.00401(8) 0.01317(7) 0.00344(8) P1 0.0213(5) 0.0394(7) 0.0278(5) -0.0057(5) 0.0085(5) 0.0074(5) C11A 0.022(2) 0.055(3) 0.026(2) -0.010(2) 0.005(2) -0.010(2) C12A 0.042(3) 0.043(3) 0.071(4) -0.008(3) 0.030(3) -0.014(3) C13A 0.064(4) 0.051(4) 0.068(4) 0.002(3) 0.028(4) -0.018(3) C14A 0.058(4) 0.108(6) 0.028(3) -0.005(3) 0.013(3) -0.049(4) C15A 0.037(3) 0.135(7) 0.027(3) 0.007(4) 0.016(3) -0.004(4) C16A 0.026(3) 0.112(6) 0.027(3) 0.001(3) 0.009(2) 0.012(3) C11B 0.026(3) 0.052(3) 0.038(3) -0.013(2) 0.008(2) 0.015(2) C12B 0.028(3) 0.050(3) 0.050(3) -0.013(3) 0.014(2) 0.009(2) C13B 0.040(3) 0.050(3) 0.065(4) -0.023(3) 0.019(3) 0.006(3) C14B 0.051(4) 0.056(4) 0.056(3) -0.018(3) 0.008(3) 0.031(3) C15B 0.042(4) 0.083(5) 0.082(5) -0.041(4) -0.013(3) 0.037(4) C16B 0.033(3) 0.069(4) 0.061(4) -0.032(3) -0.006(3) 0.023(3) C11C 0.028(3) 0.049(3) 0.031(3) -0.012(2) 0.003(2) 0.016(2) C12C 0.044(4) 0.103(6) 0.037(3) -0.024(3) 0.015(3) -0.037(4) C13C 0.054(4) 0.146(8) 0.043(4) -0.047(5) 0.018(3) -0.043(5) C14C 0.052(4) 0.120(7) 0.030(3) -0.023(4) -0.008(3) 0.047(4) C15C 0.177(10) 0.070(6) 0.027(3) -0.001(3) 0.005(4) 0.066(6) C16C 0.165(9) 0.041(4) 0.032(3) 0.000(3) 0.012(4) 0.030(5) N21 0.0239(18) 0.0094(15) 0.046(2) -0.0023(16) 0.0170(17) 0.0045(14) C211 0.021(2) 0.018(2) 0.030(2) -0.0021(16) 0.0171(18) -0.0003(16) C212 0.030(2) 0.027(2) 0.019(2) 0.0016(17) 0.0053(19) -0.0031(19) C213 0.054(3) 0.022(3) 0.033(3) 0.0066(19) 0.002(2) -0.012(2) C214 0.046(3) 0.023(3) 0.035(3) 0.0064(19) 0.008(2) 0.001(2) C215 0.022(2) 0.026(2) 0.029(2) -0.0043(18) 0.0092(19) 0.0024(17) C216 0.017(2) 0.018(2) 0.043(3) -0.0070(18) 0.014(2) -0.0016(16) F21A 0.150(4) 0.0215(18) 0.067(3) 0.0006(17) 0.018(3) -0.015(2) F21X 0.150(4) 0.0215(18) 0.067(3) 0.0006(17) 0.018(3) -0.015(2) C21D 0.024(3) 0.047(3) 0.058(3) -0.008(3) 0.013(3) 0.005(2) F21D 0.0378(19) 0.054(2) 0.067(2) -0.0217(18) -0.0093(17) 0.0021(16) F21E 0.044(2) 0.064(3) 0.088(3) 0.028(2) -0.015(2) 0.0042(19) F21F 0.0300(19) 0.132(4) 0.097(3) -0.030(3) 0.026(2) 0.005(2) C22 0.034(3) 0.015(2) 0.056(3) -0.005(2) 0.020(2) -0.0018(19) C221 0.038(3) 0.017(3) 0.086(5) -0.013(3) 0.017(3) 0.004(2) F22A 0.052(2) 0.0160(16) 0.119(3) -0.0159(17) 0.026(2) -0.0035(14) F22B 0.049(2) 0.0241(16) 0.090(3) -0.0039(16) 0.013(2) 0.0157(15) F22C 0.056(2) 0.0342(18) 0.080(2) -0.0220(17) 0.034(2) 0.0034(15) C23 0.038(3) 0.022(3) 0.079(4) 0.001(3) 0.030(3) -0.008(2) C24 0.038(3) 0.029(3) 0.078(4) 0.007(3) 0.041(3) -0.005(2) C241 0.043(3) 0.045(4) 0.118(6) -0.021(4) 0.053(4) -0.018(3) F24A 0.0328(19) 0.101(4) 0.106(3) -0.040(3) 0.035(2) -0.018(2) F24B 0.043(2) 0.084(3) 0.116(3) -0.031(3) 0.037(2) 0.005(2) F24C 0.080(3) 0.079(3) 0.210(6) 0.002(3) 0.094(4) -0.038(3) N25 0.049(3) 0.035(2) 0.068(3) 0.009(2) 0.043(3) 0.001(2) C251 0.059(4) 0.044(3) 0.045(3) 0.010(3) 0.039(3) 0.005(3) C252 0.115(7) 0.045(4) 0.056(4) 0.026(3) 0.051(4) 0.010(4) C253 0.129(8) 0.083(6) 0.039(4) 0.040(4) 0.027(5) 0.057(6) C254 0.089(6) 0.083(6) 0.032(3) 0.007(4) 0.001(4) 0.041(5) C255 0.053(4) 0.066(4) 0.024(2) -0.006(3) 0.009(3) 0.019(3) C256 0.044(3) 0.043(3) 0.028(2) 0.006(2) 0.019(2) 0.016(2) F25A 0.133(5) 0.146(5) 0.090(4) 0.079(3) 0.043(3) 0.080(4) F25X 0.133(5) 0.146(5) 0.090(4) 0.079(3) 0.043(3) 0.080(4) C25D 0.046(4) 0.074(5) 0.045(4) -0.024(3) -0.009(3) 0.024(3) F25D 0.055(2) 0.071(3) 0.097(3) -0.050(2) 0.001(2) 0.016(2) F25E 0.072(3) 0.139(5) 0.054(3) -0.039(3) -0.020(2) 0.010(3) F25F 0.054(2) 0.068(3) 0.069(2) -0.029(2) 0.016(2) -0.010(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N21 2.075(4) . ? Au1 P1 2.2360(12) . ? P1 C11A 1.808(6) . ? P1 C11B 1.816(5) . ? P1 C11C 1.825(5) . ? C11A C12A 1.382(8) . ? C11A C16A 1.388(7) . ? C12A C13A 1.384(8) . ? C12A H12A 0.9300 . ? C13A C14A 1.373(10) . ? C13A H13A 0.9300 . ? C14A C15A 1.367(11) . ? C14A H14A 0.9300 . ? C15A C16A 1.396(9) . ? C15A H15A 0.9300 . ? C16A H16A 0.9300 . ? C11B C12B 1.379(8) . ? C11B C16B 1.388(7) . ? C12B C13B 1.359(8) . ? C12B H12B 0.9300 . ? C13B C14B 1.399(8) . ? C13B H13B 0.9300 . ? C14B C15B 1.379(9) . ? C14B H14B 0.9300 . ? C15B C16B 1.396(8) . ? C15B H15B 0.9300 . ? C16B H16B 0.9300 . ? C11C C12C 1.369(9) . ? C11C C16C 1.381(9) . ? C12C C13C 1.398(8) . ? C12C H12C 0.9300 . ? C13C C14C 1.358(11) . ? C13C H13C 0.9300 . ? C14C C15C 1.358(12) . ? C14C H14C 0.9300 . ? C15C C16C 1.397(9) . ? C15C H15C 0.9300 . ? C16C H16C 0.9300 . ? N21 C22 1.368(6) . ? N21 C211 1.413(5) . ? C211 C216 1.400(6) . ? C211 C212 1.402(6) . ? C212 C213 1.383(7) . ? C212 H212 0.9300 . ? C213 C214 1.378(7) . ? C213 C21X 1.531(19) . ? C213 C21A 1.537(11) . ? C214 C215 1.376(6) . ? C214 H214 0.9300 . ? C215 C216 1.367(6) . ? C215 C21D 1.503(7) . ? C216 H216 0.9300 . ? C21A C21X 0.593(19) . ? C21A F21A 1.170(10) . ? C21A F21C 1.306(10) . ? C21A F21B 1.388(12) . ? C21A F21Z 1.57(2) . ? F21A C21X 1.54(2) . ? F21B C21X 0.878(19) . ? F21B F21Y 0.972(12) . ? F21B F21Z 1.112(17) . ? F21C F21Z 1.546(17) . ? F21C C21X 1.625(19) . ? C21X F21Z 1.25(2) . ? C21X F21Y 1.50(2) . ? C21D F21D 1.320(6) . ? C21D F21F 1.322(6) . ? C21D F21E 1.335(7) . ? C22 C23 1.342(7) . ? C22 C221 1.525(7) . ? C221 F22C 1.328(7) . ? C221 F22A 1.335(6) . ? C221 F22B 1.343(7) . ? C23 C24 1.467(7) . ? C23 H23 0.9300 . ? C24 N25 1.263(7) . ? C24 C241 1.512(8) . ? C241 F24A 1.315(9) . ? C241 F24B 1.315(7) . ? C241 F24C 1.345(7) . ? N25 C251 1.421(8) . ? C251 C256 1.387(8) . ? C251 C252 1.416(8) . ? C252 C253 1.376(12) . ? C252 H252 0.9300 . ? C253 C254 1.357(13) . ? C253 C25A 1.47(2) . ? C253 C25X 1.67(2) . ? C254 C255 1.381(9) . ? C254 H254 0.9300 . ? C255 C256 1.378(8) . ? C255 C25D 1.523(10) . ? C256 H256 0.9300 . ? C25A C25X 0.76(2) . ? C25A F25Z 0.85(2) . ? C25A F25B 1.37(2) . ? C25A F25C 1.46(2) . ? C25A F25A 1.48(2) . ? C25A F25Y 1.87(2) . ? F25A C25X 1.114(17) . ? F25B F25Z 1.195(12) . ? F25B F25Y 1.446(13) . ? F25B C25X 1.45(2) . ? F25C F25Z 1.025(11) . ? C25X F25Y 1.284(19) . ? C25X F25Z 1.36(2) . ? C25D F25D 1.314(7) . ? C25D F25E 1.321(6) . ? C25D F25F 1.325(8) . ? 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 N21 Au1 P1 175.59(11) . . ? C11A P1 C11B 107.9(3) . . ? C11A P1 C11C 106.6(3) . . ? C11B P1 C11C 104.9(2) . . ? C11A P1 Au1 109.69(17) . . ? C11B P1 Au1 112.76(19) . . ? C11C P1 Au1 114.56(17) . . ? C12A C11A C16A 119.1(6) . . ? C12A C11A P1 119.5(4) . . ? C16A C11A P1 121.4(5) . . ? C11A C12A C13A 121.2(6) . . ? C11A C12A H12A 119.4 . . ? C13A C12A H12A 119.4 . . ? C14A C13A C12A 119.5(7) . . ? C14A C13A H13A 120.3 . . ? C12A C13A H13A 120.3 . . ? C15A C14A C13A 120.1(6) . . ? C15A C14A H14A 119.9 . . ? C13A C14A H14A 119.9 . . ? C14A C15A C16A 120.9(6) . . ? C14A C15A H15A 119.5 . . ? C16A C15A H15A 119.5 . . ? C11A C16A C15A 119.2(7) . . ? C11A C16A H16A 120.4 . . ? C15A C16A H16A 120.4 . . ? C12B C11B C16B 119.9(5) . . ? C12B C11B P1 119.5(4) . . ? C16B C11B P1 120.6(4) . . ? C13B C12B C11B 120.5(5) . . ? C13B C12B H12B 119.7 . . ? C11B C12B H12B 119.7 . . ? C12B C13B C14B 120.5(6) . . ? C12B C13B H13B 119.7 . . ? C14B C13B H13B 119.7 . . ? C15B C14B C13B 119.4(5) . . ? C15B C14B H14B 120.3 . . ? C13B C14B H14B 120.3 . . ? C14B C15B C16B 120.0(6) . . ? C14B C15B H15B 120.0 . . ? C16B C15B H15B 120.0 . . ? C11B C16B C15B 119.6(6) . . ? C11B C16B H16B 120.2 . . ? C15B C16B H16B 120.2 . . ? C12C C11C C16C 119.2(5) . . ? C12C C11C P1 122.9(5) . . ? C16C C11C P1 117.8(5) . . ? C11C C12C C13C 120.4(7) . . ? C11C C12C H12C 119.8 . . ? C13C C12C H12C 119.8 . . ? C14C C13C C12C 119.8(8) . . ? C14C C13C H13C 120.1 . . ? C12C C13C H13C 120.1 . . ? C13C C14C C15C 120.7(6) . . ? C13C C14C H14C 119.6 . . ? C15C C14C H14C 119.6 . . ? C14C C15C C16C 120.0(8) . . ? C14C C15C H15C 120.0 . . ? C16C C15C H15C 120.0 . . ? C11C C16C C15C 119.9(8) . . ? C11C C16C H16C 120.1 . . ? C15C C16C H16C 120.1 . . ? C22 N21 C211 119.9(4) . . ? C22 N21 Au1 123.6(3) . . ? C211 N21 Au1 116.2(3) . . ? C216 C211 C212 116.8(4) . . ? C216 C211 N21 123.4(4) . . ? C212 C211 N21 119.7(4) . . ? C213 C212 C211 120.3(4) . . ? C213 C212 H212 119.9 . . ? C211 C212 H212 119.9 . . ? C214 C213 C212 122.0(4) . . ? C214 C213 C21X 121.8(8) . . ? C212 C213 C21X 114.0(8) . . ? C214 C213 C21A 116.5(5) . . ? C212 C213 C21A 121.2(5) . . ? C21X C213 C21A 22.3(7) . . ? C215 C214 C213 117.8(4) . . ? C215 C214 H214 121.1 . . ? C213 C214 H214 121.1 . . ? C216 C215 C214 121.4(4) . . ? C216 C215 C21D 119.5(4) . . ? C214 C215 C21D 119.1(4) . . ? C215 C216 C211 121.8(4) . . ? C215 C216 H216 119.1 . . ? C211 C216 H216 119.1 . . ? C21X C21A F21A 118(2) . . ? C21X C21A F21C 112(2) . . ? F21A C21A F21C 111.7(9) . . ? C21X C21A F21B 24(2) . . ? F21A C21A F21B 102.9(8) . . ? F21C C21A F21B 104.9(7) . . ? C21X C21A C213 78(2) . . ? F21A C21A C213 120.3(8) . . ? F21C C21A C213 112.9(7) . . ? F21B C21A C213 101.9(8) . . ? C21X C21A F21Z 48(2) . . ? F21A C21A F21Z 131.9(11) . . ? F21C C21A F21Z 64.4(7) . . ? F21B C21A F21Z 43.7(7) . . ? C213 C21A F21Z 102.6(9) . . ? C21A F21A C21X 20.0(8) . . ? C21X F21B F21Y 108.6(16) . . ? C21X F21B F21Z 77.1(15) . . ? F21Y F21B F21Z 159.3(14) . . ? C21X F21B C21A 15.7(14) . . ? F21Y F21B C21A 114.3(11) . . ? F21Z F21B C21A 76.8(11) . . ? C21A F21C F21Z 66.1(8) . . ? C21A F21C C21X 19.7(7) . . ? F21Z F21C C21X 46.5(9) . . ? C21A C21X F21B 141(3) . . ? C21A C21X F21Z 111(3) . . ? F21B C21X F21Z 59.8(14) . . ? C21A C21X F21Y 140(3) . . ? F21B C21X F21Y 37.8(10) . . ? F21Z C21X F21Y 95.6(17) . . ? C21A C21X C213 79(2) . . ? F21B C21X C213 140(2) . . ? F21Z C21X C213 120.6(15) . . ? F21Y C21X C213 112.5(12) . . ? C21A C21X F21A 42.3(19) . . ? F21B C21X F21A 109.1(16) . . ? F21Z C21X F21A 127.3(15) . . ? F21Y C21X F21A 98.0(11) . . ? C213 C21X F21A 100.2(12) . . ? C21A C21X F21C 48.1(19) . . ? F21B C21X F21C 113.9(16) . . ? F21Z C21X F21C 63.4(11) . . ? F21Y C21X F21C 149.7(15) . . ? C213 C21X F21C 97.4(11) . . ? F21A C21X F21C 80.7(10) . . ? F21B F21Y C21X 33.6(9) . . ? F21B F21Z C21X 43.0(11) . . ? F21B F21Z F21C 105.9(14) . . ? C21X F21Z F21C 70.1(13) . . ? F21B F21Z C21A 59.6(10) . . ? C21X F21Z C21A 20.7(10) . . ? F21C F21Z C21A 49.6(7) . . ? F21D C21D F21F 106.8(5) . . ? F21D C21D F21E 105.2(5) . . ? F21F C21D F21E 106.7(5) . . ? F21D C21D C215 113.8(4) . . ? F21F C21D C215 111.4(5) . . ? F21E C21D C215 112.4(5) . . ? C23 C22 N21 128.6(4) . . ? C23 C22 C221 117.4(5) . . ? N21 C22 C221 114.0(4) . . ? F22C C221 F22A 107.5(5) . . ? F22C C221 F22B 107.5(5) . . ? F22A C221 F22B 106.0(5) . . ? F22C C221 C22 112.6(5) . . ? F22A C221 C22 112.1(5) . . ? F22B C221 C22 110.8(5) . . ? C22 C23 C24 126.3(5) . . ? C22 C23 H23 116.8 . . ? C24 C23 H23 116.8 . . ? N25 C24 C23 129.8(5) . . ? N25 C24 C241 115.5(5) . . ? C23 C24 C241 114.7(5) . . ? F24A C241 F24B 108.8(6) . . ? F24A C241 F24C 107.2(6) . . ? F24B C241 F24C 105.1(5) . . ? F24A C241 C24 113.0(5) . . ? F24B C241 C24 113.7(5) . . ? F24C C241 C24 108.6(6) . . ? C24 N25 C251 122.1(5) . . ? C256 C251 C252 117.2(6) . . ? C256 C251 N25 119.6(5) . . ? C252 C251 N25 123.0(6) . . ? C253 C252 C251 120.0(7) . . ? C253 C252 H252 120.0 . . ? C251 C252 H252 120.0 . . ? C254 C253 C252 121.9(6) . . ? C254 C253 C25A 127.9(12) . . ? C252 C253 C25A 110.1(12) . . ? C254 C253 C25X 106.5(10) . . ? C252 C253 C25X 129.5(10) . . ? C25A C253 C25X 27.1(9) . . ? C253 C254 C255 118.8(7) . . ? C253 C254 H254 120.6 . . ? C255 C254 H254 120.6 . . ? C256 C255 C254 120.7(7) . . ? C256 C255 C25D 119.8(5) . . ? C254 C255 C25D 119.3(6) . . ? C255 C256 C251 121.2(5) . . ? C255 C256 H256 119.4 . . ? C251 C256 H256 119.4 . . ? C25X C25A F25Z 115(4) . . ? C25X C25A F25B 80(3) . . ? F25Z C25A F25B 60.0(16) . . ? C25X C25A F25C 151(3) . . ? F25Z C25A F25C 43.7(15) . . ? F25B C25A F25C 96.6(16) . . ? C25X C25A C253 91(3) . . ? F25Z C25A C253 149(3) . . ? F25B C25A C253 112.2(16) . . ? F25C C25A C253 116.3(16) . . ? C25X C25A F25A 47(2) . . ? F25Z C25A F25A 103(2) . . ? F25B C25A F25A 113.6(16) . . ? F25C C25A F25A 111.6(15) . . ? C253 C25A F25A 106.6(16) . . ? C25X C25A F25Y 31(2) . . ? F25Z C25A F25Y 99(2) . . ? F25B C25A F25Y 50.1(9) . . ? F25C C25A F25Y 142.1(16) . . ? C253 C25A F25Y 95.5(13) . . ? F25A C25A F25Y 75.0(11) . . ? C25X F25A C25A 30.0(12) . . ? F25Z F25B C25A 38.2(10) . . ? F25Z F25B F25Y 110.2(10) . . ? C25A F25B F25Y 83.5(12) . . ? F25Z F25B C25X 61.1(11) . . ? C25A F25B C25X 31.2(10) . . ? F25Y F25B C25X 52.7(9) . . ? F25Z F25C C25A 35.1(10) . . ? C25A C25X F25A 103(3) . . ? C25A C25X F25Y 131(3) . . ? F25A C25X F25Y 118.9(18) . . ? C25A C25X F25Z 35(2) . . ? F25A C25X F25Z 98.0(14) . . ? F25Y C25X F25Z 110.3(14) . . ? C25A C25X F25B 68(2) . . ? F25A C25X F25B 136.9(16) . . ? F25Y C25X F25B 63.6(10) . . ? F25Z C25X F25B 50.3(8) . . ? C25A C25X C253 62(3) . . ? F25A C25X C253 115.4(14) . . ? F25Y C25X C253 114.4(14) . . ? F25Z C25X C253 95.2(13) . . ? F25B C25X C253 98.0(12) . . ? C25X F25Y F25B 63.7(10) . . ? C25X F25Y C25A 17.9(11) . . ? F25B F25Y C25A 46.5(8) . . ? C25A F25Z F25C 101(2) . . ? C25A F25Z F25B 81.8(18) . . ? F25C F25Z F25B 143.2(12) . . ? C25A F25Z C25X 30.5(17) . . ? F25C F25Z C25X 128.5(14) . . ? F25B F25Z C25X 68.6(10) . . ? F25D C25D F25E 107.2(5) . . ? F25D C25D F25F 108.5(6) . . ? F25E C25D F25F 107.1(6) . . ? F25D C25D C255 111.4(6) . . ? F25E C25D C255 112.5(6) . . ? F25F C25D C255 110.0(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N21 Au1 P1 C11A 19.6(13) . . . . ? N21 Au1 P1 C11B -100.7(13) . . . . ? N21 Au1 P1 C11C 139.4(13) . . . . ? C11B P1 C11A C12A 164.3(4) . . . . ? C11C P1 C11A C12A -83.5(5) . . . . ? Au1 P1 C11A C12A 41.1(5) . . . . ? C11B P1 C11A C16A -14.9(5) . . . . ? C11C P1 C11A C16A 97.3(5) . . . . ? Au1 P1 C11A C16A -138.1(4) . . . . ? C16A C11A C12A C13A -0.4(9) . . . . ? P1 C11A C12A C13A -179.6(5) . . . . ? C11A C12A C13A C14A -0.4(10) . . . . ? C12A C13A C14A C15A 1.6(10) . . . . ? C13A C14A C15A C16A -1.9(10) . . . . ? C12A C11A C16A C15A 0.0(8) . . . . ? P1 C11A C16A C15A 179.2(4) . . . . ? C14A C15A C16A C11A 1.1(9) . . . . ? C11A P1 C11B C12B -100.3(5) . . . . ? C11C P1 C11B C12B 146.4(5) . . . . ? Au1 P1 C11B C12B 21.1(6) . . . . ? C11A P1 C11B C16B 81.0(6) . . . . ? C11C P1 C11B C16B -32.4(6) . . . . ? Au1 P1 C11B C16B -157.7(5) . . . . ? C16B C11B C12B C13B -1.0(10) . . . . ? P1 C11B C12B C13B -179.7(5) . . . . ? C11B C12B C13B C14B 1.8(10) . . . . ? C12B C13B C14B C15B -1.6(11) . . . . ? C13B C14B C15B C16B 0.7(12) . . . . ? C12B C11B C16B C15B 0.0(11) . . . . ? P1 C11B C16B C15B 178.7(6) . . . . ? C14B C15B C16B C11B 0.1(13) . . . . ? C11A P1 C11C C12C 11.8(6) . . . . ? C11B P1 C11C C12C 126.2(5) . . . . ? Au1 P1 C11C C12C -109.7(5) . . . . ? C11A P1 C11C C16C -171.7(5) . . . . ? C11B P1 C11C C16C -57.4(6) . . . . ? Au1 P1 C11C C16C 66.7(6) . . . . ? C16C C11C C12C C13C 0.6(10) . . . . ? P1 C11C C12C C13C 176.9(5) . . . . ? C11C C12C C13C C14C -0.6(11) . . . . ? C12C C13C C14C C15C 0.5(12) . . . . ? C13C C14C C15C C16C -0.4(13) . . . . ? C12C C11C C16C C15C -0.5(12) . . . . ? P1 C11C C16C C15C -177.0(7) . . . . ? C14C C15C C16C C11C 0.4(14) . . . . ? P1 Au1 N21 C22 123.6(12) . . . . ? P1 Au1 N21 C211 -50.6(14) . . . . ? C22 N21 C211 C216 -25.4(6) . . . . ? Au1 N21 C211 C216 148.9(3) . . . . ? C22 N21 C211 C212 158.9(4) . . . . ? Au1 N21 C211 C212 -26.7(5) . . . . ? C216 C211 C212 C213 0.5(6) . . . . ? N21 C211 C212 C213 176.5(4) . . . . ? C211 C212 C213 C214 -1.3(8) . . . . ? C211 C212 C213 C21X -164.4(9) . . . . ? C211 C212 C213 C21A 171.8(6) . . . . ? C212 C213 C214 C215 1.3(9) . . . . ? C21X C213 C214 C215 163.0(10) . . . . ? C21A C213 C214 C215 -172.1(6) . . . . ? C213 C214 C215 C216 -0.5(8) . . . . ? C213 C214 C215 C21D 176.9(5) . . . . ? C214 C215 C216 C211 -0.3(7) . . . . ? C21D C215 C216 C211 -177.6(4) . . . . ? C212 C211 C216 C215 0.3(6) . . . . ? N21 C211 C216 C215 -175.5(4) . . . . ? C214 C213 C21A C21X -110(2) . . . . ? C212 C213 C21A C21X 77(2) . . . . ? C214 C213 C21A F21A 5.8(13) . . . . ? C212 C213 C21A F21A -167.7(8) . . . . ? C21X C213 C21A F21A 115(3) . . . . ? C214 C213 C21A F21C 141.0(7) . . . . ? C212 C213 C21A F21C -32.4(11) . . . . ? C21X C213 C21A F21C -109(2) . . . . ? C214 C213 C21A F21B -107.0(7) . . . . ? C212 C213 C21A F21B 79.6(8) . . . . ? C21X C213 C21A F21B 3(2) . . . . ? C214 C213 C21A F21Z -151.7(8) . . . . ? C212 C213 C21A F21Z 34.8(11) . . . . ? C21X C213 C21A F21Z -42(2) . . . . ? F21C C21A F21A C21X 132(3) . . . . ? F21B C21A F21A C21X 20(2) . . . . ? C213 C21A F21A C21X -92(3) . . . . ? F21Z C21A F21A C21X 57(3) . . . . ? F21A C21A F21B C21X -132(5) . . . . ? F21C C21A F21B C21X 111(5) . . . . ? C213 C21A F21B C21X -6(5) . . . . ? F21Z C21A F21B C21X 90(5) . . . . ? C21X C21A F21B F21Y 72(5) . . . . ? F21A C21A F21B F21Y -59.7(13) . . . . ? F21C C21A F21B F21Y -176.7(11) . . . . ? C213 C21A F21B F21Y 65.5(12) . . . . ? F21Z C21A F21B F21Y 161.5(16) . . . . ? C21X C21A F21B F21Z -90(5) . . . . ? F21A C21A F21B F21Z 138.8(12) . . . . ? F21C C21A F21B F21Z 21.9(12) . . . . ? C213 C21A F21B F21Z -95.9(11) . . . . ? C21X C21A F21C F21Z 7(3) . . . . ? F21A C21A F21C F21Z -127.4(12) . . . . ? F21B C21A F21C F21Z -16.6(9) . . . . ? C213 C21A F21C F21Z 93.5(10) . . . . ? F21A C21A F21C C21X -135(3) . . . . ? F21B C21A F21C C21X -24(2) . . . . ? C213 C21A F21C C21X 86(3) . . . . ? F21Z C21A F21C C21X -7(3) . . . . ? F21A C21A C21X F21B 55(6) . . . . ? F21C C21A C21X F21B -76(5) . . . . ? C213 C21A C21X F21B 174(5) . . . . ? F21Z C21A C21X F21B -68(4) . . . . ? F21A C21A C21X F21Z 122.9(19) . . . . ? F21C C21A C21X F21Z -9(3) . . . . ? F21B C21A C21X F21Z 68(4) . . . . ? C213 C21A C21X F21Z -119(2) . . . . ? F21A C21A C21X F21Y -6(5) . . . . ? F21C C21A C21X F21Y -137(3) . . . . ? F21B C21A C21X F21Y -61(4) . . . . ? C213 C21A C21X F21Y 113(4) . . . . ? F21Z C21A C21X F21Y -129(5) . . . . ? F21A C21A C21X C213 -118.3(16) . . . . ? F21C C21A C21X C213 110.1(14) . . . . ? F21B C21A C21X C213 -174(5) . . . . ? F21Z C21A C21X C213 119(2) . . . . ? F21C C21A C21X F21A -132(3) . . . . ? F21B C21A C21X F21A -55(6) . . . . ? C213 C21A C21X F21A 118.3(16) . . . . ? F21Z C21A C21X F21A -122.9(19) . . . . ? F21A C21A C21X F21C 132(3) . . . . ? F21B C21A C21X F21C 76(5) . . . . ? C213 C21A C21X F21C -110.1(14) . . . . ? F21Z C21A C21X F21C 9(3) . . . . ? F21Y F21B C21X C21A -114(5) . . . . ? F21Z F21B C21X C21A 87(5) . . . . ? F21Y F21B C21X F21Z 159.3(15) . . . . ? C21A F21B C21X F21Z -87(5) . . . . ? F21Z F21B C21X F21Y -159.3(15) . . . . ? C21A F21B C21X F21Y 114(5) . . . . ? F21Y F21B C21X C213 56(3) . . . . ? F21Z F21B C21X C213 -103(3) . . . . ? C21A F21B C21X C213 170(7) . . . . ? F21Y F21B C21X F21A -78.0(17) . . . . ? F21Z F21B C21X F21A 122.7(16) . . . . ? C21A F21B C21X F21A 36(4) . . . . ? F21Y F21B C21X F21C -166.1(12) . . . . ? F21Z F21B C21X F21C 34.6(15) . . . . ? C21A F21B C21X F21C -52(4) . . . . ? C214 C213 C21X C21A 83(2) . . . . ? C212 C213 C21X C21A -114(2) . . . . ? C214 C213 C21X F21B -91(3) . . . . ? C212 C213 C21X F21B 72(3) . . . . ? C21A C213 C21X F21B -174(5) . . . . ? C214 C213 C21X F21Z -169.2(15) . . . . ? C212 C213 C21X F21Z -6(2) . . . . ? C21A C213 C21X F21Z 108(3) . . . . ? C214 C213 C21X F21Y -57.5(17) . . . . ? C212 C213 C21X F21Y 105.5(12) . . . . ? C21A C213 C21X F21Y -140(3) . . . . ? C214 C213 C21X F21A 45.6(14) . . . . ? C212 C213 C21X F21A -151.3(7) . . . . ? C21A C213 C21X F21A -37.1(17) . . . . ? C214 C213 C21X F21C 127.4(8) . . . . ? C212 C213 C21X F21C -69.5(11) . . . . ? C21A C213 C21X F21C 44.8(18) . . . . ? C21A F21A C21X F21B -146(4) . . . . ? C21A F21A C21X F21Z -80(3) . . . . ? C21A F21A C21X F21Y 176(3) . . . . ? C21A F21A C21X C213 62(3) . . . . ? C21A F21A C21X F21C -34(2) . . . . ? F21Z F21C C21X C21A -171(3) . . . . ? C21A F21C C21X F21B 138(4) . . . . ? F21Z F21C C21X F21B -33.3(16) . . . . ? C21A F21C C21X F21Z 171(3) . . . . ? C21A F21C C21X F21Y 121(4) . . . . ? F21Z F21C C21X F21Y -50(3) . . . . ? C21A F21C C21X C213 -69(3) . . . . ? F21Z F21C C21X C213 120.6(15) . . . . ? C21A F21C C21X F21A 31(2) . . . . ? F21Z F21C C21X F21A -140.2(15) . . . . ? F21Z F21B F21Y C21X 103(5) . . . . ? C21A F21B F21Y C21X -15.8(14) . . . . ? C21A C21X F21Y F21B 115(5) . . . . ? F21Z C21X F21Y F21B -17.9(14) . . . . ? C213 C21X F21Y F21B -144(2) . . . . ? F21A C21X F21Y F21B 111.1(19) . . . . ? F21C C21X F21Y F21B 26(2) . . . . ? F21Y F21B F21Z C21X -109(4) . . . . ? C21A F21B F21Z C21X 16.2(14) . . . . ? C21X F21B F21Z F21C -34.6(16) . . . . ? F21Y F21B F21Z F21C -143(4) . . . . ? C21A F21B F21Z F21C -18.4(9) . . . . ? C21X F21B F21Z C21A -16.2(14) . . . . ? F21Y F21B F21Z C21A -125(4) . . . . ? C21A C21X F21Z F21B -137(4) . . . . ? F21Y C21X F21Z F21B 12.6(10) . . . . ? C213 C21X F21Z F21B 133(2) . . . . ? F21A C21X F21Z F21B -92(2) . . . . ? F21C C21X F21Z F21B -144.5(16) . . . . ? C21A C21X F21Z F21C 7(3) . . . . ? F21B C21X F21Z F21C 144.5(16) . . . . ? F21Y C21X F21Z F21C 157.0(12) . . . . ? C213 C21X F21Z F21C -82.6(16) . . . . ? F21A C21X F21Z F21C 52.6(18) . . . . ? F21B C21X F21Z C21A 137(4) . . . . ? F21Y C21X F21Z C21A 150(3) . . . . ? C213 C21X F21Z C21A -90(3) . . . . ? F21A C21X F21Z C21A 45(2) . . . . ? F21C C21X F21Z C21A -7(3) . . . . ? C21A F21C F21Z F21B 21.0(11) . . . . ? C21X F21C F21Z F21B 24.3(11) . . . . ? C21A F21C F21Z C21X -3.4(12) . . . . ? C21X F21C F21Z C21A 3.4(12) . . . . ? C21X C21A F21Z F21B 33(3) . . . . ? F21A C21A F21Z F21B -59.6(15) . . . . ? F21C C21A F21Z F21B -156.5(12) . . . . ? C213 C21A F21Z F21B 94.1(10) . . . . ? F21A C21A F21Z C21X -92(3) . . . . ? F21C C21A F21Z C21X 171(3) . . . . ? F21B C21A F21Z C21X -33(3) . . . . ? C213 C21A F21Z C21X 62(3) . . . . ? C21X C21A F21Z F21C -171(3) . . . . ? F21A C21A F21Z F21C 96.8(14) . . . . ? F21B C21A F21Z F21C 156.5(12) . . . . ? C213 C21A F21Z F21C -109.5(8) . . . . ? C216 C215 C21D F21D -31.4(7) . . . . ? C214 C215 C21D F21D 151.3(5) . . . . ? C216 C215 C21D F21F 89.4(6) . . . . ? C214 C215 C21D F21F -87.9(6) . . . . ? C216 C215 C21D F21E -150.9(5) . . . . ? C214 C215 C21D F21E 31.7(7) . . . . ? C211 N21 C22 C23 -40.2(8) . . . . ? Au1 N21 C22 C23 145.9(5) . . . . ? C211 N21 C22 C221 140.8(5) . . . . ? Au1 N21 C22 C221 -33.1(6) . . . . ? C23 C22 C221 F22C 132.5(6) . . . . ? N21 C22 C221 F22C -48.4(6) . . . . ? C23 C22 C221 F22A 11.1(8) . . . . ? N21 C22 C221 F22A -169.8(5) . . . . ? C23 C22 C221 F22B -107.1(6) . . . . ? N21 C22 C221 F22B 72.0(7) . . . . ? N21 C22 C23 C24 -9.2(10) . . . . ? C221 C22 C23 C24 169.7(6) . . . . ? C22 C23 C24 N25 -44.0(10) . . . . ? C22 C23 C24 C241 138.5(6) . . . . ? N25 C24 C241 F24A 135.1(6) . . . . ? C23 C24 C241 F24A -47.0(7) . . . . ? N25 C24 C241 F24B 10.5(8) . . . . ? C23 C24 C241 F24B -171.6(6) . . . . ? N25 C24 C241 F24C -106.1(6) . . . . ? C23 C24 C241 F24C 71.8(7) . . . . ? C23 C24 N25 C251 -5.6(9) . . . . ? C241 C24 N25 C251 171.9(5) . . . . ? C24 N25 C251 C256 136.5(5) . . . . ? C24 N25 C251 C252 -47.5(7) . . . . ? C256 C251 C252 C253 -2.1(8) . . . . ? N25 C251 C252 C253 -178.2(6) . . . . ? C251 C252 C253 C254 0.0(11) . . . . ? C251 C252 C253 C25A 176.6(10) . . . . ? C251 C252 C253 C25X -161.2(10) . . . . ? C252 C253 C254 C255 1.6(12) . . . . ? C25A C253 C254 C255 -174.5(13) . . . . ? C25X C253 C254 C255 166.5(9) . . . . ? C253 C254 C255 C256 -0.9(10) . . . . ? C253 C254 C255 C25D -175.7(7) . . . . ? C254 C255 C256 C251 -1.3(8) . . . . ? C25D C255 C256 C251 173.5(5) . . . . ? C252 C251 C256 C255 2.7(7) . . . . ? N25 C251 C256 C255 179.0(5) . . . . ? C254 C253 C25A C25X -43(3) . . . . ? C252 C253 C25A C25X 140(2) . . . . ? C254 C253 C25A F25Z 169(4) . . . . ? C252 C253 C25A F25Z -8(5) . . . . ? C25X C253 C25A F25Z -148(7) . . . . ? C254 C253 C25A F25B -123.2(15) . . . . ? C252 C253 C25A F25B 60.4(19) . . . . ? C25X C253 C25A F25B -80(3) . . . . ? C254 C253 C25A F25C 126.9(15) . . . . ? C252 C253 C25A F25C -49.5(17) . . . . ? C25X C253 C25A F25C 170(4) . . . . ? C254 C253 C25A F25A 2(2) . . . . ? C252 C253 C25A F25A -174.7(10) . . . . ? C25X C253 C25A F25A 45(2) . . . . ? C254 C253 C25A F25Y -74.3(14) . . . . ? C252 C253 C25A F25Y 109.3(10) . . . . ? C25X C253 C25A F25Y -31(2) . . . . ? F25Z C25A F25A C25X 112(4) . . . . ? F25B C25A F25A C25X 49(2) . . . . ? F25C C25A F25A C25X 157(4) . . . . ? C253 C25A F25A C25X -75(3) . . . . ? F25Y C25A F25A C25X 16(2) . . . . ? C25X C25A F25B F25Z 126(3) . . . . ? F25C C25A F25B F25Z -24.9(11) . . . . ? C253 C25A F25B F25Z -147(3) . . . . ? F25A C25A F25B F25Z 92(2) . . . . ? F25Y C25A F25B F25Z 135.1(18) . . . . ? C25X C25A F25B F25Y -9(2) . . . . ? F25Z C25A F25B F25Y -135.1(18) . . . . ? F25C C25A F25B F25Y -160.0(12) . . . . ? C253 C25A F25B F25Y 78.1(16) . . . . ? F25A C25A F25B F25Y -42.9(16) . . . . ? F25Z C25A F25B C25X -126(3) . . . . ? F25C C25A F25B C25X -151(3) . . . . ? C253 C25A F25B C25X 87(3) . . . . ? F25A C25A F25B C25X -33.9(18) . . . . ? F25Y C25A F25B C25X 9(2) . . . . ? C25X C25A F25C F25Z -50(6) . . . . ? F25B C25A F25C F25Z 31.8(13) . . . . ? C253 C25A F25C F25Z 151(3) . . . . ? F25A C25A F25C F25Z -87(2) . . . . ? F25Y C25A F25C F25Z 6.5(15) . . . . ? F25Z C25A C25X F25A -85(3) . . . . ? F25B C25A C25X F25A -135.6(16) . . . . ? F25C C25A C25X F25A -50(7) . . . . ? C253 C25A C25X F25A 112.0(16) . . . . ? F25Y C25A C25X F25A -149(5) . . . . ? F25Z C25A C25X F25Y 64(5) . . . . ? F25B C25A C25X F25Y 13(4) . . . . ? F25C C25A C25X F25Y 99(6) . . . . ? C253 C25A C25X F25Y -99(3) . . . . ? F25A C25A C25X F25Y 149(5) . . . . ? F25B C25A C25X F25Z -50(3) . . . . ? F25C C25A C25X F25Z 36(4) . . . . ? C253 C25A C25X F25Z -163(4) . . . . ? F25A C25A C25X F25Z 85(3) . . . . ? F25Y C25A C25X F25Z -64(5) . . . . ? F25Z C25A C25X F25B 50(3) . . . . ? F25C C25A C25X F25B 86(6) . . . . ? C253 C25A C25X F25B -112.4(14) . . . . ? F25A C25A C25X F25B 135.6(16) . . . . ? F25Y C25A C25X F25B -13(4) . . . . ? F25Z C25A C25X C253 163(4) . . . . ? F25B C25A C25X C253 112.4(14) . . . . ? F25C C25A C25X C253 -162(7) . . . . ? F25A C25A C25X C253 -112.0(16) . . . . ? F25Y C25A C25X C253 99(3) . . . . ? C25A F25A C25X F25Y -154(4) . . . . ? C25A F25A C25X F25Z -35(2) . . . . ? C25A F25A C25X F25B -72(3) . . . . ? C25A F25A C25X C253 65(3) . . . . ? F25Z F25B C25X C25A -35(2) . . . . ? F25Y F25B C25X C25A 169(3) . . . . ? F25Z F25B C25X F25A 51(2) . . . . ? C25A F25B C25X F25A 86(3) . . . . ? F25Y F25B C25X F25A -105(3) . . . . ? F25Z F25B C25X F25Y 156.5(14) . . . . ? C25A F25B C25X F25Y -169(3) . . . . ? C25A F25B C25X F25Z 35(2) . . . . ? F25Y F25B C25X F25Z -156.5(14) . . . . ? F25Z F25B C25X C253 -90.2(12) . . . . ? C25A F25B C25X C253 -55(2) . . . . ? F25Y F25B C25X C253 113.3(13) . . . . ? C254 C253 C25X C25A 146(2) . . . . ? C252 C253 C25X C25A -51(3) . . . . ? C254 C253 C25X F25A 54.0(17) . . . . ? C252 C253 C25X F25A -142.6(13) . . . . ? C25A C253 C25X F25A -92(3) . . . . ? C254 C253 C25X F25Y -89.5(14) . . . . ? C252 C253 C25X F25Y 73.9(18) . . . . ? C25A C253 C25X F25Y 125(3) . . . . ? C254 C253 C25X F25Z 155.4(9) . . . . ? C252 C253 C25X F25Z -41.2(15) . . . . ? C25A C253 C25X F25Z 10(2) . . . . ? C254 C253 C25X F25B -154.0(10) . . . . ? C252 C253 C25X F25B 9.3(17) . . . . ? C25A C253 C25X F25B 60(2) . . . . ? C25A C25X F25Y F25B -14(4) . . . . ? F25A C25X F25Y F25B 131.1(19) . . . . ? F25Z C25X F25Y F25B 19.1(11) . . . . ? C253 C25X F25Y F25B -86.9(14) . . . . ? F25A C25X F25Y C25A 145(5) . . . . ? F25Z C25X F25Y C25A 33(3) . . . . ? F25B C25X F25Y C25A 14(4) . . . . ? C253 C25X F25Y C25A -73(4) . . . . ? F25Z F25B F25Y C25X -21.8(13) . . . . ? C25A F25B F25Y C25X 5.9(16) . . . . ? F25Z F25B F25Y C25A -27.7(11) . . . . ? C25X F25B F25Y C25A -5.9(16) . . . . ? F25Z C25A F25Y C25X -125(5) . . . . ? F25B C25A F25Y C25X -163(5) . . . . ? F25C C25A F25Y C25X -129(5) . . . . ? C253 C25A F25Y C25X 83(4) . . . . ? F25A C25A F25Y C25X -23(4) . . . . ? C25X C25A F25Y F25B 163(5) . . . . ? F25Z C25A F25Y F25B 38.2(16) . . . . ? F25C C25A F25Y F25B 34(2) . . . . ? C253 C25A F25Y F25B -114.5(15) . . . . ? F25A C25A F25Y F25B 139.7(15) . . . . ? C25X C25A F25Z F25C 156(3) . . . . ? F25B C25A F25Z F25C -142.8(13) . . . . ? C253 C25A F25Z F25C -60(5) . . . . ? F25A C25A F25Z F25C 107.5(15) . . . . ? F25Y C25A F25Z F25C -176.0(9) . . . . ? C25X C25A F25Z F25B -61(3) . . . . ? F25C C25A F25Z F25B 142.8(13) . . . . ? C253 C25A F25Z F25B 83(5) . . . . ? F25A C25A F25Z F25B -109.7(15) . . . . ? F25Y C25A F25Z F25B -33.2(11) . . . . ? F25B C25A F25Z C25X 61(3) . . . . ? F25C C25A F25Z C25X -156(3) . . . . ? C253 C25A F25Z C25X 145(7) . . . . ? F25A C25A F25Z C25X -48(3) . . . . ? F25Y C25A F25Z C25X 28(3) . . . . ? C25A F25C F25Z F25B -91(3) . . . . ? C25A F25C F25Z C25X 15(2) . . . . ? F25Y F25B F25Z C25A 48(2) . . . . ? C25X F25B F25Z C25A 28.6(18) . . . . ? C25A F25B F25Z F25C 98(3) . . . . ? F25Y F25B F25Z F25C 146.1(19) . . . . ? C25X F25B F25Z F25C 126(3) . . . . ? C25A F25B F25Z C25X -28.6(18) . . . . ? F25Y F25B F25Z C25X 19.8(12) . . . . ? F25A C25X F25Z C25A 101(4) . . . . ? F25Y C25X F25Z C25A -134(4) . . . . ? F25B C25X F25Z C25A -111(4) . . . . ? C253 C25X F25Z C25A -15(3) . . . . ? C25A C25X F25Z F25C -31(4) . . . . ? F25A C25X F25Z F25C 71(2) . . . . ? F25Y C25X F25Z F25C -164.4(13) . . . . ? F25B C25X F25Z F25C -142.0(16) . . . . ? C253 C25X F25Z F25C -45.9(17) . . . . ? C25A C25X F25Z F25B 111(4) . . . . ? F25A C25X F25Z F25B -147.4(16) . . . . ? F25Y C25X F25Z F25B -22.4(13) . . . . ? C253 C25X F25Z F25B 96.1(11) . . . . ? C256 C255 C25D F25D 32.0(8) . . . . ? C254 C255 C25D F25D -153.2(6) . . . . ? C256 C255 C25D F25E 152.4(5) . . . . ? C254 C255 C25D F25E -32.8(8) . . . . ? C256 C255 C25D F25F -88.4(6) . . . . ? C254 C255 C25D F25F 86.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.922 _refine_diff_density_min -1.619 _refine_diff_density_rms 0.132