# Supplementary Material (ESI) for Chemical Science # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 _journal_year 2011 _journal_volume 2 _journal_page_first 2407 _publ_contact_author_name 'Carlos Peinador' _publ_contact_author_email carlos.peinador@udc.es loop_ _publ_author_name V.Blanco M.D.Garcia C.Peinador J.M.Quintela data_0830348_b1_0s _database_code_depnum_ccdc_archive 'CCDC 837131' #TrackingRef '- Catenano 3(9)2-6OTf-2PF6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H76 F15 N8 O22 P Pd S3' _chemical_formula_weight 1947.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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 12.518(5) _cell_length_b 18.378(5) _cell_length_c 20.119(5) _cell_angle_alpha 97.003(5) _cell_angle_beta 102.035(5) _cell_angle_gamma 107.893(5) _cell_volume 4221(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 14442 _cell_measurement_theta_min 4.333 _cell_measurement_theta_max 42.452 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1992 _exptl_absorpt_coefficient_mu 0.422 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8493 _exptl_absorpt_correction_T_max 0.9874 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 96651 _diffrn_reflns_av_R_equivalents 0.0717 _diffrn_reflns_av_sigmaI/netI 0.0899 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 28.41 _reflns_number_total 21129 _reflns_number_gt 11518 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.2000P)^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 21129 _refine_ls_number_parameters 1119 _refine_ls_number_restraints 119 _refine_ls_R_factor_all 0.1940 _refine_ls_R_factor_gt 0.1162 _refine_ls_wR_factor_ref 0.3874 _refine_ls_wR_factor_gt 0.3326 _refine_ls_goodness_of_fit_ref 1.299 _refine_ls_restrained_S_all 1.308 _refine_ls_shift/su_max 2.446 _refine_ls_shift/su_mean 0.045 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 0.6878(6) 0.7537(4) 0.7825(3) 0.0359(15) Uani 1 1 d . . . H1 H 0.6328 0.7762 0.7930 0.043 Uiso 1 1 calc R . . C2 C 0.6613(5) 0.6723(3) 0.7767(3) 0.0292(13) Uani 1 1 d . . . C3 C 0.7447(6) 0.6407(4) 0.7619(3) 0.0299(13) Uani 1 1 d . . . C4 C 0.8515(5) 0.6907(4) 0.7530(3) 0.0309(14) Uani 1 1 d . . . C5 C 0.8684(6) 0.7703(4) 0.7600(3) 0.0350(15) Uani 1 1 d . . . H5 H 0.9390 0.8048 0.7549 0.042 Uiso 1 1 calc R . . C6 C 0.9332(6) 0.6574(4) 0.7368(4) 0.0380(15) Uani 1 1 d . . . H6 H 1.0034 0.6904 0.7301 0.046 Uiso 1 1 calc R . . C7 C 0.9148(6) 0.5802(4) 0.7307(4) 0.0370(15) Uani 1 1 d . . . H7 H 0.9719 0.5598 0.7204 0.044 Uiso 1 1 calc R . . C8 C 0.8064(6) 0.5285(4) 0.7398(3) 0.0333(14) Uani 1 1 d . . . C9 C 0.7232(6) 0.5603(4) 0.7542(3) 0.0286(13) Uani 1 1 d . . . C10 C 0.5542(6) 0.6216(4) 0.7848(3) 0.0311(13) Uani 1 1 d . . . H10 H 0.4973 0.6427 0.7944 0.037 Uiso 1 1 calc R . . C11 C 0.5333(6) 0.5445(4) 0.7789(3) 0.0311(14) Uani 1 1 d . . . H11 H 0.4622 0.5117 0.7850 0.037 Uiso 1 1 calc R . . C12 C 0.6170(6) 0.5115(4) 0.7637(3) 0.0300(13) Uani 1 1 d . . . C13 C 0.5995(6) 0.4322(4) 0.7578(3) 0.0311(14) Uani 1 1 d . . . H13 H 0.5295 0.3981 0.7639 0.037 Uiso 1 1 calc R . . C14 C 0.7833(6) 0.4504(4) 0.7347(3) 0.0332(14) Uani 1 1 d . . . H14 H 0.8390 0.4283 0.7249 0.040 Uiso 1 1 calc R . . C15 C 0.6582(6) 0.3196(4) 0.7367(3) 0.0360(15) Uani 1 1 d . . . H15A H 0.6145 0.2996 0.7703 0.043 Uiso 1 1 calc R . . H15B H 0.7326 0.3095 0.7472 0.043 Uiso 1 1 calc R . . C16 C 0.4745(6) 0.2465(4) 0.6534(4) 0.0367(15) Uani 1 1 d . . . H16 H 0.4385 0.2482 0.6904 0.044 Uiso 1 1 calc R . . C17 C 0.4077(6) 0.2107(4) 0.5868(4) 0.0361(15) Uani 1 1 d . . . C18 C 0.4655(6) 0.2061(3) 0.5333(4) 0.0343(15) Uani 1 1 d . . . C19 C 0.5877(6) 0.2369(4) 0.5500(4) 0.0358(15) Uani 1 1 d . . . C20 C 0.6475(6) 0.2728(4) 0.6173(3) 0.0356(15) Uani 1 1 d . . . H20 H 0.7301 0.2933 0.6296 0.043 Uiso 1 1 calc R . . C21 C 0.6453(7) 0.2306(4) 0.4957(4) 0.0422(17) Uani 1 1 d . . . H21 H 0.7278 0.2495 0.5066 0.051 Uiso 1 1 calc R . . C22 C 0.5830(7) 0.1982(4) 0.4295(4) 0.0441(17) Uani 1 1 d . . . H22 H 0.6221 0.1938 0.3943 0.053 Uiso 1 1 calc R . . C23 C 0.4577(6) 0.1702(3) 0.4118(4) 0.0357(15) Uani 1 1 d . . . C24 C 0.3990(6) 0.1718(4) 0.4640(3) 0.0335(14) Uani 1 1 d . . . C25 C 0.2820(6) 0.1783(4) 0.5686(4) 0.0393(16) Uani 1 1 d . . . H25 H 0.2425 0.1787 0.6041 0.047 Uiso 1 1 calc R . . C26 C 0.2202(6) 0.1477(4) 0.5025(4) 0.0381(15) Uani 1 1 d . . . H26 H 0.1376 0.1287 0.4916 0.046 Uiso 1 1 calc R . . C27 C 0.2784(6) 0.1434(4) 0.4477(4) 0.0369(15) Uani 1 1 d . . . C28 C 0.7823(7) 0.8835(4) 0.6221(4) 0.0399(16) Uani 1 1 d . . . H28 H 0.8649 0.9020 0.6346 0.048 Uiso 1 1 calc R . . C29 C 0.6089(7) 0.8587(4) 0.6562(4) 0.0422(17) Uani 1 1 d . . . H29 H 0.5718 0.8611 0.6927 0.051 Uiso 1 1 calc R . . C30 C 0.9688(10) 1.0356(5) 0.8862(5) 0.074(3) Uani 1 1 d . . . H30A H 1.0391 1.0428 0.8689 0.089 Uiso 1 1 calc R . . H30B H 0.9936 1.0589 0.9363 0.089 Uiso 1 1 calc R . . C31 C 0.8927(11) 1.0742(5) 0.8477(5) 0.083(4) Uani 1 1 d . . . H31A H 0.8273 1.0726 0.8685 0.100 Uiso 1 1 calc R . . H31B H 0.9380 1.1294 0.8495 0.100 Uiso 1 1 calc R . . C32 C 0.5498(6) 0.6350(3) 0.6040(3) 0.0320(14) Uani 1 1 d . . . H32 H 0.5143 0.6722 0.6145 0.038 Uiso 1 1 calc R . . C33 C 0.6561(6) 0.6584(4) 0.5890(3) 0.0344(15) Uani 1 1 d . . . H33 H 0.6921 0.7118 0.5881 0.041 Uiso 1 1 calc R . . C34 C 0.7130(6) 0.6053(4) 0.5750(3) 0.0341(14) Uani 1 1 d . . . H34 H 0.7874 0.6228 0.5661 0.041 Uiso 1 1 calc R . . C35 C 0.6594(6) 0.5281(4) 0.5744(3) 0.0300(13) Uani 1 1 d . . . C36 C 0.5490(6) 0.5001(3) 0.5878(3) 0.0288(13) Uani 1 1 d . . . C36A C 0.4915(6) 0.4201(4) 0.5870(3) 0.0304(14) Uani 1 1 d . . . H36A H 0.5263 0.3826 0.5759 0.036 Uiso 1 1 calc R . . C37 C 0.3852(6) 0.3969(4) 0.6024(3) 0.0346(15) Uani 1 1 d . . . H37 H 0.3463 0.3433 0.6009 0.042 Uiso 1 1 calc R . . C38 C 0.3341(6) 0.4523(4) 0.6202(3) 0.0342(14) Uani 1 1 d . . . H38 H 0.2625 0.4361 0.6327 0.041 Uiso 1 1 calc R . . C39 C 0.3868(6) 0.5292(4) 0.6196(3) 0.0299(13) Uani 1 1 d . . . C40 C 0.4942(5) 0.5561(3) 0.6038(3) 0.0279(13) Uani 1 1 d . . . C41 C 0.8158(6) 0.4981(4) 0.5443(4) 0.0385(16) Uani 1 1 d . . . H41A H 0.8749 0.5383 0.5828 0.046 Uiso 1 1 calc R . . H41B H 0.8057 0.5217 0.5027 0.046 Uiso 1 1 calc R . . C42 C 0.8544(7) 0.4300(5) 0.5297(4) 0.050(2) Uani 1 1 d . . . H42A H 0.7885 0.3850 0.4998 0.060 Uiso 1 1 calc R . . H42B H 0.9167 0.4434 0.5053 0.060 Uiso 1 1 calc R . . C43 C 0.9679(8) 0.3663(6) 0.5908(5) 0.062(2) Uani 1 1 d . . . H43A H 1.0374 0.3971 0.5775 0.075 Uiso 1 1 calc R . . H43B H 0.9253 0.3194 0.5537 0.075 Uiso 1 1 calc R . . C44 C 1.0051(7) 0.3421(5) 0.6552(5) 0.055(2) Uani 1 1 d . . . H44A H 1.0540 0.3099 0.6485 0.065 Uiso 1 1 calc R . . H44B H 1.0528 0.3888 0.6916 0.065 Uiso 1 1 calc R . . C45 C 0.9354(9) 0.2487(6) 0.7213(6) 0.072(3) Uani 1 1 d . . . H45A H 0.9947 0.2293 0.7075 0.086 Uiso 1 1 calc R . . H45B H 0.8642 0.2030 0.7146 0.086 Uiso 1 1 calc R . . C46 C 0.9779(9) 0.2854(7) 0.7949(6) 0.077(3) Uani 1 1 d . . . H46A H 1.0420 0.3355 0.8016 0.093 Uiso 1 1 calc R . . H46B H 1.0085 0.2509 0.8216 0.093 Uiso 1 1 calc R . . C47 C 0.9096(9) 0.3160(6) 0.8914(5) 0.071(3) Uani 1 1 d . . . H47A H 0.9866 0.3576 0.9103 0.086 Uiso 1 1 calc R . . H47B H 0.9126 0.2690 0.9100 0.086 Uiso 1 1 calc R . . C48 C 0.8170(9) 0.3427(6) 0.9128(5) 0.067(3) Uani 1 1 d . . . H48A H 0.7386 0.3066 0.8868 0.080 Uiso 1 1 calc R . . H48B H 0.8244 0.3451 0.9631 0.080 Uiso 1 1 calc R . . C49 C 0.7673(9) 0.4579(6) 0.9161(4) 0.060(2) Uani 1 1 d . . . C50 C 0.6591(9) 0.4252(6) 0.9242(4) 0.060(2) Uani 1 1 d . . . H50 H 0.6266 0.3703 0.9200 0.072 Uiso 1 1 calc R . . C51 C 0.5934(9) 0.4752(6) 0.9392(4) 0.062(2) Uani 1 1 d . . . H51 H 0.5177 0.4527 0.9451 0.074 Uiso 1 1 calc R . . C52 C 0.6387(8) 0.5533(5) 0.9450(4) 0.053(2) Uani 1 1 d . . . H52 H 0.5951 0.5854 0.9551 0.063 Uiso 1 1 calc R . . C53 C 0.7529(7) 0.5875(5) 0.9357(4) 0.0468(19) Uani 1 1 d . . . C55 C 0.8056(8) 0.6692(6) 0.9423(4) 0.056(2) Uani 1 1 d . . . C56 C 0.9129(8) 0.7011(6) 0.9374(4) 0.058(2) Uani 1 1 d . . . H56 H 0.9469 0.7562 0.9441 0.069 Uiso 1 1 calc R . . C57 C 0.9772(8) 0.6524(6) 0.9220(4) 0.061(2) Uani 1 1 d . . . H57 H 1.0538 0.6758 0.9177 0.074 Uiso 1 1 calc R . . C58 C 0.9326(8) 0.5732(6) 0.9132(4) 0.057(2) Uani 1 1 d . . . H58 H 0.9759 0.5415 0.9015 0.069 Uiso 1 1 calc R . . C59 C 0.8181(7) 0.5395(5) 0.9221(4) 0.051(2) Uani 1 1 d . . . C60 C 0.7857(9) 0.7939(6) 0.9757(6) 0.075(3) Uani 1 1 d . . . H60A H 0.8397 0.8058 1.0223 0.090 Uiso 1 1 calc R . . H60B H 0.8311 0.8161 0.9436 0.090 Uiso 1 1 calc R . . C61 C 0.6992(10) 0.8278(6) 0.9782(5) 0.073(3) Uani 1 1 d . . . H61A H 0.7307 0.8746 1.0160 0.087 Uiso 1 1 calc R . . H61B H 0.6321 0.7901 0.9886 0.087 Uiso 1 1 calc R . . C62 C 0.5734(9) 0.8851(5) 0.9120(5) 0.068(3) Uani 1 1 d . . . H62A H 0.6018 0.9315 0.9500 0.082 Uiso 1 1 calc R . . H62B H 0.5024 0.8477 0.9188 0.082 Uiso 1 1 calc R . . C63 C 0.5467(9) 0.9082(5) 0.8445(5) 0.066(3) Uani 1 1 d . . . H63A H 0.4986 0.9418 0.8470 0.079 Uiso 1 1 calc R . . H63B H 0.6204 0.9397 0.8357 0.079 Uiso 1 1 calc R . . C64 C 0.3644(9) 0.8186(6) 0.7696(6) 0.074(3) Uani 1 1 d . . . H64A H 0.3347 0.8102 0.7186 0.089 Uiso 1 1 calc R . . H64B H 0.3397 0.8601 0.7909 0.089 Uiso 1 1 calc R . . C65 C 0.3113(8) 0.7433(5) 0.7939(6) 0.071(3) Uani 1 1 d . . . H65A H 0.3500 0.7493 0.8434 0.086 Uiso 1 1 calc R . . H65B H 0.2279 0.7345 0.7899 0.086 Uiso 1 1 calc R . . C66 C 0.2319(7) 0.6410(4) 0.6943(5) 0.052(2) Uani 1 1 d . . . H66A H 0.2369 0.6757 0.6602 0.062 Uiso 1 1 calc R . . H66B H 0.1553 0.6305 0.7047 0.062 Uiso 1 1 calc R . . C67 C 0.2436(6) 0.5674(4) 0.6652(4) 0.0426(17) Uani 1 1 d . . . H67A H 0.2553 0.5372 0.7019 0.051 Uiso 1 1 calc R . . H67B H 0.1724 0.5354 0.6286 0.051 Uiso 1 1 calc R . . C70 C 0.303(2) 0.9264(9) 0.9457(10) 0.33(3) Uani 1 1 d D . . C71 C 0.2863(14) 0.2709(18) 0.8663(10) 0.187(5) Uani 1 1 d DU . . C72 C 0.493(3) 0.0371(16) 0.6138(11) 0.229(7) Uani 1 1 d DU . . C78 C 0.2918(15) 0.5389(12) 0.8897(7) 0.149(7) Uani 1 1 d . . . H78A H 0.3419 0.5139 0.8720 0.223 Uiso 1 1 calc R . . H78B H 0.2764 0.5205 0.9316 0.223 Uiso 1 1 calc R . . H78C H 0.3307 0.5956 0.9008 0.223 Uiso 1 1 calc R . . C79 C 0.1865(10) 0.5197(6) 0.8391(5) 0.065(3) Uani 1 1 d . . . C80 C 0.4148(13) 0.7981(11) 1.0400(10) 0.112(5) Uani 1 1 d . . . C81 C 0.465(2) 0.8555(11) 1.1027(13) 0.218(14) Uani 1 1 d . . . H81A H 0.4316 0.8352 1.1396 0.326 Uiso 1 1 calc R . . H81B H 0.4471 0.9029 1.0956 0.326 Uiso 1 1 calc R . . H81C H 0.5490 0.8678 1.1160 0.326 Uiso 1 1 calc R . . N1 N 0.7857(5) 0.7996(3) 0.7738(3) 0.0321(12) Uani 1 1 d . . . N2 N 0.6812(5) 0.4034(3) 0.7434(3) 0.0314(12) Uani 1 1 d . . . N3 N 0.5899(5) 0.2790(3) 0.6655(3) 0.0353(13) Uani 1 1 d . . . N4 N 0.7265(5) 0.8836(3) 0.6710(3) 0.0344(13) Uani 1 1 d . . . N5 N 0.9010(6) 0.9522(4) 0.8747(3) 0.0530(17) Uani 1 1 d . . . H5A H 0.8494 0.9444 0.9019 0.064 Uiso 1 1 calc R . . H5B H 0.9498 0.9246 0.8865 0.064 Uiso 1 1 calc R . . N6 N 0.8478(7) 1.0298(4) 0.7738(4) 0.061(2) Uani 1 1 d . . . H6A H 0.9023 1.0470 0.7496 0.073 Uiso 1 1 calc R . . H6B H 0.7811 1.0381 0.7527 0.073 Uiso 1 1 calc R . . N7 N 0.1017(9) 0.5019(6) 0.7985(6) 0.092(3) Uani 1 1 d . . . N8 N 0.3822(13) 0.7406(7) 0.9920(8) 0.122(5) Uani 1 1 d . . . O1 O 0.7090(4) 0.4718(3) 0.5623(2) 0.0354(10) Uani 1 1 d . . . O2 O 0.8976(6) 0.4103(4) 0.5958(3) 0.0635(17) Uani 1 1 d . . . O3 O 0.9099(5) 0.2990(4) 0.6768(4) 0.0658(18) Uani 1 1 d . . . O4 O 0.8835(5) 0.2991(4) 0.8199(3) 0.0605(16) Uani 1 1 d . . . O5 O 0.8356(6) 0.4167(4) 0.8972(3) 0.0666(17) Uani 1 1 d . . . O6 O 0.7325(5) 0.7111(3) 0.9524(3) 0.0543(14) Uani 1 1 d . . . O7 O 0.6603(6) 0.8500(3) 0.9130(3) 0.0639(16) Uani 1 1 d . . . O8 O 0.4866(5) 0.8436(3) 0.7871(3) 0.0598(16) Uani 1 1 d . . . O9 O 0.3217(5) 0.6780(3) 0.7559(3) 0.0573(15) Uani 1 1 d . . . O10 O 0.3434(4) 0.5870(3) 0.6363(2) 0.0379(11) Uani 1 1 d . . . O11 O 0.0532(8) 0.8727(5) 0.9165(6) 0.134(4) Uani 1 1 d . . . O12 O 0.1852(8) 0.8476(5) 1.0171(5) 0.113(3) Uani 1 1 d . . . O13 O 0.1760(8) 0.9815(4) 1.0025(5) 0.100(3) Uani 1 1 d . . . O14 O 0.3015(13) 0.3739(7) 0.8029(6) 0.157(5) Uani 1 1 d U . . O15 O 0.4211(7) 0.2924(5) 0.7929(4) 0.100(3) Uani 1 1 d U . . O16 O 0.2139(9) 0.2475(6) 0.7322(6) 0.154(5) Uani 1 1 d U . . O17 O 0.4967(18) 0.1165(10) 0.7238(10) 0.248(7) Uani 1 1 d U . . O18 O 0.6495(10) 0.1379(6) 0.6844(10) 0.209(6) Uani 1 1 d U . . O19 O 0.6204(11) 0.0396(7) 0.7400(7) 0.158(5) Uani 1 1 d U . . O20 O 0.859(3) 0.0712(7) 0.5776(19) 0.48(3) Uani 1 1 d . . . O21 O 0.0829(18) 0.9603(8) 0.7410(6) 0.230(9) Uani 1 1 d . . . O22 O 0.414(2) 0.0178(17) 0.741(2) 0.42(2) Uani 1 1 d . . . F1 F 0.1051(5) 0.7940(3) 0.6692(3) 0.0712(14) Uani 1 1 d . . . F2 F -0.0791(4) 0.7694(3) 0.6099(3) 0.0608(13) Uani 1 1 d . . . F3 F 0.0132(4) 0.6838(3) 0.5868(3) 0.0614(13) Uani 1 1 d . . . F4 F -0.0291(5) 0.7566(4) 0.5092(3) 0.0763(16) Uani 1 1 d . . . F5 F 0.1563(5) 0.7808(3) 0.5678(3) 0.0785(17) Uani 1 1 d . . . F6 F 0.0622(5) 0.8657(3) 0.5895(3) 0.0700(15) Uani 1 1 d . . . F7 F 0.2483(15) 0.8483(10) 0.8957(10) 0.307(11) Uani 1 1 d . . . F8 F 0.3591(14) 0.9313(15) 0.9905(16) 0.43(2) Uani 1 1 d . . . F9 F 0.2598(11) 0.9669(7) 0.8924(6) 0.184(5) Uani 1 1 d . . . F10 F 0.3750(10) 0.3063(8) 0.9193(5) 0.164(4) Uani 1 1 d U . . F11 F 0.2801(12) 0.1830(10) 0.8532(8) 0.266(7) Uani 1 1 d U . . F12 F 0.1999(12) 0.2861(15) 0.8834(9) 0.342(10) Uani 1 1 d U . . F13 F 0.448(2) 0.0635(8) 0.5947(10) 0.347(9) Uani 1 1 d U . . F14 F 0.4249(13) -0.0389(6) 0.6449(9) 0.218(5) Uani 1 1 d U . . F15 F 0.544(3) -0.0159(10) 0.5780(11) 0.335(11) Uani 1 1 d U . . P1 P 0.03868(19) 0.77571(13) 0.58808(12) 0.0497(5) Uani 1 1 d . . . S1 S 0.1667(5) 0.9098(3) 0.9628(4) 0.185(3) Uani 1 1 d D . . S2 S 0.3051(2) 0.29671(18) 0.78856(16) 0.0786(8) Uani 1 1 d DU . . S3 S 0.5681(3) 0.0801(2) 0.6981(2) 0.1013(12) Uani 1 1 d DU . . Pd01 Pd 0.81397(5) 0.91479(3) 0.77349(3) 0.0415(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.038(4) 0.033(3) 0.035(3) -0.002(3) 0.000(3) 0.020(3) C2 0.030(3) 0.029(3) 0.026(3) 0.000(2) 0.001(2) 0.012(2) C3 0.033(3) 0.032(3) 0.025(3) 0.003(2) 0.004(3) 0.016(3) C4 0.026(3) 0.032(3) 0.031(3) 0.006(3) 0.000(3) 0.011(3) C5 0.028(3) 0.038(3) 0.038(4) 0.010(3) 0.005(3) 0.011(3) C6 0.032(4) 0.044(4) 0.037(4) 0.012(3) 0.005(3) 0.014(3) C7 0.031(4) 0.045(4) 0.038(4) 0.012(3) 0.006(3) 0.018(3) C8 0.034(4) 0.035(3) 0.029(3) 0.006(3) 0.003(3) 0.013(3) C9 0.037(4) 0.032(3) 0.021(3) 0.006(2) 0.005(2) 0.018(3) C10 0.031(3) 0.035(3) 0.030(3) 0.004(3) 0.007(3) 0.016(3) C11 0.035(4) 0.034(3) 0.027(3) 0.005(2) 0.006(3) 0.016(3) C12 0.032(3) 0.030(3) 0.027(3) 0.001(2) 0.002(3) 0.015(3) C13 0.032(3) 0.028(3) 0.034(3) 0.008(2) 0.002(3) 0.016(3) C14 0.038(4) 0.041(3) 0.028(3) 0.007(3) 0.007(3) 0.025(3) C15 0.047(4) 0.031(3) 0.038(4) 0.009(3) 0.010(3) 0.024(3) C16 0.045(4) 0.033(3) 0.045(4) 0.010(3) 0.013(3) 0.028(3) C17 0.045(4) 0.027(3) 0.042(4) 0.006(3) 0.012(3) 0.021(3) C18 0.046(4) 0.018(3) 0.041(4) 0.006(2) 0.010(3) 0.013(3) C19 0.043(4) 0.025(3) 0.044(4) 0.004(3) 0.010(3) 0.020(3) C20 0.036(4) 0.032(3) 0.038(4) 0.003(3) 0.006(3) 0.014(3) C21 0.042(4) 0.040(4) 0.044(4) 0.000(3) 0.013(3) 0.016(3) C22 0.047(4) 0.042(4) 0.045(4) 0.000(3) 0.015(3) 0.018(3) C23 0.040(4) 0.023(3) 0.043(4) -0.001(3) 0.006(3) 0.015(3) C24 0.041(4) 0.027(3) 0.037(3) 0.006(3) 0.005(3) 0.020(3) C25 0.043(4) 0.032(3) 0.044(4) 0.006(3) 0.012(3) 0.014(3) C26 0.033(4) 0.035(3) 0.050(4) 0.010(3) 0.011(3) 0.017(3) C27 0.046(4) 0.024(3) 0.041(4) 0.005(3) 0.007(3) 0.016(3) C28 0.043(4) 0.026(3) 0.046(4) 0.003(3) 0.004(3) 0.011(3) C29 0.050(5) 0.023(3) 0.053(4) 0.000(3) 0.010(3) 0.016(3) C30 0.088(7) 0.038(4) 0.061(6) -0.011(4) -0.010(5) 0.002(4) C31 0.125(9) 0.023(4) 0.071(6) -0.009(4) -0.011(6) 0.012(5) C32 0.044(4) 0.027(3) 0.029(3) 0.007(2) 0.006(3) 0.019(3) C33 0.043(4) 0.024(3) 0.035(3) 0.008(3) 0.005(3) 0.012(3) C34 0.035(4) 0.040(3) 0.033(3) 0.013(3) 0.011(3) 0.017(3) C35 0.033(3) 0.032(3) 0.028(3) 0.004(2) 0.001(3) 0.020(3) C36 0.040(4) 0.028(3) 0.021(3) 0.003(2) 0.002(3) 0.020(3) C36A 0.033(3) 0.029(3) 0.031(3) 0.003(2) 0.001(3) 0.020(3) C37 0.040(4) 0.027(3) 0.035(3) 0.006(3) 0.002(3) 0.013(3) C38 0.031(4) 0.038(3) 0.032(3) 0.004(3) 0.003(3) 0.015(3) C39 0.036(4) 0.030(3) 0.029(3) 0.005(2) 0.002(3) 0.022(3) C40 0.033(3) 0.025(3) 0.025(3) 0.005(2) 0.001(2) 0.013(2) C41 0.034(4) 0.046(4) 0.048(4) 0.017(3) 0.014(3) 0.027(3) C42 0.053(5) 0.061(5) 0.061(5) 0.026(4) 0.027(4) 0.040(4) C43 0.045(5) 0.083(6) 0.077(6) 0.034(5) 0.018(4) 0.040(5) C44 0.050(5) 0.043(4) 0.088(6) 0.023(4) 0.028(5) 0.029(4) C45 0.069(6) 0.071(6) 0.106(9) 0.043(6) 0.047(6) 0.041(5) C46 0.055(6) 0.092(7) 0.108(9) 0.066(7) 0.022(6) 0.039(5) C47 0.066(6) 0.090(7) 0.063(6) 0.038(5) 0.006(5) 0.033(6) C48 0.074(7) 0.088(7) 0.052(5) 0.030(5) 0.013(5) 0.044(6) C49 0.075(6) 0.074(6) 0.031(4) 0.015(4) 0.004(4) 0.031(5) C50 0.070(6) 0.063(5) 0.049(5) 0.021(4) 0.015(4) 0.021(5) C51 0.074(6) 0.069(6) 0.044(5) 0.027(4) 0.012(4) 0.022(5) C52 0.060(5) 0.063(5) 0.033(4) 0.016(4) 0.004(4) 0.022(4) C53 0.053(5) 0.052(4) 0.032(4) 0.012(3) 0.000(3) 0.019(4) C55 0.048(5) 0.077(6) 0.036(4) 0.022(4) 0.004(3) 0.012(4) C56 0.049(5) 0.070(6) 0.043(4) 0.012(4) 0.001(4) 0.010(4) C57 0.046(5) 0.085(7) 0.040(4) 0.010(4) 0.001(4) 0.013(5) C58 0.056(5) 0.081(6) 0.034(4) 0.009(4) 0.006(4) 0.026(5) C59 0.055(5) 0.060(5) 0.028(4) 0.013(3) -0.003(3) 0.012(4) C60 0.064(6) 0.065(6) 0.083(7) 0.013(5) -0.001(5) 0.018(5) C61 0.081(7) 0.054(5) 0.076(7) 0.005(5) 0.025(6) 0.013(5) C62 0.072(7) 0.047(5) 0.084(7) 0.000(5) 0.022(5) 0.022(5) C63 0.060(6) 0.045(5) 0.083(7) 0.010(4) 0.007(5) 0.014(4) C64 0.061(6) 0.063(6) 0.098(8) -0.005(5) 0.018(6) 0.031(5) C65 0.047(5) 0.058(5) 0.111(8) -0.009(5) 0.033(5) 0.024(4) C66 0.035(4) 0.042(4) 0.076(6) -0.006(4) 0.008(4) 0.021(3) C67 0.035(4) 0.039(4) 0.058(5) 0.003(3) 0.015(3) 0.018(3) C70 0.88(8) 0.134(16) 0.20(2) 0.121(16) 0.37(4) 0.31(3) C71 0.060(8) 0.361(15) 0.179(9) 0.172(12) 0.039(6) 0.075(11) C72 0.27(2) 0.243(15) 0.189(10) 0.081(8) -0.032(10) 0.154(9) C78 0.152(15) 0.23(2) 0.058(8) -0.002(10) -0.023(8) 0.101(15) C79 0.078(7) 0.086(7) 0.045(5) 0.027(5) 0.013(5) 0.042(6) C80 0.100(11) 0.121(12) 0.137(14) 0.072(11) 0.053(10) 0.035(10) C81 0.24(3) 0.123(15) 0.27(3) -0.068(17) 0.17(2) 0.007(16) N1 0.033(3) 0.031(3) 0.027(3) -0.001(2) -0.001(2) 0.012(2) N2 0.039(3) 0.033(3) 0.026(3) 0.005(2) 0.006(2) 0.021(2) N3 0.046(4) 0.024(2) 0.038(3) 0.011(2) 0.007(3) 0.016(2) N4 0.038(3) 0.022(2) 0.042(3) 0.005(2) 0.008(3) 0.011(2) N5 0.051(4) 0.042(3) 0.048(4) -0.002(3) 0.001(3) 0.002(3) N6 0.082(5) 0.032(3) 0.054(4) 0.004(3) 0.005(4) 0.009(3) N7 0.099(8) 0.076(6) 0.100(7) 0.012(5) -0.004(6) 0.049(6) N8 0.152(12) 0.075(7) 0.155(13) 0.041(8) 0.060(10) 0.041(8) O1 0.038(3) 0.034(2) 0.041(3) 0.010(2) 0.010(2) 0.021(2) O2 0.074(4) 0.084(4) 0.074(4) 0.044(3) 0.039(3) 0.061(4) O3 0.054(4) 0.082(4) 0.091(5) 0.051(4) 0.033(3) 0.042(3) O4 0.058(4) 0.071(4) 0.063(4) 0.025(3) 0.010(3) 0.036(3) O5 0.075(4) 0.080(4) 0.061(4) 0.027(3) 0.020(3) 0.042(4) O6 0.056(4) 0.052(3) 0.045(3) 0.008(2) 0.000(3) 0.015(3) O7 0.087(5) 0.050(3) 0.059(4) 0.011(3) 0.014(3) 0.032(3) O8 0.051(4) 0.039(3) 0.086(4) -0.002(3) 0.015(3) 0.016(3) O9 0.038(3) 0.052(3) 0.073(4) -0.021(3) 0.012(3) 0.018(2) O10 0.042(3) 0.031(2) 0.044(3) 0.003(2) 0.009(2) 0.020(2) O11 0.085(6) 0.059(5) 0.208(11) 0.027(6) -0.042(6) 0.008(4) O12 0.113(7) 0.096(6) 0.112(7) 0.011(5) -0.004(5) 0.038(5) O13 0.121(7) 0.051(4) 0.132(7) 0.012(4) 0.062(6) 0.018(4) O14 0.248(14) 0.162(8) 0.115(8) 0.010(6) 0.047(8) 0.151(9) O15 0.069(4) 0.099(6) 0.114(6) -0.030(5) 0.049(4) 0.006(4) O16 0.115(7) 0.119(7) 0.164(8) 0.038(6) -0.044(7) -0.001(6) O17 0.43(2) 0.239(13) 0.343(12) 0.237(10) 0.309(15) 0.276(14) O18 0.130(8) 0.094(6) 0.48(2) 0.167(9) 0.126(8) 0.070(5) O19 0.160(10) 0.134(9) 0.215(11) 0.108(8) 0.023(8) 0.087(8) O20 0.69(6) 0.050(7) 0.72(6) -0.016(17) 0.51(5) 0.006(16) O21 0.39(2) 0.166(12) 0.080(7) -0.054(7) -0.048(10) 0.123(14) O22 0.20(2) 0.30(3) 0.65(6) 0.05(3) -0.13(3) 0.10(2) F1 0.067(3) 0.072(3) 0.070(3) 0.014(3) 0.010(3) 0.024(3) F2 0.050(3) 0.055(3) 0.086(4) 0.008(3) 0.027(3) 0.026(2) F3 0.057(3) 0.053(3) 0.087(4) 0.012(3) 0.028(3) 0.030(2) F4 0.093(4) 0.094(4) 0.067(3) 0.016(3) 0.024(3) 0.066(4) F5 0.063(3) 0.085(4) 0.114(5) 0.038(4) 0.047(3) 0.039(3) F6 0.083(4) 0.055(3) 0.096(4) 0.031(3) 0.044(3) 0.036(3) F7 0.273(18) 0.241(15) 0.35(2) -0.167(15) 0.154(16) 0.040(13) F8 0.120(11) 0.44(3) 0.54(4) -0.25(3) -0.127(18) 0.111(15) F9 0.195(11) 0.164(10) 0.178(10) 0.010(8) 0.116(9) 0.008(8) F10 0.153(7) 0.283(11) 0.117(6) 0.082(7) 0.052(5) 0.131(8) F11 0.205(12) 0.254(10) 0.223(12) 0.173(9) -0.063(9) -0.054(9) F12 0.161(9) 0.76(3) 0.271(15) 0.33(2) 0.155(11) 0.234(16) F13 0.51(2) 0.165(10) 0.306(11) 0.057(9) -0.129(12) 0.182(11) F14 0.264(13) 0.094(6) 0.288(16) 0.000(7) 0.028(10) 0.096(7) F15 0.61(3) 0.167(13) 0.293(16) 0.063(11) 0.20(2) 0.164(17) P1 0.0450(12) 0.0507(12) 0.0650(14) 0.0189(10) 0.0242(10) 0.0230(9) S1 0.138(4) 0.088(3) 0.244(7) -0.058(4) -0.085(4) 0.042(3) S2 0.0566(15) 0.0866(18) 0.0844(18) 0.0043(15) 0.0268(13) 0.0126(13) S3 0.080(2) 0.096(2) 0.166(3) 0.086(2) 0.042(2) 0.0547(17) Pd01 0.0501(4) 0.0244(3) 0.0408(3) -0.0009(2) 0.0009(2) 0.0098(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.317(9) . ? C1 C2 1.414(9) . ? C2 C3 1.407(9) . ? C2 C10 1.432(9) . ? C3 C9 1.400(8) . ? C3 C4 1.431(9) . ? C4 C5 1.397(9) . ? C4 C6 1.415(10) . ? C5 N1 1.367(9) . ? C6 C7 1.350(10) . ? C7 C8 1.460(10) . ? C8 C14 1.360(9) . ? C8 C9 1.404(9) . ? C9 C12 1.422(9) . ? C10 C11 1.345(9) . ? C11 C12 1.428(9) . ? C12 C13 1.392(8) . ? C13 N2 1.353(8) . ? C14 N2 1.364(9) . ? C15 N2 1.461(8) . ? C15 N3 1.475(9) . ? C16 N3 1.339(9) . ? C16 C17 1.381(10) . ? C17 C18 1.425(10) . ? C17 C25 1.448(10) . ? C18 C19 1.407(10) . ? C18 C24 1.419(9) . ? C19 C20 1.373(9) . ? C19 C21 1.438(10) . ? C20 N3 1.338(9) . ? C21 C22 1.353(10) . ? C22 C23 1.442(10) . ? C23 C29 1.387(10) 2_666 ? C23 C24 1.404(10) . ? C24 C27 1.388(10) . ? C25 C26 1.343(10) . ? C26 C27 1.451(10) . ? C27 C28 1.396(10) 2_666 ? C28 N4 1.321(9) . ? C28 C27 1.396(10) 2_666 ? C29 N4 1.355(9) . ? C29 C23 1.387(10) 2_666 ? C30 N5 1.469(10) . ? C30 C31 1.501(14) . ? C31 N6 1.504(11) . ? C32 C33 1.377(10) . ? C32 C40 1.402(8) . ? C33 C34 1.408(9) . ? C34 C35 1.367(9) . ? C35 O1 1.383(7) . ? C35 C36 1.415(9) . ? C36 C36A 1.421(8) . ? C36 C40 1.440(8) . ? C36A C37 1.379(10) . ? C37 C38 1.407(9) . ? C38 C39 1.368(9) . ? C39 O10 1.371(7) . ? C39 C40 1.401(9) . ? C41 O1 1.415(8) . ? C41 C42 1.493(10) . ? C42 O2 1.459(9) . ? C43 O2 1.376(10) . ? C43 C44 1.451(12) . ? C44 O3 1.398(10) . ? C45 O3 1.423(11) . ? C45 C46 1.463(16) . ? C46 O4 1.454(12) . ? C47 O4 1.380(11) . ? C47 C48 1.508(14) . ? C48 O5 1.393(11) . ? C49 C50 1.355(13) . ? C49 O5 1.383(11) . ? C49 C59 1.417(12) . ? C50 C51 1.453(14) . ? C51 C52 1.351(12) . ? C52 C53 1.437(12) . ? C53 C59 1.413(12) . ? C53 C55 1.418(12) . ? C55 C56 1.321(12) . ? C55 O6 1.394(11) . ? C56 C57 1.423(13) . ? C57 C58 1.362(13) . ? C58 C59 1.435(12) . ? C60 C61 1.412(14) . ? C60 O6 1.432(11) . ? C61 O7 1.453(12) . ? C62 O7 1.424(11) . ? C62 C63 1.475(14) . ? C63 O8 1.438(11) . ? C64 O8 1.406(11) . ? C64 C65 1.528(14) . ? C65 O9 1.399(10) . ? C66 O9 1.415(10) . ? C66 C67 1.470(10) . ? C67 O10 1.452(9) . ? C70 F8 1.00(3) . ? C70 F7 1.52(2) . ? C70 F9 1.48(2) . ? C70 S1 1.747(19) . ? C71 F12 1.30(2) . ? C71 F10 1.30(2) . ? C71 F11 1.58(3) . ? C71 S2 1.731(14) . ? C72 F13 0.91(2) . ? C72 F14 1.67(4) . ? C72 F15 1.50(3) . ? C72 S3 1.713(17) . ? C78 C79 1.402(17) . ? C79 N7 1.123(12) . ? C80 N8 1.24(2) . ? C80 C81 1.43(3) . ? N1 Pd01 2.037(5) . ? N4 Pd01 2.040(6) . ? N5 Pd01 2.020(6) . ? N6 Pd01 2.024(6) . ? O11 S1 1.430(9) . ? O12 S1 1.707(11) . ? O13 S1 1.414(9) . ? O14 S2 1.429(11) . ? O15 S2 1.464(8) . ? O16 S2 1.407(10) . ? O17 S3 1.410(12) . ? O18 S3 1.328(10) . ? O19 S3 1.386(9) . ? F1 P1 1.612(6) . ? F2 P1 1.599(5) . ? F3 P1 1.615(5) . ? F4 P1 1.575(6) . ? F5 P1 1.587(6) . ? F6 P1 1.584(5) . ? F13 S3 2.223(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 122.5(6) . . ? C1 C2 C3 117.6(6) . . ? C1 C2 C10 123.1(6) . . ? C3 C2 C10 119.3(6) . . ? C9 C3 C2 120.6(6) . . ? C9 C3 C4 119.5(6) . . ? C2 C3 C4 119.9(6) . . ? C5 C4 C6 123.5(6) . . ? C5 C4 C3 117.6(6) . . ? C6 C4 C3 118.9(6) . . ? N1 C5 C4 121.5(6) . . ? C7 C6 C4 122.3(6) . . ? C6 C7 C8 119.5(7) . . ? C14 C8 C9 118.9(6) . . ? C14 C8 C7 122.2(6) . . ? C9 C8 C7 118.9(6) . . ? C3 C9 C8 120.8(6) . . ? C3 C9 C12 118.8(6) . . ? C8 C9 C12 120.3(6) . . ? C11 C10 C2 120.8(6) . . ? C10 C11 C12 120.5(6) . . ? C13 C12 C9 117.6(6) . . ? C13 C12 C11 122.5(6) . . ? C9 C12 C11 120.0(6) . . ? N2 C13 C12 120.6(6) . . ? N2 C14 C8 120.9(6) . . ? N2 C15 N3 109.7(5) . . ? N3 C16 C17 119.8(7) . . ? C16 C17 C18 118.3(7) . . ? C16 C17 C25 123.2(7) . . ? C18 C17 C25 118.5(6) . . ? C19 C18 C24 121.1(6) . . ? C19 C18 C17 119.3(6) . . ? C24 C18 C17 119.5(6) . . ? C20 C19 C18 118.7(7) . . ? C20 C19 C21 122.4(7) . . ? C18 C19 C21 118.9(6) . . ? N3 C20 C19 120.3(7) . . ? C22 C21 C19 120.6(7) . . ? C21 C22 C23 120.5(7) . . ? C29 C23 C24 117.8(7) 2_666 . ? C29 C23 C22 122.1(7) 2_666 . ? C24 C23 C22 120.2(6) . . ? C27 C24 C23 120.6(6) . . ? C27 C24 C18 120.8(6) . . ? C23 C24 C18 118.5(6) . . ? C26 C25 C17 121.2(7) . . ? C25 C26 C27 120.5(7) . . ? C24 C27 C28 118.1(7) . 2_666 ? C24 C27 C26 119.3(6) . . ? C28 C27 C26 122.4(7) 2_666 . ? N4 C28 C27 120.9(7) . 2_666 ? N4 C29 C23 120.5(7) . 2_666 ? N5 C30 C31 107.8(8) . . ? N6 C31 C30 107.0(8) . . ? C33 C32 C40 119.8(6) . . ? C32 C33 C34 121.7(6) . . ? C35 C34 C33 119.0(6) . . ? C34 C35 O1 123.3(6) . . ? C34 C35 C36 122.0(6) . . ? O1 C35 C36 114.7(5) . . ? C35 C36 C36A 122.9(6) . . ? C35 C36 C40 117.8(5) . . ? C36A C36 C40 119.3(6) . . ? C37 C36A C36 120.0(6) . . ? C36A C37 C38 120.4(6) . . ? C39 C38 C37 120.4(6) . . ? C38 C39 O10 124.3(6) . . ? C38 C39 C40 121.7(6) . . ? O10 C39 C40 113.9(5) . . ? C32 C40 C39 122.2(6) . . ? C32 C40 C36 119.7(6) . . ? C39 C40 C36 118.2(5) . . ? O1 C41 C42 108.5(6) . . ? O2 C42 C41 108.1(7) . . ? O2 C43 C44 112.7(8) . . ? O3 C44 C43 111.4(7) . . ? O3 C45 C46 114.2(8) . . ? C45 C46 O4 109.5(8) . . ? O4 C47 C48 108.8(7) . . ? O5 C48 C47 105.5(8) . . ? C50 C49 O5 124.9(9) . . ? C50 C49 C59 121.8(9) . . ? O5 C49 C59 113.2(9) . . ? C49 C50 C51 119.1(9) . . ? C52 C51 C50 120.9(9) . . ? C51 C52 C53 119.7(9) . . ? C59 C53 C55 118.0(8) . . ? C59 C53 C52 119.8(8) . . ? C55 C53 C52 122.2(8) . . ? C56 C55 O6 124.0(9) . . ? C56 C55 C53 122.3(10) . . ? O6 C55 C53 113.7(7) . . ? C55 C56 C57 119.5(9) . . ? C58 C57 C56 122.3(9) . . ? C57 C58 C59 117.7(9) . . ? C53 C59 C49 118.7(8) . . ? C53 C59 C58 120.2(8) . . ? C49 C59 C58 121.1(9) . . ? C61 C60 O6 109.8(8) . . ? C60 C61 O7 111.4(9) . . ? O7 C62 C63 108.6(8) . . ? O8 C63 C62 114.0(7) . . ? O8 C64 C65 112.1(8) . . ? O9 C65 C64 113.0(8) . . ? O9 C66 C67 109.5(6) . . ? O10 C67 C66 107.4(6) . . ? F8 C70 F7 119(2) . . ? F8 C70 F9 147(3) . . ? F7 C70 F9 91.7(17) . . ? F8 C70 S1 107(2) . . ? F7 C70 S1 86.8(13) . . ? F9 C70 S1 84.7(13) . . ? F12 C71 F10 105(2) . . ? F12 C71 F11 118(2) . . ? F10 C71 F11 105.4(14) . . ? F12 C71 S2 112.4(12) . . ? F10 C71 S2 114.6(13) . . ? F11 C71 S2 101.5(16) . . ? F13 C72 F14 115(4) . . ? F13 C72 F15 129(3) . . ? F14 C72 F15 87.1(17) . . ? F13 C72 S3 112(2) . . ? F14 C72 S3 86.5(13) . . ? F15 C72 S3 114.9(17) . . ? N7 C79 C78 177.8(13) . . ? N8 C80 C81 168(2) . . ? C1 N1 C5 120.9(6) . . ? C1 N1 Pd01 121.2(5) . . ? C5 N1 Pd01 117.7(4) . . ? C13 N2 C14 121.8(5) . . ? C13 N2 C15 118.6(6) . . ? C14 N2 C15 119.7(5) . . ? C16 N3 C20 123.4(6) . . ? C16 N3 C15 118.4(6) . . ? C20 N3 C15 118.1(6) . . ? C28 N4 C29 122.1(6) . . ? C28 N4 Pd01 121.2(5) . . ? C29 N4 Pd01 116.6(5) . . ? C30 N5 Pd01 108.5(5) . . ? C31 N6 Pd01 108.9(5) . . ? C35 O1 C41 115.2(5) . . ? C43 O2 C42 112.3(6) . . ? C44 O3 C45 114.0(6) . . ? C47 O4 C46 112.2(7) . . ? C49 O5 C48 118.0(7) . . ? C55 O6 C60 117.0(7) . . ? C62 O7 C61 114.4(7) . . ? C64 O8 C63 116.4(7) . . ? C65 O9 C66 115.1(7) . . ? C39 O10 C67 117.9(5) . . ? C72 F13 S3 45.6(17) . . ? F4 P1 F6 89.7(3) . . ? F4 P1 F5 90.8(3) . . ? F6 P1 F5 91.8(3) . . ? F4 P1 F2 90.2(3) . . ? F6 P1 F2 89.1(3) . . ? F5 P1 F2 178.6(3) . . ? F4 P1 F3 90.2(3) . . ? F6 P1 F3 179.3(3) . . ? F5 P1 F3 88.8(3) . . ? F2 P1 F3 90.2(3) . . ? F4 P1 F1 178.6(3) . . ? F6 P1 F1 90.9(3) . . ? F5 P1 F1 90.5(3) . . ? F2 P1 F1 88.5(3) . . ? F3 P1 F1 89.1(3) . . ? O13 S1 O11 111.3(7) . . ? O13 S1 O12 109.0(7) . . ? O11 S1 O12 106.3(6) . . ? O13 S1 C70 104.6(7) . . ? O11 S1 C70 129.2(11) . . ? O12 S1 C70 94.1(7) . . ? O16 S2 O14 113.0(8) . . ? O16 S2 O15 117.3(7) . . ? O14 S2 O15 115.0(7) . . ? O16 S2 C71 111.3(10) . . ? O14 S2 C71 97.9(12) . . ? O15 S2 C71 99.3(7) . . ? O18 S3 O19 109.4(8) . . ? O18 S3 O17 104.4(9) . . ? O19 S3 O17 118.1(9) . . ? O18 S3 C72 97.0(15) . . ? O19 S3 C72 120.0(11) . . ? O17 S3 C72 104.9(14) . . ? O18 S3 F13 91.7(10) . . ? O19 S3 F13 141.4(7) . . ? O17 S3 F13 85.3(11) . . ? C72 S3 F13 22.3(9) . . ? N5 Pd01 N6 84.1(3) . . ? N5 Pd01 N1 95.1(2) . . ? N6 Pd01 N1 178.1(3) . . ? N5 Pd01 N4 176.7(2) . . ? N6 Pd01 N4 92.6(2) . . ? N1 Pd01 N4 88.2(2) . . ? 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 N1 C1 C2 C3 0.7(9) . . . . ? N1 C1 C2 C10 -178.8(6) . . . . ? C1 C2 C3 C9 -178.8(6) . . . . ? C10 C2 C3 C9 0.8(9) . . . . ? C1 C2 C3 C4 -0.2(9) . . . . ? C10 C2 C3 C4 179.3(5) . . . . ? C9 C3 C4 C5 178.9(6) . . . . ? C2 C3 C4 C5 0.3(9) . . . . ? C9 C3 C4 C6 -0.2(9) . . . . ? C2 C3 C4 C6 -178.8(6) . . . . ? C6 C4 C5 N1 178.2(6) . . . . ? C3 C4 C5 N1 -0.8(9) . . . . ? C5 C4 C6 C7 179.8(6) . . . . ? C3 C4 C6 C7 -1.2(10) . . . . ? C4 C6 C7 C8 1.0(10) . . . . ? C6 C7 C8 C14 -179.5(6) . . . . ? C6 C7 C8 C9 0.6(9) . . . . ? C2 C3 C9 C8 -179.7(6) . . . . ? C4 C3 C9 C8 1.7(9) . . . . ? C2 C3 C9 C12 -1.9(9) . . . . ? C4 C3 C9 C12 179.6(5) . . . . ? C14 C8 C9 C3 178.1(6) . . . . ? C7 C8 C9 C3 -1.9(9) . . . . ? C14 C8 C9 C12 0.4(9) . . . . ? C7 C8 C9 C12 -179.7(6) . . . . ? C1 C2 C10 C11 -179.9(6) . . . . ? C3 C2 C10 C11 0.6(9) . . . . ? C2 C10 C11 C12 -0.8(9) . . . . ? C3 C9 C12 C13 -178.1(5) . . . . ? C8 C9 C12 C13 -0.3(9) . . . . ? C3 C9 C12 C11 1.6(9) . . . . ? C8 C9 C12 C11 179.5(6) . . . . ? C10 C11 C12 C13 179.4(6) . . . . ? C10 C11 C12 C9 -0.3(9) . . . . ? C9 C12 C13 N2 -0.1(9) . . . . ? C11 C12 C13 N2 -179.9(6) . . . . ? C9 C8 C14 N2 0.0(9) . . . . ? C7 C8 C14 N2 -179.9(6) . . . . ? N3 C16 C17 C18 3.1(9) . . . . ? N3 C16 C17 C25 -176.3(6) . . . . ? C16 C17 C18 C19 0.9(9) . . . . ? C25 C17 C18 C19 -179.7(6) . . . . ? C16 C17 C18 C24 -178.0(5) . . . . ? C25 C17 C18 C24 1.4(9) . . . . ? C24 C18 C19 C20 176.9(6) . . . . ? C17 C18 C19 C20 -2.0(9) . . . . ? C24 C18 C19 C21 -2.2(9) . . . . ? C17 C18 C19 C21 178.9(6) . . . . ? C18 C19 C20 N3 -0.8(9) . . . . ? C21 C19 C20 N3 178.2(6) . . . . ? C20 C19 C21 C22 -176.8(7) . . . . ? C18 C19 C21 C22 2.3(10) . . . . ? C19 C21 C22 C23 0.8(11) . . . . ? C21 C22 C23 C29 175.7(7) . . . 2_666 ? C21 C22 C23 C24 -4.1(10) . . . . ? C29 C23 C24 C27 1.7(9) 2_666 . . . ? C22 C23 C24 C27 -178.6(6) . . . . ? C29 C23 C24 C18 -175.7(5) 2_666 . . . ? C22 C23 C24 C18 4.0(9) . . . . ? C19 C18 C24 C27 -178.3(6) . . . . ? C17 C18 C24 C27 0.6(9) . . . . ? C19 C18 C24 C23 -0.9(9) . . . . ? C17 C18 C24 C23 177.9(6) . . . . ? C16 C17 C25 C26 176.4(6) . . . . ? C18 C17 C25 C26 -3.0(9) . . . . ? C17 C25 C26 C27 2.6(10) . . . . ? C23 C24 C27 C28 -2.8(9) . . . 2_666 ? C18 C24 C27 C28 174.5(6) . . . 2_666 ? C23 C24 C27 C26 -178.4(6) . . . . ? C18 C24 C27 C26 -1.1(9) . . . . ? C25 C26 C27 C24 -0.5(9) . . . . ? C25 C26 C27 C28 -175.9(6) . . . 2_666 ? N5 C30 C31 N6 -53.4(12) . . . . ? C40 C32 C33 C34 -1.7(9) . . . . ? C32 C33 C34 C35 1.9(10) . . . . ? C33 C34 C35 O1 -178.9(6) . . . . ? C33 C34 C35 C36 -0.4(9) . . . . ? C34 C35 C36 C36A 179.6(6) . . . . ? O1 C35 C36 C36A -1.9(8) . . . . ? C34 C35 C36 C40 -1.1(9) . . . . ? O1 C35 C36 C40 177.4(5) . . . . ? C35 C36 C36A C37 178.4(6) . . . . ? C40 C36 C36A C37 -0.9(9) . . . . ? C36 C36A C37 C38 -1.2(9) . . . . ? C36A C37 C38 C39 2.8(9) . . . . ? C37 C38 C39 O10 -179.9(6) . . . . ? C37 C38 C39 C40 -2.2(9) . . . . ? C33 C32 C40 C39 179.1(6) . . . . ? C33 C32 C40 C36 0.1(9) . . . . ? C38 C39 C40 C32 -179.0(6) . . . . ? O10 C39 C40 C32 -1.1(8) . . . . ? C38 C39 C40 C36 0.0(9) . . . . ? O10 C39 C40 C36 177.9(5) . . . . ? C35 C36 C40 C32 1.3(8) . . . . ? C36A C36 C40 C32 -179.4(5) . . . . ? C35 C36 C40 C39 -177.8(5) . . . . ? C36A C36 C40 C39 1.5(8) . . . . ? O1 C41 C42 O2 -74.6(8) . . . . ? O2 C43 C44 O3 58.0(11) . . . . ? O3 C45 C46 O4 70.6(10) . . . . ? O4 C47 C48 O5 -71.6(10) . . . . ? O5 C49 C50 C51 -175.5(7) . . . . ? C59 C49 C50 C51 0.1(12) . . . . ? C49 C50 C51 C52 0.3(12) . . . . ? C50 C51 C52 C53 0.4(12) . . . . ? C51 C52 C53 C59 -1.4(11) . . . . ? C51 C52 C53 C55 -178.8(7) . . . . ? C59 C53 C55 C56 -1.1(11) . . . . ? C52 C53 C55 C56 176.4(7) . . . . ? C59 C53 C55 O6 177.2(6) . . . . ? C52 C53 C55 O6 -5.3(10) . . . . ? O6 C55 C56 C57 -175.4(7) . . . . ? C53 C55 C56 C57 2.7(12) . . . . ? C55 C56 C57 C58 -1.1(12) . . . . ? C56 C57 C58 C59 -1.9(12) . . . . ? C55 C53 C59 C49 179.2(6) . . . . ? C52 C53 C59 C49 1.7(10) . . . . ? C55 C53 C59 C58 -2.1(10) . . . . ? C52 C53 C59 C58 -179.6(7) . . . . ? C50 C49 C59 C53 -1.1(11) . . . . ? O5 C49 C59 C53 175.0(6) . . . . ? C50 C49 C59 C58 -179.7(7) . . . . ? O5 C49 C59 C58 -3.7(10) . . . . ? C57 C58 C59 C53 3.5(11) . . . . ? C57 C58 C59 C49 -177.9(7) . . . . ? O6 C60 C61 O7 -90.6(10) . . . . ? O7 C62 C63 O8 69.6(10) . . . . ? O8 C64 C65 O9 -71.1(12) . . . . ? O9 C66 C67 O10 -72.5(8) . . . . ? C2 C1 N1 C5 -1.3(9) . . . . ? C2 C1 N1 Pd01 174.1(4) . . . . ? C4 C5 N1 C1 1.4(9) . . . . ? C4 C5 N1 Pd01 -174.3(5) . . . . ? C12 C13 N2 C14 0.5(9) . . . . ? C12 C13 N2 C15 -179.2(5) . . . . ? C8 C14 N2 C13 -0.4(9) . . . . ? C8 C14 N2 C15 179.2(6) . . . . ? N3 C15 N2 C13 84.6(7) . . . . ? N3 C15 N2 C14 -95.0(7) . . . . ? C17 C16 N3 C20 -6.3(9) . . . . ? C17 C16 N3 C15 177.5(5) . . . . ? C19 C20 N3 C16 5.1(9) . . . . ? C19 C20 N3 C15 -178.7(5) . . . . ? N2 C15 N3 C16 -97.3(7) . . . . ? N2 C15 N3 C20 86.3(7) . . . . ? C27 C28 N4 C29 -0.8(9) 2_666 . . . ? C27 C28 N4 Pd01 175.3(4) 2_666 . . . ? C23 C29 N4 C28 1.9(9) 2_666 . . . ? C23 C29 N4 Pd01 -174.3(5) 2_666 . . . ? C31 C30 N5 Pd01 43.3(10) . . . . ? C30 C31 N6 Pd01 37.8(10) . . . . ? C34 C35 O1 C41 -5.5(8) . . . . ? C36 C35 O1 C41 176.0(5) . . . . ? C42 C41 O1 C35 -177.3(6) . . . . ? C44 C43 O2 C42 -176.2(8) . . . . ? C41 C42 O2 C43 -160.6(7) . . . . ? C43 C44 O3 C45 156.5(9) . . . . ? C46 C45 O3 C44 88.0(10) . . . . ? C48 C47 O4 C46 170.5(8) . . . . ? C45 C46 O4 C47 165.5(8) . . . . ? C50 C49 O5 C48 -26.2(12) . . . . ? C59 C49 O5 C48 158.0(7) . . . . ? C47 C48 O5 C49 -175.6(7) . . . . ? C56 C55 O6 C60 -16.0(11) . . . . ? C53 C55 O6 C60 165.7(7) . . . . ? C61 C60 O6 C55 175.6(8) . . . . ? C63 C62 O7 C61 177.1(7) . . . . ? C60 C61 O7 C62 -179.6(8) . . . . ? C65 C64 O8 C63 -104.0(9) . . . . ? C62 C63 O8 C64 91.9(10) . . . . ? C64 C65 O9 C66 -86.3(10) . . . . ? C67 C66 O9 C65 -171.6(8) . . . . ? C38 C39 O10 C67 8.5(9) . . . . ? C40 C39 O10 C67 -169.3(6) . . . . ? C66 C67 O10 C39 166.2(6) . . . . ? F14 C72 F13 S3 97(4) . . . . ? F15 C72 F13 S3 -155(7) . . . . ? F8 C70 S1 O13 70(2) . . . . ? F7 C70 S1 O13 -170.1(12) . . . . ? F9 C70 S1 O13 -78.1(11) . . . . ? F8 C70 S1 O11 -156(2) . . . . ? F7 C70 S1 O11 -36.0(15) . . . . ? F9 C70 S1 O11 56.0(11) . . . . ? F8 C70 S1 O12 -41(2) . . . . ? F7 C70 S1 O12 79.0(13) . . . . ? F9 C70 S1 O12 171.0(8) . . . . ? F12 C71 S2 O16 -70(3) . . . . ? F10 C71 S2 O16 170.6(17) . . . . ? F11 C71 S2 O16 57.5(12) . . . . ? F12 C71 S2 O14 49(2) . . . . ? F10 C71 S2 O14 -71(2) . . . . ? F11 C71 S2 O14 176.1(11) . . . . ? F12 C71 S2 O15 166(2) . . . . ? F10 C71 S2 O15 46(2) . . . . ? F11 C71 S2 O15 -66.8(11) . . . . ? F13 C72 S3 O18 -77(4) . . . . ? F14 C72 S3 O18 167.0(11) . . . . ? F15 C72 S3 O18 82(2) . . . . ? F13 C72 S3 O19 165(3) . . . . ? F14 C72 S3 O19 49.7(19) . . . . ? F15 C72 S3 O19 -35(3) . . . . ? F13 C72 S3 O17 30(4) . . . . ? F14 C72 S3 O17 -86.0(12) . . . . ? F15 C72 S3 O17 -171(2) . . . . ? F14 C72 S3 F13 -116(5) . . . . ? F15 C72 S3 F13 159(6) . . . . ? C72 F13 S3 O18 104(4) . . . . ? C72 F13 S3 O19 -20(5) . . . . ? C72 F13 S3 O17 -151(4) . . . . ? C30 N5 Pd01 N6 -17.5(7) . . . . ? C30 N5 Pd01 N1 160.7(7) . . . . ? C30 N5 Pd01 N4 -25(5) . . . . ? C31 N6 Pd01 N5 -11.5(7) . . . . ? C31 N6 Pd01 N1 -77(7) . . . . ? C31 N6 Pd01 N4 168.0(7) . . . . ? C1 N1 Pd01 N5 95.6(5) . . . . ? C5 N1 Pd01 N5 -88.8(5) . . . . ? C1 N1 Pd01 N6 161(7) . . . . ? C5 N1 Pd01 N6 -23(8) . . . . ? C1 N1 Pd01 N4 -84.1(5) . . . . ? C5 N1 Pd01 N4 91.5(5) . . . . ? C28 N4 Pd01 N5 91(5) . . . . ? C29 N4 Pd01 N5 -93(5) . . . . ? C28 N4 Pd01 N6 84.0(5) . . . . ? C29 N4 Pd01 N6 -99.7(5) . . . . ? C28 N4 Pd01 N1 -94.2(5) . . . . ? C29 N4 Pd01 N1 82.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.41 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.501 _refine_diff_density_min -1.661 _refine_diff_density_rms 0.170 # Attachment '- Catenano 6(8)2-6PF6.cif' data_0854549_b2_0s _database_code_depnum_ccdc_archive 'CCDC 837132' #TrackingRef '- Catenano 6(8)2-6PF6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C122 H144 F18 N14 O46 Pd2 S6' _chemical_formula_weight 3289.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.0255(5) _cell_length_b 20.4941(8) _cell_length_c 28.0429(12) _cell_angle_alpha 90.00 _cell_angle_beta 93.676(2) _cell_angle_gamma 90.00 _cell_volume 6897.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 30755 _cell_measurement_theta_min 5.823 _cell_measurement_theta_max 52.705 _exptl_crystal_description 'irregular block' _exptl_crystal_colour orange _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3384 _exptl_absorpt_coefficient_mu 0.467 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7899 _exptl_absorpt_correction_T_max 0.9248 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 155604 _diffrn_reflns_av_R_equivalents 0.0594 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 28.37 _reflns_number_total 17198 _reflns_number_gt 13781 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0947P)^2^+58.5774P] 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 17198 _refine_ls_number_parameters 949 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.1270 _refine_ls_R_factor_gt 0.1062 _refine_ls_wR_factor_ref 0.2712 _refine_ls_wR_factor_gt 0.2562 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.125 _refine_ls_shift/su_max 0.033 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0797(5) 0.2987(3) 0.5832(2) 0.0266(11) Uani 1 1 d . . . H1 H 0.0281 0.3305 0.5709 0.032 Uiso 1 1 calc R . . C2 C 0.0412(4) 0.2469(2) 0.60910(19) 0.0202(10) Uani 1 1 d . . . C3 C 0.1189(4) 0.2005(2) 0.62740(18) 0.0181(9) Uani 1 1 d . . . C4 C 0.2329(4) 0.2077(3) 0.61873(19) 0.0217(10) Uani 1 1 d . . . C5 C 0.2630(5) 0.2612(3) 0.5920(2) 0.0255(11) Uani 1 1 d . . . H5 H 0.3391 0.2666 0.5856 0.031 Uiso 1 1 calc R . . C6 C -0.0749(4) 0.2389(3) 0.6185(2) 0.0258(11) Uani 1 1 d . . . H6 H -0.1278 0.2705 0.6070 0.031 Uiso 1 1 calc R . . C7 C -0.1090(5) 0.1872(3) 0.6434(2) 0.0274(11) Uani 1 1 d . . . H7 H -0.1857 0.1825 0.6489 0.033 Uiso 1 1 calc R . . C8 C -0.0305(4) 0.1391(2) 0.66165(18) 0.0206(10) Uani 1 1 d . . . C9 C 0.0839(4) 0.1463(2) 0.65359(17) 0.0189(9) Uani 1 1 d . . . C10 C 0.3114(5) 0.1593(3) 0.6363(2) 0.0257(11) Uani 1 1 d . . . H10 H 0.3876 0.1634 0.6297 0.031 Uiso 1 1 calc R . . C11 C 0.2786(5) 0.1082(3) 0.6618(2) 0.0292(12) Uani 1 1 d . . . H11 H 0.3320 0.0771 0.6736 0.035 Uiso 1 1 calc R . . C12 C 0.1626(4) 0.1000(3) 0.67147(19) 0.0231(10) Uani 1 1 d . . . C13 C 0.1243(5) 0.0476(3) 0.6966(2) 0.0261(11) Uani 1 1 d . . . H13 H 0.1754 0.0153 0.7086 0.031 Uiso 1 1 calc R . . C14 C -0.0619(5) 0.0850(3) 0.68739(18) 0.0241(11) Uani 1 1 d . . . H14 H -0.1381 0.0786 0.6932 0.029 Uiso 1 1 calc R . . C15 C -0.0247(5) -0.0175(3) 0.7295(2) 0.0310(12) Uani 1 1 d . . . H15A H -0.0880 -0.0054 0.7486 0.037 Uiso 1 1 calc R . . H15B H 0.0360 -0.0344 0.7517 0.037 Uiso 1 1 calc R . . C16 C -0.0610(5) -0.0700(3) 0.69418(19) 0.0268(11) Uani 1 1 d . . . C17 C -0.1709(5) -0.0902(3) 0.6898(2) 0.0302(12) Uani 1 1 d . . . H17 H -0.2241 -0.0709 0.7091 0.036 Uiso 1 1 calc R . . C18 C -0.2041(5) -0.1390(3) 0.6572(2) 0.0291(12) Uani 1 1 d . . . H18 H -0.2794 -0.1534 0.6548 0.035 Uiso 1 1 calc R . . C19 C -0.1277(5) -0.1665(3) 0.6284(2) 0.0256(11) Uani 1 1 d . . . C20 C -0.0170(5) -0.1461(3) 0.6331(2) 0.0295(12) Uani 1 1 d . . . H20 H 0.0359 -0.1652 0.6135 0.035 Uiso 1 1 calc R . . C21 C 0.0164(5) -0.0990(3) 0.6655(2) 0.0272(11) Uani 1 1 d . . . H21 H 0.0923 -0.0860 0.6686 0.033 Uiso 1 1 calc R . . C22 C -0.1606(5) -0.2177(3) 0.5929(2) 0.0269(11) Uani 1 1 d . . . C23 C -0.0860(5) -0.2663(3) 0.5818(2) 0.0308(13) Uani 1 1 d . . . H23 H -0.0139 -0.2675 0.5977 0.037 Uiso 1 1 calc R . . C24 C -0.2649(5) -0.2188(3) 0.5681(2) 0.0308(12) Uani 1 1 d . . . H24 H -0.3195 -0.1872 0.5749 0.037 Uiso 1 1 calc R . . C25 C -0.1155(5) -0.3124(3) 0.5480(2) 0.0292(12) Uani 1 1 d . . . H25 H -0.0643 -0.3462 0.5418 0.035 Uiso 1 1 calc R . . C26 C -0.2891(5) -0.2657(3) 0.5336(2) 0.0318(13) Uani 1 1 d . . . H26 H -0.3601 -0.2657 0.5167 0.038 Uiso 1 1 calc R . . C27 C 0.3077(7) 0.5086(3) 0.5130(3) 0.0453(17) Uani 1 1 d . . . H27A H 0.3874 0.5071 0.5242 0.054 Uiso 1 1 calc R . . H27B H 0.2954 0.5478 0.4926 0.054 Uiso 1 1 calc R . . C28 C 0.2376(7) 0.5120(3) 0.5543(3) 0.0428(16) Uani 1 1 d . . . H28A H 0.1589 0.5200 0.5432 0.051 Uiso 1 1 calc R . . H28B H 0.2628 0.5480 0.5758 0.051 Uiso 1 1 calc R . . C29 C 0.2047(6) 0.2657(3) 0.2564(2) 0.0353(14) Uani 1 1 d . . . H29 H 0.2290 0.3027 0.2747 0.042 Uiso 1 1 calc R . . C30 C 0.0923(5) 0.2508(3) 0.2514(2) 0.0332(13) Uani 1 1 d . . . C31 C 0.0580(5) 0.1973(3) 0.2241(2) 0.0343(14) Uani 1 1 d . . . H31 H -0.0191 0.1868 0.2204 0.041 Uiso 1 1 calc R . . C32 C 0.1335(5) 0.1594(3) 0.2025(2) 0.0340(14) Uani 1 1 d . . . H32 H 0.1084 0.1231 0.1838 0.041 Uiso 1 1 calc R . . C33 C 0.2478(5) 0.1736(3) 0.2077(2) 0.0327(13) Uani 1 1 d . . . C34 C 0.2816(5) 0.2272(3) 0.2352(2) 0.0347(14) Uani 1 1 d . . . H34 H 0.3586 0.2376 0.2393 0.042 Uiso 1 1 calc R . . C35 C 0.4321(6) 0.1491(4) 0.1881(3) 0.0401(15) Uani 1 1 d . . . H35A H 0.4632 0.1422 0.2212 0.048 Uiso 1 1 calc R . . H35B H 0.4423 0.1955 0.1797 0.048 Uiso 1 1 calc R . . C36 C 0.4912(6) 0.1070(4) 0.1549(3) 0.0439(16) Uani 1 1 d . . . H36A H 0.5724 0.1150 0.1589 0.053 Uiso 1 1 calc R . . H36B H 0.4771 0.0605 0.1618 0.053 Uiso 1 1 calc R . . C37 C 0.5319(6) 0.1145(3) 0.0724(3) 0.0390(15) Uani 1 1 d . . . H37A H 0.4925 0.1106 0.0404 0.047 Uiso 1 1 calc R . . H37B H 0.5737 0.0735 0.0789 0.047 Uiso 1 1 calc R . . C38 C 0.6119(6) 0.1697(3) 0.0720(3) 0.0405(15) Uani 1 1 d . . . H38A H 0.6442 0.1781 0.1048 0.049 Uiso 1 1 calc R . . H38B H 0.6734 0.1587 0.0515 0.049 Uiso 1 1 calc R . . C39 C 0.6244(5) 0.2826(3) 0.0588(3) 0.0388(15) Uani 1 1 d . . . H39A H 0.7015 0.2711 0.0516 0.047 Uiso 1 1 calc R . . H39B H 0.6261 0.2986 0.0922 0.047 Uiso 1 1 calc R . . C40 C 0.5816(5) 0.3347(3) 0.0258(3) 0.0391(15) Uani 1 1 d . . . H40A H 0.6376 0.3700 0.0247 0.047 Uiso 1 1 calc R . . H40B H 0.5686 0.3166 -0.0068 0.047 Uiso 1 1 calc R . . C41 C 0.4430(5) 0.4123(3) 0.0115(2) 0.0282(12) Uani 1 1 d . . . H41A H 0.4294 0.3964 -0.0217 0.034 Uiso 1 1 calc R . . H41B H 0.5006 0.4468 0.0116 0.034 Uiso 1 1 calc R . . C42 C 0.3377(4) 0.4398(3) 0.0288(2) 0.0239(10) Uani 1 1 d . . . H42A H 0.3460 0.4474 0.0637 0.029 Uiso 1 1 calc R . . H42B H 0.3195 0.4818 0.0127 0.029 Uiso 1 1 calc R . . C43 C 0.1469(4) 0.4109(2) 0.02925(18) 0.0192(9) Uani 1 1 d . . . C44 C 0.0628(5) 0.3657(3) 0.01611(19) 0.0235(10) Uani 1 1 d . . . H44 H 0.0807 0.3263 0.0004 0.028 Uiso 1 1 calc R . . C45 C -0.0457(5) 0.3785(3) 0.02600(19) 0.0241(10) Uani 1 1 d . . . H45 H -0.1025 0.3477 0.0172 0.029 Uiso 1 1 calc R . . C46 C -0.0730(4) 0.4359(3) 0.04876(18) 0.0199(10) Uani 1 1 d . . . C47 C 0.0093(4) 0.4809(3) 0.06113(18) 0.0211(10) Uani 1 1 d . . . H47 H -0.0093 0.5206 0.0762 0.025 Uiso 1 1 calc R . . C48 C 0.1199(4) 0.4683(2) 0.05144(18) 0.0206(10) Uani 1 1 d . . . H48 H 0.1764 0.4992 0.0601 0.025 Uiso 1 1 calc R . . C49 C -0.2118(5) 0.4975(3) 0.08578(19) 0.0254(11) Uani 1 1 d . . . H49A H -0.2150 0.5379 0.0664 0.031 Uiso 1 1 calc R . . H49B H -0.1550 0.5034 0.1126 0.031 Uiso 1 1 calc R . . C50 C -0.3237(5) 0.4839(3) 0.1047(2) 0.0274(11) Uani 1 1 d . C . H50A H -0.3508 0.5229 0.1212 0.033 Uiso 1 1 calc R . . H50B H -0.3784 0.4728 0.0780 0.033 Uiso 1 1 calc R . . C51 C -0.4077(5) 0.4217(5) 0.1632(3) 0.0474(19) Uani 1 1 d . C . H51A H -0.4148 0.3747 0.1706 0.057 Uiso 1 1 calc R . . H51B H -0.4746 0.4348 0.1430 0.057 Uiso 1 1 calc R . . C52 C -0.4043(6) 0.4586(8) 0.2076(3) 0.094(5) Uani 1 1 d . . . H52A H -0.4765 0.4567 0.2226 0.113 Uiso 1 1 calc R A 1 H52B H -0.3838 0.5047 0.2025 0.113 Uiso 1 1 calc R A 1 C53 C -0.3074(9) 0.4474(6) 0.2809(3) 0.079(4) Uani 1 1 d . . . H53A H -0.3815 0.4435 0.2941 0.094 Uiso 1 1 calc R B 1 H53B H -0.2896 0.4944 0.2787 0.094 Uiso 1 1 calc R B 1 C54 C -0.2259(7) 0.4167(6) 0.3133(3) 0.067(3) Uani 1 1 d . C . H54A H -0.2044 0.4477 0.3393 0.081 Uiso 1 1 calc R . . H54B H -0.2604 0.3783 0.3278 0.081 Uiso 1 1 calc R . . C55 C -0.0531(6) 0.3647(5) 0.3256(3) 0.052(2) Uani 1 1 d . C . H55A H -0.0911 0.3279 0.3406 0.062 Uiso 1 1 calc R . . H55B H -0.0282 0.3959 0.3510 0.062 Uiso 1 1 calc R . . C56 C 0.0447(6) 0.3400(4) 0.3016(2) 0.0380(15) Uani 1 1 d . . . H56A H 0.0756 0.3751 0.2821 0.046 Uiso 1 1 calc R . . H56B H 0.1034 0.3259 0.3258 0.046 Uiso 1 1 calc R . . C57 C 0.8372(7) 0.4634(5) 0.6460(4) 0.066(3) Uani 1 1 d . . . C58 C 0.6008(9) 0.6354(5) 0.6443(3) 0.063(2) Uani 1 1 d . . . C59 C 0.4404(16) 0.8425(9) 0.6453(6) 0.129(4) Uani 1 1 d DU . . C60 C 0.7442(11) 0.2499(8) 0.2651(8) 0.137(7) Uani 1 1 d . . . H60A H 0.7798 0.2069 0.2662 0.205 Uiso 1 1 calc R . . H60B H 0.7087 0.2578 0.2950 0.205 Uiso 1 1 calc R . . H60C H 0.8006 0.2836 0.2607 0.205 Uiso 1 1 calc R . . N1 N 0.1884(4) 0.3054(2) 0.57485(18) 0.0262(10) Uani 1 1 d . . . N2 N 0.0150(4) 0.0415(2) 0.70425(15) 0.0246(9) Uani 1 1 d . . . N3 N -0.2144(4) -0.3113(2) 0.52364(18) 0.0283(10) Uani 1 1 d . . . N4 N 0.2771(5) 0.4488(3) 0.4851(2) 0.0372(13) Uani 1 1 d . . . H4A H 0.3364 0.4356 0.4683 0.045 Uiso 1 1 calc R . . H4B H 0.2181 0.4577 0.4636 0.045 Uiso 1 1 calc R . . N5 N 0.2480(5) 0.4480(3) 0.5801(2) 0.0340(11) Uani 1 1 d . . . H5A H 0.1924 0.4438 0.6010 0.041 Uiso 1 1 calc R . . H5B H 0.3157 0.4453 0.5972 0.041 Uiso 1 1 calc R . . N6 N 0.6600(13) 0.2521(7) 0.2252(4) 0.112(5) Uani 1 1 d . . . N7 N 0.8209(7) 0.2979(4) 0.4615(3) 0.0593(19) Uani 1 1 d . . . O1 O 0.3160(4) 0.1331(2) 0.18467(18) 0.0386(10) Uani 1 1 d . . . O2 O 0.4512(4) 0.1222(2) 0.10753(18) 0.0389(10) Uani 1 1 d . . . O3 O 0.5552(4) 0.2263(2) 0.05395(18) 0.0396(11) Uani 1 1 d . . . O4 O 0.4811(3) 0.3602(2) 0.04143(16) 0.0304(9) Uani 1 1 d . . . O5 O 0.2522(3) 0.39316(18) 0.01765(15) 0.0250(8) Uani 1 1 d . . . O6 O -0.1833(3) 0.4432(2) 0.05702(14) 0.0257(8) Uani 1 1 d . . . O7 O -0.3115(3) 0.4312(2) 0.13688(15) 0.0324(9) Uani 1 1 d . . . O8A O -0.3120(6) 0.4216(4) 0.2375(3) 0.036(2) Uani 0.631(16) 1 d P C 1 O8B O -0.3129(10) 0.4763(7) 0.2370(4) 0.034(4) Uani 0.369(16) 1 d P C 2 O9 O -0.1290(4) 0.3964(3) 0.29186(17) 0.0445(12) Uani 1 1 d . . . O10 O 0.0107(4) 0.2862(2) 0.27177(17) 0.0374(10) Uani 1 1 d . . . O11 O 1.0376(5) 0.4601(4) 0.6251(3) 0.075(2) Uani 1 1 d . . . O12 O 0.8929(8) 0.4185(3) 0.5664(3) 0.096(3) Uani 1 1 d . . . O13 O 0.9158(5) 0.5356(3) 0.5823(2) 0.0530(14) Uani 1 1 d . . . O14 O 0.4951(14) 0.5403(5) 0.6087(5) 0.177(7) Uani 1 1 d . . . O15 O 0.3989(7) 0.6309(7) 0.6166(4) 0.153(5) Uani 1 1 d . . . O16 O 0.5327(7) 0.6250(7) 0.5586(3) 0.132(5) Uani 1 1 d . . . O17 O 0.2700(10) 0.8878(6) 0.6063(6) 0.174(6) Uani 1 1 d U . . O18 O 0.4092(10) 0.9653(5) 0.6251(5) 0.166(5) Uani 1 1 d U . . O19 O 0.3062(10) 0.9209(8) 0.6870(6) 0.175(5) Uani 1 1 d U . . O20 O 0.5733(11) 0.2764(6) 0.2388(5) 0.138(5) Uani 1 1 d . . . O21 O 0.6769(17) 0.2301(10) 0.1925(6) 0.303(16) Uani 1 1 d . . . O22 O 0.8614(7) 0.2798(4) 0.5000(3) 0.082(2) Uani 1 1 d . . . O23 O 0.8577(6) 0.3432(4) 0.4393(3) 0.078(2) Uani 1 1 d . . . F1 F 0.8455(7) 0.4050(4) 0.6670(3) 0.110(3) Uani 1 1 d . . . F2 F 0.7315(5) 0.4708(4) 0.6280(3) 0.093(2) Uani 1 1 d . . . F3 F 0.8563(4) 0.5087(3) 0.6779(2) 0.0719(16) Uani 1 1 d . . . F4 F 0.5957(9) 0.6119(6) 0.6859(3) 0.177(6) Uani 1 1 d . . . F5 F 0.7046(5) 0.6241(4) 0.6309(3) 0.104(2) Uani 1 1 d . . . F6 F 0.5990(6) 0.6994(3) 0.6470(3) 0.094(2) Uani 1 1 d . . . F7 F 0.4795(11) 0.8479(7) 0.6070(3) 0.180(4) Uani 1 1 d U . . F8 F 0.3903(18) 0.8038(8) 0.6609(8) 0.279(8) Uani 1 1 d U . . F9 F 0.5095(14) 0.8798(9) 0.6802(4) 0.217(6) Uani 1 1 d U . . S1 S 0.9311(2) 0.46911(10) 0.59925(8) 0.0561(5) Uani 1 1 d . . . S2 S 0.49598(18) 0.60619(10) 0.60002(8) 0.0516(5) Uani 1 1 d . . . S3 S 0.3578(4) 0.90592(19) 0.63894(15) 0.1129(13) Uani 1 1 d DU . . Pd1 Pd 0.23476(4) 0.37683(2) 0.529939(17) 0.02862(14) Uani 1 1 d . . . C61 C 0.7360(16) 0.2608(9) 0.4359(7) 0.163(10) Uani 1 1 d . . . H61A H 0.6639 0.2825 0.4381 0.244 Uiso 1 1 calc R . . H61B H 0.7328 0.2170 0.4499 0.244 Uiso 1 1 calc R . . H61C H 0.7531 0.2573 0.4023 0.244 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 C1 0.023(3) 0.018(2) 0.038(3) -0.006(2) -0.004(2) 0.000(2) C2 0.018(2) 0.016(2) 0.026(3) -0.0095(19) -0.0022(19) -0.0010(18) C3 0.017(2) 0.017(2) 0.021(2) -0.0073(18) 0.0012(18) -0.0009(17) C4 0.021(2) 0.019(2) 0.025(3) -0.0049(19) 0.0029(19) -0.0019(19) C5 0.020(2) 0.024(3) 0.032(3) -0.003(2) 0.001(2) -0.002(2) C6 0.017(2) 0.026(3) 0.034(3) -0.005(2) -0.002(2) 0.002(2) C7 0.019(2) 0.031(3) 0.032(3) -0.006(2) 0.001(2) 0.003(2) C8 0.022(2) 0.020(2) 0.019(2) -0.0068(18) -0.0010(18) 0.0017(19) C9 0.020(2) 0.021(2) 0.016(2) -0.0087(18) 0.0013(18) 0.0013(18) C10 0.020(2) 0.025(3) 0.032(3) -0.003(2) 0.002(2) 0.003(2) C11 0.021(3) 0.027(3) 0.039(3) -0.001(2) 0.002(2) 0.006(2) C12 0.023(2) 0.025(2) 0.021(2) -0.004(2) 0.000(2) 0.001(2) C13 0.028(3) 0.027(3) 0.023(3) -0.003(2) -0.002(2) 0.003(2) C14 0.022(2) 0.034(3) 0.016(2) -0.008(2) 0.0021(19) -0.006(2) C15 0.036(3) 0.037(3) 0.020(3) 0.008(2) 0.003(2) -0.002(3) C16 0.036(3) 0.026(3) 0.018(2) 0.010(2) 0.001(2) -0.004(2) C17 0.032(3) 0.036(3) 0.022(3) 0.012(2) 0.006(2) 0.000(2) C18 0.030(3) 0.028(3) 0.029(3) 0.015(2) 0.002(2) -0.002(2) C19 0.031(3) 0.018(2) 0.027(3) 0.012(2) 0.000(2) -0.004(2) C20 0.031(3) 0.026(3) 0.033(3) 0.007(2) 0.006(2) -0.002(2) C21 0.027(3) 0.026(3) 0.029(3) 0.006(2) 0.003(2) -0.003(2) C22 0.029(3) 0.021(2) 0.030(3) 0.013(2) 0.002(2) -0.004(2) C23 0.031(3) 0.021(3) 0.040(3) 0.012(2) -0.008(2) -0.003(2) C24 0.030(3) 0.026(3) 0.036(3) 0.011(2) 0.001(2) -0.003(2) C25 0.031(3) 0.019(2) 0.037(3) 0.005(2) -0.005(2) 0.000(2) C26 0.027(3) 0.031(3) 0.037(3) 0.008(2) -0.002(2) -0.004(2) C27 0.059(5) 0.031(3) 0.044(4) 0.003(3) -0.005(3) -0.019(3) C28 0.057(4) 0.020(3) 0.051(4) 0.003(3) -0.001(3) -0.010(3) C29 0.039(3) 0.038(3) 0.029(3) 0.010(3) -0.007(3) -0.007(3) C30 0.035(3) 0.033(3) 0.031(3) 0.015(2) -0.005(2) -0.001(2) C31 0.033(3) 0.035(3) 0.033(3) 0.019(3) -0.010(2) -0.009(3) C32 0.034(3) 0.033(3) 0.034(3) 0.017(3) -0.007(2) -0.007(2) C33 0.034(3) 0.035(3) 0.028(3) 0.012(2) -0.003(2) -0.006(3) C34 0.030(3) 0.045(4) 0.028(3) 0.011(3) -0.005(2) -0.007(3) C35 0.036(3) 0.043(4) 0.041(4) 0.010(3) -0.002(3) -0.002(3) C36 0.038(4) 0.042(4) 0.051(4) 0.007(3) -0.003(3) 0.005(3) C37 0.041(4) 0.031(3) 0.046(4) 0.000(3) 0.005(3) 0.013(3) C38 0.031(3) 0.039(4) 0.052(4) 0.005(3) 0.003(3) 0.012(3) C39 0.025(3) 0.036(3) 0.055(4) -0.002(3) -0.002(3) 0.003(2) C40 0.025(3) 0.035(3) 0.059(4) -0.001(3) 0.009(3) 0.002(2) C41 0.025(3) 0.028(3) 0.032(3) 0.002(2) 0.005(2) -0.004(2) C42 0.024(2) 0.020(2) 0.028(3) -0.002(2) -0.002(2) -0.004(2) C43 0.022(2) 0.017(2) 0.019(2) 0.0014(18) 0.0027(18) -0.0011(18) C44 0.030(3) 0.017(2) 0.024(3) -0.0041(19) 0.002(2) -0.001(2) C45 0.026(3) 0.021(2) 0.025(3) -0.001(2) 0.001(2) -0.008(2) C46 0.020(2) 0.023(2) 0.017(2) -0.0010(18) 0.0027(18) 0.0014(19) C47 0.028(3) 0.019(2) 0.017(2) 0.0003(18) 0.0032(19) 0.0019(19) C48 0.027(3) 0.016(2) 0.020(2) -0.0021(18) 0.0020(19) -0.0027(19) C49 0.027(3) 0.029(3) 0.020(2) -0.009(2) -0.001(2) 0.002(2) C50 0.023(3) 0.032(3) 0.026(3) -0.005(2) -0.002(2) 0.006(2) C51 0.022(3) 0.079(6) 0.041(4) 0.012(4) 0.005(3) -0.002(3) C52 0.017(3) 0.224(15) 0.040(4) -0.024(7) 0.007(3) -0.004(6) C53 0.090(7) 0.108(8) 0.043(5) 0.031(5) 0.043(5) 0.059(6) C54 0.045(4) 0.130(9) 0.028(4) -0.006(5) 0.012(3) 0.009(5) C55 0.042(4) 0.087(6) 0.026(3) 0.004(4) 0.002(3) -0.003(4) C56 0.040(3) 0.053(4) 0.020(3) 0.007(3) -0.002(2) -0.004(3) C57 0.048(5) 0.061(6) 0.084(7) 0.036(5) -0.023(4) -0.017(4) C58 0.072(6) 0.068(6) 0.047(5) 0.012(4) -0.009(4) -0.027(5) C59 0.139(11) 0.153(9) 0.099(8) 0.063(7) 0.030(6) 0.011(6) C60 0.066(8) 0.102(11) 0.24(2) 0.007(13) -0.039(11) -0.018(8) N1 0.025(2) 0.018(2) 0.034(3) 0.0000(18) -0.0010(19) -0.0027(17) N2 0.030(2) 0.030(2) 0.0139(19) 0.0018(17) 0.0031(17) -0.0026(19) N3 0.027(2) 0.021(2) 0.036(3) 0.0102(19) -0.001(2) -0.0052(18) N4 0.048(3) 0.026(3) 0.037(3) 0.008(2) -0.006(2) -0.017(2) N5 0.038(3) 0.027(3) 0.036(3) -0.001(2) -0.001(2) -0.006(2) N6 0.132(10) 0.124(10) 0.087(7) -0.038(7) 0.060(8) -0.101(9) N7 0.066(5) 0.046(4) 0.068(5) 0.012(4) 0.016(4) 0.002(3) O1 0.035(2) 0.037(3) 0.043(3) 0.007(2) 0.000(2) -0.0051(19) O2 0.032(2) 0.041(3) 0.044(3) -0.001(2) -0.0005(19) 0.008(2) O3 0.035(2) 0.030(2) 0.054(3) 0.003(2) -0.005(2) 0.0106(19) O4 0.0233(19) 0.028(2) 0.040(2) 0.0030(17) 0.0030(17) 0.0036(16) O5 0.0229(18) 0.0202(18) 0.032(2) -0.0066(15) 0.0048(15) -0.0020(14) O6 0.0213(18) 0.032(2) 0.0242(19) -0.0096(16) 0.0022(15) 0.0007(15) O7 0.0202(19) 0.045(3) 0.032(2) 0.0032(19) 0.0043(16) 0.0037(17) O8A 0.032(4) 0.044(5) 0.032(4) 0.001(3) 0.006(3) 0.011(3) O8B 0.035(7) 0.043(9) 0.023(6) 0.001(5) 0.003(5) -0.013(5) O9 0.048(3) 0.058(3) 0.030(2) 0.010(2) 0.016(2) 0.007(2) O10 0.029(2) 0.042(3) 0.039(2) 0.011(2) -0.0078(18) -0.0034(19) O11 0.051(4) 0.087(5) 0.088(5) 0.041(4) 0.007(3) 0.029(3) O12 0.153(8) 0.047(4) 0.082(5) -0.016(4) -0.031(5) 0.040(4) O13 0.058(3) 0.039(3) 0.060(3) 0.018(3) -0.008(3) 0.004(2) O14 0.267(16) 0.060(6) 0.185(12) 0.005(7) -0.133(12) -0.012(8) O15 0.048(5) 0.265(16) 0.150(10) -0.048(10) 0.044(5) -0.044(7) O16 0.083(5) 0.269(14) 0.045(4) -0.027(6) 0.016(4) -0.094(7) O17 0.130(8) 0.108(8) 0.271(13) -0.086(10) -0.084(9) 0.012(6) O18 0.131(8) 0.114(6) 0.242(13) 0.109(8) -0.082(7) -0.065(5) O19 0.108(9) 0.219(14) 0.204(10) -0.078(10) 0.051(8) -0.017(9) O20 0.135(10) 0.092(8) 0.180(13) 0.021(8) -0.040(9) -0.042(7) O21 0.35(2) 0.36(3) 0.219(16) -0.209(18) 0.216(17) -0.31(2) O22 0.096(6) 0.081(5) 0.069(5) 0.031(4) 0.004(4) 0.004(4) O23 0.063(4) 0.066(4) 0.107(6) 0.040(4) 0.013(4) 0.002(3) F1 0.117(6) 0.081(5) 0.127(6) 0.064(4) -0.037(5) -0.035(4) F2 0.053(3) 0.104(5) 0.117(5) 0.030(4) -0.039(3) -0.025(3) F3 0.057(3) 0.098(4) 0.059(3) 0.007(3) -0.014(2) -0.002(3) F4 0.174(9) 0.264(13) 0.084(5) 0.085(7) -0.049(6) -0.137(9) F5 0.050(3) 0.144(7) 0.114(6) -0.002(5) -0.024(3) -0.001(4) F6 0.109(5) 0.072(4) 0.099(5) -0.033(4) -0.003(4) -0.014(4) F7 0.203(9) 0.262(11) 0.079(5) 0.005(7) 0.051(6) 0.031(8) F8 0.35(2) 0.177(11) 0.33(2) 0.102(13) 0.135(15) -0.046(10) F9 0.250(13) 0.303(18) 0.093(7) -0.015(9) -0.023(8) 0.016(11) S1 0.0679(13) 0.0382(10) 0.0602(12) 0.0092(9) -0.0101(10) 0.0173(9) S2 0.0510(11) 0.0405(10) 0.0624(13) -0.0082(9) -0.0044(9) -0.0088(8) S3 0.153(3) 0.082(2) 0.103(3) 0.0221(19) 0.007(2) -0.059(2) Pd1 0.0282(2) 0.0218(2) 0.0353(3) 0.00348(18) -0.00249(17) -0.00758(17) C61 0.177(17) 0.140(15) 0.156(16) 0.053(13) -0.100(14) -0.090(14) _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 N1 1.349(7) . ? C1 C2 1.381(8) . ? C2 C3 1.407(7) . ? C2 C6 1.447(7) . ? C3 C9 1.411(7) . ? C3 C4 1.415(7) . ? C4 C5 1.388(8) . ? C4 C10 1.435(7) . ? C5 N1 1.344(7) . ? C6 C7 1.347(8) . ? C7 C8 1.436(7) . ? C8 C14 1.387(8) . ? C8 C9 1.416(7) . ? C9 C12 1.410(7) . ? C10 C11 1.341(8) . ? C11 C12 1.448(8) . ? C12 C13 1.379(8) . ? C13 N2 1.351(7) . ? C14 N2 1.349(7) . ? C15 N2 1.497(7) . ? C15 C16 1.507(8) . ? C16 C17 1.384(8) . ? C16 C21 1.401(8) . ? C17 C18 1.396(9) . ? C18 C19 1.382(9) . ? C19 C20 1.392(8) . ? C19 C22 1.482(8) . ? C20 C21 1.369(9) . ? C22 C23 1.389(9) . ? C22 C24 1.396(8) . ? C23 C25 1.369(9) . ? C24 C26 1.382(9) . ? C25 N3 1.333(7) . ? C26 N3 1.338(8) . ? C27 C28 1.477(11) . ? C27 N4 1.487(8) . ? C28 N5 1.501(8) . ? C29 C34 1.380(10) . ? C29 C30 1.384(9) . ? C30 O10 1.374(8) . ? C30 C31 1.384(9) . ? C31 C32 1.365(10) . ? C32 C33 1.404(9) . ? C33 O1 1.359(8) . ? C33 C34 1.387(9) . ? C35 O1 1.431(8) . ? C35 C36 1.482(11) . ? C36 O2 1.418(9) . ? C37 O2 1.434(8) . ? C37 C38 1.486(10) . ? C38 O3 1.422(8) . ? C39 O3 1.424(8) . ? C39 C40 1.482(10) . ? C40 O4 1.413(7) . ? C41 O4 1.416(7) . ? C41 C42 1.495(8) . ? C42 O5 1.424(6) . ? C43 O5 1.376(6) . ? C43 C48 1.379(7) . ? C43 C44 1.403(7) . ? C44 C45 1.377(8) . ? C45 C46 1.387(7) . ? C46 O6 1.369(6) . ? C46 C47 1.381(7) . ? C47 C48 1.399(7) . ? C49 O6 1.428(6) . ? C49 C50 1.504(8) . ? C50 O7 1.410(7) . ? C51 O7 1.425(8) . ? C51 C52 1.455(13) . ? C52 O8B 1.380(14) . ? C52 O8A 1.547(13) . ? C53 O8A 1.325(12) . ? C53 O8B 1.366(14) . ? C53 C54 1.436(13) . ? C54 O9 1.406(9) . ? C55 O9 1.428(9) . ? C55 C56 1.482(10) . ? C56 O10 1.428(8) . ? C57 F3 1.297(12) . ? C57 F1 1.334(10) . ? C57 F2 1.346(10) . ? C57 S1 1.788(11) . ? C58 F4 1.266(11) . ? C58 F6 1.314(12) . ? C58 F5 1.347(13) . ? C58 S2 1.814(9) . ? C59 F8 1.104(19) . ? C59 F7 1.202(17) . ? C59 F9 1.46(2) . ? C59 S3 1.638(14) . ? C60 N6 1.46(2) . ? N1 Pd1 2.032(5) . ? N3 Pd1 2.019(5) 3_556 ? N4 Pd1 2.024(5) . ? N5 Pd1 2.026(5) . ? N6 O21 1.052(14) . ? N6 O20 1.238(17) . ? N7 O22 1.214(10) . ? N7 O23 1.215(9) . ? N7 C61 1.429(15) . ? O11 S1 1.443(7) . ? O12 S1 1.442(8) . ? O13 S1 1.451(5) . ? O14 S2 1.372(10) . ? O15 S2 1.380(10) . ? O16 S2 1.327(8) . ? O17 S3 1.401(11) . ? O18 S3 1.429(9) . ? O19 S3 1.551(14) . ? F7 S3 2.126(13) . ? Pd1 N3 2.019(5) 3_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 122.1(5) . . ? C1 C2 C3 118.2(5) . . ? C1 C2 C6 122.9(5) . . ? C3 C2 C6 118.9(5) . . ? C2 C3 C9 120.5(5) . . ? C2 C3 C4 119.7(5) . . ? C9 C3 C4 119.8(5) . . ? C5 C4 C3 117.6(5) . . ? C5 C4 C10 122.9(5) . . ? C3 C4 C10 119.5(5) . . ? N1 C5 C4 122.3(5) . . ? C7 C6 C2 120.8(5) . . ? C6 C7 C8 120.7(5) . . ? C14 C8 C9 117.8(5) . . ? C14 C8 C7 122.6(5) . . ? C9 C8 C7 119.6(5) . . ? C12 C9 C3 119.9(5) . . ? C12 C9 C8 120.6(5) . . ? C3 C9 C8 119.5(5) . . ? C11 C10 C4 120.9(5) . . ? C10 C11 C12 120.7(5) . . ? C13 C12 C9 117.8(5) . . ? C13 C12 C11 122.9(5) . . ? C9 C12 C11 119.2(5) . . ? N2 C13 C12 120.9(5) . . ? N2 C14 C8 120.4(5) . . ? N2 C15 C16 110.6(4) . . ? C17 C16 C21 119.2(6) . . ? C17 C16 C15 120.5(6) . . ? C21 C16 C15 120.4(5) . . ? C16 C17 C18 120.3(6) . . ? C19 C18 C17 120.1(6) . . ? C18 C19 C20 119.4(6) . . ? C18 C19 C22 121.4(5) . . ? C20 C19 C22 119.2(6) . . ? C21 C20 C19 120.8(6) . . ? C20 C21 C16 120.2(5) . . ? C23 C22 C24 116.7(6) . . ? C23 C22 C19 120.7(5) . . ? C24 C22 C19 122.6(6) . . ? C25 C23 C22 120.5(5) . . ? C26 C24 C22 120.2(6) . . ? N3 C25 C23 121.7(6) . . ? N3 C26 C24 121.2(6) . . ? C28 C27 N4 108.4(6) . . ? C27 C28 N5 107.7(6) . . ? C34 C29 C30 120.4(6) . . ? O10 C30 C31 116.9(6) . . ? O10 C30 C29 124.0(6) . . ? C31 C30 C29 119.1(7) . . ? C32 C31 C30 120.8(6) . . ? C31 C32 C33 120.7(6) . . ? O1 C33 C34 125.7(6) . . ? O1 C33 C32 116.1(6) . . ? C34 C33 C32 118.2(6) . . ? C29 C34 C33 120.8(6) . . ? O1 C35 C36 109.3(6) . . ? O2 C36 C35 108.3(6) . . ? O2 C37 C38 112.9(6) . . ? O3 C38 C37 109.1(5) . . ? O3 C39 C40 110.2(5) . . ? O4 C40 C39 110.1(6) . . ? O4 C41 C42 109.8(5) . . ? O5 C42 C41 106.9(4) . . ? O5 C43 C48 125.3(5) . . ? O5 C43 C44 115.0(4) . . ? C48 C43 C44 119.7(5) . . ? C45 C44 C43 119.9(5) . . ? C44 C45 C46 120.6(5) . . ? O6 C46 C47 124.7(5) . . ? O6 C46 C45 115.6(5) . . ? C47 C46 C45 119.7(5) . . ? C46 C47 C48 120.1(5) . . ? C43 C48 C47 120.0(5) . . ? O6 C49 C50 107.9(5) . . ? O7 C50 C49 108.0(4) . . ? O7 C51 C52 113.1(7) . . ? O8B C52 C51 128.7(9) . . ? O8B C52 O8A 44.6(7) . . ? C51 C52 O8A 100.9(9) . . ? O8A C53 O8B 49.2(7) . . ? O8A C53 C54 113.1(8) . . ? O8B C53 C54 138.7(10) . . ? O9 C54 C53 114.2(6) . . ? O9 C55 C56 110.3(5) . . ? O10 C56 C55 108.9(6) . . ? F3 C57 F1 109.4(8) . . ? F3 C57 F2 107.4(9) . . ? F1 C57 F2 107.9(7) . . ? F3 C57 S1 111.5(6) . . ? F1 C57 S1 110.4(9) . . ? F2 C57 S1 110.1(7) . . ? F4 C58 F6 108.9(11) . . ? F4 C58 F5 107.0(10) . . ? F6 C58 F5 101.9(8) . . ? F4 C58 S2 115.7(7) . . ? F6 C58 S2 110.8(7) . . ? F5 C58 S2 111.6(7) . . ? F8 C59 F7 132(3) . . ? F8 C59 F9 114(2) . . ? F7 C59 F9 108.2(18) . . ? F8 C59 S3 105.7(16) . . ? F7 C59 S3 95.7(11) . . ? F9 C59 S3 88.4(13) . . ? C5 N1 C1 120.0(5) . . ? C5 N1 Pd1 120.3(4) . . ? C1 N1 Pd1 119.3(4) . . ? C14 N2 C13 122.4(5) . . ? C14 N2 C15 117.9(5) . . ? C13 N2 C15 119.6(5) . . ? C25 N3 C26 119.6(6) . . ? C25 N3 Pd1 115.6(4) . 3_556 ? C26 N3 Pd1 124.6(4) . 3_556 ? C27 N4 Pd1 109.8(4) . . ? C28 N5 Pd1 107.0(4) . . ? O21 N6 O20 131(2) . . ? O21 N6 C60 119(2) . . ? O20 N6 C60 109.4(13) . . ? O22 N7 O23 123.3(9) . . ? O22 N7 C61 121.1(10) . . ? O23 N7 C61 115.0(10) . . ? C33 O1 C35 116.4(5) . . ? C36 O2 C37 114.6(5) . . ? C38 O3 C39 111.2(5) . . ? C40 O4 C41 110.3(5) . . ? C43 O5 C42 115.7(4) . . ? C46 O6 C49 116.8(4) . . ? C50 O7 C51 112.5(5) . . ? C53 O8A C52 106.9(7) . . ? C53 O8B C52 114.6(11) . . ? C54 O9 C55 111.3(6) . . ? C30 O10 C56 117.8(5) . . ? C59 F7 S3 50.0(8) . . ? O12 S1 O11 117.7(5) . . ? O12 S1 O13 115.9(4) . . ? O11 S1 O13 112.0(4) . . ? O12 S1 C57 103.4(6) . . ? O11 S1 C57 101.8(4) . . ? O13 S1 C57 103.2(4) . . ? O16 S2 O14 116.7(10) . . ? O16 S2 O15 121.6(9) . . ? O14 S2 O15 106.5(10) . . ? O16 S2 C58 104.4(5) . . ? O14 S2 C58 102.5(6) . . ? O15 S2 C58 102.3(6) . . ? O17 S3 O18 111.7(9) . . ? O17 S3 O19 107.0(9) . . ? O18 S3 O19 105.8(10) . . ? O17 S3 C59 106.6(10) . . ? O18 S3 C59 115.7(9) . . ? O19 S3 C59 109.7(9) . . ? O17 S3 F7 95.0(7) . . ? O18 S3 F7 92.3(8) . . ? O19 S3 F7 143.2(8) . . ? C59 S3 F7 34.2(6) . . ? N3 Pd1 N4 92.7(2) 3_556 . ? N3 Pd1 N5 175.2(2) 3_556 . ? N4 Pd1 N5 84.0(2) . . ? N3 Pd1 N1 87.54(19) 3_556 . ? N4 Pd1 N1 178.6(2) . . ? N5 Pd1 N1 95.7(2) . . ? 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 N1 C1 C2 C3 0.5(8) . . . . ? N1 C1 C2 C6 179.9(5) . . . . ? C1 C2 C3 C9 -179.2(5) . . . . ? C6 C2 C3 C9 1.4(7) . . . . ? C1 C2 C3 C4 -0.3(7) . . . . ? C6 C2 C3 C4 -179.7(5) . . . . ? C2 C3 C4 C5 -0.1(7) . . . . ? C9 C3 C4 C5 178.8(5) . . . . ? C2 C3 C4 C10 -178.2(5) . . . . ? C9 C3 C4 C10 0.7(7) . . . . ? C3 C4 C5 N1 0.5(8) . . . . ? C10 C4 C5 N1 178.5(5) . . . . ? C1 C2 C6 C7 179.1(5) . . . . ? C3 C2 C6 C7 -1.5(8) . . . . ? C2 C6 C7 C8 0.7(8) . . . . ? C6 C7 C8 C14 -179.9(5) . . . . ? C6 C7 C8 C9 0.3(8) . . . . ? C2 C3 C9 C12 179.6(5) . . . . ? C4 C3 C9 C12 0.7(7) . . . . ? C2 C3 C9 C8 -0.4(7) . . . . ? C4 C3 C9 C8 -179.3(5) . . . . ? C14 C8 C9 C12 -0.2(7) . . . . ? C7 C8 C9 C12 179.5(5) . . . . ? C14 C8 C9 C3 179.8(5) . . . . ? C7 C8 C9 C3 -0.5(7) . . . . ? C5 C4 C10 C11 -179.7(6) . . . . ? C3 C4 C10 C11 -1.7(8) . . . . ? C4 C10 C11 C12 1.2(9) . . . . ? C3 C9 C12 C13 -179.5(5) . . . . ? C8 C9 C12 C13 0.5(7) . . . . ? C3 C9 C12 C11 -1.2(7) . . . . ? C8 C9 C12 C11 178.8(5) . . . . ? C10 C11 C12 C13 178.5(6) . . . . ? C10 C11 C12 C9 0.2(8) . . . . ? C9 C12 C13 N2 -0.9(8) . . . . ? C11 C12 C13 N2 -179.2(5) . . . . ? C9 C8 C14 N2 0.4(7) . . . . ? C7 C8 C14 N2 -179.3(5) . . . . ? N2 C15 C16 C17 -116.1(6) . . . . ? N2 C15 C16 C21 64.2(7) . . . . ? C21 C16 C17 C18 0.0(8) . . . . ? C15 C16 C17 C18 -179.7(5) . . . . ? C16 C17 C18 C19 -1.3(8) . . . . ? C17 C18 C19 C20 1.6(8) . . . . ? C17 C18 C19 C22 -179.1(5) . . . . ? C18 C19 C20 C21 -0.6(8) . . . . ? C22 C19 C20 C21 -179.9(5) . . . . ? C19 C20 C21 C16 -0.7(9) . . . . ? C17 C16 C21 C20 1.0(8) . . . . ? C15 C16 C21 C20 -179.3(5) . . . . ? C18 C19 C22 C23 -147.8(6) . . . . ? C20 C19 C22 C23 31.5(8) . . . . ? C18 C19 C22 C24 34.3(8) . . . . ? C20 C19 C22 C24 -146.4(6) . . . . ? C24 C22 C23 C25 -0.1(8) . . . . ? C19 C22 C23 C25 -178.1(5) . . . . ? C23 C22 C24 C26 -1.4(8) . . . . ? C19 C22 C24 C26 176.6(5) . . . . ? C22 C23 C25 N3 2.3(9) . . . . ? C22 C24 C26 N3 0.8(9) . . . . ? N4 C27 C28 N5 52.3(8) . . . . ? C34 C29 C30 O10 179.4(5) . . . . ? C34 C29 C30 C31 -0.9(9) . . . . ? O10 C30 C31 C32 179.9(5) . . . . ? C29 C30 C31 C32 0.2(9) . . . . ? C30 C31 C32 C33 0.4(9) . . . . ? C31 C32 C33 O1 -179.8(5) . . . . ? C31 C32 C33 C34 -0.3(9) . . . . ? C30 C29 C34 C33 1.1(9) . . . . ? O1 C33 C34 C29 179.0(6) . . . . ? C32 C33 C34 C29 -0.4(9) . . . . ? O1 C35 C36 O2 64.5(7) . . . . ? O2 C37 C38 O3 -69.6(8) . . . . ? O3 C39 C40 O4 70.4(7) . . . . ? O4 C41 C42 O5 -72.4(6) . . . . ? O5 C43 C44 C45 -180.0(5) . . . . ? C48 C43 C44 C45 -0.9(8) . . . . ? C43 C44 C45 C46 0.2(8) . . . . ? C44 C45 C46 O6 -179.6(5) . . . . ? C44 C45 C46 C47 0.8(8) . . . . ? O6 C46 C47 C48 179.4(5) . . . . ? C45 C46 C47 C48 -1.1(8) . . . . ? O5 C43 C48 C47 179.6(5) . . . . ? C44 C43 C48 C47 0.6(8) . . . . ? C46 C47 C48 C43 0.4(8) . . . . ? O6 C49 C50 O7 67.3(5) . . . . ? O7 C51 C52 O8B -31.0(19) . . . . ? O7 C51 C52 O8A -70.2(10) . . . . ? O8A C53 C54 O9 35.4(15) . . . . ? O8B C53 C54 O9 -18(2) . . . . ? O9 C55 C56 O10 -70.5(8) . . . . ? C4 C5 N1 C1 -0.3(8) . . . . ? C4 C5 N1 Pd1 -173.2(4) . . . . ? C2 C1 N1 C5 -0.2(8) . . . . ? C2 C1 N1 Pd1 172.8(4) . . . . ? C8 C14 N2 C13 -0.9(8) . . . . ? C8 C14 N2 C15 -176.9(5) . . . . ? C12 C13 N2 C14 1.2(8) . . . . ? C12 C13 N2 C15 177.1(5) . . . . ? C16 C15 N2 C14 84.0(6) . . . . ? C16 C15 N2 C13 -92.1(6) . . . . ? C23 C25 N3 C26 -3.0(9) . . . . ? C23 C25 N3 Pd1 172.8(5) . . . 3_556 ? C24 C26 N3 C25 1.5(9) . . . . ? C24 C26 N3 Pd1 -174.0(4) . . . 3_556 ? C28 C27 N4 Pd1 -34.2(7) . . . . ? C27 C28 N5 Pd1 -45.0(6) . . . . ? C34 C33 O1 C35 -2.1(9) . . . . ? C32 C33 O1 C35 177.3(5) . . . . ? C36 C35 O1 C33 -170.9(5) . . . . ? C35 C36 O2 C37 148.6(6) . . . . ? C38 C37 O2 C36 -78.5(7) . . . . ? C37 C38 O3 C39 172.1(6) . . . . ? C40 C39 O3 C38 160.2(6) . . . . ? C39 C40 O4 C41 176.9(5) . . . . ? C42 C41 O4 C40 -178.9(5) . . . . ? C48 C43 O5 C42 -1.8(7) . . . . ? C44 C43 O5 C42 177.3(5) . . . . ? C41 C42 O5 C43 -177.6(4) . . . . ? C47 C46 O6 C49 -8.3(7) . . . . ? C45 C46 O6 C49 172.1(5) . . . . ? C50 C49 O6 C46 -160.2(4) . . . . ? C49 C50 O7 C51 169.6(5) . . . . ? C52 C51 O7 C50 -89.7(9) . . . . ? O8B C53 O8A C52 -45.8(9) . . . . ? C54 C53 O8A C52 178.9(10) . . . . ? O8B C52 O8A C53 50.0(10) . . . . ? C51 C52 O8A C53 -174.7(9) . . . . ? O8A C53 O8B C52 57.8(11) . . . . ? C54 C53 O8B C52 136.4(17) . . . . ? C51 C52 O8B C53 -113.6(15) . . . . ? O8A C52 O8B C53 -51.4(9) . . . . ? C53 C54 O9 C55 -178.3(10) . . . . ? C56 C55 O9 C54 176.3(8) . . . . ? C31 C30 O10 C56 177.6(5) . . . . ? C29 C30 O10 C56 -2.8(8) . . . . ? C55 C56 O10 C30 -171.3(5) . . . . ? F8 C59 F7 S3 117(3) . . . . ? F9 C59 F7 S3 -90.2(15) . . . . ? F3 C57 S1 O12 -176.4(6) . . . . ? F1 C57 S1 O12 61.7(7) . . . . ? F2 C57 S1 O12 -57.3(8) . . . . ? F3 C57 S1 O11 61.0(7) . . . . ? F1 C57 S1 O11 -60.9(8) . . . . ? F2 C57 S1 O11 -179.9(7) . . . . ? F3 C57 S1 O13 -55.3(7) . . . . ? F1 C57 S1 O13 -177.1(6) . . . . ? F2 C57 S1 O13 63.8(8) . . . . ? F4 C58 S2 O16 -166.2(12) . . . . ? F6 C58 S2 O16 69.2(10) . . . . ? F5 C58 S2 O16 -43.6(10) . . . . ? F4 C58 S2 O14 -44.1(14) . . . . ? F6 C58 S2 O14 -168.7(11) . . . . ? F5 C58 S2 O14 78.5(11) . . . . ? F4 C58 S2 O15 66.2(13) . . . . ? F6 C58 S2 O15 -58.4(10) . . . . ? F5 C58 S2 O15 -171.2(9) . . . . ? F8 C59 S3 O17 -63(2) . . . . ? F7 C59 S3 O17 73.9(17) . . . . ? F9 C59 S3 O17 -178.0(11) . . . . ? F8 C59 S3 O18 172.0(19) . . . . ? F7 C59 S3 O18 -51.0(19) . . . . ? F9 C59 S3 O18 57.1(13) . . . . ? F8 C59 S3 O19 52(2) . . . . ? F7 C59 S3 O19 -170.6(13) . . . . ? F9 C59 S3 O19 -62.4(12) . . . . ? F8 C59 S3 F7 -137(3) . . . . ? F9 C59 S3 F7 108.1(18) . . . . ? C59 F7 S3 O17 -112.5(18) . . . . ? C59 F7 S3 O18 135.5(17) . . . . ? C59 F7 S3 O19 15(2) . . . . ? C27 N4 Pd1 N3 -176.3(5) . . . 3_556 ? C27 N4 Pd1 N5 7.2(5) . . . . ? C27 N4 Pd1 N1 86(9) . . . . ? C28 N5 Pd1 N3 -25(3) . . . 3_556 ? C28 N5 Pd1 N4 20.6(5) . . . . ? C28 N5 Pd1 N1 -158.0(4) . . . . ? C5 N1 Pd1 N3 82.3(4) . . . 3_556 ? C1 N1 Pd1 N3 -90.6(4) . . . 3_556 ? C5 N1 Pd1 N4 -180(100) . . . . ? C1 N1 Pd1 N4 7(9) . . . . ? C5 N1 Pd1 N5 -101.1(5) . . . . ? C1 N1 Pd1 N5 85.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.935 _refine_diff_density_min -1.534 _refine_diff_density_rms 0.154 data_0852153_b2_0s _database_code_depnum_ccdc_archive 'CCDC 861118' #TrackingRef 'web_deposit_cif_file_0_CarlosPeinador_1323360296.Ligand1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H42 F24 N10 P4' _chemical_formula_weight 1506.94 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' _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 13.067(5) _cell_length_b 14.272(5) _cell_length_c 17.273(5) _cell_angle_alpha 67.392(5) _cell_angle_beta 77.696(5) _cell_angle_gamma 87.835(5) _cell_volume 2902.0(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6044 _cell_measurement_theta_min 4.338 _cell_measurement_theta_max 56.642 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.725 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 0.263 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9469 _exptl_absorpt_correction_T_max 0.9870 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48225 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.0829 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 28.44 _reflns_number_total 14379 _reflns_number_gt 8167 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1270P)^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 14379 _refine_ls_number_parameters 903 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1278 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.2228 _refine_ls_wR_factor_gt 0.1725 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.092 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.1468(3) 0.3806(3) 0.4986(3) 0.0280(9) Uani 1 1 d . . . H1 H 1.1519 0.4331 0.4434 0.034 Uiso 1 1 calc R . . C2 C 1.0468(3) 0.3404(3) 0.5464(2) 0.0237(8) Uani 1 1 d . . . C3 C 1.0413(3) 0.2625(3) 0.6280(2) 0.0226(8) Uani 1 1 d . . . C4 C 1.1352(3) 0.2283(3) 0.6566(3) 0.0259(8) Uani 1 1 d . . . C5 C 1.2286(3) 0.2757(3) 0.6012(3) 0.0300(9) Uani 1 1 d . . . H5 H 1.2920 0.2527 0.6193 0.036 Uiso 1 1 calc R . . C6 C 0.9513(3) 0.3719(3) 0.5172(2) 0.0217(8) Uani 1 1 d . . . H6 H 0.9547 0.4225 0.4614 0.026 Uiso 1 1 calc R . . C7 C 0.8568(3) 0.3312(3) 0.5675(2) 0.0206(8) Uani 1 1 d . . . H7 H 0.7947 0.3541 0.5472 0.025 Uiso 1 1 calc R . . C8 C 0.8502(3) 0.2534(3) 0.6516(2) 0.0184(7) Uani 1 1 d . . . C9 C 0.9432(3) 0.2196(3) 0.6811(2) 0.0206(8) Uani 1 1 d . . . C10 C 1.1275(3) 0.1479(3) 0.7389(3) 0.0284(9) Uani 1 1 d . . . H10 H 1.1899 0.1224 0.7577 0.034 Uiso 1 1 calc R . . C11 C 1.0344(3) 0.1077(3) 0.7901(3) 0.0293(9) Uani 1 1 d . . . H11 H 1.0319 0.0556 0.8451 0.035 Uiso 1 1 calc R . . C12 C 0.9380(3) 0.1421(3) 0.7629(2) 0.0223(8) Uani 1 1 d . . . C13 C 0.8404(3) 0.1033(3) 0.8134(2) 0.0248(8) Uani 1 1 d . . . H13 H 0.8349 0.0516 0.8690 0.030 Uiso 1 1 calc R . . C14 C 0.7555(3) 0.2104(3) 0.7051(2) 0.0202(7) Uani 1 1 d . . . H14 H 0.6922 0.2316 0.6863 0.024 Uiso 1 1 calc R . . C15 C 0.6482(3) 0.0954(3) 0.8400(2) 0.0254(8) Uani 1 1 d . . . H15A H 0.6130 0.0583 0.8141 0.030 Uiso 1 1 calc R . . H15B H 0.6567 0.0471 0.8972 0.030 Uiso 1 1 calc R . . C16 C 0.4878(3) 0.1867(3) 0.8312(2) 0.0232(8) Uani 1 1 d . . . H16 H 0.4623 0.1373 0.8146 0.028 Uiso 1 1 calc R . . C17 C 0.4256(3) 0.2663(3) 0.8372(2) 0.0239(8) Uani 1 1 d . . . C18 C 0.4662(3) 0.3370(3) 0.8619(2) 0.0187(7) Uani 1 1 d . . . C19 C 0.5670(3) 0.3279(3) 0.8814(2) 0.0196(7) Uani 1 1 d . . . C20 C 0.6239(3) 0.2463(3) 0.8751(2) 0.0202(7) Uani 1 1 d . . . H20 H 0.6910 0.2369 0.8891 0.024 Uiso 1 1 calc R . . C21 C 0.3235(3) 0.2777(3) 0.8173(3) 0.0318(9) Uani 1 1 d . . . H21 H 0.2957 0.2293 0.8009 0.038 Uiso 1 1 calc R . . C22 C 0.2668(3) 0.3574(3) 0.8217(3) 0.0316(10) Uani 1 1 d . . . H22 H 0.1997 0.3647 0.8079 0.038 Uiso 1 1 calc R . . C23 C 0.3062(3) 0.4312(3) 0.8470(2) 0.0236(8) Uani 1 1 d . . . C24 C 0.4064(3) 0.4204(3) 0.8667(2) 0.0212(8) Uani 1 1 d . . . C25 C 0.6076(3) 0.4023(3) 0.9043(2) 0.0224(8) Uani 1 1 d . . . H25 H 0.6751 0.3957 0.9175 0.027 Uiso 1 1 calc R . . C26 C 0.5505(3) 0.4832(3) 0.9075(2) 0.0234(8) Uani 1 1 d . . . H26 H 0.5792 0.5334 0.9215 0.028 Uiso 1 1 calc R . . C27 C 0.4474(3) 0.4928(3) 0.8899(2) 0.0231(8) Uani 1 1 d . . . C28 C 0.3840(3) 0.5737(3) 0.8929(2) 0.0262(8) Uani 1 1 d . . . H28 H 0.4105 0.6229 0.9092 0.031 Uiso 1 1 calc R . . C29 C 0.2516(3) 0.5152(3) 0.8522(2) 0.0283(9) Uani 1 1 d . . . H29 H 0.1838 0.5231 0.8393 0.034 Uiso 1 1 calc R . . C30 C 1.1508(3) -0.1483(3) 0.5034(2) 0.0226(8) Uani 1 1 d . . . H30 H 1.2251 -0.1425 0.4862 0.027 Uiso 1 1 calc R . . C31 C 1.0931(3) -0.0875(3) 0.4446(2) 0.0188(7) Uani 1 1 d . . . C32 C 0.9825(3) -0.0978(3) 0.4727(2) 0.0162(7) Uani 1 1 d . . . C33 C 0.9364(3) -0.1668(3) 0.5551(2) 0.0189(7) Uani 1 1 d . . . C34 C 1.0035(3) -0.2237(3) 0.6075(2) 0.0224(8) Uani 1 1 d . . . H34 H 0.9734 -0.2714 0.6633 0.027 Uiso 1 1 calc R . . C35 C 1.1382(3) -0.0165(3) 0.3607(2) 0.0214(8) Uani 1 1 d . . . H35 H 1.2124 -0.0094 0.3419 0.026 Uiso 1 1 calc R . . C36 C 0.8240(3) -0.1753(3) 0.5830(2) 0.0240(8) Uani 1 1 d . . . H36 H 0.7929 -0.2217 0.6391 0.029 Uiso 1 1 calc R . . C37 C 1.0778(3) 0.0411(3) 0.3071(2) 0.0214(8) Uani 1 1 d . . . H37 H 1.1094 0.0881 0.2513 0.026 Uiso 1 1 calc R . . C38 C 0.9653(3) 0.0307(3) 0.3352(2) 0.0183(7) Uani 1 1 d . . . C39 C 0.7622(3) -0.1185(3) 0.5311(2) 0.0228(8) Uani 1 1 d . . . H39 H 0.6882 -0.1254 0.5507 0.027 Uiso 1 1 calc R . . C40 C 0.9187(3) -0.0381(3) 0.4176(2) 0.0168(7) Uani 1 1 d . . . C41 C 0.8078(3) -0.0479(3) 0.4465(2) 0.0185(7) Uani 1 1 d . . . C42 C 0.7481(3) 0.0145(3) 0.3915(2) 0.0200(7) Uani 1 1 d . . . H42 H 0.6739 0.0105 0.4093 0.024 Uiso 1 1 calc R . . C43 C 0.9001(3) 0.0903(3) 0.2828(2) 0.0192(7) Uani 1 1 d . . . H43 H 0.9295 0.1373 0.2265 0.023 Uiso 1 1 calc R . . C44 C 0.7293(3) 0.1442(3) 0.2546(2) 0.0219(8) Uani 1 1 d . . . H44A H 0.6828 0.0998 0.2435 0.026 Uiso 1 1 calc R . . H44B H 0.7747 0.1870 0.1990 0.026 Uiso 1 1 calc R . . C45 C 0.5644(3) 0.2200(3) 0.2830(2) 0.0210(8) Uani 1 1 d . . . H45 H 0.5341 0.1764 0.2631 0.025 Uiso 1 1 calc R . . C46 C 0.5052(3) 0.2941(3) 0.3030(2) 0.0189(7) Uani 1 1 d . . . C47 C 0.5524(3) 0.3553(3) 0.3342(2) 0.0187(7) Uani 1 1 d . . . C48 C 0.6565(3) 0.3404(3) 0.3463(2) 0.0200(7) Uani 1 1 d . . . C49 C 0.7111(3) 0.2673(3) 0.3225(2) 0.0211(8) Uani 1 1 d . . . H49 H 0.7820 0.2573 0.3277 0.025 Uiso 1 1 calc R . . C50 C 0.4014(3) 0.3128(3) 0.2876(2) 0.0212(8) Uani 1 1 d . . . H50 H 0.3684 0.2698 0.2688 0.025 Uiso 1 1 calc R . . C51 C 0.3510(3) 0.3918(3) 0.2998(2) 0.0218(8) Uani 1 1 d . . . H51 H 0.2827 0.4045 0.2883 0.026 Uiso 1 1 calc R . . C52 C 0.3977(3) 0.4568(3) 0.3296(2) 0.0218(8) Uani 1 1 d . . . C53 C 0.4973(3) 0.4369(3) 0.3486(2) 0.0188(7) Uani 1 1 d . . . C54 C 0.7029(3) 0.4043(3) 0.3773(2) 0.0227(8) Uani 1 1 d . . . H54 H 0.7720 0.3933 0.3870 0.027 Uiso 1 1 calc R . . C55 C 0.6488(3) 0.4808(3) 0.3932(2) 0.0245(8) Uani 1 1 d . . . H55 H 0.6802 0.5218 0.4148 0.029 Uiso 1 1 calc R . . C56 C 0.5453(3) 0.5002(3) 0.3776(2) 0.0203(7) Uani 1 1 d . . . C57 C 0.4883(3) 0.5826(3) 0.3858(2) 0.0250(8) Uani 1 1 d . . . H57 H 0.5181 0.6251 0.4070 0.030 Uiso 1 1 calc R . . C58 C 0.3514(3) 0.5439(3) 0.3385(2) 0.0232(8) Uani 1 1 d . . . H58 H 0.2849 0.5599 0.3243 0.028 Uiso 1 1 calc R . . C59 C 0.8907(4) 0.5939(4) 0.9361(4) 0.0600(16) Uani 1 1 d . . . H59A H 0.9102 0.5319 0.9793 0.090 Uiso 1 1 calc R . . H59B H 0.8394 0.5764 0.9093 0.090 Uiso 1 1 calc R . . H59C H 0.8600 0.6400 0.9638 0.090 Uiso 1 1 calc R . . C60 C 0.9820(4) 0.6427(4) 0.8720(3) 0.0397(11) Uani 1 1 d . . . C61 C 0.9700(5) 0.7952(6) 1.0480(4) 0.082(2) Uani 1 1 d . . . H61A H 0.9849 0.7233 1.0627 0.123 Uiso 1 1 calc R . . H61B H 0.9071 0.8013 1.0879 0.123 Uiso 1 1 calc R . . H61C H 1.0297 0.8315 1.0519 0.123 Uiso 1 1 calc R . . C62 C 0.9537(4) 0.8373(4) 0.9643(3) 0.0453(12) Uani 1 1 d . . . N1 N 1.2358(3) 0.3503(3) 0.5253(2) 0.0335(8) Uani 1 1 d . . . N2 N 0.7523(2) 0.1379(2) 0.78444(19) 0.0218(7) Uani 1 1 d . . . N3 N 0.5843(2) 0.1798(2) 0.84892(18) 0.0207(6) Uani 1 1 d . . . N4 N 0.2892(2) 0.5859(3) 0.8745(2) 0.0292(8) Uani 1 1 d . . . N5 N 1.1083(2) -0.2138(2) 0.5820(2) 0.0238(7) Uani 1 1 d . . . N6 N 0.7952(2) 0.0810(2) 0.31255(18) 0.0175(6) Uani 1 1 d . . . N7 N 0.6648(2) 0.2102(2) 0.29188(18) 0.0186(6) Uani 1 1 d . . . N8 N 0.3948(2) 0.6050(2) 0.3655(2) 0.0260(7) Uani 1 1 d . . . N9 N 1.0554(3) 0.6825(3) 0.8215(3) 0.0502(11) Uani 1 1 d . . . N10 N 0.9403(3) 0.8700(4) 0.8959(3) 0.0604(13) Uani 1 1 d . . . F1 F 0.9187(2) 0.4492(2) 0.67854(16) 0.0429(7) Uani 1 1 d . . . F2 F 0.8579(2) 0.3619(2) 0.8188(2) 0.0606(9) Uani 1 1 d . . . F3 F 1.0277(2) 0.3573(2) 0.76108(17) 0.0420(7) Uani 1 1 d . . . F4 F 1.0421(2) 0.5283(2) 0.70829(19) 0.0544(8) Uani 1 1 d . . . F5 F 0.9836(2) 0.4415(2) 0.84835(17) 0.0485(7) Uani 1 1 d . . . F6 F 0.8726(2) 0.5333(2) 0.7665(2) 0.0528(8) Uani 1 1 d . . . F7 F 0.72990(19) -0.23738(19) 0.82409(16) 0.0372(6) Uani 1 1 d . . . F8 F 0.7065(2) -0.2462(2) 0.96047(16) 0.0499(7) Uani 1 1 d . . . F9 F 0.72638(18) -0.09281(18) 0.84830(17) 0.0385(6) Uani 1 1 d . . . F10 F 0.5913(2) -0.1377(2) 0.80671(19) 0.0549(8) Uani 1 1 d . . . F11 F 0.5713(2) -0.2885(2) 0.9168(2) 0.0597(9) Uani 1 1 d . . . F12 F 0.57135(19) -0.1438(2) 0.94199(17) 0.0423(7) Uani 1 1 d . . . F13 F 0.44708(19) 0.1520(2) 0.53387(16) 0.0430(7) Uani 1 1 d . . . F14 F 0.5906(2) 0.2272(2) 0.54478(16) 0.0412(6) Uani 1 1 d . . . F15 F 0.60672(18) 0.0874(2) 0.66033(17) 0.0405(6) Uani 1 1 d . . . F16 F 0.46492(18) 0.01127(19) 0.64902(16) 0.0384(6) Uani 1 1 d . . . F17 F 0.6003(2) 0.0737(2) 0.5344(2) 0.0556(8) Uani 1 1 d . . . F18 F 0.45404(19) 0.1660(2) 0.65858(16) 0.0404(6) Uani 1 1 d . . . F19 F 0.3321(2) 0.0149(2) 0.82858(16) 0.0498(7) Uani 1 1 d . . . F20 F 0.32832(19) -0.1524(2) 0.91505(18) 0.0444(7) Uani 1 1 d . . . F21 F 0.17869(18) -0.0764(2) 0.88603(15) 0.0380(6) Uani 1 1 d . . . F22 F 0.2117(2) -0.1226(2) 1.01905(16) 0.0528(8) Uani 1 1 d . . . F23 F 0.2144(3) 0.0428(3) 0.9331(2) 0.0707(10) Uani 1 1 d . . . F24 F 0.3657(2) -0.0307(2) 0.96140(17) 0.0483(7) Uani 1 1 d . . . P1 P 0.94991(7) 0.44477(8) 0.76402(6) 0.0228(2) Uani 1 1 d . . . P2 P 0.65000(8) -0.19109(8) 0.88351(7) 0.0268(2) Uani 1 1 d . . . P3 P 0.52776(7) 0.11965(8) 0.59645(7) 0.0243(2) Uani 1 1 d . . . P4 P 0.27245(9) -0.05431(9) 0.92399(7) 0.0312(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 0.0249(19) 0.028(2) 0.030(2) -0.0132(18) -0.0005(16) 0.0019(16) C2 0.033(2) 0.020(2) 0.0253(19) -0.0146(16) -0.0096(16) 0.0081(16) C3 0.0288(19) 0.0169(19) 0.031(2) -0.0162(16) -0.0113(16) 0.0044(15) C4 0.029(2) 0.020(2) 0.039(2) -0.0181(18) -0.0173(17) 0.0077(16) C5 0.0247(19) 0.028(2) 0.050(3) -0.025(2) -0.0136(18) 0.0075(17) C6 0.0283(19) 0.0192(19) 0.0189(17) -0.0082(15) -0.0063(14) 0.0034(15) C7 0.0253(18) 0.0204(19) 0.0195(17) -0.0099(15) -0.0084(14) 0.0067(15) C8 0.0264(18) 0.0140(18) 0.0186(17) -0.0096(14) -0.0070(14) 0.0040(14) C9 0.0268(19) 0.0160(19) 0.0231(18) -0.0104(15) -0.0091(15) 0.0049(15) C10 0.031(2) 0.018(2) 0.044(2) -0.0144(18) -0.0226(18) 0.0057(16) C11 0.043(2) 0.017(2) 0.036(2) -0.0098(17) -0.0271(19) 0.0098(17) C12 0.032(2) 0.0096(17) 0.030(2) -0.0090(15) -0.0144(16) 0.0042(15) C13 0.039(2) 0.0174(19) 0.0205(18) -0.0057(15) -0.0148(16) 0.0062(16) C14 0.0315(19) 0.0147(18) 0.0194(17) -0.0087(14) -0.0123(15) 0.0068(15) C15 0.032(2) 0.0168(19) 0.0224(19) -0.0038(15) -0.0037(16) 0.0006(16) C16 0.0263(19) 0.024(2) 0.0194(18) -0.0071(16) -0.0061(15) -0.0052(15) C17 0.0220(18) 0.025(2) 0.0217(18) -0.0043(16) -0.0054(14) -0.0051(15) C18 0.0207(17) 0.0174(18) 0.0131(16) -0.0012(14) -0.0016(13) -0.0033(14) C19 0.0195(17) 0.0203(19) 0.0159(17) -0.0034(14) -0.0034(13) -0.0024(14) C20 0.0233(17) 0.0179(19) 0.0184(17) -0.0044(15) -0.0072(14) -0.0003(14) C21 0.027(2) 0.037(3) 0.029(2) -0.0080(19) -0.0106(17) -0.0051(18) C22 0.0223(19) 0.038(3) 0.030(2) -0.0053(19) -0.0100(16) -0.0040(17) C23 0.0210(18) 0.024(2) 0.0199(18) -0.0026(15) -0.0015(14) -0.0017(15) C24 0.0209(17) 0.022(2) 0.0147(16) -0.0008(14) -0.0030(13) -0.0022(15) C25 0.0197(17) 0.026(2) 0.0224(18) -0.0090(16) -0.0058(14) -0.0005(15) C26 0.0237(18) 0.025(2) 0.0186(18) -0.0056(15) -0.0024(14) -0.0026(15) C27 0.0223(18) 0.024(2) 0.0155(17) -0.0009(15) -0.0004(14) -0.0015(15) C28 0.029(2) 0.026(2) 0.0174(18) -0.0035(16) -0.0011(15) 0.0019(16) C29 0.0208(18) 0.032(2) 0.0232(19) -0.0027(17) -0.0022(15) 0.0028(16) C30 0.0173(17) 0.027(2) 0.034(2) -0.0189(17) -0.0127(15) 0.0059(15) C31 0.0179(16) 0.0183(19) 0.0254(18) -0.0132(15) -0.0069(14) 0.0031(14) C32 0.0161(16) 0.0156(18) 0.0226(17) -0.0119(15) -0.0072(13) 0.0024(13) C33 0.0224(17) 0.0141(18) 0.0225(18) -0.0083(15) -0.0073(14) -0.0003(14) C34 0.0266(19) 0.0199(19) 0.0240(19) -0.0099(16) -0.0098(15) 0.0035(15) C35 0.0128(16) 0.029(2) 0.0256(19) -0.0148(16) -0.0017(14) -0.0004(14) C36 0.0235(18) 0.024(2) 0.0189(18) -0.0027(15) -0.0032(14) -0.0033(15) C37 0.0195(17) 0.024(2) 0.0210(18) -0.0114(16) 0.0001(14) 0.0005(15) C38 0.0132(15) 0.0219(19) 0.0208(17) -0.0095(15) -0.0033(13) 0.0022(13) C39 0.0155(16) 0.025(2) 0.0264(19) -0.0077(16) -0.0038(14) -0.0047(14) C40 0.0170(16) 0.0163(18) 0.0199(17) -0.0088(14) -0.0060(13) 0.0005(13) C41 0.0163(16) 0.0198(19) 0.0198(17) -0.0079(15) -0.0039(13) -0.0018(14) C42 0.0156(16) 0.022(2) 0.0232(18) -0.0097(15) -0.0040(14) -0.0003(14) C43 0.0197(17) 0.0186(19) 0.0203(17) -0.0097(15) -0.0020(13) 0.0019(14) C44 0.0237(18) 0.024(2) 0.0184(17) -0.0076(15) -0.0068(14) 0.0053(15) C45 0.0191(17) 0.022(2) 0.0181(17) -0.0033(15) -0.0056(14) -0.0010(14) C46 0.0164(16) 0.0166(18) 0.0174(17) 0.0005(14) -0.0035(13) -0.0015(13) C47 0.0178(16) 0.0181(18) 0.0151(16) -0.0003(14) -0.0042(13) -0.0011(14) C48 0.0195(17) 0.0188(19) 0.0190(17) -0.0033(15) -0.0058(14) -0.0008(14) C49 0.0190(17) 0.022(2) 0.0222(18) -0.0051(15) -0.0096(14) 0.0028(14) C50 0.0161(16) 0.024(2) 0.0219(18) -0.0072(16) -0.0036(14) -0.0042(14) C51 0.0148(16) 0.021(2) 0.0266(19) -0.0052(16) -0.0049(14) -0.0009(14) C52 0.0199(17) 0.0203(19) 0.0181(17) -0.0021(15) 0.0005(14) -0.0011(14) C53 0.0194(17) 0.0166(18) 0.0143(16) -0.0001(14) -0.0015(13) -0.0012(14) C54 0.0221(18) 0.023(2) 0.0235(19) -0.0060(16) -0.0120(15) 0.0015(15) C55 0.0270(19) 0.022(2) 0.0247(19) -0.0066(16) -0.0101(15) 0.0003(15) C56 0.0211(17) 0.0193(19) 0.0180(17) -0.0051(15) -0.0030(14) 0.0017(14) C57 0.029(2) 0.023(2) 0.0233(19) -0.0081(16) -0.0071(15) 0.0008(16) C58 0.0168(17) 0.021(2) 0.0267(19) -0.0043(16) -0.0035(14) 0.0035(14) C59 0.065(4) 0.048(3) 0.054(3) -0.019(3) 0.012(3) 0.013(3) C60 0.050(3) 0.029(3) 0.039(3) -0.014(2) -0.010(2) 0.014(2) C61 0.064(4) 0.111(6) 0.047(3) -0.002(4) -0.015(3) -0.001(4) C62 0.045(3) 0.040(3) 0.042(3) -0.007(2) -0.009(2) 0.001(2) N1 0.0265(17) 0.033(2) 0.044(2) -0.0187(18) -0.0084(15) 0.0066(15) N2 0.0272(16) 0.0190(17) 0.0181(15) -0.0052(13) -0.0067(12) 0.0029(13) N3 0.0265(16) 0.0169(16) 0.0165(15) -0.0046(12) -0.0036(12) -0.0007(13) N4 0.0268(17) 0.030(2) 0.0218(16) -0.0017(14) -0.0022(13) 0.0049(14) N5 0.0273(16) 0.0201(17) 0.0280(17) -0.0103(14) -0.0127(13) 0.0049(13) N6 0.0204(14) 0.0170(16) 0.0178(14) -0.0085(12) -0.0066(11) 0.0053(12) N7 0.0184(14) 0.0180(16) 0.0185(15) -0.0046(12) -0.0069(11) 0.0032(12) N8 0.0234(16) 0.0231(18) 0.0273(17) -0.0077(14) -0.0011(13) 0.0038(13) N9 0.052(3) 0.030(2) 0.061(3) -0.010(2) -0.013(2) 0.005(2) N10 0.044(2) 0.085(4) 0.042(3) -0.012(3) -0.010(2) -0.001(2) F1 0.0604(17) 0.0403(16) 0.0379(14) -0.0171(12) -0.0288(13) 0.0135(13) F2 0.0440(16) 0.057(2) 0.062(2) -0.0107(16) 0.0085(14) -0.0206(15) F3 0.0455(15) 0.0449(16) 0.0587(17) -0.0366(14) -0.0316(13) 0.0256(13) F4 0.0404(15) 0.0466(18) 0.065(2) -0.0115(15) -0.0030(14) -0.0175(13) F5 0.0732(19) 0.0474(17) 0.0429(16) -0.0285(14) -0.0315(14) 0.0216(15) F6 0.0445(15) 0.057(2) 0.078(2) -0.0418(17) -0.0332(15) 0.0305(14) F7 0.0410(14) 0.0358(15) 0.0410(14) -0.0221(12) -0.0084(11) 0.0077(11) F8 0.0574(17) 0.0530(19) 0.0327(14) -0.0092(13) -0.0124(13) 0.0185(14) F9 0.0309(13) 0.0238(13) 0.0547(16) -0.0169(12) 0.0082(11) -0.0066(10) F10 0.0465(16) 0.071(2) 0.0552(18) -0.0263(16) -0.0265(14) 0.0194(15) F11 0.0504(17) 0.0378(17) 0.086(2) -0.0276(17) 0.0062(16) -0.0171(14) F12 0.0371(14) 0.0369(15) 0.0450(15) -0.0174(13) 0.0109(11) -0.0017(11) F13 0.0389(14) 0.0483(17) 0.0382(14) -0.0080(13) -0.0176(11) 0.0014(12) F14 0.0471(15) 0.0340(15) 0.0354(14) -0.0102(12) 0.0028(11) -0.0150(12) F15 0.0308(13) 0.0360(15) 0.0552(16) -0.0093(13) -0.0259(12) 0.0004(11) F16 0.0343(13) 0.0264(14) 0.0494(15) -0.0031(12) -0.0195(11) -0.0067(11) F17 0.0332(14) 0.074(2) 0.081(2) -0.0614(19) 0.0039(14) -0.0001(14) F18 0.0368(14) 0.0455(17) 0.0352(14) -0.0163(12) 0.0006(11) 0.0060(12) F19 0.0621(18) 0.0515(18) 0.0288(14) -0.0054(13) -0.0105(12) -0.0198(14) F20 0.0386(14) 0.0479(17) 0.0546(17) -0.0255(14) -0.0181(12) 0.0154(12) F21 0.0347(13) 0.0475(17) 0.0324(13) -0.0146(12) -0.0109(10) 0.0098(12) F22 0.0505(16) 0.073(2) 0.0238(13) -0.0079(14) -0.0055(12) 0.0057(15) F23 0.103(3) 0.060(2) 0.075(2) -0.0442(19) -0.044(2) 0.044(2) F24 0.0585(17) 0.0552(19) 0.0406(15) -0.0226(14) -0.0216(13) 0.0002(14) P1 0.0219(5) 0.0234(5) 0.0257(5) -0.0104(4) -0.0096(4) 0.0046(4) P2 0.0307(5) 0.0197(5) 0.0261(5) -0.0064(4) -0.0025(4) -0.0020(4) P3 0.0180(4) 0.0257(6) 0.0290(5) -0.0098(4) -0.0058(4) -0.0001(4) P4 0.0395(6) 0.0316(6) 0.0223(5) -0.0093(5) -0.0090(4) 0.0057(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 N1 1.338(5) . ? C1 C2 1.396(5) . ? C2 C3 1.409(5) . ? C2 C6 1.437(5) . ? C3 C9 1.410(5) . ? C3 C4 1.419(5) . ? C4 C5 1.389(6) . ? C4 C10 1.428(6) . ? C5 N1 1.321(6) . ? C6 C7 1.351(5) . ? C7 C8 1.438(5) . ? C8 C14 1.376(5) . ? C8 C9 1.414(5) . ? C9 C12 1.410(5) . ? C10 C11 1.340(6) . ? C11 C12 1.441(5) . ? C12 C13 1.379(5) . ? C13 N2 1.354(5) . ? C14 N2 1.356(4) . ? C15 N3 1.478(5) . ? C15 N2 1.482(5) . ? C16 N3 1.352(5) . ? C16 C17 1.396(5) . ? C17 C18 1.397(5) . ? C17 C21 1.435(5) . ? C18 C24 1.418(5) . ? C18 C19 1.418(5) . ? C19 C20 1.385(5) . ? C19 C25 1.422(5) . ? C20 N3 1.355(5) . ? C21 C22 1.352(6) . ? C22 C23 1.432(6) . ? C23 C29 1.395(5) . ? C23 C24 1.411(5) . ? C24 C27 1.403(6) . ? C25 C26 1.363(5) . ? C26 C27 1.433(5) . ? C27 C28 1.407(5) . ? C28 N4 1.332(5) . ? C29 N4 1.352(6) . ? C30 N5 1.329(5) . ? C30 C31 1.398(5) . ? C31 C32 1.416(5) . ? C31 C35 1.424(5) . ? C32 C33 1.399(5) . ? C32 C40 1.411(5) . ? C33 C34 1.402(5) . ? C33 C36 1.439(5) . ? C34 N5 1.342(5) . ? C35 C37 1.354(5) . ? C36 C39 1.347(5) . ? C37 C38 1.441(5) . ? C38 C43 1.396(5) . ? C38 C40 1.400(5) . ? C39 C41 1.431(5) . ? C40 C41 1.421(5) . ? C41 C42 1.385(5) . ? C42 N6 1.353(5) . ? C43 N6 1.350(4) . ? C44 N6 1.474(4) . ? C44 N7 1.480(4) . ? C45 N7 1.348(4) . ? C45 C46 1.394(5) . ? C46 C47 1.406(5) . ? C46 C50 1.432(5) . ? C47 C48 1.416(5) . ? C47 C53 1.421(5) . ? C48 C49 1.384(5) . ? C48 C54 1.429(5) . ? C49 N7 1.347(5) . ? C50 C51 1.347(5) . ? C51 C52 1.430(5) . ? C52 C53 1.401(5) . ? C52 C58 1.408(5) . ? C53 C56 1.410(5) . ? C54 C55 1.362(5) . ? C55 C56 1.431(5) . ? C56 C57 1.404(5) . ? C57 N8 1.335(5) . ? C58 N8 1.327(5) . ? C59 C60 1.429(7) . ? C60 N9 1.143(6) . ? C61 C62 1.397(7) . ? C62 N10 1.141(6) . ? F1 P1 1.592(3) . ? F2 P1 1.582(3) . ? F3 P1 1.589(2) . ? F4 P1 1.591(3) . ? F5 P1 1.593(3) . ? F6 P1 1.595(3) . ? F7 P2 1.610(3) . ? F8 P2 1.582(3) . ? F9 P2 1.589(3) . ? F10 P2 1.594(3) . ? F11 P2 1.601(3) . ? F12 P2 1.600(3) . ? F13 P3 1.599(3) . ? F14 P3 1.599(3) . ? F15 P3 1.598(2) . ? F16 P3 1.609(3) . ? F17 P3 1.594(3) . ? F18 P3 1.604(3) . ? F19 P4 1.599(3) . ? F20 P4 1.599(3) . ? F21 P4 1.600(3) . ? F22 P4 1.596(3) . ? F23 P4 1.599(3) . ? F24 P4 1.597(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 N1 C1 C2 124.4(4) . . ? C1 C2 C3 116.7(3) . . ? C1 C2 C6 124.5(4) . . ? C3 C2 C6 118.9(3) . . ? C2 C3 C9 120.2(3) . . ? C2 C3 C4 119.5(4) . . ? C9 C3 C4 120.3(3) . . ? C5 C4 C3 116.8(4) . . ? C5 C4 C10 124.8(4) . . ? C3 C4 C10 118.4(4) . . ? N1 C5 C4 124.8(4) . . ? C7 C6 C2 121.5(3) . . ? C6 C7 C8 120.1(3) . . ? C14 C8 C9 118.5(3) . . ? C14 C8 C7 122.0(3) . . ? C9 C8 C7 119.5(3) . . ? C3 C9 C12 120.0(3) . . ? C3 C9 C8 119.9(3) . . ? C12 C9 C8 120.1(3) . . ? C11 C10 C4 121.5(3) . . ? C10 C11 C12 121.0(4) . . ? C13 C12 C9 118.2(3) . . ? C13 C12 C11 123.1(3) . . ? C9 C12 C11 118.7(4) . . ? N2 C13 C12 120.7(3) . . ? N2 C14 C8 120.3(3) . . ? N3 C15 N2 108.7(3) . . ? N3 C16 C17 120.0(3) . . ? C16 C17 C18 118.0(3) . . ? C16 C17 C21 121.9(4) . . ? C18 C17 C21 120.1(4) . . ? C17 C18 C24 119.7(3) . . ? C17 C18 C19 121.2(3) . . ? C24 C18 C19 119.0(3) . . ? C20 C19 C18 117.6(3) . . ? C20 C19 C25 122.3(3) . . ? C18 C19 C25 120.1(3) . . ? N3 C20 C19 120.4(3) . . ? C22 C21 C17 120.0(4) . . ? C21 C22 C23 121.3(4) . . ? C29 C23 C24 117.2(4) . . ? C29 C23 C22 123.8(4) . . ? C24 C23 C22 119.0(4) . . ? C27 C24 C23 120.0(4) . . ? C27 C24 C18 120.1(3) . . ? C23 C24 C18 119.9(4) . . ? C26 C25 C19 120.6(3) . . ? C25 C26 C27 120.2(4) . . ? C24 C27 C28 117.0(3) . . ? C24 C27 C26 119.9(4) . . ? C28 C27 C26 123.2(4) . . ? N4 C28 C27 124.3(4) . . ? N4 C29 C23 123.9(4) . . ? N5 C30 C31 124.2(3) . . ? C30 C31 C32 116.4(3) . . ? C30 C31 C35 124.4(3) . . ? C32 C31 C35 119.2(3) . . ? C33 C32 C40 119.9(3) . . ? C33 C32 C31 120.2(3) . . ? C40 C32 C31 119.9(3) . . ? C32 C33 C34 117.6(3) . . ? C32 C33 C36 119.5(3) . . ? C34 C33 C36 122.9(3) . . ? N5 C34 C33 122.8(3) . . ? C37 C35 C31 121.5(3) . . ? C39 C36 C33 121.2(3) . . ? C35 C37 C38 119.6(3) . . ? C43 C38 C40 118.2(3) . . ? C43 C38 C37 121.5(3) . . ? C40 C38 C37 120.3(3) . . ? C36 C39 C41 120.1(3) . . ? C38 C40 C32 119.6(3) . . ? C38 C40 C41 120.8(3) . . ? C32 C40 C41 119.6(3) . . ? C42 C41 C40 117.8(3) . . ? C42 C41 C39 122.5(3) . . ? C40 C41 C39 119.7(3) . . ? N6 C42 C41 120.2(3) . . ? N6 C43 C38 119.8(3) . . ? N6 C44 N7 111.4(3) . . ? N7 C45 C46 119.9(3) . . ? C45 C46 C47 118.1(3) . . ? C45 C46 C50 121.7(3) . . ? C47 C46 C50 120.1(3) . . ? C46 C47 C48 120.7(3) . . ? C46 C47 C53 119.5(3) . . ? C48 C47 C53 119.7(3) . . ? C49 C48 C47 117.7(3) . . ? C49 C48 C54 122.7(3) . . ? C47 C48 C54 119.5(3) . . ? N7 C49 C48 120.6(3) . . ? C51 C50 C46 119.7(3) . . ? C50 C51 C52 121.5(3) . . ? C53 C52 C58 116.6(3) . . ? C53 C52 C51 119.4(3) . . ? C58 C52 C51 124.0(3) . . ? C52 C53 C56 120.5(3) . . ? C52 C53 C47 119.6(3) . . ? C56 C53 C47 119.8(3) . . ? C55 C54 C48 120.6(3) . . ? C54 C55 C56 120.9(4) . . ? C57 C56 C53 116.5(3) . . ? C57 C56 C55 124.0(4) . . ? C53 C56 C55 119.4(3) . . ? N8 C57 C56 124.0(4) . . ? N8 C58 C52 124.2(3) . . ? N9 C60 C59 178.9(6) . . ? N10 C62 C61 178.8(7) . . ? C5 N1 C1 117.7(4) . . ? C13 N2 C14 122.1(3) . . ? C13 N2 C15 119.7(3) . . ? C14 N2 C15 118.2(3) . . ? C16 N3 C20 122.8(3) . . ? C16 N3 C15 118.0(3) . . ? C20 N3 C15 119.2(3) . . ? C28 N4 C29 117.5(4) . . ? C30 N5 C34 118.8(3) . . ? C43 N6 C42 123.2(3) . . ? C43 N6 C44 117.9(3) . . ? C42 N6 C44 118.9(3) . . ? C49 N7 C45 122.9(3) . . ? C49 N7 C44 119.3(3) . . ? C45 N7 C44 117.3(3) . . ? C58 N8 C57 118.1(3) . . ? F2 P1 F3 89.91(17) . . ? F2 P1 F4 179.59(18) . . ? F3 P1 F4 90.21(16) . . ? F2 P1 F1 89.48(17) . . ? F3 P1 F1 90.10(14) . . ? F4 P1 F1 90.12(16) . . ? F2 P1 F5 91.73(17) . . ? F3 P1 F5 89.49(14) . . ? F4 P1 F5 88.67(17) . . ? F1 P1 F5 178.71(17) . . ? F2 P1 F6 90.58(17) . . ? F3 P1 F6 179.52(19) . . ? F4 P1 F6 89.31(17) . . ? F1 P1 F6 89.91(15) . . ? F5 P1 F6 90.49(15) . . ? F8 P2 F9 91.78(16) . . ? F8 P2 F10 178.74(18) . . ? F9 P2 F10 89.49(16) . . ? F8 P2 F12 89.78(15) . . ? F9 P2 F12 89.73(14) . . ? F10 P2 F12 90.21(16) . . ? F8 P2 F11 89.88(18) . . ? F9 P2 F11 178.35(18) . . ? F10 P2 F11 88.86(18) . . ? F12 P2 F11 90.25(15) . . ? F8 P2 F7 90.37(14) . . ? F9 P2 F7 89.61(14) . . ? F10 P2 F7 89.66(15) . . ? F12 P2 F7 179.33(16) . . ? F11 P2 F7 90.41(15) . . ? F17 P3 F15 91.05(16) . . ? F17 P3 F13 89.91(16) . . ? F15 P3 F13 178.98(15) . . ? F17 P3 F14 90.29(16) . . ? F15 P3 F14 89.81(14) . . ? F13 P3 F14 90.56(15) . . ? F17 P3 F18 179.59(16) . . ? F15 P3 F18 89.35(15) . . ? F13 P3 F18 89.70(14) . . ? F14 P3 F18 89.82(15) . . ? F17 P3 F16 89.83(16) . . ? F15 P3 F16 89.78(13) . . ? F13 P3 F16 89.84(14) . . ? F14 P3 F16 179.58(15) . . ? F18 P3 F16 90.07(15) . . ? F22 P4 F24 90.03(16) . . ? F22 P4 F23 89.56(18) . . ? F24 P4 F23 90.01(17) . . ? F22 P4 F20 89.97(16) . . ? F24 P4 F20 91.01(15) . . ? F23 P4 F20 178.88(19) . . ? F22 P4 F19 179.29(18) . . ? F24 P4 F19 90.37(15) . . ? F23 P4 F19 89.86(19) . . ? F20 P4 F19 90.60(16) . . ? F22 P4 F21 90.31(15) . . ? F24 P4 F21 179.23(17) . . ? F23 P4 F21 89.30(16) . . ? F20 P4 F21 89.69(14) . . ? F19 P4 F21 89.28(14) . . ? 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 N1 C1 C2 C3 -0.1(6) . . . . ? N1 C1 C2 C6 -179.1(4) . . . . ? C1 C2 C3 C9 178.4(3) . . . . ? C6 C2 C3 C9 -2.5(5) . . . . ? C1 C2 C3 C4 -0.9(5) . . . . ? C6 C2 C3 C4 178.1(3) . . . . ? C2 C3 C4 C5 0.6(5) . . . . ? C9 C3 C4 C5 -178.8(3) . . . . ? C2 C3 C4 C10 -178.8(3) . . . . ? C9 C3 C4 C10 1.9(5) . . . . ? C3 C4 C5 N1 1.0(6) . . . . ? C10 C4 C5 N1 -179.7(4) . . . . ? C1 C2 C6 C7 -178.6(4) . . . . ? C3 C2 C6 C7 2.4(6) . . . . ? C2 C6 C7 C8 -1.0(6) . . . . ? C6 C7 C8 C14 179.6(3) . . . . ? C6 C7 C8 C9 -0.3(5) . . . . ? C2 C3 C9 C12 -179.6(3) . . . . ? C4 C3 C9 C12 -0.3(5) . . . . ? C2 C3 C9 C8 1.3(5) . . . . ? C4 C3 C9 C8 -179.3(3) . . . . ? C14 C8 C9 C3 -179.7(3) . . . . ? C7 C8 C9 C3 0.1(5) . . . . ? C14 C8 C9 C12 1.2(5) . . . . ? C7 C8 C9 C12 -179.0(3) . . . . ? C5 C4 C10 C11 178.0(4) . . . . ? C3 C4 C10 C11 -2.7(6) . . . . ? C4 C10 C11 C12 1.8(6) . . . . ? C3 C9 C12 C13 179.0(3) . . . . ? C8 C9 C12 C13 -1.9(5) . . . . ? C3 C9 C12 C11 -0.6(5) . . . . ? C8 C9 C12 C11 178.5(3) . . . . ? C10 C11 C12 C13 -179.8(4) . . . . ? C10 C11 C12 C9 -0.2(6) . . . . ? C9 C12 C13 N2 0.8(6) . . . . ? C11 C12 C13 N2 -179.6(3) . . . . ? C9 C8 C14 N2 0.6(5) . . . . ? C7 C8 C14 N2 -179.2(3) . . . . ? N3 C16 C17 C18 0.0(5) . . . . ? N3 C16 C17 C21 178.7(3) . . . . ? C16 C17 C18 C24 178.5(3) . . . . ? C21 C17 C18 C24 -0.3(5) . . . . ? C16 C17 C18 C19 -0.9(5) . . . . ? C21 C17 C18 C19 -179.6(3) . . . . ? C17 C18 C19 C20 0.1(5) . . . . ? C24 C18 C19 C20 -179.2(3) . . . . ? C17 C18 C19 C25 178.4(3) . . . . ? C24 C18 C19 C25 -0.9(5) . . . . ? C18 C19 C20 N3 1.6(5) . . . . ? C25 C19 C20 N3 -176.7(3) . . . . ? C16 C17 C21 C22 -178.2(4) . . . . ? C18 C17 C21 C22 0.5(6) . . . . ? C17 C21 C22 C23 -0.6(6) . . . . ? C21 C22 C23 C29 179.6(4) . . . . ? C21 C22 C23 C24 0.6(6) . . . . ? C29 C23 C24 C27 -0.4(5) . . . . ? C22 C23 C24 C27 178.7(3) . . . . ? C29 C23 C24 C18 -179.5(3) . . . . ? C22 C23 C24 C18 -0.4(5) . . . . ? C17 C18 C24 C27 -178.8(3) . . . . ? C19 C18 C24 C27 0.5(5) . . . . ? C17 C18 C24 C23 0.2(5) . . . . ? C19 C18 C24 C23 179.6(3) . . . . ? C20 C19 C25 C26 178.1(3) . . . . ? C18 C19 C25 C26 -0.2(5) . . . . ? C19 C25 C26 C27 1.6(5) . . . . ? C23 C24 C27 C28 0.6(5) . . . . ? C18 C24 C27 C28 179.6(3) . . . . ? C23 C24 C27 C26 -178.2(3) . . . . ? C18 C24 C27 C26 0.9(5) . . . . ? C25 C26 C27 C24 -2.0(5) . . . . ? C25 C26 C27 C28 179.4(3) . . . . ? C24 C27 C28 N4 -0.7(5) . . . . ? C26 C27 C28 N4 178.0(3) . . . . ? C24 C23 C29 N4 0.3(6) . . . . ? C22 C23 C29 N4 -178.8(4) . . . . ? N5 C30 C31 C32 0.3(5) . . . . ? N5 C30 C31 C35 179.3(4) . . . . ? C30 C31 C32 C33 -0.6(5) . . . . ? C35 C31 C32 C33 -179.7(3) . . . . ? C30 C31 C32 C40 179.1(3) . . . . ? C35 C31 C32 C40 0.0(5) . . . . ? C40 C32 C33 C34 -179.5(3) . . . . ? C31 C32 C33 C34 0.2(5) . . . . ? C40 C32 C33 C36 -0.6(5) . . . . ? C31 C32 C33 C36 179.1(3) . . . . ? C32 C33 C34 N5 0.7(5) . . . . ? C36 C33 C34 N5 -178.2(4) . . . . ? C30 C31 C35 C37 -179.2(4) . . . . ? C32 C31 C35 C37 -0.2(5) . . . . ? C32 C33 C36 C39 0.5(6) . . . . ? C34 C33 C36 C39 179.4(4) . . . . ? C31 C35 C37 C38 0.0(6) . . . . ? C35 C37 C38 C43 178.4(4) . . . . ? C35 C37 C38 C40 0.4(5) . . . . ? C33 C36 C39 C41 -0.2(6) . . . . ? C43 C38 C40 C32 -178.7(3) . . . . ? C37 C38 C40 C32 -0.6(5) . . . . ? C43 C38 C40 C41 0.9(5) . . . . ? C37 C38 C40 C41 179.0(3) . . . . ? C33 C32 C40 C38 -179.9(3) . . . . ? C31 C32 C40 C38 0.4(5) . . . . ? C33 C32 C40 C41 0.5(5) . . . . ? C31 C32 C40 C41 -179.2(3) . . . . ? C38 C40 C41 C42 -1.6(5) . . . . ? C32 C40 C41 C42 178.0(3) . . . . ? C38 C40 C41 C39 -179.8(3) . . . . ? C32 C40 C41 C39 -0.2(5) . . . . ? C36 C39 C41 C42 -178.0(4) . . . . ? C36 C39 C41 C40 0.1(6) . . . . ? C40 C41 C42 N6 1.0(5) . . . . ? C39 C41 C42 N6 179.1(3) . . . . ? C40 C38 C43 N6 0.4(5) . . . . ? C37 C38 C43 N6 -177.6(3) . . . . ? N7 C45 C46 C47 -1.6(5) . . . . ? N7 C45 C46 C50 174.6(3) . . . . ? C45 C46 C47 C48 -1.1(5) . . . . ? C50 C46 C47 C48 -177.3(3) . . . . ? C45 C46 C47 C53 174.9(3) . . . . ? C50 C46 C47 C53 -1.3(5) . . . . ? C46 C47 C48 C49 3.1(5) . . . . ? C53 C47 C48 C49 -173.0(3) . . . . ? C46 C47 C48 C54 179.4(3) . . . . ? C53 C47 C48 C54 3.3(5) . . . . ? C47 C48 C49 N7 -2.4(5) . . . . ? C54 C48 C49 N7 -178.6(3) . . . . ? C45 C46 C50 C51 -173.4(3) . . . . ? C47 C46 C50 C51 2.7(5) . . . . ? C46 C50 C51 C52 -1.2(5) . . . . ? C50 C51 C52 C53 -1.6(5) . . . . ? C50 C51 C52 C58 175.9(3) . . . . ? C58 C52 C53 C56 1.9(5) . . . . ? C51 C52 C53 C56 179.6(3) . . . . ? C58 C52 C53 C47 -174.8(3) . . . . ? C51 C52 C53 C47 2.9(5) . . . . ? C46 C47 C53 C52 -1.5(5) . . . . ? C48 C47 C53 C52 174.6(3) . . . . ? C46 C47 C53 C56 -178.2(3) . . . . ? C48 C47 C53 C56 -2.1(5) . . . . ? C49 C48 C54 C55 174.4(3) . . . . ? C47 C48 C54 C55 -1.7(5) . . . . ? C48 C54 C55 C56 -1.2(6) . . . . ? C52 C53 C56 C57 -0.2(5) . . . . ? C47 C53 C56 C57 176.5(3) . . . . ? C52 C53 C56 C55 -177.4(3) . . . . ? C47 C53 C56 C55 -0.7(5) . . . . ? C54 C55 C56 C57 -174.6(3) . . . . ? C54 C55 C56 C53 2.4(5) . . . . ? C53 C56 C57 N8 -2.0(5) . . . . ? C55 C56 C57 N8 175.1(4) . . . . ? C53 C52 C58 N8 -1.9(5) . . . . ? C51 C52 C58 N8 -179.4(3) . . . . ? C4 C5 N1 C1 -2.0(6) . . . . ? C2 C1 N1 C5 1.5(6) . . . . ? C12 C13 N2 C14 1.0(6) . . . . ? C12 C13 N2 C15 -179.7(3) . . . . ? C8 C14 N2 C13 -1.7(5) . . . . ? C8 C14 N2 C15 179.0(3) . . . . ? N3 C15 N2 C13 125.0(3) . . . . ? N3 C15 N2 C14 -55.7(4) . . . . ? C17 C16 N3 C20 1.8(5) . . . . ? C17 C16 N3 C15 -178.8(3) . . . . ? C19 C20 N3 C16 -2.6(5) . . . . ? C19 C20 N3 C15 178.0(3) . . . . ? N2 C15 N3 C16 127.6(3) . . . . ? N2 C15 N3 C20 -53.0(4) . . . . ? C27 C28 N4 C29 0.6(5) . . . . ? C23 C29 N4 C28 -0.4(6) . . . . ? C31 C30 N5 C34 0.5(6) . . . . ? C33 C34 N5 C30 -1.1(6) . . . . ? C38 C43 N6 C42 -1.1(5) . . . . ? C38 C43 N6 C44 -179.1(3) . . . . ? C41 C42 N6 C43 0.4(5) . . . . ? C41 C42 N6 C44 178.3(3) . . . . ? N7 C44 N6 C43 -121.1(3) . . . . ? N7 C44 N6 C42 60.9(4) . . . . ? C48 C49 N7 C45 -0.2(5) . . . . ? C48 C49 N7 C44 170.7(3) . . . . ? C46 C45 N7 C49 2.3(5) . . . . ? C46 C45 N7 C44 -168.8(3) . . . . ? N6 C44 N7 C49 50.3(4) . . . . ? N6 C44 N7 C45 -138.3(3) . . . . ? C52 C58 N8 C57 -0.1(6) . . . . ? C56 C57 N8 C58 2.2(6) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 28.44 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.868 _refine_diff_density_min -0.533 _refine_diff_density_rms 0.114