Electronic Supplementary Material for PCCP This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Phys.Chem.Chem.Phys.(PCCP) #=============================================================== # PROCESSING SUMMARY _journal_coden_Cambridge 1326 #=================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Christian Bruckner' _publ_contact_author_address ; Department of Chemistry University of Connecticut 55 N. Eagleville Road Storrs CT 06269-3060 UNITED STATES OF AMERICA ; _publ_contact_author_email C.BRUCKNER@UCONN.EDU _publ_requested_category ? # TITLE AND AUTHOR LIST _publ_section_title ; Origin of the bathochromically shifted optical spectra of meso-tetrathien-2'- and 3'-ylporphyrins as compared to meso-tetraphenylporphyrin ; loop_ _publ_author_name _publ_author_address C.Bruckner ; Department of Chemistry University of Connecticut Storrs, Connecticut 06269-3060 ; P.C.D.Foss ; Department of Chemistry Central Connecticut State University New Britain, CT 06053 ; J.O.Sullivan ; Department of Chemistry Central Connecticut State University New Britain, CT 06053 ; R.Pelto ; Department of Chemistry Central Connecticut State University New Britain, CT 06053 ; M.Zeller ; Department of Chemistry Youngstown State University One University Plaza Youngstown, Ohio 44555-3663 ; R.R.Birge ; Department of Chemistry University of Connecticut Storrs, Connecticut 06269-3060 ; ; G.Crundwell ; ; Department of Chemistry Central Connecticut State University New Britain, CT 06053 ; # Attachment 'ccsu02_revised.cif' data_04mz27bm _database_code_depnum_ccdc_archive 'CCDC 272182' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ;5,10,15,20-Tetrakis(5'-methyl-2'-thienyl)porphyrin bis(trifluoroacetate) ; _chemical_melting_point ? _chemical_formula_moiety 'C40 H32 N4 S4, 2(C2 F3 O2)' _chemical_formula_sum 'C44 H32 F6 N4 O4 S4' _chemical_formula_weight 923.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M I2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 16.2521(7) _cell_length_b 16.252 _cell_length_c 15.5357(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4103.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used **** _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 31.61 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 0.309 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.835 _exptl_absorpt_correction_T_max 0.940 _exptl_absorpt_process_details 'SADABS in SAINT+ (Bruker, 2003)' _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 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 21340 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 28.28 _reflns_number_total 9813 _reflns_number_gt 9775 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART 5.630 (Bruker, 1997-2002)' _computing_cell_refinement 'SAINT+ 6.45 (Bruker, 2003)' _computing_data_reduction 'SAINT+ 6.45' _computing_structure_solution 'SHELXTL 6.10 (Bruker, 2000)' _computing_structure_refinement 'SHELXTL 6.10' _computing_molecular_graphics 'SHELXTL 6.10' _computing_publication_material 'SHELXTL 6.10' _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^)+(0.0470P)^2^+11.4425P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 9813 _refine_ls_number_parameters 848 _refine_ls_number_restraints 1438 _refine_ls_R_factor_all 0.0777 _refine_ls_R_factor_gt 0.0775 _refine_ls_wR_factor_ref 0.1825 _refine_ls_wR_factor_gt 0.1824 _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_restrained_S_all 1.199 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C31 C 0.9898(7) 0.7188(5) 0.4692(5) 0.0384(15) Uani 0.50 1 d PDU . . F11 F 1.0727(4) 0.6019(6) 0.5195(6) 0.0648(18) Uani 0.50 1 d PDU . . O6 O 0.9634(6) 0.6872(7) 0.4043(6) 0.057(2) Uani 0.50 1 d PDU . . C22 C 0.5000 0.4677(4) 0.5000 0.0477(17) Uani 1 2 d SDU . . C23 C 0.5168(7) 0.3692(4) 0.4968(7) 0.0563(15) Uani 0.50 1 d PDU . . O3 O 1.0000 0.0350(3) 0.5000 0.0502(13) Uani 1 2 d SDU . . C25 C 0.0000 0.3546(5) 0.0000 0.0417(15) Uani 1 2 d SDU . . C27 C 0.0029(8) 0.4549(6) 0.0131(7) 0.0594(16) Uani 0.50 1 d PDU . . C29 C 0.9688(6) 0.1798(6) 0.5039(6) 0.0459(14) Uani 0.50 1 d PDU . . C1A C 0.5742(3) 0.6886(3) 0.6676(3) 0.0266(8) Uani 1 1 d U . . C2A C 0.5469(3) 0.7420(3) 0.7368(3) 0.0351(10) Uani 1 1 d U . . H2A H 0.5813 0.7723 0.7748 0.042 Uiso 1 1 calc R . . C3A C 0.4657(3) 0.7408(3) 0.7376(3) 0.0350(10) Uani 1 1 d U . . H3A H 0.4319 0.7723 0.7750 0.042 Uiso 1 1 calc R . . C4A C 0.4365(3) 0.6850(3) 0.6735(3) 0.0287(8) Uani 1 1 d U A . C5A C 0.3573(3) 0.65940(14) 0.6542(3) 0.0317(8) Uani 1 1 d DU . . C6A C 0.3334(3) 0.6350(4) 0.5733(3) 0.0333(9) Uani 1 1 d U A . C7A C 0.2631(4) 0.5839(4) 0.5477(3) 0.0404(11) Uani 1 1 d U . . H7A H 0.2256 0.5560 0.5844 0.048 Uiso 1 1 calc R A . C8A C 0.2630(3) 0.5850(4) 0.4640(3) 0.0409(11) Uani 1 1 d U A . H8A H 0.2274 0.5550 0.4270 0.049 Uiso 1 1 calc R . . C9A C 0.3268(3) 0.6399(4) 0.4385(3) 0.0331(9) Uani 1 1 d U . . C10A C 0.3456(3) 0.66624(14) 0.3568(3) 0.0285(8) Uani 1 1 d DU . . C11A C 0.2933(3) 0.65672(9) 0.7185(3) 0.0471(9) Uani 0.752(3) 1 d PDU A 1 C12A C 0.2129(5) 0.6674(3) 0.7115(6) 0.0488(14) Uani 0.752(3) 1 d PDU A 1 H12A H 0.1868 0.6790 0.6582 0.059 Uiso 0.752(3) 1 calc PR A 1 C13A C 0.1697(5) 0.6603(4) 0.7883(5) 0.0546(13) Uani 0.752(3) 1 d PDU A 1 H13A H 0.1119 0.6662 0.7946 0.066 Uiso 0.752(3) 1 calc PR A 1 C14A C 0.2223(5) 0.6437(4) 0.8517(5) 0.0619(14) Uani 0.752(3) 1 d PDU A 1 S1A S 0.32087(14) 0.63712(18) 0.81959(11) 0.0581(6) Uani 0.752(3) 1 d PDU A 1 C15A C 0.2000(7) 0.6320(6) 0.9428(6) 0.096(3) Uani 0.752(3) 1 d PDU A 1 H15A H 0.2495 0.6189 0.9761 0.143 Uiso 0.752(3) 1 calc PR A 1 H15B H 0.1605 0.5867 0.9477 0.143 Uiso 0.752(3) 1 calc PR A 1 H15C H 0.1752 0.6826 0.9651 0.143 Uiso 0.752(3) 1 calc PR A 1 C11C C 0.2933(3) 0.65672(9) 0.7185(3) 0.0471(9) Uani 0.248(3) 1 d PDU A 2 C12C C 0.3042(12) 0.6443(4) 0.8041(10) 0.0534(16) Uani 0.248(3) 1 d PDU A 2 H12C H 0.3578 0.6363 0.8268 0.064 Uiso 0.248(3) 1 calc PR A 2 C13C C 0.2361(11) 0.6433(5) 0.8583(11) 0.0582(16) Uani 0.248(3) 1 d PDU A 2 H13C H 0.2374 0.6350 0.9188 0.070 Uiso 0.248(3) 1 calc PR A 2 C14C C 0.1686(9) 0.6558(5) 0.8112(10) 0.058(2) Uani 0.248(3) 1 d PDU A 2 S1C S 0.1888(3) 0.6684(3) 0.7045(4) 0.0330(10) Uani 0.248(3) 1 d PDU A 2 C15C C 0.0755(10) 0.6615(6) 0.8318(13) 0.041(3) Uani 0.248(3) 1 d PDU A 2 H15H H 0.0441 0.6631 0.7780 0.062 Uiso 0.248(3) 1 calc PR A 2 H15I H 0.0647 0.7116 0.8650 0.062 Uiso 0.248(3) 1 calc PR A 2 H15G H 0.0588 0.6133 0.8656 0.062 Uiso 0.248(3) 1 calc PR A 2 C16A C 0.2796(3) 0.66936(9) 0.2956(3) 0.0387(8) Uani 0.752(3) 1 d PDU A 1 C17A C 0.2906(6) 0.6581(3) 0.2120(5) 0.0429(13) Uani 0.752(3) 1 d PDU A 1 H17A H 0.3417 0.6472 0.1845 0.051 Uiso 0.752(3) 1 calc PR A 1 C18A C 0.2116(4) 0.6653(4) 0.1696(5) 0.0524(13) Uani 0.752(3) 1 d PDU A 1 H18A H 0.2064 0.6589 0.1091 0.063 Uiso 0.752(3) 1 calc PR A 1 C19A C 0.1472(4) 0.6809(4) 0.2185(5) 0.0579(14) Uani 0.752(3) 1 d PDU A 1 S2A S 0.17998(11) 0.68714(17) 0.31975(14) 0.0526(6) Uani 0.752(3) 1 d PDU A 1 C20A C 0.0581(5) 0.6924(5) 0.2012(7) 0.085(3) Uani 0.752(3) 1 d PDU A 1 H20A H 0.0307 0.7113 0.2537 0.127 Uiso 0.752(3) 1 calc PR A 1 H20B H 0.0341 0.6399 0.1829 0.127 Uiso 0.752(3) 1 calc PR A 1 H20C H 0.0509 0.7334 0.1556 0.127 Uiso 0.752(3) 1 calc PR A 1 C16C C 0.2796(3) 0.66936(9) 0.2956(3) 0.0387(8) Uani 0.248(3) 1 d PDU A 2 C17C C 0.2010(10) 0.6809(4) 0.3187(12) 0.0476(17) Uani 0.248(3) 1 d PDU A 2 H17C H 0.1819 0.6879 0.3761 0.057 Uiso 0.248(3) 1 calc PR A 2 C18C C 0.1512(10) 0.6811(5) 0.2448(11) 0.0534(16) Uani 0.248(3) 1 d PDU A 2 H18C H 0.0933 0.6885 0.2486 0.064 Uiso 0.248(3) 1 calc PR A 2 C19C C 0.1881(9) 0.6704(4) 0.1698(9) 0.053(2) Uani 0.248(3) 1 d PDU A 2 S2C S 0.2923(4) 0.6589(4) 0.1898(4) 0.0378(11) Uani 0.248(3) 1 d PDU A 2 C20C C 0.1684(12) 0.6651(6) 0.0750(10) 0.035(3) Uani 0.248(3) 1 d PDU A 2 H20D H 0.2196 0.6598 0.0421 0.052 Uiso 0.248(3) 1 calc PR A 2 H20E H 0.1393 0.7150 0.0569 0.052 Uiso 0.248(3) 1 calc PR A 2 H20F H 0.1335 0.6170 0.0643 0.052 Uiso 0.248(3) 1 calc PR A 2 C1B C 0.5660(4) 0.4213(3) 0.1769(3) 0.0339(10) Uani 1 1 d U . . C2B C 0.5333(4) 0.4703(4) 0.2492(4) 0.0509(13) Uani 1 1 d U . . H2B H 0.5657 0.4942 0.2935 0.061 Uiso 1 1 calc R . . C3B C 0.4524(4) 0.4758(4) 0.2431(4) 0.0460(12) Uani 1 1 d U . . H3B H 0.4184 0.5045 0.2828 0.055 Uiso 1 1 calc R . . C4B C 0.4234(4) 0.4340(4) 0.1706(4) 0.0419(10) Uani 1 1 d U B . C5B C 0.3455(3) 0.4177(2) 0.1468(4) 0.0486(9) Uani 1 1 d DU . . C6B C 0.3226(4) 0.3985(3) 0.0619(4) 0.0405(10) Uani 1 1 d U B . C7B C 0.2502(4) 0.3546(4) 0.0352(4) 0.0530(14) Uani 1 1 d U . . H7B H 0.2068 0.3344 0.0703 0.064 Uiso 1 1 calc R B . C8B C 0.2576(4) 0.3489(4) -0.0490(4) 0.0432(12) Uani 1 1 d U B . H8B H 0.2191 0.3228 -0.0861 0.052 Uiso 1 1 calc R . . C9B C 0.3283(4) 0.3857(3) -0.0750(3) 0.0361(9) Uani 1 1 d U . . C10B C 0.3553(3) 0.4060(2) -0.1559(4) 0.0489(10) Uani 1 1 d DU . . C11B C 0.2763(3) 0.42125(15) 0.2031(3) 0.0526(9) Uani 0.272(3) 1 d PDU B 3 C12B C 0.2823(10) 0.3910(6) 0.2838(10) 0.0559(18) Uani 0.272(3) 1 d PDU B 3 H12B H 0.3314 0.3669 0.3054 0.067 Uiso 0.272(3) 1 calc PR B 3 C13B C 0.2112(10) 0.3977(7) 0.3329(10) 0.0591(18) Uani 0.272(3) 1 d PDU B 3 H13B H 0.2058 0.3793 0.3907 0.071 Uiso 0.272(3) 1 calc PR B 3 C14B C 0.1509(8) 0.4340(6) 0.2872(10) 0.060(2) Uani 0.272(3) 1 d PDU B 3 S1B S 0.1812(4) 0.4597(4) 0.1846(5) 0.0542(12) Uani 0.272(3) 1 d PDU B 3 C15B C 0.0640(10) 0.4569(8) 0.3058(15) 0.065(3) Uani 0.272(3) 1 d PDU B 3 H15J H 0.0307 0.4494 0.2539 0.097 Uiso 0.272(3) 1 calc PR B 3 H15L H 0.0616 0.5147 0.3239 0.097 Uiso 0.272(3) 1 calc PR B 3 H15K H 0.0426 0.4218 0.3520 0.097 Uiso 0.272(3) 1 calc PR B 3 C11D C 0.2763(3) 0.42125(15) 0.2031(3) 0.0526(9) Uani 0.728(3) 1 d PDU B 4 C12D C 0.1973(6) 0.4501(4) 0.1866(8) 0.0585(15) Uani 0.728(3) 1 d PDU B 4 H12D H 0.1806 0.4717 0.1325 0.070 Uiso 0.728(3) 1 calc PR B 4 C13D C 0.1454(5) 0.4441(5) 0.2575(6) 0.0595(14) Uani 0.728(3) 1 d PDU B 4 H13D H 0.0893 0.4606 0.2578 0.071 Uiso 0.728(3) 1 calc PR B 4 C14D C 0.1843(5) 0.4122(5) 0.3247(5) 0.0613(14) Uani 0.728(3) 1 d PDU B 4 S1D S 0.28585(18) 0.38814(19) 0.30497(15) 0.0589(6) Uani 0.728(3) 1 d PDU B 4 C15D C 0.1505(6) 0.3944(5) 0.4098(5) 0.064(2) Uani 0.728(3) 1 d PDU B 4 H15D H 0.1931 0.3691 0.4457 0.096 Uiso 0.728(3) 1 calc PR B 4 H15E H 0.1039 0.3566 0.4041 0.096 Uiso 0.728(3) 1 calc PR B 4 H15F H 0.1319 0.4457 0.4366 0.096 Uiso 0.728(3) 1 calc PR B 4 C16B C 0.2962(3) 0.40474(15) -0.2228(3) 0.0540(10) Uani 0.272(3) 1 d PDU B 3 C17B C 0.2208(9) 0.4359(6) -0.2089(11) 0.0583(18) Uani 0.272(3) 1 d PDU B 3 H17B H 0.2013 0.4600 -0.1571 0.070 Uiso 0.272(3) 1 calc PR B 3 C18B C 0.1766(10) 0.4261(7) -0.2857(10) 0.0628(17) Uani 0.272(3) 1 d PDU B 3 H18B H 0.1211 0.4440 -0.2907 0.075 Uiso 0.272(3) 1 calc PR B 3 C19B C 0.2158(9) 0.3906(6) -0.3514(9) 0.064(2) Uani 0.272(3) 1 d PDU B 3 S2B S 0.3143(5) 0.3667(4) -0.3189(5) 0.0594(13) Uani 0.272(3) 1 d PDU B 3 C20B C 0.1994(16) 0.3665(9) -0.4411(11) 0.078(4) Uani 0.272(3) 1 d PDU B 3 H20G H 0.2489 0.3416 -0.4659 0.117 Uiso 0.272(3) 1 calc PR B 3 H20H H 0.1841 0.4153 -0.4746 0.117 Uiso 0.272(3) 1 calc PR B 3 H20I H 0.1542 0.3266 -0.4426 0.117 Uiso 0.272(3) 1 calc PR B 3 C16D C 0.2962(3) 0.40474(15) -0.2228(3) 0.0540(10) Uani 0.728(3) 1 d PDU B 4 C17D C 0.3142(7) 0.3754(4) -0.3024(6) 0.0594(15) Uani 0.728(3) 1 d PDU B 4 H17D H 0.3658 0.3541 -0.3206 0.071 Uiso 0.728(3) 1 calc PR B 4 C18D C 0.2423(6) 0.3825(5) -0.3535(6) 0.0634(14) Uani 0.728(3) 1 d PDU B 4 H18D H 0.2425 0.3651 -0.4119 0.076 Uiso 0.728(3) 1 calc PR B 4 C19D C 0.1746(5) 0.4137(4) -0.3184(5) 0.0626(14) Uani 0.728(3) 1 d PDU B 4 S2D S 0.19517(14) 0.43748(18) -0.21521(16) 0.0579(6) Uani 0.728(3) 1 d PDU B 4 C20D C 0.0902(5) 0.4335(5) -0.3495(6) 0.070(2) Uani 0.728(3) 1 d PDU B 4 H20J H 0.0587 0.4591 -0.3029 0.105 Uiso 0.728(3) 1 calc PR B 4 H20K H 0.0627 0.3828 -0.3678 0.105 Uiso 0.728(3) 1 calc PR B 4 H20M H 0.0938 0.4716 -0.3983 0.105 Uiso 0.728(3) 1 calc PR B 4 F2 F 0.5037(7) 0.3365(5) 0.4212(4) 0.070(2) Uani 0.50 1 d PDU . . F3 F 0.5898(6) 0.3443(6) 0.5199(6) 0.085(2) Uani 0.50 1 d PDU . . F1 F 0.4659(7) 0.3299(5) 0.5468(5) 0.074(2) Uani 0.50 1 d PDU . . F6 F -0.0182(6) 0.4770(6) 0.0913(6) 0.077(2) Uani 0.50 1 d PDU . . F4 F -0.0502(6) 0.4939(5) -0.0360(6) 0.0685(19) Uani 0.50 1 d PDU . . F5 F 0.0740(5) 0.4907(7) -0.0011(7) 0.072(2) Uani 0.50 1 d PDU . . N1 N 0.5044(2) 0.6604(2) 0.6303(2) 0.0215(7) Uani 1 1 d DU . . H1 H 0.501(3) 0.6123(16) 0.605(3) 0.026 Uiso 1 1 d D . . N2 N 0.3709(2) 0.6645(3) 0.5037(2) 0.0270(8) Uani 1 1 d DU A . H2 H 0.399(3) 0.710(2) 0.496(4) 0.032 Uiso 1 1 d D . . N3 N 0.4944(4) 0.4060(3) 0.1337(3) 0.0429(10) Uani 1 1 d DU . . H3 H 0.483(4) 0.369(3) 0.094(3) 0.051 Uiso 1 1 d D . . N4 N 0.3698(3) 0.4204(3) -0.0053(3) 0.0422(10) Uani 1 1 d DU B . H4 H 0.411(2) 0.456(3) -0.010(4) 0.051 Uiso 1 1 d D . . O1 O 0.5034(4) 0.5025(3) 0.5672(2) 0.0540(13) Uani 1 1 d DU . . O5 O 1.0000 0.7896(4) 0.5000 0.0486(13) Uani 1 2 d SDU . . O2 O 0.0664(3) 0.3233(3) -0.0032(4) 0.0586(13) Uani 1 1 d DU . . O4 O 1.0960(6) 0.1347(7) 0.4628(6) 0.053(2) Uani 0.50 1 d PDU . . C28 C 1.0318(6) 0.1043(6) 0.4895(7) 0.0410(15) Uani 0.50 1 d PDU . . F7 F 0.9710(6) 0.2388(5) 0.4446(5) 0.0626(19) Uani 0.50 1 d PDU . . F8 F 0.9805(5) 0.2225(6) 0.5742(5) 0.0659(19) Uani 0.50 1 d PDU . . F9 F 0.8906(4) 0.1552(5) 0.5084(5) 0.0531(16) Uani 0.50 1 d PDU . . C32 C 1.0029(6) 0.6415(6) 0.5309(6) 0.0447(14) Uani 0.50 1 d PDU . . F10 F 1.0070(5) 0.6719(6) 0.6093(5) 0.0595(19) Uani 0.50 1 d PDU . . F12 F 0.9456(5) 0.5840(5) 0.5316(6) 0.0633(19) Uani 0.50 1 d PDU . . 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 C31 0.046(4) 0.044(3) 0.026(3) 0.000(2) 0.002(3) 0.002(3) F11 0.047(3) 0.073(4) 0.074(4) 0.022(3) 0.000(3) 0.020(3) O6 0.057(5) 0.068(5) 0.045(3) -0.015(3) -0.019(4) 0.013(4) C22 0.103(5) 0.0086(19) 0.032(3) 0.000 0.018(3) 0.000 C23 0.126(4) 0.007(2) 0.035(3) 0.007(3) -0.004(3) 0.008(3) O3 0.051(3) 0.035(2) 0.064(4) 0.000 0.007(3) 0.000 C25 0.033(3) 0.036(2) 0.057(4) 0.000 -0.009(3) 0.000 C27 0.060(3) 0.040(3) 0.077(4) -0.010(3) 0.004(3) -0.004(3) C29 0.059(3) 0.045(3) 0.033(3) 0.000(2) 0.000(3) 0.017(3) C1A 0.0355(17) 0.0214(17) 0.0230(16) -0.0182(14) -0.0006(14) 0.0026(16) C2A 0.036(2) 0.031(2) 0.038(2) -0.0247(18) 0.0073(17) -0.0002(18) C3A 0.037(2) 0.037(2) 0.032(2) -0.0155(17) 0.0052(17) -0.0052(19) C4A 0.0355(15) 0.035(2) 0.0152(15) 0.0000(15) 0.0016(13) -0.0029(17) C5A 0.0336(15) 0.0408(19) 0.0208(13) 0.0040(16) 0.0045(13) -0.0113(18) C6A 0.032(2) 0.046(2) 0.0227(14) 0.0006(17) 0.0018(14) -0.0103(19) C7A 0.044(2) 0.053(3) 0.0243(18) 0.0028(19) -0.0011(17) -0.022(2) C8A 0.037(2) 0.061(3) 0.0248(18) 0.0015(19) -0.0066(17) -0.015(2) C9A 0.0273(19) 0.047(2) 0.0253(14) -0.0002(17) -0.0041(14) 0.0018(18) C10A 0.0249(16) 0.0364(19) 0.0242(14) 0.0051(17) -0.0053(13) 0.0002(18) C11A 0.0401(15) 0.075(2) 0.0267(13) -0.0020(18) 0.0080(13) -0.0223(19) C12A 0.041(2) 0.063(3) 0.042(2) -0.001(3) 0.008(2) -0.014(3) C13A 0.040(2) 0.077(3) 0.047(2) -0.010(3) 0.0181(18) -0.016(3) C14A 0.048(2) 0.101(3) 0.037(2) -0.007(3) 0.0186(19) -0.022(3) S1A 0.0483(10) 0.1084(16) 0.0175(7) -0.0181(9) 0.0110(6) -0.0227(11) C15A 0.082(5) 0.166(9) 0.038(3) -0.020(5) 0.032(3) -0.017(7) C11C 0.0401(15) 0.075(2) 0.0267(13) -0.0020(18) 0.0080(13) -0.0223(19) C12C 0.043(3) 0.092(4) 0.025(2) -0.005(3) 0.011(2) -0.018(4) C13C 0.042(3) 0.098(4) 0.034(2) -0.010(3) 0.015(2) -0.019(3) C14C 0.042(3) 0.089(5) 0.042(3) -0.008(4) 0.015(3) -0.019(4) S1C 0.040(2) 0.0136(17) 0.045(2) -0.0017(16) 0.0123(17) 0.0079(17) C15C 0.041(3) 0.042(5) 0.041(4) -0.002(4) 0.009(3) -0.008(4) C16A 0.0268(14) 0.0579(19) 0.0315(14) 0.0145(17) -0.0086(12) -0.0005(17) C17A 0.044(2) 0.052(3) 0.032(2) 0.005(3) -0.0114(19) 0.002(3) C18A 0.044(2) 0.074(3) 0.039(2) 0.012(3) -0.0199(18) -0.019(3) C19A 0.036(2) 0.095(4) 0.043(2) 0.017(3) -0.023(2) -0.016(3) S2A 0.0169(7) 0.0963(15) 0.0445(9) 0.0205(10) -0.0109(6) -0.0183(9) C20A 0.041(3) 0.141(8) 0.073(5) 0.018(6) -0.034(3) -0.013(5) C16C 0.0268(14) 0.0579(19) 0.0315(14) 0.0145(17) -0.0086(12) -0.0005(17) C17C 0.026(3) 0.077(4) 0.040(3) 0.009(4) -0.011(2) -0.007(4) C18C 0.031(2) 0.087(4) 0.041(3) 0.015(4) -0.015(2) -0.015(3) C19C 0.038(3) 0.081(5) 0.039(3) 0.017(4) -0.017(3) -0.016(4) S2C 0.044(2) 0.036(2) 0.034(2) -0.0093(19) -0.0144(18) -0.001(2) C20C 0.036(4) 0.033(5) 0.036(3) 0.017(4) -0.009(3) -0.003(4) C1B 0.0500(19) 0.0229(18) 0.0287(18) -0.0227(15) 0.0050(15) -0.0105(16) C2B 0.050(2) 0.060(3) 0.043(2) -0.034(2) 0.008(2) -0.002(3) C3B 0.048(2) 0.047(3) 0.043(2) -0.020(2) 0.012(2) -0.014(2) C4B 0.0497(17) 0.043(3) 0.033(2) -0.0086(19) 0.0067(16) -0.016(2) C5B 0.0539(17) 0.045(2) 0.0465(18) -0.009(2) 0.0004(15) -0.024(2) C6B 0.049(2) 0.028(2) 0.0441(17) 0.0067(18) -0.0055(16) -0.025(2) C7B 0.060(3) 0.054(3) 0.045(2) 0.001(2) -0.005(2) -0.035(2) C8B 0.055(3) 0.036(3) 0.038(2) 0.0102(19) -0.0106(19) -0.022(2) C9B 0.052(2) 0.0136(17) 0.0425(16) 0.0132(17) -0.0074(17) -0.0097(19) C10B 0.058(2) 0.045(2) 0.0435(18) 0.0338(19) -0.0066(17) -0.004(2) C11B 0.0486(15) 0.060(2) 0.0486(16) -0.0132(17) -0.0035(14) -0.0222(18) C12B 0.054(3) 0.070(4) 0.044(3) -0.016(3) -0.001(3) -0.018(3) C13B 0.054(3) 0.076(4) 0.047(3) -0.022(3) -0.001(3) -0.019(3) C14B 0.050(3) 0.074(4) 0.055(4) -0.019(4) -0.002(3) -0.022(4) S1B 0.049(2) 0.052(3) 0.061(2) -0.014(2) -0.001(2) -0.015(2) C15B 0.064(3) 0.066(5) 0.064(5) -0.003(4) 0.009(3) -0.002(4) C11D 0.0486(15) 0.060(2) 0.0486(16) -0.0132(17) -0.0035(14) -0.0222(18) C12D 0.049(3) 0.063(3) 0.063(3) -0.011(3) 0.000(2) -0.024(3) C13D 0.048(2) 0.067(3) 0.063(3) -0.019(3) 0.000(2) -0.027(3) C14D 0.052(3) 0.081(4) 0.051(2) -0.026(3) -0.004(2) -0.029(3) S1D 0.0612(13) 0.0765(15) 0.0389(10) -0.0251(10) 0.0040(9) -0.0197(12) C15D 0.067(4) 0.076(5) 0.050(3) -0.035(3) 0.007(3) -0.042(4) C16B 0.0556(18) 0.063(2) 0.0430(16) 0.0266(18) -0.0047(15) -0.0146(19) C17B 0.052(3) 0.075(4) 0.048(3) 0.027(3) -0.008(3) -0.018(3) C18B 0.055(3) 0.086(4) 0.048(3) 0.032(3) -0.008(3) -0.027(3) C19B 0.060(4) 0.086(4) 0.045(3) 0.031(4) -0.009(3) -0.029(4) S2B 0.065(2) 0.067(3) 0.046(2) 0.017(2) -0.007(2) -0.022(2) C20B 0.080(8) 0.100(10) 0.055(5) 0.016(7) -0.022(5) -0.023(9) C16D 0.0556(18) 0.063(2) 0.0430(16) 0.0266(18) -0.0047(15) -0.0146(19) C17D 0.067(3) 0.070(3) 0.041(2) 0.030(3) -0.009(2) -0.014(3) C18D 0.065(3) 0.083(3) 0.042(2) 0.034(2) -0.009(2) -0.030(3) C19D 0.056(2) 0.088(3) 0.043(2) 0.039(3) -0.012(2) -0.033(3) S2D 0.0395(10) 0.0828(15) 0.0514(11) 0.0313(11) -0.0107(9) -0.0337(10) C20D 0.059(3) 0.087(6) 0.065(4) 0.059(4) -0.022(3) -0.039(4) F2 0.153(6) 0.017(3) 0.040(3) -0.009(2) -0.011(3) 0.011(4) F3 0.133(4) 0.046(4) 0.075(5) 0.012(4) -0.020(4) 0.028(3) F1 0.152(5) 0.013(2) 0.058(4) 0.010(3) 0.008(4) -0.015(4) F6 0.092(5) 0.056(4) 0.084(4) -0.022(3) 0.013(3) -0.007(4) F4 0.086(4) 0.026(3) 0.094(4) 0.004(4) -0.002(4) 0.004(3) F5 0.073(3) 0.052(3) 0.091(4) -0.009(3) 0.006(3) -0.017(3) N1 0.0320(15) 0.0203(15) 0.0123(12) 0.0031(12) -0.0004(12) 0.0041(14) N2 0.0238(16) 0.036(2) 0.0211(13) -0.0054(14) -0.0007(12) -0.0067(15) N3 0.056(2) 0.044(3) 0.0289(19) -0.0120(17) 0.0034(17) -0.004(2) N4 0.045(2) 0.034(2) 0.0473(18) 0.0103(18) -0.0059(18) -0.0183(18) O1 0.113(4) 0.0215(17) 0.0276(18) -0.0041(14) 0.004(2) 0.007(2) O5 0.069(4) 0.036(2) 0.041(3) 0.000 -0.002(2) 0.000 O2 0.028(2) 0.054(3) 0.093(4) 0.006(3) -0.005(2) 0.0054(18) O4 0.050(3) 0.060(4) 0.051(4) -0.022(4) 0.016(3) -0.011(3) C28 0.040(3) 0.041(3) 0.042(4) -0.007(3) 0.006(3) 0.005(2) F7 0.086(5) 0.047(3) 0.056(3) 0.018(3) -0.004(4) 0.011(3) F8 0.080(4) 0.077(4) 0.041(3) -0.023(3) 0.008(3) 0.031(4) F9 0.050(3) 0.062(4) 0.047(4) 0.021(3) 0.003(3) 0.028(3) C32 0.045(3) 0.042(3) 0.048(3) 0.006(2) 0.003(3) -0.001(3) F10 0.064(4) 0.081(5) 0.033(2) 0.012(3) 0.000(3) -0.020(4) F12 0.061(3) 0.054(3) 0.075(4) 0.012(3) 0.007(4) -0.021(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C31 O6 1.209(10) . ? C31 O5 1.257(9) . ? C31 C32 1.595(11) . ? F11 C32 1.318(10) . ? C22 O1 1.188(5) . ? C22 O1 1.188(5) 2_656 ? C22 C23 1.625(8) . ? C23 F1 1.303(11) . ? C23 F3 1.304(11) . ? C23 F2 1.307(11) . ? O3 C28 1.250(9) . ? C25 O2 1.193(5) 2 ? C25 O2 1.193(5) . ? C25 C27 1.643(11) . ? C27 F6 1.312(11) . ? C27 F5 1.312(12) . ? C27 F4 1.315(11) . ? C29 F8 1.309(10) . ? C29 F7 1.330(10) . ? C29 F9 1.335(10) . ? C29 C28 1.612(11) . ? C1A N1 1.353(6) . ? C1A C10A 1.405(6) 2_656 ? C1A C2A 1.451(6) . ? C2A C3A 1.320(8) . ? C2A H2A 0.9500 . ? C3A C4A 1.427(7) . ? C3A H3A 0.9500 . ? C4A N1 1.353(6) . ? C4A C5A 1.385(7) . ? C5A C6A 1.374(6) . ? C5A C11A 1.442(6) . ? C6A N2 1.330(6) . ? C6A C7A 1.466(7) . ? C7A C8A 1.301(7) . ? C7A H7A 0.9500 . ? C8A C9A 1.424(8) . ? C8A H8A 0.9500 . ? C9A N2 1.304(6) . ? C9A C10A 1.374(6) . ? C10A C1A 1.405(6) 2_656 ? C10A C16A 1.435(5) . ? C11A C12A 1.323(9) . ? C11A S1A 1.664(5) . ? C12A C13A 1.390(10) . ? C12A H12A 0.9500 . ? C13A C14A 1.332(10) . ? C13A H13A 0.9500 . ? C14A C15A 1.472(10) . ? C14A S1A 1.681(8) . ? C15A H15A 0.9800 . ? C15A H15B 0.9800 . ? C15A H15C 0.9800 . ? C12C C13C 1.390(17) . ? C12C H12C 0.9500 . ? C13C C14C 1.335(17) . ? C13C H13C 0.9500 . ? C14C C15C 1.549(16) . ? C14C S1C 1.701(15) . ? C15C H15H 0.9800 . ? C15C H15I 0.9800 . ? C15C H15G 0.9800 . ? C16A C17A 1.323(9) . ? C16A S2A 1.686(5) . ? C17A C18A 1.448(10) . ? C17A H17A 0.9500 . ? C18A C19A 1.317(10) . ? C18A H18A 0.9500 . ? C19A C20A 1.484(10) . ? C19A S2A 1.664(7) . ? C20A H20A 0.9800 . ? C20A H20B 0.9800 . ? C20A H20C 0.9800 . ? C17C C18C 1.404(17) . ? C17C H17C 0.9500 . ? C18C C19C 1.323(17) . ? C18C H18C 0.9500 . ? C19C C20C 1.510(16) . ? C19C S2C 1.732(15) . ? C20C H20D 0.9800 . ? C20C H20E 0.9800 . ? C20C H20F 0.9800 . ? C1B C10B 1.343(8) 2_655 ? C1B N3 1.366(8) . ? C1B C2B 1.476(7) . ? C2B C3B 1.322(9) . ? C2B H2B 0.9500 . ? C3B C4B 1.398(8) . ? C3B H3B 0.9500 . ? C4B C5B 1.345(8) . ? C4B N3 1.366(8) . ? C5B C6B 1.405(8) . ? C5B C11B 1.427(7) . ? C6B N4 1.344(8) . ? C6B C7B 1.438(8) . ? C7B C8B 1.318(9) . ? C7B H7B 0.9500 . ? C8B C9B 1.356(8) . ? C8B H8B 0.9500 . ? C9B C10B 1.372(8) . ? C9B N4 1.395(7) . ? C10B C1B 1.343(8) 2_655 ? C10B C16B 1.414(7) . ? C11B C12B 1.350(15) . ? C11B S1B 1.691(8) . ? C12B C13B 1.389(17) . ? C12B H12B 0.9500 . ? C13B C14B 1.345(16) . ? C13B H13B 0.9500 . ? C14B C15B 1.490(17) . ? C14B S1B 1.720(15) . ? C15B H15J 0.9800 . ? C15B H15L 0.9800 . ? C15B H15K 0.9800 . ? C12D C13D 1.392(13) . ? C12D H12D 0.9500 . ? C13D C14D 1.325(12) . ? C13D H13D 0.9500 . ? C14D C15D 1.461(11) . ? C14D S1D 1.723(9) . ? C15D H15D 0.9800 . ? C15D H15E 0.9800 . ? C15D H15F 0.9800 . ? C16B C17B 1.343(14) . ? C16B S2B 1.643(9) . ? C17B C18B 1.401(17) . ? C17B H17B 0.9500 . ? C18B C19B 1.335(16) . ? C18B H18B 0.9500 . ? C19B C20B 1.472(17) . ? C19B S2B 1.724(15) . ? C20B H20G 0.9800 . ? C20B H20H 0.9800 . ? C20B H20I 0.9800 . ? C17D C18D 1.418(12) . ? C17D H17D 0.9500 . ? C18D C19D 1.329(12) . ? C18D H18D 0.9500 . ? C19D C20D 1.489(10) . ? C19D S2D 1.682(8) . ? C20D H20J 0.9800 . ? C20D H20K 0.9800 . ? C20D H20M 0.9800 . ? N1 H1 0.874(19) . ? N2 H2 0.88(2) . ? N3 H3 0.88(2) . ? N4 H4 0.88(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 C31 O5 138.8(10) . . ? O6 C31 C32 102.4(8) . . ? O5 C31 C32 118.3(7) . . ? O1 C22 O1 123.1(6) . 2_656 ? O1 C22 C23 116.8(5) . 2_656 ? O1 C22 C23 119.2(5) . . ? O1 C22 C23 116.8(5) 2_656 . ? F1 C23 F3 105.2(9) . . ? F1 C23 F2 103.5(8) . . ? F3 C23 F2 105.7(9) . . ? F1 C23 C22 110.9(7) . . ? F3 C23 C22 116.8(8) . . ? F2 C23 C22 113.6(7) . . ? O2 C25 O2 129.6(8) 2 . ? O2 C25 C27 116.3(6) 2 . ? O2 C25 C27 113.7(6) . . ? O2 C25 C27 113.7(6) 2 2 ? O2 C25 C27 116.3(6) . 2 ? F6 C27 F5 105.4(9) . . ? F6 C27 F4 103.5(9) . . ? F5 C27 F4 105.5(9) . . ? F6 C27 C25 112.2(8) . . ? F5 C27 C25 116.4(9) . . ? F4 C27 C25 112.7(8) . . ? F8 C29 F7 101.0(8) . . ? F8 C29 F9 104.7(8) . . ? F7 C29 F9 106.2(8) . . ? F8 C29 C28 115.3(8) . . ? F7 C29 C28 115.9(8) . . ? F9 C29 C28 112.6(8) . . ? N1 C1A C10A 125.0(3) . 2_656 ? N1 C1A C2A 105.3(4) . . ? C10A C1A C2A 129.6(4) 2_656 . ? C3A C2A C1A 107.7(4) . . ? C3A C2A H2A 126.2 . . ? C1A C2A H2A 126.2 . . ? C2A C3A C4A 109.6(4) . . ? C2A C3A H3A 125.2 . . ? C4A C3A H3A 125.2 . . ? N1 C4A C5A 124.2(4) . . ? N1 C4A C3A 105.2(4) . . ? C5A C4A C3A 130.6(4) . . ? C6A C5A C4A 123.2(4) . . ? C6A C5A C11A 114.9(4) . . ? C4A C5A C11A 121.9(4) . . ? N2 C6A C5A 120.6(4) . . ? N2 C6A C7A 109.9(4) . . ? C5A C6A C7A 129.2(4) . . ? C8A C7A C6A 105.3(5) . . ? C8A C7A H7A 127.3 . . ? C6A C7A H7A 127.3 . . ? C7A C8A C9A 106.6(5) . . ? C7A C8A H8A 126.7 . . ? C9A C8A H8A 126.7 . . ? N2 C9A C10A 120.1(5) . . ? N2 C9A C8A 112.0(4) . . ? C10A C9A C8A 127.9(4) . . ? C9A C10A C1A 122.4(4) . 2_656 ? C9A C10A C16A 117.2(4) . . ? C1A C10A C16A 120.4(4) 2_656 . ? C12A C11A C5A 130.7(6) . . ? C12A C11A S1A 111.6(5) . . ? C5A C11A S1A 117.8(4) . . ? C11A C12A C13A 114.7(7) . . ? C11A C12A H12A 122.6 . . ? C13A C12A H12A 122.6 . . ? C14A C13A C12A 109.1(7) . . ? C14A C13A H13A 125.4 . . ? C12A C13A H13A 125.4 . . ? C13A C14A C15A 125.3(9) . . ? C13A C14A S1A 113.9(6) . . ? C15A C14A S1A 120.8(7) . . ? C11A S1A C14A 90.7(3) . . ? C14A C15A H15A 109.5 . . ? C14A C15A H15B 109.5 . . ? H15A C15A H15B 109.5 . . ? C14A C15A H15C 109.5 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? C13C C12C H12C 120.2 . . ? C14C C13C C12C 108.6(15) . . ? C14C C13C H13C 125.7 . . ? C12C C13C H13C 125.7 . . ? C13C C14C C15C 134.3(16) . . ? C13C C14C S1C 113.2(12) . . ? C15C C14C S1C 112.5(12) . . ? C14C C15C H15H 109.5 . . ? C14C C15C H15I 109.5 . . ? H15H C15C H15I 109.5 . . ? C14C C15C H15G 109.5 . . ? H15H C15C H15G 109.5 . . ? H15I C15C H15G 109.5 . . ? C17A C16A C10A 122.9(6) . . ? C17A C16A S2A 111.9(5) . . ? C10A C16A S2A 125.2(4) . . ? C16A C17A C18A 108.4(7) . . ? C16A C17A H17A 125.8 . . ? C18A C17A H17A 125.8 . . ? C19A C18A C17A 117.2(7) . . ? C19A C18A H18A 121.4 . . ? C17A C18A H18A 121.4 . . ? C18A C19A C20A 134.0(8) . . ? C18A C19A S2A 107.6(5) . . ? C20A C19A S2A 118.4(7) . . ? C19A S2A C16A 95.0(3) . . ? C19A C20A H20A 109.5 . . ? C19A C20A H20B 109.5 . . ? H20A C20A H20B 109.5 . . ? C19A C20A H20C 109.5 . . ? H20A C20A H20C 109.5 . . ? H20B C20A H20C 109.5 . . ? C18C C17C H17C 125.4 . . ? C19C C18C C17C 117.3(15) . . ? C19C C18C H18C 121.3 . . ? C17C C18C H18C 121.3 . . ? C18C C19C C20C 140.4(15) . . ? C18C C19C S2C 107.4(11) . . ? C20C C19C S2C 112.1(12) . . ? C19C C20C H20D 109.5 . . ? C19C C20C H20E 109.5 . . ? H20D C20C H20E 109.5 . . ? C19C C20C H20F 109.5 . . ? H20D C20C H20F 109.5 . . ? H20E C20C H20F 109.5 . . ? C10B C1B N3 131.2(4) 2_655 . ? C10B C1B C2B 128.8(5) 2_655 . ? N3 C1B C2B 99.5(5) . . ? C3B C2B C1B 109.9(5) . . ? C3B C2B H2B 125.0 . . ? C1B C2B H2B 125.0 . . ? C2B C3B C4B 111.1(5) . . ? C2B C3B H3B 124.5 . . ? C4B C3B H3B 124.5 . . ? C5B C4B N3 127.9(5) . . ? C5B C4B C3B 129.4(6) . . ? N3 C4B C3B 102.4(5) . . ? C4B C5B C6B 123.4(5) . . ? C4B C5B C11B 124.5(5) . . ? C6B C5B C11B 112.1(5) . . ? N4 C6B C5B 121.3(5) . . ? N4 C6B C7B 112.0(5) . . ? C5B C6B C7B 126.7(5) . . ? C8B C7B C6B 104.3(6) . . ? C8B C7B H7B 127.9 . . ? C6B C7B H7B 127.9 . . ? C7B C8B C9B 110.0(5) . . ? C7B C8B H8B 125.0 . . ? C9B C8B H8B 125.0 . . ? C8B C9B C10B 130.5(5) . . ? C8B C9B N4 111.0(5) . . ? C10B C9B N4 117.3(5) . . ? C1B C10B C9B 124.8(5) 2_655 . ? C1B C10B C16B 118.1(5) 2_655 . ? C9B C10B C16B 116.9(4) . . ? C12B C11B C5B 119.8(8) . . ? C12B C11B S1B 111.0(8) . . ? C5B C11B S1B 129.2(5) . . ? C11B C12B C13B 114.9(13) . . ? C11B C12B H12B 122.6 . . ? C13B C12B H12B 122.6 . . ? C14B C13B C12B 110.5(14) . . ? C14B C13B H13B 124.7 . . ? C12B C13B H13B 124.7 . . ? C13B C14B C15B 134.2(17) . . ? C13B C14B S1B 112.8(11) . . ? C15B C14B S1B 113.0(13) . . ? C11B S1B C14B 90.8(6) . . ? C14B C15B H15J 109.5 . . ? C14B C15B H15L 109.5 . . ? H15J C15B H15L 109.5 . . ? C14B C15B H15K 109.5 . . ? H15J C15B H15K 109.5 . . ? H15L C15B H15K 109.5 . . ? C13D C12D H12D 123.5 . . ? C14D C13D C12D 111.2(9) . . ? C14D C13D H13D 124.4 . . ? C12D C13D H13D 124.4 . . ? C13D C14D C15D 127.6(9) . . ? C13D C14D S1D 114.0(7) . . ? C15D C14D S1D 118.4(7) . . ? C14D C15D H15D 109.5 . . ? C14D C15D H15E 109.5 . . ? H15D C15D H15E 109.5 . . ? C14D C15D H15F 109.5 . . ? H15D C15D H15F 109.5 . . ? H15E C15D H15F 109.5 . . ? C17B C16B C10B 119.8(9) . . ? C17B C16B S2B 116.8(9) . . ? C10B C16B S2B 123.5(5) . . ? C16B C17B C18B 106.8(13) . . ? C16B C17B H17B 126.6 . . ? C18B C17B H17B 126.6 . . ? C19B C18B C17B 117.1(14) . . ? C19B C18B H18B 121.5 . . ? C17B C18B H18B 121.5 . . ? C18B C19B C20B 138.9(17) . . ? C18B C19B S2B 108.5(11) . . ? C20B C19B S2B 112.7(14) . . ? C16B S2B C19B 90.9(7) . . ? C19B C20B H20G 109.5 . . ? C19B C20B H20H 109.5 . . ? H20G C20B H20H 109.5 . . ? C19B C20B H20I 109.5 . . ? H20G C20B H20I 109.5 . . ? H20H C20B H20I 109.5 . . ? C18D C17D H17D 126.1 . . ? C19D C18D C17D 118.9(9) . . ? C19D C18D H18D 120.6 . . ? C17D C18D H18D 120.6 . . ? C18D C19D C20D 135.3(8) . . ? C18D C19D S2D 108.3(6) . . ? C20D C19D S2D 116.3(7) . . ? C19D C20D H20J 109.5 . . ? C19D C20D H20K 109.5 . . ? H20J C20D H20K 109.5 . . ? C19D C20D H20M 109.5 . . ? H20J C20D H20M 109.5 . . ? H20K C20D H20M 109.5 . . ? C1A N1 C4A 111.8(4) . . ? C1A N1 H1 123(4) . . ? C4A N1 H1 116(4) . . ? C9A N2 C6A 105.6(4) . . ? C9A N2 H2 116(4) . . ? C6A N2 H2 131(4) . . ? C4B N3 C1B 116.9(5) . . ? C4B N3 H3 110(5) . . ? C1B N3 H3 131(4) . . ? C6B N4 C9B 102.7(5) . . ? C6B N4 H4 132(4) . . ? C9B N4 H4 124(4) . . ? O4 C28 O3 139.3(10) . . ? O4 C28 C29 106.3(8) . . ? O3 C28 C29 113.9(7) . . ? F10 C32 F11 105.3(8) . . ? F10 C32 F12 107.1(8) . . ? F11 C32 F12 105.2(8) . . ? F10 C32 C31 105.5(8) . . ? F11 C32 C31 114.8(8) . . ? F12 C32 C31 117.9(8) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.422 _refine_diff_density_min -0.322 _refine_diff_density_rms 0.073