# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_na1cult _database_code_depnum_ccdc_archive 'CCDC 883789' #TrackingRef 'na1cult.cif' _audit_creation_date 2011-11-11 _audit_creation_method ; Olex2 1.1-beta (compiled Nov 1 2011 20:42:30, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C37 H30 N S, F6 P' _chemical_formula_sum 'C37 H30 F6 N P S' _chemical_formula_weight 665.65 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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 _space_group_IT_number 2 _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 9.6816(4) _cell_length_b 17.8079(10) _cell_length_c 20.1801(10) _cell_angle_alpha 73.460(5) _cell_angle_beta 76.508(4) _cell_angle_gamma 84.393(4) _cell_volume 3241.4(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6420 _cell_measurement_temperature 173.1(5) _cell_measurement_theta_max 71.4595 _cell_measurement_theta_min 4.6777 _exptl_absorpt_coefficient_mu 1.895 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.91989 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1376 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.15 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_av_unetI/netI 0.0535 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 20032 _diffrn_reflns_theta_full 66.50 _diffrn_reflns_theta_max 66.99 _diffrn_reflns_theta_min 4.68 _diffrn_ambient_temperature 173.1(5) _diffrn_detector_area_resol_mean 15.9578 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 84.00 123.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 38.0000 90.0000 39 #__ type_ start__ end____ width___ exp.time_ 2 omega 46.00 79.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -50.0000 -30.0000 33 #__ type_ start__ end____ width___ exp.time_ 3 omega 33.00 77.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -178.0000 -90.0000 44 #__ type_ start__ end____ width___ exp.time_ 4 omega -106.00 -18.00 1.0000 7.0000 omega____ theta____ kappa____ phi______ frames - -55.0000 125.0000 60.0000 88 #__ type_ start__ end____ width___ exp.time_ 5 omega -18.00 97.00 1.0000 7.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 -19.0000 -150.0000 115 #__ type_ start__ end____ width___ exp.time_ 6 omega -9.00 75.00 1.0000 7.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 -57.0000 -30.0000 84 #__ type_ start__ end____ width___ exp.time_ 7 omega 26.00 124.00 1.0000 7.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 77.0000 -180.0000 98 #__ type_ start__ end____ width___ exp.time_ 8 omega -87.00 -23.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 64.0000 -30.0000 64 #__ type_ start__ end____ width___ exp.time_ 9 omega 122.00 178.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 38.0000 0.0000 56 #__ type_ start__ end____ width___ exp.time_ 10 omega 39.00 71.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 120.0000 32 #__ type_ start__ end____ width___ exp.time_ 11 omega 41.00 72.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 -30.0000 31 #__ type_ start__ end____ width___ exp.time_ 12 omega 39.00 72.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 60.0000 33 #__ type_ start__ end____ width___ exp.time_ 13 omega 41.00 67.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 -60.0000 26 #__ type_ start__ end____ width___ exp.time_ 14 omega 40.00 81.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -50.0000 90.0000 41 #__ type_ start__ end____ width___ exp.time_ 15 omega 41.00 70.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 60.0000 29 #__ type_ start__ end____ width___ exp.time_ 16 omega 37.00 72.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 -120.0000 35 #__ type_ start__ end____ width___ exp.time_ 17 omega 46.00 72.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 30.0000 26 #__ type_ start__ end____ width___ exp.time_ 18 omega 81.00 143.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 60.0000 62 #__ type_ start__ end____ width___ exp.time_ 19 omega 40.00 65.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 -180.0000 25 #__ type_ start__ end____ width___ exp.time_ 20 omega 42.00 105.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 12.0000 -30.0000 63 #__ type_ start__ end____ width___ exp.time_ 21 omega 122.00 174.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 12.0000 -30.0000 52 #__ type_ start__ end____ width___ exp.time_ 22 omega 46.00 83.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -50.0000 -150.0000 37 #__ type_ start__ end____ width___ exp.time_ 23 omega 38.00 127.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 -150.0000 89 #__ type_ start__ end____ width___ exp.time_ 24 omega 38.00 148.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 -30.0000 110 #__ type_ start__ end____ width___ exp.time_ 25 omega 85.00 112.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 38.0000 0.0000 27 ; _diffrn_measurement_device 'kappa diffractometer' _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0200557000 _diffrn_orient_matrix_UB_12 0.0689792000 _diffrn_orient_matrix_UB_13 0.0283715000 _diffrn_orient_matrix_UB_21 0.1624751000 _diffrn_orient_matrix_UB_22 -0.0125176000 _diffrn_orient_matrix_UB_23 -0.0199729000 _diffrn_orient_matrix_UB_31 0.0027072000 _diffrn_orient_matrix_UB_32 0.0569076000 _diffrn_orient_matrix_UB_33 -0.0738008000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.5418 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 30 _diffrn_source_power 1.5 _diffrn_source_target Cu _diffrn_source_voltage 50 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 8948 _reflns_number_total 11388 _reflns_odcompleteness_completeness 98.61 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 68.13 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; XS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.895 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.089 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 855 _refine_ls_number_reflns 11388 _refine_ls_number_restraints 132 _refine_ls_R_factor_all 0.0895 _refine_ls_R_factor_gt 0.0751 _refine_ls_restrained_S_all 1.158 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1527P)^2^+0.6140P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2030 _refine_ls_wR_factor_ref 0.2193 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 S1 S 0.93534(7) 0.14833(4) 0.46572(4) 0.0326(2) Uani 1 1 d . . . C1 C 0.9158(3) 0.22725(17) 0.39482(16) 0.0322(6) Uani 1 1 d . . . C2 C 1.0215(4) 0.2737(2) 0.34558(18) 0.0426(8) Uani 1 1 d . . . H2 H 1.1187 0.2639 0.3480 0.051 Uiso 1 1 calc R . . C3 C 0.9807(4) 0.3342(2) 0.29339(19) 0.0493(9) Uani 1 1 d . . . H3 H 1.0505 0.3665 0.2588 0.059 Uiso 1 1 calc R . . C4 C 0.8376(5) 0.3486(2) 0.2908(2) 0.0520(9) Uani 1 1 d . . . H4 H 0.8123 0.3909 0.2543 0.062 Uiso 1 1 calc R . . C5 C 0.7321(4) 0.3039(2) 0.33922(18) 0.0424(8) Uani 1 1 d . . . H5 H 0.6349 0.3145 0.3370 0.051 Uiso 1 1 calc R . . C6 C 0.7736(3) 0.24204(17) 0.39199(16) 0.0329(6) Uani 1 1 d . . . N7 N 0.6847(3) 0.19039(14) 0.44795(13) 0.0299(5) Uani 1 1 d . . . C8 C 0.7545(3) 0.13765(17) 0.49073(15) 0.0286(6) Uani 1 1 d . . . C9 C 0.5277(3) 0.19685(19) 0.45563(18) 0.0371(7) Uani 1 1 d . . . H9A H 0.4965 0.2528 0.4450 0.045 Uiso 1 1 calc R . . H9B H 0.4812 0.1710 0.5051 0.045 Uiso 1 1 calc R . . C10 C 0.4825(4) 0.1591(2) 0.4064(2) 0.0510(9) Uani 1 1 d . . . H10A H 0.5279 0.1849 0.3574 0.076 Uiso 1 1 calc R . . H10B H 0.3790 0.1645 0.4121 0.076 Uiso 1 1 calc R . . H10C H 0.5113 0.1034 0.4177 0.076 Uiso 1 1 calc R . . C11 C 0.6909(3) 0.07844(17) 0.55280(15) 0.0307(6) Uani 1 1 d . . . H11 H 0.5912 0.0721 0.5634 0.037 Uiso 1 1 calc R . . C12 C 0.7692(3) 0.03246(18) 0.59551(16) 0.0325(6) Uani 1 1 d . . . H12 H 0.8688 0.0394 0.5815 0.039 Uiso 1 1 calc R . . C13 C 0.7201(3) -0.02737(17) 0.66133(16) 0.0313(6) Uani 1 1 d . . . C14 C 0.5765(3) -0.04322(19) 0.68922(16) 0.0349(7) Uani 1 1 d . . . H14 H 0.5068 -0.0147 0.6647 0.042 Uiso 1 1 calc R . . C15 C 0.5351(3) -0.10008(19) 0.75220(16) 0.0344(7) Uani 1 1 d . . . H15 H 0.4374 -0.1117 0.7695 0.041 Uiso 1 1 calc R . . C16 C 0.6345(3) -0.14080(17) 0.79084(15) 0.0302(6) Uani 1 1 d . . . C17 C 0.7780(3) -0.1250(2) 0.76291(17) 0.0406(8) Uani 1 1 d . . . H17 H 0.8473 -0.1527 0.7881 0.049 Uiso 1 1 calc R . . C18 C 0.8208(3) -0.0693(2) 0.69864(18) 0.0409(8) Uani 1 1 d . . . H18 H 0.9189 -0.0597 0.6800 0.049 Uiso 1 1 calc R . . C20 C 0.5875(3) -0.20097(16) 0.85991(15) 0.0293(6) Uani 1 1 d . . . C21 C 0.5358(3) -0.27360(17) 0.85339(16) 0.0330(6) Uani 1 1 d . . . C22 C 0.4169(3) -0.31210(18) 0.90049(17) 0.0365(7) Uani 1 1 d . . . H22 H 0.3686 -0.2927 0.9393 0.044 Uiso 1 1 calc R . . C23 C 0.3698(4) -0.37856(19) 0.89057(19) 0.0426(7) Uani 1 1 d . . . H23 H 0.2907 -0.4049 0.9234 0.051 Uiso 1 1 calc R . . C24 C 0.4357(4) -0.4067(2) 0.8340(2) 0.0488(9) Uani 1 1 d . . . H24 H 0.4011 -0.4515 0.8273 0.059 Uiso 1 1 calc R . . C25 C 0.5535(5) -0.3693(2) 0.78666(19) 0.0488(9) Uani 1 1 d . . . H25 H 0.6019 -0.3890 0.7481 0.059 Uiso 1 1 calc R . . C26 C 0.5985(4) -0.30330(19) 0.79673(17) 0.0409(7) Uani 1 1 d . . . H26 H 0.6766 -0.2768 0.7631 0.049 Uiso 1 1 calc R . . C30 C 0.5974(3) -0.18587(17) 0.92093(16) 0.0322(6) Uani 1 1 d . . . C31 C 0.6450(3) -0.10734(17) 0.91812(15) 0.0329(6) Uani 1 1 d . . . C32 C 0.7770(4) -0.1007(2) 0.93176(19) 0.0429(8) Uani 1 1 d . . . H32 H 0.8343 -0.1465 0.9453 0.051 Uiso 1 1 calc R . . C33 C 0.8255(4) -0.0279(2) 0.9258(2) 0.0499(9) Uani 1 1 d . . . H33 H 0.9170 -0.0240 0.9339 0.060 Uiso 1 1 calc R . . C34 C 0.7417(4) 0.0391(2) 0.9083(2) 0.0464(8) Uani 1 1 d . . . H34 H 0.7750 0.0889 0.9045 0.056 Uiso 1 1 calc R . . C35 C 0.6088(4) 0.03288(19) 0.89622(19) 0.0431(8) Uani 1 1 d . . . H35 H 0.5501 0.0786 0.8848 0.052 Uiso 1 1 calc R . . C36 C 0.5608(3) -0.03983(18) 0.90075(16) 0.0336(6) Uani 1 1 d . . . H36 H 0.4698 -0.0435 0.8919 0.040 Uiso 1 1 calc R . . C41 C 0.5619(3) -0.24178(18) 0.99279(16) 0.0322(6) Uani 1 1 d . . . C42 C 0.6138(4) -0.3190(2) 1.0066(2) 0.0460(8) Uani 1 1 d . . . H42 H 0.6740 -0.3375 0.9697 0.055 Uiso 1 1 calc R . . C43 C 0.5778(5) -0.3693(2) 1.0742(2) 0.0596(11) Uani 1 1 d . . . H43 H 0.6145 -0.4218 1.0833 0.071 Uiso 1 1 calc R . . C44 C 0.4894(5) -0.3437(3) 1.1284(2) 0.0619(11) Uani 1 1 d . . . H44 H 0.4641 -0.3786 1.1744 0.074 Uiso 1 1 calc R . . C45 C 0.4377(5) -0.2668(3) 1.11524(19) 0.0538(10) Uani 1 1 d . . . H45 H 0.3767 -0.2487 1.1521 0.065 Uiso 1 1 calc R . . C46 C 0.4758(4) -0.2160(2) 1.04741(17) 0.0392(7) Uani 1 1 d . . . H46 H 0.4421 -0.1629 1.0388 0.047 Uiso 1 1 calc R . . S2 S 0.41554(8) 0.65633(4) 0.45928(4) 0.0341(2) Uani 1 1 d . . . C51 C 0.3938(4) 0.73450(18) 0.38796(16) 0.0352(7) Uani 1 1 d . . . C52 C 0.4971(4) 0.7804(2) 0.3375(2) 0.0478(8) Uani 1 1 d . . . H52 H 0.5949 0.7707 0.3385 0.057 Uiso 1 1 calc R . . C53 C 0.4533(5) 0.8407(2) 0.2856(2) 0.0577(11) Uani 1 1 d . . . H53 H 0.5220 0.8732 0.2504 0.069 Uiso 1 1 calc R . . C54 C 0.3105(5) 0.8544(2) 0.2841(2) 0.0570(11) Uani 1 1 d . . . H54 H 0.2837 0.8960 0.2475 0.068 Uiso 1 1 calc R . . C55 C 0.2057(4) 0.80952(19) 0.33419(18) 0.0429(8) Uani 1 1 d . . . H55 H 0.1081 0.8197 0.3330 0.051 Uiso 1 1 calc R . . C56 C 0.2498(3) 0.74869(17) 0.38652(16) 0.0335(6) Uani 1 1 d . . . N57 N 0.1630(3) 0.69719(14) 0.44333(12) 0.0281(5) Uani 1 1 d . . . C58 C 0.2349(3) 0.64471(16) 0.48559(15) 0.0280(6) Uani 1 1 d . . . C59 C 0.0061(3) 0.70079(18) 0.45149(16) 0.0328(6) Uani 1 1 d . . . H59A H -0.0277 0.7562 0.4377 0.039 Uiso 1 1 calc R . . H59B H -0.0396 0.6777 0.5017 0.039 Uiso 1 1 calc R . . C60 C -0.0354(4) 0.6565(2) 0.4057(2) 0.0493(9) Uani 1 1 d . . . H60A H 0.0132 0.6779 0.3563 0.074 Uiso 1 1 calc R . . H60B H -0.1384 0.6618 0.4094 0.074 Uiso 1 1 calc R . . H60C H -0.0078 0.6009 0.4216 0.074 Uiso 1 1 calc R . . C61 C 0.1714(3) 0.58623(17) 0.54774(15) 0.0296(6) Uani 1 1 d . . . H61 H 0.0709 0.5829 0.5604 0.036 Uiso 1 1 calc R . . C62 C 0.2506(3) 0.53606(17) 0.58842(16) 0.0309(6) Uani 1 1 d . . . H62 H 0.3508 0.5391 0.5727 0.037 Uiso 1 1 calc R . . C63 C 0.1975(3) 0.47764(16) 0.65408(15) 0.0291(6) Uani 1 1 d . . . C64 C 0.2947(3) 0.42547(19) 0.68631(18) 0.0388(7) Uani 1 1 d . . . H64 H 0.3931 0.4288 0.6649 0.047 Uiso 1 1 calc R . . C65 C 0.2497(3) 0.36893(19) 0.74907(17) 0.0375(7) Uani 1 1 d . . . H65 H 0.3170 0.3325 0.7693 0.045 Uiso 1 1 calc R . . C66 C 0.1065(3) 0.36486(17) 0.78293(16) 0.0310(6) Uani 1 1 d . . . C67 C 0.0080(3) 0.41675(17) 0.75053(16) 0.0318(6) Uani 1 1 d . . . H67 H -0.0902 0.4139 0.7725 0.038 Uiso 1 1 calc R . . C68 C 0.0526(3) 0.47187(18) 0.68710(16) 0.0315(6) Uani 1 1 d . . . H68 H -0.0153 0.5064 0.6655 0.038 Uiso 1 1 calc R . . C70 C 0.0627(3) 0.30482(17) 0.85198(16) 0.0313(6) Uani 1 1 d . . . C71 C 0.1071(4) 0.22309(17) 0.84945(17) 0.0373(7) Uani 1 1 d . . . C72 C 0.0708(5) 0.1924(2) 0.80120(19) 0.0501(9) Uani 1 1 d . . . H72 H 0.0157 0.2241 0.7697 0.060 Uiso 1 1 calc R . . C73 C 0.1106(6) 0.1176(2) 0.7963(2) 0.0613(12) Uani 1 1 d . . . H73 H 0.0799 0.0971 0.7638 0.074 Uiso 1 1 calc R . . C74 C 0.1976(5) 0.0723(2) 0.8405(2) 0.0598(11) Uani 1 1 d . . . H74 H 0.2282 0.0209 0.8375 0.072 Uiso 1 1 calc R . . C75 C 0.2385(4) 0.1020(2) 0.8879(2) 0.0533(9) Uani 1 1 d . . . H75 H 0.2966 0.0709 0.9181 0.064 Uiso 1 1 calc R . . C76 C 0.1955(4) 0.1779(2) 0.89236(19) 0.0427(7) Uani 1 1 d . . . H76 H 0.2264 0.1987 0.9246 0.051 Uiso 1 1 calc R . . C80 C -0.0113(3) 0.32458(18) 0.91011(16) 0.0329(6) Uani 1 1 d . . . C81 C -0.0501(3) 0.40846(17) 0.90815(15) 0.0318(6) Uani 1 1 d . . . C82 C -0.1928(3) 0.4332(2) 0.92086(18) 0.0401(7) Uani 1 1 d . . . H82 H -0.2650 0.3959 0.9341 0.048 Uiso 1 1 calc R . . C83 C -0.2300(4) 0.5120(2) 0.9143(2) 0.0481(8) Uani 1 1 d . . . H83 H -0.3272 0.5288 0.9212 0.058 Uiso 1 1 calc R . . C84 C -0.1254(4) 0.5658(2) 0.89779(19) 0.0457(8) Uani 1 1 d . . . H84 H -0.1507 0.6197 0.8932 0.055 Uiso 1 1 calc R . . C85 C 0.0167(4) 0.5414(2) 0.88787(19) 0.0449(8) Uani 1 1 d . . . H85 H 0.0884 0.5785 0.8771 0.054 Uiso 1 1 calc R . . C86 C 0.0538(3) 0.46340(18) 0.89361(17) 0.0337(6) Uani 1 1 d . . . H86 H 0.1512 0.4469 0.8876 0.040 Uiso 1 1 calc R . . C91 C -0.0577(3) 0.26684(18) 0.98070(16) 0.0331(6) Uani 1 1 d . . . C92 C -0.1236(3) 0.19749(19) 0.98855(19) 0.0409(7) Uani 1 1 d . . . H92 H -0.1396 0.1854 0.9481 0.049 Uiso 1 1 calc R . . C93 C -0.1656(4) 0.1463(2) 1.0550(2) 0.0516(9) Uani 1 1 d . . . H93 H -0.2097 0.0991 1.0598 0.062 Uiso 1 1 calc R . . C94 C -0.1440(4) 0.1631(2) 1.1140(2) 0.0560(10) Uani 1 1 d . . . H94 H -0.1733 0.1276 1.1593 0.067 Uiso 1 1 calc R . . C95 C -0.0791(4) 0.2324(2) 1.10783(18) 0.0466(8) Uani 1 1 d . . . H95 H -0.0641 0.2439 1.1487 0.056 Uiso 1 1 calc R . . C96 C -0.0369(3) 0.28407(18) 1.04141(16) 0.0346(7) Uani 1 1 d . . . H96 H 0.0063 0.3314 1.0369 0.042 Uiso 1 1 calc R . . P1 P 0.69090(9) 0.55472(6) 0.59976(5) 0.0436(3) Uani 1 1 d D . . F1 F 0.6073(7) 0.5058(4) 0.5703(4) 0.0513(19) Uiso 0.40 1 d PD A 2 F1A F 0.6879(8) 0.4647(4) 0.6494(4) 0.0578(17) Uiso 0.40 1 d PD A 1 F1B F 0.6682(16) 0.4555(7) 0.6294(9) 0.066(4) Uiso 0.20 1 d PD A 3 F2 F 0.8421(2) 0.53195(14) 0.55812(13) 0.0543(6) Uani 1 1 d . A . F2A F 0.6115(5) 0.5267(4) 0.5489(4) 0.0285(11) Uiso 0.40 1 d PD A 1 F2B F 0.6275(17) 0.5560(11) 0.5352(8) 0.074(5) Uiso 0.20 1 d PD A 3 F3 F 0.6921(6) 0.6312(3) 0.5263(3) 0.0489(14) Uiso 0.40 1 d PD A 2 F3A F 0.6919(7) 0.6421(4) 0.5498(4) 0.0567(16) Uiso 0.40 1 d PD A 1 F3B F 0.7078(18) 0.6424(7) 0.5915(10) 0.084(4) Uiso 0.20 1 d PD A 3 F4 F 0.7778(6) 0.6128(4) 0.6238(3) 0.0455(12) Uiso 0.40 1 d PD A 2 F4A F 0.7662(6) 0.5795(4) 0.6515(4) 0.0542(14) Uiso 0.40 1 d PD A 1 F4B F 0.7407(11) 0.5338(7) 0.6782(5) 0.044(2) Uiso 0.20 1 d PD A 3 F5 F 0.5400(3) 0.5791(2) 0.64035(18) 0.0925(11) Uani 1 1 d . A . F6 F 0.6941(7) 0.4917(4) 0.6660(4) 0.0621(17) Uiso 0.40 1 d PD A 2 P2 P 0.78512(9) 0.94637(6) 0.39680(5) 0.0435(3) Uani 1 1 d D . . F11 F 0.7913(6) 0.8720(3) 0.4708(3) 0.0434(14) Uiso 0.40 1 d PD B 1 F11A F 0.7898(7) 0.8620(4) 0.4498(4) 0.0527(16) Uiso 0.40 1 d PD B 2 F11B F 0.7617(19) 0.8598(7) 0.4054(10) 0.087(4) Uiso 0.20 1 d PD B 3 F12 F 0.6942(6) 0.8871(4) 0.3764(3) 0.0444(12) Uiso 0.40 1 d PD B 1 F12A F 0.6995(7) 0.9167(5) 0.3514(4) 0.0616(17) Uiso 0.40 1 d PD B 2 F12B F 0.7298(14) 0.9697(9) 0.3208(6) 0.062(3) Uiso 0.20 1 d PD B 3 F13 F 0.7759(7) 1.0084(4) 0.3279(3) 0.0541(15) Uiso 0.40 1 d PD B 1 F13A F 0.7809(7) 1.0327(4) 0.3433(4) 0.0542(15) Uiso 0.40 1 d PD B 2 F13B F 0.8102(14) 1.0462(6) 0.3666(7) 0.056(3) Uiso 0.20 1 d PD B 3 F14 F 0.8706(7) 0.9995(4) 0.4212(4) 0.057(2) Uiso 0.40 1 d PD B 1 F14A F 0.8741(5) 0.9795(4) 0.4409(4) 0.0291(11) Uiso 0.40 1 d PD B 2 F14B F 0.860(2) 0.9471(13) 0.4567(9) 0.093(6) Uiso 0.20 1 d PD B 3 F15 F 0.6377(2) 0.97059(13) 0.44071(13) 0.0553(6) Uani 1 1 d . B . F16 F 0.9326(3) 0.9210(2) 0.35347(18) 0.0864(10) Uani 1 1 d . B . 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 S1 0.0277(4) 0.0340(4) 0.0297(4) 0.0016(3) -0.0046(3) -0.0055(3) C1 0.0380(16) 0.0294(14) 0.0250(14) -0.0029(11) -0.0017(12) -0.0067(12) C2 0.0423(18) 0.0420(18) 0.0341(17) -0.0041(14) 0.0055(14) -0.0091(14) C3 0.063(2) 0.0373(18) 0.0333(17) 0.0052(14) 0.0040(16) -0.0113(16) C4 0.074(3) 0.0350(18) 0.0362(18) 0.0067(14) -0.0103(17) -0.0055(17) C5 0.053(2) 0.0356(17) 0.0341(17) -0.0006(13) -0.0129(15) 0.0022(14) C6 0.0402(16) 0.0286(14) 0.0269(14) -0.0031(12) -0.0058(12) -0.0037(12) N7 0.0316(13) 0.0291(12) 0.0254(12) -0.0016(10) -0.0057(10) -0.0021(10) C8 0.0293(14) 0.0286(14) 0.0259(14) -0.0042(11) -0.0056(11) -0.0025(11) C9 0.0315(15) 0.0363(16) 0.0420(17) -0.0088(13) -0.0090(13) 0.0030(12) C10 0.047(2) 0.054(2) 0.059(2) -0.0174(18) -0.0223(18) -0.0011(16) C11 0.0311(14) 0.0325(14) 0.0252(14) -0.0021(11) -0.0039(11) -0.0080(11) C12 0.0292(14) 0.0361(16) 0.0267(14) -0.0017(12) -0.0006(11) -0.0086(12) C13 0.0328(15) 0.0289(14) 0.0277(14) -0.0018(11) -0.0030(12) -0.0061(11) C14 0.0339(16) 0.0393(16) 0.0276(15) 0.0018(12) -0.0088(12) -0.0103(13) C15 0.0323(15) 0.0404(16) 0.0264(14) -0.0014(12) -0.0026(12) -0.0135(12) C16 0.0330(15) 0.0286(14) 0.0243(14) -0.0034(11) 0.0000(11) -0.0052(11) C17 0.0291(15) 0.0439(18) 0.0328(16) 0.0095(13) -0.0004(12) -0.0008(13) C18 0.0262(15) 0.0450(18) 0.0371(17) 0.0079(14) -0.0015(13) -0.0034(13) C20 0.0298(14) 0.0273(14) 0.0248(14) -0.0034(11) 0.0021(11) -0.0039(11) C21 0.0401(16) 0.0264(14) 0.0287(15) -0.0026(11) -0.0055(12) -0.0017(12) C22 0.0339(15) 0.0367(16) 0.0354(16) -0.0064(13) -0.0046(13) -0.0024(12) C23 0.0429(18) 0.0382(17) 0.0441(18) -0.0036(14) -0.0102(14) -0.0094(14) C24 0.065(2) 0.0335(17) 0.051(2) -0.0058(15) -0.0241(18) -0.0045(15) C25 0.071(3) 0.0398(18) 0.0348(18) -0.0140(14) -0.0048(16) -0.0037(17) C26 0.0516(19) 0.0362(16) 0.0304(16) -0.0085(13) 0.0009(14) -0.0047(14) C30 0.0278(14) 0.0333(15) 0.0320(15) -0.0060(12) -0.0039(11) 0.0000(11) C31 0.0364(15) 0.0325(15) 0.0263(14) -0.0044(11) -0.0033(12) -0.0035(12) C32 0.0363(17) 0.0407(17) 0.050(2) -0.0063(15) -0.0143(15) -0.0007(13) C33 0.0401(18) 0.049(2) 0.062(2) -0.0111(17) -0.0170(17) -0.0076(15) C34 0.052(2) 0.0374(17) 0.051(2) -0.0114(15) -0.0105(16) -0.0135(15) C35 0.050(2) 0.0323(16) 0.0459(19) -0.0102(14) -0.0107(15) 0.0012(14) C36 0.0305(15) 0.0322(15) 0.0366(16) -0.0078(12) -0.0070(12) 0.0005(12) C41 0.0287(14) 0.0356(15) 0.0298(15) -0.0028(12) -0.0072(11) -0.0053(12) C42 0.0422(18) 0.0435(18) 0.0444(19) -0.0011(15) -0.0100(15) 0.0052(14) C43 0.057(2) 0.042(2) 0.068(3) 0.0152(18) -0.027(2) -0.0032(17) C44 0.067(3) 0.068(3) 0.042(2) 0.0142(18) -0.0232(19) -0.023(2) C45 0.063(2) 0.069(3) 0.0254(16) -0.0087(16) 0.0008(15) -0.019(2) C46 0.0471(18) 0.0398(17) 0.0276(15) -0.0066(13) -0.0024(13) -0.0075(14) S2 0.0278(4) 0.0336(4) 0.0352(4) -0.0020(3) -0.0032(3) -0.0051(3) C51 0.0403(17) 0.0317(15) 0.0295(15) -0.0058(12) 0.0004(13) -0.0084(13) C52 0.049(2) 0.0432(19) 0.0427(19) -0.0069(15) 0.0072(16) -0.0160(15) C53 0.073(3) 0.043(2) 0.040(2) 0.0014(16) 0.0113(18) -0.0183(19) C54 0.090(3) 0.0366(18) 0.0311(18) 0.0090(14) -0.0056(18) -0.0104(19) C55 0.058(2) 0.0340(16) 0.0306(16) -0.0003(13) -0.0090(15) -0.0015(15) C56 0.0439(17) 0.0274(14) 0.0248(14) -0.0027(11) -0.0022(12) -0.0062(12) N57 0.0293(12) 0.0288(12) 0.0235(11) -0.0026(9) -0.0052(9) -0.0028(9) C58 0.0289(14) 0.0266(13) 0.0273(14) -0.0044(11) -0.0068(11) -0.0024(11) C59 0.0297(15) 0.0349(15) 0.0337(15) -0.0071(12) -0.0099(12) 0.0005(12) C60 0.052(2) 0.054(2) 0.049(2) -0.0131(17) -0.0233(17) -0.0066(17) C61 0.0313(14) 0.0306(14) 0.0239(13) -0.0024(11) -0.0041(11) -0.0060(11) C62 0.0293(14) 0.0300(14) 0.0293(15) -0.0028(12) -0.0029(11) -0.0049(11) C63 0.0322(15) 0.0257(13) 0.0244(13) -0.0002(11) -0.0028(11) -0.0055(11) C64 0.0334(16) 0.0356(16) 0.0374(17) 0.0015(13) -0.0019(13) -0.0013(13) C65 0.0375(16) 0.0331(15) 0.0317(16) 0.0034(12) -0.0040(13) 0.0035(13) C66 0.0376(16) 0.0269(14) 0.0268(14) -0.0054(11) -0.0055(12) -0.0022(11) C67 0.0325(15) 0.0334(15) 0.0271(14) -0.0035(12) -0.0055(11) -0.0061(12) C68 0.0337(15) 0.0327(15) 0.0263(14) -0.0025(11) -0.0078(12) -0.0056(12) C70 0.0340(15) 0.0266(14) 0.0297(15) -0.0030(11) -0.0047(12) -0.0037(11) C71 0.0509(19) 0.0251(14) 0.0310(15) -0.0036(12) -0.0043(13) -0.0016(13) C72 0.081(3) 0.0370(18) 0.0347(18) -0.0077(14) -0.0204(18) -0.0017(17) C73 0.101(3) 0.042(2) 0.042(2) -0.0181(16) -0.001(2) -0.016(2) C74 0.073(3) 0.0328(18) 0.057(2) -0.0073(16) 0.012(2) 0.0010(17) C75 0.051(2) 0.0386(18) 0.057(2) -0.0041(16) -0.0010(17) 0.0123(16) C76 0.0400(17) 0.0421(18) 0.0422(18) -0.0084(14) -0.0081(14) 0.0057(14) C80 0.0313(15) 0.0338(15) 0.0343(16) -0.0077(12) -0.0088(12) -0.0042(12) C81 0.0339(15) 0.0334(15) 0.0261(14) -0.0049(11) -0.0066(11) -0.0004(12) C82 0.0335(16) 0.0432(18) 0.0412(18) -0.0092(14) -0.0055(13) -0.0029(13) C83 0.0393(18) 0.0470(19) 0.053(2) -0.0110(16) -0.0068(15) 0.0095(15) C84 0.052(2) 0.0362(17) 0.047(2) -0.0131(14) -0.0073(16) 0.0045(15) C85 0.051(2) 0.0395(18) 0.0458(19) -0.0137(15) -0.0085(15) -0.0059(15) C86 0.0318(15) 0.0331(15) 0.0370(16) -0.0104(12) -0.0075(12) -0.0016(12) C91 0.0314(14) 0.0341(15) 0.0297(15) -0.0035(12) -0.0043(11) -0.0019(12) C92 0.0359(16) 0.0364(16) 0.0464(19) -0.0074(14) -0.0035(14) -0.0064(13) C93 0.0417(19) 0.0375(18) 0.060(2) 0.0026(16) 0.0024(16) -0.0072(15) C94 0.047(2) 0.049(2) 0.044(2) 0.0146(16) 0.0066(16) 0.0055(16) C95 0.051(2) 0.052(2) 0.0267(16) -0.0025(14) -0.0040(14) 0.0122(16) C96 0.0376(16) 0.0330(15) 0.0296(15) -0.0041(12) -0.0072(12) 0.0028(12) P1 0.0263(4) 0.0553(5) 0.0573(6) -0.0295(4) -0.0105(4) 0.0065(4) F2 0.0272(10) 0.0641(14) 0.0680(15) -0.0212(11) -0.0022(9) 0.0062(9) F5 0.0350(12) 0.169(3) 0.107(2) -0.099(2) -0.0137(14) 0.0250(16) P2 0.0243(4) 0.0516(5) 0.0596(6) -0.0252(4) -0.0081(4) 0.0040(3) F15 0.0270(10) 0.0543(12) 0.0741(16) -0.0138(11) 0.0031(10) 0.0038(9) F16 0.0373(13) 0.144(3) 0.102(2) -0.084(2) -0.0093(13) 0.0198(15) _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 S1 C1 1.728(3) . ? S1 C8 1.719(3) . ? C1 C2 1.394(4) . ? C1 C6 1.388(5) . ? C2 C3 1.376(5) . ? C3 C4 1.394(6) . ? C4 C5 1.372(5) . ? C5 C6 1.398(4) . ? C6 N7 1.404(4) . ? N7 C8 1.331(4) . ? N7 C9 1.488(4) . ? C8 C11 1.440(4) . ? C9 C10 1.507(5) . ? C11 C12 1.330(4) . ? C12 C13 1.457(4) . ? C13 C14 1.396(4) . ? C13 C18 1.398(4) . ? C14 C15 1.382(4) . ? C15 C16 1.397(4) . ? C16 C17 1.396(4) . ? C16 C20 1.499(4) . ? C17 C18 1.391(4) . ? C20 C21 1.481(4) . ? C20 C30 1.359(4) . ? C21 C22 1.404(4) . ? C21 C26 1.383(4) . ? C22 C23 1.390(5) . ? C23 C24 1.372(5) . ? C24 C25 1.391(6) . ? C25 C26 1.375(5) . ? C30 C31 1.496(4) . ? C30 C41 1.492(4) . ? C31 C32 1.391(5) . ? C31 C36 1.391(4) . ? C32 C33 1.385(5) . ? C33 C34 1.384(5) . ? C34 C35 1.384(5) . ? C35 C36 1.390(5) . ? C41 C42 1.391(5) . ? C41 C46 1.380(5) . ? C42 C43 1.388(5) . ? C43 C44 1.381(7) . ? C44 C45 1.385(6) . ? C45 C46 1.398(5) . ? S2 C51 1.731(3) . ? S2 C58 1.719(3) . ? C51 C52 1.384(5) . ? C51 C56 1.398(5) . ? C52 C53 1.381(6) . ? C53 C54 1.386(7) . ? C54 C55 1.381(5) . ? C55 C56 1.392(4) . ? C56 N57 1.401(4) . ? N57 C58 1.335(4) . ? N57 C59 1.487(4) . ? C58 C61 1.434(4) . ? C59 C60 1.513(4) . ? C61 C62 1.342(4) . ? C62 C63 1.450(4) . ? C63 C64 1.394(4) . ? C63 C68 1.406(4) . ? C64 C65 1.382(4) . ? C65 C66 1.395(4) . ? C66 C67 1.402(4) . ? C66 C70 1.493(4) . ? C67 C68 1.378(4) . ? C70 C71 1.488(4) . ? C70 C80 1.344(4) . ? C71 C72 1.368(5) . ? C71 C76 1.395(5) . ? C72 C73 1.374(5) . ? C73 C74 1.402(7) . ? C74 C75 1.362(6) . ? C75 C76 1.395(5) . ? C80 C81 1.496(4) . ? C80 C91 1.499(4) . ? C81 C82 1.396(4) . ? C81 C86 1.395(4) . ? C82 C83 1.391(5) . ? C83 C84 1.380(5) . ? C84 C85 1.387(5) . ? C85 C86 1.380(5) . ? C91 C92 1.397(4) . ? C91 C96 1.406(4) . ? C92 C93 1.384(5) . ? C93 C94 1.371(6) . ? C94 C95 1.400(6) . ? C95 C96 1.388(5) . ? P1 F1 1.557(6) . ? P1 F1A 1.629(7) . ? P1 F1B 1.715(11) . ? P1 F2 1.587(2) . ? P1 F2A 1.621(5) . ? P1 F2B 1.557(12) . ? P1 F3 1.702(6) . ? P1 F3A 1.594(6) . ? P1 F3B 1.544(12) . ? P1 F4 1.631(5) . ? P1 F4A 1.580(6) . ? P1 F4B 1.693(9) . ? P1 F5 1.585(2) . ? P1 F6 1.484(6) . ? P2 F11 1.700(6) . ? P2 F11A 1.580(6) . ? P2 F11B 1.535(12) . ? P2 F12 1.629(5) . ? P2 F12A 1.589(6) . ? P2 F12B 1.669(10) . ? P2 F13 1.525(6) . ? P2 F13A 1.611(6) . ? P2 F13B 1.728(10) . ? P2 F14 1.559(7) . ? P2 F14A 1.625(5) . ? P2 F14B 1.548(13) . ? P2 F15 1.586(2) . ? P2 F16 1.589(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 C8 S1 C1 91.03(14) . . ? C2 C1 S1 128.0(3) . . ? C6 C1 S1 110.8(2) . . ? C6 C1 C2 121.2(3) . . ? C3 C2 C1 117.9(3) . . ? C2 C3 C4 120.6(3) . . ? C5 C4 C3 122.3(3) . . ? C4 C5 C6 117.2(3) . . ? C1 C6 C5 120.9(3) . . ? C1 C6 N7 112.0(3) . . ? C5 C6 N7 127.1(3) . . ? C6 N7 C9 120.8(2) . . ? C8 N7 C6 113.7(3) . . ? C8 N7 C9 125.5(3) . . ? N7 C8 S1 112.5(2) . . ? N7 C8 C11 125.9(3) . . ? C11 C8 S1 121.6(2) . . ? N7 C9 C10 111.0(3) . . ? C12 C11 C8 121.3(3) . . ? C11 C12 C13 127.7(3) . . ? C14 C13 C12 122.6(3) . . ? C14 C13 C18 118.8(3) . . ? C18 C13 C12 118.6(3) . . ? C15 C14 C13 120.4(3) . . ? C14 C15 C16 121.1(3) . . ? C15 C16 C20 120.5(3) . . ? C17 C16 C15 118.4(3) . . ? C17 C16 C20 121.1(3) . . ? C18 C17 C16 120.8(3) . . ? C17 C18 C13 120.4(3) . . ? C21 C20 C16 114.4(2) . . ? C30 C20 C16 119.2(3) . . ? C30 C20 C21 126.4(3) . . ? C22 C21 C20 122.5(3) . . ? C26 C21 C20 120.3(3) . . ? C26 C21 C22 117.0(3) . . ? C23 C22 C21 120.2(3) . . ? C24 C23 C22 121.0(3) . . ? C23 C24 C25 119.7(3) . . ? C26 C25 C24 118.7(3) . . ? C25 C26 C21 123.3(3) . . ? C20 C30 C31 119.2(3) . . ? C20 C30 C41 125.0(3) . . ? C41 C30 C31 115.8(3) . . ? C32 C31 C30 119.9(3) . . ? C32 C31 C36 118.7(3) . . ? C36 C31 C30 121.3(3) . . ? C33 C32 C31 120.5(3) . . ? C34 C33 C32 120.6(3) . . ? C33 C34 C35 119.3(3) . . ? C34 C35 C36 120.4(3) . . ? C35 C36 C31 120.5(3) . . ? C42 C41 C30 122.0(3) . . ? C46 C41 C30 119.1(3) . . ? C46 C41 C42 118.9(3) . . ? C43 C42 C41 120.2(4) . . ? C44 C43 C42 120.7(4) . . ? C43 C44 C45 119.5(3) . . ? C44 C45 C46 119.7(4) . . ? C41 C46 C45 120.9(3) . . ? C58 S2 C51 91.18(14) . . ? C52 C51 S2 128.4(3) . . ? C52 C51 C56 121.1(3) . . ? C56 C51 S2 110.5(2) . . ? C53 C52 C51 117.8(4) . . ? C52 C53 C54 120.9(3) . . ? C55 C54 C53 122.1(3) . . ? C54 C55 C56 117.0(4) . . ? C51 C56 N57 112.0(3) . . ? C55 C56 C51 121.0(3) . . ? C55 C56 N57 127.0(3) . . ? C56 N57 C59 121.1(2) . . ? C58 N57 C56 113.8(3) . . ? C58 N57 C59 125.0(2) . . ? N57 C58 S2 112.5(2) . . ? N57 C58 C61 124.9(3) . . ? C61 C58 S2 122.6(2) . . ? N57 C59 C60 110.3(3) . . ? C62 C61 C58 121.6(3) . . ? C61 C62 C63 126.2(3) . . ? C64 C63 C62 118.5(3) . . ? C64 C63 C68 118.5(3) . . ? C68 C63 C62 122.9(3) . . ? C65 C64 C63 120.8(3) . . ? C64 C65 C66 120.6(3) . . ? C65 C66 C67 118.8(3) . . ? C65 C66 C70 119.0(3) . . ? C67 C66 C70 122.1(3) . . ? C68 C67 C66 120.4(3) . . ? C67 C68 C63 120.7(3) . . ? C71 C70 C66 113.9(3) . . ? C80 C70 C66 121.7(3) . . ? C80 C70 C71 124.3(3) . . ? C72 C71 C70 120.7(3) . . ? C72 C71 C76 118.1(3) . . ? C76 C71 C70 121.0(3) . . ? C71 C72 C73 122.8(4) . . ? C72 C73 C74 118.4(4) . . ? C75 C74 C73 120.1(3) . . ? C74 C75 C76 120.5(4) . . ? C71 C76 C75 120.0(3) . . ? C70 C80 C81 120.8(3) . . ? C70 C80 C91 124.0(3) . . ? C81 C80 C91 115.2(3) . . ? C82 C81 C80 119.9(3) . . ? C86 C81 C80 121.4(3) . . ? C86 C81 C82 118.7(3) . . ? C83 C82 C81 120.4(3) . . ? C84 C83 C82 119.9(3) . . ? C83 C84 C85 120.2(3) . . ? C86 C85 C84 120.0(3) . . ? C85 C86 C81 120.7(3) . . ? C92 C91 C80 122.5(3) . . ? C92 C91 C96 118.9(3) . . ? C96 C91 C80 118.6(3) . . ? C93 C92 C91 120.3(3) . . ? C94 C93 C92 120.6(4) . . ? C93 C94 C95 120.5(3) . . ? C96 C95 C94 119.3(3) . . ? C95 C96 C91 120.5(3) . . ? F1 P1 F1A 71.8(4) . . ? F1 P1 F1B 53.5(6) . . ? F1 P1 F2 94.4(3) . . ? F1 P1 F2A 17.2(3) . . ? F1 P1 F2B 36.4(7) . . ? F1 P1 F3 90.2(4) . . ? F1 P1 F3A 106.7(4) . . ? F1 P1 F4 174.5(4) . . ? F1 P1 F4A 160.8(4) . . ? F1 P1 F4B 130.6(5) . . ? F1 P1 F5 85.8(3) . . ? F1A P1 F1B 18.8(5) . . ? F1A P1 F3 159.3(4) . . ? F1A P1 F4 113.7(4) . . ? F1A P1 F4B 60.2(5) . . ? F2 P1 F1A 86.6(3) . . ? F2 P1 F1B 84.8(5) . . ? F2 P1 F2A 91.4(2) . . ? F2 P1 F3 84.8(2) . . ? F2 P1 F3A 93.4(3) . . ? F2 P1 F4 85.2(2) . . ? F2 P1 F4B 94.1(4) . . ? F2A P1 F1A 88.5(4) . . ? F2A P1 F1B 69.9(6) . . ? F2A P1 F3 73.0(4) . . ? F2A P1 F4 157.3(4) . . ? F2A P1 F4B 147.8(5) . . ? F2B P1 F1A 107.4(8) . . ? F2B P1 F1B 88.7(9) . . ? F2B P1 F2 89.2(6) . . ? F2B P1 F2A 19.2(6) . . ? F2B P1 F3 53.7(8) . . ? F2B P1 F3A 71.0(8) . . ? F2B P1 F4 138.0(8) . . ? F2B P1 F4A 162.6(8) . . ? F2B P1 F4B 166.9(8) . . ? F2B P1 F5 90.4(6) . . ? F3 P1 F1B 141.1(6) . . ? F3A P1 F1A 178.5(5) . . ? F3A P1 F1B 159.7(6) . . ? F3A P1 F2A 90.0(4) . . ? F3A P1 F3 19.2(3) . . ? F3A P1 F4 67.9(4) . . ? F3A P1 F4B 121.3(5) . . ? F3B P1 F1 136.6(8) . . ? F3B P1 F1A 148.5(8) . . ? F3B P1 F1B 166.7(9) . . ? F3B P1 F2 101.3(6) . . ? F3B P1 F2A 121.3(8) . . ? F3B P1 F2B 103.1(10) . . ? F3B P1 F3 52.0(7) . . ? F3B P1 F3A 33.0(6) . . ? F3B P1 F4 38.5(7) . . ? F3B P1 F4A 60.3(7) . . ? F3B P1 F4B 88.6(8) . . ? F3B P1 F5 77.8(6) . . ? F4 P1 F1B 131.9(6) . . ? F4 P1 F3 84.3(3) . . ? F4 P1 F4B 55.0(4) . . ? F4A P1 F1A 89.7(4) . . ? F4A P1 F1B 108.4(6) . . ? F4A P1 F2 89.3(2) . . ? F4A P1 F2A 178.0(4) . . ? F4A P1 F3 108.9(4) . . ? F4A P1 F3A 91.8(4) . . ? F4A P1 F4 24.7(2) . . ? F4A P1 F4B 30.3(4) . . ? F4A P1 F5 90.8(2) . . ? F4B P1 F1B 79.0(7) . . ? F4B P1 F3 139.1(5) . . ? F5 P1 F1A 94.5(3) . . ? F5 P1 F1B 96.2(5) . . ? F5 P1 F2 178.9(2) . . ? F5 P1 F2A 88.6(2) . . ? F5 P1 F3 94.1(3) . . ? F5 P1 F3A 85.6(3) . . ? F5 P1 F4 94.4(2) . . ? F5 P1 F4B 86.5(4) . . ? F6 P1 F1 93.8(4) . . ? F6 P1 F1A 24.4(3) . . ? F6 P1 F1B 42.8(6) . . ? F6 P1 F2 95.3(3) . . ? F6 P1 F2A 111.0(4) . . ? F6 P1 F2B 130.2(8) . . ? F6 P1 F3 176.0(4) . . ? F6 P1 F3A 157.0(5) . . ? F6 P1 F3B 124.2(8) . . ? F6 P1 F4 91.7(4) . . ? F6 P1 F4A 67.1(4) . . ? F6 P1 F4B 36.9(4) . . ? F6 P1 F5 85.7(3) . . ? F11 P2 F13B 138.8(5) . . ? F11A P2 F11 17.3(3) . . ? F11A P2 F12 70.5(4) . . ? F11A P2 F12A 92.1(4) . . ? F11A P2 F12B 126.7(6) . . ? F11A P2 F13A 179.4(5) . . ? F11A P2 F13B 155.3(6) . . ? F11A P2 F14A 89.9(4) . . ? F11A P2 F15 93.4(3) . . ? F11A P2 F16 85.9(3) . . ? F11B P2 F11 54.6(7) . . ? F11B P2 F11A 37.7(7) . . ? F11B P2 F12 35.9(7) . . ? F11B P2 F12A 55.8(7) . . ? F11B P2 F12B 89.1(9) . . ? F11B P2 F13A 142.9(8) . . ? F11B P2 F13B 166.5(9) . . ? F11B P2 F14 141.3(8) . . ? F11B P2 F14A 126.1(8) . . ? F11B P2 F14B 105.8(11) . . ? F11B P2 F15 100.8(7) . . ? F11B P2 F16 78.6(7) . . ? F12 P2 F11 85.2(3) . . ? F12 P2 F12B 57.5(5) . . ? F12 P2 F13B 133.5(5) . . ? F12A P2 F11 107.1(4) . . ? F12A P2 F12 22.0(3) . . ? F12A P2 F12B 35.6(5) . . ? F12A P2 F13A 88.5(4) . . ? F12A P2 F13B 112.4(6) . . ? F12A P2 F14A 177.9(4) . . ? F12A P2 F16 91.5(3) . . ? F12B P2 F11 142.6(6) . . ? F12B P2 F13B 78.0(7) . . ? F13 P2 F11 175.4(4) . . ? F13 P2 F11A 158.3(4) . . ? F13 P2 F11B 120.9(8) . . ? F13 P2 F12 90.4(4) . . ? F13 P2 F12A 68.5(4) . . ? F13 P2 F12B 33.0(5) . . ? F13 P2 F13A 22.3(3) . . ? F13 P2 F13B 45.8(5) . . ? F13 P2 F14 93.2(4) . . ? F13 P2 F14A 109.5(4) . . ? F13 P2 F14B 130.6(9) . . ? F13 P2 F15 95.5(3) . . ? F13 P2 F16 85.1(3) . . ? F13A P2 F11 162.2(4) . . ? F13A P2 F12 110.1(4) . . ? F13A P2 F12B 53.9(5) . . ? F13A P2 F13B 24.1(4) . . ? F13A P2 F14A 89.5(4) . . ? F14 P2 F11 91.3(4) . . ? F14 P2 F11A 106.1(4) . . ? F14 P2 F12 176.3(4) . . ? F14 P2 F12A 161.6(5) . . ? F14 P2 F12B 126.1(6) . . ? F14 P2 F13A 73.3(4) . . ? F14 P2 F13B 49.7(6) . . ? F14 P2 F14A 16.3(3) . . ? F14 P2 F15 93.0(3) . . ? F14 P2 F16 87.3(3) . . ? F14A P2 F11 74.9(4) . . ? F14A P2 F12 160.1(4) . . ? F14A P2 F12B 142.4(6) . . ? F14A P2 F13B 65.7(6) . . ? F14B P2 F11 53.8(9) . . ? F14B P2 F11A 68.9(9) . . ? F14B P2 F12 139.0(9) . . ? F14B P2 F12A 160.9(9) . . ? F14B P2 F12B 163.3(10) . . ? F14B P2 F13A 110.5(9) . . ? F14B P2 F13B 86.5(10) . . ? F14B P2 F14 37.5(8) . . ? F14B P2 F14A 21.1(8) . . ? F14B P2 F15 90.6(7) . . ? F14B P2 F16 89.2(7) . . ? F15 P2 F11 85.4(2) . . ? F15 P2 F12 85.9(2) . . ? F15 P2 F12A 88.4(3) . . ? F15 P2 F12B 93.9(5) . . ? F15 P2 F13A 86.5(3) . . ? F15 P2 F13B 84.4(4) . . ? F15 P2 F14A 92.0(2) . . ? F15 P2 F16 179.3(2) . . ? F16 P2 F11 94.0(2) . . ? F16 P2 F12 93.8(2) . . ? F16 P2 F12B 86.5(5) . . ? F16 P2 F13A 94.2(3) . . ? F16 P2 F13B 96.3(4) . . ? F16 P2 F14A 88.0(2) . . ? data_na3cult _database_code_depnum_ccdc_archive 'CCDC 883790' #TrackingRef 'na3cult.cif' _audit_creation_date 2011-12-12 _audit_creation_method ; Olex2 1.1-beta (compiled Nov 1 2011 20:42:30, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C37 H30 N S, F6 P, 0.5(C4 H8 O), C4 O' _chemical_formula_sum 'C43 H42 F6 N O1.50 P S' _chemical_formula_weight 773.81 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 9.7467(4) _cell_length_b 17.3887(8) _cell_length_c 23.8490(10) _cell_angle_alpha 72.962(4) _cell_angle_beta 85.952(3) _cell_angle_gamma 83.053(4) _cell_volume 3833.6(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 7069 _cell_measurement_temperature 173.00(14) _cell_measurement_theta_max 71.5033 _cell_measurement_theta_min 3.8766 _exptl_absorpt_coefficient_mu 1.707 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.74292 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.341 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1616 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.06 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_unetI/netI 0.0521 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 22938 _diffrn_reflns_theta_full 66.50 _diffrn_reflns_theta_max 66.75 _diffrn_reflns_theta_min 3.88 _diffrn_ambient_temperature 173.00(14) _diffrn_detector_area_resol_mean 15.9578 _diffrn_measured_fraction_theta_full 0.975 _diffrn_measured_fraction_theta_max 0.975 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -121.00 -55.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 178.0000 -60.0000 66 #__ type_ start__ end____ width___ exp.time_ 2 omega -20.00 21.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -57.0000 -30.0000 41 #__ type_ start__ end____ width___ exp.time_ 3 omega -67.00 -25.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -57.0000 -30.0000 42 #__ type_ start__ end____ width___ exp.time_ 4 omega 74.00 104.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 125.0000 -90.0000 30 #__ type_ start__ end____ width___ exp.time_ 5 omega -3.00 83.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 -125.0000 -30.0000 86 #__ type_ start__ end____ width___ exp.time_ 6 omega -15.00 82.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 -77.0000 90.0000 97 #__ type_ start__ end____ width___ exp.time_ 7 omega 29.00 119.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 77.0000 -150.0000 90 #__ type_ start__ end____ width___ exp.time_ 8 omega -130.00 -41.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 -64.0000 0.0000 89 #__ type_ start__ end____ width___ exp.time_ 9 omega 38.00 148.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 -120.0000 110 #__ type_ start__ end____ width___ exp.time_ 10 omega 38.00 69.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 60.0000 31 #__ type_ start__ end____ width___ exp.time_ 11 omega 44.00 71.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 0.0000 27 #__ type_ start__ end____ width___ exp.time_ 12 omega 37.00 66.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 -30.0000 29 #__ type_ start__ end____ width___ exp.time_ 13 omega 39.00 105.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 30.0000 66 #__ type_ start__ end____ width___ exp.time_ 14 omega 42.00 72.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 -180.0000 30 #__ type_ start__ end____ width___ exp.time_ 15 omega 39.00 70.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 -90.0000 31 #__ type_ start__ end____ width___ exp.time_ 16 omega 89.00 177.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 50.0000 0.0000 88 #__ type_ start__ end____ width___ exp.time_ 17 omega 42.00 71.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 90.0000 29 #__ type_ start__ end____ width___ exp.time_ 18 omega 37.00 62.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 -150.0000 25 #__ type_ start__ end____ width___ exp.time_ 19 omega 41.00 71.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 120.0000 30 #__ type_ start__ end____ width___ exp.time_ 20 omega 38.00 71.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 -120.0000 33 #__ type_ start__ end____ width___ exp.time_ 21 omega 123.00 148.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 30.0000 25 #__ type_ start__ end____ width___ exp.time_ 22 omega 38.00 147.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 90.0000 109 #__ type_ start__ end____ width___ exp.time_ 23 omega 38.00 174.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 12.0000 150.0000 136 ; _diffrn_measurement_device 'kappa diffractometer' _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0466094000 _diffrn_orient_matrix_UB_12 0.0568185000 _diffrn_orient_matrix_UB_13 0.0321741000 _diffrn_orient_matrix_UB_21 -0.1522273000 _diffrn_orient_matrix_UB_22 0.0246593000 _diffrn_orient_matrix_UB_23 0.0149444000 _diffrn_orient_matrix_UB_31 0.0065398000 _diffrn_orient_matrix_UB_32 -0.0696124000 _diffrn_orient_matrix_UB_33 0.0575528000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.5418 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40 _diffrn_source_power 2.0 _diffrn_source_target Cu _diffrn_source_voltage 50 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 9945 _reflns_number_total 13263 _reflns_odcompleteness_completeness 98.01 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 68.13 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; XS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.549 _refine_diff_density_min -0.456 _refine_diff_density_rms 0.070 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 984 _refine_ls_number_reflns 13263 _refine_ls_number_restraints 78 _refine_ls_R_factor_all 0.0859 _refine_ls_R_factor_gt 0.0680 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0986P)^2^+2.2000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1762 _refine_ls_wR_factor_ref 0.1897 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 S1 S 0.66095(7) 0.87708(4) 0.53024(3) 0.03110(17) Uani 1 1 d . . . C1 C 0.5993(3) 0.91284(16) 0.58906(12) 0.0310(6) Uani 1 1 d . . . C2 C 0.6755(3) 0.92966(18) 0.63064(13) 0.0405(7) Uani 1 1 d . . . H2 H 0.7737 0.9220 0.6294 0.049 Uiso 1 1 calc R . . C3 C 0.6035(4) 0.95765(19) 0.67334(14) 0.0458(8) Uani 1 1 d . . . H3 H 0.6527 0.9687 0.7026 0.055 Uiso 1 1 calc R . . C4 C 0.4593(4) 0.97034(18) 0.67477(13) 0.0422(7) Uani 1 1 d . . . H4 H 0.4126 0.9903 0.7048 0.051 Uiso 1 1 calc R . . C5 C 0.3825(3) 0.95456(17) 0.63336(12) 0.0376(6) Uani 1 1 d . . . H5 H 0.2843 0.9633 0.6344 0.045 Uiso 1 1 calc R . . C6 C 0.4558(3) 0.92523(15) 0.59002(11) 0.0285(5) Uani 1 1 d . . . N7 N 0.4004(2) 0.90702(13) 0.54339(9) 0.0258(4) Uani 1 1 d . . . C8 C 0.4951(3) 0.88068(15) 0.50834(11) 0.0263(5) Uani 1 1 d . . . C9 C 0.2482(3) 0.91721(16) 0.53606(12) 0.0312(6) Uani 1 1 d . . . H9B H 0.2295 0.9224 0.4948 0.037 Uiso 1 1 calc R . . H9C H 0.2076 0.9675 0.5450 0.037 Uiso 1 1 calc R . . C10 C 0.1810(3) 0.84620(19) 0.57606(15) 0.0434(7) Uani 1 1 d . . . H10B H 0.2204 0.7965 0.5670 0.065 Uiso 1 1 calc R . . H10C H 0.0812 0.8544 0.5702 0.065 Uiso 1 1 calc R . . H10D H 0.1978 0.8417 0.6170 0.065 Uiso 1 1 calc R . . C11 C 0.4663(3) 0.85952(15) 0.45674(11) 0.0280(5) Uani 1 1 d . . . H11 H 0.3729 0.8595 0.4477 0.034 Uiso 1 1 calc R . . C12 C 0.5685(3) 0.83973(16) 0.42091(11) 0.0301(6) Uani 1 1 d . . . H12 H 0.6603 0.8369 0.4329 0.036 Uiso 1 1 calc R . . C13 C 0.5534(3) 0.82219(16) 0.36568(11) 0.0284(5) Uani 1 1 d . . . C14 C 0.6725(3) 0.80503(19) 0.33333(12) 0.0362(6) Uani 1 1 d . . . H14 H 0.7608 0.8017 0.3488 0.043 Uiso 1 1 calc R . . C15 C 0.6630(3) 0.79275(19) 0.27868(13) 0.0376(6) Uani 1 1 d . . . H15 H 0.7451 0.7818 0.2571 0.045 Uiso 1 1 calc R . . C16 C 0.5357(3) 0.79624(15) 0.25541(11) 0.0279(5) Uani 1 1 d . . . C17 C 0.4174(3) 0.81080(18) 0.28856(12) 0.0339(6) Uani 1 1 d . . . H17 H 0.3292 0.8115 0.2737 0.041 Uiso 1 1 calc R . . C18 C 0.4250(3) 0.82412(17) 0.34222(12) 0.0325(6) Uani 1 1 d . . . H18 H 0.3424 0.8347 0.3636 0.039 Uiso 1 1 calc R . . C20 C 0.5262(3) 0.78428(16) 0.19614(11) 0.0280(5) Uani 1 1 d . . . C21 C 0.4752(3) 0.70696(17) 0.19665(12) 0.0338(6) Uani 1 1 d . . . C22 C 0.3959(3) 0.69895(19) 0.15229(14) 0.0405(7) Uani 1 1 d . . . H22 H 0.3747 0.7444 0.1194 0.049 Uiso 1 1 calc R . . C23 C 0.3478(4) 0.6263(2) 0.15542(16) 0.0506(8) Uani 1 1 d . . . H23 H 0.2965 0.6220 0.1242 0.061 Uiso 1 1 calc R . . C24 C 0.3734(4) 0.5601(2) 0.20307(18) 0.0546(9) Uani 1 1 d . . . H24 H 0.3385 0.5106 0.2053 0.066 Uiso 1 1 calc R . . C25 C 0.4501(4) 0.5660(2) 0.24775(17) 0.0548(9) Uani 1 1 d . . . H25 H 0.4690 0.5203 0.2807 0.066 Uiso 1 1 calc R . . C26 C 0.4997(3) 0.63893(18) 0.24440(13) 0.0396(7) Uani 1 1 d . . . H26 H 0.5518 0.6424 0.2756 0.048 Uiso 1 1 calc R . . C30 C 0.5646(3) 0.84229(17) 0.14746(12) 0.0330(6) Uani 1 1 d . . . C31 C 0.6024(3) 0.92108(17) 0.15185(12) 0.0337(6) Uani 1 1 d . . . C32 C 0.5071(3) 0.97347(17) 0.17195(12) 0.0350(6) Uani 1 1 d . . . H32 H 0.4164 0.9585 0.1834 0.042 Uiso 1 1 calc R . . C33 C 0.5395(4) 1.04685(18) 0.17585(13) 0.0449(8) Uani 1 1 d . . . H33 H 0.4713 1.0827 0.1885 0.054 Uiso 1 1 calc R . . C34 C 0.6741(4) 1.0675(2) 0.16089(15) 0.0523(9) Uani 1 1 d . . . H34 H 0.6995 1.1165 0.1650 0.063 Uiso 1 1 calc R . . C35 C 0.7705(4) 1.0161(2) 0.14002(16) 0.0528(9) Uani 1 1 d . . . H35 H 0.8619 1.0302 0.1296 0.063 Uiso 1 1 calc R . . C36 C 0.7338(3) 0.94418(19) 0.13436(14) 0.0437(7) Uani 1 1 d . . . H36 H 0.7992 0.9104 0.1184 0.052 Uiso 1 1 calc R . . C41 C 0.5722(3) 0.83415(16) 0.08674(12) 0.0343(6) Uani 1 1 d . . . C42 C 0.6561(4) 0.7720(2) 0.07163(14) 0.0456(7) Uani 1 1 d . . . H42 H 0.7130 0.7345 0.1002 0.055 Uiso 1 1 calc R . . C43 C 0.6579(4) 0.7640(2) 0.01546(16) 0.0561(9) Uani 1 1 d . . . H43 H 0.7163 0.7217 0.0055 0.067 Uiso 1 1 calc R . . C44 C 0.5739(4) 0.8181(2) -0.02617(15) 0.0571(9) Uani 1 1 d . . . H44 H 0.5717 0.8114 -0.0642 0.069 Uiso 1 1 calc R . . C45 C 0.4942(4) 0.8808(2) -0.01266(14) 0.0513(8) Uani 1 1 d . . . H45 H 0.4391 0.9187 -0.0417 0.062 Uiso 1 1 calc R . . C46 C 0.4937(4) 0.88925(18) 0.04380(13) 0.0414(7) Uani 1 1 d . . . H46 H 0.4388 0.9334 0.0528 0.050 Uiso 1 1 calc R . . S1A S -0.15688(7) 0.63091(4) 0.46836(3) 0.03552(18) Uani 1 1 d . . . C1A C -0.0979(3) 0.59135(17) 0.41102(13) 0.0363(6) Uani 1 1 d . . . C2A C -0.1769(4) 0.5762(2) 0.36921(13) 0.0462(8) Uani 1 1 d . . . H2A H -0.2748 0.5873 0.3696 0.055 Uiso 1 1 calc R . . C3A C -0.1072(5) 0.5446(2) 0.32781(14) 0.0532(9) Uani 1 1 d . . . H3A H -0.1573 0.5346 0.2984 0.064 Uiso 1 1 calc R . . C4A C 0.0361(4) 0.52686(19) 0.32800(14) 0.0507(9) Uani 1 1 d . . . H4A H 0.0810 0.5049 0.2986 0.061 Uiso 1 1 calc R . . C5A C 0.1147(4) 0.54004(18) 0.36919(13) 0.0436(7) Uani 1 1 d . . . H5A H 0.2123 0.5273 0.3691 0.052 Uiso 1 1 calc R . . C6A C 0.0441(3) 0.57317(16) 0.41146(12) 0.0337(6) Uani 1 1 d . . . N7A N 0.1016(2) 0.59044(13) 0.45819(10) 0.0306(5) Uani 1 1 d . . . C8A C 0.0088(3) 0.62146(16) 0.49163(12) 0.0304(6) Uani 1 1 d . . . C9A C 0.0397(3) 0.64148(16) 0.54341(11) 0.0312(6) Uani 1 1 d . . . H9A H 0.1334 0.6358 0.5540 0.037 Uiso 1 1 calc R . . C10A C -0.0600(3) 0.66800(16) 0.57727(11) 0.0316(6) Uani 1 1 d . . . H10A H -0.1514 0.6780 0.5635 0.038 Uiso 1 1 calc R . . C11A C -0.0410(3) 0.68273(16) 0.63302(11) 0.0292(6) Uani 1 1 d . . . C12A C -0.1528(3) 0.71678(17) 0.66072(12) 0.0354(6) Uani 1 1 d . . . H12A H -0.2393 0.7314 0.6423 0.042 Uiso 1 1 calc R . . C13A C -0.1402(3) 0.72968(17) 0.71447(12) 0.0356(6) Uani 1 1 d . . . H13A H -0.2164 0.7554 0.7316 0.043 Uiso 1 1 calc R . . C14A C -0.0165(3) 0.70530(15) 0.74390(11) 0.0290(6) Uani 1 1 d . . . C15A C 0.0959(3) 0.67222(17) 0.71573(12) 0.0325(6) Uani 1 1 d . . . H15A H 0.1815 0.6564 0.7347 0.039 Uiso 1 1 calc R . . C16A C 0.0858(3) 0.66194(17) 0.66119(12) 0.0314(6) Uani 1 1 d . . . H16A H 0.1646 0.6408 0.6425 0.038 Uiso 1 1 calc R . . C20A C -0.0063(3) 0.71637(16) 0.80324(12) 0.0300(6) Uani 1 1 d . . . C21A C -0.0479(3) 0.80023(17) 0.80603(13) 0.0358(6) Uani 1 1 d . . . C22A C -0.1368(3) 0.81620(18) 0.85060(14) 0.0415(7) Uani 1 1 d . . . H22A H -0.1713 0.7726 0.8803 0.050 Uiso 1 1 calc R . . C23A C -0.1757(4) 0.8950(2) 0.85209(16) 0.0468(8) Uani 1 1 d . . . H23A H -0.2356 0.9053 0.8829 0.056 Uiso 1 1 calc R . . C24A C -0.1266(4) 0.95872(19) 0.80852(17) 0.0522(9) Uani 1 1 d . . . H24A H -0.1538 1.0128 0.8093 0.063 Uiso 1 1 calc R . . C25A C -0.0390(4) 0.9443(2) 0.76430(16) 0.0516(8) Uani 1 1 d . . . H25A H -0.0038 0.9882 0.7352 0.062 Uiso 1 1 calc R . . C26A C -0.0017(3) 0.86567(18) 0.76209(14) 0.0413(7) Uani 1 1 d . . . H26A H 0.0557 0.8562 0.7304 0.050 Uiso 1 1 calc R . . C30A C 0.0407(3) 0.65476(17) 0.84926(12) 0.0334(6) Uani 1 1 d . . . C31A C 0.0632(3) 0.66562(17) 0.90746(13) 0.0383(7) Uani 1 1 d . . . C32A C 0.0033(4) 0.6172(2) 0.95809(13) 0.0470(8) Uani 1 1 d . . . H32A H -0.0491 0.5760 0.9552 0.056 Uiso 1 1 calc R . . C33A C 0.0179(5) 0.6274(3) 1.01240(16) 0.0648(11) Uani 1 1 d . . . H33A H -0.0249 0.5943 1.0465 0.078 Uiso 1 1 calc R . . C34A C 0.0957(6) 0.6867(3) 1.01655(19) 0.0858(17) Uani 1 1 d . . . H34A H 0.1040 0.6954 1.0536 0.103 Uiso 1 1 calc R . . C35A C 0.1619(5) 0.7339(3) 0.9673(2) 0.0748(13) Uani 1 1 d . . . H35A H 0.2186 0.7728 0.9710 0.090 Uiso 1 1 calc R . . C36A C 0.1449(4) 0.7241(2) 0.91287(16) 0.0526(9) Uani 1 1 d . . . H36A H 0.1888 0.7570 0.8790 0.063 Uiso 1 1 calc R . . C41A C 0.0721(3) 0.57031(16) 0.84545(12) 0.0334(6) Uani 1 1 d . . . C42A C -0.0238(3) 0.53029(17) 0.82770(12) 0.0334(6) Uani 1 1 d . . . H42A H -0.1147 0.5564 0.8197 0.040 Uiso 1 1 calc R . . C43A C 0.0083(3) 0.45412(17) 0.82136(13) 0.0387(7) Uani 1 1 d . . . H43A H -0.0601 0.4276 0.8100 0.046 Uiso 1 1 calc R . . C44A C 0.1419(4) 0.41631(18) 0.83167(13) 0.0429(7) Uani 1 1 d . . . H44A H 0.1666 0.3649 0.8252 0.051 Uiso 1 1 calc R . . C45A C 0.2393(4) 0.45349(19) 0.85137(15) 0.0469(8) Uani 1 1 d . . . H45A H 0.3298 0.4270 0.8597 0.056 Uiso 1 1 calc R . . C46A C 0.2035(3) 0.52970(18) 0.85874(14) 0.0410(7) Uani 1 1 d . . . H46A H 0.2694 0.5546 0.8731 0.049 Uiso 1 1 calc R . . C65 C 0.2526(3) 0.57614(18) 0.46661(13) 0.0373(6) Uani 1 1 d . . . H65A H 0.2896 0.5253 0.4576 0.045 Uiso 1 1 calc R . . H65B H 0.2705 0.5698 0.5081 0.045 Uiso 1 1 calc R . . C96 C 0.3265(4) 0.6455(2) 0.42738(17) 0.0521(8) Uani 1 1 d . . . H96A H 0.3124 0.6502 0.3862 0.078 Uiso 1 1 calc R . . H96B H 0.4256 0.6351 0.4348 0.078 Uiso 1 1 calc R . . H96C H 0.2892 0.6960 0.4359 0.078 Uiso 1 1 calc R . . P1 P 0.50426(8) 0.36803(5) 0.40846(4) 0.0458(2) Uani 1 1 d D . . F1 F 0.3717(2) 0.40651(16) 0.36962(12) 0.0833(8) Uani 1 1 d D A . F2 F 0.6355(2) 0.32788(14) 0.44661(10) 0.0593(5) Uani 1 1 d D A . F3 F 0.5938(5) 0.3956(3) 0.3455(2) 0.0438(12) Uiso 0.40 1 d PD A 2 F3A F 0.6027(6) 0.4176(4) 0.3599(3) 0.0644(15) Uiso 0.45 1 d PD A 1 F3B F 0.6086(11) 0.4394(6) 0.3883(5) 0.038(2) Uiso 0.15 1 d PD A 3 F4 F 0.4979(7) 0.2830(3) 0.3928(3) 0.0526(18) Uiso 0.40 1 d PD A 2 F4A F 0.5302(7) 0.2952(4) 0.3780(3) 0.0561(16) Uiso 0.45 1 d PD A 1 F4B F 0.5670(13) 0.3358(9) 0.3593(5) 0.046(3) Uiso 0.15 1 d PD A 3 F5 F 0.4116(8) 0.3387(5) 0.4643(3) 0.076(2) Uiso 0.40 1 d PD A 2 F5A F 0.4025(4) 0.3122(3) 0.4562(2) 0.0386(10) Uiso 0.45 1 d PD A 1 F5B F 0.4132(14) 0.2983(8) 0.4355(7) 0.049(4) Uiso 0.15 1 d PD A 3 F6 F 0.5052(7) 0.4549(4) 0.4138(3) 0.0736(19) Uiso 0.40 1 d PD A 2 F6A F 0.4813(6) 0.4354(4) 0.4413(3) 0.0675(15) Uiso 0.45 1 d PD A 1 F6B F 0.4558(11) 0.4078(7) 0.4672(5) 0.034(2) Uiso 0.15 1 d PD A 3 P2 P 0.01532(7) 0.87298(5) 0.41094(4) 0.0391(2) Uani 1 1 d D . . F11 F -0.1078(2) 0.92101(15) 0.36985(11) 0.0745(7) Uani 1 1 d D B . F12 F 0.13844(19) 0.82389(12) 0.45128(9) 0.0510(5) Uani 1 1 d D B . F13 F 0.0131(6) 0.7940(3) 0.3860(2) 0.0459(15) Uiso 0.45 1 d PD B 2 F13A F 0.0423(7) 0.8096(4) 0.3742(3) 0.0435(15) Uiso 0.40 1 d PD B 1 F13B F 0.0695(16) 0.8448(11) 0.3581(6) 0.061(4) Uiso 0.15 1 d PD B 3 F14 F -0.0913(7) 0.8375(4) 0.4600(3) 0.063(2) Uiso 0.45 1 d PD B 2 F14A F -0.0936(6) 0.8158(4) 0.4548(3) 0.0385(15) Uiso 0.40 1 d PD B 1 F14B F -0.0968(14) 0.8107(9) 0.4372(7) 0.045(4) Uiso 0.15 1 d PD B 3 F15 F 0.0198(6) 0.9529(4) 0.4278(3) 0.0671(18) Uiso 0.45 1 d PD B 2 F15A F -0.0065(7) 0.9352(4) 0.4495(3) 0.0458(13) Uiso 0.40 1 d PD B 1 F15B F -0.0295(11) 0.9135(7) 0.4689(5) 0.028(3) Uiso 0.15 1 d PD B 3 F16 F 0.1193(5) 0.9088(3) 0.3534(2) 0.0491(13) Uiso 0.45 1 d PD B 2 F16A F 0.1266(6) 0.9248(4) 0.3706(3) 0.0537(15) Uiso 0.40 1 d PD B 1 F16B F 0.1276(12) 0.9385(7) 0.3953(6) 0.040(3) Uiso 0.15 1 d PD B 3 O1S O 1.0104(3) 0.28569(16) 0.77877(13) 0.0681(8) Uani 1 1 d . . . C2S C 0.9746(4) 0.2323(2) 0.83392(16) 0.0533(9) Uani 1 1 d . . . H2SA H 0.9058 0.2608 0.8555 0.064 Uiso 1 1 calc R . . H2SB H 1.0576 0.2126 0.8578 0.064 Uiso 1 1 calc R . . C3S C 0.9139(4) 0.1614(2) 0.82302(16) 0.0520(8) Uani 1 1 d . . . H3SA H 0.9510 0.1093 0.8501 0.062 Uiso 1 1 calc R . . H3SB H 0.8117 0.1672 0.8272 0.062 Uiso 1 1 calc R . . C4S C 0.9620(3) 0.16793(19) 0.76009(15) 0.0428(7) Uani 1 1 d . . . H4SA H 1.0564 0.1404 0.7579 0.051 Uiso 1 1 calc R . . H4SB H 0.8979 0.1452 0.7403 0.051 Uiso 1 1 calc R . . C5S C 0.9592(4) 0.2579(2) 0.73417(16) 0.0509(8) Uani 1 1 d . . . H5SA H 1.0190 0.2712 0.6981 0.061 Uiso 1 1 calc R . . H5SB H 0.8638 0.2829 0.7245 0.061 Uiso 1 1 calc R . . O6S O 0.4942(6) 0.3434(3) 0.2355(2) 0.1231(15) Uani 1 1 d . C . C7S C 0.4350(7) 0.3550(3) 0.1762(3) 0.0961(17) Uani 1 1 d . C . C8S C 0.4872(9) 0.2737(5) 0.1638(3) 0.130(3) Uani 1 1 d . . . C9S C 0.5974(8) 0.2358(5) 0.2065(3) 0.0551(17) Uiso 0.50 1 d P C 2 C9SA C 0.4827(10) 0.2196(6) 0.2156(5) 0.074(2) Uiso 0.50 1 d P C 1 C10S C 0.5495(6) 0.2534(3) 0.2559(3) 0.0881(15) Uani 1 1 d . . . O11S O -0.0461(15) 0.9218(8) 0.9933(6) 0.170(5) Uiso 0.50 1 d PD . . C12S C -0.097(2) 1.0087(12) 0.9638(9) 0.133(7) Uiso 0.50 1 d PD . . C13S C -0.014(2) 1.0647(12) 0.9757(9) 0.153(7) Uiso 0.50 1 d PD . . C14S C 0.099(2) 1.0131(11) 1.0138(9) 0.125(6) Uiso 0.50 1 d PD . . C15S C 0.0894(18) 0.9326(9) 1.0147(7) 0.117(5) Uiso 0.50 1 d PD . . O16S O 0.3929(14) 0.4327(8) 0.0174(6) 0.161(4) Uiso 0.50 1 d PD . . C17S C 0.358(2) 0.5018(13) 0.0284(10) 0.149(8) Uiso 0.50 1 d PD . . C18S C 0.4962(16) 0.5395(12) 0.0244(7) 0.126(5) Uiso 0.50 1 d PD . . C19S C 0.5997(19) 0.4825(9) -0.0058(8) 0.117(5) Uiso 0.50 1 d PD . . C20S C 0.5111(18) 0.4166(11) -0.0080(8) 0.133(6) Uiso 0.50 1 d PD . . 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 S1 0.0281(3) 0.0380(4) 0.0303(3) -0.0136(3) -0.0030(3) -0.0050(3) C1 0.0378(15) 0.0288(13) 0.0287(13) -0.0101(11) -0.0049(11) -0.0047(11) C2 0.0470(18) 0.0402(16) 0.0378(16) -0.0132(13) -0.0106(13) -0.0078(13) C3 0.066(2) 0.0435(17) 0.0330(16) -0.0152(13) -0.0118(15) -0.0087(15) C4 0.066(2) 0.0356(15) 0.0272(14) -0.0123(12) -0.0013(14) -0.0030(14) C5 0.0498(18) 0.0311(14) 0.0320(15) -0.0104(12) 0.0011(13) -0.0030(12) C6 0.0375(14) 0.0249(12) 0.0231(12) -0.0060(10) -0.0044(11) -0.0045(10) N7 0.0288(11) 0.0266(10) 0.0221(10) -0.0067(8) -0.0009(8) -0.0042(8) C8 0.0271(13) 0.0252(12) 0.0258(13) -0.0052(10) -0.0013(10) -0.0046(10) C9 0.0291(14) 0.0317(13) 0.0323(14) -0.0088(11) -0.0022(11) -0.0015(11) C10 0.0373(16) 0.0448(17) 0.0475(18) -0.0107(14) 0.0042(13) -0.0123(13) C11 0.0294(13) 0.0315(13) 0.0242(13) -0.0078(11) -0.0031(10) -0.0061(10) C12 0.0299(13) 0.0346(14) 0.0270(13) -0.0089(11) -0.0040(11) -0.0063(11) C13 0.0309(14) 0.0289(13) 0.0265(13) -0.0088(10) -0.0017(10) -0.0050(10) C14 0.0280(14) 0.0533(17) 0.0326(15) -0.0206(13) -0.0062(11) -0.0013(12) C15 0.0326(15) 0.0505(17) 0.0328(15) -0.0180(13) -0.0022(12) -0.0008(12) C16 0.0340(14) 0.0268(12) 0.0231(13) -0.0060(10) -0.0037(10) -0.0053(10) C17 0.0249(13) 0.0475(16) 0.0320(14) -0.0135(12) -0.0043(11) -0.0078(11) C18 0.0296(14) 0.0427(15) 0.0269(13) -0.0116(12) 0.0001(11) -0.0071(11) C20 0.0281(13) 0.0299(13) 0.0266(13) -0.0098(11) -0.0046(10) 0.0007(10) C21 0.0389(15) 0.0306(14) 0.0335(14) -0.0120(11) -0.0009(12) -0.0036(11) C22 0.0406(16) 0.0409(16) 0.0416(17) -0.0124(13) -0.0102(13) -0.0038(13) C23 0.0494(19) 0.0480(19) 0.062(2) -0.0245(17) -0.0109(16) -0.0099(15) C24 0.056(2) 0.0376(17) 0.076(2) -0.0220(17) -0.0065(18) -0.0103(15) C25 0.069(2) 0.0326(16) 0.060(2) -0.0060(15) -0.0107(18) -0.0079(15) C26 0.0496(18) 0.0350(15) 0.0340(15) -0.0075(12) -0.0079(13) -0.0054(13) C30 0.0320(14) 0.0338(14) 0.0344(15) -0.0120(12) -0.0062(11) 0.0007(11) C31 0.0410(15) 0.0329(14) 0.0272(14) -0.0078(11) -0.0040(11) -0.0040(12) C32 0.0443(16) 0.0339(14) 0.0269(14) -0.0088(11) -0.0018(12) -0.0047(12) C33 0.074(2) 0.0308(15) 0.0306(15) -0.0106(12) -0.0034(14) -0.0030(14) C34 0.076(3) 0.0383(17) 0.0459(19) -0.0109(14) -0.0126(17) -0.0180(17) C35 0.050(2) 0.052(2) 0.058(2) -0.0108(17) -0.0044(16) -0.0198(16) C36 0.0402(17) 0.0442(17) 0.0454(18) -0.0103(14) 0.0002(13) -0.0064(13) C41 0.0427(16) 0.0299(13) 0.0293(14) -0.0054(11) -0.0038(12) -0.0062(12) C42 0.0518(19) 0.0446(17) 0.0395(17) -0.0141(14) -0.0028(14) 0.0046(14) C43 0.069(2) 0.055(2) 0.049(2) -0.0260(17) 0.0037(17) 0.0023(18) C44 0.084(3) 0.058(2) 0.0347(17) -0.0189(16) -0.0017(17) -0.0139(19) C45 0.074(2) 0.0481(19) 0.0289(16) -0.0068(14) -0.0130(15) -0.0009(17) C46 0.060(2) 0.0324(14) 0.0304(15) -0.0090(12) -0.0090(14) 0.0040(13) S1A 0.0345(4) 0.0444(4) 0.0314(4) -0.0155(3) -0.0027(3) -0.0063(3) C1A 0.0480(17) 0.0312(14) 0.0309(14) -0.0089(12) -0.0006(12) -0.0090(12) C2A 0.065(2) 0.0435(17) 0.0322(16) -0.0086(13) -0.0127(14) -0.0126(15) C3A 0.090(3) 0.0442(18) 0.0316(16) -0.0147(14) -0.0099(17) -0.0164(18) C4A 0.090(3) 0.0360(16) 0.0298(16) -0.0142(13) 0.0023(16) -0.0112(17) C5A 0.066(2) 0.0319(15) 0.0319(15) -0.0103(12) 0.0044(14) -0.0037(14) C6A 0.0489(17) 0.0280(13) 0.0235(13) -0.0052(11) -0.0017(12) -0.0067(12) N7A 0.0370(13) 0.0280(11) 0.0269(11) -0.0079(9) 0.0030(9) -0.0061(9) C8A 0.0335(14) 0.0296(13) 0.0270(13) -0.0057(11) 0.0002(11) -0.0061(11) C9A 0.0338(14) 0.0339(14) 0.0274(13) -0.0098(11) -0.0010(11) -0.0074(11) C10A 0.0352(14) 0.0333(14) 0.0258(13) -0.0065(11) -0.0032(11) -0.0050(11) C11A 0.0319(14) 0.0293(13) 0.0262(13) -0.0068(11) -0.0018(11) -0.0049(10) C12A 0.0349(15) 0.0399(15) 0.0313(15) -0.0118(12) -0.0104(12) 0.0056(12) C13A 0.0347(15) 0.0393(15) 0.0325(15) -0.0130(12) -0.0055(12) 0.0062(12) C14A 0.0378(15) 0.0233(12) 0.0254(13) -0.0052(10) -0.0018(11) -0.0056(10) C15A 0.0293(14) 0.0371(14) 0.0315(14) -0.0088(12) -0.0036(11) -0.0066(11) C16A 0.0298(14) 0.0370(14) 0.0288(14) -0.0113(11) 0.0008(11) -0.0060(11) C20A 0.0335(14) 0.0295(13) 0.0282(13) -0.0090(11) -0.0038(11) -0.0051(11) C21A 0.0448(16) 0.0314(14) 0.0342(15) -0.0119(12) -0.0070(12) -0.0065(12) C22A 0.0487(18) 0.0358(15) 0.0406(17) -0.0121(13) -0.0022(13) -0.0038(13) C23A 0.0473(18) 0.0425(17) 0.055(2) -0.0238(15) -0.0007(15) 0.0003(14) C24A 0.057(2) 0.0322(16) 0.072(2) -0.0206(16) -0.0106(18) -0.0028(14) C25A 0.064(2) 0.0339(16) 0.055(2) -0.0069(15) -0.0066(17) -0.0107(15) C26A 0.0517(18) 0.0338(15) 0.0377(16) -0.0077(13) -0.0018(14) -0.0082(13) C30A 0.0365(15) 0.0334(14) 0.0313(14) -0.0103(12) -0.0006(11) -0.0062(11) C31A 0.0454(17) 0.0340(14) 0.0364(16) -0.0131(12) -0.0082(13) 0.0039(12) C32A 0.066(2) 0.0419(17) 0.0295(16) -0.0079(13) -0.0024(14) 0.0023(15) C33A 0.091(3) 0.066(2) 0.0315(18) -0.0134(17) -0.0073(18) 0.017(2) C34A 0.122(4) 0.091(3) 0.048(2) -0.041(2) -0.037(3) 0.047(3) C35A 0.091(3) 0.067(3) 0.082(3) -0.042(2) -0.046(3) 0.009(2) C36A 0.060(2) 0.0496(19) 0.055(2) -0.0225(16) -0.0186(17) -0.0037(16) C41A 0.0407(15) 0.0305(14) 0.0291(14) -0.0076(11) -0.0036(11) -0.0049(11) C42A 0.0359(15) 0.0318(14) 0.0319(14) -0.0064(11) -0.0034(11) -0.0060(11) C43A 0.0539(18) 0.0304(14) 0.0332(15) -0.0069(12) -0.0078(13) -0.0116(13) C44A 0.058(2) 0.0328(15) 0.0390(16) -0.0115(13) -0.0071(14) -0.0016(13) C45A 0.0474(18) 0.0405(17) 0.0525(19) -0.0141(15) -0.0098(15) 0.0028(14) C46A 0.0413(17) 0.0401(16) 0.0449(17) -0.0151(14) -0.0086(13) -0.0059(13) C65 0.0377(15) 0.0360(15) 0.0378(16) -0.0110(12) 0.0017(12) -0.0026(12) C96 0.0452(19) 0.0504(19) 0.058(2) -0.0109(16) 0.0112(16) -0.0129(15) P1 0.0280(4) 0.0418(4) 0.0614(5) -0.0078(4) -0.0001(4) 0.0023(3) F1 0.0443(12) 0.0815(16) 0.0940(18) 0.0156(14) -0.0126(12) 0.0136(11) F2 0.0410(11) 0.0738(14) 0.0712(14) -0.0358(11) -0.0196(10) 0.0106(9) P2 0.0244(4) 0.0422(4) 0.0514(5) -0.0146(4) -0.0047(3) -0.0009(3) F11 0.0463(12) 0.0753(15) 0.0860(17) -0.0012(13) -0.0225(12) 0.0120(11) F12 0.0376(10) 0.0613(12) 0.0612(12) -0.0297(10) -0.0186(9) 0.0066(8) O1S 0.090(2) 0.0532(15) 0.0700(18) -0.0253(13) 0.0019(15) -0.0273(14) C2S 0.062(2) 0.0501(19) 0.052(2) -0.0221(17) -0.0097(17) -0.0015(16) C3S 0.054(2) 0.0489(19) 0.053(2) -0.0114(16) -0.0054(16) -0.0094(16) C4S 0.0428(17) 0.0374(16) 0.0529(19) -0.0179(14) -0.0039(14) -0.0082(13) C5S 0.050(2) 0.0455(18) 0.057(2) -0.0137(16) -0.0036(16) -0.0080(15) O6S 0.159(4) 0.085(3) 0.129(4) -0.032(3) -0.019(3) -0.020(3) C7S 0.119(5) 0.086(4) 0.083(4) -0.022(3) -0.028(3) -0.002(3) C8S 0.167(7) 0.142(6) 0.122(5) -0.098(5) 0.003(5) -0.032(5) C10S 0.080(3) 0.058(3) 0.125(4) -0.024(3) -0.020(3) 0.002(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 S1 C1 1.737(3) . ? S1 C8 1.722(3) . ? C1 C2 1.395(4) . ? C1 C6 1.389(4) . ? C2 H2 0.9500 . ? C2 C3 1.369(5) . ? C3 H3 0.9500 . ? C3 C4 1.396(5) . ? C4 H4 0.9500 . ? C4 C5 1.387(4) . ? C5 H5 0.9500 . ? C5 C6 1.398(4) . ? C6 N7 1.400(3) . ? N7 C8 1.332(3) . ? N7 C9 1.489(3) . ? C8 C11 1.438(4) . ? C9 H9B 0.9900 . ? C9 H9C 0.9900 . ? C9 C10 1.510(4) . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C10 H10D 0.9800 . ? C11 H11 0.9500 . ? C11 C12 1.345(4) . ? C12 H12 0.9500 . ? C12 C13 1.457(4) . ? C13 C14 1.398(4) . ? C13 C18 1.400(4) . ? C14 H14 0.9500 . ? C14 C15 1.392(4) . ? C15 H15 0.9500 . ? C15 C16 1.382(4) . ? C16 C17 1.392(4) . ? C16 C20 1.498(4) . ? C17 H17 0.9500 . ? C17 C18 1.374(4) . ? C18 H18 0.9500 . ? C20 C21 1.486(4) . ? C20 C30 1.360(4) . ? C21 C22 1.402(4) . ? C21 C26 1.391(4) . ? C22 H22 0.9500 . ? C22 C23 1.380(4) . ? C23 H23 0.9500 . ? C23 C24 1.372(5) . ? C24 H24 0.9500 . ? C24 C25 1.377(5) . ? C25 H25 0.9500 . ? C25 C26 1.391(4) . ? C26 H26 0.9500 . ? C30 C31 1.495(4) . ? C30 C41 1.492(4) . ? C31 C32 1.383(4) . ? C31 C36 1.388(4) . ? C32 H32 0.9500 . ? C32 C33 1.381(4) . ? C33 H33 0.9500 . ? C33 C34 1.397(5) . ? C34 H34 0.9500 . ? C34 C35 1.386(5) . ? C35 H35 0.9500 . ? C35 C36 1.387(5) . ? C36 H36 0.9500 . ? C41 C42 1.393(4) . ? C41 C46 1.382(4) . ? C42 H42 0.9500 . ? C42 C43 1.386(5) . ? C43 H43 0.9500 . ? C43 C44 1.386(5) . ? C44 H44 0.9500 . ? C44 C45 1.364(5) . ? C45 H45 0.9500 . ? C45 C46 1.396(4) . ? C46 H46 0.9500 . ? S1A C1A 1.737(3) . ? S1A C8A 1.718(3) . ? C1A C2A 1.403(4) . ? C1A C6A 1.382(4) . ? C2A H2A 0.9500 . ? C2A C3A 1.368(5) . ? C3A H3A 0.9500 . ? C3A C4A 1.393(6) . ? C4A H4A 0.9500 . ? C4A C5A 1.373(5) . ? C5A H5A 0.9500 . ? C5A C6A 1.403(4) . ? C6A N7A 1.404(4) . ? N7A C8A 1.333(4) . ? N7A C65 1.480(4) . ? C8A C9A 1.438(4) . ? C9A H9A 0.9500 . ? C9A C10A 1.345(4) . ? C10A H10A 0.9500 . ? C10A C11A 1.454(4) . ? C11A C12A 1.396(4) . ? C11A C16A 1.406(4) . ? C12A H12A 0.9500 . ? C12A C13A 1.381(4) . ? C13A H13A 0.9500 . ? C13A C14A 1.395(4) . ? C14A C15A 1.397(4) . ? C14A C20A 1.495(4) . ? C15A H15A 0.9500 . ? C15A C16A 1.375(4) . ? C16A H16A 0.9500 . ? C20A C21A 1.485(4) . ? C20A C30A 1.351(4) . ? C21A C22A 1.394(4) . ? C21A C26A 1.398(4) . ? C22A H22A 0.9500 . ? C22A C23A 1.388(4) . ? C23A H23A 0.9500 . ? C23A C24A 1.385(5) . ? C24A H24A 0.9500 . ? C24A C25A 1.371(5) . ? C25A H25A 0.9500 . ? C25A C26A 1.387(4) . ? C26A H26A 0.9500 . ? C30A C31A 1.489(4) . ? C30A C41A 1.491(4) . ? C31A C32A 1.390(4) . ? C31A C36A 1.404(5) . ? C32A H32A 0.9500 . ? C32A C33A 1.377(5) . ? C33A H33A 0.9500 . ? C33A C34A 1.381(7) . ? C34A H34A 0.9500 . ? C34A C35A 1.387(7) . ? C35A H35A 0.9500 . ? C35A C36A 1.382(5) . ? C36A H36A 0.9500 . ? C41A C42A 1.387(4) . ? C41A C46A 1.395(4) . ? C42A H42A 0.9500 . ? C42A C43A 1.373(4) . ? C43A H43A 0.9500 . ? C43A C44A 1.390(5) . ? C44A H44A 0.9500 . ? C44A C45A 1.389(5) . ? C45A H45A 0.9500 . ? C45A C46A 1.387(4) . ? C46A H46A 0.9500 . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C65 C96 1.518(4) . ? C96 H96A 0.9800 . ? C96 H96B 0.9800 . ? C96 H96C 0.9800 . ? P1 F1 1.604(2) . ? P1 F2 1.589(2) . ? P1 F3 1.655(5) . ? P1 F3A 1.569(5) . ? P1 F3B 1.641(9) . ? P1 F4 1.636(6) . ? P1 F4A 1.622(5) . ? P1 F4B 1.505(10) . ? P1 F5 1.546(7) . ? P1 F5A 1.627(4) . ? P1 F5B 1.548(11) . ? P1 F6 1.554(6) . ? P1 F6A 1.576(5) . ? P1 F6B 1.748(9) . ? P2 F11 1.595(2) . ? P2 F12 1.5900(19) . ? P2 F13 1.651(5) . ? P2 F13A 1.585(5) . ? P2 F13B 1.520(12) . ? P2 F14 1.547(6) . ? P2 F14A 1.643(6) . ? P2 F14B 1.597(12) . ? P2 F15 1.562(5) . ? P2 F15A 1.600(5) . ? P2 F15B 1.735(9) . ? P2 F16 1.659(5) . ? P2 F16A 1.580(5) . ? P2 F16B 1.622(10) . ? O1S C2S 1.418(5) . ? O1S C5S 1.431(4) . ? C2S H2SA 0.9900 . ? C2S H2SB 0.9900 . ? C2S C3S 1.524(5) . ? C3S H3SA 0.9900 . ? C3S H3SB 0.9900 . ? C3S C4S 1.516(5) . ? C4S H4SA 0.9900 . ? C4S H4SB 0.9900 . ? C4S C5S 1.502(4) . ? C5S H5SA 0.9900 . ? C5S H5SB 0.9900 . ? O6S C7S 1.516(7) . ? O6S C10S 1.537(6) . ? C7S C8S 1.546(8) . ? C8S C9S 1.489(11) . ? C8S C9SA 1.317(12) . ? C9S C10S 1.341(9) . ? C9SA C10S 1.486(11) . ? O11S C12S 1.507(18) . ? O11S C13S 1.07(2) 2_577 ? O11S C14S 1.16(2) 2_577 ? O11S C15S 1.501(17) . ? C12S C13S 1.440(14) . ? C12S C13S 1.92(3) 2_577 ? C12S C14S 0.56(3) 2_577 ? C12S C15S 1.28(2) 2_577 ? C13S O11S 1.07(2) 2_577 ? C13S C12S 1.92(3) 2_577 ? C13S C14S 1.503(15) . ? C13S C14S 1.62(3) 2_577 ? C13S C15S 0.76(2) 2_577 ? C14S O11S 1.16(2) 2_577 ? C14S C12S 0.56(3) 2_577 ? C14S C13S 1.62(3) 2_577 ? C14S C15S 1.407(14) . ? C14S C15S 2.03(3) 2_577 ? C15S C12S 1.28(2) 2_577 ? C15S C13S 0.76(2) 2_577 ? C15S C14S 2.03(3) 2_577 ? O16S C17S 1.303(17) . ? O16S C18S 1.445(19) 2_665 ? O16S C19S 1.428(19) 2_665 ? O16S C20S 1.303(17) . ? C17S C18S 2.03(3) 2_665 ? C17S C18S 1.549(17) . ? C17S C19S 0.67(2) 2_665 ? C17S C20S 1.95(3) 2_665 ? C18S O16S 1.445(19) 2_665 ? C18S C17S 2.03(3) 2_665 ? C18S C18S 2.03(4) 2_665 ? C18S C19S 1.21(2) 2_665 ? C18S C19S 1.610(16) . ? C18S C20S 0.75(2) 2_665 ? C19S O16S 1.428(19) 2_665 ? C19S C17S 0.67(2) 2_665 ? C19S C18S 1.21(2) 2_665 ? C19S C19S 1.99(4) 2_665 ? C19S C20S 1.531(16) . ? C20S C17S 1.95(3) 2_665 ? C20S C18S 0.75(2) 2_665 ? 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 C8 S1 C1 91.07(13) . . ? C2 C1 S1 128.0(2) . . ? C6 C1 S1 110.4(2) . . ? C6 C1 C2 121.6(3) . . ? C1 C2 H2 121.2 . . ? C3 C2 C1 117.5(3) . . ? C3 C2 H2 121.2 . . ? C2 C3 H3 119.3 . . ? C2 C3 C4 121.4(3) . . ? C4 C3 H3 119.3 . . ? C3 C4 H4 119.2 . . ? C5 C4 C3 121.6(3) . . ? C5 C4 H4 119.2 . . ? C4 C5 H5 121.4 . . ? C4 C5 C6 117.1(3) . . ? C6 C5 H5 121.4 . . ? C1 C6 C5 120.8(3) . . ? C1 C6 N7 112.3(2) . . ? C5 C6 N7 126.9(3) . . ? C6 N7 C9 120.7(2) . . ? C8 N7 C6 113.9(2) . . ? C8 N7 C9 125.3(2) . . ? N7 C8 S1 112.34(19) . . ? N7 C8 C11 125.2(2) . . ? C11 C8 S1 122.5(2) . . ? N7 C9 H9B 109.4 . . ? N7 C9 H9C 109.4 . . ? N7 C9 C10 111.2(2) . . ? H9B C9 H9C 108.0 . . ? C10 C9 H9B 109.4 . . ? C10 C9 H9C 109.4 . . ? C9 C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? C9 C10 H10D 109.5 . . ? H10B C10 H10C 109.5 . . ? H10B C10 H10D 109.5 . . ? H10C C10 H10D 109.5 . . ? C8 C11 H11 119.2 . . ? C12 C11 C8 121.5(2) . . ? C12 C11 H11 119.2 . . ? C11 C12 H12 116.5 . . ? C11 C12 C13 127.0(3) . . ? C13 C12 H12 116.5 . . ? C14 C13 C12 118.9(2) . . ? C14 C13 C18 117.9(2) . . ? C18 C13 C12 123.1(2) . . ? C13 C14 H14 119.6 . . ? C15 C14 C13 120.8(3) . . ? C15 C14 H14 119.6 . . ? C14 C15 H15 119.6 . . ? C16 C15 C14 120.8(3) . . ? C16 C15 H15 119.6 . . ? C15 C16 C17 118.2(2) . . ? C15 C16 C20 120.6(2) . . ? C17 C16 C20 121.2(2) . . ? C16 C17 H17 119.2 . . ? C18 C17 C16 121.7(3) . . ? C18 C17 H17 119.2 . . ? C13 C18 H18 119.7 . . ? C17 C18 C13 120.5(3) . . ? C17 C18 H18 119.7 . . ? C21 C20 C16 115.0(2) . . ? C30 C20 C16 119.4(2) . . ? C30 C20 C21 125.6(2) . . ? C22 C21 C20 123.4(3) . . ? C26 C21 C20 119.7(3) . . ? C26 C21 C22 116.8(3) . . ? C21 C22 H22 119.4 . . ? C23 C22 C21 121.3(3) . . ? C23 C22 H22 119.4 . . ? C22 C23 H23 119.7 . . ? C24 C23 C22 120.7(3) . . ? C24 C23 H23 119.7 . . ? C23 C24 H24 120.2 . . ? C23 C24 C25 119.6(3) . . ? C25 C24 H24 120.2 . . ? C24 C25 H25 120.1 . . ? C24 C25 C26 119.8(3) . . ? C26 C25 H25 120.1 . . ? C21 C26 C25 121.8(3) . . ? C21 C26 H26 119.1 . . ? C25 C26 H26 119.1 . . ? C20 C30 C31 120.9(2) . . ? C20 C30 C41 124.3(2) . . ? C41 C30 C31 114.8(2) . . ? C32 C31 C30 121.1(3) . . ? C32 C31 C36 118.4(3) . . ? C36 C31 C30 120.5(3) . . ? C31 C32 H32 119.0 . . ? C33 C32 C31 122.0(3) . . ? C33 C32 H32 119.0 . . ? C32 C33 H33 120.5 . . ? C32 C33 C34 118.9(3) . . ? C34 C33 H33 120.5 . . ? C33 C34 H34 120.1 . . ? C35 C34 C33 119.7(3) . . ? C35 C34 H34 120.1 . . ? C34 C35 H35 119.9 . . ? C34 C35 C36 120.2(3) . . ? C36 C35 H35 119.9 . . ? C31 C36 H36 119.7 . . ? C35 C36 C31 120.6(3) . . ? C35 C36 H36 119.7 . . ? C42 C41 C30 121.9(3) . . ? C46 C41 C30 119.7(3) . . ? C46 C41 C42 118.3(3) . . ? C41 C42 H42 119.5 . . ? C43 C42 C41 120.9(3) . . ? C43 C42 H42 119.5 . . ? C42 C43 H43 120.2 . . ? C42 C43 C44 119.6(3) . . ? C44 C43 H43 120.2 . . ? C43 C44 H44 119.9 . . ? C45 C44 C43 120.2(3) . . ? C45 C44 H44 119.9 . . ? C44 C45 H45 120.0 . . ? C44 C45 C46 120.1(3) . . ? C46 C45 H45 120.0 . . ? C41 C46 C45 120.8(3) . . ? C41 C46 H46 119.6 . . ? C45 C46 H46 119.6 . . ? C8A S1A C1A 90.84(14) . . ? C2A C1A S1A 127.7(3) . . ? C6A C1A S1A 110.8(2) . . ? C6A C1A C2A 121.5(3) . . ? C1A C2A H2A 121.4 . . ? C3A C2A C1A 117.2(4) . . ? C3A C2A H2A 121.4 . . ? C2A C3A H3A 119.4 . . ? C2A C3A C4A 121.2(3) . . ? C4A C3A H3A 119.4 . . ? C3A C4A H4A 118.8 . . ? C5A C4A C3A 122.3(3) . . ? C5A C4A H4A 118.8 . . ? C4A C5A H5A 121.6 . . ? C4A C5A C6A 116.8(3) . . ? C6A C5A H5A 121.6 . . ? C1A C6A C5A 120.9(3) . . ? C1A C6A N7A 112.0(2) . . ? C5A C6A N7A 127.1(3) . . ? C6A N7A C65 121.0(2) . . ? C8A N7A C6A 113.8(2) . . ? C8A N7A C65 125.2(2) . . ? N7A C8A S1A 112.6(2) . . ? N7A C8A C9A 124.9(3) . . ? C9A C8A S1A 122.5(2) . . ? C8A C9A H9A 119.0 . . ? C10A C9A C8A 121.9(3) . . ? C10A C9A H9A 119.0 . . ? C9A C10A H10A 117.0 . . ? C9A C10A C11A 126.1(3) . . ? C11A C10A H10A 117.0 . . ? C12A C11A C10A 119.3(3) . . ? C12A C11A C16A 118.3(2) . . ? C16A C11A C10A 122.4(3) . . ? C11A C12A H12A 119.4 . . ? C13A C12A C11A 121.2(3) . . ? C13A C12A H12A 119.4 . . ? C12A C13A H13A 119.7 . . ? C12A C13A C14A 120.6(3) . . ? C14A C13A H13A 119.7 . . ? C13A C14A C15A 118.0(2) . . ? C13A C14A C20A 120.0(2) . . ? C15A C14A C20A 122.0(2) . . ? C14A C15A H15A 119.1 . . ? C16A C15A C14A 121.7(3) . . ? C16A C15A H15A 119.1 . . ? C11A C16A H16A 120.0 . . ? C15A C16A C11A 120.1(3) . . ? C15A C16A H16A 120.0 . . ? C21A C20A C14A 114.2(2) . . ? C30A C20A C14A 121.7(2) . . ? C30A C20A C21A 124.0(2) . . ? C22A C21A C20A 121.6(3) . . ? C22A C21A C26A 118.4(3) . . ? C26A C21A C20A 120.0(3) . . ? C21A C22A H22A 119.6 . . ? C23A C22A C21A 120.8(3) . . ? C23A C22A H22A 119.6 . . ? C22A C23A H23A 120.2 . . ? C24A C23A C22A 119.7(3) . . ? C24A C23A H23A 120.2 . . ? C23A C24A H24A 119.8 . . ? C25A C24A C23A 120.5(3) . . ? C25A C24A H24A 119.8 . . ? C24A C25A H25A 120.0 . . ? C24A C25A C26A 120.0(3) . . ? C26A C25A H25A 120.0 . . ? C21A C26A H26A 119.7 . . ? C25A C26A C21A 120.6(3) . . ? C25A C26A H26A 119.7 . . ? C20A C30A C31A 122.8(3) . . ? C20A C30A C41A 122.1(2) . . ? C31A C30A C41A 115.1(2) . . ? C32A C31A C30A 120.1(3) . . ? C32A C31A C36A 118.4(3) . . ? C36A C31A C30A 121.5(3) . . ? C31A C32A H32A 119.1 . . ? C33A C32A C31A 121.7(4) . . ? C33A C32A H32A 119.1 . . ? C32A C33A H33A 120.5 . . ? C32A C33A C34A 118.9(4) . . ? C34A C33A H33A 120.5 . . ? C33A C34A H34A 119.5 . . ? C33A C34A C35A 120.9(4) . . ? C35A C34A H34A 119.5 . . ? C34A C35A H35A 120.2 . . ? C36A C35A C34A 119.7(4) . . ? C36A C35A H35A 120.2 . . ? C31A C36A H36A 119.9 . . ? C35A C36A C31A 120.2(4) . . ? C35A C36A H36A 119.9 . . ? C42A C41A C30A 122.5(3) . . ? C42A C41A C46A 117.9(3) . . ? C46A C41A C30A 119.6(3) . . ? C41A C42A H42A 118.9 . . ? C43A C42A C41A 122.1(3) . . ? C43A C42A H42A 118.9 . . ? C42A C43A H43A 120.4 . . ? C42A C43A C44A 119.2(3) . . ? C44A C43A H43A 120.4 . . ? C43A C44A H44A 119.9 . . ? C45A C44A C43A 120.1(3) . . ? C45A C44A H44A 119.9 . . ? C44A C45A H45A 120.3 . . ? C46A C45A C44A 119.5(3) . . ? C46A C45A H45A 120.3 . . ? C41A C46A H46A 119.5 . . ? C45A C46A C41A 121.0(3) . . ? C45A C46A H46A 119.5 . . ? N7A C65 H65A 109.4 . . ? N7A C65 H65B 109.4 . . ? N7A C65 C96 111.3(3) . . ? H65A C65 H65B 108.0 . . ? C96 C65 H65A 109.4 . . ? C96 C65 H65B 109.4 . . ? C65 C96 H96A 109.5 . . ? C65 C96 H96B 109.5 . . ? C65 C96 H96C 109.5 . . ? H96A C96 H96B 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? F1 P1 F3 84.9(2) . . ? F1 P1 F3B 103.3(4) . . ? F1 P1 F4 89.4(2) . . ? F1 P1 F4A 90.7(2) . . ? F1 P1 F5A 87.86(19) . . ? F1 P1 F6B 97.8(4) . . ? F2 P1 F1 178.61(15) . . ? F2 P1 F3 95.0(2) . . ? F2 P1 F3B 77.8(4) . . ? F2 P1 F4 89.2(2) . . ? F2 P1 F4A 88.0(2) . . ? F2 P1 F5A 91.64(19) . . ? F2 P1 F6B 83.2(4) . . ? F3 P1 F6B 136.8(5) . . ? F3A P1 F1 91.5(2) . . ? F3A P1 F2 88.9(2) . . ? F3A P1 F3 21.3(2) . . ? F3A P1 F3B 31.6(4) . . ? F3A P1 F4 105.7(4) . . ? F3A P1 F4A 88.9(4) . . ? F3A P1 F5A 176.1(4) . . ? F3A P1 F6A 92.9(4) . . ? F3A P1 F6B 115.8(5) . . ? F3B P1 F3 52.8(4) . . ? F3B P1 F6B 85.1(6) . . ? F4 P1 F3 85.4(3) . . ? F4 P1 F3B 133.9(5) . . ? F4 P1 F6B 137.6(5) . . ? F4A P1 F3 68.8(3) . . ? F4A P1 F3B 117.5(5) . . ? F4A P1 F4 16.8(3) . . ? F4A P1 F5A 87.2(3) . . ? F4A P1 F6B 153.4(5) . . ? F4B P1 F1 88.9(5) . . ? F4B P1 F2 90.2(5) . . ? F4B P1 F3 38.6(6) . . ? F4B P1 F3A 58.7(6) . . ? F4B P1 F3B 88.6(7) . . ? F4B P1 F4 47.0(6) . . ? F4B P1 F4A 30.3(5) . . ? F4B P1 F5 137.5(7) . . ? F4B P1 F5A 117.4(6) . . ? F4B P1 F5B 95.8(9) . . ? F4B P1 F6 127.2(7) . . ? F4B P1 F6A 151.6(7) . . ? F4B P1 F6B 171.7(6) . . ? F5 P1 F1 91.5(3) . . ? F5 P1 F2 88.5(3) . . ? F5 P1 F3 174.6(4) . . ? F5 P1 F3A 163.6(4) . . ? F5 P1 F3B 132.3(6) . . ? F5 P1 F4 90.5(4) . . ? F5 P1 F4A 107.2(4) . . ? F5 P1 F5A 20.4(3) . . ? F5 P1 F5B 42.3(6) . . ? F5 P1 F6 95.0(4) . . ? F5 P1 F6A 70.8(4) . . ? F5 P1 F6B 47.7(5) . . ? F5A P1 F3 154.8(3) . . ? F5A P1 F3B 152.2(5) . . ? F5A P1 F4 70.4(3) . . ? F5A P1 F6B 68.1(5) . . ? F5B P1 F1 82.8(5) . . ? F5B P1 F2 96.3(5) . . ? F5B P1 F3 132.9(7) . . ? F5B P1 F3A 154.1(7) . . ? F5B P1 F3B 172.6(7) . . ? F5B P1 F4 49.3(7) . . ? F5B P1 F4A 66.0(7) . . ? F5B P1 F5A 21.9(5) . . ? F5B P1 F6 134.6(7) . . ? F5B P1 F6A 112.4(7) . . ? F5B P1 F6B 90.0(8) . . ? F6 P1 F1 84.3(3) . . ? F6 P1 F2 97.1(3) . . ? F6 P1 F3 88.7(4) . . ? F6 P1 F3A 69.2(4) . . ? F6 P1 F3B 43.4(5) . . ? F6 P1 F4 171.7(4) . . ? F6 P1 F4A 157.3(4) . . ? F6 P1 F5A 114.6(4) . . ? F6 P1 F6A 25.1(3) . . ? F6 P1 F6B 49.2(4) . . ? F6A P1 F1 91.7(3) . . ? F6A P1 F2 89.6(2) . . ? F6A P1 F3 113.3(4) . . ? F6A P1 F3B 63.7(5) . . ? F6A P1 F4 161.3(4) . . ? F6A P1 F4A 177.0(4) . . ? F6A P1 F5A 91.0(4) . . ? F6A P1 F6B 24.0(4) . . ? F11 P2 F13 90.9(2) . . ? F11 P2 F14A 90.4(3) . . ? F11 P2 F14B 82.6(6) . . ? F11 P2 F15A 91.6(2) . . ? F11 P2 F15B 97.1(4) . . ? F11 P2 F16 85.8(2) . . ? F11 P2 F16B 101.4(4) . . ? F12 P2 F11 178.95(14) . . ? F12 P2 F13 88.11(19) . . ? F12 P2 F14A 89.5(2) . . ? F12 P2 F14B 97.1(6) . . ? F12 P2 F15A 89.5(2) . . ? F12 P2 F15B 83.9(4) . . ? F12 P2 F16 93.87(19) . . ? F12 P2 F16B 79.0(4) . . ? F13 P2 F15B 145.9(5) . . ? F13 P2 F16 86.4(3) . . ? F13A P2 F11 90.7(2) . . ? F13A P2 F12 88.2(2) . . ? F13A P2 F13 15.6(3) . . ? F13A P2 F14A 89.7(4) . . ? F13A P2 F14B 75.7(7) . . ? F13A P2 F15A 177.7(3) . . ? F13A P2 F15B 160.7(5) . . ? F13A P2 F16 70.9(3) . . ? F13A P2 F16B 112.8(6) . . ? F13B P2 F11 84.8(6) . . ? F13B P2 F12 94.2(6) . . ? F13B P2 F13 40.9(7) . . ? F13B P2 F13A 25.6(6) . . ? F13B P2 F14 129.7(8) . . ? F13B P2 F14A 114.6(8) . . ? F13B P2 F14B 99.7(9) . . ? F13B P2 F15 133.6(8) . . ? F13B P2 F15A 154.6(8) . . ? F13B P2 F15B 172.5(8) . . ? F13B P2 F16 45.7(7) . . ? F13B P2 F16A 65.2(7) . . ? F13B P2 F16B 89.5(8) . . ? F14 P2 F11 89.9(3) . . ? F14 P2 F12 90.3(3) . . ? F14 P2 F13 89.4(3) . . ? F14 P2 F13A 105.0(4) . . ? F14 P2 F14A 15.3(4) . . ? F14 P2 F14B 30.2(6) . . ? F14 P2 F15 95.5(4) . . ? F14 P2 F15A 75.2(4) . . ? F14 P2 F15B 57.6(5) . . ? F14 P2 F16 174.0(3) . . ? F14 P2 F16A 165.1(4) . . ? F14 P2 F16B 140.2(6) . . ? F14A P2 F13 74.1(4) . . ? F14A P2 F15B 72.7(5) . . ? F14A P2 F16 160.1(4) . . ? F14B P2 F13 60.4(6) . . ? F14B P2 F14A 16.1(6) . . ? F14B P2 F15A 104.8(7) . . ? F14B P2 F15B 87.7(7) . . ? F14B P2 F16 144.4(6) . . ? F14B P2 F16B 170.3(8) . . ? F15 P2 F11 85.9(3) . . ? F15 P2 F12 95.1(2) . . ? F15 P2 F13 174.1(3) . . ? F15 P2 F13A 159.2(4) . . ? F15 P2 F14A 110.8(4) . . ? F15 P2 F14B 123.9(6) . . ? F15 P2 F15A 21.1(3) . . ? F15 P2 F15B 39.7(4) . . ? F15 P2 F16 88.4(3) . . ? F15 P2 F16A 70.0(4) . . ? F15 P2 F16B 48.4(5) . . ? F15A P2 F13 164.4(4) . . ? F15A P2 F14A 90.5(4) . . ? F15A P2 F15B 18.7(4) . . ? F15A P2 F16 109.1(4) . . ? F15A P2 F16B 66.5(6) . . ? F16 P2 F15B 127.1(5) . . ? F16A P2 F11 92.7(3) . . ? F16A P2 F12 87.4(2) . . ? F16A P2 F13 105.3(4) . . ? F16A P2 F13A 89.7(4) . . ? F16A P2 F14A 176.9(3) . . ? F16A P2 F14B 164.6(7) . . ? F16A P2 F15A 90.0(4) . . ? F16A P2 F15B 107.4(5) . . ? F16A P2 F16 20.2(3) . . ? F16A P2 F16B 25.1(4) . . ? F16B P2 F13 127.9(5) . . ? F16B P2 F14A 154.1(6) . . ? F16B P2 F15B 83.0(6) . . ? F16B P2 F16 45.2(5) . . ? C2S O1S C5S 107.7(3) . . ? O1S C2S H2SA 110.1 . . ? O1S C2S H2SB 110.1 . . ? O1S C2S C3S 108.2(3) . . ? H2SA C2S H2SB 108.4 . . ? C3S C2S H2SA 110.1 . . ? C3S C2S H2SB 110.1 . . ? C2S C3S H3SA 111.4 . . ? C2S C3S H3SB 111.4 . . ? H3SA C3S H3SB 109.2 . . ? C4S C3S C2S 102.1(3) . . ? C4S C3S H3SA 111.4 . . ? C4S C3S H3SB 111.4 . . ? C3S C4S H4SA 111.5 . . ? C3S C4S H4SB 111.5 . . ? H4SA C4S H4SB 109.3 . . ? C5S C4S C3S 101.5(3) . . ? C5S C4S H4SA 111.5 . . ? C5S C4S H4SB 111.5 . . ? O1S C5S C4S 104.9(3) . . ? O1S C5S H5SA 110.8 . . ? O1S C5S H5SB 110.8 . . ? C4S C5S H5SA 110.8 . . ? C4S C5S H5SB 110.8 . . ? H5SA C5S H5SB 108.8 . . ? C7S O6S C10S 104.6(4) . . ? O6S C7S C8S 101.8(5) . . ? C9S C8S C7S 105.2(5) . . ? C9SA C8S C7S 104.4(6) . . ? C9SA C8S C9S 49.1(6) . . ? C10S C9S C8S 104.3(6) . . ? C8S C9SA C10S 105.8(7) . . ? C9S C10S O6S 104.5(5) . . ? C9S C10S C9SA 48.8(5) . . ? C9SA C10S O6S 102.2(6) . . ? C13S O11S C12S 94.8(16) 2_577 . ? C13S O11S C14S 85.0(16) 2_577 2_577 ? C13S O11S C15S 28.3(14) 2_577 . ? C14S O11S C12S 18.9(14) 2_577 . ? C14S O11S C15S 98.5(14) 2_577 . ? C15S O11S C12S 100.1(14) . . ? O11S C12S C13S 33.6(7) . 2_577 ? C13S C12S O11S 112.6(15) . . ? C13S C12S C13S 80.5(15) . 2_577 ? C14S C12S O11S 42(3) 2_577 . ? C14S C12S C13S 99(3) 2_577 . ? C14S C12S C13S 36(3) 2_577 2_577 ? C14S C12S C15S 91(3) 2_577 2_577 ? C15S C12S O11S 124.5(16) 2_577 . ? C15S C12S C13S 91.8(15) 2_577 2_577 ? C15S C12S C13S 31.6(11) 2_577 . ? O11S C13S C12S 51.5(13) 2_577 2_577 ? O11S C13S C12S 147(2) 2_577 . ? O11S C13S C14S 127(2) 2_577 2_577 ? O11S C13S C14S 50.0(12) 2_577 . ? C12S C13S C12S 99.5(15) . 2_577 ? C12S C13S C14S 105.5(14) . . ? C12S C13S C14S 19.9(11) . 2_577 ? C14S C13S C12S 12.6(12) . 2_577 ? C14S C13S C12S 82.4(14) 2_577 2_577 ? C14S C13S C14S 90.5(15) . 2_577 ? C15S C13S O11S 110(3) 2_577 2_577 ? C15S C13S C12S 62(2) 2_577 . ? C15S C13S C12S 112(3) 2_577 2_577 ? C15S C13S C14S 60.2(19) 2_577 2_577 ? C15S C13S C14S 124(3) 2_577 . ? O11S C14S C13S 123(2) 2_577 2_577 ? O11S C14S C13S 45.0(11) 2_577 . ? O11S C14S C15S 47.1(11) 2_577 2_577 ? O11S C14S C15S 148.6(19) 2_577 . ? C12S C14S O11S 119(4) 2_577 2_577 ? C12S C14S C13S 61(3) 2_577 2_577 ? C12S C14S C13S 131(4) 2_577 . ? C12S C14S C15S 65(3) 2_577 . ? C12S C14S C15S 113(4) 2_577 2_577 ? C13S C14S C13S 89.5(15) . 2_577 ? C13S C14S C15S 78.9(13) 2_577 2_577 ? C13S C14S C15S 18.0(10) . 2_577 ? C15S C14S C13S 106.9(13) . . ? C15S C14S C13S 27.8(10) . 2_577 ? C15S C14S C15S 101.7(13) . 2_577 ? O11S C15S C14S 34.4(7) . 2_577 ? C12S C15S O11S 119.6(14) 2_577 . ? C12S C15S C14S 23.3(13) 2_577 . ? C12S C15S C14S 87.2(13) 2_577 2_577 ? C13S C15S O11S 42(2) 2_577 . ? C13S C15S C12S 86(2) 2_577 2_577 ? C13S C15S C14S 38(2) 2_577 2_577 ? C13S C15S C14S 92(2) 2_577 . ? C14S C15S O11S 112.6(14) . . ? C14S C15S C14S 78.3(13) . 2_577 ? C17S O16S C18S 95.4(15) . 2_665 ? C17S O16S C19S 27.7(11) . 2_665 ? C17S O16S C20S 122.2(17) . . ? C19S O16S C18S 68.1(10) 2_665 2_665 ? C20S O16S C18S 31.0(10) . 2_665 ? C20S O16S C19S 96.9(14) . 2_665 ? O16S C17S C18S 105.0(15) . . ? O16S C17S C18S 45.0(9) . 2_665 ? O16S C17S C20S 119.4(15) . 2_665 ? C18S C17S C18S 67.6(13) . 2_665 ? C18S C17S C20S 20.8(9) . 2_665 ? C19S C17S O16S 87(3) 2_665 . ? C19S C17S C18S 48(2) 2_665 . ? C19S C17S C18S 43(2) 2_665 2_665 ? C19S C17S C20S 43(2) 2_665 2_665 ? C20S C17S C18S 76.2(12) 2_665 2_665 ? O16S C18S C17S 39.6(8) 2_665 2_665 ? O16S C18S C17S 140.3(16) 2_665 . ? O16S C18S C18S 79.3(12) 2_665 2_665 ? O16S C18S C19S 55.4(10) 2_665 . ? C17S C18S C17S 112.4(13) . 2_665 ? C17S C18S C18S 67.6(12) . 2_665 ? C17S C18S C19S 101.8(15) . . ? C18S C18S C17S 44.8(7) 2_665 2_665 ? C19S C18S O16S 116.4(18) 2_665 2_665 ? C19S C18S C17S 24.1(12) 2_665 . ? C19S C18S C17S 16.3(8) . 2_665 ? C19S C18S C17S 94.8(17) 2_665 2_665 ? C19S C18S C18S 36.4(8) . 2_665 ? C19S C18S C18S 52.3(13) 2_665 2_665 ? C19S C18S C19S 88.7(18) 2_665 . ? C20S C18S O16S 63.9(18) 2_665 2_665 ? C20S C18S C17S 100(2) 2_665 2_665 ? C20S C18S C17S 112(2) 2_665 . ? C20S C18S C18S 117(3) 2_665 2_665 ? C20S C18S C19S 116(2) 2_665 . ? C20S C18S C19S 101(2) 2_665 2_665 ? O16S C19S C18S 56.4(10) 2_665 . ? O16S C19S C19S 80.9(12) 2_665 2_665 ? O16S C19S C20S 146.1(16) 2_665 . ? C17S C19S O16S 66(2) 2_665 2_665 ? C17S C19S C18S 121(3) 2_665 . ? C17S C19S C18S 108(3) 2_665 2_665 ? C17S C19S C19S 127(3) 2_665 2_665 ? C17S C19S C20S 120(3) 2_665 . ? C18S C19S O16S 118.5(19) 2_665 2_665 ? C18S C19S C18S 91.3(18) 2_665 . ? C18S C19S C19S 54.0(13) 2_665 2_665 ? C18S C19S C19S 37.3(9) . 2_665 ? C18S C19S C20S 28.6(11) 2_665 . ? C20S C19S C18S 103.2(14) . . ? C20S C19S C19S 69.7(11) . 2_665 ? O16S C20S C17S 118.4(13) . 2_665 ? O16S C20S C19S 105.4(15) . . ? C18S C20S O16S 85(2) 2_665 . ? C18S C20S C17S 47.4(17) 2_665 2_665 ? C18S C20S C19S 50.8(18) 2_665 . ? C19S C20S C17S 17.1(10) . 2_665 ? data_na5cult _database_code_depnum_ccdc_archive 'CCDC 883791' #TrackingRef 'na5cult.cif' _audit_creation_date 2012-01-18 _audit_creation_method ; Olex2 1.1-beta (compiled Nov 1 2011 20:42:30, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C37 H30 N S, C4 H8 O2, F6 P' _chemical_formula_sum 'C41 H38 F6 N O2 P S' _chemical_formula_weight 753.75 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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 _space_group_IT_number 2 _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 9.6552(4) _cell_length_b 17.4019(11) _cell_length_c 23.8103(11) _cell_angle_alpha 72.469(5) _cell_angle_beta 84.653(4) _cell_angle_gamma 82.064(4) _cell_volume 3772.6(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 5699 _cell_measurement_temperature 172.9(3) _cell_measurement_theta_max 71.4630 _cell_measurement_theta_min 3.8965 _exptl_absorpt_coefficient_mu 1.731 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.84439 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1568 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.04 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0462 _diffrn_reflns_av_unetI/netI 0.0542 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 22017 _diffrn_reflns_theta_full 66.50 _diffrn_reflns_theta_max 67.00 _diffrn_reflns_theta_min 3.90 _diffrn_ambient_temperature 172.9(3) _diffrn_detector_area_resol_mean 15.9578 _diffrn_measured_fraction_theta_full 0.977 _diffrn_measured_fraction_theta_max 0.976 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 45.00 77.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.9945 -45.0000 -120.0000 32 #__ type_ start__ end____ width___ exp.time_ 2 omega 35.00 76.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -178.0000 120.0000 41 #__ type_ start__ end____ width___ exp.time_ 3 omega -111.00 -18.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -54.9973 125.0000 120.0000 93 #__ type_ start__ end____ width___ exp.time_ 4 omega -85.00 -25.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -54.9973 -77.0000 30.0000 60 #__ type_ start__ end____ width___ exp.time_ 5 omega 36.00 124.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 54.9973 57.0000 -120.0000 88 #__ type_ start__ end____ width___ exp.time_ 6 omega 27.00 123.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 54.9973 77.0000 -30.0000 96 #__ type_ start__ end____ width___ exp.time_ 7 omega 73.00 126.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 54.9973 125.0000 -120.0000 53 #__ type_ start__ end____ width___ exp.time_ 8 omega 13.00 71.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 54.9973 -38.0000 -150.0000 58 #__ type_ start__ end____ width___ exp.time_ 9 omega 41.00 174.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.9945 0.0000 -60.0000 133 #__ type_ start__ end____ width___ exp.time_ 10 omega 41.00 126.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.9945 -92.0000 46.0000 85 #__ type_ start__ end____ width___ exp.time_ 11 omega 49.00 76.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.9945 -45.0000 -30.0000 27 #__ type_ start__ end____ width___ exp.time_ 12 omega 37.00 67.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.9945 -30.0000 90.0000 30 #__ type_ start__ end____ width___ exp.time_ 13 omega 37.00 69.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.9945 -30.0000 0.0000 32 #__ type_ start__ end____ width___ exp.time_ 14 omega 46.00 77.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.9945 -45.0000 60.0000 31 #__ type_ start__ end____ width___ exp.time_ 15 omega 37.00 67.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.9945 -30.0000 -180.0000 30 #__ type_ start__ end____ width___ exp.time_ 16 omega 88.00 162.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.9945 61.0000 -30.0000 74 #__ type_ start__ end____ width___ exp.time_ 17 omega 42.00 68.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.9945 -30.0000 -60.0000 26 #__ type_ start__ end____ width___ exp.time_ 18 omega 44.00 70.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.9945 -45.0000 -150.0000 26 #__ type_ start__ end____ width___ exp.time_ 19 omega 43.00 149.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.9945 -93.0000 172.0000 106 #__ type_ start__ end____ width___ exp.time_ 20 omega 85.00 146.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.9945 -92.0000 -121.0000 61 #__ type_ start__ end____ width___ exp.time_ 21 omega 40.00 77.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.9945 -45.0000 150.0000 37 #__ type_ start__ end____ width___ exp.time_ 22 omega 50.00 77.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.9945 -45.0000 30.0000 27 #__ type_ start__ end____ width___ exp.time_ 23 omega 48.00 73.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.9945 -92.0000 -121.0000 25 ; _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0461550000 _diffrn_orient_matrix_UB_12 -0.0683740000 _diffrn_orient_matrix_UB_13 -0.0201186000 _diffrn_orient_matrix_UB_21 -0.0647051000 _diffrn_orient_matrix_UB_22 0.0634782000 _diffrn_orient_matrix_UB_23 -0.0541265000 _diffrn_orient_matrix_UB_31 0.1404066000 _diffrn_orient_matrix_UB_32 -0.0056661000 _diffrn_orient_matrix_UB_33 -0.0358242000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_source_current 35 _diffrn_source_voltage 50 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 9409 _reflns_number_total 13132 _reflns_odcompleteness_completeness 98.53 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.49 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; XS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.696 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.056 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1025 _refine_ls_number_reflns 13132 _refine_ls_number_restraints 165 _refine_ls_R_factor_all 0.0824 _refine_ls_R_factor_gt 0.0597 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0989P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1583 _refine_ls_wR_factor_ref 0.1760 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 S1 S 0.66267(6) 0.37863(4) 0.52857(3) 0.03347(16) Uani 1 1 d . . . C1 C 0.5999(3) 0.40967(15) 0.58976(11) 0.0345(5) Uani 1 1 d . . . C2 C 0.6764(3) 0.42425(17) 0.63158(12) 0.0437(6) Uani 1 1 d . . . H2 H 0.7759 0.4175 0.6290 0.052 Uiso 1 1 calc R . . C3 C 0.6024(4) 0.44889(19) 0.67682(13) 0.0519(8) Uani 1 1 d . . . H3 H 0.6516 0.4589 0.7062 0.062 Uiso 1 1 calc R . . C4 C 0.4567(4) 0.45920(19) 0.67992(13) 0.0512(7) Uani 1 1 d . . . H4 H 0.4086 0.4760 0.7117 0.061 Uiso 1 1 calc R . . C5 C 0.3797(3) 0.44586(17) 0.63837(12) 0.0416(6) Uani 1 1 d . . . H5 H 0.2802 0.4537 0.6407 0.050 Uiso 1 1 calc R . . C6 C 0.4546(3) 0.42038(14) 0.59285(10) 0.0327(5) Uani 1 1 d . . . N7 N 0.3989(2) 0.40552(12) 0.54528(8) 0.0289(4) Uani 1 1 d . . . C8 C 0.4945(2) 0.38222(14) 0.50802(10) 0.0283(5) Uani 1 1 d . . . C9 C 0.2451(3) 0.41542(15) 0.53944(11) 0.0340(5) Uani 1 1 d . . . H9A H 0.2258 0.4229 0.4979 0.041 Uiso 1 1 calc R . . H9B H 0.2024 0.4646 0.5500 0.041 Uiso 1 1 calc R . . C10 C 0.1791(3) 0.34223(18) 0.57896(14) 0.0485(7) Uani 1 1 d . . . H10A H 0.2171 0.2940 0.5669 0.073 Uiso 1 1 calc R . . H10B H 0.0774 0.3516 0.5755 0.073 Uiso 1 1 calc R . . H10C H 0.2002 0.3339 0.6200 0.073 Uiso 1 1 calc R . . C11 C 0.4673(3) 0.36310(15) 0.45597(10) 0.0313(5) Uani 1 1 d . . . H11 H 0.3730 0.3624 0.4478 0.038 Uiso 1 1 calc R . . C12 C 0.5710(3) 0.34604(15) 0.41824(10) 0.0330(5) Uani 1 1 d . . . H12 H 0.6638 0.3451 0.4289 0.040 Uiso 1 1 calc R . . C13 C 0.5573(3) 0.32886(15) 0.36310(10) 0.0326(5) Uani 1 1 d . . . C14 C 0.4279(3) 0.32904(17) 0.34143(11) 0.0370(6) Uani 1 1 d . . . H14 H 0.3440 0.3392 0.3636 0.044 Uiso 1 1 calc R . . C15 C 0.4209(3) 0.31443(16) 0.28770(11) 0.0371(6) Uani 1 1 d . . . H15 H 0.3321 0.3131 0.2741 0.044 Uiso 1 1 calc R . . C16 C 0.5420(3) 0.30157(15) 0.25330(10) 0.0333(5) Uani 1 1 d . . . C17 C 0.6704(3) 0.30171(19) 0.27509(12) 0.0451(7) Uani 1 1 d . . . H17 H 0.7541 0.2929 0.2524 0.054 Uiso 1 1 calc R . . C18 C 0.6787(3) 0.31443(19) 0.32926(12) 0.0441(7) Uani 1 1 d . . . H18 H 0.7678 0.3133 0.3436 0.053 Uiso 1 1 calc R . . C20 C 0.5340(3) 0.28850(15) 0.19438(11) 0.0344(5) Uani 1 1 d . . . C21 C 0.4877(3) 0.21026(16) 0.19558(11) 0.0372(6) Uani 1 1 d . . . C22 C 0.4134(3) 0.20068(18) 0.15113(13) 0.0454(7) Uani 1 1 d . . . H22 H 0.3899 0.2462 0.1182 0.054 Uiso 1 1 calc R . . C23 C 0.3732(4) 0.1264(2) 0.15383(15) 0.0583(8) Uani 1 1 d . . . H23 H 0.3240 0.1215 0.1226 0.070 Uiso 1 1 calc R . . C24 C 0.4036(4) 0.0591(2) 0.20143(16) 0.0611(9) Uani 1 1 d . . . H24 H 0.3758 0.0081 0.2031 0.073 Uiso 1 1 calc R . . C25 C 0.4747(4) 0.06726(19) 0.24622(15) 0.0579(8) Uani 1 1 d . . . H25 H 0.4968 0.0213 0.2790 0.070 Uiso 1 1 calc R . . C26 C 0.5148(3) 0.14153(18) 0.24428(13) 0.0464(7) Uani 1 1 d . . . H26 H 0.5613 0.1461 0.2764 0.056 Uiso 1 1 calc R . . C30 C 0.5726(3) 0.34650(16) 0.14505(11) 0.0359(5) Uani 1 1 d . . . C31 C 0.6051(3) 0.42610(16) 0.14824(11) 0.0395(6) Uani 1 1 d . . . C32 C 0.5037(4) 0.47866(17) 0.16763(11) 0.0459(7) Uani 1 1 d . . . H32 H 0.4122 0.4633 0.1790 0.055 Uiso 1 1 calc R . . C33 C 0.5327(4) 0.55260(18) 0.17084(13) 0.0552(8) Uani 1 1 d . . . H33 H 0.4612 0.5882 0.1832 0.066 Uiso 1 1 calc R . . C34 C 0.6655(5) 0.5742(2) 0.15601(15) 0.0698(11) Uani 1 1 d . . . H34 H 0.6869 0.6242 0.1596 0.084 Uiso 1 1 calc R . . C35 C 0.7692(5) 0.5236(2) 0.13580(17) 0.0712(11) Uani 1 1 d . . . H35 H 0.8608 0.5391 0.1252 0.085 Uiso 1 1 calc R . . C36 C 0.7384(4) 0.4496(2) 0.13110(14) 0.0552(8) Uani 1 1 d . . . H36 H 0.8082 0.4156 0.1162 0.066 Uiso 1 1 calc R . . C41 C 0.5844(3) 0.33728(15) 0.08406(11) 0.0369(6) Uani 1 1 d . . . C42 C 0.4999(4) 0.38966(18) 0.04112(13) 0.0525(8) Uani 1 1 d . . . H42 H 0.4400 0.4329 0.0502 0.063 Uiso 1 1 calc R . . C43 C 0.5013(4) 0.38009(19) -0.01427(13) 0.0591(9) Uani 1 1 d . . . H43 H 0.4403 0.4153 -0.0426 0.071 Uiso 1 1 calc R . . C44 C 0.5914(4) 0.3193(2) -0.02833(13) 0.0563(8) Uani 1 1 d . . . H44 H 0.5921 0.3121 -0.0664 0.068 Uiso 1 1 calc R . . C45 C 0.6807(4) 0.2688(2) 0.01286(14) 0.0615(9) Uani 1 1 d . . . H45 H 0.7456 0.2282 0.0028 0.074 Uiso 1 1 calc R . . C46 C 0.6751(4) 0.2776(2) 0.06902(13) 0.0520(7) Uani 1 1 d . . . H46 H 0.7350 0.2419 0.0976 0.062 Uiso 1 1 calc R . . S2 S 0.16141(7) 0.86941(4) 0.53353(3) 0.03823(17) Uani 1 1 d . . . C51 C 0.0980(3) 0.90514(17) 0.59276(11) 0.0407(6) Uani 1 1 d . . . C52 C 0.1747(4) 0.91819(19) 0.63496(13) 0.0526(8) Uani 1 1 d . . . H52 H 0.2738 0.9065 0.6345 0.063 Uiso 1 1 calc R . . C53 C 0.1005(4) 0.9489(2) 0.67760(13) 0.0602(9) Uani 1 1 d . . . H53 H 0.1498 0.9583 0.7072 0.072 Uiso 1 1 calc R . . C54 C -0.0440(5) 0.9662(2) 0.67821(13) 0.0614(10) Uani 1 1 d . . . H54 H -0.0919 0.9868 0.7083 0.074 Uiso 1 1 calc R . . C55 C -0.1197(4) 0.95398(18) 0.63577(13) 0.0500(7) Uani 1 1 d . . . H55 H -0.2186 0.9665 0.6359 0.060 Uiso 1 1 calc R . . C56 C -0.0465(3) 0.92279(15) 0.59276(11) 0.0379(6) Uani 1 1 d . . . N57 N -0.1016(2) 0.90832(12) 0.54480(9) 0.0335(5) Uani 1 1 d . . . C58 C -0.0051(3) 0.87904(15) 0.51019(11) 0.0315(5) Uani 1 1 d . . . C59 C -0.2534(3) 0.92355(17) 0.53628(13) 0.0409(6) Uani 1 1 d . . . H59A H -0.2695 0.9310 0.4944 0.049 Uiso 1 1 calc R . . H59B H -0.2921 0.9742 0.5457 0.049 Uiso 1 1 calc R . . C60 C -0.3289(4) 0.8542(2) 0.57497(17) 0.0595(9) Uani 1 1 d . . . H60A H -0.2913 0.8041 0.5655 0.089 Uiso 1 1 calc R . . H60B H -0.4291 0.8659 0.5681 0.089 Uiso 1 1 calc R . . H60C H -0.3152 0.8477 0.6165 0.089 Uiso 1 1 calc R . . C61 C -0.0331(3) 0.86119(15) 0.45781(11) 0.0330(5) Uani 1 1 d . . . H61 H -0.1274 0.8676 0.4472 0.040 Uiso 1 1 calc R . . C62 C 0.0693(3) 0.83559(15) 0.42291(10) 0.0325(5) Uani 1 1 d . . . H62 H 0.1620 0.8259 0.4358 0.039 Uiso 1 1 calc R . . C63 C 0.0497(3) 0.82160(15) 0.36711(10) 0.0312(5) Uani 1 1 d . . . C64 C -0.0785(3) 0.84377(16) 0.34031(11) 0.0332(5) Uani 1 1 d . . . H64 H -0.1565 0.8672 0.3594 0.040 Uiso 1 1 calc R . . C65 C -0.0929(3) 0.83205(15) 0.28660(11) 0.0337(5) Uani 1 1 d . . . H65 H -0.1805 0.8484 0.2688 0.040 Uiso 1 1 calc R . . C66 C 0.0190(3) 0.79652(15) 0.25787(10) 0.0320(5) Uani 1 1 d . . . C67 C 0.1445(3) 0.77172(16) 0.28546(11) 0.0380(6) Uani 1 1 d . . . H67 H 0.2202 0.7448 0.2676 0.046 Uiso 1 1 calc R . . C68 C 0.1614(3) 0.78542(16) 0.33855(11) 0.0369(6) Uani 1 1 d . . . H68 H 0.2497 0.7701 0.3558 0.044 Uiso 1 1 calc R . . C70 C 0.0021(3) 0.78403(15) 0.19969(11) 0.0343(5) Uani 1 1 d . . . C71 C 0.0381(3) 0.69882(16) 0.19788(11) 0.0375(6) Uani 1 1 d . . . C72 C -0.0057(4) 0.63497(18) 0.24429(13) 0.0505(7) Uani 1 1 d . . . H72 H -0.0584 0.6464 0.2771 0.061 Uiso 1 1 calc R . . C73 C 0.0257(4) 0.55548(19) 0.24366(15) 0.0608(9) Uani 1 1 d . . . H73 H -0.0077 0.5131 0.2753 0.073 Uiso 1 1 calc R . . C74 C 0.1053(4) 0.53756(19) 0.19737(16) 0.0582(8) Uani 1 1 d . . . H74 H 0.1280 0.4828 0.1970 0.070 Uiso 1 1 calc R . . C75 C 0.1522(4) 0.6001(2) 0.15127(16) 0.0596(8) Uani 1 1 d . . . H75 H 0.2078 0.5881 0.1192 0.072 Uiso 1 1 calc R . . C76 C 0.1189(4) 0.67969(18) 0.15146(14) 0.0507(7) Uani 1 1 d . . . H76 H 0.1516 0.7219 0.1195 0.061 Uiso 1 1 calc R . . C80 C -0.0462(3) 0.84625(16) 0.15347(11) 0.0367(6) Uani 1 1 d . . . C81 C -0.0809(3) 0.83580(17) 0.09702(12) 0.0434(6) Uani 1 1 d . . . C82 C -0.1726(5) 0.7820(2) 0.09589(16) 0.0678(10) Uani 1 1 d . . . H82 H -0.2144 0.7510 0.1318 0.081 Uiso 1 1 calc R . . C83 C -0.2039(7) 0.7730(3) 0.0426(2) 0.112(2) Uani 1 1 d . . . H83 H -0.2676 0.7364 0.0419 0.135 Uiso 1 1 calc R . . C84 C -0.1404(7) 0.8187(3) -0.01036(19) 0.110(2) Uani 1 1 d . . . H84 H -0.1605 0.8122 -0.0468 0.132 Uiso 1 1 calc R . . C85 C -0.0489(6) 0.8733(2) -0.00971(15) 0.0781(13) Uani 1 1 d . . . H85 H -0.0048 0.9034 -0.0453 0.094 Uiso 1 1 calc R . . C86 C -0.0231(4) 0.88291(19) 0.04367(13) 0.0533(8) Uani 1 1 d . . . H86 H 0.0352 0.9224 0.0443 0.064 Uiso 1 1 calc R . . C91 C -0.0664(3) 0.93180(16) 0.15564(11) 0.0364(6) Uani 1 1 d . . . C92 C -0.1954(3) 0.97877(18) 0.14227(13) 0.0454(6) Uani 1 1 d . . . H92 H -0.2681 0.9563 0.1305 0.055 Uiso 1 1 calc R . . C93 C -0.2188(3) 1.05754(18) 0.14591(14) 0.0504(7) Uani 1 1 d . . . H93 H -0.3079 1.0881 0.1380 0.061 Uiso 1 1 calc R . . C94 C -0.1112(4) 1.09155(18) 0.16112(13) 0.0502(7) Uani 1 1 d . . . H94 H -0.1267 1.1456 0.1636 0.060 Uiso 1 1 calc R . . C95 C 0.0185(3) 1.04690(17) 0.17270(11) 0.0427(6) Uani 1 1 d . . . H95 H 0.0927 1.0705 0.1823 0.051 Uiso 1 1 calc R . . C96 C 0.0394(3) 0.96759(16) 0.17020(11) 0.0379(6) Uani 1 1 d . . . H96 H 0.1283 0.9370 0.1787 0.045 Uiso 1 1 calc R . . O1S O 0.4524(5) 0.7431(2) 0.17082(19) 0.1213(14) Uani 1 1 d . . . O2S O 0.4420(4) 0.8750(2) 0.14598(16) 0.0999(11) Uani 1 1 d . . . C1S C 0.4724(4) 0.8026(3) 0.1819(2) 0.0731(11) Uani 1 1 d . . . C2S C 0.5292(6) 0.8046(4) 0.2370(2) 0.1112(19) Uani 1 1 d . . . H2SA H 0.4597 0.8347 0.2575 0.167 Uiso 1 1 calc R . . H2SB H 0.6149 0.8313 0.2275 0.167 Uiso 1 1 calc R . . H2SC H 0.5505 0.7490 0.2625 0.167 Uiso 1 1 calc R . . C3S C 0.3866(7) 0.8803(4) 0.0894(3) 0.1133(19) Uani 1 1 d . . . H3SA H 0.4565 0.8529 0.0665 0.136 Uiso 1 1 calc R . . H3SB H 0.3006 0.8529 0.0964 0.136 Uiso 1 1 calc R . . C4S C 0.3557(8) 0.9638(5) 0.0571(3) 0.148(3) Uani 1 1 d . . . H4SA H 0.3135 0.9678 0.0203 0.222 Uiso 1 1 calc R . . H4SB H 0.4423 0.9896 0.0480 0.222 Uiso 1 1 calc R . . H4SC H 0.2900 0.9912 0.0808 0.222 Uiso 1 1 calc R . . O11S O 0.0163(10) 0.2548(6) 0.1451(4) 0.128(3) Uiso 0.50 1 d PD A 1 O12S O 0.1235(7) 0.3632(4) 0.1381(3) 0.0915(18) Uiso 0.50 1 d PD A 1 C11S C 0.0678(9) 0.3036(5) 0.1596(4) 0.0671(19) Uiso 0.50 1 d PD A 1 C12S C 0.0685(14) 0.2867(8) 0.2268(5) 0.109(4) Uiso 0.50 1 d PD A 1 H12A H 0.0113 0.3311 0.2385 0.164 Uiso 0.50 1 calc PR A 1 H12B H 0.1648 0.2827 0.2381 0.164 Uiso 0.50 1 calc PR A 1 H12C H 0.0298 0.2356 0.2466 0.164 Uiso 0.50 1 calc PR A 1 C13S C 0.118(2) 0.3884(10) 0.0696(6) 0.125(7) Uiso 0.50 1 d PD A 1 H13A H 0.1869 0.3528 0.0527 0.150 Uiso 0.50 1 calc PR A 1 H13B H 0.0231 0.3846 0.0584 0.150 Uiso 0.50 1 calc PR A 1 C14S C 0.1515(15) 0.4754(8) 0.0477(6) 0.124(4) Uiso 0.50 1 d PD A 1 H14A H 0.1580 0.4931 0.0045 0.186 Uiso 0.50 1 calc PR A 1 H14B H 0.2412 0.4789 0.0625 0.186 Uiso 0.50 1 calc PR A 1 H14C H 0.0774 0.5106 0.0620 0.186 Uiso 0.50 1 calc PR A 1 O21S O 0.1347(9) 0.4373(5) 0.0943(4) 0.115(2) Uiso 0.50 1 d PD B 2 O22S O 0.0643(6) 0.3151(4) 0.1236(3) 0.0725(14) Uiso 0.50 1 d PD B 2 C21S C 0.0929(13) 0.3782(7) 0.0834(5) 0.075(3) Uiso 0.50 1 d PD B 2 C22S C 0.0411(14) 0.3759(8) 0.0256(5) 0.123(4) Uiso 0.50 1 d PD B 2 H22A H -0.0211 0.4256 0.0090 0.184 Uiso 0.50 1 calc PR B 2 H22B H -0.0102 0.3288 0.0328 0.184 Uiso 0.50 1 calc PR B 2 H22C H 0.1213 0.3719 -0.0022 0.184 Uiso 0.50 1 calc PR B 2 C23S C 0.0958(10) 0.3164(5) 0.1855(5) 0.076(2) Uiso 0.50 1 d PD B 2 H23A H 0.1935 0.3282 0.1848 0.091 Uiso 0.50 1 calc PR B 2 H23B H 0.0331 0.3607 0.1960 0.091 Uiso 0.50 1 calc PR B 2 C24S C 0.0767(9) 0.2385(5) 0.2315(4) 0.073(2) Uiso 0.50 1 d PD B 2 H24A H 0.1605 0.1998 0.2311 0.109 Uiso 0.50 1 calc PR B 2 H24B H -0.0049 0.2165 0.2233 0.109 Uiso 0.50 1 calc PR B 2 H24C H 0.0619 0.2478 0.2703 0.109 Uiso 0.50 1 calc PR B 2 P1 P 0.98092(7) 0.62618(4) 0.58756(4) 0.04260(19) Uani 1 1 d D . . P2 P 0.5101(7) 0.8690(4) 0.4000(2) 0.0387(10) Uani 0.50 1 d PD C 1 F1 F 0.85655(17) 0.68264(11) 0.55060(8) 0.0533(4) Uani 1 1 d D D 1 F2 F 1.1061(2) 0.56947(14) 0.62398(11) 0.0826(8) Uani 1 1 d D D 1 F3 F 1.0193(5) 0.5808(4) 0.5353(3) 0.0498(13) Uani 0.50 1 d PD D 1 F3B F 0.9860(16) 0.5527(7) 0.5666(7) 0.101(5) Uiso 0.25 1 d PD D 2 F3A F 1.0308(14) 0.6053(7) 0.5260(5) 0.051(4) Uiso 0.25 1 d PD D 3 F4 F 0.8690(5) 0.5638(4) 0.6155(4) 0.063(2) Uani 0.50 1 d PD D 1 F4B F 0.8765(11) 0.5909(8) 0.6448(4) 0.079(3) Uiso 0.25 1 d PD D 2 F4A F 0.8931(15) 0.5499(8) 0.6044(8) 0.064(5) Uiso 0.25 1 d PD D 3 F5 F 0.9436(5) 0.6695(4) 0.6363(2) 0.0564(12) Uani 0.50 1 d PD D 1 F5B F 0.9789(11) 0.7030(6) 0.6177(5) 0.062(3) Uiso 0.25 1 d PD D 2 F5A F 0.9223(13) 0.6411(7) 0.6488(5) 0.057(3) Uiso 0.25 1 d PD D 3 F6 F 1.0922(4) 0.6880(3) 0.5541(2) 0.0355(8) Uani 0.50 1 d PD D 1 F6B F 1.0868(12) 0.6694(7) 0.5391(5) 0.070(4) Uiso 0.25 1 d PD D 2 F6A F 1.0712(11) 0.6998(6) 0.5701(5) 0.051(3) Uiso 0.25 1 d PD D 3 P3 P 0.5113(7) 0.8746(4) 0.4142(2) 0.0433(11) Uani 0.50 1 d PD C 2 F11 F 0.64272(19) 0.83055(13) 0.44439(9) 0.0643(5) Uani 1 1 d D . . F12 F 0.3763(6) 0.9017(4) 0.3602(3) 0.0540(12) Uani 0.50 1 d PD C 1 F12A F 0.3801(7) 0.9252(4) 0.3801(3) 0.0760(18) Uani 0.50 1 d PD C 2 F13 F 0.5053(7) 0.9568(3) 0.4083(4) 0.106(2) Uani 0.50 1 d PD C 1 F13A F 0.4202(7) 0.8046(3) 0.4428(4) 0.092(3) Uani 0.50 1 d PD C 2 F14 F 0.6045(4) 0.8967(4) 0.3426(2) 0.0697(15) Uani 0.50 1 d PD C 1 F14A F 0.4646(5) 0.9131(4) 0.4658(3) 0.0939(18) Uani 0.50 1 d PD C 2 F15 F 0.5101(6) 0.7836(2) 0.3908(3) 0.0693(14) Uani 0.50 1 d PD C 1 F15A F 0.6059(6) 0.9449(4) 0.3857(4) 0.112(2) Uani 0.50 1 d PD C 2 F16 F 0.4123(7) 0.8425(7) 0.4578(3) 0.120(4) Uani 0.50 1 d PD C 1 F16A F 0.5684(7) 0.8371(7) 0.3619(3) 0.115(3) Uani 0.50 1 d PD C 2 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 S1 0.0309(3) 0.0412(3) 0.0306(3) -0.0137(3) -0.0028(2) -0.0040(2) C1 0.0435(14) 0.0311(12) 0.0287(12) -0.0088(10) -0.0058(10) -0.0014(10) C2 0.0530(16) 0.0425(15) 0.0369(15) -0.0105(12) -0.0144(12) -0.0041(12) C3 0.076(2) 0.0501(17) 0.0338(15) -0.0173(13) -0.0164(14) -0.0030(15) C4 0.076(2) 0.0509(17) 0.0296(14) -0.0190(13) -0.0018(14) -0.0013(15) C5 0.0519(16) 0.0409(14) 0.0311(13) -0.0131(11) 0.0015(12) 0.0012(12) C6 0.0454(14) 0.0288(12) 0.0228(11) -0.0063(9) -0.0029(10) -0.0021(10) N7 0.0332(10) 0.0301(10) 0.0221(9) -0.0064(8) -0.0011(8) -0.0022(8) C8 0.0333(12) 0.0265(11) 0.0233(11) -0.0053(9) -0.0003(9) -0.0025(9) C9 0.0306(12) 0.0375(13) 0.0334(13) -0.0126(11) 0.0006(10) 0.0009(10) C10 0.0413(15) 0.0491(17) 0.0519(17) -0.0115(14) 0.0098(13) -0.0095(12) C11 0.0354(12) 0.0362(13) 0.0229(11) -0.0093(10) -0.0013(9) -0.0053(10) C12 0.0327(12) 0.0406(14) 0.0262(12) -0.0109(10) -0.0024(10) -0.0033(10) C13 0.0380(13) 0.0351(13) 0.0241(12) -0.0092(10) -0.0014(10) -0.0012(10) C14 0.0338(13) 0.0509(15) 0.0281(12) -0.0143(11) 0.0025(10) -0.0082(11) C15 0.0370(13) 0.0490(15) 0.0265(12) -0.0113(11) -0.0032(10) -0.0076(11) C16 0.0419(13) 0.0338(13) 0.0226(11) -0.0068(10) -0.0031(10) -0.0012(10) C17 0.0395(14) 0.0684(19) 0.0279(13) -0.0206(13) -0.0012(11) 0.0065(13) C18 0.0323(13) 0.0673(19) 0.0362(14) -0.0236(14) -0.0076(11) 0.0056(12) C20 0.0398(13) 0.0362(13) 0.0255(12) -0.0089(10) -0.0050(10) 0.0040(10) C21 0.0449(14) 0.0359(13) 0.0288(13) -0.0089(11) -0.0006(11) -0.0008(10) C22 0.0468(15) 0.0492(16) 0.0378(15) -0.0055(12) -0.0097(12) -0.0088(12) C23 0.065(2) 0.061(2) 0.0552(19) -0.0162(16) -0.0107(16) -0.0222(16) C24 0.069(2) 0.0488(18) 0.068(2) -0.0157(16) -0.0015(18) -0.0197(15) C25 0.080(2) 0.0369(16) 0.0500(18) -0.0012(14) -0.0063(16) -0.0092(15) C26 0.0616(18) 0.0414(15) 0.0341(14) -0.0069(12) -0.0103(13) -0.0035(13) C30 0.0434(14) 0.0366(13) 0.0270(12) -0.0097(10) -0.0051(10) 0.0004(10) C31 0.0568(16) 0.0369(14) 0.0239(12) -0.0068(10) -0.0070(11) -0.0034(12) C32 0.077(2) 0.0349(14) 0.0245(12) -0.0066(11) -0.0028(13) -0.0057(13) C33 0.101(3) 0.0361(15) 0.0298(14) -0.0119(12) -0.0030(15) -0.0060(16) C34 0.123(3) 0.0512(19) 0.0433(18) -0.0140(15) -0.018(2) -0.026(2) C35 0.084(3) 0.075(2) 0.060(2) -0.0107(19) -0.0152(19) -0.038(2) C36 0.0575(19) 0.0587(19) 0.0504(18) -0.0150(15) -0.0082(15) -0.0085(15) C41 0.0520(15) 0.0333(13) 0.0236(12) -0.0064(10) -0.0002(11) -0.0047(11) C42 0.086(2) 0.0377(15) 0.0304(14) -0.0109(12) -0.0099(14) 0.0122(14) C43 0.100(3) 0.0449(17) 0.0295(15) -0.0086(13) -0.0166(16) 0.0041(17) C44 0.087(2) 0.0581(19) 0.0270(14) -0.0164(13) 0.0038(14) -0.0151(17) C45 0.072(2) 0.067(2) 0.0477(18) -0.0306(17) 0.0030(16) 0.0092(17) C46 0.0599(18) 0.0567(18) 0.0380(16) -0.0176(14) -0.0052(13) 0.0083(14) S2 0.0370(3) 0.0504(4) 0.0322(3) -0.0191(3) -0.0029(3) -0.0054(3) C51 0.0581(17) 0.0389(14) 0.0251(12) -0.0099(11) -0.0018(11) -0.0051(12) C52 0.070(2) 0.0536(18) 0.0377(16) -0.0155(14) -0.0136(14) -0.0084(15) C53 0.100(3) 0.0571(19) 0.0312(15) -0.0208(14) -0.0140(16) -0.0110(18) C54 0.106(3) 0.0516(19) 0.0296(15) -0.0203(14) 0.0031(16) -0.0046(18) C55 0.071(2) 0.0424(16) 0.0347(15) -0.0153(12) 0.0088(14) -0.0010(14) C56 0.0538(16) 0.0343(13) 0.0255(12) -0.0101(10) 0.0008(11) -0.0044(11) N57 0.0404(11) 0.0330(11) 0.0258(10) -0.0086(8) 0.0022(8) -0.0032(8) C58 0.0363(12) 0.0333(12) 0.0254(12) -0.0094(10) 0.0004(10) -0.0047(10) C59 0.0384(14) 0.0419(15) 0.0413(15) -0.0146(12) 0.0031(11) 0.0011(11) C60 0.0503(17) 0.0548(19) 0.070(2) -0.0179(17) 0.0171(16) -0.0099(14) C61 0.0341(12) 0.0394(13) 0.0267(12) -0.0111(10) -0.0020(10) -0.0049(10) C62 0.0349(12) 0.0386(13) 0.0251(12) -0.0103(10) -0.0034(10) -0.0043(10) C63 0.0370(12) 0.0325(12) 0.0250(12) -0.0089(10) -0.0024(10) -0.0049(10) C64 0.0329(12) 0.0432(14) 0.0253(12) -0.0136(10) 0.0041(9) -0.0059(10) C65 0.0334(12) 0.0411(14) 0.0261(12) -0.0077(10) -0.0031(10) -0.0058(10) C66 0.0429(13) 0.0308(12) 0.0229(11) -0.0079(10) -0.0026(10) -0.0053(10) C67 0.0442(14) 0.0404(14) 0.0295(13) -0.0147(11) -0.0028(11) 0.0053(11) C68 0.0365(13) 0.0451(15) 0.0290(13) -0.0131(11) -0.0072(10) 0.0047(10) C70 0.0439(14) 0.0352(13) 0.0254(12) -0.0106(10) -0.0021(10) -0.0056(10) C71 0.0503(15) 0.0368(14) 0.0280(12) -0.0115(11) -0.0066(11) -0.0068(11) C72 0.072(2) 0.0418(16) 0.0337(15) -0.0066(12) 0.0000(14) -0.0069(14) C73 0.087(3) 0.0402(17) 0.0518(19) -0.0028(14) -0.0077(18) -0.0164(16) C74 0.072(2) 0.0367(16) 0.069(2) -0.0178(15) -0.0118(18) -0.0051(14) C75 0.071(2) 0.0513(18) 0.064(2) -0.0317(17) 0.0083(17) -0.0070(15) C76 0.0666(19) 0.0414(15) 0.0458(17) -0.0172(13) 0.0076(14) -0.0086(13) C80 0.0446(14) 0.0404(14) 0.0270(12) -0.0123(11) -0.0004(10) -0.0068(11) C81 0.0602(17) 0.0406(15) 0.0299(13) -0.0100(11) -0.0104(12) -0.0032(12) C82 0.098(3) 0.065(2) 0.0474(19) -0.0126(16) -0.0247(19) -0.0284(19) C83 0.193(6) 0.085(3) 0.075(3) -0.016(3) -0.071(4) -0.045(3) C84 0.204(6) 0.090(3) 0.047(2) -0.023(2) -0.059(3) -0.011(4) C85 0.133(4) 0.069(2) 0.0285(16) -0.0110(16) -0.017(2) 0.002(2) C86 0.082(2) 0.0465(17) 0.0285(14) -0.0079(12) -0.0055(14) -0.0034(15) C91 0.0470(14) 0.0368(13) 0.0240(12) -0.0063(10) 0.0008(10) -0.0075(11) C92 0.0486(15) 0.0454(15) 0.0413(15) -0.0091(13) -0.0076(12) -0.0061(12) C93 0.0530(17) 0.0454(16) 0.0506(17) -0.0139(14) -0.0052(14) 0.0034(13) C94 0.076(2) 0.0372(15) 0.0371(15) -0.0112(12) -0.0038(14) -0.0025(14) C95 0.0631(18) 0.0399(14) 0.0278(13) -0.0090(11) -0.0050(12) -0.0151(12) C96 0.0463(14) 0.0412(14) 0.0259(12) -0.0087(11) -0.0006(11) -0.0077(11) O1S 0.168(4) 0.077(2) 0.138(3) -0.054(2) -0.029(3) -0.013(2) O2S 0.138(3) 0.075(2) 0.098(2) -0.0380(19) -0.010(2) -0.0185(19) C1S 0.063(2) 0.065(2) 0.101(3) -0.037(2) -0.001(2) -0.0115(18) C2S 0.097(4) 0.165(6) 0.091(4) -0.049(4) -0.011(3) -0.050(4) C3S 0.150(6) 0.106(4) 0.098(4) -0.050(3) -0.025(4) -0.005(4) C4S 0.139(6) 0.175(7) 0.106(5) -0.007(5) 0.014(4) -0.029(5) P1 0.0270(3) 0.0409(4) 0.0551(5) -0.0075(3) -0.0038(3) -0.0013(3) P2 0.0277(10) 0.0413(13) 0.046(2) -0.0149(13) 0.0056(13) 0.0007(8) F1 0.0361(8) 0.0638(11) 0.0630(11) -0.0258(9) -0.0161(8) 0.0094(7) F2 0.0450(10) 0.0830(15) 0.0875(16) 0.0193(12) -0.0154(11) 0.0103(10) F3 0.042(2) 0.037(3) 0.078(4) -0.032(3) -0.006(2) 0.006(2) F4 0.032(2) 0.046(3) 0.097(5) -0.002(3) 0.016(2) -0.016(2) F5 0.053(3) 0.084(4) 0.036(2) -0.023(3) 0.003(2) -0.009(3) F6 0.0253(17) 0.038(2) 0.048(2) -0.020(2) 0.0065(16) -0.0075(14) P3 0.0290(11) 0.0431(15) 0.053(3) -0.0111(15) 0.0048(15) 0.0029(9) F11 0.0396(9) 0.0880(14) 0.0751(13) -0.0428(11) -0.0104(9) 0.0065(9) F12 0.0326(19) 0.062(3) 0.064(3) -0.015(2) -0.011(2) 0.0073(18) F12A 0.056(3) 0.076(4) 0.076(4) -0.002(3) -0.015(3) 0.020(3) F13 0.084(4) 0.079(4) 0.183(7) -0.087(5) -0.024(4) 0.013(3) F13A 0.055(4) 0.054(3) 0.139(8) 0.029(3) -0.039(4) -0.023(3) F14 0.036(2) 0.084(3) 0.064(3) 0.010(3) 0.0018(18) 0.003(2) F14A 0.052(3) 0.107(4) 0.139(6) -0.077(4) 0.001(3) 0.022(3) F15 0.071(3) 0.042(2) 0.094(4) -0.012(2) -0.032(3) -0.0036(19) F15A 0.063(3) 0.077(3) 0.156(6) 0.028(4) 0.008(4) -0.026(3) F16 0.045(3) 0.221(11) 0.065(3) -0.014(6) 0.030(3) -0.002(6) F16A 0.072(4) 0.218(9) 0.083(5) -0.102(6) -0.030(3) 0.033(5) _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 S1 C1 1.732(3) . ? S1 C8 1.726(2) . ? C1 C2 1.394(4) . ? C1 C6 1.388(4) . ? C2 C3 1.380(4) . ? C3 C4 1.392(5) . ? C4 C5 1.381(4) . ? C5 C6 1.396(4) . ? C6 N7 1.403(3) . ? N7 C8 1.329(3) . ? N7 C9 1.486(3) . ? C8 C11 1.432(3) . ? C9 C10 1.518(4) . ? C11 C12 1.345(3) . ? C12 C13 1.453(3) . ? C13 C14 1.395(4) . ? C13 C18 1.397(4) . ? C14 C15 1.387(3) . ? C15 C16 1.396(4) . ? C16 C17 1.388(4) . ? C16 C20 1.498(3) . ? C17 C18 1.384(4) . ? C20 C21 1.482(4) . ? C20 C30 1.359(4) . ? C21 C22 1.394(4) . ? C21 C26 1.406(4) . ? C22 C23 1.383(4) . ? C23 C24 1.381(5) . ? C24 C25 1.372(5) . ? C25 C26 1.386(4) . ? C30 C31 1.487(4) . ? C30 C41 1.501(3) . ? C31 C32 1.389(4) . ? C31 C36 1.392(4) . ? C32 C33 1.379(4) . ? C33 C34 1.372(6) . ? C34 C35 1.390(6) . ? C35 C36 1.398(5) . ? C41 C42 1.390(4) . ? C41 C46 1.373(4) . ? C42 C43 1.377(4) . ? C43 C44 1.375(5) . ? C44 C45 1.381(5) . ? C45 C46 1.386(4) . ? S2 C51 1.736(3) . ? S2 C58 1.720(3) . ? C51 C52 1.390(4) . ? C51 C56 1.386(4) . ? C52 C53 1.384(5) . ? C53 C54 1.386(6) . ? C54 C55 1.382(5) . ? C55 C56 1.392(4) . ? C56 N57 1.405(3) . ? N57 C58 1.336(3) . ? N57 C59 1.476(3) . ? C58 C61 1.430(3) . ? C59 C60 1.511(4) . ? C61 C62 1.347(4) . ? C62 C63 1.454(3) . ? C63 C64 1.398(3) . ? C63 C68 1.398(4) . ? C64 C65 1.377(3) . ? C65 C66 1.397(4) . ? C66 C67 1.385(4) . ? C66 C70 1.492(3) . ? C67 C68 1.383(3) . ? C70 C71 1.488(4) . ? C70 C80 1.356(4) . ? C71 C72 1.392(4) . ? C71 C76 1.389(4) . ? C72 C73 1.379(4) . ? C73 C74 1.373(5) . ? C74 C75 1.385(5) . ? C75 C76 1.379(4) . ? C80 C81 1.483(4) . ? C80 C91 1.490(4) . ? C81 C82 1.381(5) . ? C81 C86 1.401(4) . ? C82 C83 1.388(5) . ? C83 C84 1.409(7) . ? C84 C85 1.387(7) . ? C85 C86 1.380(4) . ? C91 C92 1.399(4) . ? C91 C96 1.387(4) . ? C92 C93 1.386(4) . ? C93 C94 1.389(5) . ? C94 C95 1.383(4) . ? C95 C96 1.386(4) . ? O1S C1S 1.187(5) . ? O2S C1S 1.305(5) . ? O2S C3S 1.469(6) . ? C1S C2S 1.479(6) . ? C3S C4S 1.429(8) . ? O11S C11S 1.189(11) . ? O12S C11S 1.188(11) . ? O12S C13S 1.562(14) . ? C11S C12S 1.536(12) . ? C13S C14S 1.518(15) . ? O21S C21S 1.257(13) . ? O22S C21S 1.265(12) . ? O22S C23S 1.541(11) . ? C21S C22S 1.520(13) . ? C23S C24S 1.486(11) . ? P1 F1 1.5912(16) . ? P1 F2 1.5927(18) . ? P1 F3 1.654(4) . ? P1 F3B 1.500(11) . ? P1 F3A 1.629(10) . ? P1 F4 1.595(4) . ? P1 F4B 1.631(9) . ? P1 F4A 1.602(12) . ? P1 F5 1.555(4) . ? P1 F5B 1.695(8) . ? P1 F5A 1.595(10) . ? P1 F6 1.610(3) . ? P1 F6B 1.553(10) . ? P1 F6A 1.579(9) . ? P2 F11 1.672(6) . ? P2 F12 1.609(7) . ? P2 F13 1.593(7) . ? P2 F14 1.555(7) . ? P2 F15 1.566(7) . ? P2 F16 1.581(7) . ? P3 F11 1.511(7) . ? P3 F12A 1.578(8) . ? P3 F13A 1.551(8) . ? P3 F14A 1.572(7) . ? P3 F15A 1.576(8) . ? P3 F16A 1.596(6) . ? 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 C8 S1 C1 91.29(12) . . ? C2 C1 S1 128.2(2) . . ? C6 C1 S1 110.36(19) . . ? C6 C1 C2 121.5(3) . . ? C3 C2 C1 117.6(3) . . ? C2 C3 C4 120.8(3) . . ? C5 C4 C3 122.2(3) . . ? C4 C5 C6 117.0(3) . . ? C1 C6 C5 121.0(2) . . ? C1 C6 N7 112.2(2) . . ? C5 C6 N7 126.8(2) . . ? C6 N7 C9 120.8(2) . . ? C8 N7 C6 114.2(2) . . ? C8 N7 C9 125.0(2) . . ? N7 C8 S1 111.93(18) . . ? N7 C8 C11 126.0(2) . . ? C11 C8 S1 122.02(18) . . ? N7 C9 C10 111.4(2) . . ? C12 C11 C8 122.0(2) . . ? C11 C12 C13 127.4(2) . . ? C14 C13 C12 122.8(2) . . ? C14 C13 C18 118.5(2) . . ? C18 C13 C12 118.6(2) . . ? C15 C14 C13 120.4(2) . . ? C14 C15 C16 121.2(2) . . ? C15 C16 C20 121.1(2) . . ? C17 C16 C15 118.1(2) . . ? C17 C16 C20 120.8(2) . . ? C18 C17 C16 121.2(3) . . ? C17 C18 C13 120.6(3) . . ? C21 C20 C16 115.7(2) . . ? C30 C20 C16 118.8(2) . . ? C30 C20 C21 125.4(2) . . ? C22 C21 C20 123.4(2) . . ? C22 C21 C26 116.8(3) . . ? C26 C21 C20 119.8(2) . . ? C23 C22 C21 121.5(3) . . ? C24 C23 C22 120.9(3) . . ? C25 C24 C23 118.8(3) . . ? C24 C25 C26 121.0(3) . . ? C25 C26 C21 121.1(3) . . ? C20 C30 C31 121.1(2) . . ? C20 C30 C41 124.2(2) . . ? C31 C30 C41 114.7(2) . . ? C32 C31 C30 121.1(3) . . ? C32 C31 C36 118.7(3) . . ? C36 C31 C30 120.2(3) . . ? C33 C32 C31 121.7(3) . . ? C34 C33 C32 119.5(3) . . ? C33 C34 C35 120.4(3) . . ? C34 C35 C36 119.9(4) . . ? C31 C36 C35 119.8(3) . . ? C42 C41 C30 119.5(2) . . ? C46 C41 C30 122.2(2) . . ? C46 C41 C42 118.2(3) . . ? C43 C42 C41 121.3(3) . . ? C44 C43 C42 119.7(3) . . ? C43 C44 C45 120.0(3) . . ? C44 C45 C46 119.7(3) . . ? C41 C46 C45 121.1(3) . . ? C58 S2 C51 91.15(13) . . ? C52 C51 S2 127.6(3) . . ? C56 C51 S2 110.6(2) . . ? C56 C51 C52 121.7(3) . . ? C53 C52 C51 117.1(3) . . ? C52 C53 C54 121.6(3) . . ? C55 C54 C53 121.1(3) . . ? C54 C55 C56 117.9(3) . . ? C51 C56 C55 120.5(3) . . ? C51 C56 N57 112.1(2) . . ? C55 C56 N57 127.3(3) . . ? C56 N57 C59 121.0(2) . . ? C58 N57 C56 113.8(2) . . ? C58 N57 C59 125.2(2) . . ? N57 C58 S2 112.28(18) . . ? N57 C58 C61 124.9(2) . . ? C61 C58 S2 122.71(19) . . ? N57 C59 C60 111.4(2) . . ? C62 C61 C58 122.4(2) . . ? C61 C62 C63 125.4(2) . . ? C64 C63 C62 122.0(2) . . ? C68 C63 C62 119.9(2) . . ? C68 C63 C64 118.2(2) . . ? C65 C64 C63 120.7(2) . . ? C64 C65 C66 121.0(2) . . ? C65 C66 C70 120.6(2) . . ? C67 C66 C65 118.2(2) . . ? C67 C66 C70 121.2(2) . . ? C68 C67 C66 121.2(2) . . ? C67 C68 C63 120.6(2) . . ? C71 C70 C66 114.6(2) . . ? C80 C70 C66 121.3(2) . . ? C80 C70 C71 124.0(2) . . ? C72 C71 C70 120.3(3) . . ? C76 C71 C70 122.0(2) . . ? C76 C71 C72 117.7(3) . . ? C73 C72 C71 121.5(3) . . ? C74 C73 C72 120.1(3) . . ? C73 C74 C75 119.3(3) . . ? C76 C75 C74 120.6(3) . . ? C75 C76 C71 120.8(3) . . ? C70 C80 C81 123.7(2) . . ? C70 C80 C91 121.7(2) . . ? C81 C80 C91 114.6(2) . . ? C82 C81 C80 121.2(3) . . ? C82 C81 C86 119.2(3) . . ? C86 C81 C80 119.6(3) . . ? C81 C82 C83 120.4(4) . . ? C82 C83 C84 119.5(4) . . ? C85 C84 C83 120.5(4) . . ? C86 C85 C84 118.8(4) . . ? C85 C86 C81 121.5(4) . . ? C92 C91 C80 119.8(2) . . ? C96 C91 C80 122.2(2) . . ? C96 C91 C92 118.0(3) . . ? C93 C92 C91 121.0(3) . . ? C92 C93 C94 119.7(3) . . ? C95 C94 C93 120.1(3) . . ? C94 C95 C96 119.6(3) . . ? C95 C96 C91 121.5(3) . . ? C1S O2S C3S 117.1(4) . . ? O1S C1S O2S 122.2(5) . . ? O1S C1S C2S 125.4(5) . . ? O2S C1S C2S 112.4(4) . . ? C4S C3S O2S 109.0(5) . . ? C11S O12S C13S 109.7(9) . . ? O11S C11S C12S 113.9(10) . . ? O12S C11S O11S 139.7(11) . . ? O12S C11S C12S 106.4(10) . . ? C14S C13S O12S 105.7(11) . . ? C21S O22S C23S 113.1(7) . . ? O21S C21S O22S 122.4(10) . . ? O21S C21S C22S 127.6(11) . . ? O22S C21S C22S 108.9(9) . . ? C24S C23S O22S 112.6(8) . . ? F1 P1 F2 179.43(14) . . ? F1 P1 F3 89.9(2) . . ? F1 P1 F3A 84.1(5) . . ? F1 P1 F4 86.0(2) . . ? F1 P1 F4B 92.9(4) . . ? F1 P1 F4A 90.9(6) . . ? F1 P1 F5B 84.5(3) . . ? F1 P1 F5A 95.0(5) . . ? F1 P1 F6 91.89(16) . . ? F2 P1 F3 89.6(2) . . ? F2 P1 F3A 95.3(5) . . ? F2 P1 F4 94.2(2) . . ? F2 P1 F4B 87.6(4) . . ? F2 P1 F4A 89.1(6) . . ? F2 P1 F5B 95.9(4) . . ? F2 P1 F5A 85.5(5) . . ? F2 P1 F6 87.90(16) . . ? F3 P1 F5B 154.6(4) . . ? F3B P1 F1 100.0(5) . . ? F3B P1 F2 79.6(5) . . ? F3B P1 F3 29.8(6) . . ? F3B P1 F3A 45.2(6) . . ? F3B P1 F4 61.3(7) . . ? F3B P1 F4B 93.5(7) . . ? F3B P1 F4A 45.6(7) . . ? F3B P1 F5 150.5(7) . . ? F3B P1 F5B 174.5(7) . . ? F3B P1 F5A 130.4(7) . . ? F3B P1 F6 114.9(7) . . ? F3B P1 F6B 95.7(8) . . ? F3B P1 F6A 132.7(8) . . ? F3A P1 F3 15.4(4) . . ? F3A P1 F4B 136.5(7) . . ? F3A P1 F5B 139.3(5) . . ? F4 P1 F3 88.1(4) . . ? F4 P1 F3A 101.8(5) . . ? F4 P1 F4B 34.8(5) . . ? F4 P1 F4A 15.8(6) . . ? F4 P1 F5B 116.1(5) . . ? F4 P1 F5A 73.1(5) . . ? F4 P1 F6 175.1(4) . . ? F4B P1 F3 122.1(6) . . ? F4B P1 F5B 83.0(6) . . ? F4A P1 F3 73.1(6) . . ? F4A P1 F3A 87.5(7) . . ? F4A P1 F4B 49.1(6) . . ? F4A P1 F5B 131.6(7) . . ? F4A P1 F6 160.4(6) . . ? F5 P1 F1 89.5(2) . . ? F5 P1 F2 91.0(2) . . ? F5 P1 F3 179.4(3) . . ? F5 P1 F3A 164.3(5) . . ? F5 P1 F4 91.9(4) . . ? F5 P1 F4B 57.9(5) . . ? F5 P1 F4A 107.0(6) . . ? F5 P1 F5B 25.3(3) . . ? F5 P1 F5A 20.1(4) . . ? F5 P1 F6 92.4(3) . . ? F5 P1 F6A 74.5(4) . . ? F5A P1 F3 160.1(5) . . ? F5A P1 F3A 175.0(6) . . ? F5A P1 F4B 38.5(5) . . ? F5A P1 F4A 87.6(7) . . ? F5A P1 F5B 45.3(5) . . ? F5A P1 F6 111.4(5) . . ? F6 P1 F3 87.6(3) . . ? F6 P1 F3A 73.6(4) . . ? F6 P1 F4B 149.9(6) . . ? F6 P1 F5B 67.9(4) . . ? F6B P1 F1 89.0(5) . . ? F6B P1 F2 90.7(5) . . ? F6B P1 F3 67.5(5) . . ? F6B P1 F3A 53.3(6) . . ? F6B P1 F4 155.0(5) . . ? F6B P1 F4B 170.2(7) . . ? F6B P1 F4A 140.5(7) . . ? F6B P1 F5 112.5(5) . . ? F6B P1 F5B 87.6(6) . . ? F6B P1 F5A 131.7(6) . . ? F6B P1 F6 20.3(4) . . ? F6B P1 F6A 38.0(5) . . ? F6A P1 F1 90.1(4) . . ? F6A P1 F2 89.9(4) . . ? F6A P1 F3 105.5(4) . . ? F6A P1 F3A 91.2(5) . . ? F6A P1 F4 165.9(5) . . ? F6A P1 F4B 132.3(6) . . ? F6A P1 F4A 178.2(7) . . ? F6A P1 F5B 50.0(5) . . ? F6A P1 F5A 93.8(6) . . ? F6A P1 F6 18.0(3) . . ? F12 P2 F11 176.2(5) . . ? F13 P2 F11 92.8(4) . . ? F13 P2 F12 88.9(4) . . ? F14 P2 F11 95.4(4) . . ? F14 P2 F12 88.0(4) . . ? F14 P2 F13 89.2(5) . . ? F14 P2 F15 91.1(4) . . ? F14 P2 F16 178.9(7) . . ? F15 P2 F11 89.0(4) . . ? F15 P2 F12 89.2(4) . . ? F15 P2 F13 178.1(5) . . ? F15 P2 F16 89.7(6) . . ? F16 P2 F11 85.4(4) . . ? F16 P2 F12 91.2(5) . . ? F16 P2 F13 90.0(6) . . ? F11 P3 F12A 176.1(6) . . ? F11 P3 F13A 95.2(4) . . ? F11 P3 F14A 91.5(3) . . ? F11 P3 F15A 83.9(4) . . ? F11 P3 F16A 86.0(4) . . ? F12A P3 F16A 93.2(4) . . ? F13A P3 F12A 88.6(5) . . ? F13A P3 F14A 90.8(5) . . ? F13A P3 F15A 179.1(6) . . ? F13A P3 F16A 92.0(6) . . ? F14A P3 F12A 89.1(5) . . ? F14A P3 F15A 89.3(5) . . ? F14A P3 F16A 176.4(6) . . ? F15A P3 F12A 92.3(5) . . ? F15A P3 F16A 87.8(6) . . ? P3 F11 P2 12.5(4) . . ? 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 S1 C1 C2 C3 179.9(2) . . . . ? S1 C1 C6 C5 -179.6(2) . . . . ? S1 C1 C6 N7 -1.6(3) . . . . ? S1 C8 C11 C12 -4.1(3) . . . . ? C1 S1 C8 N7 0.09(18) . . . . ? C1 S1 C8 C11 179.1(2) . . . . ? C1 C2 C3 C4 -0.4(4) . . . . ? C1 C6 N7 C8 1.8(3) . . . . ? C1 C6 N7 C9 -178.6(2) . . . . ? C2 C1 C6 C5 -0.3(4) . . . . ? C2 C1 C6 N7 177.6(2) . . . . ? C2 C3 C4 C5 -0.3(5) . . . . ? C3 C4 C5 C6 0.7(4) . . . . ? C4 C5 C6 C1 -0.4(4) . . . . ? C4 C5 C6 N7 -178.1(3) . . . . ? C5 C6 N7 C8 179.6(2) . . . . ? C5 C6 N7 C9 -0.8(4) . . . . ? C6 C1 C2 C3 0.8(4) . . . . ? C6 N7 C8 S1 -1.1(3) . . . . ? C6 N7 C8 C11 180.0(2) . . . . ? C6 N7 C9 C10 -80.1(3) . . . . ? N7 C8 C11 C12 174.7(2) . . . . ? C8 S1 C1 C2 -178.3(3) . . . . ? C8 S1 C1 C6 0.9(2) . . . . ? C8 N7 C9 C10 99.5(3) . . . . ? C8 C11 C12 C13 -177.4(2) . . . . ? C9 N7 C8 S1 179.32(18) . . . . ? C9 N7 C8 C11 0.4(4) . . . . ? C11 C12 C13 C14 0.8(4) . . . . ? C11 C12 C13 C18 178.4(3) . . . . ? C12 C13 C14 C15 178.2(2) . . . . ? C12 C13 C18 C17 -176.9(3) . . . . ? C13 C14 C15 C16 -1.9(4) . . . . ? C14 C13 C18 C17 0.9(4) . . . . ? C14 C15 C16 C17 1.6(4) . . . . ? C14 C15 C16 C20 -178.0(2) . . . . ? C15 C16 C17 C18 -0.2(4) . . . . ? C15 C16 C20 C21 -70.2(3) . . . . ? C15 C16 C20 C30 111.7(3) . . . . ? C16 C17 C18 C13 -1.1(5) . . . . ? C16 C20 C21 C22 149.1(3) . . . . ? C16 C20 C21 C26 -28.8(4) . . . . ? C16 C20 C30 C31 -7.7(4) . . . . ? C16 C20 C30 C41 173.1(2) . . . . ? C17 C16 C20 C21 110.2(3) . . . . ? C17 C16 C20 C30 -67.9(3) . . . . ? C18 C13 C14 C15 0.6(4) . . . . ? C20 C16 C17 C18 179.4(3) . . . . ? C20 C21 C22 C23 179.5(3) . . . . ? C20 C21 C26 C25 -179.0(3) . . . . ? C20 C30 C31 C32 -62.6(4) . . . . ? C20 C30 C31 C36 118.1(3) . . . . ? C20 C30 C41 C42 118.4(3) . . . . ? C20 C30 C41 C46 -60.6(4) . . . . ? C21 C20 C30 C31 174.4(2) . . . . ? C21 C20 C30 C41 -4.7(4) . . . . ? C21 C22 C23 C24 1.1(5) . . . . ? C22 C21 C26 C25 2.9(5) . . . . ? C22 C23 C24 C25 0.0(6) . . . . ? C23 C24 C25 C26 0.5(6) . . . . ? C24 C25 C26 C21 -2.0(5) . . . . ? C26 C21 C22 C23 -2.4(5) . . . . ? C30 C20 C21 C22 -33.0(4) . . . . ? C30 C20 C21 C26 149.1(3) . . . . ? C30 C31 C32 C33 179.9(2) . . . . ? C30 C31 C36 C35 -178.2(3) . . . . ? C30 C41 C42 C43 -175.9(3) . . . . ? C30 C41 C46 C45 177.9(3) . . . . ? C31 C30 C41 C42 -60.7(4) . . . . ? C31 C30 C41 C46 120.2(3) . . . . ? C31 C32 C33 C34 -1.7(4) . . . . ? C32 C31 C36 C35 2.5(4) . . . . ? C32 C33 C34 C35 2.4(5) . . . . ? C33 C34 C35 C36 -0.6(5) . . . . ? C34 C35 C36 C31 -1.8(5) . . . . ? C36 C31 C32 C33 -0.7(4) . . . . ? C41 C30 C31 C32 116.6(3) . . . . ? C41 C30 C31 C36 -62.7(3) . . . . ? C41 C42 C43 C44 -2.3(6) . . . . ? C42 C41 C46 C45 -1.2(5) . . . . ? C42 C43 C44 C45 -0.6(6) . . . . ? C43 C44 C45 C46 2.5(6) . . . . ? C44 C45 C46 C41 -1.6(6) . . . . ? C46 C41 C42 C43 3.1(5) . . . . ? S2 C51 C52 C53 178.6(2) . . . . ? S2 C51 C56 C55 -178.7(2) . . . . ? S2 C51 C56 N57 -0.9(3) . . . . ? S2 C58 C61 C62 -0.1(4) . . . . ? C51 S2 C58 N57 0.7(2) . . . . ? C51 S2 C58 C61 177.7(2) . . . . ? C51 C52 C53 C54 -0.2(5) . . . . ? C51 C56 N57 C58 1.5(3) . . . . ? C51 C56 N57 C59 -179.7(2) . . . . ? C52 C51 C56 C55 -0.4(4) . . . . ? C52 C51 C56 N57 177.4(3) . . . . ? C52 C53 C54 C55 -0.5(5) . . . . ? C53 C54 C55 C56 0.8(5) . . . . ? C54 C55 C56 C51 -0.3(4) . . . . ? C54 C55 C56 N57 -177.7(3) . . . . ? C55 C56 N57 C58 179.1(3) . . . . ? C55 C56 N57 C59 -2.1(4) . . . . ? C56 C51 C52 C53 0.7(4) . . . . ? C56 N57 C58 S2 -1.4(3) . . . . ? C56 N57 C58 C61 -178.3(2) . . . . ? C56 N57 C59 C60 -80.9(3) . . . . ? N57 C58 C61 C62 176.6(2) . . . . ? C58 S2 C51 C52 -178.0(3) . . . . ? C58 S2 C51 C56 0.2(2) . . . . ? C58 N57 C59 C60 97.8(3) . . . . ? C58 C61 C62 C63 -175.6(2) . . . . ? C59 N57 C58 S2 179.89(19) . . . . ? C59 N57 C58 C61 2.9(4) . . . . ? C61 C62 C63 C64 8.4(4) . . . . ? C61 C62 C63 C68 -172.0(3) . . . . ? C62 C63 C64 C65 178.0(2) . . . . ? C62 C63 C68 C67 -180.0(2) . . . . ? C63 C64 C65 C66 1.1(4) . . . . ? C64 C63 C68 C67 -0.4(4) . . . . ? C64 C65 C66 C67 1.4(4) . . . . ? C64 C65 C66 C70 179.9(2) . . . . ? C65 C66 C67 C68 -3.4(4) . . . . ? C65 C66 C70 C71 -124.3(3) . . . . ? C65 C66 C70 C80 54.0(4) . . . . ? C66 C67 C68 C63 2.9(4) . . . . ? C66 C70 C71 C72 43.1(4) . . . . ? C66 C70 C71 C76 -135.0(3) . . . . ? C66 C70 C80 C81 -172.5(3) . . . . ? C66 C70 C80 C91 8.4(4) . . . . ? C67 C66 C70 C71 54.2(3) . . . . ? C67 C66 C70 C80 -127.5(3) . . . . ? C68 C63 C64 C65 -1.6(4) . . . . ? C70 C66 C67 C68 178.1(2) . . . . ? C70 C71 C72 C73 179.8(3) . . . . ? C70 C71 C76 C75 179.2(3) . . . . ? C70 C80 C81 C82 53.8(5) . . . . ? C70 C80 C81 C86 -128.0(3) . . . . ? C70 C80 C91 C92 -127.3(3) . . . . ? C70 C80 C91 C96 53.2(4) . . . . ? C71 C70 C80 C81 5.6(4) . . . . ? C71 C70 C80 C91 -173.5(2) . . . . ? C71 C72 C73 C74 1.9(5) . . . . ? C72 C71 C76 C75 1.0(5) . . . . ? C72 C73 C74 C75 -0.6(6) . . . . ? C73 C74 C75 C76 -0.4(6) . . . . ? C74 C75 C76 C71 0.2(6) . . . . ? C76 C71 C72 C73 -2.0(5) . . . . ? C80 C70 C71 C72 -135.1(3) . . . . ? C80 C70 C71 C76 46.8(4) . . . . ? C80 C81 C82 C83 180.0(4) . . . . ? C80 C81 C86 C85 177.8(3) . . . . ? C80 C91 C92 C93 177.7(3) . . . . ? C80 C91 C96 C95 -179.2(2) . . . . ? C81 C80 C91 C92 53.6(3) . . . . ? C81 C80 C91 C96 -125.9(3) . . . . ? C81 C82 C83 C84 0.6(8) . . . . ? C82 C81 C86 C85 -4.0(5) . . . . ? C82 C83 C84 C85 -0.9(9) . . . . ? C83 C84 C85 C86 -1.1(8) . . . . ? C84 C85 C86 C81 3.6(6) . . . . ? C86 C81 C82 C83 1.8(6) . . . . ? C91 C80 C81 C82 -127.1(3) . . . . ? C91 C80 C81 C86 51.1(4) . . . . ? C91 C92 C93 C94 2.2(5) . . . . ? C92 C91 C96 C95 1.2(4) . . . . ? C92 C93 C94 C95 -0.2(5) . . . . ? C93 C94 C95 C96 -1.3(4) . . . . ? C94 C95 C96 C91 0.7(4) . . . . ? C96 C91 C92 C93 -2.7(4) . . . . ? C1S O2S C3S C4S 178.2(5) . . . . ? C3S O2S C1S O1S -2.4(7) . . . . ? C3S O2S C1S C2S 179.2(5) . . . . ? C11S O12S C13S C14S 164.1(11) . . . . ? C13S O12S C11S O11S 5.8(19) . . . . ? C13S O12S C11S C12S -175.9(10) . . . . ? C21S O22S C23S C24S -173.7(9) . . . . ? C23S O22S C21S O21S -4.1(15) . . . . ? C23S O22S C21S C22S -172.8(8) . . . . ? F12 P2 F11 P3 -77(6) . . . . ? F12A P3 F11 P2 -83(7) . . . . ? F13 P2 F11 P3 41(2) . . . . ? F13A P3 F11 P2 87(2) . . . . ? F14 P2 F11 P3 130(2) . . . . ? F14A P3 F11 P2 178(2) . . . . ? F15 P2 F11 P3 -139(2) . . . . ? F15A P3 F11 P2 -93(2) . . . . ? F16 P2 F11 P3 -49(2) . . . . ? F16A P3 F11 P2 -4(2) . . . . ?