# Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is (c) The Royal Society of Chemistry 2009 data_1 _database_code_depnum_ccdc_archive 'CCDC 720651' # start Validation Reply Form _vrf_CHEMW03_1 ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE:The formula weight differs from that calculated due to unlocated solvent moieties - SQUEEZE used - see _refine_special_details ... ; _vrf_RFACR01_1 ; PROBLEM: The value of the weighted R factor is > 0.45 RESPONSE: Many crystals tried, best presented - disordered solvent, disordered anions and mobile alkyl chains lead to this high value. ... ; _vrf_PLAT084_1 ; PROBLEM: High R2 Value RESPONSE: Many crystals tried, best presented - disordered solvent, disordered anions and mobile alkyl chains lead to this high value. ... ; _vrf_PLAT220_1 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 6.06 Ratio RESPONSE: Many crystals tried, best presented - disordered solvent, disordered anions and mobile alkyl chains lead to this high value. ; _vrf_PLAT222_1 ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.65 Ratio RESPONSE: Many crystals tried, best presented - disordered solvent, disordered anions and mobile alkyl chains lead to this high value. ; _vrf_PLAT241_1 ; PROBLEM: Check High Ueq as Compared to Neighbors for C51 RESPONSE: Mobile alkyl chains lead to this anomalous value. ; _vrf_PLAT242_1 ; PROBLEM: Check Low Ueq as Compared to Neighbors for O52 RESPONSE: Mobile alkyl chains lead to this anomalous value. ; _vrf_PLAT043_1 ; PROBLEM: Check Reported Molecular Weight ................ 2584.44 RESPONSE: The formula weight differs from that calculated due to unlocated solvent moieties - SQUEEZE used - see _refine_special_details ; _vrf_PLAT044_1 ; PROBLEM: Calculated and Reported Dx Differ .............. ? RESPONSE:The formula weight differs from that calculated due to unlocated solvent moieties - SQUEEZE used - see _refine_special_details ; _vrf_PLAT234_1 ; PROBLEM: Large Hirshfeld Difference O49 -- C48 .. 0.32 Ang. RESPONSE:Many crystals tried, best presented - disordered solvent, disordered anions and mobile alkyl chains lead to this high value. ; _vrf_PLAT244_1 ; PROBLEM: Low Solvent Ueq as Compared to Neighbors for P1 RESPONSE: Constraints used on anion leading to low Ueq. ; _vrf_PLAT731_1 ; PROBLEM: Bond Calc 1.23(4), Rep 1.230(18) ...... 2.22 su-Ra C44 -C45 1.555 1.555 RESPONSE: Constraint used due to disorder. ; _vrf_PLAT790_1 ; PROBLEM:Centre of Gravity not Within Unit Cell: Resd. # 2 C40 H34 N4 O2 RESPONSE: Proximity to main moiety used as locator. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C74 H78 F24 N4 O12 P4 S4,6.5(H2 O),(C6 H14 O)' _chemical_formula_sum 'C80 H105 F24 N4 O19.50 P4 S4' _chemical_formula_weight 2142.80 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' 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' F F 0.0727 0.0534 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.216(4) _cell_length_b 54.971(12) _cell_length_c 13.678(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.254(7) _cell_angle_gamma 90.00 _cell_volume 10091(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5416 _cell_measurement_theta_min 21.3044 _cell_measurement_theta_max 68.5159 _exptl_crystal_description Prism _exptl_crystal_colour Green _exptl_crystal_size_max 0.8000 _exptl_crystal_size_mid 0.1000 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4436 _exptl_absorpt_coefficient_mu 2.427 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6313 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 126248 _diffrn_reflns_av_R_equivalents 0.0854 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -66 _diffrn_reflns_limit_k_max 65 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 68.05 _reflns_number_total 18198 _reflns_number_gt 11023 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Many crystal were tried. The best refinement is presented. One of the 4 Pf6 molecules is disordered into 2 halfweight occupancies. 4 water molecules in 8 disordered sites were located. SQUEEZE revealed 14 voids with a volume of 1528 A^3^ A^3^ with 334 e^-^ per unit cell. The 2 large voids were rationalised as 4 diisopropyl molecules and the reminder as 10 water molecules per unit cell. The appropriate number of C,H and O atoms are included in the refinement. Some restraints (DFIX) were used for part of the alkyl chin and the PF6 moieties. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00027(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 18198 _refine_ls_number_parameters 991 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.2291 _refine_ls_R_factor_gt 0.1969 _refine_ls_wR_factor_ref 0.5261 _refine_ls_wR_factor_gt 0.5064 _refine_ls_goodness_of_fit_ref 1.874 _refine_ls_restrained_S_all 1.877 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.8938(4) 0.39883(14) 0.0395(4) 0.0863(15) Uani 1 1 d . . . C2 C 0.8858(5) 0.37683(17) 0.0601(6) 0.092(2) Uani 1 1 d . . . H2A H 0.8884 0.3651 0.0100 0.111 Uiso 1 1 calc R . . C3 C 0.8732(5) 0.36823(16) 0.1516(6) 0.099(2) Uani 1 1 d . . . H3A H 0.8700 0.3513 0.1647 0.119 Uiso 1 1 calc R . . C4 C 0.8657(5) 0.38578(12) 0.2224(5) 0.0744(15) Uani 1 1 d . . . C5 C 0.8641(6) 0.40997(17) 0.1930(5) 0.101(2) Uani 1 1 d . . . H5A H 0.8500 0.4223 0.2350 0.121 Uiso 1 1 calc R . . C6 C 0.8833(6) 0.41652(16) 0.1017(5) 0.096(2) Uani 1 1 d . . . H6A H 0.8885 0.4331 0.0849 0.116 Uiso 1 1 calc R . . C7 C 0.8633(4) 0.37848(13) 0.3244(4) 0.0742(15) Uani 1 1 d . . . C8 C 0.8570(5) 0.35468(16) 0.3498(6) 0.098(2) Uani 1 1 d . . . H8A H 0.8496 0.3424 0.2991 0.117 Uiso 1 1 calc R . . C9 C 0.8613(5) 0.34809(14) 0.4527(5) 0.0873(18) Uani 1 1 d . . . H9A H 0.8539 0.3316 0.4694 0.105 Uiso 1 1 calc R . . N10 N 0.8756(4) 0.36498(13) 0.5230(4) 0.0832(15) Uani 1 1 d . . . C11 C 0.8764(5) 0.38851(17) 0.5021(5) 0.091(2) Uani 1 1 d . . . H11A H 0.8810 0.4002 0.5545 0.109 Uiso 1 1 calc R . . C12 C 0.8707(4) 0.39596(14) 0.4045(5) 0.0835(17) Uani 1 1 d . . . H12A H 0.8715 0.4128 0.3899 0.100 Uiso 1 1 calc R . . C13 C 0.8937(6) 0.35767(19) 0.6331(6) 0.111(3) Uani 1 1 d . . . H13A H 0.8628 0.3417 0.6358 0.134 Uiso 1 1 calc R . . H13B H 0.8643 0.3698 0.6681 0.134 Uiso 1 1 calc R . . C14 C 1.0032(6) 0.35630(18) 0.6851(6) 0.099(2) Uani 1 1 d . . . C15 C 1.0516(6) 0.3331(2) 0.6962(5) 0.112(3) Uani 1 1 d . . . H15A H 1.0131 0.3186 0.6783 0.135 Uiso 1 1 calc R . . C16 C 1.1575(8) 0.33178(18) 0.7343(6) 0.112(3) Uani 1 1 d . . . C17 C 1.2111(7) 0.3537(2) 0.7672(6) 0.116(3) Uani 1 1 d . . . C18 C 1.0574(6) 0.37661(17) 0.7246(5) 0.095(2) Uani 1 1 d . . . H18A H 1.0246 0.3916 0.7262 0.114 Uiso 1 1 calc R . . C19 C 1.1609(7) 0.37539(17) 0.7627(6) 0.103(2) Uani 1 1 d . . . H19A H 1.1980 0.3899 0.7862 0.123 Uiso 1 1 calc R . . C20 C 1.3271(6) 0.35408(19) 0.8030(5) 0.115(3) Uani 1 1 d . . . H20A H 1.3536 0.3657 0.8608 0.138 Uiso 1 1 calc R . . H20B H 1.3541 0.3377 0.8271 0.138 Uiso 1 1 calc R . . N21 N 1.3570(4) 0.36177(14) 0.7111(4) 0.0932(17) Uani 1 1 d . . . C22 C 1.3621(7) 0.38488(16) 0.6880(6) 0.101(2) Uani 1 1 d . . . H22A H 1.3554 0.3972 0.7341 0.121 Uiso 1 1 calc R . . C23 C 1.3769(5) 0.39113(18) 0.5978(6) 0.105(2) Uani 1 1 d . . . H23A H 1.3818 0.4078 0.5818 0.126 Uiso 1 1 calc R . . C24 C 1.3854(4) 0.37250(15) 0.5258(5) 0.0806(17) Uani 1 1 d . . . C25 C 1.3850(6) 0.34986(19) 0.5544(6) 0.110(3) Uani 1 1 d . . . H25A H 1.3937 0.3371 0.5112 0.132 Uiso 1 1 calc R . . C26 C 1.3718(6) 0.34442(17) 0.6495(5) 0.102(2) Uani 1 1 d . . . H26A H 1.3734 0.3279 0.6704 0.123 Uiso 1 1 calc R . . C27 C 1.3883(4) 0.38037(14) 0.4223(5) 0.0849(19) Uani 1 1 d . . . C28 C 1.3949(5) 0.40509(16) 0.3957(6) 0.092(2) Uani 1 1 d . . . H28A H 1.4035 0.4177 0.4452 0.110 Uiso 1 1 calc R . . C29 C 1.3884(5) 0.40993(15) 0.2960(7) 0.099(2) Uani 1 1 d . . . H29A H 1.3923 0.4264 0.2768 0.119 Uiso 1 1 calc R . . N30 N 1.3769(4) 0.39265(16) 0.2233(5) 0.0960(18) Uani 1 1 d . . . C31 C 1.3706(6) 0.36934(18) 0.2468(6) 0.097(2) Uani 1 1 d . . . H31A H 1.3619 0.3572 0.1951 0.116 Uiso 1 1 calc R . . C32 C 1.3769(5) 0.36273(14) 0.3482(5) 0.0874(18) Uani 1 1 d . . . H32A H 1.3732 0.3461 0.3653 0.105 Uiso 1 1 calc R . . C33 C 1.3542(5) 0.40074(19) 0.1141(6) 0.111(3) Uani 1 1 d . . . H33A H 1.3844 0.3893 0.0771 0.133 Uiso 1 1 calc R . . H33B H 1.3831 0.4171 0.1127 0.133 Uiso 1 1 calc R . . C34 C 1.2416(6) 0.4017(2) 0.0602(6) 0.109(3) Uani 1 1 d . . . C35 C 1.1971(6) 0.42429(19) 0.0584(6) 0.106(2) Uani 1 1 d . . . H35A H 1.2365 0.4382 0.0859 0.127 Uiso 1 1 calc R . . C36 C 1.0922(6) 0.4262(2) 0.0149(6) 0.112(3) Uani 1 1 d . . . H36A H 1.0594 0.4414 0.0097 0.135 Uiso 1 1 calc R . . C37 C 1.0379(6) 0.4045(2) -0.0207(4) 0.102(3) Uani 1 1 d . . . C38 C 1.0837(6) 0.38245(16) -0.0158(5) 0.095(2) Uani 1 1 d . . . H38A H 1.0449 0.3682 -0.0389 0.114 Uiso 1 1 calc R . . C39 C 1.1863(6) 0.38093(19) 0.0227(6) 0.109(2) Uani 1 1 d . . . H39A H 1.2187 0.3658 0.0234 0.131 Uiso 1 1 calc R . . C40 C 0.9251(6) 0.40534(19) -0.0532(5) 0.113(3) Uani 1 1 d . . . H40A H 0.9010 0.4218 -0.0782 0.135 Uiso 1 1 calc R . . H40B H 0.8957 0.3937 -0.1102 0.135 Uiso 1 1 calc R . . C41 C 1.2079(11) 0.3098(3) 0.7489(10) 0.165(5) Uani 1 1 d . . . O41 O 1.2930(8) 0.3040(2) 0.7613(11) 0.226(5) Uani 1 1 d . . . O42 O 1.1451(8) 0.2908(2) 0.7456(10) 0.204(4) Uani 1 1 d D . . C43 C 1.1947(13) 0.2678(4) 0.7387(17) 0.267(11) Uani 1 1 d D . . H43A H 1.2215 0.2680 0.6804 0.320 Uiso 1 1 calc R . . H43B H 1.2498 0.2644 0.8037 0.320 Uiso 1 1 calc R . . C44 C 1.1165(18) 0.2501(4) 0.7214(18) 0.237(8) Uiso 1 1 d D . . C45 C 1.042(2) 0.2375(6) 0.707(3) 0.355(16) Uiso 1 1 d D . . H45 H 0.9841 0.2277 0.6953 0.426 Uiso 1 1 calc R . . S46 S 1.11760(14) 0.34904(5) 0.47282(15) 0.1056(7) Uani 1 1 d . . . C46 C 1.1200(10) 0.3246(2) 0.4171(10) 0.166(5) Uani 1 1 d D . . S47 S 1.12491(14) 0.35320(4) 0.25934(14) 0.1017(7) Uani 1 1 d . . . C47 C 1.1260(8) 0.3254(2) 0.3075(8) 0.141(3) Uani 1 1 d D . . H47A H 1.1301 0.3111 0.2700 0.169 Uiso 1 1 calc R . . C48 C 1.1384(19) 0.2993(3) 0.4709(13) 0.223(9) Uani 1 1 d D . . H48A H 1.1403 0.2865 0.4208 0.267 Uiso 1 1 calc R . . H48B H 1.2027 0.2992 0.5285 0.267 Uiso 1 1 calc R . . O49 O 1.0666(12) 0.2956(2) 0.5051(12) 0.222(5) Uani 1 1 d . . . C50 C 0.9765(9) 0.2944(3) 0.4394(8) 0.164(6) Uani 1 1 d . . . H50A H 0.9802 0.2897 0.3709 0.197 Uiso 1 1 calc R . . H50B H 0.9462 0.3108 0.4323 0.197 Uiso 1 1 calc R . . C51 C 0.9084(18) 0.27659(18) 0.4685(12) 0.241(10) Uani 1 1 d . . . H51A H 0.9470 0.2631 0.5110 0.289 Uiso 1 1 calc R . . H51B H 0.8580 0.2698 0.4060 0.289 Uiso 1 1 calc R . . O52 O 0.8573(7) 0.29276(15) 0.5334(7) 0.156(3) Uani 1 1 d . . . C53 C 0.8033(18) 0.2844(3) 0.5730(19) 0.263(12) Uani 1 1 d . . . H53A H 0.8255 0.2672 0.5830 0.316 Uiso 1 1 calc R . . H53B H 0.7392 0.2840 0.5153 0.316 Uiso 1 1 calc R . . C54 C 0.773(2) 0.2884(3) 0.657(2) 0.278(12) Uani 1 1 d . . . H54A H 0.8008 0.2752 0.7078 0.333 Uiso 1 1 calc R . . H54B H 0.6998 0.2869 0.6341 0.333 Uiso 1 1 calc R . . O55 O 0.7985(7) 0.31050(13) 0.7096(6) 0.155(3) Uani 1 1 d . . . C56 C 0.7349(10) 0.3175(2) 0.7657(11) 0.164(5) Uani 1 1 d . . . H56A H 0.6711 0.3234 0.7166 0.197 Uiso 1 1 calc R . . H56B H 0.7203 0.3030 0.8016 0.197 Uiso 1 1 calc R . . C57 C 0.7773(10) 0.3360(2) 0.8401(8) 0.149(4) Uani 1 1 d . . . H57A H 0.8463 0.3312 0.8809 0.179 Uiso 1 1 calc R . . H57B H 0.7387 0.3370 0.8884 0.179 Uiso 1 1 calc R . . O58 O 0.7791(5) 0.35979(12) 0.7948(4) 0.1171(18) Uani 1 1 d . . . C59 C 0.6878(7) 0.3742(2) 0.7805(8) 0.128(3) Uani 1 1 d . . . H59A H 0.6921 0.3829 0.8452 0.154 Uiso 1 1 calc R . . H59B H 0.6287 0.3634 0.7618 0.154 Uiso 1 1 calc R . . C60 C 0.6793(7) 0.3926(2) 0.6918(6) 0.124(3) Uani 1 1 d . . . H60A H 0.6280 0.4051 0.6884 0.149 Uiso 1 1 calc R . . H60B H 0.7438 0.4009 0.7026 0.149 Uiso 1 1 calc R . . O61 O 0.6516(4) 0.37834(11) 0.5987(5) 0.1168(17) Uani 1 1 d D . . C62 C 0.6450(5) 0.39018(19) 0.5098(6) 0.097(2) Uani 1 1 d D . . C63 C 0.6505(5) 0.4138(2) 0.5012(7) 0.106(3) Uani 1 1 d . . . H63A H 0.6579 0.4237 0.5602 0.127 Uiso 1 1 calc R . . C64 C 0.6456(5) 0.42543(17) 0.4029(6) 0.102(2) Uani 1 1 d . . . H64A H 0.6534 0.4425 0.3968 0.123 Uiso 1 1 calc R . . C65 C 0.6294(6) 0.4101(2) 0.3219(7) 0.122(3) Uani 1 1 d . . . H65A H 0.6235 0.4169 0.2563 0.146 Uiso 1 1 calc R . . C66 C 0.6208(5) 0.38498(18) 0.3286(6) 0.100(2) Uani 1 1 d . . . C67 C 0.6069(5) 0.3700(2) 0.2379(6) 0.119(3) Uani 1 1 d D . . C68 C 0.6020(6) 0.3449(2) 0.2469(9) 0.119(3) Uani 1 1 d . . . H68A H 0.5952 0.3347 0.1889 0.142 Uiso 1 1 calc R . . C69 C 0.6071(6) 0.3349(2) 0.3420(10) 0.141(4) Uani 1 1 d . . . H69A H 0.6015 0.3178 0.3472 0.169 Uiso 1 1 calc R . . C70 C 0.6202(6) 0.34920(19) 0.4303(8) 0.116(3) Uani 1 1 d . . . H70A H 0.6245 0.3418 0.4945 0.139 Uiso 1 1 calc R . . C71 C 0.6269(5) 0.37448(17) 0.4225(6) 0.094(2) Uani 1 1 d . . . O72 O 0.5992(4) 0.38263(12) 0.1492(5) 0.121(2) Uani 1 1 d D . . C73 C 0.5915(6) 0.3688(2) 0.0568(8) 0.140(4) Uani 1 1 d D . . H73A H 0.5410 0.3558 0.0463 0.168 Uiso 1 1 calc R . . H73B H 0.6563 0.3613 0.0628 0.168 Uiso 1 1 calc R . . C74 C 0.5606(9) 0.3868(2) -0.0338(7) 0.154(4) Uani 1 1 d D . . H74A H 0.5506 0.3779 -0.0995 0.185 Uiso 1 1 calc R . . H74B H 0.4969 0.3946 -0.0375 0.185 Uiso 1 1 calc R . . O75 O 0.6381(5) 0.40549(18) -0.0202(7) 0.174(3) Uani 1 1 d D . . C76 C 0.5846(12) 0.4262(3) -0.0786(17) 0.268(12) Uani 1 1 d D . . H76A H 0.5242 0.4296 -0.0601 0.321 Uiso 1 1 calc R . . H76B H 0.5643 0.4230 -0.1538 0.321 Uiso 1 1 calc R . . C77 C 0.6529(15) 0.4469(3) -0.0514(13) 0.228(10) Uani 1 1 d D . . H77A H 0.6173 0.4620 -0.0825 0.274 Uiso 1 1 calc R . . H77B H 0.6783 0.4490 0.0248 0.274 Uiso 1 1 calc R . . O78 O 0.7333(6) 0.4428(3) -0.0885(9) 0.208(5) Uani 1 1 d D . . C79 C 0.765(2) 0.4636(4) -0.1327(18) 0.59(6) Uani 1 1 d D . . H79A H 0.7073 0.4712 -0.1855 0.710 Uiso 1 1 calc R . . H79B H 0.8139 0.4587 -0.1664 0.710 Uiso 1 1 calc R . . C80 C 0.8111(12) 0.4810(4) -0.0478(17) 0.267(13) Uani 1 1 d D . . H80A H 0.8247 0.4963 -0.0785 0.320 Uiso 1 1 calc R . . H80B H 0.7622 0.4847 -0.0124 0.320 Uiso 1 1 calc R . . O81 O 0.9032(7) 0.47289(16) 0.0297(7) 0.171(3) Uani 1 1 d D . . C82 C 0.9408(12) 0.4902(3) 0.1138(11) 0.178(5) Uiso 1 1 d D . . H82A H 0.9087 0.4876 0.1671 0.214 Uiso 1 1 calc R . . H82B H 0.9269 0.5071 0.0875 0.214 Uiso 1 1 calc R . . C83 C 1.0485(18) 0.4861(5) 0.158(2) 0.336(14) Uiso 1 1 d D . . H83A H 1.0781 0.4852 0.1016 0.403 Uiso 1 1 calc R . . H83B H 1.0804 0.4997 0.2042 0.403 Uiso 1 1 calc R . . O84 O 1.0644(13) 0.4639(3) 0.2141(14) 0.271(6) Uiso 1 1 d D . . C85 C 1.1641(16) 0.4618(4) 0.2943(17) 0.250(8) Uiso 1 1 d D . . H85A H 1.1828 0.4762 0.3399 0.300 Uiso 1 1 calc R . . H85B H 1.2175 0.4577 0.2654 0.300 Uiso 1 1 calc R . . S86 S 1.13323(14) 0.41139(4) 0.28300(16) 0.1063(7) Uani 1 1 d . . . C86 C 1.1294(13) 0.43866(18) 0.3489(10) 0.193(7) Uani 1 1 d . . . S87 S 1.12365(16) 0.40758(5) 0.49442(17) 0.1214(8) Uani 1 1 d . . . C87 C 1.1363(12) 0.4355(2) 0.4442(11) 0.172(5) Uani 1 1 d . . . H87A H 1.1489 0.4492 0.4888 0.207 Uiso 1 1 calc R . . C88 C 1.1269(6) 0.39319(19) 0.3797(6) 0.102(2) Uani 1 1 d . . . C89 C 1.1259(4) 0.3684(2) 0.3729(5) 0.103(3) Uani 1 1 d . . . P1 P -0.0469(2) 0.44931(5) 0.6796(2) 0.1217(8) Uiso 1 1 d D . . F1 F -0.0894(5) 0.44328(11) 0.5601(5) 0.161(2) Uiso 1 1 d D . . F2 F -0.0039(5) 0.45521(11) 0.7977(5) 0.155(2) Uiso 1 1 d D . . F3 F 0.0521(6) 0.43468(14) 0.6890(7) 0.190(3) Uiso 1 1 d D . . F4 F 0.0035(7) 0.47335(15) 0.6555(7) 0.212(3) Uiso 1 1 d D . . F5 F -0.0963(4) 0.42525(8) 0.7046(4) 0.1226(15) Uiso 1 1 d D . . F6 F -0.1429(5) 0.46495(12) 0.6626(6) 0.173(2) Uiso 1 1 d D . . P2 P -0.2156(3) 0.29494(7) 0.1242(3) 0.1635(12) Uiso 1 1 d D . . F7 F -0.1775(6) 0.27163(14) 0.1932(7) 0.194(3) Uiso 1 1 d D . . F8 F -0.2025(7) 0.28403(16) 0.0221(7) 0.212(3) Uiso 1 1 d D . . F9 F -0.1172(6) 0.30847(15) 0.1859(7) 0.201(3) Uiso 1 1 d D . . F10 F -0.2671(6) 0.31863(12) 0.0696(6) 0.174(2) Uiso 1 1 d D . . F11 F -0.2537(10) 0.3039(2) 0.2229(10) 0.289(5) Uiso 1 1 d D . . F12 F -0.3109(9) 0.2789(2) 0.0990(10) 0.268(5) Uiso 1 1 d D . . P3 P 0.4330(4) 0.28282(10) 0.4778(5) 0.2092(18) Uiso 1 1 d D . . F13 F 0.5071(8) 0.26323(18) 0.5425(8) 0.236(4) Uiso 1 1 d D . . F14 F 0.3547(11) 0.2614(3) 0.4290(13) 0.312(6) Uiso 1 1 d D . . F15 F 0.3643(9) 0.3027(2) 0.4061(10) 0.259(4) Uiso 1 1 d D . . F16 F 0.3853(13) 0.2890(3) 0.5636(13) 0.326(7) Uiso 1 1 d D . . F17 F 0.5116(9) 0.3037(2) 0.5230(10) 0.264(5) Uiso 1 1 d D . . F18 F 0.4969(15) 0.2780(4) 0.4032(15) 0.379(9) Uiso 1 1 d D . . P4 P 0.4223(4) 0.46398(10) 0.6325(4) 0.1290(16) Uiso 0.50 1 d PD . . F19 F 0.4008(17) 0.4590(4) 0.5129(13) 0.252(8) Uiso 0.50 1 d PD . . F20 F 0.4930(10) 0.4415(2) 0.6370(11) 0.169(4) Uiso 0.50 1 d PD . . F21 F 0.3306(14) 0.4486(3) 0.6381(18) 0.238(8) Uiso 0.50 1 d PD . . F22 F 0.3543(15) 0.4879(3) 0.6097(16) 0.309(12) Uiso 0.50 1 d PD . . F23 F 0.4546(11) 0.4693(3) 0.7520(9) 0.175(5) Uiso 0.50 1 d PD . . F24 F 0.5131(19) 0.4813(4) 0.626(4) 0.43(2) Uiso 0.50 1 d PD . . P5 P 0.5223(4) 0.52213(10) 0.8341(4) 0.1280(16) Uiso 0.50 1 d PD . . F25 F 0.5384(16) 0.5495(3) 0.8544(17) 0.237(8) Uiso 0.50 1 d PD . . F26 F 0.4620(16) 0.5139(4) 0.9019(15) 0.258(9) Uiso 0.50 1 d PD . . F27 F 0.4275(16) 0.5231(5) 0.7362(14) 0.277(10) Uiso 0.50 1 d PD . . F28 F 0.5868(17) 0.5301(4) 0.7686(17) 0.264(9) Uiso 0.50 1 d PD . . F29 F 0.613(2) 0.5114(7) 0.921(2) 0.384(18) Uiso 0.50 1 d PD . . F30 F 0.5130(14) 0.4948(3) 0.8028(14) 0.204(6) Uiso 0.50 1 d PD . . O91A O 0.3314(7) 0.42084(18) 0.8728(7) 0.088(2) Uiso 0.50 1 d P . . O91B O 0.3097(10) 0.4387(3) 0.8584(10) 0.127(4) Uiso 0.50 1 d P . . O92A O 0.3662(8) 0.3346(2) 1.0387(8) 0.100(3) Uiso 0.50 1 d P . . O92B O 0.3681(14) 0.3191(4) 1.0555(15) 0.176(6) Uiso 0.50 1 d P . . O93A O 0.5340(8) 0.3248(2) -0.1350(8) 0.099(3) Uiso 0.50 1 d P . . O93B O 0.5320(11) 0.3076(3) -0.1445(11) 0.138(4) Uiso 0.50 1 d P . . O94A O 0.8106(16) 0.4661(4) 0.2982(17) 0.191(7) Uiso 0.50 1 d P . . O94B O 0.8321(17) 0.4795(4) 0.3668(19) 0.207(8) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.064(3) 0.120(5) 0.073(3) 0.007(3) 0.021(2) 0.000(3) C2 0.066(4) 0.127(7) 0.081(4) -0.013(4) 0.020(3) -0.005(4) C3 0.083(5) 0.129(6) 0.080(4) -0.022(4) 0.021(3) 0.000(4) C4 0.069(4) 0.083(4) 0.073(3) 0.001(3) 0.027(3) 0.004(3) C5 0.083(5) 0.150(8) 0.074(4) -0.009(4) 0.030(3) -0.008(4) C6 0.094(5) 0.117(6) 0.080(4) 0.006(4) 0.032(4) -0.016(4) C7 0.060(3) 0.096(5) 0.069(3) 0.004(3) 0.026(3) 0.003(3) C8 0.082(5) 0.127(6) 0.081(4) -0.002(4) 0.023(3) -0.008(4) C9 0.076(4) 0.106(5) 0.084(4) 0.003(4) 0.033(3) -0.011(3) N10 0.051(3) 0.123(5) 0.077(3) 0.021(3) 0.023(2) 0.002(3) C11 0.055(4) 0.136(7) 0.086(4) -0.004(4) 0.028(3) 0.010(4) C12 0.056(3) 0.117(5) 0.078(4) -0.002(3) 0.023(3) -0.007(3) C13 0.091(6) 0.165(8) 0.081(4) 0.013(4) 0.032(4) 0.011(5) C14 0.077(5) 0.142(7) 0.087(4) 0.047(5) 0.038(4) 0.030(5) C15 0.091(5) 0.187(9) 0.061(4) 0.016(4) 0.029(4) -0.005(6) C16 0.136(8) 0.108(6) 0.082(4) 0.043(4) 0.023(5) 0.025(6) C17 0.101(6) 0.177(9) 0.066(4) 0.015(5) 0.020(4) 0.016(6) C18 0.081(5) 0.142(7) 0.064(3) -0.004(4) 0.026(3) 0.024(5) C19 0.104(6) 0.130(6) 0.079(4) 0.013(4) 0.037(4) 0.021(5) C20 0.083(5) 0.195(9) 0.059(3) 0.003(4) 0.012(3) 0.025(5) N21 0.071(3) 0.136(5) 0.064(3) -0.005(3) 0.011(2) 0.020(3) C22 0.134(7) 0.097(5) 0.074(4) -0.030(4) 0.037(4) -0.015(4) C23 0.076(5) 0.152(7) 0.085(4) -0.013(4) 0.022(4) -0.021(4) C24 0.056(3) 0.102(5) 0.076(4) -0.009(3) 0.012(3) 0.011(3) C25 0.099(6) 0.154(8) 0.079(4) -0.002(4) 0.030(4) 0.059(5) C26 0.094(5) 0.133(6) 0.073(4) 0.015(4) 0.019(4) 0.022(4) C27 0.050(3) 0.113(5) 0.080(4) -0.012(4) 0.005(3) 0.013(3) C28 0.069(4) 0.126(6) 0.082(4) 0.002(4) 0.027(3) -0.001(4) C29 0.073(4) 0.110(6) 0.110(6) 0.036(5) 0.024(4) -0.005(4) N30 0.058(3) 0.146(6) 0.086(4) -0.014(4) 0.027(3) 0.000(3) C31 0.083(5) 0.125(7) 0.082(4) 0.001(4) 0.027(3) 0.011(4) C32 0.065(4) 0.111(5) 0.086(4) 0.000(4) 0.024(3) 0.015(3) C33 0.059(4) 0.172(8) 0.098(5) 0.027(5) 0.023(4) -0.016(4) C34 0.069(4) 0.182(9) 0.082(4) 0.030(5) 0.033(4) 0.026(5) C35 0.070(4) 0.159(8) 0.085(4) 0.019(4) 0.023(3) -0.003(5) C36 0.084(5) 0.159(8) 0.098(5) 0.028(5) 0.035(4) 0.023(5) C37 0.079(5) 0.183(9) 0.043(3) 0.008(4) 0.017(3) -0.008(5) C38 0.080(5) 0.129(6) 0.074(4) -0.009(4) 0.023(3) 0.010(4) C39 0.075(5) 0.155(7) 0.091(5) -0.016(5) 0.021(4) -0.001(5) C40 0.082(5) 0.198(9) 0.056(3) 0.015(4) 0.020(3) 0.016(5) C41 0.126(10) 0.222(15) 0.142(9) 0.037(9) 0.037(7) -0.043(11) O41 0.102(6) 0.248(11) 0.336(16) 0.044(9) 0.082(8) 0.021(6) O42 0.164(9) 0.171(8) 0.273(12) 0.070(8) 0.066(8) 0.065(7) C43 0.171(15) 0.27(2) 0.28(2) -0.085(17) -0.034(14) -0.029(16) S46 0.0760(12) 0.159(2) 0.0800(11) 0.0126(11) 0.0235(9) 0.0078(11) C46 0.165(11) 0.155(10) 0.164(11) 0.073(9) 0.036(8) 0.003(8) S47 0.0731(11) 0.1498(18) 0.0783(10) 0.0070(10) 0.0199(8) 0.0058(10) C47 0.126(8) 0.188(10) 0.111(7) -0.010(6) 0.044(6) 0.005(7) C48 0.35(3) 0.185(13) 0.184(13) 0.000(10) 0.154(16) 0.090(15) O49 0.251(14) 0.202(9) 0.278(15) 0.002(9) 0.177(13) 0.021(9) C50 0.105(7) 0.292(18) 0.092(6) 0.042(8) 0.029(5) 0.059(9) C51 0.51(3) 0.068(6) 0.191(13) 0.002(6) 0.179(18) -0.013(10) O52 0.170(7) 0.153(6) 0.157(6) 0.007(5) 0.070(5) -0.016(5) C53 0.34(3) 0.209(17) 0.32(2) -0.158(17) 0.21(2) -0.163(18) C54 0.44(3) 0.139(11) 0.36(3) -0.089(14) 0.27(3) -0.090(15) O55 0.237(9) 0.122(5) 0.139(5) -0.021(4) 0.107(6) -0.040(5) C56 0.172(11) 0.171(10) 0.184(11) -0.043(9) 0.105(10) -0.068(9) C57 0.165(10) 0.173(10) 0.108(6) -0.018(7) 0.043(6) -0.042(8) O58 0.131(5) 0.139(5) 0.098(3) -0.011(3) 0.061(3) -0.031(4) C59 0.091(6) 0.169(8) 0.144(8) -0.032(6) 0.063(6) -0.040(6) C60 0.087(5) 0.192(9) 0.089(5) -0.025(6) 0.022(4) 0.019(5) O61 0.085(4) 0.151(5) 0.110(4) -0.027(3) 0.026(3) -0.012(3) C62 0.064(4) 0.124(7) 0.098(5) -0.005(5) 0.020(3) 0.004(4) C63 0.052(4) 0.159(8) 0.107(6) -0.026(5) 0.027(3) 0.007(4) C64 0.070(4) 0.131(6) 0.099(5) -0.019(4) 0.018(4) 0.009(4) C65 0.069(5) 0.189(10) 0.091(5) -0.050(6) 0.006(4) 0.028(5) C66 0.064(4) 0.126(6) 0.099(5) -0.041(5) 0.012(3) 0.014(4) C67 0.050(4) 0.193(10) 0.091(6) -0.029(6) -0.007(3) 0.024(5) C68 0.070(5) 0.139(8) 0.121(7) -0.054(6) -0.004(5) 0.012(5) C69 0.064(5) 0.157(8) 0.164(10) -0.063(8) -0.013(5) 0.012(5) C70 0.069(5) 0.134(8) 0.122(6) -0.029(5) 0.002(4) 0.012(4) C71 0.056(4) 0.137(7) 0.081(4) -0.019(4) 0.013(3) -0.005(4) O72 0.082(3) 0.173(5) 0.097(4) -0.041(4) 0.013(3) 0.021(3) C73 0.070(5) 0.191(10) 0.156(9) -0.071(8) 0.033(5) 0.021(5) C74 0.127(8) 0.263(14) 0.083(5) -0.046(7) 0.048(5) -0.031(9) O75 0.071(4) 0.263(10) 0.174(7) 0.006(6) 0.022(4) -0.023(5) C76 0.29(3) 0.211(18) 0.25(2) 0.030(17) 0.022(19) 0.126(19) C77 0.34(3) 0.202(15) 0.194(15) 0.085(13) 0.161(18) 0.134(17) O78 0.109(6) 0.339(15) 0.157(8) 0.027(8) 0.019(5) 0.079(7) C79 0.87(11) 0.70(9) 0.141(17) 0.11(3) 0.08(3) 0.62(9) C80 0.225(19) 0.30(2) 0.32(3) 0.20(2) 0.147(19) 0.122(18) O81 0.170(7) 0.170(7) 0.182(7) 0.066(6) 0.072(6) 0.015(6) S86 0.0714(11) 0.1495(18) 0.0953(12) 0.0068(11) 0.0238(9) 0.0013(10) C86 0.301(18) 0.092(6) 0.120(8) -0.021(6) -0.019(10) -0.021(8) S87 0.0760(12) 0.188(2) 0.0926(13) -0.0287(13) 0.0176(10) 0.0047(12) C87 0.249(15) 0.138(9) 0.128(9) 0.004(7) 0.060(9) 0.025(9) C88 0.078(5) 0.137(7) 0.086(5) 0.010(4) 0.020(4) 0.003(4) C89 0.044(3) 0.192(9) 0.064(4) 0.007(4) 0.006(3) -0.005(4) _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 N1 C2 1.256(9) . ? N1 C6 1.332(10) . ? N1 C40 1.519(9) . ? C2 C3 1.403(11) . ? C2 H2A 0.9500 . ? C3 C4 1.395(10) . ? C3 H3A 0.9500 . ? C4 C5 1.387(10) . ? C4 C7 1.462(8) . ? C5 C6 1.410(10) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C8 1.364(10) . ? C7 C12 1.435(9) . ? C8 C9 1.434(10) . ? C8 H8A 0.9500 . ? C9 N10 1.304(9) . ? C9 H9A 0.9500 . ? N10 C11 1.325(10) . ? N10 C13 1.497(9) . ? C11 C12 1.372(9) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.484(11) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C18 1.364(11) . ? C14 C15 1.434(12) . ? C15 C16 1.424(12) . ? C15 H15A 0.9500 . ? C16 C41 1.383(19) . ? C16 C17 1.415(13) . ? C17 C19 1.383(13) . ? C17 C20 1.558(12) . ? C18 C19 1.390(11) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 N21 1.514(10) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? N21 C22 1.317(10) . ? N21 C26 1.335(10) . ? C22 C23 1.363(11) . ? C22 H22A 0.9500 . ? C23 C24 1.453(11) . ? C23 H23A 0.9500 . ? C24 C25 1.305(11) . ? C24 C27 1.493(10) . ? C25 C26 1.406(11) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 C32 1.374(10) . ? C27 C28 1.418(10) . ? C28 C29 1.362(10) . ? C28 H28A 0.9500 . ? C29 N30 1.346(11) . ? C29 H29A 0.9500 . ? N30 C31 1.331(10) . ? N30 C33 1.488(10) . ? C31 C32 1.408(10) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 C34 1.527(10) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C39 1.383(13) . ? C34 C35 1.391(12) . ? C35 C36 1.416(11) . ? C35 H35A 0.9500 . ? C36 C37 1.417(13) . ? C36 H36A 0.9500 . ? C37 C38 1.366(11) . ? C37 C40 1.518(11) . ? C38 C39 1.381(11) . ? C38 H38A 0.9500 . ? C39 H39A 0.9500 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 O41 1.209(16) . ? C41 O42 1.368(15) . ? O42 C43 1.467(15) . ? C43 C44 1.435(17) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.230(18) . ? C45 H45 0.9500 . ? S46 C46 1.548(15) . ? S46 C89 1.766(9) . ? C46 C47 1.530(13) . ? C46 C48 1.556(14) . ? S47 C47 1.662(13) . ? S47 C89 1.759(9) . ? C47 H47A 0.9500 . ? C48 O49 1.27(2) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? O49 C50 1.302(16) . ? C50 C51 1.52(2) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 O52 1.591(17) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? O52 C53 1.170(19) . ? C53 C54 1.37(2) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 O55 1.394(16) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? O55 C56 1.419(13) . ? C56 C57 1.423(14) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 O58 1.453(13) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? O58 C59 1.477(12) . ? C59 C60 1.555(14) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 O61 1.436(10) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? O61 C62 1.356(9) . ? C62 C63 1.310(12) . ? C62 C71 1.425(12) . ? C63 C64 1.469(12) . ? C63 H63A 0.9500 . ? C64 C65 1.348(11) . ? C64 H64A 0.9500 . ? C65 C66 1.394(13) . ? C65 H65A 0.9500 . ? C66 C71 1.385(12) . ? C66 C67 1.447(12) . ? C67 O72 1.371(11) . ? C67 C68 1.388(14) . ? C68 C69 1.391(16) . ? C68 H68A 0.9500 . ? C69 C70 1.401(14) . ? C69 H69A 0.9500 . ? C70 C71 1.399(12) . ? C70 H70A 0.9500 . ? O72 C73 1.447(9) . ? C73 C74 1.530(13) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 O75 1.474(11) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? O75 C76 1.455(13) . ? C76 C77 1.462(16) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 O78 1.415(14) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? O78 C79 1.434(19) . ? C79 C80 1.480(18) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 O81 1.456(14) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? O81 C82 1.453(12) . ? C82 C83 1.466(17) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 O84 1.422(17) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? O84 C85 1.483(16) . ? C85 C86 1.63(3) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? S86 C88 1.685(9) . ? S86 C86 1.760(12) . ? C86 C87 1.287(18) . ? S87 C87 1.714(13) . ? S87 C88 1.771(9) . ? C87 H87A 0.9500 . ? C88 C89 1.367(13) . ? P1 F6 1.563(7) . ? P1 F2 1.561(7) . ? P1 F1 1.580(7) . ? P1 F5 1.587(5) . ? P1 F3 1.590(8) . ? P1 F4 1.589(9) . ? P2 F12 1.556(11) . ? P2 F10 1.559(7) . ? P2 F9 1.563(8) . ? P2 F7 1.578(8) . ? P2 F8 1.585(9) . ? P2 F11 1.686(12) . ? P3 F15 1.573(11) . ? P3 F13 1.561(10) . ? P3 F16 1.572(14) . ? P3 F17 1.577(11) . ? P3 F18 1.597(15) . ? P3 F14 1.607(13) . ? P4 F23 1.574(12) . ? P4 F20 1.581(12) . ? P4 F21 1.578(15) . ? P4 F19 1.586(15) . ? P4 F22 1.601(13) . ? P4 F24 1.628(16) . ? F23 F30 1.657(19) . ? P5 F26 1.525(16) . ? P5 F25 1.535(15) . ? P5 F28 1.541(16) . ? P5 F29 1.551(18) . ? P5 F30 1.558(14) . ? P5 F27 1.557(16) . ? O91A O91B 1.029(13) . ? O92A O92B 0.880(19) . ? O93A O93B 0.953(13) . ? O94A O94B 1.15(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 N1 C6 121.5(6) . . ? C2 N1 C40 119.2(7) . . ? C6 N1 C40 119.1(7) . . ? N1 C2 C3 124.9(7) . . ? N1 C2 H2A 117.6 . . ? C3 C2 H2A 117.6 . . ? C4 C3 C2 116.6(8) . . ? C4 C3 H3A 121.7 . . ? C2 C3 H3A 121.7 . . ? C5 C4 C3 117.3(7) . . ? C5 C4 C7 122.4(6) . . ? C3 C4 C7 120.2(7) . . ? C4 C5 C6 120.8(7) . . ? C4 C5 H5A 119.6 . . ? C6 C5 H5A 119.6 . . ? N1 C6 C5 118.3(7) . . ? N1 C6 H6A 120.9 . . ? C5 C6 H6A 120.9 . . ? C8 C7 C12 116.2(6) . . ? C8 C7 C4 122.1(6) . . ? C12 C7 C4 121.7(6) . . ? C7 C8 C9 120.5(7) . . ? C7 C8 H8A 119.7 . . ? C9 C8 H8A 119.7 . . ? N10 C9 C8 119.3(7) . . ? N10 C9 H9A 120.3 . . ? C8 C9 H9A 120.3 . . ? C9 N10 C11 123.0(6) . . ? C9 N10 C13 119.0(7) . . ? C11 N10 C13 118.0(7) . . ? N10 C11 C12 120.0(7) . . ? N10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C11 C12 C7 120.6(7) . . ? C11 C12 H12A 119.7 . . ? C7 C12 H12A 119.7 . . ? N10 C13 C14 107.5(6) . . ? N10 C13 H13A 110.2 . . ? C14 C13 H13A 110.2 . . ? N10 C13 H13B 110.2 . . ? C14 C13 H13B 110.2 . . ? H13A C13 H13B 108.5 . . ? C18 C14 C15 119.9(8) . . ? C18 C14 C13 121.0(8) . . ? C15 C14 C13 119.1(9) . . ? C16 C15 C14 119.8(9) . . ? C16 C15 H15A 120.1 . . ? C14 C15 H15A 120.1 . . ? C41 C16 C17 119.8(11) . . ? C41 C16 C15 122.1(11) . . ? C17 C16 C15 117.8(9) . . ? C19 C17 C16 120.3(9) . . ? C19 C17 C20 118.6(10) . . ? C16 C17 C20 121.0(10) . . ? C14 C18 C19 119.9(8) . . ? C14 C18 H18A 120.0 . . ? C19 C18 H18A 120.0 . . ? C18 C19 C17 121.7(9) . . ? C18 C19 H19A 119.2 . . ? C17 C19 H19A 119.2 . . ? N21 C20 C17 107.5(5) . . ? N21 C20 H20A 110.2 . . ? C17 C20 H20A 110.2 . . ? N21 C20 H20B 110.2 . . ? C17 C20 H20B 110.2 . . ? H20A C20 H20B 108.5 . . ? C22 N21 C26 120.3(7) . . ? C22 N21 C20 121.4(7) . . ? C26 N21 C20 118.1(8) . . ? N21 C22 C23 119.9(7) . . ? N21 C22 H22A 120.1 . . ? C23 C22 H22A 120.1 . . ? C22 C23 C24 120.5(8) . . ? C22 C23 H23A 119.7 . . ? C24 C23 H23A 119.7 . . ? C25 C24 C23 117.4(7) . . ? C25 C24 C27 124.4(6) . . ? C23 C24 C27 118.2(7) . . ? C24 C25 C26 119.7(8) . . ? C24 C25 H25A 120.2 . . ? C26 C25 H25A 120.2 . . ? N21 C26 C25 122.0(8) . . ? N21 C26 H26A 119.0 . . ? C25 C26 H26A 119.0 . . ? C32 C27 C28 119.2(7) . . ? C32 C27 C24 117.5(7) . . ? C28 C27 C24 123.1(6) . . ? C29 C28 C27 117.2(7) . . ? C29 C28 H28A 121.4 . . ? C27 C28 H28A 121.4 . . ? N30 C29 C28 123.6(7) . . ? N30 C29 H29A 118.2 . . ? C28 C29 H29A 118.2 . . ? C31 N30 C29 120.2(7) . . ? C31 N30 C33 121.3(7) . . ? C29 N30 C33 117.6(8) . . ? N30 C31 C32 119.9(7) . . ? N30 C31 H31A 120.1 . . ? C32 C31 H31A 120.1 . . ? C27 C32 C31 119.9(8) . . ? C27 C32 H32A 120.0 . . ? C31 C32 H32A 120.0 . . ? N30 C33 C34 109.9(6) . . ? N30 C33 H33A 109.7 . . ? C34 C33 H33A 109.7 . . ? N30 C33 H33B 109.7 . . ? C34 C33 H33B 109.7 . . ? H33A C33 H33B 108.2 . . ? C39 C34 C35 122.1(8) . . ? C39 C34 C33 121.9(9) . . ? C35 C34 C33 115.8(9) . . ? C34 C35 C36 118.9(9) . . ? C34 C35 H35A 120.6 . . ? C36 C35 H35A 120.6 . . ? C37 C36 C35 117.4(9) . . ? C37 C36 H36A 121.3 . . ? C35 C36 H36A 121.3 . . ? C38 C37 C36 122.3(7) . . ? C38 C37 C40 118.8(9) . . ? C36 C37 C40 118.5(9) . . ? C37 C38 C39 119.9(8) . . ? C37 C38 H38A 120.1 . . ? C39 C38 H38A 120.1 . . ? C38 C39 C34 119.4(9) . . ? C38 C39 H39A 120.3 . . ? C34 C39 H39A 120.3 . . ? N1 C40 C37 108.7(5) . . ? N1 C40 H40A 109.9 . . ? C37 C40 H40A 109.9 . . ? N1 C40 H40B 109.9 . . ? C37 C40 H40B 109.9 . . ? H40A C40 H40B 108.3 . . ? O41 C41 O42 114.5(16) . . ? O41 C41 C16 134.3(14) . . ? O42 C41 C16 111.2(13) . . ? C41 O42 C43 109.8(15) . . ? C44 C43 O42 103.3(16) . . ? C44 C43 H43A 111.1 . . ? O42 C43 H43A 111.1 . . ? C44 C43 H43B 111.1 . . ? O42 C43 H43B 111.1 . . ? H43A C43 H43B 109.1 . . ? C45 C44 C43 172(3) . . ? C44 C45 H45 180.0 . . ? C46 S46 C89 97.0(5) . . ? C47 C46 C48 115.6(12) . . ? C47 C46 S46 118.4(8) . . ? C48 C46 S46 124.7(10) . . ? C47 S47 C89 95.2(5) . . ? C46 C47 S47 114.6(8) . . ? C46 C47 H47A 122.7 . . ? S47 C47 H47A 122.7 . . ? O49 C48 C46 106.7(14) . . ? O49 C48 H48A 110.4 . . ? C46 C48 H48A 110.4 . . ? O49 C48 H48B 110.4 . . ? C46 C48 H48B 110.4 . . ? H48A C48 H48B 108.6 . . ? C48 O49 C50 118.7(18) . . ? O49 C50 C51 114.8(13) . . ? O49 C50 H50A 108.6 . . ? C51 C50 H50A 108.6 . . ? O49 C50 H50B 108.6 . . ? C51 C50 H50B 108.6 . . ? H50A C50 H50B 107.5 . . ? C50 C51 O52 103.5(9) . . ? C50 C51 H51A 111.1 . . ? O52 C51 H51A 111.1 . . ? C50 C51 H51B 111.1 . . ? O52 C51 H51B 111.1 . . ? H51A C51 H51B 109.0 . . ? C53 O52 C51 121.9(12) . . ? O52 C53 C54 139.3(15) . . ? O52 C53 H53A 102.3 . . ? C54 C53 H53A 102.3 . . ? O52 C53 H53B 102.3 . . ? C54 C53 H53B 102.3 . . ? H53A C53 H53B 104.8 . . ? C53 C54 O55 118.2(15) . . ? C53 C54 H54A 107.8 . . ? O55 C54 H54A 107.8 . . ? C53 C54 H54B 107.8 . . ? O55 C54 H54B 107.8 . . ? H54A C54 H54B 107.1 . . ? C54 O55 C56 114.2(11) . . ? C57 C56 O55 112.6(10) . . ? C57 C56 H56A 109.1 . . ? O55 C56 H56A 109.1 . . ? C57 C56 H56B 109.1 . . ? O55 C56 H56B 109.1 . . ? H56A C56 H56B 107.8 . . ? C56 C57 O58 113.7(10) . . ? C56 C57 H57A 108.8 . . ? O58 C57 H57A 108.8 . . ? C56 C57 H57B 108.8 . . ? O58 C57 H57B 108.8 . . ? H57A C57 H57B 107.7 . . ? C57 O58 C59 113.6(8) . . ? O58 C59 C60 106.9(7) . . ? O58 C59 H59A 110.3 . . ? C60 C59 H59A 110.3 . . ? O58 C59 H59B 110.3 . . ? C60 C59 H59B 110.3 . . ? H59A C59 H59B 108.6 . . ? O61 C60 C59 105.3(9) . . ? O61 C60 H60A 110.7 . . ? C59 C60 H60A 110.7 . . ? O61 C60 H60B 110.7 . . ? C59 C60 H60B 110.7 . . ? H60A C60 H60B 108.8 . . ? C62 O61 C60 116.8(8) . . ? C63 C62 O61 124.6(8) . . ? C63 C62 C71 121.7(8) . . ? O61 C62 C71 113.6(8) . . ? C62 C63 C64 121.8(8) . . ? C62 C63 H63A 119.1 . . ? C64 C63 H63A 119.1 . . ? C65 C64 C63 115.1(9) . . ? C65 C64 H64A 122.4 . . ? C63 C64 H64A 122.4 . . ? C64 C65 C66 124.0(10) . . ? C64 C65 H65A 118.0 . . ? C66 C65 H65A 118.0 . . ? C71 C66 C65 119.6(7) . . ? C71 C66 C67 120.5(10) . . ? C65 C66 C67 119.9(9) . . ? O72 C67 C68 126.2(9) . . ? O72 C67 C66 114.8(10) . . ? C68 C67 C66 119.1(9) . . ? C69 C68 C67 119.2(9) . . ? C69 C68 H68A 120.4 . . ? C67 C68 H68A 120.4 . . ? C68 C69 C70 122.3(11) . . ? C68 C69 H69A 118.8 . . ? C70 C69 H69A 118.8 . . ? C71 C70 C69 119.0(11) . . ? C71 C70 H70A 120.5 . . ? C69 C70 H70A 120.5 . . ? C66 C71 C70 120.0(8) . . ? C66 C71 C62 117.6(9) . . ? C70 C71 C62 122.4(8) . . ? C67 O72 C73 118.0(8) . . ? O72 C73 C74 106.7(8) . . ? O72 C73 H73A 110.4 . . ? C74 C73 H73A 110.4 . . ? O72 C73 H73B 110.4 . . ? C74 C73 H73B 110.4 . . ? H73A C73 H73B 108.6 . . ? O75 C74 C73 110.2(9) . . ? O75 C74 H74A 109.6 . . ? C73 C74 H74A 109.6 . . ? O75 C74 H74B 109.6 . . ? C73 C74 H74B 109.6 . . ? H74A C74 H74B 108.1 . . ? C76 O75 C74 104.2(10) . . ? O75 C76 C77 106.7(12) . . ? O75 C76 H76A 110.4 . . ? C77 C76 H76A 110.4 . . ? O75 C76 H76B 110.4 . . ? C77 C76 H76B 110.4 . . ? H76A C76 H76B 108.6 . . ? O78 C77 C76 109.3(13) . . ? O78 C77 H77A 109.8 . . ? C76 C77 H77A 109.8 . . ? O78 C77 H77B 109.8 . . ? C76 C77 H77B 109.8 . . ? H77A C77 H77B 108.3 . . ? C77 O78 C79 115.3(16) . . ? O78 C79 C80 107.7(17) . . ? O78 C79 H79A 110.2 . . ? C80 C79 H79A 110.2 . . ? O78 C79 H79B 110.2 . . ? C80 C79 H79B 110.2 . . ? H79A C79 H79B 108.5 . . ? O81 C80 C79 115.6(18) . . ? O81 C80 H80A 108.4 . . ? C79 C80 H80A 108.4 . . ? O81 C80 H80B 108.4 . . ? C79 C80 H80B 108.4 . . ? H80A C80 H80B 107.4 . . ? C82 O81 C80 112.6(14) . . ? O81 C82 C83 106.7(17) . . ? O81 C82 H82A 110.4 . . ? C83 C82 H82A 110.4 . . ? O81 C82 H82B 110.4 . . ? C83 C82 H82B 110.4 . . ? H82A C82 H82B 108.6 . . ? O84 C83 C82 108(2) . . ? O84 C83 H83A 110.1 . . ? C82 C83 H83A 110.1 . . ? O84 C83 H83B 110.1 . . ? C82 C83 H83B 110.1 . . ? H83A C83 H83B 108.4 . . ? C83 O84 C85 114.3(18) . . ? O84 C85 C86 92.4(15) . . ? O84 C85 H85A 113.2 . . ? C86 C85 H85A 113.2 . . ? O84 C85 H85B 113.2 . . ? C86 C85 H85B 113.2 . . ? H85A C85 H85B 110.6 . . ? C88 S86 C86 94.9(6) . . ? C87 C86 C85 129.5(12) . . ? C87 C86 S86 113.5(9) . . ? C85 C86 S86 111.3(14) . . ? C87 S87 C88 90.5(6) . . ? C86 C87 S87 123.0(10) . . ? C86 C87 H87A 118.5 . . ? S87 C87 H87A 118.5 . . ? C89 C88 S86 122.7(6) . . ? C89 C88 S87 120.2(6) . . ? S86 C88 S87 117.0(6) . . ? C88 C89 S47 122.0(6) . . ? C88 C89 S46 123.3(6) . . ? S47 C89 S46 114.5(7) . . ? F6 P1 F2 93.7(4) . . ? F6 P1 F1 86.8(4) . . ? F2 P1 F1 179.4(4) . . ? F6 P1 F5 93.7(4) . . ? F2 P1 F5 90.1(3) . . ? F1 P1 F5 90.1(3) . . ? F6 P1 F3 175.1(4) . . ? F2 P1 F3 89.2(4) . . ? F1 P1 F3 90.2(4) . . ? F5 P1 F3 90.2(4) . . ? F6 P1 F4 86.7(5) . . ? F2 P1 F4 89.5(4) . . ? F1 P1 F4 90.3(4) . . ? F5 P1 F4 179.5(5) . . ? F3 P1 F4 89.4(5) . . ? F12 P2 F10 97.4(6) . . ? F12 P2 F9 161.3(6) . . ? F10 P2 F9 93.2(5) . . ? F12 P2 F7 77.0(6) . . ? F10 P2 F7 168.4(5) . . ? F9 P2 F7 89.6(5) . . ? F12 P2 F8 86.5(6) . . ? F10 P2 F8 93.9(5) . . ? F9 P2 F8 108.2(5) . . ? F7 P2 F8 95.9(5) . . ? F12 P2 F11 81.7(7) . . ? F10 P2 F11 85.2(6) . . ? F9 P2 F11 84.0(5) . . ? F7 P2 F11 83.9(6) . . ? F8 P2 F11 167.9(7) . . ? F15 P3 F13 174.7(8) . . ? F15 P3 F16 89.1(8) . . ? F13 P3 F16 95.9(8) . . ? F15 P3 F17 87.3(7) . . ? F13 P3 F17 91.2(7) . . ? F16 P3 F17 88.6(8) . . ? F15 P3 F18 94.8(10) . . ? F13 P3 F18 80.0(9) . . ? F16 P3 F18 171.2(11) . . ? F17 P3 F18 83.8(9) . . ? F15 P3 F14 92.7(8) . . ? F13 P3 F14 88.6(7) . . ? F16 P3 F14 93.4(9) . . ? F17 P3 F14 178.0(9) . . ? F18 P3 F14 94.3(10) . . ? F23 P4 F20 98.1(8) . . ? F23 P4 F21 90.7(11) . . ? F20 P4 F21 95.9(9) . . ? F23 P4 F19 174.4(11) . . ? F20 P4 F19 78.9(9) . . ? F21 P4 F19 94.3(12) . . ? F23 P4 F22 90.0(8) . . ? F20 P4 F22 170.0(10) . . ? F21 P4 F22 89.8(9) . . ? F19 P4 F22 92.5(9) . . ? F23 P4 F24 88.8(18) . . ? F20 P4 F24 87.4(9) . . ? F21 P4 F24 176.7(11) . . ? F19 P4 F24 86.3(19) . . ? F22 P4 F24 86.9(9) . . ? P4 F23 F30 121.8(11) . . ? F26 P5 F25 105.3(13) . . ? F26 P5 F28 177.9(13) . . ? F25 P5 F28 75.2(12) . . ? F26 P5 F29 85.0(15) . . ? F25 P5 F29 101.4(18) . . ? F28 P5 F29 92.9(12) . . ? F26 P5 F30 82.3(12) . . ? F25 P5 F30 172.4(12) . . ? F28 P5 F30 97.3(12) . . ? F29 P5 F30 79.5(17) . . ? F26 P5 F27 91.8(10) . . ? F25 P5 F27 99.1(13) . . ? F28 P5 F27 90.1(13) . . ? F29 P5 F27 159.4(19) . . ? F30 P5 F27 79.8(12) . . ? P5 F30 F23 156.3(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 N1 C2 C3 -5.2(11) . . . . ? C40 N1 C2 C3 169.3(6) . . . . ? N1 C2 C3 C4 2.4(11) . . . . ? C2 C3 C4 C5 4.5(9) . . . . ? C2 C3 C4 C7 -173.3(6) . . . . ? C3 C4 C5 C6 -8.5(10) . . . . ? C7 C4 C5 C6 169.2(6) . . . . ? C2 N1 C6 C5 0.9(10) . . . . ? C40 N1 C6 C5 -173.6(6) . . . . ? C4 C5 C6 N1 6.1(11) . . . . ? C5 C4 C7 C8 174.7(6) . . . . ? C3 C4 C7 C8 -7.5(10) . . . . ? C5 C4 C7 C12 -7.2(9) . . . . ? C3 C4 C7 C12 170.5(6) . . . . ? C12 C7 C8 C9 -2.2(9) . . . . ? C4 C7 C8 C9 176.0(6) . . . . ? C7 C8 C9 N10 -2.8(10) . . . . ? C8 C9 N10 C11 7.0(9) . . . . ? C8 C9 N10 C13 -171.9(6) . . . . ? C9 N10 C11 C12 -5.7(9) . . . . ? C13 N10 C11 C12 173.2(6) . . . . ? N10 C11 C12 C7 0.2(9) . . . . ? C8 C7 C12 C11 3.5(9) . . . . ? C4 C7 C12 C11 -174.7(6) . . . . ? C9 N10 C13 C14 93.8(9) . . . . ? C11 N10 C13 C14 -85.2(8) . . . . ? N10 C13 C14 C18 83.8(9) . . . . ? N10 C13 C14 C15 -98.1(8) . . . . ? C18 C14 C15 C16 -9.5(10) . . . . ? C13 C14 C15 C16 172.3(6) . . . . ? C14 C15 C16 C41 178.4(9) . . . . ? C14 C15 C16 C17 4.7(10) . . . . ? C41 C16 C17 C19 -173.4(9) . . . . ? C15 C16 C17 C19 0.4(11) . . . . ? C41 C16 C17 C20 10.2(12) . . . . ? C15 C16 C17 C20 -176.0(6) . . . . ? C15 C14 C18 C19 8.9(10) . . . . ? C13 C14 C18 C19 -172.9(6) . . . . ? C14 C18 C19 C17 -3.7(11) . . . . ? C16 C17 C19 C18 -1.0(11) . . . . ? C20 C17 C19 C18 175.4(6) . . . . ? C19 C17 C20 N21 -80.4(9) . . . . ? C16 C17 C20 N21 96.1(9) . . . . ? C17 C20 N21 C22 84.3(10) . . . . ? C17 C20 N21 C26 -91.3(9) . . . . ? C26 N21 C22 C23 3.7(11) . . . . ? C20 N21 C22 C23 -171.8(7) . . . . ? N21 C22 C23 C24 1.1(12) . . . . ? C22 C23 C24 C25 -4.6(10) . . . . ? C22 C23 C24 C27 172.2(7) . . . . ? C23 C24 C25 C26 3.1(11) . . . . ? C27 C24 C25 C26 -173.4(6) . . . . ? C22 N21 C26 C25 -5.3(11) . . . . ? C20 N21 C26 C25 170.4(7) . . . . ? C24 C25 C26 N21 1.6(12) . . . . ? C25 C24 C27 C32 8.8(10) . . . . ? C23 C24 C27 C32 -167.7(6) . . . . ? C25 C24 C27 C28 -175.9(7) . . . . ? C23 C24 C27 C28 7.5(9) . . . . ? C32 C27 C28 C29 0.6(10) . . . . ? C24 C27 C28 C29 -174.6(6) . . . . ? C27 C28 C29 N30 -0.4(10) . . . . ? C28 C29 N30 C31 0.4(10) . . . . ? C28 C29 N30 C33 170.1(6) . . . . ? C29 N30 C31 C32 -0.5(10) . . . . ? C33 N30 C31 C32 -169.9(6) . . . . ? C28 C27 C32 C31 -0.8(9) . . . . ? C24 C27 C32 C31 174.6(6) . . . . ? N30 C31 C32 C27 0.8(10) . . . . ? C31 N30 C33 C34 77.6(10) . . . . ? C29 N30 C33 C34 -92.0(9) . . . . ? N30 C33 C34 C39 -79.5(10) . . . . ? N30 C33 C34 C35 95.6(9) . . . . ? C39 C34 C35 C36 -1.3(11) . . . . ? C33 C34 C35 C36 -176.4(6) . . . . ? C34 C35 C36 C37 2.6(10) . . . . ? C35 C36 C37 C38 -1.2(10) . . . . ? C35 C36 C37 C40 171.2(6) . . . . ? C36 C37 C38 C39 -1.5(10) . . . . ? C40 C37 C38 C39 -174.0(6) . . . . ? C37 C38 C39 C34 2.8(11) . . . . ? C35 C34 C39 C38 -1.4(12) . . . . ? C33 C34 C39 C38 173.4(7) . . . . ? C2 N1 C40 C37 -84.0(9) . . . . ? C6 N1 C40 C37 90.7(9) . . . . ? C38 C37 C40 N1 80.4(8) . . . . ? C36 C37 C40 N1 -92.4(8) . . . . ? C17 C16 C41 O41 -22(2) . . . . ? C15 C16 C41 O41 164.1(15) . . . . ? C17 C16 C41 O42 159.6(10) . . . . ? C15 C16 C41 O42 -14.0(15) . . . . ? O41 C41 O42 C43 -10.6(19) . . . . ? C16 C41 O42 C43 167.8(12) . . . . ? C41 O42 C43 C44 -172.3(15) . . . . ? C89 S46 C46 C47 -1.0(10) . . . . ? C89 S46 C46 C48 165.9(15) . . . . ? C48 C46 C47 S47 -170.3(13) . . . . ? S46 C46 C47 S47 -2.3(13) . . . . ? C89 S47 C47 C46 4.0(9) . . . . ? C47 C46 C48 O49 -129.7(15) . . . . ? S46 C46 C48 O49 63(2) . . . . ? C46 C48 O49 C50 62(2) . . . . ? C48 O49 C50 C51 145.6(13) . . . . ? O49 C50 C51 O52 91.0(16) . . . . ? C50 C51 O52 C53 -175.9(19) . . . . ? C51 O52 C53 C54 151(3) . . . . ? O52 C53 C54 O55 12(6) . . . . ? C53 C54 O55 C56 156(2) . . . . ? C54 O55 C56 C57 163.4(16) . . . . ? O55 C56 C57 O58 73.1(15) . . . . ? C56 C57 O58 C59 88.6(12) . . . . ? C57 O58 C59 C60 -155.3(7) . . . . ? O58 C59 C60 O61 72.4(8) . . . . ? C59 C60 O61 C62 -176.3(6) . . . . ? C60 O61 C62 C63 -8.4(10) . . . . ? C60 O61 C62 C71 174.2(6) . . . . ? O61 C62 C63 C64 178.2(6) . . . . ? C71 C62 C63 C64 -4.5(11) . . . . ? C62 C63 C64 C65 3.6(10) . . . . ? C63 C64 C65 C66 -2.1(11) . . . . ? C64 C65 C66 C71 1.4(12) . . . . ? C64 C65 C66 C67 -177.8(7) . . . . ? C71 C66 C67 O72 178.2(6) . . . . ? C65 C66 C67 O72 -2.7(10) . . . . ? C71 C66 C67 C68 -1.4(10) . . . . ? C65 C66 C67 C68 177.8(7) . . . . ? O72 C67 C68 C69 -177.4(7) . . . . ? C66 C67 C68 C69 2.1(11) . . . . ? C67 C68 C69 C70 -2.0(13) . . . . ? C68 C69 C70 C71 1.0(12) . . . . ? C65 C66 C71 C70 -178.8(7) . . . . ? C67 C66 C71 C70 0.4(11) . . . . ? C65 C66 C71 C62 -1.9(10) . . . . ? C67 C66 C71 C62 177.3(6) . . . . ? C69 C70 C71 C66 -0.2(11) . . . . ? C69 C70 C71 C62 -176.9(7) . . . . ? C63 C62 C71 C66 3.6(10) . . . . ? O61 C62 C71 C66 -178.9(6) . . . . ? C63 C62 C71 C70 -179.6(7) . . . . ? O61 C62 C71 C70 -2.1(10) . . . . ? C68 C67 O72 C73 -4.3(11) . . . . ? C66 C67 O72 C73 176.2(6) . . . . ? C67 O72 C73 C74 167.6(7) . . . . ? O72 C73 C74 O75 62.6(10) . . . . ? C73 C74 O75 C76 -154.8(12) . . . . ? C74 O75 C76 C77 168.9(13) . . . . ? O75 C76 C77 O78 66.4(19) . . . . ? C76 C77 O78 C79 139.3(16) . . . . ? C77 O78 C79 C80 69(2) . . . . ? O78 C79 C80 O81 66(2) . . . . ? C79 C80 O81 C82 -176.5(16) . . . . ? C80 O81 C82 C83 -155.1(15) . . . . ? O81 C82 C83 O84 -73(2) . . . . ? C82 C83 O84 C85 -157.7(19) . . . . ? C83 O84 C85 C86 166(2) . . . . ? O84 C85 C86 C87 -127(2) . . . . ? O84 C85 C86 S86 81.2(15) . . . . ? C88 S86 C86 C87 8.3(15) . . . . ? C88 S86 C86 C85 164.5(11) . . . . ? C85 C86 C87 S87 -163.9(15) . . . . ? S86 C86 C87 S87 -13(2) . . . . ? C88 S87 C87 C86 10.1(16) . . . . ? C86 S86 C88 C89 179.3(8) . . . . ? C86 S86 C88 S87 -1.9(7) . . . . ? C87 S87 C88 C89 175.8(8) . . . . ? C87 S87 C88 S86 -3.1(7) . . . . ? S86 C88 C89 S47 -3.2(9) . . . . ? S87 C88 C89 S47 177.9(4) . . . . ? S86 C88 C89 S46 -179.2(4) . . . . ? S87 C88 C89 S46 2.0(9) . . . . ? C47 S47 C89 C88 179.0(7) . . . . ? C47 S47 C89 S46 -4.7(5) . . . . ? C46 S46 C89 C88 179.9(7) . . . . ? C46 S46 C89 S47 3.7(6) . . . . ? F20 P4 F23 F30 114.1(13) . . . . ? F21 P4 F23 F30 -149.8(13) . . . . ? F22 P4 F23 F30 -60.0(14) . . . . ? F24 P4 F23 F30 27.0(15) . . . . ? F26 P5 F30 F23 64(3) . . . . ? F28 P5 F30 F23 -119(3) . . . . ? F29 P5 F30 F23 150(4) . . . . ? F27 P5 F30 F23 -30(3) . . . . ? P4 F23 F30 P5 82(4) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.081 0.011 -0.018 33 8 ' ' 2 0.909 -0.012 0.020 28 5 ' ' 3 0.641 0.021 0.033 22 3 ' ' 4 0.297 0.250 0.057 569 120 ' ' 5 0.703 0.750 0.006 569 130 ' ' 6 0.359 0.979 -0.033 22 5 ' ' 7 0.758 0.523 0.173 45 9 ' ' 8 0.242 0.023 0.328 45 12 ' ' 9 0.081 0.489 0.482 32 8 ' ' 10 0.359 0.521 0.467 22 5 ' ' 11 0.910 0.512 0.522 29 5 ' ' 12 0.641 0.479 0.533 22 3 ' ' 13 0.758 0.977 0.672 45 9 ' ' 14 0.242 0.477 0.828 45 12 ' ' _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 67.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.316 _refine_diff_density_min -0.937 _refine_diff_density_rms 0.132 data_stod2704smnew _database_code_depnum_ccdc_archive 'CCDC 720652' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H34 N4, C18 H24 O6, 4(F6 P), 6(C2 H3 N)' _chemical_formula_sum 'C67 H76 F24 N10 O6 P4' _chemical_formula_weight 1697.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.8934(9) _cell_length_b 23.2237(16) _cell_length_c 13.0531(9) _cell_angle_alpha 90.00 _cell_angle_beta 116.2620(10) _cell_angle_gamma 90.00 _cell_volume 3776.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5582 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 27.23 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 0.216 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9010 _exptl_absorpt_correction_T_max 0.9787 _exptl_absorpt_process_details 'Sadabs (Bruker)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23938 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0555 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 28.31 _reflns_number_total 9064 _reflns_number_gt 5614 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker Saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker Shelxtl' _computing_publication_material 'Bruker Shelxtl' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+3.4004P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9064 _refine_ls_number_parameters 562 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1083 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1538 _refine_ls_wR_factor_gt 0.1323 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.35000(7) 0.25255(4) 0.10486(7) 0.0453(2) Uani 1 1 d . . . F1 F 0.33066(17) 0.22394(9) 0.2040(2) 0.0719(7) Uani 1 1 d . . . F2 F 0.3710(2) 0.28217(10) 0.0071(2) 0.0938(8) Uani 1 1 d . . . F3 F 0.3495(3) 0.31367(9) 0.1569(2) 0.1003(9) Uani 1 1 d . . . F4 F 0.35411(19) 0.19125(9) 0.0544(2) 0.0763(7) Uani 1 1 d . . . F5 F 0.47589(16) 0.24760(11) 0.18088(19) 0.0804(7) Uani 1 1 d . . . F6 F 0.22532(19) 0.25729(14) 0.0297(2) 0.1075(10) Uani 1 1 d . . . P2 P 0.14036(6) 0.59063(3) 0.47493(6) 0.03209(18) Uani 1 1 d . . . F7 F 0.0948(6) 0.6408(2) 0.5167(7) 0.079(2) Uani 0.44 1 d P A 1 F8 F 0.2039(12) 0.5373(5) 0.4554(12) 0.079(2) Uani 0.34 1 d P A 1 F9 F 0.0900(3) 0.54669(13) 0.5335(4) 0.0572(7) Uani 0.64 1 d P A 1 F10 F 0.1951(3) 0.63283(15) 0.4240(3) 0.0572(7) Uani 0.64 1 d P A 1 F11 F 0.2419(4) 0.5988(2) 0.6017(3) 0.1065(13) Uani 0.60 1 d P A 1 F12 F 0.0465(4) 0.5804(2) 0.3640(4) 0.1065(13) Uani 0.60 1 d P A 1 F13 F 0.0422(5) 0.5471(3) 0.4277(9) 0.0868(18) Uani 0.36 1 d P A 2 F14 F 0.2323(5) 0.6350(3) 0.5045(9) 0.0868(18) Uani 0.36 1 d P A 2 F15 F 0.1200(6) 0.5935(3) 0.3414(4) 0.0871(15) Uani 0.40 1 d P A 2 F16 F 0.1503(6) 0.5876(4) 0.5931(4) 0.0871(15) Uani 0.40 1 d P A 2 F17 F 0.0567(4) 0.6420(2) 0.4517(5) 0.0717(16) Uani 0.56 1 d P A 2 F18 F 0.2197(5) 0.5406(3) 0.4887(5) 0.0717(16) Uani 0.66 1 d P A 2 O1 O 0.33922(13) 0.59501(7) -0.05787(14) 0.0254(4) Uani 1 1 d . . . O2 O 0.25862(14) 0.69239(8) 0.02054(15) 0.0303(4) Uani 1 1 d . . . O3 O 0.23823(16) 0.70121(9) 0.23505(17) 0.0392(5) Uani 1 1 d . . . H3A H 0.1777 0.6925 0.2303 0.059 Uiso 1 1 calc R . . N1 N 0.85538(16) 0.56528(9) 0.15593(18) 0.0284(5) Uani 1 1 d . . . N2 N 0.42302(16) 0.57290(9) 0.29486(17) 0.0261(5) Uani 1 1 d . . . C1 C 0.9355(2) 0.55790(13) 0.1088(2) 0.0347(6) Uani 1 1 d . . . H1A H 0.9983 0.5359 0.1634 0.042 Uiso 1 1 calc R . . H1B H 0.9606 0.5960 0.0966 0.042 Uiso 1 1 calc R . . C2 C 0.7924(2) 0.61225(11) 0.1290(2) 0.0321(6) Uani 1 1 d . . . H2 H 0.8035 0.6423 0.0859 0.039 Uiso 1 1 calc R . . C3 C 0.7119(2) 0.61748(11) 0.1628(2) 0.0295(6) Uani 1 1 d . . . H3 H 0.6693 0.6514 0.1450 0.035 Uiso 1 1 calc R . . C4 C 0.69295(19) 0.57292(10) 0.2234(2) 0.0235(5) Uani 1 1 d . . . C5 C 0.7607(2) 0.52529(12) 0.2504(2) 0.0288(6) Uani 1 1 d . . . H5 H 0.7510 0.4944 0.2927 0.035 Uiso 1 1 calc R . . C6 C 0.8409(2) 0.52253(12) 0.2168(2) 0.0330(6) Uani 1 1 d . . . H6 H 0.8869 0.4899 0.2368 0.040 Uiso 1 1 calc R . . C7 C 0.60121(18) 0.57515(10) 0.25305(19) 0.0231(5) Uani 1 1 d . . . C8 C 0.52187(19) 0.61698(11) 0.2087(2) 0.0248(5) Uani 1 1 d . . . H8 H 0.5287 0.6471 0.1631 0.030 Uiso 1 1 calc R . . C9 C 0.4336(2) 0.61521(11) 0.2303(2) 0.0270(5) Uani 1 1 d . . . H9 H 0.3798 0.6440 0.1994 0.032 Uiso 1 1 calc R . . C10 C 0.4992(2) 0.53265(12) 0.3410(2) 0.0300(6) Uani 1 1 d . . . H10 H 0.4911 0.5034 0.3874 0.036 Uiso 1 1 calc R . . C11 C 0.5885(2) 0.53304(11) 0.3222(2) 0.0280(6) Uani 1 1 d . . . H11 H 0.6423 0.5045 0.3565 0.034 Uiso 1 1 calc R . . C12 C 0.3201(2) 0.56774(13) 0.3056(2) 0.0317(6) Uani 1 1 d . . . H12A H 0.2918 0.6065 0.3087 0.038 Uiso 1 1 calc R . . H12B H 0.3329 0.5470 0.3768 0.038 Uiso 1 1 calc R . . C13 C 0.2403(2) 0.53512(12) 0.2033(2) 0.0284(6) Uani 1 1 d . . . C14 C 0.18268(19) 0.56420(11) 0.1012(2) 0.0275(5) Uani 1 1 d . . . H14 H 0.1849 0.6051 0.0994 0.033 Uiso 1 1 calc R . . C15 C 0.12208(19) 0.53394(11) 0.0022(2) 0.0276(6) Uani 1 1 d . . . H15 H 0.0829 0.5541 -0.0673 0.033 Uiso 1 1 calc R . . C16 C 0.11807(19) 0.47425(12) 0.0036(2) 0.0290(6) Uani 1 1 d . . . C17 C 0.1698(2) 0.44496(12) 0.1071(2) 0.0328(6) Uani 1 1 d . . . H17 H 0.1636 0.4043 0.1096 0.039 Uiso 0.75 1 calc PR B 2 C19A C 0.2739(12) 0.4387(7) 0.3103(14) 0.070(4) Uani 0.25 1 d P C 2 H19D H 0.3235 0.4103 0.3046 0.105 Uiso 0.25 1 calc PR C 2 H19E H 0.2145 0.4186 0.3164 0.105 Uiso 0.25 1 calc PR C 2 H19F H 0.3120 0.4626 0.3782 0.105 Uiso 0.25 1 calc PR C 2 N3A N 0.5252(15) 0.4032(8) 0.4370(15) 0.062(4) Uani 0.25 1 d P D 2 C29A C 0.5410(15) 0.3574(16) 0.448(3) 0.041(6) Uani 0.25 1 d P D 2 C30A C 0.566(3) 0.3012(16) 0.467(3) 0.105(14) Uani 0.25 1 d P D 2 H30D H 0.5024 0.2792 0.4565 0.158 Uiso 0.25 1 calc PR D 2 H30E H 0.6221 0.2961 0.5457 0.158 Uiso 0.25 1 calc PR D 2 H30F H 0.5932 0.2874 0.4137 0.158 Uiso 0.25 1 calc PR D 2 C18 C 0.2308(2) 0.47562(12) 0.2069(2) 0.0334(6) Uani 1 1 d . C . H18 H 0.2660 0.4558 0.2776 0.040 Uiso 0.75 1 calc PR E 1 N3 N 0.4667(4) 0.4069(3) 0.4299(5) 0.0490(12) Uani 0.75 1 d P F 1 C29 C 0.5004(5) 0.3608(6) 0.4392(9) 0.0409(19) Uani 0.75 1 d P F 1 C30 C 0.5449(9) 0.3014(5) 0.4546(7) 0.048(2) Uani 0.75 1 d P F 1 H30A H 0.5104 0.2772 0.4904 0.072 Uiso 0.75 1 calc PR F 1 H30B H 0.6224 0.3025 0.5035 0.072 Uiso 0.75 1 calc PR F 1 H30C H 0.5311 0.2852 0.3799 0.072 Uiso 0.75 1 calc PR F 1 C19 C 0.1558(8) 0.3833(4) 0.1217(9) 0.025(2) Uani 0.25 1 d P G 1 H19A H 0.2197 0.3685 0.1867 0.037 Uiso 0.25 1 calc PR G 1 H19B H 0.1455 0.3626 0.0522 0.037 Uiso 0.25 1 calc PR G 1 H19C H 0.0928 0.3778 0.1358 0.037 Uiso 0.25 1 calc PR G 1 C20 C 0.42803(19) 0.44039(11) 0.1112(2) 0.0254(5) Uani 1 1 d . . . H20 H 0.3888 0.4252 0.1489 0.031 Uiso 1 1 calc R . . C21 C 0.39653(18) 0.49113(10) 0.0542(2) 0.0222(5) Uani 1 1 d . . . H21 H 0.3355 0.5107 0.0518 0.027 Uiso 1 1 calc R . . C22 C 0.45472(18) 0.51485(10) -0.00169(19) 0.0200(5) Uani 1 1 d . . . C23 C 0.42584(18) 0.56836(10) -0.0613(2) 0.0218(5) Uani 1 1 d . . . C24 C 0.48243(19) 0.59037(11) -0.1159(2) 0.0253(5) Uani 1 1 d . . . H24 H 0.4617 0.6258 -0.1563 0.030 Uiso 1 1 calc R . . C25 C 0.3087(2) 0.64943(11) -0.1153(2) 0.0306(6) Uani 1 1 d . . . H25B H 0.2850 0.6441 -0.1982 0.037 Uiso 1 1 calc R . . H25A H 0.3709 0.6760 -0.0858 0.037 Uiso 1 1 calc R . . C26 C 0.2190(2) 0.67440(12) -0.0951(2) 0.0303(6) Uani 1 1 d . . . H26B H 0.1874 0.7077 -0.1465 0.036 Uiso 1 1 calc R . . H26A H 0.1621 0.6451 -0.1123 0.036 Uiso 1 1 calc R . . C27 C 0.1821(2) 0.72756(12) 0.0358(2) 0.0346(6) Uani 1 1 d . . . H27B H 0.1151 0.7055 0.0156 0.042 Uiso 1 1 calc R . . H27A H 0.1647 0.7615 -0.0152 0.042 Uiso 1 1 calc R . . C28 C 0.2268(2) 0.74693(12) 0.1575(2) 0.0378(7) Uani 1 1 d . . . H28B H 0.2979 0.7648 0.1794 0.045 Uiso 1 1 calc R . . H28A H 0.1790 0.7767 0.1643 0.045 Uiso 1 1 calc R . . N4 N 0.0165(2) 0.40602(14) 0.2668(2) 0.0601(8) Uani 1 1 d . . . C31 C 0.0693(2) 0.40158(13) 0.3613(3) 0.0413(7) Uani 1 1 d . . . C32 C 0.1363(3) 0.39740(17) 0.4828(3) 0.0581(9) Uani 1 1 d . . . H32A H 0.2118 0.3954 0.4975 0.087 Uiso 1 1 calc R . . H32B H 0.1174 0.3626 0.5124 0.087 Uiso 1 1 calc R . . H32C H 0.1252 0.4313 0.5209 0.087 Uiso 1 1 calc R . . N5 N 1.0128(2) 0.70968(14) 0.1933(3) 0.0618(8) Uani 1 1 d . . . C33 C 0.9588(3) 0.73095(17) 0.2260(3) 0.0554(9) Uani 1 1 d . . . C34 C 0.8884(4) 0.7577(2) 0.2680(4) 0.0866(14) Uani 1 1 d . . . H34A H 0.8159 0.7611 0.2053 0.130 Uiso 1 1 calc R . . H34B H 0.9156 0.7961 0.2979 0.130 Uiso 1 1 calc R . . H34C H 0.8862 0.7340 0.3289 0.130 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0457(5) 0.0356(4) 0.0467(5) 0.0140(4) 0.0132(4) -0.0012(4) F1 0.0735(14) 0.0665(14) 0.0977(17) 0.0454(12) 0.0578(14) 0.0251(11) F2 0.146(2) 0.0733(16) 0.0808(17) 0.0419(13) 0.0672(17) 0.0219(16) F3 0.169(3) 0.0397(12) 0.121(2) -0.0008(13) 0.090(2) -0.0037(15) F4 0.0913(17) 0.0479(12) 0.0934(17) -0.0100(12) 0.0442(14) -0.0103(11) F5 0.0439(12) 0.117(2) 0.0686(14) 0.0030(14) 0.0142(11) -0.0179(12) F6 0.0507(14) 0.138(2) 0.095(2) 0.0146(18) -0.0027(13) 0.0220(15) P2 0.0340(4) 0.0289(4) 0.0355(4) -0.0009(3) 0.0173(3) -0.0018(3) F7 0.132(6) 0.022(2) 0.150(6) -0.020(3) 0.124(5) -0.019(3) F8 0.132(6) 0.022(2) 0.150(6) -0.020(3) 0.124(5) -0.019(3) F9 0.0620(17) 0.0461(14) 0.0835(18) 0.0180(15) 0.0502(15) 0.0028(12) F10 0.0620(17) 0.0461(14) 0.0835(18) 0.0180(15) 0.0502(15) 0.0028(12) F11 0.087(2) 0.139(3) 0.0466(16) 0.0079(18) -0.0133(16) -0.055(2) F12 0.087(2) 0.139(3) 0.0466(16) 0.0079(18) -0.0133(16) -0.055(2) F13 0.048(3) 0.042(3) 0.161(6) -0.016(4) 0.037(4) -0.021(2) F14 0.048(3) 0.042(3) 0.161(6) -0.016(4) 0.037(4) -0.021(2) F15 0.101(4) 0.128(4) 0.033(2) 0.007(2) 0.031(2) 0.048(3) F16 0.101(4) 0.128(4) 0.033(2) 0.007(2) 0.031(2) 0.048(3) F17 0.0657(19) 0.064(3) 0.101(3) 0.039(2) 0.051(2) 0.0367(18) F18 0.0657(19) 0.064(3) 0.101(3) 0.039(2) 0.051(2) 0.0367(18) O1 0.0262(9) 0.0241(9) 0.0295(9) 0.0043(7) 0.0155(8) 0.0068(7) O2 0.0341(10) 0.0299(10) 0.0293(10) -0.0008(8) 0.0163(8) 0.0066(8) O3 0.0428(11) 0.0425(12) 0.0393(11) 0.0000(9) 0.0246(10) 0.0050(10) N1 0.0195(10) 0.0362(12) 0.0292(12) -0.0071(10) 0.0104(9) -0.0041(9) N2 0.0244(11) 0.0359(12) 0.0203(10) -0.0044(9) 0.0120(9) -0.0003(9) C1 0.0242(13) 0.0438(16) 0.0420(16) -0.0100(13) 0.0199(12) -0.0055(12) C2 0.0354(14) 0.0283(14) 0.0385(15) -0.0062(12) 0.0216(13) -0.0085(12) C3 0.0300(14) 0.0281(13) 0.0332(14) -0.0041(11) 0.0165(12) -0.0002(11) C4 0.0205(11) 0.0272(13) 0.0197(12) -0.0043(10) 0.0062(10) -0.0024(10) C5 0.0266(13) 0.0341(14) 0.0239(13) 0.0023(11) 0.0097(11) 0.0031(11) C6 0.0267(13) 0.0386(16) 0.0311(14) 0.0004(12) 0.0105(12) 0.0058(11) C7 0.0221(12) 0.0279(13) 0.0158(11) -0.0046(10) 0.0053(10) -0.0033(10) C8 0.0264(12) 0.0236(12) 0.0250(13) -0.0009(10) 0.0119(11) -0.0006(10) C9 0.0264(13) 0.0247(12) 0.0293(13) -0.0031(11) 0.0116(11) 0.0010(10) C10 0.0310(14) 0.0370(15) 0.0220(13) 0.0049(11) 0.0117(11) 0.0020(12) C11 0.0244(13) 0.0332(14) 0.0242(13) 0.0030(11) 0.0088(11) 0.0029(11) C12 0.0283(13) 0.0458(16) 0.0267(13) -0.0021(12) 0.0173(11) -0.0001(12) C13 0.0228(12) 0.0397(15) 0.0294(14) -0.0035(12) 0.0177(11) -0.0011(11) C14 0.0221(12) 0.0320(14) 0.0324(14) -0.0010(11) 0.0157(11) 0.0013(11) C15 0.0187(12) 0.0363(14) 0.0296(14) 0.0025(11) 0.0123(11) 0.0033(10) C16 0.0175(12) 0.0408(15) 0.0341(14) -0.0052(12) 0.0162(11) -0.0039(11) C17 0.0310(14) 0.0321(14) 0.0427(16) 0.0021(12) 0.0232(13) -0.0020(11) C19A 0.053(9) 0.073(11) 0.077(11) 0.010(9) 0.022(8) 0.006(8) N3A 0.091(13) 0.037(8) 0.050(8) 0.002(6) 0.024(10) 0.007(11) C29A 0.036(12) 0.042(12) 0.036(9) -0.005(7) 0.007(11) -0.012(13) C30A 0.035(13) 0.051(16) 0.19(3) -0.058(17) 0.009(13) -0.014(10) C18 0.0288(14) 0.0445(16) 0.0325(15) 0.0079(13) 0.0188(12) 0.0011(12) N3 0.061(3) 0.044(3) 0.039(2) 0.0026(18) 0.018(3) 0.003(3) C29 0.044(4) 0.046(4) 0.028(3) -0.006(2) 0.012(4) -0.009(5) C30 0.051(5) 0.049(5) 0.047(3) -0.005(3) 0.024(3) 0.000(3) C19 0.033(5) 0.008(4) 0.043(6) 0.000(4) 0.026(5) 0.001(4) C20 0.0262(12) 0.0276(13) 0.0288(13) -0.0013(11) 0.0178(11) -0.0033(10) C21 0.0205(11) 0.0252(12) 0.0220(12) -0.0034(10) 0.0103(10) 0.0005(10) C22 0.0198(11) 0.0214(11) 0.0189(11) -0.0034(9) 0.0087(9) -0.0011(9) C23 0.0194(11) 0.0231(12) 0.0224(12) -0.0031(10) 0.0088(10) -0.0001(9) C24 0.0285(13) 0.0228(12) 0.0270(13) 0.0032(10) 0.0145(11) 0.0024(10) C25 0.0388(15) 0.0287(14) 0.0274(14) 0.0066(11) 0.0176(12) 0.0088(12) C26 0.0350(14) 0.0319(14) 0.0235(13) 0.0033(11) 0.0125(11) 0.0105(11) C27 0.0417(16) 0.0281(14) 0.0371(15) -0.0008(12) 0.0201(13) 0.0089(12) C28 0.0482(17) 0.0319(15) 0.0411(16) -0.0038(13) 0.0267(14) 0.0016(13) N4 0.0506(17) 0.076(2) 0.0415(17) 0.0034(15) 0.0092(14) 0.0029(15) C31 0.0355(15) 0.0451(18) 0.0373(17) -0.0021(14) 0.0107(14) 0.0047(13) C32 0.0483(19) 0.077(3) 0.0376(18) 0.0018(17) 0.0091(15) 0.0104(18) N5 0.0422(17) 0.070(2) 0.072(2) 0.0083(17) 0.0237(16) -0.0029(15) C33 0.0381(18) 0.066(2) 0.057(2) -0.0028(19) 0.0163(17) -0.0146(17) C34 0.071(3) 0.100(4) 0.108(4) -0.033(3) 0.057(3) -0.022(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 F6 1.572(2) . ? P1 F3 1.575(2) . ? P1 F4 1.580(2) . ? P1 F1 1.580(2) . ? P1 F2 1.586(2) . ? P1 F5 1.588(2) . ? P2 F12 1.477(4) . ? P2 F16 1.488(5) . ? P2 F7 1.537(5) . ? P2 F14 1.551(6) . ? P2 F18 1.556(6) . ? P2 F10 1.558(3) . ? P2 F13 1.587(5) . ? P2 F17 1.599(5) . ? P2 F8 1.605(12) . ? P2 F9 1.609(3) . ? P2 F15 1.639(5) . ? P2 F11 1.642(4) . ? O1 C23 1.371(3) . ? O1 C25 1.435(3) . ? O2 C26 1.422(3) . ? O2 C27 1.423(3) . ? O3 C28 1.426(3) . ? O3 H3A 0.8400 . ? N1 C6 1.341(3) . ? N1 C2 1.344(3) . ? N1 C1 1.500(3) . ? N2 C10 1.339(3) . ? N2 C9 1.345(3) . ? N2 C12 1.502(3) . ? C1 C16 1.516(4) 3_665 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.378(4) . ? C2 H2 0.9500 . ? C3 C4 1.396(4) . ? C3 H3 0.9500 . ? C4 C5 1.393(3) . ? C4 C7 1.488(3) . ? C5 C6 1.368(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.389(3) . ? C7 C11 1.394(3) . ? C8 C9 1.375(3) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.368(4) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.509(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.389(4) . ? C13 C18 1.391(4) . ? C14 C15 1.382(4) . ? C14 H14 0.9500 . ? C15 C16 1.388(4) . ? C15 H15 0.9500 . ? C16 C17 1.395(4) . ? C16 C1 1.516(4) 3_665 ? C17 C18 1.395(4) . ? C17 C19 1.468(9) . ? C17 H17 0.9500 . ? C19A C18 1.484(16) . ? C19A H19D 0.9800 . ? C19A H19E 0.9800 . ? C19A H19F 0.9800 . ? N3A C29A 1.08(4) . ? C29A C30A 1.35(6) . ? C30A H30D 0.9800 . ? C30A H30E 0.9800 . ? C30A H30F 0.9800 . ? C18 H18 0.9500 . ? N3 C29 1.152(14) . ? C29 C30 1.489(16) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.359(3) . ? C20 C24 1.412(3) 3_665 ? C20 H20 0.9500 . ? C21 C22 1.418(3) . ? C21 H21 0.9500 . ? C22 C22 1.418(4) 3_665 ? C22 C23 1.426(3) . ? C23 C24 1.373(3) . ? C24 C20 1.412(3) 3_665 ? C24 H24 0.9500 . ? C25 C26 1.500(4) . ? C25 H25B 0.9900 . ? C25 H25A 0.9900 . ? C26 H26B 0.9900 . ? C26 H26A 0.9900 . ? C27 C28 1.497(4) . ? C27 H27B 0.9900 . ? C27 H27A 0.9900 . ? C28 H28B 0.9900 . ? C28 H28A 0.9900 . ? N4 C31 1.127(4) . ? C31 C32 1.443(4) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? N5 C33 1.128(5) . ? C33 C34 1.455(6) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? 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 F6 P1 F3 89.57(18) . . ? F6 P1 F4 92.06(15) . . ? F3 P1 F4 178.36(16) . . ? F6 P1 F1 90.07(15) . . ? F3 P1 F1 89.46(14) . . ? F4 P1 F1 90.78(13) . . ? F6 P1 F2 90.64(16) . . ? F3 P1 F2 89.64(14) . . ? F4 P1 F2 90.09(14) . . ? F1 P1 F2 178.85(16) . . ? F6 P1 F5 179.86(18) . . ? F3 P1 F5 90.54(16) . . ? F4 P1 F5 87.84(14) . . ? F1 P1 F5 89.84(12) . . ? F2 P1 F5 89.45(15) . . ? F12 P2 F16 130.2(4) . . ? F12 P2 F7 98.4(4) . . ? F16 P2 F7 62.1(3) . . ? F12 P2 F14 128.6(4) . . ? F16 P2 F14 94.9(5) . . ? F7 P2 F14 80.3(4) . . ? F12 P2 F18 105.4(4) . . ? F16 P2 F18 96.3(3) . . ? F7 P2 F18 155.1(4) . . ? F14 P2 F18 90.2(4) . . ? F12 P2 F10 94.0(3) . . ? F16 P2 F10 129.2(4) . . ? F7 P2 F10 91.7(2) . . ? F18 P2 F10 93.7(3) . . ? F16 P2 F13 92.4(5) . . ? F7 P2 F13 101.7(4) . . ? F14 P2 F13 172.5(5) . . ? F18 P2 F13 90.7(4) . . ? F10 P2 F13 137.1(4) . . ? F12 P2 F17 71.5(3) . . ? F16 P2 F17 87.6(3) . . ? F14 P2 F17 90.1(3) . . ? F18 P2 F17 176.1(3) . . ? F10 P2 F17 84.3(2) . . ? F13 P2 F17 88.5(3) . . ? F12 P2 F8 91.7(6) . . ? F16 P2 F8 108.9(6) . . ? F7 P2 F8 169.5(5) . . ? F14 P2 F8 95.8(5) . . ? F10 P2 F8 90.6(4) . . ? F13 P2 F8 83.4(5) . . ? F17 P2 F8 161.9(6) . . ? F12 P2 F9 89.0(2) . . ? F7 P2 F9 88.8(2) . . ? F14 P2 F9 141.8(4) . . ? F18 P2 F9 84.7(3) . . ? F10 P2 F9 176.9(2) . . ? F17 P2 F9 97.5(2) . . ? F8 P2 F9 88.4(4) . . ? F16 P2 F15 175.9(4) . . ? F7 P2 F15 116.2(4) . . ? F14 P2 F15 88.5(5) . . ? F18 P2 F15 86.1(3) . . ? F10 P2 F15 53.7(3) . . ? F13 P2 F15 84.2(5) . . ? F17 P2 F15 90.0(3) . . ? F8 P2 F15 73.2(5) . . ? F9 P2 F15 128.6(3) . . ? F12 P2 F11 176.4(3) . . ? F16 P2 F11 46.9(3) . . ? F7 P2 F11 82.0(4) . . ? F14 P2 F11 55.0(4) . . ? F18 P2 F11 73.8(3) . . ? F10 P2 F11 89.6(2) . . ? F13 P2 F11 132.2(4) . . ? F17 P2 F11 109.5(3) . . ? F8 P2 F11 87.8(6) . . ? F9 P2 F11 87.4(2) . . ? F15 P2 F11 137.2(3) . . ? C23 O1 C25 116.19(18) . . ? C26 O2 C27 110.79(19) . . ? C28 O3 H3A 109.5 . . ? C6 N1 C2 120.3(2) . . ? C6 N1 C1 119.4(2) . . ? C2 N1 C1 120.0(2) . . ? C10 N2 C9 120.6(2) . . ? C10 N2 C12 119.9(2) . . ? C9 N2 C12 119.3(2) . . ? N1 C1 C16 108.5(2) . 3_665 ? N1 C1 H1A 110.0 . . ? C16 C1 H1A 110.0 3_665 . ? N1 C1 H1B 110.0 . . ? C16 C1 H1B 110.0 3_665 . ? H1A C1 H1B 108.4 . . ? N1 C2 C3 121.0(2) . . ? N1 C2 H2 119.5 . . ? C3 C2 H2 119.5 . . ? C2 C3 C4 119.9(2) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 117.2(2) . . ? C5 C4 C7 121.5(2) . . ? C3 C4 C7 121.3(2) . . ? C6 C5 C4 120.7(2) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? N1 C6 C5 120.8(2) . . ? N1 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C8 C7 C11 117.1(2) . . ? C8 C7 C4 121.9(2) . . ? C11 C7 C4 120.8(2) . . ? C9 C8 C7 120.6(2) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? N2 C9 C8 120.3(2) . . ? N2 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? N2 C10 C11 120.9(2) . . ? N2 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C10 C11 C7 120.4(2) . . ? C10 C11 H11 119.8 . . ? C7 C11 H11 119.8 . . ? N2 C12 C13 108.28(19) . . ? N2 C12 H12A 110.0 . . ? C13 C12 H12A 110.0 . . ? N2 C12 H12B 110.0 . . ? C13 C12 H12B 110.0 . . ? H12A C12 H12B 108.4 . . ? C14 C13 C18 119.5(2) . . ? C14 C13 C12 119.4(2) . . ? C18 C13 C12 120.8(2) . . ? C15 C14 C13 120.3(2) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 120.5(2) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C17 119.6(2) . . ? C15 C16 C1 119.0(2) . 3_665 ? C17 C16 C1 121.3(2) . 3_665 ? C18 C17 C16 119.7(3) . . ? C18 C17 C19 115.9(5) . . ? C16 C17 C19 124.0(5) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C18 C19A H19D 109.5 . . ? C18 C19A H19E 109.5 . . ? H19D C19A H19E 109.5 . . ? C18 C19A H19F 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? N3A C29A C30A 176(3) . . ? C29A C30A H30D 109.5 . . ? C29A C30A H30E 109.5 . . ? H30D C30A H30E 109.5 . . ? C29A C30A H30F 109.5 . . ? H30D C30A H30F 109.5 . . ? H30E C30A H30F 109.5 . . ? C13 C18 C17 120.2(3) . . ? C13 C18 C19A 126.8(7) . . ? C17 C18 C19A 112.8(7) . . ? C13 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? N3 C29 C30 178.4(10) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C24 121.8(2) . 3_665 ? C21 C20 H20 119.1 . . ? C24 C20 H20 119.1 3_665 . ? C20 C21 C22 120.0(2) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C22 C22 C21 119.7(3) 3_665 . ? C22 C22 C23 118.2(3) 3_665 . ? C21 C22 C23 122.2(2) . . ? O1 C23 C24 124.1(2) . . ? O1 C23 C22 114.5(2) . . ? C24 C23 C22 121.4(2) . . ? C23 C24 C20 119.0(2) . 3_665 ? C23 C24 H24 120.5 . . ? C20 C24 H24 120.5 3_665 . ? O1 C25 C26 109.0(2) . . ? O1 C25 H25B 109.9 . . ? C26 C25 H25B 109.9 . . ? O1 C25 H25A 109.9 . . ? C26 C25 H25A 109.9 . . ? H25B C25 H25A 108.3 . . ? O2 C26 C25 109.8(2) . . ? O2 C26 H26B 109.7 . . ? C25 C26 H26B 109.7 . . ? O2 C26 H26A 109.7 . . ? C25 C26 H26A 109.7 . . ? H26B C26 H26A 108.2 . . ? O2 C27 C28 109.6(2) . . ? O2 C27 H27B 109.7 . . ? C28 C27 H27B 109.7 . . ? O2 C27 H27A 109.7 . . ? C28 C27 H27A 109.7 . . ? H27B C27 H27A 108.2 . . ? O3 C28 C27 113.1(2) . . ? O3 C28 H28B 109.0 . . ? C27 C28 H28B 109.0 . . ? O3 C28 H28A 109.0 . . ? C27 C28 H28A 109.0 . . ? H28B C28 H28A 107.8 . . ? N4 C31 C32 178.6(4) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N5 C33 C34 179.3(4) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 N1 C1 C16 84.1(3) . . . 3_665 ? C2 N1 C1 C16 -90.2(3) . . . 3_665 ? C6 N1 C2 C3 -0.1(4) . . . . ? C1 N1 C2 C3 174.1(2) . . . . ? N1 C2 C3 C4 -1.8(4) . . . . ? C2 C3 C4 C5 2.3(4) . . . . ? C2 C3 C4 C7 -175.0(2) . . . . ? C3 C4 C5 C6 -1.0(4) . . . . ? C7 C4 C5 C6 176.3(2) . . . . ? C2 N1 C6 C5 1.4(4) . . . . ? C1 N1 C6 C5 -172.9(2) . . . . ? C4 C5 C6 N1 -0.8(4) . . . . ? C5 C4 C7 C8 -167.8(2) . . . . ? C3 C4 C7 C8 9.3(3) . . . . ? C5 C4 C7 C11 8.6(3) . . . . ? C3 C4 C7 C11 -174.2(2) . . . . ? C11 C7 C8 C9 -1.9(3) . . . . ? C4 C7 C8 C9 174.7(2) . . . . ? C10 N2 C9 C8 1.4(4) . . . . ? C12 N2 C9 C8 -172.7(2) . . . . ? C7 C8 C9 N2 0.1(4) . . . . ? C9 N2 C10 C11 -1.0(4) . . . . ? C12 N2 C10 C11 173.0(2) . . . . ? N2 C10 C11 C7 -0.9(4) . . . . ? C8 C7 C11 C10 2.3(4) . . . . ? C4 C7 C11 C10 -174.4(2) . . . . ? C10 N2 C12 C13 -91.1(3) . . . . ? C9 N2 C12 C13 83.0(3) . . . . ? N2 C12 C13 C14 -82.1(3) . . . . ? N2 C12 C13 C18 92.2(3) . . . . ? C18 C13 C14 C15 -4.4(4) . . . . ? C12 C13 C14 C15 169.9(2) . . . . ? C13 C14 C15 C16 0.0(4) . . . . ? C14 C15 C16 C17 4.3(4) . . . . ? C14 C15 C16 C1 -171.1(2) . . . 3_665 ? C15 C16 C17 C18 -4.2(4) . . . . ? C1 C16 C17 C18 171.1(2) 3_665 . . . ? C15 C16 C17 C19 169.1(5) . . . . ? C1 C16 C17 C19 -15.6(6) 3_665 . . . ? C14 C13 C18 C17 4.5(4) . . . . ? C12 C13 C18 C17 -169.7(2) . . . . ? C14 C13 C18 C19A -171.0(8) . . . . ? C12 C13 C18 C19A 14.8(9) . . . . ? C16 C17 C18 C13 -0.2(4) . . . . ? C19 C17 C18 C13 -174.0(5) . . . . ? C16 C17 C18 C19A 175.9(7) . . . . ? C19 C17 C18 C19A 2.1(8) . . . . ? C24 C20 C21 C22 -0.6(4) 3_665 . . . ? C20 C21 C22 C22 0.4(4) . . . 3_665 ? C20 C21 C22 C23 -179.1(2) . . . . ? C25 O1 C23 C24 -0.4(3) . . . . ? C25 O1 C23 C22 179.0(2) . . . . ? C22 C22 C23 O1 -178.3(2) 3_665 . . . ? C21 C22 C23 O1 1.2(3) . . . . ? C22 C22 C23 C24 1.2(4) 3_665 . . . ? C21 C22 C23 C24 -179.3(2) . . . . ? O1 C23 C24 C20 178.5(2) . . . 3_665 ? C22 C23 C24 C20 -1.0(4) . . . 3_665 ? C23 O1 C25 C26 -175.5(2) . . . . ? C27 O2 C26 C25 166.9(2) . . . . ? O1 C25 C26 O2 70.8(3) . . . . ? C26 O2 C27 C28 -178.7(2) . . . . ? O2 C27 C28 O3 -68.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.766 _refine_diff_density_min -0.516 _refine_diff_density_rms 0.060 data_stod2604smnew _database_code_depnum_ccdc_archive 'CCDC 720653' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H34 N4, C6 H4 S4, 4(F6 P), 1.8(C2 H3 N)' _chemical_formula_sum 'C46.60 H43.40 F24 N5.80 P4 S4' _chemical_formula_weight 1392.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.8498(8) _cell_length_b 19.3989(14) _cell_length_c 13.8729(10) _cell_angle_alpha 90.00 _cell_angle_beta 106.5760(10) _cell_angle_gamma 90.00 _cell_volume 2798.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4913 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 27.10 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.653 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1407.2 _exptl_absorpt_coefficient_mu 0.406 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8012 _exptl_absorpt_correction_T_max 0.9605 _exptl_absorpt_process_details 'Sadabs (Bruker)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17729 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 28.32 _reflns_number_total 6723 _reflns_number_gt 4363 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0743P)^2^+1.5622P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6723 _refine_ls_number_parameters 436 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0895 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1562 _refine_ls_wR_factor_gt 0.1371 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.51649(8) 0.40256(4) 0.81579(7) 0.0549(2) Uani 1 1 d . . . F1 F 0.63469(17) 0.35369(10) 0.81689(15) 0.0659(5) Uani 1 1 d . . . F2 F 0.3981(2) 0.45091(11) 0.8133(2) 0.0993(8) Uani 1 1 d . . 1 F3 F 0.42955(18) 0.36073(10) 0.72108(16) 0.0716(6) Uani 1 1 d . . . F4 F 0.6046(2) 0.44376(10) 0.90997(16) 0.0741(6) Uani 1 1 d . . . F5 F 0.5602(2) 0.45387(11) 0.74176(16) 0.0817(6) Uani 1 1 d . . . F6 F 0.4744(2) 0.35073(11) 0.88897(18) 0.0865(7) Uani 1 1 d . . . P2 P 0.01554(8) 0.20616(4) 0.92930(6) 0.0511(2) Uani 1 1 d . . . F7 F 0.0951(4) 0.1868(3) 1.0430(3) 0.0942(13) Uani 0.58 1 d P A 1 F8 F -0.0634(4) 0.2272(2) 0.8225(3) 0.0781(11) Uani 0.58 1 d P A 1 F9 F 0.1097(4) 0.1571(2) 0.8948(4) 0.0829(13) Uani 0.58 1 d P A 1 F10 F -0.0655(4) 0.2577(3) 0.9721(4) 0.0916(16) Uani 0.58 1 d P A 1 F11 F 0.1189(4) 0.26773(19) 0.9377(5) 0.0914(14) Uani 0.58 1 d P A 1 F12 F -0.0787(4) 0.1461(2) 0.9308(5) 0.0876(13) Uani 0.58 1 d P A 1 F13 F -0.0661(6) 0.1848(4) 1.0016(4) 0.0830(16) Uani 0.42 1 d P A 2 F14 F 0.0854(5) 0.2287(4) 0.8494(4) 0.099(2) Uani 0.42 1 d P A 2 F15 F -0.0820(7) 0.1593(6) 0.8481(7) 0.140(3) Uani 0.42 1 d P A 2 F16 F 0.1042(8) 0.2528(6) 1.0077(8) 0.140(3) Uani 0.42 1 d P A 2 F17 F -0.0860(7) 0.2674(4) 0.8989(11) 0.145(3) Uani 0.42 1 d P A 2 F18 F 0.1073(7) 0.1469(4) 0.9643(12) 0.145(3) Uani 0.42 1 d P A 2 S1 S 0.60193(8) 0.02222(4) -0.11119(5) 0.0510(2) Uani 1 1 d . . . S2 S 0.69293(9) -0.01238(4) 0.10489(6) 0.0560(2) Uani 1 1 d . . . N1 N 0.5302(3) 0.20475(11) -0.18494(17) 0.0475(6) Uani 1 1 d . . . N2 N 0.4874(3) 0.11577(11) 0.29359(16) 0.0447(6) Uani 1 1 d . . . C1 C 0.5384(4) 0.20799(15) -0.2909(2) 0.0601(9) Uani 1 1 d . . . H1A H 0.6191 0.2310 -0.2929 0.072 Uiso 1 1 calc R . . H1B H 0.4649 0.2344 -0.3337 0.072 Uiso 1 1 calc R . . C2 C 0.6369(3) 0.20044(14) -0.1094(2) 0.0508(7) Uani 1 1 d . . . H2 H 0.7177 0.2060 -0.1223 0.061 Uiso 1 1 calc R . . C3 C 0.6330(3) 0.18798(14) -0.0121(2) 0.0447(6) Uani 1 1 d . . . H3 H 0.7107 0.1852 0.0411 0.054 Uiso 1 1 calc R . . C4 C 0.5155(3) 0.17954(12) 0.00791(19) 0.0374(6) Uani 1 1 d . . . C5 C 0.4055(3) 0.18692(14) -0.0732(2) 0.0480(7) Uani 1 1 d . . . H5 H 0.3229 0.1834 -0.0627 0.058 Uiso 1 1 calc R . . C6 C 0.4155(3) 0.19928(15) -0.1684(2) 0.0544(8) Uani 1 1 d . . . H6 H 0.3397 0.2040 -0.2229 0.065 Uiso 1 1 calc R . . C7 C 0.5071(3) 0.16057(12) 0.10952(19) 0.0370(6) Uani 1 1 d . . . C8 C 0.6151(3) 0.14437(14) 0.1871(2) 0.0457(6) Uani 1 1 d . . . H8 H 0.6981 0.1485 0.1776 0.055 Uiso 1 1 calc R . . C9 C 0.6026(3) 0.12230(16) 0.2780(2) 0.0531(7) Uani 1 1 d . . . H9 H 0.6776 0.1115 0.3308 0.064 Uiso 1 1 calc R . . C10 C 0.3817(3) 0.13274(14) 0.2217(2) 0.0502(7) Uani 1 1 d . . . H10 H 0.3002 0.1288 0.2340 0.060 Uiso 1 1 calc R . . C11 C 0.3889(3) 0.15589(14) 0.1298(2) 0.0458(7) Uani 1 1 d . . . H11 H 0.3125 0.1688 0.0797 0.055 Uiso 1 1 calc R . . C12 C 0.4754(3) 0.08286(15) 0.3880(2) 0.0539(8) Uani 1 1 d . . . H12A H 0.3956 0.0987 0.4022 0.065 Uiso 1 1 calc R . . H12B H 0.5495 0.0960 0.4454 0.065 Uiso 1 1 calc R . . C13 C 0.4719(3) 0.00520(14) 0.37438(19) 0.0471(7) Uani 1 1 d . . . C14 C 0.3555(3) -0.02849(15) 0.3380(2) 0.0508(7) Uani 1 1 d . C . H14 H 0.2776 -0.0037 0.3291 0.061 Uiso 1 1 calc R . . C15 C 0.3514(3) -0.09807(15) 0.3145(2) 0.0537(7) Uani 1 1 d . . . H15 H 0.2710 -0.1206 0.2886 0.064 Uiso 0.90 1 calc PR B 1 C19B C 0.225(4) -0.124(2) 0.310(3) 0.081(3) Uani 0.10 1 d P C 2 H19G H 0.2044 -0.1134 0.3726 0.122 Uiso 0.10 1 calc PR C 2 H19H H 0.2232 -0.1745 0.3005 0.122 Uiso 0.10 1 calc PR C 2 H19I H 0.1606 -0.1030 0.2532 0.122 Uiso 0.10 1 calc PR C 2 C16 C 0.4644(3) -0.13440(14) 0.3289(2) 0.0500(7) Uani 1 1 d . . . C17 C 0.5812(3) -0.10216(16) 0.3707(2) 0.0529(7) Uani 1 1 d . . . H17 H 0.6588 -0.1278 0.3841 0.063 Uiso 0.90 1 calc PR C 1 C19A C 0.715(4) -0.139(2) 0.386(3) 0.081(3) Uani 0.10 1 d P C 2 H19D H 0.7836 -0.1111 0.4301 0.122 Uiso 0.10 1 calc PR C 2 H19E H 0.7320 -0.1454 0.3211 0.122 Uiso 0.10 1 calc PR C 2 H19F H 0.7135 -0.1845 0.4177 0.122 Uiso 0.10 1 calc PR C 2 C18 C 0.5850(3) -0.03222(15) 0.3932(2) 0.0492(7) Uani 1 1 d . C . H18 H 0.6653 -0.0101 0.4214 0.059 Uiso 0.70 1 calc PR D 1 C19 C 0.7014(12) -0.0022(8) 0.4270(11) 0.081(3) Uani 0.30 1 d P C 2 H19A H 0.6941 0.0397 0.4643 0.122 Uiso 0.30 1 calc PR C 2 H19B H 0.7335 0.0096 0.3699 0.122 Uiso 0.30 1 calc PR C 2 H19C H 0.7614 -0.0343 0.4715 0.122 Uiso 0.30 1 calc PR C 2 C20 C 0.7657(4) 0.01862(17) -0.0541(3) 0.0653(9) Uani 1 1 d . E . H20 H 0.8250 0.0274 -0.0916 0.078 Uiso 1 1 calc R E . C21 C 0.8065(4) 0.00355(19) 0.0417(3) 0.0667(9) Uani 1 1 d . E . H21 H 0.8959 0.0014 0.0757 0.080 Uiso 1 1 calc R E . C22 C 0.5609(3) 0.00196(13) -0.0011(2) 0.0455(7) Uani 1 1 d . . . N3 N 1.1514(4) 0.18931(17) 0.6439(2) 0.0636(8) Uani 0.90 1 d P F 1 C23 C 1.0657(5) 0.15432(19) 0.6298(3) 0.0623(10) Uani 0.90 1 d P F 1 C24 C 0.9544(6) 0.1106(2) 0.6109(4) 0.1015(18) Uani 0.90 1 d P F 1 H24A H 0.9577 0.0761 0.5601 0.152 Uiso 0.90 1 calc PR F 1 H24B H 0.8765 0.1386 0.5864 0.152 Uiso 0.90 1 calc PR F 1 H24C H 0.9531 0.0873 0.6733 0.152 Uiso 0.90 1 calc PR F 1 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 P1 0.0549(5) 0.0361(4) 0.0772(6) 0.0018(4) 0.0245(4) -0.0002(3) F1 0.0566(11) 0.0578(11) 0.0859(14) 0.0035(10) 0.0244(10) 0.0091(9) F2 0.0734(14) 0.0615(13) 0.162(2) -0.0252(15) 0.0326(15) 0.0173(11) F3 0.0578(11) 0.0585(12) 0.0945(15) -0.0142(10) 0.0155(10) -0.0050(9) F4 0.0880(14) 0.0543(11) 0.0780(13) -0.0083(10) 0.0204(11) -0.0081(10) F5 0.0923(15) 0.0649(13) 0.0806(14) 0.0235(11) 0.0130(12) -0.0174(11) F6 0.1191(19) 0.0592(13) 0.1058(18) -0.0011(11) 0.0718(16) -0.0168(12) P2 0.0568(5) 0.0368(4) 0.0606(5) 0.0116(3) 0.0181(4) 0.0080(3) F7 0.073(3) 0.106(4) 0.092(3) 0.023(3) 0.005(2) 0.027(3) F8 0.101(3) 0.069(2) 0.054(2) 0.0210(18) 0.0036(19) 0.014(2) F9 0.073(3) 0.058(3) 0.125(4) -0.011(2) 0.040(3) 0.013(2) F10 0.077(3) 0.081(3) 0.100(3) -0.038(3) -0.002(2) 0.028(2) F11 0.066(2) 0.0442(19) 0.156(5) 0.019(3) 0.018(3) -0.0018(17) F12 0.071(2) 0.051(2) 0.135(4) 0.039(3) 0.020(3) -0.0067(18) F13 0.098(4) 0.094(4) 0.069(3) 0.012(3) 0.043(3) -0.004(3) F14 0.070(3) 0.169(7) 0.069(3) 0.045(4) 0.038(3) 0.000(4) F15 0.111(4) 0.194(7) 0.132(5) -0.111(5) 0.061(4) -0.077(4) F16 0.111(4) 0.194(7) 0.132(5) -0.111(5) 0.061(4) -0.077(4) F17 0.077(3) 0.076(3) 0.294(10) 0.096(6) 0.073(5) 0.031(3) F18 0.077(3) 0.076(3) 0.294(10) 0.096(6) 0.073(5) 0.031(3) S1 0.0794(5) 0.0341(3) 0.0431(4) -0.0019(3) 0.0234(4) -0.0014(3) S2 0.0733(5) 0.0476(4) 0.0436(4) -0.0015(3) 0.0110(4) 0.0020(4) N1 0.0783(18) 0.0276(11) 0.0424(13) 0.0017(9) 0.0263(13) 0.0002(11) N2 0.0729(17) 0.0302(11) 0.0373(12) -0.0048(9) 0.0260(12) 0.0001(11) C1 0.109(3) 0.0367(15) 0.0433(16) 0.0052(12) 0.0364(18) 0.0049(16) C2 0.070(2) 0.0380(15) 0.0538(17) -0.0076(13) 0.0334(16) -0.0105(14) C3 0.0559(17) 0.0399(14) 0.0418(14) -0.0090(11) 0.0197(13) -0.0083(12) C4 0.0539(16) 0.0203(10) 0.0413(14) -0.0029(10) 0.0191(12) -0.0011(10) C5 0.0550(17) 0.0430(15) 0.0484(16) 0.0012(12) 0.0186(14) 0.0044(13) C6 0.076(2) 0.0450(16) 0.0401(16) 0.0049(12) 0.0125(15) 0.0111(15) C7 0.0531(16) 0.0222(11) 0.0384(13) -0.0052(9) 0.0176(12) -0.0012(10) C8 0.0492(16) 0.0442(15) 0.0435(15) 0.0001(12) 0.0130(13) -0.0083(12) C9 0.068(2) 0.0492(17) 0.0388(15) -0.0033(12) 0.0101(14) -0.0099(15) C10 0.069(2) 0.0365(14) 0.0573(18) 0.0025(12) 0.0368(16) 0.0114(14) C11 0.0548(17) 0.0385(14) 0.0484(16) 0.0055(12) 0.0215(13) 0.0108(12) C12 0.092(2) 0.0378(15) 0.0411(15) -0.0018(12) 0.0332(16) 0.0025(15) C13 0.079(2) 0.0380(14) 0.0308(13) 0.0003(11) 0.0262(13) 0.0054(14) C14 0.067(2) 0.0459(16) 0.0466(16) 0.0048(13) 0.0283(15) 0.0079(14) C15 0.078(2) 0.0403(15) 0.0502(17) 0.0038(13) 0.0296(15) -0.0029(15) C19B 0.071(7) 0.091(9) 0.075(8) -0.007(6) 0.012(6) 0.009(7) C16 0.088(2) 0.0353(14) 0.0335(14) 0.0063(11) 0.0285(15) 0.0062(15) C17 0.076(2) 0.0478(17) 0.0378(15) 0.0025(12) 0.0209(14) 0.0133(15) C19A 0.071(7) 0.091(9) 0.075(8) -0.007(6) 0.012(6) 0.009(7) C18 0.069(2) 0.0463(16) 0.0349(14) -0.0030(12) 0.0187(13) 0.0012(14) C19 0.071(7) 0.091(9) 0.075(8) -0.007(6) 0.012(6) 0.009(7) C20 0.079(2) 0.0551(19) 0.066(2) 0.0041(16) 0.0288(18) 0.0005(17) C21 0.066(2) 0.063(2) 0.070(2) 0.0006(17) 0.0176(18) 0.0007(17) C22 0.0726(18) 0.0271(12) 0.0352(13) -0.0014(10) 0.0129(14) -0.0015(13) N3 0.080(2) 0.0495(18) 0.0577(18) 0.0077(14) 0.0141(17) 0.0119(17) C23 0.090(3) 0.0390(19) 0.065(2) 0.0055(16) 0.034(2) 0.009(2) C24 0.142(5) 0.064(3) 0.128(4) -0.014(3) 0.085(4) -0.037(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 F2 1.583(2) . ? P1 F6 1.586(2) . ? P1 F1 1.5914(19) . ? P1 F4 1.596(2) . ? P1 F5 1.596(2) . ? P1 F3 1.602(2) . ? P2 F18 1.508(6) . ? P2 F16 1.527(6) . ? P2 F8 1.539(3) . ? P2 F12 1.553(4) . ? P2 F10 1.557(4) . ? P2 F9 1.568(4) . ? P2 F13 1.571(5) . ? P2 F14 1.573(5) . ? P2 F15 1.592(6) . ? P2 F17 1.593(6) . ? P2 F7 1.612(4) . ? P2 F11 1.619(4) . ? S1 C20 1.728(4) . ? S1 C22 1.753(3) . ? S2 C21 1.731(4) . ? S2 C22 1.757(3) . ? N1 C2 1.324(4) . ? N1 C6 1.333(4) . ? N1 C1 1.500(4) . ? N2 C10 1.328(4) . ? N2 C9 1.334(4) . ? N2 C12 1.496(3) . ? C1 C16 1.519(4) 3_655 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.385(4) . ? C2 H2 0.9500 . ? C3 C4 1.390(4) . ? C3 H3 0.9500 . ? C4 C5 1.394(4) . ? C4 C7 1.485(3) . ? C5 C6 1.376(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.383(4) . ? C7 C11 1.392(4) . ? C8 C9 1.375(4) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.375(4) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.517(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.383(4) . ? C13 C18 1.385(4) . ? C14 C15 1.386(4) . ? C14 H14 0.9500 . ? C15 C16 1.379(4) . ? C15 C19B 1.45(4) . ? C15 H15 0.9500 . ? C19B H19G 0.9800 . ? C19B H19H 0.9800 . ? C19B H19I 0.9800 . ? C16 C17 1.383(5) . ? C16 C1 1.519(4) 3_655 ? C17 C18 1.390(4) . ? C17 C19A 1.58(4) . ? C17 H17 0.9500 . ? C19A H19D 0.9800 . ? C19A H19E 0.9800 . ? C19A H19F 0.9800 . ? C18 C19 1.347(13) . ? C18 H18 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.309(5) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C22 1.334(6) 3_655 ? N3 C23 1.122(5) . ? C23 C24 1.437(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? 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 F2 P1 F6 90.53(14) . . ? F2 P1 F1 179.32(14) . . ? F6 P1 F1 89.70(12) . . ? F2 P1 F4 90.77(13) . . ? F6 P1 F4 90.45(13) . . ? F1 P1 F4 89.87(11) . . ? F2 P1 F5 90.29(15) . . ? F6 P1 F5 179.15(13) . . ? F1 P1 F5 89.48(12) . . ? F4 P1 F5 89.77(12) . . ? F2 P1 F3 89.91(13) . . ? F6 P1 F3 89.66(12) . . ? F1 P1 F3 89.45(11) . . ? F4 P1 F3 179.31(12) . . ? F5 P1 F3 90.10(12) . . ? F18 P2 F16 89.9(7) . . ? F18 P2 F8 130.3(6) . . ? F16 P2 F8 126.4(6) . . ? F18 P2 F12 78.5(3) . . ? F16 P2 F12 135.9(5) . . ? F8 P2 F12 91.4(2) . . ? F18 P2 F10 139.5(6) . . ? F16 P2 F10 70.0(4) . . ? F8 P2 F10 88.7(2) . . ? F12 P2 F10 91.8(3) . . ? F16 P2 F9 104.1(4) . . ? F8 P2 F9 95.7(3) . . ? F12 P2 F9 92.2(3) . . ? F10 P2 F9 174.1(2) . . ? F18 P2 F13 91.9(5) . . ? F16 P2 F13 93.3(4) . . ? F8 P2 F13 115.1(3) . . ? F10 P2 F13 56.2(3) . . ? F9 P2 F13 124.7(3) . . ? F18 P2 F14 91.9(5) . . ? F16 P2 F14 90.3(4) . . ? F8 P2 F14 59.7(3) . . ? F12 P2 F14 132.0(4) . . ? F10 P2 F14 121.9(4) . . ? F9 P2 F14 57.8(3) . . ? F13 P2 F14 174.8(3) . . ? F18 P2 F15 92.1(7) . . ? F16 P2 F15 177.6(5) . . ? F8 P2 F15 52.8(5) . . ? F10 P2 F15 107.6(3) . . ? F9 P2 F15 78.3(3) . . ? F13 P2 F15 85.4(4) . . ? F14 P2 F15 90.9(4) . . ? F18 P2 F17 175.7(6) . . ? F16 P2 F17 89.7(7) . . ? F8 P2 F17 52.8(5) . . ? F12 P2 F17 98.9(3) . . ? F9 P2 F17 146.5(5) . . ? F13 P2 F17 83.8(4) . . ? F14 P2 F17 92.4(4) . . ? F15 P2 F17 88.2(6) . . ? F18 P2 F7 52.2(6) . . ? F16 P2 F7 52.2(5) . . ? F8 P2 F7 177.5(3) . . ? F12 P2 F7 89.0(3) . . ? F10 P2 F7 88.8(3) . . ? F9 P2 F7 86.8(3) . . ? F13 P2 F7 63.6(3) . . ? F14 P2 F7 121.6(3) . . ? F15 P2 F7 128.5(5) . . ? F17 P2 F7 124.7(6) . . ? F18 P2 F11 99.2(3) . . ? F8 P2 F11 93.3(3) . . ? F12 P2 F11 175.2(3) . . ? F10 P2 F11 87.3(3) . . ? F9 P2 F11 88.4(2) . . ? F13 P2 F11 130.8(4) . . ? F14 P2 F11 51.9(3) . . ? F15 P2 F11 141.2(4) . . ? F17 P2 F11 83.2(3) . . ? F7 P2 F11 86.2(3) . . ? C20 S1 C22 94.30(16) . . ? C21 S2 C22 94.37(16) . . ? C2 N1 C6 120.5(2) . . ? C2 N1 C1 119.7(3) . . ? C6 N1 C1 119.5(3) . . ? C10 N2 C9 120.2(2) . . ? C10 N2 C12 119.4(3) . . ? C9 N2 C12 120.1(3) . . ? N1 C1 C16 107.4(2) . 3_655 ? N1 C1 H1A 110.2 . . ? C16 C1 H1A 110.2 3_655 . ? N1 C1 H1B 110.2 . . ? C16 C1 H1B 110.2 3_655 . ? H1A C1 H1B 108.5 . . ? N1 C2 C3 121.4(3) . . ? N1 C2 H2 119.3 . . ? C3 C2 H2 119.3 . . ? C2 C3 C4 120.0(3) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C5 116.7(3) . . ? C3 C4 C7 121.8(3) . . ? C5 C4 C7 121.4(2) . . ? C6 C5 C4 120.5(3) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? N1 C6 C5 120.9(3) . . ? N1 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C8 C7 C11 117.0(2) . . ? C8 C7 C4 121.8(2) . . ? C11 C7 C4 121.1(3) . . ? C9 C8 C7 120.1(3) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? N2 C9 C8 121.4(3) . . ? N2 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? N2 C10 C11 120.8(3) . . ? N2 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C10 C11 C7 120.5(3) . . ? C10 C11 H11 119.8 . . ? C7 C11 H11 119.8 . . ? N2 C12 C13 108.7(2) . . ? N2 C12 H12A 110.0 . . ? C13 C12 H12A 110.0 . . ? N2 C12 H12B 110.0 . . ? C13 C12 H12B 110.0 . . ? H12A C12 H12B 108.3 . . ? C14 C13 C18 119.3(3) . . ? C14 C13 C12 120.1(3) . . ? C18 C13 C12 120.5(3) . . ? C13 C14 C15 120.7(3) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C16 C15 C14 119.7(3) . . ? C16 C15 C19B 128.3(18) . . ? C14 C15 C19B 108.6(17) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C19B H19G 109.5 . . ? C15 C19B H19H 109.5 . . ? H19G C19B H19H 109.5 . . ? C15 C19B H19I 109.5 . . ? H19G C19B H19I 109.5 . . ? H19H C19B H19I 109.5 . . ? C15 C16 C17 120.0(3) . . ? C15 C16 C1 120.1(3) . 3_655 ? C17 C16 C1 119.8(3) . 3_655 ? C16 C17 C18 120.1(3) . . ? C16 C17 C19A 123.2(16) . . ? C18 C17 C19A 116.5(16) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C19A H19D 109.5 . . ? C17 C19A H19E 109.5 . . ? H19D C19A H19E 109.5 . . ? C17 C19A H19F 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? C19 C18 C13 122.1(7) . . ? C19 C18 C17 117.7(7) . . ? C13 C18 C17 120.1(3) . . ? C13 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 S1 118.7(3) . . ? C21 C20 H20 120.7 . . ? S1 C20 H20 120.7 . . ? C20 C21 S2 118.1(3) . . ? C20 C21 H21 121.0 . . ? S2 C21 H21 121.0 . . ? C22 C22 S1 122.2(3) 3_655 . ? C22 C22 S2 123.3(3) 3_655 . ? S1 C22 S2 114.57(17) . . ? N3 C23 C24 178.9(5) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 N1 C1 C16 89.5(3) . . . 3_655 ? C6 N1 C1 C16 -83.8(3) . . . 3_655 ? C6 N1 C2 C3 2.1(4) . . . . ? C1 N1 C2 C3 -171.1(2) . . . . ? N1 C2 C3 C4 0.2(4) . . . . ? C2 C3 C4 C5 -2.4(4) . . . . ? C2 C3 C4 C7 175.0(2) . . . . ? C3 C4 C5 C6 2.4(4) . . . . ? C7 C4 C5 C6 -174.9(2) . . . . ? C2 N1 C6 C5 -2.0(4) . . . . ? C1 N1 C6 C5 171.2(3) . . . . ? C4 C5 C6 N1 -0.3(4) . . . . ? C3 C4 C7 C8 -5.8(4) . . . . ? C5 C4 C7 C8 171.4(2) . . . . ? C3 C4 C7 C11 176.5(2) . . . . ? C5 C4 C7 C11 -6.2(4) . . . . ? C11 C7 C8 C9 2.4(4) . . . . ? C4 C7 C8 C9 -175.3(2) . . . . ? C10 N2 C9 C8 -2.1(4) . . . . ? C12 N2 C9 C8 171.8(3) . . . . ? C7 C8 C9 N2 0.2(4) . . . . ? C9 N2 C10 C11 1.3(4) . . . . ? C12 N2 C10 C11 -172.7(2) . . . . ? N2 C10 C11 C7 1.4(4) . . . . ? C8 C7 C11 C10 -3.2(4) . . . . ? C4 C7 C11 C10 174.6(2) . . . . ? C10 N2 C12 C13 90.7(3) . . . . ? C9 N2 C12 C13 -83.3(3) . . . . ? N2 C12 C13 C14 -91.4(3) . . . . ? N2 C12 C13 C18 85.2(3) . . . . ? C18 C13 C14 C15 -4.0(4) . . . . ? C12 C13 C14 C15 172.7(2) . . . . ? C13 C14 C15 C16 1.0(4) . . . . ? C13 C14 C15 C19B 162.0(18) . . . . ? C14 C15 C16 C17 2.8(4) . . . . ? C19B C15 C16 C17 -154(2) . . . . ? C14 C15 C16 C1 -172.1(2) . . . 3_655 ? C19B C15 C16 C1 31(2) . . . 3_655 ? C15 C16 C17 C18 -3.6(4) . . . . ? C1 C16 C17 C18 171.4(2) 3_655 . . . ? C15 C16 C17 C19A -177.9(19) . . . . ? C1 C16 C17 C19A -3.0(19) 3_655 . . . ? C14 C13 C18 C19 178.9(8) . . . . ? C12 C13 C18 C19 2.2(8) . . . . ? C14 C13 C18 C17 3.3(4) . . . . ? C12 C13 C18 C17 -173.4(2) . . . . ? C16 C17 C18 C19 -175.3(7) . . . . ? C19A C17 C18 C19 -0.6(19) . . . . ? C16 C17 C18 C13 0.5(4) . . . . ? C19A C17 C18 C13 175.2(18) . . . . ? C22 S1 C20 C21 0.3(3) . . . . ? S1 C20 C21 S2 0.4(4) . . . . ? C22 S2 C21 C20 -0.9(3) . . . . ? C20 S1 C22 C22 179.0(3) . . . 3_655 ? C20 S1 C22 S2 -0.82(18) . . . . ? C21 S2 C22 C22 -178.9(3) . . . 3_655 ? C21 S2 C22 S1 0.99(19) . . . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.459 _refine_diff_density_min -0.325 _refine_diff_density_rms 0.058