# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1372 data_kaa _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C104 H112 F24 N8 O12 P4' _chemical_formula_weight 2245.88 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.9704(9) _cell_length_b 18.3237(9) _cell_length_c 19.771(1) _cell_angle_alpha 67.629(1) _cell_angle_beta 67.447(1) _cell_angle_gamma 78.767(1) _cell_volume 5550.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Needles _exptl_crystal_colour 'Pale Yellow' _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2328 _exptl_absorpt_coefficient_mu 0.169 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.9313 _exptl_absorpt_correction_T_max 0.9757 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-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 39952 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0805 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 22.50 _reflns_number_total 14505 _reflns_number_gt 7814 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0035(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 14505 _refine_ls_number_parameters 1688 _refine_ls_number_restraints 248 _refine_ls_R_factor_all 0.1552 _refine_ls_R_factor_gt 0.0846 _refine_ls_wR_factor_ref 0.2365 _refine_ls_wR_factor_gt 0.2058 _refine_ls_goodness_of_fit_ref 1.295 _refine_ls_restrained_S_all 1.284 _refine_ls_shift/su_max 0.252 _refine_ls_shift/su_mean 0.029 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 0.9017(3) 0.2709(6) 0.0190(3) 0.0673(18) Uani 0.75(3) 1 d PD A 1 F11 F 0.8899(9) 0.1793(8) 0.0421(6) 0.134(6) Uani 0.75(3) 1 d PD A 1 F12 F 0.8089(5) 0.2918(13) 0.0267(6) 0.148(6) Uani 0.75(3) 1 d PD A 1 F13 F 0.9152(7) 0.3622(7) -0.0043(5) 0.095(4) Uani 0.75(3) 1 d PD A 1 F14 F 0.9254(5) 0.2820(8) -0.0708(5) 0.077(3) Uani 0.75(3) 1 d PD A 1 F15 F 0.8796(6) 0.2596(8) 0.1087(4) 0.085(3) Uani 0.75(3) 1 d PD A 1 F16 F 0.99461(18) 0.25019(18) 0.01120(15) 0.0746(10) Uani 1 1 d D . . P1' P 0.9002(11) 0.2440(10) 0.0252(7) 0.078(5) Uani 0.25(3) 1 d PD A 2 F11' F 0.9130(13) 0.1526(13) 0.0472(13) 0.080(7) Uani 0.25(3) 1 d PD A 2 F12' F 0.8102(16) 0.2381(18) 0.0385(13) 0.085(9) Uani 0.25(3) 1 d PD A 2 F13' F 0.8863(19) 0.3353(14) 0.0034(15) 0.116(13) Uani 0.25(3) 1 d PD A 2 F14' F 0.9226(16) 0.2524(16) -0.0615(12) 0.104(11) Uani 0.25(3) 1 d PD A 2 F15' F 0.8767(15) 0.2355(15) 0.1121(11) 0.072(8) Uani 0.25(3) 1 d PD A 2 P2 P 0.3944(3) 0.4954(3) 0.3371(5) 0.070(2) Uani 0.642(19) 1 d PD B 3 F21 F 0.4625(6) 0.5402(5) 0.3331(7) 0.108(4) Uani 0.642(19) 1 d PD B 3 F22 F 0.4023(5) 0.5477(6) 0.2513(5) 0.121(4) Uani 0.642(19) 1 d PD B 3 F23 F 0.4593(5) 0.4337(5) 0.3072(7) 0.165(6) Uani 0.642(19) 1 d PD B 3 F24 F 0.3294(6) 0.5565(5) 0.3677(6) 0.095(4) Uani 0.642(19) 1 d PD B 3 F25 F 0.3262(5) 0.4500(5) 0.3418(6) 0.091(4) Uani 0.642(19) 1 d PD B 3 F26 F 0.3865(6) 0.4429(6) 0.4229(6) 0.165(7) Uani 0.642(19) 1 d PD B 3 P2' P 0.3918(5) 0.5028(8) 0.3559(9) 0.106(5) Uani 0.358(19) 1 d PD B 4 F21' F 0.4289(11) 0.5602(8) 0.3769(14) 0.115(6) Uani 0.358(19) 1 d PD B 4 F22' F 0.4035(11) 0.5677(12) 0.2719(11) 0.160(11) Uani 0.358(19) 1 d PD B 4 F23' F 0.4799(9) 0.4652(13) 0.3224(9) 0.146(10) Uani 0.358(19) 1 d PD B 4 F24' F 0.3039(9) 0.5419(13) 0.3876(13) 0.177(13) Uani 0.358(19) 1 d PD B 4 F25' F 0.3549(14) 0.4469(12) 0.3331(12) 0.151(10) Uani 0.358(19) 1 d PD B 4 F26' F 0.3801(10) 0.4381(9) 0.4399(11) 0.103(8) Uani 0.358(19) 1 d PD B 4 P3 P 0.3588(5) 0.9082(8) 0.4007(5) 0.071(3) Uani 0.428(16) 1 d PD C 5 F31 F 0.4197(8) 0.9133(9) 0.4315(8) 0.151(8) Uani 0.428(16) 1 d PD C 5 F32 F 0.2907(9) 0.9134(13) 0.3746(10) 0.222(17) Uani 0.428(16) 1 d PD C 5 F33 F 0.3142(10) 0.9729(10) 0.4299(11) 0.201(18) Uani 0.428(16) 1 d PD C 5 F34 F 0.3136(8) 0.8551(11) 0.4783(6) 0.157(9) Uani 0.428(16) 1 d PD C 5 F35 F 0.3969(11) 0.9716(10) 0.3278(8) 0.39(3) Uani 0.428(16) 1 d PD C 5 F36 F 0.4033(8) 0.8435(10) 0.3715(10) 0.101(5) Uani 0.428(16) 1 d PD C 5 P3' P 0.3714(6) 0.9302(7) 0.3901(6) 0.113(4) Uani 0.572(16) 1 d PD C 6 F31' F 0.4615(8) 0.9344(6) 0.3810(11) 0.217(10) Uani 0.572(16) 1 d PD C 6 F32' F 0.2867(6) 0.9158(9) 0.3925(9) 0.283(18) Uani 0.572(16) 1 d PD C 6 F33' F 0.3462(14) 0.9993(10) 0.4248(9) 0.141(6) Uani 0.572(16) 1 d PD C 6 F34' F 0.3597(11) 0.8610(8) 0.4702(6) 0.213(11) Uani 0.572(16) 1 d PD C 6 F35' F 0.3854(5) 0.9950(7) 0.3071(6) 0.110(4) Uani 0.572(16) 1 d PD C 6 F36' F 0.4097(8) 0.8669(8) 0.3485(8) 0.215(12) Uani 0.572(16) 1 d PD C 6 P4 P 0.44356(17) 0.6394(2) 0.00765(18) 0.097(3) Uani 0.637(16) 1 d PD D 7 F41 F 0.3685(4) 0.6000(4) 0.0792(4) 0.148(6) Uani 0.637(16) 1 d PD D 7 F42 F 0.4513(4) 0.5720(4) -0.0263(4) 0.114(4) Uani 0.637(16) 1 d PD D 7 F43 F 0.4336(4) 0.7085(4) 0.0400(4) 0.112(4) Uani 0.637(16) 1 d PD D 7 F44 F 0.5026(4) 0.5903(4) 0.0532(4) 0.142(5) Uani 0.637(16) 1 d PD D 7 F45 F 0.5166(3) 0.6805(4) -0.0655(3) 0.096(4) Uani 0.637(16) 1 d PD D 7 F46 F 0.3847(4) 0.6883(4) -0.0378(4) 0.097(3) Uani 0.637(16) 1 d PD D 7 P4' P 0.4428(8) 0.6347(9) 0.0043(7) 0.220(14) Uani 0.363(16) 1 d PD D 8 F41' F 0.3868(14) 0.5640(12) 0.0295(17) 0.30(2) Uani 0.363(16) 1 d PD D 8 F42' F 0.4870(14) 0.6252(16) -0.0797(11) 0.31(2) Uani 0.363(16) 1 d PD D 8 F43' F 0.4069(14) 0.636(2) 0.0918(12) 0.54(5) Uani 0.363(16) 1 d PD D 8 F44' F 0.5071(10) 0.5674(13) 0.0321(11) 0.206(14) Uani 0.363(16) 1 d PD D 8 F45' F 0.5071(17) 0.6968(11) -0.0175(18) 0.261(18) Uani 0.363(16) 1 d PD D 8 F46' F 0.3786(13) 0.7020(15) -0.0235(15) 0.38(4) Uani 0.363(16) 1 d PD D 8 C1 C 0.7427 1.0271 -0.0512 0.045 Uani 1 1 d . . . C2 C 0.7638 0.9993 0.0155 0.043 Uani 1 1 d . . . C3 C 0.8309 0.9473 0.0224 0.041 Uani 1 1 d . F . C4 C 0.8751 0.9213 -0.0406 0.043 Uani 1 1 d . . . H4A H 0.9203 0.8851 -0.0372 0.052 Uiso 1 1 calc R . . C5 C 0.8558 0.9462 -0.1084 0.043 Uani 1 1 d . F . C6 C 0.7880 0.9982 -0.1111 0.044 Uani 1 1 d . . . O7 O 0.7678 1.0266 -0.1788 0.048 Uani 1 1 d . . . C8 C 0.7232 0.9769 -0.1873 0.054 Uani 1 1 d . . . H8A H 0.6864 1.0102 -0.2151 0.065 Uiso 1 1 calc R . . H8B H 0.6896 0.9445 -0.1350 0.065 Uiso 1 1 calc R . . O9 O 0.7726 0.9256 -0.2285 0.048 Uani 1 1 d . F . C10 C 0.9028 0.9172 -0.1773 0.044 Uani 1 1 d . . . H11L H 0.8938 0.9584 -0.2245 0.052 Uiso 1 1 calc R E 9 C11 C 0.7563(3) 0.7863(4) -0.1694(3) 0.0446(15) Uani 1 1 d . F . C13 C 0.8637(3) 0.8430(3) -0.1619(3) 0.0413(14) Uani 1 1 d . F . C14 C 0.8876(3) 0.7673(4) -0.1229(3) 0.0443(15) Uani 1 1 d . . . H14A H 0.9318 0.7608 -0.1056 0.053 Uiso 1 1 calc R F . C15 C 0.8503(3) 0.6997(3) -0.1075(3) 0.0394(14) Uani 1 1 d . F . C16 C 0.7844(3) 0.7118(4) -0.1318(3) 0.0428(14) Uani 1 1 d . . . O17 O 0.7470(2) 0.6471(2) -0.1224(2) 0.0481(10) Uani 1 1 d . F . C18 C 0.6910(3) 0.6085(4) -0.0477(3) 0.0524(16) Uani 1 1 d . . . H18A H 0.6642 0.6480 -0.0216 0.063 Uiso 1 1 calc R F . H18B H 0.6489 0.5873 -0.0548 0.063 Uiso 1 1 calc R . . O19 O 0.7264(2) 0.5463(2) 0.0009(2) 0.0520(10) Uani 1 1 d . F . C20 C 0.8772(3) 0.6175(3) -0.0644(3) 0.0456(15) Uani 1 1 d . . . H20A H 0.8627 0.5805 -0.0832 0.055 Uiso 1 1 calc R F . C21 C 0.7008(3) 0.5512(3) 0.1269(3) 0.0467(15) Uani 1 1 d . F . C22 C 0.7513(3) 0.5672(3) 0.0496(3) 0.0467(15) Uani 1 1 d . . . C23 C 0.8248(3) 0.5985(3) 0.0219(3) 0.0431(14) Uani 1 1 d . F . C24 C 0.8484(3) 0.6157(3) 0.0741(3) 0.0454(14) Uani 1 1 d . . . H24A H 0.8989 0.6380 0.0559 0.054 Uiso 1 1 calc R F . C25 C 0.7996(3) 0.6011(3) 0.1517(3) 0.0419(14) Uani 1 1 d . F . C26 C 0.7256(3) 0.5710(3) 0.1763(3) 0.0455(14) Uani 1 1 d . . . O27 O 0.6754(2) 0.5527(2) 0.2543(2) 0.0508(10) Uani 1 1 d . F . C28 C 0.6271(3) 0.6169(4) 0.2765(3) 0.0513(16) Uani 1 1 d . . . H28A H 0.6158 0.6571 0.2307 0.062 Uiso 1 1 calc R F . H28B H 0.5748 0.5974 0.3164 0.062 Uiso 1 1 calc R . . O29 O 0.6642(2) 0.6528(2) 0.3063(2) 0.0525(10) Uani 1 1 d . F . C30 C 0.8238(3) 0.6213(3) 0.2081(3) 0.0450(14) Uani 1 1 d . . . H30A H 0.7963 0.5844 0.2614 0.054 Uiso 1 1 calc R F . C31 C 0.6754(3) 0.7918(4) 0.2504(3) 0.0475(15) Uani 1 1 d . F . C12 C 0.7969(3) 0.8507(4) -0.1844(3) 0.0466(15) Uani 1 1 d . . . C32 C 0.7100(3) 0.7171(4) 0.2529(3) 0.0459(15) Uani 1 1 d . . . C33 C 0.7887(3) 0.7045(4) 0.2067(3) 0.0428(14) Uani 1 1 d . F . C34 C 0.8317(3) 0.7708(4) 0.1571(3) 0.0424(14) Uani 1 1 d . . . H34A H 0.8854 0.7636 0.1245 0.051 Uiso 1 1 calc R F . C35 C 0.8004(3) 0.8472(4) 0.1525(3) 0.0430(14) Uani 1 1 d . F . C36 C 0.7210(3) 0.8561(4) 0.1999(3) 0.0463(15) Uani 1 1 d . . . O37 O 0.6871(2) 0.9317(2) 0.2008(2) 0.0519(10) Uani 1 1 d . F . C38 C 0.6599(4) 0.9796(4) 0.1380(4) 0.0579(17) Uani 1 1 d . . . H38A H 0.6119 1.0127 0.1574 0.070 Uiso 1 1 calc R F . H38B H 0.6430 0.9448 0.1191 0.070 Uiso 1 1 calc R . . O39 O 0.7188(2) 1.0296(2) 0.0745(2) 0.0543(10) Uani 1 1 d . F . C40 C 0.8494(3) 0.9188(3) 0.0968(3) 0.0458(15) Uani 1 1 d . . . H40A H 0.8281 0.9615 0.1204 0.055 Uiso 1 1 calc R F . C41 C 0.6743(3) 1.0886(4) -0.0602(3) 0.0560(16) Uani 1 1 d . . . H41A H 0.6465 1.0772 -0.0894 0.067 Uiso 1 1 calc R . . H41B H 0.6347 1.0858 -0.0082 0.067 Uiso 1 1 calc R . . N42 N 0.7045(3) 1.1687(3) -0.1019(3) 0.0513(13) Uani 1 1 d . . . C43 C 0.7400(4) 1.1980(4) -0.0697(4) 0.0619(18) Uani 1 1 d . . . H43A H 0.7443 1.1674 -0.0202 0.074 Uiso 1 1 calc R . . C44 C 0.7696(4) 1.2700(5) -0.1069(4) 0.0674(19) Uani 1 1 d . . . H44A H 0.7951 1.2887 -0.0830 0.081 Uiso 1 1 calc R . . C45 C 0.7646(3) 1.3181(4) -0.1787(4) 0.0544(16) Uani 1 1 d . . . C46 C 0.7285(4) 1.2858(4) -0.2103(4) 0.0624(18) Uani 1 1 d . . . H46A H 0.7238 1.3153 -0.2599 0.075 Uiso 1 1 calc R . . C47 C 0.6993(4) 1.2118(4) -0.1715(4) 0.0566(17) Uani 1 1 d . . . H47A H 0.6749 1.1909 -0.1946 0.068 Uiso 1 1 calc R . . C48 C 0.7966(4) 1.3977(4) -0.2186(4) 0.0604(17) Uani 1 1 d . . . C49 C 0.8083(4) 1.4393(5) -0.1777(5) 0.079(2) Uani 1 1 d . . . H49A H 0.7946 1.4167 -0.1228 0.094 Uiso 1 1 calc R . . C50 C 0.8387(5) 1.5112(6) -0.2154(6) 0.097(3) Uani 1 1 d . . . H50A H 0.8470 1.5373 -0.1857 0.116 Uiso 1 1 calc R . . N51 N 0.8580(4) 1.5480(4) -0.2919(6) 0.097(2) Uani 1 1 d . . . C52 C 0.8469(5) 1.5090(5) -0.3315(5) 0.094(2) Uani 1 1 d . . . H52A H 0.8597 1.5341 -0.3861 0.112 Uiso 1 1 calc R . . C53 C 0.8180(4) 1.4346(5) -0.2982(5) 0.074(2) Uani 1 1 d . . . H53A H 0.8128 1.4089 -0.3296 0.089 Uiso 1 1 calc R . . C54 C 0.6837(3) 0.7963(4) -0.1936(3) 0.0499(15) Uani 1 1 d . . . H54A H 0.6449 0.7560 -0.1546 0.060 Uiso 1 1 calc R F . H54B H 0.6565 0.8492 -0.1954 0.060 Uiso 1 1 calc R . . N55 N 0.7082(2) 0.7880(3) -0.2716(3) 0.0421(11) Uani 1 1 d . F . C56 C 0.7247(4) 0.8509(4) -0.3349(4) 0.0610(17) Uani 1 1 d . . . H56A H 0.7224 0.9010 -0.3301 0.073 Uiso 1 1 calc R F . C57 C 0.7449(4) 0.8464(4) -0.4078(3) 0.0587(17) Uani 1 1 d . F . H57A H 0.7546 0.8933 -0.4520 0.070 Uiso 1 1 calc R . . C58 C 0.7512(3) 0.7758(4) -0.4170(3) 0.0472(15) Uani 1 1 d . . . C59 C 0.7353(4) 0.7110(4) -0.3502(4) 0.072(2) Uani 1 1 d . F . H59A H 0.7390 0.6600 -0.3536 0.087 Uiso 1 1 calc R . . C60 C 0.7140(4) 0.7184(4) -0.2783(4) 0.071(2) Uani 1 1 d . . . H60A H 0.7033 0.6725 -0.2330 0.085 Uiso 1 1 calc R F . C61 C 0.7697(3) 0.7701(4) -0.4950(4) 0.0516(16) Uani 1 1 d . F . C62 C 0.8052(4) 0.8305(4) -0.5628(4) 0.0681(19) Uani 1 1 d . . . H62A H 0.8217 0.8757 -0.5609 0.082 Uiso 1 1 calc R F . C63 C 0.8160(4) 0.8237(6) -0.6329(4) 0.083(2) Uani 1 1 d . F . H63A H 0.8406 0.8657 -0.6786 0.099 Uiso 1 1 calc R . . N64 N 0.7955(4) 0.7644(5) -0.6421(4) 0.086(2) Uani 1 1 d . . . C65 C 0.7617(5) 0.7069(5) -0.5781(5) 0.084(2) Uani 1 1 d . F . H65A H 0.7456 0.6634 -0.5831 0.101 Uiso 1 1 calc R . . C66 C 0.7478(4) 0.7054(4) -0.5021(4) 0.0688(19) Uani 1 1 d . . . H66A H 0.7245 0.6617 -0.4576 0.083 Uiso 1 1 calc R F . C67 C 0.6226(3) 0.5110(3) 0.1569(3) 0.0485(15) Uani 1 1 d . . . H67A H 0.5819 0.5301 0.1980 0.058 Uiso 1 1 calc R F . H67B H 0.6014 0.5238 0.1141 0.058 Uiso 1 1 calc R . . N68 N 0.6380(3) 0.4246(3) 0.1888(3) 0.0482(12) Uani 1 1 d . F . C69 C 0.6576(4) 0.3807(4) 0.1437(4) 0.0630(18) Uani 1 1 d . . . H69A H 0.6587 0.4051 0.0915 0.076 Uiso 1 1 calc R F . C70 C 0.6759(4) 0.3021(4) 0.1703(4) 0.0668(19) Uani 1 1 d . F . H70A H 0.6882 0.2722 0.1369 0.080 Uiso 1 1 calc R . . C71 C 0.6773(3) 0.2638(4) 0.2464(3) 0.0535(16) Uani 1 1 d . . . C72 C 0.6572(4) 0.3115(4) 0.2910(3) 0.0578(17) Uani 1 1 d . F . H72A H 0.6574 0.2891 0.3428 0.069 Uiso 1 1 calc R . . C73 C 0.6367(3) 0.3905(4) 0.2624(4) 0.0565(17) Uani 1 1 d . . . H73A H 0.6215 0.4215 0.2952 0.068 Uiso 1 1 calc R F . C74 C 0.6971(3) 0.1782(4) 0.2768(4) 0.0559(17) Uani 1 1 d . F . N75 N 0.7314(4) 0.0141(4) 0.3350(5) 0.098(2) Uani 1 1 d . . . C75 C 0.7307(5) 0.1317(5) 0.2297(4) 0.082(2) Uani 1 1 d . . . H75A H 0.7431 0.1555 0.1750 0.098 Uiso 1 1 calc R F . C76 C 0.7458(5) 0.0530(5) 0.2608(6) 0.096(3) Uani 1 1 d . F . H76A H 0.7685 0.0237 0.2261 0.116 Uiso 1 1 calc R . . C78 C 0.6999(5) 0.0573(5) 0.3810(5) 0.086(2) Uani 1 1 d . F . H78A H 0.6884 0.0314 0.4354 0.103 Uiso 1 1 calc R . . C79 C 0.6827(4) 0.1380(5) 0.3545(4) 0.0715(19) Uani 1 1 d . . . H79A H 0.6608 0.1658 0.3904 0.086 Uiso 1 1 calc R F . C80 C 0.5888(3) 0.8036(4) 0.2995(3) 0.0538(16) Uani 1 1 d . . . H80A H 0.5660 0.8551 0.2723 0.065 Uiso 1 1 calc R F . H80B H 0.5569 0.7616 0.3056 0.065 Uiso 1 1 calc R . . N81 N 0.5814(3) 0.8017(3) 0.3773(3) 0.0504(13) Uani 1 1 d . F . C82 C 0.5415(4) 0.7461(4) 0.4408(4) 0.0647(18) Uani 1 1 d . . . H82A H 0.5217 0.7048 0.4357 0.078 Uiso 1 1 calc R F . C83 C 0.5279(4) 0.7465(4) 0.5144(4) 0.0694(19) Uani 1 1 d . F . H83A H 0.4998 0.7053 0.5591 0.083 Uiso 1 1 calc R . . C84 C 0.5553(3) 0.8069(4) 0.5226(4) 0.0565(17) Uani 1 1 d . . . C85 C 0.5993(3) 0.8630(4) 0.4539(4) 0.0548(16) Uani 1 1 d . F . H85A H 0.6206 0.9048 0.4568 0.066 Uiso 1 1 calc R . . C86 C 0.6122(3) 0.8588(4) 0.3838(4) 0.0528(16) Uani 1 1 d . . . H86A H 0.6436 0.8969 0.3382 0.063 Uiso 1 1 calc R F . C87 C 0.5380(3) 0.8138(5) 0.5987(4) 0.0634(19) Uani 1 1 d . F . C88 C 0.5361(4) 0.7495(5) 0.6637(4) 0.079(2) Uani 1 1 d . . . H88A H 0.5464 0.6978 0.6606 0.095 Uiso 1 1 calc R F . C89 C 0.5190(5) 0.7600(8) 0.7344(5) 0.112(4) Uani 1 1 d . F . H89A H 0.5200 0.7144 0.7782 0.134 Uiso 1 1 calc R . . N90 N 0.5016(4) 0.8297(7) 0.7441(4) 0.113(3) Uani 1 1 d . . . C91 C 0.5040(4) 0.8914(7) 0.6821(5) 0.102(3) Uani 1 1 d . F . H91A H 0.4935 0.9421 0.6874 0.122 Uiso 1 1 calc R . . C92 C 0.5213(4) 0.8875(5) 0.6080(4) 0.078(2) Uani 1 1 d . . . H92A H 0.5215 0.9343 0.5650 0.093 Uiso 1 1 calc R F . C93 C 0.982(4) 0.901(4) -0.195(5) 0.051(18) Uani 0.27(4) 1 d P F 9 H93C H 0.9895 0.8598 -0.1473 0.061 Uiso 0.27(4) 1 calc PR F 9 H93D H 1.0054 0.9487 -0.2019 0.061 Uiso 0.27(4) 1 calc PR F 9 C94 C 1.041(6) 0.870(5) -0.268(6) 0.047(15) Uani 0.27(4) 1 d P F 9 H94A H 1.0937 0.8465 -0.2614 0.057 Uiso 0.27(4) 1 calc PR F 9 H94B H 1.0152 0.8323 -0.2751 0.057 Uiso 0.27(4) 1 calc PR F 9 C95 C 1.051(3) 0.951(3) -0.335(4) 0.051(14) Uani 0.27(4) 1 d P F 9 H95A H 1.0884 0.9826 -0.3333 0.061 Uiso 0.27(4) 1 calc PR F 9 H95B H 0.9980 0.9806 -0.3301 0.061 Uiso 0.27(4) 1 calc PR F 9 C96 C 1.089(6) 0.930(5) -0.421(3) 0.41(9) Uani 0.27(4) 1 d P F 9 H96A H 1.0963 0.8783 -0.4225 0.492 Uiso 0.27(4) 1 calc PR F 9 C97 C 1.104(3) 0.986(3) -0.475(3) 0.15(3) Uani 0.27(4) 1 d P F 9 H97A H 1.1381 0.9703 -0.5202 0.219 Uiso 0.27(4) 1 calc PR F 9 H97B H 1.1330 1.0209 -0.4679 0.219 Uiso 0.27(4) 1 calc PR F 9 H97C H 1.0541 1.0132 -0.4832 0.219 Uiso 0.27(4) 1 calc PR F 9 C93' C 0.9982(14) 0.9058(15) -0.1891(16) 0.038(5) Uani 0.73(4) 1 d P F 10 H93A H 1.0164 0.9537 -0.1895 0.046 Uiso 0.73(4) 1 calc PR F 10 H93B H 1.0081 0.8602 -0.1457 0.046 Uiso 0.73(4) 1 calc PR F 10 C94' C 1.044(2) 0.8920(19) -0.264(2) 0.053(6) Uani 0.73(4) 1 d P F 10 H94C H 1.0254 0.8428 -0.2610 0.064 Uiso 0.73(4) 1 calc PR F 10 H94D H 1.1014 0.8821 -0.2692 0.064 Uiso 0.73(4) 1 calc PR F 10 C95' C 1.0380(19) 0.958(2) -0.3418(19) 0.124(13) Uani 0.73(4) 1 d P F 10 H95C H 0.9822 0.9627 -0.3418 0.149 Uiso 0.73(4) 1 calc PR F 10 H95D H 1.0490 1.0096 -0.3426 0.149 Uiso 0.73(4) 1 calc PR F 10 C96' C 1.0945(9) 0.9436(14) -0.4133(10) 0.109(8) Uani 0.73(4) 1 d P F 10 H96B H 1.0793 0.8967 -0.4173 0.130 Uiso 0.73(4) 1 calc PR F 10 H96C H 1.1500 0.9334 -0.4117 0.130 Uiso 0.73(4) 1 calc PR F 10 C97' C 1.0907(15) 1.021(2) -0.4882(14) 0.190(14) Uani 0.73(4) 1 d P F 10 H97D H 1.1317 1.0138 -0.5355 0.286 Uiso 0.73(4) 1 calc PR F 10 H97E H 1.1011 1.0679 -0.4817 0.286 Uiso 0.73(4) 1 calc PR F 10 H97F H 1.0371 1.0275 -0.4925 0.286 Uiso 0.73(4) 1 calc PR F 10 C98 C 0.9680(3) 0.6041(4) -0.0803(3) 0.0489(15) Uani 1 1 d . F . H98A H 0.9851 0.6407 -0.0635 0.059 Uiso 1 1 calc R . . H98B H 0.9798 0.5494 -0.0488 0.059 Uiso 1 1 calc R . . C99 C 1.0164(3) 0.6170(4) -0.1653(3) 0.0556(16) Uani 1 1 d . . . H99A H 1.0057 0.6721 -0.1966 0.067 Uiso 1 1 calc R F . H99B H 0.9981 0.5815 -0.1824 0.067 Uiso 1 1 calc R . . C100 C 1.1069(3) 0.6016(4) -0.1813(3) 0.0582(17) Uani 1 1 d . F . H10E H 1.1249 0.6370 -0.1639 0.070 Uiso 1 1 calc R . . H10F H 1.1174 0.5465 -0.1498 0.070 Uiso 1 1 calc R . . C101 C 1.1569(4) 0.6140(4) -0.2657(4) 0.072(2) Uani 1 1 d . . . H10G H 1.2131 0.5939 -0.2694 0.086 Uiso 1 1 calc R F . H10H H 1.1356 0.5826 -0.2847 0.086 Uiso 1 1 calc R . . C102 C 1.1575(4) 0.6981(5) -0.3171(4) 0.098(3) Uani 1 1 d . F . H10I H 1.1909 0.7020 -0.3707 0.147 Uiso 1 1 calc R . . H10J H 1.1799 0.7295 -0.2995 0.147 Uiso 1 1 calc R . . H10K H 1.1023 0.7183 -0.3148 0.147 Uiso 1 1 calc R . . C103 C 0.9151(3) 0.6095(4) 0.1944(3) 0.0505(15) Uani 1 1 d . F . H10L H 0.9346 0.5569 0.1888 0.061 Uiso 1 1 calc R . . H10M H 0.9436 0.6499 0.1448 0.061 Uiso 1 1 calc R . . C104 C 0.9372(4) 0.6149(4) 0.2593(4) 0.0592(18) Uani 1 1 d D . . H10N H 0.9965 0.6172 0.2417 0.071 Uiso 0.92(3) 1 calc PR F 11 H11I H 0.9124 0.6648 0.2689 0.071 Uiso 0.92(3) 1 calc PR F 11 H11J H 0.9105 0.6622 0.2698 0.071 Uiso 0.08(3) 1 d PR F 12 H11K H 0.9943 0.6203 0.2414 0.071 Uiso 0.08(3) 1 d PR F 12 C105 C 0.9105(7) 0.5468(6) 0.3349(5) 0.079(4) Uani 0.92(3) 1 d PD F 11 H10O H 0.8510 0.5461 0.3538 0.095 Uiso 0.92(3) 1 calc PR F 11 H10P H 0.9331 0.4967 0.3248 0.095 Uiso 0.92(3) 1 calc PR F 11 C106 C 0.9360(11) 0.5500(12) 0.3983(12) 0.105(7) Uani 0.92(3) 1 d P F 11 H10Q H 0.9107 0.5982 0.4115 0.126 Uiso 0.92(3) 1 calc PR F 11 H10R H 0.9953 0.5530 0.3792 0.126 Uiso 0.92(3) 1 calc PR F 11 C107 C 0.9108(10) 0.4770(10) 0.4711(6) 0.171(7) Uani 0.92(3) 1 d P F 11 H10S H 0.9269 0.4809 0.5117 0.257 Uiso 0.92(3) 1 calc PR F 11 H10T H 0.9374 0.4295 0.4585 0.257 Uiso 0.92(3) 1 calc PR F 11 H10U H 0.8522 0.4739 0.4898 0.257 Uiso 0.92(3) 1 calc PR F 11 C113 C 0.921(7) 0.541(5) 0.331(5) 0.3(2) Uani 0.08(3) 1 d PD F 12 H10V H 0.8652 0.5274 0.3429 0.414 Uiso 0.08(3) 1 calc PR F 12 H10W H 0.9576 0.4983 0.3150 0.414 Uiso 0.08(3) 1 calc PR F 12 C114 C 0.926(7) 0.537(6) 0.404(10) 0.03(4) Uani 0.08(3) 1 d P F 12 H10X H 0.8762 0.5662 0.4267 0.032 Uiso 0.08(3) 1 calc PR F 12 H11Z H 0.9702 0.5725 0.3870 0.032 Uiso 0.08(3) 1 calc PR F 12 C115 C 0.940(5) 0.462(5) 0.486(11) 0.14(9) Uani 0.08(3) 1 d P F 12 H10Y H 0.9555 0.4844 0.5158 0.212 Uiso 0.08(3) 1 calc PR F 12 H10Z H 0.9832 0.4239 0.4687 0.212 Uiso 0.08(3) 1 calc PR F 12 H11H H 0.8900 0.4349 0.5179 0.212 Uiso 0.08(3) 1 calc PR F 12 C108 C 0.9394(3) 0.9047(4) 0.0863(3) 0.0484(15) Uani 1 1 d . F . H10A H 0.9621 0.8610 0.0652 0.058 Uiso 1 1 calc R . . H10B H 0.9675 0.9528 0.0477 0.058 Uiso 1 1 calc R . . C109 C 0.9563(3) 0.8846(4) 0.1612(3) 0.0508(15) Uani 1 1 d . . . H10C H 0.9287 0.8362 0.1997 0.061 Uiso 1 1 calc R F . H10D H 0.9334 0.9281 0.1826 0.061 Uiso 1 1 calc R . . C110 C 1.0460(3) 0.8714(4) 0.1500(4) 0.0621(17) Uani 1 1 d . F . H11A H 1.0689 0.8281 0.1283 0.075 Uiso 1 1 calc R . . H11B H 1.0734 0.9199 0.1117 0.075 Uiso 1 1 calc R . . C111 C 1.0635(4) 0.8508(4) 0.2243(4) 0.0662(18) Uani 1 1 d . . . H11C H 1.1222 0.8533 0.2107 0.079 Uiso 1 1 calc R F . H11D H 1.0358 0.8916 0.2484 0.079 Uiso 1 1 calc R . . C112 C 1.0384(4) 0.7708(5) 0.2839(4) 0.090(2) Uani 1 1 d . F . H11E H 1.0520 0.7631 0.3298 0.135 Uiso 1 1 calc R . . H11F H 1.0669 0.7295 0.2616 0.135 Uiso 1 1 calc R . . H11G H 0.9801 0.7678 0.2992 0.135 Uiso 1 1 calc R . . C201 C 1.2673(10) 0.7740(8) -0.6528(9) 0.195(6) Uiso 1 1 d . . . O201 O 1.189(2) 0.7509(18) -0.518(2) 0.613(19) Uiso 1 1 d . . . C202 C 1.1970(19) 0.7786(17) -0.609(2) 0.367(14) Uiso 1 1 d . . . C203 C 1.1459(11) 0.8611(11) -0.6224(10) 0.244(7) Uiso 1 1 d . . . O204 O 1.3851(4) 0.6286(4) -0.4381(4) 0.142(2) Uiso 1 1 d . . . C204 C 1.4614(10) 0.5356(9) -0.4904(9) 0.109(7) Uiso 0.514(14) 1 d P . 13 C205 C 1.3823(9) 0.5702(9) -0.4515(7) 0.069(4) Uiso 0.514(14) 1 d P . 13 C206 C 1.3058(6) 0.5451(6) -0.4374(6) 0.127(3) Uiso 1 1 d . . . C207 C 1.3430(17) 0.6151(17) -0.4701(15) 0.150(9) Uiso 0.486(14) 1 d P . 14 C208 C 1.3094(16) 0.6762(15) -0.5382(15) 0.177(11) Uiso 0.486(14) 1 d P . 14 C209 C 1.4812(14) 1.0171(15) -0.9065(13) 0.148(8) Uiso 0.50 1 d P G 15 O209 O 1.5126(10) 0.9575(10) -0.9315(9) 0.353(8) Uiso 1 1 d . G 15 C210 C 1.4531(7) 1.1048(7) -0.9334(6) 0.148(4) Uiso 1 1 d . G 15 O210 O 1.6899(5) 0.7929(4) -0.9594(4) 0.163(3) Uiso 1 1 d . . . C211 C 0.9332(11) 0.6998(10) -0.3890(11) 0.235(7) Uiso 1 1 d . H 16 O211 O 0.9371(9) 0.7327(9) -0.3430(9) 0.324(7) Uiso 1 1 d . . . C212 C 1.5982(10) 0.8084(9) -0.9410(9) 0.202(6) Uiso 1 1 d . I 17 O212 O 1.011(5) 0.733(5) -0.460(4) 1.44(8) Uiso 1 1 d . . . O213 O 1.5518(6) 1.1575(5) -0.8897(5) 0.178(3) Uiso 1 1 d . J 18 C213 C 1.6215(7) 0.7840(7) -0.9838(7) 0.139(4) Uiso 1 1 d . I . C214 C 1.4502(11) 0.7455(10) -0.7446(11) 0.247(7) Uiso 1 1 d . . . O214 O 1.5086(9) 1.1200(8) -0.8768(8) 0.139(5) Uiso 0.50 1 d P K 19 O215 O 1.4253(10) 0.6937(10) -0.6407(10) 0.358(7) Uiso 1 1 d . . . O216 O 0.5974(5) 0.5752(4) -0.1733(4) 0.175(3) Uiso 1 1 d . . . O217 O 1.5182(5) 0.6897(5) -0.8491(5) 0.182(3) Uiso 1 1 d . . . O218 O 1.4436(7) 0.8652(6) -0.8069(6) 0.242(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.037(2) 0.126(5) 0.068(3) -0.066(3) -0.0143(19) -0.004(3) F11 0.145(12) 0.139(9) 0.121(8) -0.087(7) 0.026(7) -0.075(9) F12 0.035(4) 0.349(19) 0.109(7) -0.143(11) -0.019(4) 0.006(8) F13 0.120(7) 0.104(7) 0.096(5) -0.067(5) -0.061(5) 0.036(6) F14 0.045(4) 0.149(7) 0.060(5) -0.065(4) -0.008(3) -0.012(4) F15 0.070(6) 0.151(8) 0.063(6) -0.073(5) -0.015(4) -0.006(5) F16 0.047(2) 0.107(3) 0.081(3) -0.043(2) -0.0262(18) 0.0031(19) P1' 0.063(9) 0.118(12) 0.058(8) -0.050(7) -0.022(6) 0.024(9) F11' 0.057(12) 0.140(18) 0.056(13) -0.057(12) -0.017(9) 0.011(12) F12' 0.057(12) 0.16(2) 0.045(10) -0.042(13) -0.019(8) 0.003(14) F13' 0.20(4) 0.048(14) 0.14(2) -0.044(14) -0.11(2) 0.047(18) F14' 0.070(17) 0.18(3) 0.09(2) -0.074(16) -0.029(14) -0.008(15) F15' 0.045(13) 0.104(15) 0.085(18) -0.048(11) -0.040(12) 0.025(10) P2 0.052(3) 0.074(4) 0.093(5) -0.041(3) -0.026(3) 0.007(2) F21 0.073(6) 0.128(8) 0.150(9) -0.067(7) -0.037(6) -0.028(6) F22 0.113(7) 0.172(10) 0.081(7) -0.060(7) -0.006(5) -0.039(6) F23 0.083(7) 0.142(8) 0.307(15) -0.150(9) -0.043(8) 0.016(6) F24 0.069(6) 0.111(7) 0.127(7) -0.088(6) -0.029(5) 0.033(5) F25 0.063(5) 0.086(6) 0.133(8) -0.036(5) -0.040(5) -0.014(4) F26 0.143(13) 0.173(13) 0.129(10) 0.065(9) -0.083(9) -0.060(9) P2' 0.081(8) 0.166(13) 0.077(7) -0.055(8) -0.015(5) -0.018(8) F21' 0.127(14) 0.108(11) 0.139(16) -0.066(11) -0.068(12) 0.031(10) F22' 0.25(3) 0.139(17) 0.091(14) -0.022(14) -0.090(16) 0.031(15) F23' 0.047(9) 0.20(2) 0.137(14) -0.051(15) 0.002(9) 0.022(12) F24' 0.070(12) 0.33(3) 0.20(2) -0.18(2) -0.030(13) 0.012(14) F25' 0.092(15) 0.26(3) 0.18(2) -0.19(2) -0.027(13) 0.003(15) F26' 0.100(15) 0.128(16) 0.113(12) -0.085(13) -0.009(10) -0.043(12) P3 0.068(5) 0.086(5) 0.078(6) -0.054(4) -0.032(4) 0.026(4) F31 0.057(10) 0.26(2) 0.167(17) -0.088(14) -0.042(10) -0.039(11) F32 0.18(2) 0.40(4) 0.085(12) 0.005(16) -0.090(13) -0.10(2) F33 0.32(4) 0.13(2) 0.21(2) -0.132(18) -0.16(2) 0.16(2) F34 0.137(13) 0.25(2) 0.087(12) -0.090(13) 0.033(10) -0.100(15) F35 0.82(9) 0.099(16) 0.101(15) 0.057(14) -0.08(3) -0.05(3) F36 0.087(11) 0.100(9) 0.138(11) -0.070(9) -0.029(9) -0.011(8) P3' 0.103(6) 0.136(9) 0.158(9) -0.101(7) -0.078(6) 0.040(5) F31' 0.103(10) 0.098(8) 0.52(3) -0.131(14) -0.190(16) 0.060(7) F32' 0.064(11) 0.37(4) 0.35(4) -0.07(3) -0.075(14) 0.048(17) F33' 0.228(14) 0.120(10) 0.112(9) -0.079(7) -0.084(9) 0.051(10) F34' 0.36(3) 0.159(16) 0.104(12) -0.066(11) -0.107(15) 0.125(17) F35' 0.107(7) 0.163(10) 0.095(7) -0.066(7) -0.069(6) 0.031(6) F36' 0.154(15) 0.29(3) 0.216(18) -0.19(2) -0.011(11) 0.067(14) P4 0.047(3) 0.154(6) 0.049(3) -0.025(3) -0.008(2) 0.049(3) F41 0.060(6) 0.166(9) 0.141(9) -0.027(7) 0.003(6) 0.029(6) F42 0.075(6) 0.129(8) 0.127(9) -0.064(7) -0.022(6) 0.038(5) F43 0.064(6) 0.201(10) 0.100(7) -0.094(7) -0.020(5) 0.001(5) F44 0.083(7) 0.218(11) 0.076(6) -0.006(7) -0.043(5) 0.044(7) F45 0.053(5) 0.140(8) 0.062(5) -0.025(4) -0.004(4) 0.013(4) F46 0.067(5) 0.133(7) 0.134(7) -0.081(6) -0.060(5) 0.030(5) P4' 0.174(19) 0.31(3) 0.29(3) -0.16(2) -0.098(19) -0.08(2) F41' 0.13(3) 0.47(5) 0.34(4) -0.13(4) -0.06(3) -0.13(3) F42' 0.37(5) 0.45(6) 0.13(2) -0.09(3) -0.13(3) 0.05(4) F43' 0.14(3) 1.27(14) 0.14(2) -0.31(5) -0.04(2) 0.23(5) F44' 0.061(13) 0.38(4) 0.115(15) 0.015(19) -0.035(11) -0.081(17) F45' 0.32(4) 0.23(3) 0.33(5) -0.10(3) -0.23(4) 0.06(3) F46' 0.39(5) 0.51(6) 0.34(4) -0.30(5) -0.27(4) 0.38(5) C1 0.029 0.055 0.050 -0.027 -0.008 0.006 C2 0.039 0.053 0.040 -0.023 -0.012 0.000 C3 0.031 0.053 0.039 -0.021 -0.008 -0.001 C4 0.031 0.054 0.047 -0.024 -0.013 0.005 C5 0.035 0.056 0.042 -0.019 -0.015 -0.002 C6 0.037 0.052 0.047 -0.018 -0.020 -0.001 O7 0.044 0.057 0.051 -0.026 -0.022 0.006 C8 0.035 0.075 0.063 -0.037 -0.023 0.015 O9 0.043 0.062 0.047 -0.026 -0.024 0.013 C10 0.030 0.062 0.048 -0.034 -0.008 0.000 C11 0.030(3) 0.071(5) 0.040(3) -0.029(3) -0.013(3) 0.006(3) C13 0.034(3) 0.056(4) 0.037(3) -0.024(3) -0.012(3) 0.010(3) C14 0.029(3) 0.076(5) 0.038(3) -0.032(3) -0.012(3) 0.004(3) C15 0.033(3) 0.060(4) 0.036(3) -0.029(3) -0.012(3) 0.001(3) C16 0.033(3) 0.066(4) 0.035(3) -0.029(3) -0.006(3) -0.004(3) O17 0.045(2) 0.069(3) 0.043(2) -0.029(2) -0.019(2) -0.001(2) C18 0.045(4) 0.077(5) 0.041(4) -0.024(3) -0.015(3) -0.009(3) O19 0.052(2) 0.069(3) 0.048(2) -0.028(2) -0.021(2) -0.006(2) C20 0.040(3) 0.062(4) 0.043(4) -0.028(3) -0.016(3) 0.005(3) C21 0.038(3) 0.060(4) 0.045(4) -0.023(3) -0.013(3) 0.000(3) C22 0.041(4) 0.061(4) 0.050(4) -0.028(3) -0.020(3) 0.001(3) C23 0.038(3) 0.055(4) 0.044(4) -0.023(3) -0.018(3) 0.003(3) C24 0.037(3) 0.060(4) 0.049(4) -0.028(3) -0.018(3) 0.003(3) C25 0.039(3) 0.051(4) 0.042(4) -0.024(3) -0.015(3) 0.002(3) C26 0.042(4) 0.054(4) 0.046(4) -0.023(3) -0.016(3) -0.001(3) O27 0.043(2) 0.069(3) 0.041(2) -0.024(2) -0.0080(19) -0.005(2) C28 0.034(3) 0.070(4) 0.056(4) -0.035(3) -0.009(3) -0.001(3) O29 0.044(2) 0.073(3) 0.045(2) -0.032(2) -0.008(2) -0.006(2) C30 0.038(3) 0.060(4) 0.039(3) -0.022(3) -0.012(3) -0.001(3) C31 0.035(3) 0.065(4) 0.044(4) -0.031(3) -0.004(3) -0.003(3) C12 0.038(3) 0.068(4) 0.038(3) -0.031(3) -0.012(3) 0.013(3) C32 0.036(3) 0.067(4) 0.038(4) -0.022(3) -0.007(3) -0.013(3) C33 0.036(3) 0.064(4) 0.037(3) -0.029(3) -0.013(3) 0.000(3) C34 0.029(3) 0.070(4) 0.039(3) -0.031(3) -0.015(3) 0.005(3) C35 0.032(3) 0.065(4) 0.040(3) -0.030(3) -0.010(3) 0.000(3) C36 0.039(3) 0.063(4) 0.051(4) -0.036(3) -0.020(3) 0.011(3) O37 0.045(2) 0.065(3) 0.048(2) -0.031(2) -0.011(2) 0.005(2) C38 0.047(4) 0.067(4) 0.060(4) -0.035(4) -0.013(4) 0.013(3) O39 0.046(2) 0.068(3) 0.052(3) -0.033(2) -0.010(2) 0.005(2) C40 0.036(3) 0.068(4) 0.041(3) -0.030(3) -0.012(3) 0.004(3) C41 0.044(4) 0.070(5) 0.058(4) -0.032(4) -0.016(3) 0.006(3) N42 0.042(3) 0.064(4) 0.057(4) -0.032(3) -0.023(3) 0.012(3) C43 0.072(5) 0.064(5) 0.066(5) -0.028(4) -0.039(4) 0.008(4) C44 0.070(5) 0.076(5) 0.088(6) -0.048(5) -0.050(4) 0.017(4) C45 0.042(4) 0.072(5) 0.063(4) -0.038(4) -0.025(3) 0.013(3) C46 0.063(4) 0.072(5) 0.060(4) -0.030(4) -0.029(4) 0.010(4) C47 0.058(4) 0.068(5) 0.056(4) -0.033(4) -0.026(3) 0.007(4) C48 0.049(4) 0.060(5) 0.081(5) -0.037(4) -0.024(4) 0.009(3) C49 0.075(5) 0.078(6) 0.092(6) -0.046(5) -0.022(4) -0.002(4) C50 0.103(7) 0.086(7) 0.109(8) -0.056(6) -0.018(6) -0.012(5) N51 0.086(5) 0.071(5) 0.146(7) -0.053(5) -0.042(5) 0.007(4) C52 0.084(6) 0.082(7) 0.108(7) -0.022(6) -0.035(5) -0.006(5) C53 0.079(5) 0.070(5) 0.084(6) -0.033(5) -0.035(4) 0.004(4) C54 0.035(3) 0.083(5) 0.039(3) -0.033(3) -0.013(3) 0.004(3) N55 0.039(3) 0.056(3) 0.038(3) -0.024(3) -0.017(2) 0.008(2) C56 0.075(5) 0.063(5) 0.054(5) -0.025(4) -0.028(4) 0.000(4) C57 0.082(5) 0.055(4) 0.041(4) -0.020(3) -0.019(3) -0.005(3) C58 0.040(3) 0.065(4) 0.042(4) -0.024(4) -0.018(3) 0.007(3) C59 0.119(6) 0.058(5) 0.063(5) -0.029(4) -0.053(4) 0.008(4) C60 0.108(6) 0.060(5) 0.058(5) -0.016(4) -0.045(4) -0.009(4) C61 0.041(4) 0.076(5) 0.053(4) -0.038(4) -0.022(3) 0.010(3) C62 0.061(4) 0.096(6) 0.052(5) -0.039(4) -0.010(4) -0.004(4) C63 0.075(5) 0.121(7) 0.050(5) -0.036(5) -0.019(4) 0.009(5) N64 0.084(5) 0.124(6) 0.064(5) -0.052(5) -0.033(4) 0.019(4) C65 0.083(6) 0.110(7) 0.101(7) -0.075(6) -0.052(5) 0.030(5) C66 0.068(5) 0.082(5) 0.072(5) -0.040(4) -0.038(4) 0.020(4) C67 0.037(3) 0.062(4) 0.048(4) -0.021(3) -0.017(3) 0.000(3) N68 0.049(3) 0.063(4) 0.042(3) -0.026(3) -0.016(2) -0.005(2) C69 0.075(5) 0.067(5) 0.048(4) -0.018(4) -0.019(3) -0.012(4) C70 0.074(5) 0.078(6) 0.048(5) -0.032(4) -0.003(4) -0.018(4) C71 0.044(4) 0.068(5) 0.046(4) -0.022(4) -0.005(3) -0.011(3) C72 0.063(4) 0.069(5) 0.045(4) -0.025(4) -0.014(3) -0.010(4) C73 0.056(4) 0.066(5) 0.055(5) -0.034(4) -0.014(3) -0.002(3) C74 0.044(4) 0.069(5) 0.056(5) -0.029(4) -0.005(3) -0.014(3) N75 0.124(6) 0.066(5) 0.113(6) -0.042(5) -0.036(5) -0.011(4) C75 0.101(6) 0.075(6) 0.075(5) -0.037(5) -0.021(4) -0.012(5) C76 0.133(8) 0.073(7) 0.083(7) -0.034(5) -0.023(6) -0.017(5) C78 0.093(6) 0.079(6) 0.082(6) -0.014(5) -0.034(5) -0.014(5) C79 0.073(5) 0.077(6) 0.066(5) -0.029(4) -0.019(4) -0.008(4) C80 0.040(3) 0.070(4) 0.053(4) -0.032(3) -0.008(3) -0.002(3) N81 0.032(3) 0.066(4) 0.046(3) -0.027(3) 0.001(2) -0.003(3) C82 0.050(4) 0.073(5) 0.069(5) -0.037(4) -0.002(4) -0.010(4) C83 0.059(4) 0.072(5) 0.056(5) -0.019(4) 0.000(3) -0.007(4) C84 0.036(4) 0.077(5) 0.049(4) -0.020(4) -0.013(3) 0.006(3) C85 0.039(3) 0.071(5) 0.061(5) -0.031(4) -0.015(3) -0.002(3) C86 0.041(4) 0.063(4) 0.051(4) -0.026(3) -0.004(3) -0.008(3) C87 0.035(4) 0.105(6) 0.046(4) -0.026(4) -0.013(3) 0.004(4) C88 0.052(4) 0.114(6) 0.052(5) -0.014(5) -0.017(4) 0.004(4) C89 0.046(5) 0.183(11) 0.064(7) -0.001(7) -0.019(4) 0.004(6) N90 0.060(5) 0.210(10) 0.061(5) -0.037(6) -0.023(4) -0.001(6) C91 0.067(5) 0.170(9) 0.082(7) -0.065(7) -0.020(5) -0.002(6) C92 0.052(4) 0.135(7) 0.056(5) -0.051(5) -0.016(3) 0.006(4) C93 0.06(4) 0.08(2) 0.05(2) -0.006(17) -0.05(2) -0.04(2) C94 0.05(2) 0.07(4) 0.05(2) -0.05(3) -0.002(17) -0.02(2) C95 0.020(16) 0.09(3) 0.05(4) -0.05(3) 0.012(18) -0.016(17) C96 0.69(18) 0.17(6) 0.04(3) -0.03(3) 0.17(6) 0.05(7) C97 0.19(5) 0.10(3) 0.04(3) -0.02(2) 0.05(3) 0.04(3) C93' 0.019(8) 0.064(9) 0.047(10) -0.037(6) -0.013(7) 0.005(7) C94' 0.039(8) 0.071(17) 0.066(13) -0.047(13) -0.011(8) -0.003(11) C95' 0.077(17) 0.23(3) 0.053(15) -0.055(15) -0.009(12) 0.011(15) C96' 0.070(10) 0.21(2) 0.059(14) -0.047(12) -0.015(9) -0.045(11) C97' 0.19(2) 0.28(3) 0.106(15) 0.005(18) -0.063(16) -0.15(2) C98 0.039(3) 0.068(4) 0.048(4) -0.031(3) -0.016(3) 0.008(3) C99 0.041(3) 0.074(4) 0.060(4) -0.039(3) -0.015(3) 0.010(3) C100 0.044(4) 0.069(4) 0.072(5) -0.041(4) -0.017(3) 0.007(3) C101 0.043(4) 0.092(6) 0.076(5) -0.040(5) -0.006(4) -0.003(4) C102 0.064(5) 0.114(7) 0.079(6) -0.028(5) 0.004(4) 0.008(5) C103 0.043(3) 0.064(4) 0.051(4) -0.029(3) -0.017(3) 0.004(3) C104 0.038(4) 0.090(5) 0.068(5) -0.045(4) -0.025(3) 0.010(3) C105 0.068(7) 0.127(9) 0.048(7) -0.029(6) -0.030(6) 0.001(6) C106 0.073(10) 0.188(18) 0.077(12) -0.058(12) -0.040(9) 0.001(10) C107 0.124(12) 0.317(19) 0.050(7) 0.007(9) -0.055(7) -0.053(12) C113 0.07(10) 0.9(7) 0.21(18) -0.4(3) 0.11(11) -0.3(2) C114 0.01(5) 0.00(5) 0.05(9) 0.01(4) 0.01(5) -0.01(3) C115 0.06(6) 0.00(5) 0.4(2) 0.04(7) -0.17(10) 0.00(4) C108 0.043(3) 0.069(4) 0.040(3) -0.024(3) -0.013(3) -0.007(3) C109 0.045(4) 0.068(4) 0.050(4) -0.030(3) -0.017(3) -0.004(3) C110 0.048(4) 0.084(5) 0.067(4) -0.035(4) -0.025(3) -0.002(3) C111 0.059(4) 0.083(5) 0.073(5) -0.032(4) -0.034(4) -0.003(4) C112 0.068(5) 0.124(7) 0.086(6) -0.033(5) -0.042(4) 0.006(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 F16 1.598(6) . ? P1 F12 1.598(6) . ? P1 F13 1.598(6) . ? P1 F11 1.598(6) . ? P1 F15 1.598(6) . ? P1 F14 1.600(6) . ? F16 P1' 1.63(2) . ? P1' F13' 1.555(15) . ? P1' F15' 1.555(15) . ? P1' F11' 1.555(15) . ? P1' F12' 1.555(15) . ? P1' F14' 1.555(15) . ? P2 F26 1.564(5) . ? P2 F22 1.564(5) . ? P2 F21 1.564(5) . ? P2 F25 1.565(5) . ? P2 F24 1.565(5) . ? P2 F23 1.565(5) . ? P2' F23' 1.594(9) . ? P2' F26' 1.594(9) . ? P2' F22' 1.594(9) . ? P2' F24' 1.594(9) . ? P2' F21' 1.594(9) . ? P2' F25' 1.594(9) . ? P3 F31 1.474(8) . ? P3 F34 1.474(8) . ? P3 F35 1.475(8) . ? P3 F32 1.475(8) . ? P3 F36 1.475(8) . ? P3 F33 1.475(8) . ? P3' F31' 1.573(6) . ? P3' F32' 1.574(6) . ? P3' F36' 1.574(6) . ? P3' F33' 1.574(6) . ? P3' F34' 1.575(6) . ? P3' F35' 1.575(6) . ? P4 F46 1.573(5) . ? P4 F41 1.575(5) . ? P4 F45 1.576(5) . ? P4 F43 1.576(5) . ? P4 F42 1.576(5) . ? P4 F44 1.577(5) . ? P4' F41' 1.603(13) . ? P4' F46' 1.603(13) . ? P4' F42' 1.603(13) . ? P4' F43' 1.604(13) . ? P4' F44' 1.605(13) . ? P4' F45' 1.605(13) . ? C1 C6 1.3834 . ? C1 C2 1.3918 . ? C1 C41 1.513(5) . ? C2 O39 1.385(3) . ? C2 C3 1.4001 . ? C3 C4 1.3987 . ? C3 C40 1.506(5) . ? C4 C5 1.3978 . ? C5 C6 1.3989 . ? C5 C10 1.5299 . ? C6 O7 1.4024 . ? O7 C8 1.4134 . ? C8 O9 1.4282 . ? O9 C12 1.408(6) . ? C10 C93 1.33(7) . ? C10 C13 1.526(6) . ? C10 C93' 1.62(2) . ? C11 C16 1.384(7) . ? C11 C12 1.386(8) . ? C11 C54 1.510(7) . ? C13 C14 1.382(7) . ? C13 C12 1.398(7) . ? C14 C15 1.398(7) . ? C15 C16 1.392(7) . ? C15 C20 1.512(7) . ? C16 O17 1.393(6) . ? O17 C18 1.427(6) . ? C18 O19 1.408(6) . ? O19 C22 1.397(6) . ? C20 C98 1.525(7) . ? C20 C23 1.537(7) . ? C21 C22 1.393(7) . ? C21 C26 1.395(7) . ? C21 C67 1.517(7) . ? C22 C23 1.370(7) . ? C23 C24 1.408(7) . ? C24 C25 1.393(7) . ? C25 C26 1.378(7) . ? C25 C30 1.523(7) . ? C26 O27 1.401(6) . ? O27 C28 1.425(6) . ? C28 O29 1.413(6) . ? O29 C32 1.394(6) . ? C30 C33 1.526(7) . ? C30 C103 1.542(7) . ? C31 C32 1.380(7) . ? C31 C36 1.381(8) . ? C31 C80 1.510(7) . ? C32 C33 1.389(7) . ? C33 C34 1.382(7) . ? C34 C35 1.386(7) . ? C35 C36 1.394(7) . ? C35 C40 1.522(8) . ? C36 O37 1.404(6) . ? O37 C38 1.421(6) . ? C38 O39 1.421(7) . ? C40 C108 1.533(7) . ? C41 N42 1.476(7) . ? N42 C47 1.329(7) . ? N42 C43 1.343(7) . ? C43 C44 1.340(9) . ? C44 C45 1.383(8) . ? C45 C46 1.382(8) . ? C45 C48 1.476(9) . ? C46 C47 1.370(8) . ? C48 C53 1.381(9) . ? C48 C49 1.394(9) . ? C49 C50 1.346(10) . ? C50 N51 1.331(10) . ? N51 C52 1.328(10) . ? C52 C53 1.376(10) . ? C54 N55 1.493(6) . ? N55 C60 1.312(7) . ? N55 C56 1.317(7) . ? C56 C57 1.375(8) . ? C57 C58 1.352(8) . ? C58 C59 1.373(8) . ? C58 C61 1.490(8) . ? C59 C60 1.376(8) . ? C61 C62 1.385(8) . ? C61 C66 1.389(8) . ? C62 C63 1.374(9) . ? C63 N64 1.306(9) . ? N64 C65 1.313(9) . ? C65 C66 1.415(9) . ? C67 N68 1.477(7) . ? N68 C69 1.327(7) . ? N68 C73 1.341(7) . ? C69 C70 1.354(8) . ? C70 C71 1.404(8) . ? C71 C72 1.375(8) . ? C71 C74 1.476(8) . ? C72 C73 1.371(8) . ? C74 C79 1.369(8) . ? C74 C75 1.389(9) . ? N75 C76 1.308(9) . ? N75 C78 1.325(9) . ? C75 C76 1.354(10) . ? C78 C79 1.384(9) . ? C80 N81 1.480(7) . ? N81 C82 1.321(7) . ? N81 C86 1.343(7) . ? C82 C83 1.382(9) . ? C83 C84 1.380(9) . ? C84 C85 1.399(8) . ? C84 C87 1.465(9) . ? C85 C86 1.343(8) . ? C87 C88 1.367(9) . ? C87 C92 1.392(9) . ? C88 C89 1.392(12) . ? C89 N90 1.324(12) . ? N90 C91 1.306(11) . ? C91 C92 1.404(10) . ? C93 C94 1.65(14) . ? C94 C95 1.55(13) . ? C95 C96 1.72(8) . ? C96 C97 1.15(9) . ? C93' C94' 1.49(5) . ? C94' C95' 1.58(5) . ? C95' C96' 1.48(3) . ? C96' C97' 1.63(4) . ? C98 C99 1.515(7) . ? C99 C100 1.523(7) . ? C100 C101 1.511(8) . ? C101 C102 1.488(9) . ? C103 C104 1.522(8) . ? C104 C105 1.512(10) . ? C104 C113 1.512(14) . ? C105 C106 1.51(3) . ? C106 C107 1.53(2) . ? C113 C114 1.5(2) . ? C114 C115 1.7(2) . ? C108 C109 1.518(7) . ? C109 C110 1.523(8) . ? C110 C111 1.511(8) . ? C111 C112 1.509(9) . ? C201 C202 1.24(3) . ? O201 C202 1.62(4) . ? C202 C203 1.59(3) . ? O204 C205 1.208(14) . ? O204 C207 1.26(3) . ? C204 C205 1.48(2) . ? C204 C204 1.74(3) 2_864 ? C205 C206 1.427(16) . ? C206 C207 1.37(3) . ? C207 C208 1.63(3) . ? C209 O209 1.31(2) . ? C209 C210 1.54(2) . ? O210 C212 1.537(16) . ? O210 C213 1.537(13) . ? C211 O211 1.296(19) . ? C211 O212 1.58(8) . ? C212 C213 1.017(16) . ? C214 O215 1.816(19) . ? 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 F16 P1 F12 179.9(3) . . ? F16 P1 F13 89.5(4) . . ? F12 P1 F13 90.5(4) . . ? F16 P1 F11 89.5(4) . . ? F12 P1 F11 90.5(4) . . ? F13 P1 F11 179.0(7) . . ? F16 P1 F15 89.6(4) . . ? F12 P1 F15 90.5(4) . . ? F13 P1 F15 90.04(12) . . ? F11 P1 F15 90.02(12) . . ? F16 P1 F14 89.5(4) . . ? F12 P1 F14 90.4(4) . . ? F13 P1 F14 89.93(12) . . ? F11 P1 F14 89.99(12) . . ? F15 P1 F14 179.1(7) . . ? P1 F16 P1' 16.5(4) . . ? F13' P1' F15' 90.01(13) . . ? F13' P1' F11' 179.3(19) . . ? F15' P1' F11' 90.00(13) . . ? F13' P1' F12' 89.7(10) . . ? F15' P1' F12' 89.7(10) . . ? F11' P1' F12' 89.6(10) . . ? F13' P1' F14' 89.98(13) . . ? F15' P1' F14' 179.3(19) . . ? F11' P1' F14' 90.01(13) . . ? F12' P1' F14' 89.6(10) . . ? F13' P1' F16 90.4(10) . . ? F15' P1' F16 90.4(10) . . ? F11' P1' F16 90.3(10) . . ? F12' P1' F16 179.9(2) . . ? F14' P1' F16 90.3(10) . . ? F26 P2 F22 179.9(4) . . ? F26 P2 F21 89.8(4) . . ? F22 P2 F21 90.2(4) . . ? F26 P2 F25 89.8(4) . . ? F22 P2 F25 90.2(4) . . ? F21 P2 F25 179.6(8) . . ? F26 P2 F24 89.8(4) . . ? F22 P2 F24 90.3(4) . . ? F21 P2 F24 90.03(13) . . ? F25 P2 F24 90.04(13) . . ? F26 P2 F23 89.8(4) . . ? F22 P2 F23 90.2(4) . . ? F21 P2 F23 89.98(13) . . ? F25 P2 F23 89.93(13) . . ? F24 P2 F23 179.5(7) . . ? F23' P2' F26' 90.7(7) . . ? F23' P2' F22' 89.4(7) . . ? F26' P2' F22' 179.9(4) . . ? F23' P2' F24' 178.7(16) . . ? F26' P2' F24' 90.6(7) . . ? F22' P2' F24' 89.3(8) . . ? F23' P2' F21' 90.02(13) . . ? F26' P2' F21' 90.6(7) . . ? F22' P2' F21' 89.4(7) . . ? F24' P2' F21' 89.96(13) . . ? F23' P2' F25' 89.99(13) . . ? F26' P2' F25' 90.6(7) . . ? F22' P2' F25' 89.4(7) . . ? F24' P2' F25' 89.99(13) . . ? F21' P2' F25' 178.8(15) . . ? F31 P3 F34 89.63(18) . . ? F31 P3 F35 89.66(18) . . ? F34 P3 F35 170.9(15) . . ? F31 P3 F32 170.9(15) . . ? F34 P3 F32 89.64(18) . . ? F35 P3 F32 89.62(18) . . ? F31 P3 F36 94.6(7) . . ? F34 P3 F36 94.6(7) . . ? F35 P3 F36 94.5(7) . . ? F32 P3 F36 94.5(7) . . ? F31 P3 F33 85.5(7) . . ? F34 P3 F33 85.4(7) . . ? F35 P3 F33 85.4(7) . . ? F32 P3 F33 85.4(7) . . ? F36 P3 F33 179.9(2) . . ? F31' P3' F32' 170.8(12) . . ? F31' P3' F36' 82.7(8) . . ? F32' P3' F36' 88.1(6) . . ? F31' P3' F33' 89.4(10) . . ? F32' P3' F33' 99.8(11) . . ? F36' P3' F33' 171.1(9) . . ? F31' P3' F34' 89.88(14) . . ? F32' P3' F34' 89.84(14) . . ? F36' P3' F34' 88.0(5) . . ? F33' P3' F34' 96.1(10) . . ? F31' P3' F35' 89.82(14) . . ? F32' P3' F35' 89.81(14) . . ? F36' P3' F35' 88.0(5) . . ? F33' P3' F35' 87.9(7) . . ? F34' P3' F35' 176.0(11) . . ? F46 P4 F41 89.0(2) . . ? F46 P4 F45 89.0(2) . . ? F41 P4 F45 178.0(4) . . ? F46 P4 F43 88.9(2) . . ? F41 P4 F43 89.97(12) . . ? F45 P4 F43 90.02(13) . . ? F46 P4 F42 88.9(2) . . ? F41 P4 F42 89.98(13) . . ? F45 P4 F42 89.96(12) . . ? F43 P4 F42 177.9(4) . . ? F46 P4 F44 180.0(2) . . ? F41 P4 F44 91.0(2) . . ? F45 P4 F44 91.0(2) . . ? F43 P4 F44 91.1(2) . . ? F42 P4 F44 91.0(2) . . ? F41' P4' F46' 93.7(8) . . ? F41' P4' F42' 89.82(16) . . ? F46' P4' F42' 93.7(8) . . ? F41' P4' F43' 89.81(16) . . ? F46' P4' F43' 93.6(8) . . ? F42' P4' F43' 172.7(16) . . ? F41' P4' F44' 86.4(8) . . ? F46' P4' F44' 179.88(18) . . ? F42' P4' F44' 86.4(8) . . ? F43' P4' F44' 86.3(8) . . ? F41' P4' F45' 172.7(16) . . ? F46' P4' F45' 93.6(8) . . ? F42' P4' F45' 89.74(16) . . ? F43' P4' F45' 89.70(16) . . ? F44' P4' F45' 86.3(8) . . ? C6 C1 C2 117.9 . . ? C6 C1 C41 120.0(2) . . ? C2 C1 C41 122.1(2) . . ? O39 C2 C1 117.28(15) . . ? O39 C2 C3 119.73(15) . . ? C1 C2 C3 122.8 . . ? C4 C3 C2 116.6 . . ? C4 C3 C40 123.4(2) . . ? C2 C3 C40 119.9(2) . . ? C5 C4 C3 123.0 . . ? C4 C5 C6 117.2 . . ? C4 C5 C10 123.5 . . ? C6 C5 C10 119.2 . . ? C1 C6 C5 122.5 . . ? C1 C6 O7 118.2 . . ? C5 C6 O7 119.1 . . ? C6 O7 C8 116.7 . . ? O7 C8 O9 113.6 . . ? C12 O9 C8 117.4(2) . . ? C93 C10 C13 108(3) . . ? C93 C10 C5 120(3) . . ? C13 C10 C5 106.70(18) . . ? C93 C10 C93' 10(3) . . ? C13 C10 C93' 115.3(9) . . ? C5 C10 C93' 110.1(8) . . ? C16 C11 C12 118.0(5) . . ? C16 C11 C54 120.6(6) . . ? C12 C11 C54 121.3(5) . . ? C14 C13 C12 116.8(5) . . ? C14 C13 C10 124.0(4) . . ? C12 C13 C10 119.1(5) . . ? C13 C14 C15 123.7(5) . . ? C16 C15 C14 116.4(5) . . ? C16 C15 C20 120.8(5) . . ? C14 C15 C20 122.7(5) . . ? C11 C16 C15 122.7(5) . . ? C11 C16 O17 117.5(5) . . ? C15 C16 O17 119.7(5) . . ? C16 O17 C18 118.4(4) . . ? O19 C18 O17 113.8(4) . . ? C22 O19 C18 115.4(4) . . ? C15 C20 C98 114.7(5) . . ? C15 C20 C23 107.1(4) . . ? C98 C20 C23 114.9(4) . . ? C22 C21 C26 118.1(5) . . ? C22 C21 C67 120.8(5) . . ? C26 C21 C67 121.0(5) . . ? C23 C22 C21 122.4(5) . . ? C23 C22 O19 119.9(5) . . ? C21 C22 O19 117.6(5) . . ? C22 C23 C24 117.7(5) . . ? C22 C23 C20 120.5(5) . . ? C24 C23 C20 121.8(5) . . ? C25 C24 C23 121.8(5) . . ? C26 C25 C24 118.1(5) . . ? C26 C25 C30 119.7(5) . . ? C24 C25 C30 122.1(5) . . ? C25 C26 C21 121.8(5) . . ? C25 C26 O27 120.4(5) . . ? C21 C26 O27 117.6(5) . . ? C26 O27 C28 116.3(4) . . ? O29 C28 O27 112.9(4) . . ? C32 O29 C28 116.3(4) . . ? C25 C30 C33 107.9(4) . . ? C25 C30 C103 114.0(4) . . ? C33 C30 C103 113.9(5) . . ? C32 C31 C36 118.4(5) . . ? C32 C31 C80 121.1(5) . . ? C36 C31 C80 120.4(5) . . ? C11 C12 C13 122.4(5) . . ? C11 C12 O9 117.9(5) . . ? C13 C12 O9 119.6(5) . . ? C31 C32 C33 122.3(5) . . ? C31 C32 O29 117.6(5) . . ? C33 C32 O29 120.0(5) . . ? C34 C33 C32 117.0(5) . . ? C34 C33 C30 122.0(5) . . ? C32 C33 C30 121.0(5) . . ? C33 C34 C35 123.3(5) . . ? C34 C35 C36 117.1(5) . . ? C34 C35 C40 121.9(5) . . ? C36 C35 C40 121.0(5) . . ? C31 C36 C35 121.9(5) . . ? C31 C36 O37 118.2(5) . . ? C35 C36 O37 119.8(5) . . ? C36 O37 C38 116.7(4) . . ? O37 C38 O39 113.9(5) . . ? C2 O39 C38 115.2(4) . . ? C3 C40 C35 108.0(4) . . ? C3 C40 C108 114.8(4) . . ? C35 C40 C108 113.6(5) . . ? N42 C41 C1 110.9(4) . . ? C47 N42 C43 119.2(6) . . ? C47 N42 C41 121.5(5) . . ? C43 N42 C41 119.3(5) . . ? C44 C43 N42 120.6(6) . . ? C43 C44 C45 122.8(6) . . ? C46 C45 C44 115.0(6) . . ? C46 C45 C48 122.7(6) . . ? C44 C45 C48 122.3(6) . . ? C47 C46 C45 121.1(6) . . ? N42 C47 C46 121.2(6) . . ? C53 C48 C49 116.1(7) . . ? C53 C48 C45 122.5(6) . . ? C49 C48 C45 121.4(7) . . ? C50 C49 C48 120.5(8) . . ? N51 C50 C49 123.9(8) . . ? C52 N51 C50 116.2(7) . . ? N51 C52 C53 124.0(8) . . ? C52 C53 C48 119.4(7) . . ? N55 C54 C11 110.8(4) . . ? C60 N55 C56 119.0(5) . . ? C60 N55 C54 120.9(5) . . ? C56 N55 C54 120.1(5) . . ? N55 C56 C57 122.1(6) . . ? C58 C57 C56 120.5(6) . . ? C57 C58 C59 116.2(5) . . ? C57 C58 C61 121.2(6) . . ? C59 C58 C61 122.5(6) . . ? C58 C59 C60 121.3(6) . . ? N55 C60 C59 120.8(6) . . ? C62 C61 C66 117.7(6) . . ? C62 C61 C58 121.5(6) . . ? C66 C61 C58 120.7(6) . . ? C63 C62 C61 118.5(7) . . ? N64 C63 C62 125.7(8) . . ? C63 N64 C65 116.1(7) . . ? N64 C65 C66 124.4(8) . . ? C61 C66 C65 117.5(7) . . ? N68 C67 C21 109.1(4) . . ? C69 N68 C73 119.3(5) . . ? C69 N68 C67 120.4(5) . . ? C73 N68 C67 120.2(5) . . ? N68 C69 C70 121.6(6) . . ? C69 C70 C71 121.3(6) . . ? C72 C71 C70 115.2(6) . . ? C72 C71 C74 122.4(6) . . ? C70 C71 C74 122.4(6) . . ? C73 C72 C71 121.6(6) . . ? N68 C73 C72 120.9(6) . . ? C79 C74 C75 114.6(7) . . ? C79 C74 C71 122.3(6) . . ? C75 C74 C71 123.1(6) . . ? C76 N75 C78 115.4(7) . . ? C76 C75 C74 120.8(7) . . ? N75 C76 C75 124.9(8) . . ? N75 C78 C79 123.7(8) . . ? C74 C79 C78 120.6(7) . . ? N81 C80 C31 112.2(5) . . ? C82 N81 C86 119.6(5) . . ? C82 N81 C80 120.6(6) . . ? C86 N81 C80 119.8(5) . . ? N81 C82 C83 121.9(6) . . ? C84 C83 C82 119.6(6) . . ? C83 C84 C85 116.4(6) . . ? C83 C84 C87 122.4(6) . . ? C85 C84 C87 121.2(7) . . ? C86 C85 C84 121.4(6) . . ? N81 C86 C85 121.0(6) . . ? C88 C87 C92 116.7(7) . . ? C88 C87 C84 122.7(8) . . ? C92 C87 C84 120.6(6) . . ? C87 C88 C89 119.9(9) . . ? N90 C89 C88 123.8(9) . . ? C91 N90 C89 116.6(9) . . ? N90 C91 C92 124.2(10) . . ? C87 C92 C91 118.8(8) . . ? C10 C93 C94 126(5) . . ? C95 C94 C93 99(6) . . ? C94 C95 C96 107(5) . . ? C97 C96 C95 113(6) . . ? C94' C93' C10 109(2) . . ? C93' C94' C95' 119(3) . . ? C96' C95' C94' 114(3) . . ? C95' C96' C97' 109(2) . . ? C99 C98 C20 112.8(4) . . ? C98 C99 C100 113.1(5) . . ? C101 C100 C99 114.4(5) . . ? C102 C101 C100 113.6(6) . . ? C104 C103 C30 113.7(4) . . ? C105 C104 C113 7(7) . . ? C105 C104 C103 114.0(7) . . ? C113 C104 C103 113(4) . . ? C106 C105 C104 114.1(11) . . ? C105 C106 C107 110.9(16) . . ? C114 C113 C104 123(8) . . ? C113 C114 C115 136(10) . . ? C109 C108 C40 113.5(4) . . ? C108 C109 C110 113.0(4) . . ? C111 C110 C109 113.5(5) . . ? C112 C111 C110 115.6(6) . . ? C201 C202 C203 120(3) . . ? C201 C202 O201 113(3) . . ? C203 C202 O201 103(2) . . ? C205 O204 C207 49.1(12) . . ? C205 C204 C204 159.3(18) . 2_864 ? O204 C205 C206 119.3(13) . . ? O204 C205 C204 115.4(13) . . ? C206 C205 C204 124.8(13) . . ? C207 C206 C205 43.0(12) . . ? O204 C207 C206 120(2) . . ? O204 C207 C208 129(2) . . ? C206 C207 C208 110(2) . . ? O209 C209 C210 142(2) . . ? C212 O210 C213 38.6(6) . . ? O211 C211 O212 98(4) . . ? C213 C212 O210 70.7(12) . . ? C212 C213 O210 70.7(12) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.519 _refine_diff_density_min -0.538 _refine_diff_density_rms 0.113