# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_ic14788 _database_code_depnum_ccdc_archive 'CCDC 879620' #TrackingRef 'ic14788-revised-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H111 F12 N3 O18 P2' _chemical_formula_weight 1740.70 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' _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 27.0161(3) _cell_length_b 15.12550(10) _cell_length_c 24.3838(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.059(2) _cell_angle_gamma 90.00 _cell_volume 9026.11(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 21649 _cell_measurement_theta_min 3.2105 _cell_measurement_theta_max 76.9595 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3672 _exptl_absorpt_coefficient_mu 1.212 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.81488 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini A' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49844 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 67.99 _reflns_number_total 16439 _reflns_number_gt 12992 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.1000P)^2^+48.0000P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16439 _refine_ls_number_parameters 1176 _refine_ls_number_restraints 297 _refine_ls_R_factor_all 0.1745 _refine_ls_R_factor_gt 0.1497 _refine_ls_wR_factor_ref 0.3669 _refine_ls_wR_factor_gt 0.3483 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.182 _refine_ls_shift/su_max 0.047 _refine_ls_shift/su_mean 0.002 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 O1 O 0.11114(16) 0.3083(3) 0.37069(18) 0.0414(9) Uani 1 1 d . . . O2 O 0.1332(3) 0.1597(5) 0.4526(4) 0.097(2) Uani 1 1 d . . . O3 O 0.1277(3) -0.0022(4) 0.3997(4) 0.112(2) Uani 1 1 d U . . O4 O 0.1628(2) -0.1032(4) 0.3279(2) 0.0771(19) Uani 1 1 d . . . O5 O 0.04352(16) 0.2832(3) 0.26209(18) 0.0390(9) Uani 1 1 d . . . O6 O 0.00271(19) 0.1139(3) 0.2214(2) 0.0519(11) Uani 1 1 d . . . O7 O 0.01289(18) -0.0259(3) 0.1410(2) 0.0515(11) Uani 1 1 d . . . O8 O 0.10343(18) -0.1319(3) 0.2149(2) 0.0534(11) Uani 1 1 d . . . O9 O 0.35903(18) 0.4397(3) 0.2387(3) 0.0615(13) Uani 1 1 d . . . O10 O 0.4712(2) 0.3961(4) 0.2938(4) 0.099(3) Uani 1 1 d . . . O11 O 0.49726(18) 0.2146(4) 0.3052(3) 0.0668(15) Uani 1 1 d . . . O12 O 0.4310(2) 0.0627(4) 0.2456(3) 0.0694(15) Uani 1 1 d . . . O13 O 0.28486(18) 0.4218(3) 0.1242(2) 0.0502(11) Uani 1 1 d . . . O14 O 0.2849(2) 0.3127(4) 0.0262(2) 0.0691(15) Uani 1 1 d . . . O15 O 0.3492(4) 0.1530(5) 0.0366(3) 0.115(3) Uani 1 1 d . . . O16 O 0.3679(2) 0.0382(3) 0.1315(3) 0.0675(14) Uani 1 1 d . . . O17 O 0.3728(2) 0.1864(4) 0.3549(3) 0.0787(18) Uani 1 1 d . . . N1 N 0.1194(3) 0.0751(4) 0.2541(3) 0.0689(19) Uani 1 1 d . . . H1A H 0.0833 0.0923 0.2377 0.083 Uiso 1 1 calc R . . H1B H 0.1209 0.0189 0.2693 0.083 Uiso 1 1 calc R . . N2 N 0.3439(2) 0.2343(4) 0.1421(2) 0.0480(13) Uani 1 1 d . . . H2A H 0.3249 0.2731 0.1112 0.058 Uiso 1 1 calc R A 1 H2B H 0.3488 0.1829 0.1247 0.058 Uiso 1 1 calc R A 1 C1 C 0.1206(2) 0.3583(4) 0.3296(3) 0.0362(12) Uani 1 1 d . . . C2 C 0.0826(2) 0.3453(3) 0.2691(3) 0.0336(11) Uani 1 1 d . . . C3 C 0.0866(2) 0.3927(4) 0.2228(3) 0.0359(12) Uani 1 1 d . . . H3A H 0.0603 0.3843 0.1823 0.043 Uiso 1 1 calc R . . C4 C 0.1289(2) 0.4527(4) 0.2351(3) 0.0373(12) Uani 1 1 d . . . C5 C 0.1381(2) 0.5094(4) 0.1890(3) 0.0438(14) Uani 1 1 d . . . C6 C 0.1963(2) 0.4904(4) 0.1979(3) 0.0419(13) Uani 1 1 d . . . C7 C 0.2120(3) 0.4644(4) 0.1527(3) 0.0439(14) Uani 1 1 d . . . H7A H 0.1851 0.4574 0.1123 0.053 Uiso 1 1 calc R . . C8 C 0.2663(3) 0.4488(4) 0.1663(3) 0.0447(14) Uani 1 1 d . . . C9 C 0.3053(3) 0.4593(4) 0.2259(3) 0.0473(15) Uani 1 1 d . . . C10 C 0.2900(2) 0.4857(4) 0.2716(3) 0.0455(14) Uani 1 1 d . . . H10A H 0.3169 0.4928 0.3119 0.055 Uiso 1 1 calc R . . C11 C 0.2353(2) 0.5014(4) 0.2574(3) 0.0435(14) Uani 1 1 d . . . C12 C 0.2123(3) 0.5314(4) 0.3018(3) 0.0460(14) Uani 1 1 d . . . C13 C 0.1676(2) 0.4648(4) 0.2950(3) 0.0388(13) Uani 1 1 d . . . C14 C 0.1628(2) 0.4186(4) 0.3421(3) 0.0387(12) Uani 1 1 d . . . H14A H 0.1885 0.4283 0.3827 0.046 Uiso 1 1 calc R . . C15 C 0.1385(3) 0.6069(4) 0.2102(3) 0.0529(17) Uani 1 1 d . . . H15A H 0.1464 0.6471 0.1828 0.063 Uiso 1 1 calc R . . H15B H 0.1020 0.6221 0.2077 0.063 Uiso 1 1 calc R . . C16 C 0.1812(3) 0.6201(4) 0.2747(4) 0.0541(17) Uani 1 1 d . . . H16A H 0.1632 0.6415 0.3002 0.065 Uiso 1 1 calc R . . H16B H 0.2078 0.6656 0.2753 0.065 Uiso 1 1 calc R . . C17 C 0.0954(3) 0.4966(5) 0.1241(3) 0.0527(16) Uani 1 1 d . . . H17A H 0.0961 0.4350 0.1119 0.079 Uiso 1 1 calc R . . H17B H 0.1037 0.5358 0.0971 0.079 Uiso 1 1 calc R . . H17C H 0.0591 0.5106 0.1216 0.079 Uiso 1 1 calc R . . C18 C 0.2551(3) 0.5441(5) 0.3662(3) 0.0572(18) Uani 1 1 d . . . H18A H 0.2737 0.4879 0.3819 0.086 Uiso 1 1 calc R . . H18B H 0.2373 0.5644 0.3916 0.086 Uiso 1 1 calc R . . H18C H 0.2818 0.5883 0.3667 0.086 Uiso 1 1 calc R . . C19 C 0.1518(3) 0.3080(6) 0.4319(3) 0.0570(18) Uani 1 1 d . . . H19A H 0.1574 0.3687 0.4487 0.068 Uiso 1 1 calc R . . H19B H 0.1869 0.2859 0.4337 0.068 Uiso 1 1 calc R . . C20 C 0.1319(4) 0.2492(7) 0.4671(4) 0.080(3) Uani 1 1 d . . . H20A H 0.1548 0.2579 0.5108 0.096 Uiso 1 1 calc R . . H20B H 0.0939 0.2657 0.4588 0.096 Uiso 1 1 calc R . . C21 C 0.0854(4) 0.1232(8) 0.4199(5) 0.095(3) Uani 1 1 d . . . H21A H 0.0723 0.1429 0.3773 0.113 Uiso 1 1 calc R . . H21B H 0.0586 0.1429 0.4351 0.113 Uiso 1 1 calc R . . C22 C 0.0888(5) 0.0297(7) 0.4222(6) 0.110(3) Uani 1 1 d U . . H22A H 0.0523 0.0043 0.3975 0.132 Uiso 1 1 calc R . . H22B H 0.1004 0.0098 0.4645 0.132 Uiso 1 1 calc R . . C23 C 0.1429(5) -0.0877(6) 0.4117(6) 0.095(3) Uani 1 1 d U . . H23A H 0.1103 -0.1258 0.3919 0.114 Uiso 1 1 calc R . . H23B H 0.1575 -0.0976 0.4559 0.114 Uiso 1 1 calc R . . C24 C 0.1842(4) -0.1137(6) 0.3910(4) 0.080(3) Uani 1 1 d . . . H24A H 0.2172 -0.0766 0.4108 0.096 Uiso 1 1 calc R . . H24B H 0.1947 -0.1762 0.4018 0.096 Uiso 1 1 calc R . . C25 C 0.0035(2) 0.2685(4) 0.2017(3) 0.0446(14) Uani 1 1 d . . . H25A H 0.0214 0.2551 0.1747 0.054 Uiso 1 1 calc R . . H25B H -0.0196 0.3217 0.1862 0.054 Uiso 1 1 calc R . . C26 C -0.0306(3) 0.1914(5) 0.2042(3) 0.0521(16) Uani 1 1 d . . . H26A H -0.0457 0.2034 0.2340 0.063 Uiso 1 1 calc R . . H26B H -0.0614 0.1825 0.1641 0.063 Uiso 1 1 calc R . . C27 C -0.0292(3) 0.0343(5) 0.2022(3) 0.0575(18) Uani 1 1 d . . . H27A H -0.0653 0.0433 0.2026 0.069 Uiso 1 1 calc R . . H27B H -0.0104 -0.0145 0.2304 0.069 Uiso 1 1 calc R . . C28 C -0.0365(3) 0.0105(5) 0.1392(3) 0.0532(16) Uani 1 1 d . . . H28A H -0.0665 -0.0331 0.1214 0.064 Uiso 1 1 calc R . . H28B H -0.0466 0.0640 0.1133 0.064 Uiso 1 1 calc R . . C29 C 0.0122(3) -0.1195(4) 0.1414(3) 0.0505(16) Uani 1 1 d . . . H29A H -0.0148 -0.1419 0.1019 0.061 Uiso 1 1 calc R . . H29B H 0.0018 -0.1411 0.1734 0.061 Uiso 1 1 calc R . . C30 C 0.0684(3) -0.1522(5) 0.1531(3) 0.0508(15) Uani 1 1 d . . . H30A H 0.0677 -0.2168 0.1462 0.061 Uiso 1 1 calc R . . H30B H 0.0816 -0.1226 0.1256 0.061 Uiso 1 1 calc R . . C31 C 0.1903(3) -0.1347(4) 0.2951(3) 0.0500(15) Uani 1 1 d . . . C32 C 0.2463(3) -0.1473(4) 0.3189(3) 0.0496(16) Uani 1 1 d . . . H32A H 0.2680 -0.1399 0.3611 0.060 Uiso 1 1 calc R . . C33 C 0.2702(3) -0.1708(4) 0.2810(3) 0.0479(15) Uani 1 1 d . . . C34 C 0.3316(3) -0.1804(4) 0.2995(3) 0.0545(17) Uani 1 1 d . . . C35 C 0.3442(3) -0.1195(4) 0.2573(3) 0.0513(16) Uani 1 1 d . . . C36 C 0.3838(3) -0.0544(4) 0.2755(4) 0.0554(17) Uani 1 1 d . . . H36A H 0.4058 -0.0450 0.3174 0.066 Uiso 1 1 calc R . . C37 C 0.3914(3) -0.0029(5) 0.2330(4) 0.0554(18) Uani 1 1 d . . . C38 C 0.3586(3) -0.0160(4) 0.1720(4) 0.0557(18) Uani 1 1 d . . . C39 C 0.3183(3) -0.0816(4) 0.1527(3) 0.0505(15) Uani 1 1 d . . . H39A H 0.2961 -0.0908 0.1108 0.061 Uiso 1 1 calc R . . C40 C 0.3117(3) -0.1327(4) 0.1963(3) 0.0495(15) Uani 1 1 d . . . C41 C 0.2695(3) -0.2073(4) 0.1823(3) 0.0530(16) Uani 1 1 d . . . C42 C 0.2379(3) -0.1841(4) 0.2191(3) 0.0455(14) Uani 1 1 d . . . C43 C 0.1816(3) -0.1746(4) 0.1955(3) 0.0450(14) Uani 1 1 d . . . H43A H 0.1596 -0.1858 0.1539 0.054 Uiso 1 1 calc R . . C44 C 0.1580(3) -0.1485(4) 0.2332(3) 0.0442(14) Uani 1 1 d . . . C45 C 0.3395(3) -0.2766(5) 0.2798(4) 0.0624(19) Uani 1 1 d . . . H45A H 0.3783 -0.2855 0.2880 0.075 Uiso 1 1 calc R . . H45B H 0.3300 -0.3203 0.3040 0.075 Uiso 1 1 calc R . . C46 C 0.3036(4) -0.2916(4) 0.2126(4) 0.064(2) Uani 1 1 d . . . H46A H 0.2785 -0.3417 0.2078 0.076 Uiso 1 1 calc R . . H46B H 0.3269 -0.3075 0.1919 0.076 Uiso 1 1 calc R . . C47 C 0.3669(3) -0.1676(5) 0.3665(4) 0.066(2) Uani 1 1 d . . . H47A H 0.3616 -0.1077 0.3783 0.099 Uiso 1 1 calc R . . H47B H 0.4054 -0.1761 0.3748 0.099 Uiso 1 1 calc R . . H47C H 0.3564 -0.2109 0.3896 0.099 Uiso 1 1 calc R . . C48 C 0.2338(3) -0.2220(5) 0.1157(3) 0.0622(19) Uani 1 1 d . . . H48A H 0.2131 -0.1681 0.0982 0.093 Uiso 1 1 calc R . . H48B H 0.2084 -0.2707 0.1111 0.093 Uiso 1 1 calc R . . H48C H 0.2567 -0.2369 0.0949 0.093 Uiso 1 1 calc R . . C49 C 0.3995(4) 0.4977(6) 0.2725(7) 0.117(5) Uani 1 1 d . . . H49A H 0.3965 0.5496 0.2465 0.141 Uiso 1 1 calc R . . H49B H 0.3909 0.5187 0.3059 0.141 Uiso 1 1 calc R . . C50 C 0.4523(4) 0.4730(5) 0.2972(6) 0.104(4) Uani 1 1 d . . . H50A H 0.4711 0.5151 0.2814 0.125 Uiso 1 1 calc R . . H50B H 0.4659 0.4858 0.3410 0.125 Uiso 1 1 calc R . . C51 C 0.5200(3) 0.3659(6) 0.3153(7) 0.121(5) Uani 1 1 d . . . H51A H 0.5369 0.3852 0.3582 0.145 Uiso 1 1 calc R . . H51B H 0.5386 0.3998 0.2948 0.145 Uiso 1 1 calc R . . C52 C 0.5365(3) 0.2804(6) 0.3160(6) 0.093(3) Uani 1 1 d . . . H52A H 0.5670 0.2689 0.3561 0.112 Uiso 1 1 calc R . . H52B H 0.5513 0.2745 0.2853 0.112 Uiso 1 1 calc R . . C53 C 0.5149(3) 0.1298(6) 0.3108(6) 0.110(5) Uani 1 1 d . . . H53A H 0.5473 0.1227 0.3500 0.132 Uiso 1 1 calc R . . H53B H 0.5262 0.1162 0.2780 0.132 Uiso 1 1 calc R . . C54 C 0.4714(3) 0.0661(6) 0.3080(5) 0.089(3) Uani 1 1 d . . . H54A H 0.4874 0.0067 0.3215 0.107 Uiso 1 1 calc R . . H54B H 0.4543 0.0862 0.3346 0.107 Uiso 1 1 calc R . . C55 C 0.2462(3) 0.4303(6) 0.0609(3) 0.0631(19) Uani 1 1 d . . . H55A H 0.2338 0.4924 0.0519 0.076 Uiso 1 1 calc R . . H55B H 0.2138 0.3926 0.0526 0.076 Uiso 1 1 calc R . . C56 C 0.2739(4) 0.4021(6) 0.0217(4) 0.072(2) Uani 1 1 d . . . H56A H 0.2502 0.4170 -0.0210 0.086 Uiso 1 1 calc R . . H56B H 0.3086 0.4352 0.0339 0.086 Uiso 1 1 calc R . . C57 C 0.3033(4) 0.2793(7) -0.0180(3) 0.082(3) Uani 1 1 d . . . H57A H 0.3393 0.3050 -0.0108 0.098 Uiso 1 1 calc R . . H57B H 0.2768 0.2948 -0.0595 0.098 Uiso 1 1 calc R . . C58 C 0.3077(4) 0.1795(7) -0.0099(6) 0.096(4) Uani 1 1 d . . . H58A H 0.2743 0.1575 -0.0072 0.115 Uiso 1 1 calc R . . H58B H 0.3089 0.1528 -0.0464 0.115 Uiso 1 1 calc R . . C59 C 0.3658(8) 0.0679(7) 0.0358(7) 0.143(6) Uani 1 1 d . . . H59A H 0.4062 0.0654 0.0543 0.172 Uiso 1 1 calc R . . H59B H 0.3523 0.0473 -0.0066 0.172 Uiso 1 1 calc R . . C60 C 0.3452(6) 0.0101(7) 0.0689(5) 0.112(5) Uani 1 1 d . . . H60A H 0.3048 0.0131 0.0513 0.135 Uiso 1 1 calc R . . H60B H 0.3559 -0.0518 0.0663 0.135 Uiso 1 1 calc R . . C61 C 0.3938(4) 0.2710(6) 0.3521(5) 0.078(2) Uani 1 1 d . . . H61A H 0.4328 0.2660 0.3615 0.118 Uiso 1 1 calc R . . H61B H 0.3892 0.3101 0.3816 0.118 Uiso 1 1 calc R . . H61C H 0.3741 0.2954 0.3113 0.118 Uiso 1 1 calc R . . C62 C 0.3187(3) 0.1798(5) 0.3419(4) 0.0577(18) Uani 1 1 d . . . C63 C 0.3009(3) 0.0957(5) 0.3485(5) 0.074(3) Uani 1 1 d . . . H63A H 0.3259 0.0477 0.3608 0.089 Uiso 1 1 calc R . . C64 C 0.2474(3) 0.0822(5) 0.3373(4) 0.064(2) Uani 1 1 d . . . H64A H 0.2361 0.0250 0.3432 0.077 Uiso 1 1 calc R . . C65 C 0.2093(3) 0.1497(4) 0.3175(3) 0.0483(15) Uani 1 1 d . . . C66 C 0.2275(3) 0.2324(4) 0.3106(3) 0.0471(15) Uani 1 1 d . . . H66A H 0.2023 0.2801 0.2973 0.057 Uiso 1 1 calc R . . C67 C 0.2815(3) 0.2475(4) 0.3227(3) 0.0516(16) Uani 1 1 d . . . H67A H 0.2930 0.3050 0.3176 0.062 Uiso 1 1 calc R . . C68 C 0.1504(3) 0.1350(5) 0.3057(3) 0.0537(17) Uani 1 1 d . . . H68A H 0.1493 0.1103 0.3428 0.064 Uiso 1 1 calc R . . H68B H 0.1316 0.1930 0.2978 0.064 Uiso 1 1 calc R . . C69 C 0.1374(4) 0.0702(7) 0.2042(5) 0.085(3) Uani 1 1 d . . . H69A H 0.1774 0.0614 0.2210 0.102 Uiso 1 1 calc R . . H69B H 0.1192 0.0202 0.1769 0.102 Uiso 1 1 calc R . . C70 C 0.1227(4) 0.1506(7) 0.1724(4) 0.090(3) Uani 1 1 d . . . H70A H 0.1318 0.2011 0.2009 0.108 Uiso 1 1 calc R . . H70B H 0.0831 0.1520 0.1458 0.108 Uiso 1 1 calc R . . C71 C 0.1597(4) 0.1550(10) 0.1310(5) 0.118(5) Uani 1 1 d . . . H71A H 0.1579 0.0970 0.1115 0.142 Uiso 1 1 calc R . . H71B H 0.1435 0.1998 0.0986 0.142 Uiso 1 1 calc R . . C72 C 0.2185(4) 0.1782(9) 0.1696(4) 0.096(4) Uani 1 1 d . B . H72A H 0.2346 0.1326 0.2014 0.115 Uiso 1 1 calc R . . H72B H 0.2199 0.2353 0.1900 0.115 Uiso 1 1 calc R . . C73 C 0.2538(3) 0.1854(7) 0.1336(4) 0.076(3) Uani 1 1 d . . . H73A H 0.2553 0.1274 0.1156 0.091 Uiso 1 1 calc R B . H73B H 0.2373 0.2289 0.1004 0.091 Uiso 1 1 calc R . . C74 C 0.3101(3) 0.2142(5) 0.1756(3) 0.0513(16) Uani 1 1 d . B . H74A H 0.3079 0.2675 0.1979 0.062 Uiso 1 1 calc R . . H74B H 0.3280 0.1668 0.2055 0.062 Uiso 1 1 calc R . . C75 C 0.3988(3) 0.2731(5) 0.1802(3) 0.0541(17) Uani 0.656(14) 1 d P B 1 O18 O 0.5015(4) 0.3020(7) 0.0237(5) 0.081(3) Uani 0.656(14) 1 d P B 1 C76 C 0.4282(6) 0.2875(8) 0.1421(6) 0.053(5) Uani 0.656(14) 1 d PG B 1 C77 C 0.4575(6) 0.2168(7) 0.1344(6) 0.069(4) Uani 0.656(14) 1 d PG B 1 H77A H 0.4605 0.1632 0.1559 0.082 Uiso 0.656(14) 1 calc PR B 1 C78 C 0.4826(4) 0.2245(8) 0.0952(6) 0.077(4) Uani 0.656(14) 1 d PG B 1 H78A H 0.5026 0.1763 0.0899 0.092 Uiso 0.656(14) 1 calc PR B 1 C79 C 0.4782(4) 0.3029(10) 0.0637(5) 0.060(5) Uani 0.656(14) 1 d PG B 1 C80 C 0.4489(4) 0.3736(8) 0.0714(5) 0.066(5) Uani 0.656(14) 1 d PG B 1 H80A H 0.4460 0.4271 0.0499 0.079 Uiso 0.656(14) 1 calc PR B 1 C81 C 0.4239(5) 0.3658(6) 0.1107(5) 0.058(4) Uani 0.656(14) 1 d PG B 1 H81A H 0.4038 0.4141 0.1159 0.069 Uiso 0.656(14) 1 calc PR B 1 C82 C 0.5014(5) 0.3700(11) -0.0098(6) 0.114(4) Uani 0.656(14) 1 d P B 1 H82A H 0.5215 0.3548 -0.0338 0.171 Uiso 0.656(14) 1 calc PR B 1 H82B H 0.5191 0.4205 0.0164 0.171 Uiso 0.656(14) 1 calc PR B 1 H82C H 0.4637 0.3855 -0.0369 0.171 Uiso 0.656(14) 1 calc PR B 1 C75' C 0.3988(3) 0.2731(5) 0.1802(3) 0.0541(17) Uani 0.344(14) 1 d P B 2 O18' O 0.4827(8) 0.4080(14) 0.0194(10) 0.090(7) Uani 0.344(14) 1 d P B 2 C76' C 0.4268(11) 0.3074(13) 0.1405(11) 0.048(9) Uani 0.344(14) 1 d PG B 2 C77' C 0.4155(10) 0.3941(12) 0.1201(11) 0.061(7) Uani 0.344(14) 1 d PG B 2 H77B H 0.3942 0.4306 0.1336 0.073 Uiso 0.344(14) 1 calc PR B 2 C78' C 0.4351(7) 0.4274(11) 0.0800(9) 0.066(7) Uani 0.344(14) 1 d PG B 2 H78B H 0.4273 0.4867 0.0661 0.079 Uiso 0.344(14) 1 calc PR B 2 C79' C 0.4662(9) 0.3740(15) 0.0603(10) 0.058(8) Uani 0.344(14) 1 d PG B 2 C80' C 0.4776(8) 0.2872(14) 0.0806(10) 0.061(10) Uani 0.344(14) 1 d PG B 2 H80B H 0.4988 0.2507 0.0671 0.073 Uiso 0.344(14) 1 calc PR B 2 C81' C 0.4579(8) 0.2540(11) 0.1207(10) 0.050(6) Uani 0.344(14) 1 d PG B 2 H81B H 0.4657 0.1947 0.1346 0.060 Uiso 0.344(14) 1 calc PR B 2 C82' C 0.5014(5) 0.3700(11) -0.0098(6) 0.114(4) Uani 0.344(14) 1 d P B 2 H82D H 0.5087 0.4121 -0.0361 0.171 Uiso 0.344(14) 1 calc PR B 2 H82E H 0.4755 0.3251 -0.0346 0.171 Uiso 0.344(14) 1 calc PR B 2 H82F H 0.5356 0.3414 0.0172 0.171 Uiso 0.344(14) 1 calc PR B 2 P1 P 0.33026(13) 0.6733(3) 0.02323(15) 0.1021(10) Uani 1 1 d D . . F1 F 0.2710(3) 0.6571(6) 0.0189(4) 0.141(3) Uani 1 1 d D . . F2 F 0.3883(3) 0.6892(7) 0.0286(4) 0.170(4) Uani 1 1 d D . . F3 F 0.3227(4) 0.5952(5) -0.0206(4) 0.140(3) Uani 1 1 d D . . F4 F 0.3534(4) 0.6087(8) 0.0789(4) 0.178(4) Uani 1 1 d D . . F5 F 0.3369(4) 0.7539(7) 0.0652(5) 0.181(4) Uani 1 1 d D . . F6 F 0.3057(4) 0.7366(6) -0.0321(4) 0.149(3) Uani 1 1 d D . . P2 P 0.03171(14) 0.77146(19) 0.48386(11) 0.0627(8) Uani 0.713(4) 1 d PDU C 1 F7 F 0.0759(4) 0.7048(8) 0.5299(4) 0.137(3) Uani 0.713(4) 1 d PDU C 1 F8 F -0.0027(6) 0.8298(8) 0.4364(5) 0.183(4) Uani 0.713(4) 1 d PDU C 1 F9 F 0.0212(5) 0.8237(9) 0.5311(5) 0.158(4) Uani 0.713(4) 1 d PDU C 1 F10 F 0.0861(5) 0.8227(9) 0.5098(6) 0.175(4) Uani 0.713(4) 1 d PDU C 1 F11 F 0.0334(5) 0.7090(8) 0.4390(4) 0.178(4) Uani 0.713(4) 1 d PDU C 1 F12 F -0.0061(5) 0.7167(9) 0.5026(6) 0.180(4) Uani 0.713(4) 1 d PDU C 1 P2' P 0.4343(4) 0.9384(6) 0.9644(4) 0.080(2) Uani 0.287(4) 1 d PDU C 2 F7' F 0.3882(8) 0.9358(16) 0.9872(10) 0.138(6) Uani 0.287(4) 1 d PDU C 2 F8' F 0.4777(8) 0.9459(15) 0.9416(9) 0.121(5) Uani 0.287(4) 1 d PDU . 2 F9' F 0.4558(9) 0.8642(11) 1.0090(8) 0.110(5) Uani 0.287(4) 1 d PDU C 2 F10' F 0.4642(9) 1.0055(13) 1.0171(8) 0.120(5) Uani 0.287(4) 1 d PDU . 2 F11' F 0.4031(8) 1.0073(12) 0.9216(8) 0.109(5) Uani 0.287(4) 1 d PDU C 2 F12' F 0.4021(9) 0.8761(14) 0.9157(9) 0.134(6) Uani 0.287(4) 1 d PDU C 2 N5 N 0.1983(9) 0.9881(9) 1.0004(7) 0.234(11) Uani 1 1 d . . . C83 C 0.1867(5) 0.9184(9) 0.9821(5) 0.098(3) Uani 1 1 d . . . C84 C 0.1714(7) 0.8360(9) 0.9615(6) 0.130(5) Uani 1 1 d . . . H84A H 0.1465 0.8382 0.9183 0.196 Uiso 1 1 calc R . . H84B H 0.1529 0.8084 0.9840 0.196 Uiso 1 1 calc R . . H84C H 0.2038 0.8012 0.9670 0.196 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 O1 0.041(2) 0.047(2) 0.036(2) 0.0030(17) 0.0156(17) 0.0028(18) O2 0.063(4) 0.097(5) 0.146(6) 0.070(5) 0.058(4) 0.036(4) O3 0.153(5) 0.069(4) 0.188(6) 0.029(4) 0.144(5) 0.026(4) O4 0.080(4) 0.094(4) 0.040(2) -0.013(3) 0.008(2) 0.050(3) O5 0.038(2) 0.041(2) 0.038(2) -0.0003(17) 0.0161(17) -0.0048(17) O6 0.051(3) 0.043(2) 0.059(3) -0.001(2) 0.020(2) -0.013(2) O7 0.043(2) 0.051(3) 0.061(3) -0.002(2) 0.023(2) -0.008(2) O8 0.044(2) 0.071(3) 0.041(2) -0.002(2) 0.0134(19) 0.003(2) O9 0.038(2) 0.056(3) 0.083(4) -0.014(3) 0.018(2) 0.006(2) O10 0.034(3) 0.081(4) 0.177(7) -0.065(4) 0.038(4) -0.011(3) O11 0.031(2) 0.061(3) 0.104(4) 0.004(3) 0.024(3) 0.000(2) O12 0.051(3) 0.060(3) 0.103(4) -0.019(3) 0.038(3) -0.006(2) O13 0.045(2) 0.052(3) 0.056(3) 0.009(2) 0.025(2) 0.007(2) O14 0.065(3) 0.096(4) 0.054(3) 0.014(3) 0.032(3) 0.022(3) O15 0.188(9) 0.088(5) 0.074(4) 0.009(4) 0.062(5) 0.030(5) O16 0.085(4) 0.055(3) 0.082(4) -0.017(3) 0.055(3) -0.016(3) O17 0.060(3) 0.055(3) 0.133(5) 0.001(3) 0.053(4) -0.008(3) N1 0.068(4) 0.057(4) 0.107(5) -0.010(4) 0.062(4) -0.016(3) N2 0.041(3) 0.068(4) 0.038(3) -0.003(2) 0.020(2) 0.001(3) C1 0.037(3) 0.030(3) 0.042(3) 0.000(2) 0.018(2) 0.008(2) C2 0.030(3) 0.029(3) 0.043(3) -0.003(2) 0.017(2) 0.003(2) C3 0.031(3) 0.032(3) 0.043(3) 0.002(2) 0.014(2) 0.004(2) C4 0.036(3) 0.029(3) 0.050(3) 0.002(2) 0.021(3) 0.004(2) C5 0.037(3) 0.033(3) 0.061(4) 0.011(3) 0.021(3) 0.003(2) C6 0.040(3) 0.030(3) 0.058(4) 0.009(3) 0.022(3) 0.000(2) C7 0.043(3) 0.038(3) 0.051(3) 0.008(3) 0.021(3) -0.001(3) C8 0.044(3) 0.033(3) 0.059(4) 0.009(3) 0.023(3) 0.001(2) C9 0.038(3) 0.032(3) 0.075(4) 0.006(3) 0.027(3) 0.005(2) C10 0.038(3) 0.034(3) 0.060(4) 0.001(3) 0.015(3) 0.001(2) C11 0.040(3) 0.027(3) 0.065(4) 0.000(3) 0.023(3) 0.000(2) C12 0.041(3) 0.033(3) 0.064(4) -0.004(3) 0.023(3) -0.001(2) C13 0.035(3) 0.028(3) 0.052(3) -0.004(2) 0.018(3) 0.005(2) C14 0.033(3) 0.036(3) 0.042(3) -0.007(2) 0.011(2) 0.004(2) C15 0.046(4) 0.036(3) 0.081(5) 0.012(3) 0.031(3) 0.007(3) C16 0.051(4) 0.032(3) 0.085(5) -0.003(3) 0.034(4) -0.001(3) C17 0.041(3) 0.055(4) 0.062(4) 0.019(3) 0.021(3) 0.003(3) C18 0.051(4) 0.051(4) 0.071(5) -0.017(3) 0.028(4) -0.014(3) C19 0.048(4) 0.077(5) 0.042(3) 0.005(3) 0.014(3) 0.012(3) C20 0.065(5) 0.126(9) 0.046(4) 0.033(5) 0.021(4) 0.020(5) C21 0.082(7) 0.106(8) 0.117(8) -0.023(7) 0.063(7) 0.008(6) C22 0.135(6) 0.078(5) 0.190(7) 0.027(5) 0.139(6) 0.015(5) C23 0.127(6) 0.052(4) 0.165(7) 0.011(4) 0.121(6) 0.010(4) C24 0.102(7) 0.074(6) 0.080(6) 0.018(5) 0.054(6) 0.021(5) C25 0.038(3) 0.044(3) 0.045(3) 0.003(3) 0.011(3) -0.004(3) C26 0.040(3) 0.056(4) 0.054(4) 0.004(3) 0.013(3) -0.010(3) C27 0.062(4) 0.051(4) 0.068(4) -0.008(3) 0.036(4) -0.022(3) C28 0.040(3) 0.058(4) 0.057(4) -0.009(3) 0.016(3) -0.013(3) C29 0.043(3) 0.052(4) 0.049(4) 0.004(3) 0.013(3) -0.014(3) C30 0.051(4) 0.051(4) 0.042(3) -0.005(3) 0.011(3) -0.008(3) C31 0.061(4) 0.039(3) 0.044(3) -0.001(3) 0.017(3) 0.013(3) C32 0.056(4) 0.038(3) 0.043(3) -0.002(3) 0.009(3) 0.017(3) C33 0.050(4) 0.028(3) 0.054(4) 0.002(3) 0.012(3) 0.009(3) C34 0.055(4) 0.038(3) 0.063(4) 0.003(3) 0.017(3) 0.016(3) C35 0.041(3) 0.040(3) 0.065(4) -0.001(3) 0.015(3) 0.014(3) C36 0.047(4) 0.044(4) 0.067(4) -0.004(3) 0.016(3) 0.013(3) C37 0.037(3) 0.046(4) 0.081(5) -0.016(3) 0.023(3) 0.005(3) C38 0.057(4) 0.042(3) 0.087(5) -0.002(3) 0.049(4) 0.006(3) C39 0.049(4) 0.043(3) 0.063(4) -0.007(3) 0.027(3) 0.005(3) C40 0.055(4) 0.031(3) 0.071(4) 0.000(3) 0.035(3) 0.008(3) C41 0.062(4) 0.033(3) 0.067(4) -0.006(3) 0.030(4) 0.000(3) C42 0.056(4) 0.028(3) 0.054(4) -0.002(3) 0.025(3) 0.003(3) C43 0.052(4) 0.035(3) 0.044(3) -0.001(3) 0.016(3) -0.003(3) C44 0.047(3) 0.035(3) 0.046(3) 0.000(3) 0.015(3) 0.004(3) C45 0.065(5) 0.038(4) 0.086(5) 0.007(3) 0.034(4) 0.019(3) C46 0.082(5) 0.033(3) 0.087(5) -0.001(3) 0.045(5) 0.011(3) C47 0.056(4) 0.066(5) 0.063(5) 0.007(4) 0.011(4) 0.024(4) C48 0.070(5) 0.059(4) 0.065(5) -0.014(4) 0.036(4) -0.014(4) C49 0.054(5) 0.055(5) 0.251(16) -0.059(7) 0.072(7) -0.017(4) C50 0.057(5) 0.042(4) 0.159(11) -0.002(5) -0.007(6) -0.015(4) C51 0.031(4) 0.069(6) 0.231(15) 0.049(8) 0.023(6) -0.009(4) C52 0.033(4) 0.085(6) 0.157(10) -0.040(6) 0.036(5) -0.010(4) C53 0.031(4) 0.076(6) 0.189(12) -0.037(7) 0.014(5) 0.010(4) C54 0.051(4) 0.051(5) 0.124(8) -0.003(5) -0.003(5) 0.008(4) C55 0.058(4) 0.068(5) 0.058(4) 0.011(4) 0.020(4) 0.013(4) C56 0.080(6) 0.093(6) 0.054(4) 0.007(4) 0.040(4) -0.007(5) C57 0.088(6) 0.129(8) 0.032(3) -0.008(4) 0.028(4) -0.041(6) C58 0.053(5) 0.074(6) 0.125(9) -0.014(6) 0.002(5) 0.016(4) C59 0.28(2) 0.072(7) 0.136(11) -0.029(7) 0.150(14) -0.020(10) C60 0.208(14) 0.069(6) 0.122(9) -0.041(6) 0.130(10) -0.048(7) C61 0.079(6) 0.068(5) 0.105(7) -0.004(5) 0.054(5) -0.020(4) C62 0.061(4) 0.046(4) 0.084(5) -0.003(3) 0.048(4) -0.004(3) C63 0.059(4) 0.037(4) 0.135(8) 0.009(4) 0.049(5) 0.009(3) C64 0.057(4) 0.036(3) 0.106(6) 0.014(4) 0.041(4) 0.002(3) C65 0.056(4) 0.045(3) 0.058(4) 0.006(3) 0.039(3) 0.008(3) C66 0.067(4) 0.035(3) 0.054(4) 0.005(3) 0.039(3) 0.012(3) C67 0.076(5) 0.035(3) 0.063(4) 0.000(3) 0.047(4) -0.003(3) C68 0.053(4) 0.056(4) 0.064(4) 0.013(3) 0.037(3) 0.015(3) C69 0.068(6) 0.096(7) 0.087(6) -0.011(6) 0.030(5) -0.018(5) C70 0.060(5) 0.110(8) 0.069(5) -0.008(5) -0.001(4) 0.031(5) C71 0.077(6) 0.201(14) 0.067(6) 0.039(7) 0.022(5) -0.037(8) C72 0.070(6) 0.156(11) 0.065(5) 0.026(6) 0.033(5) -0.019(6) C73 0.060(5) 0.113(7) 0.054(4) 0.008(5) 0.024(4) -0.021(5) C74 0.051(4) 0.070(4) 0.039(3) 0.009(3) 0.024(3) 0.007(3) C75 0.042(3) 0.069(4) 0.048(4) -0.012(3) 0.016(3) -0.004(3) O18 0.057(5) 0.097(7) 0.100(7) 0.011(6) 0.044(5) -0.008(5) C76 0.033(9) 0.050(7) 0.065(11) -0.013(6) 0.010(8) -0.006(6) C77 0.058(8) 0.060(9) 0.104(12) 0.009(8) 0.050(8) 0.012(7) C78 0.061(8) 0.067(9) 0.125(12) 0.008(9) 0.060(9) 0.009(7) C79 0.033(7) 0.074(12) 0.076(10) 0.002(8) 0.026(6) -0.009(6) C80 0.055(9) 0.065(10) 0.067(9) 0.007(7) 0.015(7) -0.012(8) C81 0.047(7) 0.060(9) 0.058(8) -0.018(7) 0.013(6) 0.002(6) C82 0.080(7) 0.161(13) 0.104(9) 0.030(9) 0.044(7) -0.011(8) C75' 0.042(3) 0.069(4) 0.048(4) -0.012(3) 0.016(3) -0.004(3) O18' 0.091(14) 0.096(15) 0.117(16) -0.002(12) 0.077(13) -0.015(11) C76' 0.027(15) 0.056(15) 0.07(2) -0.008(13) 0.025(14) 0.003(11) C77' 0.072(17) 0.055(15) 0.075(16) -0.023(13) 0.050(14) -0.013(13) C78' 0.066(14) 0.039(12) 0.11(2) -0.013(12) 0.049(14) -0.011(11) C79' 0.047(14) 0.065(19) 0.071(16) -0.005(12) 0.034(12) -0.017(13) C80' 0.044(14) 0.07(3) 0.08(2) -0.019(17) 0.044(14) -0.005(14) C81' 0.037(10) 0.058(16) 0.059(13) -0.005(12) 0.024(10) 0.004(11) C82' 0.080(7) 0.161(13) 0.104(9) 0.030(9) 0.044(7) -0.011(8) P1 0.0856(18) 0.140(3) 0.0901(19) -0.0092(19) 0.0465(16) 0.0067(18) F1 0.101(5) 0.198(9) 0.132(6) -0.032(6) 0.058(5) -0.014(5) F2 0.131(7) 0.239(11) 0.177(8) -0.003(8) 0.100(7) 0.011(7) F3 0.184(8) 0.130(6) 0.130(6) -0.003(5) 0.091(6) 0.020(6) F4 0.156(8) 0.240(11) 0.110(6) 0.046(7) 0.031(6) 0.015(8) F5 0.147(7) 0.216(10) 0.212(10) -0.117(8) 0.108(7) -0.050(7) F6 0.166(8) 0.133(7) 0.144(7) 0.031(5) 0.063(6) 0.015(6) P2 0.100(2) 0.0561(15) 0.0358(12) -0.0011(10) 0.0323(13) -0.0164(14) F7 0.154(7) 0.182(7) 0.074(5) 0.031(5) 0.046(5) 0.028(6) F8 0.230(8) 0.166(7) 0.112(6) 0.002(6) 0.032(6) 0.108(7) F9 0.158(7) 0.207(8) 0.119(6) -0.049(6) 0.068(6) 0.020(7) F10 0.174(8) 0.179(8) 0.146(7) -0.019(7) 0.043(7) 0.034(7) F11 0.230(8) 0.166(7) 0.074(5) -0.029(5) 0.001(6) 0.118(6) F12 0.180(8) 0.176(8) 0.163(7) 0.014(7) 0.054(7) 0.020(7) P2' 0.107(6) 0.086(5) 0.074(4) -0.003(4) 0.063(4) 0.006(4) F7' 0.152(10) 0.132(10) 0.119(9) 0.001(9) 0.045(9) -0.009(9) F8' 0.137(8) 0.116(8) 0.104(7) 0.002(7) 0.044(7) -0.002(7) F9' 0.147(10) 0.096(9) 0.088(8) 0.020(8) 0.050(8) 0.003(8) F10' 0.133(8) 0.119(8) 0.104(7) -0.003(7) 0.046(7) 0.001(7) F11' 0.128(10) 0.133(10) 0.082(8) 0.017(8) 0.059(7) -0.004(9) F12' 0.138(10) 0.143(10) 0.114(9) 0.005(9) 0.046(9) 0.000(9) N5 0.32(2) 0.097(9) 0.148(12) 0.041(9) -0.039(13) -0.026(12) C83 0.111(9) 0.092(8) 0.081(7) 0.026(6) 0.030(6) 0.019(7) C84 0.177(14) 0.102(9) 0.084(8) -0.006(7) 0.027(8) -0.015(9) _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 O1 C1 1.365(7) . ? O1 C19 1.429(7) . ? O2 C21 1.319(12) . ? O2 C20 1.404(13) . ? O3 C23 1.350(10) . ? O3 C22 1.459(10) . ? O4 C31 1.387(8) . ? O4 C24 1.403(10) . ? O5 C2 1.368(7) . ? O5 C25 1.427(7) . ? O6 C26 1.429(8) . ? O6 C27 1.438(8) . ? O7 C29 1.417(8) . ? O7 C28 1.428(8) . ? O8 C44 1.371(8) . ? O8 C30 1.433(7) . ? O9 C49 1.372(10) . ? O9 C9 1.380(7) . ? O10 C51 1.279(10) . ? O10 C50 1.289(11) . ? O11 C53 1.355(10) . ? O11 C52 1.395(10) . ? O12 C37 1.393(8) . ? O12 C54 1.450(11) . ? O13 C8 1.383(8) . ? O13 C55 1.458(8) . ? O14 C56 1.379(11) . ? O14 C57 1.454(10) . ? O15 C58 1.276(11) . ? O15 C59 1.365(14) . ? O16 C38 1.385(9) . ? O16 C60 1.447(11) . ? O17 C62 1.362(9) . ? O17 C61 1.414(9) . ? N1 C68 1.487(10) . ? N1 C69 1.491(11) . ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? N2 C74 1.491(8) . ? N2 C75 1.498(8) . ? N2 H2A 0.9200 . ? N2 H2B 0.9200 . ? C1 C14 1.388(8) . ? C1 C2 1.409(8) . ? C2 C3 1.381(8) . ? C3 C4 1.389(8) . ? C3 H3A 0.9500 . ? C4 C13 1.402(8) . ? C4 C5 1.515(8) . ? C5 C6 1.520(8) . ? C5 C17 1.524(9) . ? C5 C15 1.561(9) . ? C6 C7 1.395(9) . ? C6 C11 1.396(9) . ? C7 C8 1.380(9) . ? C7 H7A 0.9500 . ? C8 C9 1.398(10) . ? C9 C10 1.399(9) . ? C10 C11 1.390(8) . ? C10 H10A 0.9500 . ? C11 C12 1.526(9) . ? C12 C18 1.517(10) . ? C12 C13 1.527(8) . ? C12 C16 1.573(9) . ? C13 C14 1.397(9) . ? C14 H14A 0.9500 . ? C15 C16 1.520(10) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.486(11) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.415(14) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.461(11) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.502(8) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.506(10) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.503(10) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.383(10) . ? C31 C44 1.404(9) . ? C32 C33 1.380(10) . ? C32 H32A 0.9500 . ? C33 C42 1.401(9) . ? C33 C34 1.532(9) . ? C34 C47 1.515(10) . ? C34 C35 1.521(10) . ? C34 C45 1.575(9) . ? C35 C36 1.383(10) . ? C35 C40 1.385(10) . ? C36 C37 1.381(11) . ? C36 H36A 0.9500 . ? C37 C38 1.386(11) . ? C38 C39 1.398(10) . ? C39 C40 1.386(10) . ? C39 H39A 0.9500 . ? C40 C41 1.535(9) . ? C41 C48 1.512(10) . ? C41 C42 1.519(9) . ? C41 C46 1.564(9) . ? C42 C43 1.387(9) . ? C43 C44 1.379(9) . ? C43 H43A 0.9500 . ? C45 C46 1.527(11) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.343(12) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.366(13) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.500(13) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.504(11) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.521(14) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.451(14) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 C67 1.370(10) . ? C62 C63 1.394(10) . ? C63 C64 1.366(10) . ? C63 H63A 0.9500 . ? C64 C65 1.383(9) . ? C64 H64A 0.9500 . ? C65 C66 1.380(9) . ? C65 C68 1.510(9) . ? C66 C67 1.380(10) . ? C66 H66A 0.9500 . ? C67 H67A 0.9500 . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 C70 1.406(14) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 C71 1.697(14) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.507(13) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C73 1.546(11) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.495(10) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C76 1.470(10) . ? O18 C82 1.313(15) . ? O18 C79 1.365(12) . ? C76 C77 1.3900 . ? C76 C81 1.3900 . ? C77 C78 1.3900 . ? C77 H77A 0.9500 . ? C78 C79 1.3900 . ? C78 H78A 0.9500 . ? C79 C80 1.3900 . ? C80 C81 1.3900 . ? C80 H80A 0.9500 . ? C81 H81A 0.9500 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? O18' C79' 1.35(2) . ? C76' C77' 1.3900 . ? C76' C81' 1.3900 . ? C77' C78' 1.3900 . ? C77' H77B 0.9500 . ? C78' C79' 1.3900 . ? C78' H78B 0.9500 . ? C79' C80' 1.3900 . ? C80' C81' 1.3900 . ? C80' H80B 0.9500 . ? C81' H81B 0.9500 . ? P1 F2 1.537(8) . ? P1 F3 1.548(8) . ? P1 F5 1.552(8) . ? P1 F6 1.555(8) . ? P1 F4 1.572(9) . ? P1 F1 1.578(7) . ? P2 F8 1.439(10) . ? P2 F11 1.459(8) . ? P2 F9 1.521(9) . ? P2 F12 1.527(12) . ? P2 F10 1.540(12) . ? P2 F7 1.603(9) . ? P2' F11' 1.462(14) . ? P2' F12' 1.476(15) . ? P2' F9' 1.499(14) . ? P2' F8' 1.502(14) . ? P2' F7' 1.564(15) . ? P2' F10' 1.567(15) . ? F8' F10' 1.64(3) 3_677 ? F10' F8' 1.64(3) 3_677 ? N5 C83 1.135(17) . ? C83 C84 1.342(17) . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 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 C1 O1 C19 117.9(5) . . ? C21 O2 C20 115.6(7) . . ? C23 O3 C22 115.9(7) . . ? C31 O4 C24 121.3(6) . . ? C2 O5 C25 116.3(4) . . ? C26 O6 C27 112.1(5) . . ? C29 O7 C28 111.8(5) . . ? C44 O8 C30 116.3(5) . . ? C49 O9 C9 119.5(6) . . ? C51 O10 C50 131.6(8) . . ? C53 O11 C52 116.7(6) . . ? C37 O12 C54 115.1(7) . . ? C8 O13 C55 116.0(5) . . ? C56 O14 C57 114.3(6) . . ? C58 O15 C59 117.0(11) . . ? C38 O16 C60 116.9(6) . . ? C62 O17 C61 117.9(7) . . ? C68 N1 C69 117.3(6) . . ? C68 N1 H1A 108.0 . . ? C69 N1 H1A 108.0 . . ? C68 N1 H1B 108.0 . . ? C69 N1 H1B 108.0 . . ? H1A N1 H1B 107.2 . . ? C74 N2 C75 114.5(5) . . ? C74 N2 H2A 108.6 . . ? C75 N2 H2A 108.6 . . ? C74 N2 H2B 108.6 . . ? C75 N2 H2B 108.6 . . ? H2A N2 H2B 107.6 . . ? O1 C1 C14 126.5(5) . . ? O1 C1 C2 114.2(5) . . ? C14 C1 C2 119.3(5) . . ? O5 C2 C3 125.3(5) . . ? O5 C2 C1 114.2(5) . . ? C3 C2 C1 120.5(5) . . ? C2 C3 C4 120.3(5) . . ? C2 C3 H3A 119.8 . . ? C4 C3 H3A 119.8 . . ? C3 C4 C13 119.5(5) . . ? C3 C4 C5 126.0(6) . . ? C13 C4 C5 114.5(5) . . ? C4 C5 C6 105.7(5) . . ? C4 C5 C17 114.1(5) . . ? C6 C5 C17 114.0(6) . . ? C4 C5 C15 105.7(5) . . ? C6 C5 C15 105.5(5) . . ? C17 C5 C15 111.1(5) . . ? C7 C6 C11 120.4(6) . . ? C7 C6 C5 125.6(6) . . ? C11 C6 C5 114.0(6) . . ? C8 C7 C6 120.4(6) . . ? C8 C7 H7A 119.8 . . ? C6 C7 H7A 119.8 . . ? C7 C8 O13 123.8(6) . . ? C7 C8 C9 119.2(6) . . ? O13 C8 C9 117.0(5) . . ? O9 C9 C8 118.0(6) . . ? O9 C9 C10 121.2(6) . . ? C8 C9 C10 120.8(6) . . ? C11 C10 C9 119.6(6) . . ? C11 C10 H10A 120.2 . . ? C9 C10 H10A 120.2 . . ? C10 C11 C6 119.6(6) . . ? C10 C11 C12 125.8(6) . . ? C6 C11 C12 114.6(5) . . ? C18 C12 C11 114.3(5) . . ? C18 C12 C13 114.6(6) . . ? C11 C12 C13 105.6(5) . . ? C18 C12 C16 111.2(5) . . ? C11 C12 C16 105.2(5) . . ? C13 C12 C16 105.0(5) . . ? C14 C13 C4 120.3(5) . . ? C14 C13 C12 125.8(6) . . ? C4 C13 C12 113.9(5) . . ? C1 C14 C13 120.0(5) . . ? C1 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C16 C15 C5 111.3(5) . . ? C16 C15 H15A 109.4 . . ? C5 C15 H15A 109.4 . . ? C16 C15 H15B 109.4 . . ? C5 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C15 C16 C12 111.0(5) . . ? C15 C16 H16A 109.4 . . ? C12 C16 H16A 109.4 . . ? C15 C16 H16B 109.4 . . ? C12 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C5 C17 H17A 109.5 . . ? C5 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C5 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C12 C18 H18A 109.5 . . ? C12 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C12 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O1 C19 C20 107.4(6) . . ? O1 C19 H19A 110.2 . . ? C20 C19 H19A 110.2 . . ? O1 C19 H19B 110.2 . . ? C20 C19 H19B 110.2 . . ? H19A C19 H19B 108.5 . . ? O2 C20 C19 112.2(7) . . ? O2 C20 H20A 109.2 . . ? C19 C20 H20A 109.2 . . ? O2 C20 H20B 109.2 . . ? C19 C20 H20B 109.2 . . ? H20A C20 H20B 107.9 . . ? O2 C21 C22 111.3(11) . . ? O2 C21 H21A 109.4 . . ? C22 C21 H21A 109.4 . . ? O2 C21 H21B 109.4 . . ? C22 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? C21 C22 O3 111.1(8) . . ? C21 C22 H22A 109.4 . . ? O3 C22 H22A 109.4 . . ? C21 C22 H22B 109.4 . . ? O3 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? O3 C23 C24 112.9(7) . . ? O3 C23 H23A 109.0 . . ? C24 C23 H23A 109.0 . . ? O3 C23 H23B 109.0 . . ? C24 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? O4 C24 C23 109.1(9) . . ? O4 C24 H24A 109.9 . . ? C23 C24 H24A 109.9 . . ? O4 C24 H24B 109.8 . . ? C23 C24 H24B 109.8 . . ? H24A C24 H24B 108.3 . . ? O5 C25 C26 106.8(5) . . ? O5 C25 H25A 110.4 . . ? C26 C25 H25A 110.4 . . ? O5 C25 H25B 110.4 . . ? C26 C25 H25B 110.4 . . ? H25A C25 H25B 108.6 . . ? O6 C26 C25 109.2(5) . . ? O6 C26 H26A 109.8 . . ? C25 C26 H26A 109.8 . . ? O6 C26 H26B 109.8 . . ? C25 C26 H26B 109.8 . . ? H26A C26 H26B 108.3 . . ? O6 C27 C28 109.5(5) . . ? O6 C27 H27A 109.8 . . ? C28 C27 H27A 109.8 . . ? O6 C27 H27B 109.8 . . ? C28 C27 H27B 109.8 . . ? H27A C27 H27B 108.2 . . ? O7 C28 C27 110.1(6) . . ? O7 C28 H28A 109.6 . . ? C27 C28 H28A 109.6 . . ? O7 C28 H28B 109.6 . . ? C27 C28 H28B 109.6 . . ? H28A C28 H28B 108.2 . . ? O7 C29 C30 108.4(5) . . ? O7 C29 H29A 110.0 . . ? C30 C29 H29A 110.0 . . ? O7 C29 H29B 110.0 . . ? C30 C29 H29B 110.0 . . ? H29A C29 H29B 108.4 . . ? O8 C30 C29 107.1(5) . . ? O8 C30 H30A 110.3 . . ? C29 C30 H30A 110.3 . . ? O8 C30 H30B 110.3 . . ? C29 C30 H30B 110.3 . . ? H30A C30 H30B 108.5 . . ? C32 C31 O4 124.3(6) . . ? C32 C31 C44 120.1(6) . . ? O4 C31 C44 115.5(6) . . ? C33 C32 C31 119.5(6) . . ? C33 C32 H32A 120.2 . . ? C31 C32 H32A 120.2 . . ? C32 C33 C42 120.3(6) . . ? C32 C33 C34 125.7(6) . . ? C42 C33 C34 113.9(6) . . ? C47 C34 C35 115.7(7) . . ? C47 C34 C33 114.4(6) . . ? C35 C34 C33 105.5(5) . . ? C47 C34 C45 110.0(6) . . ? C35 C34 C45 104.9(6) . . ? C33 C34 C45 105.5(6) . . ? C36 C35 C40 119.9(7) . . ? C36 C35 C34 125.4(7) . . ? C40 C35 C34 114.7(6) . . ? C37 C36 C35 120.2(7) . . ? C37 C36 H36A 119.9 . . ? C35 C36 H36A 119.9 . . ? C36 C37 C38 119.6(7) . . ? C36 C37 O12 125.4(7) . . ? C38 C37 O12 115.0(7) . . ? O16 C38 C37 116.9(7) . . ? O16 C38 C39 122.1(7) . . ? C37 C38 C39 121.1(7) . . ? C40 C39 C38 118.2(7) . . ? C40 C39 H39A 120.9 . . ? C38 C39 H39A 120.9 . . ? C35 C40 C39 121.0(7) . . ? C35 C40 C41 114.7(6) . . ? C39 C40 C41 124.3(7) . . ? C48 C41 C42 113.8(6) . . ? C48 C41 C40 115.1(6) . . ? C42 C41 C40 104.4(5) . . ? C48 C41 C46 111.5(6) . . ? C42 C41 C46 105.9(6) . . ? C40 C41 C46 105.2(6) . . ? C43 C42 C33 120.3(6) . . ? C43 C42 C41 124.8(6) . . ? C33 C42 C41 114.9(6) . . ? C44 C43 C42 119.2(6) . . ? C44 C43 H43A 120.4 . . ? C42 C43 H43A 120.4 . . ? O8 C44 C43 125.0(6) . . ? O8 C44 C31 114.6(6) . . ? C43 C44 C31 120.5(6) . . ? C46 C45 C34 111.0(6) . . ? C46 C45 H45A 109.4 . . ? C34 C45 H45A 109.4 . . ? C46 C45 H45B 109.4 . . ? C34 C45 H45B 109.4 . . ? H45A C45 H45B 108.0 . . ? C45 C46 C41 111.4(6) . . ? C45 C46 H46A 109.3 . . ? C41 C46 H46A 109.3 . . ? C45 C46 H46B 109.4 . . ? C41 C46 H46B 109.3 . . ? H46A C46 H46B 108.0 . . ? C34 C47 H47A 109.5 . . ? C34 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C34 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C41 C48 H48A 109.5 . . ? C41 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C41 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 O9 121.1(8) . . ? C50 C49 H49A 107.1 . . ? O9 C49 H49A 107.1 . . ? C50 C49 H49B 107.1 . . ? O9 C49 H49B 107.1 . . ? H49A C49 H49B 106.8 . . ? O10 C50 C49 126.7(8) . . ? O10 C50 H50A 105.7 . . ? C49 C50 H50A 105.6 . . ? O10 C50 H50B 105.6 . . ? C49 C50 H50B 105.6 . . ? H50A C50 H50B 106.1 . . ? O10 C51 C52 128.1(8) . . ? O10 C51 H51A 105.3 . . ? C52 C51 H51A 105.3 . . ? O10 C51 H51B 105.3 . . ? C52 C51 H51B 105.3 . . ? H51A C51 H51B 106.0 . . ? C51 C52 O11 117.1(7) . . ? C51 C52 H52A 108.0 . . ? O11 C52 H52A 108.0 . . ? C51 C52 H52B 108.0 . . ? O11 C52 H52B 108.0 . . ? H52A C52 H52B 107.3 . . ? O11 C53 C54 111.6(7) . . ? O11 C53 H53A 109.3 . . ? C54 C53 H53A 109.3 . . ? O11 C53 H53B 109.3 . . ? C54 C53 H53B 109.3 . . ? H53A C53 H53B 108.0 . . ? O12 C54 C53 107.4(9) . . ? O12 C54 H54A 110.2 . . ? C53 C54 H54A 110.2 . . ? O12 C54 H54B 110.2 . . ? C53 C54 H54B 110.2 . . ? H54A C54 H54B 108.5 . . ? O13 C55 C56 108.7(6) . . ? O13 C55 H55A 109.9 . . ? C56 C55 H55A 109.9 . . ? O13 C55 H55B 109.9 . . ? C56 C55 H55B 109.9 . . ? H55A C55 H55B 108.3 . . ? O14 C56 C55 112.1(7) . . ? O14 C56 H56A 109.2 . . ? C55 C56 H56A 109.2 . . ? O14 C56 H56B 109.2 . . ? C55 C56 H56B 109.2 . . ? H56A C56 H56B 107.9 . . ? O14 C57 C58 106.3(8) . . ? O14 C57 H57A 110.5 . . ? C58 C57 H57A 110.5 . . ? O14 C57 H57B 110.5 . . ? C58 C57 H57B 110.5 . . ? H57A C57 H57B 108.7 . . ? O15 C58 C57 114.7(9) . . ? O15 C58 H58A 108.6 . . ? C57 C58 H58A 108.6 . . ? O15 C58 H58B 108.6 . . ? C57 C58 H58B 108.6 . . ? H58A C58 H58B 107.6 . . ? O15 C59 C60 110.9(11) . . ? O15 C59 H59A 109.5 . . ? C60 C59 H59A 109.5 . . ? O15 C59 H59B 109.5 . . ? C60 C59 H59B 109.5 . . ? H59A C59 H59B 108.1 . . ? O16 C60 C59 108.5(9) . . ? O16 C60 H60A 110.0 . . ? C59 C60 H60A 110.0 . . ? O16 C60 H60B 110.0 . . ? C59 C60 H60B 110.0 . . ? H60A C60 H60B 108.4 . . ? O17 C61 H61A 109.5 . . ? O17 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? O17 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? O17 C62 C67 125.8(6) . . ? O17 C62 C63 115.4(7) . . ? C67 C62 C63 118.8(7) . . ? C64 C63 C62 120.0(7) . . ? C64 C63 H63A 120.0 . . ? C62 C63 H63A 120.0 . . ? C63 C64 C65 121.8(7) . . ? C63 C64 H64A 119.1 . . ? C65 C64 H64A 119.1 . . ? C66 C65 C64 117.4(6) . . ? C66 C65 C68 120.7(6) . . ? C64 C65 C68 121.8(6) . . ? C67 C66 C65 121.5(6) . . ? C67 C66 H66A 119.2 . . ? C65 C66 H66A 119.2 . . ? C62 C67 C66 120.4(6) . . ? C62 C67 H67A 119.8 . . ? C66 C67 H67A 119.8 . . ? N1 C68 C65 114.9(6) . . ? N1 C68 H68A 108.5 . . ? C65 C68 H68A 108.5 . . ? N1 C68 H68B 108.5 . . ? C65 C68 H68B 108.5 . . ? H68A C68 H68B 107.5 . . ? C70 C69 N1 107.1(9) . . ? C70 C69 H69A 110.3 . . ? N1 C69 H69A 110.3 . . ? C70 C69 H69B 110.3 . . ? N1 C69 H69B 110.3 . . ? H69A C69 H69B 108.5 . . ? C69 C70 C71 105.3(9) . . ? C69 C70 H70A 110.7 . . ? C71 C70 H70A 110.7 . . ? C69 C70 H70B 110.7 . . ? C71 C70 H70B 110.7 . . ? H70A C70 H70B 108.8 . . ? C72 C71 C70 111.6(8) . . ? C72 C71 H71A 109.3 . . ? C70 C71 H71A 109.3 . . ? C72 C71 H71B 109.3 . . ? C70 C71 H71B 109.3 . . ? H71A C71 H71B 108.0 . . ? C71 C72 C73 113.7(8) . . ? C71 C72 H72A 108.8 . . ? C73 C72 H72A 108.8 . . ? C71 C72 H72B 108.8 . . ? C73 C72 H72B 108.8 . . ? H72A C72 H72B 107.7 . . ? C74 C73 C72 109.0(7) . . ? C74 C73 H73A 109.9 . . ? C72 C73 H73A 109.9 . . ? C74 C73 H73B 109.9 . . ? C72 C73 H73B 109.9 . . ? H73A C73 H73B 108.3 . . ? N2 C74 C73 111.5(5) . . ? N2 C74 H74A 109.3 . . ? C73 C74 H74A 109.3 . . ? N2 C74 H74B 109.3 . . ? C73 C74 H74B 109.3 . . ? H74A C74 H74B 108.0 . . ? C76 C75 N2 108.9(8) . . ? C82 O18 C79 123.9(12) . . ? C77 C76 C81 120.0 . . ? C77 C76 C75 117.6(8) . . ? C81 C76 C75 122.2(8) . . ? C78 C77 C76 120.0 . . ? C78 C77 H77A 120.0 . . ? C76 C77 H77A 120.0 . . ? C77 C78 C79 120.0 . . ? C77 C78 H78A 120.0 . . ? C79 C78 H78A 120.0 . . ? O18 C79 C78 115.5(10) . . ? O18 C79 C80 124.4(10) . . ? C78 C79 C80 120.0 . . ? C81 C80 C79 120.0 . . ? C81 C80 H80A 120.0 . . ? C79 C80 H80A 120.0 . . ? C80 C81 C76 120.0 . . ? C80 C81 H81A 120.0 . . ? C76 C81 H81A 120.0 . . ? O18 C82 H82A 109.5 . . ? O18 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? O18 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C77' C76' C81' 120.0 . . ? C78' C77' C76' 120.0 . . ? C78' C77' H77B 120.0 . . ? C76' C77' H77B 120.0 . . ? C77' C78' C79' 120.0 . . ? C77' C78' H78B 120.0 . . ? C79' C78' H78B 120.0 . . ? O18' C79' C80' 122.0(17) . . ? O18' C79' C78' 118.0(17) . . ? C80' C79' C78' 120.0 . . ? C81' C80' C79' 120.0 . . ? C81' C80' H80B 120.0 . . ? C79' C80' H80B 120.0 . . ? C80' C81' C76' 120.0 . . ? C80' C81' H81B 120.0 . . ? C76' C81' H81B 120.0 . . ? F2 P1 F3 90.6(5) . . ? F2 P1 F5 89.5(5) . . ? F3 P1 F5 177.9(6) . . ? F2 P1 F6 91.3(5) . . ? F3 P1 F6 89.3(5) . . ? F5 P1 F6 88.6(6) . . ? F2 P1 F4 90.3(6) . . ? F3 P1 F4 90.6(6) . . ? F5 P1 F4 91.5(6) . . ? F6 P1 F4 178.3(6) . . ? F2 P1 F1 179.1(5) . . ? F3 P1 F1 90.1(5) . . ? F5 P1 F1 89.9(5) . . ? F6 P1 F1 89.4(5) . . ? F4 P1 F1 89.0(5) . . ? F8 P2 F11 90.5(6) . . ? F8 P2 F9 91.5(7) . . ? F11 P2 F9 168.2(9) . . ? F8 P2 F12 106.7(9) . . ? F11 P2 F12 96.2(8) . . ? F9 P2 F12 72.1(7) . . ? F8 P2 F10 101.6(8) . . ? F11 P2 F10 107.9(8) . . ? F9 P2 F10 83.1(7) . . ? F12 P2 F10 142.4(8) . . ? F8 P2 F7 170.2(7) . . ? F11 P2 F7 82.4(5) . . ? F9 P2 F7 96.8(6) . . ? F12 P2 F7 81.0(6) . . ? F10 P2 F7 74.4(6) . . ? F11' P2' F12' 85.1(12) . . ? F11' P2' F9' 168.6(13) . . ? F12' P2' F9' 91.2(12) . . ? F11' P2' F8' 89.2(11) . . ? F12' P2' F8' 92.1(12) . . ? F9' P2' F8' 101.7(12) . . ? F11' P2' F7' 88.1(11) . . ? F12' P2' F7' 89.0(12) . . ? F9' P2' F7' 81.1(11) . . ? F8' P2' F7' 177.0(14) . . ? F11' P2' F10' 93.7(12) . . ? F12' P2' F10' 175.4(14) . . ? F9' P2' F10' 89.1(11) . . ? F8' P2' F10' 92.4(12) . . ? F7' P2' F10' 86.4(11) . . ? P2' F8' F10' 120.1(16) . 3_677 ? P2' F10' F8' 145.5(18) . 3_677 ? N5 C83 C84 178(2) . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 67.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.461 _refine_diff_density_min -0.892 _refine_diff_density_rms 0.145 data_ic14971 _database_code_depnum_ccdc_archive 'CCDC 879621' #TrackingRef 'ic14971-revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C101 H128 F12 N6 O20 P2' _chemical_formula_weight 2036.03 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' _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 14.6500(4) _cell_length_b 15.8479(4) _cell_length_c 23.0752(7) _cell_angle_alpha 90.00 _cell_angle_beta 104.640(3) _cell_angle_gamma 90.00 _cell_volume 5183.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6717 _cell_measurement_theta_min 3.1152 _cell_measurement_theta_max 76.4433 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2148 _exptl_absorpt_coefficient_mu 1.158 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.57126 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini A' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16542 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 68.00 _reflns_number_total 9341 _reflns_number_gt 7517 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.1000P)^2^+8.0061P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9341 _refine_ls_number_parameters 648 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1138 _refine_ls_R_factor_gt 0.0987 _refine_ls_wR_factor_ref 0.2675 _refine_ls_wR_factor_gt 0.2554 _refine_ls_goodness_of_fit_ref 1.198 _refine_ls_restrained_S_all 1.276 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.003 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 O1 O 0.1209(2) 0.34142(18) -0.00119(12) 0.0399(6) Uani 1 1 d . . . O2 O -0.0589(2) 0.41846(17) -0.05744(13) 0.0406(6) Uani 1 1 d . . . O3 O -0.2502(2) 0.3747(2) -0.08484(15) 0.0518(8) Uani 1 1 d . . . O4 O -0.2905(2) 0.2326(2) -0.01855(14) 0.0524(8) Uani 1 1 d . . . O5 O 0.1887(2) 0.30938(18) 0.11190(12) 0.0395(6) Uani 1 1 d . . . O6 O 0.0673(2) 0.33694(19) 0.18432(12) 0.0416(7) Uani 1 1 d . . . O7 O -0.1296(3) 0.3150(3) 0.17946(19) 0.0724(12) Uani 1 1 d . . . O8 O -0.2154(2) 0.19259(19) 0.09568(14) 0.0459(7) Uani 1 1 d . . . N1 N -0.0175(3) 0.1853(2) 0.13558(18) 0.0459(9) Uani 1 1 d . . . H3 H -0.078(4) 0.202(3) 0.117(2) 0.045(13) Uiso 1 1 d . . . H4 H 0.014(3) 0.240(3) 0.151(2) 0.042(12) Uiso 1 1 d . . . C1 C 0.1824(3) 0.2751(2) 0.01209(17) 0.0354(8) Uani 1 1 d . . . C2 C 0.2104(3) 0.2256(3) -0.03034(17) 0.0367(8) Uani 1 1 d . . . H2A H 0.1858 0.2370 -0.0718 0.044 Uiso 1 1 calc R . . C3 C 0.2738(3) 0.1601(3) -0.01268(17) 0.0357(8) Uani 1 1 d . . . C4 C 0.3154(3) 0.1066(3) -0.05468(18) 0.0397(9) Uani 1 1 d . . . C5 C 0.3044(3) 0.0151(3) -0.03797(18) 0.0363(8) Uani 1 1 d . . . C6 C 0.2648(3) -0.0488(3) -0.07787(18) 0.0370(8) Uani 1 1 d . . . H6A H 0.2397 -0.0364 -0.1191 0.044 Uiso 1 1 calc R . . C7 C 0.2621(3) -0.1302(3) -0.05731(18) 0.0391(9) Uani 1 1 d . . . C8 C 0.2987(3) -0.1496(3) 0.0032(2) 0.0424(9) Uani 1 1 d . . . C9 C 0.3380(3) -0.0856(3) 0.04345(18) 0.0389(9) Uani 1 1 d . . . H9A H 0.3630 -0.0980 0.0847 0.047 Uiso 1 1 calc R . . C10 C 0.3401(3) -0.0036(3) 0.02248(18) 0.0372(9) Uani 1 1 d . . . C11 C 0.3835(3) 0.0722(3) 0.06081(19) 0.0405(9) Uani 1 1 d . . . C12 C 0.3098(3) 0.1423(3) 0.04785(18) 0.0370(8) Uani 1 1 d . . . C13 C 0.2827(3) 0.1913(3) 0.09084(17) 0.0377(9) Uani 1 1 d . . . H13A H 0.3074 0.1793 0.1322 0.045 Uiso 1 1 calc R . . C14 C 0.2199(3) 0.2574(2) 0.07330(17) 0.0351(8) Uani 1 1 d . . . C15 C 0.4235(3) 0.1246(3) -0.0349(2) 0.0445(10) Uani 1 1 d . . . H15A H 0.4562 0.0895 -0.0589 0.053 Uiso 1 1 calc R . . H15B H 0.4353 0.1846 -0.0424 0.053 Uiso 1 1 calc R . . C16 C 0.4634(3) 0.1047(3) 0.0324(2) 0.0452(10) Uani 1 1 d . . . H16A H 0.4922 0.1562 0.0536 0.054 Uiso 1 1 calc R . . H16B H 0.5132 0.0612 0.0371 0.054 Uiso 1 1 calc R . . C17 C 0.2757(3) 0.1249(3) -0.12072(19) 0.0452(10) Uani 1 1 d . . . H17A H 0.2078 0.1133 -0.1318 0.068 Uiso 1 1 calc R . . H17B H 0.3071 0.0889 -0.1444 0.068 Uiso 1 1 calc R . . H17C H 0.2866 0.1843 -0.1287 0.068 Uiso 1 1 calc R . . C18 C 0.4221(3) 0.0526(3) 0.1266(2) 0.0503(11) Uani 1 1 d . . . H18A H 0.3709 0.0328 0.1434 0.075 Uiso 1 1 calc R . . H18B H 0.4501 0.1037 0.1477 0.075 Uiso 1 1 calc R . . H18C H 0.4705 0.0087 0.1312 0.075 Uiso 1 1 calc R . . C19 C 0.0910(3) 0.3631(3) -0.06309(17) 0.0408(9) Uani 1 1 d . . . H19A H 0.0571 0.3148 -0.0861 0.049 Uiso 1 1 calc R . . H19B H 0.1468 0.3757 -0.0785 0.049 Uiso 1 1 calc R . . C20 C 0.0273(3) 0.4386(3) -0.07138(18) 0.0415(9) Uani 1 1 d . . . H20A H 0.0589 0.4849 -0.0451 0.050 Uiso 1 1 calc R . . H20B H 0.0145 0.4582 -0.1134 0.050 Uiso 1 1 calc R . . C21 C -0.1312(3) 0.4759(3) -0.08556(19) 0.0433(10) Uani 1 1 d . . . H21A H -0.1432 0.4708 -0.1296 0.052 Uiso 1 1 calc R . . H21B H -0.1105 0.5344 -0.0742 0.052 Uiso 1 1 calc R . . C22 C -0.2195(3) 0.4576(3) -0.0672(2) 0.0480(10) Uani 1 1 d . . . H22A H -0.2078 0.4631 -0.0232 0.058 Uiso 1 1 calc R . . H22B H -0.2690 0.4986 -0.0861 0.058 Uiso 1 1 calc R . . C23 C -0.3386(3) 0.3554(3) -0.0741(3) 0.0606(13) Uani 1 1 d . . . H23A H -0.3897 0.3808 -0.1058 0.073 Uiso 1 1 calc R . . H23B H -0.3421 0.3793 -0.0351 0.073 Uiso 1 1 calc R . . C24 C -0.3510(3) 0.2617(3) -0.0736(2) 0.0536(12) Uani 1 1 d . . . H24A H -0.4175 0.2472 -0.0758 0.064 Uiso 1 1 calc R . . H24B H -0.3330 0.2357 -0.1082 0.064 Uiso 1 1 calc R . . C25 C 0.2163(3) 0.2890(3) 0.17431(17) 0.0377(9) Uani 1 1 d . . . H25A H 0.2854 0.2952 0.1899 0.045 Uiso 1 1 calc R . . H25B H 0.1989 0.2300 0.1807 0.045 Uiso 1 1 calc R . . C26 C 0.1657(3) 0.3488(3) 0.20581(17) 0.0389(9) Uani 1 1 d . . . H26A H 0.1850 0.3384 0.2495 0.047 Uiso 1 1 calc R . . H26B H 0.1823 0.4077 0.1984 0.047 Uiso 1 1 calc R . . C27 C 0.0131(3) 0.3928(3) 0.2109(2) 0.0486(10) Uani 1 1 d . . . H27A H 0.0392 0.4506 0.2124 0.058 Uiso 1 1 calc R . . H27B H 0.0164 0.3746 0.2524 0.058 Uiso 1 1 calc R . . C28 C -0.0866(4) 0.3929(4) 0.1753(2) 0.0601(13) Uani 1 1 d . . . H28A H -0.1216 0.4381 0.1901 0.072 Uiso 1 1 calc R . . H28B H -0.0891 0.4050 0.1328 0.072 Uiso 1 1 calc R . . C29 C -0.2264(4) 0.3200(5) 0.1456(5) 0.119(4) Uani 1 1 d . . . H29A H -0.2634 0.3488 0.1701 0.143 Uiso 1 1 calc R . . H29B H -0.2299 0.3548 0.1095 0.143 Uiso 1 1 calc R . . C30 C -0.2674(4) 0.2412(4) 0.1278(3) 0.0718(16) Uani 1 1 d . . . H30A H -0.3320 0.2499 0.1023 0.086 Uiso 1 1 calc R . . H30B H -0.2724 0.2093 0.1638 0.086 Uiso 1 1 calc R . . C31 C 0.0283(3) 0.0367(3) 0.0178(2) 0.0588(13) Uani 1 1 d . . . H31A H 0.0882 0.0149 0.0435 0.071 Uiso 1 1 calc R . . H31B H 0.0438 0.0781 -0.0104 0.071 Uiso 1 1 calc R . . C32 C -0.0271(4) 0.0793(3) 0.0558(2) 0.0589(13) Uani 1 1 d . . . H32A H -0.0424 0.0379 0.0841 0.071 Uiso 1 1 calc R . . H32B H -0.0871 0.1010 0.0301 0.071 Uiso 1 1 calc R . . C33 C 0.0290(3) 0.1516(3) 0.0905(2) 0.0444(10) Uani 1 1 d . . . H33A H 0.0931 0.1317 0.1109 0.053 Uiso 1 1 calc R . . H33B H 0.0352 0.1971 0.0624 0.053 Uiso 1 1 calc R . . C34 C -0.0200(4) 0.1273(4) 0.1873(2) 0.0587(12) Uani 1 1 d . . . H34A H -0.0579 0.1537 0.2123 0.070 Uiso 1 1 calc R . . H34B H -0.0506 0.0735 0.1715 0.070 Uiso 1 1 calc R . . C35 C 0.0773(4) 0.1100(3) 0.2249(2) 0.0553(12) Uani 1 1 d . . . C36 C 0.1150(5) 0.1602(4) 0.2747(2) 0.0645(14) Uani 1 1 d . A . H36A H 0.0767 0.2030 0.2853 0.077 Uiso 1 1 calc R . . C37 C 0.2046(5) 0.1501(4) 0.3086(2) 0.0732(17) Uani 1 1 d . . . C39 C 0.2265(4) 0.0335(4) 0.2451(3) 0.0728(17) Uani 1 1 d . . . C40 C 0.1333(4) 0.0463(3) 0.2114(2) 0.0593(13) Uani 1 1 d . A . H40A H 0.1080 0.0102 0.1784 0.071 Uiso 1 1 calc R . . C38 C 0.2618(5) 0.0881(4) 0.2945(3) 0.082(2) Uani 0.50 1 d P A 1 C41 C 0.3596(7) 0.0762(5) 0.3352(5) 0.127(4) Uani 0.50 1 d PD A 1 C42 C 0.3456(12) 0.0031(12) 0.3809(8) 0.119(7) Uani 0.50 1 d P A 1 H42A H 0.3272 -0.0495 0.3587 0.179 Uiso 0.50 1 calc PR A 1 H42B H 0.2961 0.0200 0.4003 0.179 Uiso 0.50 1 calc PR A 1 H42C H 0.4049 -0.0054 0.4114 0.179 Uiso 0.50 1 calc PR A 1 C43 C 0.3857(8) 0.1564(9) 0.3800(7) 0.088(4) Uani 0.50 1 d P A 1 H43A H 0.3918 0.2070 0.3569 0.132 Uiso 0.50 1 calc PR A 1 H43B H 0.4455 0.1456 0.4096 0.132 Uiso 0.50 1 calc PR A 1 H43C H 0.3356 0.1649 0.4006 0.132 Uiso 0.50 1 calc PR A 1 C44 C 0.4227(11) 0.0551(14) 0.3013(8) 0.122(7) Uani 0.50 1 d PD A 1 H44A H 0.3991 0.0057 0.2765 0.183 Uiso 0.50 1 calc PR A 1 H44B H 0.4844 0.0420 0.3281 0.183 Uiso 0.50 1 calc PR A 1 H44C H 0.4289 0.1027 0.2755 0.183 Uiso 0.50 1 calc PR A 1 C38' C 0.2618(5) 0.0881(4) 0.2945(3) 0.082(2) Uani 0.50 1 d P A 2 C45 C 0.3596(7) 0.0762(5) 0.3352(5) 0.127(4) Uani 0.50 1 d P A 2 H45A H 0.3672 0.1125 0.3705 0.190 Uiso 0.50 1 calc PR A 2 H45B H 0.4068 0.0913 0.3135 0.190 Uiso 0.50 1 calc PR A 2 H45C H 0.3681 0.0171 0.3479 0.190 Uiso 0.50 1 calc PR A 2 P1 P 0.46874(11) 0.80886(10) 0.25130(7) 0.0664(4) Uani 1 1 d . . . F1 F 0.4070(5) 0.7384(3) 0.2149(3) 0.178(3) Uani 1 1 d . . . F2 F 0.5382(4) 0.8758(4) 0.2867(3) 0.147(2) Uani 1 1 d . . . F3 F 0.5402(4) 0.7418(4) 0.2829(4) 0.178(3) Uani 1 1 d . . . F4 F 0.4206(6) 0.8044(8) 0.2997(4) 0.251(6) Uani 1 1 d . . . F5 F 0.4015(6) 0.8740(4) 0.2136(4) 0.193(4) Uani 1 1 d . . . F6 F 0.5180(7) 0.8220(7) 0.2002(4) 0.221(4) Uani 1 1 d . . . N11 N 0.1977(5) 0.5691(4) 0.2532(3) 0.0955(19) Uani 1 1 d . . . C46 C 0.2716(5) 0.5620(4) 0.2496(2) 0.0649(14) Uani 1 1 d . . . C47 C 0.3666(5) 0.5498(6) 0.2419(4) 0.106(3) Uani 1 1 d . . . H47A H 0.4131 0.5669 0.2786 0.159 Uiso 1 1 calc R . . H47B H 0.3748 0.5842 0.2083 0.159 Uiso 1 1 calc R . . H47C H 0.3759 0.4901 0.2337 0.159 Uiso 1 1 calc R . . N12 N 0.0045(5) 0.8548(5) 0.1368(3) 0.104(2) Uani 1 1 d . . . C48 C 0.0728(6) 0.8194(5) 0.1458(4) 0.089(2) Uani 1 1 d . . . C49 C 0.1585(8) 0.7729(9) 0.1593(8) 0.203(8) Uani 1 1 d . . . H49A H 0.2109 0.8102 0.1783 0.304 Uiso 1 1 calc R . . H49B H 0.1694 0.7497 0.1223 0.304 Uiso 1 1 calc R . . H49C H 0.1542 0.7266 0.1867 0.304 Uiso 1 1 calc R . . O9 O -0.0995(3) 0.3055(3) 0.03351(16) 0.0639(10) Uani 1 1 d . . . H1 H -0.076(5) 0.335(5) 0.013(3) 0.096 Uiso 1 1 d . . . H2 H -0.1646(8) 0.2821(6) 0.0054(4) 0.096 Uiso 1 1 d . . . O10 O 0.5747(8) 0.8661(6) 0.4412(4) 0.326(8) Uani 1 1 d RDU . . C50 C 0.4339(8) 0.8130(6) 0.4696(4) 0.329(11) Uani 1 1 d RDU . . C51 C 0.4891(8) 0.8817(6) 0.4489(4) 0.339(9) Uani 1 1 d RDU . . C52 C 0.6208(8) 0.9400(6) 0.4623(4) 0.346(9) Uani 1 1 d RDU . . C53 C 0.6474(8) 0.9366(6) 0.5300(4) 0.39(2) Uani 1 1 d RD . . 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 O1 0.0475(15) 0.0413(15) 0.0307(13) 0.0048(11) 0.0097(11) 0.0125(12) O2 0.0431(15) 0.0351(14) 0.0412(15) 0.0114(12) 0.0064(12) 0.0059(12) O3 0.0533(18) 0.0425(17) 0.0542(18) -0.0016(14) 0.0036(14) -0.0056(14) O4 0.0556(18) 0.0435(17) 0.0477(17) 0.0065(14) -0.0066(14) -0.0086(14) O5 0.0491(16) 0.0405(15) 0.0291(13) 0.0020(11) 0.0100(12) 0.0089(12) O6 0.0434(15) 0.0448(16) 0.0370(14) -0.0120(12) 0.0110(12) -0.0034(12) O7 0.055(2) 0.085(3) 0.086(3) -0.042(2) 0.0341(19) -0.0241(19) O8 0.0376(15) 0.0487(17) 0.0484(17) -0.0096(14) 0.0054(12) -0.0053(13) N1 0.0385(19) 0.047(2) 0.051(2) -0.0074(17) 0.0085(16) -0.0033(16) C1 0.0350(19) 0.037(2) 0.0345(19) 0.0032(16) 0.0096(15) 0.0052(16) C2 0.039(2) 0.041(2) 0.0308(18) 0.0031(16) 0.0102(15) 0.0040(16) C3 0.0318(18) 0.039(2) 0.0361(19) 0.0007(16) 0.0091(15) 0.0022(16) C4 0.038(2) 0.044(2) 0.039(2) -0.0003(17) 0.0124(16) 0.0064(17) C5 0.0287(18) 0.041(2) 0.038(2) 0.0009(17) 0.0077(15) 0.0057(16) C6 0.0288(18) 0.047(2) 0.0342(19) 0.0005(17) 0.0065(15) 0.0029(16) C7 0.0286(18) 0.045(2) 0.042(2) -0.0030(18) 0.0045(15) -0.0020(16) C8 0.035(2) 0.040(2) 0.048(2) 0.0052(18) 0.0032(17) -0.0008(17) C9 0.0321(19) 0.044(2) 0.037(2) 0.0028(17) 0.0017(15) 0.0017(16) C10 0.0260(17) 0.043(2) 0.040(2) -0.0026(17) 0.0039(15) 0.0062(15) C11 0.036(2) 0.038(2) 0.043(2) -0.0024(17) 0.0008(16) 0.0036(17) C12 0.0306(18) 0.039(2) 0.039(2) 0.0005(17) 0.0040(15) 0.0015(16) C13 0.0362(19) 0.042(2) 0.0318(19) 0.0018(16) 0.0027(15) 0.0011(16) C14 0.0361(19) 0.037(2) 0.0319(19) -0.0010(16) 0.0077(15) 0.0014(16) C15 0.040(2) 0.042(2) 0.055(3) -0.0019(19) 0.0200(19) 0.0040(18) C16 0.0302(19) 0.042(2) 0.061(3) -0.008(2) 0.0072(18) 0.0031(17) C17 0.054(2) 0.046(2) 0.039(2) 0.0019(18) 0.0183(19) 0.0088(19) C18 0.048(2) 0.045(2) 0.047(2) -0.0047(19) -0.0076(19) 0.0107(19) C19 0.048(2) 0.043(2) 0.0304(19) 0.0045(17) 0.0083(16) 0.0071(18) C20 0.049(2) 0.037(2) 0.036(2) 0.0077(17) 0.0069(17) 0.0014(18) C21 0.050(2) 0.031(2) 0.043(2) 0.0060(17) 0.0008(18) 0.0076(17) C22 0.045(2) 0.037(2) 0.057(3) 0.003(2) 0.0014(19) 0.0067(18) C23 0.046(3) 0.053(3) 0.076(3) 0.018(3) 0.004(2) 0.000(2) C24 0.043(2) 0.053(3) 0.055(3) 0.011(2) -0.004(2) -0.005(2) C25 0.042(2) 0.038(2) 0.0304(19) 0.0003(16) 0.0029(16) -0.0010(16) C26 0.045(2) 0.041(2) 0.0281(18) -0.0046(16) 0.0047(16) -0.0047(17) C27 0.055(3) 0.047(2) 0.048(2) -0.015(2) 0.020(2) -0.007(2) C28 0.054(3) 0.066(3) 0.063(3) -0.021(3) 0.020(2) -0.002(2) C29 0.049(3) 0.119(6) 0.192(9) -0.099(7) 0.036(4) -0.015(4) C30 0.050(3) 0.089(4) 0.073(4) -0.033(3) 0.011(3) -0.002(3) C31 0.046(3) 0.063(3) 0.066(3) -0.020(3) 0.012(2) -0.006(2) C32 0.048(3) 0.062(3) 0.063(3) -0.021(3) 0.007(2) -0.007(2) C33 0.041(2) 0.044(2) 0.045(2) -0.0045(19) 0.0037(18) -0.0044(18) C34 0.057(3) 0.064(3) 0.056(3) -0.002(2) 0.017(2) -0.015(2) C35 0.071(3) 0.052(3) 0.043(2) 0.005(2) 0.015(2) -0.020(2) C36 0.092(4) 0.064(3) 0.040(2) -0.002(2) 0.022(3) -0.022(3) C37 0.107(5) 0.061(3) 0.043(3) 0.005(2) 0.003(3) -0.030(3) C39 0.075(4) 0.055(3) 0.073(4) 0.019(3) -0.010(3) -0.014(3) C40 0.073(3) 0.047(3) 0.051(3) 0.003(2) 0.003(2) -0.010(2) C38 0.089(4) 0.072(4) 0.063(3) 0.029(3) -0.023(3) -0.034(3) C41 0.107(6) 0.078(5) 0.144(8) 0.029(5) -0.063(6) -0.022(5) C42 0.093(11) 0.111(12) 0.118(13) 0.034(11) -0.041(10) -0.003(9) C43 0.049(6) 0.090(9) 0.107(10) -0.026(8) -0.014(6) -0.001(6) C44 0.066(9) 0.172(19) 0.106(12) -0.051(12) -0.020(8) 0.034(10) C38' 0.089(4) 0.072(4) 0.063(3) 0.029(3) -0.023(3) -0.034(3) C45 0.107(6) 0.078(5) 0.144(8) 0.029(5) -0.063(6) -0.022(5) P1 0.0629(8) 0.0630(8) 0.0634(8) 0.0108(7) -0.0022(7) -0.0020(6) F1 0.236(7) 0.092(3) 0.130(4) 0.025(3) -0.093(5) -0.041(4) F2 0.141(5) 0.118(4) 0.155(5) -0.010(4) -0.011(4) -0.053(4) F3 0.134(5) 0.105(4) 0.227(7) 0.041(4) -0.082(5) 0.004(3) F4 0.168(6) 0.459(16) 0.160(6) -0.076(8) 0.109(6) -0.123(9) F5 0.209(7) 0.097(4) 0.210(7) 0.009(4) -0.064(6) 0.046(4) F6 0.267(10) 0.272(11) 0.167(7) 0.023(7) 0.133(7) -0.009(9) N11 0.105(5) 0.094(4) 0.100(5) -0.036(4) 0.050(4) -0.017(4) C46 0.086(4) 0.054(3) 0.046(3) -0.008(2) 0.001(3) -0.012(3) C47 0.081(5) 0.105(6) 0.118(6) 0.011(5) -0.001(4) -0.006(4) N12 0.090(4) 0.123(6) 0.089(4) -0.021(4) 0.006(3) 0.010(4) C48 0.090(5) 0.083(5) 0.097(5) -0.041(4) 0.033(4) -0.019(4) C49 0.112(8) 0.176(12) 0.31(2) -0.112(13) 0.040(10) 0.044(8) O9 0.0522(19) 0.082(3) 0.052(2) 0.0253(18) 0.0034(15) -0.0093(18) O10 0.286(15) 0.262(13) 0.326(12) -0.074(11) -0.117(13) 0.049(12) C50 0.322(18) 0.261(17) 0.317(16) -0.068(15) -0.081(16) 0.069(15) C51 0.303(16) 0.284(14) 0.326(13) -0.071(12) -0.115(14) 0.030(13) C52 0.311(16) 0.286(15) 0.340(14) -0.070(12) -0.105(14) 0.039(13) C53 0.59(6) 0.30(3) 0.41(4) 0.14(3) 0.37(4) 0.09(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 O1 C1 1.367(5) . ? O1 C19 1.426(5) . ? O2 C20 1.416(5) . ? O2 C21 1.422(5) . ? O3 C23 1.412(6) . ? O3 C22 1.415(5) . ? O4 C8 1.375(5) 3 ? O4 C24 1.430(5) . ? O5 C14 1.373(5) . ? O5 C25 1.431(5) . ? O6 C26 1.413(5) . ? O6 C27 1.427(5) . ? O7 C28 1.401(7) . ? O7 C29 1.437(8) . ? O8 C7 1.387(5) 3 ? O8 C30 1.416(6) . ? N1 C33 1.479(6) . ? N1 C34 1.514(6) . ? N1 H3 0.92(5) . ? N1 H4 1.00(5) . ? C1 C2 1.395(6) . ? C1 C14 1.408(5) . ? C2 C3 1.384(6) . ? C2 H2A 0.9500 . ? C3 C12 1.392(5) . ? C3 C4 1.526(5) . ? C4 C17 1.516(6) . ? C4 C5 1.519(6) . ? C4 C15 1.559(6) . ? C5 C10 1.392(6) . ? C5 C6 1.393(6) . ? C6 C7 1.378(6) . ? C6 H6A 0.9500 . ? C7 O8 1.387(5) 3 ? C7 C8 1.398(6) . ? C8 O4 1.375(5) 3 ? C8 C9 1.396(6) . ? C9 C10 1.391(6) . ? C9 H9A 0.9500 . ? C10 C11 1.531(6) . ? C11 C18 1.512(6) . ? C11 C12 1.524(5) . ? C11 C16 1.567(6) . ? C12 C13 1.394(6) . ? C13 C14 1.386(6) . ? C13 H13A 0.9500 . ? C15 C16 1.546(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.500(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.488(7) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.496(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.500(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.483(7) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.402(9) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.498(7) . ? C31 C31 1.537(9) 3 ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.516(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.495(8) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C40 1.385(8) . ? C35 C36 1.392(7) . ? C36 C37 1.357(9) . ? C36 H36A 0.9500 . ? C37 C38 1.383(11) . ? C39 C40 1.403(8) . ? C39 C38 1.421(9) . ? C40 H40A 0.9500 . ? C38 C41 1.513(9) . ? C41 C44 1.393(15) . ? C41 C42 1.614(19) . ? C41 C43 1.622(16) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? P1 F4 1.465(6) . ? P1 F5 1.537(6) . ? P1 F3 1.540(5) . ? P1 F6 1.543(7) . ? P1 F1 1.546(5) . ? P1 F2 1.552(5) . ? N11 C46 1.112(8) . ? C46 C47 1.460(11) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? N12 C48 1.121(10) . ? C48 C49 1.420(13) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? O9 H1 0.80(8) . ? O9 H2 1.074(11) . ? O10 C51 1.3326 . ? O10 C52 1.3769 . ? C50 C51 1.5043 . ? C52 C53 1.5117 . ? 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 C1 O1 C19 115.3(3) . . ? C20 O2 C21 110.9(3) . . ? C23 O3 C22 112.9(4) . . ? C8 O4 C24 117.6(3) 3 . ? C14 O5 C25 117.5(3) . . ? C26 O6 C27 113.3(3) . . ? C28 O7 C29 108.3(6) . . ? C7 O8 C30 118.6(3) 3 . ? C33 N1 C34 116.2(4) . . ? C33 N1 H3 110(3) . . ? C34 N1 H3 109(3) . . ? C33 N1 H4 108(3) . . ? C34 N1 H4 110(3) . . ? H3 N1 H4 102(4) . . ? O1 C1 C2 124.7(3) . . ? O1 C1 C14 116.5(3) . . ? C2 C1 C14 118.8(3) . . ? C3 C2 C1 120.7(4) . . ? C3 C2 H2A 119.7 . . ? C1 C2 H2A 119.7 . . ? C2 C3 C12 120.2(4) . . ? C2 C3 C4 125.2(4) . . ? C12 C3 C4 114.4(3) . . ? C17 C4 C5 113.5(4) . . ? C17 C4 C3 114.8(3) . . ? C5 C4 C3 106.5(3) . . ? C17 C4 C15 111.3(4) . . ? C5 C4 C15 105.4(3) . . ? C3 C4 C15 104.5(3) . . ? C10 C5 C6 119.7(4) . . ? C10 C5 C4 114.8(4) . . ? C6 C5 C4 125.4(4) . . ? C7 C6 C5 119.8(4) . . ? C7 C6 H6A 120.1 . . ? C5 C6 H6A 120.1 . . ? C6 C7 O8 120.0(4) . 3 ? C6 C7 C8 120.9(4) . . ? O8 C7 C8 118.9(4) 3 . ? O4 C8 C9 124.9(4) 3 . ? O4 C8 C7 115.5(4) 3 . ? C9 C8 C7 119.6(4) . . ? C10 C9 C8 119.3(4) . . ? C10 C9 H9A 120.4 . . ? C8 C9 H9A 120.4 . . ? C9 C10 C5 120.8(4) . . ? C9 C10 C11 125.1(4) . . ? C5 C10 C11 114.1(4) . . ? C18 C11 C12 114.4(4) . . ? C18 C11 C10 114.5(4) . . ? C12 C11 C10 106.7(3) . . ? C18 C11 C16 111.0(4) . . ? C12 C11 C16 104.2(3) . . ? C10 C11 C16 105.1(3) . . ? C3 C12 C13 119.8(4) . . ? C3 C12 C11 114.5(4) . . ? C13 C12 C11 125.5(4) . . ? C14 C13 C12 120.1(4) . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? O5 C14 C13 124.7(3) . . ? O5 C14 C1 114.9(3) . . ? C13 C14 C1 120.4(4) . . ? C16 C15 C4 110.9(3) . . ? C16 C15 H15A 109.5 . . ? C4 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? C4 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? C15 C16 C11 110.7(3) . . ? C15 C16 H16A 109.5 . . ? C11 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? C4 C17 H17A 109.5 . . ? C4 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C4 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C11 C18 H18A 109.5 . . ? C11 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C11 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O1 C19 C20 110.1(3) . . ? O1 C19 H19A 109.6 . . ? C20 C19 H19A 109.6 . . ? O1 C19 H19B 109.6 . . ? C20 C19 H19B 109.6 . . ? H19A C19 H19B 108.2 . . ? O2 C20 C19 110.7(3) . . ? O2 C20 H20A 109.5 . . ? C19 C20 H20A 109.5 . . ? O2 C20 H20B 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 108.1 . . ? O2 C21 C22 110.2(3) . . ? O2 C21 H21A 109.6 . . ? C22 C21 H21A 109.6 . . ? O2 C21 H21B 109.6 . . ? C22 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? O3 C22 C21 109.6(4) . . ? O3 C22 H22A 109.8 . . ? C21 C22 H22A 109.8 . . ? O3 C22 H22B 109.8 . . ? C21 C22 H22B 109.8 . . ? H22A C22 H22B 108.2 . . ? O3 C23 C24 109.5(4) . . ? O3 C23 H23A 109.8 . . ? C24 C23 H23A 109.8 . . ? O3 C23 H23B 109.8 . . ? C24 C23 H23B 109.8 . . ? H23A C23 H23B 108.2 . . ? O4 C24 C23 106.1(4) . . ? O4 C24 H24A 110.5 . . ? C23 C24 H24A 110.5 . . ? O4 C24 H24B 110.5 . . ? C23 C24 H24B 110.5 . . ? H24A C24 H24B 108.7 . . ? O5 C25 C26 107.2(3) . . ? O5 C25 H25A 110.3 . . ? C26 C25 H25A 110.3 . . ? O5 C25 H25B 110.3 . . ? C26 C25 H25B 110.3 . . ? H25A C25 H25B 108.5 . . ? O6 C26 C25 109.3(3) . . ? O6 C26 H26A 109.8 . . ? C25 C26 H26A 109.8 . . ? O6 C26 H26B 109.8 . . ? C25 C26 H26B 109.8 . . ? H26A C26 H26B 108.3 . . ? O6 C27 C28 109.9(4) . . ? O6 C27 H27A 109.7 . . ? C28 C27 H27A 109.7 . . ? O6 C27 H27B 109.7 . . ? C28 C27 H27B 109.7 . . ? H27A C27 H27B 108.2 . . ? O7 C28 C27 111.0(5) . . ? O7 C28 H28A 109.4 . . ? C27 C28 H28A 109.4 . . ? O7 C28 H28B 109.4 . . ? C27 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C30 C29 O7 113.7(7) . . ? C30 C29 H29A 108.8 . . ? O7 C29 H29A 108.8 . . ? C30 C29 H29B 108.8 . . ? O7 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? C29 C30 O8 113.0(5) . . ? C29 C30 H30A 109.0 . . ? O8 C30 H30A 109.0 . . ? C29 C30 H30B 109.0 . . ? O8 C30 H30B 109.0 . . ? H30A C30 H30B 107.8 . . ? C32 C31 C31 110.8(5) . 3 ? C32 C31 H31A 109.5 . . ? C31 C31 H31A 109.5 3 . ? C32 C31 H31B 109.5 . . ? C31 C31 H31B 109.5 3 . ? H31A C31 H31B 108.1 . . ? C31 C32 C33 110.5(4) . . ? C31 C32 H32A 109.6 . . ? C33 C32 H32A 109.6 . . ? C31 C32 H32B 109.6 . . ? C33 C32 H32B 109.6 . . ? H32A C32 H32B 108.1 . . ? N1 C33 C32 111.1(4) . . ? N1 C33 H33A 109.4 . . ? C32 C33 H33A 109.4 . . ? N1 C33 H33B 109.4 . . ? C32 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? C35 C34 N1 111.1(4) . . ? C35 C34 H34A 109.4 . . ? N1 C34 H34A 109.4 . . ? C35 C34 H34B 109.4 . . ? N1 C34 H34B 109.4 . . ? H34A C34 H34B 108.0 . . ? C40 C35 C36 117.9(5) . . ? C40 C35 C34 122.4(5) . . ? C36 C35 C34 119.7(5) . . ? C37 C36 C35 122.2(6) . . ? C37 C36 H36A 118.9 . . ? C35 C36 H36A 118.9 . . ? C36 C37 C38 120.3(5) . . ? C40 C39 C38 117.5(6) . . ? C35 C40 C39 122.0(5) . . ? C35 C40 H40A 119.0 . . ? C39 C40 H40A 119.0 . . ? C37 C38 C39 120.1(6) . . ? C37 C38 C41 118.5(7) . . ? C39 C38 C41 121.2(8) . . ? C44 C41 C38 109.9(10) . . ? C44 C41 C42 114.0(14) . . ? C38 C41 C42 103.8(8) . . ? C44 C41 C43 117.6(11) . . ? C38 C41 C43 109.4(8) . . ? C42 C41 C43 101.2(12) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? F4 P1 F5 95.7(6) . . ? F4 P1 F3 90.4(6) . . ? F5 P1 F3 173.7(5) . . ? F4 P1 F6 175.0(7) . . ? F5 P1 F6 80.5(5) . . ? F3 P1 F6 93.5(6) . . ? F4 P1 F1 92.9(5) . . ? F5 P1 F1 88.5(3) . . ? F3 P1 F1 89.6(3) . . ? F6 P1 F1 90.2(5) . . ? F4 P1 F2 90.5(5) . . ? F5 P1 F2 94.6(4) . . ? F3 P1 F2 86.9(3) . . ? F6 P1 F2 86.5(5) . . ? F1 P1 F2 175.1(4) . . ? N11 C46 C47 176.8(7) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N12 C48 C49 177.6(12) . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? H1 O9 H2 107(5) . . ? C51 O10 C52 101.0 . . ? O10 C51 C50 120.6 . . ? O10 C52 C53 108.1 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 68.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.166 _refine_diff_density_min -0.841 _refine_diff_density_rms 0.080