# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Sheng-Hsien Chiu' _publ_contact_author_email SHCHIU@NTU.EDU.TW _publ_section_title ; Two Guest Complexation Modes in a Cyclotriveratrylene-Based Molecular Container ; loop_ _publ_author_name 'Sheng-Hsien Chiu.' 'Chien-Chen Lai.' 'Min-Jye Lee.' 'Yi-Hung Liu.' ; Shie-Ming Peng ; # Attachment 'B906075H-revised-722772.cif' data_ic13146 _database_code_depnum_ccdc_archive 'CCDC 722771' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C94 H110 F12 N2 O24 P2' _chemical_formula_sum 'C102 H122 F12 N6 O24 P2' _chemical_formula_weight 2106.00 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 Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 24.4430(6) _cell_length_b 110.268(3) _cell_length_c 15.7305(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 42398.0(19) _cell_formula_units_Z 16 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 11317 _cell_measurement_theta_min 3.2026 _cell_measurement_theta_max 75.7457 _exptl_crystal_description Cubes _exptl_crystal_colour colorless _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 1.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 17696 _exptl_absorpt_coefficient_mu 1.182 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7565 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 R' _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 70292 _diffrn_reflns_av_R_equivalents 0.1129 _diffrn_reflns_av_sigmaI/netI 0.0851 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -132 _diffrn_reflns_limit_k_max 123 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 67.99 _reflns_number_total 16751 _reflns_number_gt 8010 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) 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. Some atoms in the structure are modeled disorder and some solvent molecules are refined as isotropic. Because of the large correlation between thermal parameters, the restraint was necessary for convergence of the refinement process. In large supermolecular structure with poor data to parameter ratios, they often are needed with geometrical and anisotropic displacement parameters restraints. ; _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^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000048(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.06(5) _refine_ls_number_reflns 16751 _refine_ls_number_parameters 1277 _refine_ls_number_restraints 230 _refine_ls_R_factor_all 0.1689 _refine_ls_R_factor_gt 0.1111 _refine_ls_wR_factor_ref 0.2722 _refine_ls_wR_factor_gt 0.2548 _refine_ls_goodness_of_fit_ref 1.337 _refine_ls_restrained_S_all 1.384 _refine_ls_shift/su_max 0.035 _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 0.0536(2) 0.03921(6) -0.0345(4) 0.0698(16) Uani 1 1 d . . . O2 O 0.0844(3) 0.01513(9) 0.0017(6) 0.122(3) Uani 1 1 d . . . O3 O 0.1365(3) -0.00426(7) 0.0953(5) 0.097(2) Uani 1 1 d . . . O4 O 0.1962(3) 0.01000(6) 0.2137(5) 0.092(2) Uani 1 1 d . . . O5 O 0.0024(2) 0.05279(5) 0.0711(4) 0.0731(18) Uani 1 1 d . . . O6 O -0.0497(2) 0.04359(7) 0.2271(4) 0.0752(18) Uani 1 1 d . . . O7 O 0.0357(2) 0.02941(6) 0.2996(4) 0.0822(19) Uani 1 1 d . . . O8 O 0.1434(3) 0.02157(6) 0.3283(4) 0.0755(17) Uani 1 1 d . . . O9 O 0.1349(2) 0.10359(5) 0.2172(4) 0.0691(16) Uani 1 1 d . . . O10 O 0.1085(3) 0.09894(6) 0.3942(4) 0.0826(19) Uani 1 1 d . . . O11 O 0.1552(3) 0.08459(7) 0.5268(4) 0.088(2) Uani 1 1 d . . . O12 O 0.2576(3) 0.07177(6) 0.5141(4) 0.0825(19) Uani 1 1 d . . . O13 O 0.2282(2) 0.11134(5) 0.1561(4) 0.0725(17) Uani 1 1 d . . . O14 O 0.3294(5) 0.11684(7) 0.2359(6) 0.141(4) Uani 1 1 d U . . O15 O 0.3727(3) 0.10163(6) 0.3600(5) 0.087(2) Uani 1 1 d . . . O16 O 0.3499(2) 0.07891(6) 0.4431(5) 0.093(2) Uani 1 1 d . . . O17 O 0.3556(3) 0.07488(8) -0.1487(5) 0.102(2) Uani 1 1 d U A . O18 O 0.4663(3) 0.07279(8) -0.1275(6) 0.130(3) Uani 1 1 d U . . O19 O 0.5148(3) 0.05977(6) 0.0092(5) 0.088(2) Uani 1 1 d . . . O20 O 0.4790(3) 0.04127(8) 0.1284(5) 0.103(2) Uani 1 1 d . . . O21 O 0.3057(3) 0.05454(7) -0.1940(4) 0.0831(19) Uani 1 1 d . . . O22 O 0.3217(4) 0.02782(8) -0.1571(8) 0.144(4) Uani 1 1 d . . . O23 O 0.3736(7) 0.01374(9) -0.0452(7) 0.182(4) Uani 1 1 d U . . O24 O 0.4462(3) 0.01996(9) 0.0852(5) 0.105(3) Uani 1 1 d . . . N1 N 0.3870(3) 0.04844(7) 0.0008(5) 0.066(2) Uani 1 1 d . . . N2 N 0.2578(3) 0.08343(8) 0.3019(5) 0.075(2) Uani 1 1 d . . . C1 C 0.0599(3) 0.05141(9) -0.0460(5) 0.058(2) Uani 1 1 d . . . C2 C 0.0877(3) 0.05637(9) -0.1133(5) 0.062(2) Uani 1 1 d . . . H2A H 0.1037 0.0512 -0.1551 0.075 Uiso 1 1 calc R . . C3 C 0.0927(3) 0.06930(10) -0.1206(5) 0.064(3) Uani 1 1 d . . . C4 C 0.0663(3) 0.07668(8) -0.0618(5) 0.057(2) Uani 1 1 d . . . C5 C 0.0368(3) 0.07095(10) 0.0064(5) 0.064(2) Uani 1 1 d . . . H5A H 0.0189 0.0759 0.0473 0.076 Uiso 1 1 calc R . . C6 C 0.0337(3) 0.05876(9) 0.0142(5) 0.056(2) Uani 1 1 d . . . C7 C 0.0746(4) 0.03122(8) -0.0972(5) 0.064(2) Uani 1 1 d . . . H7A H 0.1150 0.0316 -0.0991 0.076 Uiso 1 1 calc R . . H7B H 0.0600 0.0333 -0.1541 0.076 Uiso 1 1 calc R . . C8 C 0.0559(4) 0.01873(10) -0.0709(7) 0.084(3) Uani 1 1 d . . . H8A H 0.0161 0.0188 -0.0589 0.101 Uiso 1 1 calc R . . H8B H 0.0626 0.0129 -0.1175 0.101 Uiso 1 1 calc R . . C9 C 0.0587(5) 0.00737(13) 0.0499(9) 0.110(4) Uani 1 1 d . . . H9A H 0.0474 0.0003 0.0152 0.132 Uiso 1 1 calc R . . H9B H 0.0253 0.0112 0.0730 0.132 Uiso 1 1 calc R . . C10 C 0.0937(5) 0.00306(9) 0.1221(7) 0.084(3) Uani 1 1 d . . . H10A H 0.1088 0.0102 0.1525 0.101 Uiso 1 1 calc R . . H10B H 0.0707 -0.0015 0.1627 0.101 Uiso 1 1 calc R . . C11 C 0.1839(5) 0.00234(12) 0.0750(7) 0.109(4) Uani 1 1 d D . . H11A H 0.1733 0.0106 0.0576 0.130 Uiso 1 1 calc R . . H11B H 0.2021 -0.0016 0.0259 0.130 Uiso 1 1 calc R . . C12 C 0.2225(5) 0.00312(13) 0.1451(7) 0.119(5) Uani 1 1 d D . . H12A H 0.2564 0.0073 0.1264 0.143 Uiso 1 1 calc R . . H12B H 0.2323 -0.0051 0.1651 0.143 Uiso 1 1 calc R . . C13 C -0.0326(4) 0.05979(9) 0.1260(7) 0.088(3) Uani 1 1 d . . . H13A H -0.0525 0.0660 0.0922 0.105 Uiso 1 1 calc R . . H13B H -0.0103 0.0640 0.1692 0.105 Uiso 1 1 calc R . . C14 C -0.0724(4) 0.05164(11) 0.1685(7) 0.092(3) Uani 1 1 d . . . H14A H -0.1000 0.0567 0.1981 0.110 Uiso 1 1 calc R . . H14B H -0.0918 0.0469 0.1244 0.110 Uiso 1 1 calc R . . C15 C -0.0314(4) 0.03251(10) 0.1927(7) 0.087(3) Uani 1 1 d . . . H15A H 0.0000 0.0339 0.1541 0.104 Uiso 1 1 calc R . . H15B H -0.0611 0.0286 0.1596 0.104 Uiso 1 1 calc R . . C16 C -0.0139(4) 0.02418(10) 0.2670(6) 0.083(3) Uani 1 1 d . . . H16A H -0.0425 0.0240 0.3115 0.100 Uiso 1 1 calc R . . H16B H -0.0073 0.0158 0.2466 0.100 Uiso 1 1 calc R . . C17 C 0.0528(4) 0.02301(11) 0.3727(7) 0.092(3) Uani 1 1 d . . . H17A H 0.0505 0.0142 0.3622 0.110 Uiso 1 1 calc R . . H17B H 0.0287 0.0250 0.4212 0.110 Uiso 1 1 calc R . . C18 C 0.1103(4) 0.02642(10) 0.3931(6) 0.078(3) Uani 1 1 d . . . H18A H 0.1142 0.0354 0.3951 0.094 Uiso 1 1 calc R . . H18B H 0.1211 0.0231 0.4489 0.094 Uiso 1 1 calc R . . C19 C 0.2263(4) 0.01384(8) 0.2819(6) 0.066(2) Uani 1 1 d . . . C20 C 0.2812(4) 0.01135(8) 0.2963(6) 0.070(2) Uani 1 1 d . . . H20A H 0.3006 0.0065 0.2564 0.084 Uiso 1 1 calc R . . C21 C 0.3080(4) 0.01564(9) 0.3659(7) 0.074(3) Uani 1 1 d . . . C22 C 0.2803(3) 0.02298(8) 0.4259(6) 0.064(2) Uani 1 1 d U . . C23 C 0.2264(3) 0.02498(7) 0.4133(6) 0.060(2) Uani 1 1 d U . . H23A H 0.2072 0.0298 0.4533 0.071 Uiso 1 1 calc R . . C24 C 0.1979(3) 0.02032(8) 0.3448(5) 0.060(2) Uani 1 1 d . . . C25 C 0.0692(3) 0.09022(7) -0.0635(5) 0.055(2) Uani 1 1 d . . . H25A H 0.0341 0.0936 -0.0423 0.065 Uiso 1 1 calc R . . H25B H 0.0738 0.0929 -0.1230 0.065 Uiso 1 1 calc R . . C26 C 0.1151(3) 0.09524(7) -0.0109(6) 0.059(2) Uani 1 1 d . . . C27 C 0.1059(3) 0.09635(7) 0.0777(6) 0.057(2) Uani 1 1 d . . . H27A H 0.0728 0.0933 0.1011 0.068 Uiso 1 1 calc R . . C28 C 0.1442(4) 0.10178(8) 0.1314(6) 0.063(2) Uani 1 1 d . . . C29 C 0.1938(4) 0.10575(8) 0.0989(7) 0.067(2) Uani 1 1 d . . . C30 C 0.2055(4) 0.10396(9) 0.0139(7) 0.080(3) Uani 1 1 d . . . H30A H 0.2406 0.1061 -0.0075 0.096 Uiso 1 1 calc R . . C31 C 0.1658(3) 0.09892(7) -0.0423(6) 0.059(2) Uani 1 1 d . . . C32 C 0.1829(4) 0.09769(9) -0.1361(6) 0.074(3) Uani 1 1 d . . . H32A H 0.1499 0.0983 -0.1723 0.089 Uiso 1 1 calc R . . H32B H 0.2074 0.1045 -0.1510 0.089 Uiso 1 1 calc R . . C33 C 0.0832(4) 0.10070(10) 0.2509(6) 0.079(3) Uani 1 1 d . . . H33A H 0.0786 0.0918 0.2511 0.094 Uiso 1 1 calc R . . H33B H 0.0545 0.1042 0.2138 0.094 Uiso 1 1 calc R . . C34 C 0.0760(4) 0.10533(10) 0.3378(6) 0.081(3) Uani 1 1 d . . . H34A H 0.0859 0.1140 0.3397 0.097 Uiso 1 1 calc R . . H34B H 0.0371 0.1045 0.3547 0.097 Uiso 1 1 calc R . . C35 C 0.0964(4) 0.10102(11) 0.4818(6) 0.086(3) Uani 1 1 d . . . H35A H 0.0925 0.1099 0.4904 0.103 Uiso 1 1 calc R . . H35B H 0.0605 0.0973 0.4945 0.103 Uiso 1 1 calc R . . C36 C 0.1345(7) 0.09667(13) 0.5412(8) 0.128(5) Uani 1 1 d . . . H36A H 0.1173 0.0969 0.5982 0.154 Uiso 1 1 calc R . . H36B H 0.1660 0.1023 0.5424 0.154 Uiso 1 1 calc R . . C37 C 0.1858(7) 0.07986(13) 0.5895(7) 0.127(5) Uani 1 1 d . . . H37A H 0.1619 0.0783 0.6393 0.152 Uiso 1 1 calc R . . H37B H 0.2134 0.0859 0.6067 0.152 Uiso 1 1 calc R . . C38 C 0.2127(5) 0.06911(11) 0.5692(8) 0.105(4) Uani 1 1 d . . . H38A H 0.1871 0.0635 0.5406 0.126 Uiso 1 1 calc R . . H38B H 0.2262 0.0652 0.6216 0.126 Uiso 1 1 calc R . . C39 C 0.2714(4) 0.11851(9) 0.1176(7) 0.079(3) Uani 1 1 d . . . H39A H 0.2559 0.1243 0.0757 0.095 Uiso 1 1 calc R . . H39B H 0.2979 0.1132 0.0881 0.095 Uiso 1 1 calc R . . C40 C 0.2980(5) 0.12503(10) 0.1867(8) 0.098(4) Uani 1 1 d . . . H40A H 0.3220 0.1314 0.1632 0.118 Uiso 1 1 calc R . . H40B H 0.2700 0.1290 0.2230 0.118 Uiso 1 1 calc R . . C41 C 0.3429(9) 0.12041(12) 0.3098(12) 0.169(6) Uani 1 1 d U . . H41A H 0.3088 0.1207 0.3438 0.203 Uiso 1 1 calc R . . H41B H 0.3556 0.1289 0.3039 0.203 Uiso 1 1 calc R . . C42 C 0.3821(5) 0.11434(11) 0.3597(9) 0.105(4) Uani 1 1 d . . . H42A H 0.3805 0.1174 0.4187 0.125 Uiso 1 1 calc R . . H42B H 0.4191 0.1160 0.3370 0.125 Uiso 1 1 calc R . . C43 C 0.4079(6) 0.09564(12) 0.4147(10) 0.141(6) Uani 1 1 d . . . H43A H 0.4003 0.0983 0.4737 0.169 Uiso 1 1 calc R . . H43B H 0.4460 0.0980 0.4010 0.169 Uiso 1 1 calc R . . C44 C 0.4028(4) 0.08300(11) 0.4097(10) 0.116(5) Uani 1 1 d . . . H44A H 0.4327 0.0792 0.4425 0.139 Uiso 1 1 calc R . . H44B H 0.4064 0.0804 0.3496 0.139 Uiso 1 1 calc R . . C45 C 0.2957(4) 0.06281(10) 0.4929(6) 0.074(3) Uani 1 1 d . . . C46 C 0.2850(4) 0.05073(9) 0.5080(5) 0.060(2) Uani 1 1 d . . . H46A H 0.2514 0.0484 0.5337 0.072 Uiso 1 1 calc R . . C47 C 0.3230(4) 0.04185(10) 0.4860(6) 0.071(3) Uani 1 1 d . . . C48 C 0.3724(4) 0.04543(10) 0.4459(6) 0.073(3) Uani 1 1 d . . . C49 C 0.3820(4) 0.05750(12) 0.4318(7) 0.081(3) Uani 1 1 d . . . H49A H 0.4154 0.0600 0.4068 0.097 Uiso 1 1 calc R . . C50 C 0.3445(5) 0.06565(11) 0.4532(7) 0.088(3) Uani 1 1 d . . . C51 C 0.3075(4) 0.02902(9) 0.5028(6) 0.073(3) Uani 1 1 d . . . H51A H 0.2820 0.0288 0.5517 0.088 Uiso 1 1 calc R . . H51B H 0.3407 0.0244 0.5184 0.088 Uiso 1 1 calc R . . C52 C 0.4188(4) 0.03733(11) 0.4324(7) 0.092(3) Uani 1 1 d . . . H52A H 0.4168 0.0306 0.4736 0.111 Uiso 1 1 calc R . . H52B H 0.4531 0.0418 0.4435 0.111 Uiso 1 1 calc R . . C53 C 0.3686(4) 0.01268(10) 0.3715(7) 0.084(3) Uani 1 1 d . . . H53A H 0.3745 0.0041 0.3548 0.100 Uiso 1 1 calc R . . H53B H 0.3810 0.0137 0.4310 0.100 Uiso 1 1 calc R . . C54 C 0.1243(3) 0.07383(9) -0.1939(5) 0.065(2) Uani 1 1 d . . . H54A H 0.1101 0.0819 -0.2097 0.078 Uiso 1 1 calc R . . H54B H 0.1179 0.0683 -0.2428 0.078 Uiso 1 1 calc R . . C55 C 0.1862(4) 0.07485(10) -0.1792(5) 0.069(3) Uani 1 1 d . A . C56 C 0.2121(4) 0.08577(9) -0.1557(6) 0.071(3) Uani 1 1 d . . . C57 C 0.2695(4) 0.08514(11) -0.1454(6) 0.072(3) Uani 1 1 d . A . H57A H 0.2882 0.0923 -0.1289 0.086 Uiso 1 1 calc R . . C58 C 0.2987(4) 0.07532(10) -0.1570(6) 0.069(3) Uani 1 1 d . . . C59 C 0.2728(4) 0.06446(10) -0.1836(5) 0.066(2) Uani 1 1 d . A . C60 C 0.2163(3) 0.06448(10) -0.1923(6) 0.071(3) Uani 1 1 d . . . H60A H 0.1980 0.0572 -0.2075 0.086 Uiso 1 1 calc R A . C61 C 0.3872(5) 0.08191(13) -0.1836(11) 0.131(4) Uani 1 1 d U . . H61A H 0.3784 0.0900 -0.1607 0.158 Uiso 1 1 calc R A . H61B H 0.3764 0.0820 -0.2442 0.158 Uiso 1 1 calc R . . C62 C 0.4428(4) 0.08114(10) -0.1833(8) 0.089(3) Uani 1 1 d U A . H62A H 0.4577 0.0893 -0.1696 0.107 Uiso 1 1 calc R . . H62B H 0.4550 0.0791 -0.2416 0.107 Uiso 1 1 calc R . . C63 C 0.5194(4) 0.07004(12) -0.1230(8) 0.105(3) Uani 1 1 d U . . H63A H 0.5385 0.0780 -0.1204 0.126 Uiso 1 1 calc R . . H63B H 0.5285 0.0665 -0.1792 0.126 Uiso 1 1 calc R . . C64 C 0.5453(5) 0.06296(14) -0.0661(10) 0.141(5) Uani 1 1 d U . . H64A H 0.5792 0.0672 -0.0481 0.169 Uiso 1 1 calc R . . H64B H 0.5563 0.0554 -0.0950 0.169 Uiso 1 1 calc R . . C65 C 0.5463(4) 0.05480(12) 0.0732(8) 0.096(3) Uani 1 1 d . . . H65A H 0.5750 0.0607 0.0903 0.115 Uiso 1 1 calc R . . H65B H 0.5646 0.0474 0.0520 0.115 Uiso 1 1 calc R . . C66 C 0.5112(6) 0.05170(12) 0.1490(8) 0.123(5) Uani 1 1 d . . . H66A H 0.5346 0.0500 0.1989 0.148 Uiso 1 1 calc R . . H66B H 0.4871 0.0586 0.1632 0.148 Uiso 1 1 calc R . . C67 C 0.2792(5) 0.04394(12) -0.2302(7) 0.102(3) Uani 0.50 1 d PU A 1 H67A H 0.2635 0.0463 -0.2859 0.122 Uiso 0.50 1 calc PR A 1 H67B H 0.2483 0.0417 -0.1927 0.122 Uiso 0.50 1 calc PR A 1 C68 C 0.3152(10) 0.0326(2) -0.2436(13) 0.092(5) Uani 0.50 1 d PU A 1 H68A H 0.2968 0.0266 -0.2809 0.111 Uiso 0.50 1 calc PR A 1 H68B H 0.3510 0.0348 -0.2687 0.111 Uiso 0.50 1 calc PR A 1 C67' C 0.2792(5) 0.04394(12) -0.2302(7) 0.102(3) Uani 0.50 1 d PU A 2 H67C H 0.2451 0.0463 -0.2597 0.122 Uiso 0.50 1 calc PR A 2 H67D H 0.3037 0.0400 -0.2719 0.122 Uiso 0.50 1 calc PR A 2 C68' C 0.2682(12) 0.0365(3) -0.1680(18) 0.127(5) Uani 0.50 1 d PU A 2 H68C H 0.2354 0.0316 -0.1815 0.153 Uiso 0.50 1 calc PR A 2 H68D H 0.2612 0.0411 -0.1149 0.153 Uiso 0.50 1 calc PR A 2 C69 C 0.3116(9) 0.01755(17) -0.1572(11) 0.180(5) Uani 1 1 d U A . H69A H 0.3336 0.0136 -0.2023 0.216 Uiso 1 1 calc R . . H69B H 0.2726 0.0166 -0.1729 0.216 Uiso 1 1 calc R . . C70 C 0.3209(10) 0.01101(15) -0.0783(12) 0.194(5) Uani 1 1 d U . . H70A H 0.2926 0.0133 -0.0362 0.232 Uiso 1 1 calc R A . H70B H 0.3180 0.0022 -0.0887 0.232 Uiso 1 1 calc R . . C71 C 0.3767(9) 0.00707(18) 0.0253(13) 0.197(6) Uani 1 1 d DU . . H71A H 0.3682 -0.0015 0.0118 0.237 Uiso 1 1 calc R A . H71B H 0.3495 0.0100 0.0672 0.237 Uiso 1 1 calc R . . C72 C 0.4298(8) 0.00787(12) 0.0603(10) 0.149(5) Uani 1 1 d DU A . H72A H 0.4563 0.0048 0.0181 0.179 Uiso 1 1 calc R . . H72B H 0.4317 0.0025 0.1108 0.179 Uiso 1 1 calc R . . C73 C 0.4350(5) 0.02346(14) 0.1679(8) 0.094(4) Uani 1 1 d . . . C74 C 0.4534(4) 0.03483(14) 0.1914(7) 0.087(4) Uani 1 1 d . . . C75 C 0.4496(4) 0.03896(12) 0.2714(8) 0.096(4) Uani 1 1 d . . . H75A H 0.4654 0.0465 0.2867 0.115 Uiso 1 1 calc R . . C76 C 0.4210(4) 0.03166(12) 0.3344(6) 0.078(3) Uani 1 1 d . . . C77 C 0.4025(4) 0.02092(12) 0.3139(7) 0.080(3) Uani 1 1 d . . . C78 C 0.4121(4) 0.01659(14) 0.2291(7) 0.103(4) Uani 1 1 d . . . H78A H 0.4018 0.0085 0.2155 0.124 Uiso 1 1 calc R . . C79 C 0.3935(4) 0.06027(8) 0.0037(7) 0.071(3) Uani 1 1 d . . . H79A H 0.4157 0.0639 -0.0388 0.086 Uiso 1 1 calc R . . C80 C 0.3705(3) 0.06768(8) 0.0639(7) 0.064(2) Uani 1 1 d . . . C81 C 0.3397(3) 0.06198(8) 0.1274(6) 0.060(2) Uani 1 1 d . . . C82 C 0.3333(3) 0.04892(7) 0.1289(5) 0.054(2) Uani 1 1 d . . . C83 C 0.3581(3) 0.04239(9) 0.0641(6) 0.067(2) Uani 1 1 d . . . H83A H 0.3554 0.0338 0.0630 0.081 Uiso 1 1 calc R . . C84 C 0.3754(4) 0.08024(9) 0.0574(8) 0.092(3) Uani 1 1 d . . . H84A H 0.3950 0.0838 0.0117 0.111 Uiso 1 1 calc R . . C85 C 0.3511(4) 0.08732(10) 0.1189(7) 0.087(3) Uani 1 1 d . . . H85A H 0.3556 0.0959 0.1174 0.105 Uiso 1 1 calc R . . C86 C 0.3186(3) 0.08185(8) 0.1860(6) 0.063(2) Uani 1 1 d . . . C87 C 0.3146(3) 0.06921(8) 0.1862(6) 0.060(2) Uani 1 1 d . . . C88 C 0.2816(4) 0.06351(9) 0.2521(6) 0.068(2) Uani 1 1 d . . . C89 C 0.2799(4) 0.04985(10) 0.2548(6) 0.079(3) Uani 1 1 d . . . H89A H 0.2607 0.0459 0.2994 0.095 Uiso 1 1 calc R . . C90 C 0.3041(4) 0.04340(9) 0.1972(6) 0.068(2) Uani 1 1 d . . . H90A H 0.3025 0.0348 0.2006 0.082 Uiso 1 1 calc R . . C91 C 0.2902(3) 0.08836(8) 0.2447(6) 0.067(2) Uani 1 1 d . . . H91A H 0.2939 0.0969 0.2445 0.081 Uiso 1 1 calc R . . C92 C 0.2553(4) 0.07121(10) 0.3089(6) 0.075(3) Uani 1 1 d . . . H92A H 0.2347 0.0678 0.3541 0.090 Uiso 1 1 calc R . . C93 C 0.4131(4) 0.04115(9) -0.0647(6) 0.074(3) Uani 1 1 d . . . H93A H 0.4321 0.0465 -0.1048 0.112 Uiso 1 1 calc R . . H93B H 0.3853 0.0364 -0.0950 0.112 Uiso 1 1 calc R . . H93C H 0.4395 0.0356 -0.0383 0.112 Uiso 1 1 calc R . . C94 C 0.2277(4) 0.09148(10) 0.3630(6) 0.083(3) Uani 1 1 d . . . H94A H 0.2345 0.1000 0.3484 0.125 Uiso 1 1 calc R . . H94B H 0.2406 0.0899 0.4209 0.125 Uiso 1 1 calc R . . H94C H 0.1884 0.0898 0.3595 0.125 Uiso 1 1 calc R . . P1 P 0.38670(15) 0.11788(3) 0.9183(3) 0.1045(11) Uani 1 1 d D . . F1 F 0.3975(5) 0.12901(8) 0.8644(6) 0.244(6) Uani 1 1 d D . . F2 F 0.3721(6) 0.10671(7) 0.9652(6) 0.242(6) Uani 1 1 d D . . F3 F 0.3860(5) 0.11013(9) 0.8345(5) 0.235(6) Uani 1 1 d D . . F4 F 0.4437(3) 0.11506(13) 0.9293(7) 0.279(8) Uani 1 1 d D . . F5 F 0.3831(5) 0.12473(8) 0.9982(6) 0.211(5) Uani 1 1 d D . . F6 F 0.3259(4) 0.11922(15) 0.9062(9) 0.355(12) Uani 1 1 d D . . P2 P 0.14674(12) 0.02575(3) 0.66870(19) 0.0842(8) Uani 1 1 d D . . F7 F 0.1386(4) 0.03709(7) 0.7227(5) 0.178(4) Uani 1 1 d D . . F8 F 0.1623(4) 0.01520(7) 0.6101(7) 0.194(5) Uani 1 1 d D . . F9 F 0.2088(3) 0.02733(10) 0.6718(8) 0.226(6) Uani 1 1 d D . . F10 F 0.1539(5) 0.03426(9) 0.5931(5) 0.220(6) Uani 1 1 d D . . F11 F 0.0913(3) 0.02456(10) 0.6482(10) 0.359(14) Uani 1 1 d D . . F12 F 0.1488(6) 0.01806(11) 0.7396(6) 0.390(14) Uani 1 1 d D . . N3 N 0.4590(4) 0.09923(10) 0.6250(7) 0.120(3) Uiso 1 1 d D . . C95 C 0.4497(5) 0.10950(12) 0.6357(8) 0.107(4) Uiso 1 1 d D . . C96 C 0.4402(7) 0.12207(14) 0.6535(13) 0.167(6) Uiso 1 1 d D . . H96A H 0.4008 0.1235 0.6591 0.250 Uiso 1 1 calc R . . H96B H 0.4547 0.1270 0.6070 0.250 Uiso 1 1 calc R . . H96C H 0.4585 0.1243 0.7067 0.250 Uiso 1 1 calc R . . N4 N 0.5396(6) 0.13563(14) 0.7802(11) 0.173(5) Uiso 1 1 d . . . C97 C 0.5361(7) 0.13929(15) 0.8516(14) 0.146(5) Uiso 1 1 d . . . C98 C 0.5268(9) 0.1418(2) 0.9405(15) 0.208(8) Uiso 1 1 d . . . H98A H 0.5373 0.1502 0.9529 0.312 Uiso 1 1 calc R . . H98B H 0.5488 0.1363 0.9752 0.312 Uiso 1 1 calc R . . H98C H 0.4880 0.1407 0.9538 0.312 Uiso 1 1 calc R . . N5 N 0.1293(6) 0.03864(14) 0.1584(10) 0.161(5) Uiso 1 1 d D . . C99 C 0.1266(9) 0.04740(18) 0.2019(14) 0.201(9) Uiso 1 1 d D . . C100 C 0.1331(9) 0.05892(19) 0.2416(16) 0.231(10) Uiso 1 1 d D . . H10F H 0.1259 0.0582 0.3027 0.346 Uiso 1 1 calc R . . H10G H 0.1073 0.0647 0.2167 0.346 Uiso 1 1 calc R . . H10H H 0.1706 0.0618 0.2329 0.346 Uiso 1 1 calc R . . N7 N 0.2550(11) 0.1564(3) 0.9605(19) 0.158(10) Uiso 0.50 1 d P . . C101 C 0.2488(10) 0.1475(2) 0.9426(17) 0.100(7) Uiso 0.50 1 d P . . C102 C 0.2245(8) 0.14083(18) 0.8833(13) 0.079(6) Uiso 0.50 1 d P . . H10C H 0.2297 0.1322 0.8963 0.119 Uiso 0.50 1 calc PR . . H10D H 0.2406 0.1427 0.8277 0.119 Uiso 0.50 1 calc PR . . H10E H 0.1853 0.1427 0.8822 0.119 Uiso 0.50 1 calc PR . . C104 C 0.1947(6) 0.06904(14) 0.0482(10) 0.049(4) Uiso 0.50 1 d P . . H10I H 0.2114 0.0755 0.0139 0.074 Uiso 0.50 1 calc PR . . H10J H 0.2037 0.0703 0.1082 0.074 Uiso 0.50 1 calc PR . . H10K H 0.1549 0.0692 0.0409 0.074 Uiso 0.50 1 calc PR . . C103 C 0.2103(9) 0.0602(2) 0.0276(15) 0.095(7) Uiso 0.50 1 d P . . N6 N 0.2159(10) 0.0478(3) 0.0115(17) 0.150(9) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.065(4) 0.082(4) 0.062(4) -0.016(3) 0.021(3) -0.006(3) O2 0.077(5) 0.156(8) 0.133(8) 0.047(7) 0.013(5) 0.038(5) O3 0.117(6) 0.083(5) 0.093(5) -0.018(4) 0.004(5) -0.015(5) O4 0.081(5) 0.095(5) 0.100(5) -0.046(4) 0.000(4) 0.017(4) O5 0.072(4) 0.079(4) 0.069(4) -0.022(3) 0.042(3) -0.006(3) O6 0.069(4) 0.107(5) 0.050(4) -0.006(4) 0.009(3) 0.009(4) O7 0.061(4) 0.117(5) 0.069(4) 0.012(4) -0.005(3) -0.009(4) O8 0.068(4) 0.096(5) 0.062(4) -0.019(3) 0.000(3) 0.007(3) O9 0.069(4) 0.078(4) 0.060(4) -0.003(3) 0.004(3) -0.008(3) O10 0.102(5) 0.090(5) 0.056(4) -0.018(3) -0.008(4) 0.010(4) O11 0.100(5) 0.097(5) 0.067(4) -0.024(4) 0.023(4) 0.011(4) O12 0.085(5) 0.079(5) 0.083(5) 0.013(4) 0.000(4) -0.004(4) O13 0.068(4) 0.073(4) 0.077(4) 0.006(3) -0.024(3) -0.012(3) O14 0.225(9) 0.082(5) 0.116(7) 0.022(5) -0.081(7) -0.060(6) O15 0.087(5) 0.085(5) 0.090(5) 0.015(4) -0.028(4) -0.019(4) O16 0.061(4) 0.102(5) 0.116(6) 0.029(5) -0.024(4) -0.023(4) O17 0.051(4) 0.142(6) 0.115(5) 0.061(5) 0.000(4) -0.006(4) O18 0.064(4) 0.137(6) 0.189(7) 0.077(5) 0.031(5) 0.013(4) O19 0.077(5) 0.096(5) 0.090(5) 0.016(4) 0.019(4) -0.008(4) O20 0.067(4) 0.138(7) 0.104(6) 0.015(5) -0.009(4) -0.008(4) O21 0.060(4) 0.107(5) 0.082(5) 0.003(4) 0.016(3) 0.002(4) O22 0.170(9) 0.068(5) 0.194(10) 0.027(6) -0.075(8) -0.022(5) O23 0.315(11) 0.101(6) 0.131(7) 0.025(6) -0.082(8) -0.026(7) O24 0.083(5) 0.166(8) 0.067(5) 0.024(5) 0.002(4) 0.008(5) N1 0.040(4) 0.086(6) 0.070(5) -0.018(4) 0.007(4) -0.005(4) N2 0.082(6) 0.094(6) 0.050(4) 0.005(4) 0.009(4) -0.020(5) C1 0.051(5) 0.078(6) 0.046(5) -0.010(5) 0.001(4) -0.004(4) C2 0.037(4) 0.096(7) 0.054(5) -0.015(5) -0.007(4) 0.014(5) C3 0.027(4) 0.125(8) 0.041(5) -0.001(5) -0.005(4) 0.001(5) C4 0.035(4) 0.087(6) 0.048(5) 0.001(5) 0.000(4) -0.001(4) C5 0.036(4) 0.104(8) 0.051(5) -0.026(5) -0.004(4) 0.011(5) C6 0.045(5) 0.075(6) 0.049(5) -0.014(5) 0.008(4) -0.008(4) C7 0.084(6) 0.064(6) 0.043(5) -0.015(4) 0.008(4) 0.030(5) C8 0.075(7) 0.108(8) 0.071(7) -0.037(7) 0.004(6) 0.031(6) C9 0.094(9) 0.122(10) 0.114(11) 0.006(9) 0.038(8) 0.013(8) C10 0.101(8) 0.073(7) 0.078(7) 0.001(6) 0.011(6) 0.004(6) C11 0.126(10) 0.117(10) 0.082(8) -0.047(7) 0.018(8) -0.040(8) C12 0.106(9) 0.168(12) 0.083(8) -0.073(9) 0.006(7) 0.007(8) C13 0.083(7) 0.096(7) 0.084(7) -0.025(6) 0.067(6) -0.004(6) C14 0.060(6) 0.128(9) 0.086(8) -0.011(7) 0.018(6) -0.001(6) C15 0.064(6) 0.107(8) 0.090(8) -0.009(7) 0.006(6) 0.014(6) C16 0.085(7) 0.105(8) 0.060(6) -0.012(6) -0.018(5) -0.011(6) C17 0.086(8) 0.114(9) 0.076(7) 0.010(7) 0.002(6) -0.007(6) C18 0.073(7) 0.102(7) 0.060(6) -0.011(5) 0.004(5) 0.012(6) C19 0.065(6) 0.068(6) 0.065(6) -0.011(5) -0.010(5) 0.007(5) C20 0.084(7) 0.064(6) 0.061(6) -0.003(5) -0.001(5) 0.012(5) C21 0.056(5) 0.084(7) 0.083(7) 0.034(6) -0.011(5) 0.016(5) C22 0.058(5) 0.073(6) 0.062(5) 0.027(5) 0.009(4) 0.007(4) C23 0.059(5) 0.063(5) 0.056(5) 0.011(4) 0.011(4) 0.008(4) C24 0.055(5) 0.077(6) 0.047(5) -0.005(5) 0.001(4) 0.018(4) C25 0.040(4) 0.072(6) 0.052(5) 0.004(4) -0.005(4) 0.006(4) C26 0.059(5) 0.038(4) 0.081(7) 0.004(4) 0.012(5) 0.007(4) C27 0.054(5) 0.060(5) 0.057(5) 0.014(4) -0.005(4) 0.000(4) C28 0.081(7) 0.050(5) 0.058(6) 0.007(4) -0.007(5) -0.002(5) C29 0.069(6) 0.054(5) 0.077(7) 0.008(5) -0.024(5) -0.009(4) C30 0.070(6) 0.072(7) 0.098(9) 0.010(6) -0.018(6) 0.005(5) C31 0.056(5) 0.054(5) 0.068(6) 0.012(4) -0.001(4) -0.007(4) C32 0.067(6) 0.091(7) 0.063(6) 0.012(5) -0.005(5) 0.007(5) C33 0.072(7) 0.103(8) 0.061(6) -0.022(6) 0.004(5) -0.006(6) C34 0.069(6) 0.112(8) 0.063(6) -0.019(6) -0.004(5) -0.006(6) C35 0.076(7) 0.128(9) 0.054(6) -0.017(6) 0.005(5) 0.010(6) C36 0.205(16) 0.118(11) 0.063(7) -0.005(7) 0.030(9) 0.037(10) C37 0.196(14) 0.135(11) 0.050(6) 0.024(7) 0.017(8) 0.070(11) C38 0.124(10) 0.107(9) 0.085(8) 0.032(7) 0.053(7) 0.010(7) C39 0.065(6) 0.079(6) 0.094(7) 0.014(6) -0.010(6) -0.021(5) C40 0.111(9) 0.073(7) 0.110(9) -0.003(7) -0.042(7) -0.022(6) C41 0.267(16) 0.071(8) 0.168(13) -0.014(9) -0.075(13) -0.038(10) C42 0.109(9) 0.089(8) 0.116(10) -0.012(8) -0.036(8) -0.020(7) C43 0.124(10) 0.132(11) 0.167(13) 0.080(10) -0.103(10) -0.058(9) C44 0.056(7) 0.109(9) 0.183(14) 0.067(10) -0.026(7) 0.002(6) C45 0.057(6) 0.098(8) 0.068(6) 0.011(6) -0.019(5) -0.011(6) C46 0.058(5) 0.074(6) 0.048(5) 0.004(5) -0.011(4) -0.005(5) C47 0.054(6) 0.101(8) 0.059(6) 0.025(5) -0.024(5) -0.007(5) C48 0.060(6) 0.089(7) 0.071(7) 0.021(6) -0.010(5) 0.010(5) C49 0.052(6) 0.117(9) 0.075(7) 0.006(7) -0.003(5) -0.009(6) C50 0.088(8) 0.107(9) 0.069(7) 0.015(6) -0.023(6) -0.038(7) C51 0.069(6) 0.089(7) 0.061(6) 0.020(5) -0.008(5) 0.005(5) C52 0.053(6) 0.136(9) 0.088(8) 0.035(7) -0.002(5) 0.000(6) C53 0.071(6) 0.113(8) 0.067(6) 0.023(6) -0.003(5) 0.040(6) C54 0.056(5) 0.090(6) 0.048(5) 0.003(5) -0.015(4) 0.005(5) C55 0.056(5) 0.114(8) 0.036(4) 0.013(5) 0.006(4) -0.003(6) C56 0.070(6) 0.090(7) 0.053(5) -0.002(5) 0.007(5) -0.012(5) C57 0.044(5) 0.114(8) 0.058(6) 0.004(6) -0.003(4) -0.007(5) C58 0.048(5) 0.106(8) 0.052(5) 0.019(5) 0.003(4) 0.004(6) C59 0.060(6) 0.091(7) 0.046(5) -0.002(5) 0.009(4) -0.002(5) C60 0.041(5) 0.109(8) 0.064(6) 0.008(6) -0.003(4) -0.004(5) C61 0.065(7) 0.121(8) 0.208(10) 0.061(8) 0.013(7) 0.000(6) C62 0.052(5) 0.093(6) 0.122(7) 0.054(6) 0.011(5) 0.002(5) C63 0.058(6) 0.135(8) 0.121(8) 0.031(7) 0.006(6) -0.003(6) C64 0.102(8) 0.165(11) 0.157(11) 0.102(10) 0.055(8) 0.045(8) C65 0.062(7) 0.117(9) 0.109(9) 0.029(8) -0.008(6) -0.002(6) C66 0.164(12) 0.112(10) 0.094(9) 0.028(8) -0.057(9) -0.035(9) C67 0.109(7) 0.117(8) 0.079(6) 0.001(6) 0.039(6) 0.021(6) C68 0.108(10) 0.104(10) 0.064(9) 0.024(9) 0.022(8) 0.015(9) C67' 0.109(7) 0.117(8) 0.079(6) 0.001(6) 0.039(6) 0.021(6) C68' 0.154(11) 0.129(11) 0.099(10) 0.023(10) 0.010(10) 0.001(10) C69 0.270(11) 0.150(9) 0.120(9) 0.024(8) -0.052(9) -0.048(9) C70 0.323(14) 0.132(9) 0.126(10) 0.020(8) -0.059(10) -0.108(10) C71 0.322(15) 0.130(9) 0.140(11) 0.000(9) -0.042(11) -0.049(11) C72 0.264(15) 0.069(7) 0.113(10) 0.000(7) -0.023(10) -0.014(10) C73 0.076(7) 0.134(11) 0.073(8) 0.038(8) 0.000(6) -0.003(7) C74 0.041(5) 0.159(12) 0.061(7) 0.059(8) 0.001(5) 0.010(6) C75 0.066(7) 0.128(10) 0.093(9) 0.026(8) -0.035(6) -0.003(6) C76 0.055(6) 0.113(9) 0.064(6) 0.008(7) -0.015(5) 0.014(6) C77 0.068(6) 0.106(8) 0.065(7) 0.027(6) 0.003(5) 0.015(6) C78 0.086(8) 0.149(11) 0.074(8) 0.015(8) -0.010(6) 0.033(7) C79 0.069(6) 0.044(5) 0.101(8) 0.017(5) 0.026(5) 0.002(4) C80 0.046(5) 0.051(5) 0.096(7) 0.003(5) 0.007(5) 0.001(4) C81 0.061(5) 0.064(5) 0.055(5) 0.000(5) 0.010(4) 0.003(4) C82 0.057(5) 0.052(5) 0.055(5) 0.000(4) 0.010(4) -0.008(4) C83 0.055(5) 0.073(6) 0.074(6) 0.011(5) 0.003(5) -0.005(5) C84 0.095(8) 0.070(7) 0.112(9) 0.018(6) 0.041(7) -0.002(6) C85 0.106(8) 0.074(6) 0.082(7) 0.000(6) 0.037(6) 0.008(6) C86 0.049(5) 0.066(6) 0.073(6) 0.012(5) 0.012(4) 0.014(4) C87 0.061(5) 0.059(5) 0.060(5) -0.001(5) 0.002(4) -0.001(4) C88 0.065(6) 0.079(6) 0.059(6) 0.005(5) 0.005(5) -0.006(5) C89 0.092(7) 0.092(7) 0.053(6) 0.006(6) 0.020(5) -0.028(6) C90 0.079(6) 0.066(6) 0.059(6) 0.020(5) 0.007(5) -0.011(5) C91 0.058(5) 0.063(6) 0.080(7) 0.004(5) -0.010(5) 0.005(5) C92 0.083(7) 0.089(7) 0.053(6) 0.012(6) 0.004(5) -0.008(6) C93 0.085(7) 0.085(6) 0.054(5) -0.022(5) 0.005(5) -0.007(5) C94 0.093(7) 0.107(8) 0.050(5) -0.021(6) 0.015(5) 0.010(6) P1 0.110(3) 0.084(2) 0.120(3) 0.029(2) 0.008(2) -0.0059(18) F1 0.370(18) 0.156(8) 0.205(11) 0.094(8) 0.071(11) -0.006(10) F2 0.424(19) 0.100(6) 0.201(11) 0.041(7) 0.089(12) -0.057(9) F3 0.41(2) 0.188(10) 0.112(7) 0.006(7) 0.032(10) 0.004(11) F4 0.101(7) 0.54(3) 0.200(12) 0.066(14) 0.008(7) 0.091(10) F5 0.318(15) 0.167(9) 0.149(8) -0.059(7) 0.040(9) -0.104(9) F6 0.099(8) 0.69(4) 0.279(17) 0.04(2) 0.020(10) 0.009(13) P2 0.085(2) 0.0849(18) 0.0823(19) -0.0033(17) -0.0064(15) 0.0117(15) F7 0.259(11) 0.138(7) 0.136(7) -0.061(6) 0.072(7) 0.036(7) F8 0.193(9) 0.112(6) 0.278(13) -0.092(7) 0.012(9) 0.015(6) F9 0.103(6) 0.298(14) 0.277(14) -0.108(12) -0.008(8) 0.035(7) F10 0.328(15) 0.221(11) 0.111(7) 0.006(7) 0.081(9) 0.118(11) F11 0.091(7) 0.227(12) 0.76(4) -0.066(19) -0.130(14) 0.011(7) F12 0.64(3) 0.347(19) 0.188(12) 0.201(13) 0.202(17) 0.30(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.366(10) . ? O1 C7 1.418(9) . ? O2 C9 1.305(13) . ? O2 C8 1.395(12) . ? O3 C10 1.387(11) . ? O3 C11 1.406(12) . ? O4 C19 1.368(10) . ? O4 C12 1.469(11) . ? O5 C6 1.349(10) . ? O5 C13 1.440(9) . ? O6 C14 1.394(12) . ? O6 C15 1.410(11) . ? O7 C17 1.413(11) . ? O7 C16 1.436(10) . ? O8 C24 1.365(9) . ? O8 C18 1.406(10) . ? O9 C28 1.383(10) . ? O9 C33 1.408(10) . ? O10 C34 1.384(11) . ? O10 C35 1.428(11) . ? O11 C37 1.344(13) . ? O11 C36 1.442(14) . ? O12 C45 1.398(12) . ? O12 C38 1.429(11) . ? O13 C29 1.376(10) . ? O13 C39 1.451(10) . ? O14 C41 1.272(17) . ? O14 C40 1.417(13) . ? O15 C43 1.385(12) . ? O15 C42 1.421(12) . ? O16 C44 1.469(12) . ? O16 C50 1.477(13) . ? O17 C61 1.225(12) . ? O17 C58 1.398(10) . ? O18 C63 1.334(12) . ? O18 C62 1.395(11) . ? O19 C65 1.380(12) . ? O19 C64 1.444(13) . ? O20 C74 1.372(12) . ? O20 C66 1.431(13) . ? O21 C59 1.369(11) . ? O21 C67 1.452(14) . ? O22 C69 1.159(17) . ? O22 C68 1.47(2) . ? O22 C68' 1.63(3) . ? O23 C71 1.33(2) . ? O23 C70 1.42(2) . ? O24 C73 1.385(14) . ? O24 C72 1.446(15) . ? N1 C79 1.315(11) . ? N1 C83 1.391(11) . ? N1 C93 1.454(10) . ? N2 C91 1.315(11) . ? N2 C92 1.354(12) . ? N2 C94 1.501(11) . ? C1 C2 1.372(12) . ? C1 C6 1.401(11) . ? C2 C3 1.436(13) . ? C3 C4 1.390(12) . ? C3 C54 1.477(12) . ? C4 C5 1.438(12) . ? C4 C25 1.495(11) . ? C5 C6 1.352(12) . ? C7 C8 1.509(13) . ? C9 C10 1.499(16) . ? C11 C12 1.454(13) . ? C13 C14 1.484(13) . ? C15 C16 1.547(14) . ? C17 C18 1.490(13) . ? C19 C20 1.390(12) . ? C19 C24 1.403(12) . ? C20 C21 1.361(13) . ? C21 C22 1.416(13) . ? C21 C53 1.519(12) . ? C22 C23 1.349(11) . ? C22 C51 1.533(13) . ? C23 C24 1.382(12) . ? C25 C26 1.500(11) . ? C26 C31 1.394(11) . ? C26 C27 1.416(12) . ? C27 C28 1.397(12) . ? C28 C29 1.386(13) . ? C29 C30 1.383(14) . ? C30 C31 1.426(13) . ? C31 C32 1.541(13) . ? C32 C56 1.527(13) . ? C33 C34 1.470(12) . ? C35 C36 1.404(16) . ? C37 C38 1.394(15) . ? C39 C40 1.457(13) . ? C41 C42 1.407(19) . ? C43 C44 1.401(16) . ? C45 C46 1.377(13) . ? C45 C50 1.382(14) . ? C46 C47 1.394(13) . ? C47 C48 1.417(13) . ? C47 C51 1.488(13) . ? C48 C49 1.369(14) . ? C48 C52 1.460(13) . ? C49 C50 1.327(14) . ? C52 C76 1.663(15) . ? C53 C77 1.527(14) . ? C54 C55 1.535(11) . ? C55 C60 1.374(13) . ? C55 C56 1.410(13) . ? C56 C57 1.414(12) . ? C57 C58 1.309(13) . ? C58 C59 1.418(13) . ? C59 C60 1.388(12) . ? C61 C62 1.361(13) . ? C63 C64 1.347(15) . ? C65 C66 1.509(17) . ? C67 C68 1.55(2) . ? C69 C70 1.45(2) . ? C71 C72 1.413(16) . ? C73 C78 1.347(16) . ? C73 C74 1.382(16) . ? C74 C75 1.341(16) . ? C75 C76 1.456(15) . ? C76 C77 1.309(14) . ? C77 C78 1.435(16) . ? C79 C80 1.372(12) . ? C80 C84 1.394(13) . ? C80 C81 1.399(12) . ? C81 C87 1.366(11) . ? C81 C82 1.449(11) . ? C82 C83 1.387(12) . ? C82 C90 1.426(11) . ? C84 C85 1.379(14) . ? C85 C86 1.452(12) . ? C86 C91 1.361(12) . ? C86 C87 1.397(11) . ? C87 C88 1.457(12) . ? C88 C92 1.390(13) . ? C88 C89 1.507(13) . ? C89 C90 1.295(13) . ? P1 F4 1.439(8) . ? P1 F5 1.469(8) . ? P1 F2 1.479(8) . ? P1 F6 1.505(9) . ? P1 F1 1.515(8) . ? P1 F3 1.572(9) . ? P2 F11 1.398(8) . ? P2 F12 1.402(8) . ? P2 F7 1.525(7) . ? P2 F10 1.525(8) . ? P2 F9 1.527(8) . ? P2 F8 1.531(7) . ? N3 C95 1.167(12) . ? C95 C96 1.434(15) . ? N4 C97 1.20(2) . ? C97 C98 1.44(2) . ? N5 C99 1.186(13) . ? C99 C100 1.424(14) . ? N7 C101 1.03(3) . ? C101 C102 1.33(3) . ? C104 C103 1.09(2) . ? C103 N6 1.40(3) . ? 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 C7 118.6(6) . . ? C9 O2 C8 115.0(11) . . ? C10 O3 C11 113.0(9) . . ? C19 O4 C12 120.1(7) . . ? C6 O5 C13 118.3(7) . . ? C14 O6 C15 115.1(8) . . ? C17 O7 C16 109.9(8) . . ? C24 O8 C18 117.5(7) . . ? C28 O9 C33 118.9(7) . . ? C34 O10 C35 114.6(8) . . ? C37 O11 C36 116.0(10) . . ? C45 O12 C38 120.7(8) . . ? C29 O13 C39 114.5(7) . . ? C41 O14 C40 116.2(12) . . ? C43 O15 C42 111.8(9) . . ? C44 O16 C50 114.9(9) . . ? C61 O17 C58 124.3(9) . . ? C63 O18 C62 125.6(9) . . ? C65 O19 C64 113.9(9) . . ? C74 O20 C66 120.3(11) . . ? C59 O21 C67 115.3(8) . . ? C69 O22 C68 108.9(16) . . ? C69 O22 C68' 113.8(17) . . ? C68 O22 C68' 66.7(13) . . ? C71 O23 C70 103.8(16) . . ? C73 O24 C72 117.1(11) . . ? C79 N1 C83 120.8(8) . . ? C79 N1 C93 121.3(8) . . ? C83 N1 C93 117.7(8) . . ? C91 N2 C92 119.7(9) . . ? C91 N2 C94 119.2(9) . . ? C92 N2 C94 121.0(8) . . ? O1 C1 C2 123.4(8) . . ? O1 C1 C6 115.4(8) . . ? C2 C1 C6 121.2(9) . . ? C1 C2 C3 119.9(8) . . ? C4 C3 C2 119.3(8) . . ? C4 C3 C54 124.4(9) . . ? C2 C3 C54 116.2(8) . . ? C3 C4 C5 118.1(8) . . ? C3 C4 C25 123.4(8) . . ? C5 C4 C25 118.4(8) . . ? C6 C5 C4 122.1(8) . . ? O5 C6 C5 125.2(8) . . ? O5 C6 C1 115.2(8) . . ? C5 C6 C1 119.3(8) . . ? O1 C7 C8 105.5(7) . . ? O2 C8 C7 109.5(9) . . ? O2 C9 C10 112.0(11) . . ? O3 C10 C9 112.6(9) . . ? O3 C11 C12 113.2(11) . . ? C11 C12 O4 107.6(9) . . ? O5 C13 C14 109.6(8) . . ? O6 C14 C13 115.1(9) . . ? O6 C15 C16 108.2(9) . . ? O7 C16 C15 105.3(8) . . ? O7 C17 C18 109.2(9) . . ? O8 C18 C17 106.9(8) . . ? O4 C19 C20 125.8(8) . . ? O4 C19 C24 116.5(8) . . ? C20 C19 C24 117.6(9) . . ? C21 C20 C19 121.8(9) . . ? C20 C21 C22 120.3(8) . . ? C20 C21 C53 116.2(10) . . ? C22 C21 C53 123.4(10) . . ? C23 C22 C21 117.5(9) . . ? C23 C22 C51 117.9(9) . . ? C21 C22 C51 124.5(8) . . ? C22 C23 C24 123.0(9) . . ? O8 C24 C23 127.1(8) . . ? O8 C24 C19 113.5(8) . . ? C23 C24 C19 119.4(8) . . ? C4 C25 C26 113.2(6) . . ? C31 C26 C27 117.7(8) . . ? C31 C26 C25 125.2(8) . . ? C27 C26 C25 117.1(7) . . ? C28 C27 C26 121.7(8) . . ? O9 C28 C29 117.2(8) . . ? O9 C28 C27 122.8(8) . . ? C29 C28 C27 120.0(9) . . ? O13 C29 C30 124.8(9) . . ? O13 C29 C28 115.8(9) . . ? C30 C29 C28 119.5(9) . . ? C29 C30 C31 121.0(9) . . ? C26 C31 C30 120.0(9) . . ? C26 C31 C32 123.7(8) . . ? C30 C31 C32 116.3(8) . . ? C56 C32 C31 113.3(8) . . ? O9 C33 C34 112.3(8) . . ? O10 C34 C33 110.5(9) . . ? C36 C35 O10 116.8(9) . . ? C35 C36 O11 116.3(11) . . ? O11 C37 C38 115.1(11) . . ? C37 C38 O12 109.1(10) . . ? O13 C39 C40 106.4(9) . . ? O14 C40 C39 109.5(9) . . ? O14 C41 C42 122.6(16) . . ? C41 C42 O15 111.1(10) . . ? O15 C43 C44 112.6(10) . . ? C43 C44 O16 111.3(12) . . ? C46 C45 C50 117.4(11) . . ? C46 C45 O12 121.1(9) . . ? C50 C45 O12 121.5(10) . . ? C45 C46 C47 120.7(9) . . ? C46 C47 C48 118.8(9) . . ? C46 C47 C51 117.0(9) . . ? C48 C47 C51 124.1(10) . . ? C49 C48 C47 119.2(10) . . ? C49 C48 C52 115.9(10) . . ? C47 C48 C52 123.8(10) . . ? C50 C49 C48 119.9(10) . . ? C49 C50 C45 123.9(11) . . ? C49 C50 O16 125.6(10) . . ? C45 C50 O16 110.5(11) . . ? C47 C51 C22 112.5(7) . . ? C48 C52 C76 113.0(8) . . ? C21 C53 C77 111.5(8) . . ? C3 C54 C55 115.1(7) . . ? C60 C55 C56 120.7(9) . . ? C60 C55 C54 116.3(9) . . ? C56 C55 C54 123.0(9) . . ? C55 C56 C57 115.7(10) . . ? C55 C56 C32 125.3(9) . . ? C57 C56 C32 118.9(9) . . ? C58 C57 C56 124.4(10) . . ? C57 C58 O17 123.9(10) . . ? C57 C58 C59 119.8(9) . . ? O17 C58 C59 116.3(9) . . ? O21 C59 C60 125.1(10) . . ? O21 C59 C58 116.6(8) . . ? C60 C59 C58 118.2(9) . . ? C55 C60 C59 121.2(10) . . ? O17 C61 C62 126.0(12) . . ? C61 C62 O18 117.0(9) . . ? O18 C63 C64 128.6(11) . . ? C63 C64 O19 116.3(10) . . ? O19 C65 C66 110.4(9) . . ? O20 C66 C65 108.4(11) . . ? O21 C67 C68 116.9(13) . . ? O22 C68 C67 103.0(14) . . ? O22 C69 C70 116.7(16) . . ? O23 C70 C69 110.4(16) . . ? O23 C71 C72 110.0(18) . . ? C71 C72 O24 114.7(14) . . ? C78 C73 C74 117.0(12) . . ? C78 C73 O24 126.6(14) . . ? C74 C73 O24 116.1(11) . . ? C75 C74 O20 122.2(14) . . ? C75 C74 C73 122.5(11) . . ? O20 C74 C73 115.2(12) . . ? C74 C75 C76 118.9(12) . . ? C77 C76 C75 119.9(11) . . ? C77 C76 C52 123.9(10) . . ? C75 C76 C52 116.0(11) . . ? C76 C77 C78 118.3(11) . . ? C76 C77 C53 125.4(11) . . ? C78 C77 C53 116.3(12) . . ? C73 C78 C77 123.0(14) . . ? N1 C79 C80 124.4(8) . . ? C79 C80 C84 120.3(9) . . ? C79 C80 C81 116.5(8) . . ? C84 C80 C81 123.1(9) . . ? C87 C81 C80 117.5(8) . . ? C87 C81 C82 121.4(8) . . ? C80 C81 C82 121.1(8) . . ? C83 C82 C90 123.4(8) . . ? C83 C82 C81 117.2(8) . . ? C90 C82 C81 119.4(8) . . ? C82 C83 N1 120.0(8) . . ? C85 C84 C80 118.3(10) . . ? C84 C85 C86 120.7(9) . . ? C91 C86 C87 119.3(8) . . ? C91 C86 C85 123.6(9) . . ? C87 C86 C85 117.0(8) . . ? C81 C87 C86 123.4(8) . . ? C81 C87 C88 118.5(8) . . ? C86 C87 C88 118.1(8) . . ? C92 C88 C87 116.8(9) . . ? C92 C88 C89 125.4(8) . . ? C87 C88 C89 117.8(8) . . ? C90 C89 C88 121.1(8) . . ? C89 C90 C82 121.4(9) . . ? N2 C91 C86 123.6(9) . . ? N2 C92 C88 122.3(9) . . ? F4 P1 F5 93.9(6) . . ? F4 P1 F2 89.7(7) . . ? F5 P1 F2 89.3(5) . . ? F4 P1 F6 173.2(9) . . ? F5 P1 F6 89.9(6) . . ? F2 P1 F6 84.7(6) . . ? F4 P1 F1 94.2(6) . . ? F5 P1 F1 94.2(5) . . ? F2 P1 F1 174.7(7) . . ? F6 P1 F1 91.2(7) . . ? F4 P1 F3 89.7(6) . . ? F5 P1 F3 175.4(6) . . ? F2 P1 F3 87.9(5) . . ? F6 P1 F3 86.3(6) . . ? F1 P1 F3 88.4(5) . . ? F11 P2 F12 99.3(7) . . ? F11 P2 F7 94.5(6) . . ? F12 P2 F7 93.3(6) . . ? F11 P2 F10 89.3(6) . . ? F12 P2 F10 171.3(7) . . ? F7 P2 F10 86.8(5) . . ? F11 P2 F9 168.4(8) . . ? F12 P2 F9 90.5(6) . . ? F7 P2 F9 91.1(5) . . ? F10 P2 F9 80.8(6) . . ? F11 P2 F8 91.8(6) . . ? F12 P2 F8 90.6(6) . . ? F7 P2 F8 172.0(5) . . ? F10 P2 F8 88.3(5) . . ? F9 P2 F8 81.9(5) . . ? N3 C95 C96 176.6(16) . . ? N4 C97 C98 170(2) . . ? N5 C99 C100 167(3) . . ? N7 C101 C102 142(3) . . ? C104 C103 N6 163(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 67.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.750 _refine_diff_density_min -0.348 _refine_diff_density_rms 0.092 # Attachment 'B906075H-revised-722771.cif' data_ic13108 _database_code_depnum_ccdc_archive 'CCDC 722772' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C90 H104 F12 N4 O24 P2' _chemical_formula_sum 'C100 H119 F12 N9 O24 P2' _chemical_formula_weight 2120.98 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.2574(6) _cell_length_b 15.6396(6) _cell_length_c 24.9315(9) _cell_angle_alpha 98.260(3) _cell_angle_beta 93.741(3) _cell_angle_gamma 116.910(4) _cell_volume 5192.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 13358 _cell_measurement_theta_min 3.2254 _cell_measurement_theta_max 73.5819 _exptl_crystal_description cubes _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224 _exptl_absorpt_coefficient_mu 1.219 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.91217 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 250(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 R' _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 24351 _diffrn_reflns_av_R_equivalents 0.0189 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 68.00 _reflns_number_total 18667 _reflns_number_gt 10023 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) 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. Some atoms in the structure are modeled disorder or refined as isotropic. Because of the large correlation between thermal parameters, the restraint was necessary for convergence of the refinement process. In large supermolecular structure with poor data to parameter ratios, they often are needed with geometrical and anisotropic displacement parameters restraints. ; _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^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18667 _refine_ls_number_parameters 1430 _refine_ls_number_restraints 386 _refine_ls_R_factor_all 0.1243 _refine_ls_R_factor_gt 0.0737 _refine_ls_wR_factor_ref 0.2295 _refine_ls_wR_factor_gt 0.2086 _refine_ls_goodness_of_fit_ref 1.318 _refine_ls_restrained_S_all 1.333 _refine_ls_shift/su_max 0.037 _refine_ls_shift/su_mean 0.001 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 1.0628(2) 0.5997(2) 0.20905(15) 0.1037(10) Uani 1 1 d . . . O2 O 1.1211(10) 0.7151(9) 0.3234(5) 0.114(3) Uani 0.491(6) 1 d PU A 1 O3 O 1.0334(15) 0.8378(16) 0.3484(6) 0.115(4) Uani 0.491(6) 1 d PU A 1 C22 C 1.1222(4) 0.5957(4) 0.2541(2) 0.1213(18) Uani 0.491(6) 1 d PU A 1 H22A H 1.1649 0.5691 0.2396 0.146 Uiso 0.491(6) 1 calc PR A 1 H22B H 1.0781 0.5498 0.2751 0.146 Uiso 0.491(6) 1 calc PR A 1 C23 C 1.1874(19) 0.692(2) 0.2929(10) 0.116(4) Uani 0.491(6) 1 d PU A 1 H23A H 1.2357 0.6854 0.3178 0.140 Uiso 0.491(6) 1 calc PR A 1 H23B H 1.2236 0.7430 0.2725 0.140 Uiso 0.491(6) 1 calc PR A 1 C24 C 1.1618(12) 0.8170(13) 0.3551(7) 0.131(4) Uani 0.491(6) 1 d PU A 1 H24A H 1.2019 0.8201 0.3884 0.157 Uiso 0.491(6) 1 calc PR A 1 H24B H 1.2086 0.8592 0.3335 0.157 Uiso 0.491(6) 1 calc PR A 1 C25 C 1.1154(11) 0.8555(12) 0.3693(7) 0.141(4) Uani 0.491(6) 1 d PU A 1 H25A H 1.1578 0.9252 0.3700 0.169 Uiso 0.491(6) 1 calc PR A 1 H25B H 1.1094 0.8492 0.4076 0.169 Uiso 0.491(6) 1 calc PR A 1 C26 C 0.9945(4) 0.8801(5) 0.3724(3) 0.143(2) Uani 0.491(6) 1 d PU A 1 H26A H 0.9994 0.9323 0.3533 0.171 Uiso 0.491(6) 1 calc PR A 1 H26B H 1.0330 0.9115 0.4090 0.171 Uiso 0.491(6) 1 calc PR A 1 O2' O 1.1249(11) 0.7427(11) 0.2992(5) 0.141(4) Uani 0.509(6) 1 d PU A 2 O3' O 1.0319(17) 0.8342(17) 0.3285(6) 0.120(4) Uani 0.509(6) 1 d PU A 2 C22' C 1.1222(4) 0.5957(4) 0.2541(2) 0.1213(18) Uani 0.509(6) 1 d PU A 2 H22C H 1.1672 0.5703 0.2419 0.146 Uiso 0.509(6) 1 calc PR A 2 H22D H 1.0816 0.5564 0.2789 0.146 Uiso 0.509(6) 1 calc PR A 2 C23' C 1.176(2) 0.700(2) 0.2793(11) 0.139(6) Uani 0.509(6) 1 d PU A 2 H23C H 1.2264 0.7084 0.3091 0.166 Uiso 0.509(6) 1 calc PR A 2 H23D H 1.2122 0.7355 0.2518 0.166 Uiso 0.509(6) 1 calc PR A 2 C24' C 1.1819(12) 0.8224(14) 0.3330(8) 0.148(5) Uani 0.509(6) 1 d PDU A 2 H24C H 1.2467 0.8552 0.3208 0.177 Uiso 0.509(6) 1 calc PR A 2 H24D H 1.1920 0.8090 0.3695 0.177 Uiso 0.509(6) 1 calc PR A 2 C25' C 1.1352(8) 0.8796(9) 0.3344(6) 0.113(4) Uani 0.509(6) 1 d PDU A 2 H25C H 1.1555 0.9176 0.3054 0.135 Uiso 0.509(6) 1 calc PR A 2 H25D H 1.1607 0.9263 0.3694 0.135 Uiso 0.509(6) 1 calc PR A 2 C26' C 0.9945(4) 0.8801(5) 0.3724(3) 0.143(2) Uani 0.509(6) 1 d PU A 2 H26C H 1.0357 0.8936 0.4075 0.171 Uiso 0.509(6) 1 calc PR A 2 H26D H 1.0040 0.9430 0.3644 0.171 Uiso 0.509(6) 1 calc PR A 2 O4 O 0.8279(2) 0.7885(2) 0.32908(11) 0.0866(8) Uani 1 1 d . A . O5 O 0.9512(2) 0.6081(2) 0.12250(15) 0.1074(10) Uani 1 1 d . A . O6 O 0.9602(2) 0.78404(19) 0.10756(11) 0.0837(8) Uani 1 1 d . . . O7 O 0.8036(2) 0.81548(19) 0.13998(11) 0.0848(8) Uani 1 1 d . . . O8 O 0.72210(19) 0.7705(2) 0.23869(10) 0.0815(7) Uani 1 1 d . . . O9 O 0.5014(2) 0.2512(3) 0.02417(14) 0.0988(9) Uani 1 1 d . . . O10 O 0.3922(3) 0.3530(3) -0.00111(11) 0.1080(11) Uani 1 1 d . . . O11 O 0.23132(19) 0.38151(19) 0.03634(10) 0.0767(7) Uani 1 1 d . B . O12 O 0.22432(17) 0.39809(17) 0.15767(9) 0.0676(6) Uani 1 1 d . A . O13 O 0.4182(2) 0.0881(2) 0.06398(12) 0.0872(8) Uani 1 1 d . A . O14 O 0.2439(3) 0.0220(2) 0.11645(16) 0.1179(12) Uani 1 1 d . . . O15 O 0.1628(9) 0.0734(7) 0.2048(4) 0.088(3) Uani 0.491(6) 1 d PU A 1 C40 C 0.1161(4) 0.1872(3) 0.2478(2) 0.0997(15) Uani 0.491(6) 1 d PD A 1 H40A H 0.1143 0.2182 0.2845 0.120 Uiso 0.491(6) 1 calc PR A 1 H40B H 0.0472 0.1431 0.2310 0.120 Uiso 0.491(6) 1 calc PR A 1 C41 C 0.1632(7) 0.1303(7) 0.2541(4) 0.089(3) Uani 0.491(6) 1 d PDU A 1 H41A H 0.1305 0.0867 0.2792 0.107 Uiso 0.491(6) 1 calc PR A 1 H41B H 0.2323 0.1733 0.2710 0.107 Uiso 0.491(6) 1 calc PR A 1 C42 C 0.230(2) 0.035(2) 0.2167(11) 0.165(13) Uani 0.491(6) 1 d P A 1 H42A H 0.2100 -0.0047 0.2449 0.198 Uiso 0.491(6) 1 calc PR A 1 H42B H 0.2985 0.0868 0.2272 0.198 Uiso 0.491(6) 1 calc PR A 1 C43 C 0.2123(5) -0.0253(4) 0.1605(2) 0.1194(17) Uani 0.491(6) 1 d P A 1 H43A H 0.2447 -0.0665 0.1633 0.143 Uiso 0.491(6) 1 calc PR A 1 H43B H 0.1407 -0.0692 0.1510 0.143 Uiso 0.491(6) 1 calc PR A 1 O15' O 0.1090(6) 0.0596(4) 0.1804(3) 0.0778(18) Uani 0.509(6) 1 d PU A 2 C40' C 0.1161(4) 0.1872(3) 0.2478(2) 0.0997(15) Uani 0.509(6) 1 d P A 2 H40C H 0.1707 0.1907 0.2727 0.120 Uiso 0.509(6) 1 calc PR A 2 H40D H 0.0724 0.2014 0.2705 0.120 Uiso 0.509(6) 1 calc PR A 2 C41' C 0.0641(6) 0.0946(5) 0.2191(3) 0.077(2) Uani 0.509(6) 1 d PU A 2 H41C H 0.0027 0.0884 0.1999 0.092 Uiso 0.509(6) 1 calc PR A 2 H41D H 0.0447 0.0509 0.2456 0.092 Uiso 0.509(6) 1 calc PR A 2 C42' C 0.1891(18) 0.0359(17) 0.2013(8) 0.111(9) Uani 0.509(6) 1 d P A 2 H42C H 0.2499 0.0973 0.2153 0.133 Uiso 0.509(6) 1 calc PR A 2 H42D H 0.1683 0.0025 0.2321 0.133 Uiso 0.509(6) 1 calc PR A 2 C43' C 0.2123(5) -0.0253(4) 0.1605(2) 0.1194(17) Uani 0.509(6) 1 d P A 2 H43C H 0.2647 -0.0371 0.1772 0.143 Uiso 0.509(6) 1 calc PR A 2 H43D H 0.1531 -0.0885 0.1473 0.143 Uiso 0.509(6) 1 calc PR A 2 O16 O 0.15718(19) 0.26197(17) 0.21630(10) 0.0744(7) Uani 1 1 d . . . O17 O 0.6707(2) 0.0609(2) 0.28072(11) 0.0829(8) Uani 1 1 d . . . O18 O 0.5760(2) 0.00768(18) 0.37187(11) 0.0854(8) Uani 1 1 d . . . O19 O 0.4436(2) 0.07924(19) 0.40178(11) 0.0846(8) Uani 1 1 d . . . O20 O 0.49016(19) 0.28854(18) 0.42044(11) 0.0766(7) Uani 1 1 d . . . O21 O 0.8518(2) 0.2204(2) 0.32440(11) 0.0958(9) Uani 1 1 d . . . O22 O 0.9300(9) 0.3884(9) 0.4198(4) 0.111(3) Uani 0.491(6) 1 d PU A 1 C55 C 1.0046(5) 0.5018(6) 0.4076(3) 0.137(2) Uani 0.491(6) 1 d PU A 1 H55A H 1.0742 0.5268 0.4233 0.164 Uiso 0.491(6) 1 calc PR A 1 H55B H 0.9996 0.5042 0.3685 0.164 Uiso 0.491(6) 1 calc PR A 1 C56 C 0.9671(9) 0.3232(9) 0.4057(4) 0.109(3) Uani 0.491(6) 1 d PU A 1 H56A H 0.9393 0.2719 0.4274 0.131 Uiso 0.491(6) 1 calc PR A 1 H56B H 1.0390 0.3584 0.4177 0.131 Uiso 0.491(6) 1 calc PR A 1 C57 C 0.9507(5) 0.2757(5) 0.3495(2) 0.132(2) Uani 0.491(6) 1 d PU A 1 H57A H 0.9853 0.3259 0.3282 0.158 Uiso 0.491(6) 1 calc PR A 1 H57B H 0.9817 0.2327 0.3475 0.158 Uiso 0.491(6) 1 calc PR A 1 O22' O 0.9555(10) 0.4127(12) 0.3960(5) 0.146(4) Uani 0.509(6) 1 d PU A 2 C55' C 1.0046(5) 0.5018(6) 0.4076(3) 0.137(2) Uani 0.509(6) 1 d PU A 2 H55C H 1.0198 0.5267 0.3736 0.164 Uiso 0.509(6) 1 calc PR A 2 H55D H 1.0678 0.5186 0.4296 0.164 Uiso 0.509(6) 1 calc PR A 2 C56' C 0.9967(10) 0.3717(11) 0.3581(6) 0.145(4) Uani 0.509(6) 1 d PU A 2 H56C H 0.9927 0.3929 0.3233 0.174 Uiso 0.509(6) 1 calc PR A 2 H56D H 1.0670 0.3956 0.3718 0.174 Uiso 0.509(6) 1 calc PR A 2 C57' C 0.9507(5) 0.2757(5) 0.3495(2) 0.132(2) Uani 0.509(6) 1 d PU A 2 H57C H 0.9545 0.2574 0.3853 0.158 Uiso 0.509(6) 1 calc PR A 2 H57D H 0.9902 0.2534 0.3277 0.158 Uiso 0.509(6) 1 calc PR A 2 O23 O 0.8614(2) 0.5250(2) 0.40946(12) 0.0931(8) Uani 1 1 d . A . O24 O 0.6622(2) 0.43981(18) 0.45647(11) 0.0837(8) Uani 1 1 d . A . N1 N 0.9081(3) 0.7355(3) 0.22556(15) 0.1025(12) Uani 1 1 d . . . N2 N 0.9487(4) 0.8125(4) 0.22331(18) 0.1269(17) Uani 1 1 d . . . N3 N 0.4888(3) 0.0782(3) 0.27452(15) 0.0888(10) Uani 1 1 d . . . N4 N 0.4313(4) 0.0090(4) 0.28176(18) 0.1183(15) Uani 1 1 d . . . C1 C 0.9478(3) 0.3442(3) 0.13282(16) 0.0707(10) Uani 1 1 d . A . C2 C 1.0054(3) 0.4280(3) 0.17308(17) 0.0783(11) Uani 1 1 d . . . H2A H 1.0432 0.4235 0.2028 0.094 Uiso 1 1 calc R A . C3 C 1.0085(3) 0.5161(3) 0.1706(2) 0.0842(12) Uani 1 1 d . A . C4 C 0.9532(3) 0.5227(3) 0.1260(2) 0.0822(12) Uani 1 1 d . . . C5 C 0.8977(3) 0.4411(3) 0.08588(18) 0.0799(11) Uani 1 1 d . A . H5A H 0.8613 0.4467 0.0559 0.096 Uiso 1 1 calc R . . C6 C 0.8930(3) 0.3506(3) 0.08767(15) 0.0681(9) Uani 1 1 d . . . C7 C 0.8285(3) 0.2653(3) 0.04252(15) 0.0709(10) Uani 1 1 d . A . H7A H 0.8548 0.2183 0.0397 0.085 Uiso 1 1 calc R . . H7B H 0.8325 0.2884 0.0078 0.085 Uiso 1 1 calc R . . C8 C 0.7197(3) 0.2128(3) 0.05033(14) 0.0645(9) Uani 1 1 d . . . C9 C 0.6592(3) 0.2515(3) 0.03419(14) 0.0667(9) Uani 1 1 d . A . H9A H 0.6871 0.3083 0.0192 0.080 Uiso 1 1 calc R . . C10 C 0.5599(3) 0.2106(3) 0.03911(14) 0.0661(9) Uani 1 1 d . A . C11 C 0.5178(3) 0.1252(3) 0.06064(14) 0.0643(9) Uani 1 1 d . . . C12 C 0.5768(3) 0.0848(2) 0.07614(14) 0.0637(9) Uani 1 1 d . A . H12A H 0.5480 0.0266 0.0898 0.076 Uiso 1 1 calc R . . C13 C 0.6777(3) 0.1274(2) 0.07213(13) 0.0590(8) Uani 1 1 d . A . C14 C 0.7370(3) 0.0796(3) 0.09375(15) 0.0697(10) Uani 1 1 d . . . H14A H 0.6944 0.0087 0.0872 0.084 Uiso 1 1 calc R A . H14B H 0.7930 0.0923 0.0733 0.084 Uiso 1 1 calc R . . C15 C 0.7765(3) 0.1169(3) 0.15444(14) 0.0652(9) Uani 1 1 d . A . C16 C 0.7135(3) 0.0738(3) 0.19191(16) 0.0699(10) Uani 1 1 d . . . H16A H 0.6504 0.0206 0.1783 0.084 Uiso 1 1 calc R A . C17 C 0.7397(3) 0.1058(3) 0.24740(16) 0.0732(10) Uani 1 1 d . A . C18 C 0.8329(3) 0.1865(3) 0.26853(16) 0.0771(11) Uani 1 1 d . A . C19 C 0.8965(3) 0.2269(3) 0.23224(16) 0.0773(11) Uani 1 1 d . . . H19A H 0.9603 0.2785 0.2462 0.093 Uiso 1 1 calc R A . C20 C 0.8707(3) 0.1948(3) 0.17544(16) 0.0684(9) Uani 1 1 d . A . C21 C 0.9474(3) 0.2497(3) 0.14013(16) 0.0761(10) Uani 1 1 d . . . H21A H 1.0135 0.2641 0.1572 0.091 Uiso 1 1 calc R A . H21B H 0.9331 0.2078 0.1041 0.091 Uiso 1 1 calc R . . C27 C 0.8920(4) 0.8237(5) 0.3788(2) 0.139(2) Uani 1 1 d . . . H27A H 0.8849 0.7682 0.3954 0.167 Uiso 1 1 calc R A 1 H27B H 0.8728 0.8644 0.4038 0.167 Uiso 1 1 calc R A 1 C28 C 0.6742(3) 0.7901(3) 0.19419(16) 0.0832(11) Uani 1 1 d . . . H28A H 0.6321 0.8181 0.2079 0.100 Uiso 1 1 calc R . . H28B H 0.6322 0.7294 0.1678 0.100 Uiso 1 1 calc R . . C29 C 0.7528(3) 0.8605(3) 0.16737(19) 0.0892(12) Uani 1 1 d . . . H29A H 0.7225 0.8840 0.1411 0.107 Uiso 1 1 calc R . . H29B H 0.8000 0.9170 0.1951 0.107 Uiso 1 1 calc R . . C30 C 0.8832(4) 0.8846(4) 0.1175(3) 0.1212(19) Uani 1 1 d . . . H30A H 0.9361 0.9307 0.1471 0.145 Uiso 1 1 calc R . . H30B H 0.8593 0.9218 0.0978 0.145 Uiso 1 1 calc R . . C31 C 0.9223(4) 0.8354(4) 0.0802(2) 0.1139(18) Uani 1 1 d . . . H31A H 0.8695 0.7898 0.0504 0.137 Uiso 1 1 calc R . . H31B H 0.9753 0.8837 0.0642 0.137 Uiso 1 1 calc R . . C32 C 0.9964(4) 0.7338(3) 0.0719(2) 0.0975(14) Uani 1 1 d . A . H32A H 1.0512 0.7803 0.0561 0.117 Uiso 1 1 calc R . . H32B H 0.9435 0.6888 0.0420 0.117 Uiso 1 1 calc R . . C33 C 1.0321(4) 0.6777(4) 0.1032(3) 0.1170(18) Uani 1 1 d . . . H33A H 1.0612 0.6453 0.0793 0.140 Uiso 1 1 calc R A . H33B H 1.0831 0.7222 0.1341 0.140 Uiso 1 1 calc R . . C34 C 0.5259(6) 0.3107(6) -0.0111(3) 0.073(2) Uani 0.500(9) 1 d PU B 1 H34A H 0.5594 0.2908 -0.0387 0.088 Uiso 0.500(9) 1 calc PR B 1 H34B H 0.5714 0.3776 0.0080 0.088 Uiso 0.500(9) 1 calc PR B 1 C35 C 0.4304(4) 0.3065(4) -0.03895(17) 0.0997(13) Uani 0.500(9) 1 d PU B 1 H35A H 0.4450 0.3391 -0.0704 0.120 Uiso 0.500(9) 1 calc PR B 1 H35B H 0.3806 0.2381 -0.0524 0.120 Uiso 0.500(9) 1 calc PR B 1 C34' C 0.4369(7) 0.2178(6) -0.0146(3) 0.079(3) Uani 0.500(9) 1 d PU B 2 H34C H 0.3731 0.1763 -0.0034 0.095 Uiso 0.500(9) 1 calc PR B 2 H34D H 0.4510 0.1775 -0.0429 0.095 Uiso 0.500(9) 1 calc PR B 2 C35' C 0.4304(4) 0.3065(4) -0.03895(17) 0.0997(13) Uani 0.500(9) 1 d PU B 2 H35C H 0.4966 0.3538 -0.0447 0.120 Uiso 0.500(9) 1 calc PR B 2 H35D H 0.3868 0.2804 -0.0743 0.120 Uiso 0.500(9) 1 calc PR B 2 C36 C 0.3474(3) 0.4002(4) -0.02640(17) 0.0896(13) Uani 1 1 d . B . H36A H 0.2912 0.3526 -0.0540 0.108 Uiso 1 1 calc R . . H36B H 0.3953 0.4487 -0.0448 0.108 Uiso 1 1 calc R . . C37 C 0.3118(4) 0.4495(3) 0.01630(19) 0.0923(13) Uani 1 1 d . . . H37A H 0.3662 0.4891 0.0466 0.111 Uiso 1 1 calc R B . H37B H 0.2923 0.4932 0.0005 0.111 Uiso 1 1 calc R . . C38 C 0.1853(3) 0.4257(3) 0.07003(15) 0.0775(11) Uani 1 1 d . . . H38A H 0.1179 0.3758 0.0721 0.093 Uiso 1 1 calc R B . H38B H 0.1792 0.4754 0.0525 0.093 Uiso 1 1 calc R . . C39 C 0.2399(3) 0.4728(3) 0.12735(14) 0.0691(9) Uani 1 1 d . A . H39A H 0.3111 0.5118 0.1263 0.083 Uiso 1 1 calc R . . H39B H 0.2153 0.5162 0.1448 0.083 Uiso 1 1 calc R . . C44 C 0.2614(3) -0.0333(3) 0.0732(2) 0.0971(14) Uani 1 1 d . A . H44A H 0.2369 -0.0237 0.0385 0.117 Uiso 1 1 calc R . . H44B H 0.2235 -0.1027 0.0748 0.117 Uiso 1 1 calc R . . C45 C 0.3673(3) -0.0080(3) 0.07416(17) 0.0842(12) Uani 1 1 d . . . H45A H 0.3949 -0.0113 0.1099 0.101 Uiso 1 1 calc R A . H45B H 0.3744 -0.0541 0.0460 0.101 Uiso 1 1 calc R . . C46 C 0.6995(4) 0.0134(3) 0.31843(19) 0.0921(13) Uani 1 1 d . . . H46A H 0.7489 0.0621 0.3488 0.111 Uiso 1 1 calc R . . H46B H 0.7285 -0.0250 0.2998 0.111 Uiso 1 1 calc R . . C47 C 0.6084(4) -0.0513(3) 0.33927(18) 0.0888(13) Uani 1 1 d . . . H47A H 0.5563 -0.0943 0.3085 0.107 Uiso 1 1 calc R . . H47B H 0.6225 -0.0920 0.3612 0.107 Uiso 1 1 calc R . . C48 C 0.4884(4) -0.0497(3) 0.3927(2) 0.0931(13) Uani 1 1 d . . . H48A H 0.4990 -0.0947 0.4126 0.112 Uiso 1 1 calc R . . H48B H 0.4340 -0.0887 0.3623 0.112 Uiso 1 1 calc R . . C49 C 0.4618(4) 0.0146(3) 0.42987(18) 0.0943(13) Uani 1 1 d . . . H49A H 0.4022 -0.0255 0.4451 0.113 Uiso 1 1 calc R . . H49B H 0.5160 0.0527 0.4604 0.113 Uiso 1 1 calc R . . C50 C 0.4007(3) 0.1269(3) 0.43503(18) 0.0833(12) Uani 1 1 d . . . H50A H 0.4408 0.1545 0.4715 0.100 Uiso 1 1 calc R . . H50B H 0.3339 0.0787 0.4394 0.100 Uiso 1 1 calc R . . C51 C 0.3940(3) 0.2055(3) 0.41180(18) 0.0802(11) Uani 1 1 d . . . H51A H 0.3692 0.1829 0.3725 0.096 Uiso 1 1 calc R . . H51B H 0.3475 0.2233 0.4295 0.096 Uiso 1 1 calc R . . C52 C 0.7553(3) 0.5216(3) 0.47956(16) 0.0784(11) Uani 1 1 d . . . H52A H 0.7951 0.4995 0.5005 0.094 Uiso 1 1 calc R . . H52B H 0.7439 0.5681 0.5051 0.094 Uiso 1 1 calc R . . C53 C 0.8136(3) 0.5735(3) 0.43671(18) 0.0862(12) Uani 1 1 d . . . H53A H 0.7683 0.5795 0.4096 0.103 Uiso 1 1 calc R . . H53B H 0.8637 0.6397 0.4545 0.103 Uiso 1 1 calc R . . C54 C 0.9560(4) 0.5520(4) 0.4380(2) 0.1094(16) Uani 1 1 d . . . H54A H 0.9489 0.5349 0.4743 0.131 Uiso 1 1 calc R A 1 H54B H 0.9975 0.6229 0.4429 0.131 Uiso 1 1 calc R A 1 C58 C 0.7282(3) 0.7549(2) 0.33063(15) 0.0649(9) Uani 1 1 d . . . C59 C 0.6825(3) 0.7329(2) 0.37662(14) 0.0673(10) Uani 1 1 d . A . H59A H 0.7211 0.7403 0.4096 0.081 Uiso 1 1 calc R . . C60 C 0.5801(3) 0.6998(2) 0.37523(13) 0.0614(9) Uani 1 1 d . . . C61 C 0.5369(3) 0.6716(2) 0.42717(13) 0.0657(9) Uani 1 1 d . A . H61A H 0.5846 0.7155 0.4595 0.079 Uiso 1 1 calc R . . H61B H 0.4758 0.6775 0.4281 0.079 Uiso 1 1 calc R . . C62 C 0.5147(3) 0.5672(3) 0.42808(12) 0.0638(9) Uani 1 1 d . . . C63 C 0.5941(3) 0.5519(3) 0.44481(13) 0.0677(10) Uani 1 1 d . A . H63A H 0.6557 0.6064 0.4593 0.081 Uiso 1 1 calc R . . C64 C 0.5861(3) 0.4590(3) 0.44097(14) 0.0696(10) Uani 1 1 d . . . C65 C 0.4935(3) 0.3787(2) 0.42166(14) 0.0640(9) Uani 1 1 d . A . C66 C 0.4139(3) 0.3931(3) 0.40621(13) 0.0636(9) Uani 1 1 d . . . H66A H 0.3517 0.3383 0.3935 0.076 Uiso 1 1 calc R A . C67 C 0.4222(3) 0.4869(3) 0.40877(13) 0.0627(9) Uani 1 1 d . A . C68 C 0.3316(3) 0.4958(3) 0.38931(13) 0.0646(9) Uani 1 1 d . . . H68A H 0.3419 0.5616 0.4046 0.078 Uiso 1 1 calc R A . H68B H 0.2743 0.4490 0.4035 0.078 Uiso 1 1 calc R . . C69 C 0.3077(2) 0.4777(2) 0.32746(13) 0.0578(8) Uani 1 1 d . A . C70 C 0.2456(3) 0.3812(2) 0.30048(14) 0.0623(9) Uani 1 1 d . . . H70A H 0.2210 0.3323 0.3216 0.075 Uiso 1 1 calc R A . C71 C 0.2191(3) 0.3547(2) 0.24460(14) 0.0614(9) Uani 1 1 d . A . C72 C 0.2566(2) 0.4279(2) 0.21306(13) 0.0564(8) Uani 1 1 d . . . C73 C 0.3177(2) 0.5228(2) 0.23914(13) 0.0566(8) Uani 1 1 d . A . H73A H 0.3420 0.5716 0.2180 0.068 Uiso 1 1 calc R . . C74 C 0.3449(2) 0.5494(2) 0.29594(13) 0.0555(8) Uani 1 1 d . . . C75 C 0.4130(3) 0.6576(2) 0.32119(13) 0.0613(9) Uani 1 1 d . A . H75A H 0.3990 0.6975 0.2986 0.074 Uiso 1 1 calc R . . H75B H 0.3965 0.6716 0.3576 0.074 Uiso 1 1 calc R . . C76 C 0.5231(3) 0.6885(2) 0.32665(13) 0.0564(8) Uani 1 1 d . A . C77 C 0.5706(3) 0.7104(2) 0.28016(14) 0.0633(9) Uani 1 1 d . . . H77A H 0.5321 0.7019 0.2469 0.076 Uiso 1 1 calc R A . C78 C 0.6708(3) 0.7436(2) 0.28168(14) 0.0629(9) Uani 1 1 d . A . C79 C 0.8560(3) 0.6372(3) 0.22958(17) 0.0810(11) Uani 1 1 d . . . C80 C 0.7755(3) 0.5768(3) 0.19033(17) 0.0918(13) Uani 1 1 d . . . H80A H 0.7563 0.5995 0.1611 0.110 Uiso 1 1 calc R . . C81 C 0.7251(3) 0.4821(3) 0.19618(16) 0.0835(12) Uani 1 1 d . . . H81A H 0.6703 0.4380 0.1698 0.100 Uiso 1 1 calc R . . C82 C 0.7520(3) 0.4485(3) 0.23992(15) 0.0695(10) Uani 1 1 d . . . C83 C 0.8351(3) 0.5135(3) 0.27723(17) 0.0822(11) Uani 1 1 d . . . H83A H 0.8551 0.4915 0.3065 0.099 Uiso 1 1 calc R . . C84 C 0.8886(3) 0.6085(3) 0.27263(18) 0.0881(12) Uani 1 1 d . . . H84A H 0.9454 0.6524 0.2978 0.106 Uiso 1 1 calc R . . C85 C 0.6898(3) 0.3479(3) 0.24846(15) 0.0674(9) Uani 1 1 d . . . C86 C 0.6336(3) 0.2703(3) 0.20404(16) 0.0814(11) Uani 1 1 d . . . H86A H 0.6413 0.2803 0.1680 0.098 Uiso 1 1 calc R . . C87 C 0.5679(3) 0.1804(3) 0.21288(17) 0.0827(12) Uani 1 1 d . . . H87A H 0.5301 0.1284 0.1834 0.099 Uiso 1 1 calc R . . C88 C 0.5589(3) 0.1682(3) 0.26552(16) 0.0757(10) Uani 1 1 d . . . C89 C 0.6141(3) 0.2393(3) 0.31131(17) 0.0854(12) Uani 1 1 d . . . H89A H 0.6066 0.2268 0.3470 0.102 Uiso 1 1 calc R . . C90 C 0.6802(3) 0.3290(3) 0.30204(16) 0.0833(12) Uani 1 1 d . . . H90A H 0.7200 0.3791 0.3321 0.100 Uiso 1 1 calc R . . P1 P 0.11095(9) 0.17084(8) 0.43785(5) 0.0853(4) Uani 1 1 d . . . F1 F 0.0565(3) 0.2176(3) 0.47032(19) 0.1888(18) Uani 1 1 d . . . F2 F 0.1639(2) 0.1182(3) 0.40760(18) 0.1760(17) Uani 1 1 d . . . F3 F 0.1561(3) 0.2557(3) 0.40820(17) 0.191(2) Uani 1 1 d . . . F4 F 0.0166(2) 0.1159(2) 0.39212(13) 0.1278(10) Uani 1 1 d . . . F5 F 0.0633(3) 0.0817(3) 0.46668(16) 0.1657(15) Uani 1 1 d . . . F6 F 0.2046(2) 0.2262(2) 0.48392(12) 0.1315(10) Uani 1 1 d . . . P2 P 0.39170(12) 0.79587(11) 0.15894(6) 0.1082(4) Uani 1 1 d . . . F7 F 0.3358(5) 0.7806(5) 0.1054(2) 0.256(3) Uani 1 1 d . . . F8 F 0.4491(6) 0.8165(5) 0.2161(2) 0.256(3) Uani 1 1 d . . . F9 F 0.4809(5) 0.8529(4) 0.1333(3) 0.258(3) Uani 1 1 d . . . F10 F 0.3767(7) 0.8804(5) 0.17808(16) 0.328(5) Uani 1 1 d . . . F11 F 0.3028(5) 0.7137(5) 0.1773(3) 0.266(3) Uani 1 1 d . . . F12 F 0.4176(5) 0.7114(3) 0.1419(2) 0.216(2) Uani 1 1 d . . . N5 N 1.0607(4) 0.9342(4) 0.9665(2) 0.1213(15) Uani 1 1 d . . . C91 C 0.9782(5) 0.8986(4) 0.9491(2) 0.0911(13) Uani 1 1 d . . . C92 C 0.8731(4) 0.8530(4) 0.9277(2) 0.1119(16) Uani 1 1 d . . . H92A H 0.8433 0.7834 0.9275 0.168 Uiso 1 1 calc R . . H92B H 0.8649 0.8634 0.8907 0.168 Uiso 1 1 calc R . . H92C H 0.8407 0.8818 0.9508 0.168 Uiso 1 1 calc R . . N6 N 0.4193(4) 0.2684(4) 0.2687(2) 0.1224(15) Uani 1 1 d . . . C93 C 0.4656(4) 0.3533(5) 0.27614(18) 0.0930(14) Uani 1 1 d . . . C94 C 0.5224(4) 0.4562(4) 0.28613(19) 0.0950(13) Uani 1 1 d . . . H94A H 0.5172 0.4834 0.3226 0.143 Uiso 1 1 calc R . . H94B H 0.4977 0.4821 0.2592 0.143 Uiso 1 1 calc R . . H94C H 0.5915 0.4739 0.2835 0.143 Uiso 1 1 calc R . . N7 N 0.5163(5) 0.4810(6) 0.1426(3) 0.180(3) Uani 1 1 d . . . C95 C 0.4572(6) 0.4008(7) 0.1338(2) 0.132(2) Uani 1 1 d . . . C96 C 0.3804(5) 0.3027(5) 0.1230(2) 0.1208(18) Uani 1 1 d . . . H96A H 0.3303 0.2968 0.1463 0.181 Uiso 1 1 calc R . . H96B H 0.4080 0.2599 0.1305 0.181 Uiso 1 1 calc R . . H96C H 0.3505 0.2845 0.0849 0.181 Uiso 1 1 calc R . . N8 N 0.6921(8) 0.2760(6) 0.5580(3) 0.217(4) Uani 1 1 d . . . C97 C 0.7013(5) 0.2688(5) 0.5140(3) 0.130(2) Uani 1 1 d . . . C98 C 0.7102(5) 0.2601(4) 0.4580(2) 0.136(2) Uani 1 1 d . . . H98A H 0.6785 0.1915 0.4407 0.205 Uiso 1 1 calc R . . H98B H 0.7800 0.2900 0.4538 0.205 Uiso 1 1 calc R . . H98C H 0.6784 0.2927 0.4408 0.205 Uiso 1 1 calc R . . N9 N 0.7799(14) 0.1127(12) 0.5025(5) 0.390(11) Uani 1 1 d . . . C99 C 0.7907(9) 0.0552(7) 0.4815(3) 0.181(4) Uani 1 1 d . . . C100 C 0.8159(6) -0.0055(6) 0.4574(3) 0.170(3) Uani 1 1 d . . . H10A H 0.8658 0.0263 0.4347 0.256 Uiso 1 1 calc R . . H10B H 0.7581 -0.0599 0.4346 0.256 Uiso 1 1 calc R . . H10C H 0.8429 -0.0295 0.4844 0.256 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 0.086(2) 0.087(2) 0.117(3) -0.0027(18) 0.0196(19) 0.0284(17) O2 0.077(4) 0.119(6) 0.128(8) -0.041(5) -0.009(5) 0.052(4) O3 0.057(4) 0.104(5) 0.144(8) -0.060(7) -0.016(7) 0.031(4) C22 0.083(3) 0.144(4) 0.123(4) -0.032(3) -0.002(3) 0.060(3) C23 0.069(6) 0.135(7) 0.127(8) -0.029(7) -0.006(6) 0.051(5) C24 0.065(6) 0.141(6) 0.138(8) -0.075(6) -0.016(6) 0.040(5) C25 0.093(6) 0.134(6) 0.159(8) -0.058(6) -0.016(7) 0.052(6) C26 0.090(4) 0.131(4) 0.152(5) -0.049(4) -0.021(3) 0.032(3) O2' 0.080(4) 0.154(7) 0.144(8) -0.060(6) -0.010(6) 0.045(5) O3' 0.078(5) 0.112(5) 0.134(8) -0.035(7) -0.012(7) 0.034(4) C22' 0.083(3) 0.144(4) 0.123(4) -0.032(3) -0.002(3) 0.060(3) C23' 0.082(7) 0.146(7) 0.145(9) -0.049(7) -0.011(7) 0.043(6) C24' 0.071(6) 0.153(7) 0.162(9) -0.056(7) 0.010(6) 0.030(6) C25' 0.069(5) 0.107(6) 0.133(8) 0.006(6) 0.000(5) 0.023(5) C26' 0.090(4) 0.131(4) 0.152(5) -0.049(4) -0.021(3) 0.032(3) O4 0.0721(18) 0.106(2) 0.0725(17) 0.0138(15) -0.0045(13) 0.0367(15) O5 0.095(2) 0.0787(19) 0.161(3) 0.0412(19) 0.054(2) 0.0424(17) O6 0.098(2) 0.0821(17) 0.0785(18) 0.0292(14) 0.0338(15) 0.0420(15) O7 0.0978(19) 0.0815(17) 0.0926(19) 0.0498(15) 0.0431(16) 0.0438(15) O8 0.0748(16) 0.112(2) 0.0670(16) 0.0328(14) 0.0134(13) 0.0469(15) O9 0.101(2) 0.142(3) 0.099(2) 0.060(2) 0.030(2) 0.084(2) O10 0.157(3) 0.173(3) 0.0561(16) 0.0283(17) 0.0192(17) 0.128(3) O11 0.0805(17) 0.0934(18) 0.0593(15) 0.0198(13) 0.0124(13) 0.0416(15) O12 0.0767(15) 0.0688(14) 0.0543(14) 0.0139(11) 0.0050(11) 0.0315(12) O13 0.0845(19) 0.0843(18) 0.106(2) 0.0377(15) 0.0276(15) 0.0435(15) O14 0.123(3) 0.098(2) 0.140(3) 0.035(2) 0.071(2) 0.048(2) O15 0.108(7) 0.080(6) 0.072(6) -0.004(4) 0.000(4) 0.047(5) C40 0.125(4) 0.066(3) 0.111(4) 0.031(2) 0.055(3) 0.038(3) C41 0.106(7) 0.090(6) 0.086(6) 0.036(5) 0.018(5) 0.052(5) C42 0.24(3) 0.131(14) 0.13(2) 0.014(13) -0.010(15) 0.105(16) C43 0.162(5) 0.111(4) 0.100(4) 0.023(3) 0.020(4) 0.076(4) O15' 0.080(4) 0.064(3) 0.084(5) 0.011(3) 0.008(3) 0.032(3) C40' 0.125(4) 0.066(3) 0.111(4) 0.031(2) 0.055(3) 0.038(3) C41' 0.078(5) 0.055(4) 0.094(6) 0.011(4) 0.027(4) 0.029(4) C42' 0.16(2) 0.083(11) 0.070(9) 0.020(9) 0.042(13) 0.032(12) C43' 0.162(5) 0.111(4) 0.100(4) 0.023(3) 0.020(4) 0.076(4) O16 0.0800(16) 0.0600(15) 0.0774(16) 0.0187(12) 0.0119(13) 0.0262(13) O17 0.0976(19) 0.1022(19) 0.0785(17) 0.0419(15) 0.0282(15) 0.0631(16) O18 0.121(2) 0.0650(15) 0.0799(18) 0.0225(13) 0.0341(16) 0.0472(16) O19 0.120(2) 0.0755(16) 0.0737(17) 0.0270(13) 0.0223(15) 0.0545(16) O20 0.0874(18) 0.0662(15) 0.0830(18) 0.0239(13) 0.0110(14) 0.0393(14) O21 0.113(2) 0.111(2) 0.0652(18) 0.0127(15) 0.0088(16) 0.0558(19) O22 0.125(6) 0.135(6) 0.091(6) 0.005(4) -0.006(4) 0.084(5) C55 0.124(4) 0.177(5) 0.108(4) -0.011(4) -0.010(3) 0.084(4) C56 0.134(6) 0.147(7) 0.072(5) -0.009(5) 0.000(5) 0.099(5) C57 0.146(5) 0.168(5) 0.097(4) -0.026(4) -0.027(3) 0.108(4) O22' 0.133(7) 0.170(8) 0.137(8) -0.035(7) -0.001(6) 0.094(6) C55' 0.124(4) 0.177(5) 0.108(4) -0.011(4) -0.010(3) 0.084(4) C56' 0.130(6) 0.177(7) 0.121(6) -0.021(6) -0.001(6) 0.083(6) C57' 0.146(5) 0.168(5) 0.097(4) -0.026(4) -0.027(3) 0.108(4) O23 0.102(2) 0.107(2) 0.0752(18) 0.0055(15) 0.0026(16) 0.0581(18) O24 0.0897(19) 0.0729(16) 0.0885(19) 0.0230(14) -0.0066(15) 0.0385(15) N1 0.103(3) 0.100(3) 0.077(2) 0.025(2) 0.013(2) 0.022(3) N2 0.133(4) 0.111(3) 0.098(3) 0.030(3) 0.015(3) 0.023(3) N3 0.103(3) 0.081(3) 0.077(2) 0.011(2) 0.004(2) 0.041(2) N4 0.136(4) 0.103(3) 0.093(3) 0.018(3) 0.003(3) 0.038(3) C1 0.064(2) 0.077(2) 0.080(3) 0.018(2) 0.027(2) 0.037(2) C2 0.064(2) 0.088(3) 0.081(3) 0.012(2) 0.015(2) 0.034(2) C3 0.069(3) 0.073(3) 0.105(3) 0.009(2) 0.031(2) 0.028(2) C4 0.064(2) 0.075(3) 0.111(4) 0.025(3) 0.030(2) 0.031(2) C5 0.068(2) 0.081(3) 0.096(3) 0.032(2) 0.025(2) 0.033(2) C6 0.059(2) 0.082(3) 0.069(2) 0.0231(19) 0.0231(18) 0.0330(19) C7 0.076(2) 0.083(2) 0.066(2) 0.0280(19) 0.0242(19) 0.043(2) C8 0.071(2) 0.073(2) 0.052(2) 0.0116(17) 0.0136(16) 0.0359(19) C9 0.074(2) 0.078(2) 0.055(2) 0.0252(17) 0.0125(17) 0.037(2) C10 0.074(2) 0.073(2) 0.059(2) 0.0175(17) 0.0102(17) 0.039(2) C11 0.064(2) 0.072(2) 0.059(2) 0.0146(17) 0.0142(17) 0.0319(19) C12 0.075(2) 0.0578(19) 0.058(2) 0.0124(16) 0.0098(17) 0.0303(18) C13 0.069(2) 0.063(2) 0.0503(19) 0.0063(15) 0.0095(16) 0.0366(18) C14 0.080(2) 0.067(2) 0.070(2) 0.0097(17) 0.0129(19) 0.0408(19) C15 0.082(3) 0.070(2) 0.062(2) 0.0153(18) 0.0130(19) 0.050(2) C16 0.077(2) 0.066(2) 0.078(3) 0.0207(19) 0.012(2) 0.0409(19) C17 0.093(3) 0.082(3) 0.068(2) 0.025(2) 0.018(2) 0.057(2) C18 0.094(3) 0.087(3) 0.059(2) 0.013(2) 0.006(2) 0.051(2) C19 0.078(3) 0.085(3) 0.072(3) 0.014(2) 0.003(2) 0.042(2) C20 0.069(2) 0.074(2) 0.073(2) 0.0144(19) 0.0088(19) 0.043(2) C21 0.066(2) 0.091(3) 0.076(3) 0.011(2) 0.0065(19) 0.042(2) C27 0.089(4) 0.171(5) 0.118(4) -0.034(4) -0.015(3) 0.048(4) C28 0.093(3) 0.106(3) 0.063(2) 0.035(2) 0.016(2) 0.051(2) C29 0.106(3) 0.090(3) 0.096(3) 0.039(2) 0.040(3) 0.059(3) C30 0.138(4) 0.116(4) 0.164(5) 0.092(4) 0.089(4) 0.078(4) C31 0.120(4) 0.141(4) 0.125(4) 0.093(4) 0.063(3) 0.073(4) C32 0.099(3) 0.087(3) 0.100(3) 0.020(3) 0.042(3) 0.034(3) C33 0.092(3) 0.094(3) 0.181(6) 0.042(3) 0.068(4) 0.046(3) C34 0.083(5) 0.072(4) 0.072(5) 0.035(4) 0.017(4) 0.036(4) C35 0.125(3) 0.145(4) 0.064(2) 0.025(2) 0.006(2) 0.092(3) C34' 0.092(5) 0.085(5) 0.063(5) 0.006(4) 0.005(4) 0.047(4) C35' 0.125(3) 0.145(4) 0.064(2) 0.025(2) 0.006(2) 0.092(3) C36 0.101(3) 0.123(3) 0.072(3) 0.046(2) 0.020(2) 0.067(3) C37 0.106(3) 0.104(3) 0.092(3) 0.038(3) 0.031(3) 0.064(3) C38 0.080(3) 0.102(3) 0.061(2) 0.016(2) 0.0061(19) 0.052(2) C39 0.082(2) 0.080(2) 0.056(2) 0.0236(18) 0.0126(18) 0.044(2) C44 0.078(3) 0.086(3) 0.100(3) 0.002(2) 0.014(2) 0.020(2) C45 0.086(3) 0.072(3) 0.073(3) 0.007(2) 0.011(2) 0.020(2) C46 0.121(4) 0.104(3) 0.085(3) 0.044(2) 0.030(3) 0.072(3) C47 0.132(4) 0.079(3) 0.079(3) 0.027(2) 0.022(3) 0.064(3) C48 0.117(4) 0.071(3) 0.103(3) 0.038(2) 0.037(3) 0.045(3) C49 0.136(4) 0.086(3) 0.087(3) 0.044(2) 0.041(3) 0.064(3) C50 0.102(3) 0.070(2) 0.088(3) 0.025(2) 0.029(2) 0.043(2) C51 0.085(3) 0.066(2) 0.090(3) 0.024(2) 0.019(2) 0.032(2) C52 0.088(3) 0.084(3) 0.064(2) 0.015(2) -0.003(2) 0.043(2) C53 0.104(3) 0.084(3) 0.078(3) 0.014(2) 0.011(2) 0.052(3) C54 0.114(4) 0.111(4) 0.100(4) -0.002(3) -0.022(3) 0.062(3) C58 0.065(2) 0.059(2) 0.066(2) 0.0079(16) -0.0017(18) 0.0281(18) C59 0.090(3) 0.059(2) 0.050(2) 0.0049(16) -0.0074(18) 0.0363(19) C60 0.087(3) 0.0489(18) 0.052(2) 0.0067(14) 0.0071(17) 0.0358(18) C61 0.095(3) 0.062(2) 0.0435(18) 0.0024(15) 0.0024(17) 0.0421(19) C62 0.092(3) 0.069(2) 0.0368(17) 0.0126(15) 0.0099(17) 0.043(2) C63 0.089(3) 0.066(2) 0.0465(19) 0.0103(16) -0.0009(17) 0.036(2) C64 0.090(3) 0.076(2) 0.052(2) 0.0199(17) 0.0039(18) 0.045(2) C65 0.084(3) 0.058(2) 0.052(2) 0.0169(16) 0.0118(18) 0.032(2) C66 0.078(2) 0.067(2) 0.0484(19) 0.0194(16) 0.0097(16) 0.0339(19) C67 0.088(3) 0.069(2) 0.0387(17) 0.0149(15) 0.0159(16) 0.042(2) C68 0.081(2) 0.074(2) 0.055(2) 0.0222(16) 0.0249(17) 0.0455(19) C69 0.067(2) 0.068(2) 0.0520(19) 0.0204(16) 0.0164(16) 0.0401(18) C70 0.070(2) 0.066(2) 0.064(2) 0.0272(17) 0.0233(17) 0.0373(19) C71 0.063(2) 0.061(2) 0.065(2) 0.0172(17) 0.0127(17) 0.0320(18) C72 0.061(2) 0.066(2) 0.0504(19) 0.0161(16) 0.0104(15) 0.0343(17) C73 0.061(2) 0.066(2) 0.056(2) 0.0234(16) 0.0176(16) 0.0355(18) C74 0.065(2) 0.0615(19) 0.0525(19) 0.0137(15) 0.0152(15) 0.0380(17) C75 0.084(3) 0.061(2) 0.0521(19) 0.0147(15) 0.0137(17) 0.0443(19) C76 0.075(2) 0.0511(18) 0.0505(19) 0.0111(14) 0.0071(16) 0.0353(16) C77 0.075(2) 0.066(2) 0.054(2) 0.0149(16) 0.0024(17) 0.0376(19) C78 0.074(2) 0.066(2) 0.054(2) 0.0182(16) 0.0136(17) 0.0354(18) C79 0.074(3) 0.085(3) 0.076(3) 0.017(2) 0.024(2) 0.028(2) C80 0.099(3) 0.097(3) 0.061(3) 0.014(2) 0.001(2) 0.032(3) C81 0.080(3) 0.093(3) 0.060(2) 0.005(2) -0.0026(19) 0.029(2) C82 0.063(2) 0.085(3) 0.060(2) 0.0036(19) 0.0068(18) 0.037(2) C83 0.075(3) 0.090(3) 0.077(3) 0.009(2) -0.008(2) 0.039(2) C84 0.074(3) 0.093(3) 0.078(3) 0.006(2) -0.007(2) 0.028(2) C85 0.067(2) 0.079(2) 0.059(2) 0.0011(18) 0.0032(17) 0.040(2) C86 0.098(3) 0.089(3) 0.055(2) 0.002(2) 0.013(2) 0.046(3) C87 0.095(3) 0.072(3) 0.070(3) -0.009(2) 0.005(2) 0.037(2) C88 0.094(3) 0.074(3) 0.067(3) 0.011(2) 0.007(2) 0.047(2) C89 0.101(3) 0.089(3) 0.063(2) 0.012(2) -0.005(2) 0.045(3) C90 0.098(3) 0.081(3) 0.064(3) 0.003(2) -0.013(2) 0.043(2) P1 0.0857(7) 0.0713(6) 0.0776(7) 0.0151(5) 0.0021(6) 0.0195(6) F1 0.136(3) 0.193(4) 0.195(4) -0.071(3) -0.005(3) 0.075(3) F2 0.107(2) 0.153(3) 0.221(4) -0.064(3) 0.002(2) 0.053(2) F3 0.163(3) 0.145(3) 0.177(3) 0.099(3) -0.019(3) -0.016(2) F4 0.108(2) 0.113(2) 0.124(2) 0.0095(17) -0.0291(17) 0.0287(16) F5 0.150(3) 0.149(3) 0.171(3) 0.090(3) 0.005(2) 0.033(2) F6 0.114(2) 0.136(2) 0.105(2) -0.0089(17) -0.0282(16) 0.0395(18) P2 0.1292(11) 0.1178(10) 0.1024(10) 0.0542(8) 0.0270(9) 0.0684(9) F7 0.289(7) 0.350(7) 0.132(4) 0.008(4) -0.059(4) 0.176(6) F8 0.399(9) 0.297(6) 0.155(4) 0.032(4) -0.054(5) 0.251(7) F9 0.242(6) 0.171(4) 0.354(8) 0.091(5) 0.165(6) 0.063(4) F10 0.736(15) 0.414(8) 0.101(3) 0.040(4) 0.039(5) 0.504(11) F11 0.264(6) 0.244(6) 0.361(9) 0.160(6) 0.171(7) 0.133(5) F12 0.301(6) 0.150(3) 0.254(5) 0.079(3) 0.097(5) 0.136(4) N5 0.110(3) 0.148(4) 0.128(4) 0.025(3) 0.040(3) 0.077(3) C91 0.121(4) 0.090(3) 0.086(3) 0.024(2) 0.036(3) 0.065(3) C92 0.112(4) 0.115(4) 0.111(4) 0.029(3) 0.008(3) 0.054(3) N6 0.119(4) 0.131(4) 0.124(4) -0.007(3) 0.001(3) 0.076(3) C93 0.109(4) 0.124(4) 0.071(3) 0.007(3) 0.010(2) 0.080(4) C94 0.123(4) 0.107(4) 0.089(3) 0.028(3) 0.034(3) 0.078(3) N7 0.134(5) 0.233(8) 0.129(5) 0.069(5) -0.012(4) 0.044(5) C95 0.101(5) 0.210(8) 0.085(4) 0.052(5) 0.009(3) 0.066(5) C96 0.116(4) 0.172(6) 0.095(4) 0.042(4) 0.023(3) 0.079(4) N8 0.368(11) 0.266(8) 0.132(5) 0.054(6) 0.068(7) 0.239(9) C97 0.190(6) 0.139(5) 0.094(4) 0.022(4) 0.024(4) 0.105(5) C98 0.196(6) 0.128(4) 0.112(5) 0.030(3) 0.025(4) 0.097(5) N9 0.76(3) 0.50(2) 0.221(11) 0.103(12) 0.124(14) 0.55(2) C99 0.323(12) 0.205(8) 0.129(6) 0.061(6) 0.066(6) 0.209(9) C100 0.172(7) 0.171(7) 0.167(7) 0.049(6) 0.006(5) 0.077(6) _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 C3 1.367(5) . ? O1 C22 1.423(7) . ? O2 C23 1.45(3) . ? O2 C24 1.493(19) . ? O3 C26 1.20(2) . ? O3 C25 1.21(2) . ? C22 C23 1.51(3) . ? C24 C25 1.162(19) . ? C26 C27 1.439(8) . ? O2' C24' 1.282(19) . ? O2' C23' 1.32(3) . ? O3' C25' 1.39(2) . ? C24' C25' 1.371(17) . ? O4 C58 1.372(4) . ? O4 C27 1.398(6) . ? O5 C4 1.366(5) . ? O5 C33 1.397(5) . ? O6 C32 1.403(5) . ? O6 C31 1.403(5) . ? O7 C29 1.410(5) . ? O7 C30 1.426(5) . ? O8 C78 1.371(4) . ? O8 C28 1.434(4) . ? O9 C34' 1.200(8) . ? O9 C34 1.320(7) . ? O9 C10 1.369(4) . ? O10 C36 1.395(5) . ? O10 C35 1.420(5) . ? O11 C37 1.392(5) . ? O11 C38 1.424(5) . ? O12 C72 1.373(4) . ? O12 C39 1.420(4) . ? O13 C11 1.373(4) . ? O13 C45 1.417(4) . ? O14 C44 1.400(5) . ? O14 C43 1.402(6) . ? O15 C41 1.408(13) . ? O15 C42 1.43(3) . ? C40 C41 1.391(9) . ? C40 O16 1.430(5) . ? C42 C43 1.51(3) . ? O15' C41' 1.406(9) . ? O15' C42' 1.51(3) . ? O16 C71 1.369(4) . ? O17 C17 1.380(5) . ? O17 C46 1.439(5) . ? O18 C48 1.414(5) . ? O18 C47 1.415(5) . ? O19 C50 1.416(5) . ? O19 C49 1.421(5) . ? O20 C65 1.384(4) . ? O20 C51 1.428(5) . ? O21 C18 1.379(5) . ? O21 C57 1.398(6) . ? O22 C56 1.389(16) . ? O22 C55 1.706(15) . ? C55 C54 1.472(8) . ? C56 C57 1.437(10) . ? O22' C56' 1.402(17) . ? O23 C53 1.409(5) . ? O23 C54 1.412(5) . ? O24 C64 1.371(4) . ? O24 C52 1.422(5) . ? N1 N2 1.089(5) . ? N1 C79 1.398(6) . ? N3 N4 1.092(5) . ? N3 C88 1.391(6) . ? C1 C6 1.400(5) . ? C1 C2 1.401(5) . ? C1 C21 1.513(5) . ? C2 C3 1.368(6) . ? C3 C4 1.396(6) . ? C4 C5 1.375(6) . ? C5 C6 1.391(5) . ? C6 C7 1.500(5) . ? C7 C8 1.524(5) . ? C8 C9 1.382(5) . ? C8 C13 1.403(5) . ? C9 C10 1.374(5) . ? C10 C11 1.399(5) . ? C11 C12 1.378(5) . ? C12 C13 1.391(5) . ? C13 C14 1.528(5) . ? C14 C15 1.517(5) . ? C15 C20 1.400(5) . ? C15 C16 1.401(5) . ? C16 C17 1.369(5) . ? C17 C18 1.407(6) . ? C18 C19 1.372(5) . ? C19 C20 1.399(5) . ? C20 C21 1.524(5) . ? C28 C29 1.489(5) . ? C30 C31 1.447(7) . ? C32 C33 1.500(7) . ? C34 C35 1.542(9) . ? C36 C37 1.496(6) . ? C38 C39 1.505(5) . ? C44 C45 1.476(6) . ? C46 C47 1.483(6) . ? C48 C49 1.479(6) . ? C50 C51 1.472(5) . ? C52 C53 1.521(6) . ? C58 C59 1.386(5) . ? C58 C78 1.395(5) . ? C59 C60 1.402(5) . ? C60 C76 1.384(5) . ? C60 C61 1.523(5) . ? C61 C62 1.513(5) . ? C62 C63 1.387(5) . ? C62 C67 1.391(5) . ? C63 C64 1.389(5) . ? C64 C65 1.391(5) . ? C65 C66 1.373(5) . ? C66 C67 1.406(5) . ? C67 C68 1.507(5) . ? C68 C69 1.516(4) . ? C69 C74 1.389(4) . ? C69 C70 1.399(5) . ? C70 C71 1.373(5) . ? C71 C72 1.407(5) . ? C72 C73 1.373(5) . ? C73 C74 1.396(4) . ? C74 C75 1.535(5) . ? C75 C76 1.513(5) . ? C76 C77 1.408(5) . ? C77 C78 1.370(5) . ? C79 C84 1.368(6) . ? C79 C80 1.374(6) . ? C80 C81 1.360(6) . ? C81 C82 1.392(5) . ? C82 C83 1.384(5) . ? C82 C85 1.480(5) . ? C83 C84 1.360(6) . ? C85 C86 1.408(5) . ? C85 C90 1.412(5) . ? C86 C87 1.369(6) . ? C87 C88 1.360(5) . ? C88 C89 1.382(5) . ? C89 C90 1.372(6) . ? P1 F3 1.518(3) . ? P1 F1 1.532(4) . ? P1 F2 1.550(4) . ? P1 F5 1.558(3) . ? P1 F6 1.578(3) . ? P1 F4 1.579(3) . ? P2 F10 1.462(4) . ? P2 F7 1.464(4) . ? P2 F9 1.494(5) . ? P2 F8 1.533(5) . ? P2 F11 1.541(5) . ? P2 F12 1.555(5) . ? N5 C91 1.143(6) . ? C91 C92 1.452(8) . ? N6 C93 1.165(6) . ? C93 C94 1.414(7) . ? N7 C95 1.143(9) . ? C95 C96 1.418(9) . ? N8 C97 1.110(8) . ? C97 C98 1.405(8) . ? N9 C99 1.058(10) . ? C99 C100 1.268(10) . ? 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 C3 O1 C22 118.0(4) . . ? C23 O2 C24 117.2(14) . . ? C26 O3 C25 116.5(13) . . ? O1 C22 C23 116.0(11) . . ? O2 C23 C22 105.9(17) . . ? C25 C24 O2 125.8(14) . . ? C24 C25 O3 127.1(15) . . ? O3 C26 C27 117.6(11) . . ? C24' O2' C23' 110.5(16) . . ? O2' C24' C25' 106.5(16) . . ? C24' C25' O3' 118.4(16) . . ? C58 O4 C27 118.3(4) . . ? C4 O5 C33 116.1(3) . . ? C32 O6 C31 111.9(4) . . ? C29 O7 C30 110.4(3) . . ? C78 O8 C28 117.1(3) . . ? C34' O9 C34 70.5(5) . . ? C34' O9 C10 125.7(5) . . ? C34 O9 C10 121.4(4) . . ? C36 O10 C35 112.1(3) . . ? C37 O11 C38 112.7(3) . . ? C72 O12 C39 116.5(3) . . ? C11 O13 C45 117.7(3) . . ? C44 O14 C43 114.1(4) . . ? C41 O15 C42 106.8(14) . . ? C41 C40 O16 118.1(5) . . ? C40 C41 O15 114.2(8) . . ? O15 C42 C43 97.1(15) . . ? O14 C43 C42 119.2(12) . . ? C41' O15' C42' 118.1(10) . . ? C71 O16 C40 117.0(3) . . ? C17 O17 C46 115.4(3) . . ? C48 O18 C47 111.5(3) . . ? C50 O19 C49 109.9(3) . . ? C65 O20 C51 116.9(3) . . ? C18 O21 C57 118.5(4) . . ? C56 O22 C55 112.4(9) . . ? C54 C55 O22 96.4(6) . . ? O22 C56 C57 119.6(9) . . ? O21 C57 C56 116.7(7) . . ? C53 O23 C54 112.3(3) . . ? C64 O24 C52 116.9(3) . . ? N2 N1 C79 178.8(5) . . ? N4 N3 C88 177.4(5) . . ? C6 C1 C2 119.3(4) . . ? C6 C1 C21 122.5(4) . . ? C2 C1 C21 118.2(4) . . ? C3 C2 C1 122.3(4) . . ? O1 C3 C2 124.5(5) . . ? O1 C3 C4 116.9(4) . . ? C2 C3 C4 118.6(4) . . ? O5 C4 C5 119.6(4) . . ? O5 C4 C3 120.9(4) . . ? C5 C4 C3 119.4(4) . . ? C4 C5 C6 122.9(4) . . ? C5 C6 C1 117.4(4) . . ? C5 C6 C7 119.0(4) . . ? C1 C6 C7 123.6(4) . . ? C6 C7 C8 114.2(3) . . ? C9 C8 C13 118.5(3) . . ? C9 C8 C7 117.5(3) . . ? C13 C8 C7 123.9(3) . . ? C10 C9 C8 122.8(3) . . ? O9 C10 C9 122.1(3) . . ? O9 C10 C11 119.2(3) . . ? C9 C10 C11 118.7(3) . . ? O13 C11 C12 125.4(3) . . ? O13 C11 C10 115.4(3) . . ? C12 C11 C10 119.2(3) . . ? C11 C12 C13 122.0(3) . . ? C12 C13 C8 118.7(3) . . ? C12 C13 C14 117.4(3) . . ? C8 C13 C14 123.9(3) . . ? C15 C14 C13 112.7(3) . . ? C20 C15 C16 117.8(3) . . ? C20 C15 C14 123.9(3) . . ? C16 C15 C14 118.2(3) . . ? C17 C16 C15 122.8(4) . . ? C16 C17 O17 118.3(4) . . ? C16 C17 C18 119.5(4) . . ? O17 C17 C18 122.1(4) . . ? C19 C18 O21 125.2(4) . . ? C19 C18 C17 118.0(4) . . ? O21 C18 C17 116.8(4) . . ? C18 C19 C20 123.0(4) . . ? C19 C20 C15 118.8(4) . . ? C19 C20 C21 117.1(3) . . ? C15 C20 C21 124.1(3) . . ? C1 C21 C20 112.3(3) . . ? O4 C27 C26 112.8(5) . . ? O8 C28 C29 108.0(3) . . ? O7 C29 C28 110.4(3) . . ? O7 C30 C31 110.5(4) . . ? O6 C31 C30 111.0(4) . . ? O6 C32 C33 109.2(4) . . ? O5 C33 C32 108.5(4) . . ? O9 C34 C35 108.6(5) . . ? O10 C35 C34 110.1(4) . . ? O10 C36 C37 108.7(3) . . ? O11 C37 C36 111.3(4) . . ? O11 C38 C39 114.4(3) . . ? O12 C39 C38 108.6(3) . . ? O14 C44 C45 113.6(4) . . ? O13 C45 C44 107.9(4) . . ? O17 C46 C47 107.0(4) . . ? O18 C47 C46 108.6(3) . . ? O18 C48 C49 109.6(3) . . ? O19 C49 C48 111.1(3) . . ? O19 C50 C51 112.5(3) . . ? O20 C51 C50 109.2(3) . . ? O24 C52 C53 113.0(3) . . ? O23 C53 C52 113.3(3) . . ? O23 C54 C55 110.7(4) . . ? O4 C58 C59 124.9(3) . . ? O4 C58 C78 116.0(3) . . ? C59 C58 C78 119.1(3) . . ? C58 C59 C60 121.7(3) . . ? C76 C60 C59 119.2(3) . . ? C76 C60 C61 123.6(3) . . ? C59 C60 C61 117.0(3) . . ? C62 C61 C60 109.1(3) . . ? C63 C62 C67 119.1(3) . . ? C63 C62 C61 117.0(3) . . ? C67 C62 C61 123.6(3) . . ? C62 C63 C64 122.6(4) . . ? O24 C64 C63 125.0(4) . . ? O24 C64 C65 116.8(3) . . ? C63 C64 C65 118.2(4) . . ? C66 C65 O20 125.1(3) . . ? C66 C65 C64 119.6(3) . . ? O20 C65 C64 115.2(3) . . ? C65 C66 C67 122.4(3) . . ? C62 C67 C66 118.0(3) . . ? C62 C67 C68 123.2(3) . . ? C66 C67 C68 118.8(3) . . ? C67 C68 C69 113.7(3) . . ? C74 C69 C70 118.2(3) . . ? C74 C69 C68 124.7(3) . . ? C70 C69 C68 117.1(3) . . ? C71 C70 C69 123.0(3) . . ? O16 C71 C70 125.3(3) . . ? O16 C71 C72 116.2(3) . . ? C70 C71 C72 118.4(3) . . ? C73 C72 O12 124.9(3) . . ? C73 C72 C71 119.0(3) . . ? O12 C72 C71 116.0(3) . . ? C72 C73 C74 122.4(3) . . ? C69 C74 C73 119.0(3) . . ? C69 C74 C75 122.6(3) . . ? C73 C74 C75 118.4(3) . . ? C76 C75 C74 115.0(3) . . ? C60 C76 C77 118.4(3) . . ? C60 C76 C75 123.6(3) . . ? C77 C76 C75 118.0(3) . . ? C78 C77 C76 122.3(3) . . ? C77 C78 O8 125.2(3) . . ? C77 C78 C58 119.2(3) . . ? O8 C78 C58 115.6(3) . . ? C84 C79 C80 124.8(4) . . ? C84 C79 N1 117.5(4) . . ? C80 C79 N1 117.7(4) . . ? C81 C80 C79 116.2(4) . . ? C80 C81 C82 122.2(4) . . ? C83 C82 C81 118.1(4) . . ? C83 C82 C85 120.7(4) . . ? C81 C82 C85 121.0(3) . . ? C84 C83 C82 121.7(4) . . ? C83 C84 C79 116.9(4) . . ? C86 C85 C90 118.2(4) . . ? C86 C85 C82 121.4(3) . . ? C90 C85 C82 120.3(3) . . ? C87 C86 C85 120.6(4) . . ? C88 C87 C86 118.2(4) . . ? C87 C88 C89 124.8(4) . . ? C87 C88 N3 118.2(4) . . ? C89 C88 N3 117.0(4) . . ? C90 C89 C88 116.5(4) . . ? C89 C90 C85 121.5(4) . . ? F3 P1 F1 92.1(3) . . ? F3 P1 F2 91.9(3) . . ? F1 P1 F2 176.0(3) . . ? F3 P1 F5 178.4(2) . . ? F1 P1 F5 88.9(3) . . ? F2 P1 F5 87.2(3) . . ? F3 P1 F6 88.89(19) . . ? F1 P1 F6 90.1(2) . . ? F2 P1 F6 89.31(19) . . ? F5 P1 F6 92.44(19) . . ? F3 P1 F4 91.18(19) . . ? F1 P1 F4 89.3(2) . . ? F2 P1 F4 91.29(19) . . ? F5 P1 F4 87.50(19) . . ? F6 P1 F4 179.4(2) . . ? F10 P2 F7 89.9(3) . . ? F10 P2 F9 93.9(4) . . ? F7 P2 F9 84.7(4) . . ? F10 P2 F8 87.0(3) . . ? F7 P2 F8 176.9(3) . . ? F9 P2 F8 95.7(4) . . ? F10 P2 F11 101.3(4) . . ? F7 P2 F11 92.9(4) . . ? F9 P2 F11 164.6(3) . . ? F8 P2 F11 87.6(4) . . ? F10 P2 F12 174.5(4) . . ? F7 P2 F12 94.6(4) . . ? F9 P2 F12 83.3(3) . . ? F8 P2 F12 88.6(3) . . ? F11 P2 F12 81.7(3) . . ? N5 C91 C92 179.2(6) . . ? N6 C93 C94 179.0(6) . . ? N7 C95 C96 177.3(9) . . ? N8 C97 C98 178.2(9) . . ? N9 C99 C100 172.4(18) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 68.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.654 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.049