# 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 _publ_contact_author_name 'Pradyut Ghosh' _publ_contact_author_email ICPG@IACS.RES.IN _publ_section_title ; Efficient Fixation of Atmospheric CO2 as Carbonate in a Capsule of a Neutral Receptor and its Release in Mild Condition ; loop_ _publ_author_name 'Pradyut Ghosh' 'I. Ravikumar' # Attachment 'complex1_revised.cif' data_carbonate _database_code_depnum_ccdc_archive 'CCDC 735771' #TrackingRef 'complex1_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C87 H108 F30 N16 O9' _chemical_formula_weight 2091.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 21.923(3) _cell_length_b 19.069(3) _cell_length_c 23.089(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.027(2) _cell_angle_gamma 90.00 _cell_volume 9615(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3546 _cell_measurement_theta_min 1.42 _cell_measurement_theta_max 27.50 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4336 _exptl_absorpt_coefficient_mu 0.134 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9447 _exptl_absorpt_correction_T_max 0.9854 _exptl_absorpt_process_details BRUKER-SADABS _exptl_special_details ; The structure is non-centrosymmetric with atoms lighter than silicon (carbon, nitrogen, oxygen and hydrogen), the anomalous dispersion effects are very small with MoKa radiation. Since no useful absolute structural parameter can be refined (i.e. the value of absolute structure parameter is meaningless because of its large s.u. value), Friedel-pair reflections are merged before final refinements. MERGE 3 instruction of SHELXL-97 is employed to merge the Friedel-pair data. The meaningless absolute structure parameter value and s.u. value are removed. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEX II' _diffrn_measurement_method 'OMEGA SCAN' _diffrn_detector_area_resol_mean 3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39541 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10625 _reflns_number_gt 8930 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART APEX II' _computing_cell_refinement 'BRUKER SMART APEX II' _computing_data_reduction 'BRUKER AXS SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER SHELXTL' _computing_publication_material 'MERCURY 2.2' _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^+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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_number_reflns 10625 _refine_ls_number_parameters 1287 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.1168 _refine_ls_wR_factor_gt 0.1062 _refine_ls_goodness_of_fit_ref 0.850 _refine_ls_restrained_S_all 0.850 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.35483(16) -0.05686(16) 0.74770(14) 0.0236(6) Uani 1 1 d . . . H1A H 0.3900 -0.0441 0.7273 0.028 Uiso 1 1 calc R . . H1B H 0.3278 -0.0852 0.7217 0.028 Uiso 1 1 calc R . . C2 C 0.37618(15) -0.09991(16) 0.80125(14) 0.0247(7) Uani 1 1 d . . . H2A H 0.3410 -0.1117 0.8221 0.030 Uiso 1 1 calc R . . H2B H 0.3940 -0.1434 0.7889 0.030 Uiso 1 1 calc R . . C3 C 0.48150(14) -0.06976(15) 0.83421(13) 0.0206(6) Uani 1 1 d . . . C4 C 0.58014(15) -0.02032(16) 0.86857(14) 0.0226(6) Uani 1 1 d . . . C5 C 0.60421(16) -0.00089(17) 0.81710(15) 0.0270(7) Uani 1 1 d . . . C6 C 0.66623(17) 0.0106(2) 0.81507(16) 0.0342(8) Uani 1 1 d . . . C7 C 0.70526(16) 0.0054(2) 0.86507(19) 0.0381(9) Uani 1 1 d . . . C8 C 0.68248(16) -0.0125(2) 0.91695(16) 0.0323(8) Uani 1 1 d . . . C9 C 0.62096(15) -0.02547(17) 0.91780(14) 0.0247(7) Uani 1 1 d . . . C10 C 0.32783(17) 0.06274(17) 0.71957(14) 0.0273(7) Uani 1 1 d . . . H10A H 0.2956 0.0970 0.7228 0.033 Uiso 1 1 calc R . . H10B H 0.3226 0.0427 0.6808 0.033 Uiso 1 1 calc R . . C11 C 0.38976(17) 0.09871(17) 0.72833(14) 0.0273(7) Uani 1 1 d . . . H11A H 0.4217 0.0635 0.7293 0.033 Uiso 1 1 calc R . . H11B H 0.3946 0.1293 0.6955 0.033 Uiso 1 1 calc R . . C12 C 0.39026(15) 0.20952(17) 0.77988(14) 0.0239(6) Uani 1 1 d . . . C13 C 0.40142(15) 0.31454(17) 0.83869(14) 0.0237(6) Uani 1 1 d . . . C14 C 0.37276(14) 0.34380(17) 0.88454(14) 0.0231(6) Uani 1 1 d . . . C15 C 0.37031(15) 0.41498(18) 0.89406(15) 0.0264(7) Uani 1 1 d . . . C16 C 0.39571(16) 0.46050(17) 0.85658(16) 0.0284(7) Uani 1 1 d . . . C17 C 0.42435(16) 0.43332(18) 0.81074(16) 0.0292(7) Uani 1 1 d . . . C18 C 0.42866(16) 0.36181(17) 0.80273(15) 0.0266(7) Uani 1 1 d . . . C19 C 0.25888(15) -0.00982(18) 0.77193(15) 0.0280(7) Uani 1 1 d . . . H19A H 0.2581 -0.0515 0.7960 0.034 Uiso 1 1 calc R . . H19B H 0.2370 -0.0204 0.7346 0.034 Uiso 1 1 calc R . . C20 C 0.22584(16) 0.0495(2) 0.80068(16) 0.0319(8) Uani 1 1 d . . . H20A H 0.2145 0.0857 0.7722 0.038 Uiso 1 1 calc R . . H20B H 0.1886 0.0316 0.8152 0.038 Uiso 1 1 calc R . . C21 C 0.24211(14) 0.12182(17) 0.88796(14) 0.0233(6) Uani 1 1 d . . . C22 C 0.27501(14) 0.19421(17) 0.97212(14) 0.0234(7) Uani 1 1 d . . . C23 C 0.23138(16) 0.24776(19) 0.97220(16) 0.0300(7) Uani 1 1 d . . . C24 C 0.22381(19) 0.2859(2) 1.02198(19) 0.0391(9) Uani 1 1 d . . . C25 C 0.2594(2) 0.2729(2) 1.07302(18) 0.0405(9) Uani 1 1 d . . . C26 C 0.30396(19) 0.2221(2) 1.07436(16) 0.0358(8) Uani 1 1 d . . . C27 C 0.31075(15) 0.18343(17) 1.02428(15) 0.0256(7) Uani 1 1 d . . . C28 C 0.54837(16) 0.09303(17) 1.14898(14) 0.0268(7) Uani 1 1 d . . . H28A H 0.5788 0.1293 1.1452 0.032 Uiso 1 1 calc R . . H28B H 0.5522 0.0768 1.1889 0.032 Uiso 1 1 calc R . . C29 C 0.48475(16) 0.12319(17) 1.13430(15) 0.0270(7) Uani 1 1 d . . . H29A H 0.4550 0.0855 1.1335 0.032 Uiso 1 1 calc R . . H29B H 0.4755 0.1557 1.1646 0.032 Uiso 1 1 calc R . . C30 C 0.48647(14) 0.22938(16) 1.07658(13) 0.0210(6) Uani 1 1 d . . . C31 C 0.47586(14) 0.33069(16) 1.01374(14) 0.0224(6) Uani 1 1 d . . . C32 C 0.45046(15) 0.37978(18) 1.04938(15) 0.0266(7) Uani 1 1 d . . . C33 C 0.45719(17) 0.45095(17) 1.04018(17) 0.0313(8) Uani 1 1 d . . . C34 C 0.48619(16) 0.47539(18) 0.99413(17) 0.0311(8) Uani 1 1 d . . . C35 C 0.50957(15) 0.42835(18) 0.95685(15) 0.0262(7) Uani 1 1 d . . . C36 C 0.50488(14) 0.35738(17) 0.96730(15) 0.0246(7) Uani 1 1 d . . . C37 C 0.62460(15) 0.02327(18) 1.10289(15) 0.0278(7) Uani 1 1 d . . . H37A H 0.6292 -0.0200 1.0816 0.033 Uiso 1 1 calc R . . H37B H 0.6467 0.0181 1.1409 0.033 Uiso 1 1 calc R . . C38 C 0.65267(16) 0.08298(19) 1.07075(16) 0.0303(7) Uani 1 1 d . . . H38A H 0.6599 0.1226 1.0968 0.036 Uiso 1 1 calc R . . H38B H 0.6918 0.0681 1.0584 0.036 Uiso 1 1 calc R . . C39 C 0.63415(14) 0.14066(16) 0.97613(14) 0.0212(6) Uani 1 1 d . . . C40 C 0.59878(14) 0.19692(16) 0.88393(14) 0.0218(6) Uani 1 1 d . . . C41 C 0.56733(15) 0.17489(16) 0.83276(15) 0.0248(7) Uani 1 1 d . . . C42 C 0.57491(17) 0.20645(19) 0.78004(15) 0.0296(7) Uani 1 1 d . . . C43 C 0.61502(18) 0.2609(2) 0.77691(16) 0.0334(8) Uani 1 1 d . . . C44 C 0.64545(16) 0.28621(18) 0.82771(16) 0.0284(7) Uani 1 1 d . . . C45 C 0.63703(15) 0.25519(17) 0.88081(14) 0.0245(6) Uani 1 1 d . . . C46 C 0.53135(15) -0.03054(16) 1.12932(13) 0.0215(6) Uani 1 1 d . . . H46A H 0.4951 -0.0189 1.1486 0.026 Uiso 1 1 calc R . . H46B H 0.5599 -0.0543 1.1572 0.026 Uiso 1 1 calc R . . C47 C 0.51375(14) -0.07955(16) 1.07863(13) 0.0209(6) Uani 1 1 d . . . H47A H 0.5501 -0.0909 1.0593 0.025 Uiso 1 1 calc R . . H47B H 0.4979 -0.1229 1.0934 0.025 Uiso 1 1 calc R . . C48 C 0.40807(14) -0.05641(15) 1.04333(13) 0.0196(6) Uani 1 1 d . . . C49 C 0.30786(14) -0.01619(16) 1.00589(13) 0.0209(6) Uani 1 1 d . . . C50 C 0.28324(15) 0.01286(16) 1.05396(14) 0.0228(6) Uani 1 1 d . . . C51 C 0.22140(16) 0.02125(18) 1.05581(15) 0.0280(7) Uani 1 1 d . . . C52 C 0.18163(16) 0.00217(19) 1.00872(17) 0.0322(8) Uani 1 1 d . . . C53 C 0.20415(16) -0.02663(19) 0.96053(16) 0.0300(7) Uani 1 1 d . . . C54 C 0.26627(16) -0.03652(16) 0.95947(14) 0.0245(7) Uani 1 1 d . . . C55 C 0.44027(15) 0.10242(15) 0.93188(13) 0.0173(5) Uani 1 1 d . . . C56 C 0.41221(14) 0.72291(15) 0.10410(13) 0.0201(6) Uani 1 1 d . . . H56A H 0.4220 0.7715 0.0966 0.024 Uiso 1 1 calc R . . H56B H 0.4129 0.7172 0.1459 0.024 Uiso 1 1 calc R . . C57 C 0.46188(15) 0.67693(17) 0.08227(14) 0.0234(6) Uani 1 1 d . . . H57A H 0.4649 0.6856 0.0412 0.028 Uiso 1 1 calc R . . H57B H 0.4517 0.6279 0.0871 0.028 Uiso 1 1 calc R . . C58 C 0.52297(14) 0.69338(17) 0.11648(14) 0.0246(7) Uani 1 1 d . . . H58A H 0.5211 0.6797 0.1567 0.029 Uiso 1 1 calc R . . H58B H 0.5303 0.7435 0.1155 0.029 Uiso 1 1 calc R . . C59 C 0.57605(16) 0.6549(2) 0.09141(16) 0.0317(8) Uani 1 1 d . . . H59A H 0.5690 0.6052 0.0925 0.048 Uiso 1 1 calc R . . H59B H 0.6136 0.6658 0.1141 0.048 Uiso 1 1 calc R . . H59C H 0.5788 0.6694 0.0519 0.048 Uiso 1 1 calc R . . C60 C 0.34337(14) 0.70897(16) 0.01121(13) 0.0205(6) Uani 1 1 d . . . H60A H 0.3697 0.6723 -0.0017 0.025 Uiso 1 1 calc R . . H60B H 0.3017 0.6978 -0.0035 0.025 Uiso 1 1 calc R . . C61 C 0.36124(16) 0.77782(18) -0.01539(14) 0.0258(7) Uani 1 1 d . . . H61A H 0.4007 0.7929 0.0026 0.031 Uiso 1 1 calc R . . H61B H 0.3313 0.8135 -0.0082 0.031 Uiso 1 1 calc R . . C62 C 0.36467(16) 0.76936(18) -0.08129(14) 0.0268(7) Uani 1 1 d . . . H62A H 0.3826 0.8114 -0.0963 0.032 Uiso 1 1 calc R . . H62B H 0.3915 0.7304 -0.0881 0.032 Uiso 1 1 calc R . . C63 C 0.30275(18) 0.7566(2) -0.11436(15) 0.0357(8) Uani 1 1 d . . . H63A H 0.2855 0.7139 -0.1009 0.054 Uiso 1 1 calc R . . H63B H 0.3077 0.7527 -0.1551 0.054 Uiso 1 1 calc R . . H63C H 0.2759 0.7950 -0.1079 0.054 Uiso 1 1 calc R . . C64 C 0.30770(14) 0.76564(16) 0.10097(13) 0.0201(6) Uani 1 1 d . . . H64A H 0.3121 0.7633 0.1431 0.024 Uiso 1 1 calc R . . H64B H 0.3233 0.8108 0.0898 0.024 Uiso 1 1 calc R . . C65 C 0.24010(16) 0.7618(2) 0.08063(18) 0.0348(8) Uani 1 1 d . . . H65A H 0.2354 0.7530 0.0391 0.042 Uiso 1 1 calc R . . H65B H 0.2216 0.7230 0.0999 0.042 Uiso 1 1 calc R . . C66 C 0.20753(16) 0.8288(2) 0.09355(17) 0.0318(8) Uani 1 1 d . . . H66A H 0.2107 0.8361 0.1353 0.038 Uiso 1 1 calc R . . H66B H 0.2279 0.8677 0.0762 0.038 Uiso 1 1 calc R . . C67 C 0.14098(18) 0.8288(3) 0.0711(2) 0.0467(10) Uani 1 1 d . . . H67A H 0.1373 0.8179 0.0303 0.070 Uiso 1 1 calc R . . H67B H 0.1237 0.8743 0.0769 0.070 Uiso 1 1 calc R . . H67C H 0.1194 0.7943 0.0917 0.070 Uiso 1 1 calc R . . C68 C 0.32630(15) 0.63562(15) 0.09347(14) 0.0217(6) Uani 1 1 d . . . H68A H 0.3478 0.6014 0.0718 0.026 Uiso 1 1 calc R . . H68B H 0.2830 0.6314 0.0810 0.026 Uiso 1 1 calc R . . C69 C 0.33569(16) 0.61656(17) 0.15799(14) 0.0261(7) Uani 1 1 d . . . H69A H 0.3780 0.6029 0.1677 0.031 Uiso 1 1 calc R . . H69B H 0.3274 0.6573 0.1812 0.031 Uiso 1 1 calc R . . C70 C 0.29355(17) 0.55662(17) 0.17235(15) 0.0281(7) Uani 1 1 d . . . H70A H 0.3018 0.5451 0.2132 0.034 Uiso 1 1 calc R . . H70B H 0.2515 0.5728 0.1665 0.034 Uiso 1 1 calc R . . C71 C 0.29961(19) 0.49042(18) 0.13695(17) 0.0354(8) Uani 1 1 d . . . H71A H 0.2908 0.5009 0.0964 0.053 Uiso 1 1 calc R . . H71B H 0.2712 0.4558 0.1485 0.053 Uiso 1 1 calc R . . H71C H 0.3406 0.4726 0.1436 0.053 Uiso 1 1 calc R . . C72 C 0.05913(15) 0.88787(16) 0.25557(14) 0.0220(6) Uani 1 1 d . . . H72A H 0.1025 0.8933 0.2669 0.026 Uiso 1 1 calc R . . H72B H 0.0377 0.9229 0.2766 0.026 Uiso 1 1 calc R . . C73 C 0.04800(16) 0.90385(17) 0.19059(14) 0.0250(7) Uani 1 1 d . . . H73A H 0.0054 0.9162 0.1811 0.030 Uiso 1 1 calc R . . H73B H 0.0570 0.8627 0.1682 0.030 Uiso 1 1 calc R . . C74 C 0.08922(17) 0.96497(18) 0.17505(15) 0.0292(7) Uani 1 1 d . . . H74A H 0.1316 0.9502 0.1815 0.035 Uiso 1 1 calc R . . H74B H 0.0810 0.9752 0.1340 0.035 Uiso 1 1 calc R . . C75 C 0.08102(19) 1.03166(18) 0.20914(17) 0.0361(8) Uani 1 1 d . . . H75A H 0.0395 1.0477 0.2021 0.054 Uiso 1 1 calc R . . H75B H 0.1083 1.0670 0.1970 0.054 Uiso 1 1 calc R . . H75C H 0.0900 1.0225 0.2499 0.054 Uiso 1 1 calc R . . C76 C 0.04700(14) 0.81957(16) 0.34136(13) 0.0197(6) Uani 1 1 d . . . H76A H 0.0880 0.8362 0.3532 0.024 Uiso 1 1 calc R . . H76B H 0.0185 0.8542 0.3537 0.024 Uiso 1 1 calc R . . C77 C 0.03702(15) 0.75229(16) 0.37317(14) 0.0232(6) Uani 1 1 d . . . H77A H 0.0681 0.7183 0.3651 0.028 Uiso 1 1 calc R . . H77B H -0.0028 0.7329 0.3604 0.028 Uiso 1 1 calc R . . C78 C 0.04068(17) 0.76798(18) 0.43830(14) 0.0284(7) Uani 1 1 d . . . H78A H 0.0793 0.7910 0.4500 0.034 Uiso 1 1 calc R . . H78B H 0.0079 0.7997 0.4462 0.034 Uiso 1 1 calc R . . C79 C 0.03566(19) 0.70130(19) 0.47365(16) 0.0359(8) Uani 1 1 d . . . H79A H -0.0022 0.6781 0.4617 0.054 Uiso 1 1 calc R . . H79B H 0.0368 0.7129 0.5142 0.054 Uiso 1 1 calc R . . H79C H 0.0693 0.6708 0.4674 0.054 Uiso 1 1 calc R . . C80 C -0.02543(14) 0.79794(16) 0.25250(13) 0.0203(6) Uani 1 1 d . . . H80A H -0.0280 0.7990 0.2104 0.024 Uiso 1 1 calc R . . H80B H -0.0339 0.7502 0.2640 0.024 Uiso 1 1 calc R . . C81 C -0.07512(15) 0.84524(17) 0.27257(14) 0.0237(6) Uani 1 1 d . . . H81A H -0.0657 0.8938 0.2645 0.028 Uiso 1 1 calc R . . H81B H -0.0771 0.8402 0.3142 0.028 Uiso 1 1 calc R . . C82 C -0.13674(15) 0.82536(18) 0.24069(15) 0.0274(7) Uani 1 1 d . . . H82A H -0.1346 0.8314 0.1992 0.033 Uiso 1 1 calc R . . H82B H -0.1450 0.7763 0.2478 0.033 Uiso 1 1 calc R . . C83 C -0.18917(17) 0.8699(2) 0.26019(17) 0.0345(8) Uani 1 1 d . . . H83A H -0.1913 0.8643 0.3013 0.052 Uiso 1 1 calc R . . H83B H -0.2271 0.8550 0.2399 0.052 Uiso 1 1 calc R . . H83C H -0.1820 0.9183 0.2516 0.052 Uiso 1 1 calc R . . C84 C 0.07888(15) 0.75812(17) 0.25262(14) 0.0233(6) Uani 1 1 d . . . H84A H 0.0643 0.7135 0.2661 0.028 Uiso 1 1 calc R . . H84B H 0.0727 0.7580 0.2105 0.028 Uiso 1 1 calc R . . C85 C 0.14667(16) 0.7629(2) 0.26994(17) 0.0342(8) Uani 1 1 d . . . H85A H 0.1535 0.7775 0.3102 0.041 Uiso 1 1 calc R . . H85B H 0.1650 0.7976 0.2461 0.041 Uiso 1 1 calc R . . C86 C 0.1766(2) 0.6908(3) 0.2620(2) 0.0572(13) Uani 1 1 d . . . H86A H 0.1553 0.6558 0.2831 0.069 Uiso 1 1 calc R . . H86B H 0.1719 0.6783 0.2211 0.069 Uiso 1 1 calc R . . C87 C 0.2432(2) 0.6891(3) 0.2828(3) 0.0663(15) Uani 1 1 d . . . H87A H 0.2647 0.7239 0.2624 0.099 Uiso 1 1 calc R . . H87B H 0.2596 0.6436 0.2757 0.099 Uiso 1 1 calc R . . H87C H 0.2481 0.6989 0.3238 0.099 Uiso 1 1 calc R . . N1 N 0.32257(13) 0.00693(13) 0.76305(12) 0.0230(5) Uani 1 1 d . . . N2 N 0.42069(12) -0.06339(13) 0.84018(12) 0.0225(5) Uani 1 1 d . . . H2 H 0.4085 -0.0374 0.8674 0.027 Uiso 1 1 calc R . . N3 N 0.51709(12) -0.02878(14) 0.87259(11) 0.0207(5) Uani 1 1 d . . . H3 H 0.5002 -0.0076 0.9000 0.025 Uiso 1 1 calc R . . N4 N 0.39717(13) 0.13957(14) 0.78132(12) 0.0249(6) Uani 1 1 d . . . H4 H 0.4061 0.1188 0.8140 0.030 Uiso 1 1 calc R . . N5 N 0.40478(14) 0.24196(14) 0.83280(12) 0.0271(6) Uani 1 1 d . . . H5 H 0.4161 0.2168 0.8627 0.032 Uiso 1 1 calc R . . N6 N 0.26517(13) 0.07914(15) 0.84838(13) 0.0281(6) Uani 1 1 d . . . H6 H 0.3036 0.0695 0.8515 0.034 Uiso 1 1 calc R . . N7 N 0.28715(12) 0.15487(15) 0.92376(12) 0.0238(6) Uani 1 1 d . . . H7 H 0.3246 0.1509 0.9157 0.029 Uiso 1 1 calc R . . N8 N 0.55956(13) 0.03441(14) 1.11003(11) 0.0224(5) Uani 1 1 d . . . N9 N 0.47888(13) 0.15943(14) 1.07851(12) 0.0247(6) Uani 1 1 d . . . H9 H 0.4706 0.1362 1.0469 0.030 Uiso 1 1 calc R . . N10 N 0.47151(12) 0.25832(14) 1.02224(11) 0.0234(6) Uani 1 1 d . . . H10 H 0.4595 0.2316 0.9935 0.028 Uiso 1 1 calc R . . N11 N 0.61286(12) 0.10466(15) 1.02023(13) 0.0272(6) Uani 1 1 d . . . H11 H 0.5746 0.0942 1.0185 0.033 Uiso 1 1 calc R . . N12 N 0.58811(12) 0.16391(14) 0.93629(12) 0.0233(6) Uani 1 1 d . . . H12 H 0.5508 0.1578 0.9440 0.028 Uiso 1 1 calc R . . N13 N 0.46839(12) -0.04954(13) 1.03682(11) 0.0216(5) Uani 1 1 d . . . H13 H 0.4799 -0.0270 1.0074 0.026 Uiso 1 1 calc R . . N14 N 0.37051(12) -0.02272(14) 1.00117(12) 0.0217(5) Uani 1 1 d . . . H14 H 0.3860 -0.0054 0.9714 0.026 Uiso 1 1 calc R . . N15 N 0.34737(11) 0.70814(13) 0.07724(11) 0.0182(5) Uani 1 1 d . . . N16 N 0.03968(12) 0.81597(13) 0.27530(11) 0.0197(5) Uani 1 1 d . . . O1 O 0.50326(11) -0.10945(11) 0.79944(10) 0.0251(5) Uani 1 1 d . . . O2 O 0.37311(13) 0.24265(12) 0.73578(10) 0.0320(6) Uani 1 1 d . . . O3 O 0.18729(10) 0.12996(13) 0.89186(11) 0.0288(5) Uani 1 1 d . . . O4 O 0.50515(11) 0.26448(12) 1.11865(9) 0.0258(5) Uani 1 1 d . . . O5 O 0.68883(10) 0.15245(12) 0.97191(10) 0.0253(5) Uani 1 1 d . . . O6 O 0.38741(10) -0.09163(11) 1.08189(9) 0.0225(5) Uani 1 1 d . . . O7 O 0.39734(9) 0.06762(11) 0.90349(9) 0.0212(4) Uani 1 1 d . . . O8 O 0.48428(9) 0.07051(11) 0.96146(9) 0.0215(4) Uani 1 1 d . . . O9 O 0.43959(14) 0.16970(11) 0.93074(10) 0.0324(5) Uani 1 1 d . . . F1 F 0.56761(9) 0.00969(11) 0.76852(8) 0.0308(4) Uani 1 1 d . . . F2 F 0.68803(11) 0.02821(15) 0.76440(10) 0.0498(6) Uani 1 1 d . . . F3 F 0.76490(11) 0.01872(17) 0.86253(13) 0.0620(8) Uani 1 1 d . . . F4 F 0.72004(10) -0.01711(13) 0.96571(10) 0.0441(6) Uani 1 1 d . . . F5 F 0.59990(9) -0.04344(10) 0.96863(8) 0.0276(4) Uani 1 1 d . . . F6 F 0.34721(10) 0.30147(10) 0.92166(8) 0.0313(4) Uani 1 1 d . . . F7 F 0.34409(10) 0.43990(11) 0.94023(9) 0.0333(5) Uani 1 1 d . . . F8 F 0.39561(10) 0.52974(10) 0.86608(10) 0.0363(5) Uani 1 1 d . . . F9 F 0.45158(11) 0.47695(11) 0.77503(11) 0.0424(6) Uani 1 1 d . . . F10 F 0.46247(10) 0.33916(11) 0.76077(9) 0.0351(5) Uani 1 1 d . . . F11 F 0.19937(10) 0.26743(12) 0.92262(9) 0.0382(5) Uani 1 1 d . . . F12 F 0.18194(12) 0.33723(14) 1.02037(12) 0.0558(7) Uani 1 1 d . . . F13 F 0.25128(14) 0.31004(16) 1.12068(12) 0.0623(8) Uani 1 1 d . . . F14 F 0.33942(12) 0.20886(13) 1.12274(10) 0.0471(6) Uani 1 1 d . . . F15 F 0.35445(9) 0.13438(10) 1.02571(8) 0.0285(4) Uani 1 1 d . . . F16 F 0.41663(10) 0.35954(11) 1.09178(9) 0.0349(5) Uani 1 1 d . . . F17 F 0.43237(12) 0.49661(11) 1.07625(11) 0.0452(6) Uani 1 1 d . . . F18 F 0.48962(11) 0.54473(11) 0.98418(11) 0.0416(5) Uani 1 1 d . . . F19 F 0.53598(9) 0.45133(11) 0.91008(9) 0.0350(5) Uani 1 1 d . . . F20 F 0.52837(9) 0.31278(11) 0.92993(9) 0.0313(4) Uani 1 1 d . . . F21 F 0.52783(9) 0.12158(10) 0.83405(9) 0.0294(4) Uani 1 1 d . . . F22 F 0.54363(12) 0.18232(12) 0.73080(9) 0.0430(5) Uani 1 1 d . . . F23 F 0.62354(12) 0.29134(13) 0.72606(9) 0.0471(6) Uani 1 1 d . . . F24 F 0.68184(10) 0.34243(11) 0.82560(10) 0.0392(5) Uani 1 1 d . . . F25 F 0.66385(9) 0.28496(10) 0.92896(8) 0.0301(4) Uani 1 1 d . . . F26 F 0.32022(9) 0.03543(10) 1.09904(8) 0.0281(4) Uani 1 1 d . . . F27 F 0.19939(10) 0.04980(12) 1.10300(9) 0.0400(5) Uani 1 1 d . . . F28 F 0.12109(10) 0.01147(13) 1.01065(11) 0.0453(6) Uani 1 1 d . . . F29 F 0.16584(10) -0.04589(12) 0.91450(10) 0.0426(5) Uani 1 1 d . . . F30 F 0.28730(9) -0.06603(10) 0.91227(8) 0.0298(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0311(17) 0.0217(15) 0.0175(16) -0.0045(12) -0.0001(12) 0.0018(12) C2 0.0299(17) 0.0204(15) 0.0233(17) -0.0028(12) -0.0006(13) 0.0004(12) C3 0.0271(16) 0.0181(14) 0.0167(15) 0.0037(11) 0.0025(12) 0.0027(12) C4 0.0251(16) 0.0209(15) 0.0222(16) -0.0007(12) 0.0035(12) 0.0004(12) C5 0.0307(18) 0.0275(16) 0.0227(17) 0.0041(13) 0.0016(14) 0.0026(13) C6 0.0318(19) 0.042(2) 0.031(2) 0.0104(16) 0.0127(15) 0.0010(15) C7 0.0205(17) 0.048(2) 0.046(2) 0.0133(18) 0.0046(16) -0.0003(15) C8 0.0259(18) 0.0374(19) 0.033(2) 0.0099(15) -0.0028(15) 0.0021(14) C9 0.0285(17) 0.0246(15) 0.0214(16) 0.0072(12) 0.0032(13) 0.0014(12) C10 0.0410(19) 0.0264(16) 0.0133(15) -0.0019(12) -0.0049(13) 0.0050(14) C11 0.042(2) 0.0217(16) 0.0192(16) 0.0009(12) 0.0079(14) -0.0019(14) C12 0.0296(17) 0.0248(15) 0.0173(15) 0.0036(12) 0.0027(13) -0.0024(12) C13 0.0283(17) 0.0228(15) 0.0188(16) 0.0057(12) -0.0053(12) 0.0004(12) C14 0.0228(15) 0.0240(15) 0.0218(16) 0.0029(12) -0.0030(12) -0.0041(12) C15 0.0252(16) 0.0294(17) 0.0246(18) -0.0025(13) 0.0013(13) 0.0029(13) C16 0.0303(18) 0.0198(15) 0.0348(19) 0.0010(13) 0.0015(15) 0.0009(13) C17 0.0287(17) 0.0257(17) 0.0335(19) 0.0107(14) 0.0047(14) -0.0003(13) C18 0.0307(17) 0.0259(16) 0.0232(17) 0.0009(13) 0.0030(13) 0.0045(13) C19 0.0240(17) 0.0335(18) 0.0254(18) -0.0041(14) -0.0032(13) -0.0013(13) C20 0.0249(17) 0.040(2) 0.0290(19) -0.0058(15) -0.0055(14) 0.0054(14) C21 0.0227(16) 0.0270(16) 0.0193(16) 0.0032(12) -0.0028(12) 0.0027(12) C22 0.0230(16) 0.0246(15) 0.0225(17) 0.0032(12) 0.0014(13) -0.0039(12) C23 0.0288(17) 0.0321(18) 0.0290(18) -0.0004(14) 0.0015(14) 0.0016(14) C24 0.039(2) 0.0310(19) 0.047(2) -0.0074(17) 0.0027(17) 0.0059(15) C25 0.048(2) 0.038(2) 0.035(2) -0.0135(17) 0.0043(18) 0.0002(17) C26 0.043(2) 0.036(2) 0.0276(19) -0.0051(15) -0.0056(16) -0.0080(15) C27 0.0267(17) 0.0240(15) 0.0259(17) 0.0008(13) 0.0012(13) -0.0040(12) C28 0.041(2) 0.0223(15) 0.0159(16) 0.0008(12) -0.0042(13) -0.0047(13) C29 0.0360(18) 0.0251(16) 0.0204(16) 0.0012(13) 0.0061(14) -0.0030(13) C30 0.0201(15) 0.0253(15) 0.0176(15) -0.0049(12) 0.0018(12) 0.0011(12) C31 0.0206(15) 0.0230(15) 0.0223(16) -0.0019(12) -0.0060(12) 0.0025(12) C32 0.0248(16) 0.0315(17) 0.0235(17) -0.0020(13) 0.0027(13) 0.0002(13) C33 0.0338(19) 0.0223(16) 0.038(2) -0.0093(14) 0.0010(15) 0.0017(13) C34 0.0264(17) 0.0259(17) 0.040(2) 0.0019(15) -0.0012(15) -0.0010(13) C35 0.0193(15) 0.0313(17) 0.0271(17) 0.0033(13) -0.0021(13) -0.0032(12) C36 0.0201(15) 0.0269(16) 0.0261(17) -0.0043(13) -0.0026(13) 0.0046(12) C37 0.0247(16) 0.0318(17) 0.0252(17) 0.0047(14) -0.0066(13) -0.0054(13) C38 0.0288(18) 0.0331(18) 0.0279(18) 0.0070(14) -0.0040(14) -0.0084(14) C39 0.0227(16) 0.0196(14) 0.0209(16) -0.0038(12) 0.0010(12) -0.0024(11) C40 0.0191(15) 0.0256(16) 0.0207(16) 0.0036(12) 0.0023(12) 0.0044(11) C41 0.0245(16) 0.0212(15) 0.0280(18) 0.0002(13) -0.0006(13) 0.0007(12) C42 0.0343(18) 0.0347(18) 0.0182(17) 0.0018(13) -0.0063(14) 0.0038(14) C43 0.041(2) 0.0352(19) 0.0240(18) 0.0125(14) 0.0013(15) -0.0008(15) C44 0.0274(17) 0.0285(17) 0.0291(18) 0.0064(14) 0.0019(14) -0.0010(13) C45 0.0240(16) 0.0268(16) 0.0222(16) -0.0009(12) -0.0004(12) -0.0016(12) C46 0.0257(16) 0.0201(14) 0.0186(16) 0.0018(12) 0.0010(12) -0.0018(12) C47 0.0221(15) 0.0192(14) 0.0214(16) 0.0009(12) 0.0023(12) -0.0013(11) C48 0.0229(15) 0.0192(14) 0.0165(15) -0.0028(11) 0.0010(12) -0.0034(11) C49 0.0231(16) 0.0202(14) 0.0198(16) 0.0047(11) 0.0034(12) -0.0012(11) C50 0.0254(16) 0.0234(15) 0.0191(15) 0.0029(12) -0.0004(12) -0.0013(12) C51 0.0331(19) 0.0248(16) 0.0274(18) -0.0009(13) 0.0094(14) 0.0025(13) C52 0.0212(16) 0.0315(18) 0.044(2) 0.0012(15) 0.0020(15) 0.0018(13) C53 0.0290(18) 0.0290(18) 0.0309(19) -0.0018(14) -0.0035(14) 0.0006(13) C54 0.0290(17) 0.0227(15) 0.0220(16) 0.0004(12) 0.0031(13) -0.0011(12) C55 0.0205(13) 0.0197(14) 0.0121(13) 0.0006(11) 0.0035(10) 0.0003(11) C56 0.0242(15) 0.0193(14) 0.0161(15) -0.0013(11) -0.0016(12) -0.0018(11) C57 0.0297(17) 0.0219(15) 0.0181(16) -0.0023(12) 0.0005(13) -0.0004(12) C58 0.0236(16) 0.0273(16) 0.0223(16) -0.0015(13) -0.0008(13) 0.0040(12) C59 0.0310(18) 0.0378(19) 0.0257(18) 0.0010(15) -0.0009(14) 0.0107(15) C60 0.0254(16) 0.0210(14) 0.0146(15) -0.0003(11) -0.0001(12) 0.0001(12) C61 0.0296(17) 0.0275(16) 0.0199(16) 0.0022(12) -0.0006(13) -0.0048(13) C62 0.0306(17) 0.0310(17) 0.0191(16) 0.0047(13) 0.0039(13) 0.0014(13) C63 0.046(2) 0.040(2) 0.0203(18) 0.0018(15) -0.0019(15) -0.0081(16) C64 0.0237(15) 0.0197(14) 0.0171(15) -0.0025(11) 0.0024(12) -0.0035(11) C65 0.0230(17) 0.0342(18) 0.047(2) -0.0157(16) 0.0003(15) -0.0038(14) C66 0.0267(18) 0.0366(19) 0.033(2) -0.0027(15) 0.0066(15) 0.0013(14) C67 0.030(2) 0.068(3) 0.043(2) -0.015(2) 0.0025(17) 0.0107(19) C68 0.0277(16) 0.0171(14) 0.0201(16) 0.0005(11) 0.0009(12) -0.0059(12) C69 0.0327(18) 0.0231(15) 0.0224(17) -0.0014(13) 0.0018(13) -0.0044(13) C70 0.0352(18) 0.0258(16) 0.0236(17) 0.0068(13) 0.0039(14) -0.0032(13) C71 0.047(2) 0.0223(16) 0.037(2) 0.0047(15) 0.0071(17) -0.0049(15) C72 0.0269(16) 0.0189(14) 0.0206(16) -0.0014(12) 0.0041(12) -0.0032(12) C73 0.0329(18) 0.0238(15) 0.0184(16) 0.0001(12) 0.0029(13) -0.0053(13) C74 0.0328(18) 0.0306(17) 0.0248(18) 0.0048(14) 0.0062(14) -0.0014(14) C75 0.048(2) 0.0262(17) 0.035(2) 0.0063(15) 0.0070(17) -0.0035(15) C76 0.0211(15) 0.0224(14) 0.0155(15) -0.0037(11) 0.0002(11) -0.0011(11) C77 0.0274(16) 0.0225(15) 0.0197(16) 0.0000(12) 0.0023(12) 0.0013(12) C78 0.0392(19) 0.0281(17) 0.0178(16) 0.0016(13) 0.0021(14) 0.0032(14) C79 0.050(2) 0.0321(19) 0.0263(19) 0.0057(15) 0.0080(16) 0.0075(16) C80 0.0247(15) 0.0218(15) 0.0139(14) -0.0041(11) 0.0002(12) -0.0036(12) C81 0.0257(16) 0.0235(15) 0.0219(16) -0.0028(12) 0.0012(13) 0.0005(12) C82 0.0263(17) 0.0304(17) 0.0257(18) -0.0026(13) 0.0038(14) 0.0009(13) C83 0.0340(19) 0.038(2) 0.032(2) 0.0015(15) 0.0028(15) 0.0077(15) C84 0.0287(17) 0.0244(15) 0.0164(15) -0.0065(12) -0.0002(12) 0.0017(12) C85 0.0262(17) 0.043(2) 0.033(2) -0.0188(16) -0.0008(15) 0.0038(14) C86 0.037(2) 0.069(3) 0.062(3) -0.037(3) -0.010(2) 0.010(2) C87 0.041(3) 0.094(4) 0.063(3) -0.029(3) -0.001(2) 0.021(3) N1 0.0290(14) 0.0219(13) 0.0178(13) -0.0007(10) 0.0005(11) 0.0028(11) N2 0.0255(14) 0.0209(12) 0.0211(13) -0.0052(10) 0.0024(11) 0.0008(10) N3 0.0219(13) 0.0221(13) 0.0185(13) -0.0023(10) 0.0048(10) 0.0016(10) N4 0.0365(15) 0.0243(13) 0.0135(13) 0.0035(10) -0.0004(11) -0.0023(11) N5 0.0431(17) 0.0223(13) 0.0142(13) 0.0025(10) -0.0063(12) -0.0012(12) N6 0.0214(13) 0.0348(15) 0.0273(15) -0.0029(12) -0.0015(11) 0.0060(11) N7 0.0175(13) 0.0321(14) 0.0217(14) -0.0005(11) 0.0013(10) 0.0009(10) N8 0.0288(14) 0.0193(12) 0.0186(14) 0.0006(10) -0.0009(11) -0.0061(10) N9 0.0330(15) 0.0227(13) 0.0179(13) -0.0021(10) -0.0008(11) -0.0011(11) N10 0.0322(15) 0.0202(13) 0.0171(13) -0.0050(10) -0.0015(11) 0.0024(10) N11 0.0198(13) 0.0336(15) 0.0274(15) 0.0096(12) -0.0026(11) -0.0097(11) N12 0.0200(13) 0.0315(14) 0.0187(13) 0.0015(11) 0.0041(10) -0.0037(10) N13 0.0247(14) 0.0230(13) 0.0173(13) 0.0031(10) 0.0018(10) -0.0045(10) N14 0.0226(13) 0.0264(13) 0.0164(13) 0.0026(10) 0.0033(10) -0.0024(10) N15 0.0220(13) 0.0179(12) 0.0148(12) 0.0002(9) 0.0018(10) -0.0044(9) N16 0.0245(13) 0.0177(12) 0.0170(13) -0.0006(10) 0.0012(10) -0.0004(10) O1 0.0321(12) 0.0216(11) 0.0219(12) -0.0022(9) 0.0043(9) 0.0039(9) O2 0.0515(16) 0.0263(12) 0.0168(12) 0.0051(9) -0.0058(10) 0.0024(11) O3 0.0201(12) 0.0363(13) 0.0300(13) -0.0003(10) 0.0007(9) 0.0059(9) O4 0.0334(12) 0.0271(11) 0.0169(11) -0.0050(9) 0.0013(9) -0.0043(9) O5 0.0209(11) 0.0295(12) 0.0252(12) 0.0040(9) 0.0007(9) -0.0059(9) O6 0.0238(11) 0.0236(11) 0.0198(11) 0.0018(9) 0.0010(9) -0.0056(8) O7 0.0190(11) 0.0247(11) 0.0196(11) 0.0007(9) -0.0003(9) -0.0018(8) O8 0.0211(11) 0.0249(11) 0.0184(11) 0.0028(8) 0.0012(9) -0.0009(8) O9 0.0624(15) 0.0176(11) 0.0156(11) -0.0005(9) -0.0054(10) -0.0002(11) F1 0.0375(11) 0.0369(11) 0.0179(10) 0.0023(8) 0.0018(8) -0.0011(9) F2 0.0382(13) 0.0786(18) 0.0352(13) 0.0186(12) 0.0172(10) -0.0010(12) F3 0.0191(11) 0.100(2) 0.0676(18) 0.0386(16) 0.0051(11) -0.0027(12) F4 0.0297(11) 0.0599(15) 0.0406(13) 0.0182(11) -0.0085(10) -0.0020(10) F5 0.0315(10) 0.0309(10) 0.0204(10) 0.0061(8) 0.0027(8) -0.0014(8) F6 0.0442(12) 0.0267(10) 0.0237(10) 0.0046(8) 0.0070(9) -0.0050(8) F7 0.0387(12) 0.0343(11) 0.0276(11) -0.0024(8) 0.0061(9) 0.0035(9) F8 0.0430(12) 0.0195(9) 0.0474(13) 0.0005(9) 0.0096(10) 0.0003(8) F9 0.0535(14) 0.0238(10) 0.0537(15) 0.0085(9) 0.0260(12) -0.0036(9) F10 0.0439(12) 0.0295(10) 0.0339(12) 0.0025(9) 0.0139(10) 0.0032(9) F11 0.0391(12) 0.0385(12) 0.0357(12) 0.0045(9) -0.0035(9) 0.0111(9) F12 0.0545(15) 0.0469(14) 0.0653(18) -0.0184(13) 0.0005(13) 0.0213(12) F13 0.0741(19) 0.0671(18) 0.0447(16) -0.0303(13) -0.0009(14) 0.0150(14) F14 0.0596(15) 0.0527(15) 0.0263(12) -0.0098(10) -0.0111(10) 0.0021(12) F15 0.0316(10) 0.0278(10) 0.0246(10) 0.0026(8) -0.0057(8) -0.0005(8) F16 0.0399(12) 0.0313(11) 0.0351(12) -0.0028(9) 0.0134(9) 0.0019(9) F17 0.0582(15) 0.0246(10) 0.0554(15) -0.0106(10) 0.0188(12) 0.0050(10) F18 0.0454(13) 0.0229(10) 0.0565(15) 0.0023(10) 0.0036(11) -0.0026(9) F19 0.0306(11) 0.0377(12) 0.0369(12) 0.0064(9) 0.0042(9) -0.0041(9) F20 0.0359(11) 0.0338(11) 0.0246(10) -0.0026(8) 0.0051(8) 0.0067(8) F21 0.0333(11) 0.0256(10) 0.0281(11) -0.0012(8) -0.0039(8) -0.0034(8) F22 0.0590(15) 0.0443(13) 0.0230(11) 0.0023(9) -0.0125(10) -0.0071(11) F23 0.0625(15) 0.0525(14) 0.0249(12) 0.0179(10) -0.0040(10) -0.0073(12) F24 0.0417(12) 0.0379(12) 0.0373(12) 0.0123(10) -0.0002(10) -0.0104(9) F25 0.0342(11) 0.0310(10) 0.0244(10) -0.0011(8) -0.0006(8) -0.0089(8) F26 0.0338(11) 0.0325(10) 0.0180(10) -0.0007(8) 0.0015(8) -0.0026(8) F27 0.0392(12) 0.0480(13) 0.0347(12) -0.0086(10) 0.0144(10) 0.0047(10) F28 0.0231(11) 0.0554(15) 0.0575(15) -0.0092(12) 0.0041(10) 0.0048(10) F29 0.0311(11) 0.0487(13) 0.0450(14) -0.0123(11) -0.0128(10) -0.0010(10) F30 0.0328(10) 0.0334(10) 0.0224(10) -0.0069(8) -0.0010(8) 0.0026(8) _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 C1 N1 1.466(4) . ? C1 C2 1.523(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.446(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 O1 1.230(4) . ? C3 N2 1.358(4) . ? C3 N3 1.373(4) . ? C4 C9 1.387(5) . ? C4 C5 1.392(5) . ? C4 N3 1.403(4) . ? C5 F1 1.336(4) . ? C5 C6 1.382(5) . ? C6 F2 1.345(4) . ? C6 C7 1.379(6) . ? C7 F3 1.338(4) . ? C7 C8 1.380(5) . ? C8 F4 1.338(4) . ? C8 C9 1.373(5) . ? C9 F5 1.343(4) . ? C10 N1 1.474(4) . ? C10 C11 1.519(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N4 1.448(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 O2 1.229(4) . ? C12 N4 1.343(4) . ? C12 N5 1.382(4) . ? C13 C14 1.394(5) . ? C13 N5 1.393(4) . ? C13 C18 1.395(5) . ? C14 F6 1.336(4) . ? C14 C15 1.377(5) . ? C15 F7 1.342(4) . ? C15 C16 1.377(5) . ? C16 F8 1.339(4) . ? C16 C17 1.378(5) . ? C17 F9 1.347(4) . ? C17 C18 1.380(5) . ? C18 F10 1.342(4) . ? C19 N1 1.464(4) . ? C19 C20 1.526(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 N6 1.452(4) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 O3 1.223(4) . ? C21 N6 1.354(4) . ? C21 N7 1.383(4) . ? C22 N7 1.390(4) . ? C22 C27 1.393(5) . ? C22 C23 1.399(5) . ? C23 F11 1.343(4) . ? C23 C24 1.383(5) . ? C24 F12 1.340(4) . ? C24 C25 1.378(6) . ? C25 F13 1.334(5) . ? C25 C26 1.374(6) . ? C26 F14 1.328(4) . ? C26 C27 1.391(5) . ? C27 F15 1.337(4) . ? C28 N8 1.469(4) . ? C28 C29 1.519(5) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 N9 1.458(4) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 O4 1.220(4) . ? C30 N9 1.346(4) . ? C30 N10 1.383(4) . ? C31 C36 1.390(5) . ? C31 C32 1.394(4) . ? C31 N10 1.398(4) . ? C32 F16 1.336(4) . ? C32 C33 1.384(5) . ? C33 F17 1.352(4) . ? C33 C34 1.368(5) . ? C34 F18 1.345(4) . ? C34 C35 1.373(5) . ? C35 F19 1.342(4) . ? C35 C36 1.380(5) . ? C36 F20 1.346(4) . ? C37 N8 1.465(4) . ? C37 C38 1.518(5) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 N11 1.454(4) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 O5 1.232(4) . ? C39 N11 1.345(4) . ? C39 N12 1.378(4) . ? C40 C41 1.380(5) . ? C40 N12 1.401(4) . ? C40 C45 1.398(5) . ? C41 F21 1.337(4) . ? C41 C42 1.381(5) . ? C42 F22 1.356(4) . ? C42 C43 1.367(5) . ? C43 F23 1.337(4) . ? C43 C44 1.384(5) . ? C44 F24 1.340(4) . ? C44 C45 1.388(5) . ? C45 F25 1.338(4) . ? C46 N8 1.471(4) . ? C46 C47 1.521(4) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 N13 1.442(4) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 O6 1.233(4) . ? C48 N13 1.350(4) . ? C48 N14 1.378(4) . ? C49 C50 1.391(4) . ? C49 C54 1.400(5) . ? C49 N14 1.393(4) . ? C50 F26 1.333(4) . ? C50 C51 1.370(5) . ? C51 F27 1.345(4) . ? C51 C52 1.382(5) . ? C52 F28 1.343(4) . ? C52 C53 1.371(5) . ? C53 F29 1.346(4) . ? C53 C54 1.377(5) . ? C54 F30 1.343(4) . ? C55 O9 1.283(4) 1 ? C55 O9 1.283(4) . ? C55 O7 1.284(4) . ? C55 O7 1.284(4) 1 ? C55 O8 1.285(4) . ? C55 O8 1.285(4) 1 ? C56 C57 1.518(4) . ? C56 N15 1.526(4) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 C58 1.527(4) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 C59 1.532(5) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 C61 1.515(4) . ? C60 N15 1.519(4) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 C62 1.539(4) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 C63 1.518(5) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 C65 1.517(5) . ? C64 N15 1.530(4) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 C66 1.506(5) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 C67 1.505(5) . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 N15 1.515(4) . ? C68 C69 1.530(4) . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C69 C70 1.524(4) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 C71 1.516(5) . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C72 N16 1.517(4) . ? C72 C73 1.530(5) . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C73 C74 1.536(5) . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C74 C75 1.515(5) . ? C74 H74A 0.9700 . ? C74 H74B 0.9700 . ? C75 H75A 0.9600 . ? C75 H75B 0.9600 . ? C75 H75C 0.9600 . ? C76 C77 1.504(4) . ? C76 N16 1.521(4) . ? C76 H76A 0.9700 . ? C76 H76B 0.9700 . ? C77 C78 1.528(4) . ? C77 H77A 0.9700 . ? C77 H77B 0.9700 . ? C78 C79 1.520(5) . ? C78 H78A 0.9700 . ? C78 H78B 0.9700 . ? C79 H79A 0.9600 . ? C79 H79B 0.9600 . ? C79 H79C 0.9600 . ? C80 C81 1.518(4) . ? C80 N16 1.517(4) . ? C80 H80A 0.9700 . ? C80 H80B 0.9700 . ? C81 C82 1.528(5) . ? C81 H81A 0.9700 . ? C81 H81B 0.9700 . ? C82 C83 1.528(5) . ? C82 H82A 0.9700 . ? C82 H82B 0.9700 . ? C83 H83A 0.9600 . ? C83 H83B 0.9600 . ? C83 H83C 0.9600 . ? C84 C85 1.508(5) . ? C84 N16 1.519(4) . ? C84 H84A 0.9700 . ? C84 H84B 0.9700 . ? C85 C86 1.541(6) . ? C85 H85A 0.9700 . ? C85 H85B 0.9700 . ? C86 C87 1.497(7) . ? C86 H86A 0.9700 . ? C86 H86B 0.9700 . ? C87 H87A 0.9600 . ? C87 H87B 0.9600 . ? C87 H87C 0.9600 . ? N2 H2 0.8600 . ? N3 H3 0.8600 . ? N4 H4 0.8600 . ? N5 H5 0.8600 . ? N6 H6 0.8600 . ? N7 H7 0.8600 . ? N9 H9 0.8600 . ? N10 H10 0.8600 . ? N11 H11 0.8600 . ? N12 H12 0.8600 . ? N13 H13 0.8600 . ? N14 H14 0.8600 . ? O7 O7 0.000(4) 1 ? O8 O8 0.000(8) 1 ? O9 O9 0.000(9) 1 ? 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 N1 C1 C2 111.8(3) . . ? N1 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? N1 C1 H1B 109.3 . . ? C2 C1 H1B 109.3 . . ? H1A C1 H1B 107.9 . . ? N2 C2 C1 112.8(3) . . ? N2 C2 H2A 109.0 . . ? C1 C2 H2A 109.0 . . ? N2 C2 H2B 109.0 . . ? C1 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? O1 C3 N2 124.2(3) . . ? O1 C3 N3 122.7(3) . . ? N2 C3 N3 113.0(3) . . ? C9 C4 C5 116.9(3) . . ? C9 C4 N3 120.4(3) . . ? C5 C4 N3 122.5(3) . . ? F1 C5 C6 117.9(3) . . ? F1 C5 C4 120.8(3) . . ? C6 C5 C4 121.2(3) . . ? F2 C6 C7 120.3(3) . . ? F2 C6 C5 119.7(3) . . ? C7 C6 C5 120.0(3) . . ? F3 C7 C8 120.9(4) . . ? F3 C7 C6 119.1(3) . . ? C8 C7 C6 119.9(3) . . ? F4 C8 C9 120.6(3) . . ? F4 C8 C7 120.3(3) . . ? C9 C8 C7 119.2(3) . . ? F5 C9 C8 118.2(3) . . ? F5 C9 C4 119.2(3) . . ? C8 C9 C4 122.6(3) . . ? N1 C10 C11 111.0(3) . . ? N1 C10 H10A 109.4 . . ? C11 C10 H10A 109.4 . . ? N1 C10 H10B 109.4 . . ? C11 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? N4 C11 C10 112.9(3) . . ? N4 C11 H11A 109.0 . . ? C10 C11 H11A 109.0 . . ? N4 C11 H11B 109.0 . . ? C10 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? O2 C12 N4 123.8(3) . . ? O2 C12 N5 122.2(3) . . ? N4 C12 N5 114.0(3) . . ? C14 C13 N5 120.2(3) . . ? C14 C13 C18 116.0(3) . . ? N5 C13 C18 123.7(3) . . ? F6 C14 C15 118.0(3) . . ? F6 C14 C13 119.2(3) . . ? C15 C14 C13 122.8(3) . . ? F7 C15 C16 120.1(3) . . ? F7 C15 C14 120.1(3) . . ? C16 C15 C14 119.8(3) . . ? F8 C16 C15 120.8(3) . . ? F8 C16 C17 120.3(3) . . ? C15 C16 C17 118.8(3) . . ? F9 C17 C18 119.3(3) . . ? F9 C17 C16 119.6(3) . . ? C18 C17 C16 121.0(3) . . ? F10 C18 C17 117.6(3) . . ? F10 C18 C13 120.9(3) . . ? C17 C18 C13 121.4(3) . . ? N1 C19 C20 113.2(3) . . ? N1 C19 H19A 108.9 . . ? C20 C19 H19A 108.9 . . ? N1 C19 H19B 108.9 . . ? C20 C19 H19B 108.9 . . ? H19A C19 H19B 107.7 . . ? N6 C20 C19 110.2(3) . . ? N6 C20 H20A 109.6 . . ? C19 C20 H20A 109.6 . . ? N6 C20 H20B 109.6 . . ? C19 C20 H20B 109.6 . . ? H20A C20 H20B 108.1 . . ? O3 C21 N6 123.6(3) . . ? O3 C21 N7 123.6(3) . . ? N6 C21 N7 112.8(3) . . ? N7 C22 C27 118.8(3) . . ? N7 C22 C23 125.0(3) . . ? C27 C22 C23 116.1(3) . . ? F11 C23 C24 118.0(3) . . ? F11 C23 C22 120.6(3) . . ? C24 C23 C22 121.1(3) . . ? F12 C24 C23 119.5(4) . . ? F12 C24 C25 119.4(4) . . ? C23 C24 C25 121.1(4) . . ? F13 C25 C26 120.1(4) . . ? F13 C25 C24 120.2(4) . . ? C26 C25 C24 119.6(4) . . ? F14 C26 C25 121.1(3) . . ? F14 C26 C27 120.0(4) . . ? C25 C26 C27 118.9(4) . . ? F15 C27 C26 118.6(3) . . ? F15 C27 C22 118.2(3) . . ? C26 C27 C22 123.2(3) . . ? N8 C28 C29 110.5(3) . . ? N8 C28 H28A 109.5 . . ? C29 C28 H28A 109.5 . . ? N8 C28 H28B 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 108.1 . . ? N9 C29 C28 112.6(3) . . ? N9 C29 H29A 109.1 . . ? C28 C29 H29A 109.1 . . ? N9 C29 H29B 109.1 . . ? C28 C29 H29B 109.1 . . ? H29A C29 H29B 107.8 . . ? O4 C30 N9 123.5(3) . . ? O4 C30 N10 122.6(3) . . ? N9 C30 N10 113.9(3) . . ? C36 C31 C32 116.3(3) . . ? C36 C31 N10 120.7(3) . . ? C32 C31 N10 123.0(3) . . ? F16 C32 C33 118.0(3) . . ? F16 C32 C31 121.0(3) . . ? C33 C32 C31 121.0(3) . . ? F17 C33 C34 119.9(3) . . ? F17 C33 C32 118.9(3) . . ? C34 C33 C32 121.1(3) . . ? F18 C34 C33 120.3(3) . . ? F18 C34 C35 120.4(3) . . ? C33 C34 C35 119.3(3) . . ? F19 C35 C34 120.1(3) . . ? F19 C35 C36 120.3(3) . . ? C34 C35 C36 119.6(3) . . ? F20 C36 C35 118.0(3) . . ? F20 C36 C31 119.3(3) . . ? C35 C36 C31 122.7(3) . . ? N8 C37 C38 112.7(3) . . ? N8 C37 H37A 109.0 . . ? C38 C37 H37A 109.0 . . ? N8 C37 H37B 109.0 . . ? C38 C37 H37B 109.0 . . ? H37A C37 H37B 107.8 . . ? N11 C38 C37 111.4(3) . . ? N11 C38 H38A 109.4 . . ? C37 C38 H38A 109.4 . . ? N11 C38 H38B 109.4 . . ? C37 C38 H38B 109.4 . . ? H38A C38 H38B 108.0 . . ? O5 C39 N11 123.9(3) . . ? O5 C39 N12 123.3(3) . . ? N11 C39 N12 112.8(3) . . ? C41 C40 N12 119.6(3) . . ? C41 C40 C45 117.1(3) . . ? N12 C40 C45 123.2(3) . . ? F21 C41 C42 118.6(3) . . ? F21 C41 C40 119.2(3) . . ? C42 C41 C40 122.1(3) . . ? F22 C42 C43 119.6(3) . . ? F22 C42 C41 120.0(3) . . ? C43 C42 C41 120.4(3) . . ? F23 C43 C42 121.1(3) . . ? F23 C43 C44 119.9(3) . . ? C42 C43 C44 119.0(3) . . ? F24 C44 C43 119.5(3) . . ? F24 C44 C45 119.9(3) . . ? C43 C44 C45 120.6(3) . . ? F25 C45 C44 118.1(3) . . ? F25 C45 C40 121.1(3) . . ? C44 C45 C40 120.7(3) . . ? N8 C46 C47 111.7(2) . . ? N8 C46 H46A 109.3 . . ? C47 C46 H46A 109.3 . . ? N8 C46 H46B 109.3 . . ? C47 C46 H46B 109.3 . . ? H46A C46 H46B 107.9 . . ? N13 C47 C46 112.6(3) . . ? N13 C47 H47A 109.1 . . ? C46 C47 H47A 109.1 . . ? N13 C47 H47B 109.1 . . ? C46 C47 H47B 109.1 . . ? H47A C47 H47B 107.8 . . ? O6 C48 N13 124.0(3) . . ? O6 C48 N14 122.0(3) . . ? N13 C48 N14 114.0(3) . . ? C50 C49 C54 116.7(3) . . ? C50 C49 N14 123.5(3) . . ? C54 C49 N14 119.7(3) . . ? F26 C50 C51 118.3(3) . . ? F26 C50 C49 120.0(3) . . ? C51 C50 C49 121.7(3) . . ? F27 C51 C50 119.9(3) . . ? F27 C51 C52 119.9(3) . . ? C50 C51 C52 120.2(3) . . ? F28 C52 C53 120.4(3) . . ? F28 C52 C51 119.8(3) . . ? C53 C52 C51 119.8(3) . . ? F29 C53 C52 120.4(3) . . ? F29 C53 C54 119.9(3) . . ? C52 C53 C54 119.7(3) . . ? F30 C54 C53 118.8(3) . . ? F30 C54 C49 119.4(3) . . ? C53 C54 C49 121.8(3) . . ? O9 C55 O9 0.0(4) 1 . ? O9 C55 O7 120.0(3) 1 . ? O9 C55 O7 120.0(3) . . ? O9 C55 O7 120.0(3) 1 1 ? O9 C55 O7 120.0(3) . 1 ? O7 C55 O7 0.0(2) . 1 ? O9 C55 O8 119.4(3) 1 . ? O9 C55 O8 119.4(3) . . ? O7 C55 O8 120.6(3) . . ? O7 C55 O8 120.6(3) 1 . ? O9 C55 O8 119.4(3) 1 1 ? O9 C55 O8 119.4(3) . 1 ? O7 C55 O8 120.6(3) . 1 ? O7 C55 O8 120.6(3) 1 1 ? O8 C55 O8 0.0(2) . 1 ? C57 C56 N15 115.4(2) . . ? C57 C56 H56A 108.4 . . ? N15 C56 H56A 108.4 . . ? C57 C56 H56B 108.4 . . ? N15 C56 H56B 108.4 . . ? H56A C56 H56B 107.5 . . ? C56 C57 C58 109.4(3) . . ? C56 C57 H57A 109.8 . . ? C58 C57 H57A 109.8 . . ? C56 C57 H57B 109.8 . . ? C58 C57 H57B 109.8 . . ? H57A C57 H57B 108.2 . . ? C57 C58 C59 111.5(3) . . ? C57 C58 H58A 109.3 . . ? C59 C58 H58A 109.3 . . ? C57 C58 H58B 109.3 . . ? C59 C58 H58B 109.3 . . ? H58A C58 H58B 108.0 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C61 C60 N15 114.9(2) . . ? C61 C60 H60A 108.5 . . ? N15 C60 H60A 108.5 . . ? C61 C60 H60B 108.5 . . ? N15 C60 H60B 108.5 . . ? H60A C60 H60B 107.5 . . ? C60 C61 C62 110.3(3) . . ? C60 C61 H61A 109.6 . . ? C62 C61 H61A 109.6 . . ? C60 C61 H61B 109.6 . . ? C62 C61 H61B 109.6 . . ? H61A C61 H61B 108.1 . . ? C63 C62 C61 113.3(3) . . ? C63 C62 H62A 108.9 . . ? C61 C62 H62A 108.9 . . ? C63 C62 H62B 108.9 . . ? C61 C62 H62B 108.9 . . ? H62A C62 H62B 107.7 . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C65 C64 N15 115.2(2) . . ? C65 C64 H64A 108.5 . . ? N15 C64 H64A 108.5 . . ? C65 C64 H64B 108.5 . . ? N15 C64 H64B 108.5 . . ? H64A C64 H64B 107.5 . . ? C66 C65 C64 111.4(3) . . ? C66 C65 H65A 109.3 . . ? C64 C65 H65A 109.3 . . ? C66 C65 H65B 109.3 . . ? C64 C65 H65B 109.3 . . ? H65A C65 H65B 108.0 . . ? C67 C66 C65 113.2(3) . . ? C67 C66 H66A 108.9 . . ? C65 C66 H66A 108.9 . . ? C67 C66 H66B 108.9 . . ? C65 C66 H66B 108.9 . . ? H66A C66 H66B 107.8 . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? N15 C68 C69 116.1(2) . . ? N15 C68 H68A 108.3 . . ? C69 C68 H68A 108.3 . . ? N15 C68 H68B 108.3 . . ? C69 C68 H68B 108.3 . . ? H68A C68 H68B 107.4 . . ? C70 C69 C68 111.0(3) . . ? C70 C69 H69A 109.4 . . ? C68 C69 H69A 109.4 . . ? C70 C69 H69B 109.4 . . ? C68 C69 H69B 109.4 . . ? H69A C69 H69B 108.0 . . ? C71 C70 C69 115.1(3) . . ? C71 C70 H70A 108.5 . . ? C69 C70 H70A 108.5 . . ? C71 C70 H70B 108.5 . . ? C69 C70 H70B 108.5 . . ? H70A C70 H70B 107.5 . . ? C70 C71 H71A 109.5 . . ? C70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C70 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? N16 C72 C73 116.7(3) . . ? N16 C72 H72A 108.1 . . ? C73 C72 H72A 108.1 . . ? N16 C72 H72B 108.1 . . ? C73 C72 H72B 108.1 . . ? H72A C72 H72B 107.3 . . ? C72 C73 C74 109.5(3) . . ? C72 C73 H73A 109.8 . . ? C74 C73 H73A 109.8 . . ? C72 C73 H73B 109.8 . . ? C74 C73 H73B 109.8 . . ? H73A C73 H73B 108.2 . . ? C75 C74 C73 114.6(3) . . ? C75 C74 H74A 108.6 . . ? C73 C74 H74A 108.6 . . ? C75 C74 H74B 108.6 . . ? C73 C74 H74B 108.6 . . ? H74A C74 H74B 107.6 . . ? C74 C75 H75A 109.5 . . ? C74 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C74 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C77 C76 N16 116.4(2) . . ? C77 C76 H76A 108.2 . . ? N16 C76 H76A 108.2 . . ? C77 C76 H76B 108.2 . . ? N16 C76 H76B 108.2 . . ? H76A C76 H76B 107.3 . . ? C76 C77 C78 108.4(3) . . ? C76 C77 H77A 110.0 . . ? C78 C77 H77A 110.0 . . ? C76 C77 H77B 110.0 . . ? C78 C77 H77B 110.0 . . ? H77A C77 H77B 108.4 . . ? C79 C78 C77 111.4(3) . . ? C79 C78 H78A 109.4 . . ? C77 C78 H78A 109.4 . . ? C79 C78 H78B 109.4 . . ? C77 C78 H78B 109.4 . . ? H78A C78 H78B 108.0 . . ? C78 C79 H79A 109.5 . . ? C78 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C78 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C81 C80 N16 116.0(2) . . ? C81 C80 H80A 108.3 . . ? N16 C80 H80A 108.3 . . ? C81 C80 H80B 108.3 . . ? N16 C80 H80B 108.3 . . ? H80A C80 H80B 107.4 . . ? C80 C81 C82 109.5(3) . . ? C80 C81 H81A 109.8 . . ? C82 C81 H81A 109.8 . . ? C80 C81 H81B 109.8 . . ? C82 C81 H81B 109.8 . . ? H81A C81 H81B 108.2 . . ? C83 C82 C81 112.1(3) . . ? C83 C82 H82A 109.2 . . ? C81 C82 H82A 109.2 . . ? C83 C82 H82B 109.2 . . ? C81 C82 H82B 109.2 . . ? H82A C82 H82B 107.9 . . ? C82 C83 H83A 109.5 . . ? C82 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C82 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C85 C84 N16 116.0(3) . . ? C85 C84 H84A 108.3 . . ? N16 C84 H84A 108.3 . . ? C85 C84 H84B 108.3 . . ? N16 C84 H84B 108.3 . . ? H84A C84 H84B 107.4 . . ? C84 C85 C86 109.6(3) . . ? C84 C85 H85A 109.8 . . ? C86 C85 H85A 109.8 . . ? C84 C85 H85B 109.8 . . ? C86 C85 H85B 109.8 . . ? H85A C85 H85B 108.2 . . ? C87 C86 C85 113.2(4) . . ? C87 C86 H86A 108.9 . . ? C85 C86 H86A 108.9 . . ? C87 C86 H86B 108.9 . . ? C85 C86 H86B 108.9 . . ? H86A C86 H86B 107.7 . . ? C86 C87 H87A 109.5 . . ? C86 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C86 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C19 N1 C1 109.8(3) . . ? C19 N1 C10 112.7(3) . . ? C1 N1 C10 111.5(3) . . ? C3 N2 C2 120.6(3) . . ? C3 N2 H2 119.7 . . ? C2 N2 H2 119.7 . . ? C3 N3 C4 122.0(3) . . ? C3 N3 H3 119.0 . . ? C4 N3 H3 119.0 . . ? C12 N4 C11 120.6(3) . . ? C12 N4 H4 119.7 . . ? C11 N4 H4 119.7 . . ? C12 N5 C13 121.4(3) . . ? C12 N5 H5 119.3 . . ? C13 N5 H5 119.3 . . ? C21 N6 C20 120.9(3) . . ? C21 N6 H6 119.5 . . ? C20 N6 H6 119.5 . . ? C21 N7 C22 123.3(3) . . ? C21 N7 H7 118.3 . . ? C22 N7 H7 118.3 . . ? C37 N8 C28 113.3(3) . . ? C37 N8 C46 110.6(3) . . ? C28 N8 C46 111.0(2) . . ? C30 N9 C29 119.8(3) . . ? C30 N9 H9 120.1 . . ? C29 N9 H9 120.1 . . ? C30 N10 C31 120.5(3) . . ? C30 N10 H10 119.8 . . ? C31 N10 H10 119.8 . . ? C39 N11 C38 121.9(3) . . ? C39 N11 H11 119.0 . . ? C38 N11 H11 119.0 . . ? C39 N12 C40 123.6(3) . . ? C39 N12 H12 118.2 . . ? C40 N12 H12 118.2 . . ? C48 N13 C47 120.8(3) . . ? C48 N13 H13 119.6 . . ? C47 N13 H13 119.6 . . ? C48 N14 C49 121.2(3) . . ? C48 N14 H14 119.4 . . ? C49 N14 H14 119.4 . . ? C60 N15 C68 105.4(2) . . ? C60 N15 C56 112.1(2) . . ? C68 N15 C56 111.2(2) . . ? C60 N15 C64 111.5(2) . . ? C68 N15 C64 111.7(2) . . ? C56 N15 C64 105.1(2) . . ? C72 N16 C80 112.4(2) . . ? C72 N16 C84 111.7(2) . . ? C80 N16 C84 105.0(2) . . ? C72 N16 C76 104.6(2) . . ? C80 N16 C76 111.8(2) . . ? C84 N16 C76 111.4(2) . . ? O7 O7 C55 0(10) 1 . ? O8 O8 C55 0(10) 1 . ? O9 O9 C55 0(10) 1 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 O7 0.86 2.19 2.962(3) 148.9 1 N3 H3 O8 0.86 2.11 2.928(3) 159.0 1 N4 H4 O7 0.86 2.31 3.136(3) 161.9 1 N5 H5 O9 0.86 1.84 2.700(4) 175.1 1 N6 H6 O7 0.86 2.29 3.069(3) 151.3 1 N7 H7 O7 0.86 2.29 3.003(3) 141.0 1 N7 H7 O9 0.86 2.54 3.344(4) 155.8 1 N9 H9 O8 0.86 2.38 3.201(3) 160.6 1 N10 H10 O9 0.86 1.89 2.748(3) 175.2 1 N11 H11 O8 0.86 2.32 3.089(3) 148.3 1 N12 H12 O8 0.86 2.27 2.987(3) 140.6 1 N12 H12 O9 0.86 2.44 3.249(4) 156.8 1 N13 H13 O8 0.86 2.15 2.915(3) 148.4 1 N14 H14 O7 0.86 2.13 2.938(3) 157.1 1 _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.461 _refine_diff_density_min -0.292 _refine_diff_density_rms 0.046