data_global _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Satu-Marjaana Ikonen' _publ_contact_author_name 'Satu-Marjaana Ikonen' _publ_contact_author_email satu.ikonen@jyu.fi _publ_section_title ; Supramolecular architectures formed by co-crystallization of bile acids and melamine ; # Attachment '- structures 1_2_3' data_1 _database_code_depnum_ccdc_archive 'CCDC 773834' #TrackingRef '- structures 1_2_3' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; Co-crystal of lithocholic acid and lithocholic acid-melamine salt ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H86 N6 O6' _chemical_formula_weight 879.26 _chemical_absolute_configuration syn 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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 20.3640(5) _cell_length_b 7.7890(2) _cell_length_c 31.1030(7) _cell_angle_alpha 90.00 _cell_angle_beta 91.8689(14) _cell_angle_gamma 90.00 _cell_volume 4930.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 10231 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 28.283 _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.184 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9817 _exptl_absorpt_correction_T_max 0.9954 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 Kappa APEX-II' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36922 _diffrn_reflns_av_R_equivalents 0.1126 _diffrn_reflns_av_sigmaI/netI 0.1523 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.00 _diffrn_reflns_theta_max 27.50 _reflns_number_total 12138 _reflns_number_gt 6603 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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^)+(0.0595P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 12138 _refine_ls_number_parameters 1195 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1566 _refine_ls_R_factor_gt 0.0790 _refine_ls_wR_factor_ref 0.1708 _refine_ls_wR_factor_gt 0.1419 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1A C 0.4042(2) 0.3561(7) 0.35361(15) 0.0257(13) Uani 1 1 d . . . H1A1 H 0.4154 0.2472 0.3685 0.031 Uiso 1 1 calc R . . H1A2 H 0.4324 0.3654 0.3284 0.031 Uiso 1 1 calc R . . C1B C 0.0945(2) 0.7497(7) 0.64536(15) 0.0260(13) Uani 1 1 d . . . H1B1 H 0.0867 0.6505 0.6260 0.031 Uiso 1 1 calc R . . H1B2 H 0.0662 0.7350 0.6704 0.031 Uiso 1 1 calc R . . C1C C 0.1235(3) 0.2378(7) 1.14802(15) 0.0304(14) Uani 1 1 d . . . H1C1 H 0.0957 0.2021 1.1720 0.037 Uiso 1 1 calc R . . H1C2 H 0.1293 0.1367 1.1292 0.037 Uiso 1 1 calc R . . C1D C 0.3980(3) -0.1357(7) 0.83947(16) 0.0317(14) Uani 1 1 d . . . H1D1 H 0.4292 -0.1439 0.8158 0.038 Uiso 1 1 calc R . . H1D2 H 0.3974 -0.2488 0.8540 0.038 Uiso 1 1 calc R . . C2A C 0.3317(2) 0.3490(7) 0.33772(15) 0.0256(13) Uani 1 1 d . . . H2A1 H 0.3251 0.2504 0.3180 0.031 Uiso 1 1 calc R . . H2A2 H 0.3031 0.3323 0.3625 0.031 Uiso 1 1 calc R . . C2B C 0.1662(2) 0.7480(7) 0.66116(15) 0.0234(12) Uani 1 1 d . . . H2B1 H 0.1758 0.6392 0.6766 0.028 Uiso 1 1 calc R . . H2B2 H 0.1951 0.7544 0.6362 0.028 Uiso 1 1 calc R . . C2C C 0.1904(3) 0.2915(7) 1.16654(15) 0.0282(13) Uani 1 1 d . . . H2C1 H 0.2099 0.1951 1.1833 0.034 Uiso 1 1 calc R . . H2C2 H 0.2199 0.3175 1.1427 0.034 Uiso 1 1 calc R . . C2D C 0.3302(3) -0.1000(7) 0.82031(16) 0.0312(14) Uani 1 1 d . . . H2D1 H 0.2976 -0.1082 0.8432 0.037 Uiso 1 1 calc R . . H2D2 H 0.3191 -0.1882 0.7983 0.037 Uiso 1 1 calc R . . C3A C 0.3131(2) 0.5122(7) 0.31483(15) 0.0264(13) Uani 1 1 d . . . H3A H 0.3398 0.5211 0.2885 0.032 Uiso 1 1 calc R . . C3B C 0.1802(3) 0.8978(7) 0.69085(16) 0.0268(13) Uani 1 1 d . . . H3B H 0.1537 0.8827 0.7171 0.032 Uiso 1 1 calc R . . C3C C 0.1856(3) 0.4459(7) 1.19493(16) 0.0286(14) Uani 1 1 d . . . H3C H 0.1584 0.4158 1.2200 0.034 Uiso 1 1 calc R . . C3D C 0.3260(3) 0.0761(7) 0.79988(15) 0.0283(13) Uani 1 1 d . . . H3D H 0.3563 0.0803 0.7752 0.034 Uiso 1 1 calc R . . C4A C 0.3272(2) 0.6697(7) 0.34262(15) 0.0255(13) Uani 1 1 d . . . H4A1 H 0.2971 0.6701 0.3670 0.031 Uiso 1 1 calc R . . H4A2 H 0.3184 0.7744 0.3253 0.031 Uiso 1 1 calc R . . C4B C 0.1606(3) 1.0668(7) 0.66979(16) 0.0274(13) Uani 1 1 d . . . H4B1 H 0.1901 1.0902 0.6458 0.033 Uiso 1 1 calc R . . H4B2 H 0.1663 1.1605 0.6911 0.033 Uiso 1 1 calc R . . C4C C 0.1521(2) 0.5907(7) 1.17003(16) 0.0289(14) Uani 1 1 d . . . H4C1 H 0.1809 0.6278 1.1467 0.035 Uiso 1 1 calc R . . H4C2 H 0.1466 0.6896 1.1896 0.035 Uiso 1 1 calc R . . C4D C 0.3463(2) 0.2119(7) 0.83206(15) 0.0267(13) Uani 1 1 d . . . H4D1 H 0.3149 0.2131 0.8557 0.032 Uiso 1 1 calc R . . H4D2 H 0.3447 0.3258 0.8179 0.032 Uiso 1 1 calc R . . C5A C 0.3989(2) 0.6745(7) 0.36039(15) 0.0240(13) Uani 1 1 d . . . H5A H 0.4277 0.6861 0.3351 0.029 Uiso 1 1 calc R . . C5B C 0.0886(2) 1.0666(7) 0.65221(15) 0.0237(13) Uani 1 1 d . . . H5B H 0.0595 1.0545 0.6773 0.028 Uiso 1 1 calc R . . C5C C 0.0847(2) 0.5412(8) 1.15032(16) 0.0300(14) Uani 1 1 d . . . H5C H 0.0559 0.5134 1.1748 0.036 Uiso 1 1 calc R . . C5D C 0.4159(3) 0.1803(7) 0.85086(15) 0.0267(13) Uani 1 1 d . . . H5D H 0.4462 0.1840 0.8263 0.032 Uiso 1 1 calc R . . C6A C 0.4105(3) 0.8337(7) 0.38830(16) 0.0305(14) Uani 1 1 d . . . H6A1 H 0.4584 0.8502 0.3934 0.037 Uiso 1 1 calc R . . H6A2 H 0.3932 0.9359 0.3728 0.037 Uiso 1 1 calc R . . C6B C 0.0725(3) 1.2400(7) 0.63051(15) 0.0287(13) Uani 1 1 d . . . H6B1 H 0.0242 1.2501 0.6262 0.034 Uiso 1 1 calc R . . H6B2 H 0.0873 1.3340 0.6499 0.034 Uiso 1 1 calc R . . C6C C 0.0529(2) 0.6939(8) 1.12632(15) 0.0314(14) Uani 1 1 d . . . H6C1 H 0.0062 0.6676 1.1195 0.038 Uiso 1 1 calc R . . H6C2 H 0.0546 0.7964 1.1452 0.038 Uiso 1 1 calc R . . C6D C 0.4370(3) 0.3242(8) 0.88167(15) 0.0346(15) Uani 1 1 d . . . H6D1 H 0.4848 0.3150 0.8881 0.042 Uiso 1 1 calc R . . H6D2 H 0.4287 0.4365 0.8676 0.042 Uiso 1 1 calc R . . C7A C 0.3774(3) 0.8182(7) 0.43136(15) 0.0263(13) Uani 1 1 d . . . H7A1 H 0.3292 0.8221 0.4263 0.032 Uiso 1 1 calc R . . H7A2 H 0.3900 0.9182 0.4495 0.032 Uiso 1 1 calc R . . C7B C 0.1048(3) 1.2621(7) 0.58689(15) 0.0262(13) Uani 1 1 d . . . H7B1 H 0.0878 1.3682 0.5730 0.031 Uiso 1 1 calc R . . H7B2 H 0.1528 1.2763 0.5919 0.031 Uiso 1 1 calc R . . C7C C 0.0879(3) 0.7336(7) 1.08463(15) 0.0287(13) Uani 1 1 d . . . H7C1 H 0.0641 0.8267 1.0690 0.034 Uiso 1 1 calc R . . H7C2 H 0.1329 0.7749 1.0918 0.034 Uiso 1 1 calc R . . C7D C 0.4003(3) 0.3169(7) 0.92358(15) 0.0276(13) Uani 1 1 d . . . H7D1 H 0.4180 0.4065 0.9433 0.033 Uiso 1 1 calc R . . H7D2 H 0.3533 0.3427 0.9175 0.033 Uiso 1 1 calc R . . C8A C 0.3951(3) 0.6541(7) 0.45581(15) 0.0245(13) Uani 1 1 d . . . H8A H 0.4428 0.6576 0.4646 0.029 Uiso 1 1 calc R . . C8B C 0.0926(3) 1.1116(7) 0.55642(15) 0.0243(13) Uani 1 1 d . . . H8B H 0.0450 1.1092 0.5475 0.029 Uiso 1 1 calc R . . C8C C 0.0917(3) 0.5775(7) 1.05554(15) 0.0251(13) Uani 1 1 d . . . H8C H 0.0459 0.5472 1.0458 0.030 Uiso 1 1 calc R . . C8D C 0.4059(3) 0.1442(7) 0.94557(14) 0.0233(12) Uani 1 1 d . . . H8D H 0.4529 0.1271 0.9549 0.028 Uiso 1 1 calc R . . C9A C 0.3823(3) 0.4959(7) 0.42725(14) 0.0233(12) Uani 1 1 d . . . H9A H 0.3343 0.4975 0.4192 0.028 Uiso 1 1 calc R . . C9B C 0.1109(3) 0.9392(6) 0.57895(15) 0.0212(12) Uani 1 1 d . . . H9B H 0.1586 0.9476 0.5873 0.025 Uiso 1 1 calc R . . C9C C 0.1216(3) 0.4188(7) 1.07923(16) 0.0278(13) Uani 1 1 d . . . H9C H 0.1678 0.4512 1.0876 0.033 Uiso 1 1 calc R . . C9D C 0.3861(2) -0.0043(7) 0.91469(14) 0.0226(12) Uani 1 1 d . . . H9D H 0.3388 0.0146 0.9063 0.027 Uiso 1 1 calc R . . C10A C 0.4198(2) 0.5055(7) 0.38408(15) 0.0232(12) Uani 1 1 d . . . C10B C 0.0741(2) 0.9134(7) 0.62156(14) 0.0201(12) Uani 1 1 d . . . C10D C 0.0871(3) 0.3788(8) 1.12192(15) 0.0292(14) Uani 1 1 d . . . C10E C 0.4243(3) 0.0004(7) 0.87225(15) 0.0272(13) Uani 1 1 d . . . C11A C 0.3948(3) 0.3280(7) 0.45207(15) 0.0295(14) Uani 1 1 d . . . H111 H 0.3814 0.2301 0.4334 0.035 Uiso 1 1 calc R . . H112 H 0.4425 0.3170 0.4587 0.035 Uiso 1 1 calc R . . C11B C 0.1044(2) 0.7879(7) 0.54719(14) 0.0238(12) Uani 1 1 d . . . H113 H 0.1204 0.6822 0.5618 0.029 Uiso 1 1 calc R . . H114 H 0.0574 0.7710 0.5393 0.029 Uiso 1 1 calc R . . C11C C 0.1268(3) 0.2669(7) 1.04897(15) 0.0284(13) Uani 1 1 d . . . H115 H 0.0820 0.2255 1.0412 0.034 Uiso 1 1 calc R . . H116 H 0.1504 0.1726 1.0642 0.034 Uiso 1 1 calc R . . C11D C 0.3895(3) -0.1782(7) 0.93776(15) 0.0274(13) Uani 1 1 d . . . H117 H 0.4361 -0.2063 0.9446 0.033 Uiso 1 1 calc R . . H118 H 0.3717 -0.2679 0.9181 0.033 Uiso 1 1 calc R . . C12A C 0.3580(3) 0.3171(7) 0.49396(14) 0.0289(14) Uani 1 1 d . . . H121 H 0.3717 0.2118 0.5096 0.035 Uiso 1 1 calc R . . H122 H 0.3103 0.3081 0.4872 0.035 Uiso 1 1 calc R . . C12B C 0.1424(2) 0.8125(6) 0.50617(14) 0.0227(12) Uani 1 1 d . . . H123 H 0.1333 0.7148 0.4865 0.027 Uiso 1 1 calc R . . H124 H 0.1901 0.8132 0.5134 0.027 Uiso 1 1 calc R . . C12C C 0.1630(2) 0.3097(7) 1.00723(14) 0.0254(13) Uani 1 1 d . . . H125 H 0.2096 0.3356 1.0146 0.031 Uiso 1 1 calc R . . H126 H 0.1618 0.2080 0.9881 0.031 Uiso 1 1 calc R . . C12D C 0.3510(3) -0.1820(7) 0.97973(15) 0.0292(14) Uani 1 1 d . . . H127 H 0.3035 -0.1716 0.9726 0.035 Uiso 1 1 calc R . . H128 H 0.3585 -0.2937 0.9942 0.035 Uiso 1 1 calc R . . C13A C 0.3706(2) 0.4737(7) 0.52313(15) 0.0220(12) Uani 1 1 d . . . C13B C 0.1234(2) 0.9811(7) 0.48322(14) 0.0204(12) Uani 1 1 d . . . C13D C 0.1325(2) 0.4621(7) 0.98321(15) 0.0229(13) Uani 1 1 d . . . C13E C 0.3718(2) -0.0372(7) 1.01043(15) 0.0212(12) Uani 1 1 d . . . C14A C 0.3547(3) 0.6346(7) 0.49593(15) 0.0254(13) Uani 1 1 d . . . H14A H 0.3079 0.6220 0.4855 0.031 Uiso 1 1 calc R . . C14B C 0.1332(2) 1.1274(6) 0.51639(14) 0.0212(12) Uani 1 1 d . . . H14B H 0.1802 1.1200 0.5267 0.025 Uiso 1 1 calc R . . C14C C 0.1310(2) 0.6119(7) 1.01556(14) 0.0224(12) Uani 1 1 d . . . H14C H 0.1775 0.6284 1.0261 0.027 Uiso 1 1 calc R . . C14D C 0.3647(2) 0.1351(7) 0.98527(14) 0.0213(12) Uani 1 1 d . . . H14D H 0.3179 0.1397 0.9745 0.026 Uiso 1 1 calc R . . C15A C 0.3556(3) 0.7809(7) 0.52836(15) 0.0297(14) Uani 1 1 d . . . H151 H 0.3272 0.8769 0.5182 0.036 Uiso 1 1 calc R . . H152 H 0.4008 0.8244 0.5338 0.036 Uiso 1 1 calc R . . C15B C 0.1281(3) 1.2905(7) 0.48943(15) 0.0278(13) Uani 1 1 d . . . H153 H 0.1520 1.3864 0.5038 0.033 Uiso 1 1 calc R . . H154 H 0.0816 1.3243 0.4844 0.033 Uiso 1 1 calc R . . C15C C 0.1145(3) 0.7682(7) 0.98766(15) 0.0299(14) Uani 1 1 d . . . H155 H 0.1296 0.8755 1.0019 0.036 Uiso 1 1 calc R . . H156 H 0.0666 0.7761 0.9814 0.036 Uiso 1 1 calc R . . C15D C 0.3712(3) 0.2728(7) 1.01970(15) 0.0267(13) Uani 1 1 d . . . H157 H 0.3478 0.3789 1.0106 0.032 Uiso 1 1 calc R . . H158 H 0.4179 0.3006 1.0261 0.032 Uiso 1 1 calc R . . C16A C 0.3286(3) 0.6974(7) 0.56903(15) 0.0277(13) Uani 1 1 d . . . H161 H 0.2847 0.7447 0.5750 0.033 Uiso 1 1 calc R . . H162 H 0.3583 0.7204 0.5942 0.033 Uiso 1 1 calc R . . C16B C 0.1598(3) 1.2424(7) 0.44706(15) 0.0268(13) Uani 1 1 d . . . H163 H 0.2028 1.3008 0.4448 0.032 Uiso 1 1 calc R . . H164 H 0.1311 1.2772 0.4223 0.032 Uiso 1 1 calc R . . C16C C 0.1523(3) 0.7344(7) 0.94622(15) 0.0275(13) Uani 1 1 d . . . H165 H 0.1907 0.8120 0.9448 0.033 Uiso 1 1 calc R . . H166 H 0.1234 0.7542 0.9205 0.033 Uiso 1 1 calc R . . C16D C 0.3392(3) 0.1922(7) 1.05907(15) 0.0272(13) Uani 1 1 d . . . H167 H 0.2975 0.2513 1.0650 0.033 Uiso 1 1 calc R . . H168 H 0.3690 0.2024 1.0848 0.033 Uiso 1 1 calc R . . C17A C 0.3238(3) 0.5014(7) 0.56055(15) 0.0263(13) Uani 1 1 d . . . H17A H 0.2783 0.4790 0.5487 0.032 Uiso 1 1 calc R . . C17B C 0.1694(3) 1.0420(7) 0.44741(15) 0.0234(13) Uani 1 1 d . . . H17B H 0.2155 1.0190 0.4578 0.028 Uiso 1 1 calc R . . C17C C 0.1753(2) 0.5432(7) 0.94804(15) 0.0249(13) Uani 1 1 d . . . H17C H 0.2218 0.5426 0.9594 0.030 Uiso 1 1 calc R . . C17D C 0.3261(2) -0.0009(7) 1.04832(15) 0.0225(12) Uani 1 1 d . . . H17D H 0.2799 -0.0092 1.0366 0.027 Uiso 1 1 calc R . . C18A C 0.4427(2) 0.4714(7) 0.54035(15) 0.0281(13) Uani 1 1 d . . . H181 H 0.4506 0.3671 0.5574 0.042 Uiso 1 1 calc R . . H182 H 0.4510 0.5725 0.5585 0.042 Uiso 1 1 calc R . . H183 H 0.4723 0.4732 0.5161 0.042 Uiso 1 1 calc R . . C18B C 0.0513(2) 0.9723(7) 0.46538(15) 0.0267(13) Uani 1 1 d . . . H184 H 0.0400 1.0799 0.4506 0.040 Uiso 1 1 calc R . . H185 H 0.0217 0.9549 0.4892 0.040 Uiso 1 1 calc R . . H186 H 0.0467 0.8764 0.4451 0.040 Uiso 1 1 calc R . . C18C C 0.0638(2) 0.4185(7) 0.96476(15) 0.0277(13) Uani 1 1 d . . . H187 H 0.0451 0.5192 0.9499 0.042 Uiso 1 1 calc R . . H188 H 0.0354 0.3852 0.9882 0.042 Uiso 1 1 calc R . . H189 H 0.0668 0.3232 0.9443 0.042 Uiso 1 1 calc R . . C18D C 0.4432(2) -0.0631(7) 1.02804(16) 0.0310(14) Uani 1 1 d . . . H18A H 0.4463 -0.1723 1.0437 0.047 Uiso 1 1 calc R . . H18B H 0.4552 0.0314 1.0476 0.047 Uiso 1 1 calc R . . H18C H 0.4732 -0.0649 1.0040 0.047 Uiso 1 1 calc R . . C19A C 0.4947(2) 0.5028(8) 0.39236(16) 0.0330(14) Uani 1 1 d . . . H19A H 0.5075 0.5977 0.4116 0.049 Uiso 1 1 calc R . . H19B H 0.5168 0.5154 0.3650 0.049 Uiso 1 1 calc R . . H19C H 0.5076 0.3935 0.4058 0.049 Uiso 1 1 calc R . . C19B C -0.0011(2) 0.9005(8) 0.61264(16) 0.0309(14) Uani 1 1 d . . . H191 H -0.0166 1.0036 0.5973 0.046 Uiso 1 1 calc R . . H192 H -0.0234 0.8910 0.6400 0.046 Uiso 1 1 calc R . . H193 H -0.0109 0.7989 0.5950 0.046 Uiso 1 1 calc R . . C19C C 0.0167(3) 0.3127(9) 1.11323(16) 0.0423(17) Uani 1 1 d . . . H194 H 0.0179 0.2098 1.0951 0.063 Uiso 1 1 calc R . . H195 H -0.0094 0.4018 1.0984 0.063 Uiso 1 1 calc R . . H196 H -0.0033 0.2843 1.1406 0.063 Uiso 1 1 calc R . . C19D C 0.4974(2) -0.0377(8) 0.88091(16) 0.0343(15) Uani 1 1 d . . . H197 H 0.5205 -0.0341 0.8538 0.051 Uiso 1 1 calc R . . H198 H 0.5023 -0.1520 0.8938 0.051 Uiso 1 1 calc R . . H199 H 0.5161 0.0485 0.9007 0.051 Uiso 1 1 calc R . . C20A C 0.3322(3) 0.3922(7) 0.60173(15) 0.0232(13) Uani 1 1 d . . . H20A H 0.3761 0.4188 0.6155 0.028 Uiso 1 1 calc R . . C20B C 0.1616(2) 0.9648(7) 0.40196(15) 0.0224(12) Uani 1 1 d . . . H20B H 0.1177 0.9999 0.3896 0.027 Uiso 1 1 calc R . . C20C C 0.1750(3) 0.4615(7) 0.90288(15) 0.0256(13) Uani 1 1 d . . . H20C H 0.1308 0.4811 0.8887 0.031 Uiso 1 1 calc R . . C20D C 0.3306(3) -0.1144(7) 1.08904(15) 0.0271(14) Uani 1 1 d . . . H20D H 0.3742 -0.0922 1.1038 0.032 Uiso 1 1 calc R . . C21A C 0.3284(3) 0.1988(7) 0.59352(16) 0.0318(14) Uani 1 1 d . . . H21A H 0.3352 0.1372 0.6208 0.048 Uiso 1 1 calc R . . H21B H 0.3626 0.1655 0.5737 0.048 Uiso 1 1 calc R . . H21C H 0.2851 0.1698 0.5809 0.048 Uiso 1 1 calc R . . C21B C 0.1648(3) 0.7676(7) 0.40201(16) 0.0338(14) Uani 1 1 d . . . H211 H 0.1298 0.7217 0.4196 0.051 Uiso 1 1 calc R . . H212 H 0.2076 0.7304 0.4140 0.051 Uiso 1 1 calc R . . H213 H 0.1592 0.7251 0.3725 0.051 Uiso 1 1 calc R . . C21C C 0.1888(3) 0.2675(7) 0.90319(15) 0.0312(14) Uani 1 1 d . . . H214 H 0.1871 0.2239 0.8736 0.047 Uiso 1 1 calc R . . H215 H 0.1556 0.2087 0.9199 0.047 Uiso 1 1 calc R . . H216 H 0.2325 0.2461 0.9162 0.047 Uiso 1 1 calc R . . C21D C 0.3258(3) -0.3074(7) 1.07992(16) 0.0356(15) Uani 1 1 d . . . H217 H 0.3603 -0.3409 1.0603 0.053 Uiso 1 1 calc R . . H218 H 0.2826 -0.3336 1.0667 0.053 Uiso 1 1 calc R . . H219 H 0.3314 -0.3711 1.1070 0.053 Uiso 1 1 calc R . . C22A C 0.2784(2) 0.4471(7) 0.63286(14) 0.0261(13) Uani 1 1 d . . . H221 H 0.2769 0.5741 0.6337 0.031 Uiso 1 1 calc R . . H222 H 0.2354 0.4068 0.6210 0.031 Uiso 1 1 calc R . . C22B C 0.2144(2) 1.0405(7) 0.37378(14) 0.0255(13) Uani 1 1 d . . . H223 H 0.2576 0.9952 0.3839 0.031 Uiso 1 1 calc R . . H224 H 0.2153 1.1664 0.3780 0.031 Uiso 1 1 calc R . . C22C C 0.2271(2) 0.5542(7) 0.87616(14) 0.0254(13) Uani 1 1 d . . . H225 H 0.2236 0.6794 0.8812 0.031 Uiso 1 1 calc R . . H226 H 0.2713 0.5174 0.8866 0.031 Uiso 1 1 calc R . . C22D C 0.2767(3) -0.0596(7) 1.11988(15) 0.0304(14) Uani 1 1 d . . . H227 H 0.2741 0.0673 1.1200 0.036 Uiso 1 1 calc R . . H228 H 0.2340 -0.1038 1.1086 0.036 Uiso 1 1 calc R . . C23A C 0.2870(2) 0.3808(7) 0.67911(14) 0.0233(12) Uani 1 1 d . . . H231 H 0.2469 0.4062 0.6951 0.028 Uiso 1 1 calc R . . H232 H 0.2931 0.2547 0.6787 0.028 Uiso 1 1 calc R . . C23B C 0.2062(2) 1.0043(7) 0.32543(14) 0.0237(12) Uani 1 1 d . . . H233 H 0.2473 1.0359 0.3112 0.028 Uiso 1 1 calc R . . H234 H 0.1991 0.8797 0.3211 0.028 Uiso 1 1 calc R . . C23C C 0.2205(2) 0.5200(7) 0.82774(14) 0.0250(13) Uani 1 1 d . . . H235 H 0.2606 0.5624 0.8140 0.030 Uiso 1 1 calc R . . H236 H 0.2182 0.3944 0.8231 0.030 Uiso 1 1 calc R . . C23D C 0.2875(2) -0.1221(7) 1.16612(15) 0.0262(13) Uani 1 1 d . . . H237 H 0.2470 -0.0996 1.1820 0.031 Uiso 1 1 calc R . . H238 H 0.2942 -0.2480 1.1656 0.031 Uiso 1 1 calc R . . C24A C 0.3449(3) 0.4629(7) 0.70135(15) 0.0249(13) Uani 1 1 d . . . C24B C 0.1497(3) 1.1016(8) 0.30449(15) 0.0262(13) Uani 1 1 d . . . C24C C 0.1622(3) 0.6008(7) 0.80581(16) 0.0264(13) Uani 1 1 d . . . C24D C 0.3435(3) -0.0430(8) 1.19010(18) 0.0316(14) Uani 1 1 d . . . C1F C 0.5043(3) -0.3165(7) 0.75069(15) 0.0264(13) Uani 1 1 d . . . C2F C 0.5538(3) -0.0617(7) 0.76482(15) 0.0233(13) Uani 1 1 d . . . C3F C 0.4571(3) -0.0597(7) 0.72736(15) 0.0237(13) Uani 1 1 d . . . N1F N 0.4532(2) -0.2334(6) 0.73027(13) 0.0240(10) Uani 1 1 d . . . N2F N 0.5008(3) -0.4860(7) 0.75236(18) 0.0495(16) Uani 1 1 d D . . H2FA H 0.467(2) -0.547(7) 0.7441(18) 0.059 Uiso 1 1 d D . . H2FB H 0.5376(19) -0.532(7) 0.7637(18) 0.059 Uiso 1 1 d D . . N3F N 0.5560(2) -0.2342(6) 0.76809(13) 0.0272(11) Uani 1 1 d . . . N4F N 0.6039(2) 0.0214(6) 0.78345(14) 0.0280(11) Uani 1 1 d D . . H4FA H 0.607(3) 0.134(3) 0.7848(17) 0.034 Uiso 1 1 d D . . H4FB H 0.6376(19) -0.032(6) 0.7953(15) 0.034 Uiso 1 1 d D . . N5F N 0.5065(2) 0.0319(6) 0.74486(12) 0.0240(10) Uani 1 1 d . . . N6F N 0.4080(2) 0.0192(6) 0.70573(14) 0.0245(10) Uani 1 1 d D . . H6FA H 0.407(3) 0.132(3) 0.7068(16) 0.029 Uiso 1 1 d D . . H6FB H 0.3735(17) -0.041(6) 0.6991(15) 0.029 Uiso 1 1 d D . . C1E C 0.0042(3) -0.1766(7) 0.75341(15) 0.0229(12) Uani 1 1 d . . . C2E C 0.0541(3) 0.0830(7) 0.76746(15) 0.0219(12) Uani 1 1 d . . . C3E C -0.0455(3) 0.0867(7) 0.73434(15) 0.0223(12) Uani 1 1 d . . . N1E N -0.0466(2) -0.0881(6) 0.73418(13) 0.0216(10) Uani 1 1 d . . . N2E N 0.0024(2) -0.3425(6) 0.75376(14) 0.0279(11) Uani 1 1 d D . . H2EA H 0.0376(17) -0.400(6) 0.7629(15) 0.033 Uiso 1 1 d D . . H2EB H -0.0308(19) -0.389(6) 0.7397(14) 0.033 Uiso 1 1 d D . . N3E N 0.0555(2) -0.0905(6) 0.77111(12) 0.0214(10) Uani 1 1 d . . . N4E N 0.1076(2) 0.1643(6) 0.78230(15) 0.0270(11) Uani 1 1 d D . . H4EA H 0.1443(16) 0.112(6) 0.7906(15) 0.032 Uiso 1 1 d D . . H4EB H 0.111(3) 0.276(3) 0.7812(16) 0.032 Uiso 1 1 d D . . N5E N 0.0048(2) 0.1765(6) 0.75082(12) 0.0259(11) Uani 1 1 d . . . N6E N -0.0976(2) 0.1640(6) 0.71674(15) 0.0292(11) Uani 1 1 d D . . H6EA H -0.1324(18) 0.105(6) 0.7087(16) 0.035 Uiso 1 1 d D . . H6EB H -0.098(3) 0.275(3) 0.7149(16) 0.035 Uiso 1 1 d D . . O3A O 0.24394(18) 0.5159(5) 0.30148(11) 0.0301(9) Uani 1 1 d D . . O3B O 0.24870(18) 0.9094(5) 0.70418(12) 0.0296(9) Uani 1 1 d D . . O3C O 0.24984(17) 0.4965(6) 1.21063(10) 0.0301(9) Uani 1 1 d D . . O3D O 0.25961(18) 0.1110(5) 0.78400(11) 0.0350(10) Uani 1 1 d D . . O24A O 0.39408(19) 0.3740(5) 0.71123(12) 0.0376(11) Uani 1 1 d . . . O24B O 0.1045(2) 1.0163(5) 0.28692(15) 0.0542(13) Uani 1 1 d . . . O24C O 0.12731(19) 0.5274(5) 0.77925(12) 0.0422(11) Uani 1 1 d . . . O24D O 0.3787(2) -0.1187(5) 1.21569(14) 0.0552(14) Uani 1 1 d . . . O25A O 0.34163(18) 0.6246(5) 0.70856(11) 0.0301(9) Uani 1 1 d . . . O25B O 0.15058(17) 1.2627(5) 0.30530(11) 0.0289(9) Uani 1 1 d . . . O25C O 0.15222(19) 0.7611(5) 0.81659(11) 0.0347(10) Uani 1 1 d D . . O25D O 0.3530(2) 0.1221(5) 1.18219(12) 0.0397(11) Uani 1 1 d . . . H25C H 0.1172(18) 0.797(7) 0.8033(16) 0.048 Uiso 1 1 d D . . H25D H 0.387(3) 0.139(8) 1.2006(17) 0.048 Uiso 1 1 d . . . H3OA H 0.227(3) 0.420(4) 0.3005(18) 0.048 Uiso 1 1 d D . . H3OB H 0.270(3) 0.820(5) 0.7072(18) 0.048 Uiso 1 1 d D . . H3OC H 0.251(3) 0.505(8) 1.2374(7) 0.048 Uiso 1 1 d D . . H3OD H 0.255(3) 0.054(6) 0.7617(11) 0.048 Uiso 1 1 d D . . H1NE H -0.079(3) -0.153(8) 0.7185(17) 0.048 Uiso 1 1 d . . . H1NF H 0.410(3) -0.309(7) 0.7209(16) 0.048 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1A 0.022(3) 0.028(3) 0.026(3) -0.002(3) 0.000(2) 0.000(3) C1B 0.030(3) 0.024(3) 0.024(3) 0.007(3) 0.000(2) -0.005(3) C1C 0.032(3) 0.039(4) 0.020(3) -0.002(3) 0.003(2) -0.009(3) C1D 0.042(4) 0.028(3) 0.025(3) -0.002(3) -0.002(3) 0.013(3) C2A 0.028(3) 0.024(3) 0.026(3) -0.007(3) 0.001(2) -0.007(3) C2B 0.025(3) 0.021(3) 0.024(3) -0.003(3) 0.001(2) 0.001(2) C2C 0.032(3) 0.029(3) 0.023(3) 0.003(3) -0.003(2) 0.002(3) C2D 0.034(4) 0.032(3) 0.028(3) -0.006(3) 0.000(3) -0.007(3) C3A 0.019(3) 0.033(3) 0.027(3) 0.005(3) 0.002(2) -0.004(3) C3B 0.023(3) 0.032(3) 0.026(3) -0.007(3) 0.003(2) -0.003(3) C3C 0.020(3) 0.038(4) 0.027(3) 0.000(3) -0.006(2) -0.001(3) C3D 0.022(3) 0.036(4) 0.027(3) -0.002(3) 0.001(2) 0.003(3) C4A 0.029(3) 0.024(3) 0.023(3) -0.003(3) -0.004(2) -0.002(3) C4B 0.028(3) 0.028(3) 0.026(3) 0.001(3) -0.003(2) -0.005(3) C4C 0.023(3) 0.032(3) 0.031(3) -0.002(3) -0.009(2) -0.007(3) C4D 0.022(3) 0.030(3) 0.027(3) 0.001(3) -0.008(2) 0.001(3) C5A 0.017(3) 0.026(3) 0.029(3) 0.006(3) -0.004(2) -0.007(2) C5B 0.023(3) 0.028(3) 0.021(2) 0.000(2) 0.000(2) 0.007(2) C5C 0.015(3) 0.045(4) 0.030(3) -0.003(3) 0.000(2) 0.000(3) C5D 0.026(3) 0.030(3) 0.024(3) -0.002(3) 0.002(2) 0.003(3) C6A 0.032(3) 0.022(3) 0.036(3) 0.007(3) -0.014(3) -0.005(3) C6B 0.029(3) 0.023(3) 0.033(3) -0.009(3) -0.002(2) 0.007(3) C6C 0.014(3) 0.045(4) 0.035(3) -0.012(3) -0.002(2) 0.009(3) C6D 0.031(4) 0.043(4) 0.030(3) 0.005(3) -0.007(3) -0.008(3) C7A 0.031(3) 0.017(3) 0.030(3) 0.003(3) -0.010(2) 0.000(2) C7B 0.031(3) 0.017(3) 0.030(3) -0.003(3) -0.002(2) -0.002(3) C7C 0.021(3) 0.034(3) 0.031(3) -0.004(3) -0.001(2) 0.006(3) C7D 0.030(3) 0.026(3) 0.027(3) -0.007(3) -0.003(2) -0.002(3) C8A 0.024(3) 0.019(3) 0.030(3) -0.004(3) -0.005(2) 0.002(2) C8B 0.023(3) 0.025(3) 0.025(3) 0.003(3) 0.000(2) -0.001(3) C8C 0.023(3) 0.030(3) 0.022(2) -0.003(3) -0.001(2) 0.002(3) C8D 0.024(3) 0.020(3) 0.025(3) -0.004(3) -0.002(2) 0.003(2) C9A 0.025(3) 0.023(3) 0.022(2) 0.003(3) -0.003(2) 0.003(3) C9B 0.025(3) 0.014(3) 0.024(3) -0.007(2) -0.001(2) -0.004(2) C9C 0.021(3) 0.034(3) 0.027(3) -0.004(3) -0.008(2) 0.003(3) C9D 0.020(3) 0.024(3) 0.024(2) 0.003(3) -0.001(2) 0.005(2) C10A 0.020(3) 0.022(3) 0.027(3) -0.001(3) -0.004(2) 0.001(2) C10B 0.016(3) 0.025(3) 0.019(2) -0.002(2) 0.001(2) -0.003(2) C10D 0.028(3) 0.038(4) 0.021(3) 0.004(3) 0.001(2) -0.009(3) C10E 0.021(3) 0.030(3) 0.030(3) -0.004(3) -0.007(2) 0.004(3) C11A 0.045(4) 0.016(3) 0.027(3) -0.004(3) -0.004(3) 0.002(3) C11B 0.026(3) 0.021(3) 0.025(3) -0.002(3) -0.001(2) 0.002(2) C11C 0.036(3) 0.023(3) 0.026(3) 0.003(3) 0.001(2) -0.001(3) C11D 0.036(3) 0.021(3) 0.026(3) -0.003(3) -0.002(2) 0.006(3) C12A 0.042(4) 0.024(3) 0.021(3) 0.005(3) -0.004(2) 0.002(3) C12B 0.027(3) 0.014(3) 0.027(3) 0.003(2) 0.002(2) 0.002(2) C12C 0.025(3) 0.029(3) 0.023(3) -0.003(3) 0.004(2) -0.001(3) C12D 0.036(4) 0.016(3) 0.035(3) -0.006(3) -0.009(3) 0.002(3) C13A 0.022(3) 0.016(3) 0.027(3) 0.000(3) -0.003(2) 0.003(2) C13B 0.017(3) 0.022(3) 0.022(2) 0.000(2) -0.003(2) -0.004(2) C13D 0.020(3) 0.029(3) 0.020(2) 0.009(3) -0.001(2) 0.000(2) C13E 0.014(3) 0.027(3) 0.023(2) 0.001(2) -0.003(2) 0.001(2) C14A 0.022(3) 0.021(3) 0.032(3) 0.001(3) -0.007(2) -0.002(2) C14B 0.018(3) 0.019(3) 0.026(3) 0.008(2) -0.005(2) 0.003(2) C14C 0.019(3) 0.026(3) 0.022(2) 0.006(3) -0.005(2) 0.001(2) C14D 0.016(3) 0.022(3) 0.026(3) 0.003(3) -0.004(2) -0.001(2) C15A 0.035(3) 0.025(3) 0.029(3) -0.004(3) -0.006(2) 0.002(3) C15B 0.033(3) 0.019(3) 0.031(3) 0.007(3) -0.001(2) 0.000(3) C15C 0.031(3) 0.030(3) 0.028(3) 0.001(3) -0.002(2) 0.009(3) C15D 0.028(3) 0.022(3) 0.029(3) -0.002(3) -0.005(2) -0.001(3) C16A 0.034(3) 0.022(3) 0.026(3) 0.000(3) -0.005(2) 0.003(3) C16B 0.020(3) 0.035(3) 0.025(3) 0.008(3) -0.002(2) -0.002(3) C16C 0.021(3) 0.030(3) 0.031(3) 0.002(3) -0.002(2) 0.001(3) C16D 0.025(3) 0.026(3) 0.030(3) -0.003(3) -0.003(2) 0.003(3) C17A 0.023(3) 0.027(3) 0.028(3) -0.003(3) -0.008(2) 0.007(3) C17B 0.024(3) 0.019(3) 0.026(3) 0.004(2) -0.008(2) -0.001(2) C17C 0.018(3) 0.032(3) 0.024(3) 0.007(3) -0.004(2) -0.001(3) C17D 0.021(3) 0.017(3) 0.029(3) 0.003(3) -0.003(2) 0.003(2) C18A 0.031(3) 0.025(3) 0.027(3) -0.001(3) -0.005(2) 0.003(3) C18B 0.024(3) 0.029(3) 0.027(3) 0.004(3) 0.001(2) -0.002(3) C18C 0.016(3) 0.042(4) 0.025(3) 0.000(3) 0.001(2) -0.005(3) C18D 0.027(3) 0.036(4) 0.030(3) 0.001(3) -0.002(2) 0.007(3) C19A 0.025(3) 0.040(4) 0.034(3) 0.003(3) -0.002(2) 0.004(3) C19B 0.022(3) 0.043(4) 0.028(3) 0.001(3) -0.001(2) 0.000(3) C19C 0.028(3) 0.072(5) 0.026(3) -0.004(3) -0.003(3) -0.016(3) C19D 0.024(3) 0.044(4) 0.034(3) 0.005(3) 0.000(2) 0.018(3) C20A 0.025(3) 0.025(3) 0.019(2) 0.000(2) -0.006(2) 0.004(2) C20B 0.015(3) 0.027(3) 0.025(3) 0.005(3) -0.004(2) -0.007(2) C20C 0.021(3) 0.029(3) 0.026(3) 0.005(3) -0.001(2) 0.003(3) C20D 0.025(3) 0.032(3) 0.024(3) -0.001(3) -0.008(2) 0.000(3) C21A 0.035(4) 0.030(3) 0.030(3) 0.005(3) 0.000(3) -0.003(3) C21B 0.038(4) 0.037(4) 0.027(3) 0.000(3) 0.012(3) -0.002(3) C21C 0.033(3) 0.034(4) 0.027(3) 0.003(3) 0.000(2) -0.006(3) C21D 0.055(4) 0.022(3) 0.029(3) 0.003(3) -0.008(3) -0.005(3) C22A 0.024(3) 0.030(3) 0.024(3) -0.009(3) -0.008(2) -0.001(3) C22B 0.017(3) 0.032(3) 0.027(3) 0.007(3) -0.001(2) -0.002(3) C22C 0.021(3) 0.031(3) 0.024(2) 0.006(3) -0.004(2) 0.002(3) C22D 0.025(3) 0.033(4) 0.033(3) 0.002(3) -0.007(2) 0.003(3) C23A 0.015(3) 0.026(3) 0.028(3) 0.000(3) 0.002(2) -0.006(2) C23B 0.018(3) 0.027(3) 0.026(3) 0.007(3) 0.000(2) -0.001(3) C23C 0.025(3) 0.025(3) 0.025(3) 0.005(3) -0.002(2) 0.000(3) C23D 0.019(3) 0.030(3) 0.029(3) 0.008(3) -0.002(2) -0.004(3) C24A 0.022(3) 0.031(4) 0.022(3) -0.002(3) 0.000(2) 0.000(3) C24B 0.024(3) 0.033(4) 0.022(3) 0.002(3) 0.000(2) -0.002(3) C24C 0.026(3) 0.024(3) 0.029(3) 0.001(3) 0.002(2) 0.004(3) C24D 0.027(3) 0.032(4) 0.036(3) 0.003(3) -0.002(3) 0.004(3) C1F 0.029(3) 0.024(3) 0.026(3) 0.006(3) -0.008(2) 0.001(3) C2F 0.023(3) 0.025(3) 0.022(3) -0.002(3) -0.001(2) -0.002(2) C3F 0.026(3) 0.029(3) 0.016(2) -0.001(2) 0.003(2) -0.001(3) N1F 0.026(3) 0.016(2) 0.029(2) 0.000(2) -0.008(2) -0.006(2) N2F 0.036(3) 0.023(3) 0.086(4) 0.003(3) -0.038(3) -0.003(3) N3F 0.018(3) 0.027(3) 0.036(2) -0.003(2) -0.004(2) 0.001(2) N4F 0.028(3) 0.026(3) 0.030(2) -0.002(3) -0.009(2) -0.001(2) N5F 0.022(3) 0.027(3) 0.024(2) -0.005(2) -0.0034(19) 0.001(2) N6F 0.021(3) 0.021(3) 0.031(2) 0.000(2) -0.004(2) 0.003(2) C1E 0.023(3) 0.019(3) 0.027(3) 0.003(3) 0.002(2) 0.002(3) C2E 0.021(3) 0.027(3) 0.018(2) -0.002(2) 0.002(2) 0.002(2) C3E 0.024(3) 0.023(3) 0.020(3) 0.006(2) 0.002(2) 0.002(2) N1E 0.021(3) 0.019(3) 0.024(2) 0.003(2) -0.0006(19) -0.001(2) N2E 0.025(3) 0.023(3) 0.034(3) 0.001(2) -0.009(2) 0.001(2) N3E 0.018(3) 0.023(3) 0.022(2) -0.005(2) -0.0070(19) 0.002(2) N4E 0.016(2) 0.019(3) 0.046(3) -0.001(3) -0.012(2) 0.001(2) N5E 0.022(3) 0.029(3) 0.027(2) -0.004(2) -0.002(2) 0.001(2) N6E 0.029(3) 0.015(3) 0.043(3) 0.005(2) -0.013(2) 0.000(2) O3A 0.024(2) 0.035(2) 0.0303(19) -0.001(2) -0.0086(16) -0.0090(19) O3B 0.020(2) 0.029(2) 0.039(2) -0.004(2) -0.0105(17) 0.0034(17) O3C 0.021(2) 0.045(2) 0.0239(17) 0.001(2) -0.0080(16) -0.0073(19) O3D 0.025(2) 0.048(3) 0.031(2) -0.011(2) -0.0079(18) 0.004(2) O24A 0.029(2) 0.031(2) 0.052(2) 0.001(2) -0.014(2) 0.003(2) O24B 0.043(3) 0.025(2) 0.092(3) 0.003(3) -0.043(3) 0.001(2) O24C 0.039(3) 0.029(2) 0.057(3) -0.008(2) -0.023(2) 0.004(2) O24D 0.058(3) 0.027(3) 0.078(3) 0.012(2) -0.041(3) -0.008(2) O25A 0.027(2) 0.022(2) 0.040(2) -0.0076(19) -0.0124(17) 0.0029(18) O25B 0.025(2) 0.023(2) 0.037(2) 0.0041(19) -0.0108(17) -0.0041(18) O25C 0.034(3) 0.033(3) 0.036(2) -0.003(2) -0.0142(18) 0.011(2) O25D 0.042(3) 0.025(2) 0.050(2) 0.003(2) -0.025(2) -0.003(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1A C10A 1.527(7) . ? C1A C2A 1.544(6) . ? C1A H1A1 0.9900 . ? C1A H1A2 0.9900 . ? C1B C10B 1.525(7) . ? C1B C2B 1.526(6) . ? C1B H1B1 0.9900 . ? C1B H1B2 0.9900 . ? C1C C2C 1.521(7) . ? C1C C10D 1.541(7) . ? C1C H1C1 0.9900 . ? C1C H1C2 0.9900 . ? C1D C2D 1.512(7) . ? C1D C10E 1.554(7) . ? C1D H1D1 0.9900 . ? C1D H1D2 0.9900 . ? C2A C3A 1.500(7) . ? C2A H2A1 0.9900 . ? C2A H2A2 0.9900 . ? C2B C3B 1.509(7) . ? C2B H2B1 0.9900 . ? C2B H2B2 0.9900 . ? C2C C3C 1.497(7) . ? C2C H2C1 0.9900 . ? C2C H2C2 0.9900 . ? C2D C3D 1.513(7) . ? C2D H2D1 0.9900 . ? C2D H2D2 0.9900 . ? C3A O3A 1.456(6) . ? C3A C4A 1.522(7) . ? C3A H3A 1.0000 . ? C3B O3B 1.445(6) . ? C3B C4B 1.518(7) . ? C3B H3B 1.0000 . ? C3C O3C 1.436(6) . ? C3C C4C 1.518(7) . ? C3C H3C 1.0000 . ? C3D O3D 1.450(6) . ? C3D C4D 1.505(7) . ? C3D H3D 1.0000 . ? C4A C5A 1.545(6) . ? C4A H4A1 0.9900 . ? C4A H4A2 0.9900 . ? C4B C5B 1.548(6) . ? C4B H4B1 0.9900 . ? C4B H4B2 0.9900 . ? C4C C5C 1.534(6) . ? C4C H4C1 0.9900 . ? C4C H4C2 0.9900 . ? C4D C5D 1.535(6) . ? C4D H4D1 0.9900 . ? C4D H4D2 0.9900 . ? C5A C6A 1.528(7) . ? C5A C10A 1.560(7) . ? C5A H5A 1.0000 . ? C5B C6B 1.540(7) . ? C5B C10B 1.550(7) . ? C5B H5B 1.0000 . ? C5C C6C 1.537(7) . ? C5C C10D 1.544(8) . ? C5C H5C 1.0000 . ? C5D C6D 1.528(7) . ? C5D C10E 1.559(8) . ? C5D H5D 1.0000 . ? C6A C7A 1.524(7) . ? C6A H6A1 0.9900 . ? C6A H6A2 0.9900 . ? C6B C7B 1.537(7) . ? C6B H6B1 0.9900 . ? C6B H6B2 0.9900 . ? C6C C7C 1.531(7) . ? C6C H6C1 0.9900 . ? C6C H6C2 0.9900 . ? C6D C7D 1.525(7) . ? C6D H6D1 0.9900 . ? C6D H6D2 0.9900 . ? C7A C8A 1.525(7) . ? C7A H7A1 0.9900 . ? C7A H7A2 0.9900 . ? C7B C8B 1.523(7) . ? C7B H7B1 0.9900 . ? C7B H7B2 0.9900 . ? C7C C8C 1.519(7) . ? C7C H7C1 0.9900 . ? C7C H7C2 0.9900 . ? C7D C8D 1.511(7) . ? C7D H7D1 0.9900 . ? C7D H7D2 0.9900 . ? C8A C14A 1.525(7) . ? C8A C9A 1.537(7) . ? C8A H8A 1.0000 . ? C8B C14B 1.522(7) . ? C8B C9B 1.554(7) . ? C8B H8B 1.0000 . ? C8C C14C 1.524(7) . ? C8C C9C 1.553(7) . ? C8C H8C 1.0000 . ? C8D C14D 1.517(7) . ? C8D C9D 1.549(7) . ? C8D H8D 1.0000 . ? C9A C11A 1.536(7) . ? C9A C10A 1.568(7) . ? C9A H9A 1.0000 . ? C9B C11B 1.541(6) . ? C9B C10B 1.556(7) . ? C9B H9B 1.0000 . ? C9C C11C 1.518(7) . ? C9C C10D 1.554(7) . ? C9C H9C 1.0000 . ? C9D C11D 1.533(7) . ? C9D C10E 1.555(7) . ? C9D H9D 1.0000 . ? C10A C19A 1.541(6) . ? C10B C19B 1.551(6) . ? C10D C19C 1.540(7) . ? C10E C19D 1.533(6) . ? C11A C12A 1.527(7) . ? C11A H111 0.9900 . ? C11A H112 0.9900 . ? C11B C12B 1.525(7) . ? C11B H113 0.9900 . ? C11B H114 0.9900 . ? C11C C12C 1.550(7) . ? C11C H115 0.9900 . ? C11C H116 0.9900 . ? C11D C12D 1.544(7) . ? C11D H117 0.9900 . ? C11D H118 0.9900 . ? C12A C13A 1.537(7) . ? C12A H121 0.9900 . ? C12A H122 0.9900 . ? C12B C13B 1.538(7) . ? C12B H123 0.9900 . ? C12B H124 0.9900 . ? C12C C13D 1.524(7) . ? C12C H125 0.9900 . ? C12C H126 0.9900 . ? C12D C13E 1.528(7) . ? C12D H127 0.9900 . ? C12D H128 0.9900 . ? C13A C14A 1.541(7) . ? C13A C17A 1.545(7) . ? C13A C18A 1.546(6) . ? C13B C14B 1.546(7) . ? C13B C17B 1.553(7) . ? C13B C18B 1.554(6) . ? C13D C18C 1.534(6) . ? C13D C14C 1.542(7) . ? C13D C17C 1.554(7) . ? C13E C18D 1.549(6) . ? C13E C17D 1.552(7) . ? C13E C14D 1.558(7) . ? C14A C15A 1.522(7) . ? C14A H14A 1.0000 . ? C14B C15B 1.524(7) . ? C14B H14B 1.0000 . ? C14C C15C 1.526(7) . ? C14C H14C 1.0000 . ? C14D C15D 1.518(7) . ? C14D H14D 1.0000 . ? C15A C16A 1.540(7) . ? C15A H151 0.9900 . ? C15A H152 0.9900 . ? C15B C16B 1.534(7) . ? C15B H153 0.9900 . ? C15B H154 0.9900 . ? C15C C16C 1.546(7) . ? C15C H155 0.9900 . ? C15C H156 0.9900 . ? C15D C16D 1.539(7) . ? C15D H157 0.9900 . ? C15D H158 0.9900 . ? C16A C17A 1.552(7) . ? C16A H161 0.9900 . ? C16A H162 0.9900 . ? C16B C17B 1.573(7) . ? C16B H163 0.9900 . ? C16B H164 0.9900 . ? C16C C17C 1.561(7) . ? C16C H165 0.9900 . ? C16C H166 0.9900 . ? C16D C17D 1.562(7) . ? C16D H167 0.9900 . ? C16D H168 0.9900 . ? C17A C20A 1.542(7) . ? C17A H17A 1.0000 . ? C17B C20B 1.540(7) . ? C17B H17B 1.0000 . ? C17C C20C 1.542(7) . ? C17C H17C 1.0000 . ? C17D C20D 1.545(7) . ? C17D H17D 1.0000 . ? C18A H181 0.9800 . ? C18A H182 0.9800 . ? C18A H183 0.9800 . ? C18B H184 0.9800 . ? C18B H185 0.9800 . ? C18B H186 0.9800 . ? C18C H187 0.9800 . ? C18C H188 0.9800 . ? C18C H189 0.9800 . ? C18D H18A 0.9800 . ? C18D H18B 0.9800 . ? C18D H18C 0.9800 . ? C19A H19A 0.9800 . ? C19A H19B 0.9800 . ? C19A H19C 0.9800 . ? C19B H191 0.9800 . ? C19B H192 0.9800 . ? C19B H193 0.9800 . ? C19C H194 0.9800 . ? C19C H195 0.9800 . ? C19C H196 0.9800 . ? C19D H197 0.9800 . ? C19D H198 0.9800 . ? C19D H199 0.9800 . ? C20A C21A 1.529(7) . ? C20A C22A 1.546(7) . ? C20A H20A 1.0000 . ? C20B C22B 1.528(7) . ? C20B C21B 1.537(7) . ? C20B H20B 1.0000 . ? C20C C21C 1.537(7) . ? C20C C22C 1.547(7) . ? C20C H20C 1.0000 . ? C20D C21D 1.532(7) . ? C20D C22D 1.541(7) . ? C20D H20D 1.0000 . ? C21A H21A 0.9800 . ? C21A H21B 0.9800 . ? C21A H21C 0.9800 . ? C21B H211 0.9800 . ? C21B H212 0.9800 . ? C21B H213 0.9800 . ? C21C H214 0.9800 . ? C21C H215 0.9800 . ? C21C H216 0.9800 . ? C21D H217 0.9800 . ? C21D H218 0.9800 . ? C21D H219 0.9800 . ? C22A C23A 1.533(6) . ? C22A H221 0.9900 . ? C22A H222 0.9900 . ? C22B C23B 1.534(6) . ? C22B H223 0.9900 . ? C22B H224 0.9900 . ? C22C C23C 1.531(6) . ? C22C H225 0.9900 . ? C22C H226 0.9900 . ? C22D C23D 1.527(6) . ? C22D H227 0.9900 . ? C22D H228 0.9900 . ? C23A C24A 1.491(7) . ? C23A H231 0.9900 . ? C23A H232 0.9900 . ? C23B C24B 1.508(7) . ? C23B H233 0.9900 . ? C23B H234 0.9900 . ? C23C C24C 1.489(6) . ? C23C H235 0.9900 . ? C23C H236 0.9900 . ? C23D C24D 1.477(7) . ? C23D H237 0.9900 . ? C23D H238 0.9900 . ? C24A O24A 1.248(6) . ? C24A O25A 1.281(6) . ? C24B O24B 1.248(6) . ? C24B O25B 1.255(6) . ? C24C O24C 1.215(6) . ? C24C O25C 1.310(6) . ? C24D O24D 1.207(6) . ? C24D O25D 1.325(7) . ? C1F N2F 1.323(7) . ? C1F N3F 1.332(6) . ? C1F N1F 1.364(6) . ? C2F N4F 1.326(6) . ? C2F N5F 1.344(6) . ? C2F N3F 1.348(7) . ? C3F N5F 1.335(6) . ? C3F N6F 1.336(6) . ? C3F N1F 1.359(6) . ? N1F H1NF 1.10(6) . ? N2F H2FA 0.87(2) . ? N2F H2FB 0.89(2) . ? N4F H4FA 0.88(2) . ? N4F H4FB 0.87(2) . ? N6F H6FA 0.88(2) . ? N6F H6FB 0.87(2) . ? C1E N2E 1.292(7) . ? C1E N3E 1.344(6) . ? C1E N1E 1.366(6) . ? C2E N4E 1.330(7) . ? C2E N5E 1.331(6) . ? C2E N3E 1.356(6) . ? C3E N6E 1.323(6) . ? C3E N5E 1.329(6) . ? C3E N1E 1.362(6) . ? N1E H1NE 0.95(5) . ? N2E H2EA 0.88(2) . ? N2E H2EB 0.87(2) . ? N4E H4EA 0.88(2) . ? N4E H4EB 0.87(2) . ? N6E H6EA 0.87(2) . ? N6E H6EB 0.87(2) . ? O3A H3OA 0.83(2) . ? O3B H3OB 0.83(2) . ? O3C H3OC 0.833(19) . ? O3D H3OD 0.83(2) . ? O25C H25C 0.86(2) . ? O25D H25D 0.89(5) . ? 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 C10A C1A C2A 113.7(4) . . ? C10A C1A H1A1 108.8 . . ? C2A C1A H1A1 108.8 . . ? C10A C1A H1A2 108.8 . . ? C2A C1A H1A2 108.8 . . ? H1A1 C1A H1A2 107.7 . . ? C10B C1B C2B 114.0(4) . . ? C10B C1B H1B1 108.8 . . ? C2B C1B H1B1 108.8 . . ? C10B C1B H1B2 108.8 . . ? C2B C1B H1B2 108.8 . . ? H1B1 C1B H1B2 107.7 . . ? C2C C1C C10D 114.4(5) . . ? C2C C1C H1C1 108.7 . . ? C10D C1C H1C1 108.7 . . ? C2C C1C H1C2 108.7 . . ? C10D C1C H1C2 108.7 . . ? H1C1 C1C H1C2 107.6 . . ? C2D C1D C10E 115.1(4) . . ? C2D C1D H1D1 108.5 . . ? C10E C1D H1D1 108.5 . . ? C2D C1D H1D2 108.5 . . ? C10E C1D H1D2 108.5 . . ? H1D1 C1D H1D2 107.5 . . ? C3A C2A C1A 110.2(4) . . ? C3A C2A H2A1 109.6 . . ? C1A C2A H2A1 109.6 . . ? C3A C2A H2A2 109.6 . . ? C1A C2A H2A2 109.6 . . ? H2A1 C2A H2A2 108.1 . . ? C3B C2B C1B 110.5(4) . . ? C3B C2B H2B1 109.6 . . ? C1B C2B H2B1 109.6 . . ? C3B C2B H2B2 109.6 . . ? C1B C2B H2B2 109.6 . . ? H2B1 C2B H2B2 108.1 . . ? C3C C2C C1C 111.7(5) . . ? C3C C2C H2C1 109.3 . . ? C1C C2C H2C1 109.3 . . ? C3C C2C H2C2 109.3 . . ? C1C C2C H2C2 109.3 . . ? H2C1 C2C H2C2 107.9 . . ? C1D C2D C3D 111.7(5) . . ? C1D C2D H2D1 109.3 . . ? C3D C2D H2D1 109.3 . . ? C1D C2D H2D2 109.3 . . ? C3D C2D H2D2 109.3 . . ? H2D1 C2D H2D2 107.9 . . ? O3A C3A C2A 112.3(4) . . ? O3A C3A C4A 108.0(4) . . ? C2A C3A C4A 111.9(4) . . ? O3A C3A H3A 108.2 . . ? C2A C3A H3A 108.2 . . ? C4A C3A H3A 108.2 . . ? O3B C3B C2B 112.6(4) . . ? O3B C3B C4B 107.9(4) . . ? C2B C3B C4B 111.4(4) . . ? O3B C3B H3B 108.3 . . ? C2B C3B H3B 108.3 . . ? C4B C3B H3B 108.3 . . ? O3C C3C C2C 110.2(4) . . ? O3C C3C C4C 111.0(4) . . ? C2C C3C C4C 109.4(4) . . ? O3C C3C H3C 108.7 . . ? C2C C3C H3C 108.7 . . ? C4C C3C H3C 108.7 . . ? O3D C3D C4D 109.1(4) . . ? O3D C3D C2D 110.6(4) . . ? C4D C3D C2D 110.3(4) . . ? O3D C3D H3D 108.9 . . ? C4D C3D H3D 108.9 . . ? C2D C3D H3D 108.9 . . ? C3A C4A C5A 112.4(4) . . ? C3A C4A H4A1 109.1 . . ? C5A C4A H4A1 109.1 . . ? C3A C4A H4A2 109.1 . . ? C5A C4A H4A2 109.1 . . ? H4A1 C4A H4A2 107.9 . . ? C3B C4B C5B 112.6(4) . . ? C3B C4B H4B1 109.1 . . ? C5B C4B H4B1 109.1 . . ? C3B C4B H4B2 109.1 . . ? C5B C4B H4B2 109.1 . . ? H4B1 C4B H4B2 107.8 . . ? C3C C4C C5C 113.5(5) . . ? C3C C4C H4C1 108.9 . . ? C5C C4C H4C1 108.9 . . ? C3C C4C H4C2 108.9 . . ? C5C C4C H4C2 108.9 . . ? H4C1 C4C H4C2 107.7 . . ? C3D C4D C5D 111.8(4) . . ? C3D C4D H4D1 109.3 . . ? C5D C4D H4D1 109.3 . . ? C3D C4D H4D2 109.3 . . ? C5D C4D H4D2 109.3 . . ? H4D1 C4D H4D2 107.9 . . ? C6A C5A C4A 110.5(4) . . ? C6A C5A C10A 112.4(4) . . ? C4A C5A C10A 112.8(4) . . ? C6A C5A H5A 106.9 . . ? C4A C5A H5A 106.9 . . ? C10A C5A H5A 106.9 . . ? C6B C5B C4B 109.9(4) . . ? C6B C5B C10B 111.8(4) . . ? C4B C5B C10B 112.2(4) . . ? C6B C5B H5B 107.6 . . ? C4B C5B H5B 107.6 . . ? C10B C5B H5B 107.6 . . ? C4C C5C C6C 110.9(5) . . ? C4C C5C C10D 113.0(4) . . ? C6C C5C C10D 112.2(4) . . ? C4C C5C H5C 106.8 . . ? C6C C5C H5C 106.8 . . ? C10D C5C H5C 106.8 . . ? C6D C5D C4D 111.1(4) . . ? C6D C5D C10E 111.5(4) . . ? C4D C5D C10E 113.2(4) . . ? C6D C5D H5D 106.9 . . ? C4D C5D H5D 106.9 . . ? C10E C5D H5D 106.9 . . ? C7A C6A C5A 111.7(4) . . ? C7A C6A H6A1 109.3 . . ? C5A C6A H6A1 109.3 . . ? C7A C6A H6A2 109.3 . . ? C5A C6A H6A2 109.3 . . ? H6A1 C6A H6A2 107.9 . . ? C7B C6B C5B 113.2(4) . . ? C7B C6B H6B1 108.9 . . ? C5B C6B H6B1 108.9 . . ? C7B C6B H6B2 108.9 . . ? C5B C6B H6B2 108.9 . . ? H6B1 C6B H6B2 107.8 . . ? C7C C6C C5C 111.5(4) . . ? C7C C6C H6C1 109.3 . . ? C5C C6C H6C1 109.3 . . ? C7C C6C H6C2 109.3 . . ? C5C C6C H6C2 109.3 . . ? H6C1 C6C H6C2 108.0 . . ? C7D C6D C5D 111.9(5) . . ? C7D C6D H6D1 109.2 . . ? C5D C6D H6D1 109.2 . . ? C7D C6D H6D2 109.2 . . ? C5D C6D H6D2 109.2 . . ? H6D1 C6D H6D2 107.9 . . ? C6A C7A C8A 113.6(5) . . ? C6A C7A H7A1 108.8 . . ? C8A C7A H7A1 108.8 . . ? C6A C7A H7A2 108.8 . . ? C8A C7A H7A2 108.8 . . ? H7A1 C7A H7A2 107.7 . . ? C8B C7B C6B 113.4(4) . . ? C8B C7B H7B1 108.9 . . ? C6B C7B H7B1 108.9 . . ? C8B C7B H7B2 108.9 . . ? C6B C7B H7B2 108.9 . . ? H7B1 C7B H7B2 107.7 . . ? C8C C7C C6C 112.1(5) . . ? C8C C7C H7C1 109.2 . . ? C6C C7C H7C1 109.2 . . ? C8C C7C H7C2 109.2 . . ? C6C C7C H7C2 109.2 . . ? H7C1 C7C H7C2 107.9 . . ? C8D C7D C6D 112.9(5) . . ? C8D C7D H7D1 109.0 . . ? C6D C7D H7D1 109.0 . . ? C8D C7D H7D2 109.0 . . ? C6D C7D H7D2 109.0 . . ? H7D1 C7D H7D2 107.8 . . ? C7A C8A C14A 111.5(4) . . ? C7A C8A C9A 110.5(4) . . ? C14A C8A C9A 107.8(4) . . ? C7A C8A H8A 109.0 . . ? C14A C8A H8A 109.0 . . ? C9A C8A H8A 109.0 . . ? C14B C8B C7B 111.4(4) . . ? C14B C8B C9B 108.1(4) . . ? C7B C8B C9B 110.6(3) . . ? C14B C8B H8B 108.9 . . ? C7B C8B H8B 108.9 . . ? C9B C8B H8B 108.9 . . ? C7C C8C C14C 112.5(4) . . ? C7C C8C C9C 112.4(4) . . ? C14C C8C C9C 108.6(4) . . ? C7C C8C H8C 107.7 . . ? C14C C8C H8C 107.7 . . ? C9C C8C H8C 107.7 . . ? C7D C8D C14D 112.0(4) . . ? C7D C8D C9D 111.7(4) . . ? C14D C8D C9D 109.2(4) . . ? C7D C8D H8D 107.9 . . ? C14D C8D H8D 107.9 . . ? C9D C8D H8D 107.9 . . ? C11A C9A C8A 111.7(3) . . ? C11A C9A C10A 113.2(4) . . ? C8A C9A C10A 112.2(4) . . ? C11A C9A H9A 106.4 . . ? C8A C9A H9A 106.4 . . ? C10A C9A H9A 106.4 . . ? C11B C9B C8B 111.0(4) . . ? C11B C9B C10B 114.5(4) . . ? C8B C9B C10B 112.4(4) . . ? C11B C9B H9B 106.1 . . ? C8B C9B H9B 106.1 . . ? C10B C9B H9B 106.1 . . ? C11C C9C C8C 111.1(4) . . ? C11C C9C C10D 114.6(5) . . ? C8C C9C C10D 112.6(4) . . ? C11C C9C H9C 105.9 . . ? C8C C9C H9C 105.9 . . ? C10D C9C H9C 105.9 . . ? C11D C9D C8D 111.3(4) . . ? C11D C9D C10E 113.7(4) . . ? C8D C9D C10E 112.4(4) . . ? C11D C9D H9D 106.3 . . ? C8D C9D H9D 106.3 . . ? C10E C9D H9D 106.3 . . ? C1A C10A C19A 106.1(4) . . ? C1A C10A C5A 107.6(3) . . ? C19A C10A C5A 110.1(4) . . ? C1A C10A C9A 113.5(4) . . ? C19A C10A C9A 111.3(4) . . ? C5A C10A C9A 108.2(4) . . ? C1B C10B C5B 107.6(4) . . ? C1B C10B C19B 106.5(4) . . ? C5B C10B C19B 109.1(4) . . ? C1B C10B C9B 113.0(4) . . ? C5B C10B C9B 109.7(4) . . ? C19B C10B C9B 110.8(4) . . ? C19C C10D C1C 106.4(5) . . ? C19C C10D C5C 109.1(5) . . ? C1C C10D C5C 107.8(4) . . ? C19C C10D C9C 111.2(4) . . ? C1C C10D C9C 111.8(5) . . ? C5C C10D C9C 110.4(5) . . ? C19D C10E C1D 107.2(4) . . ? C19D C10E C9D 110.9(4) . . ? C1D C10E C9D 111.7(5) . . ? C19D C10E C5D 110.0(5) . . ? C1D C10E C5D 107.6(4) . . ? C9D C10E C5D 109.4(4) . . ? C12A C11A C9A 113.4(4) . . ? C12A C11A H111 108.9 . . ? C9A C11A H111 108.9 . . ? C12A C11A H112 108.9 . . ? C9A C11A H112 108.9 . . ? H111 C11A H112 107.7 . . ? C12B C11B C9B 113.9(4) . . ? C12B C11B H113 108.8 . . ? C9B C11B H113 108.8 . . ? C12B C11B H114 108.8 . . ? C9B C11B H114 108.8 . . ? H113 C11B H114 107.7 . . ? C9C C11C C12C 113.3(4) . . ? C9C C11C H115 108.9 . . ? C12C C11C H115 108.9 . . ? C9C C11C H116 108.9 . . ? C12C C11C H116 108.9 . . ? H115 C11C H116 107.7 . . ? C9D C11D C12D 113.4(4) . . ? C9D C11D H117 108.9 . . ? C12D C11D H117 108.9 . . ? C9D C11D H118 108.9 . . ? C12D C11D H118 108.9 . . ? H117 C11D H118 107.7 . . ? C11A C12A C13A 112.5(5) . . ? C11A C12A H121 109.1 . . ? C13A C12A H121 109.1 . . ? C11A C12A H122 109.1 . . ? C13A C12A H122 109.1 . . ? H121 C12A H122 107.8 . . ? C11B C12B C13B 111.6(4) . . ? C11B C12B H123 109.3 . . ? C13B C12B H123 109.3 . . ? C11B C12B H124 109.3 . . ? C13B C12B H124 109.3 . . ? H123 C12B H124 108.0 . . ? C13D C12C C11C 112.4(4) . . ? C13D C12C H125 109.1 . . ? C11C C12C H125 109.1 . . ? C13D C12C H126 109.1 . . ? C11C C12C H126 109.1 . . ? H125 C12C H126 107.9 . . ? C13E C12D C11D 112.1(5) . . ? C13E C12D H127 109.2 . . ? C11D C12D H127 109.2 . . ? C13E C12D H128 109.2 . . ? C11D C12D H128 109.2 . . ? H127 C12D H128 107.9 . . ? C12A C13A C14A 107.0(4) . . ? C12A C13A C17A 117.4(4) . . ? C14A C13A C17A 100.1(4) . . ? C12A C13A C18A 109.6(4) . . ? C14A C13A C18A 112.4(4) . . ? C17A C13A C18A 110.1(4) . . ? C12B C13B C14B 107.1(3) . . ? C12B C13B C17B 116.4(4) . . ? C14B C13B C17B 100.7(4) . . ? C12B C13B C18B 110.4(4) . . ? C14B C13B C18B 111.8(4) . . ? C17B C13B C18B 110.0(4) . . ? C12C C13D C18C 111.3(4) . . ? C12C C13D C14C 106.6(4) . . ? C18C C13D C14C 112.0(4) . . ? C12C C13D C17C 115.6(4) . . ? C18C C13D C17C 110.6(4) . . ? C14C C13D C17C 100.1(4) . . ? C12D C13E C18D 111.2(4) . . ? C12D C13E C17D 116.6(4) . . ? C18D C13E C17D 109.5(4) . . ? C12D C13E C14D 107.6(4) . . ? C18D C13E C14D 111.2(4) . . ? C17D C13E C14D 100.1(4) . . ? C15A C14A C8A 118.2(4) . . ? C15A C14A C13A 104.3(4) . . ? C8A C14A C13A 114.8(4) . . ? C15A C14A H14A 106.2 . . ? C8A C14A H14A 106.2 . . ? C13A C14A H14A 106.2 . . ? C8B C14B C15B 119.2(4) . . ? C8B C14B C13B 115.1(4) . . ? C15B C14B C13B 104.0(4) . . ? C8B C14B H14B 105.8 . . ? C15B C14B H14B 105.8 . . ? C13B C14B H14B 105.8 . . ? C8C C14C C15C 119.5(4) . . ? C8C C14C C13D 114.9(4) . . ? C15C C14C C13D 104.0(3) . . ? C8C C14C H14C 105.8 . . ? C15C C14C H14C 105.8 . . ? C13D C14C H14C 105.8 . . ? C8D C14D C15D 120.2(4) . . ? C8D C14D C13E 113.8(4) . . ? C15D C14D C13E 104.5(4) . . ? C8D C14D H14D 105.7 . . ? C15D C14D H14D 105.7 . . ? C13E C14D H14D 105.7 . . ? C14A C15A C16A 103.3(4) . . ? C14A C15A H151 111.1 . . ? C16A C15A H151 111.1 . . ? C14A C15A H152 111.1 . . ? C16A C15A H152 111.1 . . ? H151 C15A H152 109.1 . . ? C14B C15B C16B 104.2(4) . . ? C14B C15B H153 110.9 . . ? C16B C15B H153 110.9 . . ? C14B C15B H154 110.9 . . ? C16B C15B H154 110.9 . . ? H153 C15B H154 108.9 . . ? C14C C15C C16C 103.4(4) . . ? C14C C15C H155 111.1 . . ? C16C C15C H155 111.1 . . ? C14C C15C H156 111.1 . . ? C16C C15C H156 111.1 . . ? H155 C15C H156 109.1 . . ? C14D C15D C16D 104.1(4) . . ? C14D C15D H157 110.9 . . ? C16D C15D H157 110.9 . . ? C14D C15D H158 110.9 . . ? C16D C15D H158 110.9 . . ? H157 C15D H158 109.0 . . ? C15A C16A C17A 107.4(4) . . ? C15A C16A H161 110.2 . . ? C17A C16A H161 110.2 . . ? C15A C16A H162 110.2 . . ? C17A C16A H162 110.2 . . ? H161 C16A H162 108.5 . . ? C15B C16B C17B 107.0(4) . . ? C15B C16B H163 110.3 . . ? C17B C16B H163 110.3 . . ? C15B C16B H164 110.3 . . ? C17B C16B H164 110.3 . . ? H163 C16B H164 108.6 . . ? C15C C16C C17C 106.8(4) . . ? C15C C16C H165 110.4 . . ? C17C C16C H165 110.4 . . ? C15C C16C H166 110.4 . . ? C17C C16C H166 110.4 . . ? H165 C16C H166 108.6 . . ? C15D C16D C17D 107.3(4) . . ? C15D C16D H167 110.3 . . ? C17D C16D H167 110.3 . . ? C15D C16D H168 110.3 . . ? C17D C16D H168 110.3 . . ? H167 C16D H168 108.5 . . ? C20A C17A C13A 119.6(4) . . ? C20A C17A C16A 113.4(4) . . ? C13A C17A C16A 103.2(4) . . ? C20A C17A H17A 106.6 . . ? C13A C17A H17A 106.6 . . ? C16A C17A H17A 106.6 . . ? C20B C17B C13B 119.5(4) . . ? C20B C17B C16B 111.8(4) . . ? C13B C17B C16B 103.3(4) . . ? C20B C17B H17B 107.2 . . ? C13B C17B H17B 107.2 . . ? C16B C17B H17B 107.2 . . ? C20C C17C C13D 119.2(4) . . ? C20C C17C C16C 111.6(4) . . ? C13D C17C C16C 103.8(4) . . ? C20C C17C H17C 107.2 . . ? C13D C17C H17C 107.2 . . ? C16C C17C H17C 107.2 . . ? C20D C17D C13E 119.8(4) . . ? C20D C17D C16D 111.7(4) . . ? C13E C17D C16D 103.6(4) . . ? C20D C17D H17D 107.0 . . ? C13E C17D H17D 107.0 . . ? C16D C17D H17D 107.0 . . ? C13A C18A H181 109.5 . . ? C13A C18A H182 109.5 . . ? H181 C18A H182 109.5 . . ? C13A C18A H183 109.5 . . ? H181 C18A H183 109.5 . . ? H182 C18A H183 109.5 . . ? C13B C18B H184 109.5 . . ? C13B C18B H185 109.5 . . ? H184 C18B H185 109.5 . . ? C13B C18B H186 109.5 . . ? H184 C18B H186 109.5 . . ? H185 C18B H186 109.5 . . ? C13D C18C H187 109.5 . . ? C13D C18C H188 109.5 . . ? H187 C18C H188 109.5 . . ? C13D C18C H189 109.5 . . ? H187 C18C H189 109.5 . . ? H188 C18C H189 109.5 . . ? C13E C18D H18A 109.5 . . ? C13E C18D H18B 109.5 . . ? H18A C18D H18B 109.5 . . ? C13E C18D H18C 109.5 . . ? H18A C18D H18C 109.5 . . ? H18B C18D H18C 109.5 . . ? C10A C19A H19A 109.5 . . ? C10A C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? C10A C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? C10B C19B H191 109.5 . . ? C10B C19B H192 109.5 . . ? H191 C19B H192 109.5 . . ? C10B C19B H193 109.5 . . ? H191 C19B H193 109.5 . . ? H192 C19B H193 109.5 . . ? C10D C19C H194 109.5 . . ? C10D C19C H195 109.5 . . ? H194 C19C H195 109.5 . . ? C10D C19C H196 109.5 . . ? H194 C19C H196 109.5 . . ? H195 C19C H196 109.5 . . ? C10E C19D H197 109.5 . . ? C10E C19D H198 109.5 . . ? H197 C19D H198 109.5 . . ? C10E C19D H199 109.5 . . ? H197 C19D H199 109.5 . . ? H198 C19D H199 109.5 . . ? C21A C20A C17A 113.6(4) . . ? C21A C20A C22A 110.1(5) . . ? C17A C20A C22A 107.8(4) . . ? C21A C20A H20A 108.4 . . ? C17A C20A H20A 108.4 . . ? C22A C20A H20A 108.4 . . ? C22B C20B C21B 110.8(5) . . ? C22B C20B C17B 108.9(4) . . ? C21B C20B C17B 112.7(4) . . ? C22B C20B H20B 108.1 . . ? C21B C20B H20B 108.1 . . ? C17B C20B H20B 108.1 . . ? C21C C20C C17C 113.9(4) . . ? C21C C20C C22C 109.5(4) . . ? C17C C20C C22C 108.3(4) . . ? C21C C20C H20C 108.3 . . ? C17C C20C H20C 108.3 . . ? C22C C20C H20C 108.3 . . ? C21D C20D C22D 110.1(5) . . ? C21D C20D C17D 114.1(4) . . ? C22D C20D C17D 109.1(4) . . ? C21D C20D H20D 107.8 . . ? C22D C20D H20D 107.8 . . ? C17D C20D H20D 107.8 . . ? C20A C21A H21A 109.5 . . ? C20A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? C20A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? C20B C21B H211 109.5 . . ? C20B C21B H212 109.5 . . ? H211 C21B H212 109.5 . . ? C20B C21B H213 109.5 . . ? H211 C21B H213 109.5 . . ? H212 C21B H213 109.5 . . ? C20C C21C H214 109.5 . . ? C20C C21C H215 109.5 . . ? H214 C21C H215 109.5 . . ? C20C C21C H216 109.5 . . ? H214 C21C H216 109.5 . . ? H215 C21C H216 109.5 . . ? C20D C21D H217 109.5 . . ? C20D C21D H218 109.5 . . ? H217 C21D H218 109.5 . . ? C20D C21D H219 109.5 . . ? H217 C21D H219 109.5 . . ? H218 C21D H219 109.5 . . ? C23A C22A C20A 115.7(4) . . ? C23A C22A H221 108.4 . . ? C20A C22A H221 108.4 . . ? C23A C22A H222 108.4 . . ? C20A C22A H222 108.4 . . ? H221 C22A H222 107.4 . . ? C20B C22B C23B 115.8(4) . . ? C20B C22B H223 108.3 . . ? C23B C22B H223 108.3 . . ? C20B C22B H224 108.3 . . ? C23B C22B H224 108.3 . . ? H223 C22B H224 107.4 . . ? C23C C22C C20C 114.1(4) . . ? C23C C22C H225 108.7 . . ? C20C C22C H225 108.7 . . ? C23C C22C H226 108.7 . . ? C20C C22C H226 108.7 . . ? H225 C22C H226 107.6 . . ? C23D C22D C20D 114.5(4) . . ? C23D C22D H227 108.6 . . ? C20D C22D H227 108.6 . . ? C23D C22D H228 108.6 . . ? C20D C22D H228 108.6 . . ? H227 C22D H228 107.6 . . ? C24A C23A C22A 110.8(4) . . ? C24A C23A H231 109.5 . . ? C22A C23A H231 109.5 . . ? C24A C23A H232 109.5 . . ? C22A C23A H232 109.5 . . ? H231 C23A H232 108.1 . . ? C24B C23B C22B 112.8(4) . . ? C24B C23B H233 109.0 . . ? C22B C23B H233 109.0 . . ? C24B C23B H234 109.0 . . ? C22B C23B H234 109.0 . . ? H233 C23B H234 107.8 . . ? C24C C23C C22C 114.8(4) . . ? C24C C23C H235 108.6 . . ? C22C C23C H235 108.6 . . ? C24C C23C H236 108.6 . . ? C22C C23C H236 108.6 . . ? H235 C23C H236 107.5 . . ? C24D C23D C22D 115.3(5) . . ? C24D C23D H237 108.5 . . ? C22D C23D H237 108.5 . . ? C24D C23D H238 108.5 . . ? C22D C23D H238 108.5 . . ? H237 C23D H238 107.5 . . ? O24A C24A O25A 123.2(5) . . ? O24A C24A C23A 119.5(5) . . ? O25A C24A C23A 117.3(5) . . ? O24B C24B O25B 123.4(5) . . ? O24B C24B C23B 117.6(5) . . ? O25B C24B C23B 118.9(5) . . ? O24C C24C O25C 122.0(5) . . ? O24C C24C C23C 123.5(5) . . ? O25C C24C C23C 114.4(5) . . ? O24D C24D O25D 120.6(5) . . ? O24D C24D C23D 124.1(6) . . ? O25D C24D C23D 115.2(5) . . ? N2F C1F N3F 120.4(5) . . ? N2F C1F N1F 116.8(5) . . ? N3F C1F N1F 122.8(5) . . ? N4F C2F N5F 117.8(5) . . ? N4F C2F N3F 115.5(5) . . ? N5F C2F N3F 126.7(5) . . ? N5F C3F N6F 120.1(5) . . ? N5F C3F N1F 123.3(5) . . ? N6F C3F N1F 116.6(5) . . ? C3F N1F C1F 117.3(5) . . ? C3F N1F H1NF 125(3) . . ? C1F N1F H1NF 118(3) . . ? C1F N2F H2FA 125(4) . . ? C1F N2F H2FB 112(4) . . ? H2FA N2F H2FB 123(6) . . ? C1F N3F C2F 115.2(5) . . ? C2F N4F H4FA 124(4) . . ? C2F N4F H4FB 122(4) . . ? H4FA N4F H4FB 113(5) . . ? C3F N5F C2F 114.7(5) . . ? C3F N6F H6FA 117(3) . . ? C3F N6F H6FB 117(3) . . ? H6FA N6F H6FB 123(5) . . ? N2E C1E N3E 121.1(5) . . ? N2E C1E N1E 119.2(5) . . ? N3E C1E N1E 119.7(5) . . ? N4E C2E N5E 118.3(5) . . ? N4E C2E N3E 115.5(5) . . ? N5E C2E N3E 126.2(5) . . ? N6E C3E N5E 121.2(5) . . ? N6E C3E N1E 116.1(5) . . ? N5E C3E N1E 122.7(5) . . ? C3E N1E C1E 119.4(5) . . ? C3E N1E H1NE 123(3) . . ? C1E N1E H1NE 117(4) . . ? C1E N2E H2EA 119(4) . . ? C1E N2E H2EB 116(4) . . ? H2EA N2E H2EB 124(5) . . ? C1E N3E C2E 116.7(4) . . ? C2E N4E H4EA 124(4) . . ? C2E N4E H4EB 122(3) . . ? H4EA N4E H4EB 113(5) . . ? C3E N5E C2E 115.1(5) . . ? C3E N6E H6EA 121(4) . . ? C3E N6E H6EB 119(4) . . ? H6EA N6E H6EB 120(5) . . ? C3A O3A H3OA 113(4) . . ? C3B O3B H3OB 119(4) . . ? C3C O3C H3OC 111(4) . . ? C3D O3D H3OD 106(4) . . ? C24C O25C H25C 109(4) . . ? C24D O25D H25D 98(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10A C1A C2A C3A 58.7(6) . . . . ? C10B C1B C2B C3B 58.4(6) . . . . ? C10D C1C C2C C3C 57.6(6) . . . . ? C10E C1D C2D C3D 54.7(6) . . . . ? C1A C2A C3A O3A -176.5(4) . . . . ? C1A C2A C3A C4A -54.9(6) . . . . ? C1B C2B C3B O3B -175.6(4) . . . . ? C1B C2B C3B C4B -54.2(6) . . . . ? C1C C2C C3C O3C -178.0(4) . . . . ? C1C C2C C3C C4C -55.6(6) . . . . ? C1D C2D C3D O3D -176.7(4) . . . . ? C1D C2D C3D C4D -55.9(6) . . . . ? O3A C3A C4A C5A 177.4(4) . . . . ? C2A C3A C4A C5A 53.3(6) . . . . ? O3B C3B C4B C5B 177.3(4) . . . . ? C2B C3B C4B C5B 53.2(6) . . . . ? O3C C3C C4C C5C 176.9(4) . . . . ? C2C C3C C4C C5C 55.0(6) . . . . ? O3D C3D C4D C5D 178.8(4) . . . . ? C2D C3D C4D C5D 57.1(6) . . . . ? C3A C4A C5A C6A -179.5(4) . . . . ? C3A C4A C5A C10A -52.7(6) . . . . ? C3B C4B C5B C6B -178.8(4) . . . . ? C3B C4B C5B C10B -53.8(6) . . . . ? C3C C4C C5C C6C 178.9(4) . . . . ? C3C C4C C5C C10D -54.2(6) . . . . ? C3D C4D C5D C6D 177.0(4) . . . . ? C3D C4D C5D C10E -56.6(6) . . . . ? C4A C5A C6A C7A 72.8(5) . . . . ? C10A C5A C6A C7A -54.2(6) . . . . ? C4B C5B C6B C7B 73.2(5) . . . . ? C10B C5B C6B C7B -52.1(6) . . . . ? C4C C5C C6C C7C 71.3(5) . . . . ? C10D C5C C6C C7C -56.0(6) . . . . ? C4D C5D C6D C7D 71.5(6) . . . . ? C10E C5D C6D C7D -55.8(6) . . . . ? C5A C6A C7A C8A 52.7(6) . . . . ? C5B C6B C7B C8B 51.1(6) . . . . ? C5C C6C C7C C8C 54.7(6) . . . . ? C5D C6D C7D C8D 54.4(6) . . . . ? C6A C7A C8A C14A -173.2(4) . . . . ? C6A C7A C8A C9A -53.3(6) . . . . ? C6B C7B C8B C14B -172.0(4) . . . . ? C6B C7B C8B C9B -51.8(6) . . . . ? C6C C7C C8C C14C -175.6(4) . . . . ? C6C C7C C8C C9C -52.6(6) . . . . ? C6D C7D C8D C14D -175.5(4) . . . . ? C6D C7D C8D C9D -52.6(6) . . . . ? C7A C8A C9A C11A -175.7(5) . . . . ? C14A C8A C9A C11A -53.7(5) . . . . ? C7A C8A C9A C10A 55.9(6) . . . . ? C14A C8A C9A C10A 178.0(4) . . . . ? C14B C8B C9B C11B -52.8(5) . . . . ? C7B C8B C9B C11B -175.0(4) . . . . ? C14B C8B C9B C10B 177.6(4) . . . . ? C7B C8B C9B C10B 55.4(6) . . . . ? C7C C8C C9C C11C -178.2(4) . . . . ? C14C C8C C9C C11C -53.0(6) . . . . ? C7C C8C C9C C10D 51.8(6) . . . . ? C14C C8C C9C C10D 177.0(4) . . . . ? C7D C8D C9D C11D -177.9(4) . . . . ? C14D C8D C9D C11D -53.4(6) . . . . ? C7D C8D C9D C10E 53.3(6) . . . . ? C14D C8D C9D C10E 177.8(4) . . . . ? C2A C1A C10A C19A -174.0(4) . . . . ? C2A C1A C10A C5A -56.2(6) . . . . ? C2A C1A C10A C9A 63.4(6) . . . . ? C6A C5A C10A C1A 178.5(5) . . . . ? C4A C5A C10A C1A 52.8(5) . . . . ? C6A C5A C10A C19A -66.3(6) . . . . ? C4A C5A C10A C19A 168.0(4) . . . . ? C6A C5A C10A C9A 55.6(5) . . . . ? C4A C5A C10A C9A -70.2(5) . . . . ? C11A C9A C10A C1A 56.4(5) . . . . ? C8A C9A C10A C1A -176.0(4) . . . . ? C11A C9A C10A C19A -63.2(6) . . . . ? C8A C9A C10A C19A 64.4(6) . . . . ? C11A C9A C10A C5A 175.8(4) . . . . ? C8A C9A C10A C5A -56.7(5) . . . . ? C2B C1B C10B C5B -56.9(5) . . . . ? C2B C1B C10B C19B -173.8(4) . . . . ? C2B C1B C10B C9B 64.3(5) . . . . ? C6B C5B C10B C1B 177.5(4) . . . . ? C4B C5B C10B C1B 53.6(5) . . . . ? C6B C5B C10B C19B -67.3(5) . . . . ? C4B C5B C10B C19B 168.7(4) . . . . ? C6B C5B C10B C9B 54.3(5) . . . . ? C4B C5B C10B C9B -69.7(5) . . . . ? C11B C9B C10B C1B 55.6(5) . . . . ? C8B C9B C10B C1B -176.7(4) . . . . ? C11B C9B C10B C5B 175.6(4) . . . . ? C8B C9B C10B C5B -56.7(5) . . . . ? C11B C9B C10B C19B -63.9(6) . . . . ? C8B C9B C10B C19B 63.9(5) . . . . ? C2C C1C C10D C19C -169.9(4) . . . . ? C2C C1C C10D C5C -52.9(6) . . . . ? C2C C1C C10D C9C 68.6(6) . . . . ? C4C C5C C10D C19C 165.6(4) . . . . ? C6C C5C C10D C19C -68.2(6) . . . . ? C4C C5C C10D C1C 50.4(6) . . . . ? C6C C5C C10D C1C 176.6(4) . . . . ? C4C C5C C10D C9C -71.9(5) . . . . ? C6C C5C C10D C9C 54.3(6) . . . . ? C11C C9C C10D C19C -59.0(6) . . . . ? C8C C9C C10D C19C 69.3(6) . . . . ? C11C C9C C10D C1C 59.8(6) . . . . ? C8C C9C C10D C1C -171.9(4) . . . . ? C11C C9C C10D C5C 179.8(4) . . . . ? C8C C9C C10D C5C -52.0(5) . . . . ? C2D C1D C10E C19D -168.8(5) . . . . ? C2D C1D C10E C9D 69.5(6) . . . . ? C2D C1D C10E C5D -50.6(6) . . . . ? C11D C9D C10E C19D -60.2(6) . . . . ? C8D C9D C10E C19D 67.4(6) . . . . ? C11D C9D C10E C1D 59.3(5) . . . . ? C8D C9D C10E C1D -173.2(4) . . . . ? C11D C9D C10E C5D 178.3(4) . . . . ? C8D C9D C10E C5D -54.2(5) . . . . ? C6D C5D C10E C19D -66.7(6) . . . . ? C4D C5D C10E C19D 167.2(4) . . . . ? C6D C5D C10E C1D 176.9(5) . . . . ? C4D C5D C10E C1D 50.8(6) . . . . ? C6D C5D C10E C9D 55.4(6) . . . . ? C4D C5D C10E C9D -70.7(5) . . . . ? C8A C9A C11A C12A 52.7(6) . . . . ? C10A C9A C11A C12A -179.5(4) . . . . ? C8B C9B C11B C12B 53.3(6) . . . . ? C10B C9B C11B C12B -178.3(4) . . . . ? C8C C9C C11C C12C 52.5(6) . . . . ? C10D C9C C11C C12C -178.5(4) . . . . ? C8D C9D C11D C12D 52.2(6) . . . . ? C10E C9D C11D C12D -179.7(4) . . . . ? C9A C11A C12A C13A -53.1(6) . . . . ? C9B C11B C12B C13B -54.7(5) . . . . ? C9C C11C C12C C13D -54.7(6) . . . . ? C9D C11D C12D C13E -53.9(6) . . . . ? C11A C12A C13A C14A 53.6(6) . . . . ? C11A C12A C13A C17A 165.0(4) . . . . ? C11A C12A C13A C18A -68.5(5) . . . . ? C11B C12B C13B C14B 54.5(5) . . . . ? C11B C12B C13B C17B 166.2(4) . . . . ? C11B C12B C13B C18B -67.5(5) . . . . ? C11C C12C C13D C18C -67.8(5) . . . . ? C11C C12C C13D C14C 54.6(5) . . . . ? C11C C12C C13D C17C 164.9(4) . . . . ? C11D C12D C13E C18D -67.5(5) . . . . ? C11D C12D C13E C17D 165.9(4) . . . . ? C11D C12D C13E C14D 54.5(5) . . . . ? C7A C8A C14A C15A -54.8(6) . . . . ? C9A C8A C14A C15A -176.3(4) . . . . ? C7A C8A C14A C13A -178.7(4) . . . . ? C9A C8A C14A C13A 59.8(5) . . . . ? C12A C13A C14A C15A 169.7(4) . . . . ? C17A C13A C14A C15A 46.8(5) . . . . ? C18A C13A C14A C15A -70.0(5) . . . . ? C12A C13A C14A C8A -59.4(5) . . . . ? C17A C13A C14A C8A 177.8(4) . . . . ? C18A C13A C14A C8A 61.0(5) . . . . ? C7B C8B C14B C15B -54.7(6) . . . . ? C9B C8B C14B C15B -176.4(4) . . . . ? C7B C8B C14B C13B -179.3(4) . . . . ? C9B C8B C14B C13B 59.0(5) . . . . ? C12B C13B C14B C8B -59.6(5) . . . . ? C17B C13B C14B C8B 178.3(4) . . . . ? C18B C13B C14B C8B 61.5(5) . . . . ? C12B C13B C14B C15B 168.2(4) . . . . ? C17B C13B C14B C15B 46.0(5) . . . . ? C18B C13B C14B C15B -70.8(5) . . . . ? C7C C8C C14C C15C -51.2(6) . . . . ? C9C C8C C14C C15C -176.4(4) . . . . ? C7C C8C C14C C13D -175.9(4) . . . . ? C9C C8C C14C C13D 59.0(5) . . . . ? C12C C13D C14C C8C -59.5(5) . . . . ? C18C C13D C14C C8C 62.5(5) . . . . ? C17C C13D C14C C8C 179.7(4) . . . . ? C12C C13D C14C C15C 168.1(4) . . . . ? C18C C13D C14C C15C -70.0(5) . . . . ? C17C C13D C14C C15C 47.3(5) . . . . ? C7D C8D C14D C15D -51.9(6) . . . . ? C9D C8D C14D C15D -176.2(4) . . . . ? C7D C8D C14D C13E -176.9(4) . . . . ? C9D C8D C14D C13E 58.8(5) . . . . ? C12D C13E C14D C8D -59.2(5) . . . . ? C18D C13E C14D C8D 62.9(5) . . . . ? C17D C13E C14D C8D 178.5(4) . . . . ? C12D C13E C14D C15D 167.8(4) . . . . ? C18D C13E C14D C15D -70.2(5) . . . . ? C17D C13E C14D C15D 45.5(5) . . . . ? C8A C14A C15A C16A -163.4(4) . . . . ? C13A C14A C15A C16A -34.5(5) . . . . ? C8B C14B C15B C16B -165.5(4) . . . . ? C13B C14B C15B C16B -35.7(5) . . . . ? C8C C14C C15C C16C -167.1(4) . . . . ? C13D C14C C15C C16C -37.4(5) . . . . ? C8D C14D C15D C16D -163.5(4) . . . . ? C13E C14D C15D C16D -34.2(5) . . . . ? C14A C15A C16A C17A 8.8(5) . . . . ? C14B C15B C16B C17B 11.3(5) . . . . ? C14C C15C C16C C17C 12.7(5) . . . . ? C14D C15D C16D C17D 9.4(5) . . . . ? C12A C13A C17A C20A 77.9(6) . . . . ? C14A C13A C17A C20A -166.8(4) . . . . ? C18A C13A C17A C20A -48.4(6) . . . . ? C12A C13A C17A C16A -155.1(4) . . . . ? C14A C13A C17A C16A -39.8(4) . . . . ? C18A C13A C17A C16A 78.6(5) . . . . ? C15A C16A C17A C20A 150.6(4) . . . . ? C15A C16A C17A C13A 19.8(5) . . . . ? C12B C13B C17B C20B 81.9(6) . . . . ? C14B C13B C17B C20B -162.8(4) . . . . ? C18B C13B C17B C20B -44.6(6) . . . . ? C12B C13B C17B C16B -153.1(4) . . . . ? C14B C13B C17B C16B -37.7(4) . . . . ? C18B C13B C17B C16B 80.4(5) . . . . ? C15B C16B C17B C20B 146.7(4) . . . . ? C15B C16B C17B C13B 16.9(5) . . . . ? C12C C13D C17C C20C 83.0(6) . . . . ? C18C C13D C17C C20C -44.7(6) . . . . ? C14C C13D C17C C20C -163.0(4) . . . . ? C12C C13D C17C C16C -152.2(4) . . . . ? C18C C13D C17C C16C 80.2(5) . . . . ? C14C C13D C17C C16C -38.1(4) . . . . ? C15C C16C C17C C20C 145.8(4) . . . . ? C15C C16C C17C C13D 16.2(5) . . . . ? C12D C13E C17D C20D 80.8(6) . . . . ? C18D C13E C17D C20D -46.7(6) . . . . ? C14D C13E C17D C20D -163.6(4) . . . . ? C12D C13E C17D C16D -154.0(4) . . . . ? C18D C13E C17D C16D 78.6(5) . . . . ? C14D C13E C17D C16D -38.3(4) . . . . ? C15D C16D C17D C20D 149.0(4) . . . . ? C15D C16D C17D C13E 18.7(5) . . . . ? C13A C17A C20A C21A -57.1(7) . . . . ? C16A C17A C20A C21A -179.2(5) . . . . ? C13A C17A C20A C22A -179.5(4) . . . . ? C16A C17A C20A C22A 58.4(6) . . . . ? C13B C17B C20B C22B -177.5(4) . . . . ? C16B C17B C20B C22B 61.6(6) . . . . ? C13B C17B C20B C21B -54.2(6) . . . . ? C16B C17B C20B C21B -175.0(4) . . . . ? C13D C17C C20C C21C -51.7(6) . . . . ? C16C C17C C20C C21C -172.8(4) . . . . ? C13D C17C C20C C22C -173.8(4) . . . . ? C16C C17C C20C C22C 65.2(5) . . . . ? C13E C17D C20D C21D -52.2(7) . . . . ? C16D C17D C20D C21D -173.5(5) . . . . ? C13E C17D C20D C22D -175.8(4) . . . . ? C16D C17D C20D C22D 62.8(5) . . . . ? C21A C20A C22A C23A 67.7(5) . . . . ? C17A C20A C22A C23A -167.8(4) . . . . ? C21B C20B C22B C23B 66.6(6) . . . . ? C17B C20B C22B C23B -168.9(4) . . . . ? C21C C20C C22C C23C 70.3(5) . . . . ? C17C C20C C22C C23C -165.0(4) . . . . ? C21D C20D C22D C23D 71.2(6) . . . . ? C17D C20D C22D C23D -162.9(4) . . . . ? C20A C22A C23A C24A 68.4(6) . . . . ? C20B C22B C23B C24B 71.1(6) . . . . ? C20C C22C C23C C24C 70.4(6) . . . . ? C20D C22D C23D C24D 68.5(7) . . . . ? C22A C23A C24A O24A -112.3(6) . . . . ? C22A C23A C24A O25A 66.2(6) . . . . ? C22B C23B C24B O24B -119.5(5) . . . . ? C22B C23B C24B O25B 60.9(6) . . . . ? C22C C23C C24C O24C -136.5(5) . . . . ? C22C C23C C24C O25C 45.2(7) . . . . ? C22D C23D C24D O24D -143.4(6) . . . . ? C22D C23D C24D O25D 37.5(7) . . . . ? N5F C3F N1F C1F -2.8(8) . . . . ? N6F C3F N1F C1F 177.3(5) . . . . ? N2F C1F N1F C3F -178.3(5) . . . . ? N3F C1F N1F C3F 1.2(8) . . . . ? N2F C1F N3F C2F -179.3(6) . . . . ? N1F C1F N3F C2F 1.2(8) . . . . ? N4F C2F N3F C1F 177.6(5) . . . . ? N5F C2F N3F C1F -2.4(8) . . . . ? N6F C3F N5F C2F -178.3(5) . . . . ? N1F C3F N5F C2F 1.8(7) . . . . ? N4F C2F N5F C3F -179.1(5) . . . . ? N3F C2F N5F C3F 0.9(8) . . . . ? N6E C3E N1E C1E -177.2(5) . . . . ? N5E C3E N1E C1E 3.2(8) . . . . ? N2E C1E N1E C3E 178.9(5) . . . . ? N3E C1E N1E C3E -1.9(7) . . . . ? N2E C1E N3E C2E 177.2(5) . . . . ? N1E C1E N3E C2E -1.9(7) . . . . ? N4E C2E N3E C1E -175.1(5) . . . . ? N5E C2E N3E C1E 5.2(8) . . . . ? N6E C3E N5E C2E -179.9(5) . . . . ? N1E C3E N5E C2E -0.4(7) . . . . ? N4E C2E N5E C3E 176.3(5) . . . . ? N3E C2E N5E C3E -4.0(8) . . . . ? 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 N1E H1NE O25B 0.95(5) 1.74(5) 2.677(5) 166(6) 2_536 N1E H1NE O24B 0.95(5) 2.63(6) 3.356(6) 133(4) 2_536 N1F H1NF O25A 1.10(6) 1.52(5) 2.597(5) 167(5) 1_545 N1F H1NF O24A 1.10(6) 2.50(6) 3.332(6) 131(4) 1_545 N2F H2FA O24A 0.87(2) 1.87(3) 2.715(6) 161(6) 1_545 N2F H2FB O24D 0.89(2) 1.92(2) 2.814(6) 175(6) 2_647 N4F H4FA O24D 0.88(2) 1.95(2) 2.826(6) 175(6) 2_657 N4F H4FB O3C 0.87(2) 2.32(4) 2.984(6) 133(5) 2_647 N6F H6FA O24A 0.88(2) 1.91(2) 2.784(6) 172(5) . N6F H6FB O3B 0.87(2) 2.58(3) 3.354(6) 149(5) 1_545 N2E H2EA O24C 0.88(2) 1.96(2) 2.827(6) 165(5) 1_545 N2E H2EB O24B 0.87(2) 1.84(2) 2.715(5) 176(5) 2_536 N4E H4EA O3D 0.88(2) 2.36(4) 3.121(6) 144(5) . N4E H4EB O24C 0.87(2) 1.99(2) 2.858(6) 176(5) . N6E H6EA O3A 0.87(2) 2.39(3) 3.228(6) 162(5) 2_546 N6E H6EB O24B 0.87(2) 1.88(2) 2.749(6) 176(6) 2_546 O25C H25C N3E 0.86(2) 1.81(2) 2.653(5) 167(6) 1_565 O25D H25D N3F 0.89(5) 1.79(5) 2.625(5) 155(6) 2_657 O3A H3OA O25B 0.83(2) 1.99(3) 2.745(5) 152(6) 1_545 O3B H3OB O25A 0.83(2) 2.10(2) 2.916(5) 167(6) . O3C H3OC O3A 0.833(19) 2.01(2) 2.836(5) 173(5) 1_556 O3D H3OD O3B 0.83(2) 2.11(2) 2.940(5) 176(6) 1_545 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.271 _refine_diff_density_min -0.292 _refine_diff_density_rms 0.059 data_2 _database_code_depnum_ccdc_archive 'CCDC 773835' #TrackingRef '- structures 1_2_3' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Salt of deoxycholic acid and melamine' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H46 N6 O4' _chemical_formula_weight 518.70 _chemical_absolute_configuration syn 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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 20.0656(3) _cell_length_b 7.6866(10) _cell_length_c 20.2789(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.3047(9) _cell_angle_gamma 90.00 _cell_volume 2827.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 34591 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 28.283 _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.218 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 Kappa APEX-II' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11264 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 28.28 _reflns_number_total 3747 _reflns_number_gt 3378 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Bruker, 2004)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR-2002 (Burla, et al., 2003)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97; MERCURY (Macrae, et al., 2006)' _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^ > 2\s(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^)+(0.0677P)^2^+1.9571P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3747 _refine_ls_number_parameters 361 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1246 _refine_ls_wR_factor_gt 0.1200 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.17044(15) 0.2413(4) 0.03403(14) 0.0304(6) Uani 1 1 d . . . H1A H 0.1996 0.2249 0.0056 0.037 Uiso 1 1 calc R . . H1B H 0.1710 0.1297 0.0586 0.037 Uiso 1 1 calc R . . C2 C 0.09097(15) 0.2826(4) -0.01883(15) 0.0273(6) Uani 1 1 d . . . H2A H 0.0714 0.1893 -0.0559 0.033 Uiso 1 1 calc R . . H2B H 0.0598 0.2886 0.0080 0.033 Uiso 1 1 calc R . . C3 C 0.08857(13) 0.4556(4) -0.05604(13) 0.0243(5) Uani 1 1 d . . . H3 H 0.1187 0.4454 -0.0844 0.029 Uiso 1 1 calc R . . C4 C 0.12112(14) 0.5984(4) 0.00022(14) 0.0247(5) Uani 1 1 d . . . H4A H 0.0904 0.6129 0.0272 0.030 Uiso 1 1 calc R . . H4B H 0.1200 0.7094 -0.0250 0.030 Uiso 1 1 calc R . . C5 C 0.20090(14) 0.5589(4) 0.05472(15) 0.0294(6) Uani 1 1 d . . . H5 H 0.2305 0.5518 0.0257 0.035 Uiso 1 1 calc R . . C6 C 0.23386(16) 0.7063(5) 0.10921(16) 0.0355(7) Uani 1 1 d . . . H6A H 0.2258 0.8179 0.0825 0.043 Uiso 1 1 calc R . . H6B H 0.2877 0.6884 0.1361 0.043 Uiso 1 1 calc R . . C7 C 0.19952(16) 0.7169(4) 0.16407(15) 0.0307(6) Uani 1 1 d . . . H7A H 0.2242 0.8097 0.2001 0.037 Uiso 1 1 calc R . . H7B H 0.1466 0.7471 0.1380 0.037 Uiso 1 1 calc R . . C8 C 0.20764(14) 0.5425(4) 0.20380(14) 0.0239(5) Uani 1 1 d . . . H8 H 0.2613 0.5180 0.2327 0.029 Uiso 1 1 calc R . . C9 C 0.17355(13) 0.3933(4) 0.14836(13) 0.0217(5) Uani 1 1 d . . . H9 H 0.1204 0.4235 0.1193 0.026 Uiso 1 1 calc R . . C10 C 0.20862(14) 0.3799(4) 0.09269(14) 0.0272(6) Uani 1 1 d . . . C11 C 0.17510(15) 0.2192(4) 0.18684(14) 0.0260(5) Uani 1 1 d . . . H11A H 0.1468 0.1318 0.1495 0.031 Uiso 1 1 calc R . . H11B H 0.2267 0.1782 0.2113 0.031 Uiso 1 1 calc R . . C12 C 0.14326(14) 0.2288(3) 0.24361(13) 0.0228(5) Uani 1 1 d . . . H12 H 0.1550 0.1161 0.2709 0.027 Uiso 1 1 calc R . . C13 C 0.18043(13) 0.3744(3) 0.29959(13) 0.0203(5) Uani 1 1 d . . . C14 C 0.17063(13) 0.5453(3) 0.25595(13) 0.0213(5) Uani 1 1 d . . . H14 H 0.1165 0.5592 0.2251 0.026 Uiso 1 1 calc R . . C15 C 0.19296(16) 0.6887(4) 0.31373(15) 0.0286(6) Uani 1 1 d . . . H15A H 0.1674 0.7991 0.2926 0.034 Uiso 1 1 calc R . . H15B H 0.2469 0.7086 0.3354 0.034 Uiso 1 1 calc R . . C16 C 0.16853(15) 0.6172(4) 0.37163(14) 0.0252(5) Uani 1 1 d . . . H16A H 0.2100 0.6224 0.4208 0.030 Uiso 1 1 calc R . . H16B H 0.1273 0.6874 0.3719 0.030 Uiso 1 1 calc R . . C17 C 0.14372(13) 0.4258(3) 0.35082(13) 0.0194(5) Uani 1 1 d . . . H17 H 0.0892 0.4275 0.3203 0.023 Uiso 1 1 calc R . . C18 C 0.26215(14) 0.3293(4) 0.34544(14) 0.0300(6) Uani 1 1 d . . . H18A H 0.2658 0.2208 0.3721 0.045 Uiso 1 1 calc R . . H18B H 0.2859 0.4235 0.3802 0.045 Uiso 1 1 calc R . . H18C H 0.2868 0.3150 0.3132 0.045 Uiso 1 1 calc R . . C19 C 0.29076(15) 0.3283(6) 0.13149(17) 0.0426(8) Uani 1 1 d . . . H19A H 0.3174 0.4140 0.1694 0.064 Uiso 1 1 calc R . . H19B H 0.3118 0.3249 0.0959 0.064 Uiso 1 1 calc R . . H19C H 0.2952 0.2132 0.1538 0.064 Uiso 1 1 calc R . . C20 C 0.15783(14) 0.3115(4) 0.41783(13) 0.0233(5) Uani 1 1 d . . . H20 H 0.2115 0.3193 0.4513 0.028 Uiso 1 1 calc R . . C21 C 0.13934(18) 0.1194(4) 0.39873(15) 0.0318(6) Uani 1 1 d . . . H21A H 0.1494 0.0534 0.4433 0.048 Uiso 1 1 calc R . . H21B H 0.1697 0.0738 0.3755 0.048 Uiso 1 1 calc R . . H21C H 0.0871 0.1080 0.3651 0.048 Uiso 1 1 calc R . . C22 C 0.11463(14) 0.3877(4) 0.45835(13) 0.0238(5) Uani 1 1 d . . . H22A H 0.1338 0.5054 0.4763 0.029 Uiso 1 1 calc R . . H22B H 0.0622 0.3998 0.4235 0.029 Uiso 1 1 calc R . . C23 C 0.11960(18) 0.2767(4) 0.52255(15) 0.0339(7) Uani 1 1 d . . . H23A H 0.0897 0.1706 0.5028 0.041 Uiso 1 1 calc R . . H23B H 0.1715 0.2391 0.5498 0.041 Uiso 1 1 calc R . . C24 C 0.09511(14) 0.3594(4) 0.57623(14) 0.0251(5) Uani 1 1 d . . . O3 O 0.01393(10) 0.4957(3) -0.10570(10) 0.0275(4) Uani 1 1 d . . . H3O H 0.0198(18) 0.563(5) -0.1387(19) 0.033 Uiso 1 1 d . . . O12 O 0.06413(10) 0.2450(3) 0.20856(10) 0.0256(4) Uani 1 1 d . . . H12O H 0.0541(19) 0.321(5) 0.1782(19) 0.031 Uiso 1 1 d . . . O24 O 0.07665(15) 0.2654(3) 0.61448(14) 0.0440(6) Uani 1 1 d . . . O25 O 0.09520(13) 0.5253(3) 0.58047(12) 0.0347(5) Uani 1 1 d . . . C1' C -0.04904(13) 0.5673(3) 0.26748(13) 0.0210(5) Uani 1 1 d . . . C2' C -0.01950(13) 0.8231(3) 0.23046(14) 0.0216(5) Uani 1 1 d . . . C3' C -0.04718(14) 0.8242(3) 0.32662(14) 0.0236(5) Uani 1 1 d . . . N1 N -0.05894(12) 0.6498(3) 0.32101(12) 0.0227(4) Uani 1 1 d . . . H1N H -0.0730(17) 0.607(5) 0.3492(18) 0.027 Uiso 1 1 d . . . N2 N -0.06034(13) 0.3953(3) 0.26061(14) 0.0265(5) Uani 1 1 d . . . H2NA H -0.0446(19) 0.348(5) 0.2360(19) 0.032 Uiso 1 1 d . . . H2NB H -0.0645(19) 0.348(5) 0.293(2) 0.032 Uiso 1 1 d . . . N3 N -0.02873(11) 0.6500(3) 0.22057(11) 0.0212(4) Uani 1 1 d . . . N4 N 0.00024(14) 0.9082(3) 0.18375(13) 0.0296(5) Uani 1 1 d . . . H4NB H 0.0062(19) 0.850(5) 0.150(2) 0.036 Uiso 1 1 d . . . H4NA H 0.0133(19) 1.015(5) 0.196(2) 0.036 Uiso 1 1 d . . . N5 N -0.02889(12) 0.9179(3) 0.28134(12) 0.0246(5) Uani 1 1 d . . . N6 N -0.05390(16) 0.9035(4) 0.38222(15) 0.0339(6) Uani 1 1 d . . . H6NA H -0.078(2) 0.849(5) 0.404(2) 0.041 Uiso 1 1 d . . . H6NB H -0.058(2) 1.016(6) 0.381(2) 0.041 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0353(14) 0.0370(15) 0.0261(13) 0.0045(12) 0.0200(11) 0.0140(12) C2 0.0366(14) 0.0254(13) 0.0239(12) -0.0009(10) 0.0167(11) 0.0010(11) C3 0.0242(11) 0.0324(14) 0.0189(11) 0.0005(10) 0.0118(9) -0.0006(10) C4 0.0265(12) 0.0277(13) 0.0233(12) 0.0036(10) 0.0137(10) -0.0028(10) C5 0.0239(12) 0.0442(17) 0.0244(13) 0.0041(12) 0.0144(10) -0.0068(12) C6 0.0339(14) 0.0458(18) 0.0283(14) 0.0018(13) 0.0146(12) -0.0147(13) C7 0.0387(15) 0.0288(14) 0.0260(13) 0.0003(11) 0.0152(12) -0.0117(12) C8 0.0240(11) 0.0294(13) 0.0198(11) 0.0008(10) 0.0108(9) -0.0035(10) C9 0.0217(11) 0.0268(13) 0.0193(11) 0.0008(10) 0.0113(9) 0.0032(10) C10 0.0216(11) 0.0407(15) 0.0243(12) 0.0071(12) 0.0147(10) 0.0082(11) C11 0.0363(14) 0.0228(12) 0.0226(12) 0.0015(10) 0.0162(11) 0.0075(11) C12 0.0294(12) 0.0202(12) 0.0217(11) 0.0017(10) 0.0137(10) 0.0036(10) C13 0.0205(11) 0.0214(11) 0.0206(11) 0.0017(9) 0.0105(9) 0.0044(9) C14 0.0212(11) 0.0222(12) 0.0200(11) -0.0008(10) 0.0085(9) -0.0022(10) C15 0.0377(14) 0.0258(14) 0.0225(13) -0.0037(10) 0.0132(11) -0.0100(11) C16 0.0321(13) 0.0218(12) 0.0235(12) -0.0025(10) 0.0137(10) -0.0039(10) C17 0.0215(11) 0.0201(12) 0.0183(11) -0.0010(9) 0.0102(9) 0.0020(9) C18 0.0243(12) 0.0438(17) 0.0224(12) 0.0043(12) 0.0105(10) 0.0089(12) C19 0.0242(13) 0.075(3) 0.0306(14) 0.0092(16) 0.0138(11) 0.0168(15) C20 0.0262(11) 0.0244(12) 0.0195(11) 0.0008(10) 0.0100(9) 0.0018(10) C21 0.0518(17) 0.0235(13) 0.0256(13) 0.0017(11) 0.0217(12) 0.0018(12) C22 0.0280(12) 0.0257(12) 0.0205(11) 0.0032(10) 0.0132(9) 0.0036(10) C23 0.0526(17) 0.0309(15) 0.0263(13) 0.0083(12) 0.0245(13) 0.0127(13) C24 0.0273(12) 0.0283(14) 0.0210(12) 0.0015(10) 0.0115(10) 0.0038(10) O3 0.0251(9) 0.0377(12) 0.0204(9) 0.0039(8) 0.0104(7) 0.0004(8) O12 0.0310(9) 0.0241(10) 0.0221(9) 0.0004(7) 0.0118(7) -0.0046(8) O24 0.0795(17) 0.0249(11) 0.0531(14) 0.0012(10) 0.0527(14) 0.0018(11) O25 0.0546(13) 0.0253(10) 0.0358(11) -0.0006(9) 0.0305(10) -0.0032(9) C1' 0.0172(10) 0.0226(12) 0.0218(12) -0.0014(9) 0.0071(9) 0.0001(9) C2' 0.0189(10) 0.0221(12) 0.0226(12) 0.0004(10) 0.0078(9) -0.0003(9) C3' 0.0241(11) 0.0216(12) 0.0277(13) -0.0029(10) 0.0135(10) -0.0005(10) N1 0.0280(10) 0.0215(11) 0.0234(11) 0.0007(9) 0.0155(9) -0.0009(8) N2 0.0362(12) 0.0212(11) 0.0287(12) -0.0034(9) 0.0202(10) -0.0043(9) N3 0.0220(9) 0.0223(10) 0.0199(10) -0.0013(8) 0.0097(8) -0.0016(8) N4 0.0409(13) 0.0244(12) 0.0299(12) -0.0022(10) 0.0211(10) -0.0058(10) N5 0.0273(10) 0.0188(11) 0.0302(11) -0.0029(9) 0.0147(9) -0.0032(8) N6 0.0481(14) 0.0251(13) 0.0411(14) -0.0063(11) 0.0311(12) -0.0050(11) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C2 1.527(4) . ? C1 C10 1.535(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.520(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 O3 1.436(3) . ? C3 C4 1.515(4) . ? C3 H3 1.0000 . ? C4 C5 1.538(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.523(4) . ? C5 C10 1.552(4) . ? C5 H5 1.0000 . ? C6 C7 1.541(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.536(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C14 1.530(3) . ? C8 C9 1.546(4) . ? C8 H8 1.0000 . ? C9 C11 1.543(4) . ? C9 C10 1.568(3) . ? C9 H9 1.0000 . ? C10 C19 1.544(4) . ? C11 C12 1.539(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O12 1.441(3) . ? C12 C13 1.541(4) . ? C12 H12 1.0000 . ? C13 C18 1.540(3) . ? C13 C14 1.549(4) . ? C13 C17 1.559(3) . ? C14 C15 1.529(4) . ? C14 H14 1.0000 . ? C15 C16 1.553(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.553(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C20 1.539(3) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.532(4) . ? C20 C22 1.542(3) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.524(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.512(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O24 1.227(3) . ? C24 O25 1.278(4) . ? O3 H3O 0.89(4) . ? O12 H12O 0.81(4) . ? C1' N2 1.339(4) . ? C1' N1 1.343(3) . ? C1' N3 1.344(3) . ? C2' N5 1.341(3) . ? C2' N4 1.342(3) . ? C2' N3 1.347(3) . ? C3' N5 1.336(3) . ? C3' N6 1.338(4) . ? C3' N1 1.357(3) . ? N1 H1N 0.81(4) . ? N2 H2NA 0.78(4) . ? N2 H2NB 0.78(4) . ? N4 H4NB 0.87(4) . ? N4 H4NA 0.87(4) . ? N6 H6NA 0.89(4) . ? N6 H6NB 0.87(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C10 115.2(2) . . ? C2 C1 H1A 108.5 . . ? C10 C1 H1A 108.5 . . ? C2 C1 H1B 108.5 . . ? C10 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? C3 C2 C1 109.4(2) . . ? C3 C2 H2A 109.8 . . ? C1 C2 H2A 109.8 . . ? C3 C2 H2B 109.8 . . ? C1 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? O3 C3 C4 110.9(2) . . ? O3 C3 C2 109.8(2) . . ? C4 C3 C2 110.4(2) . . ? O3 C3 H3 108.6 . . ? C4 C3 H3 108.6 . . ? C2 C3 H3 108.6 . . ? C3 C4 C5 112.3(2) . . ? C3 C4 H4A 109.1 . . ? C5 C4 H4A 109.1 . . ? C3 C4 H4B 109.1 . . ? C5 C4 H4B 109.1 . . ? H4A C4 H4B 107.9 . . ? C6 C5 C4 111.7(3) . . ? C6 C5 C10 112.3(2) . . ? C4 C5 C10 112.6(2) . . ? C6 C5 H5 106.6 . . ? C4 C5 H5 106.6 . . ? C10 C5 H5 106.6 . . ? C5 C6 C7 111.9(2) . . ? C5 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 . . ? C5 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C8 C7 C6 110.6(3) . . ? C8 C7 H7A 109.5 . . ? C6 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? C14 C8 C7 112.1(2) . . ? C14 C8 C9 108.57(19) . . ? C7 C8 C9 110.6(2) . . ? C14 C8 H8 108.5 . . ? C7 C8 H8 108.5 . . ? C9 C8 H8 108.5 . . ? C11 C9 C8 111.64(19) . . ? C11 C9 C10 112.9(2) . . ? C8 C9 C10 112.1(2) . . ? C11 C9 H9 106.6 . . ? C8 C9 H9 106.6 . . ? C10 C9 H9 106.6 . . ? C1 C10 C19 106.7(3) . . ? C1 C10 C5 108.6(2) . . ? C19 C10 C5 109.8(2) . . ? C1 C10 C9 112.0(2) . . ? C19 C10 C9 111.1(2) . . ? C5 C10 C9 108.6(2) . . ? C12 C11 C9 114.3(2) . . ? C12 C11 H11A 108.7 . . ? C9 C11 H11A 108.7 . . ? C12 C11 H11B 108.7 . . ? C9 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? O12 C12 C11 110.9(2) . . ? O12 C12 C13 112.64(19) . . ? C11 C12 C13 111.2(2) . . ? O12 C12 H12 107.3 . . ? C11 C12 H12 107.3 . . ? C13 C12 H12 107.3 . . ? C18 C13 C12 109.7(2) . . ? C18 C13 C14 112.2(2) . . ? C12 C13 C14 106.97(19) . . ? C18 C13 C17 109.8(2) . . ? C12 C13 C17 117.2(2) . . ? C14 C13 C17 100.66(19) . . ? C15 C14 C8 118.0(2) . . ? C15 C14 C13 104.4(2) . . ? C8 C14 C13 113.7(2) . . ? C15 C14 H14 106.7 . . ? C8 C14 H14 106.7 . . ? C13 C14 H14 106.7 . . ? C14 C15 C16 103.9(2) . . ? C14 C15 H15A 111.0 . . ? C16 C15 H15A 111.0 . . ? C14 C15 H15B 111.0 . . ? C16 C15 H15B 111.0 . . ? H15A C15 H15B 109.0 . . ? C17 C16 C15 107.3(2) . . ? C17 C16 H16A 110.2 . . ? C15 C16 H16A 110.2 . . ? C17 C16 H16B 110.2 . . ? C15 C16 H16B 110.2 . . ? H16A C16 H16B 108.5 . . ? C20 C17 C16 112.6(2) . . ? C20 C17 C13 118.8(2) . . ? C16 C17 C13 103.5(2) . . ? C20 C17 H17 107.1 . . ? C16 C17 H17 107.1 . . ? C13 C17 H17 107.1 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C10 C19 H19A 109.5 . . ? C10 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C10 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C17 113.2(2) . . ? C21 C20 C22 111.7(2) . . ? C17 C20 C22 108.7(2) . . ? C21 C20 H20 107.7 . . ? C17 C20 H20 107.7 . . ? C22 C20 H20 107.7 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C20 113.4(2) . . ? C23 C22 H22A 108.9 . . ? C20 C22 H22A 108.9 . . ? C23 C22 H22B 108.9 . . ? C20 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? C24 C23 C22 117.2(2) . . ? C24 C23 H23A 108.0 . . ? C22 C23 H23A 108.0 . . ? C24 C23 H23B 108.0 . . ? C22 C23 H23B 108.0 . . ? H23A C23 H23B 107.2 . . ? O24 C24 O25 122.5(3) . . ? O24 C24 C23 119.1(3) . . ? O25 C24 C23 118.4(3) . . ? C3 O3 H3O 103(2) . . ? C12 O12 H12O 108(2) . . ? N2 C1' N1 118.3(2) . . ? N2 C1' N3 118.8(2) . . ? N1 C1' N3 122.9(2) . . ? N5 C2' N4 117.3(2) . . ? N5 C2' N3 126.6(2) . . ? N4 C2' N3 116.1(2) . . ? N5 C3' N6 119.3(3) . . ? N5 C3' N1 124.3(2) . . ? N6 C3' N1 116.3(3) . . ? C1' N1 C3' 117.0(2) . . ? C1' N1 H1N 127(3) . . ? C3' N1 H1N 116(3) . . ? C1' N2 H2NA 115(3) . . ? C1' N2 H2NB 117(3) . . ? H2NA N2 H2NB 122(4) . . ? C1' N3 C2' 115.2(2) . . ? C2' N4 H4NB 119(3) . . ? C2' N4 H4NA 113(2) . . ? H4NB N4 H4NA 127(3) . . ? C3' N5 C2' 114.0(2) . . ? C3' N6 H6NA 119(3) . . ? C3' N6 H6NB 118(3) . . ? H6NA N6 H6NB 114(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 C1 C2 C3 57.0(3) . . . . ? C1 C2 C3 O3 -179.8(2) . . . . ? C1 C2 C3 C4 -57.2(3) . . . . ? O3 C3 C4 C5 179.5(2) . . . . ? C2 C3 C4 C5 57.7(3) . . . . ? C3 C4 C5 C6 177.9(2) . . . . ? C3 C4 C5 C10 -54.6(3) . . . . ? C4 C5 C6 C7 71.1(3) . . . . ? C10 C5 C6 C7 -56.6(3) . . . . ? C5 C6 C7 C8 56.0(3) . . . . ? C6 C7 C8 C14 -177.1(2) . . . . ? C6 C7 C8 C9 -55.8(3) . . . . ? C14 C8 C9 C11 -51.9(3) . . . . ? C7 C8 C9 C11 -175.2(2) . . . . ? C14 C8 C9 C10 -179.7(2) . . . . ? C7 C8 C9 C10 57.0(3) . . . . ? C2 C1 C10 C19 -170.9(2) . . . . ? C2 C1 C10 C5 -52.6(3) . . . . ? C2 C1 C10 C9 67.4(3) . . . . ? C6 C5 C10 C1 177.0(2) . . . . ? C4 C5 C10 C1 49.9(3) . . . . ? C6 C5 C10 C19 -66.6(3) . . . . ? C4 C5 C10 C19 166.2(2) . . . . ? C6 C5 C10 C9 55.0(3) . . . . ? C4 C5 C10 C9 -72.2(3) . . . . ? C11 C9 C10 C1 57.4(3) . . . . ? C8 C9 C10 C1 -175.4(2) . . . . ? C11 C9 C10 C19 -61.8(3) . . . . ? C8 C9 C10 C19 65.4(3) . . . . ? C11 C9 C10 C5 177.4(2) . . . . ? C8 C9 C10 C5 -55.5(3) . . . . ? C8 C9 C11 C12 50.8(3) . . . . ? C10 C9 C11 C12 178.2(2) . . . . ? C9 C11 C12 O12 72.8(3) . . . . ? C9 C11 C12 C13 -53.3(3) . . . . ? O12 C12 C13 C18 168.7(2) . . . . ? C11 C12 C13 C18 -66.1(3) . . . . ? O12 C12 C13 C14 -69.3(2) . . . . ? C11 C12 C13 C14 55.9(3) . . . . ? O12 C12 C13 C17 42.6(3) . . . . ? C11 C12 C13 C17 167.9(2) . . . . ? C7 C8 C14 C15 -54.7(3) . . . . ? C9 C8 C14 C15 -177.1(2) . . . . ? C7 C8 C14 C13 -177.5(2) . . . . ? C9 C8 C14 C13 60.1(3) . . . . ? C18 C13 C14 C15 -71.6(2) . . . . ? C12 C13 C14 C15 168.0(2) . . . . ? C17 C13 C14 C15 45.1(2) . . . . ? C18 C13 C14 C8 58.4(3) . . . . ? C12 C13 C14 C8 -61.9(2) . . . . ? C17 C13 C14 C8 175.11(19) . . . . ? C8 C14 C15 C16 -160.5(2) . . . . ? C13 C14 C15 C16 -33.1(3) . . . . ? C14 C15 C16 C17 8.1(3) . . . . ? C15 C16 C17 C20 149.1(2) . . . . ? C15 C16 C17 C13 19.5(3) . . . . ? C18 C13 C17 C20 -46.1(3) . . . . ? C12 C13 C17 C20 80.0(3) . . . . ? C14 C13 C17 C20 -164.5(2) . . . . ? C18 C13 C17 C16 79.6(2) . . . . ? C12 C13 C17 C16 -154.4(2) . . . . ? C14 C13 C17 C16 -38.9(2) . . . . ? C16 C17 C20 C21 -175.4(2) . . . . ? C13 C17 C20 C21 -54.3(3) . . . . ? C16 C17 C20 C22 59.8(3) . . . . ? C13 C17 C20 C22 -179.0(2) . . . . ? C21 C20 C22 C23 49.8(3) . . . . ? C17 C20 C22 C23 175.4(2) . . . . ? C20 C22 C23 C24 165.7(2) . . . . ? C22 C23 C24 O24 157.9(3) . . . . ? C22 C23 C24 O25 -22.8(4) . . . . ? N2 C1' N1 C3' -179.9(2) . . . . ? N3 C1' N1 C3' -0.3(4) . . . . ? N5 C3' N1 C1' 2.2(4) . . . . ? N6 C3' N1 C1' -177.0(2) . . . . ? N2 C1' N3 C2' 179.1(2) . . . . ? N1 C1' N3 C2' -0.6(3) . . . . ? N5 C2' N3 C1' -0.4(4) . . . . ? N4 C2' N3 C1' -179.5(2) . . . . ? N6 C3' N5 C2' 176.2(2) . . . . ? N1 C3' N5 C2' -2.9(4) . . . . ? N4 C2' N5 C3' -178.9(2) . . . . ? N3 C2' N5 C3' 2.0(4) . . . . ? 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 O12 H12O O3 0.81(4) 2.03(4) 2.780(3) 154(3) 2 N6 H6NA O25 0.89(4) 2.55(4) 3.201(4) 130(3) 2_556 N6 H6NB O24 0.87(4) 1.96(4) 2.825(4) 172(4) 2_566 O3 H3O N3 0.89(4) 1.87(4) 2.741(3) 165(4) 2 N2 H2NB O24 0.78(4) 2.10(4) 2.869(3) 170(4) 2_556 N2 H2NA O12 0.78(4) 2.59(4) 3.307(3) 152(3) . N4 H4NA O12 0.87(4) 2.00(4) 2.837(3) 161(3) 1_565 N1 H1N O25 0.81(4) 1.78(4) 2.585(3) 173(3) 2_556 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.977 _refine_diff_density_min -0.201 _refine_diff_density_rms 0.048 data_3 _database_code_depnum_ccdc_archive 'CCDC 773836' #TrackingRef '- structures 1_2_3' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Cholic acid-melamine co-crystal hemihydrate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H94 N12 O11' _chemical_formula_weight 1087.41 _chemical_absolute_configuration syn 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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 19.7152(7) _cell_length_b 7.7592(3) _cell_length_c 20.4722(7) _cell_angle_alpha 90.00 _cell_angle_beta 115.078(2) _cell_angle_gamma 90.00 _cell_volume 2836.49(18) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 5869 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 28.283 _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.273 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1180 _exptl_absorpt_coefficient_mu 0.090 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 Kappa APEX-II' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11218 _diffrn_reflns_av_R_equivalents 0.0541 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 28.28 _reflns_number_total 3765 _reflns_number_gt 3058 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Bruker, 2004)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR-2002 (Burla, et al., 2003)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97; MERCURY (Macrae, et al., 2006)' _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^ > 2\s(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^)+(0.0720P)^2^+3.4297P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3765 _refine_ls_number_parameters 378 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0858 _refine_ls_R_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.1615 _refine_ls_wR_factor_gt 0.1514 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8208(3) 0.0640(6) 0.9636(2) 0.0431(12) Uani 1 1 d . . . H1A H 0.7870 0.0576 0.9881 0.052 Uiso 1 1 calc R . . H1B H 0.8172 -0.0474 0.9388 0.052 Uiso 1 1 calc R . . C2 C 0.9012(3) 0.0851(6) 1.0212(2) 0.0405(11) Uani 1 1 d . . . H2A H 0.9141 -0.0114 1.0560 0.049 Uiso 1 1 calc R . . H2B H 0.9364 0.0835 0.9983 0.049 Uiso 1 1 calc R . . C3 C 0.9075(2) 0.2544(6) 1.0599(2) 0.0304(9) Uani 1 1 d . . . H3 H 0.8718 0.2541 1.0831 0.037 Uiso 1 1 calc R . . C4 C 0.8875(2) 0.3991(6) 1.0065(2) 0.0287(8) Uani 1 1 d . . . H4A H 0.9240 0.4015 0.9849 0.034 Uiso 1 1 calc R . . H4B H 0.8919 0.5095 1.0322 0.034 Uiso 1 1 calc R . . C5 C 0.8078(2) 0.3842(6) 0.9456(2) 0.0303(9) Uani 1 1 d . . . H5 H 0.7729 0.3915 0.9694 0.036 Uiso 1 1 calc R . . C6 C 0.7888(3) 0.5379(7) 0.8938(2) 0.0397(11) Uani 1 1 d . . . H6A H 0.7337 0.5454 0.8668 0.048 Uiso 1 1 calc R . . H6B H 0.8061 0.6448 0.9225 0.048 Uiso 1 1 calc R . . C7 C 0.8235(3) 0.5289(6) 0.8398(2) 0.0356(10) Uani 1 1 d . . . H7 H 0.7996 0.6214 0.8032 0.043 Uiso 1 1 calc R . . C8 C 0.8052(2) 0.3557(6) 0.7997(2) 0.0284(9) Uani 1 1 d . . . H8 H 0.7495 0.3478 0.7725 0.034 Uiso 1 1 calc R . . C9 C 0.8312(2) 0.2041(5) 0.8535(2) 0.0245(8) Uani 1 1 d . . . H9 H 0.8859 0.2213 0.8841 0.029 Uiso 1 1 calc R . . C10 C 0.7915(2) 0.2084(6) 0.9055(2) 0.0323(10) Uani 1 1 d . . . C11 C 0.8229(2) 0.0278(6) 0.8149(2) 0.0299(9) Uani 1 1 d . . . H11A H 0.8493 -0.0610 0.8516 0.036 Uiso 1 1 calc R . . H11B H 0.7692 -0.0035 0.7920 0.036 Uiso 1 1 calc R . . C12 C 0.8533(2) 0.0239(5) 0.7572(2) 0.0261(8) Uani 1 1 d . . . H12 H 0.8369 -0.0872 0.7303 0.031 Uiso 1 1 calc R . . C13 C 0.8202(2) 0.1716(5) 0.70205(19) 0.0226(8) Uani 1 1 d . . . C14 C 0.8389(2) 0.3424(5) 0.74522(19) 0.0222(8) Uani 1 1 d . . . H14 H 0.8946 0.3453 0.7735 0.027 Uiso 1 1 calc R . . C15 C 0.8194(2) 0.4820(5) 0.6876(2) 0.0270(8) Uani 1 1 d . . . H15A H 0.8491 0.5877 0.7077 0.032 Uiso 1 1 calc R . . H15B H 0.7654 0.5112 0.6677 0.032 Uiso 1 1 calc R . . C16 C 0.8393(2) 0.4015(5) 0.6295(2) 0.0264(8) Uani 1 1 d . . . H16A H 0.8835 0.4598 0.6284 0.032 Uiso 1 1 calc R . . H16B H 0.7968 0.4131 0.5814 0.032 Uiso 1 1 calc R . . C17 C 0.8569(2) 0.2057(5) 0.64951(19) 0.0216(7) Uani 1 1 d . . . H17 H 0.9123 0.1967 0.6786 0.026 Uiso 1 1 calc R . . C18 C 0.7352(2) 0.1451(6) 0.6596(2) 0.0310(9) Uani 1 1 d . . . H18A H 0.7258 0.0361 0.6331 0.047 Uiso 1 1 calc R . . H18B H 0.7141 0.2404 0.6255 0.047 Uiso 1 1 calc R . . H18C H 0.7117 0.1421 0.6932 0.047 Uiso 1 1 calc R . . C19 C 0.7072(3) 0.1835(10) 0.8645(3) 0.0585(17) Uani 1 1 d . . . H19A H 0.6841 0.1857 0.8985 0.088 Uiso 1 1 calc R . . H19B H 0.6970 0.0723 0.8395 0.088 Uiso 1 1 calc R . . H19C H 0.6862 0.2764 0.8292 0.088 Uiso 1 1 calc R . . C20 C 0.8375(2) 0.0922(5) 0.58269(19) 0.0227(8) Uani 1 1 d . . . H20 H 0.7833 0.1101 0.5500 0.027 Uiso 1 1 calc R . . C21 C 0.8497(3) -0.1015(6) 0.6006(2) 0.0324(9) Uani 1 1 d . . . H21A H 0.8360 -0.1674 0.5559 0.049 Uiso 1 1 calc R . . H21B H 0.8184 -0.1381 0.6246 0.049 Uiso 1 1 calc R . . H21C H 0.9025 -0.1222 0.6326 0.049 Uiso 1 1 calc R . . C22 C 0.8843(2) 0.1539(5) 0.5427(2) 0.0257(8) Uani 1 1 d . . . H22A H 0.8712 0.2753 0.5278 0.031 Uiso 1 1 calc R . . H22B H 0.9380 0.1504 0.5765 0.031 Uiso 1 1 calc R . . C23 C 0.8727(2) 0.0477(6) 0.4767(2) 0.0309(9) Uani 1 1 d . . . H23A H 0.8976 -0.0651 0.4930 0.037 Uiso 1 1 calc R . . H23B H 0.8184 0.0254 0.4496 0.037 Uiso 1 1 calc R . . C24 C 0.9011(2) 0.1260(5) 0.4258(2) 0.0285(9) Uani 1 1 d . . . O3 O 0.98209(17) 0.2787(5) 1.11438(15) 0.0411(8) Uani 1 1 d . . . H3O H 0.9807 0.3345 1.1489 0.062 Uiso 1 1 calc R . . O7 O 0.90221(19) 0.5617(4) 0.87258(17) 0.0379(7) Uani 1 1 d D . . H7O H 0.9253 0.4694 0.8892 0.057 Uiso 1 1 calc R . . O12 O 0.93398(16) 0.0264(4) 0.78933(15) 0.0301(6) Uani 1 1 d . . . H12O H 0.954(3) 0.093(8) 0.828(3) 0.045 Uiso 1 1 d . . . O24 O 0.9239(2) 0.0354(4) 0.39046(18) 0.0417(8) Uani 1 1 d . . . O25 O 0.8979(2) 0.2925(4) 0.41988(18) 0.0379(8) Uani 1 1 d . . . H25O H 0.904(3) 0.341(8) 0.376(3) 0.057 Uiso 1 1 d . . . C1' C 1.0509(2) 0.3499(5) 0.7267(2) 0.0235(8) Uani 1 1 d . . . C2' C 1.0203(2) 0.6071(5) 0.7605(2) 0.0260(8) Uani 1 1 d . . . C3' C 1.0459(2) 0.5968(5) 0.6632(2) 0.0236(8) Uani 1 1 d . . . N1 N 1.05930(18) 0.4245(4) 0.67094(18) 0.0256(7) Uani 1 1 d . . . N2 N 1.0647(2) 0.1795(5) 0.7364(2) 0.0294(7) Uani 1 1 d . . . H2NA H 1.050(3) 0.139(7) 0.767(3) 0.035 Uiso 1 1 d . . . H2NB H 1.069(3) 0.130(7) 0.704(3) 0.035 Uiso 1 1 d . . . N3 N 1.03090(18) 0.4353(4) 0.77229(18) 0.0258(7) Uani 1 1 d . . . N4 N 1.0001(2) 0.6974(5) 0.8044(2) 0.0308(8) Uani 1 1 d . . . H4NA H 0.985(3) 0.810(8) 0.795(3) 0.037 Uiso 1 1 d . . . H4NB H 0.989(3) 0.643(7) 0.832(3) 0.037 Uiso 1 1 d . . . N5 N 1.02867(18) 0.6950(4) 0.70750(18) 0.0271(7) Uani 1 1 d . . . N6 N 1.0493(2) 0.6702(5) 0.6056(2) 0.0322(8) Uani 1 1 d . . . H6NA H 1.072(3) 0.616(7) 0.582(3) 0.039 Uiso 1 1 d . . . H6NB H 1.056(3) 0.783(8) 0.606(3) 0.039 Uiso 1 1 d . . . O6 O 1.0000 0.743(3) 1.0000 0.335(14) Uani 1 2 d SD . . H6O H 0.971(14) 0.666(5) 0.960(5) 0.402 Uiso 1 1 d 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 0.080(4) 0.029(2) 0.042(2) -0.0054(19) 0.046(3) -0.017(2) C2 0.069(3) 0.027(2) 0.034(2) 0.0059(18) 0.030(2) 0.008(2) C3 0.038(2) 0.034(2) 0.0266(19) 0.0024(17) 0.0208(18) 0.0055(18) C4 0.033(2) 0.029(2) 0.0275(18) -0.0067(17) 0.0160(16) 0.0006(17) C5 0.030(2) 0.039(2) 0.0294(19) 0.0010(18) 0.0196(16) 0.0053(18) C6 0.050(3) 0.039(3) 0.036(2) 0.003(2) 0.024(2) 0.022(2) C7 0.055(3) 0.024(2) 0.034(2) 0.0013(18) 0.024(2) 0.015(2) C8 0.031(2) 0.031(2) 0.0260(18) -0.0033(16) 0.0148(16) 0.0064(17) C9 0.0297(19) 0.0234(19) 0.0240(17) -0.0021(15) 0.0149(15) -0.0067(16) C10 0.030(2) 0.047(3) 0.0269(19) -0.0077(19) 0.0193(17) -0.011(2) C11 0.045(2) 0.024(2) 0.0264(18) -0.0029(17) 0.0207(18) -0.0089(18) C12 0.037(2) 0.0201(18) 0.0234(17) -0.0031(15) 0.0150(16) -0.0066(17) C13 0.0278(19) 0.0216(19) 0.0208(16) 0.0001(15) 0.0127(15) -0.0011(15) C14 0.0275(18) 0.0204(18) 0.0217(17) -0.0010(14) 0.0132(15) 0.0019(15) C15 0.035(2) 0.024(2) 0.0239(18) 0.0009(15) 0.0148(17) 0.0062(16) C16 0.033(2) 0.0240(19) 0.0263(18) 0.0050(16) 0.0165(16) 0.0047(17) C17 0.0247(17) 0.0194(18) 0.0208(16) 0.0025(14) 0.0099(14) -0.0001(15) C18 0.030(2) 0.039(2) 0.0272(18) -0.0036(17) 0.0150(16) -0.0046(18) C19 0.036(2) 0.104(5) 0.045(3) -0.031(3) 0.027(2) -0.028(3) C20 0.0279(18) 0.0236(18) 0.0200(16) -0.0007(14) 0.0136(15) -0.0013(15) C21 0.053(3) 0.022(2) 0.0271(19) -0.0015(16) 0.0220(19) -0.0016(19) C22 0.0278(19) 0.026(2) 0.0258(17) -0.0044(15) 0.0136(15) -0.0067(16) C23 0.045(2) 0.027(2) 0.0287(18) -0.0039(17) 0.0232(18) -0.0052(18) C24 0.035(2) 0.026(2) 0.031(2) -0.0029(16) 0.0201(18) -0.0031(17) O3 0.0404(18) 0.056(2) 0.0266(14) -0.0034(15) 0.0143(14) 0.0144(16) O7 0.061(2) 0.0222(16) 0.0423(17) -0.0056(13) 0.0333(16) -0.0057(14) O12 0.0398(16) 0.0260(15) 0.0254(13) 0.0017(12) 0.0146(12) 0.0050(13) O24 0.068(2) 0.0244(16) 0.0552(19) 0.0007(15) 0.0477(18) 0.0019(15) O25 0.069(2) 0.0204(15) 0.0438(18) 0.0030(13) 0.0431(18) 0.0049(14) C1' 0.0217(17) 0.024(2) 0.0263(18) 0.0000(15) 0.0114(15) -0.0018(15) C2' 0.0228(18) 0.028(2) 0.0280(19) -0.0038(16) 0.0115(16) -0.0020(16) C3' 0.0200(17) 0.0238(19) 0.0286(19) 0.0019(16) 0.0118(15) -0.0015(15) N1 0.0265(16) 0.0226(17) 0.0308(16) -0.0020(14) 0.0152(14) -0.0019(14) N2 0.042(2) 0.0233(18) 0.0317(18) 0.0013(15) 0.0237(16) 0.0014(15) N3 0.0245(16) 0.0253(17) 0.0304(16) 0.0019(14) 0.0143(14) 0.0020(13) N4 0.041(2) 0.0246(18) 0.0361(18) 0.0009(15) 0.0248(16) 0.0049(16) N5 0.0275(16) 0.0220(16) 0.0355(17) 0.0017(15) 0.0168(14) 0.0018(14) N6 0.042(2) 0.0247(19) 0.0413(19) 0.0018(16) 0.0285(17) -0.0005(16) O6 0.29(3) 0.28(3) 0.40(4) 0.000 0.11(3) 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C2 1.531(7) . ? C1 C10 1.556(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.512(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 O3 1.432(5) . ? C3 C4 1.499(6) . ? C3 H3 1.0000 . ? C4 C5 1.542(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.533(7) . ? C5 C10 1.554(6) . ? C5 H5 1.0000 . ? C6 C7 1.528(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O7 1.428(6) . ? C7 C8 1.536(6) . ? C7 H7 1.0000 . ? C8 C14 1.525(5) . ? C8 C9 1.543(6) . ? C8 H8 1.0000 . ? C9 C11 1.553(6) . ? C9 C10 1.566(5) . ? C9 H9 1.0000 . ? C10 C19 1.523(6) . ? C11 C12 1.536(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O12 1.440(5) . ? C12 C13 1.546(5) . ? C12 H12 1.0000 . ? C13 C18 1.540(5) . ? C13 C14 1.548(5) . ? C13 C17 1.552(5) . ? C14 C15 1.525(5) . ? C14 H14 1.0000 . ? C15 C16 1.536(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.574(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C20 1.533(5) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.542(6) . ? C20 C22 1.547(5) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.515(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.505(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O24 1.222(5) . ? C24 O25 1.296(5) . ? O3 H3O 0.8400 . ? O7 H7O 0.8400 . ? O12 H12O 0.89(6) . ? O25 H25O 1.02(6) . ? C1' N3 1.334(5) . ? C1' N2 1.348(5) . ? C1' N1 1.350(5) . ? C2' N4 1.327(5) . ? C2' N5 1.350(5) . ? C2' N3 1.355(5) . ? C3' N5 1.334(5) . ? C3' N6 1.338(5) . ? C3' N1 1.358(5) . ? N2 H2NA 0.86(5) . ? N2 H2NB 0.80(5) . ? N4 H4NA 0.92(6) . ? N4 H4NB 0.80(5) . ? N6 H6NA 0.88(5) . ? N6 H6NB 0.88(6) . ? O6 H6O 0.980(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C10 116.1(4) . . ? C2 C1 H1A 108.3 . . ? C10 C1 H1A 108.3 . . ? C2 C1 H1B 108.3 . . ? C10 C1 H1B 108.3 . . ? H1A C1 H1B 107.4 . . ? C3 C2 C1 108.9(4) . . ? C3 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? C3 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? O3 C3 C4 109.6(4) . . ? O3 C3 C2 110.6(4) . . ? C4 C3 C2 109.3(3) . . ? O3 C3 H3 109.1 . . ? C4 C3 H3 109.1 . . ? C2 C3 H3 109.1 . . ? C3 C4 C5 113.4(4) . . ? C3 C4 H4A 108.9 . . ? C5 C4 H4A 108.9 . . ? C3 C4 H4B 108.9 . . ? C5 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? C6 C5 C4 111.6(4) . . ? C6 C5 C10 112.5(3) . . ? C4 C5 C10 113.9(4) . . ? C6 C5 H5 106.1 . . ? C4 C5 H5 106.1 . . ? C10 C5 H5 106.1 . . ? C7 C6 C5 114.3(4) . . ? C7 C6 H6A 108.7 . . ? C5 C6 H6A 108.7 . . ? C7 C6 H6B 108.7 . . ? C5 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? O7 C7 C6 112.5(4) . . ? O7 C7 C8 111.7(3) . . ? C6 C7 C8 110.6(4) . . ? O7 C7 H7 107.3 . . ? C6 C7 H7 107.3 . . ? C8 C7 H7 107.3 . . ? C14 C8 C7 112.0(4) . . ? C14 C8 C9 110.7(3) . . ? C7 C8 C9 110.7(3) . . ? C14 C8 H8 107.8 . . ? C7 C8 H8 107.8 . . ? C9 C8 H8 107.8 . . ? C8 C9 C11 112.1(3) . . ? C8 C9 C10 111.0(3) . . ? C11 C9 C10 112.9(3) . . ? C8 C9 H9 106.8 . . ? C11 C9 H9 106.8 . . ? C10 C9 H9 106.8 . . ? C19 C10 C5 109.6(4) . . ? C19 C10 C1 107.1(4) . . ? C5 C10 C1 107.5(3) . . ? C19 C10 C9 111.5(3) . . ? C5 C10 C9 109.0(3) . . ? C1 C10 C9 112.0(4) . . ? C12 C11 C9 114.7(3) . . ? C12 C11 H11A 108.6 . . ? C9 C11 H11A 108.6 . . ? C12 C11 H11B 108.6 . . ? C9 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? O12 C12 C11 111.3(3) . . ? O12 C12 C13 111.5(3) . . ? C11 C12 C13 111.4(3) . . ? O12 C12 H12 107.4 . . ? C11 C12 H12 107.4 . . ? C13 C12 H12 107.4 . . ? C18 C13 C12 109.6(3) . . ? C18 C13 C14 112.0(3) . . ? C12 C13 C14 107.1(3) . . ? C18 C13 C17 110.3(3) . . ? C12 C13 C17 117.1(3) . . ? C14 C13 C17 100.5(3) . . ? C8 C14 C15 118.1(3) . . ? C8 C14 C13 113.8(3) . . ? C15 C14 C13 104.2(3) . . ? C8 C14 H14 106.7 . . ? C15 C14 H14 106.7 . . ? C13 C14 H14 106.7 . . ? C14 C15 C16 104.3(3) . . ? C14 C15 H15A 110.9 . . ? C16 C15 H15A 110.9 . . ? C14 C15 H15B 110.9 . . ? C16 C15 H15B 110.9 . . ? H15A C15 H15B 108.9 . . ? C15 C16 C17 106.9(3) . . ? C15 C16 H16A 110.3 . . ? C17 C16 H16A 110.3 . . ? C15 C16 H16B 110.3 . . ? C17 C16 H16B 110.3 . . ? H16A C16 H16B 108.6 . . ? C20 C17 C13 120.5(3) . . ? C20 C17 C16 112.2(3) . . ? C13 C17 C16 103.2(3) . . ? C20 C17 H17 106.7 . . ? C13 C17 H17 106.7 . . ? C16 C17 H17 106.7 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C10 C19 H19A 109.5 . . ? C10 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C10 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 C21 113.2(3) . . ? C17 C20 C22 108.4(3) . . ? C21 C20 C22 111.0(3) . . ? C17 C20 H20 108.0 . . ? C21 C20 H20 108.0 . . ? C22 C20 H20 108.0 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C20 113.9(3) . . ? C23 C22 H22A 108.8 . . ? C20 C22 H22A 108.8 . . ? C23 C22 H22B 108.8 . . ? C20 C22 H22B 108.8 . . ? H22A C22 H22B 107.7 . . ? C24 C23 C22 116.0(3) . . ? C24 C23 H23A 108.3 . . ? C22 C23 H23A 108.3 . . ? C24 C23 H23B 108.3 . . ? C22 C23 H23B 108.3 . . ? H23A C23 H23B 107.4 . . ? O24 C24 O25 122.3(4) . . ? O24 C24 C23 121.0(4) . . ? O25 C24 C23 116.7(4) . . ? C3 O3 H3O 109.5 . . ? C7 O7 H7O 109.5 . . ? C12 O12 H12O 114(3) . . ? C24 O25 H25O 116(4) . . ? N3 C1' N2 119.0(4) . . ? N3 C1' N1 123.9(4) . . ? N2 C1' N1 117.1(4) . . ? N4 C2' N5 116.9(4) . . ? N4 C2' N3 117.9(4) . . ? N5 C2' N3 125.3(4) . . ? N5 C3' N6 118.6(4) . . ? N5 C3' N1 125.2(4) . . ? N6 C3' N1 116.2(4) . . ? C1' N1 C3' 115.6(3) . . ? C1' N2 H2NA 111(3) . . ? C1' N2 H2NB 116(4) . . ? H2NA N2 H2NB 128(5) . . ? C1' N3 C2' 115.7(4) . . ? C2' N4 H4NA 121(3) . . ? C2' N4 H4NB 116(4) . . ? H4NA N4 H4NB 119(5) . . ? C3' N5 C2' 114.3(3) . . ? C3' N6 H6NA 120(3) . . ? C3' N6 H6NB 118(3) . . ? H6NA N6 H6NB 112(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 C1 C2 C3 58.4(5) . . . . ? C1 C2 C3 O3 180.0(3) . . . . ? C1 C2 C3 C4 -59.4(4) . . . . ? O3 C3 C4 C5 -179.9(3) . . . . ? C2 C3 C4 C5 58.8(5) . . . . ? C3 C4 C5 C6 178.0(3) . . . . ? C3 C4 C5 C10 -53.4(4) . . . . ? C4 C5 C6 C7 77.9(5) . . . . ? C10 C5 C6 C7 -51.5(5) . . . . ? C5 C6 C7 O7 -73.3(5) . . . . ? C5 C6 C7 C8 52.2(5) . . . . ? O7 C7 C8 C14 -54.0(4) . . . . ? C6 C7 C8 C14 180.0(3) . . . . ? O7 C7 C8 C9 70.1(4) . . . . ? C6 C7 C8 C9 -56.0(5) . . . . ? C14 C8 C9 C11 -47.9(4) . . . . ? C7 C8 C9 C11 -172.7(4) . . . . ? C14 C8 C9 C10 -175.2(3) . . . . ? C7 C8 C9 C10 60.0(4) . . . . ? C6 C5 C10 C19 -69.9(5) . . . . ? C4 C5 C10 C19 162.0(4) . . . . ? C6 C5 C10 C1 174.1(4) . . . . ? C4 C5 C10 C1 45.9(4) . . . . ? C6 C5 C10 C9 52.4(4) . . . . ? C4 C5 C10 C9 -75.7(4) . . . . ? C2 C1 C10 C19 -168.0(4) . . . . ? C2 C1 C10 C5 -50.3(5) . . . . ? C2 C1 C10 C9 69.5(5) . . . . ? C8 C9 C10 C19 63.9(5) . . . . ? C11 C9 C10 C19 -63.0(5) . . . . ? C8 C9 C10 C5 -57.3(4) . . . . ? C11 C9 C10 C5 175.9(3) . . . . ? C8 C9 C10 C1 -176.2(3) . . . . ? C11 C9 C10 C1 57.0(5) . . . . ? C8 C9 C11 C12 47.3(5) . . . . ? C10 C9 C11 C12 173.5(3) . . . . ? C9 C11 C12 O12 72.5(4) . . . . ? C9 C11 C12 C13 -52.7(4) . . . . ? O12 C12 C13 C18 170.0(3) . . . . ? C11 C12 C13 C18 -64.9(4) . . . . ? O12 C12 C13 C14 -68.3(4) . . . . ? C11 C12 C13 C14 56.8(4) . . . . ? O12 C12 C13 C17 43.5(4) . . . . ? C11 C12 C13 C17 168.6(3) . . . . ? C7 C8 C14 C15 -55.9(5) . . . . ? C9 C8 C14 C15 -179.9(3) . . . . ? C7 C8 C14 C13 -178.5(3) . . . . ? C9 C8 C14 C13 57.4(4) . . . . ? C18 C13 C14 C8 58.9(4) . . . . ? C12 C13 C14 C8 -61.2(4) . . . . ? C17 C13 C14 C8 176.0(3) . . . . ? C18 C13 C14 C15 -71.0(4) . . . . ? C12 C13 C14 C15 168.8(3) . . . . ? C17 C13 C14 C15 46.1(3) . . . . ? C8 C14 C15 C16 -161.9(3) . . . . ? C13 C14 C15 C16 -34.5(4) . . . . ? C14 C15 C16 C17 9.5(4) . . . . ? C18 C13 C17 C20 -46.5(5) . . . . ? C12 C13 C17 C20 79.7(4) . . . . ? C14 C13 C17 C20 -164.9(3) . . . . ? C18 C13 C17 C16 79.6(4) . . . . ? C12 C13 C17 C16 -154.2(3) . . . . ? C14 C13 C17 C16 -38.8(3) . . . . ? C15 C16 C17 C20 149.9(3) . . . . ? C15 C16 C17 C13 18.7(4) . . . . ? C13 C17 C20 C21 -54.7(5) . . . . ? C16 C17 C20 C21 -176.5(3) . . . . ? C13 C17 C20 C22 -178.3(3) . . . . ? C16 C17 C20 C22 59.9(4) . . . . ? C17 C20 C22 C23 177.8(3) . . . . ? C21 C20 C22 C23 52.9(4) . . . . ? C20 C22 C23 C24 165.3(4) . . . . ? C22 C23 C24 O24 149.0(4) . . . . ? C22 C23 C24 O25 -33.1(6) . . . . ? N3 C1' N1 C3' 0.0(5) . . . . ? N2 C1' N1 C3' -179.2(4) . . . . ? N5 C3' N1 C1' 2.9(6) . . . . ? N6 C3' N1 C1' -175.9(3) . . . . ? N2 C1' N3 C2' 178.0(4) . . . . ? N1 C1' N3 C2' -1.2(5) . . . . ? N4 C2' N3 C1' 179.9(3) . . . . ? N5 C2' N3 C1' -0.3(6) . . . . ? N6 C3' N5 C2' 174.6(3) . . . . ? N1 C3' N5 C2' -4.1(6) . . . . ? N4 C2' N5 C3' -177.4(3) . . . . ? N3 C2' N5 C3' 2.8(6) . . . . ? 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 O3 H3O N3 0.84 1.89 2.725(4) 172.1 2_757 O7 H7O O3 0.84 2.37 3.095(5) 144.2 2_757 O12 H12O O3 0.89(6) 1.95(6) 2.774(5) 154(5) 2_757 O25 H25O N1 1.02(6) 1.58(6) 2.559(4) 160(5) 2_756 N2 H2NA O12 0.86(5) 2.66(5) 3.406(5) 146(4) . N2 H2NB O24 0.80(5) 2.13(5) 2.922(5) 171(5) 2_756 N4 H4NA O12 0.92(6) 1.93(6) 2.823(5) 162(4) 1_565 N4 H4NB O7 0.80(5) 2.29(5) 3.011(5) 150(5) . N6 H6NA O25 0.88(5) 2.59(6) 3.226(5) 130(4) 2_756 N6 H6NB O24 0.88(6) 2.00(6) 2.877(5) 177(5) 2_766 O6 H6O O7 0.980(19) 1.906(17) 2.870(13) 167(7) . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.581 _refine_diff_density_min -0.436 _refine_diff_density_rms 0.059