# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2002 data_fro1818 _database_code_CSD 183052 _journal_coden_Cambridge 182 loop_ _publ_author_name 'Waldemar, Iwanek' 'Frohlich, Roland' 'Schwab, Pia' _publ_contact_author_name 'Dr Iwanek Waldemar' _publ_contact_author_address ; Institut of Organic Chemistry University of Tuebingen Auf der Morgenstelle 18 Tuebingen 72076 GERMANY ; _publ_contact_author_email 'WALDEMAR.IWANEK@UNI-TUEBINGEN.DE' _publ_requested_journal 'Chemical Communications' _publ_section_title ; The Diastereoselective Closure Ring of the Calixresorcin[4]arene. The Synthesis and Crystallographic Structures of Novel Bora-oxazino-oxazolidine Derivatives of Calixresorcin[4]arene ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C97 H126 B4 Cl6 N4 O14' _chemical_formula_weight 1827.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'trigonal' _symmetry_space_group_name_H-M 'P31' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' _cell_length_a 19.536(1) _cell_length_b 19.536(1) _cell_length_c 21.881(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 7232.2(6) _cell_formula_units_Z 3 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.259 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2910 _exptl_absorpt_coefficient_mu 0.242 _exptl_absorpt_correction_type 'SORTAV (Blessing, 1995 & 1997)' _exptl_absorpt_correction_T_min 0.9202 _exptl_absorpt_correction_T_max 0.9763 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35372 _diffrn_reflns_av_R_equivalents 0.0740 _diffrn_reflns_av_sigmaI/netI 0.1014 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 26.30 _reflns_number_total 15767 _reflns_number_gt 9689 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & MInor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1077P)^2^+3.9738P] 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 'refined as riding atoms' _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 0.13(10) _refine_ls_number_reflns 15767 _refine_ls_number_parameters 1140 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1345 _refine_ls_R_factor_gt 0.0779 _refine_ls_wR_factor_ref 0.2159 _refine_ls_wR_factor_gt 0.1827 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 B1A B -0.0191(4) 0.0204(4) 0.2217(3) 0.0389(16) Uani 1 1 d . . . O2A O -0.0036(2) -0.0405(2) 0.2024(2) 0.0479(10) Uani 1 1 d . . . C3A C 0.0584(4) -0.0382(4) 0.2372(3) 0.0567(18) Uani 1 1 d . . . H3A1 H 0.1073 -0.0158 0.2125 0.068 Uiso 1 1 calc R . . H3A2 H 0.0444 -0.0924 0.2498 0.068 Uiso 1 1 calc R . . C4A C 0.0719(4) 0.0133(3) 0.2940(3) 0.0442(15) Uani 1 1 d . . . H4A H 0.1213 0.0656 0.2894 0.053 Uiso 1 1 calc R . . N5A N 0.0007(3) 0.0238(3) 0.2944(2) 0.0388(11) Uani 1 1 d . . . C6A C 0.0145(3) 0.0974(3) 0.3259(3) 0.0394(14) Uani 1 1 d . . . H6A1 H 0.0392 0.1009 0.3662 0.047 Uiso 1 1 calc R . . H6A2 H -0.0370 0.0941 0.3333 0.047 Uiso 1 1 calc R . . C7A C 0.0667(3) 0.1715(3) 0.2900(3) 0.0301(12) Uani 1 1 d . . . C8A C 0.1012(3) 0.2440(3) 0.3198(2) 0.0296(12) Uani 1 1 d . . . C9A C 0.1453(3) 0.3149(3) 0.2872(2) 0.0279(12) Uani 1 1 d . . . C10A C 0.1578(3) 0.3073(3) 0.2261(3) 0.0324(12) Uani 1 1 d . . . H10A H 0.1917 0.3544 0.2043 0.039 Uiso 1 1 calc R . . C11A C 0.1252(3) 0.2371(3) 0.1940(2) 0.0304(12) Uani 1 1 d . . . C12A C 0.0769(3) 0.1686(3) 0.2276(2) 0.0316(12) Uani 1 1 d . . . O13A O 0.0436(2) 0.0980(2) 0.19688(17) 0.0371(9) Uani 1 1 d . . . C14A C 0.1373(3) 0.2340(3) 0.1253(2) 0.0308(12) Uani 1 1 d . . . H14A H 0.0937 0.1819 0.1105 0.037 Uiso 1 1 calc R . . C15A C 0.1289(3) 0.2986(4) 0.0913(3) 0.0405(14) Uani 1 1 d . . . H15A H 0.1325 0.2918 0.0468 0.049 Uiso 1 1 calc R . . H15B H 0.1736 0.3510 0.1028 0.049 Uiso 1 1 calc R . . C16A C 0.0505(4) 0.2972(4) 0.1049(3) 0.0545(17) Uani 1 1 d . . . H16A H 0.0509 0.3113 0.1488 0.065 Uiso 1 1 calc R . . C17A C 0.0473(5) 0.3602(5) 0.0660(5) 0.095(3) Uani 1 1 d . . . H17A H 0.0559 0.3526 0.0231 0.143 Uiso 1 1 calc R . . H17B H 0.0885 0.4126 0.0795 0.143 Uiso 1 1 calc R . . H17C H -0.0047 0.3558 0.0706 0.143 Uiso 1 1 calc R . . C18A C -0.0192(4) 0.2193(4) 0.0944(4) 0.069(2) Uani 1 1 d . . . H18A H -0.0671 0.2221 0.1021 0.103 Uiso 1 1 calc R . . H18B H -0.0177 0.1806 0.1222 0.103 Uiso 1 1 calc R . . H18C H -0.0192 0.2030 0.0521 0.103 Uiso 1 1 calc R . . O19A O 0.0872(2) 0.2421(2) 0.38125(16) 0.0353(9) Uani 1 1 d . . . H19A H 0.1257 0.2807 0.3983 0.053 Uiso 1 1 calc R . . C20A C -0.1053(4) 0.0032(4) 0.2065(3) 0.0478(16) Uani 1 1 d . . . C21A C -0.1604(4) -0.0672(4) 0.1801(4) 0.065(2) Uani 1 1 d . . . H21A H -0.1466 -0.1067 0.1730 0.078 Uiso 1 1 calc R . . C22A C -0.2364(5) -0.0826(6) 0.1633(4) 0.090(3) Uani 1 1 d . . . H22A H -0.2727 -0.1317 0.1450 0.108 Uiso 1 1 calc R . . C23A C -0.2577(5) -0.0267(7) 0.1734(5) 0.100(3) Uani 1 1 d . . . H23A H -0.3086 -0.0362 0.1619 0.120 Uiso 1 1 calc R . . C24A C -0.2053(5) 0.0427(6) 0.2003(5) 0.098(3) Uani 1 1 d . . . H24A H -0.2204 0.0809 0.2090 0.118 Uiso 1 1 calc R . . C25A C -0.1308(4) 0.0580(4) 0.2149(4) 0.070(2) Uani 1 1 d . . . H25A H -0.0946 0.1083 0.2315 0.084 Uiso 1 1 calc R . . C26A C 0.0714(4) -0.0245(5) 0.3553(3) 0.0610(19) Uani 1 1 d . . . H26A H 0.1088 0.0157 0.3844 0.073 Uiso 1 1 calc R . . H26B H 0.0862 -0.0658 0.3499 0.073 Uiso 1 1 calc R . . C27A C -0.0143(4) -0.0610(4) 0.3785(3) 0.0570(18) Uani 1 1 d . . . H27A H -0.0369 -0.1182 0.3863 0.068 Uiso 1 1 calc R . . H27B H -0.0158 -0.0351 0.4170 0.068 Uiso 1 1 calc R . . C28A C -0.0600(4) -0.0479(3) 0.3297(3) 0.0466(15) Uani 1 1 d . . . H28A H -0.1005 -0.0377 0.3478 0.056 Uiso 1 1 calc R . . H28B H -0.0866 -0.0946 0.3026 0.056 Uiso 1 1 calc R . . B1B B 0.4333(4) 0.1619(4) 0.0740(4) 0.0415(17) Uani 1 1 d . . . O2B O 0.4986(2) 0.1757(2) 0.1138(2) 0.0467(10) Uani 1 1 d . . . C3B C 0.4740(4) 0.1700(5) 0.1756(4) 0.068(2) Uani 1 1 d . . . H3B1 H 0.4891 0.2231 0.1917 0.082 Uiso 1 1 calc R . . H3B2 H 0.4997 0.1474 0.2011 0.082 Uiso 1 1 calc R . . C4B C 0.3818(4) 0.1151(4) 0.1777(3) 0.0528(17) Uani 1 1 d . . . H4B H 0.3562 0.1449 0.1936 0.063 Uiso 1 1 calc R . . N5B N 0.3602(3) 0.0931(3) 0.1125(2) 0.0411(12) Uani 1 1 d . . . C6B C 0.2823(3) 0.0846(3) 0.0959(4) 0.0517(17) Uani 1 1 d . . . H6B1 H 0.2415 0.0477 0.1248 0.062 Uiso 1 1 calc R . . H6B2 H 0.2672 0.0617 0.0544 0.062 Uiso 1 1 calc R . . C7B C 0.2848(3) 0.1630(3) 0.0975(3) 0.0351(13) Uani 1 1 d . . . C8B C 0.2154(3) 0.1644(3) 0.1107(3) 0.0336(12) Uani 1 1 d . . . C9B C 0.2148(3) 0.2359(3) 0.1116(2) 0.0302(12) Uani 1 1 d . . . C10B C 0.2860(3) 0.3037(3) 0.0991(2) 0.0323(12) Uani 1 1 d . . . H10B H 0.2863 0.3526 0.0992 0.039 Uiso 1 1 calc R . . C11B C 0.3561(3) 0.3059(3) 0.0867(2) 0.0289(12) Uani 1 1 d . . . C12B C 0.3544(3) 0.2336(3) 0.0866(3) 0.0365(13) Uani 1 1 d . . . O13B O 0.4235(2) 0.2333(2) 0.0766(2) 0.0425(10) Uani 1 1 d . . . C14B C 0.4330(3) 0.3837(3) 0.0743(2) 0.0328(12) Uani 1 1 d . . . H14B H 0.4678 0.3689 0.0511 0.039 Uiso 1 1 calc R . . C15B C 0.4218(4) 0.4402(3) 0.0333(3) 0.0398(14) Uani 1 1 d . . . H15C H 0.3832 0.4520 0.0530 0.048 Uiso 1 1 calc R . . H15D H 0.4727 0.4905 0.0308 0.048 Uiso 1 1 calc R . . C16B C 0.3938(4) 0.4116(4) -0.0309(3) 0.0515(16) Uani 1 1 d . . . H16B H 0.3414 0.3619 -0.0277 0.062 Uiso 1 1 calc R . . C17B C 0.4494(6) 0.3917(6) -0.0659(4) 0.094(3) Uani 1 1 d . . . H17D H 0.5026 0.4381 -0.0667 0.141 Uiso 1 1 calc R . . H17E H 0.4302 0.3764 -0.1078 0.141 Uiso 1 1 calc R . . H17F H 0.4511 0.3479 -0.0456 0.141 Uiso 1 1 calc R . . C18B C 0.3817(6) 0.4699(6) -0.0676(4) 0.092(3) Uani 1 1 d . . . H18D H 0.3422 0.4790 -0.0474 0.138 Uiso 1 1 calc R . . H18E H 0.3633 0.4488 -0.1087 0.138 Uiso 1 1 calc R . . H18F H 0.4319 0.5199 -0.0705 0.138 Uiso 1 1 calc R . . O19B O 0.1500(2) 0.09219(19) 0.12119(19) 0.0392(10) Uani 1 1 d . . . H19B H 0.1150 0.0984 0.1382 0.059 Uiso 1 1 calc R . . C20B C 0.4398(3) 0.1382(3) 0.0063(3) 0.0444(15) Uani 1 1 d . . . C21B C 0.3967(5) 0.1465(4) -0.0414(4) 0.065(2) Uani 1 1 d . . . H21B H 0.3649 0.1695 -0.0326 0.078 Uiso 1 1 calc R . . C22B C 0.3981(6) 0.1226(6) -0.1008(4) 0.094(3) Uani 1 1 d . . . H22B H 0.3659 0.1271 -0.1312 0.113 Uiso 1 1 calc R . . C23B C 0.4452(7) 0.0931(5) -0.1156(4) 0.090(3) Uani 1 1 d . . . H23B H 0.4461 0.0770 -0.1564 0.108 Uiso 1 1 calc R . . C24B C 0.4920(5) 0.0860(4) -0.0719(4) 0.073(2) Uani 1 1 d . . . H24B H 0.5264 0.0668 -0.0828 0.087 Uiso 1 1 calc R . . C25B C 0.4888(4) 0.1075(4) -0.0105(4) 0.0562(18) Uani 1 1 d . . . H25B H 0.5201 0.1011 0.0197 0.067 Uiso 1 1 calc R . . C26B C 0.3532(6) 0.0395(5) 0.2126(4) 0.092(3) Uani 1 1 d . . . H26C H 0.3942 0.0435 0.2413 0.111 Uiso 1 1 calc R . . H26D H 0.3046 0.0261 0.2358 0.111 Uiso 1 1 calc R . . C27B C 0.3369(14) -0.0207(7) 0.1639(6) 0.226(11) Uani 1 1 d . . . H27C H 0.3685 -0.0466 0.1722 0.271 Uiso 1 1 calc R . . H27D H 0.2804 -0.0618 0.1652 0.271 Uiso 1 1 calc R . . C28B C 0.3556(4) 0.0134(3) 0.1055(3) 0.0515(17) Uani 1 1 d . . . H28C H 0.3141 -0.0201 0.0757 0.062 Uiso 1 1 calc R . . H28D H 0.4068 0.0203 0.0913 0.062 Uiso 1 1 calc R . . B1C B 0.6636(4) 0.5192(4) 0.3238(3) 0.0418(16) Uani 1 1 d . . . O2C O 0.6467(2) 0.4947(2) 0.38602(19) 0.0479(10) Uani 1 1 d . . . C3C C 0.5937(4) 0.4130(4) 0.3903(3) 0.0607(19) Uani 1 1 d . . . H3C1 H 0.5407 0.4034 0.4021 0.073 Uiso 1 1 calc R . . H3C2 H 0.6120 0.3896 0.4220 0.073 Uiso 1 1 calc R . . C4C C 0.5893(3) 0.3750(3) 0.3288(3) 0.0510(17) Uani 1 1 d . . . H4C H 0.5381 0.3603 0.3081 0.061 Uiso 1 1 calc R . . N5C N 0.6573(3) 0.4387(3) 0.2933(2) 0.0379(11) Uani 1 1 d . . . C6C C 0.6464(3) 0.4334(4) 0.2260(3) 0.0460(15) Uani 1 1 d . . . H6C1 H 0.6357 0.3809 0.2118 0.055 Uiso 1 1 calc R . . H6C2 H 0.6956 0.4740 0.2061 0.055 Uiso 1 1 calc R . . C7C C 0.5785(3) 0.4456(3) 0.2074(3) 0.0354(13) Uani 1 1 d . . . C8C C 0.5365(3) 0.4087(3) 0.1542(3) 0.0317(12) Uani 1 1 d . . . C9C C 0.4766(3) 0.4214(3) 0.1330(3) 0.0315(12) Uani 1 1 d . . . C10C C 0.4580(3) 0.4680(3) 0.1695(2) 0.0310(12) Uani 1 1 d . . . H10C H 0.4158 0.4755 0.1566 0.037 Uiso 1 1 calc R . . C11C C 0.4965(3) 0.5046(3) 0.2235(2) 0.0296(12) Uani 1 1 d . . . C12C C 0.5589(3) 0.4928(3) 0.2423(2) 0.0307(12) Uani 1 1 d . . . O13C O 0.5962(2) 0.5246(2) 0.29531(18) 0.0380(9) Uani 1 1 d . . . C14C C 0.4723(3) 0.5546(3) 0.2609(2) 0.0304(12) Uani 1 1 d . . . H14C H 0.5195 0.5899 0.2864 0.036 Uiso 1 1 calc R . . C15C C 0.4545(3) 0.6098(3) 0.2236(3) 0.0375(13) Uani 1 1 d . . . H15E H 0.4135 0.5779 0.1930 0.045 Uiso 1 1 calc R . . H15F H 0.4321 0.6337 0.2513 0.045 Uiso 1 1 calc R . . C16C C 0.5249(4) 0.6760(4) 0.1904(4) 0.062(2) Uani 1 1 d . . . H16C H 0.5451 0.6506 0.1615 0.074 Uiso 1 1 calc R . . C17C C 0.4962(6) 0.7223(5) 0.1513(4) 0.086(3) Uani 1 1 d . . . H17G H 0.4494 0.6852 0.1280 0.128 Uiso 1 1 calc R . . H17H H 0.5383 0.7572 0.1231 0.128 Uiso 1 1 calc R . . H17I H 0.4827 0.7541 0.1781 0.128 Uiso 1 1 calc R . . C18C C 0.5913(5) 0.7281(5) 0.2310(5) 0.109(4) Uani 1 1 d . . . H18G H 0.6311 0.7733 0.2076 0.164 Uiso 1 1 calc R . . H18H H 0.6151 0.6984 0.2480 0.164 Uiso 1 1 calc R . . H18I H 0.5717 0.7471 0.2644 0.164 Uiso 1 1 calc R . . O19C O 0.5605(2) 0.3624(2) 0.12312(19) 0.0413(10) Uani 1 1 d . . . H19C H 0.5240 0.3310 0.0999 0.062 Uiso 1 1 calc R . . C20C C 0.7463(3) 0.5982(4) 0.3132(3) 0.0407(14) Uani 1 1 d . . . C21C C 0.8105(4) 0.6184(4) 0.3512(3) 0.0522(17) Uani 1 1 d . . . H21C H 0.8062 0.5837 0.3834 0.063 Uiso 1 1 calc R . . C22C C 0.8827(4) 0.6903(5) 0.3425(4) 0.069(2) Uani 1 1 d . . . H22C H 0.9267 0.7033 0.3682 0.083 Uiso 1 1 calc R . . C23C C 0.8885(4) 0.7406(4) 0.2972(5) 0.070(2) Uani 1 1 d . . . H23C H 0.9368 0.7890 0.2921 0.084 Uiso 1 1 calc R . . C24C C 0.8267(5) 0.7233(4) 0.2587(4) 0.072(2) Uani 1 1 d . . . H24C H 0.8315 0.7588 0.2272 0.086 Uiso 1 1 calc R . . C25C C 0.7552(4) 0.6507(4) 0.2674(3) 0.0530(17) Uani 1 1 d . . . H25C H 0.7120 0.6378 0.2407 0.064 Uiso 1 1 calc R . . C26C C 0.6034(4) 0.3044(4) 0.3289(4) 0.0607(19) Uani 1 1 d . . . H26E H 0.5733 0.2673 0.2955 0.073 Uiso 1 1 calc R . . H26F H 0.5865 0.2758 0.3683 0.073 Uiso 1 1 calc R . . C27C C 0.6926(4) 0.3393(4) 0.3193(4) 0.073(2) Uani 1 1 d . . . H27E H 0.7164 0.3285 0.3553 0.087 Uiso 1 1 calc R . . H27F H 0.7026 0.3157 0.2828 0.087 Uiso 1 1 calc R . . C28C C 0.7272(4) 0.4267(4) 0.3108(3) 0.0510(16) Uani 1 1 d . . . H28E H 0.7675 0.4464 0.2780 0.061 Uiso 1 1 calc R . . H28F H 0.7524 0.4552 0.3491 0.061 Uiso 1 1 calc R . . B1D B 0.2351(4) 0.3403(4) 0.4931(3) 0.0377(15) Uani 1 1 d . . . O2D O 0.1863(2) 0.2564(2) 0.49759(19) 0.0465(11) Uani 1 1 d . . . C3D C 0.2227(4) 0.2196(4) 0.4678(4) 0.0577(19) Uani 1 1 d . . . H3D1 H 0.1948 0.1958 0.4290 0.069 Uiso 1 1 calc R . . H3D2 H 0.2199 0.1768 0.4938 0.069 Uiso 1 1 calc R . . C4D C 0.3095(4) 0.2806(3) 0.4545(3) 0.0499(16) Uani 1 1 d . . . H4D H 0.3167 0.2953 0.4102 0.060 Uiso 1 1 calc R . . N5D N 0.3215(3) 0.3493(3) 0.4926(2) 0.0364(11) Uani 1 1 d . . . C6D C 0.3844(3) 0.4274(3) 0.4695(3) 0.0362(13) Uani 1 1 d . . . H6D1 H 0.4353 0.4279 0.4679 0.043 Uiso 1 1 calc R . . H6D2 H 0.3906 0.4695 0.4980 0.043 Uiso 1 1 calc R . . C7D C 0.3646(3) 0.4439(3) 0.4073(2) 0.0289(12) Uani 1 1 d . . . C8D C 0.4226(3) 0.4865(3) 0.3646(3) 0.0303(12) Uani 1 1 d . . . C9D C 0.4058(3) 0.5046(3) 0.3069(2) 0.0274(11) Uani 1 1 d . . . C10D C 0.3261(3) 0.4747(3) 0.2930(2) 0.0281(11) Uani 1 1 d . . . H10D H 0.3129 0.4853 0.2537 0.034 Uiso 1 1 calc R . . C11D C 0.2643(3) 0.4299(3) 0.3340(3) 0.0299(12) Uani 1 1 d . . . C12D C 0.2844(3) 0.4137(3) 0.3911(2) 0.0282(11) Uani 1 1 d . . . O13D O 0.2257(2) 0.3674(2) 0.43095(17) 0.0346(8) Uani 1 1 d . . . C14D C 0.1779(3) 0.3949(3) 0.3186(2) 0.0284(12) Uani 1 1 d . . . H14D H 0.1495 0.3843 0.3585 0.034 Uiso 1 1 calc R . . C15D C 0.1573(3) 0.4497(3) 0.2825(3) 0.0390(14) Uani 1 1 d . . . H15G H 0.1820 0.4588 0.2417 0.047 Uiso 1 1 calc R . . H15H H 0.0993 0.4220 0.2765 0.047 Uiso 1 1 calc R . . C16D C 0.1828(4) 0.5301(3) 0.3118(3) 0.0448(15) Uani 1 1 d . . . H16D H 0.2416 0.5627 0.3085 0.054 Uiso 1 1 calc R . . C17D C 0.1471(5) 0.5719(4) 0.2749(4) 0.077(2) Uani 1 1 d . . . H17J H 0.0893 0.5399 0.2758 0.116 Uiso 1 1 calc R . . H17K H 0.1655 0.5786 0.2325 0.116 Uiso 1 1 calc R . . H17L H 0.1638 0.6238 0.2930 0.116 Uiso 1 1 calc R . . C18D C 0.1613(5) 0.5254(4) 0.3778(4) 0.068(2) Uani 1 1 d . . . H18J H 0.1039 0.4921 0.3824 0.102 Uiso 1 1 calc R . . H18K H 0.1781 0.5786 0.3932 0.102 Uiso 1 1 calc R . . H18L H 0.1878 0.5024 0.4010 0.102 Uiso 1 1 calc R . . O19D O 0.4985(2) 0.5122(2) 0.38510(19) 0.0439(10) Uani 1 1 d . . . H19D H 0.5158 0.5559 0.4029 0.066 Uiso 1 1 calc R . . C20D C 0.2188(3) 0.3863(4) 0.5454(3) 0.0454(15) Uani 1 1 d . . . C21D C 0.1875(5) 0.3522(5) 0.6018(3) 0.072(2) Uani 1 1 d . . . H21D H 0.1767 0.2998 0.6093 0.086 Uiso 1 1 calc R . . C22D C 0.1714(6) 0.3910(8) 0.6473(4) 0.099(3) Uani 1 1 d . . . H22D H 0.1507 0.3663 0.6856 0.119 Uiso 1 1 calc R . . C23D C 0.1860(6) 0.4663(10) 0.6357(5) 0.112(4) Uani 1 1 d . . . H23D H 0.1747 0.4933 0.6667 0.135 Uiso 1 1 calc R . . C24D C 0.2165(5) 0.5043(5) 0.5808(5) 0.078(3) Uani 1 1 d . . . H24D H 0.2252 0.5560 0.5733 0.094 Uiso 1 1 calc R . . C25D C 0.2339(3) 0.4633(4) 0.5369(3) 0.0523(17) Uani 1 1 d . . . H25D H 0.2570 0.4892 0.4994 0.063 Uiso 1 1 calc R . . C26D C 0.3733(4) 0.2605(4) 0.4757(3) 0.0553(18) Uani 1 1 d . . . H26G H 0.3501 0.2027 0.4807 0.066 Uiso 1 1 calc R . . H26H H 0.4169 0.2796 0.4456 0.066 Uiso 1 1 calc R . . C27D C 0.4032(4) 0.3026(4) 0.5364(3) 0.0567(19) Uani 1 1 d . . . H27G H 0.4015 0.2656 0.5681 0.068 Uiso 1 1 calc R . . H27H H 0.4582 0.3468 0.5325 0.068 Uiso 1 1 calc R . . C28D C 0.3482(4) 0.3335(4) 0.5531(3) 0.0471(15) Uani 1 1 d . . . H28G H 0.3025 0.2938 0.5769 0.057 Uiso 1 1 calc R . . H28H H 0.3763 0.3827 0.5774 0.057 Uiso 1 1 calc R . . C101 C 0.2838(5) 0.2298(6) 0.2745(4) 0.089(3) Uani 1 1 d . . . H10E H 0.2627 0.2091 0.2332 0.107 Uiso 1 1 calc R . . H10F H 0.2487 0.2467 0.2937 0.107 Uiso 1 1 calc R . . Cl1 Cl 0.28243(16) 0.15522(14) 0.31765(14) 0.1047(8) Uani 1 1 d . . . Cl2 Cl 0.3757(2) 0.30920(18) 0.26751(18) 0.1472(13) Uani 1 1 d . . . C102 C 0.3860(6) 0.0397(9) 0.4213(7) 0.144(5) Uani 1 1 d . . . H10G H 0.4096 0.0475 0.4625 0.173 Uiso 1 1 calc R . . H10H H 0.3860 -0.0067 0.4031 0.173 Uiso 1 1 calc R . . Cl3 Cl 0.29115(17) 0.01664(18) 0.42988(17) 0.1280(11) Uani 1 1 d . . . Cl4 Cl 0.44520(18) 0.1183(2) 0.37940(19) 0.1439(14) Uani 1 1 d . . . C103 C 0.4046(11) 0.6577(7) 0.3993(5) 0.154(6) Uani 1 1 d . . . H10I H 0.4439 0.6446 0.3829 0.184 Uiso 1 1 calc R . . H10J H 0.3522 0.6091 0.3966 0.184 Uiso 1 1 calc R . . Cl5 Cl 0.4034(5) 0.7222(3) 0.3553(2) 0.256(4) Uani 1 1 d . . . Cl6 Cl 0.4242(6) 0.6793(5) 0.4706(2) 0.292(4) Uani 1 1 d . . . O201 O 0.8292(4) 0.4649(4) 0.4456(3) 0.100(2) Uani 1 1 d . . . H201 H 0.8195 0.4204 0.4327 0.150 Uiso 1 1 calc R . . C201 C 0.7720(6) 0.4547(7) 0.4915(5) 0.109(3) Uani 1 1 d . . . H20A H 0.7984 0.4720 0.5312 0.164 Uiso 1 1 calc R . . H20B H 0.7311 0.3988 0.4938 0.164 Uiso 1 1 calc R . . H20C H 0.7476 0.4864 0.4808 0.164 Uiso 1 1 calc R . . O202 O -0.4082(9) -0.0088(13) 0.0543(10) 0.330(13) Uani 1 1 d . . . H202 H -0.4413 -0.0574 0.0553 0.495 Uiso 1 1 calc R . . C202 C -0.398(2) 0.0201(14) 0.1087(7) 0.33(2) Uani 1 1 d . . . H20D H -0.3885 -0.0129 0.1371 0.500 Uiso 1 1 calc R . . H20E H -0.4458 0.0211 0.1214 0.500 Uiso 1 1 calc R . . H20F H -0.3529 0.0739 0.1089 0.500 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1A 0.041(4) 0.029(3) 0.040(4) -0.002(3) 0.002(3) 0.012(3) O2A 0.057(3) 0.039(2) 0.049(3) -0.0058(19) 0.007(2) 0.025(2) C3A 0.075(5) 0.051(4) 0.053(5) 0.011(3) 0.018(4) 0.038(4) C4A 0.040(3) 0.037(3) 0.049(4) 0.003(3) 0.004(3) 0.014(3) N5A 0.041(3) 0.027(2) 0.043(3) 0.004(2) 0.010(2) 0.013(2) C6A 0.043(3) 0.033(3) 0.034(3) -0.001(2) 0.008(3) 0.013(3) C7A 0.027(3) 0.022(3) 0.035(3) -0.001(2) -0.001(2) 0.007(2) C8A 0.027(3) 0.035(3) 0.030(3) -0.002(2) 0.002(2) 0.018(2) C9A 0.022(3) 0.029(3) 0.035(3) -0.002(2) -0.003(2) 0.015(2) C10A 0.030(3) 0.030(3) 0.038(3) 0.005(2) -0.001(2) 0.015(2) C11A 0.021(3) 0.033(3) 0.032(3) 0.000(2) -0.003(2) 0.009(2) C12A 0.025(3) 0.030(3) 0.032(3) 0.000(2) 0.002(2) 0.008(2) O13A 0.038(2) 0.0265(19) 0.034(2) -0.0014(17) 0.0046(17) 0.0069(17) C14A 0.027(3) 0.033(3) 0.030(3) 0.001(2) -0.003(2) 0.013(2) C15A 0.044(3) 0.052(4) 0.030(3) 0.006(3) 0.000(3) 0.028(3) C16A 0.050(4) 0.059(4) 0.058(5) 0.001(3) -0.015(3) 0.031(3) C17A 0.096(6) 0.089(6) 0.130(9) 0.030(6) -0.009(6) 0.069(5) C18A 0.050(4) 0.068(5) 0.088(6) 0.000(4) -0.016(4) 0.030(4) O19A 0.034(2) 0.031(2) 0.031(2) -0.0040(17) 0.0021(17) 0.0089(16) C20A 0.041(3) 0.043(4) 0.046(4) 0.006(3) 0.014(3) 0.010(3) C21A 0.049(4) 0.051(4) 0.070(5) -0.010(4) -0.003(4) 0.006(3) C22A 0.052(5) 0.081(6) 0.090(7) -0.005(5) -0.016(5) -0.001(5) C23A 0.051(5) 0.110(8) 0.123(9) 0.012(7) -0.010(5) 0.027(6) C24A 0.052(5) 0.085(6) 0.158(10) -0.015(6) -0.019(6) 0.035(5) C25A 0.047(4) 0.055(4) 0.102(7) -0.009(4) -0.013(4) 0.021(4) C26A 0.062(4) 0.069(5) 0.055(5) 0.005(4) -0.005(4) 0.034(4) C27A 0.071(5) 0.049(4) 0.048(4) 0.004(3) 0.001(4) 0.027(4) C28A 0.057(4) 0.029(3) 0.041(4) 0.005(3) 0.010(3) 0.011(3) B1B 0.025(3) 0.033(3) 0.063(5) -0.013(3) -0.003(3) 0.012(3) O2B 0.036(2) 0.045(2) 0.055(3) 0.000(2) -0.004(2) 0.0170(19) C3B 0.065(5) 0.068(5) 0.055(5) 0.002(4) -0.011(4) 0.021(4) C4B 0.067(4) 0.044(4) 0.052(4) 0.009(3) 0.016(4) 0.031(3) N5B 0.038(3) 0.030(2) 0.057(3) -0.004(2) 0.000(2) 0.019(2) C6B 0.037(3) 0.031(3) 0.084(5) -0.012(3) 0.004(3) 0.014(3) C7B 0.034(3) 0.023(3) 0.041(3) -0.008(2) 0.002(3) 0.009(2) C8B 0.034(3) 0.033(3) 0.028(3) -0.003(2) 0.003(2) 0.012(2) C9B 0.033(3) 0.029(3) 0.029(3) -0.002(2) -0.001(2) 0.015(2) C10B 0.043(3) 0.027(3) 0.027(3) -0.002(2) -0.004(2) 0.018(3) C11B 0.033(3) 0.024(3) 0.027(3) -0.006(2) -0.001(2) 0.013(2) C12B 0.039(3) 0.038(3) 0.034(3) 0.001(3) 0.007(3) 0.020(3) O13B 0.030(2) 0.030(2) 0.066(3) -0.0091(19) 0.0073(19) 0.0135(17) C14B 0.034(3) 0.031(3) 0.028(3) 0.000(2) 0.004(2) 0.013(2) C15B 0.045(3) 0.037(3) 0.039(4) 0.003(3) 0.003(3) 0.022(3) C16B 0.064(4) 0.044(4) 0.042(4) -0.002(3) -0.006(3) 0.023(3) C17B 0.141(8) 0.117(8) 0.054(5) 0.012(5) 0.017(5) 0.088(7) C18B 0.151(9) 0.108(7) 0.055(5) 0.004(5) -0.013(5) 0.092(7) O19B 0.028(2) 0.0235(19) 0.060(3) -0.0009(18) 0.0081(18) 0.0083(16) C20B 0.043(3) 0.035(3) 0.058(4) 0.000(3) 0.009(3) 0.022(3) C21B 0.080(5) 0.064(5) 0.061(5) -0.009(4) -0.004(4) 0.043(4) C22B 0.130(8) 0.098(7) 0.057(6) -0.009(5) -0.013(5) 0.059(7) C23B 0.118(8) 0.083(6) 0.060(6) -0.012(5) 0.014(6) 0.045(6) C24B 0.078(5) 0.065(5) 0.075(6) -0.009(4) 0.024(5) 0.036(4) C25B 0.056(4) 0.048(4) 0.066(5) 0.001(3) 0.011(3) 0.027(3) C26B 0.108(7) 0.071(6) 0.071(6) 0.019(5) 0.012(5) 0.025(5) C27B 0.52(3) 0.085(8) 0.100(10) 0.045(7) 0.102(15) 0.176(15) C28B 0.051(4) 0.030(3) 0.076(5) -0.005(3) 0.002(3) 0.022(3) B1C 0.039(4) 0.043(4) 0.044(4) -0.004(3) -0.003(3) 0.021(3) O2C 0.042(2) 0.059(3) 0.041(3) 0.006(2) -0.0015(19) 0.024(2) C3C 0.059(4) 0.053(4) 0.064(5) 0.020(4) 0.009(4) 0.023(4) C4C 0.033(3) 0.037(3) 0.073(5) 0.013(3) -0.005(3) 0.010(3) N5C 0.031(2) 0.040(3) 0.045(3) -0.002(2) 0.000(2) 0.020(2) C6C 0.035(3) 0.044(3) 0.062(5) -0.005(3) -0.004(3) 0.021(3) C7C 0.032(3) 0.028(3) 0.038(3) 0.002(3) 0.002(3) 0.009(2) C8C 0.026(3) 0.024(3) 0.040(3) -0.001(2) 0.008(2) 0.008(2) C9C 0.029(3) 0.025(3) 0.034(3) 0.006(2) 0.010(2) 0.008(2) C10C 0.026(3) 0.032(3) 0.035(3) 0.002(2) 0.006(2) 0.015(2) C11C 0.031(3) 0.026(3) 0.031(3) 0.004(2) 0.008(2) 0.014(2) C12C 0.023(3) 0.030(3) 0.031(3) -0.005(2) 0.001(2) 0.008(2) O13C 0.033(2) 0.043(2) 0.039(2) -0.0093(19) -0.0038(18) 0.0199(18) C14C 0.031(3) 0.025(3) 0.030(3) -0.001(2) 0.004(2) 0.010(2) C15C 0.040(3) 0.035(3) 0.034(3) 0.000(3) 0.003(3) 0.017(3) C16C 0.073(5) 0.048(4) 0.067(5) 0.016(4) 0.028(4) 0.032(4) C17C 0.106(6) 0.055(5) 0.076(6) 0.029(4) 0.010(5) 0.026(5) C18C 0.083(6) 0.053(5) 0.126(9) 0.033(5) -0.013(6) -0.016(5) O19C 0.036(2) 0.037(2) 0.050(3) -0.0129(18) 0.0017(19) 0.0175(19) C20C 0.038(3) 0.050(4) 0.041(4) -0.009(3) 0.002(3) 0.027(3) C21C 0.043(4) 0.054(4) 0.059(5) -0.014(3) -0.006(3) 0.024(3) C22C 0.031(4) 0.062(5) 0.100(7) -0.031(5) -0.001(4) 0.012(3) C23C 0.045(4) 0.039(4) 0.109(7) -0.015(5) 0.020(5) 0.009(3) C24C 0.083(6) 0.046(4) 0.087(6) 0.014(4) 0.045(5) 0.033(4) C25C 0.048(4) 0.045(4) 0.064(5) -0.002(3) 0.009(3) 0.022(3) C26C 0.069(5) 0.037(3) 0.069(5) 0.005(3) -0.016(4) 0.021(3) C27C 0.057(5) 0.051(4) 0.117(7) -0.001(4) -0.008(5) 0.033(4) C28C 0.043(3) 0.055(4) 0.060(4) 0.000(3) -0.006(3) 0.028(3) B1D 0.035(3) 0.040(4) 0.031(4) 0.002(3) 0.000(3) 0.013(3) O2D 0.035(2) 0.040(2) 0.049(3) 0.0052(19) -0.0016(19) 0.0071(19) C3D 0.048(4) 0.031(3) 0.084(5) -0.003(3) -0.008(4) 0.012(3) C4D 0.064(4) 0.040(3) 0.051(4) 0.001(3) -0.006(3) 0.029(3) N5D 0.039(3) 0.037(3) 0.027(3) 0.003(2) -0.006(2) 0.013(2) C6D 0.024(3) 0.036(3) 0.037(3) -0.005(3) -0.004(2) 0.007(2) C7D 0.028(3) 0.027(3) 0.032(3) 0.000(2) 0.003(2) 0.015(2) C8D 0.021(3) 0.027(3) 0.038(3) -0.003(2) -0.002(2) 0.008(2) C9D 0.026(3) 0.026(3) 0.026(3) -0.002(2) 0.007(2) 0.009(2) C10D 0.032(3) 0.025(3) 0.028(3) -0.003(2) 0.000(2) 0.015(2) C11D 0.031(3) 0.023(3) 0.037(3) -0.002(2) 0.001(2) 0.015(2) C12D 0.028(3) 0.025(3) 0.032(3) 0.001(2) 0.004(2) 0.013(2) O13D 0.0295(19) 0.041(2) 0.029(2) 0.0038(17) 0.0015(17) 0.0146(17) C14D 0.023(3) 0.021(2) 0.033(3) -0.003(2) -0.005(2) 0.005(2) C15D 0.036(3) 0.032(3) 0.049(4) 0.002(3) -0.005(3) 0.017(3) C16D 0.045(3) 0.032(3) 0.059(4) 0.003(3) -0.002(3) 0.020(3) C17D 0.091(6) 0.050(4) 0.108(7) 0.021(4) 0.005(5) 0.050(4) C18D 0.088(6) 0.050(4) 0.074(6) -0.002(4) 0.002(4) 0.042(4) O19D 0.029(2) 0.055(3) 0.040(3) -0.003(2) -0.0060(18) 0.0155(19) C20D 0.036(3) 0.055(4) 0.043(4) -0.002(3) -0.007(3) 0.022(3) C21D 0.076(5) 0.102(6) 0.036(4) 0.002(4) 0.016(4) 0.043(5) C22D 0.108(8) 0.136(9) 0.053(6) 0.002(6) 0.015(5) 0.060(8) C23D 0.083(7) 0.198(13) 0.067(7) -0.052(8) -0.003(5) 0.079(8) C24D 0.065(5) 0.090(6) 0.091(7) -0.044(5) -0.019(5) 0.049(5) C25D 0.036(3) 0.061(4) 0.054(4) -0.024(3) -0.009(3) 0.020(3) C26D 0.059(4) 0.048(4) 0.066(5) 0.005(3) -0.004(4) 0.032(3) C27D 0.052(4) 0.047(4) 0.072(5) 0.021(4) -0.010(3) 0.025(3) C28D 0.046(4) 0.051(4) 0.039(4) 0.011(3) -0.007(3) 0.021(3) C101 0.104(7) 0.135(8) 0.072(6) -0.011(5) -0.029(5) 0.092(7) Cl1 0.1021(18) 0.0787(15) 0.117(2) 0.0175(14) 0.0042(15) 0.0327(13) Cl2 0.130(3) 0.0874(18) 0.167(3) 0.041(2) 0.028(2) 0.0116(17) C102 0.086(7) 0.190(13) 0.173(14) 0.070(10) 0.026(8) 0.081(8) Cl3 0.0954(19) 0.110(2) 0.159(3) 0.0106(19) 0.0086(19) 0.0363(16) Cl4 0.0943(19) 0.134(2) 0.177(3) 0.067(2) -0.005(2) 0.0370(18) C103 0.299(19) 0.119(9) 0.093(9) -0.027(7) -0.043(10) 0.142(12) Cl5 0.526(11) 0.202(4) 0.146(4) 0.072(3) 0.128(5) 0.261(6) Cl6 0.539(13) 0.366(9) 0.118(4) -0.074(5) -0.129(6) 0.336(9) O201 0.145(6) 0.079(4) 0.093(5) 0.003(4) 0.002(4) 0.069(4) C201 0.107(8) 0.170(11) 0.081(7) -0.018(7) 0.000(6) 0.091(8) O202 0.222(14) 0.48(3) 0.34(2) -0.26(2) -0.113(15) 0.212(18) C202 0.82(6) 0.33(3) 0.065(10) 0.022(12) 0.044(19) 0.45(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1A O2A 1.431(8) . ? B1A O13A 1.495(7) . ? B1A C20A 1.579(9) . ? B1A N5A 1.631(9) . ? O2A C3A 1.413(8) . ? C3A C4A 1.536(9) . ? C4A N5A 1.502(8) . ? C4A C26A 1.531(9) . ? N5A C6A 1.494(7) . ? N5A C28A 1.518(7) . ? C6A C7A 1.509(7) . ? C7A C12A 1.385(7) . ? C7A C8A 1.389(7) . ? C8A O19A 1.370(6) . ? C8A C9A 1.405(7) . ? C9A C10A 1.380(7) . ? C9A C14D 1.525(7) . ? C10A C11A 1.380(7) . ? C11A C12A 1.400(7) . ? C11A C14A 1.527(8) . ? C12A O13A 1.370(6) . ? C14A C9B 1.526(7) . ? C14A C15A 1.542(8) . ? C15A C16A 1.547(9) . ? C16A C18A 1.466(9) . ? C16A C17A 1.523(10) . ? C20A C21A 1.380(9) . ? C20A C25A 1.400(10) . ? C21A C22A 1.408(12) . ? C22A C23A 1.369(14) . ? C23A C24A 1.357(13) . ? C24A C25A 1.370(11) . ? C26A C27A 1.541(10) . ? C27A C28A 1.496(9) . ? B1B O2B 1.455(8) . ? B1B O13B 1.501(7) . ? B1B C20B 1.576(10) . ? B1B N5B 1.623(8) . ? O2B C3B 1.422(8) . ? C3B C4B 1.571(10) . ? C4B N5B 1.489(9) . ? C4B C26B 1.500(10) . ? N5B C6B 1.490(7) . ? N5B C28B 1.522(7) . ? C6B C7B 1.507(8) . ? C7B C12B 1.390(7) . ? C7B C8B 1.401(8) . ? C8B O19B 1.368(6) . ? C8B C9B 1.402(7) . ? C9B C10B 1.386(7) . ? C10B C11B 1.376(7) . ? C11B C12B 1.397(7) . ? C11B C14B 1.535(7) . ? C12B O13B 1.370(7) . ? C14B C9C 1.513(8) . ? C14B C15B 1.522(8) . ? C15B C16B 1.509(9) . ? C16B C18B 1.506(10) . ? C16B C17B 1.531(11) . ? C20B C21B 1.399(10) . ? C20B C25B 1.409(8) . ? C21B C22B 1.387(11) . ? C22B C23B 1.346(13) . ? C23B C24B 1.378(13) . ? C24B C25B 1.418(11) . ? C26B C27B 1.498(14) . ? C27B C28B 1.404(12) . ? B1C O2C 1.425(8) . ? B1C O13C 1.507(8) . ? B1C C20C 1.598(9) . ? B1C N5C 1.654(8) . ? O2C C3C 1.405(8) . ? C3C C4C 1.518(10) . ? C4C N5C 1.505(7) . ? C4C C26C 1.534(9) . ? N5C C6C 1.483(8) . ? N5C C28C 1.546(7) . ? C6C C7C 1.515(8) . ? C7C C12C 1.390(8) . ? C7C C8C 1.398(8) . ? C8C O19C 1.388(6) . ? C8C C9C 1.392(8) . ? C9C C10C 1.389(7) . ? C10C C11C 1.391(7) . ? C11C C12C 1.409(7) . ? C11C C14C 1.521(7) . ? C12C O13C 1.346(6) . ? C14C C15C 1.525(8) . ? C14C C9D 1.544(7) . ? C15C C16C 1.521(9) . ? C16C C18C 1.479(12) . ? C16C C17C 1.539(11) . ? C20C C25C 1.382(9) . ? C20C C21C 1.388(9) . ? C21C C22C 1.420(10) . ? C22C C23C 1.360(12) . ? C23C C24C 1.368(12) . ? C24C C25C 1.420(10) . ? C26C C27C 1.536(10) . ? C27C C28C 1.500(9) . ? B1D O2D 1.430(8) . ? B1D O13D 1.502(7) . ? B1D C20D 1.582(10) . ? B1D N5D 1.608(8) . ? O2D C3D 1.400(8) . ? C3D C4D 1.537(9) . ? C4D N5D 1.495(8) . ? C4D C26D 1.553(9) . ? N5D C6D 1.489(7) . ? N5D C28D 1.509(7) . ? C6D C7D 1.495(8) . ? C7D C8D 1.381(7) . ? C7D C12D 1.415(7) . ? C8D O19D 1.382(6) . ? C8D C9D 1.393(7) . ? C9D C10D 1.396(7) . ? C10D C11D 1.405(7) . ? C11D C12D 1.394(7) . ? C11D C14D 1.508(7) . ? C12D O13D 1.363(6) . ? C14D C15D 1.538(7) . ? C15D C16D 1.529(8) . ? C16D C18D 1.494(10) . ? C16D C17D 1.541(9) . ? C20D C21D 1.390(10) . ? C20D C25D 1.394(9) . ? C21D C22D 1.380(13) . ? C22D C23D 1.376(16) . ? C23D C24D 1.380(15) . ? C24D C25D 1.398(10) . ? C26D C27D 1.518(10) . ? C27D C28D 1.516(9) . ? C101 Cl2 1.694(10) . ? C101 Cl1 1.726(9) . ? C102 Cl4 1.662(12) . ? C102 Cl3 1.684(10) . ? C103 Cl5 1.595(12) . ? C103 Cl6 1.612(12) . ? O201 C201 1.440(11) . ? O202 C202 1.29(2) . ? 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 O2A B1A O13A 109.3(5) . . ? O2A B1A C20A 114.1(5) . . ? O13A B1A C20A 112.7(5) . . ? O2A B1A N5A 100.1(5) . . ? O13A B1A N5A 104.8(4) . . ? C20A B1A N5A 114.8(5) . . ? C3A O2A B1A 110.5(5) . . ? O2A C3A C4A 108.6(5) . . ? N5A C4A C26A 106.2(5) . . ? N5A C4A C3A 103.1(5) . . ? C26A C4A C3A 115.7(5) . . ? C6A N5A C4A 113.6(4) . . ? C6A N5A C28A 109.5(4) . . ? C4A N5A C28A 103.2(4) . . ? C6A N5A B1A 114.5(4) . . ? C4A N5A B1A 101.9(4) . . ? C28A N5A B1A 113.5(4) . . ? N5A C6A C7A 113.1(4) . . ? C12A C7A C8A 119.9(5) . . ? C12A C7A C6A 121.1(4) . . ? C8A C7A C6A 119.0(5) . . ? O19A C8A C7A 116.4(4) . . ? O19A C8A C9A 122.7(4) . . ? C7A C8A C9A 120.8(5) . . ? C10A C9A C8A 116.1(5) . . ? C10A C9A C14D 122.7(5) . . ? C8A C9A C14D 121.2(5) . . ? C9A C10A C11A 125.5(5) . . ? C10A C11A C12A 116.0(5) . . ? C10A C11A C14A 122.4(5) . . ? C12A C11A C14A 121.5(5) . . ? O13A C12A C7A 121.3(4) . . ? O13A C12A C11A 117.3(5) . . ? C7A C12A C11A 121.3(5) . . ? C12A O13A B1A 125.3(4) . . ? C9B C14A C11A 111.3(4) . . ? C9B C14A C15A 113.3(4) . . ? C11A C14A C15A 111.2(4) . . ? C14A C15A C16A 113.7(5) . . ? C18A C16A C17A 111.1(6) . . ? C18A C16A C15A 112.7(6) . . ? C17A C16A C15A 108.6(6) . . ? C21A C20A C25A 114.8(6) . . ? C21A C20A B1A 121.2(6) . . ? C25A C20A B1A 123.9(6) . . ? C20A C21A C22A 122.4(8) . . ? C23A C22A C21A 119.7(8) . . ? C24A C23A C22A 119.2(9) . . ? C23A C24A C25A 120.6(9) . . ? C24A C25A C20A 123.2(8) . . ? C4A C26A C27A 104.7(5) . . ? C28A C27A C26A 106.8(5) . . ? C27A C28A N5A 105.2(5) . . ? O2B B1B O13B 108.2(5) . . ? O2B B1B C20B 115.1(5) . . ? O13B B1B C20B 112.0(5) . . ? O2B B1B N5B 99.8(5) . . ? O13B B1B N5B 106.4(4) . . ? C20B B1B N5B 114.2(5) . . ? C3B O2B B1B 108.9(5) . . ? O2B C3B C4B 108.0(5) . . ? N5B C4B C26B 106.9(6) . . ? N5B C4B C3B 103.4(5) . . ? C26B C4B C3B 114.9(7) . . ? C4B N5B C6B 113.0(5) . . ? C4B N5B C28B 104.8(5) . . ? C6B N5B C28B 109.1(4) . . ? C4B N5B B1B 104.6(4) . . ? C6B N5B B1B 113.1(5) . . ? C28B N5B B1B 111.9(4) . . ? N5B C6B C7B 111.6(5) . . ? C12B C7B C8B 119.4(5) . . ? C12B C7B C6B 121.6(5) . . ? C8B C7B C6B 119.0(5) . . ? O19B C8B C7B 115.3(5) . . ? O19B C8B C9B 123.8(5) . . ? C7B C8B C9B 120.9(5) . . ? C10B C9B C8B 116.5(5) . . ? C10B C9B C14A 124.7(5) . . ? C8B C9B C14A 118.8(5) . . ? C11B C10B C9B 125.1(5) . . ? C10B C11B C12B 116.7(5) . . ? C10B C11B C14B 122.2(4) . . ? C12B C11B C14B 121.1(5) . . ? O13B C12B C7B 120.0(5) . . ? O13B C12B C11B 118.6(5) . . ? C7B C12B C11B 121.4(5) . . ? C12B O13B B1B 126.4(4) . . ? C9C C14B C15B 113.4(4) . . ? C9C C14B C11B 111.5(4) . . ? C15B C14B C11B 113.4(4) . . ? C16B C15B C14B 115.9(5) . . ? C18B C16B C15B 112.3(6) . . ? C18B C16B C17B 108.9(7) . . ? C15B C16B C17B 112.8(6) . . ? C21B C20B C25B 115.5(6) . . ? C21B C20B B1B 121.7(5) . . ? C25B C20B B1B 122.8(6) . . ? C22B C21B C20B 123.1(7) . . ? C23B C22B C21B 120.2(9) . . ? C22B C23B C24B 120.4(9) . . ? C23B C24B C25B 119.9(8) . . ? C20B C25B C24B 120.9(7) . . ? C27B C26B C4B 103.9(7) . . ? C28B C27B C26B 111.8(7) . . ? C27B C28B N5B 105.2(6) . . ? O2C B1C O13C 110.8(5) . . ? O2C B1C C20C 114.6(5) . . ? O13C B1C C20C 111.6(5) . . ? O2C B1C N5C 99.9(5) . . ? O13C B1C N5C 104.2(4) . . ? C20C B1C N5C 114.8(5) . . ? C3C O2C B1C 111.1(5) . . ? O2C C3C C4C 109.0(5) . . ? N5C C4C C3C 104.0(5) . . ? N5C C4C C26C 105.3(5) . . ? C3C C4C C26C 116.5(6) . . ? C6C N5C C4C 114.7(5) . . ? C6C N5C C28C 110.1(4) . . ? C4C N5C C28C 103.1(4) . . ? C6C N5C B1C 114.0(4) . . ? C4C N5C B1C 101.1(4) . . ? C28C N5C B1C 113.1(4) . . ? N5C C6C C7C 111.3(5) . . ? C12C C7C C8C 120.9(5) . . ? C12C C7C C6C 120.6(5) . . ? C8C C7C C6C 118.5(5) . . ? O19C C8C C9C 122.7(5) . . ? O19C C8C C7C 116.2(5) . . ? C9C C8C C7C 121.0(5) . . ? C10C C9C C8C 116.4(5) . . ? C10C C9C C14B 122.6(5) . . ? C8C C9C C14B 121.0(5) . . ? C9C C10C C11C 124.9(5) . . ? C10C C11C C12C 117.1(5) . . ? C10C C11C C14C 121.6(5) . . ? C12C C11C C14C 121.3(5) . . ? O13C C12C C7C 120.9(5) . . ? O13C C12C C11C 119.4(5) . . ? C7C C12C C11C 119.7(5) . . ? C12C O13C B1C 128.0(4) . . ? C11C C14C C15C 114.8(5) . . ? C11C C14C C9D 112.2(4) . . ? C15C C14C C9D 112.3(4) . . ? C16C C15C C14C 115.4(5) . . ? C18C C16C C15C 114.0(7) . . ? C18C C16C C17C 112.4(7) . . ? C15C C16C C17C 109.0(6) . . ? C25C C20C C21C 117.6(6) . . ? C25C C20C B1C 120.9(5) . . ? C21C C20C B1C 121.4(6) . . ? C20C C21C C22C 120.6(7) . . ? C23C C22C C21C 119.8(7) . . ? C22C C23C C24C 121.6(7) . . ? C23C C24C C25C 118.1(8) . . ? C20C C25C C24C 122.2(7) . . ? C4C C26C C27C 106.0(5) . . ? C28C C27C C26C 106.7(5) . . ? C27C C28C N5C 105.9(5) . . ? O2D B1D O13D 109.7(5) . . ? O2D B1D C20D 113.1(5) . . ? O13D B1D C20D 111.2(5) . . ? O2D B1D N5D 100.8(5) . . ? O13D B1D N5D 105.2(4) . . ? C20D B1D N5D 116.1(5) . . ? C3D O2D B1D 109.8(5) . . ? O2D C3D C4D 109.7(5) . . ? N5D C4D C3D 102.0(5) . . ? N5D C4D C26D 106.0(5) . . ? C3D C4D C26D 117.4(5) . . ? C6D N5D C4D 114.1(5) . . ? C6D N5D C28D 108.3(4) . . ? C4D N5D C28D 102.8(4) . . ? C6D N5D B1D 113.4(4) . . ? C4D N5D B1D 102.8(4) . . ? C28D N5D B1D 115.0(4) . . ? N5D C6D C7D 111.1(4) . . ? C8D C7D C12D 119.1(5) . . ? C8D C7D C6D 121.6(5) . . ? C12D C7D C6D 119.3(4) . . ? C7D C8D O19D 114.0(5) . . ? C7D C8D C9D 122.6(4) . . ? O19D C8D C9D 123.3(4) . . ? C8D C9D C10D 116.5(4) . . ? C8D C9D C14C 121.3(4) . . ? C10D C9D C14C 122.2(5) . . ? C9D C10D C11D 123.6(5) . . ? C12D C11D C10D 117.5(5) . . ? C12D C11D C14D 118.5(5) . . ? C10D C11D C14D 123.9(5) . . ? O13D C12D C11D 118.9(4) . . ? O13D C12D C7D 120.4(5) . . ? C11D C12D C7D 120.6(5) . . ? C12D O13D B1D 127.0(4) . . ? C11D C14D C9A 111.5(4) . . ? C11D C14D C15D 114.9(4) . . ? C9A C14D C15D 111.2(4) . . ? C16D C15D C14D 115.9(5) . . ? C18D C16D C15D 113.8(5) . . ? C18D C16D C17D 110.6(6) . . ? C15D C16D C17D 108.9(6) . . ? C21D C20D C25D 116.1(7) . . ? C21D C20D B1D 122.4(6) . . ? C25D C20D B1D 121.4(6) . . ? C22D C21D C20D 123.0(9) . . ? C23D C22D C21D 118.2(9) . . ? C22D C23D C24D 122.6(9) . . ? C23D C24D C25D 116.9(9) . . ? C20D C25D C24D 123.1(7) . . ? C27D C26D C4D 105.2(5) . . ? C28D C27D C26D 105.6(5) . . ? N5D C28D C27D 104.8(5) . . ? Cl2 C101 Cl1 112.6(4) . . ? Cl4 C102 Cl3 118.2(7) . . ? Cl5 C103 Cl6 118.2(7) . . ? 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 O13A B1A O2A C3A 76.5(6) . . . . ? C20A B1A O2A C3A -156.4(5) . . . . ? N5A B1A O2A C3A -33.2(6) . . . . ? B1A O2A C3A C4A 15.1(7) . . . . ? O2A C3A C4A N5A 12.2(6) . . . . ? O2A C3A C4A C26A 127.6(6) . . . . ? C26A C4A N5A C6A 83.7(6) . . . . ? C3A C4A N5A C6A -154.2(5) . . . . ? C26A C4A N5A C28A -34.8(6) . . . . ? C3A C4A N5A C28A 87.3(5) . . . . ? C26A C4A N5A B1A -152.6(5) . . . . ? C3A C4A N5A B1A -30.5(5) . . . . ? O2A B1A N5A C6A 162.3(4) . . . . ? O13A B1A N5A C6A 49.1(6) . . . . ? C20A B1A N5A C6A -75.1(6) . . . . ? O2A B1A N5A C4A 39.2(5) . . . . ? O13A B1A N5A C4A -73.9(5) . . . . ? C20A B1A N5A C4A 161.8(5) . . . . ? O2A B1A N5A C28A -71.0(5) . . . . ? O13A B1A N5A C28A 175.8(4) . . . . ? C20A B1A N5A C28A 51.6(6) . . . . ? C4A N5A C6A C7A 72.2(6) . . . . ? C28A N5A C6A C7A -173.0(5) . . . . ? B1A N5A C6A C7A -44.3(6) . . . . ? N5A C6A C7A C12A 20.5(7) . . . . ? N5A C6A C7A C8A -163.2(5) . . . . ? C12A C7A C8A O19A 178.7(5) . . . . ? C6A C7A C8A O19A 2.4(7) . . . . ? C12A C7A C8A C9A 1.2(8) . . . . ? C6A C7A C8A C9A -175.1(5) . . . . ? O19A C8A C9A C10A 176.9(4) . . . . ? C7A C8A C9A C10A -5.7(7) . . . . ? O19A C8A C9A C14D -2.2(7) . . . . ? C7A C8A C9A C14D 175.2(5) . . . . ? C8A C9A C10A C11A 5.9(7) . . . . ? C14D C9A C10A C11A -175.0(5) . . . . ? C9A C10A C11A C12A -1.3(7) . . . . ? C9A C10A C11A C14A 175.6(5) . . . . ? C8A C7A C12A O13A -179.9(5) . . . . ? C6A C7A C12A O13A -3.7(8) . . . . ? C8A C7A C12A C11A 3.8(8) . . . . ? C6A C7A C12A C11A 180.0(5) . . . . ? C10A C11A C12A O13A 179.8(4) . . . . ? C14A C11A C12A O13A 2.9(7) . . . . ? C10A C11A C12A C7A -3.7(7) . . . . ? C14A C11A C12A C7A 179.3(5) . . . . ? C7A C12A O13A B1A 13.7(8) . . . . ? C11A C12A O13A B1A -169.9(5) . . . . ? O2A B1A O13A C12A -141.0(5) . . . . ? C20A B1A O13A C12A 91.1(7) . . . . ? N5A B1A O13A C12A -34.5(7) . . . . ? C10A C11A C14A C9B 84.4(6) . . . . ? C12A C11A C14A C9B -98.9(5) . . . . ? C10A C11A C14A C15A -43.0(6) . . . . ? C12A C11A C14A C15A 133.8(5) . . . . ? C9B C14A C15A C16A 180.0(5) . . . . ? C11A C14A C15A C16A -53.7(6) . . . . ? C14A C15A C16A C18A -53.3(8) . . . . ? C14A C15A C16A C17A -176.8(6) . . . . ? O2A B1A C20A C21A 3.4(9) . . . . ? O13A B1A C20A C21A 128.7(6) . . . . ? N5A B1A C20A C21A -111.4(7) . . . . ? O2A B1A C20A C25A -172.6(7) . . . . ? O13A B1A C20A C25A -47.2(9) . . . . ? N5A B1A C20A C25A 72.7(8) . . . . ? C25A C20A C21A C22A -0.4(11) . . . . ? B1A C20A C21A C22A -176.7(7) . . . . ? C20A C21A C22A C23A -0.3(13) . . . . ? C21A C22A C23A C24A -0.7(15) . . . . ? C22A C23A C24A C25A 2.5(17) . . . . ? C23A C24A C25A C20A -3.5(16) . . . . ? C21A C20A C25A C24A 2.3(12) . . . . ? B1A C20A C25A C24A 178.5(8) . . . . ? N5A C4A C26A C27A 19.6(7) . . . . ? C3A C4A C26A C27A -94.1(7) . . . . ? C4A C26A C27A C28A 3.4(7) . . . . ? C26A C27A C28A N5A -24.9(7) . . . . ? C6A N5A C28A C27A -84.4(6) . . . . ? C4A N5A C28A C27A 36.9(6) . . . . ? B1A N5A C28A C27A 146.3(5) . . . . ? O13B B1B O2B C3B 73.2(6) . . . . ? C20B B1B O2B C3B -160.6(5) . . . . ? N5B B1B O2B C3B -37.8(6) . . . . ? B1B O2B C3B C4B 25.8(7) . . . . ? O2B C3B C4B N5B -0.4(7) . . . . ? O2B C3B C4B C26B 115.8(7) . . . . ? C26B C4B N5B C6B 92.8(7) . . . . ? C3B C4B N5B C6B -145.4(5) . . . . ? C26B C4B N5B C28B -25.8(7) . . . . ? C3B C4B N5B C28B 95.9(5) . . . . ? C26B C4B N5B B1B -143.6(6) . . . . ? C3B C4B N5B B1B -21.9(6) . . . . ? O2B B1B N5B C4B 36.6(5) . . . . ? O13B B1B N5B C4B -75.9(5) . . . . ? C20B B1B N5B C4B 160.0(5) . . . . ? O2B B1B N5B C6B 160.0(4) . . . . ? O13B B1B N5B C6B 47.6(6) . . . . ? C20B B1B N5B C6B -76.6(6) . . . . ? O2B B1B N5B C28B -76.3(6) . . . . ? O13B B1B N5B C28B 171.2(5) . . . . ? C20B B1B N5B C28B 47.1(7) . . . . ? C4B N5B C6B C7B 68.1(7) . . . . ? C28B N5B C6B C7B -175.8(5) . . . . ? B1B N5B C6B C7B -50.6(7) . . . . ? N5B C6B C7B C12B 28.2(9) . . . . ? N5B C6B C7B C8B -151.4(5) . . . . ? C12B C7B C8B O19B -179.7(5) . . . . ? C6B C7B C8B O19B 0.0(8) . . . . ? C12B C7B C8B C9B 1.5(8) . . . . ? C6B C7B C8B C9B -178.8(5) . . . . ? O19B C8B C9B C10B -179.1(5) . . . . ? C7B C8B C9B C10B -0.3(8) . . . . ? O19B C8B C9B C14A 0.4(8) . . . . ? C7B C8B C9B C14A 179.1(5) . . . . ? C11A C14A C9B C10B -93.7(6) . . . . ? C15A C14A C9B C10B 32.6(7) . . . . ? C11A C14A C9B C8B 86.9(6) . . . . ? C15A C14A C9B C8B -146.9(5) . . . . ? C8B C9B C10B C11B -0.6(8) . . . . ? C14A C9B C10B C11B 180.0(5) . . . . ? C9B C10B C11B C12B 0.3(8) . . . . ? C9B C10B C11B C14B -179.0(5) . . . . ? C8B C7B C12B O13B 176.7(5) . . . . ? C6B C7B C12B O13B -2.9(9) . . . . ? C8B C7B C12B C11B -1.8(8) . . . . ? C6B C7B C12B C11B 178.5(6) . . . . ? C10B C11B C12B O13B -177.6(5) . . . . ? C14B C11B C12B O13B 1.7(8) . . . . ? C10B C11B C12B C7B 0.9(8) . . . . ? C14B C11B C12B C7B -179.7(5) . . . . ? C7B C12B O13B B1B 2.2(8) . . . . ? C11B C12B O13B B1B -179.2(5) . . . . ? O2B B1B O13B C12B -130.3(5) . . . . ? C20B B1B O13B C12B 101.7(6) . . . . ? N5B B1B O13B C12B -23.8(8) . . . . ? C10B C11B C14B C9C 87.2(6) . . . . ? C12B C11B C14B C9C -92.1(6) . . . . ? C10B C11B C14B C15B -42.2(7) . . . . ? C12B C11B C14B C15B 138.5(5) . . . . ? C9C C14B C15B C16B 168.2(5) . . . . ? C11B C14B C15B C16B -63.4(7) . . . . ? C14B C15B C16B C18B 178.1(6) . . . . ? C14B C15B C16B C17B -58.2(8) . . . . ? O2B B1B C20B C21B -160.1(6) . . . . ? O13B B1B C20B C21B -35.9(8) . . . . ? N5B B1B C20B C21B 85.2(7) . . . . ? O2B B1B C20B C25B 19.9(8) . . . . ? O13B B1B C20B C25B 144.2(5) . . . . ? N5B B1B C20B C25B -94.8(7) . . . . ? C25B C20B C21B C22B 3.2(11) . . . . ? B1B C20B C21B C22B -176.8(7) . . . . ? C20B C21B C22B C23B -3.1(14) . . . . ? C21B C22B C23B C24B 0.3(14) . . . . ? C22B C23B C24B C25B 2.1(13) . . . . ? C21B C20B C25B C24B -0.8(9) . . . . ? B1B C20B C25B C24B 179.2(6) . . . . ? C23B C24B C25B C20B -1.8(11) . . . . ? N5B C4B C26B C27B 15.3(12) . . . . ? C3B C4B C26B C27B -98.8(12) . . . . ? C4B C26B C27B C28B 1.8(18) . . . . ? C26B C27B C28B N5B -17.7(18) . . . . ? C4B N5B C28B C27B 26.6(12) . . . . ? C6B N5B C28B C27B -94.7(11) . . . . ? B1B N5B C28B C27B 139.4(11) . . . . ? O13C B1C O2C C3C 77.2(6) . . . . ? C20C B1C O2C C3C -155.5(5) . . . . ? N5C B1C O2C C3C -32.3(6) . . . . ? B1C O2C C3C C4C 14.9(7) . . . . ? O2C C3C C4C N5C 12.0(7) . . . . ? O2C C3C C4C C26C 127.4(6) . . . . ? C3C C4C N5C C6C -152.7(5) . . . . ? C26C C4C N5C C6C 84.3(6) . . . . ? C3C C4C N5C C28C 87.6(5) . . . . ? C26C C4C N5C C28C -35.4(6) . . . . ? C3C C4C N5C B1C -29.5(6) . . . . ? C26C C4C N5C B1C -152.6(5) . . . . ? O2C B1C N5C C6C 161.3(4) . . . . ? O13C B1C N5C C6C 46.8(6) . . . . ? C20C B1C N5C C6C -75.6(6) . . . . ? O2C B1C N5C C4C 37.7(5) . . . . ? O13C B1C N5C C4C -76.8(5) . . . . ? C20C B1C N5C C4C 160.8(5) . . . . ? O2C B1C N5C C28C -71.9(6) . . . . ? O13C B1C N5C C28C 173.6(5) . . . . ? C20C B1C N5C C28C 51.2(7) . . . . ? C4C N5C C6C C7C 64.6(6) . . . . ? C28C N5C C6C C7C -179.6(4) . . . . ? B1C N5C C6C C7C -51.3(6) . . . . ? N5C C6C C7C C12C 29.5(7) . . . . ? N5C C6C C7C C8C -150.9(5) . . . . ? C12C C7C C8C O19C -179.5(5) . . . . ? C6C C7C C8C O19C 0.9(7) . . . . ? C12C C7C C8C C9C 3.3(8) . . . . ? C6C C7C C8C C9C -176.3(5) . . . . ? O19C C8C C9C C10C 179.0(4) . . . . ? C7C C8C C9C C10C -4.0(7) . . . . ? O19C C8C C9C C14B 0.9(7) . . . . ? C7C C8C C9C C14B 177.9(5) . . . . ? C15B C14B C9C C10C 46.6(7) . . . . ? C11B C14B C9C C10C -82.8(6) . . . . ? C15B C14B C9C C8C -135.4(5) . . . . ? C11B C14B C9C C8C 95.1(5) . . . . ? C8C C9C C10C C11C 2.5(7) . . . . ? C14B C9C C10C C11C -179.4(5) . . . . ? C9C C10C C11C C12C -0.2(8) . . . . ? C9C C10C C11C C14C -179.8(5) . . . . ? C8C C7C C12C O13C 176.1(5) . . . . ? C6C C7C C12C O13C -4.3(8) . . . . ? C8C C7C C12C C11C -0.8(8) . . . . ? C6C C7C C12C C11C 178.7(5) . . . . ? C10C C11C C12C O13C -177.7(4) . . . . ? C14C C11C C12C O13C 1.9(7) . . . . ? C10C C11C C12C C7C -0.7(7) . . . . ? C14C C11C C12C C7C 178.9(5) . . . . ? C7C C12C O13C B1C 2.9(8) . . . . ? C11C C12C O13C B1C 179.9(5) . . . . ? O2C B1C O13C C12C -129.5(5) . . . . ? C20C B1C O13C C12C 101.6(6) . . . . ? N5C B1C O13C C12C -22.9(7) . . . . ? C10C C11C C14C C15C -42.6(6) . . . . ? C12C C11C C14C C15C 137.8(5) . . . . ? C10C C11C C14C C9D 87.2(6) . . . . ? C12C C11C C14C C9D -92.4(6) . . . . ? C11C C14C C15C C16C -66.2(7) . . . . ? C9D C14C C15C C16C 164.0(5) . . . . ? C14C C15C C16C C18C -57.6(8) . . . . ? C14C C15C C16C C17C 175.8(6) . . . . ? O2C B1C C20C C25C -146.5(6) . . . . ? O13C B1C C20C C25C -19.6(8) . . . . ? N5C B1C C20C C25C 98.7(7) . . . . ? O2C B1C C20C C21C 30.7(8) . . . . ? O13C B1C C20C C21C 157.5(5) . . . . ? N5C B1C C20C C21C -84.2(7) . . . . ? C25C C20C C21C C22C -0.4(9) . . . . ? B1C C20C C21C C22C -177.6(6) . . . . ? C20C C21C C22C C23C 1.1(10) . . . . ? C21C C22C C23C C24C -1.0(11) . . . . ? C22C C23C C24C C25C 0.1(11) . . . . ? C21C C20C C25C C24C -0.4(9) . . . . ? B1C C20C C25C C24C 176.8(6) . . . . ? C23C C24C C25C C20C 0.6(10) . . . . ? N5C C4C C26C C27C 24.2(7) . . . . ? C3C C4C C26C C27C -90.4(7) . . . . ? C4C C26C C27C C28C -2.8(8) . . . . ? C26C C27C C28C N5C -19.0(8) . . . . ? C6C N5C C28C C27C -88.9(7) . . . . ? C4C N5C C28C C27C 34.0(7) . . . . ? B1C N5C C28C C27C 142.3(6) . . . . ? O13D B1D O2D C3D 78.8(6) . . . . ? C20D B1D O2D C3D -156.5(5) . . . . ? N5D B1D O2D C3D -31.8(6) . . . . ? B1D O2D C3D C4D 13.6(7) . . . . ? O2D C3D C4D N5D 12.6(7) . . . . ? O2D C3D C4D C26D 128.0(6) . . . . ? C3D C4D N5D C6D -153.6(5) . . . . ? C26D C4D N5D C6D 83.0(6) . . . . ? C3D C4D N5D C28D 89.4(5) . . . . ? C26D C4D N5D C28D -34.1(6) . . . . ? C3D C4D N5D B1D -30.4(6) . . . . ? C26D C4D N5D B1D -153.8(5) . . . . ? O2D B1D N5D C6D 162.5(4) . . . . ? O13D B1D N5D C6D 48.4(6) . . . . ? C20D B1D N5D C6D -75.0(6) . . . . ? O2D B1D N5D C4D 38.8(5) . . . . ? O13D B1D N5D C4D -75.3(5) . . . . ? C20D B1D N5D C4D 161.3(5) . . . . ? O2D B1D N5D C28D -72.1(6) . . . . ? O13D B1D N5D C28D 173.8(4) . . . . ? C20D B1D N5D C28D 50.4(7) . . . . ? C4D N5D C6D C7D 61.7(6) . . . . ? C28D N5D C6D C7D 175.6(5) . . . . ? B1D N5D C6D C7D -55.5(6) . . . . ? N5D C6D C7D C8D -147.0(5) . . . . ? N5D C6D C7D C12D 31.6(7) . . . . ? C12D C7D C8D O19D -179.2(4) . . . . ? C6D C7D C8D O19D -0.7(7) . . . . ? C12D C7D C8D C9D 3.3(8) . . . . ? C6D C7D C8D C9D -178.1(5) . . . . ? C7D C8D C9D C10D -2.3(7) . . . . ? O19D C8D C9D C10D -179.6(4) . . . . ? C7D C8D C9D C14C 178.1(5) . . . . ? O19D C8D C9D C14C 0.9(7) . . . . ? C11C C14C C9D C8D 85.7(6) . . . . ? C15C C14C C9D C8D -143.2(5) . . . . ? C11C C14C C9D C10D -93.9(6) . . . . ? C15C C14C C9D C10D 37.2(7) . . . . ? C8D C9D C10D C11D 1.2(7) . . . . ? C14C C9D C10D C11D -179.2(4) . . . . ? C9D C10D C11D C12D -1.2(7) . . . . ? C9D C10D C11D C14D -177.6(4) . . . . ? C10D C11D C12D O13D -177.1(4) . . . . ? C14D C11D C12D O13D -0.5(7) . . . . ? C10D C11D C12D C7D 2.1(7) . . . . ? C14D C11D C12D C7D 178.7(4) . . . . ? C8D C7D C12D O13D 176.0(4) . . . . ? C6D C7D C12D O13D -2.6(7) . . . . ? C8D C7D C12D C11D -3.2(7) . . . . ? C6D C7D C12D C11D 178.2(5) . . . . ? C11D C12D O13D B1D 177.1(5) . . . . ? C7D C12D O13D B1D -2.1(8) . . . . ? O2D B1D O13D C12D -127.7(5) . . . . ? C20D B1D O13D C12D 106.4(6) . . . . ? N5D B1D O13D C12D -20.1(7) . . . . ? C12D C11D C14D C9A -91.2(6) . . . . ? C10D C11D C14D C9A 85.1(6) . . . . ? C12D C11D C14D C15D 141.1(5) . . . . ? C10D C11D C14D C15D -42.6(7) . . . . ? C10A C9A C14D C11D -78.9(6) . . . . ? C8A C9A C14D C11D 100.1(6) . . . . ? C10A C9A C14D C15D 50.8(6) . . . . ? C8A C9A C14D C15D -130.2(5) . . . . ? C11D C14D C15D C16D -55.7(7) . . . . ? C9A C14D C15D C16D 176.5(5) . . . . ? C14D C15D C16D C18D -47.9(7) . . . . ? C14D C15D C16D C17D -171.8(5) . . . . ? O2D B1D C20D C21D 25.2(8) . . . . ? O13D B1D C20D C21D 149.2(6) . . . . ? N5D B1D C20D C21D -90.6(7) . . . . ? O2D B1D C20D C25D -153.5(5) . . . . ? O13D B1D C20D C25D -29.6(7) . . . . ? N5D B1D C20D C25D 90.7(7) . . . . ? C25D C20D C21D C22D 0.3(11) . . . . ? B1D C20D C21D C22D -178.5(8) . . . . ? C20D C21D C22D C23D 0.9(14) . . . . ? C21D C22D C23D C24D -0.4(16) . . . . ? C22D C23D C24D C25D -1.3(14) . . . . ? C21D C20D C25D C24D -2.2(9) . . . . ? B1D C20D C25D C24D 176.6(6) . . . . ? C23D C24D C25D C20D 2.7(11) . . . . ? N5D C4D C26D C27D 15.7(7) . . . . ? C3D C4D C26D C27D -97.4(7) . . . . ? C4D C26D C27D C28D 8.9(7) . . . . ? C6D N5D C28D C27D -81.2(6) . . . . ? C4D N5D C28D C27D 39.9(6) . . . . ? B1D N5D C28D C27D 150.7(5) . . . . ? C26D C27D C28D N5D -30.2(6) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.30 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.692 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.059 #========================================================================== data_fro1816 _database_code_CSD 183053 _journal_coden_Cambridge 182 loop_ _publ_author_name 'Waldemar, Iwanek' 'Frohlich, Roland' 'Schwab, Pia' _publ_contact_author_name 'Dr Iwanek Waldemar' _publ_contact_author_address ; Institut of Organic Chemistry University of Tuebingen Auf der Morgenstelle 18 Tuebingen 72076 GERMANY ; _publ_contact_author_email 'WALDEMAR.IWANEK@UNI-TUEBINGEN.DE' _publ_requested_journal 'Chemical Communications' _publ_section_title ; The Diastereoselective Closure Ring of the Calixresorcin[4]arene. The Synthesis and Crystallographic Structures of Novel Bora-oxazino-oxazolidine Derivatives of Calixresorcin[4]arene ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C104 H136 B4 N4 O16' _chemical_formula_weight 1741.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'P212121' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 15.381(1) _cell_length_b 23.282(1) _cell_length_c 29.512(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10568.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.094 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3744 _exptl_absorpt_coefficient_mu 0.072 _exptl_absorpt_correction_type 'SORTAV (Blessing, 1995 & 1997)' _exptl_absorpt_correction_T_min 0.9717 _exptl_absorpt_correction_T_max 0.9857 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63144 _diffrn_reflns_av_R_equivalents 0.1276 _diffrn_reflns_av_sigmaI/netI 0.0982 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 22.50 _reflns_number_total 13815 _reflns_number_gt 9215 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Shedlrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. In part A isopropyl group (C15A-C18A) is disordered, refined with split positions (0.51(2):0.49) and restrains (SADI), phenyl groups C20C-C25C and C20D-C25D are refined as rigid groups, solvent molecules located at five positions, two of them only half occupied (fixed to SOF 0.5), all refined with restrains (DFIX) and one isotropic thermal parameter for each molecule. Structure determination of poor quality due to disorder and solvent molecules, only as confirmation of the chemical composition. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'refined as riding atoms' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0089(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0(4) _refine_ls_number_reflns 13815 _refine_ls_number_parameters 1089 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.1755 _refine_ls_R_factor_gt 0.1297 _refine_ls_wR_factor_ref 0.3042 _refine_ls_wR_factor_gt 0.2894 _refine_ls_goodness_of_fit_ref 1.720 _refine_ls_restrained_S_all 2.766 _refine_ls_shift/su_max 0.008 _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 B1A B 0.1006(11) 0.5169(7) 0.1198(5) 0.055(4) Uani 1 1 d . . . O2A O 0.0556(7) 0.5708(4) 0.1158(4) 0.075(3) Uani 1 1 d . . . C3A C 0.014(2) 0.5786(10) 0.0755(9) 0.162(12) Uani 1 1 d . . . H3A1 H 0.0530 0.5968 0.0533 0.195 Uiso 1 1 calc R . . H3A2 H -0.0375 0.6039 0.0798 0.195 Uiso 1 1 calc R . . C4A C -0.0155(9) 0.5200(6) 0.0584(5) 0.065(4) Uani 1 1 d . . . H4A H -0.0006 0.5176 0.0254 0.078 Uiso 1 1 calc R . . N5A N 0.0426(6) 0.4765(5) 0.0841(3) 0.050(3) Uani 1 1 d . . . C6A C 0.1014(10) 0.4459(6) 0.0516(5) 0.065(4) Uani 1 1 d . . . H6A1 H 0.0660 0.4258 0.0285 0.078 Uiso 1 1 calc R . . H6A2 H 0.1359 0.4167 0.0681 0.078 Uiso 1 1 calc R . . C7A C 0.1622(8) 0.4878(5) 0.0285(4) 0.048(3) Uani 1 1 d . . . C8A C 0.1745(9) 0.4920(6) -0.0182(5) 0.058(4) Uani 1 1 d . . . C9A C 0.2307(10) 0.5336(6) -0.0358(4) 0.054(4) Uani 1 1 d . . . C10A C 0.2747(8) 0.5680(5) -0.0053(5) 0.048(3) Uani 1 1 d . . . H10A H 0.3149 0.5953 -0.0170 0.057 Uiso 1 1 calc R . . C11A C 0.2635(8) 0.5652(5) 0.0416(4) 0.045(3) Uani 1 1 d . . . C12A C 0.2056(8) 0.5252(6) 0.0582(5) 0.047(3) Uani 1 1 d . . . O13A O 0.1905(5) 0.5181(4) 0.1039(3) 0.052(2) Uani 1 1 d . . . C14A C 0.3138(9) 0.6031(5) 0.0754(4) 0.050(3) Uani 1 1 d . B . H14A H 0.2771 0.6049 0.1034 0.060 Uiso 1 1 calc R . . C15A C 0.3233(10) 0.6658(6) 0.0588(5) 0.062(4) Uani 1 1 d D . . H15A H 0.3712 0.6840 0.0759 0.075 Uiso 1 1 calc R A 1 H15B H 0.3407 0.6649 0.0265 0.075 Uiso 1 1 calc R A 1 C16A C 0.2448(16) 0.7028(9) 0.0630(10) 0.079(12) Uani 0.49(3) 1 d PD B 1 H16A H 0.2031 0.6913 0.0387 0.094 Uiso 0.49(3) 1 calc PR B 1 C17A C 0.270(3) 0.7640(10) 0.0549(16) 0.104(16) Uani 0.49(3) 1 d PD B 1 H17A H 0.2264 0.7894 0.0686 0.156 Uiso 0.49(3) 1 calc PR B 1 H17B H 0.2730 0.7713 0.0223 0.156 Uiso 0.49(3) 1 calc PR B 1 H17C H 0.3268 0.7715 0.0687 0.156 Uiso 0.49(3) 1 calc PR B 1 C18A C 0.199(3) 0.6983(17) 0.1073(13) 0.13(2) Uani 0.49(3) 1 d PD B 1 H18A H 0.1532 0.7277 0.1090 0.193 Uiso 0.49(3) 1 calc PR B 1 H18B H 0.2403 0.7041 0.1321 0.193 Uiso 0.49(3) 1 calc PR B 1 H18C H 0.1723 0.6601 0.1101 0.193 Uiso 0.49(3) 1 calc PR B 1 C16E C 0.345(2) 0.7111(7) 0.0920(8) 0.062(10) Uani 0.51(3) 1 d PD B 2 H16E H 0.4076 0.7038 0.0988 0.075 Uiso 0.51(3) 1 calc PR B 2 C17E C 0.344(3) 0.7722(11) 0.0758(17) 0.117(17) Uani 0.51(3) 1 d PD B 2 H17D H 0.3648 0.7974 0.1002 0.176 Uiso 0.51(3) 1 calc PR B 2 H17E H 0.2852 0.7832 0.0672 0.176 Uiso 0.51(3) 1 calc PR B 2 H17F H 0.3830 0.7760 0.0496 0.176 Uiso 0.51(3) 1 calc PR B 2 C18E C 0.302(3) 0.7038(13) 0.1368(11) 0.114(16) Uani 0.51(3) 1 d PD B 2 H18D H 0.3204 0.7349 0.1570 0.170 Uiso 0.51(3) 1 calc PR B 2 H18E H 0.3191 0.6668 0.1498 0.170 Uiso 0.51(3) 1 calc PR B 2 H18F H 0.2389 0.7050 0.1329 0.170 Uiso 0.51(3) 1 calc PR B 2 O19A O 0.1278(7) 0.4550(4) -0.0449(3) 0.074(3) Uani 1 1 d . . . H19A H 0.1258 0.4225 -0.0326 0.111 Uiso 1 1 calc R . . C20A C 0.0993(10) 0.4937(6) 0.1717(5) 0.059(4) Uani 1 1 d . . . C21A C 0.1548(13) 0.4534(8) 0.1863(5) 0.085(5) Uani 1 1 d . . . H21A H 0.1966 0.4380 0.1660 0.102 Uiso 1 1 calc R . . C22A C 0.1524(14) 0.4337(8) 0.2313(7) 0.108(7) Uani 1 1 d . . . H22A H 0.1929 0.4055 0.2411 0.129 Uiso 1 1 calc R . . C23A C 0.0925(15) 0.4547(11) 0.2611(6) 0.109(7) Uani 1 1 d . . . H23A H 0.0891 0.4405 0.2912 0.131 Uiso 1 1 calc R . . C24A C 0.0381(13) 0.4964(9) 0.2464(7) 0.090(5) Uani 1 1 d . . . H24A H -0.0024 0.5126 0.2671 0.108 Uiso 1 1 calc R . . C25A C 0.0397(9) 0.5154(7) 0.2035(6) 0.069(4) Uani 1 1 d . . . H25A H -0.0004 0.5442 0.1944 0.083 Uiso 1 1 calc R . . C26A C -0.1091(11) 0.4978(10) 0.0642(9) 0.128(8) Uani 1 1 d . . . H26A H -0.1405 0.5213 0.0870 0.153 Uiso 1 1 calc R . . H26B H -0.1410 0.5001 0.0351 0.153 Uiso 1 1 calc R . . C27A C -0.1029(12) 0.4374(8) 0.0796(7) 0.099(6) Uani 1 1 d . . . H27A H -0.1009 0.4110 0.0533 0.119 Uiso 1 1 calc R . . H27B H -0.1532 0.4272 0.0988 0.119 Uiso 1 1 calc R . . C28A C -0.0192(11) 0.4343(6) 0.1064(5) 0.070(5) Uani 1 1 d . . . H28A H 0.0050 0.3949 0.1054 0.085 Uiso 1 1 calc R . . H28B H -0.0296 0.4450 0.1384 0.085 Uiso 1 1 calc R . . B1B B 0.6601(13) 0.4965(8) 0.1742(6) 0.068(5) Uani 1 1 d . B . O2B O 0.7033(7) 0.5483(4) 0.1902(3) 0.075(3) Uani 1 1 d . . . C3B C 0.6375(14) 0.5889(7) 0.1994(7) 0.097(6) Uani 1 1 d . . . H3B1 H 0.6144 0.6051 0.1708 0.116 Uiso 1 1 calc R . . H3B2 H 0.6610 0.6207 0.2180 0.116 Uiso 1 1 calc R . . C4B C 0.5675(12) 0.5584(7) 0.2244(5) 0.074(4) Uani 1 1 d . . . H4B H 0.5090 0.5753 0.2179 0.089 Uiso 1 1 calc R . . N5B N 0.5744(7) 0.4968(6) 0.2070(4) 0.070(4) Uani 1 1 d . . . C6B C 0.4951(9) 0.4785(7) 0.1820(5) 0.066(4) Uani 1 1 d . . . H6B1 H 0.4436 0.4816 0.2020 0.079 Uiso 1 1 calc R . . H6B2 H 0.5010 0.4379 0.1724 0.079 Uiso 1 1 calc R . . C7B C 0.4840(10) 0.5164(6) 0.1415(5) 0.055(4) Uani 1 1 d . . . C8B C 0.4034(10) 0.5409(6) 0.1281(4) 0.058(4) Uani 1 1 d . B . C9B C 0.3972(9) 0.5744(5) 0.0893(5) 0.051(3) Uani 1 1 d . . . C10B C 0.4731(10) 0.5810(5) 0.0632(5) 0.056(4) Uani 1 1 d . B . H10B H 0.4687 0.6028 0.0361 0.067 Uiso 1 1 calc R . . C11B C 0.5538(9) 0.5582(6) 0.0739(4) 0.051(3) Uani 1 1 d . . . C12B C 0.5558(11) 0.5262(6) 0.1150(5) 0.057(4) Uani 1 1 d . B . O13B O 0.6314(7) 0.4993(4) 0.1275(3) 0.062(3) Uani 1 1 d . . . C14B C 0.6361(9) 0.5663(6) 0.0463(5) 0.058(4) Uani 1 1 d . B . H14B H 0.6861 0.5562 0.0665 0.069 Uiso 1 1 calc R . . C15B C 0.6491(10) 0.6279(5) 0.0314(5) 0.060(4) Uani 1 1 d . . . H15C H 0.5980 0.6406 0.0136 0.073 Uiso 1 1 calc R B . H15D H 0.7008 0.6302 0.0115 0.073 Uiso 1 1 calc R . . C16B C 0.6615(12) 0.6683(7) 0.0721(6) 0.085(5) Uani 1 1 d . B . H16B H 0.6114 0.6627 0.0932 0.102 Uiso 1 1 calc R . . C17B C 0.6590(19) 0.7323(6) 0.0541(7) 0.137(9) Uani 1 1 d . . . H17G H 0.6160 0.7354 0.0297 0.206 Uiso 1 1 calc R B . H17H H 0.7165 0.7429 0.0425 0.206 Uiso 1 1 calc R . . H17I H 0.6429 0.7581 0.0790 0.206 Uiso 1 1 calc R . . C18B C 0.7435(14) 0.6552(8) 0.0973(6) 0.111(7) Uani 1 1 d . . . H18G H 0.7906 0.6481 0.0756 0.167 Uiso 1 1 calc R B . H18H H 0.7348 0.6209 0.1161 0.167 Uiso 1 1 calc R . . H18I H 0.7587 0.6878 0.1167 0.167 Uiso 1 1 calc R . . O19B O 0.3325(7) 0.5308(5) 0.1554(3) 0.075(3) Uani 1 1 d . . . H19B H 0.3466 0.5081 0.1763 0.112 Uiso 1 1 calc R B . C20B C 0.7234(11) 0.4403(7) 0.1788(5) 0.070(4) Uani 1 1 d . . . C21B C 0.7026(10) 0.3894(7) 0.1593(5) 0.072(4) Uani 1 1 d . B . H21B H 0.6492 0.3872 0.1431 0.086 Uiso 1 1 calc R . . C22B C 0.7540(13) 0.3397(8) 0.1612(6) 0.096(6) Uani 1 1 d . . . H22B H 0.7361 0.3048 0.1475 0.115 Uiso 1 1 calc R B . C23B C 0.8336(13) 0.3443(7) 0.1846(7) 0.092(6) Uani 1 1 d . B . H23B H 0.8711 0.3120 0.1865 0.110 Uiso 1 1 calc R . . C24B C 0.8568(10) 0.3944(8) 0.2041(5) 0.068(4) Uani 1 1 d . . . H24B H 0.9109 0.3969 0.2195 0.082 Uiso 1 1 calc R B . C25B C 0.8040(11) 0.4421(7) 0.2022(5) 0.067(4) Uani 1 1 d . B . H25B H 0.8216 0.4765 0.2168 0.080 Uiso 1 1 calc R . . C26B C 0.5824(13) 0.5517(10) 0.2743(5) 0.091(6) Uani 1 1 d . . . H26C H 0.6454 0.5532 0.2812 0.109 Uiso 1 1 calc R . . H26D H 0.5531 0.5830 0.2912 0.109 Uiso 1 1 calc R . . C27B C 0.5468(12) 0.4966(11) 0.2872(6) 0.110(7) Uani 1 1 d . . . H27C H 0.4824 0.4971 0.2869 0.131 Uiso 1 1 calc R . . H27D H 0.5675 0.4845 0.3175 0.131 Uiso 1 1 calc R . . C28B C 0.5824(12) 0.4590(8) 0.2506(5) 0.085(5) Uani 1 1 d . . . H28C H 0.5479 0.4233 0.2477 0.103 Uiso 1 1 calc R . . H28D H 0.6437 0.4488 0.2567 0.103 Uiso 1 1 calc R . . B1C B 0.7009(13) 0.3548(7) -0.1026(6) 0.060(5) Uani 1 1 d . B . O2C O 0.7620(14) 0.3508(10) -0.1350(4) 0.168(9) Uani 1 1 d . . . C3C C 0.8314(16) 0.3866(16) -0.1205(9) 0.189(17) Uani 1 1 d . . . H3C1 H 0.8213 0.4264 -0.1313 0.227 Uiso 1 1 calc R . . H3C2 H 0.8866 0.3728 -0.1339 0.227 Uiso 1 1 calc R . . C4C C 0.8384(10) 0.3864(7) -0.0683(6) 0.081(5) Uani 1 1 d . . . H4C H 0.8326 0.4260 -0.0556 0.097 Uiso 1 1 calc R . . N5C N 0.7614(7) 0.3499(4) -0.0564(4) 0.052(3) Uani 1 1 d . . . C6C C 0.7128(12) 0.3692(6) -0.0158(5) 0.074(4) Uani 1 1 d . . . H6C1 H 0.7520 0.3700 0.0108 0.089 Uiso 1 1 calc R . . H6C2 H 0.6648 0.3421 -0.0093 0.089 Uiso 1 1 calc R . . C7C C 0.6761(9) 0.4293(6) -0.0244(5) 0.062(4) Uani 1 1 d . . . C8C C 0.6703(9) 0.4680(6) 0.0127(5) 0.056(4) Uani 1 1 d . B . C9C C 0.6362(8) 0.5230(5) 0.0069(5) 0.048(3) Uani 1 1 d . . . C10C C 0.6052(9) 0.5369(6) -0.0365(5) 0.055(4) Uani 1 1 d . B . H10C H 0.5801 0.5737 -0.0410 0.065 Uiso 1 1 calc R . . C11C C 0.6096(9) 0.4982(6) -0.0743(4) 0.054(4) Uani 1 1 d . . . C12C C 0.6472(9) 0.4457(6) -0.0669(5) 0.059(4) Uani 1 1 d . B . O13C O 0.6533(6) 0.4070(4) -0.1014(3) 0.070(3) Uani 1 1 d . . . C14C C 0.5671(10) 0.5133(6) -0.1184(4) 0.061(4) Uani 1 1 d . B . H14C H 0.5998 0.4905 -0.1415 0.073 Uiso 1 1 calc R . . C15C C 0.5755(9) 0.5751(6) -0.1344(5) 0.064(4) Uani 1 1 d . . . H15E H 0.5467 0.5785 -0.1643 0.076 Uiso 1 1 calc R B . H15F H 0.5435 0.6001 -0.1129 0.076 Uiso 1 1 calc R . . C16C C 0.6680(11) 0.5976(7) -0.1387(5) 0.074(4) Uani 1 1 d . B . H16C H 0.6937 0.6013 -0.1077 0.089 Uiso 1 1 calc R . . C17C C 0.6642(13) 0.6583(8) -0.1609(6) 0.103(6) Uani 1 1 d . . . H17J H 0.6240 0.6575 -0.1866 0.154 Uiso 1 1 calc R B . H17K H 0.7223 0.6692 -0.1714 0.154 Uiso 1 1 calc R . . H17L H 0.6438 0.6863 -0.1385 0.154 Uiso 1 1 calc R . . C18C C 0.7264(12) 0.5597(9) -0.1670(6) 0.099(6) Uani 1 1 d . . . H18J H 0.7810 0.5799 -0.1731 0.149 Uiso 1 1 calc R B . H18K H 0.6974 0.5506 -0.1956 0.149 Uiso 1 1 calc R . . H18L H 0.7385 0.5241 -0.1505 0.149 Uiso 1 1 calc R . . O19C O 0.6993(7) 0.4472(4) 0.0538(3) 0.066(3) Uani 1 1 d . . . H19C H 0.6814 0.4686 0.0747 0.099 Uiso 1 1 calc R B . C20C C 0.6169(10) 0.3053(7) -0.0996(7) 0.163(12) Uani 1 1 d G . . C21C C 0.5442(12) 0.3131(7) -0.0722(6) 0.133(8) Uani 1 1 d G B . H21C H 0.5415 0.3449 -0.0521 0.160 Uiso 1 1 calc R . . C22C C 0.4756(11) 0.2743(9) -0.0743(7) 0.175(13) Uani 1 1 d G B . H22C H 0.4260 0.2796 -0.0556 0.210 Uiso 1 1 calc R . . C23C C 0.4797(14) 0.2278(8) -0.1037(8) 0.216(19) Uani 1 1 d G B . H23C H 0.4328 0.2013 -0.1051 0.260 Uiso 1 1 calc R . . C24C C 0.5523(18) 0.2200(7) -0.1311(7) 0.157(12) Uani 1 1 d G B . H24C H 0.5551 0.1882 -0.1512 0.188 Uiso 1 1 calc R . . C25C C 0.6209(14) 0.2588(9) -0.1290(7) 0.24(2) Uani 1 1 d G B . H25C H 0.6705 0.2535 -0.1477 0.286 Uiso 1 1 calc R . . C26C C 0.9162(11) 0.3560(8) -0.0490(6) 0.087(5) Uani 1 1 d . . . H26E H 0.9580 0.3466 -0.0734 0.104 Uiso 1 1 calc R . . H26F H 0.9458 0.3809 -0.0266 0.104 Uiso 1 1 calc R . . C27C C 0.8860(13) 0.3040(10) -0.0274(8) 0.117(7) Uani 1 1 d . . . H27E H 0.8819 0.3096 0.0058 0.141 Uiso 1 1 calc R . . H27F H 0.9268 0.2720 -0.0335 0.141 Uiso 1 1 calc R . . C28C C 0.7949(12) 0.2901(6) -0.0474(6) 0.083(5) Uani 1 1 d . . . H28E H 0.7993 0.2674 -0.0757 0.100 Uiso 1 1 calc R . . H28F H 0.7579 0.2694 -0.0254 0.100 Uiso 1 1 calc R . . B1D B 0.1872(12) 0.3861(6) -0.1587(6) 0.058(5) Uani 1 1 d . B . O2D O 0.1291(7) 0.4099(4) -0.1914(4) 0.079(3) Uani 1 1 d . . . C3D C 0.1817(16) 0.4396(10) -0.2239(8) 0.142(10) Uani 1 1 d . . . H3D1 H 0.1917 0.4796 -0.2139 0.170 Uiso 1 1 calc R . . H3D2 H 0.1518 0.4405 -0.2536 0.170 Uiso 1 1 calc R . . C4D C 0.2672(10) 0.4084(6) -0.2282(5) 0.067(4) Uani 1 1 d . . . H4D H 0.3159 0.4361 -0.2230 0.081 Uiso 1 1 calc R . . N5D N 0.2653(7) 0.3642(4) -0.1892(3) 0.054(3) Uani 1 1 d . . . C6D C 0.3481(10) 0.3598(6) -0.1637(5) 0.071(4) Uani 1 1 d . . . H6D1 H 0.3956 0.3492 -0.1848 0.085 Uiso 1 1 calc R . . H6D2 H 0.3432 0.3293 -0.1405 0.085 Uiso 1 1 calc R . . C7D C 0.3692(11) 0.4163(6) -0.1411(5) 0.062(4) Uani 1 1 d . . . C8D C 0.4548(10) 0.4379(6) -0.1416(5) 0.057(4) Uani 1 1 d . B . C9D C 0.4722(9) 0.4904(6) -0.1215(4) 0.054(4) Uani 1 1 d . . . C10D C 0.4066(9) 0.5225(6) -0.1032(4) 0.055(4) Uani 1 1 d . B . H10D H 0.4199 0.5581 -0.0891 0.066 Uiso 1 1 calc R . . C11D C 0.3173(10) 0.5031(6) -0.1047(4) 0.056(4) Uani 1 1 d . . . C12D C 0.3008(10) 0.4504(6) -0.1253(5) 0.053(4) Uani 1 1 d . B . O13D O 0.2210(7) 0.4297(4) -0.1250(3) 0.068(3) Uani 1 1 d . . . C14D C 0.2417(10) 0.5397(6) -0.0866(4) 0.060(4) Uani 1 1 d . B . H14D H 0.1876 0.5239 -0.1006 0.072 Uiso 1 1 calc R . . C15D C 0.2497(10) 0.6028(6) -0.1029(5) 0.064(4) Uani 1 1 d . . . H15G H 0.2042 0.6262 -0.0880 0.076 Uiso 1 1 calc R B . H15H H 0.3069 0.6182 -0.0936 0.076 Uiso 1 1 calc R . . C16D C 0.2405(13) 0.6085(7) -0.1540(5) 0.082(5) Uani 1 1 d . B . H16D H 0.2798 0.5803 -0.1693 0.098 Uiso 1 1 calc R . . C17D C 0.268(2) 0.6715(8) -0.1678(6) 0.176(14) Uani 1 1 d . . . H17M H 0.2904 0.6916 -0.1412 0.264 Uiso 1 1 calc R B . H17N H 0.2167 0.6920 -0.1794 0.264 Uiso 1 1 calc R . . H17O H 0.3125 0.6699 -0.1913 0.264 Uiso 1 1 calc R . . C18D C 0.1472(17) 0.5978(11) -0.1688(7) 0.142(9) Uani 1 1 d . . . H18M H 0.1076 0.6200 -0.1496 0.214 Uiso 1 1 calc R B . H18N H 0.1338 0.5568 -0.1660 0.214 Uiso 1 1 calc R . . H18O H 0.1400 0.6098 -0.2005 0.214 Uiso 1 1 calc R . . O19D O 0.5189(6) 0.4056(4) -0.1610(4) 0.079(3) Uani 1 1 d . . . H19D H 0.5024 0.3713 -0.1629 0.118 Uiso 1 1 calc R B . C20D C 0.1423(8) 0.3318(4) -0.1291(4) 0.075(5) Uani 1 1 d G . . C21D C 0.0758(8) 0.2981(7) -0.1467(5) 0.107(7) Uani 1 1 d G B . H21D H 0.0506 0.3075 -0.1751 0.129 Uiso 1 1 calc R . . C22D C 0.0462(9) 0.2506(6) -0.1227(7) 0.145(11) Uani 1 1 d G B . H22D H 0.0008 0.2276 -0.1347 0.174 Uiso 1 1 calc R . . C23D C 0.0831(12) 0.2369(5) -0.0811(7) 0.158(12) Uani 1 1 d G B . H23D H 0.0629 0.2044 -0.0646 0.189 Uiso 1 1 calc R . . C24D C 0.1496(12) 0.2706(7) -0.0635(5) 0.148(10) Uani 1 1 d G B . H24D H 0.1748 0.2612 -0.0350 0.177 Uiso 1 1 calc R . . C25D C 0.1792(8) 0.3181(6) -0.0875(4) 0.093(6) Uani 1 1 d G B . H25D H 0.2246 0.3412 -0.0755 0.112 Uiso 1 1 calc R . . C26D C 0.2843(13) 0.3753(6) -0.2708(5) 0.082(5) Uani 1 1 d . . . H26G H 0.2341 0.3790 -0.2916 0.099 Uiso 1 1 calc R . . H26H H 0.3362 0.3911 -0.2863 0.099 Uiso 1 1 calc R . . C27D C 0.2990(15) 0.3136(9) -0.2599(7) 0.112(7) Uani 1 1 d . . . H27G H 0.3616 0.3050 -0.2562 0.135 Uiso 1 1 calc R . . H27H H 0.2743 0.2882 -0.2835 0.135 Uiso 1 1 calc R . . C28D C 0.2483(10) 0.3077(6) -0.2138(5) 0.066(4) Uani 1 1 d . . . H28G H 0.1854 0.3023 -0.2192 0.080 Uiso 1 1 calc R . . H28H H 0.2706 0.2748 -0.1960 0.080 Uiso 1 1 calc R . . O201 O -0.1041(9) 0.6184(6) -0.0052(5) 0.140(4) Uiso 1 1 d D . . C202 C -0.0754(11) 0.5964(6) -0.0387(6) 0.140(4) Uiso 1 1 d D . . C203 C -0.1260(14) 0.5533(8) -0.0625(7) 0.140(4) Uiso 1 1 d D . . H20A H -0.1824 0.5487 -0.0475 0.209 Uiso 1 1 calc R . . H20B H -0.0948 0.5167 -0.0622 0.209 Uiso 1 1 calc R . . H20C H -0.1352 0.5656 -0.0939 0.209 Uiso 1 1 calc R . . C204 C 0.0100(12) 0.6123(9) -0.0558(7) 0.140(4) Uiso 1 1 d D . . H20D H 0.0357 0.6413 -0.0358 0.209 Uiso 1 1 calc R . . H20E H 0.0042 0.6281 -0.0864 0.209 Uiso 1 1 calc R . . H20F H 0.0474 0.5783 -0.0566 0.209 Uiso 1 1 calc R . . O211 O 0.4688(13) 0.6660(9) -0.0479(7) 0.200(6) Uiso 1 1 d D . . C212 C 0.4811(15) 0.7134(10) -0.0614(5) 0.200(6) Uiso 1 1 d D . . C213 C 0.4113(17) 0.7484(12) -0.0795(11) 0.200(6) Uiso 1 1 d D . . H21E H 0.3600 0.7243 -0.0847 0.300 Uiso 1 1 calc R . . H21F H 0.4298 0.7656 -0.1082 0.300 Uiso 1 1 calc R . . H21G H 0.3969 0.7788 -0.0578 0.300 Uiso 1 1 calc R . . C214 C 0.5694(16) 0.7395(11) -0.0606(11) 0.200(6) Uiso 1 1 d D . . H21H H 0.6125 0.7097 -0.0539 0.300 Uiso 1 1 calc R . . H21I H 0.5717 0.7692 -0.0371 0.300 Uiso 1 1 calc R . . H21J H 0.5820 0.7567 -0.0901 0.300 Uiso 1 1 calc R . . O221 O 0.3441(17) 0.3477(11) 0.0182(9) 0.264(9) Uiso 1 1 d D . . C222 C 0.3837(14) 0.3881(11) 0.0316(9) 0.264(9) Uiso 1 1 d D . . C223 C 0.420(3) 0.4286(15) -0.0008(11) 0.264(9) Uiso 1 1 d D . . H22E H 0.4139 0.4130 -0.0315 0.396 Uiso 1 1 calc R . . H22F H 0.4813 0.4350 0.0060 0.396 Uiso 1 1 calc R . . H22G H 0.3882 0.4651 0.0012 0.396 Uiso 1 1 calc R . . C224 C 0.394(3) 0.3952(16) 0.0807(9) 0.264(9) Uiso 1 1 d D . . H22H H 0.3753 0.3602 0.0961 0.396 Uiso 1 1 calc R . . H22I H 0.3588 0.4277 0.0910 0.396 Uiso 1 1 calc R . . H22J H 0.4555 0.4026 0.0876 0.396 Uiso 1 1 calc R . . O231 O 0.6462(19) 0.3775(11) -0.2506(10) 0.144(8) Uiso 0.50 1 d PD . . C232 C 0.6342(19) 0.3278(12) -0.2625(8) 0.144(8) Uiso 0.50 1 d PD . . C233 C 0.552(2) 0.2968(17) -0.2599(16) 0.144(8) Uiso 0.50 1 d PD . . H23E H 0.5044 0.3242 -0.2557 0.216 Uiso 0.50 1 calc PR . . H23F H 0.5537 0.2701 -0.2342 0.216 Uiso 0.50 1 calc PR . . H23G H 0.5429 0.2752 -0.2880 0.216 Uiso 0.50 1 calc PR . . C234 C 0.706(2) 0.2950(15) -0.2810(16) 0.144(8) Uiso 0.50 1 d PD . . H23H H 0.7525 0.3214 -0.2906 0.216 Uiso 0.50 1 calc PR . . H23I H 0.6862 0.2727 -0.3071 0.216 Uiso 0.50 1 calc PR . . H23J H 0.7289 0.2689 -0.2578 0.216 Uiso 0.50 1 calc PR . . O241 O -0.068(2) 0.1632(13) -0.2197(10) 0.150(8) Uiso 0.50 1 d PD . . C242 C -0.1260(19) 0.1897(14) -0.2013(9) 0.150(8) Uiso 0.50 1 d PD . . C243 C -0.143(3) 0.2488(14) -0.2125(16) 0.150(8) Uiso 0.50 1 d PD . . H24E H -0.1695 0.2510 -0.2426 0.225 Uiso 0.50 1 calc PR . . H24F H -0.0878 0.2702 -0.2126 0.225 Uiso 0.50 1 calc PR . . H24G H -0.1821 0.2654 -0.1900 0.225 Uiso 0.50 1 calc PR . . C244 C -0.179(3) 0.1602(18) -0.1673(14) 0.150(8) Uiso 0.50 1 d PD . . H24H H -0.2198 0.1342 -0.1824 0.225 Uiso 0.50 1 calc PR . . H24I H -0.2116 0.1886 -0.1496 0.225 Uiso 0.50 1 calc PR . . H24J H -0.1411 0.1381 -0.1471 0.225 Uiso 0.50 1 calc PR . . 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 B1A 0.057(11) 0.059(11) 0.048(11) 0.009(8) 0.013(8) -0.004(9) O2A 0.074(7) 0.074(7) 0.077(8) -0.003(6) -0.011(6) 0.004(6) C3A 0.24(3) 0.104(17) 0.14(2) -0.038(15) -0.10(2) 0.059(18) C4A 0.073(10) 0.066(10) 0.057(10) -0.002(8) -0.015(8) 0.013(8) N5A 0.039(6) 0.068(7) 0.043(7) -0.009(6) 0.006(5) -0.005(6) C6A 0.090(11) 0.056(9) 0.049(9) 0.000(7) -0.013(8) -0.014(9) C7A 0.055(8) 0.046(8) 0.043(9) -0.002(6) -0.001(7) -0.013(7) C8A 0.069(10) 0.062(9) 0.044(10) -0.002(8) 0.002(8) -0.001(8) C9A 0.077(10) 0.054(8) 0.032(8) 0.002(7) 0.008(8) 0.016(8) C10A 0.046(8) 0.048(8) 0.049(10) 0.011(7) 0.010(7) 0.009(7) C11A 0.048(8) 0.046(7) 0.041(9) 0.000(6) 0.002(7) 0.010(7) C12A 0.041(8) 0.056(8) 0.044(9) 0.009(7) 0.012(7) 0.009(7) O13A 0.049(6) 0.066(6) 0.041(6) 0.003(4) 0.010(4) -0.009(4) C14A 0.064(9) 0.046(8) 0.039(8) -0.007(6) 0.011(7) -0.001(7) C15A 0.082(11) 0.060(9) 0.044(9) 0.001(7) 0.014(8) -0.011(9) C16A 0.08(2) 0.08(2) 0.08(3) -0.013(18) -0.02(2) 0.00(2) C17A 0.13(4) 0.04(2) 0.14(4) 0.01(2) 0.04(3) -0.01(2) C18A 0.16(4) 0.11(3) 0.12(4) 0.05(3) 0.09(4) 0.07(3) C16E 0.08(2) 0.052(18) 0.06(2) -0.001(15) -0.029(17) -0.012(15) C17E 0.10(3) 0.05(2) 0.20(5) 0.06(2) -0.04(3) -0.04(2) C18E 0.18(4) 0.06(2) 0.10(3) -0.04(2) -0.04(3) -0.01(2) O19A 0.097(8) 0.064(6) 0.061(7) -0.004(5) 0.000(6) -0.019(6) C20A 0.072(10) 0.063(9) 0.041(9) 0.004(7) -0.006(8) -0.004(8) C21A 0.111(14) 0.108(13) 0.035(10) 0.021(9) -0.009(9) 0.009(12) C22A 0.124(16) 0.112(14) 0.088(15) 0.041(12) 0.020(13) 0.044(13) C23A 0.095(15) 0.19(2) 0.046(11) -0.001(14) 0.026(11) -0.039(16) C24A 0.083(13) 0.124(16) 0.065(15) 0.008(11) -0.003(11) 0.000(12) C25A 0.053(10) 0.097(12) 0.058(12) -0.017(10) 0.003(9) -0.016(9) C26A 0.046(11) 0.16(2) 0.18(2) 0.047(17) 0.001(12) -0.016(12) C27A 0.084(13) 0.110(15) 0.103(15) 0.039(12) 0.004(11) -0.026(11) C28A 0.101(13) 0.068(10) 0.042(9) 0.011(7) -0.008(9) -0.031(9) B1B 0.097(14) 0.068(12) 0.038(11) -0.003(8) -0.013(10) 0.002(11) O2B 0.092(8) 0.073(7) 0.060(7) -0.013(5) -0.009(6) 0.002(7) C3B 0.137(16) 0.053(10) 0.100(14) -0.032(10) 0.009(13) 0.009(12) C4B 0.099(13) 0.075(11) 0.047(10) -0.013(8) -0.004(9) -0.010(10) N5B 0.053(8) 0.117(11) 0.040(7) 0.008(7) 0.002(6) 0.013(7) C6B 0.049(9) 0.102(12) 0.046(9) 0.024(8) -0.010(7) -0.004(8) C7B 0.053(9) 0.071(10) 0.040(9) -0.001(7) -0.009(8) -0.003(8) C8B 0.071(11) 0.082(10) 0.021(8) -0.002(7) 0.010(8) -0.021(9) C9B 0.049(9) 0.053(8) 0.050(9) -0.009(7) 0.003(7) 0.005(7) C10B 0.074(11) 0.052(8) 0.041(9) -0.003(7) 0.012(8) -0.009(8) C11B 0.048(9) 0.059(9) 0.045(9) 0.000(7) 0.005(7) 0.006(7) C12B 0.077(11) 0.055(9) 0.039(9) -0.004(7) 0.002(9) 0.001(9) O13B 0.076(7) 0.069(6) 0.043(6) 0.003(5) -0.002(5) 0.008(6) C14B 0.061(9) 0.065(9) 0.046(9) -0.005(7) 0.007(7) 0.000(8) C15B 0.070(10) 0.060(9) 0.052(9) -0.003(7) 0.010(8) 0.003(8) C16B 0.098(13) 0.080(11) 0.077(12) -0.020(9) -0.003(11) -0.003(10) C17B 0.27(3) 0.043(9) 0.103(16) -0.008(9) -0.032(17) 0.010(14) C18B 0.16(2) 0.099(13) 0.074(13) -0.011(10) -0.060(13) -0.014(13) O19B 0.090(8) 0.092(8) 0.043(6) 0.008(5) 0.007(6) -0.005(6) C20B 0.092(13) 0.073(11) 0.045(9) 0.004(8) 0.003(9) -0.011(10) C21B 0.056(10) 0.079(12) 0.081(12) 0.008(10) 0.003(8) -0.031(10) C22B 0.095(15) 0.084(14) 0.109(16) 0.028(11) -0.032(12) -0.019(12) C23B 0.085(14) 0.054(11) 0.137(17) 0.047(11) 0.018(13) 0.014(10) C24B 0.061(10) 0.082(12) 0.061(10) 0.003(9) 0.003(8) -0.005(10) C25B 0.084(12) 0.064(10) 0.053(10) 0.002(7) -0.024(9) -0.022(10) C26B 0.093(13) 0.154(18) 0.026(10) -0.020(10) 0.009(9) 0.013(13) C27B 0.062(11) 0.22(2) 0.044(12) 0.028(15) -0.017(9) 0.020(15) C28B 0.102(13) 0.123(14) 0.031(9) 0.012(9) 0.002(9) 0.032(11) B1C 0.079(13) 0.042(9) 0.057(12) -0.003(8) -0.026(11) 0.003(9) O2C 0.178(17) 0.29(2) 0.036(8) 0.000(10) 0.006(10) 0.158(18) C3C 0.084(17) 0.38(5) 0.10(2) 0.14(3) 0.007(15) -0.01(2) C4C 0.061(11) 0.093(12) 0.090(14) 0.013(10) 0.009(9) 0.026(10) N5C 0.064(8) 0.043(6) 0.048(7) 0.002(5) 0.009(6) 0.000(6) C6C 0.099(12) 0.078(11) 0.046(10) -0.001(8) -0.004(9) 0.011(9) C7C 0.062(10) 0.068(10) 0.056(11) -0.004(8) 0.011(8) 0.012(8) C8C 0.063(9) 0.065(10) 0.039(9) 0.000(8) -0.004(7) -0.008(8) C9C 0.036(7) 0.054(9) 0.055(9) 0.001(7) 0.006(7) 0.000(7) C10C 0.060(9) 0.059(8) 0.045(9) 0.002(7) -0.011(7) 0.008(7) C11C 0.060(9) 0.062(9) 0.041(9) 0.002(7) 0.012(7) 0.012(8) C12C 0.066(10) 0.067(10) 0.043(10) -0.004(8) 0.000(8) 0.004(8) O13C 0.085(7) 0.087(7) 0.037(6) -0.013(5) 0.001(5) 0.031(6) C14C 0.085(12) 0.062(9) 0.036(9) 0.003(7) -0.002(7) 0.026(8) C15C 0.055(10) 0.090(11) 0.046(9) -0.004(8) -0.005(7) 0.005(8) C16C 0.081(12) 0.090(11) 0.051(10) 0.000(9) -0.008(8) -0.003(10) C17C 0.107(15) 0.108(14) 0.092(14) 0.009(11) 0.017(11) -0.034(12) C18C 0.090(13) 0.134(16) 0.074(12) -0.007(11) 0.018(10) 0.005(12) O19C 0.084(7) 0.077(7) 0.038(6) 0.003(5) 0.000(5) 0.018(5) C20C 0.15(2) 0.19(3) 0.15(2) 0.006(19) 0.085(19) 0.09(2) C21C 0.14(2) 0.099(16) 0.16(2) -0.015(15) -0.021(18) -0.013(16) C22C 0.21(3) 0.114(19) 0.20(3) 0.016(19) -0.03(2) -0.09(2) C23C 0.22(4) 0.11(2) 0.32(5) 0.04(3) -0.10(4) -0.11(2) C24C 0.14(2) 0.086(16) 0.24(3) -0.006(17) -0.01(2) -0.091(17) C25C 0.31(5) 0.20(3) 0.21(4) -0.11(3) 0.01(3) 0.05(4) C26C 0.085(13) 0.106(14) 0.069(12) 0.001(10) -0.023(10) 0.014(11) C27C 0.092(16) 0.134(18) 0.126(18) 0.014(15) -0.021(13) 0.064(14) C28C 0.094(13) 0.066(10) 0.090(13) -0.006(9) -0.008(11) 0.020(9) B1D 0.082(13) 0.042(9) 0.050(11) -0.001(8) -0.018(10) 0.001(9) O2D 0.088(8) 0.084(7) 0.066(7) -0.003(6) -0.001(6) 0.023(6) C3D 0.18(2) 0.136(18) 0.110(17) 0.058(14) 0.065(17) 0.103(17) C4D 0.086(11) 0.058(9) 0.057(10) 0.004(8) 0.012(8) -0.002(9) N5D 0.071(8) 0.048(6) 0.041(7) -0.008(5) -0.014(6) 0.008(6) C6D 0.076(11) 0.056(9) 0.080(11) -0.019(8) -0.015(9) 0.016(8) C7D 0.073(11) 0.056(9) 0.056(10) 0.004(7) -0.013(8) 0.014(9) C8D 0.061(10) 0.058(10) 0.053(9) -0.004(7) -0.007(8) 0.013(9) C9D 0.051(10) 0.065(10) 0.045(9) -0.003(7) -0.003(7) 0.020(8) C10D 0.052(10) 0.064(9) 0.050(9) 0.007(7) -0.010(7) 0.000(8) C11D 0.080(12) 0.052(9) 0.036(8) -0.007(6) 0.012(7) 0.031(8) C12D 0.055(10) 0.052(9) 0.054(9) 0.007(7) 0.006(7) -0.001(8) O13D 0.075(7) 0.057(6) 0.072(7) -0.007(5) 0.007(6) 0.008(6) C14D 0.085(11) 0.062(9) 0.034(8) 0.007(7) 0.000(7) -0.015(8) C15D 0.075(10) 0.064(9) 0.052(10) 0.008(7) 0.022(8) 0.026(8) C16D 0.120(15) 0.079(11) 0.048(10) 0.005(8) 0.022(10) 0.024(10) C17D 0.38(4) 0.081(13) 0.063(13) 0.030(10) 0.047(19) 0.05(2) C18D 0.16(2) 0.19(2) 0.077(15) 0.038(14) -0.052(14) 0.000(19) O19D 0.081(7) 0.069(7) 0.085(8) -0.036(6) -0.016(6) 0.031(6) C20D 0.067(11) 0.075(10) 0.082(13) -0.030(10) 0.004(9) 0.001(9) C21D 0.113(16) 0.098(14) 0.110(16) -0.048(13) 0.041(13) -0.014(12) C22D 0.18(2) 0.090(16) 0.17(3) -0.019(15) 0.09(2) -0.057(16) C23D 0.20(3) 0.091(18) 0.18(3) 0.022(19) 0.09(3) 0.026(19) C24D 0.25(3) 0.080(15) 0.113(19) 0.027(14) 0.04(2) 0.010(18) C25D 0.119(15) 0.089(13) 0.073(13) 0.034(10) 0.018(12) 0.009(11) C26D 0.115(14) 0.062(10) 0.070(12) 0.005(8) 0.018(10) -0.003(10) C27D 0.140(17) 0.114(16) 0.084(15) -0.028(12) 0.001(13) 0.005(14) C28D 0.081(11) 0.060(9) 0.059(10) -0.008(7) -0.016(9) 0.003(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1A O2A 1.439(19) . ? B1A O13A 1.461(18) . ? B1A C20A 1.62(2) . ? B1A N5A 1.67(2) . ? O2A C3A 1.37(2) . ? C3A C4A 1.52(3) . ? C4A C26A 1.54(2) . ? C4A N5A 1.550(17) . ? N5A C6A 1.499(17) . ? N5A C28A 1.519(16) . ? C6A C7A 1.513(18) . ? C7A C8A 1.393(18) . ? C7A C12A 1.407(17) . ? C8A O19A 1.373(16) . ? C8A C9A 1.398(19) . ? C9A C10A 1.383(18) . ? C9A C14D 1.513(18) . ? C10A C11A 1.397(17) . ? C11A C12A 1.379(17) . ? C11A C14A 1.539(17) . ? C12A O13A 1.378(15) . ? C14A C9B 1.503(18) . ? C14A C15A 1.547(18) . ? C15A C16E 1.478(15) . ? C15A C16A 1.488(16) . ? C16A C18A 1.491(16) . ? C16A C17A 1.496(16) . ? C16E C18E 1.485(16) . ? C16E C17E 1.501(16) . ? C20A C21A 1.34(2) . ? C20A C25A 1.41(2) . ? C21A C22A 1.41(2) . ? C22A C23A 1.36(3) . ? C23A C24A 1.35(3) . ? C24A C25A 1.34(2) . ? C26A C27A 1.48(2) . ? C27A C28A 1.51(2) . ? B1B O2B 1.45(2) . ? B1B O13B 1.451(19) . ? B1B N5B 1.63(2) . ? B1B C20B 1.64(2) . ? O2B C3B 1.411(19) . ? C3B C4B 1.49(2) . ? C4B C26B 1.50(2) . ? C4B N5B 1.528(18) . ? N5B C6B 1.488(18) . ? N5B C28B 1.564(19) . ? C6B C7B 1.497(19) . ? C7B C12B 1.372(19) . ? C7B C8B 1.422(19) . ? C8B O19B 1.377(16) . ? C8B C9B 1.388(18) . ? C9B C10B 1.407(18) . ? C10B C11B 1.385(18) . ? C11B C12B 1.425(18) . ? C11B C14B 1.517(18) . ? C12B O13B 1.372(17) . ? C14B C15B 1.513(18) . ? C14B C9C 1.539(18) . ? C15B C16B 1.54(2) . ? C16B C18B 1.50(2) . ? C16B C17B 1.58(2) . ? C20B C21B 1.36(2) . ? C20B C25B 1.42(2) . ? C21B C22B 1.40(2) . ? C22B C23B 1.41(2) . ? C23B C24B 1.35(2) . ? C24B C25B 1.38(2) . ? C26B C27B 1.45(3) . ? C27B C28B 1.49(2) . ? B1C O2C 1.34(2) . ? B1C O13C 1.419(19) . ? B1C N5C 1.655(19) . ? B1C C20C 1.73(2) . ? O2C C3C 1.42(3) . ? C3C C4C 1.54(3) . ? C4C C26C 1.50(2) . ? C4C N5C 1.499(19) . ? N5C C6C 1.482(17) . ? N5C C28C 1.507(17) . ? C6C C7C 1.53(2) . ? C7C C12C 1.384(19) . ? C7C C8C 1.420(19) . ? C8C O19C 1.380(16) . ? C8C C9C 1.395(18) . ? C9C C10C 1.404(17) . ? C10C C11C 1.436(18) . ? C11C C12C 1.371(18) . ? C11C C14C 1.497(18) . ? C12C O13C 1.363(16) . ? C14C C15C 1.519(19) . ? C14C C9D 1.56(2) . ? C15C C16C 1.52(2) . ? C16C C18C 1.51(2) . ? C16C C17C 1.56(2) . ? C20C C21C 1.3900 . ? C20C C25C 1.3900 . ? C21C C22C 1.3900 . ? C22C C23C 1.3900 . ? C23C C24C 1.3900 . ? C24C C25C 1.3900 . ? C26C C27C 1.45(3) . ? C27C C28C 1.55(3) . ? B1D O2D 1.428(18) . ? B1D O13D 1.513(18) . ? B1D N5D 1.59(2) . ? B1D C20D 1.683(19) . ? O2D C3D 1.43(2) . ? C3D C4D 1.51(2) . ? C4D C26D 1.50(2) . ? C4D N5D 1.546(17) . ? N5D C6D 1.481(17) . ? N5D C28D 1.523(16) . ? C6D C7D 1.511(19) . ? C7D C12D 1.398(19) . ? C7D C8D 1.409(19) . ? C8D O19D 1.366(16) . ? C8D C9D 1.385(18) . ? C9D C10D 1.367(18) . ? C10D C11D 1.446(19) . ? C11D C12D 1.393(18) . ? C11D C14D 1.537(19) . ? C12D O13D 1.319(16) . ? C14D C15D 1.551(18) . ? C15D C16D 1.52(2) . ? C16D C18D 1.52(3) . ? C16D C17D 1.58(3) . ? C20D C21D 1.3900 . ? C20D C25D 1.3900 . ? C21D C22D 1.3900 . ? C22D C23D 1.3900 . ? C23D C24D 1.3900 . ? C24D C25D 1.3900 . ? C26D C27D 1.49(2) . ? C27D C28D 1.58(2) . ? O201 C202 1.198(13) . ? C202 C203 1.451(14) . ? C202 C204 1.454(14) . ? O211 C212 1.188(14) . ? C212 C213 1.449(14) . ? C212 C214 1.488(14) . ? O221 C222 1.188(15) . ? C222 C223 1.452(15) . ? C222 C224 1.466(15) . ? O231 C232 1.224(15) . ? C232 C234 1.452(15) . ? C232 C233 1.457(15) . ? O241 C242 1.211(16) . ? C242 C243 1.44(3) . ? C242 C244 1.466(16) . ? 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 O2A B1A O13A 114.4(12) . . ? O2A B1A C20A 111.1(12) . . ? O13A B1A C20A 108.7(12) . . ? O2A B1A N5A 100.6(11) . . ? O13A B1A N5A 108.3(11) . . ? C20A B1A N5A 113.7(11) . . ? C3A O2A B1A 114.4(13) . . ? O2A C3A C4A 108.1(17) . . ? C3A C4A C26A 122.5(19) . . ? C3A C4A N5A 104.7(13) . . ? C26A C4A N5A 105.4(12) . . ? C6A N5A C28A 110.3(10) . . ? C6A N5A C4A 110.2(10) . . ? C28A N5A C4A 105.9(10) . . ? C6A N5A B1A 110.5(10) . . ? C28A N5A B1A 115.2(10) . . ? C4A N5A B1A 104.5(10) . . ? N5A C6A C7A 110.7(10) . . ? C8A C7A C12A 120.6(12) . . ? C8A C7A C6A 125.1(12) . . ? C12A C7A C6A 114.3(12) . . ? O19A C8A C9A 123.0(12) . . ? O19A C8A C7A 116.9(12) . . ? C9A C8A C7A 120.1(13) . . ? C10A C9A C8A 117.5(12) . . ? C10A C9A C14D 122.3(13) . . ? C8A C9A C14D 120.2(13) . . ? C9A C10A C11A 123.9(12) . . ? C12A C11A C10A 117.6(12) . . ? C12A C11A C14A 118.7(11) . . ? C10A C11A C14A 123.7(12) . . ? O13A C12A C11A 122.6(12) . . ? O13A C12A C7A 117.2(11) . . ? C11A C12A C7A 120.2(12) . . ? C12A O13A B1A 118.3(10) . . ? C9B C14A C11A 110.6(10) . . ? C9B C14A C15A 115.1(11) . . ? C11A C14A C15A 112.4(11) . . ? C16E C15A C16A 73.3(17) . . ? C16E C15A C14A 119.0(13) . . ? C16A C15A C14A 116.3(13) . . ? C15A C16A C18A 115(2) . . ? C15A C16A C17A 109(2) . . ? C18A C16A C17A 109(3) . . ? C15A C16E C18E 114.2(18) . . ? C15A C16E C17E 118(2) . . ? C18E C16E C17E 113(3) . . ? C21A C20A C25A 116.8(14) . . ? C21A C20A B1A 122.0(14) . . ? C25A C20A B1A 121.2(14) . . ? C20A C21A C22A 121.2(17) . . ? C23A C22A C21A 120.6(19) . . ? C24A C23A C22A 118.0(19) . . ? C25A C24A C23A 121.8(19) . . ? C24A C25A C20A 121.6(17) . . ? C27A C26A C4A 107.0(15) . . ? C26A C27A C28A 105.2(15) . . ? C27A C28A N5A 105.9(11) . . ? O2B B1B O13B 114.2(13) . . ? O2B B1B N5B 100.0(12) . . ? O13B B1B N5B 108.5(13) . . ? O2B B1B C20B 111.4(14) . . ? O13B B1B C20B 107.1(12) . . ? N5B B1B C20B 115.8(13) . . ? C3B O2B B1B 106.9(13) . . ? O2B C3B C4B 107.2(13) . . ? C26B C4B C3B 115.3(16) . . ? C26B C4B N5B 102.9(13) . . ? C3B C4B N5B 103.3(12) . . ? C6B N5B C4B 112.3(12) . . ? C6B N5B C28B 108.1(12) . . ? C4B N5B C28B 104.8(11) . . ? C6B N5B B1B 111.6(11) . . ? C4B N5B B1B 105.0(12) . . ? C28B N5B B1B 114.9(11) . . ? N5B C6B C7B 108.7(12) . . ? C12B C7B C8B 118.4(13) . . ? C12B C7B C6B 117.5(13) . . ? C8B C7B C6B 124.0(13) . . ? O19B C8B C9B 121.7(14) . . ? O19B C8B C7B 117.3(12) . . ? C9B C8B C7B 121.0(12) . . ? C8B C9B C10B 117.1(13) . . ? C8B C9B C14A 122.2(12) . . ? C10B C9B C14A 120.8(12) . . ? C11B C10B C9B 125.3(13) . . ? C10B C11B C12B 114.4(12) . . ? C10B C11B C14B 125.3(12) . . ? C12B C11B C14B 120.3(13) . . ? O13B C12B C7B 117.0(12) . . ? O13B C12B C11B 119.0(13) . . ? C7B C12B C11B 123.7(14) . . ? C12B O13B B1B 122.2(11) . . ? C15B C14B C11B 112.6(11) . . ? C15B C14B C9C 113.6(11) . . ? C11B C14B C9C 108.9(11) . . ? C14B C15B C16B 111.6(12) . . ? C18B C16B C15B 111.6(14) . . ? C18B C16B C17B 112.3(16) . . ? C15B C16B C17B 108.1(14) . . ? C21B C20B C25B 116.0(15) . . ? C21B C20B B1B 121.5(15) . . ? C25B C20B B1B 122.4(15) . . ? C20B C21B C22B 124.7(16) . . ? C23B C22B C21B 116.6(17) . . ? C24B C23B C22B 120.3(16) . . ? C23B C24B C25B 121.5(15) . . ? C24B C25B C20B 120.8(14) . . ? C27B C26B C4B 107.0(15) . . ? C26B C27B C28B 101.0(15) . . ? C27B C28B N5B 103.7(13) . . ? O2C B1C O13C 115.9(15) . . ? O2C B1C N5C 100.9(13) . . ? O13C B1C N5C 109.3(11) . . ? O2C B1C C20C 120.7(17) . . ? O13C B1C C20C 100.6(14) . . ? N5C B1C C20C 109.4(12) . . ? B1C O2C C3C 105.7(18) . . ? O2C C3C C4C 110.5(17) . . ? C26C C4C N5C 105.8(13) . . ? C26C C4C C3C 115.9(17) . . ? N5C C4C C3C 100.5(16) . . ? C6C N5C C4C 114.7(11) . . ? C6C N5C C28C 108.1(11) . . ? C4C N5C C28C 107.1(11) . . ? C6C N5C B1C 111.1(12) . . ? C4C N5C B1C 102.2(11) . . ? C28C N5C B1C 113.6(10) . . ? N5C C6C C7C 109.2(11) . . ? C12C C7C C8C 120.2(13) . . ? C12C C7C C6C 121.4(13) . . ? C8C C7C C6C 118.4(13) . . ? O19C C8C C9C 123.4(12) . . ? O19C C8C C7C 115.7(12) . . ? C9C C8C C7C 120.9(13) . . ? C8C C9C C10C 116.7(12) . . ? C8C C9C C14B 120.7(12) . . ? C10C C9C C14B 122.5(12) . . ? C9C C10C C11C 123.3(12) . . ? C12C C11C C10C 117.1(12) . . ? C12C C11C C14C 122.1(12) . . ? C10C C11C C14C 120.5(12) . . ? O13C C12C C11C 119.9(12) . . ? O13C C12C C7C 118.3(13) . . ? C11C C12C C7C 121.8(13) . . ? C12C O13C B1C 128.2(11) . . ? C11C C14C C15C 117.1(12) . . ? C11C C14C C9D 112.4(11) . . ? C15C C14C C9D 112.6(11) . . ? C16C C15C C14C 115.6(12) . . ? C15C C16C C18C 113.6(14) . . ? C15C C16C C17C 108.2(13) . . ? C18C C16C C17C 108.7(14) . . ? C21C C20C C25C 120.0 . . ? C21C C20C B1C 122.8(13) . . ? C25C C20C B1C 117.0(13) . . ? C22C C21C C20C 120.0 . . ? C21C C22C C23C 120.0 . . ? C24C C23C C22C 120.0 . . ? C23C C24C C25C 120.0 . . ? C24C C25C C20C 120.0 . . ? C27C C26C C4C 107.8(15) . . ? C26C C27C C28C 107.2(15) . . ? N5C C28C C27C 100.5(13) . . ? O2D B1D O13D 113.5(11) . . ? O2D B1D N5D 102.4(11) . . ? O13D B1D N5D 109.2(12) . . ? O2D B1D C20D 112.7(13) . . ? O13D B1D C20D 107.7(11) . . ? N5D B1D C20D 111.3(10) . . ? B1D O2D C3D 106.7(14) . . ? O2D C3D C4D 108.5(13) . . ? C26D C4D C3D 118.1(16) . . ? C26D C4D N5D 106.6(11) . . ? C3D C4D N5D 104.0(12) . . ? C6D N5D C28D 109.2(10) . . ? C6D N5D C4D 114.0(11) . . ? C28D N5D C4D 102.9(10) . . ? C6D N5D B1D 112.7(10) . . ? C28D N5D B1D 114.8(11) . . ? C4D N5D B1D 102.9(10) . . ? N5D C6D C7D 110.5(11) . . ? C12D C7D C8D 120.2(13) . . ? C12D C7D C6D 118.7(14) . . ? C8D C7D C6D 120.5(13) . . ? O19D C8D C9D 121.7(13) . . ? O19D C8D C7D 118.9(12) . . ? C9D C8D C7D 119.4(13) . . ? C10D C9D C8D 120.6(13) . . ? C10D C9D C14C 118.8(12) . . ? C8D C9D C14C 120.6(12) . . ? C9D C10D C11D 121.2(13) . . ? C12D C11D C10D 117.4(12) . . ? C12D C11D C14D 120.1(14) . . ? C10D C11D C14D 122.4(12) . . ? O13D C12D C7D 119.7(12) . . ? O13D C12D C11D 119.2(13) . . ? C7D C12D C11D 120.6(14) . . ? C12D O13D B1D 124.1(11) . . ? C9A C14D C11D 112.1(11) . . ? C9A C14D C15D 113.9(11) . . ? C11D C14D C15D 110.9(11) . . ? C16D C15D C14D 112.6(12) . . ? C18D C16D C15D 111.0(14) . . ? C18D C16D C17D 109.1(19) . . ? C15D C16D C17D 108.2(14) . . ? C21D C20D C25D 120.0 . . ? C21D C20D B1D 122.2(10) . . ? C25D C20D B1D 117.6(10) . . ? C22D C21D C20D 120.0 . . ? C21D C22D C23D 120.0 . . ? C22D C23D C24D 120.0 . . ? C25D C24D C23D 120.0 . . ? C24D C25D C20D 120.0 . . ? C27D C26D C4D 110.0(13) . . ? C26D C27D C28D 101.3(14) . . ? N5D C28D C27D 104.6(12) . . ? O201 C202 C203 119.7(16) . . ? O201 C202 C204 120.6(15) . . ? C203 C202 C204 119.6(16) . . ? O211 C212 C213 121.8(19) . . ? O211 C212 C214 121.2(17) . . ? C213 C212 C214 117.0(18) . . ? O221 C222 C223 119(2) . . ? O221 C222 C224 118.3(17) . . ? C223 C222 C224 122(2) . . ? O231 C232 C234 119.3(17) . . ? O231 C232 C233 126(2) . . ? C234 C232 C233 115.0(19) . . ? O241 C242 C243 121(2) . . ? O241 C242 C244 118(2) . . ? C243 C242 C244 120(2) . . ? 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 O13A B1A O2A C3A 90(2) . . . . ? C20A B1A O2A C3A -146.7(19) . . . . ? N5A B1A O2A C3A -26(2) . . . . ? B1A O2A C3A C4A 31(3) . . . . ? O2A C3A C4A C26A 100(2) . . . . ? O2A C3A C4A N5A -20(2) . . . . ? C3A C4A N5A C6A -114.4(17) . . . . ? C26A C4A N5A C6A 115.2(15) . . . . ? C3A C4A N5A C28A 126.3(17) . . . . ? C26A C4A N5A C28A -4.1(17) . . . . ? C3A C4A N5A B1A 4.3(18) . . . . ? C26A C4A N5A B1A -126.1(14) . . . . ? O2A B1A N5A C6A 129.8(11) . . . . ? O13A B1A N5A C6A 9.6(14) . . . . ? C20A B1A N5A C6A -111.3(13) . . . . ? O2A B1A N5A C28A -104.4(12) . . . . ? O13A B1A N5A C28A 135.4(12) . . . . ? C20A B1A N5A C28A 14.5(17) . . . . ? O2A B1A N5A C4A 11.3(12) . . . . ? O13A B1A N5A C4A -109.0(12) . . . . ? C20A B1A N5A C4A 130.1(13) . . . . ? C28A N5A C6A C7A 178.9(11) . . . . ? C4A N5A C6A C7A 62.3(13) . . . . ? B1A N5A C6A C7A -52.6(14) . . . . ? N5A C6A C7A C8A -128.6(13) . . . . ? N5A C6A C7A C12A 49.4(15) . . . . ? C12A C7A C8A O19A -178.1(12) . . . . ? C6A C7A C8A O19A 0(2) . . . . ? C12A C7A C8A C9A 0(2) . . . . ? C6A C7A C8A C9A 178.2(12) . . . . ? O19A C8A C9A C10A -179.6(12) . . . . ? C7A C8A C9A C10A 2.2(19) . . . . ? O19A C8A C9A C14D 0(2) . . . . ? C7A C8A C9A C14D -177.8(12) . . . . ? C8A C9A C10A C11A -2.7(19) . . . . ? C14D C9A C10A C11A 177.3(12) . . . . ? C9A C10A C11A C12A 0.6(18) . . . . ? C9A C10A C11A C14A 179.0(12) . . . . ? C10A C11A C12A O13A 179.0(10) . . . . ? C14A C11A C12A O13A 0.5(17) . . . . ? C10A C11A C12A C7A 2.1(17) . . . . ? C14A C11A C12A C7A -176.5(11) . . . . ? C8A C7A C12A O13A -179.6(11) . . . . ? C6A C7A C12A O13A 2.3(16) . . . . ? C8A C7A C12A C11A -2.5(19) . . . . ? C6A C7A C12A C11A 179.4(11) . . . . ? C11A C12A O13A B1A 130.7(13) . . . . ? C7A C12A O13A B1A -52.3(15) . . . . ? O2A B1A O13A C12A -68.1(16) . . . . ? C20A B1A O13A C12A 167.1(10) . . . . ? N5A B1A O13A C12A 43.1(15) . . . . ? C12A C11A C14A C9B 89.1(13) . . . . ? C10A C11A C14A C9B -89.3(14) . . . . ? C12A C11A C14A C15A -140.8(11) . . . . ? C10A C11A C14A C15A 40.8(16) . . . . ? C9B C14A C15A C16E -71(2) . . . . ? C11A C14A C15A C16E 161.5(17) . . . . ? C9B C14A C15A C16A -155.4(16) . . . . ? C11A C14A C15A C16A 76.8(18) . . . . ? C16E C15A C16A C18A -70(3) . . . . ? C14A C15A C16A C18A 45(3) . . . . ? C16E C15A C16A C17A 54(3) . . . . ? C14A C15A C16A C17A 168(2) . . . . ? C16A C15A C16E C18E 73(3) . . . . ? C14A C15A C16E C18E -38(3) . . . . ? C16A C15A C16E C17E -62(3) . . . . ? C14A C15A C16E C17E -174(2) . . . . ? O2A B1A C20A C21A -161.9(14) . . . . ? O13A B1A C20A C21A -35.3(19) . . . . ? N5A B1A C20A C21A 85.5(18) . . . . ? O2A B1A C20A C25A 17.6(19) . . . . ? O13A B1A C20A C25A 144.3(13) . . . . ? N5A B1A C20A C25A -95.0(15) . . . . ? C25A C20A C21A C22A 1(2) . . . . ? B1A C20A C21A C22A -179.7(16) . . . . ? C20A C21A C22A C23A 1(3) . . . . ? C21A C22A C23A C24A -2(3) . . . . ? C22A C23A C24A C25A 3(3) . . . . ? C23A C24A C25A C20A -1(3) . . . . ? C21A C20A C25A C24A -1(2) . . . . ? B1A C20A C25A C24A 179.9(14) . . . . ? C3A C4A C26A C27A -135.3(19) . . . . ? N5A C4A C26A C27A -16(2) . . . . ? C4A C26A C27A C28A 30(2) . . . . ? C26A C27A C28A N5A -33.0(19) . . . . ? C6A N5A C28A C27A -96.7(15) . . . . ? C4A N5A C28A C27A 22.5(16) . . . . ? B1A N5A C28A C27A 137.4(14) . . . . ? O13B B1B O2B C3B 77.9(17) . . . . ? N5B B1B O2B C3B -37.7(14) . . . . ? C20B B1B O2B C3B -160.6(13) . . . . ? B1B O2B C3B C4B 44.5(17) . . . . ? O2B C3B C4B C26B 82.3(17) . . . . ? O2B C3B C4B N5B -29.1(17) . . . . ? C26B C4B N5B C6B 123.5(13) . . . . ? C3B C4B N5B C6B -116.2(14) . . . . ? C26B C4B N5B C28B 6.5(16) . . . . ? C3B C4B N5B C28B 126.7(14) . . . . ? C26B C4B N5B B1B -115.1(13) . . . . ? C3B C4B N5B B1B 5.2(15) . . . . ? O2B B1B N5B C6B 140.6(12) . . . . ? O13B B1B N5B C6B 20.8(17) . . . . ? C20B B1B N5B C6B -99.6(15) . . . . ? O2B B1B N5B C4B 18.8(13) . . . . ? O13B B1B N5B C4B -101.1(13) . . . . ? C20B B1B N5B C4B 138.5(13) . . . . ? O2B B1B N5B C28B -95.9(14) . . . . ? O13B B1B N5B C28B 144.3(13) . . . . ? C20B B1B N5B C28B 23.9(19) . . . . ? C4B N5B C6B C7B 61.9(15) . . . . ? C28B N5B C6B C7B 177.0(12) . . . . ? B1B N5B C6B C7B -55.7(16) . . . . ? N5B C6B C7B C12B 46.9(18) . . . . ? N5B C6B C7B C8B -135.3(13) . . . . ? C12B C7B C8B O19B -179.5(12) . . . . ? C6B C7B C8B O19B 3(2) . . . . ? C12B C7B C8B C9B 0(2) . . . . ? C6B C7B C8B C9B -178.2(13) . . . . ? O19B C8B C9B C10B -178.6(12) . . . . ? C7B C8B C9B C10B 2.4(19) . . . . ? O19B C8B C9B C14A 1.8(19) . . . . ? C7B C8B C9B C14A -177.2(12) . . . . ? C11A C14A C9B C8B -94.4(14) . . . . ? C15A C14A C9B C8B 136.9(13) . . . . ? C11A C14A C9B C10B 86.0(14) . . . . ? C15A C14A C9B C10B -42.7(16) . . . . ? C8B C9B C10B C11B -2.1(19) . . . . ? C14A C9B C10B C11B 177.5(12) . . . . ? C9B C10B C11B C12B -0.2(19) . . . . ? C9B C10B C11B C14B -178.6(13) . . . . ? C8B C7B C12B O13B -176.4(11) . . . . ? C6B C7B C12B O13B 1.5(19) . . . . ? C8B C7B C12B C11B -2(2) . . . . ? C6B C7B C12B C11B 175.8(13) . . . . ? C10B C11B C12B O13B 176.6(11) . . . . ? C14B C11B C12B O13B -4.9(18) . . . . ? C10B C11B C12B C7B 2.3(19) . . . . ? C14B C11B C12B C7B -179.1(12) . . . . ? C7B C12B O13B B1B -43.6(18) . . . . ? C11B C12B O13B B1B 141.8(14) . . . . ? O2B B1B O13B C12B -80.7(18) . . . . ? N5B B1B O13B C12B 29.8(17) . . . . ? C20B B1B O13B C12B 155.4(12) . . . . ? C10B C11B C14B C15B 45.0(18) . . . . ? C12B C11B C14B C15B -133.3(13) . . . . ? C10B C11B C14B C9C -82.0(16) . . . . ? C12B C11B C14B C9C 99.7(14) . . . . ? C11B C14B C15B C16B 63.6(16) . . . . ? C9C C14B C15B C16B -171.9(12) . . . . ? C14B C15B C16B C18B 65.2(18) . . . . ? C14B C15B C16B C17B -170.8(16) . . . . ? O2B B1B C20B C21B -169.0(13) . . . . ? O13B B1B C20B C21B -43(2) . . . . ? N5B B1B C20B C21B 77.7(18) . . . . ? O2B B1B C20B C25B 9(2) . . . . ? O13B B1B C20B C25B 135.0(14) . . . . ? N5B B1B C20B C25B -103.9(17) . . . . ? C25B C20B C21B C22B 1(2) . . . . ? B1B C20B C21B C22B 179.1(15) . . . . ? C20B C21B C22B C23B -1(3) . . . . ? C21B C22B C23B C24B 1(3) . . . . ? C22B C23B C24B C25B 0(3) . . . . ? C23B C24B C25B C20B -1(2) . . . . ? C21B C20B C25B C24B 1(2) . . . . ? B1B C20B C25B C24B -177.9(14) . . . . ? C3B C4B C26B C27B -144.5(16) . . . . ? N5B C4B C26B C27B -32.9(18) . . . . ? C4B C26B C27B C28B 46.3(17) . . . . ? C26B C27B C28B N5B -40.0(16) . . . . ? C6B N5B C28B C27B -99.4(15) . . . . ? C4B N5B C28B C27B 20.4(17) . . . . ? B1B N5B C28B C27B 135.2(14) . . . . ? O13C B1C O2C C3C 74(2) . . . . ? N5C B1C O2C C3C -43.9(19) . . . . ? C20C B1C O2C C3C -164.4(18) . . . . ? B1C O2C C3C C4C 33(3) . . . . ? O2C C3C C4C C26C 110(2) . . . . ? O2C C3C C4C N5C -4(3) . . . . ? C26C C4C N5C C6C 98.1(14) . . . . ? C3C C4C N5C C6C -140.9(17) . . . . ? C26C C4C N5C C28C -21.9(16) . . . . ? C3C C4C N5C C28C 99.1(17) . . . . ? C26C C4C N5C B1C -141.5(13) . . . . ? C3C C4C N5C B1C -20.6(17) . . . . ? O2C B1C N5C C6C 164.2(15) . . . . ? O13C B1C N5C C6C 41.7(16) . . . . ? C20C B1C N5C C6C -67.5(14) . . . . ? O2C B1C N5C C4C 41.4(16) . . . . ? O13C B1C N5C C4C -81.2(15) . . . . ? C20C B1C N5C C4C 169.6(12) . . . . ? O2C B1C N5C C28C -73.6(17) . . . . ? O13C B1C N5C C28C 163.8(13) . . . . ? C20C B1C N5C C28C 54.6(17) . . . . ? C4C N5C C6C C7C 62.0(16) . . . . ? C28C N5C C6C C7C -178.6(12) . . . . ? B1C N5C C6C C7C -53.3(15) . . . . ? N5C C6C C7C C12C 35.3(19) . . . . ? N5C C6C C7C C8C -146.2(13) . . . . ? C12C C7C C8C O19C 178.9(12) . . . . ? C6C C7C C8C O19C 0.3(19) . . . . ? C12C C7C C8C C9C -1(2) . . . . ? C6C C7C C8C C9C -179.1(13) . . . . ? O19C C8C C9C C10C -176.8(12) . . . . ? C7C C8C C9C C10C 2.5(18) . . . . ? O19C C8C C9C C14B 5.1(19) . . . . ? C7C C8C C9C C14B -175.5(12) . . . . ? C15B C14B C9C C8C 145.8(13) . . . . ? C11B C14B C9C C8C -87.7(14) . . . . ? C15B C14B C9C C10C -32.1(18) . . . . ? C11B C14B C9C C10C 94.3(14) . . . . ? C8C C9C C10C C11C -1.9(19) . . . . ? C14B C9C C10C C11C 176.1(12) . . . . ? C9C C10C C11C C12C -1(2) . . . . ? C9C C10C C11C C14C 173.6(13) . . . . ? C10C C11C C12C O13C 180.0(12) . . . . ? C14C C11C C12C O13C 6(2) . . . . ? C10C C11C C12C C7C 3(2) . . . . ? C14C C11C C12C C7C -171.3(13) . . . . ? C8C C7C C12C O13C -179.5(12) . . . . ? C6C C7C C12C O13C -1(2) . . . . ? C8C C7C C12C C11C -2(2) . . . . ? C6C C7C C12C C11C 176.2(14) . . . . ? C11C C12C O13C B1C 169.5(15) . . . . ? C7C C12C O13C B1C -13(2) . . . . ? O2C B1C O13C C12C -120.3(18) . . . . ? N5C B1C O13C C12C -7(2) . . . . ? C20C B1C O13C C12C 107.8(15) . . . . ? C12C C11C C14C C15C -144.9(14) . . . . ? C10C C11C C14C C15C 41.0(19) . . . . ? C12C C11C C14C C9D 82.4(16) . . . . ? C10C C11C C14C C9D -91.7(15) . . . . ? C11C C14C C15C C16C 55.8(17) . . . . ? C9D C14C C15C C16C -171.6(12) . . . . ? C14C C15C C16C C18C 52.5(18) . . . . ? C14C C15C C16C C17C 173.2(13) . . . . ? O2C B1C C20C C21C -168.2(14) . . . . ? O13C B1C C20C C21C -39.3(17) . . . . ? N5C B1C C20C C21C 75.6(16) . . . . ? O2C B1C C20C C25C 6.4(18) . . . . ? O13C B1C C20C C25C 135.3(11) . . . . ? N5C B1C C20C C25C -109.8(13) . . . . ? C25C C20C C21C C22C 0.0 . . . . ? B1C C20C C21C C22C 174.4(16) . . . . ? C20C C21C C22C C23C 0.0 . . . . ? C21C C22C C23C C24C 0.0 . . . . ? C22C C23C C24C C25C 0.0 . . . . ? C23C C24C C25C C20C 0.0 . . . . ? C21C C20C C25C C24C 0.0 . . . . ? B1C C20C C25C C24C -174.8(15) . . . . ? N5C C4C C26C C27C 0.8(19) . . . . ? C3C C4C C26C C27C -110(2) . . . . ? C4C C26C C27C C28C 20(2) . . . . ? C6C N5C C28C C27C -91.7(15) . . . . ? C4C N5C C28C C27C 32.4(16) . . . . ? B1C N5C C28C C27C 144.4(14) . . . . ? C26C C27C C28C N5C -32.2(19) . . . . ? O13D B1D O2D C3D 77.4(17) . . . . ? N5D B1D O2D C3D -40.2(15) . . . . ? C20D B1D O2D C3D -159.8(13) . . . . ? B1D O2D C3D C4D 32(2) . . . . ? O2D C3D C4D C26D 108.4(18) . . . . ? O2D C3D C4D N5D -9(2) . . . . ? C26D C4D N5D C6D 98.0(14) . . . . ? C3D C4D N5D C6D -136.4(15) . . . . ? C26D C4D N5D C28D -20.1(15) . . . . ? C3D C4D N5D C28D 105.4(16) . . . . ? C26D C4D N5D B1D -139.6(13) . . . . ? C3D C4D N5D B1D -14.1(16) . . . . ? O2D B1D N5D C6D 156.1(11) . . . . ? O13D B1D N5D C6D 35.6(14) . . . . ? C20D B1D N5D C6D -83.2(13) . . . . ? O2D B1D N5D C28D -78.0(13) . . . . ? O13D B1D N5D C28D 161.4(10) . . . . ? C20D B1D N5D C28D 42.7(15) . . . . ? O2D B1D N5D C4D 32.9(13) . . . . ? O13D B1D N5D C4D -87.7(12) . . . . ? C20D B1D N5D C4D 153.6(11) . . . . ? C28D N5D C6D C7D 176.8(12) . . . . ? C4D N5D C6D C7D 62.4(15) . . . . ? B1D N5D C6D C7D -54.4(16) . . . . ? N5D C6D C7D C12D 33.6(18) . . . . ? N5D C6D C7D C8D -137.4(13) . . . . ? C12D C7D C8D O19D -174.2(12) . . . . ? C6D C7D C8D O19D -3.3(19) . . . . ? C12D C7D C8D C9D 8(2) . . . . ? C6D C7D C8D C9D 178.5(13) . . . . ? O19D C8D C9D C10D 178.8(12) . . . . ? C7D C8D C9D C10D -3(2) . . . . ? O19D C8D C9D C14C -2.8(19) . . . . ? C7D C8D C9D C14C 175.3(12) . . . . ? C11C C14C C9D C10D 84.5(15) . . . . ? C15C C14C C9D C10D -50.4(16) . . . . ? C11C C14C C9D C8D -94.0(15) . . . . ? C15C C14C C9D C8D 131.2(13) . . . . ? C8D C9D C10D C11D -1(2) . . . . ? C14C C9D C10D C11D -179.4(12) . . . . ? C9D C10D C11D C12D 0.4(19) . . . . ? C9D C10D C11D C14D -176.7(12) . . . . ? C8D C7D C12D O13D 179.8(12) . . . . ? C6D C7D C12D O13D 8.8(19) . . . . ? C8D C7D C12D C11D -8(2) . . . . ? C6D C7D C12D C11D -179.2(12) . . . . ? C10D C11D C12D O13D 176.1(12) . . . . ? C14D C11D C12D O13D -6.7(18) . . . . ? C10D C11D C12D C7D 4.0(18) . . . . ? C14D C11D C12D C7D -178.8(12) . . . . ? C7D C12D O13D B1D -30.5(18) . . . . ? C11D C12D O13D B1D 157.3(12) . . . . ? O2D B1D O13D C12D -106.3(16) . . . . ? N5D B1D O13D C12D 7.3(17) . . . . ? C20D B1D O13D C12D 128.2(13) . . . . ? C10A C9A C14D C11D 88.3(15) . . . . ? C8A C9A C14D C11D -91.8(16) . . . . ? C10A C9A C14D C15D -38.7(19) . . . . ? C8A C9A C14D C15D 141.3(13) . . . . ? C12D C11D C14D C9A 100.0(15) . . . . ? C10D C11D C14D C9A -82.9(15) . . . . ? C12D C11D C14D C15D -131.4(13) . . . . ? C10D C11D C14D C15D 45.7(17) . . . . ? C9A C14D C15D C16D -167.3(13) . . . . ? C11D C14D C15D C16D 65.1(16) . . . . ? C14D C15D C16D C18D 71.2(18) . . . . ? C14D C15D C16D C17D -169.1(17) . . . . ? O2D B1D C20D C21D 26.6(15) . . . . ? O13D B1D C20D C21D 152.5(9) . . . . ? N5D B1D C20D C21D -87.8(12) . . . . ? O2D B1D C20D C25D -159.1(10) . . . . ? O13D B1D C20D C25D -33.1(14) . . . . ? N5D B1D C20D C25D 86.5(12) . . . . ? C25D C20D C21D C22D 0.0 . . . . ? B1D C20D C21D C22D 174.2(11) . . . . ? C20D C21D C22D C23D 0.0 . . . . ? C21D C22D C23D C24D 0.0 . . . . ? C22D C23D C24D C25D 0.0 . . . . ? C23D C24D C25D C20D 0.0 . . . . ? C21D C20D C25D C24D 0.0 . . . . ? B1D C20D C25D C24D -174.5(11) . . . . ? C3D C4D C26D C27D -120.2(18) . . . . ? N5D C4D C26D C27D -4(2) . . . . ? C4D C26D C27D C28D 25(2) . . . . ? C6D N5D C28D C27D -86.0(14) . . . . ? C4D N5D C28D C27D 35.4(15) . . . . ? B1D N5D C28D C27D 146.4(13) . . . . ? C26D C27D C28D N5D -37.5(17) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.677 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.101 #====================================================================== _eof