# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'RSC Advances' _journal_coden_cambridge 1500 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email tianjunmian@hotmail.com _publ_contact_author_name 'Jun-Mian Tian' loop_ _publ_author_name 'Weidong Zhang' 'Jun-Mian Tian' 'Si-Sheng Ou-Yang' 'Xu Zhang' 'Ying-Tong Di' 'Hualiang Jiang' 'Honglin Li' 'Weixing Dai' 'Keyv Chen' 'Maili Liu' 'Xiao-Jiang Hao' 'Yun-Heng Shen' 'Cheng Luo' data_f80122c _database_code_depnum_ccdc_archive 'CCDC 787350' #TrackingRef 'tunicyclin E.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H62 N8 O15' _chemical_formula_weight 834.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.798(17) _cell_length_b 15.09(2) _cell_length_c 27.46(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4473(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 804 _cell_measurement_theta_min 2.435 _cell_measurement_theta_max 16.480 _exptl_crystal_description column _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.097 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9808 _exptl_absorpt_correction_T_max 0.9904 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17448 _diffrn_reflns_av_R_equivalents 0.0791 _diffrn_reflns_av_sigmaI/netI 0.0837 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 26.49 _reflns_number_total 5080 _reflns_number_gt 2491 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2000)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1303P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _chemical_absolute_configuration unk _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0(10) _refine_ls_number_reflns 5080 _refine_ls_number_parameters 604 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.1705 _refine_ls_R_factor_gt 0.0810 _refine_ls_wR_factor_ref 0.2354 _refine_ls_wR_factor_gt 0.1884 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.33440(8) 0.09921(6) 0.53352(4) 0.0654(3) Uani 1 1 d . . . O2 O 0.33510(9) 0.34247(7) 0.46446(5) 0.0981(4) Uani 1 1 d . . . O3 O 0.47954(12) 0.47386(12) 0.35589(4) 0.1266(6) Uani 1 1 d . . . O4 O 0.62516(11) 0.26106(6) 0.32100(3) 0.0746(4) Uani 1 1 d . . . O5 O 0.77402(10) 0.19715(9) 0.22765(4) 0.0977(4) Uani 1 1 d . . . O6 O 0.73821(16) -0.06839(8) 0.29856(5) 0.1336(6) Uani 1 1 d . . . O7 O 0.46478(9) 0.05954(8) 0.38094(3) 0.0773(4) Uani 1 1 d . . . O8 O 0.67361(9) 0.29627(6) 0.53827(4) 0.0712(3) Uani 1 1 d . . . H8X H 0.7162 0.2513 0.5374 0.107 Uiso 1 1 calc R . . O9 O 0.68647(11) 0.19842(6) 0.41127(3) 0.0736(3) Uani 1 1 d . . . H9X H 0.6444 0.2157 0.3883 0.110 Uiso 1 1 calc R . . N1 N 0.56571(10) 0.01840(6) 0.44895(4) 0.0517(3) Uani 1 1 d . . . N2 N 0.48293(9) 0.17297(6) 0.49236(3) 0.0453(3) Uani 1 1 d D . . H2Z H 0.5264(9) 0.1717(7) 0.4661(3) 0.052(3) Uiso 1 1 d D . . N3 N 0.53191(9) 0.38409(6) 0.46987(3) 0.0463(3) Uani 1 1 d D . . H3Z H 0.6012(7) 0.3774(6) 0.4816(3) 0.031(3) Uiso 1 1 d D . . N4 N 0.66158(11) 0.41548(7) 0.37744(3) 0.0590(4) Uani 1 1 d D . . H4Z H 0.7137(9) 0.4022(7) 0.4006(3) 0.069(4) Uiso 1 1 d D . . N5 N 0.62722(13) 0.34619(9) 0.25341(4) 0.0765(4) Uani 1 1 d D . . H5Z H 0.6693(7) 0.3877(3) 0.2393(3) 0.079(4) Uiso 1 1 d D . . N6 N 0.60129(12) 0.11365(9) 0.23152(4) 0.0794(4) Uani 1 1 d D . . H6Z H 0.5260(4) 0.1006(3) 0.2386(2) 0.103(5) Uiso 1 1 d D . . N7 N 0.66398(11) 0.06318(7) 0.32393(4) 0.0661(4) Uani 1 1 d D . . H7Z H 0.6261(10) 0.1113(5) 0.3199(3) 0.082(4) Uiso 1 1 d D . . N8 N 0.52652(13) 0.58316(10) 0.59052(4) 0.0952(5) Uani 1 1 d . . . H8Z H 0.5359 0.5742 0.6212 0.114 Uiso 1 1 calc R . . C1 C 0.45234(13) 0.01424(8) 0.47794(5) 0.0574(4) Uani 1 1 d . . . H1 H 0.3831 -0.0058 0.4576 0.069 Uiso 1 1 calc R . . C2 C 0.48483(16) -0.05667(9) 0.51529(7) 0.0903(6) Uani 1 1 d . . . H2A H 0.4397 -0.0473 0.5454 0.108 Uiso 1 1 calc R . . H2B H 0.4656 -0.1153 0.5029 0.108 Uiso 1 1 calc R . . C3 C 0.6170(2) -0.04671(15) 0.52293(8) 0.1356(8) Uani 1 1 d . . . H3A H 0.6524 -0.1016 0.5350 0.163 Uiso 1 1 calc R . . H3B H 0.6332 -0.0002 0.5465 0.163 Uiso 1 1 calc R . . C4 C 0.67267(15) -0.02299(11) 0.47416(5) 0.0767(5) Uani 1 1 d . . . H4A H 0.7407 0.0185 0.4777 0.092 Uiso 1 1 calc R . . H4B H 0.7015 -0.0753 0.4570 0.092 Uiso 1 1 calc R . . C5 C 0.41849(12) 0.09959(8) 0.50359(4) 0.0472(4) Uani 1 1 d . . . C6 C 0.46029(12) 0.25685(7) 0.51784(4) 0.0463(4) Uani 1 1 d . . . H6 H 0.3821 0.2488 0.5354 0.056 Uiso 1 1 calc R . . C7 C 0.55757(12) 0.27571(9) 0.55667(5) 0.0569(4) Uani 1 1 d . . . H7A H 0.5292 0.3247 0.5766 0.068 Uiso 1 1 calc R . . H7B H 0.5650 0.2241 0.5776 0.068 Uiso 1 1 calc R . . C8 C 0.43728(11) 0.33095(8) 0.48174(4) 0.0455(4) Uani 1 1 d . . . C9 C 0.51610(12) 0.46329(8) 0.44042(4) 0.0446(4) Uani 1 1 d . . . H9 H 0.4285 0.4802 0.4419 0.054 Uiso 1 1 calc R . . C10 C 0.59202(12) 0.54008(8) 0.46156(4) 0.0503(4) Uani 1 1 d . . . H10A H 0.6780 0.5218 0.4638 0.060 Uiso 1 1 calc R . . H10B H 0.5880 0.5898 0.4392 0.060 Uiso 1 1 calc R . . C11 C 0.54931(13) 0.57050(8) 0.51114(5) 0.0546(4) Uani 1 1 d . . . C12 C 0.45830(12) 0.63639(8) 0.51978(5) 0.0546(4) Uani 1 1 d . . . C13 C 0.38608(14) 0.68932(8) 0.49076(6) 0.0663(5) Uani 1 1 d . . . H13 H 0.3922 0.6862 0.4570 0.080 Uiso 1 1 calc R . . C14 C 0.30287(18) 0.74826(11) 0.51280(8) 0.1043(8) Uani 1 1 d . . . H14 H 0.2541 0.7849 0.4935 0.125 Uiso 1 1 calc R . . C15 C 0.29275(19) 0.75241(12) 0.56193(8) 0.1181(8) Uani 1 1 d . . . H15 H 0.2353 0.7910 0.5756 0.142 Uiso 1 1 calc R . . C16 C 0.36415(18) 0.70180(12) 0.59195(7) 0.1048(7) Uani 1 1 d . . . H16 H 0.3579 0.7061 0.6257 0.126 Uiso 1 1 calc R . . C17 C 0.44547(16) 0.64433(10) 0.57032(5) 0.0733(5) Uani 1 1 d . . . C18 C 0.58794(16) 0.54016(12) 0.55543(5) 0.0820(6) Uani 1 1 d . . . H18 H 0.6475 0.4965 0.5604 0.098 Uiso 1 1 calc R . . C19 C 0.54925(15) 0.44965(9) 0.38738(4) 0.0627(5) Uani 1 1 d . . . C20 C 0.70805(15) 0.41073(10) 0.32727(4) 0.0671(5) Uani 1 1 d . . . H20 H 0.6855 0.4657 0.3104 0.081 Uiso 1 1 calc R . . C21 C 0.84835(15) 0.40210(11) 0.32684(5) 0.0838(6) Uani 1 1 d . . . H21A H 0.8707 0.3480 0.3438 0.101 Uiso 1 1 calc R . . H21B H 0.8754 0.3960 0.2933 0.101 Uiso 1 1 calc RD . . C22 C 0.9178(2) 0.47771(14) 0.34954(6) 0.1220(8) Uani 1 1 d . . . H22 H 0.8984 0.4791 0.3844 0.146 Uiso 1 1 calc R . . C23 C 1.0570(2) 0.4577(2) 0.34361(10) 0.1901(13) Uani 1 1 d . . . H23A H 1.0685 0.3952 0.3388 0.285 Uiso 1 1 calc R . . H23B H 1.1004 0.4761 0.3724 0.285 Uiso 1 1 calc R . . H23C H 1.0886 0.4894 0.3160 0.285 Uiso 1 1 calc R . . C24 C 0.8893(4) 0.56720(15) 0.32836(11) 0.1974(16) Uani 1 1 d . . . H24A H 0.8982 0.5650 0.2936 0.296 Uiso 1 1 calc R . . H24B H 0.9456 0.6103 0.3415 0.296 Uiso 1 1 calc R . . H24C H 0.8059 0.5835 0.3365 0.296 Uiso 1 1 calc R . . C25 C 0.64788(15) 0.33339(10) 0.30076(4) 0.0631(5) Uani 1 1 d D . . C26 C 0.57588(15) 0.27375(10) 0.22383(5) 0.0723(5) Uani 1 1 d . . . H26 H 0.4943 0.2585 0.2370 0.087 Uiso 1 1 calc R . . C27 C 0.55809(19) 0.30701(15) 0.17088(5) 0.1021(7) Uani 1 1 d . . . H27 H 0.5157 0.3644 0.1727 0.123 Uiso 1 1 calc R . . C28 C 0.4747(2) 0.24525(18) 0.14344(7) 0.1446(11) Uani 1 1 d . . . H28A H 0.4622 0.2675 0.1110 0.217 Uiso 1 1 calc R . . H28B H 0.3964 0.2412 0.1598 0.217 Uiso 1 1 calc R . . H28C H 0.5121 0.1876 0.1419 0.217 Uiso 1 1 calc R . . C29 C 0.6768(2) 0.32171(17) 0.14399(6) 0.1242(9) Uani 1 1 d . . . H29A H 0.7212 0.2668 0.1416 0.186 Uiso 1 1 calc R . . H29B H 0.7263 0.3643 0.1612 0.186 Uiso 1 1 calc R . . H29C H 0.6591 0.3435 0.1119 0.186 Uiso 1 1 calc R . . C30 C 0.65888(15) 0.19260(11) 0.22829(4) 0.0721(5) Uani 1 1 d . . . C31 C 0.66470(18) 0.03135(11) 0.23759(5) 0.0878(6) Uani 1 1 d . . . H31A H 0.7428 0.0348 0.2202 0.105 Uiso 1 1 calc R . . H31B H 0.6158 -0.0148 0.2222 0.105 Uiso 1 1 calc R . . C32 C 0.69142(16) 0.00331(11) 0.28969(5) 0.0775(5) Uani 1 1 d . . . C33 C 0.68746(13) 0.04931(9) 0.37500(4) 0.0579(4) Uani 1 1 d D . . H33 H 0.7347 -0.0056 0.3794 0.070 Uiso 1 1 calc R . . C34 C 0.75995(13) 0.12662(9) 0.39630(5) 0.0637(5) Uani 1 1 d . . . H34A H 0.8071 0.1055 0.4240 0.076 Uiso 1 1 calc R . . H34B H 0.8185 0.1474 0.3721 0.076 Uiso 1 1 calc R . . C35 C 0.56239(13) 0.04123(8) 0.40130(5) 0.0563(4) Uani 1 1 d . . . O10 O 0.35480(15) 0.02846(9) 0.28820(5) 0.1430(6) Uani 1 1 d D . . H10X H 0.4256(3) 0.0080(2) 0.28595(17) 0.215 Uiso 1 1 d D . . H10Y H 0.3254(4) 0.0613(4) 0.31016(13) 0.215 Uiso 1 1 d D . . O11 O 0.96667(19) 0.32807(13) 0.20825(8) 0.2061(10) Uani 1 1 d D . . H11X H 0.9413(4) 0.2790(3) 0.2180(4) 0.309 Uiso 1 1 d D . . H11Y H 0.9612(5) 0.3782(3) 0.22123(16) 0.309 Uiso 1 1 d D . . O12 O 0.5889(2) 0.49624(19) 0.69020(6) 0.2382(12) Uani 1 1 d D . . H12X H 0.5362(5) 0.4562(3) 0.6864(4) 0.357 Uiso 1 1 d D . . H12Y H 0.6489(4) 0.5024(6) 0.7086(2) 0.357 Uiso 1 1 d D . . O13 O 0.8043(2) -0.21406(12) 0.24762(9) 0.2222(11) Uani 1 1 d D . . H13X H 0.8713(3) -0.1920(5) 0.2553(3) 0.333 Uiso 1 1 d D . . H13Y H 0.7773(4) -0.2258(3) 0.21974(11) 0.333 Uiso 1 1 d D . . O14 O 0.97618(17) 0.16234(19) 0.29350(8) 0.2172(11) Uani 1 1 d D . . H14X H 0.9056(4) 0.166(2) 0.2819(4) 0.326 Uiso 1 1 d D . . H14Y H 1.0460(4) 0.1814(3) 0.2874(4) 0.326 Uiso 1 1 d D . . O15 O 0.3148(3) 0.26664(19) 0.34925(12) 0.2197(19) Uani 0.50 1 d PD . . H15X H 0.3297(8) 0.3186(3) 0.3437(2) 0.330 Uiso 0.50 1 d PD . . H15Y H 0.3252(8) 0.2153(3) 0.3414(2) 0.330 Uiso 0.50 1 d PD . . O16 O 0.3468(6) 0.1386(2) 0.23202(17) 0.281(2) Uani 0.50 1 d PDU . . H16X H 0.3245(7) 0.0862(3) 0.23127(14) 0.422 Uiso 0.50 1 d PD . . H16Y H 0.3565(4) 0.1756(3) 0.2541(2) 0.422 Uiso 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0546(5) 0.0620(5) 0.0796(6) 0.0033(5) 0.0256(5) -0.0059(5) O2 0.0521(6) 0.0782(6) 0.1642(10) 0.0412(7) -0.0403(7) -0.0168(5) O3 0.0915(8) 0.2417(14) 0.0465(5) 0.0270(8) -0.0154(6) 0.0508(9) O4 0.1021(8) 0.0838(6) 0.0378(4) -0.0046(5) -0.0001(5) -0.0066(6) O5 0.0620(7) 0.1452(9) 0.0859(7) -0.0214(7) 0.0150(6) -0.0075(7) O6 0.1975(14) 0.1103(8) 0.0931(8) -0.0410(6) -0.0301(9) 0.0599(9) O7 0.0467(5) 0.1227(8) 0.0624(5) -0.0226(5) -0.0121(5) 0.0051(6) O8 0.0519(6) 0.0855(6) 0.0762(6) 0.0119(5) 0.0018(5) 0.0122(5) O9 0.1030(8) 0.0697(5) 0.0482(5) -0.0112(4) 0.0013(6) -0.0186(6) N1 0.0475(6) 0.0493(5) 0.0583(6) -0.0066(5) 0.0076(6) 0.0030(5) N2 0.0418(6) 0.0443(5) 0.0499(5) -0.0008(5) 0.0136(5) -0.0011(5) N3 0.0379(5) 0.0577(6) 0.0432(5) 0.0087(5) -0.0063(5) -0.0014(5) N4 0.0712(7) 0.0724(6) 0.0333(5) -0.0028(5) -0.0025(6) 0.0182(6) N5 0.0778(9) 0.1056(9) 0.0462(6) -0.0069(7) -0.0046(6) -0.0066(8) N6 0.0752(8) 0.1096(9) 0.0533(6) -0.0212(6) -0.0173(6) -0.0038(8) N7 0.0661(7) 0.0783(7) 0.0540(6) -0.0240(6) 0.0089(6) 0.0017(6) N8 0.0965(10) 0.1495(12) 0.0396(6) -0.0133(7) 0.0031(7) -0.0298(10) C1 0.0473(8) 0.0484(6) 0.0766(8) -0.0128(7) 0.0135(7) -0.0126(6) C2 0.1068(12) 0.0486(8) 0.1155(12) 0.0087(9) 0.0465(10) 0.0091(8) C3 0.1393(16) 0.1526(14) 0.1150(14) 0.0629(12) 0.0378(13) 0.0693(13) C4 0.0699(10) 0.0857(9) 0.0744(9) 0.0069(8) 0.0028(9) 0.0092(9) C5 0.0440(7) 0.0465(6) 0.0513(7) 0.0044(6) 0.0043(6) -0.0009(6) C6 0.0446(7) 0.0400(6) 0.0543(7) -0.0024(6) 0.0122(6) 0.0002(6) C7 0.0437(8) 0.0721(8) 0.0547(7) 0.0166(7) 0.0097(7) 0.0051(7) C8 0.0310(6) 0.0513(6) 0.0544(7) -0.0032(6) -0.0071(6) 0.0021(6) C9 0.0403(7) 0.0474(6) 0.0461(6) 0.0048(6) -0.0008(6) 0.0030(6) C10 0.0511(8) 0.0500(6) 0.0499(7) 0.0066(6) 0.0084(6) 0.0042(6) C11 0.0526(8) 0.0566(7) 0.0545(7) -0.0014(6) 0.0008(7) 0.0027(7) C12 0.0506(8) 0.0485(6) 0.0646(7) -0.0035(6) 0.0038(7) -0.0124(6) C13 0.0619(9) 0.0439(6) 0.0930(10) 0.0053(7) 0.0161(8) 0.0018(7) C14 0.0979(13) 0.0516(7) 0.1635(18) 0.0121(11) 0.0304(14) 0.0106(9) C15 0.1261(15) 0.0778(10) 0.1502(15) -0.0099(11) 0.0772(12) -0.0035(11) C16 0.1081(13) 0.1106(12) 0.0958(11) -0.0411(10) 0.0503(10) -0.0312(11) C17 0.0679(10) 0.0858(9) 0.0662(8) -0.0190(8) 0.0181(8) -0.0174(8) C18 0.0681(10) 0.1218(12) 0.0562(8) 0.0118(9) -0.0017(8) 0.0040(10) C19 0.0742(10) 0.0708(8) 0.0431(7) 0.0096(6) -0.0107(7) 0.0030(8) C20 0.0885(10) 0.0768(8) 0.0361(6) -0.0005(7) 0.0088(7) 0.0053(9) C21 0.0809(11) 0.1139(12) 0.0566(8) -0.0071(9) 0.0185(8) -0.0074(11) C22 0.1374(15) 0.1717(16) 0.0569(9) -0.0259(11) 0.0237(11) -0.0758(13) C23 0.1094(16) 0.325(3) 0.1361(19) -0.042(2) 0.0179(16) -0.1060(18) C24 0.303(4) 0.1248(16) 0.165(2) -0.0293(18) 0.011(3) -0.076(2) C25 0.0770(10) 0.0824(9) 0.0300(6) -0.0056(7) 0.0023(7) 0.0014(8) C26 0.0580(9) 0.1099(11) 0.0490(7) -0.0049(8) -0.0046(8) -0.0001(9) C27 0.1094(14) 0.1474(15) 0.0495(8) -0.0106(10) -0.0144(10) 0.0018(14) C28 0.1321(18) 0.210(2) 0.0920(12) -0.0253(16) -0.0515(12) -0.0012(18) C29 0.1292(17) 0.201(2) 0.0428(8) 0.0096(12) -0.0043(11) -0.0136(17) C30 0.0652(9) 0.1255(11) 0.0258(5) -0.0183(7) 0.0015(7) -0.0040(10) C31 0.0931(12) 0.1017(10) 0.0687(9) -0.0352(8) -0.0074(9) 0.0092(10) C32 0.0778(11) 0.0945(10) 0.0601(8) -0.0277(8) -0.0030(8) 0.0035(10) C33 0.0523(8) 0.0761(8) 0.0454(6) -0.0163(7) -0.0031(7) -0.0006(7) C34 0.0567(9) 0.0846(9) 0.0498(7) -0.0045(7) -0.0045(7) -0.0127(8) C35 0.0576(8) 0.0556(7) 0.0557(7) -0.0185(6) -0.0007(7) -0.0022(7) O10 0.1711(13) 0.1558(10) 0.1021(8) -0.0557(8) -0.0554(8) 0.0548(10) O11 0.1597(15) 0.2590(19) 0.1995(16) -0.0710(16) 0.0543(14) -0.0619(16) O12 0.244(2) 0.375(3) 0.0960(11) 0.0460(16) 0.0115(14) -0.074(2) O13 0.237(2) 0.1737(14) 0.256(2) -0.0580(15) 0.009(2) 0.0717(15) O14 0.1463(16) 0.315(3) 0.1900(17) 0.022(2) 0.0241(16) 0.0304(18) O15 0.103(2) 0.430(5) 0.127(2) -0.117(3) 0.0073(19) -0.083(3) O16 0.272(4) 0.270(4) 0.303(4) 0.019(4) -0.004(4) -0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C5 1.225(2) . ? O2 C8 1.214(2) . ? O3 C19 1.203(2) . ? O4 C25 1.249(2) . ? O5 C30 1.245(3) . ? O6 C32 1.218(3) . ? O7 C35 1.225(2) . ? O8 C7 1.386(2) . ? O8 H8X 0.8200 . ? O9 C34 1.404(2) . ? O9 H9X 0.8200 . ? N1 C35 1.354(3) . ? N1 C1 1.462(2) . ? N1 C4 1.484(2) . ? N2 C5 1.344(2) . ? N2 C6 1.467(2) . ? N2 H2Z 0.860(8) . ? N3 C8 1.339(2) . ? N3 C9 1.453(2) . ? N3 H3Z 0.821(8) . ? N4 C19 1.346(3) . ? N4 C20 1.468(3) . ? N4 H4Z 0.873(9) . ? N5 C25 1.333(3) . ? N5 C26 1.470(2) . ? N5 H5Z 0.866(6) . ? N6 C30 1.347(3) . ? N6 C31 1.428(3) . ? N6 H6Z 0.858(5) . ? N7 C32 1.337(2) . ? N7 C33 1.440(3) . ? N7 H7Z 0.841(8) . ? N8 C18 1.338(2) . ? N8 C17 1.388(3) . ? N8 H8Z 0.8600 . ? C1 C5 1.513(2) . ? C1 C2 1.523(3) . ? C1 H1 0.9800 . ? C2 C3 1.451(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.511(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C6 C8 1.515(2) . ? C6 C7 1.523(2) . ? C6 H6 0.9800 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C9 C19 1.513(3) . ? C9 C10 1.533(2) . ? C9 H9 0.9800 . ? C10 C11 1.509(3) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C18 1.365(3) . ? C11 C12 1.418(2) . ? C12 C13 1.371(2) . ? C12 C17 1.400(3) . ? C13 C14 1.402(3) . ? C13 H13 0.9300 . ? C14 C15 1.355(4) . ? C14 H14 0.9300 . ? C15 C16 1.363(3) . ? C15 H15 0.9300 . ? C16 C17 1.370(3) . ? C16 H16 0.9300 . ? C18 H18 0.9300 . ? C20 C21 1.521(3) . ? C20 C25 1.521(3) . ? C20 H20 0.9800 . ? C21 C22 1.501(3) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C24 1.502(4) . ? C22 C23 1.541(4) . ? C22 H22 0.9800 . ? C23 H23A 0.9599 . ? C23 H23B 0.9599 . ? C23 H23C 0.9599 . ? C24 H24A 0.9599 . ? C24 H24B 0.9599 . ? C24 H24C 0.9599 . ? C26 C30 1.522(3) . ? C26 C27 1.550(3) . ? C26 H26 0.9800 . ? C27 C29 1.496(3) . ? C27 C28 1.499(3) . ? C27 H27 0.9800 . ? C28 H28A 0.9599 . ? C28 H28B 0.9599 . ? C28 H28C 0.9599 . ? C29 H29A 0.9599 . ? C29 H29B 0.9599 . ? C29 H29C 0.9599 . ? C31 C32 1.519(3) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C33 C34 1.521(2) . ? C33 C35 1.536(3) . ? C33 H33 0.9800 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? O10 H10X 0.827(4) . ? O10 H10Y 0.843(5) . ? O11 H11X 0.834(6) . ? O11 H11Y 0.838(5) . ? O12 H12X 0.836(6) . ? O12 H12Y 0.827(6) . ? O13 H13X 0.824(5) . ? O13 H13Y 0.838(4) . ? O14 H14X 0.827(7) . ? O14 H14Y 0.824(5) . ? O15 H15X 0.815(5) . ? O15 H15Y 0.812(5) . ? O16 H16X 0.826(6) . ? O16 H16Y 0.831(6) . ? 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 C7 O8 H8X 109.5 . . ? C34 O9 H9X 109.5 . . ? C35 N1 C1 121.02(13) . . ? C35 N1 C4 125.34(12) . . ? C1 N1 C4 112.31(15) . . ? C5 N2 C6 121.01(13) . . ? C5 N2 H2Z 117.2(7) . . ? C6 N2 H2Z 120.7(7) . . ? C8 N3 C9 122.56(12) . . ? C8 N3 H3Z 121.7(6) . . ? C9 N3 H3Z 115.3(6) . . ? C19 N4 C20 121.14(11) . . ? C19 N4 H4Z 121.4(6) . . ? C20 N4 H4Z 116.9(6) . . ? C25 N5 C26 119.62(14) . . ? C25 N5 H5Z 117.0(5) . . ? C26 N5 H5Z 119.2(5) . . ? C30 N6 C31 123.74(17) . . ? C30 N6 H6Z 130.9(4) . . ? C31 N6 H6Z 103.2(4) . . ? C32 N7 C33 123.19(14) . . ? C32 N7 H7Z 126.7(6) . . ? C33 N7 H7Z 109.9(6) . . ? C18 N8 C17 110.32(15) . . ? C18 N8 H8Z 124.8 . . ? C17 N8 H8Z 124.8 . . ? N1 C1 C5 114.80(11) . . ? N1 C1 C2 101.78(13) . . ? C5 C1 C2 109.88(16) . . ? N1 C1 H1 110.0 . . ? C5 C1 H1 110.0 . . ? C2 C1 H1 110.0 . . ? C3 C2 C1 104.55(14) . . ? C3 C2 H2A 110.8 . . ? C1 C2 H2A 110.8 . . ? C3 C2 H2B 110.8 . . ? C1 C2 H2B 110.8 . . ? H2A C2 H2B 108.9 . . ? C2 C3 C4 106.72(17) . . ? C2 C3 H3A 110.4 . . ? C4 C3 H3A 110.4 . . ? C2 C3 H3B 110.4 . . ? C4 C3 H3B 110.4 . . ? H3A C3 H3B 108.6 . . ? N1 C4 C3 101.75(16) . . ? N1 C4 H4A 111.4 . . ? C3 C4 H4A 111.4 . . ? N1 C4 H4B 111.4 . . ? C3 C4 H4B 111.4 . . ? H4A C4 H4B 109.3 . . ? O1 C5 N2 122.82(12) . . ? O1 C5 C1 119.18(12) . . ? N2 C5 C1 118.00(14) . . ? N2 C6 C8 110.61(14) . . ? N2 C6 C7 112.34(12) . . ? C8 C6 C7 115.67(12) . . ? N2 C6 H6 105.8 . . ? C8 C6 H6 105.8 . . ? C7 C6 H6 105.8 . . ? O8 C7 C6 114.21(15) . . ? O8 C7 H7A 108.7 . . ? C6 C7 H7A 108.7 . . ? O8 C7 H7B 108.7 . . ? C6 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? O2 C8 N3 120.85(14) . . ? O2 C8 C6 120.72(12) . . ? N3 C8 C6 118.43(13) . . ? N3 C9 C19 113.32(12) . . ? N3 C9 C10 110.35(13) . . ? C19 C9 C10 109.91(11) . . ? N3 C9 H9 107.7 . . ? C19 C9 H9 107.7 . . ? C10 C9 H9 107.7 . . ? C11 C10 C9 114.08(12) . . ? C11 C10 H10A 108.7 . . ? C9 C10 H10A 108.7 . . ? C11 C10 H10B 108.7 . . ? C9 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? C18 C11 C12 107.34(14) . . ? C18 C11 C10 127.49(15) . . ? C12 C11 C10 125.17(12) . . ? C13 C12 C17 118.03(15) . . ? C13 C12 C11 134.85(15) . . ? C17 C12 C11 107.12(12) . . ? C12 C13 C14 118.89(18) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? C15 C14 C13 120.72(18) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 122.06(19) . . ? C14 C15 H15 119.0 . . ? C16 C15 H15 119.0 . . ? C15 C16 C17 117.1(2) . . ? C15 C16 H16 121.5 . . ? C17 C16 H16 121.5 . . ? C16 C17 N8 130.70(17) . . ? C16 C17 C12 123.20(15) . . ? N8 C17 C12 106.08(14) . . ? N8 C18 C11 109.13(18) . . ? N8 C18 H18 125.4 . . ? C11 C18 H18 125.4 . . ? O3 C19 N4 122.29(15) . . ? O3 C19 C9 120.15(16) . . ? N4 C19 C9 117.41(11) . . ? N4 C20 C21 110.61(12) . . ? N4 C20 C25 109.91(13) . . ? C21 C20 C25 110.87(14) . . ? N4 C20 H20 108.5 . . ? C21 C20 H20 108.5 . . ? C25 C20 H20 108.5 . . ? C22 C21 C20 115.44(16) . . ? C22 C21 H21A 108.4 . . ? C20 C21 H21A 108.4 . . ? C22 C21 H21B 108.4 . . ? C20 C21 H21B 108.4 . . ? H21A C21 H21B 107.5 . . ? C21 C22 C24 114.8(2) . . ? C21 C22 C23 107.1(2) . . ? C24 C22 C23 109.6(2) . . ? C21 C22 H22 108.4 . . ? C24 C22 H22 108.4 . . ? C23 C22 H22 108.4 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O4 C25 N5 121.84(14) . . ? O4 C25 C20 122.77(14) . . ? N5 C25 C20 115.28(14) . . ? N5 C26 C30 109.36(16) . . ? N5 C26 C27 108.92(16) . . ? C30 C26 C27 114.13(13) . . ? N5 C26 H26 108.1 . . ? C30 C26 H26 108.1 . . ? C27 C26 H26 108.1 . . ? C29 C27 C28 111.02(18) . . ? C29 C27 C26 113.88(17) . . ? C28 C27 C26 110.17(18) . . ? C29 C27 H27 107.1 . . ? C28 C27 H27 107.1 . . ? C26 C27 H27 107.1 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O5 C30 N6 120.71(16) . . ? O5 C30 C26 122.84(16) . . ? N6 C30 C26 116.41(17) . . ? N6 C31 C32 116.30(13) . . ? N6 C31 H31A 108.2 . . ? C32 C31 H31A 108.2 . . ? N6 C31 H31B 108.2 . . ? C32 C31 H31B 108.2 . . ? H31A C31 H31B 107.4 . . ? O6 C32 N7 123.44(16) . . ? O6 C32 C31 120.93(14) . . ? N7 C32 C31 115.59(16) . . ? N7 C33 C34 110.69(12) . . ? N7 C33 C35 108.32(13) . . ? C34 C33 C35 109.42(13) . . ? N7 C33 H33 109.5 . . ? C34 C33 H33 109.5 . . ? C35 C33 H33 109.5 . . ? O9 C34 C33 114.40(16) . . ? O9 C34 H34A 108.7 . . ? C33 C34 H34A 108.7 . . ? O9 C34 H34B 108.7 . . ? C33 C34 H34B 108.7 . . ? H34A C34 H34B 107.6 . . ? O7 C35 N1 121.42(13) . . ? O7 C35 C33 121.62(15) . . ? N1 C35 C33 116.82(13) . . ? H10X O10 H10Y 128.4(5) . . ? H11X O11 H11Y 129.9(7) . . ? H12X O12 H12Y 133.7(9) . . ? H13X O13 H13Y 128.6(7) . . ? H14X O14 H14Y 138.1(16) . . ? H15X O15 H15Y 147.2(8) . . ? H16X O16 H16Y 134.3(8) . . ? 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 C35 N1 C1 C5 -90.81(15) . . . . ? C4 N1 C1 C5 101.67(15) . . . . ? C35 N1 C1 C2 150.57(12) . . . . ? C4 N1 C1 C2 -16.95(14) . . . . ? N1 C1 C2 C3 32.26(16) . . . . ? C5 C1 C2 C3 -89.81(16) . . . . ? C1 C2 C3 C4 -36.61(19) . . . . ? C35 N1 C4 C3 -171.06(13) . . . . ? C1 N1 C4 C3 -4.18(16) . . . . ? C2 C3 C4 N1 25.24(18) . . . . ? C6 N2 C5 O1 3.61(18) . . . . ? C6 N2 C5 C1 -176.31(11) . . . . ? N1 C1 C5 O1 -170.71(11) . . . . ? C2 C1 C5 O1 -56.74(18) . . . . ? N1 C1 C5 N2 9.22(17) . . . . ? C2 C1 C5 N2 123.19(15) . . . . ? C5 N2 C6 C8 -127.84(13) . . . . ? C5 N2 C6 C7 101.24(17) . . . . ? N2 C6 C7 O8 70.08(15) . . . . ? C8 C6 C7 O8 -58.22(15) . . . . ? C9 N3 C8 O2 6.92(18) . . . . ? C9 N3 C8 C6 -172.22(10) . . . . ? N2 C6 C8 O2 83.49(15) . . . . ? C7 C6 C8 O2 -147.37(13) . . . . ? N2 C6 C8 N3 -97.37(13) . . . . ? C7 C6 C8 N3 31.78(16) . . . . ? C8 N3 C9 C19 -98.94(14) . . . . ? C8 N3 C9 C10 137.31(12) . . . . ? N3 C9 C10 C11 -65.28(16) . . . . ? C19 C9 C10 C11 169.03(11) . . . . ? C9 C10 C11 C18 89.9(2) . . . . ? C9 C10 C11 C12 -89.04(19) . . . . ? C18 C11 C12 C13 -179.29(16) . . . . ? C10 C11 C12 C13 -0.1(2) . . . . ? C18 C11 C12 C17 0.49(16) . . . . ? C10 C11 C12 C17 179.64(13) . . . . ? C17 C12 C13 C14 -0.3(2) . . . . ? C11 C12 C13 C14 179.47(15) . . . . ? C12 C13 C14 C15 -0.7(2) . . . . ? C13 C14 C15 C16 1.6(3) . . . . ? C14 C15 C16 C17 -1.5(3) . . . . ? C15 C16 C17 N8 -177.80(18) . . . . ? C15 C16 C17 C12 0.5(3) . . . . ? C18 N8 C17 C16 179.36(18) . . . . ? C18 N8 C17 C12 0.82(19) . . . . ? C13 C12 C17 C16 0.4(2) . . . . ? C11 C12 C17 C16 -179.46(15) . . . . ? C13 C12 C17 N8 179.04(13) . . . . ? C11 C12 C17 N8 -0.78(16) . . . . ? C17 N8 C18 C11 -0.5(2) . . . . ? C12 C11 C18 N8 0.02(18) . . . . ? C10 C11 C18 N8 -179.11(14) . . . . ? C20 N4 C19 O3 3.6(2) . . . . ? C20 N4 C19 C9 -171.94(12) . . . . ? N3 C9 C19 O3 131.33(15) . . . . ? C10 C9 C19 O3 -104.7(2) . . . . ? N3 C9 C19 N4 -53.03(16) . . . . ? C10 C9 C19 N4 70.95(18) . . . . ? C19 N4 C20 C21 159.45(14) . . . . ? C19 N4 C20 C25 -77.79(19) . . . . ? N4 C20 C21 C22 -61.19(18) . . . . ? C25 C20 C21 C22 176.62(13) . . . . ? C20 C21 C22 C24 -56.0(2) . . . . ? C20 C21 C22 C23 -177.89(16) . . . . ? C26 N5 C25 O4 0.2(2) . . . . ? C26 N5 C25 C20 176.57(13) . . . . ? N4 C20 C25 O4 -37.6(2) . . . . ? C21 C20 C25 O4 85.00(18) . . . . ? N4 C20 C25 N5 146.08(14) . . . . ? C21 C20 C25 N5 -91.32(16) . . . . ? C25 N5 C26 C30 -56.11(18) . . . . ? C25 N5 C26 C27 178.54(15) . . . . ? N5 C26 C27 C29 70.3(2) . . . . ? C30 C26 C27 C29 -52.2(2) . . . . ? N5 C26 C27 C28 -164.23(16) . . . . ? C30 C26 C27 C28 73.3(2) . . . . ? C31 N6 C30 O5 4.3(2) . . . . ? C31 N6 C30 C26 -177.73(12) . . . . ? N5 C26 C30 O5 -41.97(18) . . . . ? C27 C26 C30 O5 80.31(18) . . . . ? N5 C26 C30 N6 140.06(13) . . . . ? C27 C26 C30 N6 -97.66(16) . . . . ? C30 N6 C31 C32 88.03(19) . . . . ? C33 N7 C32 O6 0.3(3) . . . . ? C33 N7 C32 C31 -177.58(14) . . . . ? N6 C31 C32 O6 175.42(17) . . . . ? N6 C31 C32 N7 -6.6(2) . . . . ? C32 N7 C33 C34 127.88(18) . . . . ? C32 N7 C33 C35 -112.16(16) . . . . ? N7 C33 C34 O9 85.13(15) . . . . ? C35 C33 C34 O9 -34.17(16) . . . . ? C1 N1 C35 O7 0.36(18) . . . . ? C4 N1 C35 O7 166.17(13) . . . . ? C1 N1 C35 C33 176.25(10) . . . . ? C4 N1 C35 C33 -17.93(18) . . . . ? N7 C33 C35 O7 -11.04(18) . . . . ? C34 C33 C35 O7 109.71(17) . . . . ? N7 C33 C35 N1 173.07(11) . . . . ? C34 C33 C35 N1 -66.17(17) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H9X O4 0.82 1.98 2.734(4) 152.3 . N2 H2Z O9 0.860(8) 2.327(9) 3.152(4) 160.6(9) . N3 H3Z O8 0.821(8) 2.128(9) 2.761(3) 133.9(8) . N8 H8Z O12 0.86 2.30 3.108(4) 156.4 . N6 H6Z O10 0.858(5) 2.542(6) 3.340(4) 155.2(5) . N6 H6Z O16 0.858(5) 2.027(8) 2.774(8) 145.0(5) . N7 H7Z O4 0.841(8) 2.260(8) 3.016(5) 149.7(9) . C26 H26 O16 0.98 2.41 3.214(7) 138.5 . C28 H28B O16 0.96 2.57 3.227(6) 125.7 . C29 H29A O5 0.96 2.65 3.148(4) 113.0 . O10 H10X N6 0.827(4) 2.893(5) 3.340(4) 116.0(3) . O10 H10Y O7 0.843(5) 2.458(5) 2.849(4) 109.2(4) . O11 H11X O5 0.834(6) 2.204(5) 2.918(4) 143.7(5) . O16 H16X O10 0.826(6) 1.820(5) 2.268(5) 112.6(5) . O14 H14X O5 0.827(7) 2.113(11) 2.883(4) 154.7(14) . C10 H10A O1 0.97 2.49 3.359(4) 149.3 3_556 O8 H8X O2 0.82 1.91 2.725(3) 172.0 3_556 O12 H12Y O10 0.827(6) 2.273(6) 2.956(5) 140.1(6) 3_556 N3 H3Z O1 0.821(8) 2.576(8) 3.277(5) 144.1(8) 3_556 N4 H4Z O1 0.873(9) 2.229(9) 3.084(4) 166.1(10) 3_556 N5 H5Z O10 0.866(6) 2.268(6) 2.984(4) 140.1(6) 4_655 C24 H24C O16 0.96 2.63 3.226(8) 120.2 4_655 O12 H12X O14 0.836(6) 1.981(6) 2.721(5) 147.0(8) 3_456 O11 H11Y O12 0.838(5) 2.147(6) 2.762(5) 130.2(4) 2_664 O13 H13Y O15 0.838(4) 2.142(5) 2.968(5) 168.7(5) 4_645 C31 H31B O3 0.97 2.39 3.125(4) 132.6 4_645 O14 H14Y O13 0.824(5) 2.455(7) 3.221(4) 154.9(7) 4_755 O13 H13X O11 0.824(5) 2.039(6) 2.827(5) 159.9(7) 4_745 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.49 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.547 _refine_diff_density_min -0.211 _refine_diff_density_rms 0.064