data_q388m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H76 N5 O Y' _chemical_formula_weight 936.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Y' 'Y' -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.5198(8) _cell_length_b 12.3059(9) _cell_length_c 38.706(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.323(2) _cell_angle_gamma 90.00 _cell_volume 5265.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 187(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.181 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 1.150 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7064 _exptl_absorpt_correction_T_max 0.8428 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 187(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 '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 28954 _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_sigmaI/netI 0.0724 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 26.07 _reflns_number_total 10370 _reflns_number_gt 6810 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0651P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10370 _refine_ls_number_parameters 590 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0915 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1252 _refine_ls_wR_factor_gt 0.1100 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.15108(3) -0.57177(2) -0.113115(8) 0.03030(10) Uani 1 1 d . . . O O 0.28620(18) -0.47698(18) -0.13820(6) 0.0414(5) Uani 1 1 d . . . N1 N 0.1753(2) -0.41557(19) -0.07697(6) 0.0345(6) Uani 1 1 d . . . N2 N 0.0549(2) -0.60406(19) -0.06486(6) 0.0325(6) Uani 1 1 d . . . N3 N 0.3311(2) -0.6324(2) -0.07113(7) 0.0367(6) Uani 1 1 d . . . N4 N 0.2164(2) -0.74922(19) -0.13239(7) 0.0348(6) Uani 1 1 d . . . N5 N -0.0052(2) -0.58139(19) -0.16368(7) 0.0352(6) Uani 1 1 d . . . H100 H 0.0048 -0.6435 -0.1728 0.042 Uiso 1 1 d R . . C1 C 0.4082(3) -0.5976(3) -0.04020(9) 0.0460(9) Uani 1 1 d . . . H1 H 0.3960 -0.5358 -0.0278 0.055 Uiso 1 1 calc R . . C2 C 0.5079(3) -0.6653(3) -0.02901(10) 0.0530(10) Uani 1 1 d . . . H2 H 0.5730 -0.6571 -0.0086 0.064 Uiso 1 1 calc R . . C3 C 0.4913(3) -0.7471(3) -0.05428(10) 0.0513(9) Uani 1 1 d . . . H3 H 0.5428 -0.8055 -0.0541 0.062 Uiso 1 1 calc R . . C4 C 0.3825(3) -0.7251(3) -0.08010(8) 0.0372(7) Uani 1 1 d . . . C5 C 0.3204(3) -0.7816(3) -0.11182(9) 0.0399(8) Uani 1 1 d . . . H5 H 0.3552 -0.8440 -0.1181 0.048 Uiso 1 1 calc R . . C6 C 0.1657(3) -0.8166(2) -0.16378(8) 0.0368(7) Uani 1 1 d . . . C7 C 0.0779(3) -0.8947(2) -0.16222(9) 0.0434(8) Uani 1 1 d . . . C8 C 0.0341(3) -0.9610(3) -0.19239(10) 0.0501(9) Uani 1 1 d . . . H8 H -0.0241 -1.0133 -0.1922 0.060 Uiso 1 1 calc R . . C9 C 0.0750(3) -0.9509(3) -0.22233(10) 0.0491(9) Uani 1 1 d . . . H9 H 0.0462 -0.9976 -0.2417 0.059 Uiso 1 1 calc R . . C10 C 0.1581(3) -0.8722(3) -0.22382(9) 0.0450(8) Uani 1 1 d . . . H10 H 0.1847 -0.8660 -0.2443 0.054 Uiso 1 1 calc R . . C11 C 0.2033(3) -0.8013(3) -0.19479(9) 0.0401(8) Uani 1 1 d . . . C12 C 0.0358(3) -0.9094(3) -0.12867(10) 0.0515(9) Uani 1 1 d . . . H12 H 0.0426 -0.8387 -0.1166 0.062 Uiso 1 1 calc R . . C13 C -0.0952(3) -0.9459(3) -0.13665(11) 0.0652(11) Uani 1 1 d . . . H13A H -0.1028 -1.0188 -0.1458 0.098 Uiso 1 1 calc R . . H13B H -0.1457 -0.8983 -0.1542 0.098 Uiso 1 1 calc R . . H13C H -0.1198 -0.9435 -0.1149 0.098 Uiso 1 1 calc R . . C14 C 0.1160(4) -0.9890(3) -0.10238(11) 0.0719(12) Uani 1 1 d . . . H14A H 0.1988 -0.9662 -0.0971 0.108 Uiso 1 1 calc R . . H14B H 0.1076 -1.0602 -0.1129 0.108 Uiso 1 1 calc R . . H14C H 0.0922 -0.9908 -0.0805 0.108 Uiso 1 1 calc R . . C15 C 0.2927(3) -0.7135(3) -0.19770(9) 0.0501(9) Uani 1 1 d . . . H15 H 0.3020 -0.6639 -0.1773 0.060 Uiso 1 1 calc R . . C16 C 0.2475(4) -0.6470(3) -0.23237(11) 0.0743(12) Uani 1 1 d . . . H16A H 0.1710 -0.6145 -0.2332 0.111 Uiso 1 1 calc R . . H16B H 0.2382 -0.6938 -0.2528 0.111 Uiso 1 1 calc R . . H16C H 0.3051 -0.5910 -0.2328 0.111 Uiso 1 1 calc R . . C17 C 0.4165(3) -0.7618(4) -0.19532(12) 0.0767(13) Uani 1 1 d . . . H17A H 0.4091 -0.8135 -0.2144 0.115 Uiso 1 1 calc R . . H17B H 0.4474 -0.7976 -0.1725 0.115 Uiso 1 1 calc R . . H17C H 0.4709 -0.7049 -0.1975 0.115 Uiso 1 1 calc R . . C18 C 0.2226(3) -0.3143(3) -0.07412(9) 0.0434(8) Uani 1 1 d . . . H18 H 0.2589 -0.2842 -0.0905 0.052 Uiso 1 1 calc R . . C19 C 0.2105(3) -0.2607(3) -0.04379(9) 0.0439(8) Uani 1 1 d . . . H19 H 0.2354 -0.1904 -0.0366 0.053 Uiso 1 1 calc R . . C20 C 0.1543(3) -0.3324(3) -0.02655(9) 0.0433(8) Uani 1 1 d . . . H20 H 0.1344 -0.3201 -0.0052 0.052 Uiso 1 1 calc R . . C21 C 0.1327(3) -0.4274(2) -0.04710(8) 0.0331(7) Uani 1 1 d . . . C22 C 0.0745(3) -0.5245(3) -0.04240(8) 0.0377(7) Uani 1 1 d . . . H22 H 0.0487 -0.5316 -0.0218 0.045 Uiso 1 1 calc R . . C23 C -0.0064(3) -0.6985(2) -0.05615(8) 0.0351(7) Uani 1 1 d . . . C24 C 0.0576(3) -0.7737(3) -0.03076(9) 0.0460(8) Uani 1 1 d . . . C25 C -0.0055(3) -0.8640(3) -0.02364(10) 0.0563(10) Uani 1 1 d . . . H25 H 0.0349 -0.9146 -0.0067 0.068 Uiso 1 1 calc R . . C26 C -0.1247(3) -0.8797(3) -0.04088(10) 0.0545(10) Uani 1 1 d . . . H26 H -0.1641 -0.9415 -0.0362 0.065 Uiso 1 1 calc R . . C27 C -0.1871(3) -0.8037(3) -0.06546(9) 0.0465(9) Uani 1 1 d . . . H27 H -0.2689 -0.8142 -0.0767 0.056 Uiso 1 1 calc R . . C28 C -0.1303(3) -0.7123(2) -0.07366(8) 0.0366(7) Uani 1 1 d . . . C29 C 0.1893(3) -0.7583(3) -0.00940(11) 0.0600(11) Uani 1 1 d . . . H29 H 0.2207 -0.6947 -0.0191 0.072 Uiso 1 1 calc R . . C30 C 0.2677(3) -0.8555(3) -0.01215(11) 0.0691(12) Uani 1 1 d . . . H30A H 0.2587 -0.8716 -0.0370 0.104 Uiso 1 1 calc R . . H30B H 0.2432 -0.9173 -0.0008 0.104 Uiso 1 1 calc R . . H30C H 0.3509 -0.8389 -0.0004 0.104 Uiso 1 1 calc R . . C31 C 0.1993(4) -0.7359(4) 0.03068(12) 0.0925(16) Uani 1 1 d . . . H31A H 0.1747 -0.7993 0.0412 0.139 Uiso 1 1 calc R . . H31B H 0.1478 -0.6759 0.0324 0.139 Uiso 1 1 calc R . . H31C H 0.2815 -0.7184 0.0433 0.139 Uiso 1 1 calc R . . C32 C -0.2011(3) -0.6252(3) -0.09851(8) 0.0416(8) Uani 1 1 d . . . H32 H -0.1455 -0.5878 -0.1096 0.050 Uiso 1 1 calc R . . C33 C -0.3060(3) -0.6693(3) -0.12859(9) 0.0553(10) Uani 1 1 d . . . H33A H -0.3675 -0.6969 -0.1186 0.083 Uiso 1 1 calc R . . H33B H -0.2776 -0.7268 -0.1409 0.083 Uiso 1 1 calc R . . H33C H -0.3392 -0.6120 -0.1453 0.083 Uiso 1 1 calc R . . C34 C -0.2486(3) -0.5421(3) -0.07653(10) 0.0533(9) Uani 1 1 d . . . H34A H -0.1822 -0.5125 -0.0581 0.080 Uiso 1 1 calc R . . H34B H -0.3042 -0.5768 -0.0657 0.080 Uiso 1 1 calc R . . H34C H -0.2893 -0.4846 -0.0921 0.080 Uiso 1 1 calc R . . C35 C -0.1208(3) -0.5419(2) -0.18118(7) 0.0312(7) Uani 1 1 d . . . C36 C -0.1533(3) -0.4351(2) -0.17437(8) 0.0341(7) Uani 1 1 d . . . C37 C -0.2698(3) -0.3982(3) -0.19065(8) 0.0418(8) Uani 1 1 d . . . H37 H -0.2908 -0.3284 -0.1854 0.050 Uiso 1 1 calc R . . C38 C -0.3551(3) -0.4606(3) -0.21417(9) 0.0438(8) Uani 1 1 d . . . H38 H -0.4323 -0.4337 -0.2249 0.053 Uiso 1 1 calc R . . C39 C -0.3233(3) -0.5637(3) -0.22148(8) 0.0405(8) Uani 1 1 d . . . H39 H -0.3803 -0.6061 -0.2377 0.049 Uiso 1 1 calc R . . C40 C -0.2099(3) -0.6073(2) -0.20577(8) 0.0352(7) Uani 1 1 d . . . C41 C -0.0637(3) -0.3575(2) -0.15066(9) 0.0407(8) Uani 1 1 d . . . H41 H 0.0114 -0.3981 -0.1406 0.049 Uiso 1 1 calc R . . C42 C -0.1038(3) -0.3135(3) -0.11925(10) 0.0631(11) Uani 1 1 d . . . H42A H -0.1182 -0.3729 -0.1049 0.095 Uiso 1 1 calc R . . H42B H -0.1768 -0.2723 -0.1282 0.095 Uiso 1 1 calc R . . H42C H -0.0416 -0.2675 -0.1048 0.095 Uiso 1 1 calc R . . C43 C -0.0340(3) -0.2637(3) -0.17268(10) 0.0582(10) Uani 1 1 d . . . H43A H 0.0330 -0.2230 -0.1580 0.087 Uiso 1 1 calc R . . H43B H -0.1032 -0.2170 -0.1806 0.087 Uiso 1 1 calc R . . H43C H -0.0133 -0.2922 -0.1933 0.087 Uiso 1 1 calc R . . C44 C -0.1817(3) -0.7227(3) -0.21523(9) 0.0408(8) Uani 1 1 d . . . H44 H -0.1210 -0.7521 -0.1943 0.049 Uiso 1 1 calc R . . C45 C -0.2898(3) -0.7994(3) -0.22346(10) 0.0565(10) Uani 1 1 d . . . H45A H -0.3493 -0.7754 -0.2448 0.085 Uiso 1 1 calc R . . H45B H -0.3244 -0.7996 -0.2036 0.085 Uiso 1 1 calc R . . H45C H -0.2639 -0.8715 -0.2272 0.085 Uiso 1 1 calc R . . C46 C -0.1258(3) -0.7227(3) -0.24652(10) 0.0517(9) Uani 1 1 d . . . H46A H -0.0520 -0.6815 -0.2400 0.078 Uiso 1 1 calc R . . H46B H -0.1813 -0.6904 -0.2672 0.078 Uiso 1 1 calc R . . H46C H -0.1088 -0.7960 -0.2520 0.078 Uiso 1 1 calc R . . C47 C 0.4170(3) -0.4695(3) -0.12157(11) 0.0579(10) Uani 1 1 d . . . H47A H 0.4553 -0.5389 -0.1231 0.069 Uiso 1 1 calc R . . H47B H 0.4338 -0.4494 -0.0964 0.069 Uiso 1 1 calc R . . C48 C 0.4633(3) -0.3850(3) -0.14169(11) 0.0655(11) Uani 1 1 d . . . H48A H 0.5424 -0.4045 -0.1440 0.079 Uiso 1 1 calc R . . H48B H 0.4687 -0.3149 -0.1299 0.079 Uiso 1 1 calc R . . C49 C 0.3710(4) -0.3830(4) -0.17768(11) 0.0708(12) Uani 1 1 d . . . H49A H 0.3883 -0.4380 -0.1935 0.085 Uiso 1 1 calc R . . H49B H 0.3685 -0.3124 -0.1890 0.085 Uiso 1 1 calc R . . C50 C 0.2543(3) -0.4068(3) -0.16928(10) 0.0541(10) Uani 1 1 d . . . H50A H 0.2175 -0.3403 -0.1640 0.065 Uiso 1 1 calc R . . H50B H 0.1979 -0.4428 -0.1894 0.065 Uiso 1 1 calc R . . C51 C 0.5369(5) -0.0749(4) -0.16103(17) 0.0897(15) Uani 1 1 d . . . C52 C 0.6018(5) -0.0792(4) -0.12458(17) 0.0970(17) Uani 1 1 d . . . H52 H 0.6859 -0.0798 -0.1180 0.116 Uiso 1 1 calc R . . C53 C 0.5415(7) -0.0824(5) -0.0984(2) 0.123(2) Uani 1 1 d . . . H53 H 0.5874 -0.0831 -0.0744 0.148 Uiso 1 1 calc R . . C54 C 0.4266(7) -0.0846(4) -0.1052(2) 0.118(2) Uani 1 1 d . . . H54 H 0.3891 -0.0909 -0.0869 0.141 Uiso 1 1 calc R . . C55 C 0.3577(5) -0.0769(4) -0.14228(17) 0.0963(17) Uani 1 1 d . . . H55 H 0.2737 -0.0755 -0.1479 0.116 Uiso 1 1 calc R . . C56 C 0.4114(4) -0.0714(3) -0.16983(15) 0.0797(14) Uani 1 1 d . . . H56 H 0.3650 -0.0655 -0.1937 0.096 Uiso 1 1 calc R . . C57 C 0.5958(5) -0.0739(4) -0.19010(17) 0.120(2) Uani 1 1 d . . . H57A H 0.5705 -0.0106 -0.2048 0.179 Uiso 1 1 calc R . . H57B H 0.5734 -0.1380 -0.2046 0.179 Uiso 1 1 calc R . . H57C H 0.6820 -0.0723 -0.1799 0.179 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 Y1 0.03016(17) 0.03301(17) 0.02664(16) -0.00040(13) 0.00619(12) 0.00033(14) O 0.0348(12) 0.0507(13) 0.0388(13) 0.0082(10) 0.0106(11) 0.0005(10) N1 0.0378(15) 0.0359(15) 0.0304(14) -0.0002(11) 0.0106(12) -0.0044(12) N2 0.0369(14) 0.0317(14) 0.0288(14) 0.0041(11) 0.0090(12) -0.0006(11) N3 0.0325(14) 0.0423(16) 0.0304(15) 0.0000(12) 0.0008(12) -0.0031(12) N4 0.0333(14) 0.0359(15) 0.0343(15) -0.0020(11) 0.0083(12) 0.0029(12) N5 0.0355(14) 0.0349(14) 0.0339(15) -0.0031(11) 0.0073(12) 0.0032(12) C1 0.040(2) 0.056(2) 0.037(2) 0.0014(16) 0.0035(17) -0.0037(17) C2 0.0341(19) 0.076(3) 0.041(2) 0.0068(19) -0.0018(17) -0.0057(19) C3 0.0346(19) 0.065(2) 0.051(2) 0.0128(19) 0.0062(17) 0.0098(18) C4 0.0316(17) 0.046(2) 0.0352(19) 0.0065(15) 0.0106(15) 0.0025(15) C5 0.0379(19) 0.0405(19) 0.045(2) 0.0075(15) 0.0173(17) 0.0088(15) C6 0.0368(18) 0.0339(17) 0.0386(19) -0.0082(14) 0.0086(15) 0.0098(15) C7 0.049(2) 0.0315(18) 0.050(2) -0.0050(15) 0.0152(18) 0.0031(16) C8 0.056(2) 0.0312(18) 0.063(3) -0.0082(16) 0.018(2) -0.0053(16) C9 0.049(2) 0.041(2) 0.053(2) -0.0161(16) 0.0078(19) 0.0045(17) C10 0.042(2) 0.053(2) 0.039(2) -0.0114(16) 0.0104(16) 0.0079(17) C11 0.0355(18) 0.048(2) 0.0365(19) -0.0073(15) 0.0096(15) 0.0068(15) C12 0.071(3) 0.034(2) 0.053(2) -0.0082(16) 0.023(2) -0.0086(18) C13 0.068(3) 0.061(3) 0.073(3) 0.001(2) 0.030(2) -0.006(2) C14 0.075(3) 0.075(3) 0.061(3) 0.006(2) 0.011(2) -0.013(2) C15 0.047(2) 0.066(2) 0.041(2) -0.0165(18) 0.0163(17) -0.0113(19) C16 0.077(3) 0.083(3) 0.061(3) -0.002(2) 0.017(2) -0.025(2) C17 0.043(2) 0.113(4) 0.076(3) -0.022(3) 0.019(2) -0.013(2) C18 0.049(2) 0.0401(19) 0.039(2) 0.0023(15) 0.0086(17) -0.0098(16) C19 0.051(2) 0.0353(18) 0.041(2) -0.0072(15) 0.0058(17) -0.0091(16) C20 0.048(2) 0.048(2) 0.0314(18) -0.0081(15) 0.0077(16) 0.0024(17) C21 0.0335(17) 0.0364(17) 0.0276(16) -0.0003(14) 0.0055(14) -0.0006(15) C22 0.0388(18) 0.0484(19) 0.0270(17) 0.0056(15) 0.0111(15) 0.0019(16) C23 0.0387(18) 0.0388(18) 0.0301(17) 0.0040(14) 0.0136(15) -0.0021(15) C24 0.047(2) 0.045(2) 0.045(2) 0.0125(16) 0.0116(17) -0.0046(17) C25 0.053(2) 0.047(2) 0.066(3) 0.0232(19) 0.011(2) -0.0011(19) C26 0.055(2) 0.049(2) 0.062(3) 0.0110(19) 0.020(2) -0.0131(19) C27 0.0390(19) 0.054(2) 0.046(2) 0.0042(17) 0.0119(17) -0.0110(17) C28 0.0406(19) 0.0407(18) 0.0305(18) 0.0016(14) 0.0133(15) -0.0022(15) C29 0.048(2) 0.056(2) 0.067(3) 0.031(2) 0.000(2) -0.0023(19) C30 0.049(2) 0.096(3) 0.062(3) 0.015(2) 0.015(2) 0.000(2) C31 0.086(3) 0.088(3) 0.076(3) -0.018(3) -0.022(3) 0.020(3) C32 0.0340(18) 0.055(2) 0.0366(19) 0.0077(16) 0.0110(16) -0.0042(16) C33 0.047(2) 0.074(3) 0.042(2) 0.0038(18) 0.0088(18) -0.0034(19) C34 0.052(2) 0.054(2) 0.051(2) 0.0035(17) 0.0087(19) 0.0015(18) C35 0.0305(17) 0.0417(19) 0.0206(15) 0.0047(12) 0.0059(13) -0.0022(14) C36 0.0356(17) 0.0375(17) 0.0273(16) 0.0033(14) 0.0060(14) 0.0000(15) C37 0.045(2) 0.045(2) 0.0346(19) 0.0047(15) 0.0107(17) 0.0096(16) C38 0.0316(18) 0.061(2) 0.0354(19) 0.0092(16) 0.0049(16) 0.0079(17) C39 0.0326(17) 0.056(2) 0.0295(17) 0.0055(16) 0.0034(14) -0.0048(16) C40 0.0378(18) 0.0434(18) 0.0250(16) 0.0025(13) 0.0099(15) -0.0021(15) C41 0.046(2) 0.0370(19) 0.0363(19) 0.0005(14) 0.0065(16) 0.0075(16) C42 0.077(3) 0.068(3) 0.045(2) -0.0134(19) 0.017(2) -0.012(2) C43 0.061(2) 0.055(2) 0.054(2) -0.0033(19) 0.008(2) -0.0098(19) C44 0.0414(19) 0.0431(19) 0.0350(19) -0.0010(15) 0.0059(16) -0.0036(16) C45 0.063(2) 0.052(2) 0.058(2) -0.0115(18) 0.023(2) -0.0218(19) C46 0.053(2) 0.048(2) 0.059(2) -0.0016(17) 0.0219(19) 0.0045(18) C47 0.036(2) 0.068(2) 0.068(3) 0.024(2) 0.0120(19) -0.0023(18) C48 0.053(2) 0.070(3) 0.076(3) 0.018(2) 0.024(2) -0.004(2) C49 0.072(3) 0.083(3) 0.063(3) 0.013(2) 0.028(2) -0.015(2) C50 0.055(2) 0.063(2) 0.041(2) 0.0163(17) 0.0099(18) 0.0067(19) C51 0.072(3) 0.079(3) 0.117(5) -0.001(3) 0.024(3) -0.006(3) C52 0.061(3) 0.110(4) 0.103(5) 0.015(3) -0.006(3) -0.005(3) C53 0.097(5) 0.109(5) 0.149(7) 0.006(4) 0.013(5) 0.005(4) C54 0.143(6) 0.073(4) 0.146(7) 0.001(4) 0.054(5) 0.014(4) C55 0.094(4) 0.085(4) 0.102(4) -0.015(3) 0.014(4) 0.023(3) C56 0.064(3) 0.067(3) 0.100(4) -0.008(3) 0.010(3) 0.009(2) C57 0.093(4) 0.132(5) 0.132(6) 0.017(4) 0.029(4) -0.021(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 Y1 N5 2.260(2) . ? Y1 N1 2.347(2) . ? Y1 O 2.361(2) . ? Y1 N3 2.367(2) . ? Y1 N2 2.457(2) . ? Y1 N4 2.491(2) . ? O C50 1.442(4) . ? O C47 1.465(4) . ? N1 C18 1.352(4) . ? N1 C21 1.385(4) . ? N2 C22 1.286(4) . ? N2 C23 1.448(4) . ? N3 C1 1.344(4) . ? N3 C4 1.374(4) . ? N4 C5 1.301(4) . ? N4 C6 1.451(4) . ? N5 C35 1.401(4) . ? N5 H100 0.8634 . ? C1 C2 1.386(5) . ? C1 H1 0.9300 . ? C2 C3 1.379(5) . ? C2 H2 0.9300 . ? C3 C4 1.392(4) . ? C3 H3 0.9300 . ? C4 C5 1.418(4) . ? C5 H5 0.9300 . ? C6 C11 1.399(4) . ? C6 C7 1.409(4) . ? C7 C8 1.398(5) . ? C7 C12 1.519(5) . ? C8 C9 1.374(5) . ? C8 H8 0.9300 . ? C9 C10 1.374(5) . ? C9 H9 0.9300 . ? C10 C11 1.403(4) . ? C10 H10 0.9300 . ? C11 C15 1.518(4) . ? C12 C13 1.521(5) . ? C12 C14 1.523(5) . ? C12 H12 0.9800 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C17 1.523(5) . ? C15 C16 1.533(5) . ? C15 H15 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.387(4) . ? C18 H18 0.9300 . ? C19 C20 1.373(4) . ? C19 H19 0.9300 . ? C20 C21 1.396(4) . ? C20 H20 0.9300 . ? C21 C22 1.407(4) . ? C22 H22 0.9300 . ? C23 C24 1.399(4) . ? C23 C28 1.408(4) . ? C24 C25 1.397(4) . ? C24 C29 1.521(5) . ? C25 C26 1.361(5) . ? C25 H25 0.9300 . ? C26 C27 1.383(5) . ? C26 H26 0.9300 . ? C27 C28 1.381(4) . ? C27 H27 0.9300 . ? C28 C32 1.516(4) . ? C29 C30 1.521(5) . ? C29 C31 1.548(5) . ? C29 H29 0.9800 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 C33 1.523(4) . ? C32 C34 1.527(5) . ? C32 H32 0.9800 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.411(4) . ? C35 C40 1.435(4) . ? C36 C37 1.389(4) . ? C36 C41 1.513(4) . ? C37 C38 1.371(4) . ? C37 H37 0.9300 . ? C38 C39 1.373(4) . ? C38 H38 0.9300 . ? C39 C40 1.384(4) . ? C39 H39 0.9300 . ? C40 C44 1.525(4) . ? C41 C42 1.516(4) . ? C41 C43 1.530(4) . ? C41 H41 0.9800 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 C45 1.524(4) . ? C44 C46 1.523(4) . ? C44 H44 0.9800 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 C48 1.486(5) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 C49 1.497(5) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.498(5) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C56 1.389(6) . ? C51 C52 1.400(7) . ? C51 C57 1.468(7) . ? C52 C53 1.382(8) . ? C52 H52 0.9300 . ? C53 C54 1.275(8) . ? C53 H53 0.9300 . ? C54 C55 1.437(8) . ? C54 H54 0.9300 . ? C55 C56 1.377(7) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? 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 N5 Y1 N1 119.43(8) . . ? N5 Y1 O 97.27(8) . . ? N1 Y1 O 81.88(8) . . ? N5 Y1 N3 155.39(9) . . ? N1 Y1 N3 85.10(9) . . ? O Y1 N3 83.48(8) . . ? N5 Y1 N2 103.30(8) . . ? N1 Y1 N2 71.52(8) . . ? O Y1 N2 151.96(8) . . ? N3 Y1 N2 85.56(8) . . ? N5 Y1 N4 85.93(8) . . ? N1 Y1 N4 154.27(8) . . ? O Y1 N4 91.17(7) . . ? N3 Y1 N4 69.46(8) . . ? N2 Y1 N4 108.94(8) . . ? C50 O C47 108.6(2) . . ? C50 O Y1 126.57(19) . . ? C47 O Y1 124.42(18) . . ? C18 N1 C21 104.9(2) . . ? C18 N1 Y1 141.4(2) . . ? C21 N1 Y1 113.63(18) . . ? C22 N2 C23 117.3(3) . . ? C22 N2 Y1 111.06(19) . . ? C23 N2 Y1 131.31(18) . . ? C1 N3 C4 105.4(3) . . ? C1 N3 Y1 138.0(2) . . ? C4 N3 Y1 116.44(19) . . ? C5 N4 C6 115.0(3) . . ? C5 N4 Y1 112.9(2) . . ? C6 N4 Y1 131.82(18) . . ? C35 N5 Y1 144.95(19) . . ? C35 N5 H100 109.1 . . ? Y1 N5 H100 103.6 . . ? N3 C1 C2 111.7(3) . . ? N3 C1 H1 124.2 . . ? C2 C1 H1 124.2 . . ? C3 C2 C1 106.2(3) . . ? C3 C2 H2 126.9 . . ? C1 C2 H2 126.9 . . ? C2 C3 C4 106.5(3) . . ? C2 C3 H3 126.7 . . ? C4 C3 H3 126.7 . . ? N3 C4 C3 110.2(3) . . ? N3 C4 C5 118.5(3) . . ? C3 C4 C5 131.3(3) . . ? N4 C5 C4 122.3(3) . . ? N4 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C11 C6 C7 121.9(3) . . ? C11 C6 N4 119.5(3) . . ? C7 C6 N4 118.6(3) . . ? C8 C7 C6 117.2(3) . . ? C8 C7 C12 121.2(3) . . ? C6 C7 C12 121.5(3) . . ? C9 C8 C7 121.5(3) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C10 C9 C8 120.5(3) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 120.7(3) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C6 C11 C10 118.0(3) . . ? C6 C11 C15 122.7(3) . . ? C10 C11 C15 119.4(3) . . ? C7 C12 C13 113.5(3) . . ? C7 C12 C14 111.6(3) . . ? C13 C12 C14 109.1(3) . . ? C7 C12 H12 107.5 . . ? C13 C12 H12 107.5 . . ? C14 C12 H12 107.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C17 111.1(3) . . ? C11 C15 C16 112.0(3) . . ? C17 C15 C16 110.1(3) . . ? C11 C15 H15 107.8 . . ? C17 C15 H15 107.8 . . ? C16 C15 H15 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N1 C18 C19 111.9(3) . . ? N1 C18 H18 124.0 . . ? C19 C18 H18 124.0 . . ? C20 C19 C18 106.2(3) . . ? C20 C19 H19 126.9 . . ? C18 C19 H19 126.9 . . ? C19 C20 C21 107.1(3) . . ? C19 C20 H20 126.5 . . ? C21 C20 H20 126.5 . . ? N1 C21 C20 109.8(3) . . ? N1 C21 C22 119.4(3) . . ? C20 C21 C22 130.7(3) . . ? N2 C22 C21 124.0(3) . . ? N2 C22 H22 118.0 . . ? C21 C22 H22 118.0 . . ? C24 C23 C28 121.4(3) . . ? C24 C23 N2 120.0(3) . . ? C28 C23 N2 118.6(3) . . ? C25 C24 C23 117.6(3) . . ? C25 C24 C29 119.1(3) . . ? C23 C24 C29 123.2(3) . . ? C26 C25 C24 121.7(3) . . ? C26 C25 H25 119.1 . . ? C24 C25 H25 119.1 . . ? C25 C26 C27 119.9(3) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C28 C27 C26 121.4(3) . . ? C28 C27 H27 119.3 . . ? C26 C27 H27 119.3 . . ? C27 C28 C23 118.0(3) . . ? C27 C28 C32 121.0(3) . . ? C23 C28 C32 120.8(3) . . ? C30 C29 C24 112.7(3) . . ? C30 C29 C31 109.4(3) . . ? C24 C29 C31 110.4(3) . . ? C30 C29 H29 108.1 . . ? C24 C29 H29 108.1 . . ? C31 C29 H29 108.1 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C28 C32 C33 113.8(3) . . ? C28 C32 C34 109.5(3) . . ? C33 C32 C34 109.4(3) . . ? C28 C32 H32 108.0 . . ? C33 C32 H32 108.0 . . ? C34 C32 H32 108.0 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N5 C35 C36 119.9(3) . . ? N5 C35 C40 122.1(3) . . ? C36 C35 C40 117.9(3) . . ? C37 C36 C35 119.6(3) . . ? C37 C36 C41 118.4(3) . . ? C35 C36 C41 122.0(3) . . ? C38 C37 C36 122.6(3) . . ? C38 C37 H37 118.7 . . ? C36 C37 H37 118.7 . . ? C37 C38 C39 118.1(3) . . ? C37 C38 H38 120.9 . . ? C39 C38 H38 120.9 . . ? C38 C39 C40 122.8(3) . . ? C38 C39 H39 118.6 . . ? C40 C39 H39 118.6 . . ? C39 C40 C35 119.0(3) . . ? C39 C40 C44 119.6(3) . . ? C35 C40 C44 121.4(3) . . ? C36 C41 C42 113.7(3) . . ? C36 C41 C43 111.1(3) . . ? C42 C41 C43 110.1(3) . . ? C36 C41 H41 107.2 . . ? C42 C41 H41 107.2 . . ? C43 C41 H41 107.2 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 C46 109.7(3) . . ? C45 C44 C40 114.2(3) . . ? C46 C44 C40 110.9(3) . . ? C45 C44 H44 107.2 . . ? C46 C44 H44 107.2 . . ? C40 C44 H44 107.2 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O C47 C48 106.9(3) . . ? O C47 H47A 110.4 . . ? C48 C47 H47A 110.4 . . ? O C47 H47B 110.4 . . ? C48 C47 H47B 110.4 . . ? H47A C47 H47B 108.6 . . ? C47 C48 C49 103.5(3) . . ? C47 C48 H48A 111.1 . . ? C49 C48 H48A 111.1 . . ? C47 C48 H48B 111.1 . . ? C49 C48 H48B 111.1 . . ? H48A C48 H48B 109.0 . . ? C48 C49 C50 104.0(3) . . ? C48 C49 H49A 111.0 . . ? C50 C49 H49A 111.0 . . ? C48 C49 H49B 111.0 . . ? C50 C49 H49B 111.0 . . ? H49A C49 H49B 109.0 . . ? O C50 C49 105.3(3) . . ? O C50 H50A 110.7 . . ? C49 C50 H50A 110.7 . . ? O C50 H50B 110.7 . . ? C49 C50 H50B 110.7 . . ? H50A C50 H50B 108.8 . . ? C56 C51 C52 118.2(6) . . ? C56 C51 C57 119.0(6) . . ? C52 C51 C57 122.8(5) . . ? C53 C52 C51 120.3(6) . . ? C53 C52 H52 119.8 . . ? C51 C52 H52 119.8 . . ? C54 C53 C52 123.8(8) . . ? C54 C53 H53 118.1 . . ? C52 C53 H53 118.1 . . ? C53 C54 C55 117.0(7) . . ? C53 C54 H54 121.5 . . ? C55 C54 H54 121.5 . . ? C56 C55 C54 122.4(6) . . ? C56 C55 H55 118.8 . . ? C54 C55 H55 118.8 . . ? C55 C56 C51 118.1(5) . . ? C55 C56 H56 120.9 . . ? C51 C56 H56 120.9 . . ? C51 C57 H57A 109.5 . . ? C51 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C51 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.07 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.482 _refine_diff_density_min -0.332 _refine_diff_density_rms 0.062