# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name F.Grepioni _publ_contact_author_email fabrizia.grepioni@unibo.it loop_ _publ_author_name F.Grepioni D.Braga L.Chelazzi G.Viscomi data_alfa3_finale _database_code_depnum_ccdc_archive 'CCDC 886509' #TrackingRef '- alfa_0.5w_100K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H52 N3 O11.50' _chemical_formula_weight 794.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.401(4) _cell_length_b 19.662(4) _cell_length_c 16.153(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.05(3) _cell_angle_gamma 90.00 _cell_volume 4268.6(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.237 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1692 _exptl_absorpt_coefficient_mu 0.207 _exptl_absorpt_correction_T_min 0.98216 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #============================================================================== # EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.00000 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9504 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 28.46 _reflns_number_total 6184 _reflns_number_gt 5630 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.049(7) _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_number_reflns 6184 _refine_ls_number_parameters 454 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.1893 _refine_ls_R_factor_gt 0.1767 _refine_ls_wR_factor_ref 0.4544 _refine_ls_wR_factor_gt 0.4544 _refine_ls_goodness_of_fit_ref 2.553 _refine_ls_restrained_S_all 2.572 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.005 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 C9 C -0.7814(15) -0.3746(12) -0.1159(11) 0.075(6) Uiso 1 1 d D . . C1 C -0.8771(12) -0.3978(10) -0.1516(10) 0.055(5) Uiso 1 1 d D . . C2 C -0.9583(12) -0.3644(10) -0.1429(9) 0.054(5) Uiso 1 1 d D . . C3 C -0.9287(13) -0.3072(11) -0.0888(12) 0.058(5) Uiso 1 1 d D . . C4 C -0.8342(17) -0.2795(15) -0.0567(16) 0.090(7) Uiso 1 1 d D . . C10 C -0.7482(11) -0.3165(10) -0.0690(10) 0.046(4) Uiso 1 1 d D . . C5 C -0.6546(15) -0.3027(13) -0.0314(13) 0.069(6) Uiso 1 1 d D . . C6 C -0.5771(11) -0.3344(10) -0.0326(10) 0.043(4) Uiso 1 1 d D . . C7 C -0.5971(17) -0.4006(15) -0.0906(16) 0.089(7) Uiso 1 1 d D . . C8 C -0.6982(13) -0.4142(11) -0.1308(12) 0.058(5) Uiso 1 1 d D . . C20 C -1.2021(13) -0.4290(12) 0.0608(13) 0.064(5) Uiso 1 1 d . . . H20 H -1.2318 -0.4610 0.0907 0.076 Uiso 1 1 calc R . . C22 C -1.0439(12) -0.4176(12) 0.1990(11) 0.058(5) Uiso 1 1 d . . . H22 H -1.0549 -0.3686 0.2017 0.070 Uiso 1 1 calc R . . C2A C -1.0369(12) -0.3458(10) -0.3977(9) 0.050(5) Uiso 1 1 d D . . H2A H -1.0843 -0.3192 -0.3862 0.060 Uiso 1 1 calc R . . C5A C -0.8992(12) -0.4249(9) -0.4241(9) 0.049(4) Uiso 1 1 d D . . H5A H -0.8512 -0.4519 -0.4341 0.059 Uiso 1 1 calc R . . C6A C -0.8735(13) -0.3619(9) -0.3744(9) 0.061(5) Uiso 1 1 d D . . C211 C -1.0850(15) -0.2514(13) -0.0765(14) 0.073(6) Uiso 1 1 d D . . H211 H -1.1250 -0.2880 -0.1040 0.087 Uiso 1 1 calc R . . C311 C -1.127(2) -0.1874(16) -0.0443(16) 0.094(7) Uiso 1 1 d D . . H311 H -1.1925 -0.1787 -0.0498 0.112 Uiso 1 1 calc R . . C411 C -1.0582(17) -0.1536(15) -0.0124(16) 0.084(7) Uiso 1 1 d D . . C511 C -0.9658(14) -0.1482(12) 0.0089(13) 0.067(5) Uiso 1 1 d D . . H511 H -0.9279 -0.1124 0.0414 0.081 Uiso 1 1 calc R . . C611 C -0.9264(14) -0.2056(12) -0.0240(12) 0.062(5) Uiso 1 1 d D . . C11 C -0.6013(15) -0.2428(12) 0.0353(12) 0.071(6) Uiso 1 1 d D . . C12 C -0.4890(17) -0.2517(14) 0.0571(14) 0.087(7) Uiso 1 1 d D . . C15 C -1.1336(12) -0.3750(11) -0.2230(10) 0.047(4) Uiso 1 1 d . . . C16 C -1.2271(13) -0.4139(12) -0.2541(12) 0.060(5) Uiso 1 1 d . . . H16 H -1.2656 -0.3726 -0.2552 0.072 Uiso 1 1 calc R . . C17 C -1.2527(15) -0.4395(13) -0.1915(14) 0.073(6) Uiso 1 1 d . . . H17 H -1.3057 -0.4698 -0.2100 0.088 Uiso 1 1 calc R . . C19 C -1.2405(14) -0.4467(12) -0.0336(13) 0.068(5) Uiso 1 1 d . . . H19 H -1.2946 -0.4762 -0.0508 0.081 Uiso 1 1 calc R . . C21 C -1.0916(14) -0.4389(13) 0.1001(13) 0.069(6) Uiso 1 1 d . . . H21 H -1.0613 -0.4113 0.0660 0.082 Uiso 1 1 calc R . . C23 C -0.9315(15) -0.4291(14) 0.2384(15) 0.076(6) Uiso 1 1 d . . . H23 H -0.9049 -0.4110 0.2990 0.091 Uiso 1 1 calc R . . C24 C -0.8699(14) -0.3999(13) 0.1831(14) 0.071(6) Uiso 1 1 d . . . H24 H -0.8938 -0.4220 0.1248 0.085 Uiso 1 1 calc R . . C25 C -0.7562(15) -0.4163(14) 0.2287(14) 0.077(6) Uiso 1 1 d . . . H25 H -0.7480 -0.4646 0.2445 0.092 Uiso 1 1 calc R . . C26 C -0.6962(14) -0.3996(13) 0.1755(13) 0.067(5) Uiso 1 1 d . . . H26 H -0.7159 -0.3537 0.1523 0.081 Uiso 1 1 calc R . . C27 C -0.5851(15) -0.3968(14) 0.2290(15) 0.077(6) Uiso 1 1 d . . . H27 H -0.5777 -0.3663 0.2789 0.092 Uiso 1 1 calc R . . C28 C -0.5246(15) -0.3630(14) 0.1762(15) 0.079(6) Uiso 1 1 d . . . H28 H -0.5149 -0.3857 0.1295 0.095 Uiso 1 1 calc R . . C29 C -0.4880(15) -0.3018(14) 0.1998(15) 0.077(6) Uiso 1 1 d . . . H29 H -0.4939 -0.2815 0.2497 0.092 Uiso 1 1 calc R . . C14 C -0.5219(15) -0.4412(13) -0.0917(14) 0.073(6) Uiso 1 1 d . . . H14A H -0.4594 -0.4196 -0.0598 0.110 Uiso 1 1 calc R . . H14B H -0.5273 -0.4490 -0.1519 0.110 Uiso 1 1 calc R . . H14C H -0.5254 -0.4839 -0.0641 0.110 Uiso 1 1 calc R . . C711 C -1.115(2) -0.0821(19) 0.011(2) 0.115(9) Uiso 1 1 d . . . H71A H -1.0663 -0.0477 0.0366 0.173 Uiso 1 1 calc R . . H71B H -1.1475 -0.0940 0.0515 0.173 Uiso 1 1 calc R . . H71C H -1.1640 -0.0652 -0.0433 0.173 Uiso 1 1 calc R . . C13 C -0.4345(16) -0.2037(15) 0.0347(16) 0.083(6) Uiso 1 1 d . . . H13A H -0.4653 -0.1931 -0.0272 0.124 Uiso 1 1 calc R . . H13B H -0.3685 -0.2207 0.0463 0.124 Uiso 1 1 calc R . . H13C H -0.4311 -0.1634 0.0692 0.124 Uiso 1 1 calc R . . C30 C -1.2754(19) -0.4222(17) -0.3466(17) 0.098(8) Uiso 1 1 d . . . H30A H -1.2445 -0.3934 -0.3772 0.147 Uiso 1 1 calc R . . H30B H -1.3443 -0.4102 -0.3633 0.147 Uiso 1 1 calc R . . H30C H -1.2701 -0.4688 -0.3623 0.147 Uiso 1 1 calc R . . C31 C -1.2362(17) -0.3594(14) 0.0741(16) 0.084(6) Uiso 1 1 d . . . H31A H -1.3074 -0.3571 0.0476 0.125 Uiso 1 1 calc R . . H31B H -1.2072 -0.3264 0.0468 0.125 Uiso 1 1 calc R . . H31C H -1.2158 -0.3501 0.1364 0.125 Uiso 1 1 calc R . . C32 C -1.0934(14) -0.4531(13) 0.2600(13) 0.068(5) Uiso 1 1 d . . . H32A H -1.0603 -0.4386 0.3203 0.103 Uiso 1 1 calc R . . H32B H -1.0876 -0.5015 0.2563 0.103 Uiso 1 1 calc R . . H32C H -1.1624 -0.4407 0.2407 0.103 Uiso 1 1 calc R . . C33 C -0.8895(13) -0.3197(11) 0.1680(12) 0.056(5) Uiso 1 1 d . . . H33A H -0.9595 -0.3116 0.1392 0.085 Uiso 1 1 calc R . . H33B H -0.8547 -0.3026 0.1316 0.085 Uiso 1 1 calc R . . H33C H -0.8660 -0.2968 0.2243 0.085 Uiso 1 1 calc R . . C35 C -0.6941(13) -0.4045(13) 0.3935(12) 0.064(5) Uiso 1 1 d . . . C36 C -0.6467(19) -0.3564(16) 0.4641(17) 0.099(8) Uiso 1 1 d . . . H36A H -0.6529 -0.3114 0.4399 0.148 Uiso 1 1 calc R . . H36B H -0.5776 -0.3678 0.4919 0.148 Uiso 1 1 calc R . . H36C H -0.6784 -0.3584 0.5072 0.148 Uiso 1 1 calc R . . C34 C -0.7202(15) -0.4444(13) 0.0988(13) 0.070(5) Uiso 1 1 d . . . H34A H -0.6782 -0.4337 0.0660 0.105 Uiso 1 1 calc R . . H34B H -0.7886 -0.4382 0.0614 0.105 Uiso 1 1 calc R . . H34C H -0.7097 -0.4908 0.1183 0.105 Uiso 1 1 calc R . . C37 C -0.4544(6) -0.4635(6) 0.3287(6) 0.124(10) Uiso 1 1 d . . . H37A H -0.4391 -0.5092 0.3502 0.185 Uiso 1 1 calc R . . H37B H -0.4468 -0.4336 0.3776 0.185 Uiso 1 1 calc R . . H37C H -0.4100 -0.4499 0.2995 0.185 Uiso 1 1 calc R . . N2 N -0.9880(6) -0.2498(6) -0.0616(6) 0.077(5) Uiso 1 1 d D . . N3 N -0.8314(6) -0.2151(6) -0.0112(6) 0.082(5) Uiso 1 1 d D . . N1 N -1.0473(6) -0.3921(6) -0.1730(6) 0.057(4) Uiso 1 1 d . . . H1 H -1.0464 -0.4328 -0.1533 0.069 Uiso 1 1 calc R . . O3 O -0.4878(9) -0.3218(8) 0.0079(9) 0.067(4) Uiso 1 1 d D . . O2 O -0.7225(10) -0.4701(9) -0.1771(9) 0.077(4) Uiso 1 1 d . . . O1 O -0.8998(10) -0.4529(9) -0.1997(9) 0.081(4) Uiso 1 1 d . . . H1A H -0.8497 -0.4681 -0.2059 0.122 Uiso 1 1 calc R . . O4 O -0.6286(10) -0.1937(10) 0.0638(10) 0.087(4) Uiso 1 1 d . . . O11 O -1.1385(10) -0.3119(8) -0.2627(9) 0.078(4) Uiso 1 1 d . . . O10 O -1.0708(10) -0.5100(8) 0.0888(9) 0.075(4) Uiso 1 1 d . . . H10 H -1.0106 -0.5166 0.1099 0.112 Uiso 1 1 calc R . . O9 O -0.9090(10) -0.5016(9) 0.2395(9) 0.080(4) Uiso 1 1 d . . . H9 H -0.9609 -0.5231 0.2182 0.120 Uiso 1 1 calc R . . O7 O -0.7241(9) -0.3740(8) 0.3126(9) 0.073(4) Uiso 1 1 d . . . O6 O -0.5576(10) -0.4604(9) 0.2657(9) 0.083(4) Uiso 1 1 d . . . O5 O -0.4415(10) -0.2677(9) 0.1524(9) 0.083(4) Uiso 1 1 d . . . O8 O -0.7096(13) -0.4647(12) 0.3938(12) 0.106(5) Uiso 1 1 d . . . C4A C -0.9942(13) -0.4419(11) -0.4544(11) 0.061(5) Uiso 1 1 d D . . C3A C -1.0662(13) -0.4066(11) -0.4519(11) 0.057(5) Uiso 1 1 d D . . H3A H -1.1323 -0.4184 -0.4822 0.068 Uiso 1 1 calc R . . C9' C -0.7970(13) -0.2731(11) -0.2951(11) 0.058(5) Uiso 1 1 d D . . C1' C -0.8953(13) -0.2698(11) -0.3153(11) 0.058(5) Uiso 1 1 d D . . C2' C -0.9380(15) -0.2098(13) -0.2768(12) 0.070(6) Uiso 1 1 d D . . C3' C -0.8604(14) -0.1704(12) -0.2314(12) 0.066(5) Uiso 1 1 d D . . C4' C -0.7596(12) -0.1745(10) -0.2133(10) 0.049(5) Uiso 1 1 d D . . C10' C -0.7258(11) -0.2301(10) -0.2491(10) 0.045(4) Uiso 1 1 d D . . C5' C -0.6306(14) -0.2321(12) -0.2334(12) 0.064(5) Uiso 1 1 d D . . C6' C -0.5583(16) -0.1823(14) -0.1928(14) 0.082(6) Uiso 1 1 d D . . C7' C -0.5896(13) -0.1213(10) -0.1589(10) 0.060(5) Uiso 1 1 d D . . C8' C -0.6912(13) -0.1175(11) -0.1714(11) 0.065(5) Uiso 1 1 d D . . C11' C -0.5671(14) -0.2798(12) -0.2678(11) 0.069(6) Uiso 1 1 d D . . C12' C -0.4547(15) -0.2507(13) -0.2310(13) 0.076(6) Uiso 1 1 d D . . C122 C -1.0926(14) -0.1465(12) -0.3355(13) 0.062(5) Uiso 1 1 d . . . C16' C -1.1984(15) -0.1531(14) -0.3566(15) 0.076(6) Uiso 1 1 d . . . H16' H -1.2098 -0.1058 -0.3767 0.092 Uiso 1 1 calc R . . C17' C -1.2544(13) -0.1749(11) -0.4319(11) 0.054(5) Uiso 1 1 d . . . H17' H -1.3202 -0.1848 -0.4399 0.064 Uiso 1 1 calc R . . C18' C -1.2229(17) -0.1850(15) -0.5044(15) 0.084(6) Uiso 1 1 d . . . H018' H -1.1566 -0.1749 -0.4938 0.101 Uiso 1 1 calc R . . C19' C -1.2756(17) -0.2073(14) -0.5861(15) 0.082(6) Uiso 1 1 d . . . H19' H -1.3434 -0.2145 -0.6005 0.098 Uiso 1 1 calc R . . C20' C -1.2314(16) -0.2214(14) -0.6571(15) 0.079(6) Uiso 1 1 d . . . H20' H -1.2796 -0.2048 -0.7133 0.094 Uiso 1 1 calc R . . C21' C -1.1339(14) -0.1888(13) -0.6462(14) 0.072(6) Uiso 1 1 d . . . H21' H -1.0881 -0.2022 -0.5872 0.086 Uiso 1 1 calc R . . C22' C -1.0816(14) -0.2075(14) -0.7112(13) 0.070(6) Uiso 1 1 d . . . H22' H -1.0722 -0.2569 -0.7091 0.084 Uiso 1 1 calc R . . C23' C -0.9833(13) -0.1755(12) -0.6875(12) 0.060(5) Uiso 1 1 d . . . H23' H -0.9546 -0.1920 -0.7303 0.072 Uiso 1 1 calc R . . C24' C -0.9055(14) -0.1866(12) -0.5965(13) 0.066(5) Uiso 1 1 d . . . H24' H -0.9297 -0.1672 -0.5521 0.079 Uiso 1 1 calc R . . C25' C -0.8042(13) -0.1576(13) -0.5823(13) 0.065(5) Uiso 1 1 d . . . H25' H -0.8127 -0.1103 -0.6026 0.078 Uiso 1 1 calc R . . C26' C -0.7228(15) -0.1599(14) -0.4921(14) 0.074(6) Uiso 1 1 d . . . H26' H -0.7230 -0.2068 -0.4717 0.089 Uiso 1 1 calc R . . C27' C -0.6207(14) -0.1466(13) -0.4812(13) 0.067(5) Uiso 1 1 d . . . H27' H -0.6065 -0.1737 -0.5261 0.081 Uiso 1 1 calc R . . C28' C -0.5418(14) -0.1655(12) -0.3918(13) 0.066(5) Uiso 1 1 d . . . H28' H -0.5338 -0.1381 -0.3428 0.079 Uiso 1 1 calc R . . C29' C -0.4864(16) -0.2180(14) -0.3826(16) 0.081(6) Uiso 1 1 d . . . H29' H -0.4880 -0.2386 -0.4349 0.097 Uiso 1 1 calc R . . C14' C -0.5199(13) -0.0671(11) -0.1186(12) 0.058(5) Uiso 1 1 d . . . H14D' H -0.4557 -0.0787 -0.1199 0.087 Uiso 1 1 calc R . . H14E' H -0.5151 -0.0611 -0.0582 0.087 Uiso 1 1 calc R . . H14F' H -0.5427 -0.0257 -0.1509 0.087 Uiso 1 1 calc R . . C7A C -1.0286(15) -0.5131(12) -0.5087(14) 0.073(6) Uiso 1 1 d . . . H7A1' H -0.9708 -0.5387 -0.5059 0.109 Uiso 1 1 calc R . . H7A2' H -1.0679 -0.5034 -0.5695 0.109 Uiso 1 1 calc R . . H7A3' H -1.0674 -0.5391 -0.4825 0.109 Uiso 1 1 calc R . . C13' C -0.3862(11) -0.2982(10) -0.1634(11) 0.046(4) Uiso 1 1 d . . . H13D' H -0.4068 -0.3014 -0.1132 0.069 Uiso 1 1 calc R . . H13E' H -0.3194 -0.2811 -0.1445 0.069 Uiso 1 1 calc R . . H13F' H -0.3888 -0.3424 -0.1893 0.069 Uiso 1 1 calc R . . C30' C -1.2268(16) -0.1374(15) -0.2747(15) 0.082(6) Uiso 1 1 d . . . H30D' H -1.1682 -0.1244 -0.2258 0.124 Uiso 1 1 calc R . . H30E' H -1.2554 -0.1772 -0.2590 0.124 Uiso 1 1 calc R . . H30F' H -1.2742 -0.1010 -0.2885 0.124 Uiso 1 1 calc R . . C31' C -1.2238(15) -0.3018(13) -0.6669(13) 0.070(6) Uiso 1 1 d . . . H31D' H -1.2866 -0.3223 -0.6738 0.105 Uiso 1 1 calc R . . H31E' H -1.1733 -0.3197 -0.6148 0.105 Uiso 1 1 calc R . . H31F' H -1.2070 -0.3117 -0.7180 0.105 Uiso 1 1 calc R . . C32' C -1.1484(14) -0.1874(13) -0.8101(12) 0.068(5) Uiso 1 1 d . . . H32D' H -1.1144 -0.1994 -0.8493 0.102 Uiso 1 1 calc R . . H32E' H -1.1606 -0.1393 -0.8133 0.102 Uiso 1 1 calc R . . H32F' H -1.2106 -0.2113 -0.8272 0.102 Uiso 1 1 calc R . . C33' C -0.8955(15) -0.2720(12) -0.5821(14) 0.070(5) Uiso 1 1 d . . . H33D' H -0.9602 -0.2910 -0.5929 0.104 Uiso 1 1 calc R . . H33E' H -0.8527 -0.2820 -0.5224 0.104 Uiso 1 1 calc R . . H33F' H -0.8680 -0.2913 -0.6229 0.104 Uiso 1 1 calc R . . C18 C -1.2107(16) -0.4275(14) -0.0974(14) 0.078(6) Uiso 1 1 d . . . H18' H -1.1527 -0.4017 -0.0789 0.094 Uiso 1 1 calc R . . C35' C -0.7364(17) -0.1660(16) -0.7022(16) 0.089(7) Uiso 1 1 d . . . C36' C -0.6833(18) -0.2064(16) -0.7464(18) 0.097(7) Uiso 1 1 d . . . H36A' H -0.6804 -0.2529 -0.7273 0.145 Uiso 1 1 calc R . . H36B' H -0.6170 -0.1890 -0.7315 0.145 Uiso 1 1 calc R . . H36C' H -0.7175 -0.2040 -0.8094 0.145 Uiso 1 1 calc R . . C34' C -0.7501(14) -0.1140(13) -0.4216(13) 0.069(5) Uiso 1 1 d . . . H34A' H -0.8172 -0.1234 -0.4261 0.103 Uiso 1 1 calc R . . H34B' H -0.7441 -0.0668 -0.4338 0.103 Uiso 1 1 calc R . . H34C' H -0.7054 -0.1245 -0.3627 0.103 Uiso 1 1 calc R . . C37' C -0.5317(17) -0.0547(15) -0.5202(17) 0.091(7) Uiso 1 1 d . . . H37D' H -0.5364 -0.0066 -0.5313 0.137 Uiso 1 1 calc R . . H37E' H -0.5262 -0.0780 -0.5705 0.137 Uiso 1 1 calc R . . H37F' H -0.4741 -0.0642 -0.4686 0.137 Uiso 1 1 calc R . . N2' N -0.9441(9) -0.3292(8) -0.3656(8) 0.044(4) Uiso 1 1 d D . . N3' N -0.7840(10) -0.3386(9) -0.3364(9) 0.058(4) Uiso 1 1 d D . . N1' N -1.0375(9) -0.2048(9) -0.2989(9) 0.050(4) Uiso 1 1 d . . . H1' H -1.0688 -0.2396 -0.2900 0.060 Uiso 1 1 calc R . . O3' O -0.4650(9) -0.1900(8) -0.1949(8) 0.067(4) Uiso 1 1 d D . . O2' O -0.7200(10) -0.0752(8) -0.1285(9) 0.075(4) Uiso 1 1 d . . . H2' H -0.7771 -0.0843 -0.1328 0.112 Uiso 1 1 calc R . . O1' O -0.8905(9) -0.1195(8) -0.1822(8) 0.069(4) Uiso 1 1 d . . . O6' O -0.6189(10) -0.0775(9) -0.5057(10) 0.083(4) Uiso 1 1 d . . . O4' O -0.5896(9) -0.3355(8) -0.3055(8) 0.068(4) Uiso 1 1 d . . . O11' O -1.0518(9) -0.0991(8) -0.3528(8) 0.071(4) Uiso 1 1 d . . . O10' O -1.1448(10) -0.1149(9) -0.6429(9) 0.080(4) Uiso 1 1 d . . . H10' H -1.0916 -0.0966 -0.6369 0.120 Uiso 1 1 calc R . . O9' O -0.9876(9) -0.0980(8) -0.6954(8) 0.067(3) Uiso 1 1 d . . . H9' H -0.9309 -0.0829 -0.6813 0.100 Uiso 1 1 calc R . . O7' O -0.7626(9) -0.1973(9) -0.6410(9) 0.076(4) Uiso 1 1 d . . . O5' O -0.4244(10) -0.2484(9) -0.3049(9) 0.077(4) Uiso 1 1 d . . . O8' O -0.7544(11) -0.1011(11) -0.7184(11) 0.095(5) Uiso 1 1 d . . . O1W O -1.0670(10) -0.5379(9) -0.1780(9) 0.055(8) Uiso 0.77(6) 1 d P . . _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C9 C10 1.36(3) . ? C9 C1 1.37(3) . ? C9 C8 1.52(3) . ? C1 O1 1.30(2) . ? C1 C2 1.39(3) . ? C2 N1 1.31(2) . ? C2 C3 1.39(3) . ? C3 C4 1.38(3) . ? C3 N2 1.57(2) . ? C4 N3 1.46(3) . ? C4 C10 1.51(3) . ? C10 C5 1.29(3) . ? C5 C6 1.29(3) . ? C5 C11 1.60(3) . ? C6 O3 1.240(18) . ? C6 C7 1.57(3) . ? C7 C14 1.35(3) . ? C7 C8 1.39(3) . ? C8 O2 1.31(2) . ? C20 C19 1.46(3) . ? C20 C31 1.49(4) . ? C20 C21 1.50(3) . ? C22 C23 1.53(3) . ? C22 C21 1.55(3) . ? C22 C32 1.57(3) . ? C2A N2' 1.29(2) . ? C2A C3A 1.45(3) . ? C5A C4A 1.32(2) . ? C5A C6A 1.45(3) . ? C6A N2' 1.25(2) . ? C6A N3' 1.30(2) . ? C211 N2 1.33(2) . ? C211 C311 1.56(4) . ? C311 C411 1.15(3) . ? C411 C511 1.25(3) . ? C411 C711 1.73(4) . ? C511 C611 1.45(3) . ? C611 N2 1.23(2) . ? C611 N3 1.32(2) . ? C11 O4 1.19(3) . ? C11 C12 1.54(3) . ? C12 C13 1.36(3) . ? C12 O5 1.48(2) . ? C12 O3 1.59(3) . ? C15 N1 1.260(18) . ? C15 O11 1.39(2) . ? C15 C16 1.47(3) . ? C16 C17 1.30(3) . ? C16 C30 1.41(3) . ? C17 C18 1.44(3) . ? C19 C18 1.31(3) . ? C21 O10 1.46(3) . ? C23 O9 1.46(3) . ? C23 C24 1.58(3) . ? C24 C25 1.57(3) . ? C24 C33 1.61(3) . ? C25 C26 1.46(3) . ? C25 O7 1.51(3) . ? C26 C34 1.46(3) . ? C26 C27 1.52(3) . ? C27 O6 1.38(3) . ? C27 C28 1.57(3) . ? C28 C29 1.32(3) . ? C29 O5 1.36(3) . ? C35 O8 1.21(3) . ? C35 O7 1.36(2) . ? C35 C36 1.45(4) . ? C37 O6 1.470(16) . ? C4A C3A 1.26(3) . ? C4A C7A 1.63(3) . ? C9' C10' 1.33(3) . ? C9' C1' 1.34(2) . ? C9' N3' 1.49(3) . ? C1' N2' 1.45(3) . ? C1' C2' 1.56(3) . ? C2' C3' 1.34(3) . ? C2' N1' 1.35(2) . ? C3' C4' 1.38(3) . ? C3' O1' 1.44(3) . ? C4' C10' 1.40(3) . ? C4' C8' 1.49(3) . ? C10' C5' 1.30(2) . ? C5' C6' 1.41(3) . ? C5' C11' 1.55(3) . ? C6' O3' 1.37(3) . ? C6' C7' 1.46(3) . ? C7' C8' 1.40(3) . ? C7' C14' 1.45(3) . ? C8' O2' 1.24(2) . ? C11' O4' 1.24(3) . ? C11' C12' 1.62(3) . ? C12' O3' 1.36(3) . ? C12' O5' 1.41(2) . ? C12' C13' 1.51(3) . ? C122 O11' 1.19(2) . ? C122 N1' 1.40(3) . ? C122 C16' 1.44(3) . ? C16' C17' 1.27(3) . ? C16' C30' 1.55(3) . ? C17' C18' 1.41(3) . ? C18' C19' 1.34(3) . ? C19' C20' 1.52(3) . ? C20' C21' 1.50(3) . ? C20' C31' 1.60(4) . ? C21' O10' 1.46(3) . ? C21' C22' 1.54(3) . ? C22' C23' 1.47(3) . ? C22' C32' 1.59(3) . ? C23' C24' 1.51(3) . ? C23' O9' 1.53(3) . ? C24' C25' 1.50(3) . ? C24' C33' 1.69(4) . ? C25' C26' 1.51(3) . ? C25' O7' 1.51(3) . ? C26' C27' 1.44(3) . ? C26' C34' 1.61(3) . ? C27' O6' 1.42(3) . ? C27' C28' 1.53(3) . ? C28' C29' 1.28(3) . ? C29' O5' 1.39(3) . ? C35' O8' 1.31(3) . ? C35' O7' 1.33(3) . ? C35' C36' 1.45(4) . ? C37' O6' 1.43(3) . ? 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 C10 C9 C1 128(2) . . ? C10 C9 C8 112.2(17) . . ? C1 C9 C8 120(2) . . ? O1 C1 C9 121.8(17) . . ? O1 C1 C2 114.3(16) . . ? C9 C1 C2 124(2) . . ? N1 C2 C1 120.7(18) . . ? N1 C2 C3 127.2(16) . . ? C1 C2 C3 111.4(16) . . ? C4 C3 C2 126.3(18) . . ? C4 C3 N2 100.0(18) . . ? C2 C3 N2 132.9(15) . . ? C3 C4 N3 112.1(19) . . ? C3 C4 C10 120(2) . . ? N3 C4 C10 127.6(19) . . ? C5 C10 C9 122.6(18) . . ? C5 C10 C4 127(2) . . ? C9 C10 C4 109.7(17) . . ? C6 C5 C10 131(2) . . ? C6 C5 C11 99.1(16) . . ? C10 C5 C11 129.8(19) . . ? O3 C6 C5 129.6(19) . . ? O3 C6 C7 114.5(15) . . ? C5 C6 C7 115.9(17) . . ? C14 C7 C8 126(2) . . ? C14 C7 C6 121(2) . . ? C8 C7 C6 112.0(19) . . ? O2 C8 C7 116.7(18) . . ? O2 C8 C9 117.3(16) . . ? C7 C8 C9 126(2) . . ? C19 C20 C31 110.2(18) . . ? C19 C20 C21 110.9(16) . . ? C31 C20 C21 114.3(18) . . ? C23 C22 C21 113.5(16) . . ? C23 C22 C32 108.9(15) . . ? C21 C22 C32 113.1(17) . . ? N2' C2A C3A 119.0(16) . . ? C4A C5A C6A 116.5(16) . . ? N2' C6A N3' 118(2) . . ? N2' C6A C5A 116.5(17) . . ? N3' C6A C5A 125.3(17) . . ? N2 C211 C311 115(2) . . ? C411 C311 C211 104(3) . . ? C311 C411 C511 146(3) . . ? C311 C411 C711 99(2) . . ? C511 C411 C711 114(2) . . ? C411 C511 C611 111(2) . . ? N2 C611 N3 119.8(19) . . ? N2 C611 C511 115.0(17) . . ? N3 C611 C511 125.0(17) . . ? O4 C11 C12 118.0(19) . . ? O4 C11 C5 135.4(18) . . ? C12 C11 C5 106.4(18) . . ? C13 C12 O5 109.3(19) . . ? C13 C12 C11 121.4(18) . . ? O5 C12 C11 108.5(12) . . ? C13 C12 O3 111.0(19) . . ? O5 C12 O3 104.6(16) . . ? C11 C12 O3 100.5(16) . . ? N1 C15 O11 114.1(14) . . ? N1 C15 C16 130.6(19) . . ? O11 C15 C16 114.8(15) . . ? C17 C16 C30 128(2) . . ? C17 C16 C15 114.7(16) . . ? C30 C16 C15 117.6(18) . . ? C16 C17 C18 129(2) . . ? C18 C19 C20 130(2) . . ? O10 C21 C20 107.8(16) . . ? O10 C21 C22 110.7(16) . . ? C20 C21 C22 114.3(16) . . ? O9 C23 C22 110.3(17) . . ? O9 C23 C24 101.3(17) . . ? C22 C23 C24 115.9(17) . . ? C25 C24 C23 111.3(17) . . ? C25 C24 C33 111.8(17) . . ? C23 C24 C33 109.9(17) . . ? C26 C25 O7 110.5(18) . . ? C26 C25 C24 114.6(18) . . ? O7 C25 C24 103.8(16) . . ? C25 C26 C34 110.9(19) . . ? C25 C26 C27 113.5(17) . . ? C34 C26 C27 112.6(17) . . ? O6 C27 C26 106.9(18) . . ? O6 C27 C28 119.1(18) . . ? C26 C27 C28 112.6(17) . . ? C29 C28 C27 118(2) . . ? C28 C29 O5 121(2) . . ? O8 C35 O7 116.2(19) . . ? O8 C35 C36 132(2) . . ? O7 C35 C36 111(2) . . ? C611 N2 C211 128.9(16) . . ? C611 N2 C3 106.1(13) . . ? C211 N2 C3 125.0(14) . . ? C611 N3 C4 101.8(14) . . ? C15 N1 C2 137.2(15) . . ? C6 O3 C12 104.0(14) . . ? C35 O7 C25 120.5(18) . . ? C27 O6 C37 113.5(14) . . ? C29 O5 C12 123.7(16) . . ? C3A C4A C5A 127(2) . . ? C3A C4A C7A 113.3(17) . . ? C5A C4A C7A 119.4(16) . . ? C4A C3A C2A 114.2(18) . . ? C10' C9' C1' 130(2) . . ? C10' C9' N3' 127.1(16) . . ? C1' C9' N3' 103.0(15) . . ? C9' C1' N2' 110.8(16) . . ? C9' C1' C2' 118.3(17) . . ? N2' C1' C2' 130.6(15) . . ? C3' C2' N1' 134(2) . . ? C3' C2' C1' 106.6(17) . . ? N1' C2' C1' 118.8(17) . . ? C2' C3' C4' 134(2) . . ? C2' C3' O1' 110.3(17) . . ? C4' C3' O1' 115.4(16) . . ? C3' C4' C10' 117.0(16) . . ? C3' C4' C8' 121.9(17) . . ? C10' C4' C8' 120.3(15) . . ? C5' C10' C9' 129.5(19) . . ? C5' C10' C4' 116.1(16) . . ? C9' C10' C4' 114.4(15) . . ? C10' C5' C6' 128(2) . . ? C10' C5' C11' 131.7(18) . . ? C6' C5' C11' 98.9(17) . . ? O3' C6' C5' 119(2) . . ? O3' C6' C7' 123(2) . . ? C5' C6' C7' 118.1(19) . . ? C8' C7' C14' 122.9(18) . . ? C8' C7' C6' 115.9(17) . . ? C14' C7' C6' 121.2(17) . . ? O2' C8' C7' 119.6(17) . . ? O2' C8' C4' 117.2(16) . . ? C7' C8' C4' 120.7(18) . . ? O4' C11' C5' 129.0(17) . . ? O4' C11' C12' 123.0(18) . . ? C5' C11' C12' 107.3(19) . . ? O3' C12' O5' 116.7(17) . . ? O3' C12' C13' 112.2(16) . . ? O5' C12' C13' 108.2(17) . . ? O3' C12' C11' 102.6(16) . . ? O5' C12' C11' 105.9(14) . . ? C13' C12' C11' 110.8(15) . . ? O11' C122 N1' 119.2(17) . . ? O11' C122 C16' 125.8(19) . . ? N1' C122 C16' 114.7(19) . . ? C17' C16' C122 120.7(19) . . ? C17' C16' C30' 127.9(19) . . ? C122 C16' C30' 111.1(17) . . ? C16' C17' C18' 124.0(19) . . ? C19' C18' C17' 129(2) . . ? C18' C19' C20' 124(2) . . ? C21' C20' C19' 117.5(19) . . ? C21' C20' C31' 110.0(18) . . ? C19' C20' C31' 108.5(19) . . ? O10' C21' C20' 108.8(17) . . ? O10' C21' C22' 110.3(18) . . ? C20' C21' C22' 119.0(19) . . ? C23' C22' C21' 112.4(18) . . ? C23' C22' C32' 109.6(18) . . ? C21' C22' C32' 110.9(17) . . ? C22' C23' C24' 120.1(18) . . ? C22' C23' O9' 113.5(17) . . ? C24' C23' O9' 102.7(15) . . ? C25' C24' C23' 115.7(18) . . ? C25' C24' C33' 109.0(16) . . ? C23' C24' C33' 105.9(16) . . ? C24' C25' C26' 120.7(18) . . ? C24' C25' O7' 106.9(16) . . ? C26' C25' O7' 104.2(15) . . ? C27' C26' C25' 121.2(18) . . ? C27' C26' C34' 108.1(17) . . ? C25' C26' C34' 111.4(17) . . ? O6' C27' C26' 105.1(17) . . ? O6' C27' C28' 114.5(17) . . ? C26' C27' C28' 116.8(18) . . ? C29' C28' C27' 122(2) . . ? C28' C29' O5' 129(2) . . ? C19 C18 C17 131(2) . . ? O8' C35' O7' 121(2) . . ? O8' C35' C36' 122(2) . . ? O7' C35' C36' 117(3) . . ? C6A N2' C2A 126.2(18) . . ? C6A N2' C1' 103.1(15) . . ? C2A N2' C1' 130.6(15) . . ? C6A N3' C9' 104.7(14) . . ? C2' N1' C122 124.0(16) . . ? C12' O3' C6' 111.5(16) . . ? C27' O6' C37' 116.9(17) . . ? C35' O7' C25' 120.7(19) . . ? C29' O5' C12' 119.0(16) . . ? _diffrn_measured_fraction_theta_max 0.882 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.923 _refine_diff_density_max 1.274 _refine_diff_density_min -0.709 _refine_diff_density_rms 0.200 # Attachment '- alfa_0.5w_RT.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2012-03-26 at 11:24:17 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\acta.reqdat # CIF files read : riduzione_totale_1 #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_riduzione_totale_1 _database_code_depnum_ccdc_archive 'CCDC 886510' #TrackingRef '- alfa_0.5w_RT.cif' _audit_creation_date 2012-03-26T11:24:17-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_formula_sum 'C43 H52 N3 O11.50' _chemical_formula_weight 794.89 _chemical_absolute_configuration rm #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.579(4) _cell_length_b 20.232(4) _cell_length_c 16.329(4) _cell_angle_alpha 90 _cell_angle_beta 111.23(3) _cell_angle_gamma 90 _cell_volume 4489.4(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.163 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 0.084 _exptl_absorpt_correction_T_min 0.98216 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #============================================================================== # EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_number 38620 _diffrn_reflns_av_R_equivalents 0.179 _diffrn_reflns_av_unetI/netI 0.4886 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 29.37 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_max 0.852 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 #============================================================================== # STRUCTURE SOLUTION _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _reflns_number_total 20151 _reflns_number_gt 4258 _reflns_threshold_expression >2\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.4147 _refine_ls_R_factor_gt 0.1412 _refine_ls_wR_factor_ref 0.4502 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 0.947 _refine_ls_number_reflns 20151 _refine_ls_number_parameters 992 _refine_ls_number_restraints 29 _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1489P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.126 _refine_ls_shift/su_mean 0.017 _refine_diff_density_max 1.021 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.085 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0072(11) _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' #============================================================================== # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol C9 0.2169(10) 0.6274(7) 0.8810(8) 0.067(4) Uani d D 1 . . C C1 0.1172(9) 0.6065(6) 0.8439(7) 0.061(4) Uani d D 1 . . C C2 0.0426(10) 0.6401(7) 0.8537(8) 0.076(4) Uani d D 1 . . C C3 0.0664(11) 0.6985(7) 0.9041(9) 0.063(4) Uani d D 1 . . C C4 0.1649(8) 0.7214(8) 0.9408(8) 0.062(4) Uani d D 1 . . C C10 0.2443(10) 0.6870(7) 0.9303(9) 0.071(4) Uani d D 1 . . C C5 0.3460(9) 0.6999(7) 0.9739(9) 0.068(4) Uani d D 1 . . C C6 0.4147(11) 0.6615(7) 0.9589(10) 0.074(4) Uani d D 1 . . C C7 0.3919(11) 0.6047(8) 0.9086(11) 0.078(4) Uani d D 1 . . C C8 0.2965(11) 0.5884(8) 0.8691(10) 0.078(4) Uani d D 1 . . C C20 -0.2072(11) 0.5698(8) 1.0578(10) 0.083(5) Uani d . 1 . . C C22 -0.0490(9) 0.5795(7) 1.1918(10) 0.066(4) Uani d . 1 . . C H22 -0.0565 0.6274 1.1952 0.079 Uiso calc R 1 . . H C2A -0.0402(11) 0.6562(10) 0.6002(9) 0.104(6) Uani d D 1 . . C H2A -0.0883 0.6807 0.6116 0.124 Uiso calc R 1 . . H C5A 0.1047(11) 0.5787(7) 0.5740(8) 0.084(5) Uani d D 1 . . C H5A 0.1539 0.5536 0.5654 0.101 Uiso calc R 1 . . H C6A 0.1281(10) 0.6403(6) 0.6229(7) 0.063(4) Uani d D 1 . . C C211 -0.0875(9) 0.7455(8) 0.9204(10) 0.079(5) Uani d D 1 . . C H211 -0.1294 0.7106 0.8945 0.094 Uiso calc R 1 . . H C311 -0.1253(12) 0.8010(8) 0.9487(10) 0.088(5) Uani d D 1 . . C H311 -0.1916 0.8023 0.9412 0.105 Uiso calc R 1 . . H C411 -0.0649(11) 0.8540(7) 0.9877(13) 0.096(6) Uani d D 1 . . C C511 0.0361(12) 0.8518(8) 1.0036(10) 0.081(5) Uani d D 1 . . C H511 0.0775 0.8859 1.0336 0.098 Uiso calc R 1 . . H C611 0.0725(10) 0.7982(8) 0.9737(10) 0.077(4) Uani d D 1 . . C C11 0.3948(10) 0.7517(9) 1.0325(9) 0.077(5) Uani d D 1 . . C C12 0.5114(11) 0.7424(8) 1.0561(9) 0.088(5) Uani d D 1 . . C C15 -0.1344(9) 0.6347(9) 0.7631(10) 0.068(4) Uani d . 1 . . C C16 -0.2254(11) 0.5918(9) 0.7484(10) 0.085(5) Uani d . 1 . . C C17 -0.2588(10) 0.5644(7) 0.8028(9) 0.065(4) Uani d . 1 . . C H17A -0.2594 0.5171 0.793 0.078 Uiso calc R 1 . . H H17B -0.3269 0.5781 0.7865 0.078 Uiso calc R 1 . . H C19 -0.2489(10) 0.5565(8) 0.9603(11) 0.079(4) Uani d . 1 . . C H19A -0.256 0.5089 0.9545 0.095 Uiso calc R 1 . . H H19B -0.3151 0.5743 0.9397 0.095 Uiso calc R 1 . . H C21 -0.0947(10) 0.5607(6) 1.0968(10) 0.075(4) Uani d . 1 . . C H21 -0.0654 0.588 1.0632 0.09 Uiso calc R 1 . . H C23 0.0621(9) 0.5647(7) 1.2283(10) 0.068(4) Uani d . 1 . . C H23 0.0876 0.5809 1.289 0.082 Uiso calc R 1 . . H C24 0.1238(10) 0.5976(7) 1.1809(10) 0.074(4) Uani d . 1 . . C H24 0.1048 0.5769 1.1228 0.089 Uiso calc R 1 . . H C25 0.2344(10) 0.5845(7) 1.2282(9) 0.074(5) Uani d . 1 . . C H25 0.244 0.5375 1.2433 0.089 Uiso calc R 1 . . H C26 0.2986(11) 0.6035(8) 1.1725(10) 0.078(4) Uani d . 1 . . C C27 0.4095(9) 0.6065(7) 1.2293(10) 0.075(4) Uani d . 1 . . C H27 0.4177 0.6353 1.2798 0.09 Uiso calc R 1 . . H C28 0.4674(10) 0.6372(9) 1.1761(10) 0.085(5) Uani d . 1 . . C H28 0.4772 0.6132 1.1314 0.102 Uiso calc R 1 . . H C29 0.5023(10) 0.6968(8) 1.1943(11) 0.081(5) Uani d . 1 . . C H29 0.4931 0.7201 1.2397 0.097 Uiso calc R 1 . . H C14 0.4796(11) 0.5595(8) 0.9047(13) 0.114(6) Uani d . 1 . . C H14A 0.5413 0.5778 0.9421 0.171 Uiso calc R 1 . . H H14B 0.4778 0.5576 0.8454 0.171 Uiso calc R 1 . . H H14C 0.4726 0.5157 0.9243 0.171 Uiso calc R 1 . . H C711 -0.1114(12) 0.9156(8) 1.0076(11) 0.104(6) Uani d . 1 . . C H71A -0.1803 0.9081 0.9941 0.156 Uiso calc R 1 . . H H71B -0.103 0.9516 0.9725 0.156 Uiso calc R 1 . . H H71C -0.0805 0.9265 1.0687 0.156 Uiso calc R 1 . . H C13 0.5648(10) 0.7968(9) 1.0349(10) 0.109(7) Uani d . 1 . . C H13A 0.5634 0.8347 1.0698 0.163 Uiso calc R 1 . . H H13B 0.5342 0.8077 0.9737 0.163 Uiso calc R 1 . . H H13C 0.6317 0.7838 1.0471 0.163 Uiso calc R 1 . . H C30 -0.2828(14) 0.5840(12) 0.6424(11) 0.153(10) Uani d . 1 . . C H30A -0.2464 0.6064 0.6122 0.229 Uiso calc R 1 . . H H30B -0.3473 0.6031 0.6259 0.229 Uiso calc R 1 . . H H30C -0.2885 0.538 0.627 0.229 Uiso calc R 1 . . H C31 -0.2344(10) 0.6367(8) 1.0665(10) 0.080(4) Uani d . 1 . . C H31A -0.211 0.6486 1.1275 0.12 Uiso calc R 1 . . H H31B -0.3047 0.6408 1.0421 0.12 Uiso calc R 1 . . H H31C -0.2056 0.6655 1.0356 0.12 Uiso calc R 1 . . H C32 -0.0924(11) 0.5495(7) 1.2504(9) 0.086(5) Uani d . 1 . . C H32A -0.0613 0.567 1.3086 0.129 Uiso calc R 1 . . H H32B -0.0829 0.5025 1.2517 0.129 Uiso calc R 1 . . H H32C -0.1615 0.5591 1.2297 0.129 Uiso calc R 1 . . H C33 0.1034(11) 0.6731(7) 1.1653(11) 0.100(6) Uani d . 1 . . C H33A 0.0344 0.6801 1.1338 0.149 Uiso calc R 1 . . H H33B 0.14 0.6902 1.1316 0.149 Uiso calc R 1 . . H H33C 0.1231 0.6955 1.2208 0.149 Uiso calc R 1 . . H C35 0.3039(17) 0.5942(14) 1.3897(14) 0.141(10) Uani d . 1 . . C C36 0.3426(16) 0.6483(11) 1.4613(12) 0.144(9) Uani d . 1 . . C H36A 0.34 0.6905 1.4337 0.216 Uiso calc R 1 . . H H36B 0.4093 0.6385 1.4978 0.216 Uiso calc R 1 . . H H36C 0.3024 0.6493 1.4966 0.216 Uiso calc R 1 . . H C34 0.2785(10) 0.5556(7) 1.0968(10) 0.088(5) Uani d . 1 . . C H34A 0.3204 0.5658 1.0648 0.133 Uiso calc R 1 . . H H34B 0.2109 0.5593 1.0584 0.133 Uiso calc R 1 . . H H34C 0.2913 0.5113 1.1192 0.133 Uiso calc R 1 . . H C37 0.5400(14) 0.5409(11) 1.3254(13) 0.153(9) Uani d . 1 . . C H37A 0.5603 0.4966 1.3448 0.229 Uiso calc R 1 . . H H37B 0.5427 0.5676 1.3748 0.229 Uiso calc R 1 . . H H37C 0.583 0.5591 1.2985 0.229 Uiso calc R 1 . . H N2 0.0115(9) 0.7412(6) 0.9299(7) 0.078(4) Uani d D 1 . . N N3 0.1669(8) 0.7802(5) 0.9842(8) 0.068(3) Uani d D 1 . . N N1 -0.0548(8) 0.6061(6) 0.8249(7) 0.069(3) Uani d . 1 . . N H1 -0.0606 0.5686 0.8473 0.083 Uiso calc R 1 . . H O3 0.5111(6) 0.6806(6) 1.0086(8) 0.098(4) Uani d D 1 . . O O2 0.2716(7) 0.5350(5) 0.8162(8) 0.103(4) Uani d . 1 . . O H2 0.2115 0.5321 0.7943 0.155 Uiso calc R 1 . . H O1 0.0982(7) 0.5491(5) 0.7964(7) 0.085(3) Uani d . 1 . . O O4 0.3676(7) 0.7995(6) 1.0609(7) 0.090(3) Uani d . 1 . . O O11 -0.1377(7) 0.6911(6) 0.7392(7) 0.095(4) Uani d . 1 . . O O10 -0.0772(7) 0.4922(5) 1.0828(7) 0.093(3) Uani d . 1 . . O O9 0.0838(6) 0.4962(5) 1.2319(7) 0.085(3) Uani d . 1 . . O O7 0.2682(7) 0.6235(5) 1.3099(8) 0.084(3) Uani d . 1 . . O O6 0.4403(8) 0.5398(5) 1.2622(9) 0.113(4) Uani d . 1 . . O O5 0.5537(7) 0.7261(6) 1.1458(7) 0.092(3) Uani d . 1 . . O O8 0.2994(11) 0.5361(9) 1.3963(8) 0.152(6) Uani d . 1 . . O C4A 0.0055(10) 0.5580(7) 0.5398(9) 0.071(4) Uani d D 1 . . C C3A -0.0671(10) 0.6013(7) 0.5507(9) 0.067(4) Uani d D 1 . . C H3A -0.1335 0.5914 0.5231 0.081 Uiso calc R 1 . . H C9' 0.2033(10) 0.7271(5) 0.7037(9) 0.064(4) Uani d D 1 . . C C1' 0.1009(8) 0.7336(6) 0.6854(7) 0.050(3) Uani d D 1 . . C C2' 0.0687(9) 0.7876(6) 0.7214(8) 0.058(4) Uani d D 1 . . C C3' 0.1334(9) 0.8339(6) 0.7706(9) 0.063(4) Uani d D 1 . . C C4' 0.2415(9) 0.8264(7) 0.7860(8) 0.070(4) Uani d D 1 . . C C10' 0.2772(10) 0.7711(7) 0.7497(8) 0.063(4) Uani d D 1 . . C C5' 0.3720(8) 0.7710(6) 0.7618(9) 0.060(4) Uani d D 1 . . C C6' 0.4360(8) 0.8248(6) 0.8063(8) 0.050(3) Uani d D 1 . . C C7' 0.4088(9) 0.8767(7) 0.8400(7) 0.068(4) Uani d D 1 . . C C8' 0.3086(10) 0.8826(7) 0.8307(8) 0.072(4) Uani d D 1 . . C C11' 0.4291(10) 0.7261(8) 0.7303(8) 0.078(5) Uani d D 1 . . C C12' 0.5376(9) 0.7517(7) 0.7653(9) 0.069(4) Uani d D 1 . . C C122 -0.0868(8) 0.8504(7) 0.6642(10) 0.065(4) Uani d . 1 . . C C16' -0.1937(10) 0.8479(7) 0.6475(11) 0.071(4) Uani d . 1 . . C C17' -0.2513(11) 0.8298(7) 0.5628(13) 0.083(5) Uani d . 1 . . C H17C -0.2983 0.8654 0.5406 0.1 Uiso calc R 1 . . H H17D -0.289 0.7919 0.569 0.1 Uiso calc R 1 . . H C18' -0.2186(9) 0.8136(7) 0.4931(11) 0.071(4) Uani d . 1 . . C H18' -0.151 0.8142 0.5064 0.086 Uiso calc R 1 . . H C19' -0.2734(11) 0.7979(8) 0.4118(14) 0.097(6) Uani d . 1 . . C H19C -0.3192 0.8342 0.3902 0.117 Uiso calc R 1 . . H H19D -0.3124 0.7602 0.4164 0.117 Uiso calc R 1 . . H C20' -0.2352(10) 0.7805(7) 0.3345(11) 0.083(5) Uani d . 1 . . C C21' -0.1348(9) 0.8112(8) 0.3500(10) 0.080(5) Uani d . 1 . . C H21' -0.0896 0.797 0.4079 0.096 Uiso calc R 1 . . H C22' -0.0842(10) 0.8007(9) 0.2845(11) 0.086(5) Uani d . 1 . . C H22' -0.0739 0.7528 0.2845 0.103 Uiso calc R 1 . . H C23' 0.0160(10) 0.8295(7) 0.3077(9) 0.078(5) Uani d . 1 . . C H23' 0.0433 0.8134 0.2647 0.093 Uiso calc R 1 . . H C24' 0.0944(12) 0.8144(8) 0.4031(10) 0.084(4) Uani d . 1 . . C H24' 0.0713 0.8346 0.4467 0.1 Uiso calc R 1 . . H C25' 0.1956(10) 0.8439(7) 0.4146(10) 0.076(4) Uani d . 1 . . C H25' 0.1872 0.8901 0.3954 0.091 Uiso calc R 1 . . H C26' 0.2679(8) 0.8406(8) 0.5094(9) 0.069(4) Uani d . 1 . . C H26' 0.2668 0.7958 0.5319 0.083 Uiso calc R 1 . . H C27' 0.3720(10) 0.8549(7) 0.5103(9) 0.079(4) Uani d . 1 . . C H27' 0.3845 0.8274 0.466 0.094 Uiso calc R 1 . . H C28' 0.4505(10) 0.8389(7) 0.6035(10) 0.080(5) Uani d . 1 . . C H28' 0.4564 0.8666 0.6505 0.095 Uiso calc R 1 . . H C29' 0.5078(9) 0.7871(7) 0.6158(9) 0.066(4) Uani d . 1 . . C H29' 0.5073 0.7666 0.5647 0.079 Uiso calc R 1 . . H C14' 0.4792(10) 0.9330(7) 0.8807(10) 0.083(5) Uani d . 1 . . C H14D' 0.4463 0.9659 0.9024 0.125 Uiso calc R 1 . . H H14E' 0.5009 0.9524 0.8372 0.125 Uiso calc R 1 . . H H14F' 0.535 0.9165 0.9284 0.125 Uiso calc R 1 . . H C7A -0.0224(12) 0.4965(8) 0.4996(10) 0.090(5) Uani d . 1 . . C H7A1' 0.0349 0.473 0.4998 0.135 Uiso calc R 1 . . H H7A2' -0.0667 0.5027 0.4401 0.135 Uiso calc R 1 . . H H7A3' -0.0547 0.4714 0.5312 0.135 Uiso calc R 1 . . H C13' 0.6065(9) 0.7081(8) 0.8314(10) 0.100(6) Uani d . 1 . . C H13D' 0.5847 0.7026 0.8798 0.149 Uiso calc R 1 . . H H13E' 0.6709 0.7275 0.852 0.149 Uiso calc R 1 . . H H13F' 0.6087 0.6659 0.8055 0.149 Uiso calc R 1 . . H C30' -0.2298(10) 0.8648(8) 0.7182(10) 0.086(5) Uani d . 1 . . C H30D' -0.175 0.8748 0.7709 0.13 Uiso calc R 1 . . H H30E' -0.2656 0.8279 0.7288 0.13 Uiso calc R 1 . . H H30F' -0.2724 0.9025 0.7011 0.13 Uiso calc R 1 . . H C31' -0.2285(13) 0.7042(9) 0.3264(13) 0.117(6) Uani d . 1 . . C H31A' -0.2024 0.6939 0.2817 0.176 Uiso calc R 1 . . H H31B' -0.2929 0.6852 0.311 0.176 Uiso calc R 1 . . H H31C' -0.186 0.6863 0.3816 0.176 Uiso calc R 1 . . H C32' -0.1500(11) 0.8165(9) 0.1916(11) 0.105(6) Uani d . 1 . . C H32D' -0.1168 0.8057 0.1522 0.158 Uiso calc R 1 . . H H32E' -0.1657 0.8628 0.187 0.158 Uiso calc R 1 . . H H32F' -0.2096 0.7912 0.1764 0.158 Uiso calc R 1 . . H C33' 0.0990(11) 0.7358(8) 0.4172(12) 0.102(6) Uani d . 1 . . C H33D' 0.0352 0.7198 0.4122 0.152 Uiso calc R 1 . . H H33E' 0.1458 0.7254 0.4745 0.152 Uiso calc R 1 . . H H33F' 0.1188 0.7151 0.3733 0.152 Uiso calc R 1 . . H C18 -0.2097(11) 0.5756(7) 0.9003(12) 0.086(5) Uani d . 1 . . C H018' -0.149 0.5969 0.9205 0.103 Uiso calc R 1 . . H C35' 0.2580(14) 0.8370(9) 0.2966(12) 0.097(6) Uani d . 1 . . C C36' 0.3135(15) 0.7986(10) 0.2548(14) 0.128(7) Uani d . 1 . . C H36D' 0.3187 0.7537 0.2748 0.193 Uiso calc R 1 . . H H36E' 0.3782 0.8171 0.2698 0.193 Uiso calc R 1 . . H H36F' 0.2802 0.7998 0.1922 0.193 Uiso calc R 1 . . H C34' 0.2406(11) 0.8872(8) 0.5647(11) 0.098(5) Uani d . 1 . . C H34A' 0.2875 0.8847 0.6237 0.147 Uiso calc R 1 . . H H34B' 0.1763 0.8764 0.5643 0.147 Uiso calc R 1 . . H H34C' 0.24 0.9312 0.5425 0.147 Uiso calc R 1 . . H C37' 0.46597(19) 0.93832(13) 0.46779(18) 0.121(7) Uani d . 1 . . C H37D' 0.4665 0.9848 0.456 0.181 Uiso calc R 1 . . H H37E' 0.4629 0.9137 0.4166 0.181 Uiso calc R 1 . . H H37F' 0.5249 0.9268 0.516 0.181 Uiso calc R 1 . . H N2' 0.05965(19) 0.67831(13) 0.63577(18) 0.058(3) Uani d D 1 . . N N3' 0.21887(19) 0.66882(13) 0.66445(18) 0.061(3) Uani d D 1 . . N N1' -0.03749(19) 0.79704(13) 0.70147(18) 0.064(3) Uani d . 1 . . N H1' -0.0693 0.7657 0.715 0.076 Uiso calc R 1 . . H O3' 0.53205(19) 0.81763(13) 0.80249(18) 0.088(3) Uani d D 1 . . O O2' 0.27636(19) 0.92424(13) 0.87051(18) 0.097(3) Uani d . 1 . . O H2' 0.218 0.917 0.8605 0.145 Uiso calc R 1 . . H O1' 0.10751(19) 0.88140(13) 0.81471(18) 0.080(3) Uani d . 1 . . O O6' 0.37912(19) 0.92241(13) 0.49066(18) 0.105(4) Uani d . 1 . . O O4' 0.41077(19) 0.66970(13) 0.69201(18) 0.082(3) Uani d . 1 . . O O11' -0.05127(19) 0.90097(13) 0.64638(18) 0.082(3) Uani d . 1 . . O O10' -0.14685(19) 0.88345(13) 0.35231(18) 0.104(4) Uani d . 1 . . O O9' 0.00709(19) 0.89886(13) 0.29884(18) 0.093(3) Uani d . 1 . . O O7' 0.23244(19) 0.80714(13) 0.35893(18) 0.079(3) Uani d . 1 . . O O5' 0.56826(19) 0.75864(13) 0.69200(18) 0.083(3) Uani d . 1 . . O O8' 0.24339(19) 0.89555(13) 0.27927(18) 0.126(5) Uani d . 1 . . O O1W -0.06744(19) 0.46731(13) 0.82327(18) 0.116(4) Uani d . 1 . . O loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C9 0.058(9) 0.076(10) 0.066(9) 0.010(8) 0.021(7) 0.008(8) C1 0.035(8) 0.053(8) 0.086(10) -0.005(6) 0.010(7) 0.009(8) C2 0.044(9) 0.086(11) 0.092(12) -0.007(8) 0.019(8) 0.013(10) C3 0.071(10) 0.064(9) 0.049(8) 0.002(8) 0.018(7) -0.003(8) C4 0.026(7) 0.109(12) 0.046(8) -0.008(7) 0.007(6) 0.008(8) C10 0.056(9) 0.093(11) 0.059(9) -0.014(8) 0.014(7) 0.005(9) C5 0.038(7) 0.091(10) 0.082(11) -0.003(7) 0.029(7) -0.016(9) C6 0.070(11) 0.066(9) 0.097(12) -0.002(8) 0.045(9) -0.003(9) C7 0.060(10) 0.082(11) 0.102(12) -0.001(8) 0.042(9) 0.015(10) C8 0.055(10) 0.089(12) 0.091(12) 0.014(9) 0.028(8) 0.011(10) C20 0.075(11) 0.103(12) 0.064(11) 0.034(9) 0.017(8) 0.005(9) C22 0.066(9) 0.061(8) 0.081(11) 0.010(7) 0.038(9) 0.017(8) C2A 0.057(10) 0.19(2) 0.064(10) -0.046(11) 0.024(8) 0.004(12) C5A 0.082(11) 0.069(10) 0.094(12) 0.031(9) 0.022(9) 0.008(9) C6A 0.064(9) 0.045(8) 0.083(10) 0.015(7) 0.030(8) 0.010(8) C211 0.034(8) 0.096(11) 0.110(13) -0.019(8) 0.030(8) -0.017(10) C311 0.081(11) 0.089(12) 0.086(11) 0.011(11) 0.021(9) -0.004(10) C411 0.054(9) 0.059(9) 0.178(18) 0.005(8) 0.048(11) 0.006(11) C511 0.085(12) 0.083(11) 0.077(11) -0.002(9) 0.029(9) -0.029(9) C611 0.059(10) 0.094(11) 0.079(11) -0.014(9) 0.025(8) -0.020(9) C11 0.040(8) 0.112(13) 0.088(12) -0.006(9) 0.033(8) -0.008(11) C12 0.073(10) 0.095(12) 0.064(11) 0.020(9) -0.013(8) -0.003(10) C15 0.026(7) 0.101(12) 0.073(10) -0.012(8) 0.011(7) -0.025(10) C16 0.076(11) 0.108(13) 0.066(11) -0.005(9) 0.018(9) 0.000(10) C17 0.059(9) 0.060(9) 0.060(10) 0.009(7) 0.002(8) 0.012(8) C19 0.066(10) 0.080(10) 0.097(13) -0.005(8) 0.038(10) -0.008(9) C21 0.079(10) 0.048(8) 0.090(12) -0.010(7) 0.023(9) -0.012(8) C23 0.057(9) 0.076(10) 0.077(10) 0.013(7) 0.031(8) 0.022(8) C24 0.066(9) 0.086(11) 0.073(10) 0.009(8) 0.027(8) -0.012(9) C25 0.083(11) 0.053(8) 0.062(10) -0.010(7) -0.003(8) 0.009(8) C26 0.084(11) 0.090(11) 0.079(10) -0.007(9) 0.052(9) -0.012(9) C27 0.043(8) 0.087(11) 0.082(10) -0.003(8) 0.007(7) -0.009(9) C28 0.070(10) 0.127(14) 0.065(10) -0.018(10) 0.034(8) 0.006(10) C29 0.054(9) 0.081(10) 0.109(13) -0.020(8) 0.031(9) 0.015(10) C14 0.065(10) 0.100(12) 0.19(2) 0.008(9) 0.056(12) -0.015(13) C711 0.098(13) 0.111(13) 0.106(14) 0.027(11) 0.039(11) -0.003(11) C13 0.067(10) 0.138(14) 0.095(12) -0.056(10) -0.003(9) 0.053(11) C30 0.111(15) 0.22(2) 0.095(14) -0.097(16) -0.004(12) -0.015(15) C31 0.053(8) 0.099(12) 0.084(11) 0.014(8) 0.021(8) 0.014(9) C32 0.086(11) 0.084(11) 0.072(11) 0.006(9) 0.009(9) 0.015(9) C33 0.085(11) 0.065(10) 0.120(14) 0.022(8) 0.002(10) -0.004(10) C35 0.17(2) 0.15(2) 0.099(17) 0.076(18) 0.039(14) 0.104(18) C36 0.19(2) 0.161(19) 0.074(12) 0.006(17) 0.046(14) -0.056(14) C34 0.061(9) 0.092(11) 0.109(13) -0.017(8) 0.027(9) -0.017(10) C37 0.115(16) 0.16(2) 0.135(18) 0.035(14) -0.010(14) 0.070(15) N2 0.076(9) 0.093(9) 0.054(7) -0.028(8) 0.010(7) -0.012(7) N3 0.053(7) 0.056(7) 0.092(9) 0.008(5) 0.021(6) 0.001(7) N1 0.049(7) 0.078(8) 0.077(8) -0.012(6) 0.019(6) -0.009(7) O3 0.036(5) 0.135(10) 0.118(9) -0.014(6) 0.020(5) 0.010(8) O2 0.083(7) 0.074(7) 0.160(11) -0.013(6) 0.053(7) -0.041(8) O1 0.070(6) 0.086(7) 0.101(8) 0.004(5) 0.033(6) -0.015(6) O4 0.053(6) 0.109(8) 0.089(8) -0.010(6) 0.005(5) -0.013(7) O11 0.063(6) 0.088(7) 0.119(9) -0.015(6) 0.013(6) 0.040(7) O10 0.087(7) 0.083(7) 0.118(9) 0.002(6) 0.046(7) -0.037(6) O9 0.060(6) 0.072(7) 0.120(9) 0.015(5) 0.028(6) 0.024(6) O7 0.065(6) 0.077(7) 0.109(9) 0.001(5) 0.032(6) 0.002(7) O6 0.074(7) 0.089(8) 0.164(12) 0.011(6) 0.028(8) 0.024(8) O5 0.053(6) 0.119(8) 0.080(8) -0.009(6) -0.004(5) 0.016(7) O8 0.184(15) 0.166(14) 0.067(8) 0.011(12) -0.002(8) 0.061(9) C4A 0.048(9) 0.072(10) 0.091(11) -0.008(8) 0.022(8) 0.012(9) C3A 0.061(9) 0.057(8) 0.066(9) -0.019(8) 0.003(7) -0.008(8) C9' 0.084(10) 0.025(6) 0.073(9) 0.012(7) 0.016(8) 0.009(7) C1' 0.044(7) 0.059(8) 0.046(8) 0.000(6) 0.015(6) -0.016(7) C2' 0.056(8) 0.069(9) 0.065(9) 0.002(7) 0.040(7) 0.008(8) C3' 0.054(8) 0.059(8) 0.092(11) -0.008(7) 0.045(8) -0.004(8) C4' 0.044(8) 0.083(10) 0.067(9) 0.010(7) 0.001(7) -0.019(8) C10' 0.055(8) 0.082(10) 0.044(8) -0.036(8) 0.008(7) -0.010(7) C5' 0.036(7) 0.062(8) 0.099(11) 0.010(6) 0.046(7) -0.011(8) C6' 0.044(7) 0.051(8) 0.063(8) 0.009(6) 0.031(6) 0.013(7) C7' 0.033(7) 0.080(10) 0.083(10) 0.004(7) 0.011(7) -0.010(9) C8' 0.050(9) 0.084(11) 0.068(10) 0.006(8) 0.003(7) -0.009(9) C11' 0.072(10) 0.098(12) 0.051(9) -0.019(9) 0.006(8) 0.010(9) C12' 0.055(8) 0.093(11) 0.060(9) -0.001(8) 0.024(7) 0.006(8) C122 0.030(7) 0.065(9) 0.102(11) -0.017(6) 0.025(7) 0.009(8) C16' 0.049(8) 0.072(9) 0.091(11) 0.012(7) 0.026(8) -0.020(9) C17' 0.065(10) 0.045(8) 0.145(16) 0.003(7) 0.044(11) 0.009(9) C18' 0.031(7) 0.081(10) 0.100(12) -0.001(7) 0.021(8) -0.041(9) C19' 0.067(10) 0.074(11) 0.153(18) -0.019(9) 0.042(12) -0.011(12) C20' 0.058(9) 0.058(9) 0.119(14) -0.005(7) 0.014(9) -0.011(9) C21' 0.042(8) 0.085(10) 0.088(12) -0.008(8) -0.007(8) -0.003(9) C22' 0.049(9) 0.111(12) 0.091(12) -0.002(9) 0.017(9) 0.002(10) C23' 0.061(9) 0.088(11) 0.073(10) 0.030(8) 0.012(7) 0.036(9) C24' 0.098(12) 0.087(11) 0.076(11) 0.007(10) 0.043(9) -0.002(9) C25' 0.060(9) 0.079(10) 0.093(12) 0.015(8) 0.034(9) 0.014(9) C26' 0.033(7) 0.113(12) 0.057(9) -0.006(7) 0.009(6) 0.001(8) C27' 0.078(10) 0.067(9) 0.070(10) 0.001(8) 0.002(8) 0.011(8) C28' 0.057(9) 0.079(10) 0.087(11) 0.008(8) 0.008(8) -0.003(9) C29' 0.047(7) 0.084(10) 0.060(9) 0.007(7) 0.012(7) 0.005(8) C14' 0.081(11) 0.082(10) 0.082(11) -0.034(8) 0.025(9) -0.027(9) C7A 0.097(12) 0.093(12) 0.082(11) -0.028(10) 0.034(9) -0.018(10) C13' 0.046(8) 0.128(14) 0.099(13) 0.016(9) -0.005(8) 0.014(11) C30' 0.059(9) 0.101(12) 0.108(13) 0.000(8) 0.040(9) 0.013(10) C31' 0.095(13) 0.122(15) 0.134(17) 0.024(11) 0.041(11) -0.001(13) C32' 0.071(11) 0.127(14) 0.120(15) -0.004(10) 0.037(11) 0.025(12) C33' 0.084(11) 0.089(12) 0.120(14) -0.028(10) 0.024(10) -0.007(11) C18 0.070(10) 0.075(10) 0.111(14) 0.013(8) 0.030(11) 0.022(10) C35' 0.109(14) 0.094(14) 0.083(13) -0.008(11) 0.027(11) -0.034(11) C36' 0.143(17) 0.096(13) 0.17(2) -0.018(13) 0.086(16) 0.007(14) C34' 0.071(10) 0.111(12) 0.116(14) 0.018(9) 0.039(10) -0.035(11) C37' 0.123(16) 0.122(15) 0.118(16) -0.042(12) 0.046(13) 0.021(12) N2' 0.056(7) 0.057(7) 0.066(7) -0.003(6) 0.028(6) -0.002(6) N3' 0.060(7) 0.050(6) 0.064(7) -0.007(5) 0.011(6) -0.010(6) N1' 0.043(6) 0.071(7) 0.072(8) 0.003(6) 0.015(5) 0.012(6) O3' 0.046(6) 0.088(7) 0.121(8) -0.005(5) 0.022(5) -0.035(7) O2' 0.089(8) 0.090(8) 0.115(9) -0.018(6) 0.041(7) -0.027(7) O1' 0.093(7) 0.066(6) 0.097(8) 0.015(5) 0.051(6) -0.017(6) O6' 0.078(7) 0.110(9) 0.107(9) 0.000(6) 0.008(6) 0.025(7) O4' 0.066(6) 0.076(7) 0.113(8) -0.002(5) 0.044(6) -0.015(6) O11' 0.066(6) 0.076(7) 0.098(8) 0.008(5) 0.019(6) 0.012(6) O10' 0.066(7) 0.112(9) 0.136(10) -0.029(6) 0.040(6) -0.033(8) O9' 0.076(7) 0.100(8) 0.079(7) 0.004(6) -0.002(5) 0.011(6) O7' 0.076(7) 0.071(6) 0.086(8) -0.008(5) 0.026(6) 0.002(6) O5' 0.052(5) 0.113(8) 0.071(7) 0.012(5) 0.008(5) 0.012(6) O8' 0.152(12) 0.116(10) 0.148(12) 0.033(9) 0.100(10) 0.043(9) O1W 0.131(10) 0.103(8) 0.108(9) -0.002(8) 0.036(8) 0.014(7) #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C9 C1 . 1.421(17) ? C9 C10 . 1.424(18) ? C9 C8 . 1.474(19) ? C1 C2 . 1.340(18) ? C1 O1 . 1.368(15) ? C2 C3 . 1.410(19) ? C2 N1 . 1.491(16) ? C3 N2 . 1.345(17) ? C3 C4 . 1.418(17) ? C4 N3 . 1.380(17) ? C4 C10 . 1.413(19) ? C10 C5 . 1.418(17) ? C5 C6 . 1.358(18) ? C5 C11 . 1.42(2) ? C6 C7 . 1.38(2) ? C6 O3 . 1.399(16) ? C7 C8 . 1.346(19) ? C7 C14 . 1.591(19) ? C8 O2 . 1.348(17) ? C20 C31 . 1.432(19) ? C20 C19 . 1.51(2) ? C20 C21 . 1.540(19) ? C22 C32 . 1.457(18) ? C22 C21 . 1.499(19) ? C22 C23 . 1.539(17) ? C2A C3A . 1.35(2) ? C2A N2' . 1.430(14) ? C5A C4A . 1.412(18) ? C5A C6A . 1.452(18) ? C6A N2' . 1.336(13) ? C6A N3' . 1.377(14) ? C211 N2 . 1.396(17) ? C211 C311 . 1.40(2) ? C311 C411 . 1.39(2) ? C411 C511 . 1.400(19) ? C411 C711 . 1.51(2) ? C511 C611 . 1.373(19) ? C611 N3 . 1.372(17) ? C611 N2 . 1.474(17) ? C11 O4 . 1.201(17) ? C11 C12 . 1.61(2) ? C12 O5 . 1.408(15) ? C12 C13 . 1.460(19) ? C12 O3 . 1.471(18) ? C15 O11 . 1.201(17) ? C15 N1 . 1.361(16) ? C15 C16 . 1.53(2) ? C16 C17 . 1.282(19) ? C16 C30 . 1.63(2) ? C17 C18 . 1.51(2) ? C19 C18 . 1.36(2) ? C21 O10 . 1.441(15) ? C23 O9 . 1.419(15) ? C23 C24 . 1.535(18) ? C24 C25 . 1.538(18) ? C24 C33 . 1.559(19) ? C25 O7 . 1.472(16) ? C25 C26 . 1.57(2) ? C26 C34 . 1.514(19) ? C26 C27 . 1.546(18) ? C27 O6 . 1.462(16) ? C27 C28 . 1.54(2) ? C28 C29 . 1.300(19) ? C29 O5 . 1.402(17) ? C35 O8 . 1.18(2) ? C35 O7 . 1.353(19) ? C35 C36 . 1.55(3) ? C37 O6 . 1.445(18) ? C4A C7A . 1.397(19) ? C4A C3A . 1.434(19) ? C9' C10' . 1.389(16) ? C9' N3' . 1.399(13) ? C9' C1' . 1.419(17) ? C1' N2' . 1.384(12) ? C1' C2' . 1.400(16) ? C2' C3' . 1.366(17) ? C2' N1' . 1.475(13) ? C3' O1' . 1.334(14) ? C3' C4' . 1.511(18) ? C4' C10' . 1.447(18) ? C4' C8' . 1.506(18) ? C10' C5' . 1.324(16) ? C5' C6' . 1.446(16) ? C5' C11' . 1.447(19) ? C6' C7' . 1.312(16) ? C6' O3' . 1.431(12) ? C7' C8' . 1.418(17) ? C7' C14' . 1.517(17) ? C8' O2' . 1.254(15) ? C11' O4' . 1.282(16) ? C11' C12' . 1.563(18) ? C12' O5' . 1.427(14) ? C12' C13' . 1.471(18) ? C12' O3' . 1.481(15) ? C122 O11' . 1.228(13) ? C122 N1' . 1.318(14) ? C122 C16' . 1.482(17) ? C16' C17' . 1.382(19) ? C16' C30' . 1.47(2) ? C17' C18' . 1.42(2) ? C18' C19' . 1.32(2) ? C19' C20' . 1.59(2) ? C20' C21' . 1.524(19) ? C20' C31' . 1.56(2) ? C21' O10' . 1.474(16) ? C21' C22' . 1.52(2) ? C22' C23' . 1.488(19) ? C22' C32' . 1.507(19) ? C23' O9' . 1.412(14) ? C23' C24' . 1.592(19) ? C24' C25' . 1.538(19) ? C24' C33' . 1.61(2) ? C25' O7' . 1.422(16) ? C25' C26' . 1.526(18) ? C26' C34' . 1.457(19) ? C26' C27' . 1.539(19) ? C27' O6' . 1.415(14) ? C27' C28' . 1.571(17) ? C28' C29' . 1.309(17) ? C29' O5' . 1.365(13) ? C35' O8' . 1.219(19) ? C35' O7' . 1.35(2) ? C35' C36' . 1.46(2) ? C37' O6' . 1.4795 ? 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 C1 C9 C10 121.8(13) . . ? C1 C9 C8 121.1(14) . . ? C10 C9 C8 117.1(13) . . ? C2 C1 O1 119.4(12) . . ? C2 C1 C9 123.2(13) . . ? O1 C1 C9 117.4(12) . . ? C1 C2 C3 117.1(13) . . ? C1 C2 N1 116.7(13) . . ? C3 C2 N1 125.1(13) . . ? N2 C3 C2 132.2(14) . . ? N2 C3 C4 106.5(13) . . ? C2 C3 C4 121.2(14) . . ? N3 C4 C10 128.4(11) . . ? N3 C4 C3 109.1(12) . . ? C10 C4 C3 122.4(14) . . ? C4 C10 C5 127.0(14) . . ? C4 C10 C9 114.3(12) . . ? C5 C10 C9 117.9(14) . . ? C6 C5 C10 120.6(14) . . ? C6 C5 C11 108.7(13) . . ? C10 C5 C11 130.6(13) . . ? C5 C6 C7 123.3(14) . . ? C5 C6 O3 112.8(13) . . ? C7 C6 O3 123.4(13) . . ? C8 C7 C6 118.2(15) . . ? C8 C7 C14 123.1(15) . . ? C6 C7 C14 118.6(13) . . ? O2 C8 C7 119.7(14) . . ? O2 C8 C9 118.2(13) . . ? C7 C8 C9 122.2(16) . . ? C31 C20 C19 104.6(13) . . ? C31 C20 C21 111.3(13) . . ? C19 C20 C21 112.1(13) . . ? C32 C22 C21 116.0(12) . . ? C32 C22 C23 108.1(11) . . ? C21 C22 C23 111.2(12) . . ? C3A C2A N2' 122.2(16) . . ? C4A C5A C6A 118.3(13) . . ? N2' C6A N3' 108.7(9) . . ? N2' C6A C5A 122.7(11) . . ? N3' C6A C5A 128.6(11) . . ? N2 C211 C311 121.8(14) . . ? C411 C311 C211 120.7(15) . . ? C311 C411 C511 120.7(15) . . ? C311 C411 C711 118.5(14) . . ? C511 C411 C711 120.7(15) . . ? C611 C511 C411 118.3(14) . . ? N3 C611 C511 131.6(14) . . ? N3 C611 N2 104.8(13) . . ? C511 C611 N2 123.2(14) . . ? O4 C11 C5 134.3(13) . . ? O4 C11 C12 117.9(14) . . ? C5 C11 C12 107.6(14) . . ? O5 C12 C13 110.8(13) . . ? O5 C12 O3 105.4(11) . . ? C13 C12 O3 114.5(14) . . ? O5 C12 C11 107.6(10) . . ? C13 C12 C11 117.5(11) . . ? O3 C12 C11 99.8(12) . . ? O11 C15 N1 124.6(12) . . ? O11 C15 C16 123.9(13) . . ? N1 C15 C16 109.5(15) . . ? C17 C16 C15 131.4(14) . . ? C17 C16 C30 121.0(14) . . ? C15 C16 C30 107.6(14) . . ? C16 C17 C18 120.8(14) . . ? C18 C19 C20 126.7(14) . . ? O10 C21 C22 111.7(12) . . ? O10 C21 C20 105.8(11) . . ? C22 C21 C20 113.9(13) . . ? O9 C23 C24 106.4(11) . . ? O9 C23 C22 113.2(11) . . ? C24 C23 C22 116.6(11) . . ? C23 C24 C25 111.8(12) . . ? C23 C24 C33 113.2(12) . . ? C25 C24 C33 110.7(12) . . ? O7 C25 C24 108.0(12) . . ? O7 C25 C26 108.6(11) . . ? C24 C25 C26 113.8(11) . . ? C34 C26 C27 111.5(12) . . ? C34 C26 C25 109.7(12) . . ? C27 C26 C25 112.0(12) . . ? O6 C27 C28 114.8(13) . . ? O6 C27 C26 107.4(12) . . ? C28 C27 C26 110.2(12) . . ? C29 C28 C27 119.6(16) . . ? C28 C29 O5 120.6(16) . . ? O8 C35 O7 121(2) . . ? O8 C35 C36 130.5(18) . . ? O7 C35 C36 109(2) . . ? C3 N2 C211 135.5(13) . . ? C3 N2 C611 109.3(12) . . ? C211 N2 C611 115.0(14) . . ? C611 N3 C4 109.4(11) . . ? C15 N1 C2 119.8(11) . . ? C6 O3 C12 110.6(11) . . ? C35 O7 C25 121.6(15) . . ? C37 O6 C27 110.2(12) . . ? C29 O5 C12 124.4(11) . . ? C7A C4A C5A 122.2(14) . . ? C7A C4A C3A 120.0(13) . . ? C5A C4A C3A 117.7(14) . . ? C2A C3A C4A 120.8(14) . . ? C10' C9' N3' 124.4(12) . . ? C10' C9' C1' 127.2(12) . . ? N3' C9' C1' 108.3(10) . . ? N2' C1' C2' 137.4(11) . . ? N2' C1' C9' 104.5(9) . . ? C2' C1' C9' 118.1(11) . . ? C3' C2' C1' 121.2(12) . . ? C3' C2' N1' 119.1(11) . . ? C1' C2' N1' 119.6(11) . . ? O1' C3' C2' 122.8(11) . . ? O1' C3' C4' 117.7(11) . . ? C2' C3' C4' 119.0(12) . . ? C10' C4' C8' 121.0(12) . . ? C10' C4' C3' 121.2(11) . . ? C8' C4' C3' 117.3(12) . . ? C5' C10' C9' 130.0(14) . . ? C5' C10' C4' 116.8(11) . . ? C9' C10' C4' 113.2(12) . . ? C10' C5' C6' 121.5(12) . . ? C10' C5' C11' 130.7(13) . . ? C6' C5' C11' 107.6(10) . . ? C7' C6' O3' 123.3(11) . . ? C7' C6' C5' 125.1(11) . . ? O3' C6' C5' 111.4(10) . . ? C6' C7' C8' 118.6(12) . . ? C6' C7' C14' 121.7(12) . . ? C8' C7' C14' 119.4(13) . . ? O2' C8' C7' 124.5(12) . . ? O2' C8' C4' 117.4(11) . . ? C7' C8' C4' 116.8(13) . . ? O4' C11' C5' 133.4(12) . . ? O4' C11' C12' 118.5(13) . . ? C5' C11' C12' 107.4(12) . . ? O5' C12' C13' 109.7(12) . . ? O5' C12' O3' 109.6(9) . . ? C13' C12' O3' 111.3(11) . . ? O5' C12' C11' 108.0(9) . . ? C13' C12' C11' 113.6(11) . . ? O3' C12' C11' 104.4(11) . . ? O11' C122 N1' 125.8(9) . . ? O11' C122 C16' 119.4(12) . . ? N1' C122 C16' 114.7(11) . . ? C17' C16' C30' 125.8(13) . . ? C17' C16' C122 114.2(14) . . ? C30' C16' C122 119.9(13) . . ? C16' C17' C18' 127.1(14) . . ? C19' C18' C17' 127.3(14) . . ? C18' C19' C20' 126.4(14) . . ? C21' C20' C31' 109.5(13) . . ? C21' C20' C19' 111.6(13) . . ? C31' C20' C19' 109.7(15) . . ? O10' C21' C22' 104.5(13) . . ? O10' C21' C20' 107.0(10) . . ? C22' C21' C20' 120.6(13) . . ? C23' C22' C32' 112.5(14) . . ? C23' C22' C21' 116.6(14) . . ? C32' C22' C21' 112.6(13) . . ? O9' C23' C22' 108.5(11) . . ? O9' C23' C24' 107.3(11) . . ? C22' C23' C24' 117.7(13) . . ? C25' C24' C23' 111.3(12) . . ? C25' C24' C33' 112.2(12) . . ? C23' C24' C33' 107.9(12) . . ? O7' C25' C26' 110.1(10) . . ? O7' C25' C24' 106.7(11) . . ? C26' C25' C24' 112.8(12) . . ? C34' C26' C25' 110.9(12) . . ? C34' C26' C27' 111.2(12) . . ? C25' C26' C27' 108.5(12) . . ? O6' C27' C26' 109.5(11) . . ? O6' C27' C28' 109.3(10) . . ? C26' C27' C28' 109.9(12) . . ? C29' C28' C27' 121.0(14) . . ? C28' C29' O5' 130.0(14) . . ? C19 C18 C17 123.8(15) . . ? O8' C35' O7' 122.5(16) . . ? O8' C35' C36' 119.3(18) . . ? O7' C35' C36' 117.9(16) . . ? C6A N2' C1' 111.5(8) . . ? C6A N2' C2A 117.7(11) . . ? C1' N2' C2A 130.8(10) . . ? C6A N3' C9' 107.1(8) . . ? C122 N1' C2' 124.2(7) . . ? C6' O3' C12' 108.0(7) . . ? C27' O6' C37' 114.0(7) . . ? C35' O7' C25' 121.4(10) . . ? C29' O5' C12' 120.8(8) . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF # Attachment '- alfa_0w.cif' data_alfa6_shelx _database_code_depnum_ccdc_archive 'CCDC 886511' #TrackingRef '- alfa_0w.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_moiety ? _chemical_formula_sum 'C43 H51 N3 O11' _chemical_formula_weight 785.87 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.232(4) _cell_length_b 19.822(4) _cell_length_c 16.164(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.74(3) _cell_angle_gamma 90.00 _cell_volume 4318.2(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _chemical_absolute_configuration rm _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.209 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 0.187 _exptl_absorpt_correction_T_min 0.98216 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #============================================================================== # EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.0000 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10588 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0851 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 19.83 _reflns_number_total 6941 _reflns_number_gt 4936 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1752P)^2^+0.1695P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_number_reflns 6941 _refine_ls_number_parameters 1027 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1063 _refine_ls_R_factor_gt 0.0805 _refine_ls_wR_factor_ref 0.2479 _refine_ls_wR_factor_gt 0.2215 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.100 _refine_ls_shift/su_mean 0.045 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 C9 C 0.2347(9) 0.6240(7) 0.8869(7) 0.090(3) Uani 1 1 d . . . C1 C 0.1339(10) 0.6049(7) 0.8552(7) 0.091(3) Uani 1 1 d . . . C2 C 0.0577(9) 0.6399(6) 0.8713(7) 0.086(3) Uani 1 1 d . . . C3 C 0.0880(10) 0.7015(6) 0.9191(7) 0.090(3) Uani 1 1 d . . . C4 C 0.1836(9) 0.7210(7) 0.9493(7) 0.090(3) Uani 1 1 d . . . C10 C 0.2613(8) 0.6854(6) 0.9369(6) 0.080(3) Uani 1 1 d . . . C5 C 0.3622(10) 0.7010(7) 0.9696(7) 0.093(3) Uani 1 1 d . . . C6 C 0.4331(10) 0.6593(8) 0.9581(8) 0.108(4) Uani 1 1 d . . . C7 C 0.4094(12) 0.5981(7) 0.9050(8) 0.108(4) Uani 1 1 d . . . C8 C 0.3105(10) 0.5842(8) 0.8697(8) 0.101(4) Uani 1 1 d . . . C20 C -0.1931(9) 0.5660(6) 1.0745(7) 0.095(3) Uani 1 1 d . . . H20 H -0.2236 0.5374 1.1082 0.114 Uiso 1 1 calc R . . C22 C -0.0385(8) 0.5817(6) 1.2075(7) 0.093(3) Uani 1 1 d . . . H22 H -0.0502 0.6305 1.2065 0.112 Uiso 1 1 calc R . . C2A C -0.0253(9) 0.6548(7) 0.6017(8) 0.100(3) Uani 1 1 d . . . H2A H -0.0754 0.6819 0.6092 0.120 Uiso 1 1 calc R . . C5A C 0.1211(12) 0.5733(7) 0.5793(8) 0.108(4) Uani 1 1 d . . . H5A H 0.1714 0.5461 0.5728 0.130 Uiso 1 1 calc R . . C6A C 0.1457(11) 0.6331(7) 0.6260(7) 0.091(3) Uani 1 1 d . . . C211 C -0.0659(10) 0.7574(7) 0.9364(6) 0.093(3) Uani 1 1 d . . . H211 H -0.1109 0.7241 0.9084 0.111 Uiso 1 1 calc R . . C311 C -0.0970(11) 0.8118(9) 0.9671(9) 0.113(4) Uani 1 1 d . . . H311 H -0.1636 0.8143 0.9630 0.135 Uiso 1 1 calc R . . C411 C -0.0349(15) 0.8656(8) 1.0054(8) 0.113(4) Uani 1 1 d . . . C511 C 0.0645(12) 0.8602(7) 1.0190(8) 0.103(3) Uani 1 1 d . . . H511 H 0.1089 0.8938 1.0473 0.123 Uiso 1 1 calc R . . C611 C 0.0969(10) 0.7998(7) 0.9872(7) 0.096(4) Uani 1 1 d . . . C11 C 0.4156(10) 0.7531(8) 1.0276(8) 0.105(4) Uani 1 1 d . . . C12 C 0.5243(9) 0.7361(7) 1.0476(8) 0.103(4) Uani 1 1 d . . . C15 C -0.1190(9) 0.6265(7) 0.7867(8) 0.083(3) Uani 1 1 d . . . C16 C -0.2004(8) 0.5775(7) 0.7642(7) 0.099(3) Uani 1 1 d . . . H16 H -0.1532 0.5403 0.7709 0.118 Uiso 1 1 calc R . . C17 C -0.2334(8) 0.5507(6) 0.8262(7) 0.093(3) Uani 1 1 d . . . H17 H -0.2820 0.5175 0.8083 0.111 Uiso 1 1 calc R . . C19 C -0.2274(9) 0.5407(6) 0.9799(8) 0.099(3) Uani 1 1 d . . . H19 H -0.2695 0.5035 0.9662 0.119 Uiso 1 1 calc R . . C21 C -0.0807(8) 0.5572(5) 1.1120(6) 0.085(3) Uani 1 1 d . . . H21 H -0.0506 0.5846 1.0767 0.102 Uiso 1 1 calc R . . C23 C 0.0748(8) 0.5716(6) 1.2441(7) 0.091(3) Uani 1 1 d . . . H23 H 0.0976 0.5926 1.3021 0.109 Uiso 1 1 calc R . . C24 C 0.1355(8) 0.5999(5) 1.1934(7) 0.087(3) Uani 1 1 d . . . H24 H 0.1155 0.5759 1.1374 0.105 Uiso 1 1 calc R . . C25 C 0.2481(8) 0.5878(6) 1.2351(6) 0.087(3) Uani 1 1 d . . . H25 H 0.2579 0.5403 1.2522 0.104 Uiso 1 1 calc R . . C26 C 0.3116(8) 0.6032(6) 1.1799(6) 0.091(3) Uani 1 1 d . . . H26 H 0.2914 0.6477 1.1538 0.109 Uiso 1 1 calc R . . C27 C 0.4190(9) 0.6075(6) 1.2295(7) 0.098(3) Uani 1 1 d . . . H27 H 0.4280 0.6372 1.2799 0.117 Uiso 1 1 calc R . . C28 C 0.4810(11) 0.6341(7) 1.1759(9) 0.117(4) Uani 1 1 d . . . H28 H 0.4914 0.6067 1.1329 0.140 Uiso 1 1 calc R . . C29 C 0.5196(10) 0.6933(9) 1.1882(9) 0.115(4) Uani 1 1 d . . . H29 H 0.5126 0.7175 1.2351 0.138 Uiso 1 1 calc R . . C14 C 0.4920(10) 0.5546(8) 0.8937(10) 0.139(5) Uani 1 1 d . . . H14A H 0.5550 0.5748 0.9242 0.208 Uiso 1 1 calc R . . H14B H 0.4847 0.5511 0.8327 0.208 Uiso 1 1 calc R . . H14C H 0.4886 0.5105 0.9170 0.208 Uiso 1 1 calc R . . C711 C -0.0721(12) 0.9295(7) 1.0350(11) 0.143(5) Uani 1 1 d . . . H71A H -0.1428 0.9272 1.0210 0.214 Uiso 1 1 calc R . . H71B H -0.0550 0.9675 1.0059 0.214 Uiso 1 1 calc R . . H71C H -0.0420 0.9345 1.0970 0.214 Uiso 1 1 calc R . . C13 C 0.5845(9) 0.7911(7) 1.0280(8) 0.111(4) Uani 1 1 d . . . H13A H 0.5583 0.8027 0.9672 0.167 Uiso 1 1 calc R . . H13B H 0.6520 0.7763 1.0413 0.167 Uiso 1 1 calc R . . H13C H 0.5823 0.8299 1.0629 0.167 Uiso 1 1 calc R . . C30 C -0.2462(12) 0.5615(9) 0.6696(7) 0.151(6) Uani 1 1 d . . . H30A H -0.2116 0.5853 0.6365 0.226 Uiso 1 1 calc R . . H30B H -0.3146 0.5750 0.6506 0.226 Uiso 1 1 calc R . . H30C H -0.2420 0.5138 0.6609 0.226 Uiso 1 1 calc R . . C31 C -0.2276(11) 0.6370(7) 1.0788(8) 0.128(5) Uani 1 1 d . . . H31A H -0.2064 0.6520 1.1384 0.193 Uiso 1 1 calc R . . H31B H -0.2988 0.6386 1.0557 0.193 Uiso 1 1 calc R . . H31C H -0.1999 0.6659 1.0449 0.193 Uiso 1 1 calc R . . C32 C -0.0903(10) 0.5511(6) 1.2693(8) 0.114(4) Uani 1 1 d . . . H32A H -0.1607 0.5575 1.2449 0.171 Uiso 1 1 calc R . . H32B H -0.0665 0.5730 1.3252 0.171 Uiso 1 1 calc R . . H32C H -0.0759 0.5037 1.2764 0.171 Uiso 1 1 calc R . . C33 C 0.1145(9) 0.6739(6) 1.1718(7) 0.103(3) Uani 1 1 d . . . H33A H 0.1538 0.6893 1.1371 0.155 Uiso 1 1 calc R . . H33B H 0.1310 0.6996 1.2250 0.155 Uiso 1 1 calc R . . H33C H 0.0454 0.6798 1.1397 0.155 Uiso 1 1 calc R . . C35 C 0.3095(11) 0.5970(10) 1.3932(7) 0.120(4) Uani 1 1 d . . . C36 C 0.3578(12) 0.6454(11) 1.4654(9) 0.175(8) Uani 1 1 d . . . H36A H 0.3590 0.6896 1.4414 0.262 Uiso 1 1 calc R . . H36B H 0.4245 0.6310 1.4953 0.262 Uiso 1 1 calc R . . H36C H 0.3210 0.6468 1.5057 0.262 Uiso 1 1 calc R . . C34 C 0.2894(10) 0.5520(8) 1.1035(8) 0.124(4) Uani 1 1 d . . . H34A H 0.2193 0.5512 1.0729 0.186 Uiso 1 1 calc R . . H34B H 0.3109 0.5078 1.1262 0.186 Uiso 1 1 calc R . . H34C H 0.3241 0.5651 1.0641 0.186 Uiso 1 1 calc R . . C37 C 0.5511(13) 0.5412(10) 1.3228(12) 0.168(6) Uani 1 1 d . . . H37A H 0.5693 0.4957 1.3414 0.251 Uiso 1 1 calc R . . H37B H 0.5530 0.5684 1.3724 0.251 Uiso 1 1 calc R . . H37C H 0.5969 0.5590 1.2958 0.251 Uiso 1 1 calc R . . N2 N 0.0314(8) 0.7503(5) 0.9457(5) 0.087(3) Uani 1 1 d . . . N3 N 0.1899(8) 0.7845(5) 0.9908(5) 0.089(2) Uani 1 1 d . . . N1 N -0.0357(8) 0.6094(5) 0.8484(6) 0.102(3) Uani 1 1 d . . . H1 H -0.0397 0.5745 0.8788 0.122 Uiso 1 1 calc R . . O3 O 0.5289(6) 0.6762(5) 1.0001(6) 0.110(2) Uani 1 1 d . . . O2 O 0.2838(8) 0.5289(5) 0.8249(6) 0.128(3) Uani 1 1 d . . . O1 O 0.1105(7) 0.5466(5) 0.8096(5) 0.122(3) Uani 1 1 d . . . H01 H 0.1610 0.5295 0.8049 0.182 Uiso 1 1 calc R . . O4 O 0.3851(7) 0.8028(5) 1.0587(6) 0.117(3) Uani 1 1 d . . . O11 O -0.1277(6) 0.6823(5) 0.7523(5) 0.110(2) Uani 1 1 d . . . O10 O -0.0580(7) 0.4903(4) 1.1024(5) 0.109(2) Uani 1 1 d . . . H10 H 0.0024 0.4851 1.1214 0.163 Uiso 1 1 calc R . . O9 O 0.0953(6) 0.5015(4) 1.2559(5) 0.113(3) Uani 1 1 d . . . H9 H 0.0635 0.4853 1.2854 0.169 Uiso 1 1 calc R . . O7 O 0.2808(6) 0.6284(4) 1.3144(5) 0.108(2) Uani 1 1 d . . . O6 O 0.4514(7) 0.5420(5) 1.2602(7) 0.135(3) Uani 1 1 d . . . O5 O 0.5708(6) 0.7253(5) 1.1387(5) 0.116(3) Uani 1 1 d . . . O8 O 0.2982(11) 0.5394(7) 1.4030(7) 0.180(5) Uani 1 1 d . . . C4A C 0.0261(12) 0.5538(7) 0.5434(7) 0.096(3) Uani 1 1 d . . . C3A C -0.0465(11) 0.5964(8) 0.5543(7) 0.112(4) Uani 1 1 d . . . H3A H -0.1127 0.5846 0.5281 0.135 Uiso 1 1 calc R . . C9' C 0.2171(9) 0.7211(6) 0.7058(7) 0.085(3) Uani 1 1 d . . . C1' C 0.1157(8) 0.7285(6) 0.6895(7) 0.083(3) Uani 1 1 d . . . C2' C 0.0781(8) 0.7829(6) 0.7270(8) 0.086(3) Uani 1 1 d . . . C3' C 0.1449(10) 0.8283(6) 0.7779(7) 0.090(3) Uani 1 1 d . . . C4' C 0.2463(9) 0.8223(5) 0.7887(6) 0.081(3) Uani 1 1 d . . . C10' C 0.2839(9) 0.7670(6) 0.7502(7) 0.085(3) Uani 1 1 d . . . C5' C 0.3898(8) 0.7674(6) 0.7625(7) 0.083(3) Uani 1 1 d . . . C6' C 0.4460(9) 0.8221(7) 0.7994(7) 0.090(3) Uani 1 1 d . . . C7' C 0.4189(9) 0.8762(6) 0.8394(7) 0.092(3) Uani 1 1 d . . . C8' C 0.3169(10) 0.8737(6) 0.8360(7) 0.096(3) Uani 1 1 d . . . C11' C 0.4446(8) 0.7242(7) 0.7268(8) 0.089(3) Uani 1 1 d . . . C12' C 0.5507(8) 0.7534(7) 0.7546(7) 0.097(3) Uani 1 1 d . . . C122 C -0.0730(9) 0.8460(8) 0.6684(7) 0.092(3) Uani 1 1 d . . . C16' C -0.1827(9) 0.8492(6) 0.6521(8) 0.090(3) Uani 1 1 d . . . H16' H -0.1821 0.8979 0.6418 0.109 Uiso 1 1 calc R . . C17' C -0.2464(12) 0.8404(8) 0.5728(9) 0.126(4) Uani 1 1 d . . . H17' H -0.3139 0.8441 0.5645 0.151 Uiso 1 1 calc R . . C18' C -0.2135(12) 0.8248(8) 0.4962(9) 0.131(5) Uani 1 1 d . . . H018' H -0.1451 0.8257 0.5079 0.157 Uiso 1 1 calc R . . C19' C -0.2621(11) 0.8107(10) 0.4190(12) 0.163(7) Uani 1 1 d . . . H19' H -0.3305 0.8137 0.4063 0.195 Uiso 1 1 calc R . . C20' C -0.2309(10) 0.7904(11) 0.3453(9) 0.138(6) Uani 1 1 d . . . H20' H -0.2813 0.8055 0.2914 0.166 Uiso 1 1 calc R . . C21' C -0.1328(9) 0.8249(8) 0.3517(8) 0.112(4) Uani 1 1 d . . . H21' H -0.0880 0.8167 0.4111 0.134 Uiso 1 1 calc R . . C22' C -0.0779(9) 0.7999(7) 0.2889(6) 0.100(3) Uani 1 1 d . . . H22' H -0.0704 0.7510 0.2963 0.121 Uiso 1 1 calc R . . C23' C 0.0237(9) 0.8287(6) 0.3080(7) 0.096(3) Uani 1 1 d . . . H23' H 0.0528 0.8085 0.2665 0.115 Uiso 1 1 calc R . . C24' C 0.0989(8) 0.8166(6) 0.4027(6) 0.087(3) Uani 1 1 d . . . H24' H 0.0723 0.8395 0.4441 0.105 Uiso 1 1 calc R . . C25' C 0.2016(8) 0.8470(6) 0.4137(6) 0.087(3) Uani 1 1 d . . . H25' H 0.1933 0.8945 0.3963 0.104 Uiso 1 1 calc R . . C26' C 0.2730(8) 0.8425(6) 0.5035(6) 0.091(3) Uani 1 1 d . . . H26' H 0.2715 0.7956 0.5222 0.109 Uiso 1 1 calc R . . C27' C 0.3806(8) 0.8572(6) 0.5094(6) 0.088(3) Uani 1 1 d . . . H27' H 0.3973 0.8305 0.4650 0.106 Uiso 1 1 calc R . . C28' C 0.4530(10) 0.8416(7) 0.5964(7) 0.105(4) Uani 1 1 d . . . H28' H 0.4532 0.8672 0.6447 0.126 Uiso 1 1 calc R . . C29' C 0.5164(10) 0.7920(7) 0.6058(8) 0.106(4) Uani 1 1 d . . . H29' H 0.5172 0.7713 0.5544 0.128 Uiso 1 1 calc R . . C14' C 0.4845(12) 0.9330(7) 0.8823(9) 0.136(5) Uani 1 1 d . . . H14D' H 0.4480 0.9641 0.9059 0.204 Uiso 1 1 calc R . . H14E' H 0.5078 0.9558 0.8402 0.204 Uiso 1 1 calc R . . H14F' H 0.5402 0.9159 0.9287 0.204 Uiso 1 1 calc R . . C7A C -0.0031(12) 0.4892(7) 0.4949(9) 0.132(5) Uani 1 1 d . . . H7A1' H -0.0741 0.4851 0.4753 0.198 Uiso 1 1 calc R . . H7A2' H 0.0257 0.4521 0.5327 0.198 Uiso 1 1 calc R . . H7A3' H 0.0202 0.4888 0.4454 0.198 Uiso 1 1 calc R . . C13' C 0.6323(9) 0.7113(7) 0.8163(8) 0.115(4) Uani 1 1 d . . . H13D' H 0.6151 0.7008 0.8676 0.173 Uiso 1 1 calc R . . H13E' H 0.6934 0.7361 0.8326 0.173 Uiso 1 1 calc R . . H13F' H 0.6401 0.6702 0.7877 0.173 Uiso 1 1 calc R . . C30' C -0.2141(11) 0.8614(7) 0.7299(8) 0.130(5) Uani 1 1 d . . . H30A' H -0.1565 0.8665 0.7806 0.196 Uiso 1 1 calc R . . H30B' H -0.2527 0.8238 0.7382 0.196 Uiso 1 1 calc R . . H30C' H -0.2534 0.9017 0.7214 0.196 Uiso 1 1 calc R . . C31' C -0.2232(11) 0.7141(11) 0.3426(10) 0.149(6) Uani 1 1 d . . . H31D' H -0.2033 0.7012 0.2934 0.223 Uiso 1 1 calc R . . H31E' H -0.2865 0.6944 0.3371 0.223 Uiso 1 1 calc R . . H31F' H -0.1749 0.6985 0.3955 0.223 Uiso 1 1 calc R . . C32' C -0.1424(10) 0.8131(8) 0.1911(7) 0.132(5) Uani 1 1 d . . . H32D' H -0.2073 0.7942 0.1805 0.198 Uiso 1 1 calc R . . H32E' H -0.1113 0.7924 0.1530 0.198 Uiso 1 1 calc R . . H32F' H -0.1481 0.8608 0.1804 0.198 Uiso 1 1 calc R . . C33' C 0.1026(9) 0.7418(6) 0.4231(7) 0.099(3) Uani 1 1 d . . . H33D' H 0.0367 0.7256 0.4153 0.149 Uiso 1 1 calc R . . H33E' H 0.1435 0.7344 0.4824 0.149 Uiso 1 1 calc R . . H33F' H 0.1299 0.7180 0.3844 0.149 Uiso 1 1 calc R . . C18 C -0.2009(8) 0.5681(7) 0.9176(8) 0.102(3) Uani 1 1 d . . . H18' H -0.1555 0.6033 0.9341 0.122 Uiso 1 1 calc R . . C35' C 0.2540(13) 0.8408(9) 0.2841(9) 0.123(5) Uani 1 1 d . . . C36' C 0.3218(12) 0.8051(9) 0.2494(10) 0.154(6) Uani 1 1 d . . . H36A' H 0.3389 0.7625 0.2788 0.232 Uiso 1 1 calc R . . H36B' H 0.3809 0.8314 0.2586 0.232 Uiso 1 1 calc R . . H36C' H 0.2908 0.7975 0.1880 0.232 Uiso 1 1 calc R . . C34' C 0.2410(9) 0.8861(7) 0.5683(7) 0.117(4) Uani 1 1 d . . . H34D' H 0.2892 0.8821 0.6254 0.176 Uiso 1 1 calc R . . H34E' H 0.1776 0.8711 0.5701 0.176 Uiso 1 1 calc R . . H34F' H 0.2363 0.9324 0.5499 0.176 Uiso 1 1 calc R . . C37' C 0.4723(13) 0.9471(9) 0.4717(12) 0.169(7) Uani 1 1 d . . . H37D' H 0.4700 0.9944 0.4583 0.254 Uiso 1 1 calc R . . H37E' H 0.4781 0.9217 0.4231 0.254 Uiso 1 1 calc R . . H37F' H 0.5285 0.9381 0.5224 0.254 Uiso 1 1 calc R . . N2' N 0.0733(8) 0.6720(5) 0.6377(5) 0.088(2) Uani 1 1 d . . . N3' N 0.2363(8) 0.6616(5) 0.6658(6) 0.096(3) Uani 1 1 d . . . N1' N -0.0254(8) 0.7916(5) 0.7077(7) 0.101(3) Uani 1 1 d . . . H1' H -0.0588 0.7601 0.7221 0.122 Uiso 1 1 calc R . . O3' O 0.5422(6) 0.8172(4) 0.7968(5) 0.101(2) Uani 1 1 d . . . O2' O 0.2831(6) 0.9204(4) 0.8754(6) 0.118(3) Uani 1 1 d . . . H2' H 0.2237 0.9143 0.8668 0.177 Uiso 1 1 calc R . . O1' O 0.1113(6) 0.8773(4) 0.8174(5) 0.105(2) Uani 1 1 d . . . O6' O 0.3835(6) 0.9280(5) 0.4887(5) 0.115(3) Uani 1 1 d . . . O4' O 0.4264(6) 0.6695(5) 0.6884(5) 0.107(2) Uani 1 1 d . . . O11' O -0.0321(7) 0.8929(6) 0.6455(6) 0.142(3) Uani 1 1 d . . . O10' O -0.1460(8) 0.8954(6) 0.3431(9) 0.170(4) Uani 1 1 d . . . H10' H -0.0927 0.9135 0.3475 0.255 Uiso 1 1 calc R . . O9' O 0.0185(6) 0.9004(5) 0.2930(5) 0.116(3) Uani 1 1 d . . . H9' H 0.0748 0.9155 0.3031 0.174 Uiso 1 1 calc R . . O7' O 0.2453(5) 0.8110(4) 0.3559(5) 0.099(2) Uani 1 1 d . . . O5' O 0.5824(6) 0.7662(5) 0.6821(5) 0.113(2) Uani 1 1 d . . . O8' O 0.2155(13) 0.8936(7) 0.2610(7) 0.189(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C9 0.090(9) 0.114(9) 0.063(6) 0.009(7) 0.021(6) -0.011(8) C1 0.103(10) 0.096(9) 0.065(7) 0.007(6) 0.015(7) -0.013(8) C2 0.099(9) 0.080(8) 0.084(7) 0.011(6) 0.036(7) -0.007(8) C3 0.106(10) 0.094(9) 0.073(7) 0.011(7) 0.030(7) 0.001(8) C4 0.074(9) 0.111(11) 0.075(7) 0.025(7) 0.009(6) -0.012(8) C10 0.062(8) 0.118(10) 0.052(6) 0.004(6) 0.007(5) -0.006(7) C5 0.096(10) 0.119(10) 0.054(7) 0.013(7) 0.009(7) 0.013(9) C6 0.082(10) 0.146(13) 0.090(9) 0.020(9) 0.017(8) 0.001(10) C7 0.144(13) 0.100(10) 0.078(8) 0.002(7) 0.031(8) 0.008(10) C8 0.091(9) 0.125(12) 0.084(8) -0.001(8) 0.023(8) -0.009(9) C20 0.115(9) 0.100(9) 0.077(7) -0.005(6) 0.041(7) -0.012(7) C22 0.113(9) 0.092(8) 0.079(7) 0.001(6) 0.037(7) 0.003(6) C2A 0.089(9) 0.120(10) 0.090(8) -0.014(8) 0.026(7) -0.018(7) C5A 0.137(13) 0.102(11) 0.080(8) 0.001(7) 0.028(8) 0.016(9) C6A 0.115(10) 0.081(9) 0.078(7) -0.005(7) 0.030(8) -0.003(9) C211 0.091(10) 0.124(11) 0.061(6) 0.006(6) 0.020(6) -0.001(8) C311 0.120(11) 0.132(12) 0.093(9) 0.008(9) 0.044(9) 0.011(11) C411 0.153(14) 0.102(11) 0.085(8) 0.017(8) 0.038(9) 0.031(11) C511 0.118(11) 0.096(10) 0.089(8) 0.005(7) 0.027(7) 0.001(8) C611 0.092(9) 0.112(11) 0.079(8) 0.022(7) 0.019(7) -0.023(10) C11 0.102(10) 0.140(12) 0.067(8) 0.009(8) 0.019(7) -0.014(9) C12 0.087(9) 0.136(11) 0.069(8) 0.007(8) -0.001(7) -0.016(8) C15 0.085(8) 0.086(8) 0.074(7) 0.003(7) 0.018(7) -0.019(7) C16 0.095(8) 0.116(9) 0.079(8) 0.017(7) 0.021(6) -0.010(7) C17 0.104(8) 0.083(8) 0.079(8) -0.010(6) 0.010(7) -0.011(6) C19 0.105(8) 0.089(8) 0.106(9) 0.002(7) 0.036(7) -0.004(6) C21 0.106(8) 0.074(8) 0.080(7) 0.015(5) 0.038(6) -0.004(6) C23 0.113(9) 0.075(8) 0.080(7) 0.004(5) 0.026(7) -0.002(6) C24 0.095(7) 0.086(8) 0.078(7) 0.003(6) 0.025(6) 0.001(6) C25 0.094(7) 0.089(7) 0.068(6) -0.005(6) 0.013(6) -0.007(6) C26 0.082(7) 0.104(8) 0.069(6) 0.001(6) -0.001(6) 0.003(6) C27 0.122(10) 0.091(9) 0.088(7) 0.029(6) 0.046(8) 0.006(7) C28 0.148(12) 0.076(9) 0.109(10) 0.003(8) 0.018(9) 0.018(9) C29 0.114(9) 0.135(13) 0.088(9) 0.007(9) 0.022(8) 0.008(9) C14 0.107(9) 0.144(12) 0.163(13) -0.025(10) 0.038(9) 0.002(9) C711 0.162(13) 0.102(10) 0.174(14) 0.003(9) 0.067(11) 0.015(9) C13 0.097(8) 0.139(11) 0.088(8) -0.001(7) 0.016(7) -0.017(8) C30 0.175(13) 0.202(16) 0.065(8) -0.011(9) 0.025(8) -0.077(12) C31 0.164(12) 0.129(12) 0.087(8) -0.019(8) 0.032(8) 0.022(9) C32 0.142(10) 0.117(10) 0.093(8) 0.014(7) 0.052(7) 0.020(8) C33 0.124(9) 0.091(9) 0.086(7) 0.001(6) 0.020(6) -0.001(7) C35 0.157(12) 0.150(13) 0.045(8) 0.010(9) 0.021(7) 0.027(11) C36 0.143(12) 0.26(2) 0.097(10) -0.038(13) 0.008(9) 0.041(13) C34 0.136(10) 0.155(12) 0.089(8) -0.018(8) 0.049(7) 0.001(9) C37 0.145(14) 0.191(18) 0.151(13) 0.052(13) 0.026(12) 0.029(12) N2 0.087(7) 0.116(8) 0.055(5) 0.018(5) 0.018(5) -0.007(7) N3 0.112(8) 0.075(7) 0.080(6) -0.002(5) 0.032(5) -0.006(5) N1 0.096(7) 0.103(7) 0.087(6) 0.017(5) 0.004(6) -0.022(6) O3 0.099(7) 0.126(7) 0.102(6) -0.010(5) 0.029(5) -0.005(5) O2 0.152(7) 0.120(7) 0.120(6) -0.031(6) 0.056(6) -0.005(6) O1 0.140(7) 0.109(7) 0.108(6) -0.009(5) 0.029(5) -0.017(5) O4 0.127(7) 0.110(6) 0.106(6) -0.019(5) 0.025(5) -0.008(5) O11 0.111(6) 0.108(7) 0.102(6) 0.018(5) 0.022(5) -0.016(5) O10 0.153(7) 0.076(5) 0.103(5) -0.006(4) 0.050(5) 0.011(5) O9 0.122(6) 0.093(6) 0.131(6) 0.033(5) 0.050(5) 0.013(5) O7 0.141(6) 0.110(6) 0.065(5) -0.007(5) 0.023(4) 0.004(5) O6 0.137(8) 0.123(8) 0.139(7) 0.038(6) 0.034(6) 0.015(6) O5 0.098(5) 0.159(7) 0.084(6) 0.017(5) 0.016(5) -0.017(5) O8 0.267(15) 0.141(10) 0.103(7) 0.034(7) 0.019(8) -0.010(10) C4A 0.115(10) 0.104(10) 0.067(7) 0.001(6) 0.026(7) 0.000(9) C3A 0.134(11) 0.126(11) 0.070(7) -0.007(8) 0.023(7) -0.032(11) C9' 0.102(10) 0.070(8) 0.080(7) -0.004(7) 0.028(7) -0.018(7) C1' 0.081(8) 0.074(8) 0.085(7) -0.001(6) 0.015(6) -0.008(7) C2' 0.076(8) 0.088(9) 0.099(8) 0.012(7) 0.033(7) 0.001(7) C3' 0.099(10) 0.087(9) 0.080(7) 0.012(7) 0.022(7) 0.005(8) C4' 0.096(9) 0.070(7) 0.067(6) -0.001(6) 0.012(6) -0.009(7) C10' 0.104(9) 0.076(8) 0.067(7) 0.006(6) 0.017(6) 0.002(8) C5' 0.084(8) 0.094(8) 0.073(7) 0.002(6) 0.028(6) 0.005(8) C6' 0.086(9) 0.085(9) 0.084(8) 0.006(7) 0.008(7) -0.002(8) C7' 0.092(9) 0.086(9) 0.083(7) 0.001(7) 0.007(6) -0.006(7) C8' 0.120(11) 0.089(9) 0.079(7) -0.007(7) 0.031(7) 0.014(8) C11' 0.077(7) 0.109(10) 0.078(7) 0.009(7) 0.020(6) 0.017(7) C12' 0.082(8) 0.123(11) 0.074(8) 0.005(7) 0.007(6) 0.010(7) C122 0.108(10) 0.098(10) 0.071(7) 0.012(7) 0.031(7) -0.013(9) C16' 0.109(9) 0.079(7) 0.079(8) 0.001(6) 0.022(7) -0.005(6) C17' 0.128(10) 0.160(13) 0.089(10) 0.008(9) 0.034(9) 0.006(9) C18' 0.134(11) 0.172(14) 0.078(9) -0.009(9) 0.023(9) 0.003(10) C19' 0.101(10) 0.25(2) 0.117(13) -0.035(13) 0.007(10) -0.013(11) C20' 0.095(9) 0.24(2) 0.082(9) -0.033(11) 0.030(7) -0.012(11) C21' 0.106(10) 0.126(12) 0.101(9) -0.019(8) 0.029(7) 0.001(8) C22' 0.114(9) 0.119(9) 0.055(6) -0.012(6) 0.009(6) 0.005(8) C23' 0.117(9) 0.086(9) 0.082(8) -0.003(6) 0.026(7) 0.018(7) C24' 0.095(8) 0.108(9) 0.047(6) -0.006(5) 0.006(5) 0.004(7) C25' 0.102(8) 0.091(7) 0.067(7) 0.000(5) 0.026(6) 0.022(6) C26' 0.108(8) 0.107(8) 0.047(6) -0.013(5) 0.011(6) 0.004(7) C27' 0.087(8) 0.096(9) 0.068(7) 0.002(6) 0.005(6) 0.010(6) C28' 0.128(10) 0.112(10) 0.058(7) 0.010(6) 0.006(7) 0.016(9) C29' 0.126(9) 0.116(10) 0.073(8) 0.017(7) 0.026(8) 0.018(9) C14' 0.177(14) 0.099(9) 0.125(10) -0.022(8) 0.037(10) -0.039(10) C7A 0.185(13) 0.095(9) 0.101(9) -0.021(8) 0.026(9) -0.041(9) C13' 0.099(8) 0.155(11) 0.085(8) 0.014(8) 0.019(7) 0.014(8) C30' 0.182(13) 0.130(11) 0.088(8) -0.017(8) 0.054(8) -0.011(10) C31' 0.117(11) 0.21(2) 0.111(11) -0.038(12) 0.027(9) -0.034(12) C32' 0.123(9) 0.186(13) 0.071(7) -0.013(8) 0.010(7) -0.002(10) C33' 0.110(8) 0.094(9) 0.079(7) 0.012(6) 0.010(6) -0.001(6) C18 0.102(8) 0.116(9) 0.086(9) 0.010(7) 0.028(7) -0.026(7) C35' 0.192(14) 0.098(11) 0.087(9) -0.004(8) 0.057(9) -0.021(10) C36' 0.173(13) 0.194(15) 0.124(11) -0.030(11) 0.087(11) -0.023(12) C34' 0.099(8) 0.175(13) 0.072(7) -0.012(8) 0.019(6) 0.009(8) C37' 0.147(14) 0.158(15) 0.192(17) 0.033(12) 0.040(12) -0.035(11) N2' 0.112(8) 0.072(6) 0.081(6) 0.002(5) 0.031(6) -0.006(7) N3' 0.143(9) 0.070(6) 0.068(5) -0.009(5) 0.026(6) -0.007(6) N1' 0.110(8) 0.087(7) 0.117(8) 0.012(6) 0.050(6) -0.002(6) O3' 0.083(6) 0.122(7) 0.085(5) 0.003(5) 0.007(4) 0.002(5) O2' 0.115(6) 0.109(6) 0.124(6) -0.035(5) 0.031(5) -0.004(5) O1' 0.136(6) 0.085(5) 0.101(5) -0.004(4) 0.051(5) 0.023(5) O6' 0.097(6) 0.124(7) 0.110(6) 0.021(5) 0.015(5) 0.002(5) O4' 0.109(6) 0.104(6) 0.107(6) -0.021(5) 0.032(4) 0.005(5) O11' 0.130(7) 0.149(8) 0.124(7) 0.052(7) 0.007(6) -0.012(6) O10' 0.154(9) 0.146(10) 0.226(12) -0.066(8) 0.085(8) -0.019(7) O9' 0.123(6) 0.120(7) 0.084(5) 0.014(5) 0.005(4) 0.006(5) O7' 0.124(6) 0.104(5) 0.074(5) 0.002(4) 0.041(4) -0.002(5) O5' 0.107(5) 0.144(7) 0.085(6) 0.016(5) 0.028(5) 0.017(5) O8' 0.349(19) 0.124(9) 0.120(8) 0.035(7) 0.112(10) 0.024(11) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C9 C1 1.411(15) . ? C9 C8 1.435(17) . ? C9 C10 1.443(15) . ? C1 O1 1.354(14) . ? C1 C2 1.381(15) . ? C2 N1 1.397(14) . ? C2 C3 1.435(15) . ? C3 C4 1.346(15) . ? C3 N2 1.411(14) . ? C4 C10 1.380(15) . ? C4 N3 1.416(14) . ? C10 C5 1.396(16) . ? C5 C6 1.362(16) . ? C5 C11 1.437(18) . ? C6 O3 1.356(14) . ? C6 C7 1.461(18) . ? C7 C8 1.366(17) . ? C7 C14 1.516(18) . ? C8 O2 1.300(15) . ? C20 C31 1.499(16) . ? C20 C21 1.528(15) . ? C20 C19 1.533(16) . ? C22 C23 1.543(15) . ? C22 C21 1.544(15) . ? C22 C32 1.544(16) . ? C2A C3A 1.368(17) . ? C2A N2' 1.379(14) . ? C5A C4A 1.345(17) . ? C5A C6A 1.388(17) . ? C6A N2' 1.347(14) . ? C6A N3' 1.364(15) . ? C211 C311 1.321(17) . ? C211 N2 1.352(14) . ? C311 C411 1.40(2) . ? C411 C511 1.365(18) . ? C411 C711 1.508(19) . ? C511 C611 1.436(18) . ? C611 N3 1.340(14) . ? C611 N2 1.371(14) . ? C11 O4 1.245(16) . ? C11 C12 1.513(17) . ? C12 O5 1.424(13) . ? C12 O3 1.428(15) . ? C12 C13 1.483(16) . ? C15 O11 1.226(12) . ? C15 N1 1.325(14) . ? C15 C16 1.466(16) . ? C16 C17 1.345(14) . ? C16 C30 1.491(15) . ? C17 C18 1.441(15) . ? C19 C18 1.303(15) . ? C21 O10 1.385(12) . ? C23 O9 1.421(12) . ? C23 C24 1.478(14) . ? C24 C33 1.515(16) . ? C24 C25 1.544(14) . ? C25 O7 1.457(12) . ? C25 C26 1.492(15) . ? C26 C27 1.483(15) . ? C26 C34 1.551(16) . ? C27 O6 1.412(13) . ? C27 C28 1.516(18) . ? C28 C29 1.284(17) . ? C29 O5 1.396(16) . ? C35 O8 1.171(16) . ? C35 O7 1.357(15) . ? C35 C36 1.50(2) . ? C37 O6 1.455(17) . ? C4A C3A 1.388(17) . ? C4A C7A 1.489(17) . ? C9' C10' 1.345(14) . ? C9' C1' 1.389(15) . ? C9' N3' 1.413(14) . ? C1' N2' 1.413(14) . ? C1' C2' 1.423(15) . ? C2' C3' 1.374(15) . ? C2' N1' 1.415(14) . ? C3' O1' 1.334(13) . ? C3' C4' 1.402(15) . ? C4' C10' 1.446(15) . ? C4' C8' 1.461(15) . ? C10' C5' 1.456(15) . ? C5' C6' 1.366(15) . ? C5' C11' 1.400(16) . ? C6' C7' 1.369(16) . ? C6' O3' 1.386(13) . ? C7' C8' 1.437(16) . ? C7' C14' 1.485(17) . ? C8' O2' 1.301(13) . ? C11' O4' 1.237(14) . ? C11' C12' 1.544(16) . ? C12' O5' 1.408(13) . ? C12' O3' 1.461(14) . ? C12' C13' 1.514(16) . ? C122 O11' 1.217(13) . ? C122 N1' 1.323(15) . ? C122 C16' 1.499(16) . ? C16' C17' 1.323(16) . ? C16' C30' 1.483(16) . ? C17' C18' 1.490(19) . ? C18' C19' 1.249(18) . ? C19' C20' 1.45(2) . ? C20' C31' 1.52(2) . ? C20' C21' 1.529(19) . ? C21' O10' 1.411(16) . ? C21' C22' 1.548(17) . ? C22' C23' 1.490(16) . ? C22' C32' 1.573(15) . ? C23' O9' 1.439(13) . ? C23' C24' 1.580(14) . ? C24' C33' 1.515(15) . ? C24' C25' 1.538(15) . ? C25' O7' 1.464(12) . ? C25' C26' 1.482(14) . ? C26' C27' 1.532(15) . ? C26' C34' 1.536(15) . ? C27' O6' 1.446(13) . ? C27' C28' 1.484(15) . ? C28' C29' 1.310(16) . ? C29' O5' 1.385(14) . ? C35' O8' 1.185(17) . ? C35' O7' 1.344(15) . ? C35' C36' 1.45(2) . ? C37' O6' 1.428(17) . ? 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 C1 C9 C8 121.5(13) . . ? C1 C9 C10 118.9(11) . . ? C8 C9 C10 119.6(11) . . ? O1 C1 C2 117.4(11) . . ? O1 C1 C9 118.1(12) . . ? C2 C1 C9 124.4(12) . . ? C1 C2 N1 118.1(11) . . ? C1 C2 C3 114.2(11) . . ? N1 C2 C3 127.3(12) . . ? C4 C3 N2 107.6(11) . . ? C4 C3 C2 122.3(13) . . ? N2 C3 C2 130.2(12) . . ? C3 C4 C10 124.4(13) . . ? C3 C4 N3 109.3(11) . . ? C10 C4 N3 126.3(11) . . ? C4 C10 C5 127.3(12) . . ? C4 C10 C9 115.7(10) . . ? C5 C10 C9 116.9(11) . . ? C6 C5 C10 122.0(13) . . ? C6 C5 C11 105.4(12) . . ? C10 C5 C11 132.1(13) . . ? O3 C6 C5 116.9(13) . . ? O3 C6 C7 120.2(14) . . ? C5 C6 C7 122.8(13) . . ? C8 C7 C6 115.2(13) . . ? C8 C7 C14 124.6(13) . . ? C6 C7 C14 120.1(14) . . ? O2 C8 C7 118.8(13) . . ? O2 C8 C9 117.8(12) . . ? C7 C8 C9 123.0(13) . . ? C31 C20 C21 114.0(10) . . ? C31 C20 C19 110.5(10) . . ? C21 C20 C19 108.3(9) . . ? C23 C22 C21 111.4(8) . . ? C23 C22 C32 111.0(9) . . ? C21 C22 C32 114.3(10) . . ? C3A C2A N2' 117.1(12) . . ? C4A C5A C6A 121.5(13) . . ? N2' C6A N3' 110.3(11) . . ? N2' C6A C5A 119.6(13) . . ? N3' C6A C5A 130.2(14) . . ? C311 C211 N2 119.9(12) . . ? C211 C311 C411 123.3(13) . . ? C511 C411 C311 119.1(12) . . ? C511 C411 C711 117.8(16) . . ? C311 C411 C711 123.1(16) . . ? C411 C511 C611 116.3(12) . . ? N3 C611 N2 111.5(13) . . ? N3 C611 C511 126.8(13) . . ? N2 C611 C511 121.7(12) . . ? O4 C11 C5 130.8(12) . . ? O4 C11 C12 123.6(13) . . ? C5 C11 C12 105.6(13) . . ? O5 C12 O3 110.1(11) . . ? O5 C12 C13 102.9(9) . . ? O3 C12 C13 111.5(10) . . ? O5 C12 C11 111.0(10) . . ? O3 C12 C11 107.0(10) . . ? C13 C12 C11 114.4(12) . . ? O11 C15 N1 120.5(10) . . ? O11 C15 C16 121.9(11) . . ? N1 C15 C16 117.5(11) . . ? C17 C16 C15 120.9(10) . . ? C17 C16 C30 122.5(11) . . ? C15 C16 C30 116.5(10) . . ? C16 C17 C18 126.5(11) . . ? C18 C19 C20 123.7(11) . . ? O10 C21 C20 108.5(9) . . ? O10 C21 C22 112.5(8) . . ? C20 C21 C22 112.4(8) . . ? O9 C23 C24 108.3(9) . . ? O9 C23 C22 108.8(9) . . ? C24 C23 C22 117.6(9) . . ? C23 C24 C33 112.8(9) . . ? C23 C24 C25 114.1(9) . . ? C33 C24 C25 110.5(9) . . ? O7 C25 C26 109.2(8) . . ? O7 C25 C24 107.0(8) . . ? C26 C25 C24 116.8(8) . . ? C27 C26 C25 113.9(8) . . ? C27 C26 C34 112.3(10) . . ? C25 C26 C34 109.5(9) . . ? O6 C27 C26 107.5(10) . . ? O6 C27 C28 109.6(10) . . ? C26 C27 C28 113.5(9) . . ? C29 C28 C27 121.9(13) . . ? C28 C29 O5 127.1(14) . . ? O8 C35 O7 124.1(14) . . ? O8 C35 C36 124.7(14) . . ? O7 C35 C36 111.2(16) . . ? C211 N2 C611 119.4(12) . . ? C211 N2 C3 134.6(12) . . ? C611 N2 C3 106.0(11) . . ? C611 N3 C4 105.6(10) . . ? C15 N1 C2 129.3(10) . . ? C6 O3 C12 105.1(10) . . ? C35 O7 C25 119.2(10) . . ? C27 O6 C37 112.9(12) . . ? C29 O5 C12 120.4(9) . . ? C5A C4A C3A 117.2(12) . . ? C5A C4A C7A 123.1(14) . . ? C3A C4A C7A 119.7(14) . . ? C2A C3A C4A 123.1(12) . . ? C10' C9' C1' 122.9(11) . . ? C10' C9' N3' 127.0(12) . . ? C1' C9' N3' 110.1(10) . . ? C9' C1' N2' 104.3(10) . . ? C9' C1' C2' 120.7(10) . . ? N2' C1' C2' 134.9(11) . . ? C3' C2' N1' 121.6(11) . . ? C3' C2' C1' 117.9(10) . . ? N1' C2' C1' 120.4(11) . . ? O1' C3' C2' 118.6(11) . . ? O1' C3' C4' 121.0(11) . . ? C2' C3' C4' 120.4(11) . . ? C3' C4' C10' 121.2(10) . . ? C3' C4' C8' 120.9(11) . . ? C10' C4' C8' 117.8(11) . . ? C9' C10' C4' 116.6(11) . . ? C9' C10' C5' 126.9(11) . . ? C4' C10' C5' 116.5(11) . . ? C6' C5' C11' 109.9(11) . . ? C6' C5' C10' 120.0(11) . . ? C11' C5' C10' 129.0(12) . . ? C5' C6' C7' 127.9(11) . . ? C5' C6' O3' 112.1(11) . . ? C7' C6' O3' 120.0(11) . . ? C6' C7' C8' 112.9(11) . . ? C6' C7' C14' 125.7(12) . . ? C8' C7' C14' 121.3(13) . . ? O2' C8' C7' 119.0(12) . . ? O2' C8' C4' 116.9(11) . . ? C7' C8' C4' 124.1(11) . . ? O4' C11' C5' 133.6(11) . . ? O4' C11' C12' 120.2(11) . . ? C5' C11' C12' 105.9(11) . . ? O5' C12' O3' 109.2(10) . . ? O5' C12' C13' 105.4(9) . . ? O3' C12' C13' 109.3(9) . . ? O5' C12' C11' 111.8(9) . . ? O3' C12' C11' 103.9(9) . . ? C13' C12' C11' 117.2(11) . . ? O11' C122 N1' 123.2(12) . . ? O11' C122 C16' 119.2(13) . . ? N1' C122 C16' 117.6(12) . . ? C17' C16' C30' 123.0(12) . . ? C17' C16' C122 121.0(11) . . ? C30' C16' C122 116.0(11) . . ? C16' C17' C18' 122.2(14) . . ? C19' C18' C17' 130.9(16) . . ? C18' C19' C20' 131.5(15) . . ? C19' C20' C31' 110.0(16) . . ? C19' C20' C21' 109.5(13) . . ? C31' C20' C21' 112.0(13) . . ? O10' C21' C20' 110.2(12) . . ? O10' C21' C22' 109.3(12) . . ? C20' C21' C22' 117.1(11) . . ? C23' C22' C21' 113.7(9) . . ? C23' C22' C32' 111.1(10) . . ? C21' C22' C32' 110.5(10) . . ? O9' C23' C22' 110.4(10) . . ? O9' C23' C24' 107.2(9) . . ? C22' C23' C24' 116.9(10) . . ? C33' C24' C25' 113.1(9) . . ? C33' C24' C23' 108.9(9) . . ? C25' C24' C23' 112.1(9) . . ? O7' C25' C26' 107.3(8) . . ? O7' C25' C24' 108.6(8) . . ? C26' C25' C24' 114.6(8) . . ? C25' C26' C27' 114.0(8) . . ? C25' C26' C34' 111.9(9) . . ? C27' C26' C34' 111.1(9) . . ? O6' C27' C28' 111.0(9) . . ? O6' C27' C26' 105.8(8) . . ? C28' C27' C26' 113.2(9) . . ? C29' C28' C27' 120.6(11) . . ? C28' C29' O5' 128.7(12) . . ? C19 C18 C17 127.9(12) . . ? O8' C35' O7' 119.9(14) . . ? O8' C35' C36' 127.6(15) . . ? O7' C35' C36' 112.1(16) . . ? C6A N2' C2A 121.4(11) . . ? C6A N2' C1' 109.7(10) . . ? C2A N2' C1' 128.9(11) . . ? C6A N3' C9' 105.6(10) . . ? C122 N1' C2' 122.8(10) . . ? C6' O3' C12' 107.8(9) . . ? C37' O6' C27' 113.2(10) . . ? C35' O7' C25' 120.9(10) . . ? C29' O5' C12' 120.0(9) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 19.83 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.377 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.058 _vrf_THETM01_ALERT_3_A ; PROBLEM: _diffrn_reflns_theta_max is greater than expected limits RESPONSE: This is due to the use of synchrotron radiation ; # Attachment '- alfa_1.5w.cif' data_monop _database_code_depnum_ccdc_archive 'CCDC 886512' #TrackingRef '- alfa_1.5w.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H54 N3 O12.50' _chemical_formula_weight 812.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.492(4) _cell_length_b 20.098(4) _cell_length_c 16.215(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.21(3) _cell_angle_gamma 90.00 _cell_volume 4402.7(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.226 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1732 _exptl_absorpt_coefficient_mu 0.090 _exptl_absorpt_correction_T_min 0.98216 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #============================================================================== # EXPERIMENTAL DATA _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15583 _diffrn_reflns_av_R_equivalents 0.1617 _diffrn_reflns_av_sigmaI/netI 0.6272 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 25.59 _reflns_number_total 10617 _reflns_number_gt 2415 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1057P)^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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0038(8) _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_number_reflns 10617 _refine_ls_number_parameters 592 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.4202 _refine_ls_R_factor_gt 0.1628 _refine_ls_wR_factor_ref 0.4158 _refine_ls_wR_factor_gt 0.2884 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.960 _refine_ls_shift/su_max 0.200 _refine_ls_shift/su_mean 0.031 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 C9 C 0.2170(10) 0.6264(7) 0.8787(11) 0.065(7) Uiso 1 1 d G . . C1 C 0.1200(12) 0.6034(6) 0.8444(10) 0.065(7) Uiso 1 1 d G . . C2 C 0.0449(8) 0.6394(8) 0.8580(10) 0.073(8) Uiso 1 1 d G . . C3 C 0.0667(9) 0.6985(7) 0.9058(11) 0.051(6) Uiso 1 1 d G . . C4 C 0.1637(11) 0.7215(6) 0.9401(10) 0.056(7) Uiso 1 1 d G . . C10 C 0.2388(8) 0.6854(8) 0.9266(10) 0.071(7) Uiso 1 1 d GD . . C5 C 0.3421(12) 0.6991(10) 0.9707(14) 0.056(7) Uiso 1 1 d D . . C6 C 0.4157(17) 0.6613(12) 0.9598(17) 0.074(8) Uiso 1 1 d D . . C7 C 0.3928(17) 0.6016(12) 0.9101(16) 0.068(7) Uiso 1 1 d . . . C8 C 0.2954(17) 0.5883(12) 0.8656(17) 0.062(7) Uiso 1 1 d . . . C20 C -0.2003(18) 0.5695(13) 1.0633(18) 0.079(8) Uiso 1 1 d . . . H20 H -0.2294 0.5399 1.0954 0.095 Uiso 1 1 calc R . . C22 C -0.0493(15) 0.5793(12) 1.1903(15) 0.056(6) Uiso 1 1 d . . . H22 H -0.0596 0.6274 1.1927 0.067 Uiso 1 1 calc R . . C2A C -0.046(2) 0.6627(13) 0.5932(18) 0.082(8) Uiso 1 1 d . . . H2A H -0.0972 0.6912 0.5919 0.099 Uiso 1 1 calc R . . C5A C 0.1048(19) 0.5774(13) 0.5740(17) 0.081(8) Uiso 1 1 d . . . H5A H 0.1532 0.5515 0.5644 0.097 Uiso 1 1 calc R . . C6A C 0.130(2) 0.6414(13) 0.6238(18) 0.074(8) Uiso 1 1 d . . . C211 C -0.0826(19) 0.7446(13) 0.9226(16) 0.072(8) Uiso 1 1 d . . . H211 H -0.1221 0.7076 0.8996 0.086 Uiso 1 1 calc R . . C311 C -0.127(2) 0.7976(14) 0.9483(19) 0.096(9) Uiso 1 1 d . . . H311 H -0.1944 0.7975 0.9397 0.115 Uiso 1 1 calc R . . C411 C -0.0647(19) 0.8518(13) 0.9886(18) 0.082(8) Uiso 1 1 d . . . C511 C 0.0409(17) 0.8509(12) 1.0052(16) 0.071(7) Uiso 1 1 d . . . H511 H 0.0851 0.8838 1.0360 0.085 Uiso 1 1 calc R . . C611 C 0.0670(17) 0.7951(12) 0.9697(16) 0.057(7) Uiso 1 1 d . . . C11 C 0.3948(18) 0.7495(13) 1.0298(17) 0.068(8) Uiso 1 1 d . . . C12 C 0.504(2) 0.7417(14) 1.058(2) 0.082(8) Uiso 1 1 d . . . C15 C -0.1325(19) 0.6331(14) 0.7700(18) 0.070(8) Uiso 1 1 d . . . C16 C -0.2256(15) 0.5904(10) 0.7461(14) 0.047(6) Uiso 1 1 d D . . C17 C -0.2581(17) 0.5638(12) 0.8072(16) 0.071(8) Uiso 1 1 d D . . H17 H -0.3152 0.5380 0.7861 0.085 Uiso 1 1 calc R . . C19 C -0.2499(19) 0.5554(13) 0.9612(18) 0.082(9) Uiso 1 1 d . . . H19 H -0.3109 0.5340 0.9411 0.098 Uiso 1 1 calc R . . C21 C -0.0950(15) 0.5615(11) 1.0973(15) 0.050(6) Uiso 1 1 d . . . H21 H -0.0662 0.5886 1.0624 0.060 Uiso 1 1 calc R . . C23 C 0.0647(14) 0.5695(10) 1.2265(15) 0.048(6) Uiso 1 1 d . . . H23 H 0.0905 0.5875 1.2868 0.058 Uiso 1 1 calc R . . C24 C 0.1278(16) 0.5968(11) 1.1782(16) 0.065(7) Uiso 1 1 d . . . H24 H 0.1093 0.5735 1.1214 0.078 Uiso 1 1 calc R . . C25 C 0.2391(17) 0.5870(13) 1.2270(18) 0.070(7) Uiso 1 1 d . . . H25 H 0.2487 0.5402 1.2450 0.084 Uiso 1 1 calc R . . C26 C 0.2967(19) 0.5985(13) 1.1727(18) 0.081(8) Uiso 1 1 d . . . H26 H 0.2758 0.6427 1.1473 0.098 Uiso 1 1 calc R . . C27 C 0.4053(19) 0.6076(13) 1.2312(19) 0.087(9) Uiso 1 1 d . . . H27 H 0.4126 0.6382 1.2803 0.104 Uiso 1 1 calc R . . C28 C 0.4664(18) 0.6306(13) 1.1770(18) 0.091(9) Uiso 1 1 d . . . H28 H 0.4794 0.6036 1.1359 0.109 Uiso 1 1 calc R . . C29 C 0.5009(13) 0.6962(9) 1.1950(13) 0.086(9) Uiso 1 1 d . . . H29 H 0.4872 0.7204 1.2381 0.103 Uiso 1 1 calc R . . C14 C 0.4842(13) 0.5607(9) 0.9118(13) 0.107(10) Uiso 1 1 d . . . H14A H 0.5436 0.5826 0.9488 0.160 Uiso 1 1 calc R . . H14B H 0.4844 0.5571 0.8528 0.160 Uiso 1 1 calc R . . H14C H 0.4813 0.5170 0.9347 0.160 Uiso 1 1 calc R . . C711 C -0.108(2) 0.9160(15) 1.004(2) 0.117(11) Uiso 1 1 d . . . H71A H -0.0558 0.9467 1.0332 0.175 Uiso 1 1 calc R . . H71B H -0.1470 0.9082 1.0396 0.175 Uiso 1 1 calc R . . H71C H -0.1493 0.9344 0.9478 0.175 Uiso 1 1 calc R . . C13 C 0.5619(17) 0.7968(12) 1.0343(17) 0.085(8) Uiso 1 1 d . . . H13A H 0.5574 0.8370 1.0648 0.127 Uiso 1 1 calc R . . H13B H 0.5347 0.8044 0.9716 0.127 Uiso 1 1 calc R . . H13C H 0.6300 0.7839 1.0513 0.127 Uiso 1 1 calc R . . C30 C -0.281(2) 0.5822(15) 0.648(2) 0.125(12) Uiso 1 1 d . . . H30A H -0.2465 0.6058 0.6161 0.188 Uiso 1 1 calc R . . H30B H -0.3465 0.5997 0.6323 0.188 Uiso 1 1 calc R . . H30C H -0.2841 0.5358 0.6328 0.188 Uiso 1 1 calc R . . C31 C -0.2347(16) 0.6426(10) 1.0690(16) 0.068(7) Uiso 1 1 d . . . H31A H -0.3057 0.6446 1.0454 0.102 Uiso 1 1 calc R . . H31B H -0.2087 0.6714 1.0354 0.102 Uiso 1 1 calc R . . H31C H -0.2108 0.6567 1.1297 0.102 Uiso 1 1 calc R . . C32 C -0.095(2) 0.5491(13) 1.2510(19) 0.100(10) Uiso 1 1 d . . . H32A H -0.0588 0.5630 1.3106 0.150 Uiso 1 1 calc R . . H32B H -0.0927 0.5014 1.2475 0.150 Uiso 1 1 calc R . . H32C H -0.1625 0.5633 1.2338 0.150 Uiso 1 1 calc R . . C33 C 0.0989(18) 0.6701(13) 1.1587(17) 0.088(9) Uiso 1 1 d . . . H33A H 0.1367 0.6895 1.1270 0.132 Uiso 1 1 calc R . . H33B H 0.1122 0.6936 1.2134 0.132 Uiso 1 1 calc R . . H33C H 0.0296 0.6732 1.1237 0.132 Uiso 1 1 calc R . . C35 C 0.301(3) 0.597(2) 1.380(3) 0.124(13) Uiso 1 1 d . . . C36 C 0.349(2) 0.6433(16) 1.460(2) 0.137(13) Uiso 1 1 d . . . H36A H 0.3529 0.6877 1.4399 0.206 Uiso 1 1 calc R . . H36B H 0.4138 0.6276 1.4946 0.206 Uiso 1 1 calc R . . H36C H 0.3086 0.6435 1.4961 0.206 Uiso 1 1 calc R . . C34 C 0.2830(17) 0.5546(12) 1.0932(17) 0.082(8) Uiso 1 1 d . . . H34A H 0.3264 0.5692 1.0640 0.122 Uiso 1 1 calc R . . H34B H 0.2156 0.5573 1.0530 0.122 Uiso 1 1 calc R . . H34C H 0.2983 0.5093 1.1123 0.122 Uiso 1 1 calc R . . C37 C 0.539(3) 0.5416(18) 1.326(2) 0.150(15) Uiso 1 1 d . . . H37A H 0.5611 0.4969 1.3430 0.225 Uiso 1 1 calc R . . H37B H 0.5399 0.5661 1.3772 0.225 Uiso 1 1 calc R . . H37C H 0.5825 0.5627 1.3011 0.225 Uiso 1 1 calc R . . N2 N 0.0090(13) 0.7412(9) 0.9273(12) 0.062(6) Uani 1 1 d . . . N3 N 0.1603(15) 0.7783(9) 0.9777(12) 0.074(6) Uani 1 1 d . . . H3 H 0.2115 0.8023 1.0044 0.089 Uiso 1 1 calc R . . N1 N -0.0517(10) 0.6062(8) 0.8260(12) 0.050(5) Uani 1 1 d . . . H1 H -0.0556 0.5667 0.8450 0.060 Uiso 1 1 calc R . . O3 O 0.5136(10) 0.6826(10) 1.0136(12) 0.088(6) Uani 1 1 d . . . O2 O 0.2735(13) 0.5347(9) 0.8178(13) 0.096(6) Uani 1 1 d . . . O1 O 0.0957(12) 0.5491(9) 0.7925(13) 0.091(6) Uani 1 1 d . . . H1A H 0.1422 0.5387 0.7777 0.137 Uiso 1 1 calc R . . O4 O 0.3689(10) 0.8012(9) 1.0581(11) 0.082(5) Uani 1 1 d . . . O11 O -0.1401(10) 0.6901(8) 0.7380(10) 0.066(5) Uani 1 1 d . . . O10 O -0.0782(12) 0.4932(8) 1.0858(13) 0.082(5) Uani 1 1 d . . . H10 H -0.0186 0.4866 1.1001 0.122 Uiso 1 1 calc R . . O9 O 0.0827(15) 0.4961(8) 1.2329(13) 0.086(6) Uani 1 1 d . . . H9 H 0.1070 0.4848 1.1966 0.129 Uiso 1 1 calc R . . O7 O 0.2667(13) 0.6243(9) 1.3040(12) 0.085(6) Uani 1 1 d . . . O6 O 0.4436(14) 0.5405(10) 1.2639(14) 0.113(7) Uani 1 1 d . . . O5 O 0.5556(11) 0.7259(10) 1.1491(12) 0.096(7) Uani 1 1 d . . . O8 O 0.296(2) 0.5356(14) 1.3900(13) 0.173(12) Uani 1 1 d . . . C4A C 0.011(2) 0.5591(13) 0.5443(17) 0.078(8) Uiso 1 1 d . . . C3A C -0.0603(18) 0.5986(12) 0.5514(16) 0.072(8) Uiso 1 1 d . . . H3A H -0.1250 0.5830 0.5270 0.086 Uiso 1 1 calc R . . C9' C 0.2054(8) 0.7266(5) 0.7022(8) 0.062(7) Uiso 1 1 d G . . C1' C 0.1058(8) 0.7319(6) 0.6906(8) 0.057(7) Uiso 1 1 d G . . C2' C 0.0724(6) 0.7864(6) 0.7246(9) 0.059(7) Uiso 1 1 d G . . C3' C 0.1386(7) 0.8356(6) 0.7703(9) 0.063(7) Uiso 1 1 d G . . C4' C 0.2382(7) 0.8303(4) 0.7820(6) 0.084(9) Uiso 1 1 d G . . C10' C 0.2716(6) 0.7757(4) 0.7479(6) 0.060(7) Uiso 1 1 d G . . C5' C 0.3712(7) 0.7704(6) 0.7596(9) 0.056(7) Uiso 1 1 d G . . C6' C 0.4374(7) 0.8196(7) 0.8053(9) 0.060(7) Uiso 1 1 d G . . C7' C 0.4040(8) 0.8741(6) 0.8393(8) 0.069(7) Uiso 1 1 d G . . C8' C 0.3044(9) 0.8794(5) 0.8277(8) 0.060(7) Uiso 1 1 d G . . C11' C 0.4301(16) 0.7232(12) 0.7302(15) 0.052(6) Uiso 1 1 d . . . C12' C 0.5385(17) 0.7539(12) 0.7693(17) 0.062(7) Uiso 1 1 d . . . C122 C -0.0917(19) 0.8538(14) 0.6649(17) 0.064(7) Uiso 1 1 d . . . C16' C -0.1994(17) 0.8489(12) 0.6424(17) 0.069(7) Uiso 1 1 d D . . C17' C -0.2555(18) 0.8254(11) 0.5607(16) 0.069(7) Uiso 1 1 d D . . H17' H -0.3217 0.8159 0.5494 0.083 Uiso 1 1 calc R . . C18' C -0.2187(19) 0.8147(12) 0.4929(18) 0.079(8) Uiso 1 1 d . . . H18' H -0.1509 0.8198 0.5079 0.095 Uiso 1 1 calc R . . C19' C -0.2707(17) 0.7979(11) 0.4090(16) 0.062(7) Uiso 1 1 d . . . H19' H -0.3389 0.7980 0.3942 0.074 Uiso 1 1 calc R . . C20' C -0.2379(16) 0.7792(10) 0.3358(16) 0.060(7) Uiso 1 1 d . . . H20' H -0.2859 0.7950 0.2794 0.072 Uiso 1 1 calc R . . C21' C -0.1348(18) 0.8135(13) 0.3541(18) 0.077(8) Uiso 1 1 d . . . H21' H -0.0915 0.7995 0.4133 0.092 Uiso 1 1 calc R . . C22' C -0.0795(18) 0.7966(13) 0.2905(18) 0.080(8) Uiso 1 1 d . . . H22' H -0.0680 0.7484 0.2937 0.096 Uiso 1 1 calc R . . C23' C 0.0185(16) 0.8300(11) 0.3073(16) 0.063(7) Uiso 1 1 d . . . H23' H 0.0464 0.8146 0.2638 0.076 Uiso 1 1 calc R . . C24' C 0.0905(14) 0.8121(10) 0.4025(15) 0.050(6) Uiso 1 1 d . . . H24' H 0.0655 0.8313 0.4459 0.060 Uiso 1 1 calc R . . C25' C 0.1895(17) 0.8427(12) 0.4141(17) 0.069(7) Uiso 1 1 d . . . H25' H 0.1802 0.8895 0.3959 0.083 Uiso 1 1 calc R . . C26' C 0.2697(15) 0.8375(11) 0.5076(15) 0.057(7) Uiso 1 1 d . . . H26' H 0.2688 0.7924 0.5304 0.068 Uiso 1 1 calc R . . C27' C 0.3758(17) 0.8538(13) 0.5129(17) 0.074(8) Uiso 1 1 d . . . H27' H 0.3898 0.8286 0.4671 0.089 Uiso 1 1 calc R . . C28' C 0.4557(16) 0.8344(12) 0.6071(17) 0.069(7) Uiso 1 1 d . . . H28' H 0.4619 0.8622 0.6546 0.082 Uiso 1 1 calc R . . C29' C 0.5102(18) 0.7847(13) 0.6213(19) 0.081(8) Uiso 1 1 d . . . H29' H 0.5074 0.7619 0.5706 0.097 Uiso 1 1 calc R . . C14' C 0.4732(16) 0.9345(11) 0.8838(16) 0.070(8) Uiso 1 1 d . . . H14A' H 0.4371 0.9660 0.9049 0.104 Uiso 1 1 calc R . . H14B' H 0.4953 0.9555 0.8411 0.104 Uiso 1 1 calc R . . H14C' H 0.5294 0.9188 0.9325 0.104 Uiso 1 1 calc R . . C7A C -0.0176(14) 0.4988(10) 0.4965(14) 0.046(6) Uiso 1 1 d . . . H7A1' H 0.0399 0.4770 0.4932 0.069 Uiso 1 1 calc R . . H7A2' H -0.0630 0.5082 0.4378 0.069 Uiso 1 1 calc R . . H7A3' H -0.0490 0.4703 0.5261 0.069 Uiso 1 1 calc R . . C13' C 0.6116(15) 0.7094(10) 0.8370(15) 0.060(7) Uiso 1 1 d . . . H13D' H 0.6138 0.6669 0.8109 0.090 Uiso 1 1 calc R . . H13E' H 0.5914 0.7038 0.8868 0.090 Uiso 1 1 calc R . . H13F' H 0.6761 0.7294 0.8562 0.090 Uiso 1 1 calc R . . C30' C -0.2277(17) 0.8615(12) 0.7216(17) 0.084(9) Uiso 1 1 d . . . H30D' H -0.1705 0.8755 0.7705 0.126 Uiso 1 1 calc R . . H30E' H -0.2534 0.8213 0.7371 0.126 Uiso 1 1 calc R . . H30F' H -0.2774 0.8956 0.7078 0.126 Uiso 1 1 calc R . . C31' C -0.225(2) 0.7037(13) 0.3321(19) 0.100(10) Uiso 1 1 d . . . H31D' H -0.2046 0.6930 0.2834 0.149 Uiso 1 1 calc R . . H31E' H -0.2862 0.6819 0.3244 0.149 Uiso 1 1 calc R . . H31F' H -0.1749 0.6890 0.3863 0.149 Uiso 1 1 calc R . . C32' C -0.1449(16) 0.8140(12) 0.1910(16) 0.076(8) Uiso 1 1 d . . . H32D' H -0.2086 0.7932 0.1756 0.114 Uiso 1 1 calc R . . H32E' H -0.1126 0.7979 0.1526 0.114 Uiso 1 1 calc R . . H32F' H -0.1530 0.8613 0.1846 0.114 Uiso 1 1 calc R . . C33' C 0.105(2) 0.7362(14) 0.4186(19) 0.108(10) Uiso 1 1 d . . . H33D' H 0.0432 0.7161 0.4136 0.162 Uiso 1 1 calc R . . H33E' H 0.1528 0.7284 0.4769 0.162 Uiso 1 1 calc R . . H33F' H 0.1284 0.7171 0.3755 0.162 Uiso 1 1 calc R . . C18 C -0.2120(18) 0.5715(12) 0.9044(17) 0.073(8) Uiso 1 1 d . . . H018' H -0.1489 0.5900 0.9261 0.088 Uiso 1 1 calc R . . C35' C 0.2583(18) 0.8402(14) 0.2999(19) 0.066(8) Uiso 1 1 d . . . C36' C 0.3071(19) 0.7965(14) 0.2552(19) 0.103(10) Uiso 1 1 d . . . H36D' H 0.3151 0.7529 0.2810 0.155 Uiso 1 1 calc R . . H36E' H 0.3709 0.8145 0.2621 0.155 Uiso 1 1 calc R . . H36F' H 0.2672 0.7937 0.1935 0.155 Uiso 1 1 calc R . . C34' C 0.2459(17) 0.8875(13) 0.5685(17) 0.089(9) Uiso 1 1 d . . . H34D' H 0.1802 0.8795 0.5676 0.133 Uiso 1 1 calc R . . H34E' H 0.2499 0.9319 0.5483 0.133 Uiso 1 1 calc R . . H34F' H 0.2926 0.8824 0.6278 0.133 Uiso 1 1 calc R . . C37' C 0.475(2) 0.9366(14) 0.475(2) 0.108(11) Uiso 1 1 d . . . H37D' H 0.4789 0.9833 0.4642 0.162 Uiso 1 1 calc R . . H37E' H 0.4735 0.9118 0.4240 0.162 Uiso 1 1 calc R . . H37F' H 0.5326 0.9237 0.5250 0.162 Uiso 1 1 calc R . . N2' N 0.0543(12) 0.6765(9) 0.6360(10) 0.052(5) Uani 1 1 d . . . N3' N 0.2174(12) 0.6678(8) 0.6676(10) 0.045(5) Uani 1 1 d . . . H3' H 0.2734 0.6502 0.6731 0.054 Uiso 1 1 calc R . . N1' N -0.0374(12) 0.7977(9) 0.6981(12) 0.062(6) Uani 1 1 d . . . H1' H -0.0707 0.7640 0.7047 0.074 Uiso 1 1 calc R . . O3' O 0.5334(9) 0.8158(7) 0.8051(9) 0.049(4) Uani 1 1 d . . . O2' O 0.2783(11) 0.9257(8) 0.8720(13) 0.095(7) Uani 1 1 d . . . O1' O 0.1063(10) 0.8808(8) 0.8131(11) 0.069(5) Uani 1 1 d . . . H1'1 H 0.1533 0.8963 0.8540 0.103 Uiso 1 1 calc R . . O6' O 0.3790(13) 0.9218(9) 0.4956(14) 0.106(7) Uani 1 1 d . . . O4' O 0.4070(11) 0.6707(7) 0.6928(10) 0.070(5) Uani 1 1 d . . . O11' O -0.0485(10) 0.9004(8) 0.6452(10) 0.063(5) Uani 1 1 d . . . O10' O -0.1455(14) 0.8867(9) 0.3577(15) 0.094(6) Uani 1 1 d . . . H10' H -0.1185 0.9047 0.3269 0.141 Uiso 1 1 calc R . . O9' O 0.0078(12) 0.9003(9) 0.3021(12) 0.090(6) Uani 1 1 d . . . H9' H -0.0396 0.9102 0.2576 0.135 Uiso 1 1 calc R . . O7' O 0.2349(11) 0.8065(7) 0.3587(10) 0.067(5) Uani 1 1 d . . . O5' O 0.5702(10) 0.7591(8) 0.6942(10) 0.065(5) Uani 1 1 d . . . O8' O 0.2400(16) 0.8974(12) 0.2823(15) 0.142(9) Uani 1 1 d . . . O1W O -0.0725(13) 0.4670(9) 0.8172(14) 0.106(7) Uani 1 1 d . . . O2W O 0.3253(19) 0.4320(11) 0.740(3) 0.242(18) Uani 1 1 d . . . O3W O 0.292(3) 0.4858(17) 1.558(2) 0.247(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N3 0.098(17) 0.058(13) 0.049(16) 0.011(11) 0.006(13) 0.014(12) N1 0.022(10) 0.056(12) 0.063(14) 0.019(10) 0.005(10) -0.002(9) O3 0.036(9) 0.123(16) 0.088(15) -0.006(12) 0.003(10) -0.002(10) O2 0.100(14) 0.079(13) 0.120(18) -0.035(12) 0.055(13) -0.030(11) O1 0.093(14) 0.119(16) 0.064(14) -0.019(12) 0.031(12) 0.001(13) O4 0.048(10) 0.097(14) 0.077(14) 0.005(11) -0.005(9) -0.008(10) O11 0.053(10) 0.074(12) 0.064(13) 0.013(10) 0.014(9) -0.006(9) O10 0.093(13) 0.066(12) 0.088(16) -0.021(11) 0.035(13) -0.006(10) O9 0.104(15) 0.059(11) 0.115(18) 0.030(12) 0.065(13) 0.016(10) O7 0.116(15) 0.098(14) 0.046(14) 0.026(11) 0.034(11) 0.056(12) O6 0.083(14) 0.106(15) 0.14(2) 0.059(14) 0.027(14) -0.003(12) O5 0.052(11) 0.156(18) 0.061(15) 0.031(12) -0.004(10) -0.032(11) O8 0.32(4) 0.15(2) 0.051(17) 0.032(15) 0.08(2) 0.05(2) N2' 0.057(13) 0.083(14) 0.013(12) -0.010(10) 0.009(9) -0.028(12) N3' 0.038(10) 0.047(10) 0.027(12) -0.008(9) -0.016(9) 0.008(9) N1' 0.053(12) 0.059(13) 0.077(16) -0.003(11) 0.027(11) -0.015(11) O3' 0.033(8) 0.064(10) 0.032(10) -0.019(8) -0.011(7) -0.008(7) O2' 0.075(12) 0.059(11) 0.16(2) -0.030(11) 0.059(13) -0.008(9) O1' 0.050(10) 0.081(12) 0.064(14) -0.008(10) 0.006(9) -0.012(9) O6' 0.090(14) 0.080(14) 0.16(2) 0.017(13) 0.055(14) 0.028(11) O4' 0.086(12) 0.053(10) 0.070(13) -0.023(10) 0.028(10) -0.015(10) O11' 0.027(8) 0.089(12) 0.051(12) -0.001(9) -0.013(8) 0.020(9) O10' 0.110(15) 0.079(13) 0.110(18) -0.023(12) 0.060(13) -0.023(11) O9' 0.072(12) 0.107(15) 0.053(14) 0.023(11) -0.023(9) 0.000(11) O7' 0.087(12) 0.060(10) 0.071(13) 0.025(10) 0.049(10) 0.007(10) O5' 0.053(10) 0.085(12) 0.038(12) 0.036(9) -0.006(9) 0.030(8) O8' 0.18(2) 0.117(18) 0.16(2) 0.082(17) 0.107(19) 0.039(17) O1W 0.103(15) 0.095(15) 0.13(2) 0.005(12) 0.062(14) -0.009(12) O2W 0.15(2) 0.099(18) 0.45(6) -0.10(3) 0.09(3) 0.001(17) O3W 0.33(4) 0.26(3) 0.19(3) 0.10(3) 0.13(3) 0.11(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C9 C1 1.3900 . ? C9 C10 1.3900 . ? C9 C8 1.45(2) . ? C1 O1 1.345(19) . ? C1 C2 1.3900 . ? C2 C3 1.3900 . ? C2 N1 1.466(17) . ? C3 N2 1.33(2) . ? C3 C4 1.3900 . ? C4 N3 1.30(2) . ? C4 C10 1.3900 . ? C10 C5 1.433(16) . ? C5 C6 1.371(17) . ? C5 C11 1.41(3) . ? C6 C7 1.42(3) . ? C6 O3 1.44(3) . ? C7 C8 1.36(3) . ? C7 C14 1.55(3) . ? C8 O2 1.30(3) . ? C20 C21 1.43(3) . ? C20 C31 1.57(3) . ? C20 C19 1.57(3) . ? C22 C21 1.46(3) . ? C22 C32 1.50(3) . ? C22 C23 1.55(3) . ? C2A N2' 1.40(3) . ? C2A C3A 1.43(3) . ? C5A C4A 1.32(3) . ? C5A C6A 1.49(3) . ? C6A N3' 1.32(3) . ? C6A N2' 1.37(3) . ? C211 N2 1.30(3) . ? C211 C311 1.39(3) . ? C311 C411 1.42(3) . ? C411 C511 1.45(3) . ? C411 C711 1.49(3) . ? C511 C611 1.37(3) . ? C611 N3 1.35(3) . ? C611 N2 1.39(2) . ? C11 O4 1.25(3) . ? C11 C12 1.49(3) . ? C12 O5 1.42(3) . ? C12 O3 1.42(3) . ? C12 C13 1.52(3) . ? C15 O11 1.25(3) . ? C15 N1 1.31(3) . ? C15 C16 1.53(3) . ? C16 C17 1.352(15) . ? C16 C30 1.51(3) . ? C17 C18 1.48(3) . ? C19 C18 1.27(3) . ? C21 O10 1.42(2) . ? C23 O9 1.50(2) . ? C23 C24 1.51(3) . ? C24 C25 1.53(3) . ? C24 C33 1.53(3) . ? C25 O7 1.39(3) . ? C25 C26 1.43(3) . ? C26 C34 1.51(3) . ? C26 C27 1.53(3) . ? C27 O6 1.48(3) . ? C27 C28 1.53(3) . ? C28 C29 1.40(3) . ? C29 O5 1.40(2) . ? C35 O8 1.25(4) . ? C35 O7 1.27(4) . ? C35 C36 1.55(4) . ? C37 O6 1.39(3) . ? C4A C3A 1.34(3) . ? C4A C7A 1.42(3) . ? C9' N3' 1.347(17) . ? C9' C1' 1.3900 . ? C9' C10' 1.3900 . ? C1' C2' 1.3900 . ? C1' N2' 1.450(18) . ? C2' C3' 1.3900 . ? C2' N1' 1.508(18) . ? C3' O1' 1.328(16) . ? C3' C4' 1.3900 . ? C4' C10' 1.3900 . ? C4' C8' 1.3900 . ? C10' C5' 1.3900 . ? C5' C6' 1.3900 . ? C5' C11' 1.47(2) . ? C6' C7' 1.3900 . ? C6' O3' 1.395(15) . ? C7' C8' 1.3900 . ? C7' C14' 1.57(2) . ? C8' O2' 1.312(17) . ? C11' O4' 1.20(2) . ? C11' C12' 1.59(3) . ? C12' O3' 1.39(3) . ? C12' O5' 1.45(3) . ? C12' C13' 1.51(3) . ? C122 O11' 1.23(3) . ? C122 N1' 1.37(3) . ? C122 C16' 1.47(3) . ? C16' C17' 1.364(16) . ? C16' C30' 1.50(3) . ? C17' C18' 1.40(3) . ? C18' C19' 1.34(3) . ? C19' C20' 1.48(3) . ? C20' C31' 1.53(3) . ? C20' C21' 1.57(3) . ? C21' O10' 1.48(3) . ? C21' C22' 1.56(3) . ? C22' C23' 1.50(3) . ? C22' C32' 1.59(3) . ? C23' O9' 1.42(2) . ? C23' C24' 1.56(3) . ? C24' C25' 1.51(3) . ? C24' C33' 1.55(3) . ? C25' O7' 1.48(3) . ? C25' C26' 1.54(3) . ? C26' C34' 1.53(3) . ? C26' C27' 1.54(3) . ? C27' O6' 1.40(3) . ? C27' C28' 1.59(3) . ? C28' C29' 1.24(3) . ? C29' O5' 1.29(3) . ? C35' O8' 1.19(3) . ? C35' O7' 1.31(3) . ? C35' C36' 1.47(3) . ? C37' O6' 1.58(3) . ? 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 C1 C9 C10 120.0 . . ? C1 C9 C8 119.9(15) . . ? C10 C9 C8 120.1(15) . . ? O1 C1 C9 121.2(14) . . ? O1 C1 C2 118.6(14) . . ? C9 C1 C2 120.0 . . ? C3 C2 C1 120.0 . . ? C3 C2 N1 125.6(13) . . ? C1 C2 N1 114.1(13) . . ? N2 C3 C2 131.3(13) . . ? N2 C3 C4 108.7(13) . . ? C2 C3 C4 120.0 . . ? N3 C4 C10 133.9(14) . . ? N3 C4 C3 106.0(14) . . ? C10 C4 C3 120.0 . . ? C4 C10 C9 120.0 . . ? C4 C10 C5 123.9(14) . . ? C9 C10 C5 115.3(14) . . ? C6 C5 C11 103.3(19) . . ? C6 C5 C10 123(2) . . ? C11 C5 C10 133(2) . . ? C5 C6 C7 121(2) . . ? C5 C6 O3 114(2) . . ? C7 C6 O3 125(2) . . ? C8 C7 C6 117(2) . . ? C8 C7 C14 128(2) . . ? C6 C7 C14 115(2) . . ? O2 C8 C7 118(2) . . ? O2 C8 C9 119(2) . . ? C7 C8 C9 123(2) . . ? C21 C20 C31 114(2) . . ? C21 C20 C19 114(2) . . ? C31 C20 C19 101(2) . . ? C21 C22 C32 116(2) . . ? C21 C22 C23 112.5(19) . . ? C32 C22 C23 111.2(19) . . ? N2' C2A C3A 111(2) . . ? C4A C5A C6A 117(3) . . ? N3' C6A N2' 112(2) . . ? N3' C6A C5A 129(2) . . ? N2' C6A C5A 118(2) . . ? N2 C211 C311 127(3) . . ? C211 C311 C411 116(3) . . ? C311 C411 C511 122(3) . . ? C311 C411 C711 120(2) . . ? C511 C411 C711 117(2) . . ? C611 C511 C411 111(2) . . ? N3 C611 C511 125(2) . . ? N3 C611 N2 105(2) . . ? C511 C611 N2 129(2) . . ? O4 C11 C5 133(2) . . ? O4 C11 C12 114(2) . . ? C5 C11 C12 113(2) . . ? O5 C12 O3 103(2) . . ? O5 C12 C11 116(2) . . ? O3 C12 C11 103(2) . . ? O5 C12 C13 107(2) . . ? O3 C12 C13 108(2) . . ? C11 C12 C13 118(2) . . ? O11 C15 N1 126(2) . . ? O11 C15 C16 118(2) . . ? N1 C15 C16 115(2) . . ? C17 C16 C30 123(2) . . ? C17 C16 C15 123(2) . . ? C30 C16 C15 114(2) . . ? C16 C17 C18 127(2) . . ? C18 C19 C20 124(3) . . ? O10 C21 C20 105.5(19) . . ? O10 C21 C22 109.8(19) . . ? C20 C21 C22 113(2) . . ? O9 C23 C24 105.7(16) . . ? O9 C23 C22 106.6(17) . . ? C24 C23 C22 121.4(19) . . ? C23 C24 C25 114(2) . . ? C23 C24 C33 106.5(18) . . ? C25 C24 C33 113(2) . . ? O7 C25 C26 115(2) . . ? O7 C25 C24 108(2) . . ? C26 C25 C24 114(2) . . ? C25 C26 C34 120(2) . . ? C25 C26 C27 110(2) . . ? C34 C26 C27 113(2) . . ? O6 C27 C26 106(2) . . ? O6 C27 C28 105(2) . . ? C26 C27 C28 111(2) . . ? C29 C28 C27 114(2) . . ? O5 C29 C28 121(2) . . ? O8 C35 O7 122(4) . . ? O8 C35 C36 121(4) . . ? O7 C35 C36 117(4) . . ? C211 N2 C3 137.8(19) . . ? C211 N2 C611 114(2) . . ? C3 N2 C611 108.0(17) . . ? C4 N3 C611 112(2) . . ? C15 N1 C2 123.8(19) . . ? C12 O3 C6 107.5(18) . . ? C35 O7 C25 121(3) . . ? C37 O6 C27 113(2) . . ? C29 O5 C12 117.3(17) . . ? C5A C4A C3A 122(3) . . ? C5A C4A C7A 120(2) . . ? C3A C4A C7A 118(2) . . ? C4A C3A C2A 126(2) . . ? N3' C9' C1' 107.2(9) . . ? N3' C9' C10' 132.7(9) . . ? C1' C9' C10' 120.0 . . ? C2' C1' C9' 120.0 . . ? C2' C1' N2' 132.2(10) . . ? C9' C1' N2' 107.7(10) . . ? C1' C2' C3' 120.0 . . ? C1' C2' N1' 119.2(10) . . ? C3' C2' N1' 119.9(10) . . ? O1' C3' C4' 121.8(9) . . ? O1' C3' C2' 117.3(9) . . ? C4' C3' C2' 120.0 . . ? C3' C4' C10' 120.0 . . ? C3' C4' C8' 120.0 . . ? C10' C4' C8' 120.0 . . ? C5' C10' C4' 120.0 . . ? C5' C10' C9' 120.0 . . ? C4' C10' C9' 120.0 . . ? C10' C5' C6' 120.0 . . ? C10' C5' C11' 134.8(11) . . ? C6' C5' C11' 105.2(11) . . ? C7' C6' C5' 120.0 . . ? C7' C6' O3' 122.3(9) . . ? C5' C6' O3' 117.2(9) . . ? C6' C7' C8' 120.0 . . ? C6' C7' C14' 122.3(11) . . ? C8' C7' C14' 117.5(11) . . ? O2' C8' C7' 118.1(10) . . ? O2' C8' C4' 121.0(10) . . ? C7' C8' C4' 120.0 . . ? O4' C11' C5' 130(2) . . ? O4' C11' C12' 127(2) . . ? C5' C11' C12' 103.2(17) . . ? O3' C12' O5' 111.6(19) . . ? O3' C12' C13' 111(2) . . ? O5' C12' C13' 107.4(18) . . ? O3' C12' C11' 108.7(18) . . ? O5' C12' C11' 105.1(18) . . ? C13' C12' C11' 113.1(19) . . ? O11' C122 N1' 117(2) . . ? O11' C122 C16' 125(2) . . ? N1' C122 C16' 117(2) . . ? C17' C16' C122 118(2) . . ? C17' C16' C30' 130(2) . . ? C122 C16' C30' 112(2) . . ? C16' C17' C18' 124(3) . . ? C19' C18' C17' 127(3) . . ? C18' C19' C20' 131(2) . . ? C19' C20' C31' 111(2) . . ? C19' C20' C21' 107(2) . . ? C31' C20' C21' 108.6(19) . . ? O10' C21' C22' 109(2) . . ? O10' C21' C20' 109.7(19) . . ? C22' C21' C20' 117(2) . . ? C23' C22' C21' 117(2) . . ? C23' C22' C32' 105(2) . . ? C21' C22' C32' 111(2) . . ? O9' C23' C22' 111(2) . . ? O9' C23' C24' 107.9(18) . . ? C22' C23' C24' 109.0(19) . . ? C25' C24' C33' 108.3(19) . . ? C25' C24' C23' 107.0(18) . . ? C33' C24' C23' 113(2) . . ? O7' C25' C24' 109.6(18) . . ? O7' C25' C26' 102.7(18) . . ? C24' C25' C26' 116(2) . . ? C34' C26' C27' 106.0(19) . . ? C34' C26' C25' 108.8(19) . . ? C27' C26' C25' 114.9(19) . . ? O6' C27' C26' 108(2) . . ? O6' C27' C28' 112(2) . . ? C26' C27' C28' 111(2) . . ? C29' C28' C27' 125(3) . . ? C28' C29' O5' 131(3) . . ? C19 C18 C17 127(3) . . ? O8' C35' O7' 125(3) . . ? O8' C35' C36' 124(3) . . ? O7' C35' C36' 110(2) . . ? C6A N2' C2A 125(2) . . ? C6A N2' C1' 102.9(17) . . ? C2A N2' C1' 132.1(19) . . ? C6A N3' C9' 109.4(17) . . ? C122 N1' C2' 129.2(18) . . ? C12' O3' C6' 104.8(14) . . ? C27' O6' C37' 108.8(18) . . ? C35' O7' C25' 118.4(19) . . ? C29' O5' C12' 118.8(19) . . ? _diffrn_measured_fraction_theta_max 0.783 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.831 _refine_diff_density_max 0.667 _refine_diff_density_min -0.295 _refine_diff_density_rms 0.073 # Attachment '- beta_3w.cif' data_rifax_epsilon _database_code_depnum_ccdc_archive 'CCDC 886513' #TrackingRef '- beta_3w.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H57 N3 O14' _chemical_formula_weight 839.92 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.7960(8) _cell_length_b 19.944(4) _cell_length_c 16.607(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.1800(10) _cell_angle_gamma 90.00 _cell_volume 4566.1(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_T_min 0.98216 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #============================================================================== # EXPERIMENTAL DATA _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19355 _diffrn_reflns_av_R_equivalents 0.1690 _diffrn_reflns_av_sigmaI/netI 0.5959 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 27.81 _reflns_number_total 14023 _reflns_number_gt 2253 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _chemical_absolute_configuration rm _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^)+(0.2000P)^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 noref _refine_ls_extinction_method SHELXL _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 7(5) _refine_ls_number_reflns 14023 _refine_ls_number_parameters 503 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.5247 _refine_ls_R_factor_gt 0.1946 _refine_ls_wR_factor_ref 0.4500 _refine_ls_wR_factor_gt 0.4058 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.963 _refine_ls_shift/su_max 0.100 _refine_ls_shift/su_mean 0.071 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 N1 N 1.0325(15) 0.9347(10) 1.1325(12) 0.078(6) Uani 1 1 d . . . H1 H 1.0589 0.9156 1.0924 0.093 Uiso 1 1 calc R . . N3 N 0.8292(16) 0.7915(8) 1.2669(9) 0.114(9) Uani 1 1 d D . . H3 H 0.7833 0.7731 1.2926 0.137 Uiso 1 1 calc R . . O1 O 0.8719(14) 1.0044(15) 1.0652(13) 0.149(10) Uani 1 1 d . . . H1A H 0.8238 1.0111 1.0358 0.224 Uiso 1 1 calc R . . O2 O 0.7058(12) 1.0261(10) 1.0485(12) 0.116(7) Uani 1 1 d . . . O3 O 0.4770(11) 0.9040(10) 1.1976(11) 0.122(8) Uani 1 1 d D . . O4 O 0.6251(16) 0.7799(9) 1.2870(16) 0.157(10) Uani 1 1 d . . . O5 O 0.4599(15) 0.8600(11) 1.3317(15) 0.130(8) Uani 1 1 d . . . O6 O 0.6412(19) 1.0381(12) 1.4565(13) 0.153(10) Uani 1 1 d . . . O7 O 0.7772(14) 0.9131(9) 1.5734(13) 0.102(7) Uani 1 1 d . . . O8 O 0.7549(19) 1.0103(12) 1.6457(12) 0.149(9) Uani 1 1 d . . . O9 O 0.9890(16) 1.0162(11) 1.5804(12) 0.111(6) Uiso 1 1 d . . . H9 H 0.9969 1.0368 1.5385 0.167 Uiso 1 1 calc R . . O10 O 1.1379(16) 1.0312(11) 1.4864(15) 0.135(8) Uiso 1 1 d . . . H10 H 1.1892 1.0386 1.5115 0.203 Uiso 1 1 calc R . . O11 O 1.0363(15) 1.0063(11) 1.2181(12) 0.125(7) Uiso 1 1 d . . . C9 C 0.8547(9) 0.9567(7) 1.1137(8) 0.098(10) Uiso 1 1 d GD . . C1 C 0.9298(8) 0.9161(9) 1.1433(9) 0.110(11) Uiso 1 1 d GD . . C2 C 0.9101(9) 0.8626(8) 1.1937(8) 0.076(8) Uiso 1 1 d GD . . C3 C 0.8153(10) 0.8496(6) 1.2145(6) 0.079(8) Uiso 1 1 d GD . . C4 C 0.7401(8) 0.8902(5) 1.1849(5) 0.085(8) Uiso 1 1 d GD . . C8 C 0.7598(8) 0.9437(6) 1.1345(6) 0.061(7) Uiso 1 1 d GD . . C7 C 0.6847(11) 0.9843(6) 1.1049(8) 0.120(12) Uiso 1 1 d G . . C6 C 0.5899(9) 0.9713(8) 1.1257(9) 0.128(12) Uiso 1 1 d GD . . C5 C 0.5702(8) 0.9177(8) 1.1760(8) 0.095(9) Uiso 1 1 d GD . . C10 C 0.6453(9) 0.8772(7) 1.2056(6) 0.063(7) Uiso 1 1 d GD . . C11 C 0.593(2) 0.8330(11) 1.2511(10) 0.095(9) Uiso 1 1 d D . . C12 C 0.496(3) 0.8486(12) 1.2459(14) 0.142(14) Uiso 1 1 d D . . C13 C 0.427(3) 0.8068(19) 1.212(2) 0.158(15) Uiso 1 1 d . . . H13A H 0.4242 0.7663 1.2435 0.237 Uiso 1 1 calc R . . H13B H 0.4429 0.7961 1.1582 0.237 Uiso 1 1 calc R . . H13C H 0.3648 0.8287 1.2121 0.237 Uiso 1 1 calc R . . C14 C 0.510(2) 1.0151(18) 1.1012(19) 0.137(13) Uiso 1 1 d . . . H14A H 0.4502 0.9971 1.1204 0.206 Uiso 1 1 calc R . . H14B H 0.5052 1.0180 1.0435 0.206 Uiso 1 1 calc R . . H14C H 0.5203 1.0590 1.1235 0.206 Uiso 1 1 calc R . . C15 C 1.085(2) 0.9721(14) 1.1704(16) 0.069(8) Uiso 1 1 d . . . C16 C 1.1794(18) 0.9828(14) 1.1621(15) 0.075(8) Uiso 1 1 d . . . H16 H 1.1753 1.0316 1.1677 0.090 Uiso 1 1 calc R . . C17 C 1.251(3) 0.9743(16) 1.225(2) 0.129(12) Uiso 1 1 d . . . H17 H 1.3168 0.9820 1.2172 0.155 Uiso 1 1 calc R . . C18 C 1.212(3) 0.9504(19) 1.311(2) 0.153(14) Uiso 1 1 d . . . H18 H 1.1486 0.9347 1.3152 0.184 Uiso 1 1 calc R . . C19 C 1.262(3) 0.9530(18) 1.368(2) 0.136(13) Uiso 1 1 d . . . H19 H 1.3231 0.9715 1.3601 0.163 Uiso 1 1 calc R . . C20 C 1.243(3) 0.9288(17) 1.460(2) 0.134(13) Uiso 1 1 d . . . H20 H 1.2900 0.9464 1.4998 0.161 Uiso 1 1 calc R . . C21 C 1.127(2) 0.9567(14) 1.4732(17) 0.093(9) Uiso 1 1 d . . . H21 H 1.0813 0.9453 1.4285 0.111 Uiso 1 1 calc R . . C22 C 1.096(3) 0.9282(19) 1.556(2) 0.149(14) Uiso 1 1 d . . . H22 H 1.0943 0.8795 1.5476 0.178 Uiso 1 1 calc R . . C23 C 0.9852(19) 0.9485(13) 1.5644(15) 0.080(8) Uiso 1 1 d D . . H23 H 0.9594 0.9251 1.6108 0.097 Uiso 1 1 calc R . . C24 C 0.923(2) 0.9286(18) 1.4864(19) 0.146(13) Uiso 1 1 d D . . H24 H 0.9471 0.9516 1.4389 0.175 Uiso 1 1 calc R . . C25 C 0.8118(18) 0.9550(15) 1.5076(16) 0.086(8) Uiso 1 1 d . . . H25 H 0.8113 1.0027 1.5216 0.103 Uiso 1 1 calc R . . C26 C 0.748(2) 0.9404(15) 1.4295(16) 0.101(9) Uiso 1 1 d . . . H26 H 0.7546 0.8934 1.4131 0.121 Uiso 1 1 calc R . . C27 C 0.639(2) 0.9580(14) 1.4448(17) 0.087(8) Uiso 1 1 d . . . H27 H 0.6204 0.9372 1.4956 0.104 Uiso 1 1 calc R . . C28 C 0.572(2) 0.9375(17) 1.383(2) 0.116(11) Uiso 1 1 d . . . H28 H 0.5675 0.9619 1.3356 0.139 Uiso 1 1 calc R . . C29 C 0.514(3) 0.883(2) 1.391(3) 0.159(16) Uiso 1 1 d . . . H29 H 0.5128 0.8619 1.4412 0.191 Uiso 1 1 calc R . . C30 C 1.221(2) 0.9845(16) 1.0847(17) 0.118(11) Uiso 1 1 d . . . H30A H 1.1705 0.9906 1.0439 0.177 Uiso 1 1 calc R . . H30B H 1.2542 0.9431 1.0755 0.177 Uiso 1 1 calc R . . H30C H 1.2661 1.0211 1.0827 0.177 Uiso 1 1 calc R . . C31 C 1.246(2) 0.8552(15) 1.4506(18) 0.115(11) Uiso 1 1 d . . . H31A H 1.2314 0.8343 1.5007 0.173 Uiso 1 1 calc R . . H31B H 1.3103 0.8421 1.4359 0.173 Uiso 1 1 calc R . . H31C H 1.2000 0.8413 1.4094 0.173 Uiso 1 1 calc R . . C32 C 1.171(3) 0.9378(18) 1.629(2) 0.148(14) Uiso 1 1 d . . . H32A H 1.2326 0.9202 1.6155 0.223 Uiso 1 1 calc R . . H32B H 1.1479 0.9145 1.6753 0.223 Uiso 1 1 calc R . . H32C H 1.1769 0.9847 1.6414 0.223 Uiso 1 1 calc R . . C33 C 0.928(2) 0.8548(13) 1.4763(16) 0.096(9) Uiso 1 1 d . . . H33A H 0.8876 0.8418 1.4303 0.144 Uiso 1 1 calc R . . H33B H 0.9044 0.8334 1.5237 0.144 Uiso 1 1 calc R . . H33C H 0.9933 0.8413 1.4684 0.144 Uiso 1 1 calc R . . C34 C 0.7719(17) 0.9891(12) 1.3577(13) 0.069(7) Uiso 1 1 d . . . H34A H 0.8348 0.9785 1.3384 0.104 Uiso 1 1 calc R . . H34B H 0.7714 1.0346 1.3764 0.104 Uiso 1 1 calc R . . H34C H 0.7239 0.9837 1.3148 0.104 Uiso 1 1 calc R . . C35 C 0.755(2) 0.9461(19) 1.637(2) 0.097(10) Uiso 1 1 d . . . C36 C 0.7031(19) 0.9070(15) 1.6980(15) 0.093(9) Uiso 1 1 d . . . H36A H 0.7099 0.8600 1.6873 0.140 Uiso 1 1 calc R . . H36B H 0.6356 0.9188 1.6955 0.140 Uiso 1 1 calc R . . H36C H 0.7302 0.9169 1.7508 0.140 Uiso 1 1 calc R . . C37 C 0.553(4) 1.044(3) 1.504(3) 0.25(3) Uiso 1 1 d . . . H37A H 0.5391 1.0905 1.5130 0.371 Uiso 1 1 calc R . . H37B H 0.5644 1.0222 1.5555 0.371 Uiso 1 1 calc R . . H37C H 0.4996 1.0231 1.4759 0.371 Uiso 1 1 calc R . . N2 N 0.9740(13) 0.8162(7) 1.2299(7) 0.103(8) Uani 1 1 d GD . . C211 C 1.0742(13) 0.8080(8) 1.2316(9) 0.106(10) Uiso 1 1 d GD . . H211 H 1.1127 0.8382 1.2045 0.127 Uiso 1 1 calc R . . C311 C 1.1167(9) 0.7548(9) 1.2739(9) 0.142(13) Uiso 1 1 d GD . . H311 H 1.1837 0.7494 1.2751 0.170 Uiso 1 1 calc R . . C411 C 1.0592(12) 0.7098(7) 1.3144(8) 0.055(6) Uiso 1 1 d G . . C511 C 0.9591(12) 0.7179(8) 1.3127(9) 0.072(8) Uiso 1 1 d G . . H511 H 0.9206 0.6877 1.3398 0.086 Uiso 1 1 calc R . . C611 C 0.9165(9) 0.7711(9) 1.2705(9) 0.101(10) Uiso 1 1 d G . . C711 C 1.122(2) 0.6726(18) 1.360(2) 0.153(14) Uiso 1 1 d . . . H71A H 1.1862 0.6765 1.3398 0.229 Uiso 1 1 calc R . . H71B H 1.1025 0.6264 1.3588 0.229 Uiso 1 1 calc R . . H71C H 1.1230 0.6884 1.4150 0.229 Uiso 1 1 calc R . . N1' N 1.0397(18) 0.7575(13) 1.0047(12) 0.171(15) Uani 1 1 d D . . H1' H 1.0538 0.7394 0.9596 0.205 Uiso 1 1 calc R . . N3' N 0.7819(18) 0.8954(9) 0.9166(10) 0.135(10) Uani 1 1 d D . . H3' H 0.7252 0.9116 0.9056 0.163 Uiso 1 1 calc R . . O1' O 0.9104(14) 0.6678(12) 1.0798(10) 0.130(8) Uani 1 1 d . . . O2' O 0.7397(15) 0.6408(12) 1.1173(13) 0.129(8) Uani 1 1 d . . . H2' H 0.7975 0.6325 1.1130 0.194 Uiso 1 1 calc R . . O3' O 0.4846(9) 0.7713(9) 1.0195(10) 0.131(8) Uani 1 1 d D . . O4' O 0.5998(14) 0.9028(11) 0.9173(11) 0.114(7) Uani 1 1 d . . . O5' O 0.4292(14) 0.8089(10) 0.8813(11) 0.102(6) Uani 1 1 d . . . O6' O 0.563(2) 0.6316(11) 0.7380(15) 0.148(9) Uani 1 1 d . . . O7' O 0.7227(13) 0.7289(8) 0.6402(12) 0.094(6) Uani 1 1 d . . . O8' O 0.6815(15) 0.6427(12) 0.5630(12) 0.118(7) Uiso 1 1 d . . . O9' O 0.9155(13) 0.6002(9) 0.6485(10) 0.085(5) Uiso 1 1 d . . . H9' H 0.9556 0.5870 0.6826 0.127 Uiso 1 1 calc R . . O10' O 1.0946(17) 0.6028(11) 0.7371(12) 0.124(7) Uiso 1 1 d . . . H10' H 1.1203 0.5823 0.7008 0.185 Uiso 1 1 calc R . . O11' O 1.122(2) 0.8260(16) 1.0566(16) 0.169(10) Uiso 1 1 d . . . C9' C 0.8769(8) 0.7223(4) 1.0375(8) 0.107(10) Uiso 1 1 d GD . . C1' C 0.9402(7) 0.7669(6) 1.0024(8) 0.063(7) Uiso 1 1 d GD . . C2' C 0.9041(9) 0.8237(5) 0.9630(8) 0.103(10) Uiso 1 1 d GD . . C3' C 0.8049(10) 0.8358(4) 0.9587(7) 0.093(9) Uiso 1 1 d GD . . C4' C 0.7416(8) 0.7912(4) 0.9937(5) 0.117(11) Uiso 1 1 d GD . . C8' C 0.7776(8) 0.7344(3) 1.0331(6) 0.119(11) Uiso 1 1 d GD . . C7' C 0.7143(10) 0.6898(5) 1.0682(8) 0.086(8) Uiso 1 1 d GD . . C6' C 0.6151(9) 0.7019(7) 1.0639(8) 0.090(9) Uiso 1 1 d GD . . C5' C 0.5791(7) 0.7587(8) 1.0245(8) 0.078(8) Uiso 1 1 d GD . . C10' C 0.6423(8) 0.8033(6) 0.9894(7) 0.084(8) Uiso 1 1 d GD . . C11' C 0.5765(15) 0.8444(9) 0.9523(10) 0.062(7) Uiso 1 1 d D . . C12' C 0.4793(19) 0.8268(12) 0.9662(12) 0.105(10) Uiso 1 1 d D . . C13' C 0.414(2) 0.8751(14) 0.9886(16) 0.103(10) Uiso 1 1 d . . . H13D' H 0.3503 0.8563 0.9881 0.154 Uiso 1 1 calc R . . H13E' H 0.4156 0.9119 0.9514 0.154 Uiso 1 1 calc R . . H13F' H 0.4318 0.8908 1.0418 0.154 Uiso 1 1 calc R . . C14' C 0.543(2) 0.6560(17) 1.1024(19) 0.141(13) Uiso 1 1 d . . . H14D' H 0.5767 0.6178 1.1250 0.211 Uiso 1 1 calc R . . H14E' H 0.4958 0.6413 1.0625 0.211 Uiso 1 1 calc R . . H14F' H 0.5116 0.6797 1.1443 0.211 Uiso 1 1 calc R . . C15' C 1.120(3) 0.764(2) 1.046(3) 0.154(14) Uiso 1 1 d . . . C16' C 1.2122(19) 0.7069(13) 1.0357(15) 0.081(8) Uiso 1 1 d . . . H16' H 1.2607 0.7425 1.0422 0.098 Uiso 1 1 calc R . . C17' C 1.242(3) 0.695(2) 0.958(3) 0.174(16) Uiso 1 1 d . . . H17' H 1.2950 0.6659 0.9580 0.209 Uiso 1 1 calc R . . C18' C 1.213(2) 0.7142(18) 0.877(2) 0.133(12) Uiso 1 1 d . . . H18' H 1.1796 0.7545 0.8696 0.159 Uiso 1 1 calc R . . C19' C 1.2321(19) 0.6754(15) 0.8070(16) 0.094(9) Uiso 1 1 d . . . H19' H 1.2651 0.6350 0.8132 0.113 Uiso 1 1 calc R . . C20' C 1.2020(19) 0.6971(13) 0.7275(16) 0.081(8) Uiso 1 1 d . . . H20' H 1.2408 0.6755 0.6867 0.097 Uiso 1 1 calc R . . C21' C 1.095(2) 0.6749(17) 0.7192(19) 0.118(11) Uiso 1 1 d . . . H21' H 1.0622 0.6967 0.7634 0.142 Uiso 1 1 calc R . . C22' C 1.0332(18) 0.6878(13) 0.6441(15) 0.076(8) Uiso 1 1 d . . . H22' H 1.0346 0.7368 0.6399 0.092 Uiso 1 1 calc R . . C23' C 0.921(2) 0.6723(16) 0.6418(19) 0.109(10) Uiso 1 1 d . . . H23' H 0.8894 0.6884 0.5918 0.131 Uiso 1 1 calc R . . C24' C 0.8684(17) 0.6997(12) 0.7197(14) 0.067(7) Uiso 1 1 d . . . H24' H 0.8905 0.6737 0.7670 0.081 Uiso 1 1 calc R . . C25' C 0.762(2) 0.6900(16) 0.7061(17) 0.098(9) Uiso 1 1 d . . . H25' H 0.7507 0.6426 0.6935 0.117 Uiso 1 1 calc R . . C26' C 0.7019(19) 0.7079(15) 0.7807(16) 0.090(9) Uiso 1 1 d . . . H26' H 0.7143 0.7540 0.7986 0.108 Uiso 1 1 calc R . . C27' C 0.5835(17) 0.6974(13) 0.7487(14) 0.063(7) Uiso 1 1 d . . . H27' H 0.5715 0.7215 0.6979 0.076 Uiso 1 1 calc R . . C28' C 0.523(3) 0.729(2) 0.815(3) 0.164(16) Uiso 1 1 d . . . H28' H 0.5144 0.7025 0.8603 0.197 Uiso 1 1 calc R . . C29' C 0.487(2) 0.7800(18) 0.817(2) 0.104(10) Uiso 1 1 d . . . H29' H 0.4945 0.8070 0.7721 0.125 Uiso 1 1 calc R . . C30' C 1.249(2) 0.6742(18) 1.1189(19) 0.141(13) Uiso 1 1 d . . . H30D' H 1.2243 0.6995 1.1628 0.211 Uiso 1 1 calc R . . H30E' H 1.3186 0.6746 1.1224 0.211 Uiso 1 1 calc R . . H30F' H 1.2263 0.6288 1.1217 0.211 Uiso 1 1 calc R . . C31' C 1.200(3) 0.7705(16) 0.717(2) 0.140(13) Uiso 1 1 d . . . H31D' H 1.1813 0.7808 0.6617 0.210 Uiso 1 1 calc R . . H31E' H 1.2641 0.7883 0.7284 0.210 Uiso 1 1 calc R . . H31F' H 1.1552 0.7901 0.7521 0.210 Uiso 1 1 calc R . . C32' C 1.0789(18) 0.6687(13) 0.5787(14) 0.085(8) Uiso 1 1 d . . . H32D' H 1.0442 0.6850 0.5314 0.128 Uiso 1 1 calc R . . H32E' H 1.0819 0.6206 0.5769 0.128 Uiso 1 1 calc R . . H32F' H 1.1435 0.6867 0.5806 0.128 Uiso 1 1 calc R . . C33' C 0.8979(18) 0.7780(12) 0.7332(16) 0.087(8) Uiso 1 1 d . . . H33D' H 0.8657 0.7952 0.7791 0.131 Uiso 1 1 calc R . . H33E' H 0.8784 0.8034 0.6862 0.131 Uiso 1 1 calc R . . H33F' H 0.9668 0.7815 0.7423 0.131 Uiso 1 1 calc R . . C34' C 0.7251(15) 0.6608(10) 0.8435(12) 0.052(6) Uiso 1 1 d . . . H34D' H 0.7921 0.6656 0.8603 0.078 Uiso 1 1 calc R . . H34E' H 0.7138 0.6161 0.8239 0.078 Uiso 1 1 calc R . . H34F' H 0.6851 0.6691 0.8884 0.078 Uiso 1 1 calc R . . C35' C 0.693(3) 0.704(3) 0.557(3) 0.157(15) Uiso 1 1 d . . . C36' C 0.652(2) 0.7472(18) 0.507(2) 0.139(13) Uiso 1 1 d . . . H36D' H 0.6499 0.7905 0.5322 0.209 Uiso 1 1 calc R . . H36E' H 0.5870 0.7328 0.4930 0.209 Uiso 1 1 calc R . . H36F' H 0.6886 0.7500 0.4592 0.209 Uiso 1 1 calc R . . C37' C 0.480(4) 0.634(3) 0.691(3) 0.23(2) Uiso 1 1 d . . . H37D' H 0.4572 0.5898 0.6800 0.341 Uiso 1 1 calc R . . H37E' H 0.4931 0.6566 0.6412 0.341 Uiso 1 1 calc R . . H37F' H 0.4316 0.6590 0.7186 0.341 Uiso 1 1 calc R . . N2' N 0.9447(17) 0.8787(8) 0.9235(9) 0.139(12) Uani 1 1 d GD . . C2A C 1.0409(14) 0.8913(9) 0.9067(11) 0.202(19) Uiso 1 1 d GD . . H2A' H 1.0893 0.8618 0.9247 0.242 Uiso 1 1 calc R . . C3A C 1.0649(12) 0.9480(10) 0.8631(12) 0.109(10) Uiso 1 1 d GD . . H3A' H 1.1293 0.9564 0.8518 0.131 Uiso 1 1 calc R . . C4A C 0.9926(17) 0.9921(8) 0.8362(10) 0.083(8) Uiso 1 1 d GD . . C5A C 0.8964(14) 0.9795(10) 0.8530(12) 0.111(10) Uiso 1 1 d GD . . H5A' H 0.8481 1.0090 0.8350 0.133 Uiso 1 1 calc R . . C6A C 0.8724(12) 0.9228(11) 0.8966(12) 0.163(17) Uiso 1 1 d GD . . C7A C 1.0082(10) 1.0508(7) 0.7934(8) 0.132(12) Uiso 1 1 d . . . H7A1' H 1.0758 1.0547 0.7825 0.198 Uiso 1 1 calc R . . H7A2' H 0.9887 1.0886 0.8247 0.198 Uiso 1 1 calc R . . H7A3' H 0.9707 1.0497 0.7435 0.198 Uiso 1 1 calc R . . O2W O 0.3236(10) 0.5345(7) 0.1236(8) 0.31(2) Uiso 1 1 d . . . O4W O 0.3732(10) 0.5969(7) 0.2711(8) 0.260(16) Uiso 1 1 d . . . O1W O 0.9837(10) 0.6072(7) 0.9253(8) 0.189(11) Uiso 1 1 d . . . O7W O 0.6939(10) 0.5352(7) 0.2227(8) 0.240(15) Uiso 1 1 d . . . O3W O 0.5137(10) 0.4834(7) 0.2142(8) 0.262(17) Uiso 1 1 d . . . O8W O 0.5404(10) 0.6668(7) 0.3571(8) 0.33(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.086(16) 0.064(14) 0.081(15) -0.012(13) -0.013(13) -0.002(13) O1 0.098(16) 0.24(2) 0.111(17) 0.128(19) -0.008(13) -0.052(18) O2 0.067(13) 0.134(16) 0.146(17) 0.038(15) -0.015(12) -0.049(13) O3 0.064(13) 0.093(14) 0.21(2) -0.078(16) 0.017(13) 0.020(12) O4 0.15(2) 0.061(13) 0.27(3) -0.003(16) 0.12(2) 0.051(13) O5 0.088(16) 0.126(17) 0.18(2) -0.045(17) 0.027(15) 0.013(14) O6 0.19(2) 0.15(2) 0.118(18) -0.029(16) 0.010(17) 0.089(19) O7 0.112(16) 0.075(12) 0.120(17) 0.045(14) 0.019(13) 0.033(12) O8 0.26(3) 0.096(16) 0.092(15) 0.020(13) 0.082(16) -0.030(18) N2 0.064(15) 0.15(2) 0.095(17) -0.031(17) 0.023(13) 0.024(16) N3' 0.12(2) 0.15(2) 0.14(2) -0.01(2) 0.065(17) -0.03(2) O1' 0.123(16) 0.20(2) 0.067(12) -0.048(14) -0.032(11) 0.081(17) O2' 0.160(18) 0.146(18) 0.083(14) 0.082(14) 0.015(15) 0.052(18) O3' 0.026(9) 0.162(18) 0.21(2) 0.076(18) 0.047(11) 0.023(12) O4' 0.109(16) 0.125(16) 0.107(15) -0.022(15) -0.017(12) -0.008(14) O5' 0.111(15) 0.101(14) 0.092(14) -0.026(12) -0.018(12) -0.010(13) O6' 0.17(2) 0.084(16) 0.19(2) -0.050(16) 0.04(2) -0.011(16) O7' 0.109(15) 0.061(11) 0.112(15) 0.010(11) 0.008(12) 0.014(11) N2' 0.090(19) 0.24(3) 0.093(18) -0.10(2) 0.049(16) -0.01(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C15 1.20(3) . ? N1 C1 1.48(2) . ? N3 C611 1.27(2) . ? N3 C3 1.46(2) . ? O1 C9 1.27(2) . ? O2 C7 1.29(2) . ? O3 C5 1.376(15) . ? O3 C12 1.384(14) . ? O4 C11 1.28(3) . ? O5 C29 1.30(4) . ? O5 C12 1.55(3) . ? O6 C37 1.48(5) . ? O6 C27 1.61(3) . ? O7 C35 1.29(3) . ? O7 C25 1.47(3) . ? O8 C35 1.29(3) . ? O9 C23 1.38(3) . ? O10 C21 1.51(3) . ? O11 C15 1.26(3) . ? C9 C1 1.3900 . ? C9 C8 1.3900 . ? C1 C2 1.3900 . ? C2 C3 1.3900 . ? C2 N2 1.398(17) . ? C3 C4 1.3900 . ? C4 C8 1.3900 . ? C4 C10 1.3900 . ? C8 C7 1.3900 . ? C7 C6 1.3900 . ? C6 C5 1.3900 . ? C6 C14 1.46(3) . ? C5 C10 1.3900 . ? C10 C11 1.379(13) . ? C11 C12 1.379(19) . ? C12 C13 1.37(4) . ? C15 C16 1.33(3) . ? C16 C17 1.42(3) . ? C16 C30 1.43(3) . ? C17 C18 1.63(4) . ? C18 C19 1.15(4) . ? C19 C20 1.63(4) . ? C20 C31 1.48(4) . ? C20 C21 1.71(4) . ? C21 C22 1.56(4) . ? C22 C32 1.57(4) . ? C22 C23 1.59(4) . ? C23 C24 1.573(18) . ? C24 C33 1.48(4) . ? C24 C25 1.68(4) . ? C25 C26 1.57(3) . ? C26 C27 1.58(3) . ? C26 C34 1.58(3) . ? C27 C28 1.41(4) . ? C28 C29 1.36(4) . ? C35 C36 1.48(4) . ? N2 C211 1.3900 . ? N2 C611 1.3900 . ? C211 C311 1.3900 . ? C311 C411 1.3900 . ? C411 C711 1.36(3) . ? C411 C511 1.3900 . ? C511 C611 1.3900 . ? N1' C15' 1.29(4) . ? N1' C1' 1.39(2) . ? N3' C3' 1.408(17) . ? N3' C6A 1.41(3) . ? O1' C9' 1.37(2) . ? O2' C7' 1.311(18) . ? O3' C5' 1.326(14) . ? O3' C12' 1.419(17) . ? O4' C11' 1.35(2) . ? O5' C29' 1.47(3) . ? O5' C12' 1.59(3) . ? O6' C27' 1.35(3) . ? O6' C37' 1.36(4) . ? O7' C25' 1.43(3) . ? O7' C35' 1.51(4) . ? O8' C35' 1.24(4) . ? O9' C23' 1.45(3) . ? O10' C21' 1.47(3) . ? O11' C15' 1.24(4) . ? C9' C1' 1.3900 . ? C9' C8' 1.3900 . ? C1' C2' 1.3900 . ? C2' C3' 1.3900 . ? C2' N2' 1.405(14) . ? C3' C4' 1.3900 . ? C4' C8' 1.3900 . ? C4' C10' 1.3900 . ? C8' C7' 1.3900 . ? C7' C6' 1.3900 . ? C6' C5' 1.3900 . ? C6' C14' 1.51(3) . ? C5' C10' 1.3900 . ? C10' C11' 1.355(14) . ? C11' C12' 1.413(18) . ? C12' C13' 1.38(3) . ? C15' C16' 1.72(5) . ? C16' C17' 1.39(4) . ? C16' C30' 1.59(4) . ? C17' C18' 1.44(4) . ? C18' C19' 1.43(4) . ? C19' C20' 1.44(3) . ? C20' C31' 1.47(4) . ? C20' C21' 1.54(4) . ? C21' C22' 1.51(3) . ? C22' C32' 1.33(3) . ? C22' C23' 1.57(3) . ? C23' C24' 1.61(4) . ? C24' C25' 1.49(3) . ? C24' C33' 1.63(3) . ? C25' C26' 1.56(3) . ? C26' C34' 1.43(3) . ? C26' C27' 1.71(3) . ? C27' C28' 1.55(4) . ? C28' C29' 1.13(4) . ? C35' C36' 1.31(5) . ? N2' C2A 1.3900 . ? N2' C6A 1.3900 . ? C2A C3A 1.3900 . ? C3A C4A 1.3900 . ? C4A C5A 1.3900 . ? C4A C7A 1.391(18) . ? C5A C6A 1.3900 . ? 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 C15 N1 C1 131(2) . . ? C611 N3 C3 113(2) . . ? C5 O3 C12 99(2) . . ? C29 O5 C12 124(3) . . ? C37 O6 C27 97(3) . . ? C35 O7 C25 114(2) . . ? O1 C9 C1 120.3(14) . . ? O1 C9 C8 119.7(13) . . ? C1 C9 C8 120.0 . . ? C2 C1 C9 120.0 . . ? C2 C1 N1 118.4(13) . . ? C9 C1 N1 121.0(13) . . ? C1 C2 C3 120.0 . . ? C1 C2 N2 129.3(13) . . ? C3 C2 N2 110.7(13) . . ? C4 C3 C2 120.0 . . ? C4 C3 N3 138.9(13) . . ? C2 C3 N3 101.1(12) . . ? C3 C4 C8 120.0 . . ? C3 C4 C10 120.0 . . ? C8 C4 C10 120.0 . . ? C7 C8 C4 120.0 . . ? C7 C8 C9 120.0 . . ? C4 C8 C9 120.0 . . ? O2 C7 C6 122.6(12) . . ? O2 C7 C8 116.4(12) . . ? C6 C7 C8 120.0 . . ? C7 C6 C5 120.0 . . ? C7 C6 C14 122.2(17) . . ? C5 C6 C14 117.7(18) . . ? O3 C5 C10 118.9(14) . . ? O3 C5 C6 121.1(14) . . ? C10 C5 C6 120.0 . . ? C11 C10 C5 99.8(17) . . ? C11 C10 C4 140.2(17) . . ? C5 C10 C4 120.0 . . ? O4 C11 C12 122(2) . . ? O4 C11 C10 127(3) . . ? C12 C11 C10 110(3) . . ? C13 C12 C11 123(2) . . ? C13 C12 O3 98(2) . . ? C11 C12 O3 112(3) . . ? C13 C12 O5 103(3) . . ? C11 C12 O5 108.8(16) . . ? O3 C12 O5 110.9(18) . . ? N1 C15 O11 110(3) . . ? N1 C15 C16 128(3) . . ? O11 C15 C16 122(3) . . ? C15 C16 C17 124(3) . . ? C15 C16 C30 122(3) . . ? C17 C16 C30 112(3) . . ? C16 C17 C18 116(3) . . ? C19 C18 C17 120(4) . . ? C18 C19 C20 129(4) . . ? C31 C20 C19 101(3) . . ? C31 C20 C21 112(3) . . ? C19 C20 C21 102(3) . . ? O10 C21 C22 105(3) . . ? O10 C21 C20 104(2) . . ? C22 C21 C20 106(2) . . ? C21 C22 C32 116(3) . . ? C21 C22 C23 106(3) . . ? C32 C22 C23 120(3) . . ? O9 C23 C24 115(3) . . ? O9 C23 C22 104(2) . . ? C24 C23 C22 111(2) . . ? C33 C24 C23 109(3) . . ? C33 C24 C25 112(3) . . ? C23 C24 C25 103(2) . . ? O7 C25 C26 109(2) . . ? O7 C25 C24 108(2) . . ? C26 C25 C24 105(2) . . ? C25 C26 C27 110(2) . . ? C25 C26 C34 113(2) . . ? C27 C26 C34 102(2) . . ? C28 C27 C26 115(2) . . ? C28 C27 O6 113(3) . . ? C26 C27 O6 103(2) . . ? C29 C28 C27 122(4) . . ? O5 C29 C28 122(4) . . ? O8 C35 O7 127(3) . . ? O8 C35 C36 116(3) . . ? O7 C35 C36 115(3) . . ? C211 N2 C611 120.0 . . ? C211 N2 C2 134.1(15) . . ? C611 N2 C2 105.9(15) . . ? N2 C211 C311 120.0 . . ? C411 C311 C211 120.0 . . ? C711 C411 C311 105(2) . . ? C711 C411 C511 134(2) . . ? C311 C411 C511 120.0 . . ? C411 C511 C611 120.0 . . ? N3 C611 C511 130.5(17) . . ? N3 C611 N2 109.1(17) . . ? C511 C611 N2 120.0 . . ? C15' N1' C1' 146(2) . . ? C3' N3' C6A 105.0(19) . . ? C5' O3' C12' 102.4(18) . . ? C29' O5' C12' 120(2) . . ? C27' O6' C37' 102(3) . . ? C25' O7' C35' 127(3) . . ? O1' C9' C1' 121.3(12) . . ? O1' C9' C8' 118.6(12) . . ? C1' C9' C8' 120.0 . . ? N1' C1' C9' 122.6(16) . . ? N1' C1' C2' 117.4(16) . . ? C9' C1' C2' 120.0 . . ? C3' C2' C1' 120.0 . . ? C3' C2' N2' 104.4(13) . . ? C1' C2' N2' 135.6(14) . . ? C4' C3' C2' 120.0 . . ? C4' C3' N3' 127.9(13) . . ? C2' C3' N3' 112.1(13) . . ? C8' C4' C3' 120.0 . . ? C8' C4' C10' 120.0 . . ? C3' C4' C10' 120.0 . . ? C7' C8' C4' 120.0 . . ? C7' C8' C9' 120.0 . . ? C4' C8' C9' 120.0 . . ? O2' C7' C6' 113.6(12) . . ? O2' C7' C8' 125.5(12) . . ? C6' C7' C8' 120.0 . . ? C5' C6' C7' 120.0 . . ? C5' C6' C14' 117.7(15) . . ? C7' C6' C14' 122.3(15) . . ? O3' C5' C6' 121.1(12) . . ? O3' C5' C10' 118.9(12) . . ? C6' C5' C10' 120.0 . . ? C11' C10' C5' 99.0(10) . . ? C11' C10' C4' 140.5(10) . . ? C5' C10' C4' 120.0 . . ? O4' C11' C10' 123.6(18) . . ? O4' C11' C12' 121.9(18) . . ? C10' C11' C12' 113.6(17) . . ? C13' C12' C11' 120.1(19) . . ? C13' C12' O3' 113(2) . . ? C11' C12' O3' 106(2) . . ? C13' C12' O5' 98(2) . . ? C11' C12' O5' 107.1(12) . . ? O3' C12' O5' 112.9(17) . . ? O11' C15' N1' 101(4) . . ? O11' C15' C16' 132(4) . . ? N1' C15' C16' 120(3) . . ? C17' C16' C30' 130(3) . . ? C17' C16' C15' 117(3) . . ? C30' C16' C15' 113(2) . . ? C16' C17' C18' 137(4) . . ? C19' C18' C17' 124(3) . . ? C18' C19' C20' 122(3) . . ? C19' C20' C31' 115(3) . . ? C19' C20' C21' 104(2) . . ? C31' C20' C21' 105(3) . . ? O10' C21' C22' 109(3) . . ? O10' C21' C20' 106(3) . . ? C22' C21' C20' 122(3) . . ? C32' C22' C21' 111(2) . . ? C32' C22' C23' 115(2) . . ? C21' C22' C23' 121(2) . . ? O9' C23' C22' 105(2) . . ? O9' C23' C24' 104(2) . . ? C22' C23' C24' 113(2) . . ? C25' C24' C23' 108(2) . . ? C25' C24' C33' 113(2) . . ? C23' C24' C33' 109(2) . . ? O7' C25' C24' 113(2) . . ? O7' C25' C26' 107(2) . . ? C24' C25' C26' 114(2) . . ? C34' C26' C25' 109(2) . . ? C34' C26' C27' 109(2) . . ? C25' C26' C27' 105(2) . . ? O6' C27' C28' 112(3) . . ? O6' C27' C26' 111(2) . . ? C28' C27' C26' 105(2) . . ? C29' C28' C27' 130(5) . . ? C28' C29' O5' 128(4) . . ? O8' C35' C36' 130(4) . . ? O8' C35' O7' 106(4) . . ? C36' C35' O7' 118(4) . . ? C2A N2' C6A 120.0 . . ? C2A N2' C2' 129.4(18) . . ? C6A N2' C2' 110.5(18) . . ? C3A C2A N2' 120.0 . . ? C4A C3A C2A 120.0 . . ? C3A C4A C5A 120.0 . . ? C3A C4A C7A 125.1(17) . . ? C5A C4A C7A 114.9(17) . . ? C6A C5A C4A 120.0 . . ? C5A C6A N2' 120.0 . . ? C5A C6A N3' 131.8(19) . . ? N2' C6A N3' 108.0(19) . . ? _diffrn_measured_fraction_theta_max 0.826 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.475 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.100 # Attachment '- beta_4.5w.cif' data_beta4r _database_code_depnum_ccdc_archive 'CCDC 886514' #TrackingRef '- beta_4.5w.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H60 N3 O15.5' _chemical_formula_weight 866.95 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.7530(8) _cell_length_b 19.749(4) _cell_length_c 16.378(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.9720(10) _cell_angle_gamma 90.00 _cell_volume 4445.8(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.295 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1852 _exptl_absorpt_coefficient_mu 0.248 _exptl_absorpt_correction_T_min 0.98216 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #============================================================================== # EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.0000 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11804 _diffrn_reflns_av_R_equivalents 0.0130 _diffrn_reflns_av_sigmaI/netI 0.0184 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 19.77 _reflns_number_total 6061 _reflns_number_gt 6019 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1030P)^2^+6.6989P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.048(2) _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_number_reflns 6061 _refine_ls_number_parameters 1096 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1480 _refine_ls_wR_factor_gt 0.1474 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.200 _refine_ls_shift/su_mean 0.083 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 N1 N 1.0374(4) 0.9349(3) 1.1269(3) 0.0244(16) Uani 1 1 d . . . H1 H 1.0658 0.9184 1.0854 0.029 Uiso 1 1 calc R . . N3 N 0.8312(5) 0.7819(3) 1.2599(3) 0.0258(15) Uani 1 1 d . . . O1 O 0.8774(3) 1.0056(2) 1.0631(3) 0.0362(14) Uani 1 1 d . . . H01 H 0.8259 1.0249 1.0514 0.054 Uiso 1 1 calc R . . O2 O 0.7031(4) 1.0287(3) 1.0535(3) 0.0350(13) Uani 1 1 d . . . O3 O 0.4885(5) 0.9054(2) 1.2158(3) 0.0358(15) Uani 1 1 d . . . O4 O 0.6365(4) 0.7724(3) 1.2969(4) 0.0510(16) Uani 1 1 d . . . O5 O 0.4639(4) 0.8547(3) 1.3451(3) 0.0493(17) Uani 1 1 d . . . O6 O 0.6522(6) 1.0353(3) 1.4593(4) 0.091(3) Uani 1 1 d . . . O7 O 0.7878(4) 0.9151(2) 1.5816(3) 0.0383(14) Uani 1 1 d . . . O8 O 0.7474(4) 1.0112(3) 1.6448(3) 0.0407(14) Uani 1 1 d . . . O9 O 0.9940(4) 1.0198(2) 1.5846(3) 0.0403(14) Uani 1 1 d . . . H9 H 1.0474 1.0375 1.5798 0.060 Uiso 1 1 calc R . . O10 O 1.1575(4) 1.0281(2) 1.4945(3) 0.0424(15) Uani 1 1 d . . . H10 H 1.1042 1.0432 1.5062 0.064 Uiso 1 1 calc R . . O11 O 1.0412(4) 1.0118(4) 1.2288(4) 0.079(3) Uani 1 1 d . . . H11 H 1.0796 1.0361 1.2546 0.119 Uiso 1 1 calc R . . C9 C 0.8606(6) 0.9532(4) 1.1127(4) 0.032(2) Uani 1 1 d . . . C1 C 0.9404(6) 0.9163(4) 1.1429(4) 0.029(2) Uani 1 1 d . . . C2 C 0.9180(6) 0.8607(3) 1.1928(4) 0.024(2) Uani 1 1 d . . . C3 C 0.8250(6) 0.8407(4) 1.2113(4) 0.029(2) Uani 1 1 d . . . C4 C 0.7432(6) 0.8794(3) 1.1842(4) 0.023(2) Uani 1 1 d . . . C8 C 0.7634(6) 0.9362(3) 1.1325(4) 0.0245(19) Uani 1 1 d . . . C7 C 0.6849(6) 0.9798(4) 1.1020(4) 0.031(2) Uani 1 1 d . . . C6 C 0.5888(7) 0.9710(4) 1.1298(4) 0.034(2) Uani 1 1 d . . . C5 C 0.5761(7) 0.9175(4) 1.1820(4) 0.029(2) Uani 1 1 d . . . C10 C 0.6478(6) 0.8697(4) 1.2066(4) 0.031(2) Uani 1 1 d . . . C11 C 0.6021(6) 0.8217(4) 1.2607(5) 0.036(2) Uani 1 1 d . . . C12 C 0.4951(6) 0.8437(4) 1.2653(5) 0.039(2) Uani 1 1 d . . . C13 C 0.4234(7) 0.7935(5) 1.2262(6) 0.057(3) Uani 1 1 d . . . H13A H 0.4397 0.7858 1.1705 0.086 Uiso 1 1 calc R . . H13B H 0.3587 0.8116 1.2279 0.086 Uiso 1 1 calc R . . H13C H 0.4266 0.7515 1.2557 0.086 Uiso 1 1 calc R . . C14 C 0.5097(6) 1.0195(4) 1.1050(5) 0.045(2) Uani 1 1 d . . . H14A H 0.5353 1.0536 1.0700 0.067 Uiso 1 1 calc R . . H14B H 0.4848 1.0406 1.1528 0.067 Uiso 1 1 calc R . . H14C H 0.4582 0.9956 1.0764 0.067 Uiso 1 1 calc R . . C15 C 1.0853(6) 0.9791(4) 1.1776(5) 0.036(2) Uani 1 1 d . . . H15 H 1.0748 1.0155 1.1376 0.044 Uiso 1 1 calc R . . C16 C 1.1921(5) 0.9831(3) 1.1668(4) 0.024(2) Uani 1 1 d . . . H16 H 1.1911 1.0323 1.1741 0.028 Uiso 1 1 calc R . . C17 C 1.2519(6) 0.9758(4) 1.2333(4) 0.028(2) Uani 1 1 d . . . H17 H 1.3181 0.9817 1.2258 0.034 Uiso 1 1 calc R . . C18 C 1.2227(6) 0.9597(4) 1.3154(4) 0.032(2) Uani 1 1 d . . . H18 H 1.1567 0.9531 1.3230 0.038 Uiso 1 1 calc R . . C19 C 1.2813(6) 0.9537(4) 1.3798(4) 0.035(2) Uani 1 1 d . . . H19 H 1.3461 0.9657 1.3741 0.042 Uiso 1 1 calc R . . C20 C 1.2512(6) 0.9284(4) 1.4636(4) 0.039(2) Uani 1 1 d . . . H20 H 1.2984 0.9457 1.5046 0.047 Uiso 1 1 calc R . . C21 C 1.1507(6) 0.9555(3) 1.4843(4) 0.030(2) Uani 1 1 d . . . H21 H 1.1056 0.9461 1.4381 0.036 Uiso 1 1 calc R . . C22 C 1.1063(6) 0.9267(4) 1.5633(4) 0.036(2) Uani 1 1 d . . . H22 H 1.1067 0.8772 1.5585 0.043 Uiso 1 1 calc R . . C23 C 1.0019(6) 0.9481(4) 1.5714(4) 0.034(2) Uani 1 1 d . . . H23 H 0.9783 0.9258 1.6204 0.041 Uiso 1 1 calc R . . C24 C 0.9332(6) 0.9272(4) 1.5000(4) 0.038(2) Uani 1 1 d . . . H24 H 0.9567 0.9498 1.4511 0.046 Uiso 1 1 calc R . . C25 C 0.8301(6) 0.9521(4) 1.5115(4) 0.037(2) Uani 1 1 d . . . H25 H 0.8326 1.0005 1.5249 0.045 Uiso 1 1 calc R . . C26 C 0.7593(7) 0.9421(4) 1.4371(4) 0.042(2) Uani 1 1 d . . . H26 H 0.7577 0.8935 1.4251 0.050 Uiso 1 1 calc R . . C27 C 0.6562(6) 0.9631(4) 1.4534(4) 0.047(3) Uani 1 1 d . . . H27 H 0.6380 0.9438 1.5058 0.057 Uiso 1 1 calc R . . C28 C 0.5854(8) 0.9366(5) 1.3867(5) 0.049(3) Uani 1 1 d . . . H28 H 0.5866 0.9557 1.3348 0.059 Uiso 1 1 calc R . . C29 C 0.5231(8) 0.8879(6) 1.4001(5) 0.055(3) Uani 1 1 d . . . H29 H 0.5188 0.8742 1.4542 0.066 Uiso 1 1 calc R . . C30 C 1.2248(6) 0.9909(4) 1.0810(4) 0.037(2) Uani 1 1 d . . . H30A H 1.1689 0.9932 1.0443 0.055 Uiso 1 1 calc R . . H30B H 1.2642 0.9528 1.0670 0.055 Uiso 1 1 calc R . . H30C H 1.2622 1.0317 1.0767 0.055 Uiso 1 1 calc R . . C31 C 1.2567(6) 0.8515(4) 1.4648(4) 0.041(2) Uani 1 1 d . . . H31A H 1.3212 0.8374 1.4517 0.061 Uiso 1 1 calc R . . H31B H 1.2107 0.8333 1.4252 0.061 Uiso 1 1 calc R . . H31C H 1.2419 0.8353 1.5181 0.061 Uiso 1 1 calc R . . C32 C 1.1682(7) 0.9448(4) 1.6398(4) 0.052(3) Uani 1 1 d . . . H32A H 1.2344 0.9315 1.6322 0.078 Uiso 1 1 calc R . . H32B H 1.1435 0.9214 1.6861 0.078 Uiso 1 1 calc R . . H32C H 1.1653 0.9927 1.6489 0.078 Uiso 1 1 calc R . . C33 C 0.9361(6) 0.8500(4) 1.4829(5) 0.048(2) Uani 1 1 d . . . H33A H 1.0019 0.8363 1.4744 0.072 Uiso 1 1 calc R . . H33B H 0.8966 0.8400 1.4349 0.072 Uiso 1 1 calc R . . H33C H 0.9115 0.8260 1.5288 0.072 Uiso 1 1 calc R . . C34 C 0.8015(7) 0.9776(4) 1.3617(4) 0.054(3) Uani 1 1 d . . . H34A H 0.8678 0.9639 1.3559 0.081 Uiso 1 1 calc R . . H34B H 0.7988 1.0258 1.3690 0.081 Uiso 1 1 calc R . . H34C H 0.7639 0.9653 1.3135 0.081 Uiso 1 1 calc R . . C35 C 0.7454(6) 0.9495(5) 1.6410(4) 0.040(2) Uani 1 1 d . . . C36 C 0.6956(7) 0.9051(4) 1.6989(4) 0.046(2) Uani 1 1 d . . . C37 C 0.5641(2) 1.05620(13) 1.49915(15) 0.162(9) Uani 1 1 d . . . H37A H 0.5615 1.1047 1.5015 0.243 Uiso 1 1 calc R . . H37B H 0.5645 1.0381 1.5536 0.243 Uiso 1 1 calc R . . H37C H 0.5082 1.0395 1.4687 0.243 Uiso 1 1 calc R . . N2 N 0.9808(2) 0.81519(13) 1.23386(15) 0.0232(15) Uani 1 1 d R . . C211 C 1.0816(2) 0.81313(13) 1.23997(15) 0.036(2) Uani 1 1 d R . . H211 H 1.1178 0.8464 1.2147 0.043 Uiso 1 1 calc R . . C311 C 1.1287(2) 0.76205(13) 1.28331(15) 0.0337(18) Uiso 1 1 d R . . H311 H 1.1963 0.7609 1.2872 0.040 Uiso 1 1 calc R . . C411 C 1.0750(2) 0.71303(13) 1.32053(15) 0.028(2) Uani 1 1 d R . . C511 C 0.9742(2) 0.71509(13) 1.31442(15) 0.032(2) Uani 1 1 d R . . H511 H 0.9380 0.6818 1.3397 0.038 Uiso 1 1 calc R . . C611 C 0.9271(2) 0.76617(13) 1.27109(15) 0.029(2) Uani 1 1 d R . . C711 C 1.1275(2) 0.65672(13) 1.36206(15) 0.045(2) Uani 1 1 d R . . H71A H 1.1960 0.6613 1.3542 0.067 Uiso 1 1 d R . . H71B H 1.1051 0.6144 1.3395 0.067 Uiso 1 1 d R . . H71C H 1.1153 0.6579 1.4194 0.067 Uiso 1 1 d R . . N1' N 1.0372(4) 0.7393(3) 0.9930(4) 0.0264(16) Uani 1 1 d . . . H1' H 1.0428 0.7061 0.9595 0.032 Uiso 1 1 calc R . . N3' N 0.7865(5) 0.8959(3) 0.9232(3) 0.0301(16) Uani 1 1 d . . . O1' O 0.9167(4) 0.6683(3) 1.0846(3) 0.0424(15) Uani 1 1 d . . . H01' H 0.8717 0.6458 1.1020 0.064 Uiso 1 1 calc R . . O2' O 0.7520(4) 0.6380(3) 1.1270(3) 0.0443(15) Uani 1 1 d . . . O3' O 0.4791(4) 0.7585(3) 1.0158(3) 0.0407(15) Uani 1 1 d . . . O4' O 0.5873(4) 0.8949(3) 0.9129(3) 0.0405(15) Uani 1 1 d . . . O5' O 0.4198(4) 0.8008(3) 0.8911(4) 0.0516(18) Uani 1 1 d . . . O6' O 0.5734(4) 0.6264(3) 0.7522(3) 0.0521(17) Uani 1 1 d . . . O7' O 0.7275(4) 0.7346(2) 0.6430(3) 0.0376(15) Uani 1 1 d . . . O8' O 0.6610(5) 0.6485(3) 0.5697(3) 0.0571(18) Uani 1 1 d . . . O9' O 0.8992(4) 0.6002(2) 0.6417(3) 0.0347(14) Uani 1 1 d . . . H9' H 0.9256 0.5851 0.6014 0.052 Uiso 1 1 calc R . . O10' O 1.0949(7) 0.5959(3) 0.7298(4) 0.105(3) Uani 1 1 d . . . H10' H 1.1257 0.5866 0.7721 0.158 Uiso 1 1 calc R . . O11' O 1.1224(4) 0.8169(3) 1.0647(3) 0.0448(15) Uani 1 1 d . . . H11' H 1.1767 0.8233 1.0855 0.067 Uiso 1 1 calc R . . C9' C 0.8801(6) 0.7241(4) 1.0449(4) 0.032(2) Uani 1 1 d . . . C1' C 0.9433(6) 0.7635(3) 1.0029(4) 0.030(2) Uani 1 1 d . . . C2' C 0.9004(6) 0.8216(4) 0.9655(4) 0.028(2) Uani 1 1 d . . . C3' C 0.8023(5) 0.8354(3) 0.9661(4) 0.0188(16) Uiso 1 1 d . . . C4' C 0.7384(5) 0.7926(4) 1.0035(4) 0.026(2) Uani 1 1 d . . . C8' C 0.7767(5) 0.7369(4) 1.0459(4) 0.024(2) Uani 1 1 d . . . C7' C 0.7144(6) 0.6898(4) 1.0862(4) 0.034(2) Uani 1 1 d . . . C6' C 0.6128(7) 0.6965(4) 1.0772(4) 0.039(2) Uani 1 1 d . . . C5' C 0.5769(6) 0.7489(4) 1.0332(5) 0.036(2) Uani 1 1 d . . . C10' C 0.6340(5) 0.7989(3) 0.9986(4) 0.023(2) Uani 1 1 d . . . C11' C 0.5706(6) 0.8447(4) 0.9554(5) 0.037(2) Uani 1 1 d . . . C12' C 0.4654(6) 0.8182(4) 0.9654(5) 0.043(2) Uani 1 1 d . . . C13' C 0.3995(6) 0.8676(4) 1.0047(5) 0.036(2) Uani 1 1 d . . . H13D' H 0.4254 0.8789 1.0582 0.054 Uiso 1 1 calc R . . H13E' H 0.3362 0.8478 1.0092 0.054 Uiso 1 1 calc R . . H13F' H 0.3946 0.9079 0.9720 0.054 Uiso 1 1 calc R . . C14' C 0.5453(7) 0.6433(5) 1.1146(6) 0.061(3) Uani 1 1 d . . . H14D' H 0.5838 0.6107 1.1449 0.091 Uiso 1 1 calc R . . H14E' H 0.5086 0.6208 1.0718 0.091 Uiso 1 1 calc R . . H14F' H 0.5016 0.6654 1.1506 0.091 Uiso 1 1 calc R . . C15' C 1.1206(6) 0.7616(4) 1.0298(5) 0.038(2) Uani 1 1 d . . . H15' H 1.1407 0.7826 0.9789 0.046 Uiso 1 1 calc R . . C16' C 1.2049(6) 0.7155(4) 1.0302(5) 0.033(2) Uani 1 1 d . . . H16' H 1.2492 0.7543 1.0304 0.039 Uiso 1 1 calc R . . C17' C 1.2426(6) 0.6929(4) 0.9622(6) 0.043(3) Uani 1 1 d . . . H17' H 1.2950 0.6634 0.9689 0.052 Uiso 1 1 calc R . . C18' C 1.2120(7) 0.7084(4) 0.8775(6) 0.043(2) Uani 1 1 d . . . H18' H 1.1714 0.7457 0.8697 0.052 Uiso 1 1 calc R . . C19' C 1.2355(6) 0.6758(5) 0.8128(6) 0.050(3) Uani 1 1 d . . . H19' H 1.2801 0.6406 0.8187 0.060 Uiso 1 1 calc R . . C20' C 1.1948(7) 0.6914(5) 0.7282(6) 0.063(3) Uani 1 1 d . . . H20' H 1.2326 0.6657 0.6891 0.076 Uiso 1 1 calc R . . C21' C 1.0896(6) 0.6672(4) 0.7207(4) 0.032(2) Uani 1 1 d . . . H21' H 1.0558 0.6850 0.7678 0.038 Uiso 1 1 calc R . . C22' C 1.0307(6) 0.6862(4) 0.6456(4) 0.036(2) Uani 1 1 d . . . H22' H 1.0358 0.7355 0.6410 0.043 Uiso 1 1 calc R . . C23' C 0.9197(6) 0.6704(4) 0.6492(4) 0.032(2) Uani 1 1 d . . . H23' H 0.8890 0.6921 0.6011 0.038 Uiso 1 1 calc R . . C24' C 0.8703(6) 0.6993(3) 0.7219(4) 0.030(2) Uani 1 1 d . . . H24' H 0.8919 0.6729 0.7698 0.036 Uiso 1 1 calc R . . C25' C 0.7575(6) 0.6889(4) 0.7102(4) 0.033(2) Uani 1 1 d . . . H25' H 0.7445 0.6420 0.6935 0.039 Uiso 1 1 calc R . . C26' C 0.6978(6) 0.7055(4) 0.7839(4) 0.037(2) Uani 1 1 d . . . H26' H 0.7090 0.7532 0.7977 0.044 Uiso 1 1 calc R . . C27' C 0.5903(6) 0.6969(4) 0.7627(4) 0.039(2) Uani 1 1 d . . . H27' H 0.5729 0.7214 0.7122 0.046 Uiso 1 1 calc R . . C28' C 0.5259(8) 0.7206(6) 0.8328(7) 0.073(4) Uani 1 1 d . . . H28' H 0.5240 0.6949 0.8803 0.088 Uiso 1 1 calc R . . C29' C 0.4756(8) 0.7744(6) 0.8267(7) 0.073(4) Uani 1 1 d . . . H29' H 0.4751 0.7979 0.7775 0.087 Uiso 1 1 calc R . . C30' C 1.2439(7) 0.6950(4) 1.1136(5) 0.066(3) Uani 1 1 d . . . H30D' H 1.2130 0.7215 1.1545 0.099 Uiso 1 1 calc R . . H30E' H 1.3129 0.7025 1.1171 0.099 Uiso 1 1 calc R . . H30F' H 1.2307 0.6479 1.1224 0.099 Uiso 1 1 calc R . . C31' C 1.2039(9) 0.7653(7) 0.7077(9) 0.142(8) Uani 1 1 d . . . H31D' H 1.1754 0.7735 0.6543 0.213 Uiso 1 1 calc R . . H31E' H 1.2714 0.7777 0.7085 0.213 Uiso 1 1 calc R . . H31F' H 1.1708 0.7918 0.7473 0.213 Uiso 1 1 calc R . . C32' C 1.0718(7) 0.6577(5) 0.5677(4) 0.052(3) Uani 1 1 d . . . H32D' H 1.0324 0.6723 0.5215 0.078 Uiso 1 1 calc R . . H32E' H 1.0718 0.6091 0.5702 0.078 Uiso 1 1 calc R . . H32F' H 1.1372 0.6736 0.5622 0.078 Uiso 1 1 calc R . . C33' C 0.8948(6) 0.7738(4) 0.7398(6) 0.052(2) Uani 1 1 d . . . H33D' H 0.9638 0.7786 0.7491 0.078 Uiso 1 1 calc R . . H33E' H 0.8619 0.7882 0.7875 0.078 Uiso 1 1 calc R . . H33F' H 0.8740 0.8012 0.6940 0.078 Uiso 1 1 calc R . . C34' C 0.7298(6) 0.6635(4) 0.8576(4) 0.040(2) Uani 1 1 d . . . H34D' H 0.7988 0.6680 0.8669 0.061 Uiso 1 1 calc R . . H34E' H 0.7139 0.6168 0.8477 0.061 Uiso 1 1 calc R . . H34F' H 0.6968 0.6791 0.9048 0.061 Uiso 1 1 calc R . . C35' C 0.6817(6) 0.7075(5) 0.5772(5) 0.041(2) Uani 1 1 d . . . C36' C 0.6615(10) 0.7609(6) 0.5129(7) 0.109(5) Uani 1 1 d . . . H36A' H 0.6805 0.8045 0.5340 0.163 Uiso 1 1 calc R . . H36B' H 0.5932 0.7613 0.4985 0.163 Uiso 1 1 calc R . . H36C' H 0.6978 0.7509 0.4653 0.163 Uiso 1 1 calc R . . C37' C 0.4837(7) 0.6110(5) 0.7105(5) 0.058(3) Uani 1 1 d . . . H37A' H 0.4800 0.5631 0.7004 0.087 Uiso 1 1 calc R . . H37B' H 0.4799 0.6349 0.6594 0.087 Uiso 1 1 calc R . . H37C' H 0.4307 0.6245 0.7434 0.087 Uiso 1 1 calc R . . N2' N 0.9442(5) 0.8742(3) 0.9203(3) 0.0266(16) Uani 1 1 d . . . C2A C 1.0382(6) 0.8864(4) 0.9027(4) 0.031(2) Uani 1 1 d . . . H2A' H 1.0869 0.8564 0.9200 0.038 Uiso 1 1 calc R . . C3A C 1.0604(6) 0.9423(4) 0.8600(4) 0.038(2) Uani 1 1 d . . . H3A' H 1.1250 0.9503 0.8479 0.046 Uiso 1 1 calc R . . C4A C 0.9884(8) 0.9896(4) 0.8330(4) 0.038(2) Uani 1 1 d . . . C5A C 0.8950(7) 0.9776(4) 0.8518(4) 0.039(2) Uani 1 1 d . . . H5A' H 0.8466 1.0081 0.8354 0.047 Uiso 1 1 calc R . . C6A C 0.8704(6) 0.9185(3) 0.8966(4) 0.026(2) Uani 1 1 d . . . C7A C 1.0164(7) 1.0524(4) 0.7862(4) 0.045(2) Uani 1 1 d . . . H7A1' H 1.0855 1.0526 0.7794 0.067 Uiso 1 1 calc R . . H7A2' H 0.9981 1.0919 0.8161 0.067 Uiso 1 1 calc R . . H7A3' H 0.9835 1.0523 0.7336 0.067 Uiso 1 1 calc R . . O1W O 0.7697(4) 0.6472(3) 1.3025(3) 0.0499(15) Uani 1 1 d . . . O2W O 1.0129(4) 1.1085(3) 1.0674(4) 0.0649(19) Uani 1 1 d . . . O3W O 0.6732(7) 1.0267(3) 0.8866(3) 0.099(3) Uani 1 1 d . . . O4W O 0.6065(5) 1.0779(3) 1.7375(3) 0.0577(17) Uani 1 1 d . . . O5W O 0.6692(5) 0.5760(3) 0.4284(3) 0.073(2) Uani 1 1 d . . . O6W O 0.5218(6) 0.6597(4) 1.3467(5) 0.083(2) Uani 0.91 1 d P . . O7W O 0.4771(6) 0.9685(5) 1.7882(5) 0.062(2) Uani 0.71 1 d P . . O8W O 0.2939(5) 0.9993(3) 1.8475(5) 0.080(2) Uani 1 1 d . . . O9W O 0.4601(10) 0.9417(7) 1.6154(8) 0.127(5) Uani 0.69 1 d P . . O10W O 0.4183(12) 1.0174(9) 1.6994(8) 0.093(5) Uani 0.50 1 d P . . O11W O 1.2608(13) 0.8657(7) 0.8303(9) 0.076(5) Uani 0.42 1 d P . . 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 N1 0.025(5) 0.025(3) 0.023(3) -0.003(3) -0.006(3) -0.005(3) N3 0.036(5) 0.023(4) 0.018(3) 0.005(3) 0.003(3) 0.009(3) O1 0.024(3) 0.031(3) 0.053(3) 0.013(3) -0.007(3) 0.000(2) O2 0.035(4) 0.030(3) 0.040(3) 0.020(3) -0.007(3) -0.010(2) O3 0.041(5) 0.030(3) 0.036(3) 0.008(2) 0.001(3) 0.001(3) O4 0.054(4) 0.027(3) 0.073(4) 0.028(3) 0.022(3) 0.015(3) O5 0.047(4) 0.064(4) 0.039(3) 0.012(3) 0.025(4) 0.021(3) O6 0.152(8) 0.060(5) 0.059(4) -0.031(3) -0.046(5) 0.069(5) O7 0.060(4) 0.027(3) 0.028(3) -0.008(3) 0.005(3) 0.009(3) O8 0.053(4) 0.038(4) 0.031(3) -0.008(3) 0.004(3) 0.002(3) O9 0.063(4) 0.023(3) 0.036(3) -0.010(2) 0.016(3) 0.003(3) O10 0.063(4) 0.026(3) 0.039(3) 0.000(2) 0.011(3) 0.004(3) O11 0.016(4) 0.161(7) 0.061(4) -0.085(5) 0.009(4) -0.011(4) C9 0.043(7) 0.021(5) 0.030(4) 0.013(4) -0.016(5) -0.013(4) C1 0.030(6) 0.031(5) 0.028(4) 0.001(4) 0.000(5) -0.001(4) C2 0.032(6) 0.015(4) 0.025(4) -0.006(4) -0.004(4) 0.002(4) C3 0.043(7) 0.019(5) 0.024(4) -0.005(4) -0.010(5) -0.013(4) C4 0.025(6) 0.020(5) 0.024(4) -0.009(3) -0.001(4) -0.007(4) C8 0.024(6) 0.018(4) 0.032(4) -0.007(3) -0.005(4) -0.002(4) C7 0.022(6) 0.038(5) 0.032(4) -0.007(4) -0.018(5) -0.011(5) C6 0.055(7) 0.015(5) 0.030(4) -0.006(4) -0.017(5) -0.001(4) C5 0.020(6) 0.042(6) 0.024(4) -0.010(4) 0.005(5) -0.012(5) C10 0.033(7) 0.030(5) 0.031(4) -0.011(4) -0.004(5) -0.002(5) C11 0.042(6) 0.026(5) 0.042(4) 0.000(4) 0.022(5) -0.004(5) C12 0.041(7) 0.029(5) 0.048(5) 0.005(4) 0.009(5) 0.007(4) C13 0.047(6) 0.046(6) 0.081(6) 0.008(5) 0.030(6) -0.012(5) C14 0.049(6) 0.034(5) 0.048(5) 0.012(4) -0.023(5) 0.003(4) C15 0.023(7) 0.051(6) 0.035(5) 0.021(5) 0.008(5) -0.010(5) C16 0.025(6) 0.011(4) 0.035(5) -0.001(3) 0.007(5) -0.003(3) C17 0.028(5) 0.034(5) 0.023(4) -0.002(3) 0.010(4) -0.005(4) C18 0.035(6) 0.032(5) 0.028(5) -0.001(3) 0.012(5) -0.001(4) C19 0.037(5) 0.038(5) 0.030(4) 0.004(3) 0.001(5) -0.004(4) C20 0.060(7) 0.031(5) 0.027(4) 0.007(3) -0.004(4) -0.008(4) C21 0.033(6) 0.024(5) 0.032(4) -0.008(3) 0.005(4) 0.004(4) C22 0.068(7) 0.018(4) 0.022(4) 0.006(3) 0.005(4) -0.002(4) C23 0.045(6) 0.027(5) 0.031(4) -0.002(3) 0.018(5) 0.001(4) C24 0.050(6) 0.035(5) 0.031(4) -0.006(4) 0.015(5) 0.002(4) C25 0.068(7) 0.025(4) 0.019(4) 0.000(3) 0.006(5) 0.003(4) C26 0.066(7) 0.030(5) 0.029(4) -0.006(4) 0.001(5) 0.001(4) C27 0.059(7) 0.054(7) 0.029(4) -0.001(4) 0.001(5) 0.031(5) C28 0.073(7) 0.050(6) 0.024(4) -0.001(4) 0.000(5) 0.030(6) C29 0.064(8) 0.076(8) 0.025(5) 0.016(5) 0.009(5) 0.039(7) C30 0.039(6) 0.039(5) 0.034(4) -0.001(4) 0.011(4) 0.000(4) C31 0.045(6) 0.041(5) 0.037(4) 0.005(4) 0.001(4) 0.006(4) C32 0.091(8) 0.045(6) 0.020(4) 0.002(4) 0.005(5) 0.011(5) C33 0.043(6) 0.047(6) 0.054(5) -0.009(4) 0.004(5) -0.013(4) C34 0.081(7) 0.045(5) 0.037(4) -0.002(4) 0.003(5) -0.021(5) C35 0.059(6) 0.032(6) 0.027(5) -0.010(4) -0.015(5) 0.006(5) C36 0.075(7) 0.029(5) 0.035(4) 0.008(4) 0.012(5) -0.002(4) C37 0.242(18) 0.193(15) 0.048(6) -0.054(8) -0.047(10) 0.183(15) N2 0.028(4) 0.020(4) 0.022(3) -0.002(3) 0.004(3) 0.000(3) C211 0.041(6) 0.028(5) 0.037(4) 0.011(3) -0.011(4) -0.002(4) C411 0.039(6) 0.033(5) 0.013(3) 0.001(3) 0.001(4) 0.015(4) C511 0.061(7) 0.015(4) 0.020(4) 0.012(3) 0.018(4) 0.001(4) C611 0.058(7) 0.014(4) 0.016(4) -0.002(3) 0.003(4) -0.008(5) C711 0.054(6) 0.035(5) 0.047(4) -0.004(4) 0.017(5) 0.000(4) N1' 0.008(4) 0.029(4) 0.042(3) -0.007(3) -0.004(4) 0.002(3) N3' 0.026(5) 0.035(4) 0.030(3) 0.000(3) 0.001(3) -0.005(3) O1' 0.053(4) 0.031(3) 0.043(3) 0.009(3) -0.006(3) 0.003(3) O2' 0.060(4) 0.036(3) 0.038(3) 0.005(3) 0.012(3) -0.003(3) O3' 0.013(4) 0.038(4) 0.073(4) -0.006(3) 0.018(3) -0.002(2) O4' 0.029(3) 0.034(4) 0.057(3) 0.000(3) -0.008(3) 0.000(3) O5' 0.028(4) 0.058(4) 0.069(4) -0.044(3) 0.002(4) -0.001(3) O6' 0.053(4) 0.046(4) 0.056(3) 0.003(3) -0.013(3) -0.028(3) O7' 0.040(4) 0.031(3) 0.041(3) 0.003(3) 0.001(3) 0.003(3) O8' 0.094(5) 0.047(4) 0.029(3) 0.000(3) -0.014(3) -0.005(4) O9' 0.056(4) 0.024(3) 0.025(2) -0.007(2) 0.008(3) 0.006(2) O10' 0.208(9) 0.040(4) 0.061(4) 0.018(3) -0.072(5) -0.037(5) O11' 0.034(4) 0.029(4) 0.070(3) -0.012(3) -0.020(3) 0.003(3) C9' 0.045(7) 0.018(5) 0.033(4) -0.003(4) -0.008(5) 0.006(4) C1' 0.032(6) 0.013(4) 0.043(4) 0.000(4) -0.017(5) -0.013(4) C2' 0.035(5) 0.024(5) 0.024(4) -0.006(4) 0.003(4) 0.001(4) C4' 0.026(5) 0.031(5) 0.020(3) -0.001(3) -0.008(4) -0.002(4) C8' 0.019(6) 0.036(5) 0.016(3) 0.002(4) 0.006(4) -0.010(4) C7' 0.041(6) 0.027(5) 0.033(4) -0.006(4) -0.004(5) 0.003(4) C6' 0.062(8) 0.022(5) 0.035(4) 0.007(4) 0.017(5) -0.008(5) C5' 0.037(6) 0.022(5) 0.050(5) -0.014(4) 0.005(5) -0.013(4) C10' 0.027(6) 0.021(5) 0.022(3) -0.004(3) 0.001(4) 0.009(4) C11' 0.030(6) 0.029(5) 0.053(5) -0.003(5) 0.000(5) -0.006(4) C12' 0.032(6) 0.038(6) 0.061(5) -0.024(5) 0.011(5) -0.002(5) C13' 0.031(5) 0.031(5) 0.045(4) -0.007(4) 0.006(4) -0.003(4) C14' 0.060(7) 0.048(6) 0.077(6) -0.003(5) 0.032(6) 0.008(5) C15' 0.057(7) 0.020(5) 0.036(4) -0.002(4) -0.013(5) 0.000(5) C16' 0.024(6) 0.013(4) 0.059(6) -0.003(4) -0.012(5) -0.006(4) C17' 0.029(6) 0.018(5) 0.082(7) 0.012(5) -0.025(6) 0.000(4) C18' 0.031(6) 0.030(5) 0.071(7) 0.018(5) 0.024(6) 0.005(4) C19' 0.027(6) 0.046(6) 0.078(7) 0.032(5) 0.003(6) 0.009(4) C20' 0.059(7) 0.067(7) 0.063(6) 0.045(5) 0.003(6) 0.018(5) C21' 0.029(5) 0.026(5) 0.041(4) 0.000(3) 0.014(4) -0.008(4) C22' 0.039(6) 0.034(5) 0.036(4) 0.003(4) 0.017(5) -0.005(4) C23' 0.049(6) 0.020(5) 0.027(4) 0.007(3) 0.006(4) 0.005(4) C24' 0.035(5) 0.024(4) 0.030(4) -0.003(3) 0.002(4) -0.008(4) C25' 0.049(6) 0.027(4) 0.021(4) 0.001(3) -0.010(4) -0.004(4) C26' 0.042(6) 0.026(5) 0.041(5) -0.018(4) -0.009(5) 0.000(4) C27' 0.045(6) 0.040(6) 0.031(4) -0.025(4) 0.007(5) 0.003(4) C28' 0.066(8) 0.058(8) 0.093(8) 0.000(6) -0.046(7) -0.023(6) C29' 0.079(8) 0.055(7) 0.080(8) -0.013(6) -0.041(7) -0.017(7) C30' 0.070(7) 0.047(6) 0.079(6) -0.031(5) -0.043(6) 0.028(5) C31' 0.098(10) 0.161(14) 0.160(12) 0.125(11) -0.089(10) -0.090(10) C32' 0.049(6) 0.071(6) 0.036(5) 0.015(5) 0.005(5) 0.017(5) C33' 0.028(5) 0.052(6) 0.076(6) -0.014(5) 0.005(5) -0.004(4) C34' 0.039(5) 0.053(5) 0.029(4) -0.011(4) 0.001(4) -0.008(4) C35' 0.035(6) 0.057(7) 0.030(5) 0.012(5) 0.003(5) 0.001(5) C36' 0.132(11) 0.091(9) 0.098(8) 0.047(7) -0.065(8) -0.027(8) C37' 0.060(7) 0.051(6) 0.063(5) -0.016(5) -0.011(6) -0.012(5) N2' 0.024(5) 0.024(4) 0.032(3) -0.007(3) 0.001(4) -0.001(4) C2A 0.026(6) 0.031(5) 0.036(4) 0.001(4) 0.002(4) -0.010(4) C3A 0.040(6) 0.041(6) 0.036(4) -0.011(4) 0.021(4) -0.014(5) C4A 0.071(8) 0.017(5) 0.026(4) 0.000(3) 0.010(5) -0.014(5) C5A 0.051(7) 0.040(6) 0.026(4) 0.000(4) 0.006(5) -0.004(5) C6A 0.041(6) 0.017(4) 0.020(4) -0.003(3) -0.006(4) 0.004(5) C7A 0.073(7) 0.038(5) 0.026(4) -0.004(4) 0.026(4) -0.017(5) O1W 0.054(4) 0.040(3) 0.055(3) -0.002(3) -0.007(3) 0.010(3) O2W 0.033(3) 0.043(4) 0.118(5) 0.015(3) -0.016(4) 0.000(3) O3W 0.224(10) 0.032(4) 0.042(3) -0.009(3) 0.013(4) 0.013(5) O4W 0.075(5) 0.051(4) 0.047(3) -0.006(3) -0.001(3) 0.015(3) O5W 0.103(6) 0.063(4) 0.051(3) 0.000(3) -0.009(4) 0.015(4) O6W 0.076(6) 0.082(6) 0.089(5) 0.027(4) -0.012(5) -0.019(4) O7W 0.053(6) 0.071(6) 0.061(5) -0.007(4) 0.011(5) 0.005(5) O8W 0.050(4) 0.060(5) 0.131(6) -0.009(4) 0.016(5) 0.000(3) O9W 0.119(11) 0.128(11) 0.129(10) -0.021(8) -0.053(9) 0.029(9) O10W 0.089(11) 0.116(13) 0.073(9) -0.015(9) 0.007(9) -0.020(10) O11W 0.099(13) 0.048(10) 0.077(10) -0.020(8) -0.037(10) 0.012(8) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C15 1.359(9) . ? N1 C1 1.417(10) . ? N3 C611 1.361(7) . ? N3 C3 1.410(9) . ? O1 C9 1.342(8) . ? O2 C7 1.280(9) . ? O3 C5 1.364(9) . ? O3 C12 1.464(9) . ? O4 C11 1.227(9) . ? O5 C29 1.361(12) . ? O5 C12 1.407(10) . ? O6 C27 1.430(11) . ? O6 C37 1.455(9) . ? O7 C35 1.336(10) . ? O7 C25 1.495(10) . ? O8 C35 1.221(9) . ? O9 C23 1.437(9) . ? O10 C21 1.446(8) . ? O11 C15 1.234(10) . ? C9 C1 1.393(11) . ? C9 C8 1.426(11) . ? C1 C2 1.409(11) . ? C2 C3 1.382(11) . ? C2 N2 1.402(7) . ? C3 C4 1.418(11) . ? C4 C10 1.388(11) . ? C4 C8 1.438(10) . ? C8 C7 1.456(10) . ? C7 C6 1.423(11) . ? C6 C5 1.373(11) . ? C6 C14 1.496(11) . ? C5 C10 1.415(11) . ? C10 C11 1.455(11) . ? C11 C12 1.539(12) . ? C12 C13 1.523(12) . ? C15 C16 1.488(11) . ? C16 C17 1.349(9) . ? C16 C30 1.498(11) . ? C17 C18 1.453(11) . ? C18 C19 1.310(10) . ? C19 C20 1.531(11) . ? C20 C31 1.520(11) . ? C20 C21 1.531(11) . ? C21 C22 1.558(11) . ? C22 C23 1.507(12) . ? C22 C32 1.532(10) . ? C23 C24 1.535(10) . ? C24 C25 1.519(12) . ? C24 C33 1.550(12) . ? C25 C26 1.547(10) . ? C26 C27 1.510(12) . ? C26 C34 1.550(12) . ? C27 C28 1.530(12) . ? C28 C29 1.313(13) . ? C35 C36 1.478(12) . ? N2 C611 1.3733 . ? N2 C211 1.3871 . ? C211 C311 1.3818 . ? C311 C411 1.3731 . ? C411 C511 1.3871 . ? C411 C711 1.4787 . ? C511 C611 1.3817 . ? N1' C15' 1.351(9) . ? N1' C1' 1.393(10) . ? N3' C6A 1.325(10) . ? N3' C3' 1.399(9) . ? O1' C9' 1.366(9) . ? O2' C7' 1.317(9) . ? O3' C5' 1.379(10) . ? O3' C12' 1.447(10) . ? O4' C11' 1.239(10) . ? O5' C12' 1.393(9) . ? O5' C29' 1.423(13) . ? O6' C27' 1.421(9) . ? O6' C37' 1.423(10) . ? O7' C35' 1.340(9) . ? O7' C25' 1.472(8) . ? O8' C35' 1.206(10) . ? O9' C23' 1.420(9) . ? O10' C21' 1.418(10) . ? O11' C15' 1.232(9) . ? C9' C1' 1.370(11) . ? C9' C8' 1.445(11) . ? C1' C2' 1.417(10) . ? C2' C3' 1.377(10) . ? C2' N2' 1.422(10) . ? C3' C4' 1.379(10) . ? C4' C8' 1.394(10) . ? C4' C10' 1.441(10) . ? C8' C7' 1.441(11) . ? C7' C6' 1.406(12) . ? C6' C5' 1.345(11) . ? C6' C14' 1.543(13) . ? C5' C10' 1.395(11) . ? C10' C11' 1.426(11) . ? C11' C12' 1.552(12) . ? C12' C13' 1.492(11) . ? C15' C16' 1.475(12) . ? C16' C17' 1.322(12) . ? C16' C30' 1.506(11) . ? C17' C18' 1.468(12) . ? C18' C19' 1.291(13) . ? C19' C20' 1.508(12) . ? C20' C31' 1.503(15) . ? C20' C21' 1.526(12) . ? C21' C22' 1.497(10) . ? C22' C32' 1.522(12) . ? C22' C23' 1.561(12) . ? C23' C24' 1.502(11) . ? C24' C33' 1.536(11) . ? C24' C25' 1.571(11) . ? C25' C26' 1.519(12) . ? C26' C27' 1.516(12) . ? C26' C34' 1.517(10) . ? C27' C28' 1.547(15) . ? C28' C29' 1.271(14) . ? C35' C36' 1.510(13) . ? N2' C2A 1.355(10) . ? N2' C6A 1.385(9) . ? C2A C3A 1.349(11) . ? C3A C4A 1.420(12) . ? C4A C5A 1.351(12) . ? C4A C7A 1.515(11) . ? C5A C6A 1.426(11) . ? 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 C15 N1 C1 119.6(6) . . ? C611 N3 C3 107.6(6) . . ? C5 O3 C12 109.4(6) . . ? C29 O5 C12 119.7(7) . . ? C27 O6 C37 110.4(8) . . ? C35 O7 C25 120.1(6) . . ? O1 C9 C1 117.9(8) . . ? O1 C9 C8 120.1(6) . . ? C1 C9 C8 122.0(7) . . ? C9 C1 C2 115.3(8) . . ? C9 C1 N1 122.3(7) . . ? C2 C1 N1 122.3(6) . . ? C3 C2 N2 105.7(6) . . ? C3 C2 C1 124.9(7) . . ? N2 C2 C1 129.4(7) . . ? C2 C3 N3 108.7(6) . . ? C2 C3 C4 120.5(7) . . ? N3 C3 C4 130.7(8) . . ? C10 C4 C3 126.1(7) . . ? C10 C4 C8 117.8(7) . . ? C3 C4 C8 115.9(7) . . ? C9 C8 C4 121.2(6) . . ? C9 C8 C7 118.2(7) . . ? C4 C8 C7 120.5(7) . . ? O2 C7 C6 119.6(7) . . ? O2 C7 C8 120.0(8) . . ? C6 C7 C8 120.2(7) . . ? C5 C6 C7 115.7(7) . . ? C5 C6 C14 123.6(9) . . ? C7 C6 C14 120.6(7) . . ? O3 C5 C6 121.4(7) . . ? O3 C5 C10 112.6(7) . . ? C6 C5 C10 126.0(9) . . ? C4 C10 C5 119.3(8) . . ? C4 C10 C11 133.1(7) . . ? C5 C10 C11 107.3(8) . . ? O4 C11 C10 130.1(8) . . ? O4 C11 C12 123.7(7) . . ? C10 C11 C12 106.2(7) . . ? O5 C12 O3 111.7(6) . . ? O5 C12 C13 106.1(8) . . ? O3 C12 C13 106.4(6) . . ? O5 C12 C11 114.3(6) . . ? O3 C12 C11 104.4(7) . . ? C13 C12 C11 113.7(7) . . ? O11 C15 N1 120.8(7) . . ? O11 C15 C16 124.3(7) . . ? N1 C15 C16 114.9(7) . . ? C17 C16 C15 118.4(6) . . ? C17 C16 C30 125.1(7) . . ? C15 C16 C30 116.5(6) . . ? C16 C17 C18 126.2(7) . . ? C19 C18 C17 125.7(8) . . ? C18 C19 C20 124.9(8) . . ? C31 C20 C19 108.8(7) . . ? C31 C20 C21 113.1(7) . . ? C19 C20 C21 111.0(6) . . ? O10 C21 C20 108.5(6) . . ? O10 C21 C22 107.0(6) . . ? C20 C21 C22 116.0(6) . . ? C23 C22 C32 111.5(6) . . ? C23 C22 C21 111.9(6) . . ? C32 C22 C21 111.8(6) . . ? O9 C23 C22 111.5(6) . . ? O9 C23 C24 109.3(6) . . ? C22 C23 C24 114.9(6) . . ? C25 C24 C23 111.8(6) . . ? C25 C24 C33 111.8(7) . . ? C23 C24 C33 112.5(6) . . ? O7 C25 C24 109.1(6) . . ? O7 C25 C26 107.0(6) . . ? C24 C25 C26 115.2(6) . . ? C27 C26 C25 113.3(6) . . ? C27 C26 C34 113.3(7) . . ? C25 C26 C34 109.1(7) . . ? O6 C27 C26 109.0(8) . . ? O6 C27 C28 111.4(6) . . ? C26 C27 C28 111.0(6) . . ? C29 C28 C27 122.3(8) . . ? C28 C29 O5 128.4(8) . . ? O8 C35 O7 122.4(8) . . ? O8 C35 C36 124.7(8) . . ? O7 C35 C36 112.9(7) . . ? C611 N2 C211 119.9 . . ? C611 N2 C2 109.5(4) . . ? C211 N2 C2 130.6(4) . . ? C311 C211 N2 120.5 . . ? C411 C311 C211 119.5 . . ? C311 C411 C511 119.9 . . ? C311 C411 C711 118.2 . . ? C511 C411 C711 121.7 . . ? C611 C511 C411 120.5 . . ? N3 C611 N2 108.3(3) . . ? N3 C611 C511 132.1(3) . . ? N2 C611 C511 119.5 . . ? C15' N1' C1' 127.7(6) . . ? C6A N3' C3' 109.2(6) . . ? C5' O3' C12' 109.7(6) . . ? C12' O5' C29' 120.0(6) . . ? C27' O6' C37' 113.8(6) . . ? C35' O7' C25' 118.0(6) . . ? O1' C9' C1' 118.0(7) . . ? O1' C9' C8' 118.8(7) . . ? C1' C9' C8' 123.1(6) . . ? C9' C1' N1' 118.0(6) . . ? C9' C1' C2' 114.6(7) . . ? N1' C1' C2' 127.0(7) . . ? C3' C2' C1' 123.4(7) . . ? C3' C2' N2' 106.9(6) . . ? C1' C2' N2' 129.7(7) . . ? C2' C3' C4' 121.4(7) . . ? C2' C3' N3' 107.6(7) . . ? C4' C3' N3' 131.0(7) . . ? C3' C4' C8' 118.0(7) . . ? C3' C4' C10' 124.9(6) . . ? C8' C4' C10' 117.1(7) . . ? C4' C8' C7' 121.2(7) . . ? C4' C8' C9' 119.2(7) . . ? C7' C8' C9' 119.5(7) . . ? O2' C7' C6' 119.8(8) . . ? O2' C7' C8' 120.4(7) . . ? C6' C7' C8' 119.7(7) . . ? C5' C6' C7' 118.3(8) . . ? C5' C6' C14' 121.4(8) . . ? C7' C6' C14' 120.2(7) . . ? C6' C5' O3' 123.7(8) . . ? C6' C5' C10' 124.2(7) . . ? O3' C5' C10' 112.1(7) . . ? C5' C10' C11' 107.9(7) . . ? C5' C10' C4' 119.3(6) . . ? C11' C10' C4' 132.4(7) . . ? O4' C11' C10' 131.6(8) . . ? O4' C11' C12' 121.4(7) . . ? C10' C11' C12' 106.9(7) . . ? O5' C12' O3' 110.1(6) . . ? O5' C12' C13' 106.0(6) . . ? O3' C12' C13' 110.8(7) . . ? O5' C12' C11' 112.6(7) . . ? O3' C12' C11' 103.4(6) . . ? C13' C12' C11' 114.0(6) . . ? O11' C15' N1' 120.0(7) . . ? O11' C15' C16' 122.8(7) . . ? N1' C15' C16' 117.1(7) . . ? C17' C16' C15' 122.4(7) . . ? C17' C16' C30' 122.4(7) . . ? C15' C16' C30' 115.2(8) . . ? C16' C17' C18' 128.1(8) . . ? C19' C18' C17' 126.8(8) . . ? C18' C19' C20' 123.8(9) . . ? C31' C20' C19' 111.9(9) . . ? C31' C20' C21' 111.9(7) . . ? C19' C20' C21' 109.3(7) . . ? O10' C21' C22' 111.1(6) . . ? O10' C21' C20' 104.9(7) . . ? C22' C21' C20' 118.2(6) . . ? C21' C22' C32' 113.0(7) . . ? C21' C22' C23' 114.9(6) . . ? C32' C22' C23' 110.5(6) . . ? O9' C23' C24' 110.2(6) . . ? O9' C23' C22' 112.6(6) . . ? C24' C23' C22' 115.0(6) . . ? C23' C24' C33' 114.4(7) . . ? C23' C24' C25' 109.0(5) . . ? C33' C24' C25' 110.9(6) . . ? O7' C25' C26' 108.5(6) . . ? O7' C25' C24' 105.1(6) . . ? C26' C25' C24' 115.7(5) . . ? C27' C26' C34' 112.0(7) . . ? C27' C26' C25' 110.1(6) . . ? C34' C26' C25' 111.4(6) . . ? O6' C27' C26' 106.9(6) . . ? O6' C27' C28' 106.9(7) . . ? C26' C27' C28' 112.0(6) . . ? C29' C28' C27' 121.3(11) . . ? C28' C29' O5' 123.6(11) . . ? O8' C35' O7' 124.8(7) . . ? O8' C35' C36' 124.5(8) . . ? O7' C35' C36' 110.6(9) . . ? C2A N2' C6A 121.6(7) . . ? C2A N2' C2' 131.6(6) . . ? C6A N2' C2' 106.7(7) . . ? C3A C2A N2' 119.3(7) . . ? C2A C3A C4A 122.2(8) . . ? C5A C4A C3A 118.2(7) . . ? C5A C4A C7A 121.2(8) . . ? C3A C4A C7A 120.6(9) . . ? C4A C5A C6A 120.3(8) . . ? N3' C6A N2' 109.5(6) . . ? N3' C6A C5A 132.0(7) . . ? N2' C6A C5A 118.4(8) . . ? _diffrn_measured_fraction_theta_max 0.863 _diffrn_reflns_theta_full 19.77 _diffrn_measured_fraction_theta_full 0.863 _refine_diff_density_max 0.781 _refine_diff_density_min -0.313 _refine_diff_density_rms 0.074 # Attachment '- delta_2w.cif' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # If this CIF has been generated directly or indirectly from an entry in the # Cambridge Structural Database, then it will include bibliographic, chemical, # crystal, experimental, refinement or atomic coordinate data resulting from # the CCDC's data processing and validation procedures. Files generated from # CSD entries are Copyright 2012 Cambridge Crystallographic Data Centre. They # may be used in bona fide research applications only, and may not be copied or # further disseminated in any form, whether machine-readable or not, except for # the purposes of generating routine backup copies on your local computer # system. # # Files arising from any other source may also contain material that is the # copyright of third parties, including the originator, and you should check # with the originator concerning the permitted uses of the information # contained in this CIF. # # For further information on the CCDC and the free tools enCIFer and Mercury # for validating and visualising CIF files, please visit www.ccdc.cam.ac.uk # ####################################################################### data_delta_2w _database_code_depnum_ccdc_archive 'CCDC 886515' #TrackingRef '- delta_2w.cif' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,-z _cell_length_a 13.7595(1) _cell_length_b 20.2557(1) _cell_length_c 16.3472(1) _cell_angle_alpha 90 _cell_angle_beta 106.706(1) _cell_angle_gamma 90 _cell_volume 4363.8 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z O1 O 1.0317 0.7146 0.1689 O2 O 0.193 0.6154 0.3028 O4 O 0.8141 0.593 -0.1889 O5 O 0.3894 0.0942 0.3237 N1 N 0.4258 0.803 -0.6471 N2 N 0.4985 0.9305 -0.5284 N3 N 0.6566 0.9532 -0.4811 O6 O 0.5957 0.7257 -0.6819 O7 O 0.7841 0.7058 -0.6557 O8 O 1.0354 0.8649 -0.4867 O9 O 0.8568 0.9779 -0.3979 O10 O 1.0595 0.9138 -0.3491 O11 O 0.9971 0.7099 -0.2276 O12 O 0.7677 0.7916 -0.1618 O13 O 0.8359 0.7044 -0.0935 O14 O 0.5539 0.6972 -0.2087 O15 O 0.4386 0.7098 -0.3964 O16 O 0.4348 0.7095 -0.5502 C1 C 0.6156 0.7875 -0.6254 C2 C 0.5298 0.8239 -0.6097 C3 C 0.557 0.8795 -0.5579 C4 C 0.655 0.8986 -0.5248 C5 C 0.8491 0.8827 -0.5021 C6 C 0.937 0.8386 -0.5227 C7 C 0.9204 0.782 -0.574 C8 C 0.8075 0.7621 -0.6119 C9 C 0.7135 0.8072 -0.5903 C10 C 0.7357 0.8626 -0.5396 C11 C 0.8945 0.9371 -0.4493 C12 C 1.0223 0.9312 -0.4351 C13 C 1.0725 1.006 -0.4447 C14 C 0.9955 0.7449 -0.5879 C15 C 0.3935 0.736 -0.627 C16 C 0.3054 0.7176 -0.6738 C17 C 0.229 0.7055 -0.6316 C18 C 0.2432 0.7027 -0.5416 C19 C 0.2244 0.7589 -0.4822 C20 C 0.2583 0.7583 -0.3926 C21 C 0.3754 0.7697 -0.3626 C22 C 0.4255 0.7846 -0.263 C23 C 0.5453 0.764 -0.2274 C24 C 0.6222 0.7828 -0.2897 C25 C 0.7302 0.7544 -0.2462 C26 C 0.8179 0.7637 -0.3102 C27 C 0.945 0.7761 -0.2535 C28 C 0.9964 0.8104 -0.3059 C29 C 1.0033 0.8739 -0.3092 C30 C 0.2863 0.7215 -0.7717 C31 C 0.2093 0.8057 -0.3598 C32 C 0.363 0.7602 -0.2089 C33 C 0.6245 0.8589 -0.309 C34 C 0.802 0.7081 -0.3854 C35 C 0.821 0.7598 -0.0932 C36 C 0.8735 0.8039 -0.0261 C37 C 1.055 0.7071 -0.1303 C38 C 0.3924 0.9381 -0.5421 C39 C 0.3599 0.9886 -0.5071 C40 C 0.4313 1.0394 -0.453 C41 C 0.5287 1.0291 -0.4417 C42 C 0.5626 0.9735 -0.4821 C43 C 0.3932 1.1003 -0.4179 H H 0.375216 0.833668 -0.686693 H H 0.552612 0.737511 -0.73996 H H 0.814691 0.66807 -0.618365 H H 0.52151 0.671479 -0.261172 H H 0.416472 0.708321 -0.459791 H H 1.04382 1.02301 -0.510451 H H 1.05116 1.04106 -0.402376 H H 1.15485 1.0021 -0.427456 H H 1.04304 0.725828 -0.5273 H H 0.962795 0.703866 -0.629834 H H 1.0413 0.775051 -0.617789 H H 0.152069 0.697618 -0.672484 H H 0.270335 0.655894 -0.51063 H H 0.181615 0.801887 -0.512825 H H 0.241321 0.710543 -0.369346 H H 0.383756 0.815998 -0.393766 H H 0.425704 0.838185 -0.257539 H H 0.573003 0.795048 -0.171109 H H 0.591472 0.759903 -0.352082 H H 0.726199 0.701629 -0.234849 H H 0.780305 0.763167 -0.285924 H H 0.786595 0.810306 -0.339359 H H 0.777088 0.747862 -0.265576 H H 0.948049 0.805259 -0.196849 H H 1.03176 0.781024 -0.345306 H H 0.95808 0.900843 -0.275484 H H 0.340717 0.690213 -0.790319 H H 0.209592 0.70469 -0.803666 H H 0.29515 0.772342 -0.790008 H H 0.127969 0.796225 -0.380423 H H 0.236482 0.804539 -0.29033 H H 0.224446 0.854066 -0.382539 H H 0.353439 0.706969 -0.216505 H H 0.400763 0.771705 -0.14225 H H 0.288944 0.784024 -0.228254 H H 0.652356 0.885879 -0.249194 H H 0.674536 0.867763 -0.348759 H H 0.548197 0.875657 -0.342387 H H 0.832251 0.660987 -0.35722 H H 0.7214 0.702846 -0.418067 H H 0.841758 0.723431 -0.431004 H H 0.818663 0.835028 -0.00781237 H H 0.916234 0.775315 0.0289203 H H 0.925365 0.834758 -0.0485875 H H 1.00166 0.714848 -0.0932364 H H 1.09091 0.658989 -0.114847 H H 1.11279 0.74551 -0.114973 H H 0.339105 0.902719 -0.580876 H H 0.278594 0.994318 -0.517226 H H 0.584255 1.06262 -0.401676 H H 0.347424 1.08541 -0.376673 H H 0.457589 1.1294 -0.381262 H H 0.347222 1.12983 -0.470554 N4 N 0.5735 0.4683 -0.1898 N5 N 0.5109 0.3205 -0.1289 N6 N 0.3252 0.3067 -0.1641 O17 O 0.4414 0.5353 -0.2892 O18 O 0.2564 0.592 -0.3679 O19 O 0.011 0.4777 -0.302 O20 O 0.1128 0.3201 -0.2035 O21 O -0.05 0.4283 -0.1771 O22 O 0.1444 0.5772 -0.0222 O23 O 0.2807 0.4451 0.1447 O24 O 0.2755 0.5191 0.2258 O25 O 0.4996 0.5682 0.1825 O26 O 0.676 0.5635 0.1138 O27 O 0.6229 0.4206 -0.2878 C44 C 0.4099 0.4814 -0.2645 C45 C 0.4767 0.4448 -0.2168 C46 C 0.4433 0.3869 -0.1923 C47 C 0.3456 0.3762 -0.2026 C48 C 0.1622 0.4212 -0.2635 C49 C 0.1007 0.4815 -0.3017 C50 C 0.1303 0.5303 -0.3325 C51 C 0.2184 0.5319 -0.3313 C52 C 0.3003 0.4679 -0.2903 C53 C 0.2668 0.419 -0.2602 C54 C 0.0994 0.3794 -0.2395 C55 C -0.0085 0.4145 -0.2627 C56 C -0.1026 0.3765 -0.3321 C57 C 0.0598 0.5914 -0.3722 C58 C 0.644 0.4512 -0.226 C59 C 0.7404 0.4836 -0.1927 C60 C 0.7997 0.4823 -0.1016 C61 C 0.7573 0.4944 -0.0229 C62 C 0.8119 0.4967 0.0585 C63 C 0.7772 0.4683 0.1279 C64 C 0.6747 0.4937 0.1227 C65 C 0.6214 0.4735 0.2007 C66 C 0.4996 0.5032 0.1813 C67 C 0.4359 0.483 0.1004 C68 C 0.3198 0.4969 0.088 C69 C 0.2603 0.4822 -0.003 C70 C 0.1485 0.5048 -0.023 C71 C 0.0904 0.4868 -0.0955 C72 C 0.0104 0.4625 -0.1131 C73 C 0.7904 0.5004 -0.269 C74 C 0.7911 0.3873 0.1459 C75 C 0.6928 0.4898 0.2962 C76 C 0.4536 0.4068 0.0759 C77 C 0.3141 0.508 -0.0656 C78 C 0.2446 0.466 0.2009 C79 C 0.1821 0.4345 0.2451 C80 C 0.0527 0.6008 0.006 C81 C 0.4738 0.207 -0.067 C82 C 0.4366 0.266 -0.1185 C83 C 0.6237 0.3129 -0.0864 C84 C 0.6557 0.2558 -0.0383 C85 C 0.5801 0.2004 -0.0278 C86 C 0.6232 0.1379 0.0241 H H 0.592104 0.500228 -0.139855 H H 0.490141 0.525033 -0.321949 H H 0.246605 0.631964 -0.335985 H H 0.529016 0.585166 0.137795 H H 0.694233 0.57487 0.060981 H H -0.081589 0.366711 -0.390292 H H -0.11848 0.330042 -0.304957 H H -0.169963 0.407616 -0.346949 H H 0.0302806 0.613507 -0.323475 H H 0.103959 0.627923 -0.395019 H H -0.00308833 0.574586 -0.425276 H H 0.880518 0.471984 -0.0874651 H H 0.67574 0.501523 -0.0365837 H H 0.885779 0.520738 0.0745473 H H 0.831585 0.485905 0.186222 H H 0.625471 0.468236 0.0675779 H H 0.614881 0.419907 0.198549 H H 0.47058 0.483138 0.231484 H H 0.459582 0.514294 0.055438 H H 0.310197 0.547993 0.104908 H H 0.256864 0.428798 -0.0110144 H H 0.121241 0.481359 0.0261831 H H 0.120462 0.495575 -0.149318 H H -0.0253168 0.469962 -0.0623851 H H 0.739819 0.532806 -0.315336 H H 0.863154 0.524853 -0.242475 H H 0.80175 0.454805 -0.300345 H H 0.871212 0.374464 0.161588 H H 0.761937 0.374037 0.198968 H H 0.749225 0.360521 0.0888945 H H 0.70915 0.542484 0.301761 H H 0.653651 0.475545 0.342672 H H 0.763548 0.462317 0.308301 H H 0.438674 0.373806 0.12349 H H 0.402229 0.395156 0.0133257 H H 0.53172 0.400541 0.0745195 H H 0.388286 0.484691 -0.0528231 H H 0.269126 0.496557 -0.130539 H H 0.323488 0.561263 -0.0583514 H H 0.221505 0.391624 0.279254 H H 0.165516 0.468972 0.290429 H H 0.11146 0.418804 0.199435 H H 0.0592425 0.582467 0.0699847 H H 0.0508678 0.654547 0.00621933 H H -0.0169123 0.582089 -0.0382451 H H 0.421269 0.169048 -0.0589042 H H 0.677606 0.35041 -0.0930789 H H 0.736371 0.249372 -0.00674837 H H 0.604015 0.0946765 -0.0170131 H H 0.705363 0.142105 0.0487976 H H 0.590615 0.132846 0.0771134 #END # Attachment '- epsilon_0.5w.cif' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # If this CIF has been generated directly or indirectly from an entry in the # Cambridge Structural Database, then it will include bibliographic, chemical, # crystal, experimental, refinement or atomic coordinate data resulting from # the CCDC's data processing and validation procedures. Files generated from # CSD entries are Copyright 2012 Cambridge Crystallographic Data Centre. They # may be used in bona fide research applications only, and may not be copied or # further disseminated in any form, whether machine-readable or not, except for # the purposes of generating routine backup copies on your local computer # system. # # Files arising from any other source may also contain material that is the # copyright of third parties, including the originator, and you should check # with the originator concerning the permitted uses of the information # contained in this CIF. # # For further information on the CCDC and the free tools enCIFer and Mercury # for validating and visualising CIF files, please visit www.ccdc.cam.ac.uk # ####################################################################### data_epsilon_0.5w _database_code_depnum_ccdc_archive 'CCDC 886516' #TrackingRef '- epsilon_0.5w.cif' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,-z _cell_length_a 13.479(22) _cell_length_b 20.635(34) _cell_length_c 16.002(26) _cell_angle_alpha 90.0 _cell_angle_beta 107.2207(15) _cell_angle_gamma 90.0 _cell_volume 4251.26 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z O4 O 0.8656 0.35354 0.44185 N1 N 1.0193 0.02813 1.56342 N2 N 0.90274 0.14828 1.48641 N3 N 0.73913 0.15738 1.44545 O5 O 0.89499 -0.06196 1.61878 O6 O 0.71876 -0.09234 1.63974 O7 O 0.41826 0.04248 1.49944 O8 O 0.52932 0.17615 1.41229 O9 O 0.34985 0.09899 1.34355 O10 O 0.40978 -0.08203 1.21374 O11 O 0.55233 0.01853 1.05842 O12 O 0.45987 -0.04664 0.95724 O13 O 0.75124 -0.10597 1.07461 O14 O 0.94634 -0.11657 1.12105 O15 O 0.97019 -0.07083 1.4838 C1 C 0.85216 -0.00307 1.58212 C2 C 0.91539 0.0421 1.55818 C3 C 0.86702 0.09916 1.52029 C4 C 0.76205 0.11057 1.50052 C5 C 0.58923 0.07941 1.5092 C6 C 0.52966 0.03116 1.53513 C7 C 0.56855 -0.02764 1.57916 C8 C 0.6737 -0.04005 1.59124 C9 C 0.74104 0.00931 1.56618 C10 C 0.69784 0.07011 1.53023 C11 C 0.51627 0.12312 1.44394 C12 C 0.40213 0.0995 1.43867 C13 C 0.34157 0.15007 1.47869 C14 C 0.50995 -0.06722 1.62803 C15 C 1.04214 -0.03045 1.51841 C16 C 1.15073 -0.0445 1.53026 C17 C 1.188 -0.04051 1.4544 C18 C 1.16194 0.01175 1.38397 C19 C 1.07749 0.01166 1.3071 C20 C 1.06824 -0.02769 1.2191 C21 C 0.94511 -0.05671 1.17412 C22 C 0.86256 -0.00909 1.11577 C23 C 0.75203 -0.03621 1.096 C24 C 0.7033 -0.02486 1.16674 C25 C 0.58172 -0.02469 1.1317 C26 C 0.5294 -0.00075 1.20029 C27 C 0.41401 -0.02013 1.1779 C28 C 0.35121 0.02933 1.21551 C29 C 0.39623 0.0666 1.28358 C30 C 1.20925 -0.07844 1.61978 C31 C 1.10338 0.01617 1.15309 C32 C 0.88703 0.00996 1.03097 C33 C 0.74623 0.03641 1.21796 C34 C 0.59077 -0.02086 1.29358 C35 C 0.52051 -0.00573 0.97827 C36 C 0.562 0.03197 0.91668 C37 C 0.30312 -0.09928 1.21337 C38 C 0.99888 0.16277 1.48895 C39 C 1.01528 0.21378 1.44526 C40 C 0.92996 0.25072 1.38665 C41 C 0.83957 0.23672 1.38973 C42 C 0.82264 0.18218 1.43595 C43 C 0.94748 0.29758 1.3208 H H 1.07763 0.0575977 1.59739 H H 0.951779 -0.0535683 1.67351 H H 0.682933 -0.132497 1.61241 H H 0.797782 -0.12975 1.12505 H H 0.988815 -0.150547 1.15927 H H 0.388179 0.162643 1.54474 H H 0.326379 0.193523 1.43827 H H 0.268231 0.12905 1.48077 H H 0.435867 -0.0823981 1.58318 H H 0.55541 -0.109814 1.656 H H 0.496201 -0.0380676 1.68024 H H 1.24015 -0.0788825 1.44685 H H 1.23062 0.0154358 1.36166 H H 1.15325 0.0560897 1.41804 H H 1.06705 0.0622437 1.287 H H 1.01141 -0.00427051 1.32781 H H 1.11966 -0.0695349 1.23479 H H 0.919951 -0.066018 1.2317 H H 0.866921 0.0350975 1.1539 H H 0.704615 -0.00944519 1.03962 H H 0.72399 -0.0654996 1.212 H H 0.556262 -0.0743534 1.11485 H H 0.530803 0.0519666 1.19766 H H 0.379303 -0.0205634 1.10719 H H 0.267755 0.0334231 1.18495 H H 0.479396 0.0739918 1.29637 H H 1.17185 -0.124491 1.62456 H H 1.2899 -0.0869714 1.62258 H H 1.20634 -0.0472532 1.67391 H H 1.18374 0.0310117 1.18234 H H 1.09687 -0.010952 1.09332 H H 1.05395 0.0589314 1.13773 H H 0.888545 -0.0333648 0.992507 H H 0.827428 0.0429255 0.993202 H H 0.962428 0.0337957 1.04721 H H 0.730223 0.0779056 1.17394 H H 0.709343 0.0436127 1.26929 H H 0.829789 0.0314773 1.24723 H H 0.668583 -0.000295976 1.31005 H H 0.551281 -0.00306526 1.33937 H H 0.596007 -0.073493 1.29754 H H 0.64655 0.0308084 0.938987 H H 0.534343 0.0107162 0.851602 H H 0.535462 0.081967 0.914392 H H 0.252082 -0.0991626 1.14637 H H 0.303391 -0.147342 1.24155 H H 0.275374 -0.0640335 1.25192 H H 1.06358 0.133108 1.52649 H H 1.09488 0.228954 1.453 H H 0.774252 0.267424 1.35607 H H 0.980357 0.272012 1.27566 H H 0.87379 0.319456 1.28453 H H 1.00102 0.335304 1.35439 N4 N 1.08809 0.23394 0.73441 N5 N 1.05005 0.08632 0.79066 N6 N 0.89583 0.05128 0.7905 O16 O 0.90386 0.29708 0.66999 O17 O 0.73448 0.31461 0.60222 O18 O 0.51969 0.16511 0.71063 O19 O 0.69759 0.04343 0.79254 O20 O 0.52949 0.1544 0.8272 O21 O 0.75188 0.25918 1.06282 O22 O 0.94765 0.1858 1.11654 O23 O 1.00648 0.2613 1.20913 O24 O 1.1487 0.29867 1.15894 O25 O 1.27993 0.32076 1.05673 O26 O 1.17937 0.15199 0.6794 C44 C 0.8961 0.23513 0.6937 C45 C 0.98744 0.19912 0.72299 C46 C 0.97593 0.1394 0.7539 C47 C 0.88243 0.11673 0.75424 C48 C 0.69413 0.13771 0.72488 C49 C 0.61045 0.18514 0.69522 C50 C 0.61474 0.23546 0.6576 C51 C 0.7104 0.25061 0.64236 C52 C 0.80084 0.20852 0.67538 C53 C 0.78861 0.15031 0.71208 C54 C 0.65949 0.08904 0.762 C55 C 0.5426 0.10548 0.76088 C56 C 0.46257 0.05471 0.71786 C57 C 0.52484 0.28051 0.62738 C58 C 1.17368 0.21241 0.70286 C59 C 1.26627 0.26139 0.71957 C60 C 1.3047 0.29457 0.79414 C61 C 1.39232 0.27328 0.87237 C62 C 1.40239 0.28906 0.9557 C63 C 1.38567 0.24155 1.02209 C64 C 1.28368 0.25658 1.04279 C65 C 1.26402 0.22241 1.11204 C66 C 1.15665 0.23363 1.11978 C67 C 1.06516 0.22612 1.03264 C68 C 0.95358 0.23557 1.05134 C69 C 0.85352 0.22625 0.96413 C70 C 0.74753 0.21722 0.98961 C71 C 0.64832 0.23513 0.91817 C72 C 0.60271 0.20692 0.85449 C73 C 1.30939 0.26783 0.64234 C74 C 1.38435 0.17681 0.9718 C75 C 1.34503 0.23325 1.19708 C76 C 1.07024 0.16108 0.98487 C77 C 0.84368 0.28321 0.89776 C78 C 0.97429 0.20218 1.2005 C79 C 0.94397 0.17026 1.28093 C80 C 0.65806 0.29236 1.05262 C81 C 1.04737 -0.02037 0.84031 C82 C 0.99783 0.0352 0.8099 C83 C 1.15997 0.0828 0.80634 C84 C 1.2066 0.02902 0.83733 C85 C 1.1534 -0.0235 0.85616 C86 C 1.20996 -0.08323 0.89045 H H 1.09767 0.276657 0.767288 H H 0.838667 0.0226781 0.799648 H H 0.935323 0.298341 0.621203 H H 0.727076 0.351522 0.639738 H H 1.16414 0.333109 1.12127 H H 1.28232 0.344628 1.00348 H H 0.465299 0.0459157 0.651474 H H 0.479387 0.00986997 0.755293 H H 0.385499 0.0718516 0.715891 H H 0.501085 0.296693 0.683348 H H 0.547312 0.322253 0.595474 H H 0.460408 0.255515 0.581228 H H 1.26936 0.34137 0.798769 H H 1.45223 0.242593 0.860066 H H 1.42372 0.338671 0.976641 H H 1.4431 0.241919 1.08637 H H 1.22257 0.239866 0.985725 H H 1.26769 0.171517 1.09519 H H 1.14697 0.19475 1.16272 H H 1.07372 0.264324 0.988334 H H 0.949796 0.285 1.07404 H H 0.867052 0.182045 0.931961 H H 0.743237 0.165704 1.0029 H H 0.614282 0.281399 0.92761 H H 0.621843 0.226773 0.798114 H H 1.24839 0.284796 0.585364 H H 1.37323 0.302448 0.658251 H H 1.33745 0.220862 0.628045 H H 1.45809 0.170768 0.957768 H H 1.37266 0.136494 1.01178 H H 1.32138 0.177886 0.910678 H H 1.34858 0.28461 1.21335 H H 1.32568 0.205629 1.24812 H H 1.42012 0.217445 1.192 H H 1.06596 0.120729 1.02753 H H 1.00532 0.158429 0.92519 H H 1.143 0.158563 0.968461 H H 0.913569 0.285517 0.876971 H H 0.776472 0.275109 0.841022 H H 0.834144 0.328685 0.929051 H H 0.970401 0.120141 1.28901 H H 0.980912 0.197264 1.34049 H H 0.859996 0.171686 1.26794 H H 0.595733 0.257498 1.04686 H H 0.665258 0.323241 1.1093 H H 0.640441 0.322069 0.993796 H H 1.00435 -0.0622765 0.852236 H H 1.20333 0.123963 0.792718 H H 1.29016 0.0252393 0.848805 H H 1.29381 -0.0854643 0.902877 H H 1.16808 -0.125318 0.903468 #END