Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Michel Ephritikhine' 'Lionel Salmon' 'Pierre Thuery' _publ_contact_author_name 'Dr Michel Ephritikhine' _publ_contact_author_address ; DSM/DRECAM/SCM CEA-Saclay Bat 125, P 28 Gif-sur-Yvette 91191 FRANCE ; _publ_contact_author_phone '33 (0) 1 69 08 64 36' _publ_contact_author_fax '33 (0) 1 69 08 66 40' _publ_contact_author_email ephri@drecam.cea.fr _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis and crystal structure of uranium(IV) complexes with compartmental Schiff bases: from mononuclear species to tri- and tetranuclear clusters ; data_2.thf _database_code_depnum_ccdc_archive 'CCDC 233078' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H44 N4 O9 U' _chemical_formula_weight 1058.90 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' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.8781(12) _cell_length_b 13.3968(8) _cell_length_c 14.9141(6) _cell_angle_alpha 90.00 _cell_angle_beta 110.327(3) _cell_angle_gamma 90.00 _cell_volume 4099.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13990 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 25.68 _exptl_crystal_description needle _exptl_crystal_colour 'translucent dark brown' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.716 _exptl_crystal_density_method ? _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 4.025 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.653 _exptl_absorpt_correction_T_max 0.803 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean 18 _diffrn_standards_decay_% none _diffrn_reflns_number 13990 _diffrn_reflns_av_R_equivalents 0.0652 _diffrn_reflns_av_sigmaI/netI 0.0545 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 25.68 _reflns_number_total 3766 _reflns_number_gt 3376 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by Patterson map interpretation and Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The tetrahydrofuran molecule is disordered around a symmetry centre and has been refined with restraints on bond lengths, angles and displacement parameters (the oxygen atom was not located). Some short contacts between this molecule and one of the aromatic rings of the Schiff base may be due to an imperfect description of the disorder or to the presence of CH...pi interactions. The H atoms were introduced at calculated positions (except in the disordered solvent molecule) as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH3) times that of the parent atom. The highest residual electron density peak is located near to the solvent molecule. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0535P)^2^+6.9692P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patter _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3766 _refine_ls_number_parameters 296 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.1014 _refine_ls_wR_factor_gt 0.0979 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.169 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 1.260 _refine_diff_density_min -1.009 _refine_diff_density_rms 0.153 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 U U 0.0000 0.28509(2) 0.7500 0.01886(12) Uani 1 2 d S . . N1 N 0.0666(2) 0.3495(4) 0.6485(3) 0.0227(10) Uani 1 1 d . . . N2 N -0.0277(2) 0.2111(4) 0.5790(4) 0.0227(10) Uani 1 1 d . . . O1 O 0.1587(2) 0.3960(4) 1.0187(3) 0.0314(10) Uani 1 1 d . . . O2 O 0.0799(2) 0.3867(3) 0.8383(3) 0.0232(9) Uani 1 1 d . . . O3 O -0.0711(2) 0.1613(3) 0.7279(3) 0.0240(9) Uani 1 1 d . . . O4 O -0.1110(2) 0.0076(3) 0.8233(3) 0.0290(10) Uani 1 1 d . . . C1 C 0.2014(4) 0.3963(6) 1.1163(4) 0.0357(16) Uani 1 1 d . . . H1A H 0.2274 0.3367 1.1293 0.054 Uiso 1 1 calc R . . H1B H 0.1761 0.3989 1.1576 0.054 Uiso 1 1 calc R . . H1C H 0.2294 0.4536 1.1277 0.054 Uiso 1 1 calc R . . C2 C 0.1875(3) 0.3905(5) 0.9508(4) 0.0275(13) Uani 1 1 d . . . C3 C 0.1424(3) 0.3849(4) 0.8548(4) 0.0222(12) Uani 1 1 d . . . C4 C 0.1695(3) 0.3784(4) 0.7806(4) 0.0267(13) Uani 1 1 d . . . C5 C 0.2376(3) 0.3802(5) 0.8025(5) 0.0294(14) Uani 1 1 d . . . H5 H 0.2546 0.3780 0.7534 0.035 Uiso 1 1 calc R . . C6 C 0.2787(3) 0.3853(5) 0.8951(5) 0.0344(15) Uani 1 1 d . . . H6 H 0.3235 0.3863 0.9086 0.041 Uiso 1 1 calc R . . C7 C 0.2542(3) 0.3889(5) 0.9705(5) 0.0323(15) Uani 1 1 d . . . H7 H 0.2827 0.3902 1.0335 0.039 Uiso 1 1 calc R . . C8 C 0.1285(3) 0.3703(5) 0.6815(4) 0.0250(13) Uani 1 1 d . . . H8 H 0.1484 0.3812 0.6364 0.030 Uiso 1 1 calc R . . C9 C 0.0344(3) 0.3464(4) 0.5474(4) 0.0210(12) Uani 1 1 d . . . C10 C 0.0488(3) 0.4123(4) 0.4851(4) 0.0242(13) Uani 1 1 d . . . H10 H 0.0809 0.4606 0.5089 0.029 Uiso 1 1 calc R . . C11 C 0.0148(3) 0.4056(5) 0.3874(4) 0.0280(13) Uani 1 1 d . . . H11 H 0.0251 0.4484 0.3456 0.034 Uiso 1 1 calc R . . C12 C -0.0345(3) 0.3351(5) 0.3516(4) 0.0294(14) Uani 1 1 d . . . H12 H -0.0574 0.3313 0.2862 0.035 Uiso 1 1 calc R . . C13 C -0.0493(3) 0.2705(5) 0.4142(5) 0.0276(14) Uani 1 1 d . . . H13 H -0.0826 0.2240 0.3905 0.033 Uiso 1 1 calc R . . C14 C -0.0147(3) 0.2748(4) 0.5122(4) 0.0238(13) Uani 1 1 d . . . C15 C -0.0460(3) 0.1210(5) 0.5531(4) 0.0252(13) Uani 1 1 d . . . H15 H -0.0467 0.1018 0.4929 0.030 Uiso 1 1 calc R . . C16 C -0.0658(3) 0.0464(4) 0.6079(4) 0.0221(12) Uani 1 1 d . . . C17 C -0.0788(3) 0.0703(5) 0.6921(4) 0.0228(12) Uani 1 1 d . . . C18 C -0.1003(3) -0.0083(5) 0.7380(4) 0.0258(13) Uani 1 1 d . . . C19 C -0.1051(3) -0.1041(5) 0.7044(4) 0.0298(14) Uani 1 1 d . . . H19 H -0.1184 -0.1545 0.7363 0.036 Uiso 1 1 calc R . . C20 C -0.0904(3) -0.1273(5) 0.6232(4) 0.0290(14) Uani 1 1 d . . . H20 H -0.0935 -0.1928 0.6017 0.035 Uiso 1 1 calc R . . C21 C -0.0714(3) -0.0533(5) 0.5751(4) 0.0263(13) Uani 1 1 d . . . H21 H -0.0622 -0.0688 0.5204 0.032 Uiso 1 1 calc R . . C22 C -0.1496(3) 0.0932(5) 0.8286(5) 0.0330(15) Uani 1 1 d . . . H22A H -0.1213 0.1476 0.8584 0.049 Uiso 1 1 calc R . . H22B H -0.1763 0.0767 0.8657 0.049 Uiso 1 1 calc R . . H22C H -0.1769 0.1123 0.7653 0.049 Uiso 1 1 calc R . . C23 C 0.2752(10) 0.1198(7) 0.5075(9) 0.068(5) Uani 0.50 1 d PDU . . C24 C 0.2959(12) 0.1359(12) 0.6168(9) 0.095(7) Uani 0.50 1 d PDU . . C25 C 0.2637(7) 0.2349(10) 0.6279(5) 0.043(2) Uani 0.50 1 d PDU . . C26 C 0.2374(7) 0.2800(6) 0.5345(5) 0.043(2) Uani 1 1 d DU . . 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 U 0.01879(18) 0.01939(17) 0.01815(18) 0.000 0.00611(12) 0.000 N1 0.025(3) 0.022(3) 0.021(2) 0.0004(19) 0.007(2) 0.002(2) N2 0.020(3) 0.026(3) 0.021(3) 0.001(2) 0.005(2) 0.000(2) O1 0.030(3) 0.043(3) 0.018(2) -0.0029(18) 0.0049(18) -0.001(2) O2 0.021(2) 0.024(2) 0.025(2) -0.0041(16) 0.0079(17) -0.0006(17) O3 0.023(2) 0.025(2) 0.025(2) -0.0015(17) 0.0089(17) -0.0034(18) O4 0.038(3) 0.030(2) 0.023(2) 0.0044(17) 0.0149(19) 0.002(2) C1 0.037(4) 0.046(4) 0.017(3) 0.002(3) -0.001(3) -0.005(3) C2 0.029(3) 0.025(3) 0.028(3) 0.000(2) 0.009(3) 0.002(3) C3 0.024(3) 0.014(3) 0.028(3) -0.003(2) 0.008(3) -0.002(2) C4 0.026(3) 0.022(3) 0.030(3) -0.002(2) 0.007(3) -0.002(2) C5 0.024(3) 0.034(4) 0.032(3) -0.002(3) 0.011(3) -0.001(3) C6 0.024(4) 0.036(4) 0.040(4) -0.001(3) 0.007(3) -0.003(3) C7 0.019(3) 0.037(4) 0.031(3) -0.001(3) -0.003(3) -0.001(3) C8 0.019(3) 0.025(3) 0.031(3) -0.002(2) 0.009(2) -0.003(2) C9 0.018(3) 0.021(3) 0.024(3) 0.001(2) 0.008(2) 0.003(2) C10 0.026(3) 0.020(3) 0.030(3) -0.002(2) 0.013(3) -0.004(2) C11 0.033(4) 0.027(3) 0.028(3) 0.004(2) 0.016(3) 0.003(3) C12 0.035(4) 0.033(4) 0.020(3) -0.001(2) 0.009(3) -0.005(3) C13 0.027(3) 0.028(4) 0.025(3) -0.003(2) 0.006(3) -0.011(3) C14 0.027(3) 0.025(3) 0.023(3) 0.001(2) 0.013(2) -0.001(3) C15 0.023(3) 0.034(4) 0.018(3) -0.003(2) 0.007(2) -0.003(3) C16 0.019(3) 0.025(3) 0.018(3) 0.002(2) 0.001(2) -0.001(2) C17 0.014(3) 0.027(3) 0.025(3) -0.002(2) 0.003(2) -0.002(2) C18 0.022(3) 0.031(3) 0.022(3) 0.003(2) 0.005(2) -0.001(3) C19 0.035(4) 0.024(3) 0.028(3) 0.005(2) 0.008(3) -0.002(3) C20 0.034(4) 0.020(3) 0.033(3) -0.001(2) 0.012(3) -0.002(3) C21 0.026(3) 0.028(3) 0.023(3) -0.003(2) 0.006(3) -0.001(3) C22 0.034(4) 0.035(4) 0.032(3) 0.006(3) 0.014(3) 0.004(3) C23 0.068(5) 0.068(5) 0.067(5) -0.0001(11) 0.024(2) -0.0007(11) C24 0.095(7) 0.095(7) 0.095(7) -0.0004(11) 0.033(3) 0.0000(11) C25 0.043(3) 0.043(3) 0.043(3) -0.0014(9) 0.0153(12) 0.0000(9) C26 0.042(3) 0.043(3) 0.043(3) -0.0018(9) 0.0152(12) 0.0002(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U O3 2.218(4) . ? U O3 2.218(4) 2_556 ? U O2 2.246(4) . ? U O2 2.246(4) 2_556 ? U N1 2.587(5) 2_556 ? U N1 2.587(5) . ? U N2 2.604(5) . ? U N2 2.604(5) 2_556 ? N1 C8 1.300(8) . ? N1 C9 1.427(7) . ? N1 N2 2.699(7) . ? N1 O2 2.787(6) . ? N2 C15 1.288(8) . ? N2 C14 1.414(8) . ? N2 O3 2.783(6) . ? O1 C2 1.369(8) . ? O1 C1 1.431(7) . ? O2 C3 1.303(7) . ? O2 O3 4.354(6) . ? O3 C17 1.318(7) . ? O4 C18 1.388(7) . ? O4 C22 1.442(8) . ? C2 C7 1.384(9) . ? C2 C3 1.431(9) . ? C3 C4 1.427(9) . ? C4 C5 1.410(9) . ? C4 C8 1.443(8) . ? C5 C6 1.363(9) . ? C6 C7 1.404(10) . ? C9 C10 1.394(8) . ? C9 C14 1.399(9) . ? C10 C11 1.391(9) . ? C11 C12 1.392(9) . ? C12 C13 1.392(9) . ? C13 C14 1.394(9) . ? C15 C16 1.448(8) . ? C16 C21 1.413(9) . ? C16 C17 1.418(8) . ? C17 C18 1.422(8) . ? C18 C19 1.369(9) . ? C19 C20 1.391(9) . ? C20 C21 1.370(9) . ? C23 C26 1.466(9) 7_556 ? C23 C24 1.547(9) . ? C24 C25 1.538(9) . ? C25 C26 1.443(8) . ? C26 C23 1.466(9) 7_556 ? C26 C26 1.550(9) 7_556 ? 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 O3 U O3 83.2(2) . 2_556 ? O3 U O2 154.56(15) . . ? O3 U O2 90.20(15) 2_556 . ? O3 U O2 90.20(15) . 2_556 ? O3 U O2 154.56(15) 2_556 2_556 ? O2 U O2 105.4(2) . 2_556 ? O3 U N1 80.09(15) . 2_556 ? O3 U N1 132.13(15) 2_556 2_556 ? O2 U N1 86.39(15) . 2_556 ? O2 U N1 70.04(15) 2_556 2_556 ? O3 U N1 132.13(15) . . ? O3 U N1 80.09(15) 2_556 . ? O2 U N1 70.04(15) . . ? O2 U N1 86.39(15) 2_556 . ? N1 U N1 141.0(2) 2_556 . ? O3 U N2 69.97(15) . . ? O3 U N2 76.92(15) 2_556 . ? O2 U N2 132.35(15) . . ? O2 U N2 77.74(15) 2_556 . ? N1 U N2 135.50(15) 2_556 . ? N1 U N2 62.65(15) . . ? O3 U N2 76.92(15) . 2_556 ? O3 U N2 69.97(15) 2_556 2_556 ? O2 U N2 77.74(15) . 2_556 ? O2 U N2 132.35(15) 2_556 2_556 ? N1 U N2 62.65(15) 2_556 2_556 ? N1 U N2 135.50(15) . 2_556 ? N2 U N2 135.3(2) . 2_556 ? C8 N1 C9 118.2(5) . . ? C15 N2 C14 118.2(5) . . ? C2 O1 C1 116.5(5) . . ? C18 O4 C22 117.4(5) . . ? O1 C2 C7 124.5(6) . . ? O1 C2 C3 114.1(5) . . ? C7 C2 C3 121.4(6) . . ? O2 C3 C4 123.1(5) . . ? O2 C3 C2 120.1(5) . . ? C4 C3 C2 116.8(6) . . ? C5 C4 C3 120.6(6) . . ? C5 C4 C8 118.0(6) . . ? C3 C4 C8 121.4(6) . . ? C6 C5 C4 120.5(6) . . ? C5 C6 C7 120.8(6) . . ? C2 C7 C6 119.9(6) . . ? N1 C8 C4 126.8(5) . . ? C10 C9 C14 120.4(5) . . ? C10 C9 N1 122.9(5) . . ? C14 C9 N1 116.7(5) . . ? C11 C10 C9 119.6(6) . . ? C12 C11 C10 120.5(5) . . ? C13 C12 C11 119.6(6) . . ? C12 C13 C14 120.6(6) . . ? C13 C14 C9 119.3(5) . . ? C13 C14 N2 123.0(5) . . ? C9 C14 N2 117.8(5) . . ? N2 C15 C16 126.9(5) . . ? C21 C16 C17 119.9(5) . . ? C21 C16 C15 117.7(5) . . ? C17 C16 C15 122.4(5) . . ? O3 C17 C16 122.0(5) . . ? O3 C17 C18 120.5(5) . . ? C16 C17 C18 117.5(5) . . ? C19 C18 O4 117.6(5) . . ? C19 C18 C17 120.9(6) . . ? O4 C18 C17 121.2(5) . . ? C18 C19 C20 121.1(6) . . ? C21 C20 C19 119.9(6) . . ? C20 C21 C16 120.6(6) . . ? C26 C23 C24 105.4(7) 7_556 . ? C23 C24 C25 104.8(6) . . ? C26 C25 C24 107.5(5) . . ? C25 C26 C23 138.4(9) . 7_556 ? C25 C26 C26 108.0(6) . 7_556 ? C23 C26 C26 104.4(6) 7_556 7_556 ? #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 233079' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H40 N4 O8 U' _chemical_formula_weight 1014.85 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' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 16.2340(9) _cell_length_b 15.5787(10) _cell_length_c 17.2083(10) _cell_angle_alpha 90.00 _cell_angle_beta 111.144(4) _cell_angle_gamma 90.00 _cell_volume 4059.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13741 _cell_measurement_theta_min 2.96 _cell_measurement_theta_max 25.68 _exptl_crystal_description parallelepipedic _exptl_crystal_colour 'translucent dark orange' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.661 _exptl_crystal_density_method ? _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 4.059 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.521 _exptl_absorpt_correction_T_max 0.666 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 13741 _diffrn_reflns_av_R_equivalents 0.0732 _diffrn_reflns_av_sigmaI/netI 0.0662 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 25.68 _reflns_number_total 3833 _reflns_number_gt 3235 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions as riding atoms with an isotropic displacement parameter equal to 1.2 (CH, CH2) or 1.5 (CH3) times that of the parent atom. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+3.9610P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3833 _refine_ls_number_parameters 269 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0670 _refine_ls_wR_factor_gt 0.0627 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.646 _refine_diff_density_min -1.051 _refine_diff_density_rms 0.103 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 U U 0.0000 0.527756(17) 0.2500 0.03022(9) Uani 1 2 d S . . O1 O 0.0689(2) 0.3082(2) 0.4356(2) 0.0430(8) Uani 1 1 d . . . O2 O -0.0194(2) 0.42532(19) 0.33014(19) 0.0340(7) Uani 1 1 d . . . O3 O 0.0852(2) 0.6311(2) 0.2308(2) 0.0357(7) Uani 1 1 d . . . O4 O 0.1774(2) 0.7508(2) 0.3294(2) 0.0403(8) Uani 1 1 d . . . N1 N -0.1590(2) 0.4684(3) 0.1871(2) 0.0325(8) Uani 1 1 d . . . N2 N -0.0708(2) 0.5916(2) 0.0963(2) 0.0336(9) Uani 1 1 d . . . C1 C 0.1294(3) 0.2442(3) 0.4811(3) 0.0470(13) Uani 1 1 d . . . H1A H 0.1034 0.2114 0.5136 0.071 Uiso 1 1 calc R . . H1B H 0.1825 0.2711 0.5174 0.071 Uiso 1 1 calc R . . H1C H 0.1431 0.2069 0.4430 0.071 Uiso 1 1 calc R . . C2 C -0.0066(3) 0.2809(3) 0.3746(3) 0.0365(11) Uani 1 1 d . . . C3 C -0.0530(3) 0.3472(3) 0.3190(3) 0.0351(11) Uani 1 1 d . . . C4 C -0.1332(3) 0.3277(3) 0.2546(3) 0.0358(11) Uani 1 1 d . . . C5 C -0.1663(4) 0.2427(3) 0.2469(3) 0.0419(12) Uani 1 1 d . . . H5 H -0.2202 0.2297 0.2054 0.050 Uiso 1 1 calc R . . C6 C -0.1196(4) 0.1792(3) 0.3001(3) 0.0488(14) Uani 1 1 d . . . H6 H -0.1412 0.1233 0.2937 0.059 Uiso 1 1 calc R . . C7 C -0.0397(4) 0.1986(3) 0.3637(3) 0.0434(13) Uani 1 1 d . . . H7 H -0.0083 0.1552 0.3992 0.052 Uiso 1 1 calc R . . C8 C -0.1853(3) 0.3923(3) 0.1968(3) 0.0350(11) Uani 1 1 d . . . H8 H -0.2428 0.3774 0.1638 0.042 Uiso 1 1 calc R . . C9 C -0.2228(3) 0.5227(3) 0.1232(3) 0.0358(10) Uani 1 1 d . . . H9A H -0.2140 0.5825 0.1398 0.043 Uiso 1 1 calc R . . H9B H -0.2827 0.5067 0.1169 0.043 Uiso 1 1 calc R . . C10 C -0.2090(3) 0.5102(3) 0.0415(3) 0.0339(11) Uani 1 1 d . . . C11 C -0.2697(3) 0.4651(3) -0.0229(3) 0.0385(11) Uani 1 1 d . . . H11 H -0.3217 0.4462 -0.0174 0.046 Uiso 1 1 calc R . . C12 C -0.2546(3) 0.4474(3) -0.0959(3) 0.0430(13) Uani 1 1 d . . . H12 H -0.2964 0.4173 -0.1389 0.052 Uiso 1 1 calc R . . C13 C -0.1780(3) 0.4746(3) -0.1045(3) 0.0399(11) Uani 1 1 d . . . H13 H -0.1668 0.4609 -0.1523 0.048 Uiso 1 1 calc R . . C14 C -0.1169(3) 0.5226(3) -0.0418(3) 0.0377(10) Uani 1 1 d . . . H14 H -0.0657 0.5421 -0.0485 0.045 Uiso 1 1 calc R . . C15 C -0.1322(3) 0.5416(3) 0.0315(3) 0.0346(11) Uani 1 1 d . . . C16 C -0.0525(3) 0.6663(3) 0.0740(3) 0.0360(11) Uani 1 1 d . . . H16 H -0.0795 0.6798 0.0178 0.043 Uiso 1 1 calc R . . C17 C 0.0049(3) 0.7312(3) 0.1260(3) 0.0358(11) Uani 1 1 d . . . C18 C 0.0692(3) 0.7108(3) 0.2029(3) 0.0323(11) Uani 1 1 d . . . C19 C 0.1198(3) 0.7781(3) 0.2547(3) 0.0372(11) Uani 1 1 d . . . C20 C 0.1059(3) 0.8621(3) 0.2269(3) 0.0419(12) Uani 1 1 d . . . H20 H 0.1391 0.9059 0.2604 0.050 Uiso 1 1 calc R . . C21 C 0.0424(4) 0.8820(3) 0.1489(3) 0.0458(13) Uani 1 1 d . . . H21 H 0.0335 0.9387 0.1310 0.055 Uiso 1 1 calc R . . C22 C -0.0065(3) 0.8179(3) 0.0992(3) 0.0423(12) Uani 1 1 d . . . H22 H -0.0477 0.8314 0.0470 0.051 Uiso 1 1 calc R . . C23 C 0.2290(4) 0.8150(3) 0.3858(3) 0.0500(14) Uani 1 1 d . . . H23A H 0.2649 0.8448 0.3607 0.075 Uiso 1 1 calc R . . H23B H 0.2663 0.7881 0.4365 0.075 Uiso 1 1 calc R . . H23C H 0.1904 0.8551 0.3979 0.075 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.02828(13) 0.02983(13) 0.03177(14) 0.000 0.00987(10) 0.000 O1 0.043(2) 0.0356(19) 0.045(2) 0.0019(16) 0.0089(17) 0.0037(16) O2 0.0357(18) 0.0319(17) 0.0335(17) -0.0002(14) 0.0112(15) -0.0015(14) O3 0.0305(17) 0.0323(17) 0.043(2) 0.0019(15) 0.0117(16) -0.0051(14) O4 0.0369(19) 0.0385(19) 0.041(2) -0.0054(15) 0.0089(16) -0.0072(15) N1 0.0335(19) 0.033(2) 0.0325(19) 0.0001(19) 0.0137(16) -0.0015(19) N2 0.029(2) 0.037(2) 0.032(2) 0.0009(18) 0.0085(18) 0.0018(18) C1 0.039(3) 0.045(3) 0.056(3) 0.013(3) 0.015(3) 0.006(2) C2 0.040(3) 0.034(3) 0.038(3) -0.001(2) 0.017(2) 0.000(2) C3 0.041(3) 0.036(3) 0.033(3) -0.004(2) 0.020(2) 0.001(2) C4 0.039(3) 0.041(3) 0.035(3) -0.004(2) 0.022(2) -0.008(2) C5 0.049(3) 0.039(3) 0.042(3) -0.006(2) 0.021(3) -0.011(2) C6 0.069(4) 0.031(3) 0.051(3) -0.004(2) 0.028(3) -0.008(3) C7 0.057(3) 0.034(3) 0.038(3) 0.003(2) 0.016(3) 0.000(3) C8 0.035(3) 0.043(3) 0.028(2) -0.002(2) 0.013(2) -0.003(2) C9 0.029(2) 0.038(3) 0.038(2) -0.001(2) 0.009(2) -0.003(2) C10 0.034(2) 0.033(3) 0.033(2) 0.001(2) 0.010(2) 0.003(2) C11 0.036(2) 0.037(3) 0.040(3) 0.000(2) 0.010(2) -0.004(2) C12 0.049(3) 0.039(3) 0.034(3) -0.006(2) 0.006(2) -0.003(2) C13 0.045(3) 0.040(3) 0.036(2) 0.000(2) 0.015(2) 0.004(3) C14 0.038(2) 0.035(2) 0.039(3) 0.005(2) 0.013(2) 0.006(2) C15 0.033(2) 0.032(3) 0.034(2) 0.004(2) 0.006(2) 0.005(2) C16 0.031(3) 0.040(3) 0.037(3) 0.006(2) 0.013(2) 0.006(2) C17 0.034(3) 0.038(3) 0.040(3) -0.001(2) 0.018(2) -0.001(2) C18 0.030(3) 0.030(3) 0.041(3) 0.002(2) 0.019(2) -0.004(2) C19 0.034(3) 0.042(3) 0.038(3) -0.003(2) 0.016(2) -0.009(2) C20 0.040(3) 0.035(3) 0.054(3) -0.007(2) 0.021(3) -0.010(2) C21 0.055(3) 0.031(3) 0.059(4) 0.007(2) 0.028(3) 0.002(2) C22 0.041(3) 0.043(3) 0.046(3) 0.012(2) 0.020(3) 0.005(2) C23 0.049(3) 0.052(3) 0.048(3) -0.012(3) 0.016(3) -0.020(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U O2 2.205(3) 6_556 ? U O2 2.205(3) . ? U O3 2.223(3) . ? U O3 2.223(3) 6_556 ? U N1 2.583(4) . ? U N1 2.583(4) 6_556 ? U N2 2.667(4) 6_556 ? U N2 2.667(4) . ? O1 C2 1.363(6) . ? O1 C1 1.419(6) . ? O1 O2 2.608(4) . ? O2 C3 1.319(5) . ? O2 N1 2.760(5) . ? O2 O3 4.263(4) . ? O3 C18 1.323(5) . ? O3 O4 2.601(4) . ? O3 N2 2.815(5) . ? O4 C19 1.357(6) . ? O4 C23 1.435(6) . ? N1 C8 1.291(6) . ? N1 C9 1.476(6) . ? N1 N2 3.129(5) . ? N2 C16 1.293(6) . ? N2 C15 1.428(6) . ? C2 C7 1.377(7) . ? C2 C3 1.424(7) . ? C3 C4 1.405(7) . ? C4 C5 1.417(6) . ? C4 C8 1.453(7) . ? C5 C6 1.375(7) . ? C6 C7 1.395(7) . ? C9 C10 1.514(6) . ? C10 C11 1.381(6) . ? C10 C15 1.407(6) . ? C11 C12 1.392(7) . ? C12 C13 1.372(7) . ? C13 C14 1.391(7) . ? C14 C15 1.401(6) . ? C16 C17 1.446(7) . ? C17 C18 1.396(7) . ? C17 C22 1.417(6) . ? C18 C19 1.427(6) . ? C19 C20 1.384(7) . ? C20 C21 1.400(7) . ? C21 C22 1.367(7) . ? 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 O2 U O2 87.26(16) 6_556 . ? O2 U O3 101.23(11) 6_556 . ? O2 U O3 148.63(11) . . ? O2 U O3 148.63(11) 6_556 6_556 ? O2 U O3 101.23(11) . 6_556 ? O3 U O3 87.17(16) . 6_556 ? O2 U N1 79.92(11) 6_556 . ? O2 U N1 69.90(11) . . ? O3 U N1 141.09(12) . . ? O3 U N1 74.98(12) 6_556 . ? O2 U N1 69.90(11) 6_556 6_556 ? O2 U N1 79.92(11) . 6_556 ? O3 U N1 74.98(12) . 6_556 ? O3 U N1 141.09(12) 6_556 6_556 ? N1 U N1 138.02(17) . 6_556 ? O2 U N2 141.49(11) 6_556 6_556 ? O2 U N2 75.96(11) . 6_556 ? O3 U N2 78.95(11) . 6_556 ? O3 U N2 69.61(11) 6_556 6_556 ? N1 U N2 123.87(11) . 6_556 ? N1 U N2 73.13(11) 6_556 6_556 ? O2 U N2 75.96(11) 6_556 . ? O2 U N2 141.49(11) . . ? O3 U N2 69.61(11) . . ? O3 U N2 78.95(11) 6_556 . ? N1 U N2 73.13(11) . . ? N1 U N2 123.87(11) 6_556 . ? N2 U N2 136.21(16) 6_556 . ? C2 O1 C1 117.2(4) . . ? C19 O4 C23 117.3(4) . . ? C8 N1 C9 116.6(4) . . ? C16 N2 C15 115.4(4) . . ? O1 C2 C7 126.5(5) . . ? O1 C2 C3 113.7(4) . . ? C7 C2 C3 119.9(5) . . ? O2 C3 C4 122.1(4) . . ? O2 C3 C2 118.8(4) . . ? C4 C3 C2 119.2(4) . . ? C3 C4 C5 119.2(5) . . ? C3 C4 C8 122.4(4) . . ? C5 C4 C8 118.4(5) . . ? C6 C5 C4 120.7(5) . . ? C5 C6 C7 120.0(5) . . ? C2 C7 C6 121.0(5) . . ? N1 C8 C4 125.9(4) . . ? N1 C9 C10 108.5(4) . . ? C11 C10 C15 119.1(4) . . ? C11 C10 C9 120.6(4) . . ? C15 C10 C9 120.3(4) . . ? C10 C11 C12 121.2(4) . . ? C13 C12 C11 119.8(5) . . ? C12 C13 C14 120.2(4) . . ? C13 C14 C15 120.2(4) . . ? C14 C15 C10 119.3(4) . . ? C14 C15 N2 121.2(4) . . ? C10 C15 N2 119.5(4) . . ? N2 C16 C17 127.7(4) . . ? C18 C17 C22 119.3(5) . . ? C18 C17 C16 121.5(4) . . ? C22 C17 C16 119.1(5) . . ? O3 C18 C17 122.7(4) . . ? O3 C18 C19 118.0(4) . . ? C17 C18 C19 119.4(4) . . ? O4 C19 C20 126.4(4) . . ? O4 C19 C18 114.0(4) . . ? C20 C19 C18 119.5(5) . . ? C19 C20 C21 120.8(5) . . ? C22 C21 C20 119.9(5) . . ? C21 C22 C17 121.0(5) . . ? #===END data_4.thf _database_code_depnum_ccdc_archive 'CCDC 233080' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H56 N4 O9 U' _chemical_formula_weight 1046.98 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' U U -9.6767 9.6646 '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/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.5520(8) _cell_length_b 30.4244(18) _cell_length_c 11.2771(5) _cell_angle_alpha 90.00 _cell_angle_beta 111.138(3) _cell_angle_gamma 90.00 _cell_volume 4336.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 29627 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent dark orange' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.604 _exptl_crystal_density_method ? _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 3.803 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.594 _exptl_absorpt_correction_T_max 0.925 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean 18 _diffrn_standards_decay_% none _diffrn_reflns_number 29627 _diffrn_reflns_av_R_equivalents 0.1093 _diffrn_reflns_av_sigmaI/netI 0.0941 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 25.68 _reflns_number_total 8193 _reflns_number_gt 5507 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions as riding atoms with an isotropic displacement parameter equal to 1.2 (CH, CH2) or 1.5 (CH3) times that of the parent atom. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0204P)^2^+1.3956P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8193 _refine_ls_number_parameters 549 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0868 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.0927 _refine_ls_wR_factor_gt 0.0803 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.503 _refine_diff_density_min -0.635 _refine_diff_density_rms 0.122 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 U U 0.81268(2) 0.138226(9) 0.20595(2) 0.02943(8) Uani 1 1 d . . . O1A O 0.4718(4) 0.16973(17) 0.1347(4) 0.0402(12) Uani 1 1 d . . . O2A O 0.6750(4) 0.18233(14) 0.1825(4) 0.0328(11) Uani 1 1 d . . . O3A O 0.9139(4) 0.08035(14) 0.2939(4) 0.0318(11) Uani 1 1 d . . . O4A O 0.9931(4) 0.04837(15) 0.5271(4) 0.0346(11) Uani 1 1 d . . . N1A N 0.8278(5) 0.20886(18) 0.0834(5) 0.0347(14) Uani 1 1 d . . . N2A N 0.9551(5) 0.12675(17) 0.1024(5) 0.0332(13) Uani 1 1 d . . . C1A C 0.3644(6) 0.1583(3) 0.1023(8) 0.053(2) Uani 1 1 d . . . H1A H 0.3234 0.1844 0.0978 0.080 Uiso 1 1 calc R . . H1B H 0.3571 0.1389 0.1658 0.080 Uiso 1 1 calc R . . H1C H 0.3397 0.1438 0.0213 0.080 Uiso 1 1 calc R . . C2A C 0.4974(6) 0.1967(2) 0.0512(6) 0.0373(17) Uani 1 1 d . . . C3A C 0.6068(6) 0.2022(2) 0.0807(6) 0.0324(16) Uani 1 1 d . . . C4A C 0.6397(6) 0.2293(2) 0.0011(6) 0.0332(16) Uani 1 1 d . . . C5A C 0.5643(6) 0.2505(2) -0.1035(6) 0.0397(18) Uani 1 1 d . . . H5A H 0.5868 0.2694 -0.1534 0.048 Uiso 1 1 calc R . . C6A C 0.4581(7) 0.2436(2) -0.1327(7) 0.0425(19) Uani 1 1 d . . . H6A H 0.4088 0.2571 -0.2033 0.051 Uiso 1 1 calc R . . C7A C 0.4246(7) 0.2160(3) -0.0549(7) 0.046(2) Uani 1 1 d . . . H7A H 0.3528 0.2107 -0.0752 0.055 Uiso 1 1 calc R . . C8A C 0.7523(6) 0.2347(2) 0.0201(6) 0.0336(16) Uani 1 1 d . . . H8A H 0.7705 0.2592 -0.0172 0.040 Uiso 1 1 calc R . . C9A C 0.9339(6) 0.2199(2) 0.0857(6) 0.0360(17) Uani 1 1 d . . . H9A H 0.9855 0.2124 0.1684 0.043 Uiso 1 1 calc R . . H9B H 0.9378 0.2513 0.0740 0.043 Uiso 1 1 calc R . . C10A C 0.9623(6) 0.1960(2) -0.0169(6) 0.0364(17) Uani 1 1 d . . . C11A C 0.9307(6) 0.1465(2) -0.0224(6) 0.0332(16) Uani 1 1 d . . . H11A H 0.8553 0.1438 -0.0697 0.040 Uiso 1 1 calc R . . H11B H 0.9674 0.1304 -0.0682 0.040 Uiso 1 1 calc R . . C12A C 1.0425(6) 0.1061(2) 0.1517(6) 0.0342(16) Uani 1 1 d . . . H12A H 1.0844 0.1039 0.1023 0.041 Uiso 1 1 calc R . . C13A C 1.0840(5) 0.0855(2) 0.2770(6) 0.0310(15) Uani 1 1 d . . . C14A C 1.0175(6) 0.0745(2) 0.3430(6) 0.0344(16) Uani 1 1 d . . . C15A C 1.0647(6) 0.0574(2) 0.4676(7) 0.0360(17) Uani 1 1 d . . . C16A C 1.1706(6) 0.0504(2) 0.5197(7) 0.0376(17) Uani 1 1 d . . . H16A H 1.1996 0.0388 0.6013 0.045 Uiso 1 1 calc R . . C17A C 1.2375(6) 0.0604(2) 0.4524(7) 0.0420(18) Uani 1 1 d . . . H17A H 1.3101 0.0559 0.4891 0.050 Uiso 1 1 calc R . . C18A C 1.1931(6) 0.0770(2) 0.3316(7) 0.0442(19) Uani 1 1 d . . . H18A H 1.2360 0.0827 0.2849 0.053 Uiso 1 1 calc R . . C19A C 1.0382(6) 0.0347(2) 0.6570(6) 0.0387(17) Uani 1 1 d . . . H19A H 1.0777 0.0081 0.6625 0.058 Uiso 1 1 calc R . . H19B H 0.9828 0.0297 0.6895 0.058 Uiso 1 1 calc R . . H19C H 1.0845 0.0573 0.7062 0.058 Uiso 1 1 calc R . . C20A C 1.0822(6) 0.2002(2) 0.0178(7) 0.0400(18) Uani 1 1 d . . . H20A H 1.1027 0.1852 -0.0446 0.060 Uiso 1 1 calc R . . H20B H 1.1181 0.1873 0.0999 0.060 Uiso 1 1 calc R . . H20C H 1.1010 0.2307 0.0200 0.060 Uiso 1 1 calc R . . C21A C 0.9024(6) 0.2156(2) -0.1490(6) 0.0386(18) Uani 1 1 d . . . H21A H 0.9235 0.2456 -0.1509 0.058 Uiso 1 1 calc R . . H21B H 0.8277 0.2144 -0.1664 0.058 Uiso 1 1 calc R . . H21C H 0.9185 0.1990 -0.2121 0.058 Uiso 1 1 calc R . . O1B O 0.6321(4) 0.14937(15) -0.2232(4) 0.0404(13) Uani 1 1 d . . . O2B O 0.7177(4) 0.11633(15) 0.0098(4) 0.0338(11) Uani 1 1 d . . . O3B O 0.9479(4) 0.17411(15) 0.3450(4) 0.0336(11) Uani 1 1 d . . . O4B O 1.1498(4) 0.18974(17) 0.3931(4) 0.0423(13) Uani 1 1 d . . . N1B N 0.6800(4) 0.07697(18) 0.2148(5) 0.0324(13) Uani 1 1 d . . . N2B N 0.7944(4) 0.13868(19) 0.4283(5) 0.0320(12) Uani 1 1 d . . . C1B C 0.5788(7) 0.1769(3) -0.3301(6) 0.048(2) Uani 1 1 d . . . H1D H 0.5458 0.1590 -0.4039 0.072 Uiso 1 1 calc R . . H1E H 0.6290 0.1963 -0.3452 0.072 Uiso 1 1 calc R . . H1F H 0.5258 0.1940 -0.3130 0.072 Uiso 1 1 calc R . . C2B C 0.5687(6) 0.1235(2) -0.1817(6) 0.0362(17) Uani 1 1 d . . . C3B C 0.6177(5) 0.1068(2) -0.0567(6) 0.0328(16) Uani 1 1 d . . . C4B C 0.5565(6) 0.0802(2) -0.0064(6) 0.0351(16) Uani 1 1 d . . . C5B C 0.4515(6) 0.0694(3) -0.0816(7) 0.0443(19) Uani 1 1 d . . . H5B H 0.4123 0.0510 -0.0495 0.053 Uiso 1 1 calc R . . C6B C 0.4073(6) 0.0860(3) -0.2021(7) 0.049(2) Uani 1 1 d . . . H6B H 0.3374 0.0792 -0.2507 0.059 Uiso 1 1 calc R . . C7B C 0.4648(6) 0.1128(2) -0.2529(6) 0.0390(18) Uani 1 1 d . . . H7B H 0.4336 0.1236 -0.3351 0.047 Uiso 1 1 calc R . . C8B C 0.5992(6) 0.0637(2) 0.1225(6) 0.0334(16) Uani 1 1 d . . . H8B H 0.5629 0.0402 0.1403 0.040 Uiso 1 1 calc R . . C9B C 0.7035(6) 0.0549(2) 0.3387(6) 0.0353(17) Uani 1 1 d . . . H9C H 0.7794 0.0514 0.3794 0.042 Uiso 1 1 calc R . . H9D H 0.6719 0.0259 0.3246 0.042 Uiso 1 1 calc R . . C10B C 0.6611(6) 0.0809(2) 0.4280(6) 0.0346(16) Uani 1 1 d . . . C11B C 0.6877(5) 0.1310(2) 0.4268(6) 0.0340(16) Uani 1 1 d . . . H11C H 0.6371 0.1444 0.3514 0.041 Uiso 1 1 calc R . . H11D H 0.6804 0.1450 0.5004 0.041 Uiso 1 1 calc R . . C12B C 0.8682(5) 0.1453(2) 0.5357(6) 0.0341(16) Uani 1 1 d . . . H12B H 0.8480 0.1445 0.6063 0.041 Uiso 1 1 calc R . . C13B C 0.9783(6) 0.1538(2) 0.5613(6) 0.0349(16) Uani 1 1 d . . . C14B C 1.0136(6) 0.1679(2) 0.4638(6) 0.0309(16) Uani 1 1 d . . . C15B C 1.1232(6) 0.1763(2) 0.4949(6) 0.0343(16) Uani 1 1 d . . . C16B C 1.1932(6) 0.1701(2) 0.6160(6) 0.0398(17) Uani 1 1 d . . . H16B H 1.2651 0.1748 0.6346 0.048 Uiso 1 1 calc R . . C17B C 1.1574(6) 0.1568(2) 0.7122(7) 0.0399(18) Uani 1 1 d . . . H17B H 1.2053 0.1532 0.7949 0.048 Uiso 1 1 calc R . . C18B C 1.0525(6) 0.1489(2) 0.6850(6) 0.0350(17) Uani 1 1 d . . . H18B H 1.0296 0.1401 0.7499 0.042 Uiso 1 1 calc R . . C19B C 1.2586(6) 0.1935(3) 0.4151(8) 0.058(2) Uani 1 1 d . . . H19D H 1.2903 0.2141 0.4827 0.087 Uiso 1 1 calc R . . H19E H 1.2677 0.2037 0.3391 0.087 Uiso 1 1 calc R . . H19F H 1.2919 0.1654 0.4383 0.087 Uiso 1 1 calc R . . C20B C 0.7150(7) 0.0625(2) 0.5623(7) 0.046(2) Uani 1 1 d . . . H20D H 0.6897 0.0778 0.6201 0.070 Uiso 1 1 calc R . . H20E H 0.7902 0.0663 0.5883 0.070 Uiso 1 1 calc R . . H20F H 0.6989 0.0318 0.5627 0.070 Uiso 1 1 calc R . . C21B C 0.5429(6) 0.0763(3) 0.3890(7) 0.0457(19) Uani 1 1 d . . . H21D H 0.5257 0.0465 0.4012 0.069 Uiso 1 1 calc R . . H21E H 0.5096 0.0841 0.3011 0.069 Uiso 1 1 calc R . . H21F H 0.5182 0.0955 0.4400 0.069 Uiso 1 1 calc R . . O1 O 0.2892(5) 0.04145(18) 0.0925(5) 0.0561(16) Uani 1 1 d . . . C1 C 0.3002(7) 0.0012(3) 0.1596(8) 0.052(2) Uani 1 1 d . . . H1G H 0.3228 0.0067 0.2503 0.063 Uiso 1 1 calc R . . H1H H 0.3524 -0.0173 0.1438 0.063 Uiso 1 1 calc R . . C2 C 0.1942(7) -0.0206(3) 0.1127(8) 0.054(2) Uani 1 1 d . . . H2G H 0.1537 -0.0131 0.1653 0.065 Uiso 1 1 calc R . . H2H H 0.2013 -0.0524 0.1114 0.065 Uiso 1 1 calc R . . C3 C 0.1425(9) -0.0022(3) -0.0221(9) 0.083(3) Uani 1 1 d U . . H3G H 0.1388 -0.0245 -0.0850 0.099 Uiso 1 1 calc R . . H3H H 0.0715 0.0082 -0.0361 0.099 Uiso 1 1 calc R . . C4 C 0.2106(7) 0.0342(3) -0.0294(7) 0.062(2) Uani 1 1 d U . . H4G H 0.2440 0.0272 -0.0901 0.074 Uiso 1 1 calc R . . H4H H 0.1686 0.0606 -0.0581 0.074 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.03021(13) 0.02906(12) 0.02906(12) 0.00121(14) 0.01072(9) 0.00048(15) O1A 0.032(3) 0.051(3) 0.037(3) 0.005(2) 0.012(2) 0.003(2) O2A 0.033(3) 0.032(2) 0.034(2) 0.006(2) 0.012(2) 0.005(2) O3A 0.033(3) 0.031(2) 0.027(2) 0.001(2) 0.006(2) -0.001(2) O4A 0.038(3) 0.034(3) 0.030(2) 0.004(2) 0.010(2) 0.004(2) N1A 0.039(4) 0.035(3) 0.033(3) -0.005(3) 0.015(3) -0.004(3) N2A 0.039(4) 0.031(3) 0.032(3) 0.000(2) 0.016(3) -0.003(3) C1A 0.031(5) 0.060(5) 0.061(5) -0.003(4) 0.006(4) -0.004(4) C2A 0.039(5) 0.039(4) 0.034(4) 0.002(3) 0.013(3) 0.001(3) C3A 0.036(4) 0.030(4) 0.035(4) -0.001(3) 0.018(3) 0.004(3) C4A 0.041(5) 0.028(3) 0.032(3) -0.002(3) 0.015(3) 0.003(3) C5A 0.054(5) 0.033(4) 0.037(4) -0.002(3) 0.023(4) 0.007(4) C6A 0.048(5) 0.042(4) 0.034(4) 0.004(3) 0.011(4) 0.014(4) C7A 0.040(5) 0.054(5) 0.044(4) -0.011(4) 0.015(4) 0.001(4) C8A 0.041(5) 0.031(4) 0.032(3) -0.004(3) 0.017(3) 0.002(3) C9A 0.044(5) 0.031(4) 0.036(4) -0.003(3) 0.019(3) -0.003(3) C10A 0.051(5) 0.030(4) 0.032(3) 0.003(3) 0.019(3) -0.004(3) C11A 0.040(4) 0.030(4) 0.034(3) -0.002(3) 0.020(3) 0.005(3) C12A 0.038(5) 0.031(4) 0.036(4) -0.005(3) 0.016(3) -0.006(3) C13A 0.029(4) 0.028(3) 0.035(3) 0.002(3) 0.010(3) 0.004(3) C14A 0.040(5) 0.028(4) 0.034(4) -0.003(3) 0.011(3) 0.003(3) C15A 0.034(4) 0.030(4) 0.040(4) -0.001(3) 0.009(3) 0.001(3) C16A 0.033(4) 0.036(4) 0.037(4) 0.003(3) 0.003(3) -0.005(3) C17A 0.030(4) 0.038(4) 0.051(4) 0.003(4) 0.007(4) 0.007(3) C18A 0.038(5) 0.039(4) 0.058(5) -0.008(4) 0.019(4) -0.002(4) C19A 0.040(5) 0.045(4) 0.028(3) 0.005(3) 0.009(3) 0.002(4) C20A 0.049(5) 0.035(4) 0.039(4) -0.001(3) 0.020(4) -0.003(4) C21A 0.055(5) 0.029(4) 0.036(4) -0.005(3) 0.021(4) -0.001(3) O1B 0.047(3) 0.043(3) 0.028(2) 0.006(2) 0.010(2) 0.001(2) O2B 0.034(3) 0.036(3) 0.032(2) -0.003(2) 0.013(2) -0.004(2) O3B 0.037(3) 0.035(3) 0.025(2) -0.002(2) 0.008(2) -0.004(2) O4B 0.033(3) 0.055(3) 0.040(3) -0.001(2) 0.014(2) -0.013(2) N1B 0.029(3) 0.034(3) 0.035(3) 0.005(3) 0.012(3) 0.004(3) N2B 0.038(3) 0.026(3) 0.035(3) -0.001(3) 0.017(2) 0.001(3) C1B 0.059(6) 0.052(5) 0.036(4) 0.009(4) 0.021(4) 0.011(4) C2B 0.038(4) 0.037(4) 0.030(3) 0.001(3) 0.009(3) 0.010(3) C3B 0.028(4) 0.034(4) 0.034(4) -0.009(3) 0.009(3) -0.002(3) C4B 0.034(4) 0.032(4) 0.037(4) 0.001(3) 0.011(3) 0.000(3) C5B 0.040(5) 0.054(5) 0.041(4) -0.005(4) 0.017(4) -0.010(4) C6B 0.038(5) 0.061(5) 0.044(4) -0.006(4) 0.009(4) -0.009(4) C7B 0.034(4) 0.051(4) 0.026(3) 0.001(3) 0.003(3) 0.005(4) C8B 0.033(4) 0.034(4) 0.038(4) 0.003(3) 0.019(3) -0.002(3) C9B 0.039(5) 0.032(4) 0.037(4) 0.003(3) 0.016(3) -0.005(3) C10B 0.030(4) 0.036(4) 0.039(4) -0.004(3) 0.015(3) -0.004(3) C11B 0.035(4) 0.034(4) 0.033(3) 0.005(3) 0.012(3) -0.004(3) C12B 0.037(4) 0.030(4) 0.034(3) 0.000(3) 0.012(3) 0.003(3) C13B 0.040(5) 0.031(4) 0.034(3) -0.003(3) 0.013(3) 0.002(3) C14B 0.036(4) 0.023(3) 0.035(4) -0.008(3) 0.014(3) 0.003(3) C15B 0.033(4) 0.029(4) 0.040(4) 0.000(3) 0.012(3) -0.001(3) C16B 0.034(4) 0.040(4) 0.042(4) -0.007(3) 0.009(3) -0.001(3) C17B 0.039(5) 0.041(4) 0.035(4) -0.005(3) 0.009(3) 0.000(3) C18B 0.047(5) 0.032(4) 0.030(3) -0.003(3) 0.017(3) 0.001(3) C19B 0.034(5) 0.087(7) 0.055(5) -0.001(5) 0.017(4) -0.021(5) C20B 0.055(6) 0.044(4) 0.041(4) 0.008(4) 0.019(4) -0.003(4) C21B 0.036(5) 0.049(5) 0.058(5) -0.001(4) 0.023(4) -0.012(4) O1 0.071(4) 0.058(4) 0.035(3) 0.003(3) 0.013(3) -0.016(3) C1 0.050(6) 0.053(5) 0.054(5) 0.000(4) 0.021(4) 0.003(4) C2 0.065(6) 0.046(5) 0.057(5) 0.005(4) 0.029(5) 0.001(4) C3 0.097(7) 0.075(6) 0.064(5) 0.007(5) 0.015(5) -0.030(5) C4 0.057(5) 0.081(6) 0.048(4) 0.001(4) 0.020(4) -0.015(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U O3B 2.222(4) . ? U O2B 2.222(4) . ? U O3A 2.232(4) . ? U O2A 2.236(4) . ? U N1A 2.603(6) . ? U N2B 2.606(5) . ? U N2A 2.615(6) . ? U N1B 2.616(6) . ? O1A C2A 1.383(8) . ? O1A C1A 1.411(9) . ? O2A C3A 1.332(8) . ? O2A N1A 2.804(7) . ? O2A O3A 4.331(6) . ? O3A C14A 1.323(8) . ? O3A N2A 2.800(7) . ? O4A C15A 1.391(9) . ? O4A C19A 1.430(7) . ? N1A C8A 1.284(9) . ? N1A C9A 1.467(9) . ? N1A N2A 3.000(8) . ? N2A C12A 1.278(9) . ? N2A C11A 1.455(8) . ? C2A C7A 1.378(10) . ? C2A C3A 1.408(10) . ? C3A C4A 1.404(9) . ? C4A C5A 1.408(9) . ? C4A C8A 1.472(10) . ? C5A C6A 1.373(11) . ? C6A C7A 1.403(10) . ? C9A C10A 1.528(9) . ? C10A C20A 1.534(10) . ? C10A C21A 1.537(9) . ? C10A C11A 1.559(9) . ? C12A C13A 1.460(9) . ? C13A C14A 1.401(9) . ? C13A C18A 1.406(10) . ? C14A C15A 1.415(9) . ? C15A C16A 1.358(10) . ? C16A C17A 1.409(10) . ? C17A C18A 1.372(10) . ? O1B C2B 1.367(9) . ? O1B C1B 1.432(8) . ? O2B C3B 1.323(8) . ? O2B N1B 2.809(7) . ? O2B O3B 4.313(6) . ? O3B C14B 1.328(8) . ? O3B N2B 2.789(7) . ? O4B C15B 1.383(8) . ? O4B C19B 1.410(9) . ? N1B C8B 1.275(8) . ? N1B C9B 1.477(8) . ? N1B N2B 3.005(8) . ? N2B C12B 1.278(8) . ? N2B C11B 1.459(8) . ? C2B C7B 1.384(10) . ? C2B C3B 1.417(9) . ? C3B C4B 1.417(9) . ? C4B C5B 1.408(10) . ? C4B C8B 1.447(9) . ? C5B C6B 1.369(10) . ? C6B C7B 1.387(10) . ? C9B C10B 1.544(9) . ? C10B C21B 1.507(10) . ? C10B C20B 1.531(9) . ? C10B C11B 1.566(9) . ? C12B C13B 1.438(10) . ? C13B C18B 1.403(9) . ? C13B C14B 1.415(9) . ? C14B C15B 1.420(10) . ? C15B C16B 1.367(9) . ? C16B C17B 1.399(10) . ? C17B C18B 1.364(10) . ? O1 C1 1.418(9) . ? O1 C4 1.420(9) . ? C1 C2 1.496(11) . ? C2 C3 1.533(12) . ? C3 C4 1.462(12) . ? 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 O3B U O2B 152.10(16) . . ? O3B U O3A 81.71(17) . . ? O2B U O3A 104.37(16) . . ? O3B U O2A 103.27(17) . . ? O2B U O2A 84.45(16) . . ? O3A U O2A 151.50(16) . . ? O3B U N1A 76.48(17) . . ? O2B U N1A 81.21(16) . . ? O3A U N1A 137.21(18) . . ? O2A U N1A 70.36(17) . . ? O3B U N2B 70.06(16) . . ? O2B U N2B 137.50(17) . . ? O3A U N2B 80.38(16) . . ? O2A U N2B 75.28(16) . . ? N1A U N2B 124.01(17) . . ? O3B U N2A 80.02(17) . . ? O2B U N2A 76.77(17) . . ? O3A U N2A 70.07(16) . . ? O2A U N2A 138.29(16) . . ? N1A U N2A 70.18(17) . . ? N2B U N2A 140.50(17) . . ? O3B U N1B 136.59(16) . . ? O2B U N1B 70.44(16) . . ? O3A U N1B 75.02(17) . . ? O2A U N1B 82.90(17) . . ? N1A U N1B 142.67(18) . . ? N2B U N1B 70.26(17) . . ? N2A U N1B 123.37(17) . . ? C2A O1A C1A 117.3(6) . . ? C3A O2A U 131.7(4) . . ? C15A O4A C19A 115.9(5) . . ? C8A N1A C9A 116.6(6) . . ? C8A N1A U 127.0(5) . . ? C9A N1A U 116.3(4) . . ? C12A N2A C11A 118.5(6) . . ? C12A N2A U 126.1(4) . . ? C11A N2A U 115.4(4) . . ? C7A C2A O1A 124.6(7) . . ? C7A C2A C3A 121.1(7) . . ? O1A C2A C3A 114.3(6) . . ? O2A C3A C4A 122.4(7) . . ? O2A C3A C2A 119.6(6) . . ? C4A C3A C2A 118.0(6) . . ? C3A C4A C5A 120.2(7) . . ? C3A C4A C8A 121.7(6) . . ? C5A C4A C8A 118.1(6) . . ? C6A C5A C4A 120.8(7) . . ? C5A C6A C7A 119.3(7) . . ? C2A C7A C6A 120.5(8) . . ? N1A C8A C4A 126.0(6) . . ? N1A C9A C10A 113.0(6) . . ? C9A C10A C20A 107.5(6) . . ? C9A C10A C21A 111.1(6) . . ? C20A C10A C21A 110.8(6) . . ? C9A C10A C11A 110.4(5) . . ? C20A C10A C11A 109.9(6) . . ? C21A C10A C11A 107.1(6) . . ? N2A C11A C10A 113.4(5) . . ? N2A C12A C13A 127.3(7) . . ? C14A C13A C18A 120.0(6) . . ? C14A C13A C12A 121.3(6) . . ? C18A C13A C12A 118.7(6) . . ? O3A C14A C13A 122.3(6) . . ? O3A C14A C15A 119.8(6) . . ? C13A C14A C15A 117.9(7) . . ? C16A C15A O4A 124.9(6) . . ? C16A C15A C14A 121.0(7) . . ? O4A C15A C14A 114.1(6) . . ? C15A C16A C17A 121.2(7) . . ? C18A C17A C16A 118.5(7) . . ? C17A C18A C13A 121.2(7) . . ? C2B O1B C1B 115.9(6) . . ? C3B O2B U 137.4(4) . . ? C15B O4B C19B 116.6(6) . . ? C8B N1B C9B 117.2(6) . . ? C12B N2B C11B 118.0(5) . . ? C12B N2B U 126.9(5) . . ? C11B N2B U 115.2(4) . . ? O1B C2B C7B 124.7(6) . . ? O1B C2B C3B 114.8(6) . . ? C7B C2B C3B 120.5(7) . . ? O2B C3B C4B 121.8(6) . . ? O2B C3B C2B 120.2(6) . . ? C4B C3B C2B 118.0(6) . . ? C5B C4B C3B 120.2(6) . . ? C5B C4B C8B 118.4(6) . . ? C3B C4B C8B 121.4(6) . . ? C6B C5B C4B 119.8(7) . . ? C5B C6B C7B 121.1(7) . . ? C2B C7B C6B 120.3(7) . . ? N1B C8B C4B 128.6(7) . . ? N1B C9B C10B 112.4(6) . . ? C21B C10B C20B 109.4(6) . . ? C21B C10B C9B 111.6(6) . . ? C20B C10B C9B 107.5(6) . . ? C21B C10B C11B 108.1(6) . . ? C20B C10B C11B 109.6(6) . . ? C9B C10B C11B 110.5(5) . . ? N2B C11B C10B 112.8(6) . . ? N2B C12B C13B 128.2(6) . . ? C18B C13B C14B 118.9(7) . . ? C18B C13B C12B 120.0(6) . . ? C14B C13B C12B 121.1(6) . . ? O3B C14B C13B 122.4(6) . . ? O3B C14B C15B 118.9(6) . . ? C13B C14B C15B 118.6(6) . . ? C16B C15B O4B 125.1(7) . . ? C16B C15B C14B 120.6(6) . . ? O4B C15B C14B 114.3(6) . . ? C15B C16B C17B 120.3(7) . . ? C18B C17B C16B 120.1(7) . . ? C17B C18B C13B 121.3(6) . . ? C1 O1 C4 106.3(6) . . ? O1 C1 C2 107.0(7) . . ? C1 C2 C3 103.0(7) . . ? C4 C3 C2 105.1(8) . . ? O1 C4 C3 109.3(7) . . ? #===END data_6.3thf _database_code_depnum_ccdc_archive 'CCDC 233081' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H76 N6 O19 U3' _chemical_formula_weight 2163.58 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' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7267(7) _cell_length_b 15.4321(10) _cell_length_c 19.6494(11) _cell_angle_alpha 75.846(5) _cell_angle_beta 87.788(5) _cell_angle_gamma 78.112(5) _cell_volume 3661.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 24724 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent dark brown' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.962 _exptl_crystal_density_method ? _exptl_crystal_F_000 2076 _exptl_absorpt_coefficient_mu 6.698 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.319 _exptl_absorpt_correction_T_max 0.751 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean 18 _diffrn_standards_decay_% none _diffrn_reflns_number 24724 _diffrn_reflns_av_R_equivalents 0.0720 _diffrn_reflns_av_sigmaI/netI 0.1099 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 25.68 _reflns_number_total 12772 _reflns_number_gt 8498 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The hydrogen atoms bound to O8 and O12 have not been found on the Fourier-difference map, nor introduced. All other hydrogen atoms were introduced at calculated positions as riding atoms with an isotropic displacement parameter equal to 1.2 (CH, CH2) or 1.5 (CH3) times that of the parent atom. A void of 57 A^3^ likely indicates the presence of an unresolved solvent molecule. The highest residual electron density peak is located at 0.97 A from U1. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12772 _refine_ls_number_parameters 994 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0937 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1027 _refine_ls_wR_factor_gt 0.0891 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.919 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.919 _refine_diff_density_max 1.181 _refine_diff_density_min -1.496 _refine_diff_density_rms 0.160 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 U1 U 0.03978(3) -0.18219(3) 0.20605(2) 0.03209(11) Uani 1 1 d . . . U2 U 0.21483(3) -0.01002(2) 0.183116(19) 0.03129(10) Uani 1 1 d . . . U3 U 0.33794(3) 0.15493(2) 0.262350(19) 0.03149(10) Uani 1 1 d . . . O1A O 0.0732(5) 0.1154(4) 0.1566(3) 0.0372(16) Uani 1 1 d . . . O2A O 0.0608(5) -0.0400(4) 0.1336(3) 0.0312(15) Uani 1 1 d . . . O3A O 0.2127(5) -0.1619(4) 0.1753(3) 0.0329(15) Uani 1 1 d . . . O4A O 0.3752(5) -0.1171(4) 0.2233(3) 0.0343(16) Uani 1 1 d . . . N1A N -0.0422(6) -0.1464(5) 0.0813(4) 0.0321(19) Uani 1 1 d . . . N2A N 0.1255(7) -0.2807(5) 0.1199(4) 0.035(2) Uani 1 1 d . . . C1A C -0.0156(8) 0.1151(7) 0.1202(5) 0.034(2) Uani 1 1 d . . . C2A C -0.0186(8) 0.0305(7) 0.1063(5) 0.034(2) Uani 1 1 d . . . C3A C -0.1007(8) 0.0198(6) 0.0647(5) 0.032(2) Uani 1 1 d . . . C4A C -0.1790(8) 0.0945(7) 0.0365(5) 0.034(2) Uani 1 1 d . . . H4A H -0.2308 0.0898 0.0063 0.041 Uiso 1 1 calc R . . C5A C -0.1806(7) 0.1777(7) 0.0534(5) 0.033(2) Uani 1 1 d . . . H5A H -0.2365 0.2270 0.0372 0.040 Uiso 1 1 calc R . . C6A C -0.0989(8) 0.1868(6) 0.0943(5) 0.030(2) Uani 1 1 d . . . H6A H -0.1007 0.2428 0.1045 0.036 Uiso 1 1 calc R . . C7A C -0.0962(7) -0.0677(7) 0.0467(5) 0.034(2) Uani 1 1 d . . . H7A H -0.1350 -0.0670 0.0074 0.041 Uiso 1 1 calc R . . C8A C -0.0381(8) -0.2249(6) 0.0531(5) 0.032(2) Uani 1 1 d . . . C9A C -0.1134(8) -0.2307(7) 0.0067(5) 0.038(2) Uani 1 1 d . . . H9A H -0.1735 -0.1840 -0.0055 0.046 Uiso 1 1 calc R . . C10A C -0.0996(9) -0.3055(7) -0.0216(5) 0.046(3) Uani 1 1 d . . . H10A H -0.1498 -0.3090 -0.0534 0.055 Uiso 1 1 calc R . . C11A C -0.0099(9) -0.3763(7) -0.0023(5) 0.041(3) Uani 1 1 d . . . H11A H 0.0013 -0.4262 -0.0221 0.049 Uiso 1 1 calc R . . C12A C 0.0622(8) -0.3707(7) 0.0470(5) 0.037(2) Uani 1 1 d . . . H12A H 0.1197 -0.4191 0.0622 0.044 Uiso 1 1 calc R . . C13A C 0.0501(8) -0.2955(6) 0.0736(5) 0.035(2) Uani 1 1 d . . . C14A C 0.2263(8) -0.3180(6) 0.1185(5) 0.036(2) Uani 1 1 d . . . H14A H 0.2447 -0.3595 0.0906 0.043 Uiso 1 1 calc R . . C15A C 0.3132(7) -0.3014(7) 0.1558(5) 0.034(2) Uani 1 1 d . . . C16A C 0.3049(7) -0.2228(6) 0.1801(5) 0.033(2) Uani 1 1 d . . . C17A C 0.3929(8) -0.2007(6) 0.2094(5) 0.033(2) Uani 1 1 d . . . C18A C 0.4867(8) -0.2656(6) 0.2193(5) 0.036(2) Uani 1 1 d . . . H18A H 0.5448 -0.2561 0.2417 0.043 Uiso 1 1 calc R . . C19A C 0.4960(8) -0.3459(7) 0.1960(5) 0.037(2) Uani 1 1 d . . . H19A H 0.5602 -0.3888 0.2037 0.044 Uiso 1 1 calc R . . C20A C 0.4130(8) -0.3624(6) 0.1624(5) 0.036(2) Uani 1 1 d . . . H20A H 0.4224 -0.4135 0.1440 0.043 Uiso 1 1 calc R . . O1B O 0.1079(5) -0.0758(4) 0.2725(3) 0.0322(15) Uani 1 1 d . . . O2B O 0.2096(5) 0.0593(4) 0.2842(3) 0.0328(15) Uani 1 1 d . . . O3B O 0.4498(5) 0.0293(4) 0.3096(3) 0.0364(16) Uani 1 1 d . . . O4B O 0.5513(5) -0.1431(4) 0.3079(3) 0.0409(17) Uani 1 1 d . . . N1B N 0.2143(7) 0.2001(5) 0.3583(4) 0.038(2) Uani 1 1 d . . . N2B N 0.4226(7) 0.1682(5) 0.3769(4) 0.0348(19) Uani 1 1 d . . . C1B C 0.0609(9) -0.0157(6) 0.3111(5) 0.036(2) Uani 1 1 d . . . C2B C 0.1152(7) 0.0523(6) 0.3194(5) 0.028(2) Uani 1 1 d . . . C3B C 0.0707(8) 0.1113(6) 0.3622(5) 0.035(2) Uani 1 1 d . . . C4B C -0.0271(8) 0.1043(7) 0.3937(5) 0.044(3) Uani 1 1 d . . . H4B H -0.0560 0.1424 0.4228 0.053 Uiso 1 1 calc R . . C5B C -0.0823(9) 0.0403(7) 0.3821(6) 0.050(3) Uani 1 1 d . . . H5B H -0.1494 0.0373 0.4019 0.060 Uiso 1 1 calc R . . C6B C -0.0375(9) -0.0192(7) 0.3409(5) 0.041(3) Uani 1 1 d . . . H6B H -0.0750 -0.0619 0.3336 0.050 Uiso 1 1 calc R . . C7B C 0.1230(8) 0.1776(7) 0.3794(5) 0.035(2) Uani 1 1 d . . . H7B H 0.0858 0.2093 0.4105 0.042 Uiso 1 1 calc R . . C8B C 0.2509(8) 0.2632(6) 0.3898(5) 0.033(2) Uani 1 1 d . . . C9B C 0.1866(9) 0.3389(7) 0.4070(5) 0.039(3) Uani 1 1 d . . . H9B H 0.1133 0.3524 0.3973 0.047 Uiso 1 1 calc R . . C10B C 0.2299(8) 0.3934(7) 0.4381(5) 0.041(3) Uani 1 1 d . . . H10B H 0.1866 0.4439 0.4498 0.049 Uiso 1 1 calc R . . C11B C 0.3402(9) 0.3726(7) 0.4520(5) 0.041(3) Uani 1 1 d . . . H11B H 0.3696 0.4085 0.4748 0.049 Uiso 1 1 calc R . . C12B C 0.4081(9) 0.2984(7) 0.4325(5) 0.043(3) Uani 1 1 d . . . H12B H 0.4818 0.2860 0.4406 0.052 Uiso 1 1 calc R . . C13B C 0.3612(8) 0.2446(6) 0.4007(5) 0.034(2) Uani 1 1 d . . . C14B C 0.4993(8) 0.1158(7) 0.4160(5) 0.038(2) Uani 1 1 d . . . H14B H 0.5177 0.1348 0.4546 0.046 Uiso 1 1 calc R . . C15B C 0.5605(8) 0.0299(7) 0.4063(5) 0.036(2) Uani 1 1 d . . . C16B C 0.5308(8) -0.0121(7) 0.3552(5) 0.036(2) Uani 1 1 d . . . C17B C 0.5845(8) -0.1000(7) 0.3540(5) 0.039(3) Uani 1 1 d . . . C18B C 0.6712(8) -0.1429(7) 0.3982(5) 0.038(2) Uani 1 1 d . . . H18B H 0.7090 -0.2004 0.3955 0.045 Uiso 1 1 calc R . . C19B C 0.7023(8) -0.1005(7) 0.4469(5) 0.043(3) Uani 1 1 d . . . H19B H 0.7613 -0.1292 0.4762 0.052 Uiso 1 1 calc R . . C20B C 0.6468(8) -0.0180(7) 0.4514(5) 0.037(2) Uani 1 1 d . . . H20B H 0.6664 0.0082 0.4857 0.044 Uiso 1 1 calc R . . O1C O 0.2775(5) 0.0177(4) 0.0745(3) 0.0347(16) Uani 1 1 d . . . O2C O 0.3473(5) 0.0943(4) 0.1643(3) 0.0329(15) Uani 1 1 d . . . O3C O 0.2070(5) 0.2566(4) 0.2054(3) 0.0357(16) Uani 1 1 d . . . O4C O -0.0110(5) 0.2819(5) 0.1954(4) 0.0414(17) Uani 1 1 d . . . N1C N 0.4989(6) 0.1999(5) 0.1887(4) 0.035(2) Uani 1 1 d . . . N2C N 0.3761(6) 0.3194(5) 0.2460(4) 0.0336(19) Uani 1 1 d . . . C1C C 0.3538(8) 0.0645(6) 0.0521(5) 0.032(2) Uani 1 1 d . . . C2C C 0.3936(8) 0.1063(6) 0.1006(5) 0.032(2) Uani 1 1 d . . . C3C C 0.4787(7) 0.1545(6) 0.0788(5) 0.030(2) Uani 1 1 d . . . C4C C 0.5146(8) 0.1656(6) 0.0104(5) 0.035(2) Uani 1 1 d . . . H4C H 0.5683 0.1986 -0.0039 0.042 Uiso 1 1 calc R . . C5C C 0.4719(8) 0.1283(7) -0.0371(5) 0.043(3) Uani 1 1 d . . . H5C H 0.4968 0.1365 -0.0829 0.051 Uiso 1 1 calc R . . C6C C 0.3926(8) 0.0792(7) -0.0162(5) 0.035(2) Uani 1 1 d . . . H6C H 0.3640 0.0551 -0.0486 0.042 Uiso 1 1 calc R . . C7C C 0.5250(8) 0.1953(6) 0.1254(5) 0.035(2) Uani 1 1 d . . . H7C H 0.5822 0.2225 0.1074 0.042 Uiso 1 1 calc R . . C8C C 0.5531(8) 0.2518(7) 0.2210(5) 0.037(2) Uani 1 1 d . . . C9C C 0.6655(8) 0.2411(7) 0.2229(6) 0.044(3) Uani 1 1 d . . . H9C H 0.7097 0.1979 0.2032 0.053 Uiso 1 1 calc R . . C10C C 0.7085(9) 0.2972(8) 0.2550(6) 0.050(3) Uani 1 1 d . . . H10C H 0.7827 0.2898 0.2580 0.061 Uiso 1 1 calc R . . C11C C 0.6436(9) 0.3635(8) 0.2826(6) 0.049(3) Uani 1 1 d . . . H11C H 0.6742 0.4020 0.3019 0.059 Uiso 1 1 calc R . . C12C C 0.5336(8) 0.3725(7) 0.2814(5) 0.042(3) Uani 1 1 d . . . H12C H 0.4902 0.4157 0.3015 0.050 Uiso 1 1 calc R . . C13C C 0.4875(7) 0.3175(7) 0.2505(5) 0.033(2) Uani 1 1 d . . . C14C C 0.3091(8) 0.3969(7) 0.2318(5) 0.037(2) Uani 1 1 d . . . H14C H 0.3362 0.4496 0.2267 0.044 Uiso 1 1 calc R . . C15C C 0.1943(8) 0.4065(6) 0.2233(5) 0.034(2) Uani 1 1 d . . . C16C C 0.1486(8) 0.3367(6) 0.2117(5) 0.035(2) Uani 1 1 d . . . C17C C 0.0366(8) 0.3511(6) 0.2049(5) 0.033(2) Uani 1 1 d . . . C18C C -0.0267(8) 0.4332(7) 0.2084(5) 0.043(3) Uani 1 1 d . . . H18C H -0.1008 0.4422 0.2034 0.051 Uiso 1 1 calc R . . C19C C 0.0194(9) 0.5035(7) 0.2195(5) 0.040(3) Uani 1 1 d . . . H19C H -0.0240 0.5585 0.2232 0.048 Uiso 1 1 calc R . . C20C C 0.1270(8) 0.4912(7) 0.2247(5) 0.039(3) Uani 1 1 d . . . H20C H 0.1575 0.5393 0.2294 0.047 Uiso 1 1 calc R . . O1 O -0.0900(5) -0.2679(4) 0.2038(3) 0.0340(16) Uani 1 1 d . . . O2 O -0.1266(5) -0.0908(4) 0.2150(3) 0.0373(16) Uani 1 1 d . . . C1 C -0.2286(8) -0.3240(7) 0.1657(6) 0.045(3) Uani 1 1 d . . . H1D H -0.1706 -0.3757 0.1691 0.068 Uiso 1 1 calc R . . H1E H -0.2552 -0.3028 0.1183 0.068 Uiso 1 1 calc R . . H1F H -0.2853 -0.3414 0.1964 0.068 Uiso 1 1 calc R . . C2 C -0.1893(8) -0.2494(7) 0.1867(5) 0.038(2) Uani 1 1 d . . . C3 C -0.2581(8) -0.1661(7) 0.1863(5) 0.041(3) Uani 1 1 d . . . H3D H -0.3301 -0.1591 0.1749 0.050 Uiso 1 1 calc R . . C4 C -0.2236(8) -0.0925(7) 0.2024(5) 0.038(2) Uani 1 1 d . . . C5 C -0.3036(8) -0.0039(7) 0.2019(6) 0.046(3) Uani 1 1 d . . . H5D H -0.3018 0.0104 0.2466 0.068 Uiso 1 1 calc R . . H5E H -0.3745 -0.0111 0.1928 0.068 Uiso 1 1 calc R . . H5F H -0.2848 0.0446 0.1658 0.068 Uiso 1 1 calc R . . O3 O -0.0124(5) -0.2213(4) 0.3279(3) 0.0344(16) Uani 1 1 d . . . O4 O 0.1544(5) -0.3115(4) 0.2694(3) 0.0383(17) Uani 1 1 d . . . C6 C -0.0212(9) -0.2491(8) 0.4502(6) 0.049(3) Uani 1 1 d . . . H6D H -0.0219 -0.1883 0.4544 0.073 Uiso 1 1 calc R . . H6E H 0.0158 -0.2924 0.4899 0.073 Uiso 1 1 calc R . . H6F H -0.0937 -0.2574 0.4484 0.073 Uiso 1 1 calc R . . C7 C 0.0347(8) -0.2632(7) 0.3848(5) 0.036(2) Uani 1 1 d . . . C8 C 0.1373(8) -0.3206(7) 0.3892(5) 0.039(3) Uani 1 1 d . . . H8D H 0.1697 -0.3443 0.4333 0.047 Uiso 1 1 calc R . . C9 C 0.1926(9) -0.3438(6) 0.3323(5) 0.038(2) Uani 1 1 d . . . C10 C 0.3004(8) -0.4059(7) 0.3416(5) 0.043(3) Uani 1 1 d . . . H10D H 0.2941 -0.4646 0.3357 0.064 Uiso 1 1 calc R . . H10E H 0.3278 -0.4125 0.3878 0.064 Uiso 1 1 calc R . . H10F H 0.3486 -0.3806 0.3073 0.064 Uiso 1 1 calc R . . O5 O 0.3407(7) 0.5243(6) 0.0297(5) 0.072(3) Uani 1 1 d . . . C11 C 0.3277(12) 0.5597(8) -0.0434(7) 0.074(4) Uani 1 1 d . . . H11D H 0.3928 0.5781 -0.0637 0.089 Uiso 1 1 calc R . . H11E H 0.2690 0.6123 -0.0538 0.089 Uiso 1 1 calc R . . C12 C 0.3037(11) 0.4839(7) -0.0732(6) 0.063(4) Uani 1 1 d . . . H12D H 0.2272 0.4852 -0.0738 0.076 Uiso 1 1 calc R . . H12E H 0.3315 0.4875 -0.1202 0.076 Uiso 1 1 calc R . . C13 C 0.3621(11) 0.4011(8) -0.0220(6) 0.061(3) Uani 1 1 d . . . H13D H 0.3292 0.3491 -0.0196 0.074 Uiso 1 1 calc R . . H13E H 0.4369 0.3859 -0.0347 0.074 Uiso 1 1 calc R . . C14 C 0.3518(10) 0.4288(9) 0.0458(6) 0.063(4) Uani 1 1 d . . . H14D H 0.2895 0.4111 0.0709 0.076 Uiso 1 1 calc R . . H44E H 0.4151 0.3996 0.0750 0.076 Uiso 1 1 calc R . . O6 O 0.3532(6) 0.7253(6) 0.4990(5) 0.067(2) Uani 1 1 d . . . C15 C 0.3821(9) 0.7670(8) 0.4286(6) 0.054(3) Uani 1 1 d . . . H15D H 0.3609 0.7363 0.3954 0.065 Uiso 1 1 calc R . . H15E H 0.4590 0.7636 0.4256 0.065 Uiso 1 1 calc R . . C16 C 0.3237(10) 0.8643(8) 0.4131(6) 0.057(3) Uani 1 1 d . . . H16D H 0.3049 0.8867 0.3636 0.068 Uiso 1 1 calc R . . H16E H 0.3672 0.9027 0.4260 0.068 Uiso 1 1 calc R . . C17 C 0.2236(9) 0.8626(7) 0.4577(6) 0.049(3) Uani 1 1 d . . . H17D H 0.1978 0.9204 0.4701 0.059 Uiso 1 1 calc R . . H17E H 0.1665 0.8477 0.4342 0.059 Uiso 1 1 calc R . . C18 C 0.2665(10) 0.7870(8) 0.5216(6) 0.056(3) Uani 1 1 d . . . H18D H 0.2918 0.8123 0.5569 0.067 Uiso 1 1 calc R . . H18E H 0.2102 0.7550 0.5418 0.067 Uiso 1 1 calc R . . O7 O 0.9071(10) 0.4531(7) 0.4406(6) 0.103(4) Uani 1 1 d . . . C19 C 0.9376(12) 0.5363(9) 0.4031(7) 0.078(4) Uani 1 1 d . . . H19D H 0.9868 0.5255 0.3657 0.094 Uiso 1 1 calc R . . H19E H 0.9720 0.5621 0.4345 0.094 Uiso 1 1 calc R . . C20 C 0.8349(11) 0.5993(9) 0.3736(7) 0.068(4) Uani 1 1 d . . . H20D H 0.8013 0.6325 0.4074 0.082 Uiso 1 1 calc R . . H20E H 0.8485 0.6430 0.3312 0.082 Uiso 1 1 calc R . . C21 C 0.7642(15) 0.5399(11) 0.3579(9) 0.113(7) Uani 1 1 d . . . H21D H 0.7680 0.5377 0.3089 0.135 Uiso 1 1 calc R . . H21E H 0.6900 0.5604 0.3697 0.135 Uiso 1 1 calc R . . C22 C 0.8131(14) 0.4488(10) 0.4054(8) 0.099(6) Uani 1 1 d . . . H22D H 0.7607 0.4295 0.4399 0.119 Uiso 1 1 calc R . . H22E H 0.8314 0.4037 0.3778 0.119 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.0317(2) 0.0325(2) 0.0319(2) -0.00837(17) -0.00058(16) -0.00545(17) U2 0.0304(2) 0.0317(2) 0.0316(2) -0.00846(17) -0.00106(16) -0.00474(16) U3 0.0306(2) 0.0316(2) 0.0316(2) -0.00752(17) -0.00127(16) -0.00465(17) O1A 0.037(4) 0.036(4) 0.040(4) -0.009(3) -0.007(3) -0.011(3) O2A 0.034(4) 0.029(4) 0.030(4) -0.004(3) 0.001(3) -0.009(3) O3A 0.029(4) 0.032(4) 0.034(4) -0.003(3) 0.002(3) -0.006(3) O4A 0.027(4) 0.032(4) 0.043(4) -0.016(3) -0.004(3) 0.004(3) N1A 0.028(4) 0.035(5) 0.033(5) -0.008(4) -0.001(4) -0.007(4) N2A 0.042(5) 0.033(5) 0.029(5) -0.007(4) -0.006(4) -0.008(4) C1A 0.039(6) 0.039(6) 0.032(6) -0.018(5) 0.001(5) -0.013(5) C2A 0.034(6) 0.036(6) 0.033(6) -0.006(5) -0.002(5) -0.008(5) C3A 0.035(6) 0.029(5) 0.036(6) -0.013(5) 0.003(5) -0.009(5) C4A 0.034(6) 0.042(6) 0.030(5) -0.010(5) -0.004(4) -0.012(5) C5A 0.027(5) 0.038(6) 0.036(6) -0.013(5) 0.000(4) -0.006(5) C6A 0.042(6) 0.022(5) 0.029(5) -0.008(4) 0.004(4) -0.013(4) C7A 0.024(5) 0.048(6) 0.032(5) -0.013(5) 0.004(4) -0.008(5) C8A 0.030(5) 0.032(5) 0.034(6) -0.011(5) -0.004(4) -0.002(4) C9A 0.037(6) 0.042(6) 0.036(6) -0.009(5) -0.004(5) -0.008(5) C10A 0.059(8) 0.046(7) 0.037(6) -0.005(5) -0.009(6) -0.023(6) C11A 0.049(7) 0.033(6) 0.035(6) -0.002(5) 0.001(5) -0.004(5) C12A 0.043(6) 0.034(6) 0.027(5) 0.003(5) 0.003(5) -0.010(5) C13A 0.040(6) 0.036(6) 0.031(5) -0.012(5) 0.000(5) -0.011(5) C14A 0.047(7) 0.027(5) 0.032(6) -0.002(4) 0.007(5) -0.008(5) C15A 0.023(5) 0.041(6) 0.033(6) -0.004(5) 0.001(4) 0.000(5) C16A 0.026(5) 0.028(5) 0.036(6) 0.000(5) 0.004(4) 0.006(4) C17A 0.026(5) 0.034(6) 0.036(6) -0.002(5) 0.006(4) -0.009(5) C18A 0.040(6) 0.034(6) 0.031(5) -0.001(5) -0.001(5) -0.010(5) C19A 0.026(5) 0.042(6) 0.043(6) -0.013(5) 0.011(5) -0.006(5) C20A 0.043(6) 0.032(5) 0.036(6) -0.013(5) 0.002(5) -0.010(5) O1B 0.031(4) 0.039(4) 0.031(4) -0.013(3) 0.005(3) -0.013(3) O2B 0.035(4) 0.032(4) 0.034(4) -0.011(3) -0.001(3) -0.008(3) O3B 0.042(4) 0.031(4) 0.029(4) 0.000(3) -0.008(3) 0.003(3) O4B 0.044(4) 0.039(4) 0.042(4) -0.016(4) -0.001(3) -0.004(3) N1B 0.040(5) 0.032(5) 0.036(5) -0.008(4) 0.000(4) 0.002(4) N2B 0.040(5) 0.030(4) 0.031(5) -0.004(4) 0.002(4) -0.005(4) C1B 0.047(7) 0.031(6) 0.032(6) -0.008(5) 0.005(5) -0.012(5) C2B 0.024(5) 0.031(5) 0.029(5) -0.006(4) 0.004(4) -0.007(4) C3B 0.034(6) 0.030(5) 0.039(6) -0.005(5) 0.003(5) -0.006(5) C4B 0.037(6) 0.056(7) 0.049(7) -0.024(6) 0.016(5) -0.021(5) C5B 0.042(7) 0.056(7) 0.057(7) -0.019(6) 0.018(6) -0.017(6) C6B 0.047(7) 0.042(6) 0.043(6) -0.022(5) -0.001(5) -0.013(5) C7B 0.038(6) 0.040(6) 0.022(5) -0.008(5) 0.004(4) 0.002(5) C8B 0.049(7) 0.028(5) 0.025(5) -0.005(4) -0.007(5) -0.015(5) C9B 0.046(7) 0.037(6) 0.038(6) -0.013(5) -0.001(5) -0.013(5) C10B 0.042(7) 0.041(6) 0.037(6) -0.008(5) 0.001(5) -0.008(5) C11B 0.055(7) 0.039(6) 0.030(6) -0.008(5) 0.002(5) -0.016(5) C12B 0.047(7) 0.034(6) 0.043(6) 0.001(5) -0.003(5) -0.007(5) C13B 0.041(6) 0.031(5) 0.030(5) -0.006(5) 0.000(5) -0.007(5) C14B 0.047(7) 0.043(6) 0.026(5) -0.010(5) 0.003(5) -0.011(5) C15B 0.037(6) 0.041(6) 0.025(5) 0.000(5) -0.004(5) -0.009(5) C16B 0.045(6) 0.035(6) 0.023(5) 0.001(5) 0.009(5) -0.005(5) C17B 0.035(6) 0.033(6) 0.047(6) -0.017(5) -0.006(5) 0.004(5) C18B 0.032(6) 0.039(6) 0.037(6) -0.005(5) 0.002(5) 0.002(5) C19B 0.037(6) 0.051(7) 0.042(6) -0.008(6) -0.009(5) -0.015(5) C20B 0.031(6) 0.041(6) 0.040(6) -0.014(5) 0.008(5) -0.004(5) O1C 0.040(4) 0.036(4) 0.031(4) -0.010(3) 0.000(3) -0.013(3) O2C 0.029(4) 0.036(4) 0.034(4) -0.010(3) 0.000(3) -0.004(3) O3C 0.037(4) 0.030(4) 0.036(4) -0.003(3) -0.006(3) -0.002(3) O4C 0.033(4) 0.044(4) 0.050(4) -0.017(4) -0.002(3) -0.009(3) N1C 0.029(5) 0.040(5) 0.030(5) 0.000(4) 0.002(4) -0.003(4) N2C 0.033(5) 0.036(5) 0.031(5) -0.009(4) -0.004(4) -0.002(4) C1C 0.032(6) 0.030(5) 0.033(6) -0.004(5) -0.004(5) -0.004(5) C2C 0.034(6) 0.029(5) 0.028(5) -0.001(4) 0.006(4) -0.004(4) C3C 0.019(5) 0.033(5) 0.031(5) -0.001(5) -0.002(4) 0.004(4) C4C 0.028(5) 0.037(6) 0.041(6) -0.011(5) 0.002(5) -0.008(5) C5C 0.037(6) 0.051(7) 0.033(6) -0.002(5) 0.006(5) -0.004(5) C6C 0.028(5) 0.044(6) 0.032(6) -0.007(5) -0.005(4) -0.007(5) C7C 0.027(5) 0.032(5) 0.043(6) -0.003(5) 0.006(5) -0.008(4) C8C 0.039(6) 0.034(6) 0.040(6) -0.001(5) -0.011(5) -0.014(5) C9C 0.029(6) 0.055(7) 0.052(7) -0.018(6) 0.000(5) -0.010(5) C10C 0.034(6) 0.057(7) 0.065(8) -0.020(7) 0.002(6) -0.013(6) C11C 0.053(8) 0.052(7) 0.048(7) -0.016(6) -0.007(6) -0.021(6) C12C 0.038(6) 0.053(7) 0.036(6) -0.015(5) -0.008(5) -0.006(5) C13C 0.025(5) 0.037(6) 0.033(6) -0.008(5) 0.002(4) 0.005(5) C14C 0.043(6) 0.031(6) 0.040(6) -0.009(5) 0.009(5) -0.015(5) C15C 0.041(6) 0.022(5) 0.037(6) -0.003(4) -0.007(5) -0.004(5) C16C 0.038(6) 0.030(5) 0.034(6) -0.005(5) -0.008(5) -0.003(5) C17C 0.045(6) 0.024(5) 0.028(5) -0.009(4) 0.001(5) -0.002(5) C18C 0.037(6) 0.037(6) 0.055(7) -0.017(5) -0.016(5) 0.002(5) C19C 0.050(7) 0.032(6) 0.037(6) -0.012(5) -0.002(5) -0.005(5) C20C 0.042(7) 0.046(6) 0.030(6) -0.010(5) 0.000(5) -0.008(5) O1 0.028(4) 0.036(4) 0.038(4) -0.011(3) 0.007(3) -0.005(3) O2 0.040(4) 0.035(4) 0.035(4) -0.009(3) 0.004(3) -0.005(3) C1 0.034(6) 0.048(7) 0.058(7) -0.018(6) -0.006(5) -0.011(5) C2 0.040(6) 0.048(6) 0.026(5) -0.005(5) -0.004(5) -0.012(5) C3 0.028(6) 0.054(7) 0.041(6) -0.011(5) 0.000(5) -0.003(5) C4 0.030(6) 0.046(6) 0.036(6) -0.006(5) 0.007(5) -0.008(5) C5 0.034(6) 0.047(7) 0.054(7) -0.019(6) 0.003(5) 0.003(5) O3 0.035(4) 0.034(4) 0.034(4) -0.008(3) 0.002(3) -0.007(3) O4 0.042(4) 0.036(4) 0.032(4) -0.003(3) -0.005(3) -0.003(3) C6 0.048(7) 0.057(7) 0.044(7) -0.012(6) 0.005(5) -0.017(6) C7 0.037(6) 0.038(6) 0.031(6) -0.008(5) -0.003(5) -0.003(5) C8 0.042(6) 0.038(6) 0.033(6) 0.000(5) -0.003(5) -0.012(5) C9 0.046(7) 0.023(5) 0.043(6) -0.004(5) 0.002(5) -0.006(5) C10 0.047(7) 0.040(6) 0.038(6) -0.010(5) -0.002(5) -0.001(5) O5 0.079(7) 0.078(7) 0.071(6) -0.046(6) -0.004(5) -0.006(5) C11 0.094(11) 0.045(8) 0.085(11) -0.015(8) 0.010(9) -0.019(8) C12 0.085(10) 0.045(7) 0.049(8) -0.006(6) -0.009(7) 0.005(7) C13 0.088(10) 0.042(7) 0.051(8) -0.009(6) 0.008(7) -0.010(7) C14 0.052(8) 0.077(10) 0.057(8) -0.030(7) 0.000(6) 0.010(7) O6 0.041(5) 0.076(6) 0.066(6) 0.012(5) -0.002(4) -0.002(5) C15 0.038(7) 0.059(8) 0.071(9) -0.019(7) -0.003(6) -0.017(6) C16 0.064(8) 0.062(8) 0.038(7) -0.011(6) -0.002(6) 0.000(7) C17 0.048(7) 0.042(6) 0.053(7) -0.008(6) -0.016(6) -0.001(6) C18 0.063(8) 0.059(8) 0.049(7) -0.011(6) 0.017(6) -0.025(7) O7 0.127(10) 0.079(7) 0.100(8) 0.000(6) -0.029(7) -0.032(7) C19 0.103(12) 0.061(9) 0.063(9) -0.003(8) -0.009(9) -0.013(9) C20 0.079(10) 0.061(8) 0.060(8) -0.013(7) -0.027(7) 0.000(8) C21 0.134(16) 0.100(13) 0.101(13) 0.015(11) -0.046(12) -0.054(12) C22 0.143(16) 0.088(11) 0.080(11) -0.002(9) -0.055(11) -0.070(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O2 2.316(7) . ? U1 O4 2.321(6) . ? U1 O3A 2.323(6) . ? U1 O1 2.326(6) . ? U1 O2A 2.365(6) . ? U1 O3 2.423(6) . ? U1 N1A 2.589(7) . ? U1 N2A 2.607(8) . ? U1 O1B 2.622(6) . ? U1 U2 3.7418(6) . ? U1 U3 7.3458(7) . ? U2 O1C 2.222(6) . ? U2 O1A 2.326(6) . ? U2 O1B 2.342(6) . ? U2 O4A 2.370(6) . ? U2 O3A 2.392(6) . ? U2 O2A 2.398(6) . ? U2 O2B 2.468(6) . ? U2 O2C 2.520(6) . ? U2 U3 3.8895(5) . ? U3 O3C 2.167(6) . ? U3 O3B 2.175(6) . ? U3 O2C 2.327(6) . ? U3 O2B 2.379(6) . ? U3 N1B 2.546(8) . ? U3 N1C 2.577(8) . ? U3 N2B 2.602(8) . ? U3 N2C 2.622(8) . ? O1A C1A 1.361(10) . ? O1A O4C 2.845(9) . ? O2A C2A 1.340(11) . ? O2A O3A 2.412(9) . ? O2A N1A 2.699(9) . ? O3A C16A 1.333(10) . ? O3A N2A 2.772(9) . ? O4A C17A 1.355(11) . ? O4A O4B 2.746(9) . ? N1A C7A 1.301(12) . ? N1A C8A 1.441(11) . ? N1A N2A 2.639(11) . ? N2A C14A 1.296(12) . ? N2A C13A 1.436(11) . ? C1A C6A 1.375(13) . ? C1A C2A 1.407(12) . ? C2A C3A 1.411(13) . ? C3A C4A 1.373(13) . ? C3A C7A 1.466(12) . ? C4A C5A 1.398(12) . ? C5A C6A 1.387(12) . ? C8A C9A 1.378(12) . ? C8A C13A 1.388(13) . ? C9A C10A 1.377(13) . ? C10A C11A 1.399(14) . ? C11A C12A 1.388(13) . ? C12A C13A 1.363(13) . ? C14A C15A 1.448(13) . ? C15A C16A 1.393(13) . ? C15A C20A 1.406(13) . ? C16A C17A 1.416(13) . ? C17A C18A 1.377(13) . ? C18A C19A 1.403(13) . ? C19A C20A 1.366(13) . ? O1B C1B 1.368(11) . ? O2B C2B 1.373(11) . ? O2B N1B 2.908(10) . ? O2B O3B 3.039(9) . ? O3B C16B 1.339(11) . ? O3B N2B 2.739(10) . ? O4B C17B 1.371(11) . ? N1B C7B 1.305(12) . ? N1B C8B 1.432(11) . ? N1B N2B 2.618(12) . ? N2B C14B 1.275(12) . ? N2B C13B 1.444(12) . ? C1B C6B 1.368(14) . ? C1B C2B 1.413(12) . ? C2B C3B 1.409(12) . ? C3B C4B 1.382(13) . ? C3B C7B 1.438(13) . ? C4B C5B 1.388(14) . ? C5B C6B 1.391(14) . ? C8B C9B 1.387(13) . ? C8B C13B 1.388(13) . ? C9B C10B 1.362(13) . ? C10B C11B 1.396(14) . ? C11B C12B 1.409(14) . ? C12B C13B 1.386(13) . ? C14B C15B 1.446(13) . ? C15B C20B 1.398(13) . ? C15B C16B 1.421(13) . ? C16B C17B 1.394(13) . ? C17B C18B 1.379(13) . ? C18B C19B 1.394(13) . ? C19B C20B 1.345(13) . ? O1C C1C 1.327(11) . ? O2C C2C 1.350(11) . ? O2C N1C 2.890(10) . ? O2C O3C 3.023(8) . ? O3C C16C 1.336(11) . ? O3C N2C 2.752(10) . ? O4C C17C 1.383(11) . ? N1C C7C 1.288(12) . ? N1C C8C 1.425(12) . ? N1C N2C 2.608(11) . ? N2C C14C 1.292(12) . ? N2C C13C 1.418(12) . ? C1C C6C 1.393(13) . ? C1C C2C 1.434(13) . ? C2C C3C 1.432(13) . ? C3C C4C 1.384(13) . ? C3C C7C 1.435(13) . ? C4C C5C 1.390(13) . ? C5C C6C 1.376(14) . ? C8C C13C 1.401(13) . ? C8C C9C 1.406(13) . ? C9C C10C 1.391(14) . ? C10C C11C 1.383(15) . ? C11C C12C 1.379(14) . ? C12C C13C 1.386(13) . ? C14C C15C 1.450(13) . ? C15C C16C 1.393(13) . ? C15C C20C 1.413(13) . ? C16C C17C 1.403(13) . ? C17C C18C 1.370(12) . ? C18C C19C 1.399(13) . ? C19C C20C 1.347(14) . ? O1 C2 1.277(11) . ? O2 C4 1.274(11) . ? C1 C2 1.492(13) . ? C2 C3 1.397(14) . ? C3 C4 1.407(14) . ? C4 C5 1.524(13) . ? O3 C7 1.251(11) . ? O4 C9 1.287(11) . ? C6 C7 1.486(14) . ? C7 C8 1.411(13) . ? C8 C9 1.380(14) . ? C9 C10 1.492(13) . ? O5 C14 1.407(14) . ? O5 C11 1.411(15) . ? C11 C12 1.515(16) . ? C12 C13 1.495(15) . ? C13 C14 1.488(15) . ? O6 C18 1.434(14) . ? O6 C15 1.443(14) . ? C15 C16 1.493(15) . ? C16 C17 1.520(16) . ? C17 C18 1.520(15) . ? O7 C22 1.426(15) . ? O7 C19 1.436(16) . ? C19 C20 1.499(17) . ? C20 C21 1.499(18) . ? C21 C22 1.510(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 U1 O4 140.3(2) . . ? O2 U1 O3A 137.3(2) . . ? O4 U1 O3A 74.0(2) . . ? O2 U1 O1 72.2(2) . . ? O4 U1 O1 90.1(2) . . ? O3A U1 O1 146.4(2) . . ? O2 U1 O2A 78.2(2) . . ? O4 U1 O2A 135.5(2) . . ? O3A U1 O2A 61.9(2) . . ? O1 U1 O2A 130.5(2) . . ? O2 U1 O3 72.9(2) . . ? O4 U1 O3 68.5(2) . . ? O3A U1 O3 121.3(2) . . ? O1 U1 O3 77.1(2) . . ? O2A U1 O3 130.1(2) . . ? O2 U1 N1A 76.7(2) . . ? O4 U1 N1A 130.6(2) . . ? O3A U1 N1A 98.7(2) . . ? O1 U1 N1A 69.2(2) . . ? O2A U1 N1A 65.8(2) . . ? O3 U1 N1A 140.0(2) . . ? O2 U1 N2A 135.1(2) . . ? O4 U1 N2A 71.4(2) . . ? O3A U1 N2A 68.1(2) . . ? O1 U1 N2A 78.9(2) . . ? O2A U1 N2A 96.3(2) . . ? O3 U1 N2A 132.7(2) . . ? N1A U1 N2A 61.0(2) . . ? O2 U1 O1B 83.7(2) . . ? O4 U1 O1B 92.5(2) . . ? O3A U1 O1B 67.0(2) . . ? O1 U1 O1B 144.7(2) . . ? O2A U1 O1B 65.7(2) . . ? O3 U1 O1B 71.2(2) . . ? N1A U1 O1B 130.4(2) . . ? N2A U1 O1B 135.0(2) . . ? O1C U2 O1A 93.0(2) . . ? O1C U2 O1B 154.0(2) . . ? O1A U2 O1B 87.1(2) . . ? O1C U2 O4A 90.6(2) . . ? O1A U2 O4A 167.2(2) . . ? O1B U2 O4A 95.0(2) . . ? O1C U2 O3A 88.7(2) . . ? O1A U2 O3A 126.5(2) . . ? O1B U2 O3A 70.8(2) . . ? O4A U2 O3A 65.8(2) . . ? O1C U2 O2A 86.4(2) . . ? O1A U2 O2A 66.3(2) . . ? O1B U2 O2A 69.9(2) . . ? O4A U2 O2A 126.3(2) . . ? O3A U2 O2A 60.5(2) . . ? O1C U2 O2B 136.1(2) . . ? O1A U2 O2B 75.9(2) . . ? O1B U2 O2B 69.1(2) . . ? O4A U2 O2B 93.0(2) . . ? O3A U2 O2B 132.2(2) . . ? O2A U2 O2B 124.5(2) . . ? O1C U2 O2C 66.8(2) . . ? O1A U2 O2C 90.4(2) . . ? O1B U2 O2C 139.2(2) . . ? O4A U2 O2C 79.7(2) . . ? O3A U2 O2C 137.5(2) . . ? O2A U2 O2C 143.9(2) . . ? O2B U2 O2C 70.8(2) . . ? O3C U3 O3B 165.3(2) . . ? O3C U3 O2C 84.5(2) . . ? O3B U3 O2C 84.7(2) . . ? O3C U3 O2B 84.2(2) . . ? O3B U3 O2B 83.6(2) . . ? O2C U3 O2B 75.8(2) . . ? O3C U3 N1B 76.0(2) . . ? O3B U3 N1B 107.8(2) . . ? O2C U3 N1B 143.9(2) . . ? O2B U3 N1B 72.3(2) . . ? O3C U3 N1C 100.5(2) . . ? O3B U3 N1C 85.4(3) . . ? O2C U3 N1C 72.0(2) . . ? O2B U3 N1C 146.8(2) . . ? N1B U3 N1C 140.9(3) . . ? O3C U3 N2B 123.4(2) . . ? O3B U3 N2B 69.3(2) . . ? O2C U3 N2B 150.7(2) . . ? O2B U3 N2B 112.9(2) . . ? N1B U3 N2B 61.1(3) . . ? N1C U3 N2B 92.1(3) . . ? O3C U3 N2C 69.4(2) . . ? O3B U3 N2C 124.7(2) . . ? O2C U3 N2C 118.2(2) . . ? O2B U3 N2C 147.6(2) . . ? N1B U3 N2C 83.0(3) . . ? N1C U3 N2C 60.2(2) . . ? N2B U3 N2C 70.2(2) . . ? C1A O1A U2 122.2(5) . . ? C1A O1A O4C 95.9(5) . . ? U2 O1A O4C 140.8(3) . . ? C2A O2A U1 126.1(6) . . ? C2A O2A U2 118.5(5) . . ? U1 O2A U2 103.6(2) . . ? C16A O3A U1 130.4(6) . . ? C16A O3A U2 119.5(6) . . ? U1 O3A U2 105.0(2) . . ? C17A O4A U2 120.0(5) . . ? C7A N1A C8A 118.6(7) . . ? C7A N1A U1 126.1(6) . . ? C8A N1A U1 114.8(6) . . ? C14A N2A C13A 120.1(8) . . ? C14A N2A U1 125.4(6) . . ? C13A N2A U1 114.4(6) . . ? O1A C1A C6A 128.3(8) . . ? O1A C1A C2A 114.4(8) . . ? C6A C1A C2A 117.3(8) . . ? O2A C2A C1A 117.3(8) . . ? O2A C2A C3A 120.9(8) . . ? C1A C2A C3A 121.8(9) . . ? C4A C3A C2A 118.8(8) . . ? C4A C3A C7A 120.9(8) . . ? C2A C3A C7A 120.0(9) . . ? C3A C4A C5A 119.9(8) . . ? C6A C5A C4A 120.2(9) . . ? C1A C6A C5A 121.7(8) . . ? N1A C7A C3A 125.5(8) . . ? C9A C8A C13A 120.4(8) . . ? C9A C8A N1A 123.7(8) . . ? C13A C8A N1A 115.8(7) . . ? C10A C9A C8A 120.1(10) . . ? C9A C10A C11A 119.8(9) . . ? C12A C11A C10A 118.9(9) . . ? C13A C12A C11A 121.1(9) . . ? C12A C13A C8A 119.4(8) . . ? C12A C13A N2A 124.8(9) . . ? C8A C13A N2A 115.7(8) . . ? N2A C14A C15A 126.5(9) . . ? C16A C15A C20A 118.1(8) . . ? C16A C15A C14A 122.4(9) . . ? C20A C15A C14A 119.2(9) . . ? O3A C16A C15A 121.3(8) . . ? O3A C16A C17A 115.7(8) . . ? C15A C16A C17A 122.9(8) . . ? O4A C17A C18A 127.6(8) . . ? O4A C17A C16A 115.8(8) . . ? C18A C17A C16A 116.5(8) . . ? C17A C18A C19A 121.1(9) . . ? C20A C19A C18A 121.4(9) . . ? C19A C20A C15A 119.5(9) . . ? C1B O1B U2 112.0(6) . . ? C1B O1B U1 135.4(6) . . ? U2 O1B U1 97.7(2) . . ? C2B O2B U3 139.8(5) . . ? C2B O2B U2 109.1(5) . . ? U3 O2B U2 106.7(3) . . ? C16B O3B U3 147.5(6) . . ? C7B N1B C8B 117.6(8) . . ? C7B N1B U3 129.5(6) . . ? C8B N1B U3 112.8(6) . . ? C14B N2B C13B 118.0(8) . . ? C14B N2B U3 131.3(7) . . ? C13B N2B U3 110.3(6) . . ? O1B C1B C6B 121.7(9) . . ? O1B C1B C2B 118.9(9) . . ? C6B C1B C2B 119.4(9) . . ? O2B C2B C3B 122.1(8) . . ? O2B C2B C1B 118.4(8) . . ? C3B C2B C1B 119.5(9) . . ? C4B C3B C2B 119.8(9) . . ? C4B C3B C7B 115.7(9) . . ? C2B C3B C7B 124.4(9) . . ? C3B C4B C5B 120.1(9) . . ? C4B C5B C6B 120.2(10) . . ? C1B C6B C5B 120.9(10) . . ? N1B C7B C3B 130.2(9) . . ? C9B C8B C13B 120.5(9) . . ? C9B C8B N1B 125.5(9) . . ? C13B C8B N1B 114.0(8) . . ? C10B C9B C8B 120.6(10) . . ? C9B C10B C11B 119.1(10) . . ? C10B C11B C12B 121.5(10) . . ? C13B C12B C11B 117.7(10) . . ? C12B C13B C8B 120.5(9) . . ? C12B C13B N2B 122.8(9) . . ? C8B C13B N2B 116.7(8) . . ? N2B C14B C15B 126.4(9) . . ? C20B C15B C16B 117.9(9) . . ? C20B C15B C14B 120.1(9) . . ? C16B C15B C14B 121.8(9) . . ? O3B C16B C17B 118.9(9) . . ? O3B C16B C15B 121.7(9) . . ? C17B C16B C15B 119.3(9) . . ? O4B C17B C18B 120.3(8) . . ? O4B C17B C16B 119.5(9) . . ? C18B C17B C16B 120.2(9) . . ? C17B C18B C19B 120.2(9) . . ? C20B C19B C18B 119.9(10) . . ? C19B C20B C15B 122.2(10) . . ? C1C O1C U2 125.5(6) . . ? C2C O2C U3 138.3(6) . . ? C2C O2C U2 114.6(5) . . ? U3 O2C U2 106.7(3) . . ? C2C O2C N1C 81.9(5) . . ? U3 O2C N1C 58.0(2) . . ? U2 O2C N1C 162.6(3) . . ? C16C O3C U3 136.7(6) . . ? C7C N1C C8C 117.6(9) . . ? C7C N1C U3 130.3(7) . . ? C8C N1C U3 111.1(6) . . ? C14C N2C C13C 119.6(8) . . ? C14C N2C U3 128.8(7) . . ? C13C N2C U3 111.5(6) . . ? N1C N2C U3 59.0(2) . . ? O1C C1C C6C 124.0(9) . . ? O1C C1C C2C 117.2(9) . . ? C6C C1C C2C 118.8(9) . . ? O2C C2C C3C 126.0(8) . . ? O2C C2C C1C 115.6(8) . . ? C3C C2C C1C 118.4(9) . . ? C4C C3C C2C 119.7(9) . . ? C4C C3C C7C 118.8(9) . . ? C2C C3C C7C 121.5(9) . . ? C3C C4C C5C 121.2(9) . . ? C6C C5C C4C 119.7(10) . . ? C5C C6C C1C 122.0(9) . . ? N1C C7C C3C 129.5(9) . . ? C13C C8C C9C 120.4(9) . . ? C13C C8C N1C 116.0(9) . . ? C9C C8C N1C 123.6(9) . . ? C10C C9C C8C 118.0(10) . . ? C11C C10C C9C 121.6(10) . . ? C12C C11C C10C 119.9(10) . . ? C11C C12C C13C 120.3(10) . . ? C12C C13C C8C 119.7(9) . . ? C12C C13C N2C 126.1(9) . . ? C8C C13C N2C 114.2(9) . . ? N2C C14C C15C 124.0(9) . . ? C16C C15C C20C 119.1(9) . . ? C16C C15C C14C 122.5(9) . . ? C20C C15C C14C 118.3(9) . . ? O3C C16C C15C 122.8(9) . . ? O3C C16C C17C 118.2(8) . . ? C15C C16C C17C 119.0(9) . . ? C18C C17C O4C 119.4(9) . . ? C18C C17C C16C 120.5(9) . . ? O4C C17C C16C 120.1(8) . . ? C17C C18C C19C 120.4(10) . . ? C20C C19C C18C 119.7(10) . . ? C19C C20C C15C 121.2(10) . . ? C2 O1 U1 135.1(6) . . ? C4 O2 U1 135.7(6) . . ? O1 C2 C3 123.9(9) . . ? O1 C2 C1 115.0(9) . . ? C3 C2 C1 121.1(9) . . ? C2 C3 C4 123.0(9) . . ? O2 C4 C3 125.1(9) . . ? O2 C4 C5 114.7(9) . . ? C3 C4 C5 120.1(9) . . ? C7 O3 U1 135.6(6) . . ? C9 O4 U1 138.3(6) . . ? O3 C7 C8 123.4(9) . . ? O3 C7 C6 117.1(9) . . ? C8 C7 C6 119.5(9) . . ? C9 C8 C7 124.2(9) . . ? O4 C9 C8 121.5(9) . . ? O4 C9 C10 117.6(9) . . ? C8 C9 C10 120.9(9) . . ? C14 O5 C11 109.5(9) . . ? O5 C11 C12 106.6(10) . . ? C13 C12 C11 101.3(10) . . ? C14 C13 C12 103.5(9) . . ? O5 C14 C13 107.2(10) . . ? C18 O6 C15 108.8(9) . . ? O6 C15 C16 106.5(10) . . ? C15 C16 C17 104.4(10) . . ? C18 C17 C16 100.9(9) . . ? O6 C18 C17 107.7(9) . . ? C22 O7 C19 105.4(11) . . ? O7 C19 C20 105.4(13) . . ? C21 C20 C19 106.1(12) . . ? C20 C21 C22 101.2(11) . . ? O7 C22 C21 111.7(11) . . ? #===END data_7.5thf _database_code_depnum_ccdc_archive 'CCDC 233082' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C146 H132 N12 O29 U4' _chemical_formula_weight 3470.76 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' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.1915(19) _cell_length_b 16.7590(16) _cell_length_c 27.666(3) _cell_angle_alpha 86.586(7) _cell_angle_beta 89.518(6) _cell_angle_gamma 63.252(7) _cell_volume 6690.6(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 39048 _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 25.68 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent light brown' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_method ? _exptl_crystal_F_000 3384 _exptl_absorpt_coefficient_mu 4.907 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.498 _exptl_absorpt_correction_T_max 0.675 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 39048 _diffrn_reflns_av_R_equivalents 0.0727 _diffrn_reflns_av_sigmaI/netI 0.0966 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 25.68 _reflns_number_total 21991 _reflns_number_gt 9842 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. Some restraints on bond lengths, angles and displacement parameters have been applied to the badly resolved THF molecules. The H atoms bound to O atoms have not been found, nor introduced. All other H atoms were introduced at calculated positions as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. Some voids are present, which likely indicate the presence of unresolved solvent molecules. Some short H...H contacts involving THF molecules might be due to the imperfect location of the latter. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+2.1096P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21991 _refine_ls_number_parameters 1726 _refine_ls_number_restraints 343 _refine_ls_R_factor_all 0.2031 _refine_ls_R_factor_gt 0.0820 _refine_ls_wR_factor_ref 0.2051 _refine_ls_wR_factor_gt 0.1557 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.168 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.865 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.865 _refine_diff_density_max 1.244 _refine_diff_density_min -1.470 _refine_diff_density_rms 0.167 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 U1 U -0.15615(5) 1.10246(5) 0.13446(3) 0.0442(2) Uani 1 1 d . . . U2 U 0.03245(6) 1.17178(5) 0.15673(3) 0.0463(2) Uani 1 1 d . . . U3 U 0.24754(6) 0.49719(6) 0.43218(3) 0.0547(3) Uani 1 1 d . . . U4 U 0.42870(6) 0.41364(6) 0.33519(3) 0.0584(3) Uani 1 1 d . . . O1A O -0.1943(10) 1.0750(9) 0.3061(5) 0.054(4) Uani 1 1 d . . . O2A O -0.2046(9) 1.0834(8) 0.2078(5) 0.049(4) Uani 1 1 d . . . O3A O -0.0496(9) 1.1378(8) 0.0890(5) 0.044(4) Uani 1 1 d . . . O4A O -0.0060(10) 1.2696(9) 0.0934(5) 0.056(4) Uani 1 1 d . . . N1A N -0.2970(11) 1.0711(10) 0.1247(6) 0.044(4) Uani 1 1 d . . . N2A N -0.1672(11) 1.0766(11) 0.0440(6) 0.051(5) Uani 1 1 d . . . C1A C -0.2544(16) 1.0529(15) 0.2841(9) 0.061(7) Uani 1 1 d . . . C2A C -0.2588(15) 1.0577(14) 0.2329(8) 0.051(6) Uani 1 1 d . . . C3A C -0.3233(15) 1.0341(17) 0.2097(10) 0.071(8) Uani 1 1 d . . . C4A C -0.3819(16) 1.0121(17) 0.2385(9) 0.073(8) Uani 1 1 d . . . H4A H -0.4264 1.0005 0.2238 0.088 Uiso 1 1 calc R . . C5A C -0.376(2) 1.0072(19) 0.2871(12) 0.091(9) Uani 1 1 d U . . H5A H -0.4135 0.9891 0.3055 0.109 Uiso 1 1 calc R . . C6A C -0.3139(18) 1.0287(16) 0.3097(9) 0.079(9) Uani 1 1 d . . . H6A H -0.3121 1.0269 0.3434 0.094 Uiso 1 1 calc R . . C7A C -0.3395(16) 1.0448(15) 0.1582(9) 0.065(7) Uani 1 1 d . . . H7A H -0.3856 1.0314 0.1470 0.078 Uiso 1 1 calc R . . C8A C -0.3363(14) 1.0815(14) 0.0753(7) 0.053(6) Uani 1 1 d . . . H8A1 H -0.3474 1.1395 0.0606 0.064 Uiso 1 1 calc R . . H8A2 H -0.3954 1.0800 0.0776 0.064 Uiso 1 1 calc R . . C9A C -0.2751(15) 1.0108(13) 0.0436(7) 0.044(5) Uani 1 1 d . . . C10A C -0.3024(16) 0.9501(15) 0.0276(8) 0.064(7) Uani 1 1 d . . . H10A H -0.3599 0.9542 0.0358 0.077 Uiso 1 1 calc R . . C11A C -0.2443(18) 0.8827(14) -0.0010(8) 0.069(8) Uani 1 1 d . . . H11A H -0.2621 0.8413 -0.0120 0.083 Uiso 1 1 calc R . . C12A C -0.1573(16) 0.8784(14) -0.0132(8) 0.055(6) Uani 1 1 d . . . H12A H -0.1166 0.8319 -0.0311 0.066 Uiso 1 1 calc R . . C13A C -0.1329(15) 0.9394(13) 0.0006(7) 0.048(6) Uani 1 1 d . . . H13A H -0.0759 0.9360 -0.0082 0.058 Uiso 1 1 calc R . . C14A C -0.1905(15) 1.0066(14) 0.0274(8) 0.051(6) Uani 1 1 d . . . C15A C -0.1603(12) 1.1293(15) 0.0076(7) 0.052(6) Uani 1 1 d . . . H15A H -0.1724 1.1192 -0.0237 0.062 Uiso 1 1 calc R . . C16A C -0.1360(17) 1.1994(14) 0.0134(8) 0.051(6) Uani 1 1 d . . . C17A C -0.0826(15) 1.2004(16) 0.0530(7) 0.051(6) Uani 1 1 d . . . C18A C -0.0604(15) 1.2732(15) 0.0551(7) 0.054(6) Uani 1 1 d . . . C19A C -0.0945(16) 1.3422(16) 0.0183(9) 0.070(7) Uani 1 1 d U . . H19A H -0.0837 1.3920 0.0204 0.084 Uiso 1 1 calc R . . C20A C -0.1433(17) 1.3374(17) -0.0208(10) 0.074(7) Uani 1 1 d U . . H20A H -0.1641 1.3827 -0.0454 0.089 Uiso 1 1 calc R . . C21A C -0.1606(16) 1.2669(17) -0.0231(8) 0.068(7) Uani 1 1 d . . . H21A H -0.1907 1.2628 -0.0507 0.081 Uiso 1 1 calc R . . O1B O 0.2573(10) 0.9026(9) 0.0935(5) 0.060(4) Uani 1 1 d . . . O2B O 0.1616(9) 1.0658(8) 0.1270(5) 0.050(4) Uani 1 1 d . . . O3B O -0.1304(8) 1.2223(8) 0.1691(4) 0.040(3) Uani 1 1 d . . . O4B O -0.2651(9) 1.2360(9) 0.1122(5) 0.050(4) Uani 1 1 d . . . N1B N 0.1584(13) 1.2269(11) 0.1537(6) 0.049(5) Uani 1 1 d . . . N2B N -0.0338(12) 1.3198(10) 0.2030(6) 0.048(5) Uani 1 1 d . . . C1B C 0.3003(15) 0.9547(15) 0.1012(8) 0.056(6) Uani 1 1 d . . . C2B C 0.2503(14) 1.0409(13) 0.1189(7) 0.044(5) Uani 1 1 d . . . C3B C 0.2908(14) 1.0963(12) 0.1231(7) 0.041(5) Uani 1 1 d . . . C4B C 0.3860(16) 1.0652(17) 0.1116(9) 0.070(7) Uani 1 1 d . . . H4B H 0.4133 1.1033 0.1140 0.084 Uiso 1 1 calc R . . C5B C 0.4387(17) 0.9794(18) 0.0969(9) 0.076(8) Uani 1 1 d . . . H5B H 0.5017 0.9571 0.0912 0.091 Uiso 1 1 calc R . . C6B C 0.3898(19) 0.9266(18) 0.0911(9) 0.076(8) Uani 1 1 d . . . H6B H 0.4222 0.8698 0.0796 0.091 Uiso 1 1 calc R . . C7B C 0.2460(16) 1.1855(15) 0.1385(8) 0.056(6) Uani 1 1 d . . . H7B H 0.2802 1.2177 0.1380 0.067 Uiso 1 1 calc R . . C8B C 0.1298(15) 1.3212(14) 0.1667(9) 0.062(7) Uani 1 1 d . . . H8B1 H 0.1801 1.3365 0.1600 0.074 Uiso 1 1 calc R . . H8B2 H 0.0769 1.3616 0.1467 0.074 Uiso 1 1 calc R . . C9B C 0.1057(15) 1.3333(12) 0.2182(8) 0.042(5) Uani 1 1 d U . . C10B C 0.1613(17) 1.3489(13) 0.2507(10) 0.065(7) Uani 1 1 d . . . H10B H 0.2138 1.3531 0.2397 0.078 Uiso 1 1 calc R . . C11B C 0.139(2) 1.3584(15) 0.2992(10) 0.072(8) Uani 1 1 d . . . H11B H 0.1793 1.3641 0.3208 0.086 Uiso 1 1 calc R . . C12B C 0.058(2) 1.3594(14) 0.3160(11) 0.086(10) Uani 1 1 d . . . H12B H 0.0413 1.3712 0.3480 0.103 Uiso 1 1 calc R . . C13B C 0.0003(17) 1.3425(15) 0.2847(9) 0.064(7) Uani 1 1 d . . . H13B H -0.0520 1.3378 0.2953 0.077 Uiso 1 1 calc R . . C14B C 0.0267(16) 1.3336(13) 0.2370(10) 0.062(7) Uani 1 1 d . . . C15B C -0.1186(15) 1.3840(12) 0.1970(7) 0.046(6) Uani 1 1 d . . . H15B H -0.1342 1.4343 0.2145 0.055 Uiso 1 1 calc R . . C16B C -0.1910(16) 1.3847(15) 0.1654(7) 0.056(6) Uani 1 1 d . . . C17B C -0.1916(14) 1.3035(13) 0.1544(8) 0.046(6) Uani 1 1 d . . . C18B C -0.2636(15) 1.3109(16) 0.1238(8) 0.056(6) Uani 1 1 d . . . C19B C -0.3293(16) 1.3935(17) 0.1066(8) 0.070(7) Uani 1 1 d . . . H19B H -0.3771 1.3977 0.0865 0.085 Uiso 1 1 calc R . . C20B C -0.3255(17) 1.4737(16) 0.1190(9) 0.068(7) Uani 1 1 d U . . H20B H -0.3696 1.5290 0.1061 0.082 Uiso 1 1 calc R . . C21B C -0.2561(14) 1.4697(14) 0.1504(9) 0.060(7) Uani 1 1 d . . . H21B H -0.2542 1.5208 0.1605 0.072 Uiso 1 1 calc R . . O1C O -0.0011(9) 0.5772(9) 0.3155(5) 0.055(4) Uani 1 1 d . . . O2C O 0.1107(10) 0.5376(8) 0.3961(5) 0.052(4) Uani 1 1 d . . . O3C O 0.4085(9) 0.4411(10) 0.4241(6) 0.063(4) Uani 1 1 d . . . O4C O 0.5232(9) 0.2991(9) 0.3814(6) 0.060(4) Uani 1 1 d . . . N1C N 0.1199(14) 0.5463(11) 0.4976(6) 0.058(5) Uani 1 1 d . . . N2C N 0.3223(13) 0.5082(12) 0.5127(6) 0.071(6) Uani 1 1 d . . . C1C C -0.0396(16) 0.6024(13) 0.3606(8) 0.050(6) Uani 1 1 d . . . C2C C 0.0184(16) 0.5815(12) 0.4023(9) 0.051(6) Uani 1 1 d . . . C3C C -0.0212(13) 0.6099(13) 0.4466(8) 0.048(6) Uani 1 1 d . . . C4C C -0.1150(18) 0.6494(16) 0.4514(10) 0.078(8) Uani 1 1 d U . . H4C H -0.1414 0.6598 0.4818 0.094 Uiso 1 1 calc R . . C5C C -0.170(2) 0.6735(19) 0.4098(12) 0.102(10) Uani 1 1 d U . . H5C H -0.2328 0.7089 0.4128 0.123 Uiso 1 1 calc R . . C6C C -0.1365(16) 0.6487(14) 0.3640(9) 0.066(7) Uani 1 1 d U . . H6C H -0.1758 0.6617 0.3372 0.079 Uiso 1 1 calc R . . C7C C 0.0297(18) 0.5850(14) 0.4916(9) 0.059(6) Uani 1 1 d U . . H7C H -0.0050 0.5976 0.5196 0.071 Uiso 1 1 calc R . . C8C C 0.1487(17) 0.5271(15) 0.5472(9) 0.073(7) Uani 1 1 d U . . H8C1 H 0.1955 0.4654 0.5521 0.087 Uiso 1 1 calc R . . H8C2 H 0.0965 0.5350 0.5672 0.087 Uiso 1 1 calc R . . C9C C 0.1888(17) 0.5908(15) 0.5622(8) 0.060(6) Uani 1 1 d U . . C10C C 0.1433(17) 0.6592(14) 0.5929(8) 0.066(7) Uani 1 1 d U . . H10C H 0.0863 0.6674 0.6049 0.079 Uiso 1 1 calc R . . C11C C 0.1792(17) 0.7164(16) 0.6066(9) 0.070(7) Uani 1 1 d U . . H11C H 0.1476 0.7605 0.6280 0.084 Uiso 1 1 calc R . . C12C C 0.263(2) 0.7062(19) 0.5880(10) 0.094(9) Uani 1 1 d U . . H12C H 0.2862 0.7451 0.5960 0.113 Uiso 1 1 calc R . . C13C C 0.3117(19) 0.6384(18) 0.5573(10) 0.085(8) Uani 1 1 d U . . H13C H 0.3672 0.6315 0.5438 0.102 Uiso 1 1 calc R . . C14C C 0.2716(19) 0.5788(17) 0.5474(10) 0.076(8) Uani 1 1 d U . . C15C C 0.4021(19) 0.4520(18) 0.5290(10) 0.088(8) Uani 1 1 d U . . H15C H 0.4213 0.4611 0.5589 0.106 Uiso 1 1 calc R . . C16C C 0.4675(19) 0.3713(18) 0.5029(10) 0.087(8) Uani 1 1 d U . . C17C C 0.4655(17) 0.3714(16) 0.4532(9) 0.066(7) Uani 1 1 d U . . C18C C 0.5302(19) 0.2913(18) 0.4300(11) 0.083(8) Uani 1 1 d U . . C19C C 0.5884(19) 0.2186(18) 0.4592(11) 0.090(9) Uani 1 1 d U . . H19C H 0.6290 0.1675 0.4443 0.108 Uiso 1 1 calc R . . C20C C 0.590(2) 0.217(2) 0.5097(14) 0.129(12) Uani 1 1 d U . . H20C H 0.6293 0.1648 0.5279 0.155 Uiso 1 1 calc R . . C21C C 0.532(2) 0.295(2) 0.5322(13) 0.121(11) Uani 1 1 d U . . H21C H 0.5350 0.2968 0.5656 0.145 Uiso 1 1 calc R . . O1D O 0.4858(10) 0.6667(10) 0.3552(6) 0.069(5) Uani 1 1 d . . . O2D O 0.4887(10) 0.5112(9) 0.3351(6) 0.067(5) Uani 1 1 d . . . O3D O 0.3102(9) 0.3792(9) 0.3710(5) 0.051(4) Uani 1 1 d . . . O4D O 0.2649(10) 0.3662(8) 0.4607(5) 0.056(4) Uani 1 1 d . . . N1D N 0.5864(14) 0.3474(12) 0.2931(8) 0.070(6) Uani 1 1 d . . . N2D N 0.4296(13) 0.2777(13) 0.2940(7) 0.063(6) Uani 1 1 d . . . C1D C 0.5675(19) 0.5974(17) 0.3399(9) 0.067(7) Uani 1 1 d . . . C2D C 0.5672(14) 0.5198(16) 0.3278(7) 0.052(6) Uani 1 1 d . . . C3D C 0.6445(15) 0.4547(16) 0.3082(9) 0.062(7) Uani 1 1 d . . . C4D C 0.7231(16) 0.4671(16) 0.3039(9) 0.070(7) Uani 1 1 d . . . H4D H 0.7761 0.4222 0.2915 0.084 Uiso 1 1 calc R . . C5D C 0.7256(18) 0.5442(16) 0.3174(9) 0.069(7) Uani 1 1 d . . . H5D H 0.7789 0.5515 0.3137 0.083 Uiso 1 1 calc R . . C6D C 0.6472(19) 0.6098(17) 0.3364(9) 0.070(7) Uani 1 1 d . . . H6D H 0.6474 0.6616 0.3468 0.084 Uiso 1 1 calc R . . C7D C 0.6485(17) 0.3717(16) 0.2925(8) 0.062(7) Uani 1 1 d . . . H7D H 0.7048 0.3316 0.2805 0.074 Uiso 1 1 calc R . . C8D C 0.6135(16) 0.2594(16) 0.2767(10) 0.076(8) Uani 1 1 d . . . H8D1 H 0.6128 0.2197 0.3035 0.091 Uiso 1 1 calc R . . H8D2 H 0.6759 0.2355 0.2645 0.091 Uiso 1 1 calc R . . C9D C 0.5441(15) 0.2643(13) 0.2350(9) 0.057(7) Uani 1 1 d . . . C10D C 0.5705(19) 0.2654(16) 0.1861(11) 0.086(9) Uani 1 1 d . . . H10D H 0.6257 0.2678 0.1790 0.103 Uiso 1 1 calc R . . C11D C 0.5185(15) 0.2631(16) 0.1510(10) 0.068(8) Uani 1 1 d . . . H11D H 0.5348 0.2670 0.1190 0.082 Uiso 1 1 calc R . . C12D C 0.4390(18) 0.2550(16) 0.1617(10) 0.080(8) Uani 1 1 d . . . H12D H 0.4053 0.2481 0.1367 0.096 Uiso 1 1 calc R . . C13D C 0.409(2) 0.2566(16) 0.2074(9) 0.073(8) Uani 1 1 d . . . H13D H 0.3539 0.2533 0.2135 0.088 Uiso 1 1 calc R . . C14D C 0.4593(18) 0.2630(16) 0.2441(9) 0.069(8) Uani 1 1 d . . . C15D C 0.4045(16) 0.2205(18) 0.3139(9) 0.075(8) Uani 1 1 d . . . H15D H 0.4087 0.1748 0.2951 0.089 Uiso 1 1 calc R . . C16D C 0.3702(14) 0.2203(15) 0.3631(9) 0.056(6) Uani 1 1 d . . . C17D C 0.3291(15) 0.2965(16) 0.3896(9) 0.058(7) Uani 1 1 d . . . C18D C 0.3053(15) 0.2877(17) 0.4377(10) 0.067(8) Uani 1 1 d . . . C19D C 0.3164(17) 0.2059(15) 0.4597(9) 0.069(8) Uani 1 1 d . . . H19D H 0.2975 0.2008 0.4911 0.083 Uiso 1 1 calc R . . C20D C 0.3579(19) 0.1323(18) 0.4309(11) 0.086(8) Uani 1 1 d U . . H20D H 0.3696 0.0761 0.4446 0.104 Uiso 1 1 calc R . . C21D C 0.3808(17) 0.1381(17) 0.3867(10) 0.074(7) Uani 1 1 d U . . H21D H 0.4052 0.0867 0.3694 0.089 Uiso 1 1 calc R . . O1E O 0.2855(9) 0.5496(9) 0.3548(5) 0.053(4) Uani 1 1 d . . . O2E O 0.2203(10) 0.6450(9) 0.4303(5) 0.054(4) Uani 1 1 d . . . O3E O -0.0186(10) 1.0523(9) 0.2750(5) 0.053(4) Uani 1 1 d . . . O4E O 0.0832(9) 1.1261(8) 0.2303(5) 0.052(4) Uani 1 1 d . . . N1E N 0.1475(13) 0.8035(11) 0.4659(7) 0.056(5) Uani 1 1 d . . . N2E N -0.0013(13) 0.9918(12) 0.4211(7) 0.058(5) Uani 1 1 d . . . C1E C 0.2742(16) 0.6346(15) 0.3522(8) 0.056(6) Uani 1 1 d . . . C2E C 0.2403(14) 0.6822(14) 0.3919(8) 0.050(6) Uani 1 1 d . . . C3E C 0.2284(14) 0.7737(15) 0.3898(8) 0.054(6) Uani 1 1 d . . . C4E C 0.2477(15) 0.8125(16) 0.3474(8) 0.061(6) Uani 1 1 d . . . H4E H 0.2382 0.8716 0.3460 0.073 Uiso 1 1 calc R . . C5E C 0.2808(14) 0.7618(16) 0.3080(8) 0.060(7) Uani 1 1 d . . . H5E H 0.2946 0.7860 0.2798 0.072 Uiso 1 1 calc R . . C6E C 0.2934(14) 0.6731(15) 0.3109(9) 0.061(7) Uani 1 1 d . . . H6E H 0.3155 0.6392 0.2840 0.073 Uiso 1 1 calc R . . C7E C 0.1802(14) 0.8277(14) 0.4292(8) 0.051(6) Uani 1 1 d . . . H7E H 0.1723 0.8863 0.4275 0.061 Uiso 1 1 calc R . . C8E C 0.0810(17) 0.8656(14) 0.4986(7) 0.059(7) Uani 1 1 d . . . H8E1 H 0.0902 0.9189 0.4992 0.071 Uiso 1 1 calc R . . H8E2 H 0.0916 0.8376 0.5311 0.071 Uiso 1 1 calc R . . C9E C -0.0178(16) 0.8920(14) 0.4825(7) 0.046(5) Uani 1 1 d . . . C10E C -0.068(2) 0.8556(15) 0.5050(9) 0.065(7) Uani 1 1 d . . . H10E H -0.0419 0.8131 0.5306 0.078 Uiso 1 1 calc R . . C11E C -0.161(2) 0.8810(18) 0.4903(10) 0.075(8) Uani 1 1 d . . . H11E H -0.1958 0.8563 0.5061 0.090 Uiso 1 1 calc R . . C12E C -0.196(2) 0.942(2) 0.4531(10) 0.082(9) Uani 1 1 d . . . H12E H -0.2564 0.9578 0.4426 0.099 Uiso 1 1 calc R . . C13E C -0.1464(18) 0.9820(16) 0.4289(8) 0.064(7) Uani 1 1 d . . . H13E H -0.1736 1.0261 0.4041 0.076 Uiso 1 1 calc R . . C14E C -0.0548(16) 0.9534(14) 0.4437(7) 0.050(6) Uani 1 1 d . . . C15E C -0.0048(14) 1.0082(12) 0.3763(8) 0.047(6) Uani 1 1 d . . . H15E H -0.0423 0.9925 0.3577 0.057 Uiso 1 1 calc R . . C16E C 0.0480(15) 1.0518(13) 0.3507(9) 0.054(6) Uani 1 1 d . . . C17E C 0.0400(16) 1.0706(13) 0.3015(9) 0.058(7) Uani 1 1 d . . . C18E C 0.0947(14) 1.1070(13) 0.2787(8) 0.046(5) Uani 1 1 d . . . C19E C 0.1557(15) 1.1247(13) 0.3066(8) 0.057(6) Uani 1 1 d . . . H19E H 0.1910 1.1499 0.2919 0.068 Uiso 1 1 calc R . . C20E C 0.1633(15) 1.1046(14) 0.3559(8) 0.052(6) Uani 1 1 d . . . H20E H 0.2054 1.1144 0.3743 0.063 Uiso 1 1 calc R . . C21E C 0.1100(17) 1.0709(13) 0.3777(9) 0.058(6) Uani 1 1 d . . . H21E H 0.1141 1.0600 0.4112 0.070 Uiso 1 1 calc R . . O1F O -0.0047(9) 1.0439(8) 0.1747(5) 0.046(4) Uani 1 1 d . . . O2F O -0.0774(9) 0.9516(8) 0.1324(5) 0.048(4) Uani 1 1 d . . . O3F O 0.1740(9) 0.5468(9) 0.2796(5) 0.051(4) Uani 1 1 d . . . O4F O 0.3617(10) 0.4679(10) 0.2651(6) 0.062(4) Uani 1 1 d . . . N1F N -0.0599(15) 0.7958(12) 0.1124(6) 0.059(5) Uani 1 1 d . . . N2F N -0.0078(13) 0.6034(10) 0.1663(7) 0.052(5) Uani 1 1 d . . . C1F C 0.0551(15) 0.9549(13) 0.1718(7) 0.047(6) Uani 1 1 d . . . C2F C 0.0127(15) 0.9057(12) 0.1487(7) 0.046(6) Uani 1 1 d . . . C3F C 0.0671(19) 0.8106(16) 0.1434(8) 0.065(7) Uani 1 1 d . . . C4F C 0.1602(18) 0.7712(15) 0.1605(9) 0.068(7) Uani 1 1 d . . . H4F H 0.1985 0.7113 0.1556 0.082 Uiso 1 1 calc R . . C5F C 0.1945(18) 0.8195(16) 0.1838(8) 0.067(7) Uani 1 1 d . . . H5F H 0.2542 0.7896 0.1969 0.081 Uiso 1 1 calc R . . C6F C 0.1445(15) 0.9121(13) 0.1891(7) 0.046(5) Uani 1 1 d . . . H6F H 0.1713 0.9433 0.2040 0.055 Uiso 1 1 calc R . . C7F C 0.0254(16) 0.7636(13) 0.1238(8) 0.050(6) Uani 1 1 d . . . H7F H 0.0626 0.7037 0.1184 0.061 Uiso 1 1 calc R . . C8F C -0.1059(18) 0.7393(16) 0.0983(9) 0.071(7) Uani 1 1 d . . . H8F1 H -0.1484 0.7701 0.0713 0.085 Uiso 1 1 calc R . . H8F2 H -0.0589 0.6832 0.0874 0.085 Uiso 1 1 calc R . . C9F C -0.157(2) 0.7202(17) 0.1375(10) 0.069(7) Uani 1 1 d . . . C10F C -0.249(2) 0.7708(18) 0.1429(9) 0.073(8) Uani 1 1 d . . . H10F H -0.2828 0.8193 0.1212 0.087 Uiso 1 1 calc R . . C11F C -0.294(2) 0.749(2) 0.1810(12) 0.090(9) Uani 1 1 d . . . H11F H -0.3578 0.7795 0.1833 0.108 Uiso 1 1 calc R . . C12F C -0.240(2) 0.6794(19) 0.2165(11) 0.087(9) Uani 1 1 d . . . H12F H -0.2695 0.6672 0.2430 0.105 Uiso 1 1 calc R . . C13F C -0.152(2) 0.6334(17) 0.2125(11) 0.079(8) Uani 1 1 d . . . H13F H -0.1183 0.5880 0.2359 0.095 Uiso 1 1 calc R . . C14F C -0.1051(19) 0.6511(18) 0.1730(11) 0.069(7) Uani 1 1 d . . . C15F C 0.0488(17) 0.5876(13) 0.2025(8) 0.055(6) Uani 1 1 d . . . H15F H 0.0251 0.6044 0.2330 0.066 Uiso 1 1 calc R . . C16F C 0.1456(18) 0.5455(12) 0.1967(8) 0.054(6) Uani 1 1 d . . . C17F C 0.2079(17) 0.5286(14) 0.2340(8) 0.052(6) Uani 1 1 d . . . C18F C 0.3036(17) 0.4887(13) 0.2282(9) 0.054(6) Uani 1 1 d . . . C19F C 0.341(2) 0.4668(17) 0.1828(9) 0.080(8) Uani 1 1 d . . . H19F H 0.4045 0.4409 0.1782 0.096 Uiso 1 1 calc R . . C20F C 0.275(2) 0.4866(14) 0.1418(9) 0.067(8) Uani 1 1 d . . . H20F H 0.2972 0.4766 0.1105 0.080 Uiso 1 1 calc R . . C21F C 0.1835(16) 0.5189(15) 0.1489(8) 0.057(6) Uani 1 1 d . . . H21F H 0.1442 0.5242 0.1233 0.069 Uiso 1 1 calc R . . O1 O -0.0294(16) 0.7886(14) 0.2423(8) 0.123(7) Uani 1 1 d U . . C1 C -0.110(2) 0.8146(19) 0.2729(11) 0.097(9) Uani 1 1 d U . . H1A H -0.1615 0.8675 0.2584 0.116 Uiso 1 1 calc R . . H1B H -0.1282 0.7667 0.2761 0.116 Uiso 1 1 calc R . . C2 C -0.0875(14) 0.8332(14) 0.3205(8) 0.057(6) Uani 1 1 d U . . H2A H -0.1126 0.8085 0.3459 0.068 Uiso 1 1 calc R . . H2B H -0.1120 0.8971 0.3235 0.068 Uiso 1 1 calc R . . C3 C 0.0177(18) 0.7878(17) 0.3233(10) 0.084(8) Uani 1 1 d U . . H3A H 0.0400 0.8207 0.3426 0.100 Uiso 1 1 calc R . . H3B H 0.0411 0.7270 0.3374 0.100 Uiso 1 1 calc R . . C4 C 0.046(2) 0.788(2) 0.2729(11) 0.109(10) Uani 1 1 d U . . H4G H 0.1041 0.7357 0.2679 0.130 Uiso 1 1 calc R . . H4H H 0.0549 0.8412 0.2647 0.130 Uiso 1 1 calc R . . O2 O 0.4007(14) 1.0177(13) 0.2864(8) 0.109(7) Uani 1 1 d U . . C5 C 0.424(2) 0.932(2) 0.3142(12) 0.114(11) Uani 1 1 d U . . H5G H 0.3707 0.9324 0.3304 0.137 Uiso 1 1 calc R . . H5H H 0.4732 0.9186 0.3380 0.137 Uiso 1 1 calc R . . C6 C 0.456(3) 0.868(2) 0.2749(13) 0.138(13) Uani 1 1 d U . . H6G H 0.4516 0.8129 0.2842 0.166 Uiso 1 1 calc R . . H6H H 0.5187 0.8530 0.2654 0.166 Uiso 1 1 calc R . . C7 C 0.385(3) 0.924(2) 0.2349(15) 0.161(16) Uani 1 1 d U . . H7G H 0.4085 0.9037 0.2033 0.193 Uiso 1 1 calc R . . H7H H 0.3275 0.9200 0.2395 0.193 Uiso 1 1 calc R . . C8 C 0.370(2) 1.0179(19) 0.2392(11) 0.101(10) Uani 1 1 d U . . H8A H 0.4055 1.0336 0.2155 0.122 Uiso 1 1 calc R . . H8B H 0.3050 1.0598 0.2347 0.122 Uiso 1 1 calc R . . O3 O 0.461(2) 0.677(2) 0.1360(12) 0.186(11) Uani 1 1 d U . . C9 C 0.492(4) 0.710(3) 0.1712(14) 0.086(17) Uani 1 1 d DU . . H9A H 0.4469 0.7715 0.1765 0.103 Uiso 1 1 calc R . . H9B H 0.5495 0.7105 0.1619 0.103 Uiso 1 1 calc R . . C10 C 0.506(2) 0.651(2) 0.2169(11) 0.033(9) Uani 1 1 d DU . . H10G H 0.5693 0.6252 0.2286 0.039 Uiso 1 1 calc R . . H10H H 0.4653 0.6842 0.2422 0.039 Uiso 1 1 calc R . . C11 C 0.484(3) 0.585(3) 0.2033(15) 0.094(13) Uani 1 1 d U . . H11G H 0.5400 0.5300 0.2001 0.113 Uiso 1 1 calc R . . H11H H 0.4466 0.5741 0.2280 0.113 Uiso 1 1 calc R . . C12 C 0.436(2) 0.611(2) 0.1603(13) 0.076(11) Uani 1 1 d U . . H12G H 0.3699 0.6377 0.1657 0.091 Uiso 1 1 calc R . . H12H H 0.4526 0.5605 0.1407 0.091 Uiso 1 1 calc R . . O4 O 0.315(3) 0.277(2) 0.0499(11) 0.120(14) Uani 1 1 d DU . . C13 C 0.239(2) 0.352(3) 0.0291(16) 0.103(19) Uani 1 1 d DU . . H13G H 0.2228 0.4018 0.0492 0.123 Uiso 1 1 calc R . . H13H H 0.1868 0.3390 0.0267 0.123 Uiso 1 1 calc R . . C14 C 0.264(3) 0.375(3) -0.0211(15) 0.13(2) Uani 1 1 d DU . . H14A H 0.2617 0.4339 -0.0227 0.153 Uiso 1 1 calc R . . H14B H 0.2227 0.3733 -0.0455 0.153 Uiso 1 1 calc R . . C15 C 0.363(3) 0.303(3) -0.0282(12) 0.12(2) Uani 1 1 d DU . . H15G H 0.4022 0.3302 -0.0389 0.144 Uiso 1 1 calc R . . H15H H 0.3638 0.2625 -0.0519 0.144 Uiso 1 1 calc R . . C16 C 0.3935(19) 0.255(3) 0.0215(13) 0.071(14) Uani 1 1 d DU . . H16A H 0.4256 0.1908 0.0183 0.085 Uiso 1 1 calc R . . H16B H 0.4356 0.2732 0.0366 0.085 Uiso 1 1 calc R . . O5 O -0.386(3) 0.821(2) 0.3838(12) 0.123(15) Uani 1 1 d DU . . C17 C -0.357(2) 0.877(3) 0.4060(16) 0.091(17) Uani 1 1 d DU . . H17A H -0.3369 0.9082 0.3815 0.109 Uiso 1 1 calc R . . H17B H -0.3041 0.8409 0.4275 0.109 Uiso 1 1 calc R . . C18 C -0.435(3) 0.944(2) 0.4347(18) 0.11(2) Uani 1 1 d DU . . H18A H -0.4698 0.9989 0.4151 0.132 Uiso 1 1 calc R . . H18B H -0.4105 0.9581 0.4633 0.132 Uiso 1 1 calc R . . C19 C -0.494(3) 0.898(3) 0.449(2) 0.11(2) Uani 1 1 d DU . . H19G H -0.5565 0.9320 0.4357 0.132 Uiso 1 1 calc R . . H19H H -0.4965 0.8903 0.4837 0.132 Uiso 1 1 calc R . . C20 C -0.446(3) 0.808(2) 0.4266(17) 0.100(19) Uani 1 1 d DU . . H20G H -0.4916 0.7906 0.4141 0.120 Uiso 1 1 calc R . . H20H H -0.4070 0.7617 0.4505 0.120 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.0434(5) 0.0485(5) 0.0432(5) -0.0059(4) 0.0063(4) -0.0224(4) U2 0.0481(5) 0.0513(5) 0.0451(5) -0.0004(4) 0.0036(4) -0.0276(4) U3 0.0547(6) 0.0577(5) 0.0452(6) -0.0116(4) 0.0021(4) -0.0186(5) U4 0.0434(5) 0.0674(6) 0.0679(7) -0.0274(5) 0.0093(4) -0.0255(5) O1A 0.056(10) 0.058(9) 0.046(9) 0.000(7) 0.002(7) -0.023(8) O2A 0.045(9) 0.056(9) 0.049(9) 0.007(7) 0.012(7) -0.027(7) O3A 0.050(9) 0.049(8) 0.030(8) 0.001(6) 0.013(6) -0.020(7) O4A 0.056(9) 0.074(10) 0.049(10) -0.005(8) 0.006(7) -0.040(8) N1A 0.033(10) 0.048(10) 0.054(12) -0.004(8) 0.007(8) -0.020(8) N2A 0.048(11) 0.062(11) 0.031(10) -0.003(8) 0.008(8) -0.015(9) C1A 0.043(14) 0.062(15) 0.076(19) -0.025(13) 0.016(13) -0.020(12) C2A 0.050(14) 0.069(15) 0.046(15) -0.010(11) 0.008(11) -0.036(12) C3A 0.043(14) 0.11(2) 0.09(2) -0.009(16) 0.030(13) -0.052(14) C4A 0.064(17) 0.11(2) 0.068(19) -0.001(15) 0.014(14) -0.061(16) C5A 0.083(13) 0.106(13) 0.091(13) 0.001(10) 0.013(10) -0.049(10) C6A 0.079(19) 0.10(2) 0.045(16) 0.021(13) 0.022(14) -0.028(16) C7A 0.061(16) 0.074(17) 0.063(18) -0.004(13) -0.005(13) -0.032(14) C8A 0.044(13) 0.071(15) 0.042(14) -0.015(11) 0.006(10) -0.023(12) C9A 0.067(15) 0.043(12) 0.031(12) -0.009(9) -0.003(10) -0.031(12) C10A 0.054(15) 0.072(16) 0.057(16) -0.005(13) -0.002(12) -0.020(13) C11A 0.10(2) 0.050(14) 0.057(16) -0.010(11) 0.017(14) -0.030(15) C12A 0.064(16) 0.054(14) 0.045(14) -0.008(11) 0.004(12) -0.024(13) C13A 0.058(14) 0.045(12) 0.037(13) -0.008(10) 0.001(10) -0.018(12) C14A 0.056(15) 0.046(13) 0.054(15) 0.007(11) -0.011(11) -0.025(12) C15A 0.027(11) 0.082(16) 0.033(13) -0.009(11) 0.001(9) -0.012(11) C16A 0.087(18) 0.051(13) 0.035(13) 0.000(10) 0.001(12) -0.048(13) C17A 0.050(14) 0.069(15) 0.046(15) -0.010(11) 0.008(11) -0.036(12) C18A 0.056(14) 0.068(15) 0.023(12) -0.006(10) -0.001(10) -0.015(13) C19A 0.073(11) 0.079(11) 0.065(11) 0.006(9) -0.003(9) -0.041(9) C20A 0.071(11) 0.081(11) 0.075(12) 0.006(9) 0.003(9) -0.039(9) C21A 0.072(17) 0.097(19) 0.043(15) -0.007(14) -0.006(12) -0.047(16) O1B 0.051(10) 0.056(9) 0.064(11) -0.007(8) 0.005(8) -0.015(8) O2B 0.045(9) 0.052(9) 0.051(9) 0.003(7) -0.002(7) -0.019(7) O3B 0.039(8) 0.044(8) 0.045(8) -0.002(6) 0.005(6) -0.027(7) O4B 0.051(9) 0.051(9) 0.052(10) -0.023(7) 0.013(7) -0.025(8) N1B 0.075(13) 0.047(10) 0.046(11) 0.003(8) -0.008(9) -0.047(10) N2B 0.060(12) 0.047(10) 0.047(11) 0.007(8) 0.010(9) -0.035(10) C1B 0.035(13) 0.064(15) 0.065(17) -0.005(12) 0.015(11) -0.020(12) C2B 0.041(13) 0.047(12) 0.045(13) 0.000(10) -0.005(10) -0.021(11) C3B 0.040(12) 0.036(11) 0.055(14) 0.007(9) 0.000(10) -0.026(10) C4B 0.049(15) 0.10(2) 0.079(19) -0.008(15) 0.002(13) -0.044(15) C5B 0.051(16) 0.09(2) 0.063(18) -0.006(14) 0.014(13) -0.012(16) C6B 0.07(2) 0.09(2) 0.065(18) 0.005(14) 0.013(14) -0.041(17) C7B 0.063(16) 0.069(16) 0.051(15) 0.012(11) -0.004(12) -0.045(14) C8B 0.042(13) 0.069(16) 0.086(19) 0.012(13) 0.003(12) -0.037(12) C9B 0.052(10) 0.038(8) 0.053(10) -0.006(7) -0.009(8) -0.034(8) C10B 0.080(18) 0.046(13) 0.10(2) -0.015(13) 0.008(15) -0.052(14) C11B 0.10(2) 0.058(16) 0.067(19) -0.019(13) 0.006(16) -0.036(16) C12B 0.09(2) 0.038(14) 0.10(2) -0.028(14) 0.019(19) 0.000(16) C13B 0.070(17) 0.073(16) 0.058(17) -0.040(13) 0.024(13) -0.036(14) C14B 0.044(14) 0.036(12) 0.11(2) 0.007(12) -0.027(14) -0.019(11) C15B 0.054(14) 0.023(10) 0.057(15) -0.005(9) 0.019(11) -0.014(10) C16B 0.066(16) 0.079(17) 0.020(12) -0.003(11) 0.006(10) -0.029(14) C17B 0.037(12) 0.032(11) 0.072(16) 0.002(10) 0.017(11) -0.019(10) C18B 0.045(14) 0.074(17) 0.038(14) 0.007(12) 0.001(11) -0.020(13) C19B 0.064(17) 0.10(2) 0.047(15) -0.002(14) -0.022(12) -0.043(16) C20B 0.061(11) 0.057(10) 0.071(11) 0.002(9) 0.009(9) -0.014(8) C21B 0.034(12) 0.044(13) 0.092(19) -0.006(12) -0.003(12) -0.008(11) O1C 0.049(9) 0.063(9) 0.054(10) 0.002(7) -0.005(7) -0.028(8) O2C 0.062(10) 0.044(8) 0.056(10) -0.008(7) 0.012(8) -0.028(8) O3C 0.038(8) 0.070(10) 0.072(11) -0.019(8) -0.014(8) -0.013(8) O4C 0.044(9) 0.060(9) 0.084(13) -0.038(8) 0.022(8) -0.027(8) N1C 0.084(15) 0.050(11) 0.032(11) -0.004(8) -0.004(9) -0.024(11) N2C 0.071(14) 0.067(13) 0.042(12) -0.003(9) -0.019(10) -0.002(11) C1C 0.069(16) 0.041(12) 0.046(14) -0.019(10) 0.017(12) -0.028(12) C2C 0.059(15) 0.028(11) 0.071(17) 0.004(10) 0.005(13) -0.026(11) C3C 0.031(11) 0.060(14) 0.065(16) -0.012(11) 0.032(11) -0.029(11) C4C 0.080(12) 0.084(11) 0.077(12) -0.016(9) 0.020(9) -0.042(9) C5C 0.094(13) 0.103(13) 0.106(14) -0.014(10) 0.010(10) -0.041(10) C6C 0.059(10) 0.066(10) 0.074(11) -0.009(9) -0.001(9) -0.030(8) C7C 0.073(11) 0.053(10) 0.052(10) -0.006(8) 0.008(9) -0.028(8) C8C 0.082(12) 0.068(11) 0.066(11) -0.010(9) 0.009(9) -0.031(9) C9C 0.066(10) 0.057(10) 0.042(10) -0.001(8) 0.002(8) -0.016(8) C10C 0.072(11) 0.064(10) 0.055(10) -0.008(8) -0.003(9) -0.024(8) C11C 0.070(11) 0.067(11) 0.067(11) -0.005(9) -0.006(9) -0.025(9) C12C 0.096(13) 0.094(12) 0.093(13) -0.016(10) -0.012(10) -0.044(10) C13C 0.074(12) 0.095(12) 0.076(12) -0.016(9) -0.002(9) -0.028(9) C14C 0.076(12) 0.071(11) 0.072(11) -0.012(9) -0.009(9) -0.024(9) C15C 0.088(12) 0.089(12) 0.082(12) -0.017(9) -0.009(10) -0.033(9) C16C 0.088(11) 0.084(10) 0.079(11) -0.007(7) -0.006(7) -0.030(7) C17C 0.065(11) 0.069(11) 0.063(11) -0.021(9) -0.012(9) -0.027(8) C18C 0.083(12) 0.081(12) 0.091(13) -0.009(10) -0.011(10) -0.041(9) C19C 0.083(12) 0.088(12) 0.080(12) -0.015(10) 0.001(10) -0.020(9) C20C 0.132(14) 0.126(14) 0.123(14) -0.011(8) 0.000(8) -0.052(9) C21C 0.122(13) 0.121(13) 0.111(13) -0.022(8) -0.008(8) -0.046(8) O1D 0.062(10) 0.064(10) 0.081(12) -0.026(9) -0.009(9) -0.027(9) O2D 0.064(11) 0.067(10) 0.099(13) -0.045(9) 0.015(9) -0.050(9) O3D 0.049(9) 0.052(9) 0.054(10) -0.019(7) 0.001(7) -0.023(8) O4D 0.068(10) 0.052(9) 0.047(9) -0.025(7) 0.023(7) -0.024(8) N1D 0.053(13) 0.059(13) 0.107(18) -0.031(11) 0.029(12) -0.031(11) N2D 0.057(13) 0.072(13) 0.078(15) -0.040(11) 0.013(11) -0.041(11) C1D 0.072(18) 0.066(16) 0.073(19) -0.009(13) -0.001(14) -0.040(16) C2D 0.035(12) 0.084(17) 0.040(13) -0.006(11) 0.001(10) -0.031(13) C3D 0.032(12) 0.071(16) 0.09(2) -0.010(13) 0.005(12) -0.029(12) C4D 0.045(15) 0.067(16) 0.10(2) -0.014(14) -0.014(13) -0.024(13) C5D 0.069(18) 0.063(16) 0.09(2) 0.015(14) -0.019(15) -0.042(15) C6D 0.08(2) 0.072(17) 0.075(19) 0.008(14) -0.008(15) -0.054(16) C7D 0.054(16) 0.069(16) 0.065(17) -0.019(12) 0.005(12) -0.028(14) C8D 0.062(17) 0.090(18) 0.11(2) -0.041(16) 0.012(15) -0.063(15) C9D 0.054(15) 0.049(13) 0.084(18) -0.027(12) 0.047(13) -0.035(12) C10D 0.065(19) 0.081(19) 0.12(3) -0.038(18) 0.014(18) -0.038(16) C11D 0.027(12) 0.085(18) 0.09(2) -0.046(15) 0.030(13) -0.022(13) C12D 0.077(19) 0.086(19) 0.09(2) -0.043(16) 0.008(16) -0.045(16) C13D 0.11(2) 0.088(18) 0.048(16) -0.019(13) 0.016(15) -0.069(17) C14D 0.080(18) 0.092(19) 0.060(17) -0.042(14) 0.033(14) -0.056(16) C15D 0.063(17) 0.11(2) 0.08(2) -0.054(17) 0.008(14) -0.056(17) C16D 0.045(13) 0.072(15) 0.074(18) -0.014(13) 0.017(12) -0.047(12) C17D 0.047(14) 0.065(16) 0.077(19) -0.040(13) 0.003(12) -0.034(13) C18D 0.054(15) 0.082(18) 0.08(2) -0.053(15) -0.001(13) -0.043(14) C19D 0.089(19) 0.054(14) 0.078(19) -0.030(13) 0.042(15) -0.043(15) C20D 0.098(13) 0.079(11) 0.099(13) -0.009(9) 0.011(10) -0.053(9) C21D 0.078(11) 0.079(11) 0.080(12) -0.016(9) 0.017(9) -0.047(9) O1E 0.036(8) 0.062(10) 0.052(10) -0.009(7) 0.008(7) -0.015(8) O2E 0.075(11) 0.056(9) 0.036(9) -0.011(7) 0.019(8) -0.032(8) O3E 0.066(10) 0.053(9) 0.044(9) -0.004(7) 0.006(7) -0.030(8) O4E 0.059(9) 0.050(8) 0.055(10) -0.002(7) -0.004(7) -0.032(8) N1E 0.069(13) 0.059(12) 0.055(13) -0.014(9) 0.010(10) -0.041(10) N2E 0.090(15) 0.074(13) 0.039(12) -0.021(9) 0.027(10) -0.062(12) C1E 0.065(16) 0.059(15) 0.047(15) -0.015(12) 0.009(12) -0.028(14) C2E 0.044(13) 0.051(13) 0.050(15) -0.017(11) 0.005(10) -0.015(11) C3E 0.050(14) 0.063(15) 0.053(15) -0.017(11) 0.009(11) -0.028(12) C4E 0.053(15) 0.071(16) 0.058(16) -0.012(12) 0.011(12) -0.028(13) C5E 0.050(14) 0.082(18) 0.045(15) -0.013(12) 0.014(11) -0.027(14) C6E 0.034(13) 0.066(16) 0.080(19) -0.037(14) -0.004(12) -0.015(12) C7E 0.047(13) 0.049(13) 0.059(16) -0.012(11) -0.013(11) -0.023(11) C8E 0.10(2) 0.055(14) 0.023(12) -0.006(10) 0.013(12) -0.036(14) C9E 0.070(16) 0.057(13) 0.023(12) -0.008(10) -0.003(11) -0.038(12) C10E 0.10(2) 0.057(15) 0.058(17) -0.006(12) 0.018(15) -0.049(16) C11E 0.11(2) 0.083(19) 0.064(19) -0.034(15) 0.045(17) -0.065(19) C12E 0.08(2) 0.11(2) 0.07(2) -0.024(17) 0.022(16) -0.052(19) C13E 0.085(19) 0.096(19) 0.042(15) -0.004(13) 0.003(13) -0.070(16) C14E 0.070(16) 0.065(14) 0.025(12) -0.015(10) -0.005(11) -0.037(13) C15E 0.057(14) 0.032(11) 0.058(16) -0.004(10) 0.000(11) -0.024(11) C16E 0.057(15) 0.041(12) 0.068(18) -0.012(11) 0.014(12) -0.024(12) C17E 0.058(16) 0.039(13) 0.066(18) -0.033(12) 0.003(13) -0.010(12) C18E 0.038(13) 0.047(13) 0.052(15) -0.005(10) -0.003(10) -0.017(11) C19E 0.057(15) 0.055(14) 0.060(17) -0.002(11) -0.011(12) -0.028(12) C20E 0.061(15) 0.075(15) 0.043(14) -0.002(11) -0.008(11) -0.050(13) C21E 0.083(18) 0.049(13) 0.064(17) -0.014(11) 0.004(13) -0.048(13) O1F 0.047(8) 0.043(8) 0.044(9) -0.007(6) 0.004(6) -0.016(7) O2F 0.047(9) 0.046(8) 0.047(9) -0.013(6) 0.011(7) -0.015(7) O3F 0.055(9) 0.071(10) 0.038(9) -0.014(7) 0.016(7) -0.037(8) O4F 0.062(10) 0.086(11) 0.049(10) -0.031(8) 0.027(8) -0.040(9) N1F 0.094(16) 0.069(13) 0.045(12) -0.012(9) 0.001(11) -0.063(13) N2F 0.068(13) 0.042(10) 0.056(13) -0.004(9) -0.015(10) -0.033(10) C1F 0.058(15) 0.037(12) 0.044(13) 0.008(9) 0.019(11) -0.020(11) C2F 0.062(15) 0.028(11) 0.054(14) -0.013(9) 0.017(11) -0.024(11) C3F 0.09(2) 0.073(16) 0.046(15) -0.004(12) -0.014(13) -0.047(16) C4F 0.074(19) 0.051(14) 0.066(18) -0.011(12) 0.000(14) -0.016(14) C5F 0.080(18) 0.075(17) 0.042(15) -0.013(12) 0.006(12) -0.030(15) C6F 0.058(14) 0.039(12) 0.042(13) 0.004(9) 0.003(11) -0.024(11) C7F 0.052(14) 0.038(12) 0.056(15) -0.017(10) -0.007(11) -0.013(12) C8F 0.085(19) 0.068(16) 0.059(18) 0.009(13) -0.017(14) -0.034(15) C9F 0.09(2) 0.060(16) 0.08(2) -0.024(14) -0.006(16) -0.047(17) C10F 0.08(2) 0.087(19) 0.060(18) -0.012(14) -0.021(15) -0.042(17) C11F 0.067(19) 0.12(3) 0.10(3) 0.00(2) -0.001(18) -0.063(18) C12F 0.11(3) 0.09(2) 0.08(2) 0.031(17) -0.022(19) -0.06(2) C13F 0.061(18) 0.069(18) 0.11(3) -0.015(16) 0.009(17) -0.033(16) C14F 0.08(2) 0.079(19) 0.09(2) -0.020(16) 0.000(16) -0.069(17) C15F 0.085(18) 0.041(13) 0.043(14) -0.016(10) -0.004(13) -0.030(13) C16F 0.086(18) 0.018(10) 0.053(15) 0.002(9) 0.008(13) -0.019(12) C17F 0.070(17) 0.058(14) 0.046(15) -0.003(11) -0.005(12) -0.044(13) C18F 0.059(16) 0.039(12) 0.066(17) -0.022(11) 0.019(13) -0.023(12) C19F 0.11(2) 0.09(2) 0.052(17) -0.012(14) 0.027(16) -0.061(18) C20F 0.11(2) 0.047(13) 0.044(15) -0.017(11) 0.041(15) -0.039(15) C21F 0.063(16) 0.080(17) 0.042(14) 0.002(12) 0.003(12) -0.045(14) O1 0.123(9) 0.128(9) 0.122(9) -0.004(5) 0.006(6) -0.060(6) C1 0.097(10) 0.095(10) 0.096(10) -0.010(6) 0.001(6) -0.041(6) C2 0.057(8) 0.054(7) 0.056(8) -0.004(5) 0.002(5) -0.023(5) C3 0.084(9) 0.085(9) 0.087(10) -0.004(6) 0.000(6) -0.042(6) C4 0.107(11) 0.110(11) 0.110(12) -0.003(6) 0.002(6) -0.050(7) O2 0.113(8) 0.108(8) 0.107(8) -0.011(5) -0.004(5) -0.052(6) C5 0.115(12) 0.113(12) 0.112(12) -0.007(6) 0.003(6) -0.050(7) C6 0.140(14) 0.137(14) 0.138(14) -0.009(6) 0.001(6) -0.062(8) C7 0.164(16) 0.159(16) 0.162(16) -0.014(6) -0.002(6) -0.073(9) C8 0.103(11) 0.100(11) 0.100(11) -0.009(6) 0.000(6) -0.044(6) O3 0.186(12) 0.183(12) 0.185(13) -0.006(6) 0.002(6) -0.082(7) C9 0.087(17) 0.085(17) 0.086(17) -0.006(6) -0.002(6) -0.040(9) C10 0.033(10) 0.032(10) 0.032(10) -0.002(6) 0.000(6) -0.015(6) C11 0.093(14) 0.097(14) 0.094(14) -0.003(6) 0.004(6) -0.044(8) C12 0.074(12) 0.077(12) 0.080(12) -0.007(6) 0.003(6) -0.037(7) O4 0.121(15) 0.121(15) 0.119(15) -0.007(6) 0.002(6) -0.054(8) C13 0.10(2) 0.10(2) 0.10(2) -0.006(6) 0.002(6) -0.047(10) C14 0.13(2) 0.13(2) 0.13(2) -0.009(6) 0.003(6) -0.058(12) C15 0.12(2) 0.12(2) 0.12(2) -0.004(6) 0.003(6) -0.054(11) C16 0.070(15) 0.073(15) 0.071(15) -0.003(6) 0.001(6) -0.033(8) O5 0.124(16) 0.123(15) 0.124(16) -0.009(6) 0.002(6) -0.057(8) C17 0.091(18) 0.092(18) 0.090(18) -0.004(6) 0.002(6) -0.041(9) C18 0.11(2) 0.11(2) 0.11(2) -0.008(6) 0.000(6) -0.050(11) C19 0.11(2) 0.11(2) 0.11(2) -0.006(6) 0.001(6) -0.049(11) C20 0.10(2) 0.100(19) 0.10(2) -0.008(6) 0.002(6) -0.045(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O4B 2.191(13) . ? U1 O2A 2.226(13) . ? U1 O2F 2.266(12) . ? U1 O3A 2.388(13) . ? U1 O1F 2.442(13) . ? U1 O3B 2.473(12) . ? U1 N1A 2.580(17) . ? U1 N2A 2.586(16) . ? U1 U2 3.7900(13) . ? U2 O4E 2.163(15) . ? U2 O4A 2.214(15) . ? U2 O2B 2.237(13) . ? U2 O3B 2.408(12) . ? U2 O1F 2.496(13) . ? U2 O3A 2.539(14) . ? U2 N1B 2.589(17) . ? U2 N2B 2.628(16) . ? U3 O4D 2.183(14) . ? U3 O2C 2.230(15) . ? U3 O2E 2.310(13) . ? U3 O3C 2.352(14) . ? U3 O1E 2.445(14) . ? U3 O3D 2.523(12) . ? U3 N2C 2.601(18) . ? U3 N1C 2.608(18) . ? U3 U4 3.7924(12) . ? U4 O4F 2.168(17) . ? U4 O4C 2.181(16) . ? U4 O2D 2.246(14) . ? U4 O3D 2.427(14) . ? U4 O1E 2.496(12) . ? U4 O3C 2.522(15) . ? U4 N1D 2.581(18) . ? U4 N2D 2.601(17) . ? O1A C1A 1.35(3) . ? O1A O2A 2.718(19) . ? O2A C2A 1.32(2) . ? O2A N1A 2.82(2) . ? O2A O3A 4.414(18) . ? O3A C17A 1.33(2) . ? O3A O4A 2.61(2) . ? O3A N2A 2.86(2) . ? O4A C18A 1.37(2) . ? N1A C7A 1.32(3) . ? N1A C8A 1.48(2) . ? N1A N2A 3.08(2) . ? N2A C15A 1.34(3) . ? N2A C14A 1.48(3) . ? C1A C6A 1.38(3) . ? C1A C2A 1.42(3) . ? C2A C3A 1.44(3) . ? C3A C4A 1.39(3) . ? C3A C7A 1.44(3) . ? C4A C5A 1.34(3) . ? C5A C6A 1.37(4) . ? C8A C9A 1.49(2) . ? C9A C10A 1.37(3) . ? C9A C14A 1.41(3) . ? C10A C11A 1.39(3) . ? C11A C12A 1.42(3) . ? C12A C13A 1.33(3) . ? C13A C14A 1.35(3) . ? C15A C16A 1.41(3) . ? C16A C21A 1.39(3) . ? C16A C17A 1.41(3) . ? C17A C18A 1.42(3) . ? C18A C19A 1.41(3) . ? C19A C20A 1.37(3) . ? C20A C21A 1.34(3) . ? O1B C1B 1.37(3) . ? O1B O2B 2.685(18) . ? O2B C2B 1.32(2) . ? O2B N1B 2.82(2) . ? O2B O3B 4.439(18) . ? O3B C17B 1.31(2) . ? O3B O4B 2.618(19) . ? O3B N2B 2.92(2) . ? O4B C18B 1.32(3) . ? N1B C7B 1.35(2) . ? N1B C8B 1.50(2) . ? N1B N2B 3.13(3) . ? N2B C15B 1.31(2) . ? N2B C14B 1.46(3) . ? C1B C6B 1.34(3) . ? C1B C2B 1.42(3) . ? C2B C3B 1.37(3) . ? C3B C4B 1.43(3) . ? C3B C7B 1.43(3) . ? C4B C5B 1.39(3) . ? C5B C6B 1.44(3) . ? C8B C9B 1.48(3) . ? C9B C14B 1.37(3) . ? C9B C10B 1.39(3) . ? C10B C11B 1.39(3) . ? C11B C12B 1.38(3) . ? C12B C13B 1.41(3) . ? C13B C14B 1.38(3) . ? C15B C16B 1.46(3) . ? C16B C21B 1.38(3) . ? C16B C17B 1.42(3) . ? C17B C18B 1.40(3) . ? C18B C19B 1.37(3) . ? C19B C20B 1.43(3) . ? C20B C21B 1.40(3) . ? O1C C1C 1.39(2) . ? O1C O2C 2.74(2) . ? O2C C2C 1.35(2) . ? O2C N1C 2.83(2) . ? O2C O3C 4.40(2) . ? O3C C17C 1.34(3) . ? O3C O4C 2.614(17) . ? O3C N2C 2.84(2) . ? O4C C18C 1.34(3) . ? N1C C7C 1.31(3) . ? N1C C8C 1.42(3) . ? N1C N2C 3.07(3) . ? N2C C15C 1.27(3) . ? N2C C14C 1.50(3) . ? C1C C6C 1.41(3) . ? C1C C2C 1.42(3) . ? C2C C3C 1.39(3) . ? C3C C4C 1.37(3) . ? C3C C7C 1.43(3) . ? C4C C5C 1.38(4) . ? C5C C6C 1.39(3) . ? C8C C9C 1.55(3) . ? C9C C14C 1.33(3) . ? C9C C10C 1.39(3) . ? C10C C11C 1.40(3) . ? C11C C12C 1.38(3) . ? C12C C13C 1.39(3) . ? C13C C14C 1.45(3) . ? C15C C16C 1.51(3) . ? C16C C17C 1.38(3) . ? C16C C21C 1.44(4) . ? C17C C18C 1.46(3) . ? C18C C19C 1.37(3) . ? C19C C20C 1.40(4) . ? C20C C21C 1.40(4) . ? O1D C1D 1.39(3) . ? O1D O2D 2.675(19) . ? O2D C2D 1.35(2) . ? O2D N1D 2.80(2) . ? O2D O3D 4.43(2) . ? O3D C17D 1.35(3) . ? O3D O4D 2.607(19) . ? O3D N2D 2.93(2) . ? O4D C18D 1.37(2) . ? N1D C7D 1.24(3) . ? N1D C8D 1.44(2) . ? N1D N2D 3.24(3) . ? N2D C15D 1.29(3) . ? N2D C14D 1.46(3) . ? C1D C2D 1.36(3) . ? C1D C6D 1.40(3) . ? C2D C3D 1.37(3) . ? C3D C4D 1.38(3) . ? C3D C7D 1.46(3) . ? C4D C5D 1.38(3) . ? C5D C6D 1.38(3) . ? C8D C9D 1.59(3) . ? C9D C14D 1.40(3) . ? C9D C10D 1.42(3) . ? C10D C11D 1.30(3) . ? C11D C12D 1.38(3) . ? C12D C13D 1.35(3) . ? C13D C14D 1.35(3) . ? C15D C16D 1.46(3) . ? C16D C17D 1.40(3) . ? C16D C21D 1.43(3) . ? C17D C18D 1.40(3) . ? C18D C19D 1.40(3) . ? C19D C20D 1.40(3) . ? C20D C21D 1.29(3) . ? O1E C1E 1.35(2) . ? O1E O2E 2.622(17) . ? O2E C2E 1.31(2) . ? O2E N1E 2.62(2) . ? O2E O3E 7.28(2) . ? O3E C17E 1.35(2) . ? O3E O4E 2.72(2) . ? O3E N2E 4.09(2) . ? O4E C18E 1.35(2) . ? N1E C7E 1.27(3) . ? N1E C8E 1.47(2) . ? N1E N2E 3.17(3) . ? N2E C15E 1.25(2) . ? N2E C14E 1.41(3) . ? C1E C2E 1.36(3) . ? C1E C6E 1.38(3) . ? C2E C3E 1.45(3) . ? C3E C4E 1.41(3) . ? C3E C7E 1.44(3) . ? C4E C5E 1.37(3) . ? C5E C6E 1.40(3) . ? C8E C9E 1.52(3) . ? C9E C10E 1.35(3) . ? C9E C14E 1.38(3) . ? C10E C11E 1.42(3) . ? C11E C12E 1.33(3) . ? C12E C13E 1.41(3) . ? C13E C14E 1.39(3) . ? C15E C16E 1.50(3) . ? C16E C17E 1.37(3) . ? C16E C21E 1.42(3) . ? C17E C18E 1.41(3) . ? C18E C19E 1.40(3) . ? C19E C20E 1.38(3) . ? C20E C21E 1.35(3) . ? O1F C1F 1.37(2) . ? O1F O2F 2.651(19) . ? O2F C2F 1.37(2) . ? O2F N1F 2.59(2) . ? O2F O3F 7.163(19) . ? O3F C17F 1.37(2) . ? O3F O4F 2.752(19) . ? O3F N2F 4.08(2) . ? O4F C18F 1.32(3) . ? N1F C7F 1.27(2) . ? N1F C8F 1.51(3) . ? N1F N2F 3.21(2) . ? N2F C15F 1.30(2) . ? N2F C14F 1.43(3) . ? C1F C6F 1.37(3) . ? C1F C2F 1.46(3) . ? C2F C3F 1.45(3) . ? C3F C7F 1.38(3) . ? C3F C4F 1.42(3) . ? C4F C5F 1.36(3) . ? C5F C6F 1.41(3) . ? C8F C9F 1.46(3) . ? C9F C10F 1.37(3) . ? C9F C14F 1.42(3) . ? C10F C11F 1.39(3) . ? C11F C12F 1.43(4) . ? C12F C13F 1.29(3) . ? C13F C14F 1.41(3) . ? C15F C16F 1.41(3) . ? C16F C17F 1.37(3) . ? C16F C21F 1.46(3) . ? C17F C18F 1.40(3) . ? C18F C19F 1.39(3) . ? C19F C20F 1.48(3) . ? C20F C21F 1.35(3) . ? O1 C1 1.46(3) . ? O1 C4 1.49(3) . ? C1 C2 1.45(3) . ? C2 C3 1.52(3) . ? C3 C4 1.47(3) . ? O2 C8 1.40(3) . ? O2 C5 1.47(3) . ? C5 C6 1.50(4) . ? C6 C7 1.54(4) . ? C7 C8 1.49(4) . ? O3 C9 1.35(5) . ? O3 C12 1.46(4) . ? C9 C10 1.51(5) . ? C10 C11 1.37(4) . ? C11 C12 1.36(5) . ? O4 C13 1.40(6) . ? O4 C16 1.40(6) . ? C13 C14 1.52(6) . ? C14 C15 1.53(7) . ? C15 C16 1.52(5) . ? O5 C17 1.40(6) . ? O5 C20 1.59(6) . ? C17 C18 1.52(6) . ? C18 C19 1.51(7) . ? C19 C20 1.52(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4B U1 O2A 100.1(5) . . ? O4B U1 O2F 155.0(4) . . ? O2A U1 O2F 88.7(3) . . ? O4B U1 O3A 88.4(5) . . ? O2A U1 O3A 146.2(5) . . ? O2F U1 O3A 97.2(3) . . ? O4B U1 O1F 135.3(4) . . ? O2A U1 O1F 84.4(4) . . ? O2F U1 O1F 68.4(5) . . ? O3A U1 O1F 67.4(3) . . ? O4B U1 O3B 68.0(5) . . ? O2A U1 O3B 85.5(5) . . ? O2F U1 O3B 136.5(4) . . ? O3A U1 O3B 67.4(4) . . ? O1F U1 O3B 68.1(3) . . ? O4B U1 N1A 78.4(5) . . ? O2A U1 N1A 71.5(5) . . ? O2F U1 N1A 82.4(4) . . ? O3A U1 N1A 142.3(5) . . ? O1F U1 N1A 142.5(4) . . ? O3B U1 N1A 134.9(4) . . ? O4B U1 N2A 82.2(5) . . ? O2A U1 N2A 143.2(6) . . ? O2F U1 N2A 77.0(4) . . ? O3A U1 N2A 70.1(5) . . ? O1F U1 N2A 119.8(4) . . ? O3B U1 N2A 127.8(5) . . ? N1A U1 N2A 73.1(6) . . ? O4B U1 U2 96.9(4) . . ? O2A U1 U2 105.1(4) . . ? O2F U1 U2 103.3(4) . . ? O3A U1 U2 41.2(3) . . ? O1F U1 U2 40.4(3) . . ? O3B U1 U2 38.4(3) . . ? N1A U1 U2 173.4(3) . . ? N2A U1 U2 111.2(4) . . ? O4E U2 O4A 152.7(4) . . ? O4E U2 O2B 91.4(3) . . ? O4A U2 O2B 97.6(5) . . ? O4E U2 O3B 99.4(4) . . ? O4A U2 O3B 87.5(5) . . ? O2B U2 O3B 145.7(5) . . ? O4E U2 O1F 76.2(5) . . ? O4A U2 O1F 130.3(4) . . ? O2B U2 O1F 83.1(4) . . ? O3B U2 O1F 68.3(3) . . ? O4E U2 O3A 140.5(3) . . ? O4A U2 O3A 66.3(5) . . ? O2B U2 O3A 85.0(4) . . ? O3B U2 O3A 66.1(4) . . ? O1F U2 O3A 64.3(3) . . ? O4E U2 N1B 84.0(4) . . ? O4A U2 N1B 74.8(5) . . ? O2B U2 N1B 71.1(5) . . ? O3B U2 N1B 142.1(5) . . ? O1F U2 N1B 147.0(4) . . ? O3A U2 N1B 130.7(5) . . ? O4E U2 N2B 76.3(4) . . ? O4A U2 N2B 81.3(5) . . ? O2B U2 N2B 143.7(5) . . ? O3B U2 N2B 70.6(5) . . ? O1F U2 N2B 125.1(3) . . ? O3A U2 N2B 125.9(5) . . ? N1B U2 N2B 73.7(5) . . ? O4E U2 U1 107.2(4) . . ? O4A U2 U1 95.1(4) . . ? O2B U2 U1 106.0(4) . . ? O3B U2 U1 39.7(3) . . ? O1F U2 U1 39.3(3) . . ? O3A U2 U1 38.3(3) . . ? N1B U2 U1 168.7(4) . . ? N2B U2 U1 110.3(4) . . ? O4D U3 O2C 95.7(4) . . ? O4D U3 O2E 159.9(5) . . ? O2C U3 O2E 90.4(4) . . ? O4D U3 O3C 90.8(4) . . ? O2C U3 O3C 147.6(5) . . ? O2E U3 O3C 94.3(4) . . ? O4D U3 O1E 132.7(4) . . ? O2C U3 O1E 83.9(3) . . ? O2E U3 O1E 66.9(5) . . ? O3C U3 O1E 68.8(4) . . ? O4D U3 O3D 66.8(5) . . ? O2C U3 O3D 85.4(3) . . ? O2E U3 O3D 132.9(5) . . ? O3C U3 O3D 68.1(3) . . ? O1E U3 O3D 66.1(5) . . ? O4D U3 N2C 87.5(4) . . ? O2C U3 N2C 142.0(5) . . ? O2E U3 N2C 76.1(4) . . ? O3C U3 N2C 69.8(6) . . ? O1E U3 N2C 120.8(5) . . ? O3D U3 N2C 129.6(4) . . ? O4D U3 N1C 80.1(4) . . ? O2C U3 N1C 71.1(5) . . ? O2E U3 N1C 83.8(4) . . ? O3C U3 N1C 141.3(6) . . ? O1E U3 N1C 141.3(4) . . ? O3D U3 N1C 137.1(4) . . ? N2C U3 N1C 72.2(6) . . ? O4D U3 U4 96.9(3) . . ? O2C U3 U4 107.0(3) . . ? O2E U3 U4 99.6(3) . . ? O3C U3 U4 40.5(4) . . ? O1E U3 U4 40.4(3) . . ? O3D U3 U4 39.1(3) . . ? N2C U3 U4 110.1(4) . . ? N1C U3 U4 176.2(4) . . ? O4F U4 O4C 149.3(3) . . ? O4F U4 O2D 92.0(6) . . ? O4C U4 O2D 104.6(4) . . ? O4F U4 O3D 97.9(5) . . ? O4C U4 O3D 84.2(4) . . ? O2D U4 O3D 143.2(5) . . ? O4F U4 O1E 76.4(5) . . ? O4C U4 O1E 130.9(3) . . ? O2D U4 O1E 81.6(5) . . ? O3D U4 O1E 66.7(5) . . ? O4F U4 O3C 141.7(3) . . ? O4C U4 O3C 67.1(5) . . ? O2D U4 O3C 83.4(4) . . ? O3D U4 O3C 67.0(3) . . ? O1E U4 O3C 65.4(3) . . ? O4F U4 N1D 88.9(6) . . ? O4C U4 N1D 73.1(5) . . ? O2D U4 N1D 70.5(6) . . ? O3D U4 N1D 144.5(5) . . ? O1E U4 N1D 148.0(6) . . ? O3C U4 N1D 124.2(5) . . ? O4F U4 N2D 75.1(6) . . ? O4C U4 N2D 76.7(5) . . ? O2D U4 N2D 145.5(6) . . ? O3D U4 N2D 71.1(5) . . ? O1E U4 N2D 124.3(5) . . ? O3C U4 N2D 126.2(5) . . ? N1D U4 N2D 77.3(6) . . ? O4F U4 U3 108.6(3) . . ? O4C U4 U3 93.1(4) . . ? O2D U4 U3 102.4(4) . . ? O3D U4 U3 40.9(3) . . ? O1E U4 U3 39.4(3) . . ? O3C U4 U3 37.3(3) . . ? N1D U4 U3 161.5(5) . . ? N2D U4 U3 112.0(4) . . ? C7A N1A C8A 113.6(19) . . ? C15A N2A C14A 113.0(18) . . ? O1A C1A C6A 122(2) . . ? O1A C1A C2A 119(2) . . ? C6A C1A C2A 119(2) . . ? O2A C2A C1A 120(2) . . ? O2A C2A C3A 122(2) . . ? C1A C2A C3A 118(2) . . ? C4A C3A C7A 118(2) . . ? C4A C3A C2A 119(3) . . ? C7A C3A C2A 123(2) . . ? C5A C4A C3A 122(3) . . ? C4A C5A C6A 120(3) . . ? C5A C6A C1A 122(3) . . ? N1A C7A C3A 128(2) . . ? N1A C8A C9A 113.0(16) . . ? C10A C9A C14A 118(2) . . ? C10A C9A C8A 120(2) . . ? C14A C9A C8A 121.5(19) . . ? C9A C10A C11A 120(2) . . ? C10A C11A C12A 119(2) . . ? C13A C12A C11A 121(2) . . ? C12A C13A C14A 120(2) . . ? C13A C14A C9A 121(2) . . ? C13A C14A N2A 123(2) . . ? C9A C14A N2A 115.8(19) . . ? N2A C15A C16A 125(2) . . ? C21A C16A C17A 119(2) . . ? C21A C16A C15A 119(2) . . ? C17A C16A C15A 123(2) . . ? O3A C17A C16A 125(2) . . ? O3A C17A C18A 116(2) . . ? C16A C17A C18A 119(2) . . ? O4A C18A C19A 125(2) . . ? O4A C18A C17A 116(2) . . ? C19A C18A C17A 119(2) . . ? C20A C19A C18A 121(3) . . ? C21A C20A C19A 119(3) . . ? C20A C21A C16A 124(2) . . ? C7B N1B C8B 113.3(17) . . ? C15B N2B C14B 117.1(17) . . ? C6B C1B O1B 121(2) . . ? C6B C1B C2B 119(3) . . ? O1B C1B C2B 120.6(19) . . ? O2B C2B C3B 123.2(18) . . ? O2B C2B C1B 116(2) . . ? C3B C2B C1B 121(2) . . ? C2B C3B C4B 119.4(19) . . ? C2B C3B C7B 125.6(19) . . ? C4B C3B C7B 115(2) . . ? C5B C4B C3B 121(2) . . ? C4B C5B C6B 116(2) . . ? C1B C6B C5B 124(3) . . ? N1B C7B C3B 125(2) . . ? C9B C8B N1B 111.9(17) . . ? C14B C9B C10B 116(2) . . ? C14B C9B C8B 123(2) . . ? C10B C9B C8B 121(2) . . ? C11B C10B C9B 120(2) . . ? C12B C11B C10B 121(3) . . ? C11B C12B C13B 120(3) . . ? C14B C13B C12B 115(2) . . ? C9B C14B C13B 127(2) . . ? C9B C14B N2B 116(2) . . ? C13B C14B N2B 117(2) . . ? N2B C15B C16B 126.7(18) . . ? C21B C16B C17B 126(2) . . ? C21B C16B C15B 113(2) . . ? C17B C16B C15B 121(2) . . ? O3B C17B C18B 117.1(19) . . ? O3B C17B C16B 127(2) . . ? C18B C17B C16B 116(2) . . ? O4B C18B C19B 122(2) . . ? O4B C18B C17B 118(2) . . ? C19B C18B C17B 120(2) . . ? C18B C19B C20B 121(2) . . ? C21B C20B C19B 121(2) . . ? C16B C21B C20B 115(2) . . ? C7C N1C C8C 113.0(19) . . ? C15C N2C C14C 112(2) . . ? O1C C1C C6C 119(2) . . ? O1C C1C C2C 120(2) . . ? C6C C1C C2C 121(2) . . ? O2C C2C C3C 123(2) . . ? O2C C2C C1C 117(2) . . ? C3C C2C C1C 119(2) . . ? C4C C3C C2C 121(2) . . ? C4C C3C C7C 114(2) . . ? C2C C3C C7C 124(2) . . ? C3C C4C C5C 118(3) . . ? C4C C5C C6C 125(3) . . ? C5C C6C C1C 116(2) . . ? N1C C7C C3C 127(2) . . ? N1C C8C C9C 110(2) . . ? C14C C9C C10C 117(3) . . ? C14C C9C C8C 120(2) . . ? C10C C9C C8C 123(2) . . ? C9C C10C C11C 123(3) . . ? C12C C11C C10C 119(3) . . ? C11C C12C C13C 121(3) . . ? C12C C13C C14C 116(3) . . ? C9C C14C C13C 124(2) . . ? C9C C14C N2C 119(2) . . ? C13C C14C N2C 116(2) . . ? N2C C15C C16C 124(3) . . ? C17C C16C C21C 121(3) . . ? C17C C16C C15C 121(3) . . ? C21C C16C C15C 117(3) . . ? O3C C17C C16C 124(2) . . ? O3C C17C C18C 117(2) . . ? C16C C17C C18C 119(3) . . ? O4C C18C C19C 128(3) . . ? O4C C18C C17C 114(2) . . ? C19C C18C C17C 118(3) . . ? C18C C19C C20C 124(3) . . ? C19C C20C C21C 118(3) . . ? C20C C21C C16C 119(3) . . ? C7D N1D C8D 114.9(19) . . ? C15D N2D C14D 115.3(19) . . ? C2D C1D O1D 119(2) . . ? C2D C1D C6D 122(2) . . ? O1D C1D C6D 119(2) . . ? O2D C2D C1D 118(2) . . ? O2D C2D C3D 123(2) . . ? C1D C2D C3D 120(2) . . ? C2D C3D C4D 119(2) . . ? C2D C3D C7D 123(2) . . ? C4D C3D C7D 118(2) . . ? C3D C4D C5D 122(2) . . ? C6D C5D C4D 119(2) . . ? C5D C6D C1D 119(2) . . ? N1D C7D C3D 128(2) . . ? N1D C8D C9D 110(2) . . ? C14D C9D C10D 118(3) . . ? C14D C9D C8D 123(2) . . ? C10D C9D C8D 119(2) . . ? C11D C10D C9D 121(3) . . ? C10D C11D C12D 120(3) . . ? C13D C12D C11D 122(3) . . ? C14D C13D C12D 119(3) . . ? C13D C14D C9D 120(2) . . ? C13D C14D N2D 125(2) . . ? C9D C14D N2D 114(2) . . ? N2D C15D C16D 127(2) . . ? C17D C16D C21D 117(2) . . ? C17D C16D C15D 124(2) . . ? C21D C16D C15D 119(2) . . ? O3D C17D C16D 123(2) . . ? O3D C17D C18D 117.7(19) . . ? C16D C17D C18D 119(2) . . ? O4D C18D C17D 115(2) . . ? O4D C18D C19D 122(2) . . ? C17D C18D C19D 122(2) . . ? C18D C19D C20D 115(2) . . ? C21D C20D C19D 124(3) . . ? C20D C21D C16D 123(3) . . ? C7E N1E C8E 124.1(18) . . ? C15E N2E C14E 122(2) . . ? O1E C1E C2E 117(2) . . ? O1E C1E C6E 122.2(19) . . ? C2E C1E C6E 121(2) . . ? O2E C2E C1E 120(2) . . ? O2E C2E C3E 122.5(17) . . ? C1E C2E C3E 118(2) . . ? C4E C3E C7E 121(2) . . ? C4E C3E C2E 121.0(19) . . ? C7E C3E C2E 117(2) . . ? C5E C4E C3E 119(2) . . ? C4E C5E C6E 119(2) . . ? C1E C6E C5E 122(2) . . ? N1E C7E C3E 127(2) . . ? N1E C8E C9E 111.2(18) . . ? C10E C9E C14E 120(2) . . ? C10E C9E C8E 121(2) . . ? C14E C9E C8E 118(2) . . ? C9E C10E C11E 121(2) . . ? C12E C11E C10E 118(3) . . ? C11E C12E C13E 123(3) . . ? C14E C13E C12E 117(3) . . ? C9E C14E C13E 120(2) . . ? C9E C14E N2E 119(2) . . ? C13E C14E N2E 120(2) . . ? N2E C15E C16E 124(2) . . ? C17E C16E C21E 119(2) . . ? C17E C16E C15E 122(2) . . ? C21E C16E C15E 119(2) . . ? O3E C17E C16E 120(2) . . ? O3E C17E C18E 120(2) . . ? C16E C17E C18E 120(2) . . ? O4E C18E C19E 123(2) . . ? O4E C18E C17E 118(2) . . ? C19E C18E C17E 120(2) . . ? C20E C19E C18E 120(2) . . ? C21E C20E C19E 120(2) . . ? C20E C21E C16E 121(2) . . ? C7F N1F C8F 123(2) . . ? C15F N2F C14F 120(2) . . ? C6F C1F O1F 126(2) . . ? C6F C1F C2F 120.9(19) . . ? O1F C1F C2F 112.7(19) . . ? O2F C2F C3F 122.2(19) . . ? O2F C2F C1F 118.6(16) . . ? C3F C2F C1F 119(2) . . ? C7F C3F C4F 124(2) . . ? C7F C3F C2F 119(2) . . ? C4F C3F C2F 117(2) . . ? C5F C4F C3F 121(2) . . ? C4F C5F C6F 124(2) . . ? C1F C6F C5F 118(2) . . ? N1F C7F C3F 125(2) . . ? C9F C8F N1F 114(2) . . ? C10F C9F C14F 120(3) . . ? C10F C9F C8F 122(3) . . ? C14F C9F C8F 118(3) . . ? C9F C10F C11F 119(3) . . ? C10F C11F C12F 120(3) . . ? C13F C12F C11F 121(3) . . ? C12F C13F C14F 121(3) . . ? C13F C14F C9F 119(3) . . ? C13F C14F N2F 124(3) . . ? C9F C14F N2F 117(3) . . ? N2F C15F C16F 122(2) . . ? C17F C16F C15F 123(2) . . ? C17F C16F C21F 117(2) . . ? C15F C16F C21F 120(2) . . ? O3F C17F C16F 118(2) . . ? O3F C17F C18F 119(2) . . ? C16F C17F C18F 123(2) . . ? O4F C18F C19F 117(2) . . ? O4F C18F C17F 122(2) . . ? C19F C18F C17F 121(3) . . ? C18F C19F C20F 117(2) . . ? C21F C20F C19F 121(2) . . ? C20F C21F C16F 120(2) . . ? C1 O1 C4 107(2) . . ? C2 C1 O1 109(2) . . ? C1 C2 C3 105(2) . . ? C4 C3 C2 105(2) . . ? C3 C4 O1 106(3) . . ? C8 O2 C5 112(2) . . ? O2 C5 C6 101(3) . . ? C5 C6 C7 100(3) . . ? C8 C7 C6 106(3) . . ? O2 C8 C7 104(3) . . ? C9 O3 C12 106(3) . . ? O3 C9 C10 107(4) . . ? C11 C10 C9 105(4) . . ? C12 C11 C10 110(4) . . ? C11 C12 O3 107(3) . . ? C13 O4 C16 111(3) . . ? O4 C13 C14 109(4) . . ? C13 C14 C15 105(3) . . ? C14 C15 C16 104(3) . . ? O4 C16 C15 109(3) . . ? C17 O5 C20 99.1(15) . . ? O5 C17 C18 110(4) . . ? C17 C18 C19 105(3) . . ? C18 C19 C20 104(4) . . ? C19 C20 O5 105.2(16) . . ?