# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name 'Jean-Claude Berthet' 'Michel Ephritikhine' 'Martine Nierlich' _publ_contact_author_name 'Dr Jean-Claude Berthet' _publ_contact_author_address ; DSM/DRECAM/Service de Chimie Moleculaire Commissariat a l'Energie Atomique Cntre d'etude de Saclay, Bat 125, p Gif sur Yvette Essonnes 91191 cedex FRANCE ; _publ_contact_author_email BERTHET@DRECAM.CEA.FR _publ_section_title ; A novel coordination geometry for the uranyl ion. Rhombohedral uranium environment in [UO2(OTf)2(bpy)2] and [UO2(phen)3][OTf]2 ; data_2jc _database_code_CSD 202642 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H16 F6 N4 O8 S2 U' _chemical_formula_weight 880.54 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 6.0290(12) _cell_length_b 10.031(2) _cell_length_c 11.462(2) _cell_angle_alpha 102.13(3) _cell_angle_beta 92.66(3) _cell_angle_gamma 102.87(3) _cell_volume 657.5(2) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4085 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description irregular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 418 _exptl_absorpt_coefficient_mu 6.429 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.478 _exptl_absorpt_correction_T_max 0.785 _exptl_absorpt_process_details 'MULABS in PLATON;Spek,1998' _exptl_special_details ; Unit cell dimensions were determined from more than a thousand reflections in all the angular range, taken from ten frames with \f steps of 2\%.A 180\% range in \f was scanned during data collection with 2\%\f steps and 8s exposure by frame.The crystal to detector distance was 30mm. ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method '\f rotation scans with 2\%steps' _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4085 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 24.70 _reflns_number_total 2016 _reflns_number_gt 2015 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO(Otwinowski& Minor,1997)' _computing_cell_refinement 'DENZO(Otwinowski& Minor,1997)' _computing_data_reduction 'DENZO(Otwinowski& Minor,1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1990)' _computing_molecular_graphics 'SHELXTL (Sheldrick,1997)' _computing_publication_material 'SHELXTL (Sheldrick,1997)' _refine_special_details ; Structure solved by direct method and refined by full matrix least-squares on F^2^ with anisotropic thermal parameters for all non hydrogen atoms.Hydrogen atoms were introduced at calculated positions as riding atoms, with an isotropic displacement parameter equal to 1.2 (CH) times that of the parent atom. ; _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^)+(0.0536P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2016 _refine_ls_number_parameters 196 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0248 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_ref 0.0621 _refine_ls_wR_factor_gt 0.0621 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.949 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U U 0.0000 0.0000 0.0000 0.01439(11) Uani 1 2 d S . . S S -0.01382(19) -0.26123(11) -0.27018(9) 0.0176(2) Uani 1 1 d . . . F1 F -0.1756(6) -0.4296(3) -0.4770(3) 0.0376(8) Uani 1 1 d . . . F2 F -0.3148(6) -0.2489(3) -0.4377(3) 0.0374(7) Uani 1 1 d . . . F3 F -0.4249(6) -0.4172(4) -0.3480(3) 0.0427(8) Uani 1 1 d . . . O1 O -0.2539(5) 0.0502(3) 0.0353(3) 0.0172(6) Uani 1 1 d . . . O2 O -0.1380(6) -0.1861(3) -0.1808(3) 0.0191(7) Uani 1 1 d . . . O3 O 0.0518(6) -0.3778(4) -0.2357(3) 0.0281(8) Uani 1 1 d . . . O4 O 0.1512(6) -0.1717(4) -0.3221(3) 0.0306(8) Uani 1 1 d . . . N1 N -0.2743(6) -0.2216(4) 0.0477(3) 0.0166(7) Uani 1 1 d . . . N2 N 0.1156(7) -0.0961(4) 0.1822(3) 0.0181(8) Uani 1 1 d . . . C1 C -0.4795(8) -0.2723(5) -0.0171(4) 0.0184(9) Uani 1 1 d . . . H1B H -0.5009 -0.2447 -0.0885 0.022 Uiso 1 1 calc R . . C2 C -0.6614(8) -0.3637(5) 0.0171(4) 0.0226(10) Uani 1 1 d . . . H2A H -0.8013 -0.3951 -0.0295 0.027 Uiso 1 1 calc R . . C3 C -0.6276(9) -0.4063(5) 0.1226(4) 0.0231(10) Uani 1 1 d . . . H3B H -0.7448 -0.4682 0.1476 0.028 Uiso 1 1 calc R . . C4 C -0.4190(9) -0.3563(5) 0.1901(4) 0.0220(10) Uani 1 1 d . . . H4B H -0.3938 -0.3844 0.2609 0.026 Uiso 1 1 calc R . . C5 C -0.2451(8) -0.2624(5) 0.1510(4) 0.0184(9) Uani 1 1 d . . . C6 C -0.0199(8) -0.1993(4) 0.2217(4) 0.0166(9) Uani 1 1 d . . . C7 C 0.0459(9) -0.2454(5) 0.3220(4) 0.0245(10) Uani 1 1 d . . . H7A H -0.0517 -0.3173 0.3474 0.029 Uiso 1 1 calc R . . C8 C 0.2603(9) -0.1815(5) 0.3829(4) 0.0259(10) Uani 1 1 d . . . H8A H 0.3061 -0.2076 0.4517 0.031 Uiso 1 1 calc R . . C9 C 0.4058(8) -0.0784(5) 0.3404(4) 0.0233(10) Uani 1 1 d . . . H9A H 0.5520 -0.0364 0.3783 0.028 Uiso 1 1 calc R . . C10 C 0.3273(8) -0.0396(5) 0.2399(4) 0.0207(9) Uani 1 1 d . . . H10A H 0.4251 0.0287 0.2107 0.025 Uiso 1 1 calc R . . C11 C -0.2462(9) -0.3431(5) -0.3899(4) 0.0243(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.01265(16) 0.01240(14) 0.01762(15) 0.00537(9) 0.00154(8) 0.00012(9) S 0.0159(6) 0.0168(5) 0.0179(5) 0.0045(4) 0.0018(4) -0.0012(4) F1 0.047(2) 0.0355(17) 0.0241(15) -0.0063(13) -0.0047(13) 0.0100(15) F2 0.043(2) 0.0384(17) 0.0313(16) 0.0096(13) -0.0096(13) 0.0116(15) F3 0.0296(18) 0.049(2) 0.0366(17) 0.0132(15) -0.0045(13) -0.0186(16) O1 0.0151(16) 0.0163(15) 0.0202(15) 0.0047(12) 0.0010(12) 0.0035(13) O2 0.0184(17) 0.0170(15) 0.0180(15) 0.0017(12) 0.0010(12) -0.0015(13) O3 0.033(2) 0.0246(18) 0.0289(18) 0.0058(14) 0.0006(14) 0.0110(16) O4 0.0258(19) 0.0325(19) 0.0287(18) 0.0079(15) 0.0054(14) -0.0043(16) N1 0.0166(19) 0.0137(17) 0.0208(18) 0.0069(14) 0.0046(14) 0.0026(15) N2 0.019(2) 0.0145(18) 0.0202(18) 0.0054(14) -0.0008(14) 0.0010(16) C1 0.016(2) 0.015(2) 0.023(2) 0.0054(17) -0.0006(17) -0.0003(18) C2 0.016(2) 0.018(2) 0.031(3) -0.0007(19) -0.0005(18) 0.0040(19) C3 0.022(3) 0.016(2) 0.031(2) 0.0079(19) 0.0085(19) 0.0013(19) C4 0.027(3) 0.018(2) 0.021(2) 0.0067(18) 0.0037(18) 0.003(2) C5 0.018(2) 0.015(2) 0.024(2) 0.0070(17) 0.0035(17) 0.0032(18) C6 0.014(2) 0.016(2) 0.022(2) 0.0068(17) 0.0026(16) 0.0035(17) C7 0.027(3) 0.024(2) 0.024(2) 0.0135(19) 0.0050(19) 0.001(2) C8 0.027(3) 0.030(3) 0.023(2) 0.0092(19) 0.0006(19) 0.007(2) C9 0.018(3) 0.026(2) 0.025(2) 0.0050(19) -0.0012(18) 0.006(2) C10 0.020(2) 0.016(2) 0.026(2) 0.0072(18) 0.0007(18) 0.0026(19) C11 0.025(3) 0.026(2) 0.019(2) 0.0063(19) 0.0003(18) 0.000(2) _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 O1 1.754(3) . ? U O1 1.754(3) 2 ? U O2 2.448(3) . ? U O2 2.448(3) 2 ? U N2 2.605(4) . ? U N2 2.605(4) 2 ? U N1 2.633(4) . ? U N1 2.633(4) 2 ? S O4 1.425(4) . ? S O3 1.437(4) . ? S O2 1.476(3) . ? S C11 1.832(5) . ? F1 C11 1.330(6) . ? F2 C11 1.318(6) . ? F3 C11 1.336(6) . ? N1 C1 1.347(6) . ? N1 C5 1.348(6) . ? N2 C6 1.341(6) . ? N2 C10 1.352(6) . ? C1 C2 1.392(7) . ? C2 C3 1.385(7) . ? C3 C4 1.378(7) . ? C4 C5 1.404(7) . ? C5 C6 1.484(6) . ? C6 C7 1.399(6) . ? C7 C8 1.388(7) . ? C8 C9 1.387(7) . ? C9 C10 1.386(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 O1 U O1 180.0 . 2 ? O1 U O2 100.75(12) . . ? O1 U O2 79.25(12) 2 . ? O1 U O2 79.25(12) . 2 ? O1 U O2 100.75(12) 2 2 ? O2 U O2 180.0 . 2 ? O1 U N2 104.17(13) . . ? O1 U N2 75.83(13) 2 . ? O2 U N2 112.59(11) . . ? O2 U N2 67.41(11) 2 . ? O1 U N2 75.83(13) . 2 ? O1 U N2 104.17(13) 2 2 ? O2 U N2 67.41(11) . 2 ? O2 U N2 112.59(11) 2 2 ? N2 U N2 180.00(8) . 2 ? O1 U N1 74.13(13) . . ? O1 U N1 105.87(13) 2 . ? O2 U N1 68.12(11) . . ? O2 U N1 111.88(11) 2 . ? N2 U N1 60.77(12) . . ? N2 U N1 119.23(12) 2 . ? O1 U N1 105.87(13) . 2 ? O1 U N1 74.13(13) 2 2 ? O2 U N1 111.88(11) . 2 ? O2 U N1 68.12(11) 2 2 ? N2 U N1 119.23(12) . 2 ? N2 U N1 60.77(12) 2 2 ? N1 U N1 180.0 . 2 ? O4 S O3 117.3(2) . . ? O4 S O2 114.2(2) . . ? O3 S O2 113.6(2) . . ? O4 S C11 104.9(2) . . ? O3 S C11 104.2(2) . . ? O2 S C11 99.9(2) . . ? S O2 U 131.25(19) . . ? C1 N1 C5 117.7(4) . . ? C1 N1 U 117.9(3) . . ? C5 N1 U 122.2(3) . . ? C6 N2 C10 117.8(4) . . ? C6 N2 U 124.3(3) . . ? C10 N2 U 117.9(3) . . ? N1 C1 C2 123.7(4) . . ? C3 C2 C1 118.0(4) . . ? C4 C3 C2 119.5(4) . . ? C3 C4 C5 119.3(4) . . ? N1 C5 C4 121.9(4) . . ? N1 C5 C6 115.8(4) . . ? C4 C5 C6 122.3(4) . . ? N2 C6 C7 122.7(4) . . ? N2 C6 C5 115.3(4) . . ? C7 C6 C5 122.0(4) . . ? C8 C7 C6 118.5(4) . . ? C9 C8 C7 119.5(4) . . ? C10 C9 C8 118.2(4) . . ? N2 C10 C9 123.3(4) . . ? F2 C11 F1 107.5(4) . . ? F2 C11 F3 108.6(4) . . ? F1 C11 F3 108.3(4) . . ? F2 C11 S 111.6(3) . . ? F1 C11 S 110.0(4) . . ? F3 C11 S 110.7(3) . . ? _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 24.70 _diffrn_measured_fraction_theta_full 0.905 _refine_diff_density_max 1.432 _refine_diff_density_min -2.503 _refine_diff_density_rms 0.135 data_struc _database_code_CSD 202643 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59.50 H43.50 F6 N9.50 O8.50 S2 U' _chemical_formula_weight 1443.69 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 C2/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 35.859(7) _cell_length_b 12.269(3) _cell_length_c 29.128(6) _cell_angle_alpha 90.00 _cell_angle_beta 118.34(3) _cell_angle_gamma 90.00 _cell_volume 11279(4) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 33199 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description irregular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.700 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5704 _exptl_absorpt_coefficient_mu 3.039 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.699 _exptl_absorpt_correction_T_max 0.850 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33199 _diffrn_reflns_av_R_equivalents 0.0891 _diffrn_reflns_av_sigmaI/netI 0.1144 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 24.74 _reflns_number_total 9433 _reflns_number_gt 6026 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO(Otwinowski& Minor,1997)' _computing_cell_refinement 'DENZO(Otwinowski& Minor,1997)' _computing_data_reduction 'DENZO(Otwinowski& Minor,1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1990)' _computing_molecular_graphics 'SHELXTL (Sheldrick,1997)' _computing_publication_material 'SHELXTL (Sheldrick,1997)' _refine_special_details ; Structure solved by direct method and refined by full matrix least-squares on F^2^ with anisotropic thermal parameters for all non hydrogen atoms.Hydrogen atoms (except H atoms of the disordered 1/2 pyridine solvent molecule on the center of symmetry,C56 C57 C58) were introduced at calculated positions as riding atoms, with an isotropic displacement parameter equal to 1.2 (CH, CH~2~) times that of the parent atom. ; _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^)+(0.0490P)^2^+106.0426P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9433 _refine_ls_number_parameters 780 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1129 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1306 _refine_ls_wR_factor_gt 0.1075 _refine_ls_goodness_of_fit_ref 0.933 _refine_ls_restrained_S_all 0.933 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.011 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 24.74 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.928 _refine_diff_density_min -0.856 _refine_diff_density_rms 0.140 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 0.846686(10) 0.76245(2) 0.310052(13) 0.02632(12) Uani 1 1 d . . . S1 S 0.88534(10) 0.9594(3) 0.63838(14) 0.0736(11) Uani 1 1 d . . . S2 S 0.87302(9) 0.5517(2) 0.01145(11) 0.0467(7) Uani 1 1 d . . . F1 F 0.9088(4) 0.7561(7) 0.6424(5) 0.163(5) Uani 1 1 d . . . F2 F 0.9366(3) 0.8667(8) 0.6111(3) 0.109(3) Uani 1 1 d . . . F3 F 0.9589(3) 0.8637(5) 0.6935(3) 0.075(2) Uani 1 1 d . . . F4 F 0.9121(2) 0.3676(5) 0.0504(3) 0.072(2) Uani 1 1 d . . . F5 F 0.9505(2) 0.5093(5) 0.0834(3) 0.068(2) Uani 1 1 d . . . F6 F 0.9021(2) 0.4653(5) 0.1043(3) 0.070(2) Uani 1 1 d . . . O1 O 0.84586(19) 0.9048(4) 0.3143(2) 0.0302(15) Uani 1 1 d . . . O2 O 0.84964(19) 0.6198(4) 0.3085(3) 0.0317(15) Uani 1 1 d . . . O3 O 0.9080(3) 1.0602(7) 0.6439(4) 0.084(3) Uani 1 1 d . . . O4 O 0.8777(3) 0.9361(8) 0.6822(4) 0.094(4) Uani 1 1 d . . . O5 O 0.8504(3) 0.9366(12) 0.5880(4) 0.146(6) Uani 1 1 d . . . O6 O 0.8741(2) 0.6549(5) 0.0357(3) 0.0495(19) Uani 1 1 d . . . O7 O 0.8343(2) 0.4885(7) -0.0058(3) 0.074(3) Uani 1 1 d . . . O8 O 0.8904(2) 0.5560(6) -0.0241(3) 0.053(2) Uani 1 1 d . . . O9 O 1.0000 0.653(3) 0.2500 0.30(3) Uani 1 2 d S . . N1 N 0.7810(2) 0.8252(5) 0.2238(3) 0.0276(18) Uani 1 1 d . . . N2 N 0.8470(2) 0.7240(6) 0.2225(3) 0.0309(17) Uani 1 1 d . . . N3 N 0.9169(2) 0.8302(6) 0.3130(3) 0.035(2) Uani 1 1 d . . . N4 N 0.9182(2) 0.7112(5) 0.3924(3) 0.0291(18) Uani 1 1 d . . . N5 N 0.8389(3) 0.7918(6) 0.3927(3) 0.041(2) Uani 1 1 d . . . N6 N 0.7768(2) 0.6974(5) 0.3072(3) 0.0273(18) Uani 1 1 d . . . N7 N 0.7122(3) 0.4213(6) 0.6437(4) 0.045(2) Uani 1 1 d . . . N8 N 0.7863(3) 0.5382(6) 0.6925(4) 0.042(2) Uani 1 1 d . . . N9 N 0.8898(4) 0.7390(11) 0.8364(6) 0.101(4) Uani 1 1 d . . . C1 C 0.7494(3) 0.8782(7) 0.2249(4) 0.031(2) Uani 1 1 d . . . H1B H 0.7504 0.8888 0.2571 0.038 Uiso 1 1 calc R . . C2 C 0.7143(3) 0.9195(7) 0.1803(4) 0.037(2) Uani 1 1 d . . . H2B H 0.6919 0.9529 0.1826 0.045 Uiso 1 1 calc R . . C3 C 0.7141(3) 0.9089(7) 0.1335(4) 0.043(3) Uani 1 1 d . . . H3B H 0.6913 0.9352 0.1033 0.052 Uiso 1 1 calc R . . C4 C 0.7485(3) 0.8581(7) 0.1305(3) 0.035(2) Uani 1 1 d . . . C5 C 0.7505(4) 0.8439(8) 0.0831(4) 0.051(3) Uani 1 1 d . . . H5B H 0.7288 0.8711 0.0521 0.061 Uiso 1 1 calc R . . C6 C 0.7836(3) 0.7914(8) 0.0830(4) 0.044(3) Uani 1 1 d . . . H6B H 0.7845 0.7845 0.0518 0.053 Uiso 1 1 calc R . . C7 C 0.8171(3) 0.7462(7) 0.1294(3) 0.040(2) Uani 1 1 d . . . C8 C 0.8518(4) 0.6901(8) 0.1316(4) 0.048(3) Uani 1 1 d . . . H8C H 0.8546 0.6824 0.1016 0.057 Uiso 1 1 calc R . . C9 C 0.8815(4) 0.6467(9) 0.1772(5) 0.055(3) Uani 1 1 d . . . H9B H 0.9039 0.6057 0.1788 0.066 Uiso 1 1 calc R . . C10 C 0.8771(3) 0.6659(8) 0.2217(4) 0.046(3) Uani 1 1 d . . . H10A H 0.8970 0.6350 0.2530 0.055 Uiso 1 1 calc R . . C11 C 0.8155(3) 0.7615(7) 0.1764(3) 0.030(2) Uani 1 1 d . . . C12 C 0.7806(3) 0.8167(7) 0.1769(4) 0.032(2) Uani 1 1 d . . . C13 C 0.9169(3) 0.8934(8) 0.2777(4) 0.050(3) Uani 1 1 d . . . H13A H 0.8908 0.9113 0.2498 0.060 Uiso 1 1 calc R . . C14 C 0.9534(4) 0.9381(9) 0.2776(5) 0.068(4) Uani 1 1 d . . . H14A H 0.9515 0.9828 0.2508 0.081 Uiso 1 1 calc R . . C15 C 0.9907(4) 0.9120(11) 0.3184(5) 0.078(5) Uani 1 1 d . . . H15A H 1.0155 0.9372 0.3193 0.094 Uiso 1 1 calc R . . C16 C 0.9936(3) 0.8484(9) 0.3597(5) 0.056(3) Uani 1 1 d . . . C17 C 1.0332(3) 0.8165(10) 0.4032(5) 0.067(4) Uani 1 1 d . . . H17A H 1.0585 0.8390 0.4047 0.081 Uiso 1 1 calc R . . C18 C 1.0340(3) 0.7553(9) 0.4413(4) 0.054(3) Uani 1 1 d . . . H18A H 1.0599 0.7368 0.4695 0.065 Uiso 1 1 calc R . . C19 C 0.9953(3) 0.7171(8) 0.4395(4) 0.040(2) Uani 1 1 d . . . C20 C 0.9952(3) 0.6513(8) 0.4783(5) 0.051(3) Uani 1 1 d . . . H20A H 1.0204 0.6318 0.5073 0.061 Uiso 1 1 calc R . . C21 C 0.9568(3) 0.6152(8) 0.4729(4) 0.048(3) Uani 1 1 d . . . H21A H 0.9560 0.5705 0.4982 0.057 Uiso 1 1 calc R . . C22 C 0.9193(3) 0.6464(7) 0.4291(4) 0.037(2) Uani 1 1 d . . . H22A H 0.8938 0.6201 0.4257 0.045 Uiso 1 1 calc R . . C23 C 0.9564(3) 0.7450(7) 0.3967(3) 0.033(2) Uani 1 1 d . . . C24 C 0.9555(3) 0.8094(7) 0.3559(4) 0.039(3) Uani 1 1 d . . . C25 C 0.8676(3) 0.8486(8) 0.4337(4) 0.048(3) Uani 1 1 d . . . H25A H 0.8899 0.8819 0.4314 0.058 Uiso 1 1 calc R . . C26 C 0.8649(5) 0.8594(10) 0.4800(5) 0.069(4) Uani 1 1 d . . . H26A H 0.8847 0.9000 0.5079 0.083 Uiso 1 1 calc R . . C27 C 0.8321(5) 0.8079(12) 0.4827(5) 0.076(4) Uani 1 1 d . . . H27A H 0.8312 0.8104 0.5141 0.091 Uiso 1 1 calc R . . C28 C 0.8005(4) 0.7529(9) 0.4416(4) 0.050(3) Uani 1 1 d . . . C29 C 0.7646(5) 0.7031(10) 0.4427(6) 0.067(4) Uani 1 1 d . . . H29A H 0.7626 0.7019 0.4733 0.080 Uiso 1 1 calc R . . C30 C 0.7339(5) 0.6583(9) 0.3986(6) 0.068(4) Uani 1 1 d . . . H30A H 0.7102 0.6291 0.3993 0.082 Uiso 1 1 calc R . . C31 C 0.7362(4) 0.6539(8) 0.3517(5) 0.046(3) Uani 1 1 d . . . C32 C 0.7050(4) 0.6101(7) 0.3059(6) 0.054(3) Uani 1 1 d . . . H32A H 0.6804 0.5829 0.3050 0.065 Uiso 1 1 calc R . . C33 C 0.7095(3) 0.6058(7) 0.2617(5) 0.052(3) Uani 1 1 d . . . H33A H 0.6885 0.5768 0.2307 0.062 Uiso 1 1 calc R . . C34 C 0.7468(3) 0.6470(6) 0.2656(4) 0.036(2) Uani 1 1 d . . . H34A H 0.7514 0.6388 0.2369 0.043 Uiso 1 1 calc R . . C35 C 0.7728(3) 0.6987(6) 0.3517(4) 0.033(2) Uani 1 1 d . . . C36 C 0.8053(3) 0.7509(7) 0.3963(4) 0.040(2) Uani 1 1 d . . . C37 C 0.6763(4) 0.3673(9) 0.6189(6) 0.067(4) Uani 1 1 d . . . H37A H 0.6628 0.3454 0.6378 0.080 Uiso 1 1 calc R . . C38 C 0.6570(4) 0.3404(10) 0.5652(7) 0.083(5) Uani 1 1 d . . . H38A H 0.6322 0.2993 0.5499 0.099 Uiso 1 1 calc R . . C39 C 0.6753(5) 0.3759(10) 0.5363(6) 0.079(5) Uani 1 1 d . . . H39A H 0.6630 0.3610 0.5008 0.095 Uiso 1 1 calc R . . C40 C 0.7136(4) 0.4359(8) 0.5612(4) 0.057(3) Uani 1 1 d . . . C41 C 0.7347(6) 0.4732(10) 0.5327(5) 0.073(4) Uani 1 1 d . . . H41A H 0.7227 0.4596 0.4971 0.088 Uiso 1 1 calc R . . C42 C 0.7711(5) 0.5270(10) 0.5566(6) 0.071(4) Uani 1 1 d . . . H42A H 0.7843 0.5493 0.5373 0.085 Uiso 1 1 calc R . . C43 C 0.7909(4) 0.5519(8) 0.6118(5) 0.049(3) Uani 1 1 d . . . C44 C 0.8288(4) 0.6114(9) 0.6396(6) 0.062(4) Uani 1 1 d . . . H44A H 0.8432 0.6357 0.6222 0.075 Uiso 1 1 calc R . . C45 C 0.8447(4) 0.6341(9) 0.6906(6) 0.059(3) Uani 1 1 d . . . H45A H 0.8695 0.6744 0.7085 0.071 Uiso 1 1 calc R . . C46 C 0.8224(4) 0.5943(9) 0.7158(5) 0.058(3) Uani 1 1 d . . . H46A H 0.8337 0.6080 0.7513 0.069 Uiso 1 1 calc R . . C47 C 0.7707(3) 0.5169(7) 0.6410(4) 0.040(3) Uani 1 1 d . . . C48 C 0.7308(3) 0.4570(7) 0.6150(4) 0.040(3) Uani 1 1 d . . . C49 C 0.9210(5) 0.8583(12) 0.6459(6) 0.086(5) Uani 1 1 d . . . C50 C 0.9110(4) 0.4705(9) 0.0649(4) 0.049(3) Uani 1 1 d . . . C51 C 0.9110(5) 0.6563(14) 0.8683(6) 0.090(5) Uani 1 1 d . . . H51A H 0.8991 0.6211 0.8866 0.108 Uiso 1 1 calc R . . C52 C 0.9466(6) 0.6249(17) 0.8743(8) 0.132(8) Uani 1 1 d . . . H52A H 0.9583 0.5602 0.8919 0.158 Uiso 1 1 calc R . . C53 C 0.9682(8) 0.687(3) 0.8546(12) 0.240(18) Uani 1 1 d . . . H53A H 0.9959 0.6699 0.8624 0.288 Uiso 1 1 calc R . . C54 C 0.9482(7) 0.773(2) 0.8240(12) 0.197(13) Uani 1 1 d . . . H54A H 0.9610 0.8137 0.8086 0.236 Uiso 1 1 calc R . . C55 C 0.9098(5) 0.7973(14) 0.8163(8) 0.122(7) Uani 1 1 d . . . H55A H 0.8963 0.8578 0.7959 0.146 Uiso 1 1 calc R . . C56 C 1.0372(12) 1.000(3) 0.508(3) 0.178(13) Uani 1 1 d . . . C57 C 1.010(3) 1.057(3) 0.466(2) 0.216(17) Uani 1 1 d . . . C58 C 0.9660(17) 1.053(4) 0.4503(16) 0.21(2) Uani 1 1 d . . . C59 C 1.0050(9) 0.578(3) 0.2123(13) 0.207(17) Uani 1 1 d . . . H59A H 0.9852 0.5971 0.1765 0.249 Uiso 1 1 calc R . . H59B H 1.0336 0.5808 0.2169 0.249 Uiso 1 1 calc R . . C60 C 0.9960(15) 0.478(2) 0.2250(13) 0.43(5) Uani 1 1 d . . . H60A H 0.9664 0.4600 0.2024 0.521 Uiso 1 1 calc R . . H60B H 1.0132 0.4226 0.2200 0.521 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 0.02254(17) 0.02984(18) 0.02649(18) 0.00078(17) 0.01155(13) -0.00041(16) S1 0.0383(19) 0.134(3) 0.054(2) -0.038(2) 0.0261(17) -0.0300(19) S2 0.0428(17) 0.0504(15) 0.0386(17) 0.0014(12) 0.0126(14) 0.0063(12) F1 0.190(11) 0.093(7) 0.261(14) -0.101(8) 0.152(11) -0.083(7) F2 0.078(6) 0.192(9) 0.070(6) -0.038(6) 0.046(5) 0.000(6) F3 0.096(6) 0.061(4) 0.075(6) -0.004(4) 0.047(5) 0.007(4) F4 0.104(6) 0.047(4) 0.077(5) 0.005(3) 0.053(5) 0.021(4) F5 0.036(4) 0.090(5) 0.060(5) 0.001(4) 0.008(4) 0.005(3) F6 0.092(6) 0.073(4) 0.062(5) 0.022(4) 0.050(4) 0.022(4) O1 0.030(4) 0.024(3) 0.028(4) 0.001(3) 0.007(3) -0.001(3) O2 0.023(3) 0.029(3) 0.042(4) -0.004(3) 0.015(3) 0.000(3) O3 0.052(6) 0.092(6) 0.105(8) 0.018(5) 0.035(6) 0.000(5) O4 0.074(7) 0.161(9) 0.083(7) -0.074(6) 0.066(6) -0.064(6) O5 0.039(6) 0.314(17) 0.066(7) -0.097(9) 0.009(5) -0.045(8) O6 0.056(5) 0.051(4) 0.048(5) -0.003(3) 0.029(4) 0.009(3) O7 0.035(5) 0.090(6) 0.075(6) 0.007(5) 0.009(4) -0.017(4) O8 0.065(5) 0.068(5) 0.034(4) 0.007(4) 0.031(4) 0.027(4) O9 0.27(4) 0.17(3) 0.42(8) 0.000 0.12(5) 0.000 N1 0.021(4) 0.026(4) 0.035(5) -0.001(3) 0.013(4) 0.002(3) N2 0.024(4) 0.037(4) 0.036(5) -0.008(3) 0.017(4) 0.000(3) N3 0.026(5) 0.041(4) 0.028(5) 0.014(3) 0.004(4) -0.003(3) N4 0.025(4) 0.029(4) 0.033(5) 0.009(3) 0.013(4) -0.001(3) N5 0.035(5) 0.046(5) 0.036(5) -0.005(4) 0.013(4) 0.008(4) N6 0.035(5) 0.018(3) 0.037(5) 0.002(3) 0.024(4) 0.001(3) N7 0.037(6) 0.044(5) 0.050(6) 0.003(4) 0.018(5) 0.005(4) N8 0.038(5) 0.043(5) 0.045(6) 0.002(4) 0.021(5) 0.004(4) N9 0.065(8) 0.117(10) 0.126(12) 0.017(9) 0.050(8) 0.021(8) C1 0.023(5) 0.032(5) 0.037(6) 0.004(4) 0.013(5) -0.002(4) C2 0.028(6) 0.030(5) 0.043(7) -0.003(4) 0.008(5) -0.002(4) C3 0.042(7) 0.038(5) 0.033(7) 0.008(4) 0.004(6) 0.002(5) C4 0.044(6) 0.031(5) 0.014(5) -0.001(4) 0.001(5) -0.004(4) C5 0.063(8) 0.046(6) 0.030(7) 0.004(5) 0.011(6) -0.003(5) C6 0.062(8) 0.051(6) 0.027(6) 0.001(4) 0.026(6) 0.005(5) C7 0.052(6) 0.038(5) 0.030(5) -0.005(5) 0.021(5) -0.010(5) C8 0.053(7) 0.062(7) 0.045(7) -0.010(5) 0.036(6) -0.004(6) C9 0.050(8) 0.058(7) 0.070(9) 0.002(6) 0.039(7) 0.017(6) C10 0.036(6) 0.072(7) 0.038(7) -0.002(5) 0.024(6) 0.016(5) C11 0.032(5) 0.028(5) 0.032(5) -0.007(4) 0.018(4) -0.005(4) C12 0.033(6) 0.030(5) 0.026(6) -0.012(4) 0.010(5) -0.013(4) C13 0.040(7) 0.062(7) 0.048(7) 0.030(6) 0.020(6) 0.001(5) C14 0.046(8) 0.081(8) 0.064(9) 0.038(7) 0.016(7) -0.006(6) C15 0.035(7) 0.104(10) 0.074(10) 0.041(8) 0.009(7) -0.021(7) C16 0.024(6) 0.079(8) 0.051(8) 0.029(6) 0.005(6) -0.009(5) C17 0.014(6) 0.102(9) 0.063(9) 0.033(7) 0.000(6) -0.007(5) C18 0.023(5) 0.082(8) 0.043(6) 0.015(6) 0.003(5) -0.006(6) C19 0.033(6) 0.045(6) 0.036(6) 0.006(5) 0.011(5) 0.001(4) C20 0.036(7) 0.054(6) 0.057(8) 0.013(6) 0.017(6) 0.014(5) C21 0.050(7) 0.051(6) 0.036(7) 0.025(5) 0.015(6) 0.014(5) C22 0.037(6) 0.037(5) 0.048(7) 0.014(5) 0.029(6) 0.012(4) C23 0.026(5) 0.036(5) 0.025(5) 0.007(4) 0.003(4) -0.005(4) C24 0.024(6) 0.041(5) 0.044(7) 0.006(5) 0.009(5) -0.006(4) C25 0.039(7) 0.057(6) 0.035(7) -0.018(5) 0.006(6) 0.005(5) C26 0.072(10) 0.080(9) 0.033(8) -0.014(6) 0.006(7) 0.031(7) C27 0.100(12) 0.099(10) 0.047(9) 0.019(8) 0.052(9) 0.039(9) C28 0.074(8) 0.051(6) 0.037(6) 0.015(6) 0.036(6) 0.028(6) C29 0.088(11) 0.068(8) 0.087(11) 0.031(7) 0.077(10) 0.039(7) C30 0.087(11) 0.056(7) 0.106(13) 0.043(8) 0.082(11) 0.028(7) C31 0.051(7) 0.036(5) 0.084(9) 0.021(6) 0.059(7) 0.011(5) C32 0.040(7) 0.016(5) 0.105(11) 0.013(5) 0.034(8) -0.005(4) C33 0.043(7) 0.026(5) 0.092(10) 0.002(5) 0.035(7) -0.008(4) C34 0.031(6) 0.025(5) 0.058(7) -0.008(4) 0.025(6) 0.001(4) C35 0.038(6) 0.022(4) 0.054(7) 0.011(4) 0.034(6) 0.012(4) C36 0.042(6) 0.040(6) 0.047(6) 0.014(5) 0.029(5) 0.016(5) C37 0.044(8) 0.056(7) 0.101(12) 0.005(7) 0.035(8) 0.003(6) C38 0.044(9) 0.051(8) 0.111(14) -0.018(8) 0.002(9) 0.004(6) C39 0.081(11) 0.063(8) 0.059(10) -0.024(7) 0.005(9) 0.000(8) C40 0.096(10) 0.037(6) 0.031(7) 0.001(5) 0.024(7) 0.019(6) C41 0.127(14) 0.065(8) 0.044(8) -0.003(6) 0.054(9) 0.015(9) C42 0.118(13) 0.053(7) 0.078(11) 0.011(7) 0.075(10) 0.014(8) C43 0.073(9) 0.036(6) 0.050(8) 0.006(5) 0.039(7) 0.011(5) C44 0.063(9) 0.048(7) 0.110(12) 0.014(7) 0.068(9) 0.007(6) C45 0.052(8) 0.060(7) 0.071(10) 0.001(7) 0.032(8) 0.009(6) C46 0.054(8) 0.064(7) 0.063(9) 0.004(6) 0.034(7) 0.011(6) C47 0.047(7) 0.033(5) 0.054(8) 0.009(5) 0.035(6) 0.015(5) C48 0.045(7) 0.032(5) 0.046(7) -0.002(5) 0.023(6) 0.002(5) C49 0.110(13) 0.102(11) 0.064(10) -0.051(8) 0.057(10) -0.065(10) C50 0.055(8) 0.063(7) 0.039(7) 0.005(5) 0.030(6) 0.003(6) C51 0.046(9) 0.141(14) 0.077(12) 0.022(10) 0.024(9) -0.006(9) C52 0.102(15) 0.188(19) 0.131(17) 0.102(15) 0.076(14) 0.081(14) C53 0.15(2) 0.32(4) 0.31(4) 0.24(3) 0.16(3) 0.13(2) C54 0.126(19) 0.25(3) 0.28(3) 0.12(3) 0.16(2) 0.053(19) C55 0.068(11) 0.115(13) 0.19(2) 0.070(13) 0.070(13) 0.024(9) C56 0.13(3) 0.20(3) 0.22(4) -0.02(3) 0.10(3) -0.06(2) C57 0.26(6) 0.20(3) 0.23(5) -0.02(3) 0.15(4) 0.02(4) C58 0.22(4) 0.24(5) 0.21(4) -0.12(4) 0.13(4) -0.01(3) C59 0.12(2) 0.31(5) 0.17(3) -0.08(3) 0.05(2) -0.11(3) C60 0.41(6) 0.22(3) 0.21(4) -0.12(3) -0.23(4) 0.13(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 O1 1.752(5) . ? U O2 1.755(5) . ? U N5 2.577(8) . ? U N6 2.595(7) . ? U N2 2.599(7) . ? U N3 2.613(8) . ? U N1 2.615(7) . ? U N4 2.624(7) . ? S1 O5 1.434(9) . ? S1 O3 1.445(9) . ? S1 O4 1.456(9) . ? S1 C49 1.720(18) . ? S2 O6 1.441(7) . ? S2 O8 1.441(7) . ? S2 O7 1.455(8) . ? S2 C50 1.805(11) . ? F1 C49 1.317(15) . ? F2 C49 1.375(15) . ? F3 C49 1.409(16) . ? F4 C50 1.338(12) . ? F5 C50 1.341(12) . ? F6 C50 1.332(12) . ? O9 C59 1.50(3) . ? O9 C59 1.50(3) 2_755 ? N1 C1 1.320(11) . ? N1 C12 1.363(11) . ? N2 C10 1.301(11) . ? N2 C11 1.361(11) . ? N3 C13 1.288(12) . ? N3 C24 1.379(11) . ? N4 C22 1.318(11) . ? N4 C23 1.378(11) . ? N5 C25 1.343(12) . ? N5 C36 1.356(12) . ? N6 C34 1.331(11) . ? N6 C35 1.369(11) . ? N7 C37 1.317(14) . ? N7 C48 1.365(13) . ? N8 C46 1.334(14) . ? N8 C47 1.356(13) . ? N9 C55 1.332(19) . ? N9 C51 1.342(18) . ? C1 C2 1.406(13) . ? C2 C3 1.367(14) . ? C3 C4 1.421(14) . ? C4 C12 1.391(12) . ? C4 C5 1.425(14) . ? C5 C6 1.352(14) . ? C6 C7 1.428(13) . ? C7 C8 1.396(14) . ? C7 C11 1.411(12) . ? C8 C9 1.357(15) . ? C9 C10 1.399(14) . ? C11 C12 1.428(12) . ? C13 C14 1.418(15) . ? C14 C15 1.341(16) . ? C15 C16 1.395(15) . ? C16 C24 1.404(13) . ? C16 C17 1.437(14) . ? C17 C18 1.329(14) . ? C18 C19 1.441(14) . ? C19 C20 1.390(14) . ? C19 C23 1.403(12) . ? C20 C21 1.381(14) . ? C21 C22 1.399(13) . ? C23 C24 1.413(13) . ? C25 C26 1.403(16) . ? C26 C27 1.370(18) . ? C27 C28 1.373(18) . ? C28 C36 1.408(13) . ? C28 C29 1.439(17) . ? C29 C30 1.349(18) . ? C30 C31 1.409(16) . ? C31 C32 1.380(16) . ? C31 C35 1.422(13) . ? C32 C33 1.374(16) . ? C33 C34 1.386(13) . ? C35 C36 1.422(14) . ? C37 C38 1.417(19) . ? C38 C39 1.36(2) . ? C39 C40 1.416(18) . ? C40 C48 1.410(14) . ? C40 C41 1.440(18) . ? C41 C42 1.327(18) . ? C42 C43 1.449(17) . ? C43 C44 1.410(16) . ? C43 C47 1.421(14) . ? C44 C45 1.343(17) . ? C45 C46 1.403(16) . ? C47 C48 1.460(14) . ? C51 C52 1.265(19) . ? C52 C53 1.39(3) . ? C53 C54 1.34(3) . ? C54 C55 1.32(2) . ? C56 C57 1.36(4) . ? C56 C58 1.43(5) 5_776 ? C57 C58 1.42(5) . ? C58 C56 1.43(5) 5_776 ? C59 C60 1.37(5) . ? C60 C60 1.34(10) 2_755 ? 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 O1 U O2 177.4(3) . . ? O1 U N5 77.4(3) . . ? O2 U N5 101.4(3) . . ? O1 U N6 105.1(3) . . ? O2 U N6 76.2(2) . . ? N5 U N6 62.7(2) . . ? O1 U N2 105.0(3) . . ? O2 U N2 76.4(3) . . ? N5 U N2 174.3(2) . . ? N6 U N2 111.6(2) . . ? O1 U N3 74.2(3) . . ? O2 U N3 104.4(3) . . ? N5 U N3 117.0(3) . . ? N6 U N3 179.3(2) . . ? N2 U N3 68.7(2) . . ? O1 U N1 74.7(2) . . ? O2 U N1 107.8(3) . . ? N5 U N1 114.1(2) . . ? N6 U N1 69.1(2) . . ? N2 U N1 62.1(2) . . ? N3 U N1 110.7(2) . . ? O1 U N4 102.5(2) . . ? O2 U N4 74.9(3) . . ? N5 U N4 70.8(2) . . ? N6 U N4 117.8(2) . . ? N2 U N4 113.3(2) . . ? N3 U N4 62.5(2) . . ? N1 U N4 173.1(2) . . ? O5 S1 O3 116.9(8) . . ? O5 S1 O4 115.1(6) . . ? O3 S1 O4 113.5(6) . . ? O5 S1 C49 103.0(7) . . ? O3 S1 C49 105.0(6) . . ? O4 S1 C49 100.6(7) . . ? O6 S2 O8 113.5(4) . . ? O6 S2 O7 115.9(5) . . ? O8 S2 O7 116.0(5) . . ? O6 S2 C50 103.2(5) . . ? O8 S2 C50 103.5(5) . . ? O7 S2 C50 102.0(5) . . ? C59 O9 C59 105(4) . 2_755 ? C1 N1 C12 117.5(8) . . ? C1 N1 U 120.9(6) . . ? C12 N1 U 121.0(6) . . ? C10 N2 C11 118.4(8) . . ? C10 N2 U 120.4(7) . . ? C11 N2 U 121.2(5) . . ? C13 N3 C24 117.0(8) . . ? C13 N3 U 122.1(7) . . ? C24 N3 U 120.5(6) . . ? C22 N4 C23 117.6(8) . . ? C22 N4 U 121.7(6) . . ? C23 N4 U 120.6(5) . . ? C25 N5 C36 117.1(9) . . ? C25 N5 U 121.8(7) . . ? C36 N5 U 121.0(6) . . ? C34 N6 C35 117.8(8) . . ? C34 N6 U 121.3(6) . . ? C35 N6 U 120.0(6) . . ? C37 N7 C48 117.5(11) . . ? C46 N8 C47 116.9(10) . . ? C55 N9 C51 117.7(13) . . ? N1 C1 C2 123.9(10) . . ? C3 C2 C1 117.7(10) . . ? C2 C3 C4 120.7(9) . . ? C12 C4 C3 116.2(9) . . ? C12 C4 C5 119.9(10) . . ? C3 C4 C5 123.9(9) . . ? C6 C5 C4 120.5(10) . . ? C5 C6 C7 121.9(10) . . ? C8 C7 C11 118.0(9) . . ? C8 C7 C6 124.5(9) . . ? C11 C7 C6 117.5(9) . . ? C9 C8 C7 120.3(10) . . ? C8 C9 C10 117.5(10) . . ? N2 C10 C9 124.5(10) . . ? N2 C11 C7 120.9(8) . . ? N2 C11 C12 118.2(8) . . ? C7 C11 C12 120.9(8) . . ? N1 C12 C4 123.8(9) . . ? N1 C12 C11 117.0(8) . . ? C4 C12 C11 119.2(9) . . ? N3 C13 C14 125.8(10) . . ? C15 C14 C13 116.0(11) . . ? C14 C15 C16 122.2(11) . . ? C15 C16 C24 116.8(10) . . ? C15 C16 C17 123.4(10) . . ? C24 C16 C17 119.6(10) . . ? C18 C17 C16 120.7(10) . . ? C17 C18 C19 120.9(9) . . ? C20 C19 C23 118.5(9) . . ? C20 C19 C18 122.3(9) . . ? C23 C19 C18 119.2(9) . . ? C21 C20 C19 118.8(10) . . ? C20 C21 C22 119.4(9) . . ? N4 C22 C21 123.3(9) . . ? N4 C23 C19 122.2(8) . . ? N4 C23 C24 117.8(7) . . ? C19 C23 C24 120.0(8) . . ? N3 C24 C16 122.0(9) . . ? N3 C24 C23 118.6(8) . . ? C16 C24 C23 119.4(9) . . ? N5 C25 C26 122.1(12) . . ? C27 C26 C25 117.7(12) . . ? C26 C27 C28 123.5(12) . . ? C27 C28 C36 114.1(11) . . ? C27 C28 C29 124.5(12) . . ? C36 C28 C29 121.4(11) . . ? C30 C29 C28 119.2(12) . . ? C29 C30 C31 122.7(12) . . ? C32 C31 C30 123.9(12) . . ? C32 C31 C35 118.4(11) . . ? C30 C31 C35 117.7(12) . . ? C33 C32 C31 121.2(10) . . ? C32 C33 C34 116.7(11) . . ? N6 C34 C33 125.0(10) . . ? N6 C35 C36 117.5(8) . . ? N6 C35 C31 120.4(10) . . ? C36 C35 C31 122.0(10) . . ? N5 C36 C28 125.1(10) . . ? N5 C36 C35 118.0(9) . . ? C28 C36 C35 116.9(9) . . ? N7 C37 C38 124.1(13) . . ? C39 C38 C37 118.7(13) . . ? C38 C39 C40 118.9(13) . . ? C48 C40 C39 118.2(13) . . ? C48 C40 C41 120.7(12) . . ? C39 C40 C41 121.1(13) . . ? C42 C41 C40 120.8(12) . . ? C41 C42 C43 121.9(12) . . ? C44 C43 C47 116.0(11) . . ? C44 C43 C42 125.3(12) . . ? C47 C43 C42 118.6(12) . . ? C45 C44 C43 122.0(12) . . ? C44 C45 C46 117.2(12) . . ? N8 C46 C45 124.8(12) . . ? N8 C47 C43 123.0(10) . . ? N8 C47 C48 117.2(9) . . ? C43 C47 C48 119.7(10) . . ? N7 C48 C40 122.5(10) . . ? N7 C48 C47 119.3(10) . . ? C40 C48 C47 118.2(11) . . ? F1 C49 F2 104.7(11) . . ? F1 C49 F3 104.5(14) . . ? F2 C49 F3 100.6(11) . . ? F1 C49 S1 118.4(12) . . ? F2 C49 S1 113.0(12) . . ? F3 C49 S1 113.7(9) . . ? F6 C50 F4 106.5(8) . . ? F6 C50 F5 108.1(9) . . ? F4 C50 F5 106.1(9) . . ? F6 C50 S2 112.2(8) . . ? F4 C50 S2 111.8(8) . . ? F5 C50 S2 111.8(7) . . ? C52 C51 N9 121.9(16) . . ? C51 C52 C53 120.0(18) . . ? C54 C53 C52 118(2) . . ? C55 C54 C53 119(2) . . ? C54 C55 N9 122.6(17) . . ? C57 C56 C58 134(3) . 5_776 ? C56 C57 C58 118(4) . . ? C57 C58 C56 106(4) . 5_776 ? C60 C59 O9 103(4) . . ? C60 C60 C59 109.7(19) 2_755 . ?