# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'M Ephritikhine' _publ_contact_author_email MICHEL.EPHRITIKHINE@CEA.FR _publ_section_title ; Synthesis and crystal structure of pentavalent uranyl complexes. The remarkable stability of UO2X (X = I, SO3CF3) in non-aqueous solutions ; loop_ _publ_author_name 'M Ephritikhine' 'Jean-Claude Berthet' 'Gerald Siffredi' 'Pierre Thuery' # Attachment 'revisedB820659GCIF.txt' data_4.py _database_code_depnum_ccdc_archive 'CCDC 711336' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C55 H50 F15 K3 N10 O19 S5 U2, C5 H5 N' _chemical_formula_sum 'C60 H55 F15 K3 N11 O19 S5 U2' _chemical_formula_weight 2272.81 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' K K 0.2009 0.2494 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 17.5189(6) _cell_length_b 11.7341(2) _cell_length_c 20.1579(7) _cell_angle_alpha 90.00 _cell_angle_beta 99.510(2) _cell_angle_gamma 90.00 _cell_volume 4086.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 106663 _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light orange' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.847 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2200 _exptl_absorpt_coefficient_mu 4.343 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.640 _exptl_absorpt_correction_T_max 0.805 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 40 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 area-detector diffractometer' _diffrn_measurement_method 'two \f and four \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 106663 _diffrn_reflns_av_R_equivalents 0.0742 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 25.68 _reflns_number_total 15426 _reflns_number_gt 14246 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. One of the pyridine molecules (containing N5) was refined as an idealized hexagon. Some restraints on bond lengths and/or displacement parameters were applied for some badly behaving atoms, particularly in the triflate groups. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 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^)+(0.0643P)^2^+37.0398P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.007(8) _refine_ls_number_reflns 15426 _refine_ls_number_parameters 1034 _refine_ls_number_restraints 97 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1387 _refine_ls_wR_factor_gt 0.1358 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.043 _refine_diff_density_min -1.176 _refine_diff_density_rms 0.163 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 0.47717(2) 0.55267(3) 0.75353(2) 0.02922(11) Uani 1 1 d . . . U2 U 0.03324(2) 0.63369(3) 0.24619(2) 0.03445(13) Uani 1 1 d . . . K1 K 0.40772(18) 0.6881(2) 0.54570(15) 0.0485(7) Uani 1 1 d . . . K2 K 0.0598(2) 0.5496(3) 0.46544(15) 0.0649(9) Uani 1 1 d . . . K3 K -0.0132(2) 0.7398(3) 0.02914(15) 0.0620(9) Uani 1 1 d . . . S1 S 0.4929(2) 0.4238(3) 0.46933(16) 0.0456(8) Uani 1 1 d . . . S2 S 0.2127(3) 0.7362(5) 0.5429(3) 0.113(2) Uani 1 1 d DU . . S3 S 0.07965(18) 0.2741(3) 0.48832(15) 0.0448(7) Uani 1 1 d D . . S4 S -0.0955(4) 1.0088(4) 0.0374(2) 0.0530(13) Uani 1 1 d . . . S5 S -0.2185(3) 0.5490(6) -0.0162(3) 0.0760(15) Uani 1 1 d . . . O1 O 0.4484(4) 0.5985(7) 0.6649(4) 0.037(2) Uani 1 1 d . . . O2 O 0.5047(5) 0.5072(7) 0.8403(4) 0.0396(19) Uani 1 1 d . . . O3 O 0.0427(5) 0.6038(8) 0.3359(4) 0.046(2) Uani 1 1 d . . . O4 O 0.0249(5) 0.6670(7) 0.1559(4) 0.039(2) Uani 1 1 d . . . O5 O 0.4928(7) 0.5433(8) 0.4852(5) 0.062(3) Uani 1 1 d . . . O6 O 0.5268(6) 0.3545(8) 0.5249(4) 0.051(2) Uani 1 1 d . . . O7 O 0.5163(6) 0.3914(8) 0.4059(4) 0.052(2) Uani 1 1 d . . . O8 O 0.2729(6) 0.7299(12) 0.5996(5) 0.090(4) Uani 1 1 d D . . O9 O 0.213(2) 0.683(2) 0.4802(8) 0.097(8) Uani 1 1 d D . . O10 O 0.1472(8) 0.6782(14) 0.5672(10) 0.154(7) Uani 1 1 d D . . O11 O 0.0800(8) 0.3566(10) 0.5411(5) 0.073(3) Uani 1 1 d . . . O12 O 0.0460(7) 0.3131(11) 0.4240(5) 0.068(3) Uani 1 1 d . . . O13 O 0.0597(6) 0.1585(9) 0.5040(6) 0.069(3) Uani 1 1 d . . . O14 O -0.0560(11) 0.9601(16) -0.0153(7) 0.079(5) Uani 1 1 d . . . O15 O -0.0928(7) 0.9444(16) 0.0951(6) 0.110(5) Uani 1 1 d U . . O16 O -0.0563(10) 1.1149(15) 0.0522(10) 0.132(6) Uani 1 1 d . . . O17 O -0.1447(7) 0.6023(13) 0.0118(7) 0.093(6) Uani 1 1 d D . . O18 O -0.2535(6) 0.4845(10) 0.0329(5) 0.066(3) Uani 1 1 d D . . O19 O -0.2690(7) 0.6004(12) -0.0647(6) 0.125(6) Uani 1 1 d D . . N1 N 0.3989(5) 0.7238(9) 0.7912(5) 0.035(2) Uani 1 1 d . . . N2 N 0.5675(5) 0.7274(8) 0.7866(5) 0.0278(19) Uani 1 1 d . . . N3 N 0.6110(5) 0.5097(7) 0.7167(4) 0.0259(18) Uani 1 1 d . . . N4 N 0.4672(5) 0.3360(8) 0.7229(6) 0.033(2) Uani 1 1 d . . . N6 N 0.0337(5) 0.8506(10) 0.2740(5) 0.037(3) Uani 1 1 d . . . N7 N 0.1806(6) 0.6917(11) 0.2633(6) 0.050(3) Uani 1 1 d . . . N8 N 0.1186(5) 0.4586(9) 0.2306(5) 0.033(2) Uani 1 1 d . . . N9 N -0.0510(6) 0.4507(9) 0.2216(5) 0.037(2) Uani 1 1 d . . . N10 N -0.1119(6) 0.6821(10) 0.2397(7) 0.056(3) Uani 1 1 d . . . N11 N 0.4685(10) 0.5951(13) 0.0320(7) 0.051(4) Uani 1 1 d . . . F1 F 0.3606(6) 0.4235(10) 0.5101(4) 0.077(3) Uani 1 1 d . . . F2 F 0.3514(6) 0.4445(9) 0.4037(4) 0.079(3) Uani 1 1 d . . . F3 F 0.3777(6) 0.2798(8) 0.4464(5) 0.076(3) Uani 1 1 d . . . F4 F 0.2262(15) 0.9352(15) 0.5142(11) 0.140(8) Uani 1 1 d U . . F5 F 0.1570(7) 0.9182(9) 0.5886(5) 0.089(3) Uani 1 1 d . . . F6 F 0.1147(12) 0.879(2) 0.4896(9) 0.133(7) Uani 1 1 d . . . F7 F 0.1890(9) 0.1823(14) 0.4324(7) 0.141(6) Uani 1 1 d U . . F8 F 0.2232(8) 0.2180(17) 0.5338(9) 0.155(6) Uani 1 1 d U . . F9 F 0.2062(6) 0.3590(15) 0.4596(8) 0.136(6) Uani 1 1 d U . . F10 F -0.1849(12) 1.1061(15) -0.0516(7) 0.110(6) Uani 1 1 d . . . F11 F -0.2262(11) 0.9624(18) -0.0179(10) 0.127(7) Uani 1 1 d . . . F12 F -0.2247(7) 1.1084(10) 0.0478(5) 0.102(4) Uani 1 1 d . . . F13 F -0.2343(8) 0.3748(14) -0.0839(8) 0.106(8) Uani 1 1 d D . . F14 F -0.1406(8) 0.4841(13) -0.1060(5) 0.111(6) Uani 1 1 d D . . F15 F -0.1214(6) 0.3793(10) -0.0160(5) 0.109(4) Uani 1 1 d D . . C1 C 0.3620(8) 0.7915(11) 0.7477(8) 0.045(3) Uani 1 1 d . . . H1 H 0.3655 0.7792 0.7027 0.054 Uiso 1 1 calc R . . C2 C 0.3162(8) 0.8839(12) 0.7634(8) 0.049(3) Uani 1 1 d . . . H2 H 0.2918 0.9327 0.7301 0.059 Uiso 1 1 calc R . . C3 C 0.3092(8) 0.8988(11) 0.8304(7) 0.049(3) Uani 1 1 d . . . H3 H 0.2776 0.9555 0.8433 0.059 Uiso 1 1 calc R . . C4 C 0.3507(8) 0.8266(12) 0.8772(8) 0.051(3) Uani 1 1 d . . . H4 H 0.3490 0.8354 0.9228 0.061 Uiso 1 1 calc R . . C5 C 0.3942(7) 0.7424(12) 0.8556(7) 0.046(3) Uani 1 1 d . . . H5 H 0.4223 0.6950 0.8877 0.055 Uiso 1 1 calc R . . C6 C 0.5763(7) 0.8092(11) 0.7421(6) 0.035(3) Uani 1 1 d . . . H6 H 0.5549 0.7990 0.6972 0.042 Uiso 1 1 calc R . . C7 C 0.6171(7) 0.9099(11) 0.7617(6) 0.036(3) Uani 1 1 d . . . H7 H 0.6244 0.9643 0.7298 0.043 Uiso 1 1 calc R . . C8 C 0.6462(8) 0.9273(11) 0.8286(6) 0.045(3) Uani 1 1 d . . . H8 H 0.6722 0.9942 0.8429 0.053 Uiso 1 1 calc R . . C9 C 0.6357(7) 0.8427(11) 0.8738(7) 0.044(3) Uani 1 1 d . . . H9 H 0.6552 0.8520 0.9193 0.053 Uiso 1 1 calc R . . C10 C 0.5965(6) 0.7451(10) 0.8520(6) 0.034(3) Uani 1 1 d . . . H10 H 0.5898 0.6893 0.8833 0.041 Uiso 1 1 calc R . . C11 C 0.6143(6) 0.5089(9) 0.6505(5) 0.034(2) Uani 1 1 d . . . H11 H 0.5683 0.5150 0.6202 0.040 Uiso 1 1 calc R . . C12 C 0.6829(8) 0.4995(11) 0.6254(6) 0.045(3) Uani 1 1 d . . . H12 H 0.6836 0.5010 0.5794 0.054 Uiso 1 1 calc R . . C13 C 0.7517(7) 0.4877(10) 0.6722(7) 0.040(3) Uani 1 1 d . . . H13 H 0.7995 0.4812 0.6581 0.048 Uiso 1 1 calc R . . C14 C 0.7458(6) 0.4860(11) 0.7394(7) 0.039(3) Uani 1 1 d . . . H14 H 0.7900 0.4779 0.7716 0.047 Uiso 1 1 calc R . . C15 C 0.6755(7) 0.4962(9) 0.7585(6) 0.038(3) Uani 1 1 d . . . H15 H 0.6732 0.4935 0.8043 0.045 Uiso 1 1 calc R . . C16 C 0.4764(7) 0.2558(12) 0.7728(9) 0.050(4) Uani 1 1 d . . . H16 H 0.4867 0.2814 0.8170 0.060 Uiso 1 1 calc R . . C17 C 0.4717(7) 0.1420(15) 0.7626(7) 0.044(3) Uani 1 1 d . . . H17 H 0.4797 0.0906 0.7982 0.053 Uiso 1 1 calc R . . C18 C 0.4539(7) 0.1050(12) 0.6949(9) 0.056(4) Uani 1 1 d . . . H18 H 0.4478 0.0278 0.6848 0.067 Uiso 1 1 calc R . . C19 C 0.4459(8) 0.1849(12) 0.6443(9) 0.052(4) Uani 1 1 d . . . H19 H 0.4353 0.1618 0.5995 0.062 Uiso 1 1 calc R . . C20 C 0.4535(8) 0.2994(12) 0.6598(8) 0.046(3) Uani 1 1 d . . . H20 H 0.4489 0.3523 0.6251 0.055 Uiso 1 1 calc R . . N5 N 0.3330(4) 0.4912(8) 0.7502(5) 0.056(3) Uani 1 1 d G . . C21 C 0.3044(6) 0.4712(10) 0.8095(5) 0.086(6) Uani 1 1 d GU . . H21 H 0.3382 0.4670 0.8502 0.103 Uiso 1 1 calc R . . C22 C 0.2253(7) 0.4574(12) 0.8079(7) 0.113(8) Uani 1 1 d GU . . H22 H 0.2062 0.4440 0.8476 0.135 Uiso 1 1 calc R . . C23 C 0.1749(4) 0.4636(12) 0.7471(9) 0.118(8) Uani 1 1 d GU . . H23 H 0.1219 0.4544 0.7461 0.142 Uiso 1 1 calc R . . C24 C 0.2035(6) 0.4837(11) 0.6878(8) 0.108(7) Uani 1 1 d GU . . H24 H 0.1697 0.4878 0.6471 0.130 Uiso 1 1 calc R . . C25 C 0.2825(6) 0.4974(9) 0.6894(5) 0.084(6) Uani 1 1 d GU . . H25 H 0.3017 0.5108 0.6497 0.101 Uiso 1 1 calc R . . C26 C 0.0358(6) 0.9308(12) 0.2273(6) 0.034(3) Uani 1 1 d . . . H26 H 0.0385 0.9061 0.1839 0.041 Uiso 1 1 calc R . . C27 C 0.0343(6) 1.0460(19) 0.2375(6) 0.048(3) Uani 1 1 d . . . H27 H 0.0330 1.0973 0.2021 0.058 Uiso 1 1 calc R . . C28 C 0.0350(7) 1.0838(11) 0.3046(6) 0.041(3) Uani 1 1 d . . . H28 H 0.0373 1.1609 0.3155 0.049 Uiso 1 1 calc R . . C29 C 0.0321(8) 1.0008(12) 0.3530(7) 0.047(3) Uani 1 1 d . . . H29 H 0.0301 1.0226 0.3970 0.056 Uiso 1 1 calc R . . C30 C 0.0323(7) 0.8877(11) 0.3375(6) 0.037(3) Uani 1 1 d . . . H30 H 0.0313 0.8344 0.3715 0.045 Uiso 1 1 calc R . . C31 C 0.2144(9) 0.7037(12) 0.2100(8) 0.056(4) Uani 1 1 d . . . H31 H 0.1846 0.7035 0.1673 0.067 Uiso 1 1 calc R . . C32 C 0.2954(9) 0.7168(11) 0.2171(8) 0.053(4) Uani 1 1 d . . . H32 H 0.3194 0.7260 0.1796 0.064 Uiso 1 1 calc R . . C33 C 0.3363(8) 0.7158(13) 0.2785(9) 0.062(4) Uani 1 1 d . . . H33 H 0.3899 0.7219 0.2836 0.074 Uiso 1 1 calc R . . C34 C 0.3011(8) 0.7059(12) 0.3366(8) 0.055(4) Uani 1 1 d . . . H34 H 0.3296 0.7075 0.3798 0.066 Uiso 1 1 calc R . . C35 C 0.2208(8) 0.6935(13) 0.3248(8) 0.052(4) Uani 1 1 d . . . H35 H 0.1948 0.6864 0.3613 0.063 Uiso 1 1 calc R . . C36 C 0.1535(8) 0.3963(13) 0.2798(6) 0.049(3) Uani 1 1 d . . . H36 H 0.1519 0.4210 0.3233 0.059 Uiso 1 1 calc R . . C37 C 0.1933(10) 0.2951(13) 0.2723(7) 0.059(4) Uani 1 1 d . . . H37 H 0.2164 0.2535 0.3095 0.070 Uiso 1 1 calc R . . C38 C 0.1970(9) 0.2588(12) 0.2071(7) 0.052(3) Uani 1 1 d . . . H38 H 0.2226 0.1918 0.1994 0.063 Uiso 1 1 calc R . . C39 C 0.1607(7) 0.3270(10) 0.1529(6) 0.038(3) Uani 1 1 d . . . H39 H 0.1630 0.3070 0.1086 0.046 Uiso 1 1 calc R . . C40 C 0.1230(7) 0.4205(11) 0.1669(6) 0.038(3) Uani 1 1 d . . . H40 H 0.0979 0.4631 0.1309 0.045 Uiso 1 1 calc R . . C41 C -0.0692(7) 0.3847(12) 0.2721(7) 0.041(3) Uani 1 1 d . . . H41 H -0.0517 0.4085 0.3160 0.050 Uiso 1 1 calc R . . C42 C -0.1109(8) 0.2867(11) 0.2635(7) 0.045(3) Uani 1 1 d . . . H42 H -0.1214 0.2438 0.2998 0.053 Uiso 1 1 calc R . . C43 C -0.1367(9) 0.2548(12) 0.1980(8) 0.056(4) Uani 1 1 d . . . H43 H -0.1670 0.1897 0.1890 0.068 Uiso 1 1 calc R . . C44 C -0.1179(8) 0.3189(12) 0.1453(7) 0.049(3) Uani 1 1 d . . . H44 H -0.1337 0.2962 0.1009 0.059 Uiso 1 1 calc R . . C45 C -0.0765(7) 0.4142(11) 0.1596(6) 0.041(3) Uani 1 1 d . . . H45 H -0.0649 0.4575 0.1239 0.050 Uiso 1 1 calc R . . C46 C -0.1442(11) 0.6849(13) 0.2966(11) 0.079(5) Uani 1 1 d . . . H46 H -0.1069 0.6824 0.3352 0.095 Uiso 1 1 calc R . . C47 C -0.2132(11) 0.6896(17) 0.3091(10) 0.064(5) Uani 1 1 d D . . H47 H -0.2276 0.6951 0.3514 0.077 Uiso 1 1 calc R . . C48 C -0.2622(9) 0.6851(13) 0.2484(9) 0.070(4) Uani 1 1 d D . . H48 H -0.3150 0.6820 0.2494 0.084 Uiso 1 1 calc R . . C49 C -0.2390(9) 0.6847(18) 0.1849(13) 0.074(6) Uani 1 1 d . . . H49 H -0.2757 0.6846 0.1458 0.089 Uiso 1 1 calc R . . C50 C -0.1596(8) 0.6844(14) 0.1812(9) 0.072(4) Uani 1 1 d . . . H50 H -0.1416 0.6858 0.1403 0.086 Uiso 1 1 calc R . . C51 C 0.3884(12) 0.3900(13) 0.4557(7) 0.072(5) Uani 1 1 d . . . C52 C 0.1820(12) 0.8815(17) 0.5384(9) 0.081(5) Uani 1 1 d . . . C53 C 0.1795(7) 0.258(2) 0.4790(11) 0.095(6) Uani 1 1 d D . . C54 C -0.1818(14) 1.044(2) 0.0026(10) 0.039(5) Uani 1 1 d . . . C55 C -0.1760(7) 0.4458(13) -0.0540(7) 0.079(7) Uani 1 1 d D . . C56 C 0.5458(10) 0.6086(15) 0.0273(7) 0.067(4) Uani 1 1 d . . . H56 H 0.5763 0.5463 0.0203 0.080 Uiso 1 1 calc R . . C57 C 0.5758(9) 0.7140(16) 0.0332(7) 0.079(6) Uani 1 1 d D . . H57 H 0.6274 0.7250 0.0289 0.095 Uiso 1 1 calc R . . C58 C 0.5321(11) 0.8056(16) 0.0455(10) 0.054(5) Uani 1 1 d D . . H58 H 0.5532 0.8785 0.0499 0.065 Uiso 1 1 calc R . . C59 C 0.4559(11) 0.787(2) 0.0513(11) 0.073(6) Uani 1 1 d . . . H59 H 0.4247 0.8469 0.0610 0.088 Uiso 1 1 calc R . . C60 C 0.4286(8) 0.6854(13) 0.0430(5) 0.054(4) Uani 1 1 d . . . H60 H 0.3764 0.6753 0.0450 0.065 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 0.02576(19) 0.0231(2) 0.0400(3) -0.00262(19) 0.00924(15) -0.00059(17) U2 0.0329(2) 0.0407(3) 0.0327(2) -0.0139(2) 0.01389(17) -0.01057(19) K1 0.0562(17) 0.0359(15) 0.0461(15) -0.0029(12) -0.0131(13) 0.0094(12) K2 0.101(2) 0.0559(18) 0.0483(16) -0.0173(16) 0.0422(16) -0.025(2) K3 0.071(2) 0.064(2) 0.0421(15) -0.0135(14) -0.0169(14) 0.0288(17) S1 0.068(2) 0.0322(16) 0.0346(16) -0.0026(12) 0.0014(14) -0.0055(14) S2 0.065(3) 0.085(3) 0.165(5) -0.077(4) -0.049(3) 0.032(3) S3 0.0425(17) 0.062(2) 0.0322(15) -0.0028(14) 0.0113(13) 0.0048(15) S4 0.126(4) 0.0196(18) 0.0142(17) -0.0006(15) 0.014(2) -0.013(2) S5 0.073(3) 0.089(4) 0.067(3) 0.012(3) 0.015(2) 0.027(3) O1 0.028(4) 0.033(4) 0.044(5) -0.011(4) -0.008(3) 0.003(3) O2 0.054(5) 0.032(4) 0.035(4) 0.004(3) 0.016(4) 0.001(4) O3 0.057(5) 0.054(6) 0.031(4) -0.010(4) 0.024(4) -0.018(4) O4 0.037(4) 0.049(5) 0.030(4) -0.012(4) 0.008(3) -0.002(4) O5 0.110(8) 0.023(4) 0.056(6) -0.017(4) 0.022(5) 0.001(5) O6 0.062(6) 0.047(5) 0.041(5) 0.001(4) -0.003(4) -0.008(5) O7 0.083(7) 0.038(5) 0.032(5) -0.009(4) 0.001(4) -0.004(5) O8 0.046(6) 0.109(9) 0.112(9) 0.043(8) 0.006(6) 0.020(6) O9 0.145(18) 0.085(15) 0.069(12) -0.006(11) 0.040(13) -0.006(13) O10 0.098(11) 0.105(11) 0.240(17) -0.055(12) -0.030(11) 0.008(9) O11 0.121(10) 0.070(7) 0.031(5) -0.013(5) 0.023(6) -0.032(7) O12 0.085(8) 0.077(8) 0.037(5) -0.008(5) -0.004(5) 0.032(6) O13 0.063(6) 0.060(7) 0.084(8) 0.000(6) 0.009(6) 0.007(5) O14 0.102(11) 0.081(10) 0.046(8) 0.005(8) -0.015(8) 0.009(9) O15 0.065(7) 0.191(14) 0.068(7) 0.055(8) -0.010(6) -0.026(8) O16 0.125(11) 0.099(11) 0.195(14) 0.017(11) 0.092(11) 0.010(9) O17 0.103(11) 0.056(9) 0.092(10) -0.009(8) -0.066(9) -0.022(8) O18 0.061(6) 0.090(7) 0.055(6) 0.005(5) 0.035(5) -0.009(5) O19 0.116(10) 0.126(11) 0.108(9) -0.026(8) -0.058(8) 0.080(9) N1 0.037(5) 0.025(5) 0.044(6) -0.002(4) 0.009(4) 0.005(4) N2 0.023(4) 0.025(5) 0.034(5) -0.003(4) 0.004(4) 0.000(4) N3 0.022(4) 0.024(4) 0.034(5) 0.001(4) 0.011(4) 0.009(3) N4 0.030(5) 0.021(5) 0.052(7) -0.001(5) 0.016(4) 0.003(4) N6 0.022(4) 0.054(7) 0.035(6) -0.022(5) 0.007(4) -0.006(4) N7 0.041(6) 0.053(7) 0.064(7) -0.027(6) 0.031(6) -0.026(5) N8 0.038(5) 0.031(5) 0.032(5) 0.003(4) 0.011(4) -0.006(4) N9 0.038(5) 0.044(6) 0.033(5) -0.009(5) 0.013(4) -0.012(4) N10 0.033(6) 0.045(7) 0.096(10) -0.014(6) 0.027(6) 0.000(5) N11 0.064(10) 0.046(9) 0.044(8) -0.010(7) 0.012(7) -0.006(7) F1 0.069(6) 0.106(8) 0.054(5) -0.005(5) 0.002(4) -0.001(5) F2 0.080(6) 0.103(7) 0.047(5) 0.011(5) -0.013(4) 0.017(5) F3 0.087(6) 0.061(6) 0.077(6) -0.016(5) 0.007(5) -0.020(5) F4 0.211(16) 0.087(11) 0.160(14) 0.014(10) 0.141(13) -0.035(11) F5 0.111(8) 0.087(7) 0.079(6) -0.005(5) 0.040(6) 0.036(6) F6 0.134(13) 0.165(15) 0.093(11) 0.025(11) -0.001(10) 0.087(12) F7 0.146(10) 0.172(12) 0.126(9) 0.057(9) 0.090(8) 0.095(9) F8 0.083(8) 0.195(13) 0.173(12) 0.097(11) -0.021(8) 0.005(9) F9 0.060(6) 0.187(13) 0.168(11) 0.102(10) 0.038(7) 0.012(7) F10 0.169(14) 0.100(11) 0.056(7) 0.044(8) 0.000(8) 0.046(10) F11 0.098(10) 0.150(13) 0.126(12) -0.087(11) -0.003(9) -0.057(10) F12 0.129(9) 0.096(8) 0.065(6) 0.015(6) -0.036(6) -0.030(7) F13 0.152(15) 0.047(9) 0.084(11) 0.011(8) -0.081(11) -0.044(10) F14 0.102(10) 0.181(14) 0.066(8) -0.049(9) 0.065(7) -0.063(10) F15 0.104(8) 0.106(8) 0.109(8) -0.007(7) -0.007(6) 0.065(7) C1 0.051(8) 0.026(6) 0.066(9) -0.014(6) 0.030(7) 0.004(6) C2 0.056(8) 0.033(7) 0.063(9) 0.000(7) 0.024(7) 0.010(6) C3 0.055(8) 0.027(7) 0.069(9) -0.001(6) 0.023(7) 0.006(6) C4 0.051(8) 0.045(8) 0.056(8) -0.006(7) 0.006(6) 0.005(6) C5 0.041(7) 0.044(8) 0.052(8) -0.018(6) 0.002(6) 0.009(6) C6 0.035(6) 0.036(7) 0.031(6) 0.009(5) 0.002(5) -0.002(5) C7 0.047(7) 0.028(6) 0.034(6) 0.002(5) 0.008(5) -0.004(5) C8 0.061(8) 0.032(7) 0.040(7) -0.020(5) 0.009(6) -0.017(6) C9 0.045(7) 0.042(7) 0.041(7) -0.001(6) -0.004(5) -0.002(6) C10 0.033(6) 0.037(7) 0.029(6) 0.007(5) -0.003(4) -0.003(5) C11 0.032(6) 0.035(6) 0.032(6) -0.001(5) 0.000(4) -0.003(4) C12 0.056(8) 0.050(7) 0.035(6) -0.002(5) 0.026(6) 0.004(6) C13 0.032(6) 0.025(6) 0.065(8) -0.003(5) 0.019(5) -0.005(5) C14 0.020(5) 0.033(7) 0.061(8) -0.009(6) -0.006(5) -0.001(5) C15 0.040(6) 0.021(6) 0.050(7) -0.015(5) 0.000(5) -0.007(5) C16 0.031(6) 0.038(8) 0.084(10) 0.014(7) 0.022(6) 0.005(5) C17 0.046(7) 0.026(7) 0.065(8) -0.008(7) 0.021(6) -0.014(5) C18 0.042(7) 0.027(7) 0.108(13) -0.021(8) 0.039(8) -0.004(5) C19 0.042(7) 0.036(8) 0.081(11) -0.019(7) 0.023(7) -0.010(6) C20 0.047(7) 0.034(7) 0.063(9) -0.005(7) 0.025(6) 0.000(6) N5 0.032(6) 0.019(5) 0.119(10) 0.004(6) 0.019(6) 0.008(4) C21 0.075(10) 0.063(10) 0.140(14) -0.051(10) 0.073(10) -0.046(8) C22 0.113(13) 0.084(12) 0.167(16) -0.065(12) 0.101(13) -0.017(10) C23 0.105(11) 0.092(11) 0.161(12) -0.023(9) 0.030(9) 0.008(9) C24 0.060(10) 0.049(10) 0.202(18) 0.001(12) -0.019(11) 0.011(8) C25 0.042(8) 0.048(9) 0.157(15) 0.017(10) -0.002(9) -0.012(7) C26 0.027(5) 0.047(8) 0.028(6) -0.007(6) 0.003(4) -0.003(5) C27 0.038(7) 0.072(11) 0.033(6) 0.001(8) 0.001(5) 0.013(8) C28 0.039(6) 0.037(8) 0.047(7) -0.009(6) 0.010(5) 0.005(5) C29 0.050(7) 0.054(9) 0.040(7) -0.016(6) 0.023(6) -0.004(6) C30 0.039(6) 0.041(7) 0.034(6) 0.004(6) 0.011(5) 0.006(5) C31 0.055(8) 0.040(8) 0.082(10) -0.036(7) 0.038(8) -0.015(6) C32 0.063(9) 0.026(6) 0.083(10) -0.020(7) 0.045(8) -0.008(6) C33 0.038(7) 0.046(8) 0.109(12) 0.005(8) 0.035(8) 0.010(6) C34 0.038(7) 0.042(8) 0.085(10) 0.010(7) 0.011(7) -0.008(6) C35 0.036(7) 0.049(8) 0.071(9) -0.019(7) 0.007(6) -0.004(6) C36 0.066(9) 0.059(9) 0.023(6) 0.005(6) 0.008(6) -0.010(7) C37 0.087(11) 0.041(8) 0.048(8) 0.007(7) 0.012(8) 0.000(7) C38 0.069(9) 0.034(7) 0.058(8) 0.009(6) 0.026(7) -0.001(6) C39 0.052(7) 0.030(7) 0.034(6) 0.003(5) 0.011(5) -0.008(5) C40 0.039(6) 0.038(7) 0.035(6) -0.005(5) 0.002(5) 0.006(5) C41 0.034(6) 0.046(8) 0.047(7) 0.003(6) 0.014(5) -0.005(6) C42 0.052(8) 0.025(6) 0.053(8) 0.005(6) -0.003(6) 0.003(5) C43 0.066(9) 0.034(7) 0.061(9) -0.007(7) -0.013(7) -0.015(6) C44 0.057(8) 0.038(7) 0.049(8) -0.009(6) -0.001(6) -0.003(6) C45 0.045(7) 0.037(7) 0.041(7) -0.006(5) 0.002(5) -0.007(5) C46 0.079(10) 0.044(8) 0.132(14) -0.006(9) 0.071(10) 0.001(7) C47 0.065(9) 0.049(8) 0.086(10) 0.005(7) 0.034(8) 0.010(7) C48 0.060(7) 0.056(7) 0.100(9) -0.002(7) 0.032(7) -0.001(6) C49 0.068(9) 0.052(9) 0.093(10) -0.013(8) -0.013(8) -0.018(7) C50 0.053(7) 0.068(7) 0.095(8) -0.040(7) 0.010(6) 0.002(6) C51 0.127(15) 0.048(9) 0.029(7) 0.005(6) -0.016(8) 0.008(9) C52 0.096(9) 0.077(9) 0.071(8) 0.013(7) 0.020(7) 0.030(8) C53 0.092(9) 0.103(10) 0.084(9) 0.032(8) -0.004(8) 0.008(8) C54 0.056(9) 0.028(8) 0.026(8) -0.001(7) -0.016(7) 0.006(8) C55 0.074(10) 0.089(11) 0.074(10) 0.005(9) 0.010(8) 0.011(9) C56 0.072(10) 0.071(11) 0.058(9) 0.010(8) 0.010(7) 0.010(8) C57 0.054(9) 0.125(16) 0.051(9) 0.024(10) -0.015(7) -0.038(10) C58 0.081(10) 0.029(8) 0.041(8) 0.010(7) -0.022(7) -0.002(7) C59 0.092(10) 0.056(9) 0.060(9) -0.006(7) -0.020(8) 0.031(8) C60 0.051(7) 0.083(10) 0.020(5) -0.013(6) -0.021(5) 0.026(7) _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 1.816(8) . ? U1 O1 1.855(8) . ? U1 N2 2.608(9) . ? U1 N4 2.615(10) . ? U1 N1 2.614(10) . ? U1 N5 2.617(7) . ? U1 N3 2.622(8) . ? U1 K1 4.458(3) . ? U2 O3 1.823(8) . ? U2 O4 1.844(8) . ? U2 N10 2.588(11) . ? U2 N8 2.591(10) . ? U2 N9 2.607(10) . ? U2 N6 2.606(11) . ? U2 N7 2.638(10) . ? U2 K2 4.477(3) . ? U2 K3 4.492(3) . ? K1 O1 2.611(9) . ? K1 O5 2.684(10) . ? K1 O6 2.773(10) 2_656 ? K1 O8 2.802(12) . ? K1 O7 2.826(10) 2_656 ? K2 O13 2.612(12) 2_556 ? K2 O3 2.655(9) . ? K2 O11 2.721(12) . ? K2 O10 2.791(18) . ? K2 O12 2.897(13) . ? K2 O9 3.07(3) . ? K3 O16 2.642(16) 2_545 ? K3 O4 2.672(9) . ? K3 O17 2.787(11) . ? K3 O14 2.797(18) . ? K3 O15 3.18(2) . ? S1 O6 1.431(9) . ? S1 O5 1.438(10) . ? S1 O7 1.456(9) . ? S1 C51 1.85(2) . ? S2 O9 1.409(10) . ? S2 O8 1.423(8) . ? S2 O10 1.486(10) . ? S2 C52 1.786(19) . ? S3 O12 1.409(10) . ? S3 O11 1.438(10) . ? S3 O13 1.449(12) . ? S3 C53 1.800(10) . ? S4 O15 1.381(13) . ? S4 O16 1.429(19) . ? S4 O14 1.475(19) . ? S4 C54 1.61(2) . ? S5 O19 1.349(10) . ? S5 O18 1.459(10) . ? S5 O17 1.463(11) . ? S5 C55 1.670(17) . ? O6 K1 2.774(10) 2_646 ? O7 K1 2.826(10) 2_646 ? O13 K2 2.612(12) 2_546 ? O16 K3 2.642(16) 2 ? N1 C1 1.276(17) . ? N1 C5 1.333(16) . ? N2 C6 1.341(15) . ? N2 C10 1.349(14) . ? N3 C15 1.303(14) . ? N3 C11 1.346(14) . ? N4 C20 1.325(18) . ? N4 C16 1.369(18) . ? N6 C26 1.336(18) . ? N6 C30 1.356(15) . ? N7 C31 1.316(17) . ? N7 C35 1.322(19) . ? N8 C36 1.300(16) . ? N8 C40 1.373(15) . ? N9 C45 1.328(15) . ? N9 C41 1.357(16) . ? N10 C50 1.329(17) . ? N10 C46 1.36(2) . ? N11 C60 1.31(2) . ? N11 C56 1.38(2) . ? F1 C51 1.332(19) . ? F2 C51 1.304(16) . ? F3 C51 1.316(18) . ? F4 C52 1.17(2) . ? F5 C52 1.24(2) . ? F6 C52 1.40(3) . ? F7 C53 1.32(3) . ? F8 C53 1.32(2) . ? F9 C53 1.36(2) . ? F10 C54 1.31(3) . ? F11 C54 1.26(3) . ? F12 C54 1.48(3) . ? F13 C55 1.377(10) . ? F14 C55 1.379(10) . ? F15 C55 1.367(10) . ? F15 K3 2.919(11) 2_545 ? C1 C2 1.416(17) . ? C1 H1 0.9300 . ? C2 C3 1.39(2) . ? C2 H2 0.9300 . ? C3 C4 1.382(19) . ? C3 H3 0.9300 . ? C4 C5 1.363(18) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.403(18) . ? C6 H6 0.9300 . ? C7 C8 1.374(17) . ? C7 H7 0.9300 . ? C8 C9 1.382(19) . ? C8 H8 0.9300 . ? C9 C10 1.369(17) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.382(16) . ? C11 H11 0.9300 . ? C12 C13 1.409(18) . ? C12 H12 0.9300 . ? C13 C14 1.375(18) . ? C13 H13 0.9300 . ? C14 C15 1.356(18) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.35(2) . ? C16 H16 0.9300 . ? C17 C18 1.42(2) . ? C17 H17 0.9300 . ? C18 C19 1.38(2) . ? C18 H18 0.9300 . ? C19 C20 1.381(19) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? N5 C21 1.3900 . ? N5 C25 1.3900 . ? C21 C22 1.3900 . ? C21 H21 0.9300 . ? C22 C23 1.3900 . ? C22 H22 0.9300 . ? C23 C24 1.3900 . ? C23 H23 0.9300 . ? C24 C25 1.3900 . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.37(3) . ? C26 H26 0.9300 . ? C27 C28 1.422(18) . ? C27 H27 0.9300 . ? C28 C29 1.386(19) . ? C28 H28 0.9300 . ? C29 C30 1.363(19) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.41(2) . ? C31 H31 0.9300 . ? C32 C33 1.32(2) . ? C32 H32 0.9300 . ? C33 C34 1.42(2) . ? C33 H33 0.9300 . ? C34 C35 1.394(18) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C37 1.40(2) . ? C36 H36 0.9300 . ? C37 C38 1.39(2) . ? C37 H37 0.9300 . ? C38 C39 1.418(18) . ? C38 H38 0.9300 . ? C39 C40 1.335(17) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 C42 1.359(19) . ? C41 H41 0.9300 . ? C42 C43 1.375(19) . ? C42 H42 0.9300 . ? C43 C44 1.39(2) . ? C43 H43 0.9300 . ? C44 C45 1.338(18) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 C47 1.28(3) . ? C46 H46 0.9300 . ? C47 C48 1.38(3) . ? C47 H47 0.9300 . ? C48 C49 1.41(3) . ? C48 H48 0.9300 . ? C49 C50 1.41(3) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? C56 C57 1.34(2) . ? C56 H56 0.9300 . ? C57 C58 1.37(3) . ? C57 H57 0.9300 . ? C58 C59 1.38(3) . ? C58 H58 0.9300 . ? C59 C60 1.29(3) . ? C59 H59 0.9300 . ? C60 H60 0.9300 . ? 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 O1 179.6(4) . . ? O2 U1 N2 86.1(3) . . ? O1 U1 N2 94.3(3) . . ? O2 U1 N4 86.5(4) . . ? O1 U1 N4 93.3(3) . . ? N2 U1 N4 147.0(3) . . ? O2 U1 N1 90.8(3) . . ? O1 U1 N1 89.1(3) . . ? N2 U1 N1 69.3(3) . . ? N4 U1 N1 142.9(3) . . ? O2 U1 N5 92.6(4) . . ? O1 U1 N5 87.0(3) . . ? N2 U1 N5 139.9(3) . . ? N4 U1 N5 72.5(3) . . ? N1 U1 N5 70.7(3) . . ? O2 U1 N3 96.3(3) . . ? O1 U1 N3 84.1(3) . . ? N2 U1 N3 72.0(3) . . ? N4 U1 N3 76.9(3) . . ? N1 U1 N3 140.0(3) . . ? N5 U1 N3 147.6(3) . . ? O3 U2 O4 178.7(4) . . ? O3 U2 N10 91.1(4) . . ? O4 U2 N10 89.2(4) . . ? O3 U2 N8 90.5(4) . . ? O4 U2 N8 90.1(3) . . ? N10 U2 N8 138.6(3) . . ? O3 U2 N9 89.2(4) . . ? O4 U2 N9 92.1(3) . . ? N10 U2 N9 69.5(3) . . ? N8 U2 N9 69.1(3) . . ? O3 U2 N6 88.8(4) . . ? O4 U2 N6 90.1(4) . . ? N10 U2 N6 76.4(3) . . ? N8 U2 N6 145.0(3) . . ? N9 U2 N6 145.8(3) . . ? O3 U2 N7 89.6(4) . . ? O4 U2 N7 89.5(4) . . ? N10 U2 N7 152.0(4) . . ? N8 U2 N7 69.4(3) . . ? N9 U2 N7 138.5(4) . . ? N6 U2 N7 75.6(3) . . ? O1 K1 O5 94.3(3) . . ? O1 K1 O6 133.0(3) . 2_656 ? O5 K1 O6 84.5(3) . 2_656 ? O1 K1 O8 80.4(3) . . ? O5 K1 O8 148.7(4) . . ? O6 K1 O8 121.5(4) 2_656 . ? O1 K1 O7 88.9(3) . 2_656 ? O5 K1 O7 115.2(3) . 2_656 ? O6 K1 O7 51.1(3) 2_656 2_656 ? O8 K1 O7 95.6(4) . 2_656 ? O13 K2 O3 98.6(4) 2_556 . ? O13 K2 O11 108.1(4) 2_556 . ? O3 K2 O11 137.2(3) . . ? O13 K2 O10 85.8(4) 2_556 . ? O3 K2 O10 123.5(4) . . ? O11 K2 O10 91.9(4) . . ? O13 K2 O12 120.3(4) 2_556 . ? O3 K2 O12 87.4(3) . . ? O11 K2 O12 50.3(3) . . ? O10 K2 O12 137.7(4) . . ? O13 K2 O9 116.6(5) 2_556 . ? O3 K2 O9 85.9(4) . . ? O11 K2 O9 109.9(6) . . ? O10 K2 O9 44.8(3) . . ? O12 K2 O9 123.1(5) . . ? O16 K3 O4 110.4(5) 2_545 . ? O16 K3 O17 93.3(5) 2_545 . ? O4 K3 O17 90.3(3) . . ? O16 K3 O14 116.1(6) 2_545 . ? O4 K3 O14 127.8(4) . . ? O17 K3 O14 108.8(5) . . ? O16 K3 O15 163.4(5) 2_545 . ? O4 K3 O15 84.2(3) . . ? O17 K3 O15 94.6(5) . . ? O14 K3 O15 47.3(4) . . ? O6 S1 O5 113.3(6) . . ? O6 S1 O7 113.5(6) . . ? O5 S1 O7 117.4(6) . . ? O6 S1 C51 105.5(6) . . ? O5 S1 C51 101.8(7) . . ? O7 S1 C51 103.2(6) . . ? O8 S2 O9 126.1(16) . . ? O8 S2 O10 102.7(10) . . ? O9 S2 O10 101.9(15) . . ? O8 S2 C52 105.6(9) . . ? O9 S2 C52 114.9(14) . . ? O10 S2 C52 102.2(10) . . ? O12 S3 O11 114.4(7) . . ? O12 S3 O13 115.2(7) . . ? O11 S3 O13 116.1(7) . . ? O12 S3 C53 101.8(8) . . ? O11 S3 C53 105.3(10) . . ? O13 S3 C53 101.3(9) . . ? O15 S4 O16 110.6(11) . . ? O15 S4 O14 116.1(11) . . ? O16 S4 O14 102.8(11) . . ? O15 S4 C54 114.0(11) . . ? O16 S4 C54 104.5(12) . . ? O14 S4 C54 107.8(10) . . ? O19 S5 O18 115.2(8) . . ? O19 S5 O17 121.3(9) . . ? O18 S5 O17 113.9(7) . . ? O19 S5 C55 106.4(8) . . ? O18 S5 C55 101.7(8) . . ? O17 S5 C55 93.1(9) . . ? U1 O1 K1 173.1(4) . . ? U2 O3 K2 177.0(5) . . ? U2 O4 K3 168.0(4) . . ? S1 O5 K1 137.7(7) . . ? S1 O6 K1 98.7(5) . 2_646 ? S1 O7 K1 95.9(4) . 2_646 ? S2 O8 K1 104.9(7) . . ? S2 O9 K2 100.7(14) . . ? S2 O10 K2 111.4(10) . . ? S3 O11 K2 99.3(5) . . ? S3 O12 K2 92.5(5) . . ? S3 O13 K2 137.8(6) . 2_546 ? S4 O14 K3 105.1(8) . . ? S4 O15 K3 91.0(8) . . ? S4 O16 K3 127.5(11) . 2 ? S5 O17 K3 162.9(8) . . ? C1 N1 C5 117.5(11) . . ? C1 N1 U1 120.6(8) . . ? C5 N1 U1 121.9(8) . . ? C6 N2 C10 118.5(10) . . ? C6 N2 U1 121.6(7) . . ? C10 N2 U1 119.1(7) . . ? C15 N3 C11 117.8(10) . . ? C15 N3 U1 124.1(8) . . ? C11 N3 U1 118.0(7) . . ? C20 N4 C16 117.6(13) . . ? C20 N4 U1 122.4(9) . . ? C16 N4 U1 120.0(10) . . ? C21 N5 C25 120.0 . . ? C21 N5 U1 120.5(5) . . ? C25 N5 U1 118.6(5) . . ? C26 N6 C30 116.5(12) . . ? C26 N6 U2 122.4(8) . . ? C30 N6 U2 121.1(9) . . ? C31 N7 C35 121.5(13) . . ? C31 N7 U2 118.9(10) . . ? C35 N7 U2 119.0(9) . . ? C36 N8 C40 116.0(11) . . ? C36 N8 U2 124.2(9) . . ? C40 N8 U2 119.6(7) . . ? C45 N9 C41 116.0(11) . . ? C45 N9 U2 122.4(8) . . ? C41 N9 U2 121.6(8) . . ? C50 N10 C46 117.4(7) . . ? C50 N10 U2 121.2(6) . . ? C46 N10 U2 120.3(12) . . ? C60 N11 C56 118.3(15) . . ? N1 C1 C2 124.4(13) . . ? N1 C1 H1 117.8 . . ? C2 C1 H1 117.8 . . ? C3 C2 C1 117.3(13) . . ? C3 C2 H2 121.4 . . ? C1 C2 H2 121.4 . . ? C4 C3 C2 117.9(12) . . ? C4 C3 H3 121.1 . . ? C2 C3 H3 121.1 . . ? C5 C4 C3 119.0(14) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N1 C5 C4 123.9(13) . . ? N1 C5 H5 118.0 . . ? C4 C5 H5 118.1 . . ? N2 C6 C7 121.7(11) . . ? N2 C6 H6 119.1 . . ? C7 C6 H6 119.2 . . ? C8 C7 C6 119.3(12) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.3 . . ? C7 C8 C9 118.2(11) . . ? C7 C8 H8 120.9 . . ? C9 C8 H8 120.9 . . ? C10 C9 C8 120.2(11) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? N2 C10 C9 122.1(11) . . ? N2 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? N3 C11 C12 123.0(10) . . ? N3 C11 H11 118.4 . . ? C12 C11 H11 118.5 . . ? C11 C12 C13 117.6(11) . . ? C11 C12 H12 121.2 . . ? C13 C12 H12 121.2 . . ? C14 C13 C12 117.7(10) . . ? C14 C13 H13 121.1 . . ? C12 C13 H13 121.1 . . ? C15 C14 C13 119.9(11) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? N3 C15 C14 123.9(12) . . ? N3 C15 H15 118.0 . . ? C14 C15 H15 118.0 . . ? C17 C16 N4 124.8(17) . . ? C17 C16 H16 117.4 . . ? N4 C16 H16 117.6 . . ? C16 C17 C18 116.6(16) . . ? C16 C17 H17 121.9 . . ? C18 C17 H17 121.7 . . ? C19 C18 C17 119.0(13) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C18 C19 C20 120.0(15) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? N4 C20 C19 121.9(14) . . ? N4 C20 H20 119.1 . . ? C19 C20 H20 119.1 . . ? C21 N5 C25 120.0 . . ? C21 N5 U1 120.5(5) . . ? C25 N5 U1 118.6(5) . . ? C22 C21 N5 120.0 . . ? C22 C21 H21 120.0 . . ? N5 C21 H21 120.0 . . ? C21 C22 C23 120.0 . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C22 C23 C24 120.0 . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C25 120.0 . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C24 C25 N5 120.0 . . ? C24 C25 H25 120.0 . . ? N5 C25 H25 120.0 . . ? N6 C26 C27 125.9(12) . . ? N6 C26 H26 117.0 . . ? C27 C26 H26 117.2 . . ? C26 C27 C28 117.0(15) . . ? C26 C27 H27 121.3 . . ? C28 C27 H27 121.3 . . ? C29 C28 C27 117.0(14) . . ? C29 C28 H28 121.5 . . ? C27 C28 H28 121.7 . . ? C30 C29 C28 121.5(12) . . ? C30 C29 H29 119.3 . . ? C28 C29 H29 119.3 . . ? N6 C30 C29 121.9(12) . . ? N6 C30 H30 119.0 . . ? C29 C30 H30 119.0 . . ? N7 C31 C32 120.6(16) . . ? N7 C31 H31 119.7 . . ? C32 C31 H31 119.5 . . ? C33 C32 C31 118.3(14) . . ? C33 C32 H32 120.8 . . ? C31 C32 H32 121.1 . . ? C32 C33 C34 122.1(13) . . ? C32 C33 H33 119.0 . . ? C34 C33 H33 118.9 . . ? C35 C34 C33 115.7(15) . . ? C35 C34 H34 122.2 . . ? C33 C34 H34 122.2 . . ? N7 C35 C34 121.8(14) . . ? N7 C35 H35 119.1 . . ? C34 C35 H35 119.1 . . ? N8 C36 C37 125.1(13) . . ? N8 C36 H36 117.5 . . ? C37 C36 H36 117.4 . . ? C38 C37 C36 117.6(13) . . ? C38 C37 H37 121.3 . . ? C36 C37 H37 121.2 . . ? C37 C38 C39 118.0(13) . . ? C37 C38 H38 120.9 . . ? C39 C38 H38 120.9 . . ? C40 C39 C38 118.3(12) . . ? C40 C39 H39 120.9 . . ? C38 C39 H39 120.9 . . ? C39 C40 N8 124.9(11) . . ? C39 C40 H40 117.5 . . ? N8 C40 H40 117.6 . . ? N9 C41 C42 125.2(13) . . ? N9 C41 H41 117.5 . . ? C42 C41 H41 117.4 . . ? C41 C42 C43 115.9(13) . . ? C41 C42 H42 122.0 . . ? C43 C42 H42 122.1 . . ? C42 C43 C44 120.5(13) . . ? C42 C43 H43 119.7 . . ? C44 C43 H43 119.8 . . ? C45 C44 C43 118.5(13) . . ? C45 C44 H44 120.6 . . ? C43 C44 H44 120.7 . . ? N9 C45 C44 123.9(13) . . ? N9 C45 H45 118.0 . . ? C44 C45 H45 118.1 . . ? C47 C46 N10 135(2) . . ? C47 C46 H46 112.3 . . ? N10 C46 H46 112.4 . . ? C46 C47 C48 107.1(16) . . ? C46 C47 H47 126.7 . . ? C48 C47 H47 126.6 . . ? C47 C48 C49 125.4(18) . . ? C47 C48 H48 117.2 . . ? C49 C48 H48 116.9 . . ? C50 C49 C48 119.0(19) . . ? C50 C49 H49 120.7 . . ? C48 C49 H49 120.9 . . ? N10 C50 C49 115.8(18) . . ? N10 C50 H50 122.4 . . ? C49 C50 H50 121.9 . . ? F2 C51 F3 109.1(12) . . ? F2 C51 F1 108.4(15) . . ? F3 C51 F1 110.1(15) . . ? F2 C51 S1 111.3(13) . . ? F3 C51 S1 110.2(13) . . ? F1 C51 S1 107.6(10) . . ? F4 C52 F5 120(2) . . ? F4 C52 F6 105(2) . . ? F5 C52 F6 102.0(17) . . ? F4 C52 S2 108.8(17) . . ? F5 C52 S2 115.6(14) . . ? F6 C52 S2 103.1(16) . . ? F7 C53 F8 103.7(18) . . ? F7 C53 F9 106.9(16) . . ? F8 C53 F9 111.6(18) . . ? F7 C53 S3 112.7(14) . . ? F8 C53 S3 112.9(13) . . ? F9 C53 S3 108.9(12) . . ? F11 C54 F10 102.1(19) . . ? F11 C54 F12 104(2) . . ? F10 C54 F12 106.1(18) . . ? F11 C54 S4 115.4(19) . . ? F10 C54 S4 114(2) . . ? F12 C54 S4 113.6(13) . . ? F15 C55 F13 107.4(10) . . ? F15 C55 F14 104.6(10) . . ? F13 C55 F14 105.0(10) . . ? F15 C55 S5 118.8(10) . . ? F13 C55 S5 106.5(12) . . ? F14 C55 S5 113.6(11) . . ? C57 C56 N11 118.3(16) . . ? C57 C56 H56 121.0 . . ? N11 C56 H56 120.7 . . ? C56 C57 C58 121.2(16) . . ? C56 C57 H57 119.3 . . ? C58 C57 H57 119.3 . . ? C59 C58 C57 118.2(18) . . ? C57 C58 H58 121.0 . . ? C59 C58 H58 121.3 . . ? C58 C59 C60 118.7(19) . . ? C60 C59 H59 120.5 . . ? C58 C59 H59 120.3 . . ? N11 C60 C59 125.2(16) . . ? C59 C60 H60 117.5 . . ? N11 C60 H60 117.4 . . ? #===END data_5.py _database_code_depnum_ccdc_archive 'CCDC 711337' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H60 F6 K N12 O10 S2 U2, C F3 O3 S, C5 H5 N' _chemical_formula_sum 'C68 H65 F9 K N13 O13 S3 U2' _chemical_formula_weight 2054.67 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' K K 0.2009 0.2494 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 19.0805(4) _cell_length_b 20.0091(8) _cell_length_c 20.5906(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7861.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 128320 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 25.68 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent dark orange' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4000 _exptl_absorpt_coefficient_mu 4.336 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.398 _exptl_absorpt_correction_T_max 0.621 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 40 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 area-detector diffractometer' _diffrn_measurement_method 'two \f and three \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 128320 _diffrn_reflns_av_R_equivalents 0.0722 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.68 _reflns_number_total 14875 _reflns_number_gt 12835 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _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 and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 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^)+(0.0423P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.009(3) _refine_ls_number_reflns 14875 _refine_ls_number_parameters 983 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0721 _refine_ls_wR_factor_gt 0.0691 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.815 _refine_diff_density_min -0.987 _refine_diff_density_rms 0.096 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 0.767109(11) 0.531524(10) 0.029577(11) 0.02685(6) Uani 1 1 d . . . U2 U 1.227689(10) 0.498496(10) 0.149027(9) 0.02377(6) Uani 1 1 d . . . K K 0.99685(5) 0.51236(6) 0.08893(6) 0.0263(3) Uani 1 1 d . . . S1 S 0.96443(7) 0.32644(7) 0.13595(8) 0.0310(4) Uani 1 1 d . . . S2 S 1.00839(7) 0.71235(7) 0.06139(8) 0.0285(3) Uani 1 1 d . . . S3 S 0.50224(8) 0.72287(8) 0.29365(9) 0.0416(4) Uani 1 1 d . . . O1 O 0.85777(17) 0.51079(19) 0.05222(18) 0.0315(10) Uani 1 1 d . . . O2 O 0.67846(18) 0.5543(2) 0.00450(19) 0.0346(10) Uani 1 1 d . . . O3 O 1.13682(16) 0.50406(19) 0.12096(18) 0.0275(8) Uani 1 1 d . . . O4 O 1.31823(16) 0.49393(19) 0.17722(18) 0.0271(8) Uani 1 1 d . . . O5 O 1.0051(2) 0.3868(2) 0.1320(2) 0.0465(12) Uani 1 1 d . . . O6 O 0.9985(2) 0.2726(2) 0.1690(2) 0.0438(11) Uani 1 1 d . . . O7 O 0.89194(19) 0.3369(2) 0.1518(2) 0.0448(12) Uani 1 1 d . . . O8 O 1.0125(2) 0.64659(19) 0.0910(2) 0.0398(11) Uani 1 1 d . . . O9 O 1.0459(2) 0.7186(2) 0.0011(2) 0.0355(10) Uani 1 1 d . . . O10 O 0.9401(2) 0.7427(2) 0.0627(2) 0.0401(11) Uani 1 1 d . . . O11 O 0.5023(3) 0.7056(3) 0.3623(2) 0.0590(14) Uani 1 1 d . . . O12 O 0.5688(2) 0.7170(2) 0.2628(2) 0.0539(13) Uani 1 1 d . . . O13 O 0.4434(2) 0.6958(2) 0.2579(2) 0.0419(11) Uani 1 1 d . . . N1 N 0.7884(2) 0.4770(2) -0.0837(2) 0.0294(11) Uani 1 1 d . . . N2 N 0.7179(2) 0.4077(2) 0.0309(2) 0.0334(11) Uani 1 1 d . . . N3 N 0.7275(2) 0.4940(2) 0.1457(2) 0.0300(10) Uani 1 1 d . . . N4 N 0.7679(3) 0.6369(2) 0.1051(2) 0.0311(11) Uani 1 1 d . . . N5 N 0.8110(2) 0.6255(2) -0.0475(2) 0.0299(11) Uani 1 1 d . . . N6 N 1.2645(2) 0.4570(2) 0.0333(2) 0.0297(10) Uani 1 1 d . . . N7 N 1.2302(3) 0.3675(2) 0.1445(2) 0.0323(11) Uani 1 1 d . . . N8 N 1.1770(2) 0.4562(2) 0.2585(2) 0.0252(11) Uani 1 1 d . . . N9 N 1.2189(2) 0.6050(2) 0.2217(2) 0.0256(10) Uani 1 1 d . . . N10 N 1.2543(2) 0.6008(2) 0.0760(2) 0.0262(11) Uani 1 1 d . . . N11 N 0.9547(2) 0.5405(3) 0.2242(2) 0.0353(12) Uani 1 1 d . . . N12 N 1.0396(2) 0.5054(3) -0.0487(2) 0.0365(12) Uani 1 1 d . . . F1 F 0.9232(3) 0.2441(3) 0.0454(3) 0.106(2) Uani 1 1 d . . . F2 F 0.9334(2) 0.3453(3) 0.0130(2) 0.0753(15) Uani 1 1 d . . . F3 F 1.0262(2) 0.2865(3) 0.0294(2) 0.0862(17) Uani 1 1 d . . . F4 F 1.0582(2) 0.82843(17) 0.09828(18) 0.0476(10) Uani 1 1 d . . . F5 F 1.12502(16) 0.74534(18) 0.12152(18) 0.0416(9) Uani 1 1 d . . . F6 F 1.03040(18) 0.76261(18) 0.17718(17) 0.0410(9) Uani 1 1 d . . . F7 F 0.5328(2) 0.8438(2) 0.3325(3) 0.0796(15) Uani 1 1 d . . . F8 F 0.4880(2) 0.8381(2) 0.2363(2) 0.0700(13) Uani 1 1 d . . . F9 F 0.4229(2) 0.8247(2) 0.3193(2) 0.0648(12) Uani 1 1 d . . . C1 C 0.8510(3) 0.4480(3) -0.0980(3) 0.0378(16) Uani 1 1 d . . . H1 H 0.8885 0.4536 -0.0696 0.045 Uiso 1 1 calc R . . C2 C 0.8603(3) 0.4105(3) -0.1533(3) 0.0414(16) Uani 1 1 d . . . H2 H 0.9038 0.3915 -0.1617 0.050 Uiso 1 1 calc R . . C3 C 0.8074(4) 0.4011(3) -0.1951(3) 0.0450(17) Uani 1 1 d . . . H3 H 0.8137 0.3751 -0.2321 0.054 Uiso 1 1 calc R . . C4 C 0.7433(3) 0.4305(3) -0.1823(3) 0.0399(16) Uani 1 1 d . . . H4 H 0.7060 0.4253 -0.2108 0.048 Uiso 1 1 calc R . . C5 C 0.7359(3) 0.4681(3) -0.1262(3) 0.0403(14) Uani 1 1 d . . . H5 H 0.6928 0.4879 -0.1176 0.048 Uiso 1 1 calc R . . C6 C 0.7578(3) 0.3550(3) 0.0429(3) 0.0370(16) Uani 1 1 d . . . H6 H 0.8060 0.3614 0.0456 0.044 Uiso 1 1 calc R . . C7 C 0.7322(4) 0.2918(3) 0.0517(3) 0.0444(16) Uani 1 1 d . . . H7 H 0.7623 0.2562 0.0600 0.053 Uiso 1 1 calc R . . C8 C 0.6612(4) 0.2821(3) 0.0479(3) 0.0501(19) Uani 1 1 d . . . H8 H 0.6421 0.2399 0.0544 0.060 Uiso 1 1 calc R . . C9 C 0.6185(3) 0.3361(4) 0.0343(4) 0.0467(17) Uani 1 1 d . . . H9 H 0.5702 0.3306 0.0305 0.056 Uiso 1 1 calc R . . C10 C 0.6483(3) 0.3979(3) 0.0267(3) 0.0352(14) Uani 1 1 d . . . H10 H 0.6195 0.4344 0.0184 0.042 Uiso 1 1 calc R . . C11 C 0.7696(3) 0.4528(3) 0.1806(3) 0.0330(13) Uani 1 1 d . . . H11 H 0.8157 0.4464 0.1671 0.040 Uiso 1 1 calc R . . C12 C 0.7461(3) 0.4200(3) 0.2358(3) 0.0370(16) Uani 1 1 d . . . H12 H 0.7764 0.3932 0.2597 0.044 Uiso 1 1 calc R . . C13 C 0.6771(3) 0.4276(3) 0.2547(3) 0.0401(16) Uani 1 1 d . . . H13 H 0.6598 0.4047 0.2906 0.048 Uiso 1 1 calc R . . C14 C 0.6345(3) 0.4696(3) 0.2199(3) 0.0373(15) Uani 1 1 d . . . H14 H 0.5882 0.4762 0.2323 0.045 Uiso 1 1 calc R . . C15 C 0.6614(3) 0.5022(3) 0.1655(3) 0.0325(13) Uani 1 1 d . . . H15 H 0.6323 0.5308 0.1422 0.039 Uiso 1 1 calc R . . C16 C 0.7076(3) 0.6699(3) 0.1155(3) 0.0373(16) Uani 1 1 d . . . H16 H 0.6678 0.6577 0.0923 0.045 Uiso 1 1 calc R . . C17 C 0.7031(3) 0.7222(3) 0.1602(3) 0.0404(17) Uani 1 1 d . . . H17 H 0.6608 0.7442 0.1667 0.048 Uiso 1 1 calc R . . C18 C 0.7619(4) 0.7409(3) 0.1948(3) 0.0432(17) Uani 1 1 d . . . H18 H 0.7594 0.7750 0.2254 0.052 Uiso 1 1 calc R . . C19 C 0.8239(4) 0.7085(3) 0.1834(3) 0.0436(17) Uani 1 1 d . . . H19 H 0.8646 0.7210 0.2050 0.052 Uiso 1 1 calc R . . C20 C 0.8245(3) 0.6563(3) 0.1387(3) 0.0339(15) Uani 1 1 d . . . H20 H 0.8664 0.6337 0.1319 0.041 Uiso 1 1 calc R . . C21 C 0.7658(3) 0.6593(3) -0.0855(3) 0.0303(13) Uani 1 1 d . . . H21 H 0.7181 0.6514 -0.0803 0.036 Uiso 1 1 calc R . . C22 C 0.7868(3) 0.7050(3) -0.1316(3) 0.0293(14) Uani 1 1 d . . . H22 H 0.7538 0.7272 -0.1569 0.035 Uiso 1 1 calc R . . C23 C 0.8576(3) 0.7175(3) -0.1396(3) 0.0312(14) Uani 1 1 d . . . H23 H 0.8731 0.7477 -0.1708 0.037 Uiso 1 1 calc R . . C24 C 0.9044(3) 0.6840(3) -0.1006(3) 0.0332(15) Uani 1 1 d . . . H24 H 0.9522 0.6923 -0.1043 0.040 Uiso 1 1 calc R . . C25 C 0.8802(3) 0.6384(3) -0.0560(3) 0.0312(14) Uani 1 1 d . . . H25 H 0.9126 0.6154 -0.0307 0.037 Uiso 1 1 calc R . . C26 C 1.2171(3) 0.4389(3) -0.0117(3) 0.0351(15) Uani 1 1 d . . . H26 H 1.1698 0.4445 -0.0025 0.042 Uiso 1 1 calc R . . C27 C 1.2358(4) 0.4126(3) -0.0709(3) 0.0446(17) Uani 1 1 d . . . H27 H 1.2016 0.4006 -0.1009 0.053 Uiso 1 1 calc R . . C28 C 1.3048(4) 0.4044(4) -0.0850(4) 0.053(2) Uani 1 1 d . . . H28 H 1.3184 0.3865 -0.1247 0.063 Uiso 1 1 calc R . . C29 C 1.3543(3) 0.4229(3) -0.0401(4) 0.0489(18) Uani 1 1 d . . . H29 H 1.4018 0.4180 -0.0491 0.059 Uiso 1 1 calc R . . C30 C 1.3324(3) 0.4489(3) 0.0190(3) 0.0376(16) Uani 1 1 d . . . H30 H 1.3660 0.4611 0.0496 0.045 Uiso 1 1 calc R . . C31 C 1.2924(3) 0.3363(3) 0.1442(3) 0.0334(15) Uani 1 1 d . . . H31 H 1.3323 0.3608 0.1544 0.040 Uiso 1 1 calc R . . C32 C 1.2998(3) 0.2688(3) 0.1294(3) 0.0410(17) Uani 1 1 d . . . H32 H 1.3437 0.2485 0.1292 0.049 Uiso 1 1 calc R . . C33 C 1.2402(4) 0.2330(3) 0.1150(3) 0.0493(19) Uani 1 1 d . . . H33 H 1.2435 0.1879 0.1043 0.059 Uiso 1 1 calc R . . C34 C 1.1755(3) 0.2639(3) 0.1165(4) 0.0456(18) Uani 1 1 d . . . H34 H 1.1347 0.2401 0.1077 0.055 Uiso 1 1 calc R . . C35 C 1.1734(3) 0.3312(3) 0.1314(3) 0.0356(16) Uani 1 1 d . . . H35 H 1.1300 0.3523 0.1324 0.043 Uiso 1 1 calc R . . C36 C 1.2147(3) 0.4522(3) 0.3137(3) 0.0375(16) Uani 1 1 d . . . H36 H 1.2584 0.4728 0.3152 0.045 Uiso 1 1 calc R . . C37 C 1.1910(3) 0.4187(3) 0.3685(3) 0.0443(17) Uani 1 1 d . . . H37 H 1.2173 0.4185 0.4065 0.053 Uiso 1 1 calc R . . C38 C 1.1286(3) 0.3860(3) 0.3654(3) 0.0422(17) Uani 1 1 d . . . H38 H 1.1124 0.3615 0.4007 0.051 Uiso 1 1 calc R . . C39 C 1.0896(3) 0.3897(3) 0.3091(3) 0.0396(16) Uani 1 1 d . . . H39 H 1.0466 0.3681 0.3063 0.048 Uiso 1 1 calc R . . C40 C 1.1147(3) 0.4251(3) 0.2579(3) 0.0368(15) Uani 1 1 d . . . H40 H 1.0874 0.4278 0.2206 0.044 Uiso 1 1 calc R . . C41 C 1.1574(3) 0.6348(3) 0.2329(3) 0.0302(14) Uani 1 1 d . . . H41 H 1.1171 0.6147 0.2168 0.036 Uiso 1 1 calc R . . C42 C 1.1504(3) 0.6940(3) 0.2673(3) 0.0335(14) Uani 1 1 d . . . H42 H 1.1065 0.7126 0.2746 0.040 Uiso 1 1 calc R . . C43 C 1.2108(3) 0.7247(3) 0.2905(3) 0.0309(14) Uani 1 1 d . . . H43 H 1.2080 0.7648 0.3132 0.037 Uiso 1 1 calc R . . C44 C 1.2756(3) 0.6945(3) 0.2794(3) 0.0303(13) Uani 1 1 d . . . H44 H 1.3168 0.7138 0.2947 0.036 Uiso 1 1 calc R . . C45 C 1.2768(3) 0.6351(3) 0.2451(3) 0.0281(13) Uani 1 1 d . . . H45 H 1.3199 0.6147 0.2379 0.034 Uiso 1 1 calc R . . C46 C 1.2042(3) 0.6337(3) 0.0440(3) 0.0292(14) Uani 1 1 d . . . H46 H 1.1578 0.6216 0.0514 0.035 Uiso 1 1 calc R . . C47 C 1.2175(3) 0.6846(3) 0.0005(3) 0.0280(14) Uani 1 1 d . . . H47 H 1.1811 0.7058 -0.0214 0.034 Uiso 1 1 calc R . . C48 C 1.2871(3) 0.7033(3) -0.0098(3) 0.0273(14) Uani 1 1 d . . . H48 H 1.2979 0.7379 -0.0383 0.033 Uiso 1 1 calc R . . C49 C 1.3392(3) 0.6702(3) 0.0225(3) 0.0295(14) Uani 1 1 d . . . H49 H 1.3859 0.6815 0.0158 0.035 Uiso 1 1 calc R . . C50 C 1.3216(3) 0.6195(3) 0.0655(3) 0.0271(13) Uani 1 1 d . . . H50 H 1.3572 0.5976 0.0878 0.032 Uiso 1 1 calc R . . C51 C 0.9414(3) 0.4900(3) 0.2636(3) 0.0360(15) Uani 1 1 d . . . H51 H 0.9317 0.4488 0.2448 0.043 Uiso 1 1 calc R . . C52 C 0.9408(3) 0.4935(3) 0.3301(3) 0.0348(14) Uani 1 1 d . . . H52 H 0.9303 0.4563 0.3554 0.042 Uiso 1 1 calc R . . C53 C 0.9564(3) 0.5541(3) 0.3578(3) 0.0391(15) Uani 1 1 d . . . H53 H 0.9575 0.5582 0.4028 0.047 Uiso 1 1 calc R . . C54 C 0.9703(3) 0.6085(3) 0.3194(4) 0.0420(17) Uani 1 1 d . . . H54 H 0.9801 0.6502 0.3372 0.050 Uiso 1 1 calc R . . C55 C 0.9692(3) 0.5985(3) 0.2528(3) 0.0408(17) Uani 1 1 d . . . H55 H 0.9793 0.6349 0.2263 0.049 Uiso 1 1 calc R . . C56 C 1.0422(3) 0.4530(3) -0.0895(3) 0.0390(16) Uani 1 1 d . . . H56 H 1.0276 0.4116 -0.0739 0.047 Uiso 1 1 calc R . . C57 C 1.0652(3) 0.4567(3) -0.1529(3) 0.0418(16) Uani 1 1 d . . . H57 H 1.0656 0.4187 -0.1789 0.050 Uiso 1 1 calc R . . C58 C 1.0871(3) 0.5160(3) -0.1767(3) 0.0453(17) Uani 1 1 d . . . H58 H 1.1026 0.5197 -0.2194 0.054 Uiso 1 1 calc R . . C59 C 1.0858(3) 0.5712(3) -0.1360(3) 0.0414(16) Uani 1 1 d . . . H59 H 1.1011 0.6126 -0.1507 0.050 Uiso 1 1 calc R . . C60 C 1.0617(3) 0.5638(3) -0.0737(3) 0.0379(15) Uani 1 1 d . . . H60 H 1.0606 0.6014 -0.0472 0.046 Uiso 1 1 calc R . . C61 C 0.9614(4) 0.2989(4) 0.0511(4) 0.059(2) Uani 1 1 d . . . C62 C 1.0581(3) 0.7641(3) 0.1174(3) 0.0345(15) Uani 1 1 d . . . C63 C 0.4857(4) 0.8111(4) 0.2954(4) 0.0511(19) Uani 1 1 d . . . N13 N 0.4965(2) 0.5056(3) 0.0548(3) 0.0492(15) Uani 1 1 d . . . C64 C 0.5159(3) 0.5625(3) 0.0268(4) 0.0392(15) Uani 1 1 d . . . H64 H 0.5265 0.5615 -0.0173 0.047 Uiso 1 1 calc R . . C65 C 0.5213(3) 0.6231(3) 0.0585(3) 0.0394(17) Uani 1 1 d . . . H65 H 0.5351 0.6613 0.0362 0.047 Uiso 1 1 calc R . . C66 C 0.5059(3) 0.6261(3) 0.1239(3) 0.0406(17) Uani 1 1 d . . . H66 H 0.5093 0.6661 0.1466 0.049 Uiso 1 1 calc R . . C67 C 0.4857(3) 0.5687(4) 0.1543(4) 0.0481(18) Uani 1 1 d . . . H67 H 0.4746 0.5690 0.1983 0.058 Uiso 1 1 calc R . . C68 C 0.4818(3) 0.5101(4) 0.1189(4) 0.054(2) Uani 1 1 d . . . H68 H 0.4684 0.4714 0.1405 0.065 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 0.02317(10) 0.02906(11) 0.02832(12) 0.00277(10) -0.00004(11) 0.00083(10) U2 0.02275(10) 0.02509(10) 0.02347(11) 0.00127(10) 0.00022(9) 0.00008(11) K 0.0229(5) 0.0275(7) 0.0286(7) 0.0020(5) -0.0015(5) 0.0014(5) S1 0.0289(7) 0.0253(7) 0.0388(10) 0.0045(7) 0.0006(7) -0.0008(6) S2 0.0253(7) 0.0267(7) 0.0334(9) 0.0006(7) -0.0022(7) 0.0007(6) S3 0.0361(9) 0.0377(9) 0.0510(12) -0.0020(8) -0.0059(8) 0.0062(7) O1 0.0277(18) 0.036(2) 0.031(2) 0.0008(19) -0.0071(16) 0.0023(17) O2 0.0238(19) 0.045(2) 0.035(3) 0.007(2) -0.0083(17) 0.0044(18) O3 0.0214(17) 0.030(2) 0.031(2) 0.0011(19) -0.0098(15) -0.0014(17) O4 0.0209(17) 0.031(2) 0.029(2) -0.0012(19) -0.0092(16) 0.0063(17) O5 0.044(2) 0.026(2) 0.070(4) 0.009(2) -0.006(2) -0.0032(19) O6 0.043(2) 0.036(2) 0.052(3) 0.015(2) 0.002(2) 0.004(2) O7 0.032(2) 0.051(3) 0.051(3) 0.015(3) 0.007(2) 0.003(2) O8 0.042(2) 0.022(2) 0.056(3) 0.008(2) -0.005(2) 0.0036(19) O9 0.038(2) 0.039(2) 0.030(3) -0.003(2) 0.0009(19) -0.0028(19) O10 0.029(2) 0.047(3) 0.044(3) 0.002(2) -0.004(2) 0.014(2) O11 0.083(3) 0.062(3) 0.032(3) 0.017(3) -0.011(3) 0.010(3) O12 0.030(2) 0.066(3) 0.065(4) -0.014(3) 0.008(2) 0.001(2) O13 0.034(2) 0.043(3) 0.049(3) 0.005(2) -0.005(2) -0.003(2) N1 0.032(3) 0.023(2) 0.033(3) -0.001(2) 0.002(2) -0.003(2) N2 0.036(3) 0.037(3) 0.027(3) -0.002(2) -0.009(2) -0.001(2) N3 0.031(2) 0.032(2) 0.027(2) 0.002(2) 0.004(2) -0.001(2) N4 0.034(2) 0.030(2) 0.030(3) 0.009(2) 0.004(3) 0.002(3) N5 0.034(3) 0.029(3) 0.027(3) -0.003(2) 0.001(2) 0.000(2) N6 0.036(3) 0.030(2) 0.023(3) -0.007(2) 0.011(3) 0.003(2) N7 0.032(2) 0.029(2) 0.036(3) 0.005(2) 0.003(3) 0.008(2) N8 0.027(2) 0.025(3) 0.023(3) 0.003(2) 0.006(2) -0.003(2) N9 0.023(2) 0.027(2) 0.027(3) -0.003(2) 0.003(2) 0.000(2) N10 0.030(3) 0.023(2) 0.026(3) -0.001(2) 0.0018(19) -0.0008(19) N11 0.031(3) 0.036(3) 0.039(3) 0.002(3) -0.002(2) 0.003(2) N12 0.033(2) 0.044(3) 0.033(3) -0.007(3) -0.001(2) 0.002(3) F1 0.108(4) 0.083(4) 0.127(5) -0.059(4) -0.036(4) -0.008(3) F2 0.055(3) 0.125(4) 0.046(3) 0.008(3) -0.006(2) 0.034(3) F3 0.064(3) 0.145(5) 0.050(3) -0.026(3) 0.002(2) 0.053(3) F4 0.076(3) 0.0267(19) 0.040(2) 0.0009(17) -0.005(2) -0.0046(18) F5 0.0271(18) 0.053(2) 0.045(2) -0.0029(18) -0.0036(16) -0.0038(16) F6 0.046(2) 0.050(2) 0.027(2) 0.0025(17) 0.0040(17) 0.0104(17) F7 0.080(3) 0.050(3) 0.109(4) -0.018(3) -0.045(3) -0.004(2) F8 0.088(3) 0.056(3) 0.066(3) 0.024(3) -0.006(3) -0.010(2) F9 0.065(3) 0.053(3) 0.076(3) -0.004(2) 0.016(2) 0.025(2) C1 0.031(3) 0.035(4) 0.047(4) 0.000(3) 0.002(3) 0.003(3) C2 0.045(4) 0.040(4) 0.039(4) -0.008(3) 0.010(3) -0.003(3) C3 0.061(4) 0.037(4) 0.037(4) -0.008(3) 0.011(4) -0.004(3) C4 0.044(4) 0.037(3) 0.039(4) 0.000(3) -0.011(3) -0.004(3) C5 0.043(3) 0.037(3) 0.042(4) 0.001(3) -0.002(3) -0.001(4) C6 0.050(4) 0.027(3) 0.034(4) -0.003(3) 0.001(3) 0.002(3) C7 0.061(4) 0.037(4) 0.035(4) 0.000(3) -0.012(4) -0.001(4) C8 0.073(5) 0.038(4) 0.039(5) 0.005(3) -0.010(4) -0.018(4) C9 0.039(4) 0.056(4) 0.045(4) 0.000(4) -0.009(3) -0.012(3) C10 0.027(3) 0.034(3) 0.045(4) -0.001(3) -0.006(3) -0.005(3) C11 0.033(3) 0.029(3) 0.037(4) 0.000(3) -0.001(3) -0.001(3) C12 0.044(4) 0.032(3) 0.035(4) 0.008(3) -0.005(3) -0.001(3) C13 0.040(4) 0.043(4) 0.037(4) 0.008(3) -0.001(3) -0.005(3) C14 0.032(3) 0.037(3) 0.043(4) 0.005(3) -0.001(3) -0.011(3) C15 0.027(3) 0.036(3) 0.035(4) 0.002(3) -0.003(2) -0.005(3) C16 0.031(3) 0.037(4) 0.044(4) 0.011(3) 0.006(3) 0.003(3) C17 0.044(4) 0.035(4) 0.042(5) 0.012(3) 0.015(3) 0.010(3) C18 0.064(5) 0.034(3) 0.032(4) -0.001(3) 0.009(4) 0.007(4) C19 0.053(4) 0.042(4) 0.036(4) 0.000(3) -0.002(3) 0.003(3) C20 0.034(3) 0.037(3) 0.032(4) 0.004(3) 0.003(3) 0.006(3) C21 0.029(3) 0.035(3) 0.027(3) 0.000(3) -0.004(3) 0.004(3) C22 0.035(3) 0.030(3) 0.023(4) 0.005(3) 0.002(2) 0.008(3) C23 0.043(3) 0.028(3) 0.023(4) 0.000(3) 0.004(3) 0.000(3) C24 0.028(3) 0.040(4) 0.032(4) -0.004(3) 0.001(3) -0.002(3) C25 0.026(3) 0.041(4) 0.027(4) 0.000(3) 0.004(3) -0.003(3) C26 0.036(3) 0.037(3) 0.032(4) -0.004(3) -0.008(3) -0.002(3) C27 0.045(4) 0.058(4) 0.030(4) -0.012(3) -0.009(4) 0.004(4) C28 0.077(5) 0.049(4) 0.033(4) -0.013(4) 0.011(4) -0.012(4) C29 0.042(4) 0.050(4) 0.054(5) -0.007(4) 0.021(4) 0.004(3) C30 0.029(3) 0.047(4) 0.037(4) -0.004(3) 0.005(3) 0.003(3) C31 0.033(3) 0.032(3) 0.035(4) 0.003(3) -0.003(3) 0.002(3) C32 0.040(4) 0.036(4) 0.047(5) -0.001(3) -0.006(3) 0.009(3) C33 0.067(5) 0.032(3) 0.048(5) 0.004(3) -0.009(4) 0.007(4) C34 0.041(4) 0.040(4) 0.055(5) 0.000(3) -0.012(3) 0.000(3) C35 0.031(3) 0.030(3) 0.046(5) -0.001(3) -0.004(3) 0.002(3) C36 0.037(3) 0.032(3) 0.043(4) 0.001(3) -0.007(3) -0.013(3) C37 0.048(4) 0.046(4) 0.039(4) 0.018(3) -0.013(3) -0.011(3) C38 0.049(4) 0.047(4) 0.031(4) 0.019(3) 0.003(3) -0.004(3) C39 0.033(3) 0.049(4) 0.037(4) 0.012(3) -0.001(3) -0.010(3) C40 0.030(3) 0.047(4) 0.033(4) 0.006(3) -0.002(3) 0.001(3) C41 0.029(3) 0.033(3) 0.029(4) 0.000(3) -0.002(3) -0.001(3) C42 0.037(3) 0.038(4) 0.025(4) -0.002(3) 0.001(3) 0.006(3) C43 0.049(4) 0.026(3) 0.017(3) 0.001(2) 0.008(3) 0.004(3) C44 0.035(3) 0.035(3) 0.021(3) -0.002(2) 0.000(3) -0.004(3) C45 0.026(3) 0.033(3) 0.024(3) 0.004(2) 0.001(3) -0.003(3) C46 0.028(3) 0.027(3) 0.032(4) 0.000(3) 0.006(3) 0.000(2) C47 0.024(3) 0.026(3) 0.035(4) 0.001(3) 0.000(3) 0.001(2) C48 0.036(3) 0.020(3) 0.026(3) 0.000(2) 0.005(2) 0.001(2) C49 0.030(3) 0.030(3) 0.029(4) -0.004(3) 0.009(3) -0.006(3) C50 0.023(3) 0.026(3) 0.032(4) 0.001(3) -0.005(3) 0.006(2) C51 0.029(3) 0.040(4) 0.040(4) 0.000(3) -0.001(3) -0.002(3) C52 0.032(3) 0.034(3) 0.038(4) 0.004(3) 0.005(3) 0.002(3) C53 0.037(3) 0.052(4) 0.028(4) -0.001(3) 0.000(3) -0.002(3) C54 0.037(3) 0.036(4) 0.053(5) -0.010(3) 0.006(3) -0.004(3) C55 0.030(3) 0.045(4) 0.047(5) 0.014(3) 0.004(3) 0.007(3) C56 0.027(3) 0.040(4) 0.050(5) -0.001(3) 0.001(3) -0.004(3) C57 0.041(3) 0.050(4) 0.034(4) -0.016(3) 0.000(3) -0.004(3) C58 0.046(4) 0.058(5) 0.032(4) -0.003(3) 0.005(3) -0.006(3) C59 0.044(4) 0.043(4) 0.037(4) 0.004(3) -0.002(3) -0.009(3) C60 0.034(3) 0.040(4) 0.040(4) -0.008(3) -0.006(3) 0.003(3) C61 0.052(5) 0.070(5) 0.055(6) -0.019(4) -0.002(4) 0.015(4) C62 0.044(4) 0.032(4) 0.027(4) 0.001(3) -0.002(3) 0.012(3) C63 0.049(4) 0.051(4) 0.053(5) 0.007(4) -0.009(4) -0.001(4) N13 0.029(3) 0.046(3) 0.073(5) 0.003(3) -0.011(3) 0.000(3) C64 0.028(3) 0.047(4) 0.042(4) 0.005(4) -0.001(3) 0.004(3) C65 0.028(3) 0.040(4) 0.051(5) 0.008(3) -0.004(3) 0.003(3) C66 0.026(3) 0.049(4) 0.047(5) 0.000(3) -0.002(3) 0.010(3) C67 0.029(3) 0.062(5) 0.053(5) 0.006(4) 0.002(3) 0.008(3) C68 0.026(3) 0.060(5) 0.077(6) 0.031(5) -0.006(3) -0.004(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 U1 O2 1.826(3) . ? U1 O1 1.839(3) . ? U1 N5 2.600(5) . ? U1 N1 2.606(5) . ? U1 N4 2.620(5) . ? U1 N3 2.618(4) . ? U1 N2 2.650(5) . ? U2 O4 1.825(3) . ? U2 O3 1.831(3) . ? U2 N10 2.590(5) . ? U2 N8 2.594(4) . ? U2 N9 2.609(4) . ? U2 N6 2.619(4) . ? U2 N7 2.623(4) . ? K O5 2.669(4) . ? K O8 2.703(4) . ? K O3 2.756(3) . ? K O1 2.759(3) . ? K N12 2.953(5) . ? K N11 2.953(5) . ? S1 O7 1.437(4) . ? S1 O6 1.429(4) . ? S1 O5 1.437(4) . ? S1 C61 1.832(8) . ? S2 O10 1.437(4) . ? S2 O9 1.439(4) . ? S2 O8 1.453(4) . ? S2 C62 1.818(6) . ? S3 O12 1.424(4) . ? S3 O13 1.447(4) . ? S3 O11 1.455(5) . ? S3 C63 1.793(7) . ? N1 C5 1.342(7) . ? N1 C1 1.361(7) . ? N2 C6 1.324(7) . ? N2 C10 1.344(7) . ? N3 C15 1.336(7) . ? N3 C11 1.356(7) . ? N4 C20 1.340(7) . ? N4 C16 1.345(7) . ? N5 C21 1.347(7) . ? N5 C25 1.357(7) . ? N6 C30 1.340(7) . ? N6 C26 1.345(7) . ? N7 C35 1.333(7) . ? N7 C31 1.341(7) . ? N8 C40 1.342(7) . ? N8 C36 1.348(7) . ? N9 C41 1.336(7) . ? N9 C45 1.347(7) . ? N10 C46 1.336(7) . ? N10 C50 1.354(7) . ? N11 C51 1.321(8) . ? N11 C55 1.332(8) . ? N12 C56 1.344(8) . ? N12 C60 1.344(8) . ? F1 C61 1.322(9) . ? F2 C61 1.328(9) . ? F3 C61 1.338(8) . ? F4 C62 1.346(7) . ? F5 C62 1.333(7) . ? F6 C62 1.340(7) . ? F7 C63 1.348(8) . ? F8 C63 1.333(8) . ? F9 C63 1.324(8) . ? C1 C2 1.374(9) . ? C1 H1 0.9300 . ? C2 C3 1.339(9) . ? C2 H2 0.9300 . ? C3 C4 1.383(8) . ? C3 H3 0.9300 . ? C4 C5 1.386(9) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.369(8) . ? C6 H6 0.9300 . ? C7 C8 1.370(10) . ? C7 H7 0.9300 . ? C8 C9 1.383(10) . ? C8 H8 0.9300 . ? C9 C10 1.370(9) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.388(8) . ? C11 H11 0.9300 . ? C12 C13 1.382(8) . ? C12 H12 0.9300 . ? C13 C14 1.372(8) . ? C13 H13 0.9300 . ? C14 C15 1.394(8) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.396(9) . ? C16 H16 0.9300 . ? C17 C18 1.380(9) . ? C17 H17 0.9300 . ? C18 C19 1.369(9) . ? C18 H18 0.9300 . ? C19 C20 1.391(9) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.377(8) . ? C21 H21 0.9300 . ? C22 C23 1.384(8) . ? C22 H22 0.9300 . ? C23 C24 1.377(8) . ? C23 H23 0.9300 . ? C24 C25 1.374(8) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.374(8) . ? C26 H26 0.9300 . ? C27 C28 1.359(9) . ? C27 H27 0.9300 . ? C28 C29 1.372(10) . ? C28 H28 0.9300 . ? C29 C30 1.388(9) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.393(9) . ? C31 H31 0.9300 . ? C32 C33 1.376(9) . ? C32 H32 0.9300 . ? C33 C34 1.382(9) . ? C33 H33 0.9300 . ? C34 C35 1.382(9) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C37 1.389(8) . ? C36 H36 0.9300 . ? C37 C38 1.360(9) . ? C37 H37 0.9300 . ? C38 C39 1.377(9) . ? C38 H38 0.9300 . ? C39 C40 1.357(8) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 C42 1.386(8) . ? C41 H41 0.9300 . ? C42 C43 1.390(8) . ? C42 H42 0.9300 . ? C43 C44 1.395(8) . ? C43 H43 0.9300 . ? C44 C45 1.383(8) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 C47 1.379(8) . ? C46 H46 0.9300 . ? C47 C48 1.397(8) . ? C47 H47 0.9300 . ? C48 C49 1.367(8) . ? C48 H48 0.9300 . ? C49 C50 1.387(8) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? C51 C52 1.371(8) . ? C51 H51 0.9300 . ? C52 C53 1.373(9) . ? C52 H52 0.9300 . ? C53 C54 1.372(9) . ? C53 H53 0.9300 . ? C54 C55 1.385(9) . ? C54 H54 0.9300 . ? C55 H55 0.9300 . ? C56 C57 1.380(9) . ? C56 H56 0.9300 . ? C57 C58 1.351(9) . ? C57 H57 0.9300 . ? C58 C59 1.387(9) . ? C58 H58 0.9300 . ? C59 C60 1.370(9) . ? C59 H59 0.9300 . ? C60 H60 0.9300 . ? N13 C64 1.330(8) . ? N13 C68 1.352(9) . ? C64 C65 1.381(9) . ? C64 H64 0.9300 . ? C65 C66 1.378(9) . ? C65 H65 0.9300 . ? C66 C67 1.364(10) . ? C66 H66 0.9300 . ? C67 C68 1.384(10) . ? C67 H67 0.9300 . ? C68 H68 0.9300 . ? 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 O1 177.67(17) . . ? O2 U1 N5 86.87(16) . . ? O1 U1 N5 90.84(15) . . ? O2 U1 N1 89.75(16) . . ? O1 U1 N1 89.20(15) . . ? N5 U1 N1 72.94(14) . . ? O2 U1 N4 88.43(17) . . ? O1 U1 N4 91.45(16) . . ? N5 U1 N4 77.17(14) . . ? N1 U1 N4 150.11(14) . . ? O2 U1 N3 93.60(16) . . ? O1 U1 N3 88.57(15) . . ? N5 U1 N3 149.09(14) . . ? N1 U1 N3 137.94(14) . . ? N4 U1 N3 71.95(13) . . ? O2 U1 N2 84.72(16) . . ? O1 U1 N2 96.90(15) . . ? N5 U1 N2 142.86(15) . . ? N1 U1 N2 70.92(15) . . ? N4 U1 N2 138.46(15) . . ? N3 U1 N2 67.69(14) . . ? O4 U2 O3 179.37(17) . . ? O4 U2 N10 92.20(15) . . ? O3 U2 N10 87.40(15) . . ? O4 U2 N8 93.45(15) . . ? O3 U2 N8 86.62(15) . . ? N10 U2 N8 146.64(13) . . ? O4 U2 N9 85.36(15) . . ? O3 U2 N9 94.05(15) . . ? N10 U2 N9 72.53(14) . . ? N8 U2 N9 75.20(13) . . ? O4 U2 N6 91.13(15) . . ? O3 U2 N6 89.19(16) . . ? N10 U2 N6 70.72(14) . . ? N8 U2 N6 141.89(14) . . ? N9 U2 N6 142.90(13) . . ? O4 U2 N7 86.79(16) . . ? O3 U2 N7 93.83(16) . . ? N10 U2 N7 139.96(14) . . ? N8 U2 N7 73.23(14) . . ? N9 U2 N7 146.89(14) . . ? N6 U2 N7 69.29(14) . . ? O5 K O8 157.46(15) . . ? O5 K O3 78.86(12) . . ? O8 K O3 87.07(12) . . ? O5 K O1 97.86(13) . . ? O8 K O1 97.01(12) . . ? O3 K O1 175.42(12) . . ? O5 K N12 104.99(15) . . ? O8 K N12 91.80(15) . . ? O3 K N12 87.67(12) . . ? O1 K N12 90.12(12) . . ? O5 K N11 83.21(15) . . ? O8 K N11 79.97(14) . . ? O3 K N11 92.84(12) . . ? O1 K N11 89.93(12) . . ? N12 K N11 171.71(15) . . ? O7 S1 O6 116.1(3) . . ? O7 S1 O5 114.2(3) . . ? O6 S1 O5 114.5(3) . . ? O7 S1 C61 103.3(3) . . ? O6 S1 C61 104.0(3) . . ? O5 S1 C61 102.4(3) . . ? O10 S2 O9 115.5(3) . . ? O10 S2 O8 115.1(3) . . ? O9 S2 O8 114.5(3) . . ? O10 S2 C62 102.8(3) . . ? O9 S2 C62 103.8(3) . . ? O8 S2 C62 102.8(3) . . ? O12 S3 O13 115.7(3) . . ? O12 S3 O11 114.4(3) . . ? O13 S3 O11 113.9(3) . . ? O12 S3 C63 104.3(3) . . ? O13 S3 C63 104.1(3) . . ? O11 S3 C63 102.4(3) . . ? U1 O1 K 166.3(2) . . ? U2 O3 K 175.44(19) . . ? S1 O5 K 141.1(3) . . ? S2 O8 K 152.6(3) . . ? C5 N1 C1 117.2(5) . . ? C5 N1 U1 121.5(4) . . ? C1 N1 U1 120.6(4) . . ? C6 N2 C10 117.7(5) . . ? C6 N2 U1 122.8(4) . . ? C10 N2 U1 119.0(4) . . ? C15 N3 C11 118.3(5) . . ? C15 N3 U1 121.0(4) . . ? C11 N3 U1 119.1(3) . . ? C20 N4 C16 117.7(5) . . ? C20 N4 U1 123.1(4) . . ? C16 N4 U1 119.0(4) . . ? C21 N5 C25 116.9(5) . . ? C21 N5 U1 120.8(4) . . ? C25 N5 U1 122.0(4) . . ? C30 N6 C26 117.8(5) . . ? C30 N6 U2 119.9(4) . . ? C26 N6 U2 122.2(4) . . ? C35 N7 C31 117.7(5) . . ? C35 N7 U2 122.5(4) . . ? C31 N7 U2 118.8(4) . . ? C40 N8 C36 116.9(5) . . ? C40 N8 U2 118.3(4) . . ? C36 N8 U2 123.6(3) . . ? C41 N9 C45 117.3(5) . . ? C41 N9 U2 121.3(4) . . ? C45 N9 U2 121.2(3) . . ? C46 N10 C50 117.6(5) . . ? C46 N10 U2 122.4(3) . . ? C50 N10 U2 119.9(3) . . ? C51 N11 C55 115.8(6) . . ? C51 N11 K 119.1(4) . . ? C55 N11 K 121.8(4) . . ? C56 N12 C60 115.3(5) . . ? C56 N12 K 130.2(4) . . ? C60 N12 K 114.4(4) . . ? N1 C1 C2 121.6(6) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C3 C2 C1 120.9(6) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C2 C3 C4 118.9(6) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C3 C4 C5 118.7(6) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 122.6(6) . . ? N1 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? N2 C6 C7 123.8(6) . . ? N2 C6 H6 118.1 . . ? C7 C6 H6 118.1 . . ? C6 C7 C8 118.3(6) . . ? C6 C7 H7 120.8 . . ? C8 C7 H7 120.8 . . ? C7 C8 C9 119.0(6) . . ? C7 C8 H8 120.5 . . ? C9 C8 H8 120.5 . . ? C10 C9 C8 118.9(6) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? N2 C10 C9 122.3(6) . . ? N2 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? N3 C11 C12 122.0(5) . . ? N3 C11 H11 119.0 . . ? C12 C11 H11 119.0 . . ? C13 C12 C11 119.1(6) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C14 C13 C12 119.0(6) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? C13 C14 C15 119.2(5) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? N3 C15 C14 122.3(5) . . ? N3 C15 H15 118.8 . . ? C14 C15 H15 118.8 . . ? N4 C16 C17 121.6(6) . . ? N4 C16 H16 119.2 . . ? C17 C16 H16 119.2 . . ? C18 C17 C16 119.6(6) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C19 C18 C17 119.0(6) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C18 C19 C20 118.4(6) . . ? C18 C19 H19 120.8 . . ? C20 C19 H19 120.8 . . ? N4 C20 C19 123.6(6) . . ? N4 C20 H20 118.2 . . ? C19 C20 H20 118.2 . . ? N5 C21 C22 123.2(6) . . ? N5 C21 H21 118.4 . . ? C22 C21 H21 118.4 . . ? C21 C22 C23 119.0(5) . . ? C21 C22 H22 120.5 . . ? C23 C22 H22 120.5 . . ? C24 C23 C22 118.4(5) . . ? C24 C23 H23 120.8 . . ? C22 C23 H23 120.8 . . ? C25 C24 C23 119.7(5) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? N5 C25 C24 122.6(5) . . ? N5 C25 H25 118.7 . . ? C24 C25 H25 118.7 . . ? N6 C26 C27 122.7(6) . . ? N6 C26 H26 118.6 . . ? C27 C26 H26 118.6 . . ? C28 C27 C26 119.2(6) . . ? C28 C27 H27 120.4 . . ? C26 C27 H27 120.4 . . ? C27 C28 C29 119.3(7) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C28 C29 C30 119.1(6) . . ? C28 C29 H29 120.5 . . ? C30 C29 H29 120.5 . . ? N6 C30 C29 121.9(6) . . ? N6 C30 H30 119.0 . . ? C29 C30 H30 119.0 . . ? N7 C31 C32 122.9(6) . . ? N7 C31 H31 118.5 . . ? C32 C31 H31 118.5 . . ? C33 C32 C31 117.9(6) . . ? C33 C32 H32 121.1 . . ? C31 C32 H32 121.1 . . ? C32 C33 C34 120.1(6) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C33 C34 C35 117.8(6) . . ? C33 C34 H34 121.1 . . ? C35 C34 H34 121.1 . . ? N7 C35 C34 123.6(6) . . ? N7 C35 H35 118.2 . . ? C34 C35 H35 118.2 . . ? N8 C36 C37 122.7(5) . . ? N8 C36 H36 118.7 . . ? C37 C36 H36 118.7 . . ? C38 C37 C36 118.6(6) . . ? C38 C37 H37 120.7 . . ? C36 C37 H37 120.7 . . ? C37 C38 C39 119.1(6) . . ? C37 C38 H38 120.4 . . ? C39 C38 H38 120.4 . . ? C40 C39 C38 119.4(6) . . ? C40 C39 H39 120.3 . . ? C38 C39 H39 120.3 . . ? N8 C40 C39 123.3(6) . . ? N8 C40 H40 118.4 . . ? C39 C40 H40 118.4 . . ? N9 C41 C42 123.6(5) . . ? N9 C41 H41 118.2 . . ? C42 C41 H41 118.2 . . ? C41 C42 C43 118.3(6) . . ? C41 C42 H42 120.9 . . ? C43 C42 H42 120.9 . . ? C42 C43 C44 119.1(5) . . ? C42 C43 H43 120.5 . . ? C44 C43 H43 120.4 . . ? C45 C44 C43 118.1(6) . . ? C45 C44 H44 121.0 . . ? C43 C44 H44 121.0 . . ? N9 C45 C44 123.6(6) . . ? N9 C45 H45 118.2 . . ? C44 C45 H45 118.2 . . ? N10 C46 C47 123.5(5) . . ? N10 C46 H46 118.2 . . ? C47 C46 H46 118.3 . . ? C46 C47 C48 118.2(5) . . ? C46 C47 H47 120.9 . . ? C48 C47 H47 120.9 . . ? C49 C48 C47 119.2(5) . . ? C49 C48 H48 120.4 . . ? C47 C48 H48 120.4 . . ? C48 C49 C50 119.2(5) . . ? C48 C49 H49 120.4 . . ? C50 C49 H49 120.4 . . ? N10 C50 C49 122.3(5) . . ? N10 C50 H50 118.8 . . ? C49 C50 H50 118.8 . . ? N11 C51 C52 125.2(6) . . ? N11 C51 H51 117.4 . . ? C52 C51 H51 117.4 . . ? C51 C52 C53 117.4(6) . . ? C51 C52 H52 121.3 . . ? C53 C52 H52 121.3 . . ? C54 C53 C52 120.1(6) . . ? C54 C53 H53 119.9 . . ? C52 C53 H53 119.9 . . ? C53 C54 C55 117.0(6) . . ? C53 C54 H54 121.5 . . ? C55 C54 H54 121.5 . . ? N11 C55 C54 124.5(6) . . ? N11 C55 H55 117.7 . . ? C54 C55 H55 117.7 . . ? N12 C56 C57 124.1(6) . . ? N12 C56 H56 117.9 . . ? C57 C56 H56 117.9 . . ? C58 C57 C56 119.3(6) . . ? C58 C57 H57 120.4 . . ? C56 C57 H57 120.4 . . ? C57 C58 C59 118.3(6) . . ? C57 C58 H58 120.8 . . ? C59 C58 H58 120.8 . . ? C60 C59 C58 119.1(6) . . ? C60 C59 H59 120.4 . . ? C58 C59 H59 120.5 . . ? N12 C60 C59 123.9(6) . . ? N12 C60 H60 118.1 . . ? C59 C60 H60 118.1 . . ? F1 C61 F2 107.8(6) . . ? F1 C61 F3 109.0(7) . . ? F2 C61 F3 107.7(7) . . ? F1 C61 S1 110.5(6) . . ? F2 C61 S1 111.4(5) . . ? F3 C61 S1 110.2(5) . . ? F5 C62 F6 108.3(5) . . ? F5 C62 F4 106.7(5) . . ? F6 C62 F4 106.9(5) . . ? F5 C62 S2 112.3(4) . . ? F6 C62 S2 111.3(4) . . ? F4 C62 S2 111.1(4) . . ? F9 C63 F8 106.5(6) . . ? F9 C63 F7 107.1(6) . . ? F8 C63 F7 107.4(6) . . ? F9 C63 S3 111.6(5) . . ? F8 C63 S3 112.0(5) . . ? F7 C63 S3 111.8(5) . . ? C64 N13 C68 115.1(7) . . ? N13 C64 C65 124.6(7) . . ? N13 C64 H64 117.7 . . ? C65 C64 H64 117.7 . . ? C66 C65 C64 119.0(7) . . ? C66 C65 H65 120.5 . . ? C64 C65 H65 120.5 . . ? C67 C66 C65 118.2(7) . . ? C67 C66 H66 120.9 . . ? C65 C66 H66 120.9 . . ? C66 C67 C68 119.1(7) . . ? C66 C67 H67 120.5 . . ? C68 C67 H67 120.5 . . ? N13 C68 C67 124.1(7) . . ? N13 C68 H68 118.0 . . ? C67 C68 H68 118.0 . . ? #===END data_6.py _database_code_depnum_ccdc_archive 'CCDC 711338' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H60 F6 N12 O10 S2 Tl U2, C F3 O3 S, C5 H5 N' _chemical_formula_sum 'C68 H65 F9 N13 O13 S3 Tl U2' _chemical_formula_weight 2219.94 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' Tl Tl -2.8358 9.6688 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 19.1433(5) _cell_length_b 19.9724(5) _cell_length_c 20.6551(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7897.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 175501 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent dark orange' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.867 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4248 _exptl_absorpt_coefficient_mu 6.294 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.248 _exptl_absorpt_correction_T_max 0.604 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 30 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 area-detector diffractometer' _diffrn_measurement_method 'two \f and three \w scans with 2\% steps (213 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 175501 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.68 _reflns_number_total 14973 _reflns_number_gt 13364 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _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 and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 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^)+(0.0346P)^2^+0.8059P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.007(4) _refine_ls_number_reflns 14973 _refine_ls_number_parameters 983 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0636 _refine_ls_wR_factor_gt 0.0611 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.228 _refine_diff_density_min -1.091 _refine_diff_density_rms 0.102 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 0.235138(12) 0.469497(10) 0.970297(11) 0.02783(6) Uani 1 1 d . . . U2 U -0.230608(11) 0.501594(10) 0.852518(10) 0.02454(5) Uani 1 1 d . . . Tl Tl 0.002485(12) 0.487066(11) 0.910986(11) 0.02960(6) Uani 1 1 d . . . S1 S 0.03610(8) 0.67630(7) 0.86351(8) 0.0328(4) Uani 1 1 d . . . S2 S -0.01071(8) 0.28335(7) 0.92911(8) 0.0318(3) Uani 1 1 d . . . S3 S 0.49741(10) 0.27740(8) 0.70789(10) 0.0454(4) Uani 1 1 d . . . O1 O 0.1455(2) 0.4917(2) 0.94695(19) 0.0319(9) Uani 1 1 d . . . O2 O 0.3231(2) 0.4454(2) 0.9958(2) 0.0341(10) Uani 1 1 d . . . O3 O -0.13941(19) 0.49626(19) 0.87910(18) 0.0298(9) Uani 1 1 d . . . O4 O -0.32164(19) 0.5065(2) 0.82609(19) 0.0294(9) Uani 1 1 d . . . O5 O -0.0079(2) 0.61702(19) 0.8605(2) 0.0412(11) Uani 1 1 d . . . O6 O 0.0057(2) 0.7354(2) 0.8351(2) 0.0465(12) Uani 1 1 d . . . O7 O 0.1083(2) 0.6643(2) 0.8494(3) 0.0441(12) Uani 1 1 d . . . O8 O -0.0120(3) 0.3444(2) 0.8919(3) 0.0599(16) Uani 1 1 d . . . O9 O -0.0461(2) 0.2870(2) 0.9901(2) 0.0393(11) Uani 1 1 d . . . O10 O 0.0555(2) 0.2489(3) 0.9297(2) 0.0479(13) Uani 1 1 d . . . O11 O 0.4962(3) 0.2953(3) 0.6387(3) 0.0655(15) Uani 1 1 d . . . O12 O 0.4316(3) 0.2833(3) 0.7378(3) 0.0582(15) Uani 1 1 d . . . O13 O 0.5555(2) 0.3052(2) 0.7431(2) 0.0414(11) Uani 1 1 d . . . N1 N 0.2118(3) 0.5230(2) 1.0831(3) 0.0343(12) Uani 1 1 d . . . N2 N 0.2824(3) 0.5932(2) 0.9703(3) 0.0328(12) Uani 1 1 d . . . N3 N 0.2747(3) 0.5088(2) 0.8548(2) 0.0322(11) Uani 1 1 d . . . N4 N 0.2319(3) 0.3647(2) 0.8942(2) 0.0314(11) Uani 1 1 d . . . N5 N 0.1876(2) 0.3751(2) 1.0459(2) 0.0277(11) Uani 1 1 d . . . N6 N -0.2650(3) 0.5438(2) 0.9675(2) 0.0300(10) Uani 1 1 d . . . N7 N -0.2324(3) 0.6329(2) 0.8558(3) 0.0334(11) Uani 1 1 d . . . N8 N -0.1811(2) 0.5425(2) 0.7432(2) 0.0292(11) Uani 1 1 d . . . N9 N -0.2212(2) 0.3944(2) 0.7810(2) 0.0284(11) Uani 1 1 d . . . N10 N -0.2551(2) 0.3988(2) 0.9254(2) 0.0267(11) Uani 1 1 d . . . N11 N 0.0449(3) 0.4604(3) 0.7741(3) 0.0405(14) Uani 1 1 d . . . N12 N -0.0420(3) 0.4939(3) 1.0539(3) 0.0401(13) Uani 1 1 d . . . F1 F 0.0753(3) 0.7476(2) 0.9634(3) 0.0895(18) Uani 1 1 d . . . F2 F 0.0609(2) 0.6436(2) 0.9841(2) 0.0585(12) Uani 1 1 d . . . F3 F -0.0289(2) 0.7063(3) 0.9709(2) 0.0735(15) Uani 1 1 d . . . F4 F -0.0695(3) 0.16708(18) 0.9077(2) 0.0684(15) Uani 1 1 d . . . F5 F -0.13081(18) 0.2507(2) 0.87613(19) 0.0450(10) Uani 1 1 d . . . F6 F -0.0403(2) 0.2207(2) 0.82136(19) 0.0593(12) Uani 1 1 d . . . F7 F 0.4685(3) 0.1569(2) 0.6683(3) 0.0831(17) Uani 1 1 d . . . F8 F 0.5155(3) 0.1622(2) 0.7633(3) 0.0707(14) Uani 1 1 d . . . F9 F 0.5779(2) 0.1770(2) 0.6788(2) 0.0628(13) Uani 1 1 d . . . C1 C 0.1495(3) 0.5503(3) 1.0974(3) 0.0375(15) Uani 1 1 d . . . H1 H 0.1123 0.5431 1.0692 0.045 Uiso 1 1 calc R . . C2 C 0.1384(4) 0.5882(3) 1.1517(4) 0.0431(17) Uani 1 1 d . . . H2 H 0.0952 0.6080 1.1591 0.052 Uiso 1 1 calc R . . C3 C 0.1922(4) 0.5967(3) 1.1952(4) 0.0457(18) Uani 1 1 d . . . H3 H 0.1855 0.6216 1.2327 0.055 Uiso 1 1 calc R . . C4 C 0.2556(4) 0.5681(3) 1.1824(3) 0.0412(17) Uani 1 1 d . . . H4 H 0.2927 0.5735 1.2110 0.049 Uiso 1 1 calc R . . C5 C 0.2636(3) 0.5314(3) 1.1273(3) 0.0355(14) Uani 1 1 d . . . H5 H 0.3066 0.5112 1.1196 0.043 Uiso 1 1 calc R . . C6 C 0.2404(4) 0.6455(3) 0.9576(3) 0.0397(16) Uani 1 1 d . . . H6 H 0.1926 0.6382 0.9538 0.048 Uiso 1 1 calc R . . C7 C 0.2660(4) 0.7099(3) 0.9498(3) 0.0460(17) Uani 1 1 d . . . H7 H 0.2358 0.7453 0.9418 0.055 Uiso 1 1 calc R . . C8 C 0.3378(4) 0.7208(4) 0.9542(4) 0.051(2) Uani 1 1 d . . . H8 H 0.3562 0.7635 0.9487 0.061 Uiso 1 1 calc R . . C9 C 0.3807(4) 0.6676(4) 0.9668(4) 0.0486(18) Uani 1 1 d . . . H9 H 0.4288 0.6736 0.9700 0.058 Uiso 1 1 calc R . . C10 C 0.3513(3) 0.6036(3) 0.9748(3) 0.0378(15) Uani 1 1 d . . . H10 H 0.3805 0.5675 0.9835 0.045 Uiso 1 1 calc R . . C11 C 0.2345(3) 0.5493(3) 0.8204(3) 0.0343(14) Uani 1 1 d . . . H11 H 0.1888 0.5566 0.8341 0.041 Uiso 1 1 calc R . . C12 C 0.2573(3) 0.5810(3) 0.7654(3) 0.0363(15) Uani 1 1 d . . . H12 H 0.2270 0.6078 0.7416 0.044 Uiso 1 1 calc R . . C13 C 0.3251(4) 0.5729(3) 0.7458(3) 0.0397(16) Uani 1 1 d . . . H13 H 0.3421 0.5952 0.7095 0.048 Uiso 1 1 calc R . . C14 C 0.3682(3) 0.5303(3) 0.7813(3) 0.0369(15) Uani 1 1 d . . . H14 H 0.4142 0.5229 0.7686 0.044 Uiso 1 1 calc R . . C15 C 0.3415(3) 0.4994(3) 0.8356(3) 0.0297(13) Uani 1 1 d . . . H15 H 0.3703 0.4714 0.8597 0.036 Uiso 1 1 calc R . . C16 C 0.2919(3) 0.3312(3) 0.8822(3) 0.0347(15) Uani 1 1 d . . . H16 H 0.3320 0.3434 0.9048 0.042 Uiso 1 1 calc R . . C17 C 0.2962(4) 0.2788(3) 0.8371(4) 0.0448(19) Uani 1 1 d . . . H17 H 0.3383 0.2574 0.8286 0.054 Uiso 1 1 calc R . . C18 C 0.2348(5) 0.2602(3) 0.8056(3) 0.0476(19) Uani 1 1 d . . . H18 H 0.2350 0.2245 0.7767 0.057 Uiso 1 1 calc R . . C19 C 0.1748(4) 0.2943(3) 0.8171(3) 0.0409(17) Uani 1 1 d . . . H19 H 0.1340 0.2831 0.7952 0.049 Uiso 1 1 calc R . . C20 C 0.1749(3) 0.3460(3) 0.8621(3) 0.0320(14) Uani 1 1 d . . . H20 H 0.1333 0.3685 0.8702 0.038 Uiso 1 1 calc R . . C21 C 0.2318(3) 0.3419(3) 1.0848(3) 0.0294(12) Uani 1 1 d . . . H21 H 0.2795 0.3502 1.0813 0.035 Uiso 1 1 calc R . . C22 C 0.2087(3) 0.2957(3) 1.1301(3) 0.0305(14) Uani 1 1 d . . . H22 H 0.2407 0.2730 1.1559 0.037 Uiso 1 1 calc R . . C23 C 0.1385(3) 0.2833(3) 1.1367(3) 0.0341(15) Uani 1 1 d . . . H23 H 0.1222 0.2535 1.1678 0.041 Uiso 1 1 calc R . . C24 C 0.0925(3) 0.3167(3) 1.0957(3) 0.0342(15) Uani 1 1 d . . . H24 H 0.0447 0.3086 1.0979 0.041 Uiso 1 1 calc R . . C25 C 0.1192(3) 0.3620(3) 1.0514(3) 0.0330(15) Uani 1 1 d . . . H25 H 0.0882 0.3844 1.0243 0.040 Uiso 1 1 calc R . . C26 C -0.2169(3) 0.5601(3) 1.0118(3) 0.0394(16) Uani 1 1 d . . . H26 H -0.1700 0.5543 1.0016 0.047 Uiso 1 1 calc R . . C27 C -0.2342(4) 0.5854(3) 1.0725(3) 0.0470(17) Uani 1 1 d . . . H27 H -0.1994 0.5964 1.1021 0.056 Uiso 1 1 calc R . . C28 C -0.3022(4) 0.5938(4) 1.0878(4) 0.055(2) Uani 1 1 d . . . H28 H -0.3146 0.6105 1.1282 0.067 Uiso 1 1 calc R . . C29 C -0.3537(4) 0.5775(4) 1.0428(4) 0.0501(19) Uani 1 1 d . . . H29 H -0.4008 0.5835 1.0522 0.060 Uiso 1 1 calc R . . C30 C -0.3325(3) 0.5522(3) 0.9839(3) 0.0355(15) Uani 1 1 d . . . H30 H -0.3666 0.5402 0.9540 0.043 Uiso 1 1 calc R . . C31 C -0.2935(3) 0.6648(3) 0.8571(3) 0.0369(15) Uani 1 1 d . . . H31 H -0.3339 0.6405 0.8485 0.044 Uiso 1 1 calc R . . C32 C -0.2999(4) 0.7332(3) 0.8708(4) 0.0411(17) Uani 1 1 d . . . H32 H -0.3433 0.7541 0.8708 0.049 Uiso 1 1 calc R . . C33 C -0.2400(4) 0.7687(3) 0.8842(3) 0.0473(19) Uani 1 1 d . . . H33 H -0.2423 0.8139 0.8948 0.057 Uiso 1 1 calc R . . C34 C -0.1756(4) 0.7358(3) 0.8816(4) 0.0448(18) Uani 1 1 d . . . H34 H -0.1342 0.7588 0.8890 0.054 Uiso 1 1 calc R . . C35 C -0.1751(3) 0.6688(3) 0.8679(3) 0.0360(16) Uani 1 1 d . . . H35 H -0.1322 0.6470 0.8670 0.043 Uiso 1 1 calc R . . C36 C -0.2204(3) 0.5479(3) 0.6887(3) 0.0366(15) Uani 1 1 d . . . H36 H -0.2645 0.5284 0.6880 0.044 Uiso 1 1 calc R . . C37 C -0.1970(4) 0.5817(4) 0.6338(3) 0.0458(18) Uani 1 1 d . . . H37 H -0.2247 0.5841 0.5969 0.055 Uiso 1 1 calc R . . C38 C -0.1322(4) 0.6114(4) 0.6353(4) 0.0462(18) Uani 1 1 d . . . H38 H -0.1156 0.6349 0.5996 0.055 Uiso 1 1 calc R . . C39 C -0.0924(3) 0.6058(3) 0.6903(3) 0.0390(16) Uani 1 1 d . . . H39 H -0.0485 0.6256 0.6923 0.047 Uiso 1 1 calc R . . C40 C -0.1177(3) 0.5712(3) 0.7421(3) 0.0349(15) Uani 1 1 d . . . H40 H -0.0896 0.5673 0.7786 0.042 Uiso 1 1 calc R . . C41 C -0.1588(3) 0.3663(3) 0.7688(3) 0.0323(14) Uani 1 1 d . . . H41 H -0.1188 0.3875 0.7840 0.039 Uiso 1 1 calc R . . C42 C -0.1514(3) 0.3067(3) 0.7343(3) 0.0341(15) Uani 1 1 d . . . H42 H -0.1076 0.2879 0.7274 0.041 Uiso 1 1 calc R . . C43 C -0.2116(3) 0.2763(3) 0.7105(3) 0.0360(16) Uani 1 1 d . . . H43 H -0.2083 0.2367 0.6870 0.043 Uiso 1 1 calc R . . C44 C -0.2761(3) 0.3048(3) 0.7217(3) 0.0313(14) Uani 1 1 d . . . H44 H -0.3165 0.2850 0.7057 0.038 Uiso 1 1 calc R . . C45 C -0.2794(3) 0.3647(3) 0.7580(3) 0.0255(13) Uani 1 1 d . . . H45 H -0.3227 0.3840 0.7663 0.031 Uiso 1 1 calc R . . C46 C -0.2041(3) 0.3661(3) 0.9560(3) 0.0305(14) Uani 1 1 d . . . H46 H -0.1580 0.3781 0.9478 0.037 Uiso 1 1 calc R . . C47 C -0.2173(3) 0.3141(3) 1.0003(3) 0.0299(14) Uani 1 1 d . . . H47 H -0.1809 0.2924 1.0215 0.036 Uiso 1 1 calc R . . C48 C -0.2854(3) 0.2963(3) 1.0112(3) 0.0353(15) Uani 1 1 d . . . H48 H -0.2957 0.2620 1.0401 0.042 Uiso 1 1 calc R . . C49 C -0.3385(3) 0.3290(3) 0.9796(3) 0.0260(13) Uani 1 1 d . . . H49 H -0.3849 0.3175 0.9870 0.031 Uiso 1 1 calc R . . C50 C -0.3217(3) 0.3793(3) 0.9367(3) 0.0288(14) Uani 1 1 d . . . H50 H -0.3576 0.4008 0.9145 0.035 Uiso 1 1 calc R . . C51 C 0.0603(3) 0.5129(3) 0.7367(3) 0.0385(15) Uani 1 1 d . . . H51 H 0.0715 0.5530 0.7570 0.046 Uiso 1 1 calc R . . C52 C 0.0607(3) 0.5113(3) 0.6704(3) 0.0376(15) Uani 1 1 d . . . H52 H 0.0717 0.5495 0.6468 0.045 Uiso 1 1 calc R . . C53 C 0.0445(4) 0.4524(3) 0.6394(4) 0.0438(17) Uani 1 1 d . . . H53 H 0.0445 0.4496 0.5945 0.053 Uiso 1 1 calc R . . C54 C 0.0281(4) 0.3971(3) 0.6774(4) 0.0412(16) Uani 1 1 d . . . H54 H 0.0164 0.3564 0.6585 0.049 Uiso 1 1 calc R . . C55 C 0.0296(3) 0.4040(3) 0.7438(4) 0.0432(18) Uani 1 1 d . . . H55 H 0.0192 0.3666 0.7689 0.052 Uiso 1 1 calc R . . C56 C -0.0436(3) 0.5454(3) 1.0946(4) 0.0429(16) Uani 1 1 d . . . H56 H -0.0298 0.5870 1.0788 0.052 Uiso 1 1 calc R . . C57 C -0.0643(3) 0.5417(3) 1.1585(3) 0.0400(16) Uani 1 1 d . . . H57 H -0.0645 0.5796 1.1847 0.048 Uiso 1 1 calc R . . C58 C -0.0847(3) 0.4804(4) 1.1824(3) 0.0446(17) Uani 1 1 d . . . H58 H -0.0986 0.4754 1.2253 0.054 Uiso 1 1 calc R . . C59 C -0.0839(4) 0.4265(3) 1.1402(4) 0.0443(17) Uani 1 1 d . . . H59 H -0.0976 0.3843 1.1546 0.053 Uiso 1 1 calc R . . C60 C -0.0633(3) 0.4351(3) 1.0786(4) 0.0420(17) Uani 1 1 d . . . H60 H -0.0638 0.3980 1.0513 0.050 Uiso 1 1 calc R . . C61 C 0.0357(4) 0.6943(4) 0.9494(4) 0.0485(19) Uani 1 1 d . . . C62 C -0.0648(4) 0.2285(3) 0.8810(3) 0.0396(17) Uani 1 1 d . . . C63 C 0.5162(4) 0.1896(4) 0.7032(4) 0.054(2) Uani 1 1 d . . . N13 N 0.5036(3) 0.4924(3) 0.9480(3) 0.0480(14) Uani 1 1 d . . . C64 C 0.4850(3) 0.4343(3) 0.9765(4) 0.0399(16) Uani 1 1 d . . . H64 H 0.4754 0.4344 1.0206 0.048 Uiso 1 1 calc R . . C65 C 0.4796(3) 0.3737(3) 0.9426(3) 0.0393(16) Uani 1 1 d . . . H65 H 0.4661 0.3347 0.9638 0.047 Uiso 1 1 calc R . . C66 C 0.4945(4) 0.3731(4) 0.8776(3) 0.0428(16) Uani 1 1 d . . . H66 H 0.4909 0.3335 0.8540 0.051 Uiso 1 1 calc R . . C67 C 0.5144(3) 0.4305(3) 0.8481(4) 0.0436(17) Uani 1 1 d . . . H67 H 0.5253 0.4312 0.8043 0.052 Uiso 1 1 calc R . . C68 C 0.5182(3) 0.4892(4) 0.8856(4) 0.0455(18) Uani 1 1 d . . . H68 H 0.5320 0.5284 0.8650 0.055 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 0.02379(10) 0.02747(11) 0.03224(12) 0.00344(9) 0.00017(11) 0.00150(10) U2 0.02356(10) 0.02453(10) 0.02552(11) 0.00156(9) 0.00006(9) 0.00016(11) Tl 0.02589(11) 0.03160(10) 0.03132(12) 0.00387(9) -0.00099(10) 0.00103(10) S1 0.0314(8) 0.0268(8) 0.0403(10) 0.0033(7) 0.0022(7) 0.0001(6) S2 0.0287(8) 0.0274(7) 0.0393(10) 0.0050(6) -0.0006(7) 0.0009(6) S3 0.0367(9) 0.0367(8) 0.0629(12) -0.0058(8) -0.0089(9) 0.0074(8) O1 0.031(2) 0.027(2) 0.038(2) 0.0014(18) -0.0015(17) -0.0028(18) O2 0.031(2) 0.031(2) 0.040(3) 0.0043(19) -0.0001(19) -0.0018(18) O3 0.031(2) 0.027(2) 0.031(2) -0.0012(18) 0.0003(17) -0.0043(18) O4 0.029(2) 0.031(2) 0.028(2) 0.0002(18) 0.0002(17) 0.0005(18) O5 0.038(3) 0.032(2) 0.054(3) 0.000(2) -0.002(2) -0.009(2) O6 0.043(3) 0.036(2) 0.061(3) 0.018(2) 0.006(3) 0.010(2) O7 0.032(3) 0.042(3) 0.058(3) 0.013(2) 0.007(2) 0.002(2) O8 0.051(3) 0.039(3) 0.089(4) 0.031(3) -0.010(3) -0.011(2) O9 0.036(3) 0.046(3) 0.036(3) -0.011(2) 0.007(2) 0.002(2) O10 0.029(3) 0.075(3) 0.040(3) 0.009(3) 0.005(2) 0.017(2) O11 0.086(4) 0.066(3) 0.044(3) 0.017(3) -0.014(3) 0.004(3) O12 0.033(3) 0.070(4) 0.072(4) -0.021(3) 0.010(3) 0.007(2) O13 0.042(3) 0.038(3) 0.044(3) 0.002(2) -0.005(2) -0.005(2) N1 0.035(3) 0.033(3) 0.035(3) 0.005(2) 0.004(2) 0.003(2) N2 0.034(3) 0.036(3) 0.028(3) 0.000(2) -0.003(2) 0.001(2) N3 0.036(3) 0.023(2) 0.037(3) 0.002(2) -0.001(2) -0.003(2) N4 0.033(3) 0.025(2) 0.036(3) 0.003(2) 0.006(3) 0.002(2) N5 0.026(3) 0.026(2) 0.031(3) 0.006(2) 0.002(2) 0.002(2) N6 0.035(3) 0.026(2) 0.029(3) 0.002(2) 0.002(3) 0.003(2) N7 0.031(3) 0.031(3) 0.038(3) 0.003(2) -0.006(3) 0.001(3) N8 0.024(3) 0.033(3) 0.031(3) 0.006(2) -0.001(2) -0.001(2) N9 0.030(3) 0.028(2) 0.027(3) 0.000(2) 0.001(2) 0.003(2) N10 0.025(3) 0.025(2) 0.031(3) 0.003(2) 0.001(2) -0.0030(19) N11 0.040(3) 0.038(3) 0.044(4) 0.004(3) -0.002(3) 0.005(3) N12 0.033(3) 0.048(3) 0.040(3) -0.009(3) -0.003(2) 0.002(3) F1 0.105(4) 0.064(3) 0.100(5) -0.035(3) -0.039(4) -0.005(3) F2 0.054(3) 0.074(3) 0.047(3) 0.005(2) -0.002(2) 0.018(2) F3 0.061(3) 0.113(4) 0.047(3) -0.019(3) 0.001(3) 0.043(3) F4 0.118(4) 0.0231(19) 0.064(3) 0.003(2) -0.041(3) -0.011(2) F5 0.032(2) 0.060(3) 0.043(2) -0.0031(19) -0.0048(17) -0.0048(18) F6 0.073(3) 0.077(3) 0.028(2) -0.011(2) -0.004(2) 0.037(3) F7 0.083(4) 0.051(3) 0.115(5) -0.025(3) -0.039(3) -0.003(3) F8 0.083(4) 0.051(3) 0.078(4) 0.021(2) -0.001(3) -0.004(2) F9 0.062(3) 0.051(3) 0.075(3) -0.007(2) 0.013(3) 0.020(2) C1 0.028(3) 0.035(3) 0.049(4) -0.001(3) 0.003(3) -0.001(3) C2 0.044(4) 0.033(3) 0.052(5) -0.001(3) 0.011(4) -0.004(3) C3 0.068(5) 0.030(3) 0.039(4) -0.001(3) 0.012(4) -0.005(3) C4 0.050(4) 0.034(3) 0.039(4) 0.005(3) -0.006(3) -0.013(3) C5 0.032(3) 0.038(3) 0.037(4) 0.004(3) -0.006(3) -0.002(3) C6 0.046(4) 0.031(3) 0.042(4) -0.001(3) -0.007(3) 0.007(3) C7 0.060(5) 0.032(3) 0.045(4) -0.002(3) -0.015(4) 0.003(4) C8 0.069(5) 0.034(4) 0.048(5) 0.001(3) -0.013(4) -0.010(4) C9 0.046(4) 0.051(4) 0.049(5) -0.008(4) -0.004(4) -0.021(3) C10 0.041(4) 0.032(3) 0.040(4) 0.003(3) -0.007(3) -0.004(3) C11 0.031(3) 0.038(3) 0.034(3) 0.001(3) -0.006(3) -0.003(3) C12 0.042(4) 0.030(3) 0.037(4) 0.006(3) -0.010(3) 0.002(3) C13 0.047(4) 0.039(4) 0.033(4) 0.007(3) 0.004(3) -0.015(3) C14 0.026(3) 0.043(4) 0.042(4) 0.000(3) 0.000(3) -0.002(3) C15 0.027(3) 0.026(3) 0.036(4) 0.003(3) 0.002(3) 0.001(3) C16 0.031(3) 0.029(3) 0.044(4) 0.007(3) 0.011(3) 0.000(3) C17 0.047(4) 0.030(3) 0.057(5) 0.009(3) 0.025(4) 0.005(3) C18 0.074(5) 0.036(4) 0.034(4) 0.003(3) 0.016(4) -0.003(4) C19 0.047(4) 0.038(4) 0.037(4) 0.000(3) 0.000(3) 0.001(3) C20 0.033(3) 0.027(3) 0.036(4) 0.002(3) -0.001(3) -0.003(3) C21 0.030(3) 0.029(3) 0.030(3) 0.000(3) -0.002(3) -0.001(3) C22 0.039(4) 0.024(3) 0.028(4) 0.001(2) -0.001(3) 0.005(3) C23 0.040(4) 0.026(3) 0.036(4) -0.001(3) 0.007(3) 0.002(3) C24 0.028(3) 0.036(3) 0.038(4) -0.001(3) 0.005(3) -0.001(3) C25 0.025(3) 0.034(3) 0.041(4) 0.005(3) 0.002(3) 0.000(3) C26 0.034(4) 0.045(4) 0.039(4) -0.006(3) -0.006(3) 0.004(3) C27 0.054(4) 0.053(4) 0.035(4) -0.006(3) -0.001(4) -0.002(4) C28 0.069(6) 0.052(4) 0.045(5) -0.014(4) 0.011(4) -0.006(4) C29 0.038(4) 0.058(5) 0.055(5) -0.011(4) 0.012(4) -0.006(3) C30 0.031(3) 0.037(4) 0.038(4) -0.005(3) 0.003(3) -0.004(3) C31 0.031(3) 0.034(3) 0.046(4) 0.006(3) -0.003(3) 0.005(3) C32 0.041(4) 0.030(3) 0.052(5) 0.001(3) -0.009(3) 0.011(3) C33 0.067(5) 0.031(3) 0.043(4) 0.001(3) -0.012(4) 0.001(4) C34 0.046(4) 0.036(4) 0.052(5) 0.002(3) -0.009(4) 0.003(3) C35 0.032(4) 0.027(3) 0.049(5) 0.003(3) -0.001(3) 0.004(3) C36 0.039(4) 0.041(4) 0.030(4) 0.009(3) -0.001(3) -0.006(3) C37 0.052(4) 0.057(4) 0.028(4) 0.014(3) -0.012(3) -0.017(4) C38 0.045(4) 0.047(4) 0.046(5) 0.017(3) 0.008(3) -0.001(3) C39 0.028(3) 0.043(4) 0.046(5) 0.009(3) -0.001(3) -0.003(3) C40 0.024(3) 0.043(4) 0.038(4) 0.007(3) -0.003(3) -0.002(3) C41 0.030(3) 0.032(3) 0.035(4) 0.001(3) -0.001(3) 0.004(3) C42 0.044(4) 0.032(3) 0.026(4) 0.000(3) 0.004(3) 0.008(3) C43 0.051(4) 0.025(3) 0.032(4) 0.001(3) 0.009(3) 0.003(3) C44 0.034(4) 0.029(3) 0.031(4) 0.002(2) 0.002(3) -0.006(3) C45 0.025(3) 0.028(3) 0.024(3) -0.001(2) 0.000(2) -0.002(2) C46 0.027(3) 0.030(3) 0.034(4) -0.004(3) -0.001(3) 0.009(3) C47 0.031(4) 0.031(3) 0.028(3) 0.007(3) 0.002(3) 0.006(3) C48 0.040(4) 0.032(3) 0.034(4) 0.001(3) 0.001(3) 0.002(3) C49 0.030(3) 0.023(3) 0.025(3) -0.005(2) 0.004(3) -0.002(2) C50 0.032(3) 0.029(3) 0.026(3) 0.002(2) 0.000(3) -0.003(3) C51 0.035(3) 0.028(3) 0.052(4) -0.012(3) -0.002(3) -0.002(3) C52 0.039(3) 0.037(4) 0.037(4) 0.003(3) 0.010(3) 0.002(3) C53 0.046(4) 0.046(4) 0.039(4) -0.001(3) 0.005(3) -0.003(3) C54 0.043(4) 0.038(4) 0.042(4) -0.007(3) 0.007(3) -0.005(3) C55 0.028(4) 0.036(4) 0.066(5) 0.015(4) 0.004(3) 0.000(3) C56 0.031(3) 0.044(4) 0.053(5) -0.004(3) -0.001(3) -0.006(3) C57 0.033(3) 0.046(4) 0.041(4) -0.011(3) 0.000(3) -0.002(3) C58 0.042(4) 0.060(5) 0.032(4) -0.008(3) 0.011(3) -0.005(3) C59 0.041(4) 0.042(4) 0.049(5) 0.003(3) -0.004(4) -0.008(3) C60 0.038(4) 0.043(4) 0.045(5) -0.011(3) -0.005(3) 0.005(3) C61 0.040(4) 0.047(4) 0.060(5) -0.010(4) -0.005(4) 0.015(4) C62 0.060(5) 0.033(4) 0.026(4) 0.006(3) 0.004(3) 0.010(3) C63 0.054(5) 0.053(4) 0.057(5) -0.004(4) -0.005(4) -0.008(4) N13 0.032(3) 0.043(3) 0.069(4) 0.003(3) -0.007(3) -0.001(3) C64 0.029(3) 0.049(4) 0.042(4) 0.010(3) 0.004(3) 0.003(3) C65 0.033(4) 0.039(4) 0.046(4) 0.010(3) 0.001(3) 0.000(3) C66 0.031(4) 0.050(4) 0.047(5) 0.004(3) 0.002(3) 0.001(3) C67 0.030(4) 0.056(4) 0.045(4) 0.013(4) -0.001(3) -0.001(3) C68 0.032(4) 0.042(4) 0.063(5) 0.028(4) -0.006(3) -0.002(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 U1 O2 1.828(4) . ? U1 O1 1.836(4) . ? U1 N1 2.601(5) . ? U1 N5 2.611(5) . ? U1 N4 2.618(5) . ? U1 N3 2.623(5) . ? U1 N2 2.632(5) . ? U2 O4 1.829(4) . ? U2 O3 1.833(4) . ? U2 N8 2.581(5) . ? U2 N10 2.588(5) . ? U2 N6 2.605(5) . ? U2 N9 2.606(5) . ? U2 N7 2.623(5) . ? Tl O3 2.801(4) . ? Tl O5 2.804(4) . ? Tl O1 2.839(4) . ? Tl O8 2.890(5) . ? Tl N11 2.989(6) . ? Tl N12 3.076(5) . ? S1 O7 1.433(4) . ? S1 O6 1.440(4) . ? S1 O5 1.454(4) . ? S1 C61 1.810(8) . ? S2 O9 1.432(5) . ? S2 O8 1.441(5) . ? S2 O10 1.442(4) . ? S2 C62 1.805(7) . ? S3 O12 1.409(5) . ? S3 O13 1.440(5) . ? S3 O11 1.474(6) . ? S3 C63 1.792(8) . ? N1 C1 1.345(7) . ? N1 C5 1.359(8) . ? N2 C10 1.339(8) . ? N2 C6 1.343(8) . ? N3 C11 1.324(8) . ? N3 C15 1.353(7) . ? N4 C20 1.329(8) . ? N4 C16 1.353(8) . ? N5 C25 1.340(7) . ? N5 C21 1.343(7) . ? N6 C26 1.339(8) . ? N6 C30 1.347(8) . ? N7 C31 1.333(8) . ? N7 C35 1.334(8) . ? N8 C40 1.342(7) . ? N8 C36 1.359(8) . ? N9 C41 1.344(7) . ? N9 C45 1.350(7) . ? N10 C46 1.334(7) . ? N10 C50 1.354(7) . ? N11 C55 1.322(9) . ? N11 C51 1.334(8) . ? N12 C56 1.328(8) . ? N12 C60 1.343(9) . ? F1 C61 1.339(9) . ? F2 C61 1.331(8) . ? F3 C61 1.335(8) . ? F4 C62 1.348(7) . ? F5 C62 1.344(8) . ? F6 C62 1.327(8) . ? F7 C63 1.334(8) . ? F8 C63 1.357(9) . ? F9 C63 1.308(9) . ? C1 C2 1.371(9) . ? C1 H1 0.9300 . ? C2 C3 1.376(10) . ? C2 H2 0.9300 . ? C3 C4 1.367(10) . ? C3 H3 0.9300 . ? C4 C5 1.362(9) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.386(9) . ? C6 H6 0.9300 . ? C7 C8 1.394(11) . ? C7 H7 0.9300 . ? C8 C9 1.367(10) . ? C8 H8 0.9300 . ? C9 C10 1.406(9) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.373(9) . ? C11 H11 0.9300 . ? C12 C13 1.370(9) . ? C12 H12 0.9300 . ? C13 C14 1.393(9) . ? C13 H13 0.9300 . ? C14 C15 1.377(8) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.403(9) . ? C16 H16 0.9300 . ? C17 C18 1.395(11) . ? C17 H17 0.9300 . ? C18 C19 1.356(10) . ? C18 H18 0.9300 . ? C19 C20 1.390(9) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.386(8) . ? C21 H21 0.9300 . ? C22 C23 1.372(9) . ? C22 H22 0.9300 . ? C23 C24 1.393(9) . ? C23 H23 0.9300 . ? C24 C25 1.385(9) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.391(9) . ? C26 H26 0.9300 . ? C27 C28 1.350(11) . ? C27 H27 0.9300 . ? C28 C29 1.394(11) . ? C28 H28 0.9300 . ? C29 C30 1.378(9) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.401(9) . ? C31 H31 0.9300 . ? C32 C33 1.376(10) . ? C32 H32 0.9300 . ? C33 C34 1.397(10) . ? C33 H33 0.9300 . ? C34 C35 1.367(9) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C37 1.392(9) . ? C36 H36 0.9300 . ? C37 C38 1.376(9) . ? C37 H37 0.9300 . ? C38 C39 1.372(10) . ? C38 H38 0.9300 . ? C39 C40 1.363(9) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 C42 1.395(8) . ? C41 H41 0.9300 . ? C42 C43 1.392(9) . ? C42 H42 0.9300 . ? C43 C44 1.380(9) . ? C43 H43 0.9300 . ? C44 C45 1.412(8) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 C47 1.407(8) . ? C46 H46 0.9300 . ? C47 C48 1.371(9) . ? C47 H47 0.9300 . ? C48 C49 1.374(8) . ? C48 H48 0.9300 . ? C49 C50 1.378(8) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? C51 C52 1.370(9) . ? C51 H51 0.9300 . ? C52 C53 1.374(9) . ? C52 H52 0.9300 . ? C53 C54 1.391(9) . ? C53 H53 0.9300 . ? C54 C55 1.378(10) . ? C54 H54 0.9300 . ? C55 H55 0.9300 . ? C56 C57 1.380(10) . ? C56 H56 0.9300 . ? C57 C58 1.376(10) . ? C57 H57 0.9300 . ? C58 C59 1.386(9) . ? C58 H58 0.9300 . ? C59 C60 1.343(10) . ? C59 H59 0.9300 . ? C60 H60 0.9300 . ? N13 C68 1.322(9) . ? N13 C64 1.348(8) . ? C64 C65 1.402(10) . ? C64 H64 0.9300 . ? C65 C66 1.373(10) . ? C65 H65 0.9300 . ? C66 C67 1.353(9) . ? C66 H66 0.9300 . ? C67 C68 1.406(10) . ? C67 H67 0.9300 . ? C68 H68 0.9300 . ? 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 O1 177.92(18) . . ? O2 U1 N1 90.47(18) . . ? O1 U1 N1 88.63(16) . . ? O2 U1 N5 87.63(16) . . ? O1 U1 N5 90.31(16) . . ? N1 U1 N5 72.61(15) . . ? O2 U1 N4 89.09(18) . . ? O1 U1 N4 90.73(18) . . ? N1 U1 N4 149.51(15) . . ? N5 U1 N4 76.91(15) . . ? O2 U1 N3 94.31(17) . . ? O1 U1 N3 87.62(16) . . ? N1 U1 N3 137.85(15) . . ? N5 U1 N3 149.34(15) . . ? N4 U1 N3 72.54(14) . . ? O2 U1 N2 86.04(17) . . ? O1 U1 N2 95.43(16) . . ? N1 U1 N2 70.94(16) . . ? N5 U1 N2 142.90(16) . . ? N4 U1 N2 139.37(16) . . ? N3 U1 N2 67.68(15) . . ? O4 U2 O3 179.74(19) . . ? O4 U2 N8 94.13(16) . . ? O3 U2 N8 86.01(16) . . ? O4 U2 N10 92.51(16) . . ? O3 U2 N10 87.25(16) . . ? N8 U2 N10 145.70(15) . . ? O4 U2 N6 90.80(17) . . ? O3 U2 N6 89.22(16) . . ? N8 U2 N6 141.99(15) . . ? N10 U2 N6 71.37(15) . . ? O4 U2 N9 86.62(16) . . ? O3 U2 N9 93.20(16) . . ? N8 U2 N9 74.87(15) . . ? N10 U2 N9 71.99(15) . . ? N6 U2 N9 143.11(14) . . ? O4 U2 N7 86.66(17) . . ? O3 U2 N7 93.59(17) . . ? N8 U2 N7 73.21(16) . . ? N10 U2 N7 140.83(16) . . ? N6 U2 N7 69.48(15) . . ? N9 U2 N7 146.76(16) . . ? O3 Tl O5 77.48(12) . . ? O3 Tl O1 174.18(11) . . ? O5 Tl O1 97.79(12) . . ? O3 Tl O8 86.54(13) . . ? O5 Tl O8 148.76(15) . . ? O1 Tl O8 99.21(13) . . ? O3 Tl N11 93.01(13) . . ? O5 Tl N11 80.33(14) . . ? O1 Tl N11 89.51(13) . . ? O8 Tl N11 73.82(16) . . ? O3 Tl N12 87.38(12) . . ? O5 Tl N12 107.25(14) . . ? O1 Tl N12 90.83(12) . . ? O8 Tl N12 98.52(16) . . ? N11 Tl N12 172.29(15) . . ? O7 S1 O6 116.4(3) . . ? O7 S1 O5 114.4(3) . . ? O6 S1 O5 114.5(3) . . ? O7 S1 C61 103.7(3) . . ? O6 S1 C61 103.6(3) . . ? O5 S1 C61 101.6(3) . . ? O9 S2 O8 114.7(3) . . ? O9 S2 O10 115.6(3) . . ? O8 S2 O10 115.0(3) . . ? O9 S2 C62 104.1(3) . . ? O8 S2 C62 102.1(3) . . ? O10 S2 C62 102.7(3) . . ? O12 S3 O13 115.9(3) . . ? O12 S3 O11 113.0(4) . . ? O13 S3 O11 114.1(3) . . ? O12 S3 C63 106.5(4) . . ? O13 S3 C63 104.5(3) . . ? O11 S3 C63 100.8(4) . . ? U1 O1 Tl 164.2(2) . . ? U2 O3 Tl 176.2(2) . . ? S1 O5 Tl 134.2(3) . . ? S2 O8 Tl 139.4(4) . . ? C1 N1 C5 116.7(6) . . ? C1 N1 U1 121.0(4) . . ? C5 N1 U1 121.9(4) . . ? C10 N2 C6 118.9(6) . . ? C10 N2 U1 119.0(4) . . ? C6 N2 U1 121.6(4) . . ? C11 N3 C15 118.5(5) . . ? C11 N3 U1 120.2(4) . . ? C15 N3 U1 119.9(4) . . ? C20 N4 C16 117.8(5) . . ? C20 N4 U1 123.0(4) . . ? C16 N4 U1 119.0(4) . . ? C25 N5 C21 117.9(5) . . ? C25 N5 U1 122.2(4) . . ? C21 N5 U1 119.7(4) . . ? C26 N6 C30 117.3(6) . . ? C26 N6 U2 121.9(4) . . ? C30 N6 U2 120.8(4) . . ? C31 N7 C35 117.4(5) . . ? C31 N7 U2 119.4(4) . . ? C35 N7 U2 122.2(4) . . ? C40 N8 C36 116.8(5) . . ? C40 N8 U2 118.9(4) . . ? C36 N8 U2 123.2(4) . . ? C41 N9 C45 118.9(5) . . ? C41 N9 U2 120.8(4) . . ? C45 N9 U2 120.3(4) . . ? C46 N10 C50 117.8(5) . . ? C46 N10 U2 122.2(4) . . ? C50 N10 U2 119.9(4) . . ? C55 N11 C51 116.3(6) . . ? C55 N11 Tl 122.7(5) . . ? C51 N11 Tl 117.9(4) . . ? C56 N12 C60 115.5(6) . . ? C56 N12 Tl 130.3(5) . . ? C60 N12 Tl 114.2(4) . . ? N1 C1 C2 122.7(6) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C1 C2 C3 119.1(6) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C4 C3 C2 119.1(7) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C5 C4 C3 119.1(7) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N1 C5 C4 123.1(6) . . ? N1 C5 H5 118.4 . . ? C4 C5 H5 118.4 . . ? N2 C6 C7 122.2(7) . . ? N2 C6 H6 118.9 . . ? C7 C6 H6 118.9 . . ? C6 C7 C8 119.0(7) . . ? C6 C7 H7 120.5 . . ? C8 C7 H7 120.5 . . ? C9 C8 C7 118.9(7) . . ? C9 C8 H8 120.6 . . ? C7 C8 H8 120.6 . . ? C8 C9 C10 119.2(7) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? N2 C10 C9 121.8(6) . . ? N2 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? N3 C11 C12 122.8(6) . . ? N3 C11 H11 118.6 . . ? C12 C11 H11 118.6 . . ? C13 C12 C11 119.5(6) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C14 118.5(6) . . ? C12 C13 H13 120.7 . . ? C14 C13 H13 120.7 . . ? C15 C14 C13 118.9(6) . . ? C15 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? N3 C15 C14 121.9(5) . . ? N3 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? N4 C16 C17 122.6(6) . . ? N4 C16 H16 118.7 . . ? C17 C16 H16 118.7 . . ? C18 C17 C16 117.4(6) . . ? C18 C17 H17 121.3 . . ? C16 C17 H17 121.3 . . ? C19 C18 C17 119.9(6) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 119.3(7) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? N4 C20 C19 123.0(6) . . ? N4 C20 H20 118.5 . . ? C19 C20 H20 118.5 . . ? N5 C21 C22 122.1(6) . . ? N5 C21 H21 118.9 . . ? C22 C21 H21 118.9 . . ? C23 C22 C21 120.0(6) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 118.2(6) . . ? C22 C23 H23 120.9 . . ? C24 C23 H23 120.9 . . ? C25 C24 C23 118.7(6) . . ? C25 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? N5 C25 C24 123.0(6) . . ? N5 C25 H25 118.5 . . ? C24 C25 H25 118.5 . . ? N6 C26 C27 122.7(6) . . ? N6 C26 H26 118.6 . . ? C27 C26 H26 118.6 . . ? C28 C27 C26 119.1(7) . . ? C28 C27 H27 120.5 . . ? C26 C27 H27 120.5 . . ? C27 C28 C29 119.7(7) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C30 C29 C28 117.9(7) . . ? C30 C29 H29 121.1 . . ? C28 C29 H29 121.1 . . ? N6 C30 C29 123.3(6) . . ? N6 C30 H30 118.4 . . ? C29 C30 H30 118.4 . . ? N7 C31 C32 123.2(6) . . ? N7 C31 H31 118.4 . . ? C32 C31 H31 118.4 . . ? C33 C32 C31 118.0(6) . . ? C33 C32 H32 121.0 . . ? C31 C32 H32 121.0 . . ? C32 C33 C34 119.0(6) . . ? C32 C33 H33 120.5 . . ? C34 C33 H33 120.5 . . ? C35 C34 C33 118.4(7) . . ? C35 C34 H34 120.8 . . ? C33 C34 H34 120.8 . . ? N7 C35 C34 124.0(6) . . ? N7 C35 H35 118.0 . . ? C34 C35 H35 118.0 . . ? N8 C36 C37 122.4(6) . . ? N8 C36 H36 118.8 . . ? C37 C36 H36 118.8 . . ? C38 C37 C36 118.8(6) . . ? C38 C37 H37 120.6 . . ? C36 C37 H37 120.6 . . ? C39 C38 C37 118.9(6) . . ? C39 C38 H38 120.6 . . ? C37 C38 H38 120.6 . . ? C40 C39 C38 119.6(6) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? N8 C40 C39 123.5(6) . . ? N8 C40 H40 118.3 . . ? C39 C40 H40 118.3 . . ? N9 C41 C42 122.9(6) . . ? N9 C41 H41 118.6 . . ? C42 C41 H41 118.6 . . ? C43 C42 C41 118.0(6) . . ? C43 C42 H42 121.0 . . ? C41 C42 H42 121.0 . . ? C44 C43 C42 120.0(6) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 118.6(6) . . ? C43 C44 H44 120.7 . . ? C45 C44 H44 120.7 . . ? N9 C45 C44 121.5(5) . . ? N9 C45 H45 119.3 . . ? C44 C45 H45 119.3 . . ? N10 C46 C47 122.6(6) . . ? N10 C46 H46 118.7 . . ? C47 C46 H46 118.7 . . ? C48 C47 C46 118.0(6) . . ? C48 C47 H47 121.0 . . ? C46 C47 H47 121.0 . . ? C47 C48 C49 120.2(6) . . ? C47 C48 H48 119.9 . . ? C49 C48 H48 119.9 . . ? C48 C49 C50 118.7(6) . . ? C48 C49 H49 120.6 . . ? C50 C49 H49 120.6 . . ? N10 C50 C49 122.7(6) . . ? N10 C50 H50 118.7 . . ? C49 C50 H50 118.7 . . ? N11 C51 C52 124.2(6) . . ? N11 C51 H51 117.9 . . ? C52 C51 H51 117.9 . . ? C51 C52 C53 118.9(6) . . ? C51 C52 H52 120.5 . . ? C53 C52 H52 120.5 . . ? C52 C53 C54 117.9(7) . . ? C52 C53 H53 121.1 . . ? C54 C53 H53 121.1 . . ? C55 C54 C53 118.5(7) . . ? C55 C54 H54 120.7 . . ? C53 C54 H54 120.7 . . ? N11 C55 C54 124.1(6) . . ? N11 C55 H55 118.0 . . ? C54 C55 H55 118.0 . . ? N12 C56 C57 124.7(7) . . ? N12 C56 H56 117.6 . . ? C57 C56 H56 117.6 . . ? C58 C57 C56 118.2(6) . . ? C58 C57 H57 120.9 . . ? C56 C57 H57 120.9 . . ? C57 C58 C59 117.6(6) . . ? C57 C58 H58 121.2 . . ? C59 C58 H58 121.2 . . ? C60 C59 C58 120.0(7) . . ? C60 C59 H59 120.0 . . ? C58 C59 H59 120.0 . . ? C59 C60 N12 124.1(7) . . ? C59 C60 H60 118.0 . . ? N12 C60 H60 118.0 . . ? F2 C61 F3 107.1(7) . . ? F2 C61 F1 106.5(6) . . ? F3 C61 F1 108.0(6) . . ? F2 C61 S1 112.0(5) . . ? F3 C61 S1 111.5(5) . . ? F1 C61 S1 111.5(6) . . ? F6 C62 F5 107.6(5) . . ? F6 C62 F4 107.2(6) . . ? F5 C62 F4 105.6(6) . . ? F6 C62 S2 112.3(5) . . ? F5 C62 S2 112.3(4) . . ? F4 C62 S2 111.4(5) . . ? F9 C63 F7 108.5(7) . . ? F9 C63 F8 106.4(7) . . ? F7 C63 F8 106.8(6) . . ? F9 C63 S3 112.9(5) . . ? F7 C63 S3 111.9(6) . . ? F8 C63 S3 110.1(5) . . ? C68 N13 C64 116.1(6) . . ? N13 C64 C65 123.0(7) . . ? N13 C64 H64 118.5 . . ? C65 C64 H64 118.5 . . ? C66 C65 C64 118.8(7) . . ? C66 C65 H65 120.6 . . ? C64 C65 H65 120.6 . . ? C67 C66 C65 119.3(7) . . ? C67 C66 H66 120.3 . . ? C65 C66 H66 120.3 . . ? C66 C67 C68 118.3(7) . . ? C66 C67 H67 120.8 . . ? C68 C67 H67 120.8 . . ? N13 C68 C67 124.5(6) . . ? N13 C68 H68 117.8 . . ? C67 C68 H68 117.8 . . ? #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 711339' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H35 I Li N7 O2 U, I' _chemical_formula_sum 'C35 H35 I2 Li N7 O2 U' _chemical_formula_weight 1084.47 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' Li Li -0.0003 0.0001 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' 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' _cell_length_a 17.1377(8) _cell_length_b 12.3158(11) _cell_length_c 18.5640(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3918.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 158854 _cell_measurement_theta_min 3.31 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent dark orange' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.838 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2044 _exptl_absorpt_coefficient_mu 5.757 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.448 _exptl_absorpt_correction_T_max 0.708 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 40 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 area-detector diffractometer' _diffrn_measurement_method 'two \f and ten \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 158854 _diffrn_reflns_av_R_equivalents 0.0661 _diffrn_reflns_av_sigmaI/netI 0.0439 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 25.68 _reflns_number_total 7075 _reflns_number_gt 5982 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _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 and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. The Flack parameter value of 0.500(8) is ambiguous, but no model can be found in a centrosymmetric space group. This value likely indicates that the compound is an inversion twin with equal proportions of the two forms. 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^)+(0.0640P)^2^+12.1484P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.500(8) _refine_ls_number_reflns 7075 _refine_ls_number_parameters 434 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1132 _refine_ls_wR_factor_gt 0.1088 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.767 _refine_diff_density_min -1.025 _refine_diff_density_rms 0.348 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 0.274594(19) 0.53038(3) 0.21643(3) 0.02964(11) Uani 1 1 d . . . Li Li 0.2561(12) 0.5153(13) 0.4191(11) 0.035(4) Uani 1 1 d . . . I1 I 0.40688(4) 0.49420(6) 0.48436(5) 0.03950(18) Uani 1 1 d . . . I2 I 0.08645(4) 0.47229(6) 0.94229(4) 0.03794(19) Uani 1 1 d . . . O1 O 0.2645(4) 0.5304(5) 0.3173(5) 0.0271(17) Uani 1 1 d . . . O2 O 0.2846(4) 0.5302(5) 0.1226(5) 0.0301(18) Uani 1 1 d . . . N1 N 0.3596(5) 0.3580(7) 0.2312(5) 0.033(3) Uani 1 1 d . . . N2 N 0.4185(5) 0.5918(7) 0.2281(6) 0.034(2) Uani 1 1 d . . . N3 N 0.2757(4) 0.7456(7) 0.2126(8) 0.0335(19) Uani 1 1 d . . . N4 N 0.1307(6) 0.5913(7) 0.2000(5) 0.035(2) Uani 1 1 d . . . N5 N 0.1863(5) 0.3585(8) 0.2006(5) 0.032(2) Uani 1 1 d . . . N6 N 0.2002(6) 0.3633(8) 0.4445(6) 0.041(2) Uani 1 1 d . . . N7 N 0.1984(6) 0.6478(8) 0.4579(6) 0.041(3) Uani 1 1 d . . . C1 C 0.3820(7) 0.3245(10) 0.2973(7) 0.043(3) Uani 1 1 d . . . H1 H 0.3712 0.3690 0.3365 0.051 Uiso 1 1 calc R . . C2 C 0.4211(8) 0.2253(11) 0.3101(8) 0.050(3) Uani 1 1 d . . . H2 H 0.4362 0.2041 0.3562 0.061 Uiso 1 1 calc R . . C3 C 0.4352(9) 0.1630(13) 0.2518(10) 0.059(4) Uani 1 1 d . . . H3 H 0.4599 0.0966 0.2585 0.071 Uiso 1 1 calc R . . C4 C 0.4153(8) 0.1924(11) 0.1838(9) 0.051(4) Uani 1 1 d . . . H4 H 0.4275 0.1494 0.1442 0.061 Uiso 1 1 calc R . . C5 C 0.3753(7) 0.2909(10) 0.1764(8) 0.044(3) Uani 1 1 d . . . H5 H 0.3587 0.3110 0.1306 0.053 Uiso 1 1 calc R . . C6 C 0.4499(7) 0.5980(9) 0.2948(7) 0.035(3) Uani 1 1 d . . . H6 H 0.4175 0.5916 0.3348 0.042 Uiso 1 1 calc R . . C7 C 0.5287(7) 0.6137(10) 0.3048(7) 0.040(3) Uani 1 1 d . . . H7 H 0.5494 0.6188 0.3509 0.048 Uiso 1 1 calc R . . C8 C 0.5758(7) 0.6214(11) 0.2459(9) 0.048(4) Uani 1 1 d . . . H8 H 0.6289 0.6333 0.2521 0.058 Uiso 1 1 calc R . . C9 C 0.5457(7) 0.6118(10) 0.1773(8) 0.040(3) Uani 1 1 d . . . H9 H 0.5775 0.6152 0.1368 0.048 Uiso 1 1 calc R . . C10 C 0.4654(7) 0.5969(9) 0.1717(7) 0.034(3) Uani 1 1 d . . . H10 H 0.4437 0.5901 0.1260 0.041 Uiso 1 1 calc R . . C11 C 0.2595(8) 0.7954(11) 0.1500(7) 0.041(3) Uani 1 1 d . . . H11 H 0.2515 0.7525 0.1094 0.049 Uiso 1 1 calc R . . C12 C 0.2542(7) 0.9075(9) 0.1424(8) 0.041(3) Uani 1 1 d . . . H12 H 0.2412 0.9403 0.0988 0.049 Uiso 1 1 calc R . . C13 C 0.2698(6) 0.9680(9) 0.2054(15) 0.055(5) Uani 1 1 d . . . H13 H 0.2665 1.0433 0.2039 0.066 Uiso 1 1 calc R . . C14 C 0.2892(6) 0.9192(10) 0.2667(7) 0.039(3) Uani 1 1 d . . . H14 H 0.3011 0.9595 0.3076 0.047 Uiso 1 1 calc R . . C15 C 0.2910(6) 0.8075(10) 0.2681(7) 0.038(3) Uani 1 1 d . . . H15 H 0.3041 0.7738 0.3113 0.045 Uiso 1 1 calc R . . C16 C 0.0998(7) 0.5986(9) 0.1337(7) 0.040(3) Uani 1 1 d . . . H16 H 0.1328 0.5912 0.0943 0.048 Uiso 1 1 calc R . . C17 C 0.0217(6) 0.6164(9) 0.1213(7) 0.039(3) Uani 1 1 d . . . H17 H 0.0016 0.6207 0.0748 0.046 Uiso 1 1 calc R . . C18 C -0.0249(8) 0.6276(9) 0.1803(9) 0.040(3) Uani 1 1 d . . . H18 H -0.0779 0.6404 0.1738 0.048 Uiso 1 1 calc R . . C19 C 0.0036(8) 0.6207(10) 0.2476(8) 0.042(3) Uani 1 1 d . . . H19 H -0.0292 0.6269 0.2873 0.051 Uiso 1 1 calc R . . C20 C 0.0835(6) 0.6041(9) 0.2565(8) 0.036(3) Uani 1 1 d . . . H20 H 0.1044 0.6018 0.3028 0.043 Uiso 1 1 calc R . . C21 C 0.1608(7) 0.3331(10) 0.1348(7) 0.040(3) Uani 1 1 d . . . H21 H 0.1730 0.3796 0.0969 0.048 Uiso 1 1 calc R . . C22 C 0.1175(7) 0.2420(10) 0.1199(7) 0.046(3) Uani 1 1 d . . . H22 H 0.0995 0.2285 0.0735 0.056 Uiso 1 1 calc R . . C23 C 0.1011(9) 0.1696(11) 0.1766(9) 0.055(4) Uani 1 1 d . . . H23 H 0.0734 0.1059 0.1683 0.066 Uiso 1 1 calc R . . C24 C 0.1270(9) 0.1954(10) 0.2447(9) 0.054(4) Uani 1 1 d . . . H24 H 0.1165 0.1501 0.2837 0.065 Uiso 1 1 calc R . . C25 C 0.1689(7) 0.2904(10) 0.2537(7) 0.040(3) Uani 1 1 d . . . H25 H 0.1861 0.3077 0.2998 0.048 Uiso 1 1 calc R . . C26 C 0.1234(8) 0.3467(10) 0.4466(8) 0.047(3) Uani 1 1 d . . . H26 H 0.0910 0.4071 0.4432 0.057 Uiso 1 1 calc R . . C27 C 0.0879(7) 0.2441(10) 0.4536(8) 0.049(3) Uani 1 1 d . . . H27 H 0.0339 0.2362 0.4528 0.059 Uiso 1 1 calc R . . C28 C 0.1372(9) 0.1551(11) 0.4617(9) 0.061(4) Uani 1 1 d . . . H28 H 0.1172 0.0857 0.4687 0.073 Uiso 1 1 calc R . . C29 C 0.2168(9) 0.1730(12) 0.4590(8) 0.056(4) Uani 1 1 d . . . H29 H 0.2513 0.1148 0.4619 0.067 Uiso 1 1 calc R . . C30 C 0.2446(8) 0.2755(10) 0.4521(7) 0.038(3) Uani 1 1 d . . . H30 H 0.2984 0.2851 0.4528 0.046 Uiso 1 1 calc R . . C31 C 0.1193(7) 0.6545(9) 0.4665(7) 0.042(3) Uani 1 1 d . . . H31 H 0.0903 0.5909 0.4623 0.051 Uiso 1 1 calc R . . C32 C 0.0803(7) 0.7480(9) 0.4806(8) 0.045(3) Uani 1 1 d . . . H32 H 0.0262 0.7485 0.4848 0.054 Uiso 1 1 calc R . . C33 C 0.1225(8) 0.8417(9) 0.4885(8) 0.048(3) Uani 1 1 d . . . H33 H 0.0973 0.9064 0.4996 0.058 Uiso 1 1 calc R . . C34 C 0.2034(7) 0.8399(9) 0.4798(8) 0.042(3) Uani 1 1 d . . . H34 H 0.2331 0.9028 0.4837 0.051 Uiso 1 1 calc R . . C35 C 0.2369(7) 0.7418(10) 0.4654(7) 0.039(3) Uani 1 1 d . . . H35 H 0.2909 0.7400 0.4602 0.047 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 0.02693(19) 0.02767(18) 0.0343(2) 0.0004(2) -0.0008(2) -0.00018(15) Li 0.043(11) 0.017(9) 0.046(12) 0.003(7) 0.006(9) 0.006(7) I1 0.0401(4) 0.0410(4) 0.0374(4) -0.0009(4) -0.0003(4) -0.0011(3) I2 0.0336(4) 0.0407(4) 0.0394(4) 0.0011(4) -0.0003(3) -0.0019(3) O1 0.025(3) 0.019(3) 0.037(3) -0.001(2) 0.001(2) -0.001(2) O2 0.024(3) 0.018(3) 0.048(3) 0.000(2) -0.006(2) 0.000(2) N1 0.024(4) 0.027(4) 0.050(8) 0.005(4) 0.001(4) 0.000(4) N2 0.039(5) 0.030(5) 0.034(6) 0.004(4) 0.003(5) 0.001(4) N3 0.024(4) 0.044(5) 0.032(5) -0.012(6) -0.011(5) 0.004(4) N4 0.040(5) 0.031(5) 0.033(7) -0.002(4) 0.007(4) -0.006(4) N5 0.023(4) 0.047(6) 0.026(7) 0.006(4) -0.007(4) -0.003(4) N6 0.042(6) 0.040(6) 0.040(6) -0.003(5) -0.003(5) -0.010(5) N7 0.032(5) 0.045(6) 0.047(7) -0.001(5) 0.004(5) 0.001(5) C1 0.044(7) 0.037(7) 0.047(8) 0.006(6) -0.005(6) -0.009(5) C2 0.052(8) 0.047(8) 0.053(9) 0.014(7) -0.011(6) 0.002(6) C3 0.049(9) 0.048(8) 0.081(12) -0.008(9) -0.008(8) -0.002(7) C4 0.042(8) 0.037(8) 0.073(11) -0.007(7) -0.008(7) 0.002(6) C5 0.047(8) 0.039(7) 0.046(8) -0.010(6) 0.004(6) 0.006(6) C6 0.040(7) 0.022(6) 0.043(8) 0.002(5) -0.001(6) -0.006(5) C7 0.038(7) 0.039(7) 0.043(8) -0.004(6) -0.006(6) -0.006(5) C8 0.019(6) 0.053(8) 0.072(10) -0.005(7) -0.009(6) 0.019(6) C9 0.039(8) 0.033(7) 0.049(8) -0.004(6) 0.005(7) 0.002(5) C10 0.040(7) 0.028(6) 0.035(7) -0.007(5) -0.001(6) 0.007(5) C11 0.045(7) 0.041(7) 0.037(8) -0.003(6) -0.001(6) -0.004(6) C12 0.037(7) 0.025(6) 0.059(9) 0.008(6) -0.005(6) 0.001(5) C13 0.021(5) 0.034(6) 0.112(18) 0.000(8) 0.000(8) -0.002(5) C14 0.034(7) 0.037(7) 0.047(8) -0.011(6) -0.007(6) -0.011(5) C15 0.022(6) 0.047(7) 0.043(8) 0.012(6) 0.000(5) -0.001(5) C16 0.046(7) 0.023(6) 0.050(9) -0.012(5) 0.005(6) -0.003(5) C17 0.037(7) 0.040(7) 0.038(8) 0.004(5) -0.007(5) -0.007(5) C18 0.036(7) 0.026(6) 0.057(9) 0.001(5) -0.006(6) 0.012(5) C19 0.038(8) 0.034(7) 0.054(9) -0.004(6) 0.012(7) -0.004(6) C20 0.031(6) 0.027(6) 0.049(8) -0.004(5) -0.006(6) 0.006(5) C21 0.038(7) 0.051(7) 0.031(7) 0.004(5) 0.004(5) -0.001(5) C22 0.050(8) 0.040(7) 0.049(8) -0.009(6) -0.007(6) -0.001(6) C23 0.069(10) 0.033(7) 0.063(10) -0.009(7) 0.001(8) -0.021(7) C24 0.070(10) 0.025(7) 0.067(10) 0.010(6) 0.000(7) -0.006(7) C25 0.043(7) 0.045(7) 0.031(7) -0.002(6) 0.002(5) 0.003(6) C26 0.057(8) 0.033(6) 0.051(8) 0.001(6) -0.002(7) 0.015(6) C27 0.041(7) 0.048(8) 0.060(9) -0.007(6) 0.009(6) -0.022(6) C28 0.060(9) 0.035(7) 0.086(13) 0.011(7) -0.003(8) 0.007(6) C29 0.069(11) 0.043(8) 0.056(10) -0.002(6) -0.006(7) 0.011(7) C30 0.039(7) 0.032(6) 0.043(8) 0.006(6) 0.002(6) 0.008(5) C31 0.046(7) 0.027(6) 0.053(9) -0.005(5) -0.002(6) -0.006(5) C32 0.030(6) 0.048(7) 0.056(8) -0.003(7) -0.001(6) 0.001(5) C33 0.063(9) 0.031(6) 0.051(8) -0.002(7) -0.003(7) 0.011(5) C34 0.052(8) 0.026(6) 0.048(8) 0.005(6) 0.004(6) -0.001(5) C35 0.025(6) 0.047(8) 0.045(8) 0.007(6) -0.005(5) -0.002(5) _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 1.750(10) . ? U O1 1.881(9) . ? U N2 2.589(9) . ? U N1 2.589(8) . ? U N4 2.595(10) . ? U N5 2.619(9) . ? U N3 2.652(8) . ? U Li 3.78(2) . ? Li O1 1.90(2) . ? Li N7 2.04(2) . ? Li N6 2.16(2) . ? Li I1 2.87(2) . ? N1 C5 1.337(15) . ? N1 C1 1.351(15) . ? N2 C10 1.321(15) . ? N2 C6 1.353(16) . ? N3 C15 1.307(18) . ? N3 C11 1.344(18) . ? N4 C20 1.335(15) . ? N4 C16 1.342(15) . ? N5 C25 1.328(14) . ? N5 C21 1.335(14) . ? N6 C30 1.329(16) . ? N6 C26 1.332(16) . ? N7 C35 1.340(16) . ? N7 C31 1.368(15) . ? C1 C2 1.414(18) . ? C1 H1 0.9300 . ? C2 C3 1.35(2) . ? C2 H2 0.9300 . ? C3 C4 1.36(2) . ? C3 H3 0.9300 . ? C4 C5 1.400(19) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.377(16) . ? C6 H6 0.9300 . ? C7 C8 1.362(18) . ? C7 H7 0.9300 . ? C8 C9 1.379(18) . ? C8 H8 0.9300 . ? C9 C10 1.393(17) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.391(18) . ? C11 H11 0.9300 . ? C12 C13 1.41(3) . ? C12 H12 0.9300 . ? C13 C14 1.33(3) . ? C13 H13 0.9300 . ? C14 C15 1.377(18) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.376(16) . ? C16 H16 0.9300 . ? C17 C18 1.361(18) . ? C17 H17 0.9300 . ? C18 C19 1.345(18) . ? C18 H18 0.9300 . ? C19 C20 1.395(17) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.372(17) . ? C21 H21 0.9300 . ? C22 C23 1.41(2) . ? C22 H22 0.9300 . ? C23 C24 1.38(2) . ? C23 H23 0.9300 . ? C24 C25 1.384(19) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.408(17) . ? C26 H26 0.9300 . ? C27 C28 1.392(19) . ? C27 H27 0.9300 . ? C28 C29 1.38(2) . ? C28 H28 0.9300 . ? C29 C30 1.354(19) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.357(16) . ? C31 H31 0.9300 . ? C32 C33 1.370(17) . ? C32 H32 0.9300 . ? C33 C34 1.395(17) . ? C33 H33 0.9300 . ? C34 C35 1.365(17) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? 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 O1 179.6(3) . . ? O2 U N2 89.4(3) . . ? O1 U N2 90.3(3) . . ? O2 U N1 92.8(3) . . ? O1 U N1 86.9(3) . . ? N2 U N1 72.2(3) . . ? O2 U N4 88.7(3) . . ? O1 U N4 91.7(3) . . ? N2 U N4 146.2(3) . . ? N1 U N4 141.6(3) . . ? O2 U N5 86.8(3) . . ? O1 U N5 93.4(3) . . ? N2 U N5 142.7(3) . . ? N1 U N5 71.0(2) . . ? N4 U N5 70.8(3) . . ? O2 U N3 88.5(4) . . ? O1 U N3 91.6(4) . . ? N2 U N3 72.8(2) . . ? N1 U N3 144.9(2) . . ? N4 U N3 73.4(2) . . ? N5 U N3 144.0(2) . . ? O1 Li N7 108.1(9) . . ? O1 Li N6 109.6(10) . . ? N7 Li N6 113.7(10) . . ? O1 Li I1 111.1(9) . . ? N7 Li I1 111.1(9) . . ? N6 Li I1 103.2(7) . . ? U O1 Li 174.3(6) . . ? C5 N1 C1 116.4(11) . . ? C5 N1 U 122.6(8) . . ? C1 N1 U 120.5(8) . . ? C10 N2 C6 118.8(11) . . ? C10 N2 U 121.8(8) . . ? C6 N2 U 118.1(7) . . ? C15 N3 C11 117.2(10) . . ? C15 N3 U 124.3(10) . . ? C11 N3 U 118.5(8) . . ? C20 N4 C16 118.3(11) . . ? C20 N4 U 121.1(7) . . ? C16 N4 U 120.2(7) . . ? C25 N5 C21 117.3(10) . . ? C25 N5 U 123.8(7) . . ? C21 N5 U 118.8(7) . . ? C30 N6 C26 115.9(11) . . ? C30 N6 Li 118.4(10) . . ? C26 N6 Li 125.3(10) . . ? C35 N7 C31 115.1(10) . . ? C35 N7 Li 119.2(10) . . ? C31 N7 Li 124.7(10) . . ? N1 C1 C2 123.5(13) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C3 C2 C1 116.2(14) . . ? C3 C2 H2 121.9 . . ? C1 C2 H2 121.9 . . ? C2 C3 C4 123.4(15) . . ? C2 C3 H3 118.3 . . ? C4 C3 H3 118.3 . . ? C3 C4 C5 116.5(14) . . ? C3 C4 H4 121.8 . . ? C5 C4 H4 121.8 . . ? N1 C5 C4 124.0(14) . . ? N1 C5 H5 118.0 . . ? C4 C5 H5 118.0 . . ? N2 C6 C7 121.4(12) . . ? N2 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C8 C7 C6 118.9(12) . . ? C8 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C7 C8 C9 120.9(12) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C8 C9 C10 116.8(13) . . ? C8 C9 H9 121.6 . . ? C10 C9 H9 121.6 . . ? N2 C10 C9 123.2(13) . . ? N2 C10 H10 118.4 . . ? C9 C10 H10 118.4 . . ? N3 C11 C12 123.7(12) . . ? N3 C11 H11 118.2 . . ? C12 C11 H11 118.2 . . ? C11 C12 C13 115.3(13) . . ? C11 C12 H12 122.4 . . ? C13 C12 H12 122.4 . . ? C14 C13 C12 121.2(11) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 118.3(13) . . ? C13 C14 H14 120.9 . . ? C15 C14 H14 120.9 . . ? N3 C15 C14 124.3(13) . . ? N3 C15 H15 117.9 . . ? C14 C15 H15 117.9 . . ? N4 C16 C17 123.3(12) . . ? N4 C16 H16 118.4 . . ? C17 C16 H16 118.4 . . ? C18 C17 C16 116.8(12) . . ? C18 C17 H17 121.6 . . ? C16 C17 H17 121.6 . . ? C19 C18 C17 121.9(12) . . ? C19 C18 H18 119.1 . . ? C17 C18 H18 119.1 . . ? C18 C19 C20 118.4(12) . . ? C18 C19 H19 120.8 . . ? C20 C19 H19 120.8 . . ? N4 C20 C19 121.3(12) . . ? N4 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? N5 C21 C22 123.5(12) . . ? N5 C21 H21 118.2 . . ? C22 C21 H21 118.2 . . ? C21 C22 C23 118.4(13) . . ? C21 C22 H22 120.8 . . ? C23 C22 H22 120.8 . . ? C24 C23 C22 118.4(11) . . ? C24 C23 H23 120.8 . . ? C22 C23 H23 120.8 . . ? C23 C24 C25 118.2(12) . . ? C23 C24 H24 120.9 . . ? C25 C24 H24 120.9 . . ? N5 C25 C24 124.2(12) . . ? N5 C25 H25 117.9 . . ? C24 C25 H25 117.9 . . ? N6 C26 C27 124.6(11) . . ? N6 C26 H26 117.7 . . ? C27 C26 H26 117.7 . . ? C28 C27 C26 117.0(12) . . ? C28 C27 H27 121.5 . . ? C26 C27 H27 121.5 . . ? C29 C28 C27 118.0(13) . . ? C29 C28 H28 121.0 . . ? C27 C28 H28 121.0 . . ? C30 C29 C28 119.9(13) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? N6 C30 C29 124.5(13) . . ? N6 C30 H30 117.7 . . ? C29 C30 H30 117.7 . . ? C32 C31 N7 124.2(11) . . ? C32 C31 H31 117.9 . . ? N7 C31 H31 117.9 . . ? C31 C32 C33 118.4(11) . . ? C31 C32 H32 120.8 . . ? C33 C32 H32 120.8 . . ? C32 C33 C34 119.9(11) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C35 C34 C33 117.1(11) . . ? C35 C34 H34 121.5 . . ? C33 C34 H34 121.5 . . ? N7 C35 C34 125.3(11) . . ? N7 C35 H35 117.3 . . ? C34 C35 H35 117.3 . . ? #===END data_8 _database_code_depnum_ccdc_archive 'CCDC 711340' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H25 F9 Li2 N5 O11 S3 U' _chemical_formula_sum 'C28 H25 F9 Li2 N5 O11 S3 U' _chemical_formula_weight 1126.62 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' Li Li -0.0003 0.0001 '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 '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 21.6519(4) _cell_length_b 21.3781(6) _cell_length_c 19.0730(5) _cell_angle_alpha 90.00 _cell_angle_beta 111.162(2) _cell_angle_gamma 90.00 _cell_volume 8233.1(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 264858 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 25.68 _exptl_crystal_description parallelepiped _exptl_crystal_colour 'translucent light brown' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.818 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4344 _exptl_absorpt_coefficient_mu 4.194 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.454 _exptl_absorpt_correction_T_max 0.605 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 30 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 area-detector diffractometer' _diffrn_measurement_method 'two \f and four \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 264858 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0357 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 25.68 _reflns_number_total 15603 _reflns_number_gt 12270 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by Patterson map interpretation and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 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^)+(0.0386P)^2^+0.6886P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 15603 _refine_ls_number_parameters 1063 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0719 _refine_ls_wR_factor_gt 0.0670 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.131 _refine_diff_density_min -1.281 _refine_diff_density_rms 0.093 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 0.420358(6) 0.617743(6) 0.749929(7) 0.02653(5) Uani 1 1 d . . . U2 U -0.079363(6) 0.610754(6) 0.743479(7) 0.02594(5) Uani 1 1 d . . . Li1 Li 0.5936(3) 0.6133(3) 0.7512(4) 0.0360(15) Uani 1 1 d . . . Li2 Li 0.2497(3) 0.6190(3) 0.7532(4) 0.0299(14) Uani 1 1 d . . . Li3 Li 0.0922(3) 0.6065(3) 0.7447(4) 0.0344(15) Uani 1 1 d . . . Li4 Li -0.2475(3) 0.6217(3) 0.7513(4) 0.0348(15) Uani 1 1 d . . . S1 S 0.62251(5) 0.59857(5) 0.60521(5) 0.0360(2) Uani 1 1 d . . . S2 S 0.70710(4) 0.52414(5) 0.84842(6) 0.0343(2) Uani 1 1 d . . . S3 S 0.68679(4) 0.73311(4) 0.80085(5) 0.0334(2) Uani 1 1 d . . . S4 S 0.12572(4) 0.66463(4) 0.62002(5) 0.0307(2) Uani 1 1 d . . . S5 S 0.17470(4) 0.49170(4) 0.73738(5) 0.0295(2) Uani 1 1 d . . . S6 S 0.20134(4) 0.67948(4) 0.86932(5) 0.0289(2) Uani 1 1 d . . . O1 O 0.50586(13) 0.61477(12) 0.75188(16) 0.0368(6) Uani 1 1 d . . . O2 O 0.33589(12) 0.62119(12) 0.75125(14) 0.0328(6) Uani 1 1 d . . . O3 O 0.00553(12) 0.60336(12) 0.74451(14) 0.0331(6) Uani 1 1 d . . . O4 O -0.16413(12) 0.61649(12) 0.74314(15) 0.0359(7) Uani 1 1 d . . . O5 O 0.57952(14) 0.59853(16) 0.64866(17) 0.0566(8) Uani 1 1 d . . . O6 O 0.69081(14) 0.61134(13) 0.64942(17) 0.0467(7) Uani 1 1 d . . . O7 O 0.59614(17) 0.62923(15) 0.53491(17) 0.0589(9) Uani 1 1 d . . . O8 O 0.63858(12) 0.54328(14) 0.81421(16) 0.0493(8) Uani 1 1 d . . . O9 O 0.75126(13) 0.55620(13) 0.81860(16) 0.0429(7) Uani 1 1 d . . . O10 O 0.71753(15) 0.45913(14) 0.85937(19) 0.0566(8) Uani 1 1 d . . . O11 O 0.62680(12) 0.69592(13) 0.77724(17) 0.0458(7) Uani 1 1 d . . . O12 O 0.74427(12) 0.69893(13) 0.79939(16) 0.0419(7) Uani 1 1 d . . . O13 O 0.69747(14) 0.77056(13) 0.86581(16) 0.0462(7) Uani 1 1 d . . . O14 O 0.19163(11) 0.63814(12) 0.65032(14) 0.0323(6) Uani 1 1 d . . . O15 O 0.09546(12) 0.67204(13) 0.67596(16) 0.0419(7) Uani 1 1 d . . . O16 O 0.08388(14) 0.63982(14) 0.55017(16) 0.0471(7) Uani 1 1 d . . . O17 O 0.23100(11) 0.53279(12) 0.77155(15) 0.0361(6) Uani 1 1 d . . . O18 O 0.11152(11) 0.52427(12) 0.71224(14) 0.0338(6) Uani 1 1 d . . . O19 O 0.18275(13) 0.44623(12) 0.68626(15) 0.0404(7) Uani 1 1 d . . . O20 O 0.24699(11) 0.67820(12) 0.82959(14) 0.0342(6) Uani 1 1 d . . . O21 O 0.14880(12) 0.63358(12) 0.84237(15) 0.0355(6) Uani 1 1 d . . . O22 O 0.18080(12) 0.74027(12) 0.88337(14) 0.0369(6) Uani 1 1 d . . . N1 N 0.44662(14) 0.53132(14) 0.85143(16) 0.0295(7) Uani 1 1 d . . . N2 N 0.46535(14) 0.67503(14) 0.87848(17) 0.0331(7) Uani 1 1 d . . . N3 N 0.41407(14) 0.73680(14) 0.72487(18) 0.0333(7) Uani 1 1 d . . . N4 N 0.37291(14) 0.63396(14) 0.60506(17) 0.0317(7) Uani 1 1 d . . . N5 N 0.39940(14) 0.50956(14) 0.68614(17) 0.0312(7) Uani 1 1 d . . . N6 N -0.08435(14) 0.49025(14) 0.76012(16) 0.0314(7) Uani 1 1 d . . . N7 N -0.03193(14) 0.58968(14) 0.88730(16) 0.0299(7) Uani 1 1 d . . . N8 N -0.05349(14) 0.71726(14) 0.81126(16) 0.0304(7) Uani 1 1 d . . . N9 N -0.11270(14) 0.69437(15) 0.63802(17) 0.0333(7) Uani 1 1 d . . . N10 N -0.11760(14) 0.55559(15) 0.61404(17) 0.0328(7) Uani 1 1 d . . . F1 F 0.64975(16) 0.48286(14) 0.64467(17) 0.0775(9) Uani 1 1 d . . . F2 F 0.56354(12) 0.49577(14) 0.54371(18) 0.0750(9) Uani 1 1 d . . . F3 F 0.65955(12) 0.50713(12) 0.53932(14) 0.0529(6) Uani 1 1 d . . . F4 F 0.79333(14) 0.5436(2) 0.98133(16) 0.0997(13) Uani 1 1 d . . . F5 F 0.69482(14) 0.53072(15) 0.97891(15) 0.0709(8) Uani 1 1 d . . . F6 F 0.72118(19) 0.61762(14) 0.94003(19) 0.0844(10) Uani 1 1 d . . . F7 F 0.72208(13) 0.82807(12) 0.73924(15) 0.0607(7) Uani 1 1 d . . . F8 F 0.66362(14) 0.75862(13) 0.65979(14) 0.0645(8) Uani 1 1 d . . . F9 F 0.61746(12) 0.82234(12) 0.71391(15) 0.0571(7) Uani 1 1 d . . . F10 F 0.08526(12) 0.77789(12) 0.57416(15) 0.0598(7) Uani 1 1 d . . . F11 F 0.16821(13) 0.74619(12) 0.54693(15) 0.0644(8) Uani 1 1 d . . . F12 F 0.18297(12) 0.77364(11) 0.66003(15) 0.0567(7) Uani 1 1 d . . . F13 F 0.12600(12) 0.40161(12) 0.79484(14) 0.0560(7) Uani 1 1 d . . . F14 F 0.22970(12) 0.41935(12) 0.85432(14) 0.0545(7) Uani 1 1 d . . . F15 F 0.15657(13) 0.48278(12) 0.86513(13) 0.0562(7) Uani 1 1 d . . . F16 F 0.28018(12) 0.59523(12) 0.95613(14) 0.0575(7) Uani 1 1 d . . . F17 F 0.21419(12) 0.63818(12) 1.00314(13) 0.0501(6) Uani 1 1 d . . . F18 F 0.29853(11) 0.68881(12) 0.99931(13) 0.0547(7) Uani 1 1 d . . . C1 C 0.62381(19) 0.5172(2) 0.5822(2) 0.0421(10) Uani 1 1 d . . . C2 C 0.7304(2) 0.5559(3) 0.9421(3) 0.0559(13) Uani 1 1 d . . . C3 C 0.67159(19) 0.7885(2) 0.7246(2) 0.0431(10) Uani 1 1 d . . . C4 C 0.1413(2) 0.7450(2) 0.5994(2) 0.0430(10) Uani 1 1 d . . . C5 C 0.17162(19) 0.44659(19) 0.8170(2) 0.0385(9) Uani 1 1 d . . . C6 C 0.25095(19) 0.6486(2) 0.9616(2) 0.0382(9) Uani 1 1 d . . . C7 C 0.39720(18) 0.50584(18) 0.8691(2) 0.0330(8) Uani 1 1 d . . . H7 H 0.3554 0.5240 0.8501 0.040 Uiso 1 1 calc R . . C8 C 0.40663(19) 0.45349(18) 0.9147(2) 0.0384(9) Uani 1 1 d . . . H8 H 0.3714 0.4369 0.9257 0.046 Uiso 1 1 calc R . . C9 C 0.4684(2) 0.42614(19) 0.9438(2) 0.0426(10) Uani 1 1 d . . . H9 H 0.4757 0.3911 0.9746 0.051 Uiso 1 1 calc R . . C10 C 0.51927(19) 0.45269(18) 0.9256(2) 0.0375(9) Uani 1 1 d . . . H10 H 0.5616 0.4356 0.9444 0.045 Uiso 1 1 calc R . . C11 C 0.50663(17) 0.50436(18) 0.8796(2) 0.0330(8) Uani 1 1 d . . . H11 H 0.5411 0.5214 0.8675 0.040 Uiso 1 1 calc R . . C12 C 0.42652(18) 0.68514(17) 0.9189(2) 0.0337(9) Uani 1 1 d . . . H12 H 0.3835 0.6696 0.9008 0.040 Uiso 1 1 calc R . . C13 C 0.44790(18) 0.71745(18) 0.9856(2) 0.0391(9) Uani 1 1 d . . . H13 H 0.4200 0.7228 1.0126 0.047 Uiso 1 1 calc R . . C14 C 0.51142(19) 0.74206(19) 1.0124(2) 0.0416(10) Uani 1 1 d . . . H14 H 0.5268 0.7648 1.0569 0.050 Uiso 1 1 calc R . . C15 C 0.55118(19) 0.73184(19) 0.9711(2) 0.0418(10) Uani 1 1 d . . . H15 H 0.5941 0.7476 0.9876 0.050 Uiso 1 1 calc R . . C16 C 0.52713(18) 0.69832(19) 0.9055(2) 0.0381(9) Uani 1 1 d . . . H16 H 0.5547 0.6914 0.8786 0.046 Uiso 1 1 calc R . . C17 C 0.46538(18) 0.76938(18) 0.7202(2) 0.0370(9) Uani 1 1 d . . . H17 H 0.5042 0.7481 0.7252 0.044 Uiso 1 1 calc R . . C18 C 0.4631(2) 0.83305(19) 0.7085(3) 0.0454(10) Uani 1 1 d . . . H18 H 0.4999 0.8542 0.7064 0.055 Uiso 1 1 calc R . . C19 C 0.4055(2) 0.8650(2) 0.6999(3) 0.0485(11) Uani 1 1 d . . . H19 H 0.4026 0.9079 0.6915 0.058 Uiso 1 1 calc R . . C20 C 0.3526(2) 0.8323(2) 0.7039(3) 0.0529(12) Uani 1 1 d . . . H20 H 0.3131 0.8526 0.6979 0.063 Uiso 1 1 calc R . . C21 C 0.35871(19) 0.76859(19) 0.7169(3) 0.0439(10) Uani 1 1 d . . . H21 H 0.3227 0.7468 0.7202 0.053 Uiso 1 1 calc R . . C22 C 0.41092(19) 0.63088(17) 0.5632(2) 0.0355(9) Uani 1 1 d . . . H22 H 0.4557 0.6218 0.5867 0.043 Uiso 1 1 calc R . . C23 C 0.3864(2) 0.64052(18) 0.4872(2) 0.0416(10) Uani 1 1 d . . . H23 H 0.4143 0.6379 0.4599 0.050 Uiso 1 1 calc R . . C24 C 0.3206(2) 0.65397(19) 0.4514(2) 0.0459(10) Uani 1 1 d . . . H24 H 0.3032 0.6612 0.3999 0.055 Uiso 1 1 calc R . . C25 C 0.2806(2) 0.65659(19) 0.4941(2) 0.0424(10) Uani 1 1 d . . . H25 H 0.2356 0.6652 0.4716 0.051 Uiso 1 1 calc R . . C26 C 0.30828(18) 0.64629(18) 0.5694(2) 0.0369(9) Uani 1 1 d . . . H26 H 0.2811 0.6479 0.5976 0.044 Uiso 1 1 calc R . . C27 C 0.44425(18) 0.48274(18) 0.6629(2) 0.0357(9) Uani 1 1 d . . . H27 H 0.4837 0.5039 0.6706 0.043 Uiso 1 1 calc R . . C28 C 0.4348(2) 0.42526(19) 0.6280(2) 0.0416(10) Uani 1 1 d . . . H28 H 0.4674 0.4079 0.6129 0.050 Uiso 1 1 calc R . . C29 C 0.3760(2) 0.39379(19) 0.6160(2) 0.0434(10) Uani 1 1 d . . . H29 H 0.3680 0.3551 0.5921 0.052 Uiso 1 1 calc R . . C30 C 0.3295(2) 0.42102(18) 0.6401(2) 0.0394(9) Uani 1 1 d . . . H30 H 0.2898 0.4006 0.6332 0.047 Uiso 1 1 calc R . . C31 C 0.34225(18) 0.47874(18) 0.6746(2) 0.0344(9) Uani 1 1 d . . . H31 H 0.3105 0.4970 0.6903 0.041 Uiso 1 1 calc R . . C32 C -0.13944(19) 0.4630(2) 0.7621(2) 0.0409(10) Uani 1 1 d . . . H32 H -0.1729 0.4883 0.7663 0.049 Uiso 1 1 calc R . . C33 C -0.1488(2) 0.3991(2) 0.7582(2) 0.0484(11) Uani 1 1 d . . . H33 H -0.1881 0.3820 0.7591 0.058 Uiso 1 1 calc R . . C34 C -0.0991(2) 0.3605(2) 0.7528(2) 0.0501(11) Uani 1 1 d . . . H34 H -0.1044 0.3173 0.7497 0.060 Uiso 1 1 calc R . . C35 C -0.0417(2) 0.38810(19) 0.7524(3) 0.0473(11) Uani 1 1 d . . . H35 H -0.0071 0.3636 0.7497 0.057 Uiso 1 1 calc R . . C36 C -0.03603(19) 0.45266(18) 0.7559(2) 0.0383(9) Uani 1 1 d . . . H36 H 0.0028 0.4708 0.7552 0.046 Uiso 1 1 calc R . . C37 C -0.07182(19) 0.58859(18) 0.9276(2) 0.0359(9) Uani 1 1 d . . . H37 H -0.1174 0.5914 0.9024 0.043 Uiso 1 1 calc R . . C38 C -0.0473(2) 0.58346(19) 1.0049(2) 0.0409(10) Uani 1 1 d . . . H38 H -0.0761 0.5830 1.0311 0.049 Uiso 1 1 calc R . . C39 C 0.0196(2) 0.57908(19) 1.0430(2) 0.0416(10) Uani 1 1 d . . . H39 H 0.0367 0.5758 1.0951 0.050 Uiso 1 1 calc R . . C40 C 0.06134(19) 0.57966(18) 1.0024(2) 0.0381(9) Uani 1 1 d . . . H40 H 0.1070 0.5764 1.0267 0.046 Uiso 1 1 calc R . . C41 C 0.03376(17) 0.58513(18) 0.9250(2) 0.0348(9) Uani 1 1 d . . . H41 H 0.0618 0.5857 0.8979 0.042 Uiso 1 1 calc R . . C42 C -0.10216(19) 0.75423(18) 0.8159(2) 0.0374(9) Uani 1 1 d . . . H42 H -0.1458 0.7415 0.7915 0.045 Uiso 1 1 calc R . . C43 C -0.09104(19) 0.81005(19) 0.8550(2) 0.0401(9) Uani 1 1 d . . . H43 H -0.1261 0.8346 0.8562 0.048 Uiso 1 1 calc R . . C44 C -0.0262(2) 0.82815(19) 0.8922(2) 0.0408(10) Uani 1 1 d . . . H44 H -0.0169 0.8651 0.9199 0.049 Uiso 1 1 calc R . . C45 C 0.02447(19) 0.79147(19) 0.8883(2) 0.0378(9) Uani 1 1 d . . . H45 H 0.0683 0.8033 0.9131 0.045 Uiso 1 1 calc R . . C46 C 0.00961(17) 0.73723(18) 0.8475(2) 0.0331(8) Uani 1 1 d . . . H46 H 0.0442 0.7130 0.8445 0.040 Uiso 1 1 calc R . . C47 C -0.06846(18) 0.71570(19) 0.6089(2) 0.0397(9) Uani 1 1 d . . . H47 H -0.0239 0.7062 0.6337 0.048 Uiso 1 1 calc R . . C48 C -0.0863(2) 0.7509(2) 0.5441(2) 0.0472(11) Uani 1 1 d . . . H48 H -0.0545 0.7649 0.5254 0.057 Uiso 1 1 calc R . . C49 C -0.1523(2) 0.7650(2) 0.5077(3) 0.0556(12) Uani 1 1 d . . . H49 H -0.1657 0.7883 0.4635 0.067 Uiso 1 1 calc R . . C50 C -0.1978(2) 0.7445(2) 0.5366(3) 0.0534(12) Uani 1 1 d . . . H50 H -0.2425 0.7537 0.5127 0.064 Uiso 1 1 calc R . . C51 C -0.17655(18) 0.7100(2) 0.6018(2) 0.0415(10) Uani 1 1 d . . . H51 H -0.2077 0.6969 0.6218 0.050 Uiso 1 1 calc R . . C52 C -0.0750(2) 0.5391(2) 0.5806(2) 0.0518(12) Uani 1 1 d . . . H52 H -0.0309 0.5508 0.6034 0.062 Uiso 1 1 calc R . . C53 C -0.0933(2) 0.5059(3) 0.5148(3) 0.0631(15) Uani 1 1 d . . . H53 H -0.0623 0.4960 0.4931 0.076 Uiso 1 1 calc R . . C54 C -0.1583(2) 0.4875(2) 0.4812(2) 0.0492(11) Uani 1 1 d . . . H54 H -0.1720 0.4645 0.4368 0.059 Uiso 1 1 calc R . . C55 C -0.20241(19) 0.5038(2) 0.5147(2) 0.0416(10) Uani 1 1 d . . . H55 H -0.2467 0.4921 0.4933 0.050 Uiso 1 1 calc R . . C56 C -0.18047(18) 0.53754(19) 0.5800(2) 0.0369(9) Uani 1 1 d . . . H56 H -0.2110 0.5485 0.6018 0.044 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 0.01967(7) 0.02687(8) 0.03315(9) 0.00126(6) 0.00966(6) -0.00010(5) U2 0.02069(8) 0.03161(8) 0.02694(8) -0.00116(6) 0.01030(6) -0.00098(5) Li1 0.030(3) 0.035(4) 0.040(4) 0.002(3) 0.009(3) 0.006(3) Li2 0.030(3) 0.026(3) 0.032(3) -0.003(3) 0.009(3) -0.002(2) Li3 0.028(3) 0.036(4) 0.037(4) 0.003(3) 0.009(3) 0.000(3) Li4 0.032(4) 0.038(4) 0.036(4) -0.003(3) 0.014(3) 0.002(3) S1 0.0328(5) 0.0407(6) 0.0327(5) -0.0033(4) 0.0096(4) 0.0056(4) S2 0.0308(5) 0.0332(5) 0.0391(6) 0.0037(4) 0.0128(4) -0.0011(4) S3 0.0300(5) 0.0315(5) 0.0390(6) -0.0023(4) 0.0128(4) -0.0007(4) S4 0.0249(4) 0.0336(5) 0.0329(5) 0.0057(4) 0.0096(4) 0.0018(4) S5 0.0284(5) 0.0278(5) 0.0340(5) -0.0013(4) 0.0132(4) -0.0008(4) S6 0.0254(4) 0.0315(5) 0.0288(5) -0.0042(4) 0.0085(4) -0.0005(4) O1 0.0280(14) 0.0376(16) 0.0455(17) 0.0025(12) 0.0140(12) 0.0010(11) O2 0.0260(14) 0.0350(16) 0.0370(15) -0.0004(11) 0.0108(12) -0.0006(11) O3 0.0265(13) 0.0415(16) 0.0323(14) -0.0004(12) 0.0119(11) 0.0005(11) O4 0.0271(14) 0.0457(18) 0.0352(16) 0.0000(12) 0.0115(12) -0.0003(11) O5 0.0420(17) 0.082(2) 0.053(2) -0.0171(17) 0.0254(15) 0.0018(16) O6 0.0364(16) 0.0511(19) 0.0480(18) -0.0114(14) 0.0095(13) -0.0021(13) O7 0.085(2) 0.0508(19) 0.0336(17) 0.0004(14) 0.0124(16) 0.0206(17) O8 0.0299(14) 0.061(2) 0.0547(19) 0.0114(15) 0.0127(13) 0.0039(14) O9 0.0406(15) 0.0454(17) 0.0498(18) 0.0038(14) 0.0250(14) -0.0046(13) O10 0.0581(19) 0.0331(17) 0.075(2) 0.0081(16) 0.0198(17) -0.0026(14) O11 0.0295(14) 0.0417(17) 0.067(2) 0.0013(15) 0.0186(14) -0.0041(12) O12 0.0284(14) 0.0422(17) 0.0554(18) -0.0064(14) 0.0153(13) 0.0016(12) O13 0.0583(18) 0.0373(16) 0.0434(17) -0.0044(13) 0.0188(14) 0.0088(14) O14 0.0248(13) 0.0390(15) 0.0337(15) 0.0030(12) 0.0113(11) 0.0063(11) O15 0.0377(15) 0.0452(17) 0.0524(18) 0.0124(14) 0.0277(14) 0.0099(13) O16 0.0432(16) 0.0443(18) 0.0411(17) -0.0015(14) 0.0001(13) -0.0015(14) O17 0.0270(13) 0.0331(15) 0.0441(16) 0.0024(12) 0.0078(12) -0.0033(11) O18 0.0254(13) 0.0345(15) 0.0389(15) -0.0024(12) 0.0085(11) 0.0030(11) O19 0.0483(16) 0.0342(15) 0.0461(17) -0.0059(13) 0.0259(14) 0.0012(13) O20 0.0297(13) 0.0412(16) 0.0361(15) -0.0044(12) 0.0173(12) -0.0049(11) O21 0.0289(14) 0.0375(15) 0.0389(16) -0.0078(12) 0.0108(12) -0.0059(12) O22 0.0349(14) 0.0325(15) 0.0394(16) -0.0034(12) 0.0089(12) 0.0051(12) N1 0.0270(15) 0.0307(17) 0.0284(17) 0.0026(13) 0.0070(13) 0.0031(13) N2 0.0301(17) 0.0306(17) 0.0352(18) -0.0014(14) 0.0077(14) -0.0021(13) N3 0.0280(16) 0.0292(17) 0.0409(19) 0.0018(14) 0.0102(14) -0.0004(13) N4 0.0296(16) 0.0292(17) 0.0370(19) 0.0028(14) 0.0130(14) -0.0003(13) N5 0.0322(16) 0.0292(17) 0.0328(18) 0.0019(14) 0.0124(14) 0.0005(13) N6 0.0312(16) 0.0340(18) 0.0306(17) -0.0028(13) 0.0131(14) -0.0029(14) N7 0.0329(17) 0.0298(17) 0.0277(17) -0.0006(13) 0.0116(13) -0.0033(13) N8 0.0275(16) 0.0308(17) 0.0325(17) -0.0001(13) 0.0104(13) 0.0006(13) N9 0.0271(16) 0.0385(19) 0.0327(18) 0.0009(14) 0.0088(13) 0.0033(14) N10 0.0320(17) 0.0370(19) 0.0313(18) -0.0027(14) 0.0135(14) 0.0004(14) F1 0.100(2) 0.0586(19) 0.064(2) 0.0212(15) 0.0171(17) 0.0043(17) F2 0.0417(15) 0.074(2) 0.103(2) -0.0419(18) 0.0181(15) -0.0184(14) F3 0.0595(16) 0.0459(15) 0.0616(17) -0.0108(13) 0.0319(14) 0.0045(12) F4 0.0603(19) 0.183(4) 0.0397(17) 0.012(2) -0.0008(14) -0.020(2) F5 0.086(2) 0.087(2) 0.0543(17) 0.0153(15) 0.0429(16) -0.0022(17) F6 0.137(3) 0.0490(19) 0.079(2) -0.0067(16) 0.053(2) -0.0187(18) F7 0.0627(17) 0.0467(16) 0.0753(19) 0.0052(13) 0.0281(14) -0.0178(13) F8 0.0819(19) 0.0664(19) 0.0426(16) -0.0087(14) 0.0192(14) 0.0021(15) F9 0.0555(16) 0.0450(15) 0.0649(18) 0.0117(13) 0.0146(13) 0.0166(12) F10 0.0598(16) 0.0428(15) 0.0784(19) 0.0223(13) 0.0269(14) 0.0164(13) F11 0.0833(19) 0.0581(17) 0.0743(19) 0.0165(14) 0.0554(16) -0.0020(15) F12 0.0541(15) 0.0406(15) 0.0747(19) -0.0132(13) 0.0223(14) -0.0093(12) F13 0.0607(16) 0.0501(15) 0.0602(17) 0.0043(13) 0.0256(13) -0.0232(13) F14 0.0506(15) 0.0541(16) 0.0542(16) 0.0213(13) 0.0132(12) 0.0112(12) F15 0.0721(17) 0.0637(17) 0.0418(15) 0.0020(13) 0.0316(13) 0.0075(14) F16 0.0624(17) 0.0553(16) 0.0504(16) 0.0069(13) 0.0150(13) 0.0260(14) F17 0.0560(15) 0.0618(16) 0.0364(14) 0.0054(12) 0.0216(12) 0.0030(13) F18 0.0445(14) 0.0644(17) 0.0407(14) -0.0038(12) -0.0021(11) -0.0101(13) C1 0.034(2) 0.046(3) 0.044(3) -0.007(2) 0.0114(19) -0.0012(19) C2 0.061(3) 0.075(4) 0.036(3) 0.010(2) 0.023(2) -0.009(3) C3 0.040(2) 0.038(2) 0.048(3) -0.001(2) 0.0115(19) -0.0029(19) C4 0.043(2) 0.040(2) 0.051(3) 0.004(2) 0.024(2) 0.001(2) C5 0.039(2) 0.039(2) 0.038(2) -0.0018(18) 0.0144(18) -0.0033(19) C6 0.035(2) 0.042(2) 0.038(2) 0.0015(19) 0.0129(18) 0.0052(19) C7 0.0291(19) 0.039(2) 0.032(2) 0.0029(17) 0.0121(16) 0.0009(17) C8 0.043(2) 0.036(2) 0.038(2) 0.0030(18) 0.0167(19) -0.0036(18) C9 0.059(3) 0.032(2) 0.036(2) 0.0070(18) 0.016(2) 0.004(2) C10 0.040(2) 0.036(2) 0.034(2) 0.0020(18) 0.0112(18) 0.0140(18) C11 0.030(2) 0.036(2) 0.033(2) -0.0032(17) 0.0113(16) 0.0011(16) C12 0.0268(19) 0.031(2) 0.042(2) -0.0033(17) 0.0111(17) 0.0011(16) C13 0.036(2) 0.034(2) 0.048(3) -0.0071(19) 0.0164(19) 0.0028(17) C14 0.044(2) 0.033(2) 0.043(2) -0.0105(18) 0.0094(19) -0.0027(18) C15 0.033(2) 0.040(2) 0.046(3) -0.007(2) 0.0077(19) -0.0105(18) C16 0.032(2) 0.039(2) 0.044(2) 0.0029(19) 0.0142(18) -0.0014(18) C17 0.033(2) 0.033(2) 0.046(2) 0.0051(18) 0.0160(18) 0.0010(17) C18 0.038(2) 0.036(2) 0.067(3) 0.007(2) 0.025(2) -0.0016(19) C19 0.044(3) 0.031(2) 0.071(3) 0.011(2) 0.021(2) 0.0005(19) C20 0.039(2) 0.034(2) 0.088(4) 0.009(2) 0.027(2) 0.0075(19) C21 0.034(2) 0.033(2) 0.069(3) 0.007(2) 0.023(2) 0.0047(18) C22 0.035(2) 0.028(2) 0.047(3) -0.0004(18) 0.0194(19) -0.0030(17) C23 0.054(3) 0.035(2) 0.043(3) -0.0040(18) 0.027(2) -0.0083(19) C24 0.066(3) 0.034(2) 0.034(2) 0.0030(18) 0.013(2) -0.003(2) C25 0.044(2) 0.035(2) 0.042(2) 0.0047(19) 0.0083(19) 0.0050(19) C26 0.032(2) 0.038(2) 0.041(2) 0.0061(18) 0.0137(18) 0.0079(17) C27 0.032(2) 0.040(2) 0.036(2) -0.0025(18) 0.0145(17) -0.0029(17) C28 0.053(3) 0.040(2) 0.041(2) 0.0004(19) 0.027(2) 0.005(2) C29 0.062(3) 0.033(2) 0.040(2) -0.0026(18) 0.023(2) -0.007(2) C30 0.048(2) 0.034(2) 0.038(2) -0.0009(18) 0.0182(19) -0.0112(19) C31 0.032(2) 0.034(2) 0.039(2) 0.0027(17) 0.0154(17) -0.0036(17) C32 0.032(2) 0.047(3) 0.042(2) 0.0062(19) 0.0123(18) -0.0012(19) C33 0.043(2) 0.043(3) 0.056(3) 0.006(2) 0.014(2) -0.012(2) C34 0.066(3) 0.034(2) 0.053(3) -0.008(2) 0.025(2) -0.010(2) C35 0.061(3) 0.035(2) 0.058(3) -0.009(2) 0.036(2) -0.002(2) C36 0.039(2) 0.036(2) 0.048(3) -0.0072(19) 0.0243(19) -0.0030(18) C37 0.038(2) 0.039(2) 0.036(2) -0.0012(18) 0.0191(18) -0.0017(18) C38 0.050(2) 0.042(2) 0.035(2) -0.0038(18) 0.0207(19) -0.004(2) C39 0.056(3) 0.035(2) 0.030(2) -0.0050(18) 0.0114(19) -0.007(2) C40 0.038(2) 0.034(2) 0.035(2) 0.0045(17) 0.0058(18) -0.0054(18) C41 0.0293(19) 0.038(2) 0.038(2) -0.0009(18) 0.0137(17) -0.0030(17) C42 0.033(2) 0.038(2) 0.042(2) 0.0004(18) 0.0142(18) 0.0034(17) C43 0.042(2) 0.039(2) 0.040(2) -0.0005(18) 0.0151(19) 0.0087(19) C44 0.055(3) 0.035(2) 0.028(2) -0.0043(17) 0.0094(19) -0.0006(19) C45 0.039(2) 0.041(2) 0.029(2) -0.0013(17) 0.0050(17) -0.0053(18) C46 0.0293(19) 0.037(2) 0.032(2) 0.0031(17) 0.0092(16) -0.0018(17) C47 0.028(2) 0.047(3) 0.043(2) 0.0054(19) 0.0113(18) 0.0036(18) C48 0.042(2) 0.058(3) 0.044(3) 0.017(2) 0.019(2) 0.003(2) C49 0.048(3) 0.067(3) 0.047(3) 0.023(2) 0.010(2) 0.008(2) C50 0.037(2) 0.066(3) 0.052(3) 0.017(2) 0.010(2) 0.010(2) C51 0.026(2) 0.054(3) 0.042(2) 0.010(2) 0.0092(17) 0.0042(18) C52 0.033(2) 0.077(3) 0.049(3) -0.017(2) 0.019(2) -0.007(2) C53 0.046(3) 0.100(4) 0.051(3) -0.031(3) 0.027(2) -0.008(3) C54 0.051(3) 0.057(3) 0.039(2) -0.014(2) 0.015(2) 0.001(2) C55 0.034(2) 0.054(3) 0.033(2) -0.0076(19) 0.0071(17) -0.0013(19) C56 0.030(2) 0.046(2) 0.034(2) -0.0054(18) 0.0113(17) -0.0025(18) _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 O1 1.839(3) . ? U1 O2 1.840(2) . ? U1 N5 2.576(3) . ? U1 N3 2.584(3) . ? U1 N1 2.587(3) . ? U1 N2 2.595(3) . ? U1 N4 2.600(3) . ? U1 Li2 3.719(6) . ? U1 Li1 3.743(7) . ? U2 O4 1.837(2) . ? U2 O3 1.838(2) . ? U2 N8 2.578(3) . ? U2 N10 2.587(3) . ? U2 N9 2.591(3) . ? U2 N7 2.598(3) . ? U2 N6 2.603(3) . ? U2 Li4 3.705(6) . ? U2 Li3 3.707(6) . ? Li1 O5 1.894(7) . ? Li1 O11 1.904(7) . ? Li1 O1 1.904(7) . ? Li1 O8 1.947(7) . ? Li1 Li4 3.445(10) 1_655 ? Li2 O2 1.881(6) . ? Li2 O17 1.945(7) . ? Li2 O20 1.946(7) . ? Li2 O14 1.954(7) . ? Li2 Li3 3.366(10) . ? Li3 O3 1.875(7) . ? Li3 O21 1.913(7) . ? Li3 O15 1.939(7) . ? Li3 O18 1.958(7) . ? Li4 O4 1.871(7) . ? Li4 O9 1.906(7) 1_455 ? Li4 O12 1.928(7) 1_455 ? Li4 O6 1.932(7) 1_455 ? Li4 Li1 3.444(10) 1_455 ? S1 O7 1.414(3) . ? S1 O6 1.440(3) . ? S1 O5 1.453(3) . ? S1 C1 1.796(4) . ? S2 O10 1.411(3) . ? S2 O8 1.448(3) . ? S2 O9 1.449(3) . ? S2 C2 1.804(5) . ? S3 O13 1.422(3) . ? S3 O11 1.449(3) . ? S3 O12 1.452(3) . ? S3 C3 1.810(4) . ? S4 O16 1.416(3) . ? S4 O14 1.448(2) . ? S4 O15 1.448(3) . ? S4 C4 1.822(4) . ? S5 O19 1.431(3) . ? S5 O17 1.452(3) . ? S5 O18 1.454(2) . ? S5 C5 1.820(4) . ? S6 O22 1.430(3) . ? S6 O20 1.447(2) . ? S6 O21 1.449(3) . ? S6 C6 1.822(4) . ? O6 Li4 1.932(7) 1_655 ? O9 Li4 1.906(7) 1_655 ? O12 Li4 1.928(7) 1_655 ? N1 C11 1.343(4) . ? N1 C7 1.348(4) . ? N2 C16 1.343(4) . ? N2 C12 1.347(4) . ? N3 C21 1.338(5) . ? N3 C17 1.341(4) . ? N4 C22 1.339(4) . ? N4 C26 1.343(4) . ? N5 C27 1.334(4) . ? N5 C31 1.348(4) . ? N6 C32 1.340(4) . ? N6 C36 1.345(5) . ? N7 C41 1.346(4) . ? N7 C37 1.348(4) . ? N8 C42 1.346(4) . ? N8 C46 1.358(4) . ? N9 C51 1.346(4) . ? N9 C47 1.348(4) . ? N10 C56 1.336(4) . ? N10 C52 1.343(5) . ? F1 C1 1.339(5) . ? F2 C1 1.327(4) . ? F3 C1 1.331(4) . ? F4 C2 1.322(5) . ? F5 C2 1.330(5) . ? F6 C2 1.334(6) . ? F7 C3 1.330(4) . ? F8 C3 1.346(5) . ? F9 C3 1.329(5) . ? F10 C4 1.333(5) . ? F11 C4 1.328(4) . ? F12 C4 1.331(5) . ? F13 C5 1.333(4) . ? F14 C5 1.335(4) . ? F15 C5 1.329(4) . ? F16 C6 1.327(5) . ? F17 C6 1.329(4) . ? F18 C6 1.335(5) . ? C7 C8 1.386(5) . ? C7 H7 0.9300 . ? C8 C9 1.379(5) . ? C8 H8 0.9300 . ? C9 C10 1.390(5) . ? C9 H9 0.9300 . ? C10 C11 1.375(5) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.374(5) . ? C12 H12 0.9300 . ? C13 C14 1.386(5) . ? C13 H13 0.9300 . ? C14 C15 1.378(5) . ? C14 H14 0.9300 . ? C15 C16 1.370(5) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.378(5) . ? C17 H17 0.9300 . ? C18 C19 1.379(5) . ? C18 H18 0.9300 . ? C19 C20 1.366(5) . ? C19 H19 0.9300 . ? C20 C21 1.382(6) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.368(6) . ? C22 H22 0.9300 . ? C23 C24 1.370(6) . ? C23 H23 0.9300 . ? C24 C25 1.388(6) . ? C24 H24 0.9300 . ? C25 C26 1.361(5) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.377(5) . ? C27 H27 0.9300 . ? C28 C29 1.385(5) . ? C28 H28 0.9300 . ? C29 C30 1.377(5) . ? C29 H29 0.9300 . ? C30 C31 1.378(5) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.379(6) . ? C32 H32 0.9300 . ? C33 C34 1.389(6) . ? C33 H33 0.9300 . ? C34 C35 1.378(6) . ? C34 H34 0.9300 . ? C35 C36 1.385(5) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.380(5) . ? C37 H37 0.9300 . ? C38 C39 1.369(5) . ? C38 H38 0.9300 . ? C39 C40 1.387(5) . ? C39 H39 0.9300 . ? C40 C41 1.381(5) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C43 1.381(5) . ? C42 H42 0.9300 . ? C43 C44 1.380(5) . ? C43 H43 0.9300 . ? C44 C45 1.373(5) . ? C44 H44 0.9300 . ? C45 C46 1.369(5) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 C48 1.379(5) . ? C47 H47 0.9300 . ? C48 C49 1.378(5) . ? C48 H48 0.9300 . ? C49 C50 1.365(6) . ? C49 H49 0.9300 . ? C50 C51 1.374(6) . ? C50 H50 0.9300 . ? C51 H51 0.9300 . ? C52 C53 1.371(6) . ? C52 H52 0.9300 . ? C53 C54 1.377(6) . ? C53 H53 0.9300 . ? C54 C55 1.373(5) . ? C54 H54 0.9300 . ? C55 C56 1.366(5) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? 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 U1 O2 178.16(11) . . ? O1 U1 N5 89.02(10) . . ? O2 U1 N5 92.06(10) . . ? O1 U1 N3 91.33(10) . . ? O2 U1 N3 88.67(10) . . ? N5 U1 N3 143.93(10) . . ? O1 U1 N1 90.71(10) . . ? O2 U1 N1 88.25(10) . . ? N5 U1 N1 70.48(9) . . ? N3 U1 N1 145.55(10) . . ? O1 U1 N2 88.02(11) . . ? O2 U1 N2 90.24(10) . . ? N5 U1 N2 144.28(9) . . ? N3 U1 N2 71.74(10) . . ? N1 U1 N2 73.97(9) . . ? O1 U1 N4 91.99(11) . . ? O2 U1 N4 89.76(10) . . ? N5 U1 N4 71.53(9) . . ? N3 U1 N4 72.42(10) . . ? N1 U1 N4 141.85(9) . . ? N2 U1 N4 144.15(9) . . ? O4 U2 O3 178.82(12) . . ? O4 U2 N8 88.79(10) . . ? O3 U2 N8 92.02(10) . . ? O4 U2 N10 92.98(10) . . ? O3 U2 N10 86.86(10) . . ? N8 U2 N10 144.86(9) . . ? O4 U2 N9 87.32(10) . . ? O3 U2 N9 93.72(10) . . ? N8 U2 N9 74.29(9) . . ? N10 U2 N9 70.74(10) . . ? O4 U2 N7 91.66(10) . . ? O3 U2 N7 87.77(10) . . ? N8 U2 N7 72.07(9) . . ? N10 U2 N7 142.83(10) . . ? N9 U2 N7 146.36(9) . . ? O4 U2 N6 88.91(10) . . ? O3 U2 N6 89.94(10) . . ? N8 U2 N6 145.50(9) . . ? N10 U2 N6 69.65(9) . . ? N9 U2 N6 139.93(9) . . ? N7 U2 N6 73.60(9) . . ? O5 Li1 O11 109.2(4) . . ? O5 Li1 O1 102.8(3) . . ? O11 Li1 O1 105.5(3) . . ? O5 Li1 O8 111.5(3) . . ? O11 Li1 O8 119.6(4) . . ? O1 Li1 O8 106.7(3) . . ? O2 Li2 O17 107.4(3) . . ? O2 Li2 O20 107.2(3) . . ? O17 Li2 O20 114.7(3) . . ? O2 Li2 O14 104.9(3) . . ? O17 Li2 O14 106.2(3) . . ? O20 Li2 O14 115.7(3) . . ? O3 Li3 O21 107.6(3) . . ? O3 Li3 O15 107.8(3) . . ? O21 Li3 O15 105.8(3) . . ? O3 Li3 O18 107.2(3) . . ? O21 Li3 O18 116.4(3) . . ? O15 Li3 O18 111.7(3) . . ? O4 Li4 O9 105.1(3) . 1_455 ? O4 Li4 O12 110.4(3) . 1_455 ? O9 Li4 O12 106.4(3) 1_455 1_455 ? O4 Li4 O6 104.3(3) . 1_455 ? O9 Li4 O6 114.9(4) 1_455 1_455 ? O12 Li4 O6 115.3(4) 1_455 1_455 ? O7 S1 O6 116.4(2) . . ? O7 S1 O5 114.7(2) . . ? O6 S1 O5 113.59(18) . . ? O7 S1 C1 104.7(2) . . ? O6 S1 C1 102.91(18) . . ? O5 S1 C1 102.0(2) . . ? O10 S2 O8 115.35(19) . . ? O10 S2 O9 115.53(18) . . ? O8 S2 O9 113.80(17) . . ? O10 S2 C2 104.5(2) . . ? O8 S2 C2 102.4(2) . . ? O9 S2 C2 102.85(19) . . ? O13 S3 O11 115.16(18) . . ? O13 S3 O12 115.41(17) . . ? O11 S3 O12 113.34(17) . . ? O13 S3 C3 104.89(19) . . ? O11 S3 C3 103.09(18) . . ? O12 S3 C3 102.83(18) . . ? O16 S4 O14 115.63(17) . . ? O16 S4 O15 115.35(18) . . ? O14 S4 O15 113.05(16) . . ? O16 S4 C4 104.83(19) . . ? O14 S4 C4 102.85(17) . . ? O15 S4 C4 102.96(18) . . ? O19 S5 O17 115.32(16) . . ? O19 S5 O18 115.61(16) . . ? O17 S5 O18 113.32(16) . . ? O19 S5 C5 104.98(18) . . ? O17 S5 C5 102.94(17) . . ? O18 S5 C5 102.44(16) . . ? O22 S6 O20 115.65(16) . . ? O22 S6 O21 115.12(15) . . ? O20 S6 O21 113.50(15) . . ? O22 S6 C6 105.24(17) . . ? O20 S6 C6 102.89(16) . . ? O21 S6 C6 102.19(18) . . ? U1 O1 Li1 178.2(3) . . ? U1 O2 Li2 176.2(2) . . ? U2 O3 Li3 173.0(3) . . ? U2 O4 Li4 175.4(3) . . ? S1 O5 Li1 133.8(3) . . ? S1 O6 Li4 143.3(3) . 1_655 ? S2 O8 Li1 134.3(3) . . ? S2 O9 Li4 141.5(3) . 1_655 ? S3 O11 Li1 143.3(3) . . ? S3 O12 Li4 131.8(3) . 1_655 ? S4 O14 Li2 131.8(2) . . ? S4 O15 Li3 123.8(3) . . ? S5 O17 Li2 133.5(2) . . ? S5 O18 Li3 127.5(2) . . ? S6 O20 Li2 127.9(2) . . ? S6 O21 Li3 134.1(3) . . ? C11 N1 C7 117.8(3) . . ? C11 N1 U1 121.7(2) . . ? C7 N1 U1 119.7(2) . . ? C16 N2 C12 117.5(3) . . ? C16 N2 U1 121.3(2) . . ? C12 N2 U1 121.1(2) . . ? C21 N3 C17 117.3(3) . . ? C21 N3 U1 120.4(2) . . ? C17 N3 U1 122.3(2) . . ? C22 N4 C26 117.4(3) . . ? C22 N4 U1 122.4(2) . . ? C26 N4 U1 120.2(2) . . ? C27 N5 C31 118.1(3) . . ? C27 N5 U1 121.2(2) . . ? C31 N5 U1 120.7(2) . . ? C32 N6 C36 117.5(3) . . ? C32 N6 U2 120.7(3) . . ? C36 N6 U2 121.1(2) . . ? C41 N7 C37 117.7(3) . . ? C41 N7 U2 121.1(2) . . ? C37 N7 U2 121.0(2) . . ? C42 N8 C46 116.7(3) . . ? C42 N8 U2 121.2(2) . . ? C46 N8 U2 122.0(2) . . ? C51 N9 C47 117.1(3) . . ? C51 N9 U2 121.1(2) . . ? C47 N9 U2 120.8(2) . . ? C56 N10 C52 116.5(3) . . ? C56 N10 U2 121.0(2) . . ? C52 N10 U2 122.3(3) . . ? F2 C1 F3 106.1(3) . . ? F2 C1 F1 108.4(4) . . ? F3 C1 F1 107.9(3) . . ? F2 C1 S1 111.8(3) . . ? F3 C1 S1 111.8(3) . . ? F1 C1 S1 110.6(3) . . ? F4 C2 F5 107.2(4) . . ? F4 C2 F6 109.0(4) . . ? F5 C2 F6 107.8(4) . . ? F4 C2 S2 110.4(3) . . ? F5 C2 S2 111.3(3) . . ? F6 C2 S2 111.0(3) . . ? F9 C3 F7 107.3(3) . . ? F9 C3 F8 107.7(3) . . ? F7 C3 F8 108.5(3) . . ? F9 C3 S3 112.0(3) . . ? F7 C3 S3 110.5(3) . . ? F8 C3 S3 110.7(3) . . ? F11 C4 F12 107.6(3) . . ? F11 C4 F10 107.9(3) . . ? F12 C4 F10 108.3(3) . . ? F11 C4 S4 110.3(3) . . ? F12 C4 S4 111.5(3) . . ? F10 C4 S4 111.1(3) . . ? F15 C5 F13 107.5(3) . . ? F15 C5 F14 107.7(3) . . ? F13 C5 F14 107.6(3) . . ? F15 C5 S5 111.1(3) . . ? F13 C5 S5 111.4(3) . . ? F14 C5 S5 111.4(3) . . ? F16 C6 F17 107.9(3) . . ? F16 C6 F18 107.4(3) . . ? F17 C6 F18 107.4(3) . . ? F16 C6 S6 111.5(3) . . ? F17 C6 S6 111.4(3) . . ? F18 C6 S6 111.0(3) . . ? N1 C7 C8 122.2(3) . . ? N1 C7 H7 118.9 . . ? C8 C7 H7 118.9 . . ? C9 C8 C7 119.8(4) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 117.9(4) . . ? C8 C9 H9 121.1 . . ? C10 C9 H9 121.1 . . ? C11 C10 C9 119.6(4) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? N1 C11 C10 122.7(3) . . ? N1 C11 H11 118.6 . . ? C10 C11 H11 118.6 . . ? N2 C12 C13 122.7(3) . . ? N2 C12 H12 118.7 . . ? C13 C12 H12 118.7 . . ? C12 C13 C14 119.3(4) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? C15 C14 C13 118.1(4) . . ? C15 C14 H14 121.0 . . ? C13 C14 H14 121.0 . . ? C16 C15 C14 119.6(4) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? N2 C16 C15 122.8(4) . . ? N2 C16 H16 118.6 . . ? C15 C16 H16 118.6 . . ? N3 C17 C18 122.8(4) . . ? N3 C17 H17 118.6 . . ? C18 C17 H17 118.6 . . ? C17 C18 C19 119.1(4) . . ? C17 C18 H18 120.5 . . ? C19 C18 H18 120.5 . . ? C20 C19 C18 118.7(4) . . ? C20 C19 H19 120.7 . . ? C18 C19 H19 120.7 . . ? C19 C20 C21 119.1(4) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? N3 C21 C20 123.0(4) . . ? N3 C21 H21 118.5 . . ? C20 C21 H21 118.5 . . ? N4 C22 C23 122.6(4) . . ? N4 C22 H22 118.7 . . ? C23 C22 H22 118.7 . . ? C22 C23 C24 119.7(4) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C23 C24 C25 118.3(4) . . ? C23 C24 H24 120.8 . . ? C25 C24 H24 120.8 . . ? C26 C25 C24 118.8(4) . . ? C26 C25 H25 120.6 . . ? C24 C25 H25 120.6 . . ? N4 C26 C25 123.2(4) . . ? N4 C26 H26 118.4 . . ? C25 C26 H26 118.4 . . ? N5 C27 C28 123.1(4) . . ? N5 C27 H27 118.5 . . ? C28 C27 H27 118.5 . . ? C27 C28 C29 118.7(4) . . ? C27 C28 H28 120.6 . . ? C29 C28 H28 120.6 . . ? C30 C29 C28 118.6(4) . . ? C30 C29 H29 120.7 . . ? C28 C29 H29 120.7 . . ? C29 C30 C31 119.6(4) . . ? C29 C30 H30 120.2 . . ? C31 C30 H30 120.2 . . ? N5 C31 C30 122.0(4) . . ? N5 C31 H31 119.0 . . ? C30 C31 H31 119.0 . . ? N6 C32 C33 123.0(4) . . ? N6 C32 H32 118.5 . . ? C33 C32 H32 118.5 . . ? C32 C33 C34 119.2(4) . . ? C32 C33 H33 120.4 . . ? C34 C33 H33 120.4 . . ? C35 C34 C33 118.1(4) . . ? C35 C34 H34 120.9 . . ? C33 C34 H34 120.9 . . ? C34 C35 C36 119.4(4) . . ? C34 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? N6 C36 C35 122.7(4) . . ? N6 C36 H36 118.6 . . ? C35 C36 H36 118.6 . . ? N7 C37 C38 122.1(4) . . ? N7 C37 H37 118.9 . . ? C38 C37 H37 118.9 . . ? C39 C38 C37 119.9(4) . . ? C39 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? C38 C39 C40 118.7(4) . . ? C38 C39 H39 120.6 . . ? C40 C39 H39 120.6 . . ? C41 C40 C39 118.6(4) . . ? C41 C40 H40 120.7 . . ? C39 C40 H40 120.7 . . ? N7 C41 C40 122.9(3) . . ? N7 C41 H41 118.6 . . ? C40 C41 H41 118.6 . . ? N8 C42 C43 123.7(4) . . ? N8 C42 H42 118.1 . . ? C43 C42 H42 118.1 . . ? C44 C43 C42 117.8(4) . . ? C44 C43 H43 121.1 . . ? C42 C43 H43 121.1 . . ? C45 C44 C43 119.8(4) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C46 C45 C44 119.1(4) . . ? C46 C45 H45 120.4 . . ? C44 C45 H45 120.4 . . ? N8 C46 C45 122.8(4) . . ? N8 C46 H46 118.6 . . ? C45 C46 H46 118.6 . . ? N9 C47 C48 122.9(4) . . ? N9 C47 H47 118.5 . . ? C48 C47 H47 118.5 . . ? C49 C48 C47 118.3(4) . . ? C49 C48 H48 120.8 . . ? C47 C48 H48 120.8 . . ? C50 C49 C48 119.7(4) . . ? C50 C49 H49 120.1 . . ? C48 C49 H49 120.1 . . ? C49 C50 C51 118.9(4) . . ? C49 C50 H50 120.6 . . ? C51 C50 H50 120.6 . . ? N9 C51 C50 123.0(4) . . ? N9 C51 H51 118.5 . . ? C50 C51 H51 118.5 . . ? N10 C52 C53 123.4(4) . . ? N10 C52 H52 118.3 . . ? C53 C52 H52 118.3 . . ? C52 C53 C54 118.9(4) . . ? C52 C53 H53 120.6 . . ? C54 C53 H53 120.6 . . ? C55 C54 C53 118.4(4) . . ? C55 C54 H54 120.8 . . ? C53 C54 H54 120.8 . . ? C56 C55 C54 119.2(4) . . ? C56 C55 H55 120.4 . . ? C54 C55 H55 120.4 . . ? N10 C56 C55 123.6(4) . . ? N10 C56 H56 118.2 . . ? C55 C56 H56 118.2 . . ? #===END data_12.py _database_code_depnum_ccdc_archive 'CCDC 711341' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H25 N5 O2 U, I, C5 H5 N' _chemical_formula_sum 'C30 H30 I N6 O2 U' _chemical_formula_weight 871.53 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' I I -0.4742 1.8119 '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 orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.5129(7) _cell_length_b 17.2053(8) _cell_length_c 22.4464(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6377.2(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 207093 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 25.68 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent dark orange' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.815 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3304 _exptl_absorpt_coefficient_mu 6.094 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.377 _exptl_absorpt_correction_T_max 0.512 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 30 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 area-detector diffractometer' _diffrn_measurement_method 'two \f and seven \w scans with 2\% steps (465 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 207093 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 25.68 _reflns_number_total 6034 _reflns_number_gt 4291 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters, with restraints for five C atoms from two coordinated pyridine molecules, seemingly affected with some unresolved disorder. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 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^)+(0.0415P)^2^+8.2785P] 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 6034 _refine_ls_number_parameters 361 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0719 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.0948 _refine_ls_wR_factor_gt 0.0877 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.001 _refine_diff_density_min -1.228 _refine_diff_density_rms 0.125 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 0.580990(15) 0.134662(15) 0.605853(11) 0.03308(9) Uani 1 1 d . . . I I 0.07567(3) 0.13974(3) 0.61973(2) 0.04218(13) Uani 1 1 d . . . O1 O 0.5269(3) 0.1167(3) 0.53557(19) 0.0357(12) Uani 1 1 d . . . O2 O 0.6349(3) 0.1515(3) 0.67557(19) 0.0370(12) Uani 1 1 d . . . N1 N 0.4498(3) 0.1357(3) 0.6706(2) 0.0355(13) Uani 1 1 d . . . N2 N 0.5492(4) -0.0073(3) 0.6363(2) 0.0347(14) Uani 1 1 d . . . N3 N 0.6985(4) 0.0469(3) 0.5670(3) 0.0385(14) Uani 1 1 d . . . N4 N 0.6941(3) 0.2229(4) 0.5598(2) 0.0393(15) Uani 1 1 d . . . N5 N 0.5215(3) 0.2756(3) 0.5977(2) 0.0357(14) Uani 1 1 d . . . C1 C 0.3763(4) 0.1283(4) 0.6458(3) 0.0401(17) Uani 1 1 d . . . H1 H 0.3727 0.1202 0.6049 0.048 Uiso 1 1 calc R . . C2 C 0.3058(4) 0.1323(5) 0.6789(3) 0.0453(19) Uani 1 1 d . . . H2 H 0.2557 0.1297 0.6601 0.054 Uiso 1 1 calc R . . C3 C 0.3106(5) 0.1402(5) 0.7397(3) 0.053(2) Uani 1 1 d . . . H3 H 0.2638 0.1422 0.7626 0.064 Uiso 1 1 calc R . . C4 C 0.3855(5) 0.1452(5) 0.7662(3) 0.049(2) Uani 1 1 d . . . H4 H 0.3901 0.1501 0.8073 0.059 Uiso 1 1 calc R . . C5 C 0.4551(5) 0.1428(4) 0.7301(3) 0.0401(17) Uani 1 1 d . . . H5 H 0.5059 0.1461 0.7478 0.048 Uiso 1 1 calc R . . C6 C 0.5061(4) -0.0550(4) 0.6003(3) 0.0388(17) Uani 1 1 d . . . H6 H 0.4888 -0.0363 0.5635 0.047 Uiso 1 1 calc R . . C7 C 0.4869(5) -0.1301(4) 0.6159(3) 0.0438(18) Uani 1 1 d . . . H7 H 0.4565 -0.1610 0.5903 0.053 Uiso 1 1 calc R . . C8 C 0.5127(5) -0.1592(4) 0.6696(3) 0.0460(19) Uani 1 1 d . . . H8 H 0.4995 -0.2096 0.6810 0.055 Uiso 1 1 calc R . . C9 C 0.5586(5) -0.1124(4) 0.7063(3) 0.047(2) Uani 1 1 d . . . H9 H 0.5787 -0.1310 0.7423 0.057 Uiso 1 1 calc R . . C10 C 0.5737(5) -0.0376(5) 0.6884(3) 0.048(2) Uani 1 1 d . . . H10 H 0.6029 -0.0057 0.7141 0.057 Uiso 1 1 calc R . . C11 C 0.7618(6) 0.0299(6) 0.6016(4) 0.065(2) Uani 1 1 d U . . H11 H 0.7604 0.0463 0.6411 0.079 Uiso 1 1 calc R . . C12 C 0.8279(6) -0.0098(6) 0.5829(4) 0.073(3) Uani 1 1 d U . . H12 H 0.8705 -0.0197 0.6089 0.087 Uiso 1 1 calc R . . C13 C 0.8311(5) -0.0356(5) 0.5239(4) 0.053(2) Uani 1 1 d . . . H13 H 0.8752 -0.0638 0.5100 0.064 Uiso 1 1 calc R . . C14 C 0.7671(5) -0.0179(5) 0.4870(4) 0.051(2) Uani 1 1 d . . . H14 H 0.7676 -0.0330 0.4472 0.061 Uiso 1 1 calc R . . C15 C 0.7026(5) 0.0223(4) 0.5100(3) 0.0449(19) Uani 1 1 d . . . H15 H 0.6592 0.0333 0.4849 0.054 Uiso 1 1 calc R . . C16 C 0.7462(7) 0.2583(6) 0.5958(4) 0.082(3) Uani 1 1 d U . . H16 H 0.7366 0.2549 0.6366 0.098 Uiso 1 1 calc R . . C17 C 0.8141(7) 0.3002(7) 0.5776(5) 0.087(3) Uani 1 1 d U . . H17 H 0.8469 0.3257 0.6051 0.104 Uiso 1 1 calc R . . C18 C 0.8309(5) 0.3025(5) 0.5175(4) 0.052(2) Uani 1 1 d . . . H18 H 0.8792 0.3229 0.5030 0.062 Uiso 1 1 calc R . . C19 C 0.7743(6) 0.2740(6) 0.4811(4) 0.068(3) Uani 1 1 d U . . H19 H 0.7794 0.2810 0.4402 0.082 Uiso 1 1 calc R . . C20 C 0.7084(6) 0.2343(5) 0.5032(3) 0.058(2) Uani 1 1 d . . . H20 H 0.6715 0.2142 0.4760 0.069 Uiso 1 1 calc R . . C21 C 0.4955(5) 0.2997(4) 0.5446(3) 0.0448(19) Uani 1 1 d . . . H21 H 0.4990 0.2658 0.5124 0.054 Uiso 1 1 calc R . . C22 C 0.4635(5) 0.3732(4) 0.5352(3) 0.045(2) Uani 1 1 d . . . H22 H 0.4465 0.3881 0.4974 0.054 Uiso 1 1 calc R . . C23 C 0.4571(5) 0.4233(5) 0.5820(4) 0.050(2) Uani 1 1 d . . . H23 H 0.4344 0.4724 0.5770 0.060 Uiso 1 1 calc R . . C24 C 0.4853(5) 0.3996(5) 0.6373(4) 0.047(2) Uani 1 1 d . . . H24 H 0.4830 0.4328 0.6699 0.056 Uiso 1 1 calc R . . C25 C 0.5165(5) 0.3262(4) 0.6428(3) 0.0426(18) Uani 1 1 d . . . H25 H 0.5353 0.3107 0.6800 0.051 Uiso 1 1 calc R . . N6 N 0.2434(5) 0.4421(4) 0.7489(3) 0.071(2) Uani 1 1 d . . . C26 C 0.2687(6) 0.4434(5) 0.6921(4) 0.059(2) Uani 1 1 d . . . H26 H 0.2962 0.4871 0.6784 0.071 Uiso 1 1 calc R . . C27 C 0.2555(5) 0.3821(5) 0.6528(4) 0.056(2) Uani 1 1 d . . . H27 H 0.2752 0.3840 0.6140 0.067 Uiso 1 1 calc R . . C28 C 0.2128(5) 0.3192(5) 0.6725(4) 0.057(2) Uani 1 1 d . . . H28 H 0.2005 0.2785 0.6468 0.068 Uiso 1 1 calc R . . C29 C 0.1882(5) 0.3168(5) 0.7310(4) 0.055(2) Uani 1 1 d . . . H29 H 0.1621 0.2732 0.7459 0.066 Uiso 1 1 calc R . . C30 C 0.2026(6) 0.3793(5) 0.7666(4) 0.059(2) Uani 1 1 d . . . H30 H 0.1830 0.3781 0.8054 0.071 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 0.03169(15) 0.03680(15) 0.03076(14) -0.00116(12) -0.00065(11) 0.00157(13) I 0.0422(3) 0.0420(3) 0.0423(3) -0.0055(2) 0.0017(2) -0.0006(3) O1 0.038(3) 0.034(3) 0.035(3) 0.000(2) 0.002(2) 0.004(2) O2 0.036(3) 0.042(3) 0.033(3) 0.000(2) 0.004(2) -0.003(2) N1 0.037(3) 0.035(3) 0.034(3) 0.000(3) 0.002(3) 0.003(3) N2 0.039(4) 0.034(3) 0.032(3) -0.001(3) -0.003(3) 0.004(3) N3 0.041(4) 0.035(3) 0.039(3) -0.004(3) 0.004(3) 0.008(3) N4 0.033(4) 0.052(4) 0.033(3) 0.000(3) 0.001(3) -0.006(3) N5 0.037(3) 0.033(3) 0.037(3) 0.000(3) 0.001(3) 0.003(3) C1 0.037(4) 0.041(4) 0.042(4) 0.003(3) -0.007(3) -0.001(4) C2 0.029(4) 0.060(5) 0.047(4) 0.011(4) 0.000(3) -0.007(4) C3 0.039(5) 0.070(6) 0.051(5) 0.003(4) 0.008(4) 0.004(4) C4 0.041(4) 0.066(6) 0.040(4) -0.001(4) 0.005(3) -0.008(4) C5 0.039(4) 0.049(5) 0.033(4) -0.004(3) 0.000(3) 0.001(4) C6 0.045(4) 0.040(4) 0.031(4) -0.002(3) -0.002(3) 0.004(4) C7 0.047(4) 0.041(4) 0.044(4) -0.010(4) -0.004(3) -0.002(4) C8 0.060(5) 0.040(4) 0.039(4) -0.002(4) 0.003(4) -0.002(4) C9 0.058(5) 0.043(5) 0.041(4) 0.006(4) 0.002(4) 0.002(4) C10 0.063(6) 0.043(4) 0.036(4) -0.007(3) -0.001(4) -0.001(4) C11 0.060(5) 0.092(6) 0.044(4) 0.002(4) -0.005(4) 0.032(5) C12 0.060(6) 0.098(7) 0.060(5) 0.011(5) -0.003(4) 0.034(5) C13 0.058(6) 0.047(5) 0.055(5) 0.009(4) 0.020(4) 0.018(4) C14 0.049(5) 0.060(6) 0.044(4) -0.009(4) 0.011(4) 0.001(4) C15 0.045(5) 0.043(5) 0.047(5) -0.006(4) -0.002(4) 0.000(4) C16 0.081(5) 0.099(5) 0.066(4) 0.005(4) -0.003(4) -0.024(4) C17 0.083(5) 0.102(5) 0.075(5) 0.005(4) -0.005(4) -0.030(4) C18 0.044(5) 0.061(6) 0.050(5) 0.005(4) 0.006(4) -0.005(4) C19 0.079(6) 0.082(6) 0.043(4) 0.005(4) 0.003(4) -0.037(5) C20 0.072(6) 0.062(6) 0.039(5) 0.005(4) -0.012(4) -0.030(5) C21 0.050(5) 0.037(4) 0.048(4) 0.001(4) -0.001(4) 0.004(4) C22 0.045(5) 0.041(5) 0.050(5) 0.007(4) 0.000(3) 0.015(4) C23 0.046(5) 0.045(5) 0.058(5) 0.006(4) 0.008(4) 0.009(4) C24 0.044(5) 0.038(4) 0.059(5) -0.011(4) 0.008(4) -0.006(4) C25 0.047(5) 0.039(5) 0.042(4) -0.001(4) 0.002(4) 0.002(4) N6 0.083(6) 0.065(5) 0.064(5) -0.005(4) 0.001(4) 0.001(5) C26 0.069(6) 0.045(5) 0.064(6) 0.001(4) 0.000(5) -0.009(5) C27 0.055(5) 0.059(5) 0.054(5) -0.003(4) 0.005(4) 0.001(5) C28 0.042(5) 0.058(6) 0.069(6) -0.018(5) -0.002(4) -0.011(4) C29 0.058(6) 0.051(5) 0.055(5) 0.001(4) 0.009(4) -0.006(4) C30 0.073(6) 0.061(6) 0.043(4) 0.008(4) 0.010(4) -0.012(5) _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 1.823(5) . ? U O1 1.839(4) . ? U N2 2.589(6) . ? U N3 2.609(6) . ? U N1 2.609(6) . ? U N4 2.620(6) . ? U N5 2.623(6) . ? N1 C1 1.340(9) . ? N1 C5 1.344(8) . ? N2 C10 1.344(9) . ? N2 C6 1.355(9) . ? N3 C11 1.336(9) . ? N3 C15 1.348(9) . ? N4 C20 1.305(9) . ? N4 C16 1.330(11) . ? N5 C21 1.334(9) . ? N5 C25 1.339(9) . ? C1 C2 1.382(10) . ? C1 H1 0.9300 . ? C2 C3 1.374(10) . ? C2 H2 0.9300 . ? C3 C4 1.375(11) . ? C3 H3 0.9300 . ? C4 C5 1.407(11) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.376(10) . ? C6 H6 0.9300 . ? C7 C8 1.372(10) . ? C7 H7 0.9300 . ? C8 C9 1.380(11) . ? C8 H8 0.9300 . ? C9 C10 1.372(10) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.354(11) . ? C11 H11 0.9300 . ? C12 C13 1.397(12) . ? C12 H12 0.9300 . ? C13 C14 1.378(11) . ? C13 H13 0.9300 . ? C14 C15 1.372(10) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.394(13) . ? C16 H16 0.9300 . ? C17 C18 1.379(13) . ? C17 H17 0.9300 . ? C18 C19 1.334(11) . ? C18 H18 0.9300 . ? C19 C20 1.377(11) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.386(10) . ? C21 H21 0.9300 . ? C22 C23 1.364(10) . ? C22 H22 0.9300 . ? C23 C24 1.386(11) . ? C23 H23 0.9300 . ? C24 C25 1.368(11) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? N6 C30 1.334(11) . ? N6 C26 1.342(10) . ? C26 C27 1.392(11) . ? C26 H26 0.9300 . ? C27 C28 1.366(11) . ? C27 H27 0.9300 . ? C28 C29 1.373(11) . ? C28 H28 0.9300 . ? C29 C30 1.360(12) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? 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 O1 179.5(2) . . ? O2 U N2 91.28(19) . . ? O1 U N2 88.25(19) . . ? O2 U N3 90.9(2) . . ? O1 U N3 88.67(19) . . ? N2 U N3 72.11(18) . . ? O2 U N1 85.77(19) . . ? O1 U N1 94.34(19) . . ? N2 U N1 72.03(18) . . ? N3 U N1 143.89(18) . . ? O2 U N4 84.20(19) . . ? O1 U N4 96.01(19) . . ? N2 U N4 142.65(19) . . ? N3 U N4 70.92(19) . . ? N1 U N4 143.91(18) . . ? O2 U N5 95.50(19) . . ? O1 U N5 85.03(19) . . ? N2 U N5 144.53(18) . . ? N3 U N5 142.23(18) . . ? N1 U N5 73.82(17) . . ? N4 U N5 72.78(18) . . ? C1 N1 C5 118.7(6) . . ? C1 N1 U 121.3(4) . . ? C5 N1 U 119.9(5) . . ? C10 N2 C6 116.3(6) . . ? C10 N2 U 122.3(5) . . ? C6 N2 U 121.4(4) . . ? C11 N3 C15 116.4(7) . . ? C11 N3 U 120.9(5) . . ? C15 N3 U 122.4(5) . . ? C20 N4 C16 114.0(7) . . ? C20 N4 U 126.9(5) . . ? C16 N4 U 119.1(5) . . ? C21 N5 C25 117.0(6) . . ? C21 N5 U 118.1(5) . . ? C25 N5 U 124.9(5) . . ? N1 C1 C2 122.3(7) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C3 C2 C1 119.3(7) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C4 119.2(8) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C3 C4 C5 119.0(7) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 121.4(7) . . ? N1 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? N2 C6 C7 122.6(7) . . ? N2 C6 H6 118.7 . . ? C7 C6 H6 118.7 . . ? C8 C7 C6 119.7(7) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C7 C8 C9 118.8(7) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? C10 C9 C8 118.2(7) . . ? C10 C9 H9 120.9 . . ? C8 C9 H9 120.9 . . ? N2 C10 C9 124.3(7) . . ? N2 C10 H10 117.8 . . ? C9 C10 H10 117.8 . . ? N3 C11 C12 124.1(8) . . ? N3 C11 H11 117.9 . . ? C12 C11 H11 117.9 . . ? C11 C12 C13 119.0(9) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C14 C13 C12 118.1(8) . . ? C14 C13 H13 121.0 . . ? C12 C13 H13 121.0 . . ? C15 C14 C13 118.7(7) . . ? C15 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? N3 C15 C14 123.7(7) . . ? N3 C15 H15 118.2 . . ? C14 C15 H15 118.2 . . ? N4 C16 C17 125.4(9) . . ? N4 C16 H16 117.3 . . ? C17 C16 H16 117.3 . . ? C18 C17 C16 117.6(10) . . ? C18 C17 H17 121.2 . . ? C16 C17 H17 121.2 . . ? C19 C18 C17 116.6(9) . . ? C19 C18 H18 121.7 . . ? C17 C18 H18 121.7 . . ? C18 C19 C20 121.0(8) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? N4 C20 C19 124.6(8) . . ? N4 C20 H20 117.7 . . ? C19 C20 H20 117.7 . . ? N5 C21 C22 122.8(7) . . ? N5 C21 H21 118.6 . . ? C22 C21 H21 118.6 . . ? C23 C22 C21 119.3(7) . . ? C23 C22 H22 120.4 . . ? C21 C22 H22 120.4 . . ? C22 C23 C24 118.5(7) . . ? C22 C23 H23 120.8 . . ? C24 C23 H23 120.8 . . ? C25 C24 C23 118.7(7) . . ? C25 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? N5 C25 C24 123.6(7) . . ? N5 C25 H25 118.2 . . ? C24 C25 H25 118.2 . . ? C30 N6 C26 117.0(8) . . ? N6 C26 C27 122.7(8) . . ? N6 C26 H26 118.7 . . ? C27 C26 H26 118.7 . . ? C28 C27 C26 118.4(8) . . ? C28 C27 H27 120.8 . . ? C26 C27 H27 120.8 . . ? C27 C28 C29 119.1(8) . . ? C27 C28 H28 120.5 . . ? C29 C28 H28 120.5 . . ? C30 C29 C28 119.2(8) . . ? C30 C29 H29 120.4 . . ? C28 C29 H29 120.4 . . ? N6 C30 C29 123.5(8) . . ? N6 C30 H30 118.2 . . ? C29 C30 H30 118.2 . . ? #===END data_15.1.5py _database_code_depnum_ccdc_archive 'CCDC 711342' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H43 N9 O2 U, C F3 O3 S, C7.50 H7.50 N1.50' _chemical_formula_sum 'C45.50 H50.50 F3 N10.50 O5 S U' _chemical_formula_weight 1151.55 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' 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' _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 12.5854(12) _cell_length_b 14.1686(19) _cell_length_c 14.4513(19) _cell_angle_alpha 110.201(6) _cell_angle_beta 98.845(8) _cell_angle_gamma 94.538(9) _cell_volume 2365.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 91211 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 25.68 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent dark brown-green' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.617 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 3.544 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.537 _exptl_absorpt_correction_T_max 0.609 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 40 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 area-detector diffractometer' _diffrn_measurement_method 'two \f and ten \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 91211 _diffrn_reflns_av_R_equivalents 0.0927 _diffrn_reflns_av_sigmaI/netI 0.0988 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 25.68 _reflns_number_total 8946 _reflns_number_gt 7820 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by Patterson map interpretation and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters, with restraints on bond lengths for atoms C16, C17 and C26, C27 and on displacement parameters for some badly behaving atoms. The pyridine half-molecule is disordered around a symmetry centre and the N atom was not located. The H atoms were introduced at calculated positions (except those of the disordered pyridine molecule) and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH, CH~2~) or 1.5 (CH~3~) 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^)+(0.0439P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 8946 _refine_ls_number_parameters 603 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1058 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.336 _refine_diff_density_min -1.290 _refine_diff_density_rms 0.121 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 0.766364(15) 0.520250(12) 0.518860(13) 0.03871(9) Uani 1 1 d . . . S1 S 0.21485(14) 0.10860(10) 0.87635(10) 0.0499(4) Uani 1 1 d . . . O1 O 0.6644(3) 0.5933(2) 0.4865(2) 0.0405(9) Uani 1 1 d . . . O2 O 0.8662(3) 0.4434(3) 0.5485(3) 0.0442(9) Uani 1 1 d . . . O3 O 0.2374(5) 0.2094(3) 0.8771(3) 0.0707(14) Uani 1 1 d . . . O4 O 0.1411(4) 0.0976(3) 0.9403(3) 0.0714(15) Uani 1 1 d . . . O5 O 0.2001(4) 0.0269(3) 0.7804(3) 0.0683(14) Uani 1 1 d . . . N1 N 0.6213(4) 0.4044(3) 0.5512(3) 0.0395(10) Uani 1 1 d . . . N2 N 0.7312(4) 0.5701(3) 0.7017(3) 0.0387(10) Uani 1 1 d . . . N3 N 0.8773(4) 0.6885(3) 0.6520(3) 0.0386(10) Uani 1 1 d . . . N4 N 0.8990(4) 0.6223(3) 0.4580(3) 0.0408(11) Uani 1 1 d . . . N5 N 0.5677(4) 0.3230(3) 0.4720(3) 0.0398(11) Uani 1 1 d . . . N6 N 0.5321(4) 0.3556(3) 0.6638(3) 0.0429(11) Uani 1 1 d . . . N7 N 0.9060(4) 0.5862(3) 0.3604(3) 0.0406(10) Uani 1 1 d . . . N8 N 1.0220(4) 0.7702(3) 0.4876(3) 0.0452(12) Uani 1 1 d . . . N9 N 0.7193(4) 0.3905(3) 0.3413(3) 0.0495(12) Uani 1 1 d . . . N10 N 0.1234(7) 0.7749(6) 0.0006(5) 0.106(3) Uani 1 1 d . . . F1 F 0.3443(5) 0.0054(3) 0.9518(4) 0.1036(15) Uani 1 1 d U . . F2 F 0.4253(4) 0.1045(4) 0.8962(4) 0.1106(16) Uani 1 1 d U . . F3 F 0.3705(4) 0.1619(3) 1.0365(3) 0.0833(13) Uani 1 1 d . . . C1 C 0.6009(5) 0.4176(4) 0.6422(4) 0.0427(13) Uani 1 1 d . . . C2 C 0.6645(5) 0.5071(4) 0.7259(4) 0.0421(13) Uani 1 1 d . . . C3 C 0.6536(5) 0.5237(4) 0.8247(4) 0.0536(16) Uani 1 1 d . . . H3 H 0.6058 0.4796 0.8391 0.064 Uiso 1 1 calc R . . C4 C 0.7160(5) 0.6079(4) 0.9011(4) 0.0563(17) Uani 1 1 d . . . H4 H 0.7117 0.6201 0.9678 0.068 Uiso 1 1 calc R . . C5 C 0.7840(5) 0.6727(4) 0.8771(4) 0.0511(15) Uani 1 1 d . . . H5 H 0.8254 0.7295 0.9277 0.061 Uiso 1 1 calc R . . C6 C 0.7910(5) 0.6539(4) 0.7782(4) 0.0415(12) Uani 1 1 d . . . C7 C 0.8634(4) 0.7214(4) 0.7486(4) 0.0398(12) Uani 1 1 d . . . C8 C 0.9137(5) 0.8161(4) 0.8181(4) 0.0490(14) Uani 1 1 d . . . H8 H 0.9007 0.8385 0.8833 0.059 Uiso 1 1 calc R . . C9 C 0.9828(5) 0.8761(4) 0.7887(4) 0.0546(16) Uani 1 1 d . . . H9 H 1.0185 0.9386 0.8346 0.066 Uiso 1 1 calc R . . C10 C 0.9987(5) 0.8432(4) 0.6912(4) 0.0486(14) Uani 1 1 d . . . H10 H 1.0446 0.8829 0.6702 0.058 Uiso 1 1 calc R . . C11 C 0.9448(5) 0.7495(4) 0.6250(4) 0.0424(12) Uani 1 1 d . . . C12 C 0.9564(5) 0.7116(4) 0.5172(4) 0.0416(13) Uani 1 1 d . . . C13 C 0.4969(5) 0.2599(3) 0.4872(4) 0.0396(12) Uani 1 1 d . . . C14 C 0.4773(5) 0.2747(4) 0.5859(4) 0.0410(13) Uani 1 1 d . . . C15 C 0.3992(5) 0.2024(4) 0.6094(4) 0.0494(15) Uani 1 1 d . . . C16 C 0.3630(6) 0.1046(5) 0.5169(4) 0.068(2) Uani 1 1 d D . . H16A H 0.4186 0.0607 0.5156 0.082 Uiso 1 1 calc R . . H16B H 0.2973 0.0697 0.5245 0.082 Uiso 1 1 calc R . . C17 C 0.3421(6) 0.1175(5) 0.4202(4) 0.071(2) Uani 1 1 d D . . H17A H 0.2827 0.1570 0.4196 0.085 Uiso 1 1 calc R . . H17B H 0.3183 0.0511 0.3679 0.085 Uiso 1 1 calc R . . C18 C 0.4393(5) 0.1699(4) 0.3934(4) 0.0459(14) Uani 1 1 d . . . C19 C 0.4585(6) 0.1723(5) 0.6926(5) 0.0564(16) Uani 1 1 d . . . H19A H 0.4861 0.2322 0.7511 0.085 Uiso 1 1 calc R . . H19B H 0.5178 0.1378 0.6704 0.085 Uiso 1 1 calc R . . H19C H 0.4091 0.1281 0.7090 0.085 Uiso 1 1 calc R . . C20 C 0.3034(6) 0.2546(5) 0.6419(6) 0.0650(18) Uani 1 1 d . . . H20A H 0.3292 0.3219 0.6899 0.098 Uiso 1 1 calc R . . H20B H 0.2633 0.2164 0.6719 0.098 Uiso 1 1 calc R . . H20C H 0.2571 0.2585 0.5844 0.098 Uiso 1 1 calc R . . C21 C 0.3971(5) 0.2082(4) 0.3104(4) 0.0568(15) Uani 1 1 d . . . H21A H 0.3482 0.2560 0.3332 0.085 Uiso 1 1 calc R . . H21B H 0.3596 0.1520 0.2521 0.085 Uiso 1 1 calc R . . H21C H 0.4571 0.2408 0.2934 0.085 Uiso 1 1 calc R . . C22 C 0.5221(6) 0.0997(4) 0.3598(5) 0.0583(16) Uani 1 1 d . . . H22A H 0.5830 0.1368 0.3487 0.087 Uiso 1 1 calc R . . H22B H 0.4894 0.0447 0.2985 0.087 Uiso 1 1 calc R . . H22C H 0.5464 0.0730 0.4108 0.087 Uiso 1 1 calc R . . C23 C 0.9713(5) 0.6398(4) 0.3269(4) 0.0418(13) Uani 1 1 d . . . C24 C 1.0318(5) 0.7344(4) 0.3926(4) 0.0431(13) Uani 1 1 d . . . C25 C 1.1087(6) 0.7974(4) 0.3592(4) 0.0542(16) Uani 1 1 d . . . C26 C 1.1207(8) 0.7474(6) 0.2560(5) 0.108(3) Uani 1 1 d DU . . H26A H 1.1211 0.7992 0.2262 0.129 Uiso 1 1 calc R . . H26B H 1.1928 0.7275 0.2591 0.129 Uiso 1 1 calc R . . C27 C 1.0463(8) 0.6587(6) 0.1836(5) 0.111(3) Uani 1 1 d DU . . H27A H 1.0902 0.6155 0.1422 0.134 Uiso 1 1 calc R . . H27B H 0.9992 0.6833 0.1399 0.134 Uiso 1 1 calc R . . C28 C 0.9746(5) 0.5917(4) 0.2158(4) 0.0520(15) Uani 1 1 d D . . C29 C 1.0661(7) 0.9006(5) 0.3744(6) 0.080(2) Uani 1 1 d U . . H29A H 0.9950 0.8890 0.3337 0.120 Uiso 1 1 calc R . . H29B H 1.1146 0.9431 0.3552 0.120 Uiso 1 1 calc R . . H29C H 1.0623 0.9336 0.4439 0.120 Uiso 1 1 calc R . . C30 C 1.2222(6) 0.8158(5) 0.4236(6) 0.068(2) Uani 1 1 d . . . H30A H 1.2182 0.8455 0.4933 0.103 Uiso 1 1 calc R . . H30B H 1.2695 0.8611 0.4065 0.103 Uiso 1 1 calc R . . H30C H 1.2501 0.7524 0.4113 0.103 Uiso 1 1 calc R . . C31 C 0.8627(7) 0.5783(5) 0.1528(5) 0.077(2) Uani 1 1 d . . . H31A H 0.8373 0.6431 0.1673 0.115 Uiso 1 1 calc R . . H31B H 0.8135 0.5332 0.1682 0.115 Uiso 1 1 calc R . . H31C H 0.8663 0.5503 0.0828 0.115 Uiso 1 1 calc R . . C32 C 1.0106(7) 0.4905(5) 0.1947(5) 0.087(3) Uani 1 1 d . . . H32A H 1.0166 0.4621 0.1253 0.131 Uiso 1 1 calc R . . H32B H 0.9586 0.4464 0.2085 0.131 Uiso 1 1 calc R . . H32C H 1.0801 0.4975 0.2365 0.131 Uiso 1 1 calc R . . C33 C 0.7562(6) 0.2990(5) 0.3174(5) 0.0636(17) Uani 1 1 d . . . H33 H 0.8087 0.2901 0.3653 0.076 Uiso 1 1 calc R . . C34 C 0.7224(7) 0.2199(5) 0.2288(5) 0.073(2) Uani 1 1 d . . . H34 H 0.7527 0.1599 0.2160 0.088 Uiso 1 1 calc R . . C35 C 0.6422(7) 0.2305(5) 0.1586(5) 0.071(2) Uani 1 1 d . . . H35 H 0.6160 0.1773 0.0977 0.085 Uiso 1 1 calc R . . C36 C 0.6016(7) 0.3208(5) 0.1800(5) 0.082(2) Uani 1 1 d . . . H36 H 0.5488 0.3308 0.1331 0.098 Uiso 1 1 calc R . . C37 C 0.6403(7) 0.3965(5) 0.2722(4) 0.068(2) Uani 1 1 d . . . H37 H 0.6089 0.4559 0.2871 0.081 Uiso 1 1 calc R . . C38 C 0.3468(7) 0.0920(5) 0.9418(6) 0.0657(19) Uani 1 1 d . . . C39 C 0.1273(7) 0.8745(6) 0.0479(6) 0.079(2) Uani 1 1 d . . . H39 H 0.0683 0.9079 0.0378 0.095 Uiso 1 1 calc R . . C40 C 0.2236(9) 0.9261(6) 0.1130(7) 0.091(3) Uani 1 1 d U . . H40 H 0.2293 0.9950 0.1504 0.109 Uiso 1 1 calc R . . C41 C 0.3070(9) 0.8771(8) 0.1216(8) 0.100(3) Uani 1 1 d U . . H41 H 0.3726 0.9143 0.1612 0.120 Uiso 1 1 calc R . . C42 C 0.3026(8) 0.7797(7) 0.0777(7) 0.091(3) Uani 1 1 d . . . H42 H 0.3635 0.7486 0.0877 0.110 Uiso 1 1 calc R . . C43 C 0.2141(9) 0.7263(6) 0.0206(6) 0.084(3) Uani 1 1 d . . . H43 H 0.2093 0.6560 -0.0076 0.100 Uiso 1 1 calc R . . C44 C 0.5901(9) 0.4748(7) 0.0428(7) 0.102(3) Uani 1 1 d . . . C45 C 0.5152(8) 0.3993(6) -0.0273(6) 0.084(2) Uani 1 1 d . . . C46 C 0.4260(7) 0.4274(6) -0.0732(6) 0.080(2) 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 0.03548(15) 0.02886(11) 0.04678(13) 0.00862(8) 0.00702(10) 0.00142(8) S1 0.0499(10) 0.0383(7) 0.0509(8) 0.0070(6) 0.0062(7) -0.0047(6) O1 0.041(2) 0.0333(17) 0.0453(19) 0.0155(14) 0.0034(17) 0.0008(15) O2 0.044(3) 0.0368(18) 0.0479(19) 0.0141(15) 0.0017(18) 0.0038(16) O3 0.088(4) 0.042(2) 0.078(3) 0.024(2) 0.005(3) 0.003(2) O4 0.060(3) 0.063(3) 0.068(3) -0.005(2) 0.024(2) -0.020(2) O5 0.069(3) 0.060(3) 0.055(2) -0.0012(19) 0.013(2) -0.012(2) N1 0.036(3) 0.034(2) 0.043(2) 0.0101(17) 0.006(2) -0.0010(18) N2 0.033(3) 0.034(2) 0.044(2) 0.0104(17) 0.005(2) 0.0015(18) N3 0.032(3) 0.031(2) 0.047(2) 0.0096(17) 0.004(2) 0.0012(17) N4 0.035(3) 0.036(2) 0.047(2) 0.0075(18) 0.010(2) 0.0042(19) N5 0.034(3) 0.028(2) 0.049(2) 0.0077(17) 0.004(2) -0.0034(18) N6 0.038(3) 0.037(2) 0.046(2) 0.0098(18) 0.002(2) 0.0018(19) N7 0.033(3) 0.037(2) 0.048(2) 0.0130(19) 0.003(2) 0.0054(19) N8 0.044(3) 0.037(2) 0.052(3) 0.015(2) 0.009(2) -0.001(2) N9 0.057(4) 0.051(3) 0.041(2) 0.015(2) 0.012(2) 0.010(2) N10 0.118(8) 0.087(5) 0.092(5) 0.014(4) 0.011(5) 0.001(5) F1 0.128(4) 0.077(2) 0.107(3) 0.037(2) 0.007(3) 0.038(2) F2 0.079(3) 0.149(4) 0.108(3) 0.044(3) 0.032(3) 0.024(3) F3 0.075(3) 0.086(3) 0.064(2) 0.004(2) -0.009(2) 0.017(2) C1 0.041(4) 0.036(3) 0.052(3) 0.016(2) 0.012(3) 0.004(2) C2 0.038(3) 0.034(3) 0.049(3) 0.011(2) 0.011(3) -0.002(2) C3 0.055(4) 0.046(3) 0.049(3) 0.009(2) 0.008(3) -0.011(3) C4 0.058(4) 0.052(3) 0.045(3) 0.005(2) 0.009(3) -0.006(3) C5 0.051(4) 0.039(3) 0.046(3) 0.001(2) 0.001(3) -0.006(3) C6 0.042(4) 0.034(3) 0.044(3) 0.009(2) 0.007(3) 0.006(2) C7 0.030(3) 0.034(3) 0.050(3) 0.011(2) 0.001(2) 0.003(2) C8 0.050(4) 0.037(3) 0.044(3) 0.001(2) 0.002(3) -0.005(2) C9 0.051(4) 0.043(3) 0.054(3) 0.004(2) 0.005(3) -0.007(3) C10 0.040(4) 0.035(3) 0.063(3) 0.009(2) 0.012(3) -0.005(2) C11 0.034(3) 0.036(3) 0.053(3) 0.012(2) 0.005(3) 0.003(2) C12 0.033(3) 0.033(2) 0.055(3) 0.012(2) 0.005(3) 0.002(2) C13 0.037(3) 0.029(2) 0.047(3) 0.009(2) 0.003(3) 0.005(2) C14 0.035(3) 0.031(2) 0.053(3) 0.013(2) 0.004(3) 0.002(2) C15 0.050(4) 0.036(3) 0.057(3) 0.013(2) 0.010(3) -0.007(3) C16 0.074(5) 0.051(3) 0.068(4) 0.015(3) 0.007(4) -0.018(3) C17 0.066(5) 0.070(4) 0.056(4) 0.008(3) 0.006(3) -0.036(4) C18 0.047(4) 0.032(3) 0.050(3) 0.009(2) 0.005(3) -0.005(2) C19 0.054(4) 0.054(3) 0.067(4) 0.028(3) 0.014(3) 0.008(3) C20 0.049(4) 0.068(4) 0.089(5) 0.042(4) 0.016(4) 0.003(3) C21 0.055(4) 0.045(3) 0.056(3) 0.008(2) -0.004(3) 0.007(3) C22 0.064(5) 0.038(3) 0.061(4) 0.006(2) 0.001(3) 0.014(3) C23 0.038(3) 0.034(3) 0.052(3) 0.013(2) 0.010(3) 0.008(2) C24 0.038(3) 0.034(3) 0.056(3) 0.015(2) 0.007(3) 0.002(2) C25 0.058(4) 0.046(3) 0.056(3) 0.017(3) 0.011(3) -0.006(3) C26 0.119(5) 0.105(4) 0.095(4) 0.034(4) 0.037(4) -0.023(4) C27 0.115(5) 0.110(5) 0.098(4) 0.019(3) 0.048(4) -0.022(4) C28 0.051(4) 0.047(3) 0.052(3) 0.011(2) 0.013(3) -0.001(3) C29 0.073(4) 0.067(3) 0.108(4) 0.047(3) 0.011(3) -0.004(3) C30 0.044(4) 0.063(4) 0.110(6) 0.042(4) 0.025(4) 0.005(3) C31 0.090(7) 0.088(5) 0.050(4) 0.019(3) 0.009(4) 0.035(4) C32 0.093(7) 0.086(5) 0.055(4) -0.009(3) -0.009(4) 0.056(4) C33 0.054(5) 0.058(4) 0.066(4) 0.008(3) 0.004(3) 0.018(3) C34 0.073(6) 0.062(4) 0.072(4) 0.008(3) 0.009(4) 0.021(3) C35 0.079(6) 0.059(4) 0.061(4) 0.007(3) 0.010(4) 0.006(4) C36 0.103(7) 0.060(4) 0.066(4) 0.014(3) -0.009(4) 0.006(4) C37 0.088(6) 0.046(3) 0.055(4) 0.008(3) -0.002(4) 0.007(3) C38 0.058(5) 0.066(4) 0.075(4) 0.026(3) 0.017(4) 0.011(3) C39 0.071(6) 0.063(4) 0.082(5) 0.010(4) -0.014(4) 0.018(4) C40 0.092(5) 0.065(4) 0.105(4) 0.025(3) 0.000(4) 0.007(3) C41 0.081(5) 0.104(5) 0.112(5) 0.044(4) 0.009(4) -0.003(4) C42 0.065(6) 0.105(7) 0.108(7) 0.038(6) 0.021(5) 0.023(5) C43 0.107(8) 0.068(5) 0.079(5) 0.025(4) 0.020(5) 0.036(5) C44 0.118(9) 0.082(6) 0.105(6) 0.032(5) 0.036(6) -0.015(6) C45 0.072(6) 0.098(6) 0.072(5) 0.026(4) 0.012(4) -0.008(5) C46 0.070(6) 0.080(5) 0.092(6) 0.029(4) 0.024(5) 0.012(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 1.816(4) . ? U O2 1.822(4) . ? U N9 2.533(4) . ? U N1 2.562(4) . ? U N4 2.570(4) . ? U N2 2.606(4) . ? U N3 2.611(4) . ? S1 O3 1.430(4) . ? S1 O5 1.441(4) . ? S1 O4 1.442(4) . ? S1 C38 1.855(9) . ? N1 C1 1.331(7) . ? N1 N5 1.351(6) . ? N2 C2 1.346(6) . ? N2 C6 1.377(6) . ? N3 C7 1.355(6) . ? N3 C11 1.356(6) . ? N4 C12 1.331(6) . ? N4 N7 1.344(6) . ? N5 C13 1.310(6) . ? N6 C1 1.331(6) . ? N6 C14 1.342(6) . ? N7 C23 1.328(6) . ? N8 C24 1.319(7) . ? N8 C12 1.341(6) . ? N9 C37 1.326(8) . ? N9 C33 1.361(7) . ? N10 C39 1.332(10) . ? N10 C43 1.423(11) . ? F1 C38 1.282(8) . ? F2 C38 1.303(8) . ? F3 C38 1.354(8) . ? C1 C2 1.482(7) . ? C2 C3 1.395(7) . ? C3 C4 1.391(7) . ? C3 H3 0.9300 . ? C4 C5 1.372(7) . ? C4 H4 0.9300 . ? C5 C6 1.379(7) . ? C5 H5 0.9300 . ? C6 C7 1.479(7) . ? C7 C8 1.396(7) . ? C8 C9 1.382(7) . ? C8 H8 0.9300 . ? C9 C10 1.374(7) . ? C9 H9 0.9300 . ? C10 C11 1.385(7) . ? C10 H10 0.9300 . ? C11 C12 1.498(7) . ? C13 C14 1.431(7) . ? C13 C18 1.532(7) . ? C14 C15 1.522(7) . ? C15 C20 1.515(9) . ? C15 C19 1.521(9) . ? C15 C16 1.532(8) . ? C16 C17 1.458(6) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.548(7) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C22 1.516(8) . ? C18 C21 1.522(8) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.420(7) . ? C23 C28 1.521(8) . ? C24 C25 1.508(7) . ? C25 C26 1.450(9) . ? C25 C30 1.528(10) . ? C25 C29 1.554(10) . ? C26 C27 1.468(12) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.494(11) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C32 1.483(8) . ? C28 C31 1.515(10) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C34 1.358(9) . ? C33 H33 0.9300 . ? C34 C35 1.373(10) . ? C34 H34 0.9300 . ? C35 C36 1.368(10) . ? C35 H35 0.9300 . ? C36 C37 1.377(9) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C39 C40 1.386(12) . ? C39 H39 0.9300 . ? C40 C41 1.317(14) . ? C40 H40 0.9300 . ? C41 C42 1.297(13) . ? C41 H41 0.9300 . ? C42 C43 1.283(12) . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? C44 C46 1.345(11) 2_665 ? C44 C45 1.362(12) . ? C45 C46 1.372(12) . ? C46 C44 1.345(11) 2_665 ? 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 178.25(13) . . ? O1 U N9 90.11(16) . . ? O2 U N9 88.37(16) . . ? O1 U N1 90.79(15) . . ? O2 U N1 88.17(16) . . ? N9 U N1 83.62(14) . . ? O1 U N4 86.66(15) . . ? O2 U N4 94.16(16) . . ? N9 U N4 88.05(14) . . ? N1 U N4 171.29(13) . . ? O1 U N2 92.07(15) . . ? O2 U N2 88.70(15) . . ? N9 U N2 146.05(13) . . ? N1 U N2 62.48(12) . . ? N4 U N2 125.90(12) . . ? O1 U N3 89.03(14) . . ? O2 U N3 92.72(15) . . ? N9 U N3 150.80(14) . . ? N1 U N3 125.57(13) . . ? N4 U N3 62.76(12) . . ? N2 U N3 63.14(12) . . ? O3 S1 O5 116.6(3) . . ? O3 S1 O4 114.7(3) . . ? O5 S1 O4 115.5(2) . . ? O3 S1 C38 101.9(3) . . ? O5 S1 C38 101.9(3) . . ? O4 S1 C38 103.0(3) . . ? C1 N1 N5 119.1(4) . . ? C1 N1 U 123.3(3) . . ? N5 N1 U 117.5(3) . . ? C2 N2 C6 118.1(4) . . ? C2 N2 U 120.4(3) . . ? C6 N2 U 120.9(3) . . ? C7 N3 C11 117.8(4) . . ? C7 N3 U 121.1(3) . . ? C11 N3 U 120.9(3) . . ? C12 N4 N7 118.7(4) . . ? C12 N4 U 123.1(3) . . ? N7 N4 U 118.1(3) . . ? C13 N5 N1 118.8(4) . . ? C1 N6 C14 116.3(4) . . ? C23 N7 N4 118.9(4) . . ? C24 N8 C12 116.7(4) . . ? C37 N9 C33 114.6(5) . . ? C37 N9 U 122.6(4) . . ? C33 N9 U 121.2(4) . . ? C39 N10 C43 119.9(8) . . ? N1 C1 N6 125.5(5) . . ? N1 C1 C2 116.1(4) . . ? N6 C1 C2 118.3(4) . . ? N2 C2 C3 122.7(5) . . ? N2 C2 C1 117.1(4) . . ? C3 C2 C1 120.2(4) . . ? C4 C3 C2 118.3(5) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C5 C4 C3 119.3(5) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 120.3(5) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.8 . . ? N2 C6 C5 121.2(4) . . ? N2 C6 C7 116.6(4) . . ? C5 C6 C7 122.2(5) . . ? N3 C7 C8 121.7(4) . . ? N3 C7 C6 117.7(4) . . ? C8 C7 C6 120.7(5) . . ? C9 C8 C7 119.2(5) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C10 C9 C8 119.7(5) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C11 118.6(5) . . ? C9 C10 H10 120.7 . . ? C11 C10 H10 120.7 . . ? N3 C11 C10 123.0(5) . . ? N3 C11 C12 116.3(4) . . ? C10 C11 C12 120.7(5) . . ? N4 C12 N8 125.3(5) . . ? N4 C12 C11 116.8(4) . . ? N8 C12 C11 117.9(4) . . ? N5 C13 C14 121.2(4) . . ? N5 C13 C18 115.5(4) . . ? C14 C13 C18 123.3(4) . . ? N6 C14 C13 119.1(4) . . ? N6 C14 C15 117.0(5) . . ? C13 C14 C15 123.9(5) . . ? C20 C15 C19 110.4(5) . . ? C20 C15 C14 109.2(5) . . ? C19 C15 C14 109.1(5) . . ? C20 C15 C16 111.7(6) . . ? C19 C15 C16 106.8(5) . . ? C14 C15 C16 109.6(4) . . ? C17 C16 C15 115.9(5) . . ? C17 C16 H16A 108.3 . . ? C15 C16 H16A 108.3 . . ? C17 C16 H16B 108.3 . . ? C15 C16 H16B 108.3 . . ? H16A C16 H16B 107.4 . . ? C16 C17 C18 115.8(5) . . ? C16 C17 H17A 108.3 . . ? C18 C17 H17A 108.3 . . ? C16 C17 H17B 108.3 . . ? C18 C17 H17B 108.3 . . ? H17A C17 H17B 107.4 . . ? C22 C18 C21 109.4(5) . . ? C22 C18 C13 107.7(5) . . ? C21 C18 C13 109.5(4) . . ? C22 C18 C17 112.7(5) . . ? C21 C18 C17 109.1(5) . . ? C13 C18 C17 108.5(4) . . ? C15 C19 H19A 109.5 . . ? C15 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C15 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N7 C23 C24 120.7(5) . . ? N7 C23 C28 114.9(4) . . ? C24 C23 C28 124.4(4) . . ? N8 C24 C23 119.7(5) . . ? N8 C24 C25 117.3(5) . . ? C23 C24 C25 122.9(5) . . ? C26 C25 C24 113.0(5) . . ? C26 C25 C30 106.0(7) . . ? C24 C25 C30 109.5(5) . . ? C26 C25 C29 111.2(7) . . ? C24 C25 C29 107.6(6) . . ? C30 C25 C29 109.5(5) . . ? C25 C26 C27 123.6(7) . . ? C25 C26 H26A 106.4 . . ? C27 C26 H26A 106.4 . . ? C25 C26 H26B 106.4 . . ? C27 C26 H26B 106.4 . . ? H26A C26 H26B 106.5 . . ? C26 C27 C28 122.3(6) . . ? C26 C27 H27A 106.7 . . ? C28 C27 H27A 106.7 . . ? C26 C27 H27B 106.7 . . ? C28 C27 H27B 106.7 . . ? H27A C27 H27B 106.6 . . ? C32 C28 C27 111.1(7) . . ? C32 C28 C31 108.6(5) . . ? C27 C28 C31 105.8(6) . . ? C32 C28 C23 109.7(5) . . ? C27 C28 C23 111.3(5) . . ? C31 C28 C23 110.2(5) . . ? C25 C29 H29A 109.5 . . ? C25 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C25 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C28 C32 H32A 109.5 . . ? C28 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C28 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 N9 124.9(7) . . ? C34 C33 H33 117.5 . . ? N9 C33 H33 117.5 . . ? C33 C34 C35 118.3(7) . . ? C33 C34 H34 120.8 . . ? C35 C34 H34 120.8 . . ? C36 C35 C34 118.7(7) . . ? C36 C35 H35 120.6 . . ? C34 C35 H35 120.6 . . ? C35 C36 C37 118.9(8) . . ? C35 C36 H36 120.6 . . ? C37 C36 H36 120.6 . . ? N9 C37 C36 124.4(7) . . ? N9 C37 H37 117.8 . . ? C36 C37 H37 117.8 . . ? F1 C38 F2 109.6(7) . . ? F1 C38 F3 105.6(6) . . ? F2 C38 F3 108.1(6) . . ? F1 C38 S1 112.6(6) . . ? F2 C38 S1 111.4(5) . . ? F3 C38 S1 109.2(5) . . ? N10 C39 C40 116.7(9) . . ? N10 C39 H39 121.7 . . ? C40 C39 H39 121.7 . . ? C41 C40 C39 119.8(9) . . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? C42 C41 C40 123.5(10) . . ? C42 C41 H41 118.2 . . ? C40 C41 H41 118.2 . . ? C43 C42 C41 119.9(10) . . ? C43 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? C42 C43 N10 119.8(8) . . ? C42 C43 H43 120.1 . . ? N10 C43 H43 120.1 . . ? C46 C44 C45 122.0(11) 2_665 . ? C44 C45 C46 117.5(9) . . ? C44 C46 C45 120.2(8) 2_665 . ? #===END data_19 _database_code_depnum_ccdc_archive 'CCDC 711343' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H20 F3 N4 O5 S U' _chemical_formula_sum 'C21 H20 F3 N4 O5 S U' _chemical_formula_weight 735.50 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 '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 13.2614(8) _cell_length_b 12.2270(10) _cell_length_c 15.2571(10) _cell_angle_alpha 90.00 _cell_angle_beta 98.720(5) _cell_angle_gamma 90.00 _cell_volume 2445.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 40910 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent dark red' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.998 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1396 _exptl_absorpt_coefficient_mu 6.785 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.470 _exptl_absorpt_correction_T_max 0.666 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 30 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 area-detector diffractometer' _diffrn_measurement_method 'two \f and five \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 40910 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.68 _reflns_number_total 2317 _reflns_number_gt 1801 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by Patterson map interpretation and subsequent Fourier-difference synthesis. The triflate ion is disordered over two equally populated positions related by the binary axis and sharing atoms O2 and F1. All non-hydrogen atoms were refined with anisotropic displacement parameters, with some restraints for some C atoms of the pyridine rings. One pyridine molecule was refined as an idealized hexagon and a restraint was applied on the S1-C11 bond length. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. The large displacement parameters of several C atoms of the pyridine rings, as well as a close O4...C6 contact, likely indicates some unresolved disorder of the pyridine molecules. 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^)+(0.0456P)^2^+25.2918P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00097(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2317 _refine_ls_number_parameters 176 _refine_ls_number_restraints 43 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0964 _refine_ls_wR_factor_gt 0.0890 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.483 _refine_diff_density_min -1.424 _refine_diff_density_rms 0.174 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 0.99700(3) 0.7500 0.02845(18) Uani 1 2 d S . . S1 S 0.0424(3) 0.6962(3) 0.7258(2) 0.0296(8) Uani 0.50 1 d PD . . O1 O 0.0873(4) 1.0005(5) 0.6679(4) 0.0412(14) Uani 1 1 d . . . O2 O 0.0000 0.7905(6) 0.7500 0.046(2) Uani 1 2 d S . . O3 O 0.0353(9) 0.6841(11) 0.6313(7) 0.043(3) Uani 0.50 1 d P . . O4 O 0.1412(8) 0.6793(10) 0.7787(7) 0.038(3) Uani 0.50 1 d P . . F1 F 0.0000 0.4862(5) 0.7500 0.059(2) Uani 1 2 d S . . F2 F -0.1282(7) 0.5849(8) 0.7117(6) 0.042(2) Uani 0.50 1 d P . . F3 F -0.0423(7) 0.5866(8) 0.8439(6) 0.043(2) Uani 0.50 1 d P . . N1 N 0.1526(5) 0.9413(5) 0.8700(4) 0.0326(14) Uani 1 1 d . . . C1 C 0.2465(8) 0.9342(11) 0.8517(7) 0.069(3) Uani 1 1 d U . . H1 H 0.2574 0.9480 0.7939 0.082 Uiso 1 1 calc R . . C2 C 0.3295(8) 0.9075(11) 0.9141(7) 0.073(3) Uani 1 1 d U . . H2 H 0.3941 0.9025 0.8976 0.087 Uiso 1 1 calc R . . C3 C 0.3169(6) 0.8884(7) 1.0000(6) 0.044(2) Uani 1 1 d . . . H3 H 0.3716 0.8706 1.0432 0.053 Uiso 1 1 calc R . . C4 C 0.2200(7) 0.8965(8) 1.0193(6) 0.049(2) Uani 1 1 d . . . H4 H 0.2072 0.8855 1.0769 0.059 Uiso 1 1 calc R . . C5 C 0.1419(6) 0.9212(8) 0.9527(6) 0.046(2) Uani 1 1 d . . . H5 H 0.0763 0.9239 0.9672 0.055 Uiso 1 1 calc R . . N2 N 0.0860(4) 1.1695(4) 0.8265(4) 0.0476(19) Uani 1 1 d G . . C6 C 0.1748(5) 1.2111(6) 0.8012(4) 0.069(3) Uani 1 1 d GU . . H6 H 0.1991 1.1827 0.7518 0.082 Uiso 1 1 calc R . . C7 C 0.2274(5) 1.2951(6) 0.8497(7) 0.107(5) Uani 1 1 d GU . . H7 H 0.2868 1.3229 0.8328 0.129 Uiso 1 1 calc R . . C8 C 0.1911(7) 1.3375(5) 0.9235(7) 0.121(5) Uani 1 1 d GU . . H8 H 0.2262 1.3937 0.9560 0.146 Uiso 1 1 calc R . . C9 C 0.1023(7) 1.2959(7) 0.9488(5) 0.116(5) Uani 1 1 d GU . . H9 H 0.0780 1.3243 0.9981 0.139 Uiso 1 1 calc R . . C10 C 0.0497(5) 1.2119(6) 0.9002(4) 0.071(3) Uani 1 1 d GU . . H10 H -0.0097 1.1841 0.9171 0.085 Uiso 1 1 calc R . . C11 C -0.0326(10) 0.5851(11) 0.7562(10) 0.035(4) Uani 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.0267(2) 0.0280(3) 0.0316(2) 0.000 0.00745(14) 0.000 S1 0.0275(17) 0.0326(19) 0.0296(18) 0.0005(15) 0.0064(14) -0.0019(16) O1 0.035(3) 0.057(4) 0.032(3) -0.010(3) 0.009(2) 0.003(3) O2 0.062(6) 0.026(4) 0.047(5) 0.000 0.002(4) 0.000 O3 0.044(7) 0.058(8) 0.028(6) -0.003(5) 0.010(5) -0.012(6) O4 0.036(6) 0.041(7) 0.037(6) 0.006(5) 0.006(5) -0.001(5) F1 0.065(5) 0.026(4) 0.084(6) 0.000 0.002(4) 0.000 F2 0.029(5) 0.051(6) 0.044(5) 0.002(5) 0.004(4) -0.008(4) F3 0.052(6) 0.049(6) 0.030(5) 0.004(4) 0.011(4) -0.014(5) N1 0.030(3) 0.032(3) 0.035(3) -0.003(3) 0.002(3) 0.001(3) C1 0.048(5) 0.104(7) 0.056(5) 0.010(5) 0.016(4) 0.024(5) C2 0.043(5) 0.113(8) 0.063(6) 0.014(6) 0.012(5) 0.016(5) C3 0.033(4) 0.045(5) 0.051(5) -0.009(4) -0.002(4) 0.009(4) C4 0.038(5) 0.071(6) 0.040(5) 0.009(4) 0.010(4) 0.004(5) C5 0.023(4) 0.071(6) 0.045(5) 0.012(4) 0.011(3) 0.001(4) N2 0.056(5) 0.029(3) 0.052(4) 0.004(3) -0.011(4) -0.002(3) C6 0.053(5) 0.051(5) 0.091(7) 0.023(5) -0.023(5) -0.019(5) C7 0.077(7) 0.077(7) 0.149(9) 0.030(7) -0.043(7) -0.018(6) C8 0.116(9) 0.073(7) 0.151(10) -0.011(7) -0.058(8) 0.022(7) C9 0.128(9) 0.086(8) 0.115(8) -0.044(7) -0.039(7) 0.053(7) C10 0.085(7) 0.053(5) 0.065(6) -0.020(5) -0.019(5) 0.028(5) C11 0.021(8) 0.055(10) 0.027(7) -0.007(7) -0.002(7) -0.005(6) _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 1.831(6) . ? U O1 1.831(6) 2_556 ? U O2 2.525(8) . ? U N2 2.590(5) . ? U N2 2.590(4) 2_556 ? U N1 2.605(6) 2_556 ? U N1 2.605(6) . ? S1 O2 1.359(7) . ? S1 O3 1.437(11) . ? S1 O4 1.446(11) . ? S1 C11 1.786(9) . ? F1 C11 1.292(15) . ? F2 C11 1.345(16) . ? F3 C11 1.364(17) . ? N1 C5 1.316(10) . ? N1 C1 1.321(11) . ? C1 C2 1.381(14) . ? C1 H1 0.9300 . ? C2 C3 1.367(13) . ? C2 H2 0.9300 . ? C3 C4 1.364(12) . ? C3 H3 0.9300 . ? C4 C5 1.370(11) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? N2 C6 1.3900 . ? N2 C10 1.3900 . ? C6 C7 1.3900 . ? C6 H6 0.9300 . ? C7 C8 1.3900 . ? C7 H7 0.9300 . ? C8 C9 1.3900 . ? C8 H8 0.9300 . ? C9 C10 1.3900 . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? 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 177.3(3) . 2_556 ? O1 U O2 91.34(17) . . ? O1 U O2 91.34(17) 2_556 . ? O1 U N2 90.5(2) . . ? O1 U N2 87.4(2) 2_556 . ? O2 U N2 144.52(12) . . ? O1 U N2 87.4(2) . 2_556 ? O1 U N2 90.5(2) 2_556 2_556 ? O2 U N2 144.52(12) . 2_556 ? N2 U N2 71.0(2) . 2_556 ? O1 U N1 91.7(2) . 2_556 ? O1 U N1 89.0(2) 2_556 2_556 ? O2 U N1 74.85(14) . 2_556 ? N2 U N1 140.50(18) . 2_556 ? N2 U N1 69.76(19) 2_556 2_556 ? O1 U N1 89.0(2) . . ? O1 U N1 91.7(2) 2_556 . ? O2 U N1 74.85(14) . . ? N2 U N1 69.76(19) . . ? N2 U N1 140.50(18) 2_556 . ? N1 U N1 149.7(3) 2_556 . ? O2 S1 O3 113.1(6) . . ? O2 S1 O4 110.3(5) . . ? O3 S1 O4 117.5(7) . . ? O2 S1 C11 107.8(6) . . ? O3 S1 C11 103.1(7) . . ? O4 S1 C11 103.9(7) . . ? S1 O2 U 148.1(2) . . ? C5 N1 C1 115.7(8) . . ? C5 N1 U 122.6(5) . . ? C1 N1 U 121.8(6) . . ? N1 C1 C2 123.3(10) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C3 C2 C1 120.0(10) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C4 C3 C2 116.8(8) . . ? C4 C3 H3 121.6 . . ? C2 C3 H3 121.6 . . ? C3 C4 C5 119.2(8) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N1 C5 C4 124.9(8) . . ? N1 C5 H5 117.5 . . ? C4 C5 H5 117.5 . . ? C6 N2 C10 120.0 . . ? C6 N2 U 120.5(3) . . ? C10 N2 U 119.1(4) . . ? N2 C6 C7 120.0 . . ? N2 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C8 C7 C6 120.0 . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C9 C8 C7 120.0 . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C10 C9 C8 120.0 . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 N2 120.0 . . ? C9 C10 H10 120.0 . . ? N2 C10 H10 120.0 . . ? F1 C11 F2 105.2(10) . . ? F1 C11 F3 99.6(10) . . ? F2 C11 F3 105.8(11) . . ? F1 C11 S1 119.2(9) . . ? F2 C11 S1 112.9(9) . . ? F3 C11 S1 112.5(9) . . ? #===END data_UO~2~Cl~2~(py)~3~ _database_code_depnum_ccdc_archive 'CCDC 711344' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H15 Cl2 N3 O2 U' _chemical_formula_sum 'C15 H15 Cl2 N3 O2 U' _chemical_formula_weight 578.23 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' Cl Cl 0.1484 0.1585 '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 11.1335(8) _cell_length_b 13.0944(9) _cell_length_c 13.2043(6) _cell_angle_alpha 90.00 _cell_angle_beta 112.600(4) _cell_angle_gamma 90.00 _cell_volume 1777.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 51854 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.161 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 9.445 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.333 _exptl_absorpt_correction_T_max 0.624 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 30 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 area-detector diffractometer' _diffrn_measurement_method 'two \f and three \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 51854 _diffrn_reflns_av_R_equivalents 0.0484 _diffrn_reflns_av_sigmaI/netI 0.0499 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.68 _reflns_number_total 3363 _reflns_number_gt 2968 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _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 and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 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^)+(0.0483P)^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 3363 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0786 _refine_ls_wR_factor_gt 0.0762 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.379 _refine_diff_density_min -2.085 _refine_diff_density_rms 0.171 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 0.260852(17) 0.523234(13) 0.284188(13) 0.02289(9) Uani 1 1 d . . . Cl1 Cl 0.50265(12) 0.54145(9) 0.27822(9) 0.0260(2) Uani 1 1 d . . . Cl2 Cl 0.03874(11) 0.41468(10) 0.22218(9) 0.0286(3) Uani 1 1 d . . . O1 O 0.1822(3) 0.6155(3) 0.1826(2) 0.0272(7) Uani 1 1 d . . . O2 O 0.3341(3) 0.4323(3) 0.3884(3) 0.0262(7) Uani 1 1 d . . . N1 N 0.2542(4) 0.4129(3) 0.1219(3) 0.0250(9) Uani 1 1 d . . . N2 N 0.3595(4) 0.6876(3) 0.3934(3) 0.0256(9) Uani 1 1 d . . . N3 N 0.1475(4) 0.5817(3) 0.4104(3) 0.0250(9) Uani 1 1 d . . . C1 C 0.1848(5) 0.4429(4) 0.0178(4) 0.0266(10) Uani 1 1 d . . . H1 H 0.1423 0.5055 0.0058 0.032 Uiso 1 1 calc R . . C2 C 0.1748(5) 0.3830(4) -0.0722(4) 0.0300(11) Uani 1 1 d . . . H2 H 0.1268 0.4058 -0.1430 0.036 Uiso 1 1 calc R . . C3 C 0.2366(5) 0.2897(4) -0.0556(4) 0.0320(12) Uani 1 1 d . . . H3 H 0.2301 0.2486 -0.1149 0.038 Uiso 1 1 calc R . . C4 C 0.3090(5) 0.2580(4) 0.0510(4) 0.0314(11) Uani 1 1 d . . . H4 H 0.3524 0.1958 0.0648 0.038 Uiso 1 1 calc R . . C5 C 0.3143(5) 0.3219(4) 0.1359(4) 0.0295(11) Uani 1 1 d . . . H5 H 0.3625 0.3005 0.2072 0.035 Uiso 1 1 calc R . . C6 C 0.3460(5) 0.7766(4) 0.3395(4) 0.0283(11) Uani 1 1 d . . . H6 H 0.3165 0.7750 0.2634 0.034 Uiso 1 1 calc R . . C7 C 0.3736(5) 0.8705(4) 0.3911(4) 0.0305(11) Uani 1 1 d . . . H7 H 0.3633 0.9304 0.3508 0.037 Uiso 1 1 calc R . . C8 C 0.4172(5) 0.8727(5) 0.5050(4) 0.0327(12) Uani 1 1 d . . . H8 H 0.4340 0.9348 0.5422 0.039 Uiso 1 1 calc R . . C9 C 0.4352(5) 0.7832(4) 0.5614(4) 0.0308(11) Uani 1 1 d . . . H9 H 0.4662 0.7836 0.6377 0.037 Uiso 1 1 calc R . . C10 C 0.4070(5) 0.6916(4) 0.5048(4) 0.0286(11) Uani 1 1 d . . . H10 H 0.4210 0.6309 0.5443 0.034 Uiso 1 1 calc R . . C11 C 0.0764(5) 0.6681(4) 0.3900(4) 0.0277(11) Uani 1 1 d . . . H11 H 0.0571 0.7009 0.3231 0.033 Uiso 1 1 calc R . . C12 C 0.0308(5) 0.7100(4) 0.4649(4) 0.0320(12) Uani 1 1 d . . . H12 H -0.0180 0.7698 0.4484 0.038 Uiso 1 1 calc R . . C13 C 0.0589(5) 0.6615(4) 0.5648(4) 0.0306(12) Uani 1 1 d . . . H13 H 0.0304 0.6884 0.6168 0.037 Uiso 1 1 calc R . . C14 C 0.1300(5) 0.5726(4) 0.5850(4) 0.0293(11) Uani 1 1 d . . . H14 H 0.1485 0.5378 0.6506 0.035 Uiso 1 1 calc R . . C15 C 0.1739(5) 0.5351(4) 0.5080(4) 0.0275(11) Uani 1 1 d . . . H15 H 0.2235 0.4756 0.5236 0.033 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 0.02814(12) 0.01961(17) 0.02227(12) 0.00059(6) 0.01119(8) 0.00150(7) Cl1 0.0319(6) 0.0251(6) 0.0225(5) -0.0002(5) 0.0120(5) -0.0005(5) Cl2 0.0324(6) 0.0273(7) 0.0287(6) -0.0030(5) 0.0144(5) -0.0038(5) O1 0.0294(18) 0.0228(19) 0.0241(16) 0.0007(14) 0.0045(14) 0.0029(16) O2 0.0329(18) 0.0191(19) 0.0286(16) 0.0021(15) 0.0141(14) 0.0025(16) N1 0.028(2) 0.026(2) 0.0228(19) -0.0022(17) 0.0114(16) -0.0030(19) N2 0.030(2) 0.022(2) 0.026(2) 0.0002(17) 0.0118(17) 0.0007(18) N3 0.027(2) 0.023(2) 0.0278(19) -0.0017(17) 0.0133(16) -0.0021(18) C1 0.031(3) 0.020(3) 0.030(2) 0.001(2) 0.013(2) 0.001(2) C2 0.037(3) 0.027(3) 0.028(2) -0.003(2) 0.014(2) -0.001(2) C3 0.036(3) 0.030(3) 0.034(3) -0.008(2) 0.017(2) -0.004(2) C4 0.033(3) 0.024(3) 0.041(3) -0.003(2) 0.018(2) 0.002(2) C5 0.030(3) 0.032(3) 0.027(2) 0.002(2) 0.011(2) 0.001(2) C6 0.035(3) 0.027(3) 0.024(2) 0.001(2) 0.013(2) -0.002(2) C7 0.036(3) 0.026(3) 0.031(2) 0.006(2) 0.014(2) 0.004(2) C8 0.031(3) 0.027(3) 0.040(3) -0.008(2) 0.013(2) 0.000(2) C9 0.031(3) 0.034(3) 0.028(2) -0.002(2) 0.012(2) -0.002(2) C10 0.029(3) 0.030(3) 0.029(2) 0.001(2) 0.013(2) -0.001(2) C11 0.032(3) 0.026(3) 0.026(2) 0.003(2) 0.012(2) 0.002(2) C12 0.032(3) 0.026(3) 0.039(3) 0.000(2) 0.015(2) 0.004(2) C13 0.036(3) 0.031(3) 0.030(2) -0.005(2) 0.019(2) -0.002(2) C14 0.034(3) 0.030(3) 0.026(2) 0.000(2) 0.013(2) -0.003(2) C15 0.029(3) 0.027(3) 0.031(3) 0.002(2) 0.016(2) 0.001(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 O2 1.764(3) . ? U O1 1.767(3) . ? U N1 2.561(4) . ? U N3 2.563(4) . ? U N2 2.588(4) . ? U Cl2 2.6926(12) . ? U Cl1 2.7338(12) . ? N1 C5 1.345(7) . ? N1 C1 1.351(6) . ? N2 C6 1.345(6) . ? N2 C10 1.360(6) . ? N3 C11 1.347(7) . ? N3 C15 1.352(6) . ? C1 C2 1.392(7) . ? C1 H1 0.9300 . ? C2 C3 1.377(8) . ? C2 H2 0.9300 . ? C3 C4 1.390(7) . ? C3 H3 0.9300 . ? C4 C5 1.380(7) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.381(8) . ? C6 H6 0.9300 . ? C7 C8 1.392(7) . ? C7 H7 0.9300 . ? C8 C9 1.363(8) . ? C8 H8 0.9300 . ? C9 C10 1.383(7) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.387(7) . ? C11 H11 0.9300 . ? C12 C13 1.387(7) . ? C12 H12 0.9300 . ? C13 C14 1.375(8) . ? C13 H13 0.9300 . ? C14 C15 1.377(7) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? 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 O1 177.36(14) . . ? O2 U N1 97.33(14) . . ? O1 U N1 84.50(14) . . ? O2 U N3 83.70(14) . . ? O1 U N3 93.73(14) . . ? N1 U N3 148.09(13) . . ? O2 U N2 99.00(14) . . ? O1 U N2 80.50(14) . . ? N1 U N2 143.58(12) . . ? N3 U N2 66.36(12) . . ? O2 U Cl2 88.64(11) . . ? O1 U Cl2 90.05(12) . . ? N1 U Cl2 73.74(9) . . ? N3 U Cl2 74.41(9) . . ? N2 U Cl2 138.74(9) . . ? O2 U Cl1 85.18(11) . . ? O1 U Cl1 97.16(11) . . ? N1 U Cl1 74.77(9) . . ? N3 U Cl1 136.80(9) . . ? N2 U Cl1 74.45(9) . . ? Cl2 U Cl1 146.80(4) . . ? C5 N1 C1 117.1(4) . . ? C5 N1 U 122.2(3) . . ? C1 N1 U 120.6(3) . . ? C6 N2 C10 117.2(5) . . ? C6 N2 U 119.3(3) . . ? C10 N2 U 122.7(3) . . ? C11 N3 C15 117.8(4) . . ? C11 N3 U 121.3(3) . . ? C15 N3 U 120.2(3) . . ? N1 C1 C2 122.2(5) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 119.5(5) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 119.0(5) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 118.0(5) . . ? C5 C4 H4 121.0 . . ? C3 C4 H4 121.0 . . ? N1 C5 C4 124.2(5) . . ? N1 C5 H5 117.9 . . ? C4 C5 H5 117.9 . . ? N2 C6 C7 123.5(5) . . ? N2 C6 H6 118.2 . . ? C7 C6 H6 118.2 . . ? C6 C7 C8 118.1(5) . . ? C6 C7 H7 120.9 . . ? C8 C7 H7 121.0 . . ? C9 C8 C7 119.3(5) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C8 C9 C10 119.7(5) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? N2 C10 C9 122.1(5) . . ? N2 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? N3 C11 C12 122.5(4) . . ? N3 C11 H11 118.7 . . ? C12 C11 H11 118.7 . . ? C13 C12 C11 119.1(5) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C14 C13 C12 118.3(5) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? C13 C14 C15 120.0(5) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? N3 C15 C14 122.3(5) . . ? N3 C15 H15 118.9 . . ? C14 C15 H15 118.9 . . ?