# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Anne Gorden' _publ_contact_author_email GORDEAE@AUBURN.EDU _publ_section_title ; Unusual Topology of Amine Templated Three- and Two-Dimensional Uranyl Sulfate Compounds ; loop_ _publ_author_name 'Anne Gorden' 'Mohan S Bharara' # Attachment 'b926793h_2cif.cif' data_c222 _database_code_depnum_ccdc_archive 'CCDC 724366' #TrackingRef 'b926793h_2cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H24 N2 O42 S7 U6' _chemical_formula_weight 2472.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' 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' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'C 2 2 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.2776(12) _cell_length_b 18.339(2) _cell_length_c 22.788(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4295.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 3098 _cell_measurement_theta_min 1.79 _cell_measurement_theta_max 23.27 _exptl_crystal_description blocks _exptl_crystal_colour orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.818 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4328 _exptl_absorpt_coefficient_mu 23.005 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.014 _exptl_absorpt_correction_T_max 0.100 _exptl_absorpt_process_details 'SHELXPREP-97 (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'Bruker APEX' _diffrn_measurement_method 'w/ scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12304 _diffrn_reflns_av_R_equivalents 0.0770 _diffrn_reflns_av_sigmaI/netI 0.0760 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 23.27 _reflns_number_total 3098 _reflns_number_gt 2734 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SMART, SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ATOM v6.1 (Shape Software, 2004)' _computing_publication_material 'SHELXCIF-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Disordered oxygen, nitogen and carbon atoms were refined isotropically. DFIX and DANG were used in the refinement to control the geometry and displacement parameters of the atoms. H atoms were placed at calculated positions using suitable riding models with isotropic displacement parameters derived from their carrier atoms. ; _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^)+(0.0766P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 3098 _refine_ls_number_parameters 242 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1209 _refine_ls_wR_factor_gt 0.1157 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.002 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 0.95532(8) 0.74066(5) 0.97453(4) 0.0284(3) Uani 1 1 d . . . U2 U 0.62499(9) 0.96831(5) 0.88333(4) 0.0280(3) Uani 1 1 d . . . U3 U 0.75685(10) 0.74037(6) 0.74596(4) 0.0377(3) Uani 1 1 d . . . S1 S 0.6487(5) 0.7677(3) 0.8945(2) 0.0190(12) Uani 1 1 d . . . S2 S 0.7413(6) 0.8853(3) 1.0206(2) 0.0213(12) Uani 1 1 d . . . S3 S 0.5000 0.8853(5) 0.7500 0.036(2) Uani 1 2 d S . . S4 S 0.4895(6) 1.1442(3) 0.8365(2) 0.0249(13) Uani 1 1 d . . . O1 O 1.050(2) 0.7977(10) 0.9346(9) 0.052(5) Uiso 1 1 d . . . O2 O 0.868(2) 0.6834(11) 1.0149(9) 0.056(5) Uiso 1 1 d . . . O3 O 0.763(2) 0.9618(11) 0.8398(9) 0.054(5) Uiso 1 1 d . . . O4 O 0.484(2) 0.9771(9) 0.9237(7) 0.049(5) Uani 1 1 d . . . O5 O 0.6488(19) 0.6697(13) 0.7223(9) 0.062(7) Uani 1 1 d . . . O6 O 0.873(2) 0.8058(10) 0.7747(9) 0.052(5) Uani 1 1 d . . . O7 O 0.729(3) 0.8003(14) 0.6469(9) 0.080(8) Uani 1 1 d . . . O8 O 0.591(2) 0.8371(9) 0.8859(8) 0.048(5) Uani 1 1 d . . . O10 O 0.5779(17) 0.7258(8) 0.9410(8) 0.039(5) Uani 1 1 d . . . O11 O 0.7822(16) 0.7819(9) 0.9135(6) 0.032(3) Uani 1 1 d . . . O12 O 0.9422(15) 0.6558(9) 0.8970(7) 0.033(4) Uani 1 1 d . . . O13 O 0.498(3) 0.9276(12) 0.8034(9) 0.082(6) Uani 1 1 d . . . O14 O 0.8784(18) 0.6448(9) 0.7949(7) 0.038(4) Uani 1 1 d . . . O15 O 0.6469(15) 0.7273(9) 0.8390(6) 0.032(3) Uani 1 1 d . . . O16 O 0.7385(15) 1.0689(8) 0.9258(7) 0.024(4) Uani 1 1 d . . . O17 O 0.5559(19) 1.0739(8) 0.8315(7) 0.037(4) Uani 1 1 d . . . O18 O 0.9163(17) 0.7041(9) 0.6786(7) 0.035(4) Uani 1 1 d . . . O19 O 1.133(2) 0.6683(14) 0.9793(10) 0.083(8) Uani 1 1 d . . . O20 O 0.859(2) 0.8415(12) 1.0222(8) 0.063(7) Uani 1 1 d . . . O21 O 0.739(2) 0.9272(10) 0.9678(9) 0.063(6) Uani 1 1 d . . . O9 O 0.390(3) 0.8383(12) 0.7480(10) 0.082(6) Uani 1 1 d . . . N1 N 0.586(13) 0.559(7) 0.721(4) 0.71(17) Uiso 1 1 d D . . H1 H 0.6092 0.5191 0.7186 1.071 Uiso 1 1 calc R . . C1 C 0.526(7) 0.582(5) 0.663(3) 0.24(4) Uiso 1 1 d D . . H1A H 0.6056 0.5904 0.6392 0.294 Uiso 1 1 calc R . . H1B H 0.4961 0.6321 0.6730 0.294 Uiso 1 1 calc R . . C2 C 0.430(6) 0.563(3) 0.616(3) 0.24(4) Uiso 1 1 d D . . H2A H 0.4802 0.5615 0.5785 0.287 Uiso 1 1 calc R . . H2B H 0.3696 0.6043 0.6125 0.287 Uiso 1 1 calc R . . C3 C 0.347(6) 0.495(3) 0.616(3) 0.18(3) Uiso 1 1 d D . . H3A H 0.2799 0.4932 0.6470 0.213 Uiso 1 1 calc R . . H3B H 0.3957 0.4484 0.6129 0.213 Uiso 1 1 calc R . . C4 C 0.302(8) 0.526(6) 0.559(3) 0.40(8) Uiso 1 1 d D . . H4A H 0.3359 0.4956 0.5266 0.593 Uiso 1 1 calc R . . H4B H 0.3350 0.5756 0.5548 0.593 Uiso 1 1 calc R . . H4C H 0.2071 0.5259 0.5577 0.593 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 0.0301(5) 0.0386(6) 0.0164(5) -0.0094(4) -0.0060(4) 0.0145(4) U2 0.0466(6) 0.0192(4) 0.0183(5) -0.0027(4) -0.0113(4) 0.0003(4) U3 0.0436(6) 0.0442(6) 0.0252(6) 0.0022(5) 0.0016(4) 0.0118(5) S1 0.021(3) 0.022(3) 0.014(3) -0.001(2) 0.003(2) 0.002(2) S2 0.025(3) 0.022(3) 0.017(3) -0.006(2) -0.001(3) 0.001(2) S3 0.044(6) 0.032(5) 0.031(5) 0.000 -0.010(4) 0.000 S4 0.037(4) 0.023(3) 0.015(3) -0.002(2) 0.001(3) 0.005(3) O4 0.082(14) 0.036(10) 0.027(10) 0.003(8) 0.018(10) 0.009(11) O5 0.037(12) 0.101(18) 0.049(14) -0.026(11) 0.024(10) -0.009(12) O6 0.052(13) 0.044(11) 0.061(14) 0.001(9) 0.023(11) 0.007(10) O7 0.097(19) 0.12(2) 0.028(12) 0.009(12) -0.016(12) 0.052(16) O8 0.084(15) 0.024(9) 0.035(11) -0.005(8) -0.002(11) 0.015(9) O10 0.056(12) 0.016(9) 0.044(11) 0.000(7) 0.003(9) -0.017(8) O11 0.037(7) 0.051(8) 0.006(6) -0.004(5) 0.004(5) 0.002(6) O12 0.030(9) 0.037(10) 0.033(10) 0.010(7) 0.004(8) -0.001(8) O13 0.124(16) 0.080(11) 0.043(9) -0.020(8) 0.022(10) -0.068(11) O14 0.061(12) 0.038(10) 0.014(9) 0.011(7) 0.004(9) -0.002(9) O15 0.037(7) 0.051(8) 0.006(6) -0.004(5) 0.004(5) 0.002(6) O16 0.032(9) 0.016(8) 0.026(9) -0.004(6) -0.013(8) 0.001(7) O17 0.071(13) 0.019(8) 0.020(9) 0.005(7) -0.002(9) 0.018(8) O18 0.040(11) 0.051(11) 0.016(9) 0.012(7) 0.011(8) 0.010(9) O19 0.067(15) 0.11(2) 0.071(17) -0.050(15) -0.043(14) 0.032(14) O20 0.093(17) 0.088(16) 0.009(9) -0.014(9) -0.014(11) 0.055(14) O21 0.104(17) 0.036(11) 0.048(13) -0.010(9) -0.034(13) -0.002(12) O9 0.124(16) 0.080(11) 0.043(9) -0.020(8) 0.022(10) -0.068(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O2 1.66(2) . ? U1 O1 1.69(2) . ? U1 O19 2.26(2) . ? U1 O12 2.358(17) . ? U1 O20 2.360(18) . ? U1 O10 2.381(18) 8_567 ? U1 O11 2.382(16) . ? U2 O4 1.722(19) . ? U2 O3 1.73(2) . ? U2 O13 2.36(2) . ? U2 O21 2.38(2) . ? U2 O17 2.376(14) . ? U2 O16 2.388(14) . ? U2 O8 2.432(16) . ? U3 O5 1.79(2) . ? U3 O6 1.81(2) . ? U3 O18 2.341(16) . ? U3 O9 2.350(19) 3_656 ? U3 O15 2.415(14) . ? U3 O14 2.424(17) . ? U3 O7 2.53(2) . ? S1 O8 1.419(17) . ? S1 O11 1.461(17) . ? S1 O15 1.466(16) . ? S1 O10 1.498(17) . ? S2 O21 1.43(2) . ? S2 O20 1.46(2) . ? S2 O16 1.483(15) 4_577 ? S2 O19 1.48(2) 8_467 ? S3 O9 1.42(2) . ? S3 O9 1.42(2) 3_656 ? S3 O13 1.44(2) . ? S3 O13 1.44(2) 3_656 ? S4 O17 1.463(16) . ? S4 O12 1.477(18) 5_455 ? S4 O14 1.48(2) 5_455 ? S4 O18 1.505(18) 7_656 ? O10 U1 2.381(18) 8_467 ? O12 S4 1.477(18) 5_545 ? O14 S4 1.483(19) 5_545 ? O16 S2 1.483(15) 4_577 ? O18 S4 1.505(17) 7_646 ? O19 S2 1.48(2) 8_567 ? O9 U3 2.350(19) 3_656 ? N1 C1 1.52(2) . ? C1 C2 1.50(2) . ? C2 C3 1.51(2) . ? C3 C4 1.49(2) . ? 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 177.7(10) . . ? O2 U1 O19 92.3(10) . . ? O1 U1 O19 85.6(10) . . ? O2 U1 O12 88.2(8) . . ? O1 U1 O12 92.2(8) . . ? O19 U1 O12 72.2(6) . . ? O2 U1 O20 90.8(9) . . ? O1 U1 O20 90.2(9) . . ? O19 U1 O20 140.9(7) . . ? O12 U1 O20 146.9(6) . . ? O2 U1 O10 90.1(8) . 8_567 ? O1 U1 O10 88.3(8) . 8_567 ? O19 U1 O10 71.7(6) . 8_567 ? O12 U1 O10 143.7(5) . 8_567 ? O20 U1 O10 69.3(6) . 8_567 ? O2 U1 O11 96.9(8) . . ? O1 U1 O11 85.4(8) . . ? O19 U1 O11 144.9(7) . . ? O12 U1 O11 74.3(5) . . ? O20 U1 O11 73.0(6) . . ? O10 U1 O11 141.8(5) 8_567 . ? O4 U2 O3 177.1(9) . . ? O4 U2 O13 88.7(9) . . ? O3 U2 O13 89.3(9) . . ? O4 U2 O21 90.7(9) . . ? O3 U2 O21 92.1(9) . . ? O13 U2 O21 142.9(8) . . ? O4 U2 O17 86.5(7) . . ? O3 U2 O17 90.9(8) . . ? O13 U2 O17 73.1(7) . . ? O21 U2 O17 143.9(6) . . ? O4 U2 O16 97.0(7) . . ? O3 U2 O16 83.4(8) . . ? O13 U2 O16 145.7(6) . . ? O21 U2 O16 71.1(6) . . ? O17 U2 O16 73.6(6) . . ? O4 U2 O8 87.6(7) . . ? O3 U2 O8 93.7(8) . . ? O13 U2 O8 68.1(7) . . ? O21 U2 O8 74.8(6) . . ? O17 U2 O8 140.8(6) . . ? O16 U2 O8 145.6(6) . . ? O5 U3 O6 174.6(10) . . ? O5 U3 O18 91.8(7) . . ? O6 U3 O18 88.0(8) . . ? O5 U3 O9 99.9(10) . 3_656 ? O6 U3 O9 83.9(10) . 3_656 ? O18 U3 O9 134.8(7) . 3_656 ? O5 U3 O15 84.4(7) . . ? O6 U3 O15 93.2(7) . . ? O18 U3 O15 151.0(5) . . ? O9 U3 O15 74.0(7) 3_656 . ? O5 U3 O14 86.3(9) . . ? O6 U3 O14 88.5(7) . . ? O18 U3 O14 74.7(5) . . ? O9 U3 O14 148.9(7) 3_656 . ? O15 U3 O14 76.4(6) . . ? O5 U3 O7 88.7(10) . . ? O6 U3 O7 96.2(9) . . ? O18 U3 O7 67.5(7) . . ? O9 U3 O7 69.4(8) 3_656 . ? O15 U3 O7 140.8(7) . . ? O14 U3 O7 141.6(7) . . ? O8 S1 O11 105.9(11) . . ? O8 S1 O15 109.2(10) . . ? O11 S1 O15 111.0(9) . . ? O8 S1 O10 110.8(11) . . ? O11 S1 O10 109.8(10) . . ? O15 S1 O10 110.2(10) . . ? O21 S2 O20 109.2(14) . . ? O21 S2 O16 112.9(10) . 4_577 ? O20 S2 O16 108.0(10) . 4_577 ? O21 S2 O19 110.3(15) . 8_467 ? O20 S2 O19 105.1(15) . 8_467 ? O16 S2 O19 111.0(10) 4_577 8_467 ? O9 S3 O9 105(2) . 3_656 ? O9 S3 O13 110.0(13) . . ? O9 S3 O13 108.1(16) 3_656 . ? O9 S3 O13 108.1(16) . 3_656 ? O9 S3 O13 110.0(13) 3_656 3_656 ? O13 S3 O13 115(2) . 3_656 ? O17 S4 O12 110.7(9) . 5_455 ? O17 S4 O14 108.5(11) . 5_455 ? O12 S4 O14 110.0(10) 5_455 5_455 ? O17 S4 O18 109.0(11) . 7_656 ? O12 S4 O18 108.6(9) 5_455 7_656 ? O14 S4 O18 110.1(10) 5_455 7_656 ? S1 O8 U2 146.2(13) . . ? S1 O10 U1 134.2(9) . 8_467 ? S1 O11 U1 144.8(10) . . ? S4 O12 U1 140.9(9) 5_545 . ? S3 O13 U2 144.3(19) . . ? S4 O14 U3 134.1(10) 5_545 . ? S1 O15 U3 134.5(10) . . ? S2 O16 U2 141.3(10) 4_577 . ? S4 O17 U2 145.0(10) . . ? S4 O18 U3 143.9(9) 7_646 . ? S2 O19 U1 174.0(15) 8_567 . ? S2 O20 U1 140.3(13) . . ? S2 O21 U2 149.3(15) . . ? S3 O9 U3 166.4(19) . 3_656 ? N1 C1 C2 145(10) . . ? C1 C2 C3 125(8) . . ? C2 C3 C4 82(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O11 S1 O8 U2 6(2) . . . . ? O15 S1 O8 U2 -113.3(19) . . . . ? O10 S1 O8 U2 125.2(19) . . . . ? O4 U2 O8 S1 -135(2) . . . . ? O3 U2 O8 S1 47(2) . . . . ? O13 U2 O8 S1 135(2) . . . . ? O21 U2 O8 S1 -44(2) . . . . ? O17 U2 O8 S1 143.1(17) . . . . ? O16 U2 O8 S1 -36(3) . . . . ? O8 S1 O10 U1 -28.6(18) . . . 8_467 ? O11 S1 O10 U1 87.9(15) . . . 8_467 ? O15 S1 O10 U1 -149.6(13) . . . 8_467 ? O8 S1 O11 U1 145.1(15) . . . . ? O15 S1 O11 U1 -96.5(16) . . . . ? O10 S1 O11 U1 25.5(18) . . . . ? O2 U1 O11 S1 -14.1(17) . . . . ? O1 U1 O11 S1 165.6(17) . . . . ? O19 U1 O11 S1 90(2) . . . . ? O12 U1 O11 S1 72.0(16) . . . . ? O20 U1 O11 S1 -102.9(17) . . . . ? O10 U1 O11 S1 -113.1(16) 8_567 . . . ? O2 U1 O12 S4 -176.4(17) . . . 5_545 ? O1 U1 O12 S4 1.3(17) . . . 5_545 ? O19 U1 O12 S4 -83.4(17) . . . 5_545 ? O20 U1 O12 S4 95.0(19) . . . 5_545 ? O10 U1 O12 S4 -88.8(18) 8_567 . . 5_545 ? O11 U1 O12 S4 85.9(15) . . . 5_545 ? O9 S3 O13 U2 134(2) . . . . ? O9 S3 O13 U2 19(3) 3_656 . . . ? O13 S3 O13 U2 -104(2) 3_656 . . . ? O4 U2 O13 S3 -156(2) . . . . ? O3 U2 O13 S3 27(2) . . . . ? O21 U2 O13 S3 -66(3) . . . . ? O17 U2 O13 S3 118(2) . . . . ? O16 U2 O13 S3 104(3) . . . . ? O8 U2 O13 S3 -68(2) . . . . ? O5 U3 O14 S4 -172.0(15) . . . 5_545 ? O6 U3 O14 S4 6.7(14) . . . 5_545 ? O18 U3 O14 S4 95.1(14) . . . 5_545 ? O9 U3 O14 S4 -69(2) 3_656 . . 5_545 ? O15 U3 O14 S4 -86.9(14) . . . 5_545 ? O7 U3 O14 S4 104.9(16) . . . 5_545 ? O8 S1 O15 U3 68.6(16) . . . . ? O11 S1 O15 U3 -47.8(16) . . . . ? O10 S1 O15 U3 -169.5(12) . . . . ? O5 U3 O15 S1 -172.0(16) . . . . ? O6 U3 O15 S1 12.8(15) . . . . ? O18 U3 O15 S1 104.5(17) . . . . ? O9 U3 O15 S1 -70.0(15) 3_656 . . . ? O14 U3 O15 S1 100.5(14) . . . . ? O7 U3 O15 S1 -91.1(17) . . . . ? O4 U2 O16 S2 22.7(15) . . . 4_577 ? O3 U2 O16 S2 -160.2(16) . . . 4_577 ? O13 U2 O16 S2 120.7(17) . . . 4_577 ? O21 U2 O16 S2 -65.7(15) . . . 4_577 ? O17 U2 O16 S2 106.9(15) . . . 4_577 ? O8 U2 O16 S2 -73.4(18) . . . 4_577 ? O12 S4 O17 U2 -2(2) 5_455 . . . ? O14 S4 O17 U2 -122.7(19) 5_455 . . . ? O18 S4 O17 U2 117.5(19) 7_656 . . . ? O4 U2 O17 S4 36(2) . . . . ? O3 U2 O17 S4 -146(2) . . . . ? O13 U2 O17 S4 125(2) . . . . ? O21 U2 O17 S4 -51(3) . . . . ? O16 U2 O17 S4 -63(2) . . . . ? O8 U2 O17 S4 117.6(19) . . . . ? O5 U3 O18 S4 -68(2) . . . 7_646 ? O6 U3 O18 S4 107(2) . . . 7_646 ? O9 U3 O18 S4 -173.5(17) 3_656 . . 7_646 ? O15 U3 O18 S4 14(3) . . . 7_646 ? O14 U3 O18 S4 18.0(18) . . . 7_646 ? O7 U3 O18 S4 -155(2) . . . 7_646 ? O2 U1 O19 S2 60(18) . . . 8_567 ? O1 U1 O19 S2 -121(18) . . . 8_567 ? O12 U1 O19 S2 -27(18) . . . 8_567 ? O20 U1 O19 S2 154(17) . . . 8_567 ? O10 U1 O19 S2 149(18) 8_567 . . 8_567 ? O11 U1 O19 S2 -45(19) . . . 8_567 ? O21 S2 O20 U1 -69(2) . . . . ? O16 S2 O20 U1 167.5(18) 4_577 . . . ? O19 S2 O20 U1 49(2) 8_467 . . . ? O2 U1 O20 S2 -81(2) . . . . ? O1 U1 O20 S2 101(2) . . . . ? O19 U1 O20 S2 -175.5(18) . . . . ? O12 U1 O20 S2 7(3) . . . . ? O10 U1 O20 S2 -171(3) 8_567 . . . ? O11 U1 O20 S2 16(2) . . . . ? O20 S2 O21 U2 132(3) . . . . ? O16 S2 O21 U2 -108(2) 4_577 . . . ? O19 S2 O21 U2 17(3) 8_467 . . . ? O4 U2 O21 S2 39(3) . . . . ? O3 U2 O21 S2 -142(3) . . . . ? O13 U2 O21 S2 -50(3) . . . . ? O17 U2 O21 S2 124(2) . . . . ? O16 U2 O21 S2 136(3) . . . . ? O8 U2 O21 S2 -49(2) . . . . ? O9 S3 O9 U3 21(6) 3_656 . . 3_656 ? O13 S3 O9 U3 -95(6) . . . 3_656 ? O13 S3 O9 U3 138(6) 3_656 . . 3_656 ? N1 C1 C2 C3 0(4) . . . . ? C1 C2 C3 C4 -179(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O3 0.77 2.15 2.74(11) 134.1 7_646 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.433 _refine_diff_density_min -2.625 _refine_diff_density_rms 0.339 # Attachment '3cif.CIF' data_p21b _database_code_depnum_ccdc_archive 'CCDC 724367' #TrackingRef '3cif.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H15 N O19 S3 U2' _chemical_formula_weight 953.51 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' 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' 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' H H 0.0000 0.0000 '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 1 21 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.439(5) _cell_length_b 11.912(7) _cell_length_c 10.636(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.790(10) _cell_angle_gamma 90.00 _cell_volume 1042.6(10) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 2934 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 23.3 _exptl_crystal_description blocks _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.021 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 850 _exptl_absorpt_coefficient_mu 15.899 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.012 _exptl_absorpt_correction_T_max 0.019 _exptl_absorpt_process_details 'SHELXPREP-97 (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'Bruker APEX' _diffrn_measurement_method 'w/ scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7141 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 23.28 _reflns_number_total 2995 _reflns_number_gt 2934 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SMART, SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ATOM v6.1 (Shape Software, 2004)' _computing_publication_material 'SHELXCIF-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H atoms were placed at calculated positions using suitable riding models with isotropic displacement parameters derived from their carrier atoms. Hydrogen atoms present on water molecules were not generated. ; _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^)+(0.0383P)^2^+2.0591P] 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 SHELXL _refine_ls_extinction_coef 0.00064(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.021(9) _refine_ls_number_reflns 2995 _refine_ls_number_parameters 263 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0242 _refine_ls_R_factor_gt 0.0222 _refine_ls_wR_factor_ref 0.0642 _refine_ls_wR_factor_gt 0.0524 _refine_ls_goodness_of_fit_ref 1.163 _refine_ls_restrained_S_all 1.163 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 1.00715(4) 0.46259(2) 0.06548(4) 0.01601(13) Uani 1 1 d . . . U2 U 1.00886(4) 0.24455(3) 0.52895(3) 0.01585(13) Uani 1 1 d . . . S1 S 0.8604(3) 0.7372(2) 0.1227(2) 0.0186(5) Uani 1 1 d . . . S2 S 0.8125(3) 0.4787(2) 0.3427(2) 0.0184(5) Uani 1 1 d . . . S3 S 0.9283(3) 0.1788(2) 0.1766(2) 0.0170(5) Uani 1 1 d . . . O1 O 1.2151(9) 0.4768(6) 0.1361(7) 0.0288(18) Uani 1 1 d . . . O2 O 0.7994(9) 0.4440(6) -0.0029(8) 0.0281(18) Uani 1 1 d . . . O3 O 1.0826(9) 0.3506(6) -0.0959(7) 0.0239(18) Uani 1 1 d . . . O4 O 1.0296(8) 0.2742(6) 0.1519(7) 0.0185(16) Uani 1 1 d . . . O5 O 0.9381(9) 0.4808(6) 0.2670(7) 0.0235(17) Uani 1 1 d . . . O6 O 0.9875(10) 0.6572(6) 0.1109(7) 0.0256(18) Uani 1 1 d . . . O7 O 0.8413(9) 0.1769(7) 0.5728(7) 0.0257(17) Uani 1 1 d . . . O8 O 1.1732(10) 0.3116(7) 0.4846(7) 0.0289(18) Uani 1 1 d . . . O9 O 1.1659(8) 0.2358(6) 0.7439(6) 0.0202(15) Uani 1 1 d . . . O10 O 0.8135(8) 0.3673(6) 0.4041(7) 0.0191(16) Uani 1 1 d . . . O11 O 0.9638(12) 0.4125(7) 0.6502(8) 0.035(2) Uani 1 1 d . . . O12 O 1.1426(9) 0.0639(6) 0.5502(7) 0.0183(16) Uani 1 1 d . . . O13 O 0.6528(9) 0.5001(7) 0.2653(8) 0.033(2) Uani 1 1 d . . . O14 O 0.7086(10) 0.7111(6) 0.0342(7) 0.034(2) Uani 1 1 d . . . O17 O 0.9503(9) 0.1619(6) 0.3191(7) 0.0201(16) Uani 1 1 d . . . O15 O 1.0174(9) 0.5745(6) -0.1262(8) 0.0231(17) Uani 1 1 d . . . O16 O 0.7582(10) 0.1993(7) 0.1188(7) 0.0323(19) Uani 1 1 d . . . N1 N 0.5159(14) 0.7926(10) 0.7957(10) 0.044(3) Uani 1 1 d . . . H1 H 0.4419 0.7581 0.8045 0.066 Uiso 1 1 calc R . . C1 C 0.5650(19) 0.7557(17) 0.6824(18) 0.068(5) Uani 1 1 d . . . H1A H 0.6596 0.8013 0.6726 0.081 Uiso 1 1 calc R . . H1B H 0.4756 0.7717 0.6071 0.081 Uiso 1 1 calc R . . C2 C 0.6101(18) 0.6331(14) 0.6774(16) 0.055(4) Uani 1 1 d . . . H2A H 0.6480 0.6195 0.5970 0.066 Uiso 1 1 calc R . . H2B H 0.7020 0.6169 0.7508 0.066 Uiso 1 1 calc R . . C3 C 0.476(2) 0.5542(14) 0.6822(18) 0.064(5) Uani 1 1 d . . . H3A H 0.3811 0.5730 0.6125 0.077 Uiso 1 1 calc R . . H3B H 0.4437 0.5628 0.7656 0.077 Uiso 1 1 calc R . . C4 C 0.524(3) 0.4348(16) 0.667(3) 0.105(9) Uani 1 1 d . . . H4A H 0.4325 0.3853 0.6705 0.157 Uiso 1 1 calc R . . H4B H 0.6168 0.4153 0.7372 0.157 Uiso 1 1 calc R . . H4C H 0.5549 0.4257 0.5842 0.157 Uiso 1 1 calc R . . O2W O 0.5710(14) 0.2236(12) 0.8877(11) 0.079(4) Uani 1 1 d . . . O1W O 0.4318(13) 0.6518(10) 0.3221(11) 0.058(3) 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 U1 0.0253(2) 0.0106(2) 0.0133(2) -0.00004(17) 0.00668(14) -0.00003(16) U2 0.0246(2) 0.0119(2) 0.0118(2) 0.00017(15) 0.00566(14) -0.00069(17) S1 0.0315(14) 0.0118(11) 0.0127(12) 0.0001(11) 0.0056(10) -0.0038(13) S2 0.0272(13) 0.0130(14) 0.0163(13) 0.0003(10) 0.0075(10) 0.0017(11) S3 0.0250(14) 0.0139(12) 0.0122(12) -0.0029(10) 0.0045(10) -0.0022(12) O1 0.039(4) 0.015(4) 0.037(5) 0.003(4) 0.020(4) 0.002(3) O2 0.031(4) 0.019(4) 0.035(4) 0.001(4) 0.009(3) 0.001(3) O3 0.048(5) 0.016(4) 0.008(4) 0.003(3) 0.007(3) 0.005(4) O4 0.031(4) 0.009(3) 0.016(4) 0.005(3) 0.007(3) 0.004(3) O5 0.041(4) 0.020(4) 0.011(4) -0.005(3) 0.010(3) -0.001(3) O6 0.048(5) 0.020(4) 0.011(4) 0.005(3) 0.011(4) 0.005(4) O7 0.034(4) 0.020(4) 0.026(4) -0.002(3) 0.014(3) -0.003(4) O8 0.038(5) 0.027(4) 0.024(4) 0.010(4) 0.011(4) -0.005(4) O9 0.028(4) 0.016(3) 0.017(3) 0.004(3) 0.005(3) 0.000(3) O10 0.024(4) 0.013(3) 0.024(4) 0.002(3) 0.013(3) 0.002(3) O11 0.072(6) 0.013(4) 0.017(4) -0.004(3) 0.007(4) 0.007(4) O12 0.035(4) 0.010(4) 0.011(4) -0.003(3) 0.008(3) -0.004(3) O13 0.039(5) 0.028(4) 0.030(5) 0.003(3) 0.002(4) 0.004(4) O14 0.033(5) 0.045(6) 0.019(4) 0.005(4) -0.002(3) -0.006(3) O17 0.036(4) 0.017(4) 0.011(4) -0.006(3) 0.013(3) 0.000(3) O15 0.040(5) 0.010(4) 0.024(4) -0.002(3) 0.015(4) 0.002(3) O16 0.033(5) 0.037(5) 0.029(4) 0.004(4) 0.013(3) 0.001(4) N1 0.046(7) 0.047(7) 0.036(7) 0.010(5) 0.002(5) -0.008(6) C1 0.056(10) 0.076(13) 0.086(13) 0.046(11) 0.047(9) 0.020(10) C2 0.043(9) 0.078(12) 0.045(9) 0.003(8) 0.013(7) 0.006(8) C3 0.068(11) 0.064(11) 0.057(11) 0.004(8) 0.005(9) -0.006(9) C4 0.070(12) 0.081(17) 0.15(2) -0.057(15) -0.002(13) -0.001(11) O2W 0.051(7) 0.124(13) 0.061(7) 0.017(8) 0.008(5) 0.010(7) O1W 0.057(7) 0.062(7) 0.053(7) -0.009(5) 0.008(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 U1 O2 1.757(8) . ? U1 O1 1.758(8) . ? U1 O5 2.353(7) . ? U1 O3 2.369(7) . ? U1 O6 2.381(7) . ? U1 O4 2.416(7) . ? U1 O15 2.453(8) . ? U2 O8 1.753(7) . ? U2 O7 1.778(7) . ? U2 O10 2.377(7) . ? U2 O9 2.377(6) . ? U2 O17 2.389(7) . ? U2 O12 2.418(7) . ? U2 O11 2.455(8) . ? S1 O14 1.445(8) . ? S1 O6 1.460(8) . ? S1 O3 1.482(8) 2_755 ? S1 O9 1.485(7) 2_756 ? S2 O13 1.438(8) . ? S2 O5 1.467(8) . ? S2 O10 1.478(7) . ? S2 O12 1.509(7) 2_756 ? S3 O16 1.452(9) . ? S3 O15 1.466(8) 2_745 ? S3 O4 1.481(7) . ? S3 O17 1.499(7) . ? O3 S1 1.482(8) 2_745 ? O9 S1 1.485(7) 2_746 ? O12 S2 1.509(7) 2_746 ? O15 S3 1.466(8) 2_755 ? N1 C1 1.43(2) . ? C1 C2 1.51(2) . ? C2 C3 1.48(2) . ? C3 C4 1.50(2) . ? 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 178.1(4) . . ? O2 U1 O5 87.9(3) . . ? O1 U1 O5 91.5(3) . . ? O2 U1 O3 91.9(3) . . ? O1 U1 O3 87.8(3) . . ? O5 U1 O3 150.7(3) . . ? O2 U1 O6 95.7(3) . . ? O1 U1 O6 85.8(3) . . ? O5 U1 O6 71.5(2) . . ? O3 U1 O6 137.5(3) . . ? O2 U1 O4 91.6(3) . . ? O1 U1 O4 86.6(3) . . ? O5 U1 O4 75.7(3) . . ? O3 U1 O4 75.0(2) . . ? O6 U1 O4 146.1(3) . . ? O2 U1 O15 86.6(3) . . ? O1 U1 O15 95.0(3) . . ? O5 U1 O15 140.2(2) . . ? O3 U1 O15 68.9(2) . . ? O6 U1 O15 69.9(3) . . ? O4 U1 O15 143.7(2) . . ? O8 U2 O7 179.6(4) . . ? O8 U2 O10 93.5(3) . . ? O7 U2 O10 86.1(3) . . ? O8 U2 O9 88.4(3) . . ? O7 U2 O9 92.0(3) . . ? O10 U2 O9 137.3(2) . . ? O8 U2 O17 87.1(3) . . ? O7 U2 O17 92.6(3) . . ? O10 U2 O17 75.9(2) . . ? O9 U2 O17 146.7(2) . . ? O8 U2 O12 92.9(3) . . ? O7 U2 O12 87.4(3) . . ? O10 U2 O12 148.4(2) . . ? O9 U2 O12 73.8(2) . . ? O17 U2 O12 73.5(2) . . ? O8 U2 O11 89.6(3) . . ? O7 U2 O11 90.4(3) . . ? O10 U2 O11 67.9(3) . . ? O9 U2 O11 69.5(3) . . ? O17 U2 O11 143.4(3) . . ? O12 U2 O11 143.1(3) . . ? O14 S1 O6 111.5(5) . . ? O14 S1 O3 110.4(4) . 2_755 ? O6 S1 O3 107.6(5) . 2_755 ? O14 S1 O9 108.7(4) . 2_756 ? O6 S1 O9 110.0(4) . 2_756 ? O3 S1 O9 108.5(4) 2_755 2_756 ? O13 S2 O5 112.5(5) . . ? O13 S2 O10 109.0(5) . . ? O5 S2 O10 108.8(4) . . ? O13 S2 O12 111.1(4) . 2_756 ? O5 S2 O12 108.2(4) . 2_756 ? O10 S2 O12 107.1(4) . 2_756 ? O16 S3 O15 110.3(5) . 2_745 ? O16 S3 O4 110.6(5) . . ? O15 S3 O4 110.3(4) 2_745 . ? O16 S3 O17 109.9(4) . . ? O15 S3 O17 106.1(4) 2_745 . ? O4 S3 O17 109.6(4) . . ? S1 O3 U1 143.4(4) 2_745 . ? S3 O4 U1 141.3(4) . . ? S2 O5 U1 148.6(5) . . ? S1 O6 U1 137.6(5) . . ? S1 O9 U2 138.5(4) 2_746 . ? S2 O10 U2 137.3(4) . . ? S2 O12 U2 134.6(4) 2_746 . ? S3 O17 U2 147.4(4) . . ? S3 O15 U1 146.7(5) 2_755 . ? N1 C1 C2 116.7(13) . . ? C3 C2 C1 114.3(13) . . ? C2 C3 C4 111.9(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 U1 O3 S1 -101.2(8) . . . 2_745 ? O1 U1 O3 S1 77.0(8) . . . 2_745 ? O5 U1 O3 S1 -12.1(11) . . . 2_745 ? O6 U1 O3 S1 158.3(7) . . . 2_745 ? O4 U1 O3 S1 -10.0(7) . . . 2_745 ? O15 U1 O3 S1 173.2(9) . . . 2_745 ? O16 S3 O4 U1 8.4(8) . . . . ? O15 S3 O4 U1 130.7(6) 2_745 . . . ? O17 S3 O4 U1 -112.9(6) . . . . ? O2 U1 O4 S3 -13.5(7) . . . . ? O1 U1 O4 S3 166.3(7) . . . . ? O5 U1 O4 S3 73.9(7) . . . . ? O3 U1 O4 S3 -105.1(7) . . . . ? O6 U1 O4 S3 89.1(8) . . . . ? O15 U1 O4 S3 -99.9(7) . . . . ? O13 S2 O5 U1 -23.3(11) . . . . ? O10 S2 O5 U1 97.6(9) . . . . ? O12 S2 O5 U1 -146.4(8) 2_756 . . . ? O2 U1 O5 S2 3.1(9) . . . . ? O1 U1 O5 S2 -175.1(9) . . . . ? O3 U1 O5 S2 -86.9(10) . . . . ? O6 U1 O5 S2 99.8(9) . . . . ? O4 U1 O5 S2 -89.0(9) . . . . ? O15 U1 O5 S2 85.2(10) . . . . ? O14 S1 O6 U1 -34.1(8) . . . . ? O3 S1 O6 U1 -155.3(6) 2_755 . . . ? O9 S1 O6 U1 86.6(7) 2_756 . . . ? O2 U1 O6 S1 17.7(7) . . . . ? O1 U1 O6 S1 -161.1(7) . . . . ? O5 U1 O6 S1 -68.1(6) . . . . ? O3 U1 O6 S1 116.8(6) . . . . ? O4 U1 O6 S1 -83.6(8) . . . . ? O15 U1 O6 S1 102.0(7) . . . . ? O8 U2 O9 S1 148.9(7) . . . 2_746 ? O7 U2 O9 S1 -31.0(7) . . . 2_746 ? O10 U2 O9 S1 55.4(8) . . . 2_746 ? O17 U2 O9 S1 -128.8(6) . . . 2_746 ? O12 U2 O9 S1 -117.6(7) . . . 2_746 ? O11 U2 O9 S1 58.7(7) . . . 2_746 ? O13 S2 O10 U2 172.6(6) . . . . ? O5 S2 O10 U2 49.6(7) . . . . ? O12 S2 O10 U2 -67.1(6) 2_756 . . . ? O8 U2 O10 S2 -17.7(6) . . . . ? O7 U2 O10 S2 162.5(7) . . . . ? O9 U2 O10 S2 73.8(7) . . . . ? O17 U2 O10 S2 -103.8(6) . . . . ? O12 U2 O10 S2 -119.0(6) . . . . ? O11 U2 O10 S2 70.5(6) . . . . ? O8 U2 O12 S2 123.5(6) . . . 2_746 ? O7 U2 O12 S2 -56.8(6) . . . 2_746 ? O10 U2 O12 S2 -135.0(5) . . . 2_746 ? O9 U2 O12 S2 36.0(5) . . . 2_746 ? O17 U2 O12 S2 -150.4(6) . . . 2_746 ? O11 U2 O12 S2 30.3(8) . . . 2_746 ? O16 S3 O17 U2 -92.3(9) . . . . ? O15 S3 O17 U2 148.5(8) 2_745 . . . ? O4 S3 O17 U2 29.4(9) . . . . ? O8 U2 O17 S3 -47.7(8) . . . . ? O7 U2 O17 S3 132.0(8) . . . . ? O10 U2 O17 S3 46.7(8) . . . . ? O9 U2 O17 S3 -130.4(7) . . . . ? O12 U2 O17 S3 -141.6(9) . . . . ? O11 U2 O17 S3 37.8(10) . . . . ? O2 U1 O15 S3 132.3(9) . . . 2_755 ? O1 U1 O15 S3 -48.7(9) . . . 2_755 ? O5 U1 O15 S3 49.8(10) . . . 2_755 ? O3 U1 O15 S3 -134.3(9) . . . 2_755 ? O6 U1 O15 S3 35.0(8) . . . 2_755 ? O4 U1 O15 S3 -139.7(7) . . . 2_755 ? N1 C1 C2 C3 62(2) . . . . ? C1 C2 C3 C4 175.8(18) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O16 0.77 2.15 2.889(14) 161.2 2_656 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.859 _refine_diff_density_min -0.853 _refine_diff_density_rms 0.162 # Attachment '1cif.cif' data_p21 _database_code_depnum_ccdc_archive 'CCDC 724368' #TrackingRef '1cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H82 N8 O47 S9 U5' _chemical_formula_weight 2809.73 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' 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' 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' H H 0.0000 0.0000 '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 9.4586(8) _cell_length_b 26.769(2) _cell_length_c 32.377(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8197.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 9731 _cell_measurement_theta_min 1.26 _cell_measurement_theta_max 23.27 _exptl_crystal_description needles _exptl_crystal_colour orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.275 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5232 _exptl_absorpt_coefficient_mu 10.168 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.307 _exptl_absorpt_correction_T_max 0.601 _exptl_absorpt_process_details 'SHELXPREP-97 (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'Bruker APEX' _diffrn_measurement_method 'w/ scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46987 _diffrn_reflns_av_R_equivalents 0.0827 _diffrn_reflns_av_sigmaI/netI 0.0839 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 23.27 _reflns_number_total 11719 _reflns_number_gt 9731 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SMART, SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ATOM v6.1 (Shape Software, 2004)' _computing_publication_material 'SHELXCIF-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Disordered oxygen and carbon atoms were refined isotropically. The disorder present in n-butylammonium cations contributes to unusual Ueq values and hence not be treated as anisotropic. DFIX and DANG were used in the refinement to control the geometry and displacement parameters of the atoms. H atoms were placed at calculated positions using suitable riding models with isotropic displacement parameters derived from their carrier atoms. Hydrogen atoms present on water molecules were not generated. ; _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^)+(0.0197P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.405(7) _refine_ls_number_reflns 11719 _refine_ls_number_parameters 741 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.0692 _refine_ls_wR_factor_gt 0.0655 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.955 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 1.23852(6) 0.725608(15) 0.851419(13) 0.02150(12) Uani 1 1 d . . . U2 U 0.73679(6) 0.608656(16) 0.902148(13) 0.02149(12) Uani 1 1 d . . . U3 U 0.27601(5) 0.445868(16) 0.845402(14) 0.02020(12) Uani 1 1 d . . . U4 U 0.75430(7) 0.803575(17) 0.545716(13) 0.02913(13) Uani 1 1 d . . . U5 U 0.77411(6) 0.761945(16) 0.708468(14) 0.02110(12) Uani 1 1 d . . . S1 S 1.4746(4) 0.71278(17) 0.76708(14) 0.0294(11) Uani 1 1 d . . . S2 S 1.0141(4) 0.71523(15) 0.76107(12) 0.0212(10) Uani 1 1 d . . . S3 S 0.9574(4) 0.84024(15) 0.63385(12) 0.0209(9) Uani 1 1 d . . . S4 S 0.5406(4) 0.82888(14) 0.64097(12) 0.0191(9) Uani 1 1 d . . . S5 S 1.0136(4) 0.70195(15) 0.91923(13) 0.0235(10) Uani 1 1 d . . . S6 S 0.5122(4) 0.52631(15) 0.84142(14) 0.0244(10) Uani 1 1 d . . . S7 S 1.5112(4) 0.68911(16) 0.92531(12) 0.0226(10) Uani 1 1 d . . . S8 S 0.9575(4) 0.77665(18) 0.47441(12) 0.0441(12) Uani 1 1 d . . . S9 S 0.9744(4) 0.53172(14) 0.84389(14) 0.0242(10) Uani 1 1 d . . . O1 O 1.0951(9) 0.7403(4) 0.7946(3) 0.027(2) Uani 1 1 d . . . O2 O 0.7448(11) 0.6354(2) 0.8527(2) 0.030(2) Uani 1 1 d . . . O3 O 1.2408(10) 0.6620(3) 0.8404(2) 0.0251(19) Uani 1 1 d . . . O4 O 1.4168(9) 0.7385(4) 0.8041(3) 0.028(3) Uani 1 1 d . . . O5 O 0.7338(11) 0.5839(3) 0.9518(2) 0.029(2) Uani 1 1 d . . . O6 O 0.5916(9) 0.5432(4) 0.8783(3) 0.021(2) Uani 1 1 d . . . O7 O 0.4880(9) 0.6361(3) 0.9150(3) 0.027(3) Uani 1 1 d . . . O8 O 0.0963(9) 0.3859(4) 0.8427(3) 0.028(3) Uani 1 1 d . . . O10 O 0.9909(9) 0.7213(4) 0.8765(3) 0.030(3) Uani 1 1 d . . . O11 O 0.7583(11) 0.7025(3) 0.6855(2) 0.031(2) Uani 1 1 d . . . O12 O 0.3889(9) 0.8275(4) 0.6366(3) 0.024(3) Uiso 1 1 d . . . O13 O 0.2986(9) 0.4406(3) 0.8981(3) 0.028(2) Uani 1 1 d . . . O14 O 0.7894(10) 0.8197(3) 0.7322(2) 0.032(2) Uani 1 1 d . . . O15 O 0.9211(10) 0.8433(4) 0.5902(3) 0.028(3) Uani 1 1 d . . . O16 O 0.4159(10) 0.3739(3) 0.8370(3) 0.020(2) Uani 1 1 d . . . O17 O 0.8951(9) 0.7941(3) 0.6516(3) 0.021(2) Uani 1 1 d . . . O18 O 0.2559(11) 0.4524(3) 0.7920(2) 0.031(2) Uani 1 1 d . . . O19 O 1.2342(10) 0.7889(3) 0.8632(2) 0.029(2) Uani 1 1 d . . . O20 O 1.4586(10) 0.7029(4) 0.9652(3) 0.032(2) Uani 1 1 d . . . O21 O 1.1728(8) 0.6974(3) 0.9222(2) 0.023(2) Uani 1 1 d . . . O22 O 0.7913(10) 0.7472(3) 0.5693(3) 0.040(3) Uani 1 1 d . . . O23 O 0.5917(10) 0.7843(4) 0.6645(3) 0.030(3) Uani 1 1 d . . . O24 O 0.7168(11) 0.8602(3) 0.5212(3) 0.042(3) Uani 1 1 d . . . O25 O 1.4522(9) 0.7220(3) 0.8927(3) 0.025(2) Uani 1 1 d . . . O26 O 0.8047(9) 0.7648(4) 0.4789(3) 0.044(3) Uani 1 1 d . . . O27 O 0.8578(9) 0.7187(3) 0.7709(2) 0.025(2) Uani 1 1 d . . . O28 O 0.3583(8) 0.5338(3) 0.8491(3) 0.026(2) Uani 1 1 d . . . O29 O 1.0588(9) 0.6630(4) 0.7562(3) 0.029(2) Uani 1 1 d . . . O30 O 1.0785(10) 0.4953(3) 0.8594(3) 0.036(3) Uani 1 1 d . . . O31 O 1.0264(9) 0.7447(3) 0.7219(2) 0.024(2) Uani 1 1 d . . . O32 O 0.6675(8) 0.6942(3) 0.9240(2) 0.024(2) Uani 1 1 d . . . O33 O 0.9897(11) 0.8045(4) 0.5121(4) 0.051(3) Uani 1 1 d . . . O34 O 0.9618(9) 0.7344(3) 0.9514(3) 0.031(2) Uani 1 1 d . . . O35 O 1.5791(9) 0.7488(3) 0.7502(3) 0.034(3) Uani 1 1 d . . . O36 O 1.3628(10) 0.7043(4) 0.7375(3) 0.050(3) Uani 1 1 d . . . O37 O 0.9121(9) 0.5549(4) 0.8831(3) 0.030(3) Uani 1 1 d . . . O38 O 0.6113(10) 0.8292(4) 0.6003(3) 0.029(3) Uani 1 1 d . . . O39 O 0.5546(10) 0.5527(4) 0.8047(3) 0.032(2) Uani 1 1 d . . . O40 O 0.5361(10) 0.7718(4) 0.5247(3) 0.051(3) Uani 1 1 d . . . O41 O 0.9492(9) 0.6510(4) 0.9236(3) 0.027(2) Uani 1 1 d . . . O42 O 0.8597(10) 0.5060(4) 0.8219(3) 0.045(3) Uani 1 1 d . . . O43 O 1.0449(10) 0.5698(3) 0.8202(3) 0.036(3) Uani 1 1 d . . . O44 O 0.9922(12) 0.8048(5) 0.4384(3) 0.065(4) Uani 1 1 d . . . O45 O 1.5420(11) 0.6677(3) 0.7789(3) 0.047(3) Uani 1 1 d . . . O46 O 0.5273(9) 0.4713(3) 0.8388(3) 0.029(2) Uani 1 1 d . . . O47 O 1.1091(9) 0.8381(4) 0.6376(3) 0.038(3) Uani 1 1 d . . . O1W O 0.9933(16) 0.8325(5) 0.3556(4) 0.092(5) Uani 1 1 d . . . N1 N 0.2463(14) 0.8343(4) 0.5557(3) 0.037(3) Uani 1 1 d D . . H1 H 0.2591 0.8096 0.5441 0.056 Uiso 1 1 calc R . . C1 C 0.322(2) 0.8764(6) 0.5336(6) 0.101(8) Uiso 1 1 d D . . H1A H 0.2912 0.8774 0.5044 0.121 Uiso 1 1 calc R . . H1B H 0.4252 0.8701 0.5341 0.121 Uiso 1 1 calc R . . C2 C 0.291(3) 0.9277(8) 0.5544(7) 0.122(9) Uiso 1 1 d D . . H2A H 0.3266 0.9266 0.5831 0.147 Uiso 1 1 calc R . . H2B H 0.3450 0.9537 0.5396 0.147 Uiso 1 1 calc R . . C3 C 0.133(3) 0.9438(13) 0.5556(10) 0.185(14) Uiso 1 1 d D . . H3A H 0.0767 0.9185 0.5706 0.222 Uiso 1 1 calc R . . H3B H 0.1241 0.9761 0.5703 0.222 Uiso 1 1 calc R . . C4 C 0.081(3) 0.9489(12) 0.5125(9) 0.184(14) Uiso 1 1 d D . . H4A H -0.0164 0.9611 0.5127 0.277 Uiso 1 1 calc R . . H4B H 0.0847 0.9163 0.4988 0.277 Uiso 1 1 calc R . . H4C H 0.1411 0.9726 0.4974 0.277 Uiso 1 1 calc R . . N2 N 0.2427(14) 0.9105(3) 0.6880(3) 0.030(3) Uani 1 1 d D . . H2 H 0.2273 0.8875 0.6744 0.045 Uiso 1 1 calc R . . C5 C 0.188(2) 0.9019(7) 0.7295(5) 0.098(8) Uiso 1 1 d D . . H5A H 0.2081 0.9317 0.7467 0.118 Uiso 1 1 calc R . . H5B H 0.0846 0.8976 0.7282 0.118 Uiso 1 1 calc R . . C6 C 0.251(3) 0.8582(7) 0.7492(7) 0.133(8) Uiso 1 1 d D . . H6A H 0.2442 0.8296 0.7299 0.160 Uiso 1 1 calc R . . H6B H 0.1945 0.8498 0.7741 0.160 Uiso 1 1 calc R . . C7 C 0.405(3) 0.8651(11) 0.7618(10) 0.166(13) Uiso 1 1 d D . . H7A H 0.4324 0.8339 0.7761 0.199 Uiso 1 1 calc R . . H7B H 0.4595 0.8661 0.7358 0.199 Uiso 1 1 calc R . . C8 C 0.461(4) 0.9073(13) 0.7880(12) 0.25(2) Uiso 1 1 d D . . H8A H 0.5609 0.9014 0.7941 0.375 Uiso 1 1 calc R . . H8B H 0.4073 0.9090 0.8139 0.375 Uiso 1 1 calc R . . H8C H 0.4508 0.9389 0.7730 0.375 Uiso 1 1 calc R . . N3 N 0.7909(11) 0.6044(3) 0.7698(3) 0.024(3) Uiso 1 1 d . . . H3 H 0.7303 0.5913 0.7814 0.036 Uiso 1 1 calc R . . C9 C 0.785(2) 0.5907(6) 0.7260(5) 0.069(6) Uiso 1 1 d D . . H9A H 0.6981 0.6059 0.7147 0.083 Uiso 1 1 calc R . . H9B H 0.8655 0.6080 0.7125 0.083 Uiso 1 1 calc R . . C10 C 0.788(5) 0.5390(9) 0.7110(11) 0.260(19) Uiso 1 1 d D . . H10A H 0.7126 0.5198 0.7249 0.312 Uiso 1 1 calc R . . H10B H 0.8801 0.5237 0.7186 0.312 Uiso 1 1 calc R . . C11 C 0.768(6) 0.5352(15) 0.6639(11) 0.269(18) Uiso 1 1 d D . . H11A H 0.8474 0.5546 0.6518 0.323 Uiso 1 1 calc R . . H11B H 0.7875 0.4998 0.6570 0.323 Uiso 1 1 calc R . . C12 C 0.642(8) 0.549(4) 0.639(3) 0.79(9) Uiso 1 1 d D . . H12A H 0.6570 0.5392 0.6099 1.183 Uiso 1 1 calc R . . H12B H 0.6269 0.5853 0.6401 1.183 Uiso 1 1 calc R . . H12C H 0.5582 0.5318 0.6495 1.183 Uiso 1 1 calc R . . N4 N 0.2576(14) 0.7330(4) 0.6609(3) 0.041(3) Uani 1 1 d . . . H4 H 0.2861 0.7592 0.6560 0.062 Uiso 1 1 calc R . . C13 C 0.173(2) 0.7133(7) 0.6241(6) 0.083(7) Uiso 1 1 d D . . H13A H 0.0984 0.7375 0.6163 0.100 Uiso 1 1 calc R . . H13B H 0.2360 0.7083 0.6000 0.100 Uiso 1 1 calc R . . C14 C 0.108(3) 0.6648(9) 0.6366(8) 0.147(12) Uiso 1 1 d D . . H14A H 0.1811 0.6403 0.6447 0.177 Uiso 1 1 calc R . . H14B H 0.0412 0.6695 0.6598 0.177 Uiso 1 1 calc R . . C15 C 0.032(4) 0.6484(12) 0.5981(11) 0.212(16) Uiso 1 1 d D . . H15A H -0.0646 0.6589 0.6065 0.254 Uiso 1 1 calc R . . H15B H 0.0637 0.6757 0.5798 0.254 Uiso 1 1 calc R . . C16 C -0.010(5) 0.6132(15) 0.5658(12) 0.31(3) Uiso 1 1 d D . . H16A H -0.0342 0.6317 0.5407 0.469 Uiso 1 1 calc R . . H16B H -0.0926 0.5940 0.5751 0.469 Uiso 1 1 calc R . . H16C H 0.0683 0.5903 0.5601 0.469 Uiso 1 1 calc R . . N5 N 0.2125(11) 0.5862(4) 0.9134(3) 0.029(3) Uani 1 1 d D . . H5 H 0.2590 0.5728 0.8973 0.044 Uiso 1 1 calc R . . C17 C 0.2007(18) 0.5556(6) 0.9498(5) 0.068(5) Uiso 1 1 d D . . H17A H 0.1518 0.5244 0.9416 0.082 Uiso 1 1 calc R . . H17B H 0.1372 0.5733 0.9692 0.082 Uiso 1 1 calc R . . C18 C 0.327(2) 0.5410(9) 0.9731(7) 0.113(9) Uiso 1 1 d D . . H18A H 0.3763 0.5718 0.9818 0.136 Uiso 1 1 calc R . . H18B H 0.3905 0.5226 0.9542 0.136 Uiso 1 1 calc R . . C19 C 0.301(5) 0.5084(13) 1.0117(9) 0.245(19) Uiso 1 1 d D . . H19A H 0.2269 0.5235 1.0293 0.293 Uiso 1 1 calc R . . H19B H 0.2692 0.4746 1.0034 0.293 Uiso 1 1 calc R . . C20 C 0.437(6) 0.505(3) 1.035(2) 0.55(6) Uiso 1 1 d D . . H20A H 0.4255 0.4816 1.0582 0.824 Uiso 1 1 calc R . . H20B H 0.4620 0.5380 1.0457 0.824 Uiso 1 1 calc R . . H20C H 0.5115 0.4929 1.0166 0.824 Uiso 1 1 calc R . . N6 N 0.7153(12) 0.7500(3) 0.8434(3) 0.033(3) Uani 1 1 d D . . H6 H 0.7401 0.7377 0.8232 0.050 Uiso 1 1 calc R . . C21 C 0.723(3) 0.8044(6) 0.8393(6) 0.101(7) Uiso 1 1 d D . . H21A H 0.6739 0.8121 0.8132 0.121 Uiso 1 1 calc R . . H21B H 0.8246 0.8115 0.8342 0.121 Uiso 1 1 calc R . . C22 C 0.677(5) 0.8435(14) 0.8684(11) 0.33(3) Uiso 1 1 d D . . H22A H 0.5864 0.8357 0.8822 0.394 Uiso 1 1 calc R . . H22B H 0.6750 0.8773 0.8560 0.394 Uiso 1 1 calc R . . C23 C 0.807(5) 0.8342(16) 0.8959(11) 0.28(2) Uiso 1 1 d D . . H23A H 0.8162 0.7977 0.9000 0.335 Uiso 1 1 calc R . . H23B H 0.8920 0.8453 0.8804 0.335 Uiso 1 1 calc R . . C24 C 0.810(6) 0.8580(16) 0.9364(12) 0.35(3) Uiso 1 1 d D . . H24A H 0.8612 0.8366 0.9559 0.524 Uiso 1 1 calc R . . H24B H 0.7131 0.8630 0.9462 0.524 Uiso 1 1 calc R . . H24C H 0.8579 0.8904 0.9343 0.524 Uiso 1 1 calc R . . N7 N 0.2909(12) 0.5975(4) 0.7696(3) 0.035(3) Uani 1 1 d . . . H7 H 0.2440 0.5930 0.7887 0.052 Uiso 1 1 calc R . . C25 C 0.246(3) 0.5621(7) 0.7349(6) 0.104(7) Uiso 1 1 d D . . H25A H 0.2276 0.5285 0.7466 0.124 Uiso 1 1 calc R . . H25B H 0.1564 0.5743 0.7226 0.124 Uiso 1 1 calc R . . C26 C 0.352(3) 0.5581(13) 0.7029(9) 0.199(15) Uiso 1 1 d D . . H26A H 0.4402 0.5431 0.7135 0.239 Uiso 1 1 calc R . . H26B H 0.3728 0.5910 0.6904 0.239 Uiso 1 1 calc R . . C27 C 0.276(5) 0.5228(13) 0.6716(11) 0.223(15) Uiso 1 1 d D . . H27A H 0.2775 0.5431 0.6461 0.268 Uiso 1 1 calc R . . H27B H 0.3491 0.4968 0.6671 0.268 Uiso 1 1 calc R . . C28 C 0.142(6) 0.493(2) 0.666(3) 0.63(7) Uiso 1 1 d D . . H28A H 0.1447 0.4750 0.6402 0.939 Uiso 1 1 calc R . . H28B H 0.0606 0.5162 0.6663 0.939 Uiso 1 1 calc R . . H28C H 0.1318 0.4696 0.6893 0.939 Uiso 1 1 calc R . . N8 N 0.7311(12) 0.7290(3) 0.0091(3) 0.026(2) Uani 1 1 d . . . H8 H 0.7706 0.7483 0.0224 0.040 Uiso 1 1 calc R . . C29 C 0.724(2) 0.6800(6) 0.0318(5) 0.072(5) Uiso 1 1 d D . . H29A H 0.6748 0.6854 0.0584 0.086 Uiso 1 1 calc R . . H29B H 0.6666 0.6563 0.0154 0.086 Uiso 1 1 calc R . . C30 C 0.862(2) 0.6575(8) 0.0400(7) 0.100(8) Uiso 1 1 d D . . H30A H 0.9161 0.6795 0.0587 0.120 Uiso 1 1 calc R . . H30B H 0.9146 0.6546 0.0138 0.120 Uiso 1 1 calc R . . C31 C 0.848(4) 0.6049(10) 0.0600(10) 0.179(14) Uiso 1 1 d D . . H31A H 0.8576 0.5793 0.0381 0.215 Uiso 1 1 calc R . . H31B H 0.9269 0.6002 0.0797 0.215 Uiso 1 1 calc R . . C32 C 0.712(5) 0.596(2) 0.0823(18) 0.52(5) Uiso 1 1 d D . . H32A H 0.7118 0.5623 0.0937 0.775 Uiso 1 1 calc R . . H32B H 0.6332 0.6000 0.0630 0.775 Uiso 1 1 calc R . . H32C H 0.7030 0.6205 0.1047 0.775 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 0.0143(3) 0.0284(3) 0.0218(2) -0.0003(2) -0.0003(3) 0.0010(3) U2 0.0146(3) 0.0252(2) 0.0247(3) -0.0022(2) 0.0002(3) -0.0002(3) U3 0.0150(3) 0.0197(2) 0.0259(3) 0.0001(2) -0.0001(3) 0.0008(2) U4 0.0192(3) 0.0425(3) 0.0256(3) -0.0072(2) -0.0012(3) 0.0015(3) U5 0.0151(3) 0.0242(2) 0.0241(3) 0.0043(2) 0.0003(3) 0.0001(2) S1 0.015(2) 0.042(3) 0.031(3) 0.007(2) 0.0040(18) -0.0033(18) S2 0.014(2) 0.029(3) 0.020(2) 0.0046(19) -0.0042(16) 0.0005(16) S3 0.010(2) 0.028(2) 0.024(2) 0.0016(19) -0.0005(16) -0.0019(16) S4 0.013(2) 0.023(2) 0.022(2) 0.0020(18) 0.0013(15) -0.0021(15) S5 0.011(2) 0.032(2) 0.028(2) -0.009(2) 0.0009(16) -0.0004(16) S6 0.015(2) 0.025(2) 0.033(3) 0.000(2) 0.0020(18) -0.0007(16) S7 0.016(2) 0.030(2) 0.021(2) -0.0025(19) 0.0020(16) 0.0030(17) S8 0.027(3) 0.081(3) 0.024(2) -0.016(2) 0.0011(18) 0.008(2) S9 0.018(2) 0.021(2) 0.033(3) -0.002(2) -0.0008(19) 0.0004(16) O1 0.019(5) 0.032(6) 0.029(6) -0.006(5) 0.008(5) -0.003(4) O2 0.030(6) 0.032(4) 0.028(5) -0.011(4) 0.011(6) -0.008(5) O3 0.019(5) 0.045(5) 0.011(4) 0.002(3) -0.002(5) -0.004(5) O4 0.013(5) 0.044(7) 0.025(6) 0.000(5) 0.008(4) 0.001(5) O5 0.012(5) 0.040(5) 0.036(5) -0.003(4) 0.001(5) -0.001(5) O6 0.026(6) 0.015(6) 0.022(6) -0.006(5) -0.005(4) 0.001(4) O7 0.013(6) 0.035(6) 0.034(6) 0.000(5) -0.003(4) -0.004(4) O8 0.025(6) 0.019(6) 0.042(7) 0.000(5) -0.010(5) -0.005(4) O10 0.022(6) 0.038(6) 0.030(6) 0.005(5) 0.000(5) 0.001(5) O11 0.020(5) 0.035(5) 0.038(5) 0.002(4) -0.002(6) 0.008(6) O13 0.029(6) 0.022(5) 0.032(5) -0.003(4) -0.011(4) 0.004(4) O14 0.036(7) 0.033(5) 0.026(5) 0.010(4) 0.005(5) 0.003(5) O15 0.028(6) 0.036(6) 0.021(6) 0.000(5) 0.005(5) -0.006(5) O16 0.036(6) 0.003(5) 0.021(6) 0.001(4) -0.002(4) 0.001(4) O17 0.019(5) 0.017(5) 0.027(6) 0.002(5) 0.002(5) 0.006(4) O18 0.034(6) 0.025(4) 0.035(5) -0.007(4) 0.007(6) -0.007(6) O19 0.017(5) 0.046(5) 0.022(4) 0.004(4) -0.002(5) 0.013(5) O20 0.023(6) 0.057(7) 0.016(6) -0.004(5) -0.003(4) 0.003(5) O21 0.005(5) 0.037(5) 0.028(5) -0.012(4) 0.005(4) -0.004(4) O22 0.027(7) 0.044(6) 0.048(6) -0.014(5) -0.014(5) -0.012(5) O23 0.022(6) 0.030(6) 0.037(7) 0.017(5) 0.004(4) -0.004(4) O24 0.032(7) 0.049(6) 0.046(6) 0.001(5) -0.021(6) 0.011(5) O25 0.014(6) 0.035(6) 0.026(6) 0.005(5) -0.006(4) 0.004(4) O26 0.013(6) 0.083(8) 0.035(6) -0.023(5) -0.002(4) 0.000(5) O27 0.018(6) 0.036(6) 0.020(5) 0.010(4) -0.003(4) 0.008(4) O28 0.013(5) 0.031(6) 0.032(6) -0.007(5) -0.002(5) -0.003(4) O29 0.017(6) 0.044(7) 0.027(6) 0.005(5) -0.005(5) -0.012(5) O30 0.023(6) 0.036(6) 0.049(7) -0.003(5) 0.002(5) 0.015(5) O31 0.013(5) 0.039(6) 0.019(5) 0.005(4) 0.003(4) -0.003(4) O32 0.017(6) 0.029(5) 0.027(5) -0.011(4) -0.006(4) 0.004(4) O33 0.033(7) 0.062(8) 0.060(9) -0.013(7) -0.005(6) -0.001(6) O34 0.020(6) 0.043(6) 0.030(6) -0.010(5) 0.000(5) -0.007(5) O35 0.022(6) 0.031(6) 0.048(7) 0.010(5) 0.007(5) -0.006(4) O36 0.032(7) 0.080(8) 0.037(7) -0.021(6) -0.003(5) -0.012(6) O37 0.023(6) 0.028(6) 0.038(7) -0.007(5) -0.001(5) 0.003(5) O38 0.031(6) 0.038(6) 0.018(6) 0.005(5) 0.009(5) -0.007(5) O39 0.037(7) 0.035(6) 0.023(6) 0.008(5) 0.000(5) -0.008(5) O40 0.023(7) 0.083(9) 0.046(7) -0.019(7) -0.008(5) -0.004(6) O41 0.017(6) 0.025(6) 0.039(7) -0.005(5) -0.004(5) -0.001(4) O42 0.030(7) 0.054(7) 0.050(7) -0.017(6) -0.013(5) 0.018(5) O43 0.018(6) 0.042(7) 0.048(7) 0.008(5) 0.010(5) 0.006(5) O44 0.046(8) 0.116(11) 0.033(7) -0.003(7) 0.013(6) 0.020(7) O45 0.045(8) 0.028(6) 0.068(9) 0.018(6) 0.025(6) 0.015(5) O46 0.014(6) 0.028(6) 0.044(7) -0.006(5) 0.010(5) -0.005(4) O47 0.008(6) 0.046(7) 0.059(8) 0.001(6) 0.004(5) -0.002(5) O1W 0.125(13) 0.091(11) 0.059(10) 0.006(8) 0.012(9) 0.010(9) N1 0.029(8) 0.045(7) 0.038(6) -0.005(5) -0.001(8) 0.002(7) N2 0.033(7) 0.036(6) 0.022(5) -0.001(4) 0.002(7) -0.017(7) N4 0.038(8) 0.041(6) 0.046(7) 0.011(5) -0.018(8) -0.001(8) N5 0.013(7) 0.040(6) 0.036(7) 0.000(5) 0.007(6) 0.000(5) N6 0.053(9) 0.014(5) 0.033(6) -0.001(5) 0.008(7) -0.005(6) N7 0.032(9) 0.057(8) 0.016(6) -0.013(5) 0.002(5) -0.014(6) N8 0.016(6) 0.024(6) 0.040(6) -0.009(5) -0.011(6) -0.004(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 U1 O19 1.738(7) . ? U1 O3 1.740(7) . ? U1 O4 2.305(9) . ? U1 O1 2.319(10) . ? U1 O25 2.425(8) . ? U1 O10 2.482(9) . ? U1 O21 2.492(8) . ? U2 O5 1.738(8) . ? U2 O2 1.755(7) . ? U2 O37 2.280(10) . ? U2 O6 2.358(9) . ? U2 O41 2.410(9) . ? U2 O32 2.484(8) . ? U2 O7 2.500(9) . ? U2 S7 3.123(4) 1_455 ? U3 O13 1.724(8) . ? U3 O18 1.748(7) . ? U3 O30 2.334(9) 1_455 ? U3 O8 2.339(9) . ? U3 O16 2.353(9) . ? U3 O46 2.482(8) . ? U3 O28 2.483(8) . ? U4 O22 1.727(9) . ? U4 O24 1.747(8) . ? U4 O38 2.328(10) . ? U4 O40 2.334(10) . ? U4 O15 2.387(10) . ? U4 O26 2.448(8) . ? U4 O33 2.479(11) . ? U5 O14 1.732(8) . ? U5 O11 1.761(7) . ? U5 O35 2.313(9) 1_455 ? U5 O23 2.316(10) . ? U5 O17 2.332(9) . ? U5 O27 2.459(8) . ? U5 O31 2.469(8) . ? S1 O45 1.417(10) . ? S1 O36 1.445(10) . ? S1 O35 1.485(9) . ? S1 O4 1.486(10) . ? S2 O29 1.469(10) . ? S2 O1 1.490(11) . ? S2 O31 1.498(9) . ? S2 O27 1.515(9) . ? S3 O47 1.441(9) . ? S3 O15 1.456(10) . ? S3 O17 1.485(9) . ? S3 O8 1.526(10) 3_656 ? S4 O12 1.442(9) . ? S4 O16 1.460(9) 3_656 ? S4 O38 1.478(10) . ? S4 O23 1.495(10) . ? S5 O34 1.443(10) . ? S5 O10 1.493(10) . ? S5 O41 1.500(10) . ? S5 O21 1.514(8) . ? S6 O39 1.441(9) . ? S6 O6 1.480(10) . ? S6 O46 1.482(9) . ? S6 O28 1.490(9) . ? S7 O20 1.432(9) . ? S7 O7 1.474(10) 1_655 ? S7 O25 1.483(9) . ? S7 O32 1.485(9) 1_655 ? S7 U2 3.123(4) 1_655 ? S8 O44 1.427(12) . ? S8 O33 1.461(11) . ? S8 O26 1.487(9) . ? S8 O40 1.496(11) 4_566 ? S9 O43 1.439(10) . ? S9 O42 1.468(10) . ? S9 O30 1.473(9) . ? S9 O37 1.532(10) . ? O7 S7 1.474(10) 1_455 ? O8 S3 1.526(10) 3_646 ? O16 S4 1.460(9) 3_646 ? O30 U3 2.334(9) 1_655 ? O32 S7 1.485(9) 1_455 ? O35 U5 2.313(9) 1_655 ? O40 S8 1.496(11) 4_466 ? N1 C1 1.515(15) . ? C1 C2 1.557(16) . ? C2 C3 1.550(18) . ? C3 C4 1.488(18) . ? N2 C5 1.458(15) . ? C5 C6 1.457(16) . ? C6 C7 1.525(18) . ? C7 C8 1.508(19) . ? N3 C9 1.467(16) . ? C9 C10 1.466(18) . ? C10 C11 1.541(19) . ? C11 C12 1.50(2) . ? N4 C13 1.531(19) . ? C13 C14 1.493(17) . ? C14 C15 1.504(18) . ? C15 C16 1.461(19) . ? N5 C17 1.439(13) . ? C17 C18 1.461(16) . ? C18 C19 1.546(18) . ? C19 C20 1.49(2) . ? N6 C21 1.464(14) . ? C21 C22 1.472(19) . ? C22 C23 1.54(2) . ? C23 C24 1.460(19) . ? N7 C25 1.531(19) . ? C25 C26 1.446(18) . ? C26 C27 1.556(19) . ? C27 C28 1.51(2) . ? N8 C29 1.505(16) . ? C29 C30 1.459(16) . ? C30 C31 1.556(18) . ? C31 C32 1.49(2) . ? 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 O19 U1 O3 179.0(4) . . ? O19 U1 O4 91.0(4) . . ? O3 U1 O4 90.0(4) . . ? O19 U1 O1 89.7(4) . . ? O3 U1 O1 90.6(4) . . ? O4 U1 O1 82.8(3) . . ? O19 U1 O25 86.4(4) . . ? O3 U1 O25 93.7(4) . . ? O4 U1 O25 76.3(3) . . ? O1 U1 O25 158.7(3) . . ? O19 U1 O10 87.2(4) . . ? O3 U1 O10 91.9(4) . . ? O4 U1 O10 156.2(3) . . ? O1 U1 O10 73.4(3) . . ? O25 U1 O10 127.2(3) . . ? O19 U1 O21 95.0(3) . . ? O3 U1 O21 84.0(3) . . ? O4 U1 O21 147.1(3) . . ? O1 U1 O21 129.4(3) . . ? O25 U1 O21 71.8(3) . . ? O10 U1 O21 56.6(3) . . ? O5 U2 O2 177.7(4) . . ? O5 U2 O37 91.2(4) . . ? O2 U2 O37 88.9(4) . . ? O5 U2 O6 90.6(4) . . ? O2 U2 O6 91.7(4) . . ? O37 U2 O6 82.3(3) . . ? O5 U2 O41 85.8(4) . . ? O2 U2 O41 92.0(4) . . ? O37 U2 O41 76.6(3) . . ? O6 U2 O41 158.5(3) . . ? O5 U2 O32 94.8(3) . . ? O2 U2 O32 84.0(3) . . ? O37 U2 O32 148.3(3) . . ? O6 U2 O32 128.7(3) . . ? O41 U2 O32 72.8(3) . . ? O5 U2 O7 86.7(4) . . ? O2 U2 O7 94.2(4) . . ? O37 U2 O7 156.2(3) . . ? O6 U2 O7 74.0(3) . . ? O41 U2 O7 126.8(3) . . ? O32 U2 O7 55.5(3) . . ? O5 U2 S7 91.7(3) . 1_455 ? O2 U2 S7 88.1(3) . 1_455 ? O37 U2 S7 175.5(3) . 1_455 ? O6 U2 S7 101.2(2) . 1_455 ? O41 U2 S7 100.1(2) . 1_455 ? O32 U2 S7 27.8(2) . 1_455 ? O7 U2 S7 27.7(2) . 1_455 ? O13 U3 O18 178.7(4) . . ? O13 U3 O30 87.4(4) . 1_455 ? O18 U3 O30 92.8(4) . 1_455 ? O13 U3 O8 94.0(4) . . ? O18 U3 O8 87.3(4) . . ? O30 U3 O8 79.3(3) 1_455 . ? O13 U3 O16 88.8(3) . . ? O18 U3 O16 91.6(4) . . ? O30 U3 O16 159.6(3) 1_455 . ? O8 U3 O16 81.0(3) . . ? O13 U3 O46 89.3(4) . . ? O18 U3 O46 89.6(4) . . ? O30 U3 O46 128.9(3) 1_455 . ? O8 U3 O46 151.8(3) . . ? O16 U3 O46 71.1(3) . . ? O13 U3 O28 89.5(3) . . ? O18 U3 O28 89.3(3) . . ? O30 U3 O28 72.8(3) 1_455 . ? O8 U3 O28 151.7(3) . . ? O16 U3 O28 127.3(3) . . ? O46 U3 O28 56.2(3) . . ? O22 U4 O24 179.2(4) . . ? O22 U4 O38 92.3(4) . . ? O24 U4 O38 88.3(4) . . ? O22 U4 O40 89.4(4) . . ? O24 U4 O40 90.2(4) . . ? O38 U4 O40 79.3(3) . . ? O22 U4 O15 89.3(4) . . ? O24 U4 O15 91.2(4) . . ? O38 U4 O15 78.2(3) . . ? O40 U4 O15 157.4(3) . . ? O22 U4 O26 88.9(4) . . ? O24 U4 O26 90.4(4) . . ? O38 U4 O26 155.4(3) . . ? O40 U4 O26 76.1(3) . . ? O15 U4 O26 126.4(3) . . ? O22 U4 O33 91.2(4) . . ? O24 U4 O33 88.5(4) . . ? O38 U4 O33 148.5(3) . . ? O40 U4 O33 132.0(3) . . ? O15 U4 O33 70.5(3) . . ? O26 U4 O33 56.0(3) . . ? O14 U5 O11 178.6(3) . . ? O14 U5 O35 86.8(4) . 1_455 ? O11 U5 O35 92.3(4) . 1_455 ? O14 U5 O23 95.9(4) . . ? O11 U5 O23 84.9(4) . . ? O35 U5 O23 78.7(3) 1_455 . ? O14 U5 O17 88.9(3) . . ? O11 U5 O17 92.4(3) . . ? O35 U5 O17 155.3(3) 1_455 . ? O23 U5 O17 77.6(3) . . ? O14 U5 O27 91.6(3) . . ? O11 U5 O27 87.1(3) . . ? O35 U5 O27 72.8(3) 1_455 . ? O23 U5 O27 150.1(3) . . ? O17 U5 O27 131.6(3) . . ? O14 U5 O31 90.5(4) . . ? O11 U5 O31 89.3(4) . . ? O35 U5 O31 129.7(3) 1_455 . ? O23 U5 O31 151.3(3) . . ? O17 U5 O31 74.6(3) . . ? O27 U5 O31 57.1(3) . . ? O45 S1 O36 112.1(7) . . ? O45 S1 O35 110.7(6) . . ? O36 S1 O35 110.1(6) . . ? O45 S1 O4 110.0(7) . . ? O36 S1 O4 109.7(6) . . ? O35 S1 O4 104.0(6) . . ? O29 S2 O1 111.0(6) . . ? O29 S2 O31 112.9(6) . . ? O1 S2 O31 109.9(6) . . ? O29 S2 O27 111.2(5) . . ? O1 S2 O27 108.7(5) . . ? O31 S2 O27 102.8(5) . . ? O47 S3 O15 108.6(6) . . ? O47 S3 O17 109.2(6) . . ? O15 S3 O17 109.2(6) . . ? O47 S3 O8 108.7(6) . 3_656 ? O15 S3 O8 111.0(6) . 3_656 ? O17 S3 O8 110.1(6) . 3_656 ? O12 S4 O16 110.4(6) . 3_656 ? O12 S4 O38 111.3(6) . . ? O16 S4 O38 107.7(6) 3_656 . ? O12 S4 O23 110.6(6) . . ? O16 S4 O23 108.5(6) 3_656 . ? O38 S4 O23 108.2(6) . . ? O34 S5 O10 114.4(6) . . ? O34 S5 O41 110.0(6) . . ? O10 S5 O41 110.1(6) . . ? O34 S5 O21 109.9(5) . . ? O10 S5 O21 103.3(5) . . ? O41 S5 O21 109.0(5) . . ? O39 S6 O6 112.0(6) . . ? O39 S6 O46 114.4(6) . . ? O6 S6 O46 107.4(6) . . ? O39 S6 O28 110.1(6) . . ? O6 S6 O28 108.7(6) . . ? O46 S6 O28 103.8(5) . . ? O20 S7 O7 113.6(6) . 1_655 ? O20 S7 O25 111.0(6) . . ? O7 S7 O25 110.7(6) 1_655 . ? O20 S7 O32 110.3(5) . 1_655 ? O7 S7 O32 103.2(5) 1_655 1_655 ? O25 S7 O32 107.5(5) . 1_655 ? O20 S7 U2 129.1(4) . 1_655 ? O7 S7 U2 51.9(4) 1_655 1_655 ? O25 S7 U2 119.7(4) . 1_655 ? O32 S7 U2 51.4(3) 1_655 1_655 ? O44 S8 O33 111.4(7) . . ? O44 S8 O26 114.6(6) . . ? O33 S8 O26 103.3(6) . . ? O44 S8 O40 111.2(7) . 4_566 ? O33 S8 O40 108.8(7) . 4_566 ? O26 S8 O40 107.2(7) . 4_566 ? O43 S9 O42 114.6(7) . . ? O43 S9 O30 109.8(6) . . ? O42 S9 O30 110.4(6) . . ? O43 S9 O37 109.6(6) . . ? O42 S9 O37 107.9(6) . . ? O30 S9 O37 104.0(6) . . ? S2 O1 U1 143.4(6) . . ? S1 O4 U1 137.4(6) . . ? S6 O6 U2 141.9(6) . . ? S7 O7 U2 100.4(4) 1_455 . ? S3 O8 U3 140.6(6) 3_646 . ? S5 O10 U1 100.6(4) . . ? S3 O15 U4 135.8(6) . . ? S4 O16 U3 141.0(6) 3_646 . ? S3 O17 U5 143.8(6) . . ? S5 O21 U1 99.5(4) . . ? S4 O23 U5 139.5(6) . . ? S7 O25 U1 136.9(5) . . ? S8 O26 U4 100.6(4) . . ? S2 O27 U5 99.8(4) . . ? S6 O28 U3 99.8(4) . . ? S9 O30 U3 147.6(6) . 1_655 ? S2 O31 U5 99.9(4) . . ? S7 O32 U2 100.8(4) 1_455 . ? S8 O33 U4 100.1(5) . . ? S1 O35 U5 147.6(6) . 1_655 ? S9 O37 U2 139.4(6) . . ? S4 O38 U4 159.7(6) . . ? S8 O40 U4 138.5(7) 4_466 . ? S5 O41 U2 137.6(6) . . ? S6 O46 U3 100.1(4) . . ? N1 C1 C2 111.3(16) . . ? C3 C2 C1 116(2) . . ? C4 C3 C2 109(3) . . ? C6 C5 N2 112.8(17) . . ? C5 C6 C7 114(2) . . ? C8 C7 C6 125(3) . . ? C10 C9 N3 123.8(19) . . ? C9 C10 C11 113(3) . . ? C12 C11 C10 128(6) . . ? C14 C13 N4 107.6(17) . . ? C15 C14 C13 103.2(19) . . ? C16 C15 C14 156(4) . . ? N5 C17 C18 120.8(15) . . ? C17 C18 C19 116(2) . . ? C20 C19 C18 108(4) . . ? N6 C21 C22 129(2) . . ? C21 C22 C23 91(2) . . ? C24 C23 C22 118(4) . . ? C26 C25 N7 112(2) . . ? C25 C26 C27 101(2) . . ? C28 C27 C26 141(5) . . ? C30 C29 N8 114.1(15) . . ? C29 C30 C31 112(2) . . ? C32 C31 C30 115(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O29 S2 O1 U1 -16.5(11) . . . . ? O31 S2 O1 U1 -142.1(8) . . . . ? O27 S2 O1 U1 106.2(9) . . . . ? O19 U1 O1 S2 -173.2(10) . . . . ? O3 U1 O1 S2 5.8(10) . . . . ? O4 U1 O1 S2 95.7(10) . . . . ? O25 U1 O1 S2 107.4(11) . . . . ? O10 U1 O1 S2 -86.0(9) . . . . ? O21 U1 O1 S2 -77.0(10) . . . . ? O45 S1 O4 U1 -68.8(10) . . . . ? O36 S1 O4 U1 54.9(11) . . . . ? O35 S1 O4 U1 172.7(7) . . . . ? O19 U1 O4 S1 -157.4(9) . . . . ? O3 U1 O4 S1 22.8(9) . . . . ? O1 U1 O4 S1 -67.8(8) . . . . ? O25 U1 O4 S1 116.5(9) . . . . ? O10 U1 O4 S1 -72.1(13) . . . . ? O21 U1 O4 S1 101.8(9) . . . . ? O39 S6 O6 U2 15.8(11) . . . . ? O46 S6 O6 U2 142.3(8) . . . . ? O28 S6 O6 U2 -106.1(9) . . . . ? O5 U2 O6 S6 172.8(9) . . . . ? O2 U2 O6 S6 -7.5(10) . . . . ? O37 U2 O6 S6 -96.1(9) . . . . ? O41 U2 O6 S6 -107.3(11) . . . . ? O32 U2 O6 S6 76.2(10) . . . . ? O7 U2 O6 S6 86.4(9) . . . . ? S7 U2 O6 S6 80.9(9) 1_455 . . . ? O5 U2 O7 S7 100.0(5) . . . 1_455 ? O2 U2 O7 S7 -77.8(5) . . . 1_455 ? O37 U2 O7 S7 -174.5(7) . . . 1_455 ? O6 U2 O7 S7 -168.4(6) . . . 1_455 ? O41 U2 O7 S7 17.7(6) . . . 1_455 ? O32 U2 O7 S7 1.9(4) . . . 1_455 ? O13 U3 O8 S3 -25.7(10) . . . 3_646 ? O18 U3 O8 S3 154.5(10) . . . 3_646 ? O30 U3 O8 S3 -112.2(10) 1_455 . . 3_646 ? O16 U3 O8 S3 62.4(9) . . . 3_646 ? O46 U3 O8 S3 70.5(13) . . . 3_646 ? O28 U3 O8 S3 -122.1(9) . . . 3_646 ? O34 S5 O10 U1 120.4(5) . . . . ? O41 S5 O10 U1 -115.2(5) . . . . ? O21 S5 O10 U1 1.0(5) . . . . ? O19 U1 O10 S5 -98.6(5) . . . . ? O3 U1 O10 S5 80.9(5) . . . . ? O4 U1 O10 S5 175.3(7) . . . . ? O1 U1 O10 S5 170.9(6) . . . . ? O25 U1 O10 S5 -15.2(6) . . . . ? O21 U1 O10 S5 -0.7(4) . . . . ? O47 S3 O15 U4 134.5(8) . . . . ? O17 S3 O15 U4 15.5(10) . . . . ? O8 S3 O15 U4 -106.0(8) 3_656 . . . ? O22 U4 O15 S3 -42.2(9) . . . . ? O24 U4 O15 S3 138.3(9) . . . . ? O38 U4 O15 S3 50.3(8) . . . . ? O40 U4 O15 S3 44.8(15) . . . . ? O26 U4 O15 S3 -130.3(8) . . . . ? O33 U4 O15 S3 -133.7(9) . . . . ? O13 U3 O16 S4 25.2(9) . . . 3_646 ? O18 U3 O16 S4 -156.1(9) . . . 3_646 ? O30 U3 O16 S4 -53.8(15) 1_455 . . 3_646 ? O8 U3 O16 S4 -69.1(9) . . . 3_646 ? O46 U3 O16 S4 114.9(9) . . . 3_646 ? O28 U3 O16 S4 113.6(9) . . . 3_646 ? O47 S3 O17 U5 104.7(9) . . . . ? O15 S3 O17 U5 -136.7(8) . . . . ? O8 S3 O17 U5 -14.6(11) 3_656 . . . ? O14 U5 O17 S3 -4.8(9) . . . . ? O11 U5 O17 S3 175.8(9) . . . . ? O35 U5 O17 S3 75.0(13) 1_455 . . . ? O23 U5 O17 S3 91.6(9) . . . . ? O27 U5 O17 S3 -95.9(9) . . . . ? O31 U5 O17 S3 -95.6(9) . . . . ? O34 S5 O21 U1 -123.4(5) . . . . ? O10 S5 O21 U1 -1.0(5) . . . . ? O41 S5 O21 U1 116.1(5) . . . . ? O19 U1 O21 S5 84.0(5) . . . . ? O3 U1 O21 S5 -95.5(5) . . . . ? O4 U1 O21 S5 -176.3(5) . . . . ? O1 U1 O21 S5 -9.7(6) . . . . ? O25 U1 O21 S5 168.6(5) . . . . ? O10 U1 O21 S5 0.7(4) . . . . ? O12 S4 O23 U5 -150.2(8) . . . . ? O16 S4 O23 U5 -29.0(11) 3_656 . . . ? O38 S4 O23 U5 87.6(10) . . . . ? O14 U5 O23 S4 33.7(9) . . . . ? O11 U5 O23 S4 -147.4(10) . . . . ? O35 U5 O23 S4 119.2(9) 1_455 . . . ? O17 U5 O23 S4 -53.8(8) . . . . ? O27 U5 O23 S4 137.4(7) . . . . ? O31 U5 O23 S4 -68.3(12) . . . . ? O20 S7 O25 U1 -84.2(9) . . . . ? O7 S7 O25 U1 42.9(9) 1_655 . . . ? O32 S7 O25 U1 155.0(7) 1_655 . . . ? U2 S7 O25 U1 100.0(7) 1_655 . . . ? O19 U1 O25 S7 134.3(8) . . . . ? O3 U1 O25 S7 -44.7(8) . . . . ? O4 U1 O25 S7 -133.8(9) . . . . ? O1 U1 O25 S7 -145.8(9) . . . . ? O10 U1 O25 S7 50.5(9) . . . . ? O21 U1 O25 S7 37.8(8) . . . . ? O44 S8 O26 U4 -121.4(6) . . . . ? O33 S8 O26 U4 -0.1(7) . . . . ? O40 S8 O26 U4 114.7(5) 4_566 . . . ? O22 U4 O26 S8 -92.1(6) . . . . ? O24 U4 O26 S8 88.0(6) . . . . ? O38 U4 O26 S8 174.8(6) . . . . ? O40 U4 O26 S8 178.2(6) . . . . ? O15 U4 O26 S8 -3.8(7) . . . . ? O33 U4 O26 S8 0.1(5) . . . . ? O29 S2 O27 U5 -115.2(5) . . . . ? O1 S2 O27 U5 122.2(5) . . . . ? O31 S2 O27 U5 5.9(5) . . . . ? O14 U5 O27 S2 -93.6(5) . . . . ? O11 U5 O27 S2 86.9(5) . . . . ? O35 U5 O27 S2 -179.7(5) 1_455 . . . ? O23 U5 O27 S2 161.5(5) . . . . ? O17 U5 O27 S2 -3.7(6) . . . . ? O31 U5 O27 S2 -4.1(4) . . . . ? O39 S6 O28 U3 119.3(5) . . . . ? O6 S6 O28 U3 -117.6(5) . . . . ? O46 S6 O28 U3 -3.5(6) . . . . ? O13 U3 O28 S6 92.0(5) . . . . ? O18 U3 O28 S6 -87.5(5) . . . . ? O30 U3 O28 S6 179.4(6) 1_455 . . . ? O8 U3 O28 S6 -170.4(6) . . . . ? O16 U3 O28 S6 4.0(6) . . . . ? O46 U3 O28 S6 2.5(4) . . . . ? O43 S9 O30 U3 -44.4(13) . . . 1_655 ? O42 S9 O30 U3 82.9(13) . . . 1_655 ? O37 S9 O30 U3 -161.6(10) . . . 1_655 ? O29 S2 O31 U5 114.1(5) . . . . ? O1 S2 O31 U5 -121.4(5) . . . . ? O27 S2 O31 U5 -5.8(5) . . . . ? O14 U5 O31 S2 95.8(5) . . . . ? O11 U5 O31 S2 -82.8(5) . . . . ? O35 U5 O31 S2 9.6(6) 1_455 . . . ? O23 U5 O31 S2 -160.9(5) . . . . ? O17 U5 O31 S2 -175.5(5) . . . . ? O27 U5 O31 S2 4.2(4) . . . . ? O5 U2 O32 S7 -84.6(5) . . . 1_455 ? O2 U2 O32 S7 97.4(5) . . . 1_455 ? O37 U2 O32 S7 175.4(5) . . . 1_455 ? O6 U2 O32 S7 10.0(6) . . . 1_455 ? O41 U2 O32 S7 -168.7(5) . . . 1_455 ? O7 U2 O32 S7 -1.9(4) . . . 1_455 ? O44 S8 O33 U4 123.6(6) . . . . ? O26 S8 O33 U4 0.1(7) . . . . ? O40 S8 O33 U4 -113.6(6) 4_566 . . . ? O22 U4 O33 S8 87.8(6) . . . . ? O24 U4 O33 S8 -91.5(6) . . . . ? O38 U4 O33 S8 -175.9(5) . . . . ? O40 U4 O33 S8 -2.5(9) . . . . ? O15 U4 O33 S8 176.7(7) . . . . ? O26 U4 O33 S8 -0.1(5) . . . . ? O45 S1 O35 U5 42.5(13) . . . 1_655 ? O36 S1 O35 U5 -81.9(12) . . . 1_655 ? O4 S1 O35 U5 160.6(10) . . . 1_655 ? O43 S9 O37 U2 69.0(10) . . . . ? O42 S9 O37 U2 -56.4(11) . . . . ? O30 S9 O37 U2 -173.6(9) . . . . ? O5 U2 O37 S9 157.9(10) . . . . ? O2 U2 O37 S9 -24.4(10) . . . . ? O6 U2 O37 S9 67.5(9) . . . . ? O41 U2 O37 S9 -116.7(10) . . . . ? O32 U2 O37 S9 -101.0(10) . . . . ? O7 U2 O37 S9 73.4(14) . . . . ? S7 U2 O37 S9 -72(4) 1_455 . . . ? O12 S4 O38 U4 -118.8(17) . . . . ? O16 S4 O38 U4 120.0(17) 3_656 . . . ? O23 S4 O38 U4 2.9(19) . . . . ? O22 U4 O38 S4 6.3(18) . . . . ? O24 U4 O38 S4 -174.1(18) . . . . ? O40 U4 O38 S4 95.3(18) . . . . ? O15 U4 O38 S4 -82.5(17) . . . . ? O26 U4 O38 S4 98.6(19) . . . . ? O33 U4 O38 S4 -89.7(19) . . . . ? O22 U4 O40 S8 -5.6(10) . . . 4_466 ? O24 U4 O40 S8 173.8(10) . . . 4_466 ? O38 U4 O40 S8 -98.0(10) . . . 4_466 ? O15 U4 O40 S8 -92.5(13) . . . 4_466 ? O26 U4 O40 S8 83.4(9) . . . 4_466 ? O33 U4 O40 S8 85.5(10) . . . 4_466 ? O34 S5 O41 U2 86.1(9) . . . . ? O10 S5 O41 U2 -40.8(10) . . . . ? O21 S5 O41 U2 -153.5(7) . . . . ? O5 U2 O41 S5 -137.5(9) . . . . ? O2 U2 O41 S5 42.0(9) . . . . ? O37 U2 O41 S5 130.4(9) . . . . ? O6 U2 O41 S5 141.7(8) . . . . ? O32 U2 O41 S5 -41.1(8) . . . . ? O7 U2 O41 S5 -54.7(9) . . . . ? S7 U2 O41 S5 -46.4(9) 1_455 . . . ? O39 S6 O46 U3 -116.4(5) . . . . ? O6 S6 O46 U3 118.5(5) . . . . ? O28 S6 O46 U3 3.5(6) . . . . ? O13 U3 O46 S6 -92.3(5) . . . . ? O18 U3 O46 S6 87.0(5) . . . . ? O30 U3 O46 S6 -6.2(7) 1_455 . . . ? O8 U3 O46 S6 170.4(6) . . . . ? O16 U3 O46 S6 178.8(6) . . . . ? O28 U3 O46 S6 -2.5(4) . . . . ? N1 C1 C2 C3 -60(3) . . . . ? C1 C2 C3 C4 -62(4) . . . . ? N2 C5 C6 C7 72(3) . . . . ? C5 C6 C7 C8 53(4) . . . . ? N3 C9 C10 C11 175(3) . . . . ? C9 C10 C11 C12 -65(8) . . . . ? N4 C13 C14 C15 -178(2) . . . . ? C13 C14 C15 C16 132(9) . . . . ? N5 C17 C18 C19 180(2) . . . . ? C17 C18 C19 C20 -170(4) . . . . ? N6 C21 C22 C23 76(4) . . . . ? C21 C22 C23 C24 -170(4) . . . . ? N7 C25 C26 C27 -177(2) . . . . ? C25 C26 C27 C28 -3(9) . . . . ? N8 C29 C30 C31 -174.9(19) . . . . ? C29 C30 C31 C32 -24(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O26 0.77 2.17 2.930(13) 170.6 4_466 N2 H2 O47 0.77 2.10 2.831(14) 157.9 1_455 N4 H4 O12 0.77 2.16 2.928(14) 171.7 . N5 H5 O28 0.77 2.10 2.863(13) 171.7 . N6 H6 O27 0.77 2.09 2.833(13) 162.9 . N7 H7 O43 0.77 2.23 2.940(14) 153.7 1_455 N8 H8 O20 0.77 2.24 2.941(13) 151.2 4_466 N8 H8 O21 0.77 2.49 3.023(12) 128.1 4_466 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.061 _refine_diff_density_min -0.729 _refine_diff_density_rms 0.150