# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_NH4+ #TrackingRef 'NH4 .cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H6 N2 O23 U2' _chemical_formula_sum 'C18 H6 N2 O23 U2' _chemical_formula_weight 1094.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_space_group_name_Hall '-C 2yc ' 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 7.8622(8) _cell_length_b 17.8077(17) _cell_length_c 21.8192(19) _cell_angle_alpha 90.00 _cell_angle_beta 104.023(4) _cell_angle_gamma 90.00 _cell_volume 2963.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12691 _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 27.60 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 11.012 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2418 _exptl_absorpt_correction_T_max 0.2718 _exptl_absorpt_process_details Higashi,1995 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku SCXmini diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12065 _diffrn_reflns_av_R_equivalents 0.0801 _diffrn_reflns_av_sigmaI/netI 0.0661 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.02 _reflns_number_total 2626 _reflns_number_gt 2156 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0354P)^2^+8.8290P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2626 _refine_ls_number_parameters 204 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0646 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.0961 _refine_ls_wR_factor_gt 0.0913 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.150 _refine_ls_shift/su_max 0.002 _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 O9 O 0.5938(9) 0.6967(4) 0.1155(4) 0.044(2) Uani 1 1 d . . . O10 O 0.7182(9) 0.6027(4) 0.0776(4) 0.0352(18) Uani 1 1 d . . . C9 C 0.7105(13) 0.6723(5) 0.0908(5) 0.030(2) Uani 1 1 d . . . U1 U 0.95559(5) 1.073574(19) 0.120124(19) 0.02557(15) Uani 1 1 d . . . O3 O 0.6992(9) 1.0638(3) 0.1683(4) 0.0334(18) Uani 1 1 d . . . O8 O 0.8182(8) 0.7975(3) 0.0924(3) 0.0274(16) Uani 1 1 d . . . O6 O 0.8351(9) 0.9457(3) 0.1128(4) 0.0362(19) Uani 1 1 d . . . O1 O 0.8118(9) 1.0944(3) 0.0474(3) 0.0345(18) Uani 1 1 d . . . O4 O 0.8268(9) 1.1746(4) 0.1716(4) 0.0368(19) Uani 1 1 d . . . O7 O 1.0729(9) 0.9595(3) 0.0780(4) 0.039(2) Uani 1 1 d . . . C5 C 0.9529(12) 0.8368(5) 0.0772(5) 0.026(2) Uani 1 1 d . . . C4 C 0.9522(13) 0.9183(5) 0.0905(6) 0.032(3) Uani 1 1 d . . . C1 C 0.7164(12) 1.1323(6) 0.1865(5) 0.026(2) Uani 1 1 d . . . C8 C 0.8405(12) 0.7239(5) 0.0766(5) 0.024(2) Uani 1 1 d . . . O5 O 0.5000 1.1181(5) 0.2500 0.030(2) Uani 1 2 d S . . C6 C 1.0519(13) 0.7906(5) 0.0519(5) 0.031(3) Uani 1 1 d . . . H6 H 1.1495 0.8036 0.0372 0.037 Uiso 1 1 calc R . . C3 C 0.5656(14) 1.2360(5) 0.2327(5) 0.039(3) Uani 1 1 d . . . H3 H 0.6183 1.2778 0.2196 0.046 Uiso 1 1 calc R . . C2 C 0.5981(13) 1.1646(6) 0.2227(5) 0.029(2) Uani 1 1 d . . . C7 C 0.9783(12) 0.7185(5) 0.0522(5) 0.029(2) Uani 1 1 d . . . H7 H 1.0195 0.6746 0.0377 0.035 Uiso 1 1 calc R . . O2 O 1.0992(10) 1.0528(4) 0.1924(4) 0.041(2) Uani 1 1 d . . . N2 N 0.745(4) 0.4092(9) 0.2476(10) 0.225(13) Uani 1 1 d . . . O2W O 0.5023(19) 0.8378(9) 0.1576(10) 0.217(10) Uani 1 1 d . . . O1W O 0.4443(15) 0.9798(9) 0.0616(10) 0.213(11) 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 O9 0.045(5) 0.030(4) 0.067(6) -0.004(4) 0.036(5) -0.008(3) O10 0.033(4) 0.020(4) 0.056(6) -0.002(3) 0.017(4) -0.006(3) C9 0.035(7) 0.029(6) 0.026(7) 0.000(4) 0.006(5) 0.000(5) U1 0.0292(3) 0.0222(2) 0.0274(3) -0.00209(17) 0.01097(18) -0.00628(17) O3 0.036(4) 0.029(4) 0.038(5) -0.006(3) 0.016(4) -0.010(3) O8 0.033(4) 0.019(4) 0.033(5) -0.006(3) 0.013(3) -0.007(3) O6 0.036(4) 0.023(4) 0.058(6) -0.003(3) 0.026(4) 0.004(3) O1 0.048(5) 0.027(4) 0.031(5) -0.006(3) 0.016(4) -0.004(3) O4 0.040(5) 0.033(4) 0.045(5) -0.006(3) 0.024(4) -0.008(3) O7 0.040(5) 0.016(4) 0.064(6) -0.007(3) 0.020(4) -0.010(3) C5 0.024(6) 0.019(5) 0.033(7) 0.001(4) 0.004(5) -0.009(4) C4 0.034(6) 0.020(6) 0.041(8) 0.007(5) 0.008(5) -0.009(5) C1 0.023(6) 0.037(6) 0.018(6) 0.007(5) 0.002(5) 0.004(5) C8 0.031(6) 0.009(5) 0.030(7) 0.002(4) 0.006(5) 0.003(4) O5 0.026(6) 0.030(6) 0.039(7) 0.000 0.014(5) 0.000 C6 0.029(6) 0.026(6) 0.043(8) 0.005(5) 0.019(5) -0.002(4) C3 0.047(7) 0.024(6) 0.050(9) 0.007(5) 0.022(6) -0.005(5) C2 0.027(6) 0.039(6) 0.022(7) -0.003(5) 0.007(5) -0.004(5) C7 0.030(6) 0.025(5) 0.029(7) 0.000(4) 0.001(5) 0.004(4) O2 0.053(5) 0.036(4) 0.036(5) -0.007(3) 0.014(4) -0.012(4) N2 0.41(3) 0.081(13) 0.124(18) -0.002(11) -0.06(2) 0.023(16) O2W 0.130(13) 0.156(15) 0.37(3) -0.144(16) 0.074(15) 0.011(11) O1W 0.057(8) 0.198(16) 0.37(3) -0.193(18) 0.016(11) -0.010(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O9 C9 1.248(11) . ? O9 U1 2.459(6) 3_445 ? O10 C9 1.276(11) . ? O10 U1 2.515(6) 3_445 ? C9 C8 1.464(13) . ? C9 U1 2.852(10) 3_445 ? U1 O2 1.742(8) . ? U1 O1 1.750(8) . ? U1 O6 2.456(6) . ? U1 O9 2.459(6) 3 ? U1 O4 2.465(6) . ? U1 O3 2.496(7) . ? U1 O7 2.497(6) . ? U1 O10 2.515(7) 3 ? U1 C9 2.852(10) 3 ? O3 C1 1.281(11) . ? O8 C5 1.375(10) . ? O8 C8 1.376(10) . ? O6 C4 1.241(12) . ? O4 C1 1.249(11) . ? O7 C4 1.280(11) . ? C5 C6 1.339(13) . ? C5 C4 1.481(13) . ? C1 C2 1.476(13) . ? C8 C7 1.321(12) . ? O5 C2 1.363(10) . ? O5 C2 1.363(10) 2_655 ? C6 C7 1.410(13) . ? C6 H6 0.9300 . ? C3 C2 1.325(13) . ? C3 C3 1.417(19) 2_655 ? C3 H3 0.9300 . ? C7 H7 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 C9 O9 U1 94.9(6) . 3_445 ? C9 O10 U1 91.6(6) . 3_445 ? O9 C9 O10 121.1(9) . . ? O9 C9 C8 119.8(9) . . ? O10 C9 C8 119.2(9) . . ? O9 C9 U1 59.2(5) . 3_445 ? O10 C9 U1 61.8(5) . 3_445 ? C8 C9 U1 179.0(7) . 3_445 ? O2 U1 O1 179.8(3) . . ? O2 U1 O6 91.0(3) . . ? O1 U1 O6 89.1(3) . . ? O2 U1 O9 91.7(3) . 3 ? O1 U1 O9 88.2(3) . 3 ? O6 U1 O9 172.2(2) . 3 ? O2 U1 O4 89.4(3) . . ? O1 U1 O4 90.7(3) . . ? O6 U1 O4 120.8(2) . . ? O9 U1 O4 66.6(2) 3 . ? O2 U1 O3 91.0(3) . . ? O1 U1 O3 89.2(3) . . ? O6 U1 O3 67.9(2) . . ? O9 U1 O3 119.3(2) 3 . ? O4 U1 O3 52.8(2) . . ? O2 U1 O7 86.8(3) . . ? O1 U1 O7 93.1(3) . . ? O6 U1 O7 52.6(2) . . ? O9 U1 O7 120.2(2) 3 . ? O4 U1 O7 172.2(2) . . ? O3 U1 O7 120.4(2) . . ? O2 U1 O10 88.1(3) . 3 ? O1 U1 O10 91.7(3) . 3 ? O6 U1 O10 120.4(2) . 3 ? O9 U1 O10 52.4(2) 3 3 ? O4 U1 O10 118.8(2) . 3 ? O3 U1 O10 171.7(2) . 3 ? O7 U1 O10 67.8(2) . 3 ? O2 U1 C9 89.8(3) . 3 ? O1 U1 C9 90.0(3) . 3 ? O6 U1 C9 146.9(3) . 3 ? O9 U1 C9 25.9(2) 3 3 ? O4 U1 C9 92.4(3) . 3 ? O3 U1 C9 145.2(2) . 3 ? O7 U1 C9 94.4(3) . 3 ? O10 U1 C9 26.6(2) 3 3 ? C1 O3 U1 91.6(5) . . ? C5 O8 C8 105.8(7) . . ? C4 O6 U1 94.6(6) . . ? C1 O4 U1 93.8(6) . . ? C4 O7 U1 91.7(6) . . ? C6 C5 O8 110.2(7) . . ? C6 C5 C4 135.4(9) . . ? O8 C5 C4 114.3(8) . . ? O6 C4 O7 121.1(9) . . ? O6 C4 C5 120.1(8) . . ? O7 C4 C5 118.8(9) . . ? O4 C1 O3 121.5(9) . . ? O4 C1 C2 118.2(9) . . ? O3 C1 C2 120.3(8) . . ? C7 C8 O8 109.7(8) . . ? C7 C8 C9 136.3(9) . . ? O8 C8 C9 114.0(8) . . ? C2 O5 C2 105.1(10) . 2_655 ? C5 C6 C7 106.1(8) . . ? C5 C6 H6 127.0 . . ? C7 C6 H6 127.0 . . ? C2 C3 C3 106.4(6) . 2_655 ? C2 C3 H3 126.8 . . ? C3 C3 H3 126.8 2_655 . ? C3 C2 O5 111.1(9) . . ? C3 C2 C1 129.3(9) . . ? O5 C2 C1 119.6(8) . . ? C8 C7 C6 108.2(9) . . ? C8 C7 H7 125.9 . . ? C6 C7 H7 125.9 . . ? 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 U1 O9 C9 O10 0.6(11) 3_445 . . . ? U1 O9 C9 C8 -179.6(8) 3_445 . . . ? U1 O10 C9 O9 -0.6(10) 3_445 . . . ? U1 O10 C9 C8 179.7(8) 3_445 . . . ? O2 U1 O3 C1 85.7(6) . . . . ? O1 U1 O3 C1 -94.3(6) . . . . ? O6 U1 O3 C1 176.4(6) . . . . ? O9 U1 O3 C1 -6.8(7) 3 . . . ? O4 U1 O3 C1 -2.8(5) . . . . ? O7 U1 O3 C1 172.6(5) . . . . ? O10 U1 O3 C1 2.1(19) 3 . . . ? C9 U1 O3 C1 -5.3(8) 3 . . . ? O2 U1 O6 C4 -83.6(7) . . . . ? O1 U1 O6 C4 96.2(7) . . . . ? O9 U1 O6 C4 27(2) 3 . . . ? O4 U1 O6 C4 -173.6(6) . . . . ? O3 U1 O6 C4 -174.2(7) . . . . ? O7 U1 O6 C4 1.6(6) . . . . ? O10 U1 O6 C4 4.8(7) 3 . . . ? C9 U1 O6 C4 7.6(9) 3 . . . ? O2 U1 O4 C1 -88.7(6) . . . . ? O1 U1 O4 C1 91.4(6) . . . . ? O6 U1 O4 C1 2.1(7) . . . . ? O9 U1 O4 C1 179.1(7) 3 . . . ? O3 U1 O4 C1 2.9(5) . . . . ? O7 U1 O4 C1 -28(2) . . . . ? O10 U1 O4 C1 -176.3(6) 3 . . . ? C9 U1 O4 C1 -178.5(6) 3 . . . ? O2 U1 O7 C4 92.2(7) . . . . ? O1 U1 O7 C4 -88.0(7) . . . . ? O6 U1 O7 C4 -1.5(6) . . . . ? O9 U1 O7 C4 -177.6(6) 3 . . . ? O4 U1 O7 C4 31(2) . . . . ? O3 U1 O7 C4 3.0(7) . . . . ? O10 U1 O7 C4 -178.5(7) 3 . . . ? C9 U1 O7 C4 -178.2(6) 3 . . . ? C8 O8 C5 C6 1.3(11) . . . . ? C8 O8 C5 C4 179.8(8) . . . . ? U1 O6 C4 O7 -2.8(11) . . . . ? U1 O6 C4 C5 178.0(9) . . . . ? U1 O7 C4 O6 2.8(11) . . . . ? U1 O7 C4 C5 -178.0(9) . . . . ? C6 C5 C4 O6 177.1(12) . . . . ? O8 C5 C4 O6 -0.9(15) . . . . ? C6 C5 C4 O7 -2.1(19) . . . . ? O8 C5 C4 O7 179.9(9) . . . . ? U1 O4 C1 O3 -5.3(10) . . . . ? U1 O4 C1 C2 178.1(8) . . . . ? U1 O3 C1 O4 5.2(10) . . . . ? U1 O3 C1 C2 -178.2(8) . . . . ? C5 O8 C8 C7 -1.0(11) . . . . ? C5 O8 C8 C9 178.6(8) . . . . ? O9 C9 C8 C7 179.1(12) . . . . ? O10 C9 C8 C7 -1.1(19) . . . . ? U1 C9 C8 C7 162(44) 3_445 . . . ? O9 C9 C8 O8 -0.3(14) . . . . ? O10 C9 C8 O8 179.4(9) . . . . ? U1 C9 C8 O8 -18(45) 3_445 . . . ? O8 C5 C6 C7 -1.1(12) . . . . ? C4 C5 C6 C7 -179.1(11) . . . . ? C3 C3 C2 O5 -1.6(16) 2_655 . . . ? C3 C3 C2 C1 176.5(11) 2_655 . . . ? C2 O5 C2 C3 0.6(6) 2_655 . . . ? C2 O5 C2 C1 -177.7(11) 2_655 . . . ? O4 C1 C2 C3 14.5(17) . . . . ? O3 C1 C2 C3 -162.1(11) . . . . ? O4 C1 C2 O5 -167.5(8) . . . . ? O3 C1 C2 O5 15.8(14) . . . . ? O8 C8 C7 C6 0.4(12) . . . . ? C9 C8 C7 C6 -179.1(11) . . . . ? C5 C6 C7 C8 0.4(12) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.025 _refine_diff_density_min -1.600 _refine_diff_density_rms 0.189 #===END _database_code_depnum_ccdc_archive 'CCDC 922020' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H20 Ca O26 U2' _chemical_formula_sum 'C18 H20 Ca O26 U2' _chemical_formula_weight 1168.37 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' Ca Ca 0.2262 0.3064 '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' 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 'C c ' _symmetry_space_group_name_Hall 'C -2yc ' 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 8.4231(17) _cell_length_b 17.513(3) _cell_length_c 20.761(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.89(3) _cell_angle_gamma 90.00 _cell_volume 3007.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13297 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 27.81 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.550 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 11.032 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2053 _exptl_absorpt_correction_T_max 0.2163 _exptl_absorpt_process_details Higashi,1995 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku SCXmini diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12453 _diffrn_reflns_av_R_equivalents 0.0925 _diffrn_reflns_av_sigmaI/netI 0.1357 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.20 _reflns_number_total 5356 _reflns_number_gt 4260 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0127P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.046(13) _refine_ls_number_reflns 5356 _refine_ls_number_parameters 424 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.0860 _refine_ls_R_factor_gt 0.0636 _refine_ls_wR_factor_ref 0.1012 _refine_ls_wR_factor_gt 0.0939 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.000 _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 O8 O 0.4547(15) 0.4712(7) 0.3839(7) 0.035(4) Uani 1 1 d . . . O9 O 0.6076(18) 0.3731(8) 0.4245(8) 0.043(4) Uani 1 1 d . . . C6 C 0.596(2) 0.4453(11) 0.4084(10) 0.036(6) Uani 1 1 d . . . O19 O 0.0386(15) 0.4297(7) 0.1066(7) 0.036(4) Uani 1 1 d . . . O18 O -0.1159(18) 0.3278(7) 0.0743(8) 0.032(4) Uani 1 1 d . . . C18 C -0.100(2) 0.4018(11) 0.0859(10) 0.022(5) Uani 1 1 d U . . U1 U 0.81580(7) 0.84744(4) 0.38306(4) 0.02647(19) Uani 1 1 d . . . U2 U -0.32080(6) 0.80681(4) 0.11868(4) 0.0281(2) Uani 1 1 d . . . Ca4 Ca 0.0886(5) 0.6715(2) 0.1656(2) 0.0360(11) Uani 1 1 d . . . O1 O 0.7588(16) 0.8738(8) 0.4595(7) 0.037(4) Uani 1 1 d U . . O1W O 0.1115(16) 0.7387(7) 0.0657(7) 0.048(4) Uani 1 1 d . . . O2 O 0.8676(16) 0.8253(7) 0.3101(7) 0.032(4) Uani 1 1 d U . . O2W O 0.1479(17) 0.5800(7) 0.0859(7) 0.054(4) Uani 1 1 d . . . O3 O -0.3847(17) 0.7893(7) 0.1952(7) 0.036(4) Uani 1 1 d . . . O3W O 0.0307(18) 0.6774(7) 0.2760(7) 0.056(4) Uani 1 1 d . . . O4 O -0.2680(18) 0.8220(7) 0.0456(8) 0.043(4) Uani 1 1 d U . . O4W O 0.1637(17) 0.5478(7) 0.2169(7) 0.060(4) Uani 1 1 d . . . O5 O 0.9689(16) 0.7298(8) 0.4239(7) 0.038(4) Uani 1 1 d . . . O6 O 0.7076(16) 0.7190(7) 0.3931(7) 0.041(4) Uani 1 1 d . . . O6W O 0.3528(16) 0.6971(9) 0.2237(8) 0.068(5) Uani 1 1 d . . . O7 O 0.7051(14) 0.5708(6) 0.4072(6) 0.034(3) Uani 1 1 d . . . O10 O 0.6337(14) 0.9493(7) 0.3246(7) 0.037(4) Uani 1 1 d . . . O11 O 0.5247(19) 0.8365(8) 0.3313(8) 0.029(4) Uani 1 1 d . . . O12 O 0.2466(14) 0.8776(7) 0.2499(7) 0.038(4) Uani 1 1 d . . . O13 O -0.030(2) 0.8051(7) 0.1771(9) 0.035(5) Uani 1 1 d . . . O14 O -0.1576(15) 0.9151(7) 0.1692(7) 0.036(4) Uani 1 1 d . . . O15 O -0.1976(15) 0.6765(7) 0.1224(7) 0.035(4) Uani 1 1 d . . . O16 O -0.4582(14) 0.6872(8) 0.0782(7) 0.034(4) Uani 1 1 d . . . O17 O -0.2018(15) 0.5252(7) 0.0941(7) 0.033(4) Uani 1 1 d . . . C1 C 0.847(3) 0.6889(12) 0.4142(11) 0.042(6) Uani 1 1 d . . . C2 C 0.849(2) 0.6083(11) 0.4210(9) 0.019(4) Uani 1 1 d U . . C3 C 0.966(2) 0.5579(9) 0.4420(9) 0.027(5) Uani 1 1 d U . . H3 H 1.0751 0.5698 0.4562 0.033 Uiso 1 1 calc R . . C4 C 0.898(2) 0.4832(11) 0.4393(11) 0.041(6) Uani 1 1 d . . . H4 H 0.9525 0.4369 0.4478 0.049 Uiso 1 1 calc R . . C5 C 0.734(2) 0.4948(10) 0.4211(10) 0.024(5) Uani 1 1 d . . . C7 C 0.511(2) 0.9038(13) 0.3122(9) 0.031(5) Uani 1 1 d . . . C8 C 0.359(2) 0.9303(10) 0.2758(10) 0.028(5) Uani 1 1 d . . . C9 C 0.2971(19) 1.0012(10) 0.2631(8) 0.028(5) Uani 1 1 d . . . H9 H 0.3516 1.0472 0.2731 0.033 Uiso 1 1 calc R . . C10 C 0.135(2) 0.9923(10) 0.2318(9) 0.025(5) Uani 1 1 d . . . H10 H 0.0587 1.0310 0.2204 0.030 Uiso 1 1 calc R . . C11 C 0.111(2) 0.9175(10) 0.2217(10) 0.032(5) Uani 1 1 d . . . C12 C -0.034(3) 0.8775(12) 0.1879(11) 0.032(6) Uani 1 1 d . . . C13 C -0.331(2) 0.6476(9) 0.0939(10) 0.021(5) Uani 1 1 d . . . C14 C -0.347(2) 0.5637(10) 0.0816(10) 0.033(5) Uani 1 1 d . . . C15 C -0.465(2) 0.5168(12) 0.0591(11) 0.043(6) Uani 1 1 d . . . H15 H -0.5742 0.5299 0.0482 0.052 Uiso 1 1 calc R . . C16 C -0.401(2) 0.4426(10) 0.0539(9) 0.022(4) Uani 1 1 d U . . H16 H -0.4546 0.3986 0.0370 0.027 Uiso 1 1 calc R . . C17 C -0.241(2) 0.4512(9) 0.0795(9) 0.024(5) Uani 1 1 d U . . O5W O 0.335(3) 0.6310(9) 0.3526(10) 0.119(9) Uani 1 1 d . . . O7W O 0.3933(16) 0.7671(9) 0.4431(8) 0.066(5) 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 O8 0.031(8) 0.021(7) 0.048(10) 0.014(7) -0.001(7) -0.019(6) O9 0.029(9) 0.023(8) 0.071(13) 0.005(9) -0.003(8) 0.000(9) C6 0.025(11) 0.039(13) 0.040(14) -0.013(10) -0.007(10) 0.013(11) O19 0.023(8) 0.014(7) 0.066(12) -0.004(7) -0.002(7) 0.004(6) O18 0.035(8) 0.016(7) 0.045(10) -0.005(7) 0.008(7) 0.003(7) C18 0.017(7) 0.028(8) 0.025(8) -0.001(7) 0.012(7) 0.004(7) U1 0.0233(4) 0.0216(4) 0.0340(5) 0.0013(4) 0.0041(3) -0.0030(4) U2 0.0223(4) 0.0207(4) 0.0400(5) -0.0019(4) 0.0023(3) 0.0029(4) Ca4 0.033(2) 0.033(2) 0.042(3) 0.005(2) 0.007(2) 0.003(2) O1 0.042(7) 0.037(6) 0.033(7) -0.007(6) 0.012(6) 0.006(6) O1W 0.053(9) 0.033(8) 0.065(12) -0.006(7) 0.029(8) -0.005(7) O2 0.036(7) 0.027(6) 0.031(7) 0.023(6) -0.003(6) -0.013(6) O2W 0.066(10) 0.034(8) 0.056(11) -0.011(8) -0.001(9) 0.004(8) O3 0.047(9) 0.034(8) 0.028(9) 0.002(7) 0.010(7) -0.003(8) O3W 0.085(12) 0.047(9) 0.044(10) -0.008(8) 0.033(9) 0.008(9) O4 0.049(7) 0.031(6) 0.043(8) -0.018(6) -0.005(6) 0.019(6) O4W 0.093(11) 0.030(8) 0.063(11) -0.003(8) 0.030(9) 0.017(8) O5 0.029(8) 0.032(9) 0.051(11) 0.005(8) 0.001(7) 0.002(7) O6 0.039(9) 0.015(7) 0.068(12) -0.006(7) 0.006(8) -0.015(7) O6W 0.045(9) 0.075(12) 0.081(13) 0.006(10) 0.000(9) 0.003(9) O7 0.040(8) 0.015(7) 0.041(9) 0.008(6) -0.004(7) -0.006(7) O10 0.024(7) 0.033(8) 0.045(10) -0.002(7) -0.012(7) -0.002(7) O11 0.016(8) 0.029(8) 0.038(11) 0.008(7) -0.007(7) 0.004(7) O12 0.018(6) 0.031(9) 0.061(9) -0.003(6) -0.003(6) -0.001(6) O13 0.023(8) 0.030(9) 0.053(13) 0.002(7) 0.007(8) 0.009(7) O14 0.018(7) 0.022(8) 0.064(11) -0.001(7) 0.001(7) 0.008(6) O15 0.020(7) 0.034(8) 0.048(10) 0.005(7) 0.000(7) 0.003(7) O16 0.012(7) 0.025(8) 0.062(11) -0.013(8) -0.001(7) -0.001(7) O17 0.021(7) 0.017(7) 0.057(11) -0.005(7) -0.001(7) 0.007(6) C1 0.039(14) 0.051(16) 0.027(14) 0.019(11) -0.014(11) 0.017(13) C2 0.012(7) 0.024(8) 0.021(8) 0.004(7) 0.005(6) -0.007(7) C3 0.026(8) 0.017(8) 0.033(9) -0.002(7) -0.007(7) -0.007(7) C4 0.030(12) 0.024(12) 0.065(17) -0.010(11) -0.001(11) -0.001(10) C5 0.019(10) 0.017(10) 0.034(12) 0.007(9) 0.000(9) -0.012(9) C7 0.013(10) 0.055(16) 0.024(13) 0.003(11) 0.001(9) 0.009(11) C8 0.016(10) 0.026(11) 0.038(13) 0.004(9) -0.002(9) -0.012(9) C9 0.034(12) 0.028(11) 0.025(12) 0.018(9) 0.016(10) -0.001(10) C10 0.027(10) 0.022(10) 0.027(12) -0.002(9) 0.012(9) 0.013(9) C11 0.034(11) 0.022(11) 0.043(14) -0.017(10) 0.016(10) -0.003(10) C12 0.045(14) 0.024(12) 0.032(14) 0.010(10) 0.017(11) -0.002(11) C13 0.013(10) 0.011(10) 0.043(15) 0.001(8) 0.014(10) -0.004(9) C14 0.018(10) 0.011(10) 0.065(16) 0.012(10) -0.004(10) 0.000(9) C15 0.028(12) 0.043(14) 0.054(16) 0.012(12) -0.003(11) 0.009(11) C16 0.026(8) 0.014(7) 0.025(8) 0.000(6) -0.002(7) 0.007(7) C17 0.026(8) 0.014(7) 0.032(9) 0.000(7) 0.003(7) 0.006(7) O5W 0.17(2) 0.045(11) 0.106(19) -0.003(10) -0.064(17) 0.019(13) O7W 0.048(9) 0.088(13) 0.062(12) 0.025(10) 0.009(9) 0.015(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O8 C6 1.29(2) . ? O8 U1 2.461(11) 3_445 ? O9 C6 1.31(2) . ? O9 U1 2.487(15) 3_445 ? C6 C5 1.44(2) . ? C6 U1 2.88(2) 3_445 ? O19 C18 1.262(19) . ? O19 U2 2.446(12) 3_545 ? O18 C18 1.32(2) . ? O18 U2 2.509(15) 3_545 ? C18 C17 1.46(2) . ? C18 U2 2.854(17) 3_545 ? U1 O2 1.699(15) . ? U1 O1 1.804(14) . ? U1 O6 2.451(12) . ? U1 O8 2.461(11) 3 ? U1 O9 2.487(15) 3 ? U1 O11 2.492(16) . ? U1 O5 2.493(13) . ? U1 O10 2.511(12) . ? U1 C7 2.879(18) . ? U1 C6 2.88(2) 3 ? U2 O4 1.680(17) . ? U2 O3 1.797(14) . ? U2 O19 2.446(12) 3_455 ? U2 O14 2.458(12) . ? U2 O16 2.464(13) . ? U2 O15 2.502(12) . ? U2 O18 2.509(15) 3_455 ? U2 O13 2.521(17) . ? U2 C13 2.834(16) . ? U2 C12 2.85(2) . ? U2 C18 2.854(17) 3_455 ? U2 Ca4 4.146(4) . ? Ca4 O6W 2.364(15) . ? Ca4 O15 2.410(13) . ? Ca4 O2W 2.422(14) . ? Ca4 O1W 2.424(15) . ? Ca4 O3W 2.434(14) . ? Ca4 O4W 2.443(13) . ? Ca4 O13 2.572(13) . ? O5 C1 1.24(2) . ? O6 C1 1.28(2) . ? O7 C2 1.358(19) . ? O7 C5 1.373(18) . ? O10 C7 1.29(2) . ? O11 C7 1.24(2) . ? O12 C8 1.36(2) . ? O12 C11 1.37(2) . ? O13 C12 1.29(2) . ? O14 C12 1.23(2) . ? O15 C13 1.27(2) . ? O16 C13 1.27(2) . ? O17 C17 1.357(18) . ? O17 C14 1.377(19) . ? C1 C2 1.42(2) . ? C2 C3 1.34(2) . ? C3 C4 1.43(2) . ? C3 H3 0.9300 . ? C4 C5 1.38(2) . ? C4 H4 0.9300 . ? C7 C8 1.44(2) . ? C8 C9 1.35(2) . ? C9 C10 1.41(2) . ? C9 H9 0.9300 . ? C10 C11 1.34(2) . ? C10 H10 0.9300 . ? C11 C12 1.47(3) . ? C13 C14 1.49(2) . ? C14 C15 1.31(2) . ? C15 C16 1.42(2) . ? C15 H15 0.9300 . ? C16 C17 1.36(2) . ? C16 H16 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 C6 O8 U1 95.5(11) . 3_445 ? C6 O9 U1 93.8(11) . 3_445 ? O8 C6 O9 117.4(17) . . ? O8 C6 C5 121.2(18) . . ? O9 C6 C5 121.3(17) . . ? O8 C6 U1 58.1(9) . 3_445 ? O9 C6 U1 59.4(10) . 3_445 ? C5 C6 U1 179.3(14) . 3_445 ? C18 O19 U2 95.3(11) . 3_545 ? C18 O18 U2 91.0(10) . 3_545 ? O19 C18 O18 119.9(16) . . ? O19 C18 C17 119.1(16) . . ? O18 C18 C17 120.9(16) . . ? O19 C18 U2 58.6(9) . 3_545 ? O18 C18 U2 61.5(9) . 3_545 ? C17 C18 U2 171.6(14) . 3_545 ? O2 U1 O1 178.2(7) . . ? O2 U1 O6 91.6(5) . . ? O1 U1 O6 89.7(6) . . ? O2 U1 O8 90.4(5) . 3 ? O1 U1 O8 88.5(5) . 3 ? O6 U1 O8 172.5(5) . 3 ? O2 U1 O9 86.9(6) . 3 ? O1 U1 O9 93.4(6) . 3 ? O6 U1 O9 119.7(5) . 3 ? O8 U1 O9 53.2(4) 3 3 ? O2 U1 O11 89.7(6) . . ? O1 U1 O11 89.7(6) . . ? O6 U1 O11 67.3(4) . . ? O8 U1 O11 119.9(4) 3 . ? O9 U1 O11 172.3(6) 3 . ? O2 U1 O5 84.9(5) . . ? O1 U1 O5 96.9(6) . . ? O6 U1 O5 52.3(4) . . ? O8 U1 O5 120.7(5) 3 . ? O9 U1 O5 67.5(5) 3 . ? O11 U1 O5 119.1(4) . . ? O2 U1 O10 88.1(5) . . ? O1 U1 O10 90.2(5) . . ? O6 U1 O10 119.4(4) . . ? O8 U1 O10 67.9(4) 3 . ? O9 U1 O10 120.8(4) 3 . ? O11 U1 O10 52.0(4) . . ? O5 U1 O10 168.9(4) . . ? O2 U1 C7 88.7(6) . . ? O1 U1 C7 90.1(6) . . ? O6 U1 C7 92.8(6) . . ? O8 U1 C7 94.5(5) 3 . ? O9 U1 C7 147.3(6) 3 . ? O11 U1 C7 25.4(5) . . ? O5 U1 C7 144.2(5) . . ? O10 U1 C7 26.6(5) . . ? O2 U1 C6 87.7(6) . 3 ? O1 U1 C6 91.8(6) . 3 ? O6 U1 C6 146.6(5) . 3 ? O8 U1 C6 26.3(4) 3 3 ? O9 U1 C6 26.9(4) 3 3 ? O11 U1 C6 146.0(5) . 3 ? O5 U1 C6 94.4(5) . 3 ? O10 U1 C6 94.0(5) . 3 ? C7 U1 C6 120.6(6) . 3 ? O4 U2 O3 177.8(8) . . ? O4 U2 O19 88.5(6) . 3_455 ? O3 U2 O19 91.2(5) . 3_455 ? O4 U2 O14 92.4(6) . . ? O3 U2 O14 89.5(6) . . ? O19 U2 O14 65.5(4) 3_455 . ? O4 U2 O16 90.8(6) . . ? O3 U2 O16 87.5(5) . . ? O19 U2 O16 121.7(4) 3_455 . ? O14 U2 O16 172.2(4) . . ? O4 U2 O15 89.6(5) . . ? O3 U2 O15 90.5(5) . . ? O19 U2 O15 174.5(5) 3_455 . ? O14 U2 O15 119.7(4) . . ? O16 U2 O15 53.2(4) . . ? O4 U2 O18 93.4(6) . 3_455 ? O3 U2 O18 84.7(6) . 3_455 ? O19 U2 O18 53.6(4) 3_455 3_455 ? O14 U2 O18 118.6(4) . 3_455 ? O16 U2 O18 68.3(4) . 3_455 ? O15 U2 O18 121.4(4) . 3_455 ? O4 U2 O13 92.1(6) . . ? O3 U2 O13 89.9(6) . . ? O19 U2 O13 117.9(4) 3_455 . ? O14 U2 O13 52.4(4) . . ? O16 U2 O13 120.4(4) . . ? O15 U2 O13 67.3(4) . . ? O18 U2 O13 169.7(5) 3_455 . ? O4 U2 C13 89.8(6) . . ? O3 U2 C13 89.4(6) . . ? O19 U2 C13 148.1(5) 3_455 . ? O14 U2 C13 146.3(5) . . ? O16 U2 C13 26.5(5) . . ? O15 U2 C13 26.7(5) . . ? O18 U2 C13 94.8(5) 3_455 . ? O13 U2 C13 94.0(5) . . ? O4 U2 C12 92.5(7) . . ? O3 U2 C12 89.7(6) . . ? O19 U2 C12 91.0(5) 3_455 . ? O14 U2 C12 25.4(5) . . ? O16 U2 C12 147.2(5) . . ? O15 U2 C12 94.2(5) . . ? O18 U2 C12 143.9(5) 3_455 . ? O13 U2 C12 26.9(5) . . ? C13 U2 C12 120.9(6) . . ? O4 U2 C18 92.2(6) . 3_455 ? O3 U2 C18 86.5(6) . 3_455 ? O19 U2 C18 26.1(4) 3_455 3_455 ? O14 U2 C18 91.2(5) . 3_455 ? O16 U2 C18 95.8(5) . 3_455 ? O15 U2 C18 149.0(5) . 3_455 ? O18 U2 C18 27.5(4) 3_455 3_455 ? O13 U2 C18 143.5(5) . 3_455 ? C13 U2 C18 122.3(5) . 3_455 ? C12 U2 C18 116.6(6) . 3_455 ? O4 U2 Ca4 87.3(5) . . ? O3 U2 Ca4 94.0(5) . . ? O19 U2 Ca4 153.1(3) 3_455 . ? O14 U2 Ca4 88.1(3) . . ? O16 U2 Ca4 84.9(3) . . ? O15 U2 Ca4 31.8(3) . . ? O18 U2 Ca4 153.2(3) 3_455 . ? O13 U2 Ca4 35.9(3) . . ? C13 U2 Ca4 58.4(4) . . ? C12 U2 Ca4 62.7(4) . . ? C18 U2 Ca4 179.2(4) 3_455 . ? O6W Ca4 O15 164.1(5) . . ? O6W Ca4 O2W 100.3(5) . . ? O15 Ca4 O2W 95.2(5) . . ? O6W Ca4 O1W 97.2(5) . . ? O15 Ca4 O1W 84.2(5) . . ? O2W Ca4 O1W 71.1(5) . . ? O6W Ca4 O3W 81.3(6) . . ? O15 Ca4 O3W 89.1(5) . . ? O2W Ca4 O3W 140.9(5) . . ? O1W Ca4 O3W 147.9(5) . . ? O6W Ca4 O4W 78.8(5) . . ? O15 Ca4 O4W 110.7(5) . . ? O2W Ca4 O4W 69.0(5) . . ? O1W Ca4 O4W 138.4(5) . . ? O3W Ca4 O4W 73.1(4) . . ? O6W Ca4 O13 97.2(6) . . ? O15 Ca4 O13 67.8(5) . . ? O2W Ca4 O13 143.0(6) . . ? O1W Ca4 O13 74.5(5) . . ? O3W Ca4 O13 74.0(5) . . ? O4W Ca4 O13 147.0(5) . . ? O6W Ca4 U2 132.2(4) . . ? O15 Ca4 U2 33.1(3) . . ? O2W Ca4 U2 119.1(4) . . ? O1W Ca4 U2 73.6(3) . . ? O3W Ca4 U2 83.8(4) . . ? O4W Ca4 U2 138.1(4) . . ? O13 Ca4 U2 35.1(4) . . ? C1 O5 U1 93.5(12) . . ? C1 O6 U1 94.3(12) . . ? C2 O7 C5 107.9(13) . . ? C7 O10 U1 92.8(11) . . ? C7 O11 U1 95.0(12) . . ? C8 O12 C11 106.6(14) . . ? C12 O13 U2 90.8(13) . . ? C12 O13 Ca4 159.2(15) . . ? U2 O13 Ca4 109.0(6) . . ? C12 O14 U2 95.3(12) . . ? C13 O15 Ca4 153.2(12) . . ? C13 O15 U2 91.3(10) . . ? Ca4 O15 U2 115.1(5) . . ? C13 O16 U2 93.3(10) . . ? C17 O17 C14 104.9(13) . . ? O5 C1 O6 119.7(19) . . ? O5 C1 C2 124.5(18) . . ? O6 C1 C2 115.8(19) . . ? C3 C2 O7 109.0(16) . . ? C3 C2 C1 133.0(17) . . ? O7 C2 C1 117.9(16) . . ? C2 C3 C4 108.9(17) . . ? C2 C3 H3 125.6 . . ? C4 C3 H3 125.6 . . ? C5 C4 C3 104.5(17) . . ? C5 C4 H4 127.7 . . ? C3 C4 H4 127.7 . . ? O7 C5 C4 109.3(15) . . ? O7 C5 C6 116.1(16) . . ? C4 C5 C6 134.3(18) . . ? O11 C7 O10 120.2(17) . . ? O11 C7 C8 119.6(19) . . ? O10 C7 C8 120.3(19) . . ? O11 C7 U1 59.6(10) . . ? O10 C7 U1 60.6(9) . . ? C8 C7 U1 178.6(16) . . ? C9 C8 O12 109.4(16) . . ? C9 C8 C7 132.3(18) . . ? O12 C8 C7 118.3(17) . . ? C8 C9 C10 107.1(15) . . ? C8 C9 H9 126.4 . . ? C10 C9 H9 126.4 . . ? C11 C10 C9 106.6(16) . . ? C11 C10 H10 126.7 . . ? C9 C10 H10 126.7 . . ? C10 C11 O12 110.1(16) . . ? C10 C11 C12 129.1(19) . . ? O12 C11 C12 120.8(16) . . ? O14 C12 O13 121(2) . . ? O14 C12 C11 118.2(18) . . ? O13 C12 C11 120.2(19) . . ? O14 C12 U2 59.2(11) . . ? O13 C12 U2 62.3(11) . . ? C11 C12 U2 177.1(15) . . ? O16 C13 O15 122.2(15) . . ? O16 C13 C14 116.9(16) . . ? O15 C13 C14 120.8(16) . . ? O16 C13 U2 60.2(9) . . ? O15 C13 U2 62.0(9) . . ? C14 C13 U2 176.5(12) . . ? C15 C14 O17 110.5(16) . . ? C15 C14 C13 135.7(17) . . ? O17 C14 C13 113.8(15) . . ? C14 C15 C16 108.8(18) . . ? C14 C15 H15 125.6 . . ? C16 C15 H15 125.6 . . ? C17 C16 C15 103.6(16) . . ? C17 C16 H16 128.2 . . ? C15 C16 H16 128.2 . . ? C16 C17 O17 112.0(15) . . ? C16 C17 C18 134.5(17) . . ? O17 C17 C18 112.8(15) . . ? 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 U1 O8 C6 O9 -3.1(19) 3_445 . . . ? U1 O8 C6 C5 -179.7(17) 3_445 . . . ? U1 O9 C6 O8 3.1(19) 3_445 . . . ? U1 O9 C6 C5 179.6(17) 3_445 . . . ? U2 O19 C18 O18 -5.1(19) 3_545 . . . ? U2 O19 C18 C17 170.7(16) 3_545 . . . ? U2 O18 C18 O19 5.0(18) 3_545 . . . ? U2 O18 C18 C17 -170.7(17) 3_545 . . . ? O4 U2 Ca4 O6W 96.0(8) . . . . ? O3 U2 Ca4 O6W -85.7(7) . . . . ? O19 U2 Ca4 O6W 14.8(10) 3_455 . . . ? O14 U2 Ca4 O6W 3.6(7) . . . . ? O16 U2 Ca4 O6W -172.9(7) . . . . ? O15 U2 Ca4 O6W -170.3(9) . . . . ? O18 U2 Ca4 O6W -171.9(10) 3_455 . . . ? O13 U2 Ca4 O6W -1.4(8) . . . . ? C13 U2 Ca4 O6W -172.5(8) . . . . ? C12 U2 Ca4 O6W 1.8(7) . . . . ? C18 U2 Ca4 O6W 42(29) 3_455 . . . ? O4 U2 Ca4 O15 -93.7(8) . . . . ? O3 U2 Ca4 O15 84.5(8) . . . . ? O19 U2 Ca4 O15 -174.9(11) 3_455 . . . ? O14 U2 Ca4 O15 173.9(7) . . . . ? O16 U2 Ca4 O15 -2.6(7) . . . . ? O18 U2 Ca4 O15 -1.6(10) 3_455 . . . ? O13 U2 Ca4 O15 168.9(10) . . . . ? C13 U2 Ca4 O15 -2.3(8) . . . . ? C12 U2 Ca4 O15 172.1(8) . . . . ? C18 U2 Ca4 O15 -148(28) 3_455 . . . ? O4 U2 Ca4 O2W -45.4(6) . . . . ? O3 U2 Ca4 O2W 132.8(6) . . . . ? O19 U2 Ca4 O2W -126.6(9) 3_455 . . . ? O14 U2 Ca4 O2W -137.8(5) . . . . ? O16 U2 Ca4 O2W 45.7(5) . . . . ? O15 U2 Ca4 O2W 48.3(8) . . . . ? O18 U2 Ca4 O2W 46.7(9) 3_455 . . . ? O13 U2 Ca4 O2W -142.8(8) . . . . ? C13 U2 Ca4 O2W 46.0(6) . . . . ? C12 U2 Ca4 O2W -139.6(6) . . . . ? C18 U2 Ca4 O2W -99(28) 3_455 . . . ? O4 U2 Ca4 O1W 11.3(6) . . . . ? O3 U2 Ca4 O1W -170.5(6) . . . . ? O19 U2 Ca4 O1W -70.0(9) 3_455 . . . ? O14 U2 Ca4 O1W -81.2(5) . . . . ? O16 U2 Ca4 O1W 102.3(5) . . . . ? O15 U2 Ca4 O1W 104.9(7) . . . . ? O18 U2 Ca4 O1W 103.3(9) 3_455 . . . ? O13 U2 Ca4 O1W -86.2(8) . . . . ? C13 U2 Ca4 O1W 102.7(6) . . . . ? C12 U2 Ca4 O1W -82.9(6) . . . . ? C18 U2 Ca4 O1W -43(28) 3_455 . . . ? O4 U2 Ca4 O3W 168.3(6) . . . . ? O3 U2 Ca4 O3W -13.5(6) . . . . ? O19 U2 Ca4 O3W 87.1(8) 3_455 . . . ? O14 U2 Ca4 O3W 75.8(5) . . . . ? O16 U2 Ca4 O3W -100.6(5) . . . . ? O15 U2 Ca4 O3W -98.0(7) . . . . ? O18 U2 Ca4 O3W -99.7(9) 3_455 . . . ? O13 U2 Ca4 O3W 70.9(8) . . . . ? C13 U2 Ca4 O3W -100.3(6) . . . . ? C12 U2 Ca4 O3W 74.1(6) . . . . ? C18 U2 Ca4 O3W 114(28) 3_455 . . . ? O4 U2 Ca4 O4W -135.8(7) . . . . ? O3 U2 Ca4 O4W 42.4(7) . . . . ? O19 U2 Ca4 O4W 143.0(9) 3_455 . . . ? O14 U2 Ca4 O4W 131.8(6) . . . . ? O16 U2 Ca4 O4W -44.7(6) . . . . ? O15 U2 Ca4 O4W -42.1(8) . . . . ? O18 U2 Ca4 O4W -43.7(10) 3_455 . . . ? O13 U2 Ca4 O4W 126.8(9) . . . . ? C13 U2 Ca4 O4W -44.4(7) . . . . ? C12 U2 Ca4 O4W 130.0(7) . . . . ? C18 U2 Ca4 O4W 170(60) 3_455 . . . ? O4 U2 Ca4 O13 97.4(8) . . . . ? O3 U2 Ca4 O13 -84.3(8) . . . . ? O19 U2 Ca4 O13 16.2(10) 3_455 . . . ? O14 U2 Ca4 O13 5.0(7) . . . . ? O16 U2 Ca4 O13 -171.5(7) . . . . ? O15 U2 Ca4 O13 -168.9(10) . . . . ? O18 U2 Ca4 O13 -170.5(12) 3_455 . . . ? C13 U2 Ca4 O13 -171.2(8) . . . . ? C12 U2 Ca4 O13 3.2(8) . . . . ? C18 U2 Ca4 O13 43(29) 3_455 . . . ? O2 U1 O5 C1 -94.2(14) . . . . ? O1 U1 O5 C1 86.1(14) . . . . ? O6 U1 O5 C1 1.8(13) . . . . ? O8 U1 O5 C1 178.4(13) 3 . . . ? O9 U1 O5 C1 177.0(15) 3 . . . ? O11 U1 O5 C1 -7.4(16) . . . . ? O10 U1 O5 C1 -43(3) . . . . ? C7 U1 O5 C1 -13.7(18) . . . . ? C6 U1 O5 C1 178.5(14) 3 . . . ? O2 U1 O6 C1 80.5(14) . . . . ? O1 U1 O6 C1 -100.6(14) . . . . ? O8 U1 O6 C1 -25(5) 3 . . . ? O9 U1 O6 C1 -6.8(15) 3 . . . ? O11 U1 O6 C1 169.5(14) . . . . ? O5 U1 O6 C1 -1.7(13) . . . . ? O10 U1 O6 C1 169.3(12) . . . . ? C7 U1 O6 C1 169.3(14) . . . . ? C6 U1 O6 C1 -7.7(18) 3 . . . ? O2 U1 O10 C7 90.7(12) . . . . ? O1 U1 O10 C7 -89.9(12) . . . . ? O6 U1 O10 C7 -0.1(13) . . . . ? O8 U1 O10 C7 -178.1(12) 3 . . . ? O9 U1 O10 C7 176.0(11) 3 . . . ? O11 U1 O10 C7 -0.3(11) . . . . ? O5 U1 O10 C7 40(3) . . . . ? C6 U1 O10 C7 178.3(11) 3 . . . ? O2 U1 O11 C7 -87.5(13) . . . . ? O1 U1 O11 C7 90.8(13) . . . . ? O6 U1 O11 C7 -179.4(14) . . . . ? O8 U1 O11 C7 2.7(15) 3 . . . ? O9 U1 O11 C7 -23(5) 3 . . . ? O5 U1 O11 C7 -171.5(12) . . . . ? O10 U1 O11 C7 0.3(11) . . . . ? C6 U1 O11 C7 -2.1(19) 3 . . . ? O4 U2 O13 C12 91.3(13) . . . . ? O3 U2 O13 C12 -89.4(12) . . . . ? O19 U2 O13 C12 1.9(14) 3_455 . . . ? O14 U2 O13 C12 -0.1(11) . . . . ? O16 U2 O13 C12 -176.5(11) . . . . ? O15 U2 O13 C12 180.0(13) . . . . ? O18 U2 O13 C12 -31(4) 3_455 . . . ? C13 U2 O13 C12 -178.8(12) . . . . ? C18 U2 O13 C12 -5.4(17) 3_455 . . . ? Ca4 U2 O13 C12 173.6(16) . . . . ? O4 U2 O13 Ca4 -82.4(7) . . . . ? O3 U2 O13 Ca4 96.9(7) . . . . ? O19 U2 O13 Ca4 -171.8(5) 3_455 . . . ? O14 U2 O13 Ca4 -173.7(9) . . . . ? O16 U2 O13 Ca4 9.8(9) . . . . ? O15 U2 O13 Ca4 6.3(6) . . . . ? O18 U2 O13 Ca4 155(3) 3_455 . . . ? C13 U2 O13 Ca4 7.5(7) . . . . ? C12 U2 O13 Ca4 -173.6(16) . . . . ? C18 U2 O13 Ca4 -179.0(7) 3_455 . . . ? O6W Ca4 O13 C12 17(4) . . . . ? O15 Ca4 O13 C12 -168(4) . . . . ? O2W Ca4 O13 C12 -101(4) . . . . ? O1W Ca4 O13 C12 -78(4) . . . . ? O3W Ca4 O13 C12 96(4) . . . . ? O4W Ca4 O13 C12 98(4) . . . . ? U2 Ca4 O13 C12 -162(5) . . . . ? O6W Ca4 O13 U2 179.0(6) . . . . ? O15 Ca4 O13 U2 -6.5(6) . . . . ? O2W Ca4 O13 U2 61.3(11) . . . . ? O1W Ca4 O13 U2 83.5(7) . . . . ? O3W Ca4 O13 U2 -102.3(7) . . . . ? O4W Ca4 O13 U2 -100.7(10) . . . . ? O4 U2 O14 C12 -90.8(13) . . . . ? O3 U2 O14 C12 90.4(13) . . . . ? O19 U2 O14 C12 -178.1(13) 3_455 . . . ? O16 U2 O14 C12 23(4) . . . . ? O15 U2 O14 C12 0.1(14) . . . . ? O18 U2 O14 C12 174.1(12) 3_455 . . . ? O13 U2 O14 C12 0.1(12) . . . . ? C13 U2 O14 C12 2.3(17) . . . . ? C18 U2 O14 C12 176.9(12) 3_455 . . . ? Ca4 U2 O14 C12 -3.6(12) . . . . ? O6W Ca4 O15 C13 -162(3) . . . . ? O2W Ca4 O15 C13 31(3) . . . . ? O1W Ca4 O15 C13 102(3) . . . . ? O3W Ca4 O15 C13 -110(3) . . . . ? O4W Ca4 O15 C13 -38(3) . . . . ? O13 Ca4 O15 C13 177(3) . . . . ? U2 Ca4 O15 C13 170(3) . . . . ? O6W Ca4 O15 U2 27(2) . . . . ? O2W Ca4 O15 U2 -139.1(6) . . . . ? O1W Ca4 O15 U2 -68.7(6) . . . . ? O3W Ca4 O15 U2 79.9(6) . . . . ? O4W Ca4 O15 U2 151.4(6) . . . . ? O13 Ca4 O15 U2 6.9(6) . . . . ? O4 U2 O15 C13 -90.3(12) . . . . ? O3 U2 O15 C13 87.6(12) . . . . ? O19 U2 O15 C13 -21(6) 3_455 . . . ? O14 U2 O15 C13 177.3(11) . . . . ? O16 U2 O15 C13 1.1(11) . . . . ? O18 U2 O15 C13 3.4(14) 3_455 . . . ? O13 U2 O15 C13 177.3(12) . . . . ? C12 U2 O15 C13 177.3(12) . . . . ? C18 U2 O15 C13 3.4(17) 3_455 . . . ? Ca4 U2 O15 C13 -175.7(15) . . . . ? O4 U2 O15 Ca4 85.4(7) . . . . ? O3 U2 O15 Ca4 -96.8(7) . . . . ? O19 U2 O15 Ca4 155(5) 3_455 . . . ? O14 U2 O15 Ca4 -7.1(8) . . . . ? O16 U2 O15 Ca4 176.7(9) . . . . ? O18 U2 O15 Ca4 179.1(5) 3_455 . . . ? O13 U2 O15 Ca4 -7.0(6) . . . . ? C13 U2 O15 Ca4 175.7(15) . . . . ? C12 U2 O15 Ca4 -7.0(7) . . . . ? C18 U2 O15 Ca4 179.1(8) 3_455 . . . ? O4 U2 O16 C13 87.8(13) . . . . ? O3 U2 O16 C13 -93.6(12) . . . . ? O19 U2 O16 C13 176.6(11) 3_455 . . . ? O14 U2 O16 C13 -26(4) . . . . ? O15 U2 O16 C13 -1.1(11) . . . . ? O18 U2 O16 C13 -178.9(13) 3_455 . . . ? O13 U2 O16 C13 -5.1(14) . . . . ? C12 U2 O16 C13 -8.0(17) . . . . ? C18 U2 O16 C13 -179.8(12) 3_455 . . . ? Ca4 U2 O16 C13 0.7(11) . . . . ? U1 O5 C1 O6 -3(2) . . . . ? U1 O5 C1 C2 173.0(19) . . . . ? U1 O6 C1 O5 3(2) . . . . ? U1 O6 C1 C2 -173.3(16) . . . . ? C5 O7 C2 C3 1(2) . . . . ? C5 O7 C2 C1 -176.2(17) . . . . ? O5 C1 C2 C3 5(4) . . . . ? O6 C1 C2 C3 -179(2) . . . . ? O5 C1 C2 O7 -178(2) . . . . ? O6 C1 C2 O7 -2(3) . . . . ? O7 C2 C3 C4 3(2) . . . . ? C1 C2 C3 C4 179(2) . . . . ? C2 C3 C4 C5 -5(2) . . . . ? C2 O7 C5 C4 -4(2) . . . . ? C2 O7 C5 C6 -179.0(17) . . . . ? C3 C4 C5 O7 6(2) . . . . ? C3 C4 C5 C6 179(2) . . . . ? O8 C6 C5 O7 2(3) . . . . ? O9 C6 C5 O7 -174.7(17) . . . . ? U1 C6 C5 O7 -21(100) 3_445 . . . ? O8 C6 C5 C4 -171(2) . . . . ? O9 C6 C5 C4 12(4) . . . . ? U1 C6 C5 C4 166(100) 3_445 . . . ? U1 O11 C7 O10 -1(2) . . . . ? U1 O11 C7 C8 178.8(16) . . . . ? U1 O10 C7 O11 1(2) . . . . ? U1 O10 C7 C8 -178.8(16) . . . . ? O2 U1 C7 O11 92.1(13) . . . . ? O1 U1 C7 O11 -89.2(13) . . . . ? O6 U1 C7 O11 0.6(13) . . . . ? O8 U1 C7 O11 -177.6(13) 3 . . . ? O9 U1 C7 O11 174.3(14) 3 . . . ? O5 U1 C7 O11 12.8(17) . . . . ? O10 U1 C7 O11 -179(2) . . . . ? C6 U1 C7 O11 178.6(12) 3 . . . ? O2 U1 C7 O10 -88.5(11) . . . . ? O1 U1 C7 O10 90.2(11) . . . . ? O6 U1 C7 O10 180.0(11) . . . . ? O8 U1 C7 O10 1.8(11) 3 . . . ? O9 U1 C7 O10 -6.3(17) 3 . . . ? O11 U1 C7 O10 179(2) . . . . ? O5 U1 C7 O10 -167.9(10) . . . . ? C6 U1 C7 O10 -2.0(13) 3 . . . ? O2 U1 C7 C8 40(66) . . . . ? O1 U1 C7 C8 -141(66) . . . . ? O6 U1 C7 C8 -51(66) . . . . ? O8 U1 C7 C8 131(66) 3 . . . ? O9 U1 C7 C8 123(65) 3 . . . ? O11 U1 C7 C8 -52(65) . . . . ? O5 U1 C7 C8 -39(66) . . . . ? O10 U1 C7 C8 129(66) . . . . ? C6 U1 C7 C8 127(66) 3 . . . ? C11 O12 C8 C9 -1(2) . . . . ? C11 O12 C8 C7 176.2(16) . . . . ? O11 C7 C8 C9 161(2) . . . . ? O10 C7 C8 C9 -19(3) . . . . ? U1 C7 C8 C9 -148(64) . . . . ? O11 C7 C8 O12 -15(3) . . . . ? O10 C7 C8 O12 164.0(17) . . . . ? U1 C7 C8 O12 36(66) . . . . ? O12 C8 C9 C10 4(2) . . . . ? C7 C8 C9 C10 -172.7(18) . . . . ? C8 C9 C10 C11 -6(2) . . . . ? C9 C10 C11 O12 5(2) . . . . ? C9 C10 C11 C12 -176.5(19) . . . . ? C8 O12 C11 C10 -2(2) . . . . ? C8 O12 C11 C12 178.9(16) . . . . ? U2 O14 C12 O13 0(2) . . . . ? U2 O14 C12 C11 178.3(16) . . . . ? U2 O13 C12 O14 0(2) . . . . ? Ca4 O13 C12 O14 163(3) . . . . ? U2 O13 C12 C11 -178.3(17) . . . . ? Ca4 O13 C12 C11 -15(5) . . . . ? Ca4 O13 C12 U2 163(4) . . . . ? C10 C11 C12 O14 -5(3) . . . . ? O12 C11 C12 O14 173.0(18) . . . . ? C10 C11 C12 O13 173.0(19) . . . . ? O12 C11 C12 O13 -9(3) . . . . ? C10 C11 C12 U2 25(30) . . . . ? O12 C11 C12 U2 -157(28) . . . . ? O4 U2 C12 O14 90.3(12) . . . . ? O3 U2 C12 O14 -89.4(13) . . . . ? O19 U2 C12 O14 1.7(12) 3_455 . . . ? O16 U2 C12 O14 -174.4(11) . . . . ? O15 U2 C12 O14 -179.9(12) . . . . ? O18 U2 C12 O14 -8.9(18) 3_455 . . . ? O13 U2 C12 O14 -180(2) . . . . ? C13 U2 C12 O14 -178.5(11) . . . . ? C18 U2 C12 O14 -3.5(14) 3_455 . . . ? Ca4 U2 C12 O14 175.9(14) . . . . ? O4 U2 C12 O13 -89.8(12) . . . . ? O3 U2 C12 O13 90.5(12) . . . . ? O19 U2 C12 O13 -178.4(12) 3_455 . . . ? O14 U2 C12 O13 180(2) . . . . ? O16 U2 C12 O13 5.5(18) . . . . ? O15 U2 C12 O13 0.0(12) . . . . ? O18 U2 C12 O13 171.0(12) 3_455 . . . ? C13 U2 C12 O13 1.4(14) . . . . ? C18 U2 C12 O13 176.4(11) 3_455 . . . ? Ca4 U2 C12 O13 -4.2(10) . . . . ? O4 U2 C12 C11 59(29) . . . . ? O3 U2 C12 C11 -120(29) . . . . ? O19 U2 C12 C11 -29(29) 3_455 . . . ? O14 U2 C12 C11 -31(28) . . . . ? O16 U2 C12 C11 155(28) . . . . ? O15 U2 C12 C11 149(29) . . . . ? O18 U2 C12 C11 -40(29) 3_455 . . . ? O13 U2 C12 C11 149(29) . . . . ? C13 U2 C12 C11 151(29) . . . . ? C18 U2 C12 C11 -34(29) 3_455 . . . ? Ca4 U2 C12 C11 145(29) . . . . ? U2 O16 C13 O15 2(2) . . . . ? U2 O16 C13 C14 177.8(15) . . . . ? Ca4 O15 C13 O16 -173.3(18) . . . . ? U2 O15 C13 O16 -2(2) . . . . ? Ca4 O15 C13 C14 11(4) . . . . ? U2 O15 C13 C14 -177.6(16) . . . . ? Ca4 O15 C13 U2 -171(3) . . . . ? O4 U2 C13 O16 -92.3(12) . . . . ? O3 U2 C13 O16 85.7(12) . . . . ? O19 U2 C13 O16 -5.5(18) 3_455 . . . ? O14 U2 C13 O16 173.8(10) . . . . ? O15 U2 C13 O16 178(2) . . . . ? O18 U2 C13 O16 1.1(12) 3_455 . . . ? O13 U2 C13 O16 175.6(12) . . . . ? C12 U2 C13 O16 174.9(11) . . . . ? C18 U2 C13 O16 0.2(14) 3_455 . . . ? Ca4 U2 C13 O16 -179.2(13) . . . . ? O4 U2 C13 O15 89.6(12) . . . . ? O3 U2 C13 O15 -92.4(12) . . . . ? O19 U2 C13 O15 176.4(11) 3_455 . . . ? O14 U2 C13 O15 -4.3(17) . . . . ? O16 U2 C13 O15 -178(2) . . . . ? O18 U2 C13 O15 -177.1(12) 3_455 . . . ? O13 U2 C13 O15 -2.5(11) . . . . ? C12 U2 C13 O15 -3.2(14) . . . . ? C18 U2 C13 O15 -177.9(10) 3_455 . . . ? Ca4 U2 C13 O15 2.7(9) . . . . ? O4 U2 C13 C14 -127(24) . . . . ? O3 U2 C13 C14 51(24) . . . . ? O19 U2 C13 C14 -40(25) 3_455 . . . ? O14 U2 C13 C14 139(24) . . . . ? O16 U2 C13 C14 -34(23) . . . . ? O15 U2 C13 C14 144(25) . . . . ? O18 U2 C13 C14 -33(24) 3_455 . . . ? O13 U2 C13 C14 141(24) . . . . ? C12 U2 C13 C14 141(24) . . . . ? C18 U2 C13 C14 -34(24) 3_455 . . . ? Ca4 U2 C13 C14 146(24) . . . . ? C17 O17 C14 C15 -2(2) . . . . ? C17 O17 C14 C13 -179.3(16) . . . . ? O16 C13 C14 C15 -2(4) . . . . ? O15 C13 C14 C15 174(2) . . . . ? U2 C13 C14 C15 31(26) . . . . ? O16 C13 C14 O17 174.3(17) . . . . ? O15 C13 C14 O17 -10(3) . . . . ? U2 C13 C14 O17 -152(23) . . . . ? O17 C14 C15 C16 -1(3) . . . . ? C13 C14 C15 C16 175(2) . . . . ? C14 C15 C16 C17 4(2) . . . . ? C15 C16 C17 O17 -6(2) . . . . ? C15 C16 C17 C18 -175(2) . . . . ? C14 O17 C17 C16 5(2) . . . . ? C14 O17 C17 C18 176.5(16) . . . . ? O19 C18 C17 C16 173(2) . . . . ? O18 C18 C17 C16 -12(3) . . . . ? U2 C18 C17 C16 -116(8) 3_545 . . . ? O19 C18 C17 O17 3(3) . . . . ? O18 C18 C17 O17 179.2(17) . . . . ? U2 C18 C17 O17 75(9) 3_545 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.157 _refine_diff_density_min -1.195 _refine_diff_density_rms 0.221 #===END _database_code_depnum_ccdc_archive 'CCDC 917421' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1a #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H12 Na2 O25 U2' _chemical_formula_sum 'C18 H12 Na2 O25 U2' _chemical_formula_weight 1150.27 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' 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' Na Na 0.0362 0.0249 '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 ' _symmetry_space_group_name_Hall 'C 2c 2 ' 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 7.9714(16) _cell_length_b 17.775(4) _cell_length_c 21.312(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3019.7(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 14980 _cell_measurement_theta_min 3.39 _cell_measurement_theta_max 27.60 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 10.843 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1578 _exptl_absorpt_correction_T_max 0.1724 _exptl_absorpt_process_details Higashi,1995 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku SCXmini diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13235 _diffrn_reflns_av_R_equivalents 0.0792 _diffrn_reflns_av_sigmaI/netI 0.0620 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2660 _reflns_number_gt 2433 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0454P)^2^+5.7353P] 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 0.010(17) _refine_ls_number_reflns 2660 _refine_ls_number_parameters 214 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.0942 _refine_ls_wR_factor_gt 0.0917 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.084 _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 O6 O 0.3291(12) 0.1930(4) 0.3891(6) 0.043(3) Uani 1 1 d . . . O5 O 0.1890(11) 0.1001(5) 0.4300(4) 0.033(2) Uani 1 1 d . . . C6 C 0.2013(17) 0.1705(7) 0.4137(7) 0.033(3) Uani 1 1 d . . . U1 U -0.03065(6) 0.57160(2) 0.38192(2) 0.02532(15) Uani 1 1 d . . . O4 O 0.0767(10) 0.4431(4) 0.3833(5) 0.039(2) Uani 1 1 d . . . O8 O 0.2465(11) 0.5606(6) 0.3283(4) 0.041(2) Uani 1 1 d . . . O3 O -0.1718(12) 0.4556(5) 0.4255(5) 0.035(2) Uani 1 1 d . . . O7 O 0.1271(13) 0.6722(5) 0.3310(5) 0.044(3) Uani 1 1 d . . . C5 C 0.0581(17) 0.2220(6) 0.4254(6) 0.028(3) Uani 1 1 d . . . C8 C 0.3831(19) 0.6635(8) 0.2777(6) 0.037(4) Uani 1 1 d . . . O9 O 0.0907(11) 0.2951(4) 0.4102(4) 0.030(2) Uani 1 1 d . . . O10 O 0.5000 0.6161(7) 0.2500 0.029(3) Uani 1 2 d S . . O2 O -0.1323(12) 0.5544(5) 0.3107(4) 0.039(3) Uani 1 1 d . . . O1 O 0.0719(11) 0.5896(5) 0.4540(4) 0.038(2) Uani 1 1 d . . . C2 C -0.0570(16) 0.3329(7) 0.4222(5) 0.027(3) Uani 1 1 d . . . C1 C -0.0490(19) 0.4135(7) 0.4110(6) 0.032(3) Uani 1 1 d . . . C4 C -0.1009(17) 0.2127(7) 0.4447(6) 0.030(3) Uani 1 1 d . . . H4 H -0.1527 0.1682 0.4570 0.036 Uiso 1 1 calc R . . C3 C -0.1740(17) 0.2874(7) 0.4423(6) 0.029(3) Uani 1 1 d . . . H3 H -0.2833 0.3004 0.4531 0.035 Uiso 1 1 calc R . . C7 C 0.2472(19) 0.6298(9) 0.3129(6) 0.038(4) Uani 1 1 d . . . Na2 Na 0.1101(11) 0.0000 0.5000 0.045(2) Uani 1 2 d S . . Na1 Na 0.5000 0.3859(5) 0.2500 0.099(4) Uani 1 2 d SD . . O1W O -0.0836(17) 0.0592(8) 0.5614(8) 0.104(5) Uani 1 1 d . . . O2W O 0.557(3) 0.3233(9) 0.1678(7) 0.153(8) Uani 1 1 d D . . C9 C 0.426(2) 0.7351(8) 0.2669(7) 0.050(4) Uani 1 1 d . . . H9 H 0.3674 0.7775 0.2800 0.060 Uiso 1 1 calc R . . O3W O 0.737(3) 0.4281(14) 0.271(2) 0.57(5) Uani 1 1 d 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 O6 0.036(6) 0.019(5) 0.073(7) 0.019(5) 0.037(6) 0.008(4) O5 0.029(5) 0.017(5) 0.052(6) 0.003(4) 0.011(4) 0.001(4) C6 0.028(9) 0.031(8) 0.040(8) -0.007(7) 0.008(6) -0.001(6) U1 0.0235(2) 0.0196(2) 0.0329(2) 0.0011(2) 0.0055(2) 0.0039(2) O4 0.027(5) 0.025(5) 0.065(6) 0.007(6) 0.003(5) 0.005(4) O8 0.031(5) 0.046(7) 0.045(6) 0.011(5) 0.011(4) 0.012(5) O3 0.033(6) 0.017(5) 0.054(6) -0.002(4) 0.013(5) 0.014(4) O7 0.035(6) 0.037(6) 0.060(7) 0.000(5) 0.016(5) -0.003(5) C5 0.035(9) 0.016(6) 0.032(7) -0.004(5) -0.001(6) 0.010(6) C8 0.040(9) 0.053(10) 0.019(7) -0.007(7) 0.007(6) 0.013(8) O9 0.034(5) 0.018(4) 0.037(5) 0.005(4) 0.011(4) 0.008(4) O10 0.020(8) 0.043(7) 0.025(6) 0.000 0.002(5) 0.000 O2 0.038(6) 0.037(6) 0.042(6) 0.007(5) -0.001(5) 0.001(5) O1 0.029(6) 0.047(6) 0.038(5) -0.006(4) 0.007(4) 0.001(4) C2 0.027(8) 0.028(7) 0.026(7) 0.002(6) -0.002(6) 0.018(6) C1 0.046(9) 0.020(7) 0.030(7) -0.007(5) 0.003(7) 0.002(7) C4 0.031(8) 0.016(6) 0.042(8) -0.003(6) 0.004(6) 0.003(6) C3 0.029(8) 0.027(7) 0.032(8) 0.011(7) 0.007(6) -0.004(6) C7 0.039(9) 0.051(10) 0.025(8) -0.009(7) 0.001(7) 0.005(7) Na2 0.038(5) 0.042(5) 0.055(5) 0.011(4) 0.000 0.000 Na1 0.130(12) 0.056(6) 0.111(9) 0.000 -0.020(9) 0.000 O1W 0.064(9) 0.101(11) 0.148(13) 0.005(10) 0.056(9) -0.001(9) O2W 0.141(18) 0.104(12) 0.21(2) -0.083(13) 0.046(16) 0.009(13) C9 0.063(13) 0.040(8) 0.047(10) -0.010(7) 0.015(8) 0.004(8) O3W 1.02(12) 0.21(3) 0.46(7) 0.24(4) -0.38(8) -0.36(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 O6 C6 1.214(16) . ? O6 U1 2.436(8) 5_545 ? O5 C6 1.303(14) . ? O5 Na2 2.406(9) . ? O5 U1 2.510(9) 5_545 ? C6 C5 1.483(17) . ? C6 U1 2.849(13) 5_545 ? U1 O2 1.748(10) . ? U1 O1 1.769(9) . ? U1 O6 2.436(8) 5_455 ? U1 O4 2.440(7) . ? U1 O7 2.441(9) . ? U1 O8 2.495(9) . ? U1 O5 2.510(9) 5_455 ? U1 O3 2.525(9) . ? U1 C6 2.849(13) 5_455 ? U1 Na2 4.019(6) 5_455 ? O4 C1 1.276(16) . ? O8 C7 1.273(18) . ? O3 C1 1.271(15) . ? O3 Na2 2.483(11) 5_455 ? O7 C7 1.278(17) . ? C5 C4 1.343(18) . ? C5 O9 1.365(14) . ? C8 C9 1.340(19) . ? C8 O10 1.387(14) . ? C8 C7 1.45(2) . ? O9 C2 1.379(14) . ? O10 C8 1.387(14) 3_655 ? C2 C3 1.308(17) . ? C2 C1 1.453(16) . ? C4 C3 1.451(17) . ? Na2 O1W 2.281(14) 4_556 ? Na2 O1W 2.281(14) . ? Na2 O5 2.406(9) 4_556 ? Na2 O3 2.483(11) 8_556 ? Na2 O3 2.483(11) 5_545 ? Na2 U1 4.019(6) 5_545 ? Na2 U1 4.019(6) 8_556 ? Na1 O3W 2.080(10) 3_655 ? Na1 O3W 2.080(10) . ? Na1 O2W 2.123(9) . ? Na1 O2W 2.123(9) 3_655 ? C9 C9 1.38(3) 3_655 ? 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 C6 O6 U1 96.9(8) . 5_545 ? C6 O5 Na2 153.6(9) . . ? C6 O5 U1 91.0(7) . 5_545 ? Na2 O5 U1 109.7(4) . 5_545 ? O6 C6 O5 119.7(12) . . ? O6 C6 C5 121.0(12) . . ? O5 C6 C5 119.3(12) . . ? O6 C6 U1 58.1(7) . 5_545 ? O5 C6 U1 61.8(6) . 5_545 ? C5 C6 U1 175.8(10) . 5_545 ? O2 U1 O1 179.7(4) . . ? O2 U1 O6 89.8(4) . 5_455 ? O1 U1 O6 89.9(4) . 5_455 ? O2 U1 O4 90.5(4) . . ? O1 U1 O4 89.8(4) . . ? O6 U1 O4 171.9(3) 5_455 . ? O2 U1 O7 88.9(4) . . ? O1 U1 O7 90.9(4) . . ? O6 U1 O7 67.4(3) 5_455 . ? O4 U1 O7 120.7(3) . . ? O2 U1 O8 89.9(4) . . ? O1 U1 O8 90.1(4) . . ? O6 U1 O8 120.3(3) 5_455 . ? O4 U1 O8 67.8(3) . . ? O7 U1 O8 52.9(3) . . ? O2 U1 O5 88.7(4) . 5_455 ? O1 U1 O5 91.2(3) . 5_455 ? O6 U1 O5 52.2(3) 5_455 5_455 ? O4 U1 O5 119.8(3) . 5_455 ? O7 U1 O5 119.5(3) . 5_455 ? O8 U1 O5 172.4(3) . 5_455 ? O2 U1 O3 88.3(4) . . ? O1 U1 O3 92.0(4) . . ? O6 U1 O3 119.7(3) 5_455 . ? O4 U1 O3 52.2(3) . . ? O7 U1 O3 172.3(3) . . ? O8 U1 O3 119.9(3) . . ? O5 U1 O3 67.5(3) 5_455 . ? O2 U1 C6 88.1(4) . 5_455 ? O1 U1 C6 91.6(4) . 5_455 ? O6 U1 C6 25.0(3) 5_455 5_455 ? O4 U1 C6 146.9(3) . 5_455 ? O7 U1 C6 92.3(4) . 5_455 ? O8 U1 C6 145.2(4) . 5_455 ? O5 U1 C6 27.2(3) 5_455 5_455 ? O3 U1 C6 94.7(3) . 5_455 ? O2 U1 Na2 99.1(3) . 5_455 ? O1 U1 Na2 81.0(3) . 5_455 ? O6 U1 Na2 85.1(2) 5_455 5_455 ? O4 U1 Na2 86.9(2) . 5_455 ? O7 U1 Na2 151.4(2) . 5_455 ? O8 U1 Na2 153.2(2) . 5_455 ? O5 U1 Na2 34.3(2) 5_455 5_455 ? O3 U1 Na2 36.28(19) . 5_455 ? C6 U1 Na2 60.8(3) 5_455 5_455 ? C1 O4 U1 96.7(7) . . ? C7 O8 U1 92.7(8) . . ? C1 O3 Na2 151.9(9) . 5_455 ? C1 O3 U1 92.8(8) . . ? Na2 O3 U1 106.7(3) 5_455 . ? C7 O7 U1 95.0(9) . . ? C4 C5 O9 111.7(11) . . ? C4 C5 C6 134.6(12) . . ? O9 C5 C6 113.7(11) . . ? C9 C8 O10 109.3(13) . . ? C9 C8 C7 132.4(14) . . ? O10 C8 C7 118.2(12) . . ? C5 O9 C2 105.0(9) . . ? C8 O10 C8 105.4(14) 3_655 . ? C3 C2 O9 111.6(10) . . ? C3 C2 C1 134.0(13) . . ? O9 C2 C1 114.4(11) . . ? O3 C1 O4 118.3(11) . . ? O3 C1 C2 120.5(13) . . ? O4 C1 C2 121.1(12) . . ? C5 C4 C3 104.8(12) . . ? C2 C3 C4 106.9(12) . . ? O8 C7 O7 119.3(13) . . ? O8 C7 C8 122.5(13) . . ? O7 C7 C8 118.2(14) . . ? O1W Na2 O1W 94.8(9) 4_556 . ? O1W Na2 O5 99.3(5) 4_556 . ? O1W Na2 O5 101.1(4) . . ? O1W Na2 O5 101.1(4) 4_556 4_556 ? O1W Na2 O5 99.3(5) . 4_556 ? O5 Na2 O5 149.7(6) . 4_556 ? O1W Na2 O3 170.9(4) 4_556 8_556 ? O1W Na2 O3 87.7(5) . 8_556 ? O5 Na2 O3 88.8(4) . 8_556 ? O5 Na2 O3 69.8(3) 4_556 8_556 ? O1W Na2 O3 87.7(5) 4_556 5_545 ? O1W Na2 O3 170.9(4) . 5_545 ? O5 Na2 O3 69.8(3) . 5_545 ? O5 Na2 O3 88.8(4) 4_556 5_545 ? O3 Na2 O3 91.1(6) 8_556 5_545 ? O1W Na2 U1 105.6(4) 4_556 5_545 ? O1W Na2 U1 134.1(4) . 5_545 ? O5 Na2 U1 36.0(2) . 5_545 ? O5 Na2 U1 115.9(3) 4_556 5_545 ? O3 Na2 U1 78.5(3) 8_556 5_545 ? O3 Na2 U1 37.0(2) 5_545 5_545 ? O1W Na2 U1 134.1(4) 4_556 8_556 ? O1W Na2 U1 105.6(4) . 8_556 ? O5 Na2 U1 115.9(3) . 8_556 ? O5 Na2 U1 36.0(2) 4_556 8_556 ? O3 Na2 U1 37.0(2) 8_556 8_556 ? O3 Na2 U1 78.5(3) 5_545 8_556 ? U1 Na2 U1 89.12(18) 5_545 8_556 ? O3W Na1 O3W 137.7(16) 3_655 . ? O3W Na1 O2W 101.9(12) 3_655 . ? O3W Na1 O2W 99.8(15) . . ? O3W Na1 O2W 99.8(15) 3_655 3_655 ? O3W Na1 O2W 101.9(12) . 3_655 ? O2W Na1 O2W 116.8(11) . 3_655 ? C8 C9 C9 108.0(9) . 3_655 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.981 _refine_diff_density_min -1.090 _refine_diff_density_rms 0.186 _database_code_depnum_ccdc_archive 'CCDC 917419' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1b #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H12 Na2 O25 U2' _chemical_formula_sum 'C18 H12 Na2 O25 U2' _chemical_formula_weight 1150.27 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' 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' Na Na 0.0362 0.0249 '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 ' _symmetry_space_group_name_Hall 'C 2c 2 ' 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 7.9674(16) _cell_length_b 17.755(4) _cell_length_c 21.296(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3012.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15418 _cell_measurement_theta_min 3.39 _cell_measurement_theta_max 27.56 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 10.869 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1574 _exptl_absorpt_correction_T_max 0.1720 _exptl_absorpt_process_details Higashi,1995 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku SCXmini diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13174 _diffrn_reflns_av_R_equivalents 0.0570 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2653 _reflns_number_gt 2519 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0458P)^2^+11.3794P] 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 0.045(15) _refine_ls_number_reflns 2653 _refine_ls_number_parameters 214 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0367 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0827 _refine_ls_wR_factor_gt 0.0811 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.074 _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 O6 O 0.6705(10) 0.8064(4) 0.6117(5) 0.046(2) Uani 1 1 d . . . O5 O 0.8114(9) 0.8997(4) 0.5704(3) 0.0318(17) Uani 1 1 d . . . C6 C 0.8007(14) 0.8304(6) 0.5869(5) 0.031(3) Uani 1 1 d . . . U1 U 1.03057(5) 0.428378(19) 0.618092(18) 0.02538(13) Uani 1 1 d . . . O4 O 0.9216(9) 0.5578(4) 0.6161(4) 0.0412(18) Uani 1 1 d . . . O8 O 0.7518(10) 0.4388(5) 0.6714(4) 0.042(2) Uani 1 1 d . . . O3 O 1.1722(10) 0.5445(4) 0.5747(4) 0.0356(19) Uani 1 1 d . . . O7 O 0.8715(11) 0.3277(4) 0.6691(4) 0.043(2) Uani 1 1 d . . . C5 C 0.9424(13) 0.7781(5) 0.5749(4) 0.026(2) Uani 1 1 d . . . C8 C 0.6189(13) 0.3367(6) 0.7229(5) 0.031(3) Uani 1 1 d . . . O9 O 0.9103(9) 0.7051(4) 0.5899(4) 0.0311(17) Uani 1 1 d . . . O10 O 0.5000 0.3838(6) 0.7500 0.037(3) Uani 1 2 d S . . O2 O 1.1346(11) 0.4463(4) 0.6897(4) 0.040(2) Uani 1 1 d . . . O1 O 0.9280(9) 0.4104(4) 0.5462(3) 0.0345(18) Uani 1 1 d . . . C2 C 1.0577(13) 0.6665(5) 0.5773(4) 0.029(3) Uani 1 1 d . . . C1 C 1.0511(15) 0.5859(5) 0.5884(5) 0.032(3) Uani 1 1 d . . . C4 C 1.0994(14) 0.7875(6) 0.5544(5) 0.032(3) Uani 1 1 d . . . H4 H 1.1504 0.8318 0.5411 0.038 Uiso 1 1 calc R . . C3 C 1.1730(13) 0.7121(6) 0.5577(5) 0.026(2) Uani 1 1 d . . . H3 H 1.2829 0.6993 0.5476 0.032 Uiso 1 1 calc R . . C7 C 0.7522(15) 0.3712(6) 0.6868(5) 0.032(3) Uani 1 1 d . . . Na2 Na 0.8869(10) 1.0000 0.5000 0.0486(17) Uani 1 2 d S . . Na1 Na 0.5000 0.6145(4) 0.7500 0.080(3) Uani 1 2 d SD . . O1W O 1.0831(16) 0.9404(8) 0.4385(7) 0.109(5) Uani 1 1 d . . . O2W O 0.445(3) 0.6752(8) 0.8337(6) 0.154(7) Uani 1 1 d D . . C9 C 0.5725(17) 0.2639(7) 0.7324(5) 0.050(4) Uani 1 1 d . . . H9 H 0.6288 0.2215 0.7177 0.060 Uiso 1 1 calc R . . O3W O 0.262(3) 0.5724(14) 0.731(2) 0.50(4) Uani 1 1 d 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 O6 0.038(5) 0.021(4) 0.079(6) 0.013(4) 0.035(5) 0.009(3) O5 0.030(4) 0.020(4) 0.045(4) 0.004(3) 0.007(3) 0.003(3) C6 0.029(7) 0.027(6) 0.037(6) 0.002(5) 0.009(5) 0.007(5) U1 0.02296(19) 0.01948(18) 0.0337(2) 0.00149(18) 0.00563(17) 0.00412(16) O4 0.028(4) 0.026(4) 0.070(5) 0.006(4) 0.013(4) 0.008(3) O8 0.035(5) 0.048(6) 0.042(4) 0.005(4) 0.016(3) 0.011(4) O3 0.024(4) 0.022(4) 0.062(5) -0.001(3) 0.011(4) 0.010(3) O7 0.042(5) 0.034(4) 0.054(5) 0.000(4) 0.012(4) 0.001(4) C5 0.034(7) 0.011(4) 0.031(5) 0.008(4) 0.001(5) 0.001(4) C8 0.016(6) 0.044(7) 0.033(6) -0.004(5) 0.003(5) 0.006(5) O9 0.029(4) 0.022(4) 0.043(4) 0.000(3) 0.009(3) 0.004(3) O10 0.027(7) 0.053(7) 0.033(5) 0.000 0.006(5) 0.000 O2 0.043(5) 0.034(5) 0.043(5) 0.008(4) -0.003(4) 0.001(4) O1 0.025(4) 0.045(5) 0.034(4) -0.008(3) 0.000(3) 0.005(3) C2 0.027(7) 0.028(6) 0.032(6) -0.002(4) 0.003(5) 0.020(5) C1 0.039(7) 0.024(5) 0.033(5) -0.006(4) -0.001(5) 0.010(5) C4 0.028(6) 0.019(5) 0.050(7) -0.007(5) 0.002(5) 0.008(5) C3 0.017(5) 0.030(6) 0.032(6) 0.003(5) 0.000(4) 0.002(5) C7 0.033(7) 0.032(6) 0.032(6) -0.001(5) 0.006(5) -0.003(5) Na2 0.046(4) 0.040(4) 0.059(4) 0.011(3) 0.000 0.000 Na1 0.109(8) 0.049(4) 0.083(6) 0.000 -0.006(6) 0.000 O1W 0.070(8) 0.114(11) 0.145(12) -0.002(9) 0.055(8) -0.003(8) O2W 0.155(17) 0.088(9) 0.219(19) -0.058(10) 0.053(15) 0.015(11) C9 0.057(10) 0.047(7) 0.047(8) -0.005(5) 0.016(6) 0.005(7) O3W 0.82(9) 0.21(3) 0.48(6) 0.22(4) -0.30(6) -0.29(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 O6 C6 1.239(13) . ? O6 U1 2.440(7) 5_455 ? O5 C6 1.282(12) . ? O5 Na2 2.405(7) . ? O5 U1 2.510(7) 5_455 ? C6 C5 1.484(14) . ? C6 U1 2.846(10) 5_455 ? U1 O2 1.765(8) . ? U1 O1 1.765(7) . ? U1 O6 2.440(7) 5_545 ? U1 O7 2.446(8) . ? U1 O4 2.458(6) . ? U1 O8 2.502(7) . ? U1 O5 2.510(7) 5_545 ? U1 O3 2.526(8) . ? U1 C6 2.846(10) 5_545 ? U1 Na2 4.000(6) 5_545 ? O4 C1 1.289(14) . ? O8 C7 1.244(14) . ? O3 C1 1.247(12) . ? O3 Na2 2.467(9) 5_545 ? O7 C7 1.281(13) . ? C5 C4 1.336(15) . ? C5 O9 1.359(11) . ? C8 C9 1.360(16) . ? C8 O10 1.389(12) . ? C8 C7 1.447(15) . ? O9 C2 1.386(12) . ? O10 C8 1.389(12) 3_656 ? C2 C3 1.293(15) . ? C2 C1 1.453(14) . ? C4 C3 1.463(14) . ? Na2 O1W 2.298(13) 4_576 ? Na2 O1W 2.298(13) . ? Na2 O5 2.405(7) 4_576 ? Na2 O3 2.467(9) 8_466 ? Na2 O3 2.467(9) 5_455 ? Na2 U1 4.000(6) 8_466 ? Na2 U1 4.000(6) 5_455 ? Na1 O3W 2.075(10) . ? Na1 O3W 2.075(10) 3_656 ? Na1 O2W 2.128(9) . ? Na1 O2W 2.128(9) 3_656 ? C9 C9 1.38(3) 3_656 ? 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 C6 O6 U1 95.8(6) . 5_455 ? C6 O5 Na2 154.0(7) . . ? C6 O5 U1 91.4(6) . 5_455 ? Na2 O5 U1 109.0(3) . 5_455 ? O6 C6 O5 120.2(9) . . ? O6 C6 C5 119.7(9) . . ? O5 C6 C5 120.2(10) . . ? O6 C6 U1 58.5(5) . 5_455 ? O5 C6 U1 61.8(5) . 5_455 ? C5 C6 U1 176.4(8) . 5_455 ? O2 U1 O1 179.6(4) . . ? O2 U1 O6 89.7(4) . 5_545 ? O1 U1 O6 90.1(3) . 5_545 ? O2 U1 O7 89.5(3) . . ? O1 U1 O7 90.8(3) . . ? O6 U1 O7 67.2(3) 5_545 . ? O2 U1 O4 90.7(3) . . ? O1 U1 O4 89.5(3) . . ? O6 U1 O4 172.2(3) 5_545 . ? O7 U1 O4 120.6(3) . . ? O2 U1 O8 90.6(3) . . ? O1 U1 O8 89.8(3) . . ? O6 U1 O8 119.8(3) 5_545 . ? O7 U1 O8 52.6(3) . . ? O4 U1 O8 68.0(3) . . ? O2 U1 O5 88.2(3) . 5_545 ? O1 U1 O5 91.4(3) . 5_545 ? O6 U1 O5 52.4(2) 5_545 5_545 ? O7 U1 O5 119.6(2) . 5_545 ? O4 U1 O5 119.9(2) . 5_545 ? O8 U1 O5 172.1(2) . 5_545 ? O2 U1 O3 87.6(3) . . ? O1 U1 O3 92.1(3) . . ? O6 U1 O3 120.0(2) 5_545 . ? O7 U1 O3 172.2(2) . . ? O4 U1 O3 52.3(2) . . ? O8 U1 O3 120.1(3) . . ? O5 U1 O3 67.6(2) 5_545 . ? O2 U1 C6 87.5(4) . 5_545 ? O1 U1 C6 92.1(3) . 5_545 ? O6 U1 C6 25.7(3) 5_545 5_545 ? O7 U1 C6 92.8(3) . 5_545 ? O4 U1 C6 146.6(3) . 5_545 ? O8 U1 C6 145.4(3) . 5_545 ? O5 U1 C6 26.8(3) 5_545 5_545 ? O3 U1 C6 94.4(3) . 5_545 ? O2 U1 Na2 98.8(3) . 5_545 ? O1 U1 Na2 80.8(2) . 5_545 ? O6 U1 Na2 85.57(19) 5_545 5_545 ? O7 U1 Na2 151.56(19) . 5_545 ? O4 U1 Na2 86.71(18) . 5_545 ? O8 U1 Na2 153.1(2) . 5_545 ? O5 U1 Na2 34.64(17) 5_545 5_545 ? O3 U1 Na2 36.25(17) . 5_545 ? C6 U1 Na2 60.7(2) 5_545 5_545 ? C1 O4 U1 95.0(6) . . ? C7 O8 U1 92.6(7) . . ? C1 O3 Na2 151.2(7) . 5_545 ? C1 O3 U1 92.8(7) . . ? Na2 O3 U1 106.5(3) 5_545 . ? C7 O7 U1 94.2(6) . . ? C4 C5 O9 111.8(9) . . ? C4 C5 C6 133.7(9) . . ? O9 C5 C6 114.4(9) . . ? C9 C8 O10 108.9(10) . . ? C9 C8 C7 132.9(11) . . ? O10 C8 C7 117.9(9) . . ? C5 O9 C2 105.4(8) . . ? C8 O10 C8 106.0(12) 3_656 . ? C3 C2 O9 110.8(8) . . ? C3 C2 C1 134.0(10) . . ? O9 C2 C1 115.1(9) . . ? O3 C1 O4 119.9(9) . . ? O3 C1 C2 120.9(11) . . ? O4 C1 C2 119.0(9) . . ? C5 C4 C3 104.2(10) . . ? C2 C3 C4 107.6(10) . . ? O8 C7 O7 120.5(10) . . ? O8 C7 C8 123.0(10) . . ? O7 C7 C8 116.5(10) . . ? O1W Na2 O1W 94.3(8) 4_576 . ? O1W Na2 O5 99.0(4) 4_576 . ? O1W Na2 O5 100.6(4) . . ? O1W Na2 O5 100.6(4) 4_576 4_576 ? O1W Na2 O5 99.0(4) . 4_576 ? O5 Na2 O5 151.0(5) . 4_576 ? O1W Na2 O3 170.8(4) 4_576 8_466 ? O1W Na2 O3 87.5(4) . 8_466 ? O5 Na2 O3 89.5(3) . 8_466 ? O5 Na2 O3 70.2(3) 4_576 8_466 ? O1W Na2 O3 87.5(4) 4_576 5_455 ? O1W Na2 O3 170.8(4) . 5_455 ? O5 Na2 O3 70.2(3) . 5_455 ? O5 Na2 O3 89.5(3) 4_576 5_455 ? O3 Na2 O3 92.2(5) 8_466 5_455 ? O1W Na2 U1 134.0(3) 4_576 8_466 ? O1W Na2 U1 105.7(4) . 8_466 ? O5 Na2 U1 116.7(3) . 8_466 ? O5 Na2 U1 36.4(2) 4_576 8_466 ? O3 Na2 U1 37.26(18) 8_466 8_466 ? O3 Na2 U1 79.1(3) 5_455 8_466 ? O1W Na2 U1 105.7(4) 4_576 5_455 ? O1W Na2 U1 134.0(3) . 5_455 ? O5 Na2 U1 36.4(2) . 5_455 ? O5 Na2 U1 116.7(3) 4_576 5_455 ? O3 Na2 U1 79.1(3) 8_466 5_455 ? O3 Na2 U1 37.26(19) 5_455 5_455 ? U1 Na2 U1 89.57(16) 8_466 5_455 ? O3W Na1 O3W 137.8(15) . 3_656 ? O3W Na1 O2W 99.2(15) . . ? O3W Na1 O2W 101.8(12) 3_656 . ? O3W Na1 O2W 101.8(12) . 3_656 ? O3W Na1 O2W 99.2(15) 3_656 3_656 ? O2W Na1 O2W 119.2(9) . 3_656 ? C8 C9 C9 108.0(7) . 3_656 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.973 _refine_diff_density_min -1.039 _refine_diff_density_rms 0.159 _database_code_depnum_ccdc_archive 'CCDC 917420'