data_amurselite _audit_creation_method 'SHELXL-2019/3' _shelx_SHELXL_version_number '2019/3' _chemical_name_mineral 'amurselite' _chemical_compound_source 'Burro mine, Colorado' _chemical_formula_sum 'H20 N2 O32 Se3 U5' _chemical_formula_weight 1987.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'Se' 'Se' -0.0929 2.2259 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.598(3) _cell_length_b 9.088(3) _cell_length_c 11.071(4) _cell_angle_alpha 83.644(7) _cell_angle_beta 68.776(7) _cell_angle_gamma 79.940(8) _cell_volume 792.9(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4763 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 20.7 _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_density_diffrn 4.161 _exptl_crystal_F_000 852 _exptl_crystal_size_max 0.070 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.010 _exptl_absorpt_coefficient_mu 28.996 _shelx_estimated_absorpt_T_min 0.236 _shelx_estimated_absorpt_T_max 0.760 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.407 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Higashi2001' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_source 'Sealed Tube' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type 'Rigaku R-axis RAPID II' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_reflns_number 7606 _diffrn_reflns_av_unetI/netI 0.0715 _diffrn_reflns_av_R_equivalents 0.1174 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.093 _diffrn_reflns_theta_max 19.970 _diffrn_reflns_theta_full 19.970 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.997 _reflns_number_total 1467 _reflns_number_gt 1210 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_refinement 'SHELXL-2019/2 (Sheldrick, 2019)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0584P)^2^+13.3700P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 1467 _refine_ls_number_parameters 179 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1291 _refine_ls_wR_factor_gt 0.1206 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group N N 0.958(4) 0.012(4) 0.815(2) 0.095(9) Uani 1 1 d . . . . . U1 U 0.500000 0.000000 0.500000 0.0348(5) Uani 1 2 d S . P . . U2 U 0.43483(14) 0.71135(10) 0.26846(8) 0.0372(5) Uani 1 1 d . . . . . U3 U 0.53632(14) 0.10462(11) 0.12370(8) 0.0431(5) Uani 1 1 d . . . . . Se1 Se 0.3928(4) 0.6594(3) 0.6339(2) 0.0384(8) Uani 1 1 d . . . . . Se2 Se 0.6391(8) 0.4804(6) 0.9909(5) 0.0438(15) Uani 0.5 1 d . . P . . O1 O 0.289(2) 0.0737(17) 0.5797(13) 0.041(5) Uani 1 1 d . . . . . O2 O 0.214(2) 0.7317(17) 0.3248(14) 0.046(5) Uani 1 1 d . . . . . O3 O 0.6573(18) 0.6866(16) 0.2143(13) 0.030(4) Uiso 1 1 d . . . . . O4 O 0.341(2) 0.218(2) 0.1492(17) 0.061(6) Uani 1 1 d . . . . . O5 O 0.733(3) 0.991(2) 0.0968(17) 0.075(6) Uani 1 1 d . . . . . O6 O 0.5623(19) 0.5290(16) 0.6224(15) 0.035(4) Uani 1 1 d . . . . . O7 O 0.437(2) 0.7415(17) 0.4828(15) 0.054(5) Uani 1 1 d . . . . . O8 O 0.444(2) 0.8089(17) 0.6861(15) 0.056(5) Uani 1 1 d . . . . . O9 O 0.461(2) 0.5558(18) 0.1093(15) 0.048(5) Uiso 1 1 d . . . . . O10 O 0.697(2) 0.3057(18) 0.0554(15) 0.057(5) Uani 1 1 d . . . . . O11 O 0.4101(18) 0.9652(16) 0.3250(13) 0.032(4) Uiso 1 1 d . . . . . O12 O 0.579(3) 0.1067(18) 0.9045(15) 0.087(8) Uani 1 1 d . . . . . OW1 O 0.084(3) 0.089(2) 0.395(2) 0.085(7) Uani 1 1 d . . . . . OW2 O 0.987(4) 0.724(4) 0.949(3) 0.163(13) Uani 1 1 d . . . . . OW3A O 0.929(5) 0.733(4) 0.280(4) 0.070(11) Uiso 0.5 1 d . . P . . OW3B O 0.033(6) 0.500(5) 0.207(4) 0.085(13) Uiso 0.5 1 d . . P . . OW4A O 0.891(6) 0.628(5) 0.578(4) 0.082(14) Uiso 0.5 1 d . . P . . OW4B O 0.876(7) 0.619(6) 0.507(5) 0.107(18) Uiso 0.5 1 d . . P . . 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 N 0.08(2) 0.14(3) 0.056(17) -0.007(17) -0.014(15) -0.001(19) U1 0.0693(13) 0.0230(9) 0.0216(8) 0.0064(6) -0.0268(8) -0.0124(7) U2 0.0746(10) 0.0228(7) 0.0249(7) 0.0025(5) -0.0310(6) -0.0071(5) U3 0.0872(11) 0.0316(7) 0.0172(7) 0.0034(5) -0.0209(6) -0.0230(6) Se1 0.075(2) 0.0247(16) 0.0236(15) 0.0055(11) -0.0259(14) -0.0152(14) Se2 0.087(5) 0.030(3) 0.028(3) 0.006(2) -0.031(3) -0.021(3) O1 0.050(12) 0.038(11) 0.022(9) 0.019(8) -0.006(8) 0.003(9) O2 0.075(14) 0.034(11) 0.045(10) 0.015(8) -0.039(10) -0.022(9) O4 0.046(13) 0.073(14) 0.068(13) -0.008(11) -0.030(11) 0.002(11) O5 0.095(18) 0.067(15) 0.051(12) -0.007(10) -0.015(12) 0.001(12) O6 0.033(11) 0.017(9) 0.055(11) 0.006(8) -0.017(9) -0.001(7) O7 0.121(17) 0.028(10) 0.034(10) 0.013(8) -0.055(11) -0.013(10) O8 0.124(17) 0.028(11) 0.037(10) 0.010(8) -0.054(11) -0.020(10) O10 0.101(16) 0.037(11) 0.044(10) 0.014(9) -0.036(11) -0.023(10) O12 0.23(3) 0.029(12) 0.034(11) 0.021(9) -0.074(14) -0.062(14) OW1 0.081(17) 0.077(16) 0.086(16) 0.003(12) -0.015(13) -0.017(12) OW2 0.13(3) 0.15(3) 0.19(3) 0.00(2) -0.07(2) 0.02(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N OW3A 2.63(5) 2_766 ? N OW1 2.75(4) 2_656 ? N OW2 2.88(5) 1_545 ? N O5 3.03(3) 1_546 ? N O12 3.04(4) . ? N O2 3.11(3) 2_666 ? N O5 3.14(4) 2_766 ? N O1 3.17(3) 1_655 ? U1 O1 1.751(16) 2_656 ? U1 O1 1.751(16) . ? U1 O11 2.399(14) 2_666 ? U1 O11 2.399(14) 1_545 ? U1 O8 2.505(15) 2_666 ? U1 O8 2.505(15) 1_545 ? U1 O7 2.543(16) 2_666 ? U1 O7 2.543(16) 1_545 ? U1 Se1 3.409(3) 1_545 ? U1 Se1 3.409(3) 2_666 ? U1 U3 4.0795(15) . ? U1 U3 4.0795(15) 2_656 ? U2 O2 1.754(17) . ? U2 O3 1.766(15) . ? U2 O9 2.303(15) . ? U2 O6 2.377(14) 2_666 ? U2 O12 2.410(15) 2_666 ? U2 O11 2.411(14) . ? U2 O7 2.425(14) . ? U2 Se2 3.629(5) 1_554 ? U2 Se1 3.650(3) 2_666 ? U2 Se2 3.808(5) 2_666 ? U2 U3 3.8616(16) 1_565 ? U2 Se1 3.912(3) . ? U3 O4 1.756(18) . ? U3 O5 1.76(2) 1_545 ? U3 O12 2.318(15) 1_554 ? U3 O10 2.375(16) . ? U3 O8 2.397(14) 2_666 ? U3 O12 2.404(16) 2_656 ? U3 O11 2.420(14) 1_545 ? U3 Se2 3.689(5) 1_554 ? U3 U3 3.7834(19) 2_655 ? U3 Se1 3.884(2) 2_666 ? Se1 O6 1.685(15) . ? Se1 O7 1.693(14) . ? Se1 O8 1.717(16) . ? Se1 O10 3.280(16) 2_666 ? Se1 O6 3.344(15) 2_666 ? Se1 O3 3.417(14) 2_666 ? Se2 O9 1.705(17) 1_556 ? Se2 O9 1.720(16) 2_666 ? Se2 O10 1.735(16) 1_556 ? Se2 Se2 2.293(12) 2_667 ? Se2 OW3B 2.89(4) 2_666 ? Se2 O4 3.00(2) 2_666 ? Se2 O3 3.326(15) 1_556 ? Se2 O10 3.359(19) 2_666 ? OW4A OW4B 0.86(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag OW3A N OW1 102.1(12) 2_766 2_656 ? OW3A N OW2 150.9(16) 2_766 1_545 ? OW1 N OW2 96.5(14) 2_656 1_545 ? OW3A N O5 118.1(14) 2_766 1_546 ? OW1 N O5 127.9(13) 2_656 1_546 ? OW2 N O5 63.8(10) 1_545 1_546 ? OW3A N O12 101.8(13) 2_766 . ? OW1 N O12 84.2(9) 2_656 . ? OW2 N O12 102.2(12) 1_545 . ? O5 N O12 57.3(7) 1_546 . ? OW3A N O2 54.6(10) 2_766 2_666 ? OW1 N O2 68.9(8) 2_656 2_666 ? OW2 N O2 154.5(15) 1_545 2_666 ? O5 N O2 107.9(10) 1_546 2_666 ? O12 N O2 57.0(7) . 2_666 ? OW3A N O5 75.0(12) 2_766 2_766 ? OW1 N O5 134.8(11) 2_656 2_766 ? OW2 N O5 76.0(10) 1_545 2_766 ? O5 N O5 89.2(9) 1_546 2_766 ? O12 N O5 140.9(10) . 2_766 ? O2 N O5 129.2(12) 2_666 2_766 ? OW3A N O1 50.6(10) 2_766 1_655 ? OW1 N O1 76.2(8) 2_656 1_655 ? OW2 N O1 114.4(12) 1_545 1_655 ? O5 N O1 155.6(12) 1_546 1_655 ? O12 N O1 139.9(10) . 1_655 ? O2 N O1 83.2(8) 2_666 1_655 ? O5 N O1 67.5(7) 2_766 1_655 ? O1 U1 O1 180.0 2_656 . ? O1 U1 O11 85.3(6) 2_656 2_666 ? O1 U1 O11 94.7(6) . 2_666 ? O1 U1 O11 94.7(6) 2_656 1_545 ? O1 U1 O11 85.3(6) . 1_545 ? O11 U1 O11 180.0 2_666 1_545 ? O1 U1 O8 83.5(6) 2_656 2_666 ? O1 U1 O8 96.5(6) . 2_666 ? O11 U1 O8 117.3(5) 2_666 2_666 ? O11 U1 O8 62.7(5) 1_545 2_666 ? O1 U1 O8 96.5(6) 2_656 1_545 ? O1 U1 O8 83.5(6) . 1_545 ? O11 U1 O8 62.7(5) 2_666 1_545 ? O11 U1 O8 117.3(5) 1_545 1_545 ? O8 U1 O8 180.0 2_666 1_545 ? O1 U1 O7 94.7(7) 2_656 2_666 ? O1 U1 O7 85.3(7) . 2_666 ? O11 U1 O7 62.4(5) 2_666 2_666 ? O11 U1 O7 117.6(5) 1_545 2_666 ? O8 U1 O7 57.4(5) 2_666 2_666 ? O8 U1 O7 122.6(5) 1_545 2_666 ? O1 U1 O7 85.3(7) 2_656 1_545 ? O1 U1 O7 94.7(7) . 1_545 ? O11 U1 O7 117.6(5) 2_666 1_545 ? O11 U1 O7 62.4(5) 1_545 1_545 ? O8 U1 O7 122.6(5) 2_666 1_545 ? O8 U1 O7 57.4(5) 1_545 1_545 ? O7 U1 O7 180.0 2_666 1_545 ? O1 U1 Se1 93.1(5) 2_656 1_545 ? O1 U1 Se1 86.9(5) . 1_545 ? O11 U1 Se1 90.9(3) 2_666 1_545 ? O11 U1 Se1 89.1(3) 1_545 1_545 ? O8 U1 Se1 151.1(3) 2_666 1_545 ? O8 U1 Se1 28.9(3) 1_545 1_545 ? O7 U1 Se1 151.4(3) 2_666 1_545 ? O7 U1 Se1 28.6(3) 1_545 1_545 ? O1 U1 Se1 86.9(5) 2_656 2_666 ? O1 U1 Se1 93.1(5) . 2_666 ? O11 U1 Se1 89.1(3) 2_666 2_666 ? O11 U1 Se1 90.9(3) 1_545 2_666 ? O8 U1 Se1 28.9(3) 2_666 2_666 ? O8 U1 Se1 151.1(3) 1_545 2_666 ? O7 U1 Se1 28.6(3) 2_666 2_666 ? O7 U1 Se1 151.4(3) 1_545 2_666 ? Se1 U1 Se1 180.00(3) 1_545 2_666 ? O1 U1 U3 79.9(4) 2_656 . ? O1 U1 U3 100.1(4) . . ? O11 U1 U3 147.7(3) 2_666 . ? O11 U1 U3 32.3(3) 1_545 . ? O8 U1 U3 32.8(3) 2_666 . ? O8 U1 U3 147.2(3) 1_545 . ? O7 U1 U3 90.2(3) 2_666 . ? O7 U1 U3 89.8(3) 1_545 . ? Se1 U1 U3 118.28(4) 1_545 . ? Se1 U1 U3 61.72(4) 2_666 . ? O1 U1 U3 100.1(4) 2_656 2_656 ? O1 U1 U3 79.9(4) . 2_656 ? O11 U1 U3 32.3(3) 2_666 2_656 ? O11 U1 U3 147.7(3) 1_545 2_656 ? O8 U1 U3 147.2(3) 2_666 2_656 ? O8 U1 U3 32.8(3) 1_545 2_656 ? O7 U1 U3 89.8(3) 2_666 2_656 ? O7 U1 U3 90.2(3) 1_545 2_656 ? Se1 U1 U3 61.72(4) 1_545 2_656 ? Se1 U1 U3 118.28(4) 2_666 2_656 ? U3 U1 U3 180.0 . 2_656 ? O2 U2 O3 178.5(6) . . ? O2 U2 O9 92.7(6) . . ? O3 U2 O9 87.2(6) . . ? O2 U2 O6 88.9(6) . 2_666 ? O3 U2 O6 89.6(6) . 2_666 ? O9 U2 O6 77.4(6) . 2_666 ? O2 U2 O12 88.0(8) . 2_666 ? O3 U2 O12 93.4(8) . 2_666 ? O9 U2 O12 79.7(5) . 2_666 ? O6 U2 O12 156.7(5) 2_666 2_666 ? O2 U2 O11 88.1(6) . . ? O3 U2 O11 92.8(6) . . ? O9 U2 O11 146.5(5) . . ? O6 U2 O11 136.1(5) 2_666 . ? O12 U2 O11 66.9(5) 2_666 . ? O2 U2 O7 92.1(7) . . ? O3 U2 O7 87.3(6) . . ? O9 U2 O7 149.2(5) . . ? O6 U2 O7 72.3(5) 2_666 . ? O12 U2 O7 130.9(5) 2_666 . ? O11 U2 O7 64.1(5) . . ? O2 U2 Se2 114.0(5) . 1_554 ? O3 U2 Se2 66.0(5) . 1_554 ? O9 U2 Se2 21.4(4) . 1_554 ? O6 U2 Se2 80.4(4) 2_666 1_554 ? O12 U2 Se2 79.8(5) 2_666 1_554 ? O11 U2 Se2 139.5(3) . 1_554 ? O7 U2 Se2 141.8(4) . 1_554 ? O2 U2 Se1 110.3(5) . 2_666 ? O3 U2 Se1 68.3(5) . 2_666 ? O9 U2 Se1 73.9(4) . 2_666 ? O6 U2 Se1 21.6(4) 2_666 2_666 ? O12 U2 Se1 148.2(5) 2_666 2_666 ? O11 U2 Se1 136.6(3) . 2_666 ? O7 U2 Se1 75.9(4) . 2_666 ? Se2 U2 Se1 69.17(9) 1_554 2_666 ? O2 U2 Se2 78.7(5) . 2_666 ? O3 U2 Se2 101.4(5) . 2_666 ? O9 U2 Se2 16.2(4) . 2_666 ? O6 U2 Se2 85.5(4) 2_666 2_666 ? O12 U2 Se2 71.3(4) 2_666 2_666 ? O11 U2 Se2 136.4(3) . 2_666 ? O7 U2 Se2 156.2(4) . 2_666 ? Se2 U2 Se2 35.82(17) 1_554 2_666 ? Se1 U2 Se2 86.61(9) 2_666 2_666 ? O2 U2 U3 104.0(5) . 1_565 ? O3 U2 U3 77.4(5) . 1_565 ? O9 U2 U3 111.4(4) . 1_565 ? O6 U2 U3 163.6(4) 2_666 1_565 ? O12 U2 U3 36.6(4) 2_666 1_565 ? O11 U2 U3 37.0(3) . 1_565 ? O7 U2 U3 96.9(4) . 1_565 ? Se2 U2 U3 102.78(8) 1_554 1_565 ? Se1 U2 U3 145.10(6) 2_666 1_565 ? Se2 U2 U3 106.64(8) 2_666 1_565 ? O2 U2 Se1 86.2(5) . . ? O3 U2 Se1 92.9(4) . . ? O9 U2 Se1 135.7(4) . . ? O6 U2 Se1 58.3(4) 2_666 . ? O12 U2 Se1 144.3(4) 2_666 . ? O11 U2 Se1 77.8(3) . . ? O7 U2 Se1 15.1(4) . . ? Se2 U2 Se1 134.19(9) 1_554 . ? Se1 U2 Se1 65.23(6) 2_666 . ? Se2 U2 Se1 141.06(9) 2_666 . ? U3 U2 Se1 111.82(4) 1_565 . ? O4 U3 O5 179.6(8) . 1_545 ? O4 U3 O12 89.7(8) . 1_554 ? O5 U3 O12 89.9(8) 1_545 1_554 ? O4 U3 O10 95.0(8) . . ? O5 U3 O10 84.8(8) 1_545 . ? O12 U3 O10 82.9(6) 1_554 . ? O4 U3 O8 91.0(7) . 2_666 ? O5 U3 O8 89.3(7) 1_545 2_666 ? O12 U3 O8 155.6(6) 1_554 2_666 ? O10 U3 O8 72.8(5) . 2_666 ? O4 U3 O12 90.4(9) . 2_656 ? O5 U3 O12 89.6(9) 1_545 2_656 ? O12 U3 O12 73.5(6) 1_554 2_656 ? O10 U3 O12 155.8(6) . 2_656 ? O8 U3 O12 130.8(5) 2_666 2_656 ? O4 U3 O11 89.1(7) . 1_545 ? O5 U3 O11 91.4(7) 1_545 1_545 ? O12 U3 O11 140.4(5) 1_554 1_545 ? O10 U3 O11 136.7(5) . 1_545 ? O8 U3 O11 64.1(5) 2_666 1_545 ? O12 U3 O11 66.8(5) 2_656 1_545 ? O4 U3 Se2 74.8(6) . 1_554 ? O5 U3 Se2 105.0(7) 1_545 1_554 ? O12 U3 Se2 74.5(4) 1_554 1_554 ? O10 U3 Se2 22.1(4) . 1_554 ? O8 U3 Se2 82.1(4) 2_666 1_554 ? O12 U3 Se2 144.7(4) 2_656 1_554 ? O11 U3 Se2 142.3(4) 1_545 1_554 ? O4 U3 U3 90.1(6) . 2_655 ? O5 U3 U3 89.7(6) 1_545 2_655 ? O12 U3 U3 37.6(4) 1_554 2_655 ? O10 U3 U3 120.2(4) . 2_655 ? O8 U3 U3 166.8(4) 2_666 2_655 ? O12 U3 U3 36.0(4) 2_656 2_655 ? O11 U3 U3 102.8(3) 1_545 2_655 ? Se2 U3 U3 110.79(8) 1_554 2_655 ? O4 U3 U2 106.0(6) . 1_545 ? O5 U3 U2 74.2(7) 1_545 1_545 ? O12 U3 U2 106.6(4) 1_554 1_545 ? O10 U3 U2 156.7(4) . 1_545 ? O8 U3 U2 96.6(4) 2_666 1_545 ? O12 U3 U2 36.7(4) 2_656 1_545 ? O11 U3 U2 36.8(3) 1_545 1_545 ? Se2 U3 U2 178.58(8) 1_554 1_545 ? U3 U3 U2 70.48(4) 2_655 1_545 ? O4 U3 Se1 88.1(6) . 2_666 ? O5 U3 Se1 92.2(6) 1_545 2_666 ? O12 U3 Se1 139.7(4) 1_554 2_666 ? O10 U3 Se1 57.3(4) . 2_666 ? O8 U3 Se1 16.1(4) 2_666 2_666 ? O12 U3 Se1 146.7(4) 2_656 2_666 ? O11 U3 Se1 79.9(3) 1_545 2_666 ? Se2 U3 Se1 66.07(8) 1_554 2_666 ? U3 U3 Se1 176.70(5) 2_655 2_666 ? U2 U3 Se1 112.66(4) 1_545 2_666 ? O4 U3 N 135.0(7) . 1_554 ? O5 U3 N 44.5(7) 1_545 1_554 ? O12 U3 N 48.7(7) 1_554 1_554 ? O10 U3 N 67.3(7) . 1_554 ? O8 U3 N 119.4(6) 2_666 1_554 ? O12 U3 N 92.4(7) 2_656 1_554 ? O11 U3 N 132.7(6) 1_545 1_554 ? Se2 U3 N 77.5(5) 1_554 1_554 ? U3 U3 N 67.8(4) 2_655 1_554 ? U2 U3 N 102.6(5) 1_545 1_554 ? Se1 U3 N 111.8(4) 2_666 1_554 ? O6 Se1 O7 104.2(8) . . ? O6 Se1 O8 101.8(8) . . ? O7 Se1 O8 90.6(7) . . ? O6 Se1 O10 93.2(6) . 2_666 ? O7 Se1 O10 148.3(6) . 2_666 ? O8 Se1 O10 59.6(6) . 2_666 ? O6 Se1 O6 76.5(6) . 2_666 ? O7 Se1 O6 57.8(6) . 2_666 ? O8 Se1 O6 145.8(6) . 2_666 ? O10 Se1 O6 153.6(4) 2_666 2_666 ? O6 Se1 U1 112.6(5) . 1_565 ? O7 Se1 U1 46.0(5) . 1_565 ? O8 Se1 U1 44.9(5) . 1_565 ? O10 Se1 U1 102.9(3) 2_666 1_565 ? O6 Se1 U1 103.4(2) 2_666 1_565 ? O6 Se1 O3 59.7(6) . 2_666 ? O7 Se1 O3 139.1(6) . 2_666 ? O8 Se1 O3 127.9(5) . 2_666 ? O10 Se1 O3 72.5(4) 2_666 2_666 ? O6 Se1 O3 81.4(3) 2_666 2_666 ? U1 Se1 O3 170.2(3) 1_565 2_666 ? O6 Se1 U2 31.3(5) . 2_666 ? O7 Se1 U2 128.3(6) . 2_666 ? O8 Se1 U2 116.3(5) . 2_666 ? O10 Se1 U2 78.7(3) 2_666 2_666 ? O6 Se1 U2 80.2(2) 2_666 2_666 ? U1 Se1 U2 142.84(9) 1_565 2_666 ? O3 Se1 U2 28.7(2) 2_666 2_666 ? O9 Se2 O9 95.9(8) 1_556 2_666 ? O9 Se2 O10 104.9(8) 1_556 1_556 ? O9 Se2 O10 104.5(8) 2_666 1_556 ? O9 Se2 Se2 48.2(6) 1_556 2_667 ? O9 Se2 Se2 47.7(6) 2_666 2_667 ? O10 Se2 Se2 112.3(7) 1_556 2_667 ? O9 Se2 OW3B 151.9(10) 1_556 2_666 ? O9 Se2 OW3B 97.4(10) 2_666 2_666 ? O10 Se2 OW3B 95.5(11) 1_556 2_666 ? Se2 Se2 OW3B 138.8(9) 2_667 2_666 ? O9 Se2 O4 89.0(7) 1_556 2_666 ? O9 Se2 O4 85.7(6) 2_666 2_666 ? O10 Se2 O4 161.5(8) 1_556 2_666 ? Se2 Se2 O4 86.1(4) 2_667 2_666 ? OW3B Se2 O4 67.6(9) 2_666 2_666 ? O9 Se2 O3 58.4(6) 1_556 1_556 ? O9 Se2 O3 149.8(7) 2_666 1_556 ? O10 Se2 O3 98.1(6) 1_556 1_556 ? Se2 Se2 O3 105.0(4) 2_667 1_556 ? OW3B Se2 O3 100.3(9) 2_666 1_556 ? O4 Se2 O3 78.7(4) 2_666 1_556 ? O9 Se2 O10 54.0(6) 1_556 2_666 ? O9 Se2 O10 53.9(6) 2_666 2_666 ? O10 Se2 O10 140.8(5) 1_556 2_666 ? Se2 Se2 O10 28.6(3) 2_667 2_666 ? OW3B Se2 O10 117.7(9) 2_666 2_666 ? O4 Se2 O10 57.5(4) 2_666 2_666 ? O3 Se2 O10 96.0(4) 1_556 2_666 ? U1 O1 N 143.2(9) . 1_455 ? U1 O1 Se1 65.3(4) . 1_545 ? N O1 Se1 80.2(6) 1_455 1_545 ? U1 O1 Se1 60.4(4) . 2_666 ? N O1 Se1 151.5(8) 1_455 2_666 ? Se1 O1 Se1 125.7(4) 1_545 2_666 ? U2 O2 N 115.1(8) . 2_666 ? U2 O2 Se2 74.9(5) . 2_666 ? N O2 Se2 86.9(6) 2_666 2_666 ? U2 O3 Se2 85.0(5) . 1_554 ? U2 O3 Se1 83.0(5) . 2_666 ? Se2 O3 Se1 75.6(3) 1_554 2_666 ? U3 O4 Se2 114.7(8) . 2_666 ? U3 O4 N 108.1(9) . 2_656 ? Se2 O4 N 126.1(7) 2_666 2_656 ? U3 O4 Se2 77.5(6) . 1_554 ? Se2 O4 Se2 38.9(3) 2_666 1_554 ? N O4 Se2 158.2(7) 2_656 1_554 ? U3 O5 N 111.4(10) 1_565 1_564 ? U3 O5 N 135.4(10) 1_565 2_766 ? N O5 N 90.8(9) 1_564 2_766 ? Se1 O6 U2 127.1(8) . 2_666 ? Se1 O6 Se1 103.5(6) . 2_666 ? U2 O6 Se1 84.5(4) 2_666 2_666 ? Se1 O6 Se2 82.7(6) . 2_667 ? U2 O6 Se2 63.7(3) 2_666 2_667 ? Se1 O6 Se2 142.3(4) 2_666 2_667 ? Se1 O7 U2 143.0(9) . . ? Se1 O7 U1 105.4(7) . 1_565 ? U2 O7 U1 111.2(5) . 1_565 ? Se1 O7 Se1 85.2(6) . 2_666 ? U2 O7 Se1 66.5(4) . 2_666 ? U1 O7 Se1 148.0(7) 1_565 2_666 ? Se1 O8 U3 141.0(8) . 2_666 ? Se1 O8 U1 106.2(6) . 1_565 ? U3 O8 U1 112.6(6) 2_666 1_565 ? Se1 O8 N 92.6(9) . 1_465 ? U3 O8 N 86.0(6) 2_666 1_465 ? U1 O8 N 87.9(6) 1_565 1_465 ? Se1 O8 Se2 78.5(5) . 2_667 ? U3 O8 Se2 62.6(3) 2_666 2_667 ? U1 O8 Se2 175.3(6) 1_565 2_667 ? N O8 Se2 91.9(5) 1_465 2_667 ? Se2 O9 Se2 84.1(8) 1_554 2_666 ? Se2 O9 U2 129.2(8) 1_554 . ? Se2 O9 U2 141.9(9) 2_666 . ? Se2 O9 Se1 90.9(6) 1_554 2_666 ? Se2 O9 Se1 136.0(7) 2_666 2_666 ? U2 O9 Se1 69.8(4) . 2_666 ? Se2 O10 U3 127.0(9) 1_554 . ? Se2 O10 Se1 106.9(7) 1_554 2_666 ? U3 O10 Se1 85.2(4) . 2_666 ? Se2 O10 Se2 39.2(5) 1_554 2_666 ? U3 O10 Se2 88.3(5) . 2_666 ? Se1 O10 Se2 100.8(5) 2_666 2_666 ? Se2 O10 N 116.6(8) 1_554 1_554 ? U3 O10 N 77.5(6) . 1_554 ? Se1 O10 N 135.2(6) 2_666 1_554 ? Se2 O10 N 119.3(6) 2_666 1_554 ? U1 O11 U2 116.9(6) 1_565 . ? U1 O11 U3 115.7(6) 1_565 1_565 ? U2 O11 U3 106.1(5) . 1_565 ? U1 O11 N 149.5(7) 1_565 2_666 ? U2 O11 N 77.4(6) . 2_666 ? U3 O11 N 82.3(5) 1_565 2_666 ? U1 O11 Se1 55.5(3) 1_565 . ? U2 O11 Se1 67.5(3) . . ? U3 O11 Se1 157.3(5) 1_565 . ? N O11 Se1 115.8(6) 2_666 . ? U3 O12 U3 106.5(6) 1_556 2_656 ? U3 O12 U2 137.8(8) 1_556 2_666 ? U3 O12 U2 106.7(6) 2_656 2_666 ? U3 O12 N 96.3(8) 1_556 . ? U3 O12 N 105.7(9) 2_656 . ? U2 O12 N 99.1(9) 2_666 . ? U3 O12 Se2 69.4(4) 1_556 . ? U3 O12 Se2 165.0(10) 2_656 . ? U2 O12 Se2 71.8(4) 2_666 . ? N O12 Se2 89.2(8) . . ? U3 O12 Se2 74.9(5) 1_556 2_667 ? U3 O12 Se2 131.3(9) 2_656 2_667 ? U2 O12 Se2 63.7(4) 2_666 2_667 ? N O12 Se2 122.8(8) . 2_667 ? Se2 O12 Se2 34.2(2) . 2_667 ? N OW2 Se2 127.1(13) 1_565 2_767 ? N OW2 Se2 116.3(12) 1_565 . ? Se2 OW2 Se2 114.5(8) 2_767 . ? N OW2 N 78.5(11) 1_565 2_767 ? Se2 OW2 N 78.8(7) 2_767 2_767 ? Se2 OW2 N 131.9(9) . 2_767 ? N OW2 Se1 80.2(10) 1_565 1_655 ? Se2 OW2 Se1 65.6(5) 2_767 1_655 ? Se2 OW2 Se1 115.5(8) . 1_655 ? N OW2 Se1 112.0(9) 2_767 1_655 ? N OW3A Se2 87.9(11) 2_766 2_766 ? Se2 OW3B Se1 154.2(14) 2_666 2_566 ? OW4B OW4A Se1 69(5) . . ? OW4A OW4B Se1 99(6) . . ? _refine_diff_density_max 2.257 _refine_diff_density_min -1.373 _refine_diff_density_rms 0.339 _shelx_res_file ; TITL uranylselenite 16942.res created by SHELXL-2019/3 at 23:33:09 on 19-Jul-2024 CELL 0.71075 8.59820 9.08800 11.07090 83.64430 68.77570 79.93990 ZERR 1 0.00290 0.00280 0.00350 0.00690 0.00720 0.00820 LATT 1 SFAC H O SE U N UNIT 20 32 3 5 2 L.S. 20 CONN 8 3 N CONN 8 3 SE1 CONN 8 3 SE2 FMAP 2 ACTA PLAN 10 SIZE 0.070 0.050 0.010 WGHT 0.058400 13.370000 FVAR 0.21496 N 5 0.958117 0.012043 0.814680 11.00000 0.07584 0.14075 = 0.05570 -0.00713 -0.01413 -0.00150 U1 4 0.500000 0.000000 0.500000 10.50000 0.06927 0.02298 = 0.02162 0.00637 -0.02677 -0.01243 U2 4 0.434833 0.711354 0.268457 11.00000 0.07455 0.02278 = 0.02488 0.00253 -0.03095 -0.00710 U3 4 0.536323 0.104624 0.123696 11.00000 0.08721 0.03158 = 0.01722 0.00342 -0.02094 -0.02295 SE1 3 0.392758 0.659368 0.633928 11.00000 0.07540 0.02466 = 0.02365 0.00549 -0.02587 -0.01525 SE2 3 0.639124 0.480400 0.990858 10.50000 0.08670 0.02966 = 0.02760 0.00630 -0.03136 -0.02102 O1 2 0.289030 0.073656 0.579664 11.00000 0.04956 0.03793 = 0.02241 0.01916 -0.00579 0.00274 O2 2 0.213877 0.731655 0.324803 11.00000 0.07506 0.03399 = 0.04523 0.01531 -0.03859 -0.02157 O3 2 0.657274 0.686625 0.214307 11.00000 0.02997 O4 2 0.340869 0.218141 0.149198 11.00000 0.04609 0.07339 = 0.06808 -0.00768 -0.03033 0.00154 O5 2 0.732890 0.991091 0.096824 11.00000 0.09482 0.06678 = 0.05069 -0.00682 -0.01516 0.00150 O6 2 0.562278 0.528979 0.622417 11.00000 0.03273 0.01674 = 0.05469 0.00607 -0.01715 -0.00062 O7 2 0.436904 0.741516 0.482756 11.00000 0.12064 0.02781 = 0.03388 0.01262 -0.05542 -0.01258 O8 2 0.444338 0.808893 0.686117 11.00000 0.12418 0.02849 = 0.03686 0.01010 -0.05388 -0.01981 O9 2 0.461412 0.555750 0.109303 11.00000 0.04824 O10 2 0.697030 0.305673 0.055445 11.00000 0.10074 0.03652 = 0.04415 0.01417 -0.03642 -0.02278 O11 2 0.410102 0.965210 0.325037 11.00000 0.03217 O12 2 0.578645 0.106674 0.904488 11.00000 0.23166 0.02897 = 0.03447 0.02119 -0.07351 -0.06231 OW1 2 0.083846 0.089001 0.395253 11.00000 0.08074 0.07663 = 0.08593 0.00287 -0.01508 -0.01652 OW2 2 0.986548 0.723814 0.949090 11.00000 0.13408 0.15403 = 0.19221 -0.00072 -0.06709 0.01908 OW3A 2 0.929405 0.732962 0.279850 10.50000 0.06995 OW3B 2 0.033457 0.500016 0.206785 10.50000 0.08493 OW4A 2 0.891392 0.628057 0.577548 10.50000 0.08214 OW4B 2 0.875914 0.619210 0.506511 10.50000 0.10731 HKLF 4 REM uranylselenite REM wR2 = 0.1291, GooF = S = 1.070, Restrained GooF = 1.070 for all data REM R1 = 0.0505 for 1210 Fo > 4sig(Fo) and 0.0611 for all 1467 data REM 179 parameters refined using 0 restraints END WGHT 0.0584 13.3585 REM Highest difference peak 2.257, deepest hole -1.373, 1-sigma level 0.339 Q1 1 0.6943 1.0846 0.0736 11.00000 0.05 2.26 Q2 1 0.3447 0.0073 0.5441 11.00000 0.05 2.06 Q3 1 0.5881 0.6969 0.2222 11.00000 0.05 2.04 Q4 1 0.4411 0.8446 0.2806 11.00000 0.05 1.89 Q5 1 0.4973 0.9604 0.2920 11.00000 0.05 1.64 Q6 1 0.5015 0.0265 0.9002 11.00000 0.05 1.50 Q7 1 0.3699 0.1235 0.1660 11.00000 0.05 1.49 Q8 1 0.7919 0.6045 0.0596 11.00000 0.05 1.48 Q9 1 0.4295 0.5787 0.2395 11.00000 0.05 1.39 Q10 1 0.9357 0.7977 0.1782 11.00000 0.05 1.35 ; _shelx_res_checksum 33010 _shelx_hkl_file ; 0 0 2 112.32 6.85 0 0 2 113.53 7.59 0 0 2 103.30 4.70 0 0 -2 113.76 7.65 0 0 -2 133.81 8.48 0 0 -2 121.85 7.08 0 0 3 128.85 9.81 0 0 3 120.00 10.02 0 0 3 118.63 10.83 0 0 -3 123.47 10.03 0 0 -3 142.42 10.87 0 0 -3 124.72 12.09 0 0 4 17.90 8.70 0 0 4 7.10 5.23 0 0 4 16.34 9.68 0 0 -4 20.41 9.72 0 0 -4 1.56 10.83 0 0 -4 13.69 3.55 0 0 5 1540.06 126.25 0 0 5 1490.80 115.58 0 0 5 1477.28 108.14 0 0 -5 1717.50 129.23 0 0 -5 1700.62 137.01 0 0 -5 1748.55 129.46 0 0 6 9.66 10.96 0 0 6 3.87 6.23 0 0 6 21.57 12.73 0 0 -6 13.89 12.22 0 0 -6 4.59 7.67 0 0 -6 -1.87 13.27 0 0 7 117.76 17.35 0 0 7 146.69 31.62 0 0 7 138.04 22.07 0 0 -7 155.65 22.57 0 0 -7 140.40 21.33 0 0 -7 118.35 13.37 0 0 8 2003.07 213.01 0 0 8 1837.18 304.44 0 0 8 1638.46 169.13 0 0 -8 2146.64 224.08 0 0 -8 2152.52 318.91 0 0 -8 1955.39 216.19 0 0 9 32.77 13.36 0 0 9 20.16 16.05 0 0 -9 26.58 25.85 0 0 -9 35.45 16.90 0 1 -9 98.34 36.23 0 1 -9 108.22 37.68 0 1 -9 90.64 24.72 0 -1 9 70.79 35.76 0 -1 9 47.51 19.91 0 -1 9 68.01 21.34 0 1 -8 4.12 11.83 0 1 -8 8.34 10.53 0 1 -8 8.22 10.89 0 -1 8 -0.40 15.90 0 -1 8 2.49 10.31 0 1 -7 4.87 8.80 0 1 -7 20.09 13.78 0 1 -7 1.43 13.23 0 -1 7 0.43 8.12 0 -1 7 -2.20 7.90 0 -1 7 -4.43 7.63 0 1 -6 260.53 21.10 0 1 -6 310.00 48.88 0 1 -6 312.26 29.49 0 -1 6 235.37 18.58 0 -1 6 309.02 45.97 0 -1 6 289.70 29.05 0 1 -5 5704.12 605.51 0 1 -5 6314.21 730.15 0 1 -5 6379.62 815.68 0 -1 5 5509.66 637.16 0 -1 5 5993.47 813.12 0 1 -4 626.24 33.87 0 1 -4 669.75 42.47 0 1 -4 578.91 39.92 0 -1 4 603.35 42.37 0 -1 4 619.39 45.81 0 -1 4 626.08 39.66 0 1 -3 61.09 13.39 0 1 -3 92.33 15.51 0 1 -3 67.51 11.81 0 -1 3 66.13 11.03 0 -1 3 106.97 8.08 0 -1 3 96.04 15.21 0 1 -2 1189.28 50.16 0 1 -2 1017.10 53.29 0 1 -2 1018.52 45.36 0 -1 2 1036.65 45.08 0 -1 2 1158.46 48.96 0 -1 2 1170.84 56.68 0 1 -1 142.18 7.20 0 -1 1 141.63 7.87 0 -1 1 127.39 6.46 0 -1 1 158.39 10.24 0 1 2 3.53 6.34 0 1 2 1.53 4.69 0 -1 -2 3.71 4.64 0 -1 -2 6.45 4.46 0 1 3 9351.65 1399.89 0 1 3 9307.93 1106.16 0 -1 -3 9492.41 1250.15 0 -1 -3 9840.56 1242.98 0 -1 -3 9999.00 1358.72 0 1 4 110.30 14.26 0 1 4 133.45 10.86 0 1 4 107.10 9.20 0 -1 -4 102.45 11.43 0 -1 -4 141.96 19.29 0 1 5 44.18 11.94 0 1 5 44.67 14.75 0 1 5 29.36 5.93 0 -1 -5 18.74 7.89 0 -1 -5 48.11 13.63 0 -1 -5 23.06 15.55 0 1 6 -2.32 5.77 0 1 6 -0.09 4.67 0 1 6 6.40 11.34 0 -1 -6 -2.30 6.67 0 -1 -6 6.88 11.83 0 -1 -6 4.83 6.27 0 1 7 5.52 7.96 0 1 7 -3.42 5.39 0 -1 -7 -4.89 7.51 0 -1 -7 -0.86 14.77 0 -1 -7 12.81 7.80 0 1 8 531.17 48.74 0 1 8 546.20 70.25 0 1 8 670.89 69.82 0 -1 -8 710.24 108.37 0 -1 -8 663.33 81.48 0 -1 -8 565.86 65.64 0 1 9 2.77 17.50 0 1 9 4.83 18.78 0 -1 -9 2.81 11.57 0 -1 -9 -30.54 13.32 0 -1 -9 20.89 8.05 0 2 -9 456.08 92.47 0 2 -9 403.81 91.27 0 2 -9 376.11 42.15 0 -2 9 312.91 42.33 0 -2 9 255.47 79.56 0 -2 9 345.74 57.77 0 2 -8 152.18 21.71 0 2 -8 216.46 48.84 0 2 -8 168.84 29.91 0 -2 8 166.47 29.82 0 -2 8 135.11 26.48 0 -2 8 177.61 35.89 0 2 -7 921.42 108.26 0 2 -7 993.97 136.82 0 2 -7 976.60 94.38 0 -2 7 869.38 123.77 0 -2 7 702.85 88.90 0 -2 7 838.57 103.79 0 2 -6 152.85 19.19 0 2 -6 132.28 19.53 0 2 -6 151.82 24.29 0 -2 6 134.75 15.93 0 -2 6 130.39 20.62 0 -2 6 132.94 29.94 0 2 -5 -5.09 8.94 0 2 -5 21.05 10.71 0 2 -5 17.64 10.78 0 -2 5 8.02 11.40 0 -2 5 4.75 5.63 0 -2 5 8.42 6.52 0 2 -4 151.99 18.49 0 2 -4 104.39 11.82 0 2 -4 175.17 22.35 0 -2 4 113.94 12.65 0 -2 4 119.09 12.03 0 -2 4 138.81 13.60 0 2 -3 1342.89 108.49 0 2 -3 1226.06 87.14 0 -2 3 1197.50 78.71 0 -2 3 1153.02 63.95 0 -2 3 1100.31 66.55 0 2 -2 7522.07 777.10 0 2 -2 8489.57 964.30 0 -2 2 7820.59 905.22 0 -2 2 7769.24 801.04 0 -2 2 6364.84 713.06 0 2 -1 901.84 37.26 0 2 -1 1210.42 78.05 0 2 -1 884.46 43.96 0 -2 1 1126.13 57.42 0 -2 1 881.72 42.63 0 -2 1 833.96 35.42 0 2 0 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